#==================== data_global _publ_contact_author ; Prof. Kristin Bowman-James Department of Chemistry University of Kansas 2010 Malott Hall 1251 Wescoe Hall Dr. Lawrence, KS 66045-7582 USA ; _publ_contact_author_email kbowmanjames@ku.edu _publ_contact_author_fax 1(785)8645396 _publ_contact_author_phone 1(785)8644673 _publ_requested_journal 'Inorganic Chemistry' loop_ _publ_author_name _publ_author_address 'Hossain, Md. Alamgir' ; Department of Chemistry University of Kansas 2010 Malott Hall 1251 Wescoe Hall Dr. Lawrence, KS 66045-7582 USA ; 'Morehouse, Paula' ; Department of Chemistry University of Kansas 2010 Malott Hall 1251 Wescoe Hall Dr. Lawrence, KS 66045-7582 USA ; 'Powell, Douglas' ; Department of Chemistry University of Kansas 2010 Malott Hall 1251 Wescoe Hall Dr. Lawrence, KS 66045-7582 USA ; 'Bowman-James, Kristin' ; Department of Chemistry University of Kansas 2010 Malott Hall 1251 Wescoe Hall Dr. Lawrence, KS 66045-7582 USA ; _publ_section_title ; To Cascade or Not: Ditopic Complexes of Halides with Azacryptands. ; #==================== data_compound_1_ #data_01024 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C36 H60 N8) 6+, 2(Si F6) 2-, 2F 1-, 13(H2 O)' _chemical_formula_sum 'C36 H86 F14 N8 O13 Si2' _chemical_formula_weight 1161.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8304(11) _cell_length_b 15.9973(19) _cell_length_c 17.417(2) _cell_angle_alpha 84.404(3) _cell_angle_beta 89.959(3) _cell_angle_gamma 77.098(2) _cell_volume 2656.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9504 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 30.58 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8936 _exptl_absorpt_correction_T_max 0.9632 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '\w scan frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 344 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -2.06 _diffrn_reflns_number 22911 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 30.64 _reflns_number_total 15608 _reflns_number_gt 12226 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15608 _refine_ls_number_parameters 655 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.26869(11) 0.85793(7) 0.22081(6) 0.0128(2) Uani 1 1 d . . . C2 C 0.23074(14) 0.88237(9) 0.29845(8) 0.0154(3) Uani 1 1 d . . . H2A H 0.2038 0.9460 0.2966 0.019 Uiso 1 1 calc R . . H2B H 0.3130 0.8619 0.3337 0.019 Uiso 1 1 calc R . . C3 C 0.11197(14) 0.84506(9) 0.32970(8) 0.0153(3) Uani 1 1 d . . . H3A H 0.0809 0.8698 0.3784 0.018 Uiso 1 1 calc R . . H3B H 0.0325 0.8613 0.2923 0.018 Uiso 1 1 calc R . . N4 N 0.15289(11) 0.74927(7) 0.34450(7) 0.0139(2) Uani 1 1 d . . . H4A H 0.2157 0.7341 0.3854 0.017 Uiso 1 1 calc R . . H4B H 0.1957 0.7266 0.3018 0.017 Uiso 1 1 calc R . . C5 C 0.02803(14) 0.71276(9) 0.36225(9) 0.0181(3) Uani 1 1 d . . . H5A H -0.0405 0.7310 0.3189 0.022 Uiso 1 1 calc R . . H5B H -0.0164 0.7364 0.4089 0.022 Uiso 1 1 calc R . . C6 C 0.06383(13) 0.61656(9) 0.37536(8) 0.0155(3) Uani 1 1 d . . . C7 C 0.12475(14) 0.57472(9) 0.44463(8) 0.0175(3) Uani 1 1 d . . . H7A H 0.1470 0.6073 0.4837 0.021 Uiso 1 1 calc R . . C8 C 0.15314(15) 0.48588(9) 0.45709(8) 0.0183(3) Uani 1 1 d . . . H8A H 0.1955 0.4576 0.5045 0.022 Uiso 1 1 calc R . . C9 C 0.03334(14) 0.56818(10) 0.31821(8) 0.0184(3) Uani 1 1 d . . . H9A H -0.0062 0.5962 0.2701 0.022 Uiso 1 1 calc R . . C10 C 0.06044(14) 0.47955(10) 0.33126(9) 0.0185(3) Uani 1 1 d . . . H10A H 0.0380 0.4469 0.2923 0.022 Uiso 1 1 calc R . . C11 C 0.11991(14) 0.43753(9) 0.40048(8) 0.0168(3) Uani 1 1 d . . . C12 C 0.14741(15) 0.34132(9) 0.41520(9) 0.0201(3) Uani 1 1 d . . . H12A H 0.1269 0.3250 0.4696 0.024 Uiso 1 1 calc R . . H12B H 0.0851 0.3193 0.3816 0.024 Uiso 1 1 calc R . . N13 N 0.29611(12) 0.30157(7) 0.39950(7) 0.0150(2) Uani 1 1 d . . . H13A H 0.3126 0.3147 0.3482 0.018 Uiso 1 1 calc R . . H13B H 0.3531 0.3258 0.4281 0.018 Uiso 1 1 calc R . . C14 C 0.33465(15) 0.20594(9) 0.41775(8) 0.0174(3) Uani 1 1 d . . . H14A H 0.2956 0.1903 0.4682 0.021 Uiso 1 1 calc R . . H14B H 0.4375 0.1867 0.4222 0.021 Uiso 1 1 calc R . . C15 C 0.28097(15) 0.15975(9) 0.35653(8) 0.0165(3) Uani 1 1 d . . . H15A H 0.3038 0.0970 0.3724 0.020 Uiso 1 1 calc R . . H15B H 0.1781 0.1791 0.3520 0.020 Uiso 1 1 calc R . . N16 N 0.34177(11) 0.17613(7) 0.28117(6) 0.0128(2) Uani 1 1 d . . . C17 C 0.48555(14) 0.12514(9) 0.27802(8) 0.0147(2) Uani 1 1 d . . . H17A H 0.4833 0.0665 0.2653 0.018 Uiso 1 1 calc R . . H17B H 0.5311 0.1197 0.3295 0.018 Uiso 1 1 calc R . . C18 C 0.57093(14) 0.16501(9) 0.21902(8) 0.0147(3) Uani 1 1 d . . . H18A H 0.6656 0.1274 0.2181 0.018 Uiso 1 1 calc R . . H18B H 0.5271 0.1689 0.1673 0.018 Uiso 1 1 calc R . . N19 N 0.58248(11) 0.25254(7) 0.23615(7) 0.0137(2) Uani 1 1 d . . . H19A H 0.6210 0.2492 0.2848 0.016 Uiso 1 1 calc R . . H19B H 0.4947 0.2880 0.2356 0.016 Uiso 1 1 calc R . . C20 C 0.67063(14) 0.29086(9) 0.17872(8) 0.0163(3) Uani 1 1 d . . . H20A H 0.6362 0.2880 0.1258 0.020 Uiso 1 1 calc R . . H20B H 0.7682 0.2570 0.1839 0.020 Uiso 1 1 calc R . . C21 C 0.66652(13) 0.38282(9) 0.19093(8) 0.0144(2) Uani 1 1 d . . . C22 C 0.72760(14) 0.40274(9) 0.25695(8) 0.0159(3) Uani 1 1 d . . . H22A H 0.7758 0.3578 0.2933 0.019 Uiso 1 1 calc R . . C23 C 0.71805(14) 0.48795(9) 0.26961(8) 0.0157(3) Uani 1 1 d . . . H23A H 0.7568 0.5010 0.3157 0.019 Uiso 1 1 calc R . . C24 C 0.60081(14) 0.44943(9) 0.13745(8) 0.0170(3) Uani 1 1 d . . . H24A H 0.5591 0.4365 0.0922 0.020 Uiso 1 1 calc R . . C25 C 0.59503(14) 0.53473(9) 0.14899(8) 0.0174(3) Uani 1 1 d . . . H25A H 0.5516 0.5796 0.1112 0.021 Uiso 1 1 calc R . . C26 C 0.65260(13) 0.55473(9) 0.21579(8) 0.0145(3) Uani 1 1 d . . . C27 C 0.65329(14) 0.64508(9) 0.23148(9) 0.0174(3) Uani 1 1 d . . . H27A H 0.6653 0.6462 0.2878 0.021 Uiso 1 1 calc R . . H27B H 0.7351 0.6615 0.2063 0.021 Uiso 1 1 calc R . . N28 N 0.52521(11) 0.71101(7) 0.20445(7) 0.0146(2) Uani 1 1 d . . . H28A H 0.5246 0.7208 0.1515 0.018 Uiso 1 1 calc R . . H28B H 0.4472 0.6908 0.2184 0.018 Uiso 1 1 calc R . . C29 C 0.52139(14) 0.79329(9) 0.23898(8) 0.0159(3) Uani 1 1 d . . . H29A H 0.6135 0.8083 0.2330 0.019 Uiso 1 1 calc R . . H29B H 0.5041 0.7849 0.2949 0.019 Uiso 1 1 calc R . . C30 C 0.40988(14) 0.86720(9) 0.20216(8) 0.0151(3) Uani 1 1 d . . . H30A H 0.4238 0.9218 0.2198 0.018 Uiso 1 1 calc R . . H30B H 0.4200 0.8708 0.1454 0.018 Uiso 1 1 calc R . . C31 C 0.16701(14) 0.90676(9) 0.16243(8) 0.0146(2) Uani 1 1 d . . . H31A H 0.1895 0.9634 0.1475 0.018 Uiso 1 1 calc R . . H31B H 0.0727 0.9173 0.1847 0.018 Uiso 1 1 calc R . . C32 C 0.16639(14) 0.85930(9) 0.09112(8) 0.0151(3) Uani 1 1 d . . . H32A H 0.0931 0.8928 0.0542 0.018 Uiso 1 1 calc R . . H32B H 0.2576 0.8539 0.0657 0.018 Uiso 1 1 calc R . . N33 N 0.13966(9) 0.77188(6) 0.11193(5) 0.0136(2) Uani 1 1 d . . . H33A H 0.0516 0.7772 0.1317 0.016 Uiso 1 1 calc R . . H33B H 0.2029 0.7428 0.1496 0.016 Uiso 1 1 calc R . . C34 C 0.15130(9) 0.72081(6) 0.04329(5) 0.0157(3) Uani 1 1 d R . . H34A H 0.2450 0.7164 0.0210 0.019 Uiso 1 1 calc R . . H34B H 0.0811 0.7511 0.0034 0.019 Uiso 1 1 calc R . . C35 C 0.12850(14) 0.63174(9) 0.06557(8) 0.0145(2) Uani 1 1 d . . . C36 C 0.23964(15) 0.56110(10) 0.07293(10) 0.0221(3) Uani 1 1 d . . . H36A H 0.3314 0.5688 0.0632 0.027 Uiso 1 1 calc R . . C37 C 0.21897(15) 0.47885(10) 0.09443(10) 0.0230(3) Uani 1 1 d . . . H37A H 0.2962 0.4307 0.0987 0.028 Uiso 1 1 calc R . . C38 C -0.00464(14) 0.61922(9) 0.07921(9) 0.0186(3) Uani 1 1 d . . . H38A H -0.0823 0.6670 0.0734 0.022 Uiso 1 1 calc R . . C39 C -0.02546(14) 0.53782(9) 0.10113(8) 0.0175(3) Uani 1 1 d . . . H39A H -0.1173 0.5302 0.1105 0.021 Uiso 1 1 calc R . . C40 C 0.08620(14) 0.46709(9) 0.10961(8) 0.0144(2) Uani 1 1 d . . . C41 C 0.05472(14) 0.38056(9) 0.13166(8) 0.0160(3) Uani 1 1 d . . . H41A H -0.0204 0.3872 0.1700 0.019 Uiso 1 1 calc R . . H41B H 0.0189 0.3604 0.0854 0.019 Uiso 1 1 calc R . . N42 N 0.17583(11) 0.31332(7) 0.16451(6) 0.0130(2) Uani 1 1 d . . . H42A H 0.2192 0.3349 0.2024 0.016 Uiso 1 1 calc R . . H42B H 0.2392 0.2990 0.1264 0.016 Uiso 1 1 calc R . . C43 C 0.13108(14) 0.23463(9) 0.19780(8) 0.0150(3) Uani 1 1 d . . . H43A H 0.0697 0.2177 0.1600 0.018 Uiso 1 1 calc R . . H43B H 0.0766 0.2477 0.2447 0.018 Uiso 1 1 calc R . . C44 C 0.25485(14) 0.16026(9) 0.21840(8) 0.0148(3) Uani 1 1 d . . . H44A H 0.2206 0.1075 0.2338 0.018 Uiso 1 1 calc R . . H44B H 0.3126 0.1500 0.1722 0.018 Uiso 1 1 calc R . . Si1A Si 0.16338(4) 0.79687(2) 0.57326(2) 0.01414(8) Uani 1 1 d . . . F1A F 0.23962(9) 0.80612(6) 0.48702(5) 0.02259(19) Uani 1 1 d . . . F2A F 0.31879(9) 0.79271(6) 0.61655(5) 0.02401(19) Uani 1 1 d . . . F3A F 0.20359(9) 0.68970(5) 0.57399(5) 0.02035(18) Uani 1 1 d . . . F4A F 0.09130(9) 0.78849(6) 0.66020(5) 0.02211(18) Uani 1 1 d . . . F5A F 0.01012(9) 0.80208(6) 0.52872(5) 0.02318(19) Uani 1 1 d . . . F6A F 0.12234(10) 0.90483(6) 0.57303(6) 0.0270(2) Uani 1 1 d . . . Si1B Si 0.61346(4) 0.77027(3) 0.00389(2) 0.01601(8) Uani 1 1 d . . . F1B F 0.77275(8) 0.77583(5) -0.03112(5) 0.01751(17) Uani 1 1 d . . . F2B F 0.58663(8) 0.71815(6) -0.07216(5) 0.01896(17) Uani 1 1 d . . . F3B F 0.54433(9) 0.86460(6) -0.04713(6) 0.0268(2) Uani 1 1 d . . . F4B F 0.45665(9) 0.76384(7) 0.03896(5) 0.0290(2) Uani 1 1 d . . . F5B F 0.64398(9) 0.82402(7) 0.07846(5) 0.0288(2) Uani 1 1 d . . . F6B F 0.68311(9) 0.67815(7) 0.05509(6) 0.0303(2) Uani 1 1 d . . . F1 F 0.28799(8) 0.66775(5) 0.23056(5) 0.01578(16) Uani 1 1 d . . . F2 F 0.34157(8) 0.36458(5) 0.25754(5) 0.01501(16) Uani 1 1 d . . . O1S O 0.38680(10) 0.51116(6) 0.30915(6) 0.0171(2) Uani 1 1 d . . . H1SA H 0.3505 0.5576 0.2818 0.020 Uiso 1 1 d R . . H1SB H 0.3744 0.4702 0.2844 0.020 Uiso 1 1 d R . . O2S O 0.44037(13) 0.63942(8) 0.40374(7) 0.0296(3) Uani 1 1 d . . . H2SA H 0.4334 0.5931 0.3808 0.036 Uiso 1 1 d R . . H2SB H 0.4547 0.6195 0.4544 0.036 Uiso 1 1 d R . . O3S O 0.51428(11) 0.39110(7) 0.43522(6) 0.0225(2) Uani 1 1 d . . . H3SA H 0.4894 0.4346 0.4017 0.027 Uiso 1 1 d R . . H3SB H 0.6026 0.3660 0.4236 0.027 Uiso 1 1 d R . . O4S O 0.68410(14) 0.70551(9) 0.42212(8) 0.0378(3) Uani 1 1 d . . . H4SA H 0.6761 0.7616 0.4019 0.045 Uiso 1 1 d R . . H4SB H 0.6025 0.6888 0.4102 0.045 Uiso 1 1 d R . . O5S O 0.63871(12) 0.89208(8) 0.37777(6) 0.0256(2) Uani 1 1 d . . . H5SA H 0.6986 0.9067 0.4062 0.031 Uiso 1 1 d R . . H5SB H 0.5645 0.9098 0.4004 0.031 Uiso 1 1 d R . . O6S O 0.81579(11) 0.94422(7) 0.47452(7) 0.0237(2) Uani 1 1 d . . . H6SA H 0.8536 0.9849 0.4594 0.028 Uiso 1 1 d R . . H6SB H 0.8850 0.9078 0.4981 0.028 Uiso 1 1 d R . . O7S O 0.40082(12) 0.92748(8) 0.46175(7) 0.0297(3) Uani 1 1 d . . . H7SA H 0.3658 0.8844 0.4750 0.036 Uiso 1 1 d R . . H7SB H 0.3525 0.9729 0.4787 0.036 Uiso 1 1 d R . . O8S O 0.75245(11) 0.94700(7) 0.24061(6) 0.0220(2) Uani 1 1 d . . . H8SA H 0.7181 0.9292 0.2802 0.026 Uiso 1 1 d R . . H8SB H 0.8032 0.9811 0.2530 0.026 Uiso 1 1 d R . . O9S O 0.93685(11) 1.04368(7) 0.27176(6) 0.0238(2) Uani 1 1 d . . . H9SA H 0.9238 1.0782 0.3089 0.029 Uiso 1 1 d R . . H9SB H 0.9427 1.0734 0.2258 0.029 Uiso 1 1 d R . . O10S O 0.87211(10) 0.80229(7) 0.17148(6) 0.0205(2) Uani 1 1 d . . . H10S H 0.8415 0.8450 0.1953 0.025 Uiso 1 1 d R . . H10T H 0.8127 0.8039 0.1398 0.025 Uiso 1 1 d R . . O11S O 0.71104(10) 1.03279(7) 0.08325(6) 0.0217(2) Uani 1 1 d . . . H11S H 0.6331 1.0597 0.0692 0.026 Uiso 1 1 d R . . H11T H 0.7002 0.9989 0.1278 0.026 Uiso 1 1 d R . . O12S O 0.07657(11) 0.88521(7) 0.87997(6) 0.0232(2) Uani 1 1 d . . . H12S H 0.1387 0.9055 0.8933 0.028 Uiso 1 1 d R . . H12T H 0.0072 0.9049 0.9059 0.028 Uiso 1 1 d R . . O13S O 0.85979(11) 0.92390(7) -0.02037(7) 0.0250(2) Uani 1 1 d . . . H13S H 0.8160 0.9578 0.0090 0.030 Uiso 1 1 d R . . H13T H 0.8178 0.8813 -0.0197 0.030 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0133(5) 0.0124(5) 0.0116(5) -0.0006(4) -0.0004(4) -0.0008(4) C2 0.0180(6) 0.0140(6) 0.0140(6) -0.0016(5) -0.0006(5) -0.0030(5) C3 0.0161(6) 0.0128(6) 0.0153(6) -0.0001(5) 0.0016(5) 0.0001(5) N4 0.0140(5) 0.0137(5) 0.0132(5) -0.0006(4) 0.0004(4) -0.0016(4) C5 0.0138(6) 0.0163(7) 0.0237(7) -0.0013(5) 0.0032(5) -0.0027(5) C6 0.0115(5) 0.0158(6) 0.0191(7) -0.0020(5) 0.0029(5) -0.0027(5) C7 0.0197(6) 0.0185(7) 0.0157(6) -0.0043(5) 0.0026(5) -0.0064(5) C8 0.0212(6) 0.0183(7) 0.0148(6) 0.0000(5) 0.0022(5) -0.0041(5) C9 0.0152(6) 0.0208(7) 0.0182(7) -0.0026(5) -0.0018(5) -0.0021(5) C10 0.0155(6) 0.0196(7) 0.0216(7) -0.0084(6) 0.0008(5) -0.0035(5) C11 0.0146(6) 0.0156(6) 0.0210(7) -0.0027(5) 0.0061(5) -0.0047(5) C12 0.0173(6) 0.0165(7) 0.0263(8) -0.0026(6) 0.0064(6) -0.0033(5) N13 0.0170(5) 0.0140(5) 0.0141(5) -0.0024(4) 0.0009(4) -0.0036(4) C14 0.0225(7) 0.0141(6) 0.0146(6) -0.0007(5) -0.0003(5) -0.0022(5) C15 0.0197(6) 0.0143(6) 0.0158(6) -0.0006(5) 0.0020(5) -0.0045(5) N16 0.0128(5) 0.0131(5) 0.0122(5) -0.0008(4) -0.0001(4) -0.0025(4) C17 0.0146(6) 0.0119(6) 0.0168(6) -0.0003(5) -0.0008(5) -0.0017(5) C18 0.0148(6) 0.0117(6) 0.0172(6) -0.0030(5) 0.0009(5) -0.0016(5) N19 0.0132(5) 0.0129(5) 0.0149(5) -0.0014(4) 0.0000(4) -0.0027(4) C20 0.0151(6) 0.0152(6) 0.0189(7) -0.0023(5) 0.0038(5) -0.0036(5) C21 0.0114(5) 0.0147(6) 0.0174(6) -0.0012(5) 0.0030(5) -0.0037(5) C22 0.0141(6) 0.0148(6) 0.0173(6) 0.0021(5) -0.0007(5) -0.0013(5) C23 0.0134(6) 0.0176(7) 0.0161(6) -0.0012(5) -0.0012(5) -0.0036(5) C24 0.0156(6) 0.0193(7) 0.0166(6) -0.0007(5) -0.0016(5) -0.0053(5) C25 0.0162(6) 0.0167(7) 0.0183(7) 0.0037(5) -0.0032(5) -0.0040(5) C26 0.0112(5) 0.0142(6) 0.0180(6) -0.0008(5) 0.0013(5) -0.0027(5) C27 0.0130(6) 0.0147(6) 0.0235(7) 0.0001(5) -0.0045(5) -0.0015(5) N28 0.0125(5) 0.0134(5) 0.0175(6) -0.0009(4) -0.0011(4) -0.0021(4) C29 0.0145(6) 0.0143(6) 0.0189(7) -0.0031(5) -0.0015(5) -0.0024(5) C30 0.0155(6) 0.0132(6) 0.0166(6) -0.0005(5) 0.0010(5) -0.0035(5) C31 0.0167(6) 0.0116(6) 0.0141(6) -0.0003(5) -0.0015(5) -0.0005(5) C32 0.0170(6) 0.0136(6) 0.0141(6) 0.0000(5) -0.0006(5) -0.0027(5) N33 0.0135(5) 0.0133(5) 0.0127(5) -0.0006(4) -0.0013(4) -0.0008(4) C34 0.0187(6) 0.0154(6) 0.0127(6) -0.0028(5) -0.0008(5) -0.0021(5) C35 0.0158(6) 0.0152(6) 0.0119(6) -0.0021(5) -0.0012(5) -0.0016(5) C36 0.0126(6) 0.0183(7) 0.0345(9) -0.0008(6) 0.0025(6) -0.0021(5) C37 0.0126(6) 0.0154(7) 0.0382(9) 0.0001(6) 0.0023(6) 0.0014(5) C38 0.0137(6) 0.0152(7) 0.0243(7) -0.0015(5) -0.0018(5) 0.0020(5) C39 0.0114(5) 0.0177(7) 0.0222(7) -0.0008(5) -0.0003(5) -0.0011(5) C40 0.0141(6) 0.0151(6) 0.0135(6) -0.0028(5) -0.0012(5) -0.0015(5) C41 0.0117(5) 0.0153(6) 0.0196(7) -0.0013(5) -0.0020(5) -0.0004(5) N42 0.0117(5) 0.0129(5) 0.0134(5) -0.0016(4) 0.0001(4) -0.0008(4) C43 0.0134(6) 0.0156(6) 0.0166(6) -0.0003(5) -0.0001(5) -0.0047(5) C44 0.0165(6) 0.0133(6) 0.0148(6) -0.0016(5) -0.0013(5) -0.0038(5) Si1A 0.01584(17) 0.01343(18) 0.01316(17) -0.00038(13) -0.00139(14) -0.00369(14) F1A 0.0253(4) 0.0316(5) 0.0132(4) -0.0013(3) 0.0012(3) -0.0115(4) F2A 0.0215(4) 0.0343(5) 0.0185(4) -0.0021(4) -0.0051(3) -0.0114(4) F3A 0.0249(4) 0.0138(4) 0.0209(4) -0.0031(3) -0.0031(3) -0.0008(3) F4A 0.0276(4) 0.0204(4) 0.0176(4) -0.0009(3) 0.0074(4) -0.0042(4) F5A 0.0169(4) 0.0231(5) 0.0284(5) 0.0042(4) -0.0073(4) -0.0049(3) F6A 0.0392(5) 0.0130(4) 0.0288(5) 0.0001(4) 0.0020(4) -0.0069(4) Si1B 0.01096(16) 0.0221(2) 0.01361(18) -0.00220(15) -0.00004(13) -0.00068(14) F1B 0.0154(4) 0.0185(4) 0.0187(4) -0.0017(3) 0.0041(3) -0.0040(3) F2B 0.0171(4) 0.0201(4) 0.0199(4) -0.0059(3) 0.0014(3) -0.0030(3) F3B 0.0268(5) 0.0189(5) 0.0302(5) -0.0052(4) -0.0088(4) 0.0059(4) F4B 0.0125(4) 0.0511(7) 0.0256(5) -0.0137(4) 0.0045(4) -0.0077(4) F5B 0.0183(4) 0.0511(6) 0.0192(5) -0.0148(4) 0.0009(3) -0.0080(4) F6B 0.0206(4) 0.0334(5) 0.0334(5) 0.0176(4) -0.0045(4) -0.0072(4) F1 0.0158(4) 0.0139(4) 0.0171(4) -0.0009(3) -0.0001(3) -0.0024(3) F2 0.0158(4) 0.0128(4) 0.0164(4) -0.0016(3) 0.0006(3) -0.0031(3) O1S 0.0191(5) 0.0141(5) 0.0176(5) -0.0006(4) -0.0014(4) -0.0032(4) O2S 0.0426(7) 0.0249(6) 0.0231(6) -0.0031(5) -0.0073(5) -0.0108(5) O3S 0.0216(5) 0.0220(5) 0.0220(5) 0.0004(4) -0.0016(4) -0.0018(4) O4S 0.0436(7) 0.0324(7) 0.0365(7) -0.0015(6) -0.0112(6) -0.0077(6) O5S 0.0256(5) 0.0296(6) 0.0235(6) -0.0056(5) 0.0026(4) -0.0092(5) O6S 0.0204(5) 0.0181(5) 0.0314(6) 0.0060(4) -0.0038(4) -0.0053(4) O7S 0.0293(6) 0.0246(6) 0.0367(7) -0.0037(5) 0.0105(5) -0.0090(5) O8S 0.0236(5) 0.0225(6) 0.0198(5) -0.0028(4) 0.0021(4) -0.0047(4) O9S 0.0267(5) 0.0230(6) 0.0211(5) -0.0062(4) 0.0002(4) -0.0026(4) O10S 0.0153(4) 0.0238(6) 0.0223(5) -0.0066(4) 0.0002(4) -0.0022(4) O11S 0.0184(5) 0.0210(5) 0.0236(5) -0.0016(4) 0.0008(4) -0.0001(4) O12S 0.0213(5) 0.0254(6) 0.0236(6) -0.0051(4) 0.0026(4) -0.0056(4) O13S 0.0244(5) 0.0222(6) 0.0312(6) -0.0086(5) 0.0100(5) -0.0086(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C30 1.4614(17) . ? N1 C31 1.4632(17) . ? N1 C2 1.4689(17) . ? C2 C3 1.5042(19) . ? C3 N4 1.4914(17) . ? N4 C5 1.4926(17) . ? C5 C6 1.495(2) . ? C6 C7 1.388(2) . ? C6 C9 1.3907(19) . ? C7 C8 1.381(2) . ? C8 C11 1.3926(19) . ? C9 C10 1.379(2) . ? C10 C11 1.384(2) . ? C11 C12 1.498(2) . ? C12 N13 1.4948(18) . ? N13 C14 1.4938(18) . ? C14 C15 1.5133(19) . ? C15 N16 1.4665(17) . ? N16 C44 1.4636(17) . ? N16 C17 1.4696(17) . ? C17 C18 1.5090(19) . ? C18 N19 1.4884(17) . ? N19 C20 1.4979(17) . ? C20 C21 1.4985(19) . ? C21 C24 1.3857(19) . ? C21 C22 1.3935(19) . ? C22 C23 1.3845(19) . ? C23 C26 1.3902(19) . ? C24 C25 1.387(2) . ? C25 C26 1.3895(19) . ? C26 C27 1.4983(19) . ? C27 N28 1.4935(17) . ? N28 C29 1.4926(17) . ? C29 C30 1.5117(19) . ? C31 C32 1.5182(18) . ? C32 N33 1.4904(16) . ? N33 C34 1.5028 . ? C34 C35 1.5052(16) . ? C35 C36 1.3812(19) . ? C35 C38 1.3845(19) . ? C36 C37 1.391(2) . ? C37 C40 1.3813(19) . ? C38 C39 1.380(2) . ? C39 C40 1.3856(19) . ? C40 C41 1.4989(19) . ? C41 N42 1.4869(17) . ? N42 C43 1.4896(17) . ? C43 C44 1.5151(19) . ? Si1A F3A 1.6699(9) . ? Si1A F5A 1.6768(9) . ? Si1A F4A 1.6776(9) . ? Si1A F6A 1.6833(10) . ? Si1A F1A 1.6866(10) . ? Si1A F2A 1.6893(9) . ? Si1B F6B 1.6522(10) . ? Si1B F3B 1.6763(10) . ? Si1B F4B 1.6784(9) . ? Si1B F2B 1.6832(9) . ? Si1B F5B 1.6883(10) . ? Si1B F1B 1.6977(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 N1 C31 111.18(11) . . ? C30 N1 C2 111.36(10) . . ? C31 N1 C2 111.43(10) . . ? N1 C2 C3 111.98(11) . . ? N4 C3 C2 111.84(11) . . ? C3 N4 C5 110.72(10) . . ? N4 C5 C6 112.51(11) . . ? C7 C6 C9 119.42(13) . . ? C7 C6 C5 120.79(13) . . ? C9 C6 C5 119.78(13) . . ? C8 C7 C6 120.30(13) . . ? C7 C8 C11 120.28(14) . . ? C10 C9 C6 120.04(14) . . ? C9 C10 C11 120.79(13) . . ? C10 C11 C8 119.15(13) . . ? C10 C11 C12 120.84(13) . . ? C8 C11 C12 120.01(13) . . ? N13 C12 C11 110.61(11) . . ? C14 N13 C12 113.99(11) . . ? N13 C14 C15 111.95(11) . . ? N16 C15 C14 111.92(11) . . ? C44 N16 C15 111.28(10) . . ? C44 N16 C17 111.21(10) . . ? C15 N16 C17 111.18(11) . . ? N16 C17 C18 112.49(11) . . ? N19 C18 C17 111.93(11) . . ? C18 N19 C20 111.76(10) . . ? N19 C20 C21 110.95(11) . . ? C24 C21 C22 118.89(13) . . ? C24 C21 C20 120.76(12) . . ? C22 C21 C20 120.35(12) . . ? C23 C22 C21 120.09(13) . . ? C22 C23 C26 120.96(13) . . ? C21 C24 C25 120.99(13) . . ? C24 C25 C26 120.14(13) . . ? C25 C26 C23 118.87(13) . . ? C25 C26 C27 123.20(13) . . ? C23 C26 C27 117.87(12) . . ? N28 C27 C26 114.95(11) . . ? C29 N28 C27 110.33(10) . . ? N28 C29 C30 112.57(11) . . ? N1 C30 C29 112.77(11) . . ? N1 C31 C32 111.82(11) . . ? N33 C32 C31 110.77(11) . . ? C32 N33 C34 111.64(6) . . ? N33 C34 C35 111.10(6) . . ? C36 C35 C38 118.77(13) . . ? C36 C35 C34 120.78(12) . . ? C38 C35 C34 120.46(11) . . ? C35 C36 C37 120.86(13) . . ? C40 C37 C36 120.05(13) . . ? C39 C38 C35 120.54(13) . . ? C38 C39 C40 120.72(13) . . ? C37 C40 C39 119.03(13) . . ? C37 C40 C41 123.37(12) . . ? C39 C40 C41 117.54(12) . . ? N42 C41 C40 114.65(11) . . ? C41 N42 C43 111.24(10) . . ? N42 C43 C44 111.69(11) . . ? N16 C44 C43 112.68(11) . . ? F3A Si1A F5A 90.71(5) . . ? F3A Si1A F4A 90.50(5) . . ? F5A Si1A F4A 91.33(5) . . ? F3A Si1A F6A 179.65(5) . . ? F5A Si1A F6A 89.27(5) . . ? F4A Si1A F6A 89.15(5) . . ? F3A Si1A F1A 89.99(5) . . ? F5A Si1A F1A 90.20(5) . . ? F4A Si1A F1A 178.39(5) . . ? F6A Si1A F1A 90.36(5) . . ? F3A Si1A F2A 89.78(5) . . ? F5A Si1A F2A 178.85(5) . . ? F4A Si1A F2A 89.70(5) . . ? F6A Si1A F2A 90.25(5) . . ? F1A Si1A F2A 88.77(5) . . ? F6B Si1B F3B 179.02(6) . . ? F6B Si1B F4B 89.28(5) . . ? F3B Si1B F4B 91.11(5) . . ? F6B Si1B F2B 91.17(5) . . ? F3B Si1B F2B 89.72(5) . . ? F4B Si1B F2B 91.19(5) . . ? F6B Si1B F5B 89.62(6) . . ? F3B Si1B F5B 89.47(5) . . ? F4B Si1B F5B 90.47(5) . . ? F2B Si1B F5B 178.16(5) . . ? F6B Si1B F1B 90.17(5) . . ? F3B Si1B F1B 89.44(5) . . ? F4B Si1B F1B 179.45(6) . . ? F2B Si1B F1B 88.79(4) . . ? F5B Si1B F1B 89.55(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 N1 C2 C3 -159.84(11) . . . . ? C31 N1 C2 C3 75.40(14) . . . . ? N1 C2 C3 N4 67.06(14) . . . . ? C2 C3 N4 C5 -170.17(11) . . . . ? C3 N4 C5 C6 178.43(11) . . . . ? N4 C5 C6 C7 77.29(16) . . . . ? N4 C5 C6 C9 -104.01(14) . . . . ? C9 C6 C7 C8 -0.9(2) . . . . ? C5 C6 C7 C8 177.84(12) . . . . ? C6 C7 C8 C11 -0.5(2) . . . . ? C7 C6 C9 C10 1.6(2) . . . . ? C5 C6 C9 C10 -177.13(12) . . . . ? C6 C9 C10 C11 -1.0(2) . . . . ? C9 C10 C11 C8 -0.4(2) . . . . ? C9 C10 C11 C12 179.06(12) . . . . ? C7 C8 C11 C10 1.1(2) . . . . ? C7 C8 C11 C12 -178.34(12) . . . . ? C10 C11 C12 N13 97.63(15) . . . . ? C8 C11 C12 N13 -82.93(16) . . . . ? C11 C12 N13 C14 176.20(11) . . . . ? C12 N13 C14 C15 76.88(15) . . . . ? N13 C14 C15 N16 62.32(15) . . . . ? C14 C15 N16 C44 -158.49(11) . . . . ? C14 C15 N16 C17 76.95(14) . . . . ? C44 N16 C17 C18 79.76(14) . . . . ? C15 N16 C17 C18 -155.64(11) . . . . ? N16 C17 C18 N19 60.61(14) . . . . ? C17 C18 N19 C20 178.40(11) . . . . ? C18 N19 C20 C21 172.93(11) . . . . ? N19 C20 C21 C24 -111.25(14) . . . . ? N19 C20 C21 C22 68.01(15) . . . . ? C24 C21 C22 C23 2.18(19) . . . . ? C20 C21 C22 C23 -177.10(12) . . . . ? C21 C22 C23 C26 -2.5(2) . . . . ? C22 C21 C24 C25 -0.2(2) . . . . ? C20 C21 C24 C25 179.10(12) . . . . ? C21 C24 C25 C26 -1.6(2) . . . . ? C24 C25 C26 C23 1.3(2) . . . . ? C24 C25 C26 C27 178.55(12) . . . . ? C22 C23 C26 C25 0.7(2) . . . . ? C22 C23 C26 C27 -176.69(12) . . . . ? C25 C26 C27 N28 37.13(19) . . . . ? C23 C26 C27 N28 -145.57(12) . . . . ? C26 C27 N28 C29 166.44(12) . . . . ? C27 N28 C29 C30 168.91(11) . . . . ? C31 N1 C30 C29 -156.36(11) . . . . ? C2 N1 C30 C29 78.73(14) . . . . ? N28 C29 C30 N1 69.65(15) . . . . ? C30 N1 C31 C32 79.50(13) . . . . ? C2 N1 C31 C32 -155.63(11) . . . . ? N1 C31 C32 N33 56.19(14) . . . . ? C31 C32 N33 C34 -174.91(8) . . . . ? C32 N33 C34 C35 178.23(10) . . . . ? N33 C34 C35 C36 -104.10(12) . . . . ? N33 C34 C35 C38 75.80(12) . . . . ? C38 C35 C36 C37 -0.7(2) . . . . ? C34 C35 C36 C37 179.22(13) . . . . ? C35 C36 C37 C40 -0.7(2) . . . . ? C36 C35 C38 C39 1.2(2) . . . . ? C34 C35 C38 C39 -178.72(12) . . . . ? C35 C38 C39 C40 -0.3(2) . . . . ? C36 C37 C40 C39 1.7(2) . . . . ? C36 C37 C40 C41 178.84(14) . . . . ? C38 C39 C40 C37 -1.2(2) . . . . ? C38 C39 C40 C41 -178.52(13) . . . . ? C37 C40 C41 N42 21.91(19) . . . . ? C39 C40 C41 N42 -160.87(12) . . . . ? C40 C41 N42 C43 169.73(11) . . . . ? C41 N42 C43 C44 169.79(11) . . . . ? C15 N16 C44 C43 80.09(14) . . . . ? C17 N16 C44 C43 -155.37(11) . . . . ? N42 C43 C44 N16 66.10(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A F1A 0.92 2.24 2.9163(14) 129.4 . N4 H4A O2S 0.92 2.39 3.0939(17) 133.8 . N4 H4B F1 0.92 1.76 2.6703(14) 170.4 . N13 H13A F2 0.92 1.75 2.6538(14) 166.1 . N13 H13B O3S 0.92 2.09 2.9302(16) 150.5 . N13 H13B O4S 0.92 2.65 3.1026(18) 111.2 2_666 N19 H19A F2A 0.92 1.83 2.7158(15) 160.6 2_666 N19 H19B F2 0.92 1.78 2.6820(14) 164.7 . N28 H28B F1 0.92 1.69 2.6042(14) 169.1 . N28 H28A F4B 0.92 2.07 2.9580(16) 161.1 . N28 H28A F5B 0.92 2.49 3.1003(16) 124.5 . N28 H28A F6B 0.92 2.34 3.0577(16) 135.1 . N33 H33A O10S 0.92 1.87 2.7844(13) 173.1 1_455 N33 H33B F1 0.92 1.83 2.7237(12) 163.1 . N42 H42A F2 0.92 1.72 2.6100(14) 163.4 . N42 H42B F1B 0.92 2.16 2.8302(14) 129.2 2_665 N42 H42B F2B 0.92 1.93 2.8144(14) 159.7 2_665 O1S H1SA F1 0.85 1.87 2.7090(13) 171.1 . O1S H1SB F2 0.85 1.89 2.7168(13) 163.9 . O2S H2SA O1S 0.89 2.02 2.8886(15) 165.2 . O2S H2SB O3S 0.91 1.93 2.8181(16) 164.7 2_666 O3S H3SA O1S 0.85 2.05 2.8614(15) 159.6 . O3S H3SB F3A 0.90 1.91 2.7978(14) 165.9 2_666 O4S H4SA O5S 0.92 2.04 2.9428(18) 168.2 . O4S H4SB O2S 0.93 1.94 2.8564(18) 169.0 . O5S H5SA O6S 0.85 1.89 2.7372(16) 174.3 . O5S H5SB O7S 0.83 1.91 2.7375(16) 168.7 . O6S H6SA F6A 0.84 1.86 2.6743(14) 161.4 2_676 O6S H6SB F5A 0.86 1.89 2.7120(14) 159.5 1_655 O7S H7SA F1A 0.85 1.95 2.7712(15) 163.0 . O7S H7SB O6S 0.85 2.09 2.9100(16) 159.7 2_676 O8S H8SA O5S 0.82 1.96 2.7848(16) 176.7 . O8S H8SB O9S 0.86 1.87 2.7183(15) 170.6 . O9S H9SA F4A 0.88 2.22 2.9963(14) 146.2 2_676 O9S H9SA F6A 0.88 2.13 2.9227(15) 148.3 2_676 O9S H9SB O12S 0.90 1.89 2.7646(16) 163.6 2_676 O10S H10S O8S 0.83 1.91 2.7419(15) 172.8 . O10S H10T F5B 0.80 1.92 2.7059(14) 167.2 . O11S H11S F3B 0.81 1.90 2.7116(13) 170.9 2_675 O11S H11T O8S 0.92 2.07 2.9290(16) 153.3 . O12S H12S O11S 0.80 2.01 2.8070(15) 173.4 2_676 O12S H12T O13S 0.84 1.93 2.7481(15) 166.3 1_456 O13S H13S O11S 0.83 1.98 2.8110(15) 176.7 . O13S H13T F1B 0.87 1.87 2.7147(14) 164.2 . _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.491 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.071 #===END data_compound_1A_ #data_01028 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C36 H60 N8) 6+, 2Cl 1-, (Si F6) 2-, 2F 1-, 10(H2 O)' _chemical_formula_sum 'C36 H80 Cl2 F8 N8 O10 Si' _chemical_formula_weight 1036.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2614(8) _cell_length_b 14.6708(11) _cell_length_c 17.2858(13) _cell_angle_alpha 81.842(2) _cell_angle_beta 84.129(2) _cell_angle_gamma 76.707(2) _cell_volume 2500.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6474 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 30.49 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9332 _exptl_absorpt_correction_T_max 0.9833 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '\w scan frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 231 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.03 _diffrn_reflns_number 21593 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 30.54 _reflns_number_total 14660 _reflns_number_gt 10673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14660 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.50814(13) 0.17110(9) 0.29903(7) 0.0139(2) Uani 1 1 d . . . C2 C 0.65411(15) 0.15540(11) 0.27885(9) 0.0170(3) Uani 1 1 d . . . H2A H 0.6713 0.1589 0.2212 0.020 Uiso 1 1 calc R . . H2B H 0.6977 0.0913 0.3018 0.020 Uiso 1 1 calc R . . C3 C 0.71605(16) 0.22724(11) 0.30840(10) 0.0175(3) Uani 1 1 d . . . H3A H 0.6991 0.2234 0.3661 0.021 Uiso 1 1 calc R . . H3B H 0.8145 0.2113 0.2963 0.021 Uiso 1 1 calc R . . N4 N 0.66156(13) 0.32617(9) 0.27290(8) 0.0159(3) Uani 1 1 d . . . H4A H 0.6757 0.3671 0.3052 0.019 Uiso 1 1 calc R . . H4B H 0.5703 0.3346 0.2707 0.019 Uiso 1 1 calc R . . C5 C 0.72208(17) 0.35151(12) 0.19232(10) 0.0206(3) Uani 1 1 d . . . H5A H 0.6997 0.3124 0.1556 0.025 Uiso 1 1 calc R . . H5B H 0.8210 0.3387 0.1929 0.025 Uiso 1 1 calc R . . C6 C 0.66874(16) 0.45443(11) 0.16523(9) 0.0175(3) Uani 1 1 d . . . C7 C 0.72547(16) 0.52274(12) 0.18850(10) 0.0192(3) Uani 1 1 d . . . H7A H 0.7999 0.5039 0.2201 0.023 Uiso 1 1 calc R . . C8 C 0.67494(16) 0.61765(12) 0.16626(10) 0.0194(3) Uani 1 1 d . . . H8A H 0.7147 0.6635 0.1826 0.023 Uiso 1 1 calc R . . C9 C 0.56023(17) 0.48320(12) 0.11832(10) 0.0204(3) Uani 1 1 d . . . H9A H 0.5212 0.4372 0.1015 0.024 Uiso 1 1 calc R . . C10 C 0.50889(17) 0.57808(12) 0.09607(10) 0.0210(3) Uani 1 1 d . . . H10A H 0.4346 0.5968 0.0644 0.025 Uiso 1 1 calc R . . C11 C 0.56554(16) 0.64636(12) 0.11978(9) 0.0186(3) Uani 1 1 d . . . C12 C 0.51216(18) 0.74940(12) 0.09396(10) 0.0232(3) Uani 1 1 d . . . H12A H 0.4581 0.7556 0.0485 0.028 Uiso 1 1 calc R . . H12B H 0.5886 0.7798 0.0766 0.028 Uiso 1 1 calc R . . N13 N 0.42692(13) 0.80039(9) 0.15745(8) 0.0168(3) Uani 1 1 d . . . H13A H 0.3543 0.7736 0.1732 0.020 Uiso 1 1 calc R . . H13B H 0.4762 0.7950 0.2001 0.020 Uiso 1 1 calc R . . C14 C 0.37913(17) 0.90260(11) 0.12760(10) 0.0197(3) Uani 1 1 d . . . H14A H 0.3453 0.9075 0.0752 0.024 Uiso 1 1 calc R . . H14B H 0.4560 0.9339 0.1216 0.024 Uiso 1 1 calc R . . C15 C 0.26894(16) 0.95397(11) 0.18137(10) 0.0178(3) Uani 1 1 d . . . H15A H 0.3006 0.9449 0.2347 0.021 Uiso 1 1 calc R . . H15B H 0.2515 1.0224 0.1627 0.021 Uiso 1 1 calc R . . N16 N 0.14251(13) 0.92181(9) 0.18559(8) 0.0155(2) Uani 1 1 d . . . C17 C 0.07475(16) 0.94750(11) 0.11214(9) 0.0175(3) Uani 1 1 d . . . H17A H 0.1428 0.9454 0.0671 0.021 Uiso 1 1 calc R . . H17B H 0.0201 1.0127 0.1105 0.021 Uiso 1 1 calc R . . C18 C -0.01511(16) 0.88030(11) 0.10552(9) 0.0173(3) Uani 1 1 d . . . H18A H -0.0831 0.8826 0.1506 0.021 Uiso 1 1 calc R . . H18B H -0.0630 0.9009 0.0570 0.021 Uiso 1 1 calc R . . N19 N 0.06335(13) 0.78163(9) 0.10394(8) 0.0150(2) Uani 1 1 d . . . H19A H 0.1128 0.7640 0.1472 0.018 Uiso 1 1 calc R . . H19B H 0.1222 0.7787 0.0600 0.018 Uiso 1 1 calc R . . C20 C -0.02652(16) 0.71435(11) 0.10333(10) 0.0174(3) Uani 1 1 d . . . H20A H -0.0789 0.7328 0.0564 0.021 Uiso 1 1 calc R . . H20B H -0.0906 0.7181 0.1503 0.021 Uiso 1 1 calc R . . C21 C 0.05269(15) 0.61477(11) 0.10270(9) 0.0159(3) Uani 1 1 d . . . C22 C 0.07513(16) 0.55631(12) 0.17292(9) 0.0185(3) Uani 1 1 d . . . H22A H 0.0392 0.5796 0.2210 0.022 Uiso 1 1 calc R . . C23 C 0.14950(16) 0.46423(12) 0.17368(9) 0.0184(3) Uani 1 1 d . . . H23A H 0.1631 0.4248 0.2220 0.022 Uiso 1 1 calc R . . C24 C 0.10456(17) 0.57955(12) 0.03270(9) 0.0195(3) Uani 1 1 d . . . H24A H 0.0887 0.6185 -0.0157 0.023 Uiso 1 1 calc R . . C25 C 0.17932(17) 0.48788(11) 0.03322(9) 0.0185(3) Uani 1 1 d . . . H25A H 0.2141 0.4644 -0.0149 0.022 Uiso 1 1 calc R . . C26 C 0.20397(15) 0.42977(11) 0.10391(9) 0.0149(3) Uani 1 1 d . . . C27 C 0.28877(16) 0.33216(11) 0.09912(9) 0.0171(3) Uani 1 1 d . . . H27A H 0.2404 0.2966 0.0717 0.021 Uiso 1 1 calc R . . H27B H 0.3731 0.3372 0.0671 0.021 Uiso 1 1 calc R . . N28 N 0.32303(13) 0.27768(9) 0.17658(7) 0.0143(2) Uani 1 1 d . . . H28A H 0.2460 0.2655 0.2040 0.017 Uiso 1 1 calc R . . H28B H 0.3588 0.3134 0.2049 0.017 Uiso 1 1 calc R . . C29 C 0.42119(16) 0.18676(11) 0.16797(9) 0.0158(3) Uani 1 1 d . . . H29A H 0.5078 0.1999 0.1440 0.019 Uiso 1 1 calc R . . H29B H 0.3874 0.1514 0.1326 0.019 Uiso 1 1 calc R . . C30 C 0.44332(16) 0.12681(11) 0.24693(9) 0.0160(3) Uani 1 1 d . . . H30A H 0.3558 0.1172 0.2723 0.019 Uiso 1 1 calc R . . H30B H 0.5001 0.0641 0.2386 0.019 Uiso 1 1 calc R . . C31 C 0.47854(15) 0.13813(11) 0.38206(9) 0.0155(3) Uani 1 1 d . . . H31A H 0.5457 0.1514 0.4137 0.019 Uiso 1 1 calc R . . H31B H 0.4868 0.0690 0.3883 0.019 Uiso 1 1 calc R . . C32 C 0.33902(16) 0.18502(11) 0.41290(9) 0.0161(3) Uani 1 1 d . . . H32A H 0.2715 0.1706 0.3822 0.019 Uiso 1 1 calc R . . H32B H 0.3231 0.1589 0.4682 0.019 Uiso 1 1 calc R . . N33 N 0.32178(13) 0.28945(9) 0.40786(8) 0.0142(2) Uani 1 1 d . . . H33A H 0.3435 0.3133 0.3573 0.017 Uiso 1 1 calc R . . H33B H 0.3792 0.3031 0.4399 0.017 Uiso 1 1 calc R . . C34 C 0.18009(15) 0.33549(11) 0.43200(10) 0.0176(3) Uani 1 1 d . . . H34A H 0.1598 0.3134 0.4878 0.021 Uiso 1 1 calc R . . H34B H 0.1183 0.3156 0.4007 0.021 Uiso 1 1 calc R . . C35 C 0.15467(16) 0.44163(11) 0.42130(9) 0.0165(3) Uani 1 1 d . . . C36 C 0.24729(17) 0.48829(12) 0.44054(11) 0.0241(4) Uani 1 1 d . . . H36A H 0.3310 0.4531 0.4582 0.029 Uiso 1 1 calc R . . C37 C 0.21897(18) 0.58581(12) 0.43426(11) 0.0228(3) Uani 1 1 d . . . H37A H 0.2842 0.6168 0.4470 0.027 Uiso 1 1 calc R . . C38 C 0.03233(17) 0.49449(12) 0.39532(9) 0.0187(3) Uani 1 1 d . . . H38A H -0.0315 0.4633 0.3810 0.022 Uiso 1 1 calc R . . C39 C 0.00310(17) 0.59224(12) 0.39025(10) 0.0202(3) Uani 1 1 d . . . H39A H -0.0812 0.6275 0.3735 0.024 Uiso 1 1 calc R . . C40 C 0.09704(17) 0.63898(11) 0.40969(9) 0.0180(3) Uani 1 1 d . . . C41 C 0.07162(19) 0.74436(11) 0.40837(9) 0.0213(3) Uani 1 1 d . . . H41A H -0.0152 0.7662 0.4380 0.026 Uiso 1 1 calc R . . H41B H 0.1428 0.7597 0.4355 0.026 Uiso 1 1 calc R . . N42 N 0.06815(13) 0.79717(9) 0.32737(8) 0.0157(2) Uani 1 1 d . . . H42A H 0.1355 0.7660 0.2951 0.019 Uiso 1 1 calc R . . H42B H -0.0126 0.7995 0.3076 0.019 Uiso 1 1 calc R . . C43 C 0.08592(17) 0.89526(11) 0.32860(9) 0.0168(3) Uani 1 1 d . . . H43A H 0.1800 0.8930 0.3385 0.020 Uiso 1 1 calc R . . H43B H 0.0270 0.9237 0.3719 0.020 Uiso 1 1 calc R . . C44 C 0.05233(16) 0.95616(11) 0.25177(9) 0.0178(3) Uani 1 1 d . . . H44A H -0.0413 0.9573 0.2416 0.021 Uiso 1 1 calc R . . H44B H 0.0584 1.0216 0.2561 0.021 Uiso 1 1 calc R . . Cl1 Cl 0.25249(5) 0.80518(3) -0.04833(3) 0.02879(10) Uani 1 1 d . . . Cl2 Cl 0.07088(4) 0.22202(3) 0.27071(2) 0.02314(9) Uani 1 1 d . . . Si1A Si 0.68869(4) 0.84320(3) 0.31625(3) 0.01545(9) Uani 1 1 d . . . F1A F 0.82907(10) 0.77470(7) 0.27645(6) 0.0214(2) Uani 1 1 d . . . F2A F 0.59237(11) 0.78328(8) 0.27837(7) 0.0334(3) Uani 1 1 d . . . F3A F 0.69503(11) 0.76672(8) 0.39722(6) 0.0307(3) Uani 1 1 d . . . F4A F 0.55031(11) 0.91271(7) 0.35373(7) 0.0272(2) Uani 1 1 d . . . F5A F 0.78657(12) 0.90139(9) 0.35389(8) 0.0404(3) Uani 1 1 d . . . F6A F 0.68393(14) 0.91851(9) 0.23386(7) 0.0481(4) Uani 1 1 d . . . F1 F 0.39671(9) 0.37943(6) 0.27097(5) 0.01675(18) Uani 1 1 d . . . F2 F 0.23198(9) 0.71293(6) 0.21657(5) 0.01681(18) Uani 1 1 d . . . O1S O 0.40564(12) 0.56270(8) 0.28105(7) 0.0223(2) Uani 1 1 d . . . H1SA H 0.3918 0.5086 0.2681 0.027 Uiso 1 1 d R . . H1SB H 0.3351 0.5987 0.2568 0.027 Uiso 1 1 d R . . O2S O 0.56478(13) 0.60696(9) 0.37441(7) 0.0240(3) Uani 1 1 d . . . H2SA H 0.5187 0.6037 0.3418 0.029 Uiso 1 1 d R . . H2SB H 0.5985 0.6577 0.3494 0.029 Uiso 1 1 d R . . O3S O 0.46361(12) 0.68025(8) 0.51035(7) 0.0213(2) Uani 1 1 d . . . H3SA H 0.5003 0.6555 0.4739 0.026 Uiso 1 1 d R . . H3SB H 0.4299 0.7315 0.4967 0.026 Uiso 1 1 d R . . O4S O 0.70683(14) 0.42247(9) 0.38602(8) 0.0288(3) Uani 1 1 d . . . H4SA H 0.6685 0.4905 0.3852 0.035 Uiso 1 1 d R . . H4SB H 0.6646 0.3982 0.4122 0.035 Uiso 1 1 d R . . O5S O 0.34795(12) 0.85555(9) 0.44619(7) 0.0246(3) Uani 1 1 d . . . H5SA H 0.4022 0.8754 0.4104 0.029 Uiso 1 1 d R . . H5SB H 0.3073 0.8980 0.4716 0.029 Uiso 1 1 d R . . O6S O 0.80756(12) 1.00591(9) 0.46851(7) 0.0235(3) Uani 1 1 d . . . H6SA H 0.7773 0.9758 0.4330 0.028 Uiso 1 1 d R . . H6SB H 0.8495 0.9644 0.5057 0.028 Uiso 1 1 d R . . O7S O 0.03412(14) 0.19957(10) 0.09545(8) 0.0314(3) Uani 1 1 d . . . H7SA H -0.0471 0.1982 0.0913 0.038 Uiso 1 1 d R . . H7SB H 0.0349 0.2095 0.1427 0.038 Uiso 1 1 d R . . O8S O 0.28353(14) 0.13141(10) 0.02021(8) 0.0319(3) Uani 1 1 d . . . H8SA H 0.2942 0.0812 -0.0188 0.038 Uiso 1 1 d R . . H8SB H 0.1951 0.1444 0.0435 0.038 Uiso 1 1 d R . . O9S O 0.01035(14) 0.11301(10) 0.43866(8) 0.0307(3) Uani 1 1 d . . . H9SA H -0.0543 0.0876 0.4336 0.037 Uiso 1 1 d R . . H9SB H 0.0264 0.1423 0.3939 0.037 Uiso 1 1 d R . . O10S O 0.66277(15) 1.00038(10) 0.08478(8) 0.0326(3) Uani 1 1 d . . . H10S H 0.6836 1.0593 0.0805 0.039 Uiso 1 1 d R . . H10T H 0.6725 0.9846 0.1361 0.039 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0142(6) 0.0134(6) 0.0145(6) -0.0026(5) -0.0010(4) -0.0032(5) C2 0.0159(7) 0.0141(7) 0.0208(8) -0.0028(6) -0.0011(6) -0.0025(6) C3 0.0164(7) 0.0162(7) 0.0202(8) -0.0005(6) -0.0034(6) -0.0041(6) N4 0.0158(6) 0.0151(6) 0.0174(6) -0.0034(5) 0.0003(5) -0.0044(5) C5 0.0235(8) 0.0186(8) 0.0181(8) -0.0031(6) 0.0045(6) -0.0036(6) C6 0.0188(7) 0.0164(7) 0.0160(7) -0.0026(6) 0.0040(6) -0.0035(6) C7 0.0145(7) 0.0222(8) 0.0210(8) -0.0037(6) 0.0005(6) -0.0044(6) C8 0.0186(7) 0.0194(8) 0.0218(8) -0.0053(6) 0.0042(6) -0.0083(6) C9 0.0221(8) 0.0233(8) 0.0181(7) -0.0052(6) 0.0008(6) -0.0091(6) C10 0.0197(8) 0.0250(8) 0.0176(7) -0.0016(6) 0.0006(6) -0.0054(6) C11 0.0188(7) 0.0185(7) 0.0162(7) -0.0008(6) 0.0058(6) -0.0035(6) C12 0.0262(9) 0.0198(8) 0.0198(8) 0.0005(6) 0.0075(6) -0.0026(7) N13 0.0154(6) 0.0164(6) 0.0179(6) -0.0006(5) 0.0010(5) -0.0039(5) C14 0.0196(8) 0.0160(7) 0.0219(8) 0.0016(6) 0.0014(6) -0.0045(6) C15 0.0191(7) 0.0139(7) 0.0216(8) -0.0023(6) 0.0006(6) -0.0067(6) N16 0.0173(6) 0.0139(6) 0.0154(6) -0.0013(5) 0.0003(5) -0.0042(5) C17 0.0214(8) 0.0139(7) 0.0172(7) 0.0002(6) -0.0025(6) -0.0044(6) C18 0.0172(7) 0.0146(7) 0.0196(7) -0.0017(6) -0.0018(6) -0.0022(6) N19 0.0169(6) 0.0145(6) 0.0146(6) -0.0031(5) 0.0008(5) -0.0051(5) C20 0.0166(7) 0.0147(7) 0.0221(8) -0.0029(6) -0.0017(6) -0.0054(6) C21 0.0145(7) 0.0144(7) 0.0196(7) -0.0021(6) -0.0020(5) -0.0048(5) C22 0.0198(7) 0.0201(8) 0.0153(7) -0.0034(6) 0.0000(6) -0.0039(6) C23 0.0217(8) 0.0185(7) 0.0143(7) -0.0005(6) -0.0010(6) -0.0042(6) C24 0.0248(8) 0.0175(7) 0.0152(7) 0.0006(6) -0.0017(6) -0.0042(6) C25 0.0230(8) 0.0182(7) 0.0140(7) -0.0027(6) 0.0011(6) -0.0046(6) C26 0.0162(7) 0.0146(7) 0.0147(7) -0.0021(5) -0.0006(5) -0.0052(5) C27 0.0227(8) 0.0152(7) 0.0130(7) -0.0009(6) -0.0014(6) -0.0038(6) N28 0.0150(6) 0.0137(6) 0.0143(6) -0.0025(5) 0.0000(5) -0.0033(5) C29 0.0172(7) 0.0140(7) 0.0157(7) -0.0034(6) -0.0008(5) -0.0019(6) C30 0.0169(7) 0.0126(7) 0.0189(7) -0.0029(6) -0.0020(5) -0.0035(5) C31 0.0180(7) 0.0123(7) 0.0157(7) -0.0014(5) -0.0021(5) -0.0024(5) C32 0.0189(7) 0.0120(7) 0.0175(7) -0.0014(6) 0.0003(5) -0.0049(6) N33 0.0145(6) 0.0126(6) 0.0156(6) -0.0034(5) 0.0001(5) -0.0028(5) C34 0.0138(7) 0.0141(7) 0.0237(8) -0.0023(6) 0.0022(6) -0.0020(6) C35 0.0173(7) 0.0156(7) 0.0153(7) -0.0017(6) 0.0037(5) -0.0033(6) C36 0.0184(8) 0.0196(8) 0.0350(10) -0.0036(7) -0.0058(7) -0.0034(6) C37 0.0223(8) 0.0200(8) 0.0287(9) -0.0048(7) -0.0022(7) -0.0085(7) C38 0.0197(7) 0.0183(7) 0.0179(7) -0.0026(6) -0.0022(6) -0.0033(6) C39 0.0218(8) 0.0187(8) 0.0180(7) -0.0015(6) -0.0027(6) -0.0002(6) C40 0.0242(8) 0.0150(7) 0.0136(7) -0.0021(6) 0.0049(6) -0.0042(6) C41 0.0335(9) 0.0149(7) 0.0135(7) -0.0009(6) 0.0039(6) -0.0045(7) N42 0.0171(6) 0.0131(6) 0.0164(6) -0.0021(5) 0.0021(5) -0.0037(5) C43 0.0217(7) 0.0133(7) 0.0160(7) -0.0031(6) 0.0006(6) -0.0052(6) C44 0.0203(7) 0.0126(7) 0.0196(7) -0.0023(6) 0.0014(6) -0.0026(6) Cl1 0.0338(2) 0.0381(2) 0.0197(2) -0.01000(17) 0.00822(16) -0.0192(2) Cl2 0.01687(18) 0.0324(2) 0.02082(19) 0.00172(16) -0.00075(14) -0.00998(16) Si1A 0.0177(2) 0.01211(19) 0.0161(2) -0.00275(15) 0.00031(15) -0.00247(15) F1A 0.0195(5) 0.0207(5) 0.0233(5) -0.0082(4) 0.0004(4) -0.0007(4) F2A 0.0233(5) 0.0373(6) 0.0440(7) -0.0218(5) -0.0120(5) -0.0010(5) F3A 0.0328(6) 0.0304(6) 0.0221(5) 0.0079(4) 0.0007(4) -0.0013(5) F4A 0.0254(5) 0.0179(5) 0.0356(6) -0.0070(4) 0.0085(4) -0.0014(4) F5A 0.0274(6) 0.0430(7) 0.0616(8) -0.0364(6) 0.0109(5) -0.0176(5) F6A 0.0574(9) 0.0325(7) 0.0324(7) 0.0161(5) 0.0163(6) 0.0141(6) F1 0.0181(4) 0.0135(4) 0.0186(4) -0.0026(3) -0.0014(3) -0.0031(3) F2 0.0175(4) 0.0145(4) 0.0180(4) -0.0024(3) 0.0007(3) -0.0033(3) O1S 0.0248(6) 0.0174(6) 0.0251(6) -0.0034(5) -0.0054(5) -0.0037(5) O2S 0.0307(7) 0.0198(6) 0.0233(6) -0.0043(5) -0.0028(5) -0.0079(5) O3S 0.0238(6) 0.0195(6) 0.0211(6) -0.0045(5) -0.0023(5) -0.0044(5) O4S 0.0362(7) 0.0245(6) 0.0265(7) -0.0067(5) -0.0006(5) -0.0068(6) O5S 0.0223(6) 0.0226(6) 0.0270(6) -0.0051(5) 0.0022(5) -0.0016(5) O6S 0.0253(6) 0.0225(6) 0.0221(6) -0.0049(5) -0.0005(5) -0.0031(5) O7S 0.0334(7) 0.0373(8) 0.0243(7) -0.0098(6) 0.0007(5) -0.0070(6) O8S 0.0325(7) 0.0361(8) 0.0312(7) -0.0095(6) -0.0016(6) -0.0130(6) O9S 0.0340(7) 0.0333(7) 0.0256(7) 0.0072(6) -0.0064(5) -0.0138(6) O10S 0.0395(8) 0.0290(7) 0.0299(7) -0.0057(6) -0.0058(6) -0.0059(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C30 1.4708(19) . ? N1 C31 1.472(2) . ? N1 C2 1.475(2) . ? C2 C3 1.518(2) . ? C3 N4 1.497(2) . ? N4 C5 1.499(2) . ? C5 C6 1.507(2) . ? C6 C7 1.391(2) . ? C6 C9 1.395(2) . ? C7 C8 1.383(2) . ? C8 C11 1.398(2) . ? C9 C10 1.384(2) . ? C10 C11 1.394(2) . ? C11 C12 1.504(2) . ? C12 N13 1.505(2) . ? N13 C14 1.500(2) . ? C14 C15 1.517(2) . ? C15 N16 1.471(2) . ? N16 C44 1.467(2) . ? N16 C17 1.470(2) . ? C17 C18 1.519(2) . ? C18 N19 1.488(2) . ? N19 C20 1.4995(19) . ? C20 C21 1.501(2) . ? C21 C22 1.390(2) . ? C21 C24 1.391(2) . ? C22 C23 1.389(2) . ? C23 C26 1.388(2) . ? C24 C25 1.386(2) . ? C25 C26 1.397(2) . ? C26 C27 1.504(2) . ? C27 N28 1.4895(19) . ? N28 C29 1.4912(19) . ? C29 C30 1.523(2) . ? C31 C32 1.517(2) . ? C32 N33 1.4923(19) . ? N33 C34 1.4995(19) . ? C34 C35 1.506(2) . ? C35 C36 1.382(2) . ? C35 C38 1.396(2) . ? C36 C37 1.384(2) . ? C37 C40 1.386(2) . ? C38 C39 1.388(2) . ? C39 C40 1.396(2) . ? C40 C41 1.505(2) . ? C41 N42 1.501(2) . ? N42 C43 1.4949(19) . ? C43 C44 1.515(2) . ? Si1A F3A 1.6618(11) . ? Si1A F6A 1.6716(12) . ? Si1A F4A 1.6761(11) . ? Si1A F5A 1.6872(12) . ? Si1A F2A 1.6952(12) . ? Si1A F1A 1.6988(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 N1 C31 111.61(12) . . ? C30 N1 C2 110.89(12) . . ? C31 N1 C2 111.25(12) . . ? N1 C2 C3 112.24(13) . . ? N4 C3 C2 112.84(13) . . ? C3 N4 C5 114.44(13) . . ? N4 C5 C6 109.87(13) . . ? C7 C6 C9 118.86(15) . . ? C7 C6 C5 120.10(15) . . ? C9 C6 C5 121.02(15) . . ? C8 C7 C6 120.84(15) . . ? C7 C8 C11 120.22(15) . . ? C10 C9 C6 120.59(16) . . ? C9 C10 C11 120.42(16) . . ? C10 C11 C8 119.08(15) . . ? C10 C11 C12 120.50(16) . . ? C8 C11 C12 120.41(15) . . ? C11 C12 N13 113.11(13) . . ? C14 N13 C12 109.90(12) . . ? N13 C14 C15 112.91(13) . . ? N16 C15 C14 113.52(13) . . ? C44 N16 C17 110.93(13) . . ? C44 N16 C15 110.80(13) . . ? C17 N16 C15 113.05(12) . . ? N16 C17 C18 110.77(12) . . ? N19 C18 C17 111.62(13) . . ? C18 N19 C20 111.52(12) . . ? N19 C20 C21 111.42(12) . . ? C22 C21 C24 119.08(15) . . ? C22 C21 C20 119.89(14) . . ? C24 C21 C20 121.03(14) . . ? C23 C22 C21 120.80(15) . . ? C26 C23 C22 120.12(15) . . ? C25 C24 C21 120.29(15) . . ? C24 C25 C26 120.58(15) . . ? C23 C26 C25 119.10(15) . . ? C23 C26 C27 123.88(14) . . ? C25 C26 C27 117.02(14) . . ? N28 C27 C26 114.18(13) . . ? C27 N28 C29 111.78(12) . . ? N28 C29 C30 111.25(12) . . ? N1 C30 C29 111.90(12) . . ? N1 C31 C32 112.51(12) . . ? N33 C32 C31 111.75(12) . . ? C32 N33 C34 111.05(12) . . ? N33 C34 C35 113.03(12) . . ? C36 C35 C38 118.93(15) . . ? C36 C35 C34 121.39(15) . . ? C38 C35 C34 119.60(14) . . ? C35 C36 C37 120.49(16) . . ? C36 C37 C40 121.09(16) . . ? C39 C38 C35 120.55(15) . . ? C38 C39 C40 120.26(15) . . ? C37 C40 C39 118.66(15) . . ? C37 C40 C41 117.69(15) . . ? C39 C40 C41 123.62(15) . . ? N42 C41 C40 113.70(13) . . ? C43 N42 C41 110.61(12) . . ? N42 C43 C44 111.34(13) . . ? N16 C44 C43 112.34(13) . . ? F3A Si1A F6A 178.93(7) . . ? F3A Si1A F4A 90.98(6) . . ? F6A Si1A F4A 89.99(6) . . ? F3A Si1A F5A 90.28(7) . . ? F6A Si1A F5A 90.14(8) . . ? F4A Si1A F5A 90.66(6) . . ? F3A Si1A F2A 89.37(6) . . ? F6A Si1A F2A 90.20(8) . . ? F4A Si1A F2A 90.16(6) . . ? F5A Si1A F2A 179.11(6) . . ? F3A Si1A F1A 90.34(6) . . ? F6A Si1A F1A 88.69(6) . . ? F4A Si1A F1A 178.67(6) . . ? F5A Si1A F1A 89.18(6) . . ? F2A Si1A F1A 90.01(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 N1 C2 C3 158.65(13) . . . . ? C31 N1 C2 C3 -76.51(15) . . . . ? N1 C2 C3 N4 -62.20(17) . . . . ? C2 C3 N4 C5 -80.20(17) . . . . ? C3 N4 C5 C6 -175.23(13) . . . . ? N4 C5 C6 C7 82.45(18) . . . . ? N4 C5 C6 C9 -95.95(18) . . . . ? C9 C6 C7 C8 0.5(2) . . . . ? C5 C6 C7 C8 -177.89(15) . . . . ? C6 C7 C8 C11 0.0(2) . . . . ? C7 C6 C9 C10 -0.7(2) . . . . ? C5 C6 C9 C10 177.66(15) . . . . ? C6 C9 C10 C11 0.5(2) . . . . ? C9 C10 C11 C8 0.1(2) . . . . ? C9 C10 C11 C12 178.43(15) . . . . ? C7 C8 C11 C10 -0.3(2) . . . . ? C7 C8 C11 C12 -178.64(15) . . . . ? C10 C11 C12 N13 103.91(18) . . . . ? C8 C11 C12 N13 -77.75(19) . . . . ? C11 C12 N13 C14 179.28(14) . . . . ? C12 N13 C14 C15 167.41(14) . . . . ? N13 C14 C15 N16 -66.90(18) . . . . ? C14 C15 N16 C44 166.01(13) . . . . ? C14 C15 N16 C17 -68.75(17) . . . . ? C44 N16 C17 C18 -79.78(16) . . . . ? C15 N16 C17 C18 155.05(13) . . . . ? N16 C17 C18 N19 -61.80(17) . . . . ? C17 C18 N19 C20 175.84(13) . . . . ? C18 N19 C20 C21 -179.33(13) . . . . ? N19 C20 C21 C22 93.01(17) . . . . ? N19 C20 C21 C24 -86.97(18) . . . . ? C24 C21 C22 C23 0.7(2) . . . . ? C20 C21 C22 C23 -179.26(15) . . . . ? C21 C22 C23 C26 0.8(2) . . . . ? C22 C21 C24 C25 -1.0(2) . . . . ? C20 C21 C24 C25 178.97(15) . . . . ? C21 C24 C25 C26 -0.2(2) . . . . ? C22 C23 C26 C25 -2.0(2) . . . . ? C22 C23 C26 C27 178.30(15) . . . . ? C24 C25 C26 C23 1.7(2) . . . . ? C24 C25 C26 C27 -178.57(15) . . . . ? C23 C26 C27 N28 -6.4(2) . . . . ? C25 C26 C27 N28 173.90(13) . . . . ? C26 C27 N28 C29 -172.65(13) . . . . ? C27 N28 C29 C30 -173.58(12) . . . . ? C31 N1 C30 C29 155.63(12) . . . . ? C2 N1 C30 C29 -79.72(15) . . . . ? N28 C29 C30 N1 -65.64(16) . . . . ? C30 N1 C31 C32 -77.74(15) . . . . ? C2 N1 C31 C32 157.82(12) . . . . ? N1 C31 C32 N33 -60.92(16) . . . . ? C31 C32 N33 C34 175.09(13) . . . . ? C32 N33 C34 C35 -175.05(13) . . . . ? N33 C34 C35 C36 -41.4(2) . . . . ? N33 C34 C35 C38 141.97(15) . . . . ? C38 C35 C36 C37 0.1(3) . . . . ? C34 C35 C36 C37 -176.50(16) . . . . ? C35 C36 C37 C40 0.9(3) . . . . ? C36 C35 C38 C39 -1.2(2) . . . . ? C34 C35 C38 C39 175.51(15) . . . . ? C35 C38 C39 C40 1.2(2) . . . . ? C36 C37 C40 C39 -0.8(3) . . . . ? C36 C37 C40 C41 176.98(16) . . . . ? C38 C39 C40 C37 -0.2(2) . . . . ? C38 C39 C40 C41 -177.90(15) . . . . ? C37 C40 C41 N42 111.03(17) . . . . ? C39 C40 C41 N42 -71.3(2) . . . . ? C40 C41 N42 C43 -162.23(14) . . . . ? C41 N42 C43 C44 -167.42(13) . . . . ? C17 N16 C44 C43 151.69(13) . . . . ? C15 N16 C44 C43 -81.89(15) . . . . ? N42 C43 C44 N16 -63.14(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4B F1 0.92 1.75 2.6518(16) 165.6 . N4 H4A O4S 0.92 1.80 2.7032(18) 166.1 . N13 H13A F2 0.92 1.75 2.6612(16) 170.2 . N13 H13B F2A 0.92 1.86 2.7741(17) 173.7 . N19 H19A F2 0.92 1.77 2.6704(16) 167.0 . N19 H19B Cl1 0.92 2.23 3.1337(14) 167.7 . N28 H28A Cl2 0.92 2.20 3.1212(13) 174.6 . N28 H28B F1 0.92 1.72 2.6316(16) 168.1 . N33 H33A F1 0.92 1.77 2.6722(16) 166.4 . N33 H33B O3S 0.92 1.98 2.8829(17) 166.2 2_666 N42 H42A F2 0.92 1.76 2.6607(16) 165.4 . N42 H42B F1A 0.92 1.89 2.7925(17) 166.8 1_455 N42 H42B F5A 0.92 2.39 2.9653(18) 120.7 1_455 O1S H1SA F1 0.90 1.88 2.7418(15) 160.4 . O1S H1SB F2 0.90 1.85 2.6792(15) 153.5 . O2S H2SA O1S 0.79 1.89 2.6490(17) 163.6 . O2S H2SB F2A 0.93 2.06 2.9239(18) 155.6 . O2S H2SB F3A 0.93 2.35 3.0408(17) 131.7 . O3S H3SA O2S 0.79 1.95 2.7313(17) 170.3 . O3S H3SB O5S 0.77 1.94 2.7035(17) 171.2 . O4S H4SA O2S 0.98 1.79 2.7535(18) 165.9 . O4S H4SB O3S 0.71 2.18 2.8885(18) 178.0 2_666 O5S H5SA F4A 0.85 1.87 2.7039(17) 165.0 . O5S H5SB O6S 0.82 1.96 2.7801(17) 173.6 2_676 O6S H6SA F5A 0.92 1.85 2.7249(17) 158.0 . O6S H6SB O9S 0.89 1.87 2.7257(18) 159.7 2_666 O7S H7SA Cl1 0.85 2.32 3.1494(15) 166.3 2_565 O7S H7SB Cl2 0.85 2.32 3.1627(14) 171.0 . O8S H8SA O10S 1.05 1.72 2.763(2) 171.2 2_665 O8S H8SB O7S 0.94 1.86 2.784(2) 164.3 . O9S H9SA O6S 0.85 2.05 2.8493(19) 156.0 1_445 O9S H9SB Cl2 0.85 2.33 3.1847(14) 179.8 . O10S H10S Cl1 0.93 2.21 3.1320(15) 169.5 2_675 O10S H10T F6A 0.89 1.83 2.6919(19) 162.5 . _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.545 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.073 #===END data_compound_2_ #data_01023 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C36 H60 N8) 6+, 6Cl 1-, 5(H2 O) (C H3 O H)' _chemical_formula_sum 'C37 H74 Cl6 N8 O6' _chemical_formula_weight 939.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.4706(6) _cell_length_b 15.7895(9) _cell_length_c 27.0054(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.164(2) _cell_angle_gamma 90.00 _cell_volume 4798.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2741 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 23.92 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 0.408 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9229 _exptl_absorpt_correction_T_max 0.9799 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '\w scan frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 89 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.02 _diffrn_reflns_number 30048 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_sigmaI/netI 0.1672 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9438 _reflns_number_gt 4575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9438 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 0.762 _refine_ls_restrained_S_all 0.762 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.3215(2) 0.44521(16) 0.05108(9) 0.0169(7) Uani 1 1 d . . . C2 C 0.3437(3) 0.3750(2) 0.01805(12) 0.0192(8) Uani 1 1 d . . . H2A H 0.3480 0.3980 -0.0157 0.023 Uiso 1 1 calc R . . H2B H 0.2762 0.3349 0.0139 0.023 Uiso 1 1 calc R . . C3 C 0.4569(3) 0.3279(2) 0.03851(11) 0.0183(8) Uani 1 1 d . . . H3A H 0.4674 0.2818 0.0149 0.022 Uiso 1 1 calc R . . H3B H 0.5251 0.3671 0.0409 0.022 Uiso 1 1 calc R . . N4 N 0.4555(2) 0.29133(16) 0.08918(9) 0.0185(7) Uani 1 1 d . . . H4A H 0.3925 0.2545 0.0868 0.022 Uiso 1 1 calc R . . H4B H 0.4445 0.3341 0.1109 0.022 Uiso 1 1 calc R . . C5 C 0.5677(3) 0.2456(2) 0.11014(13) 0.0287(9) Uani 1 1 d . . . H5A H 0.6357 0.2811 0.1053 0.034 Uiso 1 1 calc R . . H5B H 0.5703 0.1926 0.0907 0.034 Uiso 1 1 calc R . . C6 C 0.5823(3) 0.2237(2) 0.16530(12) 0.0206(8) Uani 1 1 d . . . C7 C 0.5106(3) 0.1642(2) 0.18265(13) 0.0215(8) Uani 1 1 d . . . H7A H 0.4467 0.1390 0.1598 0.026 Uiso 1 1 calc R . . C8 C 0.5318(3) 0.1415(2) 0.23306(13) 0.0213(8) Uani 1 1 d . . . H8A H 0.4819 0.1011 0.2447 0.026 Uiso 1 1 calc R . . C9 C 0.6729(3) 0.2608(2) 0.19932(13) 0.0226(9) Uani 1 1 d . . . H9A H 0.7214 0.3026 0.1881 0.027 Uiso 1 1 calc R . . C10 C 0.6938(3) 0.2378(2) 0.24948(13) 0.0222(8) Uani 1 1 d . . . H10A H 0.7565 0.2643 0.2724 0.027 Uiso 1 1 calc R . . C11 C 0.6257(3) 0.17752(19) 0.26691(12) 0.0170(8) Uani 1 1 d . . . C12 C 0.6541(3) 0.1507(2) 0.32113(12) 0.0217(9) Uani 1 1 d . . . H12A H 0.7381 0.1648 0.3353 0.026 Uiso 1 1 calc R . . H12B H 0.6452 0.0885 0.3230 0.026 Uiso 1 1 calc R . . N13 N 0.5756(2) 0.19251(16) 0.35276(9) 0.0170(7) Uani 1 1 d . . . H13A H 0.5640 0.2482 0.3431 0.020 Uiso 1 1 calc R . . H13B H 0.5027 0.1662 0.3470 0.020 Uiso 1 1 calc R . . C14 C 0.6277(3) 0.1887(2) 0.40757(11) 0.0184(8) Uani 1 1 d . . . H14A H 0.7071 0.2158 0.4137 0.022 Uiso 1 1 calc R . . H14B H 0.6383 0.1288 0.4182 0.022 Uiso 1 1 calc R . . C15 C 0.5500(3) 0.23285(19) 0.43905(12) 0.0184(8) Uani 1 1 d . . . H15A H 0.4729 0.2029 0.4350 0.022 Uiso 1 1 calc R . . H15B H 0.5887 0.2298 0.4751 0.022 Uiso 1 1 calc R . . N16 N 0.5285(2) 0.32205(16) 0.42454(9) 0.0171(7) Uani 1 1 d . . . C17 C 0.4320(3) 0.3573(2) 0.44730(12) 0.0203(8) Uani 1 1 d . . . H17A H 0.4301 0.4195 0.4429 0.024 Uiso 1 1 calc R . . H17B H 0.4490 0.3452 0.4840 0.024 Uiso 1 1 calc R . . C18 C 0.3119(3) 0.3216(2) 0.42448(12) 0.0213(8) Uani 1 1 d . . . H18A H 0.3129 0.2595 0.4293 0.026 Uiso 1 1 calc R . . H18B H 0.2515 0.3457 0.4421 0.026 Uiso 1 1 calc R . . N19 N 0.2784(2) 0.34112(16) 0.36960(9) 0.0192(7) Uani 1 1 d . . . H19A H 0.3396 0.3258 0.3539 0.023 Uiso 1 1 calc R . . H19B H 0.2667 0.3985 0.3654 0.023 Uiso 1 1 calc R . . C20 C 0.1680(3) 0.2955(2) 0.34546(12) 0.0222(8) Uani 1 1 d . . . H20A H 0.1019 0.3132 0.3619 0.027 Uiso 1 1 calc R . . H20B H 0.1800 0.2338 0.3510 0.027 Uiso 1 1 calc R . . C21 C 0.1338(3) 0.3122(2) 0.28965(12) 0.0193(8) Uani 1 1 d . . . C22 C 0.1763(3) 0.2608(2) 0.25582(13) 0.0212(8) Uani 1 1 d . . . H22A H 0.2282 0.2153 0.2680 0.025 Uiso 1 1 calc R . . C23 C 0.1441(3) 0.2748(2) 0.20442(13) 0.0209(8) Uani 1 1 d . . . H23A H 0.1740 0.2388 0.1816 0.025 Uiso 1 1 calc R . . C24 C 0.0579(3) 0.3783(2) 0.27144(12) 0.0234(8) Uani 1 1 d . . . H24A H 0.0280 0.4143 0.2943 0.028 Uiso 1 1 calc R . . C25 C 0.0255(3) 0.3919(2) 0.21972(13) 0.0236(9) Uani 1 1 d . . . H25A H -0.0271 0.4370 0.2075 0.028 Uiso 1 1 calc R . . C26 C 0.0689(3) 0.3408(2) 0.18604(12) 0.0185(8) Uani 1 1 d . . . C27 C 0.0377(3) 0.3566(2) 0.13019(12) 0.0228(9) Uani 1 1 d . . . H27A H -0.0400 0.3859 0.1220 0.027 Uiso 1 1 calc R . . H27B H 0.0300 0.3017 0.1121 0.027 Uiso 1 1 calc R . . N28 N 0.1306(2) 0.40954(16) 0.11252(9) 0.0185(7) Uani 1 1 d . . . H28A H 0.1286 0.4636 0.1250 0.022 Uiso 1 1 calc R . . H28B H 0.2045 0.3872 0.1249 0.022 Uiso 1 1 calc R . . C29 C 0.1110(3) 0.4128(2) 0.05667(12) 0.0201(8) Uani 1 1 d . . . H29A H 0.0285 0.4314 0.0433 0.024 Uiso 1 1 calc R . . H29B H 0.1205 0.3552 0.0436 0.024 Uiso 1 1 calc R . . C30 C 0.1961(3) 0.4723(2) 0.03771(12) 0.0176(8) Uani 1 1 d . . . H30A H 0.1731 0.4765 0.0005 0.021 Uiso 1 1 calc R . . H30B H 0.1884 0.5294 0.0519 0.021 Uiso 1 1 calc R . . C31 C 0.3996(3) 0.51782(19) 0.04585(11) 0.0180(8) Uani 1 1 d . . . H31A H 0.3656 0.5495 0.0148 0.022 Uiso 1 1 calc R . . H31B H 0.4785 0.4963 0.0421 0.022 Uiso 1 1 calc R . . C32 C 0.4152(3) 0.57769(19) 0.09048(11) 0.0179(8) Uani 1 1 d . . . H32A H 0.4517 0.6311 0.0817 0.021 Uiso 1 1 calc R . . H32B H 0.3364 0.5914 0.0982 0.021 Uiso 1 1 calc R . . N33 N 0.4918(2) 0.53939(15) 0.13587(9) 0.0164(6) Uani 1 1 d . . . H33A H 0.5653 0.5275 0.1287 0.020 Uiso 1 1 calc R . . H33B H 0.4585 0.4892 0.1435 0.020 Uiso 1 1 calc R . . C34 C 0.5064(3) 0.5968(2) 0.18050(11) 0.0177(8) Uani 1 1 d . . . H34A H 0.4277 0.6059 0.1895 0.021 Uiso 1 1 calc R . . H34B H 0.5355 0.6524 0.1711 0.021 Uiso 1 1 calc R . . C35 C 0.5915(3) 0.56354(19) 0.22645(12) 0.0163(8) Uani 1 1 d . . . C36 C 0.6635(3) 0.4933(2) 0.22513(12) 0.0198(8) Uani 1 1 d . . . H36A H 0.6594 0.4626 0.1946 0.024 Uiso 1 1 calc R . . C37 C 0.7416(3) 0.4682(2) 0.26866(12) 0.0199(8) Uani 1 1 d . . . H37A H 0.7902 0.4197 0.2676 0.024 Uiso 1 1 calc R . . C38 C 0.5991(3) 0.6066(2) 0.27164(12) 0.0181(8) Uani 1 1 d . . . H38A H 0.5493 0.6542 0.2731 0.022 Uiso 1 1 calc R . . C39 C 0.6775(3) 0.5819(2) 0.31464(12) 0.0192(8) Uani 1 1 d . . . H39A H 0.6817 0.6128 0.3451 0.023 Uiso 1 1 calc R . . C40 C 0.7499(3) 0.5120(2) 0.31325(12) 0.0173(8) Uani 1 1 d . . . C41 C 0.8381(3) 0.4828(2) 0.35905(12) 0.0210(8) Uani 1 1 d . . . H41A H 0.8818 0.4332 0.3495 0.025 Uiso 1 1 calc R . . H41B H 0.8966 0.5286 0.3696 0.025 Uiso 1 1 calc R . . N42 N 0.7831(2) 0.45911(16) 0.40300(10) 0.0204(7) Uani 1 1 d . . . H42A H 0.8384 0.4300 0.4260 0.025 Uiso 1 1 calc R . . H42B H 0.7648 0.5080 0.4184 0.025 Uiso 1 1 calc R . . C43 C 0.6734(3) 0.4063(2) 0.39019(12) 0.0176(8) Uani 1 1 d . . . H43A H 0.6878 0.3582 0.3686 0.021 Uiso 1 1 calc R . . H43B H 0.6078 0.4408 0.3710 0.021 Uiso 1 1 calc R . . C44 C 0.6382(3) 0.3729(2) 0.43762(12) 0.0211(8) Uani 1 1 d . . . H44A H 0.7031 0.3374 0.4565 0.025 Uiso 1 1 calc R . . H44B H 0.6250 0.4208 0.4595 0.025 Uiso 1 1 calc R . . Cl1 Cl 0.38515(7) 0.38477(5) 0.18129(3) 0.0188(2) Uani 1 1 d . . . Cl2 Cl 0.72224(7) 0.46380(5) 0.09780(3) 0.0234(2) Uani 1 1 d . . . Cl3 Cl 0.34343(7) 0.09550(5) 0.34601(3) 0.0247(2) Uani 1 1 d . . . Cl4 Cl 0.22450(8) 0.18485(6) 0.07308(4) 0.0330(3) Uani 1 1 d . . . Cl5 Cl 0.75071(8) 0.62976(6) 0.45505(3) 0.0291(2) Uani 1 1 d . . . Cl6 Cl 0.91253(8) 0.27085(5) 0.40106(4) 0.0329(2) Uani 1 1 d . . . O1S O 0.46135(18) 0.33354(13) 0.29951(8) 0.0231(6) Uani 1 1 d . . . H1SA H 0.4405 0.3476 0.2667 0.028 Uiso 1 1 d R . . H1SB H 0.4365 0.3841 0.3088 0.028 Uiso 1 1 d R . . O2S O 0.3845(2) 0.48665(13) 0.32718(8) 0.0269(6) Uani 1 1 d . . . H2S H 0.4191 0.5179 0.3539 0.032 Uiso 1 1 d R . . C2S C 0.3088(3) 0.5319(2) 0.28741(12) 0.0290(9) Uani 1 1 d . . . H2SB H 0.2430 0.5575 0.3005 0.044 Uiso 1 1 d R . . H2SC H 0.2770 0.4926 0.2600 0.044 Uiso 1 1 d R . . H2SD H 0.3546 0.5764 0.2746 0.044 Uiso 1 1 d R . . O3S O 0.8099(2) 0.32919(15) 0.01863(9) 0.0381(7) Uani 1 1 d . . . H3SB H 0.7937 0.2752 0.0256 0.046 Uiso 1 1 d R . . H3SA H 0.7862 0.3660 0.0401 0.046 Uiso 1 1 d R . . O4S O 0.1701(2) 0.49665(14) 0.39077(9) 0.0353(7) Uani 1 1 d . . . H4SA H 0.1408 0.4985 0.4193 0.042 Uiso 1 1 d R . . H4SB H 0.1995 0.5482 0.4004 0.042 Uiso 1 1 d R . . O5S O 1.0305(3) 0.42491(19) 0.45683(11) 0.0686(10) Uani 1 1 d . . . H5SA H 1.0189 0.3729 0.4432 0.082 Uiso 1 1 d R . . H5SB H 1.0784 0.4195 0.4873 0.082 Uiso 1 1 d R . . O6S O 0.4877(2) 0.5813(2) 0.40575(11) 0.0787(12) Uani 1 1 d . . . H6SA H 0.4256 0.6118 0.4116 0.094 Uiso 1 1 d R . . H6SB H 0.5631 0.5954 0.4195 0.094 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0148(16) 0.0177(16) 0.0176(17) -0.0001(13) 0.0019(12) -0.0019(12) C2 0.020(2) 0.0199(19) 0.017(2) 0.0007(16) 0.0029(15) -0.0017(16) C3 0.022(2) 0.0203(19) 0.013(2) 0.0002(15) 0.0047(15) -0.0016(16) N4 0.0165(17) 0.0169(16) 0.0229(17) -0.0020(13) 0.0055(13) 0.0016(12) C5 0.026(2) 0.036(2) 0.025(2) 0.0075(17) 0.0060(17) 0.0173(18) C6 0.023(2) 0.022(2) 0.019(2) 0.0032(16) 0.0092(16) 0.0104(16) C7 0.016(2) 0.025(2) 0.021(2) -0.0017(16) -0.0016(16) 0.0057(16) C8 0.022(2) 0.017(2) 0.026(2) 0.0006(16) 0.0080(16) 0.0054(16) C9 0.022(2) 0.0158(19) 0.032(2) 0.0056(17) 0.0112(17) 0.0038(16) C10 0.019(2) 0.019(2) 0.028(2) -0.0030(17) 0.0027(16) 0.0038(16) C11 0.018(2) 0.0145(18) 0.019(2) 0.0006(15) 0.0045(15) 0.0058(15) C12 0.017(2) 0.023(2) 0.024(2) -0.0019(16) 0.0022(16) 0.0050(16) N13 0.0152(16) 0.0154(15) 0.0198(17) 0.0013(12) 0.0019(12) 0.0000(12) C14 0.020(2) 0.021(2) 0.014(2) 0.0028(15) 0.0032(15) 0.0012(16) C15 0.019(2) 0.0218(19) 0.015(2) 0.0023(15) 0.0032(15) -0.0015(16) N16 0.0159(16) 0.0206(16) 0.0144(17) -0.0010(13) 0.0020(12) -0.0037(13) C17 0.023(2) 0.021(2) 0.017(2) -0.0034(15) 0.0031(16) 0.0027(16) C18 0.019(2) 0.028(2) 0.017(2) 0.0032(16) 0.0042(16) 0.0032(16) N19 0.0195(17) 0.0192(16) 0.0187(17) 0.0028(13) 0.0037(13) 0.0005(13) C20 0.020(2) 0.024(2) 0.023(2) 0.0013(16) 0.0038(16) -0.0029(16) C21 0.016(2) 0.023(2) 0.019(2) 0.0019(16) 0.0049(15) -0.0040(16) C22 0.018(2) 0.020(2) 0.025(2) 0.0025(16) 0.0020(16) -0.0013(15) C23 0.024(2) 0.0176(19) 0.022(2) -0.0035(16) 0.0072(16) -0.0021(16) C24 0.019(2) 0.029(2) 0.024(2) -0.0054(17) 0.0085(16) 0.0023(17) C25 0.018(2) 0.028(2) 0.025(2) 0.0031(17) 0.0038(16) 0.0018(16) C26 0.016(2) 0.021(2) 0.018(2) 0.0020(16) 0.0020(15) -0.0070(15) C27 0.016(2) 0.026(2) 0.027(2) -0.0007(16) 0.0038(16) -0.0039(16) N28 0.0158(16) 0.0201(16) 0.0196(17) 0.0026(13) 0.0033(12) 0.0032(12) C29 0.015(2) 0.026(2) 0.018(2) 0.0002(16) 0.0004(15) -0.0005(16) C30 0.014(2) 0.023(2) 0.0154(19) -0.0003(15) 0.0026(14) -0.0020(15) C31 0.014(2) 0.022(2) 0.018(2) 0.0021(15) 0.0031(15) -0.0008(15) C32 0.015(2) 0.0160(19) 0.022(2) 0.0060(15) 0.0020(15) 0.0008(14) N33 0.0130(16) 0.0165(15) 0.0192(16) 0.0013(13) 0.0018(12) -0.0024(12) C34 0.021(2) 0.0182(19) 0.0147(19) -0.0057(15) 0.0041(14) 0.0015(15) C35 0.0134(19) 0.0162(19) 0.019(2) 0.0043(15) 0.0036(15) -0.0052(14) C36 0.021(2) 0.0182(19) 0.020(2) -0.0034(16) 0.0042(16) -0.0024(16) C37 0.017(2) 0.0161(19) 0.028(2) 0.0024(16) 0.0060(16) 0.0023(15) C38 0.017(2) 0.0170(19) 0.020(2) -0.0002(16) 0.0031(15) 0.0003(15) C39 0.021(2) 0.022(2) 0.015(2) -0.0007(15) 0.0048(16) -0.0072(16) C40 0.017(2) 0.0177(19) 0.017(2) 0.0020(15) 0.0033(15) -0.0079(15) C41 0.022(2) 0.021(2) 0.019(2) 0.0044(16) 0.0033(16) -0.0055(16) N42 0.0165(16) 0.0243(16) 0.0189(17) 0.0020(13) -0.0005(12) -0.0002(13) C43 0.0110(19) 0.0201(19) 0.021(2) -0.0003(15) 0.0014(15) -0.0023(15) C44 0.023(2) 0.022(2) 0.018(2) -0.0010(16) 0.0031(16) -0.0013(16) Cl1 0.0189(5) 0.0202(5) 0.0173(5) 0.0003(4) 0.0033(3) 0.0005(4) Cl2 0.0211(5) 0.0269(5) 0.0220(5) -0.0025(4) 0.0039(4) 0.0009(4) Cl3 0.0220(5) 0.0239(5) 0.0282(5) 0.0047(4) 0.0046(4) -0.0035(4) Cl4 0.0321(6) 0.0309(6) 0.0339(6) 0.0066(4) 0.0009(4) -0.0113(4) Cl5 0.0337(6) 0.0322(5) 0.0236(5) -0.0049(4) 0.0115(4) -0.0063(4) Cl6 0.0220(5) 0.0262(5) 0.0531(7) 0.0049(5) 0.0132(5) 0.0025(4) O1S 0.0274(15) 0.0235(14) 0.0172(14) 0.0034(11) 0.0015(11) 0.0069(11) O2S 0.0299(15) 0.0253(14) 0.0237(15) -0.0008(11) 0.0007(11) 0.0022(11) C2S 0.026(2) 0.027(2) 0.032(2) 0.0027(18) 0.0033(18) 0.0017(18) O3S 0.0538(19) 0.0260(15) 0.0377(17) -0.0025(12) 0.0166(14) 0.0001(13) O4S 0.0424(18) 0.0263(15) 0.0386(17) -0.0009(12) 0.0114(13) 0.0059(12) O5S 0.062(2) 0.081(2) 0.055(2) -0.0104(18) -0.0061(17) 0.0111(18) O6S 0.0254(18) 0.116(3) 0.091(3) -0.074(2) -0.0001(16) 0.0076(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.476(4) . ? N1 C30 1.477(4) . ? N1 C31 1.479(4) . ? C2 C3 1.505(4) . ? C3 N4 1.488(4) . ? N4 C5 1.489(4) . ? C5 C6 1.506(4) . ? C6 C9 1.377(4) . ? C6 C7 1.389(4) . ? C7 C8 1.383(4) . ? C8 C11 1.392(4) . ? C9 C10 1.378(4) . ? C10 C11 1.372(4) . ? C11 C12 1.498(4) . ? C12 N13 1.508(4) . ? N13 C14 1.486(4) . ? C14 C15 1.516(4) . ? C15 N16 1.470(4) . ? N16 C17 1.476(4) . ? N16 C44 1.476(4) . ? C17 C18 1.505(4) . ? C18 N19 1.489(4) . ? N19 C20 1.493(4) . ? C20 C21 1.505(4) . ? C21 C22 1.380(4) . ? C21 C24 1.388(4) . ? C22 C23 1.383(4) . ? C23 C26 1.383(4) . ? C24 C25 1.391(4) . ? C25 C26 1.379(4) . ? C26 C27 1.502(4) . ? C27 N28 1.503(4) . ? N28 C29 1.482(4) . ? C29 C30 1.513(4) . ? C31 C32 1.515(4) . ? C32 N33 1.491(3) . ? N33 C34 1.491(4) . ? C34 C35 1.516(4) . ? C35 C38 1.385(4) . ? C35 C36 1.386(4) . ? C36 C37 1.391(4) . ? C37 C40 1.376(4) . ? C38 C39 1.380(4) . ? C39 C40 1.387(4) . ? C40 C41 1.511(4) . ? C41 N42 1.496(4) . ? N42 C43 1.494(4) . ? C43 C44 1.510(4) . ? O2S C2S 1.434(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C30 110.1(2) . . ? C2 N1 C31 110.2(2) . . ? C30 N1 C31 109.4(2) . . ? N1 C2 C3 112.8(2) . . ? N4 C3 C2 111.6(3) . . ? C3 N4 C5 112.0(2) . . ? N4 C5 C6 114.2(3) . . ? C9 C6 C7 118.8(3) . . ? C9 C6 C5 119.2(3) . . ? C7 C6 C5 121.9(3) . . ? C8 C7 C6 120.3(3) . . ? C7 C8 C11 120.4(3) . . ? C6 C9 C10 120.6(3) . . ? C11 C10 C9 121.2(3) . . ? C10 C11 C8 118.6(3) . . ? C10 C11 C12 120.1(3) . . ? C8 C11 C12 121.4(3) . . ? C11 C12 N13 112.9(3) . . ? C14 N13 C12 112.2(2) . . ? N13 C14 C15 111.9(3) . . ? N16 C15 C14 112.1(3) . . ? C15 N16 C17 110.5(3) . . ? C15 N16 C44 111.5(2) . . ? C17 N16 C44 111.7(2) . . ? N16 C17 C18 112.9(3) . . ? N19 C18 C17 111.7(3) . . ? C18 N19 C20 111.6(2) . . ? N19 C20 C21 112.8(3) . . ? C22 C21 C24 119.1(3) . . ? C22 C21 C20 120.2(3) . . ? C24 C21 C20 120.7(3) . . ? C21 C22 C23 120.7(3) . . ? C26 C23 C22 120.5(3) . . ? C21 C24 C25 120.0(3) . . ? C26 C25 C24 120.8(3) . . ? C25 C26 C23 119.0(3) . . ? C25 C26 C27 121.3(3) . . ? C23 C26 C27 119.7(3) . . ? C26 C27 N28 111.4(3) . . ? C29 N28 C27 111.4(2) . . ? N28 C29 C30 112.7(3) . . ? N1 C30 C29 113.5(3) . . ? N1 C31 C32 112.8(3) . . ? N33 C32 C31 111.2(2) . . ? C32 N33 C34 112.0(2) . . ? N33 C34 C35 113.9(3) . . ? C38 C35 C36 118.6(3) . . ? C38 C35 C34 118.2(3) . . ? C36 C35 C34 123.2(3) . . ? C35 C36 C37 119.8(3) . . ? C40 C37 C36 121.3(3) . . ? C39 C38 C35 121.5(3) . . ? C38 C39 C40 119.9(3) . . ? C37 C40 C39 118.9(3) . . ? C37 C40 C41 119.0(3) . . ? C39 C40 C41 122.1(3) . . ? N42 C41 C40 114.0(3) . . ? C43 N42 C41 115.0(2) . . ? N42 C43 C44 110.5(2) . . ? N16 C44 C43 110.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 N1 C2 C3 -163.3(3) . . . . ? C31 N1 C2 C3 75.9(3) . . . . ? N1 C2 C3 N4 59.1(3) . . . . ? C2 C3 N4 C5 -179.2(3) . . . . ? C3 N4 C5 C6 167.4(3) . . . . ? N4 C5 C6 C9 -114.7(3) . . . . ? N4 C5 C6 C7 68.4(4) . . . . ? C9 C6 C7 C8 -1.4(5) . . . . ? C5 C6 C7 C8 175.6(3) . . . . ? C6 C7 C8 C11 -0.5(5) . . . . ? C7 C6 C9 C10 1.5(5) . . . . ? C5 C6 C9 C10 -175.5(3) . . . . ? C6 C9 C10 C11 0.2(5) . . . . ? C9 C10 C11 C8 -2.1(5) . . . . ? C9 C10 C11 C12 177.0(3) . . . . ? C7 C8 C11 C10 2.2(5) . . . . ? C7 C8 C11 C12 -176.9(3) . . . . ? C10 C11 C12 N13 100.0(4) . . . . ? C8 C11 C12 N13 -81.0(4) . . . . ? C11 C12 N13 C14 -161.1(3) . . . . ? C12 N13 C14 C15 178.5(3) . . . . ? N13 C14 C15 N16 -57.7(3) . . . . ? C14 C15 N16 C17 167.1(3) . . . . ? C14 C15 N16 C44 -68.1(3) . . . . ? C15 N16 C17 C18 -70.1(3) . . . . ? C44 N16 C17 C18 165.2(3) . . . . ? N16 C17 C18 N19 -61.3(3) . . . . ? C17 C18 N19 C20 171.8(3) . . . . ? C18 N19 C20 C21 -178.5(3) . . . . ? N19 C20 C21 C22 90.0(4) . . . . ? N19 C20 C21 C24 -91.1(4) . . . . ? C24 C21 C22 C23 0.1(5) . . . . ? C20 C21 C22 C23 179.1(3) . . . . ? C21 C22 C23 C26 0.1(5) . . . . ? C22 C21 C24 C25 0.1(5) . . . . ? C20 C21 C24 C25 -178.8(3) . . . . ? C21 C24 C25 C26 -0.6(5) . . . . ? C24 C25 C26 C23 0.9(5) . . . . ? C24 C25 C26 C27 -178.1(3) . . . . ? C22 C23 C26 C25 -0.6(5) . . . . ? C22 C23 C26 C27 178.3(3) . . . . ? C25 C26 C27 N28 94.5(4) . . . . ? C23 C26 C27 N28 -84.4(4) . . . . ? C26 C27 N28 C29 170.2(3) . . . . ? C27 N28 C29 C30 174.6(3) . . . . ? C2 N1 C30 C29 76.6(3) . . . . ? C31 N1 C30 C29 -162.2(3) . . . . ? N28 C29 C30 N1 64.7(3) . . . . ? C2 N1 C31 C32 -159.1(2) . . . . ? C30 N1 C31 C32 79.7(3) . . . . ? N1 C31 C32 N33 72.3(3) . . . . ? C31 C32 N33 C34 -179.0(3) . . . . ? C32 N33 C34 C35 -175.4(3) . . . . ? N33 C34 C35 C38 -171.6(3) . . . . ? N33 C34 C35 C36 9.7(4) . . . . ? C38 C35 C36 C37 -0.5(5) . . . . ? C34 C35 C36 C37 178.3(3) . . . . ? C35 C36 C37 C40 -0.5(5) . . . . ? C36 C35 C38 C39 1.0(5) . . . . ? C34 C35 C38 C39 -177.7(3) . . . . ? C35 C38 C39 C40 -0.7(5) . . . . ? C36 C37 C40 C39 0.9(5) . . . . ? C36 C37 C40 C41 -178.8(3) . . . . ? C38 C39 C40 C37 -0.3(5) . . . . ? C38 C39 C40 C41 179.3(3) . . . . ? C37 C40 C41 N42 -120.3(3) . . . . ? C39 C40 C41 N42 60.1(4) . . . . ? C40 C41 N42 C43 44.4(4) . . . . ? C41 N42 C43 C44 169.7(3) . . . . ? C15 N16 C44 C43 115.6(3) . . . . ? C17 N16 C44 C43 -120.3(3) . . . . ? N42 C43 C44 N16 179.0(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A Cl4 0.92 2.19 3.096(3) 169.7 . N4 H4B Cl1 0.92 2.28 3.129(3) 152.7 . N13 H13A O1S 0.92 2.01 2.831(3) 147.4 . N13 H13B Cl3 0.92 2.14 3.047(3) 170.1 . N19 H19A O1S 0.92 2.22 3.088(3) 157.6 . N19 H19B O4S 0.92 2.10 2.859(3) 139.5 . N19 H19B O2S 0.92 2.32 2.935(3) 124.3 . N28 H28A Cl3 0.92 2.23 3.136(3) 170.2 2 N28 H28B Cl1 0.92 2.32 3.167(3) 152.6 . N33 H33B Cl1 0.92 2.19 3.089(3) 165.0 . N33 H33A Cl2 0.92 2.35 3.243(3) 163.2 . N42 H42B Cl5 0.92 2.18 3.095(3) 170.9 . N42 H42A O5S 0.92 2.20 2.977(4) 141.5 . N42 H42A Cl6 0.92 2.78 3.328(3) 119.5 . O1S H1SA Cl1 0.90 2.35 3.245(2) 179.6 . O1S H1SB O2S 0.90 1.83 2.727(3) 179.4 . O2S H2S O6S 0.90 1.78 2.676(3) 178.9 . O3S H3SB Cl5 0.90 2.43 3.331(2) 179.6 2_645 O3S H3SA Cl2 0.90 2.41 3.306(3) 179.7 . O4S H4SA O5S 0.90 2.11 2.852(4) 138.6 1_455 O4S H4SB Cl4 0.90 2.38 3.285(2) 179.2 2 O5S H5SA Cl6 0.90 2.20 3.038(3) 154.6 . O5S H5SB Cl5 0.90 2.39 3.224(3) 155.0 3_766 O6S H6SA Cl4 0.90 2.18 3.077(3) 179.1 2 O6S H6SB Cl5 0.90 2.25 3.147(3) 179.1 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.643 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.065 #===END data_compound_2A_ #data_01085 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H60 N8 6+, 2(H2 P O4) 1-, 4 Cl 1-, 7.5(H2 O), 0.25(C2 H6 O)' _chemical_formula_sum 'C36.50 H80.50 Cl4 N8 O15.75 P2' _chemical_formula_weight 1087.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.9882(17) _cell_length_b 20.6547(11) _cell_length_c 32.8991(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.456(2) _cell_angle_gamma 90.00 _cell_volume 21056(2) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5514 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.74 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9272 _exptl_absorpt_coefficient_mu 0.355 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9134 _exptl_absorpt_correction_T_max 0.9790 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '\w scan frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 325 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59671 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18493 _reflns_number_gt 13177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+252.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18493 _refine_ls_number_parameters 1305 _refine_ls_number_restraints 156 _refine_ls_R_factor_all 0.1379 _refine_ls_R_factor_gt 0.1067 _refine_ls_wR_factor_ref 0.3049 _refine_ls_wR_factor_gt 0.2839 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1A N 0.13675(18) 0.4650(3) 0.8511(2) 0.0392(14) Uani 1 1 d . A . C2A C 0.1323(3) 0.5228(5) 0.8756(3) 0.071(3) Uani 1 1 d . . . H2AA H 0.1165 0.5111 0.9006 0.086 Uiso 1 1 calc R . . H2AB H 0.1141 0.5540 0.8603 0.086 Uiso 1 1 calc R . . C3A C 0.1730(3) 0.5567(5) 0.8880(3) 0.053(2) Uani 1 1 d . . . H3AA H 0.1652 0.5966 0.9029 0.064 Uiso 1 1 calc R . . H3AB H 0.1890 0.5284 0.9071 0.064 Uiso 1 1 calc R . . N4A N 0.2018(2) 0.5744(4) 0.8547(2) 0.0546(19) Uani 1 1 d . . . H4AA H 0.2114 0.5369 0.8426 0.066 Uiso 1 1 calc R . . H4AB H 0.1861 0.5969 0.8355 0.066 Uiso 1 1 calc R . . C5A C 0.2383(3) 0.6121(6) 0.8658(3) 0.081(4) Uani 1 1 d . . . H5AA H 0.2528 0.5908 0.8891 0.097 Uiso 1 1 calc R . . H5AB H 0.2279 0.6548 0.8752 0.097 Uiso 1 1 calc R . . C6A C 0.2718(3) 0.6235(4) 0.8328(2) 0.046(2) Uani 1 1 d . . . C7A C 0.3091(3) 0.5871(4) 0.8343(2) 0.0456(19) Uani 1 1 d . . . H7A H 0.3125 0.5542 0.8543 0.055 Uiso 1 1 calc R . . C8A C 0.3414(2) 0.5987(4) 0.8067(2) 0.0407(17) Uani 1 1 d . . . H8A H 0.3669 0.5733 0.8078 0.049 Uiso 1 1 calc R . . C9A C 0.2671(2) 0.6707(4) 0.8038(3) 0.051(2) Uani 1 1 d . . . H9A H 0.2415 0.6961 0.8027 0.061 Uiso 1 1 calc R . . C10A C 0.2999(3) 0.6812(4) 0.7759(2) 0.0430(18) Uani 1 1 d . . . H10A H 0.2963 0.7132 0.7554 0.052 Uiso 1 1 calc R . . C11A C 0.3376(2) 0.6459(3) 0.7778(2) 0.0360(16) Uani 1 1 d . . . C12A C 0.3747(3) 0.6580(4) 0.7495(3) 0.051(2) Uani 1 1 d . . . H12A H 0.3722 0.7025 0.7385 0.062 Uiso 1 1 calc R . . H12B H 0.4020 0.6553 0.7652 0.062 Uiso 1 1 calc R . . N13A N 0.37620(18) 0.6131(3) 0.71642(18) 0.0352(13) Uani 1 1 d . A . H13A H 0.3507 0.6159 0.7020 0.042 Uiso 1 1 calc R . . H13B H 0.3780 0.5719 0.7269 0.042 Uiso 1 1 calc R . . C14A C 0.4124(2) 0.6226(4) 0.6878(2) 0.0434(18) Uani 1 1 d D . . H14A H 0.4390 0.6052 0.7005 0.052 Uiso 0.619(13) 1 calc PR A 1 H14B H 0.4167 0.6697 0.6839 0.052 Uiso 0.619(13) 1 calc PR A 1 H14C H 0.4360 0.6427 0.7021 0.052 Uiso 0.381(13) 1 d PR A 2 H14D H 0.4033 0.6517 0.6667 0.052 Uiso 0.381(13) 1 d PR A 2 C15A C 0.4070(4) 0.5917(4) 0.6465(2) 0.037(3) Uani 0.619(13) 1 d PD A 1 H15A H 0.3867 0.6183 0.6302 0.045 Uiso 0.619(13) 1 calc PR A 1 H15B H 0.4352 0.5921 0.6326 0.045 Uiso 0.619(13) 1 calc PR A 1 C15' C 0.4267(3) 0.5647(6) 0.6634(5) 0.040(5) Uani 0.381(13) 1 d PD A 2 H15G H 0.4441 0.5800 0.6402 0.048 Uiso 0.381(13) 1 calc PR A 2 H15H H 0.4456 0.5374 0.6807 0.048 Uiso 0.381(13) 1 calc PR A 2 N16A N 0.39076(16) 0.5243(2) 0.64766(16) 0.0333(13) Uani 1 1 d D . . C17A C 0.3734(3) 0.5027(5) 0.6078(2) 0.037(3) Uani 0.619(13) 1 d PD A 1 H17A H 0.3689 0.4552 0.6087 0.045 Uiso 0.619(13) 1 calc PR A 1 H17B H 0.3950 0.5119 0.5866 0.045 Uiso 0.619(13) 1 calc PR A 1 C17' C 0.3749(4) 0.5581(8) 0.6106(4) 0.043(6) Uani 0.381(13) 1 d PD A 2 H17C H 0.3961 0.5518 0.5886 0.052 Uiso 0.381(13) 1 calc PR A 2 H17D H 0.3732 0.6051 0.6163 0.052 Uiso 0.381(13) 1 calc PR A 2 C18A C 0.3313(2) 0.5348(4) 0.5961(2) 0.0412(17) Uani 1 1 d D . . H18A H 0.3372 0.5804 0.5888 0.049 Uiso 0.619(13) 1 calc PR A 1 H18B H 0.3195 0.5130 0.5716 0.049 Uiso 0.619(13) 1 calc PR A 1 H18C H 0.3203 0.5579 0.5729 0.049 Uiso 0.381(13) 1 d PR A 2 H18D H 0.3372 0.4912 0.5878 0.049 Uiso 0.381(13) 1 d PR A 2 N19A N 0.29790(18) 0.5339(3) 0.62817(18) 0.0381(14) Uani 1 1 d . A . H19A H 0.3042 0.5654 0.6471 0.046 Uiso 1 1 calc R . . H19B H 0.2987 0.4945 0.6412 0.046 Uiso 1 1 calc R . . C20A C 0.2535(2) 0.5450(4) 0.6118(2) 0.0420(18) Uani 1 1 d . . . H20A H 0.2475 0.5129 0.5901 0.050 Uiso 1 1 calc R A . H20B H 0.2521 0.5886 0.5994 0.050 Uiso 1 1 calc R . . C21A C 0.2190(2) 0.5396(4) 0.6442(2) 0.0379(17) Uani 1 1 d . A . C22A C 0.1933(3) 0.4849(4) 0.6448(2) 0.050(2) Uani 1 1 d . . . H22A H 0.1987 0.4503 0.6265 0.060 Uiso 1 1 calc R A . C23A C 0.1596(3) 0.4806(5) 0.6723(3) 0.064(3) Uani 1 1 d . A . H23A H 0.1416 0.4433 0.6725 0.076 Uiso 1 1 calc R . . C24A C 0.2120(2) 0.5890(4) 0.6719(3) 0.0423(18) Uani 1 1 d . . . H24A H 0.2300 0.6262 0.6721 0.051 Uiso 1 1 calc R A . C25A C 0.1784(3) 0.5836(4) 0.6995(3) 0.050(2) Uani 1 1 d . A . H25A H 0.1737 0.6170 0.7189 0.059 Uiso 1 1 calc R . . C26A C 0.1521(2) 0.5303(4) 0.6990(3) 0.047(2) Uani 1 1 d . . . C27A C 0.1139(3) 0.5269(6) 0.7280(3) 0.071(3) Uani 1 1 d . A . H27A H 0.1058 0.5716 0.7357 0.085 Uiso 1 1 calc R . . H27B H 0.0890 0.5076 0.7133 0.085 Uiso 1 1 calc R . . N28A N 0.12152(19) 0.4905(4) 0.7641(2) 0.0476(16) Uani 1 1 d . . . H28A H 0.1458 0.5067 0.7768 0.057 Uiso 1 1 calc R A . H28B H 0.1273 0.4484 0.7569 0.057 Uiso 1 1 calc R . . C29A C 0.0858(2) 0.4902(4) 0.7940(3) 0.050(2) Uani 1 1 d . A . H29A H 0.0799 0.5353 0.8025 0.060 Uiso 1 1 calc R . . H29B H 0.0594 0.4732 0.7806 0.060 Uiso 1 1 calc R . . C30A C 0.0952(3) 0.4509(6) 0.8304(3) 0.070(3) Uani 1 1 d . . . H30A H 0.0949 0.4046 0.8225 0.084 Uiso 1 1 calc R A . H30B H 0.0716 0.4575 0.8502 0.084 Uiso 1 1 calc R . . C31A C 0.1489(4) 0.4097(5) 0.8748(4) 0.081(4) Uani 1 1 d . . . H31A H 0.1231 0.3964 0.8904 0.097 Uiso 1 1 calc R A . H31B H 0.1707 0.4244 0.8949 0.097 Uiso 1 1 calc R . . C32A C 0.1658(3) 0.3521(5) 0.8556(4) 0.085(4) Uani 1 1 d . A . H32A H 0.1729 0.3206 0.8773 0.103 Uiso 1 1 calc R . . H32B H 0.1424 0.3329 0.8389 0.103 Uiso 1 1 calc R . . N33A N 0.2033(3) 0.3586(5) 0.8301(4) 0.120(5) Uani 1 1 d . . . H33A H 0.1980 0.3359 0.8065 0.144 Uiso 1 1 calc R A . H33B H 0.2057 0.4016 0.8230 0.144 Uiso 1 1 calc R . . C34A C 0.2426(3) 0.3392(6) 0.8447(4) 0.078(3) Uani 1 1 d . A . H34A H 0.2397 0.2944 0.8549 0.094 Uiso 1 1 calc R . . H34B H 0.2502 0.3670 0.8682 0.094 Uiso 1 1 calc R . . C35A C 0.2806(2) 0.3409(4) 0.8146(3) 0.048(2) Uani 1 1 d . . . C36A C 0.2895(3) 0.2906(4) 0.7889(3) 0.054(2) Uani 1 1 d . A . H36A H 0.2727 0.2522 0.7900 0.065 Uiso 1 1 calc R . . C37A C 0.3226(3) 0.2952(4) 0.7616(3) 0.050(2) Uani 1 1 d . . . H37A H 0.3279 0.2604 0.7434 0.060 Uiso 1 1 calc R A . C38A C 0.3065(2) 0.3958(3) 0.8138(2) 0.0387(17) Uani 1 1 d . A . H38A H 0.3007 0.4307 0.8318 0.046 Uiso 1 1 calc R . . C39A C 0.3405(2) 0.4001(3) 0.7873(2) 0.0298(14) Uani 1 1 d . . . H39A H 0.3586 0.4373 0.7878 0.036 Uiso 1 1 calc R A . C40A C 0.3487(2) 0.3508(3) 0.7601(2) 0.0369(16) Uani 1 1 d . A . C41A C 0.3851(3) 0.3547(4) 0.7304(2) 0.049(2) Uani 1 1 d . . . H41A H 0.4128 0.3519 0.7454 0.059 Uiso 1 1 calc R A . H41B H 0.3833 0.3172 0.7117 0.059 Uiso 1 1 calc R . . N42A N 0.38440(18) 0.4153(3) 0.70622(17) 0.0323(13) Uani 1 1 d . A . H42A H 0.3900 0.4497 0.7232 0.039 Uiso 1 1 calc R . . H42B H 0.3572 0.4210 0.6954 0.039 Uiso 1 1 calc R . . C43A C 0.4164(2) 0.4155(3) 0.6726(2) 0.0401(17) Uani 1 1 d D . . H43A H 0.4043 0.3910 0.6493 0.048 Uiso 0.619(13) 1 calc PR A 1 H43B H 0.4429 0.3929 0.6819 0.048 Uiso 0.619(13) 1 calc PR A 1 H43C H 0.4192 0.3720 0.6627 0.048 Uiso 0.381(13) 1 d PR A 2 H43D H 0.4439 0.4282 0.6835 0.048 Uiso 0.381(13) 1 d PR A 2 C44A C 0.4281(2) 0.4827(4) 0.6587(4) 0.036(3) Uani 0.619(13) 1 d PD A 1 H44A H 0.4448 0.5043 0.6806 0.043 Uiso 0.619(13) 1 calc PR A 1 H44B H 0.4472 0.4791 0.6347 0.043 Uiso 0.619(13) 1 calc PR A 1 C44' C 0.4061(6) 0.4587(5) 0.6368(3) 0.045(6) Uani 0.381(13) 1 d PD A 2 H44C H 0.4324 0.4631 0.6201 0.053 Uiso 0.381(13) 1 calc PR A 2 H44D H 0.3837 0.4374 0.6199 0.053 Uiso 0.381(13) 1 calc PR A 2 N1B N 0.61613(19) 0.2439(3) 0.6083(2) 0.0408(15) Uani 1 1 d . B . C2B C 0.6232(3) 0.1820(4) 0.6271(3) 0.067(3) Uani 1 1 d . . . H2BA H 0.6424 0.1880 0.6511 0.080 Uiso 1 1 calc R . . H2BB H 0.6384 0.1536 0.6077 0.080 Uiso 1 1 calc R . . C3B C 0.5821(3) 0.1481(4) 0.6408(3) 0.060(3) Uani 1 1 d . . . H3BA H 0.5896 0.1060 0.6533 0.072 Uiso 1 1 calc R . . H3BB H 0.5676 0.1749 0.6616 0.072 Uiso 1 1 calc R . . N4B N 0.5520(2) 0.1373(3) 0.6060(2) 0.0507(18) Uani 1 1 d . . . H4BA H 0.5659 0.1146 0.5859 0.061 Uiso 1 1 calc R . . H4BB H 0.5436 0.1766 0.5954 0.061 Uiso 1 1 calc R . . C5B C 0.5130(3) 0.1002(4) 0.6194(3) 0.0462(19) Uani 1 1 d . . . H5BA H 0.5010 0.1208 0.6440 0.055 Uiso 1 1 calc R . . H5BB H 0.5216 0.0555 0.6266 0.055 Uiso 1 1 calc R . . C6B C 0.4785(2) 0.0977(3) 0.5868(2) 0.0334(15) Uani 1 1 d . . . C7B C 0.4463(2) 0.1447(3) 0.5860(2) 0.0359(16) Uani 1 1 d . . . H7B H 0.4469 0.1790 0.6053 0.043 Uiso 1 1 calc R . . C8B C 0.4137(2) 0.1418(3) 0.5577(2) 0.0318(15) Uani 1 1 d . . . H8B H 0.3918 0.1740 0.5577 0.038 Uiso 1 1 calc R . . C9B C 0.4774(2) 0.0486(3) 0.5578(2) 0.0352(16) Uani 1 1 d . . . H9B H 0.4993 0.0164 0.5576 0.042 Uiso 1 1 calc R . . C10B C 0.4443(2) 0.0466(3) 0.5295(2) 0.0344(15) Uani 1 1 d . . . H10B H 0.4437 0.0129 0.5098 0.041 Uiso 1 1 calc R . . C11B C 0.4121(2) 0.0929(3) 0.5293(2) 0.0290(14) Uani 1 1 d . . . C12B C 0.3738(2) 0.0881(3) 0.5007(2) 0.0320(15) Uani 1 1 d . . . H12C H 0.3716 0.0430 0.4907 0.038 Uiso 1 1 calc R . . H12D H 0.3472 0.0976 0.5161 0.038 Uiso 1 1 calc R . . N13B N 0.37595(18) 0.1320(3) 0.46566(18) 0.0345(13) Uani 1 1 d . B . H13C H 0.3997 0.1213 0.4504 0.041 Uiso 1 1 calc R . . H13D H 0.3798 0.1736 0.4750 0.041 Uiso 1 1 calc R . . C14B C 0.3372(2) 0.1302(3) 0.43921(18) 0.0308(15) Uani 1 1 d D . . H14E H 0.3130 0.1510 0.4537 0.037 Uiso 0.793(12) 1 calc PR B 1 H14F H 0.3292 0.0844 0.4343 0.037 Uiso 0.793(12) 1 calc PR B 1 H14G H 0.3131 0.1152 0.4548 0.037 Uiso 0.207(12) 1 d PR B 2 H14H H 0.3420 0.0993 0.4179 0.037 Uiso 0.207(12) 1 d PR B 2 C15B C 0.3428(3) 0.1634(3) 0.3988(2) 0.032(2) Uani 0.793(12) 1 d PD B 1 H15E H 0.3635 0.1383 0.3823 0.038 Uiso 0.793(12) 1 calc PR B 1 H15F H 0.3148 0.1637 0.3841 0.038 Uiso 0.793(12) 1 calc PR B 1 C15" C 0.3224(3) 0.1911(8) 0.4180(8) 0.027(8) Uani 0.207(12) 1 d PD B 2 H15G H 0.3034 0.1793 0.3949 0.033 Uiso 0.207(12) 1 calc PR B 2 H15H H 0.3052 0.2174 0.4371 0.033 Uiso 0.207(12) 1 calc PR B 2 N16B N 0.35870(15) 0.2309(2) 0.40271(15) 0.0270(11) Uani 1 1 d D . . C17B C 0.3762(2) 0.2546(4) 0.3636(2) 0.033(2) Uani 0.793(12) 1 d PD B 1 H17E H 0.3822 0.3015 0.3661 0.039 Uiso 0.793(12) 1 calc PR B 1 H17F H 0.3539 0.2490 0.3422 0.039 Uiso 0.793(12) 1 calc PR B 1 C17" C 0.3736(5) 0.1986(12) 0.3651(6) 0.040(10) Uani 0.207(12) 1 d PD B 2 H17G H 0.3519 0.2060 0.3433 0.048 Uiso 0.207(12) 1 calc PR B 2 H17H H 0.3750 0.1513 0.3700 0.048 Uiso 0.207(12) 1 calc PR B 2 C18B C 0.41704(19) 0.2210(3) 0.3501(2) 0.0335(15) Uani 1 1 d D . . H18E H 0.4098 0.1761 0.3420 0.040 Uiso 0.793(12) 1 calc PR B 1 H18F H 0.4282 0.2435 0.3258 0.040 Uiso 0.793(12) 1 calc PR B 1 H18G H 0.4259 0.1952 0.3273 0.040 Uiso 0.207(12) 1 d PR B 2 H18H H 0.4140 0.2648 0.3407 0.040 Uiso 0.207(12) 1 d PR B 2 N19B N 0.45178(18) 0.2189(3) 0.38171(17) 0.0323(13) Uani 1 1 d . B . H19C H 0.4451 0.1878 0.4007 0.039 Uiso 1 1 calc R . . H19D H 0.4530 0.2582 0.3948 0.039 Uiso 1 1 calc R . . C20B C 0.4953(2) 0.2041(4) 0.3639(2) 0.0372(16) Uani 1 1 d . . . H20C H 0.5022 0.2372 0.3432 0.045 Uiso 1 1 calc R B . H20D H 0.4941 0.1615 0.3502 0.045 Uiso 1 1 calc R . . C21B C 0.5306(2) 0.2031(3) 0.3958(2) 0.0329(15) Uani 1 1 d . B . C22B C 0.5615(3) 0.2523(4) 0.3966(3) 0.0462(19) Uani 1 1 d . . . H22B H 0.5592 0.2872 0.3779 0.055 Uiso 1 1 calc R B . C23B C 0.5954(2) 0.2508(4) 0.4241(3) 0.0464(19) Uani 1 1 d . B . H23B H 0.6164 0.2843 0.4238 0.056 Uiso 1 1 calc R . . C24B C 0.5344(2) 0.1537(3) 0.4239(2) 0.0350(16) Uani 1 1 d . . . H24B H 0.5138 0.1197 0.4241 0.042 Uiso 1 1 calc R B . C25B C 0.5681(2) 0.1534(4) 0.4520(2) 0.0395(17) Uani 1 1 d . B . H25B H 0.5699 0.1196 0.4715 0.047 Uiso 1 1 calc R . . C26B C 0.5990(2) 0.2014(4) 0.4518(2) 0.0388(17) Uani 1 1 d . . . C27B C 0.6367(2) 0.1997(5) 0.4805(3) 0.052(2) Uani 1 1 d . B . H27C H 0.6625 0.2163 0.4664 0.062 Uiso 1 1 calc R . . H27D H 0.6424 0.1543 0.4884 0.062 Uiso 1 1 calc R . . N28B N 0.6295(2) 0.2393(4) 0.5184(2) 0.0479(17) Uani 1 1 d . . . H28C H 0.6277 0.2824 0.5115 0.058 Uiso 1 1 calc R B . H28D H 0.6037 0.2275 0.5299 0.058 Uiso 1 1 calc R . . C29B C 0.6647(2) 0.2300(5) 0.5483(3) 0.057(2) Uani 1 1 d . B . H29C H 0.6922 0.2453 0.5365 0.068 Uiso 1 1 calc R . . H29D H 0.6678 0.1833 0.5544 0.068 Uiso 1 1 calc R . . C30B C 0.6562(2) 0.2662(4) 0.5869(3) 0.051(2) Uani 1 1 d . . . H30C H 0.6534 0.3129 0.5806 0.061 Uiso 1 1 calc R B . H30D H 0.6813 0.2609 0.6054 0.061 Uiso 1 1 calc R . . C31B C 0.6042(3) 0.2928(4) 0.6385(3) 0.052(2) Uani 1 1 d . . . H31C H 0.6303 0.3047 0.6543 0.063 Uiso 1 1 calc R B . H31D H 0.5835 0.2730 0.6576 0.063 Uiso 1 1 calc R . . C32B C 0.5846(2) 0.3531(4) 0.6219(3) 0.0462(19) Uani 1 1 d . B . H32C H 0.6035 0.3705 0.6004 0.055 Uiso 1 1 calc R . . H32D H 0.5831 0.3858 0.6438 0.055 Uiso 1 1 calc R . . N33B N 0.54032(19) 0.3431(3) 0.6045(2) 0.0399(14) Uani 1 1 d . . . H33C H 0.5419 0.3152 0.5828 0.048 Uiso 1 1 calc R B . H33D H 0.5231 0.3242 0.6239 0.048 Uiso 1 1 calc R . . C34B C 0.5202(2) 0.4050(3) 0.5908(3) 0.0439(19) Uani 1 1 d . B . H34C H 0.5413 0.4287 0.5740 0.053 Uiso 1 1 calc R . . H34D H 0.5143 0.4318 0.6151 0.053 Uiso 1 1 calc R . . C35B C 0.4792(2) 0.3977(3) 0.5669(2) 0.0317(15) Uani 1 1 d . . . C36B C 0.4705(2) 0.4435(3) 0.5374(2) 0.0365(16) Uani 1 1 d . B . H36B H 0.4909 0.4769 0.5326 0.044 Uiso 1 1 calc R . . C37B C 0.4329(2) 0.4418(3) 0.5148(2) 0.0335(15) Uani 1 1 d . . . H37B H 0.4274 0.4741 0.4949 0.040 Uiso 1 1 calc R B . C38B C 0.4486(2) 0.3491(3) 0.5736(2) 0.0355(16) Uani 1 1 d . B . H38B H 0.4536 0.3176 0.5941 0.043 Uiso 1 1 calc R . . C39B C 0.4111(2) 0.3470(3) 0.5504(2) 0.0335(15) Uani 1 1 d . . . H39B H 0.3907 0.3133 0.5547 0.040 Uiso 1 1 calc R B . C40B C 0.4031(2) 0.3932(3) 0.5211(2) 0.0308(15) Uani 1 1 d . B . C41B C 0.3629(2) 0.3895(3) 0.4941(2) 0.0338(15) Uani 1 1 d . . . H41C H 0.3371 0.3845 0.5114 0.041 Uiso 1 1 calc R B . H41D H 0.3598 0.4304 0.4786 0.041 Uiso 1 1 calc R . . N42B N 0.36553(18) 0.3340(3) 0.46526(17) 0.0307(12) Uani 1 1 d . B . H42C H 0.3930 0.3321 0.4550 0.037 Uiso 1 1 calc R . . H42D H 0.3607 0.2963 0.4793 0.037 Uiso 1 1 calc R . . C43B C 0.3342(2) 0.3381(3) 0.4308(2) 0.0304(14) Uani 1 1 d D . . H43E H 0.3472 0.3636 0.4085 0.037 Uiso 0.793(12) 1 calc PR B 1 H43F H 0.3080 0.3611 0.4399 0.037 Uiso 0.793(12) 1 calc PR B 1 H43G H 0.3301 0.3827 0.4235 0.037 Uiso 0.207(12) 1 d PR B 2 H43H H 0.3069 0.3212 0.4394 0.037 Uiso 0.207(12) 1 d PR B 2 C44B C 0.3216(2) 0.2722(3) 0.4148(3) 0.032(2) Uani 0.793(12) 1 d PD B 1 H44E H 0.3050 0.2493 0.4359 0.038 Uiso 0.793(12) 1 calc PR B 1 H44F H 0.3023 0.2780 0.3909 0.038 Uiso 0.793(12) 1 calc PR B 1 C44" C 0.3490(9) 0.3001(5) 0.3942(3) 0.039(10) Uani 0.207(12) 1 d PD B 2 H44G H 0.3262 0.3023 0.3730 0.047 Uiso 0.207(12) 1 calc PR B 2 H44H H 0.3752 0.3208 0.3832 0.047 Uiso 0.207(12) 1 calc PR B 2 P1 P 0.29419(6) 0.35677(9) 0.63961(6) 0.0338(4) Uani 1 1 d . . . O1 O 0.30545(15) 0.4145(2) 0.66546(15) 0.0377(11) Uani 1 1 d . . . O2 O 0.27489(16) 0.3850(2) 0.59863(15) 0.0399(12) Uani 1 1 d . . . H2 H 0.2785 0.3500 0.5807 0.048 Uiso 1 1 d R . . O3 O 0.33070(17) 0.3117(3) 0.63024(18) 0.0545(16) Uani 1 1 d . . . O4 O 0.25727(17) 0.3168(3) 0.65902(16) 0.0454(13) Uani 1 1 d . . . H4 H 0.2432 0.3348 0.6797 0.054 Uiso 1 1 d R . . P2 P 0.29980(5) 0.23651(8) 0.53849(5) 0.0260(4) Uani 1 1 d . . . O5 O 0.33744(14) 0.2350(2) 0.51039(14) 0.0302(10) Uani 1 1 d . . . O6 O 0.27502(14) 0.3001(2) 0.53778(14) 0.0310(10) Uani 1 1 d . . . O7 O 0.31366(16) 0.2187(2) 0.58280(14) 0.0363(11) Uani 1 1 d . . . H7 H 0.3153 0.2525 0.5943 0.044 Uiso 1 1 d R . . O8 O 0.26808(14) 0.1784(2) 0.52812(15) 0.0331(10) Uani 1 1 d . . . H8 H 0.2513 0.1826 0.5014 0.040 Uiso 1 1 d R . . P3 P 0.44888(8) 0.50683(12) 0.79107(8) 0.0572(6) Uani 1 1 d . . . O9 O 0.41758(15) 0.5095(2) 0.75720(15) 0.0381(11) Uani 1 1 d . . . O10 O 0.4261(3) 0.4876(3) 0.8314(2) 0.087(3) Uani 1 1 d . . . H10 H 0.4252 0.5125 0.8520 0.105 Uiso 1 1 d R . . O11 O 0.4737(2) 0.5687(3) 0.79900(19) 0.0658(18) Uani 1 1 d . . . H11 H 0.4785 0.6085 0.7748 0.079 Uiso 1 1 d R . . O12 O 0.4800(2) 0.4507(4) 0.7854(3) 0.097(3) Uani 1 1 d . . . P4 P 0.45739(6) 0.38963(9) 0.40174(6) 0.0382(4) Uani 1 1 d . . . O13 O 0.44449(15) 0.3329(2) 0.42754(15) 0.0372(11) Uani 1 1 d . . . O14 O 0.42314(19) 0.4380(3) 0.3924(2) 0.0562(15) Uani 1 1 d . . . O15 O 0.47553(18) 0.3588(3) 0.36141(16) 0.0462(13) Uani 1 1 d . . . H15 H 0.4685 0.3923 0.3374 0.055 Uiso 1 1 d R . . O16 O 0.49568(18) 0.4268(3) 0.42146(18) 0.0495(14) Uani 1 1 d . . . H16 H 0.5161 0.4034 0.4307 0.059 Uiso 1 1 d R . . Cl1 Cl 0.22230(5) 0.48503(8) 0.77997(5) 0.0319(4) Uani 1 1 d . . . Cl2 Cl 0.52946(5) 0.23995(8) 0.53602(5) 0.0321(4) Uani 1 1 d . . . Cl3 Cl 0.30935(7) 0.68485(11) 0.65670(9) 0.0623(6) Uani 1 1 d . . . Cl4 Cl 0.12353(7) 0.33681(10) 0.74730(7) 0.0565(6) Uani 1 1 d . . . Cl5 Cl 0.43626(7) 0.06545(10) 0.39812(7) 0.0537(5) Uani 1 1 d . . . Cl6 Cl 0.63536(8) 0.39031(13) 0.50329(9) 0.0726(7) Uani 1 1 d . . . Cl7 Cl 0.13761(12) 0.64982(16) 0.79693(12) 0.0459(10) Uani 0.537(4) 1 d P C 1 Cl7' Cl 0.1561(6) 0.6849(8) 0.8207(5) 0.054(6) Uani 0.129(8) 1 d P D 2 Cl7" Cl 0.0668(5) 0.6657(7) 0.7971(5) 0.067(6) Uani 0.157(8) 1 d P E 3 Cl7# Cl 0.0600(8) 0.6787(13) 0.7364(6) 0.130(12) Uani 0.177(9) 1 d P F 4 Cl8 Cl 0.18986(12) 0.44650(18) 1.02606(14) 0.1101(12) Uani 1 1 d . . . O1S O 0.30501(14) 0.5192(2) 0.72055(14) 0.0334(11) Uani 1 1 d D . . H1SA H 0.2833 0.5369 0.7314 0.040 Uiso 1 1 d RD . . H1SB H 0.2969 0.4836 0.7102 0.040 Uiso 1 1 d RD . . O2S O 0.44650(14) 0.2210(2) 0.47466(14) 0.0346(11) Uani 1 1 d D . . H2SA H 0.4636 0.2134 0.4944 0.042 Uiso 1 1 d RD . . H2SB H 0.4493 0.2604 0.4681 0.042 Uiso 1 1 d RD . . O3S O 0.6023(2) 0.0561(2) 0.55603(17) 0.0505(14) Uani 1 1 d D . . H3SA H 0.6206 0.0462 0.5742 0.061 Uiso 1 1 d RD . . H3SB H 0.6189 0.0863 0.5355 0.061 Uiso 1 1 d RD . . O4S O 0.21942(18) 0.3574(3) 0.72394(17) 0.0502(14) Uani 1 1 d D . . H4SA H 0.2134 0.3854 0.7058 0.060 Uiso 1 1 d RD . . H4SB H 0.1964 0.3494 0.7369 0.060 Uiso 1 1 d RD . . O5S O 0.53997(18) 0.3699(3) 0.4786(2) 0.0601(16) Uani 1 1 d D . . H5SA H 0.5666 0.3704 0.4854 0.072 Uiso 1 1 d RD . . H5SB H 0.5258 0.3695 0.5007 0.072 Uiso 1 1 d RD . . O6S O 0.47821(19) 0.0378(3) 0.31408(19) 0.0585(16) Uani 1 1 d D . . H6SA H 0.4731 0.0702 0.3291 0.070 Uiso 1 1 d RD . . H6SB H 0.4891 0.0513 0.2921 0.070 Uiso 1 1 d RD . . O7S O 0.5000 0.6594(5) 0.7500 0.077(3) Uani 1 2 d SD . . H7S H 0.4981 0.6821 0.7714 0.093 Uiso 1 1 d RD . . O8S O 0.2692(2) 0.4684(4) 0.9116(2) 0.076(2) Uani 1 1 d D . . H8SA H 0.2917 0.4648 0.9264 0.092 Uiso 1 1 d RD . . H8SB H 0.2563 0.5027 0.9190 0.092 Uiso 1 1 d RD . . O9S O 0.3560(3) 0.5178(4) 0.4195(3) 0.087(2) Uani 1 1 d D . . H9SA H 0.3759 0.5342 0.4343 0.104 Uiso 1 1 d RD . . H9SB H 0.3660 0.4829 0.4095 0.104 Uiso 1 1 d RD . . O10S O 0.7321(3) 0.3620(5) 0.4838(3) 0.116(3) Uani 1 1 d D . . H10S H 0.7052 0.3618 0.4785 0.139 Uiso 1 1 d RD . . H10T H 0.7450 0.3713 0.4618 0.139 Uiso 1 1 d RD . . O11S O 0.0938(3) 0.7524(4) 0.8492(3) 0.098(3) Uani 1 1 d D . . H11S H 0.1061 0.7316 0.8301 0.118 Uiso 1 1 d RD . . H11T H 0.1134 0.7646 0.8659 0.118 Uiso 1 1 d RD . . O12S O 0.2723(3) 0.7309(5) 0.5728(3) 0.119(3) Uani 1 1 d D . . H12S H 0.2823 0.7185 0.5956 0.143 Uiso 1 1 d RD . . H12T H 0.2840 0.7056 0.5556 0.143 Uiso 1 1 d RD . . O13S O 0.2412(4) 0.5413(4) 0.9743(4) 0.144(5) Uani 1 1 d D . . H13S H 0.2272 0.5148 0.9889 0.173 Uiso 1 1 d RD . . H13T H 0.2388 0.5823 0.9736 0.173 Uiso 1 1 d RD . . O14S O 0.0363(4) 0.2717(6) 0.7693(4) 0.065(4) Uani 0.501(14) 1 d PD G 1 H14S H 0.0529 0.3008 0.7788 0.078 Uiso 0.501(14) 1 d PRD G 1 H14T H 0.0292 0.2829 0.7453 0.078 Uiso 0.501(14) 1 d PRD G 1 O14' O 0.0191(4) 0.3725(7) 0.7492(4) 0.070(5) Uani 0.499(14) 1 d P . 2 H14' H 0.0458 0.3633 0.7489 0.084 Uiso 0.499(14) 1 d PR G 2 H14" H 0.0198 0.4001 0.7300 0.084 Uiso 0.499(14) 1 d PR G 2 O15S O 0.2359(4) 0.3511(8) 0.9452(5) 0.196(7) Uani 1 1 d D . . H15S H 0.2455 0.3862 0.9353 0.235 Uiso 1 1 d RD . . H15T H 0.2477 0.3613 0.9677 0.235 Uiso 1 1 d RD . . O16S O 0.4865(7) -0.0949(10) 0.2736(6) 0.126(8) Uani 0.50 1 d P . . H16S H 0.4848 -0.0577 0.2846 0.151 Uiso 0.50 1 d PR . . H16T H 0.5097 -0.1147 0.2799 0.151 Uiso 0.50 1 d PR . . O1Z O 0.4940(2) 0.2686(3) 0.6699(2) 0.0143(14) Uani 0.50 1 d PU . . H1Z H 0.4853 0.2300 0.6695 0.017 Uiso 0.50 1 d PR . . C2Z C 0.5063(4) 0.2825(6) 0.7055(4) 0.024(2) Uani 0.50 1 d PU . . H2Z1 H 0.5299 0.3125 0.6982 0.028 Uiso 0.50 1 calc PR . . H2Z2 H 0.5214 0.2414 0.7117 0.028 Uiso 0.50 1 calc PR . . C3Z C 0.5000 0.3058(8) 0.7500 0.078(5) Uani 1 2 d SU . . H3ZA H 0.5279 0.3053 0.7642 0.117 Uiso 0.50 1 d PR . . H3ZB H 0.4798 0.2774 0.7642 0.117 Uiso 0.50 1 d PR . . H3ZC H 0.4886 0.3500 0.7496 0.117 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1A 0.029(3) 0.035(3) 0.055(4) 0.007(3) 0.013(3) 0.006(2) C2A 0.067(6) 0.080(7) 0.068(7) -0.017(5) 0.037(5) -0.015(5) C3A 0.053(5) 0.064(6) 0.044(5) -0.004(4) 0.020(4) -0.003(4) N4A 0.045(4) 0.066(5) 0.053(4) -0.018(4) 0.020(3) -0.012(3) C5A 0.080(7) 0.098(8) 0.066(6) -0.056(6) 0.040(5) -0.051(6) C6A 0.048(5) 0.047(5) 0.042(5) -0.022(4) 0.014(4) -0.020(4) C7A 0.069(5) 0.034(4) 0.034(4) -0.008(3) 0.007(4) -0.003(4) C8A 0.037(4) 0.035(4) 0.050(5) -0.012(3) 0.002(3) 0.005(3) C9A 0.031(4) 0.049(5) 0.071(6) -0.018(4) -0.004(4) 0.003(3) C10A 0.048(4) 0.035(4) 0.046(5) 0.002(3) -0.004(4) -0.004(3) C11A 0.034(4) 0.037(4) 0.037(4) -0.012(3) 0.001(3) -0.005(3) C12A 0.047(5) 0.044(5) 0.064(6) -0.019(4) 0.015(4) -0.017(4) N13A 0.028(3) 0.033(3) 0.045(4) -0.005(3) 0.009(3) -0.006(2) C14A 0.033(4) 0.047(4) 0.051(5) -0.002(4) 0.009(3) -0.012(3) C15A 0.027(6) 0.054(8) 0.031(7) -0.004(5) 0.011(5) -0.012(6) C15' 0.035(11) 0.050(13) 0.034(11) 0.014(9) -0.001(9) -0.015(9) N16A 0.027(3) 0.035(3) 0.038(3) -0.001(2) 0.006(2) -0.001(2) C17A 0.041(7) 0.041(8) 0.029(6) -0.001(5) 0.002(5) -0.008(5) C17' 0.025(9) 0.061(15) 0.045(12) 0.004(10) -0.005(8) -0.006(9) C18A 0.038(4) 0.051(5) 0.034(4) 0.007(3) 0.007(3) -0.002(3) N19A 0.028(3) 0.047(4) 0.039(3) 0.000(3) -0.001(3) -0.005(3) C20A 0.032(4) 0.053(5) 0.041(4) 0.014(4) -0.003(3) -0.001(3) C21A 0.027(3) 0.047(4) 0.039(4) 0.009(3) -0.009(3) 0.001(3) C22A 0.052(5) 0.054(5) 0.043(5) -0.012(4) 0.002(4) -0.023(4) C23A 0.047(5) 0.086(7) 0.058(6) 0.004(5) -0.005(4) -0.032(5) C24A 0.035(4) 0.032(4) 0.059(5) 0.005(3) 0.003(4) 0.003(3) C25A 0.049(5) 0.043(5) 0.057(5) 0.009(4) 0.004(4) 0.020(4) C26A 0.023(3) 0.072(6) 0.046(5) 0.020(4) -0.006(3) 0.004(4) C27A 0.035(5) 0.118(9) 0.059(6) 0.027(6) 0.009(4) 0.017(5) N28A 0.028(3) 0.065(5) 0.051(4) 0.009(3) 0.006(3) 0.004(3) C29A 0.030(4) 0.061(5) 0.058(5) 0.004(4) 0.011(4) 0.002(4) C30A 0.049(5) 0.088(8) 0.074(7) 0.004(6) 0.019(5) -0.005(5) C31A 0.085(7) 0.067(7) 0.091(8) 0.033(6) 0.045(6) 0.021(6) C32A 0.070(7) 0.061(6) 0.126(10) 0.043(6) 0.057(7) 0.033(5) N33A 0.092(7) 0.092(7) 0.177(11) 0.091(8) 0.095(8) 0.063(6) C34A 0.044(5) 0.090(8) 0.100(8) 0.050(7) 0.003(5) -0.020(5) C35A 0.027(4) 0.041(4) 0.076(6) 0.022(4) -0.008(4) -0.004(3) C36A 0.047(5) 0.036(4) 0.077(6) 0.014(4) -0.022(5) -0.020(4) C37A 0.061(5) 0.036(4) 0.053(5) -0.005(4) -0.027(4) 0.003(4) C38A 0.036(4) 0.025(4) 0.055(5) 0.007(3) 0.003(3) 0.002(3) C39A 0.021(3) 0.028(3) 0.041(4) 0.006(3) -0.001(3) -0.002(3) C40A 0.036(4) 0.035(4) 0.040(4) 0.003(3) -0.004(3) 0.008(3) C41A 0.058(5) 0.048(5) 0.042(5) 0.004(4) 0.006(4) 0.020(4) N42A 0.030(3) 0.033(3) 0.034(3) -0.009(2) -0.001(2) 0.003(2) C43A 0.037(4) 0.048(4) 0.036(4) 0.001(3) 0.005(3) 0.009(3) C44A 0.023(6) 0.043(7) 0.042(7) -0.003(5) 0.003(5) -0.002(5) C44' 0.036(11) 0.047(12) 0.050(13) -0.009(10) 0.000(10) -0.005(9) N1B 0.033(3) 0.030(3) 0.059(4) -0.008(3) -0.019(3) 0.003(2) C2B 0.056(5) 0.046(5) 0.098(8) 0.007(5) -0.048(5) 0.000(4) C3B 0.074(6) 0.035(4) 0.069(6) 0.017(4) -0.048(5) -0.012(4) N4B 0.047(4) 0.033(3) 0.072(5) 0.006(3) -0.028(3) -0.004(3) C5B 0.049(5) 0.035(4) 0.054(5) 0.013(4) -0.016(4) -0.002(3) C6B 0.033(4) 0.027(3) 0.041(4) 0.008(3) -0.005(3) -0.006(3) C7B 0.043(4) 0.027(4) 0.038(4) 0.002(3) 0.000(3) -0.001(3) C8B 0.030(3) 0.025(3) 0.041(4) 0.003(3) 0.002(3) 0.003(3) C9B 0.030(4) 0.028(4) 0.048(4) 0.005(3) -0.001(3) 0.004(3) C10B 0.041(4) 0.028(4) 0.034(4) -0.002(3) 0.002(3) -0.001(3) C11B 0.029(3) 0.025(3) 0.033(4) 0.009(3) 0.002(3) -0.004(3) C12B 0.036(4) 0.023(3) 0.037(4) 0.007(3) -0.004(3) -0.005(3) N13B 0.029(3) 0.036(3) 0.039(3) 0.013(3) -0.011(2) -0.012(2) C14B 0.025(3) 0.027(3) 0.040(4) 0.001(3) -0.008(3) -0.003(3) C15B 0.031(5) 0.024(4) 0.040(5) 0.001(4) -0.008(4) -0.004(4) C15" 0.040(18) 0.028(17) 0.014(15) 0.003(12) -0.016(13) 0.015(14) N16B 0.025(3) 0.025(3) 0.031(3) 0.000(2) -0.006(2) -0.001(2) C17B 0.035(5) 0.036(5) 0.027(5) 0.003(4) -0.004(4) -0.003(4) C17" 0.039(19) 0.05(2) 0.04(2) 0.005(16) -0.027(16) 0.000(16) C18B 0.038(4) 0.033(4) 0.029(4) 0.000(3) -0.003(3) -0.002(3) N19B 0.035(3) 0.034(3) 0.028(3) 0.002(2) 0.002(2) -0.008(2) C20B 0.034(4) 0.046(4) 0.031(4) -0.007(3) 0.004(3) -0.002(3) C21B 0.030(3) 0.035(4) 0.034(4) -0.006(3) 0.011(3) -0.002(3) C22B 0.043(4) 0.049(5) 0.048(5) 0.007(4) 0.004(4) -0.010(4) C23B 0.033(4) 0.048(5) 0.059(5) -0.008(4) 0.002(4) -0.014(3) C24B 0.027(3) 0.033(4) 0.045(4) -0.007(3) 0.004(3) -0.005(3) C25B 0.035(4) 0.039(4) 0.045(4) 0.000(3) 0.004(3) 0.008(3) C26B 0.029(4) 0.044(4) 0.043(4) -0.017(3) 0.004(3) 0.006(3) C27B 0.032(4) 0.065(6) 0.059(5) -0.026(4) -0.006(4) 0.014(4) N28B 0.030(3) 0.059(4) 0.055(4) -0.014(3) -0.004(3) 0.004(3) C29B 0.030(4) 0.069(6) 0.071(6) -0.022(5) -0.023(4) 0.011(4) C30B 0.033(4) 0.058(5) 0.062(5) -0.009(4) -0.018(4) -0.003(4) C31B 0.039(4) 0.051(5) 0.066(6) -0.011(4) -0.023(4) -0.002(4) C32B 0.033(4) 0.037(4) 0.068(6) -0.011(4) -0.012(4) 0.000(3) N33B 0.032(3) 0.035(3) 0.052(4) -0.010(3) -0.005(3) -0.001(3) C34B 0.033(4) 0.027(4) 0.072(6) -0.015(4) -0.012(4) 0.000(3) C35B 0.024(3) 0.029(3) 0.043(4) -0.013(3) 0.007(3) 0.002(3) C36B 0.039(4) 0.032(4) 0.038(4) -0.006(3) 0.007(3) -0.013(3) C37B 0.046(4) 0.024(3) 0.030(4) -0.003(3) 0.004(3) -0.009(3) C38B 0.027(3) 0.026(3) 0.053(5) 0.000(3) -0.005(3) -0.002(3) C39B 0.028(3) 0.024(3) 0.049(4) 0.002(3) 0.003(3) -0.007(3) C40B 0.033(3) 0.023(3) 0.036(4) -0.008(3) 0.003(3) 0.002(3) C41B 0.032(4) 0.031(4) 0.038(4) -0.002(3) -0.003(3) -0.001(3) N42B 0.034(3) 0.027(3) 0.032(3) 0.000(2) -0.005(2) 0.001(2) C43B 0.028(3) 0.029(3) 0.034(4) 0.004(3) -0.007(3) 0.003(3) C44B 0.028(4) 0.033(5) 0.035(5) 0.000(4) -0.004(4) 0.002(4) C44" 0.011(14) 0.05(2) 0.06(2) 0.019(18) -0.013(14) -0.004(14) P1 0.0285(9) 0.0351(10) 0.0378(10) -0.0081(8) -0.0060(7) -0.0016(7) O1 0.035(3) 0.038(3) 0.040(3) -0.007(2) -0.005(2) -0.003(2) O2 0.047(3) 0.037(3) 0.035(3) -0.010(2) -0.003(2) -0.001(2) O3 0.037(3) 0.061(4) 0.065(4) -0.029(3) -0.020(3) 0.010(3) O4 0.052(3) 0.044(3) 0.040(3) -0.010(2) 0.000(2) -0.015(2) P2 0.0245(8) 0.0240(8) 0.0295(9) 0.0009(7) -0.0002(7) -0.0007(6) O5 0.028(2) 0.031(2) 0.032(3) 0.0016(19) 0.0043(19) -0.0029(19) O6 0.032(2) 0.028(2) 0.033(3) -0.0048(19) -0.0035(19) -0.0016(19) O7 0.044(3) 0.031(3) 0.033(3) -0.001(2) -0.001(2) 0.005(2) O8 0.030(2) 0.027(2) 0.043(3) 0.001(2) 0.000(2) -0.0020(19) P3 0.0506(13) 0.0507(13) 0.0699(16) 0.0073(11) -0.0273(12) -0.0055(10) O9 0.036(3) 0.039(3) 0.039(3) -0.001(2) -0.006(2) -0.001(2) O10 0.155(8) 0.059(4) 0.048(4) 0.013(3) -0.030(4) -0.046(5) O11 0.067(4) 0.082(5) 0.048(4) -0.006(3) -0.003(3) -0.038(4) O12 0.050(4) 0.086(6) 0.155(8) -0.011(5) -0.023(5) 0.011(4) P4 0.0402(10) 0.0320(10) 0.0423(11) -0.0014(8) 0.0016(8) -0.0094(8) O13 0.039(3) 0.036(3) 0.037(3) -0.006(2) 0.004(2) -0.010(2) O14 0.055(3) 0.035(3) 0.079(4) -0.004(3) 0.006(3) -0.001(3) O15 0.056(3) 0.038(3) 0.045(3) 0.004(2) 0.004(3) -0.003(2) O16 0.048(3) 0.040(3) 0.060(4) -0.001(3) 0.000(3) -0.017(2) Cl1 0.0244(8) 0.0344(9) 0.0370(9) -0.0004(7) 0.0035(6) 0.0015(6) Cl2 0.0239(7) 0.0336(9) 0.0389(9) -0.0047(7) -0.0043(6) 0.0019(6) Cl3 0.0386(11) 0.0473(12) 0.1010(19) 0.0169(12) -0.0055(11) -0.0038(9) Cl4 0.0581(13) 0.0433(11) 0.0683(14) -0.0067(10) 0.0107(10) -0.0170(9) Cl5 0.0461(11) 0.0424(11) 0.0726(15) -0.0003(10) -0.0057(10) 0.0043(9) Cl6 0.0623(14) 0.0628(15) 0.0924(19) -0.0069(13) -0.0199(13) -0.0086(11) Cl7 0.052(2) 0.0289(17) 0.057(2) -0.0015(16) 0.0137(17) 0.0002(15) Cl7' 0.070(12) 0.042(10) 0.049(10) 0.009(7) 0.011(8) 0.020(8) Cl7" 0.067(10) 0.046(9) 0.089(12) -0.011(7) -0.004(8) 0.010(7) Cl7# 0.135(18) 0.16(2) 0.093(14) -0.046(13) -0.045(12) 0.102(17) Cl8 0.091(2) 0.092(2) 0.147(3) 0.010(2) -0.003(2) 0.0155(18) O1S 0.028(2) 0.035(3) 0.037(3) -0.003(2) 0.004(2) -0.0023(19) O2S 0.030(2) 0.038(3) 0.036(3) 0.003(2) -0.007(2) -0.007(2) O3S 0.077(4) 0.017(2) 0.057(4) -0.015(2) 0.004(3) 0.011(2) O4S 0.049(3) 0.053(3) 0.048(3) -0.008(3) 0.004(3) -0.005(3) O5S 0.039(3) 0.061(4) 0.081(5) 0.008(3) 0.007(3) -0.006(3) O6S 0.055(4) 0.056(4) 0.064(4) 0.015(3) -0.001(3) -0.002(3) O7S 0.076(7) 0.075(7) 0.081(7) 0.000 0.021(5) 0.000 O8S 0.066(4) 0.072(5) 0.091(5) 0.006(4) 0.010(4) -0.006(4) O9S 0.087(5) 0.077(5) 0.097(6) 0.002(4) 0.022(4) 0.017(4) O10S 0.093(6) 0.112(7) 0.142(9) -0.018(6) 0.017(6) -0.008(5) O11S 0.080(5) 0.093(6) 0.122(7) 0.004(5) -0.006(5) -0.005(4) O12S 0.108(7) 0.128(8) 0.120(8) -0.039(6) -0.030(6) 0.025(6) O13S 0.204(12) 0.055(5) 0.174(11) 0.014(6) 0.059(9) 0.003(6) O14S 0.051(7) 0.070(9) 0.074(9) 0.016(7) 0.015(6) 0.004(6) O14' 0.060(8) 0.071(9) 0.080(10) -0.007(7) 0.010(8) -0.022(6) O15S 0.147(11) 0.225(16) 0.216(15) 0.105(13) -0.049(10) -0.079(11) O16S 0.140(17) 0.128(16) 0.111(15) -0.041(12) -0.002(12) 0.068(14) O1Z 0.007(2) 0.012(2) 0.025(2) 0.0014(17) 0.0094(17) 0.0006(17) C2Z 0.021(3) 0.022(3) 0.028(2) 0.0026(19) 0.0019(19) -0.0001(19) C3Z 0.132(14) 0.070(9) 0.032(4) 0.000 -0.011(7) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1A C31A 1.432(11) . ? N1A C2A 1.448(11) . ? N1A C30A 1.482(12) . ? C2A C3A 1.494(13) . ? C3A N4A 1.466(10) . ? N4A C5A 1.417(11) . ? C5A C6A 1.525(11) . ? C6A C9A 1.372(13) . ? C6A C7A 1.380(12) . ? C7A C8A 1.376(11) . ? C8A C11A 1.368(11) . ? C9A C10A 1.392(12) . ? C10A C11A 1.376(11) . ? C11A C12A 1.505(10) . ? C12A N13A 1.432(10) . ? N13A C14A 1.484(9) . ? C14A C15A 1.508(5) . ? C14A C15' 1.509(5) . ? C15A N16A 1.481(5) . ? C15' N16A 1.481(6) . ? N16A C44' 1.480(6) . ? N16A C17A 1.482(5) . ? N16A C17' 1.483(6) . ? N16A C44A 1.484(5) . ? C17A C18A 1.511(5) . ? C17' C18A 1.509(5) . ? C18A N19A 1.483(9) . ? N19A C20A 1.490(9) . ? C20A C21A 1.520(10) . ? C21A C22A 1.384(11) . ? C21A C24A 1.386(11) . ? C22A C23A 1.390(12) . ? C23A C26A 1.374(13) . ? C24A C25A 1.392(11) . ? C25A C26A 1.369(12) . ? C26A C27A 1.526(11) . ? C27A N28A 1.425(11) . ? N28A C29A 1.486(9) . ? C29A C30A 1.475(13) . ? C31A C32A 1.448(15) . ? C32A N33A 1.446(11) . ? N33A C34A 1.366(14) . ? C34A C35A 1.544(13) . ? C35A C36A 1.369(13) . ? C35A C38A 1.390(10) . ? C36A C37A 1.371(13) . ? C37A C40A 1.406(11) . ? C38A C39A 1.378(10) . ? C39A C40A 1.380(10) . ? C40A C41A 1.501(11) . ? C41A N42A 1.482(10) . ? N42A C43A 1.490(9) . ? C43A C44A 1.509(5) . ? C43A C44' 1.510(5) . ? N1B C2B 1.436(11) . ? N1B C31B 1.467(11) . ? N1B C30B 1.505(11) . ? C2B C3B 1.526(14) . ? C3B N4B 1.486(10) . ? N4B C5B 1.502(10) . ? C5B C6B 1.510(10) . ? C6B C9B 1.391(10) . ? C6B C7B 1.392(10) . ? C7B C8B 1.370(10) . ? C8B C11B 1.377(10) . ? C9B C10B 1.380(10) . ? C10B C11B 1.382(9) . ? C11B C12B 1.511(9) . ? C12B N13B 1.469(8) . ? N13B C14B 1.478(8) . ? C14B C15B 1.509(5) . ? C14B C15" 1.509(5) . ? C15B N16B 1.484(5) . ? C15" N16B 1.484(5) . ? N16B C17B 1.483(5) . ? N16B C17" 1.485(5) . ? N16B C44" 1.485(5) . ? N16B C44B 1.487(5) . ? C17B C18B 1.513(5) . ? C17" C18B 1.509(5) . ? C18B N19B 1.492(8) . ? N19B C20B 1.504(9) . ? C20B C21B 1.512(10) . ? C21B C24B 1.381(10) . ? C21B C22B 1.396(10) . ? C22B C23B 1.383(11) . ? C23B C26B 1.371(12) . ? C24B C25B 1.389(10) . ? C25B C26B 1.378(11) . ? C26B C27B 1.497(11) . ? C27B N28B 1.508(10) . ? N28B C29B 1.477(10) . ? C29B C30B 1.500(12) . ? C31B C32B 1.487(11) . ? C32B N33B 1.496(9) . ? N33B C34B 1.490(9) . ? C34B C35B 1.497(10) . ? C35B C36B 1.380(10) . ? C35B C38B 1.398(9) . ? C36B C37B 1.379(10) . ? C37B C40B 1.380(9) . ? C38B C39B 1.389(10) . ? C39B C40B 1.377(10) . ? C40B C41B 1.525(9) . ? C41B N42B 1.491(9) . ? N42B C43B 1.490(8) . ? C43B C44B 1.510(5) . ? C43B C44" 1.510(5) . ? P1 O3 1.500(6) . ? P1 O1 1.504(5) . ? P1 O4 1.552(5) . ? P1 O2 1.582(5) . ? P2 O5 1.494(5) . ? P2 O6 1.522(5) . ? P2 O7 1.560(5) . ? P2 O8 1.587(5) . ? P3 O9 1.472(5) . ? P3 O11 1.514(6) . ? P3 O12 1.520(8) . ? P3 O10 1.560(8) . ? P4 O14 1.488(6) . ? P4 O13 1.502(5) . ? P4 O16 1.551(5) . ? P4 O15 1.580(6) . ? O14' O14' 1.18(2) 2_556 ? O16S O16S 1.77(4) 2_655 ? O1Z C2Z 1.262(14) . ? C2Z C3Z 1.554(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31A N1A C2A 112.3(8) . . ? C31A N1A C30A 108.4(8) . . ? C2A N1A C30A 109.4(7) . . ? N1A C2A C3A 117.0(8) . . ? N4A C3A C2A 115.5(7) . . ? C5A N4A C3A 115.8(7) . . ? N4A C5A C6A 116.6(7) . . ? C9A C6A C7A 119.8(7) . . ? C9A C6A C5A 122.3(9) . . ? C7A C6A C5A 117.8(9) . . ? C8A C7A C6A 119.6(8) . . ? C11A C8A C7A 121.6(7) . . ? C6A C9A C10A 119.6(7) . . ? C11A C10A C9A 120.8(7) . . ? C8A C11A C10A 118.5(7) . . ? C8A C11A C12A 119.1(7) . . ? C10A C11A C12A 122.4(7) . . ? N13A C12A C11A 113.1(6) . . ? C12A N13A C14A 115.3(5) . . ? N13A C14A C15A 115.9(6) . . ? N13A C14A C15' 117.3(8) . . ? C15A C14A C15' 38.5(8) . . ? N16A C15A C14A 114.2(6) . . ? N16A C15' C14A 114.1(6) . . ? C44' N16A C15A 138.1(10) . . ? C44' N16A C15' 110.9(9) . . ? C15A N16A C15' 39.3(8) . . ? C44' N16A C17A 68.1(6) . . ? C15A N16A C17A 112.5(6) . . ? C15' N16A C17A 138.3(9) . . ? C44' N16A C17' 109.7(10) . . ? C15A N16A C17' 69.3(7) . . ? C15' N16A C17' 105.4(9) . . ? C17A N16A C17' 45.6(9) . . ? C44' N16A C44A 43.7(8) . . ? C15A N16A C44A 106.6(6) . . ? C15' N16A C44A 70.0(7) . . ? C17A N16A C44A 108.6(6) . . ? C17' N16A C44A 136.4(10) . . ? N16A C17A C18A 113.6(6) . . ? N16A C17' C18A 113.6(6) . . ? N19A C18A C17' 114.0(9) . . ? N19A C18A C17A 114.7(7) . . ? C17' C18A C17A 44.7(8) . . ? C18A N19A C20A 112.8(6) . . ? N19A C20A C21A 112.8(6) . . ? C22A C21A C24A 119.9(7) . . ? C22A C21A C20A 118.6(7) . . ? C24A C21A C20A 121.5(7) . . ? C21A C22A C23A 119.8(8) . . ? C26A C23A C22A 120.1(8) . . ? C21A C24A C25A 119.5(7) . . ? C26A C25A C24A 120.3(8) . . ? C25A C26A C23A 120.3(8) . . ? C25A C26A C27A 119.6(9) . . ? C23A C26A C27A 120.0(9) . . ? N28A C27A C26A 114.9(7) . . ? C27A N28A C29A 115.8(6) . . ? C30A C29A N28A 113.4(7) . . ? C29A C30A N1A 115.4(8) . . ? N1A C31A C32A 120.8(10) . . ? N33A C32A C31A 118.3(10) . . ? C34A N33A C32A 119.1(10) . . ? N33A C34A C35A 116.6(9) . . ? C36A C35A C38A 119.3(8) . . ? C36A C35A C34A 122.5(8) . . ? C38A C35A C34A 118.2(9) . . ? C35A C36A C37A 120.5(7) . . ? C36A C37A C40A 120.8(8) . . ? C39A C38A C35A 120.6(7) . . ? C38A C39A C40A 120.5(6) . . ? C39A C40A C37A 118.3(7) . . ? C39A C40A C41A 121.6(7) . . ? C37A C40A C41A 120.1(7) . . ? N42A C41A C40A 112.8(6) . . ? C41A N42A C43A 113.2(5) . . ? N42A C43A C44A 113.1(7) . . ? N42A C43A C44' 116.3(8) . . ? C44A C43A C44' 42.9(8) . . ? N16A C44A C43A 114.7(6) . . ? N16A C44' C43A 114.8(6) . . ? C2B N1B C31B 111.1(8) . . ? C2B N1B C30B 110.5(7) . . ? C31B N1B C30B 108.6(6) . . ? N1B C2B C3B 114.2(7) . . ? N4B C3B C2B 111.3(8) . . ? C3B N4B C5B 110.6(7) . . ? N4B C5B C6B 112.1(6) . . ? C9B C6B C7B 118.9(6) . . ? C9B C6B C5B 121.6(6) . . ? C7B C6B C5B 119.5(7) . . ? C8B C7B C6B 120.4(7) . . ? C7B C8B C11B 121.0(6) . . ? C10B C9B C6B 119.8(6) . . ? C9B C10B C11B 121.0(7) . . ? C8B C11B C10B 118.9(6) . . ? C8B C11B C12B 119.6(6) . . ? C10B C11B C12B 121.4(6) . . ? N13B C12B C