data_2_838j _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H63 Ge P Si8' _chemical_formula_weight 656.00 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' 'P' 'P' 0.1023 0.0942 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.039(3) _cell_length_b 23.653(5) _cell_length_c 13.088(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.87(3) _cell_angle_gamma 90.00 _cell_volume 3862.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9047 _cell_measurement_theta_min 4.723 _cell_measurement_theta_max 52.315 _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7641 _exptl_absorpt_correction_T_max 0.8444 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30477 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.36 _reflns_number_total 7875 _reflns_number_gt 6300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0567P)^2^+2.0207P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7875 _refine_ls_number_parameters 607 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.009 _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 P1 P 0.2482(3) 0.25408(17) 0.2215(3) 0.0348(7) Uani 0.495(2) 1 d P A 1 Si1 Si 0.1584(7) 0.1167(3) 0.3368(8) 0.027(2) Uani 0.495(2) 1 d P A 1 Si2 Si 0.23659(18) 0.02512(7) 0.32585(15) 0.0317(5) Uani 0.495(2) 1 d P A 1 Si3 Si 0.29058(16) 0.02544(7) 0.1702(2) 0.0356(5) Uani 0.495(2) 1 d P A 1 Si4 Si 0.3379(6) 0.1171(2) 0.1572(6) 0.026(2) Uani 0.495(2) 1 d P A 1 Si5 Si -0.01975(16) 0.11266(11) 0.24719(17) 0.0384(5) Uani 0.495(2) 1 d P A 1 Si6 Si 0.1925(5) 0.1158(3) 0.5242(7) 0.0357(11) Uani 0.495(2) 1 d P A 1 Si7 Si 0.5252(8) 0.1159(3) 0.1932(6) 0.0366(12) Uani 0.495(2) 1 d P A 1 Si8 Si 0.27544(19) 0.14259(13) -0.03238(16) 0.0458(6) Uani 0.495(2) 1 d P A 1 C1 C 0.1461(7) -0.0371(3) 0.3283(8) 0.062(2) Uani 0.495(2) 1 d P A 1 H1A H 0.1847 -0.0724 0.3258 0.093 Uiso 0.495(2) 1 calc PR A 1 H1B H 0.0823 -0.0351 0.2663 0.093 Uiso 0.495(2) 1 calc PR A 1 H1C H 0.1244 -0.0360 0.3939 0.093 Uiso 0.495(2) 1 calc PR A 1 C2 C 0.3620(5) 0.0162(3) 0.4400(6) 0.0519(19) Uani 0.495(2) 1 d P A 1 H2A H 0.3436 0.0156 0.5075 0.078 Uiso 0.495(2) 1 calc PR A 1 H2B H 0.4108 0.0478 0.4406 0.078 Uiso 0.495(2) 1 calc PR A 1 H2C H 0.3971 -0.0194 0.4315 0.078 Uiso 0.495(2) 1 calc PR A 1 C3 C 0.1793(6) -0.0008(3) 0.0532(6) 0.0536(19) Uani 0.495(2) 1 d P A 1 H3A H 0.2046 -0.0025 -0.0103 0.080 Uiso 0.495(2) 1 calc PR A 1 H3B H 0.1182 0.0252 0.0399 0.080 Uiso 0.495(2) 1 calc PR A 1 H3C H 0.1571 -0.0385 0.0690 0.080 Uiso 0.495(2) 1 calc PR A 1 C4 C 0.4006(8) -0.0283(4) 0.1837(9) 0.072(3) Uani 0.495(2) 1 d P A 1 H4A H 0.3708 -0.0665 0.1816 0.108 Uiso 0.495(2) 1 calc PR A 1 H4B H 0.4560 -0.0226 0.2518 0.108 Uiso 0.495(2) 1 calc PR A 1 H4C H 0.4322 -0.0237 0.1248 0.108 Uiso 0.495(2) 1 calc PR A 1 C5 C 0.5786(6) 0.1965(4) 0.2228(8) 0.072(3) Uani 0.495(2) 1 d P A 1 H5A H 0.6572 0.1967 0.2459 0.108 Uiso 0.495(2) 1 calc PR A 1 H5B H 0.5519 0.2127 0.2791 0.108 Uiso 0.495(2) 1 calc PR A 1 H5C H 0.5525 0.2191 0.1576 0.108 Uiso 0.495(2) 1 calc PR A 1 C6 C 0.5889(6) 0.0836(4) 0.3256(6) 0.0511(19) Uani 0.495(2) 1 d P A 1 H6A H 0.5873 0.0423 0.3188 0.077 Uiso 0.495(2) 1 calc PR A 1 H6B H 0.5496 0.0950 0.3757 0.077 Uiso 0.495(2) 1 calc PR A 1 H6C H 0.6634 0.0964 0.3523 0.077 Uiso 0.495(2) 1 calc PR A 1 C7 C 0.5830(8) 0.0937(7) 0.0911(8) 0.098(4) Uani 0.495(2) 1 d P A 1 H7A H 0.6613 0.0949 0.1189 0.146 Uiso 0.495(2) 1 calc PR A 1 H7B H 0.5593 0.1192 0.0296 0.146 Uiso 0.495(2) 1 calc PR A 1 H7C H 0.5599 0.0551 0.0689 0.146 Uiso 0.495(2) 1 calc PR A 1 C8 C 0.312(2) 0.0645(12) -0.0892(16) 0.075(6) Uani 0.495(2) 1 d P A 1 H8A H 0.2656 0.0586 -0.1622 0.113 Uiso 0.495(2) 1 calc PR A 1 H8B H 0.2994 0.0341 -0.0431 0.113 Uiso 0.495(2) 1 calc PR A 1 H8C H 0.3870 0.0642 -0.0888 0.113 Uiso 0.495(2) 1 calc PR A 1 C9 C 0.3290(7) 0.2105(4) -0.0661(7) 0.068(3) Uani 0.495(2) 1 d P A 1 H9A H 0.3052 0.2160 -0.1436 0.102 Uiso 0.495(2) 1 calc PR A 1 H9B H 0.4075 0.2098 -0.0412 0.102 Uiso 0.495(2) 1 calc PR A 1 H9C H 0.3026 0.2417 -0.0312 0.102 Uiso 0.495(2) 1 calc PR A 1 C10 C 0.1245(6) 0.1454(4) -0.0884(6) 0.055(2) Uani 0.495(2) 1 d P A 1 H10A H 0.0962 0.1752 -0.0520 0.083 Uiso 0.495(2) 1 calc PR A 1 H10B H 0.0939 0.1089 -0.0772 0.083 Uiso 0.495(2) 1 calc PR A 1 H10C H 0.1052 0.1537 -0.1650 0.083 Uiso 0.495(2) 1 calc PR A 1 C11 C -0.0464(6) 0.0865(3) 0.1081(6) 0.053(2) Uani 0.495(2) 1 d P A 1 H11A H -0.0186 0.0480 0.1091 0.079 Uiso 0.495(2) 1 calc PR A 1 H11B H -0.0110 0.1113 0.0688 0.079 Uiso 0.495(2) 1 calc PR A 1 H11C H -0.1238 0.0865 0.0731 0.079 Uiso 0.495(2) 1 calc PR A 1 C12 C -0.0887(5) 0.1829(4) 0.2430(6) 0.0524(19) Uani 0.495(2) 1 d P A 1 H12A H -0.1658 0.1783 0.2094 0.079 Uiso 0.495(2) 1 calc PR A 1 H12B H -0.0598 0.2099 0.2016 0.079 Uiso 0.495(2) 1 calc PR A 1 H12C H -0.0763 0.1972 0.3159 0.079 Uiso 0.495(2) 1 calc PR A 1 C13 C -0.1064(10) 0.0870(6) 0.3245(12) 0.071(3) Uani 0.495(2) 1 d P A 1 H13A H -0.0861 0.1051 0.3949 0.106 Uiso 0.495(2) 1 calc PR A 1 H13B H -0.0986 0.0459 0.3333 0.106 Uiso 0.495(2) 1 calc PR A 1 H13C H -0.1812 0.0962 0.2870 0.106 Uiso 0.495(2) 1 calc PR A 1 C14 C 0.2233(8) 0.1974(4) 0.5778(6) 0.072(3) Uani 0.495(2) 1 d P A 1 H14A H 0.1583 0.2202 0.5512 0.107 Uiso 0.495(2) 1 calc PR A 1 H14B H 0.2805 0.2132 0.5517 0.107 Uiso 0.495(2) 1 calc PR A 1 H14C H 0.2458 0.1977 0.6560 0.107 Uiso 0.495(2) 1 calc PR A 1 C15 C 0.0910(8) 0.0929(7) 0.5825(8) 0.093(4) Uani 0.495(2) 1 d P A 1 H15A H 0.0694 0.0541 0.5596 0.140 Uiso 0.495(2) 1 calc PR A 1 H15B H 0.0287 0.1180 0.5594 0.140 Uiso 0.495(2) 1 calc PR A 1 H15C H 0.1193 0.0941 0.6605 0.140 Uiso 0.495(2) 1 calc PR A 1 C16 C 0.3251(6) 0.0836(4) 0.5883(6) 0.055(2) Uani 0.495(2) 1 d P A 1 H16A H 0.3525 0.0975 0.6617 0.082 Uiso 0.495(2) 1 calc PR A 1 H16B H 0.3751 0.0939 0.5481 0.082 Uiso 0.495(2) 1 calc PR A 1 H16C H 0.3178 0.0424 0.5891 0.082 Uiso 0.495(2) 1 calc PR A 1 C17 C 0.2301(15) 0.3070(7) 0.3130(12) 0.134(10) Uani 0.495(2) 1 d PD A 1 H17A H 0.2957 0.3083 0.3745 0.160 Uiso 0.495(2) 1 calc PR A 1 H17B H 0.2231 0.3442 0.2770 0.160 Uiso 0.495(2) 1 calc PR A 1 C18 C 0.1391(17) 0.2994(9) 0.3535(14) 0.150(9) Uani 0.495(2) 1 d PD A 1 H18A H 0.0759 0.3175 0.3050 0.224 Uiso 0.495(2) 1 calc PR A 1 H18B H 0.1544 0.3166 0.4245 0.224 Uiso 0.495(2) 1 calc PR A 1 H18C H 0.1252 0.2589 0.3585 0.224 Uiso 0.495(2) 1 calc PR A 1 C19 C 0.3170(11) 0.3064(6) 0.2278(15) 0.106(6) Uani 0.495(2) 1 d P A 1 H19A H 0.2748 0.3415 0.2248 0.128 Uiso 0.495(2) 1 calc PR A 1 H19B H 0.3787 0.3066 0.2932 0.128 Uiso 0.495(2) 1 calc PR A 1 C20 C 0.3504(12) 0.2993(10) 0.1342(15) 0.161(10) Uani 0.495(2) 1 d P A 1 H20A H 0.3590 0.2590 0.1219 0.241 Uiso 0.495(2) 1 calc PR A 1 H20B H 0.4189 0.3187 0.1435 0.241 Uiso 0.495(2) 1 calc PR A 1 H20C H 0.2963 0.3154 0.0727 0.241 Uiso 0.495(2) 1 calc PR A 1 C21 C 0.126(2) 0.2599(9) 0.1069(18) 0.048(4) Uani 0.495(2) 1 d PD A 1 H21A H 0.1333 0.2333 0.0509 0.058 Uiso 0.495(2) 1 calc PR A 1 H21B H 0.0644 0.2473 0.1305 0.058 Uiso 0.495(2) 1 calc PR A 1 C22 C 0.1008(9) 0.3171(6) 0.0573(12) 0.097(5) Uani 0.495(2) 1 d PD A 1 H22A H 0.0948 0.3444 0.1118 0.145 Uiso 0.495(2) 1 calc PR A 1 H22B H 0.0328 0.3156 0.0003 0.145 Uiso 0.495(2) 1 calc PR A 1 H22C H 0.1582 0.3290 0.0274 0.145 Uiso 0.495(2) 1 calc PR A 1 P2 P 0.2208(3) 0.25448(16) 0.2472(3) 0.0346(7) Uani 0.505(2) 1 d P A 2 Si9 Si 0.1558(7) 0.1175(4) 0.3426(9) 0.037(2) Uani 0.505(2) 1 d P A 2 Si10 Si 0.1707(2) 0.02533(7) 0.29086(16) 0.0369(5) Uani 0.505(2) 1 d P A 2 Si11 Si 0.32547(15) 0.02514(7) 0.23619(19) 0.0336(5) Uani 0.505(2) 1 d P A 2 Si12 Si 0.3412(7) 0.1169(3) 0.1571(6) 0.039(3) Uani 0.505(2) 1 d P A 2 Si13 Si 0.5248(8) 0.1304(3) 0.1821(8) 0.0492(18) Uani 0.505(2) 1 d P A 2 Si14 Si 0.24729(17) 0.11283(11) -0.01988(15) 0.0387(5) Uani 0.505(2) 1 d P A 2 Si15 Si -0.03201(15) 0.14248(13) 0.27512(19) 0.0465(6) Uani 0.505(2) 1 d P A 2 Si16 Si 0.1829(7) 0.1306(3) 0.5259(8) 0.0498(18) Uani 0.505(2) 1 d P A 2 C23 C 0.0531(6) -0.0006(3) 0.1787(6) 0.057(2) Uani 0.505(2) 1 d P A 2 H23A H 0.0707 -0.0372 0.1532 0.085 Uiso 0.505(2) 1 calc PR A 2 H23B H 0.0374 0.0268 0.1199 0.085 Uiso 0.505(2) 1 calc PR A 2 H23C H -0.0098 -0.0047 0.2047 0.085 Uiso 0.505(2) 1 calc PR A 2 C24 C 0.1830(9) -0.0282(4) 0.4002(8) 0.072(3) Uani 0.505(2) 1 d P A 2 H24A H 0.1215 -0.0247 0.4287 0.108 Uiso 0.505(2) 1 calc PR A 2 H24B H 0.2494 -0.0215 0.4575 0.108 Uiso 0.505(2) 1 calc PR A 2 H24C H 0.1844 -0.0663 0.3714 0.108 Uiso 0.505(2) 1 calc PR A 2 C25 C 0.4399(6) 0.0161(3) 0.3624(6) 0.056(2) Uani 0.505(2) 1 d P A 2 H25A H 0.4298 -0.0188 0.3984 0.083 Uiso 0.505(2) 1 calc PR A 2 H25B H 0.4416 0.0484 0.4099 0.083 Uiso 0.505(2) 1 calc PR A 2 H25C H 0.5077 0.0142 0.3444 0.083 Uiso 0.505(2) 1 calc PR A 2 C26 C 0.3289(8) -0.0370(3) 0.1464(7) 0.062(2) Uani 0.505(2) 1 d P A 2 H26A H 0.3942 -0.0352 0.1238 0.093 Uiso 0.505(2) 1 calc PR A 2 H26B H 0.2660 -0.0357 0.0835 0.093 Uiso 0.505(2) 1 calc PR A 2 H26C H 0.3283 -0.0723 0.1855 0.093 Uiso 0.505(2) 1 calc PR A 2 C27 C 0.6033(6) 0.1440(6) 0.3184(8) 0.090(4) Uani 0.505(2) 1 d P A 2 H27A H 0.6775 0.1523 0.3204 0.135 Uiso 0.505(2) 1 calc PR A 2 H27B H 0.6019 0.1106 0.3624 0.135 Uiso 0.505(2) 1 calc PR A 2 H27C H 0.5731 0.1764 0.3463 0.135 Uiso 0.505(2) 1 calc PR A 2 C28 C 0.5801(6) 0.0563(5) 0.1451(7) 0.075(3) Uani 0.505(2) 1 d P A 2 H28A H 0.6530 0.0613 0.1399 0.113 Uiso 0.505(2) 1 calc PR A 2 H28B H 0.5334 0.0428 0.0765 0.113 Uiso 0.505(2) 1 calc PR A 2 H28C H 0.5808 0.0284 0.2008 0.113 Uiso 0.505(2) 1 calc PR A 2 C29 C 0.5465(8) 0.1752(5) 0.0770(10) 0.098(4) Uani 0.505(2) 1 d P A 2 H29A H 0.5203 0.2134 0.0838 0.147 Uiso 0.505(2) 1 calc PR A 2 H29B H 0.5076 0.1596 0.0071 0.147 Uiso 0.505(2) 1 calc PR A 2 H29C H 0.6232 0.1767 0.0834 0.147 Uiso 0.505(2) 1 calc PR A 2 C30 C 0.328(2) 0.0844(12) -0.1093(17) 0.082(6) Uani 0.505(2) 1 d P A 2 H30A H 0.2915 0.0945 -0.1837 0.123 Uiso 0.505(2) 1 calc PR A 2 H30B H 0.3330 0.0432 -0.1025 0.123 Uiso 0.505(2) 1 calc PR A 2 H30C H 0.3996 0.1010 -0.0877 0.123 Uiso 0.505(2) 1 calc PR A 2 C31 C 0.1075(6) 0.0865(3) -0.0462(6) 0.055(2) Uani 0.505(2) 1 d P A 2 H31A H 0.0679 0.1114 -0.0112 0.083 Uiso 0.505(2) 1 calc PR A 2 H31B H 0.1087 0.0481 -0.0180 0.083 Uiso 0.505(2) 1 calc PR A 2 H31C H 0.0724 0.0862 -0.1234 0.083 Uiso 0.505(2) 1 calc PR A 2 C32 C 0.2427(6) 0.1826(3) -0.0881(6) 0.0529(19) Uani 0.505(2) 1 d P A 2 H32A H 0.2125 0.1776 -0.1654 0.079 Uiso 0.505(2) 1 calc PR A 2 H32B H 0.3154 0.1979 -0.0727 0.079 Uiso 0.505(2) 1 calc PR A 2 H32C H 0.1978 0.2089 -0.0621 0.079 Uiso 0.505(2) 1 calc PR A 2 C33 C -0.0888(5) 0.1457(4) 0.1242(6) 0.057(2) Uani 0.505(2) 1 d P A 2 H33A H -0.1655 0.1545 0.1052 0.086 Uiso 0.505(2) 1 calc PR A 2 H33B H -0.0787 0.1091 0.0935 0.086 Uiso 0.505(2) 1 calc PR A 2 H33C H -0.0516 0.1751 0.0960 0.086 Uiso 0.505(2) 1 calc PR A 2 C34 C -0.0642(6) 0.2111(4) 0.3294(7) 0.069(3) Uani 0.505(2) 1 d P A 2 H34A H -0.0299 0.2421 0.3018 0.103 Uiso 0.505(2) 1 calc PR A 2 H34B H -0.0375 0.2105 0.4075 0.103 Uiso 0.505(2) 1 calc PR A 2 H34C H -0.1420 0.2167 0.3073 0.103 Uiso 0.505(2) 1 calc PR A 2 C35 C -0.0923(12) 0.0623(5) 0.3146(13) 0.066(4) Uani 0.505(2) 1 d PU A 2 H35A H -0.0892 0.0621 0.3903 0.100 Uiso 0.505(2) 1 calc PR A 2 H35B H -0.0482 0.0314 0.3004 0.100 Uiso 0.505(2) 1 calc PR A 2 H35C H -0.1667 0.0572 0.2708 0.100 Uiso 0.505(2) 1 calc PR A 2 C36 C 0.3183(8) 0.1437(6) 0.6018(6) 0.088(4) Uani 0.505(2) 1 d P A 2 H36A H 0.3451 0.1772 0.5737 0.132 Uiso 0.505(2) 1 calc PR A 2 H36B H 0.3626 0.1109 0.5968 0.132 Uiso 0.505(2) 1 calc PR A 2 H36C H 0.3216 0.1501 0.6767 0.132 Uiso 0.505(2) 1 calc PR A 2 C37 C 0.1457(8) 0.0562(5) 0.5808(6) 0.080(3) Uani 0.505(2) 1 d P A 2 H37A H 0.2016 0.0284 0.5814 0.120 Uiso 0.505(2) 1 calc PR A 2 H37B H 0.0768 0.0428 0.5342 0.120 Uiso 0.505(2) 1 calc PR A 2 H37C H 0.1405 0.0612 0.6534 0.120 Uiso 0.505(2) 1 calc PR A 2 C38 C 0.0770(10) 0.1749(5) 0.5464(8) 0.098(4) Uani 0.505(2) 1 d P A 2 H38A H 0.0815 0.1754 0.6224 0.148 Uiso 0.505(2) 1 calc PR A 2 H38B H 0.0072 0.1597 0.5054 0.148 Uiso 0.505(2) 1 calc PR A 2 H38C H 0.0850 0.2134 0.5223 0.148 Uiso 0.505(2) 1 calc PR A 2 C39 C 0.1852(15) 0.2862(7) 0.3508(11) 0.100(7) Uani 0.505(2) 1 d PD A 2 H39A H 0.1458 0.3213 0.3225 0.120 Uiso 0.505(2) 1 calc PR A 2 H39B H 0.1338 0.2607 0.3706 0.120 Uiso 0.505(2) 1 calc PR A 2 C40 C 0.2674(14) 0.3009(7) 0.4486(9) 0.196(11) Uani 0.505(2) 1 d PD A 2 H40A H 0.2670 0.2734 0.5043 0.294 Uiso 0.505(2) 1 calc PR A 2 H40B H 0.2531 0.3388 0.4718 0.294 Uiso 0.505(2) 1 calc PR A 2 H40C H 0.3377 0.3006 0.4355 0.294 Uiso 0.505(2) 1 calc PR A 2 C41 C 0.110(2) 0.2610(8) 0.1299(19) 0.051(4) Uani 0.505(2) 1 d PD A 2 H41A H 0.1351 0.2484 0.0689 0.061 Uiso 0.505(2) 1 calc PR A 2 H41B H 0.0549 0.2339 0.1364 0.061 Uiso 0.505(2) 1 calc PR A 2 C42 C 0.0570(11) 0.3168(6) 0.1008(9) 0.096(5) Uani 0.505(2) 1 d PD A 2 H42A H 0.0407 0.3330 0.1632 0.144 Uiso 0.505(2) 1 calc PR A 2 H42B H -0.0096 0.3117 0.0429 0.144 Uiso 0.505(2) 1 calc PR A 2 H42C H 0.1048 0.3423 0.0772 0.144 Uiso 0.505(2) 1 calc PR A 2 C43 C 0.3523(13) 0.2857(6) 0.1833(14) 0.083(4) Uani 0.505(2) 1 d PU A 2 H43A H 0.3690 0.2562 0.1370 0.099 Uiso 0.505(2) 1 calc PR A 2 H43B H 0.3268 0.3196 0.1387 0.099 Uiso 0.505(2) 1 calc PR A 2 C44 C 0.4488(9) 0.3000(7) 0.2657(15) 0.197(11) Uani 0.505(2) 1 d P A 2 H44A H 0.4343 0.3312 0.3088 0.295 Uiso 0.505(2) 1 calc PR A 2 H44B H 0.5043 0.3115 0.2330 0.295 Uiso 0.505(2) 1 calc PR A 2 H44C H 0.4737 0.2670 0.3114 0.295 Uiso 0.505(2) 1 calc PR A 2 Ge1 Ge 0.30890(2) 0.168269(12) 0.30888(2) 0.02562(10) 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 P1 0.0318(17) 0.0308(11) 0.0379(17) -0.0004(11) 0.0040(10) 0.0024(11) Si1 0.033(4) 0.034(3) 0.014(2) -0.0072(19) 0.006(2) -0.017(2) Si2 0.0268(11) 0.0269(9) 0.0337(10) 0.0088(7) -0.0034(8) -0.0045(7) Si3 0.0329(10) 0.0318(10) 0.0372(13) -0.0109(8) 0.0022(9) 0.0042(7) Si4 0.019(3) 0.022(2) 0.034(4) -0.011(2) 0.003(3) -0.0040(19) Si5 0.0215(9) 0.0560(15) 0.0358(11) -0.0063(10) 0.0055(8) -0.0032(9) Si6 0.0361(15) 0.048(3) 0.0255(14) -0.0056(19) 0.0121(11) 0.0046(18) Si7 0.0248(14) 0.050(4) 0.0377(16) 0.007(2) 0.0124(11) -0.002(2) Si8 0.0435(13) 0.0709(18) 0.0222(10) 0.0031(11) 0.0081(8) -0.0099(12) C1 0.064(6) 0.043(5) 0.069(6) 0.014(4) 0.003(5) -0.017(4) C2 0.036(4) 0.062(5) 0.048(4) 0.020(4) -0.004(3) 0.012(3) C3 0.054(4) 0.053(4) 0.049(4) -0.029(4) 0.008(4) -0.011(4) C4 0.062(6) 0.053(5) 0.096(8) -0.020(5) 0.014(5) 0.031(5) C5 0.040(4) 0.089(7) 0.083(6) 0.021(5) 0.012(4) -0.023(4) C6 0.033(4) 0.065(5) 0.048(4) 0.010(4) 0.000(3) 0.004(3) C7 0.044(5) 0.207(15) 0.051(6) -0.009(7) 0.029(5) 0.015(7) C8 0.067(8) 0.138(19) 0.030(8) -0.028(8) 0.027(6) -0.004(9) C9 0.070(6) 0.095(7) 0.038(4) 0.024(4) 0.014(4) -0.017(5) C10 0.051(4) 0.076(5) 0.031(4) -0.001(3) 0.000(3) -0.013(4) C11 0.037(4) 0.057(5) 0.050(4) -0.017(4) -0.009(3) -0.002(3) C12 0.027(3) 0.076(5) 0.053(4) -0.018(4) 0.010(3) 0.009(4) C13 0.037(5) 0.087(10) 0.089(8) 0.001(8) 0.020(5) -0.022(6) C14 0.088(7) 0.085(6) 0.039(4) -0.026(4) 0.014(4) 0.022(5) C15 0.043(6) 0.196(14) 0.045(5) 0.017(7) 0.020(5) -0.013(7) C16 0.046(4) 0.073(6) 0.035(4) 0.007(4) -0.004(3) 0.001(4) C17 0.25(3) 0.067(9) 0.062(9) 0.001(7) 0.002(11) 0.068(12) C18 0.23(2) 0.17(2) 0.067(9) -0.019(10) 0.078(13) 0.079(16) C19 0.072(9) 0.061(8) 0.162(16) 0.043(9) -0.003(9) -0.019(6) C20 0.059(8) 0.24(2) 0.188(19) 0.115(17) 0.048(10) -0.014(10) C21 0.039(8) 0.064(7) 0.035(9) 0.008(5) -0.001(6) 0.008(5) C22 0.055(7) 0.117(10) 0.101(11) 0.072(10) -0.003(6) 0.020(6) P2 0.0332(16) 0.0286(10) 0.0379(17) 0.0005(10) 0.0036(10) 0.0022(11) Si9 0.023(3) 0.054(4) 0.032(4) 0.005(3) 0.005(3) 0.002(2) Si10 0.0375(13) 0.0322(10) 0.0358(10) 0.0043(7) 0.0026(9) -0.0099(8) Si11 0.0332(10) 0.0284(9) 0.0315(11) -0.0048(8) -0.0026(9) 0.0086(7) Si12 0.024(4) 0.072(5) 0.022(4) -0.004(3) 0.008(3) 0.002(3) Si13 0.0256(15) 0.053(4) 0.075(3) 0.008(2) 0.0246(19) -0.004(2) Si14 0.0338(11) 0.0576(15) 0.0229(9) -0.0045(9) 0.0051(8) -0.0041(9) Si15 0.0204(10) 0.0731(17) 0.0449(12) -0.0080(12) 0.0079(8) 0.0021(11) Si16 0.076(3) 0.052(4) 0.0294(15) -0.005(2) 0.0277(17) 0.008(2) C23 0.044(4) 0.060(5) 0.056(4) -0.009(4) 0.000(3) -0.025(4) C24 0.095(8) 0.047(5) 0.067(6) 0.027(5) 0.013(5) -0.020(5) C25 0.043(4) 0.065(5) 0.045(4) 0.005(4) -0.008(3) 0.020(3) C26 0.080(6) 0.043(5) 0.054(5) -0.014(4) 0.006(5) 0.019(4) C27 0.032(4) 0.161(11) 0.071(6) -0.048(7) 0.006(4) -0.017(5) C28 0.032(4) 0.146(10) 0.046(5) -0.030(5) 0.010(4) 0.024(5) C29 0.056(6) 0.124(9) 0.131(10) 0.014(7) 0.054(6) -0.025(6) C30 0.084(11) 0.14(2) 0.033(7) -0.017(8) 0.032(6) 0.004(10) C31 0.043(4) 0.060(5) 0.048(4) 0.002(4) -0.009(3) -0.021(3) C32 0.058(5) 0.063(5) 0.035(4) 0.009(4) 0.010(3) -0.022(4) C33 0.030(4) 0.076(5) 0.056(5) -0.013(4) -0.003(3) -0.001(3) C34 0.033(4) 0.102(7) 0.067(5) -0.017(5) 0.010(4) 0.022(4) C35 0.052(5) 0.074(6) 0.077(5) 0.005(4) 0.026(4) -0.017(4) C36 0.079(6) 0.154(10) 0.027(4) -0.018(5) 0.008(4) -0.054(7) C37 0.043(5) 0.163(11) 0.032(4) 0.029(5) 0.008(4) -0.025(6) C38 0.130(10) 0.127(9) 0.058(6) -0.020(6) 0.058(7) 0.015(7) C39 0.158(15) 0.085(10) 0.049(9) -0.020(6) 0.016(9) 0.078(11) C40 0.27(2) 0.192(15) 0.062(7) -0.067(8) -0.060(10) 0.168(15) C41 0.052(9) 0.058(7) 0.039(9) 0.003(5) 0.010(6) 0.013(5) C42 0.095(10) 0.121(10) 0.052(7) 0.019(6) -0.010(6) 0.060(9) C43 0.069(7) 0.072(7) 0.106(8) 0.046(6) 0.022(6) -0.009(5) C44 0.064(7) 0.183(14) 0.27(2) 0.162(15) -0.061(10) -0.068(8) Ge1 0.02381(16) 0.02574(16) 0.02523(16) -0.00179(12) 0.00382(11) -0.00185(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C19 1.516(12) . ? P1 C17 1.795(15) . ? P1 C21 1.85(3) . ? P1 Ge1 2.351(4) . ? Si1 Si5 2.280(9) . ? Si1 Si6 2.361(14) . ? Si1 Si2 2.416(10) . ? Si1 Ge1 2.427(9) . ? Si2 C2 1.880(7) . ? Si2 C1 1.892(8) . ? Si2 Si3 2.341(3) . ? Si3 C3 1.882(7) . ? Si3 C4 1.886(8) . ? Si3 Si4 2.275(6) . ? Si4 Si7 2.349(13) . ? Si4 Ge1 2.446(7) . ? Si4 Si8 2.451(8) . ? Si5 C13 1.826(14) . ? Si5 C11 1.857(7) . ? Si5 C12 1.882(8) . ? Si6 C15 1.793(12) . ? Si6 C16 1.852(10) . ? Si6 C14 2.054(11) . ? Si7 C7 1.792(13) . ? Si7 C6 1.855(10) . ? Si7 C5 2.030(12) . ? Si8 C9 1.855(9) . ? Si8 C10 1.892(8) . ? Si8 C8 2.10(3) . ? C17 C18 1.444(18) . ? C19 C20 1.42(3) . ? C21 C22 1.495(15) . ? P2 C39 1.728(14) . ? P2 C41 1.78(3) . ? P2 C43 2.240(16) . ? P2 Ge1 2.364(4) . ? Si9 Si10 2.307(10) . ? Si9 Si16 2.341(15) . ? Si9 Si15 2.423(9) . ? Si9 Ge1 2.477(10) . ? Si10 C24 1.882(8) . ? Si10 C23 1.891(7) . ? Si10 Si11 2.329(3) . ? Si11 C25 1.889(7) . ? Si11 C26 1.890(8) . ? Si11 Si12 2.440(8) . ? Si12 Si14 2.286(8) . ? Si12 Si13 2.342(13) . ? Si12 Ge1 2.467(7) . ? Si13 C27 1.810(13) . ? Si13 C29 1.823(13) . ? Si13 C28 2.007(13) . ? Si14 C31 1.861(7) . ? Si14 C32 1.869(8) . ? Si14 C30 1.90(2) . ? Si15 C34 1.867(9) . ? Si15 C33 1.899(8) . ? Si15 C35 2.172(13) . ? Si16 C36 1.784(12) . ? Si16 C38 1.814(12) . ? Si16 C37 2.012(14) . ? C39 C40 1.453(15) . ? C41 C42 1.488(15) . ? C43 C44 1.439(19) . ? 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 C19 P1 C17 65.5(9) . . ? C19 P1 C21 109.8(9) . . ? C17 P1 C21 103.9(8) . . ? C19 P1 Ge1 124.6(5) . . ? C17 P1 Ge1 111.6(5) . . ? C21 P1 Ge1 123.3(7) . . ? Si5 Si1 Si6 113.0(5) . . ? Si5 Si1 Si2 108.4(3) . . ? Si6 Si1 Si2 95.6(4) . . ? Si5 Si1 Ge1 133.7(5) . . ? Si6 Si1 Ge1 104.1(3) . . ? Si2 Si1 Ge1 93.9(4) . . ? C2 Si2 C1 107.6(4) . . ? C2 Si2 Si3 106.3(3) . . ? C1 Si2 Si3 111.3(3) . . ? C2 Si2 Si1 109.8(3) . . ? C1 Si2 Si1 114.9(4) . . ? Si3 Si2 Si1 106.7(3) . . ? C3 Si3 C4 103.9(4) . . ? C3 Si3 Si4 114.5(3) . . ? C4 Si3 Si4 115.7(4) . . ? C3 Si3 Si2 110.6(3) . . ? C4 Si3 Si2 109.2(4) . . ? Si4 Si3 Si2 103.0(2) . . ? Si3 Si4 Si7 105.2(3) . . ? Si3 Si4 Ge1 107.6(3) . . ? Si7 Si4 Ge1 103.9(3) . . ? Si3 Si4 Si8 107.0(3) . . ? Si7 Si4 Si8 103.1(4) . . ? Ge1 Si4 Si8 128.0(3) . . ? C13 Si5 C11 117.6(5) . . ? C13 Si5 C12 86.7(5) . . ? C11 Si5 C12 108.3(3) . . ? C13 Si5 Si1 115.5(5) . . ? C11 Si5 Si1 113.0(4) . . ? C12 Si5 Si1 112.6(3) . . ? C15 Si6 C16 113.0(7) . . ? C15 Si6 C14 103.5(7) . . ? C16 Si6 C14 99.6(5) . . ? C15 Si6 Si1 120.3(5) . . ? C16 Si6 Si1 110.1(5) . . ? C14 Si6 Si1 107.8(5) . . ? C7 Si7 C6 113.9(7) . . ? C7 Si7 C5 102.8(7) . . ? C6 Si7 C5 100.0(5) . . ? C7 Si7 Si4 119.5(6) . . ? C6 Si7 Si4 110.5(5) . . ? C5 Si7 Si4 107.8(5) . . ? C9 Si8 C10 107.3(4) . . ? C9 Si8 C8 122.7(5) . . ? C10 Si8 C8 102.1(7) . . ? C9 Si8 Si4 114.6(3) . . ? C10 Si8 Si4 113.8(3) . . ? C8 Si8 Si4 95.7(6) . . ? C18 C17 P1 116.1(14) . . ? C20 C19 P1 100.4(15) . . ? C22 C21 P1 116.8(18) . . ? C39 P2 C41 107.7(8) . . ? C39 P2 C43 124.0(9) . . ? C41 P2 C43 99.5(8) . . ? C39 P2 Ge1 108.7(5) . . ? C41 P2 Ge1 124.1(7) . . ? C43 P2 Ge1 93.6(4) . . ? Si10 Si9 Si16 115.2(5) . . ? Si10 Si9 Si15 106.6(3) . . ? Si16 Si9 Si15 100.2(5) . . ? Si10 Si9 Ge1 105.4(4) . . ? Si16 Si9 Ge1 103.2(4) . . ? Si15 Si9 Ge1 126.7(4) . . ? C24 Si10 C23 104.1(4) . . ? C24 Si10 Si9 114.1(4) . . ? C23 Si10 Si9 114.6(4) . . ? C24 Si10 Si11 110.0(4) . . ? C23 Si10 Si11 109.9(3) . . ? Si9 Si10 Si11 104.3(3) . . ? C25 Si11 C26 107.5(4) . . ? C25 Si11 Si10 105.5(3) . . ? C26 Si11 Si10 111.8(4) . . ? C25 Si11 Si12 109.2(3) . . ? C26 Si11 Si12 114.1(4) . . ? Si10 Si11 Si12 108.4(2) . . ? Si14 Si12 Si13 111.9(4) . . ? Si14 Si12 Si11 107.8(3) . . ? Si13 Si12 Si11 105.7(4) . . ? Si14 Si12 Ge1 132.1(4) . . ? Si13 Si12 Ge1 103.1(4) . . ? Si11 Si12 Ge1 92.4(3) . . ? C27 Si13 C29 118.3(7) . . ? C27 Si13 C28 104.7(6) . . ? C29 Si13 C28 100.4(7) . . ? C27 Si13 Si12 115.1(6) . . ? C29 Si13 Si12 110.4(6) . . ? C28 Si13 Si12 105.8(5) . . ? C31 Si14 C32 108.2(4) . . ? C31 Si14 C30 116.8(8) . . ? C32 Si14 C30 88.0(8) . . ? C31 Si14 Si12 114.2(3) . . ? C32 Si14 Si12 112.3(3) . . ? C30 Si14 Si12 114.1(8) . . ? C34 Si15 C33 107.3(4) . . ? C34 Si15 C35 122.1(5) . . ? C33 Si15 C35 102.9(5) . . ? C34 Si15 Si9 112.8(3) . . ? C33 Si15 Si9 115.9(4) . . ? C35 Si15 Si9 95.6(5) . . ? C36 Si16 C38 119.4(7) . . ? C36 Si16 C37 104.8(6) . . ? C38 Si16 C37 100.3(7) . . ? C36 Si16 Si9 115.1(6) . . ? C38 Si16 Si9 109.4(6) . . ? C37 Si16 Si9 105.7(5) . . ? C40 C39 P2 119.8(12) . . ? C42 C41 P2 119.9(17) . . ? C44 C43 P2 113.3(12) . . ? P1 Ge1 P2 13.57(7) . . ? P1 Ge1 Si1 109.5(2) . . ? P2 Ge1 Si1 98.7(2) . . ? P1 Ge1 Si4 98.13(18) . . ? P2 Ge1 Si4 108.88(19) . . ? Si1 Ge1 Si4 101.3(3) . . ? P1 Ge1 Si12 98.3(2) . . ? P2 Ge1 Si12 109.2(2) . . ? Si1 Ge1 Si12 102.0(3) . . ? Si4 Ge1 Si12 0.9(4) . . ? P1 Ge1 Si9 109.3(2) . . ? P2 Ge1 Si9 98.2(2) . . ? Si1 Ge1 Si9 1.8(5) . . ? Si4 Ge1 Si9 103.1(3) . . ? Si12 Ge1 Si9 103.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si5 Si1 Si2 C2 -156.5(4) . . . . ? Si6 Si1 Si2 C2 -40.0(4) . . . . ? Ge1 Si1 Si2 C2 64.7(4) . . . . ? Si5 Si1 Si2 C1 -35.1(6) . . . . ? Si6 Si1 Si2 C1 81.4(5) . . . . ? Ge1 Si1 Si2 C1 -174.0(4) . . . . ? Si5 Si1 Si2 Si3 88.7(4) . . . . ? Si6 Si1 Si2 Si3 -154.7(3) . . . . ? Ge1 Si1 Si2 Si3 -50.1(3) . . . . ? C2 Si2 Si3 C3 152.7(4) . . . . ? C1 Si2 Si3 C3 35.8(4) . . . . ? Si1 Si2 Si3 C3 -90.2(4) . . . . ? C2 Si2 Si3 C4 39.0(5) . . . . ? C1 Si2 Si3 C4 -77.9(5) . . . . ? Si1 Si2 Si3 C4 156.1(4) . . . . ? C2 Si2 Si3 Si4 -84.5(3) . . . . ? C1 Si2 Si3 Si4 158.6(4) . . . . ? Si1 Si2 Si3 Si4 32.6(3) . . . . ? C3 Si3 Si4 Si7 -129.7(4) . . . . ? C4 Si3 Si4 Si7 -8.8(6) . . . . ? Si2 Si3 Si4 Si7 110.2(3) . . . . ? C3 Si3 Si4 Ge1 120.0(3) . . . . ? C4 Si3 Si4 Ge1 -119.2(5) . . . . ? Si2 Si3 Si4 Ge1 -0.1(3) . . . . ? C3 Si3 Si4 Si8 -20.6(4) . . . . ? C4 Si3 Si4 Si8 100.3(5) . . . . ? Si2 Si3 Si4 Si8 -140.7(2) . . . . ? Si6 Si1 Si5 C13 -18.8(7) . . . . ? Si2 Si1 Si5 C13 85.9(7) . . . . ? Ge1 Si1 Si5 C13 -159.4(7) . . . . ? Si6 Si1 Si5 C11 -158.3(4) . . . . ? Si2 Si1 Si5 C11 -53.6(5) . . . . ? Ge1 Si1 Si5 C11 61.1(7) . . . . ? Si6 Si1 Si5 C12 78.6(5) . . . . ? Si2 Si1 Si5 C12 -176.7(4) . . . . ? Ge1 Si1 Si5 C12 -62.0(7) . . . . ? Si5 Si1 Si6 C15 17.3(9) . . . . ? Si2 Si1 Si6 C15 -95.5(7) . . . . ? Ge1 Si1 Si6 C15 169.1(7) . . . . ? Si5 Si1 Si6 C16 151.4(5) . . . . ? Si2 Si1 Si6 C16 38.7(5) . . . . ? Ge1 Si1 Si6 C16 -56.8(6) . . . . ? Si5 Si1 Si6 C14 -100.8(5) . . . . ? Si2 Si1 Si6 C14 146.4(4) . . . . ? Ge1 Si1 Si6 C14 50.9(5) . . . . ? Si3 Si4 Si7 C7 78.3(8) . . . . ? Ge1 Si4 Si7 C7 -168.7(7) . . . . ? Si8 Si4 Si7 C7 -33.6(8) . . . . ? Si3 Si4 Si7 C6 -56.8(6) . . . . ? Ge1 Si4 Si7 C6 56.2(5) . . . . ? Si8 Si4 Si7 C6 -168.7(4) . . . . ? Si3 Si4 Si7 C5 -165.0(4) . . . . ? Ge1 Si4 Si7 C5 -52.1(5) . . . . ? Si8 Si4 Si7 C5 83.1(5) . . . . ? Si3 Si4 Si8 C9 -168.1(4) . . . . ? Si7 Si4 Si8 C9 -57.5(5) . . . . ? Ge1 Si4 Si8 C9 62.2(6) . . . . ? Si3 Si4 Si8 C10 67.9(4) . . . . ? Si7 Si4 Si8 C10 178.5(4) . . . . ? Ge1 Si4 Si8 C10 -61.8(5) . . . . ? Si3 Si4 Si8 C8 -38.1(7) . . . . ? Si7 Si4 Si8 C8 72.5(7) . . . . ? Ge1 Si4 Si8 C8 -167.8(7) . . . . ? C19 P1 C17 C18 168.1(16) . . . . ? C21 P1 C17 C18 62.4(16) . . . . ? Ge1 P1 C17 C18 -72.5(14) . . . . ? C17 P1 C19 C20 -164.8(13) . . . . ? C21 P1 C19 C20 -68.1(14) . . . . ? Ge1 P1 C19 C20 95.0(10) . . . . ? C19 P1 C21 C22 -14.2(17) . . . . ? C17 P1 C21 C22 54.3(16) . . . . ? Ge1 P1 C21 C22 -177.6(10) . . . . ? Si16 Si9 Si10 C24 8.3(7) . . . . ? Si15 Si9 Si10 C24 -101.8(5) . . . . ? Ge1 Si9 Si10 C24 121.4(5) . . . . ? Si16 Si9 Si10 C23 128.2(5) . . . . ? Si15 Si9 Si10 C23 18.0(6) . . . . ? Ge1 Si9 Si10 C23 -118.8(4) . . . . ? Si16 Si9 Si10 Si11 -111.7(5) . . . . ? Si15 Si9 Si10 Si11 138.2(3) . . . . ? Ge1 Si9 Si10 Si11 1.4(4) . . . . ? C24 Si10 Si11 C25 -39.1(4) . . . . ? C23 Si10 Si11 C25 -153.1(4) . . . . ? Si9 Si10 Si11 C25 83.6(4) . . . . ? C24 Si10 Si11 C26 77.4(5) . . . . ? C23 Si10 Si11 C26 -36.6(4) . . . . ? Si9 Si10 Si11 C26 -159.9(4) . . . . ? C24 Si10 Si11 Si12 -155.9(4) . . . . ? C23 Si10 Si11 Si12 90.0(4) . . . . ? Si9 Si10 Si11 Si12 -33.2(3) . . . . ? C25 Si11 Si12 Si14 158.3(4) . . . . ? C26 Si11 Si12 Si14 38.0(5) . . . . ? Si10 Si11 Si12 Si14 -87.3(3) . . . . ? C25 Si11 Si12 Si13 38.5(5) . . . . ? C26 Si11 Si12 Si13 -81.8(5) . . . . ? Si10 Si11 Si12 Si13 152.9(3) . . . . ? C25 Si11 Si12 Ge1 -65.9(4) . . . . ? C26 Si11 Si12 Ge1 173.9(4) . . . . ? Si10 Si11 Si12 Ge1 48.6(3) . . . . ? Si14 Si12 Si13 C27 171.8(6) . . . . ? Si11 Si12 Si13 C27 -71.2(7) . . . . ? Ge1 Si12 Si13 C27 25.1(7) . . . . ? Si14 Si12 Si13 C29 34.6(7) . . . . ? Si11 Si12 Si13 C29 151.7(6) . . . . ? Ge1 Si12 Si13 C29 -112.0(6) . . . . ? Si14 Si12 Si13 C28 -73.2(5) . . . . ? Si11 Si12 Si13 C28 43.9(6) . . . . ? Ge1 Si12 Si13 C28 140.2(5) . . . . ? Si13 Si12 Si14 C31 167.1(4) . . . . ? Si11 Si12 Si14 C31 51.3(5) . . . . ? Ge1 Si12 Si14 C31 -59.1(6) . . . . ? Si13 Si12 Si14 C32 -69.2(5) . . . . ? Si11 Si12 Si14 C32 175.0(4) . . . . ? Ge1 Si12 Si14 C32 64.7(6) . . . . ? Si13 Si12 Si14 C30 29.0(9) . . . . ? Si11 Si12 Si14 C30 -86.8(9) . . . . ? Ge1 Si12 Si14 C30 162.9(9) . . . . ? Si10 Si9 Si15 C34 169.8(4) . . . . ? Si16 Si9 Si15 C34 49.5(6) . . . . ? Ge1 Si9 Si15 C34 -65.7(7) . . . . ? Si10 Si9 Si15 C33 -65.9(6) . . . . ? Si16 Si9 Si15 C33 173.8(4) . . . . ? Ge1 Si9 Si15 C33 58.7(6) . . . . ? Si10 Si9 Si15 C35 41.4(6) . . . . ? Si16 Si9 Si15 C35 -78.9(5) . . . . ? Ge1 Si9 Si15 C35 165.9(6) . . . . ? Si10 Si9 Si16 C36 89.5(7) . . . . ? Si15 Si9 Si16 C36 -156.6(6) . . . . ? Ge1 Si9 Si16 C36 -24.8(7) . . . . ? Si10 Si9 Si16 C38 -132.8(6) . . . . ? Si15 Si9 Si16 C38 -18.9(7) . . . . ? Ge1 Si9 Si16 C38 112.9(6) . . . . ? Si10 Si9 Si16 C37 -25.6(7) . . . . ? Si15 Si9 Si16 C37 88.4(5) . . . . ? Ge1 Si9 Si16 C37 -139.8(5) . . . . ? C41 P2 C39 C40 -163.4(16) . . . . ? C43 P2 C39 C40 -48.3(17) . . . . ? Ge1 P2 C39 C40 59.7(16) . . . . ? C39 P2 C41 C42 48.4(18) . . . . ? C43 P2 C41 C42 -82.0(16) . . . . ? Ge1 P2 C41 C42 177.0(11) . . . . ? C39 P2 C43 C44 45.4(14) . . . . ? C41 P2 C43 C44 164.4(13) . . . . ? Ge1 P2 C43 C44 -70.1(12) . . . . ? C19 P1 Ge1 P2 116.9(13) . . . . ? C17 P1 Ge1 P2 42.6(10) . . . . ? C21 P1 Ge1 P2 -82.1(10) . . . . ? C19 P1 Ge1 Si1 155.0(10) . . . . ? C17 P1 Ge1 Si1 80.7(8) . . . . ? C21 P1 Ge1 Si1 -44.0(8) . . . . ? C19 P1 Ge1 Si4 -99.8(10) . . . . ? C17 P1 Ge1 Si4 -174.2(7) . . . . ? C21 P1 Ge1 Si4 61.1(8) . . . . ? C19 P1 Ge1 Si12 -99.0(10) . . . . ? C17 P1 Ge1 Si12 -173.3(7) . . . . ? C21 P1 Ge1 Si12 62.0(8) . . . . ? C19 P1 Ge1 Si9 153.1(10) . . . . ? C17 P1 Ge1 Si9 78.7(8) . . . . ? C21 P1 Ge1 Si9 -46.0(8) . . . . ? C39 P2 Ge1 P1 -148.8(12) . . . . ? C41 P2 Ge1 P1 83.1(11) . . . . ? C43 P2 Ge1 P1 -21.0(8) . . . . ? C39 P2 Ge1 Si1 67.2(8) . . . . ? C41 P2 Ge1 Si1 -60.9(9) . . . . ? C43 P2 Ge1 Si1 -164.9(5) . . . . ? C39 P2 Ge1 Si4 172.4(8) . . . . ? C41 P2 Ge1 Si4 44.3(9) . . . . ? C43 P2 Ge1 Si4 -59.7(5) . . . . ? C39 P2 Ge1 Si12 173.3(8) . . . . ? C41 P2 Ge1 Si12 45.2(9) . . . . ? C43 P2 Ge1 Si12 -58.9(5) . . . . ? C39 P2 Ge1 Si9 65.4(8) . . . . ? C41 P2 Ge1 Si9 -62.7(9) . . . . ? C43 P2 Ge1 Si9 -166.7(5) . . . . ? Si5 Si1 Ge1 P1 29.3(6) . . . . ? Si6 Si1 Ge1 P1 -113.7(3) . . . . ? Si2 Si1 Ge1 P1 149.5(2) . . . . ? Si5 Si1 Ge1 P2 37.7(6) . . . . ? Si6 Si1 Ge1 P2 -105.2(4) . . . . ? Si2 Si1 Ge1 P2 158.0(2) . . . . ? Si5 Si1 Ge1 Si4 -73.7(6) . . . . ? Si6 Si1 Ge1 Si4 143.4(4) . . . . ? Si2 Si1 Ge1 Si4 46.6(3) . . . . ? Si5 Si1 Ge1 Si12 -74.2(6) . . . . ? Si6 Si1 Ge1 Si12 142.8(4) . . . . ? Si2 Si1 Ge1 Si12 46.1(4) . . . . ? Si5 Si1 Ge1 Si9 112(14) . . . . ? Si6 Si1 Ge1 Si9 -31(14) . . . . ? Si2 Si1 Ge1 Si9 -128(14) . . . . ? Si3 Si4 Ge1 P1 -143.3(3) . . . . ? Si7 Si4 Ge1 P1 105.6(3) . . . . ? Si8 Si4 Ge1 P1 -13.8(4) . . . . ? Si3 Si4 Ge1 P2 -134.7(3) . . . . ? Si7 Si4 Ge1 P2 114.1(3) . . . . ? Si8 Si4 Ge1 P2 -5.2(4) . . . . ? Si3 Si4 Ge1 Si1 -31.3(4) . . . . ? Si7 Si4 Ge1 Si1 -142.5(3) . . . . ? Si8 Si4 Ge1 Si1 98.1(4) . . . . ? Si3 Si4 Ge1 Si12 113(21) . . . . ? Si7 Si4 Ge1 Si12 2(21) . . . . ? Si8 Si4 Ge1 Si12 -117(21) . . . . ? Si3 Si4 Ge1 Si9 -31.2(4) . . . . ? Si7 Si4 Ge1 Si9 -142.3(3) . . . . ? Si8 Si4 Ge1 Si9 98.3(4) . . . . ? Si14 Si12 Ge1 P1 -40.4(5) . . . . ? Si13 Si12 Ge1 P1 96.2(3) . . . . ? Si11 Si12 Ge1 P1 -157.1(2) . . . . ? Si14 Si12 Ge1 P2 -32.0(5) . . . . ? Si13 Si12 Ge1 P2 104.6(3) . . . . ? Si11 Si12 Ge1 P2 -148.74(19) . . . . ? Si14 Si12 Ge1 Si1 71.7(5) . . . . ? Si13 Si12 Ge1 Si1 -151.6(4) . . . . ? Si11 Si12 Ge1 Si1 -45.0(3) . . . . ? Si14 Si12 Ge1 Si4 36(21) . . . . ? Si13 Si12 Ge1 Si4 173(21) . . . . ? Si11 Si12 Ge1 Si4 -81(21) . . . . ? Si14 Si12 Ge1 Si9 71.9(5) . . . . ? Si13 Si12 Ge1 Si9 -151.4(4) . . . . ? Si11 Si12 Ge1 Si9 -44.8(3) . . . . ? Si10 Si9 Ge1 P1 133.8(3) . . . . ? Si16 Si9 Ge1 P1 -105.0(3) . . . . ? Si15 Si9 Ge1 P1 8.7(6) . . . . ? Si10 Si9 Ge1 P2 141.9(3) . . . . ? Si16 Si9 Ge1 P2 -97.0(4) . . . . ? Si15 Si9 Ge1 P2 16.8(5) . . . . ? Si10 Si9 Ge1 Si1 36(14) . . . . ? Si16 Si9 Ge1 Si1 157(15) . . . . ? Si15 Si9 Ge1 Si1 -89(14) . . . . ? Si10 Si9 Ge1 Si4 30.2(4) . . . . ? Si16 Si9 Ge1 Si4 151.4(4) . . . . ? Si15 Si9 Ge1 Si4 -94.9(5) . . . . ? Si10 Si9 Ge1 Si12 29.6(4) . . . . ? Si16 Si9 Ge1 Si12 150.8(4) . . . . ? Si15 Si9 Ge1 Si12 -95.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.269 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.074 #===END data_2a_831j _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H63 Ge3 P Si6' _chemical_formula_weight 745.00 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' 'P' 'P' 0.1023 0.0942 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7132(19) _cell_length_b 21.392(4) _cell_length_c 19.039(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.59(3) _cell_angle_gamma 90.00 _cell_volume 3860.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11233 _cell_measurement_theta_min 4.377 _cell_measurement_theta_max 52.539 _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 2.559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4678 _exptl_absorpt_correction_T_max 0.6029 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27252 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6769 _reflns_number_gt 6090 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0691P)^2^+136.9517P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6769 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.1035 _refine_ls_wR_factor_ref 0.2721 _refine_ls_wR_factor_gt 0.2701 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 0.87314(12) 0.16577(5) 0.62385(6) 0.0195(3) Uani 1 1 d . . . Ge2 Ge 0.80626(15) 0.26114(6) 0.54466(7) 0.0305(4) Uani 1 1 d . . . Ge3 Ge 0.86101(12) 0.34718(5) 0.63512(6) 0.0188(3) Uani 1 1 d . . . P1 P 0.9981(4) 0.27762(15) 0.48662(17) 0.0281(7) Uani 1 1 d . . . Si1 Si 0.6891(4) 0.09883(17) 0.5626(2) 0.0313(8) Uani 1 1 d . . . Si2 Si 1.0859(4) 0.10641(18) 0.6526(2) 0.0341(9) Uani 1 1 d . . . Si3 Si 0.8234(4) 0.19701(16) 0.73747(19) 0.0281(8) Uani 1 1 d . . . Si4 Si 0.7511(4) 0.30131(15) 0.72351(18) 0.0248(7) Uani 1 1 d . . . Si5 Si 0.7156(4) 0.43483(16) 0.5889(2) 0.0293(8) Uani 1 1 d . . . Si6 Si 1.0799(4) 0.39196(17) 0.69634(19) 0.0275(8) Uani 1 1 d . . . C1 C 0.9729(15) 0.2319(7) 0.4031(8) 0.039(3) Uani 1 1 d . . . H1A H 0.8737 0.2357 0.3765 0.047 Uiso 1 1 calc R . . H1B H 1.0339 0.2491 0.3724 0.047 Uiso 1 1 calc R . . C2 C 1.0083(16) 0.1631(7) 0.4180(9) 0.046(4) Uani 1 1 d . . . H2A H 1.1060 0.1593 0.4451 0.070 Uiso 1 1 calc R . . H2B H 0.9970 0.1406 0.3723 0.070 Uiso 1 1 calc R . . H2C H 0.9446 0.1454 0.4462 0.070 Uiso 1 1 calc R . . C3 C 0.9907(14) 0.3586(6) 0.4540(7) 0.035(3) Uani 1 1 d . . . H3A H 1.0060 0.3872 0.4958 0.042 Uiso 1 1 calc R . . H3B H 1.0684 0.3653 0.4288 0.042 Uiso 1 1 calc R . . C4 C 0.8528(19) 0.3751(8) 0.4036(9) 0.054(4) Uani 1 1 d . . . H4A H 0.8417 0.3503 0.3595 0.081 Uiso 1 1 calc R . . H4B H 0.8525 0.4197 0.3916 0.081 Uiso 1 1 calc R . . H4C H 0.7746 0.3661 0.4271 0.081 Uiso 1 1 calc R . . C5 C 1.1794(16) 0.2634(7) 0.5308(7) 0.037(3) Uani 1 1 d . . . H5A H 1.1993 0.2865 0.5770 0.044 Uiso 1 1 calc R . . H5B H 1.1901 0.2183 0.5424 0.044 Uiso 1 1 calc R . . C6 C 1.2887(17) 0.2812(9) 0.4901(9) 0.055(4) Uani 1 1 d . . . H6A H 1.2637 0.2634 0.4415 0.083 Uiso 1 1 calc R . . H6B H 1.3807 0.2649 0.5151 0.083 Uiso 1 1 calc R . . H6C H 1.2936 0.3268 0.4869 0.083 Uiso 1 1 calc R . . C7 C 0.702(2) 0.0183(8) 0.5990(11) 0.067(5) Uani 1 1 d . . . H7A H 0.6233 -0.0068 0.5720 0.101 Uiso 1 1 calc R . . H7B H 0.6969 0.0195 0.6499 0.101 Uiso 1 1 calc R . . H7C H 0.7914 -0.0004 0.5944 0.101 Uiso 1 1 calc R . . C8 C 0.6935(16) 0.0919(8) 0.4659(8) 0.047(4) Uani 1 1 d . . . H8A H 0.6174 0.0642 0.4418 0.070 Uiso 1 1 calc R . . H8B H 0.7846 0.0745 0.4614 0.070 Uiso 1 1 calc R . . H8C H 0.6810 0.1333 0.4434 0.070 Uiso 1 1 calc R . . C9 C 0.5117(18) 0.1308(10) 0.5656(11) 0.067(5) Uani 1 1 d . . . H9A H 0.5218 0.1737 0.5841 0.101 Uiso 1 1 calc R . . H9B H 0.4684 0.1048 0.5973 0.101 Uiso 1 1 calc R . . H9C H 0.4517 0.1307 0.5170 0.101 Uiso 1 1 calc R . . C10 C 1.1306(17) 0.0645(7) 0.5745(9) 0.048(4) Uani 1 1 d . . . H10A H 1.2132 0.0378 0.5914 0.072 Uiso 1 1 calc R . . H10B H 1.1516 0.0950 0.5399 0.072 Uiso 1 1 calc R . . H10C H 1.0504 0.0386 0.5511 0.072 Uiso 1 1 calc R . . C11 C 1.0618(19) 0.0450(8) 0.7195(11) 0.061(5) Uani 1 1 d . . . H11A H 1.1509 0.0226 0.7364 0.091 Uiso 1 1 calc R . . H11B H 0.9886 0.0155 0.6966 0.091 Uiso 1 1 calc R . . H11C H 1.0335 0.0650 0.7605 0.091 Uiso 1 1 calc R . . C12 C 1.2447(14) 0.1535(8) 0.6958(8) 0.042(3) Uani 1 1 d . . . H12A H 1.2285 0.1729 0.7399 0.063 Uiso 1 1 calc R . . H12B H 1.2613 0.1861 0.6624 0.063 Uiso 1 1 calc R . . H12C H 1.3273 0.1260 0.7077 0.063 Uiso 1 1 calc R . . C13 C 0.6877(16) 0.1477(7) 0.7672(8) 0.040(3) Uani 1 1 d . . . H13A H 0.7146 0.1036 0.7667 0.060 Uiso 1 1 calc R . . H13B H 0.5959 0.1540 0.7343 0.060 Uiso 1 1 calc R . . H13C H 0.6814 0.1598 0.8160 0.060 Uiso 1 1 calc R . . C14 C 0.9864(16) 0.1917(8) 0.8138(8) 0.045(4) Uani 1 1 d . . . H14A H 0.9711 0.2160 0.8550 0.067 Uiso 1 1 calc R . . H14B H 1.0681 0.2085 0.7975 0.067 Uiso 1 1 calc R . . H14C H 1.0039 0.1479 0.8280 0.067 Uiso 1 1 calc R . . C15 C 0.5513(13) 0.3001(7) 0.6892(8) 0.038(3) Uani 1 1 d . . . H15A H 0.5089 0.2720 0.7193 0.058 Uiso 1 1 calc R . . H15B H 0.5286 0.2852 0.6393 0.058 Uiso 1 1 calc R . . H15C H 0.5137 0.3424 0.6914 0.058 Uiso 1 1 calc R . . C16 C 0.7890(18) 0.3434(7) 0.8127(8) 0.046(4) Uani 1 1 d . . . H16A H 0.7490 0.3856 0.8064 0.069 Uiso 1 1 calc R . . H16B H 0.8913 0.3461 0.8311 0.069 Uiso 1 1 calc R . . H16C H 0.7466 0.3203 0.8471 0.069 Uiso 1 1 calc R . . C17 C 0.8153(16) 0.4941(6) 0.5500(8) 0.039(3) Uani 1 1 d . . . H17A H 0.7545 0.5302 0.5340 0.059 Uiso 1 1 calc R . . H17B H 0.8469 0.4761 0.5089 0.059 Uiso 1 1 calc R . . H17C H 0.8975 0.5075 0.5866 0.059 Uiso 1 1 calc R . . C18 C 0.5612(14) 0.4078(7) 0.5194(9) 0.043(4) Uani 1 1 d . . . H18A H 0.5172 0.4437 0.4912 0.064 Uiso 1 1 calc R . . H18B H 0.4924 0.3878 0.5429 0.064 Uiso 1 1 calc R . . H18C H 0.5927 0.3776 0.4874 0.064 Uiso 1 1 calc R . . C19 C 0.6486(17) 0.4767(7) 0.6608(9) 0.046(4) Uani 1 1 d . . . H19A H 0.7244 0.4801 0.7040 0.069 Uiso 1 1 calc R . . H19B H 0.5696 0.4533 0.6723 0.069 Uiso 1 1 calc R . . H19C H 0.6166 0.5186 0.6439 0.069 Uiso 1 1 calc R . . C20 C 1.1891(14) 0.4236(7) 0.6352(8) 0.037(3) Uani 1 1 d . . . H20A H 1.2774 0.4404 0.6640 0.055 Uiso 1 1 calc R . . H20B H 1.1371 0.4570 0.6055 0.055 Uiso 1 1 calc R . . H20C H 1.2101 0.3901 0.6041 0.055 Uiso 1 1 calc R . . C21 C 1.1917(15) 0.3345(8) 0.7578(9) 0.049(4) Uani 1 1 d . . . H21A H 1.2081 0.2976 0.7302 0.073 Uiso 1 1 calc R . . H21B H 1.1432 0.3220 0.7957 0.073 Uiso 1 1 calc R . . H21C H 1.2823 0.3539 0.7798 0.073 Uiso 1 1 calc R . . C22 C 1.0447(16) 0.4593(7) 0.7540(8) 0.044(4) Uani 1 1 d . . . H22A H 1.1343 0.4749 0.7827 0.066 Uiso 1 1 calc R . . H22B H 0.9849 0.4450 0.7861 0.066 Uiso 1 1 calc R . . H22C H 0.9966 0.4928 0.7231 0.066 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 0.0145(6) 0.0202(6) 0.0246(6) -0.0009(5) 0.0063(5) 0.0026(4) Ge2 0.0368(8) 0.0278(7) 0.0276(7) 0.0005(5) 0.0083(6) -0.0003(6) Ge3 0.0156(6) 0.0191(6) 0.0212(6) 0.0041(5) 0.0031(5) -0.0017(4) P1 0.0365(18) 0.0255(16) 0.0218(16) -0.0001(13) 0.0052(13) -0.0040(14) Si1 0.0287(18) 0.0289(18) 0.037(2) -0.0042(15) 0.0078(15) -0.0092(15) Si2 0.0269(18) 0.0305(19) 0.047(2) 0.0073(16) 0.0129(16) 0.0083(15) Si3 0.0348(19) 0.0264(18) 0.0272(18) 0.0054(14) 0.0157(15) 0.0030(15) Si4 0.0272(17) 0.0238(17) 0.0277(17) 0.0000(13) 0.0156(14) 0.0016(13) Si5 0.0264(18) 0.0231(17) 0.037(2) 0.0019(14) 0.0037(15) 0.0046(14) Si6 0.0244(17) 0.0315(18) 0.0260(17) -0.0042(14) 0.0038(14) -0.0040(14) C1 0.034(8) 0.043(8) 0.040(8) -0.014(7) 0.008(6) -0.004(6) C2 0.035(8) 0.047(9) 0.056(10) -0.022(8) 0.008(7) -0.001(7) C3 0.037(7) 0.032(7) 0.037(7) 0.005(6) 0.011(6) -0.008(6) C4 0.068(11) 0.051(10) 0.039(9) 0.011(7) 0.002(8) -0.005(8) C5 0.052(9) 0.036(7) 0.021(6) 0.002(5) 0.004(6) 0.001(6) C6 0.040(9) 0.071(12) 0.050(10) -0.007(9) -0.002(7) 0.002(8) C7 0.085(14) 0.043(10) 0.068(12) -0.001(9) 0.005(10) -0.017(9) C8 0.043(9) 0.048(9) 0.047(9) -0.016(7) 0.004(7) -0.016(7) C9 0.041(10) 0.084(14) 0.079(13) -0.030(11) 0.019(9) -0.008(9) C10 0.044(9) 0.042(9) 0.059(10) -0.012(7) 0.014(8) 0.007(7) C11 0.051(10) 0.051(10) 0.084(13) 0.025(9) 0.022(9) 0.014(8) C12 0.028(7) 0.057(9) 0.040(8) -0.001(7) 0.007(6) 0.009(7) C13 0.050(9) 0.035(8) 0.044(8) 0.005(6) 0.032(7) -0.005(6) C14 0.048(9) 0.059(10) 0.030(7) 0.011(7) 0.016(7) 0.006(7) C15 0.023(7) 0.042(8) 0.058(9) 0.009(7) 0.024(6) -0.003(6) C16 0.062(10) 0.044(9) 0.039(8) -0.006(7) 0.028(8) -0.007(7) C17 0.048(9) 0.032(7) 0.042(8) 0.007(6) 0.019(7) 0.007(6) C18 0.027(7) 0.036(8) 0.056(9) -0.002(7) -0.010(6) 0.008(6) C19 0.047(9) 0.040(8) 0.052(9) -0.007(7) 0.015(7) 0.002(7) C20 0.031(7) 0.044(8) 0.039(8) -0.011(6) 0.013(6) -0.010(6) C21 0.029(7) 0.068(11) 0.043(9) 0.003(8) -0.006(6) 0.001(7) C22 0.045(9) 0.051(9) 0.038(8) -0.017(7) 0.012(7) -0.015(7) _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 Si2 2.385(4) . ? Ge1 Si1 2.386(4) . ? Ge1 Si3 2.411(4) . ? Ge1 Ge2 2.5358(18) . ? Ge2 P1 2.390(4) . ? Ge2 Ge3 2.4976(18) . ? Ge3 Si6 2.391(4) . ? Ge3 Si4 2.391(3) . ? Ge3 Si5 2.396(4) . ? P1 C5 1.805(15) . ? P1 C3 1.836(13) . ? P1 C1 1.837(14) . ? Si1 C7 1.851(18) . ? Si1 C8 1.858(16) . ? Si1 C9 1.867(18) . ? Si2 C10 1.868(15) . ? Si2 C12 1.875(15) . ? Si2 C11 1.880(17) . ? Si3 C13 1.869(13) . ? Si3 C14 1.904(16) . ? Si3 Si4 2.337(5) . ? Si4 C16 1.886(15) . ? Si4 C15 1.908(14) . ? Si5 C17 1.846(14) . ? Si5 C18 1.863(14) . ? Si5 C19 1.868(15) . ? Si6 C20 1.864(14) . ? Si6 C21 1.872(16) . ? Si6 C22 1.886(15) . ? C1 C2 1.52(2) . ? C3 C4 1.51(2) . ? C5 C6 1.49(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si2 Ge1 Si1 108.17(14) . . ? Si2 Ge1 Si3 105.94(14) . . ? Si1 Ge1 Si3 109.23(13) . . ? Si2 Ge1 Ge2 131.41(11) . . ? Si1 Ge1 Ge2 97.16(11) . . ? Si3 Ge1 Ge2 103.59(10) . . ? P1 Ge2 Ge3 98.04(10) . . ? P1 Ge2 Ge1 105.61(10) . . ? Ge3 Ge2 Ge1 101.21(6) . . ? Si6 Ge3 Si4 107.90(13) . . ? Si6 Ge3 Si5 104.81(13) . . ? Si4 Ge3 Si5 105.16(13) . . ? Si6 Ge3 Ge2 131.64(10) . . ? Si4 Ge3 Ge2 97.02(10) . . ? Si5 Ge3 Ge2 107.68(11) . . ? C5 P1 C3 106.2(6) . . ? C5 P1 C1 104.2(7) . . ? C3 P1 C1 102.8(7) . . ? C5 P1 Ge2 122.7(5) . . ? C3 P1 Ge2 108.6(5) . . ? C1 P1 Ge2 110.6(5) . . ? C7 Si1 C8 106.4(8) . . ? C7 Si1 C9 108.4(10) . . ? C8 Si1 C9 106.3(8) . . ? C7 Si1 Ge1 113.2(6) . . ? C8 Si1 Ge1 110.9(5) . . ? C9 Si1 Ge1 111.3(6) . . ? C10 Si2 C12 107.2(7) . . ? C10 Si2 C11 106.8(8) . . ? C12 Si2 C11 106.8(8) . . ? C10 Si2 Ge1 114.4(5) . . ? C12 Si2 Ge1 113.8(5) . . ? C11 Si2 Ge1 107.3(5) . . ? C13 Si3 C14 105.0(7) . . ? C13 Si3 Si4 111.0(5) . . ? C14 Si3 Si4 108.8(5) . . ? C13 Si3 Ge1 114.1(5) . . ? C14 Si3 Ge1 111.8(5) . . ? Si4 Si3 Ge1 106.06(15) . . ? C16 Si4 C15 107.4(7) . . ? C16 Si4 Si3 111.0(5) . . ? C15 Si4 Si3 106.5(5) . . ? C16 Si4 Ge3 114.1(5) . . ? C15 Si4 Ge3 110.0(5) . . ? Si3 Si4 Ge3 107.61(15) . . ? C17 Si5 C18 109.9(7) . . ? C17 Si5 C19 105.2(7) . . ? C18 Si5 C19 108.3(7) . . ? C17 Si5 Ge3 111.5(5) . . ? C18 Si5 Ge3 109.7(5) . . ? C19 Si5 Ge3 112.2(5) . . ? C20 Si6 C21 107.3(7) . . ? C20 Si6 C22 106.6(7) . . ? C21 Si6 C22 106.9(8) . . ? C20 Si6 Ge3 114.1(5) . . ? C21 Si6 Ge3 112.0(5) . . ? C22 Si6 Ge3 109.6(5) . . ? C2 C1 P1 111.8(11) . . ? C4 C3 P1 113.6(10) . . ? C6 C5 P1 116.6(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si2 Ge1 Ge2 P1 6.91(18) . . . . ? Si1 Ge1 Ge2 P1 -115.09(13) . . . . ? Si3 Ge1 Ge2 P1 133.07(13) . . . . ? Si2 Ge1 Ge2 Ge3 -94.83(16) . . . . ? Si1 Ge1 Ge2 Ge3 143.17(11) . . . . ? Si3 Ge1 Ge2 Ge3 31.34(11) . . . . ? P1 Ge2 Ge3 Si6 -32.14(17) . . . . ? Ge1 Ge2 Ge3 Si6 75.62(14) . . . . ? P1 Ge2 Ge3 Si4 -153.74(12) . . . . ? Ge1 Ge2 Ge3 Si4 -45.98(10) . . . . ? P1 Ge2 Ge3 Si5 97.85(13) . . . . ? Ge1 Ge2 Ge3 Si5 -154.39(11) . . . . ? Ge3 Ge2 P1 C5 68.0(6) . . . . ? Ge1 Ge2 P1 C5 -36.1(6) . . . . ? Ge3 Ge2 P1 C3 -56.4(5) . . . . ? Ge1 Ge2 P1 C3 -160.5(5) . . . . ? Ge3 Ge2 P1 C1 -168.5(5) . . . . ? Ge1 Ge2 P1 C1 87.4(5) . . . . ? Si2 Ge1 Si1 C7 38.1(8) . . . . ? Si3 Ge1 Si1 C7 -76.8(8) . . . . ? Ge2 Ge1 Si1 C7 176.1(8) . . . . ? Si2 Ge1 Si1 C8 -81.4(6) . . . . ? Si3 Ge1 Si1 C8 163.7(6) . . . . ? Ge2 Ge1 Si1 C8 56.5(6) . . . . ? Si2 Ge1 Si1 C9 160.5(8) . . . . ? Si3 Ge1 Si1 C9 45.6(8) . . . . ? Ge2 Ge1 Si1 C9 -61.6(8) . . . . ? Si1 Ge1 Si2 C10 52.5(6) . . . . ? Si3 Ge1 Si2 C10 169.5(6) . . . . ? Ge2 Ge1 Si2 C10 -65.2(6) . . . . ? Si1 Ge1 Si2 C12 176.2(5) . . . . ? Si3 Ge1 Si2 C12 -66.8(5) . . . . ? Ge2 Ge1 Si2 C12 58.5(6) . . . . ? Si1 Ge1 Si2 C11 -65.8(7) . . . . ? Si3 Ge1 Si2 C11 51.2(7) . . . . ? Ge2 Ge1 Si2 C11 176.5(7) . . . . ? Si2 Ge1 Si3 C13 -99.9(6) . . . . ? Si1 Ge1 Si3 C13 16.4(6) . . . . ? Ge2 Ge1 Si3 C13 119.1(5) . . . . ? Si2 Ge1 Si3 C14 19.1(6) . . . . ? Si1 Ge1 Si3 C14 135.4(6) . . . . ? Ge2 Ge1 Si3 C14 -121.9(6) . . . . ? Si2 Ge1 Si3 Si4 137.59(17) . . . . ? Si1 Ge1 Si3 Si4 -106.10(18) . . . . ? Ge2 Ge1 Si3 Si4 -3.38(18) . . . . ? C13 Si3 Si4 C16 82.1(8) . . . . ? C14 Si3 Si4 C16 -33.0(7) . . . . ? Ge1 Si3 Si4 C16 -153.5(5) . . . . ? C13 Si3 Si4 C15 -34.5(7) . . . . ? C14 Si3 Si4 C15 -149.6(7) . . . . ? Ge1 Si3 Si4 C15 89.9(5) . . . . ? C13 Si3 Si4 Ge3 -152.4(5) . . . . ? C14 Si3 Si4 Ge3 92.5(5) . . . . ? Ge1 Si3 Si4 Ge3 -28.0(2) . . . . ? Si6 Ge3 Si4 C16 32.3(6) . . . . ? Si5 Ge3 Si4 C16 -79.2(6) . . . . ? Ge2 Ge3 Si4 C16 170.3(6) . . . . ? Si6 Ge3 Si4 C15 153.1(5) . . . . ? Si5 Ge3 Si4 C15 41.6(5) . . . . ? Ge2 Ge3 Si4 C15 -68.9(5) . . . . ? Si6 Ge3 Si4 Si3 -91.32(18) . . . . ? Si5 Ge3 Si4 Si3 157.22(17) . . . . ? Ge2 Ge3 Si4 Si3 46.70(17) . . . . ? Si6 Ge3 Si5 C17 42.6(5) . . . . ? Si4 Ge3 Si5 C17 156.3(5) . . . . ? Ge2 Ge3 Si5 C17 -101.0(5) . . . . ? Si6 Ge3 Si5 C18 164.5(6) . . . . ? Si4 Ge3 Si5 C18 -81.8(6) . . . . ? Ge2 Ge3 Si5 C18 20.8(6) . . . . ? Si6 Ge3 Si5 C19 -75.1(6) . . . . ? Si4 Ge3 Si5 C19 38.6(6) . . . . ? Ge2 Ge3 Si5 C19 141.3(6) . . . . ? Si4 Ge3 Si6 C20 174.6(5) . . . . ? Si5 Ge3 Si6 C20 -73.7(5) . . . . ? Ge2 Ge3 Si6 C20 57.3(6) . . . . ? Si4 Ge3 Si6 C21 52.5(6) . . . . ? Si5 Ge3 Si6 C21 164.2(6) . . . . ? Ge2 Ge3 Si6 C21 -64.9(6) . . . . ? Si4 Ge3 Si6 C22 -66.0(6) . . . . ? Si5 Ge3 Si6 C22 45.7(6) . . . . ? Ge2 Ge3 Si6 C22 176.6(5) . . . . ? C5 P1 C1 C2 56.4(12) . . . . ? C3 P1 C1 C2 167.0(10) . . . . ? Ge2 P1 C1 C2 -77.2(11) . . . . ? C5 P1 C3 C4 169.3(11) . . . . ? C1 P1 C3 C4 60.1(12) . . . . ? Ge2 P1 C3 C4 -57.1(12) . . . . ? C3 P1 C5 C6 -49.3(13) . . . . ? C1 P1 C5 C6 58.8(13) . . . . ? Ge2 P1 C5 C6 -174.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 5.067 _refine_diff_density_min -1.919 _refine_diff_density_rms 0.244 #===END data_5_818j _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H96 Ge2 Si16' _chemical_formula_weight 1075.71 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.464(6) _cell_length_b 12.362(3) _cell_length_c 20.086(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.87(3) _cell_angle_gamma 90.00 _cell_volume 6283(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4563 _cell_measurement_theta_min 4.588 _cell_measurement_theta_max 52.511 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 1.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6696 _exptl_absorpt_correction_T_max 0.8020 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24041 _diffrn_reflns_av_R_equivalents 0.0866 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.35 _reflns_number_total 6391 _reflns_number_gt 4865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0651P)^2^+39.1281P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6391 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1809 _refine_ls_goodness_of_fit_ref 1.247 _refine_ls_restrained_S_all 1.247 _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 Ge1 Ge 0.05058(3) 0.74283(5) 0.28504(3) 0.01614(19) Uani 1 1 d . . . Si1 Si 0.11626(8) 0.67851(14) 0.23821(10) 0.0186(4) Uani 1 1 d . . . Si2 Si 0.11491(8) 0.80848(16) 0.15012(10) 0.0242(5) Uani 1 1 d . . . Si3 Si 0.05802(9) 0.94756(15) 0.15419(10) 0.0237(5) Uani 1 1 d . . . Si4 Si 0.04628(8) 0.93848(14) 0.26447(9) 0.0205(4) Uani 1 1 d . . . Si5 Si 0.07730(8) 0.65830(14) 0.40186(10) 0.0197(4) Uani 1 1 d . . . Si6 Si 0.20423(8) 0.69627(16) 0.32526(11) 0.0247(5) Uani 1 1 d . . . Si7 Si 0.11029(9) 0.49649(16) 0.19808(11) 0.0259(5) Uani 1 1 d . . . Si8 Si 0.09920(10) 1.07022(15) 0.34768(11) 0.0312(5) Uani 1 1 d . . . C1 C 0.1802(3) 0.8763(7) 0.1664(4) 0.037(2) Uani 1 1 d . . . H1A H 0.2050 0.8229 0.1617 0.056 Uiso 1 1 calc R . . H1B H 0.1946 0.9074 0.2151 0.056 Uiso 1 1 calc R . . H1C H 0.1748 0.9340 0.1307 0.056 Uiso 1 1 calc R . . C2 C 0.0946(3) 0.7596(6) 0.0541(4) 0.0319(18) Uani 1 1 d . . . H2A H 0.0851 0.8217 0.0212 0.048 Uiso 1 1 calc R . . H2B H 0.0640 0.7113 0.0420 0.048 Uiso 1 1 calc R . . H2C H 0.1240 0.7203 0.0492 0.048 Uiso 1 1 calc R . . C3 C -0.0078(3) 0.9297(6) 0.0773(4) 0.0296(17) Uani 1 1 d . . . H3A H -0.0264 0.9992 0.0663 0.044 Uiso 1 1 calc R . . H3B H -0.0289 0.8768 0.0908 0.044 Uiso 1 1 calc R . . H3C H -0.0024 0.9039 0.0345 0.044 Uiso 1 1 calc R . . C4 C 0.0852(4) 1.0792(6) 0.1341(4) 0.038(2) Uani 1 1 d . . . H4A H 0.0891 1.0732 0.0878 0.057 Uiso 1 1 calc R . . H4B H 0.1197 1.0942 0.1726 0.057 Uiso 1 1 calc R . . H4C H 0.0607 1.1384 0.1316 0.057 Uiso 1 1 calc R . . C5 C 0.1329(3) 0.7309(6) 0.4735(4) 0.0277(17) Uani 1 1 d . . . H5A H 0.1519 0.6805 0.5127 0.042 Uiso 1 1 calc R . . H5B H 0.1188 0.7907 0.4926 0.042 Uiso 1 1 calc R . . H5C H 0.1572 0.7595 0.4527 0.042 Uiso 1 1 calc R . . C6 C 0.0218(3) 0.6462(6) 0.4335(4) 0.0245(16) Uani 1 1 d . . . H6A H -0.0119 0.6466 0.3916 0.037 Uiso 1 1 calc R . . H6B H 0.0230 0.7074 0.4651 0.037 Uiso 1 1 calc R . . H6C H 0.0254 0.5784 0.4602 0.037 Uiso 1 1 calc R . . C7 C 0.0987(3) 0.5178(5) 0.3926(4) 0.0296(18) Uani 1 1 d . . . H7A H 0.1100 0.4808 0.4393 0.044 Uiso 1 1 calc R . . H7B H 0.1282 0.5206 0.3767 0.044 Uiso 1 1 calc R . . H7C H 0.0691 0.4784 0.3568 0.044 Uiso 1 1 calc R . . C8 C 0.2272(3) 0.6040(6) 0.4071(4) 0.0335(18) Uani 1 1 d . . . H8A H 0.2654 0.6127 0.4338 0.050 Uiso 1 1 calc R . . H8B H 0.2194 0.5287 0.3913 0.050 Uiso 1 1 calc R . . H8C H 0.2087 0.6230 0.4385 0.050 Uiso 1 1 calc R . . C9 C 0.2502(3) 0.6642(6) 0.2784(4) 0.0359(19) Uani 1 1 d . . . H9A H 0.2384 0.7024 0.2321 0.054 Uiso 1 1 calc R . . H9B H 0.2500 0.5860 0.2699 0.054 Uiso 1 1 calc R . . H9C H 0.2861 0.6873 0.3089 0.054 Uiso 1 1 calc R . . C10 C 0.2176(3) 0.8377(6) 0.3612(4) 0.0333(18) Uani 1 1 d . . . H10A H 0.2402 0.8357 0.4128 0.050 Uiso 1 1 calc R . . H10B H 0.1841 0.8733 0.3544 0.050 Uiso 1 1 calc R . . H10C H 0.2354 0.8780 0.3353 0.050 Uiso 1 1 calc R . . C11 C 0.1159(4) 0.4888(7) 0.1087(5) 0.052(3) Uani 1 1 d . . . H11A H 0.1501 0.5181 0.1130 0.077 Uiso 1 1 calc R . . H11B H 0.0874 0.5310 0.0732 0.077 Uiso 1 1 calc R . . H11C H 0.1131 0.4132 0.0931 0.077 Uiso 1 1 calc R . . C12 C 0.0473(3) 0.4283(6) 0.1906(5) 0.044(2) Uani 1 1 d . . . H12A H 0.0181 0.4542 0.1472 0.065 Uiso 1 1 calc R . . H12B H 0.0399 0.4453 0.2334 0.065 Uiso 1 1 calc R . . H12C H 0.0510 0.3499 0.1873 0.065 Uiso 1 1 calc R . . C13 C 0.1654(3) 0.4107(6) 0.2605(5) 0.040(2) Uani 1 1 d . . . H13A H 0.1652 0.3404 0.2379 0.060 Uiso 1 1 calc R . . H13B H 0.1606 0.4000 0.3059 0.060 Uiso 1 1 calc R . . H13C H 0.1992 0.4469 0.2704 0.060 Uiso 1 1 calc R . . C14 C 0.1375(3) 1.0226(6) 0.4421(4) 0.036(2) Uani 1 1 d . . . H14A H 0.1550 1.0844 0.4726 0.054 Uiso 1 1 calc R . . H14B H 0.1641 0.9699 0.4421 0.054 Uiso 1 1 calc R . . H14C H 0.1133 0.9886 0.4613 0.054 Uiso 1 1 calc R . . C15 C 0.0555(4) 1.1848(6) 0.3501(4) 0.046(2) Uani 1 1 d . . . H15A H 0.0278 1.1578 0.3652 0.070 Uiso 1 1 calc R . . H15B H 0.0392 1.2170 0.3019 0.070 Uiso 1 1 calc R . . H15C H 0.0766 1.2396 0.3845 0.070 Uiso 1 1 calc R . . C16 C 0.1505(4) 1.1278(7) 0.3171(5) 0.059(3) Uani 1 1 d . . . H16A H 0.1330 1.1676 0.2718 0.089 Uiso 1 1 calc R . . H16B H 0.1715 1.0689 0.3094 0.089 Uiso 1 1 calc R . . H16C H 0.1736 1.1770 0.3542 0.089 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 0.0279(4) 0.0071(3) 0.0148(3) 0.0001(3) 0.0098(3) -0.0010(3) Si1 0.0289(11) 0.0090(8) 0.0187(9) -0.0011(7) 0.0101(8) -0.0019(8) Si2 0.0362(13) 0.0192(9) 0.0207(10) 0.0000(8) 0.0148(9) -0.0053(9) Si3 0.0395(13) 0.0136(9) 0.0196(9) 0.0029(8) 0.0132(9) -0.0034(9) Si4 0.0395(12) 0.0082(8) 0.0150(9) -0.0025(7) 0.0117(9) -0.0033(8) Si5 0.0295(11) 0.0140(9) 0.0167(9) 0.0059(7) 0.0102(8) 0.0023(8) Si6 0.0294(12) 0.0187(9) 0.0271(10) -0.0007(8) 0.0121(9) -0.0008(9) Si7 0.0355(13) 0.0138(9) 0.0317(11) -0.0078(8) 0.0168(10) -0.0033(8) Si8 0.0572(15) 0.0101(9) 0.0264(11) -0.0035(8) 0.0164(11) -0.0052(10) C1 0.042(5) 0.038(4) 0.036(4) 0.006(4) 0.019(4) -0.015(4) C2 0.052(5) 0.025(4) 0.028(4) 0.000(3) 0.026(4) -0.004(4) C3 0.037(5) 0.025(4) 0.027(4) 0.001(3) 0.012(4) -0.006(3) C4 0.055(6) 0.026(4) 0.038(5) 0.006(4) 0.023(4) -0.009(4) C5 0.034(4) 0.028(4) 0.020(3) 0.000(3) 0.008(3) -0.006(3) C6 0.034(4) 0.023(4) 0.024(4) 0.008(3) 0.020(3) -0.001(3) C7 0.040(5) 0.008(3) 0.043(5) 0.000(3) 0.018(4) 0.002(3) C8 0.035(5) 0.034(4) 0.029(4) 0.006(3) 0.009(4) -0.005(4) C9 0.040(5) 0.030(4) 0.047(5) 0.005(4) 0.027(4) 0.006(4) C10 0.033(5) 0.026(4) 0.030(4) -0.009(3) 0.002(4) -0.002(3) C11 0.091(8) 0.033(5) 0.043(5) -0.015(4) 0.039(5) 0.007(5) C12 0.034(5) 0.024(4) 0.070(6) -0.008(4) 0.017(5) -0.012(4) C13 0.033(5) 0.022(4) 0.067(6) 0.000(4) 0.020(4) 0.004(3) C14 0.057(6) 0.025(4) 0.027(4) -0.002(3) 0.016(4) 0.001(4) C15 0.076(7) 0.015(4) 0.034(5) -0.001(3) 0.005(5) 0.007(4) C16 0.103(9) 0.036(5) 0.047(5) -0.006(4) 0.038(6) -0.038(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 Si5 2.4079(19) . ? Ge1 Si4 2.4487(19) . ? Ge1 Si1 2.468(2) . ? Ge1 Ge1 2.5805(17) 2 ? Si1 Si7 2.374(3) . ? Si1 Si6 2.379(3) . ? Si1 Si2 2.380(3) . ? Si2 C2 1.887(7) . ? Si2 C1 1.889(8) . ? Si2 Si3 2.346(3) . ? Si3 C3 1.880(7) . ? Si3 C4 1.898(7) . ? Si3 Si4 2.362(3) . ? Si4 Si4 2.377(4) 2 ? Si4 Si8 2.381(3) . ? Si5 C7 1.866(7) . ? Si5 C6 1.870(7) . ? Si5 C5 1.871(7) . ? Si6 C10 1.872(7) . ? Si6 C9 1.887(8) . ? Si6 C8 1.896(7) . ? Si7 C11 1.862(8) . ? Si7 C13 1.874(8) . ? Si7 C12 1.877(8) . ? Si8 C15 1.869(8) . ? Si8 C14 1.871(8) . ? Si8 C16 1.881(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 Si5 Ge1 Si4 124.71(7) . . ? Si5 Ge1 Si1 103.92(7) . . ? Si4 Ge1 Si1 104.38(7) . . ? Si5 Ge1 Ge1 112.79(7) . 2 ? Si4 Ge1 Ge1 86.38(5) . 2 ? Si1 Ge1 Ge1 125.70(6) . 2 ? Si7 Si1 Si6 104.68(10) . . ? Si7 Si1 Si2 114.11(10) . . ? Si6 Si1 Si2 101.66(10) . . ? Si7 Si1 Ge1 118.07(9) . . ? Si6 Si1 Ge1 111.97(9) . . ? Si2 Si1 Ge1 105.27(9) . . ? C2 Si2 C1 101.7(4) . . ? C2 Si2 Si3 109.5(3) . . ? C1 Si2 Si3 105.6(3) . . ? C2 Si2 Si1 117.2(2) . . ? C1 Si2 Si1 115.6(3) . . ? Si3 Si2 Si1 106.68(10) . . ? C3 Si3 C4 104.9(4) . . ? C3 Si3 Si2 109.0(3) . . ? C4 Si3 Si2 107.4(3) . . ? C3 Si3 Si4 109.1(3) . . ? C4 Si3 Si4 116.6(3) . . ? Si2 Si3 Si4 109.48(10) . . ? Si3 Si4 Si4 107.07(12) . 2 ? Si3 Si4 Si8 110.92(10) . . ? Si4 Si4 Si8 118.33(10) 2 . ? Si3 Si4 Ge1 100.95(8) . . ? Si4 Si4 Ge1 91.04(5) 2 . ? Si8 Si4 Ge1 125.51(10) . . ? C7 Si5 C6 106.8(3) . . ? C7 Si5 C5 109.2(4) . . ? C6 Si5 C5 107.9(3) . . ? C7 Si5 Ge1 107.2(3) . . ? C6 Si5 Ge1 112.7(2) . . ? C5 Si5 Ge1 112.9(2) . . ? C10 Si6 C9 108.7(4) . . ? C10 Si6 C8 106.1(4) . . ? C9 Si6 C8 104.1(4) . . ? C10 Si6 Si1 111.1(3) . . ? C9 Si6 Si1 107.4(3) . . ? C8 Si6 Si1 118.9(3) . . ? C11 Si7 C13 105.6(4) . . ? C11 Si7 C12 108.6(4) . . ? C13 Si7 C12 106.2(4) . . ? C11 Si7 Si1 110.8(3) . . ? C13 Si7 Si1 112.2(3) . . ? C12 Si7 Si1 113.1(3) . . ? C15 Si8 C14 109.0(4) . . ? C15 Si8 C16 106.9(4) . . ? C14 Si8 C16 104.7(4) . . ? C15 Si8 Si4 108.3(3) . . ? C14 Si8 Si4 116.5(3) . . ? C16 Si8 Si4 111.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si5 Ge1 Si1 Si7 73.80(11) . . . . ? Si4 Ge1 Si1 Si7 -154.19(10) . . . . ? Ge1 Ge1 Si1 Si7 -58.22(11) 2 . . . ? Si5 Ge1 Si1 Si6 -47.85(10) . . . . ? Si4 Ge1 Si1 Si6 84.16(9) . . . . ? Ge1 Ge1 Si1 Si6 -179.88(6) 2 . . . ? Si5 Ge1 Si1 Si2 -157.49(9) . . . . ? Si4 Ge1 Si1 Si2 -25.48(10) . . . . ? Ge1 Ge1 Si1 Si2 70.49(9) 2 . . . ? Si7 Si1 Si2 C2 13.0(3) . . . . ? Si6 Si1 Si2 C2 125.1(3) . . . . ? Ge1 Si1 Si2 C2 -118.0(3) . . . . ? Si7 Si1 Si2 C1 -106.9(3) . . . . ? Si6 Si1 Si2 C1 5.2(3) . . . . ? Ge1 Si1 Si2 C1 122.1(3) . . . . ? Si7 Si1 Si2 Si3 136.11(11) . . . . ? Si6 Si1 Si2 Si3 -111.81(11) . . . . ? Ge1 Si1 Si2 Si3 5.08(12) . . . . ? C2 Si2 Si3 C3 26.9(4) . . . . ? C1 Si2 Si3 C3 135.7(4) . . . . ? Si1 Si2 Si3 C3 -100.9(3) . . . . ? C2 Si2 Si3 C4 -86.3(4) . . . . ? C1 Si2 Si3 C4 22.5(4) . . . . ? Si1 Si2 Si3 C4 146.0(3) . . . . ? C2 Si2 Si3 Si4 146.2(3) . . . . ? C1 Si2 Si3 Si4 -105.1(3) . . . . ? Si1 Si2 Si3 Si4 18.42(14) . . . . ? C3 Si3 Si4 Si4 -8.9(3) . . . 2 ? C4 Si3 Si4 Si4 109.7(3) . . . 2 ? Si2 Si3 Si4 Si4 -128.17(8) . . . 2 ? C3 Si3 Si4 Si8 -139.4(3) . . . . ? C4 Si3 Si4 Si8 -20.8(3) . . . . ? Si2 Si3 Si4 Si8 101.37(12) . . . . ? C3 Si3 Si4 Ge1 85.6(3) . . . . ? C4 Si3 Si4 Ge1 -155.8(3) . . . . ? Si2 Si3 Si4 Ge1 -33.65(12) . . . . ? Si5 Ge1 Si4 Si3 154.00(9) . . . . ? Si1 Ge1 Si4 Si3 35.33(10) . . . . ? Ge1 Ge1 Si4 Si3 -90.64(9) 2 . . . ? Si5 Ge1 Si4 Si4 -98.39(11) . . . 2 ? Si1 Ge1 Si4 Si4 142.94(9) . . . 2 ? Ge1 Ge1 Si4 Si4 16.97(8) 2 . . 2 ? Si5 Ge1 Si4 Si8 28.20(16) . . . . ? Si1 Ge1 Si4 Si8 -90.47(13) . . . . ? Ge1 Ge1 Si4 Si8 143.56(12) 2 . . . ? Si4 Ge1 Si5 C7 -158.5(3) . . . . ? Si1 Ge1 Si5 C7 -39.6(3) . . . . ? Ge1 Ge1 Si5 C7 99.5(3) 2 . . . ? Si4 Ge1 Si5 C6 84.3(3) . . . . ? Si1 Ge1 Si5 C6 -156.8(3) . . . . ? Ge1 Ge1 Si5 C6 -17.7(3) 2 . . . ? Si4 Ge1 Si5 C5 -38.2(3) . . . . ? Si1 Ge1 Si5 C5 80.6(3) . . . . ? Ge1 Ge1 Si5 C5 -140.2(3) 2 . . . ? Si7 Si1 Si6 C10 177.9(3) . . . . ? Si2 Si1 Si6 C10 58.9(3) . . . . ? Ge1 Si1 Si6 C10 -53.0(3) . . . . ? Si7 Si1 Si6 C9 59.2(3) . . . . ? Si2 Si1 Si6 C9 -59.9(3) . . . . ? Ge1 Si1 Si6 C9 -171.8(3) . . . . ? Si7 Si1 Si6 C8 -58.5(3) . . . . ? Si2 Si1 Si6 C8 -177.6(3) . . . . ? Ge1 Si1 Si6 C8 70.5(3) . . . . ? Si6 Si1 Si7 C11 -101.6(4) . . . . ? Si2 Si1 Si7 C11 8.6(4) . . . . ? Ge1 Si1 Si7 C11 133.1(4) . . . . ? Si6 Si1 Si7 C13 16.1(3) . . . . ? Si2 Si1 Si7 C13 126.3(3) . . . . ? Ge1 Si1 Si7 C13 -109.2(3) . . . . ? Si6 Si1 Si7 C12 136.2(3) . . . . ? Si2 Si1 Si7 C12 -113.6(3) . . . . ? Ge1 Si1 Si7 C12 10.9(4) . . . . ? Si3 Si4 Si8 C15 103.0(3) . . . . ? Si4 Si4 Si8 C15 -21.3(3) 2 . . . ? Ge1 Si4 Si8 C15 -135.5(3) . . . . ? Si3 Si4 Si8 C14 -133.8(3) . . . . ? Si4 Si4 Si8 C14 101.9(3) 2 . . . ? Ge1 Si4 Si8 C14 -12.3(4) . . . . ? Si3 Si4 Si8 C16 -14.1(4) . . . . ? Si4 Si4 Si8 C16 -138.4(4) 2 . . . ? Ge1 Si4 Si8 C16 107.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.545 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.147 #===END data_5a_867 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H96 Ge6 Si12' _chemical_formula_weight 1253.71 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.672(6) _cell_length_b 12.496(3) _cell_length_c 20.276(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.94(3) _cell_angle_gamma 90.00 _cell_volume 6503(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6127 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 52.380 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 2.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3973 _exptl_absorpt_correction_T_max 0.5602 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24786 _diffrn_reflns_av_R_equivalents 0.1198 _diffrn_reflns_av_sigmaI/netI 0.1212 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.76 _reflns_number_total 6733 _reflns_number_gt 4786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6733 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 0.008 _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 Ge1 Ge 0.047204(18) 0.55714(4) 0.26338(3) 0.02279(14) Uani 1 1 d . . . Ge2 Ge 0.049778(18) 0.75348(4) 0.28329(3) 0.02203(13) Uani 1 1 d . . . Ge3 Ge 0.115849(19) 0.81883(4) 0.23445(3) 0.02562(15) Uani 1 1 d . . . Si1 Si 0.07600(5) 0.83711(10) 0.39822(7) 0.0284(3) Uani 1 1 d . . . Si2 Si 0.10936(6) 1.00175(11) 0.19508(8) 0.0357(4) Uani 1 1 d . . . Si3 Si 0.20434(5) 0.80018(11) 0.31920(8) 0.0332(4) Uani 1 1 d . . . Si4 Si 0.11439(5) 0.68787(11) 0.14585(8) 0.0299(3) Uani 1 1 d . . . Si5 Si 0.05847(5) 0.54964(10) 0.15161(7) 0.0270(3) Uani 1 1 d . . . Si6 Si 0.09879(5) 0.42525(11) 0.34582(8) 0.0310(3) Uani 1 1 d . . . C1 C 0.13100(19) 0.7668(4) 0.4685(3) 0.0378(13) Uani 1 1 d . . . H1A H 0.1570 0.7451 0.4489 0.057 Uiso 1 1 calc R . . H1B H 0.1177 0.7034 0.4845 0.057 Uiso 1 1 calc R . . H1C H 0.1472 0.8152 0.5088 0.057 Uiso 1 1 calc R . . C2 C 0.02147(19) 0.8478(4) 0.4315(3) 0.0383(13) Uani 1 1 d . . . H2A H 0.0247 0.9151 0.4577 0.057 Uiso 1 1 calc R . . H2B H 0.0232 0.7874 0.4632 0.057 Uiso 1 1 calc R . . H2C H -0.0120 0.8465 0.3911 0.057 Uiso 1 1 calc R . . C3 C 0.09661(19) 0.9767(4) 0.3880(3) 0.0369(13) Uani 1 1 d . . . H3A H 0.0674 1.0151 0.3529 0.055 Uiso 1 1 calc R . . H3B H 0.1259 0.9744 0.3719 0.055 Uiso 1 1 calc R . . H3C H 0.1074 1.0138 0.4338 0.055 Uiso 1 1 calc R . . C4 C 0.1134(3) 1.0109(5) 0.1050(3) 0.0620(19) Uani 1 1 d . . . H4A H 0.0846 0.9703 0.0706 0.093 Uiso 1 1 calc R . . H4B H 0.1466 0.9811 0.1070 0.093 Uiso 1 1 calc R . . H4C H 0.1109 1.0860 0.0902 0.093 Uiso 1 1 calc R . . C5 C 0.1640(2) 1.0848(4) 0.2556(3) 0.0564(17) Uani 1 1 d . . . H5A H 0.1634 1.1554 0.2342 0.085 Uiso 1 1 calc R . . H5B H 0.1972 1.0495 0.2629 0.085 Uiso 1 1 calc R . . H5C H 0.1601 1.0931 0.3014 0.085 Uiso 1 1 calc R . . C6 C 0.0478(2) 1.0675(4) 0.1911(3) 0.0542(17) Uani 1 1 d . . . H6A H 0.0410 1.0493 0.2338 0.081 Uiso 1 1 calc R . . H6B H 0.0188 1.0425 0.1489 0.081 Uiso 1 1 calc R . . H6C H 0.0513 1.1453 0.1885 0.081 Uiso 1 1 calc R . . C7 C 0.22627(19) 0.8897(4) 0.3988(3) 0.0461(15) Uani 1 1 d . . . H7A H 0.2063 0.8736 0.4286 0.069 Uiso 1 1 calc R . . H7B H 0.2206 0.9645 0.3833 0.069 Uiso 1 1 calc R . . H7C H 0.2634 0.8779 0.4262 0.069 Uiso 1 1 calc R . . C8 C 0.2484(2) 0.8334(4) 0.2708(3) 0.0483(16) Uani 1 1 d . . . H8A H 0.2845 0.8372 0.3048 0.072 Uiso 1 1 calc R . . H8B H 0.2383 0.9025 0.2468 0.072 Uiso 1 1 calc R . . H8C H 0.2455 0.7777 0.2355 0.072 Uiso 1 1 calc R . . C9 C 0.2175(2) 0.6598(4) 0.3539(3) 0.0501(16) Uani 1 1 d . . . H9A H 0.2277 0.6160 0.3212 0.075 Uiso 1 1 calc R . . H9B H 0.1860 0.6299 0.3579 0.075 Uiso 1 1 calc R . . H9C H 0.2458 0.6601 0.4009 0.075 Uiso 1 1 calc R . . C10 C 0.0937(2) 0.7369(4) 0.0521(3) 0.0416(14) Uani 1 1 d . . . H10A H 0.1204 0.7850 0.0479 0.062 Uiso 1 1 calc R . . H10B H 0.0606 0.7756 0.0392 0.062 Uiso 1 1 calc R . . H10C H 0.0892 0.6758 0.0200 0.062 Uiso 1 1 calc R . . C11 C 0.17937(19) 0.6226(4) 0.1599(3) 0.0462(15) Uani 1 1 d . . . H11A H 0.1742 0.5646 0.1254 0.069 Uiso 1 1 calc R . . H11B H 0.1944 0.5934 0.2082 0.069 Uiso 1 1 calc R . . H11C H 0.2031 0.6759 0.1534 0.069 Uiso 1 1 calc R . . C12 C -0.00726(18) 0.5661(4) 0.0778(2) 0.0342(12) Uani 1 1 d . . . H12A H -0.0026 0.5903 0.0346 0.051 Uiso 1 1 calc R . . H12B H -0.0277 0.6191 0.0918 0.051 Uiso 1 1 calc R . . H12C H -0.0256 0.4973 0.0686 0.051 Uiso 1 1 calc R . . C13 C 0.0848(2) 0.4200(4) 0.1307(3) 0.0372(13) Uani 1 1 d . . . H13A H 0.0638 0.3601 0.1364 0.056 Uiso 1 1 calc R . . H13B H 0.1211 0.4108 0.1633 0.056 Uiso 1 1 calc R . . H13C H 0.0833 0.4218 0.0817 0.056 Uiso 1 1 calc R . . C14 C 0.13565(18) 0.4757(4) 0.4375(3) 0.0372(13) Uani 1 1 d . . . H14A H 0.1537 0.4160 0.4681 0.056 Uiso 1 1 calc R . . H14B H 0.1114 0.5086 0.4564 0.056 Uiso 1 1 calc R . . H14C H 0.1612 0.5291 0.4361 0.056 Uiso 1 1 calc R . . C15 C 0.0549(2) 0.3130(4) 0.3497(3) 0.0456(15) Uani 1 1 d . . . H15A H 0.0388 0.2805 0.3025 0.068 Uiso 1 1 calc R . . H15B H 0.0276 0.3409 0.3649 0.068 Uiso 1 1 calc R . . H15C H 0.0753 0.2588 0.3837 0.068 Uiso 1 1 calc R . . C16 C 0.1479(2) 0.3665(4) 0.3125(3) 0.0454(15) Uani 1 1 d . . . H16A H 0.1693 0.4239 0.3049 0.068 Uiso 1 1 calc R . . H16B H 0.1297 0.3290 0.2676 0.068 Uiso 1 1 calc R . . H16C H 0.1702 0.3159 0.3477 0.068 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(3) 0.0178(3) 0.0285(3) 0.0014(2) 0.0102(2) 0.0023(2) Ge2 0.0194(3) 0.0192(3) 0.0285(3) -0.0014(2) 0.0102(2) -0.0007(2) Ge3 0.0223(3) 0.0211(3) 0.0370(3) 0.0004(2) 0.0151(2) 0.0000(2) Si1 0.0236(7) 0.0286(8) 0.0348(8) -0.0079(6) 0.0131(6) -0.0047(6) Si2 0.0323(9) 0.0246(8) 0.0577(10) 0.0072(7) 0.0255(8) 0.0021(6) Si3 0.0220(8) 0.0294(8) 0.0500(9) -0.0014(7) 0.0155(7) 0.0004(6) Si4 0.0251(8) 0.0294(8) 0.0402(9) -0.0015(6) 0.0179(7) 0.0018(6) Si5 0.0263(8) 0.0238(7) 0.0321(8) -0.0028(6) 0.0123(6) 0.0009(6) Si6 0.0319(8) 0.0212(7) 0.0397(8) 0.0058(6) 0.0131(7) 0.0065(6) C1 0.033(3) 0.043(3) 0.038(3) -0.007(3) 0.015(3) -0.003(3) C2 0.028(3) 0.041(3) 0.047(3) -0.010(3) 0.016(3) -0.002(2) C3 0.031(3) 0.030(3) 0.054(3) -0.008(3) 0.020(3) -0.006(2) C4 0.090(5) 0.043(4) 0.074(5) 0.018(3) 0.054(4) 0.002(4) C5 0.050(4) 0.033(3) 0.098(5) 0.000(3) 0.042(4) -0.006(3) C6 0.042(4) 0.033(3) 0.093(5) 0.006(3) 0.032(4) 0.008(3) C7 0.025(3) 0.050(4) 0.062(4) -0.004(3) 0.015(3) -0.004(3) C8 0.035(3) 0.042(4) 0.078(5) -0.008(3) 0.033(3) 0.000(3) C9 0.047(4) 0.040(4) 0.061(4) 0.008(3) 0.017(3) 0.010(3) C10 0.043(3) 0.042(3) 0.050(3) -0.003(3) 0.030(3) -0.001(3) C11 0.029(3) 0.046(4) 0.070(4) -0.013(3) 0.027(3) 0.002(3) C12 0.034(3) 0.033(3) 0.040(3) -0.006(2) 0.020(3) -0.002(2) C13 0.037(3) 0.031(3) 0.047(3) -0.005(2) 0.020(3) 0.004(2) C14 0.032(3) 0.035(3) 0.046(3) 0.009(3) 0.015(3) 0.007(2) C15 0.048(4) 0.030(3) 0.051(4) 0.006(3) 0.010(3) -0.004(3) C16 0.043(3) 0.041(3) 0.053(4) 0.007(3) 0.020(3) 0.023(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 Ge1 Si6 2.4010(15) . ? Ge1 Si5 2.4019(15) . ? Ge1 Ge1 2.4618(11) 2 ? Ge1 Ge2 2.4831(8) . ? Ge2 Si1 2.4052(15) . ? Ge2 Ge3 2.5187(8) . ? Ge2 Ge2 2.5754(13) 2 ? Ge3 Si2 2.4056(15) . ? Ge3 Si4 2.4192(15) . ? Ge3 Si3 2.4206(18) . ? Si1 C1 1.870(5) . ? Si1 C3 1.871(5) . ? Si1 C2 1.874(5) . ? Si2 C5 1.866(6) . ? Si2 C6 1.866(5) . ? Si2 C4 1.875(5) . ? Si3 C7 1.868(5) . ? Si3 C9 1.875(5) . ? Si3 C8 1.876(5) . ? Si4 C10 1.873(5) . ? Si4 C11 1.897(5) . ? Si4 Si5 2.3508(19) . ? Si5 C12 1.886(5) . ? Si5 C13 1.889(5) . ? Si6 C14 1.864(5) . ? Si6 C15 1.877(5) . ? Si6 C16 1.878(5) . ? 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 Si6 Ge1 Si5 112.16(5) . . ? Si6 Ge1 Ge1 117.34(4) . 2 ? Si5 Ge1 Ge1 107.06(5) . 2 ? Si6 Ge1 Ge2 126.26(4) . . ? Si5 Ge1 Ge2 100.72(4) . . ? Ge1 Ge1 Ge2 89.966(16) 2 . ? Si1 Ge2 Ge1 124.53(4) . . ? Si1 Ge2 Ge3 103.86(4) . . ? Ge1 Ge2 Ge3 103.73(2) . . ? Si1 Ge2 Ge2 112.60(5) . 2 ? Ge1 Ge2 Ge2 87.403(16) . 2 ? Ge3 Ge2 Ge2 125.83(3) . 2 ? Si2 Ge3 Si4 114.70(5) . . ? Si2 Ge3 Si3 104.91(5) . . ? Si4 Ge3 Si3 101.18(5) . . ? Si2 Ge3 Ge2 117.61(4) . . ? Si4 Ge3 Ge2 105.04(4) . . ? Si3 Ge3 Ge2 112.34(4) . . ? C1 Si1 C3 109.1(2) . . ? C1 Si1 C2 107.1(2) . . ? C3 Si1 C2 107.0(2) . . ? C1 Si1 Ge2 113.52(16) . . ? C3 Si1 Ge2 106.98(17) . . ? C2 Si1 Ge2 112.83(17) . . ? C5 Si2 C6 106.6(3) . . ? C5 Si2 C4 106.2(3) . . ? C6 Si2 C4 108.5(3) . . ? C5 Si2 Ge3 111.63(19) . . ? C6 Si2 Ge3 112.74(18) . . ? C4 Si2 Ge3 110.93(19) . . ? C7 Si3 C9 106.3(3) . . ? C7 Si3 C8 104.8(2) . . ? C9 Si3 C8 109.3(2) . . ? C7 Si3 Ge3 118.12(17) . . ? C9 Si3 Ge3 111.10(19) . . ? C8 Si3 Ge3 106.9(2) . . ? C10 Si4 C11 101.9(2) . . ? C10 Si4 Si5 109.51(18) . . ? C11 Si4 Si5 106.32(18) . . ? C10 Si4 Ge3 116.53(17) . . ? C11 Si4 Ge3 115.33(18) . . ? Si5 Si4 Ge3 106.79(6) . . ? C12 Si5 C13 104.7(2) . . ? C12 Si5 Si4 109.76(16) . . ? C13 Si5 Si4 107.61(17) . . ? C12 Si5 Ge1 108.54(15) . . ? C13 Si5 Ge1 116.24(17) . . ? Si4 Si5 Ge1 109.76(7) . . ? C14 Si6 C15 109.4(2) . . ? C14 Si6 C16 106.9(2) . . ? C15 Si6 C16 106.8(3) . . ? C14 Si6 Ge1 115.05(17) . . ? C15 Si6 Ge1 108.45(18) . . ? C16 Si6 Ge1 109.86(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si6 Ge1 Ge2 Si1 -25.97(7) . . . . ? Si5 Ge1 Ge2 Si1 -153.91(6) . . . . ? Ge1 Ge1 Ge2 Si1 98.72(6) 2 . . . ? Si6 Ge1 Ge2 Ge3 91.90(5) . . . . ? Si5 Ge1 Ge2 Ge3 -36.05(4) . . . . ? Ge1 Ge1 Ge2 Ge3 -143.41(3) 2 . . . ? Si6 Ge1 Ge2 Ge2 -141.80(5) . . . 2 ? Si5 Ge1 Ge2 Ge2 90.25(5) . . . 2 ? Ge1 Ge1 Ge2 Ge2 -17.11(3) 2 . . 2 ? Si1 Ge2 Ge3 Si2 -73.51(6) . . . . ? Ge1 Ge2 Ge3 Si2 155.10(5) . . . . ? Ge2 Ge2 Ge3 Si2 58.27(5) 2 . . . ? Si1 Ge2 Ge3 Si4 157.53(5) . . . . ? Ge1 Ge2 Ge3 Si4 26.14(4) . . . . ? Ge2 Ge2 Ge3 Si4 -70.69(5) 2 . . . ? Si1 Ge2 Ge3 Si3 48.42(6) . . . . ? Ge1 Ge2 Ge3 Si3 -82.97(5) . . . . ? Ge2 Ge2 Ge3 Si3 -179.80(4) 2 . . . ? Ge1 Ge2 Si1 C1 37.34(19) . . . . ? Ge3 Ge2 Si1 C1 -80.46(18) . . . . ? Ge2 Ge2 Si1 C1 140.45(18) 2 . . . ? Ge1 Ge2 Si1 C3 157.74(16) . . . . ? Ge3 Ge2 Si1 C3 39.94(17) . . . . ? Ge2 Ge2 Si1 C3 -99.15(16) 2 . . . ? Ge1 Ge2 Si1 C2 -84.79(19) . . . . ? Ge3 Ge2 Si1 C2 157.40(18) . . . . ? Ge2 Ge2 Si1 C2 18.32(19) 2 . . . ? Si4 Ge3 Si2 C5 -125.9(2) . . . . ? Si3 Ge3 Si2 C5 -15.8(2) . . . . ? Ge2 Ge3 Si2 C5 109.9(2) . . . . ? Si4 Ge3 Si2 C6 114.1(2) . . . . ? Si3 Ge3 Si2 C6 -135.8(2) . . . . ? Ge2 Ge3 Si2 C6 -10.1(2) . . . . ? Si4 Ge3 Si2 C4 -7.7(2) . . . . ? Si3 Ge3 Si2 C4 102.4(2) . . . . ? Ge2 Ge3 Si2 C4 -132.0(2) . . . . ? Si2 Ge3 Si3 C7 58.6(2) . . . . ? Si4 Ge3 Si3 C7 178.2(2) . . . . ? Ge2 Ge3 Si3 C7 -70.3(2) . . . . ? Si2 Ge3 Si3 C9 -178.2(2) . . . . ? Si4 Ge3 Si3 C9 -58.6(2) . . . . ? Ge2 Ge3 Si3 C9 52.9(2) . . . . ? Si2 Ge3 Si3 C8 -59.02(18) . . . . ? Si4 Ge3 Si3 C8 60.55(18) . . . . ? Ge2 Ge3 Si3 C8 172.08(17) . . . . ? Si2 Ge3 Si4 C10 -13.2(2) . . . . ? Si3 Ge3 Si4 C10 -125.54(19) . . . . ? Ge2 Ge3 Si4 C10 117.45(19) . . . . ? Si2 Ge3 Si4 C11 106.2(2) . . . . ? Si3 Ge3 Si4 C11 -6.1(2) . . . . ? Ge2 Ge3 Si4 C11 -123.1(2) . . . . ? Si2 Ge3 Si4 Si5 -135.94(7) . . . . ? Si3 Ge3 Si4 Si5 111.75(7) . . . . ? Ge2 Ge3 Si4 Si5 -5.27(7) . . . . ? C10 Si4 Si5 C12 -26.7(2) . . . . ? C11 Si4 Si5 C12 -136.0(2) . . . . ? Ge3 Si4 Si5 C12 100.35(16) . . . . ? C10 Si4 Si5 C13 86.8(2) . . . . ? C11 Si4 Si5 C13 -22.6(3) . . . . ? Ge3 Si4 Si5 C13 -146.24(18) . . . . ? C10 Si4 Si5 Ge1 -145.87(17) . . . . ? C11 Si4 Si5 Ge1 104.8(2) . . . . ? Ge3 Si4 Si5 Ge1 -18.87(8) . . . . ? Si6 Ge1 Si5 C12 138.10(16) . . . . ? Ge1 Ge1 Si5 C12 8.04(17) 2 . . . ? Ge2 Ge1 Si5 C12 -85.26(16) . . . . ? Si6 Ge1 Si5 C13 20.44(19) . . . . ? Ge1 Ge1 Si5 C13 -109.62(18) 2 . . . ? Ge2 Ge1 Si5 C13 157.08(18) . . . . ? Si6 Ge1 Si5 Si4 -101.94(7) . . . . ? Ge1 Ge1 Si5 Si4 128.00(5) 2 . . . ? Ge2 Ge1 Si5 Si4 34.70(7) . . . . ? Si5 Ge1 Si6 C14 133.58(18) . . . . ? Ge1 Ge1 Si6 C14 -101.87(18) 2 . . . ? Ge2 Ge1 Si6 C14 10.36(19) . . . . ? Si5 Ge1 Si6 C15 -103.5(2) . . . . ? Ge1 Ge1 Si6 C15 21.0(2) 2 . . . ? Ge2 Ge1 Si6 C15 133.27(19) . . . . ? Si5 Ge1 Si6 C16 12.9(2) . . . . ? Ge1 Ge1 Si6 C16 137.5(2) 2 . . . ? Ge2 Ge1 Si6 C16 -110.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.76 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.912 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.140 #===END data_6_853j _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H60 Ge N2 Si8' _chemical_formula_weight 662.04 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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.388(2) _cell_length_b 20.813(4) _cell_length_c 16.958(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.35(3) _cell_angle_gamma 90.00 _cell_volume 3836.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7243 _cell_measurement_theta_min 4.638 _cell_measurement_theta_max 52.429 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7339 _exptl_absorpt_correction_T_max 0.8483 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30500 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7829 _reflns_number_gt 6530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0443P)^2^+0.4178P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7829 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.003 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 0.16077(2) 0.186957(13) 0.221461(16) 0.01563(8) Uani 1 1 d . . . Si1 Si -0.05309(6) 0.16524(4) 0.22025(4) 0.01599(16) Uani 1 1 d . . . Si2 Si -0.07221(6) 0.10006(3) 0.32935(4) 0.01630(16) Uani 1 1 d . . . Si3 Si 0.12433(7) 0.05380(4) 0.38615(4) 0.01717(17) Uani 1 1 d . . . Si4 Si 0.26249(6) 0.10632(3) 0.32745(4) 0.01573(16) Uani 1 1 d . . . Si5 Si -0.14157(7) 0.10832(4) 0.09597(5) 0.02261(18) Uani 1 1 d . . . Si6 Si -0.17420(7) 0.25815(4) 0.20364(5) 0.02222(18) Uani 1 1 d . . . Si7 Si 0.34035(7) 0.03545(4) 0.24710(5) 0.02001(17) Uani 1 1 d . . . Si8 Si 0.44576(7) 0.14327(4) 0.42424(4) 0.01842(17) Uani 1 1 d . . . N1 N 0.27601(19) 0.31509(10) 0.28261(13) 0.0184(5) Uani 1 1 d . . . N2 N 0.2027(2) 0.27870(10) 0.37620(13) 0.0187(5) Uani 1 1 d . . . C1 C -0.1233(3) 0.14341(14) 0.41191(17) 0.0253(6) Uani 1 1 d . . . H1A H -0.2045 0.1626 0.3870 0.038 Uiso 1 1 calc R . . H1B H -0.0639 0.1772 0.4367 0.038 Uiso 1 1 calc R . . H1C H -0.1279 0.1127 0.4547 0.038 Uiso 1 1 calc R . . C2 C -0.1890(2) 0.03382(13) 0.29174(17) 0.0233(6) Uani 1 1 d . . . H2A H -0.2079 0.0141 0.3390 0.035 Uiso 1 1 calc R . . H2B H -0.1552 0.0012 0.2629 0.035 Uiso 1 1 calc R . . H2C H -0.2643 0.0518 0.2538 0.035 Uiso 1 1 calc R . . C3 C 0.1681(3) 0.05837(15) 0.50274(17) 0.0296(7) Uani 1 1 d . . . H3A H 0.1077 0.0346 0.5222 0.044 Uiso 1 1 calc R . . H3B H 0.1694 0.1034 0.5198 0.044 Uiso 1 1 calc R . . H3C H 0.2498 0.0394 0.5266 0.044 Uiso 1 1 calc R . . C4 C 0.1101(3) -0.03422(13) 0.35907(19) 0.0292(7) Uani 1 1 d . . . H4A H 0.1898 -0.0553 0.3826 0.044 Uiso 1 1 calc R . . H4B H 0.0840 -0.0392 0.2989 0.044 Uiso 1 1 calc R . . H4C H 0.0489 -0.0540 0.3816 0.044 Uiso 1 1 calc R . . C5 C -0.1102(3) 0.01942(14) 0.10385(19) 0.0342(7) Uani 1 1 d . . . H5A H -0.1087 0.0030 0.0500 0.051 Uiso 1 1 calc R . . H5B H -0.1751 -0.0024 0.1207 0.051 Uiso 1 1 calc R . . H5C H -0.0305 0.0114 0.1450 0.051 Uiso 1 1 calc R . . C6 C -0.0778(3) 0.14106(16) 0.01393(17) 0.0350(8) Uani 1 1 d . . . H6A H 0.0123 0.1400 0.0338 0.052 Uiso 1 1 calc R . . H6B H -0.1056 0.1855 0.0013 0.052 Uiso 1 1 calc R . . H6C H -0.1069 0.1148 -0.0361 0.052 Uiso 1 1 calc R . . C7 C -0.3141(3) 0.11538(16) 0.05673(19) 0.0375(8) Uani 1 1 d . . . H7A H -0.3370 0.1605 0.0442 0.056 Uiso 1 1 calc R . . H7B H -0.3499 0.0998 0.0991 0.056 Uiso 1 1 calc R . . H7C H -0.3453 0.0895 0.0065 0.056 Uiso 1 1 calc R . . C8 C -0.1901(3) 0.29355(14) 0.09962(17) 0.0284(7) Uani 1 1 d . . . H8A H -0.2268 0.2617 0.0568 0.043 Uiso 1 1 calc R . . H8B H -0.1087 0.3059 0.0961 0.043 Uiso 1 1 calc R . . H8C H -0.2431 0.3316 0.0915 0.043 Uiso 1 1 calc R . . C9 C -0.3320(3) 0.24039(17) 0.2117(2) 0.0443(9) Uani 1 1 d . . . H9A H -0.3793 0.2804 0.2057 0.066 Uiso 1 1 calc R . . H9B H -0.3249 0.2211 0.2657 0.066 Uiso 1 1 calc R . . H9C H -0.3742 0.2104 0.1679 0.066 Uiso 1 1 calc R . . C10 C -0.1085(3) 0.32254(15) 0.28208(18) 0.0390(8) Uani 1 1 d . . . H10A H -0.0248 0.3329 0.2815 0.058 Uiso 1 1 calc R . . H10B H -0.1064 0.3072 0.3371 0.058 Uiso 1 1 calc R . . H10C H -0.1601 0.3611 0.2685 0.058 Uiso 1 1 calc R . . C11 C 0.2220(3) 0.00857(15) 0.15028(18) 0.0316(7) Uani 1 1 d . . . H11A H 0.1746 0.0458 0.1226 0.047 Uiso 1 1 calc R . . H11B H 0.1664 -0.0224 0.1642 0.047 Uiso 1 1 calc R . . H11C H 0.2629 -0.0117 0.1134 0.047 Uiso 1 1 calc R . . C12 C 0.4123(3) -0.04000(14) 0.30153(18) 0.0286(7) Uani 1 1 d . . . H12A H 0.3570 -0.0595 0.3293 0.043 Uiso 1 1 calc R . . H12B H 0.4909 -0.0295 0.3425 0.043 Uiso 1 1 calc R . . H12C H 0.4266 -0.0703 0.2611 0.043 Uiso 1 1 calc R . . C13 C 0.4582(3) 0.08039(14) 0.21135(18) 0.0280(7) Uani 1 1 d . . . H13A H 0.4889 0.0527 0.1751 0.042 Uiso 1 1 calc R . . H13B H 0.5267 0.0930 0.2593 0.042 Uiso 1 1 calc R . . H13C H 0.4205 0.1189 0.1810 0.042 Uiso 1 1 calc R . . C14 C 0.4313(3) 0.16985(15) 0.52695(17) 0.0288(7) Uani 1 1 d . . . H14A H 0.5133 0.1783 0.5650 0.043 Uiso 1 1 calc R . . H14B H 0.3912 0.1360 0.5498 0.043 Uiso 1 1 calc R . . H14C H 0.3817 0.2091 0.5196 0.043 Uiso 1 1 calc R . . C15 C 0.5107(3) 0.21336(14) 0.38128(18) 0.0263(7) Uani 1 1 d . . . H15A H 0.5973 0.2192 0.4129 0.039 Uiso 1 1 calc R . . H15B H 0.4644 0.2523 0.3852 0.039 Uiso 1 1 calc R . . H15C H 0.5043 0.2051 0.3232 0.039 Uiso 1 1 calc R . . C16 C 0.5677(2) 0.07889(13) 0.44963(17) 0.0244(6) Uani 1 1 d . . . H16A H 0.5861 0.0658 0.3991 0.037 Uiso 1 1 calc R . . H16B H 0.5379 0.0417 0.4736 0.037 Uiso 1 1 calc R . . H16C H 0.6425 0.0957 0.4894 0.037 Uiso 1 1 calc R . . C17 C 0.2092(2) 0.26573(12) 0.29895(16) 0.0169(5) Uani 1 1 d . . . C18 C 0.3132(2) 0.35699(13) 0.34916(17) 0.0204(6) Uani 1 1 d . . . C19 C 0.2664(2) 0.33421(13) 0.40785(17) 0.0203(6) Uani 1 1 d . . . C20 C 0.3111(3) 0.32277(14) 0.20717(17) 0.0277(7) Uani 1 1 d . . . H20A H 0.2734 0.2886 0.1681 0.042 Uiso 1 1 calc R . . H20B H 0.4009 0.3203 0.2204 0.042 Uiso 1 1 calc R . . H20C H 0.2827 0.3646 0.1823 0.042 Uiso 1 1 calc R . . C21 C 0.3958(3) 0.41315(13) 0.34988(18) 0.0256(6) Uani 1 1 d . . . H21A H 0.4050 0.4386 0.3999 0.038 Uiso 1 1 calc R . . H21B H 0.3599 0.4399 0.3011 0.038 Uiso 1 1 calc R . . H21C H 0.4767 0.3976 0.3491 0.038 Uiso 1 1 calc R . . C22 C 0.2776(3) 0.35911(14) 0.49199(18) 0.0306(7) Uani 1 1 d . . . H22A H 0.3337 0.3960 0.5038 0.046 Uiso 1 1 calc R . . H22B H 0.3100 0.3252 0.5328 0.046 Uiso 1 1 calc R . . H22C H 0.1964 0.3725 0.4948 0.046 Uiso 1 1 calc R . . C23 C 0.1339(3) 0.24011(13) 0.41875(16) 0.0223(6) Uani 1 1 d . . . H23A H 0.0810 0.2098 0.3797 0.033 Uiso 1 1 calc R . . H23B H 0.0830 0.2683 0.4414 0.033 Uiso 1 1 calc R . . H23C H 0.1914 0.2162 0.4638 0.033 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 0.01532(15) 0.01815(15) 0.01423(15) 0.00017(11) 0.00565(11) -0.00064(11) Si1 0.0150(4) 0.0179(4) 0.0149(4) 0.0025(3) 0.0042(3) 0.0005(3) Si2 0.0147(4) 0.0186(4) 0.0162(4) 0.0027(3) 0.0055(3) 0.0007(3) Si3 0.0158(4) 0.0190(4) 0.0167(4) 0.0036(3) 0.0048(3) 0.0014(3) Si4 0.0133(3) 0.0186(4) 0.0154(4) -0.0003(3) 0.0045(3) 0.0006(3) Si5 0.0213(4) 0.0293(4) 0.0165(4) -0.0009(3) 0.0046(3) -0.0066(3) Si6 0.0231(4) 0.0244(4) 0.0208(4) 0.0084(3) 0.0091(3) 0.0082(3) Si7 0.0204(4) 0.0218(4) 0.0194(4) -0.0005(3) 0.0082(3) 0.0028(3) Si8 0.0149(4) 0.0226(4) 0.0174(4) 0.0002(3) 0.0042(3) -0.0005(3) N1 0.0148(11) 0.0211(12) 0.0192(12) 0.0017(9) 0.0050(9) -0.0002(9) N2 0.0186(12) 0.0192(12) 0.0191(12) 0.0001(9) 0.0069(10) -0.0006(9) C1 0.0274(16) 0.0282(16) 0.0262(15) 0.0012(13) 0.0172(13) 0.0027(13) C2 0.0166(14) 0.0285(16) 0.0229(15) 0.0047(12) 0.0031(12) -0.0068(12) C3 0.0262(16) 0.0416(19) 0.0219(15) 0.0107(13) 0.0088(13) 0.0011(14) C4 0.0280(16) 0.0209(15) 0.0421(18) 0.0050(14) 0.0155(14) 0.0018(13) C5 0.0419(19) 0.0317(18) 0.0314(17) -0.0084(14) 0.0147(15) -0.0086(15) C6 0.0422(19) 0.044(2) 0.0214(16) -0.0050(14) 0.0134(14) -0.0147(16) C7 0.0261(17) 0.050(2) 0.0310(17) 0.0014(16) -0.0003(14) -0.0088(15) C8 0.0366(18) 0.0225(15) 0.0233(15) 0.0094(12) 0.0046(14) 0.0018(13) C9 0.0319(19) 0.053(2) 0.056(2) 0.0272(18) 0.0256(18) 0.0192(16) C10 0.060(2) 0.0305(18) 0.0254(17) 0.0011(14) 0.0106(16) 0.0235(16) C11 0.0348(18) 0.0343(18) 0.0238(16) -0.0064(13) 0.0059(14) -0.0013(14) C12 0.0313(17) 0.0255(16) 0.0308(16) 0.0002(13) 0.0122(14) 0.0078(13) C13 0.0265(16) 0.0337(17) 0.0273(16) 0.0016(13) 0.0135(13) 0.0058(13) C14 0.0255(16) 0.0395(18) 0.0197(15) -0.0071(13) 0.0042(13) -0.0009(14) C15 0.0179(14) 0.0273(16) 0.0329(17) 0.0024(13) 0.0066(13) -0.0017(12) C16 0.0205(14) 0.0246(15) 0.0247(15) 0.0034(12) 0.0017(12) 0.0003(12) C17 0.0141(13) 0.0188(14) 0.0175(13) 0.0032(11) 0.0041(11) 0.0018(11) C18 0.0177(14) 0.0184(14) 0.0235(14) -0.0014(11) 0.0034(12) 0.0011(11) C19 0.0186(14) 0.0179(14) 0.0232(14) -0.0020(11) 0.0045(12) 0.0012(11) C20 0.0322(17) 0.0297(17) 0.0229(15) 0.0032(13) 0.0108(13) -0.0058(13) C21 0.0241(15) 0.0216(15) 0.0296(16) 0.0006(12) 0.0054(13) -0.0046(12) C22 0.0384(18) 0.0251(16) 0.0302(17) -0.0080(13) 0.0131(14) -0.0066(14) C23 0.0262(15) 0.0239(15) 0.0207(14) 0.0001(12) 0.0129(12) -0.0043(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 Ge1 C17 2.071(3) . ? Ge1 Si1 2.4709(9) . ? Ge1 Si4 2.4795(9) . ? Si1 Si6 2.3429(11) . ? Si1 Si2 2.3561(10) . ? Si1 Si5 2.3652(12) . ? Si2 C2 1.889(3) . ? Si2 C1 1.897(3) . ? Si2 Si3 2.3619(12) . ? Si3 C4 1.884(3) . ? Si3 C3 1.892(3) . ? Si3 Si4 2.3655(11) . ? Si4 Si7 2.3534(11) . ? Si4 Si8 2.3661(13) . ? Si5 C6 1.879(3) . ? Si5 C5 1.882(3) . ? Si5 C7 1.883(3) . ? Si6 C8 1.870(3) . ? Si6 C9 1.879(3) . ? Si6 C10 1.879(3) . ? Si7 C11 1.872(3) . ? Si7 C13 1.878(3) . ? Si7 C12 1.881(3) . ? Si8 C15 1.878(3) . ? Si8 C14 1.881(3) . ? Si8 C16 1.885(3) . ? N1 C17 1.355(3) . ? N1 C18 1.389(3) . ? N1 C20 1.458(3) . ? N2 C17 1.361(3) . ? N2 C19 1.385(3) . ? N2 C23 1.455(3) . ? C18 C19 1.347(4) . ? C18 C21 1.498(4) . ? C19 C22 1.488(4) . ? 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 Ge1 Si1 103.03(7) . . ? C17 Ge1 Si4 95.60(7) . . ? Si1 Ge1 Si4 97.38(3) . . ? Si6 Si1 Si2 112.38(4) . . ? Si6 Si1 Si5 103.13(4) . . ? Si2 Si1 Si5 107.26(4) . . ? Si6 Si1 Ge1 113.17(4) . . ? Si2 Si1 Ge1 114.86(4) . . ? Si5 Si1 Ge1 104.83(4) . . ? C2 Si2 C1 104.86(13) . . ? C2 Si2 Si1 112.06(9) . . ? C1 Si2 Si1 115.23(9) . . ? C2 Si2 Si3 109.03(9) . . ? C1 Si2 Si3 110.78(10) . . ? Si1 Si2 Si3 104.88(4) . . ? C4 Si3 C3 106.29(14) . . ? C4 Si3 Si2 107.14(10) . . ? C3 Si3 Si2 109.14(10) . . ? C4 Si3 Si4 111.50(10) . . ? C3 Si3 Si4 114.57(10) . . ? Si2 Si3 Si4 107.96(4) . . ? Si7 Si4 Si3 111.52(4) . . ? Si7 Si4 Si8 101.46(4) . . ? Si3 Si4 Si8 114.71(4) . . ? Si7 Si4 Ge1 100.36(3) . . ? Si3 Si4 Ge1 113.09(4) . . ? Si8 Si4 Ge1 114.06(4) . . ? C6 Si5 C5 107.59(15) . . ? C6 Si5 C7 107.64(15) . . ? C5 Si5 C7 104.93(15) . . ? C6 Si5 Si1 108.80(10) . . ? C5 Si5 Si1 114.07(10) . . ? C7 Si5 Si1 113.47(11) . . ? C8 Si6 C9 108.69(15) . . ? C8 Si6 C10 107.03(14) . . ? C9 Si6 C10 106.04(17) . . ? C8 Si6 Si1 109.06(10) . . ? C9 Si6 Si1 111.74(11) . . ? C10 Si6 Si1 114.06(11) . . ? C11 Si7 C13 105.23(14) . . ? C11 Si7 C12 105.97(14) . . ? C13 Si7 C12 108.98(13) . . ? C11 Si7 Si4 113.45(10) . . ? C13 Si7 Si4 107.67(10) . . ? C12 Si7 Si4 115.04(10) . . ? C15 Si8 C14 106.51(14) . . ? C15 Si8 C16 106.99(13) . . ? C14 Si8 C16 105.05(13) . . ? C15 Si8 Si4 110.57(10) . . ? C14 Si8 Si4 115.80(10) . . ? C16 Si8 Si4 111.39(9) . . ? C17 N1 C18 111.3(2) . . ? C17 N1 C20 125.5(2) . . ? C18 N1 C20 123.2(2) . . ? C17 N2 C19 111.5(2) . . ? C17 N2 C23 124.0(2) . . ? C19 N2 C23 124.5(2) . . ? N1 C17 N2 104.0(2) . . ? N1 C17 Ge1 122.00(18) . . ? N2 C17 Ge1 133.42(19) . . ? C19 C18 N1 106.7(2) . . ? C19 C18 C21 130.9(3) . . ? N1 C18 C21 122.3(2) . . ? C18 C19 N2 106.5(2) . . ? C18 C19 C22 130.3(3) . . ? N2 C19 C22 123.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Ge1 Si1 Si6 45.29(8) . . . . ? Si4 Ge1 Si1 Si6 142.81(4) . . . . ? C17 Ge1 Si1 Si2 -85.60(8) . . . . ? Si4 Ge1 Si1 Si2 11.92(4) . . . . ? C17 Ge1 Si1 Si5 156.94(8) . . . . ? Si4 Ge1 Si1 Si5 -105.54(4) . . . . ? Si6 Si1 Si2 C2 95.96(11) . . . . ? Si5 Si1 Si2 C2 -16.70(11) . . . . ? Ge1 Si1 Si2 C2 -132.77(10) . . . . ? Si6 Si1 Si2 C1 -23.83(11) . . . . ? Si5 Si1 Si2 C1 -136.49(11) . . . . ? Ge1 Si1 Si2 C1 107.44(11) . . . . ? Si6 Si1 Si2 Si3 -145.90(4) . . . . ? Si5 Si1 Si2 Si3 101.45(5) . . . . ? Ge1 Si1 Si2 Si3 -14.63(5) . . . . ? C2 Si2 Si3 C4 10.28(14) . . . . ? C1 Si2 Si3 C4 125.19(14) . . . . ? Si1 Si2 Si3 C4 -109.89(10) . . . . ? C2 Si2 Si3 C3 -104.40(14) . . . . ? C1 Si2 Si3 C3 10.50(15) . . . . ? Si1 Si2 Si3 C3 135.42(11) . . . . ? C2 Si2 Si3 Si4 130.50(10) . . . . ? C1 Si2 Si3 Si4 -114.60(10) . . . . ? Si1 Si2 Si3 Si4 10.32(5) . . . . ? C4 Si3 Si4 Si7 1.93(11) . . . . ? C3 Si3 Si4 Si7 122.69(11) . . . . ? Si2 Si3 Si4 Si7 -115.50(5) . . . . ? C4 Si3 Si4 Si8 -112.70(11) . . . . ? C3 Si3 Si4 Si8 8.07(12) . . . . ? Si2 Si3 Si4 Si8 129.87(4) . . . . ? C4 Si3 Si4 Ge1 114.15(11) . . . . ? C3 Si3 Si4 Ge1 -125.09(11) . . . . ? Si2 Si3 Si4 Ge1 -3.28(5) . . . . ? C17 Ge1 Si4 Si7 -141.97(8) . . . . ? Si1 Ge1 Si4 Si7 114.07(4) . . . . ? C17 Ge1 Si4 Si3 99.13(8) . . . . ? Si1 Ge1 Si4 Si3 -4.82(4) . . . . ? C17 Ge1 Si4 Si8 -34.34(8) . . . . ? Si1 Ge1 Si4 Si8 -138.30(4) . . . . ? Si6 Si1 Si5 C6 82.65(12) . . . . ? Si2 Si1 Si5 C6 -158.55(12) . . . . ? Ge1 Si1 Si5 C6 -36.02(12) . . . . ? Si6 Si1 Si5 C5 -157.24(12) . . . . ? Si2 Si1 Si5 C5 -38.43(12) . . . . ? Ge1 Si1 Si5 C5 84.10(12) . . . . ? Si6 Si1 Si5 C7 -37.13(12) . . . . ? Si2 Si1 Si5 C7 81.67(12) . . . . ? Ge1 Si1 Si5 C7 -155.80(11) . . . . ? Si2 Si1 Si6 C8 -163.43(11) . . . . ? Si5 Si1 Si6 C8 -48.24(11) . . . . ? Ge1 Si1 Si6 C8 64.45(11) . . . . ? Si2 Si1 Si6 C9 -43.25(13) . . . . ? Si5 Si1 Si6 C9 71.94(13) . . . . ? Ge1 Si1 Si6 C9 -175.37(12) . . . . ? Si2 Si1 Si6 C10 77.00(13) . . . . ? Si5 Si1 Si6 C10 -167.82(12) . . . . ? Ge1 Si1 Si6 C10 -55.12(13) . . . . ? Si3 Si4 Si7 C11 68.67(12) . . . . ? Si8 Si4 Si7 C11 -168.75(11) . . . . ? Ge1 Si4 Si7 C11 -51.37(12) . . . . ? Si3 Si4 Si7 C13 -175.30(10) . . . . ? Si8 Si4 Si7 C13 -52.72(10) . . . . ? Ge1 Si4 Si7 C13 64.66(10) . . . . ? Si3 Si4 Si7 C12 -53.58(12) . . . . ? Si8 Si4 Si7 C12 69.00(12) . . . . ? Ge1 Si4 Si7 C12 -173.63(11) . . . . ? Si7 Si4 Si8 C15 85.77(11) . . . . ? Si3 Si4 Si8 C15 -153.87(10) . . . . ? Ge1 Si4 Si8 C15 -21.17(11) . . . . ? Si7 Si4 Si8 C14 -152.99(11) . . . . ? Si3 Si4 Si8 C14 -32.64(12) . . . . ? Ge1 Si4 Si8 C14 100.07(12) . . . . ? Si7 Si4 Si8 C16 -33.05(10) . . . . ? Si3 Si4 Si8 C16 87.30(11) . . . . ? Ge1 Si4 Si8 C16 -139.99(10) . . . . ? C18 N1 C17 N2 1.6(3) . . . . ? C20 N1 C17 N2 178.6(2) . . . . ? C18 N1 C17 Ge1 -170.59(17) . . . . ? C20 N1 C17 Ge1 6.5(4) . . . . ? C19 N2 C17 N1 -1.3(3) . . . . ? C23 N2 C17 N1 176.8(2) . . . . ? C19 N2 C17 Ge1 169.6(2) . . . . ? C23 N2 C17 Ge1 -12.4(4) . . . . ? Si1 Ge1 C17 N1 -139.64(19) . . . . ? Si4 Ge1 C17 N1 121.4(2) . . . . ? Si1 Ge1 C17 N2 50.9(3) . . . . ? Si4 Ge1 C17 N2 -48.1(2) . . . . ? C17 N1 C18 C19 -1.3(3) . . . . ? C20 N1 C18 C19 -178.5(2) . . . . ? C17 N1 C18 C21 175.5(2) . . . . ? C20 N1 C18 C21 -1.6(4) . . . . ? N1 C18 C19 N2 0.5(3) . . . . ? C21 C18 C19 N2 -176.0(3) . . . . ? N1 C18 C19 C22 179.4(3) . . . . ? C21 C18 C19 C22 2.8(5) . . . . ? C17 N2 C19 C18 0.5(3) . . . . ? C23 N2 C19 C18 -177.6(2) . . . . ? C17 N2 C19 C22 -178.5(2) . . . . ? C23 N2 C19 C22 3.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.570 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.075 #===END data_6a_852j _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H60 Ge3 N2 Si6' _chemical_formula_weight 751.04 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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.436(2) _cell_length_b 20.832(4) _cell_length_c 17.000(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.05(3) _cell_angle_gamma 90.00 _cell_volume 3871.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13103 _cell_measurement_theta_min 4.634 _cell_measurement_theta_max 52.527 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 2.515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5394 _exptl_absorpt_correction_T_max 0.6603 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30692 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.36 _reflns_number_total 7892 _reflns_number_gt 6962 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7892 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 0.444351(18) 0.165618(10) 0.719719(12) 0.01580(6) Uani 1 1 d . . . Ge2 Ge 0.661019(18) 0.187908(10) 0.720098(12) 0.01605(6) Uani 1 1 d . . . Ge3 Ge 0.762702(18) 0.106082(10) 0.828090(12) 0.01561(6) Uani 1 1 d . . . Si1 Si 0.42660(5) 0.09926(3) 0.83034(3) 0.01668(12) Uani 1 1 d . . . Si2 Si 0.62149(5) 0.05309(3) 0.88668(3) 0.01745(12) Uani 1 1 d . . . Si3 Si 0.32174(5) 0.25958(3) 0.70402(4) 0.02339(14) Uani 1 1 d . . . Si4 Si 0.35548(5) 0.10821(3) 0.59407(4) 0.02386(14) Uani 1 1 d . . . Si5 Si 0.84152(5) 0.03421(3) 0.74664(4) 0.02073(13) Uani 1 1 d . . . Si6 Si 0.94696(5) 0.14335(3) 0.92626(3) 0.01893(13) Uani 1 1 d . . . N1 N 0.77535(15) 0.31555(8) 0.78304(10) 0.0189(4) Uani 1 1 d . . . N2 N 0.70069(15) 0.27861(8) 0.87510(10) 0.0182(4) Uani 1 1 d . . . C1 C 0.3747(2) 0.14287(11) 0.91236(13) 0.0264(5) Uani 1 1 d . . . H1A H 0.2948 0.1627 0.8872 0.040 Uiso 1 1 calc R . . H1B H 0.4344 0.1762 0.9376 0.040 Uiso 1 1 calc R . . H1C H 0.3683 0.1122 0.9546 0.040 Uiso 1 1 calc R . . C2 C 0.31085(19) 0.03294(10) 0.79278(13) 0.0240(5) Uani 1 1 d . . . H2A H 0.2946 0.0118 0.8400 0.036 Uiso 1 1 calc R . . H2B H 0.3432 0.0014 0.7618 0.036 Uiso 1 1 calc R . . H2C H 0.2347 0.0511 0.7571 0.036 Uiso 1 1 calc R . . C3 C 0.6081(2) -0.03439(10) 0.85869(16) 0.0315(5) Uani 1 1 d . . . H3A H 0.6877 -0.0552 0.8812 0.047 Uiso 1 1 calc R . . H3B H 0.5815 -0.0389 0.7987 0.047 Uiso 1 1 calc R . . H3C H 0.5479 -0.0547 0.8816 0.047 Uiso 1 1 calc R . . C4 C 0.66569(19) 0.05762(12) 1.00254(13) 0.0289(5) Uani 1 1 d . . . H4A H 0.6069 0.0331 1.0224 0.043 Uiso 1 1 calc R . . H4B H 0.6653 0.1025 1.0196 0.043 Uiso 1 1 calc R . . H4C H 0.7478 0.0396 1.0258 0.043 Uiso 1 1 calc R . . C5 C 0.3888(3) 0.32317(12) 0.78200(15) 0.0416(7) Uani 1 1 d . . . H5A H 0.3351 0.3608 0.7716 0.062 Uiso 1 1 calc R . . H5B H 0.4696 0.3354 0.7780 0.062 Uiso 1 1 calc R . . H5C H 0.3969 0.3066 0.8373 0.062 Uiso 1 1 calc R . . C6 C 0.3051(2) 0.29452(11) 0.60010(13) 0.0285(5) Uani 1 1 d . . . H6A H 0.2676 0.2627 0.5577 0.043 Uiso 1 1 calc R . . H6B H 0.3859 0.3064 0.5957 0.043 Uiso 1 1 calc R . . H6C H 0.2531 0.3328 0.5924 0.043 Uiso 1 1 calc R . . C7 C 0.1659(2) 0.24127(15) 0.71318(18) 0.0491(8) Uani 1 1 d . . . H7A H 0.1188 0.2811 0.7082 0.074 Uiso 1 1 calc R . . H7B H 0.1737 0.2215 0.7668 0.074 Uiso 1 1 calc R . . H7C H 0.1237 0.2116 0.6693 0.074 Uiso 1 1 calc R . . C8 C 0.4191(2) 0.14169(13) 0.51253(14) 0.0373(6) Uani 1 1 d . . . H8A H 0.3895 0.1161 0.4622 0.056 Uiso 1 1 calc R . . H8B H 0.5086 0.1401 0.5318 0.056 Uiso 1 1 calc R . . H8C H 0.3923 0.1863 0.5010 0.056 Uiso 1 1 calc R . . C9 C 0.1840(2) 0.11474(13) 0.55567(16) 0.0398(6) Uani 1 1 d . . . H9A H 0.1607 0.1598 0.5436 0.060 Uiso 1 1 calc R . . H9B H 0.1486 0.0987 0.5979 0.060 Uiso 1 1 calc R . . H9C H 0.1533 0.0891 0.5055 0.060 Uiso 1 1 calc R . . C10 C 0.3889(2) 0.01969(11) 0.60166(16) 0.0376(6) Uani 1 1 d . . . H10A H 0.3922 0.0036 0.5482 0.056 Uiso 1 1 calc R . . H10B H 0.3242 -0.0028 0.6178 0.056 Uiso 1 1 calc R . . H10C H 0.4677 0.0121 0.6430 0.056 Uiso 1 1 calc R . . C11 C 0.7227(2) 0.00778(12) 0.65067(14) 0.0329(6) Uani 1 1 d . . . H11A H 0.7624 -0.0139 0.6142 0.049 Uiso 1 1 calc R . . H11B H 0.6777 0.0453 0.6225 0.049 Uiso 1 1 calc R . . H11C H 0.6656 -0.0219 0.6651 0.049 Uiso 1 1 calc R . . C12 C 0.9135(2) -0.04096(11) 0.80085(14) 0.0302(5) Uani 1 1 d . . . H12A H 0.8594 -0.0601 0.8297 0.045 Uiso 1 1 calc R . . H12B H 0.9923 -0.0304 0.8407 0.045 Uiso 1 1 calc R . . H12C H 0.9265 -0.0716 0.7604 0.045 Uiso 1 1 calc R . . C13 C 0.95833(19) 0.07939(11) 0.71040(14) 0.0286(5) Uani 1 1 d . . . H13A H 0.9887 0.0519 0.6738 0.043 Uiso 1 1 calc R . . H13B H 1.0266 0.0919 0.7580 0.043 Uiso 1 1 calc R . . H13C H 0.9206 0.1179 0.6805 0.043 Uiso 1 1 calc R . . C14 C 1.06779(18) 0.07923(10) 0.95019(13) 0.0253(5) Uani 1 1 d . . . H14A H 1.1420 0.0957 0.9901 0.038 Uiso 1 1 calc R . . H14B H 1.0864 0.0668 0.8996 0.038 Uiso 1 1 calc R . . H14C H 1.0380 0.0417 0.9734 0.038 Uiso 1 1 calc R . . C15 C 1.01030(19) 0.21404(10) 0.88371(14) 0.0257(5) Uani 1 1 d . . . H15A H 1.0969 0.2196 0.9141 0.039 Uiso 1 1 calc R . . H15B H 0.9649 0.2528 0.8894 0.039 Uiso 1 1 calc R . . H15C H 1.0021 0.2066 0.8254 0.039 Uiso 1 1 calc R . . C16 C 0.9299(2) 0.16899(12) 1.02841(13) 0.0301(5) Uani 1 1 d . . . H16A H 0.8929 0.1341 1.0515 0.045 Uiso 1 1 calc R . . H16B H 0.8773 0.2070 1.0208 0.045 Uiso 1 1 calc R . . H16C H 1.0105 0.1792 1.0661 0.045 Uiso 1 1 calc R . . C17 C 0.70804(18) 0.26636(9) 0.79837(12) 0.0181(4) Uani 1 1 d . . . C18 C 0.81184(18) 0.35733(10) 0.84940(13) 0.0210(4) Uani 1 1 d . . . C19 C 0.76452(18) 0.33428(10) 0.90768(13) 0.0206(4) Uani 1 1 d . . . C20 C 0.8109(2) 0.32392(11) 0.70769(13) 0.0271(5) Uani 1 1 d . . . H20A H 0.7727 0.2903 0.6681 0.041 Uiso 1 1 calc R . . H20B H 0.9001 0.3209 0.7206 0.041 Uiso 1 1 calc R . . H20C H 0.7838 0.3661 0.6838 0.041 Uiso 1 1 calc R . . C21 C 0.8937(2) 0.41336(10) 0.85135(14) 0.0275(5) Uani 1 1 d . . . H21A H 0.9030 0.4379 0.9020 0.041 Uiso 1 1 calc R . . H21B H 0.8578 0.4409 0.8037 0.041 Uiso 1 1 calc R . . H21C H 0.9740 0.3981 0.8496 0.041 Uiso 1 1 calc R . . C22 C 0.7740(2) 0.35842(11) 0.99186(14) 0.0316(5) Uani 1 1 d . . . H22A H 0.8278 0.3960 1.0038 0.047 Uiso 1 1 calc R . . H22B H 0.8079 0.3247 1.0323 0.047 Uiso 1 1 calc R . . H22C H 0.6926 0.3704 0.9949 0.047 Uiso 1 1 calc R . . C23 C 0.63196(19) 0.23976(10) 0.91744(13) 0.0224(5) Uani 1 1 d . . . H23A H 0.5732 0.2129 0.8774 0.034 Uiso 1 1 calc R . . H23B H 0.5880 0.2679 0.9453 0.034 Uiso 1 1 calc R . . H23C H 0.6885 0.2123 0.9582 0.034 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 0.01435(11) 0.01847(12) 0.01448(11) 0.00274(8) 0.00405(8) 0.00078(8) Ge2 0.01576(11) 0.01896(12) 0.01410(11) 0.00039(8) 0.00543(9) -0.00086(8) Ge3 0.01320(11) 0.01863(12) 0.01505(11) 0.00010(8) 0.00424(8) 0.00063(8) Si1 0.0149(3) 0.0196(3) 0.0159(3) 0.0030(2) 0.0051(2) 0.0009(2) Si2 0.0157(3) 0.0194(3) 0.0169(3) 0.0042(2) 0.0041(2) 0.0013(2) Si3 0.0239(3) 0.0254(3) 0.0225(3) 0.0082(3) 0.0094(3) 0.0086(3) Si4 0.0224(3) 0.0315(3) 0.0167(3) -0.0008(2) 0.0042(2) -0.0075(3) Si5 0.0218(3) 0.0222(3) 0.0194(3) -0.0006(2) 0.0079(2) 0.0032(2) Si6 0.0147(3) 0.0234(3) 0.0177(3) -0.0002(2) 0.0032(2) -0.0003(2) N1 0.0169(9) 0.0209(9) 0.0192(9) 0.0020(7) 0.0056(7) 0.0001(7) N2 0.0185(9) 0.0177(9) 0.0199(9) -0.0003(7) 0.0080(7) -0.0024(7) C1 0.0279(12) 0.0290(12) 0.0266(12) 0.0015(10) 0.0145(10) 0.0020(10) C2 0.0209(11) 0.0277(12) 0.0225(11) 0.0052(9) 0.0049(9) -0.0053(9) C3 0.0279(12) 0.0209(12) 0.0481(15) 0.0048(11) 0.0148(11) 0.0007(10) C4 0.0208(11) 0.0434(14) 0.0213(11) 0.0092(10) 0.0041(9) -0.0021(10) C5 0.0622(18) 0.0332(14) 0.0256(13) 0.0006(11) 0.0070(12) 0.0226(13) C6 0.0325(13) 0.0267(12) 0.0232(12) 0.0085(10) 0.0034(10) 0.0027(10) C7 0.0375(15) 0.062(2) 0.0565(18) 0.0321(15) 0.0272(14) 0.0259(13) C8 0.0461(15) 0.0475(16) 0.0200(12) -0.0042(11) 0.0123(11) -0.0195(13) C9 0.0249(13) 0.0516(17) 0.0350(14) 0.0011(12) -0.0035(11) -0.0097(12) C10 0.0439(15) 0.0329(14) 0.0376(14) -0.0085(11) 0.0146(12) -0.0100(12) C11 0.0368(14) 0.0370(14) 0.0245(12) -0.0082(10) 0.0082(11) -0.0028(11) C12 0.0353(13) 0.0256(12) 0.0319(13) 0.0006(10) 0.0133(11) 0.0084(10) C13 0.0262(12) 0.0352(13) 0.0281(12) 0.0001(10) 0.0137(10) 0.0029(10) C14 0.0193(11) 0.0271(12) 0.0264(12) 0.0033(10) 0.0019(9) 0.0002(9) C15 0.0188(11) 0.0267(12) 0.0300(12) 0.0027(10) 0.0045(9) -0.0018(9) C16 0.0238(12) 0.0437(15) 0.0212(12) -0.0054(10) 0.0040(9) -0.0014(10) C17 0.0171(10) 0.0177(10) 0.0199(10) 0.0012(8) 0.0059(8) 0.0014(8) C18 0.0176(10) 0.0190(11) 0.0243(11) -0.0004(9) 0.0031(9) 0.0011(8) C19 0.0195(11) 0.0178(11) 0.0223(11) -0.0011(9) 0.0029(9) 0.0004(8) C20 0.0315(13) 0.0279(12) 0.0240(12) 0.0036(10) 0.0116(10) -0.0064(10) C21 0.0263(12) 0.0212(11) 0.0337(13) 0.0019(10) 0.0070(10) -0.0033(9) C22 0.0375(14) 0.0290(13) 0.0301(13) -0.0089(10) 0.0128(11) -0.0080(11) C23 0.0238(11) 0.0244(11) 0.0209(11) 0.0000(9) 0.0096(9) -0.0044(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 Ge1 Si3 2.3767(7) . ? Ge1 Si1 2.3900(7) . ? Ge1 Si4 2.3984(8) . ? Ge1 Ge2 2.5190(6) . ? Ge2 C17 2.076(2) . ? Ge2 Ge3 2.5251(6) . ? Ge3 Si5 2.3882(7) . ? Ge3 Si2 2.4004(7) . ? Ge3 Si6 2.4011(10) . ? Si1 C2 1.890(2) . ? Si1 C1 1.899(2) . ? Si1 Si2 2.3574(10) . ? Si2 C3 1.878(2) . ? Si2 C4 1.887(2) . ? Si3 C6 1.868(2) . ? Si3 C5 1.872(3) . ? Si3 C7 1.873(3) . ? Si4 C8 1.878(2) . ? Si4 C10 1.880(3) . ? Si4 C9 1.882(2) . ? Si5 C11 1.874(2) . ? Si5 C13 1.879(2) . ? Si5 C12 1.880(2) . ? Si6 C15 1.877(2) . ? Si6 C14 1.879(2) . ? Si6 C16 1.881(2) . ? N1 C17 1.352(3) . ? N1 C18 1.389(3) . ? N1 C20 1.464(3) . ? N2 C17 1.356(2) . ? N2 C19 1.395(3) . ? N2 C23 1.457(2) . ? C18 C19 1.349(3) . ? C18 C21 1.490(3) . ? C19 C22 1.490(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 Si3 Ge1 Si1 112.41(3) . . ? Si3 Ge1 Si4 103.22(3) . . ? Si1 Ge1 Si4 107.50(3) . . ? Si3 Ge1 Ge2 113.32(2) . . ? Si1 Ge1 Ge2 114.52(3) . . ? Si4 Ge1 Ge2 104.70(3) . . ? C17 Ge2 Ge1 102.50(6) . . ? C17 Ge2 Ge3 95.05(6) . . ? Ge1 Ge2 Ge3 96.91(2) . . ? Si5 Ge3 Si2 111.50(3) . . ? Si5 Ge3 Si6 101.66(3) . . ? Si2 Ge3 Si6 114.86(2) . . ? Si5 Ge3 Ge2 99.98(2) . . ? Si2 Ge3 Ge2 112.94(2) . . ? Si6 Ge3 Ge2 114.22(3) . . ? C2 Si1 C1 105.02(10) . . ? C2 Si1 Si2 108.90(7) . . ? C1 Si1 Si2 111.01(8) . . ? C2 Si1 Ge1 111.69(7) . . ? C1 Si1 Ge1 114.70(7) . . ? Si2 Si1 Ge1 105.50(3) . . ? C3 Si2 C4 106.85(11) . . ? C3 Si2 Si1 107.19(8) . . ? C4 Si2 Si1 109.61(8) . . ? C3 Si2 Ge3 110.86(8) . . ? C4 Si2 Ge3 113.78(7) . . ? Si1 Si2 Ge3 108.34(3) . . ? C6 Si3 C5 107.51(11) . . ? C6 Si3 C7 108.82(12) . . ? C5 Si3 C7 106.71(14) . . ? C6 Si3 Ge1 108.67(8) . . ? C5 Si3 Ge1 113.42(9) . . ? C7 Si3 Ge1 111.55(9) . . ? C8 Si4 C10 107.45(12) . . ? C8 Si4 C9 107.87(12) . . ? C10 Si4 C9 105.37(12) . . ? C8 Si4 Ge1 108.51(8) . . ? C10 Si4 Ge1 113.79(9) . . ? C9 Si4 Ge1 113.53(9) . . ? C11 Si5 C13 105.40(11) . . ? C11 Si5 C12 106.48(11) . . ? C13 Si5 C12 109.06(10) . . ? C11 Si5 Ge3 112.84(8) . . ? C13 Si5 Ge3 107.55(8) . . ? C12 Si5 Ge3 115.06(8) . . ? C15 Si6 C14 107.39(10) . . ? C15 Si6 C16 106.81(11) . . ? C14 Si6 C16 105.72(11) . . ? C15 Si6 Ge3 110.18(7) . . ? C14 Si6 Ge3 111.13(7) . . ? C16 Si6 Ge3 115.21(8) . . ? C17 N1 C18 111.77(17) . . ? C17 N1 C20 125.38(17) . . ? C18 N1 C20 122.81(17) . . ? C17 N2 C19 111.44(16) . . ? C17 N2 C23 124.43(17) . . ? C19 N2 C23 124.10(17) . . ? N1 C17 N2 104.02(17) . . ? N1 C17 Ge2 121.88(14) . . ? N2 C17 Ge2 133.41(14) . . ? C19 C18 N1 106.49(18) . . ? C19 C18 C21 130.3(2) . . ? N1 C18 C21 123.10(19) . . ? C18 C19 N2 106.27(18) . . ? C18 C19 C22 130.8(2) . . ? N2 C19 C22 122.95(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si3 Ge1 Ge2 C17 45.48(6) . . . . ? Si1 Ge1 Ge2 C17 -85.29(6) . . . . ? Si4 Ge1 Ge2 C17 157.24(6) . . . . ? Si3 Ge1 Ge2 Ge3 142.238(19) . . . . ? Si1 Ge1 Ge2 Ge3 11.469(19) . . . . ? Si4 Ge1 Ge2 Ge3 -106.01(3) . . . . ? C17 Ge2 Ge3 Si5 -142.56(6) . . . . ? Ge1 Ge2 Ge3 Si5 114.17(3) . . . . ? C17 Ge2 Ge3 Si2 98.85(6) . . . . ? Ge1 Ge2 Ge3 Si2 -4.421(19) . . . . ? C17 Ge2 Ge3 Si6 -34.85(6) . . . . ? Ge1 Ge2 Ge3 Si6 -138.12(2) . . . . ? Si3 Ge1 Si1 C2 96.11(8) . . . . ? Si4 Ge1 Si1 C2 -16.80(8) . . . . ? Ge2 Ge1 Si1 C2 -132.67(8) . . . . ? Si3 Ge1 Si1 C1 -23.22(8) . . . . ? Si4 Ge1 Si1 C1 -136.14(8) . . . . ? Ge2 Ge1 Si1 C1 107.99(8) . . . . ? Si3 Ge1 Si1 Si2 -145.71(3) . . . . ? Si4 Ge1 Si1 Si2 101.37(4) . . . . ? Ge2 Ge1 Si1 Si2 -14.50(3) . . . . ? C2 Si1 Si2 C3 10.85(11) . . . . ? C1 Si1 Si2 C3 126.00(11) . . . . ? Ge1 Si1 Si2 C3 -109.17(8) . . . . ? C2 Si1 Si2 C4 -104.77(11) . . . . ? C1 Si1 Si2 C4 10.38(11) . . . . ? Ge1 Si1 Si2 C4 135.21(8) . . . . ? C2 Si1 Si2 Ge3 130.54(7) . . . . ? C1 Si1 Si2 Ge3 -114.31(8) . . . . ? Ge1 Si1 Si2 Ge3 10.52(3) . . . . ? Si5 Ge3 Si2 C3 2.06(9) . . . . ? Si6 Ge3 Si2 C3 -112.90(9) . . . . ? Ge2 Ge3 Si2 C3 113.71(9) . . . . ? Si5 Ge3 Si2 C4 122.52(9) . . . . ? Si6 Ge3 Si2 C4 7.56(9) . . . . ? Ge2 Ge3 Si2 C4 -125.83(9) . . . . ? Si5 Ge3 Si2 Si1 -115.31(3) . . . . ? Si6 Ge3 Si2 Si1 129.73(3) . . . . ? Ge2 Ge3 Si2 Si1 -3.65(3) . . . . ? Si1 Ge1 Si3 C6 -163.28(8) . . . . ? Si4 Ge1 Si3 C6 -47.75(8) . . . . ? Ge2 Ge1 Si3 C6 64.91(9) . . . . ? Si1 Ge1 Si3 C5 77.21(10) . . . . ? Si4 Ge1 Si3 C5 -167.25(10) . . . . ? Ge2 Ge1 Si3 C5 -54.60(10) . . . . ? Si1 Ge1 Si3 C7 -43.31(11) . . . . ? Si4 Ge1 Si3 C7 72.22(11) . . . . ? Ge2 Ge1 Si3 C7 -175.12(10) . . . . ? Si3 Ge1 Si4 C8 82.66(10) . . . . ? Si1 Ge1 Si4 C8 -158.35(10) . . . . ? Ge2 Ge1 Si4 C8 -36.16(10) . . . . ? Si3 Ge1 Si4 C10 -157.78(9) . . . . ? Si1 Ge1 Si4 C10 -38.79(9) . . . . ? Ge2 Ge1 Si4 C10 83.39(9) . . . . ? Si3 Ge1 Si4 C9 -37.26(10) . . . . ? Si1 Ge1 Si4 C9 81.74(10) . . . . ? Ge2 Ge1 Si4 C9 -156.08(9) . . . . ? Si2 Ge3 Si5 C11 68.04(9) . . . . ? Si6 Ge3 Si5 C11 -169.10(9) . . . . ? Ge2 Ge3 Si5 C11 -51.60(9) . . . . ? Si2 Ge3 Si5 C13 -176.15(8) . . . . ? Si6 Ge3 Si5 C13 -53.29(8) . . . . ? Ge2 Ge3 Si5 C13 64.21(8) . . . . ? Si2 Ge3 Si5 C12 -54.42(9) . . . . ? Si6 Ge3 Si5 C12 68.44(9) . . . . ? Ge2 Ge3 Si5 C12 -174.07(9) . . . . ? Si5 Ge3 Si6 C15 86.55(8) . . . . ? Si2 Ge3 Si6 C15 -152.91(8) . . . . ? Ge2 Ge3 Si6 C15 -20.12(8) . . . . ? Si5 Ge3 Si6 C14 -32.35(8) . . . . ? Si2 Ge3 Si6 C14 88.19(8) . . . . ? Ge2 Ge3 Si6 C14 -139.02(7) . . . . ? Si5 Ge3 Si6 C16 -152.54(9) . . . . ? Si2 Ge3 Si6 C16 -32.01(9) . . . . ? Ge2 Ge3 Si6 C16 100.78(9) . . . . ? C18 N1 C17 N2 1.2(2) . . . . ? C20 N1 C17 N2 179.04(18) . . . . ? C18 N1 C17 Ge2 -170.50(14) . . . . ? C20 N1 C17 Ge2 7.4(3) . . . . ? C19 N2 C17 N1 -1.0(2) . . . . ? C23 N2 C17 N1 177.32(17) . . . . ? C19 N2 C17 Ge2 169.27(15) . . . . ? C23 N2 C17 Ge2 -12.4(3) . . . . ? Ge1 Ge2 C17 N1 -140.54(15) . . . . ? Ge3 Ge2 C17 N1 121.22(15) . . . . ? Ge1 Ge2 C17 N2 50.6(2) . . . . ? Ge3 Ge2 C17 N2 -47.6(2) . . . . ? C17 N1 C18 C19 -0.9(2) . . . . ? C20 N1 C18 C19 -178.87(18) . . . . ? C17 N1 C18 C21 175.93(18) . . . . ? C20 N1 C18 C21 -2.0(3) . . . . ? N1 C18 C19 N2 0.3(2) . . . . ? C21 C18 C19 N2 -176.3(2) . . . . ? N1 C18 C19 C22 179.3(2) . . . . ? C21 C18 C19 C22 2.8(4) . . . . ? C17 N2 C19 C18 0.4(2) . . . . ? C23 N2 C19 C18 -177.87(18) . . . . ? C17 N2 C19 C22 -178.70(19) . . . . ? C23 N2 C19 C22 3.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.507 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.071 #===END