Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-10-12 _audit_update_record ? _journal_coden_Cambridge 182 loop_ _publ_author_name 'Hosseini, M.' 'Akdas, Huriey' 'Bilyk, Alex' 'De Cian, Andre' 'Graf, Ernest' 'Harrowfield, Jack M.' 'Koutsantonis, George A.' 'Murray, Ian' 'Skelton, Brian W.' 'White, Allan H.' _publ_contact_author_name 'Prof M Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur 4 rue Blaise Pascal 67000 Strasbourg FRANCE ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_section_title ; Koilands from Thiophiles: Mercury (II) Clusters ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; data_st930 _database_code_CSD 178503 _audit_creation_method Xtal3.6 _audit_creation_date 00-10-12 _audit_update_record ? _journal_coden_Cambridge 182 loop_ _publ_author_name 'Hosseini, M.' 'Akdas, Huriey' 'Bilyk, Alex' 'De Cian, Andre' 'Graf, Ernest' 'Harrowfield, Jack M.' 'Koutsantonis, George A.' 'Murray, Ian' 'Skelton, Brian W.' 'White, Allan H.' _publ_contact_author_name 'Prof M Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur 4 rue Blaise Pascal 67000 Strasbourg FRANCE ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_section_title ; Koilands from Thiophiles: Mercury (II) Clusters ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C183 H207 Cl9 Hg9 O3 S36' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C183 H207 Cl9 Hg9 O3 S36' _chemical_formula_weight 5972.14 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Hg ? -3.084 9.223 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 S ? 0.110 0.124 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P -3 c 1' _symmetry_space_group_name_Hall '-P 3 2 c' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -y,+x-y,+z -x+y,-x,+z +y,+x,1/2-z +x-y,-y,1/2-z -x,-x+y,1/2-z -x,-y,-z +y,-x+y,-z +x-y,+x,-z -y,-x,1/2+z -x+y,+y,1/2+z +x,+x-y,1/2+z _cell_length_a 22.0184(2) _cell_length_b 22.0184(2) _cell_length_c 51.6679(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 21693.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 31519 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 17364 _exptl_absorpt_coefficient_mu 6.923 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.234 _exptl_absorpt_correction_T_max 0.330 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 31519 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 77. mm. Scan angle = 0.3 deg 1 scans of 60 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.90 Omega = 0.00 Kappa = 0.00 581 frames Friedel pairs were not averaged. Internal R = 0.03 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31519 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -65 _diffrn_reflns_limit_l_max 65 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.48 _reflns_number_total 17133 _reflns_number_gt 6062 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6062 _refine_ls_number_parameters 626 _refine_ls_number_restraints -8 _refine_ls_number_constraints 39 _refine_ls_R_factor_all 0.184 _refine_ls_R_factor_gt 0.064 _refine_ls_wR_factor_all 0.587 _refine_ls_wR_factor_ref 0.081 _refine_ls_goodness_of_fit_all 52.143 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_shift/su_max 0.028 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 1.138 _refine_diff_density_min -1.171 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol HG1 0.34458(4) 0.77417(4) 0.12137(2) 0.0472 1.000 Uani ? ? Hg HG2 0.34879(4) 0.77820(4) 0.04593(2) 0.0463 1.000 Uani ? ? Hg S1 0.2564(3) 0.7578(3) 0.0905(1) 0.051(3) 1.000 Uani ? ? S S2 0.2753(3) 0.8576(3) 0.0409(1) 0.054(3) 1.000 Uani ? ? S S3 0.2560(3) 0.7057(3) 0.0171(1) 0.049(3) 1.000 Uani ? ? S S4 0.0963(3) 0.5698(3) 0.0208(1) 0.051(3) 1.000 Uani ? ? S S5 0.4424(3) 0.8344(3) 0.0772(1) 0.047(3) 1.000 Uani ? ? S S6 0.4490(3) 0.9267(3) 0.1267(1) 0.054(3) 1.000 Uani ? ? S S7 0.4272(3) 0.7761(3) 0.1516(1) 0.043(3) 1.000 Uani ? ? S S8 0.2462(3) 0.8109(3) 0.1475(1) 0.051(3) 1.000 Uani ? ? S C1 0.251(1) 0.8596(9) 0.1196(4) 0.05(1) 1.000 Uani ? ? C C2 0.248(1) 0.919(1) 0.1226(4) 0.05(1) 1.000 Uani ? ? C C3 0.2518(9) 0.9592(9) 0.1013(4) 0.09(2) 1.000 Uani ? ? C C4 0.259(1) 0.939(1) 0.0767(4) 0.07(1) 1.000 Uani ? ? C C5 0.263(1) 0.8787(9) 0.0728(4) 0.05(1) 1.000 Uani ? ? C C6 0.257(1) 0.837(1) 0.0945(5) 0.07(1) 1.000 Uani ? ? C C7 0.2516(9) 1.0232(9) 0.1035(4) 0.19(1) 1.000 Uiso ? ? C C8 0.3086(9) 1.0750(9) 0.1294(4) 0.1969 1.000 Uiso ? ? C C9 0.2027(9) 1.0200(9) 0.1259(4) 0.1969 1.000 Uiso ? ? C C10 0.2398(9) 1.0623(9) 0.0760(4) 0.1969 1.000 Uiso ? ? C C11 0.194(1) 0.783(1) 0.0346(4) 0.06(1) 1.000 Uani ? ? C C12 0.133(1) 0.789(1) 0.0350(4) 0.06(1) 1.000 Uani ? ? C C13 0.069(1) 0.737(1) 0.0301(4) 0.06(1) 1.000 Uani ? ? C C14 0.058(1) 0.668(1) 0.0259(4) 0.06(1) 1.000 Uani ? ? C C15 0.116(1) 0.658(1) 0.0253(4) 0.05(1) 1.000 Uani ? ? C C16 0.184(1) 0.717(1) 0.0278(4) 0.04(1) 1.000 Uani ? ? C C17 0.006(1) 0.750(1) 0.0237(5) 0.08(1) 1.000 Uani ? ? C C18 0.018(2) 0.820(2) 0.0370(9) 0.19(3) 1.000 Uani ? ? C C19 -0.065(1) 0.686(2) 0.0305(6) 0.11(2) 1.000 Uani ? ? C C20 0.007(1) 0.757(1) -0.0059(6) 0.10(2) 1.000 Uani ? ? C C21 0.047(1) 0.527(1) 0.0486(4) 0.05(1) 1.000 Uani ? ? C C22 -0.023(1) 0.479(1) 0.0460(5) 0.07(2) 1.000 Uani ? ? C C23 -0.0647(8) 0.4387(9) 0.0681(3) 0.07(2) 1.000 Uani ? ? C C24 -0.031(1) 0.453(1) 0.0914(4) 0.06(1) 1.000 Uani ? ? C C25 0.468(1) 0.964(1) 0.0947(4) 0.05(1) 1.000 Uani ? ? C C26 0.462(1) 0.921(1) 0.0734(4) 0.05(1) 1.000 Uani ? ? C C27 -0.1510(8) 0.3806(9) 0.0639(3) 0.152(8) 1.000 Uiso ? ? C C28 -0.1801(8) 0.4200(9) 0.0502(3) 0.1517 1.000 Uiso ? ? C C29 -0.1479(8) 0.3225(9) 0.0425(3) 0.1517 1.000 Uiso ? ? C C30 -0.1771(8) 0.3588(9) 0.0887(3) 0.1517 1.000 Uiso ? ? C C31 0.518(1) 0.910(1) 0.1312(4) 0.04(1) 1.000 Uani ? ? C C32 0.588(1) 0.962(1) 0.1268(5) 0.05(1) 1.000 Uani ? ? C C33 0.645(1) 0.951(1) 0.1293(5) 0.04(1) 1.000 Uani ? ? C C34 0.634(1) 0.890(1) 0.1351(5) 0.05(1) 1.000 Uani ? ? C C35 0.1677(9) 0.7356(9) 0.1410(4) 0.05(1) 1.000 Uani ? ? C C36 0.509(1) 0.844(1) 0.1401(4) 0.05(1) 1.000 Uani ? ? C C37 0.721(1) 1.013(1) 0.1212(5) 0.06(2) 1.000 Uani ? ? C C38 0.718(2) 1.071(2) 0.1052(7) 0.12(2) 1.000 Uani ? ? C C39 0.755(1) 0.984(2) 0.1010(8) 0.15(2) 1.000 Uani ? ? C C40 0.759(2) 1.033(2) 0.1456(6) 0.12(2) 1.000 Uani ? ? C HG3 0.00203(4) 0.89660(4) 0.21215(2) 0.0391 1.000 Uani ? ? Hg S9 0.0941(2) 0.9243(3) 0.2428(1) 0.040(2) 1.000 Uani ? ? S S10 -0.0870(3) 0.7413(3) 0.2085(1) 0.043(3) 1.000 Uani ? ? S S11 -0.0858(2) 0.8832(3) 0.1825(1) 0.038(3) 1.000 Uani ? ? S S12 -0.1187(3) 0.7644(2) 0.3147(1) 0.041(2) 1.000 Uani ? ? S C41 -0.1176(9) 0.7153(9) 0.2877(4) 0.039(9) 1.000 Uani ? ? C C42 -0.125(1) 0.6519(9) 0.2901(4) 0.05(1) 1.000 Uani ? ? C C43 -0.119(1) 0.615(1) 0.2705(4) 0.06(1) 1.000 Uani ? ? C C44 -0.110(1) 0.642(1) 0.2458(5) 0.07(1) 1.000 Uani ? ? C C45 -0.1012(9) 0.7100(9) 0.2418(4) 0.04(1) 1.000 Uani ? ? C C46 0.1027(9) 0.8501(9) 0.2379(4) 0.035(9) 1.000 Uani ? ? C C47 -0.129(2) 0.541(1) 0.2758(5) 0.10(2) 1.000 Uani ? ? C C48 -0.204(2) 0.495(1) 0.2842(6) 0.11(2) 1.000 Uani ? ? C C49 -0.083(2) 0.544(1) 0.2948(5) 0.12(2) 1.000 Uani ? ? C C50 -0.118(2) 0.509(2) 0.2514(7) 0.19(2) 1.000 Uani ? ? C C51 -0.1649(9) 0.7466(9) 0.2027(3) 0.026(9) 1.000 Uani ? ? C C52 -0.230(1) 0.684(1) 0.2058(4) 0.04(1) 1.000 Uani ? ? C C53 -0.2922(9) 0.6815(9) 0.2014(4) 0.04(1) 1.000 Uani ? ? C C54 -0.2892(9) 0.743(1) 0.1952(4) 0.04(1) 1.000 Uani ? ? C C55 -0.1950(9) 0.7711(9) 0.3077(4) 0.037(9) 1.000 Uani ? ? C C56 -0.1631(9) 0.8075(9) 0.1939(3) 0.030(9) 1.000 Uani ? ? C C57 -0.361(1) 0.612(1) 0.2010(7) 0.10(2) 1.000 Uani ? ? C C58 -0.419(2) 0.620(2) 0.2053(8) 0.16(2) 1.000 Uiso ? ? C C59 -0.358(2) 0.557(2) 0.2132(7) 0.12(1) 1.000 Uiso ? ? C C60 -0.367(3) 0.583(3) 0.172(1) 0.22(2) 1.000 Uiso ? ? C O1 0.3338(6) 0.7412(6) 0.2774(3) 0.046(4) 1.000 Uiso ? ? O C61 0.0000 1.0000 0.124(1) 0.10(2) 0.333 Uiso ? ? C CL1 0.0122(7) 0.9314(7) 0.1169(3) 0.217(7) 1.000 Uiso ? ? Cl C62 1.0000 0.0000 0.055(3) 0.17(7) 0.167 Uiso ? ? C CL2 0.996(1) 0.070(1) 0.0400(5) 0.164(9) 0.500 Uiso ? ? Cl C63 0.5421(6) 0.3250(6) 0.1747(2) 0.24(5) 0.500 Uiso ? ? C CL3 0.5213(6) 0.3965(6) 0.1600(2) 0.155(9) 0.500 Uiso ? ? Cl CL4 0.5450(6) 0.2930(6) 0.1407(2) 0.18(1) 0.500 Uiso ? ? Cl CL5 0.4496(6) 0.2596(6) 0.1784(2) 0.115(6) 0.500 Uiso ? ? Cl H1 0.2445 0.9335 0.1395 0.0761 1.000 Uiso calc C2 H H2 0.2617 0.9674 0.0623 0.0902 1.000 Uiso calc C4 H H3 0.3082 1.1178 0.1307 0.2560 1.000 Uiso calc C8 H H4 0.2928 1.0498 0.1452 0.2560 1.000 Uiso calc C8 H H5 0.3550 1.0847 0.1259 0.2560 1.000 Uiso calc C8 H H6 0.2035 1.0634 0.1270 0.2560 1.000 Uiso calc C9 H H7 0.1562 0.9834 0.1227 0.2560 1.000 Uiso calc C9 H H8 0.2187 1.0112 0.1418 0.2560 1.000 Uiso calc C9 H H9 0.2410 1.1046 0.0807 0.2560 1.000 Uiso calc C10 H H10 0.2762 1.0725 0.0639 0.2560 1.000 Uiso calc C10 H H11 0.1958 1.0312 0.0683 0.2560 1.000 Uiso calc C10 H H12 0.1392 0.8332 0.0391 0.0735 1.000 Uiso calc C12 H H13 0.0116 0.6292 0.0236 0.0883 1.000 Uiso calc C14 H H14 -0.0200 0.8270 0.0330 0.2254 1.000 Uiso calc C18 H H15 0.0214 0.8169 0.0553 0.2254 1.000 Uiso calc C18 H H16 0.0605 0.8588 0.0307 0.2254 1.000 Uiso calc C18 H H17 -0.1012 0.6966 0.0263 0.1457 1.000 Uiso calc C19 H H18 -0.0720 0.6466 0.0209 0.1457 1.000 Uiso calc C19 H H19 -0.0670 0.6766 0.0485 0.1457 1.000 Uiso calc C19 H H20 -0.0305 0.7646 -0.0109 0.1345 1.000 Uiso calc C20 H H21 0.0501 0.7954 -0.0113 0.1345 1.000 Uiso calc C20 H H22 0.0002 0.7151 -0.0138 0.1345 1.000 Uiso calc C20 H H23 -0.0443 0.4708 0.0295 0.1051 1.000 Uiso calc C22 H H24 -0.0561 0.4261 0.1060 0.0917 1.000 Uiso calc C24 H H25 -0.2289 0.3898 0.0473 0.1972 1.000 Uiso calc C28 H H26 -0.1733 0.4586 0.0606 0.1972 1.000 Uiso calc C28 H H27 -0.1568 0.4366 0.0341 0.1972 1.000 Uiso calc C28 H H28 -0.1942 0.2865 0.0385 0.1972 1.000 Uiso calc C29 H H29 -0.1249 0.3465 0.0271 0.1972 1.000 Uiso calc C29 H H30 -0.1227 0.3023 0.0500 0.1972 1.000 Uiso calc C29 H H31 -0.2259 0.3258 0.0878 0.1972 1.000 Uiso calc C30 H H32 -0.1534 0.3377 0.0967 0.1972 1.000 Uiso calc C30 H H33 -0.1700 0.3981 0.0987 0.1972 1.000 Uiso calc C30 H H34 0.5974 1.0076 0.1219 0.0967 1.000 Uiso calc C32 H H35 0.6733 0.8826 0.1354 0.0723 1.000 Uiso calc C34 H H36 0.7647 1.1059 0.1009 0.1641 1.000 Uiso calc C38 H H37 0.6925 1.0507 0.0897 0.1641 1.000 Uiso calc C38 H H38 0.6961 1.0905 0.1150 0.1641 1.000 Uiso calc C38 H H39 0.8004 1.0212 0.0962 0.2014 1.000 Uiso calc C39 H H40 0.7595 0.9474 0.1087 0.2014 1.000 Uiso calc C39 H H41 0.7264 0.9672 0.0861 0.2014 1.000 Uiso calc C39 H H42 0.8054 1.0700 0.1427 0.2250 1.000 Uiso calc C40 H H43 0.7359 1.0478 0.1574 0.2250 1.000 Uiso calc C40 H H44 0.7603 0.9937 0.1527 0.2250 1.000 Uiso calc C40 H H45 -0.1341 0.6314 0.3068 0.0621 1.000 Uiso calc C42 H H46 -0.1104 0.6149 0.2315 0.0783 1.000 Uiso calc C44 H H47 -0.2117 0.4489 0.2876 0.1656 1.000 Uiso calc C48 H H48 -0.2122 0.5135 0.2994 0.1656 1.000 Uiso calc C48 H H49 -0.2342 0.4927 0.2708 0.1656 1.000 Uiso calc C48 H H50 -0.0895 0.4987 0.2978 0.1640 1.000 Uiso calc C49 H H51 -0.0359 0.5745 0.2892 0.1640 1.000 Uiso calc C49 H H52 -0.0908 0.5621 0.3104 0.1640 1.000 Uiso calc C49 H H53 -0.1249 0.4642 0.2552 0.2727 1.000 Uiso calc C50 H H54 -0.1515 0.5050 0.2387 0.2727 1.000 Uiso calc C50 H H55 -0.0723 0.5387 0.2451 0.2727 1.000 Uiso calc C50 H H56 -0.2306 0.6425 0.2110 0.0620 1.000 Uiso calc C52 H H57 -0.3322 0.7428 0.1929 0.0546 1.000 Uiso calc C54 H H58 -0.4600 0.5755 0.2048 0.2106 1.000 Uiso calc C58 H H59 -0.4146 0.6411 0.2217 0.2106 1.000 Uiso calc C58 H H60 -0.4210 0.6492 0.1922 0.2106 1.000 Uiso calc C58 H H61 -0.4025 0.5158 0.2122 0.1605 1.000 Uiso calc C59 H H62 -0.3239 0.5494 0.2048 0.1605 1.000 Uiso calc C59 H H63 -0.3452 0.5687 0.2309 0.1605 1.000 Uiso calc C59 H H64 -0.4098 0.5394 0.1709 0.2896 1.000 Uiso calc C60 H H65 -0.3679 0.6156 0.1604 0.2896 1.000 Uiso calc C60 H H66 -0.3287 0.5767 0.1688 0.2896 1.000 Uiso calc C60 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol HG1 0.0491 0.0516(4) 0.0416(5) 0.0291(3) -0.0008(4) 0.0004(4) Hg HG2 0.0496 0.0491(4) 0.0408(5) 0.0239(3) -0.0010(4) -0.0013(4) Hg S1 0.059(3) 0.054(2) 0.042(3) 0.036(2) -0.002(3) -0.004(2) S S2 0.069(3) 0.056(3) 0.040(3) 0.036(2) -0.003(3) 0.002(3) S S3 0.051(3) 0.058(3) 0.040(3) 0.027(2) -0.001(3) -0.006(3) S S4 0.048(3) 0.064(3) 0.044(3) 0.017(2) -0.003(3) -0.005(3) S S5 0.053(3) 0.048(3) 0.041(3) 0.024(2) -0.001(3) 0.002(3) S S6 0.071(3) 0.045(3) 0.049(4) 0.031(2) 0.002(3) 0.003(3) S S7 0.040(2) 0.053(3) 0.037(3) 0.021(2) 0.001(2) 0.004(3) S S8 0.065(3) 0.051(2) 0.041(3) 0.037(2) -0.007(3) -0.003(2) S C1 0.06(1) 0.036(8) 0.04(1) 0.032(6) -0.01(1) -0.006(9) C C2 0.09(1) 0.06(1) 0.03(1) 0.034(9) 0.01(1) 0.01(1) C C3 0.16(2) 0.06(1) 0.07(2) 0.076(9) 0.00(2) 0.00(1) C C4 0.13(1) 0.08(1) 0.03(1) 0.080(8) -0.00(1) 0.00(1) C C5 0.07(1) 0.048(9) 0.04(1) 0.041(6) -0.01(1) -0.000(9) C C6 0.06(1) 0.07(1) 0.08(2) 0.047(7) -0.02(1) -0.02(1) C C11 0.08(1) 0.09(1) 0.03(1) 0.060(7) 0.02(1) 0.02(1) C C12 0.05(1) 0.08(1) 0.05(1) 0.032(8) -0.02(1) -0.01(1) C C13 0.04(1) 0.08(1) 0.05(1) 0.029(8) 0.00(1) 0.00(1) C C14 0.09(1) 0.07(1) 0.03(1) 0.03(1) -0.02(1) 0.00(1) C C15 0.06(1) 0.07(1) 0.03(1) 0.043(7) -0.017(9) -0.01(1) C C16 0.06(1) 0.07(1) 0.02(1) 0.037(7) 0.009(9) 0.011(9) C C17 0.07(1) 0.12(2) 0.06(2) 0.057(9) -0.00(1) -0.02(1) C C18 0.15(2) 0.21(3) 0.20(4) 0.12(2) -0.09(2) -0.06(3) C C19 0.08(1) 0.22(2) 0.07(2) 0.10(1) 0.00(1) 0.02(2) C C20 0.09(2) 0.13(2) 0.10(2) 0.06(1) -0.03(2) 0.01(2) C C21 0.05(1) 0.05(1) 0.05(1) 0.013(9) -0.01(1) -0.02(1) C C22 0.07(2) 0.08(2) 0.06(2) 0.02(1) -0.01(1) 0.01(1) C C23 0.04(1) 0.13(2) 0.06(2) 0.01(1) -0.00(1) -0.03(2) C C24 0.06(1) 0.07(2) 0.04(1) 0.00(1) -0.00(1) 0.00(1) C C25 0.07(1) 0.05(1) 0.05(1) 0.027(8) -0.01(1) -0.00(1) C C26 0.06(1) 0.05(1) 0.03(1) 0.025(8) -0.00(1) 0.01(1) C C31 0.05(1) 0.06(1) 0.03(1) 0.033(7) 0.003(9) -0.002(9) C C32 0.06(2) 0.02(1) 0.09(2) -0.02(1) 0.02(2) 0.01(1) C C33 0.013(9) 0.07(1) 0.10(2) 0.010(8) -0.00(1) -0.00(1) C C34 0.06(1) 0.03(1) 0.06(1) 0.011(8) -0.01(1) 0.02(1) C C35 0.067(9) 0.055(8) 0.04(1) 0.049(6) 0.013(9) 0.012(9) C C36 0.06(1) 0.05(1) 0.04(1) 0.024(8) -0.01(1) -0.00(1) C C37 0.06(1) 0.05(1) 0.09(2) -0.00(1) -0.01(1) 0.02(1) C C38 0.08(2) 0.11(2) 0.17(3) 0.04(1) 0.05(2) 0.07(2) C C39 0.09(2) 0.15(2) 0.24(4) 0.07(1) 0.09(2) 0.06(3) C C40 0.10(2) 0.15(3) 0.12(2) -0.06(2) -0.09(2) 0.06(2) C HG3 0.0364 0.0460(3) 0.0356(4) 0.0201(2) -0.0020(3) 0.0005(4) Hg S9 0.042(2) 0.047(2) 0.031(3) 0.024(2) -0.002(2) -0.003(2) S S10 0.046(2) 0.052(2) 0.033(3) 0.028(2) -0.001(2) -0.002(2) S S11 0.036(2) 0.048(2) 0.031(3) 0.016(2) -0.000(2) 0.006(2) S S12 0.052(2) 0.045(2) 0.029(3) 0.029(2) -0.004(2) 0.003(2) S C41 0.042(8) 0.035(8) 0.04(1) 0.027(6) -0.001(9) -0.001(8) C C42 0.08(1) 0.043(9) 0.04(1) 0.039(7) 0.00(1) 0.001(9) C C43 0.11(1) 0.07(1) 0.02(1) 0.062(7) -0.00(1) 0.014(9) C C44 0.08(1) 0.054(9) 0.07(2) 0.048(7) -0.02(1) -0.02(1) C C45 0.036(8) 0.040(9) 0.05(1) 0.021(6) 0.001(9) 0.018(9) C C46 0.033(8) 0.033(9) 0.04(1) 0.015(6) -0.011(9) 0.000(9) C C47 0.29(2) 0.11(1) 0.03(1) 0.15(1) 0.03(2) 0.01(1) C C48 0.23(3) 0.07(2) 0.08(2) 0.08(1) 0.04(2) 0.03(2) C C49 0.27(2) 0.16(1) 0.04(2) 0.186(9) 0.02(2) 0.04(1) C C50 0.49(3) 0.15(2) 0.09(2) 0.24(1) -0.12(2) -0.05(2) C C51 0.035(9) 0.038(9) 0.013(9) 0.007(7) -0.010(8) -0.016(8) C C52 0.06(1) 0.04(1) 0.04(1) 0.021(8) -0.00(1) -0.00(1) C C53 0.024(8) 0.041(9) 0.05(1) 0.015(6) -0.007(9) -0.00(1) C C54 0.039(9) 0.05(1) 0.03(1) 0.019(7) 0.006(9) -0.005(9) C C55 0.053(9) 0.056(9) 0.02(1) 0.037(6) -0.006(8) -0.002(8) C C56 0.038(9) 0.041(9) 0.02(1) 0.017(6) -0.001(8) 0.000(8) C C57 0.07(1) 0.07(1) 0.20(3) 0.038(9) 0.03(2) 0.08(2) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag HG1 HG2 3.8990(9) . . ? HG1 S1 2.397(7) . . ? HG1 S5 2.959(7) . . ? HG1 S6 2.987(7) . . ? HG1 S7 2.384(7) . . ? HG2 S1 2.953(7) . . ? HG2 S2 2.928(7) . . ? HG2 S3 2.384(7) . . ? HG2 S5 2.414(8) . . ? HG3 S9 2.399(8) . . ? HG3 S10 2.977(8) . . ? HG3 S11 2.368(8) . . ? S1 C6 1.76(2) . . ? S2 C5 1.77(2) . . ? S2 C11 1.76(3) . . ? S3 C16 1.80(2) . . ? S4 C15 1.77(3) . . ? S4 C21 1.76(2) . . ? S5 C26 1.74(2) . . ? S6 C25 1.81(2) . . ? S6 C31 1.75(2) . . ? S7 C36 1.78(2) . . ? S8 C1 1.77(2) . . ? S8 C35 1.73(3) . . ? C1 C2 1.34(3) . . ? C1 C6 1.41(3) . . ? C2 C3 1.39(3) . . ? C3 C4 1.38(3) . . ? C3 C7 1.42(2) . . ? C4 C5 1.39(3) . . ? C5 C6 1.41(3) . . ? C7 C8 1.7963 . . ? C7 C9 1.5590 . . ? C7 C10 1.7491 . . ? C8 C9 2.0274 . . ? C11 C12 1.40(3) . . ? C11 C16 1.41(3) . . ? C12 C13 1.33(3) . . ? C13 C14 1.44(4) . . ? C13 C17 1.57(4) . . ? C14 C15 1.42(4) . . ? C15 C16 1.41(3) . . ? C17 C18 1.60(5) . . ? C17 C19 1.53(4) . . ? C17 C20 1.54(4) . . ? C21 C22 1.38(3) . . ? C22 C23 1.46(3) . . ? C23 C24 1.36(3) . . ? C23 C27 1.69(2) . . ? C25 C26 1.42(3) . . ? C27 C28 1.4892 . . ? C27 C29 1.7195 . . ? C27 C30 1.3885 . . ? C31 C32 1.41(3) . . ? C31 C36 1.43(3) . . ? C32 C33 1.40(4) . . ? C33 C34 1.28(3) . . ? C33 C37 1.59(3) . . ? C37 C38 1.54(4) . . ? C37 C39 1.59(5) . . ? C37 C40 1.45(4) . . ? S9 C46 1.76(2) . . ? S10 C45 1.82(2) . . ? S10 C51 1.80(2) . . ? S11 C56 1.79(2) . . ? S12 C41 1.77(2) . . ? S12 C55 1.80(2) . . ? C41 C42 1.33(3) . . ? C42 C43 1.34(3) . . ? C43 C44 1.37(3) . . ? C43 C47 1.56(4) . . ? C44 C45 1.43(3) . . ? C47 C48 1.50(6) . . ? C47 C49 1.39(5) . . ? C47 C50 1.51(5) . . ? C51 C52 1.42(3) . . ? C51 C56 1.40(3) . . ? C52 C53 1.36(3) . . ? C53 C54 1.37(3) . . ? C53 C57 1.52(4) . . ? C57 C58 1.38(5) . . ? C57 C59 1.40(4) . . ? C57 C60 1.59(6) . . ? C61 CL1 1.70(2) . . ? C62 CL2 1.77(8) . . ? C63 CL3 2.00(1) . . ? C63 CL4 1.90(1) . . ? C63 CL5 1.82(1) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 HG1 S5 84.62 . . . ? S1 HG1 S6 109.93 . . . ? S1 HG1 S7 173.30 . . . ? S1 HG1 S8 72.48 . . . ? S5 HG1 S7 96.94 . . . ? S5 HG1 S8 133.70 . . . ? S6 HG1 S7 76.57 . . . ? S6 HG1 S8 84.72 . . . ? S7 HG1 S8 110.45 . . . ? S1 HG2 S2 67.35 . . . ? S1 HG2 S3 95.23 . . . ? S1 HG2 S5 84.47 . . . ? S2 HG2 S3 78.47 . . . ? S2 HG2 S5 109.72 . . . ? S3 HG2 S5 170.80 . . . ? S9 HG3 S10 108.73 . . . ? S9 HG3 S11 173.20 . . . ? S10 HG3 S11 77.76 . . . ? C5 S2 C11 101(1) . . . ? C15 S4 C21 103(1) . . . ? C25 S6 C31 100(1) . . . ? C1 S8 C35 98(1) . . . ? S8 C1 C2 118(1) . . . ? S8 C1 C6 121(1) . . . ? C2 C1 C6 120(2) . . . ? C1 C2 C3 120(2) . . . ? C2 C3 C4 120(2) . . . ? C2 C3 C7 123(1) . . . ? C4 C3 C7 116(1) . . . ? C3 C4 C5 120(2) . . . ? S2 C5 C4 118(1) . . . ? S2 C5 C6 123(1) . . . ? C4 C5 C6 118(2) . . . ? S1 C6 C1 120(2) . . . ? S1 C6 C5 119(1) . . . ? C1 C6 C5 120(2) . . . ? C3 C7 C8 110.0(9) . . . ? C3 C7 C9 111.1(9) . . . ? C3 C7 C10 120.0(9) . . . ? C8 C7 C9 73.97 . . . ? C8 C7 C10 121.39 . . . ? C9 C7 C10 110.98 . . . ? C7 C8 C9 47.65 . . . ? C7 C9 C8 58.38 . . . ? S2 C11 C12 118(2) . . . ? S2 C11 C16 124(2) . . . ? C12 C11 C16 116(2) . . . ? C11 C12 C13 125(2) . . . ? C12 C13 C14 118(2) . . . ? C12 C13 C17 123(2) . . . ? C14 C13 C17 117(2) . . . ? C13 C14 C15 118(2) . . . ? S4 C15 C14 114(2) . . . ? S4 C15 C16 125(1) . . . ? C14 C15 C16 119(2) . . . ? S3 C16 C11 121(2) . . . ? S3 C16 C15 116(1) . . . ? C11 C16 C15 121(2) . . . ? C13 C17 C18 110(2) . . . ? C13 C17 C19 112(2) . . . ? C13 C17 C20 105(2) . . . ? C18 C17 C19 112(3) . . . ? C18 C17 C20 109(3) . . . ? C19 C17 C20 105(2) . . . ? S4 C21 C22 119(2) . . . ? C21 C22 C23 121(2) . . . ? C22 C23 C24 116(1) . . . ? C22 C23 C27 119(1) . . . ? C24 C23 C27 124(1) . . . ? S6 C25 C26 118(1) . . . ? S5 C26 C25 122(1) . . . ? C23 C27 C28 105.6(7) . . . ? C23 C27 C29 101.4(6) . . . ? C23 C27 C30 104.9(6) . . . ? C28 C27 C29 108.47 . . . ? C28 C27 C30 114.46 . . . ? C29 C27 C30 120.09 . . . ? S6 C31 C32 121(2) . . . ? S6 C31 C36 124(1) . . . ? C32 C31 C36 114(2) . . . ? C31 C32 C33 123(2) . . . ? C32 C33 C34 119(2) . . . ? C32 C33 C37 118(2) . . . ? C34 C33 C37 121(2) . . . ? S7 C36 C31 121(1) . . . ? C33 C37 C38 113(2) . . . ? C33 C37 C39 109(2) . . . ? C33 C37 C40 103(2) . . . ? C38 C37 C39 101(2) . . . ? C38 C37 C40 118(3) . . . ? C39 C37 C40 111(3) . . . ? C45 S10 C51 101(1) . . . ? C41 S12 C55 101(1) . . . ? S12 C41 C42 122(1) . . . ? C41 C42 C43 124(2) . . . ? C42 C43 C44 118(2) . . . ? C42 C43 C47 119(2) . . . ? C44 C43 C47 121(2) . . . ? C43 C44 C45 120(2) . . . ? S10 C45 C44 116(1) . . . ? C43 C47 C48 107(3) . . . ? C43 C47 C49 110(3) . . . ? C43 C47 C50 111(2) . . . ? C48 C47 C49 111(3) . . . ? C48 C47 C50 107(4) . . . ? C49 C47 C50 109(3) . . . ? S10 C51 C52 117(1) . . . ? S10 C51 C56 123(1) . . . ? C52 C51 C56 119(2) . . . ? C51 C52 C53 122(2) . . . ? C52 C53 C54 116(2) . . . ? C52 C53 C57 121(2) . . . ? C54 C53 C57 121(2) . . . ? C53 C57 C58 113(3) . . . ? C53 C57 C59 114(2) . . . ? C53 C57 C60 105(3) . . . ? C58 C57 C59 118(3) . . . ? C58 C57 C60 107(4) . . . ? C59 C57 C60 95(3) . . . ? CL3 C63 CL4 90.3(6) . . . ? CL3 C63 CL5 93.2(6) . . . ? CL4 C63 CL5 92.0(6) . . . ? data_hgs4x _database_code_CSD 179244 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C106 H136 Hg4 O12 S12' _chemical_formula_moiety ? _chemical_formula_weight 2789.39 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pban' _symmetry_space_group_name_Hall -p_2ab_2b loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2-y,+z +x,1/2-y,-z 1/2-x,+y,-z -x,-y,-z 1/2+x,1/2+y,-z -x,1/2+y,+z 1/2+x,-y,+z _cell_length_a 17.7640(10) _cell_length_b 21.016(2) _cell_length_c 14.9290(10) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 5573.4(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 24.4 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 5.773 _exptl_crystal_description prism _exptl_crystal_size_max .24 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .44 _exptl_absorpt_correction_T_max .77 _diffrn_reflns_number 88663 _reflns_number_total 7521 _reflns_Friedel_coverage 0 _reflns_number_gt 3750 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.13 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .113 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .056 _refine_ls_wR_factor_ref .067 _refine_ls_goodness_of_fit_ref 1.436 _refine_ls_number_reflns 3750 _refine_ls_number_parameters 275 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .085 _refine_diff_density_min -1.345 _refine_diff_density_max 1.903 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 212 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 272 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Hg ? 0 8 -3.084 9.223 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 24 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 24 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Hg1 .25000 .61911(2) .00000 .0353(3) Uani ? ? 1.00000 ? ? Hg2 .25000 .75000 .16918(3) .0398(3) Uani ? ? 1.00000 ? ? O11 .3358(4) .6880(3) .0846(4) .038(4) Uani ? ? 1.00000 ? ? C11 .3858(5) .6566(5) .1348(7) .030(5) Uani ? ? 1.00000 ? ? C12 .4133(5) .5964(5) .1060(7) .032(6) Uani ? ? 1.00000 ? ? C13 .4677(6) .5657(5) .1556(7) .041(6) Uani ? ? 1.00000 ? ? C14 .4957(6) .5894(6) .2376(7) .046(7) Uani ? ? 1.00000 ? ? C141 .5590(7) .5572(7) .2879(9) .064(9) Uani ? ? 1.00000 ? ? C142 .5333(11) .5466(9) .3796(12) .122(15) Uani ? ? 1.00000 ? ? C143 .6264(11) .6029(10) .3048(16) .140(19) Uani ? ? 1.00000 ? ? C144 .5901(11) .4984(9) .2469(13) .136(16) Uani ? ? 1.00000 ? ? C15 .4660(7) .6474(6) .2653(7) .050(7) Uani ? ? 1.00000 ? ? C16 .4124(7) .6785(5) .2181(7) .042(7) Uani ? ? 1.00000 ? ? S1 .37570(19) .75207(18) .25871(17) .0514(16) Uani ? ? 1.00000 ? ? O21 .3086(4) .6503(3) -.1316(4) .038(4) Uani ? ? 1.00000 ? ? C21 .3790(7) .6501(5) -.1302(7) .051(7) Uani ? ? 1.00000 ? ? C22 .4239(7) .6921(5) -.1887(7) .051(8) Uani ? ? 1.00000 ? ? C23 .5026(7) .6906(6) -.1919(7) .052(7) Uani ? ? 1.00000 ? ? C24 .5428(7) .6516(6) -.1401(8) .056(8) Uani ? ? 1.00000 ? ? C241 .6323(8) .6482(7) -.1455(12) .091(13) Uani ? ? 1.00000 ? ? C242 .663(2) .701(2) -.176(2) .116(13) Uiso ? ? .50000 ? ? C243 .664(2) .6327(19) -.049(3) .121(14) Uiso ? ? .50000 ? ? C244 .6480(18) .5900(16) -.205(2) .087(10) Uiso ? ? .50000 ? ? C242' .662(2) .689(2) -.245(3) .129(14) Uiso ? ? .50000 ? ? C243' .662(2) .7009(17) -.090(2) .099(11) Uiso ? ? .50000 ? ? C244' .6638(17) .5877(14) -.140(2) .080(9) Uiso ? ? .50000 ? ? C25 .5037(7) .6122(6) -.0794(8) .055(8) Uani ? ? 1.00000 ? ? C26 .4280(6) .6117(5) -.0751(8) .044(7) Uani ? ? 1.00000 ? ? S2 .38120(16) .56233(12) .0059(2) .0406(14) Uani ? ? 1.00000 ? ? O10 .25000 .5461(11) .50000 .52(2) Uiso ? ? 1.00000 ? ? S10 .2549(9) .5820(7) .4156(10) .52(2) Uiso ? ? .50000 ? ? C101 .313(2) .5429(15) .343(3) .52(2) Uiso ? ? .50000 ? ? C102 .289(2) .654(2) .4367(18) .52(2) Uiso ? ? .50000 ? ? O20 .9953(15) .7336(18) .496(3) .54(2) Uiso ? ? .50000 ? ? S20 .9585(8) .6920(7) .4393(10) .54(2) Uiso ? ? .50000 ? ? C201 1.0046(18) .625(2) .437(3) .54(2) Uiso ? ? .50000 ? ? C202 .872(3) .6802(13) .477(3) .54(2) Uiso ? ? .50000 ? ? C301 .5699(8) .75000 .50000 .091(5) Uiso ? ? .50000 ? ? C3011 .651(2) .75000 .50000 .091(5) Uiso ? ? .50000 ? ? C302 .5304(9) .6959(8) .534(2) .091(5) Uiso ? ? .50000 ? ? C303 .4553(6) .6956(7) .535(2) .091(5) Uiso ? ? .50000 ? ? C3031 .4145(11) .6390(13) .565(2) .091(5) Uiso ? ? .50000 ? ? C304 .4144(7) .74999 .50000 .091(5) Uiso ? ? .50000 ? ? C401 .25000 .4492(7) .50000 .186(11) Uiso ? ? .50000 ? ? C4011 .25000 .378(2) .50000 .186(11) Uiso ? ? .50000 ? ? C402 .274(2) .4803(8) .4237(12) .186(11) Uiso ? ? .50000 ? ? C403 .278(2) .5314(5) .4221(9) .186(11) Uiso ? ? .50000 ? ? C4031 .294(3) .5631(11) .334(2) .186(11) Uiso ? ? .50000 ? ? C404 .25000 .5673(6) .50000 .186(11) Uiso ? ? .50000 ? ? H13 .48973 .52594 .13127 .05500 Uiso ? ? 1.00000 ? ? H142a .57453 .52276 .41263 .19800 Uiso ? ? 1.00000 ? ? H142b .49237 .51471 .37929 .19800 Uiso ? ? 1.00000 ? ? H142c .52058 .58081 .41118 .19800 Uiso ? ? 1.00000 ? ? H143a .65979 .58290 .33653 .23300 Uiso ? ? 1.00000 ? ? H143b .60199 .63822 .33843 .23300 Uiso ? ? 1.00000 ? ? H143c .63988 .61879 .24888 .23300 Uiso ? ? 1.00000 ? ? H144a .62705 .48156 .28029 .17700 Uiso ? ? 1.00000 ? ? H144b .60654 .50840 .18660 .17700 Uiso ? ? 1.00000 ? ? H144c .54796 .46891 .23999 .17700 Uiso ? ? 1.00000 ? ? H15 .48003 .66268 .32407 .06900 Uiso ? ? 1.00000 ? ? H23 .52716 .71926 -.23807 .06400 Uiso ? ? 1.00000 ? ? H242a .71615 .69947 -.18577 .16800 Uiso ? ? .50000 ? ? H242b .65230 .73812 -.14033 .16800 Uiso ? ? .50000 ? ? H242c .64217 .71330 -.23745 .16800 Uiso ? ? .50000 ? ? H243a .71713 .63548 -.04941 .19600 Uiso ? ? .50000 ? ? H243b .64549 .59678 -.02565 .19600 Uiso ? ? .50000 ? ? H243c .64724 .66974 -.00995 .19600 Uiso ? ? .50000 ? ? H244a .70191 .58422 -.20784 .13000 Uiso ? ? .50000 ? ? H244b .62640 .59230 -.25879 .13000 Uiso ? ? .50000 ? ? H244c .62931 .55232 -.17151 .13000 Uiso ? ? .50000 ? ? H242'a .72292 .67759 -.24174 .18200 Uiso ? ? .50000 ? ? H242'b .66073 .72930 -.23682 .18200 Uiso ? ? .50000 ? ? H242'c .64775 .66815 -.29294 .18200 Uiso ? ? .50000 ? ? H243'a .72166 .69785 -.09606 .16800 Uiso ? ? .50000 ? ? H243'b .65556 .69336 -.02844 .16800 Uiso ? ? .50000 ? ? H243'c .65093 .74023 -.10853 .16800 Uiso ? ? .50000 ? ? H244'a .71789 .59318 -.14264 .12600 Uiso ? ? .50000 ? ? H244'b .64617 .56072 -.18041 .12600 Uiso ? ? .50000 ? ? H244'c .65349 .57316 -.07836 .12600 Uiso ? ? .50000 ? ? H25 .53055 .57753 -.03819 .08000 Uiso ? ? 1.00000 ? ? H101a .28237 .49300 .32977 .50300 Uiso ? ? .50000 ? ? H101b .35392 .52886 .36142 .50300 Uiso ? ? .50000 ? ? H101c .30309 .55818 .28769 .50300 Uiso ? ? .50000 ? ? H102a .25869 .66597 .48922 .50300 Uiso ? ? .50000 ? ? H102b .28768 .67070 .39142 .50300 Uiso ? ? .50000 ? ? H102c .33851 .64138 .46514 .50300 Uiso ? ? .50000 ? ? H201a 1.04781 .63464 .39709 .72500 Uiso ? ? .50000 ? ? H201b .97100 .60110 .38240 .72500 Uiso ? ? .50000 ? ? H201c 1.00741 .60187 .47684 .72500 Uiso ? ? .50000 ? ? H202a .84645 .71577 .50570 .72500 Uiso ? ? .50000 ? ? H202b .87902 .65358 .54610 .72500 Uiso ? ? .50000 ? ? H202c .84260 .65281 .45165 .72500 Uiso ? ? .50000 ? ? H3011a .66910 .71532 .53587 .13700 Uiso ? ? .25000 ? ? H3011b .67090 .74514 .44055 .13700 Uiso ? ? .25000 ? ? H3011c .67090 .78885 .52429 .13700 Uiso ? ? .25000 ? ? H302 .55634 .65704 .55564 .11500 Uiso ? ? .50000 ? ? H3031a .44657 .61015 .59603 .13700 Uiso ? ? .50000 ? ? H3031b .38925 .61635 .51769 .13700 Uiso ? ? .50000 ? ? H3031c .37340 .64991 .60830 .13700 Uiso ? ? .50000 ? ? H304 .35760 .75000 .50000 .13700 Uiso ? ? .50000 ? ? H4011a .26314 .36769 .44261 .25200 Uiso ? ? .25000 ? ? H4011b .20119 .36893 .51552 .25200 Uiso ? ? .25000 ? ? H4011c .28545 .36893 .54284 .25200 Uiso ? ? .25000 ? ? H402 .29292 .46054 .37616 .21000 Uiso ? ? .50000 ? ? H4031a .29989 .61802 .33778 .21000 Uiso ? ? .50000 ? ? H4031b .34029 .55699 .30407 .21000 Uiso ? ? .50000 ? ? H4031c .25402 .56430 .29161 .21000 Uiso ? ? .50000 ? ? H404 .25000 .62402 .50000 .21000 Uiso ? ? .50000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Hg1 .0456(3) .0361(3) .0243(2) .00000 -.0092(4) .00000 Hg2 .0583(4) .0283(3) .0328(3) .0136(5) .00000 .00000 O11 .038(4) .039(4) .038(4) .007(4) -.007(3) -.008(4) C11 .015(5) .039(6) .037(6) -.008(4) -.001(4) -.012(5) C12 .024(5) .038(6) .034(5) .006(5) -.003(4) -.016(5) C13 .031(6) .044(7) .049(7) .009(5) -.004(5) -.017(6) C14 .040(6) .050(8) .048(7) .017(6) -.021(6) -.016(6) C141 .044(8) .078(10) .069(9) .030(7) -.034(7) -.022(8) C142 .149(18) .114(15) .104(14) .086(14) -.040(13) -.006(13) C143 .102(15) .122(18) .20(2) .019(13) -.063(16) -.047(16) C144 .145(17) .140(16) .125(15) .093(14) -.101(13) -.082(13) C15 .061(8) .048(8) .040(6) .012(6) -.023(6) -.013(6) C16 .065(8) .027(6) .033(6) .014(6) -.015(6) -.015(5) S1 .086(2) .0358(14) .0324(12) .021(2) -.0129(13) -.018(2) O21 .036(4) .044(5) .034(4) -.004(4) -.003(3) -.005(4) C21 .082(9) .039(7) .031(6) .008(7) .018(6) -.023(5) C22 .072(9) .040(7) .041(6) -.002(7) .018(6) -.029(6) C23 .055(8) .047(8) .053(7) -.015(6) .022(6) -.024(6) C24 .045(7) .054(8) .068(9) -.008(6) .009(7) -.034(7) C241 .070(11) .070(11) .133(16) -.012(9) .025(11) -.023(11) C25 .047(7) .045(8) .073(9) .005(6) -.002(7) -.038(7) C26 .045(7) .031(6) .054(7) -.007(5) -.005(6) -.023(6) S2 .0539(15) .0336(12) .0342(14) .0076(11) -.0109(18) -.0140(18) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Hg1 O11 . . 2.452(7) ? Hg1 O21 . . 2.318(7) ? Hg1 S2 . . 2.620(3) ? Hg1 O11 . 4 2.452(7) ? Hg1 O21 . 4 2.318(7) ? Hg1 S2 . 4 2.620(3) ? Hg2 O11 . . 2.370(7) ? Hg2 S1 . . 2.603(3) ? Hg2 O11 . '2 565' 2.370(7) ? Hg2 S1 . '2 565' 2.603(3) ? Hg2 O21 . '3 565' 2.407(7) ? Hg2 O21 . 4 2.407(7) ? O11 C11 . . 1.335(12) ? C11 C12 . . 1.424(14) ? C11 C16 . . 1.409(14) ? C12 C13 . . 1.378(14) ? C12 S2 . . 1.751(10) ? C13 C14 . . 1.413(16) ? C13 H13 . . .991 ? C14 C141 . . 1.512(17) ? C14 C15 . . 1.391(17) ? C141 C142 . . 1.46(2) ? C141 C143 . . 1.55(2) ? C141 C144 . . 1.49(2) ? C142 H142a . . 1.015 ? C142 H142b . . .99 ? C142 H142c . . .888 ? C143 H143a . . .87 ? C143 H143b . . .99 ? C143 H143c . . .93 ? C144 H144a . . .90 ? C144 H144b . . .970 ? C144 H144c . . .98 ? C15 C16 . . 1.353(16) ? C15 H15 . . .967 ? C16 S1 . . 1.784(11) ? S1 C22 . '3 565' 1.790(12) ? O21 C21 . . 1.250(14) ? C21 C22 . . 1.476(16) ? C21 C26 . . 1.443(16) ? C22 C23 . . 1.399(18) ? C23 C24 . . 1.333(17) ? C23 H23 . . 1.015 ? C24 C241 . . 1.594(19) ? C24 C25 . . 1.411(17) ? C241 C242 . . 1.32(4) ? C241 C243 . . 1.59(4) ? C241 C244 . . 1.53(4) ? C241 C242' . . 1.80(5) ? C241 C243' . . 1.48(4) ? C241 C244' . . 1.39(3) ? C242 H242a . . .95 ? C242 H242b . . .96 ? C242 H242c . . 1.02 ? C243 H243a . . .94 ? C243 H243b . . .89 ? C243 H243c . . 1.01 ? C244 H244a . . .97 ? C244 H244b . . .90 ? C244 H244c . . .99 ? C242' H242'a . . 1.10 ? C242' H242'b . . .86 ? C242' H242'c . . .87 ? C243' H243'a . . 1.06 ? C243' H243'b . . .94 ? C243' H243'c . . .89 ? C244' H244'a . . .97 ? C244' H244'b . . .89 ? C244' H244'c . . .98 ? C25 C26 . . 1.346(17) ? C25 H25 . . 1.066 ? C26 S2 . . 1.798(12) ? O10 S10 . . 1.471(19) ? O10 S10 . '4 556' 1.471(19) ? S10 C101 . . 1.71(4) ? S10 C102 . . 1.65(5) ? C101 H101a . . 1.20 ? C101 H101b . . .83 ? C101 H101c . . .91 ? C102 H102a . . .98 ? C102 H102b . . .77 ? C102 H102c . . 1.02 ? O20 S20 . . 1.38(4) ? S20 C201 . . 1.64(4) ? S20 C202 . . 1.65(5) ? C201 H201a . . .99 ? C201 H201b . . 1.12 ? C201 H201c . . .77 ? C202 H202a . . .98 ? C202 H202b . . 1.18 ? C202 H202c . . .87 ? C301 C3011 . . 1.44(4) ? C301 C302 . . 1.43(2) ? C301 C302 . '3 566' 1.43(2) ? C3011 H3011a . . .961 ? C3011 H3011b . . .962 ? C3011 H3011c . . .962 ? C3011 H3011a . '3 566' .961 ? C3011 H3011b . '3 566' .962 ? C3011 H3011c . '3 566' .962 ? C302 C303 . . 1.34(2) ? C302 H302 . . .992 ? C303 C3031 . . 1.46(3) ? C303 C304 . . 1.453(18) ? C3031 H3031a . . .95 ? C3031 H3031b . . .96 ? C3031 H3031c . . 1.00 ? C304 H304 . . 1.009 ? C401 C4011 . . 1.49 ? C401 C402 . . 1.38(2) ? C401 C402 . '4 556' 1.38 ? C4011 H4011a . . .916 ? C4011 H4011b . . .919 ? C4011 H4011c . . .919 ? C4011 H4011a . '4 556' .916 ? C4011 H4011b . '4 556' .919 ? C4011 H4011c . '4 556' .919 ? C402 C403 . . 1.08(2) ? C402 H402 . . .89 ? C403 C4031 . . 1.50(4) ? C403 C404 . . 1.473(18) ? C4031 H4031a . . 1.16 ? C4031 H4031b . . .94 ? C4031 H4031c . . .96 ? C404 H404 . . 1.193 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published O11 Hg1 O21 . . . 89.5(2) ? O11 Hg1 S2 . . . 72.45(17) ? O11 Hg1 O11 . . 4 107.7(2) ? O11 Hg1 O21 . . 4 71.1(2) ? O11 Hg1 S2 . . 4 147.04(18) ? O21 Hg1 S2 . . . 75.96(19) ? O21 Hg1 O11 . . 4 71.1(2) ? O21 Hg1 O21 . . 4 147.2(2) ? O21 Hg1 S2 . . 4 120.00(19) ? S2 Hg1 O11 . . 4 147.04(18) ? S2 Hg1 O21 . . 4 120.00(19) ? S2 Hg1 S2 . . 4 125.81(8) ? O11 Hg1 O21 4 . 4 89.5(2) ? O11 Hg1 S2 4 . 4 72.45(17) ? O21 Hg1 S2 4 . 4 75.96(19) ? O11 Hg2 S1 . . . 74.40(18) ? O11 Hg2 O11 . . '2 565' 115.6(2) ? O11 Hg2 S1 . . '2 565' 144.69(18) ? O11 Hg2 O21 . . '3 565' 94.4(2) ? O11 Hg2 O21 . . 4 71.0(2) ? S1 Hg2 O11 . . '2 565' 144.69(19) ? S1 Hg2 S1 . . '2 565' 118.20(9) ? S1 Hg2 O21 . . '3 565' 74.56(18) ? S1 Hg2 O21 . . 4 120.38(18) ? O11 Hg2 S1 '2 565' . '2 565' 74.40(18) ? O11 Hg2 O21 '2 565' . '3 565' 71.0(2) ? O11 Hg2 O21 '2 565' . 4 94.4(2) ? S1 Hg2 O21 '2 565' . '3 565' 120.38(18) ? S1 Hg2 O21 '2 565' . 4 74.56(18) ? O21 Hg2 O21 '3 565' . 4 153.0(2) ? Hg1 O11 Hg2 . . . 101.5(3) ? Hg1 O11 C11 . . . 114.3(6) ? Hg2 O11 C11 . . . 113.6(6) ? O11 C11 C12 . . . 119.8(9) ? O11 C11 C16 . . . 123.9(9) ? C12 C11 C16 . . . 116.2(9) ? C11 C12 C13 . . . 119.7(9) ? C11 C12 S2 . . . 120.6(7) ? C13 C12 S2 . . . 119.7(8) ? C12 C13 C14 . . . 123.2(10) ? C12 C13 H13 . . . 118.4 ? C14 C13 H13 . . . 118.4 ? C13 C14 C141 . . . 122.3(10) ? C13 C14 C15 . . . 115.6(10) ? C141 C14 C15 . . . 121.8(10) ? C14 C141 C142 . . . 107.5(12) ? C14 C141 C143 . . . 112.2(12) ? C14 C141 C144 . . . 116.4(12) ? C142 C141 C143 . . . 100.5(14) ? C142 C141 C144 . . . 112.0(14) ? C143 C141 C144 . . . 107.2(13) ? C141 C142 H142a . . . 107.8 ? C141 C142 H142b . . . 109.2 ? C141 C142 H142c . . . 117.0 ? H142a C142 H142b . . . 101.4 ? H142a C142 H142c . . . 109.0 ? H142b C142 H142c . . . 111 ? C141 C143 H143a . . . 108.4 ? C141 C143 H143b . . . 102.0 ? C141 C143 H143c . . . 105.9 ? H143a C143 H143b . . . 113 ? H143a C143 H143c . . . 119 ? H143b C143 H143c . . . 107 ? C141 C144 H144a . . . 111.8 ? C141 C144 H144b . . . 108.2 ? C141 C144 H144c . . . 106.6 ? H144a C144 H144b . . . 112 ? H144a C144 H144c . . . 112 ? H144b C144 H144c . . . 105.6 ? C14 C15 C16 . . . 122.4(10) ? C14 C15 H15 . . . 117.6 ? C16 C15 H15 . . . 119.5 ? C11 C16 C15 . . . 122.5(10) ? C11 C16 S1 . . . 117.4(8) ? C15 C16 S1 . . . 120.0(8) ? Hg2 S1 C16 . . . 97.2(4) ? Hg2 S1 C22 . . '3 565' 97.0(4) ? C16 S1 C22 . . '3 565' 101.2(5) ? Hg1 O21 C21 . . . 115.7(6) ? Hg1 O21 Hg2 . . '3 565' 104.4(3) ? C21 O21 Hg2 . . '3 565' 116.1(7) ? O21 C21 C22 . . . 121.9(10) ? O21 C21 C26 . . . 128.0(10) ? C22 C21 C26 . . . 110.2(10) ? C21 C22 C23 . . . 123.1(10) ? C21 C22 S1 . . '3 565' 118.7(9) ? C23 C22 S1 . . '3 565' 118.2(9) ? C22 C23 C24 . . . 121.9(11) ? C22 C23 H23 . . . 116.1 ? C24 C23 H23 . . . 121.9 ? C23 C24 C241 . . . 122.2(12) ? C23 C24 C25 . . . 118.0(11) ? C241 C24 C25 . . . 119.8(11) ? C24 C241 C242 . . . 113(2) ? C24 C241 C243 . . . 108.5(18) ? C24 C241 C244 . . . 104.2(15) ? C24 C241 C242' . . . 108.5(16) ? C24 C241 C243' . . . 107.2(17) ? C24 C241 C244' . . . 116.0(16) ? C242 C241 C243 . . . 110(2) ? C242 C241 C244 . . . 114(2) ? C243 C241 C244 . . . 107(2) ? C242' C241 C243' . . . 90(2) ? C242' C241 C244' . . . 111(2) ? C243' C241 C244' . . . 120(2) ? C241 C242 H242a . . . 115 ? C241 C242 H242b . . . 114 ? C241 C242 H242c . . . 111 ? H242a C242 H242b . . . 108 ? H242a C242 H242c . . . 103 ? H242b C242 H242c . . . 103 ? C241 C243 H243a . . . 109 ? C241 C243 H243b . . . 113 ? C241 C243 H243c . . . 105 ? H243a C243 H243b . . . 115 ? H243a C243 H243c . . . 105 ? H243b C243 H243c . . . 109(4) ? C241 C244 H244a . . . 108 ? C241 C244 H244b . . . 114 ? C241 C244 H244c . . . 107 ? H244a C244 H244b . . . 113 ? H244a C244 H244c . . . 105 ? H244b C244 H244c . . . 110 ? C241 C242' H242'a . . . 99 ? C241 C242' H242'b . . . 110 ? C241 C242' H242'c . . . 111 ? H242'a C242' H242'b . . . 104 ? H242'a C242' H242'c . . . 103 ? H242'b C242' H242'c . . . 127 ? C241 C243' H243'a . . . 105 ? C241 C243' H243'b . . . 112 ? C241 C243' H243'c . . . 116 ? H243'a C243' H243'b . . . 101 ? H243'a C243' H243'c . . . 105 ? H243'b C243' H243'c . . . 115 ? C241 C244' H244'a . . . 107 ? C241 C244' H244'b . . . 113 ? C241 C244' H244'c . . . 106 ? H244'a C244' H244'b . . . 113 ? H244'a C244' H244'c . . . 106 ? H244'b C244' H244'c . . . 112 ? C24 C25 C26 . . . 121.7(11) ? C24 C25 H25 . . . 123.5 ? C26 C25 H25 . . . 114.5 ? C21 C26 C25 . . . 124.9(11) ? C21 C26 S2 . . . 115.2(8) ? C25 C26 S2 . . . 119.9(9) ? Hg1 S2 C12 . . . 97.6(3) ? Hg1 S2 C26 . . . 97.2(4) ? C12 S2 C26 . . . 100.8(5) ? O10 S10 C101 . . . 109.3(16) ? O10 S10 C102 . . . 109.0(15) ? C101 S10 C102 . . . 109.9(19) ? S10 C101 H101a . . . 104 ? S10 C101 H101b . . . 120 ? S10 C101 H101c . . . 107 ? H101a C101 H101b . . . 98 ? H101a C101 H101c . . . 94 ? H101b C101 H101c . . . 127 ? S10 C102 H102a . . . 101 ? S10 C102 H102b . . . 105 ? S10 C102 H102c . . . 100 ? H102a C102 H102b . . . 125 ? H102a C102 H102c . . . 102 ? H102b C102 H102c . . . 120 ? O20 S20 C201 . . . 109(2) ? O20 S20 C202 . . . 109(2) ? C201 S20 C202 . . . 110.0(18) ? S20 C201 H201a . . . 102 ? S20 C201 H201b . . . 97 ? S20 C201 H201c . . . 124 ? H201a C201 H201b . . . 94 ? H201a C201 H201c . . . 123 ? H201b C201 H201c . . . 109 ? S20 C202 H202a . . . 118 ? S20 C202 H202b . . . 106 ? S20 C202 H202c . . . 121 ? H202a C202 H202b . . . 91(3) ? H202a C202 H202c . . . 115(5) ? H202b C202 H202c . . . 97(3) ? C3011 C301 C302 . . . 119.4(9) ? C3011 C301 C302 . . '3 566' 119.4(9) ? C302 C301 C302 . . '3 566' 121.2(14) ? C301 C3011 H3011a . . . 110 ? C301 C3011 H3011b . . . 111.7 ? C301 C3011 H3011c . . . 111.7 ? C301 C3011 H3011a . . '3 566' 110 ? C301 C3011 H3011b . . '3 566' 111.7 ? C301 C3011 H3011c . . '3 566' 111.7 ? H3011a C3011 H3011b . . . 108 ? H3011a C3011 H3011c . . . 108 ? H3011b C3011 H3011c . . . 108 ? H3011a C3011 H3011b '3 566' . '3 566' 108 ? H3011a C3011 H3011c '3 566' . '3 566' 108 ? H3011b C3011 H3011c '3 566' . '3 566' 108 ? C301 C302 C303 . . . 120.0(16) ? C301 C302 H302 . . . 122.9 ? C303 C302 H302 . . . 117.1 ? C302 C303 C3031 . . . 120.2(16) ? C302 C303 C304 . . . 119.4(15) ? C3031 C303 C304 . . . 120.2(12) ? C303 C3031 H3031a . . . 111.7 ? C303 C3031 H3031b . . . 114 ? C303 C3031 H3031c . . . 112 ? H3031a C3031 H3031b . . . 109 ? H3031a C3031 H3031c . . . 106 ? H3031b C3031 H3031c . . . 104.4 ? C303 C304 C303 . . '3 566' 120.1(11) ? H304 C304 C303 . . '3 566' 119.9 ? C4011 C401 C402 . . . 118.3(9) ? C4011 C401 C402 . . '4 556' 118.3(9) ? C402 C401 C402 . . '4 556' 123.4(15) ? C401 C4011 H4011a . . . 104 ? C401 C4011 H4011b . . . 103 ? C401 C4011 H4011c . . . 102 ? C401 C4011 H4011a . . '4 556' 104 ? C401 C4011 H4011b . . '4 556' 103 ? C401 C4011 H4011c . . '4 556' 102 ? H4011a C4011 H4011b . . . 115 ? H4011a C4011 H4011c . . . 115 ? H4011b C4011 H4011c . . . 115.1 ? H4011a C4011 H4011b '4 556' . '4 556' 115 ? H4011a C4011 H4011c '4 556' . '4 556' 115 ? H4011b C4011 H4011c '4 556' . '4 556' 115.1 ? C401 C402 C403 . . . 121(2) ? C401 C402 H402 . . . 123.6 ? C403 C402 H402 . . . 115 ? C402 C403 C4031 . . . 118.4(18) ? C402 C403 C404 . . . 118(2) ? C4031 C403 C404 . . . 121.9(14) ? C403 C4031 H4031a . . . 115 ? C403 C4031 H4031b . . . 122 ? C403 C4031 H4031c . . . 117 ? H4031a C4031 H4031b . . . 95 ? H4031a C4031 H4031c . . . 94 ? H4031b C4031 H4031c . . . 109 ? C403 C404 H404 . . . 120.8 ? C403 C404 C403 . . '4 556' 118.4(11) ? H404 C404 C403 . . '4 556' 120.8 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2760 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .73 _reflns_d_resolution_low 10.486 _diffrn_reflns_av_sigmaI/netI .161 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 36 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .132 _refine_ls_wR_factor_all .073 _refine_ls_goodness_of_fit_all 1.254 _refine_ls_shift/su_mean .004 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end