# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1522 data_2a _audit_creation_date 'Thu Mar 11 14:41:45 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1056.86 _chemical_formula_analytical ? _chemical_formula_sum 'C34 H16 Cl12 Co Cr O6 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? _cell_length_a 13.961(3) _cell_length_b 14.297(3) _cell_length_c 10.950(4) _cell_angle_alpha 104.95(2) _cell_angle_beta 112.45(2) _cell_angle_gamma 81.65(2) _cell_volume 1948(1) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.3 _cell_measurement_theta_max 15.0 _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' _exptl_crystal_description 'cubic' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1046.00 _exptl_absorpt_coefficient_mu 1.571 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.909 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.51 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -1 2 -3 1 2 -3 0 2 _diffrn_reflns_number 9316 _reflns_number_total 8945 _reflns_number_gt 4538 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.124 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06770 _diffrn_orient_matrix_UB_12 -0.02848 _diffrn_orient_matrix_UB_13 -0.02290 _diffrn_orient_matrix_UB_21 0.03781 _diffrn_orient_matrix_UB_22 -0.06107 _diffrn_orient_matrix_UB_23 0.02578 _diffrn_orient_matrix_UB_31 0.00323 _diffrn_orient_matrix_UB_32 0.02675 _diffrn_orient_matrix_UB_33 0.09528 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cr' 'Cr' 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Co' 'Co' 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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_calc_flag Co(1) Co 0.17653(6) 0.34949(6) 0.81955(8) 0.0600(3) Uani 1.00 d Cr(1) Cr 0.19508(6) 0.28115(6) 0.31942(8) 0.0386(2) Uani 1.00 d Cl(1) Cl -0.1111(1) 0.3397(1) 0.4588(2) 0.0803(6) Uani 1.00 d Cl(2) Cl -0.3152(1) 0.3006(1) 0.2036(2) 0.0843(6) Uani 1.00 d Cl(3) Cl -0.3061(1) 0.2413(1) -0.0832(2) 0.0781(5) Uani 1.00 d Cl(4) Cl -0.0928(1) 0.2134(1) -0.1219(1) 0.0720(5) Uani 1.00 d Cl(5) Cl 0.2670(1) -0.0326(1) 0.4497(2) 0.0748(6) Uani 1.00 d Cl(6) Cl 0.4607(1) -0.1436(1) 0.3835(1) 0.0714(5) Uani 1.00 d Cl(7) Cl 0.5495(1) -0.0662(1) 0.2128(2) 0.0718(5) Uani 1.00 d Cl(8) Cl 0.4694(1) 0.1338(1) 0.1365(1) 0.0549(4) Uani 1.00 d Cl(9) Cl 0.4774(1) 0.3914(1) 0.7535(1) 0.0596(4) Uani 1.00 d Cl(10) Cl 0.5456(1) 0.5952(1) 0.7680(2) 0.0636(5) Uani 1.00 d Cl(11) Cl 0.4232(1) 0.7045(1) 0.5392(2) 0.0753(6) Uani 1.00 d Cl(12) Cl 0.2375(1) 0.6092(1) 0.2891(1) 0.0667(5) Uani 1.00 d O(1) O 0.0771(2) 0.3126(2) 0.3809(3) 0.047(1) Uani 1.00 d O(2) O 0.0841(2) 0.2537(2) 0.1426(3) 0.0444(10) Uani 1.00 d O(3) O 0.2093(2) 0.1529(2) 0.3548(3) 0.044(1) Uani 1.00 d O(4) O 0.2987(2) 0.2270(2) 0.2396(3) 0.0398(9) Uani 1.00 d O(5) O 0.2988(2) 0.3231(2) 0.4969(3) 0.0422(10) Uani 1.00 d O(6) O 0.2031(2) 0.4109(2) 0.3026(3) 0.0443(10) Uani 1.00 d C(1) C -0.0110(4) 0.2964(3) 0.2824(5) 0.041(1) Uani 1.00 d C(2) C -0.1078(4) 0.3051(4) 0.2985(5) 0.046(2) Uani 1.00 d C(3) C -0.1971(4) 0.2887(4) 0.1856(6) 0.051(2) Uani 1.00 d C(4) C -0.1935(4) 0.2617(4) 0.0546(5) 0.048(2) Uani 1.00 d C(5) C -0.1000(4) 0.2508(3) 0.0370(5) 0.042(1) Uani 1.00 d C(6) C -0.0073(4) 0.2668(3) 0.1495(4) 0.038(1) Uani 1.00 d C(7) C 0.2883(4) 0.1024(3) 0.3326(4) 0.039(1) Uani 1.00 d C(8) C 0.3266(4) 0.0122(4) 0.3665(5) 0.046(2) Uani 1.00 d C(9) C 0.4082(4) -0.0366(3) 0.3343(5) 0.046(1) Uani 1.00 d C(10) C 0.4519(4) 0.0002(3) 0.2613(5) 0.045(1) Uani 1.00 d C(11) C 0.4168(4) 0.0882(3) 0.2265(4) 0.040(1) Uani 1.00 d C(12) C 0.3361(3) 0.1423(3) 0.2647(4) 0.036(1) Uani 1.00 d C(13) C 0.3317(3) 0.4081(3) 0.5124(5) 0.037(1) Uani 1.00 d C(14) C 0.4130(4) 0.4523(3) 0.6247(5) 0.041(1) Uani 1.00 d C(15) C 0.4428(4) 0.5419(4) 0.6312(5) 0.044(1) Uani 1.00 d C(16) C 0.3887(4) 0.5901(3) 0.5263(5) 0.045(2) Uani 1.00 d C(17) C 0.3069(4) 0.5489(3) 0.4165(5) 0.043(1) Uani 1.00 d C(18) C 0.2787(4) 0.4569(3) 0.4054(5) 0.039(1) Uani 1.00 d C(19) C 0.1328(9) 0.4620(6) 0.9439(9) 0.115(4) Uani 1.00 d C(20) C 0.0605(6) 0.4517(6) 0.812(1) 0.112(3) Uani 1.00 d C(21) C 0.1091(8) 0.4601(5) 0.7295(8) 0.101(3) Uani 1.00 d C(22) C 0.2127(7) 0.4768(5) 0.806(1) 0.093(3) Uani 1.00 d C(23) C 0.2271(6) 0.4788(5) 0.9380(9) 0.096(3) Uani 1.00 d C(24) C 0.193(1) 0.2311(8) 0.889(1) 0.174(6) Uani 1.00 d C(25) C 0.1212(9) 0.2176(6) 0.762(1) 0.132(5) Uani 1.00 d C(26) C 0.1634(8) 0.2269(5) 0.6752(7) 0.086(3) Uani 1.00 d C(27) C 0.2635(7) 0.2447(5) 0.7430(9) 0.084(3) Uani 1.00 d C(28) C 0.2871(8) 0.2472(6) 0.878(1) 0.132(4) Uani 1.00 d C(29) C 0.147(1) -0.0156(7) 0.9212(10) 0.123(4) Uani 1.00 d C(30) C 0.046(1) -0.0275(7) 0.827(2) 0.130(5) Uani 1.00 d C(31) C 0.0321(7) -0.0517(7) 0.697(1) 0.111(4) Uani 1.00 d C(32) C 0.1111(9) -0.0646(7) 0.6536(9) 0.110(4) Uani 1.00 d C(33) C 0.2083(7) -0.0551(7) 0.744(1) 0.107(4) Uani 1.00 d C(34) C 0.2272(7) -0.0299(7) 0.878(1) 0.107(3) Uani 1.00 d H(1) H 0.1187 0.4576 1.0244 0.1349 Uiso 1.00 calc H(2) H -0.0129 0.4377 0.7819 0.1329 Uiso 1.00 calc H(3) H 0.0779 0.4539 0.6306 0.1208 Uiso 1.00 calc H(4) H 0.2667 0.4852 0.7721 0.1131 Uiso 1.00 calc H(5) H 0.2922 0.4881 1.0143 0.1181 Uiso 1.00 calc H(6) H 0.1797 0.2265 0.9670 0.1871 Uiso 1.00 calc H(7) H 0.0469 0.2061 0.7350 0.1556 Uiso 1.00 calc H(8) H 0.1273 0.2245 0.5781 0.1050 Uiso 1.00 calc H(9) H 0.3120 0.2565 0.7031 0.1028 Uiso 1.00 calc H(10) H 0.3550 0.2573 0.9520 0.1630 Uiso 1.00 calc H(11) H 0.1630 0.0022 1.0199 0.1440 Uiso 1.00 calc H(12) H -0.0100 -0.0172 0.8645 0.1539 Uiso 1.00 calc H(13) H -0.0397 -0.0593 0.6326 0.1369 Uiso 1.00 calc H(14) H 0.0975 -0.0812 0.5565 0.1312 Uiso 1.00 calc H(15) H 0.2671 -0.0683 0.7120 0.1282 Uiso 1.00 calc H(16) H 0.2989 -0.0216 0.9430 0.1265 Uiso 1.00 calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0731(6) 0.0613(5) 0.0472(4) 0.0130(4) 0.0271(4) 0.0147(4) Cr(1) 0.0340(4) 0.0464(5) 0.0367(4) -0.0004(3) 0.0129(3) 0.0112(4) Cl(1) 0.0638(10) 0.120(1) 0.0569(9) -0.0004(9) 0.0373(8) -0.0033(9) Cl(2) 0.0429(8) 0.109(1) 0.097(1) 0.0010(9) 0.0354(9) 0.000(1) Cl(3) 0.0442(8) 0.100(1) 0.065(1) -0.0022(8) -0.0048(7) 0.0122(9) Cl(4) 0.0664(10) 0.104(1) 0.0357(7) 0.0081(9) 0.0119(7) 0.0150(8) Cl(5) 0.099(1) 0.075(1) 0.070(1) -0.0256(9) 0.0310(9) 0.0347(9) Cl(6) 0.095(1) 0.0418(8) 0.0593(9) -0.0016(8) 0.0005(8) 0.0221(7) Cl(7) 0.0682(10) 0.0621(10) 0.081(1) 0.0238(8) 0.0315(9) 0.0162(8) Cl(8) 0.0565(8) 0.0633(9) 0.0596(8) 0.0038(7) 0.0335(7) 0.0216(7) Cl(9) 0.0541(8) 0.0606(9) 0.0533(8) 0.0021(7) 0.0013(7) 0.0241(7) Cl(10) 0.0498(8) 0.0610(9) 0.0705(10) -0.0129(7) 0.0167(7) -0.0010(7) Cl(11) 0.114(1) 0.0487(9) 0.081(1) -0.0219(9) 0.048(1) 0.0120(8) Cl(12) 0.097(1) 0.0550(9) 0.0555(9) 0.0122(8) 0.0298(8) 0.0299(7) O(1) 0.037(2) 0.065(2) 0.037(2) 0.001(2) 0.016(2) 0.008(2) O(2) 0.041(2) 0.059(2) 0.032(2) 0.004(2) 0.013(1) 0.010(2) O(3) 0.044(2) 0.049(2) 0.045(2) -0.012(2) 0.018(2) 0.012(2) O(4) 0.040(2) 0.042(2) 0.045(2) 0.003(1) 0.020(2) 0.017(2) O(5) 0.041(2) 0.046(2) 0.039(2) -0.004(2) 0.007(1) 0.018(2) O(6) 0.048(2) 0.044(2) 0.039(2) 0.007(2) 0.013(2) 0.016(2) C(1) 0.040(3) 0.041(3) 0.040(3) 0.001(2) 0.016(2) 0.006(2) C(2) 0.045(3) 0.052(3) 0.041(3) 0.005(2) 0.021(2) 0.008(2) C(3) 0.038(3) 0.052(3) 0.063(4) 0.003(2) 0.021(3) 0.008(3) C(4) 0.038(3) 0.044(3) 0.052(3) 0.001(2) 0.009(2) 0.008(2) C(5) 0.048(3) 0.038(3) 0.035(3) 0.005(2) 0.009(2) 0.011(2) C(6) 0.041(3) 0.037(3) 0.036(3) 0.007(2) 0.013(2) 0.013(2) C(7) 0.043(3) 0.043(3) 0.027(2) -0.013(2) 0.008(2) 0.006(2) C(8) 0.055(3) 0.046(3) 0.039(3) -0.015(3) 0.012(2) 0.014(2) C(9) 0.059(3) 0.032(3) 0.038(3) -0.006(2) 0.002(2) 0.013(2) C(10) 0.043(3) 0.041(3) 0.043(3) 0.006(2) 0.010(2) 0.007(2) C(11) 0.043(3) 0.044(3) 0.033(3) -0.003(2) 0.012(2) 0.011(2) C(12) 0.037(3) 0.041(3) 0.030(2) -0.006(2) 0.008(2) 0.010(2) C(13) 0.038(3) 0.039(3) 0.038(3) 0.001(2) 0.016(2) 0.013(2) C(14) 0.040(3) 0.045(3) 0.043(3) 0.007(2) 0.018(2) 0.016(2) C(15) 0.046(3) 0.048(3) 0.041(3) -0.006(2) 0.020(2) 0.003(2) C(16) 0.057(3) 0.036(3) 0.054(3) -0.001(2) 0.034(3) 0.008(2) C(17) 0.058(3) 0.037(3) 0.045(3) 0.007(2) 0.030(3) 0.015(2) C(18) 0.041(3) 0.041(3) 0.038(3) 0.011(2) 0.019(2) 0.012(2) C(19) 0.144(9) 0.105(7) 0.086(6) 0.023(6) 0.067(6) -0.019(5) C(20) 0.075(6) 0.106(7) 0.129(8) 0.030(5) 0.038(6) -0.005(6) C(21) 0.119(7) 0.061(5) 0.086(6) 0.023(5) 0.001(5) 0.020(4) C(22) 0.099(6) 0.059(5) 0.122(7) 0.007(4) 0.039(6) 0.024(5) C(23) 0.081(6) 0.077(5) 0.083(6) 0.007(4) -0.005(5) -0.002(4) C(24) 0.38(2) 0.103(8) 0.117(8) 0.06(1) 0.17(1) 0.070(7) C(25) 0.19(1) 0.078(6) 0.19(1) -0.022(6) 0.14(1) 0.015(7) C(26) 0.135(7) 0.057(4) 0.071(5) 0.001(5) 0.048(5) 0.008(4) C(27) 0.097(6) 0.059(4) 0.119(7) 0.030(4) 0.066(5) 0.036(4) C(28) 0.152(9) 0.083(6) 0.099(7) 0.068(6) -0.002(6) 0.025(5) C(29) 0.21(1) 0.084(6) 0.093(7) -0.040(8) 0.071(8) 0.008(5) C(30) 0.16(1) 0.080(7) 0.21(1) 0.001(7) 0.13(1) 0.028(8) C(31) 0.071(6) 0.092(7) 0.17(1) -0.007(5) 0.029(7) 0.053(7) C(32) 0.114(7) 0.126(8) 0.093(6) -0.033(6) 0.025(6) 0.033(5) C(33) 0.092(7) 0.128(8) 0.129(8) -0.014(6) 0.050(6) 0.049(7) C(34) 0.093(7) 0.108(7) 0.104(7) -0.036(5) -0.004(6) 0.041(6) _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00009|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0039(5) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4538 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0450 _refine_ls_wR_factor_gt 0.0450 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.478 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.39 _refine_diff_density_max 0.36 _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co(1) C(19) 2.008(7) 1_555 1_555 yes Co(1) C(20) 2.010(7) 1_555 1_555 yes Co(1) C(21) 2.006(7) 1_555 1_555 yes Co(1) C(22) 2.014(7) 1_555 1_555 yes Co(1) C(23) 2.011(7) 1_555 1_555 yes Co(1) C(24) 1.981(9) 1_555 1_555 yes Co(1) C(25) 1.998(8) 1_555 1_555 yes Co(1) C(26) 2.012(7) 1_555 1_555 yes Co(1) C(27) 2.006(6) 1_555 1_555 yes Co(1) C(28) 2.000(7) 1_555 1_555 yes Cr(1) O(1) 1.961(3) 1_555 1_555 yes Cr(1) O(2) 1.949(3) 1_555 1_555 yes Cr(1) O(3) 1.937(3) 1_555 1_555 yes Cr(1) O(4) 1.935(3) 1_555 1_555 yes Cr(1) O(5) 1.932(3) 1_555 1_555 yes Cr(1) O(6) 1.933(3) 1_555 1_555 yes Cl(1) C(2) 1.713(5) 1_555 1_555 yes Cl(2) C(3) 1.714(5) 1_555 1_555 yes Cl(3) C(4) 1.712(5) 1_555 1_555 yes Cl(4) C(5) 1.721(5) 1_555 1_555 yes Cl(5) C(8) 1.722(5) 1_555 1_555 yes Cl(6) C(9) 1.722(5) 1_555 1_555 yes Cl(7) C(10) 1.719(5) 1_555 1_555 yes Cl(8) C(11) 1.720(5) 1_555 1_555 yes Cl(9) C(14) 1.730(5) 1_555 1_555 yes Cl(10) C(15) 1.724(5) 1_555 1_555 yes Cl(11) C(16) 1.728(5) 1_555 1_555 yes Cl(12) C(17) 1.724(5) 1_555 1_555 yes O(1) C(1) 1.292(5) 1_555 1_555 yes O(2) C(6) 1.291(5) 1_555 1_555 yes O(3) C(7) 1.296(5) 1_555 1_555 yes O(4) C(12) 1.302(5) 1_555 1_555 yes O(5) C(13) 1.308(5) 1_555 1_555 yes O(6) C(18) 1.314(5) 1_555 1_555 yes C(1) C(2) 1.413(6) 1_555 1_555 yes C(1) C(6) 1.425(6) 1_555 1_555 yes C(2) C(3) 1.377(7) 1_555 1_555 yes C(3) C(4) 1.405(7) 1_555 1_555 yes C(4) C(5) 1.372(7) 1_555 1_555 yes C(5) C(6) 1.403(6) 1_555 1_555 yes C(7) C(8) 1.408(6) 1_555 1_555 yes C(7) C(12) 1.425(6) 1_555 1_555 yes C(8) C(9) 1.363(7) 1_555 1_555 yes C(9) C(10) 1.404(7) 1_555 1_555 yes C(10) C(11) 1.376(6) 1_555 1_555 yes C(11) C(12) 1.408(6) 1_555 1_555 yes C(13) C(14) 1.394(6) 1_555 1_555 yes C(13) C(18) 1.420(6) 1_555 1_555 yes C(14) C(15) 1.380(7) 1_555 1_555 yes C(15) C(16) 1.400(7) 1_555 1_555 yes C(16) C(17) 1.371(7) 1_555 1_555 yes C(17) C(18) 1.389(6) 1_555 1_555 yes C(19) C(20) 1.39(1) 1_555 1_555 yes C(19) C(23) 1.40(1) 1_555 1_555 yes C(20) C(21) 1.36(1) 1_555 1_555 yes C(21) C(22) 1.39(1) 1_555 1_555 yes C(22) C(23) 1.38(1) 1_555 1_555 yes C(24) C(25) 1.35(2) 1_555 1_555 yes C(24) C(28) 1.43(2) 1_555 1_555 yes C(25) C(26) 1.34(1) 1_555 1_555 yes C(26) C(27) 1.334(10) 1_555 1_555 yes C(27) C(28) 1.38(1) 1_555 1_555 yes C(29) C(30) 1.40(1) 1_555 1_555 yes C(29) C(34) 1.35(1) 1_555 1_555 yes C(30) C(31) 1.33(1) 1_555 1_555 yes C(31) C(32) 1.33(1) 1_555 1_555 yes C(32) C(33) 1.34(1) 1_555 1_555 yes C(33) C(34) 1.34(1) 1_555 1_555 yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(19) Co(1) C(20) 40.5(3) 1_555 1_555 1_555 yes C(19) Co(1) C(21) 67.7(4) 1_555 1_555 1_555 yes C(19) Co(1) C(22) 68.2(4) 1_555 1_555 1_555 yes C(19) Co(1) C(23) 40.8(3) 1_555 1_555 1_555 yes C(19) Co(1) C(24) 108.7(4) 1_555 1_555 1_555 yes C(19) Co(1) C(25) 124.1(4) 1_555 1_555 1_555 yes C(19) Co(1) C(26) 158.1(4) 1_555 1_555 1_555 yes C(19) Co(1) C(27) 161.9(4) 1_555 1_555 1_555 yes C(19) Co(1) C(28) 125.7(4) 1_555 1_555 1_555 yes C(20) Co(1) C(21) 39.6(3) 1_555 1_555 1_555 yes C(20) Co(1) C(22) 67.5(4) 1_555 1_555 1_555 yes C(20) Co(1) C(23) 67.5(3) 1_555 1_555 1_555 yes C(20) Co(1) C(24) 125.2(5) 1_555 1_555 1_555 yes C(20) Co(1) C(25) 110.2(4) 1_555 1_555 1_555 yes C(20) Co(1) C(26) 122.8(4) 1_555 1_555 1_555 yes C(20) Co(1) C(27) 155.8(4) 1_555 1_555 1_555 yes C(20) Co(1) C(28) 163.0(5) 1_555 1_555 1_555 yes C(21) Co(1) C(22) 40.3(3) 1_555 1_555 1_555 yes C(21) Co(1) C(23) 67.2(3) 1_555 1_555 1_555 yes C(21) Co(1) C(24) 160.4(6) 1_555 1_555 1_555 yes C(21) Co(1) C(25) 125.0(5) 1_555 1_555 1_555 yes C(21) Co(1) C(26) 108.5(3) 1_555 1_555 1_555 yes C(21) Co(1) C(27) 121.2(4) 1_555 1_555 1_555 yes C(21) Co(1) C(28) 155.9(5) 1_555 1_555 1_555 yes C(22) Co(1) C(23) 40.0(3) 1_555 1_555 1_555 yes C(22) Co(1) C(24) 158.2(6) 1_555 1_555 1_555 yes C(22) Co(1) C(25) 159.7(5) 1_555 1_555 1_555 yes C(22) Co(1) C(26) 123.8(3) 1_555 1_555 1_555 yes C(22) Co(1) C(27) 107.5(3) 1_555 1_555 1_555 yes C(22) Co(1) C(28) 120.9(5) 1_555 1_555 1_555 yes C(23) Co(1) C(24) 123.6(5) 1_555 1_555 1_555 yes C(23) Co(1) C(25) 159.6(5) 1_555 1_555 1_555 yes C(23) Co(1) C(26) 159.6(4) 1_555 1_555 1_555 yes C(23) Co(1) C(27) 124.8(4) 1_555 1_555 1_555 yes C(23) Co(1) C(28) 108.5(4) 1_555 1_555 1_555 yes C(24) Co(1) C(25) 39.7(5) 1_555 1_555 1_555 yes C(24) Co(1) C(26) 67.2(4) 1_555 1_555 1_555 yes C(24) Co(1) C(27) 68.3(4) 1_555 1_555 1_555 yes C(24) Co(1) C(28) 42.0(5) 1_555 1_555 1_555 yes C(25) Co(1) C(26) 39.0(3) 1_555 1_555 1_555 yes C(25) Co(1) C(27) 65.8(3) 1_555 1_555 1_555 yes C(25) Co(1) C(28) 67.4(5) 1_555 1_555 1_555 yes C(26) Co(1) C(27) 38.8(3) 1_555 1_555 1_555 yes C(26) Co(1) C(28) 66.8(3) 1_555 1_555 1_555 yes C(27) Co(1) C(28) 40.2(3) 1_555 1_555 1_555 yes O(1) Cr(1) O(2) 81.9(1) 1_555 1_555 1_555 yes O(1) Cr(1) O(3) 89.6(1) 1_555 1_555 1_555 yes O(1) Cr(1) O(4) 169.0(1) 1_555 1_555 1_555 yes O(1) Cr(1) O(5) 95.1(1) 1_555 1_555 1_555 yes O(1) Cr(1) O(6) 95.4(1) 1_555 1_555 1_555 yes O(2) Cr(1) O(3) 96.6(1) 1_555 1_555 1_555 yes O(2) Cr(1) O(4) 91.1(1) 1_555 1_555 1_555 yes O(2) Cr(1) O(5) 173.6(1) 1_555 1_555 1_555 yes O(2) Cr(1) O(6) 91.3(1) 1_555 1_555 1_555 yes O(3) Cr(1) O(4) 82.7(1) 1_555 1_555 1_555 yes O(3) Cr(1) O(5) 88.9(1) 1_555 1_555 1_555 yes O(3) Cr(1) O(6) 171.1(1) 1_555 1_555 1_555 yes O(4) Cr(1) O(5) 92.6(1) 1_555 1_555 1_555 yes O(4) Cr(1) O(6) 93.3(1) 1_555 1_555 1_555 yes O(5) Cr(1) O(6) 83.3(1) 1_555 1_555 1_555 yes Cr(1) O(1) C(1) 112.6(3) 1_555 1_555 1_555 yes Cr(1) O(2) C(6) 113.1(3) 1_555 1_555 1_555 yes Cr(1) O(3) C(7) 112.2(3) 1_555 1_555 1_555 yes Cr(1) O(4) C(12) 112.0(3) 1_555 1_555 1_555 yes Cr(1) O(5) C(13) 112.0(3) 1_555 1_555 1_555 yes Cr(1) O(6) C(18) 111.9(3) 1_555 1_555 1_555 yes O(1) C(1) C(2) 124.6(4) 1_555 1_555 1_555 yes O(1) C(1) C(6) 116.2(4) 1_555 1_555 1_555 yes C(2) C(1) C(6) 119.2(4) 1_555 1_555 1_555 yes Cl(1) C(2) C(1) 118.8(4) 1_555 1_555 1_555 yes Cl(1) C(2) C(3) 121.7(4) 1_555 1_555 1_555 yes C(1) C(2) C(3) 119.5(4) 1_555 1_555 1_555 yes Cl(2) C(3) C(2) 120.0(4) 1_555 1_555 1_555 yes Cl(2) C(3) C(4) 118.9(4) 1_555 1_555 1_555 yes C(2) C(3) C(4) 121.1(5) 1_555 1_555 1_555 yes Cl(3) C(4) C(3) 119.7(4) 1_555 1_555 1_555 yes Cl(3) C(4) C(5) 120.0(4) 1_555 1_555 1_555 yes C(3) C(4) C(5) 120.2(4) 1_555 1_555 1_555 yes Cl(4) C(5) C(4) 121.2(4) 1_555 1_555 1_555 yes Cl(4) C(5) C(6) 118.4(4) 1_555 1_555 1_555 yes C(4) C(5) C(6) 120.3(4) 1_555 1_555 1_555 yes O(2) C(6) C(1) 116.1(4) 1_555 1_555 1_555 yes O(2) C(6) C(5) 124.4(4) 1_555 1_555 1_555 yes C(1) C(6) C(5) 119.5(4) 1_555 1_555 1_555 yes O(3) C(7) C(8) 125.2(4) 1_555 1_555 1_555 yes O(3) C(7) C(12) 115.6(4) 1_555 1_555 1_555 yes C(8) C(7) C(12) 119.2(4) 1_555 1_555 1_555 yes Cl(5) C(8) C(7) 117.5(4) 1_555 1_555 1_555 yes Cl(5) C(8) C(9) 122.1(4) 1_555 1_555 1_555 yes C(7) C(8) C(9) 120.4(5) 1_555 1_555 1_555 yes Cl(6) C(9) C(8) 120.9(4) 1_555 1_555 1_555 yes Cl(6) C(9) C(10) 118.7(4) 1_555 1_555 1_555 yes C(8) C(9) C(10) 120.4(4) 1_555 1_555 1_555 yes Cl(7) C(10) C(9) 119.6(4) 1_555 1_555 1_555 yes Cl(7) C(10) C(11) 119.5(4) 1_555 1_555 1_555 yes C(9) C(10) C(11) 120.9(5) 1_555 1_555 1_555 yes Cl(8) C(11) C(10) 121.3(4) 1_555 1_555 1_555 yes Cl(8) C(11) C(12) 119.0(4) 1_555 1_555 1_555 yes C(10) C(11) C(12) 119.7(4) 1_555 1_555 1_555 yes O(4) C(12) C(7) 116.0(4) 1_555 1_555 1_555 yes O(4) C(12) C(11) 124.7(4) 1_555 1_555 1_555 yes C(7) C(12) C(11) 119.3(4) 1_555 1_555 1_555 yes O(5) C(13) C(14) 124.7(4) 1_555 1_555 1_555 yes O(5) C(13) C(18) 116.0(4) 1_555 1_555 1_555 yes C(14) C(13) C(18) 119.3(4) 1_555 1_555 1_555 yes Cl(9) C(14) C(13) 118.7(4) 1_555 1_555 1_555 yes Cl(9) C(14) C(15) 120.9(4) 1_555 1_555 1_555 yes C(13) C(14) C(15) 120.5(4) 1_555 1_555 1_555 yes Cl(10) C(15) C(14) 120.5(4) 1_555 1_555 1_555 yes Cl(10) C(15) C(16) 119.7(4) 1_555 1_555 1_555 yes C(14) C(15) C(16) 119.7(5) 1_555 1_555 1_555 yes Cl(11) C(16) C(15) 119.3(4) 1_555 1_555 1_555 yes Cl(11) C(16) C(17) 120.0(4) 1_555 1_555 1_555 yes C(15) C(16) C(17) 120.7(4) 1_555 1_555 1_555 yes Cl(12) C(17) C(16) 121.0(4) 1_555 1_555 1_555 yes Cl(12) C(17) C(18) 118.6(4) 1_555 1_555 1_555 yes C(16) C(17) C(18) 120.4(4) 1_555 1_555 1_555 yes O(6) C(18) C(13) 116.0(4) 1_555 1_555 1_555 yes O(6) C(18) C(17) 124.6(4) 1_555 1_555 1_555 yes C(13) C(18) C(17) 119.4(5) 1_555 1_555 1_555 yes Co(1) C(19) C(20) 69.8(4) 1_555 1_555 1_555 yes Co(1) C(19) C(23) 69.7(4) 1_555 1_555 1_555 yes Co(1) C(19) H(1) 125.0(7) 1_555 1_555 1_555 no C(20) C(19) C(23) 106.4(8) 1_555 1_555 1_555 yes C(20) C(19) H(1) 125(1) 1_555 1_555 1_555 no C(23) C(19) H(1) 127(1) 1_555 1_555 1_555 no Co(1) C(20) C(19) 69.7(4) 1_555 1_555 1_555 yes Co(1) C(20) C(21) 70.1(4) 1_555 1_555 1_555 yes Co(1) C(20) H(2) 124.2(7) 1_555 1_555 1_555 no C(19) C(20) C(21) 108.7(8) 1_555 1_555 1_555 yes C(19) C(20) H(2) 126(1) 1_555 1_555 1_555 no C(21) C(20) H(2) 124(1) 1_555 1_555 1_555 no Co(1) C(21) C(20) 70.3(5) 1_555 1_555 1_555 yes Co(1) C(21) C(22) 70.1(4) 1_555 1_555 1_555 yes Co(1) C(21) H(2) 82.2(4) 1_555 1_555 1_555 no Co(1) C(21) H(3) 124.3(6) 1_555 1_555 1_555 no C(20) C(21) C(22) 109.0(8) 1_555 1_555 1_555 yes C(20) C(21) H(2) 22.9(5) 1_555 1_555 1_555 no C(20) C(21) H(3) 126(1) 1_555 1_555 1_555 no C(22) C(21) H(2) 131.8(7) 1_555 1_555 1_555 no C(22) C(21) H(3) 124(1) 1_555 1_555 1_555 no H(2) C(21) H(3) 104.0(7) 1_555 1_555 1_555 no Co(1) C(22) C(21) 69.5(4) 1_555 1_555 1_555 yes Co(1) C(22) C(23) 69.9(5) 1_555 1_555 1_555 yes Co(1) C(22) H(4) 125.4(5) 1_555 1_555 1_555 no Co(1) C(22) H(5) 81.5(3) 1_555 1_555 1_555 no C(21) C(22) C(23) 107.2(8) 1_555 1_555 1_555 yes C(21) C(22) H(4) 126(1) 1_555 1_555 1_555 no C(21) C(22) H(5) 129.2(7) 1_555 1_555 1_555 no C(23) C(22) H(4) 126(1) 1_555 1_555 1_555 no C(23) C(22) H(5) 22.0(4) 1_555 1_555 1_555 no H(4) C(22) H(5) 104.1(7) 1_555 1_555 1_555 no Co(1) C(23) C(19) 69.5(4) 1_555 1_555 1_555 yes Co(1) C(23) C(22) 70.1(4) 1_555 1_555 1_555 yes Co(1) C(23) H(5) 124.7(6) 1_555 1_555 1_555 no C(19) C(23) C(22) 108.8(7) 1_555 1_555 1_555 yes C(19) C(23) H(5) 125(1) 1_555 1_555 1_555 no C(22) C(23) H(5) 125(1) 1_555 1_555 1_555 no Co(1) C(24) C(25) 70.8(5) 1_555 1_555 1_555 yes Co(1) C(24) C(28) 69.7(5) 1_555 1_555 1_555 yes Co(1) C(24) H(6) 126.6(8) 1_555 1_555 1_555 no Co(1) C(24) H(7) 81.9(5) 1_555 1_555 1_555 no C(25) C(24) C(28) 105.8(8) 1_555 1_555 1_555 yes C(25) C(24) H(6) 124(1) 1_555 1_555 1_555 no C(25) C(24) H(7) 22.2(6) 1_555 1_555 1_555 no C(28) C(24) H(6) 129(1) 1_555 1_555 1_555 no C(28) C(24) H(7) 128.0(8) 1_555 1_555 1_555 no H(6) C(24) H(7) 102(1) 1_555 1_555 1_555 no Co(1) C(25) C(24) 69.5(6) 1_555 1_555 1_555 yes Co(1) C(25) C(26) 71.0(5) 1_555 1_555 1_555 yes Co(1) C(25) H(6) 82.3(4) 1_555 1_555 1_555 no Co(1) C(25) H(7) 123.6(7) 1_555 1_555 1_555 no Co(1) C(25) H(8) 82.2(4) 1_555 1_555 1_555 no C(24) C(25) C(26) 110(1) 1_555 1_555 1_555 yes C(24) C(25) H(6) 22.6(7) 1_555 1_555 1_555 no C(24) C(25) H(7) 126(1) 1_555 1_555 1_555 no C(24) C(25) H(8) 132.4(9) 1_555 1_555 1_555 no C(26) C(25) H(6) 132.9(9) 1_555 1_555 1_555 no C(26) C(25) H(7) 123(1) 1_555 1_555 1_555 no C(26) C(25) H(8) 22.3(5) 1_555 1_555 1_555 no H(6) C(25) H(7) 104.1(8) 1_555 1_555 1_555 no H(6) C(25) H(8) 155.1(6) 1_555 1_555 1_555 no H(7) C(25) H(8) 100.8(9) 1_555 1_555 1_555 no Co(1) C(26) C(25) 69.9(5) 1_555 1_555 1_555 yes Co(1) C(26) C(27) 70.4(4) 1_555 1_555 1_555 yes Co(1) C(26) H(7) 82.3(3) 1_555 1_555 1_555 no Co(1) C(26) H(8) 123.5(5) 1_555 1_555 1_555 no Co(1) C(26) H(9) 82.3(3) 1_555 1_555 1_555 no C(25) C(26) C(27) 108.8(8) 1_555 1_555 1_555 yes C(25) C(26) H(7) 23.8(6) 1_555 1_555 1_555 no C(25) C(26) H(8) 126(1) 1_555 1_555 1_555 no C(25) C(26) H(9) 131.8(8) 1_555 1_555 1_555 no C(27) C(26) H(7) 132.7(6) 1_555 1_555 1_555 no C(27) C(26) H(8) 124.5(9) 1_555 1_555 1_555 no C(27) C(26) H(9) 22.9(4) 1_555 1_555 1_555 no H(7) C(26) H(8) 102.8(7) 1_555 1_555 1_555 no H(7) C(26) H(9) 155.5(4) 1_555 1_555 1_555 no H(8) C(26) H(9) 101.6(6) 1_555 1_555 1_555 no Co(1) C(27) C(26) 70.8(4) 1_555 1_555 1_555 yes Co(1) C(27) C(28) 69.7(4) 1_555 1_555 1_555 yes Co(1) C(27) H(8) 82.6(3) 1_555 1_555 1_555 no Co(1) C(27) H(9) 123.9(5) 1_555 1_555 1_555 no C(26) C(27) C(28) 109.1(8) 1_555 1_555 1_555 yes C(26) C(27) H(8) 23.2(4) 1_555 1_555 1_555 no C(26) C(27) H(9) 125.3(9) 1_555 1_555 1_555 no C(28) C(27) H(8) 132.2(8) 1_555 1_555 1_555 no C(28) C(27) H(9) 125(1) 1_555 1_555 1_555 no H(8) C(27) H(9) 102.1(6) 1_555 1_555 1_555 no Co(1) C(28) C(24) 68.3(5) 1_555 1_555 1_555 yes Co(1) C(28) C(27) 70.2(4) 1_555 1_555 1_555 yes Co(1) C(28) H(10) 126.6(7) 1_555 1_555 1_555 no C(24) C(28) C(27) 106.0(9) 1_555 1_555 1_555 yes C(24) C(28) H(10) 126(1) 1_555 1_555 1_555 no C(27) C(28) H(10) 127(1) 1_555 1_555 1_555 no C(30) C(29) C(34) 119.8(9) 1_555 1_555 1_555 yes C(30) C(29) H(11) 122(1) 1_555 1_555 1_555 no C(30) C(29) H(12) 25.5(7) 1_555 1_555 1_555 no C(30) C(29) H(16) 144.6(9) 1_555 1_555 1_555 no C(34) C(29) H(11) 117(1) 1_555 1_555 1_555 no C(34) C(29) H(12) 145.4(8) 1_555 1_555 1_555 no C(34) C(29) H(16) 24.8(6) 1_555 1_555 1_555 no H(11) C(29) H(12) 96.8(10) 1_555 1_555 1_555 no H(11) C(29) H(16) 93(1) 1_555 1_555 1_555 no H(12) C(29) H(16) 170.1(5) 1_555 1_555 1_555 no C(29) C(30) C(31) 118.0(10) 1_555 1_555 1_555 yes C(29) C(30) H(12) 116(1) 1_555 1_555 1_555 no C(29) C(30) H(13) 144.4(9) 1_555 1_555 1_555 no C(31) C(30) H(12) 125(1) 1_555 1_555 1_555 no C(31) C(30) H(13) 26.4(6) 1_555 1_555 1_555 no H(12) C(30) H(13) 98(1) 1_555 1_555 1_555 no C(30) C(31) C(32) 122.1(10) 1_555 1_555 1_555 yes C(30) C(31) H(12) 23.0(7) 1_555 1_555 1_555 no C(30) C(31) H(13) 116(1) 1_555 1_555 1_555 no C(30) C(31) H(14) 147.3(9) 1_555 1_555 1_555 no C(32) C(31) H(12) 145.1(8) 1_555 1_555 1_555 no C(32) C(31) H(13) 121(1) 1_555 1_555 1_555 no C(32) C(31) H(14) 25.2(5) 1_555 1_555 1_555 no H(12) C(31) H(13) 93.7(8) 1_555 1_555 1_555 no H(12) C(31) H(14) 170.2(5) 1_555 1_555 1_555 no H(13) C(31) H(14) 96.1(9) 1_555 1_555 1_555 no C(31) C(32) C(33) 119.8(9) 1_555 1_555 1_555 yes C(31) C(32) H(13) 24.5(6) 1_555 1_555 1_555 no C(31) C(32) H(14) 119(1) 1_555 1_555 1_555 no C(31) C(32) H(15) 144.7(8) 1_555 1_555 1_555 no C(33) C(32) H(13) 144.3(8) 1_555 1_555 1_555 no C(33) C(32) H(14) 120(1) 1_555 1_555 1_555 no C(33) C(32) H(15) 25.0(5) 1_555 1_555 1_555 no H(13) C(32) H(14) 94.9(7) 1_555 1_555 1_555 no H(13) C(32) H(15) 169.1(5) 1_555 1_555 1_555 no H(14) C(32) H(15) 95.8(8) 1_555 1_555 1_555 no C(32) C(33) C(34) 121.0(9) 1_555 1_555 1_555 yes C(32) C(33) H(14) 24.5(5) 1_555 1_555 1_555 no C(32) C(33) H(15) 119(1) 1_555 1_555 1_555 no C(32) C(33) H(16) 145.7(8) 1_555 1_555 1_555 no C(34) C(33) H(14) 145.5(8) 1_555 1_555 1_555 no C(34) C(33) H(15) 119(1) 1_555 1_555 1_555 no C(34) C(33) H(16) 24.8(5) 1_555 1_555 1_555 no H(14) C(33) H(15) 95.3(8) 1_555 1_555 1_555 no H(14) C(33) H(16) 170.1(5) 1_555 1_555 1_555 no H(15) C(33) H(16) 94.5(7) 1_555 1_555 1_555 no C(29) C(34) C(33) 119.3(9) 1_555 1_555 1_555 yes C(29) C(34) H(11) 25.8(6) 1_555 1_555 1_555 no C(29) C(34) H(15) 144.5(8) 1_555 1_555 1_555 no C(29) C(34) H(16) 120(1) 1_555 1_555 1_555 no C(33) C(34) H(11) 145.1(8) 1_555 1_555 1_555 no C(33) C(34) H(15) 25.2(5) 1_555 1_555 1_555 no C(33) C(34) H(16) 120(1) 1_555 1_555 1_555 no H(11) C(34) H(15) 170.2(4) 1_555 1_555 1_555 no H(11) C(34) H(16) 94.5(8) 1_555 1_555 1_555 no H(15) C(34) H(16) 95.2(8) 1_555 1_555 1_555 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(17) 3.512(5) 1_555 2_566 ? Cl(2) C(15) 3.273(5) 1_555 2_566 ? Cl(2) C(16) 3.422(5) 1_555 2_566 ? Cl(2) Cl(10) 3.434(2) 1_555 2_566 ? Cl(3) Cl(6) 3.242(2) 1_555 2_555 ? Cl(3) C(9) 3.495(5) 1_555 2_555 ? Cl(3) Cl(9) 3.593(2) 1_555 1_454 ? Cl(4) Cl(12) 3.457(2) 1_555 2_565 ? Cl(6) Cl(11) 3.288(2) 1_555 1_545 ? Cl(6) C(9) 3.534(5) 1_555 2_656 ? Cl(6) C(8) 3.550(5) 1_555 2_656 ? Cl(6) Cl(9) 3.592(2) 1_555 2_656 ? Cl(7) C(27) 3.361(7) 1_555 2_656 ? Cl(7) C(28) 3.402(9) 1_555 2_656 ? Cl(8) C(28) 3.579(8) 1_555 1_554 ? Cl(8) Cl(11) 3.592(2) 1_555 2_666 ? Cl(10) C(17) 3.517(5) 1_555 2_666 ? Cl(10) C(18) 3.532(5) 1_555 2_666 ? O(1) C(26) 3.461(8) 1_555 1_555 ? O(2) C(24) 3.56(1) 1_555 1_554 ? O(4) C(24) 3.56(1) 1_555 1_554 ? O(5) C(27) 3.390(8) 1_555 1_555 ? C(1) C(21) 3.566(8) 1_555 2_566 ? C(2) C(21) 3.445(9) 1_555 2_566 ? C(2) C(22) 3.523(9) 1_555 2_566 ? C(3) C(22) 3.307(9) 1_555 2_566 ? C(4) C(29) 3.54(1) 1_555 2_556 ? C(9) C(9) 3.544(9) 1_555 2_656 ? C(15) C(16) 3.493(6) 1_555 2_666 ? _publ_contact_author_name ; Susumu Kitagawa ; _publ_contact_author_address ; Department of Synthetic Chemistry and Biological Chemistry, Faculty of Engineering, Kyoto Universsity, Yoshida, Sakyo-ku, Kyoto 606-8501, Japan ; _publ_contact_author_email 'kitagawa@sbchem.kyoto-u.ac.jp' _publ_contact_author_fax '+81-75-753-4979' _publ_contact_author_phone '+81-75-753-5658' #====END data_3b _audit_creation_date 'Thu Mar 11 14:48:00 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1803.86 _chemical_formula_analytical ? _chemical_formula_sum 'C35 H20 Br12 Cr O6 S8 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? _cell_length_a 14.303(2) _cell_length_b 15.084(3) _cell_length_c 12.907(5) _cell_angle_alpha 109.62(2) _cell_angle_beta 99.31(2) _cell_angle_gamma 91.86(2) _cell_volume 2577(1) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.6 _cell_measurement_theta_max 15.0 _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' _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.324 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_F_000 1700.00 _exptl_absorpt_coefficient_mu 9.919 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.140 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.69 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -4 0 -2 -3 0 -1 -3 1 _diffrn_reflns_number 10193 _reflns_number_total 9815 _reflns_number_gt 3658 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.053 _diffrn_reflns_av_sigmaI/netI 0.157 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03886 _diffrn_orient_matrix_UB_12 -0.00697 _diffrn_orient_matrix_UB_13 0.05509 _diffrn_orient_matrix_UB_21 -0.05864 _diffrn_orient_matrix_UB_22 0.00933 _diffrn_orient_matrix_UB_23 -0.04762 _diffrn_orient_matrix_UB_31 -0.01069 _diffrn_orient_matrix_UB_32 -0.06973 _diffrn_orient_matrix_UB_33 -0.04121 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cr' 'Cr' 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 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_calc_flag Br(1) Br 1.0358(2) 0.2668(2) -0.0221(2) 0.0734(9) Uani 1.00 d Br(2) Br 1.2172(2) 0.2350(2) 0.1544(3) 0.092(1) Uani 1.00 d Br(3) Br 1.1807(2) 0.2198(2) 0.3940(3) 0.091(1) Uani 1.00 d Br(4) Br 0.9670(2) 0.2545(2) 0.4622(2) 0.0744(9) Uani 1.00 d Br(5) Br 0.6781(1) -0.0536(1) 0.0269(2) 0.0594(8) Uani 1.00 d Br(6) Br 0.4950(1) -0.1059(1) 0.1322(2) 0.0671(9) Uani 1.00 d Br(7) Br 0.3880(1) 0.0662(2) 0.2870(2) 0.0660(9) Uani 1.00 d Br(8) Br 0.4633(1) 0.2897(2) 0.3346(2) 0.0660(8) Uani 1.00 d Br(9) Br 0.5477(2) 0.3454(2) -0.1868(2) 0.0807(10) Uani 1.00 d Br(10) Br 0.5517(2) 0.5772(2) -0.1429(3) 0.089(1) Uani 1.00 d Br(11) Br 0.6813(2) 0.7274(2) 0.0857(3) 0.095(1) Uani 1.00 d Br(12) Br 0.7925(2) 0.6494(2) 0.2810(3) 0.094(1) Uani 1.00 d Cr(1) Cr 0.7437(2) 0.2966(2) 0.1472(3) 0.045(1) Uani 1.00 d S(1) S 1.0549(3) -0.0159(4) 0.8488(5) 0.051(2) Uani 1.00 d S(2) S 0.8775(3) 0.0461(4) 0.9161(5) 0.055(2) Uani 1.00 d S(3) S 1.0112(4) 0.0163(4) 0.6316(5) 0.063(2) Uani 1.00 d S(4) S 0.8073(4) 0.0869(5) 0.7065(5) 0.069(2) Uani 1.00 d S(5) S 1.0250(4) -0.4981(4) 0.3379(6) 0.077(2) Uani 1.00 d S(6) S 1.1514(4) -0.5093(4) 0.5315(6) 0.078(2) Uani 1.00 d S(7) S 1.1822(6) -0.4959(6) 0.2107(7) 0.114(4) Uani 1.00 d S(8) S 1.3275(5) -0.5087(5) 0.4323(7) 0.107(3) Uani 1.00 d O(1) O 0.8549(8) 0.2865(8) 0.080(1) 0.054(5) Uani 1.00 d O(2) O 0.8297(8) 0.2881(8) 0.274(1) 0.053(5) Uani 1.00 d O(3) O 0.7119(8) 0.1592(8) 0.092(1) 0.043(4) Uani 1.00 d O(4) O 0.6335(8) 0.2953(8) 0.219(1) 0.048(5) Uani 1.00 d O(5) O 0.6664(8) 0.3148(9) 0.015(1) 0.049(5) Uani 1.00 d O(6) O 0.7589(8) 0.4337(8) 0.197(1) 0.048(5) Uani 1.00 d C(1) C 0.931(1) 0.274(1) 0.148(2) 0.047(7) Uani 1.00 d C(2) C 1.021(1) 0.260(1) 0.117(2) 0.061(8) Uani 1.00 d C(3) C 1.097(1) 0.247(1) 0.192(2) 0.063(9) Uani 1.00 d C(4) C 1.080(1) 0.243(1) 0.291(2) 0.059(8) Uani 1.00 d C(5) C 0.992(2) 0.258(1) 0.324(2) 0.061(8) Uani 1.00 d C(6) C 0.916(1) 0.273(1) 0.252(2) 0.035(6) Uani 1.00 d C(7) C 0.645(1) 0.135(1) 0.135(2) 0.048(7) Uani 1.00 d C(8) C 0.613(1) 0.041(1) 0.116(2) 0.042(7) Uani 1.00 d C(9) C 0.540(1) 0.021(1) 0.160(2) 0.050(7) Uani 1.00 d C(10) C 0.491(1) 0.095(1) 0.224(2) 0.043(7) Uani 1.00 d C(11) C 0.524(1) 0.187(1) 0.249(2) 0.047(7) Uani 1.00 d C(12) C 0.600(1) 0.211(2) 0.200(2) 0.051(8) Uani 1.00 d C(13) C 0.667(1) 0.401(2) 0.024(2) 0.045(7) Uani 1.00 d C(14) C 0.618(1) 0.437(1) -0.056(2) 0.054(8) Uani 1.00 d C(15) C 0.621(1) 0.532(2) -0.037(2) 0.067(9) Uani 1.00 d C(16) C 0.675(1) 0.598(1) 0.064(2) 0.052(8) Uani 1.00 d C(17) C 0.722(1) 0.568(1) 0.146(2) 0.051(7) Uani 1.00 d C(18) C 0.718(1) 0.470(1) 0.130(2) 0.049(8) Uani 1.00 d C(19) C 0.986(1) 0.004(1) 0.949(2) 0.044(7) Uani 1.00 d C(20) C 0.977(1) 0.019(1) 0.756(2) 0.039(7) Uani 1.00 d C(21) C 0.897(1) 0.051(1) 0.789(2) 0.049(7) Uani 1.00 d C(22) C 1.057(2) 0.136(2) 0.669(2) 0.09(1) Uani 1.00 d C(23) C 0.748(1) 0.167(1) 0.812(2) 0.065(8) Uani 1.00 d C(24) C 1.037(1) -0.502(1) 0.469(2) 0.073(10) Uani 1.00 d C(25) C 1.147(2) -0.498(2) 0.332(2) 0.075(10) Uani 1.00 d C(26) C 1.206(2) -0.507(2) 0.426(2) 0.071(9) Uani 1.00 d C(27) C 1.140(4) -0.393(4) 0.199(6) 0.38(4) Uani 1.00 d C(28) C 1.367(2) -0.518(2) 0.569(2) 0.10(1) Uani 1.00 d C(29) C 0.698(2) -0.067(1) 0.373(2) 0.1469 Uiso 1.00 d C(30) C 0.732(1) 0.108(1) 0.404(1) 0.1469 Uiso 1.00 d C(31) C 0.6813(9) 0.038(1) 0.426(1) 0.1469 Uiso 1.00 d C(32) C 0.717(1) 0.202(1) 0.452(2) 0.1469 Uiso 1.00 d C(33) C 0.651(1) 0.227(1) 0.523(2) 0.1469 Uiso 1.00 d C(34) C 0.600(1) 0.158(1) 0.545(2) 0.1469 Uiso 1.00 d C(35) C 0.615(1) 0.063(1) 0.497(1) 0.1469 Uiso 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.067(2) 0.085(2) 0.060(2) -0.001(1) 0.018(1) 0.013(2) Br(2) 0.050(1) 0.094(2) 0.111(3) 0.018(1) 0.012(1) 0.009(2) Br(3) 0.078(2) 0.078(2) 0.093(3) 0.024(1) -0.025(1) 0.017(2) Br(4) 0.102(2) 0.064(2) 0.058(2) 0.012(1) -0.002(1) 0.029(2) Br(5) 0.065(1) 0.038(1) 0.073(2) 0.013(1) 0.017(1) 0.013(1) Br(6) 0.066(1) 0.045(1) 0.095(2) 0.005(1) 0.015(1) 0.030(1) Br(7) 0.058(1) 0.070(2) 0.079(2) 0.009(1) 0.022(1) 0.033(2) Br(8) 0.065(1) 0.056(1) 0.078(2) 0.021(1) 0.028(1) 0.018(1) Br(9) 0.082(2) 0.088(2) 0.067(2) 0.019(1) -0.007(1) 0.028(2) Br(10) 0.103(2) 0.104(2) 0.094(3) 0.049(2) 0.024(2) 0.070(2) Br(11) 0.128(2) 0.054(2) 0.126(3) 0.030(1) 0.041(2) 0.053(2) Br(12) 0.129(2) 0.041(1) 0.098(3) -0.004(1) -0.008(2) 0.019(2) Cr(1) 0.049(2) 0.036(2) 0.050(3) 0.010(1) 0.008(2) 0.016(2) S(1) 0.062(3) 0.058(4) 0.035(4) 0.014(3) 0.010(3) 0.017(3) S(2) 0.054(3) 0.070(4) 0.050(4) 0.013(3) 0.013(3) 0.031(3) S(3) 0.087(4) 0.070(4) 0.035(4) 0.002(3) 0.013(3) 0.023(4) S(4) 0.066(4) 0.098(5) 0.050(5) 0.014(3) 0.001(3) 0.039(4) S(5) 0.099(5) 0.062(4) 0.069(6) 0.009(3) 0.025(4) 0.019(4) S(6) 0.089(5) 0.073(5) 0.071(6) 0.011(3) 0.022(4) 0.020(4) S(7) 0.157(7) 0.113(7) 0.091(7) 0.018(5) 0.062(6) 0.040(6) S(8) 0.083(5) 0.110(6) 0.121(8) 0.013(4) 0.044(5) 0.020(6) O(1) 0.033(7) 0.054(9) 0.05(1) 0.002(6) 0.001(7) -0.005(8) O(2) 0.054(8) 0.050(9) 0.06(1) 0.015(7) 0.014(7) 0.021(8) O(3) 0.042(7) 0.042(8) 0.05(1) 0.002(6) 0.015(7) 0.016(7) O(4) 0.044(8) 0.032(8) 0.06(1) 0.004(6) 0.011(7) 0.009(8) O(5) 0.053(8) 0.033(8) 0.06(1) 0.007(6) 0.000(7) 0.020(8) O(6) 0.065(9) 0.027(8) 0.05(1) 0.010(6) 0.007(7) 0.017(8) C(1) 0.05(1) 0.04(1) 0.04(2) -0.002(9) 0.00(1) 0.00(1) C(2) 0.04(1) 0.06(2) 0.07(2) 0.00(1) 0.01(1) 0.01(1) C(3) 0.05(1) 0.03(1) 0.09(2) 0.000(10) 0.01(1) 0.00(2) C(4) 0.05(1) 0.05(1) 0.07(2) 0.01(1) -0.01(1) 0.02(1) C(5) 0.07(2) 0.03(1) 0.06(2) 0.02(1) -0.01(1) 0.01(1) C(6) 0.05(1) 0.02(1) 0.03(2) 0.006(9) 0.01(1) 0.01(1) C(7) 0.05(1) 0.05(1) 0.03(2) 0.01(1) 0.00(1) 0.01(1) C(8) 0.05(1) 0.04(1) 0.03(1) 0.009(10) 0.005(10) 0.01(1) C(9) 0.05(1) 0.04(1) 0.06(2) 0.010(10) 0.00(1) 0.01(1) C(10) 0.04(1) 0.05(1) 0.05(2) 0.002(9) 0.003(10) 0.03(1) C(11) 0.05(1) 0.03(1) 0.06(2) 0.011(9) 0.00(1) 0.01(1) C(12) 0.03(1) 0.08(2) 0.04(2) 0.01(1) 0.00(1) 0.03(1) C(13) 0.03(1) 0.06(2) 0.04(2) 0.00(1) 0.01(1) 0.02(1) C(14) 0.04(1) 0.06(2) 0.07(2) 0.02(1) 0.02(1) 0.04(1) C(15) 0.07(2) 0.07(2) 0.10(2) 0.03(1) 0.04(1) 0.06(2) C(16) 0.06(1) 0.04(1) 0.06(2) 0.02(1) 0.03(1) 0.02(1) C(17) 0.06(1) 0.04(1) 0.06(2) 0.02(1) 0.01(1) 0.03(1) C(18) 0.05(1) 0.03(1) 0.07(2) 0.003(10) 0.02(1) 0.02(1) C(19) 0.04(1) 0.05(1) 0.04(2) 0.005(9) 0.00(1) 0.03(1) C(20) 0.06(1) 0.05(1) 0.01(1) 0.002(10) 0.004(10) 0.02(1) C(21) 0.06(1) 0.05(1) 0.04(2) -0.01(1) -0.01(1) 0.03(1) C(22) 0.14(2) 0.08(2) 0.07(2) -0.01(2) 0.05(2) 0.04(2) C(23) 0.07(1) 0.07(2) 0.06(2) 0.03(1) 0.01(1) 0.03(1) C(24) 0.09(2) 0.03(1) 0.09(2) 0.00(1) 0.01(1) 0.01(1) C(25) 0.10(2) 0.05(2) 0.08(2) 0.00(1) 0.05(2) 0.01(2) C(26) 0.12(2) 0.05(2) 0.04(2) 0.00(1) 0.03(2) 0.00(1) C(27) 0.49(7) 0.34(6) 0.7(1) 0.31(6) 0.44(8) 0.47(8) C(28) 0.09(2) 0.16(3) 0.06(2) 0.02(2) 0.00(1) 0.04(2) _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00009|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3658 _refine_ls_number_parameters 503 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.239 _refine_ls_shift/su_max 0.0030 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.97 _refine_diff_density_max 0.98 _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) C(2) 1.88(3) 1_555 1_555 yes Br(2) C(3) 1.86(2) 1_555 1_555 yes Br(3) C(4) 1.92(2) 1_555 1_555 yes Br(4) C(5) 1.89(3) 1_555 1_555 yes Br(5) C(8) 1.88(2) 1_555 1_555 yes Br(6) C(9) 1.90(2) 1_555 1_555 yes Br(7) C(10) 1.90(2) 1_555 1_555 yes Br(8) C(11) 1.91(2) 1_555 1_555 yes Br(9) C(14) 1.88(2) 1_555 1_555 yes Br(10) C(15) 1.89(3) 1_555 1_555 yes Br(11) C(16) 1.87(2) 1_555 1_555 yes Br(12) C(17) 1.86(2) 1_555 1_555 yes Cr(1) O(1) 1.92(1) 1_555 1_555 yes Cr(1) O(2) 1.92(1) 1_555 1_555 yes Cr(1) O(3) 1.96(1) 1_555 1_555 yes Cr(1) O(4) 1.96(1) 1_555 1_555 yes Cr(1) O(5) 1.98(1) 1_555 1_555 yes Cr(1) O(6) 1.94(1) 1_555 1_555 yes S(1) C(19) 1.70(2) 1_555 1_555 yes S(1) C(20) 1.72(2) 1_555 1_555 yes S(2) C(19) 1.73(2) 1_555 1_555 yes S(2) C(21) 1.74(3) 1_555 1_555 yes S(3) C(20) 1.75(2) 1_555 1_555 yes S(3) C(22) 1.78(2) 1_555 1_555 yes S(4) C(21) 1.75(2) 1_555 1_555 yes S(4) C(23) 1.84(2) 1_555 1_555 yes S(5) C(24) 1.70(3) 1_555 1_555 yes S(5) C(25) 1.76(3) 1_555 1_555 yes S(6) C(24) 1.73(2) 1_555 1_555 yes S(6) C(26) 1.68(3) 1_555 1_555 yes S(7) C(25) 1.73(3) 1_555 1_555 yes S(7) C(27) 1.73(6) 1_555 1_555 yes S(8) C(26) 1.73(3) 1_555 1_555 yes S(8) C(28) 1.82(3) 1_555 1_555 yes O(1) C(1) 1.34(2) 1_555 1_555 yes O(2) C(6) 1.33(2) 1_555 1_555 yes O(3) C(7) 1.28(3) 1_555 1_555 yes O(4) C(12) 1.27(3) 1_555 1_555 yes O(5) C(13) 1.27(3) 1_555 1_555 yes O(6) C(18) 1.25(3) 1_555 1_555 yes C(1) C(2) 1.41(3) 1_555 1_555 yes C(1) C(6) 1.40(3) 1_555 1_555 yes C(2) C(3) 1.40(3) 1_555 1_555 yes C(3) C(4) 1.36(4) 1_555 1_555 yes C(4) C(5) 1.40(3) 1_555 1_555 yes C(5) C(6) 1.39(3) 1_555 1_555 yes C(7) C(8) 1.41(3) 1_555 1_555 yes C(7) C(12) 1.42(3) 1_555 1_555 yes C(8) C(9) 1.34(3) 1_555 1_555 yes C(9) C(10) 1.43(3) 1_555 1_555 yes C(10) C(11) 1.36(3) 1_555 1_555 yes C(11) C(12) 1.44(3) 1_555 1_555 yes C(13) C(14) 1.42(3) 1_555 1_555 yes C(13) C(18) 1.47(3) 1_555 1_555 yes C(14) C(15) 1.37(3) 1_555 1_555 yes C(15) C(16) 1.42(3) 1_555 1_555 yes C(16) C(17) 1.39(4) 1_555 1_555 yes C(17) C(18) 1.42(3) 1_555 1_555 yes C(19) C(19) 1.38(4) 1_555 2_757 yes C(20) C(21) 1.33(3) 1_555 1_555 yes C(24) C(24) 1.42(5) 1_555 2_746 yes C(25) C(26) 1.42(4) 1_555 1_555 yes C(31) C(30) 1.39(3) 1_555 1_555 yes C(31) C(35) 1.39(2) 1_555 1_555 yes C(31) C(36) 1.54(2) 1_555 1_555 yes C(30) C(32) 1.39(2) 1_555 1_555 yes C(32) C(33) 1.39(3) 1_555 1_555 yes C(33) C(34) 1.39(3) 1_555 1_555 yes C(34) C(35) 1.39(3) 1_555 1_555 yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Cr(1) O(2) 84.3(6) 1_555 1_555 1_555 yes O(1) Cr(1) O(3) 93.0(5) 1_555 1_555 1_555 yes O(1) Cr(1) O(4) 174.2(6) 1_555 1_555 1_555 yes O(1) Cr(1) O(5) 90.9(6) 1_555 1_555 1_555 yes O(1) Cr(1) O(6) 92.1(6) 1_555 1_555 1_555 yes O(2) Cr(1) O(3) 90.2(5) 1_555 1_555 1_555 yes O(2) Cr(1) O(4) 92.3(6) 1_555 1_555 1_555 yes O(2) Cr(1) O(5) 173.6(6) 1_555 1_555 1_555 yes O(2) Cr(1) O(6) 94.9(5) 1_555 1_555 1_555 yes O(3) Cr(1) O(4) 82.3(5) 1_555 1_555 1_555 yes O(3) Cr(1) O(5) 94.2(5) 1_555 1_555 1_555 yes O(3) Cr(1) O(6) 173.1(5) 1_555 1_555 1_555 yes O(4) Cr(1) O(5) 92.8(6) 1_555 1_555 1_555 yes O(4) Cr(1) O(6) 92.8(6) 1_555 1_555 1_555 yes O(5) Cr(1) O(6) 81.0(6) 1_555 1_555 1_555 yes C(19) S(1) C(20) 96.1(10) 1_555 1_555 1_555 yes C(19) S(2) C(21) 94(1) 1_555 1_555 1_555 yes C(20) S(3) C(22) 100(1) 1_555 1_555 1_555 yes C(21) S(4) C(23) 102(1) 1_555 1_555 1_555 yes C(24) S(5) C(25) 96(1) 1_555 1_555 1_555 yes C(24) S(6) C(26) 97(1) 1_555 1_555 1_555 yes C(25) S(7) C(27) 102(2) 1_555 1_555 1_555 yes C(26) S(8) C(28) 101(1) 1_555 1_555 1_555 yes Cr(1) O(1) C(1) 111(1) 1_555 1_555 1_555 yes Cr(1) O(2) C(6) 111(1) 1_555 1_555 1_555 yes Cr(1) O(3) C(7) 112(1) 1_555 1_555 1_555 yes Cr(1) O(4) C(12) 111(1) 1_555 1_555 1_555 yes Cr(1) O(5) C(13) 112(1) 1_555 1_555 1_555 yes Cr(1) O(6) C(18) 115(1) 1_555 1_555 1_555 yes O(1) C(1) C(2) 123(2) 1_555 1_555 1_555 yes O(1) C(1) C(6) 116(1) 1_555 1_555 1_555 yes C(2) C(1) C(6) 119(1) 1_555 1_555 1_555 yes Br(1) C(2) C(1) 117(1) 1_555 1_555 1_555 yes Br(1) C(2) C(3) 122(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 119(2) 1_555 1_555 1_555 yes Br(2) C(3) C(2) 119(2) 1_555 1_555 1_555 yes Br(2) C(3) C(4) 121(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 118(2) 1_555 1_555 1_555 yes Br(3) C(4) C(3) 120(1) 1_555 1_555 1_555 yes Br(3) C(4) C(5) 117(2) 1_555 1_555 1_555 yes C(3) C(4) C(5) 122(2) 1_555 1_555 1_555 yes Br(4) C(5) C(4) 123(1) 1_555 1_555 1_555 yes Br(4) C(5) C(6) 116(1) 1_555 1_555 1_555 yes C(4) C(5) C(6) 119(2) 1_555 1_555 1_555 yes O(2) C(6) C(1) 115(1) 1_555 1_555 1_555 yes O(2) C(6) C(5) 125(2) 1_555 1_555 1_555 yes C(1) C(6) C(5) 119(1) 1_555 1_555 1_555 yes O(3) C(7) C(8) 124(1) 1_555 1_555 1_555 yes O(3) C(7) C(12) 115(1) 1_555 1_555 1_555 yes C(8) C(7) C(12) 120(2) 1_555 1_555 1_555 yes Br(5) C(8) C(7) 116(1) 1_555 1_555 1_555 yes Br(5) C(8) C(9) 122(1) 1_555 1_555 1_555 yes C(7) C(8) C(9) 120(1) 1_555 1_555 1_555 yes Br(6) C(9) C(8) 120(1) 1_555 1_555 1_555 yes Br(6) C(9) C(10) 118(1) 1_555 1_555 1_555 yes C(8) C(9) C(10) 120(1) 1_555 1_555 1_555 yes Br(7) C(10) C(9) 120(1) 1_555 1_555 1_555 yes Br(7) C(10) C(11) 120(1) 1_555 1_555 1_555 yes C(9) C(10) C(11) 119(1) 1_555 1_555 1_555 yes Br(8) C(11) C(10) 122(1) 1_555 1_555 1_555 yes Br(8) C(11) C(12) 116(1) 1_555 1_555 1_555 yes C(10) C(11) C(12) 121(1) 1_555 1_555 1_555 yes O(4) C(12) C(7) 118(1) 1_555 1_555 1_555 yes O(4) C(12) C(11) 124(1) 1_555 1_555 1_555 yes C(7) C(12) C(11) 116(2) 1_555 1_555 1_555 yes O(5) C(13) C(14) 126(1) 1_555 1_555 1_555 yes O(5) C(13) C(18) 116(2) 1_555 1_555 1_555 yes C(14) C(13) C(18) 117(1) 1_555 1_555 1_555 yes Br(9) C(14) C(13) 115(1) 1_555 1_555 1_555 yes Br(9) C(14) C(15) 123(1) 1_555 1_555 1_555 yes C(13) C(14) C(15) 121(1) 1_555 1_555 1_555 yes Br(10) C(15) C(14) 119(1) 1_555 1_555 1_555 yes Br(10) C(15) C(16) 118(1) 1_555 1_555 1_555 yes C(14) C(15) C(16) 121(2) 1_555 1_555 1_555 yes Br(11) C(16) C(15) 120(1) 1_555 1_555 1_555 yes Br(11) C(16) C(17) 119(1) 1_555 1_555 1_555 yes C(15) C(16) C(17) 120(2) 1_555 1_555 1_555 yes Br(12) C(17) C(16) 123(1) 1_555 1_555 1_555 yes Br(12) C(17) C(18) 117(1) 1_555 1_555 1_555 yes C(16) C(17) C(18) 119(1) 1_555 1_555 1_555 yes O(6) C(18) C(13) 114(1) 1_555 1_555 1_555 yes O(6) C(18) C(17) 125(1) 1_555 1_555 1_555 yes C(13) C(18) C(17) 120(2) 1_555 1_555 1_555 yes S(1) C(19) S(2) 114(1) 1_555 1_555 1_555 yes S(1) C(19) C(19) 124(1) 1_555 1_555 2_757 yes S(2) C(19) C(19) 120(1) 1_555 1_555 2_757 yes S(1) C(20) S(3) 118(1) 1_555 1_555 1_555 yes S(1) C(20) C(21) 116(1) 1_555 1_555 1_555 yes S(3) C(20) C(21) 124(1) 1_555 1_555 1_555 yes S(2) C(21) S(4) 118(1) 1_555 1_555 1_555 yes S(2) C(21) C(20) 116(1) 1_555 1_555 1_555 yes S(4) C(21) C(20) 124(1) 1_555 1_555 1_555 yes S(5) C(24) S(6) 115(1) 1_555 1_555 1_555 yes S(5) C(24) C(24) 125(2) 1_555 1_555 2_746 yes S(6) C(24) C(24) 118(2) 1_555 1_555 2_746 yes S(5) C(25) S(7) 118(1) 1_555 1_555 1_555 yes S(5) C(25) C(26) 114(2) 1_555 1_555 1_555 yes S(7) C(25) C(26) 126(1) 1_555 1_555 1_555 yes S(6) C(26) S(8) 123(1) 1_555 1_555 1_555 yes S(6) C(26) C(25) 115(1) 1_555 1_555 1_555 yes S(8) C(26) C(25) 120(2) 1_555 1_555 1_555 yes C(30) C(31) C(35) 120(1) 1_555 1_555 1_555 yes C(30) C(31) C(36) 119(1) 1_555 1_555 1_555 yes C(35) C(31) C(36) 120(1) 1_555 1_555 1_555 yes C(31) C(30) C(32) 120(1) 1_555 1_555 1_555 yes C(30) C(32) C(33) 119(1) 1_555 1_555 1_555 yes C(32) C(33) C(34) 120(1) 1_555 1_555 1_555 yes C(33) C(34) C(35) 119(1) 1_555 1_555 1_555 yes C(31) C(35) C(34) 119(1) 1_555 1_555 1_555 yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br(2) Br(5) 3.508(3) 1_555 2_755 ? Br(4) C(24) 3.54(2) 1_555 2_756 ? Br(5) C(10) 3.57(2) 1_555 2_655 ? Br(6) C(7) 3.58(2) 1_555 2_655 ? Br(7) S(4) 3.596(7) 1_555 2_656 ? Br(10) O(4) 3.53(1) 1_555 2_665 ? S(1) C(5) 3.56(2) 1_555 2_756 ? S(2) O(1) 3.59(1) 1_555 1_556 ? S(3) S(3) 3.23(1) 1_555 2_756 ? S(4) C(35) 3.45(2) 1_555 1_555 ? S(4) C(31) 3.59(2) 1_555 1_555 ? S(5) C(6) 3.48(2) 1_555 1_545 ? S(5) C(1) 3.55(2) 1_555 1_545 ? S(6) O(6) 3.31(2) 1_555 2_756 ? S(6) O(2) 3.41(1) 1_555 2_756 ? O(1) C(23) 3.38(2) 1_555 1_554 ? O(2) C(32) 3.56(3) 1_555 1_555 ? O(4) C(28) 3.55(3) 1_555 2_756 ? O(5) C(23) 3.23(2) 1_555 1_554 ? C(5) C(24) 3.45(3) 1_555 1_565 ? C(11) C(32) 3.43(3) 1_555 1_555 ? C(11) C(33) 3.55(3) 1_555 1_555 ? C(12) C(32) 3.46(3) 1_555 1_555 ? _publ_contact_author_name ; Susumu Kitagawa ; _publ_contact_author_address ; Department of Synthetic Chemistry and Biological Chemistry, Faculty of Engineering, Kyoto Universsity, Yoshida, Sakyo-ku, Kyoto 606-8501, Japan ; _publ_contact_author_email 'kitagawa@sbchem.kyoto-u.ac.jp' _publ_contact_author_fax '+81-75-753-4979' _publ_contact_author_phone '+81-75-753-5658' #====END data_4b _audit_creation_date 'Thu Nov 5 16:26:25 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1940.95 _chemical_formula_analytical ? _chemical_formula_sum 'C30 H16 Br12 Cl4 Cr O6 Se4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? _cell_length_a 13.523(6) _cell_length_b 16.177(8) _cell_length_c 12.406(7) _cell_angle_alpha 111.43(4) _cell_angle_beta 109.39(4) _cell_angle_gamma 83.91(4) _cell_volume 2382(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 16.1 _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' _exptl_crystal_description 'cubic' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.750 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 2.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784.00 _exptl_absorpt_coefficient_mu 13.653 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.160 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -5.37 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -3 1 3 -2 -2 0 -4 2 _diffrn_reflns_number 10417 _reflns_number_total 9953 _reflns_number_gt 3232 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.083 _diffrn_reflns_av_sigmaI/netI 0.183 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05585 _diffrn_orient_matrix_UB_12 -0.04509 _diffrn_orient_matrix_UB_13 0.00854 _diffrn_orient_matrix_UB_21 0.03725 _diffrn_orient_matrix_UB_22 0.02359 _diffrn_orient_matrix_UB_23 -0.04046 _diffrn_orient_matrix_UB_31 0.04052 _diffrn_orient_matrix_UB_32 0.04269 _diffrn_orient_matrix_UB_33 0.08139 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cr' 'Cr' 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Se' 'Se' -0.093 2.226 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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_calc_flag Br(1) Br -0.4094(2) 0.9403(2) 0.1815(2) 0.078(1) Uani 1.00 d Br(2) Br -0.4175(2) 1.1468(2) 0.1777(3) 0.086(1) Uani 1.00 d Br(3) Br -0.3079(2) 1.1898(2) 0.0038(3) 0.090(1) Uani 1.00 d Br(4) Br -0.1920(2) 1.0275(2) -0.1657(3) 0.082(1) Uani 1.00 d Br(5) Br -0.5959(2) 0.6523(2) -0.4401(2) 0.0693(9) Uani 1.00 d Br(6) Br -0.5652(2) 0.5278(2) -0.7089(2) 0.0753(10) Uani 1.00 d Br(7) Br -0.3273(2) 0.4896(2) -0.7287(2) 0.077(1) Uani 1.00 d Br(8) Br -0.1218(2) 0.5592(2) -0.4798(2) 0.0580(9) Uani 1.00 d Br(9) Br -0.2558(2) 0.4787(2) -0.0032(2) 0.0653(9) Uani 1.00 d Br(10) Br -0.0249(2) 0.4592(2) 0.1914(2) 0.080(1) Uani 1.00 d Br(11) Br 0.1624(2) 0.6069(2) 0.2817(2) 0.080(1) Uani 1.00 d Br(12) Br 0.1223(2) 0.7648(2) 0.1574(2) 0.075(1) Uani 1.00 d Se(1) Se -0.0509(2) 1.0343(2) 0.2464(2) 0.0567(9) Uani 1.00 d Se(2) Se -0.1544(2) 1.1579(2) 0.4389(2) 0.0666(10) Uani 1.00 d Se(3) Se -0.0872(2) 0.8593(2) 0.3112(2) 0.0672(10) Uani 1.00 d Se(4) Se -0.1894(2) 0.9787(2) 0.5074(2) 0.0561(9) Uani 1.00 d Cr(1) Cr -0.2434(3) 0.7408(2) -0.1232(3) 0.045(1) Uani 1.00 d Cl(1) Cl 0.4696 0.0444 0.4097 1.0710 Uani 1.00 d Cl(2) Cl 0.6107 0.1704 0.6198 0.4519 Uani 1.00 d Cl(3) Cl 0.3983 0.2716 0.7713 0.5388 Uani 1.00 d Cl(4) Cl 0.5248 0.3712 0.9641 0.2467 Uani 1.00 d O(1) O -0.304(1) 0.818(1) -0.004(1) 0.054(5) Uani 1.00 d O(2) O -0.228(1) 0.8510(9) -0.145(1) 0.045(5) Uani 1.00 d O(3) O -0.381(1) 0.7102(9) -0.248(1) 0.044(5) Uani 1.00 d O(4) O -0.196(1) 0.6718(9) -0.262(1) 0.041(5) Uani 1.00 d O(5) O -0.249(1) 0.6391(9) -0.079(1) 0.044(5) Uani 1.00 d O(6) O -0.102(1) 0.7534(9) -0.011(1) 0.050(5) Uani 1.00 d C(1) C -0.307(2) 0.901(2) 0.007(2) 0.053(9) Uani 1.00 d C(2) C -0.352(2) 0.971(2) 0.080(2) 0.054(9) Uani 1.00 d C(3) C -0.351(2) 1.056(2) 0.079(2) 0.052(8) Uani 1.00 d C(4) C -0.309(2) 1.075(1) 0.006(2) 0.059(9) Uani 1.00 d C(5) C -0.259(2) 1.006(2) -0.069(2) 0.064(9) Uani 1.00 d C(6) C -0.262(2) 0.920(2) -0.072(2) 0.046(8) Uani 1.00 d C(7) C -0.377(2) 0.661(1) -0.353(2) 0.044(8) Uani 1.00 d C(8) C -0.462(2) 0.627(1) -0.460(2) 0.036(7) Uani 1.00 d C(9) C -0.450(2) 0.574(1) -0.569(2) 0.055(9) Uani 1.00 d C(10) C -0.345(2) 0.557(1) -0.577(2) 0.054(8) Uani 1.00 d C(11) C -0.260(2) 0.587(1) -0.472(2) 0.037(7) Uani 1.00 d C(12) C -0.273(2) 0.639(1) -0.364(2) 0.032(7) Uani 1.00 d C(13) C -0.162(2) 0.628(1) -0.002(2) 0.041(8) Uani 1.00 d C(14) C -0.146(2) 0.558(1) 0.043(2) 0.046(7) Uani 1.00 d C(15) C -0.050(2) 0.551(1) 0.127(2) 0.044(8) Uani 1.00 d C(16) C 0.034(2) 0.612(2) 0.166(2) 0.051(8) Uani 1.00 d C(17) C 0.019(2) 0.681(2) 0.119(2) 0.056(9) Uani 1.00 d C(18) C -0.079(2) 0.689(2) 0.036(2) 0.046(8) Uani 1.00 d C(19) C -0.113(2) 1.046(2) 0.364(2) 0.053(8) Uani 1.00 d C(20) C -0.128(2) 0.970(2) 0.390(2) 0.047(8) Uani 1.00 d C(21) C -0.064(2) 1.157(2) 0.266(2) 0.07(1) Uani 1.00 d C(22) C -0.112(2) 1.209(2) 0.349(2) 0.07(1) Uani 1.00 d C(23) C -0.024(2) 1.184(2) 0.186(2) 0.08(1) Uani 1.00 d C(24) C -0.135(2) 1.305(2) 0.371(2) 0.08(1) Uani 1.00 d C(25) C -0.140(2) 0.806(2) 0.391(2) 0.068(10) Uani 1.00 d C(26) C -0.183(2) 0.856(2) 0.476(2) 0.08(1) Uani 1.00 d C(27) C -0.123(3) 0.710(2) 0.356(3) 0.13(2) Uani 1.00 d C(28) C -0.227(2) 0.823(2) 0.547(2) 0.09(1) Uani 1.00 d C(29) C 0.5240 0.1261 0.4394 0.2619 Uani 1.00 d C(30) C 0.4302 0.3153 0.9408 0.1845 Uani 1.00 d H(1) H 0.0035 1.1345 0.1358 0.0964 Uiso 1.00 calc H(2) H 0.0295 1.2282 0.2357 0.0964 Uiso 1.00 calc H(3) H -0.0796 1.2084 0.1361 0.0964 Uiso 1.00 calc H(4) H -0.1811 1.3114 0.3000 0.0951 Uiso 1.00 calc H(5) H -0.1674 1.3259 0.4349 0.0951 Uiso 1.00 calc H(6) H -0.0719 1.3371 0.3983 0.0951 Uiso 1.00 calc H(7) H -0.0935 0.6902 0.2927 0.1479 Uiso 1.00 calc H(8) H -0.1902 0.6803 0.3282 0.1479 Uiso 1.00 calc H(9) H -0.0795 0.6967 0.4248 0.1479 Uiso 1.00 calc H(10) H -0.1751 0.7931 0.5911 0.1067 Uiso 1.00 calc H(11) H -0.2837 0.7830 0.4916 0.1067 Uiso 1.00 calc H(12) H -0.2524 0.8715 0.6016 0.1067 Uiso 1.00 calc H(13) H 0.5690 0.1156 0.3912 0.2916 Uiso 1.00 calc H(14) H 0.4743 0.1697 0.4231 0.2916 Uiso 1.00 calc H(15) H 0.3759 0.3500 0.9674 0.1949 Uiso 1.00 calc H(16) H 0.4485 0.2700 0.9754 0.1949 Uiso 1.00 calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.066(2) 0.109(3) 0.059(2) 0.006(2) 0.033(2) 0.018(2) Br(2) 0.064(2) 0.085(2) 0.084(2) 0.021(2) 0.035(2) -0.003(2) Br(3) 0.081(2) 0.056(2) 0.127(3) 0.021(2) 0.044(2) 0.022(2) Br(4) 0.107(3) 0.059(2) 0.105(2) 0.012(2) 0.063(2) 0.031(2) Br(5) 0.039(2) 0.088(2) 0.069(2) 0.016(1) 0.017(1) 0.017(2) Br(6) 0.055(2) 0.098(2) 0.045(1) 0.013(2) 0.001(1) 0.009(2) Br(7) 0.075(2) 0.100(2) 0.043(1) 0.024(2) 0.022(2) 0.015(2) Br(8) 0.046(2) 0.072(2) 0.064(2) 0.022(1) 0.027(1) 0.029(2) Br(9) 0.068(2) 0.073(2) 0.064(2) -0.002(2) 0.020(2) 0.034(2) Br(10) 0.091(2) 0.085(2) 0.080(2) 0.037(2) 0.031(2) 0.052(2) Br(11) 0.050(2) 0.120(3) 0.059(2) 0.025(2) 0.004(2) 0.037(2) Br(12) 0.045(2) 0.085(2) 0.080(2) -0.008(2) 0.008(2) 0.018(2) Se(1) 0.054(2) 0.063(2) 0.060(2) 0.008(1) 0.024(1) 0.024(1) Se(2) 0.068(2) 0.058(2) 0.091(2) 0.016(2) 0.047(2) 0.030(2) Se(3) 0.098(2) 0.053(2) 0.060(2) 0.014(2) 0.044(2) 0.016(1) Se(4) 0.060(2) 0.055(2) 0.058(2) 0.011(1) 0.030(1) 0.019(1) Cr(1) 0.040(3) 0.053(3) 0.042(2) 0.009(2) 0.012(2) 0.017(2) Cl(1) 0.3173 2.2771 0.5820 0.1244 0.3014 0.3445 Cl(2) 0.3141 0.4309 0.4509 0.0329 -0.0205 0.1066 Cl(3) 0.7994 0.1965 0.3362 -0.0617 -0.2601 0.1470 Cl(4) 0.2454 0.1972 0.2749 -0.0229 -0.0051 0.1272 O(1) 0.05(1) 0.07(1) 0.040(9) 0.011(9) 0.020(8) 0.016(9) O(2) 0.05(1) 0.05(1) 0.036(8) 0.014(8) 0.018(8) 0.016(8) O(3) 0.04(1) 0.06(1) 0.033(8) 0.022(8) 0.020(8) 0.019(8) O(4) 0.025(9) 0.05(1) 0.052(9) 0.011(7) 0.007(8) 0.030(8) O(5) 0.030(10) 0.06(1) 0.039(8) 0.003(8) 0.007(8) 0.021(8) O(6) 0.06(1) 0.05(1) 0.051(9) 0.011(8) 0.025(9) 0.026(9) C(1) 0.05(2) 0.05(2) 0.04(1) 0.00(1) 0.01(1) 0.01(1) C(2) 0.03(2) 0.09(2) 0.05(1) 0.01(1) 0.02(1) 0.02(2) C(3) 0.05(2) 0.04(2) 0.05(2) 0.01(1) 0.02(1) 0.00(1) C(4) 0.06(2) 0.03(2) 0.08(2) 0.00(1) 0.03(2) 0.00(1) C(5) 0.06(2) 0.07(2) 0.05(2) 0.01(2) 0.00(1) 0.02(2) C(6) 0.04(2) 0.05(2) 0.04(1) 0.02(1) 0.01(1) 0.01(1) C(7) 0.04(2) 0.04(2) 0.06(2) 0.01(1) 0.02(1) 0.03(1) C(8) 0.02(1) 0.05(2) 0.04(1) 0.01(1) 0.02(1) 0.02(1) C(9) 0.04(2) 0.04(2) 0.08(2) 0.02(1) 0.02(2) 0.03(2) C(10) 0.08(2) 0.05(2) 0.03(1) 0.02(1) 0.01(1) 0.02(1) C(11) 0.03(1) 0.05(2) 0.05(1) 0.01(1) 0.02(1) 0.03(1) C(12) 0.04(2) 0.03(1) 0.03(1) 0.01(1) 0.01(1) 0.01(1) C(13) 0.05(2) 0.04(2) 0.02(1) 0.01(1) 0.01(1) 0.01(1) C(14) 0.04(2) 0.06(2) 0.02(1) -0.01(1) -0.01(1) 0.00(1) C(15) 0.06(2) 0.05(2) 0.02(1) 0.00(1) 0.02(1) -0.01(1) C(16) 0.06(2) 0.06(2) 0.02(1) 0.03(2) 0.02(1) 0.01(1) C(17) 0.04(2) 0.07(2) 0.04(1) 0.00(1) 0.01(1) 0.00(1) C(18) 0.05(2) 0.06(2) 0.03(1) -0.01(1) 0.01(1) 0.00(1) C(19) 0.04(2) 0.08(2) 0.03(1) -0.01(1) 0.01(1) 0.00(1) C(20) 0.03(2) 0.06(2) 0.04(1) 0.01(1) 0.00(1) 0.02(1) C(21) 0.05(2) 0.07(2) 0.09(2) 0.01(2) 0.03(2) 0.05(2) C(22) 0.06(2) 0.05(2) 0.10(2) 0.01(1) 0.03(2) 0.05(2) C(23) 0.07(2) 0.09(2) 0.11(2) 0.00(2) 0.05(2) 0.07(2) C(24) 0.08(2) 0.04(2) 0.12(2) 0.01(2) 0.06(2) 0.02(2) C(25) 0.11(3) 0.03(2) 0.06(2) 0.02(2) 0.03(2) 0.02(1) C(26) 0.12(3) 0.03(2) 0.09(2) 0.01(2) 0.04(2) 0.02(2) C(27) 0.24(4) 0.06(2) 0.12(3) 0.02(2) 0.11(3) 0.04(2) C(28) 0.13(3) 0.07(2) 0.09(2) 0.03(2) 0.08(2) 0.04(2) C(29) 0.4831 0.0956 0.4886 0.1905 0.4733 0.1815 C(30) 0.2193 0.0839 0.4215 0.0776 0.2877 0.1328 _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00009|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3232 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.976 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.01 _refine_diff_density_max 1.28 _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) C(2) 1.90(2) 1_555 1_555 yes Br(2) C(3) 1.90(2) 1_555 1_555 yes Br(3) C(4) 1.87(2) 1_555 1_555 yes Br(4) C(5) 1.86(2) 1_555 1_555 yes Br(5) C(8) 1.88(2) 1_555 1_555 yes Br(6) C(9) 1.87(2) 1_555 1_555 yes Br(7) C(10) 1.88(2) 1_555 1_555 yes Br(8) C(11) 1.90(2) 1_555 1_555 yes Br(9) C(14) 1.87(2) 1_555 1_555 yes Br(10) C(15) 1.88(2) 1_555 1_555 yes Br(11) C(16) 1.87(2) 1_555 1_555 yes Br(12) C(17) 1.86(2) 1_555 1_555 yes Se(1) C(19) 1.85(2) 1_555 1_555 yes Se(1) C(21) 1.90(3) 1_555 1_555 yes Se(2) C(19) 1.83(2) 1_555 1_555 yes Se(2) C(22) 1.86(2) 1_555 1_555 yes Se(3) C(20) 1.82(2) 1_555 1_555 yes Se(3) C(25) 1.86(2) 1_555 1_555 yes Se(4) C(20) 1.87(2) 1_555 1_555 yes Se(4) C(26) 1.87(2) 1_555 1_555 yes Cr(1) O(1) 1.91(1) 1_555 1_555 yes Cr(1) O(2) 1.94(1) 1_555 1_555 yes Cr(1) O(3) 1.96(1) 1_555 1_555 yes Cr(1) O(4) 1.95(1) 1_555 1_555 yes Cr(1) O(5) 1.93(1) 1_555 1_555 yes Cr(1) O(6) 1.93(1) 1_555 1_555 yes Cl(1) C(29) 1.4472(2) 1_555 1_555 yes Cl(3) C(30) 1.867 1_555 1_555 yes Cl(4) C(30) 1.5316(5) 1_555 1_555 yes O(1) C(1) 1.31(2) 1_555 1_555 yes O(2) C(6) 1.31(2) 1_555 1_555 yes O(3) C(7) 1.27(2) 1_555 1_555 yes O(4) C(12) 1.31(2) 1_555 1_555 yes O(5) C(13) 1.29(2) 1_555 1_555 yes O(6) C(18) 1.33(2) 1_555 1_555 yes C(1) C(2) 1.40(3) 1_555 1_555 yes C(1) C(6) 1.44(3) 1_555 1_555 yes C(2) C(3) 1.37(3) 1_555 1_555 yes C(3) C(4) 1.35(3) 1_555 1_555 yes C(4) C(5) 1.45(3) 1_555 1_555 yes C(5) C(6) 1.39(3) 1_555 1_555 yes C(7) C(8) 1.41(3) 1_555 1_555 yes C(7) C(12) 1.45(3) 1_555 1_555 yes C(8) C(9) 1.36(3) 1_555 1_555 yes C(9) C(10) 1.45(3) 1_555 1_555 yes C(10) C(11) 1.38(3) 1_555 1_555 yes C(11) C(12) 1.36(2) 1_555 1_555 yes C(13) C(14) 1.41(3) 1_555 1_555 yes C(13) C(18) 1.41(3) 1_555 1_555 yes C(14) C(15) 1.39(3) 1_555 1_555 yes C(15) C(16) 1.43(3) 1_555 1_555 yes C(16) C(17) 1.41(3) 1_555 1_555 yes C(17) C(18) 1.41(3) 1_555 1_555 yes C(19) C(20) 1.43(3) 1_555 1_555 yes C(21) C(22) 1.36(3) 1_555 1_555 yes C(21) C(23) 1.49(3) 1_555 1_555 yes C(22) C(24) 1.49(3) 1_555 1_555 yes C(25) C(26) 1.34(3) 1_555 1_555 yes C(25) C(27) 1.46(3) 1_555 1_555 yes C(26) C(28) 1.48(3) 1_555 1_555 yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(19) Se(1) C(21) 93(1) 1_555 1_555 1_555 yes C(19) Se(2) C(22) 94(1) 1_555 1_555 1_555 yes C(20) Se(3) C(25) 93(1) 1_555 1_555 1_555 yes C(20) Se(4) C(26) 93(1) 1_555 1_555 1_555 yes O(1) Cr(1) O(2) 82.3(6) 1_555 1_555 1_555 yes O(1) Cr(1) O(3) 91.9(6) 1_555 1_555 1_555 yes O(1) Cr(1) O(4) 170.8(6) 1_555 1_555 1_555 yes O(1) Cr(1) O(5) 93.0(6) 1_555 1_555 1_555 yes O(1) Cr(1) O(6) 94.9(6) 1_555 1_555 1_555 yes O(2) Cr(1) O(3) 94.7(6) 1_555 1_555 1_555 yes O(2) Cr(1) O(4) 91.7(5) 1_555 1_555 1_555 yes O(2) Cr(1) O(5) 172.4(6) 1_555 1_555 1_555 yes O(2) Cr(1) O(6) 90.9(6) 1_555 1_555 1_555 yes O(3) Cr(1) O(4) 81.7(5) 1_555 1_555 1_555 yes O(3) Cr(1) O(5) 91.4(6) 1_555 1_555 1_555 yes O(3) Cr(1) O(6) 171.7(6) 1_555 1_555 1_555 yes O(4) Cr(1) O(5) 93.7(5) 1_555 1_555 1_555 yes O(4) Cr(1) O(6) 92.1(6) 1_555 1_555 1_555 yes O(5) Cr(1) O(6) 83.4(6) 1_555 1_555 1_555 yes C(29) Cl(1) H(13) 26.927(2) 1_555 1_555 1_555 no C(29) Cl(1) H(14) 26.927(10) 1_555 1_555 1_555 no H(13) Cl(1) H(14) 46.172(10) 1_555 1_555 1_555 no Cr(1) O(1) C(1) 114(1) 1_555 1_555 1_555 yes Cr(1) O(2) C(6) 113(1) 1_555 1_555 1_555 yes Cr(1) O(3) C(7) 113(1) 1_555 1_555 1_555 yes Cr(1) O(4) C(12) 113(1) 1_555 1_555 1_555 yes Cr(1) O(5) C(13) 111(1) 1_555 1_555 1_555 yes Cr(1) O(6) C(18) 111(1) 1_555 1_555 1_555 yes O(1) C(1) C(2) 127(2) 1_555 1_555 1_555 yes O(1) C(1) C(6) 114(2) 1_555 1_555 1_555 yes C(2) C(1) C(6) 118(2) 1_555 1_555 1_555 yes Br(1) C(2) C(1) 115(1) 1_555 1_555 1_555 yes Br(1) C(2) C(3) 124(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 120(2) 1_555 1_555 1_555 yes Br(2) C(3) C(2) 118(1) 1_555 1_555 1_555 yes Br(2) C(3) C(4) 118(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 122(2) 1_555 1_555 1_555 yes Br(3) C(4) C(3) 122(1) 1_555 1_555 1_555 yes Br(3) C(4) C(5) 117(1) 1_555 1_555 1_555 yes C(3) C(4) C(5) 119(2) 1_555 1_555 1_555 yes Br(4) C(5) C(4) 122(1) 1_555 1_555 1_555 yes Br(4) C(5) C(6) 118(2) 1_555 1_555 1_555 yes C(4) C(5) C(6) 118(2) 1_555 1_555 1_555 yes O(2) C(6) C(1) 115(2) 1_555 1_555 1_555 yes O(2) C(6) C(5) 124(2) 1_555 1_555 1_555 yes C(1) C(6) C(5) 120(2) 1_555 1_555 1_555 yes O(3) C(7) C(8) 126(2) 1_555 1_555 1_555 yes O(3) C(7) C(12) 116(2) 1_555 1_555 1_555 yes C(8) C(7) C(12) 117(2) 1_555 1_555 1_555 yes Br(5) C(8) C(7) 115(1) 1_555 1_555 1_555 yes Br(5) C(8) C(9) 121(1) 1_555 1_555 1_555 yes C(7) C(8) C(9) 122(2) 1_555 1_555 1_555 yes Br(6) C(9) C(8) 121(1) 1_555 1_555 1_555 yes Br(6) C(9) C(10) 119(1) 1_555 1_555 1_555 yes C(8) C(9) C(10) 118(2) 1_555 1_555 1_555 yes Br(7) C(10) C(9) 119(1) 1_555 1_555 1_555 yes Br(7) C(10) C(11) 121(1) 1_555 1_555 1_555 yes C(9) C(10) C(11) 119(2) 1_555 1_555 1_555 yes Br(8) C(11) C(10) 120(1) 1_555 1_555 1_555 yes Br(8) C(11) C(12) 118(1) 1_555 1_555 1_555 yes C(10) C(11) C(12) 121(2) 1_555 1_555 1_555 yes O(4) C(12) C(7) 114(1) 1_555 1_555 1_555 yes O(4) C(12) C(11) 124(2) 1_555 1_555 1_555 yes C(7) C(12) C(11) 120(2) 1_555 1_555 1_555 yes O(5) C(13) C(14) 123(2) 1_555 1_555 1_555 yes O(5) C(13) C(18) 117(2) 1_555 1_555 1_555 yes C(14) C(13) C(18) 119(2) 1_555 1_555 1_555 yes Br(9) C(14) C(13) 119(1) 1_555 1_555 1_555 yes Br(9) C(14) C(15) 120(1) 1_555 1_555 1_555 yes C(13) C(14) C(15) 120(1) 1_555 1_555 1_555 yes Br(10) C(15) C(14) 121(1) 1_555 1_555 1_555 yes Br(10) C(15) C(16) 117(1) 1_555 1_555 1_555 yes C(14) C(15) C(16) 120(1) 1_555 1_555 1_555 yes Br(11) C(16) C(15) 122(1) 1_555 1_555 1_555 yes Br(11) C(16) C(17) 118(1) 1_555 1_555 1_555 yes C(15) C(16) C(17) 119(2) 1_555 1_555 1_555 yes Br(12) C(17) C(16) 124(1) 1_555 1_555 1_555 yes Br(12) C(17) C(18) 116(1) 1_555 1_555 1_555 yes C(16) C(17) C(18) 118(2) 1_555 1_555 1_555 yes O(6) C(18) C(13) 114(2) 1_555 1_555 1_555 yes O(6) C(18) C(17) 123(1) 1_555 1_555 1_555 yes C(13) C(18) C(17) 121(2) 1_555 1_555 1_555 yes Se(1) C(19) Se(2) 116(1) 1_555 1_555 1_555 yes Se(1) C(19) C(20) 119(1) 1_555 1_555 1_555 yes Se(2) C(19) C(20) 123(1) 1_555 1_555 1_555 yes Se(3) C(20) Se(4) 116(1) 1_555 1_555 1_555 yes Se(3) C(20) C(19) 122(1) 1_555 1_555 1_555 yes Se(4) C(20) C(19) 121(1) 1_555 1_555 1_555 yes Se(1) C(21) C(22) 117(1) 1_555 1_555 1_555 yes Se(1) C(21) C(23) 115(1) 1_555 1_555 1_555 yes C(22) C(21) C(23) 127(2) 1_555 1_555 1_555 yes Se(2) C(22) C(21) 118(1) 1_555 1_555 1_555 yes Se(2) C(22) C(24) 116(1) 1_555 1_555 1_555 yes C(21) C(22) C(24) 124(2) 1_555 1_555 1_555 yes C(21) C(23) H(1) 110(2) 1_555 1_555 1_555 no C(21) C(23) H(2) 108(2) 1_555 1_555 1_555 no C(21) C(23) H(3) 109(2) 1_555 1_555 1_555 no H(1) C(23) H(2) 109(2) 1_555 1_555 1_555 no H(1) C(23) H(3) 109(2) 1_555 1_555 1_555 no H(2) C(23) H(3) 108(2) 1_555 1_555 1_555 no C(22) C(24) H(4) 109(2) 1_555 1_555 1_555 no C(22) C(24) H(5) 108(2) 1_555 1_555 1_555 no C(22) C(24) H(6) 110(2) 1_555 1_555 1_555 no H(4) C(24) H(5) 108(2) 1_555 1_555 1_555 no H(4) C(24) H(6) 111(2) 1_555 1_555 1_555 no H(5) C(24) H(6) 108(2) 1_555 1_555 1_555 no Se(3) C(25) C(26) 119(1) 1_555 1_555 1_555 yes Se(3) C(25) C(27) 113(1) 1_555 1_555 1_555 yes Se(3) C(25) H(7) 87(1) 1_555 1_555 1_555 no Se(3) C(25) H(8) 126(1) 1_555 1_555 1_555 no Se(3) C(25) H(9) 123(1) 1_555 1_555 1_555 no C(26) C(25) C(27) 126(2) 1_555 1_555 1_555 yes C(26) C(25) H(7) 153(1) 1_555 1_555 1_555 no C(26) C(25) H(8) 110(1) 1_555 1_555 1_555 no C(26) C(25) H(9) 110(1) 1_555 1_555 1_555 no C(27) C(25) H(7) 26(1) 1_555 1_555 1_555 no C(27) C(25) H(8) 27(1) 1_555 1_555 1_555 no C(27) C(25) H(9) 26(1) 1_555 1_555 1_555 no H(7) C(25) H(8) 45.8(6) 1_555 1_555 1_555 no H(7) C(25) H(9) 45.8(6) 1_555 1_555 1_555 no H(8) C(25) H(9) 45.8(5) 1_555 1_555 1_555 no Se(4) C(26) C(25) 117(1) 1_555 1_555 1_555 yes Se(4) C(26) C(28) 117(1) 1_555 1_555 1_555 yes Se(4) C(26) H(11) 126(1) 1_555 1_555 1_555 no Se(4) C(26) H(12) 90(1) 1_555 1_555 1_555 no C(25) C(26) C(28) 124(2) 1_555 1_555 1_555 yes C(25) C(26) H(11) 109(1) 1_555 1_555 1_555 no C(25) C(26) H(12) 151(1) 1_555 1_555 1_555 no C(28) C(26) H(11) 26(1) 1_555 1_555 1_555 no C(28) C(26) H(12) 26(1) 1_555 1_555 1_555 no H(11) C(26) H(12) 45.7(6) 1_555 1_555 1_555 no C(25) C(27) H(7) 110(2) 1_555 1_555 1_555 no C(25) C(27) H(8) 108(3) 1_555 1_555 1_555 no C(25) C(27) H(9) 109(2) 1_555 1_555 1_555 no H(7) C(27) H(8) 109(3) 1_555 1_555 1_555 no H(7) C(27) H(9) 110(3) 1_555 1_555 1_555 no H(8) C(27) H(9) 108(2) 1_555 1_555 1_555 no C(26) C(28) H(10) 109(2) 1_555 1_555 1_555 no C(26) C(28) H(11) 108(2) 1_555 1_555 1_555 no C(26) C(28) H(12) 108(2) 1_555 1_555 1_555 no H(10) C(28) H(11) 110(2) 1_555 1_555 1_555 no H(10) C(28) H(12) 110(2) 1_555 1_555 1_555 no H(11) C(28) H(12) 109(2) 1_555 1_555 1_555 no Cl(1) C(29) H(13) 109.45(1) 1_555 1_555 1_555 no Cl(1) C(29) H(14) 109.45(2) 1_555 1_555 1_555 no H(13) C(29) H(14) 109.46(2) 1_555 1_555 1_555 no Cl(3) C(30) Cl(4) 94.653(2) 1_555 1_555 1_555 yes Cl(3) C(30) H(15) 113.041(10) 1_555 1_555 1_555 no Cl(3) C(30) H(16) 113.041(2) 1_555 1_555 1_555 no Cl(4) C(30) H(15) 113.04(2) 1_555 1_555 1_555 no Cl(4) C(30) H(16) 113.04(1) 1_555 1_555 1_555 no H(15) C(30) H(16) 109.460(2) 1_555 1_555 1_555 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br(1) Cl(1) 3.541(3) 1_555 1_465 ? Br(2) O(3) 3.51(1) 1_555 2_475 ? Br(3) Cl(4) 3.589(3) 1_555 1_464 ? Br(4) Br(12) 3.542(4) 1_555 2_575 ? Br(6) O(5) 3.52(1) 1_555 2_464 ? Br(6) Br(9) 3.559(3) 1_555 2_464 ? Br(7) Cl(4) 3.551(3) 1_555 1_453 ? Br(8) Br(10) 3.573(3) 1_555 2_565 ? Br(9) Cl(4) 3.431(3) 1_555 1_454 ? Br(10) O(4) 3.53(1) 1_555 2_565 ? Br(10) C(18) 3.55(2) 1_555 2_565 ? Se(3) C(17) 3.52(2) 1_555 1_555 ? Se(3) C(18) 3.55(2) 1_555 1_555 ? Cl(3) C(25) 3.50(3) 1_555 2_566 ? Cl(3) C(27) 3.55(4) 1_555 2_566 ? Cl(3) C(26) 3.59(3) 1_555 2_566 ? O(1) C(30) 3.32(1) 1_555 2_566 ? O(2) C(23) 3.57(3) 1_555 2_575 ? O(5) C(30) 3.30(1) 1_555 2_566 ? C(15) C(27) 3.42(4) 1_555 1_555 ? C(16) C(27) 3.53(4) 1_555 1_555 ? C(20) C(20) 3.58(4) 1_555 2_576 ? _publ_contact_author_name ; Susumu Kitagawa ; _publ_contact_author_address ; Department of Synthetic Chemistry and Biological Chemistry, Faculty of Engineering, Kyoto Universsity, Yoshida, Sakyo-ku, Kyoto 606-8501, Japan ; _publ_contact_author_email 'kitagawa@sbchem.kyoto-u.ac.jp' _publ_contact_author_fax '+81-75-753-4979' _publ_contact_author_phone '+81-75-753-5658' #====END