# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Wing Leung.' 'Wang-Kin Chiu.' 'Kim-Hung Chong.' 'Thomas C. W. Mak' _publ_contact_author_name 'Wing Leung' _publ_contact_author_email KEVINLEUNG@CUHK.EDU.HK _publ_section_title ; Synthesis of dithiocarboxylic acid anhydride analogue of germanium from the Ge(I) pyridyl-1-azaallyl dimer ; # Attachment '1.CIF' data_CWK26 _database_code_depnum_ccdc_archive 'CCDC 743825' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H54 Ge2 N4 Si4' _chemical_formula_weight 824.39 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.346(3) _cell_length_b 11.006(3) _cell_length_c 15.589(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.301(4) _cell_angle_gamma 90.00 _cell_volume 2173.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 1.523 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.497831 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11671 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7263 _reflns_number_gt 6175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SMART CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SMART CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.0453P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(9) _refine_ls_number_reflns 7263 _refine_ls_number_parameters 433 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.007 _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 0.79274(3) 0.61529(4) 0.32455(3) 0.04231(13) Uani 1 1 d . . . Ge2 Ge 0.75241(3) 0.38382(4) 0.32273(3) 0.04321(13) Uani 1 1 d . . . Si1 Si 0.98697(10) 0.30926(11) 0.21004(9) 0.0456(3) Uani 1 1 d . . . Si2 Si 0.80294(14) 0.78030(13) 0.16263(11) 0.0690(4) Uani 1 1 d . . . Si3 Si 0.54674(12) 0.68075(13) 0.43442(11) 0.0603(4) Uani 1 1 d . . . Si4 Si 0.53685(10) 0.25231(12) 0.22855(9) 0.0502(3) Uani 1 1 d . . . N1 N 0.9461(3) 0.5595(3) 0.3836(2) 0.0420(8) Uani 1 1 d . . . N2 N 0.8291(3) 0.6373(3) 0.2134(2) 0.0481(9) Uani 1 1 d . . . N3 N 0.7556(3) 0.4095(3) 0.4541(2) 0.0465(9) Uani 1 1 d . . . N4 N 0.5984(2) 0.3799(4) 0.2908(2) 0.0441(8) Uani 1 1 d . . . C1 C 0.9924(4) 0.5850(4) 0.4721(3) 0.0526(12) Uani 1 1 d . . . H1A H 0.9518 0.6202 0.5041 0.063 Uiso 1 1 calc R . . C2 C 1.0958(4) 0.5614(5) 0.5163(4) 0.0670(15) Uani 1 1 d . . . H2A H 1.1257 0.5796 0.5773 0.080 Uiso 1 1 calc R . . C3 C 1.1549(4) 0.5096(6) 0.4675(4) 0.0713(16) Uani 1 1 d . . . H3A H 1.2261 0.4934 0.4955 0.086 Uiso 1 1 calc R . . C4 C 1.1094(4) 0.4818(5) 0.3783(3) 0.0555(12) Uani 1 1 d . . . H4A H 1.1504 0.4483 0.3458 0.067 Uiso 1 1 calc R . . C5 C 1.0020(3) 0.5031(4) 0.3352(3) 0.0401(10) Uani 1 1 d . . . C6 C 0.9510(3) 0.4676(4) 0.2404(3) 0.0401(10) Uani 1 1 d . . . C7 C 1.0217(4) 0.2128(5) 0.3151(4) 0.0664(15) Uani 1 1 d . . . H7A H 1.0406 0.1327 0.3014 0.100 Uiso 1 1 calc R . . H7B H 0.9619 0.2079 0.3368 0.100 Uiso 1 1 calc R . . H7C H 1.0801 0.2487 0.3608 0.100 Uiso 1 1 calc R . . C8 C 1.1018(5) 0.3053(6) 0.1644(5) 0.0856(19) Uani 1 1 d . . . H8A H 1.0857 0.3536 0.1105 0.128 Uiso 1 1 calc R . . H8B H 1.1148 0.2229 0.1506 0.128 Uiso 1 1 calc R . . H8C H 1.1634 0.3372 0.2088 0.128 Uiso 1 1 calc R . . C9 C 0.8739(5) 0.2291(5) 0.1293(4) 0.0708(16) Uani 1 1 d . . . H9A H 0.8514 0.2731 0.0732 0.106 Uiso 1 1 calc R . . H9B H 0.8167 0.2242 0.1541 0.106 Uiso 1 1 calc R . . H9C H 0.8953 0.1487 0.1187 0.106 Uiso 1 1 calc R . . C10 C 0.8749(3) 0.5389(4) 0.1854(3) 0.0428(10) Uani 1 1 d . . . C11 C 0.8319(4) 0.5116(5) 0.0857(3) 0.0523(12) Uani 1 1 d . . . C12 C 0.8965(6) 0.5034(6) 0.0310(4) 0.086(2) Uani 1 1 d . . . H12A H 0.9686 0.5175 0.0547 0.104 Uiso 1 1 calc R . . C13 C 0.8504(10) 0.4732(7) -0.0614(5) 0.113(3) Uani 1 1 d . . . H13A H 0.8929 0.4681 -0.0985 0.135 Uiso 1 1 calc R . . C14 C 0.7456(11) 0.4516(9) -0.0965(5) 0.131(4) Uani 1 1 d . . . H14A H 0.7169 0.4297 -0.1569 0.158 Uiso 1 1 calc R . . C15 C 0.6825(7) 0.4618(7) -0.0442(5) 0.111(3) Uani 1 1 d . . . H15A H 0.6104 0.4486 -0.0695 0.133 Uiso 1 1 calc R . . C16 C 0.7235(5) 0.4917(6) 0.0475(3) 0.0731(16) Uani 1 1 d . . . H16A H 0.6789 0.4984 0.0827 0.088 Uiso 1 1 calc R . . C17 C 0.6595(8) 0.8102(9) 0.1192(8) 0.190(6) Uani 1 1 d . . . H17A H 0.6267 0.7526 0.0726 0.286 Uiso 1 1 calc R . . H17B H 0.6476 0.8910 0.0948 0.286 Uiso 1 1 calc R . . H17C H 0.6297 0.8026 0.1675 0.286 Uiso 1 1 calc R . . C18 C 0.8605(17) 0.8026(9) 0.0742(11) 0.351(15) Uani 1 1 d . . . H18A H 0.8366 0.7399 0.0296 0.527 Uiso 1 1 calc R . . H18B H 0.9360 0.7993 0.0990 0.527 Uiso 1 1 calc R . . H18C H 0.8397 0.8805 0.0466 0.527 Uiso 1 1 calc R . . C19 C 0.8498(6) 0.8984(6) 0.2501(5) 0.119(3) Uani 1 1 d . . . H19A H 0.9251 0.8933 0.2757 0.179 Uiso 1 1 calc R . . H19B H 0.8179 0.8861 0.2968 0.179 Uiso 1 1 calc R . . H19C H 0.8306 0.9771 0.2235 0.179 Uiso 1 1 calc R . . C20 C 0.8357(4) 0.3612(6) 0.5207(4) 0.0705(16) Uani 1 1 d . . . H20A H 0.8900 0.3240 0.5051 0.085 Uiso 1 1 calc R . . C21 C 0.8425(5) 0.3634(8) 0.6094(4) 0.094(2) Uani 1 1 d . . . H21A H 0.8995 0.3290 0.6534 0.113 Uiso 1 1 calc R . . C22 C 0.7624(6) 0.4181(8) 0.6312(4) 0.100(3) Uani 1 1 d . . . H22A H 0.7636 0.4192 0.6911 0.120 Uiso 1 1 calc R . . C23 C 0.6782(5) 0.4727(6) 0.5652(3) 0.0770(19) Uani 1 1 d . . . H23A H 0.6241 0.5108 0.5808 0.092 Uiso 1 1 calc R . . C24 C 0.6769(4) 0.4688(4) 0.4738(3) 0.0469(11) Uani 1 1 d . . . C25 C 0.5898(3) 0.5271(4) 0.4039(3) 0.0440(11) Uani 1 1 d . . . C26 C 0.5082(6) 0.7879(5) 0.3371(5) 0.0852(19) Uani 1 1 d . . . H26A H 0.4482 0.7561 0.2908 0.128 Uiso 1 1 calc R . . H26B H 0.5661 0.7976 0.3135 0.128 Uiso 1 1 calc R . . H26C H 0.4905 0.8653 0.3568 0.128 Uiso 1 1 calc R . . C27 C 0.4383(5) 0.6692(6) 0.4872(4) 0.0808(17) Uani 1 1 d . . . H27A H 0.3772 0.6327 0.4450 0.121 Uiso 1 1 calc R . . H27B H 0.4206 0.7490 0.5028 0.121 Uiso 1 1 calc R . . H27C H 0.4616 0.6201 0.5407 0.121 Uiso 1 1 calc R . . C28 C 0.6647(6) 0.7546(7) 0.5196(5) 0.104(3) Uani 1 1 d . . . H28A H 0.7214 0.7612 0.4943 0.156 Uiso 1 1 calc R . . H28B H 0.6869 0.7059 0.5734 0.156 Uiso 1 1 calc R . . H28C H 0.6455 0.8342 0.5343 0.156 Uiso 1 1 calc R . . C29 C 0.5510(3) 0.4749(4) 0.3188(3) 0.0395(10) Uani 1 1 d . . . C30 C 0.4517(4) 0.5230(4) 0.2523(3) 0.0468(11) Uani 1 1 d . . . C31 C 0.4513(5) 0.5578(5) 0.1669(4) 0.0708(15) Uani 1 1 d . . . H31A H 0.5118 0.5484 0.1500 0.085 Uiso 1 1 calc R . . C32 C 0.3606(5) 0.6068(7) 0.1064(4) 0.093(2) Uani 1 1 d . . . H32A H 0.3610 0.6314 0.0495 0.112 Uiso 1 1 calc R . . C33 C 0.2703(5) 0.6191(7) 0.1300(5) 0.099(2) Uani 1 1 d . . . H33A H 0.2098 0.6523 0.0893 0.119 Uiso 1 1 calc R . . C34 C 0.2697(4) 0.5825(5) 0.2130(5) 0.0783(18) Uani 1 1 d . . . H34A H 0.2082 0.5897 0.2286 0.094 Uiso 1 1 calc R . . C35 C 0.3583(3) 0.5355(5) 0.2738(3) 0.0570(12) Uani 1 1 d . . . H35A H 0.3564 0.5113 0.3305 0.068 Uiso 1 1 calc R . . C36 C 0.3998(5) 0.2347(6) 0.2293(5) 0.097(2) Uani 1 1 d . . . H36A H 0.3594 0.3049 0.2024 0.145 Uiso 1 1 calc R . . H36B H 0.3992 0.2264 0.2905 0.145 Uiso 1 1 calc R . . H36C H 0.3692 0.1636 0.1955 0.145 Uiso 1 1 calc R . . C37 C 0.6126(5) 0.1141(6) 0.2808(4) 0.0854(17) Uani 1 1 d . . . H37A H 0.6131 0.1073 0.3423 0.128 Uiso 1 1 calc R . . H37B H 0.6837 0.1205 0.2792 0.128 Uiso 1 1 calc R . . H37C H 0.5798 0.0434 0.2477 0.128 Uiso 1 1 calc R . . C38 C 0.5410(6) 0.2583(7) 0.1100(4) 0.095(2) Uani 1 1 d . . . H38A H 0.5027 0.3283 0.0801 0.142 Uiso 1 1 calc R . . H38B H 0.5093 0.1861 0.0785 0.142 Uiso 1 1 calc R . . H38C H 0.6130 0.2636 0.1106 0.142 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 0.0455(2) 0.0358(3) 0.0520(3) -0.0028(2) 0.02450(19) 0.0018(2) Ge2 0.0384(2) 0.0358(2) 0.0581(3) -0.0038(2) 0.01907(18) -0.0001(2) Si1 0.0510(7) 0.0366(7) 0.0543(8) -0.0051(6) 0.0239(6) 0.0015(5) Si2 0.1083(12) 0.0359(8) 0.0658(9) 0.0114(7) 0.0319(8) 0.0059(8) Si3 0.0702(9) 0.0436(8) 0.0843(10) -0.0176(7) 0.0490(8) -0.0112(7) Si4 0.0488(6) 0.0453(7) 0.0581(8) -0.0144(6) 0.0192(6) -0.0103(6) N1 0.0414(18) 0.041(2) 0.046(2) -0.0085(16) 0.0177(16) -0.0073(16) N2 0.061(2) 0.037(2) 0.054(2) 0.0046(17) 0.0288(17) 0.0094(17) N3 0.0464(19) 0.042(2) 0.050(2) 0.0080(17) 0.0125(16) -0.0056(16) N4 0.0417(17) 0.039(2) 0.055(2) -0.0089(19) 0.0198(15) -0.0011(18) C1 0.061(3) 0.049(3) 0.050(3) -0.015(2) 0.021(2) -0.007(2) C2 0.064(3) 0.068(4) 0.057(3) -0.017(3) 0.001(3) -0.005(3) C3 0.048(3) 0.064(4) 0.086(4) -0.021(3) -0.002(3) 0.002(2) C4 0.043(3) 0.051(3) 0.072(3) -0.011(3) 0.018(2) -0.001(2) C5 0.044(3) 0.031(2) 0.049(2) -0.003(2) 0.020(2) -0.0053(18) C6 0.042(2) 0.035(3) 0.050(2) -0.0003(19) 0.0232(19) 0.0021(19) C7 0.066(3) 0.048(3) 0.077(4) 0.004(3) 0.010(3) 0.003(3) C8 0.079(4) 0.069(4) 0.136(6) -0.019(4) 0.072(4) 0.005(3) C9 0.091(4) 0.042(3) 0.067(4) -0.008(3) 0.008(3) -0.003(3) C10 0.054(3) 0.037(3) 0.047(2) 0.0049(19) 0.029(2) 0.000(2) C11 0.078(4) 0.037(3) 0.045(2) 0.011(2) 0.023(3) 0.012(2) C12 0.148(6) 0.071(4) 0.066(3) 0.010(3) 0.070(4) 0.022(4) C13 0.212(10) 0.079(6) 0.075(5) 0.017(4) 0.085(6) 0.032(7) C14 0.230(12) 0.100(7) 0.056(5) 0.006(4) 0.034(6) 0.050(8) C15 0.136(6) 0.081(5) 0.082(5) -0.009(4) -0.012(5) 0.020(5) C16 0.095(5) 0.057(3) 0.057(3) 0.001(3) 0.007(3) 0.007(3) C17 0.173(9) 0.087(7) 0.217(12) 0.012(7) -0.073(9) 0.022(7) C18 0.78(4) 0.068(6) 0.46(3) 0.077(10) 0.56(3) 0.074(13) C19 0.133(6) 0.046(4) 0.150(7) 0.002(4) 0.003(5) -0.007(4) C20 0.056(3) 0.072(4) 0.074(4) 0.022(3) 0.005(3) -0.008(3) C21 0.075(4) 0.112(6) 0.073(4) 0.021(4) -0.009(3) -0.012(4) C22 0.103(5) 0.138(7) 0.046(3) 0.007(4) 0.006(3) -0.038(5) C23 0.080(4) 0.102(5) 0.054(3) -0.018(3) 0.028(3) -0.037(4) C24 0.049(3) 0.043(3) 0.053(3) -0.007(2) 0.024(2) -0.019(2) C25 0.044(3) 0.041(3) 0.053(3) -0.006(2) 0.025(2) -0.008(2) C26 0.124(5) 0.040(3) 0.117(5) 0.000(3) 0.074(4) 0.002(3) C27 0.092(4) 0.068(4) 0.104(5) -0.013(3) 0.063(4) 0.002(3) C28 0.106(5) 0.089(5) 0.139(6) -0.061(5) 0.072(5) -0.050(4) C29 0.042(2) 0.032(3) 0.050(2) -0.0015(19) 0.022(2) -0.0052(18) C30 0.048(3) 0.035(3) 0.056(3) -0.001(2) 0.015(2) 0.004(2) C31 0.083(4) 0.069(4) 0.063(3) 0.016(3) 0.026(3) 0.004(3) C32 0.097(5) 0.094(5) 0.080(4) 0.036(4) 0.017(3) 0.011(4) C33 0.073(4) 0.093(5) 0.112(5) 0.040(5) 0.001(4) 0.019(4) C34 0.051(3) 0.066(4) 0.111(5) 0.023(4) 0.015(3) 0.013(3) C35 0.043(3) 0.061(3) 0.067(3) 0.010(2) 0.017(2) 0.001(2) C36 0.067(3) 0.075(5) 0.155(7) -0.049(4) 0.046(4) -0.031(3) C37 0.104(4) 0.047(3) 0.109(5) -0.011(4) 0.038(3) 0.001(3) C38 0.121(5) 0.100(5) 0.058(4) -0.026(3) 0.019(3) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 N2 1.955(4) . ? Ge1 N1 2.057(3) . ? Ge1 Ge2 2.6021(8) . ? Ge2 N4 1.957(3) . ? Ge2 N3 2.054(4) . ? Si1 C9 1.856(5) . ? Si1 C8 1.881(5) . ? Si1 C7 1.884(5) . ? Si1 C6 1.907(4) . ? Si2 N2 1.746(4) . ? Si2 C18 1.794(9) . ? Si2 C19 1.845(7) . ? Si2 C17 1.849(9) . ? Si3 C26 1.862(7) . ? Si3 C27 1.880(6) . ? Si3 C25 1.894(5) . ? Si3 C28 1.895(7) . ? Si4 N4 1.757(4) . ? Si4 C36 1.844(6) . ? Si4 C37 1.866(6) . ? Si4 C38 1.867(6) . ? N1 C1 1.352(5) . ? N1 C5 1.366(5) . ? N2 C10 1.381(5) . ? N3 C20 1.344(6) . ? N3 C24 1.352(6) . ? N4 C29 1.363(6) . ? C1 C2 1.360(7) . ? C2 C3 1.379(8) . ? C3 C4 1.365(7) . ? C4 C5 1.400(6) . ? C5 C6 1.471(6) . ? C6 C10 1.355(6) . ? C10 C11 1.508(6) . ? C11 C12 1.393(8) . ? C11 C16 1.398(7) . ? C12 C13 1.417(10) . ? C13 C14 1.354(13) . ? C14 C15 1.347(13) . ? C15 C16 1.400(8) . ? C20 C21 1.357(9) . ? C21 C22 1.358(10) . ? C22 C23 1.399(10) . ? C23 C24 1.419(7) . ? C24 C25 1.468(6) . ? C25 C29 1.388(6) . ? C29 C30 1.500(6) . ? C30 C31 1.385(7) . ? C30 C35 1.395(6) . ? C31 C32 1.389(8) . ? C32 C33 1.373(9) . ? C33 C34 1.358(9) . ? C34 C35 1.364(7) . ? 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 N2 Ge1 N1 86.86(15) . . ? N2 Ge1 Ge2 102.70(11) . . ? N1 Ge1 Ge2 83.44(10) . . ? N4 Ge2 N3 87.05(14) . . ? N4 Ge2 Ge1 102.80(12) . . ? N3 Ge2 Ge1 85.13(10) . . ? C9 Si1 C8 108.5(3) . . ? C9 Si1 C7 104.3(3) . . ? C8 Si1 C7 108.0(3) . . ? C9 Si1 C6 112.9(2) . . ? C8 Si1 C6 114.4(2) . . ? C7 Si1 C6 108.1(2) . . ? N2 Si2 C18 113.5(4) . . ? N2 Si2 C19 109.0(3) . . ? C18 Si2 C19 110.2(6) . . ? N2 Si2 C17 111.3(4) . . ? C18 Si2 C17 109.8(9) . . ? C19 Si2 C17 102.5(4) . . ? C26 Si3 C27 110.2(3) . . ? C26 Si3 C25 112.9(2) . . ? C27 Si3 C25 112.7(2) . . ? C26 Si3 C28 104.8(4) . . ? C27 Si3 C28 107.9(3) . . ? C25 Si3 C28 108.0(3) . . ? N4 Si4 C36 111.9(2) . . ? N4 Si4 C37 108.4(2) . . ? C36 Si4 C37 108.3(3) . . ? N4 Si4 C38 111.3(3) . . ? C36 Si4 C38 110.4(3) . . ? C37 Si4 C38 106.3(3) . . ? C1 N1 C5 120.3(4) . . ? C1 N1 Ge1 117.8(3) . . ? C5 N1 Ge1 121.8(3) . . ? C10 N2 Si2 127.5(3) . . ? C10 N2 Ge1 116.1(3) . . ? Si2 N2 Ge1 116.3(2) . . ? C20 N3 C24 120.1(4) . . ? C20 N3 Ge2 118.6(4) . . ? C24 N3 Ge2 121.3(3) . . ? C29 N4 Si4 127.3(3) . . ? C29 N4 Ge2 117.2(3) . . ? Si4 N4 Ge2 115.49(19) . . ? N1 C1 C2 122.9(5) . . ? C1 C2 C3 117.7(5) . . ? C4 C3 C2 120.4(5) . . ? C3 C4 C5 120.8(5) . . ? N1 C5 C4 117.7(4) . . ? N1 C5 C6 121.0(4) . . ? C4 C5 C6 121.2(4) . . ? C10 C6 C5 120.0(4) . . ? C10 C6 Si1 124.7(3) . . ? C5 C6 Si1 114.8(3) . . ? C6 C10 N2 125.0(4) . . ? C6 C10 C11 120.3(4) . . ? N2 C10 C11 114.8(4) . . ? C12 C11 C16 119.0(5) . . ? C12 C11 C10 122.4(5) . . ? C16 C11 C10 118.6(4) . . ? C11 C12 C13 119.0(7) . . ? C14 C13 C12 121.0(8) . . ? C15 C14 C13 120.2(8) . . ? C14 C15 C16 121.3(9) . . ? C11 C16 C15 119.5(7) . . ? N3 C20 C21 124.2(6) . . ? C20 C21 C22 117.1(6) . . ? C21 C22 C23 121.4(6) . . ? C22 C23 C24 118.5(6) . . ? N3 C24 C23 118.6(5) . . ? N3 C24 C25 122.2(4) . . ? C23 C24 C25 119.3(5) . . ? C29 C25 C24 120.0(4) . . ? C29 C25 Si3 123.9(3) . . ? C24 C25 Si3 115.8(3) . . ? N4 C29 C25 123.5(4) . . ? N4 C29 C30 116.6(3) . . ? C25 C29 C30 119.8(4) . . ? C31 C30 C35 118.0(4) . . ? C31 C30 C29 119.8(4) . . ? C35 C30 C29 122.1(4) . . ? C30 C31 C32 120.0(6) . . ? C33 C32 C31 120.6(6) . . ? C34 C33 C32 119.6(5) . . ? C33 C34 C35 120.8(6) . . ? C34 C35 C30 121.0(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.597 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.060 # Attachment '2.cif' data_CWK30 _database_code_depnum_ccdc_archive 'CCDC 743826' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H54 Ge2 N4 S3 Si4' _chemical_formula_weight 920.57 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 24.360(6) _cell_length_b 11.062(3) _cell_length_c 17.424(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4695(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 1.546 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5345 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SAMRT CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30667 _diffrn_reflns_av_R_equivalents 0.1514 _diffrn_reflns_av_sigmaI/netI 0.2267 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.07 _reflns_number_total 11252 _reflns_number_gt 4331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SAMRT CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SAMRT CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SAMRT CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.0731P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(17) _refine_ls_number_reflns 11252 _refine_ls_number_parameters 461 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2263 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.1943 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S3 S 0.16885(11) 0.3578(3) 0.27453(17) 0.0612(8) Uani 1 1 d . . . Ge1 Ge 0.21951(4) 0.51496(8) 0.31036(7) 0.0478(3) Uani 1 1 d . . . Ge2 Ge 0.09449(4) 0.38205(10) 0.34717(7) 0.0545(3) Uani 1 1 d . . . Si1 Si 0.30017(12) 0.1323(2) 0.31575(19) 0.0546(7) Uani 1 1 d . . . Si2 Si 0.31564(13) 0.6191(3) 0.20802(19) 0.0591(8) Uani 1 1 d . . . Si3 Si 0.07849(12) 0.3328(3) 0.08504(18) 0.0627(9) Uani 1 1 d . . . Si4 Si 0.02189(13) 0.1514(3) 0.38389(18) 0.0593(8) Uani 1 1 d . . . S1 S 0.18489(12) 0.6837(2) 0.32738(18) 0.0725(9) Uani 1 1 d . . . S2 S 0.10042(15) 0.4333(3) 0.4607(2) 0.0873(11) Uani 1 1 d . . . N1 N 0.2563(3) 0.4524(6) 0.4013(4) 0.0403(19) Uani 1 1 d . . . N2 N 0.2815(3) 0.4934(6) 0.2514(4) 0.046(2) Uani 1 1 d . . . N3 N 0.0487(3) 0.4900(7) 0.2847(5) 0.061(3) Uani 1 1 d . . . N4 N 0.0533(3) 0.2498(7) 0.3177(5) 0.0502(19) Uani 1 1 d . . . C1 C 0.2492(4) 0.5047(9) 0.4704(6) 0.055(3) Uani 1 1 d . . . H1A H 0.2249 0.5689 0.4754 0.066 Uiso 1 1 calc R . . C2 C 0.2775(5) 0.4647(11) 0.5336(6) 0.067(3) Uani 1 1 d . . . H2A H 0.2723 0.5016 0.5810 0.081 Uiso 1 1 calc R . . C3 C 0.3131(5) 0.3710(12) 0.5266(6) 0.066(3) Uani 1 1 d . . . H3A H 0.3320 0.3423 0.5693 0.079 Uiso 1 1 calc R . . C4 C 0.3211(4) 0.3190(10) 0.4558(6) 0.057(3) Uani 1 1 d . . . H4A H 0.3459 0.2555 0.4508 0.068 Uiso 1 1 calc R . . C5 C 0.2932(4) 0.3588(8) 0.3927(6) 0.041(2) Uani 1 1 d . . . C6 C 0.3018(3) 0.3028(7) 0.3167(6) 0.037(2) Uani 1 1 d . . . C7 C 0.2536(6) 0.0840(12) 0.3944(8) 0.093(4) Uani 1 1 d . . . H7A H 0.2517 -0.0027 0.3957 0.140 Uiso 1 1 calc R . . H7B H 0.2175 0.1162 0.3855 0.140 Uiso 1 1 calc R . . H7C H 0.2673 0.1134 0.4425 0.140 Uiso 1 1 calc R . . C8 C 0.2700(4) 0.0730(10) 0.2263(7) 0.067(3) Uani 1 1 d . . . H8A H 0.2699 -0.0138 0.2279 0.100 Uiso 1 1 calc R . . H8B H 0.2915 0.0997 0.1833 0.100 Uiso 1 1 calc R . . H8C H 0.2331 0.1020 0.2211 0.100 Uiso 1 1 calc R . . C9 C 0.3678(5) 0.0625(9) 0.3319(7) 0.080(4) Uani 1 1 d . . . H9A H 0.3642 -0.0240 0.3310 0.119 Uiso 1 1 calc R . . H9B H 0.3817 0.0873 0.3810 0.119 Uiso 1 1 calc R . . H9C H 0.3927 0.0876 0.2923 0.119 Uiso 1 1 calc R . . C10 C 0.3008(3) 0.3746(9) 0.2527(5) 0.038(2) Uani 1 1 d . . . C11 C 0.3201(4) 0.3277(8) 0.1767(5) 0.040(2) Uani 1 1 d . . . C12 C 0.2897(4) 0.3450(9) 0.1124(6) 0.052(3) Uani 1 1 d . . . H12A H 0.2565 0.3858 0.1156 0.062 Uiso 1 1 calc R . . C13 C 0.3079(5) 0.3021(10) 0.0416(6) 0.063(3) Uani 1 1 d . . . H13A H 0.2870 0.3155 -0.0023 0.076 Uiso 1 1 calc R . . C14 C 0.3561(5) 0.2406(10) 0.0364(7) 0.064(3) Uani 1 1 d . . . H14A H 0.3678 0.2105 -0.0107 0.077 Uiso 1 1 calc R . . C15 C 0.3879(5) 0.2228(10) 0.1017(7) 0.070(3) Uani 1 1 d . . . H15A H 0.4210 0.1814 0.0982 0.084 Uiso 1 1 calc R . . C16 C 0.3703(4) 0.2666(9) 0.1715(6) 0.054(3) Uani 1 1 d . . . H16A H 0.3918 0.2556 0.2151 0.064 Uiso 1 1 calc R . . C17 C 0.3785(5) 0.5765(10) 0.1592(7) 0.076(4) Uani 1 1 d . . . H17A H 0.3701 0.5223 0.1178 0.114 Uiso 1 1 calc R . . H17B H 0.4027 0.5370 0.1948 0.114 Uiso 1 1 calc R . . H17C H 0.3961 0.6475 0.1392 0.114 Uiso 1 1 calc R . . C18 C 0.3360(5) 0.7226(10) 0.2875(9) 0.106(5) Uani 1 1 d . . . H18A H 0.3613 0.6818 0.3210 0.159 Uiso 1 1 calc R . . H18B H 0.3040 0.7460 0.3160 0.159 Uiso 1 1 calc R . . H18C H 0.3533 0.7932 0.2665 0.159 Uiso 1 1 calc R . . C19 C 0.2684(6) 0.6958(12) 0.1425(9) 0.121(6) Uani 1 1 d . . . H19A H 0.2577 0.6411 0.1025 0.182 Uiso 1 1 calc R . . H19B H 0.2863 0.7648 0.1205 0.182 Uiso 1 1 calc R . . H19C H 0.2365 0.7217 0.1703 0.182 Uiso 1 1 calc R . . C20 C 0.0321(5) 0.5985(9) 0.3130(8) 0.071(3) Uani 1 1 d . . . H20A H 0.0441 0.6232 0.3611 0.085 Uiso 1 1 calc R . . C21 C -0.0015(6) 0.6703(13) 0.2725(11) 0.095(5) Uani 1 1 d . . . H21A H -0.0128 0.7443 0.2923 0.115 Uiso 1 1 calc R . . C22 C -0.0192(6) 0.6325(13) 0.1999(12) 0.103(5) Uani 1 1 d . . . H22A H -0.0424 0.6819 0.1714 0.123 Uiso 1 1 calc R . . C23 C -0.0036(4) 0.5289(10) 0.1719(8) 0.069(4) Uani 1 1 d . . . H23A H -0.0154 0.5056 0.1233 0.083 Uiso 1 1 calc R . . C24 C 0.0315(4) 0.4503(9) 0.2153(7) 0.051(3) Uani 1 1 d . . . C25 C 0.0490(4) 0.3314(9) 0.1847(6) 0.051(3) Uani 1 1 d . . . C26 C 0.1339(5) 0.2206(11) 0.0724(8) 0.079(4) Uani 1 1 d . . . H26A H 0.1191 0.1407 0.0777 0.118 Uiso 1 1 calc R . . H26B H 0.1616 0.2334 0.1106 0.118 Uiso 1 1 calc R . . H26C H 0.1497 0.2295 0.0222 0.118 Uiso 1 1 calc R . . C27 C 0.0287(5) 0.3121(15) 0.0040(7) 0.099(5) Uani 1 1 d . . . H27A H 0.0108 0.2352 0.0090 0.149 Uiso 1 1 calc R . . H27B H 0.0480 0.3153 -0.0440 0.149 Uiso 1 1 calc R . . H27C H 0.0017 0.3753 0.0055 0.149 Uiso 1 1 calc R . . C28 C 0.1121(6) 0.4866(12) 0.0720(9) 0.107(5) Uani 1 1 d . . . H28A H 0.1374 0.5008 0.1132 0.160 Uiso 1 1 calc R . . H28B H 0.0843 0.5483 0.0722 0.160 Uiso 1 1 calc R . . H28C H 0.1314 0.4884 0.0240 0.160 Uiso 1 1 calc R . . C29 C 0.0530(4) 0.2374(9) 0.2366(6) 0.046(2) Uani 1 1 d . . . C30 C 0.0612(4) 0.1110(8) 0.2066(5) 0.043(2) Uani 1 1 d . . . C31 C 0.0249(5) 0.0630(11) 0.1518(6) 0.063(3) Uani 1 1 d . . . H31A H -0.0029 0.1111 0.1316 0.076 Uiso 1 1 calc R . . C32 C 0.0303(6) -0.0549(13) 0.1283(8) 0.084(4) Uani 1 1 d . . . H32A H 0.0058 -0.0871 0.0928 0.101 Uiso 1 1 calc R . . C33 C 0.0718(6) -0.1251(12) 0.1571(8) 0.079(4) Uani 1 1 d . . . H33A H 0.0758 -0.2045 0.1404 0.095 Uiso 1 1 calc R . . C34 C 0.1077(5) -0.0787(11) 0.2104(7) 0.066(3) Uani 1 1 d . . . H34A H 0.1361 -0.1264 0.2294 0.079 Uiso 1 1 calc R . . C35 C 0.1017(4) 0.0362(9) 0.2352(6) 0.054(3) Uani 1 1 d . . . H35A H 0.1254 0.0658 0.2725 0.065 Uiso 1 1 calc R . . C36 C -0.0251(5) 0.0450(10) 0.3349(8) 0.093(4) Uani 1 1 d . . . H36A H -0.0525 0.0897 0.3075 0.139 Uiso 1 1 calc R . . H36B H -0.0425 -0.0059 0.3723 0.139 Uiso 1 1 calc R . . H36C H -0.0046 -0.0040 0.2996 0.139 Uiso 1 1 calc R . . C37 C -0.0182(5) 0.2457(12) 0.4488(7) 0.088(4) Uani 1 1 d . . . H37A H 0.0056 0.3018 0.4744 0.132 Uiso 1 1 calc R . . H37B H -0.0361 0.1955 0.4862 0.132 Uiso 1 1 calc R . . H37C H -0.0453 0.2894 0.4201 0.132 Uiso 1 1 calc R . . C38 C 0.0740(6) 0.0651(14) 0.4375(7) 0.104(5) Uani 1 1 d . . . H38A H 0.0984 0.1201 0.4629 0.156 Uiso 1 1 calc R . . H38B H 0.0945 0.0154 0.4025 0.156 Uiso 1 1 calc R . . H38C H 0.0562 0.0148 0.4749 0.156 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 S3 0.0480(16) 0.0687(19) 0.0668(18) -0.0223(15) 0.0045(13) -0.0020(14) Ge1 0.0515(6) 0.0453(6) 0.0465(5) -0.0080(6) 0.0046(6) 0.0078(5) Ge2 0.0537(7) 0.0563(7) 0.0534(6) -0.0095(6) 0.0058(6) 0.0002(6) Si1 0.0682(19) 0.0428(15) 0.0527(17) -0.0020(15) -0.0132(16) -0.0015(12) Si2 0.064(2) 0.0440(18) 0.069(2) 0.0041(15) 0.0095(16) -0.0027(15) Si3 0.055(2) 0.081(2) 0.0527(19) 0.0169(17) 0.0025(15) 0.0073(17) Si4 0.061(2) 0.066(2) 0.0506(18) 0.0114(15) -0.0012(15) -0.0029(16) S1 0.083(2) 0.0573(17) 0.077(3) -0.0059(15) 0.0149(17) 0.0246(15) S2 0.093(3) 0.094(3) 0.075(2) -0.029(2) 0.0099(19) -0.014(2) N1 0.039(4) 0.030(4) 0.052(5) -0.014(4) 0.012(4) -0.003(4) N2 0.057(5) 0.033(5) 0.048(5) -0.004(4) -0.001(4) 0.004(4) N3 0.067(6) 0.044(5) 0.071(7) -0.013(5) 0.023(5) -0.004(4) N4 0.048(4) 0.066(5) 0.037(5) -0.005(4) 0.004(4) -0.001(4) C1 0.060(7) 0.060(7) 0.046(6) -0.014(6) 0.013(6) -0.009(6) C2 0.084(9) 0.074(9) 0.045(7) -0.012(6) 0.014(7) -0.026(7) C3 0.073(8) 0.090(10) 0.036(7) -0.005(6) -0.010(6) -0.001(7) C4 0.059(7) 0.064(7) 0.047(7) 0.002(6) -0.009(6) 0.002(6) C5 0.046(6) 0.037(6) 0.041(6) -0.006(4) -0.009(5) 0.000(5) C6 0.038(5) 0.035(5) 0.037(5) -0.005(5) -0.007(5) 0.000(4) C7 0.103(10) 0.086(10) 0.091(10) 0.015(8) -0.006(9) -0.024(9) C8 0.081(8) 0.042(7) 0.077(9) -0.008(6) -0.022(7) -0.010(6) C9 0.094(9) 0.051(7) 0.093(11) -0.002(6) -0.040(8) 0.017(6) C10 0.032(5) 0.045(6) 0.038(6) -0.007(4) 0.004(4) 0.007(4) C11 0.040(6) 0.039(6) 0.041(6) -0.007(5) -0.004(5) 0.012(5) C12 0.051(7) 0.058(7) 0.047(7) -0.013(5) 0.010(5) 0.003(5) C13 0.083(9) 0.059(7) 0.048(7) 0.000(6) 0.015(6) 0.007(7) C14 0.085(9) 0.059(7) 0.048(7) -0.011(5) 0.025(7) -0.008(6) C15 0.057(8) 0.075(9) 0.079(10) -0.015(7) 0.013(7) 0.020(6) C16 0.050(6) 0.055(7) 0.056(7) -0.019(5) 0.005(5) 0.004(5) C17 0.078(8) 0.064(8) 0.086(10) -0.007(6) 0.024(7) -0.029(7) C18 0.092(10) 0.066(8) 0.160(15) -0.044(9) 0.022(9) -0.030(7) C19 0.149(14) 0.073(10) 0.142(14) 0.060(9) -0.003(11) 0.021(10) C20 0.074(8) 0.059(7) 0.080(8) -0.010(7) 0.028(7) 0.015(6) C21 0.094(11) 0.058(9) 0.134(15) -0.010(9) 0.042(10) 0.008(8) C22 0.075(10) 0.061(10) 0.172(18) 0.044(11) 0.031(11) 0.028(7) C23 0.050(7) 0.043(7) 0.115(11) 0.023(7) 0.017(7) 0.008(6) C24 0.039(6) 0.046(7) 0.068(8) 0.006(5) 0.017(5) 0.000(5) C25 0.053(7) 0.044(6) 0.055(7) 0.008(5) -0.001(5) 0.010(5) C26 0.063(8) 0.098(9) 0.076(8) -0.025(7) 0.017(6) 0.009(7) C27 0.069(9) 0.169(15) 0.060(9) 0.002(9) 0.000(7) 0.020(9) C28 0.106(11) 0.118(12) 0.097(11) 0.046(9) 0.029(9) -0.001(9) C29 0.041(6) 0.053(7) 0.046(7) 0.004(5) -0.003(5) 0.004(5) C30 0.049(6) 0.028(5) 0.051(6) -0.005(4) 0.005(5) 0.001(5) C31 0.052(7) 0.066(8) 0.072(8) -0.013(6) -0.013(6) 0.002(6) C32 0.083(10) 0.074(10) 0.095(10) -0.033(8) 0.022(8) -0.013(8) C33 0.095(11) 0.056(8) 0.086(10) -0.014(7) 0.031(8) -0.017(8) C34 0.061(8) 0.063(8) 0.073(8) 0.009(6) 0.025(7) 0.013(6) C35 0.046(6) 0.049(7) 0.066(7) 0.009(6) 0.001(5) 0.018(5) C36 0.117(10) 0.080(9) 0.081(11) 0.007(7) 0.019(8) -0.043(8) C37 0.067(9) 0.120(12) 0.076(9) 0.028(8) 0.013(7) 0.017(8) C38 0.122(12) 0.108(11) 0.082(11) 0.038(8) 0.008(9) 0.045(10) _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 S3 Ge1 2.222(3) . ? S3 Ge2 2.226(3) . ? Ge1 N2 1.842(8) . ? Ge1 N1 1.947(8) . ? Ge1 S1 2.070(3) . ? Ge2 N4 1.846(7) . ? Ge2 N3 1.963(9) . ? Ge2 S2 2.062(4) . ? Si1 C9 1.841(10) . ? Si1 C8 1.843(11) . ? Si1 C7 1.858(13) . ? Si1 C6 1.887(8) . ? Si2 N2 1.787(8) . ? Si2 C17 1.814(11) . ? Si2 C19 1.829(13) . ? Si2 C18 1.865(13) . ? Si3 C26 1.846(11) . ? Si3 C27 1.876(12) . ? Si3 C25 1.880(11) . ? Si3 C28 1.901(14) . ? Si4 N4 1.761(8) . ? Si4 C37 1.823(12) . ? Si4 C38 1.842(12) . ? Si4 C36 1.850(11) . ? N1 C1 1.346(12) . ? N1 C5 1.380(11) . ? N2 C10 1.396(10) . ? N3 C24 1.354(13) . ? N3 C20 1.359(12) . ? N4 C29 1.420(12) . ? C1 C2 1.372(15) . ? C2 C3 1.357(15) . ? C3 C4 1.375(14) . ? C4 C5 1.366(13) . ? C5 C6 1.476(13) . ? C6 C10 1.370(12) . ? C10 C11 1.498(12) . ? C11 C12 1.355(13) . ? C11 C16 1.400(13) . ? C12 C13 1.395(13) . ? C13 C14 1.360(14) . ? C14 C15 1.390(14) . ? C15 C16 1.377(14) . ? C20 C21 1.340(18) . ? C21 C22 1.40(2) . ? C22 C23 1.302(18) . ? C23 C24 1.435(15) . ? C24 C25 1.481(13) . ? C25 C29 1.381(13) . ? C29 C30 1.507(12) . ? C30 C35 1.380(12) . ? C30 C31 1.405(13) . ? C31 C32 1.374(16) . ? C32 C33 1.371(18) . ? C33 C34 1.375(17) . ? C34 C35 1.351(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ge1 S3 Ge2 101.41(11) . . ? N2 Ge1 N1 91.8(3) . . ? N2 Ge1 S1 122.0(2) . . ? N1 Ge1 S1 113.0(2) . . ? N2 Ge1 S3 101.4(2) . . ? N1 Ge1 S3 101.9(2) . . ? S1 Ge1 S3 121.32(12) . . ? N4 Ge2 N3 91.1(4) . . ? N4 Ge2 S2 121.5(3) . . ? N3 Ge2 S2 113.8(3) . . ? N4 Ge2 S3 100.8(2) . . ? N3 Ge2 S3 102.7(2) . . ? S2 Ge2 S3 121.42(14) . . ? C9 Si1 C8 109.7(5) . . ? C9 Si1 C7 108.3(6) . . ? C8 Si1 C7 106.1(5) . . ? C9 Si1 C6 113.6(4) . . ? C8 Si1 C6 111.8(5) . . ? C7 Si1 C6 107.1(5) . . ? N2 Si2 C17 112.9(5) . . ? N2 Si2 C19 109.4(6) . . ? C17 Si2 C19 111.1(7) . . ? N2 Si2 C18 106.7(5) . . ? C17 Si2 C18 106.4(6) . . ? C19 Si2 C18 110.2(7) . . ? C26 Si3 C27 107.5(6) . . ? C26 Si3 C25 112.6(5) . . ? C27 Si3 C25 116.5(5) . . ? C26 Si3 C28 105.8(6) . . ? C27 Si3 C28 107.3(7) . . ? C25 Si3 C28 106.4(6) . . ? N4 Si4 C37 106.6(5) . . ? N4 Si4 C38 110.6(5) . . ? C37 Si4 C38 110.6(6) . . ? N4 Si4 C36 111.1(5) . . ? C37 Si4 C36 108.6(6) . . ? C38 Si4 C36 109.3(7) . . ? C1 N1 C5 120.2(9) . . ? C1 N1 Ge1 121.1(7) . . ? C5 N1 Ge1 118.5(6) . . ? C10 N2 Si2 125.6(6) . . ? C10 N2 Ge1 112.9(6) . . ? Si2 N2 Ge1 121.1(4) . . ? C24 N3 C20 121.1(10) . . ? C24 N3 Ge2 118.3(7) . . ? C20 N3 Ge2 120.4(8) . . ? C29 N4 Si4 126.1(6) . . ? C29 N4 Ge2 110.9(6) . . ? Si4 N4 Ge2 122.9(5) . . ? N1 C1 C2 121.0(10) . . ? C3 C2 C1 119.6(10) . . ? C2 C3 C4 119.4(11) . . ? C5 C4 C3 121.2(11) . . ? C4 C5 N1 118.6(9) . . ? C4 C5 C6 121.1(9) . . ? N1 C5 C6 120.3(8) . . ? C10 C6 C5 119.0(7) . . ? C10 C6 Si1 124.9(7) . . ? C5 C6 Si1 115.1(7) . . ? C6 C10 N2 124.4(8) . . ? C6 C10 C11 120.9(8) . . ? N2 C10 C11 114.7(8) . . ? C12 C11 C16 119.4(9) . . ? C12 C11 C10 120.7(8) . . ? C16 C11 C10 119.9(8) . . ? C11 C12 C13 120.7(10) . . ? C14 C13 C12 120.2(11) . . ? C13 C14 C15 119.8(10) . . ? C16 C15 C14 120.0(10) . . ? C15 C16 C11 119.9(10) . . ? C21 C20 N3 121.0(13) . . ? C20 C21 C22 119.1(13) . . ? C23 C22 C21 120.8(14) . . ? C22 C23 C24 120.6(15) . . ? N3 C24 C23 117.4(10) . . ? N3 C24 C25 121.3(9) . . ? C23 C24 C25 121.3(11) . . ? C29 C25 C24 117.0(9) . . ? C29 C25 Si3 125.7(7) . . ? C24 C25 Si3 115.8(7) . . ? C25 C29 N4 125.4(9) . . ? C25 C29 C30 118.8(9) . . ? N4 C29 C30 115.7(8) . . ? C35 C30 C31 118.0(9) . . ? C35 C30 C29 121.7(9) . . ? C31 C30 C29 120.1(9) . . ? C32 C31 C30 120.1(11) . . ? C33 C32 C31 119.9(13) . . ? C32 C33 C34 120.4(12) . . ? C35 C34 C33 119.9(12) . . ? C34 C35 C30 121.7(11) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.602 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.106