# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Hiromi Tobita' _publ_contact_author_email tobita@m.tains.tohoku.ac.jp _publ_section_title ; Reactions of a Hydrido(hydrogermylene)tungsten Complex with Some Heterocumulenes: Hydrogermylation and Thermal Rearrangement ; loop_ _publ_author_name 'Hisako Hashimoto' 'Tetsuya Fukuda' 'Hiromi Tobita' # Attachment '- combinedCIFsRev.cif' data_PhNCO _database_code_depnum_ccdc_archive 'CCDC 767386' #TrackingRef '- combinedCIFsRev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H49 Ge N O3 Si3 W, C6 D6' _chemical_formula_sum 'C35 H49 D6 Ge N O3 Si3 W' _chemical_formula_weight 884.53 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' D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.8560(3) _cell_length_b 13.7380(5) _cell_length_c 15.9500(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.9596(18) _cell_angle_gamma 90.00 _cell_volume 1911.29(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8545 _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour 'reddish orange' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 3.920 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4658 _exptl_absorpt_correction_T_max 0.6098 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18067 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8545 _reflns_number_gt 8291 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material 'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' _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^)+(0.0525P)^2^+1.2974P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(7) _refine_ls_number_reflns 8545 _refine_ls_number_parameters 411 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _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 W1 W 0.163107(16) 0.009533(15) 0.171663(9) 0.01724(5) Uani 1 1 d . . . Ge1 Ge 0.27064(6) -0.08978(3) 0.30833(3) 0.01736(10) Uani 1 1 d . . . O1 O 0.3342(4) 0.0231(3) 0.3793(2) 0.0256(8) Uani 1 1 d . . . C1 C 0.2683(6) 0.1022(4) 0.3538(3) 0.0212(9) Uani 1 1 d . . . H2 H 0.2809 0.1553 0.3926 0.025 Uiso 1 1 calc R . . N1 N 0.1846(5) 0.1175(3) 0.2792(3) 0.0191(8) Uani 1 1 d . . . C2 C -0.0450(6) 0.0586(4) 0.1410(3) 0.0295(11) Uani 1 1 d . . . O2 O -0.1698(5) 0.0832(4) 0.1122(3) 0.0487(13) Uani 1 1 d . . . C3 C 0.0297(7) -0.1051(4) 0.1467(3) 0.0303(11) Uani 1 1 d . . . O3 O -0.0523(6) -0.1681(4) 0.1223(3) 0.0451(12) Uani 1 1 d . . . C4 C 0.4094(6) -0.0155(4) 0.1297(3) 0.0254(11) Uani 1 1 d . . . C5 C 0.3872(6) 0.0865(4) 0.1357(3) 0.0222(10) Uani 1 1 d . . . C6 C 0.2526(6) 0.1142(4) 0.0780(3) 0.0230(10) Uani 1 1 d . . . C7 C 0.1920(6) 0.0271(4) 0.0329(3) 0.0271(12) Uani 1 1 d . . . C8 C 0.2869(7) -0.0533(4) 0.0653(4) 0.0295(12) Uani 1 1 d . . . C9 C 0.5500(7) -0.0706(5) 0.1705(4) 0.0400(14) Uani 1 1 d . . . H3 H 0.6249 -0.0714 0.1319 0.060 Uiso 1 1 calc R . . H4 H 0.5216 -0.1376 0.1822 0.060 Uiso 1 1 calc R . . H5 H 0.5952 -0.0388 0.2239 0.060 Uiso 1 1 calc R . . C10 C 0.4991(6) 0.1544(4) 0.1887(4) 0.0321(12) Uani 1 1 d . . . H6 H 0.5092 0.1364 0.2489 0.048 Uiso 1 1 calc R . . H7 H 0.4614 0.2214 0.1808 0.048 Uiso 1 1 calc R . . H8 H 0.5992 0.1494 0.1708 0.048 Uiso 1 1 calc R . . C11 C 0.1963(8) 0.2151(4) 0.0552(4) 0.0336(12) Uani 1 1 d . . . H9 H 0.2039 0.2543 0.1071 0.050 Uiso 1 1 calc R . . H10 H 0.0892 0.2124 0.0266 0.050 Uiso 1 1 calc R . . H11 H 0.2591 0.2446 0.0170 0.050 Uiso 1 1 calc R . . C12 C 0.0642(8) 0.0236(7) -0.0419(4) 0.0448(18) Uani 1 1 d . . . H12 H 0.1055 0.0339 -0.0944 0.067 Uiso 1 1 calc R . . H13 H -0.0106 0.0747 -0.0363 0.067 Uiso 1 1 calc R . . H14 H 0.0139 -0.0401 -0.0441 0.067 Uiso 1 1 calc R . . C13 C 0.2797(9) -0.1542(5) 0.0304(5) 0.0461(16) Uani 1 1 d . . . H15 H 0.1725 -0.1724 0.0108 0.069 Uiso 1 1 calc R . . H16 H 0.3264 -0.1994 0.0750 0.069 Uiso 1 1 calc R . . H17 H 0.3356 -0.1570 -0.0175 0.069 Uiso 1 1 calc R . . C14 C 0.1212(6) 0.2138(4) 0.2688(3) 0.0206(9) Uani 1 1 d . . . C15 C -0.0372(6) 0.2270(4) 0.2578(3) 0.0282(11) Uani 1 1 d . . . H18 H -0.1030 0.1722 0.2571 0.034 Uiso 1 1 calc R . . C16 C -0.0986(7) 0.3202(5) 0.2479(4) 0.0371(13) Uani 1 1 d . . . H19 H -0.2066 0.3288 0.2387 0.045 Uiso 1 1 calc R . . C17 C -0.0031(9) 0.4006(4) 0.2513(4) 0.0412(15) Uani 1 1 d . . . H20 H -0.0454 0.4642 0.2441 0.049 Uiso 1 1 calc R . . C18 C 0.1528(9) 0.3877(4) 0.2651(4) 0.0382(14) Uani 1 1 d . . . H21 H 0.2183 0.4428 0.2685 0.046 Uiso 1 1 calc R . . C19 C 0.2163(7) 0.2948(4) 0.2742(4) 0.0271(11) Uani 1 1 d . . . H22 H 0.3245 0.2868 0.2841 0.033 Uiso 1 1 calc R . . C20 C 0.1997(5) -0.1769(3) 0.3957(3) 0.0174(8) Uani 1 1 d . . . Si1 Si -0.01250(15) -0.16119(11) 0.39743(9) 0.0219(3) Uani 1 1 d . . . Si2 Si 0.24912(18) -0.30407(9) 0.36273(9) 0.0241(3) Uani 1 1 d . . . Si3 Si 0.31627(15) -0.14601(10) 0.50473(9) 0.0214(3) Uani 1 1 d . . . C21 C -0.1398(6) -0.2275(5) 0.3101(4) 0.0350(13) Uani 1 1 d . . . H23 H -0.1180 -0.2974 0.3149 0.052 Uiso 1 1 calc R . . H24 H -0.1209 -0.2038 0.2549 0.052 Uiso 1 1 calc R . . H25 H -0.2473 -0.2159 0.3147 0.052 Uiso 1 1 calc R . . C22 C -0.0724(6) -0.0304(4) 0.3862(4) 0.0304(11) Uani 1 1 d . . . H26 H -0.1804 -0.0246 0.3922 0.046 Uiso 1 1 calc R . . H27 H -0.0593 -0.0064 0.3300 0.046 Uiso 1 1 calc R . . H28 H -0.0089 0.0083 0.4305 0.046 Uiso 1 1 calc R . . C23 C -0.0689(6) -0.2103(5) 0.4974(4) 0.0342(13) Uani 1 1 d . . . H29 H -0.1809 -0.2095 0.4918 0.051 Uiso 1 1 calc R . . H30 H -0.0238 -0.1697 0.5458 0.051 Uiso 1 1 calc R . . H31 H -0.0316 -0.2772 0.5067 0.051 Uiso 1 1 calc R . . C24 C 0.2010(8) -0.3194(4) 0.2441(4) 0.0354(13) Uani 1 1 d . . . H32 H 0.2345 -0.3838 0.2283 0.053 Uiso 1 1 calc R . . H33 H 0.2534 -0.2691 0.2163 0.053 Uiso 1 1 calc R . . H34 H 0.0900 -0.3133 0.2257 0.053 Uiso 1 1 calc R . . C25 C 0.4578(7) -0.3360(4) 0.3912(4) 0.0380(14) Uani 1 1 d . . . H35 H 0.4872 -0.3391 0.4533 0.057 Uiso 1 1 calc R . . H36 H 0.5192 -0.2862 0.3687 0.057 Uiso 1 1 calc R . . H37 H 0.4759 -0.3994 0.3665 0.057 Uiso 1 1 calc R . . C26 C 0.1455(8) -0.4013(4) 0.4127(4) 0.0368(13) Uani 1 1 d . . . H38 H 0.0347 -0.3932 0.3946 0.055 Uiso 1 1 calc R . . H39 H 0.1711 -0.3960 0.4748 0.055 Uiso 1 1 calc R . . H40 H 0.1767 -0.4654 0.3948 0.055 Uiso 1 1 calc R . . C27 C 0.5227(6) -0.1163(5) 0.5039(4) 0.0332(12) Uani 1 1 d . . . H41 H 0.5773 -0.1098 0.5625 0.050 Uiso 1 1 calc R . . H42 H 0.5293 -0.0549 0.4734 0.050 Uiso 1 1 calc R . . H43 H 0.5693 -0.1686 0.4752 0.050 Uiso 1 1 calc R . . C28 C 0.3212(7) -0.2501(4) 0.5822(4) 0.0311(12) Uani 1 1 d . . . H44 H 0.3843 -0.3029 0.5656 0.047 Uiso 1 1 calc R . . H45 H 0.2167 -0.2739 0.5818 0.047 Uiso 1 1 calc R . . H46 H 0.3651 -0.2276 0.6396 0.047 Uiso 1 1 calc R . . C29 C 0.2384(7) -0.0394(4) 0.5579(4) 0.0301(11) Uani 1 1 d . . . H47 H 0.3016 -0.0285 0.6139 0.045 Uiso 1 1 calc R . . H48 H 0.1327 -0.0531 0.5648 0.045 Uiso 1 1 calc R . . H49 H 0.2404 0.0189 0.5227 0.045 Uiso 1 1 calc R . . C30 C 0.4311(9) 0.4556(5) 0.1298(5) 0.0471(16) Uani 1 1 d . . . H50 H 0.3736 0.3969 0.1271 0.056 Uiso 1 1 calc R . . C31 C 0.4083(8) 0.5202(8) 0.0615(4) 0.053(2) Uani 1 1 d . . . H51 H 0.3352 0.5063 0.0120 0.063 Uiso 1 1 calc R . . C32 C 0.4946(10) 0.6056(6) 0.0670(5) 0.059(2) Uani 1 1 d . . . H52 H 0.4792 0.6508 0.0212 0.071 Uiso 1 1 calc R . . C33 C 0.6021(10) 0.6248(5) 0.1384(5) 0.0518(19) Uani 1 1 d . . . H53 H 0.6624 0.6823 0.1418 0.062 Uiso 1 1 calc R . . C34 C 0.6208(8) 0.5596(5) 0.2046(4) 0.0404(14) Uani 1 1 d . . . H54 H 0.6940 0.5726 0.2543 0.049 Uiso 1 1 calc R . . C35 C 0.5358(8) 0.4767(5) 0.2001(5) 0.0411(14) Uani 1 1 d . . . H55 H 0.5499 0.4329 0.2468 0.049 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 W1 0.01881(8) 0.01929(8) 0.01399(8) -0.00193(8) 0.00390(5) -0.00150(8) Ge1 0.0182(2) 0.0170(2) 0.0177(2) 0.00058(19) 0.00514(18) -0.00063(19) O1 0.0290(16) 0.022(2) 0.0230(15) 0.0017(15) -0.0041(12) -0.0041(15) C1 0.025(2) 0.019(2) 0.018(2) -0.0021(19) 0.0003(18) -0.0042(19) N1 0.0198(19) 0.0196(19) 0.0182(19) -0.0032(15) 0.0043(15) 0.0013(16) C2 0.027(3) 0.042(3) 0.019(2) -0.009(2) 0.001(2) 0.000(2) O2 0.023(2) 0.083(4) 0.037(2) -0.017(2) -0.0055(18) 0.009(2) C3 0.035(3) 0.038(3) 0.018(2) -0.004(2) 0.006(2) -0.006(2) O3 0.056(3) 0.048(3) 0.029(2) -0.0081(19) 0.003(2) -0.030(2) C4 0.026(2) 0.025(3) 0.027(2) 0.0014(18) 0.012(2) 0.0045(19) C5 0.021(2) 0.025(3) 0.021(2) 0.0070(19) 0.0059(18) -0.0004(19) C6 0.032(3) 0.023(2) 0.015(2) 0.0007(19) 0.0089(19) 0.001(2) C7 0.035(2) 0.034(3) 0.015(2) -0.0001(19) 0.0104(18) -0.003(2) C8 0.042(3) 0.029(3) 0.024(3) -0.005(2) 0.023(2) 0.001(2) C9 0.032(3) 0.048(4) 0.045(3) 0.017(3) 0.020(3) 0.016(3) C10 0.026(3) 0.037(3) 0.034(3) -0.006(2) 0.007(2) -0.005(2) C11 0.043(3) 0.031(3) 0.028(3) 0.010(2) 0.010(2) 0.007(3) C12 0.047(3) 0.065(5) 0.021(2) -0.004(3) 0.003(2) -0.010(4) C13 0.066(5) 0.036(3) 0.043(4) -0.016(3) 0.026(3) -0.002(3) C14 0.027(2) 0.019(2) 0.017(2) -0.0011(17) 0.0060(18) 0.0032(19) C15 0.026(2) 0.033(3) 0.025(3) 0.000(2) 0.006(2) 0.009(2) C16 0.037(3) 0.043(3) 0.030(3) 0.000(3) 0.005(2) 0.016(3) C17 0.071(4) 0.027(3) 0.028(3) 0.006(2) 0.015(3) 0.022(3) C18 0.062(4) 0.019(2) 0.038(3) -0.003(2) 0.020(3) 0.001(3) C19 0.032(3) 0.023(2) 0.029(3) -0.004(2) 0.013(2) -0.002(2) C20 0.0163(19) 0.019(2) 0.019(2) -0.0004(17) 0.0078(16) 0.0010(17) Si1 0.0161(6) 0.0301(7) 0.0201(6) 0.0023(5) 0.0047(5) 0.0002(5) Si2 0.0325(7) 0.0172(6) 0.0258(7) 0.0010(5) 0.0143(6) 0.0015(5) Si3 0.0176(6) 0.0272(6) 0.0188(6) 0.0018(5) 0.0019(5) 0.0029(5) C21 0.023(2) 0.048(3) 0.033(3) -0.003(3) 0.002(2) -0.014(2) C22 0.023(2) 0.035(3) 0.033(3) 0.003(2) 0.007(2) 0.008(2) C23 0.022(2) 0.051(4) 0.032(3) 0.010(3) 0.010(2) 0.003(2) C24 0.059(4) 0.023(3) 0.028(3) -0.006(2) 0.017(3) -0.001(3) C25 0.039(3) 0.031(3) 0.050(4) 0.006(3) 0.025(3) 0.019(2) C26 0.052(4) 0.022(2) 0.040(3) 0.006(2) 0.016(3) -0.004(2) C27 0.020(2) 0.044(3) 0.033(3) 0.006(2) -0.003(2) 0.001(2) C28 0.029(3) 0.035(3) 0.030(3) 0.010(2) 0.006(2) 0.001(2) C29 0.031(3) 0.035(3) 0.023(3) -0.009(2) 0.001(2) 0.001(2) C30 0.048(4) 0.046(4) 0.045(4) -0.007(3) 0.001(3) -0.005(3) C31 0.044(3) 0.084(6) 0.028(3) -0.006(4) 0.001(2) 0.022(5) C32 0.082(6) 0.059(4) 0.046(4) 0.023(4) 0.039(4) 0.043(5) C33 0.075(5) 0.037(3) 0.054(4) -0.006(3) 0.040(4) -0.003(3) C34 0.040(3) 0.044(3) 0.038(3) -0.011(3) 0.006(3) 0.002(3) C35 0.044(3) 0.039(3) 0.039(3) 0.003(2) 0.006(3) 0.009(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 W1 C2 1.944(6) . ? W1 C3 1.968(6) . ? W1 N1 2.250(4) . ? W1 C7 2.284(5) . ? W1 C6 2.311(5) . ? W1 C8 2.339(5) . ? W1 C5 2.404(5) . ? W1 C4 2.414(5) . ? W1 Ge1 2.6080(5) . ? Ge1 O1 1.945(4) . ? Ge1 C20 2.017(5) . ? O1 C1 1.267(7) . ? C1 N1 1.306(6) . ? C1 H2 0.9500 . ? N1 C14 1.436(6) . ? C2 O2 1.171(7) . ? C3 O3 1.153(7) . ? C4 C5 1.420(8) . ? C4 C8 1.456(8) . ? C4 C9 1.505(8) . ? C5 C6 1.426(7) . ? C5 C10 1.509(7) . ? C6 C7 1.450(7) . ? C6 C11 1.497(8) . ? C7 C8 1.429(8) . ? C7 C12 1.498(7) . ? C8 C13 1.491(8) . ? C9 H3 0.9800 . ? C9 H4 0.9800 . ? C9 H5 0.9800 . ? C10 H6 0.9800 . ? C10 H7 0.9800 . ? C10 H8 0.9800 . ? C11 H9 0.9800 . ? C11 H10 0.9800 . ? C11 H11 0.9800 . ? C12 H12 0.9800 . ? C12 H13 0.9800 . ? C12 H14 0.9800 . ? C13 H15 0.9800 . ? C13 H16 0.9800 . ? C13 H17 0.9800 . ? C14 C19 1.389(7) . ? C14 C15 1.396(7) . ? C15 C16 1.389(8) . ? C15 H18 0.9500 . ? C16 C17 1.387(10) . ? C16 H19 0.9500 . ? C17 C18 1.372(10) . ? C17 H20 0.9500 . ? C18 C19 1.391(8) . ? C18 H21 0.9500 . ? C19 H22 0.9500 . ? C20 Si1 1.897(5) . ? C20 Si2 1.898(5) . ? C20 Si3 1.910(5) . ? Si1 C21 1.870(6) . ? Si1 C22 1.874(6) . ? Si1 C23 1.877(6) . ? Si2 C26 1.874(6) . ? Si2 C25 1.877(6) . ? Si2 C24 1.878(6) . ? Si3 C27 1.875(6) . ? Si3 C29 1.882(6) . ? Si3 C28 1.886(6) . ? C21 H23 0.9800 . ? C21 H24 0.9800 . ? C21 H25 0.9800 . ? C22 H26 0.9800 . ? C22 H27 0.9800 . ? C22 H28 0.9800 . ? C23 H29 0.9800 . ? C23 H30 0.9800 . ? C23 H31 0.9800 . ? C24 H32 0.9800 . ? C24 H33 0.9800 . ? C24 H34 0.9800 . ? C25 H35 0.9800 . ? C25 H36 0.9800 . ? C25 H37 0.9800 . ? C26 H38 0.9800 . ? C26 H39 0.9800 . ? C26 H40 0.9800 . ? C27 H41 0.9800 . ? C27 H42 0.9800 . ? C27 H43 0.9800 . ? C28 H44 0.9800 . ? C28 H45 0.9800 . ? C28 H46 0.9800 . ? C29 H47 0.9800 . ? C29 H48 0.9800 . ? C29 H49 0.9800 . ? C30 C35 1.357(10) . ? C30 C31 1.392(12) . ? C30 H50 0.9500 . ? C31 C32 1.395(14) . ? C31 H51 0.9500 . ? C32 C33 1.378(12) . ? C32 H52 0.9500 . ? C33 C34 1.372(10) . ? C33 H53 0.9500 . ? C34 C35 1.361(10) . ? C34 H54 0.9500 . ? C35 H55 0.9500 . ? 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 C2 W1 C3 73.5(2) . . ? C2 W1 N1 85.13(19) . . ? C3 W1 N1 130.55(19) . . ? C2 W1 C7 88.8(2) . . ? C3 W1 C7 93.0(2) . . ? N1 W1 C7 131.28(17) . . ? C2 W1 C6 92.2(2) . . ? C3 W1 C6 128.9(2) . . ? N1 W1 C6 95.14(17) . . ? C7 W1 C6 36.78(18) . . ? C2 W1 C8 119.2(2) . . ? C3 W1 C8 84.2(2) . . ? N1 W1 C8 143.87(19) . . ? C7 W1 C8 36.0(2) . . ? C6 W1 C8 60.3(2) . . ? C2 W1 C5 125.0(2) . . ? C3 W1 C5 142.7(2) . . ? N1 W1 C5 85.84(16) . . ? C7 W1 C5 59.12(18) . . ? C6 W1 C5 35.14(17) . . ? C8 W1 C5 58.6(2) . . ? C2 W1 C4 147.4(2) . . ? C3 W1 C4 111.7(2) . . ? N1 W1 C4 110.10(17) . . ? C7 W1 C4 59.24(19) . . ? C6 W1 C4 58.80(18) . . ? C8 W1 C4 35.6(2) . . ? C5 W1 C4 34.29(19) . . ? C2 W1 Ge1 125.82(17) . . ? C3 W1 Ge1 82.52(16) . . ? N1 W1 Ge1 74.77(11) . . ? C7 W1 Ge1 141.18(14) . . ? C6 W1 Ge1 138.55(13) . . ? C8 W1 Ge1 105.32(15) . . ? C5 W1 Ge1 103.43(11) . . ? C4 W1 Ge1 86.57(13) . . ? O1 Ge1 C20 99.44(17) . . ? O1 Ge1 W1 95.54(11) . . ? C20 Ge1 W1 140.82(13) . . ? C1 O1 Ge1 115.2(3) . . ? O1 C1 N1 126.0(5) . . ? O1 C1 H2 117.0 . . ? N1 C1 H2 117.0 . . ? C1 N1 C14 113.7(4) . . ? C1 N1 W1 123.3(3) . . ? C14 N1 W1 122.7(3) . . ? O2 C2 W1 171.3(5) . . ? O3 C3 W1 171.8(5) . . ? C5 C4 C8 107.7(5) . . ? C5 C4 C9 125.5(5) . . ? C8 C4 C9 125.9(5) . . ? C5 C4 W1 72.5(3) . . ? C8 C4 W1 69.3(3) . . ? C9 C4 W1 132.2(4) . . ? C4 C5 C6 109.3(5) . . ? C4 C5 C10 124.2(5) . . ? C6 C5 C10 126.2(5) . . ? C4 C5 W1 73.3(3) . . ? C6 C5 W1 68.8(3) . . ? C10 C5 W1 128.9(4) . . ? C5 C6 C7 107.2(5) . . ? C5 C6 C11 127.6(5) . . ? C7 C6 C11 124.4(5) . . ? C5 C6 W1 76.0(3) . . ? C7 C6 W1 70.6(3) . . ? C11 C6 W1 126.6(4) . . ? C8 C7 C6 108.4(5) . . ? C8 C7 C12 125.4(6) . . ? C6 C7 C12 125.9(6) . . ? C8 C7 W1 74.1(3) . . ? C6 C7 W1 72.6(3) . . ? C12 C7 W1 125.0(4) . . ? C7 C8 C4 107.4(5) . . ? C7 C8 C13 126.9(6) . . ? C4 C8 C13 125.0(6) . . ? C7 C8 W1 69.9(3) . . ? C4 C8 W1 75.0(3) . . ? C13 C8 W1 128.2(4) . . ? C4 C9 H3 109.5 . . ? C4 C9 H4 109.5 . . ? H3 C9 H4 109.5 . . ? C4 C9 H5 109.5 . . ? H3 C9 H5 109.5 . . ? H4 C9 H5 109.5 . . ? C5 C10 H6 109.5 . . ? C5 C10 H7 109.5 . . ? H6 C10 H7 109.5 . . ? C5 C10 H8 109.5 . . ? H6 C10 H8 109.5 . . ? H7 C10 H8 109.5 . . ? C6 C11 H9 109.5 . . ? C6 C11 H10 109.5 . . ? H9 C11 H10 109.5 . . ? C6 C11 H11 109.5 . . ? H9 C11 H11 109.5 . . ? H10 C11 H11 109.5 . . ? C7 C12 H12 109.5 . . ? C7 C12 H13 109.5 . . ? H12 C12 H13 109.5 . . ? C7 C12 H14 109.5 . . ? H12 C12 H14 109.5 . . ? H13 C12 H14 109.5 . . ? C8 C13 H15 109.5 . . ? C8 C13 H16 109.5 . . ? H15 C13 H16 109.5 . . ? C8 C13 H17 109.5 . . ? H15 C13 H17 109.5 . . ? H16 C13 H17 109.5 . . ? C19 C14 C15 119.3(5) . . ? C19 C14 N1 120.7(5) . . ? C15 C14 N1 119.9(5) . . ? C16 C15 C14 119.9(6) . . ? C16 C15 H18 120.1 . . ? C14 C15 H18 120.1 . . ? C17 C16 C15 120.4(6) . . ? C17 C16 H19 119.8 . . ? C15 C16 H19 119.8 . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H20 120.2 . . ? C16 C17 H20 120.2 . . ? C17 C18 C19 120.8(6) . . ? C17 C18 H21 119.6 . . ? C19 C18 H21 119.6 . . ? C14 C19 C18 119.9(5) . . ? C14 C19 H22 120.1 . . ? C18 C19 H22 120.1 . . ? Si1 C20 Si2 112.7(2) . . ? Si1 C20 Si3 110.0(2) . . ? Si2 C20 Si3 110.0(2) . . ? Si1 C20 Ge1 111.7(2) . . ? Si2 C20 Ge1 103.9(2) . . ? Si3 C20 Ge1 108.3(2) . . ? C21 Si1 C22 105.8(3) . . ? C21 Si1 C23 104.1(3) . . ? C22 Si1 C23 108.2(3) . . ? C21 Si1 C20 113.9(3) . . ? C22 Si1 C20 111.9(2) . . ? C23 Si1 C20 112.4(2) . . ? C26 Si2 C25 105.3(3) . . ? C26 Si2 C24 107.8(3) . . ? C25 Si2 C24 105.1(3) . . ? C26 Si2 C20 112.6(2) . . ? C25 Si2 C20 114.4(3) . . ? C24 Si2 C20 111.1(2) . . ? C27 Si3 C29 105.5(3) . . ? C27 Si3 C28 105.0(3) . . ? C29 Si3 C28 105.3(3) . . ? C27 Si3 C20 114.6(2) . . ? C29 Si3 C20 113.6(2) . . ? C28 Si3 C20 112.1(2) . . ? Si1 C21 H23 109.5 . . ? Si1 C21 H24 109.5 . . ? H23 C21 H24 109.5 . . ? Si1 C21 H25 109.5 . . ? H23 C21 H25 109.5 . . ? H24 C21 H25 109.5 . . ? Si1 C22 H26 109.5 . . ? Si1 C22 H27 109.5 . . ? H26 C22 H27 109.5 . . ? Si1 C22 H28 109.5 . . ? H26 C22 H28 109.5 . . ? H27 C22 H28 109.5 . . ? Si1 C23 H29 109.5 . . ? Si1 C23 H30 109.5 . . ? H29 C23 H30 109.5 . . ? Si1 C23 H31 109.5 . . ? H29 C23 H31 109.5 . . ? H30 C23 H31 109.5 . . ? Si2 C24 H32 109.5 . . ? Si2 C24 H33 109.5 . . ? H32 C24 H33 109.5 . . ? Si2 C24 H34 109.5 . . ? H32 C24 H34 109.5 . . ? H33 C24 H34 109.5 . . ? Si2 C25 H35 109.5 . . ? Si2 C25 H36 109.5 . . ? H35 C25 H36 109.5 . . ? Si2 C25 H37 109.5 . . ? H35 C25 H37 109.5 . . ? H36 C25 H37 109.5 . . ? Si2 C26 H38 109.5 . . ? Si2 C26 H39 109.5 . . ? H38 C26 H39 109.5 . . ? Si2 C26 H40 109.5 . . ? H38 C26 H40 109.5 . . ? H39 C26 H40 109.5 . . ? Si3 C27 H41 109.5 . . ? Si3 C27 H42 109.5 . . ? H41 C27 H42 109.5 . . ? Si3 C27 H43 109.5 . . ? H41 C27 H43 109.5 . . ? H42 C27 H43 109.5 . . ? Si3 C28 H44 109.5 . . ? Si3 C28 H45 109.5 . . ? H44 C28 H45 109.5 . . ? Si3 C28 H46 109.5 . . ? H44 C28 H46 109.5 . . ? H45 C28 H46 109.5 . . ? Si3 C29 H47 109.5 . . ? Si3 C29 H48 109.5 . . ? H47 C29 H48 109.5 . . ? Si3 C29 H49 109.5 . . ? H47 C29 H49 109.5 . . ? H48 C29 H49 109.5 . . ? C35 C30 C31 119.7(7) . . ? C35 C30 H50 120.1 . . ? C31 C30 H50 120.1 . . ? C30 C31 C32 119.0(7) . . ? C30 C31 H51 120.5 . . ? C32 C31 H51 120.5 . . ? C33 C32 C31 120.3(7) . . ? C33 C32 H52 119.8 . . ? C31 C32 H52 119.8 . . ? C34 C33 C32 119.1(7) . . ? C34 C33 H53 120.5 . . ? C32 C33 H53 120.5 . . ? C35 C34 C33 120.8(7) . . ? C35 C34 H54 119.6 . . ? C33 C34 H54 119.6 . . ? C30 C35 C34 121.1(7) . . ? C30 C35 H55 119.5 . . ? C34 C35 H55 119.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.671 _refine_diff_density_min -1.873 _refine_diff_density_rms 0.242 #===END data_PhNCS1 _database_code_depnum_ccdc_archive 'CCDC 767387' #TrackingRef '- combinedCIFsRev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H49 Ge N O2 S Si3 W' _chemical_formula_sum 'C29 H49 Ge N O2 S Si3 W' _chemical_formula_weight 816.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' W W -0.8490 6.8722 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 12.8240(6) _cell_length_b 16.7658(5) _cell_length_c 17.5750(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.9913(9) _cell_angle_gamma 90.00 _cell_volume 3573.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 32360 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 4.242 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3530 _exptl_absorpt_correction_T_max 0.4420 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32360 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8159 _reflns_number_gt 7542 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material 'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' _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^)+(0.0436P)^2^+2.3543P] 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 8159 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.267 _refine_ls_restrained_S_all 1.267 _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 W1 W 0.044012(9) 0.243856(7) 0.032500(7) 0.01350(5) Uani 1 1 d . . . Ge1 Ge -0.06284(3) 0.305513(18) 0.123499(18) 0.01386(7) Uani 1 1 d . . . N1 N 0.0223(2) 0.41226(15) 0.14880(15) 0.0157(5) Uani 1 1 d . . . C1 C 0.0592(3) 0.43857(18) 0.09263(18) 0.0181(6) Uani 1 1 d . . . H1A H 0.0885 0.4911 0.0989 0.022 Uiso 1 1 calc R . . S1 S 0.05969(7) 0.38785(4) 0.00979(4) 0.01749(15) Uani 1 1 d . . . C2 C -0.0762(3) 0.1662(2) -0.0020(2) 0.0228(7) Uani 1 1 d . . . O1 O -0.1377(2) 0.11450(15) -0.02733(17) 0.0325(6) Uani 1 1 d . . . C3 C -0.0104(3) 0.25043(18) -0.0848(2) 0.0231(7) Uani 1 1 d . . . O2 O -0.0368(3) 0.24982(16) -0.15488(17) 0.0375(7) Uani 1 1 d . . . C4 C 0.1875(3) 0.20129(19) 0.15295(18) 0.0190(6) Uani 1 1 d . . . C5 C 0.1470(3) 0.13533(18) 0.10038(19) 0.0197(6) Uani 1 1 d . . . C6 C 0.1704(3) 0.14981(19) 0.02752(19) 0.0189(6) Uani 1 1 d . . . C7 C 0.2233(3) 0.2257(2) 0.03460(19) 0.0182(6) Uani 1 1 d . . . C8 C 0.2352(3) 0.25670(18) 0.1129(2) 0.0186(6) Uani 1 1 d . . . C9 C 0.1937(3) 0.2048(2) 0.2394(2) 0.0290(8) Uani 1 1 d . . . H9 H 0.1276 0.1802 0.2456 0.044 Uiso 1 1 calc R . . H9A H 0.1983 0.2606 0.2569 0.044 Uiso 1 1 calc R . . H9B H 0.2593 0.1759 0.2725 0.044 Uiso 1 1 calc R . . C10 C 0.1044(3) 0.0594(2) 0.1242(3) 0.0326(8) Uani 1 1 d . . . H10 H 0.1665 0.0261 0.1549 0.049 Uiso 1 1 calc R . . H10A H 0.0605 0.0307 0.0758 0.049 Uiso 1 1 calc R . . H10B H 0.0581 0.0718 0.1574 0.049 Uiso 1 1 calc R . . C11 C 0.1550(3) 0.0911(2) -0.0402(2) 0.0295(8) Uani 1 1 d . . . H11 H 0.1421 0.1201 -0.0908 0.044 Uiso 1 1 calc R . . H11A H 0.0914 0.0569 -0.0443 0.044 Uiso 1 1 calc R . . H11B H 0.2213 0.0582 -0.0295 0.044 Uiso 1 1 calc R . . C12 C 0.2711(3) 0.2614(2) -0.0253(3) 0.0314(9) Uani 1 1 d . . . H12 H 0.3464 0.2415 -0.0149 0.047 Uiso 1 1 calc R . . H12A H 0.2726 0.3196 -0.0202 0.047 Uiso 1 1 calc R . . H12B H 0.2255 0.2464 -0.0799 0.047 Uiso 1 1 calc R . . C13 C 0.2981(3) 0.3305(2) 0.1499(2) 0.0297(8) Uani 1 1 d . . . H13 H 0.2634 0.3551 0.1862 0.044 Uiso 1 1 calc R . . H13A H 0.2976 0.3684 0.1073 0.044 Uiso 1 1 calc R . . H13B H 0.3744 0.3162 0.1803 0.044 Uiso 1 1 calc R . . C14 C 0.0475(2) 0.46115(18) 0.22037(18) 0.0167(6) Uani 1 1 d . . . C15 C 0.0944(3) 0.42543(19) 0.29482(19) 0.0200(6) Uani 1 1 d . . . H15 H 0.1081 0.3696 0.2985 0.024 Uiso 1 1 calc R . . C16 C 0.1215(3) 0.4720(2) 0.36455(19) 0.0236(7) Uani 1 1 d . . . H16 H 0.1531 0.4477 0.4158 0.028 Uiso 1 1 calc R . . C17 C 0.1025(3) 0.5533(2) 0.35915(19) 0.0228(7) Uani 1 1 d . . . H17 H 0.1192 0.5845 0.4067 0.027 Uiso 1 1 calc R . . C18 C 0.0588(3) 0.5895(2) 0.2842(2) 0.0226(7) Uani 1 1 d . . . H18 H 0.0477 0.6456 0.2805 0.027 Uiso 1 1 calc R . . C19 C 0.0314(3) 0.54330(19) 0.21487(19) 0.0191(6) Uani 1 1 d . . . H19 H 0.0017 0.5678 0.1636 0.023 Uiso 1 1 calc R . . C20 C -0.2268(2) 0.32630(18) 0.10666(18) 0.0173(6) Uani 1 1 d . . . Si1 Si -0.27284(8) 0.23237(6) 0.14843(6) 0.02270(19) Uani 1 1 d . . . Si2 Si -0.25671(7) 0.41508(6) 0.16504(6) 0.02192(19) Uani 1 1 d . . . Si3 Si -0.30728(7) 0.34057(5) -0.00515(5) 0.01763(17) Uani 1 1 d . . . C21 C -0.2042(4) 0.1376(2) 0.1330(3) 0.0352(9) Uani 1 1 d . . . H21 H -0.1240 0.1451 0.1516 0.053 Uiso 1 1 calc R . . H21A H -0.2294 0.1239 0.0756 0.053 Uiso 1 1 calc R . . H21B H -0.2233 0.0944 0.1636 0.053 Uiso 1 1 calc R . . C22 C -0.2447(4) 0.2342(3) 0.2599(3) 0.0393(10) Uani 1 1 d . . . H22 H -0.2722 0.1849 0.2766 0.059 Uiso 1 1 calc R . . H22A H -0.2822 0.2801 0.2740 0.059 Uiso 1 1 calc R . . H22B H -0.1651 0.2386 0.2875 0.059 Uiso 1 1 calc R . . C23 C -0.4243(3) 0.2131(3) 0.1026(3) 0.0353(9) Uani 1 1 d . . . H23 H -0.4429 0.1626 0.1232 0.053 Uiso 1 1 calc R . . H23A H -0.4437 0.2100 0.0440 0.053 Uiso 1 1 calc R . . H23B H -0.4657 0.2566 0.1167 0.053 Uiso 1 1 calc R . . C24 C -0.1664(3) 0.4209(3) 0.2740(2) 0.0319(8) Uani 1 1 d . . . H24 H -0.1300 0.4730 0.2844 0.048 Uiso 1 1 calc R . . H24A H -0.1105 0.3787 0.2852 0.048 Uiso 1 1 calc R . . H24B H -0.2118 0.4139 0.3088 0.048 Uiso 1 1 calc R . . C25 C -0.2458(3) 0.5126(2) 0.1159(2) 0.0303(8) Uani 1 1 d . . . H25 H -0.3086 0.5184 0.0663 0.045 Uiso 1 1 calc R . . H25A H -0.1770 0.5139 0.1030 0.045 Uiso 1 1 calc R . . H25B H -0.2462 0.5565 0.1526 0.045 Uiso 1 1 calc R . . C26 C -0.4006(3) 0.4147(3) 0.1723(2) 0.0340(9) Uani 1 1 d . . . H26 H -0.4130 0.4644 0.1974 0.051 Uiso 1 1 calc R . . H26A H -0.4086 0.3692 0.2050 0.051 Uiso 1 1 calc R . . H26B H -0.4547 0.4103 0.1182 0.051 Uiso 1 1 calc R . . C27 C -0.3305(3) 0.24580(19) -0.0657(2) 0.0268(8) Uani 1 1 d . . . H27 H -0.3921 0.2532 -0.1157 0.040 Uiso 1 1 calc R . . H27A H -0.3479 0.2024 -0.0344 0.040 Uiso 1 1 calc R . . H27B H -0.2637 0.2324 -0.0784 0.040 Uiso 1 1 calc R . . C28 C -0.2367(3) 0.4105(2) -0.0557(2) 0.0246(7) Uani 1 1 d . . . H28 H -0.2860 0.4226 -0.1101 0.037 Uiso 1 1 calc R . . H28A H -0.1692 0.3855 -0.0590 0.037 Uiso 1 1 calc R . . H28B H -0.2179 0.4600 -0.0246 0.037 Uiso 1 1 calc R . . C29 C -0.4502(3) 0.3830(2) -0.0273(2) 0.0287(8) Uani 1 1 d . . . H29 H -0.4453 0.4366 -0.0042 0.043 Uiso 1 1 calc R . . H29A H -0.4931 0.3486 -0.0035 0.043 Uiso 1 1 calc R . . H29B H -0.4865 0.3858 -0.0857 0.043 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 W1 0.01327(8) 0.01186(7) 0.01460(8) -0.00077(4) 0.00349(5) 0.00028(4) Ge1 0.01507(15) 0.01161(14) 0.01560(14) -0.00004(11) 0.00595(12) -0.00080(11) N1 0.0183(12) 0.0122(11) 0.0171(12) -0.0010(10) 0.0065(10) -0.0015(10) C1 0.0208(15) 0.0130(13) 0.0201(14) 0.0012(12) 0.0060(12) -0.0002(12) S1 0.0230(4) 0.0140(3) 0.0171(3) 0.0010(3) 0.0087(3) -0.0003(3) C2 0.0219(16) 0.0188(15) 0.0281(16) -0.0034(13) 0.0086(13) 0.0022(13) O1 0.0227(12) 0.0223(12) 0.0500(16) -0.0124(12) 0.0085(12) -0.0073(10) C3 0.0255(18) 0.0200(17) 0.0203(17) -0.0029(12) 0.0026(14) 0.0015(12) O2 0.0477(19) 0.0397(17) 0.0182(14) 0.0006(10) 0.0015(13) 0.0060(12) C4 0.0178(14) 0.0216(15) 0.0171(14) 0.0029(12) 0.0049(12) 0.0054(12) C5 0.0187(15) 0.0155(14) 0.0250(15) 0.0046(12) 0.0074(12) 0.0047(12) C6 0.0164(14) 0.0188(15) 0.0206(15) 0.0006(12) 0.0048(12) 0.0077(12) C7 0.0140(14) 0.0213(15) 0.0184(15) 0.0001(13) 0.0041(12) 0.0018(12) C8 0.0154(15) 0.0177(15) 0.0190(16) -0.0017(12) 0.0003(13) 0.0006(11) C9 0.0290(18) 0.041(2) 0.0159(15) 0.0041(15) 0.0063(13) 0.0095(16) C10 0.031(2) 0.0220(17) 0.046(2) 0.0130(16) 0.0134(17) 0.0061(15) C11 0.0281(18) 0.0269(17) 0.0303(18) -0.0099(15) 0.0051(15) 0.0069(15) C12 0.0246(19) 0.042(2) 0.032(2) 0.0081(16) 0.0152(17) 0.0016(16) C13 0.0247(17) 0.0279(18) 0.0312(18) -0.0037(15) 0.0020(14) -0.0036(15) C14 0.0161(14) 0.0161(14) 0.0173(14) -0.0012(12) 0.0046(11) -0.0007(11) C15 0.0207(15) 0.0176(14) 0.0209(15) 0.0002(12) 0.0055(12) 0.0012(12) C16 0.0222(16) 0.0272(17) 0.0175(14) 0.0001(13) 0.0012(12) 0.0038(13) C17 0.0188(15) 0.0268(17) 0.0210(15) -0.0099(13) 0.0037(12) -0.0029(13) C18 0.0222(16) 0.0180(15) 0.0285(17) -0.0058(13) 0.0092(13) -0.0019(13) C19 0.0193(15) 0.0187(15) 0.0192(14) 0.0005(12) 0.0060(12) 0.0004(12) C20 0.0160(14) 0.0175(14) 0.0194(14) 0.0010(12) 0.0073(12) -0.0013(12) Si1 0.0254(5) 0.0213(4) 0.0250(5) 0.0028(4) 0.0130(4) -0.0054(4) Si2 0.0190(4) 0.0232(4) 0.0266(4) -0.0062(4) 0.0117(4) -0.0015(3) Si3 0.0162(4) 0.0164(4) 0.0197(4) 0.0004(3) 0.0051(3) -0.0014(3) C21 0.043(2) 0.0176(16) 0.051(2) 0.0065(16) 0.0223(19) -0.0016(16) C22 0.056(3) 0.037(2) 0.028(2) 0.0095(17) 0.019(2) -0.009(2) C23 0.0289(19) 0.036(2) 0.045(2) 0.0036(18) 0.0174(17) -0.0116(17) C24 0.0288(19) 0.043(2) 0.0278(18) -0.0122(16) 0.0139(15) -0.0073(16) C25 0.0290(18) 0.0210(16) 0.040(2) -0.0043(15) 0.0099(16) 0.0007(14) C26 0.0224(18) 0.040(2) 0.045(2) -0.0102(18) 0.0184(16) -0.0018(16) C27 0.030(2) 0.0233(17) 0.0248(18) -0.0068(13) 0.0051(16) -0.0040(13) C28 0.0247(16) 0.0255(17) 0.0221(16) 0.0042(13) 0.0054(13) -0.0013(14) C29 0.0187(16) 0.0287(18) 0.0348(19) -0.0005(15) 0.0033(14) 0.0008(14) _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 W1 C3 1.953(4) . ? W1 C2 1.957(3) . ? W1 C6 2.283(3) . ? W1 C7 2.308(3) . ? W1 C5 2.335(3) . ? W1 C8 2.408(3) . ? W1 C4 2.417(3) . ? W1 S1 2.4657(7) . ? W1 Ge1 2.6326(3) . ? Ge1 C20 2.055(3) . ? Ge1 N1 2.068(2) . ? N1 C1 1.303(4) . ? N1 C14 1.447(4) . ? C1 S1 1.688(3) . ? C1 H1A 0.9500 . ? C2 O1 1.159(4) . ? C3 O2 1.166(5) . ? C4 C8 1.419(5) . ? C4 C5 1.426(5) . ? C4 C9 1.497(4) . ? C5 C6 1.428(4) . ? C5 C10 1.498(5) . ? C6 C7 1.428(5) . ? C6 C11 1.507(4) . ? C7 C8 1.432(5) . ? C7 C12 1.505(5) . ? C8 C13 1.505(5) . ? C9 H9 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 H11 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.386(4) . ? C14 C19 1.391(4) . ? C15 C16 1.398(4) . ? C15 H15 0.9500 . ? C16 C17 1.382(5) . ? C16 H16 0.9500 . ? C17 C18 1.392(5) . ? C17 H17 0.9500 . ? C18 C19 1.389(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 Si1 1.911(3) . ? C20 Si3 1.914(3) . ? C20 Si2 1.916(3) . ? Si1 C23 1.873(4) . ? Si1 C22 1.874(4) . ? Si1 C21 1.879(4) . ? Si2 C25 1.876(4) . ? Si2 C26 1.890(4) . ? Si2 C24 1.890(4) . ? Si3 C28 1.873(3) . ? Si3 C27 1.881(3) . ? Si3 C29 1.885(4) . ? C21 H21 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 H23 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 H24 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 H25 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 H27 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 H28 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? 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 C3 W1 C2 74.68(14) . . ? C3 W1 C6 90.72(13) . . ? C2 W1 C6 91.51(13) . . ? C3 W1 C7 92.06(14) . . ? C2 W1 C7 126.67(13) . . ? C6 W1 C7 36.22(11) . . ? C3 W1 C5 122.11(12) . . ? C2 W1 C5 84.13(13) . . ? C6 W1 C5 35.99(11) . . ? C7 W1 C5 59.59(11) . . ? C3 W1 C8 124.06(14) . . ? C2 W1 C8 142.20(12) . . ? C6 W1 C8 58.96(11) . . ? C7 W1 C8 35.28(11) . . ? C5 W1 C8 58.08(11) . . ? C3 W1 C4 148.20(13) . . ? C2 W1 C4 111.93(13) . . ? C6 W1 C4 58.80(11) . . ? C7 W1 C4 58.42(11) . . ? C5 W1 C4 34.87(11) . . ? C8 W1 C4 34.20(11) . . ? C3 W1 S1 78.10(9) . . ? C2 W1 S1 134.31(10) . . ? C6 W1 S1 125.00(9) . . ? C7 W1 S1 89.93(9) . . ? C5 W1 S1 141.55(8) . . ? C8 W1 S1 83.47(7) . . ? C4 W1 S1 110.60(8) . . ? C3 W1 Ge1 122.79(11) . . ? C2 W1 Ge1 86.34(10) . . ? C6 W1 Ge1 144.18(8) . . ? C7 W1 Ge1 139.03(8) . . ? C5 W1 Ge1 108.38(8) . . ? C8 W1 Ge1 103.90(8) . . ? C4 W1 Ge1 88.99(7) . . ? S1 W1 Ge1 78.453(19) . . ? C20 Ge1 N1 109.13(11) . . ? C20 Ge1 W1 133.58(9) . . ? N1 Ge1 W1 97.35(7) . . ? C1 N1 C14 115.7(3) . . ? C1 N1 Ge1 115.3(2) . . ? C14 N1 Ge1 129.1(2) . . ? N1 C1 S1 126.0(2) . . ? N1 C1 H1A 117.0 . . ? S1 C1 H1A 117.0 . . ? C1 S1 W1 109.29(11) . . ? O1 C2 W1 170.2(3) . . ? O2 C3 W1 174.7(3) . . ? C8 C4 C5 108.1(3) . . ? C8 C4 C9 126.1(3) . . ? C5 C4 C9 125.2(3) . . ? C8 C4 W1 72.54(18) . . ? C5 C4 W1 69.43(17) . . ? C9 C4 W1 130.6(2) . . ? C4 C5 C6 108.1(3) . . ? C4 C5 C10 124.6(3) . . ? C6 C5 C10 126.7(3) . . ? C4 C5 W1 75.70(18) . . ? C6 C5 W1 70.03(17) . . ? C10 C5 W1 127.4(2) . . ? C5 C6 C7 107.8(3) . . ? C5 C6 C11 125.8(3) . . ? C7 C6 C11 126.0(3) . . ? C5 C6 W1 73.98(17) . . ? C7 C6 W1 72.83(17) . . ? C11 C6 W1 124.7(2) . . ? C6 C7 C8 107.8(3) . . ? C6 C7 C12 125.7(3) . . ? C8 C7 C12 126.0(3) . . ? C6 C7 W1 70.95(17) . . ? C8 C7 W1 76.16(19) . . ? C12 C7 W1 124.5(2) . . ? C4 C8 C7 108.1(3) . . ? C4 C8 C13 125.5(3) . . ? C7 C8 C13 126.0(3) . . ? C4 C8 W1 73.26(18) . . ? C7 C8 W1 68.57(18) . . ? C13 C8 W1 128.9(2) . . ? C4 C9 H9 109.5 . . ? C4 C9 H9A 109.5 . . ? H9 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C10 H10 109.5 . . ? C5 C10 H10A 109.5 . . ? H10 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C11 H11 109.5 . . ? C6 C11 H11A 109.5 . . ? H11 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C12 H12 109.5 . . ? C7 C12 H12A 109.5 . . ? H12 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C13 H13 109.5 . . ? C8 C13 H13A 109.5 . . ? H13 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C15 C14 C19 120.2(3) . . ? C15 C14 N1 118.8(3) . . ? C19 C14 N1 120.9(3) . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.2(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 119.8(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C14 120.1(3) . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? Si1 C20 Si3 111.50(16) . . ? Si1 C20 Si2 107.07(15) . . ? Si3 C20 Si2 108.52(15) . . ? Si1 C20 Ge1 103.57(14) . . ? Si3 C20 Ge1 110.72(15) . . ? Si2 C20 Ge1 115.37(15) . . ? C23 Si1 C22 105.8(2) . . ? C23 Si1 C21 105.15(19) . . ? C22 Si1 C21 103.0(2) . . ? C23 Si1 C20 112.58(16) . . ? C22 Si1 C20 114.20(17) . . ? C21 Si1 C20 115.05(16) . . ? C25 Si2 C26 104.75(18) . . ? C25 Si2 C24 107.99(18) . . ? C26 Si2 C24 102.81(17) . . ? C25 Si2 C20 111.86(15) . . ? C26 Si2 C20 113.80(16) . . ? C24 Si2 C20 114.76(16) . . ? C28 Si3 C27 105.81(17) . . ? C28 Si3 C29 104.69(16) . . ? C27 Si3 C29 103.73(18) . . ? C28 Si3 C20 112.51(14) . . ? C27 Si3 C20 114.10(16) . . ? C29 Si3 C20 115.00(15) . . ? Si1 C21 H21 109.5 . . ? Si1 C21 H21A 109.5 . . ? H21 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C22 H22 109.5 . . ? Si1 C22 H22A 109.5 . . ? H22 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C23 H23 109.5 . . ? Si1 C23 H23A 109.5 . . ? H23 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C24 H24 109.5 . . ? Si2 C24 H24A 109.5 . . ? H24 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C25 H25 109.5 . . ? Si2 C25 H25A 109.5 . . ? H25 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C26 H26 109.5 . . ? Si2 C26 H26A 109.5 . . ? H26 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si3 C27 H27 109.5 . . ? Si3 C27 H27A 109.5 . . ? H27 C27 H27A 109.5 . . ? Si3 C27 H27B 109.5 . . ? H27 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si3 C28 H28 109.5 . . ? Si3 C28 H28A 109.5 . . ? H28 C28 H28A 109.5 . . ? Si3 C28 H28B 109.5 . . ? H28 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si3 C29 H29 109.5 . . ? Si3 C29 H29A 109.5 . . ? H29 C29 H29A 109.5 . . ? Si3 C29 H29B 109.5 . . ? H29 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? 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 C3 W1 Ge1 C20 29.10(17) . . . . ? C2 W1 Ge1 C20 -40.04(15) . . . . ? C6 W1 Ge1 C20 -127.54(18) . . . . ? C7 W1 Ge1 C20 172.92(17) . . . . ? C5 W1 Ge1 C20 -122.61(14) . . . . ? C8 W1 Ge1 C20 176.85(14) . . . . ? C4 W1 Ge1 C20 -152.09(14) . . . . ? S1 W1 Ge1 C20 96.64(12) . . . . ? C3 W1 Ge1 N1 -96.27(14) . . . . ? C2 W1 Ge1 N1 -165.41(12) . . . . ? C6 W1 Ge1 N1 107.09(16) . . . . ? C7 W1 Ge1 N1 47.55(15) . . . . ? C5 W1 Ge1 N1 112.02(11) . . . . ? C8 W1 Ge1 N1 51.48(10) . . . . ? C4 W1 Ge1 N1 82.55(11) . . . . ? S1 W1 Ge1 N1 -28.73(7) . . . . ? C20 Ge1 N1 C1 -110.6(2) . . . . ? W1 Ge1 N1 C1 30.7(2) . . . . ? C20 Ge1 N1 C14 70.2(3) . . . . ? W1 Ge1 N1 C14 -148.5(2) . . . . ? C14 N1 C1 S1 169.9(2) . . . . ? Ge1 N1 C1 S1 -9.4(4) . . . . ? N1 C1 S1 W1 -20.2(3) . . . . ? C3 W1 S1 C1 156.98(17) . . . . ? C2 W1 S1 C1 102.64(18) . . . . ? C6 W1 S1 C1 -120.60(15) . . . . ? C7 W1 S1 C1 -110.90(14) . . . . ? C5 W1 S1 C1 -75.56(18) . . . . ? C8 W1 S1 C1 -76.14(15) . . . . ? C4 W1 S1 C1 -54.95(14) . . . . ? Ge1 W1 S1 C1 29.53(12) . . . . ? C3 W1 C2 O1 65.7(18) . . . . ? C6 W1 C2 O1 -24.6(18) . . . . ? C7 W1 C2 O1 -15.2(19) . . . . ? C5 W1 C2 O1 -59.9(18) . . . . ? C8 W1 C2 O1 -60.8(19) . . . . ? C4 W1 C2 O1 -81.4(18) . . . . ? S1 W1 C2 O1 121.2(18) . . . . ? Ge1 W1 C2 O1 -168.8(18) . . . . ? C2 W1 C3 O2 -91(4) . . . . ? C6 W1 C3 O2 1(4) . . . . ? C7 W1 C3 O2 37(4) . . . . ? C5 W1 C3 O2 -18(4) . . . . ? C8 W1 C3 O2 53(4) . . . . ? C4 W1 C3 O2 16(4) . . . . ? S1 W1 C3 O2 127(4) . . . . ? Ge1 W1 C3 O2 -166(4) . . . . ? C3 W1 C4 C8 61.1(3) . . . . ? C2 W1 C4 C8 157.39(19) . . . . ? C6 W1 C4 C8 79.5(2) . . . . ? C7 W1 C4 C8 36.84(19) . . . . ? C5 W1 C4 C8 117.8(3) . . . . ? S1 W1 C4 C8 -39.7(2) . . . . ? Ge1 W1 C4 C8 -116.97(18) . . . . ? C3 W1 C4 C5 -56.6(3) . . . . ? C2 W1 C4 C5 39.6(2) . . . . ? C6 W1 C4 C5 -38.25(18) . . . . ? C7 W1 C4 C5 -81.0(2) . . . . ? C8 W1 C4 C5 -117.8(3) . . . . ? S1 W1 C4 C5 -157.50(16) . . . . ? Ge1 W1 C4 C5 125.24(18) . . . . ? C3 W1 C4 C9 -175.9(3) . . . . ? C2 W1 C4 C9 -79.6(3) . . . . ? C6 W1 C4 C9 -157.5(4) . . . . ? C7 W1 C4 C9 159.8(4) . . . . ? C5 W1 C4 C9 -119.2(4) . . . . ? C8 W1 C4 C9 123.0(4) . . . . ? S1 W1 C4 C9 83.3(3) . . . . ? Ge1 W1 C4 C9 6.0(3) . . . . ? C8 C4 C5 C6 0.4(4) . . . . ? C9 C4 C5 C6 -171.1(3) . . . . ? W1 C4 C5 C6 63.0(2) . . . . ? C8 C4 C5 C10 171.5(3) . . . . ? C9 C4 C5 C10 0.1(5) . . . . ? W1 C4 C5 C10 -125.8(3) . . . . ? C8 C4 C5 W1 -62.6(2) . . . . ? C9 C4 C5 W1 125.9(3) . . . . ? C3 W1 C5 C4 148.7(2) . . . . ? C2 W1 C5 C4 -143.5(2) . . . . ? C6 W1 C5 C4 115.7(3) . . . . ? C7 W1 C5 C4 77.3(2) . . . . ? C8 W1 C5 C4 35.86(18) . . . . ? S1 W1 C5 C4 35.2(2) . . . . ? Ge1 W1 C5 C4 -59.37(18) . . . . ? C3 W1 C5 C6 33.0(2) . . . . ? C2 W1 C5 C6 100.8(2) . . . . ? C7 W1 C5 C6 -38.41(18) . . . . ? C8 W1 C5 C6 -79.9(2) . . . . ? C4 W1 C5 C6 -115.7(3) . . . . ? S1 W1 C5 C6 -80.5(2) . . . . ? Ge1 W1 C5 C6 -175.09(16) . . . . ? C3 W1 C5 C10 -88.5(3) . . . . ? C2 W1 C5 C10 -20.7(3) . . . . ? C6 W1 C5 C10 -121.5(4) . . . . ? C7 W1 C5 C10 -159.9(4) . . . . ? C8 W1 C5 C10 158.7(4) . . . . ? C4 W1 C5 C10 122.8(4) . . . . ? S1 W1 C5 C10 158.0(2) . . . . ? Ge1 W1 C5 C10 63.4(3) . . . . ? C4 C5 C6 C7 -1.2(3) . . . . ? C10 C5 C6 C7 -172.2(3) . . . . ? W1 C5 C6 C7 65.5(2) . . . . ? C4 C5 C6 C11 171.8(3) . . . . ? C10 C5 C6 C11 0.9(5) . . . . ? W1 C5 C6 C11 -121.5(3) . . . . ? C4 C5 C6 W1 -66.7(2) . . . . ? C10 C5 C6 W1 122.3(3) . . . . ? C3 W1 C6 C5 -152.5(2) . . . . ? C2 W1 C6 C5 -77.9(2) . . . . ? C7 W1 C6 C5 114.9(3) . . . . ? C8 W1 C6 C5 77.2(2) . . . . ? C4 W1 C6 C5 37.03(18) . . . . ? S1 W1 C6 C5 131.52(16) . . . . ? Ge1 W1 C6 C5 8.0(3) . . . . ? C3 W1 C6 C7 92.5(2) . . . . ? C2 W1 C6 C7 167.2(2) . . . . ? C5 W1 C6 C7 -114.9(3) . . . . ? C8 W1 C6 C7 -37.74(18) . . . . ? C4 W1 C6 C7 -77.92(19) . . . . ? S1 W1 C6 C7 16.6(2) . . . . ? Ge1 W1 C6 C7 -106.96(19) . . . . ? C3 W1 C6 C11 -29.8(3) . . . . ? C2 W1 C6 C11 44.9(3) . . . . ? C7 W1 C6 C11 -122.3(4) . . . . ? C5 W1 C6 C11 122.8(4) . . . . ? C8 W1 C6 C11 -160.0(3) . . . . ? C4 W1 C6 C11 159.8(3) . . . . ? S1 W1 C6 C11 -105.7(3) . . . . ? Ge1 W1 C6 C11 130.8(2) . . . . ? C5 C6 C7 C8 1.6(3) . . . . ? C11 C6 C7 C8 -171.4(3) . . . . ? W1 C6 C7 C8 67.9(2) . . . . ? C5 C6 C7 C12 174.4(3) . . . . ? C11 C6 C7 C12 1.4(5) . . . . ? W1 C6 C7 C12 -119.4(3) . . . . ? C5 C6 C7 W1 -66.3(2) . . . . ? C11 C6 C7 W1 120.7(3) . . . . ? C3 W1 C7 C6 -88.40(19) . . . . ? C2 W1 C7 C6 -16.0(2) . . . . ? C5 W1 C7 C6 38.16(18) . . . . ? C8 W1 C7 C6 114.8(3) . . . . ? C4 W1 C7 C6 79.1(2) . . . . ? S1 W1 C7 C6 -166.49(17) . . . . ? Ge1 W1 C7 C6 121.37(17) . . . . ? C3 W1 C7 C8 156.84(19) . . . . ? C2 W1 C7 C8 -130.8(2) . . . . ? C6 W1 C7 C8 -114.8(3) . . . . ? C5 W1 C7 C8 -76.6(2) . . . . ? C4 W1 C7 C8 -35.69(18) . . . . ? S1 W1 C7 C8 78.75(18) . . . . ? Ge1 W1 C7 C8 6.6(2) . . . . ? C3 W1 C7 C12 32.4(3) . . . . ? C2 W1 C7 C12 104.8(3) . . . . ? C6 W1 C7 C12 120.8(4) . . . . ? C5 W1 C7 C12 159.0(3) . . . . ? C8 W1 C7 C12 -124.4(4) . . . . ? C4 W1 C7 C12 -160.1(3) . . . . ? S1 W1 C7 C12 -45.7(3) . . . . ? Ge1 W1 C7 C12 -117.8(3) . . . . ? C5 C4 C8 C7 0.6(4) . . . . ? C9 C4 C8 C7 172.0(3) . . . . ? W1 C4 C8 C7 -60.0(2) . . . . ? C5 C4 C8 C13 -173.2(3) . . . . ? C9 C4 C8 C13 -1.8(5) . . . . ? W1 C4 C8 C13 126.2(3) . . . . ? C5 C4 C8 W1 60.6(2) . . . . ? C9 C4 C8 W1 -128.0(3) . . . . ? C6 C7 C8 C4 -1.4(4) . . . . ? C12 C7 C8 C4 -174.1(3) . . . . ? W1 C7 C8 C4 63.0(2) . . . . ? C6 C7 C8 C13 172.4(3) . . . . ? C12 C7 C8 C13 -0.4(5) . . . . ? W1 C7 C8 C13 -123.2(3) . . . . ? C6 C7 C8 W1 -64.4(2) . . . . ? C12 C7 C8 W1 122.9(3) . . . . ? C3 W1 C8 C4 -146.15(19) . . . . ? C2 W1 C8 C4 -35.6(3) . . . . ? C6 W1 C8 C4 -79.1(2) . . . . ? C7 W1 C8 C4 -117.8(3) . . . . ? C5 W1 C8 C4 -36.58(18) . . . . ? S1 W1 C8 C4 142.99(19) . . . . ? Ge1 W1 C8 C4 66.64(18) . . . . ? C3 W1 C8 C7 -28.3(2) . . . . ? C2 W1 C8 C7 82.2(3) . . . . ? C6 W1 C8 C7 38.78(19) . . . . ? C5 W1 C8 C7 81.2(2) . . . . ? C4 W1 C8 C7 117.8(3) . . . . ? S1 W1 C8 C7 -99.18(18) . . . . ? Ge1 W1 C8 C7 -175.54(17) . . . . ? C3 W1 C8 C13 91.4(3) . . . . ? C2 W1 C8 C13 -158.1(3) . . . . ? C6 W1 C8 C13 158.5(4) . . . . ? C7 W1 C8 C13 119.7(4) . . . . ? C5 W1 C8 C13 -159.0(4) . . . . ? C4 W1 C8 C13 -122.5(4) . . . . ? S1 W1 C8 C13 20.5(3) . . . . ? Ge1 W1 C8 C13 -55.8(3) . . . . ? C1 N1 C14 C15 -129.3(3) . . . . ? Ge1 N1 C14 C15 49.9(4) . . . . ? C1 N1 C14 C19 46.9(4) . . . . ? Ge1 N1 C14 C19 -133.9(3) . . . . ? C19 C14 C15 C16 2.5(5) . . . . ? N1 C14 C15 C16 178.7(3) . . . . ? C14 C15 C16 C17 -0.5(5) . . . . ? C15 C16 C17 C18 -1.6(5) . . . . ? C16 C17 C18 C19 1.8(5) . . . . ? C17 C18 C19 C14 0.1(5) . . . . ? C15 C14 C19 C18 -2.3(5) . . . . ? N1 C14 C19 C18 -178.4(3) . . . . ? N1 Ge1 C20 Si1 -146.00(12) . . . . ? W1 Ge1 C20 Si1 92.87(14) . . . . ? N1 Ge1 C20 Si3 94.37(15) . . . . ? W1 Ge1 C20 Si3 -26.8(2) . . . . ? N1 Ge1 C20 Si2 -29.35(18) . . . . ? W1 Ge1 C20 Si2 -150.48(9) . . . . ? Si3 C20 Si1 C23 -35.7(2) . . . . ? Si2 C20 Si1 C23 82.9(2) . . . . ? Ge1 C20 Si1 C23 -154.75(17) . . . . ? Si3 C20 Si1 C22 -156.3(2) . . . . ? Si2 C20 Si1 C22 -37.8(2) . . . . ? Ge1 C20 Si1 C22 84.6(2) . . . . ? Si3 C20 Si1 C21 84.8(2) . . . . ? Si2 C20 Si1 C21 -156.65(18) . . . . ? Ge1 C20 Si1 C21 -34.3(2) . . . . ? Si1 C20 Si2 C25 -167.14(16) . . . . ? Si3 C20 Si2 C25 -46.7(2) . . . . ? Ge1 C20 Si2 C25 78.2(2) . . . . ? Si1 C20 Si2 C26 -48.7(2) . . . . ? Si3 C20 Si2 C26 71.8(2) . . . . ? Ge1 C20 Si2 C26 -163.32(18) . . . . ? Si1 C20 Si2 C24 69.4(2) . . . . ? Si3 C20 Si2 C24 -170.13(16) . . . . ? Ge1 C20 Si2 C24 -45.3(2) . . . . ? Si1 C20 Si3 C28 -161.62(16) . . . . ? Si2 C20 Si3 C28 80.70(19) . . . . ? Ge1 C20 Si3 C28 -46.9(2) . . . . ? Si1 C20 Si3 C27 -41.1(2) . . . . ? Si2 C20 Si3 C27 -158.75(17) . . . . ? Ge1 C20 Si3 C27 73.7(2) . . . . ? Si1 C20 Si3 C29 78.6(2) . . . . ? Si2 C20 Si3 C29 -39.1(2) . . . . ? Ge1 C20 Si3 C29 -166.62(15) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.810 _refine_diff_density_min -1.460 _refine_diff_density_rms 0.224 #===END data_PhNCS2 _database_code_depnum_ccdc_archive 'CCDC 767388' #TrackingRef '- combinedCIFsRev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H49 Ge N O2 S Si3 W' _chemical_formula_weight 816.46 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 8.9678(4) _cell_length_b 25.2891(6) _cell_length_c 15.0542(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.9373(10) _cell_angle_gamma 90.00 _cell_volume 3401.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7689 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 4.456 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6169 _exptl_absorpt_correction_T_max 0.7170 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30578 _diffrn_reflns_av_R_equivalents 0.0802 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7689 _reflns_number_gt 6505 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material 'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' _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^)+(0.0444P)^2^+26.1991P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7689 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.326 _refine_ls_restrained_S_all 1.326 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.06110(4) 0.109432(12) 0.19480(2) 0.01104(10) Uani 1 1 d . . . Ge1 Ge -0.01043(9) 0.20580(3) 0.13958(6) 0.01097(18) Uani 1 1 d . . . H1 H -0.014(10) 0.213(3) 0.043(6) 0.02(2) Uiso 1 1 d . . . S1 S -0.2689(2) 0.19488(8) 0.14505(15) 0.0183(4) Uani 1 1 d . . . C1 C -0.2582(10) 0.1532(3) 0.2352(6) 0.0162(17) Uani 1 1 d . . . H2 H -0.3453 0.1509 0.2667 0.019 Uiso 1 1 calc R . . N1 N -0.1449(8) 0.1242(3) 0.2657(5) 0.0139(14) Uani 1 1 d . . . C2 C 0.2617(10) 0.1397(3) 0.2012(6) 0.0179(18) Uani 1 1 d . . . O1 O 0.3875(8) 0.1504(3) 0.2066(5) 0.0306(16) Uani 1 1 d . . . C3 C 0.1663(10) 0.0898(3) 0.3101(6) 0.0167(17) Uani 1 1 d . . . O2 O 0.2464(8) 0.0747(3) 0.3695(4) 0.0268(15) Uani 1 1 d . . . C4 C -0.0307(10) 0.0803(3) 0.0470(6) 0.0182(18) Uani 1 1 d . . . C5 C 0.1286(11) 0.0724(3) 0.0631(6) 0.0207(19) Uani 1 1 d . . . C6 C 0.1518(10) 0.0349(3) 0.1348(6) 0.0186(18) Uani 1 1 d . . . C7 C 0.0109(9) 0.0212(3) 0.1657(6) 0.0150(16) Uiso 1 1 d . . . C8 C -0.1039(10) 0.0491(3) 0.1079(6) 0.0166(17) Uani 1 1 d . . . C9 C -0.1059(12) 0.1102(4) -0.0311(6) 0.027(2) Uani 1 1 d . . . H3 H -0.1235 0.0862 -0.0822 0.040 Uiso 1 1 calc R . . H4 H -0.0414 0.1393 -0.0470 0.040 Uiso 1 1 calc R . . H5 H -0.2017 0.1243 -0.0151 0.040 Uiso 1 1 calc R . . C10 C 0.2451(12) 0.0938(4) 0.0067(7) 0.030(2) Uani 1 1 d . . . H6 H 0.3438 0.0916 0.0399 0.044 Uiso 1 1 calc R . . H7 H 0.2222 0.1308 -0.0085 0.044 Uiso 1 1 calc R . . H8 H 0.2452 0.0729 -0.0481 0.044 Uiso 1 1 calc R . . C11 C 0.3003(10) 0.0103(3) 0.1650(6) 0.0208(18) Uani 1 1 d . . . H9 H 0.2987 -0.0021 0.2266 0.031 Uiso 1 1 calc R . . H10 H 0.3798 0.0366 0.1618 0.031 Uiso 1 1 calc R . . H11 H 0.3191 -0.0197 0.1263 0.031 Uiso 1 1 calc R . . C12 C -0.0213(12) -0.0207(4) 0.2317(7) 0.028(2) Uani 1 1 d . . . H12 H -0.0490 -0.0536 0.2001 0.042 Uiso 1 1 calc R . . H13 H -0.1039 -0.0091 0.2656 0.042 Uiso 1 1 calc R . . H14 H 0.0681 -0.0267 0.2726 0.042 Uiso 1 1 calc R . . C13 C -0.2711(11) 0.0419(4) 0.1059(7) 0.027(2) Uani 1 1 d . . . H15 H -0.3194 0.0765 0.1090 0.040 Uiso 1 1 calc R . . H16 H -0.2947 0.0203 0.1570 0.040 Uiso 1 1 calc R . . H17 H -0.3079 0.0241 0.0505 0.040 Uiso 1 1 calc R . . C14 C -0.1737(11) 0.0942(3) 0.3442(6) 0.0211(19) Uani 1 1 d . . . C15 C -0.0796(11) 0.0981(4) 0.4219(6) 0.024(2) Uani 1 1 d . . . H18 H 0.0034 0.1216 0.4250 0.029 Uiso 1 1 calc R . . C16 C -0.1068(14) 0.0679(4) 0.4945(7) 0.038(3) Uani 1 1 d . . . H19 H -0.0393 0.0700 0.5466 0.046 Uiso 1 1 calc R . . C17 C -0.2272(16) 0.0349(4) 0.4947(8) 0.046(3) Uani 1 1 d . . . H20 H -0.2419 0.0137 0.5454 0.055 Uiso 1 1 calc R . . C18 C -0.3279(15) 0.0329(4) 0.4192(8) 0.041(3) Uani 1 1 d . . . H21 H -0.4147 0.0113 0.4187 0.049 Uiso 1 1 calc R . . C19 C -0.3012(12) 0.0624(4) 0.3448(7) 0.028(2) Uani 1 1 d . . . H22 H -0.3705 0.0611 0.2935 0.033 Uiso 1 1 calc R . . C20 C 0.0226(9) 0.2827(3) 0.1752(5) 0.0121(16) Uani 1 1 d . . . Si1 Si 0.2353(3) 0.28963(9) 0.19503(15) 0.0133(4) Uani 1 1 d . . . Si2 Si -0.0524(3) 0.32471(9) 0.07661(16) 0.0156(5) Uani 1 1 d . . . Si3 Si -0.0689(3) 0.30025(9) 0.28057(16) 0.0163(5) Uani 1 1 d . . . C21 C 0.3031(10) 0.3601(3) 0.1967(6) 0.0198(18) Uani 1 1 d . . . H23 H 0.2630 0.3790 0.2463 0.030 Uiso 1 1 calc R . . H24 H 0.2688 0.3773 0.1404 0.030 Uiso 1 1 calc R . . H25 H 0.4127 0.3606 0.2045 0.030 Uiso 1 1 calc R . . C22 C 0.3091(10) 0.2608(4) 0.3053(6) 0.0201(18) Uani 1 1 d . . . H26 H 0.4185 0.2585 0.3079 0.030 Uiso 1 1 calc R . . H27 H 0.2673 0.2253 0.3117 0.030 Uiso 1 1 calc R . . H28 H 0.2801 0.2835 0.3537 0.030 Uiso 1 1 calc R . . C23 C 0.3322(10) 0.2573(3) 0.1035(6) 0.0196(18) Uani 1 1 d . . . H29 H 0.3350 0.2819 0.0533 0.029 Uiso 1 1 calc R . . H30 H 0.2775 0.2253 0.0835 0.029 Uiso 1 1 calc R . . H31 H 0.4346 0.2479 0.1258 0.029 Uiso 1 1 calc R . . C24 C -0.2458(10) 0.3060(4) 0.0309(7) 0.024(2) Uani 1 1 d . . . H32 H -0.2458 0.2694 0.0096 0.036 Uiso 1 1 calc R . . H33 H -0.2784 0.3296 -0.0188 0.036 Uiso 1 1 calc R . . H34 H -0.3145 0.3093 0.0778 0.036 Uiso 1 1 calc R . . C25 C -0.0664(12) 0.3970(3) 0.1057(7) 0.029(2) Uani 1 1 d . . . H35 H 0.0340 0.4111 0.1223 0.044 Uiso 1 1 calc R . . H36 H -0.1281 0.4010 0.1559 0.044 Uiso 1 1 calc R . . H37 H -0.1123 0.4164 0.0541 0.044 Uiso 1 1 calc R . . C26 C 0.0633(11) 0.3226(4) -0.0208(6) 0.0218(19) Uani 1 1 d . . . H38 H 0.0770 0.2858 -0.0387 0.033 Uiso 1 1 calc R . . H39 H 0.1613 0.3386 -0.0041 0.033 Uiso 1 1 calc R . . H40 H 0.0125 0.3423 -0.0707 0.033 Uiso 1 1 calc R . . C27 C 0.0170(11) 0.3606(4) 0.3391(6) 0.027(2) Uani 1 1 d . . . H41 H 0.0137 0.3904 0.2973 0.040 Uiso 1 1 calc R . . H42 H 0.1212 0.3531 0.3603 0.040 Uiso 1 1 calc R . . H43 H -0.0395 0.3696 0.3899 0.040 Uiso 1 1 calc R . . C28 C -0.2724(11) 0.3188(4) 0.2633(7) 0.030(2) Uani 1 1 d . . . H44 H -0.3300 0.2887 0.2377 0.044 Uiso 1 1 calc R . . H45 H -0.2844 0.3490 0.2225 0.044 Uiso 1 1 calc R . . H46 H -0.3089 0.3283 0.3207 0.044 Uiso 1 1 calc R . . C29 C -0.0559(11) 0.2455(4) 0.3646(6) 0.026(2) Uani 1 1 d . . . H47 H -0.0277 0.2601 0.4240 0.039 Uiso 1 1 calc R . . H48 H 0.0200 0.2199 0.3494 0.039 Uiso 1 1 calc R . . H49 H -0.1531 0.2278 0.3645 0.039 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 W1 0.00967(16) 0.00995(15) 0.01331(16) 0.00156(12) -0.00011(10) 0.00057(13) Ge1 0.0107(4) 0.0092(4) 0.0128(4) 0.0013(3) 0.0000(3) -0.0001(3) S1 0.0114(10) 0.0177(10) 0.0252(12) 0.0047(8) -0.0014(8) 0.0003(8) C1 0.014(4) 0.015(4) 0.019(4) 0.001(3) 0.000(3) -0.002(3) N1 0.011(4) 0.010(3) 0.021(4) -0.001(2) 0.004(3) -0.002(2) C2 0.012(5) 0.014(4) 0.027(5) 0.002(3) 0.002(3) 0.000(3) O1 0.022(4) 0.026(4) 0.043(4) 0.000(3) -0.001(3) -0.002(3) C3 0.015(4) 0.018(4) 0.017(4) 0.004(3) 0.003(3) 0.004(3) O2 0.026(4) 0.033(4) 0.020(3) 0.008(3) -0.004(3) 0.006(3) C4 0.023(5) 0.013(4) 0.017(4) -0.003(3) -0.005(3) 0.008(3) C5 0.028(5) 0.014(4) 0.020(5) -0.003(3) 0.003(4) 0.006(3) C6 0.021(5) 0.016(4) 0.020(5) 0.002(3) 0.005(4) 0.005(3) C8 0.017(5) 0.010(4) 0.022(5) -0.004(3) -0.003(3) 0.001(3) C9 0.038(6) 0.022(4) 0.019(4) -0.001(4) -0.010(4) 0.005(4) C10 0.034(6) 0.034(5) 0.022(5) -0.002(4) 0.003(4) 0.003(4) C11 0.017(5) 0.022(4) 0.024(5) 0.000(3) 0.000(4) 0.006(3) C12 0.040(6) 0.015(4) 0.030(5) 0.006(4) 0.002(4) -0.004(4) C13 0.021(5) 0.025(5) 0.033(6) -0.007(4) 0.000(4) -0.003(4) C14 0.028(5) 0.013(4) 0.025(5) 0.005(3) 0.013(4) 0.002(3) C15 0.026(5) 0.028(5) 0.020(5) 0.003(4) 0.009(4) 0.003(4) C16 0.050(7) 0.040(6) 0.027(6) 0.012(5) 0.017(5) 0.029(5) C17 0.074(9) 0.024(6) 0.044(7) 0.022(5) 0.032(7) 0.019(6) C18 0.069(9) 0.009(5) 0.049(7) -0.004(4) 0.037(7) -0.007(5) C19 0.032(6) 0.021(5) 0.033(6) 0.003(4) 0.016(4) -0.007(4) C20 0.016(4) 0.005(3) 0.015(4) -0.003(3) -0.002(3) -0.004(3) Si1 0.0098(11) 0.0153(11) 0.0147(11) 0.0011(8) 0.0008(8) -0.0025(8) Si2 0.0165(12) 0.0111(10) 0.0186(12) 0.0024(8) -0.0014(9) -0.0003(8) Si3 0.0125(12) 0.0204(12) 0.0162(12) -0.0045(9) 0.0023(9) -0.0012(9) C21 0.016(5) 0.023(5) 0.020(5) 0.001(3) -0.001(3) -0.007(3) C22 0.014(5) 0.027(5) 0.019(5) 0.003(3) 0.000(3) -0.001(3) C23 0.020(5) 0.025(5) 0.014(4) 0.002(3) 0.004(3) 0.004(3) C24 0.016(5) 0.024(5) 0.031(5) 0.005(4) -0.005(4) 0.002(4) C25 0.037(6) 0.013(5) 0.037(6) 0.004(4) 0.002(4) 0.004(4) C26 0.024(5) 0.024(5) 0.017(4) 0.010(3) 0.000(4) -0.003(4) C27 0.026(5) 0.034(5) 0.021(5) -0.010(4) 0.005(4) -0.005(4) C28 0.026(6) 0.028(5) 0.036(6) -0.009(4) 0.009(4) 0.005(4) C29 0.025(5) 0.040(6) 0.015(4) 0.000(4) 0.010(4) -0.005(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 W1 C2 1.949(9) . ? W1 C3 1.966(9) . ? W1 N1 2.243(7) . ? W1 C6 2.272(8) . ? W1 C7 2.312(8) . ? W1 C5 2.319(9) . ? W1 C4 2.420(8) . ? W1 C8 2.428(8) . ? W1 Ge1 2.6364(8) . ? Ge1 C20 2.031(7) . ? Ge1 S1 2.343(2) . ? Ge1 H1 1.47(9) . ? S1 C1 1.715(8) . ? C1 N1 1.303(11) . ? C1 H2 0.9500 . ? N1 C14 1.447(11) . ? C2 O1 1.157(11) . ? C3 O2 1.162(10) . ? C4 C8 1.413(12) . ? C4 C5 1.442(13) . ? C4 C9 1.507(12) . ? C5 C6 1.438(12) . ? C5 C10 1.503(14) . ? C6 C7 1.426(12) . ? C6 C11 1.504(12) . ? C7 C8 1.470(12) . ? C7 C12 1.497(12) . ? C8 C13 1.508(13) . ? C9 H3 0.9800 . ? C9 H4 0.9800 . ? C9 H5 0.9800 . ? C10 H6 0.9800 . ? C10 H7 0.9800 . ? C10 H8 0.9800 . ? C11 H9 0.9800 . ? C11 H10 0.9800 . ? C11 H11 0.9800 . ? C12 H12 0.9800 . ? C12 H13 0.9800 . ? C12 H14 0.9800 . ? C13 H15 0.9800 . ? C13 H16 0.9800 . ? C13 H17 0.9800 . ? C14 C15 1.386(14) . ? C14 C19 1.399(13) . ? C15 C16 1.373(13) . ? C15 H18 0.9500 . ? C16 C17 1.365(18) . ? C16 H19 0.9500 . ? C17 C18 1.390(19) . ? C17 H20 0.9500 . ? C18 C19 1.385(14) . ? C18 H21 0.9500 . ? C19 H22 0.9500 . ? C20 Si3 1.900(8) . ? C20 Si2 1.901(8) . ? C20 Si1 1.913(8) . ? Si1 C23 1.878(9) . ? Si1 C22 1.880(9) . ? Si1 C21 1.882(9) . ? Si2 C26 1.869(9) . ? Si2 C24 1.870(9) . ? Si2 C25 1.887(9) . ? Si3 C29 1.873(10) . ? Si3 C28 1.881(10) . ? Si3 C27 1.893(10) . ? C21 H23 0.9800 . ? C21 H24 0.9800 . ? C21 H25 0.9800 . ? C22 H26 0.9800 . ? C22 H27 0.9800 . ? C22 H28 0.9800 . ? C23 H29 0.9800 . ? C23 H30 0.9800 . ? C23 H31 0.9800 . ? C24 H32 0.9800 . ? C24 H33 0.9800 . ? C24 H34 0.9800 . ? C25 H35 0.9800 . ? C25 H36 0.9800 . ? C25 H37 0.9800 . ? C26 H38 0.9800 . ? C26 H39 0.9800 . ? C26 H40 0.9800 . ? C27 H41 0.9800 . ? C27 H42 0.9800 . ? C27 H43 0.9800 . ? C28 H44 0.9800 . ? C28 H45 0.9800 . ? C28 H46 0.9800 . ? C29 H47 0.9800 . ? C29 H48 0.9800 . ? C29 H49 0.9800 . ? 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 C2 W1 C3 71.6(4) . . ? C2 W1 N1 134.9(3) . . ? C3 W1 N1 88.6(3) . . ? C2 W1 C6 89.1(3) . . ? C3 W1 C6 88.9(3) . . ? N1 W1 C6 131.7(3) . . ? C2 W1 C7 123.5(3) . . ? C3 W1 C7 89.7(3) . . ? N1 W1 C7 95.5(3) . . ? C6 W1 C7 36.2(3) . . ? C2 W1 C5 83.9(4) . . ? C3 W1 C5 120.8(3) . . ? N1 W1 C5 139.5(3) . . ? C6 W1 C5 36.5(3) . . ? C7 W1 C5 60.6(3) . . ? C2 W1 C4 113.8(3) . . ? C3 W1 C4 146.5(3) . . ? N1 W1 C4 105.0(3) . . ? C6 W1 C4 59.1(3) . . ? C7 W1 C4 59.1(3) . . ? C5 W1 C4 35.3(3) . . ? C2 W1 C8 142.2(3) . . ? C3 W1 C8 122.7(3) . . ? N1 W1 C8 82.7(3) . . ? C6 W1 C8 59.1(3) . . ? C7 W1 C8 36.0(3) . . ? C5 W1 C8 58.5(3) . . ? C4 W1 C8 33.9(3) . . ? C2 W1 Ge1 81.5(2) . . ? C3 W1 Ge1 126.7(3) . . ? N1 W1 Ge1 78.91(17) . . ? C6 W1 Ge1 136.7(2) . . ? C7 W1 Ge1 142.6(2) . . ? C5 W1 Ge1 100.3(2) . . ? C4 W1 Ge1 86.40(19) . . ? C8 W1 Ge1 106.9(2) . . ? C20 Ge1 S1 103.0(2) . . ? C20 Ge1 W1 140.8(2) . . ? S1 Ge1 W1 95.42(6) . . ? C20 Ge1 H1 98(3) . . ? S1 Ge1 H1 96(4) . . ? W1 Ge1 H1 114(3) . . ? C1 S1 Ge1 96.4(3) . . ? N1 C1 S1 127.8(7) . . ? N1 C1 H2 116.1 . . ? S1 C1 H2 116.1 . . ? C1 N1 C14 113.2(7) . . ? C1 N1 W1 125.1(6) . . ? C14 N1 W1 120.9(5) . . ? O1 C2 W1 170.4(7) . . ? O2 C3 W1 168.5(8) . . ? C8 C4 C5 108.8(7) . . ? C8 C4 C9 125.7(8) . . ? C5 C4 C9 124.8(9) . . ? C8 C4 W1 73.4(5) . . ? C5 C4 W1 68.5(5) . . ? C9 C4 W1 131.2(6) . . ? C6 C5 C4 107.2(8) . . ? C6 C5 C10 126.8(8) . . ? C4 C5 C10 125.5(8) . . ? C6 C5 W1 69.9(5) . . ? C4 C5 W1 76.1(5) . . ? C10 C5 W1 125.7(6) . . ? C7 C6 C5 109.3(8) . . ? C7 C6 C11 125.9(8) . . ? C5 C6 C11 124.5(8) . . ? C7 C6 W1 73.4(5) . . ? C5 C6 W1 73.6(5) . . ? C11 C6 W1 124.1(6) . . ? C6 C7 C8 106.6(7) . . ? C6 C7 C12 128.0(8) . . ? C8 C7 C12 124.6(8) . . ? C6 C7 W1 70.3(5) . . ? C8 C7 W1 76.3(5) . . ? C12 C7 W1 127.0(6) . . ? C4 C8 C7 108.1(7) . . ? C4 C8 C13 124.8(8) . . ? C7 C8 C13 126.7(8) . . ? C4 C8 W1 72.7(5) . . ? C7 C8 W1 67.7(4) . . ? C13 C8 W1 130.2(6) . . ? C4 C9 H3 109.5 . . ? C4 C9 H4 109.5 . . ? H3 C9 H4 109.5 . . ? C4 C9 H5 109.5 . . ? H3 C9 H5 109.5 . . ? H4 C9 H5 109.5 . . ? C5 C10 H6 109.5 . . ? C5 C10 H7 109.5 . . ? H6 C10 H7 109.5 . . ? C5 C10 H8 109.5 . . ? H6 C10 H8 109.5 . . ? H7 C10 H8 109.5 . . ? C6 C11 H9 109.5 . . ? C6 C11 H10 109.5 . . ? H9 C11 H10 109.5 . . ? C6 C11 H11 109.5 . . ? H9 C11 H11 109.5 . . ? H10 C11 H11 109.5 . . ? C7 C12 H12 109.5 . . ? C7 C12 H13 109.5 . . ? H12 C12 H13 109.5 . . ? C7 C12 H14 109.5 . . ? H12 C12 H14 109.5 . . ? H13 C12 H14 109.5 . . ? C8 C13 H15 109.5 . . ? C8 C13 H16 109.5 . . ? H15 C13 H16 109.5 . . ? C8 C13 H17 109.5 . . ? H15 C13 H17 109.5 . . ? H16 C13 H17 109.5 . . ? C15 C14 C19 118.3(9) . . ? C15 C14 N1 121.0(8) . . ? C19 C14 N1 120.7(9) . . ? C16 C15 C14 119.7(10) . . ? C16 C15 H18 120.2 . . ? C14 C15 H18 120.2 . . ? C17 C16 C15 122.5(12) . . ? C17 C16 H19 118.7 . . ? C15 C16 H19 118.7 . . ? C16 C17 C18 118.6(10) . . ? C16 C17 H20 120.7 . . ? C18 C17 H20 120.7 . . ? C19 C18 C17 119.7(11) . . ? C19 C18 H21 120.1 . . ? C17 C18 H21 120.1 . . ? C18 C19 C14 120.9(11) . . ? C18 C19 H22 119.5 . . ? C14 C19 H22 119.5 . . ? Si3 C20 Si2 111.8(4) . . ? Si3 C20 Si1 110.1(4) . . ? Si2 C20 Si1 110.6(4) . . ? Si3 C20 Ge1 112.4(4) . . ? Si2 C20 Ge1 107.2(4) . . ? Si1 C20 Ge1 104.5(4) . . ? C23 Si1 C22 109.2(4) . . ? C23 Si1 C21 104.6(4) . . ? C22 Si1 C21 105.4(4) . . ? C23 Si1 C20 111.3(4) . . ? C22 Si1 C20 111.9(4) . . ? C21 Si1 C20 113.9(4) . . ? C26 Si2 C24 105.3(4) . . ? C26 Si2 C25 105.2(4) . . ? C24 Si2 C25 104.6(4) . . ? C26 Si2 C20 114.4(4) . . ? C24 Si2 C20 113.6(4) . . ? C25 Si2 C20 112.7(4) . . ? C29 Si3 C28 106.3(5) . . ? C29 Si3 C27 106.4(4) . . ? C28 Si3 C27 102.4(4) . . ? C29 Si3 C20 112.6(4) . . ? C28 Si3 C20 115.2(4) . . ? C27 Si3 C20 112.9(4) . . ? Si1 C21 H23 109.5 . . ? Si1 C21 H24 109.5 . . ? H23 C21 H24 109.5 . . ? Si1 C21 H25 109.5 . . ? H23 C21 H25 109.5 . . ? H24 C21 H25 109.5 . . ? Si1 C22 H26 109.5 . . ? Si1 C22 H27 109.5 . . ? H26 C22 H27 109.5 . . ? Si1 C22 H28 109.5 . . ? H26 C22 H28 109.5 . . ? H27 C22 H28 109.5 . . ? Si1 C23 H29 109.5 . . ? Si1 C23 H30 109.5 . . ? H29 C23 H30 109.5 . . ? Si1 C23 H31 109.5 . . ? H29 C23 H31 109.5 . . ? H30 C23 H31 109.5 . . ? Si2 C24 H32 109.5 . . ? Si2 C24 H33 109.5 . . ? H32 C24 H33 109.5 . . ? Si2 C24 H34 109.5 . . ? H32 C24 H34 109.5 . . ? H33 C24 H34 109.5 . . ? Si2 C25 H35 109.5 . . ? Si2 C25 H36 109.5 . . ? H35 C25 H36 109.5 . . ? Si2 C25 H37 109.5 . . ? H35 C25 H37 109.5 . . ? H36 C25 H37 109.5 . . ? Si2 C26 H38 109.5 . . ? Si2 C26 H39 109.5 . . ? H38 C26 H39 109.5 . . ? Si2 C26 H40 109.5 . . ? H38 C26 H40 109.5 . . ? H39 C26 H40 109.5 . . ? Si3 C27 H41 109.5 . . ? Si3 C27 H42 109.5 . . ? H41 C27 H42 109.5 . . ? Si3 C27 H43 109.5 . . ? H41 C27 H43 109.5 . . ? H42 C27 H43 109.5 . . ? Si3 C28 H44 109.5 . . ? Si3 C28 H45 109.5 . . ? H44 C28 H45 109.5 . . ? Si3 C28 H46 109.5 . . ? H44 C28 H46 109.5 . . ? H45 C28 H46 109.5 . . ? Si3 C29 H47 109.5 . . ? Si3 C29 H48 109.5 . . ? H47 C29 H48 109.5 . . ? Si3 C29 H49 109.5 . . ? H47 C29 H49 109.5 . . ? H48 C29 H49 109.5 . . ? 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 C2 W1 Ge1 C20 -51.8(5) . . . . ? C3 W1 Ge1 C20 7.6(5) . . . . ? N1 W1 Ge1 C20 87.3(4) . . . . ? C6 W1 Ge1 C20 -131.4(5) . . . . ? C7 W1 Ge1 C20 171.9(5) . . . . ? C5 W1 Ge1 C20 -134.0(4) . . . . ? C4 W1 Ge1 C20 -166.6(4) . . . . ? C8 W1 Ge1 C20 166.1(4) . . . . ? C2 W1 Ge1 S1 -170.2(3) . . . . ? C3 W1 Ge1 S1 -110.8(3) . . . . ? N1 W1 Ge1 S1 -31.07(19) . . . . ? C6 W1 Ge1 S1 110.3(3) . . . . ? C7 W1 Ge1 S1 53.5(3) . . . . ? C5 W1 Ge1 S1 107.7(2) . . . . ? C4 W1 Ge1 S1 75.0(2) . . . . ? C8 W1 Ge1 S1 47.7(2) . . . . ? C20 Ge1 S1 C1 -111.6(4) . . . . ? W1 Ge1 S1 C1 33.6(3) . . . . ? Ge1 S1 C1 N1 -20.8(8) . . . . ? S1 C1 N1 C14 179.0(6) . . . . ? S1 C1 N1 W1 -11.1(11) . . . . ? C2 W1 N1 C1 97.9(8) . . . . ? C3 W1 N1 C1 159.9(7) . . . . ? C6 W1 N1 C1 -113.0(7) . . . . ? C7 W1 N1 C1 -110.6(7) . . . . ? C5 W1 N1 C1 -60.9(8) . . . . ? C4 W1 N1 C1 -51.2(7) . . . . ? C8 W1 N1 C1 -76.9(7) . . . . ? Ge1 W1 N1 C1 32.0(6) . . . . ? C2 W1 N1 C14 -93.0(7) . . . . ? C3 W1 N1 C14 -31.0(7) . . . . ? C6 W1 N1 C14 56.1(8) . . . . ? C7 W1 N1 C14 58.5(6) . . . . ? C5 W1 N1 C14 108.2(7) . . . . ? C4 W1 N1 C14 117.9(6) . . . . ? C8 W1 N1 C14 92.2(6) . . . . ? Ge1 W1 N1 C14 -158.9(6) . . . . ? C3 W1 C2 O1 58(5) . . . . ? N1 W1 C2 O1 127(5) . . . . ? C6 W1 C2 O1 -31(5) . . . . ? C7 W1 C2 O1 -19(5) . . . . ? C5 W1 C2 O1 -67(5) . . . . ? C4 W1 C2 O1 -86(5) . . . . ? C8 W1 C2 O1 -62(5) . . . . ? Ge1 W1 C2 O1 -168(5) . . . . ? C2 W1 C3 O2 -55(4) . . . . ? N1 W1 C3 O2 166(4) . . . . ? C6 W1 C3 O2 34(4) . . . . ? C7 W1 C3 O2 70(4) . . . . ? C5 W1 C3 O2 15(4) . . . . ? C4 W1 C3 O2 50(4) . . . . ? C8 W1 C3 O2 85(4) . . . . ? Ge1 W1 C3 O2 -119(4) . . . . ? C2 W1 C4 C8 153.0(5) . . . . ? C3 W1 C4 C8 60.5(8) . . . . ? N1 W1 C4 C8 -50.5(5) . . . . ? C6 W1 C4 C8 79.5(5) . . . . ? C7 W1 C4 C8 37.0(5) . . . . ? C5 W1 C4 C8 118.6(7) . . . . ? Ge1 W1 C4 C8 -128.0(5) . . . . ? C2 W1 C4 C5 34.4(6) . . . . ? C3 W1 C4 C5 -58.1(8) . . . . ? N1 W1 C4 C5 -169.1(5) . . . . ? C6 W1 C4 C5 -39.1(5) . . . . ? C7 W1 C4 C5 -81.6(5) . . . . ? C8 W1 C4 C5 -118.6(7) . . . . ? Ge1 W1 C4 C5 113.4(5) . . . . ? C2 W1 C4 C9 -83.7(9) . . . . ? C3 W1 C4 C9 -176.2(8) . . . . ? N1 W1 C4 C9 72.8(9) . . . . ? C6 W1 C4 C9 -157.2(10) . . . . ? C7 W1 C4 C9 160.3(10) . . . . ? C5 W1 C4 C9 -118.1(11) . . . . ? C8 W1 C4 C9 123.3(11) . . . . ? Ge1 W1 C4 C9 -4.7(9) . . . . ? C8 C4 C5 C6 0.8(10) . . . . ? C9 C4 C5 C6 -170.4(8) . . . . ? W1 C4 C5 C6 63.5(6) . . . . ? C8 C4 C5 C10 173.1(8) . . . . ? C9 C4 C5 C10 1.9(14) . . . . ? W1 C4 C5 C10 -124.2(9) . . . . ? C8 C4 C5 W1 -62.7(6) . . . . ? C9 C4 C5 W1 126.1(8) . . . . ? C2 W1 C5 C6 96.9(6) . . . . ? C3 W1 C5 C6 32.5(7) . . . . ? N1 W1 C5 C6 -98.1(6) . . . . ? C7 W1 C5 C6 -37.4(5) . . . . ? C4 W1 C5 C6 -114.4(8) . . . . ? C8 W1 C5 C6 -79.4(6) . . . . ? Ge1 W1 C5 C6 177.0(5) . . . . ? C2 W1 C5 C4 -148.7(5) . . . . ? C3 W1 C5 C4 147.0(5) . . . . ? N1 W1 C5 C4 16.3(7) . . . . ? C6 W1 C5 C4 114.4(8) . . . . ? C7 W1 C5 C4 77.1(5) . . . . ? C8 W1 C5 C4 35.1(5) . . . . ? Ge1 W1 C5 C4 -68.5(5) . . . . ? C2 W1 C5 C10 -24.6(8) . . . . ? C3 W1 C5 C10 -89.0(8) . . . . ? N1 W1 C5 C10 140.4(7) . . . . ? C6 W1 C5 C10 -121.5(10) . . . . ? C7 W1 C5 C10 -158.9(9) . . . . ? C4 W1 C5 C10 124.1(10) . . . . ? C8 W1 C5 C10 159.1(9) . . . . ? Ge1 W1 C5 C10 55.5(8) . . . . ? C4 C5 C6 C7 -2.4(10) . . . . ? C10 C5 C6 C7 -174.6(8) . . . . ? W1 C5 C6 C7 65.3(6) . . . . ? C4 C5 C6 C11 171.9(8) . . . . ? C10 C5 C6 C11 -0.3(14) . . . . ? W1 C5 C6 C11 -120.4(9) . . . . ? C4 C5 C6 W1 -67.7(6) . . . . ? C10 C5 C6 W1 120.1(9) . . . . ? C2 W1 C6 C7 162.6(5) . . . . ? C3 W1 C6 C7 91.0(5) . . . . ? N1 W1 C6 C7 3.9(7) . . . . ? C5 W1 C6 C7 -116.5(8) . . . . ? C4 W1 C6 C7 -78.7(5) . . . . ? C8 W1 C6 C7 -39.0(5) . . . . ? Ge1 W1 C6 C7 -120.8(4) . . . . ? C2 W1 C6 C5 -80.8(6) . . . . ? C3 W1 C6 C5 -152.5(6) . . . . ? N1 W1 C6 C5 120.5(5) . . . . ? C7 W1 C6 C5 116.5(8) . . . . ? C4 W1 C6 C5 37.9(5) . . . . ? C8 W1 C6 C5 77.6(6) . . . . ? Ge1 W1 C6 C5 -4.3(7) . . . . ? C2 W1 C6 C11 40.1(7) . . . . ? C3 W1 C6 C11 -31.6(7) . . . . ? N1 W1 C6 C11 -118.6(7) . . . . ? C7 W1 C6 C11 -122.5(9) . . . . ? C5 W1 C6 C11 120.9(10) . . . . ? C4 W1 C6 C11 158.8(8) . . . . ? C8 W1 C6 C11 -161.5(8) . . . . ? Ge1 W1 C6 C11 116.6(7) . . . . ? C5 C6 C7 C8 3.0(9) . . . . ? C11 C6 C7 C8 -171.2(8) . . . . ? W1 C6 C7 C8 68.4(6) . . . . ? C5 C6 C7 C12 172.5(8) . . . . ? C11 C6 C7 C12 -1.7(15) . . . . ? W1 C6 C7 C12 -122.2(9) . . . . ? C5 C6 C7 W1 -65.4(6) . . . . ? C11 C6 C7 W1 120.4(9) . . . . ? C2 W1 C7 C6 -21.0(6) . . . . ? C3 W1 C7 C6 -88.5(5) . . . . ? N1 W1 C7 C6 -177.1(5) . . . . ? C5 W1 C7 C6 37.7(5) . . . . ? C4 W1 C7 C6 78.7(5) . . . . ? C8 W1 C7 C6 113.5(7) . . . . ? Ge1 W1 C7 C6 104.0(5) . . . . ? C2 W1 C7 C8 -134.5(5) . . . . ? C3 W1 C7 C8 158.0(5) . . . . ? N1 W1 C7 C8 69.5(5) . . . . ? C6 W1 C7 C8 -113.5(7) . . . . ? C5 W1 C7 C8 -75.8(5) . . . . ? C4 W1 C7 C8 -34.8(5) . . . . ? Ge1 W1 C7 C8 -9.5(7) . . . . ? C2 W1 C7 C12 102.3(8) . . . . ? C3 W1 C7 C12 34.8(8) . . . . ? N1 W1 C7 C12 -53.7(8) . . . . ? C6 W1 C7 C12 123.3(10) . . . . ? C5 W1 C7 C12 161.0(9) . . . . ? C4 W1 C7 C12 -158.0(9) . . . . ? C8 W1 C7 C12 -123.2(10) . . . . ? Ge1 W1 C7 C12 -132.7(7) . . . . ? C5 C4 C8 C7 1.1(9) . . . . ? C9 C4 C8 C7 172.1(8) . . . . ? W1 C4 C8 C7 -58.6(5) . . . . ? C5 C4 C8 C13 -173.0(8) . . . . ? C9 C4 C8 C13 -1.9(14) . . . . ? W1 C4 C8 C13 127.4(8) . . . . ? C5 C4 C8 W1 59.7(6) . . . . ? C9 C4 C8 W1 -129.2(8) . . . . ? C6 C7 C8 C4 -2.5(9) . . . . ? C12 C7 C8 C4 -172.4(8) . . . . ? W1 C7 C8 C4 61.8(6) . . . . ? C6 C7 C8 C13 171.4(8) . . . . ? C12 C7 C8 C13 1.5(13) . . . . ? W1 C7 C8 C13 -124.3(8) . . . . ? C6 C7 C8 W1 -64.3(6) . . . . ? C12 C7 C8 W1 125.8(9) . . . . ? C2 W1 C8 C4 -42.6(7) . . . . ? C3 W1 C8 C4 -145.2(5) . . . . ? N1 W1 C8 C4 131.3(5) . . . . ? C6 W1 C8 C4 -79.5(5) . . . . ? C7 W1 C8 C4 -118.7(7) . . . . ? C5 W1 C8 C4 -36.6(5) . . . . ? Ge1 W1 C8 C4 55.3(5) . . . . ? C2 W1 C8 C7 76.1(7) . . . . ? C3 W1 C8 C7 -26.5(6) . . . . ? N1 W1 C8 C7 -110.0(5) . . . . ? C6 W1 C8 C7 39.2(5) . . . . ? C5 W1 C8 C7 82.1(5) . . . . ? C4 W1 C8 C7 118.7(7) . . . . ? Ge1 W1 C8 C7 174.0(4) . . . . ? C2 W1 C8 C13 -164.0(8) . . . . ? C3 W1 C8 C13 93.5(8) . . . . ? N1 W1 C8 C13 9.9(8) . . . . ? C6 W1 C8 C13 159.1(9) . . . . ? C7 W1 C8 C13 119.9(10) . . . . ? C5 W1 C8 C13 -157.9(9) . . . . ? C4 W1 C8 C13 -121.4(10) . . . . ? Ge1 W1 C8 C13 -66.1(8) . . . . ? C1 N1 C14 C15 -125.2(9) . . . . ? W1 N1 C14 C15 64.4(10) . . . . ? C1 N1 C14 C19 51.8(11) . . . . ? W1 N1 C14 C19 -118.5(8) . . . . ? C19 C14 C15 C16 5.0(14) . . . . ? N1 C14 C15 C16 -177.9(8) . . . . ? C14 C15 C16 C17 -2.2(15) . . . . ? C15 C16 C17 C18 -1.6(16) . . . . ? C16 C17 C18 C19 2.6(16) . . . . ? C17 C18 C19 C14 0.3(15) . . . . ? C15 C14 C19 C18 -4.1(14) . . . . ? N1 C14 C19 C18 178.8(8) . . . . ? S1 Ge1 C20 Si3 49.3(4) . . . . ? W1 Ge1 C20 Si3 -66.6(6) . . . . ? S1 Ge1 C20 Si2 -73.9(4) . . . . ? W1 Ge1 C20 Si2 170.11(12) . . . . ? S1 Ge1 C20 Si1 168.7(3) . . . . ? W1 Ge1 C20 Si1 52.8(5) . . . . ? Si3 C20 Si1 C23 166.2(4) . . . . ? Si2 C20 Si1 C23 -69.7(5) . . . . ? Ge1 C20 Si1 C23 45.3(5) . . . . ? Si3 C20 Si1 C22 43.7(5) . . . . ? Si2 C20 Si1 C22 167.8(4) . . . . ? Ge1 C20 Si1 C22 -77.2(5) . . . . ? Si3 C20 Si1 C21 -75.8(5) . . . . ? Si2 C20 Si1 C21 48.3(5) . . . . ? Ge1 C20 Si1 C21 163.3(4) . . . . ? Si3 C20 Si2 C26 165.1(4) . . . . ? Si1 C20 Si2 C26 42.0(5) . . . . ? Ge1 C20 Si2 C26 -71.3(5) . . . . ? Si3 C20 Si2 C24 -73.9(5) . . . . ? Si1 C20 Si2 C24 162.9(4) . . . . ? Ge1 C20 Si2 C24 49.7(5) . . . . ? Si3 C20 Si2 C25 44.9(6) . . . . ? Si1 C20 Si2 C25 -78.2(5) . . . . ? Ge1 C20 Si2 C25 168.5(4) . . . . ? Si2 C20 Si3 C29 158.2(4) . . . . ? Si1 C20 Si3 C29 -78.5(5) . . . . ? Ge1 C20 Si3 C29 37.6(6) . . . . ? Si2 C20 Si3 C28 36.0(6) . . . . ? Si1 C20 Si3 C28 159.3(4) . . . . ? Ge1 C20 Si3 C28 -84.6(5) . . . . ? Si2 C20 Si3 C27 -81.2(5) . . . . ? Si1 C20 Si3 C27 42.1(6) . . . . ? Ge1 C20 Si3 C27 158.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.115 _refine_diff_density_min -2.884 _refine_diff_density_rms 0.294