Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author ; Paul Peringer Institut fur Allgemeine, Anorganische und Theoretische Chemie Universitat Innsbruck Innrain 52a A-6020 Innsbruck Austria ; _publ_contact_author_phone '043 512 5075112' _publ_contact_author_fax ? _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 ; [triangulo-Hg3(mu-dppm)3](O3SCF3)4: First complete NMR analysis of a homoleptic [M3(mu-dppm)3] type system and study of the conformation dynamics in solution by use of its dpam/mdppm derivatives ; loop_ _publ_author_name _publ_author_address 'Schuh, Walter' ; Institut fur Allgemeine und Anorganische Chemie Universitat Innsbruck Innrain 52a A-6020 Innsbruck Austria ; 'Hagele, Gerhard' ; Institut fur Anorganische und Strukturchemie Universitat Dusseldorf Universitatsstr. 1 D-40225 Dusseldorf Germany ; 'Olschner, Ralf' ; Institut fur Anorganische und Strukturchemie Universitat Dusseldorf Universitatsstr. 1 D-40225 Dusseldorf Germany ; 'Lindner, Andreas' ; Institut fur Anorganische und Strukturchemie Universitat Dusseldorf Universitatsstr. 1 D-40225 Dusseldorf Germany ; 'Dvortsak, Peter' ; Bruker Analytik GmbH Silberstreifen D-76287 Rheinstatten Germany ; 'Kopacka, Holger' ; Institut fur Allgemeine und Anorganische Chemie Universitat Innsbruck Innrain 52a A-6020 Innsbruck Austria ; 'Wurst,Klaus' ; Institut fur Allgemeine und Anorganische Chemie Universitat Innsbruck Innrain 52a A-6020 Innsbruck Austria ; 'Peringer, Paul' ; Institut fur Allgemeine und Anorganische Chemie Universitat Innsbruck Innrain 52a A-6020 Innsbruck Austria ; #============================================================================ data_4x4CHCl3 _database_code_CSD 154492 _audit_creation_method SHELXL _chemical_name_systematic ; [Hg3(dppa)3](O3SCF3)4 x 4CHCl3 ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C80 H67 Cl12 F12 Hg3 N3 O12 P6 S4' _chemical_formula_weight 2831.60 _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' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.809(4) _cell_length_b 21.900(9) _cell_length_c 25.080(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.81(2) _cell_angle_gamma 90.00 _cell_volume 10277.8(56) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 5.3 _cell_measurement_theta_max 12.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method ? _exptl_crystal_F_000 5480 _exptl_absorpt_coefficient_mu 5.034 _exptl_absorpt_correction_type PSI-scan _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_T_max 0.832 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 9668 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 19.99 _reflns_number_total 8684 _reflns_number_observed 6793 _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 506 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^)+(0.0363P)^2^+14.3660P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'mixed, refined at N12, N13 and N23' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8178 _refine_ls_number_parameters 1229 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_all 0.0865 _refine_ls_wR_factor_obs 0.0752 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_goodness_of_fit_obs 1.101 _refine_ls_restrained_S_all 1.096 _refine_ls_restrained_S_obs 1.101 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group H12N H 0.7407(12) 0.5101(38) 0.2123(34) 0.014(28) Uiso 1 d D . H13N H 0.3629(55) 0.3257(43) 0.1539(34) 0.061(46) Uiso 1 d D . H23N H 0.3630(49) 0.6334(40) 0.3364(44) 0.064(47) Uiso 1 d D . Hg1 Hg 0.53179(2) 0.44230(2) 0.20205(2) 0.02460(14) Uani 1 d . . Hg2 Hg 0.53673(2) 0.55050(2) 0.26354(2) 0.02454(14) Uani 1 d . . Hg3 Hg 0.42032(2) 0.47080(2) 0.26296(2) 0.02505(15) Uani 1 d . . P12 P 0.65306(14) 0.46179(13) 0.17246(12) 0.0258(8) Uani 1 d . . P13 P 0.47124(15) 0.34508(13) 0.17012(12) 0.0284(8) Uani 1 d . . P21 P 0.66264(14) 0.57269(13) 0.24337(12) 0.0251(8) Uani 1 d . . P23 P 0.47368(14) 0.62967(13) 0.31561(12) 0.0265(8) Uani 1 d . . P31 P 0.34227(14) 0.38459(13) 0.22437(12) 0.0266(8) Uani 1 d . . P32 P 0.36118(14) 0.53562(13) 0.32817(12) 0.0269(8) Uani 1 d . . S1 S 0.58098(15) 0.41400(14) 0.33863(12) 0.0329(8) Uani 1 d . . S2 S 0.4163(2) 0.5600(2) 0.14513(14) 0.0476(9) Uani 1 d . . S3 S 0.9072(2) 0.49487(14) 0.21093(13) 0.0384(8) Uani 1 d . . S4 S 0.2515(2) 0.2139(2) 0.10245(14) 0.0515(10) Uani 1 d . . O1 O 0.6241(4) 0.4112(3) 0.2945(3) 0.037(2) Uani 1 d . . O2 O 0.5793(4) 0.4734(3) 0.3639(3) 0.044(2) Uani 1 d . . O3 O 0.5124(4) 0.3841(3) 0.3292(3) 0.043(2) Uani 1 d . . O4 O 0.4255(4) 0.5015(4) 0.1202(3) 0.049(2) Uani 1 d . . O5 O 0.4814(4) 0.5933(4) 0.1576(4) 0.068(3) Uani 1 d . . O6 O 0.3701(4) 0.5588(4) 0.1884(4) 0.058(2) Uani 1 d . . O7 O 0.9023(5) 0.4358(4) 0.1861(3) 0.061(3) Uani 1 d . . O8 O 0.9676(4) 0.5318(4) 0.2010(3) 0.049(2) Uani 1 d . . O9 O 0.8412(4) 0.5291(4) 0.2082(3) 0.054(2) Uani 1 d . . O10 O 0.3019(5) 0.2553(4) 0.1264(4) 0.087(3) Uani 1 d . . O11 O 0.2812(7) 0.1618(5) 0.0786(5) 0.133(5) Uani 1 d . . O12 O 0.1944(4) 0.1987(4) 0.1330(4) 0.070(3) Uani 1 d . . F1 F 0.5961(5) 0.3607(4) 0.4320(3) 0.089(3) Uani 1 d . . F2 F 0.6401(5) 0.3103(4) 0.3693(3) 0.088(3) Uani 1 d . . F3 F 0.6953(4) 0.3893(4) 0.4030(3) 0.079(3) Uani 1 d . . F4 F 0.3536(6) 0.6621(5) 0.1128(5) 0.147(5) Uani 1 d . . F5 F 0.3011(5) 0.5804(4) 0.0806(4) 0.109(4) Uani 1 d . . F6 F 0.3955(6) 0.6096(5) 0.0508(4) 0.134(5) Uani 1 d . . F7 F 0.9302(4) 0.5274(4) 0.3113(3) 0.072(2) Uani 1 d . . F8 F 0.8712(4) 0.4454(4) 0.2993(3) 0.074(2) Uani 1 d . . F9 F 0.9830(4) 0.4458(3) 0.2932(3) 0.075(2) Uani 1 d . . F10 F 0.1603(6) 0.2255(7) 0.0194(4) 0.178(7) Uani 1 d . . F11 F 0.1799(11) 0.3051(7) 0.0633(7) 0.235(10) Uani 1 d . . F12 F 0.2541(7) 0.2714(8) 0.0134(5) 0.197(8) Uani 1 d . . C1 C 0.6318(8) 0.3647(6) 0.3881(6) 0.055(4) Uani 1 d . . C2 C 0.3645(11) 0.6064(9) 0.0949(8) 0.097(6) Uani 1 d . . C3 C 0.9243(7) 0.4780(6) 0.2809(5) 0.045(3) Uani 1 d . . C4 C 0.2083(11) 0.2566(11) 0.0475(8) 0.103(7) Uani 1 d . . C5 C 0.9859(8) 0.6439(7) 0.1183(8) 0.098(6) Uani 1 d . . H5 H 0.9787 0.6218 0.1517 0.118 Uiso 1 calc . . C6 C 0.8913(8) 0.4028(6) 0.0640(6) 0.073(5) Uani 1 d . . H6 H 0.8692 0.4073 0.0980 0.088 Uiso 1 calc . . C7 C 0.1806(12) 0.3387(13) 0.4403(11) 0.196(12) Uani 1 d . . H7 H 0.1923 0.3290 0.4037 0.235 Uiso 1 calc . . Cl1 Cl 0.9080(3) 0.6408(3) 0.0766(3) 0.187(3) Uani 1 d . . Cl2 Cl 1.0560(3) 0.6111(3) 0.0905(2) 0.142(2) Uani 1 d . . Cl3 Cl 1.0053(3) 0.7204(3) 0.1342(3) 0.155(2) Uani 1 d . . Cl4 Cl 0.9599(3) 0.3498(2) 0.0742(2) 0.118(2) Uani 1 d . . Cl5 Cl 0.8257(2) 0.3795(2) 0.0151(2) 0.103(2) Uani 1 d . . Cl6 Cl 0.9256(2) 0.4739(2) 0.0477(2) 0.105(2) Uani 1 d . . Cl7 Cl 0.0982(4) 0.3517(4) 0.4334(3) 0.223(4) Uani 1 d . . Cl8 Cl 0.2352(3) 0.3997(3) 0.4598(2) 0.143(2) Uani 1 d . . Cl9 Cl 0.2069(3) 0.2738(3) 0.4778(2) 0.140(2) Uani 1 d . . N12 N 0.6963(4) 0.5111(4) 0.2159(4) 0.024(2) Uani 1 d D . N13 N 0.3830(4) 0.3494(4) 0.1777(4) 0.031(2) Uani 1 d D . N23 N 0.3900(5) 0.6080(4) 0.3226(4) 0.028(2) Uani 1 d D . C101 C 0.7120(6) 0.3950(5) 0.1775(5) 0.032(3) Uani 1 d . . C102 C 0.7454(6) 0.3774(5) 0.2263(5) 0.036(3) Uani 1 d . . H102 H 0.7399 0.4000 0.2575 0.043 Uiso 1 calc . . C103 C 0.7881(7) 0.3248(7) 0.2283(6) 0.057(4) Uani 1 d . . H103 H 0.8107 0.3112 0.2613 0.069 Uiso 1 calc . . C104 C 0.7970(7) 0.2935(6) 0.1825(8) 0.058(4) Uani 1 d . . H104 H 0.8273 0.2593 0.1844 0.069 Uiso 1 calc . . C105 C 0.7637(8) 0.3102(6) 0.1348(7) 0.072(5) Uani 1 d . . H105 H 0.7700 0.2868 0.1041 0.087 Uiso 1 calc . . C106 C 0.7193(7) 0.3624(6) 0.1302(5) 0.046(3) Uani 1 d . . H106 H 0.6959 0.3747 0.0970 0.056 Uiso 1 calc . . C107 C 0.6563(6) 0.4912(5) 0.1056(4) 0.027(3) Uani 1 d . . C108 C 0.5969(6) 0.4916(7) 0.0709(5) 0.062(4) Uani 1 d . . H108 H 0.5532 0.4777 0.0815 0.074 Uiso 1 calc . . C109 C 0.6013(8) 0.5127(9) 0.0194(7) 0.100(6) Uani 1 d . . H109 H 0.5596 0.5150 -0.0046 0.120 Uiso 1 calc . . C110 C 0.6661(9) 0.5304(8) 0.0027(6) 0.077(5) Uani 1 d . . H110 H 0.6687 0.5430 -0.0328 0.093 Uiso 1 calc . . C111 C 0.7253(7) 0.5295(6) 0.0376(6) 0.054(4) Uani 1 d . . H111 H 0.7692 0.5425 0.0267 0.065 Uiso 1 calc . . C112 C 0.7213(6) 0.5093(5) 0.0898(5) 0.040(3) Uani 1 d . . H112 H 0.7627 0.5080 0.1142 0.048 Uiso 1 calc . . C113 C 0.5102(6) 0.2789(5) 0.2029(4) 0.029(3) Uani 1 d . . C114 C 0.5761(6) 0.2814(5) 0.2324(5) 0.030(3) Uani 1 d . . H114 H 0.5990 0.3195 0.2374 0.036 Uiso 1 calc . . C115 C 0.6089(7) 0.2312(7) 0.2542(5) 0.052(4) Uani 1 d . . H115 H 0.6535 0.2348 0.2745 0.062 Uiso 1 calc . . C116 C 0.5778(8) 0.1752(6) 0.2470(6) 0.061(4) Uani 1 d . . H116 H 0.6011 0.1403 0.2619 0.074 Uiso 1 calc . . C117 C 0.5116(9) 0.1702(6) 0.2175(7) 0.082(5) Uani 1 d . . H117 H 0.4896 0.1318 0.2126 0.099 Uiso 1 calc . . C118 C 0.4787(6) 0.2211(6) 0.1955(6) 0.061(4) Uani 1 d . . H118 H 0.4341 0.2174 0.1751 0.074 Uiso 1 calc . . C119 C 0.4741(6) 0.3296(5) 0.0992(5) 0.035(3) Uani 1 d . . C120 C 0.4181(7) 0.3408(7) 0.0622(6) 0.071(5) Uani 1 d . . H120 H 0.3753 0.3570 0.0726 0.085 Uiso 1 calc . . C121 C 0.4245(9) 0.3281(9) 0.0087(6) 0.094(6) Uani 1 d . . H121 H 0.3848 0.3353 -0.0163 0.113 Uiso 1 calc . . C122 C 0.4845(12) 0.3060(10) -0.0096(7) 0.104(7) Uani 1 d . . H122 H 0.4876 0.2979 -0.0461 0.125 Uiso 1 calc . . C123 C 0.5408(10) 0.2961(10) 0.0290(9) 0.127(8) Uani 1 d . . H123 H 0.5837 0.2800 0.0187 0.152 Uiso 1 calc . . C124 C 0.5360(7) 0.3089(8) 0.0820(6) 0.079(5) Uani 1 d . . H124 H 0.5763 0.3034 0.1070 0.095 Uiso 1 calc . . C201 C 0.7258(5) 0.5853(5) 0.3006(4) 0.027(3) Uani 1 d . . C202 C 0.7357(6) 0.5376(5) 0.3388(5) 0.046(4) Uani 1 d . . H202 H 0.7110 0.5005 0.3334 0.055 Uiso 1 calc . . C203 C 0.7836(7) 0.5474(7) 0.3850(5) 0.059(4) Uani 1 d . . H203 H 0.7914 0.5161 0.4105 0.071 Uiso 1 calc . . C204 C 0.8188(7) 0.6016(8) 0.3933(6) 0.061(4) Uani 1 d . . H204 H 0.8502 0.6074 0.4245 0.073 Uiso 1 calc . . C205 C 0.8087(7) 0.6471(6) 0.3567(6) 0.049(4) Uani 1 d . . H205 H 0.8336 0.6841 0.3625 0.059 Uiso 1 calc . . C206 C 0.7620(6) 0.6396(6) 0.3109(5) 0.043(3) Uani 1 d . . H206 H 0.7548 0.6720 0.2864 0.052 Uiso 1 calc . . C207 C 0.6686(6) 0.6378(5) 0.1985(4) 0.026(3) Uani 1 d . . C208 C 0.7274(6) 0.6444(5) 0.1696(5) 0.037(3) Uani 1 d . . H208 H 0.7649 0.6159 0.1736 0.044 Uiso 1 calc . . C209 C 0.7302(7) 0.6929(6) 0.1352(5) 0.047(4) Uani 1 d . . H209 H 0.7702 0.6977 0.1161 0.056 Uiso 1 calc . . C210 C 0.6755(8) 0.7342(5) 0.1284(5) 0.048(4) Uani 1 d . . H210 H 0.6776 0.7668 0.1042 0.058 Uiso 1 calc . . C211 C 0.6167(7) 0.7275(6) 0.1575(5) 0.048(4) Uani 1 d . . H211 H 0.5796 0.7564 0.1537 0.058 Uiso 1 calc . . C212 C 0.6124(6) 0.6787(5) 0.1921(5) 0.035(3) Uani 1 d . . H212 H 0.5720 0.6734 0.2109 0.042 Uiso 1 calc . . C213 C 0.5188(6) 0.6488(4) 0.3803(5) 0.029(3) Uani 1 d . . C214 C 0.4828(6) 0.6739(5) 0.4197(5) 0.042(3) Uani 1 d . . H214 H 0.4326 0.6752 0.4151 0.050 Uiso 1 calc . . C215 C 0.5186(8) 0.6973(6) 0.4660(5) 0.050(4) Uani 1 d . . H215 H 0.4933 0.7153 0.4924 0.060 Uiso 1 calc . . C216 C 0.5935(8) 0.6937(6) 0.4730(5) 0.052(4) Uani 1 d . . H216 H 0.6184 0.7091 0.5045 0.062 Uiso 1 calc . . C217 C 0.6301(6) 0.6685(6) 0.4349(6) 0.053(4) Uani 1 d . . H217 H 0.6803 0.6671 0.4397 0.064 Uiso 1 calc . . C218 C 0.5940(6) 0.6446(5) 0.3888(5) 0.044(3) Uani 1 d . . H218 H 0.6195 0.6255 0.3631 0.053 Uiso 1 calc . . C219 C 0.4631(5) 0.7017(5) 0.2816(5) 0.028(3) Uani 1 d . . C220 C 0.5050(6) 0.7527(6) 0.2974(5) 0.043(3) Uani 1 d . . H220 H 0.5377 0.7506 0.3283 0.051 Uiso 1 calc . . C221 C 0.4985(7) 0.8058(5) 0.2678(6) 0.044(4) Uani 1 d . . H221 H 0.5264 0.8400 0.2790 0.053 Uiso 1 calc . . C222 C 0.4523(8) 0.8094(6) 0.2230(6) 0.060(4) Uani 1 d . . H222 H 0.4488 0.8456 0.2029 0.073 Uiso 1 calc . . C223 C 0.4103(8) 0.7597(7) 0.2068(6) 0.077(5) Uani 1 d . . H223 H 0.3777 0.7624 0.1759 0.092 Uiso 1 calc . . C224 C 0.4160(7) 0.7060(6) 0.2359(6) 0.058(4) Uani 1 d . . H224 H 0.3876 0.6723 0.2244 0.069 Uiso 1 calc . . C301 C 0.3237(5) 0.3301(5) 0.2756(5) 0.025(3) Uani 1 d . . C302 C 0.3409(7) 0.3430(6) 0.3275(6) 0.068(4) Uani 1 d . . H302 H 0.3616 0.3809 0.3374 0.082 Uiso 1 calc . . C303 C 0.3282(10) 0.3005(10) 0.3670(6) 0.109(7) Uani 1 d . . H303 H 0.3410 0.3103 0.4032 0.131 Uiso 1 calc . . C304 C 0.2989(8) 0.2475(8) 0.3548(7) 0.068(5) Uani 1 d . . H304 H 0.2896 0.2199 0.3819 0.082 Uiso 1 calc . . C305 C 0.2817(9) 0.2328(6) 0.3015(8) 0.080(5) Uani 1 d . . H305 H 0.2616 0.1945 0.2924 0.096 Uiso 1 calc . . C306 C 0.2937(8) 0.2737(7) 0.2616(6) 0.070(5) Uani 1 d . . H306 H 0.2818 0.2635 0.2254 0.083 Uiso 1 calc . . C307 C 0.2592(5) 0.4077(5) 0.1903(5) 0.030(3) Uani 1 d . . C308 C 0.2580(6) 0.4414(6) 0.1437(6) 0.054(4) Uani 1 d . . H308 H 0.3015 0.4507 0.1301 0.065 Uiso 1 calc . . C309 C 0.1948(8) 0.4621(6) 0.1163(6) 0.067(4) Uani 1 d . . H309 H 0.1956 0.4868 0.0857 0.080 Uiso 1 calc . . C310 C 0.1310(7) 0.4459(7) 0.1348(8) 0.086(6) Uani 1 d . . H310 H 0.0877 0.4570 0.1153 0.103 Uiso 1 calc . . C311 C 0.1304(7) 0.4146(9) 0.1802(8) 0.109(7) Uani 1 d . . H311 H 0.0869 0.4059 0.1939 0.131 Uiso 1 calc . . C312 C 0.1933(7) 0.3951(7) 0.2068(6) 0.080(5) Uani 1 d . . H312 H 0.1914 0.3718 0.2381 0.096 Uiso 1 calc . . C313 C 0.3709(5) 0.5135(5) 0.3975(4) 0.026(3) Uani 1 d . . C314 C 0.4218(6) 0.4693(5) 0.4146(5) 0.036(3) Uani 1 d . . H314 H 0.4488 0.4496 0.3901 0.044 Uiso 1 calc . . C315 C 0.4313(7) 0.4554(6) 0.4694(7) 0.062(4) Uani 1 d . . H315 H 0.4661 0.4264 0.4813 0.074 Uiso 1 calc . . C316 C 0.3924(10) 0.4819(8) 0.5065(6) 0.076(5) Uani 1 d . . H316 H 0.3982 0.4699 0.5426 0.091 Uiso 1 calc . . C317 C 0.3452(10) 0.5261(8) 0.4892(7) 0.079(5) Uani 1 d . . H317 H 0.3198 0.5465 0.5142 0.094 Uiso 1 calc . . C318 C 0.3336(7) 0.5421(5) 0.4358(6) 0.054(4) Uani 1 d . . H318 H 0.3000 0.5727 0.4250 0.065 Uiso 1 calc . . C319 C 0.2664(6) 0.5399(5) 0.3074(5) 0.037(3) Uani 1 d . . C320 C 0.2427(7) 0.5740(6) 0.2651(7) 0.071(5) Uani 1 d . . H320 H 0.2742 0.5987 0.2480 0.085 Uiso 1 calc . . C321 C 0.1694(8) 0.5720(8) 0.2468(7) 0.097(6) Uani 1 d . . H321 H 0.1522 0.5943 0.2161 0.116 Uiso 1 calc . . C322 C 0.1243(7) 0.5389(8) 0.2725(9) 0.094(6) Uani 1 d . . H322 H 0.0756 0.5380 0.2596 0.113 Uiso 1 calc . . C323 C 0.1475(9) 0.5057(9) 0.3180(9) 0.114(7) Uani 1 d . . H323 H 0.1154 0.4835 0.3369 0.136 Uiso 1 calc . . C324 C 0.2186(7) 0.5065(7) 0.3343(6) 0.074(5) Uani 1 d . . H324 H 0.2359 0.4838 0.3647 0.089 Uiso 1 calc . . C8 C -0.0935(10) 0.3976(9) 0.5285(10) 0.126(8) Uani 1 d . 1 H8 H -0.1295 0.3705 0.5424 0.151 Uiso 1 calc . 1 Cl10 Cl -0.0200(7) 0.3886(13) 0.5644(6) 0.224(12) Uani 0.63(2) d P 1 Cl11 Cl -0.1282(8) 0.4707(5) 0.5238(5) 0.169(7) Uani 0.63(2) d P 1 Cl12 Cl -0.0874(8) 0.3782(7) 0.4570(6) 0.187(7) Uani 0.63(2) d P 1 Cl1A Cl -0.0412(20) 0.4585(15) 0.5565(17) 0.298(24) Uani 0.37(2) d P 2 Cl2A Cl -0.1210(17) 0.4155(21) 0.4743(14) 0.299(21) Uani 0.37(2) d P 2 Cl3A Cl -0.0408(18) 0.3346(13) 0.5347(16) 0.220(18) Uani 0.37(2) d P 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0203(2) 0.0246(3) 0.0289(3) -0.0007(2) 0.0019(2) -0.0035(2) Hg2 0.0196(2) 0.0229(3) 0.0310(3) -0.0005(2) 0.0019(2) -0.0017(2) Hg3 0.0219(2) 0.0231(3) 0.0301(3) -0.0007(2) 0.0025(2) -0.0026(2) P12 0.023(2) 0.029(2) 0.027(2) -0.0012(15) 0.0060(14) -0.0011(14) P13 0.025(2) 0.026(2) 0.034(2) -0.005(2) 0.006(2) -0.0083(14) P21 0.020(2) 0.026(2) 0.029(2) -0.003(2) 0.0016(14) -0.0080(14) P23 0.022(2) 0.024(2) 0.033(2) -0.003(2) 0.0024(15) 0.0021(14) P31 0.020(2) 0.029(2) 0.030(2) -0.001(2) 0.0015(15) -0.0047(14) P32 0.022(2) 0.023(2) 0.037(2) -0.002(2) 0.0052(15) 0.0002(14) S1 0.032(2) 0.036(2) 0.030(2) 0.005(2) -0.001(2) 0.003(2) S2 0.047(2) 0.043(2) 0.048(3) 0.015(2) -0.016(2) -0.005(2) S3 0.025(2) 0.036(2) 0.053(2) -0.002(2) 0.000(2) -0.001(2) S4 0.052(2) 0.050(2) 0.053(3) -0.009(2) 0.008(2) -0.028(2) O1 0.032(4) 0.049(5) 0.029(5) 0.004(4) 0.001(4) 0.005(4) O2 0.051(5) 0.035(5) 0.045(6) -0.013(4) 0.008(4) -0.001(4) O3 0.037(5) 0.037(5) 0.054(6) 0.002(4) 0.001(4) -0.008(4) O4 0.053(5) 0.055(6) 0.037(5) 0.009(5) -0.011(4) -0.008(5) O5 0.062(6) 0.062(6) 0.074(7) 0.023(5) -0.026(5) -0.028(5) O6 0.058(6) 0.055(6) 0.060(7) 0.014(5) -0.001(5) 0.015(5) O7 0.089(7) 0.040(6) 0.052(6) -0.014(5) -0.004(5) -0.004(5) O8 0.025(5) 0.063(6) 0.060(6) 0.007(5) 0.004(4) -0.009(4) O9 0.019(5) 0.056(6) 0.086(7) 0.010(5) 0.001(4) -0.002(4) O10 0.113(8) 0.093(8) 0.052(7) -0.007(6) -0.006(6) -0.077(7) O11 0.140(11) 0.104(10) 0.165(13) -0.054(9) 0.063(10) 0.007(8) O12 0.054(6) 0.083(7) 0.074(7) 0.027(6) 0.011(5) -0.021(5) F1 0.119(7) 0.098(7) 0.051(6) 0.028(5) 0.006(6) 0.007(6) F2 0.125(8) 0.045(6) 0.087(7) 0.011(5) -0.028(6) 0.039(5) F3 0.066(6) 0.093(6) 0.072(6) -0.011(5) -0.031(5) 0.019(5) F4 0.204(12) 0.058(7) 0.155(11) 0.008(7) -0.100(9) 0.030(7) F5 0.103(7) 0.107(7) 0.101(8) 0.032(6) -0.067(6) -0.007(6) F6 0.180(11) 0.146(10) 0.069(8) 0.067(8) -0.022(8) -0.023(8) F7 0.089(6) 0.063(5) 0.062(6) -0.025(5) -0.002(5) 0.000(5) F8 0.068(5) 0.088(6) 0.067(6) 0.009(5) 0.012(5) -0.022(5) F9 0.049(5) 0.074(6) 0.098(7) 0.008(5) -0.014(4) 0.025(4) F10 0.126(9) 0.331(19) 0.066(8) 0.043(9) -0.037(7) -0.127(12) F11 0.348(25) 0.131(12) 0.208(18) 0.061(12) -0.069(17) 0.092(14) F12 0.168(12) 0.331(20) 0.086(9) 0.084(11) -0.016(8) -0.141(13) C1 0.082(12) 0.035(10) 0.045(11) 0.005(8) -0.007(9) 0.014(9) C2 0.120(17) 0.098(17) 0.063(15) 0.015(13) -0.032(13) -0.016(13) C3 0.042(9) 0.039(9) 0.056(10) -0.001(8) 0.008(8) -0.003(8) C4 0.100(15) 0.136(19) 0.069(15) 0.034(14) -0.012(13) -0.070(15) C5 0.073(11) 0.075(12) 0.154(18) 0.029(12) 0.046(12) 0.017(10) C6 0.090(11) 0.048(10) 0.080(12) -0.003(8) 0.004(9) -0.005(9) C7 0.116(20) 0.236(31) 0.217(29) 0.004(25) -0.075(19) -0.027(20) Cl1 0.130(5) 0.155(6) 0.261(9) 0.005(6) -0.047(5) 0.030(4) Cl2 0.126(4) 0.136(5) 0.174(6) 0.003(4) 0.071(4) 0.030(4) Cl3 0.155(5) 0.122(5) 0.203(7) -0.011(4) 0.082(5) -0.014(4) Cl4 0.143(4) 0.084(3) 0.120(4) -0.005(3) -0.015(3) 0.036(3) Cl5 0.082(3) 0.165(5) 0.063(3) -0.026(3) 0.007(2) -0.025(3) Cl6 0.107(3) 0.070(3) 0.134(4) 0.009(3) 0.001(3) -0.010(3) Cl7 0.105(5) 0.306(10) 0.257(9) -0.060(8) 0.010(5) -0.007(6) Cl8 0.195(6) 0.132(5) 0.097(4) 0.024(3) -0.017(4) -0.075(4) Cl9 0.166(5) 0.126(5) 0.127(5) 0.004(4) 0.015(4) -0.072(4) N12 0.009(5) 0.024(6) 0.040(6) -0.006(5) 0.006(5) -0.009(4) N13 0.017(5) 0.043(7) 0.033(7) -0.008(6) -0.002(5) -0.014(5) N23 0.029(6) 0.021(6) 0.035(7) -0.005(5) 0.007(5) 0.006(5) C101 0.031(7) 0.033(8) 0.036(9) -0.008(7) 0.017(7) -0.006(6) C102 0.028(7) 0.037(9) 0.042(10) -0.002(7) -0.006(7) 0.003(7) C103 0.047(9) 0.046(10) 0.078(13) 0.023(9) 0.008(8) 0.006(8) C104 0.032(8) 0.041(10) 0.100(15) 0.019(11) 0.011(9) 0.005(7) C105 0.076(11) 0.036(10) 0.108(16) -0.027(10) 0.025(11) 0.000(9) C106 0.066(9) 0.031(8) 0.043(10) -0.009(7) 0.012(7) -0.001(7) C107 0.024(7) 0.035(7) 0.023(7) -0.010(6) 0.002(6) -0.001(6) C108 0.036(9) 0.122(13) 0.028(9) 0.023(9) 0.008(7) 0.015(8) C109 0.057(11) 0.186(19) 0.055(13) 0.026(12) -0.008(9) 0.007(12) C110 0.070(11) 0.129(14) 0.034(10) 0.034(10) 0.012(9) 0.019(11) C111 0.052(9) 0.069(10) 0.043(10) 0.007(8) 0.017(8) -0.012(8) C112 0.031(8) 0.058(9) 0.032(9) 0.010(7) 0.007(6) -0.009(6) C113 0.026(7) 0.022(8) 0.039(8) -0.004(6) 0.008(6) 0.002(6) C114 0.041(8) 0.014(7) 0.035(8) -0.008(6) 0.002(7) -0.001(6) C115 0.056(9) 0.045(10) 0.052(10) -0.002(8) -0.006(7) 0.003(9) C116 0.051(10) 0.035(10) 0.100(13) 0.023(8) 0.017(9) 0.023(8) C117 0.066(11) 0.027(10) 0.154(17) 0.016(10) 0.007(11) -0.006(9) C118 0.036(8) 0.036(10) 0.108(13) -0.010(9) -0.010(8) -0.008(8) C119 0.043(8) 0.033(7) 0.031(9) -0.011(6) 0.019(8) -0.024(6) C120 0.059(10) 0.114(13) 0.035(11) 0.010(9) -0.017(9) 0.009(9) C121 0.104(15) 0.155(17) 0.025(12) -0.016(10) 0.012(10) -0.030(13) C122 0.115(16) 0.176(20) 0.029(12) -0.035(12) 0.046(13) -0.021(15) C123 0.104(16) 0.216(24) 0.067(16) -0.047(16) 0.039(14) 0.040(16) C124 0.047(10) 0.135(15) 0.057(12) -0.007(10) 0.022(9) 0.018(10) C201 0.011(6) 0.038(8) 0.034(8) 0.002(7) 0.005(5) 0.001(6) C202 0.037(8) 0.048(9) 0.050(10) 0.013(8) -0.006(7) -0.003(7) C203 0.057(9) 0.093(13) 0.023(9) 0.014(8) -0.016(8) 0.006(9) C204 0.045(9) 0.082(12) 0.053(11) -0.019(10) -0.015(8) -0.012(9) C205 0.048(9) 0.055(10) 0.044(10) -0.011(9) -0.001(8) -0.011(7) C206 0.046(8) 0.044(9) 0.038(9) -0.013(7) -0.004(7) -0.015(7) C207 0.024(7) 0.032(7) 0.021(7) 0.003(6) 0.001(6) -0.002(6) C208 0.032(8) 0.034(8) 0.045(9) 0.005(7) 0.007(7) 0.005(6) C209 0.049(9) 0.042(9) 0.052(10) 0.010(8) 0.018(7) 0.000(8) C210 0.067(10) 0.031(8) 0.048(10) 0.012(7) 0.007(8) -0.020(8) C211 0.051(9) 0.046(9) 0.046(10) 0.018(8) -0.007(8) 0.000(7) C212 0.029(7) 0.042(8) 0.034(8) 0.014(7) 0.004(6) -0.001(7) C213 0.035(8) 0.015(7) 0.036(8) -0.003(6) -0.003(6) 0.006(6) C214 0.050(8) 0.046(8) 0.029(9) -0.004(7) 0.007(8) 0.003(7) C215 0.072(11) 0.051(9) 0.029(10) -0.013(7) 0.010(8) 0.011(8) C216 0.065(11) 0.055(9) 0.033(10) -0.005(7) -0.006(8) 0.001(8) C217 0.033(8) 0.078(11) 0.044(10) 0.000(8) -0.018(8) -0.002(8) C218 0.039(9) 0.049(9) 0.044(10) -0.012(7) 0.005(7) 0.005(7) C219 0.022(6) 0.018(7) 0.045(9) 0.004(6) -0.002(6) -0.003(6) C220 0.043(8) 0.027(8) 0.057(10) 0.005(8) -0.002(7) -0.007(7) C221 0.045(9) 0.029(9) 0.057(11) 0.001(8) -0.004(8) -0.014(7) C222 0.073(10) 0.029(9) 0.079(13) 0.021(8) 0.003(10) -0.004(8) C223 0.090(12) 0.043(10) 0.087(13) 0.027(10) -0.041(10) -0.028(9) C224 0.062(9) 0.035(9) 0.068(11) 0.015(8) -0.034(9) -0.022(7) C301 0.022(6) 0.026(8) 0.025(9) 0.002(6) -0.007(6) -0.006(6) C302 0.082(11) 0.072(11) 0.048(12) 0.005(10) -0.001(9) -0.043(9) C303 0.140(17) 0.137(17) 0.044(12) 0.037(12) -0.020(11) -0.083(15) C304 0.066(10) 0.082(13) 0.059(13) 0.033(10) 0.011(9) -0.014(9) C305 0.109(14) 0.036(10) 0.101(16) 0.000(11) 0.040(12) -0.030(9) C306 0.118(13) 0.044(10) 0.052(11) -0.005(9) 0.034(10) -0.026(10) C307 0.026(7) 0.030(7) 0.034(9) 0.007(7) 0.009(6) -0.016(6) C308 0.034(8) 0.064(10) 0.062(11) 0.019(9) -0.002(7) -0.006(7) C309 0.070(11) 0.063(10) 0.061(11) 0.026(8) -0.023(9) 0.004(9) C310 0.016(8) 0.100(13) 0.133(17) 0.037(12) -0.034(9) -0.011(8) C311 0.028(9) 0.174(19) 0.118(16) 0.100(15) -0.023(10) -0.007(10) C312 0.045(10) 0.109(13) 0.085(13) 0.063(11) 0.000(9) -0.009(9) C313 0.025(6) 0.019(7) 0.035(8) -0.007(6) 0.003(6) -0.014(6) C314 0.038(7) 0.031(8) 0.040(10) 0.008(7) 0.002(6) 0.002(7) C315 0.059(10) 0.066(11) 0.052(12) 0.013(10) -0.031(9) -0.013(8) C316 0.119(15) 0.061(12) 0.044(12) 0.008(10) -0.004(11) -0.037(11) C317 0.149(17) 0.060(11) 0.034(12) -0.011(9) 0.047(11) -0.021(12) C318 0.074(10) 0.031(8) 0.062(12) -0.018(8) 0.027(9) -0.003(7) C319 0.023(7) 0.030(8) 0.058(10) -0.009(7) 0.004(7) -0.006(6) C320 0.045(10) 0.067(11) 0.100(13) 0.050(10) 0.002(9) -0.005(8) C321 0.035(10) 0.120(15) 0.127(16) 0.038(13) -0.038(10) -0.005(10) C322 0.015(8) 0.088(14) 0.176(21) -0.017(13) -0.003(11) -0.021(9) C323 0.050(13) 0.131(18) 0.159(20) 0.055(15) 0.009(12) -0.021(11) C324 0.026(8) 0.098(12) 0.097(13) 0.032(10) -0.007(8) -0.006(8) C8 0.071(13) 0.122(19) 0.188(24) 0.060(17) 0.030(15) -0.018(13) Cl10 0.097(8) 0.384(36) 0.184(14) 0.050(19) -0.019(8) 0.046(16) Cl11 0.211(15) 0.163(11) 0.139(11) 0.022(8) 0.045(9) 0.065(9) Cl12 0.164(12) 0.218(15) 0.187(14) -0.069(11) 0.060(10) -0.011(10) Cl1A 0.263(46) 0.202(30) 0.427(53) -0.095(34) 0.024(39) -0.104(32) Cl2A 0.275(35) 0.466(58) 0.159(30) 0.067(35) 0.034(24) 0.185(39) Cl3A 0.212(28) 0.174(23) 0.291(43) 0.118(23) 0.115(27) 0.092(21) _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 2.506(3) . ? Hg1 P13 2.508(3) . ? Hg1 Hg3 2.7871(8) . ? Hg1 Hg2 2.8235(11) . ? Hg2 P21 2.519(3) . ? Hg2 P23 2.536(3) . ? Hg2 Hg3 2.7989(8) . ? Hg3 P32 2.509(3) . ? Hg3 P31 2.524(3) . ? P12 N12 1.684(9) . ? P12 C107 1.802(11) . ? P12 C101 1.831(11) . ? P13 N13 1.692(9) . ? P13 C113 1.787(11) . ? P13 C119 1.816(12) . ? P21 N12 1.669(9) . ? P21 C201 1.790(11) . ? P21 C207 1.826(11) . ? P23 N23 1.669(9) . ? P23 C219 1.795(11) . ? P23 C213 1.803(11) . ? P31 N13 1.653(10) . ? P31 C307 1.777(11) . ? P31 C301 1.813(11) . ? P32 N23 1.687(9) . ? P32 C313 1.798(11) . ? P32 C319 1.807(11) . ? S1 O1 1.438(7) . ? S1 O3 1.445(7) . ? S1 O2 1.448(8) . ? S1 C1 1.838(13) . ? S2 O5 1.432(8) . ? S2 O4 1.443(8) . ? S2 O6 1.458(9) . ? S2 C2 1.82(2) . ? S3 O7 1.434(8) . ? S3 O8 1.437(7) . ? S3 O9 1.445(8) . ? S3 C3 1.790(13) . ? S4 O10 1.402(8) . ? S4 O12 1.421(9) . ? S4 O11 1.429(11) . ? S4 C4 1.79(2) . ? O12 H23N 1.99(2) 2_545 ? F1 C1 1.35(2) . ? F2 C1 1.298(14) . ? F3 C1 1.329(15) . ? F4 C2 1.32(2) . ? F5 C2 1.34(2) . ? F6 C2 1.30(2) . ? F7 C3 1.323(13) . ? F8 C3 1.346(13) . ? F9 C3 1.321(13) . ? F10 C4 1.28(2) . ? F11 C4 1.27(3) . ? F12 C4 1.31(2) . ? C5 Cl2 1.710(15) . ? C5 Cl1 1.71(2) . ? C5 Cl3 1.75(2) . ? C6 Cl5 1.726(14) . ? C6 Cl4 1.735(14) . ? C6 Cl6 1.750(14) . ? C7 Cl7 1.57(2) . ? C7 Cl8 1.73(2) . ? C7 Cl9 1.75(3) . ? C101 C102 1.374(15) . ? C101 C106 1.404(15) . ? C102 C103 1.40(2) . ? C103 C104 1.36(2) . ? C104 C105 1.34(2) . ? C105 C106 1.41(2) . ? C107 C108 1.345(15) . ? C107 C112 1.382(14) . ? C108 C109 1.38(2) . ? C109 C110 1.38(2) . ? C110 C111 1.34(2) . ? C111 C112 1.39(2) . ? C113 C114 1.378(14) . ? C113 C118 1.40(2) . ? C114 C115 1.35(2) . ? C115 C116 1.36(2) . ? C116 C117 1.39(2) . ? C117 C118 1.37(2) . ? C119 C120 1.35(2) . ? C119 C124 1.36(2) . ? C120 C121 1.39(2) . ? C121 C122 1.35(2) . ? C122 C123 1.38(2) . ? C123 C124 1.37(2) . ? C201 C206 1.382(14) . ? C201 C202 1.415(15) . ? C202 C203 1.41(2) . ? C203 C204 1.37(2) . ? C204 C205 1.35(2) . ? C205 C206 1.38(2) . ? C207 C212 1.382(14) . ? C207 C208 1.390(14) . ? C208 C209 1.37(2) . ? C209 C210 1.37(2) . ? C210 C211 1.39(2) . ? C211 C212 1.38(2) . ? C213 C214 1.367(15) . ? C213 C218 1.412(15) . ? C214 C215 1.38(2) . ? C215 C216 1.40(2) . ? C216 C217 1.35(2) . ? C217 C218 1.38(2) . ? C219 C224 1.378(15) . ? C219 C220 1.401(14) . ? C220 C221 1.38(2) . ? C221 C222 1.35(2) . ? C222 C223 1.38(2) . ? C223 C224 1.38(2) . ? C301 C302 1.34(2) . ? C301 C306 1.39(2) . ? C302 C303 1.40(2) . ? C303 C304 1.31(2) . ? C304 C305 1.38(2) . ? C305 C306 1.38(2) . ? C307 C312 1.37(2) . ? C307 C308 1.38(2) . ? C308 C309 1.39(2) . ? C309 C310 1.38(2) . ? C310 C311 1.33(2) . ? C311 C312 1.37(2) . ? C313 C318 1.39(2) . ? C313 C314 1.396(14) . ? C314 C315 1.40(2) . ? C315 C316 1.37(2) . ? C316 C317 1.35(2) . ? C317 C318 1.38(2) . ? C319 C320 1.34(2) . ? C319 C324 1.39(2) . ? C320 C321 1.41(2) . ? C321 C322 1.33(2) . ? C322 C323 1.39(2) . ? C323 C324 1.36(2) . ? C8 Cl10 1.58(2) . ? C8 Cl11 1.73(2) . ? C8 Cl12 1.86(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 P12 Hg1 P13 116.59(9) . . ? P12 Hg1 Hg3 151.89(7) . . ? P13 Hg1 Hg3 91.30(7) . . ? P12 Hg1 Hg2 92.19(7) . . ? P13 Hg1 Hg2 151.14(7) . . ? Hg3 Hg1 Hg2 59.84(2) . . ? P21 Hg2 P23 118.02(9) . . ? P21 Hg2 Hg3 150.49(7) . . ? P23 Hg2 Hg3 91.30(7) . . ? P21 Hg2 Hg1 91.82(7) . . ? P23 Hg2 Hg1 149.74(6) . . ? Hg3 Hg2 Hg1 59.43(2) . . ? P32 Hg3 P31 113.22(9) . . ? P32 Hg3 Hg1 153.09(7) . . ? P31 Hg3 Hg1 93.61(7) . . ? P32 Hg3 Hg2 92.41(7) . . ? P31 Hg3 Hg2 153.24(7) . . ? Hg1 Hg3 Hg2 60.72(2) . . ? N12 P12 C107 108.2(5) . . ? N12 P12 C101 102.6(5) . . ? C107 P12 C101 105.8(5) . . ? N12 P12 Hg1 108.2(3) . . ? C107 P12 Hg1 117.0(4) . . ? C101 P12 Hg1 114.0(3) . . ? N13 P13 C113 110.8(5) . . ? N13 P13 C119 104.3(5) . . ? C113 P13 C119 104.3(5) . . ? N13 P13 Hg1 109.6(4) . . ? C113 P13 Hg1 112.9(4) . . ? C119 P13 Hg1 114.5(3) . . ? N12 P21 C201 101.9(5) . . ? N12 P21 C207 109.1(5) . . ? C201 P21 C207 107.3(5) . . ? N12 P21 Hg2 109.3(3) . . ? C201 P21 Hg2 115.5(3) . . ? C207 P21 Hg2 113.1(4) . . ? N23 P23 C219 103.8(5) . . ? N23 P23 C213 109.5(5) . . ? C219 P23 C213 104.1(5) . . ? N23 P23 Hg2 110.8(3) . . ? C219 P23 Hg2 113.0(4) . . ? C213 P23 Hg2 114.9(4) . . ? N13 P31 C307 104.0(5) . . ? N13 P31 C301 109.3(5) . . ? C307 P31 C301 107.7(5) . . ? N13 P31 Hg3 109.1(3) . . ? C307 P31 Hg3 114.9(4) . . ? C301 P31 Hg3 111.5(4) . . ? N23 P32 C313 109.4(5) . . ? N23 P32 C319 104.1(5) . . ? C313 P32 C319 107.1(6) . . ? N23 P32 Hg3 108.1(3) . . ? C313 P32 Hg3 118.0(4) . . ? C319 P32 Hg3 109.3(4) . . ? O1 S1 O3 114.7(5) . . ? O1 S1 O2 114.4(5) . . ? O3 S1 O2 114.8(5) . . ? O1 S1 C1 101.6(6) . . ? O3 S1 C1 103.8(6) . . ? O2 S1 C1 105.3(6) . . ? O5 S2 O4 114.2(5) . . ? O5 S2 O6 114.0(6) . . ? O4 S2 O6 114.5(5) . . ? O5 S2 C2 104.6(8) . . ? O4 S2 C2 105.9(8) . . ? O6 S2 C2 102.0(8) . . ? O7 S3 O8 116.7(5) . . ? O7 S3 O9 115.5(5) . . ? O8 S3 O9 113.0(5) . . ? O7 S3 C3 103.7(6) . . ? O8 S3 C3 102.6(5) . . ? O9 S3 C3 102.8(6) . . ? O10 S4 O12 115.8(6) . . ? O10 S4 O11 114.8(7) . . ? O12 S4 O11 112.9(7) . . ? O10 S4 C4 103.1(8) . . ? O12 S4 C4 103.3(8) . . ? O11 S4 C4 105.2(10) . . ? S3 O9 H12N 136.0(25) . . ? S4 O10 H13N 169.8(33) . . ? S4 O12 H23N 147.6(34) . 2_545 ? F2 C1 F3 109.7(12) . . ? F2 C1 F1 109.0(12) . . ? F3 C1 F1 107.8(12) . . ? F2 C1 S1 111.5(10) . . ? F3 C1 S1 110.0(10) . . ? F1 C1 S1 108.8(10) . . ? F6 C2 F4 109.6(17) . . ? F6 C2 F5 105.1(16) . . ? F4 C2 F5 108.7(18) . . ? F6 C2 S2 111.2(15) . . ? F4 C2 S2 111.7(13) . . ? F5 C2 S2 110.3(13) . . ? F9 C3 F7 106.5(10) . . ? F9 C3 F8 105.6(10) . . ? F7 C3 F8 104.9(10) . . ? F9 C3 S3 113.7(9) . . ? F7 C3 S3 113.1(9) . . ? F8 C3 S3 112.3(9) . . ? F11 C4 F10 108.6(22) . . ? F11 C4 F12 108.7(19) . . ? F10 C4 F12 104.3(17) . . ? F11 C4 S4 111.7(16) . . ? F10 C4 S4 112.6(14) . . ? F12 C4 S4 110.7(16) . . ? Cl2 C5 Cl1 112.5(11) . . ? Cl2 C5 Cl3 110.1(9) . . ? Cl1 C5 Cl3 108.8(9) . . ? Cl5 C6 Cl4 111.9(8) . . ? Cl5 C6 Cl6 110.5(8) . . ? Cl4 C6 Cl6 110.1(8) . . ? Cl7 C7 Cl8 116.3(19) . . ? Cl7 C7 Cl9 115.6(18) . . ? Cl8 C7 Cl9 110.4(12) . . ? H12N N12 P21 118.9(60) . . ? H12N N12 P12 109.3(60) . . ? P21 N12 P12 127.3(5) . . ? H13N N13 P31 125.2(81) . . ? H13N N13 P13 105.0(81) . . ? P31 N13 P13 129.5(6) . . ? H23N N23 P23 117.8(80) . . ? H23N N23 P32 111.7(80) . . ? P23 N23 P32 126.2(6) . . ? C102 C101 C106 122.3(11) . . ? C102 C101 P12 120.3(9) . . ? C106 C101 P12 117.3(10) . . ? C101 C102 C103 118.1(12) . . ? C104 C103 C102 120.2(13) . . ? C105 C104 C103 121.9(13) . . ? C104 C105 C106 120.6(14) . . ? C101 C106 C105 116.8(12) . . ? C108 C107 C112 120.9(11) . . ? C108 C107 P12 120.0(9) . . ? C112 C107 P12 119.0(9) . . ? C107 C108 C109 118.9(12) . . ? C108 C109 C110 120.9(13) . . ? C111 C110 C109 119.8(13) . . ? C110 C111 C112 119.8(12) . . ? C107 C112 C111 119.7(11) . . ? C114 C113 C118 116.9(10) . . ? C114 C113 P13 121.3(9) . . ? C118 C113 P13 121.5(9) . . ? C115 C114 C113 122.2(10) . . ? C114 C115 C116 120.5(11) . . ? C115 C116 C117 119.5(12) . . ? C118 C117 C116 119.8(12) . . ? C117 C118 C113 121.0(11) . . ? C120 C119 C124 118.3(12) . . ? C120 C119 P13 122.6(10) . . ? C124 C119 P13 118.9(11) . . ? C119 C120 C121 119.2(14) . . ? C122 C121 C120 123.9(16) . . ? C121 C122 C123 115.3(15) . . ? C124 C123 C122 121.8(15) . . ? C119 C124 C123 121.2(14) . . ? C206 C201 C202 118.7(10) . . ? C206 C201 P21 123.8(9) . . ? C202 C201 P21 117.4(9) . . ? C203 C202 C201 118.2(11) . . ? C204 C203 C202 121.1(12) . . ? C205 C204 C203 120.3(12) . . ? C204 C205 C206 120.6(12) . . ? C201 C206 C205 121.1(11) . . ? C212 C207 C208 120.8(10) . . ? C212 C207 P21 118.9(8) . . ? C208 C207 P21 120.3(9) . . ? C209 C208 C207 119.4(10) . . ? C210 C209 C208 121.0(11) . . ? C209 C210 C211 119.3(11) . . ? C212 C211 C210 120.7(11) . . ? C207 C212 C211 118.7(10) . . ? C214 C213 C218 118.6(11) . . ? C214 C213 P23 121.4(9) . . ? C218 C213 P23 119.6(9) . . ? C213 C214 C215 121.4(11) . . ? C214 C215 C216 118.9(11) . . ? C217 C216 C215 120.7(12) . . ? C216 C217 C218 120.2(11) . . ? C217 C218 C213 120.1(11) . . ? C224 C219 C220 118.5(10) . . ? C224 C219 P23 119.2(9) . . ? C220 C219 P23 122.2(9) . . ? C221 C220 C219 120.1(11) . . ? C222 C221 C220 120.7(11) . . ? C221 C222 C223 120.0(11) . . ? C224 C223 C222 120.2(12) . . ? C219 C224 C223 120.4(11) . . ? C302 C301 C306 119.0(11) . . ? C302 C301 P31 120.3(9) . . ? C306 C301 P31 120.7(10) . . ? C301 C302 C303 120.5(13) . . ? C304 C303 C302 121.5(15) . . ? C303 C304 C305 119.1(14) . . ? C306 C305 C304 120.7(13) . . ? C305 C306 C301 119.2(13) . . ? C312 C307 C308 115.1(11) . . ? C312 C307 P31 125.1(10) . . ? C308 C307 P31 119.8(8) . . ? C307 C308 C309 122.3(12) . . ? C310 C309 C308 118.7(12) . . ? C311 C310 C309 120.4(12) . . ? C310 C311 C312 119.8(14) . . ? C311 C312 C307 123.6(13) . . ? C318 C313 C314 118.6(11) . . ? C318 C313 P32 122.4(10) . . ? C314 C313 P32 118.9(9) . . ? C313 C314 C315 117.8(11) . . ? C316 C315 C314 123.4(13) . . ? C317 C316 C315 117.6(14) . . ? C316 C317 C318 121.8(14) . . ? C317 C318 C313 120.8(13) . . ? C320 C319 C324 119.9(11) . . ? C320 C319 P32 119.9(10) . . ? C324 C319 P32 120.1(10) . . ? C319 C320 C321 118.7(13) . . ? C322 C321 C320 120.5(15) . . ? C321 C322 C323 121.4(14) . . ? C324 C323 C322 117.4(15) . . ? C323 C324 C319 121.9(14) . . ? Cl10 C8 Cl11 117.1(18) . . ? Cl10 C8 Cl12 112.6(14) . . ? Cl11 C8 Cl12 101.9(14) . . ? _refine_diff_density_max 0.618 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.104 #============================================================================ _eof # End of Crystallographic Information File