# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Winpenny, Richard' _publ_contact_author_email richard.winpenny@manchester.ac.uk _publ_section_title ; Synthesis and Structural and Magnetic Characterisation of Cobalt(II) Complexes of Mixed Phosphonate-Antimonate Ligands ; _publ_author_name R.Winpenny # Attachment '- 3.cif' data_mono769 _database_code_depnum_ccdc_archive 'CCDC 700895' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H58 Cl4 Co2 N2 O20 P4 Sb4' _chemical_formula_weight 2021.64 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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)/n 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 12.3692(3) _cell_length_b 12.0030(4) _cell_length_c 24.8174(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.803(3) _cell_angle_gamma 90.00 _cell_volume 3606.67(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12301 _cell_measurement_theta_min 2.6371 _cell_measurement_theta_max 30.1111 _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 2.234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6635 _exptl_absorpt_correction_T_max 0.8075 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23484 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7343 _reflns_number_gt 5495 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The phenyl ring c31-c73 was modelled successfully. A few residual peaks around the heavy element Sb were found. 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^)+(0.0358P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7343 _refine_ls_number_parameters 475 _refine_ls_number_restraints 181 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.003 _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 Sb1 Sb 0.072420(18) 0.826934(18) 0.456575(8) 0.01512(6) Uani 1 1 d . . . Sb2 Sb 0.032576(18) 0.898141(18) 0.594690(9) 0.01594(6) Uani 1 1 d . . . Co1 Co 0.18224(4) 1.12087(4) 0.597614(18) 0.01906(11) Uani 1 1 d . . . P1 P -0.00621(7) 0.89271(7) 0.33067(3) 0.0189(2) Uani 1 1 d . . . P2 P 0.22439(7) 1.05756(7) 0.47363(3) 0.01632(19) Uani 1 1 d D . . N1 N 0.3204(2) 1.2158(3) 0.63549(12) 0.0274(7) Uani 1 1 d . . . C1 C 0.0338(3) 0.7472(3) 0.63990(13) 0.0196(8) Uani 1 1 d . C . C2 C 0.0792(3) 0.6524(3) 0.62183(15) 0.0302(9) Uani 1 1 d . . . H2 H 0.1141 0.6566 0.5912 0.036 Uiso 1 1 calc R . . C3 C 0.0738(3) 0.5510(3) 0.64834(15) 0.0342(10) Uani 1 1 d . C . H3 H 0.1047 0.4859 0.6358 0.041 Uiso 1 1 calc R . . C4 C 0.0242(3) 0.5456(3) 0.69234(14) 0.0282(9) Uani 1 1 d . . . C5 C -0.0198(3) 0.6382(3) 0.71155(16) 0.0338(10) Uani 1 1 d . C . H5 H -0.0530 0.6333 0.7428 0.041 Uiso 1 1 calc R . . C6 C -0.0155(3) 0.7399(3) 0.68501(15) 0.0322(9) Uani 1 1 d . . . H6 H -0.0466 0.8044 0.6980 0.039 Uiso 1 1 calc R C . C7 C 0.1748(3) 0.6852(3) 0.46369(13) 0.0168(7) Uani 1 1 d . B . C8 C 0.1625(3) 0.6058(3) 0.42237(14) 0.0287(9) Uani 1 1 d . . . H8A H 0.1093 0.6173 0.3894 0.034 Uiso 1 1 calc R . . C9 C 0.2259(3) 0.5107(3) 0.42827(15) 0.0366(10) Uani 1 1 d . B . H9A H 0.2161 0.4564 0.3998 0.044 Uiso 1 1 calc R . . C10 C 0.3041(3) 0.4951(3) 0.47624(14) 0.0260(8) Uani 1 1 d . . . C11 C 0.3189(3) 0.5729(3) 0.51785(15) 0.0288(9) Uani 1 1 d . B . H11 H 0.3732 0.5616 0.5505 0.035 Uiso 1 1 calc R . . C12 C 0.2541(3) 0.6674(3) 0.51181(14) 0.0234(8) Uani 1 1 d . . . H12 H 0.2634 0.7208 0.5406 0.028 Uiso 1 1 calc R B . C13 C 0.0292(3) 0.8658(3) 0.26582(14) 0.0250(8) Uani 1 1 d . . . C14 C -0.0541(3) 0.8443(3) 0.22001(14) 0.0308(9) Uani 1 1 d . . . H14 H -0.1288 0.8416 0.2240 0.037 Uiso 1 1 calc R . . C15 C -0.0292(4) 0.8269(3) 0.16876(16) 0.0429(11) Uani 1 1 d . . . H15 H -0.0868 0.8146 0.1376 0.051 Uiso 1 1 calc R . . C16 C 0.0778(4) 0.8273(4) 0.16305(17) 0.0516(13) Uani 1 1 d . . . H16 H 0.0948 0.8138 0.1280 0.062 Uiso 1 1 calc R . . C17 C 0.1617(4) 0.8472(5) 0.20771(18) 0.0604(15) Uani 1 1 d . . . H17 H 0.2363 0.8477 0.2035 0.072 Uiso 1 1 calc R . . C18 C 0.1366(4) 0.8665(4) 0.25926(17) 0.0459(12) Uani 1 1 d . . . H18 H 0.1945 0.8804 0.2901 0.055 Uiso 1 1 calc R . . C25 C 0.4180(4) 1.2104(4) 0.62017(18) 0.0499(12) Uani 1 1 d . . . H25 H 0.4282 1.1533 0.5951 0.060 Uiso 1 1 calc R . . C26 C 0.5044(4) 1.2821(4) 0.63829(19) 0.0590(14) Uani 1 1 d . . . H26 H 0.5725 1.2744 0.6266 0.071 Uiso 1 1 calc R . . C27 C 0.4887(5) 1.3660(4) 0.67427(19) 0.0616(15) Uani 1 1 d . . . H27 H 0.5459 1.4179 0.6875 0.074 Uiso 1 1 calc R . . C28 C 0.3898(4) 1.3729(4) 0.69040(19) 0.0590(15) Uani 1 1 d . . . H28 H 0.3776 1.4297 0.7152 0.071 Uiso 1 1 calc R . . C29 C 0.3079(4) 1.2971(3) 0.67049(16) 0.0389(10) Uani 1 1 d . . . H29 H 0.2395 1.3028 0.6821 0.047 Uiso 1 1 calc R . . C30 C 0.2452(3) 0.9167(3) 0.67739(13) 0.0260(8) Uani 1 1 d . . . H30A H 0.1903 0.9047 0.7002 0.039 Uiso 1 1 calc R . . H30B H 0.2957 0.9765 0.6934 0.039 Uiso 1 1 calc R . . H30C H 0.2872 0.8479 0.6759 0.039 Uiso 1 1 calc R . . C31 C 0.3466(5) 1.0718(8) 0.4467(4) 0.0208(19) Uani 0.421(8) 1 d PGDU A 1 C32 C 0.3535(6) 1.0254(7) 0.3962(4) 0.036(2) Uani 0.421(8) 1 d PGU A 1 H32 H 0.2908 0.9902 0.3743 0.043 Uiso 0.421(8) 1 calc PR A 1 C33 C 0.4521(8) 1.0305(6) 0.3777(3) 0.041(2) Uani 0.421(8) 1 d PGU A 1 H33 H 0.4568 0.9988 0.3432 0.050 Uiso 0.421(8) 1 calc PR A 1 C34 C 0.5438(6) 1.0820(6) 0.4097(4) 0.034(2) Uani 0.421(8) 1 d PGU A 1 H34 H 0.6112 1.0855 0.3971 0.041 Uiso 0.421(8) 1 calc PR A 1 C35 C 0.5369(6) 1.1284(7) 0.4602(4) 0.031(2) Uani 0.421(8) 1 d PGU A 1 H35 H 0.5996 1.1636 0.4821 0.037 Uiso 0.421(8) 1 calc PR A 1 C36 C 0.4383(7) 1.1233(8) 0.4787(3) 0.0238(19) Uani 0.421(8) 1 d PGU A 1 H36 H 0.4336 1.1550 0.5132 0.029 Uiso 0.421(8) 1 calc PR A 1 Cl1 Cl 0.38337(10) 0.37462(9) 0.48460(4) 0.0451(3) Uani 1 1 d . B 1 Cl2 Cl 0.01228(9) 0.41638(8) 0.72320(4) 0.0389(3) Uani 1 1 d . C 1 C31A C 0.3355(4) 1.0742(6) 0.4377(2) 0.0238(16) Uani 0.579(8) 1 d PGDU A 2 C32A C 0.3122(4) 1.0492(5) 0.3818(2) 0.0305(16) Uani 0.579(8) 1 d PGU A 2 H32A H 0.2388 1.0316 0.3638 0.037 Uiso 0.579(8) 1 calc PR A 2 C33A C 0.3964(5) 1.0500(5) 0.3523(2) 0.0400(17) Uani 0.579(8) 1 d PGU A 2 H33A H 0.3805 1.0330 0.3141 0.048 Uiso 0.579(8) 1 calc PR A 2 C34A C 0.5037(4) 1.0758(5) 0.3786(3) 0.0406(18) Uani 0.579(8) 1 d PGU A 2 H34A H 0.5612 1.0763 0.3585 0.049 Uiso 0.579(8) 1 calc PR A 2 C35A C 0.5270(4) 1.1007(5) 0.4345(3) 0.0268(17) Uani 0.579(8) 1 d PGU A 2 H35A H 0.6004 1.1183 0.4525 0.032 Uiso 0.579(8) 1 calc PR A 2 C36A C 0.4429(5) 1.0999(6) 0.4641(2) 0.0252(15) Uani 0.579(8) 1 d PGU A 2 H36A H 0.4588 1.1170 0.5022 0.030 Uiso 0.579(8) 1 calc PR A 2 C37 C -0.1018(3) 0.6598(3) 0.46866(14) 0.0247(8) Uani 1 1 d . . . H37A H -0.0420 0.6051 0.4773 0.037 Uiso 1 1 calc R . . H37B H -0.1696 0.6226 0.4498 0.037 Uiso 1 1 calc R . . H37C H -0.1142 0.6937 0.5028 0.037 Uiso 1 1 calc R . . O1 O -0.07212(18) 0.74490(18) 0.43363(9) 0.0189(5) Uani 1 1 d . . . O2 O 0.07993(18) 0.83136(18) 0.37456(9) 0.0194(5) Uani 1 1 d . . . O3 O 0.20192(18) 0.93097(18) 0.47082(9) 0.0180(5) Uani 1 1 d . A . O4 O 0.07084(18) 0.82079(17) 0.53392(8) 0.0176(5) Uani 1 1 d . . . O5 O 0.25099(18) 1.10154(18) 0.53115(9) 0.0196(5) Uani 1 1 d . A . O6 O 0.19027(18) 0.94750(18) 0.62271(8) 0.0187(5) Uani 1 1 d . . . O7 O 0.02925(17) 1.04514(17) 0.55871(8) 0.0160(5) Uani 1 1 d . . . O8 O 0.12185(19) 1.14328(19) 0.67020(9) 0.0216(5) Uani 1 1 d . . . O9 O -0.01024(18) 0.97976(18) 0.66026(8) 0.0185(5) Uani 1 1 d . . . O10 O -0.12954(18) 0.87914(18) 0.56394(9) 0.0187(5) Uani 1 1 d . . . 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 Sb1 0.01798(12) 0.01478(12) 0.01204(11) 0.00179(9) 0.00176(8) 0.00028(9) Sb2 0.01916(12) 0.01655(12) 0.01154(11) 0.00315(9) 0.00178(8) 0.00196(9) Co1 0.0193(3) 0.0205(3) 0.0156(2) 0.00013(19) -0.00056(18) -0.00104(19) P1 0.0241(5) 0.0208(5) 0.0115(4) 0.0008(4) 0.0028(3) 0.0013(4) P2 0.0156(4) 0.0161(5) 0.0171(5) 0.0031(4) 0.0028(3) -0.0003(3) N1 0.0256(17) 0.0329(19) 0.0219(17) -0.0030(14) 0.0006(13) -0.0056(14) C1 0.0227(19) 0.0217(19) 0.0142(17) 0.0048(14) 0.0033(14) 0.0023(15) C2 0.047(3) 0.025(2) 0.021(2) 0.0073(16) 0.0132(18) 0.0058(18) C3 0.057(3) 0.019(2) 0.029(2) 0.0058(17) 0.013(2) 0.0070(19) C4 0.038(2) 0.021(2) 0.0199(19) 0.0104(16) -0.0073(16) -0.0087(17) C5 0.044(3) 0.030(2) 0.030(2) 0.0082(18) 0.0140(19) -0.0058(19) C6 0.036(2) 0.028(2) 0.033(2) 0.0070(18) 0.0106(18) 0.0045(18) C7 0.0185(17) 0.0174(18) 0.0157(17) 0.0015(14) 0.0065(13) -0.0003(14) C8 0.036(2) 0.033(2) 0.0146(18) 0.0003(16) -0.0004(15) 0.0093(18) C9 0.055(3) 0.028(2) 0.025(2) -0.0080(17) 0.0022(19) 0.012(2) C10 0.032(2) 0.023(2) 0.026(2) 0.0021(16) 0.0126(16) 0.0115(16) C11 0.031(2) 0.029(2) 0.025(2) 0.0029(17) 0.0006(16) 0.0087(17) C12 0.030(2) 0.0186(19) 0.0195(18) -0.0026(15) 0.0007(15) 0.0015(16) C13 0.038(2) 0.0212(19) 0.0158(18) 0.0020(15) 0.0059(16) 0.0003(16) C14 0.043(2) 0.029(2) 0.0195(19) 0.0037(16) 0.0041(17) -0.0033(18) C15 0.063(3) 0.046(3) 0.018(2) 0.0004(19) 0.004(2) -0.008(2) C16 0.070(4) 0.067(3) 0.023(2) -0.005(2) 0.021(2) -0.017(3) C17 0.051(3) 0.102(4) 0.036(3) -0.015(3) 0.027(2) -0.017(3) C18 0.042(3) 0.071(3) 0.026(2) -0.012(2) 0.0111(19) -0.003(2) C25 0.040(3) 0.066(3) 0.040(3) -0.019(2) 0.000(2) -0.012(2) C26 0.036(3) 0.087(4) 0.053(3) -0.011(3) 0.007(2) -0.032(3) C27 0.070(4) 0.073(4) 0.039(3) -0.015(3) 0.004(3) -0.044(3) C28 0.076(4) 0.064(3) 0.043(3) -0.023(2) 0.026(3) -0.037(3) C29 0.047(3) 0.035(2) 0.036(2) -0.009(2) 0.011(2) -0.014(2) C30 0.024(2) 0.036(2) 0.0162(18) 0.0023(16) 0.0004(15) 0.0076(16) C31 0.024(3) 0.014(4) 0.029(4) 0.012(3) 0.016(3) 0.007(3) C32 0.031(4) 0.034(4) 0.046(4) 0.002(3) 0.016(4) 0.005(4) C33 0.040(5) 0.042(4) 0.052(5) 0.004(4) 0.031(4) 0.004(4) C34 0.032(4) 0.035(4) 0.046(5) 0.019(4) 0.032(4) 0.011(3) C35 0.027(3) 0.024(4) 0.046(5) 0.017(4) 0.017(4) 0.006(3) C36 0.018(3) 0.020(4) 0.037(4) 0.011(3) 0.015(3) 0.009(3) Cl1 0.0577(7) 0.0384(6) 0.0392(6) 0.0016(5) 0.0101(5) 0.0284(5) Cl2 0.0585(7) 0.0278(5) 0.0239(5) 0.0110(4) -0.0067(5) -0.0139(5) C31A 0.021(3) 0.017(3) 0.035(3) 0.006(3) 0.008(3) 0.003(3) C32A 0.029(3) 0.027(3) 0.039(4) 0.002(3) 0.017(3) 0.006(3) C33A 0.044(4) 0.043(4) 0.040(4) -0.001(3) 0.025(3) 0.003(3) C34A 0.036(4) 0.038(4) 0.056(4) 0.005(4) 0.030(3) -0.004(3) C35A 0.026(3) 0.022(3) 0.041(4) 0.011(3) 0.027(3) 0.006(3) C36A 0.022(3) 0.021(3) 0.036(4) 0.009(3) 0.014(3) 0.009(3) C37 0.030(2) 0.020(2) 0.0239(19) 0.0014(16) 0.0053(16) -0.0056(16) O1 0.0213(13) 0.0177(12) 0.0172(12) 0.0025(10) 0.0025(9) -0.0058(10) O2 0.0226(13) 0.0204(13) 0.0155(12) 0.0011(10) 0.0045(9) 0.0027(10) O3 0.0164(12) 0.0185(12) 0.0190(12) 0.0035(10) 0.0031(9) -0.0001(9) O4 0.0250(13) 0.0159(12) 0.0126(11) 0.0034(9) 0.0059(9) 0.0041(10) O5 0.0196(13) 0.0229(13) 0.0156(12) -0.0001(10) 0.0022(9) -0.0012(10) O6 0.0177(12) 0.0245(13) 0.0126(11) 0.0050(10) -0.0004(9) -0.0007(10) O7 0.0176(12) 0.0153(12) 0.0136(11) 0.0013(9) -0.0004(9) 0.0022(10) O8 0.0258(14) 0.0233(13) 0.0146(12) -0.0028(10) 0.0016(10) 0.0030(10) O9 0.0262(13) 0.0194(13) 0.0107(11) 0.0025(9) 0.0059(9) 0.0028(10) O10 0.0205(13) 0.0162(12) 0.0183(12) 0.0033(10) 0.0016(10) -0.0028(10) _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 Sb1 O4 1.925(2) . ? Sb1 O7 1.972(2) 3_576 ? Sb1 O3 2.005(2) . ? Sb1 O1 2.018(2) . ? Sb1 O2 2.057(2) . ? Sb1 C7 2.106(3) . ? Sb2 O4 1.911(2) . ? Sb2 O7 1.974(2) . ? Sb2 O10 2.007(2) . ? Sb2 O6 2.021(2) . ? Sb2 O9 2.059(2) . ? Sb2 C1 2.130(3) . ? Co1 O5 2.018(2) . ? Co1 O8 2.104(2) . ? Co1 N1 2.109(3) . ? Co1 O7 2.143(2) . ? Co1 O1 2.150(2) 3_576 ? Co1 O6 2.169(2) . ? P1 O8 1.490(2) 3_576 ? P1 O2 1.546(2) . ? P1 O9 1.555(2) 3_576 ? P1 C13 1.782(4) . ? P2 O5 1.494(2) . ? P2 O10 1.541(2) 3_576 ? P2 O3 1.544(2) . ? P2 C31 1.781(5) . ? P2 C31A 1.795(4) . ? N1 C29 1.337(5) . ? N1 C25 1.339(5) . ? C1 C6 1.383(5) . ? C1 C2 1.383(5) . ? C2 C3 1.391(5) . ? C2 H2 0.9500 . ? C3 C4 1.359(5) . ? C3 H3 0.9500 . ? C4 C5 1.365(5) . ? C4 Cl2 1.750(3) . ? C5 C6 1.393(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.385(5) . ? C7 C12 1.398(4) . ? C8 C9 1.376(5) . ? C8 H8A 0.9500 . ? C9 C10 1.385(5) . ? C9 H9A 0.9500 . ? C10 C11 1.376(5) . ? C10 Cl1 1.736(3) . ? C11 C12 1.379(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.370(6) . ? C13 C14 1.394(5) . ? C14 C15 1.384(5) . ? C14 H14 0.9500 . ? C15 C16 1.360(6) . ? C15 H15 0.9500 . ? C16 C17 1.375(6) . ? C16 H16 0.9500 . ? C17 C18 1.397(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C25 C26 1.374(6) . ? C25 H25 0.9500 . ? C26 C27 1.386(7) . ? C26 H26 0.9500 . ? C27 C28 1.365(7) . ? C27 H27 0.9500 . ? C28 C29 1.377(6) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 O6 1.436(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C31A C32A 1.3900 . ? C31A C36A 1.3900 . ? C32A C33A 1.3900 . ? C32A H32A 0.9500 . ? C33A C34A 1.3900 . ? C33A H33A 0.9500 . ? C34A C35A 1.3900 . ? C34A H34A 0.9500 . ? C35A C36A 1.3900 . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? C37 O1 1.437(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? O1 Co1 2.150(2) 3_576 ? O7 Sb1 1.972(2) 3_576 ? O8 P1 1.490(2) 3_576 ? O9 P1 1.554(2) 3_576 ? O10 P2 1.541(2) 3_576 ? 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 O4 Sb1 O7 94.90(9) . 3_576 ? O4 Sb1 O3 91.07(9) . . ? O7 Sb1 O3 90.23(9) 3_576 . ? O4 Sb1 O1 94.22(9) . . ? O7 Sb1 O1 80.35(9) 3_576 . ? O3 Sb1 O1 169.55(9) . . ? O4 Sb1 O2 177.91(9) . . ? O7 Sb1 O2 86.89(8) 3_576 . ? O3 Sb1 O2 87.83(9) . . ? O1 Sb1 O2 87.14(9) . . ? O4 Sb1 C7 90.80(11) . . ? O7 Sb1 C7 173.64(10) 3_576 . ? O3 Sb1 C7 92.47(11) . . ? O1 Sb1 C7 96.46(11) . . ? O2 Sb1 C7 87.46(10) . . ? O4 Sb2 O7 93.60(9) . . ? O4 Sb2 O10 91.96(9) . . ? O7 Sb2 O10 90.16(9) . . ? O4 Sb2 O6 92.09(9) . . ? O7 Sb2 O6 79.80(9) . . ? O10 Sb2 O6 169.39(9) . . ? O4 Sb2 O9 179.20(9) . . ? O7 Sb2 O9 86.98(8) . . ? O10 Sb2 O9 87.48(9) . . ? O6 Sb2 O9 88.55(9) . . ? O4 Sb2 C1 91.51(11) . . ? O7 Sb2 C1 174.87(11) . . ? O10 Sb2 C1 90.13(11) . . ? O6 Sb2 C1 99.55(11) . . ? O9 Sb2 C1 87.92(11) . . ? O5 Co1 O8 175.94(9) . . ? O5 Co1 N1 89.30(11) . . ? O8 Co1 N1 86.94(11) . . ? O5 Co1 O7 93.66(8) . . ? O8 Co1 O7 90.26(9) . . ? N1 Co1 O7 172.19(10) . . ? O5 Co1 O1 97.66(9) . 3_576 ? O8 Co1 O1 84.45(9) . 3_576 ? N1 Co1 O1 98.75(10) . 3_576 ? O7 Co1 O1 73.70(8) . 3_576 ? O5 Co1 O6 97.02(9) . . ? O8 Co1 O6 83.12(9) . . ? N1 Co1 O6 113.89(10) . . ? O7 Co1 O6 72.94(8) . . ? O1 Co1 O6 144.22(8) 3_576 . ? O8 P1 O2 113.16(13) 3_576 . ? O8 P1 O9 112.60(13) 3_576 3_576 ? O2 P1 O9 108.43(12) . 3_576 ? O8 P1 C13 110.31(15) 3_576 . ? O2 P1 C13 106.77(15) . . ? O9 P1 C13 105.10(14) 3_576 . ? O5 P2 O10 113.29(13) . 3_576 ? O5 P2 O3 113.16(13) . . ? O10 P2 O3 110.50(13) 3_576 . ? O5 P2 C31 106.6(3) . . ? O10 P2 C31 109.0(3) 3_576 . ? O3 P2 C31 103.7(3) . . ? O5 P2 C31A 113.2(2) . . ? O10 P2 C31A 102.1(2) 3_576 . ? O3 P2 C31A 103.6(2) . . ? C31 P2 C31A 7.6(5) . . ? C29 N1 C25 116.8(4) . . ? C29 N1 Co1 119.5(3) . . ? C25 N1 Co1 122.9(3) . . ? C6 C1 C2 119.1(3) . . ? C6 C1 Sb2 121.6(3) . . ? C2 C1 Sb2 119.2(2) . . ? C1 C2 C3 120.3(4) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 119.6(4) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 121.3(3) . . ? C3 C4 Cl2 119.1(3) . . ? C5 C4 Cl2 119.6(3) . . ? C4 C5 C6 119.4(4) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 120.3(4) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C12 118.6(3) . . ? C8 C7 Sb1 121.3(2) . . ? C12 C7 Sb1 120.0(2) . . ? C9 C8 C7 121.2(3) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C8 C9 C10 119.1(3) . . ? C8 C9 H9A 120.5 . . ? C10 C9 H9A 120.5 . . ? C11 C10 C9 121.1(3) . . ? C11 C10 Cl1 119.4(3) . . ? C9 C10 Cl1 119.6(3) . . ? C10 C11 C12 119.4(3) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C7 120.6(3) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C18 C13 C14 118.5(4) . . ? C18 C13 P1 122.0(3) . . ? C14 C13 P1 119.5(3) . . ? C15 C14 C13 120.7(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.4(4) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 119.6(4) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C13 C18 C17 120.7(4) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? N1 C25 C26 124.2(4) . . ? N1 C25 H25 117.9 . . ? C26 C25 H25 117.9 . . ? C25 C26 C27 117.6(5) . . ? C25 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? C28 C27 C26 119.1(4) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 119.5(5) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? N1 C29 C28 122.8(4) . . ? N1 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? O6 C30 H30A 109.5 . . ? O6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 120.0 . . ? C32 C31 P2 120.9(5) . . ? C36 C31 P2 119.0(5) . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C32A C31A C36A 120.0 . . ? C32A C31A P2 116.6(3) . . ? C36A C31A P2 123.1(3) . . ? C33A C32A C31A 120.0 . . ? C33A C32A H32A 120.0 . . ? C31A C32A H32A 120.0 . . ? C32A C33A C34A 120.0 . . ? C32A C33A H33A 120.0 . . ? C34A C33A H33A 120.0 . . ? C35A C34A C33A 120.0 . . ? C35A C34A H34A 120.0 . . ? C33A C34A H34A 120.0 . . ? C34A C35A C36A 120.0 . . ? C34A C35A H35A 120.0 . . ? C36A C35A H35A 120.0 . . ? C35A C36A C31A 120.0 . . ? C35A C36A H36A 120.0 . . ? C31A C36A H36A 120.0 . . ? O1 C37 H37A 109.5 . . ? O1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C37 O1 Sb1 119.84(19) . . ? C37 O1 Co1 122.0(2) . 3_576 ? Sb1 O1 Co1 101.27(9) . 3_576 ? P1 O2 Sb1 123.06(13) . . ? P2 O3 Sb1 138.69(14) . . ? Sb2 O4 Sb1 145.38(12) . . ? P2 O5 Co1 140.75(14) . . ? C30 O6 Sb2 119.1(2) . . ? C30 O6 Co1 120.21(19) . . ? Sb2 O6 Co1 101.43(9) . . ? Sb1 O7 Sb2 137.43(12) 3_576 . ? Sb1 O7 Co1 103.06(9) 3_576 . ? Sb2 O7 Co1 103.92(9) . . ? P1 O8 Co1 117.29(13) 3_576 . ? P1 O9 Sb2 122.39(12) 3_576 . ? P2 O10 Sb2 138.72(14) 3_576 . ? 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 O5 Co1 N1 C29 149.0(3) . . . . ? O8 Co1 N1 C29 -32.6(3) . . . . ? O7 Co1 N1 C29 36.6(9) . . . . ? O1 Co1 N1 C29 51.3(3) 3_576 . . . ? O6 Co1 N1 C29 -113.7(3) . . . . ? O5 Co1 N1 C25 -20.6(3) . . . . ? O8 Co1 N1 C25 157.9(3) . . . . ? O7 Co1 N1 C25 -132.9(7) . . . . ? O1 Co1 N1 C25 -118.2(3) 3_576 . . . ? O6 Co1 N1 C25 76.8(3) . . . . ? O4 Sb2 C1 C6 -163.3(3) . . . . ? O7 Sb2 C1 C6 21.9(14) . . . . ? O10 Sb2 C1 C6 -71.4(3) . . . . ? O6 Sb2 C1 C6 104.3(3) . . . . ? O9 Sb2 C1 C6 16.1(3) . . . . ? O4 Sb2 C1 C2 12.8(3) . . . . ? O7 Sb2 C1 C2 -162.0(11) . . . . ? O10 Sb2 C1 C2 104.8(3) . . . . ? O6 Sb2 C1 C2 -79.6(3) . . . . ? O9 Sb2 C1 C2 -167.8(3) . . . . ? C6 C1 C2 C3 0.8(6) . . . . ? Sb2 C1 C2 C3 -175.4(3) . . . . ? C1 C2 C3 C4 -0.3(6) . . . . ? C2 C3 C4 C5 -0.7(6) . . . . ? C2 C3 C4 Cl2 177.0(3) . . . . ? C3 C4 C5 C6 1.1(6) . . . . ? Cl2 C4 C5 C6 -176.5(3) . . . . ? C2 C1 C6 C5 -0.4(6) . . . . ? Sb2 C1 C6 C5 175.8(3) . . . . ? C4 C5 C6 C1 -0.6(6) . . . . ? O4 Sb1 C7 C8 143.0(3) . . . . ? O7 Sb1 C7 C8 -10.8(12) 3_576 . . . ? O3 Sb1 C7 C8 -125.9(3) . . . . ? O1 Sb1 C7 C8 48.7(3) . . . . ? O2 Sb1 C7 C8 -38.1(3) . . . . ? O4 Sb1 C7 C12 -34.2(3) . . . . ? O7 Sb1 C7 C12 172.0(8) 3_576 . . . ? O3 Sb1 C7 C12 56.9(3) . . . . ? O1 Sb1 C7 C12 -128.5(3) . . . . ? O2 Sb1 C7 C12 144.7(3) . . . . ? C12 C7 C8 C9 0.5(6) . . . . ? Sb1 C7 C8 C9 -176.8(3) . . . . ? C7 C8 C9 C10 -0.7(6) . . . . ? C8 C9 C10 C11 0.2(6) . . . . ? C8 C9 C10 Cl1 179.2(3) . . . . ? C9 C10 C11 C12 0.5(6) . . . . ? Cl1 C10 C11 C12 -178.4(3) . . . . ? C10 C11 C12 C7 -0.8(6) . . . . ? C8 C7 C12 C11 0.3(5) . . . . ? Sb1 C7 C12 C11 177.6(3) . . . . ? O8 P1 C13 C18 -164.6(3) 3_576 . . . ? O2 P1 C13 C18 -41.2(4) . . . . ? O9 P1 C13 C18 73.8(4) 3_576 . . . ? O8 P1 C13 C14 16.1(3) 3_576 . . . ? O2 P1 C13 C14 139.4(3) . . . . ? O9 P1 C13 C14 -105.5(3) 3_576 . . . ? C18 C13 C14 C15 -1.6(6) . . . . ? P1 C13 C14 C15 177.8(3) . . . . ? C13 C14 C15 C16 2.0(6) . . . . ? C14 C15 C16 C17 -1.3(7) . . . . ? C15 C16 C17 C18 0.2(8) . . . . ? C14 C13 C18 C17 0.5(7) . . . . ? P1 C13 C18 C17 -178.8(4) . . . . ? C16 C17 C18 C13 0.1(8) . . . . ? C29 N1 C25 C26 0.3(7) . . . . ? Co1 N1 C25 C26 170.2(4) . . . . ? N1 C25 C26 C27 -0.7(8) . . . . ? C25 C26 C27 C28 0.7(8) . . . . ? C26 C27 C28 C29 -0.3(8) . . . . ? C25 N1 C29 C28 0.1(6) . . . . ? Co1 N1 C29 C28 -170.1(4) . . . . ? C27 C28 C29 N1 -0.1(7) . . . . ? O5 P2 C31 C32 171.8(5) . . . . ? O10 P2 C31 C32 -65.6(6) 3_576 . . . ? O3 P2 C31 C32 52.1(6) . . . . ? C31A P2 C31 C32 -39(4) . . . . ? O5 P2 C31 C36 -3.7(5) . . . . ? O10 P2 C31 C36 118.9(4) 3_576 . . . ? O3 P2 C31 C36 -123.4(4) . . . . ? C31A P2 C31 C36 146(4) . . . . ? C36 C31 C32 C33 0.0 . . . . ? P2 C31 C32 C33 -175.4(7) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? P2 C31 C36 C35 175.5(7) . . . . ? O5 P2 C31A C32A -171.6(3) . . . . ? O10 P2 C31A C32A -49.5(4) 3_576 . . . ? O3 P2 C31A C32A 65.4(4) . . . . ? C31 P2 C31A C32A 156(4) . . . . ? O5 P2 C31A C36A 14.6(4) . . . . ? O10 P2 C31A C36A 136.7(3) 3_576 . . . ? O3 P2 C31A C36A -108.4(3) . . . . ? C31 P2 C31A C36A -17(4) . . . . ? C36A C31A C32A C33A 0.0 . . . . ? P2 C31A C32A C33A -174.0(5) . . . . ? C31A C32A C33A C34A 0.0 . . . . ? C32A C33A C34A C35A 0.0 . . . . ? C33A C34A C35A C36A 0.0 . . . . ? C34A C35A C36A C31A 0.0 . . . . ? C32A C31A C36A C35A 0.0 . . . . ? P2 C31A C36A C35A 173.6(5) . . . . ? O4 Sb1 O1 C37 -33.3(2) . . . . ? O7 Sb1 O1 C37 -127.6(2) 3_576 . . . ? O3 Sb1 O1 C37 -153.5(4) . . . . ? O2 Sb1 O1 C37 145.1(2) . . . . ? C7 Sb1 O1 C37 58.0(2) . . . . ? O4 Sb1 O1 Co1 104.16(9) . . . 3_576 ? O7 Sb1 O1 Co1 9.89(9) 3_576 . . 3_576 ? O3 Sb1 O1 Co1 -16.1(5) . . . 3_576 ? O2 Sb1 O1 Co1 -77.44(9) . . . 3_576 ? C7 Sb1 O1 Co1 -164.55(11) . . . 3_576 ? O8 P1 O2 Sb1 -54.70(18) 3_576 . . . ? O9 P1 O2 Sb1 70.97(17) 3_576 . . . ? C13 P1 O2 Sb1 -176.25(16) . . . . ? O4 Sb1 O2 P1 -167(2) . . . . ? O7 Sb1 O2 P1 -17.66(15) 3_576 . . . ? O3 Sb1 O2 P1 -108.01(16) . . . . ? O1 Sb1 O2 P1 62.82(15) . . . . ? C7 Sb1 O2 P1 159.43(17) . . . . ? O5 P2 O3 Sb1 100.0(2) . . . . ? O10 P2 O3 Sb1 -28.3(2) 3_576 . . . ? C31 P2 O3 Sb1 -144.9(4) . . . . ? C31A P2 O3 Sb1 -137.1(3) . . . . ? O4 Sb1 O3 P2 -91.5(2) . . . . ? O7 Sb1 O3 P2 3.4(2) 3_576 . . . ? O1 Sb1 O3 P2 29.0(6) . . . . ? O2 Sb1 O3 P2 90.3(2) . . . . ? C7 Sb1 O3 P2 177.7(2) . . . . ? O7 Sb2 O4 Sb1 -19.8(2) . . . . ? O10 Sb2 O4 Sb1 70.5(2) . . . . ? O6 Sb2 O4 Sb1 -99.7(2) . . . . ? O9 Sb2 O4 Sb1 117(6) . . . . ? C1 Sb2 O4 Sb1 160.7(2) . . . . ? O7 Sb1 O4 Sb2 -14.5(2) 3_576 . . . ? O3 Sb1 O4 Sb2 75.8(2) . . . . ? O1 Sb1 O4 Sb2 -95.2(2) . . . . ? O2 Sb1 O4 Sb2 134(2) . . . . ? C7 Sb1 O4 Sb2 168.3(2) . . . . ? O10 P2 O5 Co1 62.9(2) 3_576 . . . ? O3 P2 O5 Co1 -63.8(2) . . . . ? C31 P2 O5 Co1 -177.2(4) . . . . ? C31A P2 O5 Co1 178.6(3) . . . . ? O8 Co1 O5 P2 165.9(12) . . . . ? N1 Co1 O5 P2 -171.8(2) . . . . ? O7 Co1 O5 P2 0.9(2) . . . . ? O1 Co1 O5 P2 -73.1(2) 3_576 . . . ? O6 Co1 O5 P2 74.2(2) . . . . ? O4 Sb2 O6 C30 -121.6(2) . . . . ? O7 Sb2 O6 C30 145.1(2) . . . . ? O10 Sb2 O6 C30 126.0(5) . . . . ? O9 Sb2 O6 C30 58.0(2) . . . . ? C1 Sb2 O6 C30 -29.7(2) . . . . ? O4 Sb2 O6 Co1 103.97(9) . . . . ? O7 Sb2 O6 Co1 10.69(9) . . . . ? O10 Sb2 O6 Co1 -8.4(5) . . . . ? O9 Sb2 O6 Co1 -76.50(9) . . . . ? C1 Sb2 O6 Co1 -164.15(11) . . . . ? O5 Co1 O6 C30 124.4(2) . . . . ? O8 Co1 O6 C30 -51.6(2) . . . . ? N1 Co1 O6 C30 32.0(3) . . . . ? O7 Co1 O6 C30 -144.0(2) . . . . ? O1 Co1 O6 C30 -122.0(2) 3_576 . . . ? O5 Co1 O6 Sb2 -101.82(10) . . . . ? O8 Co1 O6 Sb2 82.27(10) . . . . ? N1 Co1 O6 Sb2 165.83(11) . . . . ? O7 Co1 O6 Sb2 -10.13(8) . . . . ? O1 Co1 O6 Sb2 11.78(19) 3_576 . . . ? O4 Sb2 O7 Sb1 129.72(16) . . . 3_576 ? O10 Sb2 O7 Sb1 37.74(16) . . . 3_576 ? O6 Sb2 O7 Sb1 -138.80(17) . . . 3_576 ? O9 Sb2 O7 Sb1 -49.73(16) . . . 3_576 ? C1 Sb2 O7 Sb1 -55.5(13) . . . 3_576 ? O4 Sb2 O7 Co1 -102.41(10) . . . . ? O10 Sb2 O7 Co1 165.62(10) . . . . ? O6 Sb2 O7 Co1 -10.93(9) . . . . ? O9 Sb2 O7 Co1 78.15(10) . . . . ? C1 Sb2 O7 Co1 72.3(12) . . . . ? O5 Co1 O7 Sb1 -106.54(10) . . . 3_576 ? O8 Co1 O7 Sb1 74.51(10) . . . 3_576 ? N1 Co1 O7 Sb1 5.5(8) . . . 3_576 ? O1 Co1 O7 Sb1 -9.63(8) 3_576 . . 3_576 ? O6 Co1 O7 Sb1 157.23(11) . . . 3_576 ? O5 Co1 O7 Sb2 106.70(10) . . . . ? O8 Co1 O7 Sb2 -72.25(10) . . . . ? N1 Co1 O7 Sb2 -141.2(7) . . . . ? O1 Co1 O7 Sb2 -156.39(11) 3_576 . . . ? O6 Co1 O7 Sb2 10.48(9) . . . . ? O5 Co1 O8 P1 -167.0(12) . . . 3_576 ? N1 Co1 O8 P1 170.71(16) . . . 3_576 ? O7 Co1 O8 P1 -1.99(15) . . . 3_576 ? O1 Co1 O8 P1 71.60(15) 3_576 . . 3_576 ? O6 Co1 O8 P1 -74.78(14) . . . 3_576 ? O4 Sb2 O9 P1 -156(6) . . . 3_576 ? O7 Sb2 O9 P1 -19.19(15) . . . 3_576 ? O10 Sb2 O9 P1 -109.49(15) . . . 3_576 ? O6 Sb2 O9 P1 60.67(15) . . . 3_576 ? C1 Sb2 O9 P1 160.29(17) . . . 3_576 ? O4 Sb2 O10 P2 -91.5(2) . . . 3_576 ? O7 Sb2 O10 P2 2.1(2) . . . 3_576 ? O6 Sb2 O10 P2 20.9(6) . . . 3_576 ? O9 Sb2 O10 P2 89.1(2) . . . 3_576 ? C1 Sb2 O10 P2 177.0(2) . . . 3_576 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.884 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.105 # Attachment '- 4.cif' data_orepw787mono _database_code_depnum_ccdc_archive 'CCDC 778674' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H62 Cl4 Co2 N2 O20 P4 Sb4' _chemical_formula_weight 2049.70 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n 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 12.4428(4) _cell_length_b 11.9106(4) _cell_length_c 24.8044(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.870(3) _cell_angle_gamma 90.00 _cell_volume 3597.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9443 _cell_measurement_theta_min 2.6393 _cell_measurement_theta_max 23.8988 _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2012 _exptl_absorpt_coefficient_mu 2.241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6042 _exptl_absorpt_correction_T_max 0.8069 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20379 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7300 _reflns_number_gt 5456 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; A larger than usual U(eq) range for carbon was due to slight disorder in one of the phenyl ring. 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^)+(0.0315P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7300 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 Sb1 Sb 0.535647(19) 0.60227(2) 0.094406(9) 0.01168(7) Uani 1 1 d . . . Sb2 Sb 0.571081(19) 0.67460(2) -0.044001(9) 0.01110(7) Uani 1 1 d . . . Co1 Co 0.68403(4) 0.37783(4) 0.096668(19) 0.01388(12) Uani 1 1 d . . . O1 O 0.42737(19) 0.7576(2) -0.06611(9) 0.0138(6) Uani 1 1 d . . . O2 O 0.69974(19) 0.5693(2) -0.03113(10) 0.0142(6) Uani 1 1 d . . . O3 O 0.5772(2) 0.6706(2) -0.12620(9) 0.0134(5) Uani 1 1 d . . . O4 O 0.37446(19) 0.6233(2) 0.06382(10) 0.0143(6) Uani 1 1 d . . . O5 O 0.49255(19) 0.5203(2) 0.16003(9) 0.0135(6) Uani 1 1 d . . . O6 O 0.69228(19) 0.5518(2) 0.12199(9) 0.0144(6) Uani 1 1 d . . . O7 O 0.75236(19) 0.3983(2) 0.02951(9) 0.0151(6) Uani 1 1 d . . . O8 O 0.6244(2) 0.3558(2) 0.16994(10) 0.0161(6) Uani 1 1 d . . . O9 O 0.53105(18) 0.45428(19) 0.05824(9) 0.0112(5) Uani 1 1 d . . . O10 O 0.57343(19) 0.68096(19) 0.03385(9) 0.0124(5) Uani 1 1 d . . . P1 P 0.72198(8) 0.44161(8) -0.02820(4) 0.0121(2) Uani 1 1 d . . . P2 P 0.50945(8) 0.39190(8) 0.16957(4) 0.0132(2) Uani 1 1 d . . . N1 N 0.8238(3) 0.2865(3) 0.13530(12) 0.0179(7) Uani 1 1 d . . . C1 C 0.6728(3) 0.8173(3) -0.03690(14) 0.0124(8) Uani 1 1 d . . . C2 C 0.7583(3) 0.8301(3) 0.00922(14) 0.0183(9) Uani 1 1 d . . . H2 H 0.7727 0.7723 0.0361 0.022 Uiso 1 1 calc R . . C3 C 0.8220(3) 0.9265(3) 0.01590(16) 0.0224(9) Uani 1 1 d . . . H3 H 0.8803 0.9348 0.0470 0.027 Uiso 1 1 calc R . . C4 C 0.7997(3) 1.0102(3) -0.02316(15) 0.0189(9) Uani 1 1 d . . . C5 C 0.7151(3) 1.0000(3) -0.06918(15) 0.0217(9) Uani 1 1 d . . . H5 H 0.7003 1.0586 -0.0957 0.026 Uiso 1 1 calc R . . C6 C 0.6531(3) 0.9030(3) -0.07562(15) 0.0188(9) Uani 1 1 d . . . H6 H 0.5958 0.8947 -0.1072 0.023 Uiso 1 1 calc R . . C7 C 0.5383(3) 0.7531(3) 0.13980(14) 0.0161(9) Uani 1 1 d . . . C8 C 0.5922(3) 0.8472(3) 0.12454(16) 0.0258(10) Uani 1 1 d . . . H8 H 0.6323 0.8410 0.0960 0.031 Uiso 1 1 calc R . . C9 C 0.5877(4) 0.9500(4) 0.15082(16) 0.0276(10) Uani 1 1 d . . . H9 H 0.6244 1.0137 0.1402 0.033 Uiso 1 1 calc R . . C10 C 0.5303(3) 0.9585(3) 0.19199(15) 0.0215(10) Uani 1 1 d . . . C11 C 0.4779(4) 0.8667(4) 0.20846(17) 0.0287(10) Uani 1 1 d . . . H11 H 0.4393 0.8733 0.2376 0.034 Uiso 1 1 calc R . . C12 C 0.4818(3) 0.7646(3) 0.18211(17) 0.0262(10) Uani 1 1 d . . . H12 H 0.4451 0.7015 0.1933 0.031 Uiso 1 1 calc R . . C13 C 0.8326(3) 0.4261(3) -0.06321(16) 0.0177(9) Uani 1 1 d . . . C14 C 0.9384(3) 0.4000(4) -0.03770(19) 0.0305(11) Uani 1 1 d . . . H14 H 0.9549 0.3805 0.0002 0.037 Uiso 1 1 calc R . . C15 C 1.0238(4) 0.4026(4) -0.0686(3) 0.0446(14) Uani 1 1 d . . . H15 H 1.0978 0.3873 -0.0514 0.053 Uiso 1 1 calc R . . C16 C 0.9963(5) 0.4275(4) -0.1234(2) 0.0524(15) Uani 1 1 d . . . H16 H 1.0530 0.4315 -0.1438 0.063 Uiso 1 1 calc R . . C17 C 0.8911(5) 0.4467(5) -0.1501(2) 0.0521(15) Uani 1 1 d . . . H17 H 0.8742 0.4595 -0.1887 0.063 Uiso 1 1 calc R . . C18 C 0.8101(4) 0.4474(4) -0.12041(19) 0.0378(12) Uani 1 1 d . . . H18 H 0.7367 0.4626 -0.1387 0.045 Uiso 1 1 calc R . . C19 C 0.4760(3) 0.3669(3) 0.23495(14) 0.0164(8) Uani 1 1 d . . . C20 C 0.3685(4) 0.3690(4) 0.24188(17) 0.0279(10) Uani 1 1 d . . . H20 H 0.3105 0.3810 0.2109 0.033 Uiso 1 1 calc R . . C21 C 0.3444(4) 0.3537(4) 0.29376(18) 0.0368(12) Uani 1 1 d . . . H21 H 0.2702 0.3535 0.2980 0.044 Uiso 1 1 calc R . . C22 C 0.4284(4) 0.3387(4) 0.33899(17) 0.0367(12) Uani 1 1 d . . . H22 H 0.4124 0.3297 0.3746 0.044 Uiso 1 1 calc R . . C23 C 0.5355(4) 0.3370(4) 0.33245(17) 0.0330(11) Uani 1 1 d . . . H23 H 0.5932 0.3263 0.3637 0.040 Uiso 1 1 calc R . . C24 C 0.5601(4) 0.3508(3) 0.28106(15) 0.0242(10) Uani 1 1 d . . . H24 H 0.6344 0.3492 0.2771 0.029 Uiso 1 1 calc R . . C25 C 0.8150(4) 0.2096(4) 0.17336(17) 0.0283(10) Uani 1 1 d . . . H25 H 0.7481 0.2037 0.1859 0.034 Uiso 1 1 calc R . . C26 C 0.9006(4) 0.1383(4) 0.19490(19) 0.0411(13) Uani 1 1 d . . . H26 H 0.8922 0.0845 0.2220 0.049 Uiso 1 1 calc R . . C27 C 0.9983(4) 0.1453(4) 0.17706(18) 0.0361(12) Uani 1 1 d . . . H27 H 1.0576 0.0966 0.1918 0.043 Uiso 1 1 calc R . . C28 C 1.0087(3) 0.2240(4) 0.13741(16) 0.0266(10) Uani 1 1 d . . . C29 C 0.9189(3) 0.2916(3) 0.11800(16) 0.0233(10) Uani 1 1 d . . . H29 H 0.9250 0.3454 0.0905 0.028 Uiso 1 1 calc R . . C31 C 0.7474(3) 0.5824(3) 0.17671(15) 0.0229(10) Uani 1 1 d . . . H31A H 0.7910 0.6504 0.1751 0.034 Uiso 1 1 calc R . . H31B H 0.7959 0.5211 0.1930 0.034 Uiso 1 1 calc R . . H31C H 0.6929 0.5967 0.1994 0.034 Uiso 1 1 calc R . . C32 C 0.3978(3) 0.8436(3) -0.03066(15) 0.0189(9) Uani 1 1 d . . . H32A H 0.3872 0.8095 0.0038 0.028 Uiso 1 1 calc R . . H32B H 0.3296 0.8801 -0.0492 0.028 Uiso 1 1 calc R . . H32C H 0.4567 0.8996 -0.0226 0.028 Uiso 1 1 calc R . . C34 C 1.1120(4) 0.2348(4) 0.11502(19) 0.0394(12) Uani 1 1 d . . . H34A H 1.1761 0.2235 0.1449 0.059 Uiso 1 1 calc R . . H34B H 1.1153 0.3099 0.0993 0.059 Uiso 1 1 calc R . . H34C H 1.1118 0.1781 0.0864 0.059 Uiso 1 1 calc R . . Cl1 Cl 0.87850(9) 1.13216(9) -0.01423(4) 0.0314(3) Uani 1 1 d . . . Cl2 Cl 0.51895(9) 1.08873(8) 0.22223(4) 0.0291(3) Uani 1 1 d . . . 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 Sb1 0.01351(13) 0.01182(14) 0.01022(11) -0.00147(9) 0.00363(9) -0.00101(10) Sb2 0.01188(13) 0.01126(13) 0.01063(11) -0.00067(9) 0.00344(9) -0.00048(10) Co1 0.0122(3) 0.0156(3) 0.0137(2) 0.0003(2) 0.00253(19) 0.0010(2) O1 0.0134(13) 0.0143(14) 0.0147(12) -0.0009(10) 0.0051(10) 0.0046(11) O2 0.0108(13) 0.0167(14) 0.0153(13) 0.0010(10) 0.0033(10) 0.0007(11) O3 0.0181(14) 0.0139(14) 0.0096(11) 0.0021(10) 0.0057(10) -0.0010(11) O4 0.0134(13) 0.0138(14) 0.0161(13) -0.0003(10) 0.0039(10) 0.0052(11) O5 0.0166(13) 0.0139(14) 0.0116(12) -0.0001(10) 0.0064(10) -0.0022(11) O6 0.0121(13) 0.0196(15) 0.0112(12) -0.0002(10) 0.0015(10) -0.0012(11) O7 0.0123(13) 0.0191(15) 0.0145(12) 0.0030(11) 0.0042(10) 0.0010(11) O8 0.0171(14) 0.0167(14) 0.0138(13) 0.0019(10) 0.0018(10) 0.0010(11) O9 0.0089(12) 0.0092(13) 0.0148(12) -0.0014(10) 0.0009(10) -0.0019(10) O10 0.0181(13) 0.0105(13) 0.0094(11) -0.0023(10) 0.0044(10) -0.0030(11) P1 0.0107(5) 0.0121(5) 0.0143(5) -0.0011(4) 0.0045(4) 0.0008(4) P2 0.0160(5) 0.0133(5) 0.0106(4) 0.0004(4) 0.0036(4) -0.0008(4) N1 0.0204(18) 0.0174(18) 0.0172(16) 0.0020(13) 0.0068(14) 0.0041(14) C1 0.0121(18) 0.013(2) 0.0127(17) -0.0013(15) 0.0035(14) -0.0007(16) C2 0.018(2) 0.022(2) 0.0142(18) 0.0047(16) 0.0038(15) 0.0018(18) C3 0.020(2) 0.026(2) 0.021(2) -0.0007(17) 0.0014(16) -0.0045(18) C4 0.018(2) 0.015(2) 0.026(2) -0.0072(16) 0.0107(16) -0.0060(17) C5 0.027(2) 0.021(2) 0.019(2) 0.0042(16) 0.0093(17) -0.0008(18) C6 0.017(2) 0.025(2) 0.0127(18) -0.0002(16) -0.0004(15) -0.0008(18) C7 0.018(2) 0.018(2) 0.0111(18) -0.0025(15) 0.0007(15) -0.0006(17) C8 0.036(3) 0.021(2) 0.024(2) -0.0008(17) 0.0147(19) -0.0044(19) C9 0.045(3) 0.014(2) 0.027(2) -0.0020(17) 0.014(2) -0.006(2) C10 0.030(2) 0.014(2) 0.0175(19) -0.0054(16) -0.0023(17) 0.0071(18) C11 0.037(3) 0.025(2) 0.028(2) -0.0075(18) 0.0180(19) 0.000(2) C12 0.032(3) 0.018(2) 0.031(2) -0.0027(18) 0.0120(19) -0.0069(19) C13 0.020(2) 0.007(2) 0.030(2) -0.0019(16) 0.0136(17) 0.0000(16) C14 0.022(2) 0.026(3) 0.045(3) -0.020(2) 0.010(2) -0.004(2) C15 0.024(3) 0.028(3) 0.084(4) -0.032(3) 0.017(3) -0.005(2) C16 0.057(4) 0.048(4) 0.067(4) -0.011(3) 0.046(3) -0.015(3) C17 0.062(4) 0.054(4) 0.052(3) 0.012(3) 0.040(3) 0.012(3) C18 0.044(3) 0.037(3) 0.041(3) 0.009(2) 0.030(2) 0.014(2) C19 0.026(2) 0.011(2) 0.0138(18) -0.0007(14) 0.0075(16) 0.0003(17) C20 0.034(3) 0.032(3) 0.020(2) 0.0077(18) 0.0098(18) -0.002(2) C21 0.034(3) 0.047(3) 0.034(3) 0.004(2) 0.019(2) 0.008(2) C22 0.061(3) 0.037(3) 0.016(2) 0.0019(19) 0.017(2) 0.013(3) C23 0.045(3) 0.037(3) 0.016(2) -0.0002(19) 0.004(2) 0.007(2) C24 0.034(2) 0.021(2) 0.017(2) -0.0006(16) 0.0034(18) 0.0023(19) C25 0.031(2) 0.027(3) 0.031(2) 0.0078(19) 0.0152(19) 0.009(2) C26 0.049(3) 0.040(3) 0.040(3) 0.021(2) 0.023(2) 0.023(2) C27 0.038(3) 0.041(3) 0.030(2) 0.010(2) 0.007(2) 0.022(2) C28 0.023(2) 0.032(3) 0.023(2) -0.0073(18) 0.0010(18) 0.010(2) C29 0.020(2) 0.027(2) 0.022(2) 0.0015(17) 0.0026(17) 0.0041(18) C31 0.021(2) 0.026(2) 0.020(2) -0.0033(17) 0.0004(16) -0.0057(18) C32 0.021(2) 0.017(2) 0.021(2) -0.0019(16) 0.0092(16) 0.0033(17) C34 0.026(3) 0.051(3) 0.042(3) 0.000(2) 0.008(2) 0.013(2) Cl1 0.0378(6) 0.0264(6) 0.0321(6) -0.0051(4) 0.0117(5) -0.0177(5) Cl2 0.0432(6) 0.0202(6) 0.0212(5) -0.0061(4) 0.0003(4) 0.0060(5) _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 Sb1 O10 1.910(2) . ? Sb1 O9 1.973(2) . ? Sb1 O4 2.009(2) . ? Sb1 O6 2.020(2) . ? Sb1 O5 2.062(2) . ? Sb1 C7 2.117(4) . ? Sb2 O10 1.927(2) . ? Sb2 O9 1.978(2) 3_665 ? Sb2 O2 2.006(2) . ? Sb2 O1 2.018(2) . ? Sb2 O3 2.057(2) . ? Sb2 C1 2.105(4) . ? Co1 O7 2.035(3) . ? Co1 N1 2.107(3) . ? Co1 O8 2.116(3) . ? Co1 O9 2.148(2) . ? Co1 O1 2.160(2) 3_665 ? Co1 O6 2.161(2) . ? O1 C32 1.446(4) . ? O1 Co1 2.160(2) 3_665 ? O2 P1 1.545(3) . ? O3 P2 1.548(2) 3_665 ? O4 P1 1.543(2) 3_665 ? O5 P2 1.555(3) . ? O6 C31 1.436(4) . ? O7 P1 1.495(2) . ? O8 P2 1.492(3) . ? O9 Sb2 1.978(2) 3_665 ? P1 O4 1.543(2) 3_665 ? P1 C13 1.782(4) . ? P2 O3 1.548(2) 3_665 ? P2 C19 1.780(4) . ? N1 C25 1.337(5) . ? N1 C29 1.341(5) . ? C1 C6 1.388(5) . ? C1 C2 1.401(4) . ? C2 C3 1.385(5) . ? C2 H2 0.9500 . ? C3 C4 1.378(5) . ? C3 H3 0.9500 . ? C4 C5 1.390(5) . ? C4 Cl1 1.741(4) . ? C5 C6 1.380(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.386(6) . ? C7 C8 1.397(5) . ? C8 C9 1.394(6) . ? C8 H8 0.9500 . ? C9 C10 1.365(6) . ? C9 H9 0.9500 . ? C10 C11 1.377(6) . ? C10 Cl2 1.742(4) . ? C11 C12 1.386(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.374(5) . ? C13 C18 1.412(6) . ? C14 C15 1.433(7) . ? C14 H14 0.9500 . ? C15 C16 1.364(7) . ? C15 H15 0.9500 . ? C16 C17 1.359(7) . ? C16 H16 0.9500 . ? C17 C18 1.365(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.383(6) . ? C19 C24 1.396(5) . ? C20 C21 1.392(6) . ? C20 H20 0.9500 . ? C21 C22 1.379(6) . ? C21 H21 0.9500 . ? C22 C23 1.374(7) . ? C22 H22 0.9500 . ? C23 C24 1.380(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.381(6) . ? C25 H25 0.9500 . ? C26 C27 1.379(7) . ? C26 H26 0.9500 . ? C27 C28 1.384(6) . ? C27 H27 0.9500 . ? C28 C29 1.381(5) . ? C28 C34 1.507(6) . ? C29 H29 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? 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 O10 Sb1 O9 93.99(10) . . ? O10 Sb1 O4 91.72(10) . . ? O9 Sb1 O4 90.36(9) . . ? O10 Sb1 O6 92.07(10) . . ? O9 Sb1 O6 79.85(9) . . ? O4 Sb1 O6 169.72(10) . . ? O10 Sb1 O5 178.70(10) . . ? O9 Sb1 O5 87.02(10) . . ? O4 Sb1 O5 87.45(10) . . ? O6 Sb1 O5 88.91(10) . . ? O10 Sb1 C7 91.28(12) . . ? O9 Sb1 C7 174.70(12) . . ? O4 Sb1 C7 90.02(12) . . ? O6 Sb1 C7 99.44(11) . . ? O5 Sb1 C7 87.72(12) . . ? O10 Sb2 O9 94.95(10) . 3_665 ? O10 Sb2 O2 91.03(10) . . ? O9 Sb2 O2 90.33(10) 3_665 . ? O10 Sb2 O1 94.76(10) . . ? O9 Sb2 O1 80.25(9) 3_665 . ? O2 Sb2 O1 169.32(9) . . ? O10 Sb2 O3 176.94(10) . . ? O9 Sb2 O3 87.61(10) 3_665 . ? O2 Sb2 O3 87.26(10) . . ? O1 Sb2 O3 87.33(10) . . ? O10 Sb2 C1 89.97(12) . . ? O9 Sb2 C1 174.25(11) 3_665 . ? O2 Sb2 C1 92.57(12) . . ? O1 Sb2 C1 96.39(12) . . ? O3 Sb2 C1 87.57(12) . . ? O7 Co1 N1 89.40(11) . . ? O7 Co1 O8 175.93(9) . . ? N1 Co1 O8 87.01(11) . . ? O7 Co1 O9 93.85(9) . . ? N1 Co1 O9 173.57(11) . . ? O8 Co1 O9 89.91(9) . . ? O7 Co1 O1 98.54(9) . 3_665 ? N1 Co1 O1 100.62(11) . 3_665 ? O8 Co1 O1 84.02(9) . 3_665 ? O9 Co1 O1 73.42(8) . 3_665 ? O7 Co1 O6 96.89(10) . . ? N1 Co1 O6 112.15(10) . . ? O8 Co1 O6 82.71(10) . . ? O9 Co1 O6 72.99(8) . . ? O1 Co1 O6 143.75(9) 3_665 . ? C32 O1 Sb2 120.24(19) . . ? C32 O1 Co1 121.2(2) . 3_665 ? Sb2 O1 Co1 101.45(10) . 3_665 ? P1 O2 Sb2 138.75(15) . . ? P2 O3 Sb2 122.53(15) 3_665 . ? P1 O4 Sb1 138.78(15) 3_665 . ? P2 O5 Sb1 122.48(15) . . ? C31 O6 Sb1 119.0(2) . . ? C31 O6 Co1 120.2(2) . . ? Sb1 O6 Co1 101.67(10) . . ? P1 O7 Co1 139.41(15) . . ? P2 O8 Co1 117.66(13) . . ? Sb1 O9 Sb2 137.05(14) . 3_665 ? Sb1 O9 Co1 103.69(9) . . ? Sb2 O9 Co1 103.21(10) 3_665 . ? Sb1 O10 Sb2 144.46(13) . . ? O7 P1 O4 112.90(14) . 3_665 ? O7 P1 O2 113.08(14) . . ? O4 P1 O2 110.83(13) 3_665 . ? O7 P1 C13 111.24(16) . . ? O4 P1 C13 104.87(16) 3_665 . ? O2 P1 C13 103.19(16) . . ? O8 P2 O3 113.31(14) . 3_665 ? O8 P2 O5 112.57(15) . . ? O3 P2 O5 108.29(13) 3_665 . ? O8 P2 C19 110.50(16) . . ? O3 P2 C19 107.02(16) 3_665 . ? O5 P2 C19 104.66(16) . . ? C25 N1 C29 117.6(3) . . ? C25 N1 Co1 119.7(3) . . ? C29 N1 Co1 122.1(3) . . ? C6 C1 C2 118.8(3) . . ? C6 C1 Sb2 121.2(2) . . ? C2 C1 Sb2 119.9(3) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 119.2(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 121.5(3) . . ? C3 C4 Cl1 119.2(3) . . ? C5 C4 Cl1 119.3(3) . . ? C6 C5 C4 118.6(3) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C1 121.4(3) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? C12 C7 C8 118.2(4) . . ? C12 C7 Sb1 122.1(3) . . ? C8 C7 Sb1 119.5(3) . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 119.5(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 121.1(4) . . ? C9 C10 Cl2 119.3(3) . . ? C11 C10 Cl2 119.6(3) . . ? C10 C11 C12 119.4(4) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C7 C12 C11 121.1(4) . . ? C7 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C18 118.5(4) . . ? C14 C13 P1 124.2(3) . . ? C18 C13 P1 117.2(3) . . ? C13 C14 C15 119.6(4) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 118.5(5) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C17 C16 C15 122.7(5) . . ? C17 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? C16 C17 C18 118.9(5) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C17 C18 C13 121.7(5) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? C20 C19 C24 118.8(4) . . ? C20 C19 P2 121.6(3) . . ? C24 C19 P2 119.5(3) . . ? C19 C20 C21 120.7(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 C20 119.8(4) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 119.8(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.8(4) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C19 120.1(4) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? N1 C25 C26 121.7(4) . . ? N1 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C27 C26 C25 120.0(4) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 119.1(4) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C29 C28 C27 117.1(4) . . ? C29 C28 C34 120.8(4) . . ? C27 C28 C34 122.1(4) . . ? N1 C29 C28 124.5(4) . . ? N1 C29 H29 117.7 . . ? C28 C29 H29 117.7 . . ? O6 C31 H31A 109.5 . . ? O6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O1 C32 H32A 109.5 . . ? O1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C34 H34A 109.5 . . ? C28 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C28 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? 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 O10 Sb2 O1 C32 32.5(3) . . . . ? O9 Sb2 O1 C32 126.8(3) 3_665 . . . ? O2 Sb2 O1 C32 155.2(5) . . . . ? O3 Sb2 O1 C32 -145.2(3) . . . . ? C1 Sb2 O1 C32 -58.0(3) . . . . ? O10 Sb2 O1 Co1 -104.28(11) . . . 3_665 ? O9 Sb2 O1 Co1 -10.07(10) 3_665 . . 3_665 ? O2 Sb2 O1 Co1 18.4(6) . . . 3_665 ? O3 Sb2 O1 Co1 77.96(10) . . . 3_665 ? C1 Sb2 O1 Co1 165.22(12) . . . 3_665 ? O10 Sb2 O2 P1 91.1(2) . . . . ? O9 Sb2 O2 P1 -3.9(2) 3_665 . . . ? O1 Sb2 O2 P1 -31.9(7) . . . . ? O3 Sb2 O2 P1 -91.5(2) . . . . ? C1 Sb2 O2 P1 -178.9(2) . . . . ? O10 Sb2 O3 P2 163.7(17) . . . 3_665 ? O9 Sb2 O3 P2 17.17(16) 3_665 . . 3_665 ? O2 Sb2 O3 P2 107.62(17) . . . 3_665 ? O1 Sb2 O3 P2 -63.17(17) . . . 3_665 ? C1 Sb2 O3 P2 -159.69(18) . . . 3_665 ? O10 Sb1 O4 P1 95.3(2) . . . 3_665 ? O9 Sb1 O4 P1 1.3(2) . . . 3_665 ? O6 Sb1 O4 P1 -16.2(7) . . . 3_665 ? O5 Sb1 O4 P1 -85.7(2) . . . 3_665 ? C7 Sb1 O4 P1 -173.4(3) . . . 3_665 ? O10 Sb1 O5 P2 161(4) . . . . ? O9 Sb1 O5 P2 20.15(15) . . . . ? O4 Sb1 O5 P2 110.65(16) . . . . ? O6 Sb1 O5 P2 -59.73(16) . . . . ? C7 Sb1 O5 P2 -159.23(17) . . . . ? O10 Sb1 O6 C31 121.3(3) . . . . ? O9 Sb1 O6 C31 -145.0(3) . . . . ? O4 Sb1 O6 C31 -127.2(5) . . . . ? O5 Sb1 O6 C31 -57.9(3) . . . . ? C7 Sb1 O6 C31 29.6(3) . . . . ? O10 Sb1 O6 Co1 -104.14(11) . . . . ? O9 Sb1 O6 Co1 -10.46(10) . . . . ? O4 Sb1 O6 Co1 7.4(6) . . . . ? O5 Sb1 O6 Co1 76.70(10) . . . . ? C7 Sb1 O6 Co1 164.21(13) . . . . ? O7 Co1 O6 C31 -124.3(3) . . . . ? N1 Co1 O6 C31 -32.2(3) . . . . ? O8 Co1 O6 C31 51.6(3) . . . . ? O9 Co1 O6 C31 143.7(3) . . . . ? O1 Co1 O6 C31 121.0(3) 3_665 . . . ? O7 Co1 O6 Sb1 101.82(11) . . . . ? N1 Co1 O6 Sb1 -166.01(12) . . . . ? O8 Co1 O6 Sb1 -82.26(11) . . . . ? O9 Co1 O6 Sb1 9.89(10) . . . . ? O1 Co1 O6 Sb1 -12.9(2) 3_665 . . . ? N1 Co1 O7 P1 171.7(2) . . . . ? O8 Co1 O7 P1 -160.2(13) . . . . ? O9 Co1 O7 P1 -2.7(2) . . . . ? O1 Co1 O7 P1 71.1(2) 3_665 . . . ? O6 Co1 O7 P1 -76.0(2) . . . . ? O7 Co1 O8 P2 159.7(13) . . . . ? N1 Co1 O8 P2 -172.21(17) . . . . ? O9 Co1 O8 P2 2.14(16) . . . . ? O1 Co1 O8 P2 -71.19(16) 3_665 . . . ? O6 Co1 O8 P2 75.00(16) . . . . ? O10 Sb1 O9 Sb2 -130.63(17) . . . 3_665 ? O4 Sb1 O9 Sb2 -38.89(17) . . . 3_665 ? O6 Sb1 O9 Sb2 137.97(18) . . . 3_665 ? O5 Sb1 O9 Sb2 48.54(17) . . . 3_665 ? C7 Sb1 O9 Sb2 55.2(13) . . . 3_665 ? O10 Sb1 O9 Co1 102.01(11) . . . . ? O4 Sb1 O9 Co1 -166.25(11) . . . . ? O6 Sb1 O9 Co1 10.61(11) . . . . ? O5 Sb1 O9 Co1 -78.82(11) . . . . ? C7 Sb1 O9 Co1 -72.1(13) . . . . ? O7 Co1 O9 Sb1 -106.24(11) . . . . ? N1 Co1 O9 Sb1 133.5(10) . . . . ? O8 Co1 O9 Sb1 72.20(11) . . . . ? O1 Co1 O9 Sb1 155.99(13) 3_665 . . . ? O6 Co1 O9 Sb1 -10.20(10) . . . . ? O7 Co1 O9 Sb2 107.56(11) . . . 3_665 ? N1 Co1 O9 Sb2 -12.7(10) . . . 3_665 ? O8 Co1 O9 Sb2 -74.00(11) . . . 3_665 ? O1 Co1 O9 Sb2 9.79(10) 3_665 . . 3_665 ? O6 Co1 O9 Sb2 -156.40(13) . . . 3_665 ? O9 Sb1 O10 Sb2 21.3(2) . . . . ? O4 Sb1 O10 Sb2 -69.2(2) . . . . ? O6 Sb1 O10 Sb2 101.2(2) . . . . ? O5 Sb1 O10 Sb2 -119(4) . . . . ? C7 Sb1 O10 Sb2 -159.3(2) . . . . ? O9 Sb2 O10 Sb1 13.2(2) 3_665 . . . ? O2 Sb2 O10 Sb1 -77.2(2) . . . . ? O1 Sb2 O10 Sb1 93.8(2) . . . . ? O3 Sb2 O10 Sb1 -133.1(17) . . . . ? C1 Sb2 O10 Sb1 -169.7(2) . . . . ? Co1 O7 P1 O4 -60.7(3) . . . 3_665 ? Co1 O7 P1 O2 66.2(3) . . . . ? Co1 O7 P1 C13 -178.3(2) . . . . ? Sb2 O2 P1 O7 -100.4(2) . . . . ? Sb2 O2 P1 O4 27.5(3) . . . 3_665 ? Sb2 O2 P1 C13 139.3(2) . . . . ? Co1 O8 P2 O3 60.23(19) . . . 3_665 ? Co1 O8 P2 O5 -63.08(18) . . . . ? Co1 O8 P2 C19 -179.68(15) . . . . ? Sb1 O5 P2 O8 52.93(18) . . . . ? Sb1 O5 P2 O3 -73.13(18) . . . 3_665 ? Sb1 O5 P2 C19 172.97(16) . . . . ? O7 Co1 N1 C25 -153.1(3) . . . . ? O8 Co1 N1 C25 28.8(3) . . . . ? O9 Co1 N1 C25 -32.6(11) . . . . ? O1 Co1 N1 C25 -54.5(3) 3_665 . . . ? O6 Co1 N1 C25 109.7(3) . . . . ? O7 Co1 N1 C29 17.7(3) . . . . ? O8 Co1 N1 C29 -160.4(3) . . . . ? O9 Co1 N1 C29 138.2(9) . . . . ? O1 Co1 N1 C29 116.3(3) 3_665 . . . ? O6 Co1 N1 C29 -79.5(3) . . . . ? O10 Sb2 C1 C6 -137.3(3) . . . . ? O9 Sb2 C1 C6 11.4(15) 3_665 . . . ? O2 Sb2 C1 C6 131.6(3) . . . . ? O1 Sb2 C1 C6 -42.5(3) . . . . ? O3 Sb2 C1 C6 44.5(3) . . . . ? O10 Sb2 C1 C2 38.9(3) . . . . ? O9 Sb2 C1 C2 -172.4(11) 3_665 . . . ? O2 Sb2 C1 C2 -52.2(3) . . . . ? O1 Sb2 C1 C2 133.7(3) . . . . ? O3 Sb2 C1 C2 -139.3(3) . . . . ? C6 C1 C2 C3 -0.1(6) . . . . ? Sb2 C1 C2 C3 -176.4(3) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? C2 C3 C4 C5 -0.3(6) . . . . ? C2 C3 C4 Cl1 179.1(3) . . . . ? C3 C4 C5 C6 -0.5(6) . . . . ? Cl1 C4 C5 C6 -179.8(3) . . . . ? C4 C5 C6 C1 0.9(6) . . . . ? C2 C1 C6 C5 -0.6(6) . . . . ? Sb2 C1 C6 C5 175.6(3) . . . . ? O10 Sb1 C7 C12 157.3(3) . . . . ? O9 Sb1 C7 C12 -28.5(14) . . . . ? O4 Sb1 C7 C12 65.6(3) . . . . ? O6 Sb1 C7 C12 -110.4(3) . . . . ? O5 Sb1 C7 C12 -21.8(3) . . . . ? O10 Sb1 C7 C8 -18.1(3) . . . . ? O9 Sb1 C7 C8 156.1(11) . . . . ? O4 Sb1 C7 C8 -109.8(3) . . . . ? O6 Sb1 C7 C8 74.2(3) . . . . ? O5 Sb1 C7 C8 162.7(3) . . . . ? C12 C7 C8 C9 -0.8(6) . . . . ? Sb1 C7 C8 C9 174.8(3) . . . . ? C7 C8 C9 C10 0.2(6) . . . . ? C8 C9 C10 C11 0.9(6) . . . . ? C8 C9 C10 Cl2 -176.7(3) . . . . ? C9 C10 C11 C12 -1.2(6) . . . . ? Cl2 C10 C11 C12 176.3(3) . . . . ? C8 C7 C12 C11 0.4(6) . . . . ? Sb1 C7 C12 C11 -175.0(3) . . . . ? C10 C11 C12 C7 0.6(6) . . . . ? O7 P1 C13 C14 -12.6(4) . . . . ? O4 P1 C13 C14 -135.0(3) 3_665 . . . ? O2 P1 C13 C14 108.9(3) . . . . ? O7 P1 C13 C18 170.5(3) . . . . ? O4 P1 C13 C18 48.2(3) 3_665 . . . ? O2 P1 C13 C18 -67.9(3) . . . . ? C18 C13 C14 C15 4.2(6) . . . . ? P1 C13 C14 C15 -172.6(3) . . . . ? C13 C14 C15 C16 -2.1(6) . . . . ? C14 C15 C16 C17 -1.9(8) . . . . ? C15 C16 C17 C18 3.7(9) . . . . ? C16 C17 C18 C13 -1.5(8) . . . . ? C14 C13 C18 C17 -2.4(7) . . . . ? P1 C13 C18 C17 174.6(4) . . . . ? O8 P2 C19 C20 -165.1(3) . . . . ? O3 P2 C19 C20 -41.3(4) 3_665 . . . ? O5 P2 C19 C20 73.4(4) . . . . ? O8 P2 C19 C24 18.3(4) . . . . ? O3 P2 C19 C24 142.1(3) 3_665 . . . ? O5 P2 C19 C24 -103.1(3) . . . . ? C24 C19 C20 C21 -0.9(6) . . . . ? P2 C19 C20 C21 -177.4(3) . . . . ? C19 C20 C21 C22 1.4(7) . . . . ? C20 C21 C22 C23 -1.2(7) . . . . ? C21 C22 C23 C24 0.4(7) . . . . ? C22 C23 C24 C19 0.2(7) . . . . ? C20 C19 C24 C23 0.1(6) . . . . ? P2 C19 C24 C23 176.7(3) . . . . ? C29 N1 C25 C26 0.8(6) . . . . ? Co1 N1 C25 C26 172.0(3) . . . . ? N1 C25 C26 C27 -0.2(7) . . . . ? C25 C26 C27 C28 -0.2(7) . . . . ? C26 C27 C28 C29 0.0(6) . . . . ? C26 C27 C28 C34 -178.6(4) . . . . ? C25 N1 C29 C28 -1.0(6) . . . . ? Co1 N1 C29 C28 -172.0(3) . . . . ? C27 C28 C29 N1 0.6(6) . . . . ? C34 C28 C29 N1 179.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.812 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.119 # Attachment '- 5.cif' data_orepw786 _database_code_depnum_ccdc_archive 'CCDC 778675' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H62 Cl4 Co2 N2 O20 P4 Sb4' _chemical_formula_weight 2049.70 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 12.282(5) _cell_length_b 11.946(5) _cell_length_c 24.980(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 100.970(5) _cell_angle_gamma 90.000(5) _cell_volume 3598(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9679 _cell_measurement_theta_min 2.7260 _cell_measurement_theta_max 28.5619 _exptl_crystal_description needles _exptl_crystal_colour pink _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2012 _exptl_absorpt_coefficient_mu 2.241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4004 _exptl_absorpt_correction_T_max 0.8070 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17873 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7297 _reflns_number_gt 5715 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0277P)^2^+1.9832P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7297 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.001 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 Sb1 Sb 0.432030(18) 0.324329(18) 0.044397(8) 0.01202(6) Uani 1 1 d . . . Sb2 Sb 0.537963(18) 0.600705(18) 0.093746(8) 0.01187(6) Uani 1 1 d . . . Co1 Co 0.69009(4) 0.37797(4) 0.093256(18) 0.01471(10) Uani 1 1 d . . . P2 P 0.51629(7) 0.38984(7) 0.16842(3) 0.01461(18) Uani 1 1 d . . . P1 P 0.27736(7) 0.55471(7) 0.03169(3) 0.01326(18) Uani 1 1 d . . . Cl2 Cl 0.52497(9) 1.08702(8) 0.21988(4) 0.0310(2) Uani 1 1 d . . . Cl1 Cl 0.12323(8) -0.13253(8) 0.02137(4) 0.0319(2) Uani 1 1 d . . . O1 O 0.57304(18) 0.68101(18) 0.03293(8) 0.0136(5) Uani 1 1 d . . . O2 O 0.37465(18) 0.61962(18) 0.06606(9) 0.0137(5) Uani 1 1 d . . . O6 O 0.30148(18) 0.42784(18) 0.03320(9) 0.0151(5) Uani 1 1 d . . . O4 O 0.69677(18) 0.55367(19) 0.11981(9) 0.0153(5) Uani 1 1 d . . . O3 O 0.49763(18) 0.51816(18) 0.15996(8) 0.0136(5) Uani 1 1 d . . . C12 C 0.6059(3) 0.8403(3) 0.12744(15) 0.0274(9) Uani 1 1 d . . . H12 H 0.6533 0.8306 0.1019 0.033 Uiso 1 1 calc R . . C6 C 0.2404(3) 0.1697(3) -0.00388(14) 0.0215(8) Uani 1 1 d . . . H6 H 0.2242 0.2277 -0.0302 0.026 Uiso 1 1 calc R . . O7 O 0.75599(18) 0.40085(18) 0.02511(9) 0.0154(5) Uani 1 1 d . . . C11 C 0.6030(3) 0.9430(3) 0.15335(16) 0.0294(9) Uani 1 1 d . . . H11 H 0.6484 1.0032 0.1459 0.035 Uiso 1 1 calc R . . O5 O 0.53408(18) 0.45396(17) 0.05766(8) 0.0126(5) Uani 1 1 d . . . O9 O 0.57787(18) 0.24369(19) 0.06380(9) 0.0160(5) Uani 1 1 d . . . O10 O 0.42866(18) 0.32747(18) 0.12624(8) 0.0148(5) Uani 1 1 d . . . C20 C 0.3757(3) 0.3338(3) 0.23879(16) 0.0297(9) Uani 1 1 d . . . H20 H 0.3186 0.3292 0.2073 0.036 Uiso 1 1 calc R . . C7 C 0.5402(3) 0.7517(3) 0.13853(13) 0.0153(7) Uani 1 1 d . . . C21 C 0.3511(4) 0.3133(4) 0.28982(17) 0.0411(11) Uani 1 1 d . . . H21 H 0.2777 0.2938 0.2932 0.049 Uiso 1 1 calc R . . C19 C 0.4828(3) 0.3609(3) 0.23338(13) 0.0172(7) Uani 1 1 d . . . C10 C 0.5336(3) 0.9560(3) 0.18992(13) 0.0213(8) Uani 1 1 d . . . C18 C 0.1953(3) 0.5390(3) 0.12521(16) 0.0304(9) Uani 1 1 d . . . H18 H 0.2700 0.5223 0.1412 0.036 Uiso 1 1 calc R . . C1 C 0.3291(3) 0.1820(3) 0.03951(13) 0.0135(7) Uani 1 1 d . . . C22 C 0.4337(4) 0.3211(4) 0.33596(16) 0.0430(12) Uani 1 1 d . . . H22 H 0.4166 0.3080 0.3709 0.052 Uiso 1 1 calc R . . C4 C 0.2010(3) -0.0098(3) 0.02886(14) 0.0201(8) Uani 1 1 d . . . C16 C 0.0069(4) 0.5590(4) 0.1332(2) 0.0461(12) Uani 1 1 d . . . H16 H -0.0489 0.5551 0.1547 0.055 Uiso 1 1 calc R . . C8 C 0.4705(3) 0.7684(3) 0.17514(15) 0.0271(9) Uani 1 1 d . . . H8 H 0.4240 0.7091 0.1826 0.032 Uiso 1 1 calc R . . C2 C 0.3520(3) 0.0965(3) 0.07752(14) 0.0204(8) Uani 1 1 d . . . H2 H 0.4119 0.1045 0.1076 0.024 Uiso 1 1 calc R . . C13 C 0.1681(3) 0.5661(3) 0.06961(15) 0.0197(8) Uani 1 1 d . . . C3 C 0.2889(3) -0.0002(3) 0.07233(14) 0.0236(8) Uani 1 1 d . . . H3 H 0.3056 -0.0590 0.0982 0.028 Uiso 1 1 calc R . . C17 C 0.1150(4) 0.5363(4) 0.15690(19) 0.0444(12) Uani 1 1 d . . . H17 H 0.1340 0.5189 0.1946 0.053 Uiso 1 1 calc R . . C15 C -0.0224(3) 0.5875(3) 0.07886(19) 0.0359(11) Uani 1 1 d . . . H15 H -0.0974 0.6040 0.0633 0.043 Uiso 1 1 calc R . . O8 O 0.63271(19) 0.35566(19) 0.16691(9) 0.0178(5) Uani 1 1 d . . . N1 N 0.8354(2) 0.2917(2) 0.12909(12) 0.0195(6) Uani 1 1 d . . . C32 C 0.6062(3) 0.1572(3) 0.02893(14) 0.0210(8) Uani 1 1 d . . . H32A H 0.5460 0.1022 0.0216 0.031 Uiso 1 1 calc R . . H32B H 0.6746 0.1200 0.0469 0.031 Uiso 1 1 calc R . . H32C H 0.6175 0.1902 -0.0055 0.031 Uiso 1 1 calc R . . C31 C 0.7482(3) 0.5828(3) 0.17469(13) 0.0210(8) Uani 1 1 d . . . H31A H 0.7951 0.6490 0.1741 0.032 Uiso 1 1 calc R . . H31B H 0.7938 0.5201 0.1914 0.032 Uiso 1 1 calc R . . H31C H 0.6908 0.5992 0.1959 0.032 Uiso 1 1 calc R . . C26 C 0.9342(3) 0.1674(3) 0.19624(17) 0.0347(10) Uani 1 1 d . . . H26 H 0.9333 0.1221 0.2274 0.042 Uiso 1 1 calc R . . C29 C 0.9270(3) 0.2953(4) 0.10752(17) 0.0339(10) Uani 1 1 d . . . H29 H 0.9249 0.3393 0.0757 0.041 Uiso 1 1 calc R . . C25 C 0.8408(3) 0.2262(3) 0.17298(15) 0.0289(9) Uani 1 1 d . . . H25 H 0.7768 0.2200 0.1889 0.035 Uiso 1 1 calc R . . C27 C 1.0295(3) 0.1739(3) 0.17436(16) 0.0300(9) Uani 1 1 d . . . C24 C 0.5659(3) 0.3669(3) 0.28015(14) 0.0276(9) Uani 1 1 d . . . H24 H 0.6399 0.3840 0.2770 0.033 Uiso 1 1 calc R . . C9 C 0.4674(3) 0.8704(3) 0.20125(15) 0.0300(9) Uani 1 1 d . . . H9 H 0.4199 0.8807 0.2267 0.036 Uiso 1 1 calc R . . C5 C 0.1755(3) 0.0740(3) -0.00913(15) 0.0238(8) Uani 1 1 d . . . H5 H 0.1143 0.0664 -0.0385 0.029 Uiso 1 1 calc R . . C14 C 0.0600(3) 0.5917(3) 0.04676(17) 0.0268(9) Uani 1 1 d . . . H14 H 0.0411 0.6121 0.0094 0.032 Uiso 1 1 calc R . . C23 C 0.5404(4) 0.3479(4) 0.33118(16) 0.0403(11) Uani 1 1 d . . . H23 H 0.5968 0.3534 0.3629 0.048 Uiso 1 1 calc R . . C28 C 1.0240(3) 0.2395(4) 0.12829(17) 0.0372(10) Uani 1 1 d . . . H28 H 1.0864 0.2461 0.1112 0.045 Uiso 1 1 calc R . . C30 C 1.1343(4) 0.1133(4) 0.1991(2) 0.0418(11) Uani 1 1 d . . . H30A H 1.1461 0.0507 0.1755 0.063 Uiso 1 1 calc R . . H30B H 1.1279 0.0847 0.2351 0.063 Uiso 1 1 calc R . . H30C H 1.1972 0.1650 0.2028 0.063 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 Sb1 0.01483(11) 0.01098(11) 0.01058(10) -0.00105(9) 0.00325(8) -0.00096(9) Sb2 0.01444(11) 0.01133(11) 0.01003(10) -0.00164(9) 0.00284(8) -0.00089(9) Co1 0.0154(2) 0.0143(2) 0.0140(2) -0.00044(19) 0.00159(18) 0.00085(18) P2 0.0194(4) 0.0139(4) 0.0104(4) -0.0001(4) 0.0024(3) -0.0007(4) P1 0.0125(4) 0.0126(4) 0.0151(4) -0.0019(4) 0.0035(4) 0.0003(3) Cl2 0.0518(6) 0.0176(5) 0.0200(4) -0.0069(4) -0.0026(4) 0.0072(4) Cl1 0.0383(6) 0.0248(5) 0.0348(5) -0.0053(4) 0.0123(5) -0.0172(4) O1 0.0188(12) 0.0142(11) 0.0085(10) -0.0013(9) 0.0041(9) -0.0017(10) O2 0.0144(12) 0.0141(12) 0.0132(11) -0.0020(10) 0.0044(9) 0.0018(9) O6 0.0155(12) 0.0145(12) 0.0159(11) -0.0009(10) 0.0043(10) -0.0009(9) O4 0.0140(12) 0.0209(13) 0.0106(11) -0.0012(10) 0.0015(9) 0.0003(10) O3 0.0195(12) 0.0120(12) 0.0101(10) -0.0012(9) 0.0048(10) -0.0008(9) C12 0.037(2) 0.024(2) 0.0264(19) -0.0033(17) 0.0178(18) -0.0037(17) C6 0.0236(19) 0.0194(19) 0.0204(17) 0.0046(16) 0.0018(15) -0.0013(15) O7 0.0129(11) 0.0171(12) 0.0157(11) 0.0009(10) 0.0015(10) 0.0006(10) C11 0.041(2) 0.0170(19) 0.032(2) -0.0062(17) 0.0118(19) -0.0075(17) O5 0.0158(12) 0.0100(11) 0.0119(11) -0.0024(9) 0.0026(10) -0.0005(9) O9 0.0163(12) 0.0149(12) 0.0166(11) -0.0023(10) 0.0028(10) 0.0026(10) O10 0.0199(12) 0.0152(12) 0.0095(10) -0.0013(10) 0.0038(10) -0.0019(10) C20 0.039(2) 0.030(2) 0.0219(19) 0.0061(17) 0.0111(18) 0.0046(19) C7 0.0200(18) 0.0127(17) 0.0119(15) 0.0000(14) -0.0001(14) 0.0011(14) C21 0.051(3) 0.043(3) 0.035(2) 0.009(2) 0.023(2) 0.007(2) C19 0.030(2) 0.0094(16) 0.0128(16) 0.0006(13) 0.0053(15) 0.0027(14) C10 0.033(2) 0.0141(18) 0.0138(16) -0.0049(15) -0.0041(16) 0.0077(16) C18 0.033(2) 0.034(2) 0.028(2) 0.0018(19) 0.0140(19) 0.0050(18) C1 0.0159(17) 0.0140(16) 0.0110(15) -0.0013(14) 0.0038(13) -0.0001(14) C22 0.069(3) 0.047(3) 0.019(2) 0.011(2) 0.023(2) 0.024(3) C4 0.0211(19) 0.0165(18) 0.0252(18) -0.0028(16) 0.0108(16) -0.0074(15) C16 0.040(3) 0.055(3) 0.053(3) -0.012(3) 0.033(2) -0.004(2) C8 0.035(2) 0.019(2) 0.030(2) -0.0034(17) 0.0132(18) -0.0053(17) C2 0.0236(19) 0.0207(19) 0.0147(16) 0.0005(15) -0.0013(15) -0.0042(16) C13 0.0201(19) 0.0110(17) 0.0292(19) -0.0065(15) 0.0078(16) -0.0044(14) C3 0.034(2) 0.0155(18) 0.0212(18) 0.0072(15) 0.0038(17) -0.0028(16) C17 0.052(3) 0.052(3) 0.036(2) 0.003(2) 0.027(2) 0.003(2) C15 0.020(2) 0.032(2) 0.058(3) -0.021(2) 0.013(2) -0.0054(17) O8 0.0205(13) 0.0166(12) 0.0152(12) -0.0004(10) 0.0009(10) 0.0022(10) N1 0.0221(16) 0.0165(15) 0.0187(15) -0.0006(13) 0.0012(13) 0.0017(12) C32 0.0234(19) 0.0155(18) 0.0239(18) -0.0052(15) 0.0041(16) 0.0020(15) C31 0.0188(18) 0.028(2) 0.0164(17) -0.0043(16) 0.0026(15) 0.0018(15) C26 0.036(2) 0.033(2) 0.033(2) 0.012(2) 0.0017(19) 0.0035(19) C29 0.023(2) 0.045(3) 0.033(2) 0.012(2) 0.0029(18) 0.0079(19) C25 0.027(2) 0.032(2) 0.028(2) 0.0080(18) 0.0052(18) 0.0049(18) C27 0.025(2) 0.029(2) 0.033(2) -0.0039(19) -0.0024(18) 0.0042(18) C24 0.037(2) 0.027(2) 0.0176(18) -0.0019(16) 0.0021(17) 0.0086(18) C9 0.045(3) 0.024(2) 0.0243(19) -0.0075(17) 0.0152(19) 0.0037(18) C5 0.0198(19) 0.028(2) 0.0217(18) -0.0003(16) -0.0003(16) -0.0061(16) C14 0.023(2) 0.022(2) 0.036(2) -0.0129(18) 0.0059(17) -0.0036(16) C23 0.058(3) 0.047(3) 0.0151(19) 0.0026(19) 0.003(2) 0.016(2) C28 0.028(2) 0.046(3) 0.037(2) 0.008(2) 0.0046(19) 0.010(2) C30 0.034(2) 0.031(2) 0.058(3) 0.011(2) 0.002(2) 0.008(2) _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 Sb1 O1 1.922(2) 3_665 ? Sb1 O5 1.980(2) . ? Sb1 O6 2.002(2) . ? Sb1 O9 2.010(2) . ? Sb1 O10 2.053(2) . ? Sb1 C1 2.108(3) . ? Sb2 O1 1.914(2) . ? Sb2 O5 1.968(2) . ? Sb2 O2 2.006(2) . ? Sb2 O4 2.015(2) . ? Sb2 O3 2.065(2) . ? Sb2 C7 2.120(3) . ? Co1 O7 2.038(2) . ? Co1 N1 2.108(3) . ? Co1 O8 2.109(2) . ? Co1 O9 2.151(2) . ? Co1 O5 2.154(2) . ? Co1 O4 2.198(2) . ? P2 O8 1.494(3) . ? P2 O10 1.547(2) . ? P2 O3 1.558(2) . ? P2 C19 1.782(3) . ? P1 O7 1.497(2) 3_665 ? P1 O2 1.541(2) . ? P1 O6 1.543(2) . ? P1 C13 1.789(4) . ? Cl2 C10 1.746(3) . ? Cl1 C4 1.740(3) . ? O1 Sb1 1.922(2) 3_665 ? O4 C31 1.439(4) . ? C12 C7 1.391(5) . ? C12 C11 1.391(5) . ? C12 H12 0.9500 . ? C6 C5 1.386(5) . ? C6 C1 1.390(5) . ? C6 H6 0.9500 . ? O7 P1 1.497(2) 3_665 ? C11 C10 1.372(5) . ? C11 H11 0.9500 . ? O9 C32 1.437(4) . ? C20 C21 1.386(5) . ? C20 C19 1.386(5) . ? C20 H20 0.9500 . ? C7 C8 1.381(5) . ? C21 C22 1.386(6) . ? C21 H21 0.9500 . ? C19 C24 1.399(5) . ? C10 C9 1.369(5) . ? C18 C17 1.378(5) . ? C18 C13 1.403(5) . ? C18 H18 0.9500 . ? C1 C2 1.386(5) . ? C22 C23 1.377(7) . ? C22 H22 0.9500 . ? C4 C5 1.374(5) . ? C4 C3 1.382(5) . ? C16 C17 1.373(6) . ? C16 C15 1.379(6) . ? C16 H16 0.9500 . ? C8 C9 1.385(5) . ? C8 H8 0.9500 . ? C2 C3 1.384(5) . ? C2 H2 0.9500 . ? C13 C14 1.375(5) . ? C3 H3 0.9500 . ? C17 H17 0.9500 . ? C15 C14 1.407(5) . ? C15 H15 0.9500 . ? N1 C29 1.336(5) . ? N1 C25 1.338(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C26 C25 1.376(5) . ? C26 C27 1.385(6) . ? C26 H26 0.9500 . ? C29 C28 1.377(5) . ? C29 H29 0.9500 . ? C25 H25 0.9500 . ? C27 C28 1.383(6) . ? C27 C30 1.503(5) . ? C24 C23 1.388(5) . ? C24 H24 0.9500 . ? C9 H9 0.9500 . ? C5 H5 0.9500 . ? C14 H14 0.9500 . ? C23 H23 0.9500 . ? C28 H28 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 Sb1 O5 95.31(9) 3_665 . ? O1 Sb1 O6 90.46(9) 3_665 . ? O5 Sb1 O6 90.28(9) . . ? O1 Sb1 O9 94.79(9) 3_665 . ? O5 Sb1 O9 80.08(9) . . ? O6 Sb1 O9 169.40(9) . . ? O1 Sb1 O10 176.92(9) 3_665 . ? O5 Sb1 O10 87.20(9) . . ? O6 Sb1 O10 87.74(9) . . ? O9 Sb1 O10 87.40(9) . . ? O1 Sb1 C1 90.61(11) 3_665 . ? O5 Sb1 C1 173.64(10) . . ? O6 Sb1 C1 91.99(11) . . ? O9 Sb1 C1 97.14(11) . . ? O10 Sb1 C1 86.96(10) . . ? O1 Sb2 O5 94.15(9) . . ? O1 Sb2 O2 91.79(9) . . ? O5 Sb2 O2 90.40(9) . . ? O1 Sb2 O4 92.63(9) . . ? O5 Sb2 O4 80.63(9) . . ? O2 Sb2 O4 170.26(9) . . ? O1 Sb2 O3 178.31(9) . . ? O5 Sb2 O3 87.30(9) . . ? O2 Sb2 O3 87.33(9) . . ? O4 Sb2 O3 88.45(9) . . ? O1 Sb2 C7 90.58(11) . . ? O5 Sb2 C7 175.25(11) . . ? O2 Sb2 C7 89.87(11) . . ? O4 Sb2 C7 98.76(11) . . ? O3 Sb2 C7 87.97(11) . . ? O7 Co1 N1 88.93(10) . . ? O7 Co1 O8 176.15(9) . . ? N1 Co1 O8 87.95(10) . . ? O7 Co1 O9 98.33(9) . . ? N1 Co1 O9 102.49(10) . . ? O8 Co1 O9 84.57(9) . . ? O7 Co1 O5 93.57(9) . . ? N1 Co1 O5 175.30(10) . . ? O8 Co1 O5 89.70(9) . . ? O9 Co1 O5 73.22(9) . . ? O7 Co1 O4 97.24(9) . . ? N1 Co1 O4 111.04(10) . . ? O8 Co1 O4 81.77(9) . . ? O9 Co1 O4 143.12(9) . . ? O5 Co1 O4 72.62(8) . . ? O8 P2 O10 113.35(13) . . ? O8 P2 O3 112.46(13) . . ? O10 P2 O3 108.43(12) . . ? O8 P2 C19 110.97(15) . . ? O10 P2 C19 105.99(15) . . ? O3 P2 C19 105.12(14) . . ? O7 P1 O2 113.13(13) 3_665 . ? O7 P1 O6 112.83(13) 3_665 . ? O2 P1 O6 110.83(13) . . ? O7 P1 C13 112.16(15) 3_665 . ? O2 P1 C13 104.30(14) . . ? O6 P1 C13 102.81(15) . . ? Sb2 O1 Sb1 144.30(12) . 3_665 ? P1 O2 Sb2 138.90(13) . . ? P1 O6 Sb1 139.02(14) . . ? C31 O4 Sb2 117.6(2) . . ? C31 O4 Co1 120.2(2) . . ? Sb2 O4 Co1 100.98(9) . . ? P2 O3 Sb2 121.79(12) . . ? C7 C12 C11 120.8(3) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C5 C6 C1 120.8(3) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? P1 O7 Co1 139.35(14) 3_665 . ? C10 C11 C12 118.9(4) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? Sb2 O5 Sb1 137.12(12) . . ? Sb2 O5 Co1 104.14(9) . . ? Sb1 O5 Co1 102.98(10) . . ? C32 O9 Sb1 120.42(19) . . ? C32 O9 Co1 122.0(2) . . ? Sb1 O9 Co1 102.04(10) . . ? P2 O10 Sb1 122.95(13) . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C8 C7 C12 118.6(3) . . ? C8 C7 Sb2 121.7(3) . . ? C12 C7 Sb2 119.5(3) . . ? C22 C21 C20 120.0(4) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C20 C19 C24 119.1(3) . . ? C20 C19 P2 121.5(3) . . ? C24 C19 P2 119.5(3) . . ? C9 C10 C11 121.4(3) . . ? C9 C10 Cl2 119.6(3) . . ? C11 C10 Cl2 118.9(3) . . ? C17 C18 C13 120.8(4) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? C2 C1 C6 118.9(3) . . ? C2 C1 Sb1 120.9(2) . . ? C6 C1 Sb1 120.1(2) . . ? C23 C22 C21 120.1(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C5 C4 C3 121.6(3) . . ? C5 C4 Cl1 119.4(3) . . ? C3 C4 Cl1 119.0(3) . . ? C17 C16 C15 121.6(4) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C7 C8 C9 121.0(4) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C3 C2 C1 120.9(3) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C14 C13 C18 119.4(4) . . ? C14 C13 P1 124.0(3) . . ? C18 C13 P1 116.4(3) . . ? C4 C3 C2 118.8(3) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C16 C17 C18 119.1(4) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C16 C15 C14 119.2(4) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? P2 O8 Co1 117.89(13) . . ? C29 N1 C25 115.8(3) . . ? C29 N1 Co1 121.5(3) . . ? C25 N1 Co1 122.7(3) . . ? O9 C32 H32A 109.5 . . ? O9 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O9 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O4 C31 H31A 109.5 . . ? O4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C25 C26 C27 120.3(4) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? N1 C29 C28 124.5(4) . . ? N1 C29 H29 117.8 . . ? C28 C29 H29 117.8 . . ? N1 C25 C26 123.5(4) . . ? N1 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C28 C27 C26 116.7(4) . . ? C28 C27 C30 121.2(4) . . ? C26 C27 C30 122.2(4) . . ? C23 C24 C19 120.2(4) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? C10 C9 C8 119.3(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C22 C23 C24 120.1(4) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C29 C28 C27 119.3(4) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 O5 Sb2 O1 Sb1 21.3(2) . . . 3_665 ? O2 Sb2 O1 Sb1 -69.2(2) . . . 3_665 ? O4 Sb2 O1 Sb1 102.1(2) . . . 3_665 ? O3 Sb2 O1 Sb1 -128(3) . . . 3_665 ? C7 Sb2 O1 Sb1 -159.1(2) . . . 3_665 ? O7 P1 O2 Sb2 -104.0(2) 3_665 . . . ? O6 P1 O2 Sb2 23.9(2) . . . . ? C13 P1 O2 Sb2 133.9(2) . . . . ? O1 Sb2 O2 P1 94.7(2) . . . . ? O5 Sb2 O2 P1 0.6(2) . . . . ? O4 Sb2 O2 P1 -22.2(7) . . . . ? O3 Sb2 O2 P1 -86.7(2) . . . . ? C7 Sb2 O2 P1 -174.7(2) . . . . ? O7 P1 O6 Sb1 102.0(2) 3_665 . . . ? O2 P1 O6 Sb1 -26.0(2) . . . . ? C13 P1 O6 Sb1 -136.9(2) . . . . ? O1 Sb1 O6 P1 -92.9(2) 3_665 . . . ? O5 Sb1 O6 P1 2.5(2) . . . . ? O9 Sb1 O6 P1 27.0(6) . . . . ? O10 Sb1 O6 P1 89.7(2) . . . . ? C1 Sb1 O6 P1 176.5(2) . . . . ? O1 Sb2 O4 C31 123.6(2) . . . . ? O5 Sb2 O4 C31 -142.7(2) . . . . ? O2 Sb2 O4 C31 -119.5(5) . . . . ? O3 Sb2 O4 C31 -55.1(2) . . . . ? C7 Sb2 O4 C31 32.6(2) . . . . ? O1 Sb2 O4 Co1 -103.65(10) . . . . ? O5 Sb2 O4 Co1 -9.87(9) . . . . ? O2 Sb2 O4 Co1 13.3(6) . . . . ? O3 Sb2 O4 Co1 77.65(9) . . . . ? C7 Sb2 O4 Co1 165.36(11) . . . . ? O7 Co1 O4 C31 -128.0(2) . . . . ? N1 Co1 O4 C31 -36.3(2) . . . . ? O8 Co1 O4 C31 48.2(2) . . . . ? O9 Co1 O4 C31 117.6(2) . . . . ? O5 Co1 O4 C31 140.5(2) . . . . ? O7 Co1 O4 Sb2 100.81(10) . . . . ? N1 Co1 O4 Sb2 -167.54(10) . . . . ? O8 Co1 O4 Sb2 -82.95(10) . . . . ? O9 Co1 O4 Sb2 -13.56(18) . . . . ? O5 Co1 O4 Sb2 9.32(8) . . . . ? O8 P2 O3 Sb2 53.48(18) . . . . ? O10 P2 O3 Sb2 -72.66(17) . . . . ? C19 P2 O3 Sb2 174.33(15) . . . . ? O1 Sb2 O3 P2 169(3) . . . . ? O5 Sb2 O3 P2 19.71(15) . . . . ? O2 Sb2 O3 P2 110.23(15) . . . . ? O4 Sb2 O3 P2 -60.98(15) . . . . ? C7 Sb2 O3 P2 -159.81(16) . . . . ? N1 Co1 O7 P1 173.3(2) . . . 3_665 ? O8 Co1 O7 P1 -150.5(12) . . . 3_665 ? O9 Co1 O7 P1 70.8(2) . . . 3_665 ? O5 Co1 O7 P1 -2.7(2) . . . 3_665 ? O4 Co1 O7 P1 -75.6(2) . . . 3_665 ? C7 C12 C11 C10 -0.4(6) . . . . ? O1 Sb2 O5 Sb1 -130.09(16) . . . . ? O2 Sb2 O5 Sb1 -38.27(17) . . . . ? O4 Sb2 O5 Sb1 137.92(17) . . . . ? O3 Sb2 O5 Sb1 49.04(16) . . . . ? C7 Sb2 O5 Sb1 54.9(14) . . . . ? O1 Sb2 O5 Co1 102.20(10) . . . . ? O2 Sb2 O5 Co1 -165.98(10) . . . . ? O4 Sb2 O5 Co1 10.21(9) . . . . ? O3 Sb2 O5 Co1 -78.67(10) . . . . ? C7 Sb2 O5 Co1 -72.8(13) . . . . ? O1 Sb1 O5 Sb2 127.83(16) 3_665 . . . ? O6 Sb1 O5 Sb2 37.34(17) . . . . ? O9 Sb1 O5 Sb2 -138.22(17) . . . . ? O10 Sb1 O5 Sb2 -50.38(16) . . . . ? C1 Sb1 O5 Sb2 -73.6(10) . . . . ? O1 Sb1 O5 Co1 -104.10(10) 3_665 . . . ? O6 Sb1 O5 Co1 165.41(9) . . . . ? O9 Sb1 O5 Co1 -10.15(9) . . . . ? O10 Sb1 O5 Co1 77.69(9) . . . . ? C1 Sb1 O5 Co1 54.4(10) . . . . ? O7 Co1 O5 Sb2 -106.15(10) . . . . ? N1 Co1 O5 Sb2 131.8(12) . . . . ? O8 Co1 O5 Sb2 71.80(10) . . . . ? O9 Co1 O5 Sb2 156.23(11) . . . . ? O4 Co1 O5 Sb2 -9.67(9) . . . . ? O7 Co1 O5 Sb1 107.39(10) . . . . ? N1 Co1 O5 Sb1 -14.6(12) . . . . ? O8 Co1 O5 Sb1 -74.67(10) . . . . ? O9 Co1 O5 Sb1 9.76(9) . . . . ? O4 Co1 O5 Sb1 -156.14(11) . . . . ? O1 Sb1 O9 C32 -34.2(2) 3_665 . . . ? O5 Sb1 O9 C32 -128.8(2) . . . . ? O6 Sb1 O9 C32 -153.7(4) . . . . ? O10 Sb1 O9 C32 143.6(2) . . . . ? C1 Sb1 O9 C32 57.0(2) . . . . ? O1 Sb1 O9 Co1 104.70(10) 3_665 . . . ? O5 Sb1 O9 Co1 10.13(9) . . . . ? O6 Sb1 O9 Co1 -14.8(5) . . . . ? O10 Sb1 O9 Co1 -77.48(10) . . . . ? C1 Sb1 O9 Co1 -164.09(11) . . . . ? O7 Co1 O9 C32 37.3(2) . . . . ? N1 Co1 O9 C32 -53.5(2) . . . . ? O8 Co1 O9 C32 -140.2(2) . . . . ? O5 Co1 O9 C32 128.5(2) . . . . ? O4 Co1 O9 C32 151.3(2) . . . . ? O7 Co1 O9 Sb1 -100.81(10) . . . . ? N1 Co1 O9 Sb1 168.44(10) . . . . ? O8 Co1 O9 Sb1 81.75(10) . . . . ? O5 Co1 O9 Sb1 -9.57(8) . . . . ? O4 Co1 O9 Sb1 13.23(18) . . . . ? O8 P2 O10 Sb1 -54.59(19) . . . . ? O3 P2 O10 Sb1 71.04(17) . . . . ? C19 P2 O10 Sb1 -176.54(15) . . . . ? O1 Sb1 O10 P2 -161.9(16) 3_665 . . . ? O5 Sb1 O10 P2 -17.25(15) . . . . ? O6 Sb1 O10 P2 -107.65(16) . . . . ? O9 Sb1 O10 P2 62.94(16) . . . . ? C1 Sb1 O10 P2 160.24(17) . . . . ? C11 C12 C7 C8 1.1(6) . . . . ? C11 C12 C7 Sb2 175.4(3) . . . . ? O1 Sb2 C7 C8 146.5(3) . . . . ? O5 Sb2 C7 C8 -38.5(15) . . . . ? O2 Sb2 C7 C8 54.7(3) . . . . ? O4 Sb2 C7 C8 -120.7(3) . . . . ? O3 Sb2 C7 C8 -32.6(3) . . . . ? O1 Sb2 C7 C12 -27.6(3) . . . . ? O5 Sb2 C7 C12 147.4(12) . . . . ? O2 Sb2 C7 C12 -119.4(3) . . . . ? O4 Sb2 C7 C12 65.2(3) . . . . ? O3 Sb2 C7 C12 153.3(3) . . . . ? C19 C20 C21 C22 0.8(6) . . . . ? C21 C20 C19 C24 0.2(6) . . . . ? C21 C20 C19 P2 -179.0(3) . . . . ? O8 P2 C19 C20 -148.9(3) . . . . ? O10 P2 C19 C20 -25.5(3) . . . . ? O3 P2 C19 C20 89.3(3) . . . . ? O8 P2 C19 C24 31.9(3) . . . . ? O10 P2 C19 C24 155.3(3) . . . . ? O3 P2 C19 C24 -90.0(3) . . . . ? C12 C11 C10 C9 -0.1(6) . . . . ? C12 C11 C10 Cl2 -176.9(3) . . . . ? C5 C6 C1 C2 0.2(5) . . . . ? C5 C6 C1 Sb1 176.7(3) . . . . ? O1 Sb1 C1 C2 136.5(3) 3_665 . . . ? O5 Sb1 C1 C2 -22.2(11) . . . . ? O6 Sb1 C1 C2 -133.1(3) . . . . ? O9 Sb1 C1 C2 41.6(3) . . . . ? O10 Sb1 C1 C2 -45.4(3) . . . . ? O1 Sb1 C1 C6 -39.9(3) 3_665 . . . ? O5 Sb1 C1 C6 161.4(8) . . . . ? O6 Sb1 C1 C6 50.6(3) . . . . ? O9 Sb1 C1 C6 -134.8(3) . . . . ? O10 Sb1 C1 C6 138.2(3) . . . . ? C20 C21 C22 C23 -0.8(7) . . . . ? C12 C7 C8 C9 -1.3(6) . . . . ? Sb2 C7 C8 C9 -175.4(3) . . . . ? C6 C1 C2 C3 0.7(5) . . . . ? Sb1 C1 C2 C3 -175.7(3) . . . . ? C17 C18 C13 C14 0.8(6) . . . . ? C17 C18 C13 P1 -174.7(3) . . . . ? O7 P1 C13 C14 12.0(3) 3_665 . . . ? O2 P1 C13 C14 134.8(3) . . . . ? O6 P1 C13 C14 -109.5(3) . . . . ? O7 P1 C13 C18 -172.7(3) 3_665 . . . ? O2 P1 C13 C18 -50.0(3) . . . . ? O6 P1 C13 C18 65.8(3) . . . . ? C5 C4 C3 C2 0.2(6) . . . . ? Cl1 C4 C3 C2 178.7(3) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C15 C16 C17 C18 -1.8(7) . . . . ? C13 C18 C17 C16 0.9(7) . . . . ? C17 C16 C15 C14 1.0(7) . . . . ? O10 P2 O8 Co1 59.31(18) . . . . ? O3 P2 O8 Co1 -64.13(17) . . . . ? C19 P2 O8 Co1 178.44(14) . . . . ? O7 Co1 O8 P2 150.8(13) . . . . ? N1 Co1 O8 P2 -173.01(16) . . . . ? O9 Co1 O8 P2 -70.26(15) . . . . ? O5 Co1 O8 P2 2.91(15) . . . . ? O4 Co1 O8 P2 75.39(15) . . . . ? O7 Co1 N1 C29 13.3(3) . . . . ? O8 Co1 N1 C29 -164.4(3) . . . . ? O9 Co1 N1 C29 111.6(3) . . . . ? O5 Co1 N1 C29 135.5(11) . . . . ? O4 Co1 N1 C29 -84.1(3) . . . . ? O7 Co1 N1 C25 -163.6(3) . . . . ? O8 Co1 N1 C25 18.7(3) . . . . ? O9 Co1 N1 C25 -65.3(3) . . . . ? O5 Co1 N1 C25 -41.4(13) . . . . ? O4 Co1 N1 C25 99.1(3) . . . . ? C25 N1 C29 C28 -1.8(6) . . . . ? Co1 N1 C29 C28 -178.9(3) . . . . ? C29 N1 C25 C26 1.6(6) . . . . ? Co1 N1 C25 C26 178.6(3) . . . . ? C27 C26 C25 N1 0.0(6) . . . . ? C25 C26 C27 C28 -1.3(6) . . . . ? C25 C26 C27 C30 178.6(4) . . . . ? C20 C19 C24 C23 -1.2(6) . . . . ? P2 C19 C24 C23 178.0(3) . . . . ? C11 C10 C9 C8 -0.1(6) . . . . ? Cl2 C10 C9 C8 176.7(3) . . . . ? C7 C8 C9 C10 0.8(6) . . . . ? C3 C4 C5 C6 0.7(6) . . . . ? Cl1 C4 C5 C6 -177.7(3) . . . . ? C1 C6 C5 C4 -0.9(5) . . . . ? C18 C13 C14 C15 -1.7(5) . . . . ? P1 C13 C14 C15 173.4(3) . . . . ? C16 C15 C14 C13 0.8(6) . . . . ? C21 C22 C23 C24 -0.1(7) . . . . ? C19 C24 C23 C22 1.2(6) . . . . ? N1 C29 C28 C27 0.6(7) . . . . ? C26 C27 C28 C29 1.0(6) . . . . ? C30 C27 C28 C29 -178.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.766 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.107 # Attachment '- 6.cif' data_mono1377 _database_code_depnum_ccdc_archive 'CCDC 778676' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H62 Cl4 Co2 N2 O20 P4 Sb4' _chemical_formula_weight 2121.76 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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)/n 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 15.4040(6) _cell_length_b 12.0434(4) _cell_length_c 20.6638(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.938(4) _cell_angle_gamma 90.00 _cell_volume 3736.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5852 _cell_measurement_theta_min 2.6726 _cell_measurement_theta_max 28.5071 _exptl_crystal_description Needle _exptl_crystal_colour Purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.886 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2084 _exptl_absorpt_coefficient_mu 2.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4784 _exptl_absorpt_correction_T_max 0.7375 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15036 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7571 _reflns_number_gt 4503 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0394P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7571 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _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 Sb1 Sb 0.52737(3) 0.17160(3) 0.43371(2) 0.01473(10) Uani 1 1 d . . . Sb2 Sb 0.36529(2) 0.10159(3) 0.53229(2) 0.01503(10) Uani 1 1 d . . . Co1 Co 0.30046(5) -0.12084(7) 0.44870(4) 0.01668(19) Uani 1 1 d . . . P1 P 0.44716(10) -0.06041(13) 0.35454(8) 0.0146(3) Uani 1 1 d . . . P2 P 0.71595(10) 0.10395(13) 0.40626(8) 0.0176(3) Uani 1 1 d . . . C1 C 0.4844(3) 0.3163(5) 0.3788(3) 0.0138(13) Uani 1 1 d . . . C2 C 0.3992(4) 0.3585(5) 0.3728(3) 0.0205(14) Uani 1 1 d . . . H2 H 0.3580 0.3196 0.3926 0.025 Uiso 1 1 calc R . . C3 C 0.3733(4) 0.4553(5) 0.3389(3) 0.0201(14) Uani 1 1 d . . . H3 H 0.3147 0.4831 0.3354 0.024 Uiso 1 1 calc R . . C4 C 0.4328(4) 0.5124(5) 0.3099(3) 0.0202(14) Uani 1 1 d . . . C5 C 0.5173(4) 0.4719(5) 0.3145(3) 0.0264(16) Uani 1 1 d . . . H5 H 0.5575 0.5102 0.2937 0.032 Uiso 1 1 calc R . . C6 C 0.5437(4) 0.3755(5) 0.3494(3) 0.0234(15) Uani 1 1 d . . . H6 H 0.6028 0.3490 0.3536 0.028 Uiso 1 1 calc R . . C7 C 0.2953(4) 0.2477(5) 0.5451(3) 0.0173(14) Uani 1 1 d . . . C8 C 0.2047(4) 0.2445(5) 0.5429(3) 0.0227(15) Uani 1 1 d . . . H8 H 0.1758 0.1745 0.5408 0.027 Uiso 1 1 calc R . . C9 C 0.1552(4) 0.3403(6) 0.5436(3) 0.0255(15) Uani 1 1 d . . . H9 H 0.0934 0.3362 0.5430 0.031 Uiso 1 1 calc R . . C10 C 0.1969(4) 0.4412(5) 0.5454(3) 0.0242(15) Uani 1 1 d . . . C11 C 0.2869(4) 0.4477(5) 0.5477(3) 0.0268(16) Uani 1 1 d . . . H11 H 0.3152 0.5181 0.5494 0.032 Uiso 1 1 calc R . . C12 C 0.3356(4) 0.3519(5) 0.5476(3) 0.0252(15) Uani 1 1 d . . . H12 H 0.3976 0.3568 0.5493 0.030 Uiso 1 1 calc R . . C13 C 0.4413(4) -0.0702(5) 0.2678(3) 0.0172(14) Uani 1 1 d . . . C14 C 0.5180(4) -0.0429(6) 0.2452(3) 0.0263(16) Uani 1 1 d . . . H14 H 0.5723 -0.0291 0.2764 0.032 Uiso 1 1 calc R . . C15 C 0.5151(4) -0.0361(6) 0.1788(3) 0.0362(18) Uani 1 1 d . . . H15 H 0.5671 -0.0156 0.1641 0.043 Uiso 1 1 calc R . . C16 C 0.4368(4) -0.0589(6) 0.1328(3) 0.0345(18) Uani 1 1 d . . . H16 H 0.4347 -0.0527 0.0867 0.041 Uiso 1 1 calc R . . C17 C 0.3620(4) -0.0907(5) 0.1542(3) 0.0266(16) Uani 1 1 d . . . H17 H 0.3087 -0.1083 0.1228 0.032 Uiso 1 1 calc R . . C18 C 0.3642(4) -0.0970(5) 0.2217(3) 0.0210(14) Uani 1 1 d . . . H18 H 0.3127 -0.1199 0.2363 0.025 Uiso 1 1 calc R . . C19 C 0.7757(4) 0.1370(5) 0.3440(3) 0.0276(16) Uani 1 1 d . . . C20 C 0.8646(5) 0.1731(6) 0.3646(4) 0.0403(19) Uani 1 1 d . . . H20 H 0.8917 0.1775 0.4106 0.048 Uiso 1 1 calc R . . C21 C 0.9137(5) 0.2030(7) 0.3167(4) 0.048(2) Uani 1 1 d . . . H21 H 0.9742 0.2252 0.3297 0.058 Uiso 1 1 calc R . . C22 C 0.8698(5) 0.1985(6) 0.2497(4) 0.044(2) Uani 1 1 d . . . H22 H 0.9009 0.2222 0.2173 0.053 Uiso 1 1 calc R . . C23 C 0.7868(5) 0.1628(7) 0.2293(4) 0.046(2) Uani 1 1 d . . . H23 H 0.7592 0.1587 0.1834 0.055 Uiso 1 1 calc R . . C24 C 0.7399(5) 0.1303(8) 0.2796(4) 0.054(2) Uani 1 1 d . . . H24 H 0.6808 0.1030 0.2659 0.065 Uiso 1 1 calc R . . C25 C 0.2126(4) -0.2557(5) 0.3342(3) 0.0263(16) Uani 1 1 d . . . H25 H 0.2740 -0.2700 0.3370 0.032 Uiso 1 1 calc R . . C26 C 0.1527(5) -0.3060(6) 0.2835(3) 0.0336(18) Uani 1 1 d . . . H26 H 0.1724 -0.3543 0.2534 0.040 Uiso 1 1 calc R . . C27 C 0.0654(5) -0.2854(6) 0.2774(4) 0.0377(19) Uani 1 1 d . . . H27 H 0.0230 -0.3197 0.2426 0.045 Uiso 1 1 calc R . . C28 C 0.0365(4) -0.2144(6) 0.3214(4) 0.0344(18) Uani 1 1 d . . . C29 C 0.1033(4) -0.1645(6) 0.3728(3) 0.0306(16) Uani 1 1 d . . . C30 C -0.0527(5) -0.1874(6) 0.3162(4) 0.042(2) Uani 1 1 d . . . H30 H -0.0967 -0.2210 0.2822 0.050 Uiso 1 1 calc R . . C31 C -0.0782(5) -0.1153(6) 0.3578(4) 0.044(2) Uani 1 1 d . . . H31 H -0.1395 -0.0979 0.3527 0.053 Uiso 1 1 calc R . . C32 C -0.0139(5) -0.0652(7) 0.4092(4) 0.047(2) Uani 1 1 d . . . H32 H -0.0318 -0.0144 0.4389 0.057 Uiso 1 1 calc R . . C33 C 0.0748(5) -0.0905(6) 0.4159(4) 0.041(2) Uani 1 1 d . . . H33 H 0.1176 -0.0569 0.4506 0.049 Uiso 1 1 calc R . . C34 C 0.2381(4) 0.1152(5) 0.3964(3) 0.0252(15) Uani 1 1 d . . . H34A H 0.1920 0.0750 0.3647 0.038 Uiso 1 1 calc R . . H34B H 0.2881 0.1320 0.3758 0.038 Uiso 1 1 calc R . . H34C H 0.2133 0.1846 0.4092 0.038 Uiso 1 1 calc R . . Cl1 Cl 0.40081(10) 0.63581(13) 0.26794(8) 0.0261(4) Uani 1 1 d . . . Cl2 Cl 0.13643(12) 0.56282(14) 0.54413(9) 0.0371(4) Uani 1 1 d . . . O1 O 0.6150(2) 0.2521(3) 0.50589(19) 0.0174(9) Uani 1 1 d . . . O2 O 0.4309(2) 0.1818(3) 0.47923(18) 0.0143(9) Uani 1 1 d . . . O3 O 0.4553(2) 0.0658(3) 0.36728(19) 0.0162(9) Uani 1 1 d . . . O4 O 0.6237(2) 0.1593(3) 0.37995(19) 0.0194(9) Uani 1 1 d . . . O5 O 0.3659(2) -0.1081(3) 0.37125(19) 0.0178(9) Uani 1 1 d . . . O6 O 0.4129(2) -0.0447(3) 0.51527(18) 0.0137(9) Uani 1 1 d . . . O7 O 0.4658(2) 0.1206(3) 0.61225(19) 0.0170(9) Uani 1 1 d . . . O8 O 0.2974(2) 0.0234(3) 0.59426(19) 0.0175(9) Uani 1 1 d . . . O9 O 0.2691(2) 0.0474(3) 0.45466(19) 0.0169(9) Uani 1 1 d . . . O10 O 0.2368(2) -0.1461(3) 0.5275(2) 0.0215(10) Uani 1 1 d . . . N1 N 0.1922(3) -0.1891(4) 0.3795(2) 0.0179(11) Uani 1 1 d . . . C35 C 0.5877(4) 0.3438(5) 0.5399(3) 0.0254(16) Uani 1 1 d . . . H35A H 0.6387 0.3720 0.5730 0.038 Uiso 1 1 calc R . . H35B H 0.5410 0.3199 0.5621 0.038 Uiso 1 1 calc R . . H35C H 0.5645 0.4027 0.5080 0.038 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 Sb1 0.0185(2) 0.0136(2) 0.0111(2) 0.00025(19) 0.00135(15) 0.00071(17) Sb2 0.0178(2) 0.0149(2) 0.0115(2) 0.00027(19) 0.00123(15) 0.00139(17) Co1 0.0185(4) 0.0162(4) 0.0142(4) -0.0009(4) 0.0011(3) -0.0002(3) P1 0.0188(8) 0.0138(8) 0.0101(8) -0.0008(7) 0.0008(6) 0.0010(6) P2 0.0216(8) 0.0174(8) 0.0143(8) 0.0013(8) 0.0049(6) 0.0018(7) C1 0.018(3) 0.012(3) 0.011(3) -0.001(3) 0.001(2) 0.004(2) C2 0.019(3) 0.025(4) 0.017(3) 0.004(3) 0.002(3) -0.004(3) C3 0.018(3) 0.020(3) 0.020(4) 0.003(3) 0.002(3) 0.005(3) C4 0.027(4) 0.020(3) 0.011(3) 0.003(3) -0.001(3) 0.000(3) C5 0.029(4) 0.026(4) 0.030(4) 0.011(3) 0.018(3) 0.003(3) C6 0.023(3) 0.024(4) 0.024(4) 0.003(3) 0.006(3) 0.004(3) C7 0.021(3) 0.023(4) 0.008(3) 0.001(3) 0.005(2) 0.000(3) C8 0.027(4) 0.020(3) 0.022(4) -0.001(3) 0.008(3) 0.001(3) C9 0.021(3) 0.033(4) 0.022(4) 0.002(3) 0.004(3) 0.008(3) C10 0.030(4) 0.025(4) 0.018(4) 0.001(3) 0.008(3) 0.014(3) C11 0.036(4) 0.020(4) 0.025(4) -0.005(3) 0.007(3) -0.002(3) C12 0.025(4) 0.022(4) 0.029(4) -0.002(3) 0.007(3) 0.002(3) C13 0.020(3) 0.013(3) 0.016(3) 0.001(3) -0.001(3) 0.003(2) C14 0.021(4) 0.039(4) 0.017(4) -0.001(3) 0.002(3) -0.007(3) C15 0.032(4) 0.057(5) 0.022(4) -0.003(4) 0.011(3) -0.009(4) C16 0.041(5) 0.047(5) 0.013(4) -0.001(4) 0.001(3) 0.005(4) C17 0.026(4) 0.031(4) 0.019(4) -0.001(3) -0.001(3) 0.002(3) C18 0.027(4) 0.017(3) 0.018(3) 0.000(3) 0.004(3) -0.006(3) C19 0.027(4) 0.030(4) 0.028(4) 0.004(3) 0.011(3) 0.006(3) C20 0.046(5) 0.042(5) 0.033(5) -0.005(4) 0.011(4) -0.005(4) C21 0.053(5) 0.052(5) 0.046(5) -0.004(5) 0.026(4) -0.001(4) C22 0.059(6) 0.038(5) 0.042(5) 0.006(4) 0.024(4) 0.003(4) C23 0.033(4) 0.070(6) 0.029(4) 0.010(4) -0.005(3) -0.001(4) C24 0.033(5) 0.094(7) 0.038(5) 0.003(5) 0.013(4) -0.011(4) C25 0.032(4) 0.019(4) 0.030(4) 0.001(3) 0.012(3) -0.006(3) C26 0.040(4) 0.035(5) 0.025(4) 0.001(4) 0.006(3) -0.002(3) C27 0.052(5) 0.027(4) 0.028(4) -0.001(4) -0.003(4) 0.000(3) C28 0.028(4) 0.035(4) 0.036(5) 0.007(4) -0.003(3) 0.000(3) C29 0.037(4) 0.029(4) 0.025(4) 0.002(4) 0.005(3) 0.001(3) C30 0.043(5) 0.041(5) 0.043(5) -0.007(4) 0.013(4) 0.002(4) C31 0.040(5) 0.049(5) 0.042(5) 0.005(5) 0.009(4) -0.006(4) C32 0.039(5) 0.059(6) 0.041(5) -0.004(5) 0.002(4) 0.011(4) C33 0.041(5) 0.057(5) 0.023(4) -0.004(4) 0.003(3) 0.008(4) C34 0.027(4) 0.025(4) 0.020(4) 0.005(3) -0.003(3) 0.008(3) Cl1 0.0348(9) 0.0196(8) 0.0235(9) 0.0073(7) 0.0055(7) 0.0052(7) Cl2 0.0495(11) 0.0278(10) 0.0362(11) 0.0012(9) 0.0140(9) 0.0162(8) O1 0.021(2) 0.016(2) 0.014(2) -0.0031(19) 0.0009(17) 0.0007(17) O2 0.020(2) 0.014(2) 0.009(2) -0.0008(18) 0.0048(16) 0.0054(17) O3 0.016(2) 0.020(2) 0.011(2) 0.0004(19) -0.0011(16) -0.0001(17) O4 0.026(2) 0.017(2) 0.015(2) 0.002(2) 0.0059(18) 0.0020(18) O5 0.023(2) 0.017(2) 0.013(2) -0.002(2) 0.0029(17) -0.0010(18) O6 0.017(2) 0.015(2) 0.008(2) 0.0013(18) 0.0009(16) 0.0021(17) O7 0.015(2) 0.020(2) 0.014(2) -0.005(2) 0.0000(16) 0.0026(17) O8 0.015(2) 0.021(2) 0.016(2) 0.003(2) 0.0022(17) 0.0021(17) O9 0.018(2) 0.021(2) 0.012(2) 0.0001(19) 0.0028(17) 0.0018(18) O10 0.015(2) 0.026(2) 0.022(2) 0.004(2) -0.0001(18) -0.0041(17) N1 0.015(3) 0.021(3) 0.018(3) 0.000(2) 0.004(2) 0.000(2) C35 0.022(3) 0.023(4) 0.027(4) -0.003(3) -0.002(3) 0.002(3) _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 Sb1 O2 1.933(3) . ? Sb1 O6 1.965(4) 3_656 ? Sb1 O3 2.015(4) . ? Sb1 O1 2.021(4) . ? Sb1 O4 2.048(4) . ? Sb1 C1 2.104(6) . ? Sb2 O2 1.911(4) . ? Sb2 O6 1.970(4) . ? Sb2 O7 2.008(4) . ? Sb2 O9 2.032(4) . ? Sb2 O8 2.054(4) . ? Sb2 C7 2.111(6) . ? Co1 O5 2.079(4) . ? Co1 O9 2.093(4) . ? Co1 O10 2.101(4) . ? Co1 N1 2.106(5) . ? Co1 O1 2.127(4) 3_656 ? Co1 O6 2.160(4) . ? P1 O5 1.487(4) . ? P1 O3 1.543(4) . ? P1 O7 1.544(4) 3_656 ? P1 C13 1.779(6) . ? P2 O10 1.489(4) 3_656 ? P2 O8 1.547(4) 3_656 ? P2 O4 1.554(4) . ? P2 C19 1.787(7) . ? C1 C2 1.386(7) . ? C1 C6 1.400(8) . ? C2 C3 1.373(8) . ? C2 H2 0.9500 . ? C3 C4 1.386(8) . ? C3 H3 0.9500 . ? C4 C5 1.372(8) . ? C4 Cl1 1.736(6) . ? C5 C6 1.378(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.386(8) . ? C7 C12 1.396(8) . ? C8 C9 1.386(8) . ? C8 H8 0.9500 . ? C9 C10 1.371(9) . ? C9 H9 0.9500 . ? C10 C11 1.379(8) . ? C10 Cl2 1.733(6) . ? C11 C12 1.376(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.384(7) . ? C13 C14 1.401(8) . ? C14 C15 1.366(9) . ? C14 H14 0.9500 . ? C15 C16 1.386(9) . ? C15 H15 0.9500 . ? C16 C17 1.379(9) . ? C16 H16 0.9500 . ? C17 C18 1.389(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.322(10) . ? C19 C20 1.409(9) . ? C20 C21 1.420(10) . ? C20 H20 0.9500 . ? C21 C22 1.399(10) . ? C21 H21 0.9500 . ? C22 C23 1.325(9) . ? C22 H22 0.9500 . ? C23 C24 1.446(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 N1 1.323(7) . ? C25 C26 1.373(9) . ? C25 H25 0.9500 . ? C26 C27 1.344(9) . ? C26 H26 0.9500 . ? C27 C28 1.392(10) . ? C27 H27 0.9500 . ? C28 C30 1.392(9) . ? C28 C29 1.436(9) . ? C29 N1 1.378(7) . ? C29 C33 1.398(9) . ? C30 C31 1.340(10) . ? C30 H30 0.9500 . ? C31 C32 1.415(10) . ? C31 H31 0.9500 . ? C32 C33 1.376(9) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 O9 1.445(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O1 C35 1.423(7) . ? O1 Co1 2.127(4) 3_656 ? O6 Sb1 1.965(4) 3_656 ? O7 P1 1.544(4) 3_656 ? O8 P2 1.547(4) 3_656 ? O10 P2 1.489(4) 3_656 ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 O2 Sb1 O6 96.14(15) . 3_656 ? O2 Sb1 O3 90.29(15) . . ? O6 Sb1 O3 89.64(15) 3_656 . ? O2 Sb1 O1 94.01(15) . . ? O6 Sb1 O1 79.74(15) 3_656 . ? O3 Sb1 O1 168.91(15) . . ? O2 Sb1 O4 176.34(16) . . ? O6 Sb1 O4 85.75(15) 3_656 . ? O3 Sb1 O4 86.58(15) . . ? O1 Sb1 O4 89.40(15) . . ? O2 Sb1 C1 91.50(19) . . ? O6 Sb1 C1 170.71(18) 3_656 . ? O3 Sb1 C1 95.61(18) . . ? O1 Sb1 C1 94.49(18) . . ? O4 Sb1 C1 86.91(18) . . ? O2 Sb2 O6 94.80(15) . . ? O2 Sb2 O7 90.32(16) . . ? O6 Sb2 O7 89.97(15) . . ? O2 Sb2 O9 95.45(15) . . ? O6 Sb2 O9 78.85(15) . . ? O7 Sb2 O9 167.80(16) . . ? O2 Sb2 O8 176.10(16) . . ? O6 Sb2 O8 87.91(15) . . ? O7 Sb2 O8 86.88(15) . . ? O9 Sb2 O8 87.82(15) . . ? O2 Sb2 C7 90.04(19) . . ? O6 Sb2 C7 171.43(19) . . ? O7 Sb2 C7 97.08(19) . . ? O9 Sb2 C7 93.67(19) . . ? O8 Sb2 C7 87.62(19) . . ? O5 Co1 O9 97.58(15) . . ? O5 Co1 O10 175.80(16) . . ? O9 Co1 O10 86.61(15) . . ? O5 Co1 N1 87.26(17) . . ? O9 Co1 N1 105.07(17) . . ? O10 Co1 N1 91.93(17) . . ? O5 Co1 O1 92.29(15) . 3_656 ? O9 Co1 O1 145.05(15) . 3_656 ? O10 Co1 O1 84.06(15) . 3_656 ? N1 Co1 O1 108.83(17) . 3_656 ? O5 Co1 O6 90.07(14) . . ? O9 Co1 O6 73.38(14) . . ? O10 Co1 O6 90.86(14) . . ? N1 Co1 O6 176.72(17) . . ? O1 Co1 O6 73.16(14) 3_656 . ? O5 P1 O3 112.4(2) . . ? O5 P1 O7 114.1(2) . 3_656 ? O3 P1 O7 110.9(2) . 3_656 ? O5 P1 C13 110.7(3) . . ? O3 P1 C13 102.8(2) . . ? O7 P1 C13 105.1(2) 3_656 . ? O10 P2 O8 112.4(2) 3_656 3_656 ? O10 P2 O4 113.3(2) 3_656 . ? O8 P2 O4 108.3(2) 3_656 . ? O10 P2 C19 111.2(3) 3_656 . ? O8 P2 C19 107.7(3) 3_656 . ? O4 P2 C19 103.3(3) . . ? C2 C1 C6 118.1(5) . . ? C2 C1 Sb1 121.9(4) . . ? C6 C1 Sb1 119.9(4) . . ? C3 C2 C1 121.2(6) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 119.8(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.1(6) . . ? C5 C4 Cl1 119.9(5) . . ? C3 C4 Cl1 120.0(5) . . ? C4 C5 C6 120.0(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.7(6) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C8 C7 C12 117.5(6) . . ? C8 C7 Sb2 120.7(4) . . ? C12 C7 Sb2 121.3(4) . . ? C7 C8 C9 121.9(6) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C10 C9 C8 118.8(6) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 120.9(6) . . ? C9 C10 Cl2 120.1(5) . . ? C11 C10 Cl2 119.0(5) . . ? C12 C11 C10 119.7(6) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C7 121.1(6) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? C18 C13 C14 118.9(6) . . ? C18 C13 P1 123.4(5) . . ? C14 C13 P1 117.6(4) . . ? C15 C14 C13 120.5(6) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.3(6) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.8(6) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.2(6) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 120.1(6) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C24 C19 C20 118.8(7) . . ? C24 C19 P2 123.0(5) . . ? C20 C19 P2 118.2(5) . . ? C19 C20 C21 120.0(7) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 117.8(7) . . ? C22 C21 H21 121.1 . . ? C20 C21 H21 121.1 . . ? C23 C22 C21 123.0(7) . . ? C23 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C22 C23 C24 117.5(7) . . ? C22 C23 H23 121.3 . . ? C24 C23 H23 121.3 . . ? C19 C24 C23 122.9(7) . . ? C19 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? N1 C25 C26 125.5(6) . . ? N1 C25 H25 117.2 . . ? C26 C25 H25 117.2 . . ? C27 C26 C25 118.6(7) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C26 C27 C28 120.8(7) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C30 C28 C27 123.2(7) . . ? C30 C28 C29 119.4(7) . . ? C27 C28 C29 117.4(6) . . ? N1 C29 C33 121.4(6) . . ? N1 C29 C28 121.0(6) . . ? C33 C29 C28 117.6(6) . . ? C31 C30 C28 121.8(7) . . ? C31 C30 H30 119.1 . . ? C28 C30 H30 119.1 . . ? C30 C31 C32 120.1(7) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 119.5(8) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C29 121.6(7) . . ? C32 C33 H33 119.2 . . ? C29 C33 H33 119.2 . . ? O9 C34 H34A 109.5 . . ? O9 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O9 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 O1 Sb1 120.9(3) . . ? C35 O1 Co1 125.4(3) . 3_656 ? Sb1 O1 Co1 102.18(16) . 3_656 ? Sb2 O2 Sb1 144.1(2) . . ? P1 O3 Sb1 138.7(2) . . ? P2 O4 Sb1 123.9(2) . . ? P1 O5 Co1 141.8(2) . . ? Sb1 O6 Sb2 138.4(2) 3_656 . ? Sb1 O6 Co1 102.92(16) 3_656 . ? Sb2 O6 Co1 102.47(15) . . ? P1 O7 Sb2 138.2(2) 3_656 . ? P2 O8 Sb2 122.4(2) 3_656 . ? C34 O9 Sb2 121.5(3) . . ? C34 O9 Co1 122.4(3) . . ? Sb2 O9 Co1 102.73(16) . . ? P2 O10 Co1 116.5(2) 3_656 . ? C25 N1 C29 116.7(5) . . ? C25 N1 Co1 116.1(4) . . ? C29 N1 Co1 127.0(4) . . ? O1 C35 H35A 109.5 . . ? O1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? 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 O2 Sb1 C1 C2 -17.5(5) . . . . ? O6 Sb1 C1 C2 -162.8(9) 3_656 . . . ? O3 Sb1 C1 C2 73.0(5) . . . . ? O1 Sb1 C1 C2 -111.6(5) . . . . ? O4 Sb1 C1 C2 159.2(5) . . . . ? O2 Sb1 C1 C6 159.8(5) . . . . ? O6 Sb1 C1 C6 14.4(15) 3_656 . . . ? O3 Sb1 C1 C6 -109.7(5) . . . . ? O1 Sb1 C1 C6 65.7(5) . . . . ? O4 Sb1 C1 C6 -23.5(5) . . . . ? C6 C1 C2 C3 0.2(9) . . . . ? Sb1 C1 C2 C3 177.5(4) . . . . ? C1 C2 C3 C4 0.1(9) . . . . ? C2 C3 C4 C5 0.5(9) . . . . ? C2 C3 C4 Cl1 -179.1(5) . . . . ? C3 C4 C5 C6 -1.5(10) . . . . ? Cl1 C4 C5 C6 178.2(5) . . . . ? C4 C5 C6 C1 1.9(10) . . . . ? C2 C1 C6 C5 -1.2(9) . . . . ? Sb1 C1 C6 C5 -178.6(5) . . . . ? O2 Sb2 C7 C8 139.4(5) . . . . ? O6 Sb2 C7 C8 14.9(16) . . . . ? O7 Sb2 C7 C8 -130.3(5) . . . . ? O9 Sb2 C7 C8 43.9(5) . . . . ? O8 Sb2 C7 C8 -43.7(5) . . . . ? O2 Sb2 C7 C12 -32.5(5) . . . . ? O6 Sb2 C7 C12 -157.0(11) . . . . ? O7 Sb2 C7 C12 57.8(5) . . . . ? O9 Sb2 C7 C12 -127.9(5) . . . . ? O8 Sb2 C7 C12 144.4(5) . . . . ? C12 C7 C8 C9 -0.5(9) . . . . ? Sb2 C7 C8 C9 -172.6(5) . . . . ? C7 C8 C9 C10 1.2(10) . . . . ? C8 C9 C10 C11 -1.3(10) . . . . ? C8 C9 C10 Cl2 178.3(5) . . . . ? C9 C10 C11 C12 0.7(10) . . . . ? Cl2 C10 C11 C12 -178.9(5) . . . . ? C10 C11 C12 C7 0.1(10) . . . . ? C8 C7 C12 C11 -0.2(9) . . . . ? Sb2 C7 C12 C11 171.9(5) . . . . ? O5 P1 C13 C18 12.3(6) . . . . ? O3 P1 C13 C18 -107.9(5) . . . . ? O7 P1 C13 C18 136.0(5) 3_656 . . . ? O5 P1 C13 C14 -171.4(5) . . . . ? O3 P1 C13 C14 68.4(5) . . . . ? O7 P1 C13 C14 -47.7(5) 3_656 . . . ? C18 C13 C14 C15 4.1(10) . . . . ? P1 C13 C14 C15 -172.3(6) . . . . ? C13 C14 C15 C16 -1.7(11) . . . . ? C14 C15 C16 C17 -1.2(11) . . . . ? C15 C16 C17 C18 1.7(10) . . . . ? C14 C13 C18 C17 -3.7(9) . . . . ? P1 C13 C18 C17 172.6(5) . . . . ? C16 C17 C18 C13 0.8(10) . . . . ? O10 P2 C19 C24 -165.2(7) 3_656 . . . ? O8 P2 C19 C24 71.1(7) 3_656 . . . ? O4 P2 C19 C24 -43.3(7) . . . . ? O10 P2 C19 C20 13.9(6) 3_656 . . . ? O8 P2 C19 C20 -109.7(5) 3_656 . . . ? O4 P2 C19 C20 135.9(5) . . . . ? C24 C19 C20 C21 0.8(11) . . . . ? P2 C19 C20 C21 -178.4(6) . . . . ? C19 C20 C21 C22 2.1(11) . . . . ? C20 C21 C22 C23 -3.4(12) . . . . ? C21 C22 C23 C24 1.8(13) . . . . ? C20 C19 C24 C23 -2.6(13) . . . . ? P2 C19 C24 C23 176.6(6) . . . . ? C22 C23 C24 C19 1.4(13) . . . . ? N1 C25 C26 C27 1.4(10) . . . . ? C25 C26 C27 C28 0.2(10) . . . . ? C26 C27 C28 C30 177.9(7) . . . . ? C26 C27 C28 C29 0.2(10) . . . . ? C30 C28 C29 N1 -179.9(6) . . . . ? C27 C28 C29 N1 -2.1(10) . . . . ? C30 C28 C29 C33 0.3(10) . . . . ? C27 C28 C29 C33 178.1(7) . . . . ? C27 C28 C30 C31 -177.3(7) . . . . ? C29 C28 C30 C31 0.4(11) . . . . ? C28 C30 C31 C32 -0.7(12) . . . . ? C30 C31 C32 C33 0.3(12) . . . . ? C31 C32 C33 C29 0.3(12) . . . . ? N1 C29 C33 C32 179.6(7) . . . . ? C28 C29 C33 C32 -0.6(11) . . . . ? O2 Sb1 O1 C35 -38.4(4) . . . . ? O6 Sb1 O1 C35 -133.9(4) 3_656 . . . ? O3 Sb1 O1 C35 -151.0(8) . . . . ? O4 Sb1 O1 C35 140.3(4) . . . . ? C1 Sb1 O1 C35 53.4(4) . . . . ? O2 Sb1 O1 Co1 106.64(17) . . . 3_656 ? O6 Sb1 O1 Co1 11.11(15) 3_656 . . 3_656 ? O3 Sb1 O1 Co1 -6.0(9) . . . 3_656 ? O4 Sb1 O1 Co1 -74.68(17) . . . 3_656 ? C1 Sb1 O1 Co1 -161.5(2) . . . 3_656 ? O6 Sb2 O2 Sb1 -13.0(4) . . . . ? O7 Sb2 O2 Sb1 77.0(3) . . . . ? O9 Sb2 O2 Sb1 -92.2(3) . . . . ? O8 Sb2 O2 Sb1 121(2) . . . . ? C7 Sb2 O2 Sb1 174.1(4) . . . . ? O6 Sb1 O2 Sb2 -21.1(4) 3_656 . . . ? O3 Sb1 O2 Sb2 68.5(3) . . . . ? O1 Sb1 O2 Sb2 -101.2(3) . . . . ? O4 Sb1 O2 Sb2 100(2) . . . . ? C1 Sb1 O2 Sb2 164.2(4) . . . . ? O5 P1 O3 Sb1 105.6(4) . . . . ? O7 P1 O3 Sb1 -23.5(4) 3_656 . . . ? C13 P1 O3 Sb1 -135.4(4) . . . . ? O2 Sb1 O3 P1 -98.7(4) . . . . ? O6 Sb1 O3 P1 -2.5(4) 3_656 . . . ? O1 Sb1 O3 P1 14.3(11) . . . . ? O4 Sb1 O3 P1 83.2(4) . . . . ? C1 Sb1 O3 P1 169.8(4) . . . . ? O10 P2 O4 Sb1 -50.9(3) 3_656 . . . ? O8 P2 O4 Sb1 74.5(3) 3_656 . . . ? C19 P2 O4 Sb1 -171.4(3) . . . . ? O2 Sb1 O4 P2 -144(2) . . . . ? O6 Sb1 O4 P2 -22.9(3) 3_656 . . . ? O3 Sb1 O4 P2 -112.8(3) . . . . ? O1 Sb1 O4 P2 56.8(3) . . . . ? C1 Sb1 O4 P2 151.3(3) . . . . ? O3 P1 O5 Co1 -55.5(4) . . . . ? O7 P1 O5 Co1 71.9(4) 3_656 . . . ? C13 P1 O5 Co1 -169.8(4) . . . . ? O9 Co1 O5 P1 66.3(4) . . . . ? O10 Co1 O5 P1 -110(2) . . . . ? N1 Co1 O5 P1 171.1(4) . . . . ? O1 Co1 O5 P1 -80.1(4) 3_656 . . . ? O6 Co1 O5 P1 -7.0(4) . . . . ? O2 Sb2 O6 Sb1 126.6(3) . . . 3_656 ? O7 Sb2 O6 Sb1 36.3(3) . . . 3_656 ? O9 Sb2 O6 Sb1 -138.8(3) . . . 3_656 ? O8 Sb2 O6 Sb1 -50.6(3) . . . 3_656 ? C7 Sb2 O6 Sb1 -109.2(12) . . . 3_656 ? O2 Sb2 O6 Co1 -106.89(16) . . . . ? O7 Sb2 O6 Co1 162.79(17) . . . . ? O9 Sb2 O6 Co1 -12.27(15) . . . . ? O8 Sb2 O6 Co1 75.92(16) . . . . ? C7 Sb2 O6 Co1 17.3(13) . . . . ? O5 Co1 O6 Sb1 -103.08(17) . . . 3_656 ? O9 Co1 O6 Sb1 159.03(19) . . . 3_656 ? O10 Co1 O6 Sb1 72.82(17) . . . 3_656 ? N1 Co1 O6 Sb1 -139(3) . . . 3_656 ? O1 Co1 O6 Sb1 -10.71(15) 3_656 . . 3_656 ? O5 Co1 O6 Sb2 110.09(17) . . . . ? O9 Co1 O6 Sb2 12.20(15) . . . . ? O10 Co1 O6 Sb2 -74.01(17) . . . . ? N1 Co1 O6 Sb2 74(3) . . . . ? O1 Co1 O6 Sb2 -157.54(19) 3_656 . . . ? O2 Sb2 O7 P1 -87.4(4) . . . 3_656 ? O6 Sb2 O7 P1 7.4(4) . . . 3_656 ? O9 Sb2 O7 P1 30.9(10) . . . 3_656 ? O8 Sb2 O7 P1 95.3(4) . . . 3_656 ? C7 Sb2 O7 P1 -177.5(4) . . . 3_656 ? O2 Sb2 O8 P2 -149(2) . . . 3_656 ? O6 Sb2 O8 P2 -15.3(3) . . . 3_656 ? O7 Sb2 O8 P2 -105.4(3) . . . 3_656 ? O9 Sb2 O8 P2 63.6(3) . . . 3_656 ? C7 Sb2 O8 P2 157.3(3) . . . 3_656 ? O2 Sb2 O9 C34 -35.0(4) . . . . ? O6 Sb2 O9 C34 -128.9(4) . . . . ? O7 Sb2 O9 C34 -152.9(7) . . . . ? O8 Sb2 O9 C34 142.8(4) . . . . ? C7 Sb2 O9 C34 55.4(4) . . . . ? O2 Sb2 O9 Co1 106.52(17) . . . . ? O6 Sb2 O9 Co1 12.69(16) . . . . ? O7 Sb2 O9 Co1 -11.3(8) . . . . ? O8 Sb2 O9 Co1 -75.61(17) . . . . ? C7 Sb2 O9 Co1 -163.1(2) . . . . ? O5 Co1 O9 C34 41.5(4) . . . . ? O10 Co1 O9 C34 -138.8(4) . . . . ? N1 Co1 O9 C34 -47.7(4) . . . . ? O1 Co1 O9 C34 146.6(4) 3_656 . . . ? O6 Co1 O9 C34 129.3(4) . . . . ? O5 Co1 O9 Sb2 -99.63(17) . . . . ? O10 Co1 O9 Sb2 80.08(17) . . . . ? N1 Co1 O9 Sb2 171.17(18) . . . . ? O1 Co1 O9 Sb2 5.5(3) 3_656 . . . ? O6 Co1 O9 Sb2 -11.83(15) . . . . ? O5 Co1 O10 P2 105(2) . . . 3_656 ? O9 Co1 O10 P2 -71.3(3) . . . 3_656 ? N1 Co1 O10 P2 -176.3(3) . . . 3_656 ? O1 Co1 O10 P2 75.0(3) 3_656 . . 3_656 ? O6 Co1 O10 P2 2.0(3) . . . 3_656 ? C26 C25 N1 C29 -3.2(9) . . . . ? C26 C25 N1 Co1 -177.8(5) . . . . ? C33 C29 N1 C25 -176.7(6) . . . . ? C28 C29 N1 C25 3.5(9) . . . . ? C33 C29 N1 Co1 -2.8(9) . . . . ? C28 C29 N1 Co1 177.4(5) . . . . ? O5 Co1 N1 C25 37.5(4) . . . . ? O9 Co1 N1 C25 134.6(4) . . . . ? O10 Co1 N1 C25 -138.4(4) . . . . ? O1 Co1 N1 C25 -54.0(5) 3_656 . . . ? O6 Co1 N1 C25 73(3) . . . . ? O5 Co1 N1 C29 -136.5(5) . . . . ? O9 Co1 N1 C29 -39.4(5) . . . . ? O10 Co1 N1 C29 47.7(5) . . . . ? O1 Co1 N1 C29 132.0(5) 3_656 . . . ? O6 Co1 N1 C29 -101(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.092 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.156 # Attachment '- 7.cif' data_mono1394 _database_code_depnum_ccdc_archive 'CCDC 778677' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H68 Cl4 Co2 N4 O23 P4 Sb4' _chemical_formula_weight 2107.74 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 28.3131(12) _cell_length_b 11.9629(4) _cell_length_c 22.1246(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.140(4) _cell_angle_gamma 90.00 _cell_volume 7352.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7610 _cell_measurement_theta_min 2.7304 _cell_measurement_theta_max 28.3741 _exptl_crystal_description Needles _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.904 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4152 _exptl_absorpt_coefficient_mu 2.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5582 _exptl_absorpt_correction_T_max 0.8100 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14819 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.15 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7499 _reflns_number_gt 5498 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; A larger than usual U(eq) range was due to disorder of a phenyl ring C50-O50 which was modelled. The disorer of a sovent molecule C50-O50 was also modelled. 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^)+(0.0221P)^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 7499 _refine_ls_number_parameters 532 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.898 _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 Sb1 Sb 0.323423(9) 0.641764(18) 0.063326(10) 0.00974(6) Uani 1 1 d . . . Sb2 Sb 0.303753(9) 0.922595(18) -0.003869(10) 0.00974(6) Uani 1 1 d . . . Co1 Co 0.205755(17) 0.64002(4) -0.13367(2) 0.01130(11) Uani 1 1 d . . . P1 P 0.39557(3) 0.84655(7) 0.09668(4) 0.0128(2) Uani 1 1 d D . . P2 P 0.32105(3) 0.69739(7) -0.08471(4) 0.0110(2) Uani 1 1 d . . . N1 N 0.15891(12) 0.4884(3) -0.23143(16) 0.0242(8) Uani 1 1 d . . . N2 N 0.20084(11) 0.5402(2) -0.21073(13) 0.0149(7) Uani 1 1 d . . . O1 O 0.31129(9) 0.68924(18) 0.14729(10) 0.0128(5) Uani 1 1 d . . . O2 O 0.38958(8) 0.71910(17) 0.08398(10) 0.0125(5) Uani 1 1 d . A . O3 O 0.26314(8) 0.56490(17) 0.04263(10) 0.0113(5) Uani 1 1 d . . . O4 O 0.33590(8) 0.63192(18) -0.02361(10) 0.0122(5) Uani 1 1 d . . . O5 O 0.29418(8) 0.79006(17) 0.04508(10) 0.0096(5) Uani 1 1 d . . . O6 O 0.37544(8) 0.90997(18) 0.03625(10) 0.0124(5) Uani 1 1 d . A . O7 O 0.31649(9) 0.82387(17) -0.07166(10) 0.0124(5) Uani 1 1 d . . . O8 O 0.29387(8) 0.99942(17) 0.07359(10) 0.0114(5) Uani 1 1 d . . . O9 O 0.27803(9) 0.65082(18) -0.12666(10) 0.0141(5) Uani 1 1 d . . . O10 O 0.12720(8) 0.61839(18) -0.14954(10) 0.0136(5) Uani 1 1 d . . . C1 C 0.35883(13) 0.4897(3) 0.09126(15) 0.0125(8) Uani 1 1 d . . . C2 C 0.40774(14) 0.4749(3) 0.09648(18) 0.0257(10) Uani 1 1 d . . . H2 H 0.4268 0.5354 0.0868 0.031 Uiso 1 1 calc R . . C3 C 0.42982(15) 0.3746(3) 0.11537(19) 0.0278(10) Uani 1 1 d . . . H3 H 0.4635 0.3654 0.1177 0.033 Uiso 1 1 calc R . . C4 C 0.40223(14) 0.2874(3) 0.13078(16) 0.0166(8) Uani 1 1 d . . . C5 C 0.35378(14) 0.2984(3) 0.12691(18) 0.0227(9) Uani 1 1 d . . . H5 H 0.3353 0.2381 0.1378 0.027 Uiso 1 1 calc R . . C6 C 0.33199(14) 0.3995(3) 0.10673(17) 0.0205(9) Uani 1 1 d . . . H6 H 0.2982 0.4074 0.1034 0.025 Uiso 1 1 calc R . . C7 C 0.32222(13) 1.0689(3) -0.04637(15) 0.0121(8) Uani 1 1 d . . . C8 C 0.35315(14) 1.1458(3) -0.01171(16) 0.0197(8) Uani 1 1 d . . . H8 H 0.3670 1.1296 0.0300 0.024 Uiso 1 1 calc R . . C9 C 0.36384(15) 1.2461(3) -0.03779(17) 0.0225(9) Uani 1 1 d . . . H9 H 0.3842 1.2997 -0.0140 0.027 Uiso 1 1 calc R . . C10 C 0.34428(14) 1.2664(3) -0.09880(17) 0.0185(9) Uani 1 1 d . . . C11 C 0.31371(14) 1.1914(3) -0.13420(17) 0.0196(9) Uani 1 1 d . . . H11 H 0.3004 1.2072 -0.1761 0.023 Uiso 1 1 calc R . . C12 C 0.30279(13) 1.0921(3) -0.10726(16) 0.0177(8) Uani 1 1 d . . . H12 H 0.2817 1.0397 -0.1310 0.021 Uiso 1 1 calc R . . C13 C 0.4590(2) 0.8718(7) 0.1107(3) 0.0204(18) Uani 0.727(9) 1 d PDU A 1 C14 C 0.4880(3) 0.8319(8) 0.1613(4) 0.064(2) Uani 0.727(9) 1 d PU A 1 H14 H 0.4750 0.7901 0.1908 0.077 Uiso 0.727(9) 1 calc PR A 1 C15 C 0.5379(3) 0.8527(9) 0.1705(4) 0.079(3) Uani 0.727(9) 1 d PU A 1 H15 H 0.5580 0.8235 0.2064 0.094 Uiso 0.727(9) 1 calc PR A 1 C16 C 0.5582(3) 0.9114(9) 0.1311(5) 0.056(2) Uani 0.727(9) 1 d PU A 1 H16 H 0.5919 0.9238 0.1385 0.067 Uiso 0.727(9) 1 calc PR A 1 C17 C 0.5297(3) 0.9517(8) 0.0814(4) 0.062(2) Uani 0.727(9) 1 d PU A 1 H17 H 0.5434 0.9936 0.0528 0.074 Uiso 0.727(9) 1 calc PR A 1 C18 C 0.4801(2) 0.9346(7) 0.0698(4) 0.0472(19) Uani 0.727(9) 1 d PU A 1 H18 H 0.4606 0.9657 0.0340 0.057 Uiso 0.727(9) 1 calc PR A 1 C13A C 0.4586(3) 0.8715(15) 0.1162(6) 0.022(5) Uani 0.273(9) 1 d PGDU A 2 C14A C 0.4806(4) 0.9041(13) 0.1752(5) 0.030(4) Uani 0.273(9) 1 d PGU A 2 H14A H 0.4618 0.9144 0.2060 0.036 Uiso 0.273(9) 1 calc PR A 2 C15A C 0.5300(4) 0.9217(13) 0.1892(5) 0.038(4) Uani 0.273(9) 1 d PGU A 2 H15A H 0.5450 0.9440 0.2296 0.046 Uiso 0.273(9) 1 calc PR A 2 C16A C 0.5575(3) 0.9066(15) 0.1442(6) 0.040(4) Uani 0.273(9) 1 d PGU A 2 H16A H 0.5913 0.9186 0.1537 0.048 Uiso 0.273(9) 1 calc PR A 2 C17A C 0.5356(4) 0.8740(15) 0.0851(6) 0.041(4) Uani 0.273(9) 1 d PGU A 2 H17A H 0.5543 0.8637 0.0543 0.049 Uiso 0.273(9) 1 calc PR A 2 C18A C 0.4861(4) 0.8564(15) 0.0711(5) 0.035(4) Uani 0.273(9) 1 d PGU A 2 H18A H 0.4711 0.8341 0.0307 0.042 Uiso 0.273(9) 1 calc PR A 2 C19 C 0.37115(13) 0.6935(3) -0.12307(15) 0.0112(8) Uani 1 1 d . . . C20 C 0.41178(14) 0.7558(3) -0.10011(19) 0.0302(11) Uani 1 1 d . . . H20 H 0.4139 0.7948 -0.0623 0.036 Uiso 1 1 calc R . . C21 C 0.44942(15) 0.7620(4) -0.13155(19) 0.0338(11) Uani 1 1 d . . . H21 H 0.4770 0.8055 -0.1154 0.041 Uiso 1 1 calc R . . C22 C 0.44698(15) 0.7048(3) -0.18664(18) 0.0236(9) Uani 1 1 d . . . H22 H 0.4728 0.7094 -0.2083 0.028 Uiso 1 1 calc R . . C23 C 0.40720(14) 0.6419(3) -0.20963(17) 0.0215(9) Uani 1 1 d . . . H23 H 0.4058 0.6009 -0.2467 0.026 Uiso 1 1 calc R . . C24 C 0.36877(14) 0.6379(3) -0.17877(16) 0.0173(8) Uani 1 1 d . . . H24 H 0.3407 0.5968 -0.1959 0.021 Uiso 1 1 calc R . . C25 C 0.23271(14) 0.4845(3) -0.23566(16) 0.0214(9) Uani 1 1 d . . . H25 H 0.2660 0.5019 -0.2293 0.026 Uiso 1 1 calc R . . C26 C 0.21095(15) 0.3968(3) -0.27247(17) 0.0226(9) Uani 1 1 d . . . H26 H 0.2258 0.3449 -0.2954 0.027 Uiso 1 1 calc R . . C27 C 0.16370(16) 0.4022(3) -0.26821(19) 0.0319(11) Uani 1 1 d . . . H27 H 0.1388 0.3537 -0.2877 0.038 Uiso 1 1 calc R . . C28 C 0.25758(13) 1.0845(3) 0.06998(16) 0.0168(8) Uani 1 1 d . . . H28A H 0.2634 1.1430 0.0413 0.025 Uiso 1 1 calc R . . H28B H 0.2588 1.1171 0.1109 0.025 Uiso 1 1 calc R . . H28C H 0.2258 1.0514 0.0553 0.025 Uiso 1 1 calc R . . C29 C 0.34155(14) 0.6504(3) 0.20337(15) 0.0206(9) Uani 1 1 d . . . H29A H 0.3345 0.5716 0.2099 0.031 Uiso 1 1 calc R . . H29B H 0.3353 0.6948 0.2382 0.031 Uiso 1 1 calc R . . H29C H 0.3754 0.6584 0.2002 0.031 Uiso 1 1 calc R . . Cl1 Cl 0.42960(4) 0.16050(7) 0.15571(5) 0.0229(2) Uani 1 1 d . . . Cl2 Cl 0.35925(4) 1.39051(8) -0.13124(5) 0.0298(3) Uani 1 1 d . . . C50 C 0.5151(7) 0.6225(14) 0.0521(8) 0.142(4) Uani 0.577(8) 1 d PDU B 1 H50A H 0.5258 0.6958 0.0691 0.212 Uiso 0.577(8) 1 calc PR B 1 H50B H 0.4809 0.6262 0.0327 0.212 Uiso 0.577(8) 1 calc PR B 1 H50C H 0.5340 0.6008 0.0212 0.212 Uiso 0.577(8) 1 calc PR B 1 O50 O 0.5216(3) 0.5426(7) 0.0998(5) 0.119(4) Uani 0.577(8) 1 d PDU B 1 O50A O 0.4958(7) 0.6237(15) 0.0079(9) 0.167(5) Uani 0.423(8) 1 d PDU B 2 C50A C 0.4562(8) 0.5600(18) -0.0158(10) 0.169(6) Uani 0.423(8) 1 d PDU B 2 H50D H 0.4534 0.4985 0.0126 0.254 Uiso 0.423(8) 1 calc PR B 2 H50E H 0.4597 0.5295 -0.0558 0.254 Uiso 0.423(8) 1 calc PR B 2 H50F H 0.4272 0.6065 -0.0210 0.254 Uiso 0.423(8) 1 calc PR B 2 O51 O 0.5000 0.5529(11) 0.2500 0.292(6) Uani 1 2 d SU . . C51 C 0.5328(5) 0.6091(10) 0.2120(8) 0.281(6) Uani 1 1 d U . . H51A H 0.5499 0.5518 0.1929 0.422 Uiso 1 1 calc R . . H51B H 0.5562 0.6564 0.2389 0.422 Uiso 1 1 calc R . . H51C H 0.5134 0.6551 0.1798 0.422 Uiso 1 1 calc R . . H1N H 0.1341(15) 0.507(3) -0.2141(19) 0.040(13) Uiso 1 1 d . . . 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 Sb1 0.01147(12) 0.00865(12) 0.00938(11) 0.00045(10) 0.00273(9) 0.00119(10) Sb2 0.01192(12) 0.00796(12) 0.00988(11) -0.00013(10) 0.00345(9) 0.00009(10) Co1 0.0134(3) 0.0110(2) 0.0098(2) -0.0011(2) 0.0031(2) 0.0008(2) P1 0.0105(5) 0.0133(5) 0.0143(5) -0.0015(4) 0.0018(4) 0.0004(4) P2 0.0133(5) 0.0104(5) 0.0101(5) -0.0005(4) 0.0044(4) 0.0007(4) N1 0.0196(19) 0.0226(19) 0.032(2) -0.0137(16) 0.0082(17) 0.0000(16) N2 0.0147(16) 0.0160(16) 0.0136(15) -0.0021(13) 0.0020(14) -0.0016(14) O1 0.0150(13) 0.0158(13) 0.0079(12) 0.0025(10) 0.0026(11) 0.0062(11) O2 0.0117(13) 0.0100(12) 0.0156(13) 0.0007(10) 0.0024(11) 0.0004(11) O3 0.0112(13) 0.0087(12) 0.0139(12) 0.0020(10) 0.0020(11) 0.0023(10) O4 0.0175(13) 0.0098(12) 0.0103(12) 0.0002(10) 0.0055(11) 0.0027(11) O5 0.0138(13) 0.0068(11) 0.0079(12) 0.0020(10) 0.0016(10) 0.0018(10) O6 0.0120(13) 0.0116(12) 0.0145(12) 0.0009(10) 0.0052(11) -0.0006(11) O7 0.0182(14) 0.0097(12) 0.0103(12) -0.0006(10) 0.0050(11) 0.0006(11) O8 0.0135(13) 0.0099(12) 0.0119(12) -0.0006(10) 0.0050(11) 0.0037(10) O9 0.0153(13) 0.0146(13) 0.0136(12) -0.0022(10) 0.0061(11) -0.0002(11) O10 0.0136(13) 0.0129(12) 0.0139(12) -0.0022(10) 0.0017(11) 0.0002(11) C1 0.016(2) 0.0152(19) 0.0056(16) -0.0013(14) 0.0000(15) 0.0017(16) C2 0.022(2) 0.018(2) 0.037(2) 0.0094(19) 0.008(2) 0.0024(19) C3 0.020(2) 0.023(2) 0.042(3) 0.010(2) 0.008(2) 0.0057(19) C4 0.021(2) 0.0111(19) 0.017(2) 0.0027(16) 0.0014(17) 0.0021(17) C5 0.023(2) 0.017(2) 0.028(2) 0.0049(18) 0.0056(19) -0.0010(18) C6 0.014(2) 0.0136(19) 0.034(2) 0.0017(17) 0.0048(18) 0.0020(16) C7 0.0166(19) 0.0071(17) 0.0146(18) -0.0003(15) 0.0084(16) 0.0007(16) C8 0.026(2) 0.021(2) 0.0125(18) -0.0001(17) 0.0037(17) -0.0007(19) C9 0.034(3) 0.013(2) 0.020(2) -0.0023(16) 0.005(2) -0.0099(18) C10 0.027(2) 0.0074(18) 0.024(2) 0.0030(16) 0.0143(19) -0.0016(17) C11 0.024(2) 0.017(2) 0.016(2) 0.0066(16) 0.0025(18) 0.0012(18) C12 0.021(2) 0.0124(19) 0.020(2) -0.0042(16) 0.0055(17) -0.0050(17) C13 0.018(3) 0.016(4) 0.027(3) -0.003(3) 0.006(3) 0.004(3) C14 0.026(4) 0.113(6) 0.050(4) 0.018(4) -0.003(3) -0.006(4) C15 0.029(4) 0.133(7) 0.067(5) 0.003(5) -0.010(4) -0.003(5) C16 0.020(4) 0.062(5) 0.086(6) -0.029(4) 0.011(4) -0.010(4) C17 0.028(4) 0.049(5) 0.110(5) -0.003(4) 0.019(4) -0.015(4) C18 0.024(3) 0.036(4) 0.082(4) 0.011(3) 0.012(3) -0.006(3) C13A 0.009(7) 0.027(10) 0.029(8) -0.017(7) 0.001(6) -0.001(8) C14A 0.009(6) 0.039(8) 0.040(7) -0.024(6) -0.001(5) 0.000(6) C15A 0.012(6) 0.045(9) 0.053(7) -0.026(7) -0.003(6) -0.006(6) C16A 0.008(6) 0.049(10) 0.061(8) -0.015(8) 0.002(6) -0.011(7) C17A 0.012(6) 0.062(10) 0.051(7) -0.001(7) 0.009(6) -0.006(7) C18A 0.012(6) 0.059(10) 0.036(7) -0.008(7) 0.006(5) -0.003(7) C19 0.0126(19) 0.0115(18) 0.0103(18) 0.0031(15) 0.0044(15) 0.0051(15) C20 0.021(2) 0.048(3) 0.025(2) -0.016(2) 0.013(2) -0.005(2) C21 0.017(2) 0.050(3) 0.036(3) -0.011(2) 0.010(2) -0.011(2) C22 0.021(2) 0.027(2) 0.027(2) 0.0093(19) 0.0153(19) 0.0099(19) C23 0.029(2) 0.019(2) 0.020(2) -0.0004(18) 0.0132(18) 0.0047(19) C24 0.023(2) 0.0132(19) 0.0169(19) 0.0028(16) 0.0079(17) 0.0007(17) C25 0.021(2) 0.029(2) 0.0155(19) -0.0025(17) 0.0053(18) -0.0002(19) C26 0.029(2) 0.019(2) 0.020(2) -0.0098(17) 0.0033(19) 0.0021(18) C27 0.032(3) 0.028(2) 0.037(3) -0.023(2) 0.009(2) -0.011(2) C28 0.020(2) 0.0138(19) 0.0174(19) -0.0029(16) 0.0047(17) 0.0032(17) C29 0.028(2) 0.021(2) 0.0128(18) 0.0000(17) 0.0013(17) 0.0081(19) Cl1 0.0225(5) 0.0135(5) 0.0328(6) 0.0064(4) 0.0056(5) 0.0044(4) Cl2 0.0466(7) 0.0158(5) 0.0288(5) 0.0060(4) 0.0113(5) -0.0076(5) C50 0.117(9) 0.138(8) 0.166(11) 0.060(7) 0.019(9) -0.015(7) O50 0.084(6) 0.102(6) 0.176(9) 0.044(6) 0.037(6) -0.009(5) O50A 0.161(11) 0.161(9) 0.167(11) 0.091(9) 0.003(10) -0.025(8) C50A 0.151(13) 0.190(12) 0.156(13) 0.112(11) 0.002(12) -0.033(9) O51 0.242(13) 0.230(11) 0.47(2) 0.000 0.220(12) 0.000 C51 0.228(14) 0.193(10) 0.48(2) -0.006(8) 0.205(12) -0.016(7) _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 Sb1 O3 1.915(2) . ? Sb1 O5 1.966(2) . ? Sb1 O4 2.025(2) . ? Sb1 O1 2.034(2) . ? Sb1 O2 2.060(2) . ? Sb1 C1 2.111(3) . ? Sb2 O3 1.928(2) 7_565 ? Sb2 O5 1.968(2) . ? Sb2 O7 1.996(2) . ? Sb2 O8 2.011(2) . ? Sb2 O6 2.058(2) . ? Sb2 C7 2.100(3) . ? Co1 O9 2.026(2) . ? Co1 N2 2.064(3) . ? Co1 O1 2.107(2) 7_565 ? Co1 O5 2.131(2) 7_565 ? Co1 O8 2.132(2) 7_565 ? Co1 O10 2.199(2) . ? P1 O10 1.500(2) 7_565 ? P1 O6 1.547(2) . ? P1 O2 1.554(2) . ? P1 C13A 1.779(7) . ? P1 C13 1.787(6) . ? P2 O9 1.489(2) . ? P2 O4 1.549(2) . ? P2 O7 1.550(2) . ? P2 C19 1.789(3) . ? N1 C27 1.337(5) . ? N1 N2 1.339(4) . ? N1 H1N 0.89(4) . ? N2 C25 1.325(4) . ? O1 C29 1.442(4) . ? O1 Co1 2.107(2) 7_565 ? O3 Sb2 1.928(2) 7_565 ? O5 Co1 2.131(2) 7_565 ? O8 C28 1.437(4) . ? O8 Co1 2.132(2) 7_565 ? O10 P1 1.500(2) 7_565 ? C1 C2 1.379(5) . ? C1 C6 1.401(5) . ? C2 C3 1.381(5) . ? C2 H2 0.9500 . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.364(5) . ? C4 Cl1 1.745(4) . ? C5 C6 1.391(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.382(5) . ? C7 C8 1.394(5) . ? C8 C9 1.390(5) . ? C8 H8 0.9500 . ? C9 C10 1.378(5) . ? C9 H9 0.9500 . ? C10 C11 1.381(5) . ? C10 Cl2 1.737(3) . ? C11 C12 1.390(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.342(9) . ? C13 C18 1.396(10) . ? C14 C15 1.411(10) . ? C14 H14 0.9500 . ? C15 C16 1.332(12) . ? C15 H15 0.9500 . ? C16 C17 1.323(12) . ? C16 H16 0.9500 . ? C17 C18 1.392(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C13A C14A 1.3900 . ? C13A C18A 1.3900 . ? C14A C15A 1.3900 . ? C14A H14A 0.9500 . ? C15A C16A 1.3900 . ? C15A H15A 0.9500 . ? C16A C17A 1.3900 . ? C16A H16A 0.9500 . ? C17A C18A 1.3900 . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C19 C20 1.382(5) . ? C19 C24 1.390(5) . ? C20 C21 1.383(5) . ? C20 H20 0.9500 . ? C21 C22 1.387(5) . ? C21 H21 0.9500 . ? C22 C23 1.368(5) . ? C22 H22 0.9500 . ? C23 C24 1.393(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.396(5) . ? C25 H25 0.9500 . ? C26 C27 1.361(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C50 O50 1.410(12) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O50A C50A 1.374(13) . ? C50A H50D 0.9800 . ? C50A H50E 0.9800 . ? C50A H50F 0.9800 . ? O51 C51 1.524(12) . ? O51 C51 1.524(12) 2_655 ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? 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 O3 Sb1 O5 93.65(9) . . ? O3 Sb1 O4 93.21(9) . . ? O5 Sb1 O4 90.07(9) . . ? O3 Sb1 O1 93.01(9) . . ? O5 Sb1 O1 78.28(9) . . ? O4 Sb1 O1 167.12(9) . . ? O3 Sb1 O2 177.63(9) . . ? O5 Sb1 O2 88.23(9) . . ? O4 Sb1 O2 85.34(9) . . ? O1 Sb1 O2 88.78(9) . . ? O3 Sb1 C1 90.42(12) . . ? O5 Sb1 C1 174.16(11) . . ? O4 Sb1 C1 93.89(11) . . ? O1 Sb1 C1 97.33(11) . . ? O2 Sb1 C1 87.82(11) . . ? O3 Sb2 O5 94.55(9) 7_565 . ? O3 Sb2 O7 90.94(9) 7_565 . ? O5 Sb2 O7 90.05(9) . . ? O3 Sb2 O8 93.27(9) 7_565 . ? O5 Sb2 O8 80.95(9) . . ? O7 Sb2 O8 170.33(9) . . ? O3 Sb2 O6 179.13(9) 7_565 . ? O5 Sb2 O6 86.14(9) . . ? O7 Sb2 O6 88.53(9) . . ? O8 Sb2 O6 87.36(9) . . ? O3 Sb2 C7 92.55(12) 7_565 . ? O5 Sb2 C7 172.05(12) . . ? O7 Sb2 C7 93.43(11) . . ? O8 Sb2 C7 95.08(11) . . ? O6 Sb2 C7 86.80(11) . . ? O9 Co1 N2 90.35(11) . . ? O9 Co1 O1 98.58(9) . 7_565 ? N2 Co1 O1 117.76(10) . 7_565 ? O9 Co1 O5 94.77(9) . 7_565 ? N2 Co1 O5 167.13(10) . 7_565 ? O1 Co1 O5 73.17(8) 7_565 7_565 ? O9 Co1 O8 96.83(9) . 7_565 ? N2 Co1 O8 93.08(10) . 7_565 ? O1 Co1 O8 145.20(8) 7_565 7_565 ? O5 Co1 O8 74.61(8) 7_565 7_565 ? O9 Co1 O10 174.33(9) . . ? N2 Co1 O10 83.99(10) . . ? O1 Co1 O10 83.95(9) 7_565 . ? O5 Co1 O10 90.81(9) 7_565 . ? O8 Co1 O10 83.72(9) 7_565 . ? O10 P1 O6 113.24(13) 7_565 . ? O10 P1 O2 111.54(13) 7_565 . ? O6 P1 O2 108.41(13) . . ? O10 P1 C13A 109.1(4) 7_565 . ? O6 P1 C13A 108.2(5) . . ? O2 P1 C13A 106.1(6) . . ? O10 P1 C13 112.7(2) 7_565 . ? O6 P1 C13 104.9(3) . . ? O2 P1 C13 105.5(3) . . ? C13A P1 C13 3.9(5) . . ? O9 P2 O4 113.97(13) . . ? O9 P2 O7 113.17(13) . . ? O4 P2 O7 110.45(12) . . ? O9 P2 C19 108.83(14) . . ? O4 P2 C19 107.13(14) . . ? O7 P2 C19 102.46(14) . . ? C27 N1 N2 112.2(3) . . ? C27 N1 H1N 129(3) . . ? N2 N1 H1N 117(3) . . ? C25 N2 N1 104.8(3) . . ? C25 N2 Co1 133.8(3) . . ? N1 N2 Co1 117.7(2) . . ? C29 O1 Sb1 121.25(19) . . ? C29 O1 Co1 121.15(19) . 7_565 ? Sb1 O1 Co1 102.38(9) . 7_565 ? P1 O2 Sb1 122.93(13) . . ? Sb1 O3 Sb2 145.36(12) . 7_565 ? P2 O4 Sb1 137.05(14) . . ? Sb1 O5 Sb2 137.95(12) . . ? Sb1 O5 Co1 103.87(9) . 7_565 ? Sb2 O5 Co1 102.37(9) . 7_565 ? P1 O6 Sb2 125.23(13) . . ? P2 O7 Sb2 138.68(14) . . ? C28 O8 Sb2 119.46(19) . . ? C28 O8 Co1 120.41(19) . 7_565 ? Sb2 O8 Co1 100.89(9) . 7_565 ? P2 O9 Co1 139.80(14) . . ? P1 O10 Co1 114.60(13) 7_565 . ? C2 C1 C6 117.6(3) . . ? C2 C1 Sb1 123.2(3) . . ? C6 C1 Sb1 119.1(3) . . ? C1 C2 C3 121.7(4) . . ? C1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? C2 C3 C4 119.0(4) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 121.4(3) . . ? C5 C4 Cl1 118.9(3) . . ? C3 C4 Cl1 119.7(3) . . ? C4 C5 C6 118.8(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C5 C6 C1 121.4(3) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? C12 C7 C8 119.5(3) . . ? C12 C7 Sb2 121.2(3) . . ? C8 C7 Sb2 119.2(3) . . ? C9 C8 C7 120.4(3) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 118.7(3) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C11 122.1(3) . . ? C9 C10 Cl2 118.1(3) . . ? C11 C10 Cl2 119.8(3) . . ? C10 C11 C12 118.6(3) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C7 C12 C11 120.7(3) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C18 117.5(6) . . ? C14 C13 P1 121.1(6) . . ? C18 C13 P1 121.4(6) . . ? C13 C14 C15 119.5(8) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 123.1(8) . . ? C16 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C17 C16 C15 117.7(8) . . ? C17 C16 H16 121.2 . . ? C15 C16 H16 121.2 . . ? C16 C17 C18 122.1(8) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C17 C18 C13 120.2(7) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C14A C13A C18A 120.0 . . ? C14A C13A P1 121.3(6) . . ? C18A C13A P1 118.7(6) . . ? C13A C14A C15A 120.0 . . ? C13A C14A H14A 120.0 . . ? C15A C14A H14A 120.0 . . ? C16A C15A C14A 120.0 . . ? C16A C15A H15A 120.0 . . ? C14A C15A H15A 120.0 . . ? C17A C16A C15A 120.0 . . ? C17A C16A H16A 120.0 . . ? C15A C16A H16A 120.0 . . ? C16A C17A C18A 120.0 . . ? C16A C17A H17A 120.0 . . ? C18A C17A H17A 120.0 . . ? C17A C18A C13A 120.0 . . ? C17A C18A H18A 120.0 . . ? C13A C18A H18A 120.0 . . ? C20 C19 C24 118.5(3) . . ? C20 C19 P2 119.5(3) . . ? C24 C19 P2 121.7(3) . . ? C19 C20 C21 120.8(4) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C22 120.2(4) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.7(4) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 120.1(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C19 C24 C23 120.6(4) . . ? C19 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? N2 C25 C26 111.2(4) . . ? N2 C25 H25 124.4 . . ? C26 C25 H25 124.4 . . ? C27 C26 C25 104.7(3) . . ? C27 C26 H26 127.7 . . ? C25 C26 H26 127.7 . . ? N1 C27 C26 107.2(4) . . ? N1 C27 H27 126.4 . . ? C26 C27 H27 126.4 . . ? O8 C28 H28A 109.5 . . ? O8 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O8 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O1 C29 H29A 109.5 . . ? O1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O50 C50 H50A 109.5 . . ? O50 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O50 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O50A C50A H50D 109.5 . . ? O50A C50A H50E 109.5 . . ? H50D C50A H50E 109.5 . . ? O50A C50A H50F 109.5 . . ? H50D C50A H50F 109.5 . . ? H50E C50A H50F 109.5 . . ? C51 O51 C51 127.7(15) . 2_655 ? O51 C51 H51A 109.5 . . ? O51 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O51 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? 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 C27 N1 N2 C25 0.2(4) . . . . ? C27 N1 N2 Co1 -161.0(3) . . . . ? O9 Co1 N2 C25 14.3(3) . . . . ? O1 Co1 N2 C25 114.2(3) 7_565 . . . ? O5 Co1 N2 C25 -99.3(6) 7_565 . . . ? O8 Co1 N2 C25 -82.6(3) 7_565 . . . ? O10 Co1 N2 C25 -165.9(3) . . . . ? O9 Co1 N2 N1 168.6(3) . . . . ? O1 Co1 N2 N1 -91.5(3) 7_565 . . . ? O5 Co1 N2 N1 55.1(6) 7_565 . . . ? O8 Co1 N2 N1 71.8(3) 7_565 . . . ? O10 Co1 N2 N1 -11.6(3) . . . . ? O3 Sb1 O1 C29 116.3(2) . . . . ? O5 Sb1 O1 C29 -150.6(2) . . . . ? O4 Sb1 O1 C29 -125.0(4) . . . . ? O2 Sb1 O1 C29 -62.2(2) . . . . ? C1 Sb1 O1 C29 25.5(3) . . . . ? O3 Sb1 O1 Co1 -104.92(10) . . . 7_565 ? O5 Sb1 O1 Co1 -11.81(10) . . . 7_565 ? O4 Sb1 O1 Co1 13.9(5) . . . 7_565 ? O2 Sb1 O1 Co1 76.64(10) . . . 7_565 ? C1 Sb1 O1 Co1 164.28(12) . . . 7_565 ? O10 P1 O2 Sb1 58.30(19) 7_565 . . . ? O6 P1 O2 Sb1 -67.05(17) . . . . ? C13A P1 O2 Sb1 176.9(4) . . . . ? C13 P1 O2 Sb1 -179.0(3) . . . . ? O3 Sb1 O2 P1 159(2) . . . . ? O5 Sb1 O2 P1 16.46(15) . . . . ? O4 Sb1 O2 P1 106.68(16) . . . . ? O1 Sb1 O2 P1 -61.85(15) . . . . ? C1 Sb1 O2 P1 -159.24(17) . . . . ? O5 Sb1 O3 Sb2 13.2(2) . . . 7_565 ? O4 Sb1 O3 Sb2 -77.0(2) . . . 7_565 ? O1 Sb1 O3 Sb2 91.7(2) . . . 7_565 ? O2 Sb1 O3 Sb2 -129(2) . . . 7_565 ? C1 Sb1 O3 Sb2 -171.0(2) . . . 7_565 ? O9 P2 O4 Sb1 -94.1(2) . . . . ? O7 P2 O4 Sb1 34.6(3) . . . . ? C19 P2 O4 Sb1 145.5(2) . . . . ? O3 Sb1 O4 P2 82.7(2) . . . . ? O5 Sb1 O4 P2 -10.9(2) . . . . ? O1 Sb1 O4 P2 -36.0(6) . . . . ? O2 Sb1 O4 P2 -99.1(2) . . . . ? C1 Sb1 O4 P2 173.4(2) . . . . ? O3 Sb1 O5 Sb2 -128.83(18) . . . . ? O4 Sb1 O5 Sb2 -35.62(18) . . . . ? O1 Sb1 O5 Sb2 138.84(19) . . . . ? O2 Sb1 O5 Sb2 49.72(18) . . . . ? C1 Sb1 O5 Sb2 97.2(11) . . . . ? O3 Sb1 O5 Co1 104.07(10) . . . 7_565 ? O4 Sb1 O5 Co1 -162.71(10) . . . 7_565 ? O1 Sb1 O5 Co1 11.75(10) . . . 7_565 ? O2 Sb1 O5 Co1 -77.37(10) . . . 7_565 ? C1 Sb1 O5 Co1 -29.9(12) . . . 7_565 ? O3 Sb2 O5 Sb1 131.32(18) 7_565 . . . ? O7 Sb2 O5 Sb1 40.38(18) . . . . ? O8 Sb2 O5 Sb1 -136.08(19) . . . . ? O6 Sb2 O5 Sb1 -48.14(17) . . . . ? C7 Sb2 O5 Sb1 -75.6(8) . . . . ? O3 Sb2 O5 Co1 -101.12(10) 7_565 . . 7_565 ? O7 Sb2 O5 Co1 167.93(10) . . . 7_565 ? O8 Sb2 O5 Co1 -8.53(10) . . . 7_565 ? O6 Sb2 O5 Co1 79.41(10) . . . 7_565 ? C7 Sb2 O5 Co1 51.9(8) . . . 7_565 ? O10 P1 O6 Sb2 -53.33(19) 7_565 . . . ? O2 P1 O6 Sb2 71.01(17) . . . . ? C13A P1 O6 Sb2 -174.3(5) . . . . ? C13 P1 O6 Sb2 -176.6(3) . . . . ? O3 Sb2 O6 P1 -163(6) 7_565 . . . ? O5 Sb2 O6 P1 -20.21(15) . . . . ? O7 Sb2 O6 P1 -110.36(15) . . . . ? O8 Sb2 O6 P1 60.89(15) . . . . ? C7 Sb2 O6 P1 156.12(17) . . . . ? O9 P2 O7 Sb2 104.2(2) . . . . ? O4 P2 O7 Sb2 -24.9(3) . . . . ? C19 P2 O7 Sb2 -138.8(2) . . . . ? O3 Sb2 O7 P2 -97.9(2) 7_565 . . . ? O5 Sb2 O7 P2 -3.3(2) . . . . ? O8 Sb2 O7 P2 17.9(7) . . . . ? O6 Sb2 O7 P2 82.8(2) . . . . ? C7 Sb2 O7 P2 169.5(2) . . . . ? O3 Sb2 O8 C28 -31.9(2) 7_565 . . . ? O5 Sb2 O8 C28 -126.0(2) . . . . ? O7 Sb2 O8 C28 -147.6(5) . . . . ? O6 Sb2 O8 C28 147.5(2) . . . . ? C7 Sb2 O8 C28 60.9(2) . . . . ? O3 Sb2 O8 Co1 102.57(10) 7_565 . . 7_565 ? O5 Sb2 O8 Co1 8.48(10) . . . 7_565 ? O7 Sb2 O8 Co1 -13.1(6) . . . 7_565 ? O6 Sb2 O8 Co1 -78.03(10) . . . 7_565 ? C7 Sb2 O8 Co1 -164.58(12) . . . 7_565 ? O4 P2 O9 Co1 72.7(2) . . . . ? O7 P2 O9 Co1 -54.7(2) . . . . ? C19 P2 O9 Co1 -167.9(2) . . . . ? N2 Co1 O9 P2 -174.9(2) . . . . ? O1 Co1 O9 P2 66.9(2) 7_565 . . . ? O5 Co1 O9 P2 -6.7(2) 7_565 . . . ? O8 Co1 O9 P2 -81.8(2) 7_565 . . . ? O10 Co1 O9 P2 -177.0(8) . . . . ? O9 Co1 O10 P1 168.4(8) . . . 7_565 ? N2 Co1 O10 P1 166.35(15) . . . 7_565 ? O1 Co1 O10 P1 -74.82(14) 7_565 . . 7_565 ? O5 Co1 O10 P1 -1.84(14) 7_565 . . 7_565 ? O8 Co1 O10 P1 72.57(13) 7_565 . . 7_565 ? O3 Sb1 C1 C2 160.6(3) . . . . ? O5 Sb1 C1 C2 -65.3(12) . . . . ? O4 Sb1 C1 C2 67.3(3) . . . . ? O1 Sb1 C1 C2 -106.4(3) . . . . ? O2 Sb1 C1 C2 -17.9(3) . . . . ? O3 Sb1 C1 C6 -20.9(3) . . . . ? O5 Sb1 C1 C6 113.2(11) . . . . ? O4 Sb1 C1 C6 -114.2(3) . . . . ? O1 Sb1 C1 C6 72.2(3) . . . . ? O2 Sb1 C1 C6 160.7(3) . . . . ? C6 C1 C2 C3 0.9(6) . . . . ? Sb1 C1 C2 C3 179.5(3) . . . . ? C1 C2 C3 C4 -1.5(6) . . . . ? C2 C3 C4 C5 0.8(6) . . . . ? C2 C3 C4 Cl1 -179.2(3) . . . . ? C3 C4 C5 C6 0.3(6) . . . . ? Cl1 C4 C5 C6 -179.7(3) . . . . ? C4 C5 C6 C1 -0.9(6) . . . . ? C2 C1 C6 C5 0.3(5) . . . . ? Sb1 C1 C6 C5 -178.3(3) . . . . ? O3 Sb2 C7 C12 -41.1(3) 7_565 . . . ? O5 Sb2 C7 C12 165.8(7) . . . . ? O7 Sb2 C7 C12 50.0(3) . . . . ? O8 Sb2 C7 C12 -134.6(3) . . . . ? O6 Sb2 C7 C12 138.3(3) . . . . ? O3 Sb2 C7 C8 136.3(3) 7_565 . . . ? O5 Sb2 C7 C8 -16.8(10) . . . . ? O7 Sb2 C7 C8 -132.6(3) . . . . ? O8 Sb2 C7 C8 42.8(3) . . . . ? O6 Sb2 C7 C8 -44.2(3) . . . . ? C12 C7 C8 C9 1.0(5) . . . . ? Sb2 C7 C8 C9 -176.4(3) . . . . ? C7 C8 C9 C10 -1.7(6) . . . . ? C8 C9 C10 C11 1.4(6) . . . . ? C8 C9 C10 Cl2 -178.3(3) . . . . ? C9 C10 C11 C12 -0.5(6) . . . . ? Cl2 C10 C11 C12 179.3(3) . . . . ? C8 C7 C12 C11 -0.1(5) . . . . ? Sb2 C7 C12 C11 177.3(3) . . . . ? C10 C11 C12 C7 -0.2(5) . . . . ? O10 P1 C13 C14 53.9(8) 7_565 . . . ? O6 P1 C13 C14 177.5(7) . . . . ? O2 P1 C13 C14 -68.1(8) . . . . ? C13A P1 C13 C14 31(11) . . . . ? O10 P1 C13 C18 -125.4(6) 7_565 . . . ? O6 P1 C13 C18 -1.8(8) . . . . ? O2 P1 C13 C18 112.6(7) . . . . ? C13A P1 C13 C18 -149(12) . . . . ? C18 C13 C14 C15 -1.3(13) . . . . ? P1 C13 C14 C15 179.4(6) . . . . ? C13 C14 C15 C16 0.5(16) . . . . ? C14 C15 C16 C17 0.2(17) . . . . ? C15 C16 C17 C18 0.1(16) . . . . ? C16 C17 C18 C13 -1.0(14) . . . . ? C14 C13 C18 C17 1.5(12) . . . . ? P1 C13 C18 C17 -179.1(5) . . . . ? O10 P1 C13A C14A 7.7(11) 7_565 . . . ? O6 P1 C13A C14A 131.3(9) . . . . ? O2 P1 C13A C14A -112.5(9) . . . . ? C13 P1 C13A C14A 165(12) . . . . ? O10 P1 C13A C18A -173.0(8) 7_565 . . . ? O6 P1 C13A C18A -49.5(10) . . . . ? O2 P1 C13A C18A 66.7(9) . . . . ? C13 P1 C13A C18A -16(11) . . . . ? C18A C13A C14A C15A 0.0 . . . . ? P1 C13A C14A C15A 179.2(14) . . . . ? C13A C14A C15A C16A 0.0 . . . . ? C14A C15A C16A C17A 0.0 . . . . ? C15A C16A C17A C18A 0.0 . . . . ? C16A C17A C18A C13A 0.0 . . . . ? C14A C13A C18A C17A 0.0 . . . . ? P1 C13A C18A C17A -179.3(14) . . . . ? O9 P2 C19 C20 164.5(3) . . . . ? O4 P2 C19 C20 -71.8(3) . . . . ? O7 P2 C19 C20 44.4(3) . . . . ? O9 P2 C19 C24 -9.3(3) . . . . ? O4 P2 C19 C24 114.4(3) . . . . ? O7 P2 C19 C24 -129.4(3) . . . . ? C24 C19 C20 C21 -0.5(6) . . . . ? P2 C19 C20 C21 -174.5(3) . . . . ? C19 C20 C21 C22 -0.4(6) . . . . ? C20 C21 C22 C23 -0.3(6) . . . . ? C21 C22 C23 C24 1.9(6) . . . . ? C20 C19 C24 C23 2.1(5) . . . . ? P2 C19 C24 C23 176.0(3) . . . . ? C22 C23 C24 C19 -2.8(5) . . . . ? N1 N2 C25 C26 0.1(4) . . . . ? Co1 N2 C25 C26 156.7(3) . . . . ? N2 C25 C26 C27 -0.3(5) . . . . ? N2 N1 C27 C26 -0.4(5) . . . . ? C25 C26 C27 N1 0.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.165 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.105 # Attachment '- 8.cif' data_tri818 _database_code_depnum_ccdc_archive 'CCDC 778678' #TrackingRef '- 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H66 Cl4 Co2 N2 O20 P4 Sb4' _chemical_formula_weight 2173.83 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 12.4607(4) _cell_length_b 12.8811(4) _cell_length_c 13.7595(4) _cell_angle_alpha 83.906(2) _cell_angle_beta 73.185(2) _cell_angle_gamma 75.036(3) _cell_volume 2041.20(11) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13181 _cell_measurement_theta_min 2.6391 _cell_measurement_theta_max 28.5352 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1070 _exptl_absorpt_coefficient_mu 1.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5046 _exptl_absorpt_correction_T_max 0.8265 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21231 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8295 _reflns_number_gt 6250 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0471P)^2^+1.6879P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8295 _refine_ls_number_parameters 486 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.001 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 Sb1 Sb 1.05612(2) 0.977077(19) 0.167704(18) 0.01398(7) Uani 1 1 d . . . Sb2 Sb 0.82597(2) 0.912970(19) 0.085597(18) 0.01416(7) Uani 1 1 d . . . Co1 Co 0.80362(4) 1.13415(4) 0.18797(4) 0.01600(12) Uani 1 1 d . . . P1 P 1.09349(8) 0.75995(7) 0.04038(7) 0.0148(2) Uani 1 1 d . . . P2 P 0.82797(8) 0.92113(8) 0.31459(7) 0.0162(2) Uani 1 1 d . . . O1 O 0.8380(2) 1.2376(2) 0.0693(2) 0.0190(6) Uani 1 1 d . . . O2 O 0.9613(2) 1.11959(19) 0.22821(19) 0.0173(6) Uani 1 1 d . . . O3 O 0.9257(2) 0.99874(19) 0.10809(19) 0.0153(5) Uani 1 1 d . . . O4 O 0.7073(2) 1.0522(2) 0.12994(19) 0.0171(6) Uani 1 1 d . . . O5 O 0.9602(2) 0.9054(2) 0.29000(19) 0.0179(6) Uani 1 1 d . . . O6 O 1.1225(2) 0.8317(2) 0.10684(19) 0.0186(6) Uani 1 1 d . . . O7 O 1.1513(2) 1.0429(2) 0.05478(18) 0.0164(6) Uani 1 1 d . . . O8 O 0.8009(2) 0.8626(2) 0.23540(19) 0.0178(6) Uani 1 1 d . . . O9 O 0.7633(2) 1.0371(2) 0.32113(19) 0.0182(6) Uani 1 1 d . . . O10 O 0.9613(2) 0.7855(2) 0.0531(2) 0.0182(6) Uani 1 1 d . . . N1 N 0.6720(3) 1.2607(2) 0.2619(2) 0.0183(7) Uani 1 1 d . . . C1 C 0.6444(3) 1.2706(3) 0.3617(3) 0.0208(9) Uani 1 1 d . . . H1 H 0.6904 1.2226 0.3994 0.025 Uiso 1 1 calc R . . C2 C 0.5505(4) 1.3487(3) 0.4137(3) 0.0238(9) Uani 1 1 d . . . H2 H 0.5360 1.3553 0.4847 0.029 Uiso 1 1 calc R . . C3 C 0.4785(3) 1.4168(3) 0.3611(3) 0.0218(9) Uani 1 1 d . . . C4 C 0.5086(3) 1.4062(3) 0.2561(3) 0.0234(9) Uani 1 1 d . . . H4 H 0.4634 1.4520 0.2164 0.028 Uiso 1 1 calc R . . C5 C 0.6044(3) 1.3290(3) 0.2105(3) 0.0229(9) Uani 1 1 d . . . H5 H 0.6240 1.3236 0.1389 0.027 Uiso 1 1 calc R . . C6 C 0.3725(4) 1.4956(3) 0.4124(3) 0.0267(9) Uani 1 1 d . . . C7 C 0.3078(4) 1.4711(4) 0.5094(4) 0.0358(11) Uani 1 1 d . . . H7 H 0.3323 1.4046 0.5430 0.043 Uiso 1 1 calc R . . C8 C 0.2064(4) 1.5450(4) 0.5570(4) 0.0448(13) Uani 1 1 d . . . H8 H 0.1620 1.5282 0.6228 0.054 Uiso 1 1 calc R . . C9 C 0.1708(4) 1.6416(4) 0.5092(4) 0.0430(13) Uani 1 1 d . . . H9 H 0.1023 1.6913 0.5424 0.052 Uiso 1 1 calc R . . C10 C 0.2336(4) 1.6669(4) 0.4138(4) 0.0360(11) Uani 1 1 d . . . H10 H 0.2083 1.7335 0.3809 0.043 Uiso 1 1 calc R . . C11 C 0.3345(4) 1.5943(3) 0.3657(3) 0.0280(10) Uani 1 1 d . . . H11 H 0.3782 1.6122 0.3000 0.034 Uiso 1 1 calc R . . C13 C 1.1268(3) 0.6260(3) 0.0921(3) 0.0173(8) Uani 1 1 d . . . C14 C 1.1255(4) 0.5403(3) 0.0395(3) 0.0312(10) Uani 1 1 d . . . H14 H 1.1115 0.5526 -0.0255 0.037 Uiso 1 1 calc R . . C15 C 1.1446(4) 0.4364(3) 0.0819(4) 0.0357(11) Uani 1 1 d . . . H15 H 1.1435 0.3779 0.0458 0.043 Uiso 1 1 calc R . . C16 C 1.1649(4) 0.4186(4) 0.1752(4) 0.0373(12) Uani 1 1 d . . . H16 H 1.1772 0.3476 0.2040 0.045 Uiso 1 1 calc R . . C17 C 1.1678(5) 0.5015(4) 0.2277(4) 0.0470(14) Uani 1 1 d . . . H17 H 1.1832 0.4881 0.2922 0.056 Uiso 1 1 calc R . . C18 C 1.1480(4) 0.6059(3) 0.1862(4) 0.0355(11) Uani 1 1 d . . . H18 H 1.1491 0.6638 0.2231 0.043 Uiso 1 1 calc R . . C19 C 0.7131(3) 0.8193(3) 0.0763(3) 0.0180(8) Uani 1 1 d . . . C20 C 0.6994(3) 0.7288(3) 0.1407(3) 0.0221(9) Uani 1 1 d . . . H20 H 0.7407 0.7100 0.1907 0.027 Uiso 1 1 calc R . . C21 C 0.6276(4) 0.6666(3) 0.1333(3) 0.0263(9) Uani 1 1 d . . . H21 H 0.6195 0.6052 0.1770 0.032 Uiso 1 1 calc R . . C22 C 0.5670(4) 0.6960(3) 0.0601(3) 0.0270(10) Uani 1 1 d . . . C23 C 0.5798(4) 0.7830(3) -0.0057(3) 0.0278(10) Uani 1 1 d . . . H23 H 0.5385 0.8011 -0.0557 0.033 Uiso 1 1 calc R . . C24 C 0.6541(4) 0.8440(3) 0.0020(3) 0.0253(9) Uani 1 1 d . . . H24 H 0.6646 0.9033 -0.0441 0.030 Uiso 1 1 calc R . . C25 C 1.18421(17) 0.9474(2) 0.24538(17) 0.0176(7) Uani 1 1 d GU . . C26 C 1.15683(15) 0.9645(2) 0.34867(16) 0.0220(7) Uani 1 1 d GU . . H26 H 1.0790 0.9932 0.3853 0.026 Uiso 1 1 calc R . . C27 C 1.2433(2) 0.9396(2) 0.39837(13) 0.0239(7) Uani 1 1 d GU . . H27 H 1.2246 0.9513 0.4690 0.029 Uiso 1 1 calc R . . C28 C 1.35712(17) 0.8975(2) 0.34477(17) 0.0235(7) Uani 1 1 d GU . . C29 C 1.38450(14) 0.8804(2) 0.24148(17) 0.0227(7) Uani 1 1 d GU . . H29 H 1.4623 0.8517 0.2049 0.027 Uiso 1 1 calc R . . C30 C 1.29805(19) 0.9053(2) 0.19179(13) 0.0212(7) Uani 1 1 d GU . . H30 H 1.3168 0.8936 0.1212 0.025 Uiso 1 1 calc R . . C31 C 0.8662(4) 0.7664(4) 0.4663(3) 0.0314(11) Uani 1 1 d . . . H31 H 0.9433 0.7446 0.4250 0.038 Uiso 1 1 calc R . . C32 C 0.7885(3) 0.8496(3) 0.4330(3) 0.0188(8) Uani 1 1 d . . . C33 C 0.6743(3) 0.8797(3) 0.4942(3) 0.0225(9) Uani 1 1 d . . . H33 H 0.6202 0.9369 0.4723 0.027 Uiso 1 1 calc R . . C34 C 0.6405(4) 0.8262(4) 0.5860(3) 0.0296(10) Uani 1 1 d . . . H34 H 0.5630 0.8460 0.6269 0.036 Uiso 1 1 calc R . . C35 C 0.7188(4) 0.7445(4) 0.6177(3) 0.0356(12) Uani 1 1 d . . . H39 H 0.6950 0.7076 0.6807 0.043 Uiso 1 1 calc R . . C36 C 0.8319(4) 0.7148(4) 0.5597(4) 0.0407(13) Uani 1 1 d . . . H38 H 0.8859 0.6593 0.5837 0.049 Uiso 1 1 calc R . . C37 C 1.0150(3) 1.2069(3) 0.2208(3) 0.0259(9) Uani 1 1 d . . . H40A H 1.0794 1.1847 0.2517 0.039 Uiso 1 1 calc R . . H40B H 0.9584 1.2684 0.2566 0.039 Uiso 1 1 calc R . . H40C H 1.0439 1.2275 0.1492 0.039 Uiso 1 1 calc R . . C38 C 0.5903(3) 1.0490(3) 0.1827(3) 0.0236(9) Uani 1 1 d . . . H37A H 0.5555 1.0235 0.1373 0.035 Uiso 1 1 calc R . . H37B H 0.5458 1.1213 0.2046 0.035 Uiso 1 1 calc R . . H37C H 0.5898 1.0000 0.2423 0.035 Uiso 1 1 calc R . . Cl1 Cl 0.47131(12) 0.62213(10) 0.05174(10) 0.0455(3) Uani 1 1 d . . . Cl2 Cl 1.46605(9) 0.86171(9) 0.40429(8) 0.0316(2) Uani 1 1 d . . . 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 Sb1 0.01591(13) 0.01239(13) 0.01366(13) 0.00112(9) -0.00388(10) -0.00420(10) Sb2 0.01557(13) 0.01285(13) 0.01410(13) 0.00159(9) -0.00364(10) -0.00474(10) Co1 0.0181(3) 0.0131(3) 0.0153(3) 0.0007(2) -0.0032(2) -0.0030(2) P1 0.0162(5) 0.0103(5) 0.0175(5) 0.0011(4) -0.0053(4) -0.0025(4) P2 0.0188(5) 0.0150(5) 0.0141(5) 0.0023(4) -0.0035(4) -0.0050(4) O1 0.0208(14) 0.0133(13) 0.0203(14) -0.0005(11) -0.0040(11) -0.0014(11) O2 0.0240(14) 0.0104(13) 0.0173(14) -0.0013(10) -0.0039(11) -0.0052(11) O3 0.0160(13) 0.0137(13) 0.0177(14) -0.0006(10) -0.0070(11) -0.0036(10) O4 0.0141(13) 0.0154(13) 0.0180(14) 0.0032(11) -0.0014(11) -0.0019(11) O5 0.0215(14) 0.0173(14) 0.0140(13) 0.0036(10) -0.0029(11) -0.0067(11) O6 0.0175(13) 0.0177(14) 0.0184(14) -0.0035(11) -0.0049(11) 0.0011(11) O7 0.0189(13) 0.0205(14) 0.0107(13) 0.0039(10) -0.0027(11) -0.0099(11) O8 0.0226(14) 0.0186(14) 0.0135(13) 0.0024(11) -0.0046(11) -0.0089(11) O9 0.0222(14) 0.0158(14) 0.0140(13) 0.0000(10) -0.0015(11) -0.0044(11) O10 0.0180(13) 0.0146(13) 0.0210(14) -0.0020(11) -0.0022(11) -0.0050(11) N1 0.0213(17) 0.0146(16) 0.0174(17) 0.0002(13) -0.0033(14) -0.0042(13) C1 0.020(2) 0.018(2) 0.024(2) 0.0035(16) -0.0087(17) -0.0030(16) C2 0.031(2) 0.020(2) 0.019(2) -0.0014(16) -0.0043(18) -0.0063(18) C3 0.019(2) 0.016(2) 0.029(2) -0.0007(17) -0.0039(17) -0.0057(16) C4 0.024(2) 0.020(2) 0.024(2) 0.0028(17) -0.0066(18) -0.0030(17) C5 0.031(2) 0.019(2) 0.015(2) -0.0006(16) -0.0012(17) -0.0054(18) C6 0.027(2) 0.025(2) 0.027(2) -0.0072(18) -0.0049(19) -0.0055(18) C7 0.034(3) 0.032(3) 0.036(3) -0.003(2) -0.005(2) -0.002(2) C8 0.032(3) 0.056(3) 0.036(3) -0.012(2) 0.005(2) -0.005(2) C9 0.029(3) 0.042(3) 0.054(3) -0.021(3) -0.010(2) 0.003(2) C10 0.031(3) 0.027(2) 0.050(3) -0.009(2) -0.015(2) 0.001(2) C11 0.028(2) 0.021(2) 0.035(3) -0.0044(18) -0.009(2) -0.0038(18) C13 0.0142(18) 0.0159(19) 0.020(2) 0.0028(15) -0.0022(16) -0.0043(15) C14 0.049(3) 0.020(2) 0.023(2) 0.0022(17) -0.008(2) -0.008(2) C15 0.053(3) 0.017(2) 0.039(3) -0.0017(19) -0.013(2) -0.011(2) C16 0.051(3) 0.021(2) 0.046(3) 0.013(2) -0.023(2) -0.013(2) C17 0.082(4) 0.031(3) 0.047(3) 0.020(2) -0.042(3) -0.026(3) C18 0.058(3) 0.020(2) 0.038(3) 0.0075(19) -0.024(2) -0.016(2) C19 0.020(2) 0.022(2) 0.0121(18) -0.0023(15) -0.0021(16) -0.0077(16) C20 0.022(2) 0.027(2) 0.021(2) 0.0010(17) -0.0112(17) -0.0065(17) C21 0.031(2) 0.020(2) 0.030(2) 0.0045(18) -0.0090(19) -0.0123(18) C22 0.033(2) 0.028(2) 0.029(2) 0.0027(18) -0.0125(19) -0.019(2) C23 0.036(2) 0.028(2) 0.029(2) 0.0072(18) -0.020(2) -0.014(2) C24 0.042(3) 0.019(2) 0.017(2) 0.0046(16) -0.0085(19) -0.0123(19) C25 0.0198(14) 0.0161(15) 0.0191(15) 0.0019(13) -0.0065(13) -0.0078(13) C26 0.0243(15) 0.0193(16) 0.0223(15) 0.0003(13) -0.0050(13) -0.0068(13) C27 0.0285(16) 0.0232(16) 0.0216(16) 0.0001(13) -0.0076(13) -0.0082(14) C28 0.0252(15) 0.0238(16) 0.0235(15) 0.0031(14) -0.0105(14) -0.0066(14) C29 0.0212(15) 0.0228(16) 0.0241(16) -0.0010(13) -0.0049(13) -0.0064(13) C30 0.0231(15) 0.0208(16) 0.0201(15) 0.0003(13) -0.0047(13) -0.0080(13) C31 0.022(2) 0.031(2) 0.033(3) 0.009(2) -0.0009(19) -0.0040(19) C32 0.020(2) 0.021(2) 0.018(2) 0.0003(16) -0.0051(16) -0.0095(16) C33 0.022(2) 0.024(2) 0.023(2) 0.0017(17) -0.0079(17) -0.0074(17) C34 0.027(2) 0.040(3) 0.024(2) 0.0027(19) -0.0024(19) -0.018(2) C35 0.040(3) 0.048(3) 0.026(2) 0.019(2) -0.015(2) -0.025(2) C36 0.035(3) 0.042(3) 0.042(3) 0.025(2) -0.014(2) -0.010(2) C37 0.024(2) 0.017(2) 0.036(3) -0.0076(18) 0.0001(19) -0.0108(17) C38 0.0157(19) 0.026(2) 0.025(2) -0.0006(17) 0.0008(17) -0.0061(17) Cl1 0.0659(9) 0.0476(8) 0.0472(8) 0.0164(6) -0.0333(7) -0.0424(7) Cl2 0.0293(6) 0.0384(6) 0.0319(6) 0.0051(5) -0.0176(5) -0.0083(5) _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 Sb1 O7 1.927(2) . ? Sb1 O3 1.970(2) . ? Sb1 O6 2.007(3) . ? Sb1 O2 2.023(2) . ? Sb1 O5 2.046(2) . ? Sb1 C25 2.1027(17) . ? Sb2 O7 1.915(2) 2_775 ? Sb2 O3 1.965(2) . ? Sb2 O10 2.008(2) . ? Sb2 O4 2.029(2) . ? Sb2 O8 2.053(2) . ? Sb2 C19 2.112(4) . ? Co1 O1 2.013(3) . ? Co1 N1 2.095(3) . ? Co1 O9 2.116(2) . ? Co1 O4 2.140(3) . ? Co1 O2 2.150(3) . ? Co1 O3 2.152(2) . ? P1 O1 1.505(3) 2_775 ? P1 O6 1.537(3) . ? P1 O10 1.555(3) . ? P1 C13 1.787(4) . ? P2 O9 1.501(3) . ? P2 O8 1.545(3) . ? P2 O5 1.546(3) . ? P2 C32 1.788(4) . ? O1 P1 1.505(3) 2_775 ? O2 C37 1.431(4) . ? O4 C38 1.438(4) . ? O7 Sb2 1.915(2) 2_775 ? N1 C1 1.327(5) . ? N1 C5 1.346(5) . ? C1 C2 1.397(5) . ? C1 H1 0.9500 . ? C2 C3 1.390(6) . ? C2 H2 0.9500 . ? C3 C4 1.395(6) . ? C3 C6 1.481(5) . ? C4 C5 1.376(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C11 1.394(6) . ? C6 C7 1.397(6) . ? C7 C8 1.401(6) . ? C7 H7 0.9500 . ? C8 C9 1.373(7) . ? C8 H8 0.9500 . ? C9 C10 1.374(7) . ? C9 H9 0.9500 . ? C10 C11 1.391(6) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C13 C18 1.380(6) . ? C13 C14 1.389(6) . ? C14 C15 1.392(6) . ? C14 H14 0.9500 . ? C15 C16 1.364(7) . ? C15 H15 0.9500 . ? C16 C17 1.365(7) . ? C16 H16 0.9500 . ? C17 C18 1.394(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.391(6) . ? C19 C20 1.403(5) . ? C20 C21 1.377(6) . ? C20 H20 0.9500 . ? C21 C22 1.392(6) . ? C21 H21 0.9500 . ? C22 C23 1.376(6) . ? C22 Cl1 1.740(4) . ? C23 C24 1.391(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.3900 . ? C28 Cl2 1.7221(19) . ? C29 C30 1.3900 . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.382(6) . ? C31 C36 1.388(6) . ? C31 H31 0.9500 . ? C32 C33 1.406(5) . ? C33 C34 1.380(6) . ? C33 H33 0.9500 . ? C34 C35 1.367(6) . ? C34 H34 0.9500 . ? C35 C36 1.380(7) . ? C35 H39 0.9500 . ? C36 H38 0.9500 . ? C37 H40A 0.9800 . ? C37 H40B 0.9800 . ? C37 H40C 0.9800 . ? C38 H37A 0.9800 . ? C38 H37B 0.9800 . ? C38 H37C 0.9800 . ? 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 O7 Sb1 O3 95.42(10) . . ? O7 Sb1 O6 91.85(11) . . ? O3 Sb1 O6 89.97(10) . . ? O7 Sb1 O2 93.61(10) . . ? O3 Sb1 O2 80.65(10) . . ? O6 Sb1 O2 169.55(10) . . ? O7 Sb1 O5 177.80(10) . . ? O3 Sb1 O5 86.76(10) . . ? O6 Sb1 O5 87.88(10) . . ? O2 Sb1 O5 87.01(10) . . ? O7 Sb1 C25 90.71(10) . . ? O3 Sb1 C25 173.85(10) . . ? O6 Sb1 C25 90.30(10) . . ? O2 Sb1 C25 98.53(10) . . ? O5 Sb1 C25 87.11(10) . . ? O7 Sb2 O3 93.54(10) 2_775 . ? O7 Sb2 O10 92.00(11) 2_775 . ? O3 Sb2 O10 90.29(10) . . ? O7 Sb2 O4 91.75(10) 2_775 . ? O3 Sb2 O4 79.84(10) . . ? O10 Sb2 O4 169.64(10) . . ? O7 Sb2 O8 178.74(10) 2_775 . ? O3 Sb2 O8 87.58(10) . . ? O10 Sb2 O8 87.43(10) . . ? O4 Sb2 O8 89.01(10) . . ? O7 Sb2 C19 91.64(13) 2_775 . ? O3 Sb2 C19 174.65(12) . . ? O10 Sb2 C19 90.86(13) . . ? O4 Sb2 C19 98.68(13) . . ? O8 Sb2 C19 87.25(12) . . ? O1 Co1 N1 87.48(11) . . ? O1 Co1 O9 174.96(10) . . ? N1 Co1 O9 88.27(11) . . ? O1 Co1 O4 98.10(10) . . ? N1 Co1 O4 100.90(11) . . ? O9 Co1 O4 85.37(10) . . ? O1 Co1 O2 95.39(10) . . ? N1 Co1 O2 111.74(11) . . ? O9 Co1 O2 83.67(10) . . ? O4 Co1 O2 145.10(10) . . ? O1 Co1 O3 93.38(10) . . ? N1 Co1 O3 174.25(11) . . ? O9 Co1 O3 91.12(10) . . ? O4 Co1 O3 73.35(9) . . ? O2 Co1 O3 73.86(9) . . ? O1 P1 O6 113.21(15) 2_775 . ? O1 P1 O10 112.39(15) 2_775 . ? O6 P1 O10 111.14(15) . . ? O1 P1 C13 109.04(16) 2_775 . ? O6 P1 C13 106.25(17) . . ? O10 P1 C13 104.21(16) . . ? O9 P2 O8 111.76(15) . . ? O9 P2 O5 113.29(15) . . ? O8 P2 O5 108.88(15) . . ? O9 P2 C32 111.28(16) . . ? O8 P2 C32 106.12(16) . . ? O5 P2 C32 105.05(16) . . ? P1 O1 Co1 141.16(16) 2_775 . ? C37 O2 Sb1 119.8(2) . . ? C37 O2 Co1 123.6(2) . . ? Sb1 O2 Co1 101.14(11) . . ? Sb2 O3 Sb1 137.75(13) . . ? Sb2 O3 Co1 102.96(10) . . ? Sb1 O3 Co1 102.81(11) . . ? C38 O4 Sb2 119.4(2) . . ? C38 O4 Co1 122.0(2) . . ? Sb2 O4 Co1 101.25(10) . . ? P2 O5 Sb1 123.91(15) . . ? P1 O6 Sb1 138.43(16) . . ? Sb2 O7 Sb1 144.29(15) 2_775 . ? P2 O8 Sb2 122.99(14) . . ? P2 O9 Co1 116.00(14) . . ? P1 O10 Sb2 137.51(16) . . ? C1 N1 C5 117.3(3) . . ? C1 N1 Co1 121.9(3) . . ? C5 N1 Co1 120.5(3) . . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.8(4) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 116.9(4) . . ? C2 C3 C6 122.6(4) . . ? C4 C3 C6 120.5(4) . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 123.6(4) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C11 C6 C7 118.7(4) . . ? C11 C6 C3 121.5(4) . . ? C7 C6 C3 119.8(4) . . ? C6 C7 C8 119.7(5) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 120.5(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.5(4) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 119.6(5) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C6 121.0(4) . . ? C10 C11 H11 119.5 . . ? C6 C11 H11 119.5 . . ? C18 C13 C14 118.7(4) . . ? C18 C13 P1 121.4(3) . . ? C14 C13 P1 119.8(3) . . ? C13 C14 C15 120.2(4) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.8(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C18 119.6(5) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C13 C18 C17 120.7(4) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C24 C19 C20 118.3(4) . . ? C24 C19 Sb2 119.9(3) . . ? C20 C19 Sb2 121.7(3) . . ? C21 C20 C19 121.7(4) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 118.3(4) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? C23 C22 C21 121.7(4) . . ? C23 C22 Cl1 118.8(3) . . ? C21 C22 Cl1 119.5(3) . . ? C22 C23 C24 119.2(4) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C19 C24 C23 120.7(4) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 C30 120.0 . . ? C26 C25 Sb1 121.63(12) . . ? C30 C25 Sb1 118.32(12) . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 Cl2 121.43(15) . . ? C29 C28 Cl2 118.54(15) . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C32 C31 C36 120.2(4) . . ? C32 C31 H31 119.9 . . ? C36 C31 H31 119.9 . . ? C31 C32 C33 119.1(4) . . ? C31 C32 P2 122.4(3) . . ? C33 C32 P2 118.5(3) . . ? C34 C33 C32 120.2(4) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 121.1(4) . . ? C34 C35 H39 119.4 . . ? C36 C35 H39 119.4 . . ? C35 C36 C31 119.6(4) . . ? C35 C36 H38 120.2 . . ? C31 C36 H38 120.2 . . ? O2 C37 H40A 109.5 . . ? O2 C37 H40B 109.5 . . ? H40A C37 H40B 109.5 . . ? O2 C37 H40C 109.5 . . ? H40A C37 H40C 109.5 . . ? H40B C37 H40C 109.5 . . ? O4 C38 H37A 109.5 . . ? O4 C38 H37B 109.5 . . ? H37A C38 H37B 109.5 . . ? O4 C38 H37C 109.5 . . ? H37A C38 H37C 109.5 . . ? H37B C38 H37C 109.5 . . ? 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 N1 Co1 O1 P1 -168.7(3) . . . 2_775 ? O9 Co1 O1 P1 158.8(10) . . . 2_775 ? O4 Co1 O1 P1 -68.0(3) . . . 2_775 ? O2 Co1 O1 P1 79.7(3) . . . 2_775 ? O3 Co1 O1 P1 5.7(3) . . . 2_775 ? O7 Sb1 O2 C37 -35.2(3) . . . . ? O3 Sb1 O2 C37 -130.1(3) . . . . ? O6 Sb1 O2 C37 -156.5(5) . . . . ? O5 Sb1 O2 C37 142.7(3) . . . . ? C25 Sb1 O2 C37 56.1(3) . . . . ? O7 Sb1 O2 Co1 104.60(11) . . . . ? O3 Sb1 O2 Co1 9.69(10) . . . . ? O6 Sb1 O2 Co1 -16.8(6) . . . . ? O5 Sb1 O2 Co1 -77.52(11) . . . . ? C25 Sb1 O2 Co1 -164.14(10) . . . . ? O1 Co1 O2 C37 36.6(3) . . . . ? N1 Co1 O2 C37 -52.8(3) . . . . ? O9 Co1 O2 C37 -138.4(3) . . . . ? O4 Co1 O2 C37 149.1(3) . . . . ? O3 Co1 O2 C37 128.6(3) . . . . ? O1 Co1 O2 Sb1 -101.07(11) . . . . ? N1 Co1 O2 Sb1 169.50(11) . . . . ? O9 Co1 O2 Sb1 83.91(11) . . . . ? O4 Co1 O2 Sb1 11.4(2) . . . . ? O3 Co1 O2 Sb1 -9.10(9) . . . . ? O7 Sb2 O3 Sb1 -130.0(2) 2_775 . . . ? O10 Sb2 O3 Sb1 -38.0(2) . . . . ? O4 Sb2 O3 Sb1 138.9(2) . . . . ? O8 Sb2 O3 Sb1 49.5(2) . . . . ? C19 Sb2 O3 Sb1 64.4(14) . . . . ? O7 Sb2 O3 Co1 103.74(11) 2_775 . . . ? O10 Sb2 O3 Co1 -164.24(11) . . . . ? O4 Sb2 O3 Co1 12.60(10) . . . . ? O8 Sb2 O3 Co1 -76.82(11) . . . . ? C19 Sb2 O3 Co1 -61.8(14) . . . . ? O7 Sb1 O3 Sb2 131.2(2) . . . . ? O6 Sb1 O3 Sb2 39.3(2) . . . . ? O2 Sb1 O3 Sb2 -136.1(2) . . . . ? O5 Sb1 O3 Sb2 -48.6(2) . . . . ? C25 Sb1 O3 Sb2 -53.2(10) . . . . ? O7 Sb1 O3 Co1 -102.51(11) . . . . ? O6 Sb1 O3 Co1 165.63(11) . . . . ? O2 Sb1 O3 Co1 -9.74(10) . . . . ? O5 Sb1 O3 Co1 77.76(11) . . . . ? C25 Sb1 O3 Co1 73.1(9) . . . . ? O1 Co1 O3 Sb2 -109.72(12) . . . . ? N1 Co1 O3 Sb2 -11.3(12) . . . . ? O9 Co1 O3 Sb2 72.56(11) . . . . ? O4 Co1 O3 Sb2 -12.27(10) . . . . ? O2 Co1 O3 Sb2 155.64(13) . . . . ? O1 Co1 O3 Sb1 104.05(11) . . . . ? N1 Co1 O3 Sb1 -157.6(11) . . . . ? O9 Co1 O3 Sb1 -73.67(11) . . . . ? O4 Co1 O3 Sb1 -158.50(13) . . . . ? O2 Co1 O3 Sb1 9.41(10) . . . . ? O7 Sb2 O4 C38 117.0(3) 2_775 . . . ? O3 Sb2 O4 C38 -149.7(3) . . . . ? O10 Sb2 O4 C38 -131.9(5) . . . . ? O8 Sb2 O4 C38 -62.0(3) . . . . ? C19 Sb2 O4 C38 25.1(3) . . . . ? O7 Sb2 O4 Co1 -105.88(11) 2_775 . . . ? O3 Sb2 O4 Co1 -12.59(10) . . . . ? O10 Sb2 O4 Co1 5.3(6) . . . . ? O8 Sb2 O4 Co1 75.13(11) . . . . ? C19 Sb2 O4 Co1 162.19(12) . . . . ? O1 Co1 O4 C38 -121.4(3) . . . . ? N1 Co1 O4 C38 -32.5(3) . . . . ? O9 Co1 O4 C38 54.9(3) . . . . ? O2 Co1 O4 C38 126.9(3) . . . . ? O3 Co1 O4 C38 147.5(3) . . . . ? O1 Co1 O4 Sb2 102.92(11) . . . . ? N1 Co1 O4 Sb2 -168.10(11) . . . . ? O9 Co1 O4 Sb2 -80.76(11) . . . . ? O2 Co1 O4 Sb2 -8.8(2) . . . . ? O3 Co1 O4 Sb2 11.80(9) . . . . ? O9 P2 O5 Sb1 -54.0(2) . . . . ? O8 P2 O5 Sb1 71.0(2) . . . . ? C32 P2 O5 Sb1 -175.68(18) . . . . ? O7 Sb1 O5 P2 168(3) . . . . ? O3 Sb1 O5 P2 -19.29(18) . . . . ? O6 Sb1 O5 P2 -109.39(19) . . . . ? O2 Sb1 O5 P2 61.51(18) . . . . ? C25 Sb1 O5 P2 160.21(19) . . . . ? O1 P1 O6 Sb1 100.7(2) 2_775 . . . ? O10 P1 O6 Sb1 -26.9(3) . . . . ? C13 P1 O6 Sb1 -139.6(2) . . . . ? O7 Sb1 O6 P1 -94.8(2) . . . . ? O3 Sb1 O6 P1 0.7(2) . . . . ? O2 Sb1 O6 P1 26.7(7) . . . . ? O5 Sb1 O6 P1 87.4(2) . . . . ? C25 Sb1 O6 P1 174.5(2) . . . . ? O3 Sb1 O7 Sb2 -17.7(3) . . . 2_775 ? O6 Sb1 O7 Sb2 72.5(2) . . . 2_775 ? O2 Sb1 O7 Sb2 -98.6(2) . . . 2_775 ? O5 Sb1 O7 Sb2 155(3) . . . 2_775 ? C25 Sb1 O7 Sb2 162.8(2) . . . 2_775 ? O9 P2 O8 Sb2 57.0(2) . . . . ? O5 P2 O8 Sb2 -68.9(2) . . . . ? C32 P2 O8 Sb2 178.48(17) . . . . ? O7 Sb2 O8 P2 171(5) 2_775 . . . ? O3 Sb2 O8 P2 17.19(18) . . . . ? O10 Sb2 O8 P2 107.59(18) . . . . ? O4 Sb2 O8 P2 -62.68(18) . . . . ? C19 Sb2 O8 P2 -161.4(2) . . . . ? O8 P2 O9 Co1 -63.19(19) . . . . ? O5 P2 O9 Co1 60.3(2) . . . . ? C32 P2 O9 Co1 178.36(16) . . . . ? O1 Co1 O9 P2 -152.3(11) . . . . ? N1 Co1 O9 P2 175.14(18) . . . . ? O4 Co1 O9 P2 74.05(16) . . . . ? O2 Co1 O9 P2 -72.76(16) . . . . ? O3 Co1 O9 P2 0.86(17) . . . . ? O1 P1 O10 Sb2 -98.6(2) 2_775 . . . ? O6 P1 O10 Sb2 29.5(3) . . . . ? C13 P1 O10 Sb2 143.5(2) . . . . ? O7 Sb2 O10 P1 89.0(2) 2_775 . . . ? O3 Sb2 O10 P1 -4.5(2) . . . . ? O4 Sb2 O10 P1 -22.1(7) . . . . ? O8 Sb2 O10 P1 -92.1(2) . . . . ? C19 Sb2 O10 P1 -179.3(2) . . . . ? O1 Co1 N1 C1 -146.1(3) . . . . ? O9 Co1 N1 C1 31.2(3) . . . . ? O4 Co1 N1 C1 116.1(3) . . . . ? O2 Co1 N1 C1 -51.3(3) . . . . ? O3 Co1 N1 C1 115.2(11) . . . . ? O1 Co1 N1 C5 40.6(3) . . . . ? O9 Co1 N1 C5 -142.1(3) . . . . ? O4 Co1 N1 C5 -57.1(3) . . . . ? O2 Co1 N1 C5 135.4(3) . . . . ? O3 Co1 N1 C5 -58.1(12) . . . . ? C5 N1 C1 C2 -0.7(6) . . . . ? Co1 N1 C1 C2 -174.2(3) . . . . ? N1 C1 C2 C3 3.0(6) . . . . ? C1 C2 C3 C4 -3.3(6) . . . . ? C1 C2 C3 C6 175.2(4) . . . . ? C2 C3 C4 C5 1.6(6) . . . . ? C6 C3 C4 C5 -176.9(4) . . . . ? C1 N1 C5 C4 -1.1(6) . . . . ? Co1 N1 C5 C4 172.5(3) . . . . ? C3 C4 C5 N1 0.7(6) . . . . ? C2 C3 C6 C11 146.8(4) . . . . ? C4 C3 C6 C11 -34.8(6) . . . . ? C2 C3 C6 C7 -33.8(6) . . . . ? C4 C3 C6 C7 144.6(4) . . . . ? C11 C6 C7 C8 0.6(7) . . . . ? C3 C6 C7 C8 -178.8(4) . . . . ? C6 C7 C8 C9 -0.5(8) . . . . ? C7 C8 C9 C10 0.5(8) . . . . ? C8 C9 C10 C11 -0.5(7) . . . . ? C9 C10 C11 C6 0.6(7) . . . . ? C7 C6 C11 C10 -0.6(7) . . . . ? C3 C6 C11 C10 178.8(4) . . . . ? O1 P1 C13 C18 135.1(3) 2_775 . . . ? O6 P1 C13 C18 12.8(4) . . . . ? O10 P1 C13 C18 -104.7(4) . . . . ? O1 P1 C13 C14 -48.4(4) 2_775 . . . ? O6 P1 C13 C14 -170.7(3) . . . . ? O10 P1 C13 C14 71.8(3) . . . . ? C18 C13 C14 C15 0.4(6) . . . . ? P1 C13 C14 C15 -176.2(3) . . . . ? C13 C14 C15 C16 -0.1(7) . . . . ? C14 C15 C16 C17 -0.6(8) . . . . ? C15 C16 C17 C18 1.0(8) . . . . ? C14 C13 C18 C17 0.1(7) . . . . ? P1 C13 C18 C17 176.6(4) . . . . ? C16 C17 C18 C13 -0.7(8) . . . . ? O7 Sb2 C19 C24 -24.3(3) 2_775 . . . ? O3 Sb2 C19 C24 141.3(12) . . . . ? O10 Sb2 C19 C24 -116.4(3) . . . . ? O4 Sb2 C19 C24 67.7(3) . . . . ? O8 Sb2 C19 C24 156.3(3) . . . . ? O7 Sb2 C19 C20 152.7(3) 2_775 . . . ? O3 Sb2 C19 C20 -41.7(15) . . . . ? O10 Sb2 C19 C20 60.7(3) . . . . ? O4 Sb2 C19 C20 -115.3(3) . . . . ? O8 Sb2 C19 C20 -26.7(3) . . . . ? C24 C19 C20 C21 -1.6(6) . . . . ? Sb2 C19 C20 C21 -178.7(3) . . . . ? C19 C20 C21 C22 -0.6(6) . . . . ? C20 C21 C22 C23 1.8(7) . . . . ? C20 C21 C22 Cl1 -177.6(3) . . . . ? C21 C22 C23 C24 -0.9(7) . . . . ? Cl1 C22 C23 C24 178.5(3) . . . . ? C20 C19 C24 C23 2.5(6) . . . . ? Sb2 C19 C24 C23 179.7(3) . . . . ? C22 C23 C24 C19 -1.3(7) . . . . ? O7 Sb1 C25 C26 137.55(15) . . . . ? O3 Sb1 C25 C26 -38.1(10) . . . . ? O6 Sb1 C25 C26 -130.60(15) . . . . ? O2 Sb1 C25 C26 43.79(15) . . . . ? O5 Sb1 C25 C26 -42.74(14) . . . . ? O7 Sb1 C25 C30 -45.18(14) . . . . ? O3 Sb1 C25 C30 139.2(9) . . . . ? O6 Sb1 C25 C30 46.67(14) . . . . ? O2 Sb1 C25 C30 -138.94(14) . . . . ? O5 Sb1 C25 C30 134.53(14) . . . . ? C30 C25 C26 C27 0.0 . . . . ? Sb1 C25 C26 C27 177.23(18) . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C26 C27 C28 Cl2 -178.0(2) . . . . ? C27 C28 C29 C30 0.0 . . . . ? Cl2 C28 C29 C30 178.0(2) . . . . ? C28 C29 C30 C25 0.0 . . . . ? C26 C25 C30 C29 0.0 . . . . ? Sb1 C25 C30 C29 -177.32(17) . . . . ? C36 C31 C32 C33 -1.1(7) . . . . ? C36 C31 C32 P2 178.8(4) . . . . ? O9 P2 C32 C31 -146.3(4) . . . . ? O8 P2 C32 C31 91.9(4) . . . . ? O5 P2 C32 C31 -23.4(4) . . . . ? O9 P2 C32 C33 33.5(4) . . . . ? O8 P2 C32 C33 -88.3(3) . . . . ? O5 P2 C32 C33 156.5(3) . . . . ? C31 C32 C33 C34 -0.3(6) . . . . ? P2 C32 C33 C34 179.8(3) . . . . ? C32 C33 C34 C35 0.7(7) . . . . ? C33 C34 C35 C36 0.4(7) . . . . ? C34 C35 C36 C31 -1.8(8) . . . . ? C32 C31 C36 C35 2.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.736 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.125 # Attachment '- 9.cif' data_mono820 _database_code_depnum_ccdc_archive 'CCDC 778679' #TrackingRef '- 9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H66 Cl4 Co2 N2 O20 P4 Sb4' _chemical_formula_weight 2077.75 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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)/n 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 12.5774(5) _cell_length_b 11.8992(4) _cell_length_c 24.9253(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.943(3) _cell_angle_gamma 90.00 _cell_volume 3662.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9167 _cell_measurement_theta_min 2.7100 _cell_measurement_theta_max 28.4909 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 2.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5578 _exptl_absorpt_correction_T_max 0.8098 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23272 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7456 _reflns_number_gt 4875 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0368P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7456 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 P1 P 0.97966(10) 0.89436(10) 0.83021(5) 0.0168(3) Uani 1 1 d . . . Sb1 Sb 1.03966(2) 0.89648(2) 1.092935(12) 0.01459(9) Uani 1 1 d . . . Sb2 Sb 1.06572(2) 0.82479(2) 0.953354(12) 0.01463(9) Uani 1 1 d . . . Co3 Co 0.81331(5) 0.88003(5) 0.90733(3) 0.01677(15) Uani 1 1 d . . . P2 P 0.78357(10) 0.94375(10) 1.03356(5) 0.0155(3) Uani 1 1 d . . . Cl2 Cl 1.04032(11) 0.40566(10) 1.21854(5) 0.0307(3) Uani 1 1 d . . . Cl1 Cl 1.36828(11) 0.36658(10) 0.98148(6) 0.0344(3) Uani 1 1 d . . . O4 O 1.0725(2) 0.8182(2) 1.03121(11) 0.0142(7) Uani 1 1 d . . . O9 O 1.1952(2) 0.9441(2) 1.11752(12) 0.0169(7) Uani 1 1 d . . . O10 O 1.0015(2) 0.9768(2) 1.16029(12) 0.0164(7) Uani 1 1 d . . . O7 O 0.7501(2) 0.9019(2) 0.97618(12) 0.0173(7) Uani 1 1 d . . . O2 O 1.0664(2) 0.8303(2) 0.87099(12) 0.0168(7) Uani 1 1 d . . . O5 O 0.9228(2) 0.7434(2) 0.93420(12) 0.0170(7) Uani 1 1 d . . . O3 O 1.1935(2) 0.9287(2) 0.96335(12) 0.0163(7) Uani 1 1 d . . . O6 O 0.8796(2) 0.8775(2) 1.06656(12) 0.0159(7) Uani 1 1 d . . . N1 N 0.6698(3) 0.7993(3) 0.87049(16) 0.0209(9) Uani 1 1 d . . . C10 C 1.0449(4) 0.5377(4) 1.18828(19) 0.0227(11) Uani 1 1 d . . . O8 O 0.8669(3) 0.8593(2) 0.83260(12) 0.0197(7) Uani 1 1 d . . . C9 C 1.1122(4) 0.5544(4) 1.1523(2) 0.0269(12) Uani 1 1 d . . . H8 H 1.1587 0.4958 1.1450 0.032 Uiso 1 1 calc R . . C1 C 1.1652(4) 0.6816(4) 0.95834(18) 0.0154(10) Uani 1 1 d . . . C7 C 1.0453(4) 0.7440(4) 1.13717(17) 0.0160(10) Uani 1 1 d . . . C4 C 1.2913(4) 0.4898(4) 0.9722(2) 0.0202(11) Uani 1 1 d . . . C14 C 0.7048(4) 0.9444(4) 1.1284(2) 0.0306(13) Uani 1 1 d . . . H4 H 0.7780 0.9574 1.1452 0.037 Uiso 1 1 calc R . . C2 C 1.2612(4) 0.6777(4) 0.9971(2) 0.0239(11) Uani 1 1 d . . . H18 H 1.2830 0.7416 1.0194 0.029 Uiso 1 1 calc R . . C6 C 1.1348(4) 0.5877(4) 0.92657(19) 0.0213(11) Uani 1 1 d . . . H14 H 1.0706 0.5897 0.8994 0.026 Uiso 1 1 calc R . . C13 C 0.6783(4) 0.9285(4) 1.0717(2) 0.0205(11) Uani 1 1 d . . . C3 C 1.3255(4) 0.5817(4) 1.0037(2) 0.0259(12) Uani 1 1 d . . . H17 H 1.3916 0.5800 1.0295 0.031 Uiso 1 1 calc R . . C18 C 0.5719(4) 0.9084(4) 1.0484(2) 0.0257(12) Uani 1 1 d . . . H2 H 0.5524 0.8966 1.0101 0.031 Uiso 1 1 calc R . . C15 C 0.6263(5) 0.9414(5) 1.1602(2) 0.0431(16) Uani 1 1 d . . . H5 H 0.6453 0.9531 1.1985 0.052 Uiso 1 1 calc R . . C11 C 0.9758(4) 0.6214(4) 1.1995(2) 0.0280(12) Uani 1 1 d . . . H12 H 0.9288 0.6083 1.2245 0.034 Uiso 1 1 calc R . . C5 C 1.1969(4) 0.4902(4) 0.9338(2) 0.0244(12) Uani 1 1 d . . . H15 H 1.1745 0.4251 0.9126 0.029 Uiso 1 1 calc R . . C17 C 0.4924(4) 0.9052(4) 1.0805(3) 0.0369(14) Uani 1 1 d . . . H3 H 0.4190 0.8919 1.0640 0.044 Uiso 1 1 calc R . . O11 O 1.0337(2) 1.0450(2) 1.05783(12) 0.0147(7) Uani 1 1 d . . . C28 C 0.5700(4) 0.6812(4) 0.8017(2) 0.0293(13) Uani 1 1 d . . . H27 H 0.5700 0.6344 0.7709 0.035 Uiso 1 1 calc R . . C19 C 1.0086(4) 0.8713(4) 0.76339(19) 0.0188(11) Uani 1 1 d . . . C27 C 0.4737(4) 0.6989(4) 0.8208(2) 0.0295(13) Uani 1 1 d . . . C29 C 0.6645(4) 0.7312(4) 0.8274(2) 0.0241(12) Uani 1 1 d . . . H26 H 0.7289 0.7168 0.8139 0.029 Uiso 1 1 calc R . . C32 C 1.2514(4) 0.9146(4) 1.1705(2) 0.0263(12) Uani 1 1 d . . . H25A H 1.1991 0.8998 1.1942 0.040 Uiso 1 1 calc R . . H25B H 1.2990 0.9767 1.1857 0.040 Uiso 1 1 calc R . . H25C H 1.2949 0.8471 1.1682 0.040 Uiso 1 1 calc R . . C25 C 0.5780(4) 0.8138(5) 0.8895(2) 0.0349(13) Uani 1 1 d . . . H30 H 0.5804 0.8594 0.9210 0.042 Uiso 1 1 calc R . . C20 C 0.9231(4) 0.8759(4) 0.7184(2) 0.0297(13) Uani 1 1 d . . . H22 H 0.8507 0.8848 0.7238 0.036 Uiso 1 1 calc R . . C24 C 1.1125(4) 0.8551(4) 0.7551(2) 0.0308(13) Uani 1 1 d . . . H20 H 1.1707 0.8514 0.7855 0.037 Uiso 1 1 calc R . . C26 C 0.4806(5) 0.7664(5) 0.8660(2) 0.0434(16) Uani 1 1 d . . . H29 H 0.4179 0.7803 0.8811 0.052 Uiso 1 1 calc R . . C16 C 0.5203(5) 0.9214(5) 1.1360(3) 0.0457(16) Uani 1 1 d . . . H31 H 0.4660 0.9188 1.1578 0.055 Uiso 1 1 calc R . . C12 C 0.9763(4) 0.7243(4) 1.1738(2) 0.0243(12) Uani 1 1 d . . . H23 H 0.9292 0.7822 1.1812 0.029 Uiso 1 1 calc R . . C8 C 1.1126(4) 0.6569(4) 1.1264(2) 0.0253(12) Uani 1 1 d . . . H24 H 1.1591 0.6682 1.1010 0.030 Uiso 1 1 calc R . . C23 C 1.1328(5) 0.8443(5) 0.7025(2) 0.0417(15) Uani 1 1 d . . . H36 H 1.2045 0.8321 0.6968 0.050 Uiso 1 1 calc R . . C21 C 0.9442(5) 0.8674(5) 0.6666(2) 0.0392(15) Uani 1 1 d . . . H37 H 0.8864 0.8726 0.6360 0.047 Uiso 1 1 calc R . . C22 C 1.0483(5) 0.8513(5) 0.6585(2) 0.0408(16) Uani 1 1 d . . . H38 H 1.0619 0.8451 0.6224 0.049 Uiso 1 1 calc R . . C35 C 0.8949(4) 0.6598(4) 0.97077(19) 0.0202(11) Uani 1 1 d . . . H35A H 0.9529 0.6037 0.9784 0.030 Uiso 1 1 calc R . . H35B H 0.8271 0.6230 0.9538 0.030 Uiso 1 1 calc R . . H35C H 0.8858 0.6957 1.0050 0.030 Uiso 1 1 calc R . . C50 C 0.3671(4) 0.6507(5) 0.7909(2) 0.0362(14) Uani 1 1 d . . . H50A H 0.3326 0.7060 0.7633 0.043 Uiso 1 1 calc R . . H50B H 0.3822 0.5821 0.7712 0.043 Uiso 1 1 calc R . . C51 C 0.2879(5) 0.6214(5) 0.8274(3) 0.0507(17) Uani 1 1 d . . . H51A H 0.3237 0.5734 0.8574 0.076 Uiso 1 1 calc R . . H51B H 0.2259 0.5813 0.8061 0.076 Uiso 1 1 calc R . . H51C H 0.2627 0.6905 0.8423 0.076 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 P1 0.0207(7) 0.0146(6) 0.0155(6) -0.0002(5) 0.0046(5) 0.0003(6) Sb1 0.01686(18) 0.01274(16) 0.01480(16) 0.00122(13) 0.00456(13) 0.00076(14) Sb2 0.01704(18) 0.01226(16) 0.01556(16) 0.00073(13) 0.00556(13) 0.00064(14) Co3 0.0164(4) 0.0163(3) 0.0179(3) 0.0003(3) 0.0039(3) -0.0008(3) P2 0.0146(7) 0.0146(6) 0.0182(6) 0.0012(5) 0.0053(5) -0.0002(5) Cl2 0.0464(9) 0.0173(6) 0.0254(7) 0.0058(5) -0.0011(6) -0.0043(6) Cl1 0.0381(9) 0.0242(7) 0.0453(8) 0.0087(6) 0.0189(7) 0.0153(6) O4 0.0169(18) 0.0135(15) 0.0134(16) 0.0018(13) 0.0053(13) 0.0043(14) O9 0.0156(18) 0.0187(17) 0.0155(16) 0.0020(14) 0.0006(14) 0.0007(14) O10 0.0193(18) 0.0154(16) 0.0151(16) 0.0008(13) 0.0048(14) 0.0015(14) O7 0.0143(17) 0.0178(17) 0.0201(17) -0.0038(14) 0.0034(14) -0.0037(14) O2 0.0221(18) 0.0157(17) 0.0134(16) -0.0016(14) 0.0053(14) 0.0005(14) O5 0.0180(18) 0.0183(17) 0.0161(16) 0.0001(14) 0.0069(14) -0.0036(14) O3 0.0113(17) 0.0178(17) 0.0207(17) -0.0005(14) 0.0054(14) -0.0010(13) O6 0.0164(18) 0.0125(16) 0.0185(16) 0.0019(13) 0.0023(14) -0.0027(14) N1 0.021(2) 0.019(2) 0.023(2) 0.0022(18) 0.0044(19) 0.0006(18) C10 0.031(3) 0.015(3) 0.020(3) 0.000(2) -0.002(2) -0.012(2) O8 0.0223(19) 0.0179(17) 0.0187(18) -0.0004(14) 0.0037(15) -0.0032(14) C9 0.038(3) 0.014(3) 0.027(3) -0.001(2) 0.004(3) 0.007(2) C1 0.018(3) 0.015(2) 0.016(2) 0.000(2) 0.009(2) -0.003(2) C7 0.019(3) 0.014(2) 0.013(2) -0.0007(19) -0.001(2) -0.001(2) C4 0.016(3) 0.015(3) 0.033(3) 0.007(2) 0.012(2) 0.005(2) C14 0.027(3) 0.033(3) 0.034(3) 0.000(3) 0.012(3) 0.000(2) C2 0.018(3) 0.019(3) 0.035(3) -0.005(2) 0.005(2) 0.000(2) C6 0.025(3) 0.023(3) 0.016(2) 0.000(2) 0.002(2) 0.001(2) C13 0.021(3) 0.013(2) 0.030(3) 0.002(2) 0.010(2) 0.002(2) C3 0.017(3) 0.029(3) 0.030(3) 0.006(2) 0.002(2) 0.003(2) C18 0.033(3) 0.013(3) 0.033(3) 0.005(2) 0.010(3) 0.004(2) C15 0.054(4) 0.046(4) 0.036(3) -0.001(3) 0.027(3) 0.008(3) C11 0.032(3) 0.028(3) 0.028(3) 0.001(2) 0.014(2) -0.003(2) C5 0.037(3) 0.015(3) 0.023(3) -0.007(2) 0.010(3) 0.000(2) C17 0.026(3) 0.031(3) 0.056(4) 0.006(3) 0.013(3) 0.000(3) O11 0.0138(17) 0.0099(16) 0.0209(17) 0.0030(14) 0.0043(14) 0.0004(13) C28 0.029(3) 0.027(3) 0.034(3) -0.011(2) 0.012(3) -0.003(3) C19 0.026(3) 0.016(2) 0.016(2) 0.001(2) 0.008(2) -0.006(2) C27 0.025(3) 0.037(3) 0.028(3) -0.001(3) 0.009(3) -0.005(2) C29 0.015(3) 0.026(3) 0.031(3) -0.010(2) 0.004(2) -0.002(2) C32 0.029(3) 0.024(3) 0.026(3) 0.005(2) 0.004(2) 0.003(2) C25 0.031(3) 0.043(3) 0.032(3) -0.011(3) 0.009(3) -0.005(3) C20 0.035(3) 0.033(3) 0.022(3) 0.002(2) 0.007(2) -0.003(3) C24 0.033(3) 0.031(3) 0.030(3) -0.007(2) 0.009(3) -0.001(2) C26 0.029(3) 0.060(4) 0.046(4) -0.019(3) 0.017(3) -0.014(3) C16 0.036(4) 0.052(4) 0.057(4) 0.005(3) 0.030(3) -0.001(3) C12 0.030(3) 0.014(3) 0.030(3) 0.000(2) 0.008(2) 0.003(2) C8 0.030(3) 0.027(3) 0.022(3) 0.001(2) 0.013(2) -0.004(2) C23 0.045(4) 0.048(4) 0.039(4) -0.009(3) 0.026(3) -0.005(3) C21 0.049(4) 0.051(4) 0.016(3) -0.004(3) 0.002(3) -0.009(3) C22 0.059(4) 0.050(4) 0.018(3) -0.007(3) 0.018(3) -0.015(3) C35 0.023(3) 0.015(3) 0.025(3) 0.000(2) 0.008(2) -0.003(2) C50 0.031(3) 0.041(3) 0.037(3) -0.009(3) 0.007(3) -0.017(3) C51 0.041(4) 0.063(4) 0.048(4) -0.007(3) 0.010(3) -0.023(3) _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 P1 O8 1.491(3) . ? P1 O2 1.544(3) . ? P1 O10 1.563(3) 3_777 ? P1 C19 1.792(4) . ? Sb1 O4 1.910(3) . ? Sb1 O11 1.967(3) . ? Sb1 O6 2.008(3) . ? Sb1 O9 2.017(3) . ? Sb1 O10 2.066(3) . ? Sb1 C7 2.117(4) . ? Sb2 O4 1.928(3) . ? Sb2 O11 1.977(3) 3_777 ? Sb2 O3 2.005(3) . ? Sb2 O5 2.018(3) . ? Sb2 O2 2.056(3) . ? Sb2 C1 2.103(4) . ? Co3 O7 2.041(3) . ? Co3 N1 2.096(4) . ? Co3 O8 2.112(3) . ? Co3 O11 2.149(3) 3_777 ? Co3 O5 2.153(3) . ? Co3 O9 2.180(3) 3_777 ? P2 O7 1.497(3) . ? P2 O6 1.542(3) . ? P2 O3 1.544(3) 3_777 ? P2 C13 1.780(5) . ? Cl2 C10 1.748(5) . ? Cl1 C4 1.748(4) . ? O9 C32 1.418(5) . ? O9 Co3 2.180(3) 3_777 ? O10 P1 1.563(3) 3_777 ? O5 C35 1.437(5) . ? O3 P2 1.544(3) 3_777 ? N1 C29 1.337(6) . ? N1 C25 1.340(6) . ? C10 C9 1.359(6) . ? C10 C11 1.386(6) . ? C9 C8 1.381(6) . ? C9 H8 0.9500 . ? C1 C6 1.381(6) . ? C1 C2 1.397(6) . ? C7 C12 1.394(6) . ? C7 C8 1.396(6) . ? C4 C3 1.367(6) . ? C4 C5 1.376(7) . ? C14 C15 1.377(7) . ? C14 C13 1.402(7) . ? C14 H4 0.9500 . ? C2 C3 1.391(6) . ? C2 H18 0.9500 . ? C6 C5 1.391(6) . ? C6 H14 0.9500 . ? C13 C18 1.375(7) . ? C3 H17 0.9500 . ? C18 C17 1.395(7) . ? C18 H2 0.9500 . ? C15 C16 1.376(8) . ? C15 H5 0.9500 . ? C11 C12 1.382(6) . ? C11 H12 0.9500 . ? C5 H15 0.9500 . ? C17 C16 1.374(8) . ? C17 H3 0.9500 . ? O11 Sb2 1.977(3) 3_777 ? O11 Co3 2.149(3) 3_777 ? C28 C29 1.373(7) . ? C28 C27 1.397(6) . ? C28 H27 0.9500 . ? C19 C24 1.374(7) . ? C19 C20 1.400(7) . ? C27 C26 1.375(7) . ? C27 C50 1.517(7) . ? C29 H26 0.9500 . ? C32 H25A 0.9800 . ? C32 H25B 0.9800 . ? C32 H25C 0.9800 . ? C25 C26 1.375(7) . ? C25 H30 0.9500 . ? C20 C21 1.370(7) . ? C20 H22 0.9500 . ? C24 C23 1.390(7) . ? C24 H20 0.9500 . ? C26 H29 0.9500 . ? C16 H31 0.9500 . ? C12 H23 0.9500 . ? C8 H24 0.9500 . ? C23 C22 1.377(8) . ? C23 H36 0.9500 . ? C21 C22 1.376(8) . ? C21 H37 0.9500 . ? C22 H38 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C50 C51 1.511(7) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? 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 O8 P1 O2 113.25(17) . . ? O8 P1 O10 112.76(17) . 3_777 ? O2 P1 O10 108.45(17) . 3_777 ? O8 P1 C19 110.9(2) . . ? O2 P1 C19 107.1(2) . . ? O10 P1 C19 103.86(18) 3_777 . ? O4 Sb1 O11 94.35(12) . . ? O4 Sb1 O6 92.19(12) . . ? O11 Sb1 O6 90.24(12) . . ? O4 Sb1 O9 92.06(12) . . ? O11 Sb1 O9 80.55(12) . . ? O6 Sb1 O9 170.12(11) . . ? O4 Sb1 O10 178.18(12) . . ? O11 Sb1 O10 87.18(11) . . ? O6 Sb1 O10 86.83(11) . . ? O9 Sb1 O10 89.14(12) . . ? O4 Sb1 C7 90.59(14) . . ? O11 Sb1 C7 174.99(14) . . ? O6 Sb1 C7 90.38(15) . . ? O9 Sb1 C7 98.49(15) . . ? O10 Sb1 C7 87.89(14) . . ? O4 Sb2 O11 94.58(11) . 3_777 ? O4 Sb2 O3 91.08(12) . . ? O11 Sb2 O3 90.28(12) 3_777 . ? O4 Sb2 O5 94.92(12) . . ? O11 Sb2 O5 80.29(12) 3_777 . ? O3 Sb2 O5 169.18(12) . . ? O4 Sb2 O2 177.21(12) . . ? O11 Sb2 O2 87.51(11) 3_777 . ? O3 Sb2 O2 87.07(12) . . ? O5 Sb2 O2 87.23(12) . . ? O4 Sb2 C1 89.73(14) . . ? O11 Sb2 C1 174.98(15) 3_777 . ? O3 Sb2 C1 92.21(14) . . ? O5 Sb2 C1 96.80(15) . . ? O2 Sb2 C1 88.26(14) . . ? O7 Co3 N1 89.21(13) . . ? O7 Co3 O8 175.66(12) . . ? N1 Co3 O8 87.26(13) . . ? O7 Co3 O11 93.97(11) . 3_777 ? N1 Co3 O11 176.08(13) . 3_777 ? O8 Co3 O11 89.65(11) . 3_777 ? O7 Co3 O5 99.39(11) . . ? N1 Co3 O5 103.68(13) . . ? O8 Co3 O5 83.92(11) . . ? O11 Co3 O5 73.57(11) 3_777 . ? O7 Co3 O9 96.33(11) . 3_777 ? N1 Co3 O9 108.90(13) . 3_777 ? O8 Co3 O9 82.43(11) . 3_777 ? O11 Co3 O9 73.04(11) 3_777 3_777 ? O5 Co3 O9 143.85(11) . 3_777 ? O7 P2 O6 112.93(17) . . ? O7 P2 O3 112.96(17) . 3_777 ? O6 P2 O3 110.84(17) . 3_777 ? O7 P2 C13 111.9(2) . . ? O6 P2 C13 104.4(2) . . ? O3 P2 C13 102.98(18) 3_777 . ? Sb1 O4 Sb2 144.68(16) . . ? C32 O9 Sb1 119.8(3) . . ? C32 O9 Co3 119.4(3) . 3_777 ? Sb1 O9 Co3 100.99(12) . 3_777 ? P1 O10 Sb1 121.65(16) 3_777 . ? P2 O7 Co3 139.62(18) . . ? P1 O2 Sb2 122.46(17) . . ? C35 O5 Sb2 119.7(3) . . ? C35 O5 Co3 120.1(2) . . ? Sb2 O5 Co3 101.51(12) . . ? P2 O3 Sb2 138.60(18) 3_777 . ? P2 O6 Sb1 138.75(17) . . ? C29 N1 C25 116.6(4) . . ? C29 N1 Co3 122.5(3) . . ? C25 N1 Co3 120.9(3) . . ? C9 C10 C11 121.4(4) . . ? C9 C10 Cl2 119.5(4) . . ? C11 C10 Cl2 119.0(4) . . ? P1 O8 Co3 117.89(18) . . ? C10 C9 C8 119.7(5) . . ? C10 C9 H8 120.1 . . ? C8 C9 H8 120.1 . . ? C6 C1 C2 118.6(4) . . ? C6 C1 Sb2 121.7(3) . . ? C2 C1 Sb2 119.6(3) . . ? C12 C7 C8 118.5(4) . . ? C12 C7 Sb1 121.5(3) . . ? C8 C7 Sb1 119.9(3) . . ? C3 C4 C5 122.2(4) . . ? C3 C4 Cl1 119.2(4) . . ? C5 C4 Cl1 118.6(4) . . ? C15 C14 C13 121.1(5) . . ? C15 C14 H4 119.4 . . ? C13 C14 H4 119.5 . . ? C3 C2 C1 121.0(5) . . ? C3 C2 H18 119.5 . . ? C1 C2 H18 119.5 . . ? C1 C6 C5 120.9(5) . . ? C1 C6 H14 119.5 . . ? C5 C6 H14 119.5 . . ? C18 C13 C14 118.4(4) . . ? C18 C13 P2 123.7(4) . . ? C14 C13 P2 117.8(4) . . ? C4 C3 C2 118.5(5) . . ? C4 C3 H17 120.8 . . ? C2 C3 H17 120.8 . . ? C13 C18 C17 120.6(5) . . ? C13 C18 H2 119.7 . . ? C17 C18 H2 119.7 . . ? C16 C15 C14 119.6(5) . . ? C16 C15 H5 120.2 . . ? C14 C15 H5 120.2 . . ? C12 C11 C10 119.0(4) . . ? C12 C11 H12 120.5 . . ? C10 C11 H12 120.5 . . ? C4 C5 C6 118.8(4) . . ? C4 C5 H15 120.6 . . ? C6 C5 H15 120.6 . . ? C16 C17 C18 120.0(5) . . ? C16 C17 H3 120.0 . . ? C18 C17 H3 120.0 . . ? Sb1 O11 Sb2 137.42(15) . 3_777 ? Sb1 O11 Co3 103.74(13) . 3_777 ? Sb2 O11 Co3 103.05(12) 3_777 3_777 ? C29 C28 C27 120.4(5) . . ? C29 C28 H27 119.8 . . ? C27 C28 H27 119.8 . . ? C24 C19 C20 119.5(5) . . ? C24 C19 P1 121.8(4) . . ? C20 C19 P1 118.5(4) . . ? C26 C27 C28 116.3(5) . . ? C26 C27 C50 122.3(5) . . ? C28 C27 C50 121.3(5) . . ? N1 C29 C28 122.9(4) . . ? N1 C29 H26 118.5 . . ? C28 C29 H26 118.5 . . ? O9 C32 H25A 109.5 . . ? O9 C32 H25B 109.5 . . ? H25A C32 H25B 109.5 . . ? O9 C32 H25C 109.5 . . ? H25A C32 H25C 109.5 . . ? H25B C32 H25C 109.5 . . ? N1 C25 C26 123.6(5) . . ? N1 C25 H30 118.2 . . ? C26 C25 H30 118.2 . . ? C21 C20 C19 119.7(5) . . ? C21 C20 H22 120.2 . . ? C19 C20 H22 120.2 . . ? C19 C24 C23 120.4(5) . . ? C19 C24 H20 119.8 . . ? C23 C24 H20 119.8 . . ? C27 C26 C25 120.1(5) . . ? C27 C26 H29 120.0 . . ? C25 C26 H29 120.0 . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H31 119.8 . . ? C15 C16 H31 119.8 . . ? C11 C12 C7 120.7(4) . . ? C11 C12 H23 119.6 . . ? C7 C12 H23 119.6 . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H24 119.7 . . ? C7 C8 H24 119.7 . . ? C22 C23 C24 119.5(5) . . ? C22 C23 H36 120.2 . . ? C24 C23 H36 120.2 . . ? C20 C21 C22 120.6(5) . . ? C20 C21 H37 119.7 . . ? C22 C21 H37 119.7 . . ? C21 C22 C23 120.3(5) . . ? C21 C22 H38 119.9 . . ? C23 C22 H38 119.9 . . ? O5 C35 H35A 109.5 . . ? O5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C51 C50 C27 114.5(5) . . ? C51 C50 H50A 108.6 . . ? C27 C50 H50A 108.6 . . ? C51 C50 H50B 108.6 . . ? C27 C50 H50B 108.6 . . ? H50A C50 H50B 107.6 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? 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 O11 Sb1 O4 Sb2 -21.3(3) . . . . ? O6 Sb1 O4 Sb2 69.1(3) . . . . ? O9 Sb1 O4 Sb2 -102.0(3) . . . . ? O10 Sb1 O4 Sb2 126(4) . . . . ? C7 Sb1 O4 Sb2 159.5(3) . . . . ? O11 Sb2 O4 Sb1 -12.9(3) 3_777 . . . ? O3 Sb2 O4 Sb1 77.5(3) . . . . ? O5 Sb2 O4 Sb1 -93.5(3) . . . . ? O2 Sb2 O4 Sb1 126(2) . . . . ? C1 Sb2 O4 Sb1 169.7(3) . . . . ? O4 Sb1 O9 C32 -122.5(3) . . . . ? O11 Sb1 O9 C32 143.4(3) . . . . ? O6 Sb1 O9 C32 122.1(7) . . . . ? O10 Sb1 O9 C32 56.2(3) . . . . ? C7 Sb1 O9 C32 -31.6(3) . . . . ? O4 Sb1 O9 Co3 104.12(12) . . . 3_777 ? O11 Sb1 O9 Co3 10.05(12) . . . 3_777 ? O6 Sb1 O9 Co3 -11.3(7) . . . 3_777 ? O10 Sb1 O9 Co3 -77.24(12) . . . 3_777 ? C7 Sb1 O9 Co3 -164.98(14) . . . 3_777 ? O4 Sb1 O10 P1 -168(4) . . . 3_777 ? O11 Sb1 O10 P1 -20.5(2) . . . 3_777 ? O6 Sb1 O10 P1 -110.9(2) . . . 3_777 ? O9 Sb1 O10 P1 60.1(2) . . . 3_777 ? C7 Sb1 O10 P1 158.6(2) . . . 3_777 ? O6 P2 O7 Co3 -59.3(3) . . . . ? O3 P2 O7 Co3 67.5(3) 3_777 . . . ? C13 P2 O7 Co3 -176.9(3) . . . . ? N1 Co3 O7 P2 173.8(3) . . . . ? O8 Co3 O7 P2 -150.5(14) . . . . ? O11 Co3 O7 P2 -3.9(3) 3_777 . . . ? O5 Co3 O7 P2 70.1(3) . . . . ? O9 Co3 O7 P2 -77.3(3) 3_777 . . . ? O8 P1 O2 Sb2 -54.9(2) . . . . ? O10 P1 O2 Sb2 71.0(2) 3_777 . . . ? C19 P1 O2 Sb2 -177.5(2) . . . . ? O4 Sb2 O2 P1 -156(2) . . . . ? O11 Sb2 O2 P1 -17.2(2) 3_777 . . . ? O3 Sb2 O2 P1 -107.6(2) . . . . ? O5 Sb2 O2 P1 63.2(2) . . . . ? C1 Sb2 O2 P1 160.1(2) . . . . ? O4 Sb2 O5 C35 -31.2(3) . . . . ? O11 Sb2 O5 C35 -125.1(3) 3_777 . . . ? O3 Sb2 O5 C35 -154.7(5) . . . . ? O2 Sb2 O5 C35 147.0(3) . . . . ? C1 Sb2 O5 C35 59.1(3) . . . . ? O4 Sb2 O5 Co3 103.64(12) . . . . ? O11 Sb2 O5 Co3 9.82(11) 3_777 . . . ? O3 Sb2 O5 Co3 -19.8(7) . . . . ? O2 Sb2 O5 Co3 -78.12(12) . . . . ? C1 Sb2 O5 Co3 -166.04(14) . . . . ? O7 Co3 O5 C35 34.0(3) . . . . ? N1 Co3 O5 C35 -57.5(3) . . . . ? O8 Co3 O5 C35 -143.2(3) . . . . ? O11 Co3 O5 C35 125.4(3) 3_777 . . . ? O9 Co3 O5 C35 148.5(3) 3_777 . . . ? O7 Co3 O5 Sb2 -100.68(12) . . . . ? N1 Co3 O5 Sb2 167.83(13) . . . . ? O8 Co3 O5 Sb2 82.15(13) . . . . ? O11 Co3 O5 Sb2 -9.29(11) 3_777 . . . ? O9 Co3 O5 Sb2 13.9(2) 3_777 . . . ? O4 Sb2 O3 P2 -90.3(3) . . . 3_777 ? O11 Sb2 O3 P2 4.3(3) 3_777 . . 3_777 ? O5 Sb2 O3 P2 33.4(8) . . . 3_777 ? O2 Sb2 O3 P2 91.8(3) . . . 3_777 ? C1 Sb2 O3 P2 179.9(3) . . . 3_777 ? O7 P2 O6 Sb1 103.3(3) . . . . ? O3 P2 O6 Sb1 -24.6(3) 3_777 . . . ? C13 P2 O6 Sb1 -134.8(3) . . . . ? O4 Sb1 O6 P2 -95.1(3) . . . . ? O11 Sb1 O6 P2 -0.7(3) . . . . ? O9 Sb1 O6 P2 20.4(9) . . . . ? O10 Sb1 O6 P2 86.5(3) . . . . ? C7 Sb1 O6 P2 174.3(3) . . . . ? O7 Co3 N1 C29 -160.0(4) . . . . ? O8 Co3 N1 C29 22.5(4) . . . . ? O11 Co3 N1 C29 -16(2) 3_777 . . . ? O5 Co3 N1 C29 -60.6(4) . . . . ? O9 Co3 N1 C29 103.5(4) 3_777 . . . ? O7 Co3 N1 C25 19.9(4) . . . . ? O8 Co3 N1 C25 -157.6(4) . . . . ? O11 Co3 N1 C25 164.3(17) 3_777 . . . ? O5 Co3 N1 C25 119.3(4) . . . . ? O9 Co3 N1 C25 -76.6(4) 3_777 . . . ? O2 P1 O8 Co3 60.2(2) . . . . ? O10 P1 O8 Co3 -63.4(2) 3_777 . . . ? C19 P1 O8 Co3 -179.43(19) . . . . ? O7 Co3 O8 P1 149.0(14) . . . . ? N1 Co3 O8 P1 -175.2(2) . . . . ? O11 Co3 O8 P1 2.34(19) 3_777 . . . ? O5 Co3 O8 P1 -71.17(19) . . . . ? O9 Co3 O8 P1 75.27(19) 3_777 . . . ? C11 C10 C9 C8 0.3(8) . . . . ? Cl2 C10 C9 C8 177.1(4) . . . . ? O4 Sb2 C1 C6 126.1(3) . . . . ? O11 Sb2 C1 C6 -23.1(18) 3_777 . . . ? O3 Sb2 C1 C6 -142.8(3) . . . . ? O5 Sb2 C1 C6 31.2(4) . . . . ? O2 Sb2 C1 C6 -55.8(3) . . . . ? O4 Sb2 C1 C2 -49.7(3) . . . . ? O11 Sb2 C1 C2 161.1(14) 3_777 . . . ? O3 Sb2 C1 C2 41.4(3) . . . . ? O5 Sb2 C1 C2 -144.6(3) . . . . ? O2 Sb2 C1 C2 128.4(3) . . . . ? O4 Sb1 C7 C12 -144.8(4) . . . . ? O11 Sb1 C7 C12 44.5(19) . . . . ? O6 Sb1 C7 C12 -52.6(4) . . . . ? O9 Sb1 C7 C12 123.0(4) . . . . ? O10 Sb1 C7 C12 34.2(4) . . . . ? O4 Sb1 C7 C8 29.6(4) . . . . ? O11 Sb1 C7 C8 -141.1(15) . . . . ? O6 Sb1 C7 C8 121.8(4) . . . . ? O9 Sb1 C7 C8 -62.6(4) . . . . ? O10 Sb1 C7 C8 -151.4(4) . . . . ? C6 C1 C2 C3 0.2(7) . . . . ? Sb2 C1 C2 C3 176.1(3) . . . . ? C2 C1 C6 C5 1.5(6) . . . . ? Sb2 C1 C6 C5 -174.3(3) . . . . ? C15 C14 C13 C18 -0.7(7) . . . . ? C15 C14 C13 P2 175.6(4) . . . . ? O7 P2 C13 C18 -15.5(4) . . . . ? O6 P2 C13 C18 -138.0(4) . . . . ? O3 P2 C13 C18 106.1(4) 3_777 . . . ? O7 P2 C13 C14 168.3(4) . . . . ? O6 P2 C13 C14 45.8(4) . . . . ? O3 P2 C13 C14 -70.1(4) 3_777 . . . ? C5 C4 C3 C2 1.2(7) . . . . ? Cl1 C4 C3 C2 -177.7(3) . . . . ? C1 C2 C3 C4 -1.6(7) . . . . ? C14 C13 C18 C17 0.7(7) . . . . ? P2 C13 C18 C17 -175.5(4) . . . . ? C13 C14 C15 C16 0.6(8) . . . . ? C9 C10 C11 C12 -0.6(8) . . . . ? Cl2 C10 C11 C12 -177.3(4) . . . . ? C3 C4 C5 C6 0.5(7) . . . . ? Cl1 C4 C5 C6 179.4(3) . . . . ? C1 C6 C5 C4 -1.9(7) . . . . ? C13 C18 C17 C16 -0.5(8) . . . . ? O4 Sb1 O11 Sb2 130.8(2) . . . 3_777 ? O6 Sb1 O11 Sb2 38.6(2) . . . 3_777 ? O9 Sb1 O11 Sb2 -137.9(2) . . . 3_777 ? O10 Sb1 O11 Sb2 -48.3(2) . . . 3_777 ? C7 Sb1 O11 Sb2 -58.6(18) . . . 3_777 ? O4 Sb1 O11 Co3 -101.68(13) . . . 3_777 ? O6 Sb1 O11 Co3 166.11(13) . . . 3_777 ? O9 Sb1 O11 Co3 -10.30(12) . . . 3_777 ? O10 Sb1 O11 Co3 79.30(13) . . . 3_777 ? C7 Sb1 O11 Co3 69.0(17) . . . 3_777 ? O8 P1 C19 C24 -154.7(4) . . . . ? O2 P1 C19 C24 -30.7(4) . . . . ? O10 P1 C19 C24 83.9(4) 3_777 . . . ? O8 P1 C19 C20 28.7(4) . . . . ? O2 P1 C19 C20 152.7(4) . . . . ? O10 P1 C19 C20 -92.7(4) 3_777 . . . ? C29 C28 C27 C26 -0.9(8) . . . . ? C29 C28 C27 C50 176.0(5) . . . . ? C25 N1 C29 C28 2.6(7) . . . . ? Co3 N1 C29 C28 -177.5(4) . . . . ? C27 C28 C29 N1 -0.9(8) . . . . ? C29 N1 C25 C26 -2.4(8) . . . . ? Co3 N1 C25 C26 177.7(4) . . . . ? C24 C19 C20 C21 -1.8(7) . . . . ? P1 C19 C20 C21 174.9(4) . . . . ? C20 C19 C24 C23 0.5(7) . . . . ? P1 C19 C24 C23 -176.0(4) . . . . ? C28 C27 C26 C25 1.0(8) . . . . ? C50 C27 C26 C25 -175.8(5) . . . . ? N1 C25 C26 C27 0.7(9) . . . . ? C18 C17 C16 C15 0.4(9) . . . . ? C14 C15 C16 C17 -0.4(9) . . . . ? C10 C11 C12 C7 -0.1(7) . . . . ? C8 C7 C12 C11 1.0(7) . . . . ? Sb1 C7 C12 C11 175.5(4) . . . . ? C10 C9 C8 C7 0.6(8) . . . . ? C12 C7 C8 C9 -1.2(7) . . . . ? Sb1 C7 C8 C9 -175.8(4) . . . . ? C19 C24 C23 C22 0.9(8) . . . . ? C19 C20 C21 C22 1.8(8) . . . . ? C20 C21 C22 C23 -0.4(9) . . . . ? C24 C23 C22 C21 -0.9(8) . . . . ? C26 C27 C50 C51 -34.3(8) . . . . ? C28 C27 C50 C51 149.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.159 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.137 # Attachment '- 10.cif' data_orepw819 _database_code_depnum_ccdc_archive 'CCDC 778680' #TrackingRef '- 10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H60 Cl4 Co2 O24 P4 Sb4' _chemical_formula_weight 1987.58 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 11.1154(2) _cell_length_b 12.1890(2) _cell_length_c 14.4207(3) _cell_angle_alpha 101.7145(18) _cell_angle_beta 106.7716(17) _cell_angle_gamma 101.3563(15) _cell_volume 1762.39(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24364 _cell_measurement_theta_min 2.6436 _cell_measurement_theta_max 28.3598 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 974 _exptl_absorpt_coefficient_mu 2.287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4614 _exptl_absorpt_correction_T_max 0.8035 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35037 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7175 _reflns_number_gt 6152 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The short intermolecular contacts were due to the disorder of two methanol solvent molecules and a phenyl rings C21-C26 which was modelled susscssfully. A slight diorder in phenyl ring C13-C18 was also present. 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^)+(0.0221P)^2^+3.1128P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7175 _refine_ls_number_parameters 479 _refine_ls_number_restraints 308 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0539 _refine_ls_wR_factor_gt 0.0477 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.027 _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 Sb1 Sb 0.285623(15) 0.332547(14) 0.408640(12) 0.01182(5) Uani 1 1 d . . . Sb2 Sb 0.589216(15) 0.373837(14) 0.614727(12) 0.01152(5) Uani 1 1 d . . . P1 P 0.50671(6) 0.60718(5) 0.71258(5) 0.01163(12) Uani 1 1 d . . . P2 P 0.88635(6) 0.52705(6) 0.71298(5) 0.01550(14) Uani 1 1 d . . . O1 O 0.41433(16) 0.30951(15) 0.51926(13) 0.0149(4) Uani 1 1 d . . . O2 O 0.77140(17) 0.44045(16) 0.72267(13) 0.0162(4) Uani 1 1 d . A . O3 O 0.92088(17) 0.47818(17) 0.62226(13) 0.0181(4) Uani 1 1 d . A . O4 O 0.52679(17) 0.48387(15) 0.70127(13) 0.0146(4) Uani 1 1 d . . . O5 O 0.35907(16) 0.50367(14) 0.44835(12) 0.0117(3) Uani 1 1 d . . . O6 O 0.39574(17) 0.31607(15) 0.32144(13) 0.0148(4) Uani 1 1 d . . . O7 O 0.18106(17) 0.38306(16) 0.49476(13) 0.0164(4) Uani 1 1 d . . . O8 O 0.14814(16) 0.35610(16) 0.28924(13) 0.0159(4) Uani 1 1 d . . . O9 O 0.89075(18) 0.37835(18) 0.41461(14) 0.0224(4) Uani 1 1 d . . . O10 O 0.63171(17) 0.39281(16) 0.33675(13) 0.0165(4) Uani 1 1 d . . . O11 O 0.67136(18) 0.29078(15) 0.52353(13) 0.0166(4) Uani 1 1 d . . . C1 C 0.1857(3) 0.1528(2) 0.3568(2) 0.0182(5) Uani 1 1 d U . . C2 C 0.2177(3) 0.0800(3) 0.4178(2) 0.0251(6) Uani 1 1 d U . . H2 H 0.2863 0.1112 0.4811 0.030 Uiso 1 1 calc R . . C3 C 0.1507(3) -0.0371(3) 0.3876(2) 0.0293(7) Uani 1 1 d U . . H3 H 0.1715 -0.0858 0.4301 0.035 Uiso 1 1 calc R . . C4 C 0.0534(3) -0.0815(3) 0.2944(2) 0.0278(7) Uani 1 1 d U . . C5 C 0.0214(3) -0.0128(3) 0.2313(2) 0.0333(7) Uani 1 1 d U . . H5 H -0.0451 -0.0452 0.1670 0.040 Uiso 1 1 calc R . . C6 C 0.0881(3) 0.1046(3) 0.2631(2) 0.0277(7) Uani 1 1 d U . . H6 H 0.0667 0.1527 0.2201 0.033 Uiso 1 1 calc R . . C7 C 0.5621(3) 0.2416(2) 0.68751(19) 0.0187(5) Uani 1 1 d U . . C8 C 0.6642(3) 0.1948(3) 0.7247(2) 0.0265(6) Uani 1 1 d U . . H8 H 0.7477 0.2263 0.7215 0.032 Uiso 1 1 calc R . . C9 C 0.6457(4) 0.1025(3) 0.7665(2) 0.0347(7) Uani 1 1 d U . . H9 H 0.7158 0.0708 0.7920 0.042 Uiso 1 1 calc R . . C10 C 0.5243(4) 0.0577(3) 0.7704(2) 0.0317(7) Uani 1 1 d U . . C11 C 0.4207(3) 0.1017(3) 0.7335(2) 0.0310(7) Uani 1 1 d U . . H11 H 0.3373 0.0690 0.7364 0.037 Uiso 1 1 calc R . . C12 C 0.4398(3) 0.1944(2) 0.6919(2) 0.0247(6) Uani 1 1 d U . . H12 H 0.3693 0.2256 0.6665 0.030 Uiso 1 1 calc R . . C13 C 0.5590(3) 0.6692(2) 0.84614(19) 0.0167(5) Uani 1 1 d . . . C14 C 0.4796(3) 0.7053(3) 0.8958(2) 0.0279(7) Uani 1 1 d . . . H14 H 0.3913 0.6987 0.8589 0.033 Uiso 1 1 calc R . . C15 C 0.5275(3) 0.7517(3) 1.0003(2) 0.0350(8) Uani 1 1 d . . . H15 H 0.4723 0.7771 1.0344 0.042 Uiso 1 1 calc R . . C16 C 0.6548(3) 0.7605(3) 1.0537(2) 0.0369(8) Uani 1 1 d . . . H16 H 0.6868 0.7896 1.1251 0.044 Uiso 1 1 calc R . . C17 C 0.7353(4) 0.7278(5) 1.0049(3) 0.0676(16) Uani 1 1 d . . . H17 H 0.8240 0.7358 1.0418 0.081 Uiso 1 1 calc R . . C18 C 0.6876(4) 0.6825(5) 0.9009(3) 0.0624(15) Uani 1 1 d . . . H18 H 0.7443 0.6603 0.8669 0.075 Uiso 1 1 calc R . . C19 C 0.6006(3) 0.1760(2) 0.4583(2) 0.0222(6) Uani 1 1 d . . . H19A H 0.5632 0.1291 0.4961 0.033 Uiso 1 1 calc R . . H19B H 0.6601 0.1393 0.4330 0.033 Uiso 1 1 calc R . . H19C H 0.5303 0.1815 0.4015 0.033 Uiso 1 1 calc R . . C20 C 0.1563(3) 0.3271(3) 0.5681(2) 0.0234(6) Uani 1 1 d . . . H20A H 0.1411 0.2429 0.5424 0.035 Uiso 1 1 calc R . . H20B H 0.0791 0.3431 0.5816 0.035 Uiso 1 1 calc R . . H20C H 0.2320 0.3571 0.6306 0.035 Uiso 1 1 calc R . . Cl1 Cl -0.02761(9) -0.22989(7) 0.25493(6) 0.0423(2) Uani 1 1 d . . . C21 C 1.0236(9) 0.5690(7) 0.8299(4) 0.019(2) Uani 0.491(11) 1 d PGU A 1 C22 C 1.1187(12) 0.5091(8) 0.8365(7) 0.023(2) Uani 0.491(11) 1 d PGU A 1 H22 H 1.1182 0.4565 0.7778 0.028 Uiso 0.491(11) 1 calc PR A 1 C23 C 1.2144(9) 0.5261(9) 0.9289(9) 0.025(2) Uani 0.491(11) 1 d PGU A 1 H23 H 1.2794 0.4852 0.9333 0.030 Uiso 0.491(11) 1 calc PR A 1 C24 C 1.2151(6) 0.6031(8) 1.0147(7) 0.038(3) Uani 0.491(11) 1 d PGU A 1 H24 H 1.2805 0.6147 1.0778 0.046 Uiso 0.491(11) 1 calc PR A 1 C25 C 1.1200(6) 0.6630(8) 1.0081(4) 0.0335(18) Uani 0.491(11) 1 d PGU A 1 H25 H 1.1205 0.7155 1.0668 0.040 Uiso 0.491(11) 1 calc PR A 1 C26 C 1.0243(6) 0.6459(7) 0.9158(4) 0.0267(16) Uani 0.491(11) 1 d PGU A 1 H26 H 0.9593 0.6868 0.9113 0.032 Uiso 0.491(11) 1 calc PR A 1 Co1 Co 0.76349(3) 0.43351(3) 0.47893(3) 0.01440(8) Uani 1 1 d . . 1 C21A C 1.0158(8) 0.5471(6) 0.8276(4) 0.0150(18) Uani 0.509(11) 1 d PGU A 2 C22A C 1.1327(10) 0.5233(9) 0.8267(6) 0.0163(18) Uani 0.509(11) 1 d PGU A 2 H22A H 1.1447 0.4955 0.7644 0.020 Uiso 0.509(11) 1 calc PR A 2 C23A C 1.2322(8) 0.5400(9) 0.9170(9) 0.029(2) Uani 0.509(11) 1 d PGU A 2 H23A H 1.3122 0.5237 0.9163 0.035 Uiso 0.509(11) 1 calc PR A 2 C24A C 1.2148(5) 0.5806(7) 1.0081(6) 0.032(2) Uani 0.509(11) 1 d PGU A 2 H24A H 1.2828 0.5920 1.0698 0.038 Uiso 0.509(11) 1 calc PR A 2 C25A C 1.0978(6) 0.6045(7) 1.0090(4) 0.0338(17) Uani 0.509(11) 1 d PGU A 2 H25A H 1.0859 0.6322 1.0713 0.041 Uiso 0.509(11) 1 calc PR A 2 C26A C 0.9983(5) 0.5877(7) 0.9188(4) 0.0266(16) Uani 0.509(11) 1 d PGU A 2 H26A H 0.9184 0.6040 0.9194 0.032 Uiso 0.509(11) 1 calc PR A 2 Cl2 Cl 0.50028(12) -0.05774(7) 0.82337(7) 0.0501(3) Uani 1 1 d . . . C27 C 0.8561(3) 0.2688(3) 0.3422(3) 0.0318(7) Uani 1 1 d . . . H27A H 0.7622 0.2328 0.3221 0.048 Uiso 1 1 calc R . . H27B H 0.9047 0.2180 0.3716 0.048 Uiso 1 1 calc R . . H27C H 0.8777 0.2802 0.2829 0.048 Uiso 1 1 calc R . . C28 C 0.2180(18) 0.9069(15) 0.9492(10) 0.153(10) Uani 0.491(11) 1 d PD A 1 H56A H 0.3129 0.9217 0.9674 0.229 Uiso 0.491(11) 1 calc PR A 1 H56B H 0.1796 0.9053 0.8785 0.229 Uiso 0.491(11) 1 calc PR A 1 H56C H 0.1815 0.8318 0.9588 0.229 Uiso 0.491(11) 1 calc PR A 1 O20 O 0.189(2) 0.995(2) 1.0105(19) 0.164(7) Uani 0.491(11) 1 d PDU A 1 C28A C -0.011(3) 0.9039(12) 0.9829(9) 0.158(10) Uani 0.509(11) 1 d PD A 2 H56D H -0.0116 0.8217 0.9677 0.237 Uiso 0.509(11) 1 calc PR A 2 H56E H -0.0649 0.9193 0.9225 0.237 Uiso 0.509(11) 1 calc PR A 2 H56F H -0.0468 0.9218 1.0371 0.237 Uiso 0.509(11) 1 calc PR A 2 O20A O 0.123(2) 0.977(3) 1.015(2) 0.218(10) Uani 0.509(11) 1 d PDU A 2 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 Sb1 0.00958(8) 0.01360(9) 0.00996(8) 0.00174(6) 0.00256(6) 0.00076(6) Sb2 0.01185(8) 0.01173(8) 0.00972(8) 0.00184(6) 0.00247(6) 0.00345(6) P1 0.0117(3) 0.0132(3) 0.0095(3) 0.0009(2) 0.0044(2) 0.0034(2) P2 0.0103(3) 0.0232(3) 0.0108(3) 0.0022(3) 0.0014(2) 0.0056(3) O1 0.0131(8) 0.0136(9) 0.0135(9) 0.0042(7) 0.0002(7) -0.0002(7) O2 0.0133(9) 0.0207(9) 0.0126(9) 0.0039(7) 0.0020(7) 0.0049(7) O3 0.0114(8) 0.0271(10) 0.0147(9) 0.0028(8) 0.0029(7) 0.0085(8) O4 0.0168(9) 0.0152(9) 0.0127(9) 0.0025(7) 0.0070(7) 0.0048(7) O5 0.0122(8) 0.0122(8) 0.0109(8) 0.0021(7) 0.0053(7) 0.0026(7) O6 0.0147(9) 0.0145(9) 0.0156(9) 0.0024(7) 0.0069(7) 0.0043(7) O7 0.0138(9) 0.0223(10) 0.0143(9) 0.0056(7) 0.0075(7) 0.0027(7) O8 0.0119(8) 0.0193(9) 0.0123(9) 0.0012(7) 0.0010(7) 0.0026(7) O9 0.0145(9) 0.0322(11) 0.0187(10) -0.0014(8) 0.0070(8) 0.0094(8) O10 0.0122(9) 0.0226(10) 0.0136(9) 0.0021(7) 0.0041(7) 0.0057(7) O11 0.0201(9) 0.0161(9) 0.0136(9) 0.0008(7) 0.0056(7) 0.0084(7) C1 0.0153(12) 0.0202(13) 0.0159(13) 0.0022(10) 0.0072(10) -0.0020(10) C2 0.0262(15) 0.0224(14) 0.0166(13) 0.0027(11) -0.0006(11) -0.0009(12) C3 0.0351(17) 0.0220(15) 0.0211(14) 0.0078(12) 0.0014(13) -0.0033(13) C4 0.0320(16) 0.0180(14) 0.0216(14) 0.0020(11) 0.0047(12) -0.0086(12) C5 0.0359(17) 0.0257(16) 0.0199(15) 0.0022(12) -0.0036(13) -0.0085(13) C6 0.0295(16) 0.0244(15) 0.0203(14) 0.0094(12) -0.0004(12) -0.0024(12) C7 0.0278(14) 0.0138(12) 0.0114(12) 0.0013(10) 0.0038(11) 0.0052(11) C8 0.0324(16) 0.0233(15) 0.0223(15) 0.0072(12) 0.0049(12) 0.0096(12) C9 0.051(2) 0.0251(16) 0.0281(16) 0.0114(13) 0.0057(15) 0.0167(15) C10 0.062(2) 0.0151(14) 0.0163(14) 0.0068(11) 0.0124(14) 0.0073(14) C11 0.0466(19) 0.0192(15) 0.0253(15) 0.0034(12) 0.0162(14) 0.0018(13) C12 0.0342(16) 0.0196(14) 0.0210(14) 0.0055(11) 0.0115(12) 0.0062(12) C13 0.0188(13) 0.0170(13) 0.0126(12) 0.0013(10) 0.0049(10) 0.0047(10) C14 0.0194(14) 0.0412(18) 0.0183(14) 0.0008(13) 0.0064(12) 0.0054(13) C15 0.0337(17) 0.048(2) 0.0196(15) -0.0026(14) 0.0142(13) 0.0074(15) C16 0.0397(19) 0.048(2) 0.0119(14) -0.0032(13) 0.0032(13) 0.0078(16) C17 0.036(2) 0.126(4) 0.0209(18) -0.016(2) -0.0073(16) 0.042(3) C18 0.034(2) 0.123(4) 0.0187(17) -0.013(2) 0.0004(15) 0.043(2) C19 0.0303(15) 0.0176(13) 0.0171(13) 0.0002(11) 0.0064(12) 0.0099(12) C20 0.0244(14) 0.0331(16) 0.0207(14) 0.0120(12) 0.0147(12) 0.0105(12) Cl1 0.0512(5) 0.0238(4) 0.0277(4) 0.0059(3) -0.0035(4) -0.0163(4) C21 0.016(4) 0.020(4) 0.017(3) 0.007(2) -0.001(3) 0.004(3) C22 0.021(4) 0.020(4) 0.023(4) 0.005(3) 0.003(3) 0.002(3) C23 0.011(3) 0.032(4) 0.028(4) 0.015(3) 0.000(3) 0.004(3) C24 0.025(4) 0.052(5) 0.022(4) 0.004(4) -0.007(4) 0.004(3) C25 0.027(3) 0.044(5) 0.018(3) -0.001(3) 0.002(2) 0.006(3) C26 0.021(3) 0.031(4) 0.021(3) 0.000(3) 0.003(2) 0.006(3) Co1 0.01039(16) 0.02068(18) 0.01160(16) 0.00181(14) 0.00388(13) 0.00563(14) C21A 0.009(3) 0.013(3) 0.016(3) 0.001(2) 0.000(3) -0.003(2) C22A 0.011(3) 0.015(3) 0.021(3) 0.007(3) 0.004(2) 0.001(3) C23A 0.018(4) 0.032(4) 0.030(4) 0.013(3) 0.001(3) -0.002(3) C24A 0.021(4) 0.043(4) 0.023(4) 0.017(3) -0.006(3) 0.002(3) C25A 0.035(4) 0.041(4) 0.018(3) 0.007(3) 0.002(2) 0.008(3) C26A 0.020(3) 0.035(4) 0.022(3) 0.006(3) 0.003(2) 0.009(3) Cl2 0.0923(8) 0.0238(4) 0.0319(4) 0.0163(3) 0.0172(5) 0.0078(4) C27 0.0289(16) 0.0295(17) 0.0378(18) 0.0011(14) 0.0180(14) 0.0083(13) C28 0.178(17) 0.156(15) 0.075(9) -0.026(9) -0.045(10) 0.129(14) O20 0.135(15) 0.257(15) 0.125(9) 0.094(10) 0.023(11) 0.103(14) C28A 0.31(3) 0.067(8) 0.039(6) 0.005(5) 0.035(10) -0.041(12) O20A 0.22(2) 0.317(18) 0.127(10) 0.090(11) 0.032(16) 0.092(19) _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 Sb1 O1 1.9218(17) . ? Sb1 O5 1.9798(17) . ? Sb1 O6 2.0005(17) . ? Sb1 O7 2.0191(17) . ? Sb1 O8 2.0584(17) . ? Sb1 C1 2.119(3) . ? Sb2 O1 1.9251(17) . ? Sb2 O5 1.9755(17) 2_666 ? Sb2 O4 2.0061(17) . ? Sb2 O11 2.0259(18) . ? Sb2 O2 2.0501(17) . ? Sb2 C7 2.114(3) . ? P1 O10 1.4973(18) 2_666 ? P1 O6 1.5445(18) 2_666 ? P1 O4 1.5457(18) . ? P1 C13 1.791(3) . ? P2 O3 1.5091(19) . ? P2 O2 1.5486(19) . ? P2 O8 1.5502(19) 2_666 ? P2 C21A 1.785(6) . ? P2 C21 1.815(7) . ? O3 Co1 2.1704(18) . ? O5 Sb2 1.9755(17) 2_666 ? O5 Co1 2.1097(17) 2_666 ? O6 P1 1.5445(18) 2_666 ? O7 C20 1.430(3) . ? O7 Co1 2.1214(19) 2_666 ? O8 P2 1.5502(19) 2_666 ? O9 C27 1.422(4) . ? O9 Co1 2.0474(18) . ? O10 P1 1.4972(18) 2_666 ? O10 Co1 2.0403(18) . ? O11 C19 1.437(3) . ? O11 Co1 2.1499(19) . ? C1 C6 1.389(4) . ? C1 C2 1.395(4) . ? C2 C3 1.387(4) . ? C2 H2 0.9500 . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C4 C5 1.377(4) . ? C4 Cl1 1.746(3) . ? C5 C6 1.388(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.389(4) . ? C7 C12 1.392(4) . ? C8 C9 1.388(4) . ? C8 H8 0.9500 . ? C9 C10 1.375(5) . ? C9 H9 0.9500 . ? C10 C11 1.379(5) . ? C10 Cl2 1.743(3) . ? C11 C12 1.392(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.370(4) . ? C13 C18 1.377(4) . ? C14 C15 1.395(4) . ? C14 H14 0.9500 . ? C15 C16 1.373(5) . ? C15 H15 0.9500 . ? C16 C17 1.358(5) . ? C16 H16 0.9500 . ? C17 C18 1.387(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 H22 0.9500 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? Co1 O5 2.1097(17) 2_666 ? Co1 O7 2.1215(19) 2_666 ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A H22A 0.9500 . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 O20 1.398(18) . ? C28 H56A 0.9800 . ? C28 H56B 0.9800 . ? C28 H56C 0.9800 . ? C28A O20A 1.460(17) . ? C28A H56D 0.9800 . ? C28A H56E 0.9800 . ? C28A H56F 0.9800 . ? 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 Sb1 O5 94.55(7) . . ? O1 Sb1 O6 91.86(7) . . ? O5 Sb1 O6 89.43(7) . . ? O1 Sb1 O7 92.93(7) . . ? O5 Sb1 O7 79.52(7) . . ? O6 Sb1 O7 168.26(7) . . ? O1 Sb1 O8 179.47(8) . . ? O5 Sb1 O8 85.77(7) . . ? O6 Sb1 O8 87.72(7) . . ? O7 Sb1 O8 87.54(7) . . ? O1 Sb1 C1 91.73(9) . . ? O5 Sb1 C1 173.18(9) . . ? O6 Sb1 C1 93.02(9) . . ? O7 Sb1 C1 97.53(9) . . ? O8 Sb1 C1 87.97(9) . . ? O1 Sb2 O5 95.81(7) . 2_666 ? O1 Sb2 O4 90.25(7) . . ? O5 Sb2 O4 89.99(7) 2_666 . ? O1 Sb2 O11 94.18(7) . . ? O5 Sb2 O11 79.56(7) 2_666 . ? O4 Sb2 O11 169.00(7) . . ? O1 Sb2 O2 176.75(7) . . ? O5 Sb2 O2 86.82(7) 2_666 . ? O4 Sb2 O2 87.84(7) . . ? O11 Sb2 O2 88.17(7) . . ? O1 Sb2 C7 91.03(9) . . ? O5 Sb2 C7 171.74(9) 2_666 . ? O4 Sb2 C7 94.63(9) . . ? O11 Sb2 C7 95.35(9) . . ? O2 Sb2 C7 86.51(9) . . ? O10 P1 O6 112.79(10) 2_666 2_666 ? O10 P1 O4 113.60(10) 2_666 . ? O6 P1 O4 110.62(10) 2_666 . ? O10 P1 C13 110.79(11) 2_666 . ? O6 P1 C13 104.37(11) 2_666 . ? O4 P1 C13 103.92(11) . . ? O3 P2 O2 112.01(11) . . ? O3 P2 O8 111.91(11) . 2_666 ? O2 P2 O8 109.04(10) . 2_666 ? O3 P2 C21A 111.3(2) . . ? O2 P2 C21A 102.7(3) . . ? O8 P2 C21A 109.4(3) 2_666 . ? O3 P2 C21 112.7(3) . . ? O2 P2 C21 108.7(3) . . ? O8 P2 C21 102.0(3) 2_666 . ? C21A P2 C21 8.1(4) . . ? Sb1 O1 Sb2 144.32(10) . . ? P2 O2 Sb2 124.52(10) . . ? P2 O3 Co1 114.66(10) . . ? P1 O4 Sb2 138.61(11) . . ? Sb2 O5 Sb1 138.24(9) 2_666 . ? Sb2 O5 Co1 103.71(7) 2_666 2_666 ? Sb1 O5 Co1 103.38(7) . 2_666 ? P1 O6 Sb1 139.77(11) 2_666 . ? C20 O7 Sb1 123.25(16) . . ? C20 O7 Co1 123.48(16) . 2_666 ? Sb1 O7 Co1 101.63(7) . 2_666 ? P2 O8 Sb1 124.23(10) 2_666 . ? C27 O9 Co1 122.70(17) . . ? P1 O10 Co1 138.26(11) 2_666 . ? C19 O11 Sb2 119.01(16) . . ? C19 O11 Co1 125.66(16) . . ? Sb2 O11 Co1 100.60(8) . . ? C6 C1 C2 118.6(3) . . ? C6 C1 Sb1 121.7(2) . . ? C2 C1 Sb1 119.72(19) . . ? C3 C2 C1 121.1(3) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 118.7(3) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C5 C4 C3 121.8(3) . . ? C5 C4 Cl1 119.6(2) . . ? C3 C4 Cl1 118.6(2) . . ? C4 C5 C6 118.9(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C5 C6 C1 121.0(3) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C12 119.3(3) . . ? C8 C7 Sb2 119.9(2) . . ? C12 C7 Sb2 120.6(2) . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 119.0(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 121.7(3) . . ? C9 C10 Cl2 119.3(3) . . ? C11 C10 Cl2 119.0(3) . . ? C10 C11 C12 119.2(3) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C11 C12 C7 120.1(3) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 C18 118.8(3) . . ? C14 C13 P1 123.9(2) . . ? C18 C13 P1 117.3(2) . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.8(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.3(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.8(3) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 120.9(3) . . ? C13 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? O11 C19 H19A 109.5 . . ? O11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O7 C20 H20A 109.5 . . ? O7 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O7 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 120.0 . . ? C22 C21 P2 118.3(5) . . ? C26 C21 P2 121.0(5) . . ? C21 C22 C23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? O10 Co1 O9 87.54(7) . . ? O10 Co1 O5 95.13(7) . 2_666 ? O9 Co1 O5 176.97(7) . 2_666 ? O10 Co1 O7 97.85(7) . 2_666 ? O9 Co1 O7 103.88(8) . 2_666 ? O5 Co1 O7 74.39(7) 2_666 2_666 ? O10 Co1 O11 97.21(7) . . ? O9 Co1 O11 107.22(8) . . ? O5 Co1 O11 73.89(7) 2_666 . ? O7 Co1 O11 145.86(7) 2_666 . ? O10 Co1 O3 173.42(7) . . ? O9 Co1 O3 86.38(7) . . ? O5 Co1 O3 90.88(7) 2_666 . ? O7 Co1 O3 81.20(7) 2_666 . ? O11 Co1 O3 86.99(7) . . ? C22A C21A C26A 120.0 . . ? C22A C21A P2 121.1(5) . . ? C26A C21A P2 118.9(5) . . ? C23A C22A C21A 120.0 . . ? C23A C22A H22A 120.0 . . ? C21A C22A H22A 120.0 . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C25A C26A C21A 120.0 . . ? C25A C26A H26A 120.0 . . ? C21A C26A H26A 120.0 . . ? O9 C27 H27A 109.5 . . ? O9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O20A C28A H56D 109.5 . . ? O20A C28A H56E 109.5 . . ? H56D C28A H56E 109.5 . . ? O20A C28A H56F 109.5 . . ? H56D C28A H56F 109.5 . . ? H56E C28A H56F 109.5 . . ? 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 O5 Sb1 O1 Sb2 -24.76(18) . . . . ? O6 Sb1 O1 Sb2 64.81(18) . . . . ? O7 Sb1 O1 Sb2 -104.48(17) . . . . ? O8 Sb1 O1 Sb2 102(8) . . . . ? C1 Sb1 O1 Sb2 157.89(18) . . . . ? O5 Sb2 O1 Sb1 -9.42(18) 2_666 . . . ? O4 Sb2 O1 Sb1 80.60(18) . . . . ? O11 Sb2 O1 Sb1 -89.33(18) . . . . ? O2 Sb2 O1 Sb1 134.5(12) . . . . ? C7 Sb2 O1 Sb1 175.23(18) . . . . ? O3 P2 O2 Sb2 -58.71(15) . . . . ? O8 P2 O2 Sb2 65.72(14) 2_666 . . . ? C21A P2 O2 Sb2 -178.3(3) . . . . ? C21 P2 O2 Sb2 176.1(3) . . . . ? O1 Sb2 O2 P2 -158.0(12) . . . . ? O5 Sb2 O2 P2 -13.97(13) 2_666 . . . ? O4 Sb2 O2 P2 -104.08(13) . . . . ? O11 Sb2 O2 P2 65.67(13) . . . . ? C7 Sb2 O2 P2 161.14(14) . . . . ? O2 P2 O3 Co1 59.74(14) . . . . ? O8 P2 O3 Co1 -63.08(13) 2_666 . . . ? C21A P2 O3 Co1 174.1(3) . . . . ? C21 P2 O3 Co1 -177.3(3) . . . . ? O10 P1 O4 Sb2 99.15(17) 2_666 . . . ? O6 P1 O4 Sb2 -28.87(19) 2_666 . . . ? C13 P1 O4 Sb2 -140.36(16) . . . . ? O1 Sb2 O4 P1 -89.12(17) . . . . ? O5 Sb2 O4 P1 6.69(17) 2_666 . . . ? O11 Sb2 O4 P1 24.7(5) . . . . ? O2 Sb2 O4 P1 93.50(17) . . . . ? C7 Sb2 O4 P1 179.82(17) . . . . ? O1 Sb1 O5 Sb2 130.49(13) . . . 2_666 ? O6 Sb1 O5 Sb2 38.67(14) . . . 2_666 ? O7 Sb1 O5 Sb2 -137.36(14) . . . 2_666 ? O8 Sb1 O5 Sb2 -49.08(13) . . . 2_666 ? C1 Sb1 O5 Sb2 -72.4(7) . . . 2_666 ? O1 Sb1 O5 Co1 -100.28(8) . . . 2_666 ? O6 Sb1 O5 Co1 167.90(8) . . . 2_666 ? O7 Sb1 O5 Co1 -8.13(7) . . . 2_666 ? O8 Sb1 O5 Co1 80.14(8) . . . 2_666 ? C1 Sb1 O5 Co1 56.8(7) . . . 2_666 ? O1 Sb1 O6 P1 -97.54(17) . . . 2_666 ? O5 Sb1 O6 P1 -3.01(17) . . . 2_666 ? O7 Sb1 O6 P1 16.6(5) . . . 2_666 ? O8 Sb1 O6 P1 82.78(17) . . . 2_666 ? C1 Sb1 O6 P1 170.63(18) . . . 2_666 ? O1 Sb1 O7 C20 -41.8(2) . . . . ? O5 Sb1 O7 C20 -135.9(2) . . . . ? O6 Sb1 O7 C20 -155.8(3) . . . . ? O8 Sb1 O7 C20 137.9(2) . . . . ? C1 Sb1 O7 C20 50.3(2) . . . . ? O1 Sb1 O7 Co1 102.12(8) . . . 2_666 ? O5 Sb1 O7 Co1 8.03(7) . . . 2_666 ? O6 Sb1 O7 Co1 -11.9(4) . . . 2_666 ? O8 Sb1 O7 Co1 -78.12(8) . . . 2_666 ? C1 Sb1 O7 Co1 -165.75(9) . . . 2_666 ? O1 Sb1 O8 P2 -148(8) . . . 2_666 ? O5 Sb1 O8 P2 -21.18(12) . . . 2_666 ? O6 Sb1 O8 P2 -110.77(13) . . . 2_666 ? O7 Sb1 O8 P2 58.49(13) . . . 2_666 ? C1 Sb1 O8 P2 156.12(14) . . . 2_666 ? O1 Sb2 O11 C19 -34.84(18) . . . . ? O5 Sb2 O11 C19 -129.99(18) 2_666 . . . ? O4 Sb2 O11 C19 -148.3(3) . . . . ? O2 Sb2 O11 C19 142.91(18) . . . . ? C7 Sb2 O11 C19 56.59(19) . . . . ? O1 Sb2 O11 Co1 106.61(8) . . . . ? O5 Sb2 O11 Co1 11.46(7) 2_666 . . . ? O4 Sb2 O11 Co1 -6.9(4) . . . . ? O2 Sb2 O11 Co1 -75.64(8) . . . . ? C7 Sb2 O11 Co1 -161.96(9) . . . . ? O1 Sb1 C1 C6 -168.6(2) . . . . ? O5 Sb1 C1 C6 34.2(8) . . . . ? O6 Sb1 C1 C6 -76.7(2) . . . . ? O7 Sb1 C1 C6 98.2(2) . . . . ? O8 Sb1 C1 C6 10.9(2) . . . . ? O1 Sb1 C1 C2 11.5(2) . . . . ? O5 Sb1 C1 C2 -145.6(6) . . . . ? O6 Sb1 C1 C2 103.5(2) . . . . ? O7 Sb1 C1 C2 -81.6(2) . . . . ? O8 Sb1 C1 C2 -168.9(2) . . . . ? C6 C1 C2 C3 -2.2(5) . . . . ? Sb1 C1 C2 C3 177.6(2) . . . . ? C1 C2 C3 C4 1.5(5) . . . . ? C2 C3 C4 C5 0.0(5) . . . . ? C2 C3 C4 Cl1 178.2(3) . . . . ? C3 C4 C5 C6 -0.8(5) . . . . ? Cl1 C4 C5 C6 -179.0(3) . . . . ? C4 C5 C6 C1 0.1(5) . . . . ? C2 C1 C6 C5 1.4(5) . . . . ? Sb1 C1 C6 C5 -178.4(3) . . . . ? O1 Sb2 C7 C8 142.6(2) . . . . ? O5 Sb2 C7 C8 -3.3(7) 2_666 . . . ? O4 Sb2 C7 C8 -127.1(2) . . . . ? O11 Sb2 C7 C8 48.3(2) . . . . ? O2 Sb2 C7 C8 -39.6(2) . . . . ? O1 Sb2 C7 C12 -32.5(2) . . . . ? O5 Sb2 C7 C12 -178.4(5) 2_666 . . . ? O4 Sb2 C7 C12 57.8(2) . . . . ? O11 Sb2 C7 C12 -126.8(2) . . . . ? O2 Sb2 C7 C12 145.3(2) . . . . ? C12 C7 C8 C9 -0.4(4) . . . . ? Sb2 C7 C8 C9 -175.6(2) . . . . ? C7 C8 C9 C10 0.1(5) . . . . ? C8 C9 C10 C11 0.4(5) . . . . ? C8 C9 C10 Cl2 -179.7(2) . . . . ? C9 C10 C11 C12 -0.6(5) . . . . ? Cl2 C10 C11 C12 179.5(2) . . . . ? C10 C11 C12 C7 0.3(4) . . . . ? C8 C7 C12 C11 0.2(4) . . . . ? Sb2 C7 C12 C11 175.3(2) . . . . ? O10 P1 C13 C14 3.4(3) 2_666 . . . ? O6 P1 C13 C14 125.1(3) 2_666 . . . ? O4 P1 C13 C14 -119.0(3) . . . . ? O10 P1 C13 C18 -175.6(3) 2_666 . . . ? O6 P1 C13 C18 -53.9(3) 2_666 . . . ? O4 P1 C13 C18 62.1(3) . . . . ? C18 C13 C14 C15 -1.7(5) . . . . ? P1 C13 C14 C15 179.3(3) . . . . ? C13 C14 C15 C16 -0.4(5) . . . . ? C14 C15 C16 C17 2.2(6) . . . . ? C15 C16 C17 C18 -1.7(8) . . . . ? C14 C13 C18 C17 2.2(7) . . . . ? P1 C13 C18 C17 -178.8(4) . . . . ? C16 C17 C18 C13 -0.5(9) . . . . ? O3 P2 C21 C22 -29.3(5) . . . . ? O2 P2 C21 C22 95.4(4) . . . . ? O8 P2 C21 C22 -149.5(4) 2_666 . . . ? C21A P2 C21 C22 53(3) . . . . ? O3 P2 C21 C26 160.5(4) . . . . ? O2 P2 C21 C26 -74.7(5) . . . . ? O8 P2 C21 C26 40.4(5) 2_666 . . . ? C21A P2 C21 C26 -117(4) . . . . ? C26 C21 C22 C23 0.0 . . . . ? P2 C21 C22 C23 -170.3(6) . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C21 0.0 . . . . ? C22 C21 C26 C25 0.0 . . . . ? P2 C21 C26 C25 170.0(6) . . . . ? P1 O10 Co1 O9 177.36(18) 2_666 . . . ? P1 O10 Co1 O5 -4.06(18) 2_666 . . 2_666 ? P1 O10 Co1 O7 -78.97(18) 2_666 . . 2_666 ? P1 O10 Co1 O11 70.31(18) 2_666 . . . ? P1 O10 Co1 O3 -160.2(6) 2_666 . . . ? C27 O9 Co1 O10 -50.6(2) . . . . ? C27 O9 Co1 O5 157.2(14) . . . 2_666 ? C27 O9 Co1 O7 -148.1(2) . . . 2_666 ? C27 O9 Co1 O11 46.2(2) . . . . ? C27 O9 Co1 O3 131.9(2) . . . . ? C19 O11 Co1 O10 33.6(2) . . . . ? Sb2 O11 Co1 O10 -104.27(8) . . . . ? C19 O11 Co1 O9 -56.1(2) . . . . ? Sb2 O11 Co1 O9 166.08(7) . . . . ? C19 O11 Co1 O5 126.9(2) . . . 2_666 ? Sb2 O11 Co1 O5 -10.98(7) . . . 2_666 ? C19 O11 Co1 O7 149.20(18) . . . 2_666 ? Sb2 O11 Co1 O7 11.32(16) . . . 2_666 ? C19 O11 Co1 O3 -141.32(19) . . . . ? Sb2 O11 Co1 O3 80.81(8) . . . . ? P2 O3 Co1 O10 159.0(6) . . . . ? P2 O3 Co1 O9 -178.49(13) . . . . ? P2 O3 Co1 O5 2.81(12) . . . 2_666 ? P2 O3 Co1 O7 76.86(12) . . . 2_666 ? P2 O3 Co1 O11 -71.01(12) . . . . ? O3 P2 C21A C22A 2.5(5) . . . . ? O2 P2 C21A C22A 122.5(4) . . . . ? O8 P2 C21A C22A -121.8(4) 2_666 . . . ? C21 P2 C21A C22A -99(3) . . . . ? O3 P2 C21A C26A -177.7(4) . . . . ? O2 P2 C21A C26A -57.7(5) . . . . ? O8 P2 C21A C26A 58.0(5) 2_666 . . . ? C21 P2 C21A C26A 81(3) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? P2 C21A C22A C23A 179.8(5) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C22A C21A C26A C25A 0.0 . . . . ? P2 C21A C26A C25A -179.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.909 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.091 # Attachment '- 11.cif' data_orepw855 _database_code_depnum_ccdc_archive 'CCDC 700896' #TrackingRef '- 11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H26 Cl2 Co N O10 P2 Sb2' _chemical_formula_weight 971.77 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 11.221(5) _cell_length_b 11.658(5) _cell_length_c 14.044(5) _cell_angle_alpha 74.222(5) _cell_angle_beta 77.714(5) _cell_angle_gamma 70.916(5) _cell_volume 1655.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8869 _cell_measurement_theta_min 3.0332 _cell_measurement_theta_max 28.3567 _exptl_crystal_description block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 2.430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6422 _exptl_absorpt_correction_T_max 0.7932 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15385 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.22 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6731 _reflns_number_gt 5122 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The residual Q peaks were around heavy element Sb and were left as such. 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^)+(0.0470P)^2^+1.0067P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6731 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Sb1 Sb 0.17073(2) 0.59040(2) 0.37774(2) 0.01304(8) Uani 1 1 d . . . Sb2 Sb 0.00962(2) 0.36101(2) 0.38103(2) 0.01310(8) Uani 1 1 d . . . Co1 Co 0.27561(5) 0.29484(5) 0.46161(4) 0.01376(13) Uani 1 1 d . . . P1 P -0.12061(10) 0.66626(9) 0.31589(8) 0.0139(2) Uani 1 1 d . . . P2 P 0.25976(10) 0.39759(9) 0.23596(8) 0.0149(2) Uani 1 1 d . . . C1 C 0.2496(4) 0.7405(4) 0.3132(3) 0.0164(9) Uani 1 1 d . . . C2 C 0.2735(5) 0.8051(4) 0.3741(3) 0.0287(11) Uani 1 1 d . . . H2 H 0.2539 0.7815 0.4446 0.034 Uiso 1 1 calc R . . C3 C 0.3251(5) 0.9027(5) 0.3330(4) 0.0319(12) Uani 1 1 d . . . H3 H 0.3409 0.9465 0.3747 0.038 Uiso 1 1 calc R . . C4 C 0.3534(4) 0.9361(4) 0.2315(4) 0.0220(10) Uani 1 1 d . . . C5 C 0.3273(5) 0.8768(4) 0.1695(4) 0.0272(11) Uani 1 1 d . . . H5 H 0.3457 0.9018 0.0990 0.033 Uiso 1 1 calc R . . C6 C 0.2741(5) 0.7803(4) 0.2113(4) 0.0257(10) Uani 1 1 d . . . H6 H 0.2539 0.7404 0.1688 0.031 Uiso 1 1 calc R . . C7 C -0.0746(4) 0.2659(4) 0.3188(3) 0.0160(9) Uani 1 1 d . . . C8 C -0.0001(4) 0.1621(4) 0.2814(3) 0.0217(10) Uani 1 1 d . . . H8 H 0.0889 0.1338 0.2845 0.026 Uiso 1 1 calc R . . C9 C -0.0545(5) 0.0993(4) 0.2397(4) 0.0266(11) Uani 1 1 d . . . H9 H -0.0042 0.0271 0.2158 0.032 Uiso 1 1 calc R . . C10 C -0.1829(5) 0.1439(4) 0.2338(3) 0.0244(10) Uani 1 1 d . . . C11 C -0.2588(5) 0.2461(4) 0.2722(4) 0.0286(11) Uani 1 1 d . . . H11 H -0.3476 0.2744 0.2686 0.034 Uiso 1 1 calc R . . C12 C -0.2048(4) 0.3064(4) 0.3155(4) 0.0235(10) Uani 1 1 d . . . H12 H -0.2566 0.3754 0.3430 0.028 Uiso 1 1 calc R . . C13 C 0.3259(4) 0.3958(4) 0.1091(3) 0.0194(9) Uani 1 1 d . . . C14 C 0.4562(4) 0.3460(4) 0.0844(4) 0.0264(11) Uani 1 1 d . . . H14 H 0.5092 0.3090 0.1357 0.032 Uiso 1 1 calc R . . C15 C 0.5086(5) 0.3500(5) -0.0142(4) 0.0360(13) Uani 1 1 d . . . H15 H 0.5976 0.3153 -0.0305 0.043 Uiso 1 1 calc R . . C16 C 0.4329(6) 0.4040(5) -0.0891(4) 0.0407(14) Uani 1 1 d . . . H16 H 0.4698 0.4072 -0.1569 0.049 Uiso 1 1 calc R . . C17 C 0.3040(6) 0.4532(5) -0.0659(4) 0.0394(14) Uani 1 1 d . . . H17 H 0.2519 0.4898 -0.1176 0.047 Uiso 1 1 calc R . . C18 C 0.2495(5) 0.4495(4) 0.0334(4) 0.0296(11) Uani 1 1 d . . . H18 H 0.1603 0.4837 0.0494 0.036 Uiso 1 1 calc R . . C19 C -0.0462(5) 0.7259(5) 0.1148(4) 0.0388(13) Uani 1 1 d . . . H19 H 0.0377 0.6872 0.1316 0.047 Uiso 1 1 calc R . . C20 C -0.0646(5) 0.7701(6) 0.0157(4) 0.0455(15) Uani 1 1 d . . . H20 H 0.0064 0.7616 -0.0353 0.055 Uiso 1 1 calc R . . C21 C -0.1855(5) 0.8262(5) -0.0091(4) 0.0399(14) Uani 1 1 d . . . H21 H -0.1978 0.8567 -0.0773 0.048 Uiso 1 1 calc R . . C22 C -0.2878(5) 0.8382(5) 0.0639(4) 0.0312(12) Uani 1 1 d . . . H22 H -0.3711 0.8778 0.0463 0.037 Uiso 1 1 calc R . . C23 C -0.2707(4) 0.7931(4) 0.1635(3) 0.0224(10) Uani 1 1 d . . . H23 H -0.3425 0.8002 0.2139 0.027 Uiso 1 1 calc R . . C24 C -0.1490(4) 0.7375(4) 0.1902(3) 0.0179(9) Uani 1 1 d . . . C25 C 0.4195(4) 0.0432(4) 0.5751(3) 0.0217(10) Uani 1 1 d . . . H25 H 0.3634 0.0708 0.6306 0.026 Uiso 1 1 calc R . . C26 C 0.5024(4) 0.0783(4) 0.4117(3) 0.0179(9) Uani 1 1 d . . . H26 H 0.5069 0.1319 0.3474 0.021 Uiso 1 1 calc R . . C27 C 0.1081(4) 0.1095(4) 0.5115(3) 0.0215(10) Uani 1 1 d . . . H27A H 0.0820 0.1320 0.5767 0.032 Uiso 1 1 calc R . . H27B H 0.1800 0.0338 0.5159 0.032 Uiso 1 1 calc R . . H27C H 0.0368 0.0947 0.4916 0.032 Uiso 1 1 calc R . . C28 C 0.4517(4) 0.4696(4) 0.3921(4) 0.0262(11) Uani 1 1 d . . . H28A H 0.4660 0.4624 0.3224 0.039 Uiso 1 1 calc R . . H28B H 0.5140 0.4014 0.4292 0.039 Uiso 1 1 calc R . . H28C H 0.4610 0.5493 0.3947 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.41977(12) 1.05840(11) 0.18018(10) 0.0307(3) Uani 1 1 d . . . Cl2 Cl -0.25229(13) 0.07006(12) 0.17799(11) 0.0369(3) Uani 1 1 d . . . N1 N 0.4212(3) 0.1221(3) 0.4865(3) 0.0168(7) Uani 1 1 d . . . O1 O 0.1082(2) 0.4423(2) 0.4282(2) 0.0122(6) Uani 1 1 d . . . O2 O 0.1453(3) 0.2084(2) 0.4391(2) 0.0171(6) Uani 1 1 d . . . O3 O 0.3253(3) 0.4633(3) 0.4360(2) 0.0170(6) Uani 1 1 d . . . O4 O 0.2293(3) 0.2765(3) 0.6123(2) 0.0166(6) Uani 1 1 d . . . O5 O -0.1089(3) 0.3504(3) 0.5008(2) 0.0164(6) Uani 1 1 d . . . O6 O 0.1302(3) 0.3722(3) 0.2493(2) 0.0170(6) Uani 1 1 d . . . O7 O 0.2354(3) 0.5337(2) 0.2448(2) 0.0156(6) Uani 1 1 d . . . O8 O 0.0058(3) 0.6865(2) 0.3232(2) 0.0168(6) Uani 1 1 d . . . O9 O -0.1034(3) 0.5279(3) 0.3236(2) 0.0186(6) Uani 1 1 d . . . O10 O 0.3456(3) 0.3069(3) 0.3079(2) 0.0176(6) Uani 1 1 d . . . 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 Sb1 0.01422(14) 0.01045(14) 0.01197(15) -0.00283(11) 0.00040(11) -0.00133(10) Sb2 0.01443(14) 0.01100(14) 0.01200(15) -0.00326(11) -0.00061(11) -0.00131(10) Co1 0.0144(3) 0.0108(3) 0.0127(3) -0.0028(2) -0.0008(2) 0.0005(2) P1 0.0161(5) 0.0090(5) 0.0135(6) -0.0009(4) -0.0038(4) 0.0003(4) P2 0.0175(5) 0.0115(5) 0.0116(5) -0.0027(4) 0.0012(4) -0.0007(4) C1 0.015(2) 0.018(2) 0.017(2) -0.0049(18) -0.0008(17) -0.0062(16) C2 0.047(3) 0.031(3) 0.010(2) -0.005(2) 0.005(2) -0.018(2) C3 0.035(3) 0.038(3) 0.029(3) -0.017(2) 0.005(2) -0.017(2) C4 0.020(2) 0.017(2) 0.029(3) -0.004(2) 0.0006(19) -0.0089(18) C5 0.038(3) 0.026(2) 0.015(2) -0.001(2) 0.005(2) -0.014(2) C6 0.037(3) 0.024(2) 0.020(3) -0.011(2) 0.002(2) -0.013(2) C7 0.021(2) 0.012(2) 0.011(2) -0.0019(17) 0.0007(17) -0.0032(16) C8 0.016(2) 0.029(2) 0.021(2) -0.012(2) 0.0018(18) -0.0052(18) C9 0.036(3) 0.017(2) 0.029(3) -0.012(2) 0.002(2) -0.008(2) C10 0.033(3) 0.025(2) 0.018(2) -0.008(2) -0.001(2) -0.011(2) C11 0.028(3) 0.025(2) 0.034(3) -0.006(2) -0.005(2) -0.010(2) C12 0.025(2) 0.018(2) 0.029(3) -0.007(2) -0.004(2) -0.0050(18) C13 0.028(2) 0.013(2) 0.015(2) -0.0030(18) -0.0004(19) -0.0047(18) C14 0.029(3) 0.028(3) 0.023(3) -0.009(2) 0.005(2) -0.011(2) C15 0.043(3) 0.040(3) 0.025(3) -0.018(3) 0.017(2) -0.017(3) C16 0.065(4) 0.034(3) 0.024(3) -0.011(2) 0.016(3) -0.025(3) C17 0.062(4) 0.033(3) 0.021(3) -0.003(2) -0.014(3) -0.008(3) C18 0.039(3) 0.025(3) 0.019(3) -0.005(2) 0.000(2) -0.004(2) C19 0.029(3) 0.050(3) 0.027(3) -0.005(3) -0.003(2) 0.001(2) C20 0.030(3) 0.071(4) 0.020(3) 0.000(3) 0.005(2) -0.007(3) C21 0.046(3) 0.048(3) 0.019(3) 0.001(3) -0.011(2) -0.006(3) C22 0.029(3) 0.036(3) 0.025(3) -0.008(2) -0.010(2) -0.001(2) C23 0.025(2) 0.021(2) 0.019(2) -0.0025(19) -0.0046(19) -0.0042(18) C24 0.020(2) 0.015(2) 0.015(2) -0.0018(18) -0.0044(18) -0.0002(17) C25 0.022(2) 0.018(2) 0.018(2) -0.0047(19) -0.0016(18) 0.0032(18) C26 0.022(2) 0.015(2) 0.010(2) 0.0010(17) -0.0004(17) -0.0005(17) C27 0.020(2) 0.015(2) 0.023(3) 0.0001(19) -0.0004(19) -0.0004(17) C28 0.018(2) 0.026(2) 0.029(3) -0.003(2) 0.000(2) -0.0034(19) Cl1 0.0372(7) 0.0274(6) 0.0322(7) -0.0046(5) -0.0016(5) -0.0190(5) Cl2 0.0415(7) 0.0387(7) 0.0431(8) -0.0180(6) -0.0072(6) -0.0197(6) N1 0.0153(17) 0.0153(17) 0.0165(19) -0.0056(15) -0.0026(15) 0.0020(14) O1 0.0155(14) 0.0067(13) 0.0127(15) -0.0004(11) -0.0028(11) -0.0020(10) O2 0.0184(15) 0.0119(14) 0.0160(16) -0.0001(12) 0.0001(12) -0.0018(11) O3 0.0117(14) 0.0185(15) 0.0181(16) -0.0051(13) 0.0005(12) -0.0015(11) O4 0.0181(15) 0.0157(14) 0.0103(15) -0.0027(12) -0.0020(12) 0.0025(11) O5 0.0142(14) 0.0214(15) 0.0116(15) -0.0084(13) 0.0043(11) -0.0024(12) O6 0.0225(16) 0.0161(15) 0.0101(15) -0.0042(12) 0.0037(12) -0.0053(12) O7 0.0219(15) 0.0100(14) 0.0114(15) -0.0010(12) 0.0022(12) -0.0037(11) O8 0.0184(15) 0.0107(14) 0.0185(16) -0.0020(12) -0.0041(12) -0.0004(11) O9 0.0207(15) 0.0125(14) 0.0210(17) -0.0039(13) -0.0056(13) -0.0007(12) O10 0.0166(15) 0.0127(14) 0.0170(16) -0.0023(13) -0.0010(12) 0.0028(11) _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 Sb1 O5 1.922(3) 2_566 ? Sb1 O1 1.972(3) . ? Sb1 O8 2.012(3) . ? Sb1 O3 2.034(3) . ? Sb1 O7 2.056(3) . ? Sb1 C1 2.115(4) . ? Sb2 O5 1.912(3) . ? Sb2 O1 1.975(3) . ? Sb2 O9 2.003(3) . ? Sb2 O2 2.029(3) . ? Sb2 O6 2.047(3) . ? Sb2 C7 2.109(4) . ? Co1 O4 2.039(3) . ? Co1 O10 2.117(3) . ? Co1 O1 2.128(3) . ? Co1 O3 2.132(3) . ? Co1 N1 2.135(3) . ? Co1 O2 2.142(3) . ? P1 O4 1.503(3) 2_566 ? P1 O9 1.537(3) . ? P1 O8 1.540(3) . ? P1 C24 1.782(4) . ? P2 O10 1.494(3) . ? P2 O6 1.540(3) . ? P2 O7 1.555(3) . ? P2 C13 1.782(4) . ? C1 C6 1.377(6) . ? C1 C2 1.396(6) . ? C2 C3 1.376(7) . ? C2 H2 0.9500 . ? C3 C4 1.368(7) . ? C3 H3 0.9500 . ? C4 C5 1.375(6) . ? C4 Cl1 1.736(4) . ? C5 C6 1.377(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.388(6) . ? C7 C8 1.392(6) . ? C8 C9 1.389(6) . ? C8 H8 0.9500 . ? C9 C10 1.375(7) . ? C9 H9 0.9500 . ? C10 C11 1.387(6) . ? C10 Cl2 1.740(5) . ? C11 C12 1.378(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.390(6) . ? C13 C14 1.390(6) . ? C14 C15 1.379(7) . ? C14 H14 0.9500 . ? C15 C16 1.377(8) . ? C15 H15 0.9500 . ? C16 C17 1.372(8) . ? C16 H16 0.9500 . ? C17 C18 1.394(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.382(7) . ? C19 C24 1.387(7) . ? C19 H19 0.9500 . ? C20 C21 1.373(7) . ? C20 H20 0.9500 . ? C21 C22 1.364(7) . ? C21 H21 0.9500 . ? C22 C23 1.385(7) . ? C22 H22 0.9500 . ? C23 C24 1.390(6) . ? C23 H23 0.9500 . ? C25 N1 1.332(6) . ? C25 C26 1.387(6) 2_656 ? C25 H25 0.9500 . ? C26 N1 1.332(5) . ? C26 C25 1.387(6) 2_656 ? C26 H26 0.9500 . ? C27 O2 1.426(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 O3 1.437(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O4 P1 1.503(3) 2_566 ? O5 Sb1 1.922(3) 2_566 ? 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 O5 Sb1 O1 94.38(12) 2_566 . ? O5 Sb1 O8 91.57(12) 2_566 . ? O1 Sb1 O8 89.72(11) . . ? O5 Sb1 O3 91.83(12) 2_566 . ? O1 Sb1 O3 79.21(11) . . ? O8 Sb1 O3 168.64(11) . . ? O5 Sb1 O7 177.91(11) 2_566 . ? O1 Sb1 O7 87.35(11) . . ? O8 Sb1 O7 87.25(12) . . ? O3 Sb1 O7 89.66(11) . . ? O5 Sb1 C1 90.74(14) 2_566 . ? O1 Sb1 C1 174.56(14) . . ? O8 Sb1 C1 91.99(14) . . ? O3 Sb1 C1 98.81(14) . . ? O7 Sb1 C1 87.58(14) . . ? O5 Sb2 O1 94.75(12) . . ? O5 Sb2 O9 90.20(12) . . ? O1 Sb2 O9 90.14(12) . . ? O5 Sb2 O2 93.68(12) . . ? O1 Sb2 O2 80.47(11) . . ? O9 Sb2 O2 170.10(11) . . ? O5 Sb2 O6 177.31(12) . . ? O1 Sb2 O6 87.69(12) . . ? O9 Sb2 O6 88.63(12) . . ? O2 Sb2 O6 87.86(12) . . ? O5 Sb2 C7 91.76(14) . . ? O1 Sb2 C7 172.80(14) . . ? O9 Sb2 C7 92.92(14) . . ? O2 Sb2 C7 96.06(14) . . ? O6 Sb2 C7 85.88(14) . . ? O4 Co1 O10 173.50(11) . . ? O4 Co1 O1 94.25(11) . . ? O10 Co1 O1 91.37(11) . . ? O4 Co1 O3 95.28(11) . . ? O10 Co1 O3 83.17(11) . . ? O1 Co1 O3 73.68(11) . . ? O4 Co1 N1 89.13(12) . . ? O10 Co1 N1 86.11(12) . . ? O1 Co1 N1 166.81(12) . . ? O3 Co1 N1 118.75(13) . . ? O4 Co1 O2 97.97(12) . . ? O10 Co1 O2 86.66(11) . . ? O1 Co1 O2 74.58(11) . . ? O3 Co1 O2 146.33(11) . . ? N1 Co1 O2 92.33(12) . . ? O4 P1 O9 113.65(17) 2_566 . ? O4 P1 O8 112.69(17) 2_566 . ? O9 P1 O8 110.54(16) . . ? O4 P1 C24 110.56(18) 2_566 . ? O9 P1 C24 103.80(18) . . ? O8 P1 C24 104.88(18) . . ? O10 P2 O6 112.99(17) . . ? O10 P2 O7 111.55(17) . . ? O6 P2 O7 108.37(16) . . ? O10 P2 C13 112.67(19) . . ? O6 P2 C13 105.76(19) . . ? O7 P2 C13 105.01(18) . . ? C6 C1 C2 118.2(4) . . ? C6 C1 Sb1 121.6(3) . . ? C2 C1 Sb1 120.1(3) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 119.4(5) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 121.3(4) . . ? C3 C4 Cl1 119.2(4) . . ? C5 C4 Cl1 119.5(4) . . ? C4 C5 C6 118.8(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C5 C6 C1 121.5(4) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? C12 C7 C8 119.7(4) . . ? C12 C7 Sb2 120.0(3) . . ? C8 C7 Sb2 120.2(3) . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 118.5(4) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C11 121.4(4) . . ? C9 C10 Cl2 119.4(4) . . ? C11 C10 Cl2 119.2(4) . . ? C12 C11 C10 119.8(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C7 119.8(4) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C18 C13 C14 119.3(4) . . ? C18 C13 P2 120.6(3) . . ? C14 C13 P2 120.0(4) . . ? C15 C14 C13 120.1(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.5(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 120.0(5) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.2(5) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 119.8(5) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C24 120.6(5) . . ? C20 C19 H19 119.7 . . ? C24 C19 H19 119.7 . . ? C21 C20 C19 120.1(5) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.2(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.3(5) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 120.3(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 118.5(4) . . ? C19 C24 P1 118.5(4) . . ? C23 C24 P1 122.7(3) . . ? N1 C25 C26 121.6(4) . 2_656 ? N1 C25 H25 119.2 . . ? C26 C25 H25 119.2 2_656 . ? N1 C26 C25 121.9(4) . 2_656 ? N1 C26 H26 119.1 . . ? C25 C26 H26 119.1 2_656 . ? O2 C27 H27A 109.5 . . ? O2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O3 C28 H28A 109.5 . . ? O3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 N1 C26 116.5(4) . . ? C25 N1 Co1 120.4(3) . . ? C26 N1 Co1 122.0(3) . . ? Sb1 O1 Sb2 136.92(15) . . ? Sb1 O1 Co1 103.50(12) . . ? Sb2 O1 Co1 102.44(12) . . ? C27 O2 Sb2 119.5(2) . . ? C27 O2 Co1 123.2(3) . . ? Sb2 O2 Co1 100.20(12) . . ? C28 O3 Sb1 120.5(3) . . ? C28 O3 Co1 120.6(2) . . ? Sb1 O3 Co1 101.24(12) . . ? P1 O4 Co1 137.59(17) 2_566 . ? Sb2 O5 Sb1 143.72(17) . 2_566 ? P2 O6 Sb2 124.00(17) . . ? P2 O7 Sb1 123.07(16) . . ? P1 O8 Sb1 139.38(17) . . ? P1 O9 Sb2 139.18(18) . . ? P2 O10 Co1 116.59(16) . . ? 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 O5 Sb1 C1 C6 -157.4(4) 2_566 . . . ? O1 Sb1 C1 C6 42.3(16) . . . . ? O8 Sb1 C1 C6 -65.8(4) . . . . ? O3 Sb1 C1 C6 110.6(4) . . . . ? O7 Sb1 C1 C6 21.3(4) . . . . ? O5 Sb1 C1 C2 19.9(4) 2_566 . . . ? O1 Sb1 C1 C2 -140.3(13) . . . . ? O8 Sb1 C1 C2 111.5(4) . . . . ? O3 Sb1 C1 C2 -72.0(4) . . . . ? O7 Sb1 C1 C2 -161.3(4) . . . . ? C6 C1 C2 C3 -2.7(7) . . . . ? Sb1 C1 C2 C3 179.8(4) . . . . ? C1 C2 C3 C4 -0.1(8) . . . . ? C2 C3 C4 C5 2.2(7) . . . . ? C2 C3 C4 Cl1 -179.4(4) . . . . ? C3 C4 C5 C6 -1.3(7) . . . . ? Cl1 C4 C5 C6 -179.7(4) . . . . ? C4 C5 C6 C1 -1.6(7) . . . . ? C2 C1 C6 C5 3.6(7) . . . . ? Sb1 C1 C6 C5 -179.0(4) . . . . ? O5 Sb2 C7 C12 52.1(4) . . . . ? O1 Sb2 C7 C12 -153.2(9) . . . . ? O9 Sb2 C7 C12 -38.2(4) . . . . ? O2 Sb2 C7 C12 146.0(3) . . . . ? O6 Sb2 C7 C12 -126.6(4) . . . . ? O5 Sb2 C7 C8 -127.5(4) . . . . ? O1 Sb2 C7 C8 27.2(13) . . . . ? O9 Sb2 C7 C8 142.2(3) . . . . ? O2 Sb2 C7 C8 -33.6(4) . . . . ? O6 Sb2 C7 C8 53.8(3) . . . . ? C12 C7 C8 C9 0.8(7) . . . . ? Sb2 C7 C8 C9 -179.6(4) . . . . ? C7 C8 C9 C10 1.7(7) . . . . ? C8 C9 C10 C11 -2.7(7) . . . . ? C8 C9 C10 Cl2 177.8(4) . . . . ? C9 C10 C11 C12 1.3(7) . . . . ? Cl2 C10 C11 C12 -179.2(4) . . . . ? C10 C11 C12 C7 1.2(7) . . . . ? C8 C7 C12 C11 -2.2(7) . . . . ? Sb2 C7 C12 C11 178.2(4) . . . . ? O10 P2 C13 C18 164.0(4) . . . . ? O6 P2 C13 C18 40.1(4) . . . . ? O7 P2 C13 C18 -74.4(4) . . . . ? O10 P2 C13 C14 -19.3(4) . . . . ? O6 P2 C13 C14 -143.2(3) . . . . ? O7 P2 C13 C14 102.3(4) . . . . ? C18 C13 C14 C15 0.0(7) . . . . ? P2 C13 C14 C15 -176.8(4) . . . . ? C13 C14 C15 C16 0.4(7) . . . . ? C14 C15 C16 C17 -0.6(8) . . . . ? C15 C16 C17 C18 0.5(8) . . . . ? C14 C13 C18 C17 -0.2(7) . . . . ? P2 C13 C18 C17 176.6(4) . . . . ? C16 C17 C18 C13 -0.1(8) . . . . ? C24 C19 C20 C21 0.0(10) . . . . ? C19 C20 C21 C22 -0.2(10) . . . . ? C20 C21 C22 C23 -0.5(9) . . . . ? C21 C22 C23 C24 1.4(8) . . . . ? C20 C19 C24 C23 0.8(8) . . . . ? C20 C19 C24 P1 174.3(5) . . . . ? C22 C23 C24 C19 -1.5(7) . . . . ? C22 C23 C24 P1 -174.7(4) . . . . ? O4 P1 C24 C19 160.3(4) 2_566 . . . ? O9 P1 C24 C19 -77.4(4) . . . . ? O8 P1 C24 C19 38.6(4) . . . . ? O4 P1 C24 C23 -26.4(4) 2_566 . . . ? O9 P1 C24 C23 95.8(4) . . . . ? O8 P1 C24 C23 -148.2(4) . . . . ? C26 C25 N1 C26 -0.5(7) 2_656 . . . ? C26 C25 N1 Co1 167.7(3) 2_656 . . . ? C25 C26 N1 C25 0.5(7) 2_656 . . . ? C25 C26 N1 Co1 -167.5(3) 2_656 . . . ? O4 Co1 N1 C25 17.7(3) . . . . ? O10 Co1 N1 C25 -166.7(3) . . . . ? O1 Co1 N1 C25 -87.3(6) . . . . ? O3 Co1 N1 C25 113.3(3) . . . . ? O2 Co1 N1 C25 -80.2(3) . . . . ? O4 Co1 N1 C26 -174.8(3) . . . . ? O10 Co1 N1 C26 0.8(3) . . . . ? O1 Co1 N1 C26 80.1(7) . . . . ? O3 Co1 N1 C26 -79.3(3) . . . . ? O2 Co1 N1 C26 87.2(3) . . . . ? O5 Sb1 O1 Sb2 131.4(2) 2_566 . . . ? O8 Sb1 O1 Sb2 39.8(2) . . . . ? O3 Sb1 O1 Sb2 -137.6(2) . . . . ? O7 Sb1 O1 Sb2 -47.4(2) . . . . ? C1 Sb1 O1 Sb2 -68.5(15) . . . . ? O5 Sb1 O1 Co1 -103.10(13) 2_566 . . . ? O8 Sb1 O1 Co1 165.35(13) . . . . ? O3 Sb1 O1 Co1 -12.07(12) . . . . ? O7 Sb1 O1 Co1 78.09(12) . . . . ? C1 Sb1 O1 Co1 57.1(15) . . . . ? O5 Sb2 O1 Sb1 -129.3(2) . . . . ? O9 Sb2 O1 Sb1 -39.1(2) . . . . ? O2 Sb2 O1 Sb1 137.8(2) . . . . ? O6 Sb2 O1 Sb1 49.6(2) . . . . ? C7 Sb2 O1 Sb1 76.1(11) . . . . ? O5 Sb2 O1 Co1 104.87(13) . . . . ? O9 Sb2 O1 Co1 -164.92(13) . . . . ? O2 Sb2 O1 Co1 11.92(12) . . . . ? O6 Sb2 O1 Co1 -76.30(12) . . . . ? C7 Sb2 O1 Co1 -49.8(11) . . . . ? O4 Co1 O1 Sb1 106.05(13) . . . . ? O10 Co1 O1 Sb1 -70.69(13) . . . . ? O3 Co1 O1 Sb1 11.78(11) . . . . ? N1 Co1 O1 Sb1 -149.4(5) . . . . ? O2 Co1 O1 Sb1 -156.85(14) . . . . ? O4 Co1 O1 Sb2 -108.66(13) . . . . ? O10 Co1 O1 Sb2 74.61(13) . . . . ? O3 Co1 O1 Sb2 157.08(14) . . . . ? N1 Co1 O1 Sb2 -4.1(6) . . . . ? O2 Co1 O1 Sb2 -11.55(11) . . . . ? O5 Sb2 O2 C27 31.8(3) . . . . ? O1 Sb2 O2 C27 126.0(3) . . . . ? O9 Sb2 O2 C27 144.7(6) . . . . ? O6 Sb2 O2 C27 -146.0(3) . . . . ? C7 Sb2 O2 C27 -60.3(3) . . . . ? O5 Sb2 O2 Co1 -105.96(13) . . . . ? O1 Sb2 O2 Co1 -11.75(11) . . . . ? O9 Sb2 O2 Co1 6.9(7) . . . . ? O6 Sb2 O2 Co1 76.26(12) . . . . ? C7 Sb2 O2 Co1 161.88(14) . . . . ? O4 Co1 O2 C27 -32.3(3) . . . . ? O10 Co1 O2 C27 143.2(3) . . . . ? O1 Co1 O2 C27 -124.5(3) . . . . ? O3 Co1 O2 C27 -144.5(3) . . . . ? N1 Co1 O2 C27 57.2(3) . . . . ? O4 Co1 O2 Sb2 103.39(12) . . . . ? O10 Co1 O2 Sb2 -81.19(12) . . . . ? O1 Co1 O2 Sb2 11.15(11) . . . . ? O3 Co1 O2 Sb2 -8.8(3) . . . . ? N1 Co1 O2 Sb2 -167.16(13) . . . . ? O5 Sb1 O3 C28 -117.9(3) 2_566 . . . ? O1 Sb1 O3 C28 148.0(3) . . . . ? O8 Sb1 O3 C28 134.7(6) . . . . ? O7 Sb1 O3 C28 60.6(3) . . . . ? C1 Sb1 O3 C28 -26.9(3) . . . . ? O5 Sb1 O3 Co1 106.05(13) 2_566 . . . ? O1 Sb1 O3 Co1 11.94(11) . . . . ? O8 Sb1 O3 Co1 -1.3(6) . . . . ? O7 Sb1 O3 Co1 -75.43(12) . . . . ? C1 Sb1 O3 Co1 -162.92(14) . . . . ? O4 Co1 O3 C28 119.8(3) . . . . ? O10 Co1 O3 C28 -53.8(3) . . . . ? O1 Co1 O3 C28 -147.3(3) . . . . ? N1 Co1 O3 C28 27.9(3) . . . . ? O2 Co1 O3 C28 -127.2(3) . . . . ? O4 Co1 O3 Sb1 -104.21(12) . . . . ? O10 Co1 O3 Sb1 82.13(12) . . . . ? O1 Co1 O3 Sb1 -11.31(11) . . . . ? N1 Co1 O3 Sb1 163.88(12) . . . . ? O2 Co1 O3 Sb1 8.7(3) . . . . ? O10 Co1 O4 P1 152.1(8) . . . 2_566 ? O1 Co1 O4 P1 2.3(3) . . . 2_566 ? O3 Co1 O4 P1 76.3(3) . . . 2_566 ? N1 Co1 O4 P1 -164.9(3) . . . 2_566 ? O2 Co1 O4 P1 -72.7(3) . . . 2_566 ? O1 Sb2 O5 Sb1 13.8(3) . . . 2_566 ? O9 Sb2 O5 Sb1 -76.3(3) . . . 2_566 ? O2 Sb2 O5 Sb1 94.5(3) . . . 2_566 ? O6 Sb2 O5 Sb1 -141(2) . . . 2_566 ? C7 Sb2 O5 Sb1 -169.3(3) . . . 2_566 ? O10 P2 O6 Sb2 55.6(2) . . . . ? O7 P2 O6 Sb2 -68.6(2) . . . . ? C13 P2 O6 Sb2 179.25(19) . . . . ? O5 Sb2 O6 P2 171(2) . . . . ? O1 Sb2 O6 P2 16.2(2) . . . . ? O9 Sb2 O6 P2 106.4(2) . . . . ? O2 Sb2 O6 P2 -64.4(2) . . . . ? C7 Sb2 O6 P2 -160.6(2) . . . . ? O10 P2 O7 Sb1 -53.2(2) . . . . ? O6 P2 O7 Sb1 71.8(2) . . . . ? C13 P2 O7 Sb1 -175.5(2) . . . . ? O5 Sb1 O7 P2 -166(3) 2_566 . . . ? O1 Sb1 O7 P2 -20.55(19) . . . . ? O8 Sb1 O7 P2 -110.4(2) . . . . ? O3 Sb1 O7 P2 58.7(2) . . . . ? C1 Sb1 O7 P2 157.5(2) . . . . ? O4 P1 O8 Sb1 104.9(3) 2_566 . . . ? O9 P1 O8 Sb1 -23.5(3) . . . . ? C24 P1 O8 Sb1 -134.8(3) . . . . ? O5 Sb1 O8 P1 -95.6(3) 2_566 . . . ? O1 Sb1 O8 P1 -1.2(3) . . . . ? O3 Sb1 O8 P1 11.8(8) . . . . ? O7 Sb1 O8 P1 86.1(3) . . . . ? C1 Sb1 O8 P1 173.6(3) . . . . ? O4 P1 O9 Sb2 -102.5(3) 2_566 . . . ? O8 P1 O9 Sb2 25.4(3) . . . . ? C24 P1 O9 Sb2 137.4(3) . . . . ? O5 Sb2 O9 P1 93.2(3) . . . . ? O1 Sb2 O9 P1 -1.5(3) . . . . ? O2 Sb2 O9 P1 -20.0(9) . . . . ? O6 Sb2 O9 P1 -89.2(3) . . . . ? C7 Sb2 O9 P1 -175.0(3) . . . . ? O6 P2 O10 Co1 -58.1(2) . . . . ? O7 P2 O10 Co1 64.3(2) . . . . ? C13 P2 O10 Co1 -177.87(18) . . . . ? O4 Co1 O10 P2 -153.9(9) . . . . ? O1 Co1 O10 P2 -4.02(19) . . . . ? O3 Co1 O10 P2 -77.40(18) . . . . ? N1 Co1 O10 P2 163.0(2) . . . . ? O2 Co1 O10 P2 70.45(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.802 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.139 # Attachment '- 12.cif' data_tri1068 _database_code_depnum_ccdc_archive 'CCDC 778681' #TrackingRef '- 12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H54 Cl4 Co2 N2 O20 P4 Sb4' _chemical_formula_weight 2041.63 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 12.6584(4) _cell_length_b 13.8300(4) _cell_length_c 24.5262(6) _cell_angle_alpha 78.288(2) _cell_angle_beta 87.421(2) _cell_angle_gamma 69.051(3) _cell_volume 3924.61(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10428 _cell_measurement_theta_min 2.7124 _cell_measurement_theta_max 28.4601 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1996 _exptl_absorpt_coefficient_mu 2.054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4938 _exptl_absorpt_correction_T_max 0.8209 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25361 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 26.37 _reflns_number_total 15034 _reflns_number_gt 9997 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The disorder in one phenyl ring was modelled. A very large solvent viods found in the structure could not be modelled due to a large disorder. Ratio of maximum to minimum residual density is also associated with disordered solvent. 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^)+(0.0779P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15034 _refine_ls_number_parameters 989 _refine_ls_number_restraints 367 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.042 _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 Sb1 Sb 0.43711(4) -0.07556(3) 0.424166(18) 0.01793(12) Uani 1 1 d . C . Sb2 Sb 0.28799(4) 0.10968(3) 0.515381(19) 0.01864(12) Uani 1 1 d . . . Sb3 Sb 0.98748(4) 0.11623(3) 0.073122(18) 0.01748(12) Uani 1 1 d . . . Sb4 Sb 1.16809(4) -0.15067(3) 0.056835(18) 0.01717(12) Uani 1 1 d . . . Co1 Co 0.59246(9) 0.05902(7) 0.37468(4) 0.0217(2) Uani 1 1 d . . . Co2 Co 1.04194(8) 0.22699(7) -0.04691(4) 0.0195(2) Uani 1 1 d . . . P1 P 0.45522(16) 0.23339(13) 0.45513(8) 0.0198(4) Uani 1 1 d . . . P2 P 0.67710(16) -0.17646(13) 0.37129(7) 0.0197(4) Uani 1 1 d . . . P3 P 0.81596(16) 0.33617(13) 0.00539(7) 0.0195(4) Uani 1 1 d . . . P4 P 0.78653(16) 0.01707(13) 0.06513(7) 0.0183(4) Uani 1 1 d . . . N2 N 1.1285(5) 0.3263(4) -0.0849(3) 0.0262(14) Uani 1 1 d . . . C1 C 0.3167(6) -0.1214(5) 0.3892(3) 0.0217(16) Uani 1 1 d . . . C2 C 0.3172(7) -0.1242(6) 0.3334(3) 0.0294(18) Uani 1 1 d . . . H2 H 0.3724 -0.1059 0.3104 0.035 Uiso 1 1 calc R . . C3 C 0.2380(7) -0.1537(6) 0.3105(3) 0.0340(19) Uani 1 1 d . . . H3 H 0.2410 -0.1589 0.2724 0.041 Uiso 1 1 calc R . . C4 C 0.1546(7) -0.1754(6) 0.3436(3) 0.0325(19) Uani 1 1 d . . . C5 C 0.1518(7) -0.1719(7) 0.3987(3) 0.036(2) Uani 1 1 d . . . H5 H 0.0945 -0.1876 0.4211 0.044 Uiso 1 1 calc R . . C6 C 0.2334(6) -0.1450(6) 0.4223(3) 0.0266(17) Uani 1 1 d . . . H6 H 0.2320 -0.1428 0.4608 0.032 Uiso 1 1 calc R . . C7 C 0.1197(7) 0.1898(6) 0.4876(3) 0.0285(18) Uani 1 1 d . . . C8 C 0.0583(8) 0.1369(7) 0.4664(4) 0.045(2) Uani 1 1 d . C . H8 H 0.0966 0.0664 0.4616 0.054 Uiso 1 1 calc R . . C9 C -0.0572(8) 0.1856(7) 0.4525(4) 0.044(2) Uani 1 1 d . . . H9 H -0.0976 0.1479 0.4397 0.053 Uiso 1 1 calc R C . C10 C -0.1112(7) 0.2884(7) 0.4574(4) 0.039(2) Uani 1 1 d . C . C11 C -0.0553(8) 0.3436(7) 0.4765(4) 0.048(2) Uani 1 1 d . . . H11 H -0.0939 0.4152 0.4792 0.057 Uiso 1 1 calc R A 1 C13 C 0.4390(11) 0.3726(6) 0.4392(4) 0.028(4) Uani 0.503(9) 1 d PGU B 1 C14 C 0.4551(11) 0.4277(8) 0.4777(4) 0.041(4) Uani 0.503(9) 1 d PGU B 1 H14 H 0.4729 0.3934 0.5155 0.049 Uiso 0.503(9) 1 calc PR B 1 C15 C 0.4452(12) 0.5328(8) 0.4607(4) 0.046(4) Uani 0.503(9) 1 d PGU B 1 H15 H 0.4562 0.5705 0.4870 0.055 Uiso 0.503(9) 1 calc PR B 1 C16 C 0.4192(12) 0.5829(6) 0.4053(5) 0.046(4) Uani 0.503(9) 1 d PGU B 1 H16 H 0.4124 0.6548 0.3937 0.055 Uiso 0.503(9) 1 calc PR B 1 C17 C 0.4031(12) 0.5279(8) 0.3668(4) 0.045(4) Uani 0.503(9) 1 d PGU B 1 H17 H 0.3854 0.5621 0.3289 0.055 Uiso 0.503(9) 1 calc PR B 1 C18 C 0.4130(12) 0.4228(8) 0.3837(4) 0.041(3) Uani 0.503(9) 1 d PGU B 1 H18 H 0.4020 0.3851 0.3574 0.049 Uiso 0.503(9) 1 calc PR B 1 C12 C 0.0583(8) 0.2940(7) 0.4920(4) 0.046(2) Uani 1 1 d . C 1 H12 H 0.0959 0.3325 0.5062 0.056 Uiso 1 1 calc R C 1 C13A C 0.4175(10) 0.3727(6) 0.4324(5) 0.024(3) Uani 0.497(9) 1 d PGU B 2 C14A C 0.3241(10) 0.4440(8) 0.4527(5) 0.042(4) Uani 0.497(9) 1 d PGU B 2 H14A H 0.2755 0.4189 0.4776 0.050 Uiso 0.497(9) 1 calc PR B 2 C15A C 0.3016(10) 0.5519(7) 0.4366(6) 0.059(5) Uani 0.497(9) 1 d PGU B 2 H15A H 0.2378 0.6006 0.4505 0.071 Uiso 0.497(9) 1 calc PR B 2 C16A C 0.3726(11) 0.5886(6) 0.4002(6) 0.048(4) Uani 0.497(9) 1 d PGU B 2 H16A H 0.3573 0.6623 0.3892 0.057 Uiso 0.497(9) 1 calc PR B 2 C17A C 0.4661(10) 0.5173(8) 0.3799(5) 0.038(3) Uani 0.497(9) 1 d PGU B 2 H17A H 0.5146 0.5424 0.3550 0.045 Uiso 0.497(9) 1 calc PR B 2 C18A C 0.4885(9) 0.4094(7) 0.3960(5) 0.029(3) Uani 0.497(9) 1 d PGU B 2 H18A H 0.5524 0.3607 0.3821 0.035 Uiso 0.497(9) 1 calc PR B 2 C19 C 0.7506(6) -0.2822(5) 0.3370(3) 0.0226(16) Uani 1 1 d . D . C20 C 0.8091(7) -0.2643(6) 0.2887(3) 0.0344(19) Uani 1 1 d . . . H20 H 0.8075 -0.1949 0.2735 0.041 Uiso 1 1 calc R D . C21 C 0.8698(7) -0.3472(7) 0.2627(4) 0.039(2) Uani 1 1 d . D . H21 H 0.9092 -0.3340 0.2297 0.047 Uiso 1 1 calc R . . C22 C 0.8730(8) -0.4472(7) 0.2842(4) 0.042(2) Uani 1 1 d . . . H22 H 0.9146 -0.5036 0.2663 0.051 Uiso 1 1 calc R D . C23 C 0.8153(8) -0.4666(6) 0.3324(4) 0.041(2) Uani 1 1 d . D . H23 H 0.8184 -0.5366 0.3475 0.049 Uiso 1 1 calc R . . C24 C 0.7543(7) -0.3860(6) 0.3581(3) 0.0271(17) Uani 1 1 d . . . H24 H 0.7141 -0.4000 0.3906 0.033 Uiso 1 1 calc R D . C25 C 0.1500(7) 0.0191(7) 0.6008(4) 0.039(2) Uani 1 1 d . C . H25A H 0.1319 0.0833 0.6159 0.059 Uiso 1 1 calc R . . H25B H 0.1536 -0.0405 0.6311 0.059 Uiso 1 1 calc R . . H25C H 0.0911 0.0292 0.5733 0.059 Uiso 1 1 calc R . . C26 C 0.3387(7) 0.1218(6) 0.3353(3) 0.0312(18) Uani 1 1 d . . . H26A H 0.2840 0.0935 0.3242 0.047 Uiso 1 1 calc R D . H26B H 0.3566 0.1670 0.3028 0.047 Uiso 1 1 calc R . . H26C H 0.3060 0.1635 0.3638 0.047 Uiso 1 1 calc R . . C27 C 1.0081(6) 0.1318(5) 0.1555(3) 0.0243(16) Uani 1 1 d . E . C28 C 0.9903(9) 0.0623(7) 0.2011(4) 0.052(3) Uani 1 1 d . . . H28 H 0.9725 0.0038 0.1955 0.062 Uiso 1 1 calc R . . C29 C 0.9981(10) 0.0773(9) 0.2550(4) 0.065(3) Uani 1 1 d . E . H29 H 0.9851 0.0302 0.2863 0.078 Uiso 1 1 calc R . . C30 C 1.0250(8) 0.1616(10) 0.2617(4) 0.061(3) Uani 1 1 d D . . C31 C 1.0482(8) 0.2292(9) 0.2185(5) 0.060(3) Uani 1 1 d . E . H31 H 1.0688 0.2857 0.2249 0.072 Uiso 1 1 calc R . . C32 C 1.0409(8) 0.2137(7) 0.1648(4) 0.044(2) Uani 1 1 d . . . H32 H 1.0584 0.2591 0.1341 0.053 Uiso 1 1 calc R E . C33 C 1.3023(6) -0.2053(5) 0.1170(3) 0.0168(14) Uani 1 1 d . . . C34 C 1.3507(7) -0.1397(6) 0.1307(4) 0.036(2) Uani 1 1 d . . . H34 H 1.3330 -0.0704 0.1090 0.043 Uiso 1 1 calc R . . C35 C 1.4255(8) -0.1729(6) 0.1760(4) 0.040(2) Uani 1 1 d . . . H35 H 1.4584 -0.1262 0.1852 0.048 Uiso 1 1 calc R . . C36 C 1.4519(7) -0.2717(6) 0.2071(3) 0.0310(18) Uani 1 1 d . . . C37 C 1.4027(7) -0.3409(6) 0.1945(3) 0.0304(18) Uani 1 1 d . . . H37 H 1.4210 -0.4102 0.2164 0.036 Uiso 1 1 calc R . . C38 C 1.3269(7) -0.3065(6) 0.1497(3) 0.0319(19) Uani 1 1 d . . . H38 H 1.2915 -0.3518 0.1410 0.038 Uiso 1 1 calc R . . C39 C 0.7095(6) 0.4521(5) 0.0200(3) 0.0212(15) Uani 1 1 d . . . C40 C 0.7128(7) 0.5527(5) -0.0010(3) 0.0290(18) Uani 1 1 d . . . H40 H 0.7730 0.5600 -0.0240 0.035 Uiso 1 1 calc R . . C41 C 0.6303(7) 0.6405(6) 0.0110(3) 0.0306(18) Uani 1 1 d . . . H41 H 0.6342 0.7083 -0.0033 0.037 Uiso 1 1 calc R . . C42 C 0.5419(7) 0.6317(6) 0.0434(3) 0.0292(18) Uani 1 1 d . . . H42 H 0.4849 0.6936 0.0512 0.035 Uiso 1 1 calc R . . C43 C 0.5344(7) 0.5331(6) 0.0650(3) 0.0306(18) Uani 1 1 d . . . H43 H 0.4733 0.5269 0.0876 0.037 Uiso 1 1 calc R . . C44 C 0.6191(6) 0.4440(6) 0.0526(3) 0.0258(17) Uani 1 1 d . . . H44 H 0.6150 0.3762 0.0667 0.031 Uiso 1 1 calc R . . C45 C 0.6616(6) 0.0531(5) 0.1038(3) 0.0228(16) Uani 1 1 d . . . C46 C 0.5726(8) 0.1486(7) 0.0876(4) 0.043(2) Uani 1 1 d . . . H46 H 0.5772 0.1947 0.0538 0.051 Uiso 1 1 calc R . . C47 C 0.4789(8) 0.1776(9) 0.1190(4) 0.060(3) Uani 1 1 d . . . H47 H 0.4173 0.2416 0.1065 0.072 Uiso 1 1 calc R . . C48 C 0.4748(8) 0.1110(9) 0.1703(4) 0.060(3) Uani 1 1 d . . . H48 H 0.4115 0.1316 0.1933 0.072 Uiso 1 1 calc R . . C49 C 0.5620(8) 0.0162(8) 0.1871(4) 0.047(2) Uani 1 1 d . . . H49 H 0.5582 -0.0296 0.2211 0.057 Uiso 1 1 calc R . . C50 C 0.6541(7) -0.0115(6) 0.1546(3) 0.0329(19) Uani 1 1 d . . . H50 H 0.7148 -0.0763 0.1669 0.039 Uiso 1 1 calc R . . C51 C 1.0522(7) -0.2105(6) 0.1625(3) 0.0313(18) Uani 1 1 d . . . H51A H 1.1070 -0.1841 0.1753 0.047 Uiso 1 1 calc R . . H51B H 1.0587 -0.2784 0.1866 0.047 Uiso 1 1 calc R . . H51C H 0.9754 -0.1596 0.1642 0.047 Uiso 1 1 calc R . . C52 C 1.2080(7) 0.1560(7) 0.0555(4) 0.039(2) Uani 1 1 d . . . H52A H 1.2155 0.1231 0.0951 0.058 Uiso 1 1 calc R . . H52B H 1.2335 0.2164 0.0497 0.058 Uiso 1 1 calc R . . H52C H 1.2546 0.1042 0.0340 0.058 Uiso 1 1 calc R . . N1 N 0.6478(10) 0.1565(8) 0.3110(4) 0.026(2) Uani 0.707(10) 1 d PU D 1 C53 C 0.6643(12) 0.2410(9) 0.3231(4) 0.037(3) Uani 0.707(10) 1 d PU D 1 H53 H 0.6536 0.2537 0.3600 0.045 Uiso 0.707(10) 1 calc PR D 1 C54 C 0.6962(12) 0.3088(9) 0.2830(5) 0.042(3) Uani 0.707(10) 1 d PU D 1 H54 H 0.7035 0.3696 0.2922 0.050 Uiso 0.707(10) 1 calc PR D 1 C55 C 0.7180(12) 0.2917(9) 0.2299(5) 0.026(3) Uani 0.707(10) 1 d PU D 1 C56 C 0.7037(10) 0.2022(9) 0.2186(4) 0.018(2) Uani 0.707(10) 1 d PU D 1 H56 H 0.7167 0.1862 0.1825 0.021 Uiso 0.707(10) 1 calc PR D 1 C57 C 0.6707(11) 0.1377(9) 0.2602(5) 0.022(3) Uani 0.707(10) 1 d PU D 1 H57 H 0.6638 0.0759 0.2521 0.026 Uiso 0.707(10) 1 calc PR D 1 N1A N 0.6123(18) 0.1596(13) 0.2984(8) 0.030(5) Uani 0.293(10) 1 d PGU D 2 C53A C 0.5545(16) 0.2679(14) 0.2913(8) 0.041(5) Uani 0.293(10) 1 d PGU D 2 H53A H 0.4907 0.2946 0.3131 0.049 Uiso 0.293(10) 1 calc PR D 2 C54A C 0.5899(18) 0.3372(12) 0.2523(9) 0.041(5) Uani 0.293(10) 1 d PGU D 2 H54A H 0.5504 0.4113 0.2475 0.049 Uiso 0.293(10) 1 calc PR D 2 C55A C 0.6832(18) 0.2982(17) 0.2204(8) 0.031(6) Uani 0.293(10) 1 d PGU D 2 C56A C 0.7410(17) 0.1899(19) 0.2274(10) 0.035(6) Uani 0.293(10) 1 d PGU D 2 H56A H 0.8048 0.1632 0.2056 0.042 Uiso 0.293(10) 1 calc PR D 2 C57A C 0.7056(18) 0.1206(13) 0.2665(10) 0.028(5) Uani 0.293(10) 1 d PGU D 2 H57A H 0.7451 0.0466 0.2713 0.033 Uiso 0.293(10) 1 calc PR D 2 C58 C 0.7518(7) 0.3618(6) 0.1850(3) 0.0284(18) Uani 1 1 d . . . C59 C 0.7290(8) 0.4649(6) 0.1870(3) 0.037(2) Uani 1 1 d . D . C60 C 0.9122(8) 0.5705(6) 0.0839(4) 0.041(2) Uani 1 1 d . . . H60 H 0.9735 0.5446 0.0606 0.049 Uiso 1 1 calc R . . C61 C 0.8678(8) 0.5002(6) 0.1159(4) 0.040(2) Uani 1 1 d . D . H61 H 0.8993 0.4274 0.1141 0.048 Uiso 1 1 calc R . . C62 C 0.7792(7) 0.5340(5) 0.1499(3) 0.0235(17) Uani 1 1 d . . . C63 C 0.7337(8) 0.6412(6) 0.1481(3) 0.039(2) Uani 1 1 d . D . C64 C 0.7822(7) 0.7071(6) 0.1153(4) 0.039(2) Uani 1 1 d . . . O1 O 0.5096(4) 0.1877(3) 0.40624(19) 0.0214(11) Uani 1 1 d . B . O2 O 0.3386(4) 0.2221(3) 0.46765(19) 0.0231(11) Uani 1 1 d . B . O3 O 0.3203(4) 0.0220(4) 0.45999(19) 0.0230(11) Uani 1 1 d . . . O4 O 0.2579(4) -0.0027(4) 0.57431(19) 0.0233(11) Uani 1 1 d . . . O5 O 0.2534(4) 0.2044(3) 0.57278(19) 0.0210(11) Uani 1 1 d . . . O6 O 0.4401(4) 0.0362(3) 0.35737(19) 0.0229(11) Uani 1 1 d . C . O7 O 0.5605(4) -0.0382(3) 0.44891(18) 0.0169(10) Uani 1 1 d . . . O8 O 0.5584(4) -0.1812(3) 0.38453(19) 0.0205(11) Uani 1 1 d . C . O9 O 0.6722(4) -0.0723(4) 0.33645(19) 0.0252(12) Uani 1 1 d . D . O10 O 0.4684(4) -0.1937(3) 0.49249(19) 0.0222(11) Uani 1 1 d . . . O11 O 1.0749(4) -0.2246(3) 0.10589(18) 0.0224(11) Uani 1 1 d . . . O12 O 1.2463(4) -0.2860(3) 0.02655(19) 0.0205(11) Uani 1 1 d . . . O13 O 1.2457(4) -0.0826(3) -0.00475(19) 0.0211(11) Uani 1 1 d . . . O14 O 1.1057(4) -0.0209(3) 0.08394(18) 0.0183(10) Uani 1 1 d . . . O15 O 1.1700(4) 0.1006(4) -0.06735(19) 0.0243(11) Uani 1 1 d . . . O16 O 0.9595(4) 0.1213(3) -0.00526(17) 0.0180(10) Uani 1 1 d . . . O17 O 1.0923(4) 0.1915(3) 0.0373(2) 0.0241(11) Uani 1 1 d . . . O18 O 0.9086(4) 0.3613(3) -0.0288(2) 0.0230(11) Uani 1 1 d . . . O19 O 0.8595(4) 0.2639(3) 0.06228(19) 0.0198(10) Uani 1 1 d . . . O20 O 0.8695(4) 0.0516(3) 0.09465(18) 0.0225(11) Uani 1 1 d . . . Cl1 Cl 0.0575(2) -0.2146(2) 0.31510(9) 0.0506(6) Uani 1 1 d . . . Cl2 Cl -0.25476(19) 0.3467(2) 0.44094(10) 0.0518(6) Uani 1 1 d . . . Cl3 Cl 1.0283(12) 0.2084(16) 0.3238(6) 0.078(4) Uani 0.54(3) 1 d PDU E 1 Cl3A Cl 1.0330(12) 0.1578(18) 0.3337(4) 0.057(3) Uani 0.46(3) 1 d PDU E 2 Cl4 Cl 1.54254(18) -0.31207(19) 0.26475(8) 0.0442(5) Uani 1 1 d . . . 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 Sb1 0.0217(3) 0.0174(2) 0.0187(2) -0.00345(18) 0.00352(19) -0.0123(2) Sb2 0.0208(3) 0.0186(2) 0.0197(2) -0.00404(18) 0.00377(19) -0.0110(2) Sb3 0.0207(3) 0.0171(2) 0.0180(2) -0.00681(18) 0.00364(19) -0.0094(2) Sb4 0.0185(2) 0.0162(2) 0.0193(2) -0.00589(18) 0.00318(19) -0.00818(19) Co1 0.0291(6) 0.0174(5) 0.0217(5) -0.0021(4) 0.0082(4) -0.0138(4) Co2 0.0219(5) 0.0181(5) 0.0229(5) -0.0060(4) 0.0061(4) -0.0119(4) P1 0.0239(10) 0.0137(9) 0.0221(10) -0.0006(7) 0.0049(8) -0.0090(8) P2 0.0253(10) 0.0169(9) 0.0199(9) -0.0033(7) 0.0030(8) -0.0116(8) P3 0.0213(10) 0.0163(9) 0.0232(10) -0.0083(7) 0.0036(8) -0.0075(8) P4 0.0211(10) 0.0192(9) 0.0182(9) -0.0052(7) 0.0071(7) -0.0116(8) N2 0.026(4) 0.017(3) 0.036(4) -0.006(3) 0.008(3) -0.010(3) C1 0.024(4) 0.009(3) 0.031(4) -0.003(3) -0.001(3) -0.005(3) C2 0.025(4) 0.028(4) 0.042(5) -0.016(3) 0.012(4) -0.014(3) C3 0.041(5) 0.051(5) 0.024(4) -0.023(4) 0.014(4) -0.026(4) C4 0.039(5) 0.051(5) 0.024(4) -0.017(4) 0.007(4) -0.031(4) C5 0.029(5) 0.050(5) 0.034(5) -0.005(4) 0.009(4) -0.021(4) C6 0.028(4) 0.034(4) 0.025(4) -0.016(3) 0.008(3) -0.016(4) C7 0.032(5) 0.025(4) 0.025(4) -0.002(3) 0.008(3) -0.008(4) C8 0.050(6) 0.041(5) 0.044(5) -0.026(4) 0.009(5) -0.009(5) C9 0.036(5) 0.050(6) 0.051(6) -0.017(4) 0.002(4) -0.019(5) C10 0.015(4) 0.049(5) 0.042(5) 0.002(4) 0.001(4) -0.005(4) C11 0.025(5) 0.043(5) 0.071(7) -0.010(5) -0.003(5) -0.007(4) C13 0.037(7) 0.012(6) 0.038(7) -0.009(5) 0.006(6) -0.010(5) C14 0.055(9) 0.023(6) 0.051(8) -0.011(6) 0.005(7) -0.021(6) C15 0.071(10) 0.023(6) 0.052(8) -0.019(6) 0.013(8) -0.022(7) C16 0.059(10) 0.023(7) 0.057(8) -0.003(6) 0.007(8) -0.020(7) C17 0.057(9) 0.024(6) 0.049(7) 0.010(6) -0.013(7) -0.015(7) C18 0.058(8) 0.018(6) 0.046(7) 0.001(5) -0.003(7) -0.017(6) C12 0.030(5) 0.034(5) 0.079(7) -0.013(5) 0.001(5) -0.015(4) C13A 0.031(7) 0.018(6) 0.027(6) -0.003(5) -0.010(6) -0.016(5) C14A 0.052(8) 0.028(7) 0.049(8) -0.010(6) 0.012(7) -0.020(6) C15A 0.064(11) 0.034(8) 0.074(11) -0.012(8) 0.006(9) -0.011(8) C16A 0.058(9) 0.021(6) 0.063(8) 0.000(6) -0.002(7) -0.018(6) C17A 0.042(8) 0.022(6) 0.055(8) 0.007(6) -0.011(6) -0.025(6) C18A 0.035(7) 0.021(6) 0.032(7) 0.007(5) -0.001(6) -0.018(6) C19 0.025(4) 0.018(4) 0.029(4) -0.002(3) -0.005(3) -0.014(3) C20 0.039(5) 0.033(4) 0.039(5) -0.011(4) 0.001(4) -0.021(4) C21 0.036(5) 0.049(5) 0.040(5) -0.022(4) 0.017(4) -0.020(4) C22 0.045(6) 0.035(5) 0.051(6) -0.022(4) 0.011(5) -0.014(4) C23 0.054(6) 0.031(5) 0.042(5) -0.019(4) 0.001(4) -0.014(4) C24 0.027(4) 0.027(4) 0.028(4) -0.006(3) -0.005(3) -0.010(3) C25 0.032(5) 0.054(5) 0.040(5) -0.010(4) 0.010(4) -0.026(4) C26 0.028(4) 0.032(4) 0.026(4) 0.000(3) 0.000(3) -0.005(4) C27 0.025(4) 0.024(4) 0.021(4) -0.015(3) -0.003(3) -0.001(3) C28 0.060(7) 0.041(5) 0.043(6) -0.007(4) 0.011(5) -0.005(5) C29 0.068(8) 0.080(8) 0.020(5) -0.012(5) 0.003(5) 0.007(6) C30 0.030(5) 0.107(9) 0.039(6) -0.044(6) 0.003(4) 0.000(6) C31 0.039(6) 0.089(8) 0.071(8) -0.054(6) 0.007(5) -0.025(6) C32 0.043(6) 0.045(5) 0.041(5) -0.021(4) 0.003(4) -0.005(4) C33 0.010(3) 0.020(3) 0.017(3) -0.002(3) -0.005(3) -0.002(3) C34 0.038(5) 0.029(4) 0.047(5) -0.013(4) 0.003(4) -0.018(4) C35 0.039(5) 0.036(5) 0.050(6) -0.018(4) -0.011(4) -0.015(4) C36 0.027(4) 0.044(5) 0.022(4) -0.013(4) 0.007(3) -0.010(4) C37 0.030(4) 0.034(4) 0.030(4) 0.000(3) -0.009(3) -0.015(4) C38 0.043(5) 0.029(4) 0.033(5) -0.013(3) 0.008(4) -0.020(4) C39 0.027(4) 0.016(3) 0.021(4) -0.007(3) 0.004(3) -0.006(3) C40 0.029(4) 0.026(4) 0.035(4) -0.009(3) 0.013(4) -0.013(4) C41 0.029(5) 0.028(4) 0.032(4) -0.008(3) -0.003(4) -0.006(4) C42 0.021(4) 0.026(4) 0.036(5) -0.011(3) -0.003(3) 0.000(3) C43 0.028(4) 0.036(4) 0.036(5) -0.021(4) 0.008(4) -0.013(4) C44 0.022(4) 0.022(4) 0.033(4) -0.004(3) -0.002(3) -0.007(3) C45 0.020(4) 0.025(4) 0.026(4) -0.005(3) 0.001(3) -0.011(3) C46 0.034(5) 0.062(6) 0.031(5) -0.019(4) 0.004(4) -0.012(5) C47 0.031(5) 0.097(8) 0.036(6) -0.019(5) 0.006(4) 0.000(5) C48 0.026(5) 0.112(9) 0.043(6) -0.034(6) 0.013(4) -0.018(6) C49 0.037(6) 0.066(6) 0.055(6) -0.024(5) 0.015(5) -0.032(5) C50 0.032(5) 0.034(4) 0.041(5) -0.016(4) 0.004(4) -0.016(4) C51 0.033(5) 0.042(5) 0.026(4) -0.012(3) 0.012(4) -0.020(4) C52 0.033(5) 0.041(5) 0.053(6) -0.013(4) 0.003(4) -0.026(4) N1 0.036(6) 0.028(4) 0.022(5) -0.008(4) 0.001(4) -0.021(4) C53 0.071(8) 0.045(6) 0.017(5) -0.016(4) 0.012(5) -0.042(6) C54 0.076(8) 0.036(5) 0.039(6) -0.016(4) 0.014(5) -0.047(5) C55 0.044(7) 0.023(5) 0.021(5) -0.012(4) 0.019(5) -0.022(5) C56 0.021(5) 0.024(5) 0.013(4) -0.002(4) -0.001(4) -0.014(4) C57 0.026(6) 0.022(5) 0.024(5) -0.006(4) 0.003(5) -0.014(4) N1A 0.036(10) 0.035(7) 0.029(9) -0.008(7) 0.008(8) -0.024(8) C53A 0.053(10) 0.035(8) 0.031(9) 0.003(8) 0.017(8) -0.020(8) C54A 0.054(10) 0.037(8) 0.031(9) -0.006(8) 0.014(8) -0.019(8) C55A 0.048(10) 0.033(7) 0.022(8) -0.007(7) 0.008(8) -0.023(8) C56A 0.041(10) 0.033(8) 0.027(9) -0.001(7) 0.013(8) -0.013(8) C57A 0.034(10) 0.026(8) 0.025(8) -0.003(7) -0.001(8) -0.014(7) C58 0.039(5) 0.035(4) 0.015(4) 0.004(3) 0.008(3) -0.024(4) C59 0.062(6) 0.029(4) 0.022(4) -0.001(3) 0.016(4) -0.023(4) C60 0.043(5) 0.035(5) 0.051(6) -0.015(4) 0.027(4) -0.022(4) C61 0.044(5) 0.024(4) 0.058(6) -0.007(4) 0.013(5) -0.023(4) C62 0.038(5) 0.017(3) 0.021(4) -0.005(3) 0.010(3) -0.017(3) C63 0.055(6) 0.032(4) 0.037(5) -0.007(4) 0.027(4) -0.026(4) C64 0.034(5) 0.027(4) 0.054(6) -0.005(4) 0.020(4) -0.012(4) O1 0.027(3) 0.016(2) 0.022(3) 0.0010(19) 0.000(2) -0.010(2) O2 0.023(3) 0.021(3) 0.021(3) 0.003(2) -0.003(2) -0.006(2) O3 0.019(3) 0.025(3) 0.026(3) -0.006(2) -0.001(2) -0.007(2) O4 0.025(3) 0.023(3) 0.026(3) -0.004(2) 0.009(2) -0.015(2) O5 0.021(3) 0.018(2) 0.023(3) -0.001(2) 0.005(2) -0.007(2) O6 0.032(3) 0.019(2) 0.020(3) 0.002(2) 0.002(2) -0.014(2) O7 0.016(2) 0.017(2) 0.019(2) -0.0019(19) -0.0038(19) -0.008(2) O8 0.024(3) 0.014(2) 0.025(3) -0.0059(19) 0.008(2) -0.008(2) O9 0.035(3) 0.020(2) 0.023(3) 0.000(2) 0.007(2) -0.016(2) O10 0.025(3) 0.023(3) 0.022(3) -0.002(2) 0.005(2) -0.015(2) O11 0.031(3) 0.021(2) 0.019(3) -0.007(2) 0.007(2) -0.013(2) O12 0.021(3) 0.016(2) 0.027(3) -0.009(2) 0.008(2) -0.007(2) O13 0.018(3) 0.018(2) 0.027(3) 0.000(2) -0.001(2) -0.008(2) O14 0.020(3) 0.015(2) 0.023(3) -0.0030(19) -0.007(2) -0.009(2) O15 0.030(3) 0.024(3) 0.024(3) -0.002(2) 0.007(2) -0.018(2) O16 0.025(3) 0.023(2) 0.013(2) -0.0035(19) 0.002(2) -0.016(2) O17 0.019(3) 0.020(2) 0.036(3) -0.007(2) 0.005(2) -0.009(2) O18 0.024(3) 0.018(2) 0.031(3) -0.008(2) 0.007(2) -0.011(2) O19 0.023(3) 0.016(2) 0.024(3) -0.0094(19) 0.005(2) -0.009(2) O20 0.042(3) 0.019(2) 0.015(2) -0.0053(19) 0.011(2) -0.020(2) Cl1 0.0481(14) 0.0835(17) 0.0455(13) -0.0314(12) 0.0078(11) -0.0445(14) Cl2 0.0260(12) 0.0645(16) 0.0565(15) -0.0014(12) -0.0031(10) -0.0115(11) Cl3 0.078(4) 0.102(8) 0.041(4) -0.043(5) -0.005(4) -0.001(6) Cl3A 0.050(4) 0.111(9) 0.022(3) -0.032(4) 0.002(3) -0.032(6) Cl4 0.0308(12) 0.0740(16) 0.0299(11) -0.0190(10) 0.0011(9) -0.0168(11) _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 Sb1 O3 1.928(5) . ? Sb1 O7 1.965(5) . ? Sb1 O6 2.021(4) . ? Sb1 O10 2.030(4) . ? Sb1 O8 2.068(4) . ? Sb1 C1 2.118(7) . ? Sb2 O3 1.936(5) . ? Sb2 O7 1.967(5) 2_656 ? Sb2 O2 2.026(4) . ? Sb2 O4 2.028(4) . ? Sb2 O5 2.043(5) . ? Sb2 C7 2.090(8) . ? Sb3 O14 1.925(4) . ? Sb3 O16 1.953(4) . ? Sb3 O20 2.000(5) . ? Sb3 O17 2.031(5) . ? Sb3 O19 2.078(4) . ? Sb3 C27 2.112(7) . ? Sb4 O14 1.927(4) . ? Sb4 O16 1.970(5) 2_755 ? Sb4 O13 2.020(4) . ? Sb4 O11 2.030(5) . ? Sb4 O12 2.051(4) . ? Sb4 C33 2.119(6) . ? Co1 O1 2.005(5) . ? Co1 N1 2.114(10) . ? Co1 O9 2.119(5) . ? Co1 O4 2.126(5) 2_656 ? Co1 O6 2.136(5) . ? Co1 O7 2.148(4) . ? Co1 N1A 2.156(15) . ? Co2 O15 2.047(5) . ? Co2 O17 2.097(5) . ? Co2 N2 2.103(6) . ? Co2 O18 2.126(5) . ? Co2 O11 2.128(5) 2_755 ? Co2 O16 2.158(4) . ? P1 O1 1.494(5) . ? P1 O10 1.527(5) 2_656 ? P1 O2 1.550(5) . ? P1 C13A 1.784(7) . ? P1 C13 1.823(7) . ? P2 O9 1.500(5) . ? P2 O8 1.544(5) . ? P2 O5 1.567(5) 2_656 ? P2 C19 1.781(7) . ? P3 O18 1.511(5) . ? P3 O19 1.536(5) . ? P3 O12 1.544(5) 2_755 ? P3 C39 1.778(7) . ? P4 O15 1.510(5) 2_755 ? P4 O20 1.556(5) . ? P4 O13 1.558(5) 2_755 ? P4 C45 1.773(7) . ? N2 C64 1.317(10) 2_765 ? N2 C60 1.338(9) 2_765 ? C1 C2 1.377(10) . ? C1 C6 1.392(10) . ? C2 C3 1.387(11) . ? C2 H2 0.9500 . ? C3 C4 1.383(10) . ? C3 H3 0.9500 . ? C4 C5 1.362(11) . ? C4 Cl1 1.732(8) . ? C5 C6 1.399(11) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.396(11) . ? C7 C8 1.415(12) . ? C8 C9 1.400(13) . ? C8 H8 0.9500 . ? C9 C10 1.367(12) . ? C9 H9 0.9500 . ? C10 C11 1.365(13) . ? C10 Cl2 1.733(8) . ? C11 C12 1.386(12) . ? C11 H11 0.9500 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9500 . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C12 H12 0.9500 . ? C13A C14A 1.3900 . ? C13A C18A 1.3900 . ? C14A C15A 1.3900 . ? C14A H14A 0.9500 . ? C15A C16A 1.3900 . ? C15A H15A 0.9500 . ? C16A C17A 1.3900 . ? C16A H16A 0.9500 . ? C17A C18A 1.3900 . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C19 C20 1.393(10) . ? C19 C24 1.408(9) . ? C20 C21 1.392(11) . ? C20 H20 0.9500 . ? C21 C22 1.364(11) . ? C21 H21 0.9500 . ? C22 C23 1.392(12) . ? C22 H22 0.9500 . ? C23 C24 1.365(11) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 O4 1.444(9) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 O6 1.435(9) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.385(11) . ? C27 C32 1.400(11) . ? C28 C29 1.393(13) . ? C28 H28 0.9500 . ? C29 C30 1.367(16) . ? C29 H29 0.9500 . ? C30 C31 1.359(15) . ? C30 Cl3A 1.763(12) . ? C30 Cl3 1.781(12) . ? C31 C32 1.388(13) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.361(10) . ? C33 C38 1.397(9) . ? C34 C35 1.384(11) . ? C34 H34 0.9500 . ? C35 C36 1.355(11) . ? C35 H35 0.9500 . ? C36 C37 1.402(11) . ? C36 Cl4 1.731(8) . ? C37 C38 1.382(11) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.391(10) . ? C39 C40 1.396(9) . ? C40 C41 1.365(10) . ? C40 H40 0.9500 . ? C41 C42 1.370(11) . ? C41 H41 0.9500 . ? C42 C43 1.394(10) . ? C42 H42 0.9500 . ? C43 C44 1.392(10) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.390(11) . ? C45 C50 1.400(10) . ? C46 C47 1.366(12) . ? C46 H46 0.9500 . ? C47 C48 1.412(13) . ? C47 H47 0.9500 . ? C48 C49 1.377(13) . ? C48 H48 0.9500 . ? C49 C50 1.364(11) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 O11 1.443(8) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O17 1.429(9) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? N1 C57 1.323(14) . ? N1 C53 1.350(14) . ? C53 C54 1.369(14) . ? C53 H53 0.9500 . ? C54 C55 1.367(16) . ? C54 H54 0.9500 . ? C55 C56 1.396(15) . ? C55 C58 1.469(12) . ? C56 C57 1.365(13) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? N1A C53A 1.3900 . ? N1A C57A 1.3900 . ? C53A C54A 1.3900 . ? C53A H53A 0.9500 . ? C54A C55A 1.3900 . ? C54A H54A 0.9500 . ? C55A C56A 1.3900 . ? C55A C58 1.565(17) . ? C56A C57A 1.3900 . ? C56A H56A 0.9500 . ? C57A H57A 0.9500 . ? C58 C59 1.360(10) . ? C59 C62 1.475(9) . ? C60 N2 1.338(9) 2_765 ? C60 C61 1.384(10) . ? C60 H60 0.9500 . ? C61 C62 1.368(11) . ? C61 H61 0.9500 . ? C62 C63 1.377(10) . ? C63 C64 1.382(10) . ? C64 N2 1.317(10) 2_765 ? O4 Co1 2.126(5) 2_656 ? O5 P2 1.567(5) 2_656 ? O7 Sb2 1.967(5) 2_656 ? O10 P1 1.527(5) 2_656 ? O11 Co2 2.128(5) 2_755 ? O12 P3 1.544(5) 2_755 ? O13 P4 1.558(5) 2_755 ? O15 P4 1.510(5) 2_755 ? O16 Sb4 1.970(5) 2_755 ? 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 O3 Sb1 O7 94.8(2) . . ? O3 Sb1 O6 93.98(19) . . ? O7 Sb1 O6 80.76(19) . . ? O3 Sb1 O10 92.80(19) . . ? O7 Sb1 O10 89.19(19) . . ? O6 Sb1 O10 168.3(2) . . ? O3 Sb1 O8 178.2(2) . . ? O7 Sb1 O8 86.99(19) . . ? O6 Sb1 O8 86.07(18) . . ? O10 Sb1 O8 87.46(18) . . ? O3 Sb1 C1 91.5(2) . . ? O7 Sb1 C1 173.0(2) . . ? O6 Sb1 C1 95.8(2) . . ? O10 Sb1 C1 93.6(2) . . ? O8 Sb1 C1 86.7(2) . . ? O3 Sb2 O7 93.41(19) . 2_656 ? O3 Sb2 O2 94.15(19) . . ? O7 Sb2 O2 90.81(19) 2_656 . ? O3 Sb2 O4 92.55(19) . . ? O7 Sb2 O4 80.13(19) 2_656 . ? O2 Sb2 O4 169.0(2) . . ? O3 Sb2 O5 179.03(18) . . ? O7 Sb2 O5 87.07(19) 2_656 . ? O2 Sb2 O5 85.00(18) . . ? O4 Sb2 O5 88.36(18) . . ? O3 Sb2 C7 93.1(3) . . ? O7 Sb2 C7 172.6(2) 2_656 . ? O2 Sb2 C7 92.2(2) . . ? O4 Sb2 C7 96.1(2) . . ? O5 Sb2 C7 86.4(3) . . ? O14 Sb3 O16 94.34(19) . . ? O14 Sb3 O20 91.47(19) . . ? O16 Sb3 O20 89.93(18) . . ? O14 Sb3 O17 93.12(19) . . ? O16 Sb3 O17 80.23(19) . . ? O20 Sb3 O17 169.4(2) . . ? O14 Sb3 O19 179.43(19) . . ? O16 Sb3 O19 86.16(18) . . ? O20 Sb3 O19 88.26(19) . . ? O17 Sb3 O19 87.22(18) . . ? O14 Sb3 C27 92.4(2) . . ? O16 Sb3 C27 172.8(2) . . ? O20 Sb3 C27 92.5(2) . . ? O17 Sb3 C27 96.8(3) . . ? O19 Sb3 C27 87.1(2) . . ? O14 Sb4 O16 95.99(19) . 2_755 ? O14 Sb4 O13 90.97(19) . . ? O16 Sb4 O13 90.09(18) 2_755 . ? O14 Sb4 O11 95.14(18) . . ? O16 Sb4 O11 79.50(19) 2_755 . ? O13 Sb4 O11 168.41(19) . . ? O14 Sb4 O12 175.31(19) . . ? O16 Sb4 O12 86.86(19) 2_755 . ? O13 Sb4 O12 85.28(18) . . ? O11 Sb4 O12 89.04(17) . . ? O14 Sb4 C33 89.7(2) . . ? O16 Sb4 C33 171.0(2) 2_755 . ? O13 Sb4 C33 96.7(2) . . ? O11 Sb4 C33 93.1(2) . . ? O12 Sb4 C33 87.9(2) . . ? O1 Co1 N1 88.1(3) . . ? O1 Co1 O9 176.0(2) . . ? N1 Co1 O9 90.3(3) . . ? O1 Co1 O4 97.68(19) . 2_656 ? N1 Co1 O4 95.9(3) . 2_656 ? O9 Co1 O4 86.10(19) . 2_656 ? O1 Co1 O6 93.04(19) . . ? N1 Co1 O6 116.5(3) . . ? O9 Co1 O6 84.41(19) . . ? O4 Co1 O6 146.16(17) 2_656 . ? O1 Co1 O7 89.57(17) . . ? N1 Co1 O7 169.2(3) . . ? O9 Co1 O7 92.65(17) . . ? O4 Co1 O7 73.95(17) 2_656 . ? O6 Co1 O7 74.13(17) . . ? O1 Co1 N1A 89.4(6) . . ? N1 Co1 N1A 14.5(6) . . ? O9 Co1 N1A 88.1(6) . . ? O4 Co1 N1A 110.1(6) 2_656 . ? O6 Co1 N1A 102.0(6) . . ? O7 Co1 N1A 176.0(6) . . ? O15 Co2 O17 95.00(19) . . ? O15 Co2 N2 89.3(2) . . ? O17 Co2 N2 103.6(2) . . ? O15 Co2 O18 177.87(18) . . ? O17 Co2 O18 86.93(19) . . ? N2 Co2 O18 89.3(2) . . ? O15 Co2 O11 93.48(19) . 2_755 ? O17 Co2 O11 146.27(18) . 2_755 ? N2 Co2 O11 109.1(2) . 2_755 ? O18 Co2 O11 85.40(19) . 2_755 ? O15 Co2 O16 89.45(17) . . ? O17 Co2 O16 74.21(17) . . ? N2 Co2 O16 177.4(2) . . ? O18 Co2 O16 91.95(17) . . ? O11 Co2 O16 73.28(17) 2_755 . ? O1 P1 O10 113.9(3) . 2_656 ? O1 P1 O2 113.0(3) . . ? O10 P1 O2 111.2(3) 2_656 . ? O1 P1 C13A 104.8(4) . . ? O10 P1 C13A 110.7(5) 2_656 . ? O2 P1 C13A 102.3(4) . . ? O1 P1 C13 106.8(4) . . ? O10 P1 C13 101.1(4) 2_656 . ? O2 P1 C13 110.0(5) . . ? C13A P1 C13 10.3(6) . . ? O9 P2 O8 112.5(3) . . ? O9 P2 O5 112.3(3) . 2_656 ? O8 P2 O5 109.0(3) . 2_656 ? O9 P2 C19 111.1(3) . . ? O8 P2 C19 107.5(3) . . ? O5 P2 C19 104.0(3) 2_656 . ? O18 P3 O19 112.8(3) . . ? O18 P3 O12 111.3(3) . 2_755 ? O19 P3 O12 109.6(3) . 2_755 ? O18 P3 C39 111.8(3) . . ? O19 P3 C39 105.7(3) . . ? O12 P3 C39 105.2(3) 2_755 . ? O15 P4 O20 112.2(3) 2_755 . ? O15 P4 O13 112.6(3) 2_755 2_755 ? O20 P4 O13 111.5(3) . 2_755 ? O15 P4 C45 109.7(3) 2_755 . ? O20 P4 C45 103.8(3) . . ? O13 P4 C45 106.4(3) 2_755 . ? C64 N2 C60 116.9(6) 2_765 2_765 ? C64 N2 Co2 122.0(5) 2_765 . ? C60 N2 Co2 120.8(5) 2_765 . ? C2 C1 C6 119.4(7) . . ? C2 C1 Sb1 120.6(5) . . ? C6 C1 Sb1 120.0(5) . . ? C1 C2 C3 120.6(7) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 119.5(7) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 120.8(7) . . ? C5 C4 Cl1 119.8(6) . . ? C3 C4 Cl1 119.3(6) . . ? C4 C5 C6 119.8(7) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 119.8(7) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C12 C7 C8 115.8(8) . . ? C12 C7 Sb2 123.5(6) . . ? C8 C7 Sb2 120.6(6) . . ? C9 C8 C7 121.7(8) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C10 C9 C8 119.0(9) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 121.5(8) . . ? C11 C10 Cl2 120.2(7) . . ? C9 C10 Cl2 118.3(7) . . ? C10 C11 C12 119.3(9) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C14 C13 C18 120.0 . . ? C14 C13 P1 124.5(6) . . ? C18 C13 P1 115.5(6) . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C11 C12 C7 122.6(9) . . ? C11 C12 H12 118.7 . . ? C7 C12 H12 118.7 . . ? C14A C13A C18A 120.0 . . ? C14A C13A P1 121.8(6) . . ? C18A C13A P1 118.1(6) . . ? C15A C14A C13A 120.0 . . ? C15A C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C14A C15A C16A 120.0 . . ? C14A C15A H15A 120.0 . . ? C16A C15A H15A 120.0 . . ? C17A C16A C15A 120.0 . . ? C17A C16A H16A 120.0 . . ? C15A C16A H16A 120.0 . . ? C18A C17A C16A 120.0 . . ? C18A C17A H17A 120.0 . . ? C16A C17A H17A 120.0 . . ? C17A C18A C13A 120.0 . . ? C17A C18A H18A 120.0 . . ? C13A C18A H18A 120.0 . . ? C20 C19 C24 118.2(7) . . ? C20 C19 P2 120.2(5) . . ? C24 C19 P2 121.6(6) . . ? C21 C20 C19 120.6(7) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 120.3(8) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.0(8) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.5(8) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C19 120.5(7) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? O4 C25 H25A 109.5 . . ? O4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 118.6(8) . . ? C28 C27 Sb3 121.6(6) . . ? C32 C27 Sb3 119.7(6) . . ? C27 C28 C29 120.8(10) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 118.2(10) . . ? C30 C29 H29 120.9 . . ? C28 C29 H29 120.9 . . ? C31 C30 C29 123.3(9) . . ? C31 C30 Cl3A 128.6(12) . . ? C29 C30 Cl3A 107.9(11) . . ? C31 C30 Cl3 108.0(12) . . ? C29 C30 Cl3 128.7(12) . . ? Cl3A C30 Cl3 21.9(4) . . ? C30 C31 C32 118.4(10) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? C31 C32 C27 120.6(9) . . ? C31 C32 H32 119.7 . . ? C27 C32 H32 119.7 . . ? C34 C33 C38 119.5(7) . . ? C34 C33 Sb4 121.9(5) . . ? C38 C33 Sb4 117.7(5) . . ? C33 C34 C35 120.7(7) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C36 C35 C34 120.2(8) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 120.6(8) . . ? C35 C36 Cl4 120.2(7) . . ? C37 C36 Cl4 119.1(6) . . ? C38 C37 C36 118.7(7) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? C37 C38 C33 120.3(7) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? C44 C39 C40 118.3(6) . . ? C44 C39 P3 119.9(5) . . ? C40 C39 P3 121.8(5) . . ? C41 C40 C39 120.7(7) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C42 120.6(7) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C43 120.8(7) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 118.2(7) . . ? C44 C43 H43 120.9 . . ? C42 C43 H43 120.9 . . ? C39 C44 C43 121.4(7) . . ? C39 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C46 C45 C50 117.9(7) . . ? C46 C45 P4 122.1(6) . . ? C50 C45 P4 119.9(6) . . ? C47 C46 C45 121.5(9) . . ? C47 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C46 C47 C48 119.0(9) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C49 C48 C47 120.3(9) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C50 C49 C48 119.5(9) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C45 121.7(8) . . ? C49 C50 H50 119.1 . . ? C45 C50 H50 119.1 . . ? O11 C51 H51A 109.5 . . ? O11 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O11 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O17 C52 H52A 109.5 . . ? O17 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O17 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C57 N1 C53 117.7(9) . . ? C57 N1 Co1 123.8(8) . . ? C53 N1 Co1 118.4(8) . . ? N1 C53 C54 120.8(10) . . ? N1 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? C55 C54 C53 122.1(10) . . ? C55 C54 H54 119.0 . . ? C53 C54 H54 119.0 . . ? C54 C55 C56 116.2(9) . . ? C54 C55 C58 124.6(10) . . ? C56 C55 C58 119.2(10) . . ? C57 C56 C55 119.2(10) . . ? C57 C56 H56 120.4 . . ? C55 C56 H56 120.4 . . ? N1 C57 C56 123.8(10) . . ? N1 C57 H57 118.1 . . ? C56 C57 H57 118.1 . . ? C53A N1A C57A 120.0 . . ? C53A N1A Co1 118.7(11) . . ? C57A N1A Co1 118.4(11) . . ? C54A C53A N1A 120.0 . . ? C54A C53A H53A 120.0 . . ? N1A C53A H53A 120.0 . . ? C53A C54A C55A 120.0 . . ? C53A C54A H54A 120.0 . . ? C55A C54A H54A 120.0 . . ? C56A C55A C54A 120.0 . . ? C56A C55A C58 111.4(14) . . ? C54A C55A C58 127.1(14) . . ? C57A C56A C55A 120.0 . . ? C57A C56A H56A 120.0 . . ? C55A C56A H56A 120.0 . . ? C56A C57A N1A 120.0 . . ? C56A C57A H57A 120.0 . . ? N1A C57A H57A 120.0 . . ? C59 C58 C55 121.0(8) . . ? C59 C58 C55A 120.6(11) . . ? C55 C58 C55A 17.8(11) . . ? C58 C59 C62 123.9(7) . . ? N2 C60 C61 122.1(7) 2_765 . ? N2 C60 H60 119.0 2_765 . ? C61 C60 H60 119.0 . . ? C62 C61 C60 120.9(7) . . ? C62 C61 H61 119.5 . . ? C60 C61 H61 119.5 . . ? C61 C62 C63 116.5(6) . . ? C61 C62 C59 125.0(6) . . ? C63 C62 C59 118.5(7) . . ? C62 C63 C64 119.5(7) . . ? N2 C64 C63 123.9(7) 2_765 . ? P1 O1 Co1 148.4(3) . . ? P1 O2 Sb2 134.1(3) . . ? Sb1 O3 Sb2 145.6(3) . . ? C25 O4 Sb2 120.6(5) . . ? C25 O4 Co1 118.7(5) . 2_656 ? Sb2 O4 Co1 101.1(2) . 2_656 ? P2 O5 Sb2 124.1(3) 2_656 . ? C26 O6 Sb1 121.3(4) . . ? C26 O6 Co1 122.9(4) . . ? Sb1 O6 Co1 101.0(2) . . ? Sb1 O7 Sb2 138.7(2) . 2_656 ? Sb1 O7 Co1 102.39(19) . . ? Sb2 O7 Co1 102.4(2) 2_656 . ? P2 O8 Sb1 123.7(3) . . ? P2 O9 Co1 114.4(3) . . ? P1 O10 Sb1 137.2(3) 2_656 . ? C51 O11 Sb4 120.9(4) . . ? C51 O11 Co2 126.6(4) . 2_755 ? Sb4 O11 Co2 101.77(19) . 2_755 ? P3 O12 Sb4 124.1(3) 2_755 . ? P4 O13 Sb4 136.2(3) 2_755 . ? Sb3 O14 Sb4 145.0(3) . . ? P4 O15 Co2 145.9(3) 2_755 . ? Sb3 O16 Sb4 139.5(3) . 2_755 ? Sb3 O16 Co2 102.02(19) . . ? Sb4 O16 Co2 102.72(18) 2_755 . ? C52 O17 Sb3 121.3(4) . . ? C52 O17 Co2 122.8(5) . . ? Sb3 O17 Co2 101.6(2) . . ? P3 O18 Co2 114.6(2) . . ? P3 O19 Sb3 124.3(3) . . ? P4 O20 Sb3 137.8(3) . . ? 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 O15 Co2 N2 C64 9.9(7) . . . 2_765 ? O17 Co2 N2 C64 104.9(7) . . . 2_765 ? O18 Co2 N2 C64 -168.4(7) . . . 2_765 ? O11 Co2 N2 C64 -83.5(7) 2_755 . . 2_765 ? O16 Co2 N2 C64 72(5) . . . 2_765 ? O15 Co2 N2 C60 -177.1(7) . . . 2_765 ? O17 Co2 N2 C60 -82.1(7) . . . 2_765 ? O18 Co2 N2 C60 4.6(7) . . . 2_765 ? O11 Co2 N2 C60 89.5(7) 2_755 . . 2_765 ? O16 Co2 N2 C60 -115(4) . . . 2_765 ? O3 Sb1 C1 C2 131.0(6) . . . . ? O7 Sb1 C1 C2 -23(2) . . . . ? O6 Sb1 C1 C2 36.8(6) . . . . ? O10 Sb1 C1 C2 -136.1(5) . . . . ? O8 Sb1 C1 C2 -48.9(5) . . . . ? O3 Sb1 C1 C6 -46.6(6) . . . . ? O7 Sb1 C1 C6 159.2(15) . . . . ? O6 Sb1 C1 C6 -140.7(5) . . . . ? O10 Sb1 C1 C6 46.3(6) . . . . ? O8 Sb1 C1 C6 133.6(6) . . . . ? C6 C1 C2 C3 -2.1(11) . . . . ? Sb1 C1 C2 C3 -179.6(6) . . . . ? C1 C2 C3 C4 3.1(12) . . . . ? C2 C3 C4 C5 -2.3(13) . . . . ? C2 C3 C4 Cl1 -178.8(6) . . . . ? C3 C4 C5 C6 0.6(13) . . . . ? Cl1 C4 C5 C6 177.1(6) . . . . ? C2 C1 C6 C5 0.4(11) . . . . ? Sb1 C1 C6 C5 177.9(6) . . . . ? C4 C5 C6 C1 0.4(12) . . . . ? O3 Sb2 C7 C12 -150.5(7) . . . . ? O7 Sb2 C7 C12 57(2) 2_656 . . . ? O2 Sb2 C7 C12 -56.2(7) . . . . ? O4 Sb2 C7 C12 116.6(7) . . . . ? O5 Sb2 C7 C12 28.6(7) . . . . ? O3 Sb2 C7 C8 34.3(6) . . . . ? O7 Sb2 C7 C8 -117.7(18) 2_656 . . . ? O2 Sb2 C7 C8 128.5(6) . . . . ? O4 Sb2 C7 C8 -58.7(6) . . . . ? O5 Sb2 C7 C8 -146.6(6) . . . . ? C12 C7 C8 C9 -1.7(12) . . . . ? Sb2 C7 C8 C9 173.9(7) . . . . ? C7 C8 C9 C10 2.5(13) . . . . ? C8 C9 C10 C11 -1.1(14) . . . . ? C8 C9 C10 Cl2 -179.0(7) . . . . ? C9 C10 C11 C12 -0.9(14) . . . . ? Cl2 C10 C11 C12 177.0(7) . . . . ? O1 P1 C13 C14 -141.3(7) . . . . ? O10 P1 C13 C14 -21.9(8) 2_656 . . . ? O2 P1 C13 C14 95.8(8) . . . . ? C13A P1 C13 C14 138(4) . . . . ? O1 P1 C13 C18 36.1(7) . . . . ? O10 P1 C13 C18 155.5(6) 2_656 . . . ? O2 P1 C13 C18 -86.8(7) . . . . ? C13A P1 C13 C18 -44(3) . . . . ? C18 C13 C14 C15 0.0 . . . . ? P1 C13 C14 C15 177.3(10) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? P1 C13 C18 C17 -177.6(10) . . . . ? C10 C11 C12 C7 1.7(15) . . . . ? C8 C7 C12 C11 -0.4(13) . . . . ? Sb2 C7 C12 C11 -175.8(7) . . . . ? O1 P1 C13A C14A 149.4(7) . . . . ? O10 P1 C13A C14A -87.3(7) 2_656 . . . ? O2 P1 C13A C14A 31.3(8) . . . . ? C13 P1 C13A C14A -108(4) . . . . ? O1 P1 C13A C18A -34.6(8) . . . . ? O10 P1 C13A C18A 88.7(7) 2_656 . . . ? O2 P1 C13A C18A -152.7(6) . . . . ? C13 P1 C13A C18A 68(3) . . . . ? C18A C13A C14A C15A 0.0 . . . . ? P1 C13A C14A C15A 175.9(10) . . . . ? C13A C14A C15A C16A 0.0 . . . . ? C14A C15A C16A C17A 0.0 . . . . ? C15A C16A C17A C18A 0.0 . . . . ? C16A C17A C18A C13A 0.0 . . . . ? C14A C13A C18A C17A 0.0 . . . . ? P1 C13A C18A C17A -176.1(9) . . . . ? O9 P2 C19 C20 9.7(8) . . . . ? O8 P2 C19 C20 133.2(6) . . . . ? O5 P2 C19 C20 -111.2(6) 2_656 . . . ? O9 P2 C19 C24 -172.1(6) . . . . ? O8 P2 C19 C24 -48.6(7) . . . . ? O5 P2 C19 C24 67.0(7) 2_656 . . . ? C24 C19 C20 C21 -0.3(12) . . . . ? P2 C19 C20 C21 177.9(7) . . . . ? C19 C20 C21 C22 -0.2(13) . . . . ? C20 C21 C22 C23 0.1(14) . . . . ? C21 C22 C23 C24 0.7(14) . . . . ? C22 C23 C24 C19 -1.3(13) . . . . ? C20 C19 C24 C23 1.1(12) . . . . ? P2 C19 C24 C23 -177.2(7) . . . . ? O14 Sb3 C27 C28 -61.9(7) . . . . ? O16 Sb3 C27 C28 139.4(18) . . . . ? O20 Sb3 C27 C28 29.7(7) . . . . ? O17 Sb3 C27 C28 -155.4(7) . . . . ? O19 Sb3 C27 C28 117.8(7) . . . . ? O14 Sb3 C27 C32 117.9(6) . . . . ? O16 Sb3 C27 C32 -41(2) . . . . ? O20 Sb3 C27 C32 -150.6(6) . . . . ? O17 Sb3 C27 C32 24.4(6) . . . . ? O19 Sb3 C27 C32 -62.4(6) . . . . ? C32 C27 C28 C29 3.8(13) . . . . ? Sb3 C27 C28 C29 -176.4(7) . . . . ? C27 C28 C29 C30 -0.7(15) . . . . ? C28 C29 C30 C31 -2.3(16) . . . . ? C28 C29 C30 Cl3A -178.2(10) . . . . ? C28 C29 C30 Cl3 173.6(9) . . . . ? C29 C30 C31 C32 1.9(16) . . . . ? Cl3A C30 C31 C32 177.0(10) . . . . ? Cl3 C30 C31 C32 -174.7(9) . . . . ? C30 C31 C32 C27 1.4(14) . . . . ? C28 C27 C32 C31 -4.2(13) . . . . ? Sb3 C27 C32 C31 176.0(7) . . . . ? O14 Sb4 C33 C34 -38.2(6) . . . . ? O16 Sb4 C33 C34 -167.8(12) 2_755 . . . ? O13 Sb4 C33 C34 52.8(6) . . . . ? O11 Sb4 C33 C34 -133.3(6) . . . . ? O12 Sb4 C33 C34 137.8(6) . . . . ? O14 Sb4 C33 C38 130.7(5) . . . . ? O16 Sb4 C33 C38 1.0(18) 2_755 . . . ? O13 Sb4 C33 C38 -138.4(5) . . . . ? O11 Sb4 C33 C38 35.5(5) . . . . ? O12 Sb4 C33 C38 -53.4(5) . . . . ? C38 C33 C34 C35 1.2(12) . . . . ? Sb4 C33 C34 C35 169.8(6) . . . . ? C33 C34 C35 C36 0.4(13) . . . . ? C34 C35 C36 C37 -1.0(13) . . . . ? C34 C35 C36 Cl4 -178.3(7) . . . . ? C35 C36 C37 C38 0.2(12) . . . . ? Cl4 C36 C37 C38 177.4(6) . . . . ? C36 C37 C38 C33 1.4(11) . . . . ? C34 C33 C38 C37 -2.1(11) . . . . ? Sb4 C33 C38 C37 -171.2(6) . . . . ? O18 P3 C39 C44 -178.0(6) . . . . ? O19 P3 C39 C44 -54.9(7) . . . . ? O12 P3 C39 C44 61.1(7) 2_755 . . . ? O18 P3 C39 C40 3.0(7) . . . . ? O19 P3 C39 C40 126.1(6) . . . . ? O12 P3 C39 C40 -117.9(6) 2_755 . . . ? C44 C39 C40 C41 1.2(12) . . . . ? P3 C39 C40 C41 -179.7(6) . . . . ? C39 C40 C41 C42 -0.8(12) . . . . ? C40 C41 C42 C43 0.3(12) . . . . ? C41 C42 C43 C44 -0.2(12) . . . . ? C40 C39 C44 C43 -1.1(11) . . . . ? P3 C39 C44 C43 179.8(6) . . . . ? C42 C43 C44 C39 0.6(11) . . . . ? O15 P4 C45 C46 -144.6(7) 2_755 . . . ? O20 P4 C45 C46 95.2(7) . . . . ? O13 P4 C45 C46 -22.6(7) 2_755 . . . ? O15 P4 C45 C50 40.5(7) 2_755 . . . ? O20 P4 C45 C50 -79.6(6) . . . . ? O13 P4 C45 C50 162.6(6) 2_755 . . . ? C50 C45 C46 C47 -2.2(13) . . . . ? P4 C45 C46 C47 -177.1(8) . . . . ? C45 C46 C47 C48 2.8(16) . . . . ? C46 C47 C48 C49 -2.7(16) . . . . ? C47 C48 C49 C50 2.0(15) . . . . ? C48 C49 C50 C45 -1.4(14) . . . . ? C46 C45 C50 C49 1.4(12) . . . . ? P4 C45 C50 C49 176.4(7) . . . . ? O1 Co1 N1 C57 -150.7(12) . . . . ? O9 Co1 N1 C57 25.6(12) . . . . ? O4 Co1 N1 C57 111.8(11) 2_656 . . . ? O6 Co1 N1 C57 -58.3(12) . . . . ? O7 Co1 N1 C57 131.8(15) . . . . ? N1A Co1 N1 C57 -56(3) . . . . ? O1 Co1 N1 C53 31.5(10) . . . . ? O9 Co1 N1 C53 -152.2(10) . . . . ? O4 Co1 N1 C53 -66.1(10) 2_656 . . . ? O6 Co1 N1 C53 123.9(9) . . . . ? O7 Co1 N1 C53 -46(2) . . . . ? N1A Co1 N1 C53 127(3) . . . . ? C57 N1 C53 C54 4(2) . . . . ? Co1 N1 C53 C54 -177.7(10) . . . . ? N1 C53 C54 C55 -3(2) . . . . ? C53 C54 C55 C56 1(2) . . . . ? C53 C54 C55 C58 179.6(13) . . . . ? C54 C55 C56 C57 -0.6(19) . . . . ? C58 C55 C56 C57 -179.1(10) . . . . ? C53 N1 C57 C56 -4(2) . . . . ? Co1 N1 C57 C56 178.3(8) . . . . ? C55 C56 C57 N1 2.1(18) . . . . ? O1 Co1 N1A C53A -9.1(11) . . . . ? N1 Co1 N1A C53A -94(3) . . . . ? O9 Co1 N1A C53A 167.8(11) . . . . ? O4 Co1 N1A C53A -107.1(11) 2_656 . . . ? O6 Co1 N1A C53A 83.9(12) . . . . ? O7 Co1 N1A C53A 67(9) . . . . ? O1 Co1 N1A C57A 151.5(12) . . . . ? N1 Co1 N1A C57A 67(3) . . . . ? O9 Co1 N1A C57A -31.6(11) . . . . ? O4 Co1 N1A C57A 53.5(12) 2_656 . . . ? O6 Co1 N1A C57A -115.5(11) . . . . ? O7 Co1 N1A C57A -133(8) . . . . ? C57A N1A C53A C54A 0.0 . . . . ? Co1 N1A C53A C54A 160.3(15) . . . . ? N1A C53A C54A C55A 0.0 . . . . ? C53A C54A C55A C56A 0.0 . . . . ? C53A C54A C55A C58 -165(2) . . . . ? C54A C55A C56A C57A 0.0 . . . . ? C58 C55A C56A C57A 167.1(18) . . . . ? C55A C56A C57A N1A 0.0 . . . . ? C53A N1A C57A C56A 0.0 . . . . ? Co1 N1A C57A C56A -160.3(15) . . . . ? C54 C55 C58 C59 -21.7(19) . . . . ? C56 C55 C58 C59 156.6(11) . . . . ? C54 C55 C58 C55A -116(4) . . . . ? C56 C55 C58 C55A 62(4) . . . . ? C56A C55A C58 C59 -160.0(11) . . . . ? C54A C55A C58 C59 6(2) . . . . ? C56A C55A C58 C55 -64(4) . . . . ? C54A C55A C58 C55 102(4) . . . . ? C55 C58 C59 C62 167.3(10) . . . . ? C55A C58 C59 C62 -171.9(12) . . . . ? N2 C60 C61 C62 0.2(15) 2_765 . . . ? C60 C61 C62 C63 3.4(13) . . . . ? C60 C61 C62 C59 -177.5(8) . . . . ? C58 C59 C62 C61 -11.7(14) . . . . ? C58 C59 C62 C63 167.3(9) . . . . ? C61 C62 C63 C64 -3.4(13) . . . . ? C59 C62 C63 C64 177.5(9) . . . . ? C62 C63 C64 N2 -0.3(15) . . . 2_765 ? O10 P1 O1 Co1 53.1(7) 2_656 . . . ? O2 P1 O1 Co1 -75.1(7) . . . . ? C13A P1 O1 Co1 174.3(7) . . . . ? C13 P1 O1 Co1 163.8(7) . . . . ? N1 Co1 O1 P1 -159.9(7) . . . . ? O9 Co1 O1 P1 134(2) . . . . ? O4 Co1 O1 P1 -64.2(6) 2_656 . . . ? O6 Co1 O1 P1 83.6(6) . . . . ? O7 Co1 O1 P1 9.5(6) . . . . ? N1A Co1 O1 P1 -174.4(8) . . . . ? O1 P1 O2 Sb2 89.5(4) . . . . ? O10 P1 O2 Sb2 -40.1(5) 2_656 . . . ? C13A P1 O2 Sb2 -158.4(5) . . . . ? C13 P1 O2 Sb2 -151.3(5) . . . . ? O3 Sb2 O2 P1 -81.9(4) . . . . ? O7 Sb2 O2 P1 11.6(4) 2_656 . . . ? O4 Sb2 O2 P1 45.6(12) . . . . ? O5 Sb2 O2 P1 98.6(4) . . . . ? C7 Sb2 O2 P1 -175.2(4) . . . . ? O7 Sb1 O3 Sb2 -16.7(5) . . . . ? O6 Sb1 O3 Sb2 -97.7(5) . . . . ? O10 Sb1 O3 Sb2 72.7(5) . . . . ? O8 Sb1 O3 Sb2 171(6) . . . . ? C1 Sb1 O3 Sb2 166.4(5) . . . . ? O7 Sb2 O3 Sb1 -15.9(5) 2_656 . . . ? O2 Sb2 O3 Sb1 75.1(5) . . . . ? O4 Sb2 O3 Sb1 -96.2(5) . . . . ? O5 Sb2 O3 Sb1 104(12) . . . . ? C7 Sb2 O3 Sb1 167.6(5) . . . . ? O3 Sb2 O4 C25 -121.5(5) . . . . ? O7 Sb2 O4 C25 145.5(6) 2_656 . . . ? O2 Sb2 O4 C25 110.9(11) . . . . ? O5 Sb2 O4 C25 58.2(5) . . . . ? C7 Sb2 O4 C25 -28.0(6) . . . . ? O3 Sb2 O4 Co1 105.3(2) . . . 2_656 ? O7 Sb2 O4 Co1 12.28(19) 2_656 . . 2_656 ? O2 Sb2 O4 Co1 -22.4(11) . . . 2_656 ? O5 Sb2 O4 Co1 -75.0(2) . . . 2_656 ? C7 Sb2 O4 Co1 -161.3(3) . . . 2_656 ? O3 Sb2 O5 P2 -138(12) . . . 2_656 ? O7 Sb2 O5 P2 -18.5(3) 2_656 . . 2_656 ? O2 Sb2 O5 P2 -109.6(3) . . . 2_656 ? O4 Sb2 O5 P2 61.7(3) . . . 2_656 ? C7 Sb2 O5 P2 157.9(4) . . . 2_656 ? O3 Sb1 O6 C26 -35.4(5) . . . . ? O7 Sb1 O6 C26 -129.6(5) . . . . ? O10 Sb1 O6 C26 -160.7(9) . . . . ? O8 Sb1 O6 C26 142.8(5) . . . . ? C1 Sb1 O6 C26 56.5(5) . . . . ? O3 Sb1 O6 Co1 104.6(2) . . . . ? O7 Sb1 O6 Co1 10.32(19) . . . . ? O10 Sb1 O6 Co1 -20.7(10) . . . . ? O8 Sb1 O6 Co1 -77.3(2) . . . . ? C1 Sb1 O6 Co1 -163.5(2) . . . . ? O1 Co1 O6 C26 40.7(5) . . . . ? N1 Co1 O6 C26 -48.7(6) . . . . ? O9 Co1 O6 C26 -136.2(5) . . . . ? O4 Co1 O6 C26 149.3(5) 2_656 . . . ? O7 Co1 O6 C26 129.4(5) . . . . ? N1A Co1 O6 C26 -49.4(7) . . . . ? O1 Co1 O6 Sb1 -98.4(2) . . . . ? N1 Co1 O6 Sb1 172.3(3) . . . . ? O9 Co1 O6 Sb1 84.7(2) . . . . ? O4 Co1 O6 Sb1 10.3(4) 2_656 . . . ? O7 Co1 O6 Sb1 -9.68(18) . . . . ? N1A Co1 O6 Sb1 171.6(6) . . . . ? O3 Sb1 O7 Sb2 130.9(4) . . . 2_656 ? O6 Sb1 O7 Sb2 -135.9(4) . . . 2_656 ? O10 Sb1 O7 Sb2 38.1(4) . . . 2_656 ? O8 Sb1 O7 Sb2 -49.4(4) . . . 2_656 ? C1 Sb1 O7 Sb2 -75.0(18) . . . 2_656 ? O3 Sb1 O7 Co1 -103.6(2) . . . . ? O6 Sb1 O7 Co1 -10.32(19) . . . . ? O10 Sb1 O7 Co1 163.7(2) . . . . ? O8 Sb1 O7 Co1 76.18(19) . . . . ? C1 Sb1 O7 Co1 50.5(18) . . . . ? O1 Co1 O7 Sb1 103.3(2) . . . . ? N1 Co1 O7 Sb1 -179.3(17) . . . . ? O9 Co1 O7 Sb1 -73.4(2) . . . . ? O4 Co1 O7 Sb1 -158.6(2) 2_656 . . . ? O6 Co1 O7 Sb1 10.01(18) . . . . ? N1A Co1 O7 Sb1 28(8) . . . . ? O1 Co1 O7 Sb2 -110.1(2) . . . 2_656 ? N1 Co1 O7 Sb2 -32.7(18) . . . 2_656 ? O9 Co1 O7 Sb2 73.2(2) . . . 2_656 ? O4 Co1 O7 Sb2 -11.94(18) 2_656 . . 2_656 ? O6 Co1 O7 Sb2 156.7(2) . . . 2_656 ? N1A Co1 O7 Sb2 174(8) . . . 2_656 ? O9 P2 O8 Sb1 -57.1(4) . . . . ? O5 P2 O8 Sb1 68.1(4) 2_656 . . . ? C19 P2 O8 Sb1 -179.7(3) . . . . ? O3 Sb1 O8 P2 155(6) . . . . ? O7 Sb1 O8 P2 -17.7(3) . . . . ? O6 Sb1 O8 P2 63.2(3) . . . . ? O10 Sb1 O8 P2 -107.1(3) . . . . ? C1 Sb1 O8 P2 159.2(4) . . . . ? O8 P2 O9 Co1 61.9(4) . . . . ? O5 P2 O9 Co1 -61.6(4) 2_656 . . . ? C19 P2 O9 Co1 -177.5(3) . . . . ? O1 Co1 O9 P2 -124(3) . . . . ? N1 Co1 O9 P2 169.9(4) . . . . ? O4 Co1 O9 P2 74.0(3) 2_656 . . . ? O6 Co1 O9 P2 -73.5(3) . . . . ? O7 Co1 O9 P2 0.2(3) . . . . ? N1A Co1 O9 P2 -175.8(7) . . . . ? O3 Sb1 O10 P1 -89.2(4) . . . 2_656 ? O7 Sb1 O10 P1 5.6(4) . . . 2_656 ? O6 Sb1 O10 P1 36.1(12) . . . 2_656 ? O8 Sb1 O10 P1 92.6(4) . . . 2_656 ? C1 Sb1 O10 P1 179.1(4) . . . 2_656 ? O14 Sb4 O11 C51 -38.4(5) . . . . ? O16 Sb4 O11 C51 -133.6(5) 2_755 . . . ? O13 Sb4 O11 C51 -160.0(8) . . . . ? O12 Sb4 O11 C51 139.4(5) . . . . ? C33 Sb4 O11 C51 51.6(5) . . . . ? O14 Sb4 O11 Co2 108.1(2) . . . 2_755 ? O16 Sb4 O11 Co2 12.94(18) 2_755 . . 2_755 ? O13 Sb4 O11 Co2 -13.5(10) . . . 2_755 ? O12 Sb4 O11 Co2 -74.0(2) . . . 2_755 ? C33 Sb4 O11 Co2 -161.9(2) . . . 2_755 ? O14 Sb4 O12 P3 -146(2) . . . 2_755 ? O16 Sb4 O12 P3 -18.1(3) 2_755 . . 2_755 ? O13 Sb4 O12 P3 -108.5(3) . . . 2_755 ? O11 Sb4 O12 P3 61.4(3) . . . 2_755 ? C33 Sb4 O12 P3 154.6(3) . . . 2_755 ? O14 Sb4 O13 P4 -87.0(4) . . . 2_755 ? O16 Sb4 O13 P4 9.0(4) 2_755 . . 2_755 ? O11 Sb4 O13 P4 34.9(12) . . . 2_755 ? O12 Sb4 O13 P4 95.8(4) . . . 2_755 ? C33 Sb4 O13 P4 -176.9(4) . . . 2_755 ? O16 Sb3 O14 Sb4 -22.7(4) . . . . ? O20 Sb3 O14 Sb4 67.3(4) . . . . ? O17 Sb3 O14 Sb4 -103.2(4) . . . . ? O19 Sb3 O14 Sb4 129(20) . . . . ? C27 Sb3 O14 Sb4 159.9(5) . . . . ? O16 Sb4 O14 Sb3 -10.3(5) 2_755 . . . ? O13 Sb4 O14 Sb3 79.9(4) . . . . ? O11 Sb4 O14 Sb3 -90.2(4) . . . . ? O12 Sb4 O14 Sb3 117(2) . . . . ? C33 Sb4 O14 Sb3 176.7(5) . . . . ? O17 Co2 O15 P4 77.3(6) . . . 2_755 ? N2 Co2 O15 P4 -179.1(6) . . . 2_755 ? O18 Co2 O15 P4 -128(5) . . . 2_755 ? O11 Co2 O15 P4 -70.0(6) 2_755 . . 2_755 ? O16 Co2 O15 P4 3.2(6) . . . 2_755 ? O14 Sb3 O16 Sb4 130.3(4) . . . 2_755 ? O20 Sb3 O16 Sb4 38.8(4) . . . 2_755 ? O17 Sb3 O16 Sb4 -137.3(4) . . . 2_755 ? O19 Sb3 O16 Sb4 -49.5(4) . . . 2_755 ? C27 Sb3 O16 Sb4 -71(2) . . . 2_755 ? O14 Sb3 O16 Co2 -103.2(2) . . . . ? O20 Sb3 O16 Co2 165.3(2) . . . . ? O17 Sb3 O16 Co2 -10.78(19) . . . . ? O19 Sb3 O16 Co2 77.1(2) . . . . ? C27 Sb3 O16 Co2 55(2) . . . . ? O15 Co2 O16 Sb3 106.0(2) . . . . ? O17 Co2 O16 Sb3 10.69(19) . . . . ? N2 Co2 O16 Sb3 44(5) . . . . ? O18 Co2 O16 Sb3 -75.6(2) . . . . ? O11 Co2 O16 Sb3 -160.2(2) 2_755 . . . ? O15 Co2 O16 Sb4 -106.3(2) . . . 2_755 ? O17 Co2 O16 Sb4 158.3(2) . . . 2_755 ? N2 Co2 O16 Sb4 -168(4) . . . 2_755 ? O18 Co2 O16 Sb4 72.1(2) . . . 2_755 ? O11 Co2 O16 Sb4 -12.53(18) 2_755 . . 2_755 ? O14 Sb3 O17 C52 -35.5(5) . . . . ? O16 Sb3 O17 C52 -129.4(5) . . . . ? O20 Sb3 O17 C52 -151.2(9) . . . . ? O19 Sb3 O17 C52 144.0(5) . . . . ? C27 Sb3 O17 C52 57.3(6) . . . . ? O14 Sb3 O17 Co2 104.9(2) . . . . ? O16 Sb3 O17 Co2 11.08(19) . . . . ? O20 Sb3 O17 Co2 -10.7(11) . . . . ? O19 Sb3 O17 Co2 -75.5(2) . . . . ? C27 Sb3 O17 Co2 -162.3(2) . . . . ? O15 Co2 O17 C52 41.4(5) . . . . ? N2 Co2 O17 C52 -49.1(5) . . . . ? O18 Co2 O17 C52 -137.7(5) . . . . ? O11 Co2 O17 C52 145.3(5) 2_755 . . . ? O16 Co2 O17 C52 129.4(5) . . . . ? O15 Co2 O17 Sb3 -98.3(2) . . . . ? N2 Co2 O17 Sb3 171.2(2) . . . . ? O18 Co2 O17 Sb3 82.6(2) . . . . ? O11 Co2 O17 Sb3 5.7(4) 2_755 . . . ? O16 Co2 O17 Sb3 -10.26(18) . . . . ? O19 P3 O18 Co2 59.7(3) . . . . ? O12 P3 O18 Co2 -64.0(3) 2_755 . . . ? C39 P3 O18 Co2 178.7(3) . . . . ? O15 Co2 O18 P3 133(5) . . . . ? O17 Co2 O18 P3 -71.8(3) . . . . ? N2 Co2 O18 P3 -175.5(3) . . . . ? O11 Co2 O18 P3 75.3(3) 2_755 . . . ? O16 Co2 O18 P3 2.3(3) . . . . ? O18 P3 O19 Sb3 -56.6(4) . . . . ? O12 P3 O19 Sb3 68.0(4) 2_755 . . . ? C39 P3 O19 Sb3 -179.0(3) . . . . ? O14 Sb3 O19 P3 -169(62) . . . . ? O16 Sb3 O19 P3 -17.8(3) . . . . ? O20 Sb3 O19 P3 -107.8(3) . . . . ? O17 Sb3 O19 P3 62.6(3) . . . . ? C27 Sb3 O19 P3 159.6(4) . . . . ? O15 P4 O20 Sb3 100.2(4) 2_755 . . . ? O13 P4 O20 Sb3 -27.2(5) 2_755 . . . ? C45 P4 O20 Sb3 -141.5(4) . . . . ? O14 Sb3 O20 P4 -94.3(4) . . . . ? O16 Sb3 O20 P4 0.0(4) . . . . ? O17 Sb3 O20 P4 21.4(13) . . . . ? O19 Sb3 O20 P4 86.2(4) . . . . ? C27 Sb3 O20 P4 173.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 2.937 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.161 # Attachment '- 13.cif' data_orepw844p43212 _database_code_depnum_ccdc_archive 'CCDC 700897' #TrackingRef '- 13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H82 Cl5 Co4 N8 O27 P6 Sb5' _chemical_formula_weight 2963.22 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' Cl Cl 0.1484 0.1585 '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' 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' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+3/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+1/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' _cell_length_a 16.8698(7) _cell_length_b 16.8698(7) _cell_length_c 40.0183(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11388.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22749 _cell_measurement_theta_min 2.7133 _cell_measurement_theta_max 27.5902 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5824 _exptl_absorpt_coefficient_mu 2.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5006 _exptl_absorpt_correction_T_max 0.6896 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102156 _diffrn_reflns_av_R_equivalents 0.1096 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 26.43 _reflns_number_total 11687 _reflns_number_gt 11544 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Three residual Q-peaks could not be solved due to centro-symmetric solvent disorder. O8 & O12 were left as isotropic due to NPDs.Making them anisotropic results in NPDs that might be because of twinning of crystal or data integration problem. 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^)+(0.0000P)^2^+454.8685P] 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 constr _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 0.13(5) _refine_ls_number_reflns 11687 _refine_ls_number_parameters 655 _refine_ls_number_restraints 339 _refine_ls_R_factor_all 0.1087 _refine_ls_R_factor_gt 0.1080 _refine_ls_wR_factor_ref 0.2123 _refine_ls_wR_factor_gt 0.2119 _refine_ls_goodness_of_fit_ref 1.292 _refine_ls_restrained_S_all 1.273 _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 Sb1 Sb 0.14947(6) 0.12639(5) 0.21599(2) 0.0110(2) Uani 1 1 d . . . Sb2 Sb 0.14943(6) 0.11676(5) 0.29078(2) 0.0121(2) Uani 1 1 d . . . Sb3 Sb 0.00650(5) -0.00650(5) 0.2500 0.0098(2) Uani 1 2 d S . . P1 P 0.2622(2) -0.0087(2) 0.18411(9) 0.0154(8) Uani 1 1 d . . . P2 P 0.2622(2) -0.0278(2) 0.31713(9) 0.0155(8) Uani 1 1 d . . . P3 P 0.2874(2) 0.2151(2) 0.25546(9) 0.0172(8) Uani 1 1 d . . . Co1 Co 0.08818(12) -0.08189(12) 0.19325(4) 0.0119(4) Uani 1 1 d . . . Co2 Co 0.34199(12) 0.04310(12) 0.25148(5) 0.0177(4) Uani 1 1 d . . . N1 N 0.0541(8) -0.0517(8) 0.1443(3) 0.017(2) Uani 1 1 d . . . N2 N 0.0588(16) 0.178(2) 0.0478(8) 0.102(11) Uani 1 1 d . . . N3 N 0.3196(11) 0.2737(17) 0.1096(4) 0.071(8) Uani 1 1 d . . . N4 N 0.4661(7) 0.0246(8) 0.2520(3) 0.020(3) Uani 1 1 d . . . C1 C 0.1033(12) 0.1992(11) 0.1787(4) 0.0291(16) Uani 1 1 d U . . C2 C 0.1541(12) 0.2191(11) 0.1516(4) 0.0293(16) Uani 1 1 d U . . H2 H 0.2051 0.1957 0.1498 0.035 Uiso 1 1 calc R . . C3 C 0.1279(12) 0.2737(11) 0.1274(4) 0.0294(16) Uani 1 1 d U . . H3 H 0.1602 0.2852 0.1086 0.035 Uiso 1 1 calc R . . C4 C 0.0565(12) 0.3098(11) 0.1310(4) 0.0294(16) Uani 1 1 d U . . C5 C 0.0068(12) 0.2893(11) 0.1578(4) 0.0294(16) Uani 1 1 d U . . H5 H -0.0444 0.3123 0.1594 0.035 Uiso 1 1 calc R . . C6 C 0.0319(12) 0.2356(11) 0.1818(4) 0.0292(16) Uani 1 1 d U . . H6 H -0.0010 0.2243 0.2005 0.035 Uiso 1 1 calc R . . C7 C 0.0965(7) 0.1739(7) 0.33122(18) 0.0261(16) Uani 1 1 d GU . . C8 C 0.0298(7) 0.2205(7) 0.32586(16) 0.0263(16) Uani 1 1 d GU . . H8 H 0.0103 0.2282 0.3038 0.032 Uiso 1 1 calc R . . C9 C -0.0085(6) 0.2559(7) 0.3527(2) 0.0265(16) Uani 1 1 d GU . . H9 H -0.0542 0.2878 0.3491 0.032 Uiso 1 1 calc R . . C10 C 0.0199(7) 0.2447(7) 0.38500(18) 0.0265(16) Uani 1 1 d GU . . C11 C 0.0867(7) 0.1981(7) 0.39037(16) 0.0263(16) Uani 1 1 d GU . . H11 H 0.1061 0.1905 0.4124 0.032 Uiso 1 1 calc R . . C12 C 0.1250(6) 0.1627(7) 0.3635(2) 0.0262(16) Uani 1 1 d GU . . H12 H 0.1706 0.1309 0.3671 0.031 Uiso 1 1 calc R . . C13 C -0.0817(9) 0.0817(9) 0.2500 0.029(2) Uani 1 2 d SU . . C14 C -0.1140(11) 0.1080(11) 0.2194(4) 0.029(2) Uani 1 1 d U . . H14 H -0.0961 0.0854 0.1990 0.035 Uiso 1 1 calc R . . C15 C -0.1708(11) 0.1659(11) 0.2190(4) 0.029(2) Uani 1 1 d U . . H15 H -0.1918 0.1844 0.1984 0.035 Uiso 1 1 calc R . . C16 C -0.1983(10) 0.1983(10) 0.2500 0.030(2) Uani 1 2 d SU . . C17 C 0.2943(11) -0.0251(12) 0.1419(4) 0.0295(17) Uani 1 1 d U . . C18 C 0.3404(12) 0.0299(12) 0.1252(4) 0.0297(17) Uani 1 1 d U . . H18 H 0.3586 0.0760 0.1365 0.036 Uiso 1 1 calc R . . C19 C 0.3602(11) 0.0177(12) 0.0920(4) 0.0299(17) Uani 1 1 d U . . H19 H 0.3940 0.0544 0.0810 0.036 Uiso 1 1 calc R . . C20 C 0.3321(11) -0.0453(11) 0.0750(4) 0.0299(17) Uani 1 1 d U . . H20 H 0.3454 -0.0512 0.0521 0.036 Uiso 1 1 calc R . . C21 C 0.2862(11) -0.0996(12) 0.0896(4) 0.0297(17) Uani 1 1 d U . . H21 H 0.2660 -0.1432 0.0772 0.036 Uiso 1 1 calc R . . C22 C 0.2684(11) -0.0906(12) 0.1240(4) 0.0296(17) Uani 1 1 d U . . H22 H 0.2381 -0.1302 0.1350 0.036 Uiso 1 1 calc R . . C23 C 0.3072(11) -0.0423(12) 0.3579(4) 0.0282(16) Uani 1 1 d U . . C24 C 0.3022(11) -0.1179(12) 0.3732(4) 0.0282(16) Uani 1 1 d U . . H24 H 0.2784 -0.1610 0.3617 0.034 Uiso 1 1 calc R . . C25 C 0.3328(10) -0.1284(11) 0.4055(4) 0.0283(16) Uani 1 1 d U . . H25 H 0.3269 -0.1775 0.4168 0.034 Uiso 1 1 calc R . . C26 C 0.3718(11) -0.0654(11) 0.4206(4) 0.0283(16) Uani 1 1 d U . . H26 H 0.3931 -0.0722 0.4424 0.034 Uiso 1 1 calc R . . C27 C 0.3805(11) 0.0059(11) 0.4051(4) 0.0284(16) Uani 1 1 d U . . H27 H 0.4090 0.0476 0.4155 0.034 Uiso 1 1 calc R . . C28 C 0.3464(11) 0.0170(11) 0.3730(4) 0.0283(16) Uani 1 1 d U . . H28 H 0.3513 0.0669 0.3622 0.034 Uiso 1 1 calc R . . C29 C 0.3200(15) 0.3153(12) 0.2561(5) 0.048(2) Uani 1 1 d U . . C30 C 0.3975(14) 0.3378(11) 0.2508(5) 0.048(2) Uani 1 1 d U . . H30 H 0.4375 0.2986 0.2484 0.057 Uiso 1 1 calc R . . C31 C 0.4175(15) 0.4184(12) 0.2491(5) 0.048(2) Uani 1 1 d U . . H31 H 0.4712 0.4339 0.2461 0.057 Uiso 1 1 calc R . . C32 C 0.3596(14) 0.4744(12) 0.2518(5) 0.048(2) Uani 1 1 d U . . H32 H 0.3732 0.5290 0.2507 0.057 Uiso 1 1 calc R . . C33 C 0.2810(15) 0.4525(12) 0.2562(5) 0.048(2) Uani 1 1 d U . . H33 H 0.2405 0.4916 0.2571 0.057 Uiso 1 1 calc R . . C34 C 0.2629(16) 0.3759(12) 0.2591(5) 0.048(2) Uani 1 1 d U . . H34 H 0.2094 0.3616 0.2634 0.057 Uiso 1 1 calc R . . C35 C 0.0133(12) 0.0166(12) 0.1393(4) 0.0347(19) Uani 1 1 d U . . H35 H 0.0051 0.0511 0.1577 0.042 Uiso 1 1 calc R . . C36 C -0.0163(12) 0.0375(12) 0.1088(4) 0.0349(19) Uani 1 1 d U . . H36 H -0.0426 0.0867 0.1057 0.042 Uiso 1 1 calc R . . C37 C -0.0072(12) -0.0142(11) 0.0828(4) 0.0350(19) Uani 1 1 d U . . H37 H -0.0291 -0.0024 0.0615 0.042 Uiso 1 1 calc R . . C38 C 0.0344(12) -0.0844(12) 0.0878(5) 0.0348(19) Uani 1 1 d U . . H38 H 0.0428 -0.1208 0.0700 0.042 Uiso 1 1 calc R . . C39 C 0.0622(12) -0.0990(12) 0.1186(4) 0.0347(19) Uani 1 1 d U . . H39 H 0.0900 -0.1473 0.1220 0.042 Uiso 1 1 calc R . . C40 C 0.5017(12) -0.0323(13) 0.2714(5) 0.035(2) Uani 1 1 d U . . H40 H 0.4685 -0.0641 0.2851 0.042 Uiso 1 1 calc R . . C41 C 0.5836(12) -0.0468(13) 0.2725(5) 0.035(2) Uani 1 1 d U . . H41 H 0.6058 -0.0868 0.2863 0.042 Uiso 1 1 calc R . . C42 C 0.6301(11) 0.0008(12) 0.2522(5) 0.035(2) Uani 1 1 d U . . H42 H 0.6861 -0.0053 0.2521 0.042 Uiso 1 1 calc R . . C43 C 0.5952(12) 0.0564(13) 0.2322(5) 0.035(2) Uani 1 1 d U . . H43 H 0.6258 0.0864 0.2168 0.042 Uiso 1 1 calc R . . C44 C 0.5136(12) 0.0680(13) 0.2350(5) 0.035(2) Uani 1 1 d U . . H44 H 0.4914 0.1118 0.2234 0.042 Uiso 1 1 calc R . . C45 C 0.3699(14) 0.2768(18) 0.1709(5) 0.060(5) Uani 1 1 d U . . H45A H 0.3319 0.2478 0.1848 0.091 Uiso 1 1 calc R . . H45B H 0.3741 0.3316 0.1788 0.091 Uiso 1 1 calc R . . H45C H 0.4219 0.2511 0.1723 0.091 Uiso 1 1 calc R . . C46 C 0.3429(15) 0.2765(18) 0.1364(5) 0.060(5) Uani 1 1 d U . . C47 C 0.1798(18) 0.103(2) 0.0711(9) 0.084(7) Uani 1 1 d U . . H47A H 0.1988 0.0674 0.0533 0.126 Uiso 1 1 calc R . . H47B H 0.1662 0.0710 0.0909 0.126 Uiso 1 1 calc R . . H47C H 0.2215 0.1406 0.0769 0.126 Uiso 1 1 calc R . . C48 C 0.1122(18) 0.144(2) 0.0600(9) 0.084(7) Uani 1 1 d U . . O1 O 0.2063(6) -0.0746(6) 0.1934(3) 0.016(2) Uani 1 1 d . . . O2 O 0.2204(7) 0.0738(7) 0.1820(2) 0.019(2) Uani 1 1 d . . . O3 O 0.3347(6) -0.0041(7) 0.2065(3) 0.018(2) Uani 1 1 d . . . O4 O 0.3575(6) 0.1599(6) 0.2536(3) 0.023(2) Uani 1 1 d . . . O5 O 0.2369(6) 0.2101(6) 0.2233(2) 0.015(2) Uani 1 1 d . . . O6 O 0.2361(6) 0.2041(6) 0.2873(2) 0.018(2) Uani 1 1 d . . . O7 O 0.0712(6) 0.0394(6) 0.2128(2) 0.016(2) Uani 1 1 d . . . O8 O 0.2071(6) 0.0687(5) 0.2522(3) 0.0132(19) Uiso 1 1 d . . . O9 O 0.0916(6) 0.1712(6) 0.2548(2) 0.016(2) Uani 1 1 d . . . O10 O 0.0701(6) 0.0298(6) 0.2892(2) 0.010(2) Uani 1 1 d . . . O11 O 0.3264(7) -0.0241(7) 0.2914(3) 0.022(3) Uani 1 1 d . . . O12 O 0.2216(6) 0.0551(6) 0.3216(3) 0.017(2) Uiso 1 1 d . . . O13 O 0.2025(7) -0.0920(7) 0.3116(3) 0.025(3) Uani 1 1 d . . . O14 O 0.0931(6) -0.0931(6) 0.2500 0.019(3) Uani 1 2 d S . . Cl1 Cl 0.0263(3) 0.3809(4) 0.10234(15) 0.0550(16) Uani 1 1 d . . . Cl2 Cl -0.2698(3) 0.2698(3) 0.2500 0.095(4) Uani 1 2 d S . . Cl3 Cl -0.0295(5) 0.2877(5) 0.41831(14) 0.068(2) Uani 1 1 d . . . 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 Sb1 0.0173(5) 0.0104(4) 0.0054(4) -0.0019(3) 0.0004(3) -0.0038(4) Sb2 0.0172(5) 0.0130(4) 0.0060(4) 0.0005(3) -0.0005(4) -0.0047(4) Sb3 0.0112(4) 0.0112(4) 0.0071(5) 0.0005(3) 0.0005(3) -0.0020(4) P1 0.018(2) 0.018(2) 0.0100(16) -0.0048(15) 0.0022(14) -0.0058(16) P2 0.0152(19) 0.019(2) 0.0126(17) -0.0014(15) -0.0029(15) 0.0006(16) P3 0.024(2) 0.019(2) 0.0085(17) -0.0021(15) -0.0009(15) -0.0104(15) Co1 0.0141(10) 0.0149(10) 0.0069(8) -0.0015(7) -0.0004(7) -0.0011(7) Co2 0.0163(10) 0.0247(10) 0.0122(9) -0.0005(9) -0.0018(9) -0.0031(8) N1 0.023(7) 0.016(7) 0.013(6) -0.008(5) -0.006(5) -0.001(5) N2 0.058(16) 0.16(3) 0.09(2) 0.03(2) -0.012(15) 0.013(18) N3 0.035(11) 0.16(3) 0.018(8) 0.020(12) -0.008(8) 0.008(13) N4 0.020(6) 0.035(8) 0.005(5) -0.004(6) 0.001(5) -0.003(5) C1 0.041(4) 0.032(4) 0.015(3) 0.008(3) -0.001(3) 0.000(3) C2 0.041(4) 0.032(4) 0.015(3) 0.008(3) -0.001(3) 0.000(3) C3 0.041(4) 0.032(4) 0.015(3) 0.008(3) -0.001(3) 0.000(3) C4 0.041(4) 0.032(4) 0.015(3) 0.008(3) -0.001(3) 0.000(3) C5 0.041(4) 0.032(4) 0.015(3) 0.008(3) -0.001(3) 0.000(3) C6 0.041(4) 0.032(4) 0.015(3) 0.008(3) -0.001(3) 0.000(3) C7 0.039(4) 0.036(4) 0.003(3) -0.002(3) 0.008(3) 0.000(3) C8 0.039(4) 0.036(4) 0.004(3) -0.002(3) 0.008(3) 0.000(3) C9 0.040(4) 0.036(4) 0.004(3) -0.002(3) 0.008(3) 0.000(3) C10 0.040(4) 0.036(4) 0.004(3) -0.002(3) 0.008(3) 0.000(3) C11 0.040(4) 0.036(4) 0.003(3) -0.002(3) 0.008(3) 0.000(3) C12 0.039(4) 0.036(4) 0.003(3) -0.002(3) 0.008(3) 0.000(3) C13 0.028(3) 0.028(3) 0.030(5) 0.002(3) 0.002(3) 0.007(4) C14 0.029(3) 0.029(3) 0.030(5) 0.003(3) 0.002(3) 0.007(4) C15 0.029(3) 0.029(3) 0.030(5) 0.003(3) 0.002(3) 0.007(4) C16 0.029(3) 0.029(3) 0.031(5) 0.002(3) 0.002(3) 0.008(4) C17 0.032(4) 0.039(4) 0.018(3) -0.010(3) 0.003(3) 0.004(3) C18 0.032(4) 0.040(4) 0.018(3) -0.010(3) 0.003(3) 0.004(3) C19 0.032(4) 0.040(4) 0.018(3) -0.010(3) 0.003(3) 0.004(3) C20 0.032(4) 0.040(4) 0.018(3) -0.010(3) 0.003(3) 0.004(3) C21 0.032(4) 0.040(4) 0.018(3) -0.011(3) 0.003(3) 0.004(3) C22 0.032(4) 0.040(4) 0.018(3) -0.010(3) 0.003(3) 0.004(3) C23 0.030(4) 0.034(4) 0.021(3) 0.001(3) -0.010(3) -0.003(3) C24 0.029(4) 0.034(4) 0.021(3) 0.001(3) -0.010(3) -0.003(3) C25 0.030(4) 0.034(4) 0.021(3) 0.001(3) -0.010(3) -0.003(3) C26 0.030(4) 0.034(4) 0.021(3) 0.001(3) -0.010(3) -0.003(3) C27 0.030(4) 0.034(4) 0.021(3) 0.001(3) -0.010(3) -0.003(3) C28 0.030(4) 0.034(4) 0.021(3) 0.001(3) -0.010(3) -0.003(3) C29 0.083(6) 0.033(4) 0.028(3) -0.002(4) -0.005(4) -0.032(4) C30 0.083(6) 0.033(4) 0.028(3) -0.002(4) -0.005(4) -0.032(4) C31 0.083(6) 0.033(4) 0.028(3) -0.002(4) -0.005(4) -0.032(4) C32 0.083(6) 0.033(4) 0.028(3) -0.002(4) -0.005(4) -0.032(4) C33 0.083(6) 0.033(4) 0.028(3) -0.002(4) -0.005(4) -0.032(4) C34 0.083(6) 0.033(4) 0.028(3) -0.002(4) -0.006(4) -0.032(4) C35 0.048(5) 0.035(5) 0.022(3) 0.001(3) -0.007(4) -0.002(4) C36 0.048(5) 0.035(5) 0.022(3) 0.001(3) -0.007(4) -0.002(4) C37 0.048(5) 0.035(5) 0.022(3) 0.001(3) -0.007(4) -0.002(4) C38 0.048(5) 0.035(5) 0.021(3) 0.001(3) -0.007(4) -0.003(4) C39 0.048(5) 0.035(5) 0.021(4) 0.001(3) -0.007(4) -0.003(4) C40 0.028(4) 0.051(6) 0.025(4) -0.009(4) -0.004(4) 0.003(4) C41 0.028(4) 0.051(5) 0.025(4) -0.009(4) -0.004(4) 0.003(4) C42 0.028(4) 0.051(5) 0.026(4) -0.009(4) -0.004(3) 0.003(4) C43 0.028(4) 0.051(5) 0.026(4) -0.008(4) -0.004(4) 0.003(4) C44 0.029(4) 0.052(6) 0.026(4) -0.008(4) -0.004(4) 0.003(4) C45 0.042(9) 0.112(14) 0.027(8) 0.015(9) 0.008(7) -0.032(10) C46 0.042(9) 0.112(14) 0.027(8) 0.015(9) 0.007(7) -0.032(10) C47 0.061(12) 0.082(15) 0.109(16) 0.033(13) -0.005(12) 0.008(11) C48 0.061(12) 0.082(15) 0.109(16) 0.033(13) -0.005(12) 0.008(11) O1 0.011(5) 0.016(6) 0.020(5) 0.000(4) 0.000(4) 0.003(4) O2 0.020(6) 0.032(7) 0.006(5) -0.005(4) 0.003(4) -0.005(5) O3 0.012(5) 0.030(6) 0.012(5) -0.002(5) 0.004(4) -0.007(5) O4 0.030(6) 0.026(6) 0.014(5) -0.011(5) 0.004(5) -0.012(5) O5 0.016(5) 0.022(6) 0.008(4) 0.001(4) -0.001(4) -0.012(4) O6 0.019(6) 0.023(6) 0.012(5) -0.009(4) 0.002(4) -0.006(4) O7 0.023(6) 0.017(5) 0.009(5) -0.004(4) 0.012(4) -0.011(4) O9 0.024(6) 0.022(5) 0.002(4) 0.001(4) 0.004(4) -0.001(4) O10 0.012(5) 0.011(5) 0.007(4) 0.002(4) 0.005(4) -0.004(4) O11 0.024(6) 0.030(6) 0.013(5) 0.014(5) 0.000(5) -0.002(5) O13 0.020(6) 0.021(6) 0.035(7) 0.010(5) -0.013(5) 0.000(5) O14 0.024(5) 0.024(5) 0.008(6) -0.001(5) -0.001(5) 0.008(6) Cl1 0.047(3) 0.072(4) 0.046(3) 0.038(3) 0.004(2) 0.019(3) Cl2 0.098(6) 0.098(6) 0.089(7) 0.026(7) 0.026(7) 0.086(7) Cl3 0.084(5) 0.086(5) 0.035(3) -0.026(3) 0.024(3) 0.023(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 Sb1 O7 1.977(10) . ? Sb1 O9 1.984(9) . ? Sb1 O8 2.000(10) . ? Sb1 O2 2.017(11) . ? Sb1 O5 2.063(9) . ? Sb1 C1 2.086(17) . ? Sb1 Sb2 2.9975(11) . ? Sb2 O9 1.966(10) . ? Sb2 O10 1.986(9) . ? Sb2 O8 1.997(10) . ? Sb2 O12 2.021(11) . ? Sb2 O6 2.080(10) . ? Sb2 C7 2.085(6) . ? Sb3 O10 1.998(10) . ? Sb3 O10 1.998(10) 8 ? Sb3 O7 2.002(9) . ? Sb3 O7 2.002(9) 8 ? Sb3 O14 2.067(14) . ? Sb3 C13 2.11(2) . ? Sb3 Co1 2.9452(19) 8 ? Sb3 Co1 2.9452(19) . ? P1 O1 1.504(11) . ? P1 O3 1.518(11) . ? P1 O2 1.562(13) . ? P1 C17 1.794(17) . ? P2 O11 1.494(12) . ? P2 O13 1.495(12) . ? P2 O12 1.568(11) . ? P2 C23 1.815(17) . ? P3 O4 1.507(12) . ? P3 O5 1.545(10) . ? P3 O6 1.553(11) . ? P3 C29 1.778(18) . ? Co1 O1 1.996(11) . ? Co1 O13 2.046(12) 8 ? Co1 N1 2.105(12) . ? Co1 O10 2.120(10) 8 ? Co1 O7 2.210(11) . ? Co1 O14 2.281(2) . ? Co2 O3 1.972(11) . ? Co2 O11 1.978(11) . ? Co2 O4 1.989(11) . ? Co2 N4 2.117(12) . ? Co2 O8 2.316(9) . ? N1 C39 1.31(2) . ? N1 C35 1.36(2) . ? N2 C48 1.17(4) . ? N3 C46 1.14(3) . ? N4 C44 1.28(2) . ? N4 C40 1.37(2) . ? C1 C6 1.36(3) . ? C1 C2 1.42(2) . ? C2 C3 1.41(2) . ? C2 H2 0.9500 . ? C3 C4 1.36(3) . ? C3 H3 0.9500 . ? C4 C5 1.40(2) . ? C4 Cl1 1.736(18) . ? C5 C6 1.39(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C8 H8 0.9500 . ? C9 C10 1.3900 . ? C9 H9 0.9500 . ? C10 C11 1.3900 . ? C10 Cl3 1.731(8) . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.411(19) . ? C13 C14 1.411(19) 8 ? C14 C15 1.37(2) . ? C14 H14 0.9500 . ? C15 C16 1.43(2) . ? C15 H15 0.9500 . ? C16 C15 1.43(2) 8 ? C16 Cl2 1.70(2) . ? C17 C18 1.38(3) . ? C17 C22 1.39(3) . ? C18 C19 1.39(2) . ? C18 H18 0.9500 . ? C19 C20 1.35(3) . ? C19 H19 0.9500 . ? C20 C21 1.33(3) . ? C20 H20 0.9500 . ? C21 C22 1.42(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.34(3) . ? C23 C24 1.42(3) . ? C24 C25 1.40(2) . ? C24 H24 0.9500 . ? C25 C26 1.39(2) . ? C25 H25 0.9500 . ? C26 C27 1.36(3) . ? C26 H26 0.9500 . ? C27 C28 1.42(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.38(3) . ? C29 C34 1.41(4) . ? C30 C31 1.40(2) . ? C30 H30 0.9500 . ? C31 C32 1.36(3) . ? C31 H31 0.9500 . ? C32 C33 1.39(3) . ? C32 H32 0.9500 . ? C33 C34 1.33(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.36(2) . ? C35 H35 0.9500 . ? C36 C37 1.37(2) . ? C36 H36 0.9500 . ? C37 C38 1.39(3) . ? C37 H37 0.9500 . ? C38 C39 1.34(2) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.40(3) . ? C40 H40 0.9500 . ? C41 C42 1.39(3) . ? C41 H41 0.9500 . ? C42 C43 1.37(3) . ? C42 H42 0.9500 . ? C43 C44 1.40(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.45(3) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 C48 1.41(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? O10 Co1 2.120(10) 8 ? O13 Co1 2.046(12) 8 ? O14 Co1 2.281(2) 8 ? 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 O7 Sb1 O9 90.2(4) . . ? O7 Sb1 O8 90.6(4) . . ? O9 Sb1 O8 81.8(4) . . ? O7 Sb1 O2 91.5(4) . . ? O9 Sb1 O2 170.8(4) . . ? O8 Sb1 O2 89.2(4) . . ? O7 Sb1 O5 173.8(4) . . ? O9 Sb1 O5 88.8(4) . . ? O8 Sb1 O5 83.2(4) . . ? O2 Sb1 O5 88.5(4) . . ? O7 Sb1 C1 98.1(6) . . ? O9 Sb1 C1 98.8(6) . . ? O8 Sb1 C1 171.3(6) . . ? O2 Sb1 C1 89.9(6) . . ? O5 Sb1 C1 88.0(6) . . ? O7 Sb1 Sb2 91.4(3) . . ? O9 Sb1 Sb2 40.4(3) . . ? O8 Sb1 Sb2 41.4(3) . . ? O2 Sb1 Sb2 130.5(3) . . ? O5 Sb1 Sb2 84.0(3) . . ? C1 Sb1 Sb2 138.3(5) . . ? O9 Sb2 O10 89.3(4) . . ? O9 Sb2 O8 82.3(4) . . ? O10 Sb2 O8 90.2(4) . . ? O9 Sb2 O12 170.3(4) . . ? O10 Sb2 O12 92.6(4) . . ? O8 Sb2 O12 88.2(4) . . ? O9 Sb2 O6 88.3(4) . . ? O10 Sb2 O6 173.9(4) . . ? O8 Sb2 O6 83.9(4) . . ? O12 Sb2 O6 88.9(4) . . ? O9 Sb2 C7 98.1(4) . . ? O10 Sb2 C7 94.4(4) . . ? O8 Sb2 C7 175.3(5) . . ? O12 Sb2 C7 91.3(4) . . ? O6 Sb2 C7 91.4(4) . . ? O9 Sb2 Sb1 40.9(3) . . ? O10 Sb2 Sb1 90.5(3) . . ? O8 Sb2 Sb1 41.4(3) . . ? O12 Sb2 Sb1 129.5(3) . . ? O6 Sb2 Sb1 84.0(3) . . ? C7 Sb2 Sb1 138.6(3) . . ? O10 Sb3 O10 161.2(6) . 8 ? O10 Sb3 O7 99.9(4) . . ? O10 Sb3 O7 77.9(4) 8 . ? O10 Sb3 O7 77.9(4) . 8 ? O10 Sb3 O7 99.9(4) 8 8 ? O7 Sb3 O7 167.2(7) . 8 ? O10 Sb3 O14 80.6(3) . . ? O10 Sb3 O14 80.6(3) 8 . ? O7 Sb3 O14 83.6(3) . . ? O7 Sb3 O14 83.6(3) 8 . ? O10 Sb3 C13 99.4(3) . . ? O10 Sb3 C13 99.4(3) 8 . ? O7 Sb3 C13 96.4(3) . . ? O7 Sb3 C13 96.4(3) 8 . ? O14 Sb3 C13 180.000(1) . . ? O10 Sb3 Co1 46.0(3) . 8 ? O10 Sb3 Co1 119.1(3) 8 8 ? O7 Sb3 Co1 121.3(3) . 8 ? O7 Sb3 Co1 48.6(3) 8 8 ? O14 Sb3 Co1 50.50(4) . 8 ? C13 Sb3 Co1 129.50(4) . 8 ? O10 Sb3 Co1 119.1(3) . . ? O10 Sb3 Co1 46.0(3) 8 . ? O7 Sb3 Co1 48.6(3) . . ? O7 Sb3 Co1 121.3(3) 8 . ? O14 Sb3 Co1 50.49(4) . . ? C13 Sb3 Co1 129.51(4) . . ? Co1 Sb3 Co1 100.99(8) 8 . ? O1 P1 O3 113.4(6) . . ? O1 P1 O2 112.8(6) . . ? O3 P1 O2 110.4(6) . . ? O1 P1 C17 107.9(8) . . ? O3 P1 C17 108.7(8) . . ? O2 P1 C17 102.9(8) . . ? O11 P2 O13 114.6(7) . . ? O11 P2 O12 110.9(7) . . ? O13 P2 O12 111.6(7) . . ? O11 P2 C23 108.7(8) . . ? O13 P2 C23 108.5(8) . . ? O12 P2 C23 101.6(7) . . ? O4 P3 O5 111.0(6) . . ? O4 P3 O6 113.8(6) . . ? O5 P3 O6 111.7(6) . . ? O4 P3 C29 110.2(10) . . ? O5 P3 C29 103.5(8) . . ? O6 P3 C29 106.0(8) . . ? O1 Co1 O13 91.7(4) . 8 ? O1 Co1 N1 105.1(5) . . ? O13 Co1 N1 99.3(5) 8 . ? O1 Co1 O10 158.6(4) . 8 ? O13 Co1 O10 98.9(4) 8 8 ? N1 Co1 O10 91.6(4) . 8 ? O1 Co1 O7 94.1(4) . . ? O13 Co1 O7 163.6(4) 8 . ? N1 Co1 O7 94.0(4) . . ? O10 Co1 O7 71.0(3) 8 . ? O1 Co1 O14 88.1(4) . . ? O13 Co1 O14 90.6(4) 8 . ? N1 Co1 O14 163.2(5) . . ? O10 Co1 O14 73.3(4) 8 . ? O7 Co1 O14 74.3(4) . . ? O1 Co1 Sb3 116.0(3) . . ? O13 Co1 Sb3 121.2(3) 8 . ? N1 Co1 Sb3 119.1(3) . . ? O10 Co1 Sb3 42.7(3) 8 . ? O7 Co1 Sb3 42.8(2) . . ? O14 Co1 Sb3 44.4(3) . . ? O3 Co2 O11 119.9(5) . . ? O3 Co2 O4 116.6(5) . . ? O11 Co2 O4 123.4(5) . . ? O3 Co2 N4 90.6(5) . . ? O11 Co2 N4 92.3(5) . . ? O4 Co2 N4 90.9(5) . . ? O3 Co2 O8 91.5(4) . . ? O11 Co2 O8 88.0(4) . . ? O4 Co2 O8 86.8(4) . . ? N4 Co2 O8 177.4(5) . . ? C39 N1 C35 117.1(14) . . ? C39 N1 Co1 123.8(11) . . ? C35 N1 Co1 118.7(10) . . ? C44 N4 C40 115.2(16) . . ? C44 N4 Co2 122.0(13) . . ? C40 N4 Co2 122.7(12) . . ? C6 C1 C2 119.9(16) . . ? C6 C1 Sb1 122.2(13) . . ? C2 C1 Sb1 117.3(14) . . ? C3 C2 C1 119.2(18) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 120.1(17) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.9(16) . . ? C3 C4 Cl1 120.1(14) . . ? C5 C4 Cl1 120.0(15) . . ? C6 C5 C4 120.5(18) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C1 C6 C5 120.1(17) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C12 120.0 . . ? C8 C7 Sb2 119.2(5) . . ? C12 C7 Sb2 120.7(5) . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.0 . . ? C9 C10 Cl3 119.5(6) . . ? C11 C10 Cl3 120.5(6) . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C14 121(2) . 8 ? C14 C13 Sb3 119.7(10) . . ? C14 C13 Sb3 119.7(10) 8 . ? C15 C14 C13 120.4(17) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.1(17) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C15 120(2) 8 . ? C15 C16 Cl2 119.9(10) 8 . ? C15 C16 Cl2 119.9(10) . . ? C18 C17 C22 117.4(16) . . ? C18 C17 P1 121.5(14) . . ? C22 C17 P1 120.9(15) . . ? C17 C18 C19 119.9(18) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 121.1(19) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C19 121.7(16) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 118.3(18) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? C17 C22 C21 121.4(19) . . ? C17 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C28 C23 C24 120.3(16) . . ? C28 C23 P2 120.7(14) . . ? C24 C23 P2 119.0(13) . . ? C25 C24 C23 119.4(17) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C26 C25 C24 118.5(17) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C27 C26 C25 122.0(16) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 119.1(17) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C23 C28 C27 120.6(17) . . ? C23 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C34 117.6(18) . . ? C30 C29 P3 124(2) . . ? C34 C29 P3 118.6(17) . . ? C29 C30 C31 120(2) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 120(2) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 120.7(19) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 119(2) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C29 123(2) . . ? C33 C34 H34 118.7 . . ? C29 C34 H34 118.7 . . ? N1 C35 C36 122.5(17) . . ? N1 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C35 C36 C37 118.3(18) . . ? C35 C36 H36 120.8 . . ? C37 C36 H36 120.8 . . ? C36 C37 C38 119.3(16) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 117.7(18) . . ? C39 C38 H38 121.2 . . ? C37 C38 H38 121.2 . . ? N1 C39 C38 125.1(19) . . ? N1 C39 H39 117.5 . . ? C38 C39 H39 117.5 . . ? N4 C40 C41 124.7(19) . . ? N4 C40 H40 117.6 . . ? C41 C40 H40 117.6 . . ? C42 C41 C40 116.1(19) . . ? C42 C41 H41 122.0 . . ? C40 C41 H41 122.0 . . ? C43 C42 C41 119.8(18) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 118(2) . . ? C42 C43 H43 120.8 . . ? C44 C43 H43 120.8 . . ? N4 C44 C43 125(2) . . ? N4 C44 H44 117.3 . . ? C43 C44 H44 117.3 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N3 C46 C45 177(3) . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N2 C48 C47 174(4) . . ? P1 O1 Co1 132.1(7) . . ? P1 O2 Sb1 128.6(6) . . ? P1 O3 Co2 127.6(7) . . ? P3 O4 Co2 120.8(6) . . ? P3 O5 Sb1 123.4(6) . . ? P3 O6 Sb2 122.1(6) . . ? Sb1 O7 Sb3 127.1(5) . . ? Sb1 O7 Co1 128.6(5) . . ? Sb3 O7 Co1 88.6(4) . . ? Sb2 O8 Sb1 97.2(4) . . ? Sb2 O8 Co2 124.4(5) . . ? Sb1 O8 Co2 124.0(5) . . ? Sb2 O9 Sb1 98.7(4) . . ? Sb2 O10 Sb3 127.8(5) . . ? Sb2 O10 Co1 128.3(5) . 8 ? Sb3 O10 Co1 91.3(4) . 8 ? P2 O11 Co2 132.5(7) . . ? P2 O12 Sb2 130.8(6) . . ? P2 O13 Co1 131.4(8) . 8 ? Sb3 O14 Co1 85.1(3) . . ? Sb3 O14 Co1 85.1(3) . 8 ? Co1 O14 Co1 170.3(7) . 8 ? 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 O7 Sb1 Sb2 O9 -88.8(6) . . . . ? O8 Sb1 Sb2 O9 -178.1(6) . . . . ? O2 Sb1 Sb2 O9 178.1(6) . . . . ? O5 Sb1 Sb2 O9 95.3(6) . . . . ? C1 Sb1 Sb2 O9 15.1(10) . . . . ? O7 Sb1 Sb2 O10 -0.4(5) . . . . ? O9 Sb1 Sb2 O10 88.3(6) . . . . ? O8 Sb1 Sb2 O10 -89.8(5) . . . . ? O2 Sb1 Sb2 O10 -93.6(5) . . . . ? O5 Sb1 Sb2 O10 -176.4(4) . . . . ? C1 Sb1 Sb2 O10 103.4(9) . . . . ? O7 Sb1 Sb2 O8 89.3(5) . . . . ? O9 Sb1 Sb2 O8 178.1(6) . . . . ? O2 Sb1 Sb2 O8 -3.8(6) . . . . ? O5 Sb1 Sb2 O8 -86.6(5) . . . . ? C1 Sb1 Sb2 O8 -166.8(9) . . . . ? O7 Sb1 Sb2 O12 93.3(5) . . . . ? O9 Sb1 Sb2 O12 -178.0(6) . . . . ? O8 Sb1 Sb2 O12 4.0(6) . . . . ? O2 Sb1 Sb2 O12 0.1(6) . . . . ? O5 Sb1 Sb2 O12 -82.7(5) . . . . ? C1 Sb1 Sb2 O12 -162.8(9) . . . . ? O7 Sb1 Sb2 O6 176.9(5) . . . . ? O9 Sb1 Sb2 O6 -94.3(6) . . . . ? O8 Sb1 Sb2 O6 87.6(5) . . . . ? O2 Sb1 Sb2 O6 83.8(5) . . . . ? O5 Sb1 Sb2 O6 1.0(5) . . . . ? C1 Sb1 Sb2 O6 -79.2(9) . . . . ? O7 Sb1 Sb2 C7 -97.8(6) . . . . ? O9 Sb1 Sb2 C7 -9.0(7) . . . . ? O8 Sb1 Sb2 C7 172.9(7) . . . . ? O2 Sb1 Sb2 C7 169.1(7) . . . . ? O5 Sb1 Sb2 C7 86.3(6) . . . . ? C1 Sb1 Sb2 C7 6.1(10) . . . . ? O10 Sb3 Co1 O1 -11.0(5) . . . . ? O10 Sb3 Co1 O1 -176.6(5) 8 . . . ? O7 Sb3 Co1 O1 65.8(6) . . . . ? O7 Sb3 Co1 O1 -104.4(5) 8 . . . ? O14 Sb3 Co1 O1 -56.4(4) . . . . ? C13 Sb3 Co1 O1 123.6(4) . . . . ? Co1 Sb3 Co1 O1 -56.4(4) 8 . . . ? O10 Sb3 Co1 O13 98.5(5) . . . 8 ? O10 Sb3 Co1 O13 -67.1(6) 8 . . 8 ? O7 Sb3 Co1 O13 175.3(6) . . . 8 ? O7 Sb3 Co1 O13 5.1(6) 8 . . 8 ? O14 Sb3 Co1 O13 53.1(4) . . . 8 ? C13 Sb3 Co1 O13 -126.9(4) . . . 8 ? Co1 Sb3 Co1 O13 53.0(4) 8 . . 8 ? O10 Sb3 Co1 N1 -138.0(5) . . . . ? O10 Sb3 Co1 N1 56.4(6) 8 . . . ? O7 Sb3 Co1 N1 -61.2(6) . . . . ? O7 Sb3 Co1 N1 128.6(6) 8 . . . ? O14 Sb3 Co1 N1 176.5(5) . . . . ? C13 Sb3 Co1 N1 -3.5(5) . . . . ? Co1 Sb3 Co1 N1 176.5(5) 8 . . . ? O10 Sb3 Co1 O10 165.6(5) . . . 8 ? O7 Sb3 Co1 O10 -117.6(5) . . . 8 ? O7 Sb3 Co1 O10 72.2(5) 8 . . 8 ? O14 Sb3 Co1 O10 120.1(4) . . . 8 ? C13 Sb3 Co1 O10 -59.9(4) . . . 8 ? Co1 Sb3 Co1 O10 120.1(4) 8 . . 8 ? O10 Sb3 Co1 O7 -76.8(5) . . . . ? O10 Sb3 Co1 O7 117.6(5) 8 . . . ? O7 Sb3 Co1 O7 -170.2(5) 8 . . . ? O14 Sb3 Co1 O7 -122.3(4) . . . . ? C13 Sb3 Co1 O7 57.7(4) . . . . ? Co1 Sb3 Co1 O7 -122.3(4) 8 . . . ? O10 Sb3 Co1 O14 45.4(3) . . . . ? O10 Sb3 Co1 O14 -120.1(4) 8 . . . ? O7 Sb3 Co1 O14 122.3(4) . . . . ? O7 Sb3 Co1 O14 -47.9(3) 8 . . . ? C13 Sb3 Co1 O14 180.000(1) . . . . ? Co1 Sb3 Co1 O14 0.0 8 . . . ? O1 Co1 N1 C39 74.8(16) . . . . ? O13 Co1 N1 C39 -19.5(16) 8 . . . ? O10 Co1 N1 C39 -118.8(15) 8 . . . ? O7 Co1 N1 C39 170.2(15) . . . . ? O14 Co1 N1 C39 -144.7(13) . . . . ? Sb3 Co1 N1 C39 -153.2(14) . . . . ? O1 Co1 N1 C35 -112.9(13) . . . . ? O13 Co1 N1 C35 152.8(13) 8 . . . ? O10 Co1 N1 C35 53.5(13) 8 . . . ? O7 Co1 N1 C35 -17.5(13) . . . . ? O14 Co1 N1 C35 28(2) . . . . ? Sb3 Co1 N1 C35 19.1(14) . . . . ? O3 Co2 N4 C44 75.1(14) . . . . ? O11 Co2 N4 C44 -165.0(14) . . . . ? O4 Co2 N4 C44 -41.5(14) . . . . ? O8 Co2 N4 C44 -68(11) . . . . ? O3 Co2 N4 C40 -107.8(13) . . . . ? O11 Co2 N4 C40 12.2(13) . . . . ? O4 Co2 N4 C40 135.6(13) . . . . ? O8 Co2 N4 C40 109(11) . . . . ? O7 Sb1 C1 C6 67.1(17) . . . . ? O9 Sb1 C1 C6 -24.4(17) . . . . ? O8 Sb1 C1 C6 -117(4) . . . . ? O2 Sb1 C1 C6 158.6(17) . . . . ? O5 Sb1 C1 C6 -112.9(17) . . . . ? Sb2 Sb1 C1 C6 -34(2) . . . . ? O7 Sb1 C1 C2 -121.8(14) . . . . ? O9 Sb1 C1 C2 146.7(14) . . . . ? O8 Sb1 C1 C2 54(5) . . . . ? O2 Sb1 C1 C2 -30.3(14) . . . . ? O5 Sb1 C1 C2 58.2(15) . . . . ? Sb2 Sb1 C1 C2 136.9(12) . . . . ? C6 C1 C2 C3 -3(3) . . . . ? Sb1 C1 C2 C3 -174.3(14) . . . . ? C1 C2 C3 C4 3(3) . . . . ? C2 C3 C4 C5 -4(3) . . . . ? C2 C3 C4 Cl1 176.8(15) . . . . ? C3 C4 C5 C6 4(3) . . . . ? Cl1 C4 C5 C6 -176.7(15) . . . . ? C2 C1 C6 C5 3(3) . . . . ? Sb1 C1 C6 C5 174.0(14) . . . . ? C4 C5 C6 C1 -3(3) . . . . ? O9 Sb2 C7 C8 11.2(7) . . . . ? O10 Sb2 C7 C8 -78.7(6) . . . . ? O8 Sb2 C7 C8 105(5) . . . . ? O12 Sb2 C7 C8 -171.4(7) . . . . ? O6 Sb2 C7 C8 99.7(7) . . . . ? Sb1 Sb2 C7 C8 17.1(9) . . . . ? O9 Sb2 C7 C12 -171.9(7) . . . . ? O10 Sb2 C7 C12 98.2(7) . . . . ? O8 Sb2 C7 C12 -78(5) . . . . ? O12 Sb2 C7 C12 5.5(7) . . . . ? O6 Sb2 C7 C12 -83.5(7) . . . . ? Sb1 Sb2 C7 C12 -166.0(5) . . . . ? C12 C7 C8 C9 0.0 . . . . ? Sb2 C7 C8 C9 176.9(9) . . . . ? C7 C8 C9 C10 0.0 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C8 C9 C10 Cl3 -178.8(10) . . . . ? C9 C10 C11 C12 0.0 . . . . ? Cl3 C10 C11 C12 178.8(10) . . . . ? C10 C11 C12 C7 0.0 . . . . ? C8 C7 C12 C11 0.0 . . . . ? Sb2 C7 C12 C11 -176.8(9) . . . . ? O10 Sb3 C13 C14 146.1(10) . . . . ? O10 Sb3 C13 C14 -33.9(10) 8 . . . ? O7 Sb3 C13 C14 44.9(10) . . . . ? O7 Sb3 C13 C14 -135.1(10) 8 . . . ? O14 Sb3 C13 C14 93.3(10) . . . . ? Co1 Sb3 C13 C14 -174.8(10) 8 . . . ? Co1 Sb3 C13 C14 5.2(10) . . . . ? O10 Sb3 C13 C14 -33.9(10) . . . 8 ? O10 Sb3 C13 C14 146.1(10) 8 . . 8 ? O7 Sb3 C13 C14 -135.1(10) . . . 8 ? O7 Sb3 C13 C14 44.9(10) 8 . . 8 ? O14 Sb3 C13 C14 -86.7(10) . . . 8 ? Co1 Sb3 C13 C14 5.2(10) 8 . . 8 ? Co1 Sb3 C13 C14 -174.8(10) . . . 8 ? C14 C13 C14 C15 0.6(15) 8 . . . ? Sb3 C13 C14 C15 -179.4(15) . . . . ? C13 C14 C15 C16 -1(3) . . . . ? C14 C15 C16 C15 0.6(14) . . . 8 ? C14 C15 C16 Cl2 -179.4(15) . . . . ? O1 P1 C17 C18 173.8(15) . . . . ? O3 P1 C17 C18 -62.8(17) . . . . ? O2 P1 C17 C18 54.3(17) . . . . ? O1 P1 C17 C22 -1.0(18) . . . . ? O3 P1 C17 C22 122.4(16) . . . . ? O2 P1 C17 C22 -120.5(16) . . . . ? C22 C17 C18 C19 -1(3) . . . . ? P1 C17 C18 C19 -176.1(15) . . . . ? C17 C18 C19 C20 3(3) . . . . ? C18 C19 C20 C21 -2(3) . . . . ? C19 C20 C21 C22 -1(3) . . . . ? C18 C17 C22 C21 -2(3) . . . . ? P1 C17 C22 C21 173.0(15) . . . . ? C20 C21 C22 C17 3(3) . . . . ? O11 P2 C23 C28 72.8(18) . . . . ? O13 P2 C23 C28 -162.0(16) . . . . ? O12 P2 C23 C28 -44.2(18) . . . . ? O11 P2 C23 C24 -105.6(16) . . . . ? O13 P2 C23 C24 19.6(18) . . . . ? O12 P2 C23 C24 137.3(15) . . . . ? C28 C23 C24 C25 5(3) . . . . ? P2 C23 C24 C25 -176.3(14) . . . . ? C23 C24 C25 C26 -4(3) . . . . ? C24 C25 C26 C27 1(3) . . . . ? C25 C26 C27 C28 2(3) . . . . ? C24 C23 C28 C27 -3(3) . . . . ? P2 C23 C28 C27 179.1(15) . . . . ? C26 C27 C28 C23 -1(3) . . . . ? O4 P3 C29 C30 8.4(19) . . . . ? O5 P3 C29 C30 -110.4(17) . . . . ? O6 P3 C29 C30 131.9(16) . . . . ? O4 P3 C29 C34 -177.5(14) . . . . ? O5 P3 C29 C34 63.7(16) . . . . ? O6 P3 C29 C34 -53.9(17) . . . . ? C34 C29 C30 C31 1(3) . . . . ? P3 C29 C30 C31 175.1(16) . . . . ? C29 C30 C31 C32 -2(3) . . . . ? C30 C31 C32 C33 0(3) . . . . ? C31 C32 C33 C34 3(3) . . . . ? C32 C33 C34 C29 -4(3) . . . . ? C30 C29 C34 C33 2(3) . . . . ? P3 C29 C34 C33 -172.7(16) . . . . ? C39 N1 C35 C36 -2(3) . . . . ? Co1 N1 C35 C36 -174.8(15) . . . . ? N1 C35 C36 C37 3(3) . . . . ? C35 C36 C37 C38 -3(3) . . . . ? C36 C37 C38 C39 2(3) . . . . ? C35 N1 C39 C38 1(3) . . . . ? Co1 N1 C39 C38 173.4(16) . . . . ? C37 C38 C39 N1 -1(3) . . . . ? C44 N4 C40 C41 -3(3) . . . . ? Co2 N4 C40 C41 179.9(14) . . . . ? N4 C40 C41 C42 0(3) . . . . ? C40 C41 C42 C43 -1(3) . . . . ? C41 C42 C43 C44 5(3) . . . . ? C40 N4 C44 C43 7(3) . . . . ? Co2 N4 C44 C43 -175.4(15) . . . . ? C42 C43 C44 N4 -9(3) . . . . ? O3 P1 O1 Co1 142.7(8) . . . . ? O2 P1 O1 Co1 16.2(11) . . . . ? C17 P1 O1 Co1 -96.8(10) . . . . ? O13 Co1 O1 P1 155.1(9) 8 . . . ? N1 Co1 O1 P1 55.0(10) . . . . ? O10 Co1 O1 P1 -85.1(14) 8 . . . ? O7 Co1 O1 P1 -40.3(9) . . . . ? O14 Co1 O1 P1 -114.4(9) . . . . ? Sb3 Co1 O1 P1 -78.8(9) . . . . ? O1 P1 O2 Sb1 50.8(10) . . . . ? O3 P1 O2 Sb1 -77.3(9) . . . . ? C17 P1 O2 Sb1 166.8(9) . . . . ? O7 Sb1 O2 P1 -61.6(8) . . . . ? O9 Sb1 O2 P1 39(3) . . . . ? O8 Sb1 O2 P1 29.0(8) . . . . ? O5 Sb1 O2 P1 112.3(8) . . . . ? C1 Sb1 O2 P1 -159.7(10) . . . . ? Sb2 Sb1 O2 P1 31.5(10) . . . . ? O1 P1 O3 Co2 -79.7(10) . . . . ? O2 P1 O3 Co2 48.1(10) . . . . ? C17 P1 O3 Co2 160.3(9) . . . . ? O11 Co2 O3 P1 93.1(9) . . . . ? O4 Co2 O3 P1 -82.7(9) . . . . ? N4 Co2 O3 P1 -174.0(9) . . . . ? O8 Co2 O3 P1 4.5(9) . . . . ? O5 P3 O4 Co2 -64.5(8) . . . . ? O6 P3 O4 Co2 62.5(9) . . . . ? C29 P3 O4 Co2 -178.6(8) . . . . ? O3 Co2 O4 P3 91.2(8) . . . . ? O11 Co2 O4 P3 -84.4(9) . . . . ? N4 Co2 O4 P3 -177.7(8) . . . . ? O8 Co2 O4 P3 1.2(7) . . . . ? O4 P3 O5 Sb1 85.1(8) . . . . ? O6 P3 O5 Sb1 -43.0(9) . . . . ? C29 P3 O5 Sb1 -156.7(10) . . . . ? O7 Sb1 O5 P3 -19(4) . . . . ? O9 Sb1 O5 P3 62.2(8) . . . . ? O8 Sb1 O5 P3 -19.7(8) . . . . ? O2 Sb1 O5 P3 -109.0(8) . . . . ? C1 Sb1 O5 P3 161.0(9) . . . . ? Sb2 Sb1 O5 P3 22.0(7) . . . . ? O4 P3 O6 Sb2 -82.8(8) . . . . ? O5 P3 O6 Sb2 43.9(9) . . . . ? C29 P3 O6 Sb2 155.9(10) . . . . ? O9 Sb2 O6 P3 -64.5(8) . . . . ? O10 Sb2 O6 P3 2(5) . . . . ? O8 Sb2 O6 P3 17.9(7) . . . . ? O12 Sb2 O6 P3 106.2(8) . . . . ? C7 Sb2 O6 P3 -162.5(8) . . . . ? Sb1 Sb2 O6 P3 -23.7(7) . . . . ? O9 Sb1 O7 Sb3 -27.8(7) . . . . ? O8 Sb1 O7 Sb3 54.0(7) . . . . ? O2 Sb1 O7 Sb3 143.2(7) . . . . ? O5 Sb1 O7 Sb3 54(4) . . . . ? C1 Sb1 O7 Sb3 -126.7(8) . . . . ? Sb2 Sb1 O7 Sb3 12.6(7) . . . . ? O9 Sb1 O7 Co1 -152.1(6) . . . . ? O8 Sb1 O7 Co1 -70.3(6) . . . . ? O2 Sb1 O7 Co1 18.9(7) . . . . ? O5 Sb1 O7 Co1 -71(4) . . . . ? C1 Sb1 O7 Co1 109.0(8) . . . . ? Sb2 Sb1 O7 Co1 -111.6(6) . . . . ? O10 Sb3 O7 Sb1 -19.4(7) . . . . ? O10 Sb3 O7 Sb1 179.6(8) 8 . . . ? O7 Sb3 O7 Sb1 -98.7(7) 8 . . . ? O14 Sb3 O7 Sb1 -98.7(7) . . . . ? C13 Sb3 O7 Sb1 81.3(7) . . . . ? Co1 Sb3 O7 Sb1 -63.5(8) 8 . . . ? Co1 Sb3 O7 Sb1 -139.7(9) . . . . ? O10 Sb3 O7 Co1 120.3(4) . . . . ? O10 Sb3 O7 Co1 -40.7(3) 8 . . . ? O7 Sb3 O7 Co1 41.0(3) 8 . . . ? O14 Sb3 O7 Co1 41.0(3) . . . . ? C13 Sb3 O7 Co1 -139.0(3) . . . . ? Co1 Sb3 O7 Co1 76.2(4) 8 . . . ? O1 Co1 O7 Sb1 14.0(7) . . . . ? O13 Co1 O7 Sb1 124.4(15) 8 . . . ? N1 Co1 O7 Sb1 -91.4(7) . . . . ? O10 Co1 O7 Sb1 178.2(8) 8 . . . ? O14 Co1 O7 Sb1 100.9(7) . . . . ? Sb3 Co1 O7 Sb1 138.8(9) . . . . ? O1 Co1 O7 Sb3 -124.7(4) . . . . ? O13 Co1 O7 Sb3 -14.3(18) 8 . . . ? N1 Co1 O7 Sb3 129.8(5) . . . . ? O10 Co1 O7 Sb3 39.5(3) 8 . . . ? O14 Co1 O7 Sb3 -37.9(3) . . . . ? O9 Sb2 O8 Sb1 1.3(4) . . . . ? O10 Sb2 O8 Sb1 90.5(4) . . . . ? O12 Sb2 O8 Sb1 -176.9(4) . . . . ? O6 Sb2 O8 Sb1 -87.8(4) . . . . ? C7 Sb2 O8 Sb1 -93(5) . . . . ? O9 Sb2 O8 Co2 141.6(6) . . . . ? O10 Sb2 O8 Co2 -129.2(6) . . . . ? O12 Sb2 O8 Co2 -36.7(6) . . . . ? O6 Sb2 O8 Co2 52.5(6) . . . . ? C7 Sb2 O8 Co2 47(5) . . . . ? Sb1 Sb2 O8 Co2 140.3(8) . . . . ? O7 Sb1 O8 Sb2 -91.4(4) . . . . ? O9 Sb1 O8 Sb2 -1.3(4) . . . . ? O2 Sb1 O8 Sb2 177.1(5) . . . . ? O5 Sb1 O8 Sb2 88.5(4) . . . . ? C1 Sb1 O8 Sb2 93(4) . . . . ? O7 Sb1 O8 Co2 128.1(6) . . . . ? O9 Sb1 O8 Co2 -141.8(6) . . . . ? O2 Sb1 O8 Co2 36.6(6) . . . . ? O5 Sb1 O8 Co2 -52.0(5) . . . . ? C1 Sb1 O8 Co2 -48(4) . . . . ? Sb2 Sb1 O8 Co2 -140.5(8) . . . . ? O3 Co2 O8 Sb2 177.9(6) . . . . ? O11 Co2 O8 Sb2 58.0(6) . . . . ? O4 Co2 O8 Sb2 -65.6(6) . . . . ? N4 Co2 O8 Sb2 -39(11) . . . . ? O3 Co2 O8 Sb1 -52.0(6) . . . . ? O11 Co2 O8 Sb1 -171.9(6) . . . . ? O4 Co2 O8 Sb1 64.5(6) . . . . ? N4 Co2 O8 Sb1 91(11) . . . . ? O10 Sb2 O9 Sb1 -91.6(5) . . . . ? O8 Sb2 O9 Sb1 -1.3(4) . . . . ? O12 Sb2 O9 Sb1 9(3) . . . . ? O6 Sb2 O9 Sb1 82.8(5) . . . . ? C7 Sb2 O9 Sb1 174.0(5) . . . . ? O7 Sb1 O9 Sb2 91.8(5) . . . . ? O8 Sb1 O9 Sb2 1.3(4) . . . . ? O2 Sb1 O9 Sb2 -9(3) . . . . ? O5 Sb1 O9 Sb2 -82.1(5) . . . . ? C1 Sb1 O9 Sb2 -169.9(6) . . . . ? O9 Sb2 O10 Sb3 29.0(6) . . . . ? O8 Sb2 O10 Sb3 -53.3(6) . . . . ? O12 Sb2 O10 Sb3 -141.5(7) . . . . ? O6 Sb2 O10 Sb3 -37(4) . . . . ? C7 Sb2 O10 Sb3 127.0(6) . . . . ? Sb1 Sb2 O10 Sb3 -11.8(6) . . . . ? O9 Sb2 O10 Co1 159.4(6) . . . 8 ? O8 Sb2 O10 Co1 77.2(6) . . . 8 ? O12 Sb2 O10 Co1 -11.0(6) . . . 8 ? O6 Sb2 O10 Co1 93(4) . . . 8 ? C7 Sb2 O10 Co1 -102.5(6) . . . 8 ? Sb1 Sb2 O10 Co1 118.6(5) . . . 8 ? O10 Sb3 O10 Sb2 100.8(6) 8 . . . ? O7 Sb3 O10 Sb2 19.1(7) . . . . ? O7 Sb3 O10 Sb2 -173.8(8) 8 . . . ? O14 Sb3 O10 Sb2 100.8(6) . . . . ? C13 Sb3 O10 Sb2 -79.2(6) . . . . ? Co1 Sb3 O10 Sb2 143.3(8) 8 . . . ? Co1 Sb3 O10 Sb2 66.9(7) . . . . ? O10 Sb3 O10 Co1 -42.6(2) 8 . . 8 ? O7 Sb3 O10 Co1 -124.3(4) . . . 8 ? O7 Sb3 O10 Co1 42.8(4) 8 . . 8 ? O14 Sb3 O10 Co1 -42.6(2) . . . 8 ? C13 Sb3 O10 Co1 137.4(2) . . . 8 ? Co1 Sb3 O10 Co1 -76.4(3) . . . 8 ? O13 P2 O11 Co2 98.9(11) . . . . ? O12 P2 O11 Co2 -28.7(12) . . . . ? C23 P2 O11 Co2 -139.6(10) . . . . ? O3 Co2 O11 P2 -111.0(10) . . . . ? O4 Co2 O11 P2 64.5(11) . . . . ? N4 Co2 O11 P2 157.0(10) . . . . ? O8 Co2 O11 P2 -20.4(10) . . . . ? O11 P2 O12 Sb2 70.3(10) . . . . ? O13 P2 O12 Sb2 -58.8(10) . . . . ? C23 P2 O12 Sb2 -174.3(9) . . . . ? O9 Sb2 O12 P2 -42(3) . . . . ? O10 Sb2 O12 P2 58.3(9) . . . . ? O8 Sb2 O12 P2 -31.8(9) . . . . ? O6 Sb2 O12 P2 -115.8(9) . . . . ? C7 Sb2 O12 P2 152.8(9) . . . . ? Sb1 Sb2 O12 P2 -34.5(10) . . . . ? O11 P2 O13 Co1 -123.8(10) . . . 8 ? O12 P2 O13 Co1 3.3(12) . . . 8 ? C23 P2 O13 Co1 114.5(11) . . . 8 ? O10 Sb3 O14 Co1 -140.9(3) . . . . ? O10 Sb3 O14 Co1 39.1(3) 8 . . . ? O7 Sb3 O14 Co1 -39.7(3) . . . . ? O7 Sb3 O14 Co1 140.3(3) 8 . . . ? C13 Sb3 O14 Co1 -88.11(5) . . . . ? Co1 Sb3 O14 Co1 180.0 8 . . . ? O10 Sb3 O14 Co1 39.1(3) . . . 8 ? O10 Sb3 O14 Co1 -140.9(3) 8 . . 8 ? O7 Sb3 O14 Co1 140.3(3) . . . 8 ? O7 Sb3 O14 Co1 -39.7(3) 8 . . 8 ? C13 Sb3 O14 Co1 91.89(5) . . . 8 ? Co1 Sb3 O14 Co1 180.0 . . . 8 ? O1 Co1 O14 Sb3 131.5(3) . . . . ? O13 Co1 O14 Sb3 -136.8(3) 8 . . . ? N1 Co1 O14 Sb3 -10.6(14) . . . . ? O10 Co1 O14 Sb3 -37.8(3) 8 . . . ? O7 Co1 O14 Sb3 36.7(3) . . . . ? O1 Co1 O14 Co1 131.5(3) . . . 8 ? O13 Co1 O14 Co1 -136.8(3) 8 . . 8 ? N1 Co1 O14 Co1 -10.6(14) . . . 8 ? O10 Co1 O14 Co1 -37.7(3) 8 . . 8 ? O7 Co1 O14 Co1 36.7(3) . . . 8 ? Sb3 Co1 O14 Co1 0.011(5) . . . 8 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.875 _refine_diff_density_min -2.077 _refine_diff_density_rms 0.274 # Attachment '- 14.cif' data_mono1013 _database_code_depnum_ccdc_archive 'CCDC 700899' #TrackingRef '- 14.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H51 Cl2 Co2 N2 O13 P3 Sb2' _chemical_formula_weight 1244.96 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 9.9052(2) _cell_length_b 22.5257(5) _cell_length_c 20.5666(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.694(2) _cell_angle_gamma 90.00 _cell_volume 4586.85(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12521 _cell_measurement_theta_min 2.6791 _cell_measurement_theta_max 28.5243 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 2.159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4789 _exptl_absorpt_correction_T_max 0.7378 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25685 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9325 _reflns_number_gt 6917 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0434P)^2^+0.0205P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9325 _refine_ls_number_parameters 552 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Sb1 Sb 0.37148(2) 0.228415(11) 0.879551(12) 0.01427(7) Uani 1 1 d . . . Sb2 Sb 0.35710(2) 0.347574(11) 0.811315(12) 0.01354(7) Uani 1 1 d . . . Co1 Co 0.57643(5) 0.35393(2) 0.97722(2) 0.01398(12) Uani 1 1 d . . . Co2 Co 0.63673(5) 0.27821(2) 0.81037(2) 0.01556(12) Uani 1 1 d . . . P1 P 0.66234(10) 0.22232(4) 0.94995(5) 0.0146(2) Uani 1 1 d . . . P2 P 0.26842(9) 0.34156(4) 0.95934(5) 0.0144(2) Uani 1 1 d . . . P3 P 0.63593(10) 0.41376(5) 0.84519(5) 0.0157(2) Uani 1 1 d . . . N1 N 0.7626(3) 0.25339(16) 0.73602(16) 0.0240(8) Uani 1 1 d . . . N2 N 0.6718(3) 0.39106(14) 1.06083(15) 0.0170(7) Uani 1 1 d . . . C1 C 0.2519(4) 0.15227(17) 0.89123(18) 0.0150(8) Uani 1 1 d . . . C2 C 0.2737(4) 0.11405(18) 0.94358(18) 0.0185(8) Uani 1 1 d . . . H2 H 0.3440 0.1222 0.9747 0.022 Uiso 1 1 calc R . . C3 C 0.1932(4) 0.06398(18) 0.95079(19) 0.0192(8) Uani 1 1 d . . . H3 H 0.2086 0.0377 0.9864 0.023 Uiso 1 1 calc R . . C4 C 0.0904(4) 0.05300(17) 0.90538(19) 0.0185(8) Uani 1 1 d . . . C5 C 0.0662(4) 0.09081(18) 0.85338(19) 0.0216(9) Uani 1 1 d . . . H5 H -0.0044 0.0826 0.8224 0.026 Uiso 1 1 calc R . . C6 C 0.1468(4) 0.14108(18) 0.8470(2) 0.0228(9) Uani 1 1 d . . . H6 H 0.1295 0.1679 0.8121 0.027 Uiso 1 1 calc R . . C7 C 0.2198(4) 0.39295(17) 0.74908(18) 0.0151(8) Uani 1 1 d . . . C8 C 0.0899(4) 0.37019(19) 0.7410(2) 0.0255(10) Uani 1 1 d . . . H8 H 0.0640 0.3358 0.7643 0.031 Uiso 1 1 calc R . . C9 C -0.0015(4) 0.39818(19) 0.6988(2) 0.0284(10) Uani 1 1 d . . . H9 H -0.0910 0.3835 0.6933 0.034 Uiso 1 1 calc R . . C10 C 0.0388(4) 0.44749(19) 0.66484(19) 0.0223(9) Uani 1 1 d . . . C11 C 0.1650(4) 0.4713(2) 0.67368(19) 0.0239(9) Uani 1 1 d . . . H11 H 0.1898 0.5064 0.6514 0.029 Uiso 1 1 calc R . . C12 C 0.2564(4) 0.44299(18) 0.71611(18) 0.0184(9) Uani 1 1 d . . . H12 H 0.3451 0.4585 0.7222 0.022 Uiso 1 1 calc R . . C13 C 0.7577(4) 0.2855(2) 0.6796(2) 0.0306(11) Uani 1 1 d . . . H13 H 0.6969 0.3181 0.6761 0.037 Uiso 1 1 calc R . . C14 C 0.8374(5) 0.2727(2) 0.6278(2) 0.0349(11) Uani 1 1 d . . . H14 H 0.8290 0.2949 0.5886 0.042 Uiso 1 1 calc R . . C15 C 0.9304(4) 0.2268(2) 0.6339(2) 0.0356(12) Uani 1 1 d . . . H15 H 0.9874 0.2173 0.5990 0.043 Uiso 1 1 calc R . . C16 C 0.9389(5) 0.1953(2) 0.6912(2) 0.0355(11) Uani 1 1 d . . . H16 H 1.0020 0.1638 0.6962 0.043 Uiso 1 1 calc R . . C17 C 0.8540(4) 0.2100(2) 0.7420(2) 0.0299(10) Uani 1 1 d . . . H17 H 0.8616 0.1885 0.7817 0.036 Uiso 1 1 calc R . . C18 C 0.6817(4) 0.44913(18) 1.0684(2) 0.0212(9) Uani 1 1 d . . . H18 H 0.6451 0.4740 1.0349 0.025 Uiso 1 1 calc R . . C19 C 0.7425(4) 0.4757(2) 1.1223(2) 0.0280(10) Uani 1 1 d . . . H19 H 0.7472 0.5177 1.1261 0.034 Uiso 1 1 calc R . . C20 C 0.7961(4) 0.43927(19) 1.1704(2) 0.0243(9) Uani 1 1 d . . . H20 H 0.8383 0.4559 1.2083 0.029 Uiso 1 1 calc R . . C21 C 0.7878(4) 0.37896(19) 1.1632(2) 0.0246(9) Uani 1 1 d . . . H21 H 0.8238 0.3532 1.1960 0.030 Uiso 1 1 calc R . . C22 C 0.7265(4) 0.35614(18) 1.10759(19) 0.0198(9) Uani 1 1 d . . . H22 H 0.7227 0.3143 1.1021 0.024 Uiso 1 1 calc R . . C23 C 0.7499(4) 0.16386(17) 0.99487(19) 0.0173(8) Uani 1 1 d . . . C24 C 0.7407(4) 0.10510(19) 0.9576(2) 0.0305(11) Uani 1 1 d . . . H24A H 0.7886 0.0741 0.9825 0.046 Uiso 1 1 calc R . . H24B H 0.7818 0.1097 0.9152 0.046 Uiso 1 1 calc R . . H24C H 0.6456 0.0938 0.9514 0.046 Uiso 1 1 calc R . . C25 C 0.6856(4) 0.1562(2) 1.06055(19) 0.0249(9) Uani 1 1 d . . . H25A H 0.5912 0.1440 1.0540 0.037 Uiso 1 1 calc R . . H25B H 0.6892 0.1940 1.0842 0.037 Uiso 1 1 calc R . . H25C H 0.7349 0.1258 1.0857 0.037 Uiso 1 1 calc R . . C26 C 0.8995(4) 0.18166(19) 1.0043(2) 0.0227(9) Uani 1 1 d . . . H26A H 0.9057 0.2191 1.0284 0.034 Uiso 1 1 calc R . . H26B H 0.9399 0.1866 0.9617 0.034 Uiso 1 1 calc R . . H26C H 0.9480 0.1506 1.0288 0.034 Uiso 1 1 calc R . . C27 C 0.1080(4) 0.35821(17) 0.99517(19) 0.0170(8) Uani 1 1 d . . . C28 C 0.1012(4) 0.3276(2) 1.0616(2) 0.0266(10) Uani 1 1 d . . . H28A H 0.0124 0.3346 1.0799 0.040 Uiso 1 1 calc R . . H28B H 0.1717 0.3437 1.0910 0.040 Uiso 1 1 calc R . . H28C H 0.1152 0.2848 1.0563 0.040 Uiso 1 1 calc R . . C29 C -0.0059(4) 0.3354(2) 0.9487(2) 0.0260(10) Uani 1 1 d . . . H29A H 0.0084 0.2932 0.9397 0.039 Uiso 1 1 calc R . . H29B H -0.0049 0.3578 0.9079 0.039 Uiso 1 1 calc R . . H29C H -0.0933 0.3407 0.9690 0.039 Uiso 1 1 calc R . . C30 C 0.0940(4) 0.42559(19) 1.0036(2) 0.0274(10) Uani 1 1 d . . . H30A H 0.0095 0.4344 1.0253 0.041 Uiso 1 1 calc R . . H30B H 0.0933 0.4448 0.9609 0.041 Uiso 1 1 calc R . . H30C H 0.1704 0.4406 1.0302 0.041 Uiso 1 1 calc R . . C31 C 0.7078(4) 0.48349(18) 0.81796(19) 0.0198(9) Uani 1 1 d . . . C32 C 0.6333(4) 0.53557(18) 0.8482(2) 0.0284(10) Uani 1 1 d . . . H32A H 0.6737 0.5730 0.8341 0.043 Uiso 1 1 calc R . . H32B H 0.6405 0.5327 0.8957 0.043 Uiso 1 1 calc R . . H32C H 0.5379 0.5345 0.8342 0.043 Uiso 1 1 calc R . . C33 C 0.6936(4) 0.4876(2) 0.74400(19) 0.0256(10) Uani 1 1 d . . . H33A H 0.5977 0.4862 0.7308 0.038 Uiso 1 1 calc R . . H33B H 0.7409 0.4542 0.7244 0.038 Uiso 1 1 calc R . . H33C H 0.7330 0.5250 0.7293 0.038 Uiso 1 1 calc R . . C34 C 0.8576(4) 0.48439(19) 0.8389(2) 0.0253(9) Uani 1 1 d . . . H34A H 0.9042 0.4512 0.8185 0.038 Uiso 1 1 calc R . . H34B H 0.8662 0.4806 0.8863 0.038 Uiso 1 1 calc R . . H34C H 0.8982 0.5219 0.8254 0.038 Uiso 1 1 calc R . . C35 C 0.4245(4) 0.2839(2) 0.6893(2) 0.0277(10) Uani 1 1 d . . . H35A H 0.3366 0.2674 0.7004 0.042 Uiso 1 1 calc R . . H35B H 0.4851 0.2517 0.6771 0.042 Uiso 1 1 calc R . . H35C H 0.4127 0.3115 0.6527 0.042 Uiso 1 1 calc R . . C36 C 0.5346(4) 0.14112(17) 0.8021(2) 0.0220(9) Uani 1 1 d . . . H36A H 0.6105 0.1351 0.8330 0.033 Uiso 1 1 calc R . . H36B H 0.5641 0.1333 0.7578 0.033 Uiso 1 1 calc R . . H36C H 0.4610 0.1139 0.8124 0.033 Uiso 1 1 calc R . . O1 O 0.6640(2) 0.27766(11) 0.99238(12) 0.0154(6) Uani 1 1 d . . . O2 O 0.5125(2) 0.19816(11) 0.94306(12) 0.0148(5) Uani 1 1 d . . . O3 O 0.7237(2) 0.23007(12) 0.88417(13) 0.0171(6) Uani 1 1 d . . . O4 O 0.3856(2) 0.36333(12) 1.00145(12) 0.0159(6) Uani 1 1 d . . . O5 O 0.6411(2) 0.41447(12) 0.91907(12) 0.0174(6) Uani 1 1 d . . . O6 O 0.2735(2) 0.27291(11) 0.95145(12) 0.0158(6) Uani 1 1 d . . . O7 O 0.2619(2) 0.37380(11) 0.89213(12) 0.0152(6) Uani 1 1 d . . . O8 O 0.2583(2) 0.27151(11) 0.81486(12) 0.0158(6) Uani 1 1 d . . . O9 O 0.4816(2) 0.30378(11) 0.87412(12) 0.0122(5) Uani 1 1 d . . . O10 O 0.4832(2) 0.41637(11) 0.81965(12) 0.0161(6) Uani 1 1 d . . . O11 O 0.7094(2) 0.36221(12) 0.81471(13) 0.0185(6) Uani 1 1 d . . . O12 O 0.4883(2) 0.20075(12) 0.80635(12) 0.0161(6) Uani 1 1 d . . . O13 O 0.4816(2) 0.31499(12) 0.74459(12) 0.0155(6) Uani 1 1 d . . . Cl1 Cl -0.00516(10) -0.01144(5) 0.91180(5) 0.0264(2) Uani 1 1 d . . . Cl2 Cl -0.07360(11) 0.48023(5) 0.60862(5) 0.0351(3) Uani 1 1 d . . . 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 Sb1 0.01516(13) 0.01203(13) 0.01537(13) 0.00000(11) -0.00367(10) -0.00057(10) Sb2 0.01436(13) 0.01202(13) 0.01398(12) 0.00121(11) -0.00411(9) -0.00008(10) Co1 0.0140(3) 0.0129(3) 0.0148(3) 0.0008(2) -0.0022(2) 0.0001(2) Co2 0.0188(3) 0.0144(3) 0.0133(2) -0.0009(2) -0.0029(2) 0.0024(2) P1 0.0158(5) 0.0126(5) 0.0153(5) 0.0002(4) -0.0045(4) -0.0001(4) P2 0.0142(5) 0.0131(5) 0.0156(5) -0.0002(4) -0.0022(4) -0.0005(4) P3 0.0148(5) 0.0150(5) 0.0172(5) 0.0025(4) -0.0035(4) -0.0019(4) N1 0.0261(19) 0.025(2) 0.0204(18) -0.0025(16) -0.0007(15) 0.0022(16) N2 0.0186(17) 0.0138(17) 0.0187(17) -0.0034(15) 0.0014(13) -0.0017(14) C1 0.0140(18) 0.0110(19) 0.0197(19) -0.0024(16) -0.0020(15) 0.0021(15) C2 0.019(2) 0.020(2) 0.0158(19) 0.0004(17) -0.0046(16) -0.0025(17) C3 0.024(2) 0.015(2) 0.0184(19) 0.0051(17) 0.0004(16) -0.0022(17) C4 0.019(2) 0.016(2) 0.021(2) -0.0066(17) 0.0070(16) -0.0024(16) C5 0.021(2) 0.023(2) 0.020(2) -0.0019(18) -0.0075(16) -0.0022(18) C6 0.025(2) 0.019(2) 0.024(2) -0.0005(19) -0.0057(17) -0.0020(17) C7 0.0165(19) 0.014(2) 0.0142(18) -0.0006(16) -0.0035(15) 0.0009(16) C8 0.022(2) 0.021(2) 0.032(2) 0.003(2) -0.0074(18) 0.0001(18) C9 0.025(2) 0.017(2) 0.042(3) 0.001(2) -0.011(2) -0.0037(18) C10 0.026(2) 0.023(2) 0.017(2) -0.0019(18) -0.0057(17) 0.0091(18) C11 0.028(2) 0.023(2) 0.020(2) 0.0105(19) 0.0004(17) 0.0033(19) C12 0.0120(19) 0.025(2) 0.0182(19) -0.0011(18) -0.0027(15) 0.0018(16) C13 0.026(2) 0.031(3) 0.034(3) -0.002(2) -0.001(2) -0.003(2) C14 0.037(3) 0.045(3) 0.022(2) -0.002(2) 0.003(2) -0.012(2) C15 0.028(2) 0.043(3) 0.036(3) -0.013(2) 0.008(2) -0.004(2) C16 0.032(3) 0.036(3) 0.038(3) -0.005(2) 0.005(2) 0.002(2) C17 0.029(2) 0.033(3) 0.028(2) -0.003(2) 0.0001(19) 0.002(2) C18 0.021(2) 0.019(2) 0.024(2) 0.0000(18) -0.0007(17) -0.0004(17) C19 0.034(2) 0.021(2) 0.030(2) -0.006(2) 0.0026(19) -0.0057(19) C20 0.022(2) 0.028(2) 0.023(2) -0.011(2) -0.0027(17) -0.0010(18) C21 0.030(2) 0.026(2) 0.018(2) -0.0049(19) -0.0055(18) 0.0012(19) C22 0.022(2) 0.016(2) 0.021(2) -0.0015(18) -0.0040(16) -0.0007(17) C23 0.019(2) 0.012(2) 0.021(2) 0.0039(17) -0.0047(16) 0.0014(16) C24 0.031(2) 0.018(2) 0.041(3) -0.003(2) -0.015(2) 0.0046(19) C25 0.026(2) 0.028(2) 0.020(2) 0.009(2) -0.0032(17) 0.0021(19) C26 0.021(2) 0.024(2) 0.022(2) 0.0060(19) -0.0108(17) 0.0045(18) C27 0.0159(19) 0.016(2) 0.0191(19) -0.0045(17) 0.0017(15) -0.0017(16) C28 0.021(2) 0.039(3) 0.020(2) 0.003(2) 0.0036(17) 0.001(2) C29 0.019(2) 0.033(3) 0.026(2) 0.002(2) -0.0034(17) -0.0024(19) C30 0.021(2) 0.024(2) 0.038(3) -0.009(2) 0.0010(19) 0.0052(18) C31 0.018(2) 0.020(2) 0.021(2) 0.0029(18) -0.0037(16) -0.0021(17) C32 0.028(2) 0.015(2) 0.042(3) 0.004(2) -0.006(2) -0.0009(18) C33 0.030(2) 0.026(2) 0.021(2) 0.0161(19) -0.0017(18) -0.0060(19) C34 0.020(2) 0.025(2) 0.030(2) 0.003(2) -0.0038(18) -0.0068(18) C35 0.029(2) 0.034(3) 0.020(2) -0.003(2) -0.0062(18) 0.001(2) C36 0.025(2) 0.017(2) 0.024(2) -0.0074(18) -0.0087(17) 0.0058(17) O1 0.0163(13) 0.0151(14) 0.0144(13) 0.0004(11) -0.0057(10) -0.0001(11) O2 0.0177(13) 0.0115(13) 0.0149(13) 0.0033(11) -0.0044(10) 0.0008(11) O3 0.0127(13) 0.0187(14) 0.0197(14) 0.0021(12) -0.0038(10) -0.0009(11) O4 0.0131(13) 0.0205(15) 0.0139(13) -0.0051(12) -0.0012(10) 0.0003(11) O5 0.0181(14) 0.0167(14) 0.0172(13) 0.0014(12) -0.0042(11) -0.0050(11) O6 0.0157(13) 0.0147(14) 0.0169(13) 0.0000(12) 0.0004(11) 0.0003(11) O7 0.0181(13) 0.0122(13) 0.0153(13) 0.0013(11) 0.0001(11) 0.0033(11) O8 0.0150(13) 0.0152(14) 0.0169(13) 0.0003(12) -0.0076(10) -0.0011(11) O9 0.0129(12) 0.0095(13) 0.0139(13) 0.0046(11) -0.0044(10) -0.0005(10) O10 0.0125(13) 0.0142(14) 0.0213(14) 0.0018(12) -0.0051(11) 0.0012(11) O11 0.0181(14) 0.0193(15) 0.0178(14) 0.0026(12) -0.0029(11) -0.0019(11) O12 0.0193(13) 0.0160(14) 0.0129(13) -0.0008(12) -0.0010(11) 0.0010(11) O13 0.0187(13) 0.0174(14) 0.0102(12) -0.0002(11) -0.0015(10) 0.0003(11) Cl1 0.0298(5) 0.0212(5) 0.0281(5) 0.0003(5) 0.0004(4) -0.0099(4) Cl2 0.0352(6) 0.0384(7) 0.0308(6) 0.0092(5) -0.0144(5) 0.0103(5) _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 Sb1 O8 1.970(2) . ? Sb1 O2 2.003(2) . ? Sb1 O9 2.023(2) . ? Sb1 O12 2.024(2) . ? Sb1 O6 2.054(3) . ? Sb1 C1 2.102(4) . ? Sb1 Sb2 3.0303(4) . ? Sb2 O8 1.975(3) . ? Sb2 O10 1.995(3) . ? Sb2 O13 2.011(2) . ? Sb2 O9 2.017(2) . ? Sb2 O7 2.023(2) . ? Sb2 C7 2.105(4) . ? Co1 O5 1.935(3) . ? Co1 O1 1.945(3) . ? Co1 O4 1.980(2) . ? Co1 N2 2.110(3) . ? Co2 O11 2.026(3) . ? Co2 O3 2.036(3) . ? Co2 N1 2.078(3) . ? Co2 O9 2.129(2) . ? Co2 O13 2.180(2) . ? Co2 O12 2.282(3) . ? P1 O3 1.510(3) . ? P1 O1 1.521(3) . ? P1 O2 1.584(3) . ? P1 C23 1.815(4) . ? P2 O4 1.509(3) . ? P2 O6 1.556(3) . ? P2 O7 1.561(3) . ? P2 C27 1.810(4) . ? P3 O11 1.516(3) . ? P3 O5 1.519(3) . ? P3 O10 1.588(3) . ? P3 C31 1.820(4) . ? N1 C17 1.336(5) . ? N1 C13 1.367(6) . ? N2 C18 1.320(5) . ? N2 C22 1.344(5) . ? C1 C6 1.385(5) . ? C1 C2 1.390(5) . ? C2 C3 1.391(5) . ? C2 H2 0.9500 . ? C3 C4 1.383(5) . ? C3 H3 0.9500 . ? C4 C5 1.383(6) . ? C4 Cl1 1.740(4) . ? C5 C6 1.394(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.370(5) . ? C7 C8 1.390(5) . ? C8 C9 1.388(6) . ? C8 H8 0.9500 . ? C9 C10 1.377(6) . ? C9 H9 0.9500 . ? C10 C11 1.368(6) . ? C10 Cl2 1.745(4) . ? C11 C12 1.393(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.375(6) . ? C13 H13 0.9500 . ? C14 C15 1.388(7) . ? C14 H14 0.9500 . ? C15 C16 1.376(7) . ? C15 H15 0.9500 . ? C16 C17 1.401(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.382(6) . ? C18 H18 0.9500 . ? C19 C20 1.380(6) . ? C19 H19 0.9500 . ? C20 C21 1.369(6) . ? C20 H20 0.9500 . ? C21 C22 1.379(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C25 1.520(5) . ? C23 C24 1.531(5) . ? C23 C26 1.541(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.533(5) . ? C27 C30 1.535(5) . ? C27 C29 1.544(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.526(5) . ? C31 C32 1.528(6) . ? C31 C34 1.533(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 O13 1.437(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 O12 1.423(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 O8 Sb1 O2 168.46(10) . . ? O8 Sb1 O9 81.15(10) . . ? O2 Sb1 O9 87.41(10) . . ? O8 Sb1 O12 88.62(10) . . ? O2 Sb1 O12 88.70(10) . . ? O9 Sb1 O12 84.05(10) . . ? O8 Sb1 O6 88.52(10) . . ? O2 Sb1 O6 91.82(10) . . ? O9 Sb1 O6 84.10(10) . . ? O12 Sb1 O6 168.10(10) . . ? O8 Sb1 C1 99.68(12) . . ? O2 Sb1 C1 91.84(12) . . ? O9 Sb1 C1 176.08(12) . . ? O12 Sb1 C1 99.79(13) . . ? O6 Sb1 C1 92.08(12) . . ? O8 Sb1 Sb2 39.89(7) . . ? O2 Sb1 Sb2 128.73(7) . . ? O9 Sb1 Sb2 41.33(7) . . ? O12 Sb1 Sb2 87.04(7) . . ? O6 Sb1 Sb2 83.36(7) . . ? C1 Sb1 Sb2 139.18(10) . . ? O8 Sb2 O10 168.60(10) . . ? O8 Sb2 O13 91.32(11) . . ? O10 Sb2 O13 86.97(10) . . ? O8 Sb2 O9 81.17(10) . . ? O10 Sb2 O9 87.44(10) . . ? O13 Sb2 O9 83.27(10) . . ? O8 Sb2 O7 88.82(10) . . ? O10 Sb2 O7 90.49(10) . . ? O13 Sb2 O7 167.81(10) . . ? O9 Sb2 O7 84.71(10) . . ? O8 Sb2 C7 97.57(12) . . ? O10 Sb2 C7 93.83(12) . . ? O13 Sb2 C7 99.24(12) . . ? O9 Sb2 C7 177.24(12) . . ? O7 Sb2 C7 92.82(12) . . ? O8 Sb2 Sb1 39.76(7) . . ? O10 Sb2 Sb1 128.88(7) . . ? O13 Sb2 Sb1 88.36(7) . . ? O9 Sb2 Sb1 41.48(7) . . ? O7 Sb2 Sb1 83.97(7) . . ? C7 Sb2 Sb1 137.09(10) . . ? O5 Co1 O1 124.56(11) . . ? O5 Co1 O4 114.58(11) . . ? O1 Co1 O4 118.58(11) . . ? O5 Co1 N2 94.36(12) . . ? O1 Co1 N2 91.88(11) . . ? O4 Co1 N2 99.22(11) . . ? O11 Co2 O3 108.82(11) . . ? O11 Co2 N1 93.64(13) . . ? O3 Co2 N1 98.94(12) . . ? O11 Co2 O9 88.98(10) . . ? O3 Co2 O9 88.97(10) . . ? N1 Co2 O9 170.36(11) . . ? O11 Co2 O13 85.16(10) . . ? O3 Co2 O13 160.03(10) . . ? N1 Co2 O13 94.18(12) . . ? O9 Co2 O13 76.77(9) . . ? O11 Co2 O12 160.71(10) . . ? O3 Co2 O12 82.97(10) . . ? N1 Co2 O12 99.66(12) . . ? O9 Co2 O12 75.71(9) . . ? O13 Co2 O12 80.02(9) . . ? O3 P1 O1 114.92(15) . . ? O3 P1 O2 111.15(14) . . ? O1 P1 O2 109.08(14) . . ? O3 P1 C23 109.94(17) . . ? O1 P1 C23 107.81(16) . . ? O2 P1 C23 103.25(16) . . ? O4 P2 O6 110.86(15) . . ? O4 P2 O7 111.60(15) . . ? O6 P2 O7 111.75(15) . . ? O4 P2 C27 111.62(16) . . ? O6 P2 C27 106.24(16) . . ? O7 P2 C27 104.48(16) . . ? O11 P3 O5 114.80(15) . . ? O11 P3 O10 110.87(15) . . ? O5 P3 O10 109.52(15) . . ? O11 P3 C31 109.69(17) . . ? O5 P3 C31 107.26(17) . . ? O10 P3 C31 104.11(16) . . ? C17 N1 C13 118.2(4) . . ? C17 N1 Co2 123.3(3) . . ? C13 N1 Co2 118.3(3) . . ? C18 N2 C22 118.0(3) . . ? C18 N2 Co1 121.2(3) . . ? C22 N2 Co1 120.8(3) . . ? C6 C1 C2 119.5(4) . . ? C6 C1 Sb1 119.2(3) . . ? C2 C1 Sb1 121.3(3) . . ? C1 C2 C3 120.6(4) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 119.0(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C5 C4 C3 121.3(4) . . ? C5 C4 Cl1 119.4(3) . . ? C3 C4 Cl1 119.3(3) . . ? C4 C5 C6 119.1(4) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C1 C6 C5 120.5(4) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C12 C7 C8 120.2(4) . . ? C12 C7 Sb2 121.6(3) . . ? C8 C7 Sb2 118.2(3) . . ? C9 C8 C7 119.4(4) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 119.4(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 121.8(4) . . ? C11 C10 Cl2 119.0(3) . . ? C9 C10 Cl2 119.2(3) . . ? C10 C11 C12 118.6(4) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C7 C12 C11 120.6(4) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? N1 C13 C14 122.6(4) . . ? N1 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C13 C14 C15 118.8(5) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 119.0(4) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 119.7(5) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N1 C17 C16 121.6(4) . . ? N1 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? N2 C18 C19 123.5(4) . . ? N2 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? C20 C19 C18 117.9(4) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? C21 C20 C19 119.4(4) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 118.9(4) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N2 C22 C21 122.3(4) . . ? N2 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C25 C23 C24 109.0(3) . . ? C25 C23 C26 110.1(3) . . ? C24 C23 C26 109.3(3) . . ? C25 C23 P1 109.1(3) . . ? C24 C23 P1 110.6(3) . . ? C26 C23 P1 108.6(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C30 109.7(3) . . ? C28 C27 C29 110.5(3) . . ? C30 C27 C29 109.4(3) . . ? C28 C27 P2 109.4(3) . . ? C30 C27 P2 109.5(3) . . ? C29 C27 P2 108.2(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 109.1(3) . . ? C33 C31 C34 109.8(3) . . ? C32 C31 C34 110.5(3) . . ? C33 C31 P3 109.5(3) . . ? C32 C31 P3 109.8(3) . . ? C34 C31 P3 108.0(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O13 C35 H35A 109.5 . . ? O13 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O13 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O12 C36 H36A 109.5 . . ? O12 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O12 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P1 O1 Co1 129.39(15) . . ? P1 O2 Sb1 125.11(15) . . ? P1 O3 Co2 123.86(15) . . ? P2 O4 Co1 122.98(15) . . ? P3 O5 Co1 127.50(16) . . ? P2 O6 Sb1 125.28(15) . . ? P2 O7 Sb2 125.69(15) . . ? Sb1 O8 Sb2 100.36(11) . . ? Sb2 O9 Sb1 97.19(10) . . ? Sb2 O9 Co2 100.18(10) . . ? Sb1 O9 Co2 101.95(11) . . ? P3 O10 Sb2 125.99(15) . . ? P3 O11 Co2 124.00(15) . . ? C36 O12 Sb1 121.9(2) . . ? C36 O12 Co2 121.0(2) . . ? Sb1 O12 Co2 96.87(10) . . ? C35 O13 Sb2 118.9(2) . . ? C35 O13 Co2 124.0(2) . . ? Sb2 O13 Co2 98.66(10) . . ? 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 O2 Sb1 Sb2 O8 177.34(15) . . . . ? O9 Sb1 Sb2 O8 175.73(16) . . . . ? O12 Sb1 Sb2 O8 91.38(14) . . . . ? O6 Sb1 Sb2 O8 -95.66(14) . . . . ? C1 Sb1 Sb2 O8 -10.19(19) . . . . ? O8 Sb1 Sb2 O10 -178.82(15) . . . . ? O2 Sb1 Sb2 O10 -1.48(13) . . . . ? O9 Sb1 Sb2 O10 -3.09(14) . . . . ? O12 Sb1 Sb2 O10 -87.44(12) . . . . ? O6 Sb1 Sb2 O10 85.52(12) . . . . ? C1 Sb1 Sb2 O10 170.99(18) . . . . ? O8 Sb1 Sb2 O13 -94.05(14) . . . . ? O2 Sb1 Sb2 O13 83.29(12) . . . . ? O9 Sb1 Sb2 O13 81.68(13) . . . . ? O12 Sb1 Sb2 O13 -2.67(10) . . . . ? O6 Sb1 Sb2 O13 170.29(10) . . . . ? C1 Sb1 Sb2 O13 -104.24(17) . . . . ? O8 Sb1 Sb2 O9 -175.73(16) . . . . ? O2 Sb1 Sb2 O9 1.61(14) . . . . ? O12 Sb1 Sb2 O9 -84.35(13) . . . . ? O6 Sb1 Sb2 O9 88.61(13) . . . . ? C1 Sb1 Sb2 O9 174.08(19) . . . . ? O8 Sb1 Sb2 O7 95.44(14) . . . . ? O2 Sb1 Sb2 O7 -87.22(12) . . . . ? O9 Sb1 Sb2 O7 -88.83(13) . . . . ? O12 Sb1 Sb2 O7 -173.18(10) . . . . ? O6 Sb1 Sb2 O7 -0.22(10) . . . . ? C1 Sb1 Sb2 O7 85.25(17) . . . . ? O8 Sb1 Sb2 C7 7.79(19) . . . . ? O2 Sb1 Sb2 C7 -174.87(17) . . . . ? O9 Sb1 Sb2 C7 -176.48(18) . . . . ? O12 Sb1 Sb2 C7 99.18(16) . . . . ? O6 Sb1 Sb2 C7 -87.87(16) . . . . ? C1 Sb1 Sb2 C7 -2.4(2) . . . . ? O11 Co2 N1 C17 119.1(3) . . . . ? O3 Co2 N1 C17 9.4(4) . . . . ? O9 Co2 N1 C17 -135.4(7) . . . . ? O13 Co2 N1 C17 -155.5(3) . . . . ? O12 Co2 N1 C17 -74.9(3) . . . . ? O11 Co2 N1 C13 -56.6(3) . . . . ? O3 Co2 N1 C13 -166.3(3) . . . . ? O9 Co2 N1 C13 48.9(9) . . . . ? O13 Co2 N1 C13 28.8(3) . . . . ? O12 Co2 N1 C13 109.4(3) . . . . ? O5 Co1 N2 C18 36.0(3) . . . . ? O1 Co1 N2 C18 160.9(3) . . . . ? O4 Co1 N2 C18 -79.8(3) . . . . ? O5 Co1 N2 C22 -142.8(3) . . . . ? O1 Co1 N2 C22 -17.9(3) . . . . ? O4 Co1 N2 C22 101.4(3) . . . . ? O8 Sb1 C1 C6 13.2(3) . . . . ? O2 Sb1 C1 C6 -166.1(3) . . . . ? O9 Sb1 C1 C6 115.1(17) . . . . ? O12 Sb1 C1 C6 -77.1(3) . . . . ? O6 Sb1 C1 C6 102.0(3) . . . . ? Sb2 Sb1 C1 C6 19.8(4) . . . . ? O8 Sb1 C1 C2 -164.7(3) . . . . ? O2 Sb1 C1 C2 16.0(3) . . . . ? O9 Sb1 C1 C2 -62.8(19) . . . . ? O12 Sb1 C1 C2 105.0(3) . . . . ? O6 Sb1 C1 C2 -75.9(3) . . . . ? Sb2 Sb1 C1 C2 -158.1(2) . . . . ? C6 C1 C2 C3 1.8(6) . . . . ? Sb1 C1 C2 C3 179.7(3) . . . . ? C1 C2 C3 C4 -0.5(6) . . . . ? C2 C3 C4 C5 -0.2(6) . . . . ? C2 C3 C4 Cl1 176.8(3) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? Cl1 C4 C5 C6 -177.3(3) . . . . ? C2 C1 C6 C5 -2.3(6) . . . . ? Sb1 C1 C6 C5 179.7(3) . . . . ? C4 C5 C6 C1 1.6(6) . . . . ? O8 Sb2 C7 C12 -161.8(3) . . . . ? O10 Sb2 C7 C12 18.4(3) . . . . ? O13 Sb2 C7 C12 -69.2(3) . . . . ? O9 Sb2 C7 C12 136(2) . . . . ? O7 Sb2 C7 C12 109.0(3) . . . . ? Sb1 Sb2 C7 C12 -166.8(2) . . . . ? O8 Sb2 C7 C8 17.1(3) . . . . ? O10 Sb2 C7 C8 -162.8(3) . . . . ? O13 Sb2 C7 C8 109.6(3) . . . . ? O9 Sb2 C7 C8 -46(3) . . . . ? O7 Sb2 C7 C8 -72.1(3) . . . . ? Sb1 Sb2 C7 C8 12.0(4) . . . . ? C12 C7 C8 C9 0.8(6) . . . . ? Sb2 C7 C8 C9 -178.1(3) . . . . ? C7 C8 C9 C10 1.0(7) . . . . ? C8 C9 C10 C11 -2.9(7) . . . . ? C8 C9 C10 Cl2 176.7(3) . . . . ? C9 C10 C11 C12 2.9(6) . . . . ? Cl2 C10 C11 C12 -176.6(3) . . . . ? C8 C7 C12 C11 -0.7(6) . . . . ? Sb2 C7 C12 C11 178.1(3) . . . . ? C10 C11 C12 C7 -1.1(6) . . . . ? C17 N1 C13 C14 3.8(6) . . . . ? Co2 N1 C13 C14 179.7(3) . . . . ? N1 C13 C14 C15 -2.7(7) . . . . ? C13 C14 C15 C16 0.7(7) . . . . ? C14 C15 C16 C17 0.0(7) . . . . ? C13 N1 C17 C16 -3.0(6) . . . . ? Co2 N1 C17 C16 -178.7(3) . . . . ? C15 C16 C17 N1 1.2(7) . . . . ? C22 N2 C18 C19 -1.5(6) . . . . ? Co1 N2 C18 C19 179.7(3) . . . . ? N2 C18 C19 C20 0.4(6) . . . . ? C18 C19 C20 C21 0.2(6) . . . . ? C19 C20 C21 C22 0.3(6) . . . . ? C18 N2 C22 C21 2.1(6) . . . . ? Co1 N2 C22 C21 -179.1(3) . . . . ? C20 C21 C22 N2 -1.5(6) . . . . ? O3 P1 C23 C25 -179.3(3) . . . . ? O1 P1 C23 C25 54.7(3) . . . . ? O2 P1 C23 C25 -60.6(3) . . . . ? O3 P1 C23 C24 -59.3(3) . . . . ? O1 P1 C23 C24 174.7(3) . . . . ? O2 P1 C23 C24 59.3(3) . . . . ? O3 P1 C23 C26 60.6(3) . . . . ? O1 P1 C23 C26 -65.3(3) . . . . ? O2 P1 C23 C26 179.3(3) . . . . ? O4 P2 C27 C28 -60.4(3) . . . . ? O6 P2 C27 C28 60.6(3) . . . . ? O7 P2 C27 C28 178.9(3) . . . . ? O4 P2 C27 C30 59.9(3) . . . . ? O6 P2 C27 C30 -179.1(3) . . . . ? O7 P2 C27 C30 -60.8(3) . . . . ? O4 P2 C27 C29 179.2(3) . . . . ? O6 P2 C27 C29 -59.9(3) . . . . ? O7 P2 C27 C29 58.4(3) . . . . ? O11 P3 C31 C33 59.8(3) . . . . ? O5 P3 C31 C33 -174.9(3) . . . . ? O10 P3 C31 C33 -58.9(3) . . . . ? O11 P3 C31 C32 179.6(3) . . . . ? O5 P3 C31 C32 -55.1(3) . . . . ? O10 P3 C31 C32 60.9(3) . . . . ? O11 P3 C31 C34 -59.8(3) . . . . ? O5 P3 C31 C34 65.5(3) . . . . ? O10 P3 C31 C34 -178.5(3) . . . . ? O3 P1 O1 Co1 62.5(2) . . . . ? O2 P1 O1 Co1 -63.1(2) . . . . ? C23 P1 O1 Co1 -174.55(19) . . . . ? O5 Co1 O1 P1 -77.4(2) . . . . ? O4 Co1 O1 P1 84.4(2) . . . . ? N2 Co1 O1 P1 -174.0(2) . . . . ? O3 P1 O2 Sb1 -45.0(2) . . . . ? O1 P1 O2 Sb1 82.8(2) . . . . ? C23 P1 O2 Sb1 -162.79(19) . . . . ? O8 Sb1 O2 P1 -13.5(6) . . . . ? O9 Sb1 O2 P1 -20.97(18) . . . . ? O12 Sb1 O2 P1 63.13(19) . . . . ? O6 Sb1 O2 P1 -104.98(18) . . . . ? C1 Sb1 O2 P1 162.9(2) . . . . ? Sb2 Sb1 O2 P1 -22.0(2) . . . . ? O1 P1 O3 Co2 -70.9(2) . . . . ? O2 P1 O3 Co2 53.6(2) . . . . ? C23 P1 O3 Co2 167.28(18) . . . . ? O11 Co2 O3 P1 92.98(19) . . . . ? N1 Co2 O3 P1 -170.04(19) . . . . ? O9 Co2 O3 P1 4.41(19) . . . . ? O13 Co2 O3 P1 -39.6(4) . . . . ? O12 Co2 O3 P1 -71.32(18) . . . . ? O6 P2 O4 Co1 62.6(2) . . . . ? O7 P2 O4 Co1 -62.6(2) . . . . ? C27 P2 O4 Co1 -179.14(18) . . . . ? O5 Co1 O4 P2 83.3(2) . . . . ? O1 Co1 O4 P2 -80.3(2) . . . . ? N2 Co1 O4 P2 -177.57(19) . . . . ? O11 P3 O5 Co1 -59.3(2) . . . . ? O10 P3 O5 Co1 66.2(2) . . . . ? C31 P3 O5 Co1 178.55(19) . . . . ? O1 Co1 O5 P3 72.8(2) . . . . ? O4 Co1 O5 P3 -89.6(2) . . . . ? N2 Co1 O5 P3 168.1(2) . . . . ? O4 P2 O6 Sb1 -89.57(19) . . . . ? O7 P2 O6 Sb1 35.6(2) . . . . ? C27 P2 O6 Sb1 148.98(18) . . . . ? O8 Sb1 O6 P2 -58.70(18) . . . . ? O2 Sb1 O6 P2 109.76(18) . . . . ? O9 Sb1 O6 P2 22.56(17) . . . . ? O12 Sb1 O6 P2 17.4(6) . . . . ? C1 Sb1 O6 P2 -158.33(19) . . . . ? Sb2 Sb1 O6 P2 -19.03(16) . . . . ? O4 P2 O7 Sb2 88.7(2) . . . . ? O6 P2 O7 Sb2 -36.1(2) . . . . ? C27 P2 O7 Sb2 -150.58(18) . . . . ? O8 Sb2 O7 P2 59.14(18) . . . . ? O10 Sb2 O7 P2 -109.48(18) . . . . ? O13 Sb2 O7 P2 -31.7(6) . . . . ? O9 Sb2 O7 P2 -22.10(18) . . . . ? C7 Sb2 O7 P2 156.7(2) . . . . ? Sb1 Sb2 O7 P2 19.59(16) . . . . ? O2 Sb1 O8 Sb2 -10.4(6) . . . . ? O9 Sb1 O8 Sb2 -2.85(11) . . . . ? O12 Sb1 O8 Sb2 -87.04(12) . . . . ? O6 Sb1 O8 Sb2 81.41(11) . . . . ? C1 Sb1 O8 Sb2 173.26(13) . . . . ? O10 Sb2 O8 Sb1 4.7(6) . . . . ? O13 Sb2 O8 Sb1 85.84(11) . . . . ? O9 Sb2 O8 Sb1 2.86(11) . . . . ? O7 Sb2 O8 Sb1 -81.97(11) . . . . ? C7 Sb2 O8 Sb1 -174.66(13) . . . . ? O8 Sb2 O9 Sb1 -2.76(10) . . . . ? O10 Sb2 O9 Sb1 177.59(11) . . . . ? O13 Sb2 O9 Sb1 -95.16(11) . . . . ? O7 Sb2 O9 Sb1 86.87(11) . . . . ? C7 Sb2 O9 Sb1 60(3) . . . . ? O8 Sb2 O9 Co2 100.81(11) . . . . ? O10 Sb2 O9 Co2 -78.83(11) . . . . ? O13 Sb2 O9 Co2 8.41(10) . . . . ? O7 Sb2 O9 Co2 -169.56(11) . . . . ? C7 Sb2 O9 Co2 164(3) . . . . ? Sb1 Sb2 O9 Co2 103.57(13) . . . . ? O8 Sb1 O9 Sb2 2.77(10) . . . . ? O2 Sb1 O9 Sb2 -178.74(11) . . . . ? O12 Sb1 O9 Sb2 92.29(11) . . . . ? O6 Sb1 O9 Sb2 -86.65(11) . . . . ? C1 Sb1 O9 Sb2 -99.7(17) . . . . ? O8 Sb1 O9 Co2 -99.28(11) . . . . ? O2 Sb1 O9 Co2 79.21(11) . . . . ? O12 Sb1 O9 Co2 -9.76(10) . . . . ? O6 Sb1 O9 Co2 171.31(11) . . . . ? C1 Sb1 O9 Co2 158.2(17) . . . . ? Sb2 Sb1 O9 Co2 -102.05(12) . . . . ? O11 Co2 O9 Sb2 77.35(11) . . . . ? O3 Co2 O9 Sb2 -173.81(11) . . . . ? N1 Co2 O9 Sb2 -28.5(8) . . . . ? O13 Co2 O9 Sb2 -7.91(10) . . . . ? O12 Co2 O9 Sb2 -90.79(10) . . . . ? O11 Co2 O9 Sb1 177.02(11) . . . . ? O3 Co2 O9 Sb1 -74.14(11) . . . . ? N1 Co2 O9 Sb1 71.2(8) . . . . ? O13 Co2 O9 Sb1 91.76(11) . . . . ? O12 Co2 O9 Sb1 8.88(9) . . . . ? O11 P3 O10 Sb2 45.2(2) . . . . ? O5 P3 O10 Sb2 -82.5(2) . . . . ? C31 P3 O10 Sb2 163.07(19) . . . . ? O8 Sb2 O10 P3 17.6(7) . . . . ? O13 Sb2 O10 P3 -63.99(19) . . . . ? O9 Sb2 O10 P3 19.40(19) . . . . ? O7 Sb2 O10 P3 104.08(19) . . . . ? C7 Sb2 O10 P3 -163.1(2) . . . . ? Sb1 Sb2 O10 P3 21.4(2) . . . . ? O5 P3 O11 Co2 76.2(2) . . . . ? O10 P3 O11 Co2 -48.5(2) . . . . ? C31 P3 O11 Co2 -162.93(18) . . . . ? O3 Co2 O11 P3 -98.58(19) . . . . ? N1 Co2 O11 P3 160.69(19) . . . . ? O9 Co2 O11 P3 -10.02(18) . . . . ? O13 Co2 O11 P3 66.79(18) . . . . ? O12 Co2 O11 P3 27.0(4) . . . . ? O8 Sb1 O12 C36 -136.4(3) . . . . ? O2 Sb1 O12 C36 54.8(3) . . . . ? O9 Sb1 O12 C36 142.4(3) . . . . ? O6 Sb1 O12 C36 147.5(4) . . . . ? C1 Sb1 O12 C36 -36.8(3) . . . . ? Sb2 Sb1 O12 C36 -176.3(3) . . . . ? O8 Sb1 O12 Co2 90.21(10) . . . . ? O2 Sb1 O12 Co2 -78.56(10) . . . . ? O9 Sb1 O12 Co2 8.96(9) . . . . ? O6 Sb1 O12 Co2 14.1(5) . . . . ? C1 Sb1 O12 Co2 -170.21(12) . . . . ? Sb2 Sb1 O12 Co2 50.32(7) . . . . ? O11 Co2 O12 C36 178.8(3) . . . . ? O3 Co2 O12 C36 -52.0(3) . . . . ? N1 Co2 O12 C36 45.9(3) . . . . ? O9 Co2 O12 C36 -142.7(3) . . . . ? O13 Co2 O12 C36 138.5(3) . . . . ? O11 Co2 O12 Sb1 -47.2(3) . . . . ? O3 Co2 O12 Sb1 81.99(11) . . . . ? N1 Co2 O12 Sb1 179.91(12) . . . . ? O9 Co2 O12 Sb1 -8.74(9) . . . . ? O13 Co2 O12 Sb1 -87.50(10) . . . . ? O8 Sb2 O13 C35 47.8(3) . . . . ? O10 Sb2 O13 C35 -143.5(3) . . . . ? O9 Sb2 O13 C35 128.8(3) . . . . ? O7 Sb2 O13 C35 138.4(5) . . . . ? C7 Sb2 O13 C35 -50.1(3) . . . . ? Sb1 Sb2 O13 C35 87.5(3) . . . . ? O8 Sb2 O13 Co2 -89.12(11) . . . . ? O10 Sb2 O13 Co2 79.61(11) . . . . ? O9 Sb2 O13 Co2 -8.17(10) . . . . ? O7 Sb2 O13 Co2 1.4(5) . . . . ? C7 Sb2 O13 Co2 172.99(12) . . . . ? Sb1 Sb2 O13 Co2 -49.47(8) . . . . ? O11 Co2 O13 C35 144.0(3) . . . . ? O3 Co2 O13 C35 -80.4(4) . . . . ? N1 Co2 O13 C35 50.7(3) . . . . ? O9 Co2 O13 C35 -125.9(3) . . . . ? O12 Co2 O13 C35 -48.4(3) . . . . ? O11 Co2 O13 Sb2 -82.19(11) . . . . ? O3 Co2 O13 Sb2 53.4(3) . . . . ? N1 Co2 O13 Sb2 -175.49(13) . . . . ? O9 Co2 O13 Sb2 7.90(10) . . . . ? O12 Co2 O13 Sb2 85.43(11) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.526 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.121