# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H48 Ag2 I9 La O8 Pb2 S8' _chemical_formula_sum 'C16 H48 Ag2 I9 La O8 Pb2 S8' _chemical_formula_weight 2536.15 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' Ag Ag -0.8971 1.1015 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 24.102(2) _cell_length_b 11.0566(9) _cell_length_c 21.667(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.299(3) _cell_angle_gamma 90.00 _cell_volume 5773.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13537 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4512 _exptl_absorpt_coefficient_mu 12.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1193 _exptl_absorpt_correction_T_max 0.1297 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14388 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5255 _reflns_number_gt 4583 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0804P)^2^+300.9778P] 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 5255 _refine_ls_number_parameters 147 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1529 _refine_ls_wR_factor_gt 0.1472 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _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 Pb1 Pb 0.20899(2) 0.48332(5) 0.01092(3) 0.03858(19) Uani 1 1 d . . . Ag1 Ag 0.27735(9) 0.24949(14) 0.09578(8) 0.0524(5) Uani 1 1 d . . . La1 La 1.0000 0.99596(11) 0.2500 0.0587(3) Uani 1 2 d SD . . I1 I 0.16981(4) 0.19146(9) 0.02406(5) 0.0454(3) Uani 1 1 d . . . I2 I 0.25564(5) 0.46720(10) 0.15012(5) 0.0540(3) Uani 1 1 d . . . I3 I 0.09192(5) 0.54769(12) 0.03984(7) 0.0666(4) Uani 1 1 d . . . I4 I 0.19461(6) 0.47316(10) -0.14065(6) 0.0569(3) Uani 1 1 d . . . I5 I 0.2500 0.7500 0.0000 0.0758(6) Uani 1 2 d S . . O1 O 0.9801(7) 0.8274(19) 0.1793(10) 0.090(3) Uani 1 1 d . . . O2 O 0.9087(7) 0.9191(17) 0.2800(8) 0.0930(17) Uani 1 1 d . . . O3 O 1.0627(7) 1.1709(19) 0.2435(13) 0.084(4) Uani 1 1 d . . . O4 O 0.9790(10) 1.060(3) 0.1447(9) 0.085(4) Uani 1 1 d D . . S1 S 0.9377(3) 0.7509(8) 0.1543(4) 0.116(3) Uani 1 1 d D . . S2 S 0.8920(3) 0.8239(7) 0.3210(3) 0.0930(17) Uani 1 1 d . . . S3 S 1.1020(3) 1.2206(8) 0.2110(6) 0.144(4) Uani 1 1 d . . . S4 S 0.9668(4) 1.1221(12) 0.0895(5) 0.161(4) Uani 1 1 d D . . C1 C 0.9531(11) 0.735(2) 0.0783(11) 0.116(3) Uani 1 1 d D . . H1A H 0.9435 0.8086 0.0564 0.174 Uiso 1 1 calc R . . H1B H 0.9322 0.6677 0.0612 0.174 Uiso 1 1 calc R . . H1C H 0.9925 0.7194 0.0739 0.174 Uiso 1 1 calc R . . C2 C 0.9593(11) 0.6164(18) 0.1839(12) 0.116(3) Uani 1 1 d D . . H2A H 0.9989 0.6199 0.1922 0.174 Uiso 1 1 calc R . . H2B H 0.9517 0.5524 0.1544 0.174 Uiso 1 1 calc R . . H2C H 0.9397 0.6001 0.2220 0.174 Uiso 1 1 calc R . . C3 C 0.8237(11) 0.783(3) 0.3018(13) 0.0930(17) Uani 1 1 d . . . H3A H 0.7997 0.8533 0.3059 0.139 Uiso 1 1 calc R . . H3B H 0.8113 0.7198 0.3292 0.139 Uiso 1 1 calc R . . H3C H 0.8225 0.7546 0.2595 0.139 Uiso 1 1 calc R . . C4 C 0.8787(11) 0.891(3) 0.3933(12) 0.0930(17) Uani 1 1 d . . . H4A H 0.9097 0.9420 0.4050 0.139 Uiso 1 1 calc R . . H4B H 0.8738 0.8280 0.4241 0.139 Uiso 1 1 calc R . . H4C H 0.8452 0.9393 0.3906 0.139 Uiso 1 1 calc R . . C5 C 1.1011(11) 1.374(3) 0.2053(19) 0.144(4) Uani 1 1 d . . . H5A H 1.0671 1.3999 0.1849 0.216 Uiso 1 1 calc R . . H5B H 1.1327 1.4013 0.1814 0.216 Uiso 1 1 calc R . . H5C H 1.1028 1.4098 0.2462 0.216 Uiso 1 1 calc R . . C6 C 1.1681(11) 1.202(3) 0.2397(19) 0.144(4) Uani 1 1 d . . . H6A H 1.1703 1.2363 0.2809 0.216 Uiso 1 1 calc R . . H6B H 1.1943 1.2428 0.2130 0.216 Uiso 1 1 calc R . . H6C H 1.1769 1.1165 0.2415 0.216 Uiso 1 1 calc R . . C7 C 0.9929(15) 1.267(2) 0.0830(18) 0.161(4) Uani 1 1 d D . . H7A H 1.0023 1.2975 0.1236 0.242 Uiso 1 1 calc R . . H7B H 0.9652 1.3187 0.0641 0.242 Uiso 1 1 calc R . . H7C H 1.0259 1.2654 0.0575 0.242 Uiso 1 1 calc R . . C8 C 0.8948(8) 1.134(4) 0.0823(18) 0.161(4) Uani 1 1 d D . . H8A H 0.8809 1.0681 0.0571 0.242 Uiso 1 1 calc R . . H8B H 0.8855 1.2106 0.0628 0.242 Uiso 1 1 calc R . . H8C H 0.8780 1.1304 0.1228 0.242 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0426(3) 0.0337(3) 0.0474(4) -0.0010(2) 0.0009(2) 0.0005(2) Ag1 0.0607(16) 0.0478(8) 0.0427(9) -0.0009(7) 0.0028(9) 0.0171(9) La1 0.0592(6) 0.0520(6) 0.0609(9) 0.033 -0.0128(6) 0.000 I1 0.0420(5) 0.0359(5) 0.0583(6) 0.0044(4) 0.0086(5) -0.0033(4) I2 0.0679(8) 0.0452(6) 0.0487(6) -0.0105(5) -0.0046(5) -0.0053(5) I3 0.0443(6) 0.0578(7) 0.0978(10) 0.0069(7) 0.0129(6) 0.0118(5) I4 0.0705(8) 0.0487(6) 0.0515(7) 0.0118(5) -0.0094(6) -0.0044(5) I5 0.0786(13) 0.0308(8) 0.1182(17) -0.0005(9) 0.0192(12) -0.0156(8) O1 0.071(4) 0.095(5) 0.102(7) -0.051(5) -0.017(4) -0.006(3) O2 0.088(4) 0.091(4) 0.101(4) 0.012(3) 0.017(3) 0.002(3) O3 0.068(4) 0.079(5) 0.095(10) 0.030(6) -0.026(5) -0.013(3) O4 0.080(6) 0.078(10) 0.095(9) 0.060(8) -0.030(6) -0.026(6) S1 0.071(4) 0.115(5) 0.162(7) -0.061(5) -0.017(4) -0.006(3) S2 0.088(4) 0.091(4) 0.101(4) 0.012(3) 0.017(3) 0.002(3) S3 0.068(4) 0.109(5) 0.255(10) 0.090(6) -0.026(5) -0.013(3) S4 0.110(6) 0.198(10) 0.175(9) 0.100(8) -0.030(6) -0.026(6) C1 0.071(4) 0.115(5) 0.162(7) -0.061(5) -0.017(4) -0.006(3) C2 0.071(4) 0.115(5) 0.162(7) -0.061(5) -0.017(4) -0.006(3) C3 0.088(4) 0.091(4) 0.101(4) 0.012(3) 0.017(3) 0.002(3) C4 0.088(4) 0.091(4) 0.101(4) 0.012(3) 0.017(3) 0.002(3) C5 0.068(4) 0.109(5) 0.255(10) 0.090(6) -0.026(5) -0.013(3) C6 0.068(4) 0.109(5) 0.255(10) 0.090(6) -0.026(5) -0.013(3) C7 0.110(6) 0.198(10) 0.175(9) 0.100(8) -0.030(6) -0.026(6) C8 0.110(6) 0.198(10) 0.175(9) 0.100(8) -0.030(6) -0.026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 I3 2.9798(13) . ? Pb1 I5 3.1193(6) . ? Pb1 I2 3.2181(13) . ? Pb1 I4 3.3023(14) . ? Pb1 I1 3.3747(11) . ? Pb1 Ag1 3.4767(17) 7 ? Ag1 I4 2.7305(19) 7 ? Ag1 I2 2.7313(19) . ? Ag1 I1 2.971(2) 7 ? Ag1 I1 3.083(2) . ? Ag1 Pb1 3.4767(17) 7 ? La1 O4 2.439(14) 2_755 ? La1 O4 2.439(14) . ? La1 O2 2.449(17) 2_755 ? La1 O2 2.449(17) . ? La1 O1 2.458(18) . ? La1 O1 2.458(17) 2_755 ? La1 O3 2.459(19) . ? La1 O3 2.459(19) 2_755 ? I1 Ag1 2.971(2) 7 ? I4 Ag1 2.7305(19) 7 ? I5 Pb1 3.1193(6) 7_565 ? O1 S1 1.430(17) . ? O2 S2 1.436(18) . ? O3 S3 1.31(2) . ? O4 S4 1.408(13) . ? S1 C1 1.70(3) . ? S1 C2 1.700(17) . ? S2 C3 1.75(3) . ? S2 C4 1.76(3) . ? S3 C5 1.71(3) . ? S3 C6 1.72(3) . ? S4 C7 1.725(18) . ? S4 C8 1.746(17) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? 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 I3 Pb1 I5 95.22(3) . . ? I3 Pb1 I2 98.21(4) . . ? I5 Pb1 I2 90.81(2) . . ? I3 Pb1 I4 97.05(4) . . ? I5 Pb1 I4 89.33(2) . . ? I2 Pb1 I4 164.67(4) . . ? I3 Pb1 I1 86.84(3) . . ? I5 Pb1 I1 177.73(3) . . ? I2 Pb1 I1 87.97(3) . . ? I4 Pb1 I1 91.34(3) . . ? I3 Pb1 Ag1 114.19(5) . 7 ? I5 Pb1 Ag1 128.20(4) . 7 ? I2 Pb1 Ag1 123.25(4) . 7 ? I4 Pb1 Ag1 47.42(3) . 7 ? I1 Pb1 Ag1 51.36(4) . 7 ? I4 Ag1 I2 133.53(8) 7 . ? I4 Ag1 I1 113.76(7) 7 7 ? I2 Ag1 I1 105.50(6) . 7 ? I4 Ag1 I1 101.39(7) 7 . ? I2 Ag1 I1 103.78(7) . . ? I1 Ag1 I1 88.19(5) 7 . ? I4 Ag1 Pb1 62.94(4) 7 7 ? I2 Ag1 Pb1 163.37(7) . 7 ? I1 Ag1 Pb1 62.55(4) 7 7 ? I1 Ag1 Pb1 65.98(4) . 7 ? O4 La1 O4 146.1(15) 2_755 . ? O4 La1 O2 99.6(7) 2_755 2_755 ? O4 La1 O2 92.0(8) . 2_755 ? O4 La1 O2 92.0(8) 2_755 . ? O4 La1 O2 99.6(7) . . ? O2 La1 O2 139.4(9) 2_755 . ? O4 La1 O1 147.4(10) 2_755 . ? O4 La1 O1 66.4(9) . . ? O2 La1 O1 75.2(6) 2_755 . ? O2 La1 O1 74.3(6) . . ? O4 La1 O1 66.4(9) 2_755 2_755 ? O4 La1 O1 147.4(10) . 2_755 ? O2 La1 O1 74.3(6) 2_755 2_755 ? O2 La1 O1 75.2(6) . 2_755 ? O1 La1 O1 81.4(11) . 2_755 ? O4 La1 O3 72.5(10) 2_755 . ? O4 La1 O3 80.9(9) . . ? O2 La1 O3 72.8(7) 2_755 . ? O2 La1 O3 147.3(7) . . ? O1 La1 O3 132.7(9) . . ? O1 La1 O3 120.9(6) 2_755 . ? O4 La1 O3 80.9(9) 2_755 2_755 ? O4 La1 O3 72.5(10) . 2_755 ? O2 La1 O3 147.3(7) 2_755 2_755 ? O2 La1 O3 72.8(7) . 2_755 ? O1 La1 O3 120.9(6) . 2_755 ? O1 La1 O3 132.7(9) 2_755 2_755 ? O3 La1 O3 76.3(10) . 2_755 ? Ag1 I1 Ag1 91.81(5) 7 . ? Ag1 I1 Pb1 66.09(4) 7 . ? Ag1 I1 Pb1 66.95(4) . . ? Ag1 I2 Pb1 73.24(5) . . ? Ag1 I4 Pb1 69.64(4) 7 . ? Pb1 I5 Pb1 180.0 7_565 . ? S1 O1 La1 145.2(12) . . ? S2 O2 La1 132.4(11) . . ? S3 O3 La1 144(2) . . ? S4 O4 La1 168(2) . . ? O1 S1 C1 105.6(13) . . ? O1 S1 C2 99.1(13) . . ? C1 S1 C2 101.9(11) . . ? O2 S2 C3 107.9(12) . . ? O2 S2 C4 107.1(12) . . ? C3 S2 C4 98.2(13) . . ? O3 S3 C5 116.7(18) . . ? O3 S3 C6 115.4(15) . . ? C5 S3 C6 99.1(15) . . ? O4 S4 C7 116.4(19) . . ? O4 S4 C8 108.6(16) . . ? C7 S4 C8 107(2) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? S2 C3 H3A 109.5 . . ? S2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S3 C5 H5A 109.5 . . ? S3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S3 C6 H6A 109.5 . . ? S3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S4 C7 H7A 109.5 . . ? S4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S4 C8 H8A 109.5 . . ? S4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 I4 Ag1 I1 Ag1 -113.88(7) 7 . . 7 ? I2 Ag1 I1 Ag1 105.51(7) . . . 7 ? I1 Ag1 I1 Ag1 0.0 7 . . 7 ? Pb1 Ag1 I1 Ag1 -60.60(3) 7 . . 7 ? I4 Ag1 I1 Pb1 -176.88(7) 7 . . . ? I2 Ag1 I1 Pb1 42.52(5) . . . . ? I1 Ag1 I1 Pb1 -62.99(3) 7 . . . ? Pb1 Ag1 I1 Pb1 -123.59(3) 7 . . . ? I3 Pb1 I1 Ag1 124.71(6) . . . 7 ? I5 Pb1 I1 Ag1 -79.6(7) . . . 7 ? I2 Pb1 I1 Ag1 -136.95(5) . . . 7 ? I4 Pb1 I1 Ag1 27.72(5) . . . 7 ? I3 Pb1 I1 Ag1 -132.22(5) . . . . ? I5 Pb1 I1 Ag1 23.5(7) . . . . ? I2 Pb1 I1 Ag1 -33.88(5) . . . . ? I4 Pb1 I1 Ag1 130.79(5) . . . . ? Ag1 Pb1 I1 Ag1 103.07(5) 7 . . . ? I4 Ag1 I2 Pb1 -163.82(13) 7 . . . ? I1 Ag1 I2 Pb1 49.03(6) 7 . . . ? I1 Ag1 I2 Pb1 -42.93(5) . . . . ? Pb1 Ag1 I2 Pb1 7.0(3) 7 . . . ? I3 Pb1 I2 Ag1 123.72(6) . . . . ? I5 Pb1 I2 Ag1 -140.89(5) . . . . ? I4 Pb1 I2 Ag1 -50.46(14) . . . . ? I1 Pb1 I2 Ag1 37.21(5) . . . . ? Ag1 Pb1 I2 Ag1 -2.40(10) 7 . . . ? I3 Pb1 I4 Ag1 -116.55(6) . . . 7 ? I5 Pb1 I4 Ag1 148.27(6) . . . 7 ? I2 Pb1 I4 Ag1 57.65(14) . . . 7 ? I1 Pb1 I4 Ag1 -29.57(6) . . . 7 ? I3 Pb1 I5 Pb1 11(7) . . . 7_565 ? I2 Pb1 I5 Pb1 -87(7) . . . 7_565 ? I4 Pb1 I5 Pb1 108(7) . . . 7_565 ? I1 Pb1 I5 Pb1 -144(7) . . . 7_565 ? Ag1 Pb1 I5 Pb1 138(7) 7 . . 7_565 ? O4 La1 O1 S1 86(3) 2_755 . . . ? O4 La1 O1 S1 -90(3) . . . . ? O2 La1 O1 S1 171(3) 2_755 . . . ? O2 La1 O1 S1 18(3) . . . . ? O1 La1 O1 S1 95(3) 2_755 . . . ? O3 La1 O1 S1 -141(2) . . . . ? O3 La1 O1 S1 -40(3) 2_755 . . . ? O4 La1 O2 S2 -63.4(16) 2_755 . . . ? O4 La1 O2 S2 148.5(16) . . . . ? O2 La1 O2 S2 43.9(14) 2_755 . . . ? O1 La1 O2 S2 86.5(16) . . . . ? O1 La1 O2 S2 1.5(15) 2_755 . . . ? O3 La1 O2 S2 -123.3(16) . . . . ? O3 La1 O2 S2 -143.3(17) 2_755 . . . ? O4 La1 O3 S3 149(2) 2_755 . . . ? O4 La1 O3 S3 -53(2) . . . . ? O2 La1 O3 S3 42(2) 2_755 . . . ? O2 La1 O3 S3 -146.3(17) . . . . ? O1 La1 O3 S3 -7(2) . . . . ? O1 La1 O3 S3 101(2) 2_755 . . . ? O3 La1 O3 S3 -127(3) 2_755 . . . ? O4 La1 O4 S4 -6(7) 2_755 . . . ? O2 La1 O4 S4 -117(7) 2_755 . . . ? O2 La1 O4 S4 103(7) . . . . ? O1 La1 O4 S4 171(8) . . . . ? O1 La1 O4 S4 -179(7) 2_755 . . . ? O3 La1 O4 S4 -44(7) . . . . ? O3 La1 O4 S4 34(7) 2_755 . . . ? La1 O1 S1 C1 140(2) . . . . ? La1 O1 S1 C2 -115(3) . . . . ? La1 O2 S2 C3 -160.3(14) . . . . ? La1 O2 S2 C4 94.8(16) . . . . ? La1 O3 S3 C5 143(2) . . . . ? La1 O3 S3 C6 -102(3) . . . . ? La1 O4 S4 C7 31(8) . . . . ? La1 O4 S4 C8 -89(8) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.660 _refine_diff_density_min -1.487 _refine_diff_density_rms 0.202 _database_code_depnum_ccdc_archive 'CCDC 958524' data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H48 Ag2 Gd I9 O8 Pb2 S8' _chemical_formula_sum 'C16 H48 Ag2 Gd I9 O8 Pb2 S8' _chemical_formula_weight 2554.49 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C c c m' _symmetry_space_group_name_Hall '-C 2 2c' _symmetry_Int_Tables_number 66 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, z+1/2' 'x, -y, z+1/2' '-x, -y, z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, -y+1/2, z' '-x, -y, -z' 'x, -y, -z-1/2' '-x, y, -z-1/2' 'x, y, -z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, -z-1/2' '-x+1/2, y+1/2, -z-1/2' 'x+1/2, y+1/2, -z' _cell_length_a 10.6777(10) _cell_length_b 24.857(2) _cell_length_c 22.051(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5852.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10015 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4540 _exptl_absorpt_coefficient_mu 12.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0355 _exptl_absorpt_correction_T_max 0.4329 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11612 _diffrn_reflns_av_R_equivalents 0.0894 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2753 _reflns_number_gt 2172 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens - _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00054(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2753 _refine_ls_number_parameters 96 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.000 _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 Pb1 Pb 0.51571(7) 0.29952(3) 0.5000 0.0563(4) Uani 1 2 d S . . Ag1 Ag 0.7500 0.2500 0.59958(11) 0.0677(8) Uani 1 2 d S . . I1 I 0.82640(14) 0.32769(6) 0.5000 0.0636(5) Uani 1 2 d S . . I2 I 0.53399(13) 0.28987(7) 0.64689(6) 0.0681(5) Uani 1 1 d . . . I3 I 0.42801(18) 0.41367(6) 0.5000 0.0827(6) Uani 1 2 d S . . I4 I 0.2500 0.2500 0.5000 0.0650(6) Uani 1 4 d S . . Gd1 Gd 0.0000 0.5000 0.7500 0.0662(4) Uani 1 4 d S . . O1 O 0.0814(12) 0.4241(5) 0.6970(6) 0.0777(17) Uani 1 1 d . . . O2 O 0.1625(15) 0.5286(7) 0.6872(8) 0.0892(3) Uani 1 1 d . . . S1A S 0.0749(9) 0.3738(4) 0.6799(5) 0.0777(17) Uani 0.50 1 d PD . . S1B S 0.1694(9) 0.3912(4) 0.6817(5) 0.0777(17) Uani 0.50 1 d PD . . S2A S 0.2738(12) 0.5213(6) 0.6614(6) 0.0911(3) Uani 0.50 1 d PD . . S2B S 0.2327(11) 0.5623(6) 0.6559(6) 0.0977(3) Uani 0.50 1 d PD . . C1 C 0.178(2) 0.3319(8) 0.7228(11) 0.087(8) Uani 1 1 d D . . C2 C 0.143(3) 0.3624(11) 0.6091(9) 0.082(12) Uani 1 1 d D . . C3 C 0.244(2) 0.5365(9) 0.5830(7) 0.0881(3) Uani 1 1 d D . . C4 C 0.3949(15) 0.5680(9) 0.6702(11) 0.0911(3) Uani 1 1 d 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 Pb1 0.0471(5) 0.0637(5) 0.0582(6) 0.023 0.000 -0.0017(3) Ag1 0.0521(12) 0.084(2) 0.0677(15) 0.000 0.000 0.0234(14) I1 0.0481(8) 0.0439(8) 0.0989(12) 0.000 0.000 -0.0084(6) I2 0.0619(8) 0.0857(13) 0.0575(8) -0.0141(7) 0.0032(6) 0.0158(8) I3 0.0704(11) 0.0438(9) 0.1338(17) 0.000 0.000 0.0001(8) I4 0.0389(10) 0.0569(12) 0.0992(17) 0.000 0.000 -0.0133(9) Gd1 0.0599(6) 0.0676(7) 0.0652(7) 0.015 0.019 0.000 O1 0.070(3) 0.068(3) 0.096(4) -0.024(3) 0.007(4) 0.008(3) O2 0.093(5) 0.078(5) 0.092(6) 0.015(5) 0.010(4) 0.007(4) S1A 0.070(3) 0.068(3) 0.096(4) -0.024(3) 0.007(4) 0.008(3) S1B 0.070(3) 0.068(3) 0.096(4) -0.024(3) 0.007(4) 0.008(3) S2A 0.093(5) 0.108(5) 0.082(6) 0.015(5) 0.010(4) 0.007(4) S2B 0.093(5) 0.108(5) 0.092(6) 0.015(5) 0.0260(4) 0.007(4) C1 0.087(16) 0.088(18) 0.093(2) -0.009(16) 0.019(15) 0.018(14) C2 0.090(2) 0.081(17) 0.091(3) -0.011(17) 0.026(2) -0.014(17) C3 0.093(5) 0.078(5) 0.087(6) 0.015(5) 0.0160(4) 0.007(4) C4 0.094(5) 0.088(5) 0.091(6) 0.035(5) 0.0160(4) 0.007(4) _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 Pb1 I3 2.9879(18) . ? Pb1 I4 3.0928(8) . ? Pb1 I2 3.2538(14) 12_556 ? Pb1 I2 3.2538(14) . ? Pb1 I1 3.3905(17) . ? Ag1 I2 2.7184(16) 8_655 ? Ag1 I2 2.7184(16) . ? Ag1 I1 3.036(2) 13_656 ? Ag1 I1 3.036(2) . ? I1 Ag1 3.036(2) 13_656 ? I4 Pb1 3.0928(8) 13_556 ? Gd1 O2 2.331(13) 4_565 ? Gd1 O2 2.331(13) 10_567 ? Gd1 O2 2.331(13) . ? Gd1 O2 2.331(13) 11_557 ? Gd1 O1 2.383(12) 10_567 ? Gd1 O1 2.383(12) . ? Gd1 O1 2.383(12) 11_557 ? Gd1 O1 2.383(12) 4_565 ? O1 S1B 1.291(15) . ? O1 S1A 1.307(15) . ? O2 S2B 1.319(18) . ? O2 S2A 1.329(18) . ? S1A C2 1.748(15) . ? S1A C1 1.785(16) . ? S1B C1 1.733(16) . ? S1B C2 1.775(16) . ? S2A C4 1.749(16) . ? S2A C3 1.798(16) . ? S2B C3 1.734(16) . ? S2B C4 1.767(16) . ? 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 I3 Pb1 I4 95.19(4) . . ? I3 Pb1 I2 95.10(3) . 12_556 ? I4 Pb1 I2 91.47(3) . 12_556 ? I3 Pb1 I2 95.10(3) . . ? I4 Pb1 I2 91.47(3) . . ? I2 Pb1 I2 169.09(6) 12_556 . ? I3 Pb1 I1 96.35(5) . . ? I4 Pb1 I1 168.46(4) . . ? I2 Pb1 I1 87.51(3) 12_556 . ? I2 Pb1 I1 87.51(3) . . ? I2 Ag1 I2 134.87(11) 8_655 . ? I2 Ag1 I1 105.88(5) 8_655 13_656 ? I2 Ag1 I1 106.35(5) . 13_656 ? I2 Ag1 I1 106.35(5) 8_655 . ? I2 Ag1 I1 105.88(5) . . ? I1 Ag1 I1 87.34(8) 13_656 . ? Ag1 I1 Ag1 92.66(8) 13_656 . ? Ag1 I1 Pb1 66.78(3) 13_656 . ? Ag1 I1 Pb1 66.78(3) . . ? Ag1 I2 Pb1 72.29(6) . . ? Pb1 I4 Pb1 180.0 13_556 . ? O2 Gd1 O2 144.5(8) 4_565 10_567 ? O2 Gd1 O2 107.1(10) 4_565 . ? O2 Gd1 O2 83.8(9) 10_567 . ? O2 Gd1 O2 83.8(9) 4_565 11_557 ? O2 Gd1 O2 107.1(10) 10_567 11_557 ? O2 Gd1 O2 144.5(8) . 11_557 ? O2 Gd1 O1 143.5(5) 4_565 10_567 ? O2 Gd1 O1 71.2(5) 10_567 10_567 ? O2 Gd1 O1 77.2(6) . 10_567 ? O2 Gd1 O1 74.9(5) 11_557 10_567 ? O2 Gd1 O1 74.9(5) 4_565 . ? O2 Gd1 O1 77.2(6) 10_567 . ? O2 Gd1 O1 71.2(5) . . ? O2 Gd1 O1 143.5(5) 11_557 . ? O1 Gd1 O1 137.2(6) 10_567 . ? O2 Gd1 O1 77.2(6) 4_565 11_557 ? O2 Gd1 O1 74.9(5) 10_567 11_557 ? O2 Gd1 O1 143.5(5) . 11_557 ? O2 Gd1 O1 71.2(5) 11_557 11_557 ? O1 Gd1 O1 121.2(7) 10_567 11_557 ? O1 Gd1 O1 75.4(7) . 11_557 ? O2 Gd1 O1 71.2(5) 4_565 4_565 ? O2 Gd1 O1 143.5(5) 10_567 4_565 ? O2 Gd1 O1 74.9(5) . 4_565 ? O2 Gd1 O1 77.2(6) 11_557 4_565 ? O1 Gd1 O1 75.4(7) 10_567 4_565 ? O1 Gd1 O1 121.2(7) . 4_565 ? O1 Gd1 O1 137.2(6) 11_557 4_565 ? S1B O1 S1A 50.0(8) . . ? S1B O1 Gd1 153.5(10) . . ? S1A O1 Gd1 151.5(10) . . ? S2B O2 S2A 49.9(9) . . ? S2B O2 Gd1 158.0(12) . . ? S2A O2 Gd1 151.4(12) . . ? O1 S1A C2 113.0(12) . . ? O1 S1A C1 111.9(12) . . ? C2 S1A C1 97.0(14) . . ? O1 S1B C1 116.1(12) . . ? O1 S1B C2 112.1(13) . . ? C1 S1B C2 97.9(14) . . ? O2 S2A C4 121.6(15) . . ? O2 S2A C3 102.9(13) . . ? C4 S2A C3 95.6(12) . . ? O2 S2B C3 106.8(14) . . ? O2 S2B C4 120.9(14) . . ? C3 S2B C4 97.3(13) . . ? S1B C1 S1A 36.3(5) . . ? S1A C2 S1B 36.3(5) . . ? S2B C3 S2A 36.8(7) . . ? S2A C4 S2B 37.0(7) . . ? 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 I2 Ag1 I1 Ag1 105.78(6) 8_655 . . 13_656 ? I2 Ag1 I1 Ag1 -106.24(6) . . . 13_656 ? I1 Ag1 I1 Ag1 0.0 13_656 . . 13_656 ? I2 Ag1 I1 Pb1 169.07(7) 8_655 . . . ? I2 Ag1 I1 Pb1 -42.95(5) . . . . ? I1 Ag1 I1 Pb1 63.30(3) 13_656 . . . ? I3 Pb1 I1 Ag1 -128.09(4) . . . 13_656 ? I4 Pb1 I1 Ag1 51.91(4) . . . 13_656 ? I2 Pb1 I1 Ag1 -33.23(5) 12_556 . . 13_656 ? I2 Pb1 I1 Ag1 137.06(5) . . . 13_656 ? I3 Pb1 I1 Ag1 128.09(4) . . . . ? I4 Pb1 I1 Ag1 -51.91(4) . . . . ? I2 Pb1 I1 Ag1 -137.06(5) 12_556 . . . ? I2 Pb1 I1 Ag1 33.23(5) . . . . ? I2 Ag1 I2 Pb1 177.35(4) 8_655 . . . ? I1 Ag1 I2 Pb1 -48.67(6) 13_656 . . . ? I1 Ag1 I2 Pb1 43.23(6) . . . . ? I3 Pb1 I2 Ag1 -132.34(5) . . . . ? I4 Pb1 I2 Ag1 132.31(3) . . . . ? I2 Pb1 I2 Ag1 26.7(3) 12_556 . . . ? I1 Pb1 I2 Ag1 -36.18(4) . . . . ? I3 Pb1 I4 Pb1 180.0 . . . 13_556 ? I2 Pb1 I4 Pb1 84.74(3) 12_556 . . 13_556 ? I2 Pb1 I4 Pb1 -84.74(3) . . . 13_556 ? I1 Pb1 I4 Pb1 0.0 . . . 13_556 ? O2 Gd1 O1 S1B 174(3) 4_565 . . . ? O2 Gd1 O1 S1B -28(2) 10_567 . . . ? O2 Gd1 O1 S1B 59(2) . . . . ? O2 Gd1 O1 S1B -130(2) 11_557 . . . ? O1 Gd1 O1 S1B 15(2) 10_567 . . . ? O1 Gd1 O1 S1B -106(3) 11_557 . . . ? O1 Gd1 O1 S1B 117(2) 4_565 . . . ? O2 Gd1 O1 S1A -54(2) 4_565 . . . ? O2 Gd1 O1 S1A 104(2) 10_567 . . . ? O2 Gd1 O1 S1A -168(2) . . . . ? O2 Gd1 O1 S1A 3(3) 11_557 . . . ? O1 Gd1 O1 S1A 147(2) 10_567 . . . ? O1 Gd1 O1 S1A 26.7(19) 11_557 . . . ? O1 Gd1 O1 S1A -110(2) 4_565 . . . ? O2 Gd1 O2 S2B 95(4) 4_565 . . . ? O2 Gd1 O2 S2B -119(4) 10_567 . . . ? O2 Gd1 O2 S2B -8(4) 11_557 . . . ? O1 Gd1 O2 S2B -47(4) 10_567 . . . ? O1 Gd1 O2 S2B 162(4) . . . . ? O1 Gd1 O2 S2B -173(4) 11_557 . . . ? O1 Gd1 O2 S2B 31(4) 4_565 . . . ? O2 Gd1 O2 S2A -104(3) 4_565 . . . ? O2 Gd1 O2 S2A 41(3) 10_567 . . . ? O2 Gd1 O2 S2A 152(3) 11_557 . . . ? O1 Gd1 O2 S2A 113(3) 10_567 . . . ? O1 Gd1 O2 S2A -37(3) . . . . ? O1 Gd1 O2 S2A -13(4) 11_557 . . . ? O1 Gd1 O2 S2A -169(3) 4_565 . . . ? S1B O1 S1A C2 -56.4(13) . . . . ? Gd1 O1 S1A C2 149(2) . . . . ? S1B O1 S1A C1 51.8(11) . . . . ? Gd1 O1 S1A C1 -103(2) . . . . ? S1A O1 S1B C1 -56.7(13) . . . . ? Gd1 O1 S1B C1 96(2) . . . . ? S1A O1 S1B C2 54.6(12) . . . . ? Gd1 O1 S1B C2 -153(2) . . . . ? S2B O2 S2A C4 46.7(16) . . . . ? Gd1 O2 S2A C4 -124(3) . . . . ? S2B O2 S2A C3 -58.3(12) . . . . ? Gd1 O2 S2A C3 131(3) . . . . ? S2A O2 S2B C3 63.9(13) . . . . ? Gd1 O2 S2B C3 -128(4) . . . . ? S2A O2 S2B C4 -45.7(15) . . . . ? Gd1 O2 S2B C4 122(4) . . . . ? O1 S1B C1 S1A 52.3(12) . . . . ? C2 S1B C1 S1A -67.1(10) . . . . ? O1 S1A C1 S1B -49.2(11) . . . . ? C2 S1A C1 S1B 69.0(10) . . . . ? O1 S1A C2 S1B 51.6(12) . . . . ? C1 S1A C2 S1B -65.8(10) . . . . ? O1 S1B C2 S1A -52.1(12) . . . . ? C1 S1B C2 S1A 70.3(10) . . . . ? O2 S2B C3 S2A -57.9(13) . . . . ? C4 S2B C3 S2A 67.5(10) . . . . ? O2 S2A C3 S2B 55.7(13) . . . . ? C4 S2A C3 S2B -68.5(11) . . . . ? O2 S2A C4 S2B -43.7(15) . . . . ? C3 S2A C4 S2B 65.3(10) . . . . ? O2 S2B C4 S2A 43.7(15) . . . . ? C3 S2B C4 S2A -70.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.665 _refine_diff_density_min -1.488 _refine_diff_density_rms 0.306 _database_code_depnum_ccdc_archive 'CCDC 958525' data_o66-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H48 Ag2 I9 O8 Pb2 S8 Tm' _chemical_formula_sum 'C16 H48 Ag2 I9 O8 Pb2 S8 Tm' _chemical_formula_weight 2566.17 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 '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 orthorhombic _symmetry_space_group_name_H-M 'C c c m' _symmetry_space_group_name_Hall '-C 2 2c' _symmetry_Int_Tables_number 66 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z-1/2' _cell_length_a 10.717(2) _cell_length_b 24.883(5) _cell_length_c 21.972(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5859(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10027 _cell_measurement_theta_min 3.1052 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Prism _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4560 _exptl_absorpt_coefficient_mu 12.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0596 _exptl_absorpt_correction_T_max 0.1125 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27049 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2764 _reflns_number_gt 2532 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0250P)^2^+94.9515P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000204(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2764 _refine_ls_number_parameters 131 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.278 _refine_ls_restrained_S_all 1.280 _refine_ls_shift/su_max 0.000 _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 Pb1 Pb 0.01635(6) 0.20016(2) 0.0000 0.0636(2) Uani 1 2 d S . . Ag1 Ag 0.2500 0.2500 0.10044(9) 0.0840(7) Uani 1 2 d S . . I1 I 0.03497(10) 0.21040(5) 0.14743(5) 0.0761(4) Uani 1 1 d . . . I2 I 0.32592(11) 0.17238(4) 0.0000 0.0669(4) Uani 1 2 d S . . I3 I -0.06878(13) 0.08570(5) 0.0000 0.0831(5) Uani 1 2 d S . . I4 I -0.2500 0.2500 0.0000 0.0752(5) Uani 1 4 d S . . Tm1 Tm 0.0000 0.5000 0.2500 0.0674(2) Uani 1 4 d S . . O1 O 0.1552(10) 0.4731(6) 0.1892(6) 0.099(5) Uani 1 1 d . . . O2 O 0.0745(15) 0.4262(5) 0.3016(6) 0.096(6) Uani 1 1 d . . . S1A S 0.2259(8) 0.4395(3) 0.1566(4) 0.097(3) Uani 0.50 1 d PD . . S1B S 0.2645(8) 0.4795(4) 0.1608(5) 0.103(3) Uani 0.50 1 d PD . . S2A S 0.1674(7) 0.3933(3) 0.3176(4) 0.083(2) Uani 0.50 1 d PD . . S2B S 0.0721(7) 0.3756(3) 0.3197(3) 0.0681(19) Uani 0.50 1 d PD . . C1 C 0.240(3) 0.4682(11) 0.0833(6) 0.103(19) Uani 1 1 d D . . C2 C 0.3874(17) 0.4351(13) 0.1668(18) 0.097(2) Uani 1 1 d D . . C3 C 0.1355(19) 0.3670(8) 0.3913(6) 0.095(8) Uani 1 1 d D . . C4 C 0.1784(16) 0.3324(6) 0.2780(10) 0.087(8) Uani 1 1 d 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 Pb1 0.0637(4) 0.0678(4) 0.0603(4) 0.000 0.000 0.0027(3) Ag1 0.0780(11) 0.0797(18) 0.0933(14) 0.000 0.000 -0.0323(12) I1 0.0788(7) 0.0866(9) 0.0619(6) 0.0078(6) 0.0097(5) -0.0146(6) I2 0.0598(7) 0.0492(6) 0.0918(9) 0.000 0.000 0.0105(5) I3 0.0771(9) 0.0489(7) 0.1234(13) 0.000 0.000 -0.0019(6) I4 0.0486(9) 0.0647(10) 0.1123(16) 0.000 0.000 0.0151(8) Tm1 0.0757(5) 0.0736(4) 0.0538(5) 0.000 0.000 0.000 O1 0.088(8) 0.104(13) 0.105(9) -0.028(9) 0.020(7) 0.018(8) O2 0.092(15) 0.109(9) 0.088(10) 0.024(8) 0.010(10) 0.016(10) S1A 0.107(6) 0.056(4) 0.129(8) -0.019(5) 0.024(6) -0.010(4) S1B 0.090(6) 0.094(6) 0.126(8) -0.024(6) 0.023(6) -0.0121(5) S2A 0.067(5) 0.065(4) 0.117(7) 0.029(4) -0.020(4) 0.002(4) S2B 0.058(4) 0.051(4) 0.094(5) 0.023(3) -0.015(4) -0.001(3) C1 0.094(5) 0.107(4) 0.102(2) -0.015(2) 0.013(3) -0.019(3) C2 0.104(2) 0.102(6) 0.090(5) 0.013(4) 0.016(3) 0.010(3) C3 0.094(19) 0.090(15) 0.103(14) 0.022(12) -0.0250(14) -0.015(14) C4 0.0912(15) 0.081(11) 0.090(2) -0.022(13) -0.008(15) 0.016(11) _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 Pb1 I3 2.9909(15) . ? Pb1 I4 3.1122(8) . ? Pb1 I1 3.2555(12) . ? Pb1 I1 3.2555(12) 10 ? Pb1 I2 3.3889(14) . ? Ag1 I1 2.7107(13) 6 ? Ag1 I1 2.7107(13) . ? Ag1 I2 3.0436(17) . ? Ag1 I2 3.0436(17) 13 ? I2 Ag1 3.0436(17) 13 ? I4 Pb1 3.1122(8) 13_455 ? Tm1 O1 2.235(9) 4_565 ? Tm1 O1 2.235(9) 2_565 ? Tm1 O1 2.235(9) . ? Tm1 O1 2.235(9) 3 ? Tm1 O2 2.301(10) 3 ? Tm1 O2 2.301(10) 2_565 ? Tm1 O2 2.301(10) 4_565 ? Tm1 O2 2.301(10) . ? O1 S1B 1.337(13) . ? O1 S1A 1.337(12) . ? O2 S2B 1.321(13) . ? O2 S2A 1.336(13) . ? S1A C2 1.749(17) . ? S1A C1 1.769(16) . ? S1B C2 1.725(17) . ? S1B C1 1.744(16) . ? S2A C4 1.752(14) . ? S2A C3 1.780(14) . ? S2B C3 1.727(13) . ? S2B C4 1.815(14) . ? 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 I3 Pb1 I4 95.72(3) . . ? I3 Pb1 I1 95.35(2) . . ? I4 Pb1 I1 91.44(2) . . ? I3 Pb1 I1 95.35(2) . 10 ? I4 Pb1 I1 91.44(2) . 10 ? I1 Pb1 I1 168.60(4) . 10 ? I3 Pb1 I2 95.99(4) . . ? I4 Pb1 I2 168.29(3) . . ? I1 Pb1 I2 87.48(2) . . ? I1 Pb1 I2 87.48(2) 10 . ? I1 Ag1 I1 135.22(9) 6 . ? I1 Ag1 I2 106.24(4) 6 . ? I1 Ag1 I2 105.83(4) . . ? I1 Ag1 I2 105.83(4) 6 13 ? I1 Ag1 I2 106.24(4) . 13 ? I2 Ag1 I2 87.04(6) . 13 ? Ag1 I1 Pb1 72.64(5) . . ? Ag1 I2 Ag1 92.96(6) . 13 ? Ag1 I2 Pb1 66.97(2) . . ? Ag1 I2 Pb1 66.97(2) 13 . ? Pb1 I4 Pb1 180.00(2) . 13_455 ? O1 Tm1 O1 145.2(8) 4_565 2_565 ? O1 Tm1 O1 83.8(7) 4_565 . ? O1 Tm1 O1 106.6(7) 2_565 . ? O1 Tm1 O1 106.6(7) 4_565 3 ? O1 Tm1 O1 83.8(7) 2_565 3 ? O1 Tm1 O1 145.2(8) . 3 ? O1 Tm1 O2 142.3(6) 4_565 3 ? O1 Tm1 O2 71.7(6) 2_565 3 ? O1 Tm1 O2 74.1(5) . 3 ? O1 Tm1 O2 78.3(5) 3 3 ? O1 Tm1 O2 74.1(5) 4_565 2_565 ? O1 Tm1 O2 78.3(5) 2_565 2_565 ? O1 Tm1 O2 142.3(6) . 2_565 ? O1 Tm1 O2 71.7(6) 3 2_565 ? O2 Tm1 O2 139.4(8) 3 2_565 ? O1 Tm1 O2 78.3(5) 4_565 4_565 ? O1 Tm1 O2 74.1(5) 2_565 4_565 ? O1 Tm1 O2 71.7(6) . 4_565 ? O1 Tm1 O2 142.3(6) 3 4_565 ? O2 Tm1 O2 120.9(7) 3 4_565 ? O2 Tm1 O2 74.2(8) 2_565 4_565 ? O1 Tm1 O2 71.7(6) 4_565 . ? O1 Tm1 O2 142.3(6) 2_565 . ? O1 Tm1 O2 78.3(5) . . ? O1 Tm1 O2 74.1(5) 3 . ? O2 Tm1 O2 74.2(8) 3 . ? O2 Tm1 O2 120.9(7) 2_565 . ? O2 Tm1 O2 139.4(8) 4_565 . ? S1B O1 S1A 47.7(5) . . ? S1B O1 Tm1 153.6(10) . . ? S1A O1 Tm1 158.2(11) . . ? S2B O2 S2A 49.5(5) . . ? S2B O2 Tm1 154.4(12) . . ? S2A O2 Tm1 151.3(11) . . ? O1 S1A C2 122.1(15) . . ? O1 S1A C1 106.4(14) . . ? C2 S1A C1 93.3(18) . . ? O1 S1B C2 123.9(14) . . ? O1 S1B C1 107.8(14) . . ? C2 S1B C1 95.0(19) . . ? O2 S2A C4 116.7(11) . . ? O2 S2A C3 108.7(10) . . ? C4 S2A C3 98.5(11) . . ? O2 S2B C3 112.6(10) . . ? O2 S2B C4 113.6(10) . . ? C3 S2B C4 98.1(11) . . ? S1B C1 S1A 35.9(4) . . ? S1B C2 S1A 36.3(4) . . ? S2B C3 S2A 37.0(4) . . ? S2A C4 S2B 36.3(4) . . ? 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 I1 Ag1 I1 Pb1 -177.13(3) 6 . . . ? I2 Ag1 I1 Pb1 -42.83(4) . . . . ? I2 Ag1 I1 Pb1 48.70(5) 13 . . . ? I3 Pb1 I1 Ag1 131.80(4) . . . . ? I4 Pb1 I1 Ag1 -132.32(3) . . . . ? I1 Pb1 I1 Ag1 -27.8(2) 10 . . . ? I2 Pb1 I1 Ag1 36.02(3) . . . . ? I1 Ag1 I2 Ag1 -105.63(5) 6 . . 13 ? I1 Ag1 I2 Ag1 106.04(5) . . . 13 ? I2 Ag1 I2 Ag1 0.0 13 . . 13 ? I1 Ag1 I2 Pb1 -169.04(5) 6 . . . ? I1 Ag1 I2 Pb1 42.63(4) . . . . ? I2 Ag1 I2 Pb1 -63.41(2) 13 . . . ? I3 Pb1 I2 Ag1 -128.01(3) . . . . ? I4 Pb1 I2 Ag1 51.99(3) . . . . ? I1 Pb1 I2 Ag1 -32.90(4) . . . . ? I1 Pb1 I2 Ag1 136.88(4) 10 . . . ? I3 Pb1 I2 Ag1 128.01(3) . . . 13 ? I4 Pb1 I2 Ag1 -51.99(3) . . . 13 ? I1 Pb1 I2 Ag1 -136.88(4) . . . 13 ? I1 Pb1 I2 Ag1 32.90(4) 10 . . 13 ? I3 Pb1 I4 Pb1 0.0 . . . 13_455 ? I1 Pb1 I4 Pb1 -95.52(2) . . . 13_455 ? I1 Pb1 I4 Pb1 95.52(2) 10 . . 13_455 ? I2 Pb1 I4 Pb1 180.0 . . . 13_455 ? O1 Tm1 O1 S1B -45(2) 4_565 . . . ? O1 Tm1 O1 S1B 101(3) 2_565 . . . ? O1 Tm1 O1 S1B -156(3) 3 . . . ? O2 Tm1 O1 S1B 166(3) 3 . . . ? O2 Tm1 O1 S1B 9(3) 2_565 . . . ? O2 Tm1 O1 S1B 35(2) 4_565 . . . ? O2 Tm1 O1 S1B -118(3) . . . . ? O1 Tm1 O1 S1A 120(3) 4_565 . . . ? O1 Tm1 O1 S1A -94(3) 2_565 . . . ? O1 Tm1 O1 S1A 10(3) 3 . . . ? O2 Tm1 O1 S1A -29(3) 3 . . . ? O2 Tm1 O1 S1A 174(2) 2_565 . . . ? O2 Tm1 O1 S1A -160(3) 4_565 . . . ? O2 Tm1 O1 S1A 48(3) . . . . ? O1 Tm1 O2 S2B 170(2) 4_565 . . . ? O1 Tm1 O2 S2B 0(3) 2_565 . . . ? O1 Tm1 O2 S2B -102(2) . . . . ? O1 Tm1 O2 S2B 56(2) 3 . . . ? O2 Tm1 O2 S2B -26.0(19) 3 . . . ? O2 Tm1 O2 S2B 113(2) 2_565 . . . ? O2 Tm1 O2 S2B -145(2) 4_565 . . . ? O1 Tm1 O2 S2A -56(2) 4_565 . . . ? O1 Tm1 O2 S2A 133(2) 2_565 . . . ? O1 Tm1 O2 S2A 31(2) . . . . ? O1 Tm1 O2 S2A -170(2) 3 . . . ? O2 Tm1 O2 S2A 107(2) 3 . . . ? O2 Tm1 O2 S2A -114(2) 2_565 . . . ? O2 Tm1 O2 S2A -12(2) 4_565 . . . ? S1B O1 S1A C2 45.1(16) . . . . ? Tm1 O1 S1A C2 -126(3) . . . . ? S1B O1 S1A C1 -59.7(12) . . . . ? Tm1 O1 S1A C1 129(3) . . . . ? S1A O1 S1B C2 -47.1(17) . . . . ? Tm1 O1 S1B C2 126(3) . . . . ? S1A O1 S1B C1 61.9(13) . . . . ? Tm1 O1 S1B C1 -125(2) . . . . ? S2B O2 S2A C4 55.8(11) . . . . ? Tm1 O2 S2A C4 -100(2) . . . . ? S2B O2 S2A C3 -54.4(9) . . . . ? Tm1 O2 S2A C3 150(2) . . . . ? S2A O2 S2B C3 59.3(10) . . . . ? Tm1 O2 S2B C3 -148(2) . . . . ? S2A O2 S2B C4 -51.1(10) . . . . ? Tm1 O2 S2B C4 102(2) . . . . ? O1 S1B C1 S1A -57.4(11) . . . . ? C2 S1B C1 S1A 70.6(12) . . . . ? O1 S1A C1 S1B 56.7(11) . . . . ? C2 S1A C1 S1B -68.2(13) . . . . ? O1 S1B C2 S1A 44.5(15) . . . . ? C1 S1B C2 S1A -70.9(11) . . . . ? O1 S1A C2 S1B -43.4(15) . . . . ? C1 S1A C2 S1B 68.3(11) . . . . ? O2 S2B C3 S2A -54.7(10) . . . . ? C4 S2B C3 S2A 65.1(8) . . . . ? O2 S2A C3 S2B 51.9(10) . . . . ? C4 S2A C3 S2B -70.2(8) . . . . ? O2 S2A C4 S2B -50.6(10) . . . . ? C3 S2A C4 S2B 65.4(8) . . . . ? O2 S2B C4 S2A 49.7(11) . . . . ? C3 S2B C4 S2A -69.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.869 _refine_diff_density_min -1.494 _refine_diff_density_rms 0.159 _database_code_depnum_ccdc_archive 'CCDC 958526' data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H54 I11 La O9 Pb4 S9' _chemical_formula_sum 'C18 H54 I11 La O9 Pb4 S9' _chemical_formula_weight 3066.72 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.634(3) _cell_length_b 15.6835(17) _cell_length_c 24.675(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.995(3) _cell_angle_gamma 90.00 _cell_volume 6858.7(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11901 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.970 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5384 _exptl_absorpt_coefficient_mu 15.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1459 _exptl_absorpt_correction_T_max 0.3036 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65503 _diffrn_reflns_av_R_equivalents 0.0802 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12527 _reflns_number_gt 10089 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0799P)^2^+128.3163P] 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 12527 _refine_ls_number_parameters 474 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.37361(7) 0.70192(9) 0.65220(5) 0.0639(4) Uani 1 1 d . . . Pb2 Pb 0.22623(7) 0.72184(8) 0.49329(5) 0.0649(3) Uani 1 1 d . . . Pb3 Pb 0.08718(7) 0.71645(8) 0.33048(5) 0.0636(3) Uani 1 1 d . . . Pb4 Pb 0.23264(7) 0.75664(8) 0.74352(5) 0.0641(3) Uani 1 1 d . . . I1 I 0.33180(13) 0.56588(14) 0.55275(9) 0.0722(6) Uani 1 1 d . . . I2 I 0.36576(15) 0.84061(15) 0.55574(10) 0.0768(7) Uani 1 1 d . . . I3 I 0.32300(16) 0.58052(15) 0.74477(10) 0.0734(7) Uani 1 1 d . . . I4 I 0.36984(15) 0.86100(17) 0.74194(10) 0.0767(7) Uani 1 1 d . . . I5 I 0.53789(15) 0.6615(2) 0.68549(12) 0.0841(11) Uani 1 1 d . . . I6 I 0.17013(13) 0.73320(16) 0.60438(8) 0.0689(6) Uani 1 1 d . . . I7 I 0.10858(14) 0.57501(15) 0.42163(10) 0.0717(7) Uani 1 1 d . . . I8 I 0.09500(15) 0.85574(16) 0.42895(11) 0.0748(7) Uani 1 1 d . . . I9 I -0.08155(14) 0.7084(2) 0.28538(13) 0.0849(9) Uani 1 1 d . . . I10 I 0.12628(15) 0.91596(15) 0.74057(10) 0.0800(7) Uani 1 1 d . . . I11 I 0.28370(12) 0.75959(15) 0.88120(8) 0.0669(6) Uani 1 1 d . . . La1 La 0.71802(10) 0.73995(11) 0.98074(7) 0.0642(4) Uani 1 1 d . . . O1 O 0.6322(11) 0.6413(17) 0.9194(12) 0.076(9) Uani 1 1 d D . . O2 O 0.5939(11) 0.8184(14) 0.9515(8) 0.068(6) Uani 1 1 d . . . O3 O 0.6631(15) 0.6518(14) 1.0407(9) 0.070(10) Uani 1 1 d D . . O4 O 0.7039(14) 0.7945(16) 0.8866(9) 0.078(12) Uani 1 1 d D . . O5 O 0.7954(13) 0.6379(14) 0.9461(9) 0.071(8) Uani 1 1 d D . . O6 O 0.8219(13) 0.8358(17) 0.9840(12) 0.077(11) Uani 1 1 d D . . O7 O 0.8278(10) 0.686(2) 1.0671(12) 0.079(13) Uani 1 1 d D . . O8 O 0.7159(15) 0.8331(16) 1.0604(9) 0.081(9) Uani 1 1 d D . . O9 O 0.1064(12) 0.8258(10) 0.2519(9) 0.068(7) Uani 1 1 d D . . S1 S 0.5539(8) 0.6125(13) 0.8916(8) 0.082(9) Uani 1 1 d D . . S2 S 0.5559(5) 0.8774(6) 0.9837(4) 0.068(3) Uani 1 1 d D . . S3A S 0.6833(11) 0.6019(11) 1.0945(7) 0.074(6) Uani 0.70 1 d PD . . S3B S 0.6338(16) 0.5715(16) 1.0556(11) 0.069(16) Uani 0.30 1 d PD . . S4A S 0.6548(10) 0.7871(13) 0.8269(7) 0.078(6) Uani 0.50 1 d PD . . S4B S 0.6809(10) 0.8644(11) 0.8420(6) 0.071(5) Uani 0.50 1 d PD . . S5 S 0.7840(9) 0.5798(11) 0.8956(7) 0.073(7) Uani 1 1 d D . . S6A S 0.8670(11) 0.8456(12) 0.9429(8) 0.078(6) Uani 0.50 1 d PD . . S6B S 0.8924(13) 0.8800(13) 0.9825(9) 0.078(8) Uani 0.50 1 d PD . . S7A S 0.9008(13) 0.658(2) 1.1105(11) 0.076(12) Uani 0.40 1 d PD . . S7B S 0.9076(10) 0.6943(15) 1.0716(9) 0.084(8) Uani 0.60 1 d PD . . S8 S 0.7651(5) 0.8850(6) 1.1093(4) 0.080(3) Uani 1 1 d D . . S9 S 0.0921(14) 0.9184(10) 0.2462(8) 0.080(12) Uani 1 1 d D . . C1 C 0.486(4) 0.687(4) 0.858(3) 0.075(11) Uani 1 1 d D . . H1A H 0.4788 0.7269 0.8851 0.090 Uiso 1 1 calc R . . H1B H 0.4391 0.6587 0.8392 0.090 Uiso 1 1 calc R . . H1C H 0.5022 0.7175 0.8296 0.090 Uiso 1 1 calc R . . C2 C 0.549(3) 0.541(3) 0.8371(14) 0.078(2) Uani 1 1 d D . . H2A H 0.5433 0.5712 0.8023 0.095 Uiso 1 1 calc R . . H2B H 0.5070 0.5032 0.8325 0.095 Uiso 1 1 calc R . . H2C H 0.5949 0.5078 0.8465 0.095 Uiso 1 1 calc R . . C3 C 0.4770(14) 0.915(2) 0.9294(13) 0.083(12) Uani 1 1 d D . . H3A H 0.4933 0.9410 0.9000 0.099 Uiso 1 1 calc R . . H3B H 0.4506 0.9564 0.9448 0.099 Uiso 1 1 calc R . . H3C H 0.4439 0.8682 0.9136 0.099 Uiso 1 1 calc R . . C4 C 0.512(3) 0.809(3) 1.017(2) 0.074(19) Uani 1 1 d . . . H4A H 0.4858 0.7665 0.9910 0.086 Uiso 1 1 calc R . . H4B H 0.4774 0.8406 1.0313 0.086 Uiso 1 1 calc R . . H4C H 0.5495 0.7827 1.0488 0.086 Uiso 1 1 calc R . . C5 C 0.707(3) 0.4989(17) 1.080(2) 0.071(19) Uani 1 1 d D . . C6 C 0.605(2) 0.584(3) 1.1159(18) 0.073(19) Uani 1 1 d D . . C7 C 0.5835(12) 0.868(2) 0.8092(14) 0.076(14) Uani 1 1 d D . . C8 C 0.707(2) 0.825(2) 0.7836(14) 0.076(13) Uani 1 1 d D . . C9 C 0.789(3) 0.4697(17) 0.910(2) 0.073(7) Uani 1 1 d D . . H9A H 0.8376 0.4559 0.9358 0.089 Uiso 1 1 calc R . . H9B H 0.7807 0.4385 0.8752 0.089 Uiso 1 1 calc R . . H9C H 0.7506 0.4545 0.9270 0.089 Uiso 1 1 calc R . . C10 C 0.8752(18) 0.589(3) 0.888(2) 0.083(7) Uani 1 1 d D . . H10A H 0.8951 0.6445 0.8994 0.099 Uiso 1 1 calc R . . H10B H 0.8718 0.5799 0.8484 0.099 Uiso 1 1 calc R . . H10C H 0.9079 0.5465 0.9108 0.099 Uiso 1 1 calc R . . C11 C 0.9597(19) 0.810(3) 0.970(2) 0.078(19) Uani 1 1 d D . . C12 C 0.866(3) 0.9549(19) 0.9269(19) 0.074(19) Uani 1 1 d D . . C13 C 0.956(2) 0.749(3) 1.1327(19) 0.069(2) Uani 1 1 d D . . C14 C 0.955(2) 0.600(2) 1.077(2) 0.069(2) Uani 1 1 d D . . C15 C 0.716(2) 0.9789(16) 1.1147(16) 0.074(12) Uani 1 1 d D . . H15A H 0.7143 1.0155 1.0830 0.091 Uiso 1 1 calc R . . H15B H 0.7422 1.0075 1.1496 0.091 Uiso 1 1 calc R . . H15C H 0.6661 0.9649 1.1142 0.091 Uiso 1 1 calc R . . C16 C 0.760(2) 0.830(3) 1.1697(14) 0.073(18) Uani 1 1 d D . . H16A H 0.7076 0.8238 1.1678 0.085 Uiso 1 1 calc R . . H16B H 0.7859 0.8617 1.2033 0.085 Uiso 1 1 calc R . . H16C H 0.7822 0.7748 1.1711 0.085 Uiso 1 1 calc R . . C17 C 0.076(4) 0.949(3) 0.1762(15) 0.079(12) Uani 1 1 d D . . H17A H 0.1231 0.9545 0.1686 0.090 Uiso 1 1 calc R . . H17B H 0.0497 1.0025 0.1697 0.090 Uiso 1 1 calc R . . H17C H 0.0456 0.9064 0.1514 0.090 Uiso 1 1 calc R . . C18 C 0.004(2) 0.939(3) 0.254(2) 0.080(12) Uani 1 1 d D . . H18A H -0.0318 0.9475 0.2172 0.090 Uiso 1 1 calc R . . H18B H 0.0073 0.9892 0.2767 0.090 Uiso 1 1 calc R . . H18C H -0.0107 0.8914 0.2725 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0654(8) 0.0814(9) 0.0447(7) -0.0016(6) 0.0168(6) 0.0010(6) Pb2 0.0671(8) 0.0710(8) 0.0515(6) -0.0013(6) 0.0121(6) 0.0016(6) Pb3 0.0586(7) 0.0688(8) 0.0592(7) 0.0029(6) 0.0133(6) 0.0015(6) Pb4 0.0678(8) 0.0684(8) 0.0563(7) -0.0016(5) 0.0108(6) 0.0012(6) I1 0.0780(15) 0.0662(14) 0.0677(14) -0.0029(11) 0.0156(12) 0.0071(11) I2 0.0951(19) 0.0727(15) 0.0624(14) -0.0049(11) 0.0225(13) -0.0160(13) I3 0.0753(19) 0.0742(16) 0.0762(16) 0.0091(12) 0.0319(15) 0.0162(14) I4 0.0685(17) 0.0950(18) 0.0734(16) -0.0075(13) 0.0249(14) -0.0234(14) I5 0.0663(16) 0.0903(3) 0.0830(19) -0.008(2) 0.0144(15) 0.0136(18) I6 0.0708(14) 0.0906(18) 0.0427(12) -0.0014(11) 0.0195(11) 0.0022(13) I7 0.0662(16) 0.0745(16) 0.0748(16) 0.0120(12) 0.0198(13) -0.0047(13) I8 0.0720(19) 0.0751(16) 0.0778(16) -0.0053(12) 0.0242(14) 0.0218(14) I9 0.0587(14) 0.0899(3) 0.098(2) 0.0088(17) 0.0129(14) 0.0066(15) I10 0.0905(18) 0.0728(16) 0.0732(16) 0.0163(12) 0.0208(14) 0.0104(13) I11 0.0661(13) 0.0935(16) 0.0427(11) 0.0005(10) 0.0191(10) 0.0054(11) La1 0.0622(10) 0.0580(11) 0.0716(11) 0.0014(8) 0.0194(9) 0.0047(8) O1 0.065(16) 0.072(2) 0.073(2) -0.013(18) -0.004(16) 0.011(15) O2 0.057(13) 0.094(16) 0.057(13) 0.018(11) 0.022(11) 0.015(11) O3 0.065(3) 0.073(2) 0.070(2) 0.005(17) 0.017(2) -0.014(2) O4 0.072(2) 0.068(2) 0.087(3) 0.015(2) 0.017(2) 0.015(2) O5 0.074(18) 0.084(17) 0.051(2) -0.019(14) 0.010(16) 0.008(14) O6 0.084(18) 0.071(2) 0.070(3) -0.014(2) 0.008(2) -0.020(16) O7 0.068(2) 0.071(4) 0.068(2) -0.014(2) -0.013(18) 0.02(2) O8 0.073(2) 0.082(2) 0.081(19) -0.023(16) 0.019(17) 0.017(18) O9 0.084(16) 0.042(12) 0.076(18) 0.012(12) 0.018(14) 0.022(11) S1 0.072(10) 0.066(2) 0.084(16) -0.013(16) -0.015(10) 0.011(12) S2 0.062(5) 0.070(7) 0.072(6) -0.011(5) 0.024(5) 0.009(5) S3A 0.054(17) 0.072(13) 0.097(13) 0.023(10) 0.007(13) 0.016(12) S3B 0.055(3) 0.081(3) 0.047(18) 0.015(17) -0.01(2) -0.001(3) S4A 0.080(11) 0.084(16) 0.059(12) 0.012(10) 0.009(10) -0.008(11) S4B 0.089(13) 0.068(12) 0.060(11) 0.010(9) 0.017(10) 0.004(10) S5 0.067(13) 0.076(15) 0.051(12) -0.025(12) 0.001(11) 0.013(12) S6A 0.085(13) 0.085(14) 0.060(15) -0.020(11) 0.017(12) -0.009(11) S6B 0.078(3) 0.088(15) 0.080(15) 0.015(12) 0.012(16) -0.006(16) S7A 0.074(19) 0.071(4) 0.068(2) -0.002(2) 0.012(18) -0.01(2) S7B 0.079(13) 0.069(2) 0.080(14) -0.019(14) -0.003(11) 0.007(14) S8 0.073(6) 0.082(7) 0.085(7) -0.007(5) 0.025(5) -0.004(5) S9 0.070(3) 0.068(12) 0.084(17) 0.016(11) 0.016(2) 0.014(17) C1 0.080(5) 0.066(19) 0.065(18) -0.011(16) -0.019(8) 0.000(8) C2 0.074(4) 0.065(5) 0.078(3) -0.013(3) 0.00(3) 0.018(4) C3 0.08(3) 0.08(3) 0.13(4) 0.01(2) 0.05(3) 0.00(2) C4 0.077(5) 0.073(4) 0.064(4) 0.014(3) 0.012(4) 0.003(3) C5 0.065(4) 0.069(5) 0.072(5) 0.015(4) 0.009(4) 0.014(3) C6 0.059(4) 0.081(5) 0.074(5) 0.015(4) 0.012(4) 0.004(3) C7 0.077(2) 0.078(4) 0.069(3) -0.01(3) 0.016(2) 0.013(3) C8 0.081(3) 0.070(3) 0.071(3) 0.00(2) 0.016(3) 0.002(2) C9 0.067(13) 0.076(15) 0.081(12) -0.015(12) 0.011(11) 0.013(12) C10 0.077(13) 0.056(15) 0.091(12) -0.015(12) 0.013(11) 0.008(12) C11 0.074(5) 0.075(4) 0.073(5) 0.02(3) 0.011(4) -0.01(3) C12 0.080(5) 0.065(4) 0.071(5) 0.002(3) 0.011(4) -0.01(3) C13 0.062(5) 0.074(4) 0.058(5) -0.013(3) 0.00(4) -0.002(4) C14 0.063(5) 0.066(4) 0.065(5) -0.003(3) 0.00(4) -0.011(4) C15 0.091(3) 0.065(2) 0.055(3) 0.001(19) 0.008(3) 0.013(2) C16 0.066(4) 0.070(4) 0.071(4) 0.013(3) -0.001(3) 0.005(3) C17 0.080(3) 0.068(12) 0.084(17) 0.016(11) 0.016(2) 0.014(17) C18 0.076(3) 0.067(12) 0.074(17) 0.008(11) 0.006(2) 0.021(17) _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 Pb1 I5 2.982(3) . ? Pb1 I1 3.162(3) . ? Pb1 I2 3.194(3) . ? Pb1 I3 3.326(3) . ? Pb1 I4 3.351(3) . ? Pb2 I2 3.183(3) . ? Pb2 I1 3.197(3) . ? Pb2 I6 3.226(2) . ? Pb2 I8 3.242(3) . ? Pb2 I11 3.273(2) 4_575 ? Pb2 I7 3.292(3) . ? Pb3 O9 2.694(19) . ? Pb3 I9 2.997(3) . ? Pb3 I7 3.096(3) . ? Pb3 I8 3.237(3) . ? Pb3 I10 3.281(3) 4_575 ? Pb4 O9 2.748(19) 4_576 ? Pb4 I4 3.046(3) . ? Pb4 I10 3.176(3) . ? Pb4 I3 3.230(3) . ? Pb4 I11 3.233(2) . ? Pb4 I6 3.288(2) . ? I10 Pb3 3.281(3) 4_576 ? I11 Pb2 3.273(2) 4_576 ? La1 O1 2.40(2) . ? La1 O4 2.413(19) . ? La1 O6 2.433(19) . ? La1 O8 2.46(2) . ? La1 O3 2.465(16) . ? La1 O5 2.476(17) . ? La1 O2 2.520(19) . ? La1 O7 2.60(2) . ? O1 S1 1.477(16) . ? O2 S2 1.53(2) . ? O3 S3B 1.465(17) . ? O3 S3A 1.486(16) . ? O4 S4A 1.480(18) . ? O4 S4B 1.518(17) . ? O5 S5 1.505(16) . ? O6 S6B 1.495(17) . ? O6 S6A 1.512(17) . ? O7 S7B 1.462(17) . ? O7 S7A 1.515(18) . ? O8 S8 1.508(16) . ? O9 S9 1.475(15) . ? O9 Pb4 2.748(19) 4_575 ? S1 C2 1.735(18) . ? S1 C1 1.74(2) . ? S2 C4 1.70(4) . ? S2 C3 1.759(18) . ? S3A C6 1.723(18) . ? S3A C5 1.743(18) . ? S3B C5 1.735(19) . ? S3B C6 1.741(19) . ? S4A C8 1.757(18) . ? S4A C7 1.787(18) . ? S4B C7 1.745(18) . ? S4B C8 1.774(18) . ? S5 C9 1.761(19) . ? S5 C10 1.776(19) . ? S6A C11 1.741(19) . ? S6A C12 1.757(19) . ? S6B C12 1.757(19) . ? S6B C11 1.763(19) . ? S7A C14 1.730(19) . ? S7A C13 1.751(19) . ? S7B C14 1.697(18) . ? S7B C13 1.727(18) . ? S8 C16 1.752(19) . ? S8 C15 1.755(17) . ? S9 C17 1.726(18) . ? S9 C18 1.732(19) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C9 H9A 0.9611 . ? C9 H9B 0.9611 . ? C9 H9C 0.9611 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9604 . ? C18 H18B 0.9604 . ? C18 H18C 0.9604 . ? 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 I5 Pb1 I1 93.23(8) . . ? I5 Pb1 I2 99.01(9) . . ? I1 Pb1 I2 86.42(7) . . ? I5 Pb1 I3 100.02(9) . . ? I1 Pb1 I3 95.31(7) . . ? I2 Pb1 I3 160.75(8) . . ? I5 Pb1 I4 101.85(9) . . ? I1 Pb1 I4 164.73(8) . . ? I2 Pb1 I4 88.85(7) . . ? I3 Pb1 I4 84.49(7) . . ? I2 Pb2 I1 86.03(7) . . ? I2 Pb2 I6 89.25(7) . . ? I1 Pb2 I6 88.12(7) . . ? I2 Pb2 I8 103.75(8) . . ? I1 Pb2 I8 169.84(8) . . ? I6 Pb2 I8 89.25(7) . . ? I2 Pb2 I11 85.72(6) . 4_575 ? I1 Pb2 I11 98.07(7) . 4_575 ? I6 Pb2 I11 171.72(8) . 4_575 ? I8 Pb2 I11 85.57(7) . 4_575 ? I2 Pb2 I7 168.02(8) . . ? I1 Pb2 I7 85.68(7) . . ? I6 Pb2 I7 99.10(7) . . ? I8 Pb2 I7 85.05(7) . . ? I11 Pb2 I7 86.90(6) 4_575 . ? O9 Pb3 I9 96.7(5) . . ? O9 Pb3 I7 164.4(4) . . ? I9 Pb3 I7 97.14(8) . . ? O9 Pb3 I8 97.2(4) . . ? I9 Pb3 I8 96.09(8) . . ? I7 Pb3 I8 88.42(7) . . ? O9 Pb3 I10 79.0(4) . 4_575 ? I9 Pb3 I10 98.56(8) . 4_575 ? I7 Pb3 I10 91.84(7) . 4_575 ? I8 Pb3 I10 165.20(8) . 4_575 ? O9 Pb4 I4 174.5(4) 4_576 . ? O9 Pb4 I10 80.2(4) 4_576 . ? I4 Pb4 I10 95.58(8) . . ? O9 Pb4 I3 93.0(4) 4_576 . ? I4 Pb4 I3 91.29(8) . . ? I10 Pb4 I3 173.08(8) . . ? O9 Pb4 I11 84.7(5) 4_576 . ? I4 Pb4 I11 91.72(7) . . ? I10 Pb4 I11 89.53(6) . . ? I3 Pb4 I11 91.08(7) . . ? O9 Pb4 I6 89.5(5) 4_576 . ? I4 Pb4 I6 94.29(7) . . ? I10 Pb4 I6 92.68(7) . . ? I3 Pb4 I6 85.98(7) . . ? I11 Pb4 I6 173.36(7) . . ? Pb1 I1 Pb2 79.00(6) . . ? Pb2 I2 Pb1 78.74(6) . . ? Pb4 I3 Pb1 76.20(6) . . ? Pb4 I4 Pb1 78.31(6) . . ? Pb2 I6 Pb4 142.20(8) . . ? Pb3 I7 Pb2 78.69(6) . . ? Pb3 I8 Pb2 77.45(6) . . ? Pb4 I10 Pb3 75.75(6) . 4_576 ? Pb4 I11 Pb2 145.33(8) . 4_576 ? O1 La1 O4 76.6(10) . . ? O1 La1 O6 142.1(9) . . ? O4 La1 O6 70.2(10) . . ? O1 La1 O8 135.7(9) . . ? O4 La1 O8 122.4(9) . . ? O6 La1 O8 79.4(9) . . ? O1 La1 O3 72.4(10) . . ? O4 La1 O3 146.5(9) . . ? O6 La1 O3 143.2(9) . . ? O8 La1 O3 75.0(9) . . ? O1 La1 O5 73.2(8) . . ? O4 La1 O5 78.4(8) . . ? O6 La1 O5 82.5(8) . . ? O8 La1 O5 144.6(8) . . ? O3 La1 O5 103.8(9) . . ? O1 La1 O2 76.1(8) . . ? O4 La1 O2 74.6(7) . . ? O6 La1 O2 111.0(9) . . ? O8 La1 O2 72.5(8) . . ? O3 La1 O2 86.1(8) . . ? O5 La1 O2 142.8(7) . . ? O1 La1 O7 120.7(10) . . ? O4 La1 O7 136.8(9) . . ? O6 La1 O7 76.0(10) . . ? O8 La1 O7 75.0(9) . . ? O3 La1 O7 72.1(9) . . ? O5 La1 O7 71.2(8) . . ? O2 La1 O7 144.6(8) . . ? S1 O1 La1 149.5(17) . . ? S2 O2 La1 132.6(12) . . ? S3B O3 S3A 48.2(11) . . ? S3B O3 La1 152.8(18) . . ? S3A O3 La1 142.6(17) . . ? S4A O4 S4B 52.1(12) . . ? S4A O4 La1 141.3(17) . . ? S4B O4 La1 151.2(16) . . ? S5 O5 La1 136.8(14) . . ? S6B O6 S6A 42.4(11) . . ? S6B O6 La1 168.9(18) . . ? S6A O6 La1 130.0(16) . . ? S7B O7 S7A 45.8(12) . . ? S7B O7 La1 123.8(19) . . ? S7A O7 La1 169(2) . . ? S8 O8 La1 143.5(17) . . ? S9 O9 Pb3 129.4(13) . . ? S9 O9 Pb4 126.1(14) . 4_575 ? Pb3 O9 Pb4 93.5(5) . 4_575 ? O1 S1 C2 111(2) . . ? O1 S1 C1 119(3) . . ? C2 S1 C1 102(3) . . ? O2 S2 C4 103.9(18) . . ? O2 S2 C3 102.6(15) . . ? C4 S2 C3 100(2) . . ? O3 S3A C6 111.0(14) . . ? O3 S3A C5 108.3(14) . . ? C6 S3A C5 101.6(13) . . ? O3 S3B C5 109.7(15) . . ? O3 S3B C6 111.1(15) . . ? C5 S3B C6 101.2(13) . . ? O4 S4A C8 106.8(18) . . ? O4 S4A C7 111.9(17) . . ? C8 S4A C7 97.2(18) . . ? O4 S4B C7 112.2(17) . . ? O4 S4B C8 104.3(17) . . ? C7 S4B C8 98.2(18) . . ? O5 S5 C9 116(2) . . ? O5 S5 C10 99(2) . . ? C9 S5 C10 96(3) . . ? O6 S6A C11 114(2) . . ? O6 S6A C12 106(2) . . ? C11 S6A C12 110(3) . . ? O6 S6B C12 107(3) . . ? O6 S6B C11 113(2) . . ? C12 S6B C11 109(3) . . ? O7 S7A C14 110.0(16) . . ? O7 S7A C13 107.2(16) . . ? C14 S7A C13 101.5(14) . . ? O7 S7B C14 114.5(16) . . ? O7 S7B C13 111.0(15) . . ? C14 S7B C13 103.8(13) . . ? O8 S8 C16 104(2) . . ? O8 S8 C15 108.2(18) . . ? C16 S8 C15 100.4(19) . . ? O9 S9 C17 109.8(15) . . ? O9 S9 C18 108.7(16) . . ? C17 S9 C18 100(3) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? S2 C3 H3A 109.5 . . ? S2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S3B C5 S3A 40.5(9) . . ? S3A C6 S3B 40.7(9) . . ? S4B C7 S4A 43.7(9) . . ? S4A C8 S4B 43.8(9) . . ? S5 C9 H9A 109.6 . . ? S5 C9 H9B 109.6 . . ? H9A C9 H9B 109.4 . . ? S5 C9 H9C 109.6 . . ? H9A C9 H9C 109.4 . . ? H9B C9 H9C 109.4 . . ? S5 C10 H10A 109.5 . . ? S5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? S6A C11 S6B 36.2(9) . . ? S6B C12 S6A 36.1(9) . . ? S7B C13 S7A 39.0(11) . . ? S7B C14 S7A 39.6(11) . . ? S8 C15 H15A 109.5 . . ? S8 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S8 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? S8 C16 H16A 109.5 . . ? S8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S9 C17 H17A 109.5 . . ? S9 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S9 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S9 C18 H18A 109.5 . . ? S9 C18 H18B 109.5 . . ? H18A C18 H18B 109.4 . . ? S9 C18 H18C 109.5 . . ? H18A C18 H18C 109.4 . . ? H18B C18 H18C 109.4 . . ? 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 I5 Pb1 I1 Pb2 -138.44(8) . . . . ? I2 Pb1 I1 Pb2 -39.60(7) . . . . ? I3 Pb1 I1 Pb2 121.17(7) . . . . ? I4 Pb1 I1 Pb2 32.6(3) . . . . ? I2 Pb2 I1 Pb1 39.79(6) . . . . ? I6 Pb2 I1 Pb1 -49.59(6) . . . . ? I8 Pb2 I1 Pb1 -124.7(4) . . . . ? I11 Pb2 I1 Pb1 124.90(6) 4_575 . . . ? I7 Pb2 I1 Pb1 -148.86(7) . . . . ? I1 Pb2 I2 Pb1 -39.36(6) . . . . ? I6 Pb2 I2 Pb1 48.81(6) . . . . ? I8 Pb2 I2 Pb1 137.86(7) . . . . ? I11 Pb2 I2 Pb1 -137.77(7) 4_575 . . . ? I7 Pb2 I2 Pb1 -85.6(3) . . . . ? I5 Pb1 I2 Pb2 132.57(8) . . . . ? I1 Pb1 I2 Pb2 39.86(6) . . . . ? I3 Pb1 I2 Pb2 -56.0(2) . . . . ? I4 Pb1 I2 Pb2 -125.62(7) . . . . ? O9 Pb4 I3 Pb1 142.1(5) 4_576 . . . ? I4 Pb4 I3 Pb1 -41.41(7) . . . . ? I10 Pb4 I3 Pb1 131.8(6) . . . . ? I11 Pb4 I3 Pb1 -133.16(6) . . . . ? I6 Pb4 I3 Pb1 52.80(6) . . . . ? I5 Pb1 I3 Pb4 138.24(8) . . . . ? I1 Pb1 I3 Pb4 -127.52(7) . . . . ? I2 Pb1 I3 Pb4 -33.1(2) . . . . ? I4 Pb1 I3 Pb4 37.15(6) . . . . ? O9 Pb4 I4 Pb1 -178(5) 4_576 . . . ? I10 Pb4 I4 Pb1 -138.56(7) . . . . ? I3 Pb4 I4 Pb1 40.62(6) . . . . ? I11 Pb4 I4 Pb1 131.74(6) . . . . ? I6 Pb4 I4 Pb1 -45.44(7) . . . . ? I5 Pb1 I4 Pb4 -138.54(9) . . . . ? I1 Pb1 I4 Pb4 50.6(3) . . . . ? I2 Pb1 I4 Pb4 122.49(7) . . . . ? I3 Pb1 I4 Pb4 -39.43(7) . . . . ? I2 Pb2 I6 Pb4 -29.44(15) . . . . ? I1 Pb2 I6 Pb4 56.60(15) . . . . ? I8 Pb2 I6 Pb4 -133.21(14) . . . . ? I11 Pb2 I6 Pb4 -82.0(5) 4_575 . . . ? I7 Pb2 I6 Pb4 141.92(14) . . . . ? O9 Pb4 I6 Pb2 -154.9(4) 4_576 . . . ? I4 Pb4 I6 Pb2 29.15(16) . . . . ? I10 Pb4 I6 Pb2 124.95(14) . . . . ? I3 Pb4 I6 Pb2 -61.85(15) . . . . ? I11 Pb4 I6 Pb2 -125.7(6) . . . . ? O9 Pb3 I7 Pb2 71.3(17) . . . . ? I9 Pb3 I7 Pb2 -136.15(8) . . . . ? I8 Pb3 I7 Pb2 -40.21(7) . . . . ? I10 Pb3 I7 Pb2 124.99(7) 4_575 . . . ? I2 Pb2 I7 Pb3 -97.6(3) . . . . ? I1 Pb2 I7 Pb3 -143.86(7) . . . . ? I6 Pb2 I7 Pb3 128.74(7) . . . . ? I8 Pb2 I7 Pb3 40.29(6) . . . . ? I11 Pb2 I7 Pb3 -45.52(6) 4_575 . . . ? O9 Pb3 I8 Pb2 -124.2(5) . . . . ? I9 Pb3 I8 Pb2 138.21(8) . . . . ? I7 Pb3 I8 Pb2 41.19(7) . . . . ? I10 Pb3 I8 Pb2 -50.0(3) 4_575 . . . ? I2 Pb2 I8 Pb3 133.34(7) . . . . ? I1 Pb2 I8 Pb3 -62.6(4) . . . . ? I6 Pb2 I8 Pb3 -137.62(7) . . . . ? I11 Pb2 I8 Pb3 48.84(6) 4_575 . . . ? I7 Pb2 I8 Pb3 -38.41(6) . . . . ? O9 Pb4 I10 Pb3 36.8(5) 4_576 . . 4_576 ? I4 Pb4 I10 Pb3 -139.66(7) . . . 4_576 ? I3 Pb4 I10 Pb3 47.2(6) . . . 4_576 ? I11 Pb4 I10 Pb3 -47.98(6) . . . 4_576 ? I6 Pb4 I10 Pb3 125.77(6) . . . 4_576 ? O9 Pb4 I11 Pb2 -36.1(4) 4_576 . . 4_576 ? I4 Pb4 I11 Pb2 139.64(15) . . . 4_576 ? I10 Pb4 I11 Pb2 44.07(15) . . . 4_576 ? I3 Pb4 I11 Pb2 -129.04(15) . . . 4_576 ? I6 Pb4 I11 Pb2 -65.5(7) . . . 4_576 ? O4 La1 O1 S1 -97(4) . . . . ? O6 La1 O1 S1 -126(4) . . . . ? O8 La1 O1 S1 26(5) . . . . ? O3 La1 O1 S1 70(4) . . . . ? O5 La1 O1 S1 -179(4) . . . . ? O2 La1 O1 S1 -20(4) . . . . ? O7 La1 O1 S1 126(4) . . . . ? O1 La1 O2 S2 141.1(18) . . . . ? O4 La1 O2 S2 -139.2(18) . . . . ? O6 La1 O2 S2 -78.0(17) . . . . ? O8 La1 O2 S2 -7.2(16) . . . . ? O3 La1 O2 S2 68.4(17) . . . . ? O5 La1 O2 S2 176.1(14) . . . . ? O7 La1 O2 S2 17(3) . . . . ? O1 La1 O3 S3B 36(4) . . . . ? O4 La1 O3 S3B 58(4) . . . . ? O6 La1 O3 S3B -127(4) . . . . ? O8 La1 O3 S3B -175(4) . . . . ? O5 La1 O3 S3B -31(4) . . . . ? O2 La1 O3 S3B 112(4) . . . . ? O7 La1 O3 S3B -96(4) . . . . ? O1 La1 O3 S3A 134(3) . . . . ? O4 La1 O3 S3A 156(2) . . . . ? O6 La1 O3 S3A -29(4) . . . . ? O8 La1 O3 S3A -77(3) . . . . ? O5 La1 O3 S3A 67(3) . . . . ? O2 La1 O3 S3A -150(3) . . . . ? O7 La1 O3 S3A 2(3) . . . . ? O1 La1 O4 S4A 16(3) . . . . ? O6 La1 O4 S4A 177(3) . . . . ? O8 La1 O4 S4A -120(3) . . . . ? O3 La1 O4 S4A -6(4) . . . . ? O5 La1 O4 S4A 91(3) . . . . ? O2 La1 O4 S4A -63(3) . . . . ? O7 La1 O4 S4A 136(2) . . . . ? O1 La1 O4 S4B 119(4) . . . . ? O6 La1 O4 S4B -80(4) . . . . ? O8 La1 O4 S4B -17(4) . . . . ? O3 La1 O4 S4B 97(4) . . . . ? O5 La1 O4 S4B -166(4) . . . . ? O2 La1 O4 S4B 40(4) . . . . ? O7 La1 O4 S4B -120(3) . . . . ? O1 La1 O5 S5 24(2) . . . . ? O4 La1 O5 S5 -55(2) . . . . ? O6 La1 O5 S5 -127(3) . . . . ? O8 La1 O5 S5 174(2) . . . . ? O3 La1 O5 S5 90(2) . . . . ? O2 La1 O5 S5 -12(3) . . . . ? O7 La1 O5 S5 156(3) . . . . ? O1 La1 O6 S6B -53(11) . . . . ? O4 La1 O6 S6B -84(11) . . . . ? O8 La1 O6 S6B 146(11) . . . . ? O3 La1 O6 S6B 100(10) . . . . ? O5 La1 O6 S6B -3(11) . . . . ? O2 La1 O6 S6B -147(11) . . . . ? O7 La1 O6 S6B 69(11) . . . . ? O1 La1 O6 S6A -10(3) . . . . ? O4 La1 O6 S6A -41(2) . . . . ? O8 La1 O6 S6A -171(3) . . . . ? O3 La1 O6 S6A 143(2) . . . . ? O5 La1 O6 S6A 40(2) . . . . ? O2 La1 O6 S6A -105(2) . . . . ? O7 La1 O6 S6A 112(3) . . . . ? O1 La1 O7 S7B 114(2) . . . . ? O4 La1 O7 S7B 10(3) . . . . ? O6 La1 O7 S7B -29(2) . . . . ? O8 La1 O7 S7B -112(2) . . . . ? O3 La1 O7 S7B 170(2) . . . . ? O5 La1 O7 S7B 57(2) . . . . ? O2 La1 O7 S7B -135.8(18) . . . . ? O1 La1 O7 S7A 103(11) . . . . ? O4 La1 O7 S7A -1(12) . . . . ? O6 La1 O7 S7A -40(11) . . . . ? O8 La1 O7 S7A -123(11) . . . . ? O3 La1 O7 S7A 159(11) . . . . ? O5 La1 O7 S7A 47(11) . . . . ? O2 La1 O7 S7A -147(10) . . . . ? O1 La1 O8 S8 164(2) . . . . ? O4 La1 O8 S8 -91(3) . . . . ? O6 La1 O8 S8 -33(3) . . . . ? O3 La1 O8 S8 121(3) . . . . ? O5 La1 O8 S8 28(4) . . . . ? O2 La1 O8 S8 -149(3) . . . . ? O7 La1 O8 S8 46(3) . . . . ? I9 Pb3 O9 S9 74.4(19) . . . . ? I7 Pb3 O9 S9 -133.0(16) . . . . ? I8 Pb3 O9 S9 -22.6(19) . . . . ? I10 Pb3 O9 S9 172(2) 4_575 . . . ? I9 Pb3 O9 Pb4 -140.9(5) . . . 4_575 ? I7 Pb3 O9 Pb4 12(2) . . . 4_575 ? I8 Pb3 O9 Pb4 122.1(5) . . . 4_575 ? I10 Pb3 O9 Pb4 -43.5(4) 4_575 . . 4_575 ? La1 O1 S1 C2 165(4) . . . . ? La1 O1 S1 C1 47(6) . . . . ? La1 O2 S2 C4 -84(2) . . . . ? La1 O2 S2 C3 172.5(17) . . . . ? S3B O3 S3A C6 -54.9(15) . . . . ? La1 O3 S3A C6 162(3) . . . . ? S3B O3 S3A C5 55.7(15) . . . . ? La1 O3 S3A C5 -87(3) . . . . ? S3A O3 S3B C5 -56.9(15) . . . . ? La1 O3 S3B C5 69(4) . . . . ? S3A O3 S3B C6 54.2(15) . . . . ? La1 O3 S3B C6 -180(4) . . . . ? S4B O4 S4A C8 56.4(15) . . . . ? La1 O4 S4A C8 -160(2) . . . . ? S4B O4 S4A C7 -48.9(16) . . . . ? La1 O4 S4A C7 95(3) . . . . ? S4A O4 S4B C7 50.7(16) . . . . ? La1 O4 S4B C7 -79(4) . . . . ? S4A O4 S4B C8 -54.6(16) . . . . ? La1 O4 S4B C8 176(3) . . . . ? La1 O5 S5 C9 -113(3) . . . . ? La1 O5 S5 C10 146(2) . . . . ? S6B O6 S6A C11 59(2) . . . . ? La1 O6 S6A C11 -110(3) . . . . ? S6B O6 S6A C12 -62.4(19) . . . . ? La1 O6 S6A C12 129(3) . . . . ? S6A O6 S6B C12 62.9(18) . . . . ? La1 O6 S6B C12 114(11) . . . . ? S6A O6 S6B C11 -57(2) . . . . ? La1 O6 S6B C11 -7(12) . . . . ? S7B O7 S7A C14 -53.1(15) . . . . ? La1 O7 S7A C14 -41(12) . . . . ? S7B O7 S7A C13 56.4(15) . . . . ? La1 O7 S7A C13 69(11) . . . . ? S7A O7 S7B C14 57.4(17) . . . . ? La1 O7 S7B C14 -120(2) . . . . ? S7A O7 S7B C13 -59.7(16) . . . . ? La1 O7 S7B C13 123(3) . . . . ? La1 O8 S8 C16 -112(3) . . . . ? La1 O8 S8 C15 142(3) . . . . ? Pb3 O9 S9 C17 -155(3) . . . . ? Pb4 O9 S9 C17 70(3) 4_575 . . . ? Pb3 O9 S9 C18 -46(3) . . . . ? Pb4 O9 S9 C18 179(2) 4_575 . . . ? O3 S3B C5 S3A 55.0(14) . . . . ? C6 S3B C5 S3A -62.4(13) . . . . ? O3 S3A C5 S3B -53.1(13) . . . . ? C6 S3A C5 S3B 63.8(13) . . . . ? O3 S3A C6 S3B 51.9(14) . . . . ? C5 S3A C6 S3B -63.0(13) . . . . ? O3 S3B C6 S3A -53.0(14) . . . . ? C5 S3B C6 S3A 63.3(14) . . . . ? O4 S4B C7 S4A -47.0(15) . . . . ? C8 S4B C7 S4A 62.2(13) . . . . ? O4 S4A C7 S4B 48.4(15) . . . . ? C8 S4A C7 S4B -63.0(13) . . . . ? O4 S4A C8 S4B -54.3(15) . . . . ? C7 S4A C8 S4B 61.2(13) . . . . ? O4 S4B C8 S4A 51.5(15) . . . . ? C7 S4B C8 S4A -64.1(14) . . . . ? O6 S6A C11 S6B -55.9(18) . . . . ? C12 S6A C11 S6B 62.8(19) . . . . ? O6 S6B C11 S6A 57(2) . . . . ? C12 S6B C11 S6A -62(2) . . . . ? O6 S6B C12 S6A -61.3(17) . . . . ? C11 S6B C12 S6A 61.4(19) . . . . ? O6 S6A C12 S6B 59.7(18) . . . . ? C11 S6A C12 S6B -64(2) . . . . ? O7 S7B C13 S7A 58.5(16) . . . . ? C14 S7B C13 S7A -65.1(15) . . . . ? O7 S7A C13 S7B -53.5(14) . . . . ? C14 S7A C13 S7B 61.8(14) . . . . ? O7 S7B C14 S7A -56.2(17) . . . . ? C13 S7B C14 S7A 65.0(14) . . . . ? O7 S7A C14 S7B 50.9(15) . . . . ? C13 S7A C14 S7B -62.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.422 _refine_diff_density_min -1.817 _refine_diff_density_rms 0.278 _database_code_depnum_ccdc_archive 'CCDC 958527' data_m14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H54 I11 O9 Pb4 Pr S9' _chemical_formula_sum 'C18 H54 I11 O9 Pb4 Pr S9' _chemical_formula_weight 3068.72 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 '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 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.549(4) _cell_length_b 15.654(3) _cell_length_c 24.592(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.85(3) _cell_angle_gamma 90.00 _cell_volume 6797(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20771 _cell_measurement_theta_min 3.0770 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.999 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5392 _exptl_absorpt_coefficient_mu 15.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0488 _exptl_absorpt_correction_T_max 0.1094 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56867 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12345 _reflns_number_gt 8275 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0629P)^2^+88.4934P] 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 12345 _refine_ls_number_parameters 513 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.37420(7) 0.79759(7) 0.65235(4) 0.0677(3) Uani 1 1 d . . . Pb2 Pb 0.22595(6) 0.77771(7) 0.49308(4) 0.0642(3) Uani 1 1 d . . . Pb3 Pb 0.08672(6) 0.78427(7) 0.33076(4) 0.0674(3) Uani 1 1 d . . . Pb4 Pb 0.23218(6) 0.75774(7) 0.24333(4) 0.0637(3) Uani 1 1 d . . . I1 I 0.33199(11) 0.93328(12) 0.55280(8) 0.0671(5) Uani 1 1 d . . . I2 I 0.36654(14) 0.65887(12) 0.55548(9) 0.0788(6) Uani 1 1 d . . . I3 I 0.16949(12) 0.76586(13) 0.60452(8) 0.0698(6) Uani 1 1 d . . . I4 I 0.32290(14) 0.91897(13) 0.74462(9) 0.0835(7) Uani 1 1 d . . . I5 I 0.36945(13) 0.63754(14) 0.74130(9) 0.0821(6) Uani 1 1 d . . . I6 I 0.53869(13) 0.8384(2) 0.68548(11) 0.1091(9) Uani 1 1 d . . . I7 I 0.10791(13) 0.92429(14) 0.42247(10) 0.0779(7) Uani 1 1 d . . . I8 I 0.09434(14) 0.64363(13) 0.42870(9) 0.0755(7) Uani 1 1 d . . . I9 I 0.28415(11) 0.75954(13) 0.38134(7) 0.0640(5) Uani 1 1 d . . . I10 I 0.12596(13) 0.91789(13) 0.24131(9) 0.0763(6) Uani 1 1 d . . . I11 I -0.08213(13) 0.79287(18) 0.28601(12) 0.1017(8) Uani 1 1 d . . . Pr1 Pr 0.71731(8) 0.75955(9) 0.97981(6) 0.0667(4) Uani 1 1 d . . . O1 O 0.7131(12) 0.6638(14) 1.0579(10) 0.090(7) Uani 1 1 d . . . O2 O 0.5976(11) 0.6820(12) 0.9516(8) 0.073(5) Uani 1 1 d . . . O3 O 0.7912(16) 0.8631(16) 0.9445(13) 0.088(8) Uani 1 1 d . . . O4 O 0.6310(12) 0.8580(13) 0.9190(10) 0.095(6) Uani 1 1 d . . . O5 O 0.6982(17) 0.7094(16) 0.8837(11) 0.085(9) Uani 1 1 d . . . O6 O 0.6662(17) 0.8503(14) 1.0401(9) 0.081(10) Uani 1 1 d . . . O7 O 0.8251(16) 0.804(2) 1.0619(16) 0.091(15) Uani 1 1 d . . . O8 O 0.8181(13) 0.6645(15) 0.9828(14) 0.074(10) Uani 1 1 d . . . O9 O 0.1073(13) 0.6754(12) 0.2519(9) 0.083(7) Uani 1 1 d D . . S1 S 0.7660(5) 0.6179(5) 1.1064(3) 0.078(2) Uani 1 1 d D . . S2 S 0.5563(4) 0.6227(5) 0.9830(3) 0.074(2) Uani 1 1 d . . . S3 S 0.7808(8) 0.9168(10) 0.8951(5) 0.097(6) Uani 1 1 d D . . S4A S 0.5631(12) 0.8561(13) 0.8713(12) 0.113(10) Uani 0.50 1 d PD . . S4B S 0.5507(13) 0.8935(16) 0.8957(10) 0.095(7) Uani 0.50 1 d PD . . S5A S 0.6557(9) 0.7124(11) 0.8295(7) 0.075(5) Uani 0.50 1 d PD . . S5B S 0.6797(9) 0.6385(11) 0.8424(6) 0.071(4) Uani 0.50 1 d PD . . S6A S 0.6837(10) 0.8978(11) 1.0921(7) 0.084(6) Uani 0.70 1 d P . . S6B S 0.6368(17) 0.923(2) 1.0547(12) 0.081(17) Uani 0.30 1 d PD . . S7 S 0.8999(8) 0.8163(12) 1.0768(8) 0.102(9) Uani 1 1 d D . . S8A S 0.8668(10) 0.6535(10) 0.9446(9) 0.087(5) Uani 0.60 1 d P . . S8B S 0.8806(19) 0.6140(15) 0.9829(11) 0.083(12) Uani 0.40 1 d PD . . S9A S 0.059(2) 0.5952(15) 0.2429(11) 0.102(13) Uani 0.50 1 d PD . . S9B S 0.1094(14) 0.5747(19) 0.2424(17) 0.101(17) Uani 0.50 1 d PD . . C1 C 0.760(2) 0.671(2) 1.1678(11) 0.105(12) Uani 1 1 d D . . H1A H 0.7708 0.7304 1.1654 0.157 Uiso 1 1 calc R . . H1B H 0.7957 0.6464 1.2010 0.157 Uiso 1 1 calc R . . H1C H 0.7096 0.6645 1.1706 0.157 Uiso 1 1 calc R . . C2 C 0.7163(16) 0.5251(15) 1.1133(13) 0.084(10) Uani 1 1 d D . . H2A H 0.6762 0.5397 1.1287 0.126 Uiso 1 1 calc R . . H2B H 0.7503 0.4857 1.1385 0.126 Uiso 1 1 calc R . . H2C H 0.6952 0.4991 1.0765 0.126 Uiso 1 1 calc R . . C3 C 0.509(2) 0.692(2) 1.0160(13) 0.087(14) Uani 1 1 d . . . H3A H 0.5451 0.7224 1.0464 0.128 Uiso 1 1 calc R . . H3B H 0.4753 0.6605 1.0313 0.128 Uiso 1 1 calc R . . H3C H 0.4801 0.7329 0.9884 0.128 Uiso 1 1 calc R . . C4 C 0.4773(16) 0.584(2) 0.9298(15) 0.098(12) Uani 1 1 d . . . H4A H 0.4490 0.6310 0.9086 0.148 Uiso 1 1 calc R . . H4B H 0.4459 0.5520 0.9470 0.148 Uiso 1 1 calc R . . H4C H 0.4937 0.5475 0.9044 0.148 Uiso 1 1 calc R . . C5 C 0.816(5) 1.019(2) 0.910(2) 0.086(5) Uani 1 1 d D . . H5A H 0.8122 1.0489 0.8755 0.121 Uiso 1 1 calc R . . H5B H 0.8681 1.0165 0.9335 0.121 Uiso 1 1 calc R . . H5C H 0.7872 1.0491 0.9309 0.121 Uiso 1 1 calc R . . C6 C 0.851(2) 0.900(2) 0.8616(18) 0.100(8) Uani 1 1 d D . . H6A H 0.8876 0.9452 0.8721 0.137 Uiso 1 1 calc R . . H6B H 0.8278 0.9001 0.8209 0.137 Uiso 1 1 calc R . . H6C H 0.8751 0.8462 0.8735 0.137 Uiso 1 1 calc R . . C7 C 0.5499(18) 0.9587(17) 0.8400(15) 0.095(6) Uani 1 1 d D . . C8 C 0.4748(18) 0.821(4) 0.872(3) 0.097(10) Uani 1 1 d D . . C9 C 0.7039(17) 0.676(2) 0.7821(10) 0.074(11) Uani 1 1 d D . . C10 C 0.5839(12) 0.631(2) 0.8074(14) 0.083(13) Uani 1 1 d D . . C11 C 0.607(3) 0.911(4) 1.1160(19) 0.097(3) Uani 1 1 d D . . C12 C 0.707(3) 1.001(3) 1.080(2) 0.087(2) Uani 1 1 d D . . C13 C 0.950(3) 0.743(3) 1.1248(18) 0.098(2) Uani 1 1 d . . . H13A H 0.9241 0.7308 1.1521 0.130 Uiso 1 1 calc R . . H13B H 0.9995 0.7656 1.1443 0.130 Uiso 1 1 calc R . . H13C H 0.9553 0.6915 1.1052 0.130 Uiso 1 1 calc R . . C14 C 0.936(2) 0.910(2) 1.111(2) 0.094(15) Uani 1 1 d D . . H14A H 0.9049 0.9568 1.0926 0.126 Uiso 1 1 calc R . . H14B H 0.9866 0.9177 1.1104 0.126 Uiso 1 1 calc R . . H14C H 0.9356 0.9067 1.1503 0.126 Uiso 1 1 calc R . . C15 C 0.949(4) 0.679(4) 0.968(4) 0.091(7) Uani 1 1 d D . . C16 C 0.864(2) 0.545(2) 0.9261(18) 0.084(13) Uani 1 1 d . . . C17 C 0.048(5) 0.558(4) 0.1731(13) 0.094(8) Uani 1 1 d D . . C18A C 0.102(3) 0.538(5) 0.2830(16) 0.098(2) Uani 0.60 1 d PD . . C18B C 0.044(4) 0.540(3) 0.277(2) 0.082(7) Uani 0.40 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 Pb1 0.0579(7) 0.0766(8) 0.0665(6) 0.0011(5) 0.0143(6) -0.0005(6) Pb2 0.0584(7) 0.0655(7) 0.0638(6) 0.0014(5) 0.0098(6) -0.0026(5) Pb3 0.0712(7) 0.0623(7) 0.0628(6) -0.0028(5) 0.0116(6) -0.0018(5) Pb4 0.0596(7) 0.0627(7) 0.0693(6) -0.0027(5) 0.0188(6) -0.0003(5) I1 0.0670(13) 0.0595(11) 0.0710(13) 0.0040(9) 0.0153(11) -0.0051(9) I2 0.1014(17) 0.0631(12) 0.0685(13) 0.0042(9) 0.0211(13) 0.0166(11) I3 0.0649(13) 0.0997(15) 0.0455(10) 0.0013(9) 0.0177(10) -0.0049(11) I4 0.1036(18) 0.0706(13) 0.0799(15) -0.0099(10) 0.0333(14) -0.0178(12) I5 0.0821(16) 0.0875(15) 0.0775(14) 0.0096(11) 0.0255(13) 0.0238(12) I6 0.0554(14) 0.181(3) 0.0835(17) 0.0058(16) 0.0099(13) -0.0104(15) I7 0.0849(16) 0.0802(14) 0.0634(15) -0.0132(11) 0.0165(13) 0.0031(12) I8 0.0751(17) 0.0700(13) 0.0818(15) 0.0063(11) 0.0219(13) -0.0215(12) I9 0.0583(12) 0.0891(13) 0.0436(10) 0.0011(9) 0.0144(10) 0.0059(10) I10 0.0797(16) 0.0679(13) 0.0775(14) 0.0136(10) 0.0167(13) 0.0081(11) I11 0.0503(13) 0.140(2) 0.106(2) -0.0071(16) 0.0112(14) -0.0058(13) Pr1 0.0703(8) 0.0615(8) 0.0656(9) -0.0003(6) 0.0167(7) -0.0030(6) O1 0.067(15) 0.097(16) 0.082(17) 0.014(13) 0.020(14) -0.010(12) O2 0.062(13) 0.075(13) 0.079(14) -0.006(10) 0.020(12) -0.017(10) O3 0.073(2) 0.100(15) 0.087(2) 0.036(14) 0.017(17) 0.003(14) O4 0.059(12) 0.088(13) 0.121(16) 0.019(11) 0.002(12) 0.006(10) O5 0.075(3) 0.082(2) 0.090(2) -0.043(16) 0.019(2) -0.027(18) O6 0.079(3) 0.097(17) 0.076(15) -0.024(12) 0.026(18) 0.021(18) O7 0.082(17) 0.087(2) 0.083(3) 0.014(2) -0.018(2) -0.016(16) O8 0.074(17) 0.087(17) 0.082(3) 0.024(17) 0.062(19) 0.036(14) O9 0.103(2) 0.064(13) 0.077(14) -0.022(11) 0.020(14) -0.021(13) S1 0.075(5) 0.080(5) 0.068(5) 0.010(4) 0.008(5) 0.004(4) S2 0.077(5) 0.075(5) 0.066(5) 0.013(4) 0.016(4) -0.006(4) S3 0.094(13) 0.097(13) 0.098(8) 0.016(8) 0.023(9) -0.013(11) S4A 0.065(15) 0.091(16) 0.14(2) -0.013(14) -0.027(15) 0.026(11) S4B 0.075(14) 0.113(19) 0.102(17) 0.043(14) 0.033(13) 0.027(14) S5A 0.074(12) 0.085(12) 0.057(10) 0.003(8) 0.008(10) -0.012(9) S5B 0.083(12) 0.073(11) 0.060(10) 0.001(8) 0.025(9) -0.006(9) S6A 0.084(14) 0.0719(12) 0.103(13) -0.054(10) 0.038(12) 0.003(10) S6B 0.082(3) 0.075(3) 0.057(18) -0.001(18) -0.025(19) 0.003(3) S7 0.094(10) 0.087(2) 0.081(18) 0.039(15) -0.041(11) -0.019(12) S8A 0.092(12) 0.078(11) 0.0960(17) 0.009(11) 0.036(13) 0.015(9) S8B 0.091(3) 0.067(15) 0.089(17) 0.032(13) 0.026(2) 0.022(18) S9A 0.090(4) 0.080(16) 0.12(2) -0.036(14) 0.01(2) -0.04(2) S9B 0.10(2) 0.082(2) 0.091(5) -0.03(2) 0.012(3) -0.026(17) C1 0.08(3) 0.094(3) 0.10(3) 0.00(2) 0.02(2) -0.01(2) C2 0.08(2) 0.08(2) 0.09(2) 0.027(17) 0.01(2) -0.018(17) C3 0.107(4) 0.083(3) 0.07(2) -0.015(2) 0.029(3) -0.04(3) C4 0.039(18) 0.10(2) 0.13(3) 0.00(2) -0.02(2) -0.021(17) C5 0.092(15) 0.080(4) 0.075(5) -0.016(3) 0.014(7) -0.020(6) C6 0.103(2) 0.100(15) 0.107(2) 0.036(14) 0.047(17) 0.003(14) C7 0.059(12) 0.088(13) 0.121(16) 0.019(11) 0.002(12) 0.006(10) C8 0.073(3) 0.096(18) 0.090(17) 0.017(15) -0.016(5) -0.01(6) C9 0.077(2) 0.086(3) 0.054(19) -0.005(19) 0.015(18) -0.02(2) C10 0.077(2) 0.086(4) 0.102(3) -0.04(3) 0.05(2) -0.03(2) C11 0.104(5) 0.081(8) 0.093(6) -0.015(6) 0.011(5) -0.018(5) C12 0.075(7) 0.091(4) 0.090(5) 0.013(3) 0.019(5) -0.009(4) C13 0.103(4) 0.094(6) 0.09(3) 0.02(3) 0.02(3) 0.03(4) C14 0.082(17) 0.087(2) 0.083(3) 0.014(2) -0.018(2) -0.026(16) C15 0.087(6) 0.077(13) 0.099(13) -0.033(11) 0.021(8) -0.017(8) C16 0.073(3) 0.079(3) 0.094(3) -0.04(2) 0.017(3) -0.02(2) C17 0.088(2) 0.078(7) 0.111(7) -0.020(6) 0.019(11) -0.021(10) C18A 0.091(3) 0.094(16) 0.094(4) -0.017(2) 0.03(3) -0.013(19) C18B 0.097(15) 0.081(3) 0.073(13) -0.019(5) 0.037(14) -0.07(5) _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 Pb1 I6 2.976(3) . ? Pb1 I1 3.153(2) . ? Pb1 I2 3.194(2) . ? Pb1 I4 3.315(2) . ? Pb1 I5 3.345(2) . ? Pb1 I3 3.648(3) . ? Pb2 I2 3.188(2) . ? Pb2 I1 3.192(2) . ? Pb2 I3 3.225(2) . ? Pb2 I8 3.240(2) . ? Pb2 I9 3.258(2) . ? Pb2 I7 3.278(3) . ? Pb3 O9 2.696(19) . ? Pb3 I11 2.988(3) . ? Pb3 I7 3.083(2) . ? Pb3 I8 3.234(2) . ? Pb3 I10 3.275(2) . ? Pb3 I9 3.509(2) . ? Pb4 O9 2.72(2) . ? Pb4 I5 3.042(2) 4_575 ? Pb4 I10 3.180(2) . ? Pb4 I9 3.231(2) . ? Pb4 I4 3.233(2) 4_575 ? Pb4 I3 3.272(2) 4_575 ? I3 Pb4 3.272(2) 4_576 ? I4 Pb4 3.233(2) 4_576 ? I5 Pb4 3.042(2) 4_576 ? Pr1 O8 2.37(2) . ? Pr1 O4 2.39(2) . ? Pr1 O5 2.41(2) . ? Pr1 O2 2.437(18) . ? Pr1 O6 2.444(19) . ? Pr1 O3 2.45(2) . ? Pr1 O1 2.46(2) . ? Pr1 O7 2.46(3) . ? O1 S1 1.48(2) . ? O2 S2 1.552(19) . ? O3 S3 1.44(3) . ? O4 S4A 1.44(3) . ? O4 S4B 1.53(3) . ? O5 S5A 1.32(3) . ? O5 S5B 1.47(3) . ? O6 S6B 1.36(3) . ? O6 S6A 1.43(2) . ? O7 S7 1.34(3) . ? O8 S8B 1.40(3) . ? O8 S8A 1.50(3) . ? O9 S9A 1.512(18) . ? O9 S9B 1.60(4) . ? S1 C1 1.756(18) . ? S1 C2 1.757(16) . ? S2 C4 1.75(3) . ? S2 C3 1.75(3) . ? S3 C5 1.729(19) . ? S3 C6 1.756(18) . ? S4A S4B 0.92(3) . ? S4A C8 1.734(19) . ? S4A C7 1.766(18) . ? S4B C7 1.71(4) . ? S4B C8 1.76(2) . ? S5A S5B 1.24(2) . ? S5A C9 1.767(17) . ? S5A C10 1.798(18) . ? S5B C10 1.725(18) . ? S5B C9 1.777(17) . ? S6A S6B 1.13(3) . ? S6A C11 1.71(5) . ? S6A C12 1.72(4) . ? S6B C12 1.75(2) . ? S6B C11 1.77(2) . ? S7 C13 1.71(4) . ? S7 C14 1.718(19) . ? S8A S8B 1.09(2) . ? S8A C15 1.51(6) . ? S8A C16 1.76(4) . ? S8B C16 1.72(4) . ? S8B C15 1.75(2) . ? S9A S9B 0.98(4) . ? S9A C18B 1.29(4) . ? S9A C18A 1.39(7) . ? S9A C17 1.762(19) . ? S9B C18A 1.19(5) . ? S9B C17 1.75(2) . ? S9B C18B 1.76(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9601 . ? C6 H6B 0.9601 . ? C6 H6C 0.9601 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 I6 Pb1 I1 93.30(8) . . ? I6 Pb1 I2 99.07(8) . . ? I1 Pb1 I2 86.29(6) . . ? I6 Pb1 I4 100.07(8) . . ? I1 Pb1 I4 95.18(6) . . ? I2 Pb1 I4 160.68(7) . . ? I6 Pb1 I5 102.25(8) . . ? I1 Pb1 I5 164.21(7) . . ? I2 Pb1 I5 88.54(6) . . ? I4 Pb1 I5 84.89(6) . . ? I6 Pb1 I3 174.77(8) . . ? I1 Pb1 I3 81.68(6) . . ? I2 Pb1 I3 82.13(6) . . ? I4 Pb1 I3 79.04(6) . . ? I5 Pb1 I3 82.84(6) . . ? I2 Pb2 I1 85.75(6) . . ? I2 Pb2 I3 89.33(6) . . ? I1 Pb2 I3 88.15(6) . . ? I2 Pb2 I8 103.87(7) . . ? I1 Pb2 I8 169.98(7) . . ? I3 Pb2 I8 89.18(6) . . ? I2 Pb2 I9 85.49(6) . . ? I1 Pb2 I9 97.92(6) . . ? I3 Pb2 I9 171.68(6) . . ? I8 Pb2 I9 85.77(6) . . ? I2 Pb2 I7 168.12(7) . . ? I1 Pb2 I7 85.81(6) . . ? I3 Pb2 I7 98.75(7) . . ? I8 Pb2 I7 85.05(7) . . ? I9 Pb2 I7 87.40(6) . . ? O9 Pb3 I11 97.3(5) . . ? O9 Pb3 I7 164.1(5) . . ? I11 Pb3 I7 96.98(8) . . ? O9 Pb3 I8 97.0(4) . . ? I11 Pb3 I8 96.12(8) . . ? I7 Pb3 I8 88.42(7) . . ? O9 Pb3 I10 79.1(4) . . ? I11 Pb3 I10 98.49(8) . . ? I7 Pb3 I10 91.87(7) . . ? I8 Pb3 I10 165.24(7) . . ? O9 Pb3 I9 79.8(5) . . ? I11 Pb3 I9 176.19(7) . . ? I7 Pb3 I9 86.21(6) . . ? I8 Pb3 I9 81.85(6) . . ? I10 Pb3 I9 83.44(6) . . ? O9 Pb4 I5 174.7(4) . 4_575 ? O9 Pb4 I10 80.6(5) . . ? I5 Pb4 I10 95.32(7) 4_575 . ? O9 Pb4 I9 84.8(4) . . ? I5 Pb4 I9 91.77(7) 4_575 . ? I10 Pb4 I9 89.62(6) . . ? O9 Pb4 I4 92.7(5) . 4_575 ? I5 Pb4 I4 91.46(7) 4_575 4_575 ? I10 Pb4 I4 173.21(7) . 4_575 ? I9 Pb4 I4 90.60(6) . 4_575 ? O9 Pb4 I3 89.3(4) . 4_575 ? I5 Pb4 I3 94.31(7) 4_575 4_575 ? I10 Pb4 I3 93.00(6) . 4_575 ? I9 Pb4 I3 173.12(6) . 4_575 ? I4 Pb4 I3 86.05(6) 4_575 4_575 ? Pb1 I1 Pb2 79.31(5) . . ? Pb2 I2 Pb1 78.76(6) . . ? Pb2 I3 Pb4 142.08(7) . 4_576 ? Pb2 I3 Pb1 71.89(5) . . ? Pb4 I3 Pb1 71.17(5) 4_576 . ? Pb4 I4 Pb1 76.15(5) 4_576 . ? Pb4 I5 Pb1 78.29(6) 4_576 . ? Pb3 I7 Pb2 78.72(6) . . ? Pb3 I8 Pb2 77.14(5) . . ? Pb4 I9 Pb2 144.81(7) . . ? Pb4 I9 Pb3 71.69(5) . . ? Pb2 I9 Pb3 73.12(5) . . ? Pb4 I10 Pb3 75.53(5) . . ? O8 Pr1 O4 142.6(9) . . ? O8 Pr1 O5 72.8(11) . . ? O4 Pr1 O5 74.2(9) . . ? O8 Pr1 O2 109.7(8) . . ? O4 Pr1 O2 76.5(7) . . ? O5 Pr1 O2 73.2(7) . . ? O8 Pr1 O6 142.5(10) . . ? O4 Pr1 O6 72.2(8) . . ? O5 Pr1 O6 144.7(10) . . ? O2 Pr1 O6 88.5(9) . . ? O8 Pr1 O3 84.6(9) . . ? O4 Pr1 O3 72.0(8) . . ? O5 Pr1 O3 78.3(9) . . ? O2 Pr1 O3 142.1(8) . . ? O6 Pr1 O3 101.1(10) . . ? O8 Pr1 O1 78.8(9) . . ? O4 Pr1 O1 135.0(8) . . ? O5 Pr1 O1 122.5(8) . . ? O2 Pr1 O1 71.0(7) . . ? O6 Pr1 O1 76.7(8) . . ? O3 Pr1 O1 146.8(9) . . ? O8 Pr1 O7 73.6(12) . . ? O4 Pr1 O7 123.4(10) . . ? O5 Pr1 O7 137.1(12) . . ? O2 Pr1 O7 144.3(10) . . ? O6 Pr1 O7 73.0(12) . . ? O3 Pr1 O7 72.7(11) . . ? O1 Pr1 O7 75.2(9) . . ? S1 O1 Pr1 139.1(13) . . ? S2 O2 Pr1 134.5(11) . . ? S3 O3 Pr1 137.8(18) . . ? S4A O4 S4B 35.9(12) . . ? S4A O4 Pr1 138.6(16) . . ? S4B O4 Pr1 149.2(16) . . ? S5A O5 S5B 52.6(12) . . ? S5A O5 Pr1 147(2) . . ? S5B O5 Pr1 148.7(16) . . ? S6B O6 S6A 47.6(13) . . ? S6B O6 Pr1 155(2) . . ? S6A O6 Pr1 145.3(19) . . ? S7 O7 Pr1 141(3) . . ? S8B O8 S8A 43.9(13) . . ? S8B O8 Pr1 175(2) . . ? S8A O8 Pr1 132.2(17) . . ? S9A O9 S9B 36.8(16) . . ? S9A O9 Pb3 115.0(16) . . ? S9B O9 Pb3 138.1(17) . . ? S9A O9 Pb4 149.2(19) . . ? S9B O9 Pb4 113.5(14) . . ? Pb3 O9 Pb4 93.9(5) . . ? O1 S1 C1 105.3(16) . . ? O1 S1 C2 104.0(14) . . ? C1 S1 C2 97.6(17) . . ? O2 S2 C4 105.2(15) . . ? O2 S2 C3 104.7(14) . . ? C4 S2 C3 98.0(18) . . ? O3 S3 C5 114(2) . . ? O3 S3 C6 112(2) . . ? C5 S3 C6 87(3) . . ? S4B S4A O4 77(3) . . ? S4B S4A C8 76.3(18) . . ? O4 S4A C8 126(3) . . ? S4B S4A C7 71(2) . . ? O4 S4A C7 107.9(19) . . ? C8 S4A C7 107(2) . . ? S4A S4B O4 67(2) . . ? S4A S4B C7 78(2) . . ? O4 S4B C7 106.7(19) . . ? S4A S4B C8 73.2(17) . . ? O4 S4B C8 119(2) . . ? C7 S4B C8 108(2) . . ? S5B S5A O5 69.8(16) . . ? S5B S5A C9 69.8(11) . . ? O5 S5A C9 112.8(18) . . ? S5B S5A C10 66.2(11) . . ? O5 S5A C10 115.9(18) . . ? C9 S5A C10 92.9(16) . . ? S5A S5B O5 57.6(15) . . ? S5A S5B C10 72.5(11) . . ? O5 S5B C10 112.3(18) . . ? S5A S5B C9 69.0(10) . . ? O5 S5B C9 105.2(16) . . ? C10 S5B C9 95.1(16) . . ? S6B S6A O6 63.1(18) . . ? S6B S6A C11 74(2) . . ? O6 S6A C11 113(2) . . ? S6B S6A C12 73(2) . . ? O6 S6A C12 110(2) . . ? C11 S6A C12 103(3) . . ? S6A S6B O6 69.3(17) . . ? S6A S6B C12 70(2) . . ? O6 S6B C12 111(3) . . ? S6A S6B C11 68(2) . . ? O6 S6B C11 113(3) . . ? C12 S6B C11 99(3) . . ? O7 S7 C13 113(2) . . ? O7 S7 C14 118(3) . . ? C13 S7 C14 101(2) . . ? S8B S8A O8 63.3(19) . . ? S8B S8A C15 83(3) . . ? O8 S8A C15 118(3) . . ? S8B S8A C16 70(2) . . ? O8 S8A C16 107.1(18) . . ? C15 S8A C16 107(3) . . ? S8A S8B O8 72.8(19) . . ? S8A S8B C16 74(2) . . ? O8 S8B C16 114(3) . . ? S8A S8B C15 59(3) . . ? O8 S8B C15 109(3) . . ? C16 S8B C15 99(3) . . ? S9B S9A C18B 101(4) . . ? S9B S9A C18A 57(3) . . ? C18B S9A C18A 46(3) . . ? S9B S9A O9 76(3) . . ? C18B S9A O9 134(3) . . ? C18A S9A O9 104(3) . . ? S9B S9A C17 73.1(17) . . ? C18B S9A C17 116(2) . . ? C18A S9A C17 110(3) . . ? O9 S9A C17 108(3) . . ? S9A S9B C18A 79(4) . . ? S9A S9B O9 67(2) . . ? C18A S9B O9 110(4) . . ? S9A S9B C17 74.4(17) . . ? C18A S9B C17 123(3) . . ? O9 S9B C17 104(3) . . ? S9A S9B C18B 46(3) . . ? C18A S9B C18B 35(3) . . ? O9 S9B C18B 100(2) . . ? C17 S9B C18B 95.3(14) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.4 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? S2 C3 H3A 109.5 . . ? S2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S3 C5 H5A 110.0 . . ? S3 C5 H5B 110.5 . . ? H5A C5 H5B 110.0 . . ? S3 C5 H5C 109.0 . . ? H5A C5 H5C 109.1 . . ? H5B C5 H5C 108.0 . . ? S3 C6 H6A 109.9 . . ? S3 C6 H6B 109.0 . . ? H6A C6 H6B 109.5 . . ? S3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S4B C7 S4A 30.6(10) . . ? S4A C8 S4B 30.4(10) . . ? S5A C9 S5B 41.1(8) . . ? S5B C10 S5A 41.3(8) . . ? S6A C11 S6B 37.8(11) . . ? S6A C12 S6B 37.8(10) . . ? S7 C13 H13A 109.5 . . ? S7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? S7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? S7 C14 H14A 109.5 . . ? S7 C14 H14B 109.5 . . ? H14A C14 H14B 111.0 . . ? S7 C14 H14C 109.4 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? S8A C15 S8B 38.1(10) . . ? S8B C16 S8A 36.4(11) . . ? S9B C17 S9A 32.5(14) . . ? S9B C18A S9A 44(2) . . ? S9A C18B S9B 33(2) . . ? 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 I6 Pb1 I1 Pb2 138.62(7) . . . . ? I2 Pb1 I1 Pb2 39.73(6) . . . . ? I4 Pb1 I1 Pb2 -120.95(6) . . . . ? I5 Pb1 I1 Pb2 -31.4(2) . . . . ? I3 Pb1 I1 Pb2 -42.85(5) . . . . ? I2 Pb2 I1 Pb1 -39.85(6) . . . . ? I3 Pb2 I1 Pb1 49.61(6) . . . . ? I8 Pb2 I1 Pb1 124.2(4) . . . . ? I9 Pb2 I1 Pb1 -124.69(6) . . . . ? I7 Pb2 I1 Pb1 148.53(6) . . . . ? I1 Pb2 I2 Pb1 39.33(6) . . . . ? I3 Pb2 I2 Pb1 -48.87(6) . . . . ? I8 Pb2 I2 Pb1 -137.85(6) . . . . ? I9 Pb2 I2 Pb1 137.64(6) . . . . ? I7 Pb2 I2 Pb1 84.2(3) . . . . ? I6 Pb1 I2 Pb2 -132.62(7) . . . . ? I1 Pb1 I2 Pb2 -39.87(6) . . . . ? I4 Pb1 I2 Pb2 55.2(2) . . . . ? I5 Pb1 I2 Pb2 125.20(6) . . . . ? I3 Pb1 I2 Pb2 42.23(5) . . . . ? I2 Pb2 I3 Pb4 29.41(13) . . . 4_576 ? I1 Pb2 I3 Pb4 -56.37(12) . . . 4_576 ? I8 Pb2 I3 Pb4 133.29(12) . . . 4_576 ? I9 Pb2 I3 Pb4 80.8(4) . . . 4_576 ? I7 Pb2 I3 Pb4 -141.84(12) . . . 4_576 ? I2 Pb2 I3 Pb1 42.88(5) . . . . ? I1 Pb2 I3 Pb1 -42.89(5) . . . . ? I8 Pb2 I3 Pb1 146.77(6) . . . . ? I9 Pb2 I3 Pb1 94.2(4) . . . . ? I7 Pb2 I3 Pb1 -128.36(6) . . . . ? I6 Pb1 I3 Pb2 60.4(8) . . . . ? I1 Pb1 I3 Pb2 44.09(5) . . . . ? I2 Pb1 I3 Pb2 -43.28(5) . . . . ? I4 Pb1 I3 Pb2 141.06(6) . . . . ? I5 Pb1 I3 Pb2 -132.79(6) . . . . ? I6 Pb1 I3 Pb4 -128.3(8) . . . 4_576 ? I1 Pb1 I3 Pb4 -144.61(6) . . . 4_576 ? I2 Pb1 I3 Pb4 128.01(6) . . . 4_576 ? I4 Pb1 I3 Pb4 -47.65(5) . . . 4_576 ? I5 Pb1 I3 Pb4 38.51(5) . . . 4_576 ? I6 Pb1 I4 Pb4 -138.43(7) . . . 4_576 ? I1 Pb1 I4 Pb4 127.29(6) . . . 4_576 ? I2 Pb1 I4 Pb4 33.7(2) . . . 4_576 ? I5 Pb1 I4 Pb4 -36.86(6) . . . 4_576 ? I3 Pb1 I4 Pb4 46.82(5) . . . 4_576 ? I6 Pb1 I5 Pb4 138.43(7) . . . 4_576 ? I1 Pb1 I5 Pb4 -51.8(2) . . . 4_576 ? I2 Pb1 I5 Pb4 -122.60(7) . . . 4_576 ? I4 Pb1 I5 Pb4 39.21(6) . . . 4_576 ? I3 Pb1 I5 Pb4 -40.35(5) . . . 4_576 ? O9 Pb3 I7 Pb2 -69.9(17) . . . . ? I11 Pb3 I7 Pb2 136.41(7) . . . . ? I8 Pb3 I7 Pb2 40.44(6) . . . . ? I10 Pb3 I7 Pb2 -124.80(6) . . . . ? I9 Pb3 I7 Pb2 -41.49(5) . . . . ? I2 Pb2 I7 Pb3 98.7(3) . . . . ? I1 Pb2 I7 Pb3 143.61(6) . . . . ? I3 Pb2 I7 Pb3 -128.91(6) . . . . ? I8 Pb2 I7 Pb3 -40.51(6) . . . . ? I9 Pb2 I7 Pb3 45.46(6) . . . . ? O9 Pb3 I8 Pb2 123.7(5) . . . . ? I11 Pb3 I8 Pb2 -138.16(7) . . . . ? I7 Pb3 I8 Pb2 -41.30(6) . . . . ? I10 Pb3 I8 Pb2 50.0(3) . . . . ? I9 Pb3 I8 Pb2 45.10(5) . . . . ? I2 Pb2 I8 Pb3 -133.51(6) . . . . ? I1 Pb2 I8 Pb3 62.9(4) . . . . ? I3 Pb2 I8 Pb3 137.38(6) . . . . ? I9 Pb2 I8 Pb3 -49.22(5) . . . . ? I7 Pb2 I8 Pb3 38.52(6) . . . . ? O9 Pb4 I9 Pb2 -36.5(5) . . . . ? I5 Pb4 I9 Pb2 139.35(12) 4_575 . . . ? I10 Pb4 I9 Pb2 44.05(13) . . . . ? I4 Pb4 I9 Pb2 -129.17(12) 4_575 . . . ? I3 Pb4 I9 Pb2 -68.5(6) 4_575 . . . ? O9 Pb4 I9 Pb3 -35.4(5) . . . . ? I5 Pb4 I9 Pb3 140.51(6) 4_575 . . . ? I10 Pb4 I9 Pb3 45.20(5) . . . . ? I4 Pb4 I9 Pb3 -128.01(6) 4_575 . . . ? I3 Pb4 I9 Pb3 -67.3(5) 4_575 . . . ? I2 Pb2 I9 Pb4 150.76(12) . . . . ? I1 Pb2 I9 Pb4 -124.17(12) . . . . ? I3 Pb2 I9 Pb4 99.2(4) . . . . ? I8 Pb2 I9 Pb4 46.46(13) . . . . ? I7 Pb2 I9 Pb4 -38.77(13) . . . . ? I2 Pb2 I9 Pb3 149.61(6) . . . . ? I1 Pb2 I9 Pb3 -125.32(5) . . . . ? I3 Pb2 I9 Pb3 98.0(4) . . . . ? I8 Pb2 I9 Pb3 45.31(5) . . . . ? I7 Pb2 I9 Pb3 -39.91(5) . . . . ? O9 Pb3 I9 Pb4 36.2(4) . . . . ? I11 Pb3 I9 Pb4 76.8(11) . . . . ? I7 Pb3 I9 Pb4 -136.22(6) . . . . ? I8 Pb3 I9 Pb4 134.83(6) . . . . ? I10 Pb3 I9 Pb4 -43.90(5) . . . . ? O9 Pb3 I9 Pb2 -144.5(4) . . . . ? I11 Pb3 I9 Pb2 -103.9(11) . . . . ? I7 Pb3 I9 Pb2 43.08(6) . . . . ? I8 Pb3 I9 Pb2 -45.86(5) . . . . ? I10 Pb3 I9 Pb2 135.40(6) . . . . ? O9 Pb4 I10 Pb3 36.6(4) . . . . ? I5 Pb4 I10 Pb3 -139.95(6) 4_575 . . . ? I9 Pb4 I10 Pb3 -48.21(5) . . . . ? I4 Pb4 I10 Pb3 43.7(6) 4_575 . . . ? I3 Pb4 I10 Pb3 125.43(6) 4_575 . . . ? O9 Pb3 I10 Pb4 -37.1(5) . . . . ? I11 Pb3 I10 Pb4 -132.98(7) . . . . ? I7 Pb3 I10 Pb4 129.68(6) . . . . ? I8 Pb3 I10 Pb4 38.8(3) . . . . ? I9 Pb3 I10 Pb4 43.71(5) . . . . ? O8 Pr1 O1 S1 38(2) . . . . ? O4 Pr1 O1 S1 -160.3(18) . . . . ? O5 Pr1 O1 S1 99(2) . . . . ? O2 Pr1 O1 S1 154(2) . . . . ? O6 Pr1 O1 S1 -113(2) . . . . ? O3 Pr1 O1 S1 -23(3) . . . . ? O7 Pr1 O1 S1 -38(2) . . . . ? O8 Pr1 O2 S2 79.5(17) . . . . ? O4 Pr1 O2 S2 -139.1(17) . . . . ? O5 Pr1 O2 S2 143.6(18) . . . . ? O6 Pr1 O2 S2 -67.0(16) . . . . ? O3 Pr1 O2 S2 -173.3(14) . . . . ? O1 Pr1 O2 S2 9.4(15) . . . . ? O7 Pr1 O2 S2 -10(3) . . . . ? O8 Pr1 O3 S3 123(3) . . . . ? O4 Pr1 O3 S3 -28(2) . . . . ? O5 Pr1 O3 S3 49(3) . . . . ? O2 Pr1 O3 S3 7(3) . . . . ? O6 Pr1 O3 S3 -95(3) . . . . ? O1 Pr1 O3 S3 -177(2) . . . . ? O7 Pr1 O3 S3 -163(3) . . . . ? O8 Pr1 O4 S4A 76(3) . . . . ? O5 Pr1 O4 S4A 47(3) . . . . ? O2 Pr1 O4 S4A -29(3) . . . . ? O6 Pr1 O4 S4A -122(3) . . . . ? O3 Pr1 O4 S4A 130(3) . . . . ? O1 Pr1 O4 S4A -73(3) . . . . ? O7 Pr1 O4 S4A -176(3) . . . . ? O8 Pr1 O4 S4B 137(3) . . . . ? O5 Pr1 O4 S4B 108(4) . . . . ? O2 Pr1 O4 S4B 32(3) . . . . ? O6 Pr1 O4 S4B -61(4) . . . . ? O3 Pr1 O4 S4B -170(4) . . . . ? O1 Pr1 O4 S4B -13(4) . . . . ? O7 Pr1 O4 S4B -116(4) . . . . ? O8 Pr1 O5 S5A -179(3) . . . . ? O4 Pr1 O5 S5A -17(3) . . . . ? O2 Pr1 O5 S5A 63(3) . . . . ? O6 Pr1 O5 S5A 1(4) . . . . ? O3 Pr1 O5 S5A -92(3) . . . . ? O1 Pr1 O5 S5A 117(3) . . . . ? O7 Pr1 O5 S5A -140(3) . . . . ? O8 Pr1 O5 S5B 68(4) . . . . ? O4 Pr1 O5 S5B -130(4) . . . . ? O2 Pr1 O5 S5B -49(4) . . . . ? O6 Pr1 O5 S5B -111(4) . . . . ? O3 Pr1 O5 S5B 156(4) . . . . ? O1 Pr1 O5 S5B 4(4) . . . . ? O7 Pr1 O5 S5B 108(4) . . . . ? O8 Pr1 O6 S6B 133(5) . . . . ? O4 Pr1 O6 S6B -29(6) . . . . ? O5 Pr1 O6 S6B -48(6) . . . . ? O2 Pr1 O6 S6B -106(6) . . . . ? O3 Pr1 O6 S6B 37(6) . . . . ? O1 Pr1 O6 S6B -177(6) . . . . ? O7 Pr1 O6 S6B 105(6) . . . . ? O8 Pr1 O6 S6A 25(4) . . . . ? O4 Pr1 O6 S6A -138(3) . . . . ? O5 Pr1 O6 S6A -156(3) . . . . ? O2 Pr1 O6 S6A 146(3) . . . . ? O3 Pr1 O6 S6A -71(3) . . . . ? O1 Pr1 O6 S6A 75(3) . . . . ? O7 Pr1 O6 S6A -3(3) . . . . ? O8 Pr1 O7 S7 43(3) . . . . ? O4 Pr1 O7 S7 -100(3) . . . . ? O5 Pr1 O7 S7 3(4) . . . . ? O2 Pr1 O7 S7 144(3) . . . . ? O6 Pr1 O7 S7 -154(4) . . . . ? O3 Pr1 O7 S7 -46(3) . . . . ? O1 Pr1 O7 S7 126(4) . . . . ? O4 Pr1 O8 S8B 51(29) . . . . ? O5 Pr1 O8 S8B 79(29) . . . . ? O2 Pr1 O8 S8B 144(29) . . . . ? O6 Pr1 O8 S8B -101(29) . . . . ? O3 Pr1 O8 S8B 0(29) . . . . ? O1 Pr1 O8 S8B -151(29) . . . . ? O7 Pr1 O8 S8B -73(29) . . . . ? O4 Pr1 O8 S8A 14(3) . . . . ? O5 Pr1 O8 S8A 43(2) . . . . ? O2 Pr1 O8 S8A 107(2) . . . . ? O6 Pr1 O8 S8A -138(2) . . . . ? O3 Pr1 O8 S8A -36(2) . . . . ? O1 Pr1 O8 S8A 172(2) . . . . ? O7 Pr1 O8 S8A -110(2) . . . . ? I11 Pb3 O9 S9A -50.5(19) . . . . ? I7 Pb3 O9 S9A 155.8(15) . . . . ? I8 Pb3 O9 S9A 46.6(19) . . . . ? I10 Pb3 O9 S9A -147.8(19) . . . . ? I9 Pb3 O9 S9A 127.0(19) . . . . ? I11 Pb3 O9 S9B -87(2) . . . . ? I7 Pb3 O9 S9B 119(2) . . . . ? I8 Pb3 O9 S9B 10(2) . . . . ? I10 Pb3 O9 S9B 176(2) . . . . ? I9 Pb3 O9 S9B 90(2) . . . . ? I11 Pb3 O9 Pb4 140.6(5) . . . . ? I7 Pb3 O9 Pb4 -13(2) . . . . ? I8 Pb3 O9 Pb4 -122.3(5) . . . . ? I10 Pb3 O9 Pb4 43.3(4) . . . . ? I9 Pb3 O9 Pb4 -41.9(5) . . . . ? I5 Pb4 O9 S9A -165(4) 4_575 . . . ? I10 Pb4 O9 S9A 155(3) . . . . ? I9 Pb4 O9 S9A -114(3) . . . . ? I4 Pb4 O9 S9A -24(3) 4_575 . . . ? I3 Pb4 O9 S9A 62(3) 4_575 . . . ? I5 Pb4 O9 S9B -152(4) 4_575 . . . ? I10 Pb4 O9 S9B 167.9(19) . . . . ? I9 Pb4 O9 S9B -101.7(19) . . . . ? I4 Pb4 O9 S9B -11.3(19) 4_575 . . . ? I3 Pb4 O9 S9B 74.7(19) 4_575 . . . ? I5 Pb4 O9 Pb3 -5(6) 4_575 . . . ? I10 Pb4 O9 Pb3 -44.7(5) . . . . ? I9 Pb4 O9 Pb3 45.8(5) . . . . ? I4 Pb4 O9 Pb3 136.2(5) 4_575 . . . ? I3 Pb4 O9 Pb3 -137.8(5) 4_575 . . . ? Pr1 O1 S1 C1 110(2) . . . . ? Pr1 O1 S1 C2 -148(2) . . . . ? Pr1 O2 S2 C4 -173.7(16) . . . . ? Pr1 O2 S2 C3 84(2) . . . . ? Pr1 O3 S3 C5 137(4) . . . . ? Pr1 O3 S3 C6 -125(3) . . . . ? Pr1 O4 S4A S4B 130(3) . . . . ? S4B O4 S4A C8 -62(3) . . . . ? Pr1 O4 S4A C8 68(4) . . . . ? S4B O4 S4A C7 65(2) . . . . ? Pr1 O4 S4A C7 -165(2) . . . . ? C8 S4A S4B O4 133(2) . . . . ? C7 S4A S4B O4 -114.1(17) . . . . ? O4 S4A S4B C7 114.1(17) . . . . ? C8 S4A S4B C7 -113(2) . . . . ? O4 S4A S4B C8 -133(2) . . . . ? C7 S4A S4B C8 113(2) . . . . ? Pr1 O4 S4B S4A -100(4) . . . . ? S4A O4 S4B C7 -69(2) . . . . ? Pr1 O4 S4B C7 -169(3) . . . . ? S4A O4 S4B C8 54(3) . . . . ? Pr1 O4 S4B C8 -47(5) . . . . ? Pr1 O5 S5A S5B -143(3) . . . . ? S5B O5 S5A C9 -56.5(15) . . . . ? Pr1 O5 S5A C9 161(2) . . . . ? S5B O5 S5A C10 48.9(16) . . . . ? Pr1 O5 S5A C10 -94(3) . . . . ? C9 S5A S5B O5 125.1(18) . . . . ? C10 S5A S5B O5 -132.2(18) . . . . ? O5 S5A S5B C10 132.2(18) . . . . ? C9 S5A S5B C10 -102.7(17) . . . . ? O5 S5A S5B C9 -125.1(18) . . . . ? C10 S5A S5B C9 102.7(17) . . . . ? Pr1 O5 S5B S5A 141(4) . . . . ? S5A O5 S5B C10 -49.8(17) . . . . ? Pr1 O5 S5B C10 91(4) . . . . ? S5A O5 S5B C9 52.4(15) . . . . ? Pr1 O5 S5B C9 -167(3) . . . . ? Pr1 O6 S6A S6B 148(4) . . . . ? S6B O6 S6A C11 56(3) . . . . ? Pr1 O6 S6A C11 -156(3) . . . . ? S6B O6 S6A C12 -58(3) . . . . ? Pr1 O6 S6A C12 90(4) . . . . ? C11 S6A S6B O6 -127(3) . . . . ? C12 S6A S6B O6 124(3) . . . . ? O6 S6A S6B C12 -124(3) . . . . ? C11 S6A S6B C12 110(3) . . . . ? O6 S6A S6B C11 127(3) . . . . ? C12 S6A S6B C11 -110(3) . . . . ? Pr1 O6 S6B S6A -133(5) . . . . ? S6A O6 S6B C12 57(2) . . . . ? Pr1 O6 S6B C12 -76(6) . . . . ? S6A O6 S6B C11 -54(3) . . . . ? Pr1 O6 S6B C11 173(5) . . . . ? Pr1 O7 S7 C13 -111(3) . . . . ? Pr1 O7 S7 C14 132(3) . . . . ? Pr1 O8 S8A S8B 176(3) . . . . ? S8B O8 S8A C15 -65(4) . . . . ? Pr1 O8 S8A C15 111(4) . . . . ? S8B O8 S8A C16 56(3) . . . . ? Pr1 O8 S8A C16 -128(2) . . . . ? C15 S8A S8B O8 126(3) . . . . ? C16 S8A S8B O8 -122(2) . . . . ? O8 S8A S8B C16 122(2) . . . . ? C15 S8A S8B C16 -112(3) . . . . ? O8 S8A S8B C15 -126(3) . . . . ? C16 S8A S8B C15 112(3) . . . . ? Pr1 O8 S8B S8A -39(29) . . . . ? S8A O8 S8B C16 -63(2) . . . . ? Pr1 O8 S8B C16 -102(29) . . . . ? S8A O8 S8B C15 47(3) . . . . ? Pr1 O8 S8B C15 8(30) . . . . ? Pb3 O9 S9A S9B -138(3) . . . . ? Pb4 O9 S9A S9B 20(5) . . . . ? S9B O9 S9A C18B 92(6) . . . . ? Pb3 O9 S9A C18B -47(6) . . . . ? Pb4 O9 S9A C18B 111(6) . . . . ? S9B O9 S9A C18A 50(3) . . . . ? Pb3 O9 S9A C18A -88(3) . . . . ? Pb4 O9 S9A C18A 70(4) . . . . ? S9B O9 S9A C17 -67(2) . . . . ? Pb3 O9 S9A C17 155(3) . . . . ? Pb4 O9 S9A C17 -47(5) . . . . ? C18B S9A S9B C18A -15(4) . . . . ? O9 S9A S9B C18A 117(4) . . . . ? C17 S9A S9B C18A -129(4) . . . . ? C18B S9A S9B O9 -133(3) . . . . ? C18A S9A S9B O9 -117(4) . . . . ? C17 S9A S9B O9 114(3) . . . . ? C18B S9A S9B C17 114(2) . . . . ? C18A S9A S9B C17 129(4) . . . . ? O9 S9A S9B C17 -114(3) . . . . ? C18A S9A S9B C18B 15(4) . . . . ? O9 S9A S9B C18B 133(3) . . . . ? C17 S9A S9B C18B -114(2) . . . . ? Pb3 O9 S9B S9A 64(4) . . . . ? Pb4 O9 S9B S9A -169(3) . . . . ? S9A O9 S9B C18A -68(3) . . . . ? Pb3 O9 S9B C18A -3(4) . . . . ? Pb4 O9 S9B C18A 123(3) . . . . ? S9A O9 S9B C17 66(2) . . . . ? Pb3 O9 S9B C17 130(4) . . . . ? Pb4 O9 S9B C17 -103(3) . . . . ? S9A O9 S9B C18B -32(2) . . . . ? Pb3 O9 S9B C18B 32(4) . . . . ? Pb4 O9 S9B C18B 158(3) . . . . ? O4 S4B C7 S4A 61(2) . . . . ? C8 S4B C7 S4A -68(2) . . . . ? O4 S4A C7 S4B -69(3) . . . . ? C8 S4A C7 S4B 69(2) . . . . ? O4 S4A C8 S4B 63(3) . . . . ? C7 S4A C8 S4B -65(3) . . . . ? O4 S4B C8 S4A -50(3) . . . . ? C7 S4B C8 S4A 71(3) . . . . ? O5 S5A C9 S5B 56.4(18) . . . . ? C10 S5A C9 S5B -63.3(12) . . . . ? O5 S5B C9 S5A -45.7(17) . . . . ? C10 S5B C9 S5A 69.1(12) . . . . ? O5 S5B C10 S5A 42.5(16) . . . . ? C9 S5B C10 S5A -66.1(12) . . . . ? O5 S5A C10 S5B -50.6(19) . . . . ? C9 S5A C10 S5B 66.5(12) . . . . ? O6 S6A C11 S6B -51(3) . . . . ? C12 S6A C11 S6B 67(2) . . . . ? O6 S6B C11 S6A 54(2) . . . . ? C12 S6B C11 S6A -64(3) . . . . ? O6 S6A C12 S6B 52(2) . . . . ? C11 S6A C12 S6B -68(2) . . . . ? O6 S6B C12 S6A -57(2) . . . . ? C11 S6B C12 S6A 63(3) . . . . ? O8 S8A C15 S8B 55(3) . . . . ? C16 S8A C15 S8B -66(2) . . . . ? O8 S8B C15 S8A -55(3) . . . . ? C16 S8B C15 S8A 65(3) . . . . ? O8 S8B C16 S8A 62(2) . . . . ? C15 S8B C16 S8A -54(3) . . . . ? O8 S8A C16 S8B -52(3) . . . . ? C15 S8A C16 S8B 75(3) . . . . ? C18A S9B C17 S9A 65(5) . . . . ? O9 S9B C17 S9A -61(2) . . . . ? C18B S9B C17 S9A 41(3) . . . . ? C18B S9A C17 S9B -94(4) . . . . ? C18A S9A C17 S9B -44(4) . . . . ? O9 S9A C17 S9B 69(3) . . . . ? O9 S9B C18A S9A 60(2) . . . . ? C17 S9B C18A S9A -63(4) . . . . ? C18B S9B C18A S9A -19(5) . . . . ? C18B S9A C18A S9B 159(5) . . . . ? O9 S9A C18A S9B -63(4) . . . . ? C17 S9A C18A S9B 53(3) . . . . ? C18A S9A C18B S9B -18(4) . . . . ? O9 S9A C18B S9B -81(5) . . . . ? C17 S9A C18B S9B 76(3) . . . . ? C18A S9B C18B S9A 153(7) . . . . ? O9 S9B C18B S9A 43(3) . . . . ? C17 S9B C18B S9A -62(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.618 _refine_diff_density_min -1.670 _refine_diff_density_rms 0.253 _database_code_depnum_ccdc_archive 'CCDC 958528' data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H54 I11 Nd O9 Pb4 S9' _chemical_formula_sum 'C18 H54 I11 Nd O9 Pb4 S9' _chemical_formula_weight 3072.05 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' I I -0.4742 1.8119 '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' Nd Nd -0.1943 3.0179 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.6984(19) _cell_length_b 15.5382(12) _cell_length_c 24.498(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.218(2) _cell_angle_gamma 90.00 _cell_volume 6760.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17806 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5396 _exptl_absorpt_coefficient_mu 16.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0687 _exptl_absorpt_correction_T_max 0.1974 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40499 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12340 _reflns_number_gt 10193 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0409P)^2^+113.4895P] 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 SHELXL _refine_ls_extinction_coef 0.000132(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12340 _refine_ls_number_parameters 385 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.112 _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 Pb1 Pb 0.62223(4) 0.79683(5) 0.34685(3) 0.04190(19) Uani 1 1 d . . . Pb2 Pb 0.76975(4) 0.78046(5) 0.50683(3) 0.04006(19) Uani 1 1 d . . . Pb3 Pb 0.90803(4) 0.78529(5) 0.67050(3) 0.04541(19) Uani 1 1 d . . . Pb4 Pb 0.76292(4) 0.74238(5) 0.25720(3) 0.04597(19) Uani 1 1 d . . . I1 I 0.63009(8) 0.65867(8) 0.44512(5) 0.0518(3) Uani 1 1 d . . . I2 I 0.66478(7) 0.93647(8) 0.44613(5) 0.0470(3) Uani 1 1 d . . . I3 I 0.45786(8) 0.83370(12) 0.31395(6) 0.0708(5) Uani 1 1 d . . . I4 I 0.67078(9) 0.92054(9) 0.25420(6) 0.0553(4) Uani 1 1 d . . . I5 I 0.62578(8) 0.63647(9) 0.25759(6) 0.0554(3) Uani 1 1 d . . . I6 I 0.88604(8) 0.92937(9) 0.57989(6) 0.0529(3) Uani 1 1 d . . . I7 I 0.90100(8) 0.64557(9) 0.57221(6) 0.0532(4) Uani 1 1 d . . . I8 I 0.82673(7) 0.76697(9) 0.39648(5) 0.0497(3) Uani 1 1 d . . . I9 I 1.07713(7) 0.79444(11) 0.71327(7) 0.0684(4) Uani 1 1 d . . . I10 I 0.71216(7) 0.74156(8) 0.11886(5) 0.0438(3) Uani 1 1 d . . . I11 I 0.86806(8) 0.58200(9) 0.26246(6) 0.0561(4) Uani 1 1 d . . . Nd1 Nd 0.71893(5) 0.25668(6) 0.48338(4) 0.0456(2) Uani 1 1 d . . . O1 O 0.5971(6) 0.1838(8) 0.4521(5) 0.045(3) Uani 1 1 d . . . O2 O 0.6370(7) 0.3587(9) 0.4178(6) 0.0610(19) Uani 1 1 d . . . O3 O 0.6604(10) 0.3443(11) 0.5395(7) 0.0557(17) Uani 1 1 d . . . O4 O 0.7992(8) 0.3585(10) 0.4547(6) 0.0643(15) Uani 1 1 d . . . O5 O 0.8190(8) 0.3053(11) 0.5689(7) 0.0641(17) Uani 1 1 d . . . O6 O 0.8255(9) 0.1652(11) 0.4899(7) 0.0668(17) Uani 1 1 d . . . O7 O 0.7085(8) 0.2006(9) 0.3892(5) 0.054(3) Uani 1 1 d . . . O8 O 0.7128(7) 0.1603(9) 0.5584(6) 0.054(3) Uani 1 1 d . . . S1 S 0.5577(2) 0.1225(3) 0.4818(2) 0.0481(10) Uani 1 1 d . . . S2A S 0.5601(7) 0.3543(8) 0.3735(5) 0.0610(19) Uani 0.50 1 d PD . . S2B S 0.5592(7) 0.3932(8) 0.3966(5) 0.0610(19) Uani 0.50 1 d PD . . S3 S 0.6840(4) 0.3920(5) 0.5959(3) 0.0817(17) Uani 1 1 d . . . S4 S 0.7917(3) 0.4010(4) 0.3975(3) 0.0713(15) Uani 1 1 d D . . S5 S 0.9035(3) 0.3052(5) 0.5735(3) 0.0791(17) Uani 1 1 d D . . S6 S 0.8676(4) 0.1558(5) 0.4458(3) 0.0738(17) Uani 1 1 d . . . S7 S 0.6609(4) 0.2169(4) 0.3298(3) 0.0700(16) Uani 1 1 d . . . S8 S 0.7640(2) 0.1142(3) 0.6097(2) 0.0446(11) Uani 1 1 d . . . C1 C 0.5061(13) 0.1876(15) 0.5150(9) 0.068(7) Uani 1 1 d . . . H1A H 0.5405 0.2239 0.5436 0.102 Uiso 1 1 calc R . . H1B H 0.4781 0.1514 0.5334 0.102 Uiso 1 1 calc R . . H1C H 0.4714 0.2235 0.4863 0.102 Uiso 1 1 calc R . . C2 C 0.4791(11) 0.0799(15) 0.4281(10) 0.066(6) Uani 1 1 d . . . H2A H 0.4517 0.1263 0.4040 0.099 Uiso 1 1 calc R . . H2B H 0.4463 0.0509 0.4460 0.099 Uiso 1 1 calc R . . H2C H 0.4961 0.0392 0.4048 0.099 Uiso 1 1 calc R . . C3 C 0.5541(11) 0.4530(12) 0.3347(8) 0.0610(19) Uani 1 1 d D . . C4A C 0.503(2) 0.393(3) 0.4145(16) 0.0610(19) Uani 0.50 1 d PD . . C4B C 0.4848(18) 0.324(2) 0.3612(17) 0.0610(19) Uani 0.50 1 d PD . . C5 C 0.7021(15) 0.4982(16) 0.5785(11) 0.0817(17) Uani 1 1 d . . . H5A H 0.7449 0.4984 0.5642 0.123 Uiso 1 1 calc R . . H5B H 0.7130 0.5340 0.6126 0.123 Uiso 1 1 calc R . . H5C H 0.6582 0.5206 0.5492 0.123 Uiso 1 1 calc R . . C6 C 0.6021(14) 0.4024(17) 0.6157(11) 0.0817(17) Uani 1 1 d . . . H6A H 0.5632 0.4302 0.5850 0.123 Uiso 1 1 calc R . . H6B H 0.6128 0.4370 0.6504 0.123 Uiso 1 1 calc R . . H6C H 0.5849 0.3459 0.6229 0.123 Uiso 1 1 calc R . . C7 C 0.8854(12) 0.4041(16) 0.3943(10) 0.0713(15) Uani 1 1 d . . . H7A H 0.9171 0.4361 0.4269 0.107 Uiso 1 1 calc R . . H7B H 0.8858 0.4319 0.3589 0.107 Uiso 1 1 calc R . . H7C H 0.9045 0.3458 0.3953 0.107 Uiso 1 1 calc R . . C8 C 0.7817(13) 0.5100(10) 0.4066(10) 0.0713(15) Uani 1 1 d D . . H8A H 0.7334 0.5209 0.4122 0.107 Uiso 1 1 calc R . . H8B H 0.7845 0.5406 0.3728 0.107 Uiso 1 1 calc R . . H8C H 0.8218 0.5297 0.4401 0.107 Uiso 1 1 calc R . . C9 C 0.9397(12) 0.3936(11) 0.6155(9) 0.0791(17) Uani 1 1 d D . . H9A H 0.9188 0.3966 0.6470 0.119 Uiso 1 1 calc R . . H9B H 0.9265 0.4454 0.5924 0.119 Uiso 1 1 calc R . . H9C H 0.9940 0.3887 0.6306 0.119 Uiso 1 1 calc R . . C10 C 0.9501(13) 0.2350(13) 0.6271(10) 0.0791(17) Uani 1 1 d D . . H10A H 0.9400 0.2501 0.6624 0.119 Uiso 1 1 calc R . . H10B H 1.0038 0.2384 0.6331 0.119 Uiso 1 1 calc R . . H10C H 0.9328 0.1768 0.6160 0.119 Uiso 1 1 calc R . . C11 C 0.9603(12) 0.1420(17) 0.4861(11) 0.0788(17) Uani 1 1 d . . . H11A H 0.9630 0.1091 0.5203 0.118 Uiso 1 1 calc R . . H11B H 0.9836 0.1978 0.4971 0.118 Uiso 1 1 calc R . . H11C H 0.9866 0.1113 0.4636 0.118 Uiso 1 1 calc R . . C12 C 0.8571(14) 0.0493(16) 0.4247(11) 0.0788(17) Uani 1 1 d . . . H12A H 0.8644 0.0128 0.4581 0.118 Uiso 1 1 calc R . . H12B H 0.8940 0.0348 0.4058 0.118 Uiso 1 1 calc R . . H12C H 0.8069 0.0404 0.3982 0.118 Uiso 1 1 calc R . . C13 C 0.7127(13) 0.1829(16) 0.2841(8) 0.066(6) Uani 1 1 d . . . H13A H 0.7593 0.2152 0.2930 0.099 Uiso 1 1 calc R . . H13B H 0.6831 0.1929 0.2443 0.099 Uiso 1 1 calc R . . H13C H 0.7239 0.1220 0.2899 0.099 Uiso 1 1 calc R . . C14 C 0.5907(10) 0.1321(14) 0.3129(9) 0.056(5) Uani 1 1 d . . . H14A H 0.6147 0.0774 0.3263 0.084 Uiso 1 1 calc R . . H14B H 0.5667 0.1296 0.2716 0.084 Uiso 1 1 calc R . . H14C H 0.5531 0.1440 0.3316 0.084 Uiso 1 1 calc R . . C15 C 0.7127(12) 0.0228(12) 0.6194(8) 0.055(5) Uani 1 1 d . . . H15A H 0.6677 0.0413 0.6277 0.082 Uiso 1 1 calc R . . H15B H 0.7437 -0.0113 0.6511 0.082 Uiso 1 1 calc R . . H15C H 0.6986 -0.0115 0.5846 0.082 Uiso 1 1 calc R . . C16 C 0.7587(12) 0.1751(14) 0.6704(8) 0.059(6) Uani 1 1 d . . . H16A H 0.7812 0.2313 0.6701 0.089 Uiso 1 1 calc R . . H16B H 0.7856 0.1450 0.7055 0.089 Uiso 1 1 calc R . . H16C H 0.7063 0.1819 0.6684 0.089 Uiso 1 1 calc R . . O9 O 0.8880(12) 0.8234(12) 0.2498(11) 0.060(3) Uani 1 1 d . . . S9 S 0.8956(5) 0.9216(5) 0.2580(5) 0.059(3) Uani 1 1 d D . . C17 C 0.9830(10) 0.9429(17) 0.2513(14) 0.063(3) Uani 1 1 d D . . H17A H 1.0217 0.9297 0.2872 0.094 Uiso 1 1 calc R . . H17B H 0.9860 1.0032 0.2421 0.094 Uiso 1 1 calc R . . H17C H 0.9904 0.9077 0.2208 0.094 Uiso 1 1 calc R . . C18 C 0.8432(13) 0.9806(17) 0.2031(15) 0.066(3) Uani 1 1 d D . . H18A H 0.8373 0.9504 0.1673 0.099 Uiso 1 1 calc R . . H18B H 0.8677 1.0355 0.2025 0.099 Uiso 1 1 calc R . . H18C H 0.7940 0.9903 0.2075 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0442(4) 0.0501(5) 0.0318(4) -0.0007(3) 0.0125(3) 0.0017(3) Pb2 0.0458(4) 0.0443(4) 0.0287(3) -0.0006(3) 0.0097(3) 0.0034(3) Pb3 0.0477(4) 0.0449(4) 0.0346(4) -0.0001(3) 0.0097(3) 0.0012(3) Pb4 0.0449(4) 0.0432(4) 0.0436(4) -0.0017(3) 0.0147(3) 0.0005(3) I1 0.0685(8) 0.0419(8) 0.0452(7) -0.0032(5) 0.0180(6) -0.0053(6) I2 0.0525(7) 0.0388(7) 0.0470(7) -0.0023(5) 0.0118(6) 0.0051(6) I3 0.0446(8) 0.1121(14) 0.0530(8) -0.0012(8) 0.0116(7) 0.0069(8) I4 0.0596(10) 0.0474(8) 0.0583(8) 0.0103(6) 0.0277(8) 0.0155(7) I5 0.0580(8) 0.0603(9) 0.0502(7) -0.0069(6) 0.0204(6) -0.0141(7) I6 0.0602(8) 0.0472(8) 0.0518(8) 0.0050(6) 0.0182(7) 0.0025(6) I7 0.0556(8) 0.0490(8) 0.0552(8) -0.0020(6) 0.0161(7) 0.0164(7) I8 0.0485(7) 0.0722(9) 0.0299(6) -0.0011(6) 0.0144(5) 0.0012(6) I9 0.0375(7) 0.0875(12) 0.0753(10) 0.0040(8) 0.0105(7) 0.0037(7) I10 0.0437(6) 0.0601(8) 0.0289(6) 0.0015(5) 0.0132(5) 0.0032(6) I11 0.0692(9) 0.0474(8) 0.0503(8) 0.0096(6) 0.0167(7) 0.0114(7) Nd1 0.0448(5) 0.0463(5) 0.0448(5) 0.0022(4) 0.0140(4) -0.0002(4) O1 0.044(7) 0.053(8) 0.043(7) 0.009(6) 0.024(6) -0.005(6) O2 0.056(3) 0.054(5) 0.065(5) 0.017(3) 0.006(4) 0.001(4) O3 0.045(4) 0.073(4) 0.060(4) -0.021(3) 0.032(3) -0.005(3) O4 0.070(3) 0.052(4) 0.070(3) 0.018(3) 0.020(3) -0.015(3) O5 0.055(3) 0.056(5) 0.074(4) 0.021(3) 0.002(3) -0.009(3) O6 0.076(3) 0.080(4) 0.048(4) 0.013(3) 0.023(3) 0.015(3) O7 0.062(8) 0.059(9) 0.042(7) -0.001(6) 0.018(7) -0.002(7) O8 0.048(7) 0.062(9) 0.054(8) 0.017(7) 0.018(7) -0.004(7) S1 0.055(2) 0.042(3) 0.046(3) 0.001(2) 0.013(2) -0.003(2) S2A 0.056(3) 0.054(5) 0.065(5) 0.017(3) 0.006(4) 0.001(4) S2B 0.056(3) 0.054(5) 0.065(5) 0.017(3) 0.006(4) 0.001(4) S3 0.095(4) 0.073(4) 0.080(4) -0.021(3) 0.032(3) -0.005(3) S4 0.070(3) 0.072(4) 0.070(3) 0.018(3) 0.020(3) -0.015(3) S5 0.055(3) 0.096(5) 0.074(4) 0.021(3) 0.002(3) -0.009(3) S6 0.076(3) 0.080(4) 0.058(4) 0.013(3) 0.013(3) 0.005(3) S7 0.070(4) 0.083(5) 0.058(4) -0.004(3) 0.022(3) -0.001(3) S8 0.038(2) 0.043(3) 0.050(3) 0.006(2) 0.009(2) 0.003(2) C1 0.085(16) 0.074(16) 0.065(14) -0.023(12) 0.056(13) -0.008(13) C2 0.044(11) 0.064(15) 0.086(16) -0.016(12) 0.016(11) -0.013(11) C3 0.056(3) 0.054(5) 0.065(5) 0.017(3) 0.006(4) 0.001(4) C4A 0.056(3) 0.054(5) 0.065(5) 0.017(3) 0.006(4) 0.001(4) C4B 0.056(3) 0.054(5) 0.065(5) 0.017(3) 0.006(4) 0.001(4) C5 0.095(4) 0.073(4) 0.080(4) -0.021(3) 0.032(3) -0.005(3) C6 0.095(4) 0.073(4) 0.080(4) -0.021(3) 0.032(3) -0.005(3) C7 0.070(3) 0.072(4) 0.070(3) 0.018(3) 0.020(3) -0.015(3) C8 0.070(3) 0.072(4) 0.070(3) 0.018(3) 0.020(3) -0.015(3) C9 0.055(3) 0.096(5) 0.074(4) 0.021(3) 0.002(3) -0.009(3) C10 0.055(3) 0.096(5) 0.074(4) 0.021(3) 0.002(3) -0.009(3) C11 0.076(3) 0.080(4) 0.098(4) 0.013(3) 0.053(3) 0.015(3) C12 0.076(3) 0.080(4) 0.098(4) 0.013(3) 0.053(3) 0.015(3) C13 0.077(15) 0.085(17) 0.039(11) -0.001(11) 0.023(11) -0.001(13) C14 0.035(10) 0.072(15) 0.057(12) -0.002(11) 0.007(9) 0.000(10) C15 0.070(13) 0.043(12) 0.052(12) -0.002(9) 0.020(11) -0.010(10) C16 0.065(13) 0.068(15) 0.045(11) -0.004(10) 0.017(11) -0.017(11) O9 0.072(6) 0.047(4) 0.060(8) -0.001(4) 0.019(6) -0.018(4) S9 0.065(6) 0.049(4) 0.066(8) -0.001(4) 0.021(6) -0.018(4) C17 0.069(6) 0.057(4) 0.058(8) -0.001(4) 0.009(6) -0.018(4) C18 0.057(6) 0.061(4) 0.069(8) -0.001(4) 0.011(6) -0.018(4) _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 Pb1 I3 2.9792(16) . ? Pb1 I2 3.1696(14) . ? Pb1 I1 3.1945(15) . ? Pb1 I4 3.3103(15) . ? Pb1 I5 3.3294(15) . ? Pb2 I2 3.1804(14) . ? Pb2 I1 3.1964(15) . ? Pb2 I8 3.2074(13) . ? Pb2 I7 3.2441(15) . ? Pb2 I10 3.2644(13) 4_576 ? Pb2 I6 3.2943(16) . ? Pb3 O9 2.69(2) 4_576 ? Pb3 I9 3.0073(15) . ? Pb3 I6 3.0883(15) . ? Pb3 I7 3.2141(15) . ? Pb3 I11 3.3076(15) 4_576 ? Pb4 O9 2.712(19) . ? Pb4 I5 3.0494(15) . ? Pb4 I11 3.1518(15) . ? Pb4 I10 3.2211(13) . ? Pb4 I4 3.2492(15) . ? Pb4 I8 3.2659(13) . ? I10 Pb2 3.2644(13) 4_575 ? I11 Pb3 3.3076(15) 4_575 ? Nd1 O8 2.401(12) . ? Nd1 O6 2.412(15) . ? Nd1 O7 2.415(12) . ? Nd1 O3 2.426(15) . ? Nd1 O2 2.429(13) . ? Nd1 O4 2.431(14) . ? Nd1 O1 2.443(12) . ? Nd1 O5 2.451(16) . ? O1 S1 1.522(12) . ? O2 S2B 1.484(18) . ? O2 S2A 1.507(18) . ? O3 S3 1.508(16) . ? O4 S4 1.516(15) . ? O5 S5 1.549(16) . ? O6 S6 1.529(15) . ? O7 S7 1.472(14) . ? O8 S8 1.502(13) . ? S1 C1 1.761(19) . ? S1 C2 1.77(2) . ? S2A C4A 1.782(19) . ? S2A C3 1.790(15) . ? S2B C4B 1.752(19) . ? S2B C3 1.755(15) . ? S3 C6 1.75(2) . ? S3 C5 1.76(3) . ? S4 C8 1.725(16) . ? S4 C7 1.78(2) . ? S5 C10 1.72(2) . ? S5 C9 1.722(15) . ? S6 C11 1.72(2) . ? S6 C12 1.73(3) . ? S7 C13 1.78(2) . ? S7 C14 1.81(2) . ? S8 C15 1.770(19) . ? S8 C16 1.79(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? O9 S9 1.539(19) . ? O9 Pb3 2.69(2) 4_575 ? S9 C18 1.67(3) . ? S9 C17 1.724(16) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? 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 I3 Pb1 I2 93.79(4) . . ? I3 Pb1 I1 97.68(4) . . ? I2 Pb1 I1 86.58(4) . . ? I3 Pb1 I4 100.58(5) . . ? I2 Pb1 I4 94.12(4) . . ? I1 Pb1 I4 161.63(4) . . ? I3 Pb1 I5 101.36(4) . . ? I2 Pb1 I5 164.69(4) . . ? I1 Pb1 I5 89.22(4) . . ? I4 Pb1 I5 85.31(4) . . ? I2 Pb2 I1 86.36(4) . . ? I2 Pb2 I8 88.56(4) . . ? I1 Pb2 I8 90.01(4) . . ? I2 Pb2 I7 169.85(4) . . ? I1 Pb2 I7 103.36(4) . . ? I8 Pb2 I7 88.54(4) . . ? I2 Pb2 I10 98.94(4) . 4_576 ? I1 Pb2 I10 84.27(4) . 4_576 ? I8 Pb2 I10 170.24(4) . 4_576 ? I7 Pb2 I10 85.11(4) . 4_576 ? I2 Pb2 I6 85.68(4) . . ? I1 Pb2 I6 167.34(4) . . ? I8 Pb2 I6 99.61(4) . . ? I7 Pb2 I6 85.21(4) . . ? I10 Pb2 I6 87.25(4) 4_576 . ? O9 Pb3 I9 98.4(5) 4_576 . ? O9 Pb3 I6 163.3(4) 4_576 . ? I9 Pb3 I6 96.05(4) . . ? O9 Pb3 I7 97.8(4) 4_576 . ? I9 Pb3 I7 94.89(4) . . ? I6 Pb3 I7 89.21(4) . . ? O9 Pb3 I11 77.7(4) 4_576 4_576 ? I9 Pb3 I11 99.79(4) . 4_576 ? I6 Pb3 I11 91.71(4) . 4_576 ? I7 Pb3 I11 165.11(4) . 4_576 ? O9 Pb4 I5 174.0(5) . . ? O9 Pb4 I11 80.2(4) . . ? I5 Pb4 I11 95.02(4) . . ? O9 Pb4 I10 84.7(5) . . ? I5 Pb4 I10 91.70(4) . . ? I11 Pb4 I10 90.84(4) . . ? O9 Pb4 I4 93.7(4) . . ? I5 Pb4 I4 91.11(4) . . ? I11 Pb4 I4 173.78(5) . . ? I10 Pb4 I4 89.99(4) . . ? O9 Pb4 I8 88.5(5) . . ? I5 Pb4 I8 95.33(4) . . ? I11 Pb4 I8 91.74(4) . . ? I10 Pb4 I8 172.27(4) . . ? I4 Pb4 I8 86.67(4) . . ? Pb1 I1 Pb2 78.28(3) . . ? Pb1 I2 Pb2 78.88(3) . . ? Pb4 I4 Pb1 75.34(3) . . ? Pb4 I5 Pb1 77.74(4) . . ? Pb3 I6 Pb2 78.36(4) . . ? Pb3 I7 Pb2 77.34(3) . . ? Pb2 I8 Pb4 141.17(5) . . ? Pb4 I10 Pb2 144.97(4) . 4_575 ? Pb4 I11 Pb3 75.53(3) . 4_575 ? O8 Nd1 O6 79.5(5) . . ? O8 Nd1 O7 119.8(5) . . ? O6 Nd1 O7 70.7(5) . . ? O8 Nd1 O3 77.2(5) . . ? O6 Nd1 O3 143.5(6) . . ? O7 Nd1 O3 145.8(5) . . ? O8 Nd1 O2 137.9(4) . . ? O6 Nd1 O2 139.9(5) . . ? O7 Nd1 O2 76.0(5) . . ? O3 Nd1 O2 72.9(6) . . ? O8 Nd1 O4 144.0(5) . . ? O6 Nd1 O4 80.3(5) . . ? O7 Nd1 O4 80.3(5) . . ? O3 Nd1 O4 103.1(6) . . ? O2 Nd1 O4 72.7(5) . . ? O8 Nd1 O1 71.8(4) . . ? O6 Nd1 O1 114.7(5) . . ? O7 Nd1 O1 75.2(4) . . ? O3 Nd1 O1 84.0(5) . . ? O2 Nd1 O1 76.2(4) . . ? O4 Nd1 O1 144.2(4) . . ? O8 Nd1 O5 75.2(5) . . ? O6 Nd1 O5 74.4(6) . . ? O7 Nd1 O5 137.7(5) . . ? O3 Nd1 O5 72.7(6) . . ? O2 Nd1 O5 121.3(5) . . ? O4 Nd1 O5 70.8(5) . . ? O1 Nd1 O5 143.0(4) . . ? S1 O1 Nd1 133.2(7) . . ? S2B O2 S2A 32.2(6) . . ? S2B O2 Nd1 144.5(9) . . ? S2A O2 Nd1 135.1(9) . . ? S3 O3 Nd1 137.8(10) . . ? S4 O4 Nd1 131.6(9) . . ? S5 O5 Nd1 123.5(10) . . ? S6 O6 Nd1 127.4(9) . . ? S7 O7 Nd1 136.6(8) . . ? S8 O8 Nd1 140.1(7) . . ? O1 S1 C1 106.2(9) . . ? O1 S1 C2 107.0(9) . . ? C1 S1 C2 96.4(11) . . ? O2 S2A C4A 100.6(16) . . ? O2 S2A C3 103.4(11) . . ? C4A S2A C3 93.6(16) . . ? O2 S2B C4B 119.5(17) . . ? O2 S2B C3 106.1(11) . . ? C4B S2B C3 94.3(16) . . ? O3 S3 C6 105.5(11) . . ? O3 S3 C5 105.2(11) . . ? C6 S3 C5 103.3(12) . . ? O4 S4 C8 106.9(11) . . ? O4 S4 C7 104.2(10) . . ? C8 S4 C7 97.3(11) . . ? O5 S5 C10 108.6(10) . . ? O5 S5 C9 104.1(11) . . ? C10 S5 C9 92.3(9) . . ? O6 S6 C11 104.8(11) . . ? O6 S6 C12 105.5(10) . . ? C11 S6 C12 93.0(13) . . ? O7 S7 C13 107.1(9) . . ? O7 S7 C14 105.8(9) . . ? C13 S7 C14 98.0(11) . . ? O8 S8 C15 105.3(9) . . ? O8 S8 C16 104.9(9) . . ? C15 S8 C16 98.0(9) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? S2B C3 S2A 27.1(5) . . ? S3 C5 H5A 109.5 . . ? S3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S3 C6 H6A 109.5 . . ? S3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S4 C7 H7A 109.5 . . ? S4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S4 C8 H8A 109.5 . . ? S4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? S5 C9 H9A 109.5 . . ? S5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? S5 C10 H10A 109.5 . . ? S5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? S6 C11 H11A 109.5 . . ? S6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S6 C12 H12A 109.5 . . ? S6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? S7 C13 H13A 109.5 . . ? S7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? S7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? S7 C14 H14A 109.5 . . ? S7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? S7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? S8 C15 H15A 109.5 . . ? S8 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S8 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? S8 C16 H16A 109.5 . . ? S8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S9 O9 Pb3 133.5(13) . 4_575 ? S9 O9 Pb4 119.8(12) . . ? Pb3 O9 Pb4 94.3(6) 4_575 . ? O9 S9 C18 115.6(15) . . ? O9 S9 C17 103.2(13) . . ? C18 S9 C17 98.8(12) . . ? S9 C17 H17A 109.5 . . ? S9 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S9 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S9 C18 H18A 109.5 . . ? S9 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S9 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? 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 I3 Pb1 I1 Pb2 -133.05(4) . . . . ? I2 Pb1 I1 Pb2 -39.68(3) . . . . ? I4 Pb1 I1 Pb2 53.09(14) . . . . ? I5 Pb1 I1 Pb2 125.59(4) . . . . ? I2 Pb2 I1 Pb1 39.53(3) . . . . ? I8 Pb2 I1 Pb1 -49.02(4) . . . . ? I7 Pb2 I1 Pb1 -137.53(4) . . . . ? I10 Pb2 I1 Pb1 138.90(4) 4_576 . . . ? I6 Pb2 I1 Pb1 90.71(18) . . . . ? I3 Pb1 I2 Pb2 137.30(4) . . . . ? I1 Pb1 I2 Pb2 39.82(3) . . . . ? I4 Pb1 I2 Pb2 -121.79(4) . . . . ? I5 Pb1 I2 Pb2 -34.51(16) . . . . ? I1 Pb2 I2 Pb1 -39.80(3) . . . . ? I8 Pb2 I2 Pb1 50.31(3) . . . . ? I7 Pb2 I2 Pb1 123.7(2) . . . . ? I10 Pb2 I2 Pb1 -123.41(3) 4_576 . . . ? I6 Pb2 I2 Pb1 150.06(4) . . . . ? O9 Pb4 I4 Pb1 -141.8(5) . . . . ? I5 Pb4 I4 Pb1 41.75(4) . . . . ? I11 Pb4 I4 Pb1 -128.8(4) . . . . ? I10 Pb4 I4 Pb1 133.45(4) . . . . ? I8 Pb4 I4 Pb1 -53.52(3) . . . . ? I3 Pb1 I4 Pb4 -138.42(4) . . . . ? I2 Pb1 I4 Pb4 126.94(4) . . . . ? I1 Pb1 I4 Pb4 35.39(14) . . . . ? I5 Pb1 I4 Pb4 -37.72(3) . . . . ? O9 Pb4 I5 Pb1 175(5) . . . . ? I11 Pb4 I5 Pb1 138.03(4) . . . . ? I10 Pb4 I5 Pb1 -130.97(4) . . . . ? I4 Pb4 I5 Pb1 -40.95(4) . . . . ? I8 Pb4 I5 Pb1 45.81(4) . . . . ? I3 Pb1 I5 Pb4 140.07(4) . . . . ? I2 Pb1 I5 Pb4 -48.27(16) . . . . ? I1 Pb1 I5 Pb4 -122.26(4) . . . . ? I4 Pb1 I5 Pb4 40.19(4) . . . . ? O9 Pb3 I6 Pb2 -75.0(17) 4_576 . . . ? I9 Pb3 I6 Pb2 134.89(4) . . . . ? I7 Pb3 I6 Pb2 40.05(3) . . . . ? I11 Pb3 I6 Pb2 -125.08(4) 4_576 . . . ? I2 Pb2 I6 Pb3 144.74(4) . . . . ? I1 Pb2 I6 Pb3 93.50(18) . . . . ? I8 Pb2 I6 Pb3 -127.47(4) . . . . ? I7 Pb2 I6 Pb3 -39.77(3) . . . . ? I10 Pb2 I6 Pb3 45.55(3) 4_576 . . . ? O9 Pb3 I7 Pb2 123.8(5) 4_576 . . . ? I9 Pb3 I7 Pb2 -136.99(4) . . . . ? I6 Pb3 I7 Pb2 -40.99(4) . . . . ? I11 Pb3 I7 Pb2 52.70(17) 4_576 . . . ? I2 Pb2 I7 Pb3 64.5(2) . . . . ? I1 Pb2 I7 Pb3 -132.46(4) . . . . ? I8 Pb2 I7 Pb3 137.87(4) . . . . ? I10 Pb2 I7 Pb3 -49.55(3) 4_576 . . . ? I6 Pb2 I7 Pb3 38.10(3) . . . . ? I2 Pb2 I8 Pb4 -56.04(8) . . . . ? I1 Pb2 I8 Pb4 30.32(8) . . . . ? I7 Pb2 I8 Pb4 133.69(8) . . . . ? I10 Pb2 I8 Pb4 84.4(2) 4_576 . . . ? I6 Pb2 I8 Pb4 -141.41(8) . . . . ? O9 Pb4 I8 Pb2 154.7(4) . . . . ? I5 Pb4 I8 Pb2 -29.95(9) . . . . ? I11 Pb4 I8 Pb2 -125.16(8) . . . . ? I10 Pb4 I8 Pb2 125.4(3) . . . . ? I4 Pb4 I8 Pb2 60.86(8) . . . . ? O9 Pb4 I10 Pb2 38.0(4) . . . 4_575 ? I5 Pb4 I10 Pb2 -137.12(8) . . . 4_575 ? I11 Pb4 I10 Pb2 -42.07(9) . . . 4_575 ? I4 Pb4 I10 Pb2 131.77(8) . . . 4_575 ? I8 Pb4 I10 Pb2 67.4(3) . . . 4_575 ? O9 Pb4 I11 Pb3 -37.1(5) . . . 4_575 ? I5 Pb4 I11 Pb3 139.16(4) . . . 4_575 ? I10 Pb4 I11 Pb3 47.38(3) . . . 4_575 ? I4 Pb4 I11 Pb3 -50.3(4) . . . 4_575 ? I8 Pb4 I11 Pb3 -125.33(4) . . . 4_575 ? O8 Nd1 O1 S1 6.2(9) . . . . ? O6 Nd1 O1 S1 75.0(11) . . . . ? O7 Nd1 O1 S1 135.1(11) . . . . ? O3 Nd1 O1 S1 -72.2(10) . . . . ? O2 Nd1 O1 S1 -146.0(11) . . . . ? O4 Nd1 O1 S1 -176.5(9) . . . . ? O5 Nd1 O1 S1 -21.8(15) . . . . ? O8 Nd1 O2 S2B -7(2) . . . . ? O6 Nd1 O2 S2B 146.6(16) . . . . ? O7 Nd1 O2 S2B 112.4(18) . . . . ? O3 Nd1 O2 S2B -53.4(17) . . . . ? O4 Nd1 O2 S2B -163.5(19) . . . . ? O1 Nd1 O2 S2B 34.6(17) . . . . ? O5 Nd1 O2 S2B -109.9(17) . . . . ? O8 Nd1 O2 S2A -55.7(17) . . . . ? O6 Nd1 O2 S2A 97.6(15) . . . . ? O7 Nd1 O2 S2A 63.4(14) . . . . ? O3 Nd1 O2 S2A -102.4(14) . . . . ? O4 Nd1 O2 S2A 147.5(15) . . . . ? O1 Nd1 O2 S2A -14.4(13) . . . . ? O5 Nd1 O2 S2A -158.9(13) . . . . ? O8 Nd1 O3 S3 75.8(15) . . . . ? O6 Nd1 O3 S3 24(2) . . . . ? O7 Nd1 O3 S3 -159.2(12) . . . . ? O2 Nd1 O3 S3 -134.1(16) . . . . ? O4 Nd1 O3 S3 -67.2(16) . . . . ? O1 Nd1 O3 S3 148.5(16) . . . . ? O5 Nd1 O3 S3 -2.4(15) . . . . ? O8 Nd1 O4 S4 167.7(10) . . . . ? O6 Nd1 O4 S4 111.1(14) . . . . ? O7 Nd1 O4 S4 39.3(13) . . . . ? O3 Nd1 O4 S4 -106.0(13) . . . . ? O2 Nd1 O4 S4 -38.9(12) . . . . ? O1 Nd1 O4 S4 -7.9(19) . . . . ? O5 Nd1 O4 S4 -172.1(15) . . . . ? O8 Nd1 O5 S5 117.7(12) . . . . ? O6 Nd1 O5 S5 34.7(11) . . . . ? O7 Nd1 O5 S5 -0.6(15) . . . . ? O3 Nd1 O5 S5 -161.4(12) . . . . ? O2 Nd1 O5 S5 -104.8(11) . . . . ? O4 Nd1 O5 S5 -50.2(10) . . . . ? O1 Nd1 O5 S5 145.2(8) . . . . ? O8 Nd1 O6 S6 163.6(13) . . . . ? O7 Nd1 O6 S6 36.7(12) . . . . ? O3 Nd1 O6 S6 -145.3(11) . . . . ? O2 Nd1 O6 S6 1.4(18) . . . . ? O4 Nd1 O6 S6 -46.4(12) . . . . ? O1 Nd1 O6 S6 99.3(12) . . . . ? O5 Nd1 O6 S6 -119.0(13) . . . . ? O8 Nd1 O7 S7 125.3(11) . . . . ? O6 Nd1 O7 S7 -169.8(13) . . . . ? O3 Nd1 O7 S7 12.4(17) . . . . ? O2 Nd1 O7 S7 -12.3(11) . . . . ? O4 Nd1 O7 S7 -86.8(12) . . . . ? O1 Nd1 O7 S7 66.8(12) . . . . ? O5 Nd1 O7 S7 -133.7(11) . . . . ? O6 Nd1 O8 S8 38.6(13) . . . . ? O7 Nd1 O8 S8 99.0(13) . . . . ? O3 Nd1 O8 S8 -113.1(14) . . . . ? O2 Nd1 O8 S8 -158.5(11) . . . . ? O4 Nd1 O8 S8 -18.2(19) . . . . ? O1 Nd1 O8 S8 159.1(14) . . . . ? O5 Nd1 O8 S8 -37.9(13) . . . . ? Nd1 O1 S1 C1 89.1(12) . . . . ? Nd1 O1 S1 C2 -168.8(10) . . . . ? S2B O2 S2A C4A -28.0(17) . . . . ? Nd1 O2 S2A C4A 96.8(19) . . . . ? S2B O2 S2A C3 68.2(13) . . . . ? Nd1 O2 S2A C3 -166.9(12) . . . . ? S2A O2 S2B C4B 31.1(19) . . . . ? Nd1 O2 S2B C4B -63(3) . . . . ? S2A O2 S2B C3 -73.5(13) . . . . ? Nd1 O2 S2B C3 -167.2(15) . . . . ? Nd1 O3 S3 C6 -157.6(15) . . . . ? Nd1 O3 S3 C5 93.5(17) . . . . ? Nd1 O4 S4 C8 115.4(13) . . . . ? Nd1 O4 S4 C7 -142.2(13) . . . . ? Nd1 O5 S5 C10 -116.2(12) . . . . ? Nd1 O5 S5 C9 146.4(11) . . . . ? Nd1 O6 S6 C11 143.8(13) . . . . ? Nd1 O6 S6 C12 -118.8(13) . . . . ? Nd1 O7 S7 C13 155.9(12) . . . . ? Nd1 O7 S7 C14 -100.3(13) . . . . ? Nd1 O8 S8 C15 -154.4(12) . . . . ? Nd1 O8 S8 C16 102.7(14) . . . . ? O2 S2B C3 S2A 71.1(16) . . . . ? C4B S2B C3 S2A -51.3(19) . . . . ? O2 S2A C3 S2B -66.9(15) . . . . ? C4A S2A C3 S2B 34.8(18) . . . . ? I5 Pb4 O9 S9 155(4) . . . . ? I11 Pb4 O9 S9 -166.8(15) . . . . ? I10 Pb4 O9 S9 101.4(15) . . . . ? I4 Pb4 O9 S9 11.8(15) . . . . ? I8 Pb4 O9 S9 -74.8(14) . . . . ? I5 Pb4 O9 Pb3 8(5) . . . 4_575 ? I11 Pb4 O9 Pb3 46.2(5) . . . 4_575 ? I10 Pb4 O9 Pb3 -45.6(5) . . . 4_575 ? I4 Pb4 O9 Pb3 -135.3(5) . . . 4_575 ? I8 Pb4 O9 Pb3 138.2(5) . . . 4_575 ? Pb3 O9 S9 C18 57(2) 4_575 . . . ? Pb4 O9 S9 C18 -74.6(19) . . . . ? Pb3 O9 S9 C17 -50(2) 4_575 . . . ? Pb4 O9 S9 C17 178.7(14) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.670 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.162 _database_code_depnum_ccdc_archive 'CCDC 958529'