# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xian-Qiang Li' _publ_contact_author_email lixianqiang@fjirsm.ac.cn _publ_author_name 'Shaowu Du' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 835032' #TrackingRef '- Cif date.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H64 K6 N2 O39 Pb6' _chemical_formula_weight 3155.13 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P63/mmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-y, -x, -z+1/2' 'x-y, -y, -z' 'x, x-y, -z+1/2' 'y, x, -z' '-x+y, y, -z+1/2' '-x, -x+y, -z' '-x, -y, -z' '-x+y, -x, -z-1/2' 'y, -x+y, -z' 'x, y, -z-1/2' 'x-y, x, -z' '-y, x-y, -z-1/2' 'y, x, z-1/2' '-x+y, y, z' '-x, -x+y, z-1/2' '-y, -x, z' 'x-y, -y, z-1/2' 'x, x-y, z' _cell_length_a 15.8708(6) _cell_length_b 15.8708(6) _cell_length_c 24.2726(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5294.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5073 _cell_measurement_theta_min 2.2386 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2951 _exptl_absorpt_coefficient_mu 9.820 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6444 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 ; Mercury2 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34219 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.50 _reflns_number_total 1874 _reflns_number_gt 1809 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0624P)^2^+45.5334P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1874 _refine_ls_number_parameters 126 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.050 _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 -0.28067(2) -0.140335(12) 0.475857(14) 0.02920(17) Uani 1 2 d S . . K1 K -0.1770(2) -0.08851(11) 0.63826(13) 0.0629(8) Uani 1 2 d S . . O1 O -0.4040(3) -0.2919(3) 0.50769(19) 0.0354(10) Uani 1 1 d . . . O2 O -0.2958(4) -0.2517(4) 0.5751(2) 0.0453(13) Uani 1 1 d . . . O3 O -0.3712(5) -0.1856(2) 0.3962(3) 0.0358(15) Uani 1 2 d S . . O4 O -0.2234(5) -0.1117(2) 0.3560(3) 0.0371(15) Uani 1 2 d S . . O5 O 0.0000 0.0000 0.7068(12) 0.112(7) Uani 1 6 d SU . . O6W O 0.0000 0.0000 0.530(2) 0.109(17) Uani 0.50 6 d SPU . . N1 N -0.6667 -0.3333 0.4499(6) 0.032(3) Uani 1 6 d S . . C1 C -0.3763(5) -0.3073(5) 0.5540(3) 0.0340(15) Uani 1 1 d . . . C2 C -0.3138(8) -0.1569(4) 0.3546(4) 0.0303(19) Uani 1 2 d S . . C3 C -0.5341(3) -0.4659(3) 0.5580(4) 0.030(2) Uani 1 2 d S . . H3 H -0.5485 -0.4515 0.5233 0.037 Uiso 1 2 calc SR . . C4 C -0.4472(5) -0.3998(5) 0.5831(3) 0.0320(14) Uani 1 1 d . . . C5 C -0.4263(6) -0.4230(6) 0.6350(3) 0.0453(19) Uani 1 1 d . . . H5 H -0.3686 -0.3797 0.6526 0.054 Uiso 1 1 calc R . . C6 C -0.4906(5) -0.5094(5) 0.6602(4) 0.053(3) Uani 1 2 d S . . H6 H -0.4754 -0.5246 0.6944 0.064 Uiso 1 2 calc SR . . C7 C -0.3125(11) -0.1562(5) 0.2500 0.032(3) Uani 1 4 d S . . H7 H -0.2448 -0.1224 0.2500 0.038 Uiso 1 4 calc SR . . C8 C -0.3659(7) -0.1830(3) 0.3000(4) 0.032(2) Uani 1 2 d S . . C9 C -0.4653(9) -0.2327(4) 0.2990(5) 0.108(8) Uani 1 2 d SU . . H9 H -0.5000 -0.2500 0.3319 0.129 Uiso 1 2 calc SR . . C10 C -0.5139(16) -0.2570(8) 0.2500 0.19(2) Uani 1 4 d SU . . H10 H -0.5816 -0.2908 0.2500 0.225 Uiso 1 4 calc SR . . C11 C -0.6667 -0.3333 0.5113(8) 0.063(6) Uani 1 6 d S . . H11A H -0.6996 -0.3992 0.5245 0.094 Uiso 0.33 2 calc SPR . . H11B H -0.6996 -0.3004 0.5245 0.094 Uiso 0.33 2 calc SPR . . H11C H -0.6008 -0.3004 0.5245 0.094 Uiso 0.33 2 calc SPR . . C12 C -0.6149(4) -0.2298(7) 0.4300(4) 0.046(3) Uani 1 2 d S . . H12A H -0.6147 -0.2290 0.3904 0.069 Uiso 1 2 calc SR . . H12B H -0.5491 -0.1972 0.4433 0.069 Uiso 0.50 1 calc PR . . H12C H -0.6478 -0.1971 0.4435 0.069 Uiso 0.50 1 calc PR . . 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 0.0234(2) 0.0288(2) 0.0336(2) 0.00004(6) 0.00008(13) 0.01171(11) K1 0.0708(19) 0.0428(9) 0.0843(19) -0.0189(8) -0.0379(16) 0.0354(9) O1 0.032(3) 0.030(2) 0.040(2) 0.009(2) 0.001(2) 0.013(2) O2 0.032(3) 0.034(3) 0.055(3) -0.004(2) -0.014(2) 0.005(2) O3 0.027(3) 0.042(3) 0.033(3) 0.0016(14) 0.003(3) 0.0137(17) O4 0.030(4) 0.044(3) 0.033(3) 0.0003(14) 0.001(3) 0.0150(18) O5 0.053(6) 0.053(6) 0.23(2) 0.000 0.000 0.027(3) O6W 0.060(13) 0.060(13) 0.21(5) 0.000 0.000 0.030(7) N1 0.029(4) 0.029(4) 0.038(7) 0.000 0.000 0.015(2) C1 0.036(4) 0.028(3) 0.040(4) -0.001(3) 0.003(3) 0.018(3) C2 0.038(5) 0.029(3) 0.027(4) -0.001(2) -0.002(4) 0.019(3) C3 0.029(3) 0.029(3) 0.035(5) 0.0006(19) -0.0006(19) 0.014(4) C4 0.030(3) 0.024(3) 0.038(3) -0.004(3) -0.003(3) 0.010(3) C5 0.044(5) 0.045(5) 0.039(4) -0.002(3) -0.011(3) 0.016(4) C6 0.053(5) 0.053(5) 0.037(5) 0.012(3) -0.012(3) 0.014(6) C7 0.033(7) 0.030(5) 0.035(7) 0.000 0.000 0.016(4) C8 0.025(5) 0.034(4) 0.034(5) 0.0004(19) 0.001(4) 0.013(2) C9 0.019(6) 0.200(18) 0.044(7) 0.004(3) 0.008(5) 0.009(3) C10 0.027(10) 0.37(5) 0.044(11) 0.000 0.000 0.013(5) C11 0.074(10) 0.074(10) 0.040(11) 0.000 0.000 0.037(5) C12 0.049(5) 0.023(5) 0.057(6) -0.004(5) -0.002(2) 0.012(2) _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 O3 2.299(7) . ? Pb1 O1 2.347(5) 24 ? Pb1 O1 2.347(5) . ? Pb1 O2 2.925(5) 24 ? Pb1 O2 2.925(5) . ? Pb1 C2 2.978(9) . ? Pb1 C1 2.984(7) 24 ? Pb1 C1 2.984(7) . ? Pb1 O2 2.994(6) 15_556 ? Pb1 O2 2.994(6) 10_556 ? Pb1 O4 3.014(6) . ? Pb1 Pb1 4.0318(4) 15_556 ? K1 O2 2.780(5) . ? K1 O2 2.780(5) 24 ? K1 O4 2.810(5) 8_556 ? K1 O4 2.810(5) 10_556 ? K1 O5 2.948(17) 1 ? O1 C1 1.275(8) . ? O2 C1 1.242(8) . ? O2 Pb1 2.994(6) 17_556 ? O3 C2 1.282(11) . ? O4 C2 1.243(12) . ? O5 O5 0.00(6) 1 ? O6W O6W 1.45(9) 13_556 ? N1 C11 1.49(2) . ? N1 C12 1.503(11) 3_455 ? N1 C12 1.503(11) . ? N1 C12 1.503(11) 5_445 ? C1 C4 1.506(9) . ? C2 C8 1.507(13) . ? C3 C4 1.388(8) . ? C3 C4 1.388(8) 22_445 ? C3 H3 0.9300 . ? C4 C5 1.397(9) . ? C5 C6 1.377(9) . ? C5 H5 0.9300 . ? C6 C5 1.377(9) 22_445 ? C6 H6 0.9300 . ? C7 C8 1.418(12) 16_556 ? C7 C8 1.418(12) . ? C7 H7 0.9300 . ? C8 C9 1.366(14) . ? C9 C10 1.364(17) . ? C9 H9 0.9300 . ? C10 C9 1.364(17) 16_556 ? C10 H10 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 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 O3 Pb1 O1 83.45(17) . 24 ? O3 Pb1 O1 83.45(17) . . ? O1 Pb1 O1 74.9(2) 24 . ? O3 Pb1 O2 130.84(14) . 24 ? O1 Pb1 O2 48.33(15) 24 24 ? O1 Pb1 O2 91.14(17) . 24 ? O3 Pb1 O2 130.84(14) . . ? O1 Pb1 O2 91.14(17) 24 . ? O1 Pb1 O2 48.33(15) . . ? O2 Pb1 O2 68.5(2) 24 . ? O3 Pb1 C2 24.0(3) . . ? O1 Pb1 C2 102.41(19) 24 . ? O1 Pb1 C2 102.4(2) . . ? O2 Pb1 C2 143.40(12) 24 . ? O2 Pb1 C2 143.40(12) . . ? O3 Pb1 C1 107.25(18) . 24 ? O1 Pb1 C1 24.10(17) 24 24 ? O1 Pb1 C1 81.81(18) . 24 ? O2 Pb1 C1 24.24(16) 24 24 ? O2 Pb1 C1 78.57(17) . 24 ? C2 Pb1 C1 124.14(18) . 24 ? O3 Pb1 C1 107.25(18) . . ? O1 Pb1 C1 81.81(18) 24 . ? O1 Pb1 C1 24.10(17) . . ? O2 Pb1 C1 78.57(17) 24 . ? O2 Pb1 C1 24.24(16) . . ? C2 Pb1 C1 124.14(19) . . ? C1 Pb1 C1 78.6(2) 24 . ? O3 Pb1 O2 74.02(12) . 15_556 ? O1 Pb1 O2 71.60(15) 24 15_556 ? O1 Pb1 O2 141.24(15) . 15_556 ? O2 Pb1 O2 80.92(17) 24 15_556 ? O2 Pb1 O2 148.96(12) . 15_556 ? C2 Pb1 O2 67.19(11) . 15_556 ? C1 Pb1 O2 75.54(15) 24 15_556 ? C1 Pb1 O2 153.14(16) . 15_556 ? O3 Pb1 O2 74.02(12) . 10_556 ? O1 Pb1 O2 141.24(15) 24 10_556 ? O1 Pb1 O2 71.60(15) . 10_556 ? O2 Pb1 O2 148.96(12) 24 10_556 ? O2 Pb1 O2 80.92(16) . 10_556 ? C2 Pb1 O2 67.19(11) . 10_556 ? C1 Pb1 O2 153.14(16) 24 10_556 ? C1 Pb1 O2 75.54(15) . 10_556 ? O2 Pb1 O2 128.58(19) 15_556 10_556 ? O3 Pb1 O4 47.9(2) . . ? O1 Pb1 O4 120.43(15) 24 . ? O1 Pb1 O4 120.43(15) . . ? O2 Pb1 O4 144.42(12) 24 . ? O2 Pb1 O4 144.42(12) . . ? C2 Pb1 O4 23.9(2) . . ? C1 Pb1 O4 136.80(14) 24 . ? C1 Pb1 O4 136.80(14) . . ? O2 Pb1 O4 64.32(9) 15_556 . ? O2 Pb1 O4 64.32(9) 10_556 . ? O3 Pb1 Pb1 120.22(5) . 15_556 ? O1 Pb1 Pb1 75.30(12) 24 15_556 ? O1 Pb1 Pb1 138.91(12) . 15_556 ? O2 Pb1 Pb1 47.79(11) 24 15_556 ? O2 Pb1 Pb1 105.15(10) . 15_556 ? C2 Pb1 Pb1 111.13(9) . 15_556 ? C1 Pb1 Pb1 60.05(13) 24 15_556 ? C1 Pb1 Pb1 123.42(13) . 15_556 ? O2 Pb1 Pb1 46.35(10) 15_556 15_556 ? O2 Pb1 Pb1 143.41(9) 10_556 15_556 ? O4 Pb1 Pb1 98.96(7) . 15_556 ? O2 K1 O2 72.7(2) . 24 ? O2 K1 O4 140.85(19) . 8_556 ? O2 K1 O4 69.78(17) 24 8_556 ? O2 K1 O4 69.78(17) . 10_556 ? O2 K1 O4 140.85(19) 24 10_556 ? O4 K1 O4 142.3(2) 8_556 10_556 ? O2 K1 O5 142.76(15) . 1 ? O2 K1 O5 142.76(16) 24 1 ? O4 K1 O5 73.04(14) 8_556 1 ? O4 K1 O5 73.04(14) 10_556 1 ? C1 O1 Pb1 107.2(4) . . ? C1 O2 K1 150.0(5) . . ? C1 O2 Pb1 80.5(4) . . ? K1 O2 Pb1 94.52(16) . . ? C1 O2 Pb1 110.8(4) . 17_556 ? K1 O2 Pb1 98.26(16) . 17_556 ? Pb1 O2 Pb1 85.86(14) . 17_556 ? C2 O3 Pb1 109.3(6) . . ? C2 O4 Pb1 76.4(5) . . ? C11 N1 C12 108.8(7) . 3_455 ? C11 N1 C12 108.8(7) . . ? C12 N1 C12 110.1(6) 3_455 . ? C11 N1 C12 108.8(7) . 5_445 ? C12 N1 C12 110.1(6) 3_455 5_445 ? C12 N1 C12 110.1(6) . 5_445 ? O2 C1 O1 123.9(6) . . ? O2 C1 C4 120.1(6) . . ? O1 C1 C4 116.0(6) . . ? O2 C1 Pb1 75.2(4) . . ? O1 C1 Pb1 48.7(3) . . ? C4 C1 Pb1 164.6(5) . . ? O4 C2 O3 126.4(8) . . ? O4 C2 C8 120.0(8) . . ? O3 C2 C8 113.7(8) . . ? O4 C2 Pb1 79.6(5) . . ? O3 C2 Pb1 46.8(4) . . ? C8 C2 Pb1 160.4(7) . . ? C4 C3 C4 122.1(9) . 22_445 ? C4 C3 H3 119.0 . . ? C4 C3 H3 119.0 22_445 . ? C3 C4 C5 118.2(7) . . ? C3 C4 C1 120.5(6) . . ? C5 C4 C1 121.2(6) . . ? C6 C5 C4 120.5(7) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C5 120.5(10) . 22_445 ? C5 C6 H6 119.7 . . ? C5 C6 H6 119.7 22_445 . ? C8 C7 C8 117.6(13) 16_556 . ? C8 C7 H7 121.2 16_556 . ? C8 C7 H7 121.2 . . ? C9 C8 C7 120.2(10) . . ? C9 C8 C2 119.4(10) . . ? C7 C8 C2 120.4(9) . . ? C10 C9 C8 120.4(13) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C9 121.3(19) . 16_556 ? C9 C10 H10 119.3 . . ? C9 C10 H10 119.3 16_556 . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.225 _refine_diff_density_min -1.590 _refine_diff_density_rms 0.161 #===END data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 835033' #TrackingRef '- Cif date.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H64 N2 O39 Pb6 Rb6' _chemical_formula_weight 3433.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P63/mmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-y, -x, -z+1/2' 'x-y, -y, -z' 'x, x-y, -z+1/2' 'y, x, -z' '-x+y, y, -z+1/2' '-x, -x+y, -z' '-x, -y, -z' '-x+y, -x, -z-1/2' 'y, -x+y, -z' 'x, y, -z-1/2' 'x-y, x, -z' '-y, x-y, -z-1/2' 'y, x, z-1/2' '-x+y, y, z' '-x, -x+y, z-1/2' '-y, -x, z' 'x-y, -y, z-1/2' 'x, x-y, z' _cell_length_a 16.03340(10) _cell_length_b 16.03340(10) _cell_length_c 24.3028(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5410.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15965 _cell_measurement_theta_min 2.2063 _cell_measurement_theta_max 27.4816 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3167 _exptl_absorpt_coefficient_mu 12.060 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4480 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33913 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 24.00 _reflns_number_total 1615 _reflns_number_gt 1609 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0955P)^2^+65.3576P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1615 _refine_ls_number_parameters 127 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.081 _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 0.28491(4) 0.142453(18) 0.02547(2) 0.0295(3) Uani 1 2 d S . . Rb1 Rb 0.17889(14) 0.08945(7) -0.13822(9) 0.0630(6) Uani 1 2 d S . . O1 O 0.4067(5) 0.1139(5) -0.0063(3) 0.0372(16) Uani 1 1 d . . . O2 O 0.2980(5) 0.0437(6) -0.0725(3) 0.0460(19) Uani 1 1 d . . . O3 O 0.3766(7) 0.1883(3) 0.1039(4) 0.039(2) Uani 1 2 d S . . O4 O 0.2322(7) 0.1161(4) 0.1441(4) 0.039(2) Uani 1 2 d S . . O5 O 0.0000 0.0000 -0.2073(13) 0.083(7) Uani 1 6 d S . . O6W O 0.0000 0.0000 0.0000 0.15(2) Uani 1 12 d SU . . N1 N 0.6667 0.3333 0.0530(12) 0.079(9) Uani 1 6 d S . . C1 C 0.3786(7) 0.0701(7) -0.0513(4) 0.034(2) Uani 1 1 d . . . C2 C 0.3214(11) 0.1607(6) 0.1459(6) 0.032(3) Uani 1 2 d S . . C3 C 0.5347(5) 0.0694(10) -0.0564(6) 0.028(3) Uani 1 2 d S . . H3A H 0.5499 0.0997 -0.0223 0.034 Uiso 1 2 calc SR . . C4 C 0.4483(8) 0.0478(8) -0.0808(4) 0.038(2) Uani 1 1 d . . . C5 C 0.4267(9) 0.0033(10) -0.1325(5) 0.050(3) Uani 1 1 d . . . H5A H 0.3694 -0.0117 -0.1502 0.060 Uiso 1 1 calc R . . C6 C 0.4912(8) -0.0176(16) -0.1567(7) 0.063(5) Uani 1 2 d S . . H6A H 0.4763 -0.0474 -0.1910 0.076 Uiso 1 2 calc SR . . C7 C 0.3234(15) 0.1617(7) 0.2500 0.031(4) Uani 1 4 d S . . H7A H 0.2564 0.1282 0.2500 0.037 Uiso 1 4 calc SR . . C8 C 0.3721(11) 0.1860(5) 0.2001(6) 0.045(4) Uani 1 2 d SU . . C9 C 0.4700(13) 0.2350(6) 0.2020(8) 0.070(4) Uani 1 2 d SU . . H9A H 0.5070 0.2783 0.1726 0.084 Uiso 0.50 1 d PR . . C10 C 0.518(2) 0.220(3) 0.2500 0.058(7) Uani 0.50 2 d SPU . . H10A H 0.5731 0.2112 0.2500 0.069 Uiso 0.50 2 d SPR . . C11 C 0.6667 0.3333 -0.0136(14) 0.087(13) Uani 1 6 d S . . H11A H 0.6993 0.3007 -0.0267 0.131 Uiso 0.33 2 calc SPR . . H11B H 0.6993 0.3985 -0.0267 0.131 Uiso 0.33 2 calc SPR . . H11C H 0.6015 0.3007 -0.0267 0.131 Uiso 0.33 2 calc SPR . . C12 C 0.6152(8) 0.3848(8) 0.0703(8) 0.082(7) Uani 1 2 d S . . H12A H 0.6135 0.3870 0.1097 0.123 Uiso 1 2 calc SR . . H12B H 0.5506 0.3514 0.0562 0.123 Uiso 0.50 1 calc PR . . H12C H 0.6483 0.4493 0.0560 0.123 Uiso 0.50 1 calc PR . . 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 0.0253(4) 0.0317(4) 0.0294(4) -0.00005(10) -0.00010(19) 0.01264(19) Rb1 0.0710(12) 0.0440(7) 0.0829(13) -0.0217(5) -0.0434(10) 0.0355(6) O1 0.038(4) 0.045(4) 0.034(4) -0.001(4) 0.000(3) 0.025(3) O2 0.037(4) 0.063(5) 0.047(5) -0.001(4) -0.009(3) 0.032(4) O3 0.034(6) 0.048(5) 0.029(5) 0.002(2) 0.004(4) 0.017(3) O4 0.026(5) 0.043(4) 0.042(6) -0.003(2) -0.005(4) 0.013(3) O5 0.060(9) 0.060(9) 0.13(2) 0.000 0.000 0.030(5) O6W 0.077(19) 0.077(19) 0.30(6) 0.000 0.000 0.038(9) N1 0.096(15) 0.096(15) 0.046(17) 0.000 0.000 0.048(8) C1 0.036(6) 0.033(5) 0.038(6) 0.003(4) -0.001(5) 0.022(5) C2 0.036(9) 0.030(5) 0.033(8) 0.003(3) 0.006(7) 0.018(4) C3 0.029(5) 0.036(7) 0.021(6) -0.006(6) -0.003(3) 0.018(4) C4 0.037(6) 0.043(6) 0.032(5) -0.001(5) -0.001(5) 0.019(5) C5 0.048(7) 0.071(8) 0.041(7) -0.008(6) -0.009(5) 0.037(7) C6 0.072(9) 0.090(15) 0.034(9) -0.027(10) -0.013(5) 0.045(8) C7 0.024(10) 0.032(8) 0.032(11) 0.000 0.000 0.012(5) C8 0.028(6) 0.067(8) 0.025(7) 0.002(3) 0.004(5) 0.014(3) C9 0.035(7) 0.111(9) 0.040(7) 0.003(3) 0.006(5) 0.018(3) C10 0.031(9) 0.095(12) 0.036(10) 0.000 0.000 0.023(9) C11 0.11(2) 0.11(2) 0.040(19) 0.000 0.000 0.055(11) C12 0.109(15) 0.109(15) 0.054(12) 0.004(5) -0.004(5) 0.073(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 O3 2.293(10) . ? Pb1 O1 2.348(7) 24 ? Pb1 O1 2.348(7) . ? Pb1 O2 2.924(8) 24 ? Pb1 O2 2.924(8) . ? Pb1 C2 2.969(15) . ? Pb1 C1 2.971(10) 24 ? Pb1 C1 2.971(10) . ? Pb1 O4 2.976(10) . ? Pb1 O2 2.998(9) 17 ? Pb1 O2 2.998(9) 8 ? Pb1 Pb1 4.1451(6) 15 ? Rb1 O2 2.854(7) . ? Rb1 O2 2.854(7) 24 ? Rb1 O4 2.929(7) 8 ? Rb1 O4 2.929(7) 10 ? Rb1 O5 2.998(18) 1 ? O1 C1 1.256(13) . ? O2 C1 1.250(12) . ? O2 Pb1 2.998(9) 15 ? O3 C2 1.276(17) . ? O4 C2 1.239(19) . ? O5 O5 0.00(6) 1 ? N1 C12 1.49(2) 5_665 ? N1 C12 1.49(2) 3_655 ? N1 C12 1.49(2) . ? N1 C11 1.62(5) . ? C1 C4 1.514(15) . ? C2 C8 1.50(2) . ? C3 C4 1.382(13) 20_655 ? C3 C4 1.382(13) . ? C3 H3A 0.9300 . ? C4 C5 1.401(15) . ? C5 C6 1.369(14) . ? C5 H5A 0.9300 . ? C6 C5 1.369(14) 20_655 ? C6 H6A 0.9300 . ? C7 C8 1.388(18) . ? C7 C8 1.388(18) 16_556 ? C7 H7A 0.9300 . ? C8 C9 1.36(2) . ? C9 C10 1.48(3) . ? C9 C10 1.48(3) 9 ? C9 H9A 0.9643 . ? C10 C10 1.25(8) 9 ? C10 C9 1.48(3) 16_556 ? C10 H10A 0.9601 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 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 O3 Pb1 O1 82.7(3) . 24 ? O3 Pb1 O1 82.7(3) . . ? O1 Pb1 O1 75.3(4) 24 . ? O3 Pb1 O2 129.9(2) . 24 ? O1 Pb1 O2 48.3(2) 24 24 ? O1 Pb1 O2 92.3(2) . 24 ? O3 Pb1 O2 129.9(2) . . ? O1 Pb1 O2 92.3(2) 24 . ? O1 Pb1 O2 48.3(2) . . ? O2 Pb1 O2 70.6(3) 24 . ? O3 Pb1 C2 23.9(4) . . ? O1 Pb1 C2 101.6(3) 24 . ? O1 Pb1 C2 101.6(3) . . ? O2 Pb1 C2 142.31(18) 24 . ? O2 Pb1 C2 142.31(18) . . ? O3 Pb1 C1 106.2(3) . 24 ? O1 Pb1 C1 23.8(3) 24 24 ? O1 Pb1 C1 82.6(3) . 24 ? O2 Pb1 C1 24.5(2) 24 24 ? O2 Pb1 C1 80.4(3) . 24 ? C2 Pb1 C1 123.0(3) . 24 ? O3 Pb1 C1 106.2(3) . . ? O1 Pb1 C1 82.6(3) 24 . ? O1 Pb1 C1 23.8(3) . . ? O2 Pb1 C1 80.4(3) 24 . ? O2 Pb1 C1 24.5(2) . . ? C2 Pb1 C1 123.0(3) . . ? C1 Pb1 C1 80.1(4) 24 . ? O3 Pb1 O4 48.0(3) . . ? O1 Pb1 O4 119.7(2) 24 . ? O1 Pb1 O4 119.7(2) . . ? O2 Pb1 O4 143.53(17) 24 . ? O2 Pb1 O4 143.53(17) . . ? C2 Pb1 O4 24.1(4) . . ? C1 Pb1 O4 135.8(2) 24 . ? C1 Pb1 O4 135.8(2) . . ? O3 Pb1 O2 76.22(18) . 17 ? O1 Pb1 O2 70.7(2) 24 17 ? O1 Pb1 O2 141.7(2) . 17 ? O2 Pb1 O2 77.9(2) 24 17 ? O2 Pb1 O2 147.85(18) . 17 ? C2 Pb1 O2 69.44(17) . 17 ? C1 Pb1 O2 73.3(2) 24 17 ? C1 Pb1 O2 152.7(2) . 17 ? O4 Pb1 O2 66.17(14) . 17 ? O3 Pb1 O2 76.22(18) . 8 ? O1 Pb1 O2 141.7(2) 24 8 ? O1 Pb1 O2 70.7(2) . 8 ? O2 Pb1 O2 147.85(18) 24 8 ? O2 Pb1 O2 77.9(2) . 8 ? C2 Pb1 O2 69.44(17) . 8 ? C1 Pb1 O2 152.7(2) 24 8 ? C1 Pb1 O2 73.3(2) . 8 ? O4 Pb1 O2 66.17(14) . 8 ? O2 Pb1 O2 132.1(3) 17 8 ? O3 Pb1 Pb1 120.89(7) . 15 ? O1 Pb1 Pb1 138.63(18) 24 15 ? O1 Pb1 Pb1 74.98(18) . 15 ? O2 Pb1 Pb1 105.32(14) 24 15 ? O2 Pb1 Pb1 46.31(17) . 15 ? C2 Pb1 Pb1 112.06(14) . 15 ? C1 Pb1 Pb1 123.6(2) 24 15 ? C1 Pb1 Pb1 59.31(19) . 15 ? O4 Pb1 Pb1 99.91(10) . 15 ? O2 Pb1 Pb1 143.27(14) 17 15 ? O2 Pb1 Pb1 44.85(15) 8 15 ? O2 Rb1 O2 72.6(3) . 24 ? O2 Rb1 O4 68.6(2) . 8 ? O2 Rb1 O4 139.9(3) 24 8 ? O2 Rb1 O4 139.9(3) . 10 ? O2 Rb1 O4 68.6(2) 24 10 ? O4 Rb1 O4 144.9(3) 8 10 ? O2 Rb1 O5 142.5(2) . 1 ? O2 Rb1 O5 142.5(2) 24 1 ? O4 Rb1 O5 74.08(18) 8 1 ? O4 Rb1 O5 74.08(18) 10 1 ? C1 O1 Pb1 107.1(6) . . ? C1 O2 Rb1 148.6(7) . . ? C1 O2 Pb1 79.9(6) . . ? Rb1 O2 Pb1 94.5(2) . . ? C1 O2 Pb1 112.7(6) . 15 ? Rb1 O2 Pb1 98.0(2) . 15 ? Pb1 O2 Pb1 88.8(2) . 15 ? C2 O3 Pb1 109.3(9) . . ? C2 O4 Pb1 77.7(8) . . ? C12 N1 C12 112.4(12) 5_665 3_655 ? C12 N1 C12 112.4(12) 5_665 . ? C12 N1 C12 112.4(12) 3_655 . ? C12 N1 C11 106.3(14) 5_665 . ? C12 N1 C11 106.3(14) 3_655 . ? C12 N1 C11 106.3(14) . . ? O2 C1 O1 124.7(10) . . ? O2 C1 C4 119.0(9) . . ? O1 C1 C4 116.3(9) . . ? O2 C1 Pb1 75.7(6) . . ? O1 C1 Pb1 49.1(5) . . ? C4 C1 Pb1 165.2(7) . . ? O4 C2 O3 125.0(14) . . ? O4 C2 C8 120.0(13) . . ? O3 C2 C8 114.9(13) . . ? O4 C2 Pb1 78.3(8) . . ? O3 C2 Pb1 46.8(7) . . ? C8 C2 Pb1 161.7(10) . . ? C4 C3 C4 122.5(13) 20_655 . ? C4 C3 H3A 118.7 20_655 . ? C4 C3 H3A 118.7 . . ? C3 C4 C5 118.3(10) . . ? C3 C4 C1 120.3(9) . . ? C5 C4 C1 121.4(10) . . ? C6 C5 C4 119.1(11) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C5 C6 C5 122.7(16) . 20_655 ? C5 C6 H6A 118.7 . . ? C5 C6 H6A 118.7 20_655 . ? C8 C7 C8 122(2) . 16_556 ? C8 C7 H7A 119.2 . . ? C8 C7 H7A 119.2 16_556 . ? C9 C8 C7 117.3(16) . . ? C9 C8 C2 119.9(15) . . ? C7 C8 C2 122.7(14) . . ? C8 C9 C10 118.4(18) . . ? C8 C9 C10 118.4(18) . 9 ? C10 C9 C10 50(3) . 9 ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 121.0 . . ? C10 C9 H9A 99.7 9 . ? C10 C10 C9 65.1(15) 9 . ? C10 C10 C9 65.1(15) 9 16_556 ? C9 C10 C9 104(2) . 16_556 ? C10 C10 H10A 127.4 9 . ? C9 C10 H10A 127.9 . . ? C9 C10 H10A 127.9 16_556 . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.459 _refine_diff_density_min -1.287 _refine_diff_density_rms 0.232 #===END data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 835034' #TrackingRef '- Cif date.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H64 Cs6 N2 O39 Pb6' _chemical_formula_weight 3717.99 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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P63/mmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-y, -x, -z+1/2' 'x-y, -y, -z' 'x, x-y, -z+1/2' 'y, x, -z' '-x+y, y, -z+1/2' '-x, -x+y, -z' '-x, -y, -z' '-x+y, -x, -z-1/2' 'y, -x+y, -z' 'x, y, -z-1/2' 'x-y, x, -z' '-y, x-y, -z-1/2' 'y, x, z-1/2' '-x+y, y, z' '-x, -x+y, z-1/2' '-y, -x, z' 'x-y, -y, z-1/2' 'x, x-y, z' _cell_length_a 16.231(3) _cell_length_b 16.231(3) _cell_length_c 24.466(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5581.9(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16790 _cell_measurement_theta_min 2.2063 _cell_measurement_theta_max 27.4816 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3383 _exptl_absorpt_coefficient_mu 11.019 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5447 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35165 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.00 _reflns_number_total 1681 _reflns_number_gt 1678 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1863P)^2^+126.3105P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1681 _refine_ls_number_parameters 139 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.2407 _refine_ls_wR_factor_gt 0.2397 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.002 _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 0.29019(5) 0.14510(3) 0.02660(3) 0.0299(5) Uani 1 2 d S . . Cs1 Cs 0.1724(7) 0.0862(3) -0.1394(7) 0.071(3) Uani 0.50 2 d SP . 1 Cs1' Cs 0.2056(7) 0.1028(4) -0.1527(7) 0.081(3) Uani 0.50 2 d SP A 2 O1 O 0.4094(7) 0.2938(7) -0.0065(4) 0.033(2) Uani 1 1 d . . . O2 O 0.3000(7) 0.2574(7) -0.0700(5) 0.047(3) Uani 1 1 d . . . O3 O 0.3847(11) 0.1924(5) 0.1044(6) 0.043(4) Uani 1 2 d S . . O4 O 0.2429(12) 0.1214(6) 0.1448(6) 0.043(4) Uani 1 2 d S . . O5 O 0.042(3) 0.084(5) -0.2500 0.050(16) Uani 0.33 4 d SPU . 1 O5' O 0.0000 0.0000 -0.2500 0.050(10) Uani 1 12 d S B 2 O6W O 0.0000 0.0000 0.0000 0.28(7) Uani 1 12 d SU . . N1 N 0.6667 0.3333 0.0501(12) 0.036(7) Uani 1 6 d SU . . C1 C 0.3803(10) 0.3098(11) -0.0497(6) 0.037(4) Uani 1 1 d . . . C2 C 0.3292(15) 0.1646(8) 0.1456(8) 0.032(4) Uani 1 2 d S . . C3 C 0.5349(7) 0.4651(7) -0.0542(8) 0.031(4) Uani 1 2 d S . . H3A H 0.5502 0.4498 -0.0205 0.037 Uiso 1 2 calc SR . . C4 C 0.4493(10) 0.4019(10) -0.0787(6) 0.033(3) Uani 1 1 d . . . C5 C 0.4237(13) 0.4244(12) -0.1290(7) 0.051(4) Uani 1 1 d . . . H5A H 0.3645 0.3841 -0.1444 0.061 Uiso 1 1 calc R . . C6 C 0.4898(10) 0.5102(10) -0.1559(10) 0.057(7) Uani 1 2 d S . . H6A H 0.4771 0.5229 -0.1910 0.069 Uiso 1 2 calc SR . . C7 C 0.334(2) 0.1669(10) 0.2500 0.033(6) Uani 1 4 d S . . H7A H 0.2677 0.1339 0.2500 0.040 Uiso 1 4 calc SR . . C8 C 0.3809(13) 0.1904(7) 0.2015(10) 0.034(5) Uani 1 2 d S . . C9 C 0.478(2) 0.210(2) 0.2021(12) 0.039(7) Uani 0.50 1 d PU . . H9A H 0.5003 0.1940 0.1687 0.047 Uiso 0.50 1 calc PR . . C10 C 0.524(3) 0.212(3) 0.2500 0.044(10) Uani 0.50 2 d SP . . H10A H 0.5842 0.2140 0.2500 0.052 Uiso 0.50 2 d SPR . . C11 C 0.6163(8) 0.3837(8) 0.0700(10) 0.050(6) Uani 1 2 d SU . . H11A H 0.6161 0.3839 0.1092 0.075 Uiso 1 2 calc SR . . H11C H 0.5520 0.3514 0.0568 0.075 Uiso 0.50 1 calc PR . . H11B H 0.6486 0.4480 0.0568 0.075 Uiso 0.50 1 calc PR . . C12 C 0.6667 0.3333 -0.011(3) 0.093(19) Uani 1 6 d SU . . H12B H 0.6989 0.3011 -0.0240 0.140 Uiso 0.33 2 calc SPR . . H12C H 0.6989 0.3977 -0.0240 0.140 Uiso 0.33 2 calc SPR . . H12A H 0.6023 0.3011 -0.0240 0.140 Uiso 0.33 2 calc SPR . . 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 0.0253(6) 0.0323(5) 0.0298(6) -0.00030(13) -0.0006(3) 0.0127(3) Cs1 0.067(5) 0.0374(19) 0.119(8) -0.028(2) -0.056(5) 0.033(3) Cs1' 0.085(7) 0.058(3) 0.109(7) -0.028(3) -0.057(6) 0.043(4) O1 0.034(5) 0.035(5) 0.032(5) 0.007(4) -0.002(4) 0.019(5) O2 0.035(6) 0.038(6) 0.049(7) -0.005(5) -0.010(5) 0.003(5) O3 0.042(9) 0.051(7) 0.032(8) -0.006(3) -0.012(7) 0.021(4) O4 0.051(10) 0.042(6) 0.040(8) -0.005(4) -0.011(7) 0.025(5) O5 0.05(3) 0.05(4) 0.05(4) 0.000 0.000 0.03(2) O5' 0.050(16) 0.050(16) 0.05(2) 0.000 0.000 0.025(8) O6W 0.26(7) 0.26(7) 0.30(10) 0.000 0.000 0.13(4) N1 0.036(10) 0.036(10) 0.036(16) 0.000 0.000 0.018(5) C1 0.028(8) 0.037(8) 0.044(9) -0.006(7) 0.008(6) 0.014(7) C2 0.028(11) 0.030(7) 0.036(11) 0.000(5) 0.001(9) 0.014(6) C3 0.031(8) 0.031(8) 0.034(11) -0.006(4) 0.006(4) 0.019(9) C4 0.026(7) 0.040(8) 0.039(7) 0.000(6) 0.003(6) 0.020(7) C5 0.048(10) 0.042(10) 0.049(10) 0.001(8) -0.004(8) 0.013(7) C6 0.065(12) 0.065(12) 0.047(14) 0.015(6) -0.015(6) 0.036(15) C7 0.019(14) 0.017(9) 0.06(2) 0.000 0.000 0.010(7) C8 0.022(9) 0.031(8) 0.046(12) 0.001(4) 0.001(8) 0.011(5) C9 0.039(15) 0.039(15) 0.039(15) 0.000(12) 0.000(13) 0.020(12) C10 0.04(3) 0.04(3) 0.04(2) 0.000 0.000 0.02(2) C11 0.054(11) 0.054(11) 0.056(14) -0.003(5) 0.003(5) 0.036(12) C12 0.09(3) 0.09(3) 0.09(4) 0.000 0.000 0.047(13) _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 O3 2.320(14) . ? Pb1 O1 2.357(9) 24 ? Pb1 O1 2.357(9) . ? Pb1 O2 2.939(12) 24 ? Pb1 O2 2.939(12) . ? Pb1 C2 2.96(2) . ? Pb1 O4 2.967(15) . ? Pb1 C1 2.976(16) 24 ? Pb1 C1 2.976(16) . ? Pb1 O2 3.012(13) 15 ? Pb1 O2 3.012(13) 10 ? Pb1 Pb1 4.2817(11) 15 ? Cs1 O2 3.023(15) . ? Cs1 O2 3.023(15) 24 ? Cs1 O4 3.045(12) 8 ? Cs1 O4 3.045(12) 10 ? Cs1 O5 3.424(14) 1 ? O1 C1 1.235(19) . ? O2 C1 1.249(18) . ? O2 Pb1 3.012(13) 17 ? O3 C2 1.28(3) . ? O4 C2 1.21(3) . ? O5 O5 0.00(17) 1 ? N1 C12 1.49(7) . ? N1 C11 1.50(2) 5_665 ? N1 C11 1.50(2) 3_655 ? N1 C11 1.50(2) . ? C1 C4 1.52(2) . ? C2 C8 1.55(3) . ? C3 C4 1.384(18) . ? C3 C4 1.384(18) 22_665 ? C3 H3A 0.9300 . ? C4 C5 1.40(2) . ? C5 C6 1.42(2) . ? C5 H5A 0.9300 . ? C6 C5 1.42(2) 22_665 ? C6 H6A 0.9300 . ? C7 C8 1.36(3) 16_556 ? C7 C8 1.36(3) . ? C7 H7A 0.9300 . ? C8 C9 1.44(3) 24 ? C8 C9 1.44(3) . ? C9 C9 0.95(6) 24 ? C9 C10 1.38(4) . ? C9 C10 1.86(5) 9 ? C9 H9A 0.9800 . ? C10 C9 1.38(4) 16_556 ? C10 C10 1.61(9) 9 ? C10 C9 1.86(5) 9 ? C10 C9 1.86(5) 24 ? C10 H10A 0.9599 . ? C11 H11A 0.9600 . ? C11 H11C 0.9600 . ? C11 H11B 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 H12A 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 O3 Pb1 O1 82.8(4) . 24 ? O3 Pb1 O1 82.8(4) . . ? O1 Pb1 O1 75.7(5) 24 . ? O3 Pb1 O2 129.2(3) . 24 ? O1 Pb1 O2 47.7(3) 24 24 ? O1 Pb1 O2 93.1(3) . 24 ? O3 Pb1 O2 129.2(3) . . ? O1 Pb1 O2 93.1(3) 24 . ? O1 Pb1 O2 47.7(3) . . ? O2 Pb1 O2 72.7(5) 24 . ? O3 Pb1 C2 24.3(6) . . ? O1 Pb1 C2 101.9(4) 24 . ? O1 Pb1 C2 101.9(4) . . ? O2 Pb1 C2 141.4(3) 24 . ? O2 Pb1 C2 141.4(3) . . ? O3 Pb1 O4 47.9(5) . . ? O1 Pb1 O4 119.6(3) 24 . ? O1 Pb1 O4 119.6(3) . . ? O2 Pb1 O4 142.6(3) 24 . ? O2 Pb1 O4 142.6(3) . . ? C2 Pb1 O4 23.6(5) . . ? O3 Pb1 C1 105.7(4) . 24 ? O1 Pb1 C1 23.3(4) 24 24 ? O1 Pb1 C1 83.2(4) . 24 ? O2 Pb1 C1 24.4(3) 24 24 ? O2 Pb1 C1 82.1(4) . 24 ? C2 Pb1 C1 122.5(4) . 24 ? O4 Pb1 C1 135.0(3) . 24 ? O3 Pb1 C1 105.7(4) . . ? O1 Pb1 C1 83.2(4) 24 . ? O1 Pb1 C1 23.3(4) . . ? O2 Pb1 C1 82.1(4) 24 . ? O2 Pb1 C1 24.4(3) . . ? C2 Pb1 C1 122.5(4) . . ? O4 Pb1 C1 135.0(3) . . ? C1 Pb1 C1 81.4(5) 24 . ? O3 Pb1 O2 78.4(3) . 15 ? O1 Pb1 O2 70.3(3) 24 15 ? O1 Pb1 O2 142.8(3) . 15 ? O2 Pb1 O2 75.1(4) 24 15 ? O2 Pb1 O2 146.9(3) . 15 ? C2 Pb1 O2 71.5(2) . 15 ? O4 Pb1 O2 67.8(2) . 15 ? C1 Pb1 O2 71.6(3) 24 15 ? C1 Pb1 O2 152.7(3) . 15 ? O3 Pb1 O2 78.4(3) . 10 ? O1 Pb1 O2 142.8(3) 24 10 ? O1 Pb1 O2 70.3(3) . 10 ? O2 Pb1 O2 146.9(3) 24 10 ? O2 Pb1 O2 75.1(4) . 10 ? C2 Pb1 O2 71.5(2) . 10 ? O4 Pb1 O2 67.8(2) . 10 ? C1 Pb1 O2 152.7(3) 24 10 ? C1 Pb1 O2 71.6(3) . 10 ? O2 Pb1 O2 134.8(4) 15 10 ? O3 Pb1 Pb1 121.47(10) . 15 ? O1 Pb1 Pb1 74.2(2) 24 15 ? O1 Pb1 Pb1 137.8(2) . 15 ? O2 Pb1 Pb1 44.7(3) 24 15 ? O2 Pb1 Pb1 105.5(2) . 15 ? C2 Pb1 Pb1 112.77(19) . 15 ? O4 Pb1 Pb1 100.93(17) . 15 ? C1 Pb1 Pb1 58.3(3) 24 15 ? C1 Pb1 Pb1 123.4(3) . 15 ? O2 Pb1 Pb1 43.3(2) 15 15 ? O2 Pb1 Pb1 142.74(19) 10 15 ? O2 Cs1 O2 70.4(6) . 24 ? O2 Cs1 O4 136.3(6) . 8 ? O2 Cs1 O4 66.7(4) 24 8 ? O2 Cs1 O4 66.7(4) . 10 ? O2 Cs1 O4 136.3(6) 24 10 ? O4 Cs1 O4 152.3(6) 8 10 ? O2 Cs1 O5 126.1(12) . 1 ? O2 Cs1 O5 159.0(8) 24 1 ? O4 Cs1 O5 97.5(13) 8 1 ? O4 Cs1 O5 63.3(11) 10 1 ? C1 O1 Pb1 107.7(9) . . ? C1 O2 Pb1 79.5(9) . . ? C1 O2 Pb1 114.8(10) . 17 ? Pb1 O2 Pb1 92.0(3) . 17 ? C1 O2 Cs1 148.3(11) . . ? Pb1 O2 Cs1 94.7(4) . . ? Pb1 O2 Cs1 96.4(3) 17 . ? C2 O3 Pb1 107.3(13) . . ? C2 O4 Pb1 78.0(12) . . ? C12 N1 C11 109.0(15) . 5_665 ? C12 N1 C11 109.0(15) . 3_655 ? C11 N1 C11 109.9(14) 5_665 3_655 ? C12 N1 C11 109.0(15) . . ? C11 N1 C11 109.9(14) 5_665 . ? C11 N1 C11 109.9(14) 3_655 . ? O1 C1 O2 125.1(14) . . ? O1 C1 C4 115.8(13) . . ? O2 C1 C4 119.1(14) . . ? O1 C1 Pb1 49.0(7) . . ? O2 C1 Pb1 76.2(9) . . ? C4 C1 Pb1 164.7(10) . . ? O4 C2 O3 126.8(19) . . ? O4 C2 C8 118.9(17) . . ? O3 C2 C8 114.3(18) . . ? O4 C2 Pb1 78.4(11) . . ? O3 C2 Pb1 48.4(10) . . ? C8 C2 Pb1 162.7(14) . . ? C4 C3 C4 121(2) . 22_665 ? C4 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 22_665 . ? C3 C4 C5 120.3(15) . . ? C3 C4 C1 119.9(14) . . ? C5 C4 C1 119.8(13) . . ? C4 C5 C6 118.9(16) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C5 C6 C5 120(2) 22_665 . ? C5 C6 H6A 120.1 22_665 . ? C5 C6 H6A 120.1 . . ? C8 C7 C8 122(3) 16_556 . ? C8 C7 H7A 119.1 16_556 . ? C8 C7 H7A 119.1 . . ? C7 C8 C9 117(2) . 24 ? C7 C8 C9 117(2) . . ? C9 C8 C9 38(2) 24 . ? C7 C8 C2 122.9(18) . . ? C9 C8 C2 117(2) 24 . ? C9 C8 C2 117(2) . . ? C9 C9 C10 104(2) 24 . ? C9 C9 C8 70.8(12) 24 . ? C10 C9 C8 122(3) . . ? C9 C9 C10 46.3(14) 24 9 ? C10 C9 C10 58(3) . 9 ? C8 C9 C10 96(2) . 9 ? C9 C9 H9A 116.5 24 . ? C10 C9 H9A 116.5 . . ? C8 C9 H9A 116.5 . . ? C10 C9 H9A 136.0 9 . ? C9 C10 C9 116(4) . 16_556 ? C9 C10 C10 76(2) . 9 ? C9 C10 C10 76(2) 16_556 9 ? C9 C10 C9 102(3) . 9 ? C9 C10 C9 30(2) 16_556 9 ? C10 C10 C9 46.3(14) 9 9 ? C9 C10 C9 30(2) . 24 ? C9 C10 C9 102(3) 16_556 24 ? C10 C10 C9 46.3(14) 9 24 ? C9 C10 C9 78(3) 9 24 ? C9 C10 H10A 122.1 . . ? C9 C10 H10A 122.1 16_556 . ? C10 C10 H10A 118.7 9 . ? C9 C10 H10A 129.9 9 . ? C9 C10 H10A 129.9 24 . ? N1 C11 H11A 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? H11C C11 H11B 109.5 . . ? N1 C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.327 _refine_diff_density_min -2.058 _refine_diff_density_rms 0.311 #===END data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 835035' #TrackingRef '- Cif date.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 K2 O16 Pb S2' _chemical_formula_weight 965.98 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' K K 0.2009 0.2494 '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 p_m_m_n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z' 'x, -y-1/2, z' _cell_length_a 13.5107(16) _cell_length_b 23.380(3) _cell_length_c 5.8727(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1855.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4596 _cell_measurement_theta_min 2.3030 _cell_measurement_theta_max 27.4817 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 4.951 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6613 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11399 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 25.49 _reflns_number_total 1834 _reflns_number_gt 1547 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1347P)^2^+0.2159P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1834 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.2034 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 -0.2500 0.7500 0.66987(17) 0.0347(4) Uani 0.6100(10) 4 d SP . . Pb2 Pb -0.2500 0.7500 0.5025(3) 0.0347(4) Uani 0.3900(10) 4 d SP . . K1 K -0.2500 0.87312(10) 1.0918(4) 0.0369(6) Uani 1 2 d S . . S1 S 0.2500 1.00589(10) 0.3873(4) 0.0302(6) Uani 1 2 d S . . O1 O -0.1280(4) 0.8209(3) 0.4090(9) 0.0466(14) Uani 1 1 d . . . O2 O -0.1189(4) 0.8408(3) 0.7748(10) 0.0539(15) Uani 1 1 d . . . O3 O 0.2500 1.0193(3) 0.1464(11) 0.0397(17) Uani 1 2 d S . . O4 O 0.2500 1.0509(3) 0.5537(13) 0.0420(18) Uani 1 2 d S . . O5 O -0.2500 0.7500 0.0907(19) 0.050(3) Uiso 1 4 d S . . O6W O 0.2500 0.6501(15) -0.093(5) 0.121(11) Uani 0.50 2 d SP . . O7W O -0.4202(6) 0.7500 0.0463(13) 0.050(2) Uiso 1 2 d S . . H1A H -0.4583 0.7803 0.0108 0.060 Uiso 0.50 1 d PR . . H1B H -0.4176 0.7197 -0.0480 0.060 Uiso 0.50 1 d PR . . C1 C -0.0935(6) 0.8474(3) 0.5766(13) 0.0360(17) Uani 1 1 d . . . C2 C -0.0106(5) 0.8889(3) 0.5278(12) 0.0325(15) Uani 1 1 d . . . C3 C 0.0219(6) 0.9266(3) 0.6916(11) 0.0361(16) Uani 1 1 d . . . H3 H -0.0096 0.9279 0.8323 0.043 Uiso 1 1 calc R . . C4 C 0.1014(6) 0.9628(3) 0.6488(12) 0.0384(17) Uani 1 1 d . . . H4 H 0.1235 0.9877 0.7610 0.046 Uiso 1 1 calc R . . C5 C 0.1465(5) 0.9615(3) 0.4420(11) 0.0306(15) Uani 1 1 d . . . C6 C 0.1151(6) 0.9244(3) 0.2691(13) 0.0385(17) Uani 1 1 d . . . H6 H 0.1470 0.9235 0.1288 0.046 Uiso 1 1 calc R . . C7 C 0.0350(6) 0.8892(4) 0.3138(12) 0.0414(18) Uani 1 1 d . . . H7 H 0.0111 0.8653 0.1998 0.050 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 0.0297(5) 0.0316(5) 0.0429(5) 0.000 0.000 0.000 Pb2 0.0297(5) 0.0316(5) 0.0429(5) 0.000 0.000 0.000 K1 0.0444(15) 0.0359(13) 0.0305(12) -0.0006(9) 0.000 0.000 S1 0.0358(14) 0.0231(12) 0.0317(13) 0.0021(9) 0.000 0.000 O1 0.043(4) 0.049(4) 0.047(4) -0.002(2) -0.002(2) -0.010(3) O2 0.053(4) 0.062(4) 0.047(3) 0.005(3) 0.008(3) -0.014(3) O3 0.053(5) 0.036(4) 0.030(4) 0.007(3) 0.000 0.000 O4 0.051(5) 0.027(4) 0.048(4) -0.010(3) 0.000 0.000 O6W 0.13(3) 0.09(2) 0.14(3) 0.035(16) 0.000 0.000 C1 0.029(4) 0.037(4) 0.042(4) 0.005(3) 0.001(3) 0.004(3) C2 0.032(4) 0.034(4) 0.032(4) 0.004(3) -0.003(3) 0.004(3) C3 0.035(4) 0.044(4) 0.029(4) 0.003(3) 0.006(3) -0.001(3) C4 0.044(5) 0.038(4) 0.034(4) -0.008(3) -0.004(3) 0.000(3) C5 0.031(4) 0.029(3) 0.032(4) 0.001(3) 0.002(3) 0.000(3) C6 0.045(4) 0.042(4) 0.029(4) -0.004(3) 0.006(3) -0.005(3) C7 0.044(5) 0.048(5) 0.033(4) -0.011(3) 0.001(3) -0.010(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 Pb2 0.9830(17) . ? Pb1 O5 2.471(11) 1_556 ? Pb1 O1 2.795(6) 2_465 ? Pb1 O1 2.795(6) 7 ? Pb1 O1 2.795(6) . ? Pb1 O1 2.795(6) 8_575 ? Pb1 O2 2.833(6) . ? Pb1 O2 2.833(6) 2_465 ? Pb1 O2 2.833(6) 7 ? Pb1 O2 2.833(6) 8_575 ? Pb1 K1 3.798(2) . ? Pb1 K1 3.798(2) 2_465 ? Pb2 O1 2.402(6) 2_465 ? Pb2 O1 2.402(6) . ? Pb2 O1 2.402(6) 7 ? Pb2 O1 2.402(6) 8_575 ? Pb2 O5 2.418(11) . ? Pb2 O2 3.194(6) . ? Pb2 O2 3.194(6) 2_465 ? Pb2 O2 3.194(6) 7 ? Pb2 O2 3.194(6) 8_575 ? Pb2 K1 3.755(2) 2_464 ? Pb2 K1 3.755(2) 1_554 ? K1 O2 2.679(6) 7 ? K1 O2 2.679(6) . ? K1 O4 2.736(7) 5_577 ? K1 O1 2.770(6) 1_556 ? K1 O1 2.770(6) 7_556 ? K1 O3 2.878(8) 5_576 ? K1 O5 2.879(2) 1_556 ? K1 Pb2 3.755(2) 1_556 ? S1 O4 1.437(7) . ? S1 O3 1.449(7) . ? S1 C5 1.771(7) 7_655 ? S1 C5 1.771(7) . ? O1 C1 1.253(9) . ? O1 K1 2.770(6) 1_554 ? O2 C1 1.223(9) . ? O3 K1 2.878(8) 5_576 ? O4 K1 2.736(7) 5_577 ? O5 Pb1 2.471(11) 1_554 ? O5 K1 2.879(2) 1_554 ? O5 K1 2.879(2) 2_464 ? O7W H1A 0.9000 . ? O7W H1B 0.9000 . ? C1 C2 1.510(11) . ? C2 C3 1.376(10) . ? C2 C7 1.399(10) . ? C3 C4 1.389(11) . ? C3 H3 0.9300 . ? C4 C5 1.359(10) . ? C4 H4 0.9300 . ? C5 C6 1.401(10) . ? C6 C7 1.385(11) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? 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 Pb2 Pb1 O5 180.000(12) . 1_556 ? Pb2 Pb1 O1 56.76(11) . 2_465 ? O5 Pb1 O1 123.24(11) 1_556 2_465 ? Pb2 Pb1 O1 56.76(11) . 7 ? O5 Pb1 O1 123.24(11) 1_556 7 ? O1 Pb1 O1 72.8(3) 2_465 7 ? Pb2 Pb1 O1 56.76(11) . . ? O5 Pb1 O1 123.24(11) 1_556 . ? O1 Pb1 O1 113.5(2) 2_465 . ? O1 Pb1 O1 72.2(2) 7 . ? Pb2 Pb1 O1 56.76(11) . 8_575 ? O5 Pb1 O1 123.24(11) 1_556 8_575 ? O1 Pb1 O1 72.2(2) 2_465 8_575 ? O1 Pb1 O1 113.5(2) 7 8_575 ? O1 Pb1 O1 72.8(3) . 8_575 ? Pb2 Pb1 O2 102.57(12) . . ? O5 Pb1 O2 77.43(12) 1_556 . ? O1 Pb1 O2 158.84(16) 2_465 . ? O1 Pb1 O2 92.48(19) 7 . ? O1 Pb1 O2 46.05(17) . . ? O1 Pb1 O2 101.26(19) 8_575 . ? Pb2 Pb1 O2 102.57(12) . 2_465 ? O5 Pb1 O2 77.43(12) 1_556 2_465 ? O1 Pb1 O2 46.05(17) 2_465 2_465 ? O1 Pb1 O2 101.26(19) 7 2_465 ? O1 Pb1 O2 158.84(16) . 2_465 ? O1 Pb1 O2 92.48(19) 8_575 2_465 ? O2 Pb1 O2 154.9(2) . 2_465 ? Pb2 Pb1 O2 102.57(12) . 7 ? O5 Pb1 O2 77.43(12) 1_556 7 ? O1 Pb1 O2 101.26(19) 2_465 7 ? O1 Pb1 O2 46.05(17) 7 7 ? O1 Pb1 O2 92.48(19) . 7 ? O1 Pb1 O2 158.84(16) 8_575 7 ? O2 Pb1 O2 77.4(3) . 7 ? O2 Pb1 O2 97.1(3) 2_465 7 ? Pb2 Pb1 O2 102.57(12) . 8_575 ? O5 Pb1 O2 77.43(12) 1_556 8_575 ? O1 Pb1 O2 92.48(19) 2_465 8_575 ? O1 Pb1 O2 158.84(16) 7 8_575 ? O1 Pb1 O2 101.26(19) . 8_575 ? O1 Pb1 O2 46.05(17) 8_575 8_575 ? O2 Pb1 O2 97.1(3) . 8_575 ? O2 Pb1 O2 77.4(3) 2_465 8_575 ? O2 Pb1 O2 154.9(2) 7 8_575 ? Pb2 Pb1 K1 130.72(4) . . ? O5 Pb1 K1 49.28(3) 1_556 . ? O1 Pb1 K1 143.83(12) 2_465 . ? O1 Pb1 K1 84.71(12) 7 . ? O1 Pb1 K1 84.71(12) . . ? O1 Pb1 K1 143.83(12) 8_575 . ? O2 Pb1 K1 44.77(13) . . ? O2 Pb1 K1 115.21(13) 2_465 . ? O2 Pb1 K1 44.77(13) 7 . ? O2 Pb1 K1 115.21(13) 8_575 . ? Pb2 Pb1 K1 130.72(4) . 2_465 ? O5 Pb1 K1 49.28(3) 1_556 2_465 ? O1 Pb1 K1 84.71(12) 2_465 2_465 ? O1 Pb1 K1 143.83(12) 7 2_465 ? O1 Pb1 K1 143.83(12) . 2_465 ? O1 Pb1 K1 84.71(12) 8_575 2_465 ? O2 Pb1 K1 115.21(13) . 2_465 ? O2 Pb1 K1 44.77(13) 2_465 2_465 ? O2 Pb1 K1 115.21(13) 7 2_465 ? O2 Pb1 K1 44.77(13) 8_575 2_465 ? K1 Pb1 K1 98.55(7) . 2_465 ? Pb1 Pb2 O1 103.21(13) . 2_465 ? Pb1 Pb2 O1 103.21(13) . . ? O1 Pb2 O1 153.6(3) 2_465 . ? Pb1 Pb2 O1 103.21(13) . 7 ? O1 Pb2 O1 87.4(3) 2_465 7 ? O1 Pb2 O1 86.6(3) . 7 ? Pb1 Pb2 O1 103.21(13) . 8_575 ? O1 Pb2 O1 86.6(3) 2_465 8_575 ? O1 Pb2 O1 87.4(3) . 8_575 ? O1 Pb2 O1 153.6(3) 7 8_575 ? Pb1 Pb2 O5 180.000(11) . . ? O1 Pb2 O5 76.79(13) 2_465 . ? O1 Pb2 O5 76.79(13) . . ? O1 Pb2 O5 76.79(13) 7 . ? O1 Pb2 O5 76.79(13) 8_575 . ? Pb1 Pb2 O2 59.95(11) . . ? O1 Pb2 O2 162.55(16) 2_465 . ? O1 Pb2 O2 43.52(17) . . ? O1 Pb2 O2 92.06(19) 7 . ? O1 Pb2 O2 101.12(19) 8_575 . ? O5 Pb2 O2 120.05(11) . . ? Pb1 Pb2 O2 59.95(11) . 2_465 ? O1 Pb2 O2 43.52(17) 2_465 2_465 ? O1 Pb2 O2 162.55(16) . 2_465 ? O1 Pb2 O2 101.12(19) 7 2_465 ? O1 Pb2 O2 92.06(19) 8_575 2_465 ? O5 Pb2 O2 120.05(11) . 2_465 ? O2 Pb2 O2 119.9(2) . 2_465 ? Pb1 Pb2 O2 59.95(11) . 7 ? O1 Pb2 O2 101.12(19) 2_465 7 ? O1 Pb2 O2 92.06(19) . 7 ? O1 Pb2 O2 43.52(17) 7 7 ? O1 Pb2 O2 162.55(16) 8_575 7 ? O5 Pb2 O2 120.05(11) . 7 ? O2 Pb2 O2 67.4(2) . 7 ? O2 Pb2 O2 83.3(2) 2_465 7 ? Pb1 Pb2 O2 59.95(11) . 8_575 ? O1 Pb2 O2 92.06(19) 2_465 8_575 ? O1 Pb2 O2 101.12(19) . 8_575 ? O1 Pb2 O2 162.55(16) 7 8_575 ? O1 Pb2 O2 43.52(17) 8_575 8_575 ? O5 Pb2 O2 120.05(11) . 8_575 ? O2 Pb2 O2 83.3(2) . 8_575 ? O2 Pb2 O2 67.4(2) 2_465 8_575 ? O2 Pb2 O2 119.9(2) 7 8_575 ? Pb1 Pb2 K1 129.96(4) . 2_464 ? O1 Pb2 K1 47.45(14) 2_465 2_464 ? O1 Pb2 K1 112.49(14) . 2_464 ? O1 Pb2 K1 112.49(14) 7 2_464 ? O1 Pb2 K1 47.45(14) 8_575 2_464 ? O5 Pb2 K1 50.04(4) . 2_464 ? O2 Pb2 K1 146.20(11) . 2_464 ? O2 Pb2 K1 79.17(11) 2_465 2_464 ? O2 Pb2 K1 146.20(11) 7 2_464 ? O2 Pb2 K1 79.17(11) 8_575 2_464 ? Pb1 Pb2 K1 129.96(4) . 1_554 ? O1 Pb2 K1 112.49(14) 2_465 1_554 ? O1 Pb2 K1 47.45(14) . 1_554 ? O1 Pb2 K1 47.45(14) 7 1_554 ? O1 Pb2 K1 112.49(14) 8_575 1_554 ? O5 Pb2 K1 50.04(4) . 1_554 ? O2 Pb2 K1 79.17(11) . 1_554 ? O2 Pb2 K1 146.20(11) 2_465 1_554 ? O2 Pb2 K1 79.17(11) 7 1_554 ? O2 Pb2 K1 146.20(11) 8_575 1_554 ? K1 Pb2 K1 100.09(8) 2_464 1_554 ? O2 K1 O2 82.8(3) 7 . ? O2 K1 O4 135.38(15) 7 5_577 ? O2 K1 O4 135.38(15) . 5_577 ? O2 K1 O1 137.4(2) 7 1_556 ? O2 K1 O1 87.12(19) . 1_556 ? O4 K1 O1 76.95(18) 5_577 1_556 ? O2 K1 O1 87.12(19) 7 7_556 ? O2 K1 O1 137.4(2) . 7_556 ? O4 K1 O1 76.95(18) 5_577 7_556 ? O1 K1 O1 73.0(2) 1_556 7_556 ? O2 K1 O3 84.76(18) 7 5_576 ? O2 K1 O3 84.76(18) . 5_576 ? O4 K1 O3 78.6(2) 5_577 5_576 ? O1 K1 O3 135.38(15) 1_556 5_576 ? O1 K1 O3 135.38(15) 7_556 5_576 ? O2 K1 O5 73.5(2) 7 1_556 ? O2 K1 O5 73.5(2) . 1_556 ? O4 K1 O5 130.6(3) 5_577 1_556 ? O1 K1 O5 64.0(2) 1_556 1_556 ? O1 K1 O5 64.0(2) 7_556 1_556 ? O3 K1 O5 150.8(3) 5_576 1_556 ? O2 K1 Pb2 103.31(15) 7 1_556 ? O2 K1 Pb2 103.31(15) . 1_556 ? O4 K1 Pb2 90.51(17) 5_577 1_556 ? O1 K1 Pb2 39.70(12) 1_556 1_556 ? O1 K1 Pb2 39.70(12) 7_556 1_556 ? O3 K1 Pb2 169.13(16) 5_576 1_556 ? O5 K1 Pb2 40.1(2) 1_556 1_556 ? O2 K1 Pb1 48.15(13) 7 . ? O2 K1 Pb1 48.15(13) . . ? O4 K1 Pb1 171.19(18) 5_577 . ? O1 K1 Pb1 96.02(13) 1_556 . ? O1 K1 Pb1 96.02(13) 7_556 . ? O3 K1 Pb1 110.19(16) 5_576 . ? O5 K1 Pb1 40.6(2) 1_556 . ? Pb2 K1 Pb1 80.68(5) 1_556 . ? O4 S1 O3 120.4(5) . . ? O4 S1 C5 107.8(3) . 7_655 ? O3 S1 C5 107.7(3) . 7_655 ? O4 S1 C5 107.8(3) . . ? O3 S1 C5 107.7(3) . . ? C5 S1 C5 104.3(5) 7_655 . ? C1 O1 Pb2 114.7(5) . . ? C1 O1 K1 122.1(5) . 1_554 ? Pb2 O1 K1 92.85(19) . 1_554 ? C1 O1 Pb1 94.7(4) . . ? Pb2 O1 Pb1 20.02(6) . . ? K1 O1 Pb1 106.21(19) 1_554 . ? C1 O2 K1 144.2(5) . . ? C1 O2 Pb1 93.6(5) . . ? K1 O2 Pb1 87.07(17) . . ? C1 O2 Pb2 76.3(5) . . ? K1 O2 Pb2 99.71(18) . . ? Pb1 O2 Pb2 17.48(5) . . ? S1 O3 K1 131.6(4) . 5_576 ? S1 O4 K1 173.3(5) . 5_577 ? Pb2 O5 Pb1 180.000(1) . 1_554 ? Pb2 O5 K1 89.9(2) . 1_554 ? Pb1 O5 K1 90.1(2) 1_554 1_554 ? Pb2 O5 K1 89.9(2) . 2_464 ? Pb1 O5 K1 90.1(2) 1_554 2_464 ? K1 O5 K1 179.7(4) 1_554 2_464 ? H1A O7W H1B 120.0 . . ? O2 C1 O1 125.5(8) . . ? O2 C1 C2 118.0(7) . . ? O1 C1 C2 116.4(6) . . ? C3 C2 C7 119.0(7) . . ? C3 C2 C1 121.0(7) . . ? C7 C2 C1 120.0(6) . . ? C2 C3 C4 120.6(7) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.7(7) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.7(7) . . ? C4 C5 S1 120.3(5) . . ? C6 C5 S1 118.1(5) . . ? C7 C6 C5 117.8(7) . . ? C7 C6 H6 121.1 . . ? C5 C6 H6 121.1 . . ? C6 C7 C2 121.1(7) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.587 _refine_diff_density_min -2.903 _refine_diff_density_rms 0.186 #===END data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 835036' #TrackingRef '- Cif date.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H38 Cs2 N2 O20 Pb2 S3' _chemical_formula_weight 1739.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3401(5) _cell_length_b 25.0935(10) _cell_length_c 22.8740(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.895(4) _cell_angle_gamma 90.00 _cell_volume 6462.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14740 _cell_measurement_theta_min 2.0847 _cell_measurement_theta_max 27.5011 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 6.476 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6385 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48312 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14218 _reflns_number_gt 11538 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1434P)^2^+38.6233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14218 _refine_ls_number_parameters 689 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2345 _refine_ls_wR_factor_gt 0.2212 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 1.48840(4) 0.088190(16) 0.29503(2) 0.04572(15) Uani 1 1 d . . . Pb2 Pb 1.66105(3) 0.358550(14) -0.233330(16) 0.03811(14) Uani 1 1 d . . . Cs1 Cs 1.26847(7) 0.03819(3) 0.11361(3) 0.04868(19) Uani 1 1 d . . . Cs2 Cs 0.84871(8) 0.12056(4) 0.34958(4) 0.0672(3) Uani 1 1 d . . . S1 S 1.3940(7) 0.34343(16) 0.02171(18) 0.1022(19) Uani 1 1 d . . . S2 S 0.9557(2) -0.07865(9) 0.06553(11) 0.0395(5) Uani 1 1 d . . . S3 S 1.5478(2) 0.08429(9) -0.00456(10) 0.0348(5) Uani 1 1 d . . . O1 O 1.5386(9) 0.1557(4) 0.2265(4) 0.063(2) Uani 1 1 d . . . O2 O 1.3528(8) 0.1293(4) 0.1978(4) 0.060(2) Uani 1 1 d . . . O3 O 1.4241(8) 0.5653(4) 0.1875(5) 0.066(3) Uani 1 1 d . . . O4 O 1.2274(8) 0.5478(3) 0.1824(4) 0.0500(18) Uani 1 1 d . . . O5 O 1.511(2) 0.3492(5) 0.0007(7) 0.135(7) Uani 1 1 d . . . O6 O 1.285(2) 0.3367(5) -0.0175(6) 0.159(9) Uani 1 1 d . . . O7 O 1.1019(8) -0.3225(4) 0.1700(5) 0.063(2) Uani 1 1 d . . . O8 O 0.9072(8) -0.3351(3) 0.1465(4) 0.060(2) Uani 1 1 d . . . O9 O 0.6867(8) 0.0513(4) 0.2700(4) 0.063(2) Uani 1 1 d . . . O10 O 0.5306(8) 0.0264(4) 0.2065(5) 0.072(3) Uani 1 1 d . . . O11 O 1.0715(7) -0.0551(3) 0.0756(4) 0.0491(18) Uani 1 1 d . . . O12 O 0.8915(8) -0.0781(3) 0.0076(3) 0.0507(19) Uani 1 1 d . . . O13 O 1.5689(8) 0.3128(3) -0.1553(4) 0.0492(18) Uani 1 1 d . . . O14 O 1.6219(10) 0.2553(3) -0.2208(4) 0.064(2) Uani 1 1 d . . . O15 O 1.9541(7) 0.1437(3) 0.2222(4) 0.053(2) Uani 1 1 d . . . O16 O 2.0728(8) 0.1063(5) 0.1641(4) 0.077(3) Uani 1 1 d . . . O17 O 1.4429(7) 0.0894(3) 0.0240(3) 0.0421(16) Uani 1 1 d . . . O18 O 1.5704(7) 0.0366(3) -0.0358(3) 0.0430(16) Uani 1 1 d . . . O19 O 1.2278(7) -0.0542(3) 0.2043(4) 0.0500(18) Uiso 1 1 d . . . O20 O 0.0513(8) 0.3309(3) 0.0346(4) 0.0500(18) Uani 1 1 d . . . N1 N 1.3130(9) -0.1081(4) 0.2790(4) 0.050(2) Uani 1 1 d . . . N2 N -0.0953(9) 0.2715(4) 0.0265(4) 0.050(2) Uani 1 1 d . . . C1 C 1.4374(12) 0.1606(5) 0.1932(5) 0.051(3) Uani 1 1 d . . . C2 C 1.4237(11) 0.2058(5) 0.1504(5) 0.050(3) Uani 1 1 d . . . C3 C 1.5256(15) 0.2382(5) 0.1459(7) 0.070(4) Uani 1 1 d . . . H3A H 1.5972 0.2318 0.1691 0.084 Uiso 1 1 calc R . . C4 C 1.5136(19) 0.2802(6) 0.1049(8) 0.079(5) Uani 1 1 d . . . H4A H 1.5779 0.3020 0.0998 0.095 Uiso 1 1 calc R . . C5 C 1.4039(19) 0.2885(6) 0.0724(6) 0.076(5) Uani 1 1 d . . . C6 C 1.3068(18) 0.2590(6) 0.0757(7) 0.079(4) Uani 1 1 d . . . H6A H 1.2349 0.2664 0.0531 0.095 Uiso 1 1 calc R . . C7 C 1.3208(16) 0.2150(6) 0.1166(7) 0.074(4) Uani 1 1 d . . . H7A H 1.2567 0.1925 0.1196 0.088 Uiso 1 1 calc R . . C8 C 1.3750(19) 0.3998(5) 0.0679(6) 0.074(4) Uani 1 1 d . . . C9 C 1.476(2) 0.4232(7) 0.0929(9) 0.095(6) Uani 1 1 d . . . H9A H 1.5502 0.4101 0.0867 0.114 Uiso 1 1 calc R . . C10 C 1.4646(18) 0.4695(6) 0.1295(8) 0.084(5) Uani 1 1 d . . . H10A H 1.5311 0.4868 0.1485 0.101 Uiso 1 1 calc R . . C11 C 1.3491(12) 0.4874(4) 0.1352(7) 0.061(3) Uani 1 1 d . . . C12 C 1.255(2) 0.4631(8) 0.1054(12) 0.120(8) Uani 1 1 d . . . H12A H 1.1795 0.4764 0.1087 0.144 Uiso 1 1 calc R . . C13 C 1.266(2) 0.4170(7) 0.0683(9) 0.091(5) Uani 1 1 d . . . H13A H 1.2016 0.4009 0.0465 0.109 Uiso 1 1 calc R . . C14 C 1.3327(13) 0.5364(5) 0.1731(8) 0.068(4) Uani 1 1 d . . . C15 C 0.9984(10) -0.3074(4) 0.1495(5) 0.045(2) Uani 1 1 d . . . C16 C 0.9884(10) -0.2506(4) 0.1260(5) 0.043(2) Uani 1 1 d . . . C17 C 1.0790(11) -0.2153(4) 0.1439(6) 0.050(3) Uani 1 1 d . . . H17A H 1.1463 -0.2268 0.1679 0.060 Uiso 1 1 calc R . . C18 C 1.0683(11) -0.1610(5) 0.1251(6) 0.053(3) Uani 1 1 d . . . H18A H 1.1268 -0.1362 0.1379 0.064 Uiso 1 1 calc R . . C19 C 0.9706(9) -0.1463(4) 0.0882(5) 0.037(2) Uani 1 1 d . . . C20 C 0.8812(12) -0.1821(4) 0.0689(5) 0.051(3) Uani 1 1 d . . . H20A H 0.8162 -0.1714 0.0428 0.061 Uiso 1 1 calc R . . C21 C 0.8907(11) -0.2349(5) 0.0895(6) 0.053(3) Uani 1 1 d . . . H21A H 0.8303 -0.2592 0.0783 0.064 Uiso 1 1 calc R . . C22 C 0.8652(9) -0.0496(4) 0.1138(5) 0.039(2) Uani 1 1 d . . . C23 C 0.9212(10) -0.0282(4) 0.1679(5) 0.045(2) Uani 1 1 d . . . H23A H 0.9797 -0.0020 0.1591 0.054 Uiso 1 1 calc R . . H23B H 0.9634 -0.0566 0.1902 0.054 Uiso 1 1 calc R . . C24 C 0.8421(10) -0.0034(4) 0.2041(5) 0.043(2) Uani 1 1 d . . . H24A H 0.8727 0.0116 0.2399 0.052 Uiso 1 1 calc R . . C25 C 0.7206(9) -0.0015(4) 0.1868(5) 0.038(2) Uani 1 1 d . . . C26 C 0.6732(11) -0.0229(5) 0.1341(6) 0.053(3) Uani 1 1 d . . . H26A H 0.5918 -0.0203 0.1227 0.063 Uiso 1 1 calc R . . C27 C 0.7441(10) -0.0482(4) 0.0976(5) 0.045(2) Uani 1 1 d . . . H27A H 0.7108 -0.0641 0.0627 0.053 Uiso 1 1 calc R . . C28 C 0.6403(11) 0.0272(5) 0.2254(6) 0.053(3) Uani 1 1 d . . . C29 C 1.5859(10) 0.2653(4) -0.1732(5) 0.043(2) Uani 1 1 d . . . C30 C 1.5687(9) 0.2208(4) -0.1317(5) 0.039(2) Uani 1 1 d . . . C31 C 1.6052(12) 0.1698(4) -0.1462(5) 0.052(3) Uani 1 1 d . . . H31A H 1.6348 0.1638 -0.1818 0.063 Uiso 1 1 calc R . . C32 C 1.5969(12) 0.1287(4) -0.1073(5) 0.050(3) Uani 1 1 d . . . H32A H 1.6224 0.0948 -0.1162 0.060 Uiso 1 1 calc R . . C33 C 1.5503(9) 0.1377(3) -0.0545(4) 0.0341(19) Uani 1 1 d . . . C34 C 1.5114(12) 0.1863(4) -0.0406(5) 0.049(3) Uani 1 1 d . . . H34A H 1.4789 0.1915 -0.0056 0.059 Uiso 1 1 calc R . . C35 C 1.5207(12) 0.2296(5) -0.0800(5) 0.051(3) Uani 1 1 d . . . H35A H 1.4946 0.2634 -0.0709 0.062 Uiso 1 1 calc R . . C36 C 1.6717(9) 0.0962(3) 0.0478(4) 0.0333(19) Uani 1 1 d . . . C37 C 1.7816(10) 0.0826(5) 0.0339(5) 0.046(2) Uani 1 1 d . . . H37A H 1.7902 0.0681 -0.0028 0.055 Uiso 1 1 calc R . . C38 C 1.8825(11) 0.0907(5) 0.0762(5) 0.049(3) Uani 1 1 d . . . H38A H 1.9583 0.0815 0.0682 0.058 Uiso 1 1 calc R . . C39 C 1.8635(10) 0.1132(4) 0.1304(4) 0.042(2) Uani 1 1 d . . . C40 C 1.7528(10) 0.1269(5) 0.1423(5) 0.046(2) Uani 1 1 d . . . H40A H 1.7433 0.1421 0.1785 0.055 Uiso 1 1 calc R . . C41 C 1.6524(10) 0.1184(4) 0.1009(4) 0.041(2) Uani 1 1 d . . . H41A H 1.5765 0.1274 0.1091 0.049 Uiso 1 1 calc R . . C42 C 1.9700(10) 0.1215(5) 0.1747(5) 0.048(2) Uani 1 1 d . . . C43 C 1.3118(11) -0.0671(5) 0.2409(5) 0.050(3) Uani 1 1 d . . . H52A H 1.3805 -0.0467 0.2423 0.060 Uiso 1 1 calc R . . C44 C 1.4207(11) -0.1247(5) 0.3130(5) 0.050(3) Uani 1 1 d . . . H44A H 1.4828 -0.0998 0.3077 0.075 Uiso 1 1 calc R . . H44B H 1.4425 -0.1594 0.3003 0.075 Uiso 1 1 calc R . . H44C H 1.4092 -0.1261 0.3539 0.075 Uiso 1 1 calc R . . C45 C 1.2100(11) -0.1395(5) 0.2806(5) 0.050(3) Uani 1 1 d . . . H45A H 1.1449 -0.1237 0.2559 0.075 Uiso 1 1 calc R . . H45B H 1.1909 -0.1414 0.3203 0.075 Uiso 1 1 calc R . . H45C H 1.2242 -0.1747 0.2667 0.075 Uiso 1 1 calc R . . C46 C -0.1967(11) 0.2388(5) 0.0155(5) 0.050(3) Uani 1 1 d . . . H46A H -0.2503 0.2539 -0.0158 0.075 Uiso 1 1 calc R . . H46B H -0.2355 0.2364 0.0505 0.075 Uiso 1 1 calc R . . H46C H -0.1733 0.2038 0.0044 0.075 Uiso 1 1 calc R . . C47 C -0.0235(11) 0.2371(5) 0.0796(5) 0.050(3) Uani 1 1 d . . . H47A H 0.0504 0.2544 0.0927 0.075 Uiso 1 1 calc R . . H47B H -0.0081 0.2020 0.0657 0.075 Uiso 1 1 calc R . . H47C H -0.0704 0.2346 0.1117 0.075 Uiso 1 1 calc R . . C48 C -0.0411(11) 0.3115(5) 0.0163(5) 0.050(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0404(3) 0.0390(2) 0.0590(3) -0.00970(16) 0.0108(2) 0.00119(15) Pb2 0.0369(3) 0.0355(2) 0.0422(2) 0.00684(13) 0.00592(17) -0.00029(14) Cs1 0.0506(4) 0.0392(3) 0.0574(4) -0.0103(3) 0.0111(3) -0.0012(3) Cs2 0.0477(5) 0.0761(6) 0.0796(6) -0.0333(4) 0.0152(4) -0.0130(4) S1 0.201(6) 0.0488(19) 0.056(2) -0.0100(16) 0.011(3) 0.008(3) S2 0.0444(15) 0.0331(10) 0.0433(12) 0.0026(9) 0.0152(11) 0.0046(10) S3 0.0382(13) 0.0293(10) 0.0369(11) 0.0019(8) 0.0049(9) -0.0036(9) O1 0.058(6) 0.062(5) 0.072(6) -0.009(5) 0.022(5) -0.006(4) O2 0.057(6) 0.056(5) 0.069(5) -0.014(4) 0.018(4) -0.016(4) O3 0.050(5) 0.051(5) 0.099(7) -0.019(5) 0.020(5) -0.005(4) O4 0.050(5) 0.050(4) 0.050(4) 0.000(3) 0.006(4) 0.000(4) O5 0.25(2) 0.073(8) 0.106(10) -0.009(7) 0.097(13) 0.017(10) O6 0.33(3) 0.052(6) 0.075(8) -0.012(6) -0.060(12) 0.006(10) O7 0.048(5) 0.053(5) 0.085(6) 0.027(4) 0.001(4) 0.004(4) O8 0.060(6) 0.045(4) 0.071(5) 0.018(4) -0.001(4) -0.015(4) O9 0.055(5) 0.064(5) 0.071(6) -0.039(5) 0.009(4) 0.000(4) O10 0.038(5) 0.084(7) 0.095(7) -0.050(6) 0.009(5) 0.002(4) O11 0.046(5) 0.040(4) 0.065(5) 0.003(3) 0.021(4) -0.004(3) O12 0.062(5) 0.049(4) 0.042(4) 0.007(3) 0.010(4) 0.011(4) O13 0.064(5) 0.029(3) 0.057(4) 0.009(3) 0.019(4) 0.008(3) O14 0.099(7) 0.045(4) 0.052(5) 0.011(4) 0.025(5) 0.007(4) O15 0.039(5) 0.068(5) 0.051(4) -0.022(4) -0.002(3) 0.012(4) O16 0.038(5) 0.133(9) 0.059(5) -0.031(6) -0.004(4) 0.015(5) O17 0.034(4) 0.046(4) 0.048(4) 0.002(3) 0.011(3) -0.008(3) O18 0.051(5) 0.026(3) 0.052(4) -0.004(3) 0.005(3) -0.005(3) O20 0.050(5) 0.050(4) 0.050(4) 0.000(3) 0.006(4) 0.000(4) N1 0.050(6) 0.050(5) 0.050(5) 0.000(4) 0.006(4) 0.000(4) N2 0.050(6) 0.050(5) 0.050(5) 0.000(4) 0.006(4) 0.000(4) C1 0.052(7) 0.048(6) 0.053(6) -0.015(5) 0.014(5) 0.000(5) C2 0.049(7) 0.048(6) 0.055(6) -0.008(5) 0.016(5) -0.001(5) C3 0.074(10) 0.052(7) 0.086(10) 0.015(7) 0.016(8) -0.007(7) C4 0.112(14) 0.050(7) 0.079(10) -0.001(7) 0.027(10) -0.007(8) C5 0.125(15) 0.049(7) 0.055(7) -0.012(6) 0.018(9) -0.002(8) C6 0.096(13) 0.066(9) 0.072(9) -0.004(7) -0.003(9) 0.009(9) C7 0.081(11) 0.066(8) 0.075(9) -0.010(7) 0.013(8) -0.002(8) C8 0.116(14) 0.041(6) 0.060(8) -0.008(6) -0.004(8) 0.008(8) C9 0.126(17) 0.065(9) 0.094(12) -0.024(9) 0.020(12) 0.013(10) C10 0.102(13) 0.049(7) 0.102(12) -0.028(8) 0.015(10) 0.009(8) C11 0.053(8) 0.033(5) 0.093(9) -0.014(6) -0.010(7) 0.004(5) C12 0.112(17) 0.066(11) 0.18(3) -0.034(13) 0.018(16) -0.019(11) C13 0.099(15) 0.064(9) 0.108(14) -0.026(9) 0.006(11) -0.008(9) C14 0.056(9) 0.049(7) 0.098(11) -0.013(7) 0.013(8) -0.001(6) C15 0.037(6) 0.044(5) 0.054(6) 0.011(5) -0.002(5) -0.003(4) C16 0.039(6) 0.039(5) 0.051(6) 0.005(4) 0.008(5) 0.004(4) C17 0.039(6) 0.037(5) 0.073(7) 0.006(5) 0.002(5) -0.001(4) C18 0.043(7) 0.040(5) 0.075(8) 0.004(5) 0.001(6) 0.002(5) C19 0.032(5) 0.035(4) 0.045(5) -0.001(4) 0.007(4) 0.002(4) C20 0.056(7) 0.041(5) 0.056(6) 0.004(5) 0.007(5) 0.002(5) C21 0.048(7) 0.041(5) 0.067(7) 0.009(5) -0.006(6) -0.004(5) C22 0.037(6) 0.032(4) 0.046(5) 0.003(4) 0.005(4) 0.007(4) C23 0.039(6) 0.040(5) 0.056(6) -0.006(4) 0.005(5) 0.008(4) C24 0.046(6) 0.038(5) 0.046(5) -0.001(4) 0.009(5) 0.008(4) C25 0.034(5) 0.031(4) 0.050(5) -0.008(4) 0.006(4) 0.007(4) C26 0.046(7) 0.044(6) 0.069(7) -0.018(5) 0.014(6) 0.001(5) C27 0.037(6) 0.048(5) 0.048(5) -0.011(4) 0.003(4) 0.002(4) C28 0.043(7) 0.050(6) 0.067(7) -0.024(5) 0.012(6) -0.002(5) C29 0.044(6) 0.033(5) 0.051(6) 0.012(4) 0.004(5) 0.002(4) C30 0.035(5) 0.033(4) 0.048(5) 0.006(4) 0.003(4) 0.000(4) C31 0.081(9) 0.036(5) 0.044(5) 0.003(4) 0.026(6) 0.002(5) C32 0.074(8) 0.031(4) 0.049(6) 0.005(4) 0.021(6) 0.010(5) C33 0.038(5) 0.030(4) 0.035(4) 0.005(3) 0.005(4) 0.004(4) C34 0.069(8) 0.036(5) 0.044(5) 0.005(4) 0.015(5) 0.011(5) C35 0.064(8) 0.044(5) 0.049(6) -0.002(5) 0.015(5) 0.017(5) C36 0.038(5) 0.028(4) 0.034(4) 0.003(3) 0.005(4) 0.002(3) C37 0.043(6) 0.058(6) 0.038(5) -0.009(4) 0.010(4) 0.010(5) C38 0.047(7) 0.065(7) 0.035(5) -0.010(4) 0.010(5) 0.008(5) C39 0.041(6) 0.049(5) 0.035(5) -0.011(4) 0.002(4) 0.005(4) C40 0.042(6) 0.054(6) 0.042(5) -0.012(5) 0.009(5) 0.013(5) C41 0.039(6) 0.042(5) 0.041(5) -0.006(4) 0.006(4) 0.009(4) C42 0.037(6) 0.060(7) 0.045(5) -0.005(5) -0.004(5) 0.007(5) C43 0.050(7) 0.050(6) 0.050(6) 0.000(5) 0.006(5) 0.000(5) C44 0.050(7) 0.050(6) 0.050(6) 0.000(5) 0.006(5) 0.000(5) C45 0.050(7) 0.050(6) 0.050(6) 0.000(5) 0.006(5) 0.000(5) C46 0.050(7) 0.050(6) 0.050(6) 0.000(5) 0.006(5) 0.000(5) C47 0.050(7) 0.050(6) 0.050(6) 0.000(5) 0.006(5) 0.000(5) C48 0.050(7) 0.050(6) 0.050(6) 0.000(5) 0.006(5) 0.000(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 O1 2.422(10) . ? Pb1 O8 2.553(8) 2_755 ? Pb1 O9 2.560(9) 1_655 ? Pb1 O7 2.627(8) 2_755 ? Pb1 O10 2.639(8) 1_655 ? Pb1 O2 2.748(11) . ? Pb1 O4 2.754(8) 2_745 ? Pb1 Cs2 4.2057(10) 1_655 ? Pb1 Cs1 4.7466(9) . ? Pb2 O3 2.435(9) 3_865 ? Pb2 O15 2.444(8) 4_565 ? Pb2 O13 2.460(7) . ? Pb2 O16 2.593(9) 4_565 ? Pb2 O14 2.651(8) . ? Pb2 O4 2.851(8) 3_865 ? Pb2 O2 2.851(9) 4_665 ? Pb2 O7 3.034(9) 3_855 ? Pb2 Cs2 4.2462(10) 4_665 ? Pb2 Cs1 4.6346(7) 4_665 ? Cs1 O2 3.066(9) . ? Cs1 O16 3.130(10) 1_455 ? Cs1 O19 3.181(8) . ? Cs1 O17 3.276(7) . ? Cs1 O11 3.280(8) . ? Cs1 O12 3.283(8) 3_755 ? Cs1 O18 3.287(7) 3_855 ? Cs1 O10 3.452(10) 1_655 ? Cs1 C43 3.919(12) . ? Cs1 Pb2 4.6346(8) 4_566 ? Cs2 O9 2.984(8) . ? Cs2 O13 3.018(8) 4_566 ? Cs2 O8 3.119(9) 2_655 ? Cs2 O3 3.132(9) 2_745 ? Cs2 O15 3.329(9) 1_455 ? Cs2 O6 3.385(17) 4_566 ? Cs2 O5 3.79(2) 4_566 ? Cs2 S1 4.012(4) 4_566 ? Cs2 Pb1 4.2057(10) 1_455 ? Cs2 Pb2 4.2461(9) 4_566 ? S1 O6 1.45(2) . ? S1 O5 1.470(19) . ? S1 C8 1.794(14) . ? S1 C5 1.796(16) . ? S1 Cs2 4.012(4) 4_665 ? S2 O12 1.433(8) . ? S2 O11 1.434(8) . ? S2 C22 1.753(10) . ? S2 C19 1.777(10) . ? S3 O17 1.430(7) . ? S3 O18 1.434(7) . ? S3 C36 1.759(10) . ? S3 C33 1.764(9) . ? O1 C1 1.304(16) . ? O2 C1 1.255(15) . ? O3 C14 1.275(17) . ? O3 Pb2 2.435(9) 3_865 ? O3 Cs2 3.132(9) 2_755 ? O4 C14 1.270(16) . ? O4 Pb1 2.754(8) 2_755 ? O5 Cs2 3.79(2) 4_665 ? O6 Cs2 3.385(17) 4_665 ? O7 C15 1.269(14) . ? O7 Pb1 2.627(8) 2_745 ? O8 C15 1.241(13) . ? O8 Pb1 2.553(8) 2_745 ? O8 Cs2 3.119(9) 2_645 ? O9 C28 1.247(14) . ? O9 Pb1 2.560(9) 1_455 ? O10 C28 1.268(15) . ? O10 Pb1 2.639(8) 1_455 ? O10 Cs1 3.452(10) 1_455 ? O12 Cs1 3.283(8) 3_755 ? O13 C29 1.281(13) . ? O13 Cs2 3.018(8) 4_665 ? O14 C29 1.236(14) . ? O15 C42 1.255(13) . ? O15 Pb2 2.444(8) 4_666 ? O15 Cs2 3.329(9) 1_655 ? O16 C42 1.276(14) . ? O16 Pb2 2.593(9) 4_666 ? O16 Cs1 3.130(10) 1_655 ? O18 Cs1 3.287(7) 3_855 ? O19 C43 1.234(14) . ? O20 C48 1.185(14) . ? N1 C43 1.347(15) . ? N1 C45 1.413(15) . ? N1 C44 1.429(16) . ? N2 C48 1.214(15) . ? N2 C46 1.410(15) . ? N2 C47 1.627(15) . ? C1 C2 1.494(18) . ? C2 C7 1.34(2) . ? C2 C3 1.427(19) . ? C3 C4 1.41(2) . ? C3 H3A 0.9300 . ? C4 C5 1.39(3) . ? C4 H4A 0.9300 . ? C5 C6 1.34(3) . ? C6 C7 1.44(2) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.30(3) . ? C8 C9 1.35(3) . ? C9 C10 1.45(2) . ? C9 H9A 0.9300 . ? C10 C11 1.41(2) . ? C10 H10A 0.9300 . ? C11 C12 1.34(3) . ? C11 C14 1.527(18) . ? C12 C13 1.45(3) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C15 C16 1.524(14) . ? C16 C21 1.362(16) . ? C16 C17 1.380(16) . ? C17 C18 1.430(15) . ? C17 H17A 0.9300 . ? C18 C19 1.362(16) . ? C18 H18A 0.9300 . ? C19 C20 1.386(16) . ? C20 C21 1.406(15) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C27 1.379(15) . ? C22 C23 1.427(15) . ? C23 C24 1.434(14) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.388(16) . ? C24 H24A 0.9300 . ? C25 C26 1.367(16) . ? C25 C28 1.523(14) . ? C26 C27 1.383(15) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C29 C30 1.493(13) . ? C30 C35 1.379(15) . ? C30 C31 1.397(14) . ? C31 C32 1.372(14) . ? C31 H31A 0.9300 . ? C32 C33 1.392(14) . ? C32 H32A 0.9300 . ? C33 C34 1.348(13) . ? C34 C35 1.422(15) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 C37 1.367(14) . ? C36 C41 1.378(13) . ? C37 C38 1.422(17) . ? C37 H37A 0.9300 . ? C38 C39 1.402(13) . ? C38 H38A 0.9300 . ? C39 C40 1.360(15) . ? C39 C42 1.495(15) . ? C40 C41 1.406(16) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C43 H52A 0.9300 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 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 O1 Pb1 O8 71.4(3) . 2_755 ? O1 Pb1 O9 80.1(3) . 1_655 ? O8 Pb1 O9 91.4(3) 2_755 1_655 ? O1 Pb1 O7 74.4(3) . 2_755 ? O8 Pb1 O7 51.0(3) 2_755 2_755 ? O9 Pb1 O7 139.6(3) 1_655 2_755 ? O1 Pb1 O10 80.6(3) . 1_655 ? O8 Pb1 O10 136.8(3) 2_755 1_655 ? O9 Pb1 O10 51.0(3) 1_655 1_655 ? O7 Pb1 O10 147.9(4) 2_755 1_655 ? O1 Pb1 O2 50.6(3) . . ? O8 Pb1 O2 108.7(3) 2_755 . ? O9 Pb1 O2 112.1(3) 1_655 . ? O7 Pb1 O2 74.1(3) 2_755 . ? O10 Pb1 O2 74.6(3) 1_655 . ? O1 Pb1 O4 131.4(3) . 2_745 ? O8 Pb1 O4 123.1(3) 2_755 2_745 ? O9 Pb1 O4 137.1(3) 1_655 2_745 ? O7 Pb1 O4 82.5(3) 2_755 2_745 ? O10 Pb1 O4 100.1(3) 1_655 2_745 ? O2 Pb1 O4 82.3(3) . 2_745 ? O1 Pb1 Cs2 76.2(2) . 1_655 ? O8 Pb1 Cs2 47.61(19) 2_755 1_655 ? O9 Pb1 Cs2 44.59(18) 1_655 1_655 ? O7 Pb1 Cs2 98.35(19) 2_755 1_655 ? O10 Pb1 Cs2 94.7(2) 1_655 1_655 ? O2 Pb1 Cs2 126.65(18) . 1_655 ? O4 Pb1 Cs2 150.33(17) 2_745 1_655 ? O1 Pb1 Cs1 76.0(2) . . ? O8 Pb1 Cs1 145.0(2) 2_755 . ? O9 Pb1 Cs1 95.30(19) 1_655 . ? O7 Pb1 Cs1 108.0(2) 2_755 . ? O10 Pb1 Cs1 45.4(2) 1_655 . ? O2 Pb1 Cs1 37.57(18) . . ? O4 Pb1 Cs1 71.41(17) 2_745 . ? Cs2 Pb1 Cs1 134.446(18) 1_655 . ? O3 Pb2 O15 77.7(3) 3_865 4_565 ? O3 Pb2 O13 80.2(3) 3_865 . ? O15 Pb2 O13 79.7(3) 4_565 . ? O3 Pb2 O16 89.6(4) 3_865 4_565 ? O15 Pb2 O16 52.0(3) 4_565 4_565 ? O13 Pb2 O16 131.6(3) . 4_565 ? O3 Pb2 O14 129.9(3) 3_865 . ? O15 Pb2 O14 81.8(3) 4_565 . ? O13 Pb2 O14 51.2(3) . . ? O16 Pb2 O14 112.2(4) 4_565 . ? O3 Pb2 O4 49.9(3) 3_865 3_865 ? O15 Pb2 O4 123.1(3) 4_565 3_865 ? O13 Pb2 O4 107.1(3) . 3_865 ? O16 Pb2 O4 101.2(3) 4_565 3_865 ? O14 Pb2 O4 146.5(3) . 3_865 ? O3 Pb2 O2 121.4(3) 3_865 4_665 ? O15 Pb2 O2 122.1(3) 4_565 4_665 ? O13 Pb2 O2 150.5(2) . 4_665 ? O16 Pb2 O2 72.6(3) 4_565 4_665 ? O14 Pb2 O2 108.2(3) . 4_665 ? O4 Pb2 O2 78.9(3) 3_865 4_665 ? O3 Pb2 O7 113.8(3) 3_865 3_855 ? O15 Pb2 O7 160.6(2) 4_565 3_855 ? O13 Pb2 O7 86.8(3) . 3_855 ? O16 Pb2 O7 139.2(3) 4_565 3_855 ? O14 Pb2 O7 78.9(3) . 3_855 ? O4 Pb2 O7 74.1(2) 3_865 3_855 ? O2 Pb2 O7 66.7(3) 4_665 3_855 ? O3 Pb2 Cs2 46.8(2) 3_865 4_665 ? O15 Pb2 Cs2 51.5(2) 4_565 4_665 ? O13 Pb2 Cs2 44.23(18) . 4_665 ? O16 Pb2 Cs2 96.3(2) 4_565 4_665 ? O14 Pb2 Cs2 85.0(2) . 4_665 ? O4 Pb2 Cs2 93.94(17) 3_865 4_665 ? O2 Pb2 Cs2 165.05(17) 4_665 4_665 ? O7 Pb2 Cs2 124.22(19) 3_855 4_665 ? O3 Pb2 Cs1 92.3(3) 3_865 4_665 ? O15 Pb2 Cs1 91.45(17) 4_565 4_665 ? O13 Pb2 Cs1 169.35(18) . 4_665 ? O16 Pb2 Cs1 40.0(2) 4_565 4_665 ? O14 Pb2 Cs1 133.68(18) . 4_665 ? O4 Pb2 Cs1 72.77(16) 3_865 4_665 ? O2 Pb2 Cs1 40.13(17) 4_665 4_665 ? O7 Pb2 Cs1 103.23(17) 3_855 4_665 ? Cs2 Pb2 Cs1 125.266(16) 4_665 4_665 ? O2 Cs1 O16 62.8(3) . 1_455 ? O2 Cs1 O19 101.1(2) . . ? O16 Cs1 O19 89.6(3) 1_455 . ? O2 Cs1 O17 86.2(2) . . ? O16 Cs1 O17 121.6(3) 1_455 . ? O19 Cs1 O17 147.1(2) . . ? O2 Cs1 O11 148.2(2) . . ? O16 Cs1 O11 89.8(3) 1_455 . ? O19 Cs1 O11 60.4(2) . . ? O17 Cs1 O11 123.83(19) . . ? O2 Cs1 O12 113.7(2) . 3_755 ? O16 Cs1 O12 78.5(2) 1_455 3_755 ? O19 Cs1 O12 131.6(2) . 3_755 ? O17 Cs1 O12 70.5(2) . 3_755 ? O11 Cs1 O12 72.8(2) . 3_755 ? O2 Cs1 O18 127.8(2) . 3_855 ? O16 Cs1 O18 167.5(2) 1_455 3_855 ? O19 Cs1 O18 94.05(19) . 3_855 ? O17 Cs1 O18 57.89(17) . 3_855 ? O11 Cs1 O18 81.63(18) . 3_855 ? O12 Cs1 O18 90.20(19) 3_755 3_855 ? O2 Cs1 O10 59.8(2) . 1_655 ? O16 Cs1 O10 114.6(2) 1_455 1_655 ? O19 Cs1 O10 73.6(3) . 1_655 ? O17 Cs1 O10 83.0(2) . 1_655 ? O11 Cs1 O10 127.7(2) . 1_655 ? O12 Cs1 O10 153.3(2) 3_755 1_655 ? O18 Cs1 O10 77.92(19) 3_855 1_655 ? O2 Cs1 C43 92.0(3) . . ? O16 Cs1 C43 97.2(3) 1_455 . ? O19 Cs1 C43 16.1(2) . . ? O17 Cs1 C43 134.2(2) . . ? O11 Cs1 C43 74.7(2) . . ? O12 Cs1 C43 147.2(2) 3_755 . ? O18 Cs1 C43 89.4(2) 3_855 . ? O10 Cs1 C43 57.5(3) 1_655 . ? O2 Cs1 Pb2 36.82(17) . 4_566 ? O16 Cs1 Pb2 32.19(17) 1_455 4_566 ? O19 Cs1 Pb2 80.97(14) . 4_566 ? O17 Cs1 Pb2 119.12(13) . 4_566 ? O11 Cs1 Pb2 111.53(14) . 4_566 ? O12 Cs1 Pb2 107.40(14) 3_755 4_566 ? O18 Cs1 Pb2 160.32(14) 3_855 4_566 ? O10 Cs1 Pb2 82.41(14) 1_655 4_566 ? C43 Cs1 Pb2 80.59(17) . 4_566 ? O2 Cs1 Pb1 33.1(2) . . ? O16 Cs1 Pb1 81.64(17) 1_455 . ? O19 Cs1 Pb1 74.02(15) . . ? O17 Cs1 Pb1 98.63(13) . . ? O11 Cs1 Pb1 133.65(15) . . ? O12 Cs1 Pb1 146.84(14) 3_755 . ? O18 Cs1 Pb1 110.86(14) 3_855 . ? O10 Cs1 Pb1 33.01(14) 1_655 . ? C43 Cs1 Pb1 61.50(18) . . ? Pb2 Cs1 Pb1 49.454(10) 4_566 . ? O9 Cs2 O13 138.7(2) . 4_566 ? O9 Cs2 O8 73.7(2) . 2_655 ? O13 Cs2 O8 125.4(2) 4_566 2_655 ? O9 Cs2 O3 92.4(3) . 2_745 ? O13 Cs2 O3 61.6(2) 4_566 2_745 ? O8 Cs2 O3 164.6(3) 2_655 2_745 ? O9 Cs2 O15 80.0(2) . 1_455 ? O13 Cs2 O15 59.1(2) 4_566 1_455 ? O8 Cs2 O15 113.3(2) 2_655 1_455 ? O3 Cs2 O15 56.4(2) 2_745 1_455 ? O9 Cs2 O6 123.3(4) . 4_566 ? O13 Cs2 O6 97.2(4) 4_566 4_566 ? O8 Cs2 O6 63.9(4) 2_655 4_566 ? O3 Cs2 O6 131.0(4) 2_745 4_566 ? O15 Cs2 O6 150.4(3) 1_455 4_566 ? O9 Cs2 O5 150.3(3) . 4_566 ? O13 Cs2 O5 67.0(3) 4_566 4_566 ? O8 Cs2 O5 104.6(3) 2_655 4_566 ? O3 Cs2 O5 90.7(4) 2_745 4_566 ? O15 Cs2 O5 125.2(3) 1_455 4_566 ? O6 Cs2 O5 41.5(5) 4_566 4_566 ? O9 Cs2 S1 136.6(2) . 4_566 ? O13 Cs2 S1 84.39(18) 4_566 4_566 ? O8 Cs2 S1 84.3(2) 2_655 4_566 ? O3 Cs2 S1 110.7(2) 2_745 4_566 ? O15 Cs2 S1 143.34(17) 1_455 4_566 ? O6 Cs2 S1 20.4(4) 4_566 4_566 ? O5 Cs2 S1 21.5(3) 4_566 4_566 ? O9 Cs2 Pb1 37.03(16) . 1_455 ? O13 Cs2 Pb1 151.00(17) 4_566 1_455 ? O8 Cs2 Pb1 37.20(15) 2_655 1_455 ? O3 Cs2 Pb1 129.5(2) 2_745 1_455 ? O15 Cs2 Pb1 102.24(14) 1_455 1_455 ? O6 Cs2 Pb1 91.2(4) 4_566 1_455 ? O5 Cs2 Pb1 131.0(3) 4_566 1_455 ? S1 Cs2 Pb1 109.87(11) 4_566 1_455 ? O9 Cs2 Pb2 106.54(17) . 4_566 ? O13 Cs2 Pb2 34.63(14) 4_566 4_566 ? O8 Cs2 Pb2 142.91(19) 2_655 4_566 ? O3 Cs2 Pb2 34.53(16) 2_745 4_566 ? O15 Cs2 Pb2 35.07(14) 1_455 4_566 ? O6 Cs2 Pb2 130.0(4) 4_566 4_566 ? O5 Cs2 Pb2 92.5(3) 4_566 4_566 ? S1 Cs2 Pb2 113.28(11) 4_566 4_566 ? Pb1 Cs2 Pb2 136.40(3) 1_455 4_566 ? O6 S1 O5 123.1(12) . . ? O6 S1 C8 107.5(10) . . ? O5 S1 C8 107.0(9) . . ? O6 S1 C5 107.0(10) . . ? O5 S1 C5 107.3(10) . . ? C8 S1 C5 103.2(7) . . ? O6 S1 Cs2 54.6(8) . 4_665 ? O5 S1 Cs2 70.8(8) . 4_665 ? C8 S1 Cs2 113.0(5) . 4_665 ? C5 S1 Cs2 142.8(5) . 4_665 ? O12 S2 O11 119.8(5) . . ? O12 S2 C22 107.9(5) . . ? O11 S2 C22 108.8(5) . . ? O12 S2 C19 107.4(5) . . ? O11 S2 C19 107.1(5) . . ? C22 S2 C19 104.8(5) . . ? O17 S3 O18 120.7(4) . . ? O17 S3 C36 108.3(5) . . ? O18 S3 C36 107.8(5) . . ? O17 S3 C33 107.9(5) . . ? O18 S3 C33 107.1(4) . . ? C36 S3 C33 103.8(5) . . ? C1 O1 Pb1 100.7(7) . . ? C1 O2 Pb1 86.8(8) . . ? C1 O2 Cs1 126.8(7) . . ? Pb1 O2 Cs1 109.3(3) . . ? C14 O3 Pb2 101.9(8) . 3_865 ? C14 O3 Cs2 148.3(10) . 2_755 ? Pb2 O3 Cs2 98.6(3) 3_865 2_755 ? C14 O4 Pb1 171.3(8) . 2_755 ? S1 O5 Cs2 87.8(9) . 4_665 ? S1 O6 Cs2 105.0(11) . 4_665 ? C15 O7 Pb1 89.5(6) . 2_745 ? C15 O8 Pb1 93.5(7) . 2_745 ? C15 O8 Cs2 166.0(8) . 2_645 ? Pb1 O8 Cs2 95.2(2) 2_745 2_645 ? C28 O9 Pb1 93.6(7) . 1_455 ? C28 O9 Cs2 161.8(9) . . ? Pb1 O9 Cs2 98.4(2) 1_455 . ? C28 O10 Pb1 89.5(7) . 1_455 ? C28 O10 Cs1 161.1(10) . 1_455 ? Pb1 O10 Cs1 101.5(3) 1_455 1_455 ? S2 O11 Cs1 156.7(4) . . ? S2 O12 Cs1 162.2(5) . 3_755 ? C29 O13 Pb2 96.2(6) . . ? C29 O13 Cs2 133.1(7) . 4_665 ? Pb2 O13 Cs2 101.1(2) . 4_665 ? C29 O14 Pb2 88.4(6) . . ? C42 O15 Pb2 96.8(7) . 4_666 ? C42 O15 Cs2 141.8(8) . 1_655 ? Pb2 O15 Cs2 93.4(3) 4_666 1_655 ? C42 O16 Pb2 89.4(7) . 4_666 ? C42 O16 Cs1 159.5(9) . 1_655 ? Pb2 O16 Cs1 107.8(3) 4_666 1_655 ? S3 O17 Cs1 148.1(4) . . ? S3 O18 Cs1 153.0(4) . 3_855 ? C43 O19 Cs1 118.2(7) . . ? C43 N1 C45 119.9(10) . . ? C43 N1 C44 121.1(10) . . ? C45 N1 C44 118.6(10) . . ? C48 N2 C46 150.2(12) . . ? C48 N2 C47 111.3(10) . . ? C46 N2 C47 98.5(9) . . ? O2 C1 O1 121.3(12) . . ? O2 C1 C2 120.6(12) . . ? O1 C1 C2 118.0(11) . . ? C7 C2 C3 121.1(13) . . ? C7 C2 C1 121.7(12) . . ? C3 C2 C1 117.2(12) . . ? C4 C3 C2 117.4(16) . . ? C4 C3 H3A 121.3 . . ? C2 C3 H3A 121.3 . . ? C5 C4 C3 118.6(16) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? C6 C5 C4 125.4(15) . . ? C6 C5 S1 118.2(15) . . ? C4 C5 S1 116.4(14) . . ? C5 C6 C7 115.6(17) . . ? C5 C6 H6A 122.2 . . ? C7 C6 H6A 122.2 . . ? C2 C7 C6 121.8(16) . . ? C2 C7 H7A 119.1 . . ? C6 C7 H7A 119.1 . . ? C13 C8 C9 127.3(15) . . ? C13 C8 S1 116.3(14) . . ? C9 C8 S1 115.9(15) . . ? C8 C9 C10 117.6(19) . . ? C8 C9 H9A 121.2 . . ? C10 C9 H9A 121.2 . . ? C11 C10 C9 117.3(17) . . ? C11 C10 H10A 121.3 . . ? C9 C10 H10A 121.3 . . ? C12 C11 C10 120.1(15) . . ? C12 C11 C14 120.7(15) . . ? C10 C11 C14 119.2(12) . . ? C11 C12 C13 123(2) . . ? C11 C12 H12A 118.7 . . ? C13 C12 H12A 118.7 . . ? C8 C13 C12 114.6(18) . . ? C8 C13 H13A 122.7 . . ? C12 C13 H13A 122.7 . . ? O4 C14 O3 125.4(12) . . ? O4 C14 C11 117.2(12) . . ? O3 C14 C11 117.0(12) . . ? O8 C15 O7 125.5(10) . . ? O8 C15 C16 118.6(10) . . ? O7 C15 C16 115.9(9) . . ? C21 C16 C17 121.2(10) . . ? C21 C16 C15 120.5(10) . . ? C17 C16 C15 118.3(10) . . ? C16 C17 C18 119.3(11) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? C19 C18 C17 118.5(11) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? C18 C19 C20 122.1(10) . . ? C18 C19 S2 118.8(8) . . ? C20 C19 S2 119.1(8) . . ? C19 C20 C21 118.7(11) . . ? C19 C20 H20A 120.7 . . ? C21 C20 H20A 120.7 . . ? C16 C21 C20 120.1(11) . . ? C16 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C27 C22 C23 123.2(9) . . ? C27 C22 S2 118.7(8) . . ? C23 C22 S2 118.0(8) . . ? C22 C23 C24 114.8(10) . . ? C22 C23 H23A 108.6 . . ? C24 C23 H23A 108.6 . . ? C22 C23 H23B 108.6 . . ? C24 C23 H23B 108.6 . . ? H23A C23 H23B 107.5 . . ? C25 C24 C23 121.3(10) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C26 C25 C24 120.6(10) . . ? C26 C25 C28 119.8(10) . . ? C24 C25 C28 119.5(9) . . ? C25 C26 C27 121.1(12) . . ? C25 C26 H26A 119.5 . . ? C27 C26 H26A 119.5 . . ? C22 C27 C26 118.9(11) . . ? C22 C27 H27A 120.6 . . ? C26 C27 H27A 120.6 . . ? O9 C28 O10 125.9(11) . . ? O9 C28 C25 118.7(11) . . ? O10 C28 C25 115.2(10) . . ? O14 C29 O13 123.4(9) . . ? O14 C29 C30 119.3(9) . . ? O13 C29 C30 117.1(9) . . ? C35 C30 C31 120.6(9) . . ? C35 C30 C29 121.4(9) . . ? C31 C30 C29 118.0(9) . . ? C32 C31 C30 119.2(10) . . ? C32 C31 H31A 120.4 . . ? C30 C31 H31A 120.4 . . ? C31 C32 C33 120.2(9) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C34 C33 C32 121.4(9) . . ? C34 C33 S3 120.2(8) . . ? C32 C33 S3 118.4(7) . . ? C33 C34 C35 119.2(10) . . ? C33 C34 H34A 120.4 . . ? C35 C34 H34A 120.4 . . ? C30 C35 C34 119.3(10) . . ? C30 C35 H35A 120.4 . . ? C34 C35 H35A 120.4 . . ? C37 C36 C41 123.6(10) . . ? C37 C36 S3 118.3(8) . . ? C41 C36 S3 118.1(8) . . ? C36 C37 C38 119.1(9) . . ? C36 C37 H37A 120.4 . . ? C38 C37 H37A 120.4 . . ? C39 C38 C37 117.6(10) . . ? C39 C38 H38A 121.2 . . ? C37 C38 H38A 121.2 . . ? C40 C39 C38 121.5(10) . . ? C40 C39 C42 121.3(9) . . ? C38 C39 C42 117.2(10) . . ? C39 C40 C41 121.3(9) . . ? C39 C40 H40A 119.4 . . ? C41 C40 H40A 119.4 . . ? C36 C41 C40 116.9(9) . . ? C36 C41 H41A 121.5 . . ? C40 C41 H41A 121.5 . . ? O15 C42 O16 121.8(10) . . ? O15 C42 C39 117.4(10) . . ? O16 C42 C39 120.8(10) . . ? O19 C43 N1 125.9(12) . . ? O19 C43 Cs1 45.7(6) . . ? N1 C43 Cs1 170.4(8) . . ? O19 C43 H52A 117.0 . . ? N1 C43 H52A 117.0 . . ? Cs1 C43 H52A 71.6 . . ? N1 C44 H44A 109.5 . . ? N1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N1 C45 H45A 109.5 . . ? N1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N2 C46 H46A 109.5 . . ? N2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N2 C47 H47A 109.5 . . ? N2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O20 C48 N2 135.9(13) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 4.423 _refine_diff_density_min -6.680 _refine_diff_density_rms 0.266