data_am _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H24 N2 O2' _chemical_formula_weight 492.55 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.011(4) _cell_length_b 18.521(7) _cell_length_c 22.708(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5052(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9684 _exptl_absorpt_correction_T_max 0.9801 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26382 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8837 _reflns_number_gt 6901 _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^)+(0.0605P)^2^+0.4134P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(12) _refine_ls_number_reflns 8837 _refine_ls_number_parameters 689 _refine_ls_number_restraints 516 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.923 _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 C1 C 0.1765(2) 0.35019(14) 0.08990(11) 0.0389(6) Uani 1 1 d U . . C2 C 0.1108(3) 0.31722(15) 0.04791(11) 0.0477(7) Uani 1 1 d U . . H2 H 0.0353 0.3314 0.0434 0.057 Uiso 1 1 calc R . . C3 C 0.1539(3) 0.26425(15) 0.01278(11) 0.0453(7) Uani 1 1 d U . . H3 H 0.1075 0.2414 -0.0155 0.054 Uiso 1 1 calc R . . C4 C 0.2639(3) 0.24347(15) 0.01777(11) 0.0438(7) Uani 1 1 d U . . H4 H 0.2934 0.2070 -0.0072 0.053 Uiso 1 1 calc R . . C5 C 0.3297(2) 0.27610(13) 0.05911(11) 0.0392(6) Uani 1 1 d U . . H5 H 0.4055 0.2620 0.0626 0.047 Uiso 1 1 calc R . . C6 C 0.2882(2) 0.32970(13) 0.09629(10) 0.0319(6) Uani 1 1 d U . . C7 C 0.3601(2) 0.36399(13) 0.13828(10) 0.0317(6) Uani 1 1 d U . . H7 H 0.4353 0.3486 0.1409 0.038 Uiso 1 1 calc R . . C8 C 0.3972(2) 0.44919(13) 0.21268(10) 0.0303(6) Uani 1 1 d U . . C9 C 0.5144(2) 0.44123(15) 0.21235(11) 0.0392(6) Uani 1 1 d U . . H9 H 0.5486 0.4106 0.1840 0.047 Uiso 1 1 calc R . . C10 C 0.5780(2) 0.47663(15) 0.25183(11) 0.0420(7) Uani 1 1 d U . . H10 H 0.6566 0.4713 0.2504 0.050 Uiso 1 1 calc R . . C11 C 0.5301(2) 0.52131(14) 0.29501(10) 0.0364(6) Uani 1 1 d U . . C12 C 0.5962(2) 0.55740(15) 0.33697(11) 0.0439(7) Uani 1 1 d U . . H12 H 0.6748 0.5517 0.3363 0.053 Uiso 1 1 calc R . . C13 C 0.5484(3) 0.60026(16) 0.37835(12) 0.0486(8) Uani 1 1 d U . . H13 H 0.5936 0.6244 0.4065 0.058 Uiso 1 1 calc R . . C14 C 0.4329(2) 0.60892(15) 0.37960(12) 0.0449(7) Uani 1 1 d U . . H14 H 0.4000 0.6391 0.4086 0.054 Uiso 1 1 calc R . . C15 C 0.3670(2) 0.57466(14) 0.33969(11) 0.0398(6) Uani 1 1 d U . . H15 H 0.2886 0.5810 0.3413 0.048 Uiso 1 1 calc R . . C16 C 0.4133(2) 0.52986(13) 0.29596(10) 0.0301(5) Uani 1 1 d U . . C17 C 0.3469(2) 0.49402(13) 0.25314(10) 0.0302(6) Uani 1 1 d U . . C18 C 0.2248(2) 0.50942(13) 0.24814(10) 0.0320(6) Uani 1 1 d U . . C19 C 0.1479(2) 0.47658(14) 0.28386(10) 0.0342(6) Uani 1 1 d U . . C20 C 0.0323(2) 0.49025(15) 0.27623(12) 0.0428(7) Uani 1 1 d U . . H20 H -0.0202 0.4688 0.3022 0.051 Uiso 1 1 calc R . . C21 C -0.0031(2) 0.53335(16) 0.23241(11) 0.0443(7) Uani 1 1 d U . . H21 H -0.0808 0.5404 0.2269 0.053 Uiso 1 1 calc R . . C22 C 0.0720(2) 0.56803(15) 0.19463(11) 0.0420(7) Uani 1 1 d U . . C23 C 0.0373(3) 0.61385(17) 0.14896(12) 0.0530(8) Uani 1 1 d U . . H23 H -0.0400 0.6216 0.1426 0.064 Uiso 1 1 calc R . . C24 C 0.1122(3) 0.64702(19) 0.11399(14) 0.0649(9) Uani 1 1 d U . . H24 H 0.0868 0.6772 0.0829 0.078 Uiso 1 1 calc R . . C25 C 0.2261(3) 0.63784(17) 0.12257(13) 0.0557(8) Uani 1 1 d U . . H25 H 0.2777 0.6626 0.0981 0.067 Uiso 1 1 calc R . . C26 C 0.2634(2) 0.59325(15) 0.16615(11) 0.0436(7) Uani 1 1 d U . . H26 H 0.3412 0.5868 0.1715 0.052 Uiso 1 1 calc R . . C27 C 0.1888(2) 0.55692(14) 0.20306(10) 0.0359(6) Uani 1 1 d U . . C28 C 0.1305(3) 0.3794(2) 0.34803(15) 0.0725(11) Uani 1 1 d U . . H28 H 0.0593 0.3709 0.3311 0.087 Uiso 1 1 calc R . . C29 C 0.1674(3) 0.33279(17) 0.39461(13) 0.0561(8) Uani 1 1 d U . . C30 C 0.2675(3) 0.34129(18) 0.42081(13) 0.0556(8) Uani 1 1 d U . . C31 C 0.3014(3) 0.2940(2) 0.46410(15) 0.0770(11) Uani 1 1 d U . . H31 H 0.3732 0.3001 0.4809 0.092 Uiso 1 1 calc R . . C32 C 0.2379(3) 0.24044(17) 0.48318(13) 0.0526(8) Uani 1 1 d U . . H32 H 0.2618 0.2100 0.5144 0.063 Uiso 1 1 calc R . . C33 C 0.1394(4) 0.2305(3) 0.4573(2) 0.145(3) Uani 1 1 d U . . H33 H 0.0922 0.1923 0.4698 0.174 Uiso 1 1 calc R . . C34 C 0.1060(4) 0.2753(3) 0.4127(2) 0.165(3) Uani 1 1 d U . . H34 H 0.0372 0.2658 0.3936 0.198 Uiso 1 1 calc R . . C35 C 0.7064(3) 0.63926(16) 0.17980(11) 0.0483(7) Uani 1 1 d U . . C36 C 0.7527(3) 0.68168(19) 0.22334(14) 0.0662(10) Uani 1 1 d U . . H36 H 0.8222 0.6684 0.2401 0.079 Uiso 1 1 calc R . . C37 C 0.6998(3) 0.7427(2) 0.24266(13) 0.0694(10) Uani 1 1 d U . . H37 H 0.7321 0.7713 0.2729 0.083 Uiso 1 1 calc R . . C38 C 0.5995(3) 0.7622(2) 0.21806(15) 0.0746(11) Uani 1 1 d U . . H38 H 0.5623 0.8046 0.2312 0.090 Uiso 1 1 calc R . . C39 C 0.5539(3) 0.72072(19) 0.17489(14) 0.0678(10) Uani 1 1 d U . . H39 H 0.4844 0.7345 0.1584 0.081 Uiso 1 1 calc R . . C40 C 0.6058(2) 0.65932(16) 0.15459(11) 0.0446(7) Uani 1 1 d U . . C41 C 0.5555(2) 0.61678(16) 0.10817(12) 0.0442(7) Uani 1 1 d U . . H41 H 0.4861 0.6317 0.0922 0.053 Uiso 1 1 calc R . . C42 C 0.5484(2) 0.51652(14) 0.04539(10) 0.0358(6) Uani 1 1 d U . . C43 C 0.4313(2) 0.50414(17) 0.04773(12) 0.0460(7) Uani 1 1 d U . . H43 H 0.3879 0.5262 0.0777 0.055 Uiso 1 1 calc R . . C44 C 0.3823(2) 0.46137(17) 0.00759(12) 0.0508(8) Uani 1 1 d U . . H44 H 0.3038 0.4552 0.0085 0.061 Uiso 1 1 calc R . . C45 C 0.4453(2) 0.42539(16) -0.03588(12) 0.0444(7) Uani 1 1 d U . . C46 C 0.3967(3) 0.37773(17) -0.07664(13) 0.0557(9) Uani 1 1 d U . . H46 H 0.3190 0.3685 -0.0746 0.067 Uiso 1 1 calc R . . C47 C 0.4578(3) 0.34484(18) -0.11861(14) 0.0629(10) Uani 1 1 d U . . H47 H 0.4231 0.3131 -0.1459 0.075 Uiso 1 1 calc R . . C48 C 0.5726(3) 0.35756(16) -0.12191(12) 0.0533(8) Uani 1 1 d U . . H48 H 0.6156 0.3345 -0.1516 0.064 Uiso 1 1 calc R . . C49 C 0.6230(2) 0.40256(14) -0.08306(11) 0.0411(7) Uani 1 1 d U . . H49 H 0.7009 0.4106 -0.0859 0.049 Uiso 1 1 calc R . . C50 C 0.5616(2) 0.43758(14) -0.03861(10) 0.0368(6) Uani 1 1 d U . . C51 C 0.6123(2) 0.48472(14) 0.00310(10) 0.0324(6) Uani 1 1 d U . . C52 C 0.7308(2) 0.50559(14) -0.00438(9) 0.0311(6) Uani 1 1 d U . . C53 C 0.7572(2) 0.55651(14) -0.04930(10) 0.0369(6) Uani 1 1 d U . . C54 C 0.6747(3) 0.58677(15) -0.08566(11) 0.0454(7) Uani 1 1 d U . . H54 H 0.5987 0.5748 -0.0792 0.054 Uiso 1 1 calc R . . C55 C 0.7025(3) 0.63324(17) -0.13021(12) 0.0555(9) Uani 1 1 d U . . H55 H 0.6461 0.6530 -0.1547 0.067 Uiso 1 1 calc R . . C56 C 0.8136(3) 0.65157(17) -0.13970(13) 0.0595(9) Uani 1 1 d U . . H56 H 0.8324 0.6835 -0.1709 0.071 Uiso 1 1 calc R . . C57 C 0.8952(3) 0.62430(16) -0.10479(12) 0.0500(8) Uani 1 1 d U . . H57 H 0.9704 0.6378 -0.1116 0.060 Uiso 1 1 calc R . . C58 C 0.8700(2) 0.57658(14) -0.05890(11) 0.0396(6) Uani 1 1 d U . . C59 C 0.9527(2) 0.54689(15) -0.02204(12) 0.0424(7) Uani 1 1 d U . . H59 H 1.0284 0.5600 -0.0279 0.051 Uiso 1 1 calc R . . C60 C 0.9263(2) 0.50037(15) 0.02126(12) 0.0396(6) Uani 1 1 d U . . H60 H 0.9835 0.4818 0.0459 0.048 Uiso 1 1 calc R . . C61 C 0.8151(2) 0.47859(14) 0.03075(10) 0.0318(6) Uani 1 1 d U . . C62 C 0.8500(2) 0.41035(14) 0.11590(11) 0.0390(6) Uani 1 1 d U . . H62 H 0.9171 0.4366 0.1212 0.047 Uiso 1 1 calc R . . C63 C 0.8225(2) 0.35311(14) 0.15620(10) 0.0401(6) Uani 1 1 d U . . C64 C 0.9012(3) 0.33283(17) 0.19905(12) 0.0592(9) Uani 1 1 d U . . H64 H 0.9703 0.3576 0.2014 0.071 Uiso 1 1 calc R . . C65 C 0.8786(4) 0.27764(19) 0.23731(13) 0.0718(11) Uani 1 1 d U . . H65 H 0.9321 0.2637 0.2659 0.086 Uiso 1 1 calc R . . C66 C 0.7784(4) 0.24271(19) 0.23404(14) 0.0737(12) Uani 1 1 d U . . H66 H 0.7631 0.2048 0.2610 0.088 Uiso 1 1 calc R . . C67 C 0.6988(3) 0.26094(16) 0.19265(13) 0.0602(9) Uani 1 1 d U . . H67 H 0.6294 0.2363 0.1913 0.072 Uiso 1 1 calc R . . C68 C 0.7225(3) 0.31636(15) 0.15277(11) 0.0448(7) Uani 1 1 d U . . N1 N 0.32666(17) 0.41431(11) 0.17213(8) 0.0319(5) Uani 1 1 d U . . N2 N 0.18731(17) 0.43062(11) 0.32864(8) 0.0340(5) Uani 1 1 d U . . N3 N 0.60163(18) 0.55998(12) 0.08820(9) 0.0395(5) Uani 1 1 d U . . N4 N 0.78507(17) 0.42637(11) 0.07296(8) 0.0337(5) Uani 1 1 d U . . O1 O 0.13188(16) 0.40301(11) 0.12305(9) 0.0586(6) Uani 1 1 d U . . H1 H 0.1804 0.4193 0.1461 0.088 Uiso 1 1 calc R . . O2 O 0.3323(3) 0.3956(2) 0.40416(17) 0.1547(18) Uani 1 1 d U . . H2A H 0.3019 0.4179 0.3763 0.232 Uiso 1 1 calc R . . O3 O 0.76128(17) 0.58031(12) 0.16200(10) 0.0659(7) Uani 1 1 d U . . H3A H 0.7275 0.5615 0.1335 0.099 Uiso 1 1 calc R . . O4 O 0.64450(16) 0.33343(10) 0.11173(8) 0.0446(5) Uani 1 1 d U . . H4A H 0.6669 0.3686 0.0916 0.067 Uiso 1 1 calc 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 C1 0.0408(16) 0.0382(15) 0.0376(14) -0.0073(12) -0.0038(12) 0.0012(13) C2 0.0486(18) 0.0476(17) 0.0468(16) -0.0118(14) -0.0159(14) 0.0069(14) C3 0.059(2) 0.0398(16) 0.0368(15) -0.0041(13) -0.0106(14) -0.0033(14) C4 0.060(2) 0.0356(15) 0.0361(15) -0.0078(13) 0.0020(14) -0.0029(14) C5 0.0446(17) 0.0345(15) 0.0386(14) -0.0046(12) 0.0074(13) 0.0029(12) C6 0.0360(15) 0.0292(13) 0.0306(13) 0.0006(11) 0.0021(11) -0.0015(11) C7 0.0283(14) 0.0376(15) 0.0293(12) -0.0014(12) 0.0028(11) 0.0032(11) C8 0.0276(14) 0.0353(14) 0.0280(12) -0.0029(11) -0.0008(10) -0.0006(11) C9 0.0331(15) 0.0477(17) 0.0366(14) -0.0082(12) 0.0033(12) 0.0006(12) C10 0.0267(15) 0.0564(18) 0.0428(15) -0.0095(14) -0.0002(12) -0.0004(13) C11 0.0307(15) 0.0404(15) 0.0382(14) 0.0016(12) -0.0037(11) -0.0029(12) C12 0.0381(16) 0.0496(17) 0.0438(15) -0.0066(14) -0.0079(13) -0.0033(13) C13 0.0514(19) 0.0507(18) 0.0437(16) -0.0102(14) -0.0192(14) -0.0071(15) C14 0.0487(19) 0.0448(17) 0.0413(16) -0.0113(13) -0.0082(13) 0.0052(14) C15 0.0389(16) 0.0432(16) 0.0374(14) -0.0069(12) -0.0045(12) 0.0033(12) C16 0.0300(14) 0.0300(13) 0.0303(13) 0.0007(11) -0.0018(11) -0.0020(11) C17 0.0292(14) 0.0362(14) 0.0252(12) 0.0021(11) 0.0007(10) -0.0039(11) C18 0.0347(15) 0.0353(14) 0.0261(12) -0.0092(11) -0.0011(11) -0.0003(11) C19 0.0321(15) 0.0403(15) 0.0302(13) -0.0080(12) -0.0034(11) 0.0024(12) C20 0.0315(16) 0.0526(18) 0.0443(15) -0.0065(14) 0.0001(12) -0.0012(13) C21 0.0291(15) 0.0605(19) 0.0432(16) -0.0114(14) -0.0071(13) 0.0053(13) C22 0.0397(16) 0.0503(17) 0.0360(14) -0.0128(13) -0.0069(12) 0.0107(13) C23 0.0439(18) 0.069(2) 0.0466(17) -0.0006(16) -0.0146(15) 0.0167(16) C24 0.070(2) 0.074(2) 0.0515(18) 0.0136(18) -0.0100(18) 0.0204(19) C25 0.055(2) 0.065(2) 0.0466(17) 0.0139(16) -0.0037(15) 0.0059(16) C26 0.0443(17) 0.0500(17) 0.0364(14) -0.0010(13) -0.0016(13) 0.0092(13) C27 0.0376(15) 0.0407(15) 0.0293(13) -0.0081(11) -0.0057(11) 0.0051(12) C28 0.046(2) 0.090(3) 0.081(2) 0.035(2) -0.0275(18) -0.0275(19) C29 0.0427(18) 0.067(2) 0.0583(18) 0.0183(17) -0.0147(15) -0.0188(16) C30 0.0491(19) 0.061(2) 0.0566(18) 0.0160(16) -0.0131(15) -0.0177(16) C31 0.053(2) 0.097(3) 0.080(2) 0.039(2) -0.0337(19) -0.024(2) C32 0.058(2) 0.0507(19) 0.0494(17) 0.0076(15) -0.0116(16) -0.0101(16) C33 0.110(4) 0.170(5) 0.157(4) 0.123(4) -0.079(3) -0.092(4) C34 0.111(4) 0.190(5) 0.194(5) 0.144(5) -0.096(4) -0.104(4) C35 0.0549(19) 0.0535(18) 0.0365(15) -0.0076(14) 0.0004(14) 0.0152(15) C36 0.061(2) 0.084(3) 0.0540(19) -0.0267(18) -0.0099(16) 0.0223(19) C37 0.086(3) 0.079(3) 0.0434(17) -0.0240(18) -0.0055(18) 0.018(2) C38 0.092(3) 0.069(2) 0.063(2) -0.0206(19) -0.002(2) 0.037(2) C39 0.074(2) 0.070(2) 0.060(2) -0.0073(18) -0.0076(18) 0.0351(19) C40 0.0481(18) 0.0559(18) 0.0297(13) 0.0029(13) 0.0030(13) 0.0193(14) C41 0.0367(16) 0.0556(18) 0.0403(15) 0.0106(14) -0.0028(13) 0.0107(14) C42 0.0312(15) 0.0463(16) 0.0299(13) 0.0084(12) -0.0026(11) -0.0026(12) C43 0.0294(16) 0.069(2) 0.0401(15) 0.0138(15) 0.0044(12) 0.0003(14) C44 0.0297(16) 0.072(2) 0.0502(17) 0.0293(16) -0.0072(14) -0.0090(15) C45 0.0376(16) 0.0545(18) 0.0412(15) 0.0228(14) -0.0106(13) -0.0164(14) C46 0.052(2) 0.065(2) 0.0507(18) 0.0207(16) -0.0212(16) -0.0260(16) C47 0.080(3) 0.060(2) 0.0487(19) 0.0102(17) -0.0263(18) -0.0322(19) C48 0.074(2) 0.0473(18) 0.0388(16) -0.0015(14) -0.0110(15) -0.0154(16) C49 0.0495(18) 0.0417(16) 0.0319(13) 0.0057(12) -0.0034(13) -0.0109(13) C50 0.0395(16) 0.0416(15) 0.0294(13) 0.0139(12) -0.0079(11) -0.0118(13) C51 0.0294(14) 0.0400(15) 0.0277(13) 0.0080(11) -0.0016(11) -0.0058(12) C52 0.0306(14) 0.0384(15) 0.0244(12) -0.0034(11) 0.0009(10) -0.0066(12) C53 0.0406(16) 0.0428(15) 0.0271(13) -0.0045(11) 0.0009(11) -0.0121(13) C54 0.0483(18) 0.0526(18) 0.0353(14) 0.0085(13) -0.0070(13) -0.0201(14) C55 0.066(2) 0.061(2) 0.0390(15) 0.0153(15) -0.0176(15) -0.0284(17) C56 0.077(2) 0.058(2) 0.0432(16) 0.0120(15) -0.0011(17) -0.0346(18) C57 0.054(2) 0.0564(19) 0.0402(16) -0.0014(14) 0.0117(15) -0.0249(15) C58 0.0378(16) 0.0466(16) 0.0343(13) -0.0072(12) 0.0068(12) -0.0153(13) C59 0.0297(15) 0.0476(17) 0.0499(17) -0.0111(14) 0.0107(13) -0.0138(13) C60 0.0307(15) 0.0435(16) 0.0447(15) -0.0085(13) 0.0011(12) 0.0005(12) C61 0.0306(14) 0.0358(14) 0.0291(12) -0.0068(11) 0.0023(11) -0.0051(11) C62 0.0382(16) 0.0409(15) 0.0380(14) -0.0107(13) -0.0015(12) 0.0030(12) C63 0.0573(19) 0.0367(15) 0.0264(13) -0.0043(12) -0.0007(13) 0.0069(14) C64 0.085(2) 0.059(2) 0.0334(15) -0.0100(15) -0.0104(16) 0.0233(18) C65 0.123(4) 0.060(2) 0.0322(16) 0.0027(16) -0.004(2) 0.028(2) C66 0.136(4) 0.052(2) 0.0332(17) 0.0110(16) 0.023(2) 0.027(2) C67 0.091(3) 0.0420(18) 0.0475(17) -0.0019(15) 0.0250(18) 0.0071(17) C68 0.068(2) 0.0409(16) 0.0252(13) -0.0072(12) 0.0136(14) 0.0116(15) N1 0.0336(12) 0.0349(12) 0.0273(10) -0.0038(9) -0.0013(9) -0.0021(9) N2 0.0307(12) 0.0388(12) 0.0326(11) -0.0020(10) 0.0017(9) -0.0022(10) N3 0.0334(12) 0.0525(14) 0.0327(11) 0.0024(10) 0.0035(10) 0.0030(11) N4 0.0349(12) 0.0401(12) 0.0261(10) -0.0026(9) 0.0000(9) 0.0028(10) O1 0.0427(12) 0.0628(14) 0.0704(14) -0.0392(11) -0.0185(10) 0.0144(10) O2 0.091(2) 0.170(3) 0.203(4) 0.135(3) -0.096(2) -0.086(2) O3 0.0505(13) 0.0758(16) 0.0713(15) -0.0373(13) -0.0200(11) 0.0309(12) O4 0.0494(12) 0.0444(12) 0.0402(10) -0.0047(9) 0.0117(9) -0.0037(9) _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 C1 O1 1.346(3) . ? C1 C2 1.380(4) . ? C1 C6 1.401(4) . ? C2 C3 1.366(4) . ? C3 C4 1.380(4) . ? C4 C5 1.369(4) . ? C5 C6 1.395(3) . ? C6 C7 1.435(3) . ? C7 N1 1.273(3) . ? C8 C17 1.378(3) . ? C8 N1 1.408(3) . ? C8 C9 1.415(3) . ? C9 C10 1.348(3) . ? C10 C11 1.406(4) . ? C11 C12 1.409(3) . ? C11 C16 1.412(3) . ? C12 C13 1.357(4) . ? C13 C14 1.397(4) . ? C14 C15 1.361(4) . ? C15 C16 1.409(3) . ? C16 C17 1.423(3) . ? C17 C18 1.499(4) . ? C18 C19 1.371(3) . ? C18 C27 1.417(3) . ? C19 N2 1.408(3) . ? C19 C20 1.423(4) . ? C20 C21 1.345(4) . ? C21 C22 1.401(4) . ? C22 C23 1.404(4) . ? C22 C27 1.430(4) . ? C23 C24 1.348(4) . ? C24 C25 1.393(4) . ? C25 C26 1.365(4) . ? C26 C27 1.400(4) . ? C28 N2 1.249(4) . ? C28 C29 1.436(4) . ? C29 C30 1.351(4) . ? C29 C34 1.358(5) . ? C30 O2 1.326(4) . ? C30 C31 1.378(4) . ? C31 C32 1.324(4) . ? C32 C33 1.335(5) . ? C33 C34 1.369(5) . ? C35 O3 1.338(3) . ? C35 C36 1.380(4) . ? C35 C40 1.387(4) . ? C36 C37 1.368(4) . ? C37 C38 1.377(5) . ? C38 C39 1.361(5) . ? C39 C40 1.377(4) . ? C40 C41 1.448(4) . ? C41 N3 1.273(3) . ? C42 C51 1.363(3) . ? C42 N3 1.415(3) . ? C42 C43 1.425(4) . ? C43 C44 1.343(4) . ? C44 C45 1.411(4) . ? C45 C46 1.406(4) . ? C45 C50 1.416(4) . ? C46 C47 1.349(5) . ? C47 C48 1.401(5) . ? C48 C49 1.356(4) . ? C49 C50 1.408(4) . ? C50 C51 1.425(3) . ? C51 C52 1.485(3) . ? C52 C61 1.382(3) . ? C52 C53 1.425(3) . ? C53 C54 1.406(4) . ? C53 C58 1.422(3) . ? C54 C55 1.370(4) . ? C55 C56 1.393(4) . ? C56 C57 1.358(4) . ? C57 C58 1.399(4) . ? C58 C59 1.411(4) . ? C59 C60 1.345(4) . ? C60 C61 1.411(4) . ? C61 N4 1.409(3) . ? C62 N4 1.283(3) . ? C62 C63 1.439(4) . ? C63 C68 1.383(4) . ? C63 C64 1.408(4) . ? C64 C65 1.369(5) . ? C65 C66 1.368(5) . ? C66 C67 1.383(5) . ? C67 C68 1.398(4) . ? C68 O4 1.358(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 O1 C1 C2 118.7(3) . . ? O1 C1 C6 121.4(2) . . ? C2 C1 C6 119.9(2) . . ? C3 C2 C1 120.3(3) . . ? C2 C3 C4 121.0(3) . . ? C5 C4 C3 119.1(3) . . ? C4 C5 C6 121.5(3) . . ? C5 C6 C1 118.2(2) . . ? C5 C6 C7 120.1(2) . . ? C1 C6 C7 121.7(2) . . ? N1 C7 C6 122.4(2) . . ? C17 C8 N1 116.7(2) . . ? C17 C8 C9 120.2(2) . . ? N1 C8 C9 123.2(2) . . ? C10 C9 C8 120.6(2) . . ? C9 C10 C11 121.2(3) . . ? C10 C11 C12 121.4(2) . . ? C10 C11 C16 118.9(2) . . ? C12 C11 C16 119.7(2) . . ? C13 C12 C11 120.5(3) . . ? C12 C13 C14 120.1(3) . . ? C15 C14 C13 120.7(3) . . ? C14 C15 C16 120.9(3) . . ? C15 C16 C11 118.0(2) . . ? C15 C16 C17 122.3(2) . . ? C11 C16 C17 119.7(2) . . ? C8 C17 C16 119.4(2) . . ? C8 C17 C18 119.6(2) . . ? C16 C17 C18 120.8(2) . . ? C19 C18 C27 119.8(2) . . ? C19 C18 C17 122.0(2) . . ? C27 C18 C17 118.1(2) . . ? C18 C19 N2 118.0(2) . . ? C18 C19 C20 120.4(2) . . ? N2 C19 C20 121.6(2) . . ? C21 C20 C19 120.3(3) . . ? C20 C21 C22 121.5(3) . . ? C21 C22 C23 122.5(3) . . ? C21 C22 C27 118.9(2) . . ? C23 C22 C27 118.5(3) . . ? C24 C23 C22 120.8(3) . . ? C23 C24 C25 121.2(3) . . ? C26 C25 C24 119.9(3) . . ? C25 C26 C27 121.0(3) . . ? C26 C27 C18 122.4(2) . . ? C26 C27 C22 118.6(2) . . ? C18 C27 C22 119.0(2) . . ? N2 C28 C29 123.2(3) . . ? C30 C29 C34 116.2(3) . . ? C30 C29 C28 121.9(3) . . ? C34 C29 C28 121.8(3) . . ? O2 C30 C29 119.0(3) . . ? O2 C30 C31 120.8(3) . . ? C29 C30 C31 120.2(3) . . ? C32 C31 C30 122.6(3) . . ? C31 C32 C33 118.0(3) . . ? C32 C33 C34 120.2(4) . . ? C29 C34 C33 122.6(4) . . ? O3 C35 C36 118.9(3) . . ? O3 C35 C40 121.5(2) . . ? C36 C35 C40 119.6(3) . . ? C37 C36 C35 120.9(3) . . ? C36 C37 C38 119.6(3) . . ? C39 C38 C37 119.7(3) . . ? C38 C39 C40 121.7(3) . . ? C39 C40 C35 118.5(3) . . ? C39 C40 C41 120.2(3) . . ? C35 C40 C41 121.2(2) . . ? N3 C41 C40 121.8(2) . . ? C51 C42 N3 118.4(2) . . ? C51 C42 C43 120.8(2) . . ? N3 C42 C43 120.8(2) . . ? C44 C43 C42 120.1(3) . . ? C43 C44 C45 121.2(3) . . ? C46 C45 C44 122.3(3) . . ? C46 C45 C50 118.7(3) . . ? C44 C45 C50 119.0(3) . . ? C47 C46 C45 121.5(3) . . ? C46 C47 C48 119.8(3) . . ? C49 C48 C47 120.5(3) . . ? C48 C49 C50 121.1(3) . . ? C49 C50 C45 118.3(2) . . ? C49 C50 C51 122.3(2) . . ? C45 C50 C51 119.4(3) . . ? C42 C51 C50 119.5(2) . . ? C42 C51 C52 120.5(2) . . ? C50 C51 C52 119.6(2) . . ? C61 C52 C53 119.3(2) . . ? C61 C52 C51 122.8(2) . . ? C53 C52 C51 117.8(2) . . ? C54 C53 C58 118.5(2) . . ? C54 C53 C52 121.9(2) . . ? C58 C53 C52 119.6(2) . . ? C55 C54 C53 120.8(3) . . ? C54 C55 C56 120.1(3) . . ? C57 C56 C55 120.6(3) . . ? C56 C57 C58 120.9(3) . . ? C57 C58 C59 122.4(3) . . ? C57 C58 C53 119.0(3) . . ? C59 C58 C53 118.6(2) . . ? C60 C59 C58 121.1(2) . . ? C59 C60 C61 121.2(3) . . ? C52 C61 N4 117.0(2) . . ? C52 C61 C60 120.1(2) . . ? N4 C61 C60 122.9(2) . . ? N4 C62 C63 121.0(3) . . ? C68 C63 C64 119.4(3) . . ? C68 C63 C62 121.7(2) . . ? C64 C63 C62 118.8(3) . . ? C65 C64 C63 120.3(4) . . ? C66 C65 C64 119.5(3) . . ? C65 C66 C67 122.0(3) . . ? C66 C67 C68 118.6(4) . . ? O4 C68 C63 121.5(2) . . ? O4 C68 C67 118.4(3) . . ? C63 C68 C67 120.1(3) . . ? C7 N1 C8 122.8(2) . . ? C28 N2 C19 122.0(2) . . ? C41 N3 C42 121.2(2) . . ? C62 N4 C61 121.4(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.226 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.033