data_Compound12 _audit_creation_method SHELXL-97 # 1. submission details _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; _publ_contact_author_phone ' 212-854-2074 ' _publ_contact_author_fax ' 212-854-2310 ' _publ_contact_author_email ' ldoerrer@barnard.edu ' _publ_requested_journal 'Inorganic Chemistry' _publ_requested_coeditor_name ' Prof James Mayer ' #============================================================================== # 3. title and author list _publ_section_title ; homoleptic cobalt and copper phenolate A2[M(OAr)4] Compounds the effect of phenoxide fluorination ; # the loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'buzzeo, marisa c.' #<--'Last name, first name' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'iqbal, amber h.' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'long, charli m.' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'millar, david' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'patel, sonal' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'pellow, matthew a.' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'saddoughi, sahar a.' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'smenton, abigail l.' ; barnard college, chemistry department 3009 broadway new york, ny, 10027 ; 'turner, john f. c.' ; department of chemistry 408 buehler hall university of tennessee knoxville, tn 37996 ; 'wadhawan, jay d.' ; physical and theoretical chemistry Laboratory university of oxford oxford ox1 3qz, uk ; 'compton, richard g.' ; physical and theoretical chemistry Laboratory university of oxford oxford ox1 3qz, uk ; 'golen, james a.' ; department of chemistry and biochemistry mc 0358 university of california, san diego 9500 gilman drive la jolla, ca 92093 ; ; permanent address is the department of Chemistry & Biochemistry, University of massachusetts dartmouth, north dartmouth MA 02747 ; 'rheingold, arnold l.' ; department of chemistry and biochemistry mc 0358 university of california, san diego 9500 gilman drive la jolla, ca 92093 ; #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'c60 h40 cl2 co f10 o2 p2' _chemical_formula_weight 1174.69 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' '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' 'p' 'p' 0.1023 0.0942 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'co' 'co' 0.3494 0.9721 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.7866(13) _cell_length_b 14.2273(10) _cell_length_c 18.6950(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.7510(10) _cell_angle_gamma 90.00 _cell_volume 5236.3(6) _cell_formula_units_z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 2388 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_t_min 0.921 _exptl_absorpt_correction_t_max 1.000 _exptl_absorpt_process_details SADABS _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 '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 33218 _diffrn_reflns_av_r_equivalents 0.0379 _diffrn_reflns_av_sigmai/neti 0.0559 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 28.30 _reflns_number_total 12328 _reflns_number_gt 8797 _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^)+(0.0796p)^2^+2.4353P] 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 12328 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_r_factor_all 0.0795 _refine_ls_r_factor_gt 0.0527 _refine_ls_wr_factor_ref 0.1527 _refine_ls_wr_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_s_all 1.033 _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 co1 co 0.22444(2) 0.05762(3) 0.37274(2) 0.02858(11) Uani 1 1 d . . . cl1 cl 0.30632(3) 0.09374(5) 0.29981(4) 0.02966(16) Uani 1 1 d . . . cl2 cl 0.13446(3) -0.01720(6) 0.31113(4) 0.03466(18) Uani 1 1 d . . . p1 p -0.02954(4) -0.28359(5) 0.45810(4) 0.02584(16) Uani 1 1 d . . . p2 p 0.42071(4) 0.59599(5) 0.20260(4) 0.02567(16) Uani 1 1 d . . . o1 o 0.20580(12) 0.17716(15) 0.41930(11) 0.0388(5) Uani 1 1 d . . . o2 o 0.25640(12) -0.01718(16) 0.45811(11) 0.0383(5) Uani 1 1 d . . . f1 f 0.15325(10) 0.23014(15) 0.28276(10) 0.0490(5) Uani 1 1 d . . . f2 f 0.18730(11) 0.39665(16) 0.22702(10) 0.0528(5) Uani 1 1 d . . . f3 f 0.27734(10) 0.51338(13) 0.30367(11) 0.0471(5) Uani 1 1 d . . . f4 f 0.33112(11) 0.46044(15) 0.43642(11) 0.0534(5) Uani 1 1 d . . . f5 f 0.29501(10) 0.29820(14) 0.49503(9) 0.0454(5) Uani 1 1 d . . . f6 f 0.18667(11) -0.15526(14) 0.52314(11) 0.0489(5) Uani 1 1 d . . . f7 f 0.23942(13) -0.32703(14) 0.54317(12) 0.0620(6) Uani 1 1 d . . . f8 f 0.36301(13) -0.37113(15) 0.49833(13) 0.0654(6) Uani 1 1 d . . . f9 f 0.43039(11) -0.23628(16) 0.42856(12) 0.0562(6) Uani 1 1 d . . . f10 f 0.37985(10) -0.06440(14) 0.40959(11) 0.0477(5) Uani 1 1 d . . . c1 c 0.22229(15) 0.2571(2) 0.39119(15) 0.0298(6) Uani 1 1 d . . . c2 c 0.19604(16) 0.2875(2) 0.32250(16) 0.0339(7) Uani 1 1 d . . . c3 c 0.21406(16) 0.3715(2) 0.29351(15) 0.0353(7) Uani 1 1 d . . . c4 c 0.25940(16) 0.4302(2) 0.33148(17) 0.0344(7) Uani 1 1 d . . . c5 c 0.28623(16) 0.4033(2) 0.39847(16) 0.0345(7) Uani 1 1 d . . . c6 c 0.26740(16) 0.3195(2) 0.42774(15) 0.0314(6) Uani 1 1 d . . . c7 c 0.28008(16) -0.1009(2) 0.46423(16) 0.0334(7) Uani 1 1 d . . . c8 c 0.24761(17) -0.1732(2) 0.49845(17) 0.0381(7) Uani 1 1 d . . . c9 c 0.2744(2) -0.2625(2) 0.50980(18) 0.0429(8) Uani 1 1 d . . . c10 c 0.3356(2) -0.2844(2) 0.4872(2) 0.0461(9) Uani 1 1 d . . . c11 c 0.37054(18) -0.2171(2) 0.45250(17) 0.0414(8) Uani 1 1 d . . . c12 c 0.34309(17) -0.1285(2) 0.44215(16) 0.0363(7) Uani 1 1 d . . . c13 c -0.05183(14) -0.1651(2) 0.43337(14) 0.0274(6) Uani 1 1 d . . . c14 c -0.11289(15) -0.1298(2) 0.45275(15) 0.0312(6) Uani 1 1 d . . . h14a h -0.1432 -0.1697 0.4748 0.037 Uiso 1 1 calc R . . c15 c -0.12940(16) -0.0365(2) 0.43987(17) 0.0357(7) Uani 1 1 d . . . h15a h -0.1711 -0.0122 0.4531 0.043 Uiso 1 1 calc R . . c16 c -0.08492(17) 0.0214(2) 0.40753(17) 0.0382(7) Uani 1 1 d . . . h16a h -0.0962 0.0856 0.3991 0.046 Uiso 1 1 calc R . . c17 c -0.02462(17) -0.0133(2) 0.38745(17) 0.0365(7) Uani 1 1 d . . . h17a h 0.0052 0.0267 0.3647 0.044 Uiso 1 1 calc R . . c18 c -0.00738(15) -0.1066(2) 0.40037(15) 0.0313(6) Uani 1 1 d . . . h18a h 0.0343 -0.1306 0.3869 0.038 Uiso 1 1 calc R . . c19 c -0.10486(14) -0.3538(2) 0.44756(15) 0.0276(6) Uani 1 1 d . . . c20 c -0.11993(15) -0.4171(2) 0.50054(16) 0.0299(6) Uani 1 1 d . . . h20a h -0.0917 -0.4211 0.5447 0.036 Uiso 1 1 calc R . . c21 c -0.17656(16) -0.4743(2) 0.48810(17) 0.0351(7) Uani 1 1 d . . . h21a h -0.1877 -0.5170 0.5242 0.042 Uiso 1 1 calc R . . c22 c -0.21679(16) -0.4696(2) 0.42349(18) 0.0377(7) Uani 1 1 d . . . h22a h -0.2551 -0.5099 0.4152 0.045 Uiso 1 1 calc R . . c23 c -0.20196(16) -0.4066(2) 0.37054(17) 0.0381(7) Uani 1 1 d . . . h23a h -0.2300 -0.4038 0.3263 0.046 Uiso 1 1 calc R . . c24 c -0.14660(16) -0.3482(2) 0.38222(16) 0.0335(7) Uani 1 1 d . . . h24a h -0.1366 -0.3044 0.3464 0.040 Uiso 1 1 calc R . . c25 c 0.00473(14) -0.2888(2) 0.55065(15) 0.0276(6) Uani 1 1 d . . . c26 c -0.02513(15) -0.2352(2) 0.60126(16) 0.0321(6) Uani 1 1 d . . . h26a h -0.0607 -0.1925 0.5864 0.039 Uiso 1 1 calc R . . c27 c -0.00250(17) -0.2448(2) 0.67377(16) 0.0372(7) Uani 1 1 d . . . h27a h -0.0222 -0.2079 0.7086 0.045 Uiso 1 1 calc R . . c28 c 0.04860(16) -0.3080(2) 0.69530(16) 0.0371(7) Uani 1 1 d . . . h28a h 0.0636 -0.3146 0.7449 0.045 Uiso 1 1 calc R . . c29 c 0.07821(16) -0.3619(2) 0.64504(16) 0.0353(7) Uani 1 1 d . . . h29a h 0.1135 -0.4050 0.6601 0.042 Uiso 1 1 calc R . . c30 c 0.05620(15) -0.3525(2) 0.57292(16) 0.0327(7) Uani 1 1 d . . . h30a h 0.0762 -0.3895 0.5384 0.039 Uiso 1 1 calc R . . c31 c 0.03113(15) -0.3318(2) 0.40190(15) 0.0301(6) Uani 1 1 d . . . c32 c 0.01278(17) -0.4049(2) 0.35488(16) 0.0354(7) Uani 1 1 d . . . h32a h -0.0314 -0.4315 0.3533 0.043 Uiso 1 1 calc R . . c33 c 0.0592(2) -0.4392(2) 0.30999(18) 0.0450(8) Uani 1 1 d . . . h33a h 0.0467 -0.4894 0.2779 0.054 Uiso 1 1 calc R . . c34 c 0.12324(19) -0.4005(3) 0.31208(18) 0.0450(9) Uani 1 1 d . . . h34a h 0.1545 -0.4235 0.2809 0.054 Uiso 1 1 calc R . . c35 c 0.14207(17) -0.3282(3) 0.35952(18) 0.0425(8) Uani 1 1 d . . . h35a h 0.1864 -0.3021 0.3610 0.051 Uiso 1 1 calc R . . c36 c 0.09675(16) -0.2938(2) 0.40478(17) 0.0375(7) Uani 1 1 d . . . h36a h 0.1100 -0.2447 0.4377 0.045 Uiso 1 1 calc R . . c37 c 0.35416(15) 0.6773(2) 0.21793(15) 0.0289(6) Uani 1 1 d . . . c38 c 0.28740(15) 0.6620(2) 0.18869(15) 0.0320(6) Uani 1 1 d . . . h38a h 0.2756 0.6055 0.1633 0.038 Uiso 1 1 calc R . . c39 c 0.23853(16) 0.7293(2) 0.19676(17) 0.0382(7) Uani 1 1 d . . . h39a h 0.1929 0.7184 0.1776 0.046 Uiso 1 1 calc R . . c40 c 0.25542(17) 0.8125(2) 0.23253(17) 0.0411(8) Uani 1 1 d . . . h40a h 0.2216 0.8589 0.2373 0.049 Uiso 1 1 calc R . . c41 c 0.32162(18) 0.8279(2) 0.26137(17) 0.0406(8) Uani 1 1 d . . . h41a h 0.3332 0.8852 0.2858 0.049 Uiso 1 1 calc R . . c42 c 0.37111(16) 0.7604(2) 0.25488(16) 0.0334(7) Uani 1 1 d . . . h42a h 0.4164 0.7708 0.2755 0.040 Uiso 1 1 calc R . . c43 c 0.46871(15) 0.6423(2) 0.13391(15) 0.0311(6) Uani 1 1 d . . . c44 c 0.47571(17) 0.7398(2) 0.12606(17) 0.0392(7) Uani 1 1 d . . . h44a h 0.4505 0.7813 0.1530 0.047 Uiso 1 1 calc R . . c45 c 0.51909(19) 0.7756(3) 0.07941(19) 0.0472(9) Uani 1 1 d . . . h45a h 0.5240 0.8416 0.0746 0.057 Uiso 1 1 calc R . . c46 c 0.55525(19) 0.7151(3) 0.03980(19) 0.0488(9) Uani 1 1 d . . . h46a h 0.5852 0.7396 0.0078 0.059 Uiso 1 1 calc R . . c47 c 0.54803(19) 0.6189(3) 0.04656(19) 0.0489(9) Uani 1 1 d . . . h47a h 0.5725 0.5776 0.0187 0.059 Uiso 1 1 calc R . . c48 c 0.50485(17) 0.5823(3) 0.09417(18) 0.0403(8) Uani 1 1 d . . . h48a h 0.5004 0.5162 0.0992 0.048 Uiso 1 1 calc R . . c49 c 0.47676(14) 0.5841(2) 0.28380(15) 0.0270(6) Uani 1 1 d . . . c50 c 0.54605(15) 0.5744(2) 0.28009(17) 0.0351(7) Uani 1 1 d . . . h50a h 0.5642 0.5780 0.2350 0.042 Uiso 1 1 calc R . . c51 c 0.58874(17) 0.5593(3) 0.34283(18) 0.0430(8) Uani 1 1 d . . . h51a h 0.6363 0.5529 0.3407 0.052 Uiso 1 1 calc R . . c52 c 0.56219(17) 0.5537(2) 0.40811(17) 0.0388(7) Uani 1 1 d . . . h52a h 0.5915 0.5432 0.4508 0.047 Uiso 1 1 calc R . . c53 c 0.49335(17) 0.5632(2) 0.41165(16) 0.0347(7) Uani 1 1 d . . . h53a h 0.4755 0.5593 0.4569 0.042 Uiso 1 1 calc R . . c54 c 0.44980(15) 0.5782(2) 0.34985(15) 0.0286(6) Uani 1 1 d . . . h54a h 0.4023 0.5844 0.3524 0.034 Uiso 1 1 calc R . . c55 c 0.38697(14) 0.4826(2) 0.17778(15) 0.0284(6) Uani 1 1 d . . . c56 c 0.39319(16) 0.4077(2) 0.22706(16) 0.0340(7) Uani 1 1 d . . . h56a h 0.4181 0.4159 0.2728 0.041 Uiso 1 1 calc R . . c57 c 0.36282(18) 0.3219(2) 0.20880(18) 0.0409(8) Uani 1 1 d . . . h57a h 0.3667 0.2714 0.2422 0.049 Uiso 1 1 calc R . . c58 c 0.32683(17) 0.3099(2) 0.14193(18) 0.0396(7) Uani 1 1 d . . . h58a h 0.3060 0.2511 0.1299 0.047 Uiso 1 1 calc R . . c59 c 0.32092(16) 0.3833(2) 0.09208(17) 0.0372(7) Uani 1 1 d . . . h59a h 0.2963 0.3745 0.0463 0.045 Uiso 1 1 calc R . . c60 c 0.35122(15) 0.4689(2) 0.10994(16) 0.0322(6) Uani 1 1 d . . . h60a h 0.3478 0.5188 0.0760 0.039 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 co1 0.0313(2) 0.0269(2) 0.0286(2) -0.00207(15) 0.00795(16) -0.00080(16) cl1 0.0257(3) 0.0375(4) 0.0264(3) 0.0027(3) 0.0056(3) 0.0005(3) cl2 0.0248(3) 0.0449(4) 0.0357(4) -0.0195(3) 0.0101(3) -0.0164(3) p1 0.0265(4) 0.0291(4) 0.0218(3) 0.0028(3) 0.0019(3) 0.0012(3) p2 0.0266(4) 0.0300(4) 0.0202(3) 0.0025(3) 0.0016(3) 0.0030(3) o1 0.0569(14) 0.0273(11) 0.0358(12) -0.0001(9) 0.0230(10) -0.0006(10) o2 0.0494(13) 0.0354(12) 0.0308(11) 0.0064(9) 0.0072(10) 0.0079(10) f1 0.0526(12) 0.0585(13) 0.0356(10) -0.0125(9) 0.0021(9) -0.0141(10) f2 0.0586(13) 0.0711(15) 0.0269(10) 0.0131(9) -0.0041(9) 0.0078(11) f3 0.0530(12) 0.0362(11) 0.0539(12) 0.0162(9) 0.0134(10) 0.0008(9) f4 0.0564(13) 0.0524(13) 0.0489(12) -0.0008(10) -0.0069(10) -0.0199(10) f5 0.0559(12) 0.0526(12) 0.0259(9) 0.0078(8) -0.0048(8) 0.0069(9) f6 0.0550(12) 0.0390(11) 0.0552(12) -0.0003(9) 0.0183(10) -0.0029(9) f7 0.0969(18) 0.0292(11) 0.0625(14) 0.0020(10) 0.0210(13) -0.0097(11) f8 0.0938(18) 0.0333(11) 0.0682(15) 0.0017(10) 0.0038(13) 0.0182(12) f9 0.0487(12) 0.0584(14) 0.0598(14) -0.0059(11) -0.0027(10) 0.0095(10) f10 0.0492(12) 0.0411(11) 0.0537(12) -0.0009(9) 0.0100(9) -0.0059(9) c1 0.0370(16) 0.0269(15) 0.0272(15) 0.0000(11) 0.0116(12) 0.0031(12) c2 0.0374(17) 0.0367(17) 0.0278(15) -0.0064(12) 0.0045(13) -0.0022(13) c3 0.0365(17) 0.0449(18) 0.0240(15) 0.0083(13) 0.0014(12) 0.0061(14) c4 0.0364(17) 0.0309(16) 0.0366(17) 0.0115(13) 0.0078(13) 0.0024(13) c5 0.0346(16) 0.0353(17) 0.0332(16) -0.0022(13) 0.0017(13) -0.0027(13) c6 0.0370(16) 0.0344(16) 0.0227(14) 0.0035(12) 0.0023(12) 0.0059(13) c7 0.0441(18) 0.0299(16) 0.0259(15) -0.0063(12) 0.0018(13) -0.0007(13) c8 0.0463(19) 0.0355(17) 0.0326(16) -0.0066(13) 0.0040(14) -0.0010(14) c9 0.068(2) 0.0255(16) 0.0362(18) -0.0051(13) 0.0089(16) -0.0075(16) c10 0.061(2) 0.0264(17) 0.048(2) -0.0077(14) -0.0059(17) 0.0086(16) c11 0.052(2) 0.0382(18) 0.0330(17) -0.0074(14) -0.0002(15) 0.0126(15) c12 0.0434(18) 0.0338(16) 0.0308(16) -0.0043(13) -0.0005(13) -0.0058(14) c13 0.0302(15) 0.0302(15) 0.0220(13) 0.0031(11) 0.0033(11) 0.0007(12) c14 0.0307(15) 0.0348(16) 0.0285(15) 0.0049(12) 0.0050(12) -0.0011(13) c15 0.0352(17) 0.0356(17) 0.0368(17) 0.0016(13) 0.0073(13) 0.0036(13) c16 0.0470(19) 0.0286(16) 0.0398(18) 0.0062(13) 0.0074(14) 0.0030(14) c17 0.0422(18) 0.0342(17) 0.0348(16) 0.0042(13) 0.0118(14) -0.0042(14) c18 0.0325(16) 0.0335(16) 0.0286(15) 0.0004(12) 0.0069(12) -0.0010(12) c19 0.0280(14) 0.0280(15) 0.0267(14) 0.0004(11) 0.0020(11) 0.0019(11) c20 0.0320(15) 0.0300(15) 0.0275(15) 0.0016(11) 0.0015(12) 0.0024(12) c21 0.0349(16) 0.0295(16) 0.0412(18) 0.0036(13) 0.0054(13) -0.0003(13) c22 0.0289(16) 0.0339(17) 0.0488(19) -0.0033(14) -0.0029(14) 0.0007(13) c23 0.0362(17) 0.0398(18) 0.0357(17) -0.0019(14) -0.0090(13) 0.0044(14) c24 0.0344(16) 0.0362(17) 0.0294(15) 0.0041(12) -0.0001(12) 0.0027(13) c25 0.0280(14) 0.0288(15) 0.0258(14) 0.0020(11) 0.0009(11) -0.0051(11) c26 0.0328(16) 0.0318(16) 0.0307(15) 0.0007(12) -0.0017(12) -0.0018(12) c27 0.0428(18) 0.0417(18) 0.0270(15) -0.0058(13) 0.0025(13) -0.0057(14) c28 0.0416(18) 0.0421(18) 0.0255(15) 0.0022(13) -0.0069(13) -0.0116(14) c29 0.0320(16) 0.0385(17) 0.0338(16) 0.0051(13) -0.0055(13) -0.0022(13) c30 0.0313(16) 0.0355(17) 0.0303(15) 0.0029(12) -0.0014(12) -0.0002(13) c31 0.0318(15) 0.0365(16) 0.0226(14) 0.0066(12) 0.0058(11) 0.0075(12) c32 0.0436(18) 0.0331(16) 0.0302(16) 0.0041(13) 0.0068(13) 0.0024(14) c33 0.063(2) 0.0374(19) 0.0362(18) 0.0000(14) 0.0127(16) 0.0122(17) c34 0.053(2) 0.050(2) 0.0348(17) 0.0101(15) 0.0163(15) 0.0186(17) c35 0.0318(17) 0.058(2) 0.0382(18) 0.0093(16) 0.0077(14) 0.0090(15) c36 0.0326(16) 0.048(2) 0.0316(16) 0.0021(14) 0.0026(13) 0.0049(14) c37 0.0320(15) 0.0312(15) 0.0235(14) 0.0048(11) 0.0021(11) 0.0072(12) c38 0.0336(16) 0.0358(17) 0.0267(15) 0.0045(12) 0.0034(12) 0.0042(13) c39 0.0316(16) 0.047(2) 0.0358(17) 0.0044(14) 0.0034(13) 0.0084(14) c40 0.0433(19) 0.0441(19) 0.0360(17) 0.0039(14) 0.0047(14) 0.0197(15) c41 0.055(2) 0.0333(17) 0.0335(17) -0.0016(13) 0.0037(15) 0.0108(15) c42 0.0340(16) 0.0372(17) 0.0283(15) 0.0013(12) -0.0002(12) 0.0051(13) c43 0.0303(15) 0.0409(17) 0.0221(14) 0.0070(12) 0.0025(11) 0.0040(13) c44 0.0452(19) 0.0401(18) 0.0324(17) 0.0042(13) 0.0048(14) -0.0022(15) c45 0.058(2) 0.045(2) 0.0393(19) 0.0106(15) 0.0056(16) -0.0093(17) c46 0.047(2) 0.063(2) 0.0373(19) 0.0166(17) 0.0086(15) -0.0026(18) c47 0.052(2) 0.058(2) 0.0403(19) 0.0116(16) 0.0205(16) 0.0113(18) c48 0.0414(18) 0.0430(19) 0.0380(18) 0.0077(14) 0.0111(14) 0.0075(15) c49 0.0290(14) 0.0279(14) 0.0234(14) 0.0023(11) -0.0012(11) 0.0013(11) c50 0.0283(15) 0.0475(19) 0.0295(16) 0.0089(13) 0.0033(12) -0.0001(13) c51 0.0281(16) 0.062(2) 0.0378(18) 0.0109(16) -0.0024(13) 0.0011(15) c52 0.0396(18) 0.0460(19) 0.0289(16) 0.0076(14) -0.0065(13) 0.0027(15) c53 0.0443(18) 0.0358(17) 0.0234(15) 0.0047(12) 0.0006(13) 0.0058(14) c54 0.0290(14) 0.0312(15) 0.0260(14) 0.0024(11) 0.0041(11) 0.0033(12) c55 0.0276(14) 0.0308(15) 0.0269(14) -0.0020(11) 0.0034(11) 0.0002(12) c56 0.0409(17) 0.0331(16) 0.0278(15) -0.0004(12) 0.0020(13) 0.0026(13) c57 0.055(2) 0.0333(17) 0.0350(17) 0.0006(13) 0.0079(15) -0.0005(15) c58 0.0455(19) 0.0326(17) 0.0416(18) -0.0058(14) 0.0092(15) -0.0038(14) c59 0.0386(17) 0.0431(19) 0.0290(15) -0.0094(13) -0.0005(13) 0.0014(14) c60 0.0342(16) 0.0360(16) 0.0265(15) 0.0000(12) 0.0037(12) 0.0070(13) _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 co1 o1 1.962(2) . ? co1 o2 1.969(2) . ? co1 cl1 2.2782(8) . ? co1 cl2 2.2845(8) . ? p1 c19 1.789(3) . ? p1 c13 1.791(3) . ? p1 c25 1.795(3) . ? p1 c31 1.808(3) . ? p2 c55 1.789(3) . ? p2 c49 1.796(3) . ? p2 c37 1.797(3) . ? p2 c43 1.797(3) . ? o1 c1 1.308(3) . ? o2 c7 1.280(4) . ? f1 c2 1.344(4) . ? f2 c3 1.349(3) . ? f3 c4 1.355(3) . ? f4 c5 1.351(4) . ? f5 c6 1.355(3) . ? f6 c8 1.358(4) . ? f7 c9 1.341(4) . ? f8 c10 1.355(4) . ? f9 c11 1.335(4) . ? f10 c12 1.349(4) . ? c1 c6 1.389(4) . ? c1 c2 1.404(4) . ? c2 c3 1.375(4) . ? c3 c4 1.370(5) . ? c4 c5 1.365(4) . ? c5 c6 1.379(4) . ? c7 c8 1.401(5) . ? c7 c12 1.408(5) . ? c8 c9 1.385(5) . ? c9 c10 1.359(5) . ? c10 c11 1.380(5) . ? c11 c12 1.378(5) . ? c13 c14 1.390(4) . ? c13 c18 1.399(4) . ? c14 c15 1.381(4) . ? c15 c16 1.388(4) . ? c16 c17 1.378(5) . ? c17 c18 1.385(4) . ? c19 c20 1.393(4) . ? c19 c24 1.407(4) . ? c20 c21 1.385(4) . ? c21 c22 1.380(5) . ? c22 c23 1.389(5) . ? c23 c24 1.374(4) . ? c25 c26 1.392(4) . ? c25 c30 1.395(4) . ? c26 c27 1.391(4) . ? c27 c28 1.382(5) . ? c28 c29 1.387(5) . ? c29 c30 1.381(4) . ? c31 c32 1.386(4) . ? c31 c36 1.402(4) . ? c32 c33 1.393(4) . ? c33 c34 1.379(5) . ? c34 c35 1.385(5) . ? c35 c36 1.383(4) . ? c37 c42 1.394(4) . ? c37 c38 1.395(4) . ? c38 c39 1.379(4) . ? c39 c40 1.384(5) . ? c40 c41 1.383(5) . ? c41 c42 1.386(4) . ? c43 c48 1.378(4) . ? c43 c44 1.403(5) . ? c44 c45 1.381(5) . ? c45 c46 1.381(5) . ? c46 c47 1.384(5) . ? c47 c48 1.395(5) . ? c49 c50 1.387(4) . ? c49 c54 1.396(4) . ? c50 c51 1.392(4) . ? c51 c52 1.379(5) . ? c52 c53 1.377(5) . ? c53 c54 1.387(4) . ? c55 c60 1.403(4) . ? c55 c56 1.405(4) . ? c56 c57 1.388(5) . ? c57 c58 1.386(5) . ? c58 c59 1.396(5) . ? c59 c60 1.384(4) . ? 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 co1 o2 99.69(9) . . ? o1 co1 cl1 104.28(6) . . ? o2 co1 cl1 114.65(7) . . ? o1 co1 cl2 117.12(8) . . ? o2 co1 cl2 109.12(7) . . ? cl1 co1 cl2 111.62(3) . . ? c19 p1 c13 108.43(13) . . ? c19 p1 c25 108.25(13) . . ? c13 p1 c25 110.29(13) . . ? c19 p1 c31 108.57(14) . . ? c13 p1 c31 111.58(13) . . ? c25 p1 c31 109.63(13) . . ? c55 p2 c49 108.49(14) . . ? c55 p2 c37 111.19(14) . . ? c49 p2 c37 109.03(13) . . ? c55 p2 c43 110.82(14) . . ? c49 p2 c43 108.22(14) . . ? c37 p2 c43 109.02(14) . . ? c1 o1 co1 120.66(18) . . ? c7 o2 co1 131.30(19) . . ? o1 c1 c6 122.2(3) . . ? o1 c1 c2 123.4(3) . . ? c6 c1 c2 114.5(3) . . ? f1 c2 c3 118.9(3) . . ? f1 c2 c1 118.3(3) . . ? c3 c2 c1 122.8(3) . . ? f2 c3 c4 119.5(3) . . ? f2 c3 c2 120.0(3) . . ? c4 c3 c2 120.5(3) . . ? f3 c4 c5 120.3(3) . . ? f3 c4 c3 121.1(3) . . ? c5 c4 c3 118.7(3) . . ? f4 c5 c4 119.2(3) . . ? f4 c5 c6 120.1(3) . . ? c4 c5 c6 120.7(3) . . ? f5 c6 c5 117.6(3) . . ? f5 c6 c1 119.5(3) . . ? c5 c6 c1 122.9(3) . . ? o2 c7 c8 122.9(3) . . ? o2 c7 c12 124.1(3) . . ? c8 c7 c12 112.9(3) . . ? f6 c8 c9 117.3(3) . . ? f6 c8 c7 118.8(3) . . ? c9 c8 c7 123.9(3) . . ? f7 c9 c10 120.3(3) . . ? f7 c9 c8 119.5(3) . . ? c10 c9 c8 120.2(3) . . ? f8 c10 c9 121.1(3) . . ? f8 c10 c11 119.5(3) . . ? c9 c10 c11 119.4(3) . . ? f9 c11 c12 119.4(3) . . ? f9 c11 c10 121.2(3) . . ? c12 c11 c10 119.4(3) . . ? f10 c12 c11 117.3(3) . . ? f10 c12 c7 118.4(3) . . ? c11 c12 c7 124.2(3) . . ? c14 c13 c18 120.1(3) . . ? c14 c13 p1 118.1(2) . . ? c18 c13 p1 121.6(2) . . ? c15 c14 c13 119.9(3) . . ? c14 c15 c16 119.8(3) . . ? c17 c16 c15 120.7(3) . . ? c16 c17 c18 120.1(3) . . ? c17 c18 c13 119.5(3) . . ? c20 c19 c24 120.3(3) . . ? c20 c19 p1 121.2(2) . . ? c24 c19 p1 118.3(2) . . ? c21 c20 c19 119.2(3) . . ? c22 c21 c20 120.3(3) . . ? c21 c22 c23 120.7(3) . . ? c24 c23 c22 119.9(3) . . ? c23 c24 c19 119.6(3) . . ? c26 c25 c30 120.0(3) . . ? c26 c25 p1 119.2(2) . . ? c30 c25 p1 120.5(2) . . ? c27 c26 c25 119.5(3) . . ? c28 c27 c26 120.1(3) . . ? c27 c28 c29 120.5(3) . . ? c30 c29 c28 119.7(3) . . ? c29 c30 c25 120.2(3) . . ? c32 c31 c36 119.7(3) . . ? c32 c31 p1 120.4(2) . . ? c36 c31 p1 119.8(2) . . ? c31 c32 c33 119.9(3) . . ? c34 c33 c32 120.2(3) . . ? c33 c34 c35 120.1(3) . . ? c36 c35 c34 120.4(3) . . ? c35 c36 c31 119.7(3) . . ? c42 c37 c38 119.9(3) . . ? c42 c37 p2 118.8(2) . . ? c38 c37 p2 121.1(2) . . ? c39 c38 c37 119.7(3) . . ? c38 c39 c40 120.5(3) . . ? c41 c40 c39 119.9(3) . . ? c40 c41 c42 120.4(3) . . ? c41 c42 c37 119.6(3) . . ? c48 c43 c44 119.6(3) . . ? c48 c43 p2 119.9(2) . . ? c44 c43 p2 120.1(2) . . ? c45 c44 c43 120.3(3) . . ? c44 c45 c46 119.8(3) . . ? c45 c46 c47 120.3(3) . . ? c46 c47 c48 120.2(3) . . ? c43 c48 c47 119.8(3) . . ? c50 c49 c54 120.4(3) . . ? c50 c49 p2 119.8(2) . . ? c54 c49 p2 119.7(2) . . ? c49 c50 c51 119.5(3) . . ? c52 c51 c50 120.1(3) . . ? c53 c52 c51 120.2(3) . . ? c52 c53 c54 120.7(3) . . ? c53 c54 c49 119.1(3) . . ? c60 c55 c56 119.4(3) . . ? c60 c55 p2 120.0(2) . . ? c56 c55 p2 120.5(2) . . ? c57 c56 c55 119.9(3) . . ? c58 c57 c56 120.1(3) . . ? c57 c58 c59 120.7(3) . . ? c60 c59 c58 119.5(3) . . ? c59 c60 c55 120.5(3) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.394 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.080 #===end