# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Zhengtao Xu' _publ_contact_author_email ZHENGTAO@CITYU.EDU.HK _publ_section_title ; Reversible uptake of HgCl2 in a porous coordination network based on the dual functions of carboxylate and thioether ; loop_ _publ_author_name 'Zhengtao Xu.' 'Allen D Hunter' 'Matthias Zeller' 'Xiao-Ping Zhou.' #===END data_1HgCl2 _database_code_depnum_ccdc_archive 'CCDC 733810' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 O12 Pb3 S12' _chemical_formula_weight 1667.09 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 19.0345(19) _cell_length_b 27.688(3) _cell_length_c 12.1273(12) _cell_angle_alpha 90.00 _cell_angle_beta 105.293(2) _cell_angle_gamma 90.00 _cell_volume 6165.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6037 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 30.46 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 8.623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.124 _exptl_absorpt_correction_T_max 0.387 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; The HgCl2 parts of the structure were found to be severely disordered and refinement attempts under inclusion of the HgCl2 component were not successful. Hg and Cl atoms were disordered over each one to three or more positions with anisotropic displacement parameters that indicated correlation between the disordered moieties and/or additional dynamic disorder of the atom. Possible presence of solvent molecules in addition to Hg and Cl atoms can not be excluded as a possibility. Any atoms in the voids were thus omitted from the structural model and only the host net Pb(TMBD) was refined. Due to the large residual electron density some restraints were applied in this model for methyl carbon atom position and some anisotropic displacement parameters, ADPs. This model was then used as the starting point for a dataset corrected for the residual electron density using the SQUEEZE procedure implemented in the program Platon (40-M version 180209, A. L. Spek, 1980-2009). The residual electron density per void was 658 electrons (or 5.77 molecules of HgCl2 per void). Each of the two voids per unit cell void is about 839 Angstrom cubed large or 14% of the unit cell volume. The structure was then re-refined, the restraints applied before could now be omitted, and the SQUEEZE procedure was then repeated using this improved structural model with the orginal hkl file. This slightly more reliable new hkl file was then used for the final refinement cycles to obtain the final structural model and the cif file corrected for the electron density of the ill defined HgCl2 molecules in the voids (see Squeeze report appended to this cif). Finally, a refinement was made with zero cycles with the new res file and the old uncorrected hkl file, in order to generate a difference res file, and to better assess the residual electron density peaks from the HgCl2 components. The following major residual electron density peaks (larger than 10 electrons per Angstrom cubed, thus larger than could be caused by atoms of any of the solvents used) were obtained: Q1 1 0.745800 0.000000 -0.011900 10.500000 0.050000 48.92 Q2 1 0.936300 0.500000 0.259900 10.500000 0.050000 22.48 Q3 1 0.733300 0.000000 0.092000 10.500000 0.050000 12.54 Q4 1 0.849600 0.452200 0.754400 11.000000 0.050000 12.14 Q5 1 0.862300 0.417500 0.694100 11.000000 0.050000 10.33 ; _diffrn_ambient_temperature 100(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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 25732 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.1076 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7728 _reflns_number_gt 4607 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.1049P)^2^+0.0000P] 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 7728 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1826 _refine_ls_wR_factor_gt 0.1673 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.001 _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 C1 C 0.8736(8) 0.2136(5) -0.0766(13) 0.051(4) Uani 1 1 d . . . C2 C 0.8159(7) 0.2756(4) 0.0304(9) 0.035(3) Uani 1 1 d . . . C3 C 0.8084(7) 0.2312(4) -0.0339(8) 0.030(3) Uani 1 1 d . . . C4 C 0.7437(7) 0.2060(4) -0.0604(8) 0.030(3) Uani 1 1 d . . . C5 C 0.8853(12) 0.3564(8) -0.025(2) 0.113(8) Uani 1 1 d . . . H5A H 0.8402 0.3513 -0.0849 0.169 Uiso 1 1 calc R . . H5B H 0.9259 0.3612 -0.0592 0.169 Uiso 1 1 calc R . . H5C H 0.8801 0.3851 0.0201 0.169 Uiso 1 1 calc R . . C6 C 0.7075(15) 0.1715(8) -0.2805(14) 0.123(10) Uani 1 1 d . . . H6A H 0.6629 0.1905 -0.2895 0.185 Uiso 1 1 calc R . . H6B H 0.6974 0.1437 -0.3324 0.185 Uiso 1 1 calc R . . H6C H 0.7452 0.1916 -0.2988 0.185 Uiso 1 1 calc R . . C7 C 0.9826(7) 0.1050(4) 0.2349(9) 0.034(3) Uani 1 1 d . . . C8 C 0.9280(6) 0.0243(4) 0.1599(8) 0.029(2) Uani 1 1 d . . . C9 C 0.9811(7) 0.0497(4) 0.2379(9) 0.031(3) Uani 1 1 d . . . C10 C 1.0368(6) 0.0249(4) 0.3181(9) 0.029(2) Uani 1 1 d . . . C11 C 0.8938(14) 0.0697(10) -0.0470(17) 0.129(10) Uani 1 1 d . . . H11A H 0.9246 0.0987 -0.0336 0.193 Uiso 1 1 calc R . . H11B H 0.8541 0.0741 -0.1165 0.193 Uiso 1 1 calc R . . H11C H 0.9232 0.0417 -0.0562 0.193 Uiso 1 1 calc R . . C12 C 1.1674(10) 0.0797(8) 0.3532(18) 0.095(7) Uani 1 1 d . . . H12A H 1.1979 0.0525 0.3423 0.143 Uiso 1 1 calc R . . H12B H 1.1982 0.1046 0.3997 0.143 Uiso 1 1 calc R . . H12C H 1.1423 0.0933 0.2786 0.143 Uiso 1 1 calc R . . C13 C 0.8910(7) 0.2111(4) 0.5191(9) 0.039(3) Uani 1 1 d . . . C14 C 0.8101(7) 0.2748(4) 0.5661(9) 0.033(3) Uani 1 1 d . . . C15 C 0.8179(7) 0.2317(4) 0.5092(10) 0.039(3) Uani 1 1 d . . . C16 C 0.7582(7) 0.2065(4) 0.4437(9) 0.029(2) Uani 1 1 d . . . C17 C 0.9219(17) 0.3360(13) 0.555(2) 0.21(2) Uani 1 1 d . . . H17A H 0.8904 0.3641 0.5295 0.309 Uiso 1 1 calc R . . H17B H 0.9210 0.3154 0.4886 0.309 Uiso 1 1 calc R . . H17C H 0.9718 0.3469 0.5891 0.309 Uiso 1 1 calc R . . C18 C 0.7781(10) 0.1751(6) 0.2419(11) 0.067(5) Uani 1 1 d . . . H18A H 0.7328 0.1921 0.2049 0.100 Uiso 1 1 calc R . . H18B H 0.7855 0.1485 0.1930 0.100 Uiso 1 1 calc R . . H18C H 0.8191 0.1977 0.2539 0.100 Uiso 1 1 calc R . . O1 O 0.9233(6) 0.1916(4) -0.0120(9) 0.069(3) Uani 1 1 d . . . O2 O 0.9444(4) 0.1279(3) 0.2848(6) 0.0336(19) Uani 1 1 d . . . O3 O 1.0225(5) 0.1227(3) 0.1780(7) 0.039(2) Uani 1 1 d . . . O4 O 0.9187(5) 0.2149(4) 0.4364(7) 0.048(2) Uani 1 1 d . . . O5 O 0.9212(5) 0.1858(3) 0.6101(6) 0.0360(19) Uani 1 1 d . . . O6 O 1.1320(6) 0.2214(4) 0.1787(9) 0.068(3) Uani 1 1 d . . . Pb1 Pb 1.0000 0.14418(2) 0.5000 0.03130(18) Uani 1 2 d S . . Pb2 Pb 1.01020(3) 0.206479(15) 0.18998(3) 0.03355(16) Uani 1 1 d . . . S1 S 0.9031(2) 0.30473(13) 0.0670(4) 0.0580(10) Uani 1 1 d . . . S2 S 0.7392(2) 0.15018(13) -0.1325(3) 0.0525(10) Uani 1 1 d . . . S3 S 0.8583(2) 0.06061(11) 0.0666(3) 0.0457(8) Uani 1 1 d . . . S4 S 1.1014(2) 0.05904(12) 0.4246(3) 0.0545(10) Uani 1 1 d . . . S5 S 0.8899(2) 0.30284(12) 0.6567(3) 0.0476(9) Uani 1 1 d . . . S6 S 0.7723(2) 0.15144(11) 0.3783(3) 0.0440(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(9) 0.046(8) 0.066(10) -0.024(7) 0.016(8) 0.008(7) C2 0.038(8) 0.030(6) 0.031(6) 0.000(5) -0.001(5) 0.011(5) C3 0.038(7) 0.035(6) 0.014(4) 0.000(4) 0.001(5) 0.010(5) C4 0.043(8) 0.034(6) 0.010(4) 0.002(4) 0.004(4) 0.021(5) C5 0.080(16) 0.112(18) 0.14(2) 0.047(15) 0.019(14) -0.039(13) C6 0.20(3) 0.102(17) 0.041(10) -0.014(10) -0.013(13) 0.043(17) C7 0.034(7) 0.036(6) 0.025(5) -0.014(5) -0.006(5) 0.005(5) C8 0.028(7) 0.039(6) 0.014(4) 0.003(4) -0.002(4) 0.009(5) C9 0.050(8) 0.021(5) 0.026(5) 0.002(4) 0.015(5) 0.012(5) C10 0.030(7) 0.028(6) 0.026(5) 0.000(4) 0.003(5) 0.000(5) C11 0.15(2) 0.15(2) 0.079(15) 0.054(14) 0.007(15) 0.044(19) C12 0.042(11) 0.115(17) 0.123(17) -0.027(13) 0.013(11) -0.019(11) C13 0.045(8) 0.041(7) 0.020(5) -0.003(5) -0.009(5) 0.017(6) C14 0.040(8) 0.029(6) 0.028(5) 0.003(5) 0.003(5) 0.000(5) C15 0.044(8) 0.036(7) 0.033(6) 0.010(5) 0.003(6) 0.016(6) C16 0.032(7) 0.029(6) 0.023(5) 0.006(4) 0.000(5) 0.005(5) C17 0.23(4) 0.28(4) 0.093(17) 0.00(2) 0.02(2) -0.22(4) C18 0.097(14) 0.071(11) 0.026(7) -0.001(6) 0.005(8) 0.016(9) O1 0.045(7) 0.076(7) 0.067(7) -0.041(6) -0.017(5) 0.023(6) O2 0.029(5) 0.033(4) 0.035(4) -0.010(3) 0.002(4) 0.006(4) O3 0.043(6) 0.037(5) 0.036(4) 0.006(3) 0.010(4) 0.002(4) O4 0.033(6) 0.072(7) 0.040(5) 0.007(4) 0.012(4) 0.008(5) O5 0.034(5) 0.042(5) 0.027(4) 0.002(3) -0.001(4) 0.002(4) O6 0.079(9) 0.088(8) 0.055(6) -0.001(5) 0.048(6) -0.018(6) Pb1 0.0410(4) 0.0300(3) 0.0221(3) 0.000 0.0069(3) 0.000 Pb2 0.0419(3) 0.0254(2) 0.0263(2) -0.00083(16) -0.00329(18) -0.00354(19) S1 0.038(2) 0.0395(19) 0.091(3) -0.0049(18) 0.006(2) 0.0065(15) S2 0.063(3) 0.045(2) 0.0409(18) -0.0168(14) -0.0024(17) 0.0127(17) S3 0.052(2) 0.0304(16) 0.0437(17) -0.0025(13) -0.0062(16) 0.0101(14) S4 0.063(3) 0.0316(16) 0.0478(19) -0.0082(14) -0.0231(17) 0.0047(16) S5 0.037(2) 0.0436(19) 0.0501(19) -0.0038(15) -0.0101(15) 0.0022(15) S6 0.055(2) 0.0387(18) 0.0312(15) 0.0014(12) -0.0009(15) 0.0170(15) _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 C1 O1 1.220(17) . ? C1 O6 1.233(17) 2_755 ? C1 C3 1.544(18) . ? C2 C4 1.377(16) 7_655 ? C2 C3 1.442(15) . ? C2 S1 1.792(14) . ? C3 C4 1.379(17) . ? C4 C2 1.377(16) 7_655 ? C4 S2 1.767(11) . ? C5 S1 1.79(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 S2 1.834(18) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O2 1.236(13) . ? C7 O3 1.252(15) . ? C7 C9 1.532(16) . ? C8 C8 1.34(2) 6 ? C8 C9 1.381(16) . ? C8 S3 1.805(11) . ? C9 C10 1.414(15) . ? C10 C10 1.38(2) 6 ? C10 S4 1.799(11) . ? C11 S3 1.71(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 S4 1.80(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O4 1.255(15) . ? C13 O5 1.305(13) . ? C13 C15 1.479(18) . ? C13 Pb1 2.836(12) . ? C14 C16 1.376(17) 7_656 ? C14 C15 1.406(16) . ? C14 S5 1.800(12) . ? C15 C16 1.391(17) . ? C16 C14 1.376(17) 7_656 ? C16 S6 1.770(11) . ? C17 S5 1.77(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 S6 1.811(14) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O1 Pb2 2.602(10) . ? O2 Pb1 2.584(7) . ? O3 Pb2 2.340(8) . ? O4 Pb1 2.489(9) . ? O5 Pb2 2.498(7) 2_756 ? O5 Pb1 2.533(8) . ? O6 C1 1.233(17) 2_755 ? O6 Pb2 2.393(11) . ? Pb1 O4 2.489(9) 2_756 ? Pb1 O5 2.533(8) 2_756 ? Pb1 O2 2.584(7) 2_756 ? Pb1 C13 2.836(12) 2_756 ? Pb2 O5 2.498(7) 2_756 ? 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 O1 C1 O6 125.3(14) . 2_755 ? O1 C1 C3 119.9(14) . . ? O6 C1 C3 114.7(13) 2_755 . ? C4 C2 C3 119.1(11) 7_655 . ? C4 C2 S1 122.8(9) 7_655 . ? C3 C2 S1 118.1(9) . . ? C4 C3 C2 120.9(10) . . ? C4 C3 C1 120.6(10) . . ? C2 C3 C1 118.5(11) . . ? C2 C4 C3 119.9(10) 7_655 . ? C2 C4 S2 121.2(10) 7_655 . ? C3 C4 S2 118.9(8) . . ? S1 C5 H5A 109.5 . . ? S1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S2 C6 H6A 109.5 . . ? S2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O2 C7 O3 126.1(11) . . ? O2 C7 C9 119.0(11) . . ? O3 C7 C9 114.9(10) . . ? C8 C8 C9 120.7(6) 6 . ? C8 C8 S3 123.9(4) 6 . ? C9 C8 S3 115.4(8) . . ? C8 C9 C10 120.3(9) . . ? C8 C9 C7 120.6(10) . . ? C10 C9 C7 119.1(10) . . ? C10 C10 C9 119.1(6) 6 . ? C10 C10 S4 121.7(4) 6 . ? C9 C10 S4 119.1(8) . . ? S3 C11 H11A 109.5 . . ? S3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S4 C12 H12A 109.5 . . ? S4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 O5 122.5(11) . . ? O4 C13 C15 119.2(10) . . ? O5 C13 C15 118.1(11) . . ? O4 C13 Pb1 61.3(6) . . ? O5 C13 Pb1 63.3(6) . . ? C15 C13 Pb1 159.8(9) . . ? C16 C14 C15 119.9(11) 7_656 . ? C16 C14 S5 121.1(9) 7_656 . ? C15 C14 S5 118.9(10) . . ? C16 C15 C14 122.0(11) . . ? C16 C15 C13 117.5(11) . . ? C14 C15 C13 120.5(12) . . ? C14 C16 C15 118.1(10) 7_656 . ? C14 C16 S6 122.5(9) 7_656 . ? C15 C16 S6 119.4(9) . . ? S5 C17 H17A 109.5 . . ? S5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S6 C18 H18A 109.5 . . ? S6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 O1 Pb2 135.9(9) . . ? C7 O2 Pb1 116.5(7) . . ? C7 O3 Pb2 105.5(7) . . ? C13 O4 Pb1 92.5(7) . . ? C13 O5 Pb2 134.4(7) . 2_756 ? C13 O5 Pb1 89.3(7) . . ? Pb2 O5 Pb1 112.7(3) 2_756 . ? C1 O6 Pb2 101.5(10) 2_755 . ? O4 Pb1 O4 76.3(5) 2_756 . ? O4 Pb1 O5 53.1(3) 2_756 2_756 ? O4 Pb1 O5 83.4(3) . 2_756 ? O4 Pb1 O5 83.4(3) 2_756 . ? O4 Pb1 O5 53.1(3) . . ? O5 Pb1 O5 125.8(4) 2_756 . ? O4 Pb1 O2 76.6(3) 2_756 2_756 ? O4 Pb1 O2 120.4(3) . 2_756 ? O5 Pb1 O2 118.0(2) 2_756 2_756 ? O5 Pb1 O2 71.9(3) . 2_756 ? O4 Pb1 O2 120.4(3) 2_756 . ? O4 Pb1 O2 76.6(3) . . ? O5 Pb1 O2 71.9(3) 2_756 . ? O5 Pb1 O2 118.0(2) . . ? O2 Pb1 O2 160.0(3) 2_756 . ? O4 Pb1 C13 82.5(4) 2_756 . ? O4 Pb1 C13 26.2(3) . . ? O5 Pb1 C13 107.1(3) 2_756 . ? O5 Pb1 C13 27.4(3) . . ? O2 Pb1 C13 98.3(3) 2_756 . ? O2 Pb1 C13 94.7(3) . . ? O4 Pb1 C13 26.2(3) 2_756 2_756 ? O4 Pb1 C13 82.5(4) . 2_756 ? O5 Pb1 C13 27.4(3) 2_756 2_756 ? O5 Pb1 C13 107.1(3) . 2_756 ? O2 Pb1 C13 94.7(3) 2_756 2_756 ? O2 Pb1 C13 98.3(3) . 2_756 ? C13 Pb1 C13 98.5(6) . 2_756 ? O3 Pb2 O6 93.0(4) . . ? O3 Pb2 O5 78.3(3) . 2_756 ? O6 Pb2 O5 80.2(3) . 2_756 ? O3 Pb2 O1 80.4(3) . . ? O6 Pb2 O1 111.0(4) . . ? O5 Pb2 O1 156.5(3) 2_756 . ? C5 S1 C2 101.3(8) . . ? C4 S2 C6 99.4(8) . . ? C11 S3 C8 102.0(8) . . ? C12 S4 C10 104.7(7) . . ? C17 S5 C14 100.8(9) . . ? C16 S6 C18 98.6(6) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 8.559 _refine_diff_density_min -1.624 _refine_diff_density_rms 0.331 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.047 839 658 ' ' 2 0.000 0.500 -0.014 839 658 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_PLAT220_1HgCl2 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.50 Ratio RESPONSE: The methyl groups of the S-Me groups show a larger degree of thermal motion than the atoms of the core framework. ; _vrf_PLAT242_1HgCl2 ; PROBLEM: Check Low Ueq as Compared to Neighbors for S5 RESPONSE: The methyl groups of the S-Me groups show a larger degree of thermal motion than the atoms of the core framework. ; # end Validation Reply Form # Attachment '1_and_1HgCl2_rev.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 733811' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 O12 Pb3 S12, 2(C4 H9 N O), 0.8(H2 O)' _chemical_formula_sum 'C44 H55.60 N2 O14.80 Pb3 S12' _chemical_formula_weight 1855.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.8996(12) _cell_length_b 27.0362(17) _cell_length_c 12.2604(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.8960(10) _cell_angle_gamma 90.00 _cell_volume 6162.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7287 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 30.51 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3560 _exptl_absorpt_coefficient_mu 8.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.177 _exptl_absorpt_correction_T_max 0.274 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; The solvate water molecule is only partially occupied with a refined occupancy of 0.80(2). The position of its hydrogen atom was restrained so as to make sense based onm hydrogen bonding considerations. ; _diffrn_ambient_temperature 100(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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 25561 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7653 _reflns_number_gt 6590 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART 5.630 (Bruker, 1997-2002)' _computing_cell_refinement 'SAINT+ 6.45 (Bruker, 2003)' _computing_data_reduction 'SAINT+ 6.45' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0461P)^2^+0.2303P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7653 _refine_ls_number_parameters 357 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.003 _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 C1 C 0.1307(2) 0.78392(18) 0.7971(4) 0.0209(10) Uani 1 1 d . . . C2 C 0.1921(2) 0.76730(19) 0.9063(4) 0.0196(10) Uani 1 1 d . . . C3 C 0.2550(2) 0.79560(18) 0.9474(4) 0.0190(10) Uani 1 1 d . . . C4 C 0.1858(2) 0.72200(19) 0.9571(4) 0.0206(10) Uani 1 1 d . . . C5 C 0.3021(3) 0.8328(3) 0.7793(5) 0.0364(14) Uani 1 1 d . . . H5A H 0.3470 0.8156 0.8235 0.055 Uiso 1 1 calc R . . H5B H 0.3129 0.8617 0.7401 0.055 Uiso 1 1 calc R . . H5C H 0.2704 0.8103 0.7208 0.055 Uiso 1 1 calc R . . C6 C 0.1244(3) 0.6368(2) 0.8273(5) 0.0379(14) Uani 1 1 d . . . H6A H 0.1382 0.6491 0.7631 0.057 Uiso 1 1 calc R . . H6B H 0.0822 0.6154 0.7961 0.057 Uiso 1 1 calc R . . H6C H 0.1644 0.6180 0.8818 0.057 Uiso 1 1 calc R . . C7 C -0.0130(2) 0.89321(19) 0.4984(4) 0.0195(10) Uani 1 1 d . . . C8 C -0.0074(2) 0.94900(18) 0.4959(4) 0.0182(9) Uani 1 1 d . . . C9 C 0.0509(2) 0.97085(18) 0.4741(4) 0.0181(9) Uani 1 1 d . . . C10 C 0.0582(2) 1.02227(19) 0.4789(4) 0.0186(9) Uani 1 1 d . . . C11 C 0.1741(3) 0.9113(2) 0.5680(4) 0.0281(12) Uani 1 1 d . . . H11A H 0.1976 0.9398 0.6160 0.042 Uiso 1 1 calc R . . H11B H 0.2104 0.8906 0.5533 0.042 Uiso 1 1 calc R . . H11C H 0.1490 0.8919 0.6091 0.042 Uiso 1 1 calc R . . C12 C 0.1082(3) 1.0502(3) 0.3047(5) 0.0365(14) Uani 1 1 d . . . H12A H 0.0983 1.0160 0.2778 0.055 Uiso 1 1 calc R . . H12B H 0.1474 1.0634 0.2827 0.055 Uiso 1 1 calc R . . H12C H 0.0649 1.0703 0.2685 0.055 Uiso 1 1 calc R . . C13 C 0.1057(2) 0.78411(18) 0.3782(4) 0.0203(10) Uani 1 1 d . . . C14 C 0.1803(2) 0.76500(18) 0.4418(4) 0.0184(9) Uani 1 1 d . . . C15 C 0.2369(2) 0.79284(18) 0.4294(4) 0.0186(9) Uani 1 1 d . . . C16 C 0.3082(2) 0.77725(19) 0.4897(4) 0.0197(10) Uani 1 1 d . . . C17 C 0.2093(3) 0.8227(2) 0.2035(4) 0.0324(13) Uani 1 1 d . . . H17A H 0.2538 0.8054 0.2099 0.049 Uiso 1 1 calc R . . H17B H 0.2008 0.8496 0.1466 0.049 Uiso 1 1 calc R . . H17C H 0.1689 0.7994 0.1778 0.049 Uiso 1 1 calc R . . C18 C 0.4095(4) 0.8476(3) 0.6033(7) 0.070(3) Uani 1 1 d . . . H18A H 0.3729 0.8731 0.5940 0.105 Uiso 1 1 calc R . . H18B H 0.4557 0.8634 0.6135 0.105 Uiso 1 1 calc R . . H18C H 0.4144 0.8274 0.6720 0.105 Uiso 1 1 calc R . . O1 O 0.07514(17) 0.80295(14) 0.8037(3) 0.0233(7) Uani 1 1 d . . . O2 O 0.13880(17) 0.77530(15) 0.7012(3) 0.0274(8) Uani 1 1 d . . . O3 O 0.02522(17) 0.87294(13) 0.5959(3) 0.0202(7) Uani 1 1 d . . . O4 O -0.05240(17) 0.86965(13) 0.4119(3) 0.0204(7) Uani 1 1 d . . . O5 O 0.07467(16) 0.80810(13) 0.4358(3) 0.0202(7) Uani 1 1 d . . . O6 O 0.07919(18) 0.77868(14) 0.2702(3) 0.0266(8) Uani 1 1 d . . . Pb1 Pb 0.014083(8) 0.789414(7) 0.579695(14) 0.01747(6) Uani 1 1 d . . . Pb2 Pb 0.0000 0.851443(10) 0.2500 0.01811(7) Uani 1 2 d S . . S1 S 0.25815(6) 0.85262(5) 0.87778(11) 0.0258(3) Uani 1 1 d . . . S2 S 0.10322(6) 0.68849(5) 0.90304(11) 0.0262(3) Uani 1 1 d . . . S3 S 0.11014(6) 0.93291(5) 0.43048(10) 0.0195(2) Uani 1 1 d . . . S4 S 0.13367(6) 1.05224(5) 0.46172(10) 0.0221(3) Uani 1 1 d . . . S5 S 0.21743(7) 0.84796(5) 0.34438(11) 0.0247(3) Uani 1 1 d . . . S6 S 0.38330(6) 0.80920(5) 0.47642(11) 0.0251(3) Uani 1 1 d . . . C19 C 0.0747(5) 0.4399(4) 0.5559(9) 0.088(3) Uani 1 1 d . . . H19A H 0.0957 0.4095 0.5389 0.133 Uiso 1 1 calc R . . H19B H 0.0601 0.4614 0.4871 0.133 Uiso 1 1 calc R . . H19C H 0.0325 0.4317 0.5760 0.133 Uiso 1 1 calc R . . C20 C 0.1309(6) 0.4669(4) 0.6598(10) 0.086(3) Uani 1 1 d . . . C21 C 0.2249(4) 0.5273(3) 0.7330(7) 0.064(2) Uani 1 1 d . . . H21A H 0.2091 0.5618 0.7214 0.096 Uiso 1 1 calc R . . H21B H 0.2736 0.5247 0.7310 0.096 Uiso 1 1 calc R . . H21C H 0.2250 0.5157 0.8087 0.096 Uiso 1 1 calc R . . C22 C 0.1773(6) 0.5056(5) 0.5222(8) 0.105(4) Uani 1 1 d . . . H22A H 0.1575 0.4766 0.4731 0.157 Uiso 1 1 calc R . . H22B H 0.2270 0.5110 0.5272 0.157 Uiso 1 1 calc R . . H22C H 0.1482 0.5348 0.4879 0.157 Uiso 1 1 calc R . . N1 N 0.1759(4) 0.4970(3) 0.6404(6) 0.0609(17) Uani 1 1 d . . . O7 O 0.1303(5) 0.4624(3) 0.7588(6) 0.129(3) Uani 1 1 d D . . O8 O 0.0000 0.5225(7) 0.7500 0.113(6) Uani 0.80(2) 2 d SPD . . H8A H 0.034(6) 0.510(5) 0.730(9) 0.170 Uiso 0.80(2) 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(2) 0.025(3) 0.017(2) 0.0018(19) 0.0059(18) -0.0030(19) C2 0.019(2) 0.027(3) 0.015(2) 0.0027(19) 0.0078(17) 0.0033(19) C3 0.018(2) 0.027(3) 0.014(2) 0.0031(18) 0.0079(18) 0.0072(19) C4 0.022(2) 0.025(3) 0.016(2) 0.0008(19) 0.0085(19) 0.0038(19) C5 0.032(3) 0.055(4) 0.029(3) 0.011(3) 0.019(2) 0.010(3) C6 0.043(3) 0.038(4) 0.032(3) -0.006(3) 0.013(3) -0.004(3) C7 0.017(2) 0.030(3) 0.015(2) -0.0030(19) 0.0098(18) 0.0003(19) C8 0.020(2) 0.023(3) 0.011(2) 0.0014(17) 0.0028(17) 0.0028(18) C9 0.018(2) 0.021(3) 0.015(2) 0.0010(18) 0.0066(17) 0.0010(18) C10 0.017(2) 0.026(3) 0.013(2) 0.0011(18) 0.0057(17) -0.0019(19) C11 0.023(2) 0.040(3) 0.019(2) 0.001(2) 0.0046(19) 0.008(2) C12 0.039(3) 0.050(4) 0.024(3) 0.006(3) 0.014(2) -0.008(3) C13 0.016(2) 0.028(3) 0.019(2) 0.0027(19) 0.0087(18) 0.0030(19) C14 0.016(2) 0.024(3) 0.016(2) -0.0025(19) 0.0074(17) 0.0034(18) C15 0.019(2) 0.025(3) 0.014(2) 0.0009(18) 0.0076(18) 0.0058(19) C16 0.016(2) 0.025(3) 0.020(2) -0.0010(19) 0.0091(18) 0.0016(19) C17 0.033(3) 0.048(4) 0.020(2) 0.004(2) 0.014(2) 0.007(3) C18 0.076(5) 0.083(6) 0.071(5) -0.049(5) 0.051(4) -0.054(5) O1 0.0182(16) 0.034(2) 0.0205(17) 0.0069(15) 0.0097(13) 0.0042(14) O2 0.0199(16) 0.047(2) 0.0140(16) 0.0035(16) 0.0048(13) 0.0084(16) O3 0.0221(16) 0.023(2) 0.0147(15) -0.0005(13) 0.0056(13) 0.0011(14) O4 0.0195(15) 0.025(2) 0.0150(15) -0.0022(14) 0.0041(13) -0.0002(14) O5 0.0166(15) 0.028(2) 0.0173(16) 0.0034(14) 0.0076(13) 0.0022(14) O6 0.0213(16) 0.042(2) 0.0155(16) -0.0021(15) 0.0058(13) 0.0055(15) Pb1 0.01685(9) 0.02218(11) 0.01356(9) 0.00069(6) 0.00565(7) -0.00013(6) Pb2 0.01889(12) 0.02394(15) 0.01075(11) 0.000 0.00438(9) 0.000 S1 0.0247(6) 0.0326(8) 0.0210(6) 0.0091(5) 0.0093(5) 0.0049(5) S2 0.0182(5) 0.0305(7) 0.0261(6) 0.0026(5) 0.0031(5) 0.0001(5) S3 0.0198(5) 0.0235(7) 0.0171(5) 0.0001(5) 0.0088(4) 0.0030(5) S4 0.0198(5) 0.0265(7) 0.0222(6) -0.0018(5) 0.0100(5) -0.0026(5) S5 0.0263(6) 0.0277(7) 0.0226(6) 0.0063(5) 0.0115(5) 0.0068(5) S6 0.0191(5) 0.0334(8) 0.0251(6) 0.0032(5) 0.0106(5) -0.0017(5) C19 0.082(7) 0.093(8) 0.081(7) -0.025(6) 0.018(5) -0.012(6) C20 0.113(8) 0.071(7) 0.103(8) -0.020(6) 0.076(7) -0.018(6) C21 0.069(5) 0.051(5) 0.074(6) 0.003(4) 0.026(4) -0.005(4) C22 0.108(8) 0.147(12) 0.075(7) 0.026(7) 0.052(6) 0.011(7) N1 0.070(4) 0.056(4) 0.063(4) -0.001(3) 0.032(3) 0.001(3) O7 0.187(9) 0.143(8) 0.071(5) -0.016(5) 0.065(5) -0.067(6) O8 0.084(10) 0.151(16) 0.099(11) 0.000 0.025(8) 0.000 _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 C1 O1 1.249(6) . ? C1 O2 1.263(6) . ? C1 C2 1.523(6) . ? C1 Pb1 2.846(5) . ? C2 C3 1.399(7) . ? C2 C4 1.400(7) . ? C3 C4 1.415(6) 7_567 ? C3 S1 1.774(5) . ? C4 C3 1.415(6) 7_567 ? C4 S2 1.784(5) . ? C5 S1 1.807(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 S2 1.809(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O4 1.245(6) . ? C7 O3 1.288(5) . ? C7 C8 1.514(7) . ? C8 C10 1.393(6) 5_576 ? C8 C9 1.410(6) . ? C9 C10 1.397(7) . ? C9 S3 1.783(5) . ? C10 C8 1.393(6) 5_576 ? C10 S4 1.784(5) . ? C11 S3 1.809(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 S4 1.808(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O6 1.248(6) . ? C13 O5 1.269(6) . ? C13 C14 1.501(6) . ? C13 Pb2 2.802(5) . ? C14 C16 1.387(7) 7_566 ? C14 C15 1.407(6) . ? C15 C16 1.412(6) . ? C15 S5 1.780(5) . ? C16 C14 1.387(7) 7_566 ? C16 S6 1.783(5) . ? C17 S5 1.810(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 S6 1.786(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O1 Pb1 2.602(3) . ? O1 Pb1 2.672(3) 2_556 ? O2 Pb1 2.426(3) . ? O3 Pb1 2.271(4) . ? O4 Pb2 2.598(3) . ? O5 Pb1 2.518(3) . ? O5 Pb2 2.521(3) . ? O6 Pb2 2.477(4) . ? Pb1 O1 2.672(3) 2_556 ? Pb2 O6 2.477(4) 2 ? Pb2 O5 2.521(3) 2 ? Pb2 O4 2.598(3) 2 ? Pb2 C13 2.802(5) 2 ? C19 C20 1.546(13) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O7 1.226(11) . ? C20 N1 1.292(11) . ? C21 N1 1.456(10) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N1 1.478(10) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O8 H8A 0.87(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 O1 C1 O2 123.1(4) . . ? O1 C1 C2 121.0(4) . . ? O2 C1 C2 115.8(4) . . ? O1 C1 Pb1 66.0(3) . . ? O2 C1 Pb1 58.0(2) . . ? C2 C1 Pb1 165.7(3) . . ? C3 C2 C4 121.9(4) . . ? C3 C2 C1 119.3(4) . . ? C4 C2 C1 118.6(4) . . ? C2 C3 C4 119.2(4) . 7_567 ? C2 C3 S1 118.9(3) . . ? C4 C3 S1 121.9(4) 7_567 . ? C2 C4 C3 118.8(4) . 7_567 ? C2 C4 S2 119.7(3) . . ? C3 C4 S2 121.4(4) 7_567 . ? S1 C5 H5A 109.5 . . ? S1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S2 C6 H6A 109.5 . . ? S2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 O3 123.8(5) . . ? O4 C7 C8 121.4(4) . . ? O3 C7 C8 114.8(4) . . ? C10 C8 C9 121.3(4) 5_576 . ? C10 C8 C7 119.1(4) 5_576 . ? C9 C8 C7 119.5(4) . . ? C10 C9 C8 119.3(4) . . ? C10 C9 S3 121.0(3) . . ? C8 C9 S3 119.5(4) . . ? C8 C10 C9 119.4(4) 5_576 . ? C8 C10 S4 118.7(4) 5_576 . ? C9 C10 S4 121.8(3) . . ? S3 C11 H11A 109.5 . . ? S3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S4 C12 H12A 109.5 . . ? S4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O6 C13 O5 123.0(4) . . ? O6 C13 C14 118.5(4) . . ? O5 C13 C14 118.3(4) . . ? O6 C13 Pb2 62.1(3) . . ? O5 C13 Pb2 64.1(2) . . ? C14 C13 Pb2 157.0(3) . . ? C16 C14 C15 122.8(4) 7_566 . ? C16 C14 C13 121.1(4) 7_566 . ? C15 C14 C13 116.1(4) . . ? C14 C15 C16 118.5(4) . . ? C14 C15 S5 119.8(3) . . ? C16 C15 S5 121.6(4) . . ? C14 C16 C15 118.7(4) 7_566 . ? C14 C16 S6 119.5(3) 7_566 . ? C15 C16 S6 121.8(4) . . ? S5 C17 H17A 109.5 . . ? S5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S6 C18 H18A 109.5 . . ? S6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 O1 Pb1 88.0(3) . . ? C1 O1 Pb1 138.7(3) . 2_556 ? Pb1 O1 Pb1 113.34(12) . 2_556 ? C1 O2 Pb1 95.8(3) . . ? C7 O3 Pb1 109.6(3) . . ? C7 O4 Pb2 116.5(3) . . ? C13 O5 Pb1 137.4(3) . . ? C13 O5 Pb2 89.0(3) . . ? Pb1 O5 Pb2 116.82(12) . . ? C13 O6 Pb2 91.5(3) . . ? O3 Pb1 O2 93.21(13) . . ? O3 Pb1 O5 78.79(11) . . ? O2 Pb1 O5 79.71(10) . . ? O3 Pb1 O1 76.91(11) . . ? O2 Pb1 O1 51.96(10) . . ? O5 Pb1 O1 123.46(10) . . ? O3 Pb1 O1 83.09(11) . 2_556 ? O2 Pb1 O1 114.98(10) . 2_556 ? O5 Pb1 O1 157.37(12) . 2_556 ? O1 Pb1 O1 64.24(12) . 2_556 ? O3 Pb1 C1 87.04(13) . . ? O2 Pb1 C1 26.20(12) . . ? O5 Pb1 C1 103.43(12) . . ? O1 Pb1 C1 26.00(12) . . ? O1 Pb1 C1 88.96(12) 2_556 . ? O6 Pb2 O6 74.85(17) 2 . ? O6 Pb2 O5 52.53(11) 2 2 ? O6 Pb2 O5 82.53(11) . 2 ? O6 Pb2 O5 82.53(11) 2 . ? O6 Pb2 O5 52.52(11) . . ? O5 Pb2 O5 124.59(16) 2 . ? O6 Pb2 O4 79.19(11) 2 . ? O6 Pb2 O4 119.25(11) . . ? O5 Pb2 O4 120.71(10) 2 . ? O5 Pb2 O4 70.46(10) . . ? O6 Pb2 O4 119.25(11) 2 2 ? O6 Pb2 O4 79.19(11) . 2 ? O5 Pb2 O4 70.46(10) 2 2 ? O5 Pb2 O4 120.71(10) . 2 ? O4 Pb2 O4 158.15(16) . 2 ? O6 Pb2 C13 26.43(12) 2 2 ? O6 Pb2 C13 82.16(13) . 2 ? O5 Pb2 C13 26.92(12) 2 2 ? O5 Pb2 C13 106.71(13) . 2 ? O4 Pb2 C13 97.26(12) . 2 ? O4 Pb2 C13 96.89(12) 2 2 ? O6 Pb2 C13 82.16(13) 2 . ? O6 Pb2 C13 26.43(12) . . ? O5 Pb2 C13 106.71(13) 2 . ? O5 Pb2 C13 26.92(12) . . ? O4 Pb2 C13 96.89(12) . . ? O4 Pb2 C13 97.26(12) 2 . ? C13 Pb2 C13 99.0(2) 2 . ? C3 S1 C5 99.9(3) . . ? C4 S2 C6 103.3(3) . . ? C4 S2 N1 104.44(17) . . ? C9 S3 C11 103.1(2) . . ? C10 S4 C12 100.6(2) . . ? C15 S5 C17 99.7(3) . . ? C16 S6 C18 101.3(3) . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O7 C20 N1 119.9(10) . . ? O7 C20 C19 120.5(9) . . ? N1 C20 C19 119.5(9) . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 H22A 109.5 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 N1 C21 121.7(8) . . ? C20 N1 C22 122.4(9) . . ? C21 N1 C22 115.8(8) . . ? C20 N1 S2 96.8(5) . . ? C21 N1 S2 51.2(4) . . ? C22 N1 S2 116.4(6) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -105.5(5) . . . . ? O2 C1 C2 C3 77.4(6) . . . . ? Pb1 C1 C2 C3 138.4(11) . . . . ? O1 C1 C2 C4 79.5(6) . . . . ? O2 C1 C2 C4 -97.7(5) . . . . ? Pb1 C1 C2 C4 -36.6(15) . . . . ? C4 C2 C3 C4 0.2(8) . . . 7_567 ? C1 C2 C3 C4 -174.7(4) . . . 7_567 ? C4 C2 C3 S1 -179.9(4) . . . . ? C1 C2 C3 S1 5.2(6) . . . . ? C3 C2 C4 C3 -0.2(8) . . . 7_567 ? C1 C2 C4 C3 174.7(4) . . . 7_567 ? C3 C2 C4 S2 178.3(4) . . . . ? C1 C2 C4 S2 -6.8(6) . . . . ? O4 C7 C8 C10 85.0(5) . . . 5_576 ? O3 C7 C8 C10 -94.5(5) . . . 5_576 ? O4 C7 C8 C9 -98.2(5) . . . . ? O3 C7 C8 C9 82.2(5) . . . . ? C10 C8 C9 C10 0.6(7) 5_576 . . . ? C7 C8 C9 C10 -176.2(4) . . . . ? C10 C8 C9 S3 -174.8(3) 5_576 . . . ? C7 C8 C9 S3 8.5(6) . . . . ? C8 C9 C10 C8 -0.5(7) . . . 5_576 ? S3 C9 C10 C8 174.8(3) . . . 5_576 ? C8 C9 C10 S4 175.9(3) . . . . ? S3 C9 C10 S4 -8.8(6) . . . . ? O6 C13 C14 C16 -106.6(5) . . . 7_566 ? O5 C13 C14 C16 78.3(6) . . . 7_566 ? Pb2 C13 C14 C16 168.3(6) . . . 7_566 ? O6 C13 C14 C15 74.5(6) . . . . ? O5 C13 C14 C15 -100.5(5) . . . . ? Pb2 C13 C14 C15 -10.6(10) . . . . ? C16 C14 C15 C16 -0.4(8) 7_566 . . . ? C13 C14 C15 C16 178.4(4) . . . . ? C16 C14 C15 S5 -177.5(4) 7_566 . . . ? C13 C14 C15 S5 1.3(6) . . . . ? C14 C15 C16 C14 0.4(7) . . . 7_566 ? S5 C15 C16 C14 177.4(3) . . . 7_566 ? C14 C15 C16 S6 178.4(3) . . . . ? S5 C15 C16 S6 -4.6(6) . . . . ? O2 C1 O1 Pb1 11.0(5) . . . . ? C2 C1 O1 Pb1 -166.0(4) . . . . ? O2 C1 O1 Pb1 135.1(4) . . . 2_556 ? C2 C1 O1 Pb1 -41.9(7) . . . 2_556 ? Pb1 C1 O1 Pb1 124.1(4) . . . 2_556 ? O1 C1 O2 Pb1 -11.9(5) . . . . ? C2 C1 O2 Pb1 165.3(4) . . . . ? O4 C7 O3 Pb1 3.3(5) . . . . ? C8 C7 O3 Pb1 -177.2(3) . . . . ? O3 C7 O4 Pb2 -98.9(4) . . . . ? C8 C7 O4 Pb2 81.6(4) . . . . ? O6 C13 O5 Pb1 109.8(5) . . . . ? C14 C13 O5 Pb1 -75.4(6) . . . . ? Pb2 C13 O5 Pb1 130.4(4) . . . . ? O6 C13 O5 Pb2 -20.6(5) . . . . ? C14 C13 O5 Pb2 154.3(4) . . . . ? O5 C13 O6 Pb2 21.0(5) . . . . ? C14 C13 O6 Pb2 -153.9(4) . . . . ? C7 O3 Pb1 O2 143.3(3) . . . . ? C7 O3 Pb1 O5 64.5(3) . . . . ? C7 O3 Pb1 O1 -167.0(3) . . . . ? C7 O3 Pb1 O1 -101.9(3) . . . 2_556 ? C7 O3 Pb1 C1 168.8(3) . . . . ? C1 O2 Pb1 O3 76.6(3) . . . . ? C1 O2 Pb1 O5 154.6(3) . . . . ? C1 O2 Pb1 O1 6.0(3) . . . . ? C1 O2 Pb1 O1 -7.2(3) . . . 2_556 ? C13 O5 Pb1 O3 167.8(4) . . . . ? Pb2 O5 Pb1 O3 -70.80(15) . . . . ? C13 O5 Pb1 O2 72.4(4) . . . . ? Pb2 O5 Pb1 O2 -166.20(18) . . . . ? C13 O5 Pb1 O1 101.8(4) . . . . ? Pb2 O5 Pb1 O1 -136.74(13) . . . . ? C13 O5 Pb1 O1 -154.8(4) . . . 2_556 ? Pb2 O5 Pb1 O1 -33.4(4) . . . 2_556 ? C13 O5 Pb1 C1 83.6(4) . . . . ? Pb2 O5 Pb1 C1 -154.98(15) . . . . ? C1 O1 Pb1 O3 -110.8(3) . . . . ? Pb1 O1 Pb1 O3 105.69(15) 2_556 . . . ? C1 O1 Pb1 O2 -6.1(3) . . . . ? Pb1 O1 Pb1 O2 -149.5(2) 2_556 . . . ? C1 O1 Pb1 O5 -44.0(3) . . . . ? Pb1 O1 Pb1 O5 172.56(11) 2_556 . . . ? C1 O1 Pb1 O1 160.6(3) . . . 2_556 ? Pb1 O1 Pb1 O1 17.11(17) 2_556 . . 2_556 ? Pb1 O1 Pb1 C1 -143.5(4) 2_556 . . . ? O1 C1 Pb1 O3 65.7(3) . . . . ? O2 C1 Pb1 O3 -103.4(3) . . . . ? C2 C1 Pb1 O3 -171.6(13) . . . . ? O1 C1 Pb1 O2 169.1(5) . . . . ? C2 C1 Pb1 O2 -68.2(12) . . . . ? O1 C1 Pb1 O5 143.5(3) . . . . ? O2 C1 Pb1 O5 -25.7(3) . . . . ? C2 C1 Pb1 O5 -93.9(13) . . . . ? O2 C1 Pb1 O1 -169.1(5) . . . . ? C2 C1 Pb1 O1 122.6(14) . . . . ? O1 C1 Pb1 O1 -17.4(2) . . . 2_556 ? O2 C1 Pb1 O1 173.4(3) . . . 2_556 ? C2 C1 Pb1 O1 105.2(13) . . . 2_556 ? C13 O6 Pb2 O6 -103.1(3) . . . 2 ? C13 O6 Pb2 O5 -156.3(3) . . . 2 ? C13 O6 Pb2 O5 -11.0(3) . . . . ? C13 O6 Pb2 O4 -35.1(3) . . . . ? C13 O6 Pb2 O4 132.3(3) . . . 2 ? C13 O6 Pb2 C13 -129.1(3) . . . 2 ? C13 O5 Pb2 O6 87.4(3) . . . 2 ? Pb1 O5 Pb2 O6 -57.37(15) . . . 2 ? C13 O5 Pb2 O6 10.8(3) . . . . ? Pb1 O5 Pb2 O6 -134.0(2) . . . . ? C13 O5 Pb2 O5 54.1(3) . . . 2 ? Pb1 O5 Pb2 O5 -90.67(14) . . . 2 ? C13 O5 Pb2 O4 168.5(3) . . . . ? Pb1 O5 Pb2 O4 23.76(14) . . . . ? C13 O5 Pb2 O4 -32.3(3) . . . 2 ? Pb1 O5 Pb2 O4 -177.06(12) . . . 2 ? C13 O5 Pb2 C13 76.6(3) . . . 2 ? Pb1 O5 Pb2 C13 -68.15(17) . . . 2 ? Pb1 O5 Pb2 C13 -144.7(4) . . . . ? C7 O4 Pb2 O6 149.7(4) . . . 2 ? C7 O4 Pb2 O6 84.0(4) . . . . ? C7 O4 Pb2 O5 -176.8(3) . . . 2 ? C7 O4 Pb2 O5 63.9(4) . . . . ? C7 O4 Pb2 O4 -60.9(3) . . . 2 ? C7 O4 Pb2 C13 169.1(4) . . . 2 ? C7 O4 Pb2 C13 69.1(4) . . . . ? O6 C13 Pb2 O6 71.6(3) . . . 2 ? O5 C13 Pb2 O6 -88.9(3) . . . 2 ? C14 C13 Pb2 O6 169.2(8) . . . 2 ? O5 C13 Pb2 O6 -160.5(5) . . . . ? C14 C13 Pb2 O6 97.6(8) . . . . ? O6 C13 Pb2 O5 24.6(3) . . . 2 ? O5 C13 Pb2 O5 -135.9(3) . . . 2 ? C14 C13 Pb2 O5 122.2(8) . . . 2 ? O6 C13 Pb2 O5 160.5(5) . . . . ? C14 C13 Pb2 O5 -101.9(9) . . . . ? O6 C13 Pb2 O4 149.6(3) . . . . ? O5 C13 Pb2 O4 -10.9(3) . . . . ? C14 C13 Pb2 O4 -112.8(8) . . . . ? O6 C13 Pb2 O4 -47.1(3) . . . 2 ? O5 C13 Pb2 O4 152.4(3) . . . 2 ? C14 C13 Pb2 O4 50.5(8) . . . 2 ? O6 C13 Pb2 C13 51.1(2) . . . 2 ? O5 C13 Pb2 C13 -109.4(3) . . . 2 ? C14 C13 Pb2 C13 148.7(9) . . . 2 ? C2 C3 S1 C5 -96.6(4) . . . . ? C4 C3 S1 C5 83.4(4) 7_567 . . . ? C2 C4 S2 C6 107.8(4) . . . . ? C3 C4 S2 C6 -73.7(4) 7_567 . . . ? C2 C4 S2 N1 109.5(4) . . . . ? C3 C4 S2 N1 -72.1(4) 7_567 . . . ? C10 C9 S3 C11 99.4(4) . . . . ? C8 C9 S3 C11 -85.3(4) . . . . ? C8 C10 S4 C12 -104.4(4) 5_576 . . . ? C9 C10 S4 C12 79.2(4) . . . . ? C14 C15 S5 C17 -91.0(4) . . . . ? C16 C15 S5 C17 92.0(4) . . . . ? C14 C16 S6 C18 -84.7(5) 7_566 . . . ? C15 C16 S6 C18 97.4(5) . . . . ? O7 C20 N1 C21 -2.2(16) . . . . ? C19 C20 N1 C21 173.4(8) . . . . ? O7 C20 N1 C22 -177.4(10) . . . . ? C19 C20 N1 C22 -1.8(15) . . . . ? O7 C20 N1 S2 -50.2(12) . . . . ? C19 C20 N1 S2 125.3(8) . . . . ? C4 S2 N1 C20 149.5(7) . . . . ? C6 S2 N1 C20 -156(7) . . . . ? C4 S2 N1 C21 23.7(5) . . . . ? C6 S2 N1 C21 78(6) . . . . ? C4 S2 N1 C22 -79.2(6) . . . . ? C6 S2 N1 C22 -24(6) . . . . ? N1 C20 O7 H8A 101(5) . . . . ? C19 C20 O7 H8A -74(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8A O7 0.87(2) 2.23(2) 3.028(15) 153(6) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.272 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.251