# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'R. Winpenny' _publ_contact_author_email RICHARD.WINPENNY@MANCHESTER.AC.UK _publ_section_title ; Mixed Antimonate-Phosphonate Ligands as Polydentate Bridging Oxygen Donors ; loop_ _publ_author_name 'R. Winpenny' 'Shoaib Ali' 'Viswanathan Baskar' 'Christopher A. Muryn' # Attachment '1.cif' data_testnew _database_code_depnum_ccdc_archive 'CCDC 700894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H66 Cl14 O26 P8 Sb4' _chemical_formula_weight 2638.36 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' 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 13.7395(10) _cell_length_b 15.1579(11) _cell_length_c 25.9751(13) _cell_angle_alpha 75.215(5) _cell_angle_beta 88.085(5) _cell_angle_gamma 72.951(6) _cell_volume 4995.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10993 _cell_measurement_theta_min 2.6087 _cell_measurement_theta_max 23.7511 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2596 _exptl_absorpt_coefficient_mu 1.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6842 _exptl_absorpt_correction_T_max 0.8530 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) 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 28051 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.1094 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 20.82 _reflns_number_total 10266 _reflns_number_gt 6590 _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 Crystal showed poor diffraction with statistically usable intensity to only 1 angstrom even with very long collection times. Although many crystals were selected it was not possible to choose a single crystal due to the plate like nature of the crystals and the collected data was from a crystal displaying multi diffraction peaks from a number of crystals This hindered the integration of the data which twin refinement did not improve. Restraining the abnormal thermal ellipsoids associated with O16 and O24 was attempted. This resulted in numerous atoms going NPD and was therefore not used. All the alerts in CheckCIF are attributable to the poor data quality. Residual Q-peaks around Sb were found which is typical for all these structures. The disorder in the molecule was modelled and all the carbons were left isotropic due to twinning of the crystal. 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^)+(0.1476P)^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 10266 _refine_ls_number_parameters 968 _refine_ls_number_restraints 739 _refine_ls_R_factor_all 0.1120 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.2234 _refine_ls_wR_factor_gt 0.2102 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.967 _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 0.37929(7) 0.51555(7) 0.29581(3) 0.0259(3) Uani 1 1 d . . . Sb2 Sb 0.55025(7) 0.56227(7) 0.19393(3) 0.0255(3) Uani 1 1 d . . . Sb3 Sb 0.58859(7) 0.18122(7) 0.24675(4) 0.0272(3) Uani 1 1 d . . . Sb4 Sb 0.74277(7) 0.22624(7) 0.33836(4) 0.0273(3) Uani 1 1 d . . . O3 O 0.4698(9) 0.2793(9) 0.4003(5) 0.032(2) Uani 0.751(3) 1 d PDU A 1 O4 O 0.6390(14) 0.3094(11) 0.3765(7) 0.028(2) Uani 0.751(3) 1 d PDU A 1 O5 O 0.4781(11) 0.4419(12) 0.3560(5) 0.028(2) Uani 0.751(3) 1 d PDU A 1 P1 P 0.5313(4) 0.3475(4) 0.39372(18) 0.0265(12) Uani 0.751(3) 1 d PDU A 1 C1 C 0.5541(12) 0.3688(13) 0.4560(4) 0.044(3) Uiso 0.751(3) 1 d PGDU A 1 C2 C 0.5076(11) 0.3283(11) 0.5003(6) 0.048(3) Uiso 0.751(3) 1 d PGDU A 1 H2 H 0.4633 0.2924 0.4968 0.057 Uiso 0.751(3) 1 calc PR A 1 C3 C 0.5261(11) 0.3405(11) 0.5500(4) 0.051(4) Uiso 0.751(3) 1 d PGDU A 1 H3 H 0.4944 0.3129 0.5803 0.061 Uiso 0.751(3) 1 calc PR A 1 C4 C 0.5911(12) 0.3931(12) 0.5552(4) 0.051(4) Uiso 0.751(3) 1 d PGDU A 1 H4 H 0.6037 0.4014 0.5892 0.061 Uiso 0.751(3) 1 calc PR A 1 C5 C 0.6375(11) 0.4335(12) 0.5109(6) 0.052(4) Uiso 0.751(3) 1 d PGDU A 1 H5 H 0.6819 0.4695 0.5144 0.062 Uiso 0.751(3) 1 calc PR A 1 C6 C 0.6191(12) 0.4214(12) 0.4612(5) 0.048(3) Uiso 0.751(3) 1 d PGDU A 1 H6 H 0.6508 0.4490 0.4309 0.058 Uiso 0.751(3) 1 calc PR A 1 O6 O 0.7768(15) 0.3424(15) 0.2936(6) 0.0305(19) Uani 0.751(3) 1 d PU A 1 O7 O 0.6871(12) 0.4974(13) 0.2309(8) 0.030(2) Uani 0.751(3) 1 d PU A 1 O8 O 0.7132(9) 0.4863(9) 0.3286(5) 0.032(3) Uani 0.751(3) 1 d PU A 1 P2 P 0.7561(4) 0.4487(4) 0.2813(2) 0.0308(12) Uani 0.751(3) 1 d PU A 1 C7 C 0.8743(11) 0.4716(14) 0.2628(7) 0.066(4) Uiso 0.751(3) 1 d PGU A 1 C8 C 0.9227(13) 0.5019(13) 0.2982(5) 0.071(4) Uiso 0.751(3) 1 d PGU A 1 H8 H 0.8942 0.5069 0.3316 0.085 Uiso 0.751(3) 1 calc PR A 1 C9 C 1.0126(14) 0.5249(13) 0.2848(6) 0.073(4) Uiso 0.751(3) 1 d PGU A 1 H9 H 1.0457 0.5456 0.3090 0.087 Uiso 0.751(3) 1 calc PR A 1 C10 C 1.0542(11) 0.5176(15) 0.2360(7) 0.071(4) Uiso 0.751(3) 1 d PGU A 1 H10 H 1.1157 0.5333 0.2269 0.085 Uiso 0.751(3) 1 calc PR A 1 C11 C 1.0059(13) 0.4873(15) 0.2006(6) 0.071(4) Uiso 0.751(3) 1 d PGU A 1 H11 H 1.0343 0.4823 0.1673 0.085 Uiso 0.751(3) 1 calc PR A 1 C12 C 0.9159(13) 0.4643(14) 0.2140(7) 0.068(4) Uiso 0.751(3) 1 d PGU A 1 H12 H 0.8829 0.4436 0.1898 0.082 Uiso 0.751(3) 1 calc PR A 1 O9 O 0.5776(12) 0.2894(11) 0.1828(6) 0.0275(19) Uani 0.751(3) 1 d PU A 1 O10 O 0.5632(16) 0.4652(13) 0.1533(8) 0.0262(19) Uani 0.751(3) 1 d PU A 1 O11 O 0.7348(9) 0.3504(9) 0.1611(4) 0.030(2) Uani 0.751(3) 1 d PU A 1 P3 P 0.6238(4) 0.3654(4) 0.14843(18) 0.0266(11) Uani 0.751(3) 1 d PU A 1 C13 C 0.6026(16) 0.3666(18) 0.0809(9) 0.044(3) Uiso 0.751(3) 1 d PU A 1 C14 C 0.5056(17) 0.3798(18) 0.0624(9) 0.047(3) Uiso 0.751(3) 1 d PU A 1 H14 H 0.4495 0.3951 0.0842 0.057 Uiso 0.751(3) 1 calc PR A 1 C15 C 0.4886(18) 0.3699(17) 0.0082(9) 0.051(3) Uiso 0.751(3) 1 d PU A 1 H15 H 0.4238 0.3742 -0.0057 0.061 Uiso 0.751(3) 1 calc PR A 1 C16 C 0.5790(18) 0.3535(16) -0.0207(9) 0.049(4) Uiso 0.751(3) 1 d PU A 1 H16 H 0.5713 0.3525 -0.0568 0.058 Uiso 0.751(3) 1 calc PR A 1 C17 C 0.6685(18) 0.3402(16) -0.0035(9) 0.051(4) Uiso 0.751(3) 1 d PU A 1 H17 H 0.7244 0.3270 -0.0258 0.061 Uiso 0.751(3) 1 calc PR A 1 C18 C 0.6846(18) 0.3448(16) 0.0489(9) 0.049(3) Uiso 0.751(3) 1 d PU A 1 H18 H 0.7519 0.3331 0.0624 0.059 Uiso 0.751(3) 1 calc PR A 1 O12 O 0.4526(13) 0.2514(14) 0.2661(7) 0.029(2) Uani 0.751(3) 1 d PU A 1 O13 O 0.3443(17) 0.3987(11) 0.2870(9) 0.0294(18) Uani 0.751(3) 1 d PU A 1 O14 O 0.3346(9) 0.3669(10) 0.1961(5) 0.036(3) Uani 0.751(3) 1 d PU A 1 P4 P 0.3525(4) 0.3244(4) 0.2563(2) 0.0288(12) Uani 0.751(3) 1 d PU A 1 C19 C 0.2578(16) 0.2683(19) 0.2784(13) 0.032(8) Uiso 0.751(3) 1 d P A 1 C20 C 0.189(3) 0.2659(19) 0.2472(10) 0.052(8) Uiso 0.751(3) 1 d P A 1 H20 H 0.1903 0.2917 0.2099 0.062 Uiso 0.751(3) 1 calc PR A 1 C21 C 0.110(3) 0.224(2) 0.2689(13) 0.074(9) Uiso 0.751(3) 1 d P A 1 H21 H 0.0568 0.2250 0.2457 0.089 Uiso 0.751(3) 1 calc PR A 1 C22 C 0.1093(19) 0.1840(19) 0.3196(10) 0.060(7) Uiso 0.751(3) 1 d P A 1 H22 H 0.0576 0.1553 0.3330 0.072 Uiso 0.751(3) 1 calc PR A 1 C23 C 0.180(2) 0.184(2) 0.3523(13) 0.091(10) Uiso 0.751(3) 1 d P A 1 H23 H 0.1798 0.1537 0.3892 0.109 Uiso 0.751(3) 1 calc PR A 1 C24 C 0.257(2) 0.2261(17) 0.3342(10) 0.059(7) Uiso 0.751(3) 1 d P A 1 H24 H 0.3065 0.2271 0.3584 0.070 Uiso 0.751(3) 1 calc PR A 1 O3A O 0.644(2) 0.471(2) 0.3590(12) 0.028(3) Uani 0.249(3) 1 d PDU A 2 O4A O 0.472(2) 0.439(4) 0.3658(16) 0.027(2) Uani 0.249(3) 1 d PDU A 2 O5A O 0.633(4) 0.309(2) 0.3689(19) 0.027(2) Uani 0.249(3) 1 d PDU A 2 P1A P 0.5844(11) 0.4030(11) 0.3829(5) 0.0273(18) Uani 0.249(3) 1 d PDU A 2 C1A C 0.579(4) 0.387(4) 0.4531(8) 0.046(4) Uiso 0.249(3) 1 d PDU A 2 C2A C 0.523(4) 0.330(4) 0.4819(12) 0.047(4) Uiso 0.249(3) 1 d PDU A 2 H2A H 0.4726 0.3152 0.4641 0.056 Uiso 0.249(3) 1 calc PR A 2 C3A C 0.540(4) 0.294(4) 0.5369(13) 0.050(4) Uiso 0.249(3) 1 d PDU A 2 H3A H 0.5214 0.2392 0.5556 0.060 Uiso 0.249(3) 1 calc PR A 2 C4A C 0.585(4) 0.342(4) 0.5632(12) 0.049(4) Uiso 0.249(3) 1 d PDU A 2 H4A H 0.5801 0.3331 0.6007 0.059 Uiso 0.249(3) 1 calc PR A 2 C5A C 0.636(5) 0.404(4) 0.5348(14) 0.049(4) Uiso 0.249(3) 1 d PDU A 2 H5A H 0.6645 0.4393 0.5525 0.059 Uiso 0.249(3) 1 calc PR A 2 C6A C 0.646(4) 0.414(5) 0.4800(13) 0.049(4) Uiso 0.249(3) 1 d PDU A 2 H6A H 0.6977 0.4387 0.4617 0.059 Uiso 0.249(3) 1 calc PR A 2 O6A O 0.681(3) 0.486(3) 0.233(2) 0.030(2) Uani 0.249(3) 1 d PDU A 2 O7A O 0.791(4) 0.334(4) 0.2958(14) 0.031(2) Uani 0.249(3) 1 d PDU A 2 O8A O 0.796(2) 0.364(2) 0.1973(10) 0.028(4) Uani 0.249(3) 1 d PDU A 2 P2A P 0.7804(11) 0.4097(11) 0.2434(6) 0.0301(18) Uani 0.249(3) 1 d PDU A 2 C7A C 0.881(3) 0.457(4) 0.252(2) 0.067(4) Uiso 0.249(3) 1 d PDU A 2 C8A C 0.870(4) 0.518(5) 0.285(2) 0.069(4) Uiso 0.249(3) 1 d PDU A 2 H8A H 0.8089 0.5337 0.3028 0.083 Uiso 0.249(3) 1 calc PR A 2 C9A C 0.948(4) 0.556(5) 0.291(3) 0.072(4) Uiso 0.249(3) 1 d PDU A 2 H9A H 0.9434 0.5924 0.3170 0.086 Uiso 0.249(3) 1 calc PR A 2 C10A C 1.032(4) 0.541(5) 0.260(3) 0.071(4) Uiso 0.249(3) 1 d PDU A 2 H10A H 1.0859 0.5672 0.2642 0.085 Uiso 0.249(3) 1 calc PR A 2 C11A C 1.038(4) 0.489(6) 0.223(3) 0.070(4) Uiso 0.249(3) 1 d PDU A 2 H11A H 1.0962 0.4790 0.2017 0.084 Uiso 0.249(3) 1 calc PR A 2 C12A C 0.960(4) 0.451(5) 0.216(2) 0.069(4) Uiso 0.249(3) 1 d PDU A 2 H12A H 0.9600 0.4222 0.1882 0.082 Uiso 0.249(3) 1 calc PR A 2 O9A O 0.555(4) 0.460(3) 0.159(2) 0.026(2) Uani 0.249(3) 1 d PDU A 2 O10A O 0.596(3) 0.280(3) 0.1776(16) 0.027(2) Uani 0.249(3) 1 d PDU A 2 O11A O 0.4205(16) 0.389(3) 0.1500(12) 0.032(4) Uani 0.249(3) 1 d PDU A 2 P3A P 0.5338(11) 0.3768(11) 0.1451(5) 0.0260(17) Uani 0.249(3) 1 d PDU A 2 C13A C 0.571(2) 0.374(4) 0.0794(9) 0.046(4) Uiso 0.249(3) 1 d PGDU A 2 C14A C 0.667(2) 0.380(4) 0.0641(11) 0.048(4) Uiso 0.249(3) 1 d PGDU A 2 H14A H 0.7155 0.3784 0.0899 0.058 Uiso 0.249(3) 1 calc PR A 2 C15A C 0.693(3) 0.388(3) 0.0113(12) 0.051(4) Uiso 0.249(3) 1 d PGDU A 2 H15A H 0.7585 0.3922 0.0009 0.061 Uiso 0.249(3) 1 calc PR A 2 C16A C 0.622(3) 0.390(3) -0.0264(9) 0.050(4) Uiso 0.249(3) 1 d PGDU A 2 H16A H 0.6396 0.3954 -0.0626 0.060 Uiso 0.249(3) 1 calc PR A 2 C17A C 0.526(3) 0.384(4) -0.0112(11) 0.050(4) Uiso 0.249(3) 1 d PGDU A 2 H17A H 0.4777 0.3849 -0.0369 0.060 Uiso 0.249(3) 1 calc PR A 2 C18A C 0.500(2) 0.375(4) 0.0417(12) 0.049(4) Uiso 0.249(3) 1 d PGDU A 2 H18A H 0.4346 0.3712 0.0521 0.059 Uiso 0.249(3) 1 calc PR A 2 O12A O 0.352(5) 0.4019(19) 0.286(3) 0.030(2) Uani 0.249(3) 1 d PDU A 2 O13A O 0.443(3) 0.239(4) 0.2700(18) 0.029(2) Uani 0.249(3) 1 d PDU A 2 O14A O 0.403(2) 0.260(3) 0.3607(9) 0.031(4) Uani 0.249(3) 1 d PDU A 2 P4A P 0.3681(11) 0.2965(11) 0.3024(6) 0.0302(18) Uani 0.249(3) 1 d PDU A 2 C19A C 0.255(2) 0.268(4) 0.2931(14) 0.01(2) Uiso 0.249(3) 1 d PGD A 2 C20A C 0.222(3) 0.268(5) 0.2431(14) 0.14(8) Uiso 0.249(3) 1 d PGD A 2 H20A H 0.2622 0.2812 0.2131 0.168 Uiso 0.249(3) 1 calc PR A 2 C21A C 0.132(3) 0.247(4) 0.2370(18) 0.05(2) Uiso 0.249(3) 1 d PGD A 2 H21A H 0.1102 0.2460 0.2028 0.054 Uiso 0.249(3) 1 calc PR A 2 C22A C 0.074(3) 0.227(4) 0.281(2) 0.07(4) Uiso 0.249(3) 1 d PGD A 2 H22A H 0.0125 0.2123 0.2767 0.085 Uiso 0.249(3) 1 calc PR A 2 C23A C 0.106(3) 0.227(4) 0.3309(18) 0.07(3) Uiso 0.249(3) 1 d PGD A 2 H23A H 0.0668 0.2137 0.3608 0.086 Uiso 0.249(3) 1 calc PR A 2 C24A C 0.197(3) 0.248(4) 0.3370(13) 0.10(4) Uiso 0.249(3) 1 d PGD A 2 H24A H 0.2187 0.2489 0.3711 0.121 Uiso 0.249(3) 1 calc PR A 2 P5 P 0.3058(3) 0.6136(3) 0.17060(15) 0.0297(11) Uani 1 1 d . . . P6 P 0.4980(3) 0.6776(3) 0.28777(15) 0.0305(11) Uani 1 1 d . . . P7 P 0.6165(3) 0.0684(3) 0.37300(15) 0.0319(11) Uani 1 1 d . . . P8 P 0.8372(3) 0.1238(3) 0.24375(15) 0.0344(11) Uani 1 1 d . . . O1 O 0.4928(7) 0.4897(7) 0.2504(3) 0.031(3) Uani 1 1 d . A . O2 O 0.6374(7) 0.2545(7) 0.2844(3) 0.030(3) Uani 1 1 d . A . O15 O 0.2938(8) 0.5320(8) 0.1511(4) 0.046(3) Uani 1 1 d . A . O16 O 0.4090(7) 0.6301(7) 0.1594(3) 0.032(3) Uani 1 1 d . A . O17 O 0.2857(7) 0.5995(7) 0.2310(3) 0.037(3) Uani 1 1 d . A . O18 O 0.5316(7) 0.6676(7) 0.2316(3) 0.031(3) Uani 1 1 d . A . O19 O 0.5856(7) 0.6370(7) 0.3275(4) 0.040(3) Uani 1 1 d . A . O20 O 0.4099(7) 0.6346(7) 0.3023(3) 0.030(3) Uani 1 1 d . A . O21 O 0.5999(7) 0.0755(7) 0.3133(4) 0.034(3) Uani 1 1 d . A . O22 O 0.5210(7) 0.1156(7) 0.3985(4) 0.043(3) Uani 1 1 d . A . O23 O 0.7042(7) 0.1074(7) 0.3799(3) 0.036(3) Uani 1 1 d . A . O24 O 0.7342(7) 0.1120(7) 0.2328(4) 0.038(3) Uani 1 1 d . A . O25 O 0.8420(6) 0.1420(7) 0.2992(3) 0.030(3) Uani 1 1 d . A . O26 O 0.8609(8) 0.2020(8) 0.1999(4) 0.048(3) Uani 1 1 d . A . C25 C 0.2141(11) 0.7191(11) 0.1322(6) 0.032(4) Uiso 1 1 d . A . C26 C 0.2385(13) 0.8021(13) 0.1155(7) 0.053(5) Uiso 1 1 d . . . H26 H 0.3033 0.8047 0.1253 0.063 Uiso 1 1 calc R A . C27 C 0.1691(13) 0.8836(14) 0.0840(7) 0.059(5) Uiso 1 1 d . A . H27 H 0.1880 0.9406 0.0716 0.071 Uiso 1 1 calc R . . C28 C 0.0735(15) 0.8821(15) 0.0708(7) 0.067(6) Uiso 1 1 d . . . H28 H 0.0254 0.9380 0.0503 0.081 Uiso 1 1 calc R A . C29 C 0.0500(15) 0.8004(14) 0.0875(7) 0.064(6) Uiso 1 1 d . A . H29 H -0.0151 0.7983 0.0777 0.077 Uiso 1 1 calc R . . C30 C 0.1213(12) 0.7138(13) 0.1205(6) 0.051(5) Uiso 1 1 d . . . H30 H 0.1031 0.6565 0.1331 0.062 Uiso 1 1 calc R A . C31 C 0.4441(11) 0.8010(11) 0.2837(6) 0.032(4) Uiso 1 1 d . A . C32 C 0.4819(12) 0.8427(12) 0.3180(6) 0.043(4) Uiso 1 1 d . . . H32 H 0.5387 0.8070 0.3420 0.052 Uiso 1 1 calc R A . C33 C 0.4326(13) 0.9394(13) 0.3156(7) 0.058(5) Uiso 1 1 d . A . H33 H 0.4570 0.9691 0.3384 0.070 Uiso 1 1 calc R . . C34 C 0.3513(14) 0.9912(15) 0.2818(7) 0.068(6) Uiso 1 1 d . . . H34 H 0.3212 1.0569 0.2802 0.081 Uiso 1 1 calc R A . C35 C 0.3116(16) 0.9484(16) 0.2493(8) 0.078(6) Uiso 1 1 d . A . H35 H 0.2527 0.9830 0.2266 0.094 Uiso 1 1 calc R . . C36 C 0.3597(13) 0.8564(13) 0.2513(7) 0.057(5) Uiso 1 1 d . . . H36 H 0.3335 0.8276 0.2287 0.069 Uiso 1 1 calc R A . C37 C 0.6544(10) -0.0552(10) 0.4053(5) 0.028(4) Uiso 1 1 d . A . C38 C 0.6326(12) -0.0860(13) 0.4565(7) 0.049(5) Uiso 1 1 d . . . H38 H 0.5964 -0.0407 0.4750 0.059 Uiso 1 1 calc R A . C39 C 0.6618(13) -0.1830(13) 0.4831(7) 0.057(5) Uiso 1 1 d . A . H39 H 0.6467 -0.2030 0.5194 0.069 Uiso 1 1 calc R . . C40 C 0.7114(14) -0.2478(15) 0.4570(8) 0.070(6) Uiso 1 1 d . . . H40 H 0.7315 -0.3138 0.4750 0.084 Uiso 1 1 calc R A . C41 C 0.7327(13) -0.2202(14) 0.4061(7) 0.060(5) Uiso 1 1 d . A . H41 H 0.7664 -0.2660 0.3874 0.072 Uiso 1 1 calc R . . C42 C 0.7047(13) -0.1230(13) 0.3807(7) 0.057(5) Uiso 1 1 d . . . H42 H 0.7216 -0.1035 0.3447 0.068 Uiso 1 1 calc R A . C43 C 0.9298(12) 0.0159(12) 0.2459(7) 0.021(15) Uiso 0.596(17) 1 d PGD A 1 C44 C 0.9183(11) -0.0368(14) 0.2111(6) 0.051(9) Uiso 0.596(17) 1 d PGD A 1 H44 H 0.8584 -0.0163 0.1887 0.061 Uiso 0.596(17) 1 calc PR A 1 C45 C 0.9946(14) -0.1194(13) 0.2090(7) 0.069(11) Uiso 0.596(17) 1 d PGD A 1 H45 H 0.9868 -0.1554 0.1851 0.083 Uiso 0.596(17) 1 calc PR A 1 C46 C 1.0823(13) -0.1494(11) 0.2417(7) 0.038(8) Uiso 0.596(17) 1 d PGD A 1 H46 H 1.1345 -0.2059 0.2402 0.045 Uiso 0.596(17) 1 calc PR A 1 C47 C 1.0938(11) -0.0968(13) 0.2765(7) 0.051(9) Uiso 0.596(17) 1 d PGD A 1 H47 H 1.1537 -0.1173 0.2989 0.061 Uiso 0.596(17) 1 calc PR A 1 C48 C 1.0175(14) -0.0141(12) 0.2786(6) 0.040(8) Uiso 0.596(17) 1 d PGD A 1 H48 H 1.0253 0.0218 0.3025 0.049 Uiso 0.596(17) 1 calc PR A 1 C43A C 0.920(4) 0.006(3) 0.2468(18) 0.07(4) Uiso 0.404(17) 1 d PD A 2 C44A C 0.911(4) -0.073(3) 0.2854(18) 0.11(2) Uiso 0.404(17) 1 d PD A 2 H44A H 0.8634 -0.0640 0.3122 0.127 Uiso 0.404(17) 1 calc PR A 2 C45A C 0.971(4) -0.165(3) 0.286(2) 0.14(3) Uiso 0.404(17) 1 d PD A 2 H45A H 0.9593 -0.2184 0.3103 0.163 Uiso 0.404(17) 1 calc PR A 2 C46A C 1.050(3) -0.177(2) 0.2506(14) 0.039(12) Uiso 0.404(17) 1 d PD A 2 H46A H 1.0971 -0.2377 0.2536 0.047 Uiso 0.404(17) 1 calc PR A 2 C47A C 1.057(3) -0.098(2) 0.2110(15) 0.069(15) Uiso 0.404(17) 1 d PD A 2 H47A H 1.1109 -0.1056 0.1868 0.082 Uiso 0.404(17) 1 calc PR A 2 C48A C 0.987(3) -0.009(2) 0.2067(14) 0.051(13) Uiso 0.404(17) 1 d PD A 2 H48A H 0.9847 0.0414 0.1760 0.061 Uiso 0.404(17) 1 calc PR A 2 C49 C 0.2548(10) 0.5401(11) 0.3480(5) 0.028(4) Uiso 1 1 d . A . C50 C 0.2039(12) 0.6325(13) 0.3459(7) 0.051(5) Uiso 1 1 d . . . H50 H 0.2255 0.6827 0.3234 0.061 Uiso 1 1 calc R A . C51 C 0.1192(14) 0.6533(15) 0.3774(7) 0.063(5) Uiso 1 1 d . A . H51 H 0.0832 0.7170 0.3777 0.076 Uiso 1 1 calc R . . C52 C 0.0916(13) 0.5780(13) 0.4072(7) 0.051(5) Uiso 1 1 d . . . C53 C 0.1461(13) 0.4844(14) 0.4114(7) 0.061(5) Uiso 1 1 d . A . H53 H 0.1275 0.4337 0.4353 0.073 Uiso 1 1 calc R . . C54 C 0.2336(12) 0.4653(12) 0.3779(6) 0.042(4) Uiso 1 1 d . . . H54 H 0.2727 0.4022 0.3780 0.051 Uiso 1 1 calc R A . C55 C 0.6172(10) 0.6379(10) 0.1307(5) 0.025(4) Uiso 1 1 d . A . C56 C 0.7060(11) 0.5914(12) 0.1123(6) 0.043(4) Uiso 1 1 d . . . H56 H 0.7365 0.5251 0.1273 0.051 Uiso 1 1 calc R A . C57 C 0.7529(13) 0.6423(12) 0.0705(6) 0.049(5) Uiso 1 1 d . A . H57 H 0.8128 0.6105 0.0555 0.059 Uiso 1 1 calc R . . C58 C 0.7095(12) 0.7386(13) 0.0523(6) 0.045(5) Uiso 1 1 d . . . C59 C 0.6227(12) 0.7867(13) 0.0707(6) 0.043(4) Uiso 1 1 d . A . H59 H 0.5939 0.8535 0.0562 0.052 Uiso 1 1 calc R . . C60 C 0.5759(11) 0.7365(11) 0.1117(5) 0.031(4) Uiso 1 1 d . . . H60 H 0.5164 0.7693 0.1265 0.037 Uiso 1 1 calc R A . C61 C 0.5296(10) 0.1098(11) 0.2014(5) 0.028(4) Uiso 1 1 d . A . C62 C 0.4468(11) 0.1635(11) 0.1665(6) 0.033(4) Uiso 1 1 d . . . H62 H 0.4178 0.2295 0.1642 0.040 Uiso 1 1 calc R A . C63 C 0.4070(11) 0.1207(11) 0.1352(6) 0.038(4) Uiso 1 1 d . A . H63 H 0.3516 0.1568 0.1104 0.045 Uiso 1 1 calc R . . C64 C 0.4503(12) 0.0219(12) 0.1407(6) 0.043(4) Uiso 1 1 d . . . C65 C 0.5319(12) -0.0326(13) 0.1752(6) 0.047(5) Uiso 1 1 d . A . H65 H 0.5608 -0.0987 0.1776 0.056 Uiso 1 1 calc R . . C66 C 0.5705(11) 0.0126(11) 0.2066(6) 0.037(4) Uiso 1 1 d . . . H66 H 0.6253 -0.0235 0.2317 0.044 Uiso 1 1 calc R A . Cl1 Cl 0.3978(4) -0.0317(4) 0.10117(19) 0.0660(14) Uani 1 1 d . A . C67 C 0.8574(5) 0.2035(8) 0.3980(3) 0.043(4) Uiso 1 1 d G A . C68 C 0.8647(6) 0.2753(6) 0.4205(3) 0.052(5) Uiso 1 1 d G . . H68 H 0.8175 0.3373 0.4096 0.063 Uiso 1 1 calc R A . C69 C 0.9410(5) 0.2565(4) 0.4590(3) 0.065(6) Uiso 1 1 d G A . H69 H 0.9460 0.3057 0.4744 0.078 Uiso 1 1 calc R . . C70 C 1.0101(3) 0.1659(4) 0.47502(18) 0.055(5) Uiso 1 1 d G . . C71 C 1.0029(6) 0.0940(5) 0.4525(3) 0.061(5) Uiso 1 1 d G A . H71 H 1.0501 0.0321 0.4634 0.074 Uiso 1 1 calc R . . C72 C 0.9265(7) 0.1128(7) 0.4140(3) 0.046(5) Uiso 1 1 d G . . H72 H 0.9216 0.0637 0.3986 0.055 Uiso 1 1 calc R A . Cl4 Cl 1.0933(4) 0.1478(5) 0.5233(2) 0.110(2) Uani 1 1 d G A . Cl2 Cl -0.0151(4) 0.6019(5) 0.4461(2) 0.103(2) Uani 1 1 d . A . Cl3 Cl 0.7715(4) 0.8026(4) 0.00304(19) 0.0793(17) Uani 1 1 d . A . Cl10 Cl 0.6131(7) 0.0718(7) 0.0244(3) 0.140(3) Uani 1 1 d D . . C100 C 0.6733(14) 0.1054(17) 0.0675(9) 0.104(8) Uiso 1 1 d D . . H10B H 0.6570 0.1758 0.0563 0.125 Uiso 1 1 calc R . . H10C H 0.6444 0.0888 0.1028 0.125 Uiso 1 1 calc R . . Cl11 Cl 0.7951(7) 0.0617(11) 0.0749(4) 0.251(7) Uani 1 1 d D . . Cl12 Cl 0.7509(7) 0.7620(6) 0.2619(3) 0.150(3) Uani 1 1 d D . . C101 C 0.787(2) 0.7384(15) 0.2036(8) 0.116(9) Uiso 1 1 d D . . H10D H 0.8544 0.6894 0.2099 0.140 Uiso 1 1 calc R . . H10E H 0.7384 0.7092 0.1924 0.140 Uiso 1 1 calc R . . Cl13 Cl 0.7959(6) 0.8242(9) 0.1543(3) 0.174(4) Uani 1 1 d D . . Cl14 Cl 1.1633(8) -0.1143(8) 0.4069(5) 0.184(4) Uani 1 1 d D . . C102 C 1.258(3) -0.146(2) 0.4516(14) 0.213(18) Uiso 1 1 d D . . H10F H 1.2366 -0.1814 0.4853 0.256 Uiso 1 1 calc R . . H10G H 1.3163 -0.1915 0.4397 0.256 Uiso 1 1 calc R . . Cl15 Cl 1.2990(11) -0.0675(10) 0.4649(6) 0.281(8) Uani 1 1 d D . . Cl16 Cl 0.2026(10) 0.3791(9) 0.0770(4) 0.216(5) Uani 1 1 d D . . C103 C 0.188(2) 0.4944(18) 0.0521(17) 0.223(19) Uiso 1 1 d D . . H10H H 0.2132 0.5191 0.0791 0.268 Uiso 1 1 calc R . . H10I H 0.2303 0.5026 0.0207 0.268 Uiso 1 1 calc R . . Cl17 Cl 0.0729(12) 0.5567(11) 0.0347(8) 0.328(10) Uani 1 1 d D . . Cl18 Cl 1.1314(7) 0.1373(8) 0.1309(4) 0.193(5) Uani 1 1 d D . . C104 C 1.018(2) 0.204(3) 0.1011(15) 0.26(2) Uiso 1 1 d D . . H10J H 0.9649 0.2049 0.1278 0.313 Uiso 1 1 calc R . . H10K H 1.0198 0.2710 0.0865 0.313 Uiso 1 1 calc R . . Cl19 Cl 0.9894(9) 0.1645(10) 0.0538(4) 0.224(5) Uani 1 1 d 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 0.0321(6) 0.0352(7) 0.0124(6) -0.0122(5) 0.0075(4) -0.0083(5) Sb2 0.0317(6) 0.0345(7) 0.0122(6) -0.0111(5) 0.0077(4) -0.0090(5) Sb3 0.0326(6) 0.0354(7) 0.0156(6) -0.0133(5) 0.0082(5) -0.0082(5) Sb4 0.0303(6) 0.0366(7) 0.0153(6) -0.0105(5) 0.0074(5) -0.0077(5) O3 0.026(5) 0.041(5) 0.026(5) -0.010(5) 0.007(5) -0.006(4) O4 0.028(3) 0.039(4) 0.016(4) -0.014(3) 0.007(3) -0.005(3) O5 0.030(3) 0.039(4) 0.016(4) -0.013(3) 0.006(3) -0.003(3) P1 0.028(2) 0.038(3) 0.015(2) -0.014(2) 0.0066(19) -0.005(2) O6 0.033(4) 0.041(3) 0.017(3) -0.009(3) 0.008(3) -0.010(3) O7 0.032(4) 0.043(4) 0.016(3) -0.008(3) 0.011(3) -0.013(3) O8 0.038(6) 0.039(5) 0.019(4) -0.009(4) 0.004(4) -0.009(5) P2 0.032(3) 0.042(3) 0.019(2) -0.008(2) 0.0057(19) -0.011(2) O9 0.033(4) 0.035(4) 0.015(3) -0.010(3) 0.009(3) -0.011(3) O10 0.032(3) 0.036(3) 0.012(3) -0.009(3) 0.008(3) -0.011(3) O11 0.032(4) 0.035(6) 0.022(5) -0.007(5) 0.005(4) -0.008(4) P3 0.032(2) 0.036(3) 0.013(2) -0.009(2) 0.008(2) -0.010(2) O12 0.028(3) 0.040(4) 0.019(3) -0.013(3) 0.011(3) -0.008(3) O13 0.030(4) 0.039(4) 0.019(3) -0.011(3) 0.014(3) -0.008(3) O14 0.039(5) 0.047(6) 0.021(4) -0.013(4) 0.003(4) -0.008(5) P4 0.030(2) 0.039(3) 0.019(2) -0.012(2) 0.010(2) -0.009(2) O3A 0.030(6) 0.037(6) 0.017(7) -0.013(6) 0.010(7) -0.005(5) O4A 0.029(3) 0.039(4) 0.015(4) -0.014(4) 0.006(3) -0.004(3) O5A 0.028(4) 0.039(4) 0.015(4) -0.014(3) 0.007(3) -0.005(3) P1A 0.028(3) 0.039(4) 0.016(3) -0.014(3) 0.006(3) -0.006(3) O6A 0.032(4) 0.042(4) 0.017(4) -0.008(3) 0.010(3) -0.012(3) O7A 0.033(4) 0.041(4) 0.017(3) -0.008(3) 0.008(3) -0.011(4) O8A 0.030(7) 0.036(7) 0.017(5) -0.005(5) 0.007(6) -0.010(6) P2A 0.032(3) 0.042(4) 0.017(3) -0.007(3) 0.008(3) -0.012(3) O9A 0.032(4) 0.036(4) 0.012(4) -0.009(3) 0.008(4) -0.011(3) O10A 0.032(4) 0.035(4) 0.014(4) -0.010(3) 0.008(4) -0.011(3) O11A 0.031(4) 0.042(7) 0.023(7) -0.012(7) 0.003(6) -0.012(5) P3A 0.031(3) 0.036(3) 0.013(3) -0.010(3) 0.008(3) -0.011(3) O12A 0.030(4) 0.040(4) 0.019(4) -0.011(3) 0.013(4) -0.008(4) O13A 0.029(4) 0.040(4) 0.019(3) -0.012(3) 0.011(3) -0.008(4) O14A 0.029(7) 0.041(7) 0.020(4) -0.009(5) 0.014(6) -0.004(7) P4A 0.030(3) 0.040(3) 0.019(3) -0.011(3) 0.013(3) -0.007(3) P5 0.032(2) 0.037(3) 0.019(2) -0.011(2) 0.0038(19) -0.006(2) P6 0.038(3) 0.038(3) 0.019(2) -0.016(2) 0.008(2) -0.009(2) P7 0.034(3) 0.040(3) 0.022(2) -0.009(2) 0.0069(19) -0.011(2) P8 0.034(3) 0.047(3) 0.019(2) -0.014(2) 0.0090(19) -0.003(2) O1 0.033(6) 0.043(7) 0.019(5) -0.015(5) 0.010(5) -0.011(5) O2 0.034(6) 0.030(7) 0.031(6) -0.017(5) 0.005(5) -0.008(5) O15 0.060(7) 0.055(8) 0.027(6) -0.018(6) -0.003(5) -0.015(6) O16 0.049(7) 0.048(7) 0.013(5) -0.018(5) 0.016(5) -0.026(6) O17 0.031(6) 0.047(7) 0.023(6) -0.003(5) 0.014(5) -0.002(5) O18 0.056(7) 0.034(7) 0.013(5) -0.012(5) 0.012(5) -0.023(6) O19 0.044(7) 0.042(7) 0.032(6) -0.019(5) 0.001(5) -0.002(6) O20 0.044(6) 0.028(6) 0.020(5) -0.014(5) 0.014(5) -0.010(5) O21 0.042(6) 0.028(7) 0.031(6) -0.009(5) 0.002(5) -0.008(5) O22 0.049(7) 0.048(8) 0.036(6) -0.017(6) 0.020(5) -0.017(6) O23 0.045(7) 0.039(7) 0.023(6) -0.018(5) 0.014(5) -0.003(6) O24 0.034(6) 0.056(8) 0.025(6) -0.030(5) 0.016(5) 0.002(6) O25 0.021(5) 0.039(7) 0.032(6) -0.026(5) 0.011(4) -0.001(5) O26 0.060(8) 0.047(8) 0.029(6) -0.003(6) 0.011(6) -0.010(6) Cl1 0.083(4) 0.057(3) 0.069(3) -0.037(3) -0.016(3) -0.018(3) Cl4 0.092(4) 0.127(6) 0.102(5) -0.027(4) -0.060(4) -0.017(4) Cl2 0.079(4) 0.124(5) 0.078(4) -0.022(4) 0.059(3) 0.003(4) Cl3 0.092(4) 0.083(4) 0.056(3) 0.004(3) 0.040(3) -0.038(3) Cl10 0.191(8) 0.191(9) 0.080(5) -0.058(5) 0.021(5) -0.101(7) Cl11 0.125(8) 0.40(2) 0.160(9) 0.004(11) -0.004(6) -0.029(10) Cl12 0.183(8) 0.128(7) 0.112(6) -0.025(5) 0.082(6) -0.018(6) Cl13 0.129(6) 0.295(13) 0.112(6) -0.073(7) 0.034(5) -0.069(8) Cl14 0.171(9) 0.178(9) 0.222(11) -0.093(8) 0.030(8) -0.046(8) Cl15 0.304(16) 0.196(12) 0.305(16) -0.148(12) -0.127(13) 0.072(11) Cl16 0.271(13) 0.227(13) 0.167(9) -0.035(9) -0.019(9) -0.106(11) Cl17 0.248(16) 0.248(16) 0.49(3) -0.130(17) -0.132(17) -0.026(13) Cl18 0.157(8) 0.223(11) 0.149(8) 0.004(8) 0.043(6) -0.028(8) Cl19 0.235(12) 0.305(16) 0.174(10) -0.081(10) 0.029(9) -0.128(12) _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 1.931(8) . ? Sb1 O12A 1.94(4) . ? Sb1 O5 1.974(13) . ? Sb1 O20 2.016(10) . ? Sb1 O13 2.033(18) . ? Sb1 O17 2.048(9) . ? Sb1 O4A 2.12(3) . ? Sb1 C49 2.152(13) . ? Sb2 O1 1.897(9) . ? Sb2 O6A 1.97(3) . ? Sb2 O9A 1.98(3) . ? Sb2 O10 1.984(15) . ? Sb2 O7 1.995(16) . ? Sb2 O16 2.026(10) . ? Sb2 O18 2.027(9) . ? Sb2 C55 2.101(13) . ? Sb3 O2 1.918(9) . ? Sb3 O12 1.980(15) . ? Sb3 O9 1.988(15) . ? Sb3 O21 2.010(9) . ? Sb3 O24 2.037(9) . ? Sb3 O10A 2.04(4) . ? Sb3 O13A 2.08(3) . ? Sb3 C61 2.108(14) . ? Sb4 O2 1.925(9) . ? Sb4 O5A 1.95(4) . ? Sb4 O7A 2.00(4) . ? Sb4 O25 2.018(8) . ? Sb4 O6 2.018(18) . ? Sb4 O4 2.023(15) . ? Sb4 O23 2.054(10) . ? Sb4 C67 2.138(4) . ? O3 P1 1.491(13) . ? O4 P1 1.520(18) . ? O5 P1 1.504(15) . ? P1 C1 1.782(10) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? O6 P2 1.50(2) . ? O7 P2 1.53(2) . ? O8 P2 1.514(13) . ? P2 C7 1.783(13) . ? 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 H10 0.9500 . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? O9 P3 1.547(18) . ? O10 P3 1.533(19) . ? O11 P3 1.509(13) . ? P3 C13 1.78(2) . ? C13 C14 1.37(3) . ? C13 C18 1.39(3) . ? C14 C15 1.49(3) . ? C14 H14 0.9500 . ? C15 C16 1.42(3) . ? C15 H15 0.9500 . ? C16 C17 1.26(3) . ? C16 H16 0.9500 . ? C17 C18 1.41(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O12 P4 1.473(18) . ? O13 P4 1.52(2) . ? O14 P4 1.529(13) . ? P4 C19 1.76(2) . ? C19 C20 1.28(4) . ? C19 C24 1.43(4) . ? C20 C21 1.45(4) . ? C20 H20 0.9500 . ? C21 C22 1.30(4) . ? C21 H21 0.9500 . ? C22 C23 1.31(4) . ? C22 H22 0.9500 . ? C23 C24 1.39(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? O3A P1A 1.503(19) . ? O4A P1A 1.52(2) . ? O5A P1A 1.51(2) . ? P1A C1A 1.777(16) . ? C1A C2A 1.387(15) . ? C1A C6A 1.391(15) . ? C2A C3A 1.392(15) . ? C2A H2A 0.9500 . ? C3A C4A 1.391(15) . ? C3A H3A 0.9500 . ? C4A C5A 1.385(15) . ? C4A H4A 0.9500 . ? C5A C6A 1.401(15) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? O6A P2A 1.49(2) . ? O7A P2A 1.52(2) . ? O8A P2A 1.514(19) . ? P2A C7A 1.777(17) . ? C7A C8A 1.386(15) . ? C7A C12A 1.390(15) . ? C8A C9A 1.395(15) . ? C8A H8A 0.9500 . ? C9A C10A 1.389(15) . ? C9A H9A 0.9500 . ? C10A C11A 1.383(15) . ? C10A H10A 0.9500 . ? C11A C12A 1.394(15) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? O9A P3A 1.50(2) . ? O10A P3A 1.51(2) . ? O11A P3A 1.519(19) . ? P3A C13A 1.775(16) . ? 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 . ? O12A P4A 1.50(2) . ? O13A P4A 1.52(2) . ? O14A P4A 1.517(19) . ? P4A C19A 1.770(16) . ? C19A C20A 1.3900 . ? C19A C24A 1.3900 . ? C20A C21A 1.3900 . ? C20A H20A 0.9500 . ? C21A C22A 1.3900 . ? C21A H21A 0.9500 . ? C22A C23A 1.3900 . ? C22A H22A 0.9500 . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A H24A 0.9500 . ? P5 O15 1.502(11) . ? P5 O16 1.517(10) . ? P5 O17 1.555(9) . ? P5 C25 1.796(15) . ? P6 O19 1.489(10) . ? P6 O20 1.530(10) . ? P6 O18 1.547(9) . ? P6 C31 1.775(16) . ? P7 O22 1.519(10) . ? P7 O23 1.523(11) . ? P7 O21 1.547(10) . ? P7 C37 1.772(15) . ? P8 O24 1.521(10) . ? P8 O26 1.524(11) . ? P8 O25 1.541(9) . ? P8 C43 1.742(14) . ? P8 C43A 1.80(4) . ? C25 C30 1.35(2) . ? C25 C26 1.36(2) . ? C26 C27 1.40(2) . ? C26 H26 0.9500 . ? C27 C28 1.38(2) . ? C27 H27 0.9500 . ? C28 C29 1.33(2) . ? C28 H28 0.9500 . ? C29 C30 1.47(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.38(2) . ? C31 C32 1.41(2) . ? C32 C33 1.41(2) . ? C32 H32 0.9500 . ? C33 C34 1.35(2) . ? C33 H33 0.9500 . ? C34 C35 1.40(3) . ? C34 H34 0.9500 . ? C35 C36 1.35(2) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.348(19) . ? C37 C42 1.35(2) . ? C38 C39 1.40(2) . ? C38 H38 0.9500 . ? C39 C40 1.34(2) . ? C39 H39 0.9500 . ? C40 C41 1.33(2) . ? C40 H40 0.9500 . ? C41 C42 1.39(2) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C47 C48 1.3900 . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C43A C44A 1.380(18) . ? C43A C48A 1.385(18) . ? C44A C45A 1.391(18) . ? C44A H44A 0.9500 . ? C45A C46A 1.392(18) . ? C45A H45A 0.9500 . ? C46A C47A 1.385(18) . ? C46A H46A 0.9500 . ? C47A C48A 1.391(18) . ? C47A H47A 0.9500 . ? C48A H48A 0.9500 . ? C49 C54 1.305(19) . ? C49 C50 1.36(2) . ? C50 C51 1.41(2) . ? C50 H50 0.9500 . ? C51 C52 1.35(2) . ? C51 H51 0.9500 . ? C52 C53 1.37(2) . ? C52 Cl2 1.755(17) . ? C53 C54 1.46(2) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.357(19) . ? C55 C60 1.394(19) . ? C56 C57 1.42(2) . ? C56 H56 0.9500 . ? C57 C58 1.37(2) . ? C57 H57 0.9500 . ? C58 C59 1.35(2) . ? C58 Cl3 1.755(17) . ? C59 C60 1.398(19) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C66 1.39(2) . ? C61 C62 1.388(19) . ? C62 C63 1.37(2) . ? C62 H62 0.9500 . ? C63 C64 1.41(2) . ? C63 H63 0.9500 . ? C64 C65 1.37(2) . ? C64 Cl1 1.747(17) . ? C65 C66 1.39(2) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.3900 . ? C67 C72 1.3900 . ? C68 C69 1.3900 . ? C68 H68 0.9500 . ? C69 C70 1.3900 . ? C69 H69 0.9500 . ? C70 C71 1.3900 . ? C70 Cl4 1.6394 . ? C71 C72 1.3900 . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? Cl10 C100 1.672(17) . ? C100 Cl11 1.606(17) . ? C100 H10B 0.9900 . ? C100 H10C 0.9900 . ? Cl12 C101 1.669(18) . ? C101 Cl13 1.605(18) . ? C101 H10D 0.9900 . ? C101 H10E 0.9900 . ? Cl14 C102 1.65(2) . ? C102 Cl15 1.57(2) . ? C102 H10F 0.9900 . ? C102 H10G 0.9900 . ? Cl16 C103 1.66(2) . ? C103 Cl17 1.59(2) . ? C103 H10H 0.9900 . ? C103 H10I 0.9900 . ? Cl18 C104 1.68(2) . ? C104 Cl19 1.61(2) . ? C104 H10J 0.9900 . ? C104 H10K 0.9900 . ? 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 O12A 87(2) . . ? O1 Sb1 O5 86.2(5) . . ? O12A Sb1 O5 92.8(18) . . ? O1 Sb1 O20 90.6(4) . . ? O12A Sb1 O20 177(2) . . ? O5 Sb1 O20 88.5(6) . . ? O1 Sb1 O13 89.6(7) . . ? O12A Sb1 O13 3(3) . . ? O5 Sb1 O13 93.7(8) . . ? O20 Sb1 O13 177.8(7) . . ? O1 Sb1 O17 90.6(4) . . ? O12A Sb1 O17 91.3(17) . . ? O5 Sb1 O17 174.7(6) . . ? O20 Sb1 O17 87.3(4) . . ? O13 Sb1 O17 90.5(7) . . ? O1 Sb1 O4A 92.3(11) . . ? O12A Sb1 O4A 93(2) . . ? O5 Sb1 O4A 6.1(13) . . ? O20 Sb1 O4A 88.7(14) . . ? O13 Sb1 O4A 93.5(16) . . ? O17 Sb1 O4A 175.1(14) . . ? O1 Sb1 C49 178.2(5) . . ? O12A Sb1 C49 92(2) . . ? O5 Sb1 C49 92.4(5) . . ? O20 Sb1 C49 90.4(5) . . ? O13 Sb1 C49 89.4(8) . . ? O17 Sb1 C49 90.9(4) . . ? O4A Sb1 C49 86.3(11) . . ? O1 Sb2 O6A 84.0(17) . . ? O1 Sb2 O9A 84.6(14) . . ? O6A Sb2 O9A 91(2) . . ? O1 Sb2 O10 90.1(6) . . ? O6A Sb2 O10 90.5(17) . . ? O9A Sb2 O10 5.6(18) . . ? O1 Sb2 O7 89.1(6) . . ? O6A Sb2 O7 6(2) . . ? O9A Sb2 O7 94.5(19) . . ? O10 Sb2 O7 93.6(8) . . ? O1 Sb2 O16 89.4(4) . . ? O6A Sb2 O16 173.4(17) . . ? O9A Sb2 O16 87.6(18) . . ? O10 Sb2 O16 88.5(7) . . ? O7 Sb2 O16 177.4(6) . . ? O1 Sb2 O18 91.8(4) . . ? O6A Sb2 O18 92.7(16) . . ? O9A Sb2 O18 174.6(15) . . ? O10 Sb2 O18 176.4(7) . . ? O7 Sb2 O18 89.4(6) . . ? O16 Sb2 O18 88.4(4) . . ? O1 Sb2 C55 177.8(5) . . ? O6A Sb2 C55 94.8(17) . . ? O9A Sb2 C55 93.6(15) . . ? O10 Sb2 C55 88.1(6) . . ? O7 Sb2 C55 89.8(7) . . ? O16 Sb2 C55 91.7(4) . . ? O18 Sb2 C55 90.1(5) . . ? O2 Sb3 O12 84.3(6) . . ? O2 Sb3 O9 86.0(7) . . ? O12 Sb3 O9 88.5(7) . . ? O2 Sb3 O21 91.7(4) . . ? O12 Sb3 O21 90.6(6) . . ? O9 Sb3 O21 177.6(6) . . ? O2 Sb3 O24 90.6(4) . . ? O12 Sb3 O24 174.5(6) . . ? O9 Sb3 O24 93.2(5) . . ? O21 Sb3 O24 87.5(4) . . ? O2 Sb3 O10A 88.1(16) . . ? O12 Sb3 O10A 96.8(11) . . ? O9 Sb3 O10A 8.5(12) . . ? O21 Sb3 O10A 172.5(10) . . ? O24 Sb3 O10A 85.0(10) . . ? O2 Sb3 O13A 88.8(13) . . ? O12 Sb3 O13A 6.8(19) . . ? O9 Sb3 O13A 93.8(16) . . ? O21 Sb3 O13A 85.4(15) . . ? O24 Sb3 O13A 172.9(15) . . ? O10A Sb3 O13A 102.0(17) . . ? O2 Sb3 C61 175.9(5) . . ? O12 Sb3 C61 93.9(6) . . ? O9 Sb3 C61 90.3(7) . . ? O21 Sb3 C61 92.0(5) . . ? O24 Sb3 C61 91.3(5) . . ? O10A Sb3 C61 88.4(16) . . ? O13A Sb3 C61 89.8(14) . . ? O2 Sb4 O5A 81.5(15) . . ? O2 Sb4 O7A 89.9(14) . . ? O5A Sb4 O7A 93(2) . . ? O2 Sb4 O25 90.8(4) . . ? O5A Sb4 O25 172.3(15) . . ? O7A Sb4 O25 87.1(17) . . ? O2 Sb4 O6 85.6(6) . . ? O5A Sb4 O6 89.3(15) . . ? O7A Sb4 O6 6(2) . . ? O25 Sb4 O6 90.7(7) . . ? O2 Sb4 O4 87.4(6) . . ? O5A Sb4 O4 5.9(19) . . ? O7A Sb4 O4 93.9(17) . . ? O25 Sb4 O4 177.9(6) . . ? O6 Sb4 O4 90.2(8) . . ? O2 Sb4 O23 91.2(4) . . ? O5A Sb4 O23 91.5(14) . . ? O7A Sb4 O23 175.1(17) . . ? O25 Sb4 O23 88.0(4) . . ? O6 Sb4 O23 176.6(6) . . ? O4 Sb4 O23 90.9(6) . . ? O2 Sb4 C67 176.7(4) . . ? O5A Sb4 C67 96.2(15) . . ? O7A Sb4 C67 87.8(14) . . ? O25 Sb4 C67 91.5(4) . . ? O6 Sb4 C67 91.9(6) . . ? O4 Sb4 C67 90.4(6) . . ? O23 Sb4 C67 91.3(4) . . ? P1 O4 Sb4 151.8(11) . . ? P1 O5 Sb1 149.0(12) . . ? O3 P1 O5 111.4(8) . . ? O3 P1 O4 114.0(8) . . ? O5 P1 O4 110.0(9) . . ? O3 P1 C1 111.0(7) . . ? O5 P1 C1 108.0(9) . . ? O4 P1 C1 101.9(8) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 118.2(9) . . ? C6 C1 P1 121.8(9) . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? P2 O6 Sb4 146.8(13) . . ? P2 O7 Sb2 151.9(12) . . ? O6 P2 O8 111.1(9) . . ? O6 P2 O7 110.2(10) . . ? O8 P2 O7 112.5(9) . . ? O6 P2 C7 106.3(10) . . ? O8 P2 C7 112.2(8) . . ? O7 P2 C7 104.1(9) . . ? C8 C7 C12 120.0 . . ? C8 C7 P2 117.6(11) . . ? C12 C7 P2 122.3(11) . . ? C9 C8 C7 120.0 . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? P3 O9 Sb3 149.0(11) . . ? P3 O10 Sb2 145.1(14) . . ? O11 P3 O10 108.2(9) . . ? O11 P3 O9 115.2(8) . . ? O10 P3 O9 110.3(8) . . ? O11 P3 C13 111.6(8) . . ? O10 P3 C13 105.2(11) . . ? O9 P3 C13 105.9(10) . . ? C14 C13 C18 120(2) . . ? C14 C13 P3 119.4(16) . . ? C18 C13 P3 120.2(17) . . ? C13 C14 C15 120(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 113(2) . . ? C16 C15 H15 123.4 . . ? C14 C15 H15 123.4 . . ? C17 C16 C15 127(2) . . ? C17 C16 H16 116.6 . . ? C15 C16 H16 116.6 . . ? C16 C17 C18 119(2) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 120(2) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? P4 O12 Sb3 155.3(12) . . ? P4 O13 Sb1 149.8(15) . . ? O12 P4 O13 111.6(11) . . ? O12 P4 O14 108.1(8) . . ? O13 P4 O14 113.3(10) . . ? O12 P4 C19 108.6(11) . . ? O13 P4 C19 107.5(12) . . ? O14 P4 C19 107.6(12) . . ? C20 C19 C24 119(2) . . ? C20 C19 P4 123(2) . . ? C24 C19 P4 118(2) . . ? C19 C20 C21 120(2) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 121(3) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 120(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 122(3) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C23 C24 C19 118(2) . . ? C23 C24 H24 120.8 . . ? C19 C24 H24 120.8 . . ? P1A O4A Sb1 138(2) . . ? P1A O5A Sb4 151(3) . . ? O3A P1A O5A 109(2) . . ? O3A P1A O4A 114.4(19) . . ? O5A P1A O4A 110(2) . . ? O3A P1A C1A 111.0(15) . . ? O5A P1A C1A 111.3(19) . . ? O4A P1A C1A 101.6(17) . . ? C2A C1A C6A 119.4(17) . . ? C2A C1A P1A 120(2) . . ? C6A C1A P1A 120(2) . . ? C1A C2A C3A 120(2) . . ? C1A C2A H2A 119.9 . . ? C3A C2A H2A 119.9 . . ? C4A C3A C2A 117(2) . . ? C4A C3A H3A 121.4 . . ? C2A C3A H3A 121.4 . . ? C5A C4A C3A 120(2) . . ? C5A C4A H4A 120.0 . . ? C3A C4A H4A 120.0 . . ? C4A C5A C6A 119(2) . . ? C4A C5A H5A 120.3 . . ? C6A C5A H5A 120.3 . . ? C1A C6A C5A 118(2) . . ? C1A C6A H6A 121.0 . . ? C5A C6A H6A 121.0 . . ? P2A O6A Sb2 155(4) . . ? P2A O7A Sb4 146(4) . . ? O6A P2A O8A 108(2) . . ? O6A P2A O7A 115(2) . . ? O8A P2A O7A 110(2) . . ? O6A P2A C7A 111(2) . . ? O8A P2A C7A 112.1(15) . . ? O7A P2A C7A 101.1(19) . . ? C8A C7A C12A 118.6(19) . . ? C8A C7A P2A 120(2) . . ? C12A C7A P2A 120(2) . . ? C7A C8A C9A 121(2) . . ? C7A C8A H8A 119.6 . . ? C9A C8A H8A 119.6 . . ? C10A C9A C8A 119(2) . . ? C10A C9A H9A 120.6 . . ? C8A C9A H9A 120.6 . . ? C11A C10A C9A 120(2) . . ? C11A C10A H10A 119.9 . . ? C9A C10A H10A 119.9 . . ? C10A C11A C12A 120(2) . . ? C10A C11A H11A 119.8 . . ? C12A C11A H11A 119.8 . . ? C7A C12A C11A 120(2) . . ? C7A C12A H12A 120.2 . . ? C11A C12A H12A 120.2 . . ? P3A O9A Sb2 161(3) . . ? P3A O10A Sb3 139(2) . . ? O9A P3A O10A 115(2) . . ? O9A P3A O11A 108(2) . . ? O10A P3A O11A 111.1(19) . . ? O9A P3A C13A 109.7(18) . . ? O10A P3A C13A 102.1(17) . . ? O11A P3A C13A 110.9(14) . . ? C14A C13A C18A 120.0 . . ? C14A C13A P3A 119.7(16) . . ? C18A C13A P3A 119.9(16) . . ? 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 . . ? 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 . . ? P4A O12A Sb1 151(4) . . ? P4A O13A Sb3 153(3) . . ? O12A P4A O13A 115(2) . . ? O12A P4A O14A 108(2) . . ? O13A P4A O14A 109(2) . . ? O12A P4A C19A 112(2) . . ? O13A P4A C19A 102.4(18) . . ? O14A P4A C19A 109.8(15) . . ? C20A C19A C24A 120.0 . . ? C20A C19A P4A 121.4(17) . . ? C24A C19A P4A 118.6(17) . . ? C21A C20A C19A 120.0 . . ? C21A C20A H20A 120.0 . . ? C19A C20A H20A 120.0 . . ? C22A C21A C20A 120.0 . . ? C22A C21A H21A 120.0 . . ? C20A C21A H21A 120.0 . . ? C21A C22A C23A 120.0 . . ? C21A C22A H22A 120.0 . . ? C23A C22A H22A 120.0 . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C19A 120.0 . . ? C23A C24A H24A 120.0 . . ? C19A C24A H24A 120.0 . . ? O15 P5 O16 112.8(6) . . ? O15 P5 O17 111.2(6) . . ? O16 P5 O17 110.3(5) . . ? O15 P5 C25 106.2(7) . . ? O16 P5 C25 105.8(6) . . ? O17 P5 C25 110.4(6) . . ? O19 P6 O20 114.3(6) . . ? O19 P6 O18 111.6(6) . . ? O20 P6 O18 108.6(5) . . ? O19 P6 C31 109.4(7) . . ? O20 P6 C31 104.8(6) . . ? O18 P6 C31 107.9(6) . . ? O22 P7 O23 111.9(6) . . ? O22 P7 O21 113.7(6) . . ? O23 P7 O21 109.4(5) . . ? O22 P7 C37 107.9(6) . . ? O23 P7 C37 107.8(6) . . ? O21 P7 C37 105.9(6) . . ? O24 P8 O26 111.3(6) . . ? O24 P8 O25 110.6(5) . . ? O26 P8 O25 111.8(6) . . ? O24 P8 C43 107.8(8) . . ? O26 P8 C43 108.9(8) . . ? O25 P8 C43 106.3(7) . . ? O24 P8 C43A 101(2) . . ? O26 P8 C43A 114.0(15) . . ? O25 P8 C43A 107.7(17) . . ? C43 P8 C43A 7(2) . . ? Sb2 O1 Sb1 136.3(5) . . ? Sb3 O2 Sb4 135.2(5) . . ? P5 O16 Sb2 133.2(6) . . ? P5 O17 Sb1 129.6(5) . . ? P6 O18 Sb2 133.7(6) . . ? P6 O20 Sb1 135.4(5) . . ? P7 O21 Sb3 132.9(6) . . ? P7 O23 Sb4 132.6(6) . . ? P8 O24 Sb3 133.1(6) . . ? P8 O25 Sb4 133.0(6) . . ? C30 C25 C26 121.2(16) . . ? C30 C25 P5 118.7(13) . . ? C26 C25 P5 120.1(12) . . ? C25 C26 C27 120.6(17) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C28 C27 C26 120.6(19) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C29 C28 C27 118(2) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? C28 C29 C30 122.2(19) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C25 C30 C29 117.0(17) . . ? C25 C30 H30 121.5 . . ? C29 C30 H30 121.5 . . ? C36 C31 C32 117.8(15) . . ? C36 C31 P6 122.2(13) . . ? C32 C31 P6 119.7(11) . . ? C31 C32 C33 117.7(15) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C34 C33 C32 121.9(19) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C33 C34 C35 120(2) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 118(2) . . ? C36 C35 H35 121.2 . . ? C34 C35 H35 121.2 . . ? C35 C36 C31 124.8(19) . . ? C35 C36 H36 117.6 . . ? C31 C36 H36 117.6 . . ? C38 C37 C42 116.6(15) . . ? C38 C37 P7 120.4(12) . . ? C42 C37 P7 123.0(12) . . ? C37 C38 C39 121.6(16) . . ? C37 C38 H38 119.2 . . ? C39 C38 H38 119.2 . . ? C40 C39 C38 119.7(18) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 120(2) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 119.0(19) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? C37 C42 C41 122.6(17) . . ? C37 C42 H42 118.7 . . ? C41 C42 H42 118.7 . . ? C44 C43 C48 120.0 . . ? C44 C43 P8 118.6(11) . . ? C48 C43 P8 121.2(11) . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C44A C43A C48A 118(2) . . ? C44A C43A P8 121(3) . . ? C48A C43A P8 120(3) . . ? C43A C44A C45A 122(2) . . ? C43A C44A H44A 119.2 . . ? C45A C44A H44A 119.2 . . ? C44A C45A C46A 119(2) . . ? C44A C45A H45A 120.4 . . ? C46A C45A H45A 120.4 . . ? C47A C46A C45A 119(2) . . ? C47A C46A H46A 120.4 . . ? C45A C46A H46A 120.4 . . ? C46A C47A C48A 120(2) . . ? C46A C47A H47A 120.0 . . ? C48A C47A H47A 120.0 . . ? C43A C48A C47A 121(2) . . ? C43A C48A H48A 119.7 . . ? C47A C48A H48A 119.7 . . ? C54 C49 C50 125.8(15) . . ? C54 C49 Sb1 117.4(12) . . ? C50 C49 Sb1 116.8(11) . . ? C49 C50 C51 119.5(17) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C52 C51 C50 116.7(19) . . ? C52 C51 H51 121.7 . . ? C50 C51 H51 121.7 . . ? C51 C52 C53 123.7(17) . . ? C51 C52 Cl2 117.7(15) . . ? C53 C52 Cl2 118.4(14) . . ? C52 C53 C54 118.0(17) . . ? C52 C53 H53 121.0 . . ? C54 C53 H53 121.0 . . ? C49 C54 C53 116.1(16) . . ? C49 C54 H54 122.0 . . ? C53 C54 H54 122.0 . . ? C56 C55 C60 120.6(14) . . ? C56 C55 Sb2 119.3(11) . . ? C60 C55 Sb2 119.9(10) . . ? C55 C56 C57 119.7(16) . . ? C55 C56 H56 120.2 . . ? C57 C56 H56 120.2 . . ? C58 C57 C56 118.0(15) . . ? C58 C57 H57 121.0 . . ? C56 C57 H57 121.0 . . ? C59 C58 C57 123.4(16) . . ? C59 C58 Cl3 118.6(14) . . ? C57 C58 Cl3 118.0(13) . . ? C58 C59 C60 118.6(16) . . ? C58 C59 H59 120.7 . . ? C60 C59 H59 120.7 . . ? C55 C60 C59 119.6(14) . . ? C55 C60 H60 120.2 . . ? C59 C60 H60 120.2 . . ? C66 C61 C62 120.8(14) . . ? C66 C61 Sb3 121.6(11) . . ? C62 C61 Sb3 117.6(11) . . ? C63 C62 C61 119.8(15) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 118.5(15) . . ? C62 C63 H63 120.8 . . ? C64 C63 H63 120.8 . . ? C65 C64 C63 122.7(16) . . ? C65 C64 Cl1 119.4(13) . . ? C63 C64 Cl1 117.9(12) . . ? C64 C65 C66 117.6(16) . . ? C64 C65 H65 121.2 . . ? C66 C65 H65 121.2 . . ? C61 C66 C65 120.6(15) . . ? C61 C66 H66 119.7 . . ? C65 C66 H66 119.7 . . ? C68 C67 C72 120.0 . . ? C68 C67 Sb4 122.5(4) . . ? C72 C67 Sb4 117.5(4) . . ? C67 C68 C69 120.0 . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C68 C69 C70 120.0 . . ? C68 C69 H69 120.0 . . ? C70 C69 H69 120.0 . . ? C69 C70 C71 120.0 . . ? C69 C70 Cl4 116.9 . . ? C71 C70 Cl4 123.0 . . ? C72 C71 C70 120.0 . . ? C72 C71 H71 120.0 . . ? C70 C71 H71 120.0 . . ? C71 C72 C67 120.0 . . ? C71 C72 H72 120.0 . . ? C67 C72 H72 120.0 . . ? Cl11 C100 Cl10 117.9(13) . . ? Cl11 C100 H10B 107.8 . . ? Cl10 C100 H10B 107.8 . . ? Cl11 C100 H10C 107.8 . . ? Cl10 C100 H10C 107.8 . . ? H10B C100 H10C 107.2 . . ? Cl13 C101 Cl12 119.0(13) . . ? Cl13 C101 H10D 107.6 . . ? Cl12 C101 H10D 107.6 . . ? Cl13 C101 H10E 107.6 . . ? Cl12 C101 H10E 107.6 . . ? H10D C101 H10E 107.0 . . ? Cl15 C102 Cl14 119.8(18) . . ? Cl15 C102 H10F 107.4 . . ? Cl14 C102 H10F 107.4 . . ? Cl15 C102 H10G 107.4 . . ? Cl14 C102 H10G 107.4 . . ? H10F C102 H10G 106.9 . . ? Cl17 C103 Cl16 114.1(18) . . ? Cl17 C103 H10H 108.7 . . ? Cl16 C103 H10H 108.7 . . ? Cl17 C103 H10I 108.7 . . ? Cl16 C103 H10I 108.7 . . ? H10H C103 H10I 107.6 . . ? Cl19 C104 Cl18 111.3(16) . . ? Cl19 C104 H10J 109.4 . . ? Cl18 C104 H10J 109.4 . . ? Cl19 C104 H10K 109.4 . . ? Cl18 C104 H10K 109.4 . . ? H10J C104 H10K 108.0 . . ? 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 Sb4 O4 P1 37(2) . . . . ? O5A Sb4 O4 P1 41(17) . . . . ? O7A Sb4 O4 P1 126(3) . . . . ? O25 Sb4 O4 P1 7(18) . . . . ? O6 Sb4 O4 P1 122(3) . . . . ? O23 Sb4 O4 P1 -54(2) . . . . ? C67 Sb4 O4 P1 -146(2) . . . . ? O1 Sb1 O5 P1 -90.0(18) . . . . ? O12A Sb1 O5 P1 -3(3) . . . . ? O20 Sb1 O5 P1 179.2(18) . . . . ? O13 Sb1 O5 P1 -0.6(19) . . . . ? O17 Sb1 O5 P1 -143(5) . . . . ? O4A Sb1 O5 P1 87(17) . . . . ? C49 Sb1 O5 P1 88.9(18) . . . . ? Sb1 O5 P1 O3 -25(2) . . . . ? Sb1 O5 P1 O4 103(2) . . . . ? Sb1 O5 P1 C1 -147.1(16) . . . . ? Sb4 O4 P1 O3 29(3) . . . . ? Sb4 O4 P1 O5 -97(3) . . . . ? Sb4 O4 P1 C1 149(2) . . . . ? O3 P1 C1 C2 -5.0(12) . . . . ? O5 P1 C1 C2 117.3(10) . . . . ? O4 P1 C1 C2 -126.8(11) . . . . ? O3 P1 C1 C6 172.8(9) . . . . ? O5 P1 C1 C6 -64.9(12) . . . . ? O4 P1 C1 C6 51.0(12) . . . . ? C6 C1 C2 C3 0.0 . . . . ? P1 C1 C2 C3 177.8(13) . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C1 0.0 . . . . ? C2 C1 C6 C5 0.0 . . . . ? P1 C1 C6 C5 -177.8(13) . . . . ? O2 Sb4 O6 P2 88(2) . . . . ? O5A Sb4 O6 P2 6(3) . . . . ? O7A Sb4 O6 P2 -132(23) . . . . ? O25 Sb4 O6 P2 178(2) . . . . ? O4 Sb4 O6 P2 0(2) . . . . ? O23 Sb4 O6 P2 111(10) . . . . ? C67 Sb4 O6 P2 -90(2) . . . . ? O1 Sb2 O7 P2 -30(3) . . . . ? O6A Sb2 O7 P2 -62(19) . . . . ? O9A Sb2 O7 P2 -115(3) . . . . ? O10 Sb2 O7 P2 -120(3) . . . . ? O16 Sb2 O7 P2 26(16) . . . . ? O18 Sb2 O7 P2 61(3) . . . . ? C55 Sb2 O7 P2 151(3) . . . . ? Sb4 O6 P2 O8 24(3) . . . . ? Sb4 O6 P2 O7 -101(2) . . . . ? Sb4 O6 P2 C7 147(2) . . . . ? Sb2 O7 P2 O6 94(3) . . . . ? Sb2 O7 P2 O8 -30(3) . . . . ? Sb2 O7 P2 C7 -152(3) . . . . ? O6 P2 C7 C8 -109.2(12) . . . . ? O8 P2 C7 C8 12.4(13) . . . . ? O7 P2 C7 C8 134.4(12) . . . . ? O6 P2 C7 C12 73.7(12) . . . . ? O8 P2 C7 C12 -164.6(10) . . . . ? O7 P2 C7 C12 -42.7(13) . . . . ? C12 C7 C8 C9 0.0 . . . . ? P2 C7 C8 C9 -177.1(14) . . . . ? C7 C8 C9 C10 0.0 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C7 0.0 . . . . ? C8 C7 C12 C11 0.0 . . . . ? P2 C7 C12 C11 177.0(15) . . . . ? O2 Sb3 O9 P3 42.3(19) . . . . ? O12 Sb3 O9 P3 127(2) . . . . ? O21 Sb3 O9 P3 60(13) . . . . ? O24 Sb3 O9 P3 -48(2) . . . . ? O10A Sb3 O9 P3 -62(13) . . . . ? O13A Sb3 O9 P3 131(2) . . . . ? C61 Sb3 O9 P3 -139.4(19) . . . . ? O1 Sb2 O10 P3 -75.5(19) . . . . ? O6A Sb2 O10 P3 9(2) . . . . ? O9A Sb2 O10 P3 -85(25) . . . . ? O7 Sb2 O10 P3 14(2) . . . . ? O16 Sb2 O10 P3 -164.9(19) . . . . ? O18 Sb2 O10 P3 163(8) . . . . ? C55 Sb2 O10 P3 103.4(19) . . . . ? Sb2 O10 P3 O11 -37(2) . . . . ? Sb2 O10 P3 O9 90(2) . . . . ? Sb2 O10 P3 C13 -156.7(18) . . . . ? Sb3 O9 P3 O11 14(2) . . . . ? Sb3 O9 P3 O10 -109(2) . . . . ? Sb3 O9 P3 C13 138(2) . . . . ? O11 P3 C13 C14 -179.8(18) . . . . ? O10 P3 C13 C14 -63(2) . . . . ? O9 P3 C13 C14 54(2) . . . . ? O11 P3 C13 C18 7(2) . . . . ? O10 P3 C13 C18 124(2) . . . . ? O9 P3 C13 C18 -120(2) . . . . ? C18 C13 C14 C15 1(3) . . . . ? P3 C13 C14 C15 -173.1(19) . . . . ? C13 C14 C15 C16 -4(3) . . . . ? C14 C15 C16 C17 6(4) . . . . ? C15 C16 C17 C18 -3(4) . . . . ? C14 C13 C18 C17 3(4) . . . . ? P3 C13 C18 C17 176.2(19) . . . . ? C16 C17 C18 C13 -2(4) . . . . ? O2 Sb3 O12 P4 104(3) . . . . ? O9 Sb3 O12 P4 17(3) . . . . ? O21 Sb3 O12 P4 -165(3) . . . . ? O24 Sb3 O12 P4 125(6) . . . . ? O10A Sb3 O12 P4 16(3) . . . . ? O13A Sb3 O12 P4 -124(17) . . . . ? C61 Sb3 O12 P4 -73(3) . . . . ? O1 Sb1 O13 P4 -20(3) . . . . ? O12A Sb1 O13 P4 -36(47) . . . . ? O5 Sb1 O13 P4 -106(3) . . . . ? O20 Sb1 O13 P4 78(20) . . . . ? O17 Sb1 O13 P4 71(3) . . . . ? O4A Sb1 O13 P4 -112(3) . . . . ? C49 Sb1 O13 P4 162(3) . . . . ? Sb3 O12 P4 O13 -113(3) . . . . ? Sb3 O12 P4 O14 12(3) . . . . ? Sb3 O12 P4 C19 128(3) . . . . ? Sb1 O13 P4 O12 76(3) . . . . ? Sb1 O13 P4 O14 -46(3) . . . . ? Sb1 O13 P4 C19 -165(3) . . . . ? O12 P4 C19 C20 -116(2) . . . . ? O13 P4 C19 C20 123(3) . . . . ? O14 P4 C19 C20 0(3) . . . . ? O12 P4 C19 C24 66(2) . . . . ? O13 P4 C19 C24 -55(2) . . . . ? O14 P4 C19 C24 -177.7(19) . . . . ? C24 C19 C20 C21 2(4) . . . . ? P4 C19 C20 C21 -176(2) . . . . ? C19 C20 C21 C22 -3(4) . . . . ? C20 C21 C22 C23 2(5) . . . . ? C21 C22 C23 C24 1(5) . . . . ? C22 C23 C24 C19 -2(4) . . . . ? C20 C19 C24 C23 0(4) . . . . ? P4 C19 C24 C23 178(2) . . . . ? O1 Sb1 O4A P1A 19(5) . . . . ? O12A Sb1 O4A P1A 106(5) . . . . ? O5 Sb1 O4A P1A 16(13) . . . . ? O20 Sb1 O4A P1A -72(5) . . . . ? O13 Sb1 O4A P1A 109(5) . . . . ? O17 Sb1 O4A P1A -108(11) . . . . ? C49 Sb1 O4A P1A -162(5) . . . . ? O2 Sb4 O5A P1A -109(7) . . . . ? O7A Sb4 O5A P1A -19(7) . . . . ? O25 Sb4 O5A P1A -113(10) . . . . ? O6 Sb4 O5A P1A -23(7) . . . . ? O4 Sb4 O5A P1A 76(18) . . . . ? O23 Sb4 O5A P1A 160(6) . . . . ? C67 Sb4 O5A P1A 69(7) . . . . ? Sb4 O5A P1A O3A 7(7) . . . . ? Sb4 O5A P1A O4A 133(6) . . . . ? Sb4 O5A P1A C1A -115(6) . . . . ? Sb1 O4A P1A O3A 40(5) . . . . ? Sb1 O4A P1A O5A -83(5) . . . . ? Sb1 O4A P1A C1A 159(4) . . . . ? O3A P1A C1A C2A 177(4) . . . . ? O5A P1A C1A C2A -62(5) . . . . ? O4A P1A C1A C2A 54(5) . . . . ? O3A P1A C1A C6A -16(5) . . . . ? O5A P1A C1A C6A 105(5) . . . . ? O4A P1A C1A C6A -138(5) . . . . ? C6A C1A C2A C3A -5(8) . . . . ? P1A C1A C2A C3A 162(5) . . . . ? C1A C2A C3A C4A 22(9) . . . . ? C2A C3A C4A C5A -18(9) . . . . ? C3A C4A C5A C6A -3(9) . . . . ? C2A C1A C6A C5A -16(8) . . . . ? P1A C1A C6A C5A 177(5) . . . . ? C4A C5A C6A C1A 20(9) . . . . ? O1 Sb2 O6A P2A 105(9) . . . . ? O9A Sb2 O6A P2A 21(9) . . . . ? O10 Sb2 O6A P2A 15(9) . . . . ? O7 Sb2 O6A P2A -107(24) . . . . ? O16 Sb2 O6A P2A 97(16) . . . . ? O18 Sb2 O6A P2A -163(9) . . . . ? C55 Sb2 O6A P2A -73(9) . . . . ? O2 Sb4 O7A P2A -8(6) . . . . ? O5A Sb4 O7A P2A -89(7) . . . . ? O25 Sb4 O7A P2A 83(6) . . . . ? O6 Sb4 O7A P2A -47(17) . . . . ? O4 Sb4 O7A P2A -95(6) . . . . ? O23 Sb4 O7A P2A 96(17) . . . . ? C67 Sb4 O7A P2A 175(6) . . . . ? Sb2 O6A P2A O8A 4(9) . . . . ? Sb2 O6A P2A O7A -119(9) . . . . ? Sb2 O6A P2A C7A 127(9) . . . . ? Sb4 O7A P2A O6A 67(7) . . . . ? Sb4 O7A P2A O8A -55(7) . . . . ? Sb4 O7A P2A C7A -173(6) . . . . ? O6A P2A C7A C8A 46(6) . . . . ? O8A P2A C7A C8A 167(5) . . . . ? O7A P2A C7A C8A -76(6) . . . . ? O6A P2A C7A C12A -119(6) . . . . ? O8A P2A C7A C12A 2(6) . . . . ? O7A P2A C7A C12A 119(6) . . . . ? C12A C7A C8A C9A -14(10) . . . . ? P2A C7A C8A C9A -179(6) . . . . ? C7A C8A C9A C10A 7(11) . . . . ? C8A C9A C10A C11A 0(12) . . . . ? C9A C10A C11A C12A 0(12) . . . . ? C8A C7A C12A C11A 14(10) . . . . ? P2A C7A C12A C11A 180(6) . . . . ? C10A C11A C12A C7A -8(11) . . . . ? O1 Sb2 O9A P3A 19(13) . . . . ? O6A Sb2 O9A P3A 103(13) . . . . ? O10 Sb2 O9A P3A -170(37) . . . . ? O7 Sb2 O9A P3A 108(13) . . . . ? O16 Sb2 O9A P3A -70(13) . . . . ? O18 Sb2 O9A P3A -28(30) . . . . ? C55 Sb2 O9A P3A -162(13) . . . . ? O2 Sb3 O10A P3A -82(5) . . . . ? O12 Sb3 O10A P3A 2(5) . . . . ? O9 Sb3 O10A P3A -7(9) . . . . ? O21 Sb3 O10A P3A -171(8) . . . . ? O24 Sb3 O10A P3A -173(5) . . . . ? O13A Sb3 O10A P3A 6(6) . . . . ? C61 Sb3 O10A P3A 95(5) . . . . ? Sb2 O9A P3A O10A -86(13) . . . . ? Sb2 O9A P3A O11A 38(13) . . . . ? Sb2 O9A P3A C13A 159(12) . . . . ? Sb3 O10A P3A O9A 90(5) . . . . ? Sb3 O10A P3A O11A -33(6) . . . . ? Sb3 O10A P3A C13A -151(5) . . . . ? O9A P3A C13A C14A 50(4) . . . . ? O10A P3A C13A C14A -73(3) . . . . ? O11A P3A C13A C14A 169(3) . . . . ? O9A P3A C13A C18A -123(4) . . . . ? O10A P3A C13A C18A 114(3) . . . . ? O11A P3A C13A C18A -4(3) . . . . ? C18A C13A C14A C15A 0.0 . . . . ? P3A C13A C14A C15A -173(4) . . . . ? 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 . . . . ? P3A C13A C18A C17A 173(4) . . . . ? O1 Sb1 O12A P4A 89(9) . . . . ? O5 Sb1 O12A P4A 3(9) . . . . ? O20 Sb1 O12A P4A 120(33) . . . . ? O13 Sb1 O12A P4A -108(52) . . . . ? O17 Sb1 O12A P4A 179(9) . . . . ? O4A Sb1 O12A P4A -4(9) . . . . ? C49 Sb1 O12A P4A -90(9) . . . . ? O2 Sb3 O13A P4A -10(7) . . . . ? O12 Sb3 O13A P4A -58(13) . . . . ? O9 Sb3 O13A P4A -96(8) . . . . ? O21 Sb3 O13A P4A 82(7) . . . . ? O24 Sb3 O13A P4A 75(15) . . . . ? O10A Sb3 O13A P4A -98(7) . . . . ? C61 Sb3 O13A P4A 174(7) . . . . ? Sb1 O12A P4A O13A -100(9) . . . . ? Sb1 O12A P4A O14A 23(9) . . . . ? Sb1 O12A P4A C19A 144(8) . . . . ? Sb3 O13A P4A O12A 71(8) . . . . ? Sb3 O13A P4A O14A -51(8) . . . . ? Sb3 O13A P4A C19A -167(7) . . . . ? O12A P4A C19A C20A 79(4) . . . . ? O13A P4A C19A C20A -45(4) . . . . ? O14A P4A C19A C20A -161(3) . . . . ? O12A P4A C19A C24A -100(4) . . . . ? O13A P4A C19A C24A 136(4) . . . . ? O14A P4A C19A C24A 20(4) . . . . ? C24A C19A C20A C21A 0.0 . . . . ? P4A C19A C20A C21A -179(4) . . . . ? C19A C20A C21A C22A 0.0 . . . . ? C20A C21A C22A C23A 0.0 . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C22A C23A C24A C19A 0.0 . . . . ? C20A C19A C24A C23A 0.0 . . . . ? P4A C19A C24A C23A 179(4) . . . . ? O6A Sb2 O1 Sb1 133.9(17) . . . . ? O9A Sb2 O1 Sb1 -134.6(19) . . . . ? O10 Sb2 O1 Sb1 -135.5(9) . . . . ? O7 Sb2 O1 Sb1 130.8(9) . . . . ? O16 Sb2 O1 Sb1 -47.0(7) . . . . ? O18 Sb2 O1 Sb1 41.4(7) . . . . ? C55 Sb2 O1 Sb1 -167(12) . . . . ? O12A Sb1 O1 Sb2 138.1(18) . . . . ? O5 Sb1 O1 Sb2 -128.9(9) . . . . ? O20 Sb1 O1 Sb2 -40.5(7) . . . . ? O13 Sb1 O1 Sb2 137.3(9) . . . . ? O17 Sb1 O1 Sb2 46.9(7) . . . . ? O4A Sb1 O1 Sb2 -129.2(16) . . . . ? C49 Sb1 O1 Sb2 -165(15) . . . . ? O12 Sb3 O2 Sb4 131.8(8) . . . . ? O9 Sb3 O2 Sb4 -139.4(8) . . . . ? O21 Sb3 O2 Sb4 41.3(7) . . . . ? O24 Sb3 O2 Sb4 -46.2(7) . . . . ? O10A Sb3 O2 Sb4 -131.2(11) . . . . ? O13A Sb3 O2 Sb4 126.7(16) . . . . ? C61 Sb3 O2 Sb4 -164(6) . . . . ? O5A Sb4 O2 Sb3 -134.5(16) . . . . ? O7A Sb4 O2 Sb3 132.1(18) . . . . ? O25 Sb4 O2 Sb3 44.9(7) . . . . ? O6 Sb4 O2 Sb3 135.6(9) . . . . ? O4 Sb4 O2 Sb3 -134.0(8) . . . . ? O23 Sb4 O2 Sb3 -43.1(7) . . . . ? C67 Sb4 O2 Sb3 178(100) . . . . ? O15 P5 O16 Sb2 -76.8(8) . . . . ? O17 P5 O16 Sb2 48.2(9) . . . . ? C25 P5 O16 Sb2 167.5(8) . . . . ? O1 Sb2 O16 P5 -9.7(8) . . . . ? O6A Sb2 O16 P5 -1(14) . . . . ? O9A Sb2 O16 P5 74.9(16) . . . . ? O10 Sb2 O16 P5 80.4(9) . . . . ? O7 Sb2 O16 P5 -67(14) . . . . ? O18 Sb2 O16 P5 -101.5(8) . . . . ? C55 Sb2 O16 P5 168.5(8) . . . . ? O15 P5 O17 Sb1 79.1(9) . . . . ? O16 P5 O17 Sb1 -46.8(10) . . . . ? C25 P5 O17 Sb1 -163.3(8) . . . . ? O1 Sb1 O17 P5 9.4(8) . . . . ? O12A Sb1 O17 P5 -78(2) . . . . ? O5 Sb1 O17 P5 62(6) . . . . ? O20 Sb1 O17 P5 100.0(8) . . . . ? O13 Sb1 O17 P5 -80.3(10) . . . . ? O4A Sb1 O17 P5 136(12) . . . . ? C49 Sb1 O17 P5 -169.7(9) . . . . ? O19 P6 O18 Sb2 86.0(9) . . . . ? O20 P6 O18 Sb2 -40.8(10) . . . . ? C31 P6 O18 Sb2 -153.8(8) . . . . ? O1 Sb2 O18 P6 7.6(8) . . . . ? O6A Sb2 O18 P6 -76.5(18) . . . . ? O9A Sb2 O18 P6 55(19) . . . . ? O10 Sb2 O18 P6 129(9) . . . . ? O7 Sb2 O18 P6 -81.5(10) . . . . ? O16 Sb2 O18 P6 97.0(8) . . . . ? C55 Sb2 O18 P6 -171.4(9) . . . . ? O19 P6 O20 Sb1 -81.7(9) . . . . ? O18 P6 O20 Sb1 43.5(10) . . . . ? C31 P6 O20 Sb1 158.5(8) . . . . ? O1 Sb1 O20 P6 -11.1(8) . . . . ? O12A Sb1 O20 P6 -42(37) . . . . ? O5 Sb1 O20 P6 75.1(9) . . . . ? O13 Sb1 O20 P6 -108(19) . . . . ? O17 Sb1 O20 P6 -101.7(8) . . . . ? O4A Sb1 O20 P6 81.2(13) . . . . ? C49 Sb1 O20 P6 167.5(8) . . . . ? O22 P7 O21 Sb3 78.3(9) . . . . ? O23 P7 O21 Sb3 -47.6(9) . . . . ? C37 P7 O21 Sb3 -163.5(7) . . . . ? O2 Sb3 O21 P7 12.6(8) . . . . ? O12 Sb3 O21 P7 -71.7(9) . . . . ? O9 Sb3 O21 P7 -5(13) . . . . ? O24 Sb3 O21 P7 103.1(8) . . . . ? O10A Sb3 O21 P7 101(13) . . . . ? O13A Sb3 O21 P7 -76.1(15) . . . . ? C61 Sb3 O21 P7 -165.7(8) . . . . ? O22 P7 O23 Sb4 -83.2(8) . . . . ? O21 P7 O23 Sb4 43.7(9) . . . . ? C37 P7 O23 Sb4 158.3(7) . . . . ? O2 Sb4 O23 P7 -7.4(7) . . . . ? O5A Sb4 O23 P7 74.2(16) . . . . ? O7A Sb4 O23 P7 -111(17) . . . . ? O25 Sb4 O23 P7 -98.1(7) . . . . ? O6 Sb4 O23 P7 -30(11) . . . . ? O4 Sb4 O23 P7 80.0(8) . . . . ? C67 Sb4 O23 P7 170.4(7) . . . . ? O26 P8 O24 Sb3 -83.5(9) . . . . ? O25 P8 O24 Sb3 41.4(10) . . . . ? C43 P8 O24 Sb3 157.2(9) . . . . ? C43A P8 O24 Sb3 155.2(15) . . . . ? O2 Sb3 O24 P8 -5.4(8) . . . . ? O12 Sb3 O24 P8 -27(7) . . . . ? O9 Sb3 O24 P8 80.7(10) . . . . ? O21 Sb3 O24 P8 -97.1(8) . . . . ? O10A Sb3 O24 P8 82.7(18) . . . . ? O13A Sb3 O24 P8 -90(11) . . . . ? C61 Sb3 O24 P8 171.0(9) . . . . ? O24 P8 O25 Sb4 -43.9(10) . . . . ? O26 P8 O25 Sb4 80.7(9) . . . . ? C43 P8 O25 Sb4 -160.7(9) . . . . ? C43A P8 O25 Sb4 -153(2) . . . . ? O2 Sb4 O25 P8 8.9(8) . . . . ? O5A Sb4 O25 P8 13(11) . . . . ? O7A Sb4 O25 P8 -80.9(16) . . . . ? O6 Sb4 O25 P8 -76.7(10) . . . . ? O4 Sb4 O25 P8 39(16) . . . . ? O23 Sb4 O25 P8 100.1(8) . . . . ? C67 Sb4 O25 P8 -168.6(8) . . . . ? O15 P5 C25 C30 38.9(14) . . . . ? O16 P5 C25 C30 159.0(12) . . . . ? O17 P5 C25 C30 -81.7(14) . . . . ? O15 P5 C25 C26 -141.1(13) . . . . ? O16 P5 C25 C26 -21.0(14) . . . . ? O17 P5 C25 C26 98.3(13) . . . . ? C30 C25 C26 C27 -2(2) . . . . ? P5 C25 C26 C27 177.7(12) . . . . ? C25 C26 C27 C28 2(3) . . . . ? C26 C27 C28 C29 -2(3) . . . . ? C27 C28 C29 C30 2(3) . . . . ? C26 C25 C30 C29 2(2) . . . . ? P5 C25 C30 C29 -177.9(12) . . . . ? C28 C29 C30 C25 -2(3) . . . . ? O19 P6 C31 C36 -177.9(12) . . . . ? O20 P6 C31 C36 -55.0(14) . . . . ? O18 P6 C31 C36 60.6(14) . . . . ? O19 P6 C31 C32 -4.1(14) . . . . ? O20 P6 C31 C32 118.9(12) . . . . ? O18 P6 C31 C32 -125.6(12) . . . . ? C36 C31 C32 C33 -2(2) . . . . ? P6 C31 C32 C33 -176.1(11) . . . . ? C31 C32 C33 C34 0(2) . . . . ? C32 C33 C34 C35 2(3) . . . . ? C33 C34 C35 C36 -3(3) . . . . ? C34 C35 C36 C31 1(3) . . . . ? C32 C31 C36 C35 1(3) . . . . ? P6 C31 C36 C35 175.2(15) . . . . ? O22 P7 C37 C38 -28.6(14) . . . . ? O23 P7 C37 C38 92.4(13) . . . . ? O21 P7 C37 C38 -150.6(12) . . . . ? O22 P7 C37 C42 150.6(13) . . . . ? O23 P7 C37 C42 -88.4(14) . . . . ? O21 P7 C37 C42 28.6(15) . . . . ? C42 C37 C38 C39 1(2) . . . . ? P7 C37 C38 C39 -179.8(13) . . . . ? C37 C38 C39 C40 -1(3) . . . . ? C38 C39 C40 C41 0(3) . . . . ? C39 C40 C41 C42 1(3) . . . . ? C38 C37 C42 C41 0(3) . . . . ? P7 C37 C42 C41 -178.8(13) . . . . ? C40 C41 C42 C37 -2(3) . . . . ? O24 P8 C43 C44 36.8(11) . . . . ? O26 P8 C43 C44 -84.0(11) . . . . ? O25 P8 C43 C44 155.4(9) . . . . ? C43A P8 C43 C44 53(14) . . . . ? O24 P8 C43 C48 -148.1(10) . . . . ? O26 P8 C43 C48 91.0(11) . . . . ? O25 P8 C43 C48 -29.5(12) . . . . ? C43A P8 C43 C48 -132(15) . . . . ? C48 C43 C44 C45 0.0 . . . . ? P8 C43 C44 C45 175.1(15) . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C43 0.0 . . . . ? C44 C43 C48 C47 0.0 . . . . ? P8 C43 C48 C47 -175.0(15) . . . . ? O24 P8 C43A C44A -63(6) . . . . ? O26 P8 C43A C44A 178(5) . . . . ? O25 P8 C43A C44A 53(6) . . . . ? C43 P8 C43A C44A 132(18) . . . . ? O24 P8 C43A C48A 110(5) . . . . ? O26 P8 C43A C48A -9(6) . . . . ? O25 P8 C43A C48A -134(4) . . . . ? C43 P8 C43A C48A -55(12) . . . . ? C48A C43A C44A C45A 3(10) . . . . ? P8 C43A C44A C45A 176(5) . . . . ? C43A C44A C45A C46A 7(10) . . . . ? C44A C45A C46A C47A -8(9) . . . . ? C45A C46A C47A C48A -1(7) . . . . ? C44A C43A C48A C47A -12(8) . . . . ? P8 C43A C48A C47A 174(4) . . . . ? C46A C47A C48A C43A 11(7) . . . . ? O1 Sb1 C49 C54 -24(16) . . . . ? O12A Sb1 C49 C54 32(2) . . . . ? O5 Sb1 C49 C54 -60.5(13) . . . . ? O20 Sb1 C49 C54 -149.0(12) . . . . ? O13 Sb1 C49 C54 33.2(13) . . . . ? O17 Sb1 C49 C54 123.7(12) . . . . ? O4A Sb1 C49 C54 -60.3(19) . . . . ? O1 Sb1 C49 C50 157(15) . . . . ? O12A Sb1 C49 C50 -146(2) . . . . ? O5 Sb1 C49 C50 120.8(13) . . . . ? O20 Sb1 C49 C50 32.3(12) . . . . ? O13 Sb1 C49 C50 -145.5(13) . . . . ? O17 Sb1 C49 C50 -55.0(12) . . . . ? O4A Sb1 C49 C50 121.0(18) . . . . ? C54 C49 C50 C51 -1(3) . . . . ? Sb1 C49 C50 C51 177.4(12) . . . . ? C49 C50 C51 C52 -2(3) . . . . ? C50 C51 C52 C53 5(3) . . . . ? C50 C51 C52 Cl2 -179.0(13) . . . . ? C51 C52 C53 C54 -6(3) . . . . ? Cl2 C52 C53 C54 178.7(12) . . . . ? C50 C49 C54 C53 1(2) . . . . ? Sb1 C49 C54 C53 -177.7(11) . . . . ? C52 C53 C54 C49 2(2) . . . . ? O1 Sb2 C55 C56 -19(13) . . . . ? O6A Sb2 C55 C56 39.3(19) . . . . ? O9A Sb2 C55 C56 -52(2) . . . . ? O10 Sb2 C55 C56 -51.1(13) . . . . ? O7 Sb2 C55 C56 42.6(13) . . . . ? O16 Sb2 C55 C56 -139.5(12) . . . . ? O18 Sb2 C55 C56 132.0(12) . . . . ? O1 Sb2 C55 C60 167(12) . . . . ? O6A Sb2 C55 C60 -134.4(19) . . . . ? O9A Sb2 C55 C60 134(2) . . . . ? O10 Sb2 C55 C60 135.2(13) . . . . ? O7 Sb2 C55 C60 -131.1(12) . . . . ? O16 Sb2 C55 C60 46.8(11) . . . . ? O18 Sb2 C55 C60 -41.7(11) . . . . ? C60 C55 C56 C57 -5(2) . . . . ? Sb2 C55 C56 C57 -178.5(11) . . . . ? C55 C56 C57 C58 4(2) . . . . ? C56 C57 C58 C59 -2(3) . . . . ? C56 C57 C58 Cl3 176.7(12) . . . . ? C57 C58 C59 C60 2(3) . . . . ? Cl3 C58 C59 C60 -177.1(12) . . . . ? C56 C55 C60 C59 4(2) . . . . ? Sb2 C55 C60 C59 178.0(11) . . . . ? C58 C59 C60 C55 -3(2) . . . . ? O2 Sb3 C61 C66 162(6) . . . . ? O12 Sb3 C61 C66 -134.0(12) . . . . ? O9 Sb3 C61 C66 137.5(12) . . . . ? O21 Sb3 C61 C66 -43.3(12) . . . . ? O24 Sb3 C61 C66 44.3(12) . . . . ? O10A Sb3 C61 C66 129.3(15) . . . . ? O13A Sb3 C61 C66 -128.7(19) . . . . ? O2 Sb3 C61 C62 -19(7) . . . . ? O12 Sb3 C61 C62 45.1(12) . . . . ? O9 Sb3 C61 C62 -43.4(11) . . . . ? O21 Sb3 C61 C62 135.8(11) . . . . ? O24 Sb3 C61 C62 -136.6(11) . . . . ? O10A Sb3 C61 C62 -51.6(14) . . . . ? O13A Sb3 C61 C62 50.4(18) . . . . ? C66 C61 C62 C63 -2(2) . . . . ? Sb3 C61 C62 C63 178.6(11) . . . . ? C61 C62 C63 C64 2(2) . . . . ? C62 C63 C64 C65 -1(2) . . . . ? C62 C63 C64 Cl1 179.3(11) . . . . ? C63 C64 C65 C66 2(2) . . . . ? Cl1 C64 C65 C66 -179.1(12) . . . . ? C62 C61 C66 C65 3(2) . . . . ? Sb3 C61 C66 C65 -178.4(11) . . . . ? C64 C65 C66 C61 -2(2) . . . . ? O2 Sb4 C67 C68 9(6) . . . . ? O5A Sb4 C67 C68 -38.3(15) . . . . ? O7A Sb4 C67 C68 54.9(17) . . . . ? O25 Sb4 C67 C68 142.0(5) . . . . ? O6 Sb4 C67 C68 51.2(7) . . . . ? O4 Sb4 C67 C68 -39.0(7) . . . . ? O23 Sb4 C67 C68 -130.0(5) . . . . ? O2 Sb4 C67 C72 -171(6) . . . . ? O5A Sb4 C67 C72 141.9(15) . . . . ? O7A Sb4 C67 C72 -124.9(17) . . . . ? O25 Sb4 C67 C72 -37.8(5) . . . . ? O6 Sb4 C67 C72 -128.6(7) . . . . ? O4 Sb4 C67 C72 141.2(7) . . . . ? O23 Sb4 C67 C72 50.2(5) . . . . ? C72 C67 C68 C69 0.0 . . . . ? Sb4 C67 C68 C69 -179.8(5) . . . . ? C67 C68 C69 C70 0.0 . . . . ? C68 C69 C70 C71 0.0 . . . . ? C68 C69 C70 Cl4 -176.3 . . . . ? C69 C70 C71 C72 0.0 . . . . ? Cl4 C70 C71 C72 176.0 . . . . ? C70 C71 C72 C67 0.0 . . . . ? C68 C67 C72 C71 0.0 . . . . ? Sb4 C67 C72 C71 179.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.991 _refine_diff_density_min -1.399 _refine_diff_density_rms 0.223 # Attachment '2.cif' data_mono769 _database_code_depnum_ccdc_archive 'CCDC 700895' _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 which is typical in these structures. 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 '3.cif' data_orepw855 _database_code_depnum_ccdc_archive 'CCDC 700896' _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 ; 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. Largest residual peak was attempted to be modelled as an oxygen but would not refine. Remaining residuals are attributable to electron density around antimony atoms. Unaccounted for twinning was investigated and could not be found. Although there is a solvent void of 34 A**3 this could at most accomodate one solvent methanol which could not be reliably found from the data. ; _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 '4.cif' data_orepw844p43212 _database_code_depnum_ccdc_archive 'CCDC 700897' _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 ; The solvent void of 208.00 A**3 was due to solvent Q peaks but it was very difficult to solve them due to symmetry present in the solvent molecules. 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. Integration was attempted using Twin rules in the reduction program,but did not improve the data. The large ADP max/min ratio for the phenyl ring C7-C12 was investigated and modelling of disorder was found to be inapproriate. Retraints were attempted but resulted in numerous atoms going NPD so the ring was left with the inconsistent ADP parameteres. Squeeze was considered but not used as it was not expected to be very effective in this case. 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 '5.cif' data_orepw610pb1 _database_code_depnum_ccdc_archive 'CCDC 700898' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H62 Cl2 O19 P6 Sb2' _chemical_formula_weight 1299.08 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' 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 10.4506(19) _cell_length_b 11.6444(18) _cell_length_c 22.684(3) _cell_angle_alpha 94.982(13) _cell_angle_beta 99.542(14) _cell_angle_gamma 90.679(13) _cell_volume 2711.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9873 _cell_measurement_theta_min 2.6400 _cell_measurement_theta_max 28.0788 _exptl_crystal_description block _exptl_crystal_colour colourless _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 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.337 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6898 _exptl_absorpt_correction_T_max 0.8779 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) 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 29942 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.1397 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9551 _reflns_number_gt 5296 _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 few residual Q peaks were due to heavy element Sb so were left as such. Unaccounted for twinning was investigated and could not be 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^)+(0.0731P)^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 9551 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 0.28465(5) 0.68244(4) 0.33596(2) 0.02243(16) Uani 1 1 d . . . Sb2 Sb 0.26590(5) 0.71387(4) 0.17947(2) 0.02310(16) Uani 1 1 d . . . P1 P 0.57505(19) 0.81431(18) 0.35968(9) 0.0263(5) Uani 1 1 d . . . P2 P 0.2046(2) 0.91986(17) 0.27782(9) 0.0253(5) Uani 1 1 d . . . P3 P 0.5582(2) 0.8353(2) 0.16369(11) 0.0417(6) Uani 1 1 d . . . P4 P 0.46367(19) 0.45445(18) 0.31757(9) 0.0262(5) Uani 1 1 d . . . P5 P 0.08492(19) 0.53350(17) 0.23157(9) 0.0222(5) Uani 1 1 d . . . P6 P 0.4420(3) 0.4953(2) 0.12049(11) 0.0485(7) Uani 1 1 d . . . C1 C 0.2164(6) 0.6813(6) 0.4177(3) 0.0230(18) Uani 1 1 d . . . C2 C 0.1855(7) 0.5762(6) 0.4379(3) 0.0236(18) Uani 1 1 d . . . H2 H 0.1987 0.5060 0.4153 0.028 Uiso 1 1 calc R . . C3 C 0.1360(7) 0.5735(6) 0.4907(3) 0.0253(18) Uani 1 1 d . . . H3 H 0.1164 0.5023 0.5051 0.030 Uiso 1 1 calc R . . C4 C 0.1161(7) 0.6766(7) 0.5217(3) 0.0244(18) Uani 1 1 d . . . C5 C 0.1513(7) 0.7814(6) 0.5039(3) 0.029(2) Uani 1 1 d . . . H5 H 0.1412 0.8514 0.5273 0.035 Uiso 1 1 calc R . . C6 C 0.2017(7) 0.7817(6) 0.4511(3) 0.0245(18) Uani 1 1 d . . . H6 H 0.2264 0.8528 0.4381 0.029 Uiso 1 1 calc R . . C7 C 0.1780(7) 0.7540(6) 0.0934(3) 0.0267(19) Uani 1 1 d . . . C8 C 0.0590(9) 0.8015(7) 0.0860(4) 0.042(2) Uani 1 1 d . . . H8 H 0.0132 0.8122 0.1188 0.050 Uiso 1 1 calc R . . C9 C 0.0045(9) 0.8344(8) 0.0300(4) 0.050(3) Uani 1 1 d . . . H9 H -0.0789 0.8672 0.0238 0.060 Uiso 1 1 calc R . . C10 C 0.0740(9) 0.8184(8) -0.0158(3) 0.040(2) Uani 1 1 d . . . C11 C 0.1884(10) 0.7688(7) -0.0096(4) 0.046(2) Uani 1 1 d . . . H11 H 0.2308 0.7537 -0.0433 0.055 Uiso 1 1 calc R . . C12 C 0.2442(8) 0.7397(6) 0.0449(4) 0.031(2) Uani 1 1 d . . . H12 H 0.3290 0.7094 0.0502 0.038 Uiso 1 1 calc R . . C13 C 0.6879(7) 0.8292(7) 0.4301(3) 0.032(2) Uani 1 1 d . . . C14 C 0.6333(8) 0.9103(7) 0.4759(4) 0.043(2) Uani 1 1 d . . . H14A H 0.5482 0.8805 0.4813 0.064 Uiso 1 1 calc R . . H14B H 0.6240 0.9872 0.4615 0.064 Uiso 1 1 calc R . . H14C H 0.6926 0.9152 0.5144 0.064 Uiso 1 1 calc R . . C15 C 0.7130(8) 0.7091(7) 0.4521(3) 0.043(2) Uani 1 1 d . . . H15A H 0.7683 0.7168 0.4917 0.064 Uiso 1 1 calc R . . H15B H 0.7565 0.6624 0.4237 0.064 Uiso 1 1 calc R . . H15C H 0.6302 0.6714 0.4551 0.064 Uiso 1 1 calc R . . C16 C 0.8143(7) 0.8824(8) 0.4164(4) 0.047(3) Uani 1 1 d . . . H16A H 0.7941 0.9504 0.3944 0.071 Uiso 1 1 calc R . . H16B H 0.8562 0.8255 0.3920 0.071 Uiso 1 1 calc R . . H16C H 0.8730 0.9050 0.4541 0.071 Uiso 1 1 calc R . . C17 C 0.0644(8) 1.0055(7) 0.2797(3) 0.033(2) Uani 1 1 d . . . C18 C 0.0710(8) 1.0664(7) 0.3428(3) 0.038(2) Uani 1 1 d . . . H18A H -0.0052 1.1143 0.3439 0.056 Uiso 1 1 calc R . . H18B H 0.1500 1.1152 0.3530 0.056 Uiso 1 1 calc R . . H18C H 0.0724 1.0087 0.3718 0.056 Uiso 1 1 calc R . . C19 C 0.0635(10) 1.0967(7) 0.2351(4) 0.054(3) Uani 1 1 d . . . H19A H 0.0622 1.0587 0.1947 0.081 Uiso 1 1 calc R . . H19B H 0.1415 1.1464 0.2466 0.081 Uiso 1 1 calc R . . H19C H -0.0138 1.1434 0.2355 0.081 Uiso 1 1 calc R . . C20 C -0.0578(7) 0.9299(7) 0.2643(4) 0.043(2) Uani 1 1 d . . . H20A H -0.1339 0.9773 0.2669 0.065 Uiso 1 1 calc R . . H20B H -0.0546 0.8707 0.2927 0.065 Uiso 1 1 calc R . . H20C H -0.0640 0.8927 0.2234 0.065 Uiso 1 1 calc R . . C21 C 0.5602(8) 0.9798(7) 0.1411(4) 0.039(2) Uani 1 1 d . . . C22 C 0.6854(9) 1.0081(9) 0.1221(5) 0.072(3) Uani 1 1 d . . . H22A H 0.6983 0.9540 0.0881 0.108 Uiso 1 1 calc R . . H22B H 0.7567 1.0020 0.1556 0.108 Uiso 1 1 calc R . . H22C H 0.6838 1.0869 0.1099 0.108 Uiso 1 1 calc R . . C23 C 0.4439(9) 0.9908(8) 0.0910(4) 0.060(3) Uani 1 1 d . . . H23A H 0.4373 1.0712 0.0815 0.091 Uiso 1 1 calc R . . H23B H 0.3641 0.9666 0.1045 0.091 Uiso 1 1 calc R . . H23C H 0.4559 0.9416 0.0552 0.091 Uiso 1 1 calc R . . C24 C 0.5417(11) 1.0630(8) 0.1957(5) 0.076(4) Uani 1 1 d . . . H24A H 0.6267 1.0921 0.2171 0.114 Uiso 1 1 calc R . . H24B H 0.4974 1.0219 0.2228 0.114 Uiso 1 1 calc R . . H24C H 0.4894 1.1278 0.1820 0.114 Uiso 1 1 calc R . . C25 C 0.4981(7) 0.3389(6) 0.3643(4) 0.033(2) Uani 1 1 d . . . C26 C 0.5992(8) 0.2616(7) 0.3410(4) 0.048(2) Uani 1 1 d . . . H26A H 0.6820 0.3046 0.3456 0.072 Uiso 1 1 calc R . . H26B H 0.5698 0.2367 0.2985 0.072 Uiso 1 1 calc R . . H26C H 0.6109 0.1939 0.3639 0.072 Uiso 1 1 calc R . . C27 C 0.3726(8) 0.2669(7) 0.3614(4) 0.042(2) Uani 1 1 d . . . H27A H 0.3916 0.1991 0.3837 0.064 Uiso 1 1 calc R . . H27B H 0.3370 0.2421 0.3194 0.064 Uiso 1 1 calc R . . H27C H 0.3091 0.3138 0.3792 0.064 Uiso 1 1 calc R . . C28 C 0.5468(8) 0.3883(7) 0.4286(4) 0.039(2) Uani 1 1 d . . . H28A H 0.5629 0.3252 0.4546 0.058 Uiso 1 1 calc R . . H28B H 0.4812 0.4387 0.4425 0.058 Uiso 1 1 calc R . . H28C H 0.6276 0.4329 0.4302 0.058 Uiso 1 1 calc R . . C29 C -0.0871(7) 0.4950(6) 0.2170(3) 0.0259(19) Uani 1 1 d . . . C30 C -0.1157(8) 0.4165(7) 0.2639(4) 0.039(2) Uani 1 1 d . . . H30A H -0.0928 0.4574 0.3040 0.059 Uiso 1 1 calc R . . H30B H -0.0643 0.3469 0.2615 0.059 Uiso 1 1 calc R . . H30C H -0.2082 0.3949 0.2564 0.059 Uiso 1 1 calc R . . C31 C -0.1195(7) 0.4327(7) 0.1542(4) 0.039(2) Uani 1 1 d . . . H31A H -0.2124 0.4123 0.1452 0.059 Uiso 1 1 calc R . . H31B H -0.0691 0.3624 0.1523 0.059 Uiso 1 1 calc R . . H31C H -0.0977 0.4833 0.1248 0.059 Uiso 1 1 calc R . . C32 C -0.1621(7) 0.6051(7) 0.2219(4) 0.033(2) Uani 1 1 d . . . H32A H -0.1436 0.6548 0.1914 0.050 Uiso 1 1 calc R . . H32B H -0.1358 0.6454 0.2619 0.050 Uiso 1 1 calc R . . H32C H -0.2553 0.5862 0.2154 0.050 Uiso 1 1 calc R . . C33 C 0.3622(9) 0.3816(8) 0.0682(4) 0.048(2) Uani 1 1 d . . . C34 C 0.4732(10) 0.3113(7) 0.0465(4) 0.057(3) Uani 1 1 d . . . H34A H 0.4378 0.2378 0.0255 0.086 Uiso 1 1 calc R . . H34B H 0.5384 0.2966 0.0811 0.086 Uiso 1 1 calc R . . H34C H 0.5135 0.3551 0.0191 0.086 Uiso 1 1 calc R . . C35 C 0.2840(10) 0.3049(9) 0.1014(5) 0.070(3) Uani 1 1 d . . . H35A H 0.2172 0.3505 0.1175 0.104 Uiso 1 1 calc R . . H35B H 0.3421 0.2741 0.1345 0.104 Uiso 1 1 calc R . . H35C H 0.2425 0.2410 0.0736 0.104 Uiso 1 1 calc R . . C36 C 0.2760(10) 0.4296(9) 0.0176(4) 0.069(3) Uani 1 1 d . . . H36A H 0.2313 0.3662 -0.0096 0.104 Uiso 1 1 calc R . . H36B H 0.3282 0.4755 -0.0043 0.104 Uiso 1 1 calc R . . H36C H 0.2117 0.4786 0.0335 0.104 Uiso 1 1 calc R . . O1 O 0.3440(4) 0.6796(4) 0.2591(2) 0.0257(12) Uani 1 1 d . . . O2 O 0.1845(5) 0.8548(4) 0.2149(2) 0.0299(13) Uani 1 1 d . . . O3 O 0.1965(4) 0.8312(4) 0.3235(2) 0.0218(12) Uani 1 1 d . . . O4 O 0.1074(4) 0.6158(4) 0.1858(2) 0.0240(12) Uani 1 1 d . . . O5 O 0.1209(4) 0.5922(4) 0.2958(2) 0.0244(12) Uani 1 1 d . . . O6 O 0.3273(5) 0.9914(4) 0.2929(2) 0.0371(14) Uani 1 1 d . . . O7 O 0.1597(5) 0.4201(4) 0.2243(2) 0.0273(13) Uani 1 1 d . . . O8 O 0.3418(5) 0.5713(4) 0.1462(2) 0.0362(14) Uani 1 1 d . . . O9 O 0.5274(6) 0.4406(6) 0.1728(3) 0.0588(19) Uani 1 1 d . . . O10 O 0.5277(6) 0.5636(6) 0.0877(3) 0.0612(19) Uani 1 1 d . . . O11 O 0.4251(5) 0.8064(5) 0.1771(2) 0.0413(15) Uani 1 1 d . . . O12 O 0.5908(7) 0.7577(6) 0.1104(3) 0.070(2) Uani 1 1 d . . . O13 O 0.6597(5) 0.8275(4) 0.2186(2) 0.0352(14) Uani 1 1 d . . . O14 O 0.4474(5) 0.7660(4) 0.3765(2) 0.0295(13) Uani 1 1 d . . . O15 O 0.6272(5) 0.7355(4) 0.3135(2) 0.0263(12) Uani 1 1 d . . . O16 O 0.5509(5) 0.9366(5) 0.3396(2) 0.0432(15) Uani 1 1 d . . . O17 O 0.3730(5) 0.5335(4) 0.3494(2) 0.0291(13) Uani 1 1 d . . . O18 O 0.4007(5) 0.4100(5) 0.2557(2) 0.0382(15) Uani 1 1 d . . . O19 O 0.5957(5) 0.5168(4) 0.3176(2) 0.0309(13) Uani 1 1 d . . . Cl1 Cl 0.0488(2) 0.67477(18) 0.58679(9) 0.0377(5) Uani 1 1 d . . . Cl2 Cl 0.0079(3) 0.8645(2) -0.08571(10) 0.0668(8) 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 0.0174(3) 0.0253(3) 0.0235(3) -0.0014(2) 0.0020(2) 0.0017(2) Sb2 0.0189(3) 0.0251(3) 0.0255(3) -0.0001(2) 0.0057(2) -0.0036(2) P1 0.0214(12) 0.0263(12) 0.0326(12) 0.0065(10) 0.0065(10) -0.0027(10) P2 0.0259(12) 0.0200(11) 0.0291(12) -0.0021(9) 0.0045(9) -0.0051(9) P3 0.0369(15) 0.0420(15) 0.0474(15) 0.0090(12) 0.0082(12) -0.0073(12) P4 0.0185(11) 0.0260(12) 0.0320(12) -0.0047(10) 0.0020(9) 0.0029(10) P5 0.0186(11) 0.0239(12) 0.0232(11) -0.0009(9) 0.0025(9) -0.0008(9) P6 0.0463(16) 0.0495(16) 0.0502(16) 0.0041(13) 0.0095(13) 0.0000(13) C1 0.008(4) 0.030(5) 0.027(4) -0.006(4) -0.004(3) 0.001(4) C2 0.020(4) 0.016(4) 0.030(5) -0.007(4) -0.004(4) -0.007(3) C3 0.018(4) 0.026(5) 0.034(5) 0.004(4) 0.010(4) -0.004(4) C4 0.011(4) 0.041(5) 0.020(4) 0.000(4) 0.002(3) 0.001(4) C5 0.038(5) 0.017(4) 0.028(5) -0.014(4) 0.000(4) -0.004(4) C6 0.025(5) 0.017(4) 0.032(5) 0.007(4) 0.002(4) 0.004(4) C7 0.027(5) 0.028(5) 0.026(5) -0.002(4) 0.009(4) -0.003(4) C8 0.042(6) 0.041(6) 0.042(6) -0.003(5) 0.008(5) -0.002(5) C9 0.045(6) 0.055(7) 0.050(6) 0.014(5) 0.003(5) 0.011(5) C10 0.056(7) 0.042(6) 0.020(5) 0.012(4) -0.001(4) -0.006(5) C11 0.062(7) 0.045(6) 0.033(6) 0.010(5) 0.014(5) 0.004(5) C12 0.021(5) 0.027(5) 0.043(5) 0.002(4) -0.001(4) -0.001(4) C13 0.017(4) 0.039(5) 0.039(5) -0.001(4) 0.005(4) -0.005(4) C14 0.034(5) 0.046(6) 0.041(5) -0.008(4) -0.007(4) -0.001(4) C15 0.044(6) 0.044(6) 0.031(5) -0.001(4) -0.019(4) 0.010(5) C16 0.018(5) 0.061(7) 0.060(6) -0.008(5) 0.005(4) -0.018(5) C17 0.034(5) 0.029(5) 0.033(5) -0.002(4) 0.004(4) -0.004(4) C18 0.030(5) 0.036(5) 0.043(5) -0.012(4) 0.003(4) 0.004(4) C19 0.085(8) 0.029(5) 0.047(6) 0.009(5) 0.004(5) 0.007(5) C20 0.028(5) 0.027(5) 0.066(6) -0.013(4) -0.009(5) -0.005(4) C21 0.038(5) 0.044(6) 0.039(5) 0.024(5) 0.007(4) -0.010(4) C22 0.056(7) 0.086(9) 0.083(8) 0.042(7) 0.016(6) -0.001(6) C23 0.055(7) 0.061(7) 0.066(7) 0.033(6) -0.001(6) -0.009(6) C24 0.102(10) 0.039(6) 0.077(8) 0.001(6) -0.013(7) -0.009(6) C25 0.024(5) 0.022(5) 0.055(6) 0.009(4) 0.008(4) 0.006(4) C26 0.045(6) 0.034(5) 0.069(7) 0.006(5) 0.020(5) 0.013(5) C27 0.033(5) 0.035(5) 0.056(6) -0.005(5) 0.005(4) -0.001(4) C28 0.029(5) 0.036(5) 0.050(6) 0.008(4) 0.001(4) 0.006(4) C29 0.017(4) 0.030(5) 0.034(5) 0.008(4) 0.010(4) 0.006(4) C30 0.034(5) 0.033(5) 0.059(6) 0.017(5) 0.022(4) 0.001(4) C31 0.017(5) 0.046(6) 0.050(6) -0.020(5) 0.003(4) -0.010(4) C32 0.014(4) 0.036(5) 0.049(5) 0.006(4) 0.003(4) -0.003(4) C33 0.051(6) 0.040(6) 0.054(6) -0.003(5) 0.014(5) -0.007(5) C34 0.094(8) 0.036(6) 0.047(6) 0.007(5) 0.029(6) -0.016(6) C35 0.073(8) 0.063(7) 0.074(8) -0.003(6) 0.021(6) -0.007(6) C36 0.076(8) 0.072(8) 0.056(7) -0.015(6) 0.008(6) 0.004(7) O1 0.019(3) 0.036(3) 0.020(3) -0.003(2) 0.000(2) 0.004(2) O2 0.038(3) 0.030(3) 0.023(3) -0.003(2) 0.009(2) 0.007(3) O3 0.023(3) 0.020(3) 0.025(3) 0.003(2) 0.010(2) 0.000(2) O4 0.017(3) 0.031(3) 0.023(3) 0.002(2) 0.001(2) -0.001(2) O5 0.019(3) 0.026(3) 0.027(3) 0.000(2) 0.003(2) -0.006(2) O6 0.036(3) 0.030(3) 0.045(3) -0.007(3) 0.012(3) -0.017(3) O7 0.028(3) 0.021(3) 0.031(3) -0.004(2) 0.006(2) -0.001(2) O8 0.037(3) 0.039(3) 0.037(3) -0.001(3) 0.019(3) 0.020(3) O9 0.046(4) 0.075(5) 0.052(4) 0.018(4) -0.007(3) 0.006(4) O10 0.062(5) 0.062(5) 0.065(4) 0.013(4) 0.024(4) -0.015(4) O11 0.024(3) 0.055(4) 0.045(4) -0.002(3) 0.011(3) -0.018(3) O12 0.086(5) 0.071(5) 0.050(4) -0.021(4) 0.020(4) -0.001(4) O13 0.026(3) 0.041(4) 0.039(3) 0.009(3) 0.003(3) -0.003(3) O14 0.018(3) 0.040(3) 0.028(3) -0.005(3) -0.001(2) -0.002(3) O15 0.022(3) 0.029(3) 0.027(3) 0.002(2) 0.003(2) -0.009(2) O16 0.049(4) 0.034(3) 0.050(4) 0.012(3) 0.017(3) -0.002(3) O17 0.034(3) 0.030(3) 0.022(3) 0.001(2) 0.000(2) 0.004(3) O18 0.024(3) 0.049(4) 0.039(3) -0.014(3) 0.006(3) 0.009(3) O19 0.020(3) 0.036(3) 0.036(3) -0.001(3) 0.004(2) 0.004(3) Cl1 0.0441(14) 0.0416(13) 0.0296(11) -0.0050(10) 0.0166(10) -0.0034(11) Cl2 0.095(2) 0.0653(18) 0.0382(14) 0.0145(13) -0.0007(14) 0.0119(16) _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 1.944(5) . ? Sb1 O3 1.991(5) . ? Sb1 O14 1.993(5) . ? Sb1 O17 1.998(5) . ? Sb1 O5 2.034(5) . ? Sb1 C1 2.095(7) . ? Sb2 O1 1.931(4) . ? Sb2 O11 1.982(5) . ? Sb2 O8 1.992(5) . ? Sb2 O2 2.023(5) . ? Sb2 O4 2.032(5) . ? Sb2 C7 2.108(7) . ? P1 O15 1.508(5) . ? P1 O16 1.543(6) . ? P1 O14 1.559(5) . ? P1 C13 1.815(8) . ? P2 O6 1.495(5) . ? P2 O3 1.535(5) . ? P2 O2 1.537(5) . ? P2 C17 1.786(8) . ? P3 O13 1.506(5) . ? P3 O11 1.513(5) . ? P3 O12 1.532(6) . ? P3 C21 1.802(8) . ? P4 O18 1.493(5) . ? P4 O17 1.549(5) . ? P4 O19 1.552(5) . ? P4 C25 1.788(8) . ? P5 O4 1.517(5) . ? P5 O5 1.540(5) . ? P5 O7 1.552(5) . ? P5 C29 1.817(7) . ? P6 O10 1.515(6) . ? P6 O8 1.535(5) . ? P6 O9 1.550(6) . ? P6 C33 1.797(9) . ? C1 C6 1.361(9) . ? C1 C2 1.397(10) . ? C2 C3 1.383(10) . ? C2 H2 0.9500 . ? C3 C4 1.373(10) . ? C3 H3 0.9500 . ? C4 C5 1.383(10) . ? C4 Cl1 1.739(7) . ? C5 C6 1.387(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.358(10) . ? C7 C12 1.393(10) . ? C8 C9 1.391(11) . ? C8 H8 0.9500 . ? C9 C10 1.364(12) . ? C9 H9 0.9500 . ? C10 C11 1.327(12) . ? C10 Cl2 1.752(8) . ? C11 C12 1.350(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.528(11) . ? C13 C15 1.537(10) . ? C13 C16 1.541(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.517(10) . ? C17 C19 1.527(11) . ? C17 C18 1.532(10) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 1.487(11) . ? C21 C23 1.535(11) . ? C21 C24 1.545(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C28 1.524(11) . ? C25 C26 1.526(11) . ? C25 C27 1.537(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C32 1.516(10) . ? C29 C31 1.524(10) . ? C29 C30 1.525(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.490(12) . ? C33 C35 1.530(12) . ? C33 C34 1.549(12) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 O1 Sb1 O3 91.81(19) . . ? O1 Sb1 O14 90.6(2) . . ? O3 Sb1 O14 90.9(2) . . ? O1 Sb1 O17 88.8(2) . . ? O3 Sb1 O17 179.39(18) . . ? O14 Sb1 O17 88.9(2) . . ? O1 Sb1 O5 89.92(19) . . ? O3 Sb1 O5 91.00(19) . . ? O14 Sb1 O5 178.0(2) . . ? O17 Sb1 O5 89.20(19) . . ? O1 Sb1 C1 178.2(2) . . ? O3 Sb1 C1 88.7(2) . . ? O14 Sb1 C1 91.1(2) . . ? O17 Sb1 C1 90.7(2) . . ? O5 Sb1 C1 88.3(2) . . ? O1 Sb2 O11 87.5(2) . . ? O1 Sb2 O8 89.0(2) . . ? O11 Sb2 O8 91.9(2) . . ? O1 Sb2 O2 90.01(19) . . ? O11 Sb2 O2 90.1(2) . . ? O8 Sb2 O2 177.7(2) . . ? O1 Sb2 O4 89.61(19) . . ? O11 Sb2 O4 177.1(2) . . ? O8 Sb2 O4 87.6(2) . . ? O2 Sb2 O4 90.4(2) . . ? O1 Sb2 C7 178.7(3) . . ? O11 Sb2 C7 92.8(3) . . ? O8 Sb2 C7 92.3(3) . . ? O2 Sb2 C7 88.7(2) . . ? O4 Sb2 C7 90.1(2) . . ? O15 P1 O16 112.5(3) . . ? O15 P1 O14 112.8(3) . . ? O16 P1 O14 108.7(3) . . ? O15 P1 C13 110.9(3) . . ? O16 P1 C13 107.2(3) . . ? O14 P1 C13 104.3(3) . . ? O6 P2 O3 111.9(3) . . ? O6 P2 O2 114.0(3) . . ? O3 P2 O2 107.9(3) . . ? O6 P2 C17 111.8(3) . . ? O3 P2 C17 105.1(3) . . ? O2 P2 C17 105.6(3) . . ? O13 P3 O11 110.3(3) . . ? O13 P3 O12 110.8(4) . . ? O11 P3 O12 111.8(4) . . ? O13 P3 C21 109.2(4) . . ? O11 P3 C21 109.3(4) . . ? O12 P3 C21 105.3(4) . . ? O18 P4 O17 111.9(3) . . ? O18 P4 O19 111.8(3) . . ? O17 P4 O19 110.9(3) . . ? O18 P4 C25 110.9(4) . . ? O17 P4 C25 104.9(3) . . ? O19 P4 C25 106.1(3) . . ? O4 P5 O5 110.8(3) . . ? O4 P5 O7 111.9(3) . . ? O5 P5 O7 110.9(3) . . ? O4 P5 C29 106.8(3) . . ? O5 P5 C29 109.1(3) . . ? O7 P5 C29 107.2(3) . . ? O10 P6 O8 111.9(4) . . ? O10 P6 O9 109.4(4) . . ? O8 P6 O9 108.6(3) . . ? O10 P6 C33 107.6(4) . . ? O8 P6 C33 110.5(4) . . ? O9 P6 C33 108.7(4) . . ? C6 C1 C2 119.8(7) . . ? C6 C1 Sb1 120.8(6) . . ? C2 C1 Sb1 119.4(5) . . ? C3 C2 C1 120.4(7) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 118.2(7) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 122.2(7) . . ? C3 C4 Cl1 118.8(6) . . ? C5 C4 Cl1 118.9(6) . . ? C4 C5 C6 118.3(7) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? C1 C6 C5 120.9(7) . . ? C1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C12 119.5(7) . . ? C8 C7 Sb2 119.6(6) . . ? C12 C7 Sb2 120.7(6) . . ? C7 C8 C9 119.6(8) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 118.4(9) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C11 C10 C9 122.6(8) . . ? C11 C10 Cl2 119.0(7) . . ? C9 C10 Cl2 118.4(8) . . ? C10 C11 C12 119.6(8) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C7 120.2(8) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 C15 111.9(7) . . ? C14 C13 C16 109.6(7) . . ? C15 C13 C16 110.1(7) . . ? C14 C13 P1 109.8(5) . . ? C15 C13 P1 108.9(5) . . ? C16 C13 P1 106.3(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C19 110.6(7) . . ? C20 C17 C18 109.2(7) . . ? C19 C17 C18 108.7(7) . . ? C20 C17 P2 110.2(5) . . ? C19 C17 P2 109.0(6) . . ? C18 C17 P2 109.2(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 112.1(7) . . ? C22 C21 C24 109.4(8) . . ? C23 C21 C24 108.2(8) . . ? C22 C21 P3 111.2(7) . . ? C23 C21 P3 108.3(6) . . ? C24 C21 P3 107.5(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C26 110.7(7) . . ? C28 C25 C27 109.9(7) . . ? C26 C25 C27 108.6(7) . . ? C28 C25 P4 109.3(5) . . ? C26 C25 P4 109.7(6) . . ? C27 C25 P4 108.5(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C29 C31 111.3(6) . . ? C32 C29 C30 110.0(6) . . ? C31 C29 C30 110.5(7) . . ? C32 C29 P5 108.0(5) . . ? C31 C29 P5 108.3(5) . . ? C30 C29 P5 108.7(5) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C35 110.6(9) . . ? C36 C33 C34 112.0(8) . . ? C35 C33 C34 109.2(8) . . ? C36 C33 P6 110.9(7) . . ? C35 C33 P6 108.8(7) . . ? C34 C33 P6 105.2(6) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Sb2 O1 Sb1 134.5(3) . . ? P2 O2 Sb2 133.3(3) . . ? P2 O3 Sb1 131.9(3) . . ? P5 O4 Sb2 130.8(3) . . ? P5 O5 Sb1 130.0(3) . . ? P6 O8 Sb2 158.0(4) . . ? P3 O11 Sb2 158.8(4) . . ? P1 O14 Sb1 138.6(3) . . ? P4 O17 Sb1 136.9(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 O1 Sb1 C1 C6 -140(7) . . . . ? O3 Sb1 C1 C6 -32.8(6) . . . . ? O14 Sb1 C1 C6 58.1(6) . . . . ? O17 Sb1 C1 C6 147.0(6) . . . . ? O5 Sb1 C1 C6 -123.8(6) . . . . ? O1 Sb1 C1 C2 40(8) . . . . ? O3 Sb1 C1 C2 147.2(5) . . . . ? O14 Sb1 C1 C2 -121.9(5) . . . . ? O17 Sb1 C1 C2 -33.0(5) . . . . ? O5 Sb1 C1 C2 56.2(5) . . . . ? C6 C1 C2 C3 2.2(10) . . . . ? Sb1 C1 C2 C3 -177.7(5) . . . . ? C1 C2 C3 C4 1.2(10) . . . . ? C2 C3 C4 C5 -4.2(11) . . . . ? C2 C3 C4 Cl1 177.9(5) . . . . ? C3 C4 C5 C6 3.7(11) . . . . ? Cl1 C4 C5 C6 -178.4(5) . . . . ? C2 C1 C6 C5 -2.7(11) . . . . ? Sb1 C1 C6 C5 177.2(5) . . . . ? C4 C5 C6 C1 -0.1(11) . . . . ? O1 Sb2 C7 C8 -22(12) . . . . ? O11 Sb2 C7 C8 -125.0(6) . . . . ? O8 Sb2 C7 C8 143.0(6) . . . . ? O2 Sb2 C7 C8 -34.9(6) . . . . ? O4 Sb2 C7 C8 55.5(6) . . . . ? O1 Sb2 C7 C12 154(11) . . . . ? O11 Sb2 C7 C12 50.6(6) . . . . ? O8 Sb2 C7 C12 -41.4(6) . . . . ? O2 Sb2 C7 C12 140.6(6) . . . . ? O4 Sb2 C7 C12 -129.0(6) . . . . ? C12 C7 C8 C9 0.5(12) . . . . ? Sb2 C7 C8 C9 176.1(6) . . . . ? C7 C8 C9 C10 -0.5(13) . . . . ? C8 C9 C10 C11 2.8(14) . . . . ? C8 C9 C10 Cl2 -177.8(7) . . . . ? C9 C10 C11 C12 -4.9(14) . . . . ? Cl2 C10 C11 C12 175.7(6) . . . . ? C10 C11 C12 C7 4.7(13) . . . . ? C8 C7 C12 C11 -2.5(12) . . . . ? Sb2 C7 C12 C11 -178.1(6) . . . . ? O15 P1 C13 C14 179.5(5) . . . . ? O16 P1 C13 C14 56.3(6) . . . . ? O14 P1 C13 C14 -58.9(6) . . . . ? O15 P1 C13 C15 -57.7(6) . . . . ? O16 P1 C13 C15 179.2(5) . . . . ? O14 P1 C13 C15 64.0(6) . . . . ? O15 P1 C13 C16 60.9(6) . . . . ? O16 P1 C13 C16 -62.2(6) . . . . ? O14 P1 C13 C16 -177.4(5) . . . . ? O6 P2 C17 C20 -179.9(5) . . . . ? O3 P2 C17 C20 -58.2(6) . . . . ? O2 P2 C17 C20 55.6(6) . . . . ? O6 P2 C17 C19 58.6(6) . . . . ? O3 P2 C17 C19 -179.7(5) . . . . ? O2 P2 C17 C19 -65.9(6) . . . . ? O6 P2 C17 C18 -60.0(6) . . . . ? O3 P2 C17 C18 61.6(6) . . . . ? O2 P2 C17 C18 175.5(5) . . . . ? O13 P3 C21 C22 64.5(7) . . . . ? O11 P3 C21 C22 -174.8(6) . . . . ? O12 P3 C21 C22 -54.5(8) . . . . ? O13 P3 C21 C23 -171.9(6) . . . . ? O11 P3 C21 C23 -51.2(7) . . . . ? O12 P3 C21 C23 69.0(7) . . . . ? O13 P3 C21 C24 -55.3(7) . . . . ? O11 P3 C21 C24 65.5(7) . . . . ? O12 P3 C21 C24 -174.3(6) . . . . ? O18 P4 C25 C28 -173.1(5) . . . . ? O17 P4 C25 C28 -52.2(6) . . . . ? O19 P4 C25 C28 65.2(6) . . . . ? O18 P4 C25 C26 65.3(6) . . . . ? O17 P4 C25 C26 -173.8(5) . . . . ? O19 P4 C25 C26 -56.4(6) . . . . ? O18 P4 C25 C27 -53.2(6) . . . . ? O17 P4 C25 C27 67.7(6) . . . . ? O19 P4 C25 C27 -174.9(5) . . . . ? O4 P5 C29 C32 -58.1(6) . . . . ? O5 P5 C29 C32 61.7(6) . . . . ? O7 P5 C29 C32 -178.2(5) . . . . ? O4 P5 C29 C31 62.5(6) . . . . ? O5 P5 C29 C31 -177.7(5) . . . . ? O7 P5 C29 C31 -57.6(6) . . . . ? O4 P5 C29 C30 -177.3(5) . . . . ? O5 P5 C29 C30 -57.6(6) . . . . ? O7 P5 C29 C30 62.6(6) . . . . ? O10 P6 C33 C36 -63.0(8) . . . . ? O8 P6 C33 C36 59.4(8) . . . . ? O9 P6 C33 C36 178.6(7) . . . . ? O10 P6 C33 C35 175.2(7) . . . . ? O8 P6 C33 C35 -62.3(8) . . . . ? O9 P6 C33 C35 56.8(8) . . . . ? O10 P6 C33 C34 58.2(7) . . . . ? O8 P6 C33 C34 -179.3(5) . . . . ? O9 P6 C33 C34 -60.2(7) . . . . ? O11 Sb2 O1 Sb1 132.4(4) . . . . ? O8 Sb2 O1 Sb1 -135.7(4) . . . . ? O2 Sb2 O1 Sb1 42.2(4) . . . . ? O4 Sb2 O1 Sb1 -48.1(4) . . . . ? C7 Sb2 O1 Sb1 29(11) . . . . ? O3 Sb1 O1 Sb2 -42.2(4) . . . . ? O14 Sb1 O1 Sb2 -133.2(4) . . . . ? O17 Sb1 O1 Sb2 138.0(4) . . . . ? O5 Sb1 O1 Sb2 48.8(4) . . . . ? C1 Sb1 O1 Sb2 65(8) . . . . ? O6 P2 O2 Sb2 74.4(5) . . . . ? O3 P2 O2 Sb2 -50.5(5) . . . . ? C17 P2 O2 Sb2 -162.4(4) . . . . ? O1 Sb2 O2 P2 12.0(4) . . . . ? O11 Sb2 O2 P2 -75.5(4) . . . . ? O8 Sb2 O2 P2 76(5) . . . . ? O4 Sb2 O2 P2 101.6(4) . . . . ? C7 Sb2 O2 P2 -168.3(5) . . . . ? O6 P2 O3 Sb1 -75.5(4) . . . . ? O2 P2 O3 Sb1 50.6(4) . . . . ? C17 P2 O3 Sb1 162.9(4) . . . . ? O1 Sb1 O3 P2 -13.1(4) . . . . ? O14 Sb1 O3 P2 77.6(4) . . . . ? O17 Sb1 O3 P2 148(18) . . . . ? O5 Sb1 O3 P2 -103.0(4) . . . . ? C1 Sb1 O3 P2 168.7(4) . . . . ? O5 P5 O4 Sb2 51.6(5) . . . . ? O7 P5 O4 Sb2 -72.6(4) . . . . ? C29 P5 O4 Sb2 170.4(4) . . . . ? O1 Sb2 O4 P5 -10.7(4) . . . . ? O11 Sb2 O4 P5 -1(4) . . . . ? O8 Sb2 O4 P5 78.3(4) . . . . ? O2 Sb2 O4 P5 -100.7(4) . . . . ? C7 Sb2 O4 P5 170.5(4) . . . . ? O4 P5 O5 Sb1 -49.9(4) . . . . ? O7 P5 O5 Sb1 74.9(4) . . . . ? C29 P5 O5 Sb1 -167.2(4) . . . . ? O1 Sb1 O5 P5 8.7(4) . . . . ? O3 Sb1 O5 P5 100.5(4) . . . . ? O14 Sb1 O5 P5 -96(6) . . . . ? O17 Sb1 O5 P5 -80.1(4) . . . . ? C1 Sb1 O5 P5 -170.8(4) . . . . ? O10 P6 O8 Sb2 -27.6(10) . . . . ? O9 P6 O8 Sb2 93.3(9) . . . . ? C33 P6 O8 Sb2 -147.5(9) . . . . ? O1 Sb2 O8 P6 -89.9(9) . . . . ? O11 Sb2 O8 P6 -2.4(9) . . . . ? O2 Sb2 O8 P6 -154(5) . . . . ? O4 Sb2 O8 P6 -179.6(9) . . . . ? C7 Sb2 O8 P6 90.4(9) . . . . ? O13 P3 O11 Sb2 -99.7(10) . . . . ? O12 P3 O11 Sb2 24.0(11) . . . . ? C21 P3 O11 Sb2 140.3(10) . . . . ? O1 Sb2 O11 P3 95.5(10) . . . . ? O8 Sb2 O11 P3 6.6(10) . . . . ? O2 Sb2 O11 P3 -174.5(10) . . . . ? O4 Sb2 O11 P3 86(4) . . . . ? C7 Sb2 O11 P3 -85.7(10) . . . . ? O15 P1 O14 Sb1 -39.5(6) . . . . ? O16 P1 O14 Sb1 85.9(5) . . . . ? C13 P1 O14 Sb1 -159.9(5) . . . . ? O1 Sb1 O14 P1 0.3(5) . . . . ? O3 Sb1 O14 P1 -91.5(5) . . . . ? O17 Sb1 O14 P1 89.0(5) . . . . ? O5 Sb1 O14 P1 105(6) . . . . ? C1 Sb1 O14 P1 179.7(5) . . . . ? O18 P4 O17 Sb1 -61.3(5) . . . . ? O19 P4 O17 Sb1 64.3(5) . . . . ? C25 P4 O17 Sb1 178.4(4) . . . . ? O1 Sb1 O17 P4 6.3(4) . . . . ? O3 Sb1 O17 P4 -155(18) . . . . ? O14 Sb1 O17 P4 -84.3(4) . . . . ? O5 Sb1 O17 P4 96.2(4) . . . . ? C1 Sb1 O17 P4 -175.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.447 _refine_diff_density_min -1.130 _refine_diff_density_rms 0.148 # Attachment '6.cif' data_mono1013 _database_code_depnum_ccdc_archive 'CCDC 700899' _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