# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 1145/179 data_ge120 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H21 Ge N O12 S16' _chemical_formula_weight 1209.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.45450(10) _cell_length_b 10.99390(10) _cell_length_c 23.0803(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.43 _cell_angle_gamma 90.00 _cell_volume 4328.33(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour black _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 1.543 _exptl_absorpt_correction_type Sadabs _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35583 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9892 _reflns_number_gt 5750 _reflns_threshold_expression >2sigma(I) _computing_data_collection SAINT _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+55.7977P] 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 9892 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1376 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.2282 _refine_ls_wR_factor_gt 0.1879 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.015 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 0.24593(5) -0.00349(7) 0.24580(3) 0.01554(19) Uani 1 1 d . . . S14 S 0.20566(11) 0.13777(16) 0.70709(8) 0.0159(4) Uani 1 1 d . . . S6 S 0.59632(11) 0.13201(17) 0.26808(8) 0.0162(4) Uani 1 1 d . . . S16 S 0.22795(12) -0.14699(18) 0.58319(9) 0.0229(4) Uani 1 1 d . . . S8 S 0.55174(13) 0.15628(18) 0.37839(9) 0.0229(4) Uani 1 1 d . . . S13 S 0.20362(11) -0.12825(16) 0.70162(8) 0.0149(4) Uani 1 1 d . . . S5 S 0.58376(12) -0.13312(17) 0.26120(8) 0.0181(4) Uani 1 1 d . . . S4 S 0.62541(11) -0.13539(16) 0.13907(8) 0.0164(4) Uani 1 1 d . . . S12 S 0.17701(11) -0.13350(17) 0.83444(8) 0.0173(4) Uani 1 1 d . . . S15 S 0.22618(13) 0.17611(19) 0.58790(9) 0.0237(4) Uani 1 1 d . . . S11 S 0.17638(11) 0.13164(17) 0.83376(8) 0.0164(4) Uani 1 1 d . . . S3 S 0.62217(11) 0.13162(16) 0.13607(8) 0.0157(4) Uani 1 1 d . . . S10 S 0.15577(12) 0.15731(18) 0.95484(8) 0.0208(4) Uani 1 1 d . . . S7 S 0.53197(14) -0.16200(18) 0.36622(9) 0.0254(5) Uani 1 1 d . . . S2 S 0.61644(13) 0.15361(19) 0.00672(9) 0.0241(5) Uani 1 1 d . . . S1 S 0.62671(13) -0.16929(18) 0.01345(9) 0.0242(5) Uani 1 1 d . . . S9 S 0.15857(14) -0.16011(19) 0.95512(9) 0.0277(5) Uani 1 1 d . . . C17 C 0.2140(4) -0.0519(7) 0.6387(3) 0.0150(15) Uani 1 1 d . . . C18 C 0.2151(4) 0.0722(7) 0.6414(3) 0.0168(15) Uani 1 1 d . . . C14 C 0.1686(4) -0.0622(7) 0.8990(3) 0.0178(16) Uani 1 1 d . . . C15 C 0.1976(4) 0.0015(6) 0.7410(3) 0.0134(13) Uani 1 1 d . . . C4 C 0.6246(4) -0.0665(7) 0.0705(3) 0.0166(15) Uani 1 1 d . . . C7 C 0.5637(4) -0.0634(7) 0.3213(3) 0.0161(15) Uani 1 1 d . . . C3 C 0.6226(4) 0.0571(7) 0.0691(3) 0.0176(16) Uani 1 1 d . . . C16 C 0.1843(4) -0.0017(7) 0.7972(3) 0.0152(13) Uani 1 1 d . . . C13 C 0.1676(4) 0.0629(7) 0.8986(3) 0.0161(15) Uani 1 1 d . . . C5 C 0.6167(4) -0.0015(7) 0.1748(3) 0.0144(13) Uani 1 1 d . . . C8 C 0.5691(4) 0.0609(7) 0.3241(3) 0.0160(15) Uani 1 1 d . . . C10 C 0.5146(6) -0.0621(8) 0.4220(4) 0.029(2) Uani 1 1 d . . . H10A H 0.4758 -0.1014 0.4360 0.035 Uiso 1 1 calc R . . H10B H 0.5641 -0.0540 0.4591 0.035 Uiso 1 1 calc R . . C2 C 0.6347(6) -0.0681(8) -0.0448(4) 0.030(2) Uani 1 1 d . . . H2A H 0.6893 -0.0378 -0.0308 0.036 Uiso 1 1 calc R . . H2B H 0.6230 -0.1133 -0.0844 0.036 Uiso 1 1 calc R . . C6 C 0.6010(4) -0.0006(7) 0.2299(3) 0.0140(13) Uani 1 1 d . . . C20 C 0.2599(5) 0.0785(8) 0.5416(4) 0.030(2) Uani 1 1 d . . . H20A H 0.2590 0.1244 0.5045 0.036 Uiso 1 1 calc R . . H20B H 0.3151 0.0563 0.5665 0.036 Uiso 1 1 calc R . . C9 C 0.4855(5) 0.0631(8) 0.3987(4) 0.0268(18) Uani 1 1 d . . . H9A H 0.4728 0.1056 0.4315 0.032 Uiso 1 1 calc R . . H9B H 0.4362 0.0552 0.3613 0.032 Uiso 1 1 calc R . . C12 C 0.1336(6) -0.0604(9) 1.0075(4) 0.038(2) Uani 1 1 d . . . H12A H 0.0983 -0.1053 1.0232 0.045 Uiso 1 1 calc R . . H12B H 0.1822 -0.0420 1.0440 0.045 Uiso 1 1 calc R . . C31 C -0.0042(5) -0.0724(9) 0.3901(4) 0.035(2) Uani 1 1 d . . . H31A H -0.0150 -0.1077 0.4235 0.042 Uiso 1 1 calc R . . C19 C 0.2134(6) -0.0363(9) 0.5197(4) 0.036(2) Uani 1 1 d . . . H19A H 0.2284 -0.0746 0.4871 0.043 Uiso 1 1 calc R . . H19B H 0.1570 -0.0153 0.5003 0.043 Uiso 1 1 calc R . . C32 C 0.0163(6) 0.1067(9) 0.3366(4) 0.039(2) Uani 1 1 d . . . H32A H 0.0199 0.1926 0.3336 0.046 Uiso 1 1 calc R . . C30 C 0.0072(5) -0.1457(10) 0.3458(5) 0.041(2) Uani 1 1 d . . . H30A H 0.0042 -0.2317 0.3487 0.049 Uiso 1 1 calc R . . C29 C 0.0270(6) 0.0303(10) 0.2921(5) 0.042(2) Uani 1 1 d . . . H29A H 0.0371 0.0643 0.2581 0.050 Uiso 1 1 calc R . . C28 C -0.0123(6) 0.1300(11) 0.4301(5) 0.048(3) Uani 1 1 d . . . C11 C 0.0955(5) 0.0561(9) 0.9804(4) 0.032(2) Uani 1 1 d . . . H11A H 0.0809 0.0990 1.0120 0.038 Uiso 1 1 calc R . . H11B H 0.0466 0.0382 0.9440 0.038 Uiso 1 1 calc R . . C1 C 0.5811(6) 0.0358(9) -0.0563(4) 0.037(2) Uani 1 1 d . . . H1A H 0.5290 0.0063 -0.0596 0.045 Uiso 1 1 calc R . . H1B H 0.5747 0.0736 -0.0969 0.045 Uiso 1 1 calc R . . N1 N -0.0241(6) 0.1952(10) 0.4674(5) 0.063(3) Uani 1 1 d . . . C27 C 0.0002(5) 0.0538(10) 0.3857(4) 0.035(2) Uani 1 1 d . . . C24 C 0.0229(6) -0.0938(9) 0.2974(5) 0.039(2) Uani 1 1 d . . . H24A H 0.0311 -0.1447 0.2671 0.047 Uiso 1 1 calc R . . O6 O 0.2793(4) -0.1156(5) 0.1992(3) 0.0332(14) Uani 1 1 d . . . O5 O 0.2207(4) 0.1048(5) 0.2981(2) 0.0268(13) Uani 1 1 d . . . O4 O 0.3327(3) 0.0919(5) 0.2498(3) 0.0288(13) Uani 1 1 d . . . O3 O 0.1858(3) 0.0887(5) 0.1750(2) 0.0261(13) Uani 1 1 d . . . O9 O 0.4167(3) 0.1051(6) 0.1999(3) 0.0306(14) Uani 1 1 d . . . O2 O 0.1556(4) -0.0984(5) 0.2296(3) 0.0284(13) Uani 1 1 d . . . O1 O 0.3004(4) -0.0922(6) 0.3190(3) 0.0355(15) Uani 1 1 d . . . O8 O 0.2313(5) 0.1227(7) 0.3977(3) 0.050(2) Uani 1 1 d . . . C45 C 0.3679(5) 0.0516(7) 0.2126(4) 0.0215(16) Uani 1 1 d . . . O7 O 0.0309(4) -0.1077(7) 0.1611(3) 0.0472(19) Uani 1 1 d . . . C44 C 0.2948(6) -0.0449(9) 0.3696(4) 0.036(2) Uani 1 1 d . . . C43 C 0.3408(6) -0.0762(8) 0.1889(4) 0.033(2) Uani 1 1 d . . . C42 C 0.1122(5) 0.0548(8) 0.1496(4) 0.0260(18) Uani 1 1 d . . . C41 C 0.0948(5) -0.0592(9) 0.1800(4) 0.030(2) Uani 1 1 d . . . C40 C 0.2461(6) 0.0696(8) 0.3566(4) 0.030(2) Uani 1 1 d . . . O12 O 0.0615(4) 0.1048(6) 0.1052(3) 0.0363(15) Uani 1 1 d . . . O11 O 0.3739(5) -0.1351(6) 0.1617(4) 0.057(2) Uani 1 1 d . . . O10 O 0.3286(5) -0.0876(8) 0.4227(3) 0.057(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0277(4) 0.0107(3) 0.0146(4) 0.0010(3) 0.0153(3) 0.0010(3) S14 0.0280(10) 0.0111(8) 0.0123(8) 0.0017(6) 0.0118(7) 0.0025(7) S6 0.0278(10) 0.0146(9) 0.0110(8) 0.0017(7) 0.0130(7) 0.0019(7) S16 0.0342(11) 0.0235(10) 0.0156(9) -0.0089(7) 0.0147(8) -0.0031(9) S8 0.0400(12) 0.0175(10) 0.0225(9) -0.0040(7) 0.0247(9) -0.0019(8) S13 0.0253(10) 0.0111(8) 0.0120(8) -0.0025(6) 0.0114(7) -0.0027(7) S5 0.0327(11) 0.0144(9) 0.0134(8) -0.0038(7) 0.0156(8) -0.0048(8) S4 0.0292(10) 0.0136(9) 0.0109(8) -0.0021(7) 0.0125(7) -0.0025(8) S12 0.0294(10) 0.0145(9) 0.0126(8) 0.0007(7) 0.0133(8) -0.0008(8) S15 0.0363(12) 0.0253(10) 0.0162(9) 0.0084(8) 0.0176(8) 0.0035(9) S11 0.0271(10) 0.0156(9) 0.0108(8) -0.0018(7) 0.0119(7) -0.0002(8) S3 0.0255(10) 0.0137(9) 0.0116(8) 0.0000(7) 0.0114(7) 0.0030(7) S10 0.0313(11) 0.0234(10) 0.0144(8) -0.0050(7) 0.0161(8) -0.0033(8) S7 0.0470(13) 0.0177(10) 0.0241(10) 0.0001(8) 0.0275(10) -0.0052(9) S2 0.0414(12) 0.0216(10) 0.0157(9) 0.0085(7) 0.0180(9) 0.0089(9) S1 0.0440(13) 0.0205(10) 0.0160(9) -0.0076(7) 0.0203(9) -0.0066(9) S9 0.0517(14) 0.0217(11) 0.0208(10) 0.0071(8) 0.0260(10) 0.0041(10) C17 0.017(4) 0.023(4) 0.007(3) -0.004(3) 0.006(3) -0.002(3) C18 0.022(4) 0.022(4) 0.009(3) 0.000(3) 0.009(3) 0.001(3) C14 0.023(4) 0.024(4) 0.009(3) 0.000(3) 0.009(3) 0.000(3) C15 0.025(4) 0.010(3) 0.008(3) -0.001(3) 0.010(3) 0.000(3) C4 0.018(4) 0.017(4) 0.018(4) -0.001(3) 0.011(3) 0.000(3) C7 0.029(4) 0.015(4) 0.009(3) -0.001(3) 0.012(3) 0.000(3) C3 0.027(4) 0.022(4) 0.006(3) -0.002(3) 0.008(3) 0.000(3) C16 0.022(4) 0.013(3) 0.013(3) 0.000(3) 0.010(3) -0.003(3) C13 0.020(4) 0.023(4) 0.007(3) -0.003(3) 0.008(3) -0.001(3) C5 0.019(3) 0.015(3) 0.013(3) 0.001(3) 0.009(3) -0.001(3) C8 0.021(4) 0.019(4) 0.009(3) -0.001(3) 0.006(3) 0.000(3) C10 0.047(5) 0.024(5) 0.031(5) 0.003(4) 0.032(4) 0.004(4) C2 0.047(5) 0.033(5) 0.020(4) -0.003(3) 0.023(4) -0.008(4) C6 0.023(3) 0.012(3) 0.008(3) 0.000(3) 0.008(3) -0.005(3) C20 0.036(5) 0.038(5) 0.018(4) 0.003(4) 0.013(4) 0.003(4) C9 0.037(5) 0.028(5) 0.030(4) -0.002(4) 0.028(4) -0.004(4) C12 0.065(7) 0.039(6) 0.030(5) 0.006(4) 0.040(5) 0.001(5) C31 0.026(5) 0.045(6) 0.033(5) 0.003(4) 0.011(4) 0.002(4) C19 0.050(6) 0.045(6) 0.018(4) -0.003(4) 0.021(4) -0.004(5) C32 0.045(6) 0.040(6) 0.038(5) 0.002(4) 0.024(5) -0.001(5) C30 0.031(5) 0.037(6) 0.052(6) 0.003(5) 0.013(5) 0.001(4) C29 0.052(6) 0.050(7) 0.038(5) 0.002(4) 0.032(5) -0.003(5) C28 0.044(6) 0.055(7) 0.051(6) -0.009(5) 0.024(5) 0.000(5) C11 0.035(5) 0.043(5) 0.027(4) -0.008(4) 0.023(4) -0.008(4) C1 0.047(6) 0.049(6) 0.021(4) 0.002(4) 0.019(4) 0.002(5) N1 0.070(7) 0.077(8) 0.053(6) -0.027(6) 0.035(5) -0.012(6) C27 0.028(5) 0.059(6) 0.016(4) 0.002(4) 0.006(4) 0.002(4) C24 0.039(6) 0.039(6) 0.040(5) -0.005(4) 0.017(4) 0.003(4) O6 0.049(4) 0.023(3) 0.043(4) -0.003(3) 0.034(3) -0.002(3) O5 0.044(4) 0.023(3) 0.020(3) 0.004(2) 0.018(3) 0.004(3) O4 0.039(4) 0.028(3) 0.028(3) -0.004(3) 0.022(3) -0.005(3) O3 0.040(3) 0.020(3) 0.019(3) -0.001(2) 0.012(2) -0.003(3) O9 0.032(3) 0.035(4) 0.037(3) -0.005(3) 0.026(3) -0.005(3) O2 0.039(3) 0.022(3) 0.031(3) 0.003(2) 0.022(3) -0.002(3) O1 0.050(4) 0.031(3) 0.035(3) 0.014(3) 0.027(3) 0.012(3) O8 0.091(6) 0.047(4) 0.023(3) -0.002(3) 0.032(4) 0.003(4) C45 0.027(4) 0.021(4) 0.023(4) -0.006(3) 0.017(3) 0.001(3) O7 0.053(4) 0.051(5) 0.034(4) 0.000(3) 0.013(3) -0.023(4) C44 0.043(5) 0.048(6) 0.028(5) 0.014(4) 0.027(4) 0.015(5) C43 0.049(6) 0.023(4) 0.042(5) 0.011(4) 0.031(5) 0.006(4) C42 0.030(5) 0.032(5) 0.017(4) -0.007(3) 0.010(3) -0.005(4) C41 0.031(5) 0.036(5) 0.027(4) -0.008(4) 0.015(4) -0.013(4) C40 0.047(6) 0.032(5) 0.019(4) 0.002(3) 0.021(4) -0.009(4) O12 0.042(4) 0.040(4) 0.026(3) 0.000(3) 0.012(3) 0.001(3) O11 0.104(6) 0.024(4) 0.087(6) 0.008(4) 0.085(5) 0.010(4) O10 0.068(5) 0.078(6) 0.032(4) 0.028(4) 0.028(4) 0.030(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O5 1.876(5) . ? Ge1 O1 1.877(6) . ? Ge1 O2 1.879(6) . ? Ge1 O3 1.883(5) . ? Ge1 O6 1.887(6) . ? Ge1 O4 1.888(6) . ? S14 C15 1.723(7) . ? S14 C18 1.746(7) . ? S6 C6 1.722(7) . ? S6 C8 1.740(7) . ? S16 C17 1.748(7) . ? S16 C19 1.844(9) . ? S8 C8 1.755(7) . ? S8 C9 1.788(8) . ? S13 C15 1.717(7) . ? S13 C17 1.750(7) . ? S5 C6 1.709(7) . ? S5 C7 1.744(7) . ? S4 C5 1.724(7) . ? S4 C4 1.750(7) . ? S12 C16 1.717(7) . ? S12 C14 1.741(7) . ? S15 C18 1.751(7) . ? S15 C20 1.785(9) . ? S11 C16 1.725(7) . ? S11 C13 1.738(7) . ? S3 C5 1.738(7) . ? S3 C3 1.751(7) . ? S10 C13 1.740(7) . ? S10 C11 1.823(9) . ? S7 C7 1.748(7) . ? S7 C10 1.812(8) . ? S2 C3 1.758(7) . ? S2 C1 1.870(9) . ? S1 C4 1.746(7) . ? S1 C2 1.794(8) . ? S9 C14 1.748(7) . ? S9 C12 1.816(9) . ? C17 C18 1.365(11) . ? C14 C13 1.375(11) . ? C15 C16 1.409(9) . ? C4 C3 1.359(10) . ? C7 C8 1.370(10) . ? C5 C6 1.409(9) . ? C10 C9 1.500(12) . ? C2 C1 1.468(13) . ? C20 C19 1.502(13) . ? C12 C11 1.480(13) . ? C31 C30 1.379(13) . ? C31 C27 1.395(14) . ? C32 C29 1.397(13) . ? C32 C27 1.404(12) . ? C30 C24 1.382(13) . ? C29 C24 1.375(14) . ? C28 N1 1.203(13) . ? C28 C27 1.410(14) . ? O6 C43 1.319(10) . ? O5 C40 1.308(9) . ? O4 C45 1.334(9) . ? O3 C42 1.311(10) . ? O9 C45 1.201(9) . ? O2 C41 1.332(11) . ? O1 C44 1.317(10) . ? O8 C40 1.230(10) . ? C45 C43 1.521(12) . ? O7 C41 1.214(10) . ? C44 O10 1.236(10) . ? C44 C40 1.509(13) . ? C43 O11 1.215(10) . ? C42 O12 1.224(10) . ? C42 C41 1.529(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 O5 Ge1 O1 86.0(3) . . ? O5 Ge1 O2 93.5(3) . . ? O1 Ge1 O2 91.2(3) . . ? O5 Ge1 O3 90.5(2) . . ? O1 Ge1 O3 175.7(3) . . ? O2 Ge1 O3 86.7(2) . . ? O5 Ge1 O6 175.1(3) . . ? O1 Ge1 O6 89.7(3) . . ? O2 Ge1 O6 88.9(3) . . ? O3 Ge1 O6 94.0(3) . . ? O5 Ge1 O4 91.7(2) . . ? O1 Ge1 O4 95.3(3) . . ? O2 Ge1 O4 171.9(2) . . ? O3 Ge1 O4 87.2(3) . . ? O6 Ge1 O4 86.3(3) . . ? C15 S14 C18 95.1(3) . . ? C6 S6 C8 94.8(3) . . ? C17 S16 C19 99.8(4) . . ? C8 S8 C9 100.0(4) . . ? C15 S13 C17 95.2(3) . . ? C6 S5 C7 95.2(3) . . ? C5 S4 C4 95.3(3) . . ? C16 S12 C14 95.6(4) . . ? C18 S15 C20 101.0(4) . . ? C16 S11 C13 96.0(3) . . ? C5 S3 C3 94.6(3) . . ? C13 S10 C11 98.2(4) . . ? C7 S7 C10 103.6(4) . . ? C3 S2 C1 96.5(4) . . ? C4 S1 C2 101.3(4) . . ? C14 S9 C12 104.3(4) . . ? C18 C17 S16 128.9(6) . . ? C18 C17 S13 116.5(5) . . ? S16 C17 S13 114.5(4) . . ? C17 C18 S14 116.6(5) . . ? C17 C18 S15 128.5(6) . . ? S14 C18 S15 114.9(4) . . ? C13 C14 S12 116.7(5) . . ? C13 C14 S9 128.0(6) . . ? S12 C14 S9 115.2(4) . . ? C16 C15 S13 122.4(5) . . ? C16 C15 S14 121.0(5) . . ? S13 C15 S14 116.6(4) . . ? C3 C4 S1 129.6(6) . . ? C3 C4 S4 116.3(6) . . ? S1 C4 S4 114.0(4) . . ? C8 C7 S5 116.2(5) . . ? C8 C7 S7 128.8(6) . . ? S5 C7 S7 114.8(4) . . ? C4 C3 S3 117.2(6) . . ? C4 C3 S2 127.9(6) . . ? S3 C3 S2 114.8(4) . . ? C15 C16 S12 123.8(5) . . ? C15 C16 S11 120.4(5) . . ? S12 C16 S11 115.8(4) . . ? C14 C13 S11 115.8(5) . . ? C14 C13 S10 126.6(6) . . ? S11 C13 S10 117.6(4) . . ? C6 C5 S4 121.8(5) . . ? C6 C5 S3 122.1(5) . . ? S4 C5 S3 116.0(4) . . ? C7 C8 S6 116.8(6) . . ? C7 C8 S8 126.8(6) . . ? S6 C8 S8 116.4(4) . . ? C9 C10 S7 115.9(6) . . ? C1 C2 S1 112.1(6) . . ? C5 C6 S5 120.7(5) . . ? C5 C6 S6 122.4(5) . . ? S5 C6 S6 116.9(4) . . ? C19 C20 S15 114.9(6) . . ? C10 C9 S8 115.7(6) . . ? C11 C12 S9 116.2(6) . . ? C30 C31 C27 119.9(9) . . ? C20 C19 S16 113.3(6) . . ? C29 C32 C27 118.5(9) . . ? C31 C30 C24 119.7(10) . . ? C24 C29 C32 120.3(9) . . ? N1 C28 C27 179.0(12) . . ? C12 C11 S10 114.5(6) . . ? C2 C1 S2 112.7(7) . . ? C31 C27 C32 120.5(9) . . ? C31 C27 C28 120.6(9) . . ? C32 C27 C28 119.0(10) . . ? C29 C24 C30 121.1(9) . . ? C43 O6 Ge1 112.3(5) . . ? C40 O5 Ge1 113.5(5) . . ? C45 O4 Ge1 113.3(5) . . ? C42 O3 Ge1 113.7(5) . . ? C41 O2 Ge1 112.6(5) . . ? C44 O1 Ge1 113.3(5) . . ? O9 C45 O4 126.0(7) . . ? O9 C45 C43 122.6(7) . . ? O4 C45 C43 111.4(7) . . ? O10 C44 O1 123.2(9) . . ? O10 C44 C40 123.4(8) . . ? O1 C44 C40 113.4(7) . . ? O11 C43 O6 123.6(9) . . ? O11 C43 C45 121.1(8) . . ? O6 C43 C45 115.2(7) . . ? O12 C42 O3 125.3(8) . . ? O12 C42 C41 121.7(8) . . ? O3 C42 C41 113.1(7) . . ? O7 C41 O2 123.5(8) . . ? O7 C41 C42 122.7(8) . . ? O2 C41 C42 113.8(7) . . ? O8 C40 O5 123.9(9) . . ? O8 C40 C44 122.3(8) . . ? O5 C40 C44 113.7(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.984 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.206 #===END data_Ge296K _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H21 Ge N O12 S16' _chemical_formula_weight 1209.06 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' .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 18.7332(6) _cell_length_b 11.0665(3) _cell_length_c 23.0587(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.5040(10) _cell_angle_gamma 90.00 _cell_volume 4416.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method ? _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 1.512 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37525 _diffrn_reflns_av_R_equivalents 0.1550 _diffrn_reflns_av_sigmaI/netI 0.1563 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.41 _reflns_number_total 10047 _reflns_number_observed 3432 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10047 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2701 _refine_ls_R_factor_obs 0.1071 _refine_ls_wR_factor_all 0.2985 _refine_ls_wR_factor_obs 0.2345 _refine_ls_goodness_of_fit_all 1.179 _refine_ls_goodness_of_fit_obs 1.661 _refine_ls_restrained_S_all 1.179 _refine_ls_restrained_S_obs 1.661 _refine_ls_shift/esd_max 0.829 _refine_ls_shift/esd_mean 0.073 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S16 S 0.20639(18) -0.6280(3) 0.20109(13) 0.0398(8) Uani 1 d . . S15 S 0.20894(19) -0.3649(3) 0.20617(13) 0.0414(8) Uani 1 d . . S14 S 0.1794(2) -0.6330(3) 0.33210(14) 0.0462(9) Uani 1 d . . S13 S 0.18069(18) -0.3707(3) 0.33351(13) 0.0403(8) Uani 1 d . . S12 S 0.1572(2) -0.6601(3) 0.45105(17) 0.0705(12) Uani 1 d . . S11 S 0.1570(2) -0.3473(3) 0.45302(15) 0.0534(10) Uani 1 d . . S10 S 0.2263(2) -0.6477(3) 0.08140(16) 0.0637(11) Uani 1 d . . S9 S 0.2260(2) -0.3284(3) 0.08617(16) 0.0617(11) Uani 1 d . . C19 C 0.2148(7) -0.4298(11) 0.1396(5) 0.045(3) Uani 1 d . . C18 C 0.2157(7) -0.5535(11) 0.1381(5) 0.037(3) Uani 1 d . . C17 C 0.1999(6) -0.4987(10) 0.2400(4) 0.035(2) Uani 1 d . . C16 C 0.1701(7) -0.4412(11) 0.3962(5) 0.042(3) Uani 1 d . . C15 C 0.1884(6) -0.5028(10) 0.2967(5) 0.035(2) Uani 1 d . . C14 C 0.1693(7) -0.5644(12) 0.3966(5) 0.044(3) Uani 1 d . . C13 C 0.1227(12) -0.5625(15) 0.4968(8) 0.118(7) Uani 1 d . . H13A H 0.0791 -0.6028 0.5014 0.142 Uiso 1 calc R . H13B H 0.1632 -0.5578 0.5385 0.142 Uiso 1 calc R . C12 C 0.2516(11) -0.4264(16) 0.0389(7) 0.101(6) Uani 1 d . . H12A H 0.2463 -0.3816 0.0013 0.121 Uiso 1 calc R . H12B H 0.3063 -0.4427 0.0606 0.121 Uiso 1 calc R . C11 C 0.2156(11) -0.5389(15) 0.0187(7) 0.116(8) Uani 1 d . . H11A H 0.2367 -0.5746 -0.0098 0.139 Uiso 1 calc R . H11B H 0.1609 -0.5252 -0.0048 0.139 Uiso 1 calc R . S8 S 0.37978(18) 0.3680(3) 0.36443(13) 0.0400(8) Uani 1 d . . S7 S 0.38011(19) 0.6322(3) 0.36373(13) 0.0409(8) Uani 1 d . . S6 S 0.40550(18) 0.3682(3) 0.23356(13) 0.0384(8) Uani 1 d . . S5 S 0.41567(19) 0.6306(3) 0.23910(14) 0.0430(9) Uani 1 d . . S4 S 0.3812(2) 0.3438(3) 0.49187(15) 0.0601(11) Uani 1 d . . S3 S 0.3799(2) 0.6620(3) 0.48970(15) 0.0620(11) Uani 1 d . . S2 S 0.4618(2) 0.6589(3) 0.13217(16) 0.0618(11) Uani 1 d . . S1 S 0.4473(2) 0.3440(3) 0.12278(16) 0.0581(10) Uani 1 d . . C10 C 0.3867(5) 0.4976(10) 0.3271(4) 0.033(2) Uani 1 d . . C9 C 0.4350(6) 0.5636(10) 0.1805(5) 0.034(3) Uani 1 d . . C8 C 0.4306(6) 0.4403(11) 0.1764(5) 0.036(3) Uani 1 d . . C7 C 0.3813(7) 0.4413(11) 0.4325(5) 0.037(3) Uani 1 d . . C6 C 0.3800(7) 0.5617(10) 0.4322(5) 0.037(3) Uani 1 d . . C5 C 0.4012(5) 0.4987(10) 0.2717(4) 0.032(2) Uani 1 d . . C4 C 0.3755(12) 0.5579(15) 0.5474(7) 0.123(8) Uani 1 d . . H4A H 0.4099 0.5895 0.5877 0.147 Uiso 1 calc R . H4B H 0.3236 0.5644 0.5470 0.147 Uiso 1 calc R . C3 C 0.5038(9) 0.4382(13) 0.0966(7) 0.081(5) Uani 1 d . . H3A H 0.5554 0.4379 0.1290 0.097 Uiso 1 calc R . H3B H 0.5074 0.3994 0.0601 0.097 Uiso 1 calc R . C2 C 0.389(2) 0.4525(15) 0.5484(10) 0.24(2) Uani 1 d . . H2A H 0.3595 0.4182 0.5711 0.293 Uiso 1 calc R . H2B H 0.4426 0.4468 0.5770 0.293 Uiso 1 calc R . C1 C 0.4843(9) 0.5608(13) 0.0802(7) 0.085(5) Uani 1 d . . H1A H 0.4403 0.5613 0.0404 0.101 Uiso 1 calc R . H1B H 0.5271 0.5969 0.0725 0.101 Uiso 1 calc R . C27 C -0.0007(10) -0.556(2) 0.1146(8) 0.081(6) Uani 1 d . . C26 C 0.0063(10) -0.429(2) 0.1089(10) 0.097(6) Uani 1 d . . H26A H 0.0147 -0.3960 0.0750 0.02(3) Uiso 1 calc R . C25 C -0.0139(9) -0.6071(15) 0.1636(8) 0.086(5) Uani 1 d . . H25A H -0.0153 -0.6908 0.1670 0.104 Uiso 1 calc R . C28 C 0.0127(11) -0.629(3) 0.0669(14) 0.169(14) Uani 1 d . . C24 C -0.0251(12) -0.5342(18) 0.2081(10) 0.123(8) Uani 1 d . . H24A H -0.0359 -0.5648 0.2414 0.147 Uiso 1 calc R . C20 C 0.1002(10) -0.4469(15) 0.4779(8) 0.092(5) Uani 1 d . . H20A H 0.0919 -0.4073 0.5123 0.110 Uiso 1 calc R . H20B H 0.0501 -0.4522 0.4436 0.110 Uiso 1 calc R . C21 C 0.0003(11) -0.358(2) 0.1555(12) 0.124(8) Uani 1 d . . H21A H 0.0092 -0.2749 0.1566 0.149 Uiso 1 calc R . C22 C -0.0187(11) -0.412(2) 0.1989(11) 0.118(8) Uani 1 d . . H22A H -0.0292 -0.3613 0.2267 0.142 Uiso 1 calc R . N1 N 0.0133(17) -0.695(3) 0.0178(17) 0.30(2) Uani 1 d . . Ge1 Ge 0.24812(7) -0.50242(12) -0.25229(5) 0.0400(3) Uani 1 d . . O4 O 0.3283(6) -0.4057(7) -0.2520(5) 0.076(3) Uani 1 d . . O3 O 0.2854(7) -0.6140(8) -0.2954(6) 0.106(4) Uani 1 d . . C31 C 0.3635(8) -0.4486(13) -0.2870(6) 0.057(4) Uani 1 d . . O2 O 0.4113(6) -0.3935(8) -0.3006(5) 0.083(3) Uani 1 d . . C30 C 0.3465(10) -0.5695(12) -0.3046(7) 0.072(5) Uani 1 d . . O1 O 0.3799(8) -0.6304(9) -0.3307(6) 0.141(6) Uani 1 d . . O8 O 0.1856(6) -0.4138(8) -0.3245(4) 0.071(3) Uani 1 d . . O7 O 0.2230(7) -0.3967(8) -0.2014(5) 0.083(3) Uani 1 d . . O6 O 0.3003(7) -0.5886(9) -0.1778(5) 0.096(4) Uani 1 d . . O5 O 0.1618(7) -0.5973(8) -0.2670(6) 0.090(4) Uani 1 d . . O12 O 0.2427(9) -0.3753(11) -0.0998(5) 0.142(6) Uani 1 d . . O9 O 0.3312(8) -0.5744(15) -0.0772(6) 0.157(6) Uani 1 d . . C33 C 0.2862(15) -0.544(2) -0.1305(9) 0.172(12) Uani 1 d . . C32 C 0.2612(14) -0.4318(18) -0.1409(7) 0.124(9) Uani 1 d . . C34 C 0.1147(10) -0.4523(17) -0.3446(10) 0.121(8) Uani 1 d . . O10 O 0.0398(8) -0.6102(12) -0.3371(6) 0.141(6) Uani 1 d . . O11 O 0.0664(7) -0.4062(12) -0.3914(6) 0.114(4) Uani 1 d . . C35 C 0.1025(12) -0.5594(18) -0.3210(10) 0.118(8) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S16 0.064(2) 0.0299(17) 0.0347(18) -0.0037(15) 0.0285(17) -0.0038(16) S15 0.071(2) 0.0289(17) 0.0315(17) 0.0072(14) 0.0280(17) 0.0076(16) S14 0.081(3) 0.0293(18) 0.042(2) -0.0013(16) 0.0384(19) -0.0022(17) S13 0.065(2) 0.0339(18) 0.0293(17) -0.0032(15) 0.0263(17) 0.0035(16) S12 0.118(3) 0.061(3) 0.054(2) 0.017(2) 0.057(2) 0.003(2) S11 0.082(3) 0.053(2) 0.044(2) -0.0137(17) 0.044(2) -0.0098(19) S10 0.094(3) 0.068(2) 0.044(2) -0.0243(19) 0.043(2) -0.015(2) S9 0.093(3) 0.062(2) 0.047(2) 0.0219(18) 0.046(2) 0.010(2) C19 0.050(9) 0.049(9) 0.040(8) 0.019(7) 0.023(7) 0.006(7) C18 0.050(8) 0.050(7) 0.016(6) 0.005(6) 0.018(6) -0.005(6) C17 0.051(6) 0.032(5) 0.023(5) -0.003(6) 0.015(5) -0.004(7) C16 0.060(9) 0.046(8) 0.022(7) 0.006(6) 0.019(7) 0.003(7) C15 0.050(6) 0.025(5) 0.039(6) -0.004(7) 0.027(5) -0.001(7) C14 0.044(9) 0.051(8) 0.044(9) 0.001(8) 0.024(7) -0.006(7) C13 0.23(2) 0.074(12) 0.141(17) 0.024(12) 0.168(17) 0.020(14) C12 0.166(18) 0.122(15) 0.041(9) 0.028(10) 0.068(11) 0.040(14) C11 0.177(19) 0.143(18) 0.044(10) -0.029(10) 0.062(11) -0.092(15) S8 0.069(2) 0.0329(17) 0.0283(17) 0.0015(15) 0.0296(17) 0.0058(16) S7 0.071(2) 0.0288(17) 0.0323(17) -0.0055(15) 0.0301(17) -0.0062(16) S6 0.065(2) 0.0314(17) 0.0289(16) 0.0034(14) 0.0291(16) 0.0044(15) S5 0.078(2) 0.0295(17) 0.0377(18) -0.0040(15) 0.0402(18) -0.0075(16) S4 0.106(3) 0.048(2) 0.046(2) 0.0201(17) 0.051(2) 0.020(2) S3 0.109(3) 0.052(2) 0.042(2) -0.0184(18) 0.047(2) -0.013(2) S2 0.115(3) 0.041(2) 0.059(2) -0.0010(17) 0.067(2) -0.009(2) S1 0.110(3) 0.038(2) 0.055(2) -0.0108(17) 0.064(2) -0.0067(19) C10 0.048(6) 0.032(5) 0.023(5) -0.006(6) 0.019(5) 0.004(7) C9 0.045(8) 0.029(7) 0.033(7) -0.014(6) 0.020(7) -0.015(6) C8 0.043(8) 0.045(7) 0.017(6) -0.005(6) 0.009(6) -0.024(6) C7 0.053(9) 0.051(8) 0.012(6) 0.004(6) 0.018(6) 0.008(7) C6 0.054(9) 0.030(7) 0.034(8) -0.008(7) 0.024(7) -0.005(7) C5 0.049(6) 0.029(5) 0.026(5) -0.017(6) 0.024(5) -0.006(6) C4 0.25(2) 0.107(13) 0.054(11) -0.049(11) 0.105(14) -0.103(16) C3 0.118(13) 0.061(10) 0.099(13) -0.017(10) 0.081(11) 0.002(10) C2 0.65(6) 0.062(12) 0.115(18) 0.043(13) 0.25(3) 0.11(2) C1 0.135(14) 0.065(10) 0.112(13) 0.011(10) 0.113(12) 0.028(10) C27 0.061(11) 0.144(17) 0.045(10) 0.014(11) 0.027(9) -0.002(11) C26 0.087(14) 0.124(19) 0.083(15) 0.014(15) 0.035(12) -0.024(14) C25 0.100(13) 0.086(12) 0.093(13) 0.003(11) 0.060(11) -0.006(10) C28 0.062(14) 0.27(4) 0.14(2) 0.10(3) 0.011(15) -0.020(19) C24 0.17(2) 0.117(19) 0.15(2) -0.022(15) 0.132(18) -0.011(14) C20 0.120(14) 0.097(12) 0.101(13) -0.004(11) 0.090(12) -0.004(11) C21 0.080(14) 0.16(2) 0.14(2) 0.03(2) 0.045(15) 0.011(14) C22 0.102(16) 0.13(2) 0.13(2) -0.043(17) 0.060(15) 0.000(15) N1 0.33(4) 0.21(3) 0.51(6) -0.13(3) 0.33(4) -0.06(2) Ge1 0.0698(8) 0.0272(6) 0.0376(6) -0.0011(7) 0.0369(6) 0.0004(8) O4 0.127(8) 0.043(6) 0.108(8) -0.015(5) 0.100(7) -0.016(5) O3 0.205(12) 0.031(5) 0.165(11) 0.000(6) 0.164(10) 0.007(6) C31 0.069(10) 0.061(9) 0.058(9) -0.018(7) 0.046(8) -0.008(7) O2 0.113(8) 0.069(7) 0.112(8) -0.023(6) 0.093(7) -0.027(6) C30 0.136(15) 0.027(8) 0.095(12) 0.012(8) 0.091(12) 0.008(9) O1 0.264(16) 0.045(7) 0.230(15) 0.022(8) 0.226(14) 0.033(8) O8 0.114(8) 0.049(6) 0.047(6) 0.011(5) 0.029(6) 0.014(6) O7 0.171(10) 0.043(6) 0.075(7) 0.000(5) 0.094(7) 0.007(6) O6 0.165(11) 0.065(7) 0.087(8) 0.040(6) 0.080(8) 0.039(7) O5 0.127(10) 0.052(7) 0.139(11) -0.013(7) 0.103(9) -0.021(7) O12 0.297(18) 0.102(10) 0.061(7) -0.015(7) 0.109(10) -0.028(11) O9 0.158(12) 0.263(17) 0.068(8) 0.076(10) 0.063(9) 0.094(12) C33 0.30(3) 0.19(2) 0.063(12) 0.071(13) 0.112(16) 0.20(2) C32 0.25(3) 0.086(14) 0.026(9) -0.020(10) 0.043(13) -0.056(16) C34 0.044(10) 0.106(16) 0.143(18) 0.040(13) -0.043(11) -0.051(10) O10 0.135(11) 0.142(12) 0.110(10) -0.018(9) 0.008(9) -0.077(10) O11 0.105(10) 0.148(12) 0.086(9) 0.006(9) 0.036(8) -0.006(9) C35 0.097(16) 0.090(15) 0.109(16) -0.011(13) -0.024(13) -0.058(12) _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 S16 C17 1.718(11) . ? S16 C18 1.737(11) . ? S15 C17 1.712(11) . ? S15 C19 1.737(12) . ? S14 C15 1.696(11) . ? S14 C14 1.744(12) . ? S13 C16 1.721(11) . ? S13 C15 1.724(11) . ? S12 C14 1.722(12) . ? S12 C13 1.794(14) . ? S11 C16 1.761(12) . ? S11 C20 1.773(14) . ? S10 C18 1.741(12) . ? S10 C11 1.833(15) . ? S9 C12 1.731(15) . ? S9 C19 1.737(11) . ? C19 C18 1.369(15) . ? C17 C15 1.406(13) . ? C16 C14 1.364(14) . ? C13 C20 1.366(18) . ? C12 C11 1.408(19) . ? S8 C10 1.703(11) . ? S8 C7 1.758(10) . ? S7 C10 1.740(10) . ? S7 C6 1.762(11) . ? S6 C5 1.709(10) . ? S6 C8 1.751(10) . ? S5 C9 1.697(10) . ? S5 C5 1.710(11) . ? S4 C7 1.744(11) . ? S4 C2 1.738(17) . ? S3 C6 1.730(11) . ? S3 C4 1.786(15) . ? S2 C9 1.742(11) . ? S2 C1 1.784(12) . ? S1 C8 1.750(11) . ? S1 C3 1.749(14) . ? C10 C5 1.404(12) . ? C9 C8 1.368(13) . ? C7 C6 1.332(13) . ? C4 C2 1.19(2) . ? C3 C1 1.418(17) . ? C27 C25 1.37(2) . ? C27 C26 1.42(2) . ? C27 C28 1.46(4) . ? C26 C21 1.37(2) . ? C25 C24 1.38(2) . ? C28 N1 1.35(4) . ? C24 C22 1.38(3) . ? C21 C22 1.33(3) . ? Ge1 O7 1.842(8) . ? Ge1 O5 1.847(10) . ? Ge1 O4 1.841(8) . ? Ge1 O6 1.880(9) . ? Ge1 O3 1.879(9) . ? Ge1 O8 1.900(9) . ? O4 C31 1.312(13) . ? O3 C30 1.336(16) . ? C31 O2 1.219(14) . ? C31 C30 1.399(17) . ? C30 O1 1.222(15) . ? O8 C34 1.301(16) . ? O7 C32 1.357(18) . ? O6 C33 1.310(17) . ? O5 C35 1.378(19) . ? O12 C32 1.29(2) . ? O9 C33 1.241(19) . ? C33 C32 1.32(2) . ? C34 O11 1.222(18) . ? C34 C35 1.36(2) . ? O10 C35 1.226(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 C17 S16 C18 95.2(5) . . ? C17 S15 C19 95.5(5) . . ? C15 S14 C14 95.9(5) . . ? C16 S13 C15 95.0(5) . . ? C14 S12 C13 103.7(7) . . ? C16 S11 C20 98.4(6) . . ? C18 S10 C11 100.9(7) . . ? C12 S9 C19 100.3(7) . . ? C18 C19 S9 128.5(10) . . ? C18 C19 S15 116.2(9) . . ? S9 C19 S15 115.1(7) . . ? C19 C18 S16 116.6(9) . . ? C19 C18 S10 128.5(9) . . ? S16 C18 S10 114.9(7) . . ? C15 C17 S15 121.9(8) . . ? C15 C17 S16 121.7(8) . . ? S15 C17 S16 116.3(5) . . ? C14 C16 S13 117.6(10) . . ? C14 C16 S11 125.5(10) . . ? S13 C16 S11 116.8(7) . . ? C17 C15 S14 123.6(8) . . ? C17 C15 S13 120.2(8) . . ? S14 C15 S13 116.2(6) . . ? C16 C14 S12 128.6(10) . . ? C16 C14 S14 115.1(10) . . ? S12 C14 S14 116.2(7) . . ? C20 C13 S12 120.8(12) . . ? C11 C12 S9 123.3(14) . . ? C12 C11 S10 115.2(11) . . ? C10 S8 C7 94.8(5) . . ? C10 S7 C6 94.6(5) . . ? C5 S6 C8 94.7(5) . . ? C9 S5 C5 95.5(5) . . ? C7 S4 C2 97.8(7) . . ? C6 S3 C4 99.9(7) . . ? C9 S2 C1 105.2(6) . . ? C8 S1 C3 100.2(6) . . ? C5 C10 S8 123.1(8) . . ? C5 C10 S7 120.6(8) . . ? S8 C10 S7 116.3(5) . . ? C8 C9 S5 117.7(9) . . ? C8 C9 S2 125.8(9) . . ? S5 C9 S2 116.5(6) . . ? C9 C8 S1 129.3(9) . . ? C9 C8 S6 115.4(9) . . ? S1 C8 S6 115.3(7) . . ? C6 C7 S4 128.2(9) . . ? C6 C7 S8 117.5(9) . . ? S4 C7 S8 114.3(7) . . ? C7 C6 S3 129.9(10) . . ? C7 C6 S7 116.3(9) . . ? S3 C6 S7 113.8(7) . . ? C10 C5 S5 121.7(8) . . ? C10 C5 S6 121.6(8) . . ? S5 C5 S6 116.6(5) . . ? C2 C4 S3 125.1(15) . . ? C1 C3 S1 122.4(11) . . ? C4 C2 S4 135.0(17) . . ? C3 C1 S2 120.4(11) . . ? C25 C27 C26 123(2) . . ? C25 C27 C28 122(2) . . ? C26 C27 C28 115(2) . . ? C21 C26 C27 117(2) . . ? C27 C25 C24 119.7(19) . . ? N1 C28 C27 171(2) . . ? C22 C24 C25 114.2(18) . . ? C13 C20 S11 122.4(13) . . ? C22 C21 C26 117(3) . . ? C21 C22 C24 129(2) . . ? O7 Ge1 O5 93.3(4) . . ? O7 Ge1 O4 92.0(4) . . ? O5 Ge1 O4 170.4(5) . . ? O7 Ge1 O6 84.8(4) . . ? O5 Ge1 O6 89.6(6) . . ? O4 Ge1 O6 98.8(5) . . ? O7 Ge1 O3 172.7(6) . . ? O5 Ge1 O3 90.4(4) . . ? O4 Ge1 O3 85.2(4) . . ? O6 Ge1 O3 88.9(5) . . ? O7 Ge1 O8 90.5(4) . . ? O5 Ge1 O8 86.0(5) . . ? O4 Ge1 O8 86.1(5) . . ? O6 Ge1 O8 173.3(5) . . ? O3 Ge1 O8 96.1(5) . . ? C31 O4 Ge1 112.9(8) . . ? C30 O3 Ge1 111.0(9) . . ? O2 C31 O4 124.7(13) . . ? O2 C31 C30 120.7(14) . . ? O4 C31 C30 114.4(13) . . ? O1 C30 O3 120.4(14) . . ? O1 C30 C31 124.6(16) . . ? O3 C30 C31 114.7(14) . . ? C34 O8 Ge1 110.3(11) . . ? C32 O7 Ge1 108.0(11) . . ? C33 O6 Ge1 111.7(10) . . ? C35 O5 Ge1 109.8(10) . . ? O9 C33 O6 116.6(16) . . ? O9 C33 C32 119(2) . . ? O6 C33 C32 111.8(17) . . ? O12 C32 C33 120.0(17) . . ? O12 C32 O7 116(2) . . ? C33 C32 O7 117.9(16) . . ? O11 C34 O8 119.2(18) . . ? O11 C34 C35 122.5(16) . . ? O8 C34 C35 116.5(17) . . ? O10 C35 O5 118.8(19) . . ? O10 C35 C34 125(2) . . ? O5 C35 C34 115.3(16) . . ? _refine_diff_density_max 1.600 _refine_diff_density_min -1.043 _refine_diff_density_rms .187