data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H48 Cl8 Hg4 O8 S4' _chemical_formula_weight 1678.82 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' 'S' 'S' 0.1246 0.1234 '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' '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 7.3984(8) _cell_length_b 17.3535(19) _cell_length_c 17.4765(18) _cell_angle_alpha 104.620(6) _cell_angle_beta 93.011(6) _cell_angle_gamma 101.573(6) _cell_volume 2114.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9609 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.90 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 1.10 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 15.222 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0213 _exptl_absorpt_correction_T_max 0.5166 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31899 _diffrn_reflns_av_R_equivalents 0.0838 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8284 _reflns_number_gt 6252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+58.4313P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8284 _refine_ls_number_parameters 471 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1482 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.68580(8) 0.28755(3) 0.50742(3) 0.02569(16) Uani 1 1 d . B . Hg2 Hg 0.27702(8) 0.26507(3) 1.12175(3) 0.02944(17) Uani 1 1 d . . . Hg3 Hg 0.96518(9) 0.18256(4) 0.71155(4) 0.03785(19) Uani 1 1 d . . . Hg4 Hg 0.45659(9) 0.17392(4) 0.87447(4) 0.03794(19) Uani 1 1 d . . . Cl1 Cl 0.5821(5) 0.3404(2) 0.4066(2) 0.0304(8) Uani 1 1 d . . . Cl2 Cl 0.1570(6) 0.3123(2) 1.2436(2) 0.0365(9) Uani 1 1 d . . . Cl3 Cl 0.9169(5) 0.0940(2) 0.5798(2) 0.0335(9) Uani 1 1 d . . . Cl4 Cl 1.1754(5) 0.1035(2) 0.7727(2) 0.0303(8) Uani 1 1 d . . . Cl5 Cl 1.0663(6) 0.3254(2) 0.7673(3) 0.0407(10) Uani 1 1 d . . . Cl6 Cl 0.6798(5) 0.1210(2) 0.7741(2) 0.0305(8) Uani 1 1 d . . . Cl7 Cl 0.5524(5) 0.3197(2) 0.9167(3) 0.0372(9) Uani 1 1 d . . . Cl8 Cl 0.4441(5) 0.0881(2) 0.9633(2) 0.0278(8) Uani 1 1 d . . . S1 S 1.0435(5) 0.2836(2) 0.5086(2) 0.0244(8) Uani 1 1 d . . . S2 S 0.6262(5) 0.2384(2) 0.6265(2) 0.0278(8) Uani 1 1 d . . . S3 S 0.6240(5) 0.2685(2) 1.1336(2) 0.0241(8) Uani 1 1 d . . . S4 S 0.1324(4) 0.22431(19) 0.98090(19) 0.0185(7) Uani 1 1 d . A . O1 O 0.9120(13) 0.4418(6) 0.5779(6) 0.031(2) Uani 1 1 d . . . O2 O 0.5445(15) 0.4059(6) 0.6155(7) 0.037(3) Uani 1 1 d . B . O3 O 0.4175(14) 0.1475(6) 0.4598(7) 0.033(3) Uani 1 1 d . B . O4 O 0.7504(14) 0.1494(6) 0.3899(7) 0.030(2) Uani 1 1 d . . . O5 O 0.3531(15) 0.1378(6) 1.1909(7) 0.036(3) Uani 1 1 d . . . O6 O -0.002(3) 0.1318(12) 1.1070(13) 0.026(7) Uani 0.53(5) 1 d P A 1 O6' O 0.073(4) 0.1076(14) 1.0841(14) 0.020(7) Uani 0.47(5) 1 d PU A 2 O7 O 0.1347(14) 0.4040(6) 1.0787(6) 0.030(2) Uani 1 1 d . . . O8 O 0.5030(14) 0.4338(6) 1.1502(6) 0.028(2) Uani 1 1 d . . . C1 C 1.137(2) 0.3879(9) 0.5051(10) 0.032(4) Uani 1 1 d . . . H1A H 1.2719 0.3954 0.4998 0.038 Uiso 1 1 calc R . . H1B H 1.0759 0.3983 0.4582 0.038 Uiso 1 1 calc R . . C2 C 1.107(2) 0.4473(9) 0.5794(10) 0.033(4) Uani 1 1 d . . . H2A H 1.1550 0.4335 0.6270 0.039 Uiso 1 1 calc R . . H2B H 1.1723 0.5035 0.5809 0.039 Uiso 1 1 calc R . . C3 C 0.859(2) 0.4894(9) 0.6492(10) 0.037(4) Uani 1 1 d . . . H3A H 0.9310 0.5466 0.6614 0.044 Uiso 1 1 calc R . . H3B H 0.8861 0.4672 0.6943 0.044 Uiso 1 1 calc R . . C4 C 0.659(2) 0.4869(10) 0.6375(11) 0.035(4) Uani 1 1 d . . . H4A H 0.6216 0.5184 0.6874 0.042 Uiso 1 1 calc R . . H4B H 0.6366 0.5140 0.5955 0.042 Uiso 1 1 calc R . . C5 C 0.487(3) 0.3762(12) 0.6798(11) 0.053(6) Uani 1 1 d . . . H5A H 0.4872 0.4237 0.7253 0.064 Uiso 0.72(3) 1 calc PR B 1 H5B H 0.3569 0.3451 0.6651 0.064 Uiso 0.72(3) 1 calc PR B 1 H5C H 0.3698 0.3926 0.6939 0.064 Uiso 0.28(3) 1 calc PR B 2 H5D H 0.5816 0.4025 0.7262 0.064 Uiso 0.28(3) 1 calc PR B 2 C6 C 0.587(3) 0.3273(13) 0.7058(10) 0.022(5) Uani 0.72(3) 1 d P B 1 H6A H 0.5217 0.3061 0.7468 0.027 Uiso 0.72(3) 1 calc PR B 1 H6B H 0.7095 0.3613 0.7317 0.027 Uiso 0.72(3) 1 calc PR B 1 C7 C 0.404(3) 0.1736(13) 0.6040(11) 0.025(5) Uani 0.72(3) 1 d P B 1 H7A H 0.3783 0.1459 0.6465 0.030 Uiso 0.72(3) 1 calc PR B 1 H7B H 0.3096 0.2063 0.6014 0.030 Uiso 0.72(3) 1 calc PR B 1 C6' C 0.455(7) 0.281(3) 0.664(3) 0.024(13) Uani 0.28(3) 1 d PU B 2 H6'A H 0.3405 0.2552 0.6275 0.029 Uiso 0.28(3) 1 calc PR B 2 H6'B H 0.4342 0.2672 0.7153 0.029 Uiso 0.28(3) 1 calc PR B 2 C7' C 0.461(7) 0.126(3) 0.576(3) 0.019(12) Uani 0.28(3) 1 d PU B 2 H7'A H 0.5419 0.0867 0.5737 0.023 Uiso 0.28(3) 1 calc PR B 2 H7'B H 0.3720 0.1160 0.6145 0.023 Uiso 0.28(3) 1 calc PR B 2 C8 C 0.392(3) 0.1112(10) 0.5260(11) 0.048(5) Uani 1 1 d . . . H8A H 0.4875 0.0793 0.5290 0.058 Uiso 0.72(3) 1 calc PR B 1 H8B H 0.2688 0.0731 0.5161 0.058 Uiso 0.72(3) 1 calc PR B 1 H8C H 0.2627 0.1124 0.5377 0.058 Uiso 0.28(3) 1 calc PR B 2 H8D H 0.3927 0.0529 0.5035 0.058 Uiso 0.28(3) 1 calc PR B 2 C9 C 0.437(2) 0.0918(10) 0.3858(10) 0.034(4) Uani 1 1 d . . . H9A H 0.4099 0.1153 0.3416 0.041 Uiso 1 1 calc R B . H9B H 0.3437 0.0400 0.3782 0.041 Uiso 1 1 calc R . . C10 C 0.624(2) 0.0741(9) 0.3825(9) 0.035(4) Uani 1 1 d . B . H10A H 0.6539 0.0505 0.4263 0.042 Uiso 1 1 calc R . . H10B H 0.6308 0.0346 0.3313 0.042 Uiso 1 1 calc R . . C11 C 0.941(2) 0.1428(10) 0.3896(10) 0.035(4) Uani 1 1 d . . . H11A H 0.9614 0.1098 0.3370 0.042 Uiso 1 1 calc R . . H11B H 0.9732 0.1160 0.4306 0.042 Uiso 1 1 calc R . . C12 C 1.057(2) 0.2281(10) 0.4073(9) 0.033(4) Uani 1 1 d . . . H12A H 1.0121 0.2566 0.3702 0.040 Uiso 1 1 calc R . . H12B H 1.1875 0.2260 0.3994 0.040 Uiso 1 1 calc R . . C13 C 0.657(2) 0.2144(9) 1.2076(9) 0.027(3) Uani 1 1 d . . . H13A H 0.7888 0.2113 1.2141 0.033 Uiso 1 1 calc R . . H13B H 0.6257 0.2448 1.2594 0.033 Uiso 1 1 calc R . . C14 C 0.536(2) 0.1289(9) 1.1832(10) 0.031(3) Uani 1 1 d . . . H14A H 0.5487 0.1012 1.1276 0.037 Uiso 1 1 calc R . . H14B H 0.5710 0.0962 1.2181 0.037 Uiso 1 1 calc R . . C15 C 0.220(3) 0.0614(9) 1.1673(11) 0.040(4) Uani 1 1 d . A . H15A H 0.2219 0.0319 1.2089 0.048 Uiso 1 1 calc R . . H15B H 0.2484 0.0266 1.1171 0.048 Uiso 1 1 calc R . . C16 C 0.035(2) 0.0811(9) 1.1559(8) 0.026(3) Uani 1 1 d . . . H16A H -0.0560 0.0283 1.1354 0.032 Uiso 0.53(5) 1 calc PR A 1 H16B H 0.0031 0.1061 1.2096 0.032 Uiso 0.53(5) 1 calc PR A 1 H16C H -0.0693 0.0326 1.1460 0.032 Uiso 0.47(5) 1 calc PR A 2 H16D H 0.0132 0.1254 1.2004 0.032 Uiso 0.47(5) 1 calc PR A 2 C17 C -0.044(5) 0.086(2) 1.025(2) 0.034(9) Uani 0.53(5) 1 d PU A 1 H17A H 0.0516 0.0535 1.0107 0.041 Uiso 0.53(5) 1 calc PR A 1 H17B H -0.1652 0.0465 1.0187 0.041 Uiso 0.53(5) 1 calc PR A 1 C17' C -0.091(4) 0.118(2) 1.0409(17) 0.017(8) Uani 0.47(5) 1 d PU A 2 H17C H -0.1884 0.0672 1.0295 0.020 Uiso 0.47(5) 1 calc PR A 2 H17D H -0.1395 0.1626 1.0746 0.020 Uiso 0.47(5) 1 calc PR A 2 C18 C -0.052(2) 0.1356(9) 0.9725(10) 0.038(4) Uani 1 1 d . . . H18A H -0.1693 0.1547 0.9780 0.046 Uiso 0.53(5) 1 calc PR A 1 H18B H -0.0618 0.1001 0.9176 0.046 Uiso 0.53(5) 1 calc PR A 1 H18C H -0.1662 0.1440 0.9467 0.046 Uiso 0.47(5) 1 calc PR A 2 H18D H -0.0182 0.0877 0.9369 0.046 Uiso 0.47(5) 1 calc PR A 2 C19 C -0.009(2) 0.2939(9) 0.9714(10) 0.035(4) Uani 1 1 d . . . H19A H -0.0644 0.2798 0.9154 0.042 Uiso 1 1 calc R A . H19B H -0.1122 0.2876 1.0049 0.042 Uiso 1 1 calc R . . C20 C 0.096(2) 0.3814(9) 0.9952(9) 0.032(4) Uani 1 1 d . A . H20A H 0.2126 0.3871 0.9699 0.039 Uiso 1 1 calc R . . H20B H 0.0203 0.4166 0.9786 0.039 Uiso 1 1 calc R . . C21 C 0.251(2) 0.4829(9) 1.1110(10) 0.033(4) Uani 1 1 d . . . H21A H 0.2309 0.5028 1.1675 0.039 Uiso 1 1 calc R . . H21B H 0.2135 0.5207 1.0824 0.039 Uiso 1 1 calc R . . C22 C 0.450(2) 0.4850(9) 1.1058(10) 0.033(4) Uani 1 1 d . . . H22A H 0.4732 0.4654 1.0496 0.040 Uiso 1 1 calc R . . H22B H 0.5241 0.5415 1.1275 0.040 Uiso 1 1 calc R . . C23 C 0.697(2) 0.4311(9) 1.1513(11) 0.036(4) Uani 1 1 d . . . H23A H 0.7750 0.4856 1.1784 0.043 Uiso 1 1 calc R . . H23B H 0.7298 0.4148 1.0962 0.043 Uiso 1 1 calc R . . C24 C 0.729(2) 0.3714(9) 1.1938(10) 0.032(4) Uani 1 1 d . . . H24A H 0.6751 0.3821 1.2450 0.039 Uiso 1 1 calc R . . H24B H 0.8644 0.3768 1.2053 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0253(3) 0.0269(3) 0.0244(3) 0.0089(2) 0.0038(2) 0.0019(2) Hg2 0.0353(3) 0.0234(3) 0.0226(3) 0.0044(2) -0.0044(2) -0.0053(2) Hg3 0.0370(4) 0.0354(4) 0.0361(4) 0.0020(3) 0.0024(3) 0.0066(3) Hg4 0.0395(4) 0.0324(3) 0.0423(4) 0.0105(3) 0.0056(3) 0.0078(3) Cl1 0.041(2) 0.0297(18) 0.0218(17) 0.0092(15) -0.0005(16) 0.0086(16) Cl2 0.046(2) 0.033(2) 0.042(2) 0.0188(17) 0.0231(19) 0.0185(18) Cl3 0.037(2) 0.039(2) 0.0176(17) 0.0001(15) 0.0022(15) 0.0017(17) Cl4 0.0236(17) 0.0333(19) 0.032(2) 0.0066(16) -0.0068(15) 0.0076(15) Cl5 0.042(2) 0.0251(18) 0.048(2) 0.0043(17) 0.005(2) -0.0020(17) Cl6 0.0258(18) 0.0353(19) 0.033(2) 0.0099(16) 0.0139(16) 0.0091(16) Cl7 0.0294(19) 0.0199(17) 0.059(3) 0.0077(17) 0.0011(19) 0.0037(15) Cl8 0.0274(18) 0.0334(18) 0.0282(18) 0.0183(15) 0.0060(15) 0.0063(15) S1 0.0219(17) 0.0275(18) 0.0245(18) 0.0077(15) 0.0026(15) 0.0056(15) S2 0.0268(19) 0.040(2) 0.0240(18) 0.0172(16) 0.0065(15) 0.0119(17) S3 0.0279(18) 0.0178(16) 0.0240(18) 0.0022(14) 0.0002(15) 0.0044(14) S4 0.0180(16) 0.0162(15) 0.0181(16) 0.0005(13) -0.0005(13) 0.0023(13) O1 0.022(5) 0.025(5) 0.038(6) -0.007(5) 0.003(5) 0.006(4) O2 0.035(6) 0.029(6) 0.038(6) -0.006(5) 0.006(5) 0.004(5) O3 0.025(5) 0.017(5) 0.051(7) 0.004(5) 0.009(5) 0.000(4) O4 0.025(5) 0.020(5) 0.043(6) 0.004(5) 0.007(5) 0.005(4) O5 0.037(6) 0.012(5) 0.051(7) -0.003(5) 0.008(6) 0.000(4) O6 0.025(12) 0.018(10) 0.028(12) -0.002(9) -0.002(9) 0.000(9) O6' 0.019(8) 0.020(8) 0.020(8) 0.003(5) 0.000(5) 0.005(5) O7 0.033(6) 0.017(5) 0.033(6) -0.003(4) -0.006(5) 0.007(4) O8 0.027(5) 0.018(5) 0.040(6) 0.014(4) 0.004(5) 0.003(4) C1 0.024(8) 0.034(8) 0.039(9) 0.016(7) 0.007(7) -0.001(7) C2 0.015(7) 0.027(8) 0.049(10) 0.007(7) -0.005(7) -0.007(6) C3 0.050(10) 0.016(7) 0.040(9) 0.001(7) 0.010(8) 0.005(7) C4 0.031(8) 0.032(8) 0.041(9) 0.001(7) -0.003(7) 0.014(7) C5 0.065(13) 0.041(10) 0.046(11) 0.002(9) 0.035(10) 0.001(10) C6 0.024(10) 0.037(12) 0.005(9) 0.007(8) -0.004(7) 0.005(9) C7 0.026(11) 0.031(11) 0.016(10) -0.001(9) -0.003(8) 0.012(9) C6' 0.023(14) 0.024(14) 0.024(14) 0.005(6) 0.002(5) 0.006(6) C7' 0.020(13) 0.020(13) 0.019(13) 0.004(6) 0.003(5) 0.004(6) C8 0.079(14) 0.022(8) 0.031(10) -0.003(7) 0.031(10) -0.012(9) C9 0.032(8) 0.027(8) 0.040(9) 0.008(7) 0.001(7) -0.001(7) C10 0.053(10) 0.028(8) 0.023(8) 0.007(6) 0.004(7) 0.008(8) C11 0.030(8) 0.030(8) 0.040(9) -0.003(7) 0.007(7) 0.012(7) C12 0.026(8) 0.045(9) 0.023(8) 0.006(7) 0.009(6) -0.001(7) C13 0.041(9) 0.023(7) 0.022(7) 0.011(6) 0.001(7) 0.014(7) C14 0.039(9) 0.018(7) 0.039(9) 0.014(7) 0.002(7) 0.008(7) C15 0.054(11) 0.009(6) 0.052(11) 0.005(7) 0.010(9) -0.003(7) C16 0.043(9) 0.022(7) 0.015(7) 0.011(6) -0.001(6) 0.003(7) C17 0.034(10) 0.034(10) 0.034(10) 0.009(5) 0.004(5) 0.006(5) C17' 0.015(9) 0.017(9) 0.017(9) 0.002(5) 0.004(5) 0.003(5) C18 0.041(10) 0.025(8) 0.040(9) 0.021(7) -0.024(8) -0.018(7) C19 0.035(9) 0.026(8) 0.042(10) 0.003(7) -0.014(8) 0.015(7) C20 0.046(9) 0.021(7) 0.029(8) 0.000(6) -0.013(7) 0.019(7) C21 0.039(9) 0.016(7) 0.038(9) 0.001(6) -0.012(7) 0.007(7) C22 0.041(9) 0.021(7) 0.039(9) 0.013(7) 0.002(8) 0.004(7) C23 0.031(8) 0.022(7) 0.048(10) 0.006(7) 0.004(8) -0.001(7) C24 0.034(9) 0.019(7) 0.040(9) 0.005(7) -0.017(7) 0.003(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 Cl1 2.343(4) . ? Hg1 S2 2.468(4) . ? Hg1 S1 2.660(4) . ? Hg2 Cl2 2.367(4) . ? Hg2 S4 2.499(3) . ? Hg2 S3 2.552(4) . ? Hg3 Cl5 2.370(4) . ? Hg3 Cl3 2.387(3) . ? Hg3 Cl6 2.592(4) . ? Hg3 Cl4 2.620(4) . ? Hg4 Cl7 2.394(4) . ? Hg4 Cl8 2.400(4) . ? Hg4 Cl4 2.546(4) 1_455 ? Hg4 Cl6 2.598(3) . ? Cl4 Hg4 2.545(4) 1_655 ? S1 C12 1.809(15) . ? S1 C1 1.822(16) . ? S2 C6' 1.67(5) . ? S2 C7 1.76(2) . ? S2 C6 1.879(19) . ? S2 C7' 2.03(5) . ? S3 C13 1.812(15) . ? S3 C24 1.820(15) . ? S4 C19 1.782(15) . ? S4 C18 1.810(15) . ? O1 C2 1.426(17) . ? O1 C3 1.430(18) . ? O2 C5 1.40(2) . ? O2 C4 1.434(19) . ? O3 C9 1.439(19) . ? O3 C8 1.45(2) . ? O4 C10 1.418(18) . ? O4 C11 1.435(18) . ? O5 C14 1.399(19) . ? O5 C15 1.434(18) . ? O6 C16 1.42(2) . ? O6 C17 1.44(4) . ? O6' C17' 1.46(4) . ? O6' C16 1.46(3) . ? O7 C20 1.410(18) . ? O7 C21 1.421(17) . ? O8 C22 1.413(19) . ? O8 C23 1.445(19) . ? C1 C2 1.50(2) . ? C3 C4 1.48(2) . ? C5 C6 1.37(3) . ? C5 C6' 1.57(5) . ? C7 C8 1.50(2) . ? C7' C8 0.94(5) . ? C9 C10 1.48(2) . ? C11 C12 1.50(2) . ? C13 C14 1.52(2) . ? C15 C16 1.49(2) . ? C17 C18 1.42(4) . ? C17' C18 1.34(3) . ? C19 C20 1.50(2) . ? C21 C22 1.48(2) . ? C23 C24 1.47(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 Cl1 Hg1 S2 149.41(13) . . ? Cl1 Hg1 S1 112.82(13) . . ? S2 Hg1 S1 97.57(12) . . ? Cl2 Hg2 S4 131.59(14) . . ? Cl2 Hg2 S3 115.00(14) . . ? S4 Hg2 S3 113.12(11) . . ? Cl5 Hg3 Cl3 134.80(15) . . ? Cl5 Hg3 Cl6 112.07(14) . . ? Cl3 Hg3 Cl6 101.93(13) . . ? Cl5 Hg3 Cl4 110.92(14) . . ? Cl3 Hg3 Cl4 96.42(13) . . ? Cl6 Hg3 Cl4 91.74(13) . . ? Cl7 Hg4 Cl8 123.81(15) . . ? Cl7 Hg4 Cl4 121.00(14) . 1_455 ? Cl8 Hg4 Cl4 103.47(13) . 1_455 ? Cl7 Hg4 Cl6 107.42(13) . . ? Cl8 Hg4 Cl6 103.69(13) . . ? Cl4 Hg4 Cl6 91.39(12) 1_455 . ? Hg4 Cl4 Hg3 123.45(15) 1_655 . ? Hg3 Cl6 Hg4 137.56(16) . . ? C12 S1 C1 100.7(8) . . ? C12 S1 Hg1 102.3(5) . . ? C1 S1 Hg1 99.0(5) . . ? C6' S2 C7 65.0(18) . . ? C6' S2 C6 39.0(18) . . ? C7 S2 C6 102.2(9) . . ? C6' S2 C7' 95(2) . . ? C7 S2 C7' 30.4(15) . . ? C6 S2 C7' 131.1(16) . . ? C6' S2 Hg1 104.9(18) . . ? C7 S2 Hg1 105.5(7) . . ? C6 S2 Hg1 106.7(6) . . ? C7' S2 Hg1 100.7(15) . . ? C13 S3 C24 98.1(7) . . ? C13 S3 Hg2 104.7(5) . . ? C24 S3 Hg2 104.2(5) . . ? C19 S4 C18 97.8(8) . . ? C19 S4 Hg2 107.8(6) . . ? C18 S4 Hg2 105.6(5) . . ? C2 O1 C3 113.5(12) . . ? C5 O2 C4 114.6(13) . . ? C9 O3 C8 114.9(11) . . ? C10 O4 C11 113.5(12) . . ? C14 O5 C15 112.9(11) . . ? C16 O6 C17 111(2) . . ? C17' O6' C16 114(2) . . ? C20 O7 C21 114.3(13) . . ? C22 O8 C23 113.9(12) . . ? C2 C1 S1 110.2(11) . . ? O1 C2 C1 106.9(12) . . ? O1 C3 C4 108.7(13) . . ? O2 C4 C3 113.8(13) . . ? C6 C5 O2 118.0(16) . . ? C6 C5 C6' 47(2) . . ? O2 C5 C6' 115(2) . . ? C5 C6 S2 115.2(13) . . ? C8 C7 S2 110.2(14) . . ? C5 C6' S2 116(3) . . ? C8 C7' S2 124(4) . . ? C7' C8 O3 129(3) . . ? C7' C8 C7 43(3) . . ? O3 C8 C7 112.7(14) . . ? O3 C9 C10 112.9(13) . . ? O4 C10 C9 106.7(13) . . ? O4 C11 C12 106.9(12) . . ? C11 C12 S1 110.1(11) . . ? C14 C13 S3 110.8(11) . . ? O5 C14 C13 106.3(12) . . ? O5 C15 C16 106.6(12) . . ? O6 C16 O6' 33.0(10) . . ? O6 C16 C15 122.8(16) . . ? O6' C16 C15 94.3(16) . . ? C18 C17 O6 113(3) . . ? C18 C17' O6' 112(3) . . ? C17' C18 C17 30.1(15) . . ? C17' C18 S4 115.7(16) . . ? C17 C18 S4 120.2(16) . . ? C20 C19 S4 113.0(11) . . ? O7 C20 C19 106.8(13) . . ? O7 C21 C22 113.6(12) . . ? O8 C22 C21 108.0(13) . . ? O8 C23 C24 108.3(13) . . ? C23 C24 S3 109.9(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.780 _refine_diff_density_min -4.659 _refine_diff_density_rms 0.365 ######################################################### data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H48 Cd2 Hg2 I8 O8 S4' _chemical_formula_weight 2234.04 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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)/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 7.6412(2) _cell_length_b 20.9168(6) _cell_length_c 31.5266(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.078(2) _cell_angle_gamma 90.00 _cell_volume 5026.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 25.36 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4000 _exptl_absorpt_coefficient_mu 12.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0981 _exptl_absorpt_correction_T_max 0.3789 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 59621 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9886 _reflns_number_gt 7637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+6.5445P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9886 _refine_ls_number_parameters 579 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.82940(7) 0.70386(2) 0.669545(15) 0.05777(15) Uani 1 1 d . . . Hg2 Hg 0.66764(7) 0.52793(2) 0.646491(17) 0.06260(16) Uani 1 1 d . . . I1 I 1.00356(9) 0.18918(3) 0.54044(2) 0.04693(19) Uani 1 1 d . A . I2 I 0.36944(9) 1.06769(3) 0.59835(2) 0.04930(19) Uani 1 1 d . . . I3 I 0.82243(9) 0.76458(4) 0.59406(2) 0.0545(2) Uani 1 1 d . . . I4 I 0.99670(15) 0.75627(5) 0.73853(3) 0.0858(3) Uani 1 1 d . . . I5 I 1.01272(8) 0.58003(3) 0.65425(2) 0.04171(17) Uani 1 1 d . . . I6 I 0.51002(9) 0.64392(3) 0.68604(3) 0.0627(2) Uani 1 1 d . . . I7 I 0.55736(10) 0.51733(4) 0.56360(3) 0.0672(2) Uani 1 1 d . . . I8 I 0.61209(10) 0.42787(3) 0.69856(3) 0.0613(2) Uani 1 1 d . . . Cd1 Cd 0.89196(9) 0.30057(3) 0.57071(3) 0.0443(2) Uani 1 1 d . . . Cd2 Cd 0.52510(9) 0.96247(4) 0.63252(2) 0.04300(19) Uani 1 1 d . B . S1 S 0.9641(3) 0.40886(13) 0.60793(12) 0.0634(9) Uani 1 1 d . A . S2 S 0.5475(3) 0.31306(12) 0.57531(9) 0.0447(6) Uani 1 1 d . A . S3 S 0.8743(4) 0.96021(18) 0.63189(12) 0.0711(10) Uani 1 1 d . . . S4 S 0.5034(4) 0.84965(16) 0.66727(11) 0.0645(8) Uani 1 1 d . . . O1 O 1.053(3) 0.3667(11) 0.5281(7) 0.027(6) Uani 0.411(16) 1 d PU A 1 O2 O 0.723(5) 0.3357(18) 0.4982(13) 0.026(7) Uani 0.411(16) 1 d PU A 1 O1' O 1.067(2) 0.3670(7) 0.5122(7) 0.042(4) Uani 0.589(16) 1 d P A 2 O2' O 0.741(4) 0.3238(16) 0.4947(11) 0.055(7) Uani 0.589(16) 1 d P A 2 O3 O 0.7786(8) 0.2380(3) 0.6377(2) 0.0489(18) Uani 1 1 d . A . O4 O 1.1204(10) 0.2818(4) 0.6410(3) 0.057(2) Uani 1 1 d . . . O5 O 0.6332(10) 0.9413(4) 0.5541(3) 0.064(2) Uani 1 1 d . B . O6 O 0.3297(10) 0.8910(3) 0.5823(3) 0.059(2) Uani 1 1 d . . . O7 O 0.3341(11) 0.9757(4) 0.6989(3) 0.069(2) Uani 1 1 d . . . O8 O 0.6619(11) 1.0285(5) 0.6946(3) 0.074(3) Uani 1 1 d . . . C1 C 1.130(2) 0.4375(9) 0.5861(6) 0.021(5) Uani 0.411(16) 1 d PU A 1 H1A H 1.1531 0.4823 0.5949 0.025 Uiso 0.411(16) 1 calc PR A 1 H1B H 1.2368 0.4116 0.5932 0.025 Uiso 0.411(16) 1 calc PR A 1 C2 C 1.074(3) 0.4332(9) 0.5388(7) 0.013(4) Uani 0.411(16) 1 d PU A 1 H2A H 0.9613 0.4562 0.5327 0.015 Uiso 0.411(16) 1 calc PR A 1 H2B H 1.1634 0.4529 0.5218 0.015 Uiso 0.411(16) 1 calc PR A 1 C3 C 1.022(5) 0.3542(18) 0.4862(14) 0.052(10) Uani 0.411(16) 1 d PU A 1 H3A H 1.0472 0.3087 0.4806 0.063 Uiso 0.411(16) 1 calc PR A 1 H3B H 1.0991 0.3808 0.4696 0.063 Uiso 0.411(16) 1 calc PR A 1 C4 C 0.826(4) 0.3691(16) 0.4727(11) 0.045(8) Uani 0.411(16) 1 d P A 1 H4A H 0.8035 0.4155 0.4754 0.054 Uiso 0.411(16) 1 calc PR A 1 H4B H 0.7988 0.3567 0.4426 0.054 Uiso 0.411(16) 1 calc PR A 1 C5 C 0.552(3) 0.3303(14) 0.4892(8) 0.035(6) Uani 0.411(16) 1 d PU A 1 H5A H 0.5271 0.3164 0.4594 0.042 Uiso 0.411(16) 1 calc PR A 1 H5B H 0.4930 0.3717 0.4932 0.042 Uiso 0.411(16) 1 calc PR A 1 C6 C 0.486(4) 0.2793(15) 0.5204(10) 0.047(8) Uani 0.411(16) 1 d P A 1 H6A H 0.5450 0.2377 0.5166 0.056 Uiso 0.411(16) 1 calc PR A 1 H6B H 0.3580 0.2733 0.5159 0.056 Uiso 0.411(16) 1 calc PR A 1 C1' C 1.053(3) 0.4583(8) 0.5581(6) 0.044(5) Uani 0.589(16) 1 d P A 2 H1'A H 0.9510 0.4752 0.5403 0.052 Uiso 0.589(16) 1 calc PR A 2 H1'B H 1.1231 0.4952 0.5691 0.052 Uiso 0.589(16) 1 calc PR A 2 C2' C 1.166(3) 0.4165(9) 0.5301(7) 0.055(6) Uani 0.589(16) 1 d P A 2 H2'A H 1.2122 0.4430 0.5074 0.066 Uiso 0.589(16) 1 calc PR A 2 H2'B H 1.2675 0.3990 0.5478 0.066 Uiso 0.589(16) 1 calc PR A 2 C3' C 0.981(3) 0.3790(12) 0.4721(6) 0.048(5) Uani 0.589(16) 1 d P A 2 H3'A H 1.0661 0.3756 0.4500 0.057 Uiso 0.589(16) 1 calc PR A 2 H3'B H 0.9344 0.4232 0.4715 0.057 Uiso 0.589(16) 1 calc PR A 2 C4' C 0.840(3) 0.3352(13) 0.4626(7) 0.049(6) Uani 0.589(16) 1 d P A 2 H4'A H 0.7641 0.3524 0.4385 0.059 Uiso 0.589(16) 1 calc PR A 2 H4'B H 0.8892 0.2942 0.4533 0.059 Uiso 0.589(16) 1 calc PR A 2 C5' C 0.570(3) 0.3002(11) 0.4899(7) 0.048(5) Uani 0.589(16) 1 d PU A 2 H5'A H 0.5784 0.2531 0.4876 0.057 Uiso 0.589(16) 1 calc PR A 2 H5'B H 0.5173 0.3160 0.4623 0.057 Uiso 0.589(16) 1 calc PR A 2 C6' C 0.450(3) 0.3140(14) 0.5214(8) 0.060(7) Uani 0.589(16) 1 d P A 2 H6'A H 0.3536 0.2821 0.5190 0.072 Uiso 0.589(16) 1 calc PR A 2 H6'B H 0.3973 0.3566 0.5155 0.072 Uiso 0.589(16) 1 calc PR A 2 C7 C 0.5021(14) 0.2371(5) 0.5989(4) 0.054(3) Uani 1 1 d . . . H7A H 0.3742 0.2324 0.6013 0.065 Uiso 1 1 calc R A . H7B H 0.5417 0.2021 0.5808 0.065 Uiso 1 1 calc R . . C8 C 0.5929(15) 0.2335(6) 0.6407(4) 0.063(3) Uani 1 1 d . A . H8A H 0.5531 0.2687 0.6587 0.076 Uiso 1 1 calc R . . H8B H 0.5644 0.1925 0.6543 0.076 Uiso 1 1 calc R . . C9 C 0.8794(15) 0.2355(6) 0.6766(4) 0.057(3) Uani 1 1 d . . . H9A H 0.8464 0.1975 0.6929 0.068 Uiso 1 1 calc R A . H9B H 0.8582 0.2741 0.6936 0.068 Uiso 1 1 calc R . . C10 C 1.0675(15) 0.2318(6) 0.6678(4) 0.063(3) Uani 1 1 d . A . H10A H 1.1398 0.2335 0.6951 0.075 Uiso 1 1 calc R . . H10B H 1.0899 0.1901 0.6543 0.075 Uiso 1 1 calc R . . C12 C 1.079(4) 0.3847(12) 0.6647(10) 0.040(8) Uani 0.411(16) 1 d P A 1 H12A H 1.1418 0.4223 0.6774 0.048 Uiso 0.411(16) 1 calc PR A 1 H12B H 0.9882 0.3718 0.6839 0.048 Uiso 0.411(16) 1 calc PR A 1 C11 C 1.210(4) 0.3292(18) 0.6608(13) 0.040(9) Uani 0.411(16) 1 d P A 1 H11A H 1.3090 0.3427 0.6442 0.048 Uiso 0.411(16) 1 calc PR A 1 H11B H 1.2583 0.3152 0.6893 0.048 Uiso 0.411(16) 1 calc PR A 1 C11' C 1.136(4) 0.3483(14) 0.6653(6) 0.050(8) Uani 0.589(16) 1 d P A 2 H11C H 1.0263 0.3572 0.6791 0.060 Uiso 0.589(16) 1 calc PR A 2 H11D H 1.2339 0.3467 0.6876 0.060 Uiso 0.589(16) 1 calc PR A 2 C12' C 1.168(2) 0.3997(9) 0.6344(6) 0.050(5) Uani 0.589(16) 1 d P A 2 H12C H 1.2569 0.3866 0.6147 0.060 Uiso 0.589(16) 1 calc PR A 2 H12D H 1.2071 0.4397 0.6490 0.060 Uiso 0.589(16) 1 calc PR A 2 C13 C 0.8926(17) 0.9916(7) 0.5789(5) 0.089(5) Uani 1 1 d . B . H13A H 0.8315 1.0333 0.5759 0.107 Uiso 1 1 calc R . . H13B H 1.0176 0.9982 0.5737 0.107 Uiso 1 1 calc R . . C14 C 0.8108(18) 0.9445(6) 0.5475(5) 0.074(4) Uani 1 1 d . . . H14A H 0.8274 0.9587 0.5181 0.088 Uiso 1 1 calc R B . H14B H 0.8658 0.9019 0.5518 0.088 Uiso 1 1 calc R . . C15 C 0.5351(17) 0.8994(6) 0.5271(4) 0.068(3) Uani 1 1 d . . . H15A H 0.5795 0.8552 0.5311 0.082 Uiso 1 1 calc R B . H15B H 0.5444 0.9118 0.4971 0.082 Uiso 1 1 calc R . . C16 C 0.3487(17) 0.9033(6) 0.5383(4) 0.066(3) Uani 1 1 d . B . H16A H 0.3023 0.9464 0.5311 0.080 Uiso 1 1 calc R . . H16B H 0.2779 0.8719 0.5210 0.080 Uiso 1 1 calc R . . C17 C 0.3228(16) 0.8265(6) 0.5924(6) 0.084(5) Uani 1 1 d . B . H17A H 0.4298 0.8050 0.5835 0.100 Uiso 1 1 calc R . . H17B H 0.2202 0.8067 0.5765 0.100 Uiso 1 1 calc R . . C18 C 0.3098(17) 0.8170(6) 0.6371(5) 0.079(4) Uani 1 1 d . B . H18A H 0.2998 0.7708 0.6431 0.094 Uiso 1 1 calc R . . H18B H 0.2030 0.8385 0.6460 0.094 Uiso 1 1 calc R . . C19 C 0.394(4) 0.8600(14) 0.7136(9) 0.061(8) Uani 0.48(2) 1 d PU B 1 H19A H 0.3419 0.8185 0.7211 0.074 Uiso 0.48(2) 1 calc PR B 1 H19B H 0.4807 0.8719 0.7370 0.074 Uiso 0.48(2) 1 calc PR B 1 C20 C 0.261(3) 0.9060(10) 0.7111(8) 0.038(5) Uani 0.48(2) 1 d PU B 1 H20A H 0.2076 0.9086 0.7388 0.046 Uiso 0.48(2) 1 calc PR B 1 H20B H 0.1678 0.8928 0.6893 0.046 Uiso 0.48(2) 1 calc PR B 1 C21 C 0.402(3) 1.0024(12) 0.7370(9) 0.051(7) Uani 0.48(2) 1 d P B 1 H21A H 0.4705 0.9708 0.7548 0.061 Uiso 0.48(2) 1 calc PR B 1 H21B H 0.3089 1.0209 0.7535 0.061 Uiso 0.48(2) 1 calc PR B 1 C22 C 0.522(4) 1.0551(14) 0.7198(10) 0.059(8) Uani 0.48(2) 1 d PU B 1 H22A H 0.4490 1.0849 0.7017 0.071 Uiso 0.48(2) 1 calc PR B 1 H22B H 0.5769 1.0797 0.7440 0.071 Uiso 0.48(2) 1 calc PR B 1 C23 C 0.865(3) 1.0396(14) 0.6971(9) 0.049(7) Uani 0.48(2) 1 d P B 1 H23A H 0.8863 1.0861 0.6945 0.059 Uiso 0.48(2) 1 calc PR B 1 H23B H 0.9135 1.0264 0.7257 0.059 Uiso 0.48(2) 1 calc PR B 1 C24 C 0.940(4) 1.0142(16) 0.6729(11) 0.073(9) Uani 0.48(2) 1 d PU B 1 H24A H 1.0336 0.9913 0.6900 0.088 Uiso 0.48(2) 1 calc PR B 1 H24B H 0.9994 1.0490 0.6583 0.088 Uiso 0.48(2) 1 calc PR B 1 C19' C 0.467(5) 0.8772(17) 0.7192(11) 0.095(10) Uani 0.52(2) 1 d PU B 2 H19C H 0.4434 0.8394 0.7368 0.113 Uiso 0.52(2) 1 calc PR B 2 H19D H 0.5775 0.8966 0.7313 0.113 Uiso 0.52(2) 1 calc PR B 2 C20' C 0.316(4) 0.9267(14) 0.7245(10) 0.072(8) Uani 0.52(2) 1 d PU B 2 H20C H 0.2006 0.9061 0.7177 0.086 Uiso 0.52(2) 1 calc PR B 2 H20D H 0.3197 0.9417 0.7544 0.086 Uiso 0.52(2) 1 calc PR B 2 C21' C 0.387(3) 1.0392(14) 0.7174(10) 0.065(7) Uani 0.52(2) 1 d PU B 2 H21C H 0.3221 1.0466 0.7431 0.079 Uiso 0.52(2) 1 calc PR B 2 H21D H 0.3515 1.0730 0.6966 0.079 Uiso 0.52(2) 1 calc PR B 2 C22' C 0.584(4) 1.0451(14) 0.7295(9) 0.063(8) Uani 0.52(2) 1 d PU B 2 H22C H 0.6144 1.0895 0.7379 0.075 Uiso 0.52(2) 1 calc PR B 2 H22D H 0.6194 1.0162 0.7534 0.075 Uiso 0.52(2) 1 calc PR B 2 C23' C 0.793(5) 1.0562(15) 0.6851(11) 0.070(9) Uani 0.52(2) 1 d PU B 2 H23C H 0.8643 1.0603 0.7124 0.084 Uiso 0.52(2) 1 calc PR B 2 H23D H 0.7511 1.0999 0.6780 0.084 Uiso 0.52(2) 1 calc PR B 2 C24' C 0.924(3) 1.0431(11) 0.6536(8) 0.050(6) Uani 0.52(2) 1 d PU B 2 H24C H 1.0443 1.0449 0.6673 0.060 Uiso 0.52(2) 1 calc PR B 2 H24D H 0.9138 1.0751 0.6304 0.060 Uiso 0.52(2) 1 calc PR B 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 0.0769(3) 0.0467(3) 0.0497(3) -0.0047(2) 0.0048(2) -0.0194(2) Hg2 0.0742(3) 0.0489(3) 0.0648(3) -0.0026(2) 0.0052(3) -0.0211(2) I1 0.0465(4) 0.0351(3) 0.0585(5) -0.0108(3) -0.0005(3) 0.0080(3) I2 0.0529(4) 0.0390(4) 0.0561(5) 0.0079(3) 0.0048(3) -0.0015(3) I3 0.0484(4) 0.0635(5) 0.0528(5) 0.0070(4) 0.0122(3) 0.0097(3) I4 0.1090(8) 0.0987(7) 0.0505(6) -0.0310(5) 0.0097(5) -0.0356(6) I5 0.0369(3) 0.0364(3) 0.0527(4) -0.0065(3) 0.0095(3) -0.0023(3) I6 0.0431(4) 0.0454(4) 0.1027(7) -0.0059(4) 0.0260(4) -0.0042(3) I7 0.0460(4) 0.0913(6) 0.0648(6) -0.0167(5) 0.0078(4) -0.0212(4) I8 0.0514(4) 0.0458(4) 0.0875(6) 0.0091(4) 0.0115(4) -0.0114(3) Cd1 0.0282(3) 0.0386(4) 0.0666(6) -0.0203(4) 0.0077(3) -0.0017(3) Cd2 0.0382(4) 0.0501(4) 0.0406(5) 0.0019(3) 0.0025(3) 0.0020(3) S1 0.0325(13) 0.0470(15) 0.109(3) -0.0391(17) -0.0047(15) 0.0080(11) S2 0.0324(12) 0.0471(14) 0.0560(17) 0.0050(13) 0.0117(11) 0.0019(10) S3 0.0399(15) 0.094(2) 0.080(2) -0.027(2) 0.0073(15) 0.0041(15) S4 0.0607(18) 0.074(2) 0.060(2) 0.0215(17) 0.0149(15) 0.0137(16) O1 0.027(6) 0.027(6) 0.027(6) -0.0001(10) 0.0019(11) -0.0001(10) O2 0.026(7) 0.026(7) 0.026(7) 0.0000(10) 0.0018(11) 0.0000(10) O1' 0.049(8) 0.024(6) 0.056(13) -0.001(8) 0.022(9) -0.010(5) O2' 0.031(10) 0.076(19) 0.060(13) -0.010(12) 0.010(8) 0.006(10) O3 0.035(4) 0.055(4) 0.057(5) 0.000(4) 0.001(3) -0.004(3) O4 0.050(4) 0.067(5) 0.054(5) -0.009(4) 0.005(4) -0.009(4) O5 0.059(5) 0.072(5) 0.064(6) -0.022(4) 0.023(4) -0.006(4) O6 0.068(5) 0.047(4) 0.061(5) 0.008(4) 0.005(4) -0.010(4) O7 0.066(5) 0.091(6) 0.050(5) -0.007(5) 0.005(4) 0.013(5) O8 0.060(5) 0.113(7) 0.049(5) -0.028(5) -0.001(4) 0.029(5) C1 0.021(5) 0.021(5) 0.021(5) 0.0001(10) 0.0017(11) -0.0001(10) C2 0.013(4) 0.013(4) 0.013(4) 0.0002(10) 0.0011(11) -0.0001(10) C3 0.052(10) 0.052(10) 0.052(10) 0.0000(10) 0.0039(12) 0.0001(10) C4 0.050(18) 0.05(2) 0.030(18) 0.008(16) 0.007(13) 0.006(17) C5 0.035(6) 0.035(6) 0.035(6) -0.0001(10) 0.0024(11) 0.0001(10) C6 0.027(14) 0.054(19) 0.059(19) -0.019(16) -0.007(12) 0.024(13) C1' 0.067(12) 0.032(9) 0.033(11) -0.013(9) 0.009(9) -0.011(8) C2' 0.044(11) 0.048(11) 0.077(15) 0.003(10) 0.026(10) -0.001(9) C3' 0.042(11) 0.073(15) 0.031(11) -0.010(11) 0.017(9) -0.021(11) C4' 0.043(11) 0.070(17) 0.035(13) 0.004(12) 0.012(9) -0.004(12) C5' 0.048(5) 0.048(5) 0.048(5) -0.0001(10) 0.0032(11) -0.0001(10) C6' 0.025(10) 0.10(2) 0.061(14) 0.009(15) 0.014(9) 0.016(12) C7 0.036(5) 0.036(5) 0.090(10) -0.001(6) -0.002(6) -0.001(4) C8 0.052(7) 0.064(7) 0.075(9) 0.014(7) 0.014(6) -0.021(6) C9 0.060(7) 0.062(7) 0.049(7) 0.016(6) 0.005(6) -0.017(6) C10 0.049(7) 0.055(7) 0.082(10) 0.013(7) -0.008(6) 0.003(5) C12 0.045(15) 0.018(13) 0.06(2) -0.007(13) 0.008(13) 0.005(11) C11 0.021(15) 0.041(17) 0.05(2) 0.000(13) -0.004(14) 0.000(13) C11' 0.06(2) 0.08(3) 0.009(9) -0.003(14) -0.004(13) -0.034(17) C12' 0.045(10) 0.065(12) 0.042(11) 0.000(9) 0.013(8) -0.011(9) C13 0.052(7) 0.085(10) 0.136(15) 0.000(10) 0.037(9) -0.019(7) C14 0.082(9) 0.074(8) 0.071(9) 0.004(7) 0.043(8) -0.003(7) C15 0.083(9) 0.074(8) 0.047(8) -0.013(6) -0.003(7) -0.005(7) C16 0.078(9) 0.078(8) 0.042(7) -0.002(6) -0.011(6) -0.025(7) C17 0.046(7) 0.070(9) 0.132(15) 0.024(9) -0.015(8) -0.017(6) C18 0.063(8) 0.064(8) 0.111(13) 0.033(8) 0.023(8) -0.008(6) C19 0.061(8) 0.061(8) 0.061(8) 0.0002(10) 0.0044(12) 0.0000(10) C20 0.038(5) 0.038(5) 0.038(6) 0.0001(10) 0.0031(11) -0.0002(10) C21 0.058(14) 0.046(15) 0.050(16) -0.012(12) 0.010(12) 0.005(11) C22 0.059(8) 0.059(8) 0.059(8) -0.0002(10) 0.0042(12) 0.0001(10) C23 0.034(12) 0.061(16) 0.052(16) 0.003(13) -0.003(12) -0.009(11) C24 0.073(9) 0.073(9) 0.073(9) -0.0001(10) 0.0052(12) -0.0002(10) C19' 0.094(10) 0.094(10) 0.095(10) 0.0000(10) 0.0067(12) 0.0000(10) C20' 0.072(8) 0.072(8) 0.072(8) 0.0001(10) 0.0053(12) -0.0001(10) C21' 0.065(7) 0.066(7) 0.065(7) -0.0001(10) 0.0048(11) 0.0002(10) C22' 0.063(8) 0.063(8) 0.063(8) -0.0002(10) 0.0046(12) 0.0003(10) C23' 0.070(9) 0.070(9) 0.070(9) -0.0001(10) 0.0050(12) -0.0002(10) C24' 0.050(6) 0.050(6) 0.050(6) 0.0000(10) 0.0034(11) -0.0001(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 I4 2.6777(10) . ? Hg1 I3 2.6947(9) . ? Hg1 I6 2.8246(8) . ? Hg1 I5 2.9999(8) . ? Hg2 I7 2.6972(10) . ? Hg2 I8 2.7119(9) . ? Hg2 I5 2.8476(8) . ? Hg2 I6 3.0175(9) . ? I1 Cd1 2.6801(9) . ? I2 Cd2 2.6902(10) . ? Cd1 O1 2.34(2) . ? Cd1 S1 2.592(3) . ? Cd1 O2' 2.63(4) . ? Cd1 O2 2.65(4) . ? Cd1 S2 2.659(2) . ? Cd2 O8 2.557(8) . ? Cd2 O6 2.577(8) . ? Cd2 S4 2.612(3) . ? Cd2 S3 2.671(3) . ? S1 C1 1.603(18) . ? S1 C12' 1.725(19) . ? S1 C12 2.00(3) . ? S1 C1' 2.037(18) . ? S2 C7 1.799(11) . ? S2 C6' 1.81(2) . ? S2 C6 1.90(3) . ? S3 C24 1.76(3) . ? S3 C13 1.809(16) . ? S3 C24' 1.89(2) . ? S4 C19 1.75(3) . ? S4 C19' 1.78(3) . ? S4 C18 1.833(15) . ? O1 C3 1.35(5) . ? O1 C2 1.44(3) . ? O2 C5 1.32(5) . ? O2 C4 1.36(6) . ? O1' C2' 1.38(2) . ? O1' C3' 1.41(3) . ? O2' C4' 1.33(4) . ? O2' C5' 1.39(4) . ? O3 C9 1.400(13) . ? O3 C8 1.432(13) . ? O4 C11 1.34(4) . ? O4 C10 1.422(14) . ? O4 C11' 1.59(3) . ? O5 C14 1.389(15) . ? O5 C15 1.400(14) . ? O6 C17 1.388(14) . ? O6 C16 1.428(14) . ? O7 C20' 1.32(3) . ? O7 C21 1.39(2) . ? O7 C21' 1.49(3) . ? O7 C20 1.62(2) . ? O8 C23' 1.21(3) . ? O8 C22' 1.34(3) . ? O8 C22 1.48(3) . ? O8 C23 1.56(3) . ? C1 C2 1.52(3) . ? C3 C4 1.56(5) . ? C5 C6 1.56(4) . ? C1' C2' 1.55(3) . ? C3' C4' 1.43(3) . ? C5' C6' 1.43(3) . ? C7 C8 1.446(17) . ? C9 C10 1.484(16) . ? C12 C11 1.55(3) . ? C11' C12' 1.48(3) . ? C13 C14 1.50(2) . ? C15 C16 1.494(18) . ? C17 C18 1.43(2) . ? C19 C20 1.40(3) . ? C21 C22 1.56(4) . ? C23 C24 1.12(4) . ? C19' C20' 1.57(4) . ? C21' C22' 1.53(4) . ? C23' C24' 1.49(4) . ? 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 I4 Hg1 I3 120.18(3) . . ? I4 Hg1 I6 113.64(3) . . ? I3 Hg1 I6 114.12(3) . . ? I4 Hg1 I5 106.42(3) . . ? I3 Hg1 I5 104.19(3) . . ? I6 Hg1 I5 93.77(2) . . ? I7 Hg2 I8 118.13(3) . . ? I7 Hg2 I5 109.77(3) . . ? I8 Hg2 I5 115.29(3) . . ? I7 Hg2 I6 111.10(3) . . ? I8 Hg2 I6 106.63(3) . . ? I5 Hg2 I6 92.93(2) . . ? Hg2 I5 Hg1 84.50(2) . . ? Hg1 I6 Hg2 84.57(2) . . ? O1 Cd1 S1 68.9(6) . . ? O1 Cd1 O2' 65.3(9) . . ? S1 Cd1 O2' 108.5(7) . . ? O1 Cd1 O2 65.5(11) . . ? S1 Cd1 O2 102.9(8) . . ? O2' Cd1 O2 6.7(12) . . ? O1 Cd1 S2 122.5(6) . . ? S1 Cd1 S2 93.96(8) . . ? O2' Cd1 S2 70.1(6) . . ? O2 Cd1 S2 66.1(8) . . ? O1 Cd1 I1 96.7(6) . . ? S1 Cd1 I1 149.09(6) . . ? O2' Cd1 I1 88.0(6) . . ? O2 Cd1 I1 94.7(8) . . ? S2 Cd1 I1 116.49(6) . . ? O8 Cd2 O6 166.3(3) . . ? O8 Cd2 S4 101.6(2) . . ? O6 Cd2 S4 71.46(18) . . ? O8 Cd2 S3 70.2(2) . . ? O6 Cd2 S3 121.38(19) . . ? S4 Cd2 S3 94.61(11) . . ? O8 Cd2 I2 90.6(2) . . ? O6 Cd2 I2 90.48(17) . . ? S4 Cd2 I2 150.19(8) . . ? S3 Cd2 I2 115.16(9) . . ? C1 S1 C12' 62.2(9) . . ? C1 S1 C12 99.7(11) . . ? C12' S1 C12 38.3(10) . . ? C1 S1 C1' 33.1(8) . . ? C12' S1 C1' 95.2(8) . . ? C12 S1 C1' 132.0(10) . . ? C1 S1 Cd1 106.3(7) . . ? C12' S1 Cd1 106.1(7) . . ? C12 S1 Cd1 104.5(7) . . ? C1' S1 Cd1 99.6(5) . . ? C7 S2 C6' 108.6(10) . . ? C7 S2 C6 90.4(11) . . ? C6' S2 C6 24.1(9) . . ? C7 S2 Cd1 99.0(3) . . ? C6' S2 Cd1 107.1(6) . . ? C6 S2 Cd1 95.4(9) . . ? C24 S3 C13 114.1(14) . . ? C24 S3 C24' 26.9(11) . . ? C13 S3 C24' 88.5(9) . . ? C24 S3 Cd2 102.3(11) . . ? C13 S3 Cd2 98.2(5) . . ? C24' S3 Cd2 98.9(6) . . ? C19 S4 C19' 22.2(13) . . ? C19 S4 C18 93.6(12) . . ? C19' S4 C18 115.2(14) . . ? C19 S4 Cd2 106.7(10) . . ? C19' S4 Cd2 96.4(12) . . ? C18 S4 Cd2 101.0(4) . . ? C3 O1 C2 115(2) . . ? C3 O1 Cd1 113(2) . . ? C2 O1 Cd1 119.4(14) . . ? C5 O2 C4 122(4) . . ? C5 O2 Cd1 125(3) . . ? C4 O2 Cd1 113(3) . . ? C2' O1' C3' 116.3(16) . . ? C4' O2' C5' 124(3) . . ? C4' O2' Cd1 119(2) . . ? C5' O2' Cd1 112(2) . . ? C9 O3 C8 115.3(9) . . ? C11 O4 C10 115.2(19) . . ? C11 O4 C11' 26.6(11) . . ? C10 O4 C11' 111.9(11) . . ? C14 O5 C15 115.2(9) . . ? C17 O6 C16 114.0(11) . . ? C17 O6 Cd2 116.9(8) . . ? C16 O6 Cd2 113.5(6) . . ? C20' O7 C21 80.4(18) . . ? C20' O7 C21' 119.3(19) . . ? C21 O7 C21' 39.9(12) . . ? C20' O7 C20 25.9(15) . . ? C21 O7 C20 105.8(15) . . ? C21' O7 C20 142.8(16) . . ? C23' O8 C22' 120(2) . . ? C23' O8 C22 126(2) . . ? C22' O8 C22 23.0(16) . . ? C23' O8 C23 27.0(17) . . ? C22' O8 C23 114.8(17) . . ? C22 O8 C23 131.7(17) . . ? C23' O8 Cd2 111.6(17) . . ? C22' O8 Cd2 126.1(14) . . ? C22 O8 Cd2 110.0(14) . . ? C23 O8 Cd2 118.0(10) . . ? C2 C1 S1 102.7(13) . . ? O1 C2 C1 107.7(16) . . ? O1 C3 C4 109(3) . . ? O2 C4 C3 109(3) . . ? O2 C5 C6 106(3) . . ? C5 C6 S2 104.6(19) . . ? C2' C1' S1 112.5(12) . . ? O1' C2' C1' 110.1(16) . . ? O1' C3' C4' 111.9(19) . . ? O2' C4' C3' 115(2) . . ? O2' C5' C6' 120(2) . . ? C5' C6' S2 114.0(16) . . ? C8 C7 S2 109.2(8) . . ? O3 C8 C7 110.5(10) . . ? O3 C9 C10 108.7(10) . . ? O4 C10 C9 113.1(9) . . ? C11 C12 S1 111(3) . . ? O4 C11 C12 106(2) . . ? C12' C11' O4 109.2(15) . . ? C11' C12' S1 102.2(14) . . ? C14 C13 S3 108.4(9) . . ? O5 C14 C13 107.3(10) . . ? O5 C15 C16 107.6(10) . . ? O6 C16 C15 112.5(10) . . ? O6 C17 C18 111.5(13) . . ? C17 C18 S4 110.5(9) . . ? C20 C19 S4 115(2) . . ? C19 C20 O7 111.8(19) . . ? O7 C21 C22 100(2) . . ? O8 C22 C21 113(2) . . ? C24 C23 O8 116(2) . . ? C23 C24 S3 132(3) . . ? C20' C19' S4 119(2) . . ? O7 C20' C19' 110(2) . . ? O7 C21' C22' 114(2) . . ? O8 C22' C21' 105(2) . . ? O8 C23' C24' 133(3) . . ? C23' C24' S3 106.5(17) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.626 _refine_diff_density_min -1.940 _refine_diff_density_rms 0.294