# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dariush Hinderberger' _publ_contact_author_email HINDERBERGER@MPIP-MAINZ.MPG.DE _publ_section_title ; EPR-Spectroscopic Characterization of Persistent Germyl-Substituted Pb(III)- and Sn(III)-Radicals ; loop_ _publ_author_name 'Dariush Hinderberger' 'Karl-Wilhelm Klinkhammer' 'Dennis Kurzbach' 'Shenglai Yao.' # Attachment 'Kurzbach_et_al.cif' data_KGeSil3 _database_code_depnum_ccdc_archive 'CCDC 750475' #TrackingRef 'Kurzbach_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Potassium-tris(trimethylsilyl)germanide ; _chemical_name_common Potassium-tris(trimethylsilyl)germanide _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H27 Ge K Si3' _chemical_formula_weight 331.27 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' Si Si 0.0817 0.0704 '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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.595(3) _cell_length_b 13.969(3) _cell_length_c 18.131(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.94(3) _cell_angle_gamma 90.00 _cell_volume 3696.1(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prisms _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.052 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min .673 _exptl_absorpt_correction_T_max .923 _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 'Siemens P4 4-circle-diffractometer' _diffrn_measurement_method 'Profile fitted 2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8814 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.1224 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8487 _reflns_number_gt 4714 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _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^)+(0.0400P)^2^+20.6521P] 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 8487 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1612 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.002 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 Ge1 Ge 0.62466(6) 0.41713(6) 0.11330(5) 0.0257(2) Uani 1 1 d . . . Ge2 Ge 0.82034(6) 0.73141(6) 0.04960(5) 0.0281(2) Uani 1 1 d . . . K1 K 0.78441(13) 0.50326(14) 0.00048(11) 0.0396(5) Uani 1 1 d . . . Si11 Si 0.48586(14) 0.41825(17) 0.17951(12) 0.0277(5) Uani 1 1 d . . . K2 K 0.65292(14) 0.65034(14) 0.16139(11) 0.0406(5) Uani 1 1 d . . . Si21 Si 0.86287(15) 0.75945(18) -0.07498(12) 0.0320(5) Uani 1 1 d . . . Si12 Si 0.60054(16) 0.28541(17) 0.03192(13) 0.0330(5) Uani 1 1 d . . . Si13 Si 0.73070(16) 0.35511(18) 0.20331(13) 0.0331(5) Uani 1 1 d . . . Si22 Si 0.77513(16) 0.88897(17) 0.08488(14) 0.0344(5) Uani 1 1 d . . . Si23 Si 0.96936(15) 0.72137(19) 0.10575(12) 0.0330(5) Uani 1 1 d . . . C111 C 0.4599(6) 0.3121(6) 0.2397(5) 0.042(2) Uani 1 1 d . . . H11A H 0.4013 0.3209 0.2620 0.063 Uiso 1 1 calc R . . H11B H 0.5064 0.3063 0.2774 0.063 Uiso 1 1 calc R . . H11C H 0.4587 0.2550 0.2102 0.063 Uiso 1 1 calc R . . C211 C 0.9657(6) 0.8394(8) -0.0880(5) 0.047(3) Uani 1 1 d . . . H21A H 0.9777 0.8455 -0.1397 0.071 Uiso 1 1 calc R . . H21B H 1.0181 0.8119 -0.0633 0.071 Uiso 1 1 calc R . . H21C H 0.9535 0.9014 -0.0676 0.071 Uiso 1 1 calc R . . C112 C 0.4802(6) 0.5253(7) 0.2430(5) 0.045(2) Uani 1 1 d . . . H11I H 0.4746 0.5827 0.2142 0.054 Uiso 1 1 calc R . . H11D H 0.5351 0.5283 0.2728 0.054 Uiso 1 1 calc R . . H11E H 0.4281 0.5193 0.2743 0.054 Uiso 1 1 calc R . . C212 C 0.8925(6) 0.6419(7) -0.1213(5) 0.043(2) Uani 1 1 d . . . H21I H 0.8373 0.6064 -0.1312 0.051 Uiso 1 1 calc R . . H21D H 0.9321 0.6052 -0.0893 0.051 Uiso 1 1 calc R . . H21E H 0.9230 0.6545 -0.1668 0.051 Uiso 1 1 calc R . . C231 C 1.0458(6) 0.6314(7) 0.0576(5) 0.046(2) Uani 1 1 d . . . H23A H 1.0958 0.6139 0.0899 0.069 Uiso 1 1 calc R . . H23B H 1.0693 0.6594 0.0135 0.069 Uiso 1 1 calc R . . H23C H 1.0108 0.5753 0.0451 0.069 Uiso 1 1 calc R . . C213 C 0.7651(6) 0.8110(7) -0.1325(5) 0.046(2) Uani 1 1 d . . . H21F H 0.7839 0.8172 -0.1828 0.069 Uiso 1 1 calc R . . H21G H 0.7488 0.8727 -0.1136 0.069 Uiso 1 1 calc R . . H21H H 0.7132 0.7690 -0.1303 0.069 Uiso 1 1 calc R . . C113 C 0.3823(6) 0.4329(7) 0.1153(5) 0.041(2) Uani 1 1 d . . . H11F H 0.3298 0.4505 0.1435 0.062 Uiso 1 1 calc R . . H11G H 0.3703 0.3736 0.0902 0.062 Uiso 1 1 calc R . . H11H H 0.3944 0.4821 0.0798 0.062 Uiso 1 1 calc R . . C232 C 1.0416(7) 0.8318(7) 0.1133(6) 0.053(3) Uani 1 1 d . . . H23D H 1.0989 0.8163 0.1372 0.079 Uiso 1 1 calc R . . H23E H 1.0102 0.8791 0.1417 0.079 Uiso 1 1 calc R . . H23F H 1.0528 0.8564 0.0648 0.079 Uiso 1 1 calc R . . C221 C 0.7901(7) 0.9065(8) 0.1883(5) 0.056(3) Uani 1 1 d . . . H22A H 0.7719 0.9703 0.2013 0.084 Uiso 1 1 calc R . . H22B H 0.8532 0.8970 0.2021 0.084 Uiso 1 1 calc R . . H22C H 0.7528 0.8611 0.2138 0.084 Uiso 1 1 calc R . . C121 C 0.7094(8) 0.2582(10) -0.0176(7) 0.081(4) Uani 1 1 d . . . H12A H 0.6985 0.2080 -0.0529 0.121 Uiso 1 1 calc R . . H12B H 0.7556 0.2380 0.0174 0.121 Uiso 1 1 calc R . . H12C H 0.7300 0.3146 -0.0427 0.121 Uiso 1 1 calc R . . C233 C 0.9603(7) 0.6750(8) 0.2022(5) 0.056(3) Uani 1 1 d . . . H23G H 1.0206 0.6668 0.2232 0.084 Uiso 1 1 calc R . . H23H H 0.9289 0.6146 0.2015 0.084 Uiso 1 1 calc R . . H23I H 0.9266 0.7199 0.2313 0.084 Uiso 1 1 calc R . . C122 C 0.5139(8) 0.3161(7) -0.0434(5) 0.057(3) Uani 1 1 d . . . H12D H 0.5190 0.2711 -0.0831 0.085 Uiso 1 1 calc R . . H12E H 0.5257 0.3795 -0.0614 0.085 Uiso 1 1 calc R . . H12F H 0.4533 0.3134 -0.0239 0.085 Uiso 1 1 calc R . . C123 C 0.5594(9) 0.1699(7) 0.0722(6) 0.066(3) Uani 1 1 d . . . H12G H 0.5579 0.1215 0.0346 0.099 Uiso 1 1 calc R . . H12H H 0.4989 0.1785 0.0911 0.099 Uiso 1 1 calc R . . H12I H 0.6002 0.1504 0.1114 0.099 Uiso 1 1 calc R . . C131 C 0.7236(8) 0.2261(8) 0.2337(7) 0.069(4) Uani 1 1 d . . . H13A H 0.7757 0.2110 0.2645 0.104 Uiso 1 1 calc R . . H13B H 0.7229 0.1853 0.1911 0.104 Uiso 1 1 calc R . . H13C H 0.6685 0.2166 0.2609 0.104 Uiso 1 1 calc R . . C222 C 0.6492(6) 0.9054(7) 0.0627(6) 0.054(3) Uani 1 1 d . . . H22D H 0.6308 0.9688 0.0763 0.081 Uiso 1 1 calc R . . H22E H 0.6143 0.8594 0.0897 0.081 Uiso 1 1 calc R . . H22F H 0.6386 0.8963 0.0107 0.081 Uiso 1 1 calc R . . C132 C 0.7239(8) 0.4276(9) 0.2908(5) 0.063(3) Uani 1 1 d . . . H13D H 0.7531 0.3932 0.3305 0.095 Uiso 1 1 calc R . . H13E H 0.6609 0.4388 0.3023 0.095 Uiso 1 1 calc R . . H13F H 0.7544 0.4878 0.2841 0.095 Uiso 1 1 calc R . . C133 C 0.8495(6) 0.3690(10) 0.1670(6) 0.076(4) Uani 1 1 d . . . H13G H 0.8931 0.3452 0.2028 0.114 Uiso 1 1 calc R . . H13H H 0.8614 0.4354 0.1577 0.114 Uiso 1 1 calc R . . H13I H 0.8548 0.3334 0.1220 0.114 Uiso 1 1 calc R . . C223 C 0.8321(8) 0.9930(7) 0.0409(6) 0.057(3) Uani 1 1 d . . . H22G H 0.8058 1.0513 0.0590 0.085 Uiso 1 1 calc R . . H22H H 0.8235 0.9896 -0.0116 0.085 Uiso 1 1 calc R . . H22I H 0.8964 0.9918 0.0528 0.085 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 Ge1 0.0226(4) 0.0254(4) 0.0294(4) 0.0013(4) 0.0064(3) -0.0025(4) Ge2 0.0239(4) 0.0290(4) 0.0317(4) 0.0013(4) 0.0082(3) -0.0049(4) K1 0.0366(10) 0.0372(11) 0.0456(11) -0.0036(9) 0.0184(9) -0.0015(9) Si11 0.0239(11) 0.0275(11) 0.0318(11) 0.0034(10) 0.0082(9) -0.0001(10) K2 0.0416(11) 0.0335(10) 0.0472(12) -0.0064(9) 0.0184(9) -0.0049(9) Si21 0.0298(11) 0.0391(13) 0.0272(11) 0.0013(10) 0.0030(9) -0.0104(10) Si12 0.0357(13) 0.0299(12) 0.0334(12) -0.0033(10) 0.0048(10) 0.0012(10) Si13 0.0270(12) 0.0364(13) 0.0360(13) -0.0002(11) 0.0012(10) 0.0023(10) Si22 0.0310(12) 0.0304(13) 0.0421(14) -0.0011(10) 0.0053(10) -0.0036(10) Si23 0.0267(11) 0.0435(14) 0.0289(11) -0.0026(11) 0.0056(9) -0.0006(11) C111 0.044(5) 0.040(5) 0.044(5) 0.012(4) 0.019(4) 0.002(4) C211 0.043(5) 0.068(7) 0.031(5) 0.000(5) 0.004(4) -0.036(5) C112 0.045(6) 0.040(5) 0.049(6) -0.003(4) 0.017(5) 0.002(4) C212 0.033(5) 0.064(6) 0.031(5) -0.002(5) 0.004(4) 0.000(5) C231 0.033(5) 0.068(7) 0.037(5) -0.008(5) 0.003(4) 0.017(5) C213 0.046(6) 0.049(6) 0.042(5) 0.013(5) -0.011(4) 0.001(5) C113 0.029(5) 0.038(5) 0.055(6) 0.004(4) 0.002(4) 0.002(4) C232 0.050(6) 0.058(7) 0.050(6) -0.005(5) -0.003(5) -0.009(5) C221 0.043(6) 0.064(7) 0.061(7) -0.021(6) 0.001(5) 0.008(5) C121 0.056(7) 0.104(11) 0.083(9) -0.047(8) 0.029(6) 0.000(7) C233 0.059(7) 0.074(8) 0.034(5) 0.004(5) 0.004(5) 0.007(6) C122 0.078(8) 0.043(6) 0.048(6) 0.009(5) -0.019(5) -0.004(6) C123 0.098(9) 0.038(6) 0.062(7) 0.015(5) -0.025(7) -0.009(6) C131 0.063(7) 0.050(7) 0.094(9) 0.029(6) -0.038(7) 0.000(6) C222 0.038(5) 0.045(6) 0.079(8) 0.002(6) -0.006(5) 0.010(5) C132 0.069(7) 0.074(8) 0.047(6) -0.021(6) -0.015(5) 0.020(6) C133 0.027(5) 0.132(12) 0.069(8) 0.027(8) 0.004(5) 0.007(7) C223 0.065(7) 0.041(6) 0.063(7) -0.002(5) 0.006(6) -0.021(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 Ge1 Si11 2.372(2) . ? Ge1 Si12 2.381(2) . ? Ge1 Si13 2.393(3) . ? Ge1 K1 3.350(2) . ? Ge1 K2 3.396(2) . ? Ge2 Si21 2.385(2) . ? Ge2 Si22 2.388(3) . ? Ge2 Si23 2.390(3) . ? Ge2 K1 3.348(2) . ? Ge2 K2 3.395(2) . ? K1 C231 3.297(8) 3_765 ? K1 C113 3.309(9) 3_665 ? K1 K2 4.074(3) . ? Si11 C111 1.883(8) . ? Si11 C112 1.890(9) . ? Si11 C113 1.904(9) . ? K2 C122 3.248(10) 3_665 ? K2 C111 3.337(8) 2_655 ? Si21 C211 1.888(8) . ? Si21 C213 1.895(9) . ? Si21 C212 1.898(10) . ? Si12 C123 1.875(10) . ? Si12 C121 1.877(10) . ? Si12 C122 1.895(10) . ? Si13 C133 1.875(10) . ? Si13 C131 1.887(10) . ? Si13 C132 1.886(10) . ? Si22 C223 1.860(10) . ? Si22 C222 1.889(9) . ? Si22 C221 1.900(10) . ? Si23 C233 1.871(9) . ? Si23 C232 1.872(10) . ? Si23 C231 1.903(9) . ? 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 Si11 Ge1 Si12 101.53(9) . . ? Si11 Ge1 Si13 101.86(9) . . ? Si12 Ge1 Si13 103.31(9) . . ? Si11 Ge1 K1 156.26(8) . . ? Si12 Ge1 K1 89.80(7) . . ? Si13 Ge1 K1 95.61(7) . . ? Si11 Ge1 K2 87.98(7) . . ? Si12 Ge1 K2 156.42(8) . . ? Si13 Ge1 K2 95.61(8) . . ? K1 Ge1 K2 74.30(5) . . ? Si21 Ge2 Si22 100.36(9) . . ? Si21 Ge2 Si23 99.43(9) . . ? Si22 Ge2 Si23 101.16(9) . . ? Si21 Ge2 K1 86.93(7) . . ? Si22 Ge2 K1 154.93(7) . . ? Si23 Ge2 K1 101.24(8) . . ? Si21 Ge2 K2 145.23(7) . . ? Si22 Ge2 K2 86.72(7) . . ? Si23 Ge2 K2 112.64(7) . . ? K1 Ge2 K2 74.34(5) . . ? C231 K1 C113 120.0(2) 3_765 3_665 ? C231 K1 Ge2 120.83(19) 3_765 . ? C113 K1 Ge2 91.30(17) 3_665 . ? C231 K1 Ge1 121.63(19) 3_765 . ? C113 K1 Ge1 88.41(16) 3_665 . ? Ge2 K1 Ge1 106.68(6) . . ? C231 K1 K2 151.83(17) 3_765 . ? C113 K1 K2 88.19(17) 3_665 . ? Ge2 K1 K2 53.35(4) . . ? Ge1 K1 K2 53.36(4) . . ? C111 Si11 C112 105.0(4) . . ? C111 Si11 C113 105.9(4) . . ? C112 Si11 C113 104.2(4) . . ? C111 Si11 Ge1 118.0(3) . . ? C112 Si11 Ge1 111.1(3) . . ? C113 Si11 Ge1 111.6(3) . . ? C122 K2 C111 83.4(3) 3_665 2_655 ? C122 K2 Ge2 95.6(2) 3_665 . ? C111 K2 Ge2 117.48(17) 2_655 . ? C122 K2 Ge1 83.26(19) 3_665 . ? C111 K2 Ge1 136.80(17) 2_655 . ? Ge2 K2 Ge1 104.61(5) . . ? C122 K2 K1 87.6(2) 3_665 . ? C111 K2 K1 165.68(18) 2_655 . ? Ge2 K2 K1 52.30(4) . . ? Ge1 K2 K1 52.34(4) . . ? C211 Si21 C213 107.4(5) . . ? C211 Si21 C212 105.6(4) . . ? C213 Si21 C212 105.1(4) . . ? C211 Si21 Ge2 115.8(3) . . ? C213 Si21 Ge2 112.2(3) . . ? C212 Si21 Ge2 110.0(3) . . ? C123 Si12 C121 106.9(6) . . ? C123 Si12 C122 105.2(5) . . ? C121 Si12 C122 105.1(6) . . ? C123 Si12 Ge1 118.0(4) . . ? C121 Si12 Ge1 109.6(4) . . ? C122 Si12 Ge1 111.2(3) . . ? C133 Si13 C131 104.9(6) . . ? C133 Si13 C132 107.5(6) . . ? C131 Si13 C132 105.3(6) . . ? C133 Si13 Ge1 108.3(4) . . ? C131 Si13 Ge1 120.4(3) . . ? C132 Si13 Ge1 109.7(3) . . ? C223 Si22 C222 104.7(5) . . ? C223 Si22 C221 106.1(5) . . ? C222 Si22 C221 106.9(5) . . ? C223 Si22 Ge2 118.6(4) . . ? C222 Si22 Ge2 109.1(3) . . ? C221 Si22 Ge2 110.8(4) . . ? C233 Si23 C232 105.4(5) . . ? C233 Si23 C231 104.6(5) . . ? C232 Si23 C231 104.1(5) . . ? C233 Si23 Ge2 109.9(3) . . ? C232 Si23 Ge2 119.4(3) . . ? C231 Si23 Ge2 112.3(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.698 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.157 data_pbgesi3 _database_code_depnum_ccdc_archive 'CCDC 750476' #TrackingRef 'Kurzbach_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[tris(trimethylsilyl)germyl]plumbylene ; _chemical_name_common Bis(tris(trimethylsilyl)germyl)plumbylene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 Ge2 Pb Si6' _chemical_formula_weight 791.52 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.275(3) _cell_length_b 22.189(4) _cell_length_c 22.437(5) _cell_angle_alpha 110.50(3) _cell_angle_beta 100.71(3) _cell_angle_gamma 100.26(3) _cell_volume 7192(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description coffin-shaped _exptl_crystal_colour green-blue _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 6.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .347 _exptl_absorpt_correction_T_max .897 _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 'Siemens P4 4-circle-diffractometer' _diffrn_measurement_method 'Profile fitted 2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26217 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.1095 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 25254 _reflns_number_gt 14483 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _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^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25254 _refine_ls_number_parameters 994 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1666 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2021 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.011 _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 Pb4 Pb 0.29479(5) 0.95145(3) 0.16121(3) 0.0445(2) Uani 1 1 d . . . Pb2 Pb 0.32623(5) 1.45506(4) -0.33906(3) 0.0472(2) Uani 1 1 d . . . Pb31 Pb 0.2682(4) 1.8432(2) -0.44198(8) 0.0477(9) Uani 0.79(3) 1 d PD . . Pb32 Pb 0.230(4) 1.8336(7) -0.4506(11) 0.082(9) Uani 0.21(3) 1 d PD . . Pb11 Pb 0.2706(4) 1.34494(10) 0.06022(9) 0.0549(12) Uani 0.510(7) 1 d P . . Pb12 Pb 0.2037(4) 1.33316(11) 0.04801(12) 0.0534(13) Uani 0.490(7) 1 d P . . Ge41 Ge 0.26059(11) 1.06467(8) 0.15421(9) 0.0319(4) Uani 1 1 d . . . Ge42 Ge 0.27385(11) 0.85214(8) 0.04040(8) 0.0307(4) Uani 1 1 d . . . Ge21 Ge 0.25575(11) 1.55857(9) -0.33643(8) 0.0326(4) Uani 1 1 d . . . Ge31 Ge 0.25026(11) 1.83464(9) -0.56825(8) 0.0331(4) Uani 1 1 d D . . Ge11 Ge 0.23157(11) 1.45435(8) 0.14551(8) 0.0318(4) Uani 1 1 d . . . Ge12 Ge 0.24501(12) 1.33910(9) -0.06498(9) 0.0368(4) Uani 1 1 d . . . Ge22 Ge 0.27010(11) 1.35044(8) -0.45974(8) 0.0335(4) Uani 1 1 d . . . Ge32 Ge 0.23359(11) 1.95258(9) -0.35714(8) 0.0326(4) Uani 1 1 d D . . Si43 Si 0.3832(3) 1.1515(2) 0.2312(3) 0.0398(12) Uani 1 1 d . . . Si23 Si 0.1088(3) 1.5229(2) -0.3370(2) 0.0353(11) Uani 1 1 d . . . Si15 Si 0.2661(3) 1.4325(3) -0.0940(3) 0.0409(12) Uani 1 1 d . . . Si42 Si 0.1437(3) 1.0653(3) 0.2048(3) 0.0440(13) Uani 1 1 d . . . Si22 Si 0.3291(3) 1.6355(2) -0.2259(2) 0.0379(11) Uani 1 1 d . . . Si13 Si 0.2416(4) 1.4243(3) 0.2386(2) 0.0437(13) Uani 1 1 d . . . Si33 Si 0.1376(3) 1.7349(3) -0.6318(3) 0.0489(14) Uani 1 1 d . . . Si41 Si 0.2274(3) 1.0866(2) 0.0574(3) 0.0421(12) Uani 1 1 d . . . Si26 Si 0.2733(3) 1.2609(2) -0.4240(2) 0.0375(12) Uani 1 1 d . . . Si12 Si 0.3561(3) 1.5429(2) 0.1714(2) 0.0386(12) Uani 1 1 d . . . Si46 Si 0.4096(3) 0.8766(2) 0.0164(2) 0.0374(11) Uani 1 1 d . . . Si45 Si 0.1475(3) 0.8214(3) -0.0479(2) 0.0401(12) Uani 1 1 d . . . Si32 Si 0.3809(3) 1.8032(3) -0.5800(3) 0.0457(13) Uani 1 1 d . . . Si44 Si 0.2723(3) 0.7642(2) 0.0788(2) 0.0404(12) Uani 1 1 d . . . Si25 Si 0.3923(3) 1.3639(3) -0.5028(2) 0.0438(13) Uani 1 1 d . . . Si24 Si 0.1385(3) 1.3195(3) -0.5441(3) 0.0452(13) Uani 1 1 d . . . Si14 Si 0.1205(4) 1.2564(3) -0.1425(3) 0.0559(15) Uani 1 1 d . . . Si36 Si 0.2340(3) 1.9184(3) -0.2677(2) 0.0429(12) Uani 1 1 d . . . Si11 Si 0.0934(3) 1.4724(3) 0.1117(2) 0.0422(13) Uani 1 1 d . . . Si35 Si 0.1011(3) 1.9811(3) -0.3837(3) 0.0458(13) Uani 1 1 d . . . Si21 Si 0.2719(4) 1.6176(3) -0.4060(3) 0.0455(13) Uani 1 1 d . . . Si31 Si 0.2350(4) 1.9171(3) -0.6127(3) 0.0507(14) Uani 1 1 d . . . Si34 Si 0.3589(3) 2.0402(3) -0.3311(2) 0.0407(12) Uani 1 1 d . . . Si16 Si 0.3651(4) 1.2925(3) -0.0753(4) 0.074(2) Uani 1 1 d . . . C421 C 0.1868(12) 1.0818(9) 0.2939(9) 0.054(5) Uani 1 1 d . . . H42A H 0.1401 1.0820 0.3145 0.082 Uiso 1 1 calc R . . H42B H 0.2290 1.1243 0.3157 0.082 Uiso 1 1 calc R . . H42C H 0.2136 1.0475 0.2974 0.082 Uiso 1 1 calc R . . C321 C 0.3738(12) 1.7191(10) -0.5731(11) 0.068(7) Uani 1 1 d . . . H32A H 0.4262 1.7063 -0.5779 0.102 Uiso 1 1 calc R . . H32B H 0.3254 1.6861 -0.6072 0.102 Uiso 1 1 calc R . . H32C H 0.3661 1.7228 -0.5307 0.102 Uiso 1 1 calc R . . C441 C 0.1728(12) 0.7517(9) 0.1104(10) 0.052(5) Uani 1 1 d . . . H44A H 0.1715 0.7164 0.1260 0.077 Uiso 1 1 calc R . . H44B H 0.1215 0.7401 0.0753 0.077 Uiso 1 1 calc R . . H44C H 0.1751 0.7922 0.1460 0.077 Uiso 1 1 calc R . . C161 C 0.3360(14) 1.2049(9) -0.0849(9) 0.065(6) Uani 1 1 d . . . H16A H 0.3851 1.1870 -0.0892 0.098 Uiso 1 1 calc R . . H16B H 0.2887 1.1796 -0.1237 0.098 Uiso 1 1 calc R . . H16C H 0.3191 1.2026 -0.0468 0.098 Uiso 1 1 calc R . . C351 C 0.1148(13) 2.0539(10) -0.4055(11) 0.066(6) Uani 1 1 d . . . H35A H 0.0597 2.0632 -0.4157 0.099 Uiso 1 1 calc R . . H35B H 0.1376 2.0448 -0.4432 0.099 Uiso 1 1 calc R . . H35C H 0.1542 2.0918 -0.3689 0.099 Uiso 1 1 calc R . . C361 C 0.2316(14) 1.9875(9) -0.1895(8) 0.066(6) Uani 1 1 d . . . H36A H 0.2317 1.9712 -0.1551 0.099 Uiso 1 1 calc R . . H36B H 0.1801 2.0020 -0.1978 0.099 Uiso 1 1 calc R . . H36C H 0.2817 2.0243 -0.1760 0.099 Uiso 1 1 calc R . . C461 C 0.4079(11) 0.9128(9) -0.0480(8) 0.048(5) Uani 1 1 d . . . H46A H 0.4646 0.9212 -0.0549 0.071 Uiso 1 1 calc R . . H46B H 0.3914 0.9539 -0.0332 0.071 Uiso 1 1 calc R . . H46C H 0.3670 0.8819 -0.0886 0.071 Uiso 1 1 calc R . . C462 C 0.4492(13) 0.7993(10) -0.0141(11) 0.065(6) Uani 1 1 d . . . H46D H 0.5039 0.8105 -0.0232 0.097 Uiso 1 1 calc R . . H46E H 0.4077 0.7667 -0.0537 0.097 Uiso 1 1 calc R . . H46F H 0.4562 0.7813 0.0192 0.097 Uiso 1 1 calc R . . C442 C 0.2719(16) 0.6827(9) 0.0149(10) 0.076(7) Uani 1 1 d . . . H44D H 0.2712 0.6500 0.0339 0.113 Uiso 1 1 calc R . . H44E H 0.3230 0.6882 -0.0003 0.113 Uiso 1 1 calc R . . H44F H 0.2213 0.6680 -0.0216 0.113 Uiso 1 1 calc R . . C261 C 0.3840(11) 1.2762(9) -0.3693(9) 0.050(5) Uani 1 1 d . . . H26A H 0.3850 1.2402 -0.3551 0.075 Uiso 1 1 calc R . . H26B H 0.3970 1.3174 -0.3314 0.075 Uiso 1 1 calc R . . H26C H 0.4264 1.2788 -0.3934 0.075 Uiso 1 1 calc R . . C121 C 0.3842(15) 1.6024(10) 0.2592(8) 0.077(7) Uani 1 1 d . . . H12A H 0.4346 1.6375 0.2682 0.115 Uiso 1 1 calc R . . H12B H 0.3960 1.5792 0.2875 0.115 Uiso 1 1 calc R . . H12C H 0.3364 1.6210 0.2672 0.115 Uiso 1 1 calc R . . C251 C 0.3765(13) 1.4036(10) -0.5636(9) 0.062(6) Uani 1 1 d . . . H25A H 0.4268 1.4081 -0.5798 0.093 Uiso 1 1 calc R . . H25B H 0.3679 1.4469 -0.5423 0.093 Uiso 1 1 calc R . . H25C H 0.3266 1.3763 -0.5998 0.093 Uiso 1 1 calc R . . C443 C 0.3714(13) 0.7887(9) 0.1489(9) 0.064(6) Uani 1 1 d . . . H44G H 0.3710 0.7535 0.1645 0.096 Uiso 1 1 calc R . . H44H H 0.3716 0.8288 0.1842 0.096 Uiso 1 1 calc R . . H44I H 0.4223 0.7964 0.1339 0.096 Uiso 1 1 calc R . . C262 C 0.2473(15) 1.1776(10) -0.4946(11) 0.080(7) Uani 1 1 d . . . H26D H 0.2495 1.1435 -0.4777 0.119 Uiso 1 1 calc R . . H26E H 0.2888 1.1783 -0.5198 0.119 Uiso 1 1 calc R . . H26F H 0.1902 1.1683 -0.5224 0.119 Uiso 1 1 calc R . . C231 C 0.0989(12) 1.4562(8) -0.3020(9) 0.055(5) Uani 1 1 d . . . H23A H 0.0398 1.4415 -0.3019 0.083 Uiso 1 1 calc R . . H23B H 0.1355 1.4743 -0.2577 0.083 Uiso 1 1 calc R . . H23C H 0.1164 1.4191 -0.3288 0.083 Uiso 1 1 calc R . . C141 C 0.1420(14) 1.2103(11) -0.2231(9) 0.075(7) Uani 1 1 d . . . H14A H 0.0899 1.1775 -0.2527 0.112 Uiso 1 1 calc R . . H14B H 0.1866 1.1886 -0.2158 0.112 Uiso 1 1 calc R . . H14C H 0.1604 1.2412 -0.2421 0.112 Uiso 1 1 calc R . . C221 C 0.3016(14) 1.7179(9) -0.2075(9) 0.060(6) Uani 1 1 d . . . H22A H 0.3321 1.7478 -0.1628 0.091 Uiso 1 1 calc R . . H22B H 0.2403 1.7111 -0.2128 0.091 Uiso 1 1 calc R . . H22C H 0.3183 1.7368 -0.2373 0.091 Uiso 1 1 calc R . . C111 C 0.1004(13) 1.5505(11) 0.0969(11) 0.070(7) Uani 1 1 d . . . H11A H 0.0430 1.5550 0.0835 0.105 Uiso 1 1 calc R . . H11B H 0.1290 1.5486 0.0628 0.105 Uiso 1 1 calc R . . H11C H 0.1327 1.5881 0.1369 0.105 Uiso 1 1 calc R . . C322 C 0.3978(13) 1.7955(11) -0.6611(10) 0.067(6) Uani 1 1 d . . . H32D H 0.4504 1.7826 -0.6650 0.101 Uiso 1 1 calc R . . H32E H 0.4018 1.8376 -0.6649 0.101 Uiso 1 1 calc R . . H32F H 0.3498 1.7623 -0.6955 0.101 Uiso 1 1 calc R . . C252 C 0.4146(12) 1.2826(9) -0.5454(9) 0.054(5) Uani 1 1 d . . . H25D H 0.4640 1.2897 -0.5622 0.080 Uiso 1 1 calc R . . H25E H 0.3650 1.2539 -0.5813 0.080 Uiso 1 1 calc R . . H25F H 0.4263 1.2620 -0.5146 0.080 Uiso 1 1 calc R . . C411 C 0.3076(12) 1.0672(10) 0.0095(9) 0.060(6) Uani 1 1 d . . . H41A H 0.2933 1.0762 -0.0295 0.090 Uiso 1 1 calc R . . H41B H 0.3065 1.0209 -0.0030 0.090 Uiso 1 1 calc R . . H41C H 0.3645 1.0943 0.0362 0.090 Uiso 1 1 calc R . . C241 C 0.1217(14) 1.3898(11) -0.5694(11) 0.075(7) Uani 1 1 d . . . H24A H 0.0682 1.3750 -0.6032 0.113 Uiso 1 1 calc R . . H24B H 0.1689 1.4035 -0.5859 0.113 Uiso 1 1 calc R . . H24C H 0.1195 1.4267 -0.5318 0.113 Uiso 1 1 calc R . . C352 C 0.0217(13) 1.9074(10) -0.4534(11) 0.087(9) Uani 1 1 d . . . H35D H -0.0320 1.9185 -0.4645 0.131 Uiso 1 1 calc R . . H35E H 0.0116 1.8705 -0.4403 0.131 Uiso 1 1 calc R . . H35F H 0.0446 1.8955 -0.4911 0.131 Uiso 1 1 calc R . . C451 C 0.1657(13) 0.8652(10) -0.1046(9) 0.059(6) Uani 1 1 d . . . H45A H 0.1137 0.8519 -0.1396 0.088 Uiso 1 1 calc R . . H45B H 0.2121 0.8534 -0.1230 0.088 Uiso 1 1 calc R . . H45C H 0.1805 0.9126 -0.0801 0.088 Uiso 1 1 calc R . . C151 C 0.1829(12) 1.4798(9) -0.0755(10) 0.059(6) Uani 1 1 d . . . H15A H 0.1932 1.5173 -0.0877 0.089 Uiso 1 1 calc R . . H15B H 0.1869 1.4952 -0.0291 0.089 Uiso 1 1 calc R . . H15C H 0.1261 1.4510 -0.1002 0.089 Uiso 1 1 calc R . . C152 C 0.3764(12) 1.4867(9) -0.0506(10) 0.063(6) Uani 1 1 d . . . H15D H 0.3848 1.5246 -0.0623 0.094 Uiso 1 1 calc R . . H15E H 0.4179 1.4623 -0.0629 0.094 Uiso 1 1 calc R . . H15F H 0.3842 1.5017 -0.0037 0.094 Uiso 1 1 calc R . . C431 C 0.4303(12) 1.1293(10) 0.2999(10) 0.060(6) Uani 1 1 d . . . H43A H 0.4794 1.1649 0.3300 0.090 Uiso 1 1 calc R . . H43B H 0.4483 1.0892 0.2825 0.090 Uiso 1 1 calc R . . H43C H 0.3875 1.1222 0.3227 0.090 Uiso 1 1 calc R . . C242 C 0.1388(14) 1.2473(10) -0.6179(11) 0.085(8) Uani 1 1 d . . . H24D H 0.0858 1.2350 -0.6517 0.127 Uiso 1 1 calc R . . H24E H 0.1436 1.2102 -0.6060 0.127 Uiso 1 1 calc R . . H24F H 0.1871 1.2593 -0.6341 0.127 Uiso 1 1 calc R . . C452 C 0.1208(14) 0.7307(10) -0.0967(11) 0.074(7) Uani 1 1 d . . . H45D H 0.0699 0.7177 -0.1325 0.112 Uiso 1 1 calc R . . H45E H 0.1103 0.7073 -0.0689 0.112 Uiso 1 1 calc R . . H45F H 0.1684 0.7200 -0.1140 0.112 Uiso 1 1 calc R . . C362 C 0.3317(13) 1.8895(12) -0.2477(11) 0.077(7) Uani 1 1 d . . . H36D H 0.3303 1.8759 -0.2116 0.115 Uiso 1 1 calc R . . H36E H 0.3828 1.9251 -0.2355 0.115 Uiso 1 1 calc R . . H36F H 0.3326 1.8523 -0.2856 0.115 Uiso 1 1 calc R . . C153 C 0.2568(14) 1.4009(10) -0.1847(10) 0.070(7) Uani 1 1 d . . . H15G H 0.2651 1.4378 -0.1978 0.105 Uiso 1 1 calc R . . H15H H 0.2003 1.3711 -0.2086 0.105 Uiso 1 1 calc R . . H15I H 0.3002 1.3775 -0.1940 0.105 Uiso 1 1 calc R . . C412 C 0.1144(12) 1.0340(11) 0.0021(10) 0.065(6) Uani 1 1 d . . . H41D H 0.1024 1.0436 -0.0367 0.098 Uiso 1 1 calc R . . H41E H 0.0720 1.0445 0.0259 0.098 Uiso 1 1 calc R . . H41F H 0.1120 0.9875 -0.0106 0.098 Uiso 1 1 calc R . . C413 C 0.2298(16) 1.1765(10) 0.0798(11) 0.078(7) Uani 1 1 d . . . H41G H 0.2163 1.1847 0.0403 0.118 Uiso 1 1 calc R . . H41H H 0.2865 1.2039 0.1067 0.118 Uiso 1 1 calc R . . H41I H 0.1877 1.1871 0.1039 0.118 Uiso 1 1 calc R . . C311 C 0.1597(14) 1.9652(11) -0.5775(11) 0.074(7) Uani 1 1 d . . . H31A H 0.1547 1.9981 -0.5957 0.112 Uiso 1 1 calc R . . H31B H 0.1820 1.9869 -0.5304 0.112 Uiso 1 1 calc R . . H31C H 0.1036 1.9352 -0.5885 0.112 Uiso 1 1 calc R . . C341 C 0.4597(12) 2.0159(11) -0.3057(12) 0.078(7) Uani 1 1 d . . . H34A H 0.5094 2.0521 -0.2954 0.117 Uiso 1 1 calc R . . H34B H 0.4625 1.9772 -0.3411 0.117 Uiso 1 1 calc R . . H34C H 0.4589 2.0060 -0.2674 0.117 Uiso 1 1 calc R . . C453 C 0.0540(11) 0.8408(11) -0.0137(10) 0.060(6) Uani 1 1 d . . . H45G H 0.0031 0.8284 -0.0494 0.089 Uiso 1 1 calc R . . H45H H 0.0675 0.8877 0.0128 0.089 Uiso 1 1 calc R . . H45I H 0.0435 0.8162 0.0130 0.089 Uiso 1 1 calc R . . C112 C 0.0363(14) 1.4775(13) 0.1773(12) 0.085(8) Uani 1 1 d . . . H11D H -0.0194 1.4848 0.1641 0.127 Uiso 1 1 calc R . . H11E H 0.0700 1.5138 0.2178 0.127 Uiso 1 1 calc R . . H11F H 0.0288 1.4365 0.1837 0.127 Uiso 1 1 calc R . . C122 C 0.4485(11) 1.5075(10) 0.1552(12) 0.069(7) Uani 1 1 d . . . H12D H 0.4990 1.5429 0.1654 0.103 Uiso 1 1 calc R . . H12E H 0.4345 1.4780 0.1095 0.103 Uiso 1 1 calc R . . H12F H 0.4598 1.4831 0.1824 0.103 Uiso 1 1 calc R . . C432 C 0.4672(12) 1.1630(11) 0.1877(10) 0.063(6) Uani 1 1 d . . . H43D H 0.5169 1.1978 0.2181 0.094 Uiso 1 1 calc R . . H43E H 0.4444 1.1749 0.1520 0.094 Uiso 1 1 calc R . . H43F H 0.4837 1.1222 0.1705 0.094 Uiso 1 1 calc R . . C363 C 0.1333(13) 1.8469(10) -0.2933(10) 0.069(7) Uani 1 1 d . . . H36G H 0.1319 1.8323 -0.2580 0.103 Uiso 1 1 calc R . . H36H H 0.1346 1.8106 -0.3319 0.103 Uiso 1 1 calc R . . H36I H 0.0825 1.8619 -0.3031 0.103 Uiso 1 1 calc R . . C263 C 0.1926(12) 1.2560(10) -0.3753(10) 0.059(6) Uani 1 1 d . . . H26G H 0.1944 1.2200 -0.3612 0.089 Uiso 1 1 calc R . . H26H H 0.1356 1.2484 -0.4023 0.089 Uiso 1 1 calc R . . H26I H 0.2066 1.2972 -0.3373 0.089 Uiso 1 1 calc R . . C331 C 0.0325(11) 1.7547(10) -0.6462(10) 0.064(6) Uani 1 1 d . . . H33A H -0.0126 1.7143 -0.6719 0.096 Uiso 1 1 calc R . . H33B H 0.0340 1.7836 -0.6697 0.096 Uiso 1 1 calc R . . H33C H 0.0211 1.7767 -0.6046 0.096 Uiso 1 1 calc R . . C232 C 0.0338(13) 1.4848(10) -0.4218(9) 0.064(6) Uani 1 1 d . . . H23D H -0.0245 1.4714 -0.4194 0.096 Uiso 1 1 calc R . . H23E H 0.0498 1.4465 -0.4480 0.096 Uiso 1 1 calc R . . H23F H 0.0375 1.5168 -0.4416 0.096 Uiso 1 1 calc R . . C332 C 0.1534(13) 1.6886(10) -0.7150(10) 0.071(7) Uani 1 1 d . . . H33D H 0.1065 1.6490 -0.7388 0.106 Uiso 1 1 calc R . . H33E H 0.2072 1.6765 -0.7092 0.106 Uiso 1 1 calc R . . H33F H 0.1545 1.7166 -0.7393 0.106 Uiso 1 1 calc R . . C253 C 0.4906(12) 1.4217(12) -0.4328(11) 0.080(7) Uani 1 1 d . . . H25G H 0.5400 1.4272 -0.4499 0.120 Uiso 1 1 calc R . . H25H H 0.5018 1.4028 -0.4006 0.120 Uiso 1 1 calc R . . H25I H 0.4797 1.4643 -0.4125 0.120 Uiso 1 1 calc R . . C131 C 0.3502(13) 1.4096(11) 0.2599(10) 0.065(6) Uani 1 1 d . . . H13A H 0.3557 1.3974 0.2972 0.098 Uiso 1 1 calc R . . H13B H 0.3944 1.4496 0.2706 0.098 Uiso 1 1 calc R . . H13C H 0.3566 1.3743 0.2229 0.098 Uiso 1 1 calc R . . C433 C 0.3547(12) 1.2330(8) 0.2658(10) 0.061(6) Uani 1 1 d . . . H43G H 0.4054 1.2667 0.2964 0.092 Uiso 1 1 calc R . . H43H H 0.3106 1.2280 0.2881 0.092 Uiso 1 1 calc R . . H43I H 0.3336 1.2459 0.2304 0.092 Uiso 1 1 calc R . . C142 C 0.0313(12) 1.2948(11) -0.1610(10) 0.078(8) Uani 1 1 d . . . H14D H -0.0185 1.2606 -0.1923 0.117 Uiso 1 1 calc R . . H14E H 0.0500 1.3264 -0.1791 0.117 Uiso 1 1 calc R . . H14F H 0.0163 1.3170 -0.1210 0.117 Uiso 1 1 calc R . . C312 C 0.3424(13) 1.9760(9) -0.5954(11) 0.071(7) Uani 1 1 d . . . H31D H 0.3346 2.0087 -0.6133 0.107 Uiso 1 1 calc R . . H31E H 0.3801 1.9517 -0.6154 0.107 Uiso 1 1 calc R . . H31F H 0.3677 1.9980 -0.5485 0.107 Uiso 1 1 calc R . . C233 C 0.0693(11) 1.5917(9) -0.2890(8) 0.047(5) Uani 1 1 d . . . H23G H 0.0099 1.5751 -0.2906 0.071 Uiso 1 1 calc R . . H23H H 0.0733 1.6249 -0.3074 0.071 Uiso 1 1 calc R . . H23I H 0.1039 1.6112 -0.2440 0.071 Uiso 1 1 calc R . . C422 C 0.0617(13) 0.9812(11) 0.1640(10) 0.079(7) Uani 1 1 d . . . H42D H 0.0151 0.9820 0.1847 0.119 Uiso 1 1 calc R . . H42E H 0.0890 0.9476 0.1687 0.119 Uiso 1 1 calc R . . H42F H 0.0393 0.9714 0.1180 0.119 Uiso 1 1 calc R . . C222 C 0.4504(11) 1.6485(9) -0.2135(10) 0.058(6) Uani 1 1 d . . . H22D H 0.4801 1.6795 -0.1691 0.087 Uiso 1 1 calc R . . H22E H 0.4682 1.6659 -0.2440 0.087 Uiso 1 1 calc R . . H22F H 0.4643 1.6066 -0.2210 0.087 Uiso 1 1 calc R . . C313 C 0.1921(16) 1.8749(10) -0.7053(9) 0.078(7) Uani 1 1 d . . . H31G H 0.1859 1.9078 -0.7232 0.117 Uiso 1 1 calc R . . H31H H 0.1367 1.8439 -0.7167 0.117 Uiso 1 1 calc R . . H31I H 0.2318 1.8514 -0.7233 0.117 Uiso 1 1 calc R . . C123 C 0.3387(13) 1.5947(11) 0.1220(11) 0.074(7) Uani 1 1 d . . . H12G H 0.3906 1.6297 0.1341 0.111 Uiso 1 1 calc R . . H12H H 0.2917 1.6139 0.1309 0.111 Uiso 1 1 calc R . . H12I H 0.3251 1.5671 0.0758 0.111 Uiso 1 1 calc R . . C132 C 0.2281(14) 1.4902(11) 0.3130(10) 0.073(7) Uani 1 1 d . . . H13D H 0.2326 1.4754 0.3486 0.110 Uiso 1 1 calc R . . H13E H 0.1723 1.4983 0.3025 0.110 Uiso 1 1 calc R . . H13F H 0.2726 1.5306 0.3260 0.110 Uiso 1 1 calc R . . C423 C 0.0858(14) 1.1299(12) 0.1968(12) 0.082(7) Uani 1 1 d . . . H42G H 0.0393 1.1288 0.2176 0.123 Uiso 1 1 calc R . . H42H H 0.0627 1.1203 0.1509 0.123 Uiso 1 1 calc R . . H42I H 0.1259 1.1734 0.2179 0.123 Uiso 1 1 calc R . . C133 C 0.1575(15) 1.3454(9) 0.2188(11) 0.074(7) Uani 1 1 d . . . H13G H 0.1630 1.3346 0.2570 0.110 Uiso 1 1 calc R . . H13H H 0.1657 1.3098 0.1830 0.110 Uiso 1 1 calc R . . H13I H 0.1009 1.3515 0.2064 0.110 Uiso 1 1 calc R . . C113 C 0.0261(12) 1.3980(12) 0.0336(10) 0.079(7) Uani 1 1 d . . . H11G H -0.0296 1.4049 0.0196 0.118 Uiso 1 1 calc R . . H11H H 0.0188 1.3583 0.0423 0.118 Uiso 1 1 calc R . . H11I H 0.0553 1.3933 -0.0006 0.118 Uiso 1 1 calc R . . C353 C 0.0545(14) 2.0055(13) -0.3091(11) 0.083(8) Uani 1 1 d . . . H35G H 0.0013 2.0168 -0.3207 0.124 Uiso 1 1 calc R . . H35H H 0.0953 2.0432 -0.2732 0.124 Uiso 1 1 calc R . . H35I H 0.0436 1.9686 -0.2960 0.124 Uiso 1 1 calc R . . C211 C 0.1863(14) 1.6670(11) -0.4035(13) 0.084(8) Uani 1 1 d . . . H21A H 0.1917 1.6912 -0.4313 0.126 Uiso 1 1 calc R . . H21B H 0.1949 1.6978 -0.3590 0.126 Uiso 1 1 calc R . . H21C H 0.1295 1.6368 -0.4190 0.126 Uiso 1 1 calc R . . C463 C 0.4911(14) 0.9387(11) 0.0947(10) 0.079(7) Uani 1 1 d . . . H46G H 0.5464 0.9491 0.0861 0.119 Uiso 1 1 calc R . . H46H H 0.4963 0.9200 0.1275 0.119 Uiso 1 1 calc R . . H46I H 0.4724 0.9787 0.1106 0.119 Uiso 1 1 calc R . . C223 C 0.3012(15) 1.6016(10) -0.1662(9) 0.069(6) Uani 1 1 d . . . H22G H 0.3314 1.6332 -0.1222 0.103 Uiso 1 1 calc R . . H22H H 0.3179 1.5607 -0.1740 0.103 Uiso 1 1 calc R . . H22I H 0.2399 1.5931 -0.1714 0.103 Uiso 1 1 calc R . . C323 C 0.4761(12) 1.8642(11) -0.5126(11) 0.078(7) Uani 1 1 d . . . H32G H 0.5277 1.8503 -0.5184 0.116 Uiso 1 1 calc R . . H32H H 0.4680 1.8662 -0.4707 0.116 Uiso 1 1 calc R . . H32I H 0.4816 1.9074 -0.5139 0.116 Uiso 1 1 calc R . . C212 C 0.3795(14) 1.6773(12) -0.3763(11) 0.094(9) Uani 1 1 d . . . H21D H 0.3845 1.7004 -0.4051 0.141 Uiso 1 1 calc R . . H21E H 0.4236 1.6538 -0.3760 0.141 Uiso 1 1 calc R . . H21F H 0.3867 1.7090 -0.3324 0.141 Uiso 1 1 calc R . . C243 C 0.0454(13) 1.2917(11) -0.5135(10) 0.070(6) Uani 1 1 d . . . H24G H -0.0078 1.2792 -0.5472 0.106 Uiso 1 1 calc R . . H24H H 0.0441 1.3276 -0.4746 0.106 Uiso 1 1 calc R . . H24I H 0.0521 1.2542 -0.5031 0.106 Uiso 1 1 calc R . . C333 C 0.1301(15) 1.6754(11) -0.5894(12) 0.088(8) Uani 1 1 d . . . H33G H 0.0839 1.6360 -0.6165 0.132 Uiso 1 1 calc R . . H33H H 0.1187 1.6963 -0.5476 0.132 Uiso 1 1 calc R . . H33I H 0.1838 1.6633 -0.5825 0.132 Uiso 1 1 calc R . . C162 C 0.4061(15) 1.2972(12) -0.1462(16) 0.123(13) Uani 1 1 d . . . H16D H 0.4543 1.2779 -0.1484 0.185 Uiso 1 1 calc R . . H16E H 0.4243 1.3430 -0.1401 0.185 Uiso 1 1 calc R . . H16F H 0.3607 1.2731 -0.1865 0.185 Uiso 1 1 calc R . . C342 C 0.3602(16) 2.0620(15) -0.4027(13) 0.138(14) Uani 1 1 d . . . H34D H 0.4108 2.0976 -0.3920 0.207 Uiso 1 1 calc R . . H34E H 0.3092 2.0761 -0.4141 0.207 Uiso 1 1 calc R . . H34F H 0.3612 2.0238 -0.4395 0.207 Uiso 1 1 calc R . . C213 C 0.2540(19) 1.5645(14) -0.4951(13) 0.112(10) Uani 1 1 d . . . H21G H 0.2620 1.5925 -0.5190 0.167 Uiso 1 1 calc R . . H21H H 0.1961 1.5359 -0.5125 0.167 Uiso 1 1 calc R . . H21I H 0.2947 1.5379 -0.4995 0.167 Uiso 1 1 calc R . . C343 C 0.3631(16) 2.1178(12) -0.2620(14) 0.118(11) Uani 1 1 d . . . H34G H 0.4149 2.1513 -0.2539 0.177 Uiso 1 1 calc R . . H34H H 0.3632 2.1091 -0.2230 0.177 Uiso 1 1 calc R . . H34I H 0.3134 2.1333 -0.2732 0.177 Uiso 1 1 calc R . . C143 C 0.0785(17) 1.1928(14) -0.1098(15) 0.125(12) Uani 1 1 d . . . H14G H 0.0282 1.1601 -0.1421 0.187 Uiso 1 1 calc R . . H14H H 0.0632 1.2148 -0.0698 0.187 Uiso 1 1 calc R . . H14I H 0.1226 1.1713 -0.1007 0.187 Uiso 1 1 calc R . . C163 C 0.4564(19) 1.3400(11) 0.0002(19) 0.21(2) Uani 1 1 d . . . H16G H 0.5049 1.3213 -0.0040 0.318 Uiso 1 1 calc R . . H16H H 0.4387 1.3375 0.0380 0.318 Uiso 1 1 calc R . . H16I H 0.4729 1.3858 0.0058 0.318 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 Pb4 0.0729(5) 0.0304(4) 0.0311(4) 0.0131(3) 0.0097(3) 0.0185(4) Pb2 0.0653(5) 0.0401(4) 0.0293(4) 0.0080(3) -0.0021(3) 0.0246(4) Pb31 0.078(2) 0.0406(9) 0.0313(8) 0.0174(6) 0.0162(8) 0.0240(8) Pb32 0.18(2) 0.028(3) 0.050(4) 0.021(3) 0.057(9) 0.018(7) Pb11 0.105(4) 0.0346(10) 0.0341(9) 0.0206(8) 0.0199(12) 0.0251(13) Pb12 0.104(4) 0.0314(10) 0.0350(10) 0.0177(8) 0.0287(14) 0.0240(13) Ge41 0.0337(10) 0.0260(10) 0.0373(10) 0.0137(8) 0.0095(8) 0.0085(8) Ge42 0.0373(10) 0.0269(9) 0.0293(9) 0.0131(8) 0.0077(8) 0.0089(8) Ge21 0.0327(10) 0.0328(10) 0.0318(10) 0.0131(8) 0.0079(8) 0.0078(8) Ge31 0.0327(10) 0.0365(11) 0.0278(10) 0.0120(8) 0.0081(8) 0.0050(8) Ge11 0.0374(10) 0.0321(10) 0.0262(9) 0.0147(8) 0.0037(8) 0.0082(8) Ge12 0.0413(11) 0.0373(11) 0.0308(10) 0.0150(9) 0.0052(8) 0.0093(9) Ge22 0.0364(10) 0.0324(10) 0.0297(10) 0.0107(8) 0.0059(8) 0.0104(8) Ge32 0.0355(10) 0.0362(11) 0.0288(10) 0.0166(8) 0.0074(8) 0.0093(8) Si43 0.032(3) 0.034(3) 0.046(3) 0.012(2) 0.007(2) 0.004(2) Si23 0.035(3) 0.042(3) 0.026(2) 0.015(2) 0.005(2) 0.006(2) Si15 0.040(3) 0.042(3) 0.047(3) 0.023(3) 0.012(2) 0.015(2) Si42 0.036(3) 0.047(3) 0.041(3) 0.012(3) 0.010(2) 0.004(2) Si22 0.045(3) 0.029(3) 0.036(3) 0.012(2) 0.007(2) 0.005(2) Si13 0.065(4) 0.045(3) 0.031(3) 0.023(2) 0.015(2) 0.021(3) Si33 0.029(3) 0.050(3) 0.057(3) 0.020(3) 0.003(2) -0.003(2) Si41 0.052(3) 0.037(3) 0.044(3) 0.022(3) 0.013(2) 0.015(2) Si26 0.037(3) 0.036(3) 0.042(3) 0.019(2) 0.010(2) 0.009(2) Si12 0.041(3) 0.037(3) 0.035(3) 0.014(2) 0.005(2) 0.009(2) Si46 0.032(3) 0.043(3) 0.037(3) 0.020(2) 0.006(2) 0.007(2) Si45 0.035(3) 0.048(3) 0.031(3) 0.014(2) 0.003(2) 0.007(2) Si32 0.031(3) 0.060(4) 0.044(3) 0.022(3) 0.007(2) 0.008(3) Si44 0.059(3) 0.026(3) 0.030(3) 0.010(2) 0.008(2) 0.002(2) Si25 0.043(3) 0.052(3) 0.041(3) 0.027(3) 0.013(2) 0.006(3) Si24 0.038(3) 0.051(3) 0.041(3) 0.011(3) 0.004(2) 0.018(3) Si14 0.043(3) 0.059(4) 0.055(4) 0.016(3) 0.017(3) -0.002(3) Si36 0.054(3) 0.045(3) 0.031(3) 0.021(2) 0.008(2) 0.008(3) Si11 0.038(3) 0.063(4) 0.039(3) 0.032(3) 0.013(2) 0.018(3) Si35 0.037(3) 0.057(4) 0.057(4) 0.037(3) 0.012(3) 0.017(3) Si21 0.057(3) 0.041(3) 0.037(3) 0.020(2) 0.011(2) 0.003(3) Si31 0.063(4) 0.043(3) 0.047(3) 0.024(3) 0.010(3) 0.010(3) Si34 0.036(3) 0.042(3) 0.042(3) 0.019(3) 0.005(2) 0.005(2) Si16 0.052(4) 0.041(4) 0.097(5) 0.005(3) -0.021(3) 0.021(3) C421 0.071(13) 0.039(11) 0.060(13) 0.020(10) 0.027(11) 0.020(10) C321 0.046(13) 0.064(15) 0.109(19) 0.063(14) 0.010(12) 0.007(11) C441 0.057(12) 0.043(12) 0.066(14) 0.034(11) 0.023(10) 0.009(10) C161 0.083(16) 0.053(13) 0.044(12) 0.009(10) -0.005(11) 0.024(12) C351 0.064(14) 0.060(14) 0.103(18) 0.055(14) 0.025(13) 0.039(12) C361 0.109(18) 0.055(13) 0.027(10) 0.026(10) 0.006(11) -0.001(12) C461 0.049(12) 0.051(12) 0.043(11) 0.021(10) 0.014(9) 0.007(9) C462 0.061(13) 0.075(15) 0.091(17) 0.053(14) 0.031(12) 0.041(12) C442 0.14(2) 0.050(13) 0.078(16) 0.046(13) 0.049(15) 0.057(14) C261 0.048(12) 0.052(12) 0.055(12) 0.037(11) -0.001(9) 0.010(9) C121 0.108(19) 0.059(15) 0.023(11) -0.023(10) 0.006(11) 0.024(13) C251 0.064(14) 0.087(17) 0.051(13) 0.047(12) 0.016(10) 0.019(12) C443 0.093(17) 0.039(12) 0.041(12) 0.008(10) -0.002(11) 0.011(11) C262 0.095(18) 0.052(14) 0.070(16) 0.020(13) -0.005(13) 0.003(13) C231 0.062(13) 0.021(10) 0.058(13) 0.006(9) 0.003(10) -0.014(9) C141 0.076(16) 0.093(18) 0.028(11) -0.004(11) 0.013(10) 0.019(14) C221 0.086(16) 0.036(11) 0.049(12) 0.008(10) 0.011(11) 0.018(11) C111 0.065(14) 0.083(17) 0.105(19) 0.070(15) 0.034(13) 0.043(13) C322 0.058(14) 0.096(18) 0.078(16) 0.051(14) 0.041(12) 0.036(13) C252 0.054(12) 0.069(14) 0.060(13) 0.035(11) 0.037(10) 0.025(11) C411 0.055(13) 0.070(15) 0.040(12) 0.009(11) 0.013(10) 0.006(11) C241 0.071(15) 0.105(19) 0.098(18) 0.077(17) 0.040(14) 0.045(14) C352 0.061(15) 0.067(15) 0.089(17) 0.036(14) -0.060(13) -0.018(12) C451 0.071(14) 0.060(14) 0.045(12) 0.034(11) -0.002(10) 0.008(11) C151 0.049(12) 0.051(13) 0.078(15) 0.019(12) 0.016(11) 0.027(10) C152 0.060(14) 0.047(13) 0.074(15) 0.025(12) 0.011(11) 0.003(10) C431 0.047(12) 0.066(14) 0.069(14) 0.038(12) 0.001(10) 0.009(10) C242 0.063(15) 0.064(16) 0.080(17) 0.000(13) -0.032(12) 0.012(12) C452 0.064(15) 0.046(13) 0.094(18) 0.019(13) 0.005(13) 0.005(11) C362 0.067(16) 0.099(19) 0.078(17) 0.052(15) 0.010(13) 0.031(14) C153 0.095(17) 0.054(14) 0.070(15) 0.047(13) 0.017(13) 0.003(12) C412 0.050(13) 0.082(16) 0.065(14) 0.036(13) 0.007(11) 0.017(12) C413 0.12(2) 0.063(15) 0.074(16) 0.041(14) 0.032(15) 0.049(15) C311 0.084(17) 0.071(16) 0.077(17) 0.028(14) 0.040(14) 0.026(14) C341 0.042(13) 0.082(17) 0.100(19) 0.032(15) 0.016(12) 0.002(12) C453 0.040(12) 0.088(17) 0.067(14) 0.037(13) 0.031(10) 0.027(11) C112 0.068(16) 0.14(2) 0.098(19) 0.087(19) 0.044(14) 0.051(16) C122 0.028(11) 0.069(15) 0.11(2) 0.043(14) 0.019(12) 0.005(10) C432 0.045(12) 0.076(15) 0.078(15) 0.040(13) 0.024(11) 0.013(11) C363 0.066(14) 0.066(15) 0.056(13) 0.036(12) -0.008(11) -0.023(11) C263 0.060(14) 0.050(13) 0.068(14) 0.026(11) 0.025(11) 0.005(11) C331 0.026(10) 0.067(15) 0.068(14) 0.013(12) -0.013(10) -0.007(10) C232 0.071(14) 0.071(15) 0.048(12) 0.031(12) 0.003(11) 0.016(12) C332 0.044(12) 0.061(14) 0.060(14) -0.009(11) -0.001(10) -0.012(11) C253 0.025(11) 0.102(19) 0.092(18) 0.034(15) 0.003(11) -0.012(11) C131 0.085(16) 0.086(17) 0.052(13) 0.041(12) 0.026(12) 0.048(14) C433 0.044(12) 0.034(11) 0.075(15) 0.003(10) -0.014(10) 0.009(9) C142 0.044(13) 0.078(17) 0.061(15) -0.019(12) 0.014(11) -0.011(11) C312 0.078(16) 0.035(12) 0.097(18) 0.035(12) 0.023(13) -0.014(11) C233 0.037(10) 0.075(14) 0.034(10) 0.022(10) 0.020(8) 0.016(10) C422 0.068(15) 0.089(18) 0.050(13) 0.015(13) 0.013(11) -0.024(13) C222 0.046(12) 0.052(13) 0.063(14) 0.015(11) -0.006(10) 0.018(10) C313 0.12(2) 0.062(15) 0.045(13) 0.035(12) 0.008(13) -0.002(14) C123 0.058(14) 0.072(16) 0.090(18) 0.041(14) 0.013(13) 0.003(12) C132 0.068(15) 0.087(18) 0.071(16) 0.035(14) 0.021(12) 0.023(13) C423 0.073(16) 0.11(2) 0.087(18) 0.042(16) 0.039(14) 0.049(15) C133 0.12(2) 0.033(12) 0.077(16) 0.035(12) 0.026(14) 0.007(12) C113 0.041(13) 0.11(2) 0.057(14) 0.023(14) -0.006(10) 0.003(13) C353 0.081(17) 0.13(2) 0.099(19) 0.075(18) 0.061(15) 0.072(17) C211 0.070(16) 0.075(17) 0.13(2) 0.070(17) 0.021(15) 0.029(13) C463 0.078(16) 0.061(15) 0.065(16) 0.006(12) 0.011(13) -0.016(13) C223 0.113(19) 0.070(15) 0.038(12) 0.027(11) 0.026(12) 0.043(14) C323 0.033(12) 0.083(17) 0.084(17) 0.015(14) -0.009(11) 0.003(11) C212 0.071(16) 0.11(2) 0.063(16) 0.043(16) -0.012(12) -0.038(15) C243 0.074(15) 0.083(17) 0.056(14) 0.031(13) 0.012(11) 0.024(13) C333 0.083(17) 0.057(15) 0.092(19) 0.024(14) 0.010(14) -0.036(13) C162 0.070(17) 0.061(17) 0.25(4) 0.04(2) 0.10(2) 0.029(14) C342 0.083(19) 0.19(3) 0.11(2) 0.10(2) -0.009(16) -0.09(2) C213 0.16(3) 0.14(3) 0.11(2) 0.09(2) 0.09(2) 0.07(2) C343 0.081(19) 0.09(2) 0.13(3) -0.017(18) 0.048(18) -0.006(16) C143 0.10(2) 0.12(3) 0.16(3) 0.08(2) 0.04(2) -0.022(19) C163 0.14(3) 0.031(15) 0.32(5) -0.01(2) -0.13(3) 0.045(16) _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 Pb4 Ge41 2.7181(18) . ? Pb4 Ge42 2.743(2) . ? Pb2 Ge21 2.7319(19) . ? Pb2 Ge22 2.735(2) . ? Pb31 Pb32 0.59(6) . ? Pb31 Ge31 2.728(2) . ? Pb31 Ge32 2.735(3) . ? Pb32 Ge32 2.722(5) . ? Pb32 Ge31 2.726(4) . ? Pb11 Pb12 1.033(2) . ? Pb11 Ge12 2.715(2) . ? Pb11 Ge11 2.776(3) . ? Pb12 Ge11 2.702(3) . ? Pb12 Ge12 2.781(3) . ? Ge41 Si41 2.376(5) . ? Ge41 Si43 2.386(5) . ? Ge41 Si42 2.389(5) . ? Ge42 Si45 2.379(5) . ? Ge42 Si46 2.384(5) . ? Ge42 Si44 2.392(5) . ? Ge21 Si23 2.377(5) . ? Ge21 Si21 2.385(5) . ? Ge21 Si22 2.387(5) . ? Ge31 Si33 2.380(6) . ? Ge31 Si32 2.385(5) . ? Ge31 Si31 2.400(5) . ? Ge11 Si12 2.377(5) . ? Ge11 Si11 2.385(5) . ? Ge11 Si13 2.392(5) . ? Ge12 Si15 2.369(5) . ? Ge12 Si16 2.380(6) . ? Ge12 Si14 2.373(6) . ? Ge22 Si25 2.384(5) . ? Ge22 Si24 2.387(5) . ? Ge22 Si26 2.394(5) . ? Ge32 Si34 2.373(5) . ? Ge32 Si36 2.381(5) . ? Ge32 Si35 2.384(5) . ? Si43 C432 1.852(18) . ? Si43 C431 1.852(18) . ? Si43 C433 1.881(17) . ? Si23 C233 1.834(17) . ? Si23 C232 1.861(18) . ? Si23 C231 1.900(17) . ? Si15 C152 1.838(19) . ? Si15 C151 1.875(17) . ? Si15 C153 1.87(2) . ? Si42 C421 1.871(18) . ? Si42 C423 1.89(2) . ? Si42 C422 1.89(2) . ? Si22 C223 1.837(18) . ? Si22 C221 1.882(18) . ? Si22 C222 1.895(18) . ? Si13 C131 1.860(19) . ? Si13 C132 1.87(2) . ? Si13 C133 1.873(19) . ? Si33 C331 1.841(18) . ? Si33 C332 1.88(2) . ? Si33 C333 1.88(2) . ? Si41 C411 1.855(18) . ? Si41 C413 1.871(19) . ? Si41 C412 1.912(19) . ? Si26 C263 1.870(18) . ? Si26 C261 1.880(16) . ? Si26 C262 1.88(2) . ? Si12 C121 1.860(17) . ? Si12 C122 1.853(19) . ? Si12 C123 1.88(2) . ? Si46 C463 1.88(2) . ? Si46 C461 1.881(16) . ? Si46 C462 1.888(18) . ? Si45 C452 1.84(2) . ? Si45 C453 1.877(17) . ? Si45 C451 1.885(17) . ? Si32 C322 1.843(19) . ? Si32 C323 1.862(19) . ? Si32 C321 1.909(18) . ? Si44 C443 1.875(19) . ? Si44 C442 1.87(2) . ? Si44 C441 1.898(18) . ? Si25 C252 1.859(18) . ? Si25 C251 1.868(17) . ? Si25 C253 1.90(2) . ? Si24 C242 1.86(2) . ? Si24 C241 1.882(19) . ? Si24 C243 1.87(2) . ? Si14 C142 1.86(2) . ? Si14 C141 1.873(18) . ? Si14 C143 1.89(2) . ? Si36 C362 1.86(2) . ? Si36 C361 1.895(19) . ? Si36 C363 1.901(18) . ? Si11 C112 1.86(2) . ? Si11 C111 1.863(18) . ? Si11 C113 1.90(2) . ? Si35 C351 1.834(18) . ? Si35 C352 1.869(19) . ? Si35 C353 1.91(2) . ? Si21 C212 1.84(2) . ? Si21 C213 1.86(3) . ? Si21 C211 1.92(2) . ? Si31 C311 1.87(2) . ? Si31 C312 1.868(19) . ? Si31 C313 1.88(2) . ? Si34 C342 1.84(2) . ? Si34 C343 1.85(2) . ? Si34 C341 1.87(2) . ? Si16 C161 1.84(2) . ? Si16 C163 1.86(3) . ? Si16 C162 1.86(3) . ? 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 Ge41 Pb4 Ge42 113.83(6) . . ? Ge21 Pb2 Ge22 112.72(6) . . ? Pb32 Pb31 Ge31 83.6(8) . . ? Pb32 Pb31 Ge32 82.5(8) . . ? Ge31 Pb31 Ge32 115.75(11) . . ? Pb31 Pb32 Ge32 85.2(9) . . ? Pb31 Pb32 Ge31 84.1(8) . . ? Ge32 Pb32 Ge31 116.3(2) . . ? Pb12 Pb11 Ge12 82.77(17) . . ? Pb12 Pb11 Ge11 75.1(2) . . ? Ge12 Pb11 Ge11 113.19(10) . . ? Pb11 Pb12 Ge11 83.2(2) . . ? Pb11 Pb12 Ge12 75.62(17) . . ? Ge11 Pb12 Ge12 113.47(10) . . ? Si41 Ge41 Si43 107.79(19) . . ? Si41 Ge41 Si42 111.76(19) . . ? Si43 Ge41 Si42 107.82(19) . . ? Si41 Ge41 Pb4 126.60(14) . . ? Si43 Ge41 Pb4 104.07(13) . . ? Si42 Ge41 Pb4 97.34(14) . . ? Si45 Ge42 Si46 116.45(18) . . ? Si45 Ge42 Si44 109.17(19) . . ? Si46 Ge42 Si44 107.32(18) . . ? Si45 Ge42 Pb4 121.26(14) . . ? Si46 Ge42 Pb4 104.06(14) . . ? Si44 Ge42 Pb4 96.11(13) . . ? Si23 Ge21 Si21 112.49(18) . . ? Si23 Ge21 Si22 105.80(18) . . ? Si21 Ge21 Si22 106.94(18) . . ? Si23 Ge21 Pb2 106.01(13) . . ? Si21 Ge21 Pb2 124.28(15) . . ? Si22 Ge21 Pb2 99.21(13) . . ? Si33 Ge31 Si32 104.8(2) . . ? Si33 Ge31 Si31 109.8(2) . . ? Si32 Ge31 Si31 110.0(2) . . ? Si33 Ge31 Pb31 103.2(2) . . ? Si32 Ge31 Pb31 96.07(16) . . ? Si31 Ge31 Pb31 129.95(17) . . ? Si33 Ge31 Pb32 93.6(10) . . ? Si32 Ge31 Pb32 106.2(13) . . ? Si31 Ge31 Pb32 129.2(5) . . ? Pb31 Ge31 Pb32 12.3(13) . . ? Si12 Ge11 Si11 117.28(18) . . ? Si12 Ge11 Si13 107.29(19) . . ? Si11 Ge11 Si13 111.31(18) . . ? Si12 Ge11 Pb12 122.16(18) . . ? Si11 Ge11 Pb12 97.36(19) . . ? Si13 Ge11 Pb12 100.04(14) . . ? Si12 Ge11 Pb11 102.93(18) . . ? Si11 Ge11 Pb11 117.43(18) . . ? Si13 Ge11 Pb11 98.56(14) . . ? Pb12 Ge11 Pb11 21.68(5) . . ? Si15 Ge12 Si16 108.6(2) . . ? Si15 Ge12 Si14 108.7(2) . . ? Si16 Ge12 Si14 106.8(2) . . ? Si15 Ge12 Pb11 125.30(16) . . ? Si16 Ge12 Pb11 89.2(2) . . ? Si14 Ge12 Pb11 114.85(19) . . ? Si15 Ge12 Pb12 127.52(15) . . ? Si16 Ge12 Pb12 106.5(2) . . ? Si14 Ge12 Pb12 96.83(19) . . ? Pb11 Ge12 Pb12 21.62(5) . . ? Si25 Ge22 Si24 110.54(19) . . ? Si25 Ge22 Si26 106.35(18) . . ? Si24 Ge22 Si26 108.39(19) . . ? Si25 Ge22 Pb2 101.62(15) . . ? Si24 Ge22 Pb2 128.78(14) . . ? Si26 Ge22 Pb2 98.99(14) . . ? Si34 Ge32 Si36 110.62(18) . . ? Si34 Ge32 Si35 113.60(19) . . ? Si36 Ge32 Si35 108.27(19) . . ? Si34 Ge32 Pb32 114.9(12) . . ? Si36 Ge32 Pb32 97.9(2) . . ? Si35 Ge32 Pb32 110.3(14) . . ? Si34 Ge32 Pb31 103.7(2) . . ? Si36 Ge32 Pb31 98.00(15) . . ? Si35 Ge32 Pb31 121.44(18) . . ? Pb32 Ge32 Pb31 12.3(13) . . ? C432 Si43 C431 107.9(9) . . ? C432 Si43 C433 108.0(10) . . ? C431 Si43 C433 109.4(9) . . ? C432 Si43 Ge41 108.5(7) . . ? C431 Si43 Ge41 111.2(6) . . ? C433 Si43 Ge41 111.7(6) . . ? C233 Si23 C232 106.4(9) . . ? C233 Si23 C231 109.7(8) . . ? C232 Si23 C231 106.8(8) . . ? C233 Si23 Ge21 112.4(6) . . ? C232 Si23 Ge21 112.6(7) . . ? C231 Si23 Ge21 108.8(6) . . ? C152 Si15 C151 111.0(9) . . ? C152 Si15 C153 107.6(10) . . ? C151 Si15 C153 109.4(10) . . ? C152 Si15 Ge12 109.6(6) . . ? C151 Si15 Ge12 111.4(7) . . ? C153 Si15 Ge12 107.6(6) . . ? C421 Si42 C423 110.2(9) . . ? C421 Si42 C422 108.0(9) . . ? C423 Si42 C422 107.7(11) . . ? C421 Si42 Ge41 109.2(6) . . ? C423 Si42 Ge41 111.6(7) . . ? C422 Si42 Ge41 110.1(7) . . ? C223 Si22 C221 109.1(9) . . ? C223 Si22 C222 106.3(10) . . ? C221 Si22 C222 109.9(9) . . ? C223 Si22 Ge21 110.8(7) . . ? C221 Si22 Ge21 111.4(6) . . ? C222 Si22 Ge21 109.3(6) . . ? C131 Si13 C132 108.8(9) . . ? C131 Si13 C133 108.0(10) . . ? C132 Si13 C133 107.5(10) . . ? C131 Si13 Ge11 108.0(6) . . ? C132 Si13 Ge11 113.2(7) . . ? C133 Si13 Ge11 111.3(7) . . ? C331 Si33 C332 107.3(9) . . ? C331 Si33 C333 108.1(10) . . ? C332 Si33 C333 106.7(11) . . ? C331 Si33 Ge31 110.0(7) . . ? C332 Si33 Ge31 112.4(6) . . ? C333 Si33 Ge31 112.1(7) . . ? C411 Si41 C413 108.5(10) . . ? C411 Si41 C412 108.6(9) . . ? C413 Si41 C412 108.0(10) . . ? C411 Si41 Ge41 110.4(7) . . ? C413 Si41 Ge41 110.3(7) . . ? C412 Si41 Ge41 110.9(6) . . ? C263 Si26 C261 108.2(9) . . ? C263 Si26 C262 107.7(10) . . ? C261 Si26 C262 108.3(10) . . ? C263 Si26 Ge22 110.0(6) . . ? C261 Si26 Ge22 109.7(6) . . ? C262 Si26 Ge22 112.8(7) . . ? C121 Si12 C122 109.7(10) . . ? C121 Si12 C123 105.0(10) . . ? C122 Si12 C123 109.2(10) . . ? C121 Si12 Ge11 111.4(8) . . ? C122 Si12 Ge11 109.0(7) . . ? C123 Si12 Ge11 112.5(7) . . ? C463 Si46 C461 107.8(9) . . ? C463 Si46 C462 108.4(10) . . ? C461 Si46 C462 106.6(9) . . ? C463 Si46 Ge42 108.2(7) . . ? C461 Si46 Ge42 114.5(6) . . ? C462 Si46 Ge42 111.2(7) . . ? C452 Si45 C453 108.5(10) . . ? C452 Si45 C451 108.0(10) . . ? C453 Si45 C451 110.5(9) . . ? C452 Si45 Ge42 108.7(7) . . ? C453 Si45 Ge42 109.7(6) . . ? C451 Si45 Ge42 111.3(6) . . ? C322 Si32 C323 110.1(10) . . ? C322 Si32 C321 108.8(10) . . ? C323 Si32 C321 106.7(10) . . ? C322 Si32 Ge31 110.6(6) . . ? C323 Si32 Ge31 111.2(7) . . ? C321 Si32 Ge31 109.3(7) . . ? C443 Si44 C442 107.0(10) . . ? C443 Si44 C441 108.5(9) . . ? C442 Si44 C441 108.9(9) . . ? C443 Si44 Ge42 109.2(6) . . ? C442 Si44 Ge42 114.3(6) . . ? C441 Si44 Ge42 108.8(6) . . ? C252 Si25 C251 107.5(9) . . ? C252 Si25 C253 110.0(10) . . ? C251 Si25 C253 106.5(10) . . ? C252 Si25 Ge22 111.6(6) . . ? C251 Si25 Ge22 112.0(7) . . ? C253 Si25 Ge22 109.1(7) . . ? C242 Si24 C241 109.0(11) . . ? C242 Si24 C243 107.2(10) . . ? C241 Si24 C243 109.4(9) . . ? C242 Si24 Ge22 109.7(6) . . ? C241 Si24 Ge22 112.6(8) . . ? C243 Si24 Ge22 108.9(7) . . ? C142 Si14 C141 106.9(10) . . ? C142 Si14 C143 107.4(12) . . ? C141 Si14 C143 107.6(13) . . ? C142 Si14 Ge12 110.7(7) . . ? C141 Si14 Ge12 112.6(7) . . ? C143 Si14 Ge12 111.4(9) . . ? C362 Si36 C361 107.6(10) . . ? C362 Si36 C363 109.2(10) . . ? C361 Si36 C363 108.2(10) . . ? C362 Si36 Ge32 111.1(7) . . ? C361 Si36 Ge32 112.8(6) . . ? C363 Si36 Ge32 107.9(6) . . ? C112 Si11 C111 108.1(10) . . ? C112 Si11 C113 107.8(11) . . ? C111 Si11 C113 109.7(10) . . ? C112 Si11 Ge11 108.9(7) . . ? C111 Si11 Ge11 113.3(7) . . ? C113 Si11 Ge11 108.9(7) . . ? C351 Si35 C352 110.0(10) . . ? C351 Si35 C353 105.1(10) . . ? C352 Si35 C353 109.3(12) . . ? C351 Si35 Ge32 112.9(7) . . ? C352 Si35 Ge32 108.8(7) . . ? C353 Si35 Ge32 110.6(7) . . ? C212 Si21 C213 108.3(12) . . ? C212 Si21 C211 108.0(11) . . ? C213 Si21 C211 105.6(12) . . ? C212 Si21 Ge21 111.0(7) . . ? C213 Si21 Ge21 115.4(8) . . ? C211 Si21 Ge21 108.2(7) . . ? C311 Si31 C312 109.4(10) . . ? C311 Si31 C313 109.8(11) . . ? C312 Si31 C313 106.4(10) . . ? C311 Si31 Ge31 110.7(7) . . ? C312 Si31 Ge31 111.0(7) . . ? C313 Si31 Ge31 109.3(7) . . ? C342 Si34 C343 106.2(15) . . ? C342 Si34 C341 110.5(12) . . ? C343 Si34 C341 106.1(12) . . ? C342 Si34 Ge32 109.7(7) . . ? C343 Si34 Ge32 113.3(8) . . ? C341 Si34 Ge32 111.0(7) . . ? C161 Si16 C163 108.3(11) . . ? C161 Si16 C162 109.2(10) . . ? C163 Si16 C162 106.7(17) . . ? C161 Si16 Ge12 110.7(7) . . ? C163 Si16 Ge12 109.5(10) . . ? C162 Si16 Ge12 112.4(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.549 _refine_diff_density_min -1.594 _refine_diff_density_rms 0.211 data_sngesi3 _database_code_depnum_ccdc_archive 'CCDC 750477' #TrackingRef 'Kurzbach_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis[tris(trimethylsilyl)germyl]distannene ; _chemical_name_common Tetrakis(tris(trimethylsilyl)germyl)distannene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 Ge2 Si6 Sn' _chemical_formula_weight 703.02 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 23.409(6) _cell_length_b 13.216(4) _cell_length_c 23.711(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.60(4) _cell_angle_gamma 90.00 _cell_volume 7030(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelett _exptl_crystal_colour brown _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.59 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 2.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .789 _exptl_absorpt_correction_T_max .923 _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 'Siemens P4 4-circle-diffractometer' _diffrn_measurement_method 'Profile fitted 2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13666 _diffrn_reflns_av_R_equivalents 0.0769 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6909 _reflns_number_gt 4687 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _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^)+(0.0270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6909 _refine_ls_number_parameters 348 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.860 _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 Sn1 Sn 0.208227(19) 0.63457(4) 0.44303(2) 0.02264(16) Uani 0.972(3) 1 d PDU . . Ge1 Ge 0.119761(19) 0.76599(3) 0.44547(2) 0.02716(12) Uani 1 1 d D . . Ge2 Ge 0.18212(2) 0.46832(4) 0.37241(2) 0.02795(12) Uani 1 1 d D A . Sn1A Sn 0.1923(7) 0.6020(10) 0.4613(5) 0.021(4) Uani 0.028(3) 1 d PDU . . Si11 Si 0.11893(6) 0.92103(10) 0.39103(7) 0.0387(3) Uani 1 1 d . . . Si12 Si 0.02246(6) 0.69041(10) 0.41007(6) 0.0334(3) Uani 1 1 d . . . Si21 Si 0.10159(6) 0.34591(10) 0.35343(6) 0.0349(3) Uani 1 1 d . . . Si13 Si 0.12484(6) 0.81809(12) 0.54465(6) 0.0420(4) Uani 1 1 d . . . Si22 Si 0.17580(8) 0.54634(11) 0.27854(6) 0.0450(4) Uani 1 1 d . . . C211 C 0.0869(3) 0.2920(4) 0.4217(2) 0.0478(13) Uani 1 1 d . . . H21A H 0.0569 0.2403 0.4107 0.09(2) Uiso 1 1 calc R . . H21B H 0.0732 0.3449 0.4425 0.058(17) Uiso 1 1 calc R . . H21C H 0.1230 0.2635 0.4468 0.08(2) Uiso 1 1 calc R . . C111 C 0.0413(2) 0.9765(4) 0.3716(3) 0.0513(15) Uani 1 1 d . . . H11A H 0.0405 1.0386 0.3504 0.063(18) Uiso 1 1 calc R . . H11B H 0.0305 0.9896 0.4070 0.15(4) Uiso 1 1 calc R . . H11C H 0.0136 0.9294 0.3476 0.030(12) Uiso 1 1 calc R . . C212 C 0.1233(3) 0.2382(4) 0.3123(2) 0.0522(15) Uani 1 1 d . . . H21D H 0.0912 0.1904 0.3011 0.014(10) Uiso 1 1 calc R . . H21E H 0.1581 0.2054 0.3370 0.08(2) Uiso 1 1 calc R . . H21F H 0.1319 0.2636 0.2776 0.07(2) Uiso 1 1 calc R . . C213 C 0.0294(2) 0.3988(4) 0.3060(3) 0.0506(14) Uani 1 1 d . . . H21G H -0.0002 0.3463 0.2970 0.059(17) Uiso 1 1 calc R . . H21H H 0.0351 0.4245 0.2701 0.033(13) Uiso 1 1 calc R . . H21I H 0.0163 0.4525 0.3266 0.08(2) Uiso 1 1 calc R . . C121 C 0.0260(2) 0.5585(4) 0.4401(2) 0.0466(14) Uani 1 1 d . . . H12A H -0.0123 0.5268 0.4255 0.036(13) Uiso 1 1 calc R . . H12B H 0.0368 0.5610 0.4823 0.11(3) Uiso 1 1 calc R . . H12C H 0.0552 0.5202 0.4279 0.07(2) Uiso 1 1 calc R . . C221 C 0.1621(3) 0.4505(5) 0.2165(2) 0.0611(17) Uani 1 1 d . . . H22A H 0.1576 0.4850 0.1799 0.070(19) Uiso 1 1 calc R . . H22B H 0.1264 0.4130 0.2146 0.12(3) Uiso 1 1 calc R . . H22C H 0.1953 0.4048 0.2237 0.09(2) Uiso 1 1 calc R . . C131 C 0.2005(3) 0.8628(5) 0.5882(3) 0.0656(19) Uani 1 1 d . . . H13A H 0.2005 0.8753 0.6281 0.18(5) Uiso 1 1 calc R . . H13B H 0.2101 0.9241 0.5712 0.08(2) Uiso 1 1 calc R . . H13C H 0.2295 0.8119 0.5876 0.12(3) Uiso 1 1 calc R . . C112 C 0.1395(3) 0.9056(5) 0.3207(3) 0.0550(15) Uani 1 1 d . . . H11D H 0.1480 0.9708 0.3070 0.09(2) Uiso 1 1 calc R . . H11E H 0.1070 0.8749 0.2916 0.08(2) Uiso 1 1 calc R . . H11F H 0.1742 0.8634 0.3275 0.10(3) Uiso 1 1 calc R . . C122 C -0.0339(2) 0.7653(5) 0.4353(3) 0.0587(16) Uani 1 1 d . . . H12D H -0.0730 0.7381 0.4178 0.11(3) Uiso 1 1 calc R . . H12E H -0.0328 0.8347 0.4237 0.059(18) Uiso 1 1 calc R . . H12F H -0.0247 0.7614 0.4774 0.09(3) Uiso 1 1 calc R . . C123 C -0.0057(3) 0.6851(5) 0.3281(2) 0.0612(18) Uani 1 1 d . . . H12G H -0.0445 0.6543 0.3167 0.11(3) Uiso 1 1 calc R . . H12H H 0.0211 0.6458 0.3130 0.08(2) Uiso 1 1 calc R . . H12I H -0.0083 0.7524 0.3124 0.10(3) Uiso 1 1 calc R . . C113 C 0.1702(3) 1.0169(4) 0.4387(3) 0.0654(19) Uani 1 1 d . . . H11G H 0.1731 1.0752 0.4156 0.12(3) Uiso 1 1 calc R . . H11H H 0.2091 0.9876 0.4545 0.14(4) Uiso 1 1 calc R . . H11I H 0.1546 1.0367 0.4704 0.15(4) Uiso 1 1 calc R . . C132 C 0.0727(3) 0.9283(6) 0.5422(3) 0.081(3) Uani 1 1 d . . . H13D H 0.0764 0.9511 0.5815 0.10(3) Uiso 1 1 calc R . . H13E H 0.0324 0.9073 0.5240 0.15(4) Uiso 1 1 calc R . . H13F H 0.0829 0.9826 0.5199 0.09(3) Uiso 1 1 calc R . . C133 C 0.1014(3) 0.7129(6) 0.5861(3) 0.0714(19) Uani 1 1 d . . . H13G H 0.1002 0.7372 0.6239 0.14(3) Uiso 1 1 calc R . . H13H H 0.1294 0.6582 0.5912 0.13(4) Uiso 1 1 calc R . . H13I H 0.0625 0.6895 0.5643 0.09(2) Uiso 1 1 calc R . . C222 C 0.1125(5) 0.6391(6) 0.2552(3) 0.090(3) Uani 1 1 d . . . H22D H 0.1128 0.6699 0.2186 0.12(3) Uiso 1 1 calc R . . H22E H 0.1170 0.6905 0.2848 0.19(5) Uiso 1 1 calc R . . H22F H 0.0754 0.6044 0.2503 0.24(8) Uiso 1 1 calc R . . C223 C 0.2463(5) 0.6187(7) 0.2834(3) 0.098(3) Uani 1 1 d . . . H22G H 0.2423 0.6541 0.2472 0.11(3) Uiso 1 1 calc R . . H22H H 0.2792 0.5725 0.2905 0.13(4) Uiso 1 1 calc R . . H22I H 0.2533 0.6665 0.3152 0.11(3) Uiso 1 1 calc R . . Si23 Si 0.27506(6) 0.37400(11) 0.39254(7) 0.0432(3) Uani 1 1 d D . . C231 C 0.3329(7) 0.4369(15) 0.4530(8) 0.062(7) Uani 0.48(2) 1 d PDU A 1 H23A H 0.3703 0.4026 0.4589 0.093 Uiso 0.48(2) 1 calc PR A 1 H23B H 0.3211 0.4343 0.4886 0.093 Uiso 0.48(2) 1 calc PR A 1 H23C H 0.3370 0.5062 0.4427 0.093 Uiso 0.48(2) 1 calc PR A 1 C232 C 0.3083(9) 0.381(2) 0.3247(7) 0.103(10) Uani 0.48(2) 1 d PDU A 1 H23D H 0.3437 0.3401 0.3326 0.154 Uiso 0.48(2) 1 calc PR A 1 H23E H 0.3180 0.4497 0.3184 0.154 Uiso 0.48(2) 1 calc PR A 1 H23F H 0.2794 0.3559 0.2901 0.154 Uiso 0.48(2) 1 calc PR A 1 C233 C 0.2722(7) 0.2377(9) 0.4069(11) 0.078(7) Uani 0.48(2) 1 d PDU A 1 H23G H 0.3119 0.2126 0.4237 0.117 Uiso 0.48(2) 1 calc PR A 1 H23H H 0.2541 0.2030 0.3706 0.117 Uiso 0.48(2) 1 calc PR A 1 H23I H 0.2490 0.2264 0.4338 0.117 Uiso 0.48(2) 1 calc PR A 1 C234 C 0.3406(6) 0.4518(13) 0.4324(7) 0.047(5) Uani 0.52(2) 1 d PDU A 2 H23J H 0.3736 0.4082 0.4501 0.070 Uiso 0.52(2) 1 calc PR A 2 H23K H 0.3307 0.4909 0.4624 0.070 Uiso 0.52(2) 1 calc PR A 2 H23L H 0.3513 0.4965 0.4051 0.070 Uiso 0.52(2) 1 calc PR A 2 C235 C 0.2716(7) 0.2672(12) 0.4495(7) 0.082(6) Uani 0.52(2) 1 d PDU A 2 H23M H 0.2366 0.2266 0.4339 0.123 Uiso 0.52(2) 1 calc PR A 2 H23N H 0.2699 0.2977 0.4858 0.123 Uiso 0.52(2) 1 calc PR A 2 H23O H 0.3064 0.2254 0.4566 0.123 Uiso 0.52(2) 1 calc PR A 2 C236 C 0.2887(7) 0.3094(14) 0.3294(7) 0.070(6) Uani 0.52(2) 1 d PDU A 2 H23P H 0.3224 0.2652 0.3428 0.106 Uiso 0.52(2) 1 calc PR A 2 H23Q H 0.2967 0.3586 0.3028 0.106 Uiso 0.52(2) 1 calc PR A 2 H23R H 0.2542 0.2706 0.3095 0.106 Uiso 0.52(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02248(18) 0.0225(2) 0.0233(2) -0.00095(18) 0.00726(15) 0.00054(15) Ge1 0.0231(2) 0.0257(2) 0.0332(3) -0.00094(19) 0.00889(19) 0.00239(18) Ge2 0.0323(3) 0.0266(3) 0.0245(2) -0.00334(19) 0.00741(19) -0.00149(19) Sn1A 0.019(6) 0.029(7) 0.017(6) 0.005(5) 0.007(5) -0.009(5) Si11 0.0310(7) 0.0265(7) 0.0550(9) 0.0069(6) 0.0064(6) 0.0023(5) Si12 0.0285(7) 0.0399(8) 0.0312(7) 0.0050(6) 0.0078(5) -0.0053(5) Si21 0.0393(7) 0.0298(7) 0.0306(7) -0.0018(5) 0.0018(5) -0.0052(5) Si13 0.0312(7) 0.0524(9) 0.0396(8) -0.0179(7) 0.0056(6) 0.0121(6) Si22 0.0729(10) 0.0364(8) 0.0299(8) 0.0007(6) 0.0210(7) -0.0016(7) C211 0.058(4) 0.033(3) 0.049(3) 0.004(2) 0.010(3) -0.011(3) C111 0.042(3) 0.030(3) 0.076(4) 0.008(3) 0.006(3) 0.010(2) C212 0.071(4) 0.033(3) 0.044(3) -0.010(2) 0.003(3) -0.007(3) C213 0.037(3) 0.058(4) 0.047(3) -0.005(3) -0.004(2) -0.005(3) C121 0.049(3) 0.045(3) 0.045(3) 0.007(2) 0.013(3) -0.018(3) C221 0.093(5) 0.061(4) 0.029(3) -0.003(3) 0.017(3) 0.003(4) C131 0.046(4) 0.062(4) 0.073(5) -0.026(4) -0.008(3) 0.008(3) C112 0.048(4) 0.056(4) 0.060(4) 0.019(3) 0.014(3) 0.004(3) C122 0.029(3) 0.076(5) 0.073(5) 0.003(3) 0.017(3) -0.002(3) C123 0.081(5) 0.055(4) 0.040(3) 0.007(3) 0.004(3) -0.022(4) C113 0.053(4) 0.032(3) 0.096(5) 0.009(3) -0.004(4) -0.009(3) C132 0.061(5) 0.095(6) 0.074(5) -0.042(5) -0.002(4) 0.045(4) C133 0.084(5) 0.096(5) 0.043(4) -0.003(3) 0.030(4) -0.004(4) C222 0.144(8) 0.076(5) 0.051(4) 0.023(4) 0.029(4) 0.050(6) C223 0.140(8) 0.103(7) 0.070(5) -0.019(5) 0.062(5) -0.063(7) Si23 0.0384(8) 0.0368(8) 0.0497(9) -0.0102(7) 0.0048(6) 0.0063(6) C231 0.051(10) 0.044(9) 0.087(14) -0.007(10) 0.012(9) 0.014(7) C232 0.112(17) 0.17(2) 0.044(9) 0.021(12) 0.048(10) 0.080(17) C233 0.054(9) 0.049(9) 0.132(19) -0.004(9) 0.028(10) 0.001(7) C234 0.028(6) 0.043(8) 0.068(10) -0.022(8) 0.011(7) -0.006(5) C235 0.085(11) 0.054(9) 0.083(12) 0.010(8) -0.015(9) 0.004(8) C236 0.071(10) 0.084(12) 0.054(9) -0.030(9) 0.014(7) 0.026(9) _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 Sn1 Sn1A 0.78(2) . ? Sn1 Ge1 2.7161(7) . ? Sn1 Ge2 2.7239(8) . ? Sn1 Sn1A 2.781(8) 2_556 ? Sn1 Sn1 2.8469(15) 2_556 ? Ge1 Si12 2.4078(15) . ? Ge1 Si11 2.4188(15) . ? Ge1 Si13 2.4206(16) . ? Ge1 Sn1A 2.714(5) . ? Ge2 Si22 2.4190(16) . ? Ge2 Si21 2.4265(15) . ? Ge2 Si23 2.4334(16) . ? Ge2 Sn1A 2.707(5) . ? Sn1A Sn1 2.781(8) 2_556 ? Sn1A Sn1A 2.80(2) 2_556 ? Si11 C112 1.875(6) . ? Si11 C113 1.884(6) . ? Si11 C111 1.890(5) . ? Si12 C123 1.867(6) . ? Si12 C121 1.876(5) . ? Si12 C122 1.879(6) . ? Si21 C212 1.877(5) . ? Si21 C213 1.878(5) . ? Si21 C211 1.889(5) . ? Si13 C131 1.872(6) . ? Si13 C133 1.872(7) . ? Si13 C132 1.890(6) . ? Si22 C222 1.881(7) . ? Si22 C223 1.882(7) . ? Si22 C221 1.898(6) . ? Si23 C236 1.829(10) . ? Si23 C233 1.838(10) . ? Si23 C231 1.863(8) . ? Si23 C234 1.865(7) . ? Si23 C235 1.971(11) . ? Si23 C232 1.980(11) . ? 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 Sn1A Sn1 Ge1 81.6(4) . . ? Sn1A Sn1 Ge2 80.5(4) . . ? Ge1 Sn1 Ge2 119.37(3) . . ? Sn1A Sn1 Sn1A 83.2(7) . 2_556 ? Ge1 Sn1 Sn1A 123.2(5) . 2_556 ? Ge2 Sn1 Sn1A 111.4(4) . 2_556 ? Sn1A Sn1 Sn1 77.3(6) . 2_556 ? Ge1 Sn1 Sn1 107.52(4) . 2_556 ? Ge2 Sn1 Sn1 123.779(18) . 2_556 ? Sn1A Sn1 Sn1 15.8(5) 2_556 2_556 ? Si12 Ge1 Si11 107.63(5) . . ? Si12 Ge1 Si13 103.62(6) . . ? Si11 Ge1 Si13 105.56(6) . . ? Si12 Ge1 Sn1A 102.1(4) . . ? Si11 Ge1 Sn1A 131.3(5) . . ? Si13 Ge1 Sn1A 103.8(2) . . ? Si12 Ge1 Sn1 112.23(4) . . ? Si11 Ge1 Sn1 114.85(5) . . ? Si13 Ge1 Sn1 112.12(5) . . ? Sn1A Ge1 Sn1 16.4(5) . . ? Si22 Ge2 Si21 105.88(6) . . ? Si22 Ge2 Si23 102.41(6) . . ? Si21 Ge2 Si23 107.37(6) . . ? Si22 Ge2 Sn1A 114.0(4) . . ? Si21 Ge2 Sn1A 118.1(5) . . ? Si23 Ge2 Sn1A 107.83(19) . . ? Si22 Ge2 Sn1 99.54(5) . . ? Si21 Ge2 Sn1 132.67(4) . . ? Si23 Ge2 Sn1 105.17(5) . . ? Sn1A Ge2 Sn1 16.4(5) . . ? Sn1 Sn1A Ge2 83.0(5) . . ? Sn1 Sn1A Ge1 82.0(5) . . ? Ge2 Sn1A Ge1 120.1(2) . . ? Sn1 Sn1A Sn1 86.9(9) . 2_556 ? Ge2 Sn1A Sn1 127.1(3) . 2_556 ? Ge1 Sn1A Sn1 109.5(2) . 2_556 ? Sn1 Sn1A Sn1A 80.8(10) . 2_556 ? Ge2 Sn1A Sn1A 111.4(8) . 2_556 ? Ge1 Sn1A Sn1A 122.64(14) . 2_556 ? Sn1 Sn1A Sn1A 16.0(4) 2_556 2_556 ? C112 Si11 C113 109.0(3) . . ? C112 Si11 C111 107.4(3) . . ? C113 Si11 C111 106.8(3) . . ? C112 Si11 Ge1 114.7(2) . . ? C113 Si11 Ge1 110.0(2) . . ? C111 Si11 Ge1 108.61(19) . . ? C123 Si12 C121 108.9(3) . . ? C123 Si12 C122 106.3(3) . . ? C121 Si12 C122 109.1(3) . . ? C123 Si12 Ge1 113.3(2) . . ? C121 Si12 Ge1 108.59(17) . . ? C122 Si12 Ge1 110.5(2) . . ? C212 Si21 C213 107.6(3) . . ? C212 Si21 C211 107.6(3) . . ? C213 Si21 C211 107.5(3) . . ? C212 Si21 Ge2 106.9(2) . . ? C213 Si21 Ge2 112.45(19) . . ? C211 Si21 Ge2 114.51(17) . . ? C131 Si13 C133 108.5(3) . . ? C131 Si13 C132 105.9(3) . . ? C133 Si13 C132 107.7(4) . . ? C131 Si13 Ge1 113.7(2) . . ? C133 Si13 Ge1 111.0(2) . . ? C132 Si13 Ge1 109.7(2) . . ? C222 Si22 C223 106.9(5) . . ? C222 Si22 C221 105.3(4) . . ? C223 Si22 C221 109.8(3) . . ? C222 Si22 Ge2 112.6(3) . . ? C223 Si22 Ge2 109.7(3) . . ? C221 Si22 Ge2 112.4(2) . . ? C236 Si23 C233 73.6(8) . . ? C236 Si23 C231 125.5(8) . . ? C233 Si23 C231 110.6(7) . . ? C236 Si23 C234 111.2(6) . . ? C233 Si23 C234 121.0(9) . . ? C231 Si23 C234 18.6(9) . . ? C236 Si23 C235 106.1(7) . . ? C233 Si23 C235 33.0(5) . . ? C231 Si23 C235 87.4(7) . . ? C234 Si23 C235 103.7(6) . . ? C236 Si23 C232 32.3(6) . . ? C233 Si23 C232 103.8(7) . . ? C231 Si23 C232 103.7(7) . . ? C234 Si23 C232 85.9(8) . . ? C235 Si23 C232 133.8(8) . . ? C236 Si23 Ge2 115.7(5) . . ? C233 Si23 Ge2 117.4(4) . . ? C231 Si23 Ge2 109.5(6) . . ? C234 Si23 Ge2 112.2(6) . . ? C235 Si23 Ge2 106.9(5) . . ? C232 Si23 Ge2 110.8(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.721 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.123 data_kpbge3 _database_code_depnum_ccdc_archive 'CCDC 750478' #TrackingRef 'Kurzbach_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; potassium-tris[tris(trimethylsilyl)germyl]plumbanide ; _chemical_name_common potassium-tris(tris(trimethylsilyl)germyl)plumbanide _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H129 Ge3 K O6 Pb Si9' _chemical_formula_weight 1555.41 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' Si Si 0.0817 0.0704 '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' Ge Ge 0.1547 1.8001 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 19.0699(7) _cell_length_b 19.0699(7) _cell_length_c 38.370(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12084.4(11) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4836 _exptl_absorpt_coefficient_mu 3.413 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2339 _exptl_absorpt_correction_T_max 0.3422 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 92116 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.93 _reflns_number_total 6394 _reflns_number_gt 5692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-2' _computing_cell_refinement 'Bruker APEX-2' _computing_data_reduction 'Bruker APEX-2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _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^)+(0.0260P)^2^+29.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.078(4) _refine_ls_number_reflns 6394 _refine_ls_number_parameters 308 _refine_ls_number_restraints 138 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 1.0000 1.0000 0.949764(14) 0.02701(5) Uani 0.9475(6) 3 d SP . 8 Pb1B Pb 1.0000 1.0000 0.89540(10) 0.027 Uiso 0.0525(6) 3 d SP . 9 Ge1 Ge 1.07104(2) 0.91108(2) 0.921017(14) 0.03309(8) Uani 1 1 d . . . Si12 Si 1.12598(7) 0.92060(7) 0.86379(4) 0.0469(2) Uani 1 1 d . . . Si13 Si 1.16736(8) 0.92056(7) 0.96333(4) 0.0553(3) Uani 1 1 d . . . Si11 Si 0.97311(7) 0.76962(6) 0.92843(4) 0.0477(3) Uani 1 1 d . . . C111 C 0.8807(3) 0.7411(3) 0.90135(14) 0.0576(11) Uani 1 1 d . . . H11A H 0.8419 0.6833 0.9042 0.086 Uiso 1 1 calc R . . H11B H 0.8962 0.7526 0.8768 0.086 Uiso 1 1 calc R . . H11C H 0.8556 0.7727 0.9089 0.086 Uiso 1 1 calc R . . C112 C 0.9410(4) 0.7479(3) 0.97539(14) 0.0729(14) Uani 1 1 d . . . H11D H 0.9014 0.6902 0.9781 0.109 Uiso 1 1 calc R . . H11E H 0.9165 0.7802 0.9825 0.109 Uiso 1 1 calc R . . H11F H 0.9884 0.7619 0.9900 0.109 Uiso 1 1 calc R . . C113 C 1.0044(4) 0.6936(3) 0.91639(19) 0.0837(18) Uani 1 1 d . . . H11G H 0.9586 0.6388 0.9197 0.126 Uiso 1 1 calc R . . H11H H 1.0496 0.7015 0.9312 0.126 Uiso 1 1 calc R . . H11I H 1.0214 0.7011 0.8919 0.126 Uiso 1 1 calc R . . C121 C 1.1156(3) 0.9965(3) 0.83668(13) 0.0602(11) Uani 1 1 d . . . H12A H 1.1384 0.9995 0.8135 0.090 Uiso 1 1 calc R . . H12B H 1.1447 1.0498 0.8479 0.090 Uiso 1 1 calc R . . H12C H 1.0582 0.9800 0.8345 0.090 Uiso 1 1 calc R . . C122 C 1.2361(3) 0.9497(4) 0.86397(15) 0.0727(15) Uani 1 1 d . . . H12G H 1.2547 0.9524 0.8399 0.109 Uiso 1 1 calc R . . H12H H 1.2426 0.9090 0.8769 0.109 Uiso 1 1 calc R . . H12I H 1.2681 1.0027 0.8751 0.109 Uiso 1 1 calc R . . C123 C 1.0737(4) 0.8224(3) 0.83880(15) 0.0848(18) Uani 1 1 d . . . H12D H 1.0766 0.7801 0.8521 0.127 Uiso 1 1 calc R . . H12E H 1.1004 0.8294 0.8162 0.127 Uiso 1 1 calc R . . H12F H 1.0168 0.8067 0.8351 0.127 Uiso 1 1 calc R . . C131 C 1.1795(3) 0.8283(3) 0.96285(18) 0.0722(15) Uani 1 1 d . . . H13G H 1.2194 0.8343 0.9804 0.108 Uiso 1 1 calc R . . H13H H 1.1981 0.8225 0.9398 0.108 Uiso 1 1 calc R . . H13I H 1.1274 0.7800 0.9681 0.108 Uiso 1 1 calc R . . C132 C 1.1319(4) 0.9283(4) 1.00772(14) 0.0803(16) Uani 1 1 d . . . H13A H 1.1230 0.9746 1.0085 0.121 Uiso 1 1 calc R . . H13B H 1.1730 0.9358 1.0250 0.121 Uiso 1 1 calc R . . H13C H 1.0811 0.8785 1.0130 0.121 Uiso 1 1 calc R . . C133 C 1.2742(3) 1.0080(3) 0.95981(18) 0.0837(19) Uani 1 1 d . . . H13D H 1.2735 1.0590 0.9596 0.126 Uiso 1 1 calc R . . H13E H 1.2989 1.0030 0.9382 0.126 Uiso 1 1 calc R . . H13F H 1.3059 1.0075 0.9798 0.126 Uiso 1 1 calc R . . K1 K 1.0000 1.0000 1.15918(8) 0.0920(8) Uani 1 3 d S . . O3 O 1.1357(14) 1.0902(9) 1.1225(5) 0.135(7) Uani 0.575(19) 1 d PDU A 3 C31 C 1.162(2) 1.0518(10) 1.0978(9) 0.24(2) Uani 0.575(19) 1 d PD A 3 H31A H 1.1945 1.0319 1.1096 0.289 Uiso 0.575(19) 1 calc PR A 3 H31B H 1.1140 1.0048 1.0872 0.289 Uiso 0.575(19) 1 calc PR A 3 C32 C 1.203(2) 1.1013(11) 1.0745(6) 0.167(15) Uani 0.575(19) 1 d PD A 3 H32A H 1.1738 1.0852 1.0520 0.201 Uiso 0.575(19) 1 calc PR A 3 H32B H 1.2553 1.1027 1.0717 0.201 Uiso 0.575(19) 1 calc PR A 3 C33 C 1.217(2) 1.1829(9) 1.0852(6) 0.145(10) Uani 0.575(19) 1 d PD A 3 H33A H 1.2762 1.2217 1.0871 0.174 Uiso 0.575(19) 1 calc PR A 3 H33B H 1.1941 1.2038 1.0677 0.174 Uiso 0.575(19) 1 calc PR A 3 C34 C 1.1835(13) 1.1747(7) 1.1144(5) 0.141(9) Uani 0.575(19) 1 d PD A 3 H34A H 1.1485 1.1993 1.1136 0.169 Uiso 0.575(19) 1 calc PR A 3 H34B H 1.2250 1.2026 1.1327 0.169 Uiso 0.575(19) 1 calc PR A 3 O2 O 1.1891(18) 1.1003(19) 1.1300(7) 0.211(16) Uani 0.425(19) 1 d PDU A 4 C21 C 1.1134(15) 1.077(3) 1.1136(9) 0.16(2) Uani 0.425(19) 1 d PD A 4 H21A H 1.0821 1.0168 1.1116 0.192 Uiso 0.425(19) 1 calc PR A 4 H21B H 1.0819 1.0940 1.1281 0.192 Uiso 0.425(19) 1 calc PR A 4 C22 C 1.1238(15) 1.107(4) 1.0839(11) 0.23(3) Uani 0.425(19) 1 d PD A 4 H22A H 1.1061 1.1482 1.0834 0.281 Uiso 0.425(19) 1 calc PR A 4 H22B H 1.0926 1.0653 1.0663 0.281 Uiso 0.425(19) 1 calc PR A 4 C23 C 1.2129(19) 1.147(3) 1.0768(8) 0.181(19) Uani 0.425(19) 1 d PD A 4 H23A H 1.2222 1.1234 1.0554 0.218 Uiso 0.425(19) 1 calc PR A 4 H23B H 1.2360 1.2056 1.0732 0.218 Uiso 0.425(19) 1 calc PR A 4 C24 C 1.2463(16) 1.134(3) 1.1023(10) 0.22(2) Uani 0.425(19) 1 d PD A 4 H24A H 1.2936 1.1859 1.1100 0.264 Uiso 0.425(19) 1 calc PR A 4 H24B H 1.2655 1.0966 1.0956 0.264 Uiso 0.425(19) 1 calc PR A 4 O4 O 1.0705(12) 0.9283(11) 1.1919(7) 0.211(12) Uani 0.615(17) 1 d PDU A 1 C41 C 1.0384(12) 0.8564(10) 1.2116(7) 0.204(16) Uani 0.615(17) 1 d PD A 1 H41A H 0.9919 0.8501 1.2256 0.245 Uiso 0.615(17) 1 calc PR A 1 H41B H 1.0187 0.8092 1.1958 0.245 Uiso 0.615(17) 1 calc PR A 1 C42 C 1.0916(19) 0.8587(12) 1.2314(11) 0.29(3) Uani 0.615(17) 1 d PD A 1 H42A H 1.1147 0.8265 1.2217 0.347 Uiso 0.615(17) 1 calc PR A 1 H42B H 1.0688 0.8371 1.2547 0.347 Uiso 0.615(17) 1 calc PR A 1 C43 C 1.1559(14) 0.9476(12) 1.2338(7) 0.191(15) Uani 0.615(17) 1 d PD A 1 H43A H 1.1528 0.9699 1.2566 0.230 Uiso 0.615(17) 1 calc PR A 1 H43B H 1.2105 0.9540 1.2313 0.230 Uiso 0.615(17) 1 calc PR A 1 C44 C 1.1436(19) 0.9842(10) 1.2099(11) 0.32(3) Uani 0.615(17) 1 d PD A 1 H44A H 1.1899 1.0073 1.1936 0.390 Uiso 0.615(17) 1 calc PR A 1 H44B H 1.1380 1.0292 1.2197 0.390 Uiso 0.615(17) 1 calc PR A 1 O5 O 1.092(2) 0.9731(17) 1.2035(5) 0.169(9) Uani 0.385(17) 1 d PDU A 2 C51 C 1.077(3) 0.945(2) 1.2383(7) 0.166(18) Uani 0.385(17) 1 d PD A 2 H51A H 1.1182 0.9865 1.2539 0.199 Uiso 0.385(17) 1 calc PR A 2 H51B H 1.0231 0.9343 1.2456 0.199 Uiso 0.385(17) 1 calc PR A 2 C52 C 1.081(2) 0.8806(14) 1.2403(4) 0.114(12) Uani 0.385(17) 1 d PD A 2 H52A H 1.0259 0.8331 1.2429 0.137 Uiso 0.385(17) 1 calc PR A 2 H52B H 1.1141 0.8828 1.2605 0.137 Uiso 0.385(17) 1 calc PR A 2 C53 C 1.119(4) 0.875(3) 1.2066(9) 0.34(6) Uani 0.385(17) 1 d PD A 2 H53A H 1.1663 0.8687 1.2116 0.404 Uiso 0.385(17) 1 calc PR A 2 H53B H 1.0795 0.8286 1.1927 0.404 Uiso 0.385(17) 1 calc PR A 2 C54 C 1.141(3) 0.940(2) 1.1902(10) 0.17(2) Uani 0.385(17) 1 d PD A 2 H54A H 1.1320 0.9296 1.1649 0.201 Uiso 0.385(17) 1 calc PR A 2 H54B H 1.1994 0.9788 1.1941 0.201 Uiso 0.385(17) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02752(6) 0.02752(6) 0.02601(8) 0.000 0.000 0.01376(3) Ge1 0.03591(17) 0.03319(17) 0.03809(19) -0.00011(17) -0.00238(18) 0.02322(14) Si12 0.0421(5) 0.0475(6) 0.0539(6) -0.0026(5) 0.0059(5) 0.0246(5) Si13 0.0558(7) 0.0567(7) 0.0656(8) -0.0006(6) -0.0182(6) 0.0372(6) Si11 0.0517(6) 0.0343(5) 0.0604(7) 0.0049(5) 0.0010(5) 0.0240(5) C111 0.053(2) 0.042(2) 0.067(3) -0.004(2) -0.001(2) 0.0151(19) C112 0.078(3) 0.067(3) 0.063(3) 0.020(2) 0.005(3) 0.029(3) C113 0.088(4) 0.050(3) 0.130(5) -0.006(3) -0.005(4) 0.046(3) C121 0.049(2) 0.070(3) 0.058(3) 0.016(2) 0.009(2) 0.028(2) C122 0.054(3) 0.090(4) 0.087(4) 0.002(3) 0.018(3) 0.046(3) C123 0.106(5) 0.068(3) 0.065(3) -0.020(3) 0.012(3) 0.031(3) C131 0.070(3) 0.068(3) 0.096(4) 0.009(3) -0.020(3) 0.048(3) C132 0.094(4) 0.109(5) 0.058(3) -0.020(3) -0.031(3) 0.066(4) C133 0.054(3) 0.074(3) 0.125(5) 0.007(3) -0.037(3) 0.034(3) K1 0.1014(12) 0.1014(12) 0.0734(15) 0.000 0.000 0.0507(6) O3 0.105(13) 0.129(12) 0.144(14) 0.044(13) 0.042(12) 0.038(12) C31 0.33(4) 0.093(12) 0.31(4) 0.06(2) 0.22(4) 0.11(2) C32 0.29(4) 0.073(11) 0.137(18) -0.017(12) 0.05(2) 0.087(18) C33 0.22(2) 0.059(8) 0.15(2) 0.004(9) 0.043(17) 0.059(11) C34 0.167(19) 0.073(9) 0.144(16) 0.001(9) 0.063(14) 0.030(10) O2 0.16(2) 0.20(2) 0.17(2) 0.038(15) 0.000(19) 0.01(2) C21 0.074(15) 0.21(4) 0.13(3) -0.05(3) 0.018(17) 0.018(18) C22 0.10(2) 0.40(8) 0.18(4) 0.06(5) 0.01(2) 0.11(4) C23 0.27(5) 0.14(4) 0.13(3) 0.05(3) 0.12(3) 0.11(5) C24 0.16(3) 0.37(7) 0.17(3) 0.10(4) 0.02(3) 0.17(4) O4 0.179(13) 0.149(13) 0.215(17) 0.056(13) -0.120(13) 0.016(12) C41 0.134(15) 0.095(12) 0.29(3) 0.072(15) -0.115(18) -0.010(10) C42 0.21(3) 0.069(13) 0.46(6) 0.03(2) -0.12(4) -0.024(16) C43 0.131(15) 0.134(15) 0.20(2) 0.052(16) -0.092(17) -0.018(13) C44 0.21(3) 0.081(12) 0.59(8) 0.04(2) -0.28(4) 0.002(14) O5 0.23(2) 0.19(2) 0.144(16) -0.042(15) -0.097(17) 0.147(19) C51 0.28(5) 0.18(3) 0.11(2) 0.04(2) 0.05(3) 0.16(4) C52 0.23(4) 0.094(18) 0.042(8) 0.003(8) -0.011(12) 0.10(2) C53 0.57(13) 0.67(15) 0.13(3) 0.08(5) 0.08(5) 0.58(14) C54 0.18(4) 0.17(3) 0.21(4) 0.10(3) 0.12(3) 0.14(3) _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 Ge1 2.8678(4) 3_675 ? Pb1 Ge1 2.8678(4) 2_765 ? Pb1 Ge1 2.8678(4) . ? Pb1B Ge1 2.8238(14) 2_765 ? Pb1B Ge1 2.8238(14) . ? Pb1B Ge1 2.8238(14) 3_675 ? Ge1 Si13 2.3897(12) . ? Ge1 Si12 2.4003(13) . ? Ge1 Si11 2.4100(11) . ? Si12 C121 1.872(5) . ? Si12 C122 1.884(5) . ? Si12 C123 1.885(5) . ? Si13 C132 1.865(6) . ? Si13 C133 1.885(6) . ? Si13 C131 1.887(5) . ? Si11 C111 1.878(5) . ? Si11 C113 1.880(5) . ? Si11 C112 1.881(5) . ? K1 C21 2.59(3) 3_675 ? K1 C21 2.59(3) 2_765 ? K1 C21 2.59(3) . ? K1 O4 2.66(2) 2_765 ? K1 O4 2.663(19) . ? K1 O4 2.663(19) 3_675 ? K1 O5 2.68(2) . ? K1 O5 2.68(2) 2_765 ? K1 O5 2.68(2) 3_675 ? K1 O3 2.680(15) 3_675 ? K1 O3 2.680(15) 2_765 ? K1 O3 2.680(15) . ? O3 C34 1.434(14) . ? O3 C31 1.431(14) . ? C31 C32 1.250(16) . ? C32 C33 1.497(16) . ? C33 C34 1.263(15) . ? O2 C21 1.425(16) . ? O2 C24 1.425(16) . ? C21 C22 1.251(18) . ? C22 C23 1.50(2) . ? C23 C24 1.255(17) . ? O4 C41 1.411(14) . ? O4 C44 1.440(14) . ? C41 C42 1.251(17) . ? C42 C43 1.519(18) . ? C43 C44 1.241(17) . ? O5 C51 1.415(15) . ? O5 C54 1.446(15) . ? C51 C52 1.262(17) . ? C52 C53 1.51(2) . ? C53 C54 1.259(18) . ? 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 Ge1 Pb1 Ge1 106.146(9) 3_675 2_765 ? Ge1 Pb1 Ge1 106.146(9) 3_675 . ? Ge1 Pb1 Ge1 106.146(9) 2_765 . ? Ge1 Pb1B Ge1 108.56(7) 2_765 . ? Ge1 Pb1B Ge1 108.56(7) 2_765 3_675 ? Ge1 Pb1B Ge1 108.56(7) . 3_675 ? Si13 Ge1 Si12 109.02(5) . . ? Si13 Ge1 Si11 98.08(5) . . ? Si12 Ge1 Si11 104.91(5) . . ? Si13 Ge1 Pb1B 140.58(6) . . ? Si12 Ge1 Pb1B 87.62(8) . . ? Si11 Ge1 Pb1B 112.17(3) . . ? Si13 Ge1 Pb1 105.45(3) . . ? Si12 Ge1 Pb1 128.64(3) . . ? Si11 Ge1 Pb1 106.60(3) . . ? Pb1B Ge1 Pb1 42.99(7) . . ? C121 Si12 C122 107.9(2) . . ? C121 Si12 C123 106.1(3) . . ? C122 Si12 C123 104.6(3) . . ? C121 Si12 Ge1 110.84(16) . . ? C122 Si12 Ge1 113.51(19) . . ? C123 Si12 Ge1 113.34(19) . . ? C132 Si13 C133 105.6(3) . . ? C132 Si13 C131 107.5(3) . . ? C133 Si13 C131 104.0(2) . . ? C132 Si13 Ge1 109.35(19) . . ? C133 Si13 Ge1 117.92(18) . . ? C131 Si13 Ge1 111.78(18) . . ? C111 Si11 C113 104.8(3) . . ? C111 Si11 C112 108.1(2) . . ? C113 Si11 C112 105.0(3) . . ? C111 Si11 Ge1 110.40(16) . . ? C113 Si11 Ge1 117.8(2) . . ? C112 Si11 Ge1 110.13(18) . . ? C21 K1 C21 79.4(13) 3_675 2_765 ? C21 K1 C21 79.4(13) 3_675 . ? C21 K1 C21 79.4(13) 2_765 . ? C21 K1 O4 162.8(11) 3_675 2_765 ? C21 K1 O4 96.5(11) 2_765 2_765 ? C21 K1 O4 83.4(13) . 2_765 ? C21 K1 O4 83.4(13) 3_675 . ? C21 K1 O4 162.8(10) 2_765 . ? C21 K1 O4 96.5(11) . . ? O4 K1 O4 99.6(10) 2_765 . ? C21 K1 O4 96.5(11) 3_675 3_675 ? C21 K1 O4 83.4(13) 2_765 3_675 ? C21 K1 O4 162.8(10) . 3_675 ? O4 K1 O4 99.6(10) 2_765 3_675 ? O4 K1 O4 99.6(10) . 3_675 ? C21 K1 O5 101.4(12) 3_675 . ? C21 K1 O5 174.4(14) 2_765 . ? C21 K1 O5 95.3(10) . . ? O4 K1 O5 81.0(9) 2_765 . ? O4 K1 O5 18.6(5) . . ? O4 K1 O5 101.9(7) 3_675 . ? C21 K1 O5 174.4(14) 3_675 2_765 ? C21 K1 O5 95.3(10) 2_765 2_765 ? C21 K1 O5 101.4(13) . 2_765 ? O4 K1 O5 18.6(5) 2_765 2_765 ? O4 K1 O5 101.9(7) . 2_765 ? O4 K1 O5 81.0(9) 3_675 2_765 ? O5 K1 O5 84.0(7) . 2_765 ? C21 K1 O5 95.3(10) 3_675 3_675 ? C21 K1 O5 101.4(13) 2_765 3_675 ? C21 K1 O5 174.4(14) . 3_675 ? O4 K1 O5 101.9(7) 2_765 3_675 ? O4 K1 O5 81.0(9) . 3_675 ? O4 K1 O5 18.6(5) 3_675 3_675 ? O5 K1 O5 84.0(7) . 3_675 ? O5 K1 O5 84.0(7) 2_765 3_675 ? C21 K1 O3 10.8(9) 3_675 3_675 ? C21 K1 O3 87.3(11) 2_765 3_675 ? C21 K1 O3 88.0(14) . 3_675 ? O4 K1 O3 169.8(6) 2_765 3_675 ? O4 K1 O3 75.8(7) . 3_675 ? O4 K1 O3 90.2(7) 3_675 3_675 ? O5 K1 O3 94.3(6) . 3_675 ? O5 K1 O3 170.5(8) 2_765 3_675 ? O5 K1 O3 86.5(9) 3_675 3_675 ? C21 K1 O3 88.0(14) 3_675 2_765 ? C21 K1 O3 10.8(9) 2_765 2_765 ? C21 K1 O3 87.3(11) . 2_765 ? O4 K1 O3 90.2(7) 2_765 2_765 ? O4 K1 O3 169.8(6) . 2_765 ? O4 K1 O3 75.8(7) 3_675 2_765 ? O5 K1 O3 170.5(7) . 2_765 ? O5 K1 O3 86.5(8) 2_765 2_765 ? O5 K1 O3 94.3(6) 3_675 2_765 ? O3 K1 O3 95.0(8) 3_675 2_765 ? C21 K1 O3 87.3(11) 3_675 . ? C21 K1 O3 88.0(14) 2_765 . ? C21 K1 O3 10.8(9) . . ? O4 K1 O3 75.8(7) 2_765 . ? O4 K1 O3 90.2(8) . . ? O4 K1 O3 169.8(6) 3_675 . ? O5 K1 O3 86.5(9) . . ? O5 K1 O3 94.3(7) 2_765 . ? O5 K1 O3 170.5(7) 3_675 . ? O3 K1 O3 95.0(8) 3_675 . ? O3 K1 O3 95.0(7) 2_765 . ? C34 O3 C31 104.0(12) . . ? C34 O3 K1 134.6(12) . . ? C31 O3 K1 119.4(13) . . ? C32 C31 O3 109.7(10) . . ? C31 C32 C33 108.0(8) . . ? C34 C33 C32 107.3(7) . . ? C33 C34 O3 109.3(10) . . ? C21 O2 C24 103.8(17) . . ? C21 O2 K1 47.9(16) . . ? C24 O2 K1 151.3(18) . . ? C22 C21 O2 110.8(17) . . ? C22 C21 K1 140(2) . . ? O2 C21 K1 108(2) . . ? C21 C22 C23 106.0(14) . . ? C24 C23 C22 108.5(14) . . ? C23 C24 O2 108.9(16) . . ? C41 O4 C44 104.5(13) . . ? C41 O4 K1 131.8(15) . . ? C44 O4 K1 113.4(16) . . ? C42 C41 O4 110.0(14) . . ? C41 C42 C43 105.2(13) . . ? C44 C43 C42 108.1(12) . . ? C43 C44 O4 108.9(12) . . ? C43 C44 K1 147(2) . . ? O4 C44 K1 44.4(12) . . ? C51 O5 C54 102.8(17) . . ? C51 O5 K1 130(2) . . ? C54 O5 K1 119(2) . . ? C52 C51 O5 109.1(16) . . ? C51 C52 C53 105.9(13) . . ? C54 C53 C52 107.4(16) . . ? C53 C54 O5 106.1(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.635 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.065 data_kpbhyp2hge _database_code_depnum_ccdc_archive 'CCDC 750479' #TrackingRef 'Kurzbach_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H121 Ge K O4 Pb Si11' _chemical_formula_weight 1330.27 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' Si Si 0.0817 0.0704 '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' Ge Ge 0.1547 1.8001 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2196(8) _cell_length_b 24.4992(16) _cell_length_c 24.9634(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.7313(16) _cell_angle_gamma 90.00 _cell_volume 7365.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 2.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3195 _exptl_absorpt_correction_T_max 0.3843 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 73489 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.0910 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 29.74 _reflns_number_total 20753 _reflns_number_gt 14048 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-2' _computing_cell_refinement 'Bruker APEX-2' _computing_data_reduction 'Bruker APEX-2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20753 _refine_ls_number_parameters 609 _refine_ls_number_restraints 133 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.004 _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 Pb1A Pb -1.1515(1) 0.921419(5) 1.249511(5) 0.02065(4) Uani 0.9891(5) 1 d P A 1 Pb1B Pb -1.0274(12) 0.9786(6) 1.2779(6) 0.038(5) Uani 0.0109(5) 1 d P A 2 Ge1 Ge -1.22566(5) 1.00651(2) 1.31188(2) 0.0215(2) Uani 0.3189(14) 1 d P . . Ge2 Ge -0.96561(5) 0.87154(2) 1.31704(2) 0.0225(2) Uani 0.3759(14) 1 d P . . Ge3 Ge -1.06711(5) 0.97548(2) 1.16376(2) 0.0224(2) Uani 0.3538(14) 1 d P . . Si1 Si -1.22566(5) 1.00651(2) 1.31188(2) 0.0215(2) Uani 0.68 1 d P . . Si11 Si -1.14403(8) 1.09294(4) 1.33616(4) 0.0275(2) Uani 1 1 d . A . Si12 Si -1.24395(9) 0.96607(4) 1.39623(4) 0.0271(2) Uani 1 1 d . A . Si13 Si -1.41748(8) 1.01861(5) 1.27477(4) 0.0327(3) Uani 1 1 d . A . C121 C -1.3180(4) 1.00821(16) 1.44272(16) 0.0414(10) Uani 1 1 d . . . H12D H -1.3210 0.9877 1.4761 0.062 Uiso 1 1 calc R A . H12E H -1.3936 1.0163 1.4243 0.062 Uiso 1 1 calc R . . H12F H -1.2776 1.0425 1.4517 0.062 Uiso 1 1 calc R . . C131 C -1.5031(3) 1.03780(18) 1.32794(16) 0.0444(11) Uani 1 1 d . . . H13C H -1.5808 1.0422 1.3108 0.067 Uiso 1 1 calc R A . H13D H -1.4754 1.0722 1.3452 0.067 Uiso 1 1 calc R . . H13E H -1.4975 1.0090 1.3555 0.067 Uiso 1 1 calc R . . C122 C -1.3260(3) 0.90107(15) 1.38289(17) 0.0388(10) Uani 1 1 d . . . H12G H -1.3340 0.8840 1.4175 0.058 Uiso 1 1 calc R A . H12H H -1.2871 0.8760 1.3620 0.058 Uiso 1 1 calc R . . H12I H -1.3997 0.9093 1.3622 0.058 Uiso 1 1 calc R . . C112 C -1.0914(4) 1.10010(17) 1.41105(16) 0.0428(11) Uani 1 1 d . . . H11C H -1.0590 1.1365 1.4185 0.064 Uiso 1 1 calc R A . H11D H -1.0347 1.0723 1.4226 0.064 Uiso 1 1 calc R . . H11E H -1.1531 1.0953 1.4311 0.064 Uiso 1 1 calc R . . C132 C -1.4760(3) 0.95295(18) 1.24359(18) 0.0499(12) Uani 1 1 d . . . H13F H -1.5547 0.9580 1.2284 0.075 Uiso 1 1 calc R A . H13G H -1.4683 0.9244 1.2715 0.075 Uiso 1 1 calc R . . H13H H -1.4355 0.9422 1.2146 0.075 Uiso 1 1 calc R . . C111 C -1.2463(4) 1.15056(16) 1.31844(19) 0.0482(11) Uani 1 1 d . . . H11F H -1.2095 1.1854 1.3291 0.072 Uiso 1 1 calc R A . H11G H -1.3089 1.1456 1.3379 0.072 Uiso 1 1 calc R . . H11H H -1.2735 1.1506 1.2792 0.072 Uiso 1 1 calc R . . C123 C -1.1048(3) 0.95069(16) 1.43760(15) 0.0376(10) Uani 1 1 d . . . H12J H -1.1147 0.9340 1.4721 0.056 Uiso 1 1 calc R A . H12K H -1.0624 0.9846 1.4448 0.056 Uiso 1 1 calc R . . H12L H -1.0645 0.9254 1.4175 0.056 Uiso 1 1 calc R . . C113 C -1.0197(3) 1.10588(17) 1.30302(17) 0.0422(10) Uani 1 1 d . . . H11I H -0.9885 1.1418 1.3140 0.063 Uiso 1 1 calc R A . H11J H -1.0419 1.1049 1.2634 0.063 Uiso 1 1 calc R . . H11K H -0.9636 1.0777 1.3143 0.063 Uiso 1 1 calc R . . C133 C -1.4560(3) 1.07140(18) 1.22010(18) 0.0530(12) Uani 1 1 d . . . H13I H -1.5368 1.0719 1.2088 0.079 Uiso 1 1 calc R A . H13J H -1.4205 1.0624 1.1888 0.079 Uiso 1 1 calc R . . H13K H -1.4307 1.1074 1.2342 0.079 Uiso 1 1 calc R . . Si2 Si -0.96561(5) 0.87154(2) 1.31704(2) 0.0225(2) Uani 0.62 1 d P . . Si22 Si -0.81929(8) 0.91210(4) 1.37962(4) 0.0278(2) Uani 1 1 d . A . Si21 Si -1.04059(10) 0.79724(4) 1.36177(5) 0.0341(3) Uani 1 1 d . A . Si23 Si -0.87313(9) 0.81885(4) 1.25856(4) 0.0318(3) Uani 1 1 d . A . C211 C -0.9462(4) 0.73611(16) 1.3750(2) 0.0605(14) Uani 1 1 d . . . H21C H -0.9826 0.7077 1.3933 0.091 Uiso 1 1 calc R A . H21D H -0.8766 0.7469 1.3982 0.091 Uiso 1 1 calc R . . H21E H -0.9302 0.7220 1.3404 0.091 Uiso 1 1 calc R . . C221 C -0.6794(3) 0.90765(17) 1.35826(17) 0.0449(11) Uani 1 1 d . . . H22D H -0.6237 0.9251 1.3858 0.067 Uiso 1 1 calc R A . H22E H -0.6819 0.9263 1.3233 0.067 Uiso 1 1 calc R . . H22F H -0.6597 0.8692 1.3545 0.067 Uiso 1 1 calc R . . C212 C -1.0811(4) 0.81011(16) 1.42999(17) 0.0470(11) Uani 1 1 d . . . H21F H -1.1100 0.7764 1.4434 0.070 Uiso 1 1 calc R A . H21G H -1.1384 0.8384 1.4265 0.070 Uiso 1 1 calc R . . H21H H -1.0159 0.8222 1.4556 0.070 Uiso 1 1 calc R . . C231 C -0.9772(4) 0.77441(16) 1.21401(17) 0.0481(12) Uani 1 1 d . . . H23C H -0.9391 0.7526 1.1898 0.072 Uiso 1 1 calc R A . H23D H -1.0334 0.7975 1.1922 0.072 Uiso 1 1 calc R . . H23E H -1.0133 0.7500 1.2368 0.072 Uiso 1 1 calc R . . C232 C -0.8041(3) 0.86342(17) 1.21310(16) 0.0424(10) Uani 1 1 d . . . H23F H -0.7667 0.8405 1.1895 0.064 Uiso 1 1 calc R A . H23G H -0.7495 0.8869 1.2353 0.064 Uiso 1 1 calc R . . H23H H -0.8602 0.8861 1.1907 0.064 Uiso 1 1 calc R . . C222 C -0.8431(4) 0.98723(15) 1.39079(17) 0.0447(11) Uani 1 1 d . . . H22G H -0.7809 1.0019 1.4167 0.067 Uiso 1 1 calc R A . H22H H -0.9122 0.9920 1.4053 0.067 Uiso 1 1 calc R . . H22I H -0.8485 1.0067 1.3562 0.067 Uiso 1 1 calc R . . C233 C -0.7583(4) 0.77240(17) 1.29273(19) 0.0532(12) Uani 1 1 d . . . H23I H -0.7259 0.7528 1.2650 0.080 Uiso 1 1 calc R A . H23J H -0.7888 0.7461 1.3159 0.080 Uiso 1 1 calc R . . H23K H -0.7007 0.7943 1.3150 0.080 Uiso 1 1 calc R . . C213 C -1.1705(4) 0.77223(18) 1.31700(19) 0.0556(13) Uani 1 1 d . . . H21I H -1.2020 0.7418 1.3349 0.083 Uiso 1 1 calc R A . H21J H -1.1524 0.7599 1.2822 0.083 Uiso 1 1 calc R . . H21K H -1.2247 0.8020 1.3106 0.083 Uiso 1 1 calc R . . C223 C -0.8018(4) 0.87694(17) 1.44774(15) 0.0468(11) Uani 1 1 d . . . H22J H -0.7413 0.8943 1.4727 0.070 Uiso 1 1 calc R A . H22K H -0.7841 0.8384 1.4433 0.070 Uiso 1 1 calc R . . H22L H -0.8709 0.8799 1.4626 0.070 Uiso 1 1 calc R . . Si3 Si -1.06711(5) 0.97548(2) 1.16376(2) 0.0224(2) Uani 0.65 1 d P . . Si31 Si -1.09418(9) 0.91061(4) 1.09151(4) 0.0285(2) Uani 1 1 d . A . Si32 Si -0.88990(8) 1.01741(4) 1.17008(4) 0.0294(2) Uani 1 1 d . A . Si33 Si -1.19485(9) 1.04268(4) 1.12347(4) 0.0319(2) Uani 1 1 d . A . C311 C -0.9803(3) 0.85955(17) 1.08660(17) 0.0464(11) Uani 1 1 d . . . H31C H -1.0030 0.8358 1.0551 0.070 Uiso 1 1 calc R A . H31D H -0.9666 0.8374 1.1198 0.070 Uiso 1 1 calc R . . H31E H -0.9122 0.8790 1.0824 0.070 Uiso 1 1 calc R . . C321 C -0.8024(3) 0.98822(17) 1.12226(17) 0.0448(11) Uani 1 1 d . . . H32D H -0.7310 1.0073 1.1270 0.067 Uiso 1 1 calc R A . H32E H -0.8408 0.9928 1.0847 0.067 Uiso 1 1 calc R . . H32F H -0.7898 0.9493 1.1300 0.067 Uiso 1 1 calc R . . C312 C -1.1199(4) 0.94207(17) 1.02173(16) 0.0464(11) Uani 1 1 d . . . H31F H -1.1303 0.9131 0.9942 0.070 Uiso 1 1 calc R A . H31G H -1.0562 0.9647 1.0169 0.070 Uiso 1 1 calc R . . H31H H -1.1868 0.9648 1.0177 0.070 Uiso 1 1 calc R . . C331 C -1.3365(3) 1.01088(17) 1.10173(18) 0.0480(11) Uani 1 1 d . . . H33C H -1.3888 1.0388 1.0851 0.072 Uiso 1 1 calc R A . H33D H -1.3626 0.9955 1.1335 0.072 Uiso 1 1 calc R . . H33E H -1.3314 0.9819 1.0753 0.072 Uiso 1 1 calc R . . C332 C -1.1590(4) 1.07767(17) 1.06100(17) 0.0573(13) Uani 1 1 d . . . H33F H -1.2165 1.1045 1.0475 0.086 Uiso 1 1 calc R A . H33G H -1.1546 1.0504 1.0327 0.086 Uiso 1 1 calc R . . H33H H -1.0872 1.0962 1.0704 0.086 Uiso 1 1 calc R . . C333 C -1.2092(4) 1.09971(16) 1.17164(17) 0.0438(11) Uani 1 1 d . . . H33I H -1.2624 1.1266 1.1536 0.066 Uiso 1 1 calc R A . H33J H -1.1368 1.1172 1.1829 0.066 Uiso 1 1 calc R . . H33K H -1.2357 1.0852 1.2037 0.066 Uiso 1 1 calc R . . C322 C -0.8954(4) 1.09283(16) 1.1569(2) 0.0515(12) Uani 1 1 d . . . H32G H -0.8197 1.1072 1.1602 0.077 Uiso 1 1 calc R A . H32H H -0.9338 1.1109 1.1835 0.077 Uiso 1 1 calc R . . H32I H -0.9357 1.0998 1.1201 0.077 Uiso 1 1 calc R . . C323 C -0.8110(3) 1.00946(18) 1.24088(16) 0.0432(11) Uani 1 1 d . . . H32J H -0.7380 1.0267 1.2434 0.065 Uiso 1 1 calc R A . H32K H -0.8015 0.9706 1.2496 0.065 Uiso 1 1 calc R . . H32L H -0.8524 1.0269 1.2666 0.065 Uiso 1 1 calc R . . C313 C -1.2195(3) 0.86748(15) 1.09645(15) 0.0349(9) Uani 1 1 d . . . H31I H -1.2305 0.8408 1.0667 0.052 Uiso 1 1 calc R A . H31J H -1.2852 0.8909 1.0938 0.052 Uiso 1 1 calc R . . H31K H -1.2080 0.8482 1.1314 0.052 Uiso 1 1 calc R . . K1 K -1.41109(8) 0.76760(4) 1.07015(5) 0.0572(3) Uani 1 1 d . A . O1 O -1.3153(2) 0.66934(11) 1.05191(11) 0.0404(7) Uani 1 1 d . . . C11 C -1.1971(4) 0.66334(17) 1.0624(2) 0.0517(12) Uani 1 1 d . A . H11A H -1.1715 0.6467 1.0306 0.062 Uiso 1 1 calc R . . H11B H -1.1747 0.6392 1.0942 0.062 Uiso 1 1 calc R . . C12 C -1.1455(4) 0.71848(19) 1.0735(2) 0.0682(15) Uani 1 1 d . . . H12A H -1.0645 0.7149 1.0807 0.102 Uiso 1 1 calc R A . H12B H -1.1706 0.7346 1.1053 0.102 Uiso 1 1 calc R . . H12C H -1.1676 0.7421 1.0419 0.102 Uiso 1 1 calc R . . C13 C -1.3683(5) 0.6179(2) 1.0421(2) 0.0634(14) Uani 1 1 d . A . H13A H -1.3535 0.5952 1.0753 0.076 Uiso 1 1 calc R . . H13B H -1.3390 0.5985 1.0127 0.076 Uiso 1 1 calc R . . C14 C -1.4897(5) 0.6270(3) 1.0261(3) 0.119(3) Uani 1 1 d . . . H14A H -1.5273 0.5918 1.0186 0.178 Uiso 1 1 calc R A . H14B H -1.5036 0.6497 0.9933 0.178 Uiso 1 1 calc R . . H14C H -1.5184 0.6454 1.0557 0.178 Uiso 1 1 calc R . . O2 O -1.6160(3) 0.81248(16) 1.06040(17) 0.0851(12) Uani 1 1 d . . . C21 C -1.6505(5) 0.8629(2) 1.0729(2) 0.0796(17) Uani 1 1 d . A . H21A H -1.6822 0.8610 1.1069 0.095 Uiso 1 1 calc R . . H21B H -1.7093 0.8759 1.0435 0.095 Uiso 1 1 calc R . . C22 C -1.5583(5) 0.9008(3) 1.0799(4) 0.133(3) Uani 1 1 d . . . H22A H -1.5839 0.9369 1.0893 0.199 Uiso 1 1 calc R A . H22B H -1.5281 0.9032 1.0461 0.199 Uiso 1 1 calc R . . H22C H -1.5003 0.8878 1.1092 0.199 Uiso 1 1 calc R . . C23 C -1.7078(8) 0.7772(4) 1.0443(7) 0.317(12) Uani 1 1 d . A . H23A H -1.7702 0.8025 1.0463 0.380 Uiso 1 1 calc R . . H23B H -1.7061 0.7739 1.0050 0.380 Uiso 1 1 calc R . . C24 C -1.7417(12) 0.7428(5) 1.0510(5) 0.288(10) Uani 1 1 d . . . H24A H -1.7989 0.7336 1.0199 0.432 Uiso 1 1 calc R A . H24B H -1.7756 0.7458 1.0838 0.432 Uiso 1 1 calc R . . H24C H -1.6849 0.7142 1.0562 0.432 Uiso 1 1 calc R . . O3 O -1.4136(4) 0.79447(17) 0.96500(16) 0.0938(14) Uani 1 1 d . . . C31 C -1.3884(7) 0.7540(3) 0.9285(3) 0.132(3) Uani 1 1 d . A . H31A H -1.3550 0.7217 0.9489 0.159 Uiso 1 1 calc R . . H31B H -1.3345 0.7684 0.9065 0.159 Uiso 1 1 calc R . . C32 C -1.4925(8) 0.7385(4) 0.8929(4) 0.221(6) Uani 1 1 d . . . H32A H -1.4775 0.7096 0.8680 0.332 Uiso 1 1 calc R A . H32B H -1.5234 0.7704 0.8719 0.332 Uiso 1 1 calc R . . H32C H -1.5459 0.7253 0.9151 0.332 Uiso 1 1 calc R . . C33 C -1.4522(12) 0.8503(6) 0.9422(5) 0.287(10) Uani 1 1 d . A . H33A H -1.5158 0.8468 0.9121 0.345 Uiso 1 1 calc R . . H33B H -1.4737 0.8740 0.9708 0.345 Uiso 1 1 calc R . . C34 C -1.3640(10) 0.8695(6) 0.9247(5) 0.293(11) Uani 1 1 d . . . H34A H -1.3816 0.9052 0.9075 0.439 Uiso 1 1 calc R A . H34B H -1.3419 0.8442 0.8981 0.439 Uiso 1 1 calc R . . H34C H -1.3030 0.8736 0.9554 0.439 Uiso 1 1 calc R . . O4A O -1.4302(9) 0.7339(4) 1.1703(3) 0.055(3) Uani 0.571(11) 1 d PDU A 3 C41A C -1.3960(9) 0.6784(4) 1.1812(6) 0.089(4) Uani 0.571(11) 1 d PDU A 3 H41A H -1.4354 0.6643 1.2099 0.107 Uiso 0.571(11) 1 calc PR A 3 H41B H -1.4216 0.6568 1.1479 0.107 Uiso 0.571(11) 1 calc PR A 3 C42A C -1.2884(11) 0.6689(7) 1.1967(8) 0.085(6) Uani 0.571(11) 1 d PDU A 3 H42A H -1.2783 0.6337 1.2154 0.128 Uiso 0.571(11) 1 calc PR A 3 H42B H -1.2558 0.6979 1.2214 0.128 Uiso 0.571(11) 1 calc PR A 3 H42C H -1.2517 0.6681 1.1647 0.128 Uiso 0.571(11) 1 calc PR A 3 C43A C -1.4921(11) 0.7563(4) 1.2079(6) 0.103(5) Uani 0.571(11) 1 d PDU A 3 H43A H -1.5709 0.7559 1.1901 0.123 Uiso 0.571(11) 1 calc PR A 3 H43B H -1.4855 0.7306 1.2388 0.123 Uiso 0.571(11) 1 calc PR A 3 C44A C -1.4719(9) 0.8054(6) 1.2286(8) 0.125(7) Uani 0.571(11) 1 d PDU A 3 H44A H -1.5330 0.8166 1.2471 0.187 Uiso 0.571(11) 1 calc PR A 3 H44B H -1.4655 0.8314 1.1994 0.187 Uiso 0.571(11) 1 calc PR A 3 H44C H -1.4024 0.8049 1.2547 0.187 Uiso 0.571(11) 1 calc PR A 3 O4B O -1.3967(15) 0.7377(6) 1.1767(5) 0.095(6) Uani 0.429(11) 1 d PDU A 4 C41B C -1.3723(9) 0.6946(5) 1.2159(5) 0.046(3) Uani 0.429(11) 1 d PDU A 4 H41C H -1.3651 0.7110 1.2526 0.055 Uiso 0.429(11) 1 calc PR A 4 H41D H -1.4371 0.6698 1.2116 0.055 Uiso 0.429(11) 1 calc PR A 4 C42B C -1.2826(11) 0.6647(7) 1.2144(11) 0.094(10) Uani 0.429(11) 1 d PDU A 4 H42D H -1.2762 0.6365 1.2426 0.141 Uiso 0.429(11) 1 calc PR A 4 H42E H -1.2166 0.6881 1.2207 0.141 Uiso 0.429(11) 1 calc PR A 4 H42F H -1.2885 0.6473 1.1786 0.141 Uiso 0.429(11) 1 calc PR A 4 C43B C -1.4204(13) 0.7876(6) 1.2013(7) 0.131(7) Uani 0.429(11) 1 d PDU A 4 H43C H -1.3656 0.7917 1.2351 0.157 Uiso 0.429(11) 1 calc PR A 4 H43D H -1.4065 0.8175 1.1767 0.157 Uiso 0.429(11) 1 calc PR A 4 C44B C -1.5198(13) 0.7955(9) 1.2138(10) 0.143(11) Uani 0.429(11) 1 d PDU A 4 H44D H -1.5233 0.8319 1.2297 0.215 Uiso 0.429(11) 1 calc PR A 4 H44E H -1.5340 0.7678 1.2402 0.215 Uiso 0.429(11) 1 calc PR A 4 H44F H -1.5760 0.7925 1.1809 0.215 Uiso 0.429(11) 1 calc PR A 4 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 Pb1A 0.01886(6) 0.02130(7) 0.02072(7) -0.00229(6) 0.00030(4) -0.00217(6) Pb1B 0.035(9) 0.032(8) 0.046(10) 0.006(6) 0.008(6) 0.011(6) Ge1 0.0195(3) 0.0215(4) 0.0230(4) -0.0011(3) 0.0020(2) -0.0001(3) Ge2 0.0233(3) 0.0190(3) 0.0237(4) -0.0019(2) -0.0004(2) 0.0008(2) Ge3 0.0203(3) 0.0253(4) 0.0207(4) 0.0004(2) 0.0004(2) -0.0011(3) Si1 0.0195(3) 0.0215(4) 0.0230(4) -0.0011(3) 0.0020(2) -0.0001(3) Si11 0.0261(5) 0.0220(5) 0.0336(6) 0.0008(4) 0.0033(4) -0.0017(4) Si12 0.0298(6) 0.0243(5) 0.0274(6) -0.0008(4) 0.0058(4) -0.0030(4) Si13 0.0203(5) 0.0428(7) 0.0336(6) -0.0069(5) 0.0004(4) 0.0014(5) C121 0.051(3) 0.045(3) 0.031(2) -0.0027(19) 0.0137(19) 0.002(2) C131 0.021(2) 0.066(3) 0.045(3) -0.005(2) 0.0043(17) 0.005(2) C122 0.040(2) 0.029(2) 0.048(3) 0.0019(19) 0.0072(19) -0.0073(19) C112 0.050(3) 0.038(2) 0.040(3) -0.0064(19) 0.0038(19) -0.018(2) C132 0.029(2) 0.066(3) 0.052(3) -0.019(2) 0.0010(19) -0.006(2) C111 0.045(3) 0.031(2) 0.069(3) -0.002(2) 0.011(2) 0.005(2) C123 0.039(2) 0.038(2) 0.033(2) 0.0067(18) -0.0003(17) -0.0018(19) C113 0.036(2) 0.044(3) 0.048(3) 0.003(2) 0.0115(19) -0.007(2) C133 0.031(2) 0.080(4) 0.045(3) 0.007(2) -0.0028(18) 0.017(2) Si2 0.0233(3) 0.0190(3) 0.0237(4) -0.0019(2) -0.0004(2) 0.0008(2) Si22 0.0270(5) 0.0276(6) 0.0259(6) -0.0016(4) -0.0035(4) -0.0014(4) Si21 0.0401(7) 0.0206(5) 0.0415(7) 0.0009(5) 0.0061(5) -0.0034(5) Si23 0.0345(6) 0.0284(6) 0.0316(6) -0.0058(5) 0.0030(5) 0.0068(5) C211 0.084(4) 0.024(2) 0.078(4) 0.015(2) 0.028(3) 0.015(2) C221 0.029(2) 0.053(3) 0.050(3) -0.006(2) -0.0013(18) -0.003(2) C212 0.054(3) 0.037(2) 0.051(3) 0.009(2) 0.013(2) -0.001(2) C231 0.064(3) 0.039(3) 0.042(3) -0.019(2) 0.010(2) -0.004(2) C232 0.041(3) 0.050(3) 0.037(3) -0.004(2) 0.0073(18) 0.004(2) C222 0.056(3) 0.033(2) 0.043(3) -0.0120(19) 0.002(2) -0.009(2) C233 0.052(3) 0.045(3) 0.060(3) 0.003(2) 0.004(2) 0.022(2) C213 0.060(3) 0.046(3) 0.062(3) -0.016(2) 0.014(2) -0.025(2) C223 0.056(3) 0.049(3) 0.030(2) 0.002(2) -0.0081(19) -0.009(2) Si3 0.0203(3) 0.0253(4) 0.0207(4) 0.0004(2) 0.0004(2) -0.0011(3) Si31 0.0270(5) 0.0341(6) 0.0242(6) -0.0033(4) 0.0031(4) -0.0041(5) Si32 0.0230(5) 0.0307(6) 0.0338(6) 0.0001(5) 0.0028(4) -0.0033(5) Si33 0.0311(6) 0.0321(6) 0.0298(6) 0.0061(5) -0.0024(4) 0.0042(5) C311 0.034(2) 0.055(3) 0.051(3) -0.017(2) 0.007(2) 0.006(2) C321 0.039(3) 0.052(3) 0.046(3) 0.005(2) 0.016(2) -0.007(2) C312 0.058(3) 0.053(3) 0.029(2) -0.003(2) 0.008(2) -0.010(2) C331 0.032(2) 0.049(3) 0.059(3) -0.008(2) -0.006(2) 0.008(2) C332 0.083(4) 0.051(3) 0.035(3) 0.018(2) 0.000(2) -0.001(3) C333 0.044(3) 0.035(2) 0.049(3) 0.000(2) 0.000(2) 0.003(2) C322 0.046(3) 0.037(3) 0.070(3) 0.009(2) 0.005(2) -0.009(2) C323 0.030(2) 0.052(3) 0.044(3) -0.007(2) -0.0046(18) -0.001(2) C313 0.032(2) 0.034(2) 0.037(2) -0.0044(17) 0.0017(17) -0.0083(18) K1 0.0393(6) 0.0418(6) 0.0947(9) 0.0000(5) 0.0230(5) 0.0060(5) O1 0.0418(17) 0.0343(16) 0.0430(18) -0.0006(13) 0.0011(13) -0.0001(14) C11 0.047(3) 0.044(3) 0.063(3) -0.010(2) 0.007(2) 0.015(2) C12 0.040(3) 0.061(3) 0.100(5) -0.017(3) 0.003(3) 0.006(3) C13 0.086(4) 0.055(3) 0.047(3) -0.003(2) 0.007(3) -0.019(3) C14 0.072(5) 0.096(5) 0.171(8) 0.049(5) -0.028(4) -0.041(4) O2 0.056(3) 0.073(3) 0.125(4) -0.010(2) 0.013(2) 0.014(2) C21 0.055(4) 0.092(5) 0.092(5) 0.021(4) 0.013(3) 0.021(3) C22 0.054(4) 0.108(6) 0.245(10) -0.076(6) 0.049(5) -0.023(4) C23 0.067(7) 0.097(8) 0.75(4) -0.061(13) -0.027(11) -0.030(6) C24 0.44(2) 0.227(14) 0.225(14) -0.096(11) 0.129(14) -0.239(15) O3 0.133(4) 0.076(3) 0.071(3) -0.007(2) 0.010(3) 0.021(3) C31 0.143(8) 0.159(8) 0.096(6) 0.023(6) 0.026(5) 0.067(6) C32 0.204(11) 0.180(10) 0.216(11) 0.018(8) -0.148(9) -0.041(8) C33 0.306(19) 0.44(2) 0.127(9) 0.080(13) 0.056(11) 0.269(18) C34 0.209(15) 0.45(2) 0.198(14) 0.097(14) -0.023(10) -0.228(16) O4A 0.047(5) 0.056(5) 0.053(5) -0.015(4) -0.015(3) 0.015(3) C41A 0.083(8) 0.105(9) 0.078(9) 0.006(7) 0.009(7) -0.009(7) C42A 0.084(10) 0.100(11) 0.061(9) -0.036(7) -0.020(7) 0.045(8) C43A 0.157(12) 0.046(6) 0.131(10) -0.022(7) 0.098(9) -0.028(7) C44A 0.025(6) 0.096(9) 0.246(18) -0.105(10) 0.003(9) 0.020(7) O4B 0.089(12) 0.083(9) 0.099(10) -0.016(8) -0.021(7) 0.054(8) C41B 0.041(6) 0.065(8) 0.033(7) -0.019(6) 0.008(5) -0.012(6) C42B 0.101(15) 0.030(8) 0.12(2) -0.004(9) -0.068(12) -0.010(9) C43B 0.125(15) 0.149(16) 0.103(13) -0.006(12) -0.026(11) -0.004(13) C44B 0.047(12) 0.20(3) 0.18(2) 0.08(2) 0.033(13) 0.063(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1A Ge1 2.8403(6) . ? Pb1A Ge3 2.8541(6) . ? Pb1A Ge2 2.8636(6) . ? Ge1 Si12 2.3717(12) . ? Ge1 Si11 2.3752(12) . ? Ge1 Si13 2.3887(12) . ? Ge2 Si23 2.3733(12) . ? Ge2 Si22 2.3834(11) . ? Ge2 Si21 2.3969(12) . ? Ge3 Si33 2.3723(12) . ? Ge3 Si32 2.3777(12) . ? Ge3 Si31 2.3846(12) . ? Si11 C113 1.876(4) . ? Si11 C112 1.880(4) . ? Si11 C111 1.887(4) . ? Si12 C123 1.872(4) . ? Si12 C122 1.881(4) . ? Si12 C121 1.894(4) . ? Si13 C132 1.875(4) . ? Si13 C133 1.881(4) . ? Si13 C131 1.883(4) . ? Si22 C221 1.877(4) . ? Si22 C223 1.886(4) . ? Si22 C222 1.891(4) . ? Si21 C212 1.878(4) . ? Si21 C213 1.883(5) . ? Si21 C211 1.885(4) . ? Si23 C232 1.875(4) . ? Si23 C231 1.887(4) . ? Si23 C233 1.894(4) . ? Si31 C313 1.881(4) . ? Si31 C312 1.882(4) . ? Si31 C311 1.891(4) . ? Si32 C321 1.873(4) . ? Si32 C323 1.875(4) . ? Si32 C322 1.876(4) . ? Si33 C333 1.871(4) . ? Si33 C331 1.892(4) . ? Si33 C332 1.895(4) . ? C313 K1 3.374(4) . ? K1 O4A 2.680(8) . ? K1 O3 2.701(4) . ? K1 O2 2.708(4) . ? K1 O4B 2.734(12) . ? K1 O1 2.748(3) . ? K1 C43B 3.332(18) . ? K1 C12 3.449(5) . ? K1 C41A 3.510(12) . ? O1 C13 1.419(5) . ? O1 C11 1.432(5) . ? C11 C12 1.496(6) . ? C13 C14 1.487(7) . ? O2 C21 1.358(6) . ? O2 C23 1.419(9) . ? C21 C22 1.448(7) . ? C23 C24 0.964(12) . ? O3 C31 1.416(8) . ? O3 C33 1.525(12) . ? C31 C32 1.473(10) . ? C33 C34 1.316(15) . ? O4A C43A 1.412(9) . ? O4A C41A 1.433(8) . ? C41A C42A 1.327(10) . ? C43A C44A 1.316(12) . ? O4B C43B 1.420(10) . ? O4B C41B 1.438(9) . ? C41B C42B 1.325(10) . ? C43B C44B 1.319(12) . ? 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 Ge1 Pb1A Ge3 105.051(18) . . ? Ge1 Pb1A Ge2 106.579(18) . . ? Ge3 Pb1A Ge2 106.760(18) . . ? Si12 Ge1 Si11 104.14(4) . . ? Si12 Ge1 Si13 99.36(4) . . ? Si11 Ge1 Si13 109.30(4) . . ? Si12 Ge1 Pb1A 105.47(3) . . ? Si11 Ge1 Pb1A 129.42(4) . . ? Si13 Ge1 Pb1A 105.17(3) . . ? Si23 Ge2 Si22 104.33(4) . . ? Si23 Ge2 Si21 97.63(4) . . ? Si22 Ge2 Si21 108.35(4) . . ? Si23 Ge2 Pb1A 106.42(3) . . ? Si22 Ge2 Pb1A 129.83(3) . . ? Si21 Ge2 Pb1A 105.70(4) . . ? Si33 Ge3 Si32 104.77(4) . . ? Si33 Ge3 Si31 98.31(4) . . ? Si32 Ge3 Si31 110.27(4) . . ? Si33 Ge3 Pb1A 110.17(3) . . ? Si32 Ge3 Pb1A 126.24(3) . . ? Si31 Ge3 Pb1A 103.68(3) . . ? C113 Si11 C112 104.9(2) . . ? C113 Si11 C111 108.9(2) . . ? C112 Si11 C111 105.4(2) . . ? C113 Si11 Ge1 112.00(14) . . ? C112 Si11 Ge1 113.29(13) . . ? C111 Si11 Ge1 111.97(14) . . ? C123 Si12 C122 109.54(18) . . ? C123 Si12 C121 104.78(19) . . ? C122 Si12 C121 105.93(19) . . ? C123 Si12 Ge1 111.14(13) . . ? C122 Si12 Ge1 108.90(13) . . ? C121 Si12 Ge1 116.28(13) . . ? C132 Si13 C133 104.9(2) . . ? C132 Si13 C131 106.8(2) . . ? C133 Si13 C131 103.8(2) . . ? C132 Si13 Ge1 109.55(14) . . ? C133 Si13 Ge1 118.38(15) . . ? C131 Si13 Ge1 112.53(13) . . ? C221 Si22 C223 105.0(2) . . ? C221 Si22 C222 105.6(2) . . ? C223 Si22 C222 107.96(19) . . ? C221 Si22 Ge2 114.05(14) . . ? C223 Si22 Ge2 111.03(14) . . ? C222 Si22 Ge2 112.66(14) . . ? C212 Si21 C213 105.5(2) . . ? C212 Si21 C211 102.8(2) . . ? C213 Si21 C211 106.0(2) . . ? C212 Si21 Ge2 118.35(13) . . ? C213 Si21 Ge2 108.72(15) . . ? C211 Si21 Ge2 114.45(15) . . ? C232 Si23 C231 107.86(19) . . ? C232 Si23 C233 104.3(2) . . ? C231 Si23 C233 107.0(2) . . ? C232 Si23 Ge2 111.42(13) . . ? C231 Si23 Ge2 109.43(14) . . ? C233 Si23 Ge2 116.32(15) . . ? C313 Si31 C312 106.26(19) . . ? C313 Si31 C311 104.39(19) . . ? C312 Si31 C311 102.7(2) . . ? C313 Si31 Ge3 109.58(12) . . ? C312 Si31 Ge3 114.04(14) . . ? C311 Si31 Ge3 118.72(14) . . ? C321 Si32 C323 107.7(2) . . ? C321 Si32 C322 105.8(2) . . ? C323 Si32 C322 105.4(2) . . ? C321 Si32 Ge3 113.84(14) . . ? C323 Si32 Ge3 109.56(14) . . ? C322 Si32 Ge3 114.11(15) . . ? C333 Si33 C331 108.15(19) . . ? C333 Si33 C332 104.5(2) . . ? C331 Si33 C332 106.1(2) . . ? C333 Si33 Ge3 111.85(14) . . ? C331 Si33 Ge3 109.90(14) . . ? C332 Si33 Ge3 115.83(16) . . ? Si31 C313 K1 160.11(18) . . ? O4A K1 O3 173.2(3) . . ? O4A K1 O2 89.1(2) . . ? O3 K1 O2 87.44(14) . . ? O4A K1 O4B 8.9(6) . . ? O3 K1 O4B 176.7(3) . . ? O2 K1 O4B 95.9(3) . . ? O4A K1 O1 89.47(17) . . ? O3 K1 O1 89.30(11) . . ? O2 K1 O1 138.93(11) . . ? O4B K1 O1 88.1(2) . . ? O4A K1 C43B 26.6(3) . . ? O3 K1 C43B 157.3(3) . . ? O2 K1 C43B 81.0(3) . . ? O4B K1 C43B 24.6(2) . . ? O1 K1 C43B 112.2(3) . . ? O4A K1 C313 102.1(3) . . ? O3 K1 C313 84.60(12) . . ? O2 K1 C313 108.90(11) . . ? O4B K1 C313 94.4(4) . . ? O1 K1 C313 111.51(9) . . ? C43B K1 C313 80.8(3) . . ? O4A K1 C12 95.7(2) . . ? O3 K1 C12 87.98(14) . . ? O2 K1 C12 174.82(14) . . ? O4B K1 C12 88.7(3) . . ? O1 K1 C12 43.38(10) . . ? C43B K1 C12 102.4(3) . . ? C313 K1 C12 68.22(10) . . ? O4A K1 C41A 22.0(2) . . ? O3 K1 C41A 155.5(2) . . ? O2 K1 C41A 104.4(2) . . ? O4B K1 C41A 23.0(4) . . ? O1 K1 C41A 67.6(2) . . ? C43B K1 C41A 47.2(4) . . ? C313 K1 C41A 110.8(2) . . ? C12 K1 C41A 80.8(2) . . ? C13 O1 C11 110.9(3) . . ? C13 O1 K1 127.8(3) . . ? C11 O1 K1 120.3(2) . . ? O1 C11 C12 108.8(3) . . ? C11 C12 K1 86.9(3) . . ? O1 C13 C14 108.6(4) . . ? C21 O2 C23 111.0(6) . . ? C21 O2 K1 131.8(3) . . ? C23 O2 K1 116.9(5) . . ? O2 C21 C22 110.2(5) . . ? C24 C23 O2 145.5(19) . . ? C31 O3 C33 118.4(6) . . ? C31 O3 K1 119.1(4) . . ? C33 O3 K1 122.2(5) . . ? O3 C31 C32 108.0(7) . . ? C34 C33 O3 103.1(11) . . ? C43A O4A C41A 114.5(8) . . ? C43A O4A K1 129.8(7) . . ? C41A O4A K1 113.7(6) . . ? C42A C41A O4A 117.7(9) . . ? C42A C41A K1 104.9(9) . . ? O4A C41A K1 44.4(5) . . ? C44A C43A O4A 122.1(10) . . ? C43B O4B C41B 111.7(9) . . ? C43B O4B K1 101.9(8) . . ? C41B O4B K1 146.3(8) . . ? C42B C41B O4B 117.6(10) . . ? C44B C43B O4B 119.5(11) . . ? C44B C43B K1 116.1(14) . . ? O4B C43B K1 53.4(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.74 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.874 _refine_diff_density_min -2.482 _refine_diff_density_rms 0.113 data_kpbhge2hyp _database_code_depnum_ccdc_archive 'CCDC 750480' #TrackingRef 'Kurzbach_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H121 Ge K O4 Pb Si11' _chemical_formula_weight 1330.27 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' Si Si 0.0817 0.0704 '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' Ge Ge 0.1547 1.8001 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.223(2) _cell_length_b 24.446(4) _cell_length_c 24.960(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.962(5) _cell_angle_gamma 90.00 _cell_volume 7345(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 2.965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3187 _exptl_absorpt_correction_T_max 0.3835 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 111571 _diffrn_reflns_av_R_equivalents 0.1034 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 30.71 _reflns_number_total 22597 _reflns_number_gt 16124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-2' _computing_cell_refinement 'Bruker APEX-2' _computing_data_reduction 'Bruker APEX-2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _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^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22597 _refine_ls_number_parameters 599 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.191 _refine_ls_shift/su_max 0.011 _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 Pb1A Pb -1.151715(10) 0.920898(5) 1.249310(5) 0.01891(4) Uani 1 1 d . . . Ge1 Ge -1.22582(4) 1.00598(2) 1.31180(2) 0.01939(18) Uani 0.4602(15) 1 d P . . Ge2 Ge -0.96533(4) 0.87113(2) 1.31703(2) 0.01953(17) Uani 0.5076(15) 1 d P . . Ge3 Ge -1.06745(4) 0.97511(2) 1.16345(2) 0.02003(18) Uani 0.4887(15) 1 d P . . Si1 Si -1.22582(4) 1.00598(2) 1.31180(2) 0.01939(18) Uani 0.54 1 d P . . Si11 Si -1.14403(9) 1.09252(4) 1.33603(4) 0.0249(2) Uani 1 1 d . . . Si12 Si -1.24385(9) 0.96552(4) 1.39633(4) 0.0240(2) Uani 1 1 d . . . Si13 Si -1.41818(9) 1.01827(5) 1.27475(4) 0.0300(2) Uani 1 1 d . . . C121 C -1.3176(4) 1.00769(17) 1.44281(15) 0.0383(10) Uani 1 1 d . . . H12D H -1.3205 0.9871 1.4762 0.058 Uiso 1 1 calc R . . H12E H -1.3933 1.0158 1.4244 0.058 Uiso 1 1 calc R . . H12F H -1.2771 1.0420 1.4519 0.058 Uiso 1 1 calc R . . C131 C -1.5035(3) 1.03740(19) 1.32784(17) 0.0420(11) Uani 1 1 d . . . H13C H -1.5814 1.0418 1.3106 0.063 Uiso 1 1 calc R . . H13D H -1.4758 1.0719 1.3452 0.063 Uiso 1 1 calc R . . H13E H -1.4978 1.0085 1.3554 0.063 Uiso 1 1 calc R . . C122 C -1.3258(3) 0.90050(16) 1.38332(17) 0.0371(10) Uani 1 1 d . . . H12G H -1.3335 0.8836 1.4181 0.056 Uiso 1 1 calc R . . H12H H -1.2870 0.8752 1.3625 0.056 Uiso 1 1 calc R . . H12I H -1.3996 0.9087 1.3626 0.056 Uiso 1 1 calc R . . C112 C -1.0918(4) 1.09999(18) 1.41102(16) 0.0403(10) Uani 1 1 d . . . H11C H -1.0593 1.1364 1.4184 0.060 Uiso 1 1 calc R . . H11D H -1.0352 1.0721 1.4229 0.060 Uiso 1 1 calc R . . H11E H -1.1537 1.0953 1.4309 0.060 Uiso 1 1 calc R . . C132 C -1.4770(3) 0.9523(2) 1.24370(18) 0.0486(12) Uani 1 1 d . . . H13F H -1.5558 0.9573 1.2285 0.073 Uiso 1 1 calc R . . H13G H -1.4691 0.9238 1.2717 0.073 Uiso 1 1 calc R . . H13H H -1.4367 0.9414 1.2147 0.073 Uiso 1 1 calc R . . C111 C -1.2464(4) 1.15022(17) 1.3180(2) 0.0473(12) Uani 1 1 d . . . H11F H -1.2097 1.1852 1.3287 0.071 Uiso 1 1 calc R . . H11G H -1.3090 1.1453 1.3374 0.071 Uiso 1 1 calc R . . H11H H -1.2737 1.1501 1.2787 0.071 Uiso 1 1 calc R . . C123 C -1.1045(3) 0.95021(16) 1.43777(15) 0.0339(9) Uani 1 1 d . . . H12J H -1.1142 0.9335 1.4723 0.051 Uiso 1 1 calc R . . H12K H -1.0621 0.9842 1.4449 0.051 Uiso 1 1 calc R . . H12L H -1.0643 0.9249 1.4177 0.051 Uiso 1 1 calc R . . C113 C -1.0199(3) 1.10561(17) 1.30235(17) 0.0391(10) Uani 1 1 d . . . H11I H -0.9886 1.1416 1.3134 0.059 Uiso 1 1 calc R . . H11J H -1.0429 1.1047 1.2628 0.059 Uiso 1 1 calc R . . H11K H -0.9637 1.0773 1.3134 0.059 Uiso 1 1 calc R . . C133 C -1.4563(4) 1.07080(19) 1.21985(18) 0.0471(12) Uani 1 1 d . . . H13I H -1.5371 1.0714 1.2084 0.071 Uiso 1 1 calc R . . H13J H -1.4209 1.0615 1.1887 0.071 Uiso 1 1 calc R . . H13K H -1.4307 1.1069 1.2338 0.071 Uiso 1 1 calc R . . Si2 Si -0.96533(4) 0.87113(2) 1.31703(2) 0.01953(17) Uani 0.49 1 d P . . Si22 Si -0.81882(9) 0.91192(4) 1.37967(4) 0.0250(2) Uani 1 1 d . . . Si21 Si -1.04009(10) 0.79663(4) 1.36183(5) 0.0318(2) Uani 1 1 d . . . Si23 Si -0.87261(9) 0.81849(4) 1.25858(4) 0.0291(2) Uani 1 1 d . . . C211 C -0.9455(4) 0.73562(17) 1.3753(2) 0.0584(14) Uani 1 1 d . . . H21C H -0.9818 0.7071 1.3936 0.088 Uiso 1 1 calc R . . H21D H -0.8760 0.7465 1.3985 0.088 Uiso 1 1 calc R . . H21E H -0.9296 0.7214 1.3407 0.088 Uiso 1 1 calc R . . C221 C -0.6795(3) 0.90758(19) 1.35870(18) 0.0431(11) Uani 1 1 d . . . H22D H -0.6238 0.9251 1.3863 0.065 Uiso 1 1 calc R . . H22E H -0.6820 0.9263 1.3238 0.065 Uiso 1 1 calc R . . H22F H -0.6597 0.8691 1.3550 0.065 Uiso 1 1 calc R . . C212 C -1.0804(4) 0.80980(17) 1.43042(17) 0.0421(11) Uani 1 1 d . . . H21F H -1.1093 0.7760 1.4439 0.063 Uiso 1 1 calc R . . H21G H -1.1376 0.8383 1.4269 0.063 Uiso 1 1 calc R . . H21H H -1.0150 0.8219 1.4561 0.063 Uiso 1 1 calc R . . C231 C -0.9757(4) 0.77391(18) 1.21418(17) 0.0470(12) Uani 1 1 d . . . H23C H -0.9374 0.7522 1.1901 0.070 Uiso 1 1 calc R . . H23D H -1.0323 0.7969 1.1923 0.070 Uiso 1 1 calc R . . H23E H -1.0114 0.7494 1.2370 0.070 Uiso 1 1 calc R . . C232 C -0.8039(3) 0.86319(18) 1.21325(16) 0.0391(10) Uani 1 1 d . . . H23F H -0.7665 0.8403 1.1897 0.059 Uiso 1 1 calc R . . H23G H -0.7492 0.8868 1.2355 0.059 Uiso 1 1 calc R . . H23H H -0.8600 0.8859 1.1908 0.059 Uiso 1 1 calc R . . C222 C -0.8430(4) 0.98694(16) 1.39058(17) 0.0413(11) Uani 1 1 d . . . H22G H -0.7808 1.0018 1.4166 0.062 Uiso 1 1 calc R . . H22H H -0.9121 0.9916 1.4050 0.062 Uiso 1 1 calc R . . H22I H -0.8487 1.0064 1.3559 0.062 Uiso 1 1 calc R . . C233 C -0.7581(4) 0.77163(19) 1.29218(19) 0.0504(12) Uani 1 1 d . . . H23I H -0.7262 0.7522 1.2642 0.076 Uiso 1 1 calc R . . H23J H -0.7886 0.7451 1.3151 0.076 Uiso 1 1 calc R . . H23K H -0.7002 0.7933 1.3147 0.076 Uiso 1 1 calc R . . C213 C -1.1702(4) 0.77135(19) 1.31703(19) 0.0539(13) Uani 1 1 d . . . H21I H -1.2015 0.7409 1.3350 0.081 Uiso 1 1 calc R . . H21J H -1.1523 0.7588 1.2823 0.081 Uiso 1 1 calc R . . H21K H -1.2245 0.8011 1.3105 0.081 Uiso 1 1 calc R . . C223 C -0.8014(4) 0.87687(18) 1.44755(15) 0.0430(11) Uani 1 1 d . . . H22J H -0.7408 0.8942 1.4726 0.064 Uiso 1 1 calc R . . H22K H -0.7839 0.8382 1.4432 0.064 Uiso 1 1 calc R . . H22L H -0.8705 0.8799 1.4623 0.064 Uiso 1 1 calc R . . Si3 Si -1.06745(4) 0.97511(2) 1.16345(2) 0.02003(18) Uani 0.51 1 d P . . Si31 Si -1.09443(9) 0.91029(4) 1.09095(4) 0.0258(2) Uani 1 1 d . . . Si32 Si -0.88942(8) 1.01701(4) 1.16998(4) 0.0267(2) Uani 1 1 d . . . Si33 Si -1.19523(9) 1.04238(5) 1.12317(4) 0.0293(2) Uani 1 1 d . . . C311 C -0.9803(3) 0.85954(19) 1.08603(17) 0.0444(11) Uani 1 1 d . . . H31C H -1.0030 0.8357 1.0545 0.067 Uiso 1 1 calc R . . H31D H -0.9662 0.8373 1.1192 0.067 Uiso 1 1 calc R . . H31E H -0.9124 0.8792 1.0818 0.067 Uiso 1 1 calc R . . C321 C -0.8025(3) 0.98769(18) 1.12220(17) 0.0408(10) Uani 1 1 d . . . H32D H -0.7310 1.0068 1.1269 0.061 Uiso 1 1 calc R . . H32E H -0.8411 0.9923 1.0846 0.061 Uiso 1 1 calc R . . H32F H -0.7899 0.9487 1.1300 0.061 Uiso 1 1 calc R . . C312 C -1.1205(4) 0.94122(19) 1.02135(16) 0.0432(11) Uani 1 1 d . . . H31F H -1.1308 0.9120 0.9940 0.065 Uiso 1 1 calc R . . H31G H -1.0569 0.9639 1.0164 0.065 Uiso 1 1 calc R . . H31H H -1.1876 0.9639 1.0171 0.065 Uiso 1 1 calc R . . C331 C -1.3371(3) 1.01040(19) 1.10176(18) 0.0455(11) Uani 1 1 d . . . H33C H -1.3897 1.0384 1.0851 0.068 Uiso 1 1 calc R . . H33D H -1.3626 0.9951 1.1337 0.068 Uiso 1 1 calc R . . H33E H -1.3323 0.9812 1.0754 0.068 Uiso 1 1 calc R . . C332 C -1.1600(5) 1.07765(19) 1.06105(18) 0.0553(14) Uani 1 1 d . . . H33F H -1.2178 1.1045 1.0476 0.083 Uiso 1 1 calc R . . H33G H -1.1557 1.0505 1.0326 0.083 Uiso 1 1 calc R . . H33H H -1.0883 1.0963 1.0706 0.083 Uiso 1 1 calc R . . C333 C -1.2094(4) 1.09950(17) 1.17160(18) 0.0426(11) Uani 1 1 d . . . H33I H -1.2627 1.1265 1.1536 0.064 Uiso 1 1 calc R . . H33J H -1.1370 1.1171 1.1829 0.064 Uiso 1 1 calc R . . H33K H -1.2358 1.0848 1.2036 0.064 Uiso 1 1 calc R . . C322 C -0.8950(4) 1.09232(16) 1.1565(2) 0.0464(12) Uani 1 1 d . . . H32G H -0.8193 1.1067 1.1597 0.070 Uiso 1 1 calc R . . H32H H -0.9332 1.1106 1.1829 0.070 Uiso 1 1 calc R . . H32I H -0.9354 1.0991 1.1196 0.070 Uiso 1 1 calc R . . C323 C -0.8114(3) 1.00888(18) 1.24104(16) 0.0387(10) Uani 1 1 d . . . H32J H -0.7382 1.0261 1.2440 0.058 Uiso 1 1 calc R . . H32K H -0.8023 0.9699 1.2498 0.058 Uiso 1 1 calc R . . H32L H -0.8529 1.0264 1.2666 0.058 Uiso 1 1 calc R . . C313 C -1.2206(3) 0.86689(16) 1.09626(16) 0.0342(9) Uani 1 1 d . A . H31I H -1.2321 0.8401 1.0666 0.051 Uiso 1 1 calc R . . H31J H -1.2862 0.8904 1.0937 0.051 Uiso 1 1 calc R . . H31K H -1.2087 0.8477 1.1313 0.051 Uiso 1 1 calc R . . K1 K -1.41079(9) 0.76723(4) 1.07083(5) 0.0557(3) Uani 1 1 d . . . O1 O -1.3152(2) 0.66901(11) 1.05229(11) 0.0387(7) Uani 1 1 d . A . C11 C -1.1973(4) 0.66343(19) 1.0626(2) 0.0503(12) Uani 1 1 d . . . H11A H -1.1722 0.6467 1.0308 0.060 Uiso 1 1 calc R A . H11B H -1.1746 0.6392 1.0944 0.060 Uiso 1 1 calc R . . C12 C -1.1456(4) 0.7175(2) 1.0736(2) 0.0644(15) Uani 1 1 d . A . H12A H -1.0646 0.7135 1.0807 0.097 Uiso 1 1 calc R . . H12B H -1.1700 0.7338 1.1054 0.097 Uiso 1 1 calc R . . H12C H -1.1676 0.7412 1.0419 0.097 Uiso 1 1 calc R . . C13 C -1.3678(5) 0.6174(2) 1.0424(2) 0.0597(14) Uani 1 1 d . . . H13A H -1.3523 0.5944 1.0754 0.072 Uiso 1 1 calc R A . H13B H -1.3395 0.5982 1.0126 0.072 Uiso 1 1 calc R . . C14 C -1.4894(6) 0.6270(3) 1.0269(3) 0.127(3) Uani 1 1 d . A . H14A H -1.5276 0.5919 1.0194 0.190 Uiso 1 1 calc R . . H14B H -1.5037 0.6501 0.9944 0.190 Uiso 1 1 calc R . . H14C H -1.5168 0.6454 1.0569 0.190 Uiso 1 1 calc R . . O2 O -1.6158(3) 0.81165(16) 1.06089(18) 0.0844(13) Uani 1 1 d D A . C21 C -1.6486(5) 0.8641(2) 1.0736(2) 0.0751(17) Uani 1 1 d D . . H21A H -1.7074 0.8774 1.0442 0.090 Uiso 1 1 calc R A . H21B H -1.6800 0.8628 1.1076 0.090 Uiso 1 1 calc R . . C22 C -1.5611(6) 0.8995(3) 1.0801(4) 0.135(4) Uani 1 1 d D A . H22A H -1.5860 0.9359 1.0895 0.203 Uiso 1 1 calc R . . H22B H -1.5315 0.9018 1.0461 0.203 Uiso 1 1 calc R . . H22C H -1.5029 0.8864 1.1093 0.203 Uiso 1 1 calc R . . C23 C -1.7058(8) 0.7831(4) 1.0310(5) 0.288(10) Uani 1 1 d D . . H23A H -1.7682 0.8089 1.0201 0.346 Uiso 1 1 calc R A . H23B H -1.6838 0.7686 0.9974 0.346 Uiso 1 1 calc R . . C24 C -1.7403(11) 0.7420(5) 1.0586(5) 0.251(8) Uani 1 1 d D A . H24A H -1.8014 0.7229 1.0355 0.377 Uiso 1 1 calc R . . H24B H -1.7661 0.7563 1.0909 0.377 Uiso 1 1 calc R . . H24C H -1.6788 0.7165 1.0698 0.377 Uiso 1 1 calc R . . O3 O -1.4154(4) 0.79372(19) 0.96549(18) 0.0957(15) Uani 1 1 d . A . C31 C -1.3894(7) 0.7526(4) 0.9288(3) 0.129(3) Uani 1 1 d . . . H31A H -1.3341 0.7666 0.9075 0.154 Uiso 1 1 calc R A . H31B H -1.3581 0.7198 0.9492 0.154 Uiso 1 1 calc R . . C32 C -1.4907(9) 0.7389(5) 0.8933(5) 0.234(7) Uani 1 1 d . A . H32A H -1.4765 0.7100 0.8682 0.351 Uiso 1 1 calc R . . H32B H -1.5196 0.7714 0.8725 0.351 Uiso 1 1 calc R . . H32C H -1.5454 0.7261 0.9149 0.351 Uiso 1 1 calc R . . C33 C -1.4542(14) 0.8486(9) 0.9430(5) 0.375(17) Uani 1 1 d . . . H33A H -1.5197 0.8454 0.9137 0.450 Uiso 1 1 calc R A . H33B H -1.4723 0.8732 0.9718 0.450 Uiso 1 1 calc R . . C34 C -1.3634(11) 0.8663(7) 0.9235(5) 0.294(11) Uani 1 1 d . A . H34A H -1.3792 0.9019 0.9059 0.441 Uiso 1 1 calc R . . H34B H -1.3450 0.8399 0.8968 0.441 Uiso 1 1 calc R . . H34C H -1.3006 0.8697 0.9535 0.441 Uiso 1 1 calc R . . O4A O -1.4304(10) 0.7338(4) 1.1708(4) 0.055(3) Uani 0.571(11) 1 d PDU A 3 C41A C -1.3965(9) 0.6780(5) 1.1802(6) 0.085(4) Uani 0.571(11) 1 d PDU A 3 H41A H -1.4368 0.6628 1.2080 0.102 Uiso 0.571(11) 1 calc PR A 3 H41B H -1.4212 0.6574 1.1461 0.102 Uiso 0.571(11) 1 calc PR A 3 C42A C -1.2876(11) 0.6684(7) 1.1965(7) 0.079(5) Uani 0.571(11) 1 d PDU A 3 H42A H -1.2776 0.6331 1.2152 0.118 Uiso 0.571(11) 1 calc PR A 3 H42B H -1.2554 0.6975 1.2213 0.118 Uiso 0.571(11) 1 calc PR A 3 H42C H -1.2503 0.6677 1.1647 0.118 Uiso 0.571(11) 1 calc PR A 3 C43A C -1.4918(12) 0.7555(4) 1.2086(6) 0.101(5) Uani 0.571(11) 1 d PDU A 3 H43A H -1.5714 0.7532 1.1921 0.121 Uiso 0.571(11) 1 calc PR A 3 H43B H -1.4804 0.7311 1.2407 0.121 Uiso 0.571(11) 1 calc PR A 3 C44A C -1.4718(9) 0.8069(6) 1.2266(9) 0.117(7) Uani 0.571(11) 1 d PDU A 3 H44A H -1.5318 0.8190 1.2453 0.175 Uiso 0.571(11) 1 calc PR A 3 H44B H -1.4680 0.8312 1.1957 0.175 Uiso 0.571(11) 1 calc PR A 3 H44C H -1.4010 0.8081 1.2519 0.175 Uiso 0.571(11) 1 calc PR A 3 O4B O -1.3994(17) 0.7360(6) 1.1768(5) 0.085(6) Uani 0.429(11) 1 d PDU A 4 C41B C -1.3731(9) 0.6928(5) 1.2162(4) 0.046(3) Uani 0.429(11) 1 d PDU A 4 H41C H -1.3664 0.7092 1.2529 0.056 Uiso 0.429(11) 1 calc PR A 4 H41D H -1.4367 0.6672 1.2117 0.056 Uiso 0.429(11) 1 calc PR A 4 C42B C -1.2806(13) 0.6637(8) 1.2144(11) 0.098(10) Uani 0.429(11) 1 d PDU A 4 H42D H -1.2727 0.6352 1.2424 0.147 Uiso 0.429(11) 1 calc PR A 4 H42E H -1.2159 0.6880 1.2210 0.147 Uiso 0.429(11) 1 calc PR A 4 H42F H -1.2859 0.6467 1.1785 0.147 Uiso 0.429(11) 1 calc PR A 4 C43B C -1.4199(14) 0.7862(6) 1.2013(8) 0.131(7) Uani 0.429(11) 1 d PDU A 4 H43C H -1.3636 0.7906 1.2347 0.157 Uiso 0.429(11) 1 calc PR A 4 H43D H -1.4079 0.8160 1.1761 0.157 Uiso 0.429(11) 1 calc PR A 4 C44B C -1.5209(15) 0.7931(10) 1.2148(14) 0.163(12) Uani 0.429(11) 1 d PDU A 4 H44D H -1.5254 0.8296 1.2306 0.244 Uiso 0.429(11) 1 calc PR A 4 H44E H -1.5329 0.7652 1.2414 0.244 Uiso 0.429(11) 1 calc PR A 4 H44F H -1.5780 0.7896 1.1822 0.244 Uiso 0.429(11) 1 calc PR A 4 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 Pb1A 0.02106(7) 0.01813(6) 0.01738(6) -0.00218(6) 0.00293(4) -0.00207(5) Ge1 0.0215(3) 0.0184(3) 0.0185(3) -0.0008(2) 0.0040(2) 0.0007(2) Ge2 0.0236(3) 0.0151(3) 0.0193(3) -0.0022(2) 0.0022(2) 0.0007(2) Ge3 0.0224(3) 0.0209(3) 0.0168(3) 0.0009(2) 0.0033(2) -0.0006(2) Si1 0.0215(3) 0.0184(3) 0.0185(3) -0.0008(2) 0.0040(2) 0.0007(2) Si11 0.0285(6) 0.0179(5) 0.0286(5) 0.0012(4) 0.0060(4) -0.0016(4) Si12 0.0306(6) 0.0204(5) 0.0225(5) -0.0007(4) 0.0084(4) -0.0023(4) Si13 0.0231(5) 0.0375(6) 0.0288(5) -0.0059(5) 0.0026(4) 0.0015(5) C121 0.054(3) 0.039(2) 0.0246(19) -0.0018(18) 0.0151(18) 0.003(2) C131 0.027(2) 0.059(3) 0.041(2) -0.010(2) 0.0083(18) 0.004(2) C122 0.041(3) 0.029(2) 0.042(2) 0.0047(19) 0.0095(19) -0.0059(18) C112 0.051(3) 0.034(2) 0.035(2) -0.0067(19) 0.0050(19) -0.018(2) C132 0.031(2) 0.063(3) 0.050(3) -0.021(3) 0.0000(19) -0.008(2) C111 0.043(3) 0.031(2) 0.070(3) 0.001(2) 0.014(2) 0.006(2) C123 0.040(2) 0.031(2) 0.030(2) 0.0059(18) 0.0032(17) -0.0004(18) C113 0.033(2) 0.038(2) 0.049(3) 0.003(2) 0.0123(19) -0.0032(19) C133 0.035(2) 0.064(3) 0.040(2) 0.005(2) 0.0002(18) 0.012(2) Si2 0.0236(3) 0.0151(3) 0.0193(3) -0.0022(2) 0.0022(2) 0.0007(2) Si22 0.0278(5) 0.0235(5) 0.0219(5) -0.0018(4) -0.0008(4) -0.0018(4) Si21 0.0421(7) 0.0166(5) 0.0375(6) -0.0001(5) 0.0096(5) -0.0032(5) Si23 0.0366(6) 0.0238(5) 0.0271(5) -0.0063(4) 0.0059(4) 0.0064(4) C211 0.084(4) 0.023(2) 0.075(4) 0.015(2) 0.032(3) 0.013(2) C221 0.028(2) 0.052(3) 0.048(3) -0.006(2) 0.0041(19) -0.0049(19) C212 0.055(3) 0.031(2) 0.044(2) 0.005(2) 0.021(2) -0.002(2) C231 0.064(3) 0.037(3) 0.041(2) -0.021(2) 0.011(2) -0.005(2) C232 0.044(3) 0.045(3) 0.030(2) -0.002(2) 0.0115(18) 0.003(2) C222 0.052(3) 0.027(2) 0.043(2) -0.007(2) 0.002(2) -0.0076(19) C233 0.055(3) 0.040(3) 0.057(3) 0.003(2) 0.010(2) 0.023(2) C213 0.061(3) 0.044(3) 0.058(3) -0.018(2) 0.015(2) -0.029(2) C223 0.052(3) 0.044(3) 0.028(2) 0.004(2) -0.0066(18) -0.004(2) Si3 0.0224(3) 0.0209(3) 0.0168(3) 0.0009(2) 0.0033(2) -0.0006(2) Si31 0.0279(6) 0.0295(6) 0.0204(5) -0.0033(4) 0.0056(4) -0.0043(4) Si32 0.0253(6) 0.0264(5) 0.0289(5) 0.0010(5) 0.0059(4) -0.0028(4) Si33 0.0329(6) 0.0278(6) 0.0256(5) 0.0051(5) 0.0007(4) 0.0035(5) C311 0.040(3) 0.050(3) 0.044(3) -0.018(2) 0.010(2) 0.003(2) C321 0.042(3) 0.044(3) 0.041(2) 0.001(2) 0.0209(19) -0.008(2) C312 0.058(3) 0.048(3) 0.025(2) 0.000(2) 0.0106(19) -0.008(2) C331 0.034(2) 0.047(3) 0.050(3) -0.007(2) -0.005(2) 0.008(2) C332 0.081(4) 0.049(3) 0.034(2) 0.018(2) 0.005(2) 0.001(3) C333 0.048(3) 0.032(2) 0.047(3) -0.001(2) 0.006(2) 0.007(2) C322 0.045(3) 0.028(2) 0.067(3) 0.008(2) 0.012(2) -0.0089(19) C323 0.031(2) 0.047(3) 0.034(2) -0.007(2) -0.0042(17) 0.0006(19) C313 0.036(2) 0.033(2) 0.034(2) -0.0053(18) 0.0060(17) -0.0093(18) K1 0.0414(6) 0.0382(6) 0.0921(9) -0.0005(6) 0.0247(6) 0.0057(5) O1 0.0435(18) 0.0324(16) 0.0393(16) -0.0007(13) 0.0050(13) 0.0004(13) C11 0.050(3) 0.040(3) 0.061(3) -0.007(2) 0.010(2) 0.016(2) C12 0.042(3) 0.056(3) 0.092(4) -0.017(3) 0.002(3) 0.005(2) C13 0.086(4) 0.046(3) 0.046(3) -0.003(2) 0.007(3) -0.020(3) C14 0.081(5) 0.110(6) 0.170(8) 0.061(6) -0.030(5) -0.048(4) O2 0.052(2) 0.069(3) 0.128(4) -0.016(3) 0.005(2) 0.010(2) C21 0.065(4) 0.077(4) 0.082(4) 0.016(4) 0.012(3) 0.019(3) C22 0.063(5) 0.116(7) 0.235(11) -0.080(7) 0.046(6) -0.016(5) C23 0.094(9) 0.154(12) 0.59(3) 0.013(16) -0.007(13) -0.017(8) C24 0.37(2) 0.202(14) 0.212(13) -0.014(11) 0.144(14) -0.147(14) O3 0.137(4) 0.072(3) 0.073(3) -0.010(3) 0.006(3) 0.025(3) C31 0.132(8) 0.153(9) 0.104(6) 0.019(6) 0.027(6) 0.061(7) C32 0.200(12) 0.201(12) 0.236(13) -0.008(10) -0.146(10) -0.020(10) C33 0.36(2) 0.67(4) 0.116(9) 0.132(16) 0.093(12) 0.41(3) C34 0.219(16) 0.48(3) 0.173(13) 0.038(15) 0.013(10) -0.217(18) O4A 0.047(6) 0.055(5) 0.058(5) -0.016(4) -0.009(4) 0.003(4) C41A 0.080(8) 0.094(9) 0.079(8) 0.001(7) 0.008(6) -0.024(7) C42A 0.093(11) 0.083(11) 0.052(8) -0.027(7) -0.013(7) 0.034(8) C43A 0.161(12) 0.036(6) 0.136(10) -0.028(7) 0.115(9) -0.027(7) C44A 0.031(7) 0.074(8) 0.243(17) -0.097(10) 0.019(9) 0.007(6) O4B 0.083(11) 0.070(9) 0.090(9) -0.015(7) -0.017(7) 0.050(8) C41B 0.050(7) 0.060(8) 0.029(6) -0.019(5) 0.007(5) -0.014(6) C42B 0.121(17) 0.037(9) 0.11(2) -0.015(10) -0.062(13) 0.001(10) C43B 0.131(15) 0.142(16) 0.105(13) -0.009(13) -0.017(12) -0.006(13) C44B 0.051(13) 0.19(3) 0.26(3) 0.05(2) 0.083(17) 0.036(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1A Ge1 2.8404(6) . ? Pb1A Ge3 2.8589(6) . ? Pb1A Ge2 2.8626(6) . ? Ge1 Si11 2.3732(12) . ? Ge1 Si12 2.3745(12) . ? Ge1 Si13 2.3919(12) . ? Ge2 Si23 2.3750(12) . ? Ge2 Si22 2.3825(11) . ? Ge2 Si21 2.3992(12) . ? Ge3 Si33 2.3689(12) . ? Ge3 Si31 2.3848(12) . ? Ge3 Si32 2.3851(12) . ? Si11 C112 1.879(4) . ? Si11 C113 1.885(4) . ? Si11 C111 1.888(4) . ? Si12 C123 1.871(4) . ? Si12 C122 1.877(4) . ? Si12 C121 1.893(4) . ? Si13 C133 1.877(4) . ? Si13 C132 1.877(4) . ? Si13 C131 1.882(4) . ? Si22 C221 1.869(4) . ? Si22 C223 1.878(4) . ? Si22 C222 1.885(4) . ? Si21 C211 1.881(4) . ? Si21 C213 1.883(5) . ? Si21 C212 1.889(4) . ? Si23 C232 1.873(4) . ? Si23 C231 1.877(4) . ? Si23 C233 1.889(4) . ? Si31 C312 1.871(4) . ? Si31 C311 1.887(4) . ? Si31 C313 1.895(4) . ? Si32 C322 1.871(4) . ? Si32 C321 1.872(4) . ? Si32 C323 1.873(4) . ? Si33 C333 1.874(4) . ? Si33 C332 1.888(4) . ? Si33 C331 1.892(4) . ? C313 K1 3.352(4) . ? K1 O4A 2.675(8) . ? K1 O3 2.699(5) . ? K1 O2 2.703(4) . ? K1 O4B 2.734(12) . ? K1 O1 2.744(3) . ? K1 C43B 3.31(2) . ? K1 C12 3.452(5) . ? K1 C41A 3.474(13) . ? O1 C13 1.419(5) . ? O1 C11 1.425(5) . ? C11 C12 1.471(6) . ? C13 C14 1.487(8) . ? O2 C21 1.397(5) . ? O2 C23 1.404(6) . ? C21 C22 1.364(7) . ? C23 C24 1.329(8) . ? O3 C31 1.432(9) . ? O3 C33 1.500(16) . ? C31 C32 1.432(10) . ? C33 C34 1.356(19) . ? O4A C43A 1.406(10) . ? O4A C41A 1.434(9) . ? C41A C42A 1.344(10) . ? C43A C44A 1.344(12) . ? O4B C43B 1.412(10) . ? O4B C41B 1.439(9) . ? C41B C42B 1.343(10) . ? C43B C44B 1.346(12) . ? 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 Ge1 Pb1A Ge3 105.23(2) . . ? Ge1 Pb1A Ge2 106.482(18) . . ? Ge3 Pb1A Ge2 106.650(19) . . ? Si11 Ge1 Si12 104.16(4) . . ? Si11 Ge1 Si13 109.21(4) . . ? Si12 Ge1 Si13 99.20(4) . . ? Si11 Ge1 Pb1A 129.23(4) . . ? Si12 Ge1 Pb1A 105.69(3) . . ? Si13 Ge1 Pb1A 105.38(3) . . ? Si23 Ge2 Si22 104.21(4) . . ? Si23 Ge2 Si21 97.80(4) . . ? Si22 Ge2 Si21 108.39(4) . . ? Si23 Ge2 Pb1A 106.44(3) . . ? Si22 Ge2 Pb1A 129.84(3) . . ? Si21 Ge2 Pb1A 105.63(3) . . ? Si33 Ge3 Si31 98.32(4) . . ? Si33 Ge3 Si32 104.93(4) . . ? Si31 Ge3 Si32 110.00(4) . . ? Si33 Ge3 Pb1A 110.08(4) . . ? Si31 Ge3 Pb1A 103.91(3) . . ? Si32 Ge3 Pb1A 126.20(3) . . ? C112 Si11 C113 105.5(2) . . ? C112 Si11 C111 105.1(2) . . ? C113 Si11 C111 108.6(2) . . ? C112 Si11 Ge1 113.33(14) . . ? C113 Si11 Ge1 111.95(14) . . ? C111 Si11 Ge1 111.89(15) . . ? C123 Si12 C122 109.48(19) . . ? C123 Si12 C121 104.75(19) . . ? C122 Si12 C121 105.7(2) . . ? C123 Si12 Ge1 111.04(13) . . ? C122 Si12 Ge1 109.13(14) . . ? C121 Si12 Ge1 116.43(13) . . ? C133 Si13 C132 104.9(2) . . ? C133 Si13 C131 104.3(2) . . ? C132 Si13 C131 106.6(2) . . ? C133 Si13 Ge1 118.12(15) . . ? C132 Si13 Ge1 109.40(15) . . ? C131 Si13 Ge1 112.73(13) . . ? C221 Si22 C223 105.1(2) . . ? C221 Si22 C222 105.6(2) . . ? C223 Si22 C222 108.0(2) . . ? C221 Si22 Ge2 114.23(14) . . ? C223 Si22 Ge2 110.86(14) . . ? C222 Si22 Ge2 112.53(14) . . ? C211 Si21 C213 106.0(2) . . ? C211 Si21 C212 102.8(2) . . ? C213 Si21 C212 105.6(2) . . ? C211 Si21 Ge2 114.40(16) . . ? C213 Si21 Ge2 108.84(16) . . ? C212 Si21 Ge2 118.22(14) . . ? C232 Si23 C231 107.9(2) . . ? C232 Si23 C233 104.3(2) . . ? C231 Si23 C233 106.3(2) . . ? C232 Si23 Ge2 111.50(14) . . ? C231 Si23 Ge2 109.54(15) . . ? C233 Si23 Ge2 116.83(15) . . ? C312 Si31 C311 102.4(2) . . ? C312 Si31 C313 106.33(19) . . ? C311 Si31 C313 104.8(2) . . ? C312 Si31 Ge3 114.53(15) . . ? C311 Si31 Ge3 118.65(14) . . ? C313 Si31 Ge3 109.04(13) . . ? C322 Si32 C321 105.6(2) . . ? C322 Si32 C323 105.8(2) . . ? C321 Si32 C323 108.1(2) . . ? C322 Si32 Ge3 113.95(15) . . ? C321 Si32 Ge3 113.81(14) . . ? C323 Si32 Ge3 109.15(15) . . ? C333 Si33 C332 104.4(2) . . ? C333 Si33 C331 107.9(2) . . ? C332 Si33 C331 106.5(2) . . ? C333 Si33 Ge3 111.79(14) . . ? C332 Si33 Ge3 116.01(17) . . ? C331 Si33 Ge3 109.72(14) . . ? Si31 C313 K1 160.02(19) . . ? O4A K1 O3 172.6(3) . . ? O4A K1 O2 88.7(2) . . ? O3 K1 O2 87.22(15) . . ? O4A K1 O4B 8.1(6) . . ? O3 K1 O4B 177.1(3) . . ? O2 K1 O4B 95.3(4) . . ? O4A K1 O1 89.99(18) . . ? O3 K1 O1 89.05(12) . . ? O2 K1 O1 138.69(11) . . ? O4B K1 O1 88.1(2) . . ? O4A K1 C43B 26.0(4) . . ? O3 K1 C43B 157.9(3) . . ? O2 K1 C43B 81.1(3) . . ? O4B K1 C43B 24.8(2) . . ? O1 K1 C43B 112.1(3) . . ? O4A K1 C313 102.5(3) . . ? O3 K1 C313 84.66(13) . . ? O2 K1 C313 109.09(12) . . ? O4B K1 C313 95.9(4) . . ? O1 K1 C313 111.48(10) . . ? C43B K1 C313 81.5(3) . . ? O4A K1 C12 96.3(2) . . ? O3 K1 C12 87.98(15) . . ? O2 K1 C12 174.84(15) . . ? O4B K1 C12 89.5(4) . . ? O1 K1 C12 43.07(10) . . ? C43B K1 C12 102.8(3) . . ? C313 K1 C12 68.52(11) . . ? O4A K1 C41A 22.5(2) . . ? O3 K1 C41A 154.9(2) . . ? O2 K1 C41A 104.1(2) . . ? O4B K1 C41A 22.7(4) . . ? O1 K1 C41A 67.6(2) . . ? C43B K1 C41A 47.2(4) . . ? C313 K1 C41A 111.6(2) . . ? C12 K1 C41A 81.0(2) . . ? C13 O1 C11 111.1(4) . . ? C13 O1 K1 127.9(3) . . ? C11 O1 K1 120.0(2) . . ? O1 C11 C12 109.7(4) . . ? C11 C12 K1 86.6(3) . . ? O1 C13 C14 107.9(5) . . ? C21 O2 C23 110.3(6) . . ? C21 O2 K1 130.3(3) . . ? C23 O2 K1 118.6(6) . . ? C22 C21 O2 111.1(5) . . ? C24 C23 O2 112.9(8) . . ? C31 O3 C33 118.7(7) . . ? C31 O3 K1 119.0(4) . . ? C33 O3 K1 122.1(5) . . ? C32 C31 O3 107.2(8) . . ? C34 C33 O3 101.2(11) . . ? C43A O4A C41A 114.9(8) . . ? C43A O4A K1 131.0(7) . . ? C41A O4A K1 111.9(6) . . ? C42A C41A O4A 117.3(9) . . ? C42A C41A K1 105.0(9) . . ? O4A C41A K1 45.6(5) . . ? C44A C43A O4A 119.3(10) . . ? C43B O4B C41B 112.2(9) . . ? C43B O4B K1 101.1(8) . . ? C41B O4B K1 146.4(8) . . ? C42B C41B O4B 117.1(10) . . ? C44B C43B O4B 117.2(12) . . ? C44B C43B K1 116.9(16) . . ? O4B C43B K1 54.2(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.71 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.735 _refine_diff_density_min -3.253 _refine_diff_density_rms 0.135