Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global #============================================================================== # SUBMISSION DETAILS # ================== _journal_coden_Cambridge 222 _publ_contact_author_name 'Professor W. Levason' _publ_contact_author_address ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email wxl@soton.ac.uk _publ_contact_author_fax '023 8059 6805' _publ_contact_author_phone '023 8059 3792' _publ_requested_journal 'Dalton Trans.' _publ_requested_category ? #============================================================================== # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Synthesis and characterisation of transition metal halide complexes of the xylyl-distibine, 1,2-bis(dimethylstibanylmethyl)benzene ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # Note order: Family_name, first name(s) or initials (or mixture). loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Levason, William' ? ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Matthews, Melissa L.' ? ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Reid, Gillian' ? ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Webster, Michael' ? ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; #============================================================================== # TEXT OF TYPE _PUBL_SECTION_* # ============================ _publ_section_references ; Blessing, R. H. (1997). J. Appl. Cryst. 30, 421-426. Hooft, R. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter & R. M. Sweet, pp. 307-326. London: Academic Press. Sheldrick, G. M. (1997). SHELXL97. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXS97. University of Gottingen, Germany. ; data_cusb4 _database_code_depnum_ccdc_archive 'CCDC 228294' _audit_creation_method 'SHELXL-97 + hand edit' _chemical_name_systematic ; Bis(1,2-bis(dimethylstibanylmethyl)benzene)copper(I) tetrafluoroborate ethanol solvate, dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 Cu Sb4 1+, B F4 1-, 0.80(C4 H10 O), 0.20(C H2 Cl2)' _chemical_formula_sum 'C27.40 H48.40 B Cl0.40 Cu F4 O0.80 Sb4' _chemical_formula_weight 1042.19 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6315(10) _cell_length_b 18.5261(10) _cell_length_c 14.2015(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.830(3) _cell_angle_gamma 90.00 _cell_volume 3684.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 23887 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 3.530 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.44301 # shelxl 0.4173 _exptl_absorpt_correction_T_max 0.50599 # 0.5387 _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30492 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8391 _reflns_number_gt 7610 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+9.1500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8391 _refine_ls_number_parameters 333 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.070 _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 Cu1 Cu 0.29545(3) 0.40665(2) 0.27239(3) 0.01814(9) Uani 1 1 d . . . Sb1 Sb 0.306184(15) 0.459802(13) 0.437212(17) 0.01992(6) Uani 1 1 d . . . Sb2 Sb 0.124851(16) 0.364911(12) 0.211831(18) 0.02165(6) Uani 1 1 d . . . Sb3 Sb 0.331742(16) 0.485214(13) 0.143634(17) 0.02194(7) Uani 1 1 d . . . Sb4 Sb 0.398864(16) 0.296827(12) 0.278460(17) 0.02167(7) Uani 1 1 d . . . B1 B 0.2220(4) 0.2904(3) -0.0358(4) 0.0382(11) Uani 1 1 d . . . F1 F 0.1337(3) 0.2612(3) -0.0475(3) 0.0916(14) Uani 1 1 d . . . F2 F 0.2817(3) 0.23691(19) -0.0485(3) 0.0743(10) Uani 1 1 d . . . F3 F 0.2147(4) 0.34448(19) -0.1039(3) 0.0891(14) Uani 1 1 d . . . F4 F 0.25350(19) 0.32016(16) 0.05718(19) 0.0457(6) Uani 1 1 d . . . C1 C 0.4157(3) 0.4306(3) 0.5660(3) 0.0413(11) Uani 1 1 d . . . H1A H 0.4768 0.4506 0.5627 0.062 Uiso 1 1 calc R . . H1B H 0.4204 0.3779 0.5708 0.062 Uiso 1 1 calc R . . H1C H 0.4006 0.4499 0.6240 0.062 Uiso 1 1 calc R . . C2 C 0.3131(3) 0.5737(2) 0.4577(4) 0.0383(10) Uani 1 1 d . . . H2A H 0.3297 0.5846 0.5282 0.057 Uiso 1 1 calc R . . H2B H 0.2509 0.5950 0.4241 0.057 Uiso 1 1 calc R . . H2C H 0.3619 0.5938 0.4303 0.057 Uiso 1 1 calc R . . C3 C 0.1826(2) 0.4381(2) 0.4878(3) 0.0250(7) Uani 1 1 d . . . H3A H 0.1682 0.3858 0.4822 0.030 Uiso 1 1 calc R . . H3B H 0.1968 0.4518 0.5579 0.030 Uiso 1 1 calc R . . C4 C 0.0970(3) 0.4795(2) 0.4284(3) 0.0248(7) Uani 1 1 d . . . C5 C 0.0821(3) 0.5490(2) 0.4596(3) 0.0277(8) Uani 1 1 d . . . H5 H 0.1253 0.5679 0.5178 0.033 Uiso 1 1 calc R . . C6 C 0.0063(3) 0.5908(2) 0.4077(3) 0.0330(9) Uani 1 1 d . . . H6 H -0.0023 0.6379 0.4304 0.040 Uiso 1 1 calc R . . C7 C -0.0569(3) 0.5646(2) 0.3233(3) 0.0336(9) Uani 1 1 d . . . H7 H -0.1083 0.5938 0.2867 0.040 Uiso 1 1 calc R . . C8 C -0.0453(3) 0.4952(2) 0.2917(3) 0.0311(8) Uani 1 1 d . . . H8 H -0.0895 0.4771 0.2336 0.037 Uiso 1 1 calc R . . C9 C 0.0303(2) 0.4516(2) 0.3437(3) 0.0250(7) Uani 1 1 d . . . C10 C 0.0365(3) 0.3755(2) 0.3089(3) 0.0265(8) Uani 1 1 d . . . H10A H -0.0287 0.3584 0.2743 0.032 Uiso 1 1 calc R . . H10B H 0.0623 0.3440 0.3669 0.032 Uiso 1 1 calc R . . C11 C 0.0315(3) 0.4122(3) 0.0840(3) 0.0394(10) Uani 1 1 d . . . H11A H 0.0380 0.4648 0.0880 0.059 Uiso 1 1 calc R . . H11B H -0.0345 0.3987 0.0791 0.059 Uiso 1 1 calc R . . H11C H 0.0478 0.3948 0.0257 0.059 Uiso 1 1 calc R . . C12 C 0.0916(3) 0.2550(2) 0.1779(4) 0.0380(10) Uani 1 1 d . . . H12A H 0.1300 0.2246 0.2313 0.057 Uiso 1 1 calc R . . H12B H 0.1059 0.2426 0.1165 0.057 Uiso 1 1 calc R . . H12C H 0.0237 0.2468 0.1701 0.057 Uiso 1 1 calc R . . C13 C 0.2290(3) 0.5096(2) 0.0074(3) 0.0340(9) Uani 1 1 d . . . H13A H 0.1929 0.4659 -0.0191 0.051 Uiso 1 1 calc R . . H13B H 0.2615 0.5275 -0.0393 0.051 Uiso 1 1 calc R . . H13C H 0.1851 0.5466 0.0178 0.051 Uiso 1 1 calc R . . C14 C 0.3922(3) 0.5907(2) 0.1751(3) 0.0382(10) Uani 1 1 d . . . H14A H 0.4431 0.5898 0.2376 0.057 Uiso 1 1 calc R . . H14B H 0.3425 0.6248 0.1797 0.057 Uiso 1 1 calc R . . H14C H 0.4187 0.6059 0.1222 0.057 Uiso 1 1 calc R . . C15 C 0.4373(3) 0.4404(2) 0.0804(3) 0.0307(8) Uani 1 1 d . . . H15A H 0.4120 0.3947 0.0466 0.037 Uiso 1 1 calc R . . H15B H 0.4463 0.4743 0.0299 0.037 Uiso 1 1 calc R . . C16 C 0.5323(3) 0.4256(2) 0.1523(3) 0.0286(8) Uani 1 1 d . . . C17 C 0.6011(3) 0.4809(2) 0.1746(3) 0.0319(9) Uani 1 1 d . . . H17 H 0.5843 0.5273 0.1464 0.038 Uiso 1 1 calc R . . C18 C 0.6919(3) 0.4700(3) 0.2361(3) 0.0365(10) Uani 1 1 d . . . H18 H 0.7370 0.5083 0.2496 0.044 Uiso 1 1 calc R . . C19 C 0.7167(3) 0.4028(3) 0.2777(3) 0.0391(10) Uani 1 1 d . . . H19 H 0.7795 0.3943 0.3192 0.047 Uiso 1 1 calc R . . C20 C 0.6500(3) 0.3479(3) 0.2589(3) 0.0338(9) Uani 1 1 d . . . H20 H 0.6677 0.3022 0.2889 0.041 Uiso 1 1 calc R . . C21 C 0.5571(3) 0.3577(2) 0.1969(3) 0.0285(8) Uani 1 1 d . . . C22 C 0.4884(3) 0.2959(2) 0.1807(3) 0.0300(8) Uani 1 1 d . . . H22A H 0.5249 0.2501 0.1900 0.036 Uiso 1 1 calc R . . H22B H 0.4471 0.2972 0.1118 0.036 Uiso 1 1 calc R . . C23 C 0.5057(3) 0.2697(2) 0.4110(3) 0.0355(9) Uani 1 1 d . . . H23A H 0.4754 0.2592 0.4626 0.053 Uiso 1 1 calc R . . H23B H 0.5500 0.3102 0.4314 0.053 Uiso 1 1 calc R . . H23C H 0.5408 0.2270 0.3999 0.053 Uiso 1 1 calc R . . C24 C 0.3398(3) 0.1922(2) 0.2398(4) 0.0363(9) Uani 1 1 d . . . H24A H 0.3916 0.1569 0.2490 0.054 Uiso 1 1 calc R . . H24B H 0.3011 0.1921 0.1708 0.054 Uiso 1 1 calc R . . H24C H 0.2997 0.1794 0.2818 0.054 Uiso 1 1 calc R . . O1 O 0.1756(4) 0.6895(3) 0.0668(4) 0.0599(13) Uiso 0.796(4) 1 d PD . . C25 C 0.2332(6) 0.7148(4) -0.0736(6) 0.067(2) Uiso 0.796(4) 1 d PD . . H25A H 0.2398 0.7533 -0.1184 0.100 Uiso 0.796(4) 1 calc PR . . H25B H 0.1934 0.6760 -0.1114 0.100 Uiso 0.796(4) 1 calc PR . . H25C H 0.2964 0.6956 -0.0390 0.100 Uiso 0.796(4) 1 calc PR . . C26 C 0.1863(6) 0.7449(4) 0.0011(5) 0.0618(19) Uiso 0.796(4) 1 d PD . . H26A H 0.2262 0.7843 0.0390 0.074 Uiso 0.796(4) 1 calc PR . . H26B H 0.1229 0.7652 -0.0337 0.074 Uiso 0.796(4) 1 calc PR . . C27 C 0.1226(7) 0.7083(4) 0.1351(6) 0.077(2) Uiso 0.796(4) 1 d PD . . H27A H 0.0570 0.7239 0.0995 0.092 Uiso 0.796(4) 1 calc PR . . H27B H 0.1549 0.7474 0.1799 0.092 Uiso 0.796(4) 1 calc PR . . C28 C 0.1213(3) 0.6399(3) 0.1906(4) 0.096(3) Uiso 0.796(4) 1 d PD . . H28A H 0.0853 0.6475 0.2381 0.144 Uiso 0.796(4) 1 calc PR . . H28B H 0.1870 0.6258 0.2255 0.144 Uiso 0.796(4) 1 calc PR . . H28C H 0.0910 0.6016 0.1445 0.144 Uiso 0.796(4) 1 calc PR . . Cl1 Cl 0.1344(3) 0.5946(3) 0.2078(4) 0.062(2) Uiso 0.204(4) 1 d PR . . Cl2 Cl 0.1249(3) 0.7323(3) 0.0979(4) 0.062(2) Uiso 0.204(4) 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01668(19) 0.01816(19) 0.0197(2) 0.00025(15) 0.00542(16) 0.00029(15) Sb1 0.01563(11) 0.02413(12) 0.01996(12) -0.00173(9) 0.00508(9) 0.00128(8) Sb2 0.01679(12) 0.02054(12) 0.02567(13) -0.00063(9) 0.00308(9) -0.00225(8) Sb3 0.01793(12) 0.02427(13) 0.02225(12) 0.00550(9) 0.00363(9) -0.00211(9) Sb4 0.02104(12) 0.01914(12) 0.02507(13) -0.00117(9) 0.00706(10) 0.00327(9) B1 0.041(3) 0.040(3) 0.031(2) -0.010(2) 0.006(2) 0.004(2) F1 0.051(2) 0.118(3) 0.099(3) -0.062(3) 0.011(2) -0.029(2) F2 0.093(3) 0.062(2) 0.082(3) -0.0013(18) 0.048(2) 0.0267(19) F3 0.169(4) 0.056(2) 0.0447(19) 0.0031(16) 0.035(2) 0.027(2) F4 0.0440(15) 0.0560(17) 0.0330(13) -0.0124(12) 0.0050(11) -0.0114(13) C1 0.0234(19) 0.072(3) 0.027(2) 0.008(2) 0.0049(16) 0.007(2) C2 0.039(2) 0.029(2) 0.054(3) -0.0095(19) 0.023(2) -0.0072(18) C3 0.0191(16) 0.0294(19) 0.0276(19) 0.0011(15) 0.0086(14) 0.0002(14) C4 0.0187(17) 0.0270(18) 0.0311(19) 0.0038(15) 0.0112(15) 0.0002(14) C5 0.0244(18) 0.0284(19) 0.032(2) -0.0028(16) 0.0102(16) -0.0009(15) C6 0.0264(19) 0.0262(19) 0.050(3) 0.0030(17) 0.0170(18) 0.0024(16) C7 0.0210(18) 0.033(2) 0.048(2) 0.0094(18) 0.0109(17) 0.0059(16) C8 0.0180(17) 0.034(2) 0.040(2) 0.0037(17) 0.0065(16) 0.0012(15) C9 0.0164(16) 0.0272(18) 0.035(2) 0.0034(15) 0.0124(15) -0.0008(14) C10 0.0189(17) 0.0272(18) 0.034(2) -0.0008(15) 0.0085(15) -0.0047(14) C11 0.029(2) 0.048(3) 0.035(2) 0.0107(19) -0.0021(17) -0.0012(19) C12 0.035(2) 0.028(2) 0.050(3) -0.0117(19) 0.010(2) -0.0088(17) C13 0.026(2) 0.040(2) 0.030(2) 0.0090(17) -0.0003(16) 0.0028(17) C14 0.033(2) 0.030(2) 0.045(3) 0.0030(18) 0.0021(19) -0.0087(17) C15 0.0220(18) 0.048(2) 0.0234(18) 0.0032(17) 0.0094(15) -0.0017(17) C16 0.0208(17) 0.048(2) 0.0186(17) -0.0039(16) 0.0081(14) -0.0019(16) C17 0.028(2) 0.043(2) 0.027(2) -0.0042(17) 0.0127(16) -0.0054(17) C18 0.0229(19) 0.057(3) 0.031(2) -0.010(2) 0.0105(16) -0.0080(19) C19 0.0190(19) 0.066(3) 0.029(2) -0.005(2) 0.0021(16) 0.0017(19) C20 0.0213(18) 0.050(3) 0.030(2) -0.0015(18) 0.0078(16) 0.0081(18) C21 0.0217(18) 0.042(2) 0.0239(18) -0.0069(16) 0.0103(15) 0.0019(16) C22 0.0273(19) 0.036(2) 0.029(2) -0.0073(16) 0.0120(16) 0.0038(16) C23 0.034(2) 0.036(2) 0.034(2) 0.0009(18) 0.0068(18) 0.0084(18) C24 0.038(2) 0.0226(19) 0.048(3) -0.0072(18) 0.013(2) -0.0013(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Sb1 2.5021(5) . ? Cu1 Sb3 2.5111(5) . ? Cu1 Sb2 2.5150(5) . ? Cu1 Sb4 2.5222(5) . ? Sb1 C1 2.124(4) . ? Sb1 C2 2.128(4) . ? Sb1 C3 2.168(3) . ? Sb2 C12 2.117(4) . ? Sb2 C11 2.120(4) . ? Sb2 C10 2.155(4) . ? Sb3 C13 2.127(4) . ? Sb3 C14 2.139(4) . ? Sb3 C15 2.164(4) . ? Sb4 C24 2.129(4) . ? Sb4 C23 2.129(4) . ? Sb4 C22 2.168(4) . ? B1 F1 1.364(7) . ? B1 F2 1.367(6) . ? B1 F3 1.376(6) . ? B1 F4 1.381(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.501(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.399(5) . ? C4 C9 1.410(5) . ? C5 C6 1.378(6) . ? C5 H5 0.9500 . ? C6 C7 1.374(6) . ? C6 H6 0.9500 . ? C7 C8 1.387(6) . ? C7 H7 0.9500 . ? C8 C9 1.396(5) . ? C8 H8 0.9500 . ? C9 C10 1.505(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.493(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.406(6) . ? C16 C21 1.408(6) . ? C17 C18 1.377(6) . ? C17 H17 0.9500 . ? C18 C19 1.381(7) . ? C18 H18 0.9500 . ? C19 C20 1.379(6) . ? C19 H19 0.9500 . ? C20 C21 1.401(6) . ? C20 H20 0.9500 . ? C21 C22 1.497(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? O1 C26 1.426(7) . ? O1 C27 1.449(7) . ? C25 C26 1.526(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.495(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 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 Sb1 Cu1 Sb3 118.940(18) . . ? Sb1 Cu1 Sb2 103.189(16) . . ? Sb3 Cu1 Sb2 109.112(17) . . ? Sb1 Cu1 Sb4 114.264(17) . . ? Sb3 Cu1 Sb4 103.957(16) . . ? Sb2 Cu1 Sb4 106.848(17) . . ? C1 Sb1 C2 98.1(2) . . ? C1 Sb1 C3 99.30(15) . . ? C2 Sb1 C3 98.59(15) . . ? C1 Sb1 Cu1 122.20(13) . . ? C2 Sb1 Cu1 120.39(13) . . ? C3 Sb1 Cu1 113.86(10) . . ? C12 Sb2 C11 98.85(19) . . ? C12 Sb2 C10 95.33(16) . . ? C11 Sb2 C10 98.80(17) . . ? C12 Sb2 Cu1 120.88(12) . . ? C11 Sb2 Cu1 119.71(12) . . ? C10 Sb2 Cu1 118.23(10) . . ? C13 Sb3 C14 97.85(17) . . ? C13 Sb3 C15 96.04(16) . . ? C14 Sb3 C15 97.79(18) . . ? C13 Sb3 Cu1 122.86(12) . . ? C14 Sb3 Cu1 122.66(13) . . ? C15 Sb3 Cu1 113.99(11) . . ? C24 Sb4 C23 98.73(18) . . ? C24 Sb4 C22 95.90(16) . . ? C23 Sb4 C22 97.99(16) . . ? C24 Sb4 Cu1 122.09(12) . . ? C23 Sb4 Cu1 120.03(12) . . ? C22 Sb4 Cu1 116.92(11) . . ? F1 B1 F2 108.4(4) . . ? F1 B1 F3 108.9(5) . . ? F2 B1 F3 110.9(4) . . ? F1 B1 F4 108.5(4) . . ? F2 B1 F4 111.5(4) . . ? F3 B1 F4 108.5(4) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Sb1 111.0(2) . . ? C4 C3 H3A 109.4 . . ? Sb1 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? Sb1 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C9 118.3(3) . . ? C5 C4 C3 118.3(3) . . ? C9 C4 C3 123.4(3) . . ? C6 C5 C4 121.5(4) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C7 C6 C5 120.1(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 119.7(4) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C9 121.2(4) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 119.0(4) . . ? C8 C9 C10 118.8(4) . . ? C4 C9 C10 122.1(3) . . ? C9 C10 Sb2 113.6(2) . . ? C9 C10 H10A 108.8 . . ? Sb2 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? Sb2 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? Sb2 C11 H11A 109.5 . . ? Sb2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Sb2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Sb2 C12 H12A 109.5 . . ? Sb2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Sb2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Sb3 C13 H13A 109.5 . . ? Sb3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Sb3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Sb3 C14 H14A 109.5 . . ? Sb3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Sb3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 Sb3 114.9(3) . . ? C16 C15 H15A 108.5 . . ? Sb3 C15 H15A 108.5 . . ? C16 C15 H15B 108.5 . . ? Sb3 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C17 C16 C21 118.3(4) . . ? C17 C16 C15 119.0(4) . . ? C21 C16 C15 122.6(4) . . ? C18 C17 C16 122.2(4) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C19 119.3(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 119.8(4) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 121.9(4) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C20 C21 C16 118.4(4) . . ? C20 C21 C22 118.9(4) . . ? C16 C21 C22 122.7(3) . . ? C21 C22 Sb4 113.5(2) . . ? C21 C22 H22A 108.9 . . ? Sb4 C22 H22A 108.9 . . ? C21 C22 H22B 108.9 . . ? Sb4 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? Sb4 C23 H23A 109.5 . . ? Sb4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Sb4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Sb4 C24 H24A 109.5 . . ? Sb4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Sb4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 O1 C27 116.5(5) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O1 C26 C25 110.3(6) . . ? O1 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? O1 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? O1 C27 C28 103.9(6) . . ? O1 C27 H27A 111.0 . . ? C28 C27 H27A 111.0 . . ? O1 C27 H27B 111.0 . . ? C28 C27 H27B 111.0 . . ? H27A C27 H27B 109.0 . . ? 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 . . ? 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 C1 Sb1 C3 C4 158.0(3) . . . . ? C2 Sb1 C3 C4 58.3(3) . . . . ? Cu1 Sb1 C3 C4 -70.4(3) . . . . ? Sb1 C3 C4 C5 -89.0(4) . . . . ? Sb1 C3 C4 C9 91.9(4) . . . . ? C9 C4 C5 C6 -2.2(6) . . . . ? C3 C4 C5 C6 178.7(3) . . . . ? C4 C5 C6 C7 0.0(6) . . . . ? C5 C6 C7 C8 1.5(6) . . . . ? C6 C7 C8 C9 -0.6(6) . . . . ? C7 C8 C9 C4 -1.6(6) . . . . ? C7 C8 C9 C10 176.9(4) . . . . ? C5 C4 C9 C8 3.0(5) . . . . ? C3 C4 C9 C8 -177.9(3) . . . . ? C5 C4 C9 C10 -175.5(3) . . . . ? C3 C4 C9 C10 3.5(5) . . . . ? C8 C9 C10 Sb2 93.6(3) . . . . ? C4 C9 C10 Sb2 -87.8(4) . . . . ? C12 Sb2 C10 C9 -173.7(3) . . . . ? C11 Sb2 C10 C9 -73.9(3) . . . . ? Cu1 Sb2 C10 C9 56.9(3) . . . . ? C13 Sb3 C15 C16 170.7(3) . . . . ? C14 Sb3 C15 C16 71.9(3) . . . . ? Cu1 Sb3 C15 C16 -59.2(3) . . . . ? Sb3 C15 C16 C17 -88.0(4) . . . . ? Sb3 C15 C16 C21 93.8(4) . . . . ? C21 C16 C17 C18 1.9(6) . . . . ? C15 C16 C17 C18 -176.4(4) . . . . ? C16 C17 C18 C19 -0.3(6) . . . . ? C17 C18 C19 C20 -1.2(6) . . . . ? C18 C19 C20 C21 1.0(6) . . . . ? C19 C20 C21 C16 0.6(6) . . . . ? C19 C20 C21 C22 -179.5(4) . . . . ? C17 C16 C21 C20 -2.0(5) . . . . ? C15 C16 C21 C20 176.2(3) . . . . ? C17 C16 C21 C22 178.1(3) . . . . ? C15 C16 C21 C22 -3.7(5) . . . . ? C20 C21 C22 Sb4 94.5(4) . . . . ? C16 C21 C22 Sb4 -85.6(4) . . . . ? C24 Sb4 C22 C21 -170.5(3) . . . . ? C23 Sb4 C22 C21 -70.8(3) . . . . ? Cu1 Sb4 C22 C21 58.8(3) . . . . ? C27 O1 C26 C25 -173.4(7) . . . . ? C26 O1 C27 C28 178.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.914 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.127 #===END OF CIF =============================================================== data_niisb4 _database_code_depnum_ccdc_archive 'CCDC 228295' _audit_creation_method 'SHELXL-97 + hand edit' _chemical_name_systematic ; Iodobis(1,2-bis(dimethylstibanylmethyl)benzene)nickel(II) perchlorate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 I Ni Sb4 1+, Cl O4 1-' _chemical_formula_sum 'C24 H40 Cl I Ni O4 Sb4' _chemical_formula_weight 1100.62 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' I I -0.4742 1.8119 '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' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4616(15) _cell_length_b 13.608(3) _cell_length_c 27.146(4) _cell_angle_alpha 95.814(10) _cell_angle_beta 95.740(10) _cell_angle_gamma 107.789(8) _cell_volume 3279.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 47934 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 4.866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78889 # shelxl 0.5928 _exptl_absorpt_correction_T_max 0.88270 # 0.9090 _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38793 _diffrn_reflns_av_R_equivalents 0.1004 _diffrn_reflns_av_sigmaI/netI 0.1030 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11251 _reflns_number_gt 7012 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+3.4579P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00079(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11251 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1595 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.91208(18) 0.26624(13) 0.10829(6) 0.0214(4) Uani 1 1 d . . . Ni2 Ni 0.60374(18) 0.75059(13) 0.38430(6) 0.0212(4) Uani 1 1 d . . . I1 I 1.16888(10) 0.40270(7) 0.09953(4) 0.0330(3) Uani 1 1 d . . . I2 I 0.34215(10) 0.61043(7) 0.38388(4) 0.0340(3) Uani 1 1 d . . . Sb1 Sb 0.90650(10) 0.08661(7) 0.11597(3) 0.0215(2) Uani 1 1 d . . . Sb2 Sb 0.98963(10) 0.31280(7) 0.19816(3) 0.0269(2) Uani 1 1 d . . . Sb3 Sb 0.69061(10) 0.32609(7) 0.10740(3) 0.0241(2) Uani 1 1 d . . . Sb4 Sb 0.87317(10) 0.23453(7) 0.01700(3) 0.0229(2) Uani 1 1 d . . . Sb5 Sb 0.82862(10) 0.69401(7) 0.38358(3) 0.0234(2) Uani 1 1 d . . . Sb6 Sb 0.62999(10) 0.76122(7) 0.47494(3) 0.0233(2) Uani 1 1 d . . . Sb7 Sb 0.60698(10) 0.93239(7) 0.38440(3) 0.0220(2) Uani 1 1 d . . . Sb8 Sb 0.54366(10) 0.72249(7) 0.29383(3) 0.0260(2) Uani 1 1 d . . . Cl1 Cl 0.9780(4) 0.7223(3) 0.15298(12) 0.0306(8) Uani 1 1 d . . . Cl2 Cl 0.5393(4) 0.3073(3) 0.35341(13) 0.0326(8) Uani 1 1 d . . . O1 O 0.942(4) 0.6806(15) 0.1954(7) 0.142(11) Uani 1 1 d . . . O2 O 0.9024(14) 0.7978(9) 0.1461(4) 0.049(3) Uani 1 1 d . . . O3 O 1.1335(16) 0.7768(13) 0.1572(9) 0.107(7) Uani 1 1 d . . . O4 O 0.9373(13) 0.6431(9) 0.1107(4) 0.046(3) Uani 1 1 d . . . O5 O 0.5365(12) 0.3611(9) 0.4016(4) 0.044(3) Uani 1 1 d . . . O6 O 0.6470(17) 0.3742(11) 0.3288(5) 0.070(4) Uani 1 1 d . . . O7 O 0.5835(16) 0.2183(9) 0.3600(4) 0.057(3) Uani 1 1 d . . . O8 O 0.3989(15) 0.2771(13) 0.3240(5) 0.081(5) Uani 1 1 d . . . C1 C 0.7472(17) -0.0419(11) 0.0683(5) 0.030(3) Uani 1 1 d . . . H1A H 0.7565 -0.0326 0.0333 0.099(11) Uiso 1 1 calc R . . H1B H 0.6458 -0.0457 0.0748 0.099(11) Uiso 1 1 calc R . . H1C H 0.7662 -0.1066 0.0748 0.099(11) Uiso 1 1 calc R . . C2 C 1.1088(17) 0.0470(14) 0.1136(7) 0.042(4) Uani 1 1 d . . . H2A H 1.1518 0.0676 0.0834 0.099(11) Uiso 1 1 calc R . . H2B H 1.0861 -0.0283 0.1132 0.099(11) Uiso 1 1 calc R . . H2C H 1.1808 0.0838 0.1432 0.099(11) Uiso 1 1 calc R . . C3 C 0.8440(15) 0.0345(10) 0.1846(5) 0.023(3) Uani 1 1 d . . . H3A H 0.8295 -0.0410 0.1828 0.044(8) Uiso 1 1 calc R . . H3B H 0.9250 0.0716 0.2124 0.044(8) Uiso 1 1 calc R . . C4 C 0.6998(16) 0.0553(11) 0.1947(5) 0.028(3) Uani 1 1 d . . . C5 C 0.5642(16) -0.0169(12) 0.1748(5) 0.032(3) Uani 1 1 d . . . H5 H 0.5639 -0.0766 0.1533 0.044(8) Uiso 1 1 calc R . . C6 C 0.4271(18) -0.0069(14) 0.1844(6) 0.041(4) Uani 1 1 d . . . H6 H 0.3351 -0.0605 0.1725 0.044(8) Uiso 1 1 calc R . . C7 C 0.4325(19) 0.0874(13) 0.2129(6) 0.037(4) Uani 1 1 d . . . H7 H 0.3409 0.0981 0.2192 0.044(8) Uiso 1 1 calc R . . C8 C 0.5651(19) 0.1643(14) 0.2318(6) 0.038(4) Uani 1 1 d . . . H8 H 0.5649 0.2265 0.2511 0.044(8) Uiso 1 1 calc R . . C9 C 0.7011(17) 0.1494(12) 0.2223(6) 0.035(4) Uani 1 1 d . . . C10 C 0.8460(19) 0.2325(13) 0.2474(6) 0.043(4) Uani 1 1 d . . . H10A H 0.9031 0.1990 0.2689 0.044(8) Uiso 1 1 calc R . . H10B H 0.8194 0.2847 0.2696 0.044(8) Uiso 1 1 calc R . . C11 C 1.0383(19) 0.4708(11) 0.2301(6) 0.041(4) Uani 1 1 d . . . H11A H 1.1049 0.5164 0.2105 0.099(11) Uiso 1 1 calc R . . H11B H 1.0875 0.4808 0.2645 0.099(11) Uiso 1 1 calc R . . H11C H 0.9449 0.4879 0.2299 0.099(11) Uiso 1 1 calc R . . C12 C 1.1923(18) 0.2826(12) 0.2256(6) 0.039(4) Uani 1 1 d . . . H12A H 1.1842 0.2106 0.2135 0.099(11) Uiso 1 1 calc R . . H12B H 1.2066 0.2932 0.2623 0.099(11) Uiso 1 1 calc R . . H12C H 1.2780 0.3304 0.2136 0.099(11) Uiso 1 1 calc R . . C13 C 0.4784(18) 0.2078(12) 0.0872(7) 0.040(4) Uani 1 1 d . . . H13A H 0.4827 0.1601 0.0582 0.099(11) Uiso 1 1 calc R . . H13B H 0.4013 0.2400 0.0787 0.099(11) Uiso 1 1 calc R . . H13C H 0.4539 0.1688 0.1153 0.099(11) Uiso 1 1 calc R . . C14 C 0.645(2) 0.4147(13) 0.1701(6) 0.040(4) Uani 1 1 d . . . H14A H 0.7347 0.4737 0.1834 0.099(11) Uiso 1 1 calc R . . H14B H 0.6167 0.3702 0.1960 0.099(11) Uiso 1 1 calc R . . H14C H 0.5625 0.4407 0.1594 0.099(11) Uiso 1 1 calc R . . C15 C 0.6709(16) 0.4326(11) 0.0546(5) 0.028(3) Uani 1 1 d . . . H15A H 0.6044 0.4711 0.0663 0.044(8) Uiso 1 1 calc R . . H15B H 0.7711 0.4841 0.0551 0.044(8) Uiso 1 1 calc R . . C16 C 0.6116(15) 0.3828(10) 0.0020(5) 0.024(3) Uani 1 1 d . . . C17 C 0.4609(16) 0.3674(10) -0.0151(6) 0.033(3) Uani 1 1 d . . . H17 H 0.3994 0.3847 0.0077 0.044(8) Uiso 1 1 calc R . . C18 C 0.3992(17) 0.3281(11) -0.0638(6) 0.032(3) Uani 1 1 d . . . H18 H 0.2954 0.3153 -0.0738 0.044(8) Uiso 1 1 calc R . . C19 C 0.487(2) 0.3074(12) -0.0978(6) 0.045(4) Uani 1 1 d . . . H19 H 0.4458 0.2843 -0.1320 0.044(8) Uiso 1 1 calc R . . C20 C 0.6373(17) 0.3205(12) -0.0819(5) 0.030(3) Uani 1 1 d . . . H20 H 0.6986 0.3030 -0.1047 0.044(8) Uiso 1 1 calc R . . C21 C 0.6968(15) 0.3599(12) -0.0317(6) 0.033(4) Uani 1 1 d . . . C22 C 0.8598(15) 0.3670(11) -0.0173(6) 0.027(3) Uani 1 1 d . . . H22A H 0.9115 0.4315 0.0063 0.044(8) Uiso 1 1 calc R . . H22B H 0.9108 0.3705 -0.0475 0.044(8) Uiso 1 1 calc R . . C23 C 1.0426(18) 0.1882(12) -0.0134(6) 0.039(4) Uani 1 1 d . . . H23A H 1.0535 0.1274 0.0011 0.099(11) Uiso 1 1 calc R . . H23B H 1.1376 0.2455 -0.0058 0.099(11) Uiso 1 1 calc R . . H23C H 1.0157 0.1700 -0.0497 0.099(11) Uiso 1 1 calc R . . C24 C 0.6775(15) 0.1169(10) -0.0237(6) 0.031(3) Uani 1 1 d . . . H24A H 0.5873 0.1288 -0.0132 0.099(11) Uiso 1 1 calc R . . H24B H 0.6794 0.0479 -0.0169 0.099(11) Uiso 1 1 calc R . . H24C H 0.6767 0.1205 -0.0596 0.099(11) Uiso 1 1 calc R . . C25 C 1.0383(15) 0.8151(12) 0.4114(6) 0.032(3) Uani 1 1 d . . . H25A H 1.0456 0.8756 0.3939 0.099(11) Uiso 1 1 calc R . . H25B H 1.1218 0.7890 0.4056 0.099(11) Uiso 1 1 calc R . . H25C H 1.0426 0.8356 0.4473 0.099(11) Uiso 1 1 calc R . . C26 C 0.8879(18) 0.6245(12) 0.3165(6) 0.036(4) Uani 1 1 d . . . H26A H 0.8847 0.6676 0.2899 0.099(11) Uiso 1 1 calc R . . H26B H 0.8165 0.5544 0.3059 0.099(11) Uiso 1 1 calc R . . H26C H 0.9892 0.6200 0.3235 0.099(11) Uiso 1 1 calc R . . C27 C 0.8494(16) 0.5779(11) 0.4290(5) 0.028(3) Uani 1 1 d . . . H27A H 0.7515 0.5218 0.4242 0.044(8) Uiso 1 1 calc R . . H27B H 0.9229 0.5469 0.4162 0.044(8) Uiso 1 1 calc R . . C28 C 0.8960(17) 0.6113(10) 0.4841(5) 0.029(3) Uani 1 1 d . . . C29 C 1.0467(16) 0.6281(11) 0.5024(6) 0.033(3) Uani 1 1 d . . . H29 H 1.1145 0.6229 0.4794 0.044(8) Uiso 1 1 calc R . . C30 C 1.0988(17) 0.6518(11) 0.5525(6) 0.037(4) Uani 1 1 d . . . H30 H 1.2002 0.6599 0.5644 0.044(8) Uiso 1 1 calc R . . C31 C 0.9984(18) 0.6640(11) 0.5863(6) 0.039(4) Uani 1 1 d . . . H31 H 1.0329 0.6820 0.6211 0.044(8) Uiso 1 1 calc R . . C32 C 0.8499(19) 0.6499(12) 0.5686(6) 0.036(4) Uani 1 1 d . . . H32 H 0.7816 0.6556 0.5913 0.044(8) Uiso 1 1 calc R . . C33 C 0.8027(17) 0.6275(11) 0.5181(5) 0.030(3) Uani 1 1 d . . . C34 C 0.6381(17) 0.6177(11) 0.5002(6) 0.032(3) Uani 1 1 d . . . H34A H 0.5779 0.6031 0.5280 0.044(8) Uiso 1 1 calc R . . H34B H 0.5954 0.5593 0.4726 0.044(8) Uiso 1 1 calc R . . C35 C 0.4562(16) 0.7999(13) 0.5077(6) 0.039(4) Uani 1 1 d . . . H35A H 0.3588 0.7549 0.4901 0.099(11) Uiso 1 1 calc R . . H35B H 0.4657 0.8729 0.5051 0.099(11) Uiso 1 1 calc R . . H35C H 0.4638 0.7898 0.5430 0.099(11) Uiso 1 1 calc R . . C36 C 0.8199(18) 0.8710(12) 0.5211(6) 0.038(4) Uani 1 1 d . . . H36A H 0.9120 0.8630 0.5103 0.099(11) Uiso 1 1 calc R . . H36B H 0.8167 0.8585 0.5560 0.099(11) Uiso 1 1 calc R . . H36C H 0.8181 0.9419 0.5183 0.099(11) Uiso 1 1 calc R . . C37 C 0.7597(16) 1.0536(11) 0.4379(5) 0.028(3) Uani 1 1 d . . . H37A H 0.8598 1.0463 0.4395 0.099(11) Uiso 1 1 calc R . . H37B H 0.7262 1.0488 0.4708 0.099(11) Uiso 1 1 calc R . . H37C H 0.7632 1.1215 0.4279 0.099(11) Uiso 1 1 calc R . . C38 C 0.4046(16) 0.9694(14) 0.3898(6) 0.040(4) Uani 1 1 d . . . H38A H 0.3225 0.9187 0.3666 0.099(11) Uiso 1 1 calc R . . H38B H 0.4177 1.0395 0.3810 0.099(11) Uiso 1 1 calc R . . H38C H 0.3808 0.9669 0.4240 0.099(11) Uiso 1 1 calc R . . C39 C 0.6757(17) 1.0000(12) 0.3180(5) 0.033(3) Uani 1 1 d . . . H39A H 0.6016 0.9630 0.2884 0.044(8) Uiso 1 1 calc R . . H39B H 0.6813 1.0743 0.3219 0.044(8) Uiso 1 1 calc R . . C40 C 0.8238(17) 0.9907(10) 0.3109(5) 0.030(3) Uani 1 1 d . . . C41 C 0.9557(18) 1.0677(12) 0.3326(5) 0.034(4) Uani 1 1 d . . . H41 H 0.9478 1.1254 0.3537 0.044(8) Uiso 1 1 calc R . . C42 C 1.0975(17) 1.0658(13) 0.3256(5) 0.037(4) Uani 1 1 d . . . H42 H 1.1841 1.1221 0.3400 0.044(8) Uiso 1 1 calc R . . C43 C 1.1096(18) 0.9804(14) 0.2972(6) 0.042(4) Uani 1 1 d . . . H43 H 1.2055 0.9763 0.2919 0.044(8) Uiso 1 1 calc R . . C44 C 0.9787(18) 0.8983(13) 0.2759(6) 0.036(4) Uani 1 1 d . . . H44 H 0.9887 0.8382 0.2575 0.044(8) Uiso 1 1 calc R . . C45 C 0.8359(16) 0.9025(11) 0.2808(5) 0.027(3) Uani 1 1 d . . . C46 C 0.7006(17) 0.8186(12) 0.2526(5) 0.033(3) Uani 1 1 d . . . H46A H 0.7367 0.7720 0.2304 0.044(8) Uiso 1 1 calc R . . H46B H 0.6449 0.8525 0.2309 0.044(8) Uiso 1 1 calc R . . C47 C 0.3434(19) 0.7508(12) 0.2669(6) 0.040(4) Uani 1 1 d . . . H47A H 0.3456 0.8198 0.2822 0.099(11) Uiso 1 1 calc R . . H47B H 0.2571 0.6975 0.2756 0.099(11) Uiso 1 1 calc R . . H47C H 0.3350 0.7483 0.2305 0.099(11) Uiso 1 1 calc R . . C48 C 0.5085(19) 0.5723(12) 0.2554(6) 0.041(4) Uani 1 1 d . . . H48A H 0.5953 0.5497 0.2646 0.099(11) Uiso 1 1 calc R . . H48B H 0.4956 0.5743 0.2193 0.099(11) Uiso 1 1 calc R . . H48C H 0.4184 0.5233 0.2644 0.099(11) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0184(9) 0.0230(9) 0.0238(9) 0.0015(7) 0.0002(7) 0.0093(7) Ni2 0.0175(9) 0.0243(9) 0.0226(9) 0.0000(7) 0.0022(7) 0.0092(7) I1 0.0216(5) 0.0302(5) 0.0419(6) 0.0024(4) 0.0025(4) 0.0020(4) I2 0.0217(5) 0.0337(5) 0.0396(6) 0.0007(4) 0.0037(4) 0.0003(4) Sb1 0.0185(5) 0.0221(5) 0.0252(5) 0.0024(4) 0.0022(4) 0.0090(4) Sb2 0.0261(5) 0.0281(5) 0.0256(5) -0.0028(4) -0.0036(4) 0.0116(4) Sb3 0.0212(5) 0.0267(5) 0.0267(5) 0.0002(4) 0.0019(4) 0.0125(4) Sb4 0.0180(5) 0.0262(5) 0.0252(5) 0.0024(4) 0.0029(4) 0.0084(4) Sb5 0.0194(5) 0.0268(5) 0.0260(5) 0.0017(4) 0.0048(4) 0.0105(4) Sb6 0.0186(5) 0.0276(5) 0.0241(5) 0.0017(4) 0.0038(4) 0.0085(4) Sb7 0.0184(5) 0.0237(5) 0.0250(5) 0.0010(4) 0.0025(4) 0.0090(4) Sb8 0.0240(5) 0.0289(5) 0.0241(5) -0.0029(4) -0.0006(4) 0.0100(4) Cl1 0.034(2) 0.0351(19) 0.0242(18) 0.0009(15) 0.0000(15) 0.0146(16) Cl2 0.030(2) 0.037(2) 0.0250(19) 0.0035(15) -0.0028(15) 0.0049(16) O1 0.33(3) 0.095(13) 0.076(12) 0.048(11) 0.107(17) 0.131(18) O2 0.061(8) 0.040(6) 0.051(7) 0.012(6) 0.003(6) 0.021(6) O3 0.038(9) 0.077(11) 0.19(2) -0.044(11) -0.007(10) 0.017(8) O4 0.054(7) 0.053(7) 0.033(6) -0.015(5) -0.010(5) 0.031(6) O5 0.040(7) 0.051(7) 0.040(7) 0.004(5) 0.003(5) 0.012(5) O6 0.080(10) 0.068(9) 0.049(8) -0.003(7) 0.036(7) -0.002(8) O7 0.091(10) 0.043(7) 0.040(7) -0.015(5) -0.008(6) 0.036(7) O8 0.042(8) 0.119(12) 0.064(9) -0.018(9) -0.033(7) 0.020(8) C1 0.034(8) 0.026(8) 0.028(8) 0.002(6) -0.007(6) 0.009(6) C2 0.020(8) 0.060(11) 0.054(10) 0.016(9) 0.011(7) 0.019(8) C3 0.023(7) 0.025(7) 0.028(7) 0.016(6) 0.007(6) 0.014(6) C4 0.024(8) 0.028(8) 0.040(8) 0.012(7) 0.005(6) 0.016(6) C5 0.023(8) 0.046(9) 0.027(8) 0.007(7) 0.003(6) 0.012(7) C6 0.027(9) 0.063(11) 0.030(9) 0.009(8) 0.001(7) 0.011(8) C7 0.036(9) 0.051(10) 0.033(9) 0.016(8) 0.020(7) 0.020(8) C8 0.045(10) 0.055(10) 0.033(9) 0.016(8) 0.013(7) 0.037(9) C9 0.033(9) 0.038(9) 0.037(9) 0.000(7) -0.002(7) 0.019(7) C10 0.045(10) 0.055(10) 0.025(8) -0.003(7) 0.009(7) 0.014(8) C11 0.049(10) 0.030(8) 0.035(9) -0.015(7) -0.022(7) 0.016(7) C12 0.044(10) 0.036(9) 0.043(10) 0.002(7) -0.010(7) 0.027(8) C13 0.031(9) 0.025(8) 0.062(11) 0.012(7) 0.009(8) 0.005(7) C14 0.053(11) 0.045(10) 0.032(9) 0.002(7) 0.013(8) 0.027(8) C15 0.023(8) 0.031(8) 0.028(8) -0.006(6) -0.005(6) 0.014(6) C16 0.024(8) 0.019(7) 0.030(8) 0.009(6) 0.002(6) 0.004(6) C17 0.025(8) 0.020(7) 0.049(10) -0.001(7) -0.005(7) 0.004(6) C18 0.025(8) 0.026(8) 0.044(9) 0.008(7) -0.011(7) 0.012(6) C19 0.062(12) 0.033(9) 0.034(9) -0.007(7) -0.023(8) 0.019(8) C20 0.031(8) 0.043(9) 0.030(8) 0.018(7) 0.003(6) 0.026(7) C21 0.012(7) 0.043(9) 0.045(10) 0.026(7) -0.005(6) 0.008(6) C22 0.024(8) 0.023(7) 0.040(8) 0.010(6) 0.010(6) 0.012(6) C23 0.036(9) 0.038(9) 0.049(10) 0.001(7) 0.010(8) 0.020(7) C24 0.020(8) 0.022(7) 0.046(9) -0.002(7) -0.002(6) 0.002(6) C25 0.015(7) 0.037(8) 0.041(9) -0.007(7) 0.001(6) 0.008(6) C26 0.035(9) 0.035(8) 0.047(10) -0.001(7) 0.005(7) 0.026(7) C27 0.028(8) 0.024(7) 0.040(9) 0.010(6) 0.017(7) 0.013(6) C28 0.040(9) 0.014(7) 0.030(8) 0.002(6) 0.009(7) 0.004(6) C29 0.022(8) 0.023(7) 0.051(10) 0.007(7) -0.006(7) 0.007(6) C30 0.025(8) 0.026(8) 0.057(11) 0.017(7) -0.013(7) 0.005(6) C31 0.043(10) 0.019(7) 0.049(10) -0.005(7) -0.017(8) 0.013(7) C32 0.049(10) 0.035(9) 0.035(9) 0.016(7) -0.002(7) 0.026(8) C33 0.036(9) 0.022(7) 0.032(8) 0.011(6) -0.003(6) 0.009(6) C34 0.038(9) 0.026(8) 0.035(8) 0.018(7) 0.014(7) 0.008(7) C35 0.019(8) 0.058(10) 0.037(9) 0.000(8) -0.006(6) 0.012(7) C36 0.035(9) 0.033(8) 0.043(9) 0.002(7) -0.011(7) 0.013(7) C37 0.024(8) 0.033(8) 0.027(8) -0.008(6) 0.005(6) 0.011(6) C38 0.015(7) 0.058(10) 0.051(10) 0.007(8) 0.013(7) 0.013(7) C39 0.038(9) 0.044(9) 0.025(8) 0.002(7) 0.004(7) 0.023(7) C40 0.035(9) 0.022(7) 0.028(8) 0.009(6) 0.009(6) -0.001(6) C41 0.048(10) 0.040(9) 0.017(7) 0.009(7) 0.003(7) 0.018(8) C42 0.022(8) 0.056(10) 0.024(8) 0.005(7) 0.010(6) -0.003(7) C43 0.028(9) 0.073(12) 0.036(9) 0.020(9) 0.016(7) 0.024(9) C44 0.043(10) 0.044(9) 0.035(9) 0.026(7) 0.020(7) 0.021(8) C45 0.030(8) 0.041(8) 0.016(7) 0.005(6) 0.010(6) 0.019(7) C46 0.031(8) 0.038(8) 0.027(8) 0.000(7) 0.007(6) 0.007(7) C47 0.043(10) 0.034(9) 0.041(9) 0.005(7) 0.004(7) 0.012(7) C48 0.046(10) 0.035(9) 0.041(9) 0.003(7) 0.003(8) 0.012(8) _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 Ni1 Sb2 2.4364(19) . ? Ni1 Sb4 2.4427(19) . ? Ni1 Sb1 2.4592(19) . ? Ni1 Sb3 2.4681(19) . ? Ni1 I1 2.6185(19) . ? Ni2 Sb8 2.4286(19) . ? Ni2 Sb6 2.4333(19) . ? Ni2 Sb7 2.4645(19) . ? Ni2 Sb5 2.4751(19) . ? Ni2 I2 2.6209(19) . ? Sb1 C1 2.132(14) . ? Sb1 C3 2.135(12) . ? Sb1 C2 2.146(15) . ? Sb2 C11 2.126(14) . ? Sb2 C10 2.141(15) . ? Sb2 C12 2.158(15) . ? Sb3 C13 2.133(15) . ? Sb3 C14 2.141(14) . ? Sb3 C15 2.172(14) . ? Sb4 C23 2.104(15) . ? Sb4 C22 2.142(13) . ? Sb4 C24 2.152(13) . ? Sb5 C27 2.144(13) . ? Sb5 C25 2.161(14) . ? Sb5 C26 2.168(15) . ? Sb6 C35 2.121(15) . ? Sb6 C36 2.136(15) . ? Sb6 C34 2.155(14) . ? Sb7 C37 2.134(14) . ? Sb7 C38 2.138(15) . ? Sb7 C39 2.174(14) . ? Sb8 C48 2.112(16) . ? Sb8 C47 2.121(17) . ? Sb8 C46 2.147(14) . ? Cl1 O1 1.363(15) . ? Cl1 O3 1.418(15) . ? Cl1 O4 1.427(11) . ? Cl1 O2 1.436(12) . ? Cl2 O8 1.400(13) . ? Cl2 O6 1.416(13) . ? Cl2 O7 1.417(12) . ? Cl2 O5 1.439(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.520(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.37(2) . ? C4 C9 1.41(2) . ? C5 C6 1.39(2) . ? C5 H5 0.9500 . ? C6 C7 1.41(2) . ? C6 H6 0.9500 . ? C7 C8 1.38(2) . ? C7 H7 0.9500 . ? C8 C9 1.41(2) . ? C8 H8 0.9500 . ? C9 C10 1.53(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.493(19) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.35(2) . ? C16 C17 1.40(2) . ? C17 C18 1.37(2) . ? C17 H17 0.9500 . ? C18 C19 1.36(2) . ? C18 H18 0.9500 . ? C19 C20 1.40(2) . ? C19 H19 0.9500 . ? C20 C21 1.41(2) . ? C20 H20 0.9500 . ? C21 C22 1.524(19) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? 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 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 1.50(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C33 1.39(2) . ? C28 C29 1.40(2) . ? C29 C30 1.37(2) . ? C29 H29 0.9500 . ? C30 C31 1.42(2) . ? C30 H30 0.9500 . ? C31 C32 1.39(2) . ? C31 H31 0.9500 . ? C32 C33 1.37(2) . ? C32 H32 0.9500 . ? C33 C34 1.55(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.47(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.39(2) . ? C40 C45 1.42(2) . ? C41 C42 1.38(2) . ? C41 H41 0.9500 . ? C42 C43 1.37(2) . ? C42 H42 0.9500 . ? C43 C44 1.41(2) . ? C43 H43 0.9500 . ? C44 C45 1.39(2) . ? C44 H44 0.9500 . ? C45 C46 1.50(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 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 Sb2 Ni1 Sb4 171.36(8) . . ? Sb2 Ni1 Sb1 89.35(6) . . ? Sb4 Ni1 Sb1 93.19(6) . . ? Sb2 Ni1 Sb3 95.19(6) . . ? Sb4 Ni1 Sb3 90.20(6) . . ? Sb1 Ni1 Sb3 124.26(7) . . ? Sb2 Ni1 I1 85.74(6) . . ? Sb4 Ni1 I1 85.77(6) . . ? Sb1 Ni1 I1 117.99(7) . . ? Sb3 Ni1 I1 117.75(7) . . ? Sb8 Ni2 Sb6 172.07(8) . . ? Sb8 Ni2 Sb7 89.18(6) . . ? Sb6 Ni2 Sb7 94.21(6) . . ? Sb8 Ni2 Sb5 94.04(6) . . ? Sb6 Ni2 Sb5 89.97(6) . . ? Sb7 Ni2 Sb5 124.28(7) . . ? Sb8 Ni2 I2 85.85(6) . . ? Sb6 Ni2 I2 86.22(6) . . ? Sb7 Ni2 I2 116.69(7) . . ? Sb5 Ni2 I2 119.02(7) . . ? C1 Sb1 C3 96.1(6) . . ? C1 Sb1 C2 101.7(6) . . ? C3 Sb1 C2 100.3(6) . . ? C1 Sb1 Ni1 120.6(4) . . ? C3 Sb1 Ni1 114.7(4) . . ? C2 Sb1 Ni1 119.2(5) . . ? C11 Sb2 C10 101.5(7) . . ? C11 Sb2 C12 101.1(6) . . ? C10 Sb2 C12 98.8(7) . . ? C11 Sb2 Ni1 118.6(4) . . ? C10 Sb2 Ni1 118.6(4) . . ? C12 Sb2 Ni1 114.9(4) . . ? C13 Sb3 C14 100.3(7) . . ? C13 Sb3 C15 100.3(6) . . ? C14 Sb3 C15 95.6(6) . . ? C13 Sb3 Ni1 115.9(4) . . ? C14 Sb3 Ni1 123.9(5) . . ? C15 Sb3 Ni1 116.6(4) . . ? C23 Sb4 C22 106.1(6) . . ? C23 Sb4 C24 100.2(6) . . ? C22 Sb4 C24 100.0(6) . . ? C23 Sb4 Ni1 113.4(5) . . ? C22 Sb4 Ni1 113.7(4) . . ? C24 Sb4 Ni1 121.4(4) . . ? C27 Sb5 C25 99.5(6) . . ? C27 Sb5 C26 96.4(6) . . ? C25 Sb5 C26 100.3(6) . . ? C27 Sb5 Ni2 118.3(4) . . ? C25 Sb5 Ni2 114.7(4) . . ? C26 Sb5 Ni2 123.3(4) . . ? C35 Sb6 C36 99.5(6) . . ? C35 Sb6 C34 106.4(6) . . ? C36 Sb6 C34 100.9(6) . . ? C35 Sb6 Ni2 114.3(4) . . ? C36 Sb6 Ni2 121.2(5) . . ? C34 Sb6 Ni2 112.6(4) . . ? C37 Sb7 C38 100.4(6) . . ? C37 Sb7 C39 96.9(6) . . ? C38 Sb7 C39 100.9(6) . . ? C37 Sb7 Ni2 120.3(4) . . ? C38 Sb7 Ni2 119.5(5) . . ? C39 Sb7 Ni2 114.8(4) . . ? C48 Sb8 C47 101.2(6) . . ? C48 Sb8 C46 101.7(6) . . ? C47 Sb8 C46 101.0(6) . . ? C48 Sb8 Ni2 118.5(5) . . ? C47 Sb8 Ni2 114.5(4) . . ? C46 Sb8 Ni2 117.2(4) . . ? O1 Cl1 O3 111.4(17) . . ? O1 Cl1 O4 110.9(11) . . ? O3 Cl1 O4 108.8(9) . . ? O1 Cl1 O2 108.6(10) . . ? O3 Cl1 O2 106.4(9) . . ? O4 Cl1 O2 110.6(7) . . ? O8 Cl2 O6 109.4(10) . . ? O8 Cl2 O7 109.9(9) . . ? O6 Cl2 O7 108.1(9) . . ? O8 Cl2 O5 111.2(8) . . ? O6 Cl2 O5 108.9(7) . . ? O7 Cl2 O5 109.3(7) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Sb1 109.9(8) . . ? C4 C3 H3A 109.7 . . ? Sb1 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 . . ? Sb1 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C9 118.7(13) . . ? C5 C4 C3 119.6(13) . . ? C9 C4 C3 121.6(13) . . ? C4 C5 C6 123.3(15) . . ? C4 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C5 C6 C7 116.3(15) . . ? C5 C6 H6 121.9 . . ? C7 C6 H6 121.9 . . ? C8 C7 C6 122.5(15) . . ? C8 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? C7 C8 C9 119.1(15) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C8 C9 C4 119.8(14) . . ? C8 C9 C10 117.4(14) . . ? C4 C9 C10 122.5(13) . . ? C9 C10 Sb2 115.9(10) . . ? C9 C10 H10A 108.3 . . ? Sb2 C10 H10A 108.3 . . ? C9 C10 H10B 108.3 . . ? Sb2 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? Sb2 C11 H11A 109.5 . . ? Sb2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Sb2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Sb2 C12 H12A 109.5 . . ? Sb2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Sb2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Sb3 C13 H13A 109.5 . . ? Sb3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Sb3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Sb3 C14 H14A 109.5 . . ? Sb3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Sb3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 Sb3 115.3(9) . . ? C16 C15 H15A 108.4 . . ? Sb3 C15 H15A 108.4 . . ? C16 C15 H15B 108.4 . . ? Sb3 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C21 C16 C17 117.5(14) . . ? C21 C16 C15 124.3(13) . . ? C17 C16 C15 118.0(13) . . ? C18 C17 C16 121.9(15) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C19 C18 C17 120.2(14) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.3(15) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C21 119.1(14) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C16 C21 C20 121.9(13) . . ? C16 C21 C22 122.5(13) . . ? C20 C21 C22 115.4(13) . . ? C21 C22 Sb4 110.5(9) . . ? C21 C22 H22A 109.5 . . ? Sb4 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? Sb4 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? Sb4 C23 H23A 109.5 . . ? Sb4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Sb4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Sb4 C24 H24A 109.5 . . ? Sb4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Sb4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Sb5 C25 H25A 109.5 . . ? Sb5 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Sb5 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Sb5 C26 H26A 109.5 . . ? Sb5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Sb5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 Sb5 117.8(9) . . ? C28 C27 H27A 107.9 . . ? Sb5 C27 H27A 107.9 . . ? C28 C27 H27B 107.9 . . ? Sb5 C27 H27B 107.9 . . ? H27A C27 H27B 107.2 . . ? C33 C28 C29 117.6(14) . . ? C33 C28 C27 125.3(14) . . ? C29 C28 C27 117.0(13) . . ? C30 C29 C28 121.8(15) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C31 118.7(14) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? C32 C31 C30 120.2(15) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C33 C32 C31 119.3(16) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C28 122.2(15) . . ? C32 C33 C34 117.2(14) . . ? C28 C33 C34 120.6(13) . . ? C33 C34 Sb6 109.2(9) . . ? C33 C34 H34A 109.8 . . ? Sb6 C34 H34A 109.8 . . ? C33 C34 H34B 109.8 . . ? Sb6 C34 H34B 109.8 . . ? H34A C34 H34B 108.3 . . ? Sb6 C35 H35A 109.5 . . ? Sb6 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Sb6 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Sb6 C36 H36A 109.5 . . ? Sb6 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Sb6 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Sb7 C37 H37A 109.5 . . ? Sb7 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Sb7 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Sb7 C38 H38A 109.5 . . ? Sb7 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Sb7 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 Sb7 108.8(10) . . ? C40 C39 H39A 109.9 . . ? Sb7 C39 H39A 109.9 . . ? C40 C39 H39B 109.9 . . ? Sb7 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? C41 C40 C45 117.7(14) . . ? C41 C40 C39 121.6(14) . . ? C45 C40 C39 120.7(13) . . ? C42 C41 C40 124.4(15) . . ? C42 C41 H41 117.8 . . ? C40 C41 H41 117.8 . . ? C43 C42 C41 118.0(15) . . ? C43 C42 H42 121.0 . . ? C41 C42 H42 121.0 . . ? C42 C43 C44 119.6(14) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C45 C44 C43 122.4(15) . . ? C45 C44 H44 118.8 . . ? C43 C44 H44 118.8 . . ? C44 C45 C40 117.8(14) . . ? C44 C45 C46 120.2(13) . . ? C40 C45 C46 122.0(13) . . ? C45 C46 Sb8 119.1(9) . . ? C45 C46 H46A 107.6 . . ? Sb8 C46 H46A 107.6 . . ? C45 C46 H46B 107.6 . . ? Sb8 C46 H46B 107.6 . . ? H46A C46 H46B 107.0 . . ? Sb8 C47 H47A 109.5 . . ? Sb8 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Sb8 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Sb8 C48 H48A 109.5 . . ? Sb8 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Sb8 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sb2 Ni1 Sb1 C1 146.8(5) . . . . ? Sb4 Ni1 Sb1 C1 -41.5(5) . . . . ? Sb3 Ni1 Sb1 C1 51.0(5) . . . . ? I1 Ni1 Sb1 C1 -128.4(5) . . . . ? Sb2 Ni1 Sb1 C3 32.7(4) . . . . ? Sb4 Ni1 Sb1 C3 -155.6(4) . . . . ? Sb3 Ni1 Sb1 C3 -63.2(4) . . . . ? I1 Ni1 Sb1 C3 117.5(4) . . . . ? Sb2 Ni1 Sb1 C2 -86.2(5) . . . . ? Sb4 Ni1 Sb1 C2 85.5(5) . . . . ? Sb3 Ni1 Sb1 C2 178.0(5) . . . . ? I1 Ni1 Sb1 C2 -1.4(6) . . . . ? Sb1 Ni1 Sb2 C11 176.7(6) . . . . ? Sb3 Ni1 Sb2 C11 -58.9(6) . . . . ? I1 Ni1 Sb2 C11 58.6(6) . . . . ? Sb1 Ni1 Sb2 C10 -59.4(6) . . . . ? Sb3 Ni1 Sb2 C10 64.9(6) . . . . ? I1 Ni1 Sb2 C10 -177.6(6) . . . . ? Sb1 Ni1 Sb2 C12 57.1(5) . . . . ? Sb3 Ni1 Sb2 C12 -178.6(5) . . . . ? I1 Ni1 Sb2 C12 -61.1(5) . . . . ? Sb2 Ni1 Sb3 C13 -114.3(5) . . . . ? Sb4 Ni1 Sb3 C13 72.5(5) . . . . ? Sb1 Ni1 Sb3 C13 -21.5(5) . . . . ? I1 Ni1 Sb3 C13 157.8(5) . . . . ? Sb2 Ni1 Sb3 C14 10.2(5) . . . . ? Sb4 Ni1 Sb3 C14 -163.1(5) . . . . ? Sb1 Ni1 Sb3 C14 102.9(5) . . . . ? I1 Ni1 Sb3 C14 -77.8(5) . . . . ? Sb2 Ni1 Sb3 C15 128.0(4) . . . . ? Sb4 Ni1 Sb3 C15 -45.2(4) . . . . ? Sb1 Ni1 Sb3 C15 -139.2(4) . . . . ? I1 Ni1 Sb3 C15 40.1(4) . . . . ? Sb1 Ni1 Sb4 C23 -60.2(5) . . . . ? Sb3 Ni1 Sb4 C23 175.5(5) . . . . ? I1 Ni1 Sb4 C23 57.7(5) . . . . ? Sb1 Ni1 Sb4 C22 178.5(4) . . . . ? Sb3 Ni1 Sb4 C22 54.1(4) . . . . ? I1 Ni1 Sb4 C22 -63.7(4) . . . . ? Sb1 Ni1 Sb4 C24 59.1(5) . . . . ? Sb3 Ni1 Sb4 C24 -65.2(5) . . . . ? I1 Ni1 Sb4 C24 176.9(5) . . . . ? Sb8 Ni2 Sb5 C27 -128.4(5) . . . . ? Sb6 Ni2 Sb5 C27 44.7(5) . . . . ? Sb7 Ni2 Sb5 C27 139.8(5) . . . . ? I2 Ni2 Sb5 C27 -40.9(5) . . . . ? Sb8 Ni2 Sb5 C25 114.5(5) . . . . ? Sb6 Ni2 Sb5 C25 -72.4(5) . . . . ? Sb7 Ni2 Sb5 C25 22.7(5) . . . . ? I2 Ni2 Sb5 C25 -158.0(5) . . . . ? Sb8 Ni2 Sb5 C26 -8.0(5) . . . . ? Sb6 Ni2 Sb5 C26 165.1(5) . . . . ? Sb7 Ni2 Sb5 C26 -99.8(5) . . . . ? I2 Ni2 Sb5 C26 79.4(5) . . . . ? Sb7 Ni2 Sb6 C35 59.3(5) . . . . ? Sb5 Ni2 Sb6 C35 -176.3(5) . . . . ? I2 Ni2 Sb6 C35 -57.2(5) . . . . ? Sb7 Ni2 Sb6 C36 -59.7(5) . . . . ? Sb5 Ni2 Sb6 C36 64.7(5) . . . . ? I2 Ni2 Sb6 C36 -176.2(5) . . . . ? Sb7 Ni2 Sb6 C34 -179.1(4) . . . . ? Sb5 Ni2 Sb6 C34 -54.7(4) . . . . ? I2 Ni2 Sb6 C34 64.4(4) . . . . ? Sb8 Ni2 Sb7 C37 -145.7(4) . . . . ? Sb6 Ni2 Sb7 C37 41.5(4) . . . . ? Sb5 Ni2 Sb7 C37 -51.3(4) . . . . ? I2 Ni2 Sb7 C37 129.4(4) . . . . ? Sb8 Ni2 Sb7 C38 89.6(5) . . . . ? Sb6 Ni2 Sb7 C38 -83.3(5) . . . . ? Sb5 Ni2 Sb7 C38 -176.1(5) . . . . ? I2 Ni2 Sb7 C38 4.6(5) . . . . ? Sb8 Ni2 Sb7 C39 -30.5(5) . . . . ? Sb6 Ni2 Sb7 C39 156.6(5) . . . . ? Sb5 Ni2 Sb7 C39 63.8(5) . . . . ? I2 Ni2 Sb7 C39 -115.5(5) . . . . ? Sb7 Ni2 Sb8 C48 -178.0(5) . . . . ? Sb5 Ni2 Sb8 C48 57.7(5) . . . . ? I2 Ni2 Sb8 C48 -61.2(5) . . . . ? Sb7 Ni2 Sb8 C47 -58.6(5) . . . . ? Sb5 Ni2 Sb8 C47 177.1(5) . . . . ? I2 Ni2 Sb8 C47 58.2(5) . . . . ? Sb7 Ni2 Sb8 C46 59.4(5) . . . . ? Sb5 Ni2 Sb8 C46 -64.9(5) . . . . ? I2 Ni2 Sb8 C46 176.3(5) . . . . ? C1 Sb1 C3 C4 -77.1(10) . . . . ? C2 Sb1 C3 C4 179.8(10) . . . . ? Ni1 Sb1 C3 C4 50.8(10) . . . . ? Sb1 C3 C4 C5 86.4(14) . . . . ? Sb1 C3 C4 C9 -90.7(14) . . . . ? C9 C4 C5 C6 -7(2) . . . . ? C3 C4 C5 C6 176.2(13) . . . . ? C4 C5 C6 C7 5(2) . . . . ? C5 C6 C7 C8 -2(2) . . . . ? C6 C7 C8 C9 1(2) . . . . ? C7 C8 C9 C4 -2(2) . . . . ? C7 C8 C9 C10 -175.2(14) . . . . ? C5 C4 C9 C8 5(2) . . . . ? C3 C4 C9 C8 -178.3(13) . . . . ? C5 C4 C9 C10 177.7(14) . . . . ? C3 C4 C9 C10 -5(2) . . . . ? C8 C9 C10 Sb2 -118.1(14) . . . . ? C4 C9 C10 Sb2 68.6(18) . . . . ? C11 Sb2 C10 C9 131.9(12) . . . . ? C12 Sb2 C10 C9 -124.8(12) . . . . ? Ni1 Sb2 C10 C9 0.0(14) . . . . ? C13 Sb3 C15 C16 -46.1(11) . . . . ? C14 Sb3 C15 C16 -147.7(11) . . . . ? Ni1 Sb3 C15 C16 79.9(10) . . . . ? Sb3 C15 C16 C21 -85.1(15) . . . . ? Sb3 C15 C16 C17 100.9(12) . . . . ? C21 C16 C17 C18 2(2) . . . . ? C15 C16 C17 C18 176.0(13) . . . . ? C16 C17 C18 C19 -3(2) . . . . ? C17 C18 C19 C20 4(2) . . . . ? C18 C19 C20 C21 -3(2) . . . . ? C17 C16 C21 C20 -1(2) . . . . ? C15 C16 C21 C20 -175.0(13) . . . . ? C17 C16 C21 C22 -176.2(12) . . . . ? C15 C16 C21 C22 10(2) . . . . ? C19 C20 C21 C16 2(2) . . . . ? C19 C20 C21 C22 177.4(13) . . . . ? C16 C21 C22 Sb4 78.0(16) . . . . ? C20 C21 C22 Sb4 -97.6(12) . . . . ? C23 Sb4 C22 C21 137.4(11) . . . . ? C24 Sb4 C22 C21 33.6(11) . . . . ? Ni1 Sb4 C22 C21 -97.3(10) . . . . ? C25 Sb5 C27 C28 48.0(11) . . . . ? C26 Sb5 C27 C28 149.5(11) . . . . ? Ni2 Sb5 C27 C28 -77.0(11) . . . . ? Sb5 C27 C28 C33 79.0(15) . . . . ? Sb5 C27 C28 C29 -100.6(13) . . . . ? C33 C28 C29 C30 5(2) . . . . ? C27 C28 C29 C30 -175.4(12) . . . . ? C28 C29 C30 C31 -3(2) . . . . ? C29 C30 C31 C32 1(2) . . . . ? C30 C31 C32 C33 -2(2) . . . . ? C31 C32 C33 C28 5(2) . . . . ? C31 C32 C33 C34 -177.1(13) . . . . ? C29 C28 C33 C32 -6(2) . . . . ? C27 C28 C33 C32 174.5(13) . . . . ? C29 C28 C33 C34 175.9(12) . . . . ? C27 C28 C33 C34 -4(2) . . . . ? C32 C33 C34 Sb6 99.4(12) . . . . ? C28 C33 C34 Sb6 -82.3(14) . . . . ? C35 Sb6 C34 C33 -133.3(10) . . . . ? C36 Sb6 C34 C33 -29.9(11) . . . . ? Ni2 Sb6 C34 C33 100.8(10) . . . . ? C37 Sb7 C39 C40 72.6(11) . . . . ? C38 Sb7 C39 C40 174.6(10) . . . . ? Ni2 Sb7 C39 C40 -55.5(11) . . . . ? Sb7 C39 C40 C41 -89.2(14) . . . . ? Sb7 C39 C40 C45 91.6(13) . . . . ? C45 C40 C41 C42 2(2) . . . . ? C39 C40 C41 C42 -176.9(14) . . . . ? C40 C41 C42 C43 -3(2) . . . . ? C41 C42 C43 C44 1(2) . . . . ? C42 C43 C44 C45 3(2) . . . . ? C43 C44 C45 C40 -4(2) . . . . ? C43 C44 C45 C46 173.2(13) . . . . ? C41 C40 C45 C44 1.1(19) . . . . ? C39 C40 C45 C44 -179.7(13) . . . . ? C41 C40 C45 C46 -175.5(13) . . . . ? C39 C40 C45 C46 4(2) . . . . ? C44 C45 C46 Sb8 117.0(12) . . . . ? C40 C45 C46 Sb8 -66.4(17) . . . . ? C48 Sb8 C46 C45 -134.1(12) . . . . ? C47 Sb8 C46 C45 121.9(12) . . . . ? Ni2 Sb8 C46 C45 -3.2(13) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.759 _refine_diff_density_min -1.889 _refine_diff_density_rms 0.268 #===END OF CIF =============================================================== data_ptsb2 _database_code_depnum_ccdc_archive 'CCDC 228296' _audit_creation_method 'SHELXL-97 + hand edit' _chemical_name_systematic ; Dichloro(1,2-bis(dimethylstibanylmethyl)benzene)platinum(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 Cl2 Pt Sb2' _chemical_formula_sum 'C12 H20 Cl2 Pt Sb2' _chemical_formula_weight 673.77 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' Sb Sb -0.5866 1.5461 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 17.654(2) _cell_length_b 10.8090(15) _cell_length_c 17.908(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3417.3(8) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13664 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 11.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67096 # shelxl 0.3900 _exptl_absorpt_correction_T_max 1.78373 # 0.8012 _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6593 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3864 _reflns_number_gt 3357 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0997P)^2^+0.00P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3864 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1626 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.07941(2) 0.75009(3) 0.21064(2) 0.01942(17) Uani 1 1 d . . . Sb1 Sb 0.16330(3) 0.58112(5) 0.16558(3) 0.0212(2) Uani 1 1 d . . . Sb2 Sb 0.07488(3) 0.68746(5) 0.34455(4) 0.01870(19) Uani 1 1 d . . . Cl1 Cl 0.08492(17) 0.8243(2) 0.08632(16) 0.0408(7) Uani 1 1 d . . . Cl2 Cl -0.00794(11) 0.90642(17) 0.24642(13) 0.0233(5) Uani 1 1 d . . . C1 C 0.2267(5) 0.5695(7) 0.3681(5) 0.0218(19) Uani 1 1 d . . . C2 C 0.2596(5) 0.5337(9) 0.2993(5) 0.0201(18) Uani 1 1 d . . . C3 C 0.3348(5) 0.5688(9) 0.2853(6) 0.028(2) Uani 1 1 d . . . H3 H 0.3584 0.5415 0.2405 0.054(8) Uiso 1 1 calc R . . C4 C 0.3764(6) 0.6428(9) 0.3350(7) 0.043(3) Uani 1 1 d . . . H4 H 0.4263 0.6693 0.3232 0.054(8) Uiso 1 1 calc R . . C5 C 0.3429(6) 0.6757(9) 0.4011(7) 0.039(3) Uani 1 1 d . . . H5 H 0.3709 0.7229 0.4363 0.054(8) Uiso 1 1 calc R . . C6 C 0.2685(5) 0.6415(8) 0.4180(6) 0.030(2) Uani 1 1 d . . . H6 H 0.2463 0.6674 0.4637 0.054(8) Uiso 1 1 calc R . . C7 C 0.2175(5) 0.4586(8) 0.2432(5) 0.0223(19) Uani 1 1 d . . . H7A H 0.1791 0.4068 0.2686 0.054(8) Uiso 1 1 calc R . . H7B H 0.2530 0.4032 0.2164 0.054(8) Uiso 1 1 calc R . . C8 C 0.2588(5) 0.6446(9) 0.1048(7) 0.036(2) Uani 1 1 d . . . H8A H 0.2887 0.7005 0.1362 0.054(8) Uiso 1 1 calc R . . H8B H 0.2418 0.6889 0.0601 0.054(8) Uiso 1 1 calc R . . H8C H 0.2900 0.5738 0.0900 0.054(8) Uiso 1 1 calc R . . C9 C 0.1106(6) 0.4655(9) 0.0865(6) 0.037(2) Uani 1 1 d . . . H9A H 0.0647 0.4294 0.1083 0.054(8) Uiso 1 1 calc R . . H9B H 0.1455 0.3992 0.0721 0.054(8) Uiso 1 1 calc R . . H9C H 0.0970 0.5141 0.0423 0.054(8) Uiso 1 1 calc R . . C10 C 0.1457(4) 0.5415(8) 0.3863(5) 0.0214(19) Uani 1 1 d . . . H10A H 0.1394 0.5341 0.4411 0.054(8) Uiso 1 1 calc R . . H10B H 0.1308 0.4619 0.3632 0.054(8) Uiso 1 1 calc R . . C11 C -0.0334(5) 0.6494(8) 0.3903(6) 0.031(2) Uani 1 1 d . . . H11A H -0.0566 0.5804 0.3631 0.054(8) Uiso 1 1 calc R . . H11B H -0.0656 0.7229 0.3857 0.054(8) Uiso 1 1 calc R . . H11C H -0.0281 0.6273 0.4431 0.054(8) Uiso 1 1 calc R . . C12 C 0.1120(6) 0.8365(7) 0.4117(6) 0.027(2) Uani 1 1 d . . . H12A H 0.1625 0.8628 0.3953 0.054(8) Uiso 1 1 calc R . . H12B H 0.1143 0.8099 0.4640 0.054(8) Uiso 1 1 calc R . . H12C H 0.0765 0.9057 0.4069 0.054(8) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0240(3) 0.0118(2) 0.0225(3) 0.00008(13) -0.00215(13) 0.00125(12) Sb1 0.0258(4) 0.0130(3) 0.0247(4) 0.0004(2) 0.0015(2) 0.0014(2) Sb2 0.0184(3) 0.0138(3) 0.0239(4) 0.0016(2) 0.0006(2) -0.0002(2) Cl1 0.081(2) 0.0223(12) 0.0190(13) 0.0035(10) 0.0015(12) 0.0218(12) Cl2 0.0230(11) 0.0155(10) 0.0313(13) -0.0009(9) -0.0014(9) 0.0047(8) C1 0.021(4) 0.013(4) 0.032(5) -0.002(4) -0.008(4) 0.001(3) C2 0.017(4) 0.017(4) 0.026(5) 0.003(4) -0.009(4) 0.002(3) C3 0.018(5) 0.033(5) 0.033(6) 0.018(4) 0.002(4) 0.002(4) C4 0.023(5) 0.028(6) 0.077(10) 0.028(6) -0.009(5) -0.006(5) C5 0.041(6) 0.021(5) 0.054(8) 0.012(5) -0.016(6) 0.006(4) C6 0.037(6) 0.020(4) 0.033(6) 0.001(4) -0.009(5) 0.006(4) C7 0.023(4) 0.018(4) 0.026(5) 0.001(4) -0.006(4) -0.001(4) C8 0.033(5) 0.036(6) 0.040(6) 0.005(5) 0.003(5) 0.000(5) C9 0.052(6) 0.021(5) 0.038(6) -0.007(5) -0.008(6) -0.003(5) C10 0.011(4) 0.023(4) 0.030(5) 0.014(4) -0.001(4) 0.010(3) C11 0.020(5) 0.023(4) 0.050(7) -0.006(5) 0.011(5) -0.004(4) C12 0.041(5) 0.013(4) 0.026(5) 0.006(4) 0.003(5) 0.006(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 Pt1 Cl1 2.368(3) . ? Pt1 Cl2 2.3757(19) . ? Pt1 Sb1 2.4860(7) . ? Pt1 Sb2 2.4931(8) . ? Sb1 C9 2.106(10) . ? Sb1 C8 2.121(10) . ? Sb1 C7 2.146(9) . ? Sb2 C12 2.114(9) . ? Sb2 C11 2.120(8) . ? Sb2 C10 2.148(8) . ? C1 C6 1.395(12) . ? C1 C2 1.416(13) . ? C1 C10 1.498(11) . ? C2 C3 1.404(12) . ? C2 C7 1.490(12) . ? C3 C4 1.406(15) . ? C3 H3 0.9500 . ? C4 C5 1.370(16) . ? C4 H4 0.9500 . ? C5 C6 1.397(14) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 Cl1 Pt1 Cl2 92.26(8) . . ? Cl1 Pt1 Sb1 85.36(6) . . ? Cl2 Pt1 Sb1 175.41(5) . . ? Cl1 Pt1 Sb2 175.93(6) . . ? Cl2 Pt1 Sb2 85.00(6) . . ? Sb1 Pt1 Sb2 97.58(2) . . ? C9 Sb1 C8 101.4(4) . . ? C9 Sb1 C7 105.5(4) . . ? C8 Sb1 C7 100.3(4) . . ? C9 Sb1 Pt1 113.0(3) . . ? C8 Sb1 Pt1 113.7(3) . . ? C7 Sb1 Pt1 120.6(3) . . ? C12 Sb2 C11 102.0(4) . . ? C12 Sb2 C10 100.4(4) . . ? C11 Sb2 C10 104.4(4) . . ? C12 Sb2 Pt1 109.3(3) . . ? C11 Sb2 Pt1 116.9(3) . . ? C10 Sb2 Pt1 121.0(2) . . ? C6 C1 C2 119.6(8) . . ? C6 C1 C10 118.6(9) . . ? C2 C1 C10 121.6(8) . . ? C3 C2 C1 118.0(8) . . ? C3 C2 C7 119.9(9) . . ? C1 C2 C7 122.1(8) . . ? C4 C3 C2 122.4(10) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C5 C4 C3 117.9(10) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C4 C5 C6 121.7(11) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C1 C6 C5 120.3(10) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C2 C7 Sb1 108.8(6) . . ? C2 C7 H7A 109.9 . . ? Sb1 C7 H7A 109.9 . . ? C2 C7 H7B 109.9 . . ? Sb1 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? Sb1 C8 H8A 109.5 . . ? Sb1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Sb1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Sb1 C9 H9A 109.5 . . ? Sb1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Sb1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 Sb2 109.4(5) . . ? C1 C10 H10A 109.8 . . ? Sb2 C10 H10A 109.8 . . ? C1 C10 H10B 109.8 . . ? Sb2 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? Sb2 C11 H11A 109.5 . . ? Sb2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Sb2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Sb2 C12 H12A 109.5 . . ? Sb2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Sb2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pt1 Sb1 C9 -65.4(3) . . . . ? Sb2 Pt1 Sb1 C9 117.4(3) . . . . ? Cl1 Pt1 Sb1 C8 49.5(3) . . . . ? Sb2 Pt1 Sb1 C8 -127.6(3) . . . . ? Cl1 Pt1 Sb1 C7 168.6(3) . . . . ? Sb2 Pt1 Sb1 C7 -8.6(3) . . . . ? Cl2 Pt1 Sb2 C12 -60.4(3) . . . . ? Sb1 Pt1 Sb2 C12 123.5(3) . . . . ? Cl2 Pt1 Sb2 C11 54.8(3) . . . . ? Sb1 Pt1 Sb2 C11 -121.4(3) . . . . ? Cl2 Pt1 Sb2 C10 -176.1(3) . . . . ? Sb1 Pt1 Sb2 C10 7.7(3) . . . . ? C6 C1 C2 C3 2.3(13) . . . . ? C10 C1 C2 C3 177.0(7) . . . . ? C6 C1 C2 C7 -179.0(8) . . . . ? C10 C1 C2 C7 -4.4(13) . . . . ? C1 C2 C3 C4 -3.4(13) . . . . ? C7 C2 C3 C4 178.0(8) . . . . ? C2 C3 C4 C5 3.4(14) . . . . ? C3 C4 C5 C6 -2.5(14) . . . . ? C2 C1 C6 C5 -1.5(13) . . . . ? C10 C1 C6 C5 -176.3(8) . . . . ? C4 C5 C6 C1 1.6(14) . . . . ? C3 C2 C7 Sb1 -88.5(8) . . . . ? C1 C2 C7 Sb1 92.9(9) . . . . ? C9 Sb1 C7 C2 177.3(6) . . . . ? C8 Sb1 C7 C2 72.2(7) . . . . ? Pt1 Sb1 C7 C2 -53.3(7) . . . . ? C6 C1 C10 Sb2 87.4(8) . . . . ? C2 C1 C10 Sb2 -87.3(9) . . . . ? C12 Sb2 C10 C1 -65.4(7) . . . . ? C11 Sb2 C10 C1 -170.7(6) . . . . ? Pt1 Sb2 C10 C1 54.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.525 _refine_diff_density_min -2.607 _refine_diff_density_rms 0.393 #===END OF CIF =============================================================== data_ptsb4 _database_code_depnum_ccdc_archive 'CCDC 228297' _audit_creation_method 'SHELXL-97 + hand edit' _chemical_name_systematic ; Bis(1,2-bis(dimethylstibanylmethyl)benzene)platinum(II) bis(hexafluorophosphate) acetonitrile solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 Pt Sb4 2+, 2(F6 P 1-), 2(C2 H3 N)' _chemical_formula_sum 'C28 H46 F12 N2 P2 Pt Sb4' _chemical_formula_weight 1382.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.699(2) _cell_length_b 15.344(2) _cell_length_c 18.052(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.898(4) _cell_angle_gamma 90.00 _cell_volume 4114.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 34010 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 6.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74080 # shelxl 0.4047 _exptl_absorpt_correction_T_max 0.86235 # 0.5264 _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34097 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9343 _reflns_number_gt 5751 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+14.9672P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9343 _refine_ls_number_parameters 413 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.005 _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 Pt1 Pt 0.00056(2) 0.23383(2) 0.24984(2) 0.01714(10) Uani 1 1 d . . . Sb1 Sb 0.17209(4) 0.23953(4) 0.27828(3) 0.01910(15) Uani 1 1 d . . . Sb2 Sb 0.00219(4) 0.06695(4) 0.26534(3) 0.01881(15) Uani 1 1 d . . . Sb3 Sb -0.17119(4) 0.22736(4) 0.21739(3) 0.02079(16) Uani 1 1 d . . . Sb4 Sb -0.00129(4) 0.40137(4) 0.23718(3) 0.01889(15) Uani 1 1 d . . . P1 P 0.00274(18) 0.73378(15) 0.25840(15) 0.0230(5) Uani 1 1 d . . . P2 P 0.75381(19) 0.97878(19) 0.49888(16) 0.0349(7) Uani 1 1 d . . . F1 F 0.0937(4) 0.7235(4) 0.3303(4) 0.0528(18) Uani 1 1 d . . . F2 F 0.0576(4) 0.7786(3) 0.2073(3) 0.0362(14) Uani 1 1 d . . . F3 F 0.0199(4) 0.6410(3) 0.2255(4) 0.0479(16) Uani 1 1 d . . . F4 F -0.0880(4) 0.7433(5) 0.1876(4) 0.058(2) Uani 1 1 d . . . F5 F -0.0519(4) 0.6893(3) 0.3094(3) 0.0427(15) Uani 1 1 d . . . F6 F -0.0142(4) 0.8263(3) 0.2905(3) 0.0409(15) Uani 1 1 d . . . F7 F 0.8095(4) 1.0577(4) 0.5482(4) 0.0567(18) Uani 1 1 d . . . F8 F 0.8182(4) 0.9112(4) 0.5608(3) 0.0482(16) Uani 1 1 d . . . F9 F 0.8203(5) 0.9758(5) 0.4484(4) 0.068(2) Uani 1 1 d . . . F10 F 0.6999(4) 0.8985(4) 0.4487(4) 0.0555(18) Uani 1 1 d . . . F11 F 0.6903(4) 1.0447(4) 0.4375(3) 0.0498(16) Uani 1 1 d . . . F12 F 0.6876(4) 0.9800(4) 0.5492(4) 0.0579(18) Uani 1 1 d . . . C1 C 0.2510(6) 0.2762(6) 0.3936(5) 0.029(2) Uani 1 1 d . . . H1A H 0.2353 0.2392 0.4315 0.043 Uiso 1 1 calc R . . H1B H 0.2390 0.3373 0.4025 0.043 Uiso 1 1 calc R . . H1C H 0.3150 0.2689 0.3998 0.043 Uiso 1 1 calc R . . C2 C 0.2158(6) 0.3263(6) 0.2057(5) 0.030(2) Uani 1 1 d . . . H2A H 0.1825 0.3142 0.1506 0.045 Uiso 1 1 calc R . . H2B H 0.2803 0.3181 0.2152 0.045 Uiso 1 1 calc R . . H2C H 0.2045 0.3866 0.2180 0.045 Uiso 1 1 calc R . . C3 C 0.2457(6) 0.1280(6) 0.2602(5) 0.024(2) Uani 1 1 d U . . H3A H 0.3046 0.1476 0.2574 0.029 Uiso 1 1 calc R . . H3B H 0.2573 0.0885 0.3058 0.029 Uiso 1 1 calc R . . C4 C 0.1974(5) 0.0781(5) 0.1870(5) 0.0204(19) Uani 1 1 d U . . C5 C 0.2103(6) 0.0977(6) 0.1157(5) 0.024(2) Uani 1 1 d U . . H5 H 0.2494 0.1442 0.1137 0.029 Uiso 1 1 calc R . . C6 C 0.1682(7) 0.0519(7) 0.0484(6) 0.037(3) Uani 1 1 d . . . H6 H 0.1779 0.0669 0.0008 0.044 Uiso 1 1 calc R . . C7 C 0.1124(6) -0.0155(6) 0.0507(5) 0.026(2) Uani 1 1 d . . . H7 H 0.0840 -0.0486 0.0048 0.031 Uiso 1 1 calc R . . C8 C 0.0973(6) -0.0353(6) 0.1204(5) 0.024(2) Uani 1 1 d . . . H8 H 0.0581 -0.0820 0.1218 0.029 Uiso 1 1 calc R . . C9 C 0.1384(5) 0.0118(5) 0.1882(5) 0.0181(18) Uani 1 1 d U . . C10 C 0.1149(6) -0.0103(6) 0.2611(5) 0.023(2) Uani 1 1 d . . . H10A H 0.1675 0.0012 0.3082 0.027 Uiso 1 1 calc R . . H10B H 0.0997 -0.0730 0.2607 0.027 Uiso 1 1 calc R . . C11 C -0.0987(6) 0.0052(6) 0.1718(5) 0.032(2) Uani 1 1 d . . . H11A H -0.0934 0.0245 0.1218 0.048 Uiso 1 1 calc R . . H11B H -0.1583 0.0208 0.1742 0.048 Uiso 1 1 calc R . . H11C H -0.0909 -0.0581 0.1765 0.048 Uiso 1 1 calc R . . C12 C -0.0225(6) 0.0160(6) 0.3658(5) 0.030(2) Uani 1 1 d . . . H12A H 0.0211 0.0405 0.4131 0.045 Uiso 1 1 calc R . . H12B H -0.0164 -0.0476 0.3665 0.045 Uiso 1 1 calc R . . H12C H -0.0836 0.0315 0.3642 0.045 Uiso 1 1 calc R . . C13 C -0.2415(6) 0.1947(6) 0.0993(5) 0.037(3) Uani 1 1 d . . . H13A H -0.2229 0.2339 0.0645 0.056 Uiso 1 1 calc R . . H13B H -0.3064 0.2008 0.0894 0.056 Uiso 1 1 calc R . . H13C H -0.2278 0.1344 0.0893 0.056 Uiso 1 1 calc R . . C14 C -0.2205(6) 0.1359(6) 0.2831(6) 0.035(2) Uani 1 1 d . . . H14A H -0.1914 0.1465 0.3392 0.053 Uiso 1 1 calc R . . H14B H -0.2069 0.0766 0.2703 0.053 Uiso 1 1 calc R . . H14C H -0.2858 0.1428 0.2700 0.053 Uiso 1 1 calc R . . C15 C -0.2458(6) 0.3383(6) 0.2359(5) 0.026(2) Uani 1 1 d . . . H15A H -0.2537 0.3806 0.1929 0.031 Uiso 1 1 calc R . . H15B H -0.3063 0.3192 0.2352 0.031 Uiso 1 1 calc R . . C16 C -0.1981(6) 0.3817(6) 0.3128(5) 0.023(2) Uani 1 1 d . . . C17 C -0.2136(6) 0.3561(7) 0.3809(6) 0.038(3) Uani 1 1 d . . . H17 H -0.2529 0.3087 0.3799 0.046 Uiso 1 1 calc R . . C18 C -0.1715(7) 0.3999(8) 0.4510(6) 0.044(3) Uani 1 1 d . . . H18 H -0.1815 0.3817 0.4978 0.052 Uiso 1 1 calc R . . C19 C -0.1165(7) 0.4685(7) 0.4525(6) 0.043(3) Uani 1 1 d . . . H19 H -0.0893 0.4985 0.5004 0.051 Uiso 1 1 calc R . . C20 C -0.0997(6) 0.4949(7) 0.3873(6) 0.034(2) Uani 1 1 d . . . H20 H -0.0617 0.5438 0.3897 0.040 Uiso 1 1 calc R . . C21 C -0.1379(6) 0.4505(6) 0.3157(5) 0.024(2) Uani 1 1 d . . . C22 C -0.1133(6) 0.4753(6) 0.2456(5) 0.023(2) Uani 1 1 d . . . H22A H -0.0981 0.5381 0.2484 0.028 Uiso 1 1 calc R . . H22B H -0.1657 0.4656 0.1979 0.028 Uiso 1 1 calc R . . C23 C 0.1016(6) 0.4625(5) 0.3276(5) 0.024(2) Uani 1 1 d . . . H23A H 0.1001 0.4414 0.3784 0.036 Uiso 1 1 calc R . . H23B H 0.0923 0.5257 0.3245 0.036 Uiso 1 1 calc R . . H23C H 0.1601 0.4488 0.3220 0.036 Uiso 1 1 calc R . . C24 C 0.0140(6) 0.4556(6) 0.1344(5) 0.029(2) Uani 1 1 d . . . H24A H -0.0314 0.4309 0.0883 0.043 Uiso 1 1 calc R . . H24B H 0.0743 0.4421 0.1324 0.043 Uiso 1 1 calc R . . H24C H 0.0064 0.5190 0.1348 0.043 Uiso 1 1 calc R . . N1 N 0.9792(6) 0.2066(6) 0.0647(6) 0.054(3) Uiso 1 1 d D . . N2 N 0.4584(6) 0.8007(6) 0.0675(6) 0.055(3) Uiso 1 1 d D . . C25 C 1.0046(8) 0.2470(8) 0.0256(7) 0.053(3) Uiso 1 1 d D . . C26 C 1.0386(12) 0.3053(11) -0.0264(10) 0.112(6) Uiso 1 1 d D . . C27 C 0.4830(7) 0.7541(7) 0.0306(6) 0.041(3) Uiso 1 1 d D . . C28 C 0.5175(9) 0.6953(8) -0.0189(8) 0.068(4) Uiso 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 Pt1 0.01407(17) 0.01667(17) 0.02060(18) -0.00034(13) 0.00549(13) -0.00089(13) Sb1 0.0133(3) 0.0208(3) 0.0226(3) -0.0009(2) 0.0051(3) -0.0012(2) Sb2 0.0166(3) 0.0189(3) 0.0218(3) 0.0005(2) 0.0075(2) -0.0002(2) Sb3 0.0142(3) 0.0210(4) 0.0258(4) 0.0016(2) 0.0048(3) -0.0015(2) Sb4 0.0186(3) 0.0150(3) 0.0240(3) -0.0009(2) 0.0081(2) -0.0008(2) P1 0.0196(12) 0.0188(12) 0.0309(14) -0.0030(10) 0.0085(10) -0.0002(10) P2 0.0346(15) 0.0426(19) 0.0254(13) 0.0029(11) 0.0068(11) -0.0007(12) F1 0.031(4) 0.084(5) 0.038(4) 0.003(3) 0.004(3) 0.012(3) F2 0.043(4) 0.031(3) 0.041(4) -0.005(3) 0.022(3) -0.008(3) F3 0.065(4) 0.022(3) 0.074(5) -0.007(3) 0.046(4) 0.002(3) F4 0.025(4) 0.114(6) 0.030(4) -0.013(3) 0.000(3) 0.012(3) F5 0.057(4) 0.035(4) 0.048(4) -0.007(3) 0.034(3) -0.017(3) F6 0.058(4) 0.025(3) 0.049(4) 0.000(3) 0.030(3) 0.001(3) F7 0.055(4) 0.056(4) 0.040(4) 0.000(3) -0.010(3) -0.011(3) F8 0.044(4) 0.049(4) 0.041(4) 0.014(3) -0.001(3) 0.000(3) F9 0.061(5) 0.098(6) 0.054(5) 0.014(4) 0.033(4) 0.006(4) F10 0.055(4) 0.048(4) 0.051(4) -0.008(3) -0.001(3) -0.004(3) F11 0.052(4) 0.054(4) 0.030(3) 0.006(3) -0.005(3) 0.001(3) F12 0.052(4) 0.086(5) 0.045(4) -0.002(3) 0.028(3) 0.003(4) C1 0.027(6) 0.026(6) 0.030(5) -0.002(4) 0.004(4) -0.007(4) C2 0.028(6) 0.036(6) 0.032(6) 0.003(4) 0.016(4) -0.001(4) C3 0.014(5) 0.026(5) 0.034(5) 0.000(4) 0.011(4) -0.001(4) C4 0.010(4) 0.020(5) 0.034(5) 0.000(4) 0.010(4) 0.011(3) C5 0.021(5) 0.023(5) 0.035(5) -0.003(4) 0.018(4) 0.002(4) C6 0.041(7) 0.052(7) 0.025(6) 0.002(5) 0.022(5) 0.010(5) C7 0.016(5) 0.039(6) 0.025(5) -0.001(4) 0.011(4) 0.005(4) C8 0.018(5) 0.027(5) 0.029(5) 0.000(4) 0.011(4) 0.005(4) C9 0.010(4) 0.026(5) 0.017(4) 0.001(3) 0.003(3) 0.004(3) C10 0.023(5) 0.022(5) 0.019(5) 0.002(4) 0.001(4) 0.013(4) C11 0.037(6) 0.024(6) 0.029(6) -0.006(4) 0.002(5) -0.003(4) C12 0.032(6) 0.037(6) 0.024(5) -0.002(4) 0.014(4) 0.003(4) C13 0.030(6) 0.037(6) 0.028(6) -0.002(4) -0.014(4) -0.002(5) C14 0.031(6) 0.033(6) 0.044(6) 0.015(5) 0.016(5) 0.002(5) C15 0.011(5) 0.027(5) 0.041(6) 0.007(4) 0.008(4) 0.007(4) C16 0.016(5) 0.033(6) 0.019(5) -0.007(4) 0.006(4) 0.002(4) C17 0.025(6) 0.052(7) 0.041(7) 0.009(5) 0.017(5) 0.004(5) C18 0.036(7) 0.075(9) 0.029(6) 0.015(6) 0.023(5) 0.027(6) C19 0.037(7) 0.061(8) 0.035(6) -0.017(5) 0.016(5) 0.010(6) C20 0.025(6) 0.043(6) 0.027(5) 0.000(5) 0.000(4) 0.019(5) C21 0.023(5) 0.029(5) 0.026(5) -0.001(4) 0.015(4) 0.011(4) C22 0.018(5) 0.023(5) 0.032(5) -0.005(4) 0.012(4) 0.003(4) C23 0.019(5) 0.020(5) 0.034(5) -0.009(4) 0.010(4) -0.005(4) C24 0.032(6) 0.029(6) 0.031(5) 0.004(4) 0.018(4) 0.006(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 Pt1 Sb3 2.5690(8) . ? Pt1 Sb1 2.5742(8) . ? Pt1 Sb2 2.5750(8) . ? Pt1 Sb4 2.5802(8) . ? Sb1 C1 2.124(9) . ? Sb1 C2 2.131(9) . ? Sb1 C3 2.148(8) . ? Sb2 C12 2.123(9) . ? Sb2 C11 2.127(9) . ? Sb2 C10 2.152(8) . ? Sb3 C13 2.119(9) . ? Sb3 C14 2.137(9) . ? Sb3 C15 2.153(8) . ? Sb4 C23 2.108(8) . ? Sb4 C24 2.117(8) . ? Sb4 C22 2.139(8) . ? P1 F4 1.583(6) . ? P1 F6 1.587(6) . ? P1 F1 1.597(6) . ? P1 F3 1.598(6) . ? P1 F5 1.600(6) . ? P1 F2 1.606(6) . ? P2 F12 1.586(6) . ? P2 F7 1.587(6) . ? P2 F11 1.591(6) . ? P2 F9 1.593(7) . ? P2 F10 1.599(6) . ? P2 F8 1.617(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.501(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C9 1.381(11) . ? C4 C5 1.400(11) . ? C5 C6 1.372(12) . ? C5 H5 0.9500 . ? C6 C7 1.364(13) . ? C6 H6 0.9500 . ? C7 C8 1.388(12) . ? C7 H7 0.9500 . ? C8 C9 1.387(11) . ? C8 H8 0.9500 . ? C9 C10 1.515(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.503(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.386(12) . ? C16 C21 1.406(12) . ? C17 C18 1.396(14) . ? C17 H17 0.9500 . ? C18 C19 1.356(15) . ? C18 H18 0.9500 . ? C19 C20 1.349(14) . ? C19 H19 0.9500 . ? C20 C21 1.412(12) . ? C20 H20 0.9500 . ? C21 C22 1.487(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? N1 C25 1.106(11) . ? N2 C27 1.128(11) . ? C25 C26 1.513(14) . ? C27 C28 1.490(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb3 Pt1 Sb1 178.39(3) . . ? Sb3 Pt1 Sb2 87.66(2) . . ? Sb1 Pt1 Sb2 92.25(2) . . ? Sb3 Pt1 Sb4 92.14(2) . . ? Sb1 Pt1 Sb4 87.99(2) . . ? Sb2 Pt1 Sb4 178.82(2) . . ? C1 Sb1 C2 103.6(4) . . ? C1 Sb1 C3 100.9(3) . . ? C2 Sb1 C3 96.2(4) . . ? C1 Sb1 Pt1 116.4(3) . . ? C2 Sb1 Pt1 115.0(3) . . ? C3 Sb1 Pt1 121.5(2) . . ? C12 Sb2 C11 102.6(4) . . ? C12 Sb2 C10 102.0(3) . . ? C11 Sb2 C10 97.8(4) . . ? C12 Sb2 Pt1 117.4(3) . . ? C11 Sb2 Pt1 112.2(3) . . ? C10 Sb2 Pt1 121.5(3) . . ? C13 Sb3 C14 103.8(4) . . ? C13 Sb3 C15 102.2(4) . . ? C14 Sb3 C15 96.9(4) . . ? C13 Sb3 Pt1 113.9(3) . . ? C14 Sb3 Pt1 116.1(3) . . ? C15 Sb3 Pt1 121.2(2) . . ? C23 Sb4 C24 103.2(4) . . ? C23 Sb4 C22 98.6(3) . . ? C24 Sb4 C22 100.6(3) . . ? C23 Sb4 Pt1 113.0(2) . . ? C24 Sb4 Pt1 117.9(2) . . ? C22 Sb4 Pt1 120.5(2) . . ? F4 P1 F6 89.9(3) . . ? F4 P1 F1 179.4(4) . . ? F6 P1 F1 90.2(3) . . ? F4 P1 F3 89.9(3) . . ? F6 P1 F3 179.5(4) . . ? F1 P1 F3 90.0(3) . . ? F4 P1 F5 89.7(4) . . ? F6 P1 F5 89.3(3) . . ? F1 P1 F5 89.7(3) . . ? F3 P1 F5 91.1(3) . . ? F4 P1 F2 90.4(4) . . ? F6 P1 F2 90.6(3) . . ? F1 P1 F2 90.2(3) . . ? F3 P1 F2 88.9(3) . . ? F5 P1 F2 179.9(4) . . ? F12 P2 F7 90.8(4) . . ? F12 P2 F11 90.8(4) . . ? F7 P2 F11 90.7(3) . . ? F12 P2 F9 179.0(4) . . ? F7 P2 F9 90.0(4) . . ? F11 P2 F9 89.9(4) . . ? F12 P2 F10 90.5(4) . . ? F7 P2 F10 178.6(4) . . ? F11 P2 F10 89.8(3) . . ? F9 P2 F10 88.7(4) . . ? F12 P2 F8 89.5(3) . . ? F7 P2 F8 89.7(3) . . ? F11 P2 F8 179.5(4) . . ? F9 P2 F8 89.9(4) . . ? F10 P2 F8 89.7(3) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Sb1 113.3(5) . . ? C4 C3 H3A 108.9 . . ? Sb1 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? Sb1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C9 C4 C5 118.0(8) . . ? C9 C4 C3 120.8(8) . . ? C5 C4 C3 121.2(8) . . ? C6 C5 C4 122.2(9) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C7 C6 C5 119.4(9) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 119.5(9) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 121.2(9) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C4 C9 C8 119.6(8) . . ? C4 C9 C10 122.1(8) . . ? C8 C9 C10 118.3(8) . . ? C9 C10 Sb2 110.0(5) . . ? C9 C10 H10A 109.7 . . ? Sb2 C10 H10A 109.7 . . ? C9 C10 H10B 109.7 . . ? Sb2 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? Sb2 C11 H11A 109.5 . . ? Sb2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Sb2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Sb2 C12 H12A 109.5 . . ? Sb2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Sb2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Sb3 C13 H13A 109.5 . . ? Sb3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Sb3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Sb3 C14 H14A 109.5 . . ? Sb3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Sb3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 Sb3 111.1(5) . . ? C16 C15 H15A 109.4 . . ? Sb3 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? Sb3 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C21 119.3(8) . . ? C17 C16 C15 121.0(9) . . ? C21 C16 C15 119.7(8) . . ? C16 C17 C18 119.9(10) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 120.3(10) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 121.3(10) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 120.5(10) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C16 C21 C20 118.5(9) . . ? C16 C21 C22 121.1(8) . . ? C20 C21 C22 120.4(9) . . ? C21 C22 Sb4 111.8(6) . . ? C21 C22 H22A 109.3 . . ? Sb4 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? Sb4 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? Sb4 C23 H23A 109.5 . . ? Sb4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Sb4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Sb4 C24 H24A 109.5 . . ? Sb4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Sb4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 177.8(15) . . ? N2 C27 C28 177.8(13) . . ? 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 # Sb3 Pt1 Sb1 C1 173.3(9) . . . . ? Sb2 Pt1 Sb1 C1 -100.1(3) . . . . ? Sb4 Pt1 Sb1 C1 78.7(3) . . . . ? Sb2 Pt1 Sb1 C2 138.5(3) . . . . ? Sb4 Pt1 Sb1 C2 -42.7(3) . . . . ? Sb2 Pt1 Sb1 C3 23.3(3) . . . . ? Sb4 Pt1 Sb1 C3 -157.9(3) . . . . ? Sb3 Pt1 Sb2 C12 -72.3(3) . . . . ? Sb1 Pt1 Sb2 C12 109.3(3) . . . . ? Sb3 Pt1 Sb2 C11 46.3(3) . . . . ? Sb1 Pt1 Sb2 C11 -132.1(3) . . . . ? Sb3 Pt1 Sb2 C10 161.3(3) . . . . ? Sb1 Pt1 Sb2 C10 -17.1(3) . . . . ? Sb2 Pt1 Sb3 C13 -82.1(3) . . . . ? Sb4 Pt1 Sb3 C13 99.1(3) . . . . ? Sb2 Pt1 Sb3 C14 38.5(3) . . . . ? Sb4 Pt1 Sb3 C14 -140.4(3) . . . . ? Sb2 Pt1 Sb3 C15 155.4(3) . . . . ? Sb4 Pt1 Sb3 C15 -23.4(3) . . . . ? Sb3 Pt1 Sb4 C23 136.1(3) . . . . ? Sb1 Pt1 Sb4 C23 -45.5(3) . . . . ? Sb3 Pt1 Sb4 C24 -103.5(3) . . . . ? Sb1 Pt1 Sb4 C24 74.9(3) . . . . ? Sb3 Pt1 Sb4 C22 20.0(3) . . . . ? Sb1 Pt1 Sb4 C22 -161.6(3) . . . . ? C1 Sb1 C3 C4 170.7(6) . . . . ? C2 Sb1 C3 C4 -84.1(7) . . . . ? Pt1 Sb1 C3 C4 40.3(7) . . . . ? Sb1 C3 C4 C9 -89.0(8) . . . . ? Sb1 C3 C4 C5 90.7(8) . . . . ? C9 C4 C5 C6 -1.6(12) . . . . ? C3 C4 C5 C6 178.7(8) . . . . ? C4 C5 C6 C7 -0.5(14) . . . . ? C5 C6 C7 C8 1.5(14) . . . . ? C6 C7 C8 C9 -0.4(13) . . . . ? C5 C4 C9 C8 2.8(12) . . . . ? C3 C4 C9 C8 -177.6(7) . . . . ? C5 C4 C9 C10 -175.8(7) . . . . ? C3 C4 C9 C10 3.9(12) . . . . ? C7 C8 C9 C4 -1.8(12) . . . . ? C7 C8 C9 C10 176.8(7) . . . . ? C4 C9 C10 Sb2 88.3(8) . . . . ? C8 C9 C10 Sb2 -90.2(8) . . . . ? C12 Sb2 C10 C9 175.5(6) . . . . ? C11 Sb2 C10 C9 70.7(6) . . . . ? Pt1 Sb2 C10 C9 -51.5(7) . . . . ? C13 Sb3 C15 C16 -170.6(6) . . . . ? C14 Sb3 C15 C16 83.6(7) . . . . ? Pt1 Sb3 C15 C16 -42.6(7) . . . . ? Sb3 C15 C16 C17 -89.2(9) . . . . ? Sb3 C15 C16 C21 92.0(9) . . . . ? C21 C16 C17 C18 1.7(13) . . . . ? C15 C16 C17 C18 -177.1(8) . . . . ? C16 C17 C18 C19 1.1(15) . . . . ? C17 C18 C19 C20 -1.3(15) . . . . ? C18 C19 C20 C21 -1.1(15) . . . . ? C17 C16 C21 C20 -4.0(13) . . . . ? C15 C16 C21 C20 174.8(7) . . . . ? C17 C16 C21 C22 174.8(8) . . . . ? C15 C16 C21 C22 -6.4(12) . . . . ? C19 C20 C21 C16 3.8(13) . . . . ? C19 C20 C21 C22 -175.0(8) . . . . ? C16 C21 C22 Sb4 -87.5(9) . . . . ? C20 C21 C22 Sb4 91.3(8) . . . . ? C23 Sb4 C22 C21 -73.8(7) . . . . ? C24 Sb4 C22 C21 -179.0(6) . . . . ? Pt1 Sb4 C22 C21 49.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.522 _refine_diff_density_min -1.909 _refine_diff_density_rms 0.284 #===END OF CIF =============================================================== data_pdsb4 _database_code_depnum_ccdc_archive 'CCDC 228298' _audit_creation_method 'SHELXL-97 + hand edit' _chemical_name_systematic ; Bis(1,2-bis(dimethylstibanylmethyl)benzene)palladium(II) bishexafluorophosphate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 Pd Sb4 2+, 2(F6 P 1-)' _chemical_formula_sum 'C24 H40 F12 P2 Pd Sb4' _chemical_formula_weight 1211.90 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 21/n' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' 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 10.604(2) _cell_length_b 15.291(3) _cell_length_c 11.692(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.335(15) _cell_angle_gamma 90.00 _cell_volume 1828.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16171 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 3.564 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73231 # shelxl 0.5359 _exptl_absorpt_correction_T_max 0.81173 # 0.7636 _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13620 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4159 _reflns_number_gt 3480 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+7.4200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00119(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4159 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Pd1 Pd 0.0000 0.0000 0.5000 0.01250(14) Uani 1 2 d S . . Sb1 Sb 0.08253(3) 0.093594(19) 0.35152(3) 0.01320(11) Uani 1 1 d . . . Sb2 Sb -0.13389(3) -0.097447(19) 0.33247(3) 0.01461(12) Uani 1 1 d . . . P1 P 0.20334(15) 0.33308(9) 0.05362(13) 0.0226(3) Uani 1 1 d . . . F1 F 0.0803(4) 0.2984(2) -0.0462(3) 0.0408(9) Uani 1 1 d . . . F2 F 0.3287(4) 0.3671(3) 0.1529(3) 0.0452(10) Uani 1 1 d . . . F3 F 0.2006(6) 0.2493(4) 0.1291(5) 0.109(3) Uani 1 1 d . . . F4 F 0.1115(5) 0.3776(5) 0.1211(6) 0.113(3) Uani 1 1 d . . . F5 F 0.2961(5) 0.2852(5) -0.0090(5) 0.104(2) Uani 1 1 d . . . F6 F 0.2063(7) 0.4176(4) -0.0180(6) 0.122(3) Uani 1 1 d . . . C1 C 0.2834(5) 0.1279(4) 0.3964(5) 0.0234(12) Uani 1 1 d . . . H1A H 0.3368 0.0748 0.4152 0.041(4) Uiso 1 1 calc R . . H1B H 0.3030 0.1667 0.4656 0.041(4) Uiso 1 1 calc R . . H1C H 0.3034 0.1579 0.3293 0.041(4) Uiso 1 1 calc R . . C2 C -0.0154(5) 0.2149(3) 0.3142(5) 0.0210(11) Uani 1 1 d . . . H2A H -0.1101 0.2052 0.2924 0.041(4) Uiso 1 1 calc R . . H2B H 0.0094 0.2435 0.2483 0.041(4) Uiso 1 1 calc R . . H2C H 0.0091 0.2524 0.3845 0.041(4) Uiso 1 1 calc R . . C3 C 0.0668(5) 0.0532(3) 0.1725(4) 0.0178(11) Uani 1 1 d . . . H3A H 0.1217 0.0923 0.1383 0.041(4) Uiso 1 1 calc R . . H3B H 0.1027 -0.0066 0.1740 0.041(4) Uiso 1 1 calc R . . C4 C -0.0685(5) 0.0537(3) 0.0932(4) 0.0170(10) Uani 1 1 d . . . C5 C -0.1133(6) 0.1259(3) 0.0204(5) 0.0231(12) Uani 1 1 d . . . H5 H -0.0583 0.1756 0.0259 0.041(4) Uiso 1 1 calc R . . C6 C -0.2358(6) 0.1268(4) -0.0594(5) 0.0291(13) Uani 1 1 d . . . H6 H -0.2630 0.1757 -0.1102 0.041(4) Uiso 1 1 calc R . . C7 C -0.3186(6) 0.0555(4) -0.0645(5) 0.0300(13) Uani 1 1 d . . . H7 H -0.4039 0.0560 -0.1172 0.041(4) Uiso 1 1 calc R . . C8 C -0.2761(5) -0.0158(4) 0.0074(5) 0.0236(12) Uani 1 1 d . . . H8 H -0.3331 -0.0643 0.0030 0.041(4) Uiso 1 1 calc R . . C9 C -0.1528(5) -0.0188(3) 0.0859(4) 0.0168(10) Uani 1 1 d . . . C10 C -0.1066(6) -0.1000(3) 0.1565(5) 0.0203(11) Uani 1 1 d . . . H10A H -0.0124 -0.1083 0.1626 0.041(4) Uiso 1 1 calc R . . H10B H -0.1541 -0.1509 0.1134 0.041(4) Uiso 1 1 calc R . . C11 C -0.1215(6) -0.2355(3) 0.3599(5) 0.0232(12) Uani 1 1 d . . . H11A H -0.0296 -0.2535 0.3809 0.041(4) Uiso 1 1 calc R . . H11B H -0.1688 -0.2653 0.2870 0.041(4) Uiso 1 1 calc R . . H11C H -0.1606 -0.2510 0.4243 0.041(4) Uiso 1 1 calc R . . C12 C -0.3374(5) -0.0696(4) 0.2872(5) 0.0224(11) Uani 1 1 d . . . H12A H -0.3510 -0.0067 0.2731 0.041(4) Uiso 1 1 calc R . . H12B H -0.3738 -0.0875 0.3523 0.041(4) Uiso 1 1 calc R . . H12C H -0.3812 -0.1018 0.2151 0.041(4) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0151(3) 0.0120(3) 0.0109(3) -0.0004(2) 0.0041(2) -0.0026(2) Sb1 0.0155(2) 0.01279(18) 0.01180(19) 0.00032(12) 0.00455(13) -0.00162(12) Sb2 0.0177(2) 0.01375(18) 0.01214(19) -0.00100(12) 0.00355(14) -0.00366(12) P1 0.0237(8) 0.0191(7) 0.0264(7) -0.0033(6) 0.0090(6) -0.0052(6) F1 0.029(2) 0.038(2) 0.049(2) -0.0110(18) -0.0003(17) -0.0065(16) F2 0.037(2) 0.062(3) 0.035(2) -0.0148(19) 0.0066(17) -0.0217(19) F3 0.107(5) 0.086(4) 0.101(4) 0.065(4) -0.033(4) -0.054(4) F4 0.048(3) 0.184(7) 0.108(5) -0.083(5) 0.023(3) 0.017(4) F5 0.034(3) 0.186(6) 0.090(4) -0.091(4) 0.014(3) 0.008(3) F6 0.137(6) 0.075(4) 0.106(5) 0.064(4) -0.048(4) -0.058(4) C1 0.022(3) 0.022(3) 0.027(3) -0.002(2) 0.008(2) -0.001(2) C2 0.024(3) 0.019(3) 0.019(3) 0.000(2) 0.003(2) 0.005(2) C3 0.022(3) 0.019(2) 0.012(2) 0.000(2) 0.004(2) 0.003(2) C4 0.024(3) 0.016(2) 0.012(2) -0.0040(19) 0.007(2) 0.003(2) C5 0.039(4) 0.018(3) 0.015(3) -0.003(2) 0.012(2) 0.006(2) C6 0.040(4) 0.028(3) 0.019(3) 0.001(2) 0.008(3) 0.013(3) C7 0.024(3) 0.047(4) 0.017(3) 0.000(3) 0.004(2) 0.011(3) C8 0.021(3) 0.031(3) 0.018(3) -0.003(2) 0.004(2) 0.000(2) C9 0.019(3) 0.017(2) 0.016(2) 0.000(2) 0.007(2) 0.002(2) C10 0.027(3) 0.021(3) 0.014(3) -0.001(2) 0.008(2) -0.003(2) C11 0.034(3) 0.017(3) 0.018(3) 0.002(2) 0.006(2) -0.003(2) C12 0.015(3) 0.025(3) 0.026(3) 0.004(2) 0.002(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Sb2 2.5693(5) . ? Pd1 Sb2 2.5693(5) 3_556 ? Pd1 Sb1 2.5751(4) 3_556 ? Pd1 Sb1 2.5751(4) . ? Sb1 C2 2.115(5) . ? Sb1 C1 2.120(5) . ? Sb1 C3 2.145(5) . ? Sb2 C12 2.125(5) . ? Sb2 C11 2.133(5) . ? Sb2 C10 2.152(5) . ? P1 F6 1.545(5) . ? P1 F5 1.556(5) . ? P1 F3 1.560(5) . ? P1 F4 1.563(5) . ? P1 F1 1.594(4) . ? P1 F2 1.603(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.488(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.397(7) . ? C4 C9 1.413(7) . ? C5 C6 1.385(9) . ? C5 H5 0.9500 . ? C6 C7 1.392(9) . ? C6 H6 0.9500 . ? C7 C8 1.377(8) . ? C7 H7 0.9500 . ? C8 C9 1.385(8) . ? C8 H8 0.9500 . ? C9 C10 1.500(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 Sb2 Pd1 Sb2 180.0 . 3_556 ? Sb2 Pd1 Sb1 88.502(16) . 3_556 ? Sb2 Pd1 Sb1 91.498(16) 3_556 3_556 ? Sb2 Pd1 Sb1 91.498(16) . . ? Sb2 Pd1 Sb1 88.502(16) 3_556 . ? Sb1 Pd1 Sb1 180.0 3_556 . ? C2 Sb1 C1 103.9(2) . . ? C2 Sb1 C3 98.3(2) . . ? C1 Sb1 C3 97.3(2) . . ? C2 Sb1 Pd1 113.01(15) . . ? C1 Sb1 Pd1 117.95(15) . . ? C3 Sb1 Pd1 123.03(14) . . ? C12 Sb2 C11 104.7(2) . . ? C12 Sb2 C10 98.6(2) . . ? C11 Sb2 C10 96.1(2) . . ? C12 Sb2 Pd1 113.20(15) . . ? C11 Sb2 Pd1 117.36(15) . . ? C10 Sb2 Pd1 123.53(15) . . ? F6 P1 F5 91.9(5) . . ? F6 P1 F3 178.4(4) . . ? F5 P1 F3 89.3(4) . . ? F6 P1 F4 90.8(5) . . ? F5 P1 F4 177.3(4) . . ? F3 P1 F4 88.0(5) . . ? F6 P1 F1 90.7(3) . . ? F5 P1 F1 89.8(2) . . ? F3 P1 F1 90.4(3) . . ? F4 P1 F1 90.9(3) . . ? F6 P1 F2 89.4(3) . . ? F5 P1 F2 89.2(2) . . ? F3 P1 F2 89.6(3) . . ? F4 P1 F2 90.1(3) . . ? F1 P1 F2 179.0(2) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Sb1 114.8(3) . . ? C4 C3 H3A 108.6 . . ? Sb1 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? Sb1 C3 H3B 108.6 . . ? H3A C3 H3B 107.5 . . ? C5 C4 C9 118.4(5) . . ? C5 C4 C3 120.0(5) . . ? C9 C4 C3 121.6(4) . . ? C6 C5 C4 121.7(5) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 119.3(5) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C8 C7 C6 119.5(6) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 122.0(5) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C8 C9 C4 119.0(5) . . ? C8 C9 C10 120.4(5) . . ? C4 C9 C10 120.5(5) . . ? C9 C10 Sb2 113.8(3) . . ? C9 C10 H10A 108.8 . . ? Sb2 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? Sb2 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? Sb2 C11 H11A 109.5 . . ? Sb2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Sb2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Sb2 C12 H12A 109.5 . . ? Sb2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Sb2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sb2 Pd1 Sb1 C2 102.49(16) . . . . ? Sb2 Pd1 Sb1 C2 -77.51(16) 3_556 . . . ? Sb2 Pd1 Sb1 C1 -136.09(17) . . . . ? Sb2 Pd1 Sb1 C1 43.91(17) 3_556 . . . ? Sb2 Pd1 Sb1 C3 -15.05(16) . . . . ? Sb2 Pd1 Sb1 C3 164.95(16) 3_556 . . . ? Sb1 Pd1 Sb2 C12 76.53(16) 3_556 . . . ? Sb1 Pd1 Sb2 C12 -103.47(16) . . . . ? Sb1 Pd1 Sb2 C11 -45.65(17) 3_556 . . . ? Sb1 Pd1 Sb2 C11 134.35(17) . . . . ? Sb1 Pd1 Sb2 C10 -164.82(17) 3_556 . . . ? Sb1 Pd1 Sb2 C10 15.18(17) . . . . ? C2 Sb1 C3 C4 -53.6(4) . . . . ? C1 Sb1 C3 C4 -158.9(4) . . . . ? Pd1 Sb1 C3 C4 70.9(4) . . . . ? Sb1 C3 C4 C5 96.1(5) . . . . ? Sb1 C3 C4 C9 -86.3(5) . . . . ? C9 C4 C5 C6 -1.5(7) . . . . ? C3 C4 C5 C6 176.3(5) . . . . ? C4 C5 C6 C7 2.4(8) . . . . ? C5 C6 C7 C8 -1.9(8) . . . . ? C6 C7 C8 C9 0.4(8) . . . . ? C7 C8 C9 C4 0.6(8) . . . . ? C7 C8 C9 C10 -175.7(5) . . . . ? C5 C4 C9 C8 0.0(7) . . . . ? C3 C4 C9 C8 -177.8(5) . . . . ? C5 C4 C9 C10 176.2(4) . . . . ? C3 C4 C9 C10 -1.5(7) . . . . ? C8 C9 C10 Sb2 -96.3(5) . . . . ? C4 C9 C10 Sb2 87.5(5) . . . . ? C12 Sb2 C10 C9 54.4(4) . . . . ? C11 Sb2 C10 C9 160.3(4) . . . . ? Pd1 Sb2 C10 C9 -70.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.791 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.206 #===END OF CIF ===============================================================