# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1520 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Paul Peringer Institut f\"ur Allgemeine und Anorganische Chemie Universit\"at Innsbruck Innrainstr. 52a A-6020 Innsbruck Austria ; _publ_contact_author_phone '043 512 5075112' _publ_contact_author_fax '043 512 5072934' _publ_contact_author_email paul.peringer@uibk.ac.at _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; Host-guest chemistry of the cluster [Hg3(m-dppm)3]4+ (dppm = bis(diphenylphosphino)methane) with oxo- and fluoro-aninons. ; loop_ _publ_author_name _publ_author_address 'Knoepfler-Muehlecker, Anna' ; Institut f\"ur Allgemeine und Anorganische Chemie Universit\"at Innsbruck Innrainstr. 52a A-6020 Innsbruck Austria ; 'Scheffter, Birgit' ; Institut f\"ur Allgemeine und Anorganische Chemie Universit\"at Innsbruck Innrainstr. 52a A-6020 Innsbruck Austria ; 'Kopacka, Holger' ; Institut f\"ur Allgemeine und Anorganische Chemie Universit\"at Innsbruck Innrainstr. 52a A-6020 Innsbruck Austria ; 'Wurst, Klaus' ; Institut f\"ur Allgemeine und Anorganische Chemie Universit\"at Innsbruck Innrainstr. 52a A-6020 Innsbruck Austria ; 'Paul Peringer' ; Institut f\"ur Allgemeine und Anorganische Chemie Universit\"at Innsbruck Innrainstr. 52a A-6020 Innsbruck Austria ; #============================================================================ data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C79 H78 F12 Hg3 O4 P6 Si2' _chemical_formula_weight 2163.18 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' .0817 .0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 22.280(4) _cell_length_b 20.665(4) _cell_length_c 16.909(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7785.2(25) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 4.9 _cell_measurement_theta_max 12.5 _exptl_crystal_description quader _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method ? _exptl_crystal_F_000 4200 _exptl_absorpt_coefficient_mu 6.134 _exptl_absorpt_correction_type PSI-scan _exptl_absorpt_correction_T_min 0.366 _exptl_absorpt_correction_T_max 0.896 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method Omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6390 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 23.00 _reflns_number_total 5702 _reflns_number_observed 4111 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0501P)^2^+23.2320P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(12) _refine_ls_number_reflns 5702 _refine_ls_number_parameters 540 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_obs 0.0478 _refine_ls_wR_factor_all 0.1133 _refine_ls_wR_factor_obs 0.0985 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.054 _refine_ls_restrained_S_obs 1.099 _refine_ls_shift/esd_max 0.106 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg1 Hg 0.09414(4) 0.83440(4) 0.20613(7) 0.0204(2) Uani 1 d . . Hg2 Hg 0.09149(3) 0.69922(4) 0.21183(7) 0.0208(2) Uani 1 d . . Hg3 Hg -0.00424(3) 0.76710(4) 0.26982(5) 0.0205(2) Uani 1 d . . P12 P 0.1919(2) 0.8302(3) 0.1305(4) 0.0168(14) Uani 1 d . . P13 P 0.0537(2) 0.9404(3) 0.2558(4) 0.021(2) Uani 1 d . . P21 P 0.1810(2) 0.6840(3) 0.1275(4) 0.0163(14) Uani 1 d . . P23 P 0.0594(2) 0.5914(3) 0.2676(5) 0.0204(14) Uani 1 d . . P31 P -0.0570(2) 0.8658(3) 0.3179(4) 0.0188(15) Uani 1 d . . P32 P -0.0568(2) 0.6633(3) 0.3113(4) 0.023(2) Uani 1 d . . Si1 Si 0.1066(3) 0.7634(4) 0.4415(4) 0.031(2) Uani 1 d . . Si2 Si 0.0076(3) 0.7687(4) 0.0201(5) 0.030(2) Uani 1 d . . F1 F 0.1157(7) 0.8300(7) 0.3854(11) 0.054(5) Uani 1 d . . F2 F 0.1230(6) 0.7186(7) 0.3613(9) 0.044(4) Uani 1 d . . F3 F 0.0334(6) 0.7638(8) 0.4140(8) 0.041(4) Uani 1 d . . F4 F 0.0623(6) 0.8178(7) 0.0539(9) 0.040(4) Uani 1 d . . F5 F 0.0397(6) 0.7078(7) 0.0699(8) 0.036(4) Uani 1 d . . F6 F -0.0329(6) 0.7886(8) 0.0998(10) 0.051(5) Uani 1 d . . F7 F 0.0922(7) 0.6977(8) 0.4915(10) 0.060(5) Uani 1 d . . F8 F 0.0876(7) 0.8067(8) 0.5183(10) 0.055(5) Uani 1 d . . F9 F 0.1780(6) 0.7635(8) 0.4680(10) 0.055(4) Uani 1 d . . F10 F -0.0460(7) 0.7175(7) -0.0113(11) 0.058(5) Uani 1 d . . F11 F -0.0238(7) 0.8315(7) -0.0292(10) 0.049(4) Uani 1 d . . F12 F 0.0483(7) 0.7505(7) -0.0576(8) 0.050(5) Uani 1 d . . C12 C 0.1913(9) 0.7580(11) 0.0667(14) 0.019(5) Uiso 1 d . . H12A H 0.2292 0.7553 0.0375 0.022 Uiso 1 calc . . H12B H 0.1586 0.7615 0.0282 0.022 Uiso 1 calc . . C13 C 0.0002(10) 0.6058(12) 0.3454(17) 0.037(7) Uiso 1 d . . H13A H -0.0192 0.5646 0.3586 0.044 Uiso 1 calc . . H13B H 0.0192 0.6225 0.3934 0.044 Uiso 1 calc . . C23 C 0.0021(9) 0.9251(10) 0.3374(14) 0.017(5) Uiso 1 d . . H23A H -0.0168 0.9661 0.3522 0.021 Uiso 1 calc . . H23B H 0.0255 0.9102 0.3830 0.021 Uiso 1 calc . . C111 C 0.2525(8) 0.8266(10) 0.2004(16) 0.020(5) Uiso 1 d . . C112 C 0.3132(10) 0.8109(12) 0.1729(17) 0.039(7) Uiso 1 d . . H112 H 0.3214 0.8035 0.1190 0.046 Uiso 1 calc . . C113 C 0.3589(9) 0.8073(12) 0.2304(16) 0.031(6) Uiso 1 d . . H113 H 0.3989 0.7997 0.2154 0.037 Uiso 1 calc . . C114 C 0.3446(13) 0.8148(16) 0.3064(21) 0.061(9) Uiso 1 d . . H114 H 0.3757 0.8123 0.3438 0.073 Uiso 1 calc . . C115 C 0.2883(11) 0.8256(13) 0.3331(18) 0.044(7) Uiso 1 d . . H115 H 0.2808 0.8278 0.3877 0.053 Uiso 1 calc . . C116 C 0.2414(11) 0.8336(12) 0.2789(20) 0.046(7) Uiso 1 d . . H116 H 0.2026 0.8438 0.2968 0.055 Uiso 1 calc . . C121 C 0.2053(9) 0.8972(11) 0.0592(15) 0.026(6) Uiso 1 d . . C122 C 0.1592(9) 0.9364(11) 0.0433(16) 0.025(6) Uiso 1 d . . H122 H 0.1226 0.9332 0.0707 0.030 Uiso 1 calc . . C123 C 0.1680(11) 0.9823(14) -0.0160(19) 0.047(8) Uiso 1 d . . H123 H 0.1353 1.0083 -0.0308 0.056 Uiso 1 calc . . C124 C 0.2177(12) 0.9910(13) -0.0513(18) 0.045(8) Uiso 1 d . . H124 H 0.2222 1.0253 -0.0873 0.054 Uiso 1 calc . . C125 C 0.2658(10) 0.9493(13) -0.0362(18) 0.039(7) Uiso 1 d . . H125 H 0.3021 0.9541 -0.0639 0.047 Uiso 1 calc . . C126 C 0.2595(11) 0.8992(12) 0.0215(18) 0.038(7) Uiso 1 d . . H126 H 0.2904 0.8697 0.0327 0.046 Uiso 1 calc . . C131 C 0.1057(9) 1.0000(10) 0.2935(14) 0.023(5) Uiso 1 d . . C132 C 0.1562(11) 1.0183(12) 0.2476(17) 0.046(7) Uiso 1 d . . H132 H 0.1665 0.9952 0.2018 0.055 Uiso 1 calc . . C133 C 0.1898(10) 1.0709(12) 0.2717(21) 0.048(7) Uiso 1 d . . H133 H 0.2210 1.0851 0.2385 0.058 Uiso 1 calc . . C134 C 0.1809(11) 1.1017(12) 0.3376(17) 0.039(7) Uiso 1 d . . H134 H 0.2066 1.1354 0.3534 0.047 Uiso 1 calc . . C135 C 0.1324(12) 1.0835(14) 0.3838(19) 0.049(8) Uiso 1 d . . H135 H 0.1248 1.1071 0.4303 0.059 Uiso 1 calc . . C136 C 0.0950(11) 1.0335(13) 0.3658(17) 0.039(7) Uiso 1 d . . H136 H 0.0635 1.0215 0.3997 0.046 Uiso 1 calc . . C141 C 0.0120(9) 0.9844(11) 0.1815(14) 0.027(6) Uiso 1 d . . C142 C -0.0086(10) 0.9507(12) 0.1151(17) 0.035(6) Uiso 1 d . . H142 H 0.0025 0.9072 0.1073 0.042 Uiso 1 calc . . C143 C -0.0444(10) 0.9808(12) 0.0620(16) 0.031(6) Uiso 1 d . . H143 H -0.0610 0.9564 0.0205 0.037 Uiso 1 calc . . C144 C -0.0576(10) 1.0465(12) 0.0663(16) 0.029(6) Uiso 1 d . . H144 H -0.0799 1.0678 0.0270 0.035 Uiso 1 calc . . C145 C -0.0359(12) 1.0782(14) 0.1316(19) 0.048(8) Uiso 1 d . . H145 H -0.0429 1.1228 0.1370 0.057 Uiso 1 calc . . C146 C -0.0044(10) 1.0463(12) 0.1893(16) 0.036(6) Uiso 1 d . . H146 H 0.0061 1.0686 0.2357 0.043 Uiso 1 calc . . C211 C 0.2510(10) 0.6661(13) 0.1768(16) 0.030(7) Uiso 1 d . . C212 C 0.3034(10) 0.6596(11) 0.1332(16) 0.028(6) Uiso 1 d . . H212 H 0.3022 0.6656 0.0781 0.034 Uiso 1 calc . . C213 C 0.3554(13) 0.6450(16) 0.1682(21) 0.057(9) Uiso 1 d . . H213 H 0.3907 0.6420 0.1380 0.068 Uiso 1 calc . . C214 C 0.3572(11) 0.6339(13) 0.2520(18) 0.038(8) Uiso 1 d . . H214 H 0.3933 0.6213 0.2765 0.046 Uiso 1 calc . . C215 C 0.3065(13) 0.6419(14) 0.2957(20) 0.058(9) Uiso 1 d . . H215 H 0.3072 0.6367 0.3509 0.069 Uiso 1 calc . . C216 C 0.2517(10) 0.6584(12) 0.2554(15) 0.025(6) Uiso 1 d . . H216 H 0.2161 0.6639 0.2845 0.030 Uiso 1 calc . . C221 C 0.1678(9) 0.6160(11) 0.0613(15) 0.025(6) Uiso 1 d . . C222 C 0.1327(9) 0.6195(11) -0.0045(15) 0.024(6) Uiso 1 d . . H222 H 0.1189 0.6598 -0.0227 0.028 Uiso 1 calc . . C223 C 0.1171(12) 0.5617(14) -0.0454(18) 0.044(8) Uiso 1 d . . H223 H 0.0964 0.5634 -0.0938 0.052 Uiso 1 calc . . C224 C 0.1328(11) 0.5036(13) -0.0125(17) 0.037(7) Uiso 1 d . . H224 H 0.1177 0.4656 -0.0357 0.044 Uiso 1 calc . . C225 C 0.1675(10) 0.4979(13) 0.0488(17) 0.037(7) Uiso 1 d . . H225 H 0.1795 0.4567 0.0662 0.045 Uiso 1 calc . . C226 C 0.1875(10) 0.5551(11) 0.0900(16) 0.029(6) Uiso 1 d . . H226 H 0.2127 0.5521 0.1344 0.035 Uiso 1 calc . . C231 C 0.1204(9) 0.5498(10) 0.3172(14) 0.020(5) Uiso 1 d . . C232 C 0.1509(10) 0.5016(11) 0.2823(18) 0.041(7) Uiso 1 d . . H232 H 0.1379 0.4868 0.2326 0.049 Uiso 1 calc . . C233 C 0.2022(12) 0.4719(14) 0.3173(20) 0.055(8) Uiso 1 d . . H233 H 0.2241 0.4399 0.2903 0.066 Uiso 1 calc . . C234 C 0.2184(11) 0.4913(14) 0.3908(18) 0.043(7) Uiso 1 d . . H234 H 0.2499 0.4703 0.4174 0.052 Uiso 1 calc . . C235 C 0.1886(11) 0.5418(12) 0.4262(16) 0.036(7) Uiso 1 d . . H235 H 0.2012 0.5565 0.4761 0.043 Uiso 1 calc . . C236 C 0.1407(11) 0.5713(13) 0.3897(18) 0.042(7) Uiso 1 d . . H236 H 0.1215 0.6065 0.4144 0.050 Uiso 1 calc . . C241 C 0.0289(8) 0.5354(9) 0.1989(15) 0.018(5) Uiso 1 d . . C242 C 0.0182(9) 0.4709(11) 0.2212(17) 0.033(6) Uiso 1 d . . H242 H 0.0242 0.4589 0.2743 0.039 Uiso 1 calc . . C243 C -0.0013(11) 0.4234(13) 0.1672(17) 0.045(7) Uiso 1 d . . H243 H -0.0053 0.3796 0.1812 0.054 Uiso 1 calc . . C244 C -0.0145(11) 0.4464(14) 0.0901(18) 0.047(8) Uiso 1 d . . H244 H -0.0281 0.4165 0.0521 0.056 Uiso 1 calc . . C245 C -0.0087(10) 0.5080(12) 0.0689(17) 0.037(7) Uiso 1 d . . H245 H -0.0199 0.5205 0.0175 0.044 Uiso 1 calc . . C246 C 0.0140(9) 0.5551(11) 0.1214(15) 0.026(6) Uiso 1 d . . H246 H 0.0190 0.5983 0.1053 0.032 Uiso 1 calc . . C311 C -0.0961(10) 0.8573(12) 0.4092(15) 0.026(6) Uiso 1 d . . C312 C -0.0667(10) 0.8622(13) 0.4803(17) 0.032(7) Uiso 1 d . . H312 H -0.0249 0.8680 0.4813 0.038 Uiso 1 calc . . C313 C -0.1004(11) 0.8584(13) 0.5545(18) 0.044(7) Uiso 1 d . . H313 H -0.0812 0.8649 0.6034 0.053 Uiso 1 calc . . C314 C -0.1593(11) 0.8453(12) 0.5511(17) 0.037(7) Uiso 1 d . . H314 H -0.1812 0.8395 0.5981 0.045 Uiso 1 calc . . C315 C -0.1875(11) 0.8404(12) 0.4807(17) 0.035(7) Uiso 1 d . . H315 H -0.2288 0.8312 0.4792 0.042 Uiso 1 calc . . C316 C -0.1569(10) 0.8487(12) 0.4117(16) 0.031(6) Uiso 1 d . . H316 H -0.1784 0.8485 0.3639 0.037 Uiso 1 calc . . C321 C -0.1096(9) 0.9027(11) 0.2502(14) 0.025(6) Uiso 1 d . . C322 C -0.1283(9) 0.9664(11) 0.2588(16) 0.033(6) Uiso 1 d . . H322 H -0.1143 0.9905 0.3022 0.039 Uiso 1 calc . . C323 C -0.1678(10) 0.9963(12) 0.2041(23) 0.050(7) Uiso 1 d . . H323 H -0.1790 1.0399 0.2090 0.060 Uiso 1 calc . . C324 C -0.1892(11) 0.9576(13) 0.1426(19) 0.049(7) Uiso 1 d . . H324 H -0.2172 0.9747 0.1067 0.059 Uiso 1 calc . . C325 C -0.1707(11) 0.8976(13) 0.1342(18) 0.043(7) Uiso 1 d . . H325 H -0.1837 0.8740 0.0899 0.051 Uiso 1 calc . . C326 C -0.1331(10) 0.8677(12) 0.1878(16) 0.037(7) Uiso 1 d . . H326 H -0.1234 0.8237 0.1819 0.045 Uiso 1 calc . . C331 C -0.1065(10) 0.6651(12) 0.3974(15) 0.023(6) Uiso 1 d . . C332 C -0.0820(12) 0.6771(14) 0.4718(19) 0.047(8) Uiso 1 d . . H332 H -0.0403 0.6815 0.4785 0.056 Uiso 1 calc . . C333 C -0.1226(14) 0.6827(15) 0.5389(21) 0.061(9) Uiso 1 d . . H333 H -0.1090 0.6923 0.5902 0.073 Uiso 1 calc . . C334 C -0.1800(13) 0.6732(14) 0.5228(19) 0.050(8) Uiso 1 d . . H334 H -0.2056 0.6715 0.5670 0.060 Uiso 1 calc . . C335 C -0.2046(13) 0.6664(15) 0.4590(21) 0.056(9) Uiso 1 d . . H335 H -0.2466 0.6648 0.4546 0.067 Uiso 1 calc . . C336 C -0.1663(9) 0.6609(11) 0.3902(15) 0.024(6) Uiso 1 d . . H336 H -0.1835 0.6543 0.3400 0.028 Uiso 1 calc . . C341 C -0.1000(9) 0.6230(11) 0.2340(15) 0.030(6) Uiso 1 d . . C342 C -0.1252(9) 0.5630(11) 0.2471(15) 0.028(6) Uiso 1 d . . H342 H -0.1202 0.5411 0.2953 0.034 Uiso 1 calc . . C343 C -0.1591(11) 0.5359(13) 0.1843(18) 0.047(8) Uiso 1 d . . H343 H -0.1782 0.4959 0.1925 0.056 Uiso 1 calc . . C344 C -0.1651(12) 0.5642(14) 0.1150(19) 0.048(8) Uiso 1 d . . H344 H -0.1846 0.5431 0.0730 0.058 Uiso 1 calc . . C345 C -0.1404(13) 0.6298(15) 0.1050(21) 0.064(9) Uiso 1 d . . H345 H -0.1490 0.6534 0.0589 0.077 Uiso 1 calc . . C346 C -0.1051(11) 0.6566(13) 0.1626(18) 0.042(7) Uiso 1 d . . H346 H -0.0850 0.6960 0.1544 0.051 Uiso 1 calc . . O1 O -0.1858(25) 0.7031(29) 0.8307(44) 0.273(28) Uiso 1 d . . O2 O -0.1427(16) 0.7427(14) 0.7426(20) 0.138(12) Uiso 1 d . . C1 C -0.1985(31) 0.7334(32) 0.7658(51) 0.181(24) Uiso 1 d . . C2 C -0.2479(16) 0.7490(17) 0.7175(35) 0.103(13) Uiso 1 d . . C3 C -0.0840(34) 0.7420(32) 0.7844(57) 0.231(33) Uiso 1 d . . C4 C -0.0303(19) 0.7787(22) 0.7465(32) 0.133(17) Uiso 1 d . . O4 O -0.1648(9) 0.7726(12) -0.0060(15) 0.082(7) Uiso 1 d . . O5 O 0.0473(9) 0.9187(10) -0.1033(13) 0.062(6) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0234(4) 0.0174(4) 0.0204(5) -0.0006(7) 0.0045(6) 0.0014(3) Hg2 0.0238(4) 0.0175(4) 0.0210(5) 0.0008(7) 0.0047(6) -0.0002(4) Hg3 0.0217(4) 0.0173(4) 0.0226(5) 0.0000(8) 0.0020(5) 0.0006(4) P12 0.026(3) 0.010(3) 0.015(4) 0.000(3) -0.001(3) 0.001(2) P13 0.023(3) 0.015(3) 0.024(4) -0.006(3) 0.003(3) -0.002(2) P21 0.024(3) 0.016(3) 0.008(4) 0.003(3) -0.002(3) -0.005(2) P23 0.021(3) 0.014(3) 0.027(4) 0.004(4) 0.000(3) -0.001(2) P31 0.016(3) 0.021(3) 0.019(4) 0.001(3) 0.000(3) 0.003(3) P32 0.022(3) 0.016(3) 0.031(4) 0.001(3) 0.005(3) -0.002(3) Si1 0.037(4) 0.019(3) 0.037(5) -0.008(4) -0.014(3) 0.005(4) Si2 0.025(3) 0.032(4) 0.032(4) 0.013(4) -0.002(3) 0.005(4) F1 0.074(11) 0.032(10) 0.055(12) 0.011(9) -0.002(10) -0.004(8) F2 0.062(9) 0.045(11) 0.026(9) -0.009(8) 0.010(8) 0.015(8) F3 0.045(8) 0.066(11) 0.011(8) 0.003(9) 0.002(7) 0.001(9) F4 0.042(8) 0.045(10) 0.031(10) 0.000(8) -0.016(8) 0.001(7) F5 0.047(8) 0.049(10) 0.014(8) 0.004(8) 0.010(7) 0.006(7) F6 0.047(9) 0.075(13) 0.031(10) 0.013(10) 0.020(8) 0.008(8) F7 0.089(12) 0.061(12) 0.028(10) 0.004(10) -0.010(10) 0.011(10) F8 0.072(11) 0.051(11) 0.041(11) -0.021(9) -0.004(10) 0.007(9) F9 0.042(8) 0.078(12) 0.045(10) -0.020(10) -0.025(8) -0.001(9) F10 0.073(11) 0.042(11) 0.060(12) -0.006(9) -0.018(10) -0.017(8) F11 0.072(11) 0.024(9) 0.050(11) 0.007(8) -0.006(9) 0.016(7) F12 0.079(11) 0.056(13) 0.015(8) 0.002(8) 0.006(8) 0.035(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 Hg1 P13 2.514(6) . ? Hg1 P12 2.527(6) . ? Hg1 F4 2.693(15) . ? Hg1 Hg2 2.7957(12) . ? Hg1 Hg3 2.8104(12) . ? Hg1 F1 3.07(2) . ? Hg2 P21 2.473(6) . ? Hg2 P23 2.523(6) . ? Hg2 F2 2.65(2) . ? Hg2 F5 2.669(14) . ? Hg2 Hg3 2.7346(12) . ? Hg3 P31 2.491(6) . ? Hg3 P32 2.542(6) . ? Hg3 F3 2.579(14) . ? Hg3 F6 2.98(2) . ? P12 C111 1.80(2) . ? P12 C12 1.84(2) . ? P12 C121 1.86(2) . ? P13 C131 1.81(2) . ? P13 C141 1.81(2) . ? P13 C23 1.82(2) . ? P21 C211 1.81(2) . ? P21 C221 1.82(2) . ? P21 C12 1.86(2) . ? P23 C241 1.78(2) . ? P23 C231 1.81(2) . ? P23 C13 1.89(3) . ? P31 C311 1.78(3) . ? P31 C321 1.81(2) . ? P31 C23 1.83(2) . ? P32 C341 1.83(2) . ? P32 C331 1.83(2) . ? P32 C13 1.83(2) . ? Si1 F7 1.63(2) . ? Si1 F8 1.63(2) . ? Si1 F9 1.653(14) . ? Si1 F2 1.68(2) . ? Si1 F1 1.68(2) . ? Si1 F3 1.696(15) . ? Si2 F12 1.64(2) . ? Si2 F6 1.67(2) . ? Si2 F5 1.674(15) . ? Si2 F10 1.68(2) . ? Si2 F4 1.69(2) . ? Si2 F11 1.69(2) . ? C111 C116 1.36(4) . ? C111 C112 1.47(3) . ? C112 C113 1.41(3) . ? C113 C114 1.33(4) . ? C114 C115 1.35(4) . ? C115 C116 1.40(4) . ? C121 C122 1.34(3) . ? C121 C126 1.37(3) . ? C122 C123 1.39(4) . ? C123 C124 1.27(4) . ? C124 C125 1.40(3) . ? C125 C126 1.43(4) . ? C131 C132 1.42(3) . ? C131 C136 1.43(4) . ? C132 C133 1.38(3) . ? C133 C134 1.30(4) . ? C134 C135 1.39(4) . ? C135 C136 1.36(3) . ? C141 C146 1.34(3) . ? C141 C142 1.40(3) . ? C142 C143 1.35(3) . ? C143 C144 1.39(3) . ? C144 C145 1.37(4) . ? C145 C146 1.37(4) . ? C211 C216 1.34(3) . ? C211 C212 1.39(3) . ? C212 C213 1.33(4) . ? C213 C214 1.44(4) . ? C214 C215 1.36(4) . ? C215 C216 1.44(4) . ? C221 C222 1.36(3) . ? C221 C226 1.42(3) . ? C222 C223 1.42(3) . ? C223 C224 1.37(3) . ? C224 C225 1.30(4) . ? C225 C226 1.44(3) . ? C231 C232 1.34(3) . ? C231 C236 1.38(4) . ? C232 C233 1.43(3) . ? C233 C234 1.35(4) . ? C234 C235 1.37(3) . ? C235 C236 1.38(3) . ? C241 C242 1.41(3) . ? C241 C246 1.41(3) . ? C242 C243 1.41(3) . ? C243 C244 1.42(4) . ? C244 C245 1.33(3) . ? C245 C246 1.41(3) . ? C311 C316 1.37(3) . ? C311 C312 1.37(3) . ? C312 C313 1.46(4) . ? C313 C314 1.34(3) . ? C314 C315 1.35(4) . ? C315 C316 1.36(4) . ? C321 C326 1.38(3) . ? C321 C322 1.39(3) . ? C322 C323 1.42(4) . ? C323 C324 1.40(4) . ? C324 C325 1.31(3) . ? C325 C326 1.38(3) . ? C331 C336 1.34(3) . ? C331 C332 1.39(4) . ? C332 C333 1.46(4) . ? C333 C334 1.32(4) . ? C334 C335 1.22(4) . ? C335 C336 1.45(4) . ? C341 C342 1.38(3) . ? C341 C346 1.40(4) . ? C342 C343 1.42(3) . ? C343 C344 1.32(4) . ? C344 C345 1.47(4) . ? C345 C346 1.37(4) . ? O1 C1 1.30(9) . ? O2 C1 1.32(6) . ? O2 C3 1.49(7) . ? C1 C2 1.41(8) . ? C3 C4 1.56(7) . ? 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 P13 Hg1 P12 120.6(2) . . ? P13 Hg1 F4 109.6(3) . . ? P12 Hg1 F4 74.9(3) . . ? P13 Hg1 Hg2 148.41(14) . . ? P12 Hg1 Hg2 90.06(13) . . ? F4 Hg1 Hg2 84.3(3) . . ? P13 Hg1 Hg3 91.35(13) . . ? P12 Hg1 Hg3 148.10(13) . . ? F4 Hg1 Hg3 95.6(3) . . ? Hg2 Hg1 Hg3 58.39(3) . . ? P13 Hg1 F1 75.6(3) . . ? P12 Hg1 F1 111.3(3) . . ? F4 Hg1 F1 169.0(4) . . ? Hg2 Hg1 F1 86.6(3) . . ? Hg3 Hg1 F1 74.3(3) . . ? P21 Hg2 P23 109.4(2) . . ? P21 Hg2 F2 110.8(3) . . ? P23 Hg2 F2 81.5(4) . . ? P21 Hg2 F5 80.7(3) . . ? P23 Hg2 F5 105.8(3) . . ? F2 Hg2 F5 163.9(4) . . ? P21 Hg2 Hg3 154.33(14) . . ? P23 Hg2 Hg3 95.65(13) . . ? F2 Hg2 Hg3 77.7(3) . . ? F5 Hg2 Hg3 87.2(3) . . ? P21 Hg2 Hg1 95.16(14) . . ? P23 Hg2 Hg1 154.4(2) . . ? F2 Hg2 Hg1 82.9(3) . . ? F5 Hg2 Hg1 84.9(3) . . ? Hg3 Hg2 Hg1 61.07(3) . . ? P31 Hg3 P32 112.6(2) . . ? P31 Hg3 F3 82.3(4) . . ? P32 Hg3 F3 82.3(4) . . ? P31 Hg3 Hg2 154.84(13) . . ? P32 Hg3 Hg2 91.44(14) . . ? F3 Hg3 Hg2 94.1(3) . . ? P31 Hg3 Hg1 95.03(14) . . ? P32 Hg3 Hg1 151.92(14) . . ? F3 Hg3 Hg1 97.0(3) . . ? Hg2 Hg3 Hg1 60.54(3) . . ? P31 Hg3 F6 95.3(3) . . ? P32 Hg3 F6 107.1(3) . . ? F3 Hg3 F6 170.5(4) . . ? Hg2 Hg3 F6 84.1(3) . . ? Hg1 Hg3 F6 73.9(3) . . ? C111 P12 C12 111.0(10) . . ? C111 P12 C121 109.7(10) . . ? C12 P12 C121 103.0(11) . . ? C111 P12 Hg1 108.4(8) . . ? C12 P12 Hg1 108.6(7) . . ? C121 P12 Hg1 116.1(7) . . ? C131 P13 C141 103.5(10) . . ? C131 P13 C23 104.9(10) . . ? C141 P13 C23 106.8(10) . . ? C131 P13 Hg1 118.8(7) . . ? C141 P13 Hg1 112.9(8) . . ? C23 P13 Hg1 109.1(7) . . ? C211 P21 C221 105.4(11) . . ? C211 P21 C12 108.6(11) . . ? C221 P21 C12 108.4(11) . . ? C211 P21 Hg2 117.2(9) . . ? C221 P21 Hg2 108.8(7) . . ? C12 P21 Hg2 108.3(7) . . ? C241 P23 C231 106.3(10) . . ? C241 P23 C13 106.9(10) . . ? C231 P23 C13 106.1(12) . . ? C241 P23 Hg2 116.1(8) . . ? C231 P23 Hg2 112.3(7) . . ? C13 P23 Hg2 108.6(8) . . ? C311 P31 C321 105.9(10) . . ? C311 P31 C23 105.2(11) . . ? C321 P31 C23 107.4(10) . . ? C311 P31 Hg3 115.6(8) . . ? C321 P31 Hg3 116.4(8) . . ? C23 P31 Hg3 105.5(7) . . ? C341 P32 C331 105.0(11) . . ? C341 P32 C13 107.1(11) . . ? C331 P32 C13 100.5(12) . . ? C341 P32 Hg3 115.5(8) . . ? C331 P32 Hg3 118.8(8) . . ? C13 P32 Hg3 108.4(8) . . ? F7 Si1 F8 89.5(10) . . ? F7 Si1 F9 92.9(9) . . ? F8 Si1 F9 91.9(9) . . ? F7 Si1 F2 90.2(8) . . ? F8 Si1 F2 177.5(9) . . ? F9 Si1 F2 90.5(8) . . ? F7 Si1 F1 174.9(9) . . ? F8 Si1 F1 91.9(9) . . ? F9 Si1 F1 92.0(9) . . ? F2 Si1 F1 88.2(9) . . ? F7 Si1 F3 87.5(8) . . ? F8 Si1 F3 88.1(8) . . ? F9 Si1 F3 179.6(9) . . ? F2 Si1 F3 89.5(8) . . ? F1 Si1 F3 87.6(8) . . ? F12 Si2 F6 178.7(10) . . ? F12 Si2 F5 89.7(7) . . ? F6 Si2 F5 90.6(8) . . ? F12 Si2 F10 89.8(10) . . ? F6 Si2 F10 91.5(9) . . ? F5 Si2 F10 89.4(8) . . ? F12 Si2 F4 90.5(9) . . ? F6 Si2 F4 88.2(9) . . ? F5 Si2 F4 88.5(7) . . ? F10 Si2 F4 177.9(9) . . ? F12 Si2 F11 90.6(8) . . ? F6 Si2 F11 89.2(8) . . ? F5 Si2 F11 178.6(9) . . ? F10 Si2 F11 92.0(8) . . ? F4 Si2 F11 90.2(8) . . ? Si1 F1 Hg1 124.2(8) . . ? Si1 F2 Hg2 142.5(8) . . ? Si1 F3 Hg3 124.9(7) . . ? Si2 F4 Hg1 126.2(8) . . ? Si2 F5 Hg2 133.4(8) . . ? Si2 F6 Hg3 128.7(8) . . ? P12 C12 P21 110.1(12) . . ? P32 C13 P23 111.6(14) . . ? P13 C23 P31 115.7(12) . . ? C116 C111 C112 120.1(22) . . ? C116 C111 P12 120.2(17) . . ? C112 C111 P12 119.5(20) . . ? C113 C112 C111 117.2(24) . . ? C114 C113 C112 119.2(24) . . ? C113 C114 C115 124.2(30) . . ? C114 C115 C116 119.6(29) . . ? C111 C116 C115 119.4(23) . . ? C122 C121 C126 124.6(24) . . ? C122 C121 P12 117.3(17) . . ? C126 C121 P12 117.8(18) . . ? C121 C122 C123 116.6(22) . . ? C124 C123 C122 123.9(27) . . ? C123 C124 C125 119.5(27) . . ? C124 C125 C126 119.8(23) . . ? C121 C126 C125 115.2(22) . . ? C132 C131 C136 118.2(21) . . ? C132 C131 P13 119.9(19) . . ? C136 C131 P13 121.7(17) . . ? C133 C132 C131 118.6(26) . . ? C134 C133 C132 123.8(28) . . ? C133 C134 C135 118.0(25) . . ? C136 C135 C134 123.8(28) . . ? C135 C136 C131 117.3(25) . . ? C146 C141 C142 117.9(23) . . ? C146 C141 P13 123.5(20) . . ? C142 C141 P13 118.4(18) . . ? C143 C142 C141 119.7(23) . . ? C142 C143 C144 122.6(25) . . ? C145 C144 C143 115.7(25) . . ? C146 C145 C144 121.5(26) . . ? C141 C146 C145 122.0(25) . . ? C216 C211 C212 120.4(25) . . ? C216 C211 P21 119.5(21) . . ? C212 C211 P21 120.1(20) . . ? C213 C212 C211 121.1(27) . . ? C212 C213 C214 119.9(30) . . ? C215 C214 C213 119.5(29) . . ? C214 C215 C216 118.4(29) . . ? C211 C216 C215 120.5(26) . . ? C222 C221 C226 120.2(22) . . ? C222 C221 P21 123.7(18) . . ? C226 C221 P21 115.2(19) . . ? C221 C222 C223 119.6(23) . . ? C224 C223 C222 118.4(27) . . ? C225 C224 C223 123.8(27) . . ? C224 C225 C226 119.8(25) . . ? C221 C226 C225 117.8(23) . . ? C232 C231 C236 117.7(22) . . ? C232 C231 P23 121.9(20) . . ? C236 C231 P23 120.2(18) . . ? C231 C232 C233 122.9(27) . . ? C234 C233 C232 117.9(28) . . ? C233 C234 C235 119.7(27) . . ? C234 C235 C236 121.1(27) . . ? C235 C236 C231 120.6(25) . . ? C242 C241 C246 118.9(22) . . ? C242 C241 P23 120.5(20) . . ? C246 C241 P23 120.6(16) . . ? C241 C242 C243 122.5(26) . . ? C242 C243 C244 115.3(24) . . ? C245 C244 C243 123.2(28) . . ? C244 C245 C246 121.8(27) . . ? C241 C246 C245 117.9(21) . . ? C316 C311 C312 117.1(24) . . ? C316 C311 P31 121.6(20) . . ? C312 C311 P31 121.2(18) . . ? C311 C312 C313 120.1(21) . . ? C314 C313 C312 118.4(27) . . ? C313 C314 C315 120.5(27) . . ? C314 C315 C316 120.8(22) . . ? C315 C316 C311 122.6(25) . . ? C326 C321 C322 117.6(22) . . ? C326 C321 P31 120.5(18) . . ? C322 C321 P31 121.9(19) . . ? C321 C322 C323 122.0(24) . . ? C324 C323 C322 116.7(23) . . ? C325 C324 C323 120.9(27) . . ? C324 C325 C326 122.8(28) . . ? C325 C326 C321 119.8(24) . . ? C336 C331 C332 118.9(25) . . ? C336 C331 P32 121.8(20) . . ? C332 C331 P32 119.0(18) . . ? C331 C332 C333 118.3(25) . . ? C334 C333 C332 115.4(32) . . ? C335 C334 C333 129.4(34) . . ? C334 C335 C336 117.2(27) . . ? C331 C336 C335 120.4(25) . . ? C342 C341 C346 123.5(22) . . ? C342 C341 P32 120.7(19) . . ? C346 C341 P32 115.8(18) . . ? C341 C342 C343 116.9(23) . . ? C344 C343 C342 123.0(25) . . ? C343 C344 C345 118.2(29) . . ? C346 C345 C344 120.4(30) . . ? C345 C346 C341 117.4(25) . . ? C1 O2 C3 133.4(59) . . ? O1 C1 O2 96.7(62) . . ? O1 C1 C2 140.6(73) . . ? O2 C1 C2 122.1(72) . . ? O2 C3 C4 118.4(65) . . ? _refine_diff_density_max 1.239 _refine_diff_density_min -1.383 _refine_diff_density_rms 0.182 #===END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C77 H70 Cl4 F24 Hg3 P10' _chemical_formula_weight 2504.60 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.559(4) _cell_length_b 44.421(11) _cell_length_c 15.113(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.12(2) _cell_angle_gamma 90.00 _cell_volume 8849.5(37) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 5.1 _cell_measurement_theta_max 12.5 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method ? _exptl_crystal_F_000 4824 _exptl_absorpt_coefficient_mu 5.586 _exptl_absorpt_correction_type PSI-scan _exptl_absorpt_correction_T_min 0.507 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method Omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9046 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0841 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 19.50 _reflns_number_total 7567 _reflns_number_observed 5279 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 654 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0000P)^2^+472.5146P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6913 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1153 _refine_ls_R_factor_obs 0.0646 _refine_ls_wR_factor_all 0.2530 _refine_ls_wR_factor_obs 0.1438 _refine_ls_goodness_of_fit_all 1.142 _refine_ls_goodness_of_fit_obs 1.221 _refine_ls_restrained_S_all 1.789 _refine_ls_restrained_S_obs 1.221 _refine_ls_shift/esd_max -0.036 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg1 Hg 0.87907(7) 0.13193(2) 0.09644(7) 0.0262(3) Uani 1 d . . Hg2 Hg 0.89202(7) 0.12897(2) -0.08346(7) 0.0259(3) Uani 1 d . . Hg3 Hg 0.70905(8) 0.11481(2) -0.07147(7) 0.0253(3) Uani 1 d . . P12 P 1.0564(5) 0.1516(2) 0.1900(5) 0.028(2) Uani 1 d . . P13 P 0.7923(5) 0.1259(2) 0.2084(5) 0.029(2) Uani 1 d . . P21 P 1.0782(5) 0.13836(15) 0.0001(5) 0.027(2) Uani 1 d . . P23 P 0.8171(5) 0.12297(15) -0.2663(5) 0.026(2) Uani 1 d . . P31 P 0.6025(5) 0.1101(2) 0.0233(5) 0.026(2) Uani 1 d . . P32 P 0.6144(5) 0.1052(2) -0.2529(5) 0.027(2) Uani 1 d . . P1 P 0.7917(7) 0.2062(2) -0.0986(6) 0.055(3) Uani 1 d . . P2 P 0.8303(6) 0.0364(2) 0.0563(6) 0.041(2) Uani 1 d . . P3 P 0.5938(6) 0.0761(2) 0.3635(6) 0.045(2) Uani 1 d . . P4 P 1.2815(8) 0.2406(2) 0.1870(7) 0.064(3) Uani 1 d . . F1 F 0.8031(22) 0.1914(5) 0.0006(16) 0.130(10) Uani 1 d . . F2 F 0.8969(14) 0.1918(4) -0.0777(17) 0.093(7) Uani 1 d . . F3 F 0.7298(15) 0.1773(4) -0.1567(12) 0.084(6) Uani 1 d . . F4 F 0.8852(14) 0.0667(4) 0.1127(12) 0.075(6) Uani 1 d . . F5 F 0.8657(26) 0.0425(7) -0.0231(20) 0.183(16) Uani 1 d . . F6 F 0.7327(16) 0.0561(5) 0.0020(16) 0.115(9) Uani 1 d . . F7 F 0.7852(16) 0.2225(4) -0.1935(14) 0.088(6) Uani 1 d . . F8 F 0.6933(20) 0.2220(4) -0.1077(21) 0.129(10) Uani 1 d . . F9 F 0.8482(21) 0.2347(5) -0.0365(18) 0.135(10) Uani 1 d . . F10 F 0.7693(16) 0.0081(4) -0.0013(15) 0.084(6) Uani 1 d . . F11 F 0.7900(20) 0.0299(5) 0.1379(16) 0.115(9) Uani 1 d . . F12 F 0.9212(20) 0.0183(6) 0.1179(24) 0.179(15) Uani 1 d . . F13 F 0.6998(13) 0.0838(5) 0.3629(12) 0.080(6) Uani 1 d . . F14 F 0.5717(14) 0.0533(4) 0.2762(12) 0.076(6) Uani 1 d . . F15 F 0.5395(12) 0.1019(4) 0.2830(11) 0.058(5) Uani 1 d . . F16 F 0.4885(12) 0.0683(4) 0.3633(13) 0.070(5) Uani 1 d . . F17 F 0.6160(15) 0.0996(4) 0.4501(12) 0.076(6) Uani 1 d . . F18 F 0.6467(12) 0.0498(4) 0.4408(11) 0.058(5) Uani 1 d . . F19 F 1.2586(34) 0.2412(8) 0.2742(24) 0.224(20) Uani 1 d . . F20 F 1.1668(20) 0.2325(6) 0.1203(25) 0.158(12) Uani 1 d . . F21 F 1.2456(21) 0.2745(5) 0.1614(17) 0.135(10) Uani 1 d . . F22 F 1.2941(28) 0.2391(9) 0.0927(20) 0.221(19) Uani 1 d . . F23 F 1.3873(23) 0.2496(9) 0.2433(27) 0.227(19) Uani 1 d . . F24 F 1.3090(20) 0.2073(5) 0.2041(23) 0.148(11) Uani 1 d . . C12 C 1.1069(20) 0.1643(6) 0.1019(19) 0.038(8) Uiso 1 d . . H12A H 1.0782 0.1841 0.0761 0.046 Uiso 1 calc . . H12B H 1.1806 0.1666 0.1367 0.046 Uiso 1 calc . . C13 C 0.6843(20) 0.1012(6) 0.1527(20) 0.040(8) Uiso 1 d . . H13A H 0.6434 0.1024 0.1901 0.049 Uiso 1 calc . . H13B H 0.7086 0.0805 0.1570 0.049 Uiso 1 calc . . C23 C 0.6822(18) 0.1250(5) -0.3165(17) 0.028(7) Uiso 1 d . . H23A H 0.6558 0.1171 -0.3834 0.034 Uiso 1 calc . . H23B H 0.6635 0.1463 -0.3212 0.034 Uiso 1 calc . . C111 C 1.1435(17) 0.1229(5) 0.2672(17) 0.024(7) Uiso 1 d . . C112 C 1.1127(21) 0.0948(7) 0.2738(20) 0.045(8) Uiso 1 d . . H112 H 1.0437 0.0898 0.2399 0.054 Uiso 1 calc . . C113 C 1.1796(25) 0.0734(8) 0.3289(24) 0.064(10) Uiso 1 d . . H113 H 1.1572 0.0541 0.3363 0.077 Uiso 1 calc . . C114 C 1.2841(22) 0.0811(7) 0.3748(21) 0.049(8) Uiso 1 d . . H114 H 1.3322 0.0663 0.4094 0.059 Uiso 1 calc . . C115 C 1.3143(22) 0.1088(7) 0.3692(21) 0.049(8) Uiso 1 d . . H115 H 1.3835 0.1136 0.4030 0.059 Uiso 1 calc . . C116 C 1.2449(19) 0.1318(6) 0.3133(19) 0.036(7) Uiso 1 d . . H116 H 1.2661 0.1515 0.3080 0.044 Uiso 1 calc . . C121 C 1.0561(19) 0.1836(6) 0.2620(18) 0.029(7) Uiso 1 d . . C122 C 1.0066(24) 0.2091(7) 0.2203(23) 0.058(9) Uiso 1 d . . H122 H 0.9784 0.2104 0.1518 0.070 Uiso 1 calc . . C123 C 0.9937(27) 0.2344(8) 0.2730(27) 0.076(11) Uiso 1 d . . H123 H 0.9582 0.2518 0.2414 0.091 Uiso 1 calc . . C124 C 1.0362(24) 0.2314(7) 0.3715(24) 0.059(9) Uiso 1 d . . H124 H 1.0257 0.2466 0.4095 0.071 Uiso 1 calc . . C125 C 1.0950(28) 0.2066(9) 0.4185(27) 0.083(12) Uiso 1 d . . H125 H 1.1299 0.2062 0.4870 0.099 Uiso 1 calc . . C126 C 1.1017(22) 0.1819(7) 0.3621(21) 0.047(8) Uiso 1 d . . H126 H 1.1373 0.1645 0.3931 0.057 Uiso 1 calc . . C131 C 0.7470(19) 0.1598(6) 0.2385(18) 0.030(7) Uiso 1 d . . C132 C 0.6992(31) 0.1590(9) 0.3026(30) 0.095(13) Uiso 1 d . . H132 H 0.6940 0.1411 0.3335 0.114 Uiso 1 calc . . C133 C 0.6583(36) 0.1876(12) 0.3180(35) 0.122(16) Uiso 1 d . . H133 H 0.6273 0.1882 0.3614 0.146 Uiso 1 calc . . C134 C 0.6636(31) 0.2133(10) 0.2713(30) 0.095(13) Uiso 1 d . . H134 H 0.6317 0.2309 0.2790 0.114 Uiso 1 calc . . C135 C 0.7117(29) 0.2140(9) 0.2168(28) 0.084(12) Uiso 1 d . . H135 H 0.7170 0.2321 0.1871 0.101 Uiso 1 calc . . C136 C 0.7580(23) 0.1865(7) 0.2014(22) 0.055(9) Uiso 1 d . . H136 H 0.7964 0.1874 0.1648 0.066 Uiso 1 calc . . C141 C 0.8793(20) 0.1079(6) 0.3223(19) 0.039(8) Uiso 1 d . . C142 C 0.8961(20) 0.0775(6) 0.3276(19) 0.037(7) Uiso 1 d . . H142 H 0.8573 0.0647 0.2756 0.044 Uiso 1 calc . . C143 C 0.9750(24) 0.0659(7) 0.4152(24) 0.062(10) Uiso 1 d . . H143 H 0.9879 0.0451 0.4204 0.074 Uiso 1 calc . . C144 C 1.0304(24) 0.0836(8) 0.4894(23) 0.061(10) Uiso 1 d . . H144 H 1.0813 0.0752 0.5461 0.073 Uiso 1 calc . . C145 C 1.0147(24) 0.1125(8) 0.4841(23) 0.064(10) Uiso 1 d . . H145 H 1.0558 0.1243 0.5382 0.077 Uiso 1 calc . . C146 C 0.9366(22) 0.1283(7) 0.3986(22) 0.055(9) Uiso 1 d . . H146 H 0.9262 0.1493 0.3952 0.066 Uiso 1 calc . . C211 C 1.1395(20) 0.1557(6) -0.0696(19) 0.040(8) Uiso 1 d . . C212 C 1.1823(23) 0.1358(7) -0.1153(22) 0.060(9) Uiso 1 d . . H212 H 1.1818 0.1148 -0.1066 0.071 Uiso 1 calc . . C213 C 1.2261(25) 0.1489(8) -0.1750(25) 0.070(10) Uiso 1 d . . H213 H 1.2558 0.1367 -0.2067 0.084 Uiso 1 calc . . C214 C 1.2237(25) 0.1793(8) -0.1845(24) 0.065(10) Uiso 1 d . . H214 H 1.2536 0.1878 -0.2229 0.078 Uiso 1 calc . . C215 C 1.1810(25) 0.1982(8) -0.1424(25) 0.069(10) Uiso 1 d . . H215 H 1.1789 0.2191 -0.1523 0.082 Uiso 1 calc . . C216 C 1.1398(20) 0.1848(6) -0.0829(19) 0.039(8) Uiso 1 d . . H216 H 1.1113 0.1974 -0.0511 0.047 Uiso 1 calc . . C221 C 1.1429(19) 0.1047(6) 0.0473(18) 0.029(7) Uiso 1 d . . C222 C 1.2535(23) 0.1030(7) 0.0995(22) 0.055(9) Uiso 1 d . . H222 H 1.2946 0.1202 0.1099 0.067 Uiso 1 calc . . C223 C 1.2939(23) 0.0753(7) 0.1324(22) 0.056(9) Uiso 1 d . . H223 H 1.3647 0.0747 0.1685 0.067 Uiso 1 calc . . C224 C 1.2463(26) 0.0492(8) 0.1200(25) 0.069(10) Uiso 1 d . . H224 H 1.2817 0.0311 0.1444 0.082 Uiso 1 calc . . C225 C 1.1403(24) 0.0498(7) 0.0689(23) 0.058(9) Uiso 1 d . . H225 H 1.1027 0.0318 0.0576 0.069 Uiso 1 calc . . C226 C 1.0912(20) 0.0771(6) 0.0349(19) 0.039(8) Uiso 1 d . . H226 H 1.0200 0.0772 0.0020 0.047 Uiso 1 calc . . C231 C 0.8517(20) 0.1518(6) -0.3295(18) 0.032(7) Uiso 1 d . . C232 C 0.7886(32) 0.1739(10) -0.3790(31) 0.104(14) Uiso 1 d . . H232 H 0.7210 0.1737 -0.3869 0.125 Uiso 1 calc . . C233 C 0.8258(37) 0.1990(11) -0.4223(34) 0.118(16) Uiso 1 d . . H233 H 0.7842 0.2158 -0.4495 0.141 Uiso 1 calc . . C234 C 0.9128(28) 0.1977(8) -0.4222(25) 0.070(10) Uiso 1 d . . H234 H 0.9304 0.2116 -0.4591 0.084 Uiso 1 calc . . C235 C 0.9797(33) 0.1768(10) -0.3705(31) 0.106(14) Uiso 1 d . . H235 H 1.0479 0.1786 -0.3598 0.127 Uiso 1 calc . . C236 C 0.9460(25) 0.1497(7) -0.3283(23) 0.064(10) Uiso 1 d . . H236 H 0.9877 0.1328 -0.3030 0.076 Uiso 1 calc . . C241 C 0.8536(18) 0.0866(6) -0.2921(18) 0.028(7) Uiso 1 d . . C242 C 0.8803(22) 0.0648(7) -0.2230(21) 0.049(8) Uiso 1 d . . H242 H 0.8813 0.0696 -0.1620 0.059 Uiso 1 calc . . C243 C 0.9065(26) 0.0356(8) -0.2376(26) 0.076(11) Uiso 1 d . . H243 H 0.9224 0.0209 -0.1886 0.091 Uiso 1 calc . . C244 C 0.9084(25) 0.0289(8) -0.3255(25) 0.068(10) Uiso 1 d . . H244 H 0.9277 0.0097 -0.3367 0.081 Uiso 1 calc . . C245 C 0.8821(24) 0.0504(7) -0.3960(23) 0.060(9) Uiso 1 d . . H245 H 0.8816 0.0455 -0.4568 0.072 Uiso 1 calc . . C246 C 0.8558(20) 0.0795(6) -0.3800(19) 0.038(8) Uiso 1 d . . H246 H 0.8396 0.0942 -0.4291 0.045 Uiso 1 calc . . C311 C 0.5416(21) 0.1441(6) 0.0204(20) 0.043(8) Uiso 1 d . . C312 C 0.4827(26) 0.1491(8) 0.0736(24) 0.070(10) Uiso 1 d . . H312 H 0.4761 0.1331 0.1111 0.084 Uiso 1 calc . . C313 C 0.4336(26) 0.1762(8) 0.0747(26) 0.074(11) Uiso 1 d . . H313 H 0.3958 0.1782 0.1116 0.089 Uiso 1 calc . . C314 C 0.4422(28) 0.1993(9) 0.0215(27) 0.080(11) Uiso 1 d . . H314 H 0.4091 0.2176 0.0199 0.096 Uiso 1 calc . . C315 C 0.5016(27) 0.1962(8) -0.0330(25) 0.073(11) Uiso 1 d . . H315 H 0.5074 0.2123 -0.0708 0.087 Uiso 1 calc . . C316 C 0.5500(21) 0.1693(6) -0.0288(20) 0.042(8) Uiso 1 d . . H316 H 0.5919 0.1680 -0.0619 0.051 Uiso 1 calc . . C321 C 0.5022(18) 0.0828(5) -0.0203(17) 0.025(7) Uiso 1 d . . C322 C 0.4229(20) 0.0878(6) -0.1080(19) 0.038(8) Uiso 1 d . . H322 H 0.4184 0.1056 -0.1431 0.045 Uiso 1 calc . . C323 C 0.3492(23) 0.0659(7) -0.1441(22) 0.056(9) Uiso 1 d . . H323 H 0.2992 0.0688 -0.2081 0.067 Uiso 1 calc . . C324 C 0.3412(23) 0.0411(7) -0.0978(23) 0.055(9) Uiso 1 d . . H324 H 0.2838 0.0286 -0.1233 0.065 Uiso 1 calc . . C325 C 0.4220(25) 0.0351(7) -0.0109(24) 0.066(10) Uiso 1 d . . H325 H 0.4223 0.0173 0.0231 0.079 Uiso 1 calc . . C326 C 0.5066(21) 0.0554(6) 0.0295(20) 0.043(8) Uiso 1 d . . H326 H 0.5635 0.0507 0.0876 0.051 Uiso 1 calc . . C331 C 0.4896(16) 0.1222(5) -0.3048(16) 0.018(6) Uiso 1 d . . C332 C 0.4818(19) 0.1533(6) -0.2872(18) 0.034(7) Uiso 1 d . . H332 H 0.5392 0.1649 -0.2497 0.041 Uiso 1 calc . . C333 C 0.3835(22) 0.1660(6) -0.3291(21) 0.046(8) Uiso 1 d . . H333 H 0.3750 0.1865 -0.3200 0.055 Uiso 1 calc . . C334 C 0.3011(22) 0.1489(7) -0.3822(21) 0.047(8) Uiso 1 d . . H334 H 0.2365 0.1578 -0.4084 0.057 Uiso 1 calc . . C335 C 0.3100(22) 0.1190(7) -0.3985(20) 0.050(8) Uiso 1 d . . H335 H 0.2526 0.1076 -0.4375 0.060 Uiso 1 calc . . C336 C 0.4035(19) 0.1060(6) -0.3572(18) 0.032(7) Uiso 1 d . . H336 H 0.4092 0.0852 -0.3649 0.038 Uiso 1 calc . . C341 C 0.5987(19) 0.0662(6) -0.2828(19) 0.036(7) Uiso 1 d . . C342 C 0.6058(22) 0.0558(7) -0.3659(21) 0.050(9) Uiso 1 d . . H342 H 0.6179 0.0691 -0.4080 0.060 Uiso 1 calc . . C343 C 0.5941(24) 0.0242(7) -0.3862(23) 0.061(10) Uiso 1 d . . H343 H 0.6046 0.0163 -0.4388 0.074 Uiso 1 calc . . C344 C 0.5683(23) 0.0061(7) -0.3301(22) 0.054(9) Uiso 1 d . . H344 H 0.5547 -0.0143 -0.3472 0.065 Uiso 1 calc . . C345 C 0.5613(21) 0.0165(7) -0.2490(20) 0.044(8) Uiso 1 d . . H345 H 0.5446 0.0032 -0.2097 0.053 Uiso 1 calc . . C346 C 0.5780(19) 0.0458(6) -0.2240(19) 0.034(7) Uiso 1 d . . H346 H 0.5756 0.0525 -0.1660 0.040 Uiso 1 calc . . C1 C 0.7386(30) -0.0043(9) 0.3583(28) 0.091(13) Uiso 1 d . . H1A H 0.6809 -0.0075 0.2949 0.109 Uiso 1 calc . . H1B H 0.7381 0.0168 0.3767 0.109 Uiso 1 calc . . Cl1 Cl 0.7274(9) -0.0281(3) 0.4477(9) 0.116(4) Uiso 1 d . . Cl2 Cl 0.8505(9) -0.0122(3) 0.3492(9) 0.113(4) Uiso 1 d . . C2 C 1.4557(39) 0.2061(12) 0.4801(38) 0.140(19) Uiso 1 d . . H2A H 1.3929 0.2049 0.4889 0.168 Uiso 1 calc . . H2B H 1.4437 0.2196 0.4250 0.168 Uiso 1 calc . . Cl3 Cl 1.4860(10) 0.1714(3) 0.4540(10) 0.133(5) Uiso 1 d . . Cl4 Cl 1.5517(13) 0.2207(4) 0.5850(12) 0.172(6) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0281(6) 0.0297(6) 0.0234(6) -0.0011(5) 0.0134(5) -0.0046(5) Hg2 0.0295(6) 0.0272(6) 0.0228(6) -0.0002(5) 0.0128(5) -0.0003(5) Hg3 0.0281(6) 0.0293(6) 0.0217(6) -0.0002(5) 0.0135(5) -0.0008(5) P12 0.027(4) 0.024(4) 0.034(5) -0.002(4) 0.013(4) -0.010(3) P13 0.030(4) 0.035(5) 0.026(4) -0.009(4) 0.017(4) -0.006(4) P21 0.028(4) 0.026(4) 0.030(4) -0.002(3) 0.014(4) -0.005(3) P23 0.033(4) 0.026(4) 0.022(4) 0.003(3) 0.016(3) 0.002(3) P31 0.028(4) 0.030(4) 0.028(4) 0.001(3) 0.020(4) 0.006(3) P32 0.028(4) 0.032(5) 0.021(4) -0.001(3) 0.009(3) 0.001(3) P1 0.058(6) 0.060(6) 0.047(6) 0.009(5) 0.024(5) 0.009(5) P2 0.047(5) 0.024(5) 0.054(6) -0.001(4) 0.024(5) 0.005(4) P3 0.046(6) 0.062(6) 0.034(5) 0.002(5) 0.023(4) -0.005(5) P4 0.086(8) 0.043(7) 0.078(7) -0.028(5) 0.049(6) -0.032(5) F1 0.221(30) 0.091(18) 0.088(17) -0.013(14) 0.074(19) -0.040(18) F2 0.054(13) 0.051(12) 0.161(21) -0.012(13) 0.034(13) 0.002(10) F3 0.106(16) 0.065(14) 0.048(12) -0.005(10) -0.001(11) -0.020(12) F4 0.093(15) 0.054(12) 0.051(12) -0.007(10) 0.004(11) -0.022(11) F5 0.258(36) 0.232(34) 0.151(25) -0.097(24) 0.177(28) -0.139(29) F6 0.081(16) 0.064(15) 0.124(19) -0.031(13) -0.030(14) -0.009(12) F7 0.131(18) 0.062(13) 0.087(15) 0.019(12) 0.064(14) -0.006(13) F8 0.164(24) 0.047(13) 0.217(29) 0.033(16) 0.121(23) 0.036(15) F9 0.177(26) 0.058(15) 0.129(21) -0.041(15) 0.024(18) -0.020(16) F10 0.129(18) 0.029(11) 0.109(16) -0.019(11) 0.065(14) -0.015(11) F11 0.190(26) 0.082(16) 0.086(16) -0.023(13) 0.070(17) -0.051(17) F12 0.116(22) 0.113(22) 0.212(32) -0.010(22) -0.024(22) 0.061(18) F13 0.048(12) 0.132(18) 0.058(12) 0.028(12) 0.022(10) -0.019(11) F14 0.101(15) 0.066(13) 0.045(11) -0.019(10) 0.015(11) 0.010(11) F15 0.071(12) 0.051(11) 0.054(11) 0.020(9) 0.028(10) 0.015(9) F16 0.041(11) 0.087(14) 0.095(14) 0.016(11) 0.041(11) 0.003(10) F17 0.130(17) 0.056(12) 0.045(11) -0.016(10) 0.041(12) -0.004(11) F18 0.071(12) 0.070(12) 0.043(10) 0.013(9) 0.034(10) 0.022(10) F19 0.408(57) 0.209(35) 0.172(31) 0.054(26) 0.238(39) 0.124(37) F20 0.112(22) 0.100(20) 0.248(36) 0.036(22) 0.061(24) -0.002(17) F21 0.196(27) 0.051(15) 0.108(19) -0.018(13) 0.017(18) -0.034(16) F22 0.261(41) 0.337(50) 0.106(23) 0.006(27) 0.118(27) 0.143(37) F23 0.127(25) 0.239(38) 0.225(37) 0.032(30) -0.010(25) -0.121(27) F24 0.148(23) 0.039(14) 0.226(31) -0.015(17) 0.049(22) -0.015(14) _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 Hg1 P12 2.516(7) . ? Hg1 P13 2.519(7) . ? Hg1 Hg3 2.795(2) . ? Hg1 Hg2 2.8071(15) . ? Hg1 F4 2.91(2) . ? Hg1 F1 2.99(2) . ? Hg2 P21 2.491(7) . ? Hg2 P23 2.517(7) . ? Hg2 F2 2.79(2) . ? Hg2 Hg3 2.817(2) . ? Hg2 F5 4.01(3) . ? Hg3 P31 2.528(6) . ? Hg3 P32 2.528(7) . ? Hg3 F6 2.80(2) . ? Hg3 F3 3.13(2) . ? P12 C121 1.79(3) . ? P12 C111 1.83(2) . ? P12 C12 1.86(3) . ? P13 C131 1.78(3) . ? P13 C13 1.81(3) . ? P13 C141 1.83(3) . ? P21 C221 1.75(3) . ? P21 C211 1.82(3) . ? P21 C12 1.82(3) . ? P23 C23 1.78(2) . ? P23 C231 1.79(3) . ? P23 C241 1.80(3) . ? P31 C311 1.74(3) . ? P31 C321 1.79(2) . ? P31 C13 1.85(3) . ? P32 C341 1.78(3) . ? P32 C331 1.81(2) . ? P32 C23 1.87(2) . ? P1 F8 1.55(2) . ? P1 F2 1.56(2) . ? P1 F7 1.57(2) . ? P1 F1 1.58(2) . ? P1 F9 1.58(2) . ? P1 F3 1.60(2) . ? P2 F12 1.49(2) . ? P2 F5 1.52(2) . ? P2 F6 1.57(2) . ? P2 F10 1.57(2) . ? P2 F11 1.60(2) . ? P2 F4 1.61(2) . ? P3 F16 1.57(2) . ? P3 F13 1.58(2) . ? P3 F14 1.58(2) . ? P3 F17 1.60(2) . ? P3 F18 1.60(2) . ? P3 F15 1.61(2) . ? P4 F23 1.46(3) . ? P4 F19 1.49(2) . ? P4 F22 1.51(3) . ? P4 F24 1.53(2) . ? P4 F20 1.58(3) . ? P4 F21 1.59(2) . ? C111 C112 1.34(3) . ? C111 C116 1.40(3) . ? C112 C113 1.36(4) . ? C113 C114 1.42(4) . ? C114 C115 1.33(4) . ? C115 C116 1.43(4) . ? C121 C122 1.35(4) . ? C121 C126 1.37(4) . ? C122 C123 1.43(4) . ? C123 C124 1.36(4) . ? C124 C125 1.39(4) . ? C125 C126 1.42(4) . ? C131 C136 1.35(4) . ? C131 C132 1.41(4) . ? C132 C133 1.46(6) . ? C133 C134 1.36(5) . ? C134 C135 1.29(5) . ? C135 C136 1.46(5) . ? C141 C142 1.37(4) . ? C141 C146 1.42(4) . ? C142 C143 1.43(4) . ? C143 C144 1.33(4) . ? C144 C145 1.30(4) . ? C145 C146 1.49(4) . ? C211 C216 1.31(3) . ? C211 C212 1.42(4) . ? C212 C213 1.43(4) . ? C213 C214 1.36(4) . ? C214 C215 1.35(4) . ? C215 C216 1.41(4) . ? C221 C226 1.41(3) . ? C221 C222 1.46(4) . ? C222 C223 1.36(4) . ? C223 C224 1.32(4) . ? C224 C225 1.40(4) . ? C225 C226 1.39(4) . ? C231 C232 1.34(5) . ? C231 C236 1.37(4) . ? C232 C233 1.51(6) . ? C233 C234 1.27(5) . ? C234 C235 1.33(5) . ? C235 C236 1.53(5) . ? C241 C242 1.35(4) . ? C241 C246 1.38(3) . ? C242 C243 1.40(4) . ? C243 C244 1.37(4) . ? C244 C245 1.36(4) . ? C245 C246 1.40(4) . ? C311 C316 1.38(4) . ? C311 C312 1.42(4) . ? C312 C313 1.40(5) . ? C313 C314 1.34(5) . ? C314 C315 1.43(5) . ? C315 C316 1.38(4) . ? C321 C322 1.36(3) . ? C321 C326 1.42(3) . ? C322 C323 1.38(4) . ? C323 C324 1.34(4) . ? C324 C325 1.37(4) . ? C325 C326 1.44(4) . ? C331 C336 1.37(3) . ? C331 C332 1.42(3) . ? C332 C333 1.41(4) . ? C333 C334 1.36(4) . ? C334 C335 1.37(4) . ? C335 C336 1.36(3) . ? C341 C342 1.38(4) . ? C341 C346 1.39(3) . ? C342 C343 1.43(4) . ? C343 C344 1.33(4) . ? C344 C345 1.35(4) . ? C345 C346 1.34(4) . ? C1 Cl2 1.73(4) . ? C1 Cl1 1.78(4) . ? C2 Cl3 1.70(5) . ? C2 Cl4 1.73(5) . ? 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 P12 Hg1 P13 110.3(2) . . ? P12 Hg1 Hg3 155.1(2) . . ? P13 Hg1 Hg3 94.4(2) . . ? P12 Hg1 Hg2 94.9(2) . . ? P13 Hg1 Hg2 154.8(2) . . ? Hg3 Hg1 Hg2 60.37(4) . . ? P12 Hg1 F4 108.2(4) . . ? P13 Hg1 F4 81.0(4) . . ? Hg3 Hg1 F4 77.8(3) . . ? Hg2 Hg1 F4 91.3(4) . . ? P12 Hg1 F1 92.6(5) . . ? P13 Hg1 F1 103.4(5) . . ? Hg3 Hg1 F1 78.4(5) . . ? Hg2 Hg1 F1 74.7(4) . . ? F4 Hg1 F1 156.0(5) . . ? P21 Hg2 P23 116.4(2) . . ? P21 Hg2 F2 79.0(4) . . ? P23 Hg2 F2 97.7(5) . . ? P21 Hg2 Hg1 90.4(2) . . ? P23 Hg2 Hg1 153.1(2) . . ? F2 Hg2 Hg1 86.2(5) . . ? P21 Hg2 Hg3 149.3(2) . . ? P23 Hg2 Hg3 93.8(2) . . ? F2 Hg2 Hg3 103.5(4) . . ? Hg1 Hg2 Hg3 59.60(4) . . ? P21 Hg2 F5 103.5(5) . . ? P23 Hg2 F5 96.3(4) . . ? F2 Hg2 F5 162.8(6) . . ? Hg1 Hg2 F5 76.8(3) . . ? Hg3 Hg2 F5 65.6(5) . . ? P31 Hg3 P32 114.7(2) . . ? P31 Hg3 Hg1 91.6(2) . . ? P32 Hg3 Hg1 153.6(2) . . ? P31 Hg3 F6 72.5(6) . . ? P32 Hg3 F6 101.0(4) . . ? Hg1 Hg3 F6 88.9(4) . . ? P31 Hg3 Hg2 151.6(2) . . ? P32 Hg3 Hg2 93.6(2) . . ? Hg1 Hg3 Hg2 60.03(4) . . ? F6 Hg3 Hg2 105.9(5) . . ? P31 Hg3 F3 119.8(4) . . ? P32 Hg3 F3 78.9(3) . . ? Hg1 Hg3 F3 85.9(3) . . ? F6 Hg3 F3 166.7(7) . . ? Hg2 Hg3 F3 61.0(4) . . ? C121 P12 C111 110.2(11) . . ? C121 P12 C12 107.3(12) . . ? C111 P12 C12 106.9(11) . . ? C121 P12 Hg1 110.5(9) . . ? C111 P12 Hg1 112.6(8) . . ? C12 P12 Hg1 109.1(9) . . ? C131 P13 C13 106.8(12) . . ? C131 P13 C141 108.1(12) . . ? C13 P13 C141 106.9(13) . . ? C131 P13 Hg1 115.3(9) . . ? C13 P13 Hg1 109.7(9) . . ? C141 P13 Hg1 109.5(9) . . ? C221 P21 C211 106.7(12) . . ? C221 P21 C12 107.8(12) . . ? C211 P21 C12 103.2(12) . . ? C221 P21 Hg2 110.2(9) . . ? C211 P21 Hg2 118.3(9) . . ? C12 P21 Hg2 110.1(9) . . ? C23 P23 C231 104.2(12) . . ? C23 P23 C241 109.1(12) . . ? C231 P23 C241 110.5(12) . . ? C23 P23 Hg2 110.4(8) . . ? C231 P23 Hg2 114.9(9) . . ? C241 P23 Hg2 107.7(8) . . ? C311 P31 C321 104.5(12) . . ? C311 P31 C13 107.7(13) . . ? C321 P31 C13 107.6(12) . . ? C311 P31 Hg3 110.0(10) . . ? C321 P31 Hg3 116.6(8) . . ? C13 P31 Hg3 110.0(9) . . ? C341 P32 C331 107.5(11) . . ? C341 P32 C23 111.5(12) . . ? C331 P32 C23 103.5(11) . . ? C341 P32 Hg3 113.1(9) . . ? C331 P32 Hg3 112.6(8) . . ? C23 P32 Hg3 108.3(8) . . ? F8 P1 F2 173.6(15) . . ? F8 P1 F7 90.8(13) . . ? F2 P1 F7 92.7(12) . . ? F8 P1 F1 89.6(15) . . ? F2 P1 F1 86.5(14) . . ? F7 P1 F1 176.3(13) . . ? F8 P1 F9 85.3(14) . . ? F2 P1 F9 89.5(13) . . ? F7 P1 F9 89.3(13) . . ? F1 P1 F9 87.1(13) . . ? F8 P1 F3 91.8(13) . . ? F2 P1 F3 93.3(11) . . ? F7 P1 F3 93.8(11) . . ? F1 P1 F3 89.8(11) . . ? F9 P1 F3 175.8(15) . . ? F12 P2 F5 94.6(21) . . ? F12 P2 F6 173.6(19) . . ? F5 P2 F6 91.3(18) . . ? F12 P2 F10 93.3(13) . . ? F5 P2 F10 90.3(13) . . ? F6 P2 F10 89.0(11) . . ? F12 P2 F11 86.6(18) . . ? F5 P2 F11 178.5(17) . . ? F6 P2 F11 87.5(14) . . ? F10 P2 F11 88.7(11) . . ? F12 P2 F4 90.6(13) . . ? F5 P2 F4 90.7(13) . . ? F6 P2 F4 87.0(10) . . ? F10 P2 F4 175.9(12) . . ? F11 P2 F4 90.2(11) . . ? F16 P3 F13 179.5(11) . . ? F16 P3 F14 90.2(11) . . ? F13 P3 F14 89.3(11) . . ? F16 P3 F17 90.2(11) . . ? F13 P3 F17 90.3(11) . . ? F14 P3 F17 179.0(11) . . ? F16 P3 F18 90.5(10) . . ? F13 P3 F18 89.6(10) . . ? F14 P3 F18 90.3(10) . . ? F17 P3 F18 90.6(9) . . ? F16 P3 F15 89.4(10) . . ? F13 P3 F15 90.5(10) . . ? F14 P3 F15 88.0(9) . . ? F17 P3 F15 91.1(10) . . ? F18 P3 F15 178.4(10) . . ? F23 P4 F19 93.2(24) . . ? F23 P4 F22 92.4(23) . . ? F19 P4 F22 174.4(25) . . ? F23 P4 F24 91.7(20) . . ? F19 P4 F24 90.4(18) . . ? F22 P4 F24 89.4(19) . . ? F23 P4 F20 176.0(19) . . ? F19 P4 F20 89.7(21) . . ? F22 P4 F20 84.7(20) . . ? F24 P4 F20 91.0(14) . . ? F23 P4 F21 92.3(19) . . ? F19 P4 F21 91.5(16) . . ? F22 P4 F21 88.4(18) . . ? F24 P4 F21 175.5(15) . . ? F20 P4 F21 84.9(14) . . ? P1 F1 Hg1 134.0(14) . . ? P1 F2 Hg2 113.2(9) . . ? P1 F3 Hg3 128.0(9) . . ? P2 F4 Hg1 142.9(9) . . ? P2 F5 Hg2 116.6(15) . . ? P2 F6 Hg3 131.1(12) . . ? P21 C12 P12 113.2(14) . . ? P13 C13 P31 113.9(15) . . ? P23 C23 P32 119.1(13) . . ? C112 C111 C116 122.9(24) . . ? C112 C111 P12 122.2(20) . . ? C116 C111 P12 114.8(19) . . ? C111 C112 C113 121.2(27) . . ? C112 C113 C114 118.1(30) . . ? C115 C114 C113 120.5(29) . . ? C114 C115 C116 122.1(27) . . ? C111 C116 C115 115.0(24) . . ? C122 C121 C126 118.3(26) . . ? C122 C121 P12 121.4(22) . . ? C126 C121 P12 120.2(21) . . ? C121 C122 C123 124.7(30) . . ? C124 C123 C122 115.2(32) . . ? C123 C124 C125 122.3(33) . . ? C124 C125 C126 119.3(33) . . ? C121 C126 C125 119.9(28) . . ? C136 C131 C132 119.2(29) . . ? C136 C131 P13 121.0(22) . . ? C132 C131 P13 119.8(24) . . ? C131 C132 C133 116.0(37) . . ? C134 C133 C132 121.9(45) . . ? C135 C134 C133 121.2(45) . . ? C134 C135 C136 119.5(38) . . ? C131 C136 C135 121.7(30) . . ? C142 C141 C146 123.4(26) . . ? C142 C141 P13 121.3(21) . . ? C146 C141 P13 114.7(21) . . ? C141 C142 C143 117.5(26) . . ? C144 C143 C142 122.0(30) . . ? C145 C144 C143 120.4(32) . . ? C144 C145 C146 124.7(31) . . ? C141 C146 C145 111.9(27) . . ? C216 C211 C212 120.8(28) . . ? C216 C211 P21 122.8(23) . . ? C212 C211 P21 116.2(22) . . ? C211 C212 C213 117.3(29) . . ? C214 C213 C212 118.2(32) . . ? C215 C214 C213 124.2(34) . . ? C214 C215 C216 116.5(31) . . ? C211 C216 C215 123.0(28) . . ? C226 C221 C222 115.6(24) . . ? C226 C221 P21 121.6(20) . . ? C222 C221 P21 122.7(20) . . ? C223 C222 C221 116.6(28) . . ? C224 C223 C222 128.4(32) . . ? C223 C224 C225 116.7(32) . . ? C226 C225 C224 119.5(30) . . ? C225 C226 C221 123.2(26) . . ? C232 C231 C236 120.3(31) . . ? C232 C231 P23 122.7(27) . . ? C236 C231 P23 116.9(22) . . ? C231 C232 C233 120.0(39) . . ? C234 C233 C232 120.5(44) . . ? C233 C234 C235 121.0(42) . . ? C234 C235 C236 120.4(37) . . ? C231 C236 C235 116.0(31) . . ? C242 C241 C246 117.7(25) . . ? C242 C241 P23 119.3(21) . . ? C246 C241 P23 123.0(20) . . ? C241 C242 C243 123.3(29) . . ? C244 C243 C242 118.2(33) . . ? C245 C244 C243 119.6(34) . . ? C244 C245 C246 121.3(31) . . ? C241 C246 C245 119.8(26) . . ? C316 C311 C312 113.0(27) . . ? C316 C311 P31 123.8(23) . . ? C312 C311 P31 123.1(24) . . ? C313 C312 C311 125.0(32) . . ? C314 C313 C312 118.2(35) . . ? C313 C314 C315 120.3(36) . . ? C316 C315 C314 118.7(32) . . ? C315 C316 C311 124.8(29) . . ? C322 C321 C326 119.1(23) . . ? C322 C321 P31 118.1(19) . . ? C326 C321 P31 122.6(19) . . ? C321 C322 C323 118.0(26) . . ? C324 C323 C322 126.9(29) . . ? C323 C324 C325 115.7(30) . . ? C324 C325 C326 121.2(30) . . ? C321 C326 C325 118.5(25) . . ? C336 C331 C332 119.6(22) . . ? C336 C331 P32 122.3(18) . . ? C332 C331 P32 118.1(18) . . ? C333 C332 C331 116.7(23) . . ? C334 C333 C332 121.0(27) . . ? C333 C334 C335 121.5(28) . . ? C336 C335 C334 118.8(27) . . ? C335 C336 C331 122.2(24) . . ? C342 C341 C346 118.8(26) . . ? C342 C341 P32 120.4(22) . . ? C346 C341 P32 120.8(21) . . ? C341 C342 C343 118.4(28) . . ? C344 C343 C342 119.7(30) . . ? C343 C344 C345 121.2(30) . . ? C346 C345 C344 120.7(28) . . ? C345 C346 C341 120.9(26) . . ? Cl2 C1 Cl1 109.5(22) . . ? Cl3 C2 Cl4 111.4(30) . . ? _refine_diff_density_max 2.077 _refine_diff_density_min -1.584 _refine_diff_density_rms 0.206 #===END data_4MeOH _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C80 H70 F12 Hg3 O13 P6 S4' _chemical_formula_weight 2383.19 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.831(5) _cell_length_b 15.045(5) _cell_length_c 23.190(5) _cell_angle_alpha 100.74(3) _cell_angle_beta 96.81(4) _cell_angle_gamma 112.99(4) _cell_volume 4574.1(24) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 12.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method ? _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 5.299 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Disordering of outward CF3SO3-anions, S3:S4:S5 = 0.75:0.75:0.5; a restraint for the S=O7-bond was used and for C4 all bonds were restrained; S5 lies nearby a symmetry center, the center is in the middle of the C-S bond. ; _diffrn_ambient_temperature 188(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7223 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 20.00 _reflns_number_total 6887 _reflns_number_observed 5261 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 484 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+186.9466P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6403 _refine_ls_number_parameters 629 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_obs 0.0690 _refine_ls_wR_factor_all 0.2137 _refine_ls_wR_factor_obs 0.1473 _refine_ls_goodness_of_fit_all 1.104 _refine_ls_goodness_of_fit_obs 1.158 _refine_ls_restrained_S_all 1.460 _refine_ls_restrained_S_obs 1.158 _refine_ls_shift/esd_max -0.014 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg1 Hg 0.22324(8) 0.34129(7) 0.26086(5) 0.0466(4) Uani 1 d . . Hg2 Hg 0.18552(8) 0.50194(7) 0.25309(4) 0.0388(3) Uani 1 d . . Hg3 Hg 0.37686(9) 0.51240(8) 0.25278(5) 0.0510(4) Uani 1 d . . P12 P 0.0443(5) 0.2340(4) 0.2596(3) 0.039(2) Uani 1 d . . P13 P 0.3306(5) 0.2522(4) 0.2758(3) 0.037(2) Uani 1 d . . P21 P -0.0024(5) 0.4099(4) 0.2435(3) 0.035(2) Uani 1 d . . P23 P 0.2393(5) 0.6849(4) 0.2665(3) 0.030(2) Uani 1 d . . P31 P 0.5053(5) 0.4457(5) 0.2711(3) 0.047(2) Uani 1 d . . P32 P 0.4395(5) 0.6892(5) 0.2433(3) 0.036(2) Uani 1 d . . S1 S 0.3537(6) 0.5538(5) 0.4013(3) 0.046(2) Uani 1 d . . S2 S 0.1599(7) 0.3435(6) 0.1076(3) 0.062(2) Uani 1 d . . F1 F 0.4118(24) 0.7055(21) 0.4904(10) 0.177(12) Uani 1 d . . F2 F 0.4879(24) 0.6124(20) 0.4987(9) 0.154(11) Uani 1 d . . F3 F 0.3395(28) 0.5682(29) 0.5125(11) 0.211(17) Uani 1 d . . F4 F 0.1227(28) 0.3472(28) -0.0015(11) 0.210(15) Uani 1 d . . F5 F 0.1149(22) 0.2052(20) 0.0097(9) 0.154(11) Uani 1 d . . F6 F -0.0056(22) 0.2540(24) 0.0303(11) 0.177(13) Uani 1 d . . O1 O 0.3555(16) 0.4569(14) 0.3940(10) 0.086(7) Uani 1 d . . O2 O 0.2554(15) 0.5539(14) 0.3876(9) 0.070(6) Uani 1 d . . O3 O 0.4238(13) 0.6162(13) 0.3732(8) 0.061(5) Uani 1 d . . O4 O 0.1235(16) 0.2685(12) 0.1371(8) 0.072(6) Uani 1 d . . O5 O 0.1337(14) 0.4252(14) 0.1240(9) 0.068(6) Uani 1 d . . O6 O 0.2640(19) 0.3713(17) 0.1064(12) 0.105(8) Uani 1 d . . C1 C 0.3990(41) 0.6096(32) 0.4814(16) 0.099(13) Uani 1 d . . C2 C 0.0925(41) 0.2879(40) 0.0326(21) 0.127(17) Uani 1 d . . C12 C -0.0353(19) 0.2783(18) 0.2163(11) 0.048(7) Uiso 1 d . . H12A H -0.0296 0.2646 0.1737 0.058 Uiso 1 calc . . H12B H -0.1061 0.2400 0.2178 0.058 Uiso 1 calc . . C13 C 0.4593(18) 0.3467(17) 0.3090(10) 0.041(7) Uiso 1 d . . H13A H 0.4625 0.3771 0.3514 0.049 Uiso 1 calc . . H13B H 0.5047 0.3129 0.3091 0.049 Uiso 1 calc . . C23 C 0.3778(18) 0.7473(17) 0.2886(10) 0.041(7) Uiso 1 d . . H23A H 0.4007 0.8175 0.2862 0.049 Uiso 1 calc . . H23B H 0.3983 0.7480 0.3309 0.049 Uiso 1 calc . . C111 C 0.0057(18) 0.1022(17) 0.2247(11) 0.043(7) Uiso 1 d . . C112 C -0.0353(24) 0.0635(23) 0.1649(14) 0.077(10) Uiso 1 d . . H112 H -0.0483 0.1028 0.1402 0.093 Uiso 1 calc . . C113 C -0.0576(24) -0.0393(24) 0.1409(14) 0.079(10) Uiso 1 d . . H113 H -0.0931 -0.0715 0.1006 0.095 Uiso 1 calc . . C114 C -0.0291(26) -0.0909(25) 0.1748(16) 0.090(11) Uiso 1 d . . H114 H -0.0371 -0.1563 0.1565 0.108 Uiso 1 calc . . C115 C 0.0100(24) -0.0531(23) 0.2335(15) 0.081(10) Uiso 1 d . . H115 H 0.0269 -0.0908 0.2579 0.097 Uiso 1 calc . . C116 C 0.0255(23) 0.0502(23) 0.2581(14) 0.076(9) Uiso 1 d . . H116 H 0.0509 0.0795 0.3000 0.092 Uiso 1 calc . . C121 C 0.0116(19) 0.2432(17) 0.3328(11) 0.041(7) Uiso 1 d . . C122 C -0.0804(23) 0.1798(21) 0.3409(14) 0.069(9) Uiso 1 d . . H122 H -0.1274 0.1299 0.3073 0.082 Uiso 1 calc . . C123 C -0.1060(28) 0.1869(27) 0.3965(17) 0.099(12) Uiso 1 d . . H123 H -0.1693 0.1445 0.4024 0.119 Uiso 1 calc . . C124 C -0.0347(31) 0.2582(29) 0.4410(18) 0.106(12) Uiso 1 d . . H124 H -0.0508 0.2642 0.4795 0.127 Uiso 1 calc . . C125 C 0.0549(26) 0.3210(23) 0.4385(14) 0.079(10) Uiso 1 d . . H125 H 0.0997 0.3715 0.4726 0.095 Uiso 1 calc . . C126 C 0.0814(23) 0.3083(22) 0.3796(14) 0.072(9) Uiso 1 d . . H126 H 0.1473 0.3460 0.3750 0.087 Uiso 1 calc . . C131 C 0.3304(20) 0.1725(18) 0.2067(11) 0.046(7) Uiso 1 d . . C132 C 0.2515(21) 0.1435(20) 0.1598(13) 0.059(8) Uiso 1 d . . H132 H 0.2006 0.1661 0.1643 0.070 Uiso 1 calc . . C133 C 0.2448(26) 0.0801(24) 0.1047(15) 0.088(10) Uiso 1 d . . H133 H 0.1892 0.0555 0.0720 0.105 Uiso 1 calc . . C134 C 0.3263(30) 0.0567(26) 0.1024(17) 0.101(12) Uiso 1 d . . H134 H 0.3263 0.0166 0.0656 0.121 Uiso 1 calc . . C135 C 0.4014(25) 0.0848(23) 0.1459(15) 0.081(10) Uiso 1 d . . H135 H 0.4546 0.0660 0.1405 0.097 Uiso 1 calc . . C136 C 0.4046(22) 0.1437(20) 0.2019(13) 0.062(8) Uiso 1 d . . H136 H 0.4580 0.1624 0.2352 0.074 Uiso 1 calc . . C141 C 0.3007(19) 0.1793(18) 0.3295(11) 0.047(7) Uiso 1 d . . C142 C 0.2944(21) 0.0851(20) 0.3210(12) 0.059(8) Uiso 1 d . . H142 H 0.3103 0.0562 0.2858 0.071 Uiso 1 calc . . C143 C 0.2649(20) 0.0299(19) 0.3629(12) 0.053(8) Uiso 1 d . . H143 H 0.2591 -0.0366 0.3546 0.064 Uiso 1 calc . . C144 C 0.2447(25) 0.0660(25) 0.4138(15) 0.086(10) Uiso 1 d . . H144 H 0.2202 0.0255 0.4404 0.103 Uiso 1 calc . . C145 C 0.2603(33) 0.1624(35) 0.4264(20) 0.134(15) Uiso 1 d . . H145 H 0.2530 0.1933 0.4641 0.161 Uiso 1 calc . . C146 C 0.2890(27) 0.2203(26) 0.3810(17) 0.098(11) Uiso 1 d . . H146 H 0.2990 0.2881 0.3897 0.118 Uiso 1 calc . . C211 C -0.0729(17) 0.4409(16) 0.1868(10) 0.037(6) Uiso 1 d . . C212 C -0.0903(21) 0.3997(19) 0.1285(13) 0.059(8) Uiso 1 d . . H212 H -0.0730 0.3460 0.1152 0.070 Uiso 1 calc . . C213 C -0.1354(23) 0.4359(23) 0.0853(14) 0.077(9) Uiso 1 d . . H213 H -0.1455 0.4090 0.0434 0.092 Uiso 1 calc . . C214 C -0.1627(21) 0.5091(20) 0.1064(13) 0.061(8) Uiso 1 d . . H214 H -0.1965 0.5302 0.0782 0.073 Uiso 1 calc . . C215 C -0.1445(23) 0.5552(21) 0.1663(14) 0.072(9) Uiso 1 d . . H215 H -0.1618 0.6091 0.1791 0.086 Uiso 1 calc . . C216 C -0.0998(19) 0.5202(17) 0.2076(11) 0.045(7) Uiso 1 d . . H216 H -0.0874 0.5493 0.2494 0.054 Uiso 1 calc . . C221 C -0.0529(19) 0.4293(18) 0.3106(11) 0.045(7) Uiso 1 d . . C222 C -0.1490(21) 0.3714(19) 0.3115(12) 0.053(8) Uiso 1 d . . H222 H -0.1914 0.3201 0.2770 0.064 Uiso 1 calc . . C223 C -0.1849(21) 0.3873(20) 0.3629(13) 0.062(8) Uiso 1 d . . H223 H -0.2508 0.3434 0.3641 0.074 Uiso 1 calc . . C224 C -0.1307(26) 0.4612(24) 0.4101(15) 0.082(10) Uiso 1 d . . H224 H -0.1592 0.4754 0.4432 0.099 Uiso 1 calc . . C225 C -0.0279(26) 0.5200(23) 0.4107(15) 0.082(10) Uiso 1 d . . H225 H 0.0142 0.5707 0.4455 0.099 Uiso 1 calc . . C226 C 0.0085(19) 0.5024(18) 0.3613(12) 0.048(7) Uiso 1 d . . H226 H 0.0768 0.5406 0.3614 0.058 Uiso 1 calc . . C231 C 0.2019(18) 0.7247(17) 0.2033(10) 0.038(7) Uiso 1 d . . C232 C 0.2275(20) 0.8274(19) 0.2094(12) 0.053(8) Uiso 1 d . . H232 H 0.2669 0.8740 0.2462 0.064 Uiso 1 calc . . C233 C 0.1966(20) 0.8613(19) 0.1628(12) 0.054(8) Uiso 1 d . . H233 H 0.2167 0.9307 0.1668 0.065 Uiso 1 calc . . C234 C 0.1371(20) 0.7937(19) 0.1114(12) 0.051(7) Uiso 1 d . . H234 H 0.1131 0.8165 0.0800 0.062 Uiso 1 calc . . C235 C 0.1105(21) 0.6943(20) 0.1034(12) 0.059(8) Uiso 1 d . . H235 H 0.0713 0.6497 0.0658 0.070 Uiso 1 calc . . C236 C 0.1402(19) 0.6554(18) 0.1502(11) 0.050(7) Uiso 1 d . . H236 H 0.1190 0.5857 0.1454 0.060 Uiso 1 calc . . C241 C 0.1965(18) 0.7417(16) 0.3267(10) 0.035(6) Uiso 1 d . . C242 C 0.1069(20) 0.7498(18) 0.3126(12) 0.052(7) Uiso 1 d . . H242 H 0.0710 0.7293 0.2722 0.062 Uiso 1 calc . . C243 C 0.0699(22) 0.7901(20) 0.3609(13) 0.066(9) Uiso 1 d . . H243 H 0.0125 0.8030 0.3526 0.079 Uiso 1 calc . . C244 C 0.1171(24) 0.8090(21) 0.4171(14) 0.070(9) Uiso 1 d . . H244 H 0.0881 0.8291 0.4485 0.084 Uiso 1 calc . . C245 C 0.2017(23) 0.8015(21) 0.4315(13) 0.067(9) Uiso 1 d . . H245 H 0.2351 0.8228 0.4725 0.080 Uiso 1 calc . . C246 C 0.2451(21) 0.7618(19) 0.3868(12) 0.057(8) Uiso 1 d . . H246 H 0.3027 0.7500 0.3971 0.069 Uiso 1 calc . . C311 C 0.5399(20) 0.3923(18) 0.2041(11) 0.049(7) Uiso 1 d . . C312 C 0.4757(25) 0.3686(24) 0.1503(16) 0.085(10) Uiso 1 d . . H312 H 0.4210 0.3865 0.1470 0.102 Uiso 1 calc . . C313 C 0.4959(29) 0.3155(27) 0.0997(17) 0.102(12) Uiso 1 d . . H313 H 0.4529 0.2961 0.0615 0.122 Uiso 1 calc . . C314 C 0.5749(31) 0.2923(27) 0.1051(18) 0.106(12) Uiso 1 d . . H314 H 0.5889 0.2600 0.0703 0.127 Uiso 1 calc . . C315 C 0.6347(29) 0.3144(28) 0.1595(19) 0.107(12) Uiso 1 d . . H315 H 0.6893 0.2963 0.1630 0.129 Uiso 1 calc . . C316 C 0.6156(23) 0.3627(22) 0.2090(14) 0.071(9) Uiso 1 d . . H316 H 0.6556 0.3759 0.2474 0.085 Uiso 1 calc . . C321 C 0.6230(20) 0.5350(18) 0.3209(12) 0.050(7) Uiso 1 d . . C322 C 0.6380(22) 0.5590(21) 0.3780(13) 0.064(8) Uiso 1 d . . H322 H 0.5846 0.5232 0.3954 0.076 Uiso 1 calc . . C323 C 0.7236(27) 0.6316(25) 0.4173(16) 0.089(11) Uiso 1 d . . H323 H 0.7289 0.6473 0.4596 0.107 Uiso 1 calc . . C324 C 0.7992(29) 0.6789(27) 0.3912(18) 0.102(12) Uiso 1 d . . H324 H 0.8635 0.7222 0.4156 0.122 Uiso 1 calc . . C325 C 0.7859(31) 0.6663(29) 0.3351(20) 0.114(13) Uiso 1 d . . H325 H 0.8362 0.7085 0.3184 0.136 Uiso 1 calc . . C326 C 0.6952(32) 0.5886(30) 0.2959(18) 0.114(13) Uiso 1 d . . H326 H 0.6872 0.5761 0.2535 0.137 Uiso 1 calc . . C331 C 0.4066(18) 0.7010(17) 0.1683(11) 0.043(7) Uiso 1 d . . C332 C 0.4218(19) 0.7922(18) 0.1574(12) 0.050(7) Uiso 1 d . . H332 H 0.4536 0.8516 0.1890 0.061 Uiso 1 calc . . C333 C 0.3906(25) 0.7959(25) 0.1002(16) 0.087(10) Uiso 1 d . . H333 H 0.3958 0.8577 0.0930 0.104 Uiso 1 calc . . C334 C 0.3541(25) 0.7167(26) 0.0558(15) 0.086(10) Uiso 1 d . . H334 H 0.3359 0.7230 0.0166 0.103 Uiso 1 calc . . C335 C 0.3408(25) 0.6260(25) 0.0630(15) 0.086(10) Uiso 1 d . . H335 H 0.3122 0.5695 0.0294 0.104 Uiso 1 calc . . C336 C 0.3705(20) 0.6149(19) 0.1222(12) 0.057(8) Uiso 1 d . . H336 H 0.3655 0.5528 0.1288 0.068 Uiso 1 calc . . C341 C 0.5719(18) 0.7683(16) 0.2721(11) 0.037(6) Uiso 1 d . . C342 C 0.6076(23) 0.7902(21) 0.3316(13) 0.069(9) Uiso 1 d . . H342 H 0.5650 0.7653 0.3579 0.082 Uiso 1 calc . . C343 C 0.7145(26) 0.8538(24) 0.3543(15) 0.083(10) Uiso 1 d . . H343 H 0.7427 0.8697 0.3959 0.099 Uiso 1 calc . . C344 C 0.7729(25) 0.8899(23) 0.3166(16) 0.082(10) Uiso 1 d . . H344 H 0.8426 0.9304 0.3313 0.098 Uiso 1 calc . . C345 C 0.7341(29) 0.8693(27) 0.2600(18) 0.103(12) Uiso 1 d . . H345 H 0.7763 0.8989 0.2347 0.123 Uiso 1 calc . . C346 C 0.6350(24) 0.8069(22) 0.2345(13) 0.071(9) Uiso 1 d . . H346 H 0.6106 0.7907 0.1924 0.085 Uiso 1 calc . . S3 S 0.7270(29) 0.1103(18) 0.0776(11) 0.225(14) Uani 0.75 d PD . C3 C 0.6673(66) -0.0225(63) 0.0746(43) 0.164(28) Uiso 0.75 d P . O7 O 0.7272(86) 0.1277(82) 0.1414(31) 0.421(57) Uiso 0.75 d PD . O8 O 0.6737(35) 0.1191(33) 0.0282(23) 0.171(17) Uiso 0.75 d P . O9 O 0.7896(66) 0.0703(68) 0.0487(42) 0.325(42) Uiso 0.75 d P . F7 F 0.6167(45) -0.0827(45) 0.0296(29) 0.257(24) Uiso 0.75 d P . F8 F 0.6961(39) -0.0452(39) 0.1156(27) 0.236(22) Uiso 0.75 d P . F9 F 0.5762(66) 0.0061(60) 0.0801(37) 0.360(37) Uiso 0.75 d P . S4 S 0.5635(14) 0.0778(14) 0.3218(9) 0.141(6) Uani 0.75 d PD . C4 C 0.5821(72) 0.0658(64) 0.3911(26) 0.445(114) Uiso 0.75 d PD . O10 O 0.5779(35) 0.1738(38) 0.3237(22) 0.177(18) Uiso 0.75 d P . O11 O 0.4746(26) -0.0051(24) 0.2890(15) 0.103(10) Uiso 0.75 d P . O12 O 0.6415(50) 0.0668(44) 0.2996(28) 0.233(25) Uiso 0.75 d P . F10 F 0.5644(42) -0.0157(42) 0.4091(26) 0.268(24) Uiso 0.75 d PD . F11 F 0.6539(49) 0.1450(47) 0.4267(29) 0.285(26) Uiso 0.75 d PD . F12 F 0.5171(38) 0.0926(35) 0.4157(22) 0.222(19) Uiso 0.75 d PD . S5 S -0.0321(22) 0.0175(12) 0.4738(7) 0.158(11) Uani 0.50 d P . C5 C -0.0321(22) 0.0175(12) 0.4738(7) 0.158(11) Uani 0.50 d P . O13 O -0.1270(28) 0.0066(26) 0.4746(16) 0.188(15) Uiso 0.50 d P . F13 F -0.1270(28) 0.0066(26) 0.4746(16) 0.188(15) Uiso 0.50 d P . O14 O 0.0609(23) 0.1261(23) 0.4888(14) 0.166(11) Uiso 0.50 d P . F14 F 0.0609(23) 0.1261(23) 0.4888(14) 0.166(11) Uiso 0.50 d P . O15 O -0.0009(19) -0.0263(18) 0.4183(12) 0.137(9) Uiso 0.50 d P . F15 F -0.0009(19) -0.0263(18) 0.4183(12) 0.137(9) Uiso 0.50 d P . O16 O 0.4346(32) 0.4243(31) -0.0325(19) 0.225(17) Uiso 1 d . . C16 C 0.3322(44) 0.3203(43) -0.0817(27) 0.190(22) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0464(8) 0.0414(6) 0.0497(7) 0.0099(5) 0.0075(6) 0.0178(6) Hg2 0.0372(8) 0.0390(6) 0.0366(6) 0.0085(5) 0.0063(5) 0.0135(6) Hg3 0.0527(9) 0.0519(7) 0.0544(8) 0.0182(6) 0.0167(6) 0.0247(6) P12 0.034(5) 0.025(4) 0.051(4) 0.006(3) 0.010(4) 0.008(3) P13 0.034(5) 0.029(4) 0.055(5) 0.015(3) 0.018(4) 0.016(3) P21 0.026(4) 0.032(4) 0.044(4) 0.007(3) 0.007(3) 0.010(3) P23 0.028(4) 0.034(4) 0.029(4) 0.003(3) 0.009(3) 0.017(3) P31 0.029(5) 0.044(4) 0.059(5) 0.019(4) 0.010(4) 0.005(4) P32 0.033(5) 0.036(4) 0.038(4) 0.007(3) 0.014(3) 0.011(4) S1 0.056(6) 0.044(4) 0.039(4) 0.011(3) 0.005(4) 0.023(4) S2 0.067(7) 0.076(6) 0.054(5) 0.024(4) 0.023(5) 0.036(5) F1 0.285(36) 0.133(21) 0.076(16) -0.047(15) -0.035(19) 0.104(23) F2 0.187(27) 0.190(26) 0.054(14) -0.003(14) -0.059(16) 0.089(23) F3 0.263(39) 0.340(46) 0.073(18) 0.107(24) 0.084(22) 0.134(33) F4 0.330(44) 0.312(40) 0.085(18) 0.118(24) 0.070(23) 0.196(35) F5 0.224(30) 0.144(21) 0.057(14) -0.022(14) 0.014(15) 0.064(22) F6 0.096(20) 0.271(35) 0.092(18) -0.015(19) -0.047(16) 0.052(22) O1 0.096(18) 0.062(14) 0.104(18) 0.016(12) 0.013(14) 0.042(13) O2 0.047(14) 0.081(14) 0.078(15) 0.016(11) 0.008(11) 0.025(12) O3 0.046(13) 0.073(13) 0.053(12) 0.031(11) 0.001(10) 0.010(11) O4 0.134(19) 0.043(11) 0.043(11) 0.021(9) 0.033(12) 0.033(12) O5 0.069(15) 0.084(14) 0.090(15) 0.035(12) 0.023(12) 0.065(13) O6 0.081(20) 0.103(18) 0.150(24) 0.033(16) 0.045(17) 0.051(15) C1 0.138(41) 0.095(31) 0.049(26) -0.006(22) -0.005(29) 0.050(30) C2 0.120(44) 0.160(46) 0.098(38) 0.082(37) 0.014(33) 0.037(38) S3 0.408(43) 0.181(21) 0.134(18) 0.055(15) 0.014(23) 0.181(27) S4 0.118(15) 0.134(15) 0.179(18) 0.026(12) 0.005(13) 0.077(13) S5 0.267(30) 0.077(12) 0.058(11) -0.021(9) 0.059(15) 0.009(14) C5 0.267(30) 0.077(12) 0.058(11) -0.021(9) 0.059(15) 0.009(14) _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 Hg1 P13 2.483(7) . ? Hg1 P12 2.504(7) . ? Hg1 Hg2 2.717(2) . ? Hg1 Hg3 2.748(2) . ? Hg1 O4 2.86(2) . ? Hg1 O1 3.21(2) . ? Hg2 P23 2.494(6) . ? Hg2 P21 2.541(7) . ? Hg2 Hg3 2.781(2) . ? Hg2 O5 2.89(2) . ? Hg2 O2 3.02(2) . ? Hg3 P31 2.505(7) . ? Hg3 P32 2.515(6) . ? Hg3 O3 2.79(2) . ? Hg3 O6 3.47(3) . ? P12 C121 1.81(2) . ? P12 C111 1.82(2) . ? P12 C12 1.85(3) . ? P13 C141 1.79(3) . ? P13 C131 1.81(3) . ? P13 C13 1.84(2) . ? P21 C12 1.81(2) . ? P21 C211 1.82(2) . ? P21 C221 1.83(3) . ? P23 C231 1.79(2) . ? P23 C241 1.81(2) . ? P23 C23 1.85(3) . ? P31 C13 1.82(2) . ? P31 C321 1.82(3) . ? P31 C311 1.84(3) . ? P32 C23 1.79(3) . ? P32 C331 1.81(2) . ? P32 C341 1.81(2) . ? S1 O3 1.42(2) . ? S1 O1 1.45(2) . ? S1 O2 1.45(2) . ? S1 C1 1.81(4) . ? S2 O4 1.39(2) . ? S2 O5 1.43(2) . ? S2 O6 1.44(2) . ? S2 C2 1.77(5) . ? F1 C1 1.35(4) . ? F2 C1 1.31(5) . ? F3 C1 1.25(5) . ? F4 C2 1.29(4) . ? F5 C2 1.44(5) . ? F6 C2 1.33(5) . ? C111 C116 1.29(3) . ? C111 C112 1.36(4) . ? C112 C113 1.43(4) . ? C113 C114 1.34(4) . ? C114 C115 1.33(4) . ? C115 C116 1.47(4) . ? C121 C126 1.32(3) . ? C121 C122 1.39(3) . ? C122 C123 1.38(4) . ? C123 C124 1.33(4) . ? C124 C125 1.31(4) . ? C125 C126 1.47(4) . ? C131 C136 1.34(3) . ? C131 C132 1.36(3) . ? C132 C133 1.41(4) . ? C133 C134 1.39(4) . ? C134 C135 1.28(4) . ? C135 C136 1.41(4) . ? C141 C146 1.30(4) . ? C141 C142 1.36(3) . ? C142 C143 1.39(3) . ? C143 C144 1.32(4) . ? C144 C145 1.34(5) . ? C145 C146 1.49(5) . ? C211 C212 1.33(3) . ? C211 C216 1.42(3) . ? C212 C213 1.44(4) . ? C213 C214 1.35(4) . ? C214 C215 1.37(4) . ? C215 C216 1.39(3) . ? C221 C222 1.35(3) . ? C221 C226 1.38(3) . ? C222 C223 1.38(4) . ? C223 C224 1.31(4) . ? C224 C225 1.43(4) . ? C225 C226 1.35(4) . ? C231 C236 1.40(3) . ? C231 C232 1.41(3) . ? C232 C233 1.38(3) . ? C233 C234 1.35(3) . ? C234 C235 1.36(3) . ? C235 C236 1.43(3) . ? C241 C242 1.39(3) . ? C241 C246 1.41(3) . ? C242 C243 1.44(4) . ? C243 C244 1.33(4) . ? C244 C245 1.31(4) . ? C245 C246 1.44(4) . ? C311 C316 1.36(3) . ? C311 C312 1.37(4) . ? C312 C313 1.42(4) . ? C313 C314 1.35(4) . ? C314 C315 1.36(5) . ? C315 C316 1.36(4) . ? C321 C322 1.27(3) . ? C321 C326 1.33(4) . ? C322 C323 1.38(4) . ? C323 C324 1.35(4) . ? C324 C325 1.26(5) . ? C325 C326 1.45(5) . ? C331 C332 1.38(3) . ? C331 C336 1.38(3) . ? C332 C333 1.37(4) . ? C333 C334 1.30(4) . ? C334 C335 1.35(4) . ? C335 C336 1.45(4) . ? C341 C342 1.35(3) . ? C341 C346 1.39(3) . ? C342 C343 1.46(4) . ? C343 C344 1.34(4) . ? C344 C345 1.30(4) . ? C345 C346 1.38(4) . ? S3 O8 1.37(5) . ? S3 O7 1.45(6) . ? S3 O9 1.45(9) . ? S3 C3 1.83(8) . ? C3 F8 1.16(8) . ? C3 F7 1.18(8) . ? C3 F9 1.58(10) . ? S4 O10 1.37(5) . ? S4 O12 1.37(6) . ? S4 O11 1.41(3) . ? S4 C4 1.65(5) . ? C4 F11 1.29(7) . ? C4 F10 1.31(6) . ? C4 F12 1.33(7) . ? S5 F13 1.35(4) . ? S5 O13 1.35(4) . ? S5 F15 1.54(3) . ? S5 O15 1.54(3) . ? S5 O14 1.61(3) . ? S5 F14 1.61(3) . ? S5 C5 1.74(5) 2_556 ? S5 S5 1.74(5) 2_556 ? C5 F13 1.35(4) . ? C5 O13 1.35(4) . ? C5 F15 1.54(3) . ? C5 O15 1.54(3) . ? C5 O14 1.61(3) . ? C5 F14 1.61(3) . ? C5 C5 1.74(5) 2_556 ? C5 S5 1.74(5) 2_556 ? O16 C16 1.77(6) . ? 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 P13 Hg1 P12 111.2(2) . . ? P13 Hg1 Hg2 155.4(2) . . ? P12 Hg1 Hg2 93.0(2) . . ? P13 Hg1 Hg3 94.8(2) . . ? P12 Hg1 Hg3 154.0(2) . . ? Hg2 Hg1 Hg3 61.17(5) . . ? P13 Hg1 O4 106.5(4) . . ? P12 Hg1 O4 74.3(4) . . ? Hg2 Hg1 O4 83.4(3) . . ? Hg3 Hg1 O4 98.1(4) . . ? P13 Hg1 O1 76.9(4) . . ? P12 Hg1 O1 113.1(4) . . ? Hg2 Hg1 O1 90.0(3) . . ? Hg3 Hg1 O1 72.6(4) . . ? O4 Hg1 O1 170.5(5) . . ? P23 Hg2 P21 111.9(2) . . ? P23 Hg2 Hg1 152.1(2) . . ? P21 Hg2 Hg1 94.63(15) . . ? P23 Hg2 Hg3 94.2(2) . . ? P21 Hg2 Hg3 153.80(15) . . ? Hg1 Hg2 Hg3 59.97(5) . . ? P23 Hg2 O5 103.0(4) . . ? P21 Hg2 O5 82.9(4) . . ? Hg1 Hg2 O5 88.1(3) . . ? Hg3 Hg2 O5 89.4(4) . . ? P23 Hg2 O2 85.4(4) . . ? P21 Hg2 O2 100.2(4) . . ? Hg1 Hg2 O2 81.5(4) . . ? Hg3 Hg2 O2 83.3(4) . . ? O5 Hg2 O2 169.4(5) . . ? P31 Hg3 P32 117.0(2) . . ? P31 Hg3 Hg1 92.9(2) . . ? P32 Hg3 Hg1 150.0(2) . . ? P31 Hg3 Hg2 150.8(2) . . ? P32 Hg3 Hg2 91.1(2) . . ? Hg1 Hg3 Hg2 58.86(5) . . ? P31 Hg3 O3 91.7(4) . . ? P32 Hg3 O3 79.5(4) . . ? Hg1 Hg3 O3 97.3(4) . . ? Hg2 Hg3 O3 85.6(4) . . ? P31 Hg3 O6 97.9(4) . . ? P32 Hg3 O6 103.4(4) . . ? Hg1 Hg3 O6 74.0(4) . . ? Hg2 Hg3 O6 81.9(4) . . ? O3 Hg3 O6 167.2(5) . . ? C121 P12 C111 107.6(11) . . ? C121 P12 C12 104.8(11) . . ? C111 P12 C12 108.1(11) . . ? C121 P12 Hg1 114.6(8) . . ? C111 P12 Hg1 113.4(8) . . ? C12 P12 Hg1 107.7(8) . . ? C141 P13 C131 108.4(12) . . ? C141 P13 C13 103.9(11) . . ? C131 P13 C13 109.1(12) . . ? C141 P13 Hg1 114.0(9) . . ? C131 P13 Hg1 113.2(9) . . ? C13 P13 Hg1 107.8(8) . . ? C12 P21 C211 105.6(11) . . ? C12 P21 C221 109.0(11) . . ? C211 P21 C221 104.9(11) . . ? C12 P21 Hg2 107.2(9) . . ? C211 P21 Hg2 111.8(8) . . ? C221 P21 Hg2 117.7(9) . . ? C231 P23 C241 104.1(11) . . ? C231 P23 C23 107.9(11) . . ? C241 P23 C23 105.0(11) . . ? C231 P23 Hg2 117.2(8) . . ? C241 P23 Hg2 113.8(7) . . ? C23 P23 Hg2 108.2(8) . . ? C13 P31 C321 103.9(12) . . ? C13 P31 C311 105.9(11) . . ? C321 P31 C311 105.4(13) . . ? C13 P31 Hg3 109.7(8) . . ? C321 P31 Hg3 114.9(9) . . ? C311 P31 Hg3 116.1(9) . . ? C23 P32 C331 105.6(11) . . ? C23 P32 C341 104.5(11) . . ? C331 P32 C341 108.0(11) . . ? C23 P32 Hg3 106.1(8) . . ? C331 P32 Hg3 114.6(8) . . ? C341 P32 Hg3 116.9(8) . . ? O3 S1 O1 112.1(13) . . ? O3 S1 O2 112.6(11) . . ? O1 S1 O2 116.2(12) . . ? O3 S1 C1 106.0(19) . . ? O1 S1 C1 103.4(18) . . ? O2 S1 C1 105.3(20) . . ? O4 S2 O5 115.2(12) . . ? O4 S2 O6 111.8(14) . . ? O5 S2 O6 115.0(13) . . ? O4 S2 C2 104.5(18) . . ? O5 S2 C2 102.1(22) . . ? O6 S2 C2 106.7(22) . . ? S1 O1 Hg1 102.3(10) . . ? S1 O2 Hg2 109.1(10) . . ? S1 O3 Hg3 106.2(9) . . ? S2 O4 Hg1 109.7(10) . . ? S2 O5 Hg2 109.9(9) . . ? S2 O6 Hg3 101.0(12) . . ? F3 C1 F2 111.2(40) . . ? F3 C1 F1 108.4(42) . . ? F2 C1 F1 106.5(38) . . ? F3 C1 S1 113.7(35) . . ? F2 C1 S1 110.2(31) . . ? F1 C1 S1 106.4(28) . . ? F4 C2 F6 113.0(44) . . ? F4 C2 F5 104.9(45) . . ? F6 C2 F5 108.8(42) . . ? F4 C2 S2 111.7(36) . . ? F6 C2 S2 110.4(35) . . ? F5 C2 S2 107.8(30) . . ? P21 C12 P12 113.5(13) . . ? P31 C13 P13 114.9(13) . . ? P32 C23 P23 114.1(12) . . ? C116 C111 C112 122.2(27) . . ? C116 C111 P12 116.8(22) . . ? C112 C111 P12 120.9(21) . . ? C111 C112 C113 116.7(28) . . ? C114 C113 C112 120.8(31) . . ? C115 C114 C113 121.9(33) . . ? C114 C115 C116 116.1(30) . . ? C111 C116 C115 121.9(29) . . ? C126 C121 C122 120.2(26) . . ? C126 C121 P12 117.8(22) . . ? C122 C121 P12 121.8(20) . . ? C123 C122 C121 122.1(29) . . ? C124 C123 C122 114.5(36) . . ? C125 C124 C123 128.4(39) . . ? C124 C125 C126 115.6(32) . . ? C121 C126 C125 118.7(28) . . ? C136 C131 C132 121.6(25) . . ? C136 C131 P13 121.3(21) . . ? C132 C131 P13 117.1(21) . . ? C131 C132 C133 120.6(28) . . ? C134 C133 C132 114.4(31) . . ? C135 C134 C133 125.4(37) . . ? C134 C135 C136 119.7(34) . . ? C131 C136 C135 118.2(27) . . ? C146 C141 C142 117.6(28) . . ? C146 C141 P13 118.5(23) . . ? C142 C141 P13 123.8(21) . . ? C141 C142 C143 121.1(26) . . ? C144 C143 C142 123.0(27) . . ? C143 C144 C145 117.2(35) . . ? C144 C145 C146 119.6(40) . . ? C141 C146 C145 120.9(34) . . ? C212 C211 C216 120.5(23) . . ? C212 C211 P21 122.8(20) . . ? C216 C211 P21 116.4(17) . . ? C211 C212 C213 120.4(26) . . ? C214 C213 C212 117.7(28) . . ? C213 C214 C215 123.9(28) . . ? C214 C215 C216 117.7(27) . . ? C215 C216 C211 119.7(24) . . ? C222 C221 C226 119.7(24) . . ? C222 C221 P21 120.8(19) . . ? C226 C221 P21 119.4(20) . . ? C221 C222 C223 119.6(25) . . ? C224 C223 C222 122.0(29) . . ? C223 C224 C225 118.7(31) . . ? C226 C225 C224 119.2(29) . . ? C225 C226 C221 120.4(27) . . ? C236 C231 C232 119.5(22) . . ? C236 C231 P23 121.0(18) . . ? C232 C231 P23 119.2(18) . . ? C233 C232 C231 121.4(24) . . ? C234 C233 C232 118.7(24) . . ? C233 C234 C235 122.1(25) . . ? C234 C235 C236 121.3(25) . . ? C231 C236 C235 116.9(22) . . ? C242 C241 C246 121.5(23) . . ? C242 C241 P23 118.0(18) . . ? C246 C241 P23 119.8(19) . . ? C241 C242 C243 118.1(24) . . ? C244 C243 C242 119.1(28) . . ? C245 C244 C243 123.6(31) . . ? C244 C245 C246 121.6(28) . . ? C241 C246 C245 115.5(25) . . ? C316 C311 C312 121.7(28) . . ? C316 C311 P31 121.0(21) . . ? C312 C311 P31 116.4(23) . . ? C311 C312 C313 116.1(31) . . ? C314 C313 C312 121.1(36) . . ? C313 C314 C315 120.9(39) . . ? C314 C315 C316 119.4(37) . . ? C311 C316 C315 120.7(31) . . ? C322 C321 C326 117.0(30) . . ? C322 C321 P31 124.9(24) . . ? C326 C321 P31 117.5(26) . . ? C321 C322 C323 126.9(30) . . ? C324 C323 C322 115.0(33) . . ? C325 C324 C323 121.1(40) . . ? C324 C325 C326 121.0(41) . . ? C321 C326 C325 118.1(37) . . ? C332 C331 C336 121.7(23) . . ? C332 C331 P32 121.6(19) . . ? C336 C331 P32 116.7(19) . . ? C333 C332 C331 119.0(25) . . ? C334 C333 C332 121.2(32) . . ? C333 C334 C335 122.7(34) . . ? C334 C335 C336 119.8(30) . . ? C331 C336 C335 115.3(25) . . ? C342 C341 C346 120.5(25) . . ? C342 C341 P32 118.0(21) . . ? C346 C341 P32 121.4(20) . . ? C341 C342 C343 117.5(27) . . ? C344 C343 C342 120.2(31) . . ? C345 C344 C343 119.8(35) . . ? C344 C345 C346 123.7(36) . . ? C345 C346 C341 118.1(29) . . ? O8 S3 O7 135.7(58) . . ? O8 S3 O9 99.5(45) . . ? O7 S3 O9 124.8(61) . . ? O8 S3 C3 104.0(41) . . ? O7 S3 C3 86.2(54) . . ? O9 S3 C3 76.4(41) . . ? F8 C3 F7 121.6(91) . . ? F8 C3 F9 115.1(83) . . ? F7 C3 F9 87.3(71) . . ? F8 C3 S3 115.4(75) . . ? F7 C3 S3 121.6(77) . . ? F9 C3 S3 79.6(50) . . ? O10 S4 O12 105.7(37) . . ? O10 S4 O11 122.2(27) . . ? O12 S4 O11 107.0(33) . . ? O10 S4 C4 109.3(38) . . ? O12 S4 C4 104.0(42) . . ? O11 S4 C4 107.3(38) . . ? F11 C4 F10 114.3(61) . . ? F11 C4 F12 88.7(58) . . ? F10 C4 F12 98.6(61) . . ? F11 C4 S4 111.8(58) . . ? F10 C4 S4 128.6(65) . . ? F12 C4 S4 104.0(54) . . ? F13 S5 O13 0.0(52) . . ? F13 S5 F15 123.5(25) . . ? O13 S5 F15 123.5(25) . . ? F13 S5 O15 123.5(25) . . ? O13 S5 O15 123.5(25) . . ? F15 S5 O15 0.0(36) . . ? F13 S5 O14 121.9(26) . . ? O13 S5 O14 121.9(26) . . ? F15 S5 O14 94.6(19) . . ? O15 S5 O14 94.6(19) . . ? F13 S5 F14 121.9(26) . . ? O13 S5 F14 121.9(26) . . ? F15 S5 F14 94.6(19) . . ? O15 S5 F14 94.6(19) . . ? O14 S5 F14 0.0(45) . . ? F13 S5 C5 121.2(25) . 2_556 ? O13 S5 C5 121.2(25) . 2_556 ? F15 S5 C5 97.3(24) . 2_556 ? O15 S5 C5 97.3(24) . 2_556 ? O14 S5 C5 90.5(21) . 2_556 ? F14 S5 C5 90.5(21) . 2_556 ? F13 S5 S5 121.2(25) . 2_556 ? O13 S5 S5 121.2(25) . 2_556 ? F15 S5 S5 97.3(24) . 2_556 ? O15 S5 S5 97.3(24) . 2_556 ? O14 S5 S5 90.5(21) . 2_556 ? F14 S5 S5 90.5(21) . 2_556 ? C5 S5 S5 0.0(24) 2_556 2_556 ? F13 C5 O13 0.0(52) . . ? F13 C5 F15 123.5(25) . . ? O13 C5 F15 123.5(25) . . ? F13 C5 O15 123.5(25) . . ? O13 C5 O15 123.5(25) . . ? F15 C5 O15 0.0(36) . . ? F13 C5 O14 121.9(26) . . ? O13 C5 O14 121.9(26) . . ? F15 C5 O14 94.6(19) . . ? O15 C5 O14 94.6(19) . . ? F13 C5 F14 121.9(26) . . ? O13 C5 F14 121.9(26) . . ? F15 C5 F14 94.6(19) . . ? O15 C5 F14 94.6(19) . . ? O14 C5 F14 0.0(45) . . ? F13 C5 C5 121.2(25) . 2_556 ? O13 C5 C5 121.2(25) . 2_556 ? F15 C5 C5 97.3(24) . 2_556 ? O15 C5 C5 97.3(24) . 2_556 ? O14 C5 C5 90.5(21) . 2_556 ? F14 C5 C5 90.5(21) . 2_556 ? F13 C5 S5 121.2(25) . 2_556 ? O13 C5 S5 121.2(25) . 2_556 ? F15 C5 S5 97.3(24) . 2_556 ? O15 C5 S5 97.3(24) . 2_556 ? O14 C5 S5 90.5(21) . 2_556 ? F14 C5 S5 90.5(21) . 2_556 ? C5 C5 S5 0.0(24) 2_556 2_556 ? C5 O13 S5 0.0(22) . . ? C5 F13 S5 0.0(22) . . ? C5 O14 S5 0.0(30) . . ? C5 F14 S5 0.0(30) . . ? C5 O15 S5 0.0(28) . . ? C5 F15 S5 0.0(28) . . ? _refine_diff_density_max 1.130 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.165 #===END data_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C79 H66 F12 Hg3 O12 P6 S4' _chemical_formula_weight 2351.15 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.392(3) _cell_length_b 26.773(5) _cell_length_c 23.723(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.51(3) _cell_angle_gamma 90.00 _cell_volume 9015.3(26) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 12.5 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method ? _exptl_crystal_F_000 4552 _exptl_absorpt_coefficient_mu 5.375 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.763 _exptl_absorpt_correction_T_max 0.540 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method Omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13090 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.1089 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 23.50 _reflns_number_total 10753 _reflns_number_observed 6008 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1527 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.1023P)^2^+0.0011P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00014(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_ls_number_reflns 9226 _refine_ls_number_parameters 671 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_obs 0.0656 _refine_ls_wR_factor_all 0.2228 _refine_ls_wR_factor_obs 0.1628 _refine_ls_goodness_of_fit_all 1.041 _refine_ls_goodness_of_fit_obs 1.145 _refine_ls_restrained_S_all 1.153 _refine_ls_restrained_S_obs 1.145 _refine_ls_shift/esd_max 0.820 _refine_ls_shift/esd_mean 0.034 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg1 Hg 0.14384(6) 0.29452(3) 0.23877(3) 0.0407(3) Uani 1 d . . Hg2 Hg 0.14375(6) 0.19175(3) 0.24197(3) 0.0400(3) Uani 1 d . . Hg3 Hg 0.29151(6) 0.24077(3) 0.19792(3) 0.0400(3) Uani 1 d . . P12 P 0.0054(4) 0.3042(2) 0.2923(2) 0.044(2) Uani 1 d . . P13 P 0.1943(4) 0.3775(2) 0.2065(2) 0.0406(15) Uani 1 d . . P21 P -0.0040(4) 0.1888(2) 0.2869(2) 0.046(2) Uani 1 d . . P23 P 0.1787(4) 0.1077(2) 0.2060(2) 0.0414(15) Uani 1 d . . P31 P 0.3682(4) 0.3228(2) 0.1781(2) 0.0403(15) Uani 1 d . . P32 P 0.3545(4) 0.1573(2) 0.1697(2) 0.0413(15) Uani 1 d . . S1 S 0.1040(5) 0.2503(2) 0.0896(2) 0.059(2) Uani 1 d . . S2 S 0.3009(5) 0.2303(2) 0.3602(3) 0.067(2) Uani 1 d . . S3 S 0.2664(8) -0.0143(4) 0.0661(5) 0.114(3) Uani 1 d . . S4 S 0.2664(10) 0.4865(4) 0.0534(5) 0.120(4) Uani 1 d . . O1 O 0.0610(14) 0.2852(6) 0.1223(7) 0.098(6) Uani 1 d . . O2 O 0.0952(17) 0.2007(7) 0.0990(9) 0.124(8) Uani 1 d . . O3 O 0.2017(15) 0.2644(8) 0.0909(7) 0.106(7) Uani 1 d . . O4 O 0.3003(15) 0.2845(6) 0.3674(7) 0.099(6) Uani 1 d . . O5 O 0.2134(14) 0.2043(7) 0.3554(7) 0.106(7) Uani 1 d . . O6 O 0.3556(14) 0.2163(7) 0.3169(7) 0.098(6) Uani 1 d . . O7 O 0.2614(36) -0.0603(15) 0.0410(35) 0.538(57) Uani 1 d . . O8 O 0.2085(28) 0.0192(18) 0.0465(13) 0.310(29) Uani 1 d . . O9 O 0.3118(28) -0.0044(11) 0.1208(9) 0.237(20) Uani 1 d . . O10 O 0.1922(22) 0.5113(14) 0.0208(16) 0.267(21) Uani 1 d . . O11 O 0.2755(23) 0.4355(8) 0.0311(12) 0.200(14) Uani 1 d . . O12 O 0.2921(21) 0.4890(9) 0.1123(9) 0.166(12) Uani 1 d . . F1 F 0.0892(26) 0.2396(9) -0.0187(8) 0.213(14) Uani 1 d . . F2 F 0.0627(35) 0.3113(9) 0.0065(10) 0.241(20) Uani 1 d . . F3 F -0.0241(26) 0.2577(18) 0.0082(14) 0.299(28) Uani 1 d . . F4 F 0.3753(21) 0.1567(7) 0.4250(8) 0.198(14) Uani 1 d . . F5 F 0.4553(17) 0.2271(10) 0.4330(9) 0.174(9) Uani 1 d . . F6 F 0.3294(15) 0.2159(8) 0.4691(7) 0.141(8) Uani 1 d . . F7 F 0.3716(44) 0.0400(16) 0.0274(38) 0.444(45) Uani 1 d . . F8 F 0.4211(20) -0.0407(12) 0.0412(11) 0.216(13) Uani 1 d . . F9 F 0.3503(33) -0.0007(20) -0.0170(15) 0.289(26) Uani 1 d . . F10 F 0.4323(27) 0.4900(14) 0.0468(19) 0.287(18) Uani 1 d . . F11 F 0.3797(25) 0.5552(10) 0.0456(10) 0.245(16) Uani 1 d . . F12 F 0.3423(43) 0.5121(24) -0.0254(12) 0.530(56) Uani 1 d . . C1 C 0.0594(40) 0.2638(19) 0.0193(13) 0.141(18) Uani 1 d . . C2 C 0.3681(28) 0.2034(14) 0.4242(12) 0.109(12) Uani 1 d . . C3 C 0.3601(59) -0.0080(22) 0.0320(38) 0.277(53) Uani 1 d . . C4 C 0.3501(49) 0.5105(20) 0.0279(41) 0.394(72) Uani 1 d . . C12 C -0.0066(16) 0.2458(7) 0.3306(9) 0.056(6) Uiso 1 d . . H12A H -0.0656 0.2465 0.3453 0.067 Uiso 1 calc . . H12B H 0.0439 0.2438 0.3631 0.067 Uiso 1 calc . . C13 C 0.2779(15) 0.3681(7) 0.1569(8) 0.044(5) Uiso 1 d . . H13A H 0.2428 0.3582 0.1201 0.053 Uiso 1 calc . . H13B H 0.3077 0.3999 0.1516 0.053 Uiso 1 calc . . C23 C 0.2554(15) 0.1147(7) 0.1512(8) 0.045(5) Uiso 1 d . . H23A H 0.2798 0.0821 0.1436 0.054 Uiso 1 calc . . H23B H 0.2172 0.1264 0.1162 0.054 Uiso 1 calc . . C111 C -0.1087(16) 0.3176(7) 0.2481(8) 0.047(5) Uiso 1 d . . C112 C -0.1098(17) 0.3260(8) 0.1901(9) 0.060(6) Uiso 1 d . . H112 H -0.0565 0.3240 0.1727 0.072 Uiso 1 calc . . C113 C -0.1995(20) 0.3377(8) 0.1608(10) 0.072(7) Uiso 1 d . . H113 H -0.2051 0.3448 0.1220 0.086 Uiso 1 calc . . C114 C -0.2793(18) 0.3395(8) 0.1844(10) 0.065(7) Uiso 1 d . . H114 H -0.3366 0.3461 0.1611 0.078 Uiso 1 calc . . C115 C -0.2775(20) 0.3320(9) 0.2403(11) 0.083(8) Uiso 1 d . . H115 H -0.3313 0.3352 0.2570 0.099 Uiso 1 calc . . C116 C -0.1886(19) 0.3190(8) 0.2729(10) 0.067(7) Uiso 1 d . . H116 H -0.1845 0.3114 0.3115 0.080 Uiso 1 calc . . C121 C 0.0267(15) 0.3504(7) 0.3490(8) 0.043(5) Uiso 1 d . . C122 C 0.1003(17) 0.3449(8) 0.3915(9) 0.058(6) Uiso 1 d . . H122 H 0.1371 0.3163 0.3924 0.069 Uiso 1 calc . . C123 C 0.1237(19) 0.3809(9) 0.4346(10) 0.078(8) Uiso 1 d . . H123 H 0.1767 0.3780 0.4628 0.094 Uiso 1 calc . . C124 C 0.0613(20) 0.4213(9) 0.4322(11) 0.080(8) Uiso 1 d . . H124 H 0.0716 0.4449 0.4612 0.096 Uiso 1 calc . . C125 C -0.0151(21) 0.4279(10) 0.3886(12) 0.089(9) Uiso 1 d . . H125 H -0.0532 0.4561 0.3878 0.107 Uiso 1 calc . . C126 C -0.0337(18) 0.3916(8) 0.3458(10) 0.068(7) Uiso 1 d . . H126 H -0.0845 0.3948 0.3162 0.081 Uiso 1 calc . . C131 C 0.2489(14) 0.4188(6) 0.2614(8) 0.036(5) Uiso 1 d . . C132 C 0.2703(16) 0.4028(7) 0.3155(9) 0.056(6) Uiso 1 d . . H132 H 0.2566 0.3701 0.3244 0.067 Uiso 1 calc . . C133 C 0.3116(20) 0.4337(10) 0.3574(11) 0.087(8) Uiso 1 d . . H133 H 0.3248 0.4225 0.3950 0.105 Uiso 1 calc . . C134 C 0.3346(19) 0.4828(9) 0.3438(10) 0.075(7) Uiso 1 d . . H134 H 0.3675 0.5032 0.3720 0.090 Uiso 1 calc . . C135 C 0.3097(17) 0.5000(8) 0.2913(10) 0.065(7) Uiso 1 d . . H135 H 0.3201 0.5333 0.2828 0.078 Uiso 1 calc . . C136 C 0.2683(17) 0.4680(8) 0.2495(9) 0.059(6) Uiso 1 d . . H136 H 0.2528 0.4796 0.2122 0.071 Uiso 1 calc . . C141 C 0.0916(14) 0.4098(6) 0.1682(8) 0.039(5) Uiso 1 d . . C142 C 0.0352(17) 0.4328(7) 0.2003(9) 0.056(6) Uiso 1 d . . H142 H 0.0539 0.4351 0.2396 0.068 Uiso 1 calc . . C143 C -0.0477(19) 0.4525(9) 0.1760(11) 0.076(7) Uiso 1 d . . H143 H -0.0864 0.4671 0.1991 0.091 Uiso 1 calc . . C144 C -0.0761(19) 0.4515(9) 0.1186(11) 0.072(7) Uiso 1 d . . H144 H -0.1316 0.4669 0.1014 0.087 Uiso 1 calc . . C145 C -0.0190(18) 0.4269(8) 0.0875(10) 0.066(7) Uiso 1 d . . H145 H -0.0377 0.4240 0.0482 0.079 Uiso 1 calc . . C146 C 0.0632(15) 0.4068(6) 0.1115(8) 0.041(5) Uiso 1 d . . H146 H 0.1008 0.3906 0.0888 0.049 Uiso 1 calc . . C211 C -0.1036(18) 0.1867(8) 0.2300(10) 0.062(6) Uiso 1 d . . C212 C -0.0947(21) 0.1826(9) 0.1746(12) 0.084(8) Uiso 1 d . . H212 H -0.0352 0.1821 0.1640 0.100 Uiso 1 calc . . C213 C -0.1720(29) 0.1791(12) 0.1347(15) 0.122(12) Uiso 1 d . . H213 H -0.1639 0.1729 0.0973 0.147 Uiso 1 calc . . C214 C -0.2584(28) 0.1839(12) 0.1449(15) 0.121(12) Uiso 1 d . . H214 H -0.3080 0.1828 0.1143 0.146 Uiso 1 calc . . C215 C -0.2779(27) 0.1907(12) 0.1991(16) 0.129(12) Uiso 1 d . . H215 H -0.3391 0.1921 0.2069 0.155 Uiso 1 calc . . C216 C -0.1970(27) 0.1955(11) 0.2424(14) 0.116(11) Uiso 1 d . . H216 H -0.2045 0.2043 0.2793 0.139 Uiso 1 calc . . C221 C -0.0142(16) 0.1378(7) 0.3359(9) 0.051(6) Uiso 1 d . . C222 C 0.0522(19) 0.1354(9) 0.3829(11) 0.075(7) Uiso 1 d . . H222 H 0.0982 0.1600 0.3902 0.091 Uiso 1 calc . . C223 C 0.0510(23) 0.0919(11) 0.4239(13) 0.108(10) Uiso 1 d . . H223 H 0.0972 0.0869 0.4558 0.129 Uiso 1 calc . . C224 C -0.0269(22) 0.0598(10) 0.4089(12) 0.086(8) Uiso 1 d . . H224 H -0.0276 0.0311 0.4310 0.103 Uiso 1 calc . . C225 C -0.0990(22) 0.0658(10) 0.3671(12) 0.096(9) Uiso 1 d . . H225 H -0.1515 0.0452 0.3644 0.115 Uiso 1 calc . . C226 C -0.0948(20) 0.1047(9) 0.3262(11) 0.084(8) Uiso 1 d . . H226 H -0.1419 0.1085 0.2946 0.100 Uiso 1 calc . . C231 C 0.2304(16) 0.0619(7) 0.2597(9) 0.055(6) Uiso 1 d . . C232 C 0.2588(18) 0.0777(9) 0.3134(10) 0.072(7) Uiso 1 d . . H232 H 0.2535 0.1108 0.3241 0.087 Uiso 1 calc . . C233 C 0.2964(23) 0.0414(11) 0.3515(13) 0.106(10) Uiso 1 d . . H233 H 0.3102 0.0500 0.3900 0.128 Uiso 1 calc . . C234 C 0.3149(21) -0.0075(10) 0.3361(12) 0.097(9) Uiso 1 d . . H234 H 0.3481 -0.0292 0.3627 0.116 Uiso 1 calc . . C235 C 0.2850(18) -0.0223(8) 0.2835(10) 0.073(7) Uiso 1 d . . H235 H 0.2916 -0.0555 0.2730 0.088 Uiso 1 calc . . C236 C 0.2435(17) 0.0123(8) 0.2442(9) 0.064(7) Uiso 1 d . . H236 H 0.2238 0.0025 0.2065 0.077 Uiso 1 calc . . C241 C 0.0647(16) 0.0787(7) 0.1685(9) 0.052(6) Uiso 1 d . . C242 C -0.0469(18) 0.0644(8) 0.0873(10) 0.068(7) Uiso 1 d . . H242 H -0.0661 0.0670 0.0480 0.081 Uiso 1 calc . . C243 C 0.0396(17) 0.0819(8) 0.1108(9) 0.057(6) Uiso 1 d . . H243 H 0.0801 0.0956 0.0882 0.068 Uiso 1 calc . . C244 C -0.1077(20) 0.0426(9) 0.1205(12) 0.085(8) Uiso 1 d . . H244 H -0.1659 0.0296 0.1043 0.102 Uiso 1 calc . . C245 C -0.0770(22) 0.0415(10) 0.1769(13) 0.098(9) Uiso 1 d . . H245 H -0.1169 0.0275 0.1996 0.117 Uiso 1 calc . . C246 C 0.0097(18) 0.0596(8) 0.2047(9) 0.063(7) Uiso 1 d . . H246 H 0.0280 0.0587 0.2442 0.076 Uiso 1 calc . . C311 C 0.4354(15) 0.3226(7) 0.1223(8) 0.047(5) Uiso 1 d . . C312 C 0.4446(20) 0.3643(9) 0.0906(11) 0.080(8) Uiso 1 d . . H312 H 0.4088 0.3926 0.0944 0.096 Uiso 1 calc . . C313 C 0.5088(20) 0.3639(10) 0.0522(11) 0.084(8) Uiso 1 d . . H313 H 0.5160 0.3919 0.0302 0.101 Uiso 1 calc . . C314 C 0.5608(22) 0.3219(11) 0.0471(12) 0.097(9) Uiso 1 d . . H314 H 0.6029 0.3220 0.0213 0.116 Uiso 1 calc . . C315 C 0.5536(20) 0.2810(10) 0.0777(11) 0.086(8) Uiso 1 d . . H315 H 0.5892 0.2528 0.0734 0.103 Uiso 1 calc . . C316 C 0.4888(18) 0.2819(9) 0.1179(10) 0.075(7) Uiso 1 d . . H316 H 0.4838 0.2542 0.1409 0.090 Uiso 1 calc . . C321 C 0.4397(16) 0.3472(7) 0.2413(9) 0.053(6) Uiso 1 d . . C322 C 0.4808(16) 0.3955(7) 0.2414(9) 0.054(6) Uiso 1 d . . H322 H 0.4687 0.4151 0.2086 0.065 Uiso 1 calc . . C323 C 0.5377(19) 0.4139(9) 0.2887(11) 0.080(8) Uiso 1 d . . H323 H 0.5643 0.4455 0.2879 0.096 Uiso 1 calc . . C324 C 0.5552(21) 0.3854(10) 0.3370(12) 0.095(9) Uiso 1 d . . H324 H 0.5913 0.3982 0.3700 0.114 Uiso 1 calc . . C325 C 0.5193(19) 0.3372(9) 0.3370(11) 0.080(8) Uiso 1 d . . H325 H 0.5337 0.3176 0.3696 0.095 Uiso 1 calc . . C326 C 0.4624(17) 0.3178(8) 0.2891(9) 0.059(6) Uiso 1 d . . H326 H 0.4397 0.2853 0.2894 0.071 Uiso 1 calc . . C331 C 0.4388(16) 0.1314(8) 0.2253(9) 0.055(6) Uiso 1 d . . C332 C 0.4535(19) 0.0793(9) 0.2333(11) 0.082(8) Uiso 1 d . . H332 H 0.4167 0.0569 0.2093 0.099 Uiso 1 calc . . C333 C 0.5247(23) 0.0607(11) 0.2780(13) 0.105(10) Uiso 1 d . . H333 H 0.5358 0.0268 0.2841 0.126 Uiso 1 calc . . C334 C 0.5729(23) 0.0952(12) 0.3098(13) 0.110(10) Uiso 1 d . . H334 H 0.6170 0.0834 0.3400 0.132 Uiso 1 calc . . C335 C 0.5671(26) 0.1445(14) 0.3045(15) 0.134(13) Uiso 1 d . . H335 H 0.6077 0.1646 0.3293 0.161 Uiso 1 calc . . C336 C 0.5006(23) 0.1668(11) 0.2619(13) 0.101(10) Uiso 1 d . . H336 H 0.4958 0.2012 0.2571 0.122 Uiso 1 calc . . C341 C 0.4043(16) 0.1535(7) 0.1033(9) 0.053(6) Uiso 1 d . . C342 C 0.4911(18) 0.1325(8) 0.1042(10) 0.065(7) Uiso 1 d . . H342 H 0.5270 0.1216 0.1382 0.077 Uiso 1 calc . . C343 C 0.5246(20) 0.1280(9) 0.0516(12) 0.083(8) Uiso 1 d . . H343 H 0.5836 0.1141 0.0509 0.100 Uiso 1 calc . . C344 C 0.4735(21) 0.1432(9) 0.0042(11) 0.081(8) Uiso 1 d . . H344 H 0.4964 0.1382 -0.0298 0.097 Uiso 1 calc . . C345 C 0.3906(21) 0.1653(9) 0.0020(11) 0.085(8) Uiso 1 d . . H345 H 0.3565 0.1763 -0.0325 0.101 Uiso 1 calc . . C346 C 0.3561(17) 0.1715(8) 0.0536(9) 0.060(6) Uiso 1 d . . H346 H 0.2994 0.1882 0.0536 0.072 Uiso 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0414(7) 0.0380(4) 0.0439(5) 0.0008(4) 0.0112(4) -0.0024(4) Hg2 0.0423(7) 0.0384(5) 0.0400(5) -0.0018(3) 0.0085(4) -0.0023(4) Hg3 0.0397(6) 0.0369(4) 0.0427(4) -0.0009(3) 0.0045(4) -0.0021(4) P12 0.046(5) 0.042(3) 0.048(3) -0.001(2) 0.013(3) 0.005(3) P13 0.043(4) 0.036(3) 0.045(3) 0.000(2) 0.013(3) 0.000(3) P21 0.045(5) 0.045(3) 0.052(4) -0.004(3) 0.017(3) -0.008(3) P23 0.045(5) 0.037(3) 0.044(3) 0.000(2) 0.013(3) -0.006(3) P31 0.041(4) 0.040(3) 0.044(3) -0.002(2) 0.016(3) -0.002(3) P32 0.041(5) 0.036(3) 0.047(3) -0.002(2) 0.007(3) -0.001(3) S1 0.073(6) 0.055(4) 0.046(3) -0.003(3) -0.001(3) 0.004(3) S2 0.074(6) 0.068(5) 0.053(4) 0.002(3) -0.008(4) 0.000(4) S3 0.098(9) 0.125(8) 0.122(8) -0.005(6) 0.025(7) 0.016(6) S4 0.123(12) 0.124(9) 0.119(9) 0.034(7) 0.042(8) 0.022(7) O1 0.119(18) 0.088(13) 0.085(13) -0.007(10) 0.013(12) 0.049(12) O2 0.181(24) 0.071(13) 0.122(17) -0.006(11) 0.031(16) -0.001(14) O3 0.071(17) 0.185(21) 0.058(11) -0.003(12) 0.003(10) -0.011(14) O4 0.141(19) 0.077(12) 0.084(13) 0.009(10) 0.032(13) 0.017(12) O5 0.102(18) 0.132(16) 0.073(12) 0.042(11) -0.017(11) -0.060(14) O6 0.102(17) 0.128(15) 0.058(11) -0.005(11) -0.003(11) 0.039(13) O7 0.286(61) 0.167(36) 1.090(166) -0.194(67) -0.098(75) -0.086(40) O8 0.297(52) 0.468(64) 0.150(29) 0.037(33) -0.006(30) 0.284(51) O9 0.441(54) 0.219(29) 0.054(14) -0.017(16) 0.048(23) 0.172(33) O10 0.169(33) 0.315(44) 0.292(43) 0.133(36) -0.038(31) 0.115(31) O11 0.253(36) 0.089(17) 0.228(31) -0.047(18) -0.045(27) 0.024(20) O12 0.242(34) 0.176(23) 0.076(16) -0.006(15) 0.013(19) -0.082(21) F1 0.361(44) 0.206(24) 0.068(12) -0.052(14) 0.019(19) 0.053(24) F2 0.462(61) 0.162(22) 0.102(17) 0.055(17) 0.055(26) 0.117(31) F3 0.192(35) 0.511(81) 0.150(26) -0.006(34) -0.098(26) 0.131(38) F4 0.340(36) 0.096(14) 0.118(16) 0.007(13) -0.078(19) 0.052(19) F5 0.130(20) 0.239(24) 0.124(17) 0.006(16) -0.062(15) 0.028(19) F6 0.169(21) 0.191(19) 0.056(11) 0.026(12) 0.001(12) -0.028(15) F7 0.497(83) 0.210(41) 0.714(111) -0.071(60) 0.364(89) -0.155(52) F8 0.215(32) 0.266(32) 0.180(24) 0.020(22) 0.074(22) 0.104(27) F9 0.334(50) 0.339(54) 0.238(35) 0.188(37) 0.176(36) 0.164(45) F10 0.232(41) 0.228(36) 0.432(59) 0.035(38) 0.146(40) -0.008(30) F11 0.402(47) 0.199(26) 0.131(19) 0.000(18) 0.036(24) -0.162(30) F12 0.628(99) 0.902(117) 0.095(20) -0.166(40) 0.159(39) -0.489(89) C1 0.181(44) 0.170(39) 0.049(18) -0.005(21) -0.046(23) 0.122(34) C2 0.111(33) 0.155(34) 0.045(18) 0.002(20) -0.032(19) -0.033(26) C3 0.374(94) 0.198(52) 0.356(81) 0.224(62) 0.343(82) 0.221(65) C4 0.194(74) 0.135(45) 0.737(158) -0.252(73) -0.265(91) 0.141(51) _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 Hg1 P13 2.497(5) . ? Hg1 P12 2.548(6) . ? Hg1 Hg2 2.7526(11) . ? Hg1 O1 2.83(2) . ? Hg1 Hg3 2.8649(13) . ? Hg1 O4 3.49(2) . ? Hg2 P23 2.488(5) . ? Hg2 P21 2.533(6) . ? Hg2 O5 2.73(2) . ? Hg2 Hg3 2.8409(13) . ? Hg2 O2 3.36(2) . ? Hg3 P31 2.538(5) . ? Hg3 P32 2.542(5) . ? Hg3 O3 2.73(2) . ? Hg3 O6 2.90(2) . ? P12 C121 1.81(2) . ? P12 C111 1.83(2) . ? P12 C12 1.83(2) . ? P13 C131 1.79(2) . ? P13 C141 1.82(2) . ? P13 C13 1.83(2) . ? P21 C211 1.80(2) . ? P21 C221 1.81(2) . ? P21 C12 1.85(2) . ? P23 C231 1.83(2) . ? P23 C23 1.85(2) . ? P23 C241 1.90(2) . ? P31 C311 1.76(2) . ? P31 C13 1.79(2) . ? P31 C321 1.79(2) . ? P32 C331 1.78(2) . ? P32 C23 1.82(2) . ? P32 C341 1.84(2) . ? S1 O2 1.36(2) . ? S1 O1 1.42(2) . ? S1 O3 1.45(2) . ? S1 C1 1.72(3) . ? S2 O5 1.43(2) . ? S2 O6 1.44(2) . ? S2 O4 1.46(2) . ? S2 C2 1.81(3) . ? S3 O8 1.26(3) . ? S3 O7 1.36(4) . ? S3 O9 1.38(3) . ? S3 C3 1.69(4) . ? S4 O12 1.39(2) . ? S4 O10 1.38(3) . ? S4 O11 1.48(2) . ? S4 C4 1.57(11) . ? F1 C1 1.24(4) . ? F2 C1 1.31(5) . ? F3 C1 1.20(6) . ? F4 C2 1.26(4) . ? F5 C2 1.39(4) . ? F6 C2 1.32(4) . ? F7 C3 1.30(6) . ? F7 F9 1.51(6) . ? F8 C3 1.23(4) . ? F9 C3 1.16(8) . ? F10 C4 1.31(5) . ? F11 C4 1.32(5) . ? F12 C4 1.25(10) . ? C111 C116 1.38(3) . ? C111 C112 1.39(3) . ? C112 C113 1.40(3) . ? C113 C114 1.36(3) . ? C114 C115 1.34(3) . ? C115 C116 1.42(3) . ? C121 C122 1.35(3) . ? C121 C126 1.40(3) . ? C122 C123 1.40(3) . ? C123 C124 1.40(3) . ? C124 C125 1.39(3) . ? C125 C126 1.40(3) . ? C131 C132 1.34(2) . ? C131 C136 1.39(3) . ? C132 C133 1.35(3) . ? C133 C134 1.41(3) . ? C134 C135 1.32(3) . ? C135 C136 1.37(3) . ? C141 C146 1.34(2) . ? C141 C142 1.35(3) . ? C142 C143 1.34(3) . ? C143 C144 1.36(3) . ? C144 C145 1.36(3) . ? C145 C146 1.34(3) . ? C211 C212 1.35(3) . ? C211 C216 1.44(4) . ? C212 C213 1.34(4) . ? C213 C214 1.31(4) . ? C214 C215 1.37(4) . ? C215 C216 1.43(4) . ? C221 C222 1.35(3) . ? C221 C226 1.45(3) . ? C222 C223 1.52(3) . ? C223 C224 1.41(4) . ? C224 C225 1.32(3) . ? C225 C226 1.43(3) . ? C231 C232 1.34(3) . ? C231 C236 1.40(3) . ? C232 C233 1.38(3) . ? C233 C234 1.40(3) . ? C234 C235 1.31(3) . ? C235 C236 1.38(3) . ? C241 C243 1.36(3) . ? C241 C246 1.36(3) . ? C242 C243 1.36(3) . ? C242 C244 1.40(3) . ? C244 C245 1.34(3) . ? C245 C246 1.40(3) . ? C311 C316 1.35(3) . ? C311 C312 1.37(3) . ? C312 C313 1.40(3) . ? C313 C314 1.36(3) . ? C314 C315 1.33(3) . ? C315 C316 1.44(3) . ? C321 C326 1.37(3) . ? C321 C322 1.42(3) . ? C322 C323 1.37(3) . ? C323 C324 1.37(3) . ? C324 C325 1.39(3) . ? C325 C326 1.38(3) . ? C331 C332 1.42(3) . ? C331 C336 1.48(3) . ? C332 C333 1.44(3) . ? C333 C334 1.31(4) . ? C334 C335 1.33(4) . ? C335 C336 1.40(4) . ? C341 C346 1.36(3) . ? C341 C342 1.37(3) . ? C342 C343 1.41(3) . ? C343 C344 1.30(3) . ? C344 C345 1.32(3) . ? C345 C346 1.41(3) . ? 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 P13 Hg1 P12 110.7(2) . . ? P13 Hg1 Hg2 154.10(13) . . ? P12 Hg1 Hg2 94.83(12) . . ? P13 Hg1 O1 82.9(4) . . ? P12 Hg1 O1 104.9(4) . . ? Hg2 Hg1 O1 86.4(3) . . ? P13 Hg1 Hg3 94.23(13) . . ? P12 Hg1 Hg3 154.84(12) . . ? Hg2 Hg1 Hg3 60.72(3) . . ? O1 Hg1 Hg3 80.9(3) . . ? P13 Hg1 O4 99.1(3) . . ? P12 Hg1 O4 90.9(3) . . ? Hg2 Hg1 O4 84.4(3) . . ? O1 Hg1 O4 162.3(5) . . ? Hg3 Hg1 O4 81.4(3) . . ? P23 Hg2 P21 110.3(2) . . ? P23 Hg2 O5 112.8(4) . . ? P21 Hg2 O5 77.6(4) . . ? P23 Hg2 Hg1 153.36(13) . . ? P21 Hg2 Hg1 92.69(12) . . ? O5 Hg2 Hg1 84.4(4) . . ? P23 Hg2 Hg3 94.91(13) . . ? P21 Hg2 Hg3 154.27(12) . . ? O5 Hg2 Hg3 97.5(4) . . ? Hg1 Hg2 Hg3 61.59(3) . . ? P23 Hg2 O2 74.8(3) . . ? P21 Hg2 O2 112.2(4) . . ? O5 Hg2 O2 165.3(5) . . ? Hg1 Hg2 O2 84.3(3) . . ? Hg3 Hg2 O2 68.8(4) . . ? P31 Hg3 P32 121.9(2) . . ? P31 Hg3 O3 77.3(5) . . ? P32 Hg3 O3 95.4(4) . . ? P31 Hg3 Hg2 147.46(13) . . ? P32 Hg3 Hg2 90.67(13) . . ? O3 Hg3 Hg2 100.4(4) . . ? P31 Hg3 Hg1 89.84(13) . . ? P32 Hg3 Hg1 147.91(14) . . ? O3 Hg3 Hg1 86.2(4) . . ? Hg2 Hg3 Hg1 57.69(3) . . ? P31 Hg3 O6 107.3(4) . . ? P32 Hg3 O6 89.3(4) . . ? O3 Hg3 O6 170.3(6) . . ? Hg2 Hg3 O6 71.0(4) . . ? Hg1 Hg3 O6 85.3(4) . . ? C121 P12 C111 108.5(9) . . ? C121 P12 C12 103.5(9) . . ? C111 P12 C12 107.6(10) . . ? C121 P12 Hg1 112.8(7) . . ? C111 P12 Hg1 115.8(7) . . ? C12 P12 Hg1 107.8(7) . . ? C131 P13 C141 107.1(8) . . ? C131 P13 C13 107.2(9) . . ? C141 P13 C13 108.0(9) . . ? C131 P13 Hg1 116.2(6) . . ? C141 P13 Hg1 108.8(6) . . ? C13 P13 Hg1 109.2(6) . . ? C211 P21 C221 108.5(11) . . ? C211 P21 C12 111.0(10) . . ? C221 P21 C12 104.5(9) . . ? C211 P21 Hg2 107.8(9) . . ? C221 P21 Hg2 117.1(8) . . ? C12 P21 Hg2 107.9(7) . . ? C231 P23 C23 109.6(10) . . ? C231 P23 C241 105.8(9) . . ? C23 P23 C241 106.4(9) . . ? C231 P23 Hg2 116.6(7) . . ? C23 P23 Hg2 109.1(6) . . ? C241 P23 Hg2 108.8(7) . . ? C311 P31 C13 104.7(9) . . ? C311 P31 C321 108.6(10) . . ? C13 P31 C321 106.2(9) . . ? C311 P31 Hg3 116.4(7) . . ? C13 P31 Hg3 108.7(7) . . ? C321 P31 Hg3 111.5(7) . . ? C331 P32 C23 110.2(9) . . ? C331 P32 C341 107.4(10) . . ? C23 P32 C341 99.2(9) . . ? C331 P32 Hg3 112.2(7) . . ? C23 P32 Hg3 108.3(7) . . ? C341 P32 Hg3 118.7(7) . . ? O2 S1 O1 119.5(13) . . ? O2 S1 O3 111.5(13) . . ? O1 S1 O3 109.1(12) . . ? O2 S1 C1 109.5(21) . . ? O1 S1 C1 105.4(14) . . ? O3 S1 C1 99.9(23) . . ? O5 S2 O6 113.2(12) . . ? O5 S2 O4 118.1(13) . . ? O6 S2 O4 110.9(11) . . ? O5 S2 C2 102.4(14) . . ? O6 S2 C2 102.4(16) . . ? O4 S2 C2 108.1(14) . . ? O8 S3 O7 119.8(34) . . ? O8 S3 O9 113.2(22) . . ? O7 S3 O9 124.5(32) . . ? O8 S3 C3 106.4(27) . . ? O7 S3 C3 82.5(40) . . ? O9 S3 C3 98.0(43) . . ? O12 S4 O10 126.4(23) . . ? O12 S4 O11 112.4(17) . . ? O10 S4 O11 110.5(23) . . ? O12 S4 C4 105.9(32) . . ? O10 S4 C4 99.2(28) . . ? O11 S4 C4 97.0(21) . . ? S1 O1 Hg1 116.1(9) . . ? S1 O2 Hg2 103.1(10) . . ? S1 O3 Hg3 105.6(9) . . ? S2 O4 Hg1 89.4(8) . . ? S2 O5 Hg2 108.3(9) . . ? S2 O6 Hg3 120.7(9) . . ? C3 F7 F9 48.1(40) . . ? C3 F9 F7 56.5(40) . . ? F3 C1 F1 103.0(44) . . ? F3 C1 F2 98.9(32) . . ? F1 C1 F2 107.9(45) . . ? F3 C1 S1 112.6(47) . . ? F1 C1 S1 118.4(26) . . ? F2 C1 S1 113.9(36) . . ? F4 C2 F6 106.5(32) . . ? F4 C2 F5 112.4(38) . . ? F6 C2 F5 104.7(26) . . ? F4 C2 S2 116.2(22) . . ? F6 C2 S2 109.7(28) . . ? F5 C2 S2 106.8(23) . . ? F9 C3 F8 105.1(47) . . ? F9 C3 F7 75.4(40) . . ? F8 C3 F7 128.3(90) . . ? F9 C3 S3 121.4(83) . . ? F8 C3 S3 116.4(28) . . ? F7 C3 S3 105.1(38) . . ? F12 C4 F11 105.2(83) . . ? F12 C4 F10 106.6(82) . . ? F11 C4 F10 92.6(45) . . ? F12 C4 S4 117.1(49) . . ? F11 C4 S4 118.4(65) . . ? F10 C4 S4 113.7(70) . . ? P12 C12 P21 114.5(11) . . ? P31 C13 P13 115.8(10) . . ? P32 C23 P23 115.4(10) . . ? C116 C111 C112 123.1(21) . . ? C116 C111 P12 119.5(17) . . ? C112 C111 P12 117.4(18) . . ? C111 C112 C113 112.7(22) . . ? C114 C113 C112 125.3(23) . . ? C115 C114 C113 121.6(25) . . ? C114 C115 C116 116.4(26) . . ? C111 C116 C115 120.9(22) . . ? C122 C121 C126 122.1(20) . . ? C122 C121 P12 119.9(16) . . ? C126 C121 P12 118.0(16) . . ? C121 C122 C123 122.5(21) . . ? C122 C123 C124 115.1(24) . . ? C125 C124 C123 123.5(25) . . ? C124 C125 C126 118.9(25) . . ? C121 C126 C125 117.8(23) . . ? C132 C131 C136 118.4(18) . . ? C132 C131 P13 120.3(15) . . ? C136 C131 P13 121.3(15) . . ? C131 C132 C133 120.9(21) . . ? C132 C133 C134 119.7(24) . . ? C135 C134 C133 120.3(24) . . ? C134 C135 C136 118.7(22) . . ? C135 C136 C131 121.8(20) . . ? C146 C141 C142 118.8(20) . . ? C146 C141 P13 124.0(16) . . ? C142 C141 P13 116.7(15) . . ? C143 C142 C141 120.7(21) . . ? C142 C143 C144 121.5(25) . . ? C145 C144 C143 116.4(25) . . ? C146 C145 C144 122.3(22) . . ? C145 C146 C141 120.2(20) . . ? C212 C211 C216 117.1(25) . . ? C212 C211 P21 122.8(22) . . ? C216 C211 P21 119.6(21) . . ? C213 C212 C211 119.5(30) . . ? C214 C213 C212 124.6(36) . . ? C213 C214 C215 122.1(38) . . ? C214 C215 C216 114.7(36) . . ? C215 C216 C211 121.0(30) . . ? C222 C221 C226 122.8(22) . . ? C222 C221 P21 116.5(18) . . ? C226 C221 P21 120.5(18) . . ? C221 C222 C223 119.2(24) . . ? C224 C223 C222 113.4(26) . . ? C225 C224 C223 127.5(28) . . ? C224 C225 C226 118.8(28) . . ? C225 C226 C221 117.4(25) . . ? C232 C231 C236 121.1(21) . . ? C232 C231 P23 118.4(17) . . ? C236 C231 P23 120.5(16) . . ? C231 C232 C233 115.3(23) . . ? C232 C233 C234 124.1(28) . . ? C235 C234 C233 119.1(28) . . ? C234 C235 C236 118.4(24) . . ? C235 C236 C231 121.5(21) . . ? C243 C241 C246 125.1(23) . . ? C243 C241 P23 120.8(18) . . ? C246 C241 P23 113.9(17) . . ? C243 C242 C244 122.0(23) . . ? C242 C243 C241 117.6(22) . . ? C245 C244 C242 116.0(27) . . ? C244 C245 C246 125.9(28) . . ? C241 C246 C245 113.5(23) . . ? C316 C311 C312 120.7(23) . . ? C316 C311 P31 116.9(17) . . ? C312 C311 P31 121.7(18) . . ? C311 C312 C313 119.1(24) . . ? C314 C313 C312 119.6(26) . . ? C315 C314 C313 122.5(30) . . ? C314 C315 C316 117.8(27) . . ? C311 C316 C315 120.3(23) . . ? C326 C321 C322 118.5(20) . . ? C326 C321 P31 120.5(16) . . ? C322 C321 P31 120.8(16) . . ? C323 C322 C321 121.4(21) . . ? C322 C323 C324 119.4(25) . . ? C323 C324 C325 120.1(27) . . ? C326 C325 C324 121.1(24) . . ? C321 C326 C325 119.4(21) . . ? C332 C331 C336 119.3(22) . . ? C332 C331 P32 123.4(18) . . ? C336 C331 P32 117.1(18) . . ? C331 C332 C333 120.8(24) . . ? C334 C333 C332 115.2(29) . . ? C333 C334 C335 128.7(36) . . ? C334 C335 C336 121.0(34) . . ? C335 C336 C331 115.0(27) . . ? C346 C341 C342 119.6(22) . . ? C346 C341 P32 120.7(18) . . ? C342 C341 P32 119.7(17) . . ? C341 C342 C343 117.8(23) . . ? C344 C343 C342 120.5(27) . . ? C343 C344 C345 123.4(28) . . ? C344 C345 C346 117.7(26) . . ? C341 C346 C345 120.8(23) . . ? _refine_diff_density_max 2.377 _refine_diff_density_min -.672 _refine_diff_density_rms .189 #===END data_5H2O _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C79 H86 Hg3 O16 P6 S4' _chemical_formula_weight 2207.31 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.920(3) _cell_length_b 15.036(3) _cell_length_c 22.182(4) _cell_angle_alpha 83.19(2) _cell_angle_beta 71.49(2) _cell_angle_gamma 65.96(2) _cell_volume 4309.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 5.2 _cell_measurement_theta_max 12.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.9 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method ? _exptl_crystal_F_000 2164 _exptl_absorpt_coefficient_mu 5.601 _exptl_absorpt_correction_type PSI-scan _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14022 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 23.50 _reflns_number_total 12409 _reflns_number_observed 9801 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 371 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.1119P)^2^+53.9688P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12038 _refine_ls_number_parameters 973 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_obs 0.0642 _refine_ls_wR_factor_all 0.2192 _refine_ls_wR_factor_obs 0.1732 _refine_ls_goodness_of_fit_all 1.052 _refine_ls_goodness_of_fit_obs 1.094 _refine_ls_restrained_S_all 1.225 _refine_ls_restrained_S_obs 1.094 _refine_ls_shift/esd_max 0.027 _refine_ls_shift/esd_mean 0.004 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg1 Hg 0.25668(4) 0.82142(4) 0.24845(3) 0.0324(2) Uani 1 d . . Hg2 Hg 0.06245(4) 0.83592(4) 0.24802(2) 0.0292(2) Uani 1 d . . Hg3 Hg 0.10172(4) 1.00100(4) 0.24931(3) 0.0320(2) Uani 1 d . . P12 P 0.3188(3) 0.6395(3) 0.2599(2) 0.0330(8) Uani 1 d . . P13 P 0.3864(3) 0.8945(3) 0.2366(2) 0.0306(8) Uani 1 d . . P21 P 0.1273(3) 0.6549(2) 0.2301(2) 0.0317(8) Uani 1 d . . P23 P -0.1285(2) 0.9319(2) 0.2636(2) 0.0262(7) Uani 1 d . . P31 P 0.2121(3) 1.0949(2) 0.2348(2) 0.0293(8) Uani 1 d . . P32 P -0.0763(3) 1.1108(2) 0.2461(2) 0.0273(7) Uani 1 d . . S1 S 0.2555(3) 0.8396(3) 0.0938(2) 0.0345(8) Uani 1 d . . S2 S 0.0009(3) 0.9362(3) 0.4057(2) 0.0400(9) Uani 1 d . . S3 S -0.4387(3) 1.1972(4) 0.3943(2) 0.0566(11) Uani 1 d . . S4 S 0.4455(4) 0.2981(4) 0.1710(3) 0.0636(13) Uani 1 d . . O1 O 0.3220(9) 0.7685(8) 0.1282(5) 0.058(3) Uani 1 d . . O2 O 0.1601(9) 0.8329(9) 0.1079(5) 0.053(3) Uani 1 d . . O3 O 0.2440(10) 0.9404(8) 0.1027(6) 0.059(3) Uani 1 d . . O4 O 0.0887(14) 0.8860(13) 0.4287(9) 0.122(7) Uani 1 d . . O5 O -0.0188(9) 0.8703(9) 0.3739(5) 0.056(3) Uani 1 d . . O6 O 0.0035(10) 1.0200(8) 0.3658(6) 0.063(3) Uani 1 d . . O7 O -0.4140(11) 1.1436(12) 0.3376(6) 0.082(4) Uani 1 d . . O8 O -0.3556(11) 1.1602(11) 0.4229(6) 0.074(4) Uani 1 d . . O9 O -0.5376(11) 1.2120(15) 0.4381(7) 0.104(6) Uani 1 d . . O10 O 0.3546(11) 0.3578(10) 0.2155(8) 0.093(5) Uani 1 d . . O11 O 0.4465(11) 0.2021(10) 0.1634(7) 0.080(4) Uani 1 d . . O12 O 0.4682(19) 0.3465(16) 0.1116(9) 0.130(7) Uani 1 d . . C1 C 0.3187(15) 0.8110(15) 0.0134(7) 0.061(5) Uani 1 d . . H1A H 0.3845 0.8152 0.0023 0.091 Uiso 1 calc . . H1B H 0.2783 0.8561 -0.0117 0.091 Uiso 1 calc . . H1C H 0.3280 0.7461 0.0052 0.091 Uiso 1 calc . . C2 C -0.1075(19) 0.9858(15) 0.4700(8) 0.072(6) Uani 1 d . . H2A H -0.1665 1.0194 0.4551 0.109 Uiso 1 calc . . H2B H -0.0984 1.0307 0.4925 0.109 Uiso 1 calc . . H2C H -0.1176 0.9346 0.4980 0.109 Uiso 1 calc . . C3 C -0.4422(24) 1.3147(18) 0.3665(16) 0.120(10) Uani 1 d . . H3A H -0.3770 1.3081 0.3368 0.179 Uiso 1 calc . . H3B H -0.4567 1.3547 0.4019 0.179 Uiso 1 calc . . H3C H -0.4950 1.3445 0.3460 0.179 Uiso 1 calc . . C4 C 0.5501(22) 0.2758(21) 0.1987(16) 0.118(10) Uani 1 d . . H4A H 0.6123 0.2352 0.1686 0.177 Uiso 1 calc . . H4B H 0.5413 0.2437 0.2389 0.177 Uiso 1 calc . . H4C H 0.5541 0.3365 0.2038 0.177 Uiso 1 calc . . C12 C 0.2663(11) 0.5989(10) 0.2093(7) 0.038(3) Uani 1 d . . H12A H 0.2948 0.6138 0.1655 0.045 Uiso 1 calc . . H12B H 0.2877 0.5288 0.2125 0.045 Uiso 1 calc . . C13 C 0.3480(11) 1.0124(10) 0.1978(6) 0.034(3) Uani 1 d . . H13A H 0.3578 1.0019 0.1535 0.040 Uiso 1 calc . . H13B H 0.3925 1.0439 0.1993 0.040 Uiso 1 calc . . C23 C -0.1682(10) 1.0550(9) 0.2902(6) 0.032(3) Uani 1 d . . H23A H -0.1748 1.0546 0.3351 0.038 Uiso 1 calc . . H23B H -0.2351 1.0945 0.2848 0.038 Uiso 1 calc . . C111 C 0.2748(11) 0.5974(11) 0.3408(7) 0.041(4) Uani 1 d . . C112 C 0.2227(12) 0.6612(11) 0.3889(7) 0.043(4) Uani 1 d . . H112 H 0.2076 0.7270 0.3805 0.052 Uiso 1 calc . . C113 C 0.1908(17) 0.6332(18) 0.4501(9) 0.077(6) Uani 1 d . . H113 H 0.1534 0.6786 0.4832 0.092 Uiso 1 calc . . C114 C 0.2173(14) 0.5316(15) 0.4611(8) 0.061(5) Uani 1 d . . H114 H 0.1983 0.5095 0.5023 0.073 Uiso 1 calc . . C115 C 0.2708(14) 0.4660(13) 0.4113(9) 0.060(5) Uani 1 d . . H115 H 0.2899 0.3996 0.4190 0.071 Uiso 1 calc . . C116 C 0.2960(13) 0.4976(12) 0.3509(7) 0.047(4) Uani 1 d . . H116 H 0.3267 0.4542 0.3167 0.056 Uiso 1 calc . . C121 C 0.4562(13) 0.5768(11) 0.2315(8) 0.046(4) Uani 1 d . . C122 C 0.5099(14) 0.5670(15) 0.1673(10) 0.071(6) Uani 1 d . . H122 H 0.4737 0.5909 0.1377 0.085 Uiso 1 calc . . C123 C 0.6140(20) 0.5235(20) 0.1466(15) 0.102(8) Uani 1 d . . H123 H 0.6491 0.5192 0.1034 0.123 Uiso 1 calc . . C124 C 0.6675(15) 0.4851(17) 0.1918(15) 0.092(8) Uani 1 d . . H124 H 0.7384 0.4512 0.1778 0.110 Uiso 1 calc . . C125 C 0.6207(15) 0.4954(18) 0.2533(13) 0.086(7) Uani 1 d . . H125 H 0.6589 0.4747 0.2820 0.104 Uiso 1 calc . . C126 C 0.5142(12) 0.5373(15) 0.2753(9) 0.062(5) Uani 1 d . . H126 H 0.4808 0.5396 0.3187 0.074 Uiso 1 calc . . C131 C 0.5137(11) 0.8273(10) 0.1852(6) 0.036(3) Uani 1 d . . C132 C 0.5909(14) 0.7662(14) 0.2113(8) 0.068(6) Uani 1 d . . H132 H 0.5777 0.7618 0.2552 0.081 Uiso 1 calc . . C133 C 0.6876(14) 0.7121(16) 0.1715(11) 0.078(6) Uani 1 d . . H133 H 0.7394 0.6719 0.1890 0.093 Uiso 1 calc . . C134 C 0.7070(14) 0.7172(17) 0.1080(9) 0.074(6) Uani 1 d . . H134 H 0.7721 0.6799 0.0822 0.089 Uiso 1 calc . . C135 C 0.6335(13) 0.7759(14) 0.0804(8) 0.062(5) Uani 1 d . . H135 H 0.6484 0.7806 0.0364 0.074 Uiso 1 calc . . C136 C 0.5330(12) 0.8298(12) 0.1210(8) 0.055(4) Uani 1 d . . H136 H 0.4804 0.8668 0.1034 0.066 Uiso 1 calc . . C141 C 0.4016(11) 0.9129(11) 0.3117(7) 0.043(4) Uani 1 d . . C142 C 0.4735(13) 0.9514(13) 0.3100(8) 0.054(4) Uani 1 d . . H142 H 0.5112 0.9683 0.2717 0.065 Uiso 1 calc . . C143 C 0.4869(17) 0.9639(16) 0.3676(12) 0.073(6) Uani 1 d . . H143 H 0.5353 0.9881 0.3676 0.088 Uiso 1 calc . . C144 C 0.4324(21) 0.9419(18) 0.4214(12) 0.087(8) Uani 1 d . . H144 H 0.4409 0.9526 0.4593 0.104 Uiso 1 calc . . C145 C 0.3621(21) 0.9030(20) 0.4229(10) 0.095(8) Uani 1 d . . H145 H 0.3265 0.8849 0.4616 0.114 Uiso 1 calc . . C146 C 0.3443(13) 0.8907(14) 0.3677(8) 0.060(5) Uani 1 d . . H146 H 0.2945 0.8678 0.3689 0.072 Uiso 1 calc . . C211 C 0.0972(13) 0.6227(10) 0.1641(7) 0.042(4) Uani 1 d . . C212 C 0.0070(14) 0.6063(13) 0.1764(10) 0.064(5) Uani 1 d . . H212 H -0.0335 0.6061 0.2180 0.077 Uiso 1 calc . . C213 C -0.0208(15) 0.5911(15) 0.1276(12) 0.075(7) Uani 1 d . . H213 H -0.0807 0.5803 0.1361 0.090 Uiso 1 calc . . C214 C 0.0364(21) 0.5910(16) 0.0664(12) 0.082(7) Uani 1 d . . H214 H 0.0140 0.5842 0.0333 0.098 Uiso 1 calc . . C215 C 0.1302(22) 0.6015(15) 0.0536(10) 0.083(7) Uani 1 d . . H215 H 0.1727 0.5967 0.0121 0.099 Uiso 1 calc . . C216 C 0.1584(18) 0.6185(14) 0.1019(9) 0.067(6) Uani 1 d . . H216 H 0.2194 0.6275 0.0933 0.080 Uiso 1 calc . . C221 C 0.0793(10) 0.5896(10) 0.2972(7) 0.034(3) Uani 1 d . . C222 C 0.1097(14) 0.4879(12) 0.2935(8) 0.055(5) Uani 1 d . . H222 H 0.1538 0.4540 0.2560 0.066 Uiso 1 calc . . C223 C 0.0731(15) 0.4387(12) 0.3465(10) 0.059(5) Uani 1 d . . H223 H 0.0921 0.3718 0.3444 0.071 Uiso 1 calc . . C224 C 0.0129(16) 0.4865(14) 0.3982(11) 0.069(5) Uani 1 d . . H224 H -0.0119 0.4525 0.4327 0.083 Uiso 1 calc . . C225 C -0.0164(17) 0.5830(16) 0.4053(9) 0.069(5) Uani 1 d . . H225 H -0.0582 0.6137 0.4442 0.083 Uiso 1 calc . . C226 C 0.0161(12) 0.6351(12) 0.3545(8) 0.049(4) Uani 1 d . . H226 H -0.0048 0.7020 0.3588 0.059 Uiso 1 calc . . C231 C -0.2038(12) 0.8778(11) 0.3243(7) 0.042(4) Uani 1 d . . C232 C -0.2105(15) 0.7928(13) 0.3081(9) 0.062(5) Uani 1 d . . H232 H -0.1838 0.7715 0.2660 0.075 Uiso 1 calc . . C233 C -0.2553(17) 0.7421(14) 0.3534(9) 0.076(7) Uani 1 d . . H233 H -0.2560 0.6846 0.3424 0.091 Uiso 1 calc . . C234 C -0.3005(14) 0.7756(15) 0.4162(9) 0.064(5) Uani 1 d . . H234 H -0.3315 0.7407 0.4469 0.077 Uiso 1 calc . . C235 C -0.2991(13) 0.8592(15) 0.4326(8) 0.058(5) Uani 1 d . . H235 H -0.3303 0.8817 0.4744 0.069 Uiso 1 calc . . C236 C -0.2515(12) 0.9119(12) 0.3873(7) 0.045(4) Uani 1 d . . H236 H -0.2516 0.9694 0.3990 0.054 Uiso 1 calc . . C241 C -0.1724(10) 0.9390(10) 0.1957(6) 0.033(3) Uani 1 d . . C242 C -0.2737(12) 1.0008(11) 0.1988(7) 0.044(4) Uani 1 d . . H242 H -0.3169 1.0407 0.2341 0.053 Uiso 1 calc . . C243 C -0.3082(14) 1.0005(14) 0.1461(9) 0.059(5) Uani 1 d . . H243 H -0.3746 1.0422 0.1464 0.070 Uiso 1 calc . . C244 C -0.2475(17) 0.9416(15) 0.0963(9) 0.064(5) Uani 1 d . . H244 H -0.2730 0.9417 0.0631 0.077 Uiso 1 calc . . C245 C -0.1448(16) 0.8789(14) 0.0926(8) 0.060(5) Uani 1 d . . H245 H -0.1032 0.8377 0.0576 0.072 Uiso 1 calc . . C246 C -0.1069(12) 0.8802(12) 0.1434(7) 0.046(4) Uani 1 d . . H246 H -0.0389 0.8420 0.1415 0.055 Uiso 1 calc . . C311 C 0.2048(11) 1.1481(9) 0.3075(7) 0.035(3) Uani 1 d . . C312 C 0.2853(15) 1.1676(13) 0.3103(9) 0.057(5) Uani 1 d . . H312 H 0.3425 1.1597 0.2752 0.069 Uiso 1 calc . . C313 C 0.2760(16) 1.1998(14) 0.3686(10) 0.064(5) Uani 1 d . . H313 H 0.3310 1.2099 0.3732 0.077 Uiso 1 calc . . C314 C 0.1916(23) 1.2175(14) 0.4191(10) 0.081(8) Uani 1 d . . H314 H 0.1891 1.2392 0.4574 0.098 Uiso 1 calc . . C315 C 0.1105(20) 1.2032(15) 0.4137(11) 0.082(7) Uani 1 d . . H315 H 0.0505 1.2190 0.4476 0.098 Uiso 1 calc . . C316 C 0.1159(14) 1.1650(11) 0.3576(8) 0.049(4) Uani 1 d . . H316 H 0.0622 1.1516 0.3541 0.059 Uiso 1 calc . . C321 C 0.1901(10) 1.1895(9) 0.1741(7) 0.033(3) Uani 1 d . . C322 C 0.1999(11) 1.2752(10) 0.1788(7) 0.038(3) Uani 1 d . . H322 H 0.2169 1.2870 0.2131 0.046 Uiso 1 calc . . C323 C 0.1841(16) 1.3440(12) 0.1315(9) 0.059(5) Uani 1 d . . H323 H 0.1923 1.4017 0.1330 0.071 Uiso 1 calc . . C324 C 0.1559(16) 1.3258(12) 0.0821(9) 0.063(5) Uani 1 d . . H324 H 0.1441 1.3719 0.0506 0.075 Uiso 1 calc . . C325 C 0.1453(15) 1.2400(13) 0.0793(8) 0.058(5) Uani 1 d . . H325 H 0.1262 1.2281 0.0460 0.070 Uiso 1 calc . . C326 C 0.1627(12) 1.1729(10) 0.1252(7) 0.043(4) Uani 1 d . . H326 H 0.1557 1.1147 0.1232 0.051 Uiso 1 calc . . C331 C -0.1200(10) 1.2284(9) 0.2833(7) 0.030(3) Uani 1 d . . C332 C -0.0825(13) 1.2953(10) 0.2476(7) 0.044(4) Uani 1 d . . H332 H -0.0479 1.2848 0.2044 0.053 Uiso 1 calc . . C333 C -0.0984(14) 1.3786(13) 0.2783(11) 0.062(5) Uani 1 d . . H333 H -0.0683 1.4209 0.2563 0.075 Uiso 1 calc . . C334 C -0.1557(15) 1.3983(13) 0.3386(11) 0.068(6) Uani 1 d . . H334 H -0.1690 1.4566 0.3569 0.082 Uiso 1 calc . . C335 C -0.1960(15) 1.3348(15) 0.3746(9) 0.066(5) Uani 1 d . . H335 H -0.2368 1.3500 0.4165 0.080 Uiso 1 calc . . C336 C -0.1741(13) 1.2470(11) 0.3466(7) 0.046(4) Uani 1 d . . H336 H -0.1963 1.2009 0.3708 0.055 Uiso 1 calc . . C341 C -0.0891(11) 1.1358(9) 0.1679(7) 0.035(3) Uani 1 d . . C342 C -0.1754(13) 1.2154(12) 0.1556(7) 0.047(4) Uani 1 d . . H342 H -0.2265 1.2562 0.1887 0.056 Uiso 1 calc . . C343 C -0.1822(13) 1.2309(14) 0.0947(9) 0.066(5) Uani 1 d . . H343 H -0.2379 1.2820 0.0860 0.079 Uiso 1 calc . . C344 C -0.1037(19) 1.1686(17) 0.0457(10) 0.078(7) Uani 1 d . . H344 H -0.1071 1.1808 0.0042 0.094 Uiso 1 calc . . C345 C -0.0218(14) 1.0900(14) 0.0569(8) 0.059(5) Uani 1 d . . H345 H 0.0294 1.0493 0.0239 0.071 Uiso 1 calc . . C346 C -0.0182(11) 1.0738(10) 0.1180(7) 0.039(3) Uani 1 d . . H346 H 0.0343 1.0187 0.1265 0.047 Uiso 1 calc . . O13 O 0.3988(9) 0.6469(11) 0.4538(6) 0.076(4) Uani 1 d . . O14 O -0.3697(11) 0.9785(10) -0.0203(7) 0.075(4) Uani 1 d . . O15 O 0.5406(12) 0.8712(15) -0.0507(7) 0.103(6) Uani 1 d . . O16 O -0.3846(10) 1.5722(9) 0.4256(11) 0.121(8) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0276(3) 0.0268(3) 0.0442(3) 0.0036(2) -0.0153(2) -0.0094(2) Hg2 0.0226(3) 0.0231(3) 0.0396(3) -0.0015(2) -0.0106(2) -0.0051(2) Hg3 0.0234(3) 0.0263(3) 0.0448(3) -0.0004(2) -0.0090(2) -0.0087(2) P12 0.026(2) 0.024(2) 0.045(2) 0.004(2) -0.014(2) -0.004(2) P13 0.020(2) 0.031(2) 0.039(2) 0.0029(15) -0.011(2) -0.008(2) P21 0.030(2) 0.023(2) 0.044(2) -0.0004(15) -0.016(2) -0.008(2) P23 0.019(2) 0.022(2) 0.036(2) -0.0002(14) -0.0101(14) -0.0058(14) P31 0.026(2) 0.024(2) 0.038(2) 0.0020(14) -0.009(2) -0.011(2) P32 0.018(2) 0.021(2) 0.038(2) -0.0035(14) -0.0059(14) -0.0033(14) S1 0.032(2) 0.036(2) 0.033(2) 0.0014(15) -0.008(2) -0.013(2) S2 0.043(2) 0.038(2) 0.038(2) -0.001(2) -0.013(2) -0.014(2) S3 0.041(2) 0.063(3) 0.057(3) -0.003(2) -0.006(2) -0.017(2) S4 0.044(3) 0.068(3) 0.077(3) -0.014(3) -0.019(2) -0.016(2) O1 0.050(7) 0.039(6) 0.056(7) 0.000(5) -0.009(6) 0.005(5) O2 0.044(7) 0.068(8) 0.058(7) -0.001(6) -0.005(5) -0.040(6) O3 0.072(8) 0.033(6) 0.065(7) -0.004(5) -0.002(6) -0.027(6) O4 0.100(13) 0.097(12) 0.163(16) -0.059(12) -0.097(13) 0.027(10) O5 0.062(8) 0.060(8) 0.045(6) -0.014(5) -0.005(6) -0.029(6) O6 0.068(8) 0.039(7) 0.067(8) -0.014(6) 0.006(6) -0.021(6) O7 0.075(10) 0.104(12) 0.061(8) -0.023(8) -0.016(7) -0.026(9) O8 0.079(10) 0.085(10) 0.070(8) 0.020(7) -0.038(7) -0.038(8) O9 0.055(9) 0.167(17) 0.072(10) -0.017(10) 0.020(7) -0.052(11) O10 0.049(8) 0.063(9) 0.139(14) -0.042(9) 0.005(9) -0.008(7) O11 0.071(9) 0.053(8) 0.115(11) -0.032(8) -0.031(8) -0.012(7) O12 0.179(21) 0.148(18) 0.089(12) 0.038(12) -0.048(13) -0.093(17) C1 0.070(13) 0.088(14) 0.028(8) -0.009(8) -0.003(8) -0.041(11) C2 0.111(18) 0.073(13) 0.041(10) -0.001(9) -0.004(10) -0.057(13) C3 0.118(23) 0.055(15) 0.163(27) 0.039(16) -0.049(20) -0.016(15) C4 0.103(21) 0.098(20) 0.191(30) 0.003(19) -0.096(22) -0.038(17) C12 0.039(9) 0.021(7) 0.054(9) -0.002(6) -0.017(7) -0.009(6) C13 0.030(8) 0.027(7) 0.039(8) -0.003(6) -0.006(6) -0.008(6) C23 0.023(7) 0.021(7) 0.040(8) -0.012(6) 0.010(6) -0.009(6) C111 0.021(7) 0.044(9) 0.054(9) 0.005(7) -0.010(7) -0.011(7) C112 0.040(9) 0.038(9) 0.047(9) -0.006(7) -0.010(7) -0.011(7) C113 0.069(14) 0.093(17) 0.051(11) -0.004(11) -0.013(10) -0.017(12) C114 0.044(10) 0.073(13) 0.047(10) 0.013(9) -0.011(8) -0.009(10) C115 0.057(11) 0.047(10) 0.071(12) 0.028(9) -0.019(10) -0.024(9) C116 0.047(10) 0.043(9) 0.049(9) 0.013(7) -0.026(8) -0.011(8) C121 0.049(10) 0.026(8) 0.066(11) 0.010(7) -0.014(8) -0.021(7) C122 0.033(10) 0.073(14) 0.084(14) 0.003(11) 0.003(10) -0.013(10) C123 0.063(16) 0.087(18) 0.156(25) 0.003(17) -0.031(17) -0.029(14) C124 0.028(11) 0.065(14) 0.157(25) -0.008(15) 0.000(14) -0.010(10) C125 0.032(11) 0.101(18) 0.113(19) 0.027(15) -0.012(12) -0.027(12) C126 0.023(9) 0.081(14) 0.072(12) 0.011(10) -0.019(8) -0.011(9) C131 0.028(8) 0.035(8) 0.032(8) 0.015(6) -0.003(6) -0.009(7) C132 0.050(11) 0.070(13) 0.055(11) 0.010(9) -0.031(9) 0.014(10) C133 0.038(11) 0.077(14) 0.089(15) -0.005(11) -0.029(10) 0.016(10) C134 0.035(10) 0.104(17) 0.058(12) -0.011(11) 0.003(9) -0.011(11) C135 0.036(10) 0.068(12) 0.054(10) -0.006(9) -0.001(8) -0.001(9) C136 0.033(9) 0.048(10) 0.063(11) 0.009(8) -0.007(8) -0.004(8) C141 0.022(8) 0.045(9) 0.034(8) -0.010(7) 0.003(6) 0.009(7) C142 0.049(10) 0.065(12) 0.067(11) 0.008(9) -0.040(9) -0.026(9) C143 0.057(13) 0.076(14) 0.096(17) -0.022(12) -0.046(13) -0.011(11) C144 0.082(17) 0.084(16) 0.082(17) -0.034(13) -0.054(15) 0.011(13) C145 0.096(19) 0.109(20) 0.046(12) -0.008(11) -0.029(12) 0.000(16) C146 0.030(9) 0.071(13) 0.055(11) 0.001(9) -0.003(8) -0.003(9) C211 0.063(11) 0.028(8) 0.043(9) 0.007(6) -0.036(8) -0.012(8) C212 0.050(11) 0.040(10) 0.098(15) -0.012(9) -0.029(10) -0.005(9) C213 0.049(12) 0.070(13) 0.111(18) -0.040(12) -0.055(12) 0.005(10) C214 0.106(19) 0.065(13) 0.090(17) -0.010(12) -0.073(16) -0.013(13) C215 0.133(22) 0.063(13) 0.075(14) 0.009(11) -0.056(15) -0.044(14) C216 0.109(17) 0.056(12) 0.060(12) -0.005(9) -0.035(12) -0.047(12) C221 0.023(7) 0.031(8) 0.051(9) 0.000(6) -0.013(7) -0.011(6) C222 0.059(11) 0.039(10) 0.050(10) -0.008(8) -0.013(9) -0.002(8) C223 0.055(11) 0.032(9) 0.084(13) -0.002(9) -0.012(10) -0.017(9) C224 0.058(12) 0.043(11) 0.105(16) 0.010(11) -0.025(12) -0.021(10) C225 0.074(14) 0.083(15) 0.054(11) 0.003(10) -0.015(10) -0.038(12) C226 0.039(9) 0.047(10) 0.048(9) -0.005(8) -0.008(8) -0.007(8) C231 0.035(8) 0.039(9) 0.042(8) 0.011(7) -0.013(7) -0.008(7) C232 0.062(12) 0.043(10) 0.078(12) -0.004(9) -0.003(10) -0.028(9) C233 0.085(15) 0.057(12) 0.072(13) -0.005(10) 0.028(11) -0.052(12) C234 0.039(10) 0.070(13) 0.070(13) 0.016(10) -0.003(9) -0.024(10) C235 0.043(10) 0.074(13) 0.042(9) 0.000(9) -0.007(8) -0.013(9) C236 0.037(9) 0.048(10) 0.036(8) -0.003(7) 0.000(7) -0.010(8) C241 0.024(7) 0.038(8) 0.040(8) 0.004(6) -0.018(6) -0.010(6) C242 0.033(9) 0.038(9) 0.053(9) 0.001(7) -0.016(7) -0.004(7) C243 0.046(10) 0.071(12) 0.066(12) 0.001(10) -0.040(9) -0.013(9) C244 0.082(15) 0.074(13) 0.069(12) 0.018(10) -0.049(12) -0.048(12) C245 0.085(15) 0.068(12) 0.044(10) 0.008(8) -0.016(9) -0.051(12) C246 0.038(9) 0.054(10) 0.033(8) 0.006(7) -0.012(7) -0.006(8) C311 0.037(8) 0.013(6) 0.049(9) 0.001(6) -0.014(7) -0.005(6) C312 0.074(13) 0.048(10) 0.072(12) 0.013(9) -0.047(10) -0.030(10) C313 0.065(13) 0.053(11) 0.074(13) -0.021(10) -0.029(11) -0.010(10) C314 0.125(22) 0.049(12) 0.059(13) -0.001(9) -0.057(15) 0.001(13) C315 0.088(17) 0.053(13) 0.075(14) -0.015(10) 0.003(13) -0.014(12) C316 0.057(11) 0.031(8) 0.054(10) 0.004(7) -0.006(8) -0.021(8) C321 0.016(7) 0.019(7) 0.047(8) -0.006(6) 0.000(6) 0.004(5) C322 0.037(8) 0.026(8) 0.051(9) 0.006(6) -0.019(7) -0.008(7) C323 0.081(14) 0.034(9) 0.070(12) 0.013(8) -0.038(11) -0.022(9) C324 0.085(14) 0.026(9) 0.065(11) 0.006(8) -0.021(10) -0.012(9) C325 0.078(13) 0.047(10) 0.043(9) 0.005(8) -0.031(9) -0.010(9) C326 0.047(9) 0.026(8) 0.047(9) -0.002(7) 0.003(7) -0.019(7) C331 0.030(8) 0.018(7) 0.046(8) -0.005(6) -0.022(7) -0.005(6) C332 0.051(10) 0.017(7) 0.052(9) -0.005(6) -0.004(8) -0.010(7) C333 0.047(11) 0.040(10) 0.110(16) -0.012(10) -0.025(11) -0.023(9) C334 0.052(11) 0.041(10) 0.107(16) -0.038(11) -0.004(11) -0.018(9) C335 0.057(12) 0.066(13) 0.058(11) -0.030(10) 0.000(9) -0.011(10) C336 0.046(10) 0.038(9) 0.049(9) -0.007(7) -0.008(8) -0.014(8) C341 0.034(8) 0.020(7) 0.051(9) -0.002(6) -0.019(7) -0.005(6) C342 0.047(10) 0.058(10) 0.037(8) -0.001(7) -0.021(7) -0.016(8) C343 0.027(9) 0.064(12) 0.069(12) -0.005(10) 0.001(8) 0.010(8) C344 0.099(17) 0.098(17) 0.071(13) 0.034(12) -0.063(13) -0.051(15) C345 0.052(11) 0.064(12) 0.049(10) -0.011(9) -0.007(9) -0.013(9) C346 0.033(8) 0.024(7) 0.058(10) -0.005(7) -0.011(7) -0.011(6) O13 0.037(7) 0.119(12) 0.083(9) -0.031(8) -0.007(6) -0.041(8) O14 0.066(9) 0.081(10) 0.082(9) 0.005(7) -0.005(7) -0.047(8) O15 0.072(10) 0.169(17) 0.075(10) -0.033(10) -0.010(8) -0.053(11) O16 0.039(8) 0.030(7) 0.277(24) -0.009(10) -0.028(11) -0.008(6) _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 Hg1 P12 2.515(4) . ? Hg1 P13 2.522(4) . ? Hg1 O1 2.630(11) . ? Hg1 Hg3 2.7449(11) . ? Hg1 Hg2 2.8191(9) . ? Hg1 O4 3.97(2) . ? Hg2 P21 2.523(3) . ? Hg2 P23 2.542(3) . ? Hg2 O5 2.685(10) . ? Hg2 Hg3 2.7780(9) . ? Hg2 O2 2.981(11) . ? Hg3 P31 2.502(3) . ? Hg3 P32 2.511(3) . ? Hg3 O6 2.516(12) . ? Hg3 O3 3.264(11) . ? P12 C121 1.80(2) . ? P12 C12 1.832(15) . ? P12 C111 1.84(2) . ? P13 C131 1.807(14) . ? P13 C141 1.82(2) . ? P13 C13 1.826(14) . ? P21 C221 1.801(14) . ? P21 C12 1.81(2) . ? P21 C211 1.829(14) . ? P23 C241 1.801(13) . ? P23 C231 1.81(2) . ? P23 C23 1.809(13) . ? P31 C311 1.837(14) . ? P31 C321 1.842(14) . ? P31 C13 1.860(14) . ? P32 C341 1.785(14) . ? P32 C331 1.815(12) . ? P32 C23 1.851(13) . ? S1 O2 1.402(11) . ? S1 O1 1.459(12) . ? S1 O3 1.484(11) . ? S1 C1 1.74(2) . ? S2 O4 1.439(14) . ? S2 O5 1.450(11) . ? S2 O6 1.460(12) . ? S2 C2 1.74(2) . ? S3 O9 1.430(13) . ? S3 O7 1.440(13) . ? S3 O8 1.449(14) . ? S3 C3 1.79(2) . ? S4 O10 1.410(14) . ? S4 O12 1.44(2) . ? S4 O11 1.465(14) . ? S4 C4 1.75(2) . ? C111 C112 1.33(2) . ? C111 C116 1.41(2) . ? C112 C113 1.36(2) . ? C113 C114 1.43(3) . ? C114 C115 1.37(3) . ? C115 C116 1.36(2) . ? C121 C122 1.39(3) . ? C121 C126 1.42(2) . ? C122 C123 1.36(3) . ? C123 C124 1.40(4) . ? C124 C125 1.32(3) . ? C125 C126 1.39(3) . ? C131 C136 1.36(2) . ? C131 C132 1.39(2) . ? C132 C133 1.39(3) . ? C133 C134 1.35(3) . ? C134 C135 1.37(3) . ? C135 C136 1.43(2) . ? C141 C146 1.36(2) . ? C141 C142 1.40(2) . ? C142 C143 1.40(3) . ? C143 C144 1.30(3) . ? C144 C145 1.39(4) . ? C145 C146 1.38(3) . ? C211 C216 1.38(3) . ? C211 C212 1.40(2) . ? C212 C213 1.35(3) . ? C213 C214 1.35(3) . ? C214 C215 1.41(3) . ? C215 C216 1.35(3) . ? C221 C226 1.38(2) . ? C221 C222 1.41(2) . ? C222 C223 1.39(2) . ? C223 C224 1.29(3) . ? C224 C225 1.35(3) . ? C225 C226 1.37(2) . ? C231 C236 1.40(2) . ? C231 C232 1.42(2) . ? C232 C233 1.36(2) . ? C233 C234 1.39(3) . ? C234 C235 1.36(3) . ? C235 C236 1.40(2) . ? C241 C246 1.38(2) . ? C241 C242 1.40(2) . ? C242 C243 1.42(2) . ? C243 C244 1.33(3) . ? C244 C245 1.42(3) . ? C245 C246 1.42(2) . ? C311 C312 1.37(2) . ? C311 C316 1.38(2) . ? C312 C313 1.38(2) . ? C313 C314 1.35(3) . ? C314 C315 1.36(3) . ? C315 C316 1.40(3) . ? C321 C326 1.35(2) . ? C321 C322 1.38(2) . ? C322 C323 1.39(2) . ? C323 C324 1.38(3) . ? C324 C325 1.37(3) . ? C325 C326 1.36(2) . ? C331 C336 1.38(2) . ? C331 C332 1.39(2) . ? C332 C333 1.39(2) . ? C333 C334 1.33(3) . ? C334 C335 1.38(3) . ? C335 C336 1.40(2) . ? C341 C346 1.38(2) . ? C341 C342 1.43(2) . ? C342 C343 1.37(2) . ? C343 C344 1.40(3) . ? C344 C345 1.38(3) . ? C345 C346 1.36(2) . ? 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 P12 Hg1 P13 116.44(12) . . ? P12 Hg1 O1 80.0(3) . . ? P13 Hg1 O1 94.5(3) . . ? P12 Hg1 Hg3 150.92(9) . . ? P13 Hg1 Hg3 92.44(8) . . ? O1 Hg1 Hg3 102.2(2) . . ? P12 Hg1 Hg2 91.61(9) . . ? P13 Hg1 Hg2 151.74(8) . . ? O1 Hg1 Hg2 86.6(3) . . ? Hg3 Hg1 Hg2 59.89(2) . . ? P12 Hg1 O4 96.3(3) . . ? P13 Hg1 O4 101.7(3) . . ? O1 Hg1 O4 163.2(4) . . ? Hg3 Hg1 O4 73.2(2) . . ? Hg2 Hg1 O4 77.1(2) . . ? P21 Hg2 P23 115.96(11) . . ? P21 Hg2 O5 107.7(3) . . ? P23 Hg2 O5 75.6(3) . . ? P21 Hg2 Hg3 149.84(9) . . ? P23 Hg2 Hg3 93.82(8) . . ? O5 Hg2 Hg3 83.2(2) . . ? P21 Hg2 Hg1 92.08(9) . . ? P23 Hg2 Hg1 151.69(8) . . ? O5 Hg2 Hg1 92.9(3) . . ? Hg3 Hg2 Hg1 58.73(3) . . ? P21 Hg2 O2 82.3(2) . . ? P23 Hg2 O2 104.9(2) . . ? O5 Hg2 O2 168.8(3) . . ? Hg3 Hg2 O2 85.6(2) . . ? Hg1 Hg2 O2 81.5(2) . . ? P31 Hg3 P32 111.30(11) . . ? P31 Hg3 O6 104.4(3) . . ? P32 Hg3 O6 78.6(3) . . ? P31 Hg3 Hg1 95.23(8) . . ? P32 Hg3 Hg1 152.95(8) . . ? O6 Hg3 Hg1 100.4(3) . . ? P31 Hg3 Hg2 155.56(8) . . ? P32 Hg3 Hg2 91.61(8) . . ? O6 Hg3 Hg2 87.9(3) . . ? Hg1 Hg3 Hg2 61.38(2) . . ? P31 Hg3 O3 79.9(2) . . ? P32 Hg3 O3 107.3(2) . . ? O6 Hg3 O3 171.1(3) . . ? Hg1 Hg3 O3 71.2(2) . . ? Hg2 Hg3 O3 85.4(2) . . ? C121 P12 C12 106.5(7) . . ? C121 P12 C111 107.8(7) . . ? C12 P12 C111 107.4(7) . . ? C121 P12 Hg1 113.9(5) . . ? C12 P12 Hg1 105.8(4) . . ? C111 P12 Hg1 115.0(5) . . ? C131 P13 C141 106.7(7) . . ? C131 P13 C13 102.9(6) . . ? C141 P13 C13 107.8(7) . . ? C131 P13 Hg1 115.2(5) . . ? C141 P13 Hg1 113.7(5) . . ? C13 P13 Hg1 109.8(5) . . ? C221 P21 C12 106.7(7) . . ? C221 P21 C211 105.0(7) . . ? C12 P21 C211 104.5(7) . . ? C221 P21 Hg2 114.8(5) . . ? C12 P21 Hg2 111.0(5) . . ? C211 P21 Hg2 114.0(5) . . ? C241 P23 C231 104.2(7) . . ? C241 P23 C23 107.6(7) . . ? C231 P23 C23 106.5(7) . . ? C241 P23 Hg2 116.3(5) . . ? C231 P23 Hg2 110.8(5) . . ? C23 P23 Hg2 110.9(5) . . ? C311 P31 C321 109.8(6) . . ? C311 P31 C13 108.3(6) . . ? C321 P31 C13 101.9(6) . . ? C311 P31 Hg3 115.8(5) . . ? C321 P31 Hg3 111.8(5) . . ? C13 P31 Hg3 108.3(5) . . ? C341 P32 C331 106.0(6) . . ? C341 P32 C23 107.3(7) . . ? C331 P32 C23 107.1(6) . . ? C341 P32 Hg3 114.3(5) . . ? C331 P32 Hg3 112.0(4) . . ? C23 P32 Hg3 109.9(5) . . ? O2 S1 O1 112.5(7) . . ? O2 S1 O3 111.8(7) . . ? O1 S1 O3 112.3(8) . . ? O2 S1 C1 107.6(8) . . ? O1 S1 C1 105.9(8) . . ? O3 S1 C1 106.3(8) . . ? O4 S2 O5 111.8(9) . . ? O4 S2 O6 115.3(11) . . ? O5 S2 O6 110.1(7) . . ? O4 S2 C2 108.9(11) . . ? O5 S2 C2 106.3(8) . . ? O6 S2 C2 103.7(8) . . ? O9 S3 O7 114.4(10) . . ? O9 S3 O8 114.3(10) . . ? O7 S3 O8 112.0(9) . . ? O9 S3 C3 106.7(13) . . ? O7 S3 C3 104.4(13) . . ? O8 S3 C3 103.8(12) . . ? O10 S4 O12 112.2(13) . . ? O10 S4 O11 112.5(9) . . ? O12 S4 O11 113.1(11) . . ? O10 S4 C4 109.0(13) . . ? O12 S4 C4 103.5(15) . . ? O11 S4 C4 105.8(11) . . ? S1 O1 Hg1 109.8(6) . . ? S1 O2 Hg2 110.9(6) . . ? S1 O3 Hg3 105.7(5) . . ? S2 O4 Hg1 87.3(8) . . ? S2 O5 Hg2 122.0(6) . . ? S2 O6 Hg3 121.8(6) . . ? P21 C12 P12 113.4(8) . . ? P13 C13 P31 113.4(7) . . ? P23 C23 P32 112.5(6) . . ? C112 C111 C116 120.8(15) . . ? C112 C111 P12 119.9(12) . . ? C116 C111 P12 119.3(12) . . ? C111 C112 C113 122.1(17) . . ? C112 C113 C114 117.2(18) . . ? C115 C114 C113 120.4(16) . . ? C116 C115 C114 120.3(16) . . ? C115 C116 C111 118.9(16) . . ? C122 C121 C126 117.4(16) . . ? C122 C121 P12 122.3(14) . . ? C126 C121 P12 120.2(13) . . ? C123 C122 C121 121.7(23) . . ? C122 C123 C124 118.5(26) . . ? C125 C124 C123 122.2(21) . . ? C124 C125 C126 119.9(22) . . ? C125 C126 C121 120.0(18) . . ? C136 C131 C132 119.4(14) . . ? C136 C131 P13 120.5(11) . . ? C132 C131 P13 119.9(11) . . ? C133 C132 C131 119.7(16) . . ? C134 C133 C132 120.5(17) . . ? C133 C134 C135 121.6(17) . . ? C134 C135 C136 118.1(16) . . ? C131 C136 C135 120.4(15) . . ? C146 C141 C142 121.2(16) . . ? C146 C141 P13 120.9(14) . . ? C142 C141 P13 117.9(12) . . ? C143 C142 C141 118.1(18) . . ? C144 C143 C142 120.7(20) . . ? C143 C144 C145 121.1(19) . . ? C146 C145 C144 120.8(23) . . ? C141 C146 C145 118.1(21) . . ? C216 C211 C212 119.0(15) . . ? C216 C211 P21 121.8(13) . . ? C212 C211 P21 119.2(13) . . ? C213 C212 C211 119.7(20) . . ? C212 C213 C214 121.6(21) . . ? C213 C214 C215 119.1(17) . . ? C216 C215 C214 119.9(22) . . ? C215 C216 C211 120.4(21) . . ? C226 C221 C222 117.4(14) . . ? C226 C221 P21 122.0(11) . . ? C222 C221 P21 120.6(12) . . ? C223 C222 C221 119.5(15) . . ? C224 C223 C222 119.5(17) . . ? C223 C224 C225 123.7(19) . . ? C224 C225 C226 119.1(19) . . ? C225 C226 C221 120.6(16) . . ? C236 C231 C232 118.1(15) . . ? C236 C231 P23 123.9(13) . . ? C232 C231 P23 118.0(12) . . ? C233 C232 C231 120.7(17) . . ? C232 C233 C234 120.5(18) . . ? C235 C234 C233 120.0(16) . . ? C234 C235 C236 120.9(16) . . ? C235 C236 C231 119.7(16) . . ? C246 C241 C242 122.0(13) . . ? C246 C241 P23 119.1(10) . . ? C242 C241 P23 118.8(11) . . ? C241 C242 C243 117.7(14) . . ? C244 C243 C242 121.3(16) . . ? C243 C244 C245 121.6(16) . . ? C244 C245 C246 118.5(16) . . ? C241 C246 C245 119.0(15) . . ? C312 C311 C316 123.5(15) . . ? C312 C311 P31 120.0(12) . . ? C316 C311 P31 116.5(12) . . ? C311 C312 C313 115.6(18) . . ? C314 C313 C312 123.6(20) . . ? C313 C314 C315 119.4(18) . . ? C314 C315 C316 120.7(20) . . ? C311 C316 C315 117.0(18) . . ? C326 C321 C322 121.0(13) . . ? C326 C321 P31 118.3(11) . . ? C322 C321 P31 120.7(11) . . ? C321 C322 C323 118.9(14) . . ? C324 C323 C322 119.2(15) . . ? C325 C324 C323 120.5(15) . . ? C326 C325 C324 119.7(16) . . ? C321 C326 C325 120.7(14) . . ? C336 C331 C332 119.9(12) . . ? C336 C331 P32 122.5(11) . . ? C332 C331 P32 116.8(10) . . ? C331 C332 C333 118.2(15) . . ? C334 C333 C332 121.1(17) . . ? C333 C334 C335 121.8(16) . . ? C334 C335 C336 118.3(16) . . ? C331 C336 C335 120.3(15) . . ? C346 C341 C342 118.2(13) . . ? C346 C341 P32 119.9(11) . . ? C342 C341 P32 121.8(11) . . ? C343 C342 C341 119.4(14) . . ? C342 C343 C344 119.0(16) . . ? C345 C344 C343 122.3(17) . . ? C346 C345 C344 117.8(16) . . ? C345 C346 C341 123.0(14) . . ? _refine_diff_density_max 2.473 _refine_diff_density_min -2.169 _refine_diff_density_rms .242 #===END data_5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C79 H78 Hg3 O12 P6 S4' _chemical_formula_weight 2135.24 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.950(2) _cell_length_b 21.752(3) _cell_length_c 19.594(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.13(1) _cell_angle_gamma 90.00 _cell_volume 9521.4(21) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.9 _cell_measurement_theta_max 12.0 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method ? _exptl_crystal_F_000 4168 _exptl_absorpt_coefficient_mu 5.064 _exptl_absorpt_correction_type PSI-scan _exptl_absorpt_correction_T_min 0.541 _exptl_absorpt_correction_T_max 0.983 _exptl_special_details ; Disordering of the two outward CH3SO3-anions, S3:S4:S5:S6 = 0.666:0.666:0.333:0.333; for the anions at S4, S5 and S6 restraints for S=O-bonds were necessary, and for S5 restraints for C5..O. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9145 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0963 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 21.50 _reflns_number_total 7469 _reflns_number_observed 4783 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 825 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+107.1541P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6644 _refine_ls_number_parameters 562 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_obs 0.0628 _refine_ls_wR_factor_all 0.1810 _refine_ls_wR_factor_obs 0.1436 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.128 _refine_ls_restrained_S_all 1.119 _refine_ls_restrained_S_obs 1.127 _refine_ls_shift/esd_max -0.031 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg1 Hg 0.31607(4) 0.63204(4) 0.16507(6) 0.0493(4) Uani 1 d . . Hg2 Hg 0.32599(4) 0.50483(4) 0.16475(5) 0.0460(3) Uani 1 d . . Hg3 Hg 0.21658(4) 0.56106(4) 0.14740(6) 0.0575(4) Uani 1 d . . P12 P 0.4249(3) 0.6490(3) 0.1807(3) 0.042(2) Uani 1 d . . P13 P 0.2595(3) 0.7324(3) 0.1478(4) 0.049(2) Uani 1 d . . P21 P 0.4370(3) 0.5093(3) 0.1845(3) 0.041(2) Uani 1 d . . P23 P 0.2873(3) 0.3996(3) 0.1788(4) 0.047(2) Uani 1 d . . P31 P 0.1510(3) 0.6516(3) 0.1430(4) 0.051(2) Uani 1 d . . P32 P 0.1642(3) 0.4597(3) 0.1244(4) 0.045(2) Uani 1 d . . S1 S 0.2975(3) 0.5761(4) 0.3340(4) 0.066(2) Uani 1 d . . S2 S 0.3030(5) 0.5593(5) -0.0150(4) 0.106(3) Uani 1 d . . O1 O 0.2927(11) 0.6367(9) 0.3024(10) 0.115(8) Uani 1 d . . O2 O 0.3560(10) 0.5523(11) 0.3559(16) 0.161(11) Uani 1 d . . O3 O 0.2523(9) 0.5351(9) 0.2885(10) 0.096(6) Uani 1 d . . O4 O 0.3353(16) 0.6048(17) 0.0138(22) 0.382(39) Uani 1 d . . O5 O 0.3104(8) 0.5038(9) 0.0249(10) 0.085(6) Uani 1 d . . O6 O 0.2371(15) 0.5798(15) -0.0185(36) 0.380(39) Uani 1 d . . C1 C 0.2850(16) 0.5845(16) 0.4132(20) 0.124(12) Uiso 1 d . . H1A H 0.2456 0.6008 0.4030 0.186 Uiso 1 calc . . H1B H 0.3141 0.6122 0.4449 0.186 Uiso 1 calc . . H1C H 0.2884 0.5452 0.4368 0.186 Uiso 1 calc . . C2 C 0.2754(31) 0.5456(31) -0.1053(37) 0.260(28) Uiso 1 d . . H2A H 0.2521 0.5085 -0.1148 0.390 Uiso 1 calc . . H2B H 0.3078 0.5410 -0.1228 0.390 Uiso 1 calc . . H2C H 0.2505 0.5794 -0.1301 0.390 Uiso 1 calc . . C12 C 0.4518(9) 0.5817(9) 0.1480(11) 0.037(6) Uiso 1 d . . H12A H 0.4947 0.5857 0.1604 0.044 Uiso 1 calc . . H12B H 0.4334 0.5805 0.0951 0.044 Uiso 1 calc . . C13 C 0.1952(10) 0.7197(10) 0.1755(13) 0.055(7) Uiso 1 d . . H13A H 0.2097 0.7191 0.2285 0.067 Uiso 1 calc . . H13B H 0.1689 0.7550 0.1596 0.067 Uiso 1 calc . . C23 C 0.2148(10) 0.4058(10) 0.1882(12) 0.051(7) Uiso 1 d . . H23A H 0.2207 0.4186 0.2377 0.061 Uiso 1 calc . . H23B H 0.1962 0.3655 0.1807 0.061 Uiso 1 calc . . C111 C 0.4811(10) 0.6634(10) 0.2736(12) 0.046(6) Uiso 1 d . . C112 C 0.4656(10) 0.6543(10) 0.3325(13) 0.051(7) Uiso 1 d . . H112 H 0.4262 0.6455 0.3272 0.061 Uiso 1 calc . . C113 C 0.5115(14) 0.6585(13) 0.4037(16) 0.090(9) Uiso 1 d . . H113 H 0.5037 0.6493 0.4457 0.108 Uiso 1 calc . . C114 C 0.5685(14) 0.6770(13) 0.4076(17) 0.090(9) Uiso 1 d . . H114 H 0.5978 0.6850 0.4530 0.107 Uiso 1 calc . . C115 C 0.5812(12) 0.6832(12) 0.3482(16) 0.074(8) Uiso 1 d . . H115 H 0.6205 0.6917 0.3530 0.089 Uiso 1 calc . . C116 C 0.5388(11) 0.6777(10) 0.2793(14) 0.057(7) Uiso 1 d . . H116 H 0.5486 0.6835 0.2378 0.069 Uiso 1 calc . . C121 C 0.4310(9) 0.7141(9) 0.1260(12) 0.036(6) Uiso 1 d . . C122 C 0.4302(11) 0.7082(11) 0.0557(15) 0.068(8) Uiso 1 d . . H122 H 0.4309 0.6697 0.0352 0.082 Uiso 1 calc . . C123 C 0.4281(12) 0.7631(13) 0.0159(15) 0.079(8) Uiso 1 d . . H123 H 0.4276 0.7602 -0.0317 0.095 Uiso 1 calc . . C124 C 0.4268(11) 0.8209(12) 0.0450(15) 0.069(8) Uiso 1 d . . H124 H 0.4241 0.8563 0.0174 0.083 Uiso 1 calc . . C125 C 0.4296(11) 0.8238(12) 0.1155(15) 0.072(8) Uiso 1 d . . H125 H 0.4295 0.8620 0.1366 0.086 Uiso 1 calc . . C126 C 0.4327(11) 0.7706(12) 0.1571(14) 0.066(8) Uiso 1 d . . H126 H 0.4360 0.7737 0.2057 0.079 Uiso 1 calc . . C131 C 0.2995(10) 0.7959(10) 0.2065(13) 0.047(6) Uiso 1 d . . C132 C 0.3273(13) 0.7860(13) 0.2788(17) 0.087(9) Uiso 1 d . . H132 H 0.3279 0.7471 0.2987 0.105 Uiso 1 calc . . C133 C 0.3552(15) 0.8360(16) 0.3234(19) 0.111(11) Uiso 1 d . . H133 H 0.3702 0.8321 0.3741 0.133 Uiso 1 calc . . C134 C 0.3600(13) 0.8891(14) 0.2919(17) 0.085(9) Uiso 1 d . . H134 H 0.3820 0.9210 0.3209 0.102 Uiso 1 calc . . C135 C 0.3341(13) 0.8977(13) 0.2202(17) 0.082(9) Uiso 1 d . . H135 H 0.3375 0.9357 0.2003 0.098 Uiso 1 calc . . C136 C 0.3030(11) 0.8524(11) 0.1757(13) 0.059(7) Uiso 1 d . . H136 H 0.2845 0.8588 0.1256 0.071 Uiso 1 calc . . C141 C 0.2295(11) 0.7593(11) 0.0539(13) 0.059(7) Uiso 1 d . . C142 C 0.2570(13) 0.7373(13) 0.0088(17) 0.087(9) Uiso 1 d . . H142 H 0.2881 0.7092 0.0269 0.105 Uiso 1 calc . . C143 C 0.2392(19) 0.7566(18) -0.0654(23) 0.146(14) Uiso 1 d . . H143 H 0.2610 0.7476 -0.0949 0.175 Uiso 1 calc . . C144 C 0.1848(16) 0.7910(16) -0.0905(19) 0.115(12) Uiso 1 d . . H144 H 0.1664 0.7978 -0.1406 0.138 Uiso 1 calc . . C145 C 0.1589(14) 0.8141(14) -0.0456(18) 0.096(10) Uiso 1 d . . H145 H 0.1275 0.8419 -0.0631 0.115 Uiso 1 calc . . C146 C 0.1799(12) 0.7956(12) 0.0281(16) 0.077(8) Uiso 1 d . . H146 H 0.1602 0.8081 0.0589 0.093 Uiso 1 calc . . C211 C 0.4869(10) 0.5027(10) 0.2787(12) 0.049(6) Uiso 1 d . . C212 C 0.4634(12) 0.4886(12) 0.3337(16) 0.076(8) Uiso 1 d . . H212 H 0.4224 0.4838 0.3222 0.091 Uiso 1 calc . . C213 C 0.5025(13) 0.4821(12) 0.4041(16) 0.081(9) Uiso 1 d . . H213 H 0.4874 0.4681 0.4388 0.098 Uiso 1 calc . . C214 C 0.5608(12) 0.4947(11) 0.4263(14) 0.069(8) Uiso 1 d . . H214 H 0.5850 0.4939 0.4756 0.083 Uiso 1 calc . . C215 C 0.5839(13) 0.5090(12) 0.3729(17) 0.083(9) Uiso 1 d . . H215 H 0.6250 0.5145 0.3864 0.100 Uiso 1 calc . . C216 C 0.5483(10) 0.5153(10) 0.3012(14) 0.055(7) Uiso 1 d . . H216 H 0.5647 0.5280 0.2672 0.066 Uiso 1 calc . . C221 C 0.4579(9) 0.4484(9) 0.1366(12) 0.039(6) Uiso 1 d . . C222 C 0.4715(11) 0.3934(11) 0.1697(14) 0.063(7) Uiso 1 d . . H222 H 0.4750 0.3888 0.2182 0.076 Uiso 1 calc . . C223 C 0.4804(12) 0.3418(13) 0.1291(17) 0.084(9) Uiso 1 d . . H223 H 0.4870 0.3029 0.1504 0.101 Uiso 1 calc . . C224 C 0.4793(11) 0.3492(12) 0.0609(15) 0.068(8) Uiso 1 d . . H224 H 0.4862 0.3156 0.0356 0.081 Uiso 1 calc . . C225 C 0.4684(13) 0.4047(14) 0.0282(17) 0.091(9) Uiso 1 d . . H225 H 0.4679 0.4098 -0.0191 0.109 Uiso 1 calc . . C226 C 0.4575(12) 0.4553(12) 0.0676(16) 0.080(9) Uiso 1 d . . H226 H 0.4500 0.4938 0.0456 0.096 Uiso 1 calc . . C231 C 0.3332(9) 0.3629(10) 0.2628(12) 0.043(6) Uiso 1 d . . C232 C 0.3640(13) 0.3114(13) 0.2638(16) 0.083(9) Uiso 1 d . . H232 H 0.3618 0.2926 0.2202 0.100 Uiso 1 calc . . C233 C 0.4004(14) 0.2857(14) 0.3324(19) 0.101(10) Uiso 1 d . . H233 H 0.4220 0.2499 0.3331 0.122 Uiso 1 calc . . C234 C 0.4042(13) 0.3117(13) 0.3952(16) 0.084(9) Uiso 1 d . . H234 H 0.4284 0.2944 0.4393 0.101 Uiso 1 calc . . C235 C 0.3732(14) 0.3626(14) 0.3947(17) 0.095(10) Uiso 1 d . . H235 H 0.3761 0.3810 0.4388 0.114 Uiso 1 calc . . C236 C 0.3353(13) 0.3893(13) 0.3270(18) 0.090(9) Uiso 1 d . . H236 H 0.3126 0.4241 0.3267 0.108 Uiso 1 calc . . C241 C 0.2820(10) 0.3452(10) 0.1072(13) 0.057(7) Uiso 1 d . . C242 C 0.3130(11) 0.3555(12) 0.0603(15) 0.071(8) Uiso 1 d . . H242 H 0.3366 0.3904 0.0652 0.085 Uiso 1 calc . . C243 C 0.3078(13) 0.3128(14) 0.0064(16) 0.090(9) Uiso 1 d . . H243 H 0.3240 0.3204 -0.0293 0.108 Uiso 1 calc . . C244 C 0.2787(13) 0.2598(13) 0.0065(16) 0.082(9) Uiso 1 d . . H244 H 0.2787 0.2299 -0.0274 0.099 Uiso 1 calc . . C245 C 0.2510(14) 0.2476(14) 0.0499(18) 0.099(10) Uiso 1 d . . H245 H 0.2315 0.2102 0.0470 0.118 Uiso 1 calc . . C246 C 0.2505(11) 0.2908(12) 0.1007(15) 0.074(8) Uiso 1 d . . H246 H 0.2288 0.2836 0.1308 0.089 Uiso 1 calc . . C311 C 0.1064(10) 0.6485(11) 0.1982(13) 0.057(7) Uiso 1 d . . C312 C 0.1066(13) 0.6013(14) 0.2407(17) 0.088(9) Uiso 1 d . . H312 H 0.1309 0.5679 0.2412 0.105 Uiso 1 calc . . C313 C 0.0705(15) 0.5987(16) 0.2873(18) 0.110(11) Uiso 1 d . . H313 H 0.0722 0.5663 0.3190 0.132 Uiso 1 calc . . C314 C 0.0354(15) 0.6471(17) 0.2795(18) 0.103(11) Uiso 1 d . . H314 H 0.0086 0.6439 0.3037 0.124 Uiso 1 calc . . C315 C 0.0320(15) 0.6938(17) 0.2471(19) 0.112(11) Uiso 1 d . . H315 H 0.0077 0.7261 0.2502 0.134 Uiso 1 calc . . C316 C 0.0704(14) 0.6968(14) 0.2006(17) 0.095(10) Uiso 1 d . . H316 H 0.0696 0.7319 0.1732 0.115 Uiso 1 calc . . C321 C 0.1052(12) 0.6619(11) 0.0511(14) 0.064(8) Uiso 1 d . . C322 C 0.0542(18) 0.6976(18) 0.0295(22) 0.138(13) Uiso 1 d . . H322 H 0.0418 0.7126 0.0662 0.166 Uiso 1 calc . . C323 C 0.0168(17) 0.7143(17) -0.0480(22) 0.130(13) Uiso 1 d . . H323 H -0.0155 0.7413 -0.0621 0.156 Uiso 1 calc . . C324 C 0.0382(16) 0.6834(15) -0.0944(18) 0.104(11) Uiso 1 d . . H324 H 0.0153 0.6868 -0.1440 0.125 Uiso 1 calc . . C325 C 0.0855(18) 0.6504(17) -0.0787(22) 0.132(13) Uiso 1 d . . H325 H 0.0967 0.6332 -0.1152 0.159 Uiso 1 calc . . C326 C 0.1212(14) 0.6406(14) -0.0015(19) 0.095(10) Uiso 1 d . . H326 H 0.1567 0.6184 0.0107 0.114 Uiso 1 calc . . C331 C 0.0958(10) 0.4597(9) 0.1455(13) 0.044(6) Uiso 1 d . . C332 C 0.0919(11) 0.4328(12) 0.2047(14) 0.069(7) Uiso 1 d . . H332 H 0.1235 0.4098 0.2361 0.083 Uiso 1 calc . . C333 C 0.0376(14) 0.4404(13) 0.2186(16) 0.087(9) Uiso 1 d . . H333 H 0.0333 0.4219 0.2593 0.105 Uiso 1 calc . . C334 C -0.0064(14) 0.4736(14) 0.1736(18) 0.091(10) Uiso 1 d . . H334 H -0.0424 0.4758 0.1813 0.110 Uiso 1 calc . . C335 C -0.0008(13) 0.5053(13) 0.1153(17) 0.087(9) Uiso 1 d . . H335 H -0.0312 0.5309 0.0865 0.104 Uiso 1 calc . . C336 C 0.0504(11) 0.4981(11) 0.1012(14) 0.063(7) Uiso 1 d . . H336 H 0.0552 0.5187 0.0621 0.076 Uiso 1 calc . . C341 C 0.1449(10) 0.4270(11) 0.0351(13) 0.056(7) Uiso 1 d . . C342 C 0.1112(13) 0.3738(13) 0.0186(17) 0.090(9) Uiso 1 d . . H342 H 0.0962 0.3567 0.0520 0.108 Uiso 1 calc . . C343 C 0.1004(13) 0.3466(13) -0.0482(19) 0.093(10) Uiso 1 d . . H343 H 0.0800 0.3094 -0.0575 0.112 Uiso 1 calc . . C344 C 0.1170(15) 0.3699(16) -0.1000(19) 0.110(11) Uiso 1 d . . H344 H 0.1062 0.3510 -0.1455 0.132 Uiso 1 calc . . C345 C 0.1501(13) 0.4216(13) -0.0857(16) 0.086(9) Uiso 1 d . . H345 H 0.1636 0.4381 -0.1207 0.103 Uiso 1 calc . . C346 C 0.1645(12) 0.4518(12) -0.0148(16) 0.074(8) Uiso 1 d . . H346 H 0.1870 0.4877 -0.0044 0.089 Uiso 1 calc . . S3 S -0.1387(7) 0.7452(9) 0.2646(11) 0.148(7) Uani 0.67 d P . C3 C -0.2069(35) 0.7477(33) 0.2011(41) 0.190(28) Uiso 0.67 d P . H3A H -0.2230 0.7883 0.1991 0.285 Uiso 0.67 calc P . H3B H -0.2323 0.7188 0.2130 0.285 Uiso 0.67 calc P . H3C H -0.2049 0.7374 0.1544 0.285 Uiso 0.67 calc P . O7 O -0.1012(28) 0.7758(27) 0.2290(31) 0.232(25) Uiso 0.67 d P . O8 O -0.1414(13) 0.7766(14) 0.3212(17) 0.100(10) Uiso 0.67 d P . O9 O -0.1084(26) 0.6965(28) 0.2775(30) 0.226(23) Uiso 0.67 d P . S4 S 0.6423(12) 0.5974(13) 0.1950(14) 0.193(10) Uani 0.67 d PD . C4 C 0.6827(42) 0.5984(46) 0.1432(50) 0.275(44) Uiso 0.67 d PD . H4A H 0.6844 0.6395 0.1263 0.412 Uiso 0.67 calc P . H4B H 0.6649 0.5718 0.1019 0.412 Uiso 0.67 calc P . H4C H 0.7224 0.5843 0.1708 0.412 Uiso 0.67 calc P . O10 O 0.5898(18) 0.6185(17) 0.1585(20) 0.135(14) Uiso 0.67 d PD . O11 O 0.6485(35) 0.5418(26) 0.2057(43) 0.369(55) Uiso 0.67 d PD . O12 O 0.6682(29) 0.6311(29) 0.2563(33) 0.309(39) Uiso 0.67 d PD . S5 S 0.1115(15) 0.8864(10) 0.1973(19) 0.118(11) Uani 0.33 d PD . C5 C 0.1587(38) 0.8581(42) 0.2615(41) 0.171(51) Uiso 0.33 d PD . H5A H 0.1504 0.8151 0.2637 0.256 Uiso 0.33 calc P . H5B H 0.1593 0.8780 0.3055 0.256 Uiso 0.33 calc P . H5C H 0.1970 0.8630 0.2567 0.256 Uiso 0.33 calc P . O13 O 0.1116(18) 0.8506(19) 0.1442(22) 0.050(13) Uiso 0.33 d PD . O14 O 0.0633(28) 0.8742(34) 0.2142(43) 0.184(36) Uiso 0.33 d PD . O15 O 0.1245(45) 0.9392(26) 0.1977(53) 0.275(59) Uiso 0.33 d PD . S6 S 0.7807(20) 0.5712(22) 0.5400(43) 0.333(49) Uani 0.33 d PD . C6 C 0.8384(55) 0.5261(66) 0.5725(89) 0.229(71) Uiso 0.33 d PD . H6A H 0.8380 0.5069 0.6164 0.343 Uiso 0.33 calc P . H6B H 0.8744 0.5497 0.5834 0.343 Uiso 0.33 calc P . H6C H 0.8368 0.4952 0.5370 0.343 Uiso 0.33 calc P . O16 O 0.7989(47) 0.6124(66) 0.5962(54) 0.282(75) Uiso 0.33 d PD . O17 O 0.7178(28) 0.5673(37) 0.5162(40) 0.159(29) Uiso 0.33 d PD . O18 O 0.7963(43) 0.5880(53) 0.4837(46) 0.244(52) Uiso 0.33 d PD . 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 Hg1 0.0413(6) 0.0466(6) 0.0619(8) -0.0006(6) 0.0208(6) 0.0026(5) Hg2 0.0397(6) 0.0451(6) 0.0514(7) 0.0013(5) 0.0145(5) -0.0019(5) Hg3 0.0468(6) 0.0518(6) 0.0703(8) -0.0037(6) 0.0170(6) -0.0036(5) P12 0.038(4) 0.039(4) 0.047(4) 0.001(3) 0.012(3) -0.006(3) P13 0.045(4) 0.045(4) 0.055(5) -0.001(4) 0.014(4) 0.008(3) P21 0.041(4) 0.041(4) 0.043(4) 0.002(3) 0.017(3) 0.003(3) P23 0.042(4) 0.042(4) 0.054(5) 0.002(4) 0.014(4) -0.006(3) P31 0.035(4) 0.059(4) 0.054(5) -0.009(4) 0.012(4) 0.004(3) P32 0.038(4) 0.044(4) 0.050(5) 0.000(3) 0.012(4) -0.011(3) S1 0.072(5) 0.073(5) 0.057(5) 0.003(5) 0.028(4) 0.010(4) S2 0.149(10) 0.092(7) 0.045(5) 0.009(6) -0.005(6) 0.004(7) O1 0.200(24) 0.080(14) 0.073(15) 0.019(12) 0.059(15) 0.005(15) O2 0.084(17) 0.135(20) 0.260(32) 0.030(21) 0.059(19) 0.045(15) O3 0.093(15) 0.105(15) 0.085(15) 0.000(13) 0.026(12) -0.044(13) O4 0.271(40) 0.255(35) 0.325(47) 0.249(35) -0.249(36) -0.224(34) O5 0.105(15) 0.098(15) 0.052(13) 0.000(12) 0.031(12) -0.001(12) O6 0.112(26) 0.161(30) 0.703(103) -0.006(44) -0.053(41) 0.040(23) S3 0.102(12) 0.145(14) 0.177(17) -0.103(14) 0.027(12) 0.022(11) S4 0.212(26) 0.218(25) 0.217(26) -0.008(22) 0.160(24) 0.035(21) S5 0.162(28) 0.050(15) 0.183(33) 0.009(19) 0.112(27) 0.022(16) S6 0.153(39) 0.192(46) 0.703(139) 0.270(73) 0.214(68) 0.043(36) _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 Hg1 P13 2.526(6) . ? Hg1 P12 2.540(6) . ? Hg1 Hg3 2.7545(13) . ? Hg1 Hg2 2.7776(13) . ? Hg1 O1 2.94(2) . ? Hg1 O4 3.22(6) . ? Hg2 P23 2.521(6) . ? Hg2 P21 2.546(6) . ? Hg2 O5 2.63(2) . ? Hg2 Hg3 2.7994(13) . ? Hg2 O2 3.70(3) . ? Hg3 P32 2.495(6) . ? Hg3 P31 2.502(6) . ? Hg3 O3 2.64(2) . ? Hg3 O6 3.48(7) . ? P12 C12 1.81(2) . ? P12 C121 1.81(2) . ? P12 C111 1.86(2) . ? P13 C141 1.81(3) . ? P13 C13 1.83(2) . ? P13 C131 1.83(2) . ? P21 C221 1.80(2) . ? P21 C211 1.81(2) . ? P21 C12 1.82(2) . ? P23 C231 1.80(2) . ? P23 C241 1.81(2) . ? P23 C23 1.82(2) . ? P31 C321 1.75(3) . ? P31 C311 1.78(2) . ? P31 C13 1.80(2) . ? P32 C341 1.79(2) . ? P32 C23 1.82(2) . ? P32 C331 1.83(2) . ? S1 O2 1.41(2) . ? S1 O3 1.44(2) . ? S1 O1 1.44(2) . ? S1 C1 1.69(4) . ? S2 O4 1.26(3) . ? S2 O5 1.41(2) . ? S2 O6 1.62(4) . ? S2 C2 1.68(7) . ? C111 C112 1.35(3) . ? C111 C116 1.38(3) . ? C112 C113 1.43(3) . ? C113 C114 1.40(4) . ? C114 C115 1.31(3) . ? C115 C116 1.37(3) . ? C121 C126 1.36(3) . ? C121 C122 1.38(3) . ? C122 C123 1.42(3) . ? C123 C124 1.39(3) . ? C124 C125 1.36(3) . ? C125 C126 1.40(3) . ? C131 C132 1.35(3) . ? C131 C136 1.39(3) . ? C132 C133 1.40(4) . ? C133 C134 1.33(4) . ? C134 C135 1.33(3) . ? C135 C136 1.35(3) . ? C141 C146 1.36(3) . ? C141 C142 1.37(3) . ? C142 C143 1.42(4) . ? C143 C144 1.43(4) . ? C144 C145 1.34(4) . ? C145 C146 1.41(3) . ? C211 C216 1.40(3) . ? C211 C212 1.42(3) . ? C212 C213 1.37(3) . ? C213 C214 1.33(3) . ? C214 C215 1.38(3) . ? C215 C216 1.36(3) . ? C221 C222 1.34(3) . ? C221 C226 1.36(3) . ? C222 C223 1.43(3) . ? C223 C224 1.34(3) . ? C224 C225 1.35(3) . ? C225 C226 1.42(3) . ? C231 C232 1.34(3) . ? C231 C236 1.37(3) . ? C232 C233 1.43(4) . ? C233 C234 1.33(3) . ? C234 C235 1.33(3) . ? C235 C236 1.43(4) . ? C241 C246 1.38(3) . ? C241 C242 1.39(3) . ? C242 C243 1.38(3) . ? C243 C244 1.35(3) . ? C244 C245 1.28(3) . ? C245 C246 1.37(3) . ? C311 C312 1.32(3) . ? C311 C316 1.37(3) . ? C312 C313 1.47(4) . ? C313 C314 1.32(4) . ? C314 C315 1.19(4) . ? C315 C316 1.51(4) . ? C321 C326 1.31(3) . ? C321 C322 1.38(4) . ? C322 C323 1.50(4) . ? C323 C324 1.37(4) . ? C324 C325 1.28(4) . ? C325 C326 1.46(4) . ? C331 C332 1.33(3) . ? C331 C336 1.40(3) . ? C332 C333 1.43(3) . ? C333 C334 1.32(3) . ? C334 C335 1.38(4) . ? C335 C336 1.36(3) . ? C341 C346 1.34(3) . ? C341 C342 1.38(3) . ? C342 C343 1.37(4) . ? C343 C344 1.32(4) . ? C344 C345 1.35(4) . ? C345 C346 1.46(3) . ? S3 O9 1.26(6) . ? S3 O8 1.32(3) . ? S3 O7 1.48(6) . ? S3 C3 1.66(8) . ? S4 O11 1.23(5) . ? S4 O10 1.29(3) . ? S4 O12 1.35(5) . ? S4 C4 1.64(6) . ? S5 O15 1.19(5) . ? S5 O13 1.30(4) . ? S5 O14 1.34(5) . ? S5 C5 1.49(7) . ? S6 O18 1.34(6) . ? S6 O16 1.36(7) . ? S6 O17 1.41(6) . ? S6 C6 1.62(7) . ? 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 P13 Hg1 P12 111.6(2) . . ? P13 Hg1 Hg3 93.99(15) . . ? P12 Hg1 Hg3 154.23(14) . . ? P13 Hg1 Hg2 154.49(15) . . ? P12 Hg1 Hg2 93.46(13) . . ? Hg3 Hg1 Hg2 60.80(3) . . ? P13 Hg1 O1 79.8(4) . . ? P12 Hg1 O1 114.2(5) . . ? Hg3 Hg1 O1 72.1(4) . . ? Hg2 Hg1 O1 94.6(4) . . ? P13 Hg1 O4 106.5(6) . . ? P12 Hg1 O4 69.9(5) . . ? Hg3 Hg1 O4 100.7(4) . . ? Hg2 Hg1 O4 76.9(5) . . ? O1 Hg1 O4 171.0(6) . . ? P23 Hg2 P21 115.0(2) . . ? P23 Hg2 O5 100.7(4) . . ? P21 Hg2 O5 84.7(4) . . ? P23 Hg2 Hg1 150.34(15) . . ? P21 Hg2 Hg1 92.68(13) . . ? O5 Hg2 Hg1 91.8(4) . . ? P23 Hg2 Hg3 92.58(14) . . ? P21 Hg2 Hg3 151.86(13) . . ? O5 Hg2 Hg3 95.8(4) . . ? Hg1 Hg2 Hg3 59.19(3) . . ? P23 Hg2 O2 95.0(4) . . ? P21 Hg2 O2 91.4(4) . . ? O5 Hg2 O2 164.0(6) . . ? Hg1 Hg2 O2 72.8(4) . . ? Hg3 Hg2 O2 80.4(3) . . ? P32 Hg3 P31 114.9(2) . . ? P32 Hg3 O3 87.2(4) . . ? P31 Hg3 O3 99.6(5) . . ? P32 Hg3 Hg1 150.86(15) . . ? P31 Hg3 Hg1 93.86(15) . . ? O3 Hg3 Hg1 92.8(4) . . ? P32 Hg3 Hg2 91.34(15) . . ? P31 Hg3 Hg2 153.78(15) . . ? O3 Hg3 Hg2 81.0(4) . . ? Hg1 Hg3 Hg2 60.01(3) . . ? P32 Hg3 O6 99.5(6) . . ? P31 Hg3 O6 100.0(6) . . ? O3 Hg3 O6 154.1(7) . . ? Hg1 Hg3 O6 69.2(6) . . ? Hg2 Hg3 O6 74.0(5) . . ? C12 P12 C121 108.0(9) . . ? C12 P12 C111 105.0(10) . . ? C121 P12 C111 105.3(10) . . ? C12 P12 Hg1 108.7(7) . . ? C121 P12 Hg1 109.9(7) . . ? C111 P12 Hg1 119.4(8) . . ? C141 P13 C13 106.3(11) . . ? C141 P13 C131 108.6(11) . . ? C13 P13 C131 103.4(10) . . ? C141 P13 Hg1 114.4(8) . . ? C13 P13 Hg1 107.4(7) . . ? C131 P13 Hg1 115.7(7) . . ? C221 P21 C211 105.6(10) . . ? C221 P21 C12 107.6(10) . . ? C211 P21 C12 108.7(10) . . ? C221 P21 Hg2 111.4(7) . . ? C211 P21 Hg2 115.0(8) . . ? C12 P21 Hg2 108.4(7) . . ? C231 P23 C241 105.5(11) . . ? C231 P23 C23 103.4(10) . . ? C241 P23 C23 109.0(11) . . ? C231 P23 Hg2 112.0(7) . . ? C241 P23 Hg2 115.9(8) . . ? C23 P23 Hg2 110.3(7) . . ? C321 P31 C311 109.9(12) . . ? C321 P31 C13 109.2(11) . . ? C311 P31 C13 102.8(11) . . ? C321 P31 Hg3 106.8(9) . . ? C311 P31 Hg3 117.2(9) . . ? C13 P31 Hg3 110.7(8) . . ? C341 P32 C23 106.8(11) . . ? C341 P32 C331 106.5(11) . . ? C23 P32 C331 105.9(11) . . ? C341 P32 Hg3 117.6(8) . . ? C23 P32 Hg3 106.2(7) . . ? C331 P32 Hg3 113.1(7) . . ? O2 S1 O3 113.9(15) . . ? O2 S1 O1 112.6(15) . . ? O3 S1 O1 112.0(13) . . ? O2 S1 C1 104.2(18) . . ? O3 S1 C1 107.0(15) . . ? O1 S1 C1 106.4(15) . . ? O4 S2 O5 119.4(14) . . ? O4 S2 O6 103.7(30) . . ? O5 S2 O6 100.7(21) . . ? O4 S2 C2 123.8(30) . . ? O5 S2 C2 110.7(24) . . ? O6 S2 C2 89.9(29) . . ? S1 O1 Hg1 110.5(10) . . ? S1 O2 Hg2 89.1(13) . . ? S1 O3 Hg3 113.7(10) . . ? S2 O4 Hg1 106.7(27) . . ? S2 O5 Hg2 120.7(10) . . ? S2 O6 Hg3 113.1(25) . . ? P12 C12 P21 114.7(11) . . ? P31 C13 P13 118.0(13) . . ? P23 C23 P32 113.8(12) . . ? C112 C111 C116 122.7(22) . . ? C112 C111 P12 119.3(17) . . ? C116 C111 P12 117.8(18) . . ? C111 C112 C113 118.1(22) . . ? C114 C113 C112 117.6(26) . . ? C115 C114 C113 121.0(29) . . ? C114 C115 C116 122.6(27) . . ? C115 C116 C111 117.6(23) . . ? C126 C121 C122 121.2(22) . . ? C126 C121 P12 115.8(18) . . ? C122 C121 P12 122.9(17) . . ? C121 C122 C123 117.2(23) . . ? C124 C123 C122 122.6(25) . . ? C125 C124 C123 117.4(25) . . ? C124 C125 C126 121.7(25) . . ? C121 C126 C125 119.8(23) . . ? C132 C131 C136 121.0(23) . . ? C132 C131 P13 119.3(20) . . ? C136 C131 P13 119.7(18) . . ? C131 C132 C133 118.3(27) . . ? C134 C133 C132 119.0(31) . . ? C135 C134 C133 121.7(31) . . ? C134 C135 C136 121.3(28) . . ? C135 C136 C131 118.2(23) . . ? C146 C141 C142 121.5(25) . . ? C146 C141 P13 122.5(21) . . ? C142 C141 P13 115.9(20) . . ? C141 C142 C143 121.4(29) . . ? C142 C143 C144 114.1(34) . . ? C145 C144 C143 123.3(35) . . ? C144 C145 C146 119.2(30) . . ? C141 C146 C145 119.2(26) . . ? C216 C211 C212 117.5(22) . . ? C216 C211 P21 122.6(18) . . ? C212 C211 P21 119.7(18) . . ? C213 C212 C211 118.3(25) . . ? C214 C213 C212 124.4(28) . . ? C213 C214 C215 117.2(27) . . ? C216 C215 C214 122.0(26) . . ? C215 C216 C211 120.1(23) . . ? C222 C221 C226 119.5(22) . . ? C222 C221 P21 118.0(18) . . ? C226 C221 P21 122.5(18) . . ? C221 C222 C223 119.2(23) . . ? C224 C223 C222 120.4(26) . . ? C223 C224 C225 120.9(27) . . ? C224 C225 C226 118.6(27) . . ? C221 C226 C225 121.3(25) . . ? C232 C231 C236 120.1(24) . . ? C232 C231 P23 122.4(20) . . ? C236 C231 P23 117.5(19) . . ? C231 C232 C233 119.2(26) . . ? C234 C233 C232 121.4(29) . . ? C233 C234 C235 119.8(30) . . ? C234 C235 C236 120.5(30) . . ? C231 C236 C235 118.9(26) . . ? C246 C241 C242 118.7(24) . . ? C246 C241 P23 121.1(20) . . ? C242 C241 P23 120.2(19) . . ? C243 C242 C241 118.3(25) . . ? C244 C243 C242 118.7(28) . . ? C245 C244 C243 124.7(31) . . ? C244 C245 C246 118.8(30) . . ? C245 C246 C241 120.4(26) . . ? C312 C311 C316 115.7(26) . . ? C312 C311 P31 123.2(21) . . ? C316 C311 P31 121.0(21) . . ? C311 C312 C313 123.6(28) . . ? C314 C313 C312 112.9(31) . . ? C315 C314 C313 131.6(38) . . ? C314 C315 C316 114.9(34) . . ? C311 C316 C315 120.9(28) . . ? C326 C321 C322 115.9(30) . . ? C326 C321 P31 120.7(23) . . ? C322 C321 P31 123.0(26) . . ? C321 C322 C323 125.8(34) . . ? C324 C323 C322 108.8(33) . . ? C325 C324 C323 128.6(37) . . ? C324 C325 C326 118.0(36) . . ? C321 C326 C325 122.4(31) . . ? C332 C331 C336 121.2(22) . . ? C332 C331 P32 123.2(18) . . ? C336 C331 P32 114.9(18) . . ? C331 C332 C333 118.0(24) . . ? C334 C333 C332 119.8(28) . . ? C333 C334 C335 122.3(30) . . ? C336 C335 C334 118.3(27) . . ? C335 C336 C331 120.0(24) . . ? C346 C341 C342 119.7(25) . . ? C346 C341 P32 121.3(20) . . ? C342 C341 P32 118.9(21) . . ? C343 C342 C341 118.4(27) . . ? C344 C343 C342 124.3(30) . . ? C343 C344 C345 118.6(32) . . ? C344 C345 C346 119.6(28) . . ? C341 C346 C345 119.3(24) . . ? O9 S3 O8 117.8(35) . . ? O9 S3 O7 93.9(35) . . ? O8 S3 O7 112.5(29) . . ? O9 S3 C3 121.3(39) . . ? O8 S3 C3 106.2(30) . . ? O7 S3 C3 103.4(39) . . ? O11 S4 O10 118.6(38) . . ? O11 S4 O12 113.2(34) . . ? O10 S4 O12 110.2(30) . . ? O11 S4 C4 93.3(57) . . ? O10 S4 C4 109.2(47) . . ? O12 S4 C4 111.1(57) . . ? O15 S5 O13 120.5(41) . . ? O15 S5 O14 115.9(36) . . ? O13 S5 O14 109.4(36) . . ? O15 S5 C5 106.0(42) . . ? O13 S5 C5 102.1(33) . . ? O14 S5 C5 99.7(37) . . ? O18 S6 O16 112.5(50) . . ? O18 S6 O17 109.1(51) . . ? O16 S6 O17 107.4(49) . . ? O18 S6 C6 92.2(84) . . ? O16 S6 C6 95.8(100) . . ? O17 S6 C6 138.6(77) . . ? _refine_diff_density_max 1.032 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.145 #============================================================================