# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) the Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_author_address ; Department of Chemistry, Graduate School of Science Tohoku University Sendai 980-8578 JAPAN ; _publ_contact_author_name 'Professor Hiromi Tobita' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science Tohoku University Sendai 980-8578 JAPAN ; _publ_contact_author_email tobita@m.tohoku.ac.jp _publ_section_title ; Synthesis and characterisation of hydrido molybdenum and tungsten complexes having a hemilabile tridentate Si,Si,O-ligand and their two-step reaction with nitriles: observation of stepwise hydrosilylation of nitrile to form N-silylimine on the metal centre ; loop_ _publ_author_name 'Takashi Komuro' 'Rockshana Begum' 'Rikima Ono' 'Hiromi Tobita' data_compound-1a #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 789738' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 Mo O3 Si2' _chemical_formula_sum 'C31 H40 Mo O3 Si2' _chemical_formula_weight 612.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.0607(3) _cell_length_b 8.3977(4) _cell_length_c 17.5907(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.1177(7) _cell_angle_gamma 90.00 _cell_volume 1480.26(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10950 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.554 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.912503 _exptl_absorpt_correction_T_max 0.987242 _exptl_absorpt_process_details ; HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera. Rigaku Corporation, Tokyo, Japan. HIGASHI, T. (1999). Numabs - Numerical Absorption Correction, Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _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 13385 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 6606 _reflns_number_gt 6134 _reflns_threshold_expression >2\s(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+2.3734P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 6606 _refine_ls_number_parameters 349 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.196 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.657 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.146 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 Mo1 Mo 0.17920(3) 0.49951(4) 0.842921(19) 0.01249(9) Uani 1 1 d . . . Si1 Si 0.41259(12) 0.45896(14) 0.78342(7) 0.0160(3) Uani 1 1 d . . . H1 H 0.229(7) 0.496(14) 0.747(4) 0.08(2) Uiso 1 1 d . . . Si2 Si 0.03307(13) 0.45134(15) 0.70985(7) 0.0151(3) Uani 1 1 d . . . O1 O -0.0106(4) 0.2090(5) 0.8513(2) 0.0293(9) Uani 1 1 d . . . O2 O 0.3335(4) 0.2135(5) 0.9202(2) 0.0289(9) Uani 1 1 d . . . O3 O 0.2683(3) 0.5879(4) 0.63662(19) 0.0146(7) Uani 1 1 d . . . C1 C 0.0591(5) 0.3170(7) 0.8441(3) 0.0189(11) Uani 1 1 d . . . C2 C 0.2815(5) 0.3194(7) 0.8892(3) 0.0191(11) Uani 1 1 d . . . C3 C 0.4279(6) 0.2781(7) 0.7217(4) 0.0292(13) Uani 1 1 d . . . H2 H 0.3697 0.2901 0.6744 0.044 Uiso 1 1 calc R . . H3 H 0.4014 0.1832 0.7491 0.044 Uiso 1 1 calc R . . H4 H 0.5206 0.2667 0.7096 0.044 Uiso 1 1 calc R . . C4 C 0.5569(5) 0.4399(7) 0.8598(3) 0.0275(12) Uani 1 1 d . . . H5 H 0.5463 0.3425 0.8894 0.041 Uiso 1 1 calc R . . H6 H 0.5580 0.5324 0.8939 0.041 Uiso 1 1 calc R . . H7 H 0.6410 0.4351 0.8358 0.041 Uiso 1 1 calc R . . C5 C 0.4581(5) 0.6361(6) 0.7237(3) 0.0173(10) Uani 1 1 d . . . C6 C 0.5691(5) 0.7327(6) 0.7440(3) 0.0207(10) Uani 1 1 d . . . H8 H 0.6258 0.7075 0.7884 0.025 Uiso 1 1 calc R . . C7 C 0.5984(5) 0.8649(6) 0.7005(3) 0.0225(11) Uani 1 1 d . . . H9 H 0.6748 0.9278 0.7152 0.027 Uiso 1 1 calc R . . C8 C 0.5160(5) 0.9049(6) 0.6356(3) 0.0214(10) Uani 1 1 d . . . H10 H 0.5359 0.9964 0.6070 0.026 Uiso 1 1 calc R . . C9 C 0.4048(5) 0.8129(6) 0.6120(3) 0.0167(10) Uani 1 1 d . . . C10 C 0.3810(4) 0.6814(6) 0.6573(3) 0.0139(9) Uani 1 1 d . . . C11 C 0.3067(5) 0.8460(6) 0.5431(3) 0.0180(10) Uani 1 1 d . . . C12 C 0.3352(6) 0.7281(6) 0.4789(3) 0.0235(11) Uani 1 1 d . . . H11 H 0.4247 0.7481 0.4631 0.035 Uiso 1 1 calc R . . H12 H 0.2689 0.7430 0.4352 0.035 Uiso 1 1 calc R . . H13 H 0.3302 0.6187 0.4978 0.035 Uiso 1 1 calc R . . C13 C 0.3187(5) 1.0158(8) 0.5132(3) 0.0229(10) Uani 1 1 d . . . H14 H 0.3050 1.0917 0.5541 0.034 Uiso 1 1 calc R . . H15 H 0.2510 1.0333 0.4704 0.034 Uiso 1 1 calc R . . H16 H 0.4077 1.0313 0.4959 0.034 Uiso 1 1 calc R . . C14 C 0.1542(5) 0.6786(6) 0.6145(3) 0.0152(9) Uani 1 1 d . . . C15 C 0.1675(5) 0.8108(6) 0.5683(3) 0.0174(9) Uani 1 1 d . . . C16 C 0.0532(5) 0.9007(6) 0.5480(3) 0.0194(10) Uani 1 1 d . . . H17 H 0.0578 0.9921 0.5165 0.023 Uiso 1 1 calc R . . C17 C -0.0689(5) 0.8547(6) 0.5745(3) 0.0215(10) Uani 1 1 d . . . H18 H -0.1473 0.9145 0.5600 0.026 Uiso 1 1 calc R . . C18 C -0.0761(5) 0.7239(6) 0.6213(3) 0.0183(10) Uani 1 1 d . . . H19 H -0.1597 0.6961 0.6387 0.022 Uiso 1 1 calc R . . C19 C 0.0366(5) 0.6302(6) 0.6440(3) 0.0157(9) Uani 1 1 d . . . C20 C -0.1510(5) 0.4240(7) 0.7222(3) 0.0232(11) Uani 1 1 d . . . H20 H -0.2014 0.4199 0.6719 0.035 Uiso 1 1 calc R . . H21 H -0.1827 0.5137 0.7513 0.035 Uiso 1 1 calc R . . H22 H -0.1640 0.3245 0.7496 0.035 Uiso 1 1 calc R . . C21 C 0.0778(6) 0.2719(6) 0.6542(3) 0.0250(11) Uani 1 1 d . . . H23 H 0.0099 0.2552 0.6114 0.037 Uiso 1 1 calc R . . H24 H 0.0820 0.1781 0.6875 0.037 Uiso 1 1 calc R . . H25 H 0.1648 0.2886 0.6345 0.037 Uiso 1 1 calc R . . C22 C 0.1755(5) 0.7836(6) 0.8501(3) 0.0166(9) Uani 1 1 d . . . C23 C 0.2687(5) 0.7281(6) 0.9100(3) 0.0170(10) Uani 1 1 d . . . C24 C 0.1973(5) 0.6337(6) 0.9603(3) 0.0193(10) Uani 1 1 d . . . C25 C 0.0599(5) 0.6326(6) 0.9314(3) 0.0198(10) Uani 1 1 d . . . C26 C 0.0467(5) 0.7278(7) 0.8638(3) 0.0201(11) Uani 1 1 d . . . C27 C 0.2044(6) 0.9018(6) 0.7888(3) 0.0238(11) Uani 1 1 d . . . H26 H 0.1402 0.8870 0.7441 0.036 Uiso 1 1 calc R . . H27 H 0.2951 0.8847 0.7742 0.036 Uiso 1 1 calc R . . H28 H 0.1968 1.0103 0.8084 0.036 Uiso 1 1 calc R . . C28 C 0.4081(6) 0.7911(7) 0.9264(3) 0.0259(12) Uani 1 1 d . . . H29 H 0.4495 0.8034 0.8784 0.039 Uiso 1 1 calc R . . H30 H 0.4606 0.7162 0.9596 0.039 Uiso 1 1 calc R . . H31 H 0.4050 0.8946 0.9519 0.039 Uiso 1 1 calc R . . C29 C 0.2545(6) 0.5625(7) 1.0343(3) 0.0263(12) Uani 1 1 d . . . H32 H 0.2470 0.6392 1.0756 0.039 Uiso 1 1 calc R . . H33 H 0.3486 0.5362 1.0308 0.039 Uiso 1 1 calc R . . H34 H 0.2051 0.4655 1.0447 0.039 Uiso 1 1 calc R . . C30 C -0.0537(6) 0.5601(7) 0.9702(3) 0.0304(13) Uani 1 1 d . . . H35 H -0.0214 0.4666 0.9997 0.046 Uiso 1 1 calc R . . H36 H -0.1249 0.5279 0.9316 0.046 Uiso 1 1 calc R . . H37 H -0.0885 0.6386 1.0046 0.046 Uiso 1 1 calc R . . C31 C -0.0822(6) 0.7869(7) 0.8239(3) 0.0276(12) Uani 1 1 d . . . H38 H -0.1005 0.8945 0.8420 0.041 Uiso 1 1 calc R . . H39 H -0.1550 0.7155 0.8351 0.041 Uiso 1 1 calc R . . H40 H -0.0750 0.7895 0.7687 0.041 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 Mo1 0.01267(15) 0.01376(16) 0.01115(15) -0.00081(18) 0.00171(10) -0.00009(19) Si1 0.0139(5) 0.0174(7) 0.0169(6) 0.0050(4) 0.0020(4) 0.0039(4) Si2 0.0153(6) 0.0157(6) 0.0144(6) -0.0027(4) 0.0015(5) -0.0022(4) O1 0.029(2) 0.028(2) 0.031(2) 0.0048(17) 0.0026(18) -0.0103(18) O2 0.029(2) 0.024(2) 0.033(2) 0.0096(17) 0.0003(18) 0.0003(18) O3 0.0142(16) 0.0123(16) 0.0172(17) 0.0015(12) 0.0000(13) 0.0025(13) C1 0.021(3) 0.024(3) 0.012(3) 0.000(2) 0.0027(19) -0.001(2) C2 0.021(3) 0.023(3) 0.013(3) 0.006(2) 0.003(2) -0.005(2) C3 0.028(3) 0.026(3) 0.036(3) 0.002(2) 0.013(2) 0.009(2) C4 0.014(2) 0.042(3) 0.027(3) 0.009(2) 0.0012(19) 0.004(2) C5 0.015(2) 0.019(3) 0.019(2) 0.0019(19) 0.0076(18) 0.003(2) C6 0.014(2) 0.026(3) 0.022(3) 0.006(2) -0.0016(19) 0.003(2) C7 0.018(2) 0.021(3) 0.029(3) 0.005(2) 0.004(2) 0.001(2) C8 0.021(2) 0.016(2) 0.028(3) 0.002(2) 0.006(2) -0.005(2) C9 0.017(2) 0.019(2) 0.014(2) 0.0011(18) 0.0031(18) 0.0032(19) C10 0.0090(19) 0.015(2) 0.017(2) 0.0002(17) 0.0024(16) 0.0012(17) C11 0.022(2) 0.016(2) 0.016(2) 0.0015(18) 0.0047(19) 0.0013(19) C12 0.033(3) 0.024(3) 0.014(2) -0.002(2) 0.003(2) 0.004(2) C13 0.026(2) 0.021(3) 0.021(2) 0.007(2) 0.0012(17) 0.002(2) C14 0.014(2) 0.017(2) 0.014(2) -0.0010(17) -0.0015(17) 0.0029(18) C15 0.021(2) 0.016(2) 0.016(2) -0.0006(18) 0.0013(18) 0.0016(19) C16 0.024(2) 0.020(2) 0.014(2) -0.0023(18) -0.0040(19) 0.003(2) C17 0.021(2) 0.024(3) 0.019(2) -0.0003(19) -0.0031(19) 0.004(2) C18 0.014(2) 0.021(2) 0.019(2) -0.0058(19) -0.0009(18) 0.0027(19) C19 0.020(2) 0.015(2) 0.012(2) -0.0013(18) 0.0016(17) 0.0017(19) C20 0.018(2) 0.031(3) 0.021(3) 0.000(2) 0.0008(19) -0.009(2) C21 0.035(3) 0.020(3) 0.019(3) -0.003(2) -0.004(2) 0.000(2) C22 0.022(2) 0.017(2) 0.012(2) -0.0024(17) 0.0028(18) 0.0028(19) C23 0.020(3) 0.017(3) 0.015(3) -0.0070(19) 0.004(2) -0.001(2) C24 0.022(2) 0.021(3) 0.014(2) -0.0050(19) -0.0004(19) -0.003(2) C25 0.020(2) 0.022(3) 0.017(2) -0.004(2) 0.0049(19) 0.001(2) C26 0.017(2) 0.022(3) 0.021(3) -0.011(2) 0.001(2) 0.007(2) C27 0.032(3) 0.020(2) 0.018(2) 0.001(2) 0.002(2) 0.002(2) C28 0.022(3) 0.029(3) 0.025(3) -0.006(2) -0.005(2) -0.008(2) C29 0.035(3) 0.033(3) 0.011(2) 0.000(2) 0.001(2) 0.002(2) C30 0.028(3) 0.039(3) 0.027(3) -0.010(2) 0.014(2) -0.009(2) C31 0.020(3) 0.033(3) 0.028(3) -0.013(2) -0.004(2) 0.008(2) _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 Mo1 C1 1.953(6) . ? Mo1 C2 1.965(6) . ? Mo1 C25 2.334(5) . ? Mo1 C24 2.345(5) . ? Mo1 C26 2.382(5) . ? Mo1 C23 2.387(5) . ? Mo1 C22 2.389(5) . ? Mo1 Si1 2.6765(13) . ? Mo1 Si2 2.6815(13) . ? Mo1 H1 1.80(8) . ? Si1 C3 1.881(6) . ? Si1 C4 1.895(5) . ? Si1 C5 1.900(5) . ? Si1 H1 1.93(8) . ? Si2 C21 1.874(5) . ? Si2 C20 1.897(5) . ? Si2 C19 1.899(5) . ? O1 C1 1.160(7) . ? O2 C2 1.145(7) . ? O3 C10 1.401(6) . ? O3 C14 1.403(5) . ? C3 H2 0.9800 . ? C3 H3 0.9800 . ? C3 H4 0.9800 . ? C4 H5 0.9800 . ? C4 H6 0.9800 . ? C4 H7 0.9800 . ? C5 C10 1.396(7) . ? C5 C6 1.400(7) . ? C6 C7 1.395(7) . ? C6 H8 0.9500 . ? C7 C8 1.389(8) . ? C7 H9 0.9500 . ? C8 C9 1.393(7) . ? C8 H10 0.9500 . ? C9 C10 1.394(7) . ? C9 C11 1.518(7) . ? C11 C13 1.529(8) . ? C11 C15 1.534(7) . ? C11 C12 1.548(7) . ? C12 H11 0.9800 . ? C12 H12 0.9800 . ? C12 H13 0.9800 . ? C13 H14 0.9800 . ? C13 H15 0.9800 . ? C13 H16 0.9800 . ? C14 C15 1.389(7) . ? C14 C19 1.394(7) . ? C15 C16 1.395(7) . ? C16 C17 1.406(7) . ? C16 H17 0.9500 . ? C17 C18 1.379(7) . ? C17 H18 0.9500 . ? C18 C19 1.408(7) . ? C18 H19 0.9500 . ? C20 H20 0.9800 . ? C20 H21 0.9800 . ? C20 H22 0.9800 . ? C21 H23 0.9800 . ? C21 H24 0.9800 . ? C21 H25 0.9800 . ? C22 C26 1.419(7) . ? C22 C23 1.425(7) . ? C22 C27 1.513(7) . ? C23 C24 1.429(7) . ? C23 C28 1.502(7) . ? C24 C25 1.429(7) . ? C24 C29 1.500(7) . ? C25 C26 1.429(8) . ? C25 C30 1.511(7) . ? C26 C31 1.502(7) . ? C27 H26 0.9800 . ? C27 H27 0.9800 . ? C27 H28 0.9800 . ? C28 H29 0.9800 . ? C28 H30 0.9800 . ? C28 H31 0.9800 . ? C29 H32 0.9800 . ? C29 H33 0.9800 . ? C29 H34 0.9800 . ? C30 H35 0.9800 . ? C30 H36 0.9800 . ? C30 H37 0.9800 . ? C31 H38 0.9800 . ? C31 H39 0.9800 . ? C31 H40 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 C1 Mo1 C2 72.2(2) . . ? C1 Mo1 C25 90.8(2) . . ? C2 Mo1 C25 111.9(2) . . ? C1 Mo1 C24 111.56(19) . . ? C2 Mo1 C24 90.5(2) . . ? C25 Mo1 C24 35.58(17) . . ? C1 Mo1 C26 105.9(2) . . ? C2 Mo1 C26 146.6(2) . . ? C25 Mo1 C26 35.3(2) . . ? C24 Mo1 C26 58.53(18) . . ? C1 Mo1 C23 146.4(2) . . ? C2 Mo1 C23 104.68(19) . . ? C25 Mo1 C23 58.60(18) . . ? C24 Mo1 C23 35.14(18) . . ? C26 Mo1 C23 57.88(18) . . ? C1 Mo1 C22 140.4(2) . . ? C2 Mo1 C22 139.2(2) . . ? C25 Mo1 C22 58.35(17) . . ? C24 Mo1 C22 58.28(17) . . ? C26 Mo1 C22 34.60(18) . . ? C23 Mo1 C22 34.72(17) . . ? C1 Mo1 Si1 118.01(16) . . ? C2 Mo1 Si1 67.59(16) . . ? C25 Mo1 Si1 147.46(13) . . ? C24 Mo1 Si1 113.79(13) . . ? C26 Mo1 Si1 133.26(15) . . ? C23 Mo1 Si1 89.43(13) . . ? C22 Mo1 Si1 99.55(12) . . ? C1 Mo1 Si2 66.37(16) . . ? C2 Mo1 Si2 118.17(16) . . ? C25 Mo1 Si2 112.34(13) . . ? C24 Mo1 Si2 146.57(13) . . ? C26 Mo1 Si2 89.15(14) . . ? C23 Mo1 Si2 134.90(13) . . ? C22 Mo1 Si2 100.75(12) . . ? Si1 Mo1 Si2 94.08(4) . . ? C1 Mo1 H1 103(3) . . ? C2 Mo1 H1 101(3) . . ? C25 Mo1 H1 147(3) . . ? C24 Mo1 H1 146(3) . . ? C26 Mo1 H1 111(3) . . ? C23 Mo1 H1 111(3) . . ? C22 Mo1 H1 94(4) . . ? Si1 Mo1 H1 46(2) . . ? Si2 Mo1 H1 50(2) . . ? C3 Si1 C4 104.1(3) . . ? C3 Si1 C5 106.1(3) . . ? C4 Si1 C5 104.5(2) . . ? C3 Si1 Mo1 116.63(19) . . ? C4 Si1 Mo1 112.12(17) . . ? C5 Si1 Mo1 112.29(15) . . ? C3 Si1 H1 94(3) . . ? C4 Si1 H1 154(2) . . ? C5 Si1 H1 88(3) . . ? Mo1 Si1 H1 42(2) . . ? C21 Si2 C20 104.2(3) . . ? C21 Si2 C19 107.4(2) . . ? C20 Si2 C19 103.7(2) . . ? C21 Si2 Mo1 116.06(18) . . ? C20 Si2 Mo1 112.54(17) . . ? C19 Si2 Mo1 112.00(15) . . ? C10 O3 C14 113.0(3) . . ? O1 C1 Mo1 174.3(5) . . ? O2 C2 Mo1 174.5(5) . . ? Si1 C3 H2 109.5 . . ? Si1 C3 H3 109.5 . . ? H2 C3 H3 109.5 . . ? Si1 C3 H4 109.5 . . ? H2 C3 H4 109.5 . . ? H3 C3 H4 109.5 . . ? Si1 C4 H5 109.5 . . ? Si1 C4 H6 109.5 . . ? H5 C4 H6 109.5 . . ? Si1 C4 H7 109.5 . . ? H5 C4 H7 109.5 . . ? H6 C4 H7 109.5 . . ? C10 C5 C6 115.2(5) . . ? C10 C5 Si1 122.2(4) . . ? C6 C5 Si1 122.6(4) . . ? C7 C6 C5 121.6(5) . . ? C7 C6 H8 119.2 . . ? C5 C6 H8 119.2 . . ? C8 C7 C6 120.2(5) . . ? C8 C7 H9 119.9 . . ? C6 C7 H9 119.9 . . ? C7 C8 C9 121.0(5) . . ? C7 C8 H10 119.5 . . ? C9 C8 H10 119.5 . . ? C8 C9 C10 116.3(4) . . ? C8 C9 C11 125.8(5) . . ? C10 C9 C11 117.9(4) . . ? C9 C10 C5 125.7(5) . . ? C9 C10 O3 118.1(4) . . ? C5 C10 O3 116.1(4) . . ? C9 C11 C13 112.3(4) . . ? C9 C11 C15 106.2(4) . . ? C13 C11 C15 112.4(4) . . ? C9 C11 C12 108.4(4) . . ? C13 C11 C12 108.6(4) . . ? C15 C11 C12 108.7(4) . . ? C11 C12 H11 109.5 . . ? C11 C12 H12 109.5 . . ? H11 C12 H12 109.5 . . ? C11 C12 H13 109.5 . . ? H11 C12 H13 109.5 . . ? H12 C12 H13 109.5 . . ? C11 C13 H14 109.5 . . ? C11 C13 H15 109.5 . . ? H14 C13 H15 109.5 . . ? C11 C13 H16 109.5 . . ? H14 C13 H16 109.5 . . ? H15 C13 H16 109.5 . . ? C15 C14 C19 125.4(4) . . ? C15 C14 O3 118.5(4) . . ? C19 C14 O3 116.0(4) . . ? C14 C15 C16 117.5(5) . . ? C14 C15 C11 117.4(4) . . ? C16 C15 C11 125.0(4) . . ? C15 C16 C17 119.4(5) . . ? C15 C16 H17 120.3 . . ? C17 C16 H17 120.3 . . ? C18 C17 C16 120.7(5) . . ? C18 C17 H18 119.6 . . ? C16 C17 H18 119.6 . . ? C17 C18 C19 122.1(5) . . ? C17 C18 H19 119.0 . . ? C19 C18 H19 119.0 . . ? C14 C19 C18 114.8(4) . . ? C14 C19 Si2 121.3(4) . . ? C18 C19 Si2 123.8(4) . . ? Si2 C20 H20 109.5 . . ? Si2 C20 H21 109.5 . . ? H20 C20 H21 109.5 . . ? Si2 C20 H22 109.5 . . ? H20 C20 H22 109.5 . . ? H21 C20 H22 109.5 . . ? Si2 C21 H23 109.5 . . ? Si2 C21 H24 109.5 . . ? H23 C21 H24 109.5 . . ? Si2 C21 H25 109.5 . . ? H23 C21 H25 109.5 . . ? H24 C21 H25 109.5 . . ? C26 C22 C23 108.5(5) . . ? C26 C22 C27 125.1(5) . . ? C23 C22 C27 125.8(5) . . ? C26 C22 Mo1 72.4(3) . . ? C23 C22 Mo1 72.6(3) . . ? C27 C22 Mo1 127.8(3) . . ? C22 C23 C24 107.8(4) . . ? C22 C23 C28 124.7(5) . . ? C24 C23 C28 126.0(5) . . ? C22 C23 Mo1 72.7(3) . . ? C24 C23 Mo1 70.8(3) . . ? C28 C23 Mo1 133.0(4) . . ? C23 C24 C25 107.9(4) . . ? C23 C24 C29 125.7(5) . . ? C25 C24 C29 126.1(5) . . ? C23 C24 Mo1 74.1(3) . . ? C25 C24 Mo1 71.8(3) . . ? C29 C24 Mo1 124.5(4) . . ? C26 C25 C24 107.9(5) . . ? C26 C25 C30 125.7(5) . . ? C24 C25 C30 126.1(5) . . ? C26 C25 Mo1 74.2(3) . . ? C24 C25 Mo1 72.6(3) . . ? C30 C25 Mo1 124.3(4) . . ? C22 C26 C25 107.9(5) . . ? C22 C26 C31 125.1(5) . . ? C25 C26 C31 125.9(5) . . ? C22 C26 Mo1 73.0(3) . . ? C25 C26 Mo1 70.5(3) . . ? C31 C26 Mo1 131.7(4) . . ? C22 C27 H26 109.5 . . ? C22 C27 H27 109.5 . . ? H26 C27 H27 109.5 . . ? C22 C27 H28 109.5 . . ? H26 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? C23 C28 H29 109.5 . . ? C23 C28 H30 109.5 . . ? H29 C28 H30 109.5 . . ? C23 C28 H31 109.5 . . ? H29 C28 H31 109.5 . . ? H30 C28 H31 109.5 . . ? C24 C29 H32 109.5 . . ? C24 C29 H33 109.5 . . ? H32 C29 H33 109.5 . . ? C24 C29 H34 109.5 . . ? H32 C29 H34 109.5 . . ? H33 C29 H34 109.5 . . ? C25 C30 H35 109.5 . . ? C25 C30 H36 109.5 . . ? H35 C30 H36 109.5 . . ? C25 C30 H37 109.5 . . ? H35 C30 H37 109.5 . . ? H36 C30 H37 109.5 . . ? C26 C31 H38 109.5 . . ? C26 C31 H39 109.5 . . ? H38 C31 H39 109.5 . . ? C26 C31 H40 109.5 . . ? H38 C31 H40 109.5 . . ? H39 C31 H40 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 C1 Mo1 Si1 C3 16.8(3) . . . . ? C2 Mo1 Si1 C3 70.3(3) . . . . ? C25 Mo1 Si1 C3 166.3(3) . . . . ? C24 Mo1 Si1 C3 150.4(3) . . . . ? C26 Mo1 Si1 C3 -141.2(3) . . . . ? C23 Mo1 Si1 C3 176.5(3) . . . . ? C22 Mo1 Si1 C3 -150.2(2) . . . . ? Si2 Mo1 Si1 C3 -48.5(2) . . . . ? C1 Mo1 Si1 C4 -103.1(3) . . . . ? C2 Mo1 Si1 C4 -49.6(3) . . . . ? C25 Mo1 Si1 C4 46.4(3) . . . . ? C24 Mo1 Si1 C4 30.5(3) . . . . ? C26 Mo1 Si1 C4 98.9(3) . . . . ? C23 Mo1 Si1 C4 56.6(2) . . . . ? C22 Mo1 Si1 C4 89.9(2) . . . . ? Si2 Mo1 Si1 C4 -168.4(2) . . . . ? C1 Mo1 Si1 C5 139.6(2) . . . . ? C2 Mo1 Si1 C5 -166.9(3) . . . . ? C25 Mo1 Si1 C5 -70.9(3) . . . . ? C24 Mo1 Si1 C5 -86.9(2) . . . . ? C26 Mo1 Si1 C5 -18.5(3) . . . . ? C23 Mo1 Si1 C5 -60.8(2) . . . . ? C22 Mo1 Si1 C5 -27.4(2) . . . . ? Si2 Mo1 Si1 C5 74.21(18) . . . . ? C1 Mo1 Si2 C21 -70.7(3) . . . . ? C2 Mo1 Si2 C21 -18.6(3) . . . . ? C25 Mo1 Si2 C21 -151.3(3) . . . . ? C24 Mo1 Si2 C21 -164.5(3) . . . . ? C26 Mo1 Si2 C21 -178.5(3) . . . . ? C23 Mo1 Si2 C21 141.4(3) . . . . ? C22 Mo1 Si2 C21 148.7(2) . . . . ? Si1 Mo1 Si2 C21 48.1(2) . . . . ? C1 Mo1 Si2 C20 49.1(3) . . . . ? C2 Mo1 Si2 C20 101.3(3) . . . . ? C25 Mo1 Si2 C20 -31.4(2) . . . . ? C24 Mo1 Si2 C20 -44.6(3) . . . . ? C26 Mo1 Si2 C20 -58.7(2) . . . . ? C23 Mo1 Si2 C20 -98.7(3) . . . . ? C22 Mo1 Si2 C20 -91.5(2) . . . . ? Si1 Mo1 Si2 C20 168.0(2) . . . . ? C1 Mo1 Si2 C19 165.5(2) . . . . ? C2 Mo1 Si2 C19 -142.4(2) . . . . ? C25 Mo1 Si2 C19 84.9(2) . . . . ? C24 Mo1 Si2 C19 71.7(3) . . . . ? C26 Mo1 Si2 C19 57.7(2) . . . . ? C23 Mo1 Si2 C19 17.6(2) . . . . ? C22 Mo1 Si2 C19 24.9(2) . . . . ? Si1 Mo1 Si2 C19 -75.64(16) . . . . ? C3 Si1 C5 C10 65.1(5) . . . . ? C4 Si1 C5 C10 174.8(4) . . . . ? Mo1 Si1 C5 C10 -63.4(4) . . . . ? C3 Si1 C5 C6 -116.4(5) . . . . ? C4 Si1 C5 C6 -6.7(5) . . . . ? Mo1 Si1 C5 C6 115.0(4) . . . . ? C10 C5 C6 C7 0.5(7) . . . . ? Si1 C5 C6 C7 -178.1(4) . . . . ? C5 C6 C7 C8 0.6(8) . . . . ? C6 C7 C8 C9 -1.2(8) . . . . ? C7 C8 C9 C10 0.7(7) . . . . ? C7 C8 C9 C11 179.0(5) . . . . ? C8 C9 C10 C5 0.5(7) . . . . ? C11 C9 C10 C5 -177.9(4) . . . . ? C8 C9 C10 O3 178.5(4) . . . . ? C11 C9 C10 O3 0.0(6) . . . . ? C6 C5 C10 C9 -1.1(7) . . . . ? Si1 C5 C10 C9 177.5(4) . . . . ? C6 C5 C10 O3 -179.0(4) . . . . ? Si1 C5 C10 O3 -0.5(6) . . . . ? C14 O3 C10 C9 -42.8(6) . . . . ? C14 O3 C10 C5 135.3(4) . . . . ? C8 C9 C11 C13 -15.6(7) . . . . ? C10 C9 C11 C13 162.7(4) . . . . ? C8 C9 C11 C15 -138.9(5) . . . . ? C10 C9 C11 C15 39.4(6) . . . . ? C8 C9 C11 C12 104.4(6) . . . . ? C10 C9 C11 C12 -77.3(5) . . . . ? C10 O3 C14 C15 42.0(6) . . . . ? C10 O3 C14 C19 -135.5(4) . . . . ? C19 C14 C15 C16 -1.8(7) . . . . ? O3 C14 C15 C16 -179.0(4) . . . . ? C19 C14 C15 C11 178.6(4) . . . . ? O3 C14 C15 C11 1.5(6) . . . . ? C9 C11 C15 C14 -40.1(6) . . . . ? C13 C11 C15 C14 -163.4(4) . . . . ? C12 C11 C15 C14 76.3(5) . . . . ? C9 C11 C15 C16 140.4(5) . . . . ? C13 C11 C15 C16 17.2(7) . . . . ? C12 C11 C15 C16 -103.2(5) . . . . ? C14 C15 C16 C17 0.0(7) . . . . ? C11 C15 C16 C17 179.5(5) . . . . ? C15 C16 C17 C18 1.1(7) . . . . ? C16 C17 C18 C19 -0.6(8) . . . . ? C15 C14 C19 C18 2.3(7) . . . . ? O3 C14 C19 C18 179.6(4) . . . . ? C15 C14 C19 Si2 -177.5(4) . . . . ? O3 C14 C19 Si2 -0.3(6) . . . . ? C17 C18 C19 C14 -1.1(7) . . . . ? C17 C18 C19 Si2 178.8(4) . . . . ? C21 Si2 C19 C14 -63.2(5) . . . . ? C20 Si2 C19 C14 -173.1(4) . . . . ? Mo1 Si2 C19 C14 65.3(4) . . . . ? C21 Si2 C19 C18 116.9(4) . . . . ? C20 Si2 C19 C18 7.1(5) . . . . ? Mo1 Si2 C19 C18 -114.5(4) . . . . ? C1 Mo1 C22 C26 6.7(5) . . . . ? C2 Mo1 C22 C26 -124.9(4) . . . . ? C25 Mo1 C22 C26 -37.3(3) . . . . ? C24 Mo1 C22 C26 -79.4(3) . . . . ? C23 Mo1 C22 C26 -116.6(4) . . . . ? Si1 Mo1 C22 C26 168.5(3) . . . . ? Si2 Mo1 C22 C26 72.4(3) . . . . ? C1 Mo1 C22 C23 123.3(4) . . . . ? C2 Mo1 C22 C23 -8.3(4) . . . . ? C25 Mo1 C22 C23 79.3(3) . . . . ? C24 Mo1 C22 C23 37.3(3) . . . . ? C26 Mo1 C22 C23 116.6(4) . . . . ? Si1 Mo1 C22 C23 -74.9(3) . . . . ? Si2 Mo1 C22 C23 -170.9(3) . . . . ? C1 Mo1 C22 C27 -114.5(5) . . . . ? C2 Mo1 C22 C27 113.9(5) . . . . ? C25 Mo1 C22 C27 -158.5(5) . . . . ? C24 Mo1 C22 C27 159.5(5) . . . . ? C26 Mo1 C22 C27 -121.2(6) . . . . ? C23 Mo1 C22 C27 122.2(6) . . . . ? Si1 Mo1 C22 C27 47.3(4) . . . . ? Si2 Mo1 C22 C27 -48.7(4) . . . . ? C26 C22 C23 C24 1.5(6) . . . . ? C27 C22 C23 C24 173.0(5) . . . . ? Mo1 C22 C23 C24 -62.5(3) . . . . ? C26 C22 C23 C28 -165.2(5) . . . . ? C27 C22 C23 C28 6.4(8) . . . . ? Mo1 C22 C23 C28 130.8(5) . . . . ? C26 C22 C23 Mo1 64.0(3) . . . . ? C27 C22 C23 Mo1 -124.5(5) . . . . ? C1 Mo1 C23 C22 -105.8(4) . . . . ? C2 Mo1 C23 C22 174.4(3) . . . . ? C25 Mo1 C23 C22 -78.6(3) . . . . ? C24 Mo1 C23 C22 -116.5(4) . . . . ? C26 Mo1 C23 C22 -36.8(3) . . . . ? Si1 Mo1 C23 C22 107.8(3) . . . . ? Si2 Mo1 C23 C22 12.6(4) . . . . ? C1 Mo1 C23 C24 10.7(5) . . . . ? C2 Mo1 C23 C24 -69.0(3) . . . . ? C25 Mo1 C23 C24 38.0(3) . . . . ? C26 Mo1 C23 C24 79.7(3) . . . . ? C22 Mo1 C23 C24 116.5(4) . . . . ? Si1 Mo1 C23 C24 -135.7(3) . . . . ? Si2 Mo1 C23 C24 129.1(3) . . . . ? C1 Mo1 C23 C28 132.5(5) . . . . ? C2 Mo1 C23 C28 52.8(5) . . . . ? C25 Mo1 C23 C28 159.8(6) . . . . ? C24 Mo1 C23 C28 121.8(7) . . . . ? C26 Mo1 C23 C28 -158.5(6) . . . . ? C22 Mo1 C23 C28 -121.6(6) . . . . ? Si1 Mo1 C23 C28 -13.8(5) . . . . ? Si2 Mo1 C23 C28 -109.0(5) . . . . ? C22 C23 C24 C25 -0.5(6) . . . . ? C28 C23 C24 C25 165.9(5) . . . . ? Mo1 C23 C24 C25 -64.3(3) . . . . ? C22 C23 C24 C29 -174.9(5) . . . . ? C28 C23 C24 C29 -8.5(9) . . . . ? Mo1 C23 C24 C29 121.3(5) . . . . ? C22 C23 C24 Mo1 63.8(3) . . . . ? C28 C23 C24 Mo1 -129.8(5) . . . . ? C1 Mo1 C24 C23 -173.6(3) . . . . ? C2 Mo1 C24 C23 115.4(3) . . . . ? C25 Mo1 C24 C23 -115.5(4) . . . . ? C26 Mo1 C24 C23 -77.7(3) . . . . ? C22 Mo1 C24 C23 -36.8(3) . . . . ? Si1 Mo1 C24 C23 49.8(3) . . . . ? Si2 Mo1 C24 C23 -94.2(3) . . . . ? C1 Mo1 C24 C25 -58.2(4) . . . . ? C2 Mo1 C24 C25 -129.1(3) . . . . ? C26 Mo1 C24 C25 37.8(3) . . . . ? C23 Mo1 C24 C25 115.5(4) . . . . ? C22 Mo1 C24 C25 78.7(3) . . . . ? Si1 Mo1 C24 C25 165.3(3) . . . . ? Si2 Mo1 C24 C25 21.3(4) . . . . ? C1 Mo1 C24 C29 63.6(5) . . . . ? C2 Mo1 C24 C29 -7.3(5) . . . . ? C25 Mo1 C24 C29 121.8(6) . . . . ? C26 Mo1 C24 C29 159.6(5) . . . . ? C23 Mo1 C24 C29 -122.7(6) . . . . ? C22 Mo1 C24 C29 -159.5(5) . . . . ? Si1 Mo1 C24 C29 -72.9(5) . . . . ? Si2 Mo1 C24 C29 143.1(4) . . . . ? C23 C24 C25 C26 -0.6(6) . . . . ? C29 C24 C25 C26 173.8(5) . . . . ? Mo1 C24 C25 C26 -66.4(3) . . . . ? C23 C24 C25 C30 -174.1(5) . . . . ? C29 C24 C25 C30 0.3(9) . . . . ? Mo1 C24 C25 C30 120.1(5) . . . . ? C23 C24 C25 Mo1 65.8(3) . . . . ? C29 C24 C25 Mo1 -119.8(5) . . . . ? C1 Mo1 C25 C26 -117.2(3) . . . . ? C2 Mo1 C25 C26 171.8(3) . . . . ? C24 Mo1 C25 C26 115.0(4) . . . . ? C23 Mo1 C25 C26 77.5(3) . . . . ? C22 Mo1 C25 C26 36.6(3) . . . . ? Si1 Mo1 C25 C26 89.4(4) . . . . ? Si2 Mo1 C25 C26 -52.5(3) . . . . ? C1 Mo1 C25 C24 127.8(3) . . . . ? C2 Mo1 C25 C24 56.8(4) . . . . ? C26 Mo1 C25 C24 -115.0(4) . . . . ? C23 Mo1 C25 C24 -37.5(3) . . . . ? C22 Mo1 C25 C24 -78.5(3) . . . . ? Si1 Mo1 C25 C24 -25.6(4) . . . . ? Si2 Mo1 C25 C24 -167.5(3) . . . . ? C1 Mo1 C25 C30 5.6(5) . . . . ? C2 Mo1 C25 C30 -65.5(5) . . . . ? C24 Mo1 C25 C30 -122.2(6) . . . . ? C26 Mo1 C25 C30 122.7(6) . . . . ? C23 Mo1 C25 C30 -159.7(5) . . . . ? C22 Mo1 C25 C30 159.3(5) . . . . ? Si1 Mo1 C25 C30 -147.8(4) . . . . ? Si2 Mo1 C25 C30 70.3(5) . . . . ? C23 C22 C26 C25 -1.8(6) . . . . ? C27 C22 C26 C25 -173.5(5) . . . . ? Mo1 C22 C26 C25 62.2(3) . . . . ? C23 C22 C26 C31 166.5(5) . . . . ? C27 C22 C26 C31 -5.1(8) . . . . ? Mo1 C22 C26 C31 -129.4(5) . . . . ? C23 C22 C26 Mo1 -64.1(3) . . . . ? C27 C22 C26 Mo1 124.3(5) . . . . ? C24 C25 C26 C22 1.5(6) . . . . ? C30 C25 C26 C22 175.0(5) . . . . ? Mo1 C25 C26 C22 -63.8(3) . . . . ? C24 C25 C26 C31 -166.7(5) . . . . ? C30 C25 C26 C31 6.8(8) . . . . ? Mo1 C25 C26 C31 128.0(5) . . . . ? C24 C25 C26 Mo1 65.3(3) . . . . ? C30 C25 C26 Mo1 -121.2(5) . . . . ? C1 Mo1 C26 C22 -175.6(3) . . . . ? C2 Mo1 C26 C22 102.8(4) . . . . ? C25 Mo1 C26 C22 116.7(4) . . . . ? C24 Mo1 C26 C22 78.6(3) . . . . ? C23 Mo1 C26 C22 37.0(3) . . . . ? Si1 Mo1 C26 C22 -15.7(4) . . . . ? Si2 Mo1 C26 C22 -110.5(3) . . . . ? C1 Mo1 C26 C25 67.7(3) . . . . ? C2 Mo1 C26 C25 -13.9(5) . . . . ? C24 Mo1 C26 C25 -38.2(3) . . . . ? C23 Mo1 C26 C25 -79.8(3) . . . . ? C22 Mo1 C26 C25 -116.7(4) . . . . ? Si1 Mo1 C26 C25 -132.4(3) . . . . ? Si2 Mo1 C26 C25 132.8(3) . . . . ? C1 Mo1 C26 C31 -53.5(6) . . . . ? C2 Mo1 C26 C31 -135.1(6) . . . . ? C25 Mo1 C26 C31 -121.2(7) . . . . ? C24 Mo1 C26 C31 -159.3(6) . . . . ? C23 Mo1 C26 C31 159.1(7) . . . . ? C22 Mo1 C26 C31 122.1(7) . . . . ? Si1 Mo1 C26 C31 106.4(5) . . . . ? Si2 Mo1 C26 C31 11.6(6) . . . . ? #===END data_compound-3a #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 789739' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H49 Mo N O2 Si2' _chemical_formula_sum 'C35 H49 Mo N O2 Si2' _chemical_formula_weight 667.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.2178(3) _cell_length_b 14.7149(5) _cell_length_c 20.4190(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3370.54(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 38015 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour dark-purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.879674 _exptl_absorpt_correction_T_max 0.951140 _exptl_absorpt_process_details ; HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera. Rigaku Corporation, Tokyo, Japan. HIGASHI, T. (1999). Numabs - Numerical Absorption Correction, Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _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 29007 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 7699 _reflns_number_gt 7526 _reflns_threshold_expression >2\s(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+1.6625P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(9) _refine_ls_number_reflns 7699 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.277 _refine_ls_restrained_S_all 1.277 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.579 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.198 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 Mo1 Mo 0.134008(19) 0.234221(15) 0.168526(10) 0.01149(6) Uani 1 1 d . . . Si1 Si 0.38153(7) 0.40511(5) 0.20163(4) 0.01559(15) Uani 1 1 d . . . Si2 Si 0.08059(6) 0.25042(5) 0.29521(3) 0.01277(14) Uani 1 1 d . . . H1 H 0.093(4) 0.312(3) 0.2263(19) 0.030(11) Uiso 1 1 d . . . O1 O 0.1324(2) 0.04972(14) 0.24002(10) 0.0229(4) Uani 1 1 d . . . O2 O 0.33622(16) 0.31563(12) 0.33062(10) 0.0156(4) Uani 1 1 d . . . N1 N 0.3094(2) 0.30543(16) 0.17734(11) 0.0146(4) Uani 1 1 d . . . C1 C 0.1358(3) 0.12214(18) 0.21642(12) 0.0158(5) Uani 1 1 d . . . C2 C 0.3177(2) 0.22310(19) 0.16063(12) 0.0143(5) Uani 1 1 d . . . C3 C 0.4240(3) 0.1608(2) 0.15477(14) 0.0194(6) Uani 1 1 d . . . C4 C 0.3939(3) 0.0760(2) 0.11540(16) 0.0264(7) Uani 1 1 d . . . H2 H 0.3220 0.0476 0.1335 0.040 Uiso 1 1 calc R . . H3 H 0.4605 0.0330 0.1178 0.040 Uiso 1 1 calc R . . H4 H 0.3797 0.0927 0.0696 0.040 Uiso 1 1 calc R . . C5 C 0.4533(3) 0.1329(2) 0.22592(16) 0.0255(7) Uani 1 1 d . . . H5 H 0.4827 0.1859 0.2501 0.038 Uiso 1 1 calc R . . H6 H 0.5146 0.0855 0.2256 0.038 Uiso 1 1 calc R . . H7 H 0.3812 0.1097 0.2472 0.038 Uiso 1 1 calc R . . C6 C 0.5303(3) 0.2100(3) 0.12464(18) 0.0300(7) Uani 1 1 d . . . H8 H 0.5078 0.2344 0.0817 0.045 Uiso 1 1 calc R . . H9 H 0.5966 0.1673 0.1194 0.045 Uiso 1 1 calc R . . H10 H 0.5547 0.2600 0.1534 0.045 Uiso 1 1 calc R . . C7 C 0.2644(3) 0.4858(2) 0.22958(17) 0.0231(6) Uani 1 1 d . . . H11 H 0.1885 0.4706 0.2085 0.035 Uiso 1 1 calc R . . H12 H 0.2874 0.5479 0.2177 0.035 Uiso 1 1 calc R . . H13 H 0.2556 0.4814 0.2772 0.035 Uiso 1 1 calc R . . C8 C 0.4590(3) 0.4548(2) 0.12917(16) 0.0272(7) Uani 1 1 d . . . H14 H 0.5199 0.4123 0.1135 0.041 Uiso 1 1 calc R . . H15 H 0.4969 0.5122 0.1417 0.041 Uiso 1 1 calc R . . H16 H 0.4009 0.4660 0.0942 0.041 Uiso 1 1 calc R . . C9 C 0.4927(3) 0.3784(2) 0.26715(14) 0.0158(5) Uani 1 1 d . . . C10 C 0.6140(3) 0.3965(2) 0.26007(15) 0.0205(6) Uani 1 1 d . . . H17 H 0.6412 0.4269 0.2219 0.025 Uiso 1 1 calc R . . C11 C 0.6960(3) 0.3711(2) 0.30772(16) 0.0224(6) Uani 1 1 d . . . H18 H 0.7785 0.3833 0.3017 0.027 Uiso 1 1 calc R . . C12 C 0.6570(3) 0.3279(2) 0.36401(16) 0.0211(6) Uani 1 1 d . . . H19 H 0.7134 0.3107 0.3964 0.025 Uiso 1 1 calc R . . C13 C 0.5364(3) 0.30926(19) 0.37410(14) 0.0168(5) Uani 1 1 d . . . C14 C 0.4567(2) 0.33451(18) 0.32509(14) 0.0165(5) Uani 1 1 d . . . C15 C 0.4870(3) 0.2680(2) 0.43675(13) 0.0183(5) Uani 1 1 d . . . C16 C 0.4397(3) 0.3464(2) 0.48005(16) 0.0284(7) Uani 1 1 d . . . H20 H 0.4057 0.3214 0.5204 0.043 Uiso 1 1 calc R . . H21 H 0.3780 0.3800 0.4562 0.043 Uiso 1 1 calc R . . H22 H 0.5054 0.3876 0.4910 0.043 Uiso 1 1 calc R . . C17 C 0.5812(3) 0.2155(2) 0.47451(15) 0.0288(7) Uani 1 1 d . . . H23 H 0.6079 0.1635 0.4484 0.043 Uiso 1 1 calc R . . H24 H 0.5473 0.1938 0.5159 0.043 Uiso 1 1 calc R . . H25 H 0.6492 0.2553 0.4836 0.043 Uiso 1 1 calc R . . C18 C 0.3049(2) 0.23958(19) 0.36749(12) 0.0150(5) Uani 1 1 d . . . C19 C 0.3804(3) 0.20913(19) 0.41749(13) 0.0168(5) Uani 1 1 d . . . C20 C 0.3483(3) 0.1297(2) 0.44965(14) 0.0205(6) Uani 1 1 d . . . H26 H 0.3987 0.1061 0.4830 0.025 Uiso 1 1 calc R . . C21 C 0.2440(3) 0.0842(2) 0.43388(14) 0.0207(6) Uani 1 1 d . . . H27 H 0.2244 0.0290 0.4555 0.025 Uiso 1 1 calc R . . C22 C 0.1678(3) 0.1194(2) 0.38623(14) 0.0182(6) Uani 1 1 d . . . H28 H 0.0954 0.0886 0.3767 0.022 Uiso 1 1 calc R . . C23 C 0.1958(2) 0.1990(2) 0.35226(13) 0.0140(5) Uani 1 1 d . . . C24 C -0.0646(3) 0.1886(2) 0.30912(15) 0.0205(6) Uani 1 1 d . . . H29 H -0.0829 0.1878 0.3560 0.031 Uiso 1 1 calc R . . H30 H -0.0576 0.1261 0.2930 0.031 Uiso 1 1 calc R . . H31 H -0.1287 0.2198 0.2855 0.031 Uiso 1 1 calc R . . C25 C 0.0531(3) 0.36446(19) 0.33522(15) 0.0210(6) Uani 1 1 d . . . H32 H 0.0044 0.4023 0.3061 0.032 Uiso 1 1 calc R . . H33 H 0.1295 0.3947 0.3434 0.032 Uiso 1 1 calc R . . H34 H 0.0110 0.3555 0.3768 0.032 Uiso 1 1 calc R . . C26 C 0.0637(3) 0.1647(2) 0.07511(14) 0.0172(6) Uani 1 1 d . . . C27 C 0.1264(3) 0.2447(2) 0.05408(11) 0.0190(5) Uani 1 1 d . . . C28 C 0.0637(3) 0.3219(2) 0.07807(14) 0.0186(6) Uani 1 1 d . . . C29 C -0.0382(3) 0.2901(2) 0.11352(14) 0.0172(6) Uani 1 1 d . . . C30 C -0.0385(3) 0.1937(2) 0.11236(14) 0.0163(5) Uani 1 1 d . . . C31 C 0.0866(3) 0.0680(2) 0.05469(17) 0.0283(7) Uani 1 1 d . . . H35 H 0.0333 0.0519 0.0185 0.042 Uiso 1 1 calc R . . H36 H 0.0719 0.0274 0.0919 0.042 Uiso 1 1 calc R . . H37 H 0.1696 0.0618 0.0404 0.042 Uiso 1 1 calc R . . C32 C 0.2340(3) 0.2478(3) 0.01008(14) 0.0293(7) Uani 1 1 d . . . H38 H 0.2702 0.1873 0.0078 0.044 Uiso 1 1 calc R . . H39 H 0.2921 0.2911 0.0277 0.044 Uiso 1 1 calc R . . H40 H 0.2098 0.2671 -0.0339 0.044 Uiso 1 1 calc R . . C33 C 0.0943(4) 0.4187(2) 0.06335(17) 0.0293(7) Uani 1 1 d . . . H41 H 0.0613 0.4356 0.0206 0.044 Uiso 1 1 calc R . . H42 H 0.1811 0.4258 0.0625 0.044 Uiso 1 1 calc R . . H43 H 0.0605 0.4582 0.0973 0.044 Uiso 1 1 calc R . . C34 C -0.1318(3) 0.3493(2) 0.14414(15) 0.0251(6) Uani 1 1 d . . . H44 H -0.0934 0.4002 0.1669 0.038 Uiso 1 1 calc R . . H45 H -0.1783 0.3136 0.1756 0.038 Uiso 1 1 calc R . . H46 H -0.1848 0.3729 0.1100 0.038 Uiso 1 1 calc R . . C35 C -0.1336(3) 0.1306(2) 0.13691(15) 0.0228(6) Uani 1 1 d . . . H47 H -0.1845 0.1120 0.1003 0.034 Uiso 1 1 calc R . . H48 H -0.1819 0.1619 0.1699 0.034 Uiso 1 1 calc R . . H49 H -0.0964 0.0769 0.1565 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01220(10) 0.01245(10) 0.00983(9) 0.00014(8) -0.00008(8) 0.00063(8) Si1 0.0154(4) 0.0142(3) 0.0171(3) 0.0032(3) -0.0005(3) -0.0016(3) Si2 0.0135(3) 0.0125(4) 0.0123(3) 0.0003(3) 0.0006(2) -0.0003(3) O1 0.0331(11) 0.0148(9) 0.0208(10) 0.0009(7) 0.0030(10) 0.0006(10) O2 0.0145(9) 0.0159(9) 0.0165(9) 0.0059(8) -0.0017(8) -0.0006(7) N1 0.0128(10) 0.0173(11) 0.0137(11) 0.0009(9) 0.0007(9) -0.0012(8) C1 0.0164(12) 0.0167(12) 0.0143(11) -0.0017(9) 0.0027(11) 0.0006(12) C2 0.0107(11) 0.0218(13) 0.0105(11) 0.0029(10) 0.0015(9) 0.0006(10) C3 0.0182(14) 0.0199(14) 0.0201(14) -0.0009(11) 0.0013(11) 0.0061(11) C4 0.0307(17) 0.0242(16) 0.0243(15) -0.0044(12) -0.0001(13) 0.0086(13) C5 0.0292(17) 0.0212(15) 0.0260(15) -0.0003(12) -0.0067(13) 0.0100(13) C6 0.0177(15) 0.0336(19) 0.0386(18) 0.0040(15) 0.0087(13) 0.0045(13) C7 0.0217(15) 0.0138(13) 0.0340(16) 0.0003(12) -0.0035(13) 0.0019(12) C8 0.0275(16) 0.0297(17) 0.0245(15) 0.0120(13) 0.0005(13) -0.0043(13) C9 0.0124(13) 0.0160(13) 0.0191(13) 0.0001(10) 0.0011(10) -0.0009(10) C10 0.0176(15) 0.0195(14) 0.0244(14) 0.0006(11) 0.0017(11) -0.0022(11) C11 0.0140(13) 0.0221(14) 0.0310(15) -0.0008(12) -0.0013(12) -0.0011(11) C12 0.0156(14) 0.0214(14) 0.0264(14) 0.0006(12) -0.0050(11) 0.0021(11) C13 0.0214(14) 0.0126(13) 0.0163(13) -0.0012(10) -0.0031(11) 0.0008(11) C14 0.0169(13) 0.0135(12) 0.0192(13) -0.0013(11) -0.0006(11) -0.0001(10) C15 0.0180(12) 0.0210(13) 0.0160(12) 0.0007(12) -0.0038(9) 0.0018(12) C16 0.0333(18) 0.0315(18) 0.0205(15) -0.0090(13) -0.0024(13) -0.0002(14) C17 0.0260(16) 0.036(2) 0.0244(15) 0.0081(13) -0.0114(13) -0.0002(14) C18 0.0213(13) 0.0110(11) 0.0128(11) 0.0000(10) 0.0013(9) 0.0010(10) C19 0.0201(13) 0.0156(12) 0.0145(11) -0.0003(9) -0.0005(11) 0.0017(10) C20 0.0270(17) 0.0178(13) 0.0168(12) 0.0022(10) -0.0020(12) 0.0046(12) C21 0.0255(16) 0.0157(14) 0.0210(14) 0.0064(11) 0.0006(11) -0.0003(11) C22 0.0194(14) 0.0172(13) 0.0179(13) 0.0010(11) 0.0014(10) 0.0012(10) C23 0.0127(12) 0.0167(12) 0.0125(11) -0.0028(10) 0.0014(9) 0.0023(10) C24 0.0193(14) 0.0221(14) 0.0202(13) -0.0009(11) 0.0026(11) 0.0007(11) C25 0.0268(14) 0.0193(13) 0.0170(12) -0.0009(12) 0.0007(12) 0.0029(11) C26 0.0184(14) 0.0203(14) 0.0129(12) -0.0046(10) -0.0015(11) 0.0018(11) C27 0.0220(13) 0.0254(14) 0.0096(10) 0.0023(10) -0.0035(10) -0.0001(13) C28 0.0216(15) 0.0189(14) 0.0153(13) 0.0068(11) -0.0070(12) 0.0005(11) C29 0.0204(14) 0.0172(14) 0.0140(12) 0.0005(10) -0.0053(11) 0.0035(10) C30 0.0155(13) 0.0166(13) 0.0168(13) 0.0007(11) -0.0025(11) 0.0011(10) C31 0.0348(18) 0.0247(16) 0.0255(16) -0.0096(13) -0.0065(14) 0.0067(14) C32 0.0228(14) 0.050(2) 0.0155(12) 0.0052(14) 0.0015(11) 0.0009(15) C33 0.0354(18) 0.0238(16) 0.0288(17) 0.0118(13) -0.0080(13) -0.0042(14) C34 0.0230(14) 0.0268(15) 0.0255(14) -0.0039(12) -0.0064(14) 0.0130(14) C35 0.0195(14) 0.0254(15) 0.0235(14) 0.0027(11) -0.0019(14) -0.0033(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 Mo1 C1 1.917(3) . ? Mo1 C2 2.073(3) . ? Mo1 N1 2.236(2) . ? Mo1 C26 2.304(3) . ? Mo1 C30 2.327(3) . ? Mo1 C27 2.343(2) . ? Mo1 C29 2.382(3) . ? Mo1 C28 2.387(3) . ? Mo1 Si2 2.6659(7) . ? Mo1 H1 1.71(4) . ? Si1 N1 1.747(2) . ? Si1 C7 1.861(3) . ? Si1 C8 1.865(3) . ? Si1 C9 1.870(3) . ? Si2 C24 1.887(3) . ? Si2 C25 1.892(3) . ? Si2 C23 1.897(3) . ? Si2 H1 1.68(4) . ? O1 C1 1.170(3) . ? O2 C14 1.385(3) . ? O2 C18 1.394(3) . ? N1 C2 1.262(4) . ? C2 C3 1.509(4) . ? C3 C4 1.523(4) . ? C3 C6 1.524(4) . ? C3 C5 1.545(4) . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C5 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C6 H10 0.9800 . ? C7 H11 0.9800 . ? C7 H12 0.9800 . ? C7 H13 0.9800 . ? C8 H14 0.9800 . ? C8 H15 0.9800 . ? C8 H16 0.9800 . ? C9 C10 1.395(4) . ? C9 C14 1.407(4) . ? C10 C11 1.390(4) . ? C10 H17 0.9500 . ? C11 C12 1.384(4) . ? C11 H18 0.9500 . ? C12 C13 1.396(4) . ? C12 H19 0.9500 . ? C13 C14 1.392(4) . ? C13 C15 1.520(4) . ? C15 C17 1.520(4) . ? C15 C19 1.528(4) . ? C15 C16 1.547(4) . ? C16 H20 0.9800 . ? C16 H21 0.9800 . ? C16 H22 0.9800 . ? C17 H23 0.9800 . ? C17 H24 0.9800 . ? C17 H25 0.9800 . ? C18 C23 1.397(4) . ? C18 C19 1.400(4) . ? C19 C20 1.389(4) . ? C20 C21 1.386(4) . ? C20 H26 0.9500 . ? C21 C22 1.395(4) . ? C21 H27 0.9500 . ? C22 C23 1.397(4) . ? C22 H28 0.9500 . ? C24 H29 0.9800 . ? C24 H30 0.9800 . ? C24 H31 0.9800 . ? C25 H32 0.9800 . ? C25 H33 0.9800 . ? C25 H34 0.9800 . ? C26 C27 1.437(4) . ? C26 C30 1.440(4) . ? C26 C31 1.505(4) . ? C27 C28 1.424(4) . ? C27 C32 1.506(4) . ? C28 C29 1.432(4) . ? C28 C33 1.495(4) . ? C29 C30 1.419(4) . ? C29 C34 1.501(4) . ? C30 C35 1.500(4) . ? C31 H35 0.9800 . ? C31 H36 0.9800 . ? C31 H37 0.9800 . ? C32 H38 0.9800 . ? C32 H39 0.9800 . ? C32 H40 0.9800 . ? C33 H41 0.9800 . ? C33 H42 0.9800 . ? C33 H43 0.9800 . ? C34 H44 0.9800 . ? C34 H45 0.9800 . ? C34 H46 0.9800 . ? C35 H47 0.9800 . ? C35 H48 0.9800 . ? C35 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 C1 Mo1 C2 87.78(12) . . ? C1 Mo1 N1 110.65(11) . . ? C2 Mo1 N1 33.79(10) . . ? C1 Mo1 C26 92.52(11) . . ? C2 Mo1 C26 103.94(10) . . ? N1 Mo1 C26 125.17(10) . . ? C1 Mo1 C30 92.29(12) . . ? C2 Mo1 C30 140.16(10) . . ? N1 Mo1 C30 153.03(9) . . ? C26 Mo1 C30 36.23(10) . . ? C1 Mo1 C27 124.42(10) . . ? C2 Mo1 C27 87.92(10) . . ? N1 Mo1 C27 94.68(9) . . ? C26 Mo1 C27 36.00(10) . . ? C30 Mo1 C27 59.67(10) . . ? C1 Mo1 C29 123.11(12) . . ? C2 Mo1 C29 142.83(10) . . ? N1 Mo1 C29 126.14(9) . . ? C26 Mo1 C29 59.00(10) . . ? C30 Mo1 C29 35.05(10) . . ? C27 Mo1 C29 58.50(10) . . ? C1 Mo1 C28 149.66(11) . . ? C2 Mo1 C28 108.11(10) . . ? N1 Mo1 C28 95.72(10) . . ? C26 Mo1 C28 59.09(10) . . ? C30 Mo1 C28 58.83(10) . . ? C27 Mo1 C28 35.02(10) . . ? C29 Mo1 C28 34.94(10) . . ? C1 Mo1 Si2 65.45(8) . . ? C2 Mo1 Si2 107.82(7) . . ? N1 Mo1 Si2 94.46(6) . . ? C26 Mo1 Si2 140.00(8) . . ? C30 Mo1 Si2 108.31(7) . . ? C27 Mo1 Si2 162.46(7) . . ? C29 Mo1 Si2 104.14(7) . . ? C28 Mo1 Si2 128.90(8) . . ? C1 Mo1 H1 103.2(13) . . ? C2 Mo1 H1 112.1(14) . . ? N1 Mo1 H1 82.4(14) . . ? C26 Mo1 H1 140.9(14) . . ? C30 Mo1 H1 106.6(14) . . ? C27 Mo1 H1 129.3(13) . . ? C29 Mo1 H1 82.7(14) . . ? C28 Mo1 H1 94.6(13) . . ? Si2 Mo1 H1 37.8(13) . . ? N1 Si1 C7 107.21(13) . . ? N1 Si1 C8 108.64(14) . . ? C7 Si1 C8 108.79(15) . . ? N1 Si1 C9 109.58(12) . . ? C7 Si1 C9 112.68(14) . . ? C8 Si1 C9 109.83(14) . . ? C24 Si2 C25 102.82(14) . . ? C24 Si2 C23 107.63(13) . . ? C25 Si2 C23 101.53(13) . . ? C24 Si2 Mo1 107.27(10) . . ? C25 Si2 Mo1 122.35(10) . . ? C23 Si2 Mo1 114.02(8) . . ? C24 Si2 H1 117.2(14) . . ? C25 Si2 H1 83.9(14) . . ? C23 Si2 H1 132.5(14) . . ? Mo1 Si2 H1 38.6(14) . . ? C14 O2 C18 116.8(2) . . ? C2 N1 Si1 148.1(2) . . ? C2 N1 Mo1 65.99(15) . . ? Si1 N1 Mo1 145.45(13) . . ? O1 C1 Mo1 173.2(2) . . ? N1 C2 C3 131.5(3) . . ? N1 C2 Mo1 80.22(17) . . ? C3 C2 Mo1 147.1(2) . . ? C2 C3 C4 111.4(3) . . ? C2 C3 C6 111.2(2) . . ? C4 C3 C6 110.5(3) . . ? C2 C3 C5 104.8(2) . . ? C4 C3 C5 109.0(3) . . ? C6 C3 C5 109.8(3) . . ? C3 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C4 H4 109.5 . . ? H2 C4 H4 109.5 . . ? H3 C4 H4 109.5 . . ? C3 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C5 H7 109.5 . . ? H5 C5 H7 109.5 . . ? H6 C5 H7 109.5 . . ? C3 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C3 C6 H10 109.5 . . ? H8 C6 H10 109.5 . . ? H9 C6 H10 109.5 . . ? Si1 C7 H11 109.5 . . ? Si1 C7 H12 109.5 . . ? H11 C7 H12 109.5 . . ? Si1 C7 H13 109.5 . . ? H11 C7 H13 109.5 . . ? H12 C7 H13 109.5 . . ? Si1 C8 H14 109.5 . . ? Si1 C8 H15 109.5 . . ? H14 C8 H15 109.5 . . ? Si1 C8 H16 109.5 . . ? H14 C8 H16 109.5 . . ? H15 C8 H16 109.5 . . ? C10 C9 C14 117.0(3) . . ? C10 C9 Si1 122.4(2) . . ? C14 C9 Si1 120.5(2) . . ? C11 C10 C9 121.5(3) . . ? C11 C10 H17 119.3 . . ? C9 C10 H17 119.3 . . ? C12 C11 C10 119.7(3) . . ? C12 C11 H18 120.2 . . ? C10 C11 H18 120.2 . . ? C11 C12 C13 121.3(3) . . ? C11 C12 H19 119.3 . . ? C13 C12 H19 119.3 . . ? C14 C13 C12 117.6(3) . . ? C14 C13 C15 118.5(3) . . ? C12 C13 C15 123.8(3) . . ? O2 C14 C13 121.0(3) . . ? O2 C14 C9 116.1(3) . . ? C13 C14 C9 122.9(3) . . ? C17 C15 C13 112.1(2) . . ? C17 C15 C19 112.7(3) . . ? C13 C15 C19 107.2(2) . . ? C17 C15 C16 109.1(3) . . ? C13 C15 C16 108.0(3) . . ? C19 C15 C16 107.6(2) . . ? C15 C16 H20 109.5 . . ? C15 C16 H21 109.5 . . ? H20 C16 H21 109.5 . . ? C15 C16 H22 109.5 . . ? H20 C16 H22 109.5 . . ? H21 C16 H22 109.5 . . ? C15 C17 H23 109.5 . . ? C15 C17 H24 109.5 . . ? H23 C17 H24 109.5 . . ? C15 C17 H25 109.5 . . ? H23 C17 H25 109.5 . . ? H24 C17 H25 109.5 . . ? O2 C18 C23 116.4(2) . . ? O2 C18 C19 119.9(2) . . ? C23 C18 C19 123.7(3) . . ? C20 C19 C18 117.2(3) . . ? C20 C19 C15 124.0(3) . . ? C18 C19 C15 118.6(2) . . ? C21 C20 C19 121.0(3) . . ? C21 C20 H26 119.5 . . ? C19 C20 H26 119.5 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H27 120.0 . . ? C22 C21 H27 120.0 . . ? C21 C22 C23 121.4(3) . . ? C21 C22 H28 119.3 . . ? C23 C22 H28 119.3 . . ? C22 C23 C18 116.4(3) . . ? C22 C23 Si2 119.1(2) . . ? C18 C23 Si2 124.2(2) . . ? Si2 C24 H29 109.5 . . ? Si2 C24 H30 109.5 . . ? H29 C24 H30 109.5 . . ? Si2 C24 H31 109.5 . . ? H29 C24 H31 109.5 . . ? H30 C24 H31 109.5 . . ? Si2 C25 H32 109.5 . . ? Si2 C25 H33 109.5 . . ? H32 C25 H33 109.5 . . ? Si2 C25 H34 109.5 . . ? H32 C25 H34 109.5 . . ? H33 C25 H34 109.5 . . ? C27 C26 C30 107.7(3) . . ? C27 C26 C31 127.4(3) . . ? C30 C26 C31 124.3(3) . . ? C27 C26 Mo1 73.50(15) . . ? C30 C26 Mo1 72.75(16) . . ? C31 C26 Mo1 126.2(2) . . ? C28 C27 C26 108.0(2) . . ? C28 C27 C32 125.2(3) . . ? C26 C27 C32 126.6(3) . . ? C28 C27 Mo1 74.18(15) . . ? C26 C27 Mo1 70.50(14) . . ? C32 C27 Mo1 124.61(19) . . ? C27 C28 C29 107.9(2) . . ? C27 C28 C33 125.3(3) . . ? C29 C28 C33 126.6(3) . . ? C27 C28 Mo1 70.80(14) . . ? C29 C28 Mo1 72.30(15) . . ? C33 C28 Mo1 126.5(2) . . ? C30 C29 C28 108.7(3) . . ? C30 C29 C34 125.9(3) . . ? C28 C29 C34 125.4(3) . . ? C30 C29 Mo1 70.36(17) . . ? C28 C29 Mo1 72.76(16) . . ? C34 C29 Mo1 124.9(2) . . ? C29 C30 C26 107.7(3) . . ? C29 C30 C35 127.9(3) . . ? C26 C30 C35 124.0(3) . . ? C29 C30 Mo1 74.59(18) . . ? C26 C30 Mo1 71.02(16) . . ? C35 C30 Mo1 125.8(2) . . ? C26 C31 H35 109.5 . . ? C26 C31 H36 109.5 . . ? H35 C31 H36 109.5 . . ? C26 C31 H37 109.5 . . ? H35 C31 H37 109.5 . . ? H36 C31 H37 109.5 . . ? C27 C32 H38 109.5 . . ? C27 C32 H39 109.5 . . ? H38 C32 H39 109.5 . . ? C27 C32 H40 109.5 . . ? H38 C32 H40 109.5 . . ? H39 C32 H40 109.5 . . ? C28 C33 H41 109.5 . . ? C28 C33 H42 109.5 . . ? H41 C33 H42 109.5 . . ? C28 C33 H43 109.5 . . ? H41 C33 H43 109.5 . . ? H42 C33 H43 109.5 . . ? C29 C34 H44 109.5 . . ? C29 C34 H45 109.5 . . ? H44 C34 H45 109.5 . . ? C29 C34 H46 109.5 . . ? H44 C34 H46 109.5 . . ? H45 C34 H46 109.5 . . ? C30 C35 H47 109.5 . . ? C30 C35 H48 109.5 . . ? H47 C35 H48 109.5 . . ? C30 C35 H49 109.5 . . ? H47 C35 H49 109.5 . . ? H48 C35 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 C1 Mo1 Si2 C24 -65.58(14) . . . . ? C2 Mo1 Si2 C24 -144.54(13) . . . . ? N1 Mo1 Si2 C24 -176.26(12) . . . . ? C26 Mo1 Si2 C24 -3.56(16) . . . . ? C30 Mo1 Si2 C24 18.40(13) . . . . ? C27 Mo1 Si2 C24 62.5(3) . . . . ? C29 Mo1 Si2 C24 54.70(13) . . . . ? C28 Mo1 Si2 C24 82.70(14) . . . . ? C1 Mo1 Si2 C25 176.26(16) . . . . ? C2 Mo1 Si2 C25 97.30(14) . . . . ? N1 Mo1 Si2 C25 65.57(13) . . . . ? C26 Mo1 Si2 C25 -121.73(17) . . . . ? C30 Mo1 Si2 C25 -99.77(14) . . . . ? C27 Mo1 Si2 C25 -55.6(3) . . . . ? C29 Mo1 Si2 C25 -63.46(14) . . . . ? C28 Mo1 Si2 C25 -35.46(15) . . . . ? C1 Mo1 Si2 C23 53.48(14) . . . . ? C2 Mo1 Si2 C23 -25.48(13) . . . . ? N1 Mo1 Si2 C23 -57.20(12) . . . . ? C26 Mo1 Si2 C23 115.50(15) . . . . ? C30 Mo1 Si2 C23 137.46(13) . . . . ? C27 Mo1 Si2 C23 -178.4(3) . . . . ? C29 Mo1 Si2 C23 173.76(13) . . . . ? C28 Mo1 Si2 C23 -158.24(13) . . . . ? C7 Si1 N1 C2 -169.3(4) . . . . ? C8 Si1 N1 C2 73.3(4) . . . . ? C9 Si1 N1 C2 -46.7(4) . . . . ? C7 Si1 N1 Mo1 -2.3(3) . . . . ? C8 Si1 N1 Mo1 -119.7(2) . . . . ? C9 Si1 N1 Mo1 120.3(2) . . . . ? C1 Mo1 N1 C2 50.39(19) . . . . ? C26 Mo1 N1 C2 -58.5(2) . . . . ? C30 Mo1 N1 C2 -96.2(2) . . . . ? C27 Mo1 N1 C2 -79.18(17) . . . . ? C29 Mo1 N1 C2 -133.07(17) . . . . ? C28 Mo1 N1 C2 -114.34(17) . . . . ? Si2 Mo1 N1 C2 115.80(16) . . . . ? C1 Mo1 N1 Si1 -122.1(2) . . . . ? C2 Mo1 N1 Si1 -172.5(3) . . . . ? C26 Mo1 N1 Si1 129.1(2) . . . . ? C30 Mo1 N1 Si1 91.3(3) . . . . ? C27 Mo1 N1 Si1 108.3(2) . . . . ? C29 Mo1 N1 Si1 54.4(3) . . . . ? C28 Mo1 N1 Si1 73.2(2) . . . . ? Si2 Mo1 N1 Si1 -56.7(2) . . . . ? Si1 N1 C2 C3 1.8(6) . . . . ? Mo1 N1 C2 C3 -170.1(3) . . . . ? Si1 N1 C2 Mo1 171.9(4) . . . . ? C1 Mo1 C2 N1 -133.83(17) . . . . ? C26 Mo1 C2 N1 134.12(17) . . . . ? C30 Mo1 C2 N1 135.26(18) . . . . ? C27 Mo1 C2 N1 101.59(17) . . . . ? C29 Mo1 C2 N1 77.5(2) . . . . ? C28 Mo1 C2 N1 72.52(18) . . . . ? Si2 Mo1 C2 N1 -70.52(16) . . . . ? C1 Mo1 C2 C3 32.5(4) . . . . ? N1 Mo1 C2 C3 166.3(5) . . . . ? C26 Mo1 C2 C3 -59.6(4) . . . . ? C30 Mo1 C2 C3 -58.5(4) . . . . ? C27 Mo1 C2 C3 -92.1(4) . . . . ? C29 Mo1 C2 C3 -116.2(3) . . . . ? C28 Mo1 C2 C3 -121.2(3) . . . . ? Si2 Mo1 C2 C3 95.8(3) . . . . ? N1 C2 C3 C4 -164.5(3) . . . . ? Mo1 C2 C3 C4 33.7(5) . . . . ? N1 C2 C3 C6 -40.8(4) . . . . ? Mo1 C2 C3 C6 157.4(3) . . . . ? N1 C2 C3 C5 77.8(4) . . . . ? Mo1 C2 C3 C5 -84.0(4) . . . . ? N1 Si1 C9 C10 120.5(3) . . . . ? C7 Si1 C9 C10 -120.2(3) . . . . ? C8 Si1 C9 C10 1.2(3) . . . . ? N1 Si1 C9 C14 -56.4(3) . . . . ? C7 Si1 C9 C14 62.9(3) . . . . ? C8 Si1 C9 C14 -175.7(2) . . . . ? C14 C9 C10 C11 1.0(4) . . . . ? Si1 C9 C10 C11 -176.1(2) . . . . ? C9 C10 C11 C12 -0.9(5) . . . . ? C10 C11 C12 C13 0.0(5) . . . . ? C11 C12 C13 C14 0.9(4) . . . . ? C11 C12 C13 C15 -175.6(3) . . . . ? C18 O2 C14 C13 -28.4(4) . . . . ? C18 O2 C14 C9 150.3(2) . . . . ? C12 C13 C14 O2 177.9(3) . . . . ? C15 C13 C14 O2 -5.4(4) . . . . ? C12 C13 C14 C9 -0.8(4) . . . . ? C15 C13 C14 C9 175.9(3) . . . . ? C10 C9 C14 O2 -178.9(2) . . . . ? Si1 C9 C14 O2 -1.8(4) . . . . ? C10 C9 C14 C13 -0.1(4) . . . . ? Si1 C9 C14 C13 177.0(2) . . . . ? C14 C13 C15 C17 160.5(3) . . . . ? C12 C13 C15 C17 -23.1(4) . . . . ? C14 C13 C15 C19 36.3(4) . . . . ? C12 C13 C15 C19 -147.3(3) . . . . ? C14 C13 C15 C16 -79.3(3) . . . . ? C12 C13 C15 C16 97.2(3) . . . . ? C14 O2 C18 C23 -154.7(2) . . . . ? C14 O2 C18 C19 26.6(4) . . . . ? O2 C18 C19 C20 -175.9(2) . . . . ? C23 C18 C19 C20 5.5(4) . . . . ? O2 C18 C19 C15 8.5(4) . . . . ? C23 C18 C19 C15 -170.1(3) . . . . ? C17 C15 C19 C20 23.1(4) . . . . ? C13 C15 C19 C20 146.9(3) . . . . ? C16 C15 C19 C20 -97.3(3) . . . . ? C17 C15 C19 C18 -161.7(3) . . . . ? C13 C15 C19 C18 -37.9(3) . . . . ? C16 C15 C19 C18 78.0(3) . . . . ? C18 C19 C20 C21 -1.8(4) . . . . ? C15 C19 C20 C21 173.6(3) . . . . ? C19 C20 C21 C22 -1.7(5) . . . . ? C20 C21 C22 C23 1.8(4) . . . . ? C21 C22 C23 C18 1.5(4) . . . . ? C21 C22 C23 Si2 -173.1(2) . . . . ? O2 C18 C23 C22 176.0(2) . . . . ? C19 C18 C23 C22 -5.3(4) . . . . ? O2 C18 C23 Si2 -9.7(3) . . . . ? C19 C18 C23 Si2 169.0(2) . . . . ? C24 Si2 C23 C22 9.9(3) . . . . ? C25 Si2 C23 C22 117.5(2) . . . . ? Mo1 Si2 C23 C22 -109.0(2) . . . . ? C24 Si2 C23 C18 -164.3(2) . . . . ? C25 Si2 C23 C18 -56.7(3) . . . . ? Mo1 Si2 C23 C18 76.8(2) . . . . ? C1 Mo1 C26 C27 -154.43(18) . . . . ? C2 Mo1 C26 C27 -66.09(18) . . . . ? N1 Mo1 C26 C27 -36.9(2) . . . . ? C30 Mo1 C26 C27 115.1(2) . . . . ? C29 Mo1 C26 C27 77.88(18) . . . . ? C28 Mo1 C26 C27 36.89(16) . . . . ? Si2 Mo1 C26 C27 152.06(14) . . . . ? C1 Mo1 C26 C30 90.43(18) . . . . ? C2 Mo1 C26 C30 178.77(17) . . . . ? N1 Mo1 C26 C30 -151.99(16) . . . . ? C27 Mo1 C26 C30 -115.1(2) . . . . ? C29 Mo1 C26 C30 -37.26(17) . . . . ? C28 Mo1 C26 C30 -78.25(18) . . . . ? Si2 Mo1 C26 C30 36.9(2) . . . . ? C1 Mo1 C26 C31 -29.8(3) . . . . ? C2 Mo1 C26 C31 58.5(3) . . . . ? N1 Mo1 C26 C31 87.8(3) . . . . ? C30 Mo1 C26 C31 -120.2(4) . . . . ? C27 Mo1 C26 C31 124.6(4) . . . . ? C29 Mo1 C26 C31 -157.5(3) . . . . ? C28 Mo1 C26 C31 161.5(3) . . . . ? Si2 Mo1 C26 C31 -83.3(3) . . . . ? C30 C26 C27 C28 0.0(3) . . . . ? C31 C26 C27 C28 171.5(3) . . . . ? Mo1 C26 C27 C28 -65.22(18) . . . . ? C30 C26 C27 C32 -175.6(3) . . . . ? C31 C26 C27 C32 -4.1(5) . . . . ? Mo1 C26 C27 C32 119.2(3) . . . . ? C30 C26 C27 Mo1 65.19(19) . . . . ? C31 C26 C27 Mo1 -123.3(3) . . . . ? C1 Mo1 C27 C28 147.70(18) . . . . ? C2 Mo1 C27 C28 -126.42(18) . . . . ? N1 Mo1 C27 C28 -93.29(17) . . . . ? C26 Mo1 C27 C28 116.2(2) . . . . ? C30 Mo1 C27 C28 77.87(18) . . . . ? C29 Mo1 C27 C28 36.79(17) . . . . ? Si2 Mo1 C27 C28 27.9(3) . . . . ? C1 Mo1 C27 C26 31.5(2) . . . . ? C2 Mo1 C27 C26 117.40(18) . . . . ? N1 Mo1 C27 C26 150.53(17) . . . . ? C30 Mo1 C27 C26 -38.31(17) . . . . ? C29 Mo1 C27 C26 -79.38(18) . . . . ? C28 Mo1 C27 C26 -116.2(2) . . . . ? Si2 Mo1 C27 C26 -88.3(3) . . . . ? C1 Mo1 C27 C32 -90.1(3) . . . . ? C2 Mo1 C27 C32 -4.2(3) . . . . ? N1 Mo1 C27 C32 28.9(3) . . . . ? C26 Mo1 C27 C32 -121.6(3) . . . . ? C30 Mo1 C27 C32 -159.9(3) . . . . ? C29 Mo1 C27 C32 159.0(3) . . . . ? C28 Mo1 C27 C32 122.2(3) . . . . ? Si2 Mo1 C27 C32 150.1(2) . . . . ? C26 C27 C28 C29 -0.4(3) . . . . ? C32 C27 C28 C29 175.3(2) . . . . ? Mo1 C27 C28 C29 -63.20(19) . . . . ? C26 C27 C28 C33 -175.5(3) . . . . ? C32 C27 C28 C33 0.2(4) . . . . ? Mo1 C27 C28 C33 121.7(3) . . . . ? C26 C27 C28 Mo1 62.81(17) . . . . ? C32 C27 C28 Mo1 -121.5(3) . . . . ? C1 Mo1 C28 C27 -60.8(3) . . . . ? C2 Mo1 C28 C27 57.78(19) . . . . ? N1 Mo1 C28 C27 90.00(17) . . . . ? C26 Mo1 C28 C27 -37.94(16) . . . . ? C30 Mo1 C28 C27 -80.50(18) . . . . ? C29 Mo1 C28 C27 -116.9(2) . . . . ? Si2 Mo1 C28 C27 -169.56(14) . . . . ? C1 Mo1 C28 C29 56.1(3) . . . . ? C2 Mo1 C28 C29 174.70(17) . . . . ? N1 Mo1 C28 C29 -153.08(17) . . . . ? C26 Mo1 C28 C29 78.98(18) . . . . ? C30 Mo1 C28 C29 36.42(16) . . . . ? C27 Mo1 C28 C29 116.9(2) . . . . ? Si2 Mo1 C28 C29 -52.64(19) . . . . ? C1 Mo1 C28 C33 179.0(3) . . . . ? C2 Mo1 C28 C33 -62.5(3) . . . . ? N1 Mo1 C28 C33 -30.2(3) . . . . ? C26 Mo1 C28 C33 -158.2(3) . . . . ? C30 Mo1 C28 C33 159.3(3) . . . . ? C27 Mo1 C28 C33 -120.2(4) . . . . ? C29 Mo1 C28 C33 122.8(4) . . . . ? Si2 Mo1 C28 C33 70.2(3) . . . . ? C27 C28 C29 C30 0.7(3) . . . . ? C33 C28 C29 C30 175.7(3) . . . . ? Mo1 C28 C29 C30 -61.6(2) . . . . ? C27 C28 C29 C34 -176.9(3) . . . . ? C33 C28 C29 C34 -1.8(5) . . . . ? Mo1 C28 C29 C34 120.9(3) . . . . ? C27 C28 C29 Mo1 62.23(18) . . . . ? C33 C28 C29 Mo1 -122.7(3) . . . . ? C1 Mo1 C29 C30 -32.2(2) . . . . ? C2 Mo1 C29 C30 109.5(2) . . . . ? N1 Mo1 C29 C30 151.71(16) . . . . ? C26 Mo1 C29 C30 38.54(17) . . . . ? C27 Mo1 C29 C30 80.92(19) . . . . ? C28 Mo1 C29 C30 117.8(3) . . . . ? Si2 Mo1 C29 C30 -101.83(17) . . . . ? C1 Mo1 C29 C28 -149.95(17) . . . . ? C2 Mo1 C29 C28 -8.3(3) . . . . ? N1 Mo1 C29 C28 33.9(2) . . . . ? C26 Mo1 C29 C28 -79.26(18) . . . . ? C30 Mo1 C29 C28 -117.8(3) . . . . ? C27 Mo1 C29 C28 -36.88(16) . . . . ? Si2 Mo1 C29 C28 140.37(16) . . . . ? C1 Mo1 C29 C34 88.5(3) . . . . ? C2 Mo1 C29 C34 -129.9(3) . . . . ? N1 Mo1 C29 C34 -87.6(3) . . . . ? C26 Mo1 C29 C34 159.2(3) . . . . ? C30 Mo1 C29 C34 120.7(3) . . . . ? C27 Mo1 C29 C34 -158.4(3) . . . . ? C28 Mo1 C29 C34 -121.5(3) . . . . ? Si2 Mo1 C29 C34 18.8(3) . . . . ? C28 C29 C30 C26 -0.7(3) . . . . ? C34 C29 C30 C26 176.8(3) . . . . ? Mo1 C29 C30 C26 -63.76(19) . . . . ? C28 C29 C30 C35 -173.2(3) . . . . ? C34 C29 C30 C35 4.3(5) . . . . ? Mo1 C29 C30 C35 123.7(3) . . . . ? C28 C29 C30 Mo1 63.1(2) . . . . ? C34 C29 C30 Mo1 -119.4(3) . . . . ? C27 C26 C30 C29 0.4(3) . . . . ? C31 C26 C30 C29 -171.4(3) . . . . ? Mo1 C26 C30 C29 66.1(2) . . . . ? C27 C26 C30 C35 173.4(3) . . . . ? C31 C26 C30 C35 1.5(5) . . . . ? Mo1 C26 C30 C35 -120.9(3) . . . . ? C27 C26 C30 Mo1 -65.69(19) . . . . ? C31 C26 C30 Mo1 122.5(3) . . . . ? C1 Mo1 C30 C29 153.50(19) . . . . ? C2 Mo1 C30 C29 -117.2(2) . . . . ? N1 Mo1 C30 C29 -57.6(3) . . . . ? C26 Mo1 C30 C29 -115.4(3) . . . . ? C27 Mo1 C30 C29 -77.29(19) . . . . ? C28 Mo1 C30 C29 -36.31(17) . . . . ? Si2 Mo1 C30 C29 88.64(18) . . . . ? C1 Mo1 C30 C26 -91.14(18) . . . . ? C2 Mo1 C30 C26 -1.9(3) . . . . ? N1 Mo1 C30 C26 57.8(3) . . . . ? C27 Mo1 C30 C26 38.06(17) . . . . ? C29 Mo1 C30 C26 115.4(3) . . . . ? C28 Mo1 C30 C26 79.04(18) . . . . ? Si2 Mo1 C30 C26 -156.00(15) . . . . ? C1 Mo1 C30 C35 27.6(3) . . . . ? C2 Mo1 C30 C35 116.8(3) . . . . ? N1 Mo1 C30 C35 176.5(2) . . . . ? C26 Mo1 C30 C35 118.7(3) . . . . ? C27 Mo1 C30 C35 156.8(3) . . . . ? C29 Mo1 C30 C35 -125.9(3) . . . . ? C28 Mo1 C30 C35 -162.3(3) . . . . ? Si2 Mo1 C30 C35 -37.3(3) . . . . ? #===END data_compound-5b #TrackingRef '- cif.cif' _database_code_depnum_ccdc_archive 'CCDC 789740' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H45 N O2 Si2 W' _chemical_formula_sum 'C37 H45 N O2 Si2 W' _chemical_formula_weight 775.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 21.5695(7) _cell_length_b 8.7738(2) _cell_length_c 21.5198(7) _cell_angle_alpha 90.00 _cell_angle_beta 124.2959(12) _cell_angle_gamma 90.00 _cell_volume 3364.49(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20975 _cell_measurement_theta_min 1.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 3.538 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.451600 _exptl_absorpt_correction_T_max 0.784820 _exptl_absorpt_process_details ; HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera. Rigaku Corporation, Tokyo, Japan. HIGASHI, T. (1999). Numabs - Numerical Absorption Correction, Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _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 25937 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _reflns_number_total 7306 _reflns_number_gt 6724 _reflns_threshold_expression >2\s(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+6.9201P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 7306 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.789 _refine_diff_density_min -2.521 _refine_diff_density_rms 0.213 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 0.015141(9) 0.192900(18) 0.196233(9) 0.01406(8) Uani 1 1 d . . . Si1 Si 0.02096(7) 0.38450(14) 0.34822(7) 0.0171(2) Uani 1 1 d . . . Si2 Si 0.15956(7) 0.16024(15) 0.28824(7) 0.0174(2) Uani 1 1 d . . . O1 O 0.0605(2) 0.5204(4) 0.1786(2) 0.0401(10) Uani 1 1 d . . . O2 O 0.14664(18) 0.1549(4) 0.42210(18) 0.0187(6) Uani 1 1 d . . . N1 N 0.0113(2) 0.2559(4) 0.2808(2) 0.0158(7) Uani 1 1 d . . . C1 C 0.0443(3) 0.4014(5) 0.1882(3) 0.0212(9) Uani 1 1 d . . . C2 C -0.0067(2) 0.0975(5) 0.2754(2) 0.0169(8) Uani 1 1 d . . . H1 H 0.032(3) 0.026(6) 0.318(3) 0.015(12) Uiso 1 1 d . . . C3 C -0.0833(2) 0.0522(5) 0.2534(2) 0.0171(8) Uani 1 1 d . . . C4 C -0.0951(3) -0.0941(5) 0.2706(3) 0.0204(9) Uani 1 1 d . . . H2 H -0.0543 -0.1638 0.2953 0.025 Uiso 1 1 calc R . . C5 C -0.1657(3) -0.1398(6) 0.2521(3) 0.0290(11) Uani 1 1 d . . . H3 H -0.1725 -0.2399 0.2641 0.035 Uiso 1 1 calc R . . C6 C -0.2253(3) -0.0404(7) 0.2165(3) 0.0303(11) Uani 1 1 d . . . H4 H -0.2732 -0.0716 0.2041 0.036 Uiso 1 1 calc R . . C7 C -0.2153(3) 0.1065(6) 0.1988(3) 0.0300(11) Uani 1 1 d . . . H5 H -0.2563 0.1754 0.1740 0.036 Uiso 1 1 calc R . . C8 C -0.1449(3) 0.1513(6) 0.2177(3) 0.0226(9) Uani 1 1 d . . . H6 H -0.1383 0.2519 0.2060 0.027 Uiso 1 1 calc R . . C9 C -0.0728(3) 0.4579(6) 0.3211(3) 0.0282(11) Uani 1 1 d . . . H7 H -0.0992 0.5024 0.2706 0.042 Uiso 1 1 calc R . . H8 H -0.0657 0.5360 0.3571 0.042 Uiso 1 1 calc R . . H9 H -0.1025 0.3737 0.3214 0.042 Uiso 1 1 calc R . . C10 C 0.0751(3) 0.5561(6) 0.3557(3) 0.0337(12) Uani 1 1 d . . . H10 H 0.1277 0.5281 0.3788 0.051 Uiso 1 1 calc R . . H11 H 0.0718 0.6329 0.3868 0.051 Uiso 1 1 calc R . . H12 H 0.0543 0.5978 0.3053 0.051 Uiso 1 1 calc R . . C11 C 0.0594(3) 0.2761(5) 0.4383(2) 0.0188(9) Uani 1 1 d . . . C12 C 0.0289(3) 0.2924(6) 0.4798(3) 0.0262(11) Uani 1 1 d . . . H13 H -0.0083 0.3681 0.4659 0.031 Uiso 1 1 calc R . . C13 C 0.0517(4) 0.2001(6) 0.5413(3) 0.0312(13) Uani 1 1 d . . . H14 H 0.0314 0.2159 0.5702 0.037 Uiso 1 1 calc R . . C14 C 0.1033(3) 0.0856(6) 0.5612(3) 0.0280(10) Uani 1 1 d . . . H15 H 0.1172 0.0220 0.6029 0.034 Uiso 1 1 calc R . . C15 C 0.1356(3) 0.0617(5) 0.5213(2) 0.0201(9) Uani 1 1 d . . . C16 C 0.1147(3) 0.1618(5) 0.4618(2) 0.0174(8) Uani 1 1 d . . . C17 C 0.1922(3) -0.0660(5) 0.5417(2) 0.0199(9) Uani 1 1 d . . . C18 C 0.1631(4) -0.2139(6) 0.5546(3) 0.0315(12) Uani 1 1 d . . . H16 H 0.1135 -0.2380 0.5096 0.047 Uiso 1 1 calc R . . H17 H 0.1593 -0.2009 0.5976 0.047 Uiso 1 1 calc R . . H18 H 0.1980 -0.2972 0.5650 0.047 Uiso 1 1 calc R . . C19 C 0.2680(3) -0.0240(7) 0.6142(3) 0.0324(12) Uani 1 1 d . . . H19 H 0.3038 -0.1071 0.6278 0.049 Uiso 1 1 calc R . . H20 H 0.2611 -0.0078 0.6550 0.049 Uiso 1 1 calc R . . H21 H 0.2872 0.0696 0.6060 0.049 Uiso 1 1 calc R . . C20 C 0.1804(2) 0.0197(5) 0.4221(2) 0.0151(8) Uani 1 1 d . . . C21 C 0.2033(2) -0.0889(5) 0.4785(2) 0.0182(8) Uani 1 1 d . . . C22 C 0.2394(3) -0.2169(5) 0.4757(3) 0.0247(10) Uani 1 1 d . . . H22 H 0.2567 -0.2925 0.5137 0.030 Uiso 1 1 calc R . . C23 C 0.2510(3) -0.2375(6) 0.4190(3) 0.0264(10) Uani 1 1 d . . . H23 H 0.2758 -0.3262 0.4182 0.032 Uiso 1 1 calc R . . C24 C 0.2258(3) -0.1265(6) 0.3631(3) 0.0253(10) Uani 1 1 d . . . H24 H 0.2333 -0.1419 0.3241 0.030 Uiso 1 1 calc R . . C25 C 0.1899(2) 0.0067(5) 0.3628(3) 0.0175(8) Uani 1 1 d . . . C26 C 0.2074(3) 0.3392(6) 0.3450(3) 0.0265(10) Uani 1 1 d . . . H25 H 0.1888 0.3630 0.3762 0.040 Uiso 1 1 calc R . . H26 H 0.1964 0.4243 0.3107 0.040 Uiso 1 1 calc R . . H27 H 0.2618 0.3226 0.3773 0.040 Uiso 1 1 calc R . . C27 C 0.2222(3) 0.1245(7) 0.2536(3) 0.0320(12) Uani 1 1 d . . . H28 H 0.2743 0.1128 0.2969 0.048 Uiso 1 1 calc R . . H29 H 0.2187 0.2109 0.2229 0.048 Uiso 1 1 calc R . . H30 H 0.2060 0.0312 0.2233 0.048 Uiso 1 1 calc R . . C28 C -0.0404(3) -0.0235(5) 0.1163(3) 0.0218(9) Uani 1 1 d . . . C29 C 0.0279(3) 0.0066(5) 0.1232(2) 0.0218(9) Uani 1 1 d . . . C30 C 0.0223(3) 0.1551(6) 0.0925(3) 0.0241(10) Uani 1 1 d . . . C31 C -0.0501(3) 0.2158(6) 0.0666(3) 0.0243(10) Uani 1 1 d . . . C32 C -0.0885(3) 0.1054(5) 0.0815(2) 0.0214(9) Uani 1 1 d . . . C33 C -0.0601(3) -0.1723(5) 0.1354(3) 0.0276(11) Uani 1 1 d . . . H31 H -0.0770 -0.2446 0.0941 0.041 Uiso 1 1 calc R . . H32 H -0.1003 -0.1561 0.1430 0.041 Uiso 1 1 calc R . . H33 H -0.0157 -0.2135 0.1815 0.041 Uiso 1 1 calc R . . C34 C 0.0845(3) -0.1162(6) 0.1408(3) 0.0313(11) Uani 1 1 d . . . H34 H 0.1122 -0.1425 0.1943 0.047 Uiso 1 1 calc R . . H35 H 0.1196 -0.0792 0.1290 0.047 Uiso 1 1 calc R . . H36 H 0.0584 -0.2068 0.1104 0.047 Uiso 1 1 calc R . . C35 C 0.0735(4) 0.2223(8) 0.0723(3) 0.0381(13) Uani 1 1 d . . . H37 H 0.0544 0.1962 0.0202 0.057 Uiso 1 1 calc R . . H38 H 0.1242 0.1808 0.1060 0.057 Uiso 1 1 calc R . . H39 H 0.0750 0.3334 0.0777 0.057 Uiso 1 1 calc R . . C36 C -0.0854(4) 0.3587(7) 0.0201(3) 0.0361(13) Uani 1 1 d . . . H40 H -0.1133 0.3330 -0.0335 0.054 Uiso 1 1 calc R . . H41 H -0.0461 0.4327 0.0324 0.054 Uiso 1 1 calc R . . H42 H -0.1199 0.4028 0.0313 0.054 Uiso 1 1 calc R . . C37 C -0.1695(3) 0.1136(6) 0.0562(3) 0.0277(11) Uani 1 1 d . . . H43 H -0.1817 0.2184 0.0614 0.042 Uiso 1 1 calc R . . H44 H -0.1773 0.0456 0.0873 0.042 Uiso 1 1 calc R . . H45 H -0.2021 0.0821 0.0034 0.042 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 0.01585(12) 0.01364(12) 0.01318(12) 0.00022(5) 0.00848(9) -0.00040(5) Si1 0.0191(6) 0.0157(6) 0.0161(6) -0.0026(4) 0.0097(5) 0.0020(4) Si2 0.0170(6) 0.0207(6) 0.0174(6) 0.0006(5) 0.0115(5) -0.0009(5) O1 0.051(3) 0.0210(19) 0.045(2) 0.0061(16) 0.025(2) -0.0043(17) O2 0.0197(16) 0.0211(15) 0.0192(16) 0.0048(13) 0.0134(14) 0.0057(13) N1 0.0183(18) 0.0175(18) 0.0128(17) -0.0057(14) 0.0094(15) -0.0016(14) C1 0.027(2) 0.020(2) 0.019(2) 0.0032(17) 0.015(2) 0.0039(18) C2 0.017(2) 0.017(2) 0.0146(19) 0.0054(15) 0.0074(18) 0.0009(16) C3 0.020(2) 0.021(2) 0.014(2) -0.0044(15) 0.0122(18) -0.0004(16) C4 0.029(2) 0.021(2) 0.020(2) -0.0026(17) 0.019(2) -0.0008(18) C5 0.037(3) 0.032(3) 0.029(3) -0.010(2) 0.024(2) -0.013(2) C6 0.022(2) 0.045(3) 0.029(3) -0.012(2) 0.017(2) -0.012(2) C7 0.022(2) 0.039(3) 0.028(3) -0.008(2) 0.014(2) 0.001(2) C8 0.022(2) 0.026(2) 0.019(2) -0.0014(18) 0.011(2) 0.0026(19) C9 0.026(3) 0.029(3) 0.024(2) -0.0031(19) 0.011(2) 0.011(2) C10 0.042(3) 0.019(2) 0.044(3) -0.011(2) 0.027(3) -0.008(2) C11 0.022(2) 0.021(2) 0.015(2) 0.0009(16) 0.0116(19) 0.0029(17) C12 0.025(3) 0.028(3) 0.024(3) -0.0044(18) 0.013(2) 0.0071(18) C13 0.044(4) 0.040(3) 0.021(3) 0.0000(19) 0.025(3) 0.006(2) C14 0.031(3) 0.034(3) 0.018(2) 0.0046(19) 0.014(2) 0.001(2) C15 0.024(2) 0.024(2) 0.0119(19) -0.0038(16) 0.0097(19) -0.0012(17) C16 0.020(2) 0.023(2) 0.0108(19) -0.0058(16) 0.0096(18) -0.0015(17) C17 0.020(2) 0.022(2) 0.015(2) 0.0027(16) 0.0084(18) -0.0017(17) C18 0.041(3) 0.026(3) 0.035(3) 0.004(2) 0.026(3) 0.001(2) C19 0.030(3) 0.040(3) 0.018(2) 0.000(2) 0.008(2) 0.000(2) C20 0.014(2) 0.0147(19) 0.016(2) 0.0001(15) 0.0082(18) 0.0012(15) C21 0.016(2) 0.019(2) 0.017(2) -0.0018(16) 0.0081(18) 0.0006(16) C22 0.024(3) 0.019(2) 0.029(3) 0.0055(18) 0.014(2) 0.0050(18) C23 0.026(3) 0.023(2) 0.032(3) 0.000(2) 0.017(2) 0.0092(19) C24 0.024(2) 0.028(3) 0.028(3) -0.0012(19) 0.017(2) 0.0022(19) C25 0.014(2) 0.019(2) 0.020(2) 0.0014(16) 0.0108(18) 0.0012(16) C26 0.022(2) 0.026(2) 0.032(3) -0.002(2) 0.015(2) -0.0052(19) C27 0.023(3) 0.043(3) 0.036(3) -0.001(2) 0.021(2) -0.002(2) C28 0.022(2) 0.017(2) 0.020(2) -0.0025(16) 0.008(2) -0.0037(17) C29 0.029(3) 0.026(2) 0.013(2) -0.0048(17) 0.013(2) -0.0002(18) C30 0.031(3) 0.024(2) 0.020(2) 0.0017(18) 0.015(2) -0.007(2) C31 0.032(3) 0.025(2) 0.013(2) 0.0018(17) 0.011(2) -0.0020(19) C32 0.023(2) 0.025(2) 0.015(2) -0.0042(17) 0.0100(19) -0.0019(18) C33 0.035(3) 0.018(2) 0.031(3) -0.0059(19) 0.020(2) -0.0066(19) C34 0.033(3) 0.023(3) 0.040(3) -0.007(2) 0.022(3) 0.003(2) C35 0.044(4) 0.048(3) 0.033(3) 0.002(3) 0.029(3) -0.011(3) C36 0.045(3) 0.030(3) 0.022(2) 0.007(2) 0.012(3) 0.001(2) C37 0.019(2) 0.040(3) 0.019(2) -0.009(2) 0.008(2) -0.001(2) _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 N1 1.948(3) . ? W1 C1 1.974(5) . ? W1 C2 2.175(4) . ? W1 C31 2.320(5) . ? W1 C32 2.337(4) . ? W1 C30 2.345(5) . ? W1 C28 2.382(4) . ? W1 C29 2.387(4) . ? W1 Si2 2.5991(13) . ? Si1 N1 1.755(4) . ? Si1 C10 1.856(5) . ? Si1 C9 1.874(5) . ? Si1 C11 1.881(5) . ? Si2 C26 1.897(5) . ? Si2 C27 1.901(5) . ? Si2 C25 1.906(5) . ? O1 C1 1.156(6) . ? O2 C16 1.367(5) . ? O2 C20 1.391(5) . ? N1 C2 1.430(6) . ? C2 C3 1.493(6) . ? C2 H1 1.03(5) . ? C3 C4 1.398(6) . ? C3 C8 1.401(6) . ? C4 C5 1.398(7) . ? C4 H2 0.9500 . ? C5 C6 1.376(8) . ? C5 H3 0.9500 . ? C6 C7 1.395(8) . ? C6 H4 0.9500 . ? C7 C8 1.389(7) . ? C7 H5 0.9500 . ? C8 H6 0.9500 . ? C9 H7 0.9800 . ? C9 H8 0.9800 . ? C9 H9 0.9800 . ? C10 H10 0.9800 . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C11 C12 1.383(7) . ? C11 C16 1.417(6) . ? C12 C13 1.384(7) . ? C12 H13 0.9500 . ? C13 C14 1.377(8) . ? C13 H14 0.9500 . ? C14 C15 1.394(7) . ? C14 H15 0.9500 . ? C15 C16 1.401(6) . ? C15 C17 1.527(6) . ? C17 C21 1.522(6) . ? C17 C18 1.534(7) . ? C17 C19 1.540(7) . ? C18 H16 0.9800 . ? C18 H17 0.9800 . ? C18 H18 0.9800 . ? C19 H19 0.9800 . ? C19 H20 0.9800 . ? C19 H21 0.9800 . ? C20 C21 1.395(6) . ? C20 C25 1.408(6) . ? C21 C22 1.386(6) . ? C22 C23 1.388(7) . ? C22 H22 0.9500 . ? C23 C24 1.398(7) . ? C23 H23 0.9500 . ? C24 C25 1.400(6) . ? C24 H24 0.9500 . ? C26 H25 0.9800 . ? C26 H26 0.9800 . ? C26 H27 0.9800 . ? C27 H28 0.9800 . ? C27 H29 0.9800 . ? C27 H30 0.9800 . ? C28 C29 1.418(7) . ? C28 C32 1.428(7) . ? C28 C33 1.500(7) . ? C29 C30 1.435(7) . ? C29 C34 1.509(7) . ? C30 C31 1.432(8) . ? C30 C35 1.517(7) . ? C31 C32 1.424(7) . ? C31 C36 1.514(7) . ? C32 C37 1.510(7) . ? C33 H31 0.9800 . ? C33 H32 0.9800 . ? C33 H33 0.9800 . ? C34 H34 0.9800 . ? C34 H35 0.9800 . ? C34 H36 0.9800 . ? C35 H37 0.9800 . ? C35 H38 0.9800 . ? C35 H39 0.9800 . ? C36 H40 0.9800 . ? C36 H41 0.9800 . ? C36 H42 0.9800 . ? C37 H43 0.9800 . ? C37 H44 0.9800 . ? C37 H45 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 N1 W1 C1 90.12(18) . . ? N1 W1 C2 40.12(17) . . ? C1 W1 C2 130.23(18) . . ? N1 W1 C31 141.50(18) . . ? C1 W1 C31 79.73(18) . . ? C2 W1 C31 136.31(18) . . ? N1 W1 C32 124.13(16) . . ? C1 W1 C32 112.00(18) . . ? C2 W1 C32 101.56(17) . . ? C31 W1 C32 35.61(17) . . ? N1 W1 C30 171.58(17) . . ? C1 W1 C30 81.53(18) . . ? C2 W1 C30 148.24(17) . . ? C31 W1 C30 35.76(19) . . ? C32 W1 C30 59.01(17) . . ? N1 W1 C28 129.19(16) . . ? C1 W1 C28 136.96(17) . . ? C2 W1 C28 90.93(17) . . ? C31 W1 C28 58.88(17) . . ? C32 W1 C28 35.21(16) . . ? C30 W1 C28 58.41(17) . . ? N1 W1 C29 152.91(16) . . ? C1 W1 C29 114.61(18) . . ? C2 W1 C29 114.08(16) . . ? C31 W1 C29 58.99(17) . . ? C32 W1 C29 58.41(16) . . ? C30 W1 C29 35.28(17) . . ? C28 W1 C29 34.60(17) . . ? N1 W1 Si2 89.05(11) . . ? C1 W1 Si2 82.21(14) . . ? C2 W1 Si2 93.24(12) . . ? C31 W1 Si2 125.48(14) . . ? C32 W1 Si2 142.27(12) . . ? C30 W1 Si2 90.93(13) . . ? C28 W1 Si2 111.18(12) . . ? C29 W1 Si2 83.86(12) . . ? N1 Si1 C10 111.6(2) . . ? N1 Si1 C9 111.0(2) . . ? C10 Si1 C9 105.3(3) . . ? N1 Si1 C11 107.8(2) . . ? C10 Si1 C11 115.5(2) . . ? C9 Si1 C11 105.4(2) . . ? C26 Si2 C27 98.0(2) . . ? C26 Si2 C25 103.8(2) . . ? C27 Si2 C25 103.3(2) . . ? C26 Si2 W1 112.51(17) . . ? C27 Si2 W1 122.10(18) . . ? C25 Si2 W1 114.50(14) . . ? C16 O2 C20 118.9(3) . . ? C2 N1 Si1 126.3(3) . . ? C2 N1 W1 78.5(2) . . ? Si1 N1 W1 155.1(2) . . ? O1 C1 W1 175.0(4) . . ? N1 C2 C3 119.1(4) . . ? N1 C2 W1 61.4(2) . . ? C3 C2 W1 123.0(3) . . ? N1 C2 H1 118(3) . . ? C3 C2 H1 108(3) . . ? W1 C2 H1 121(3) . . ? C4 C3 C8 117.3(4) . . ? C4 C3 C2 119.6(4) . . ? C8 C3 C2 123.1(4) . . ? C5 C4 C3 121.3(5) . . ? C5 C4 H2 119.4 . . ? C3 C4 H2 119.4 . . ? C6 C5 C4 120.2(5) . . ? C6 C5 H3 119.9 . . ? C4 C5 H3 119.9 . . ? C5 C6 C7 119.8(5) . . ? C5 C6 H4 120.1 . . ? C7 C6 H4 120.1 . . ? C8 C7 C6 119.6(5) . . ? C8 C7 H5 120.2 . . ? C6 C7 H5 120.2 . . ? C7 C8 C3 121.8(5) . . ? C7 C8 H6 119.1 . . ? C3 C8 H6 119.1 . . ? Si1 C9 H7 109.5 . . ? Si1 C9 H8 109.5 . . ? H7 C9 H8 109.5 . . ? Si1 C9 H9 109.5 . . ? H7 C9 H9 109.5 . . ? H8 C9 H9 109.5 . . ? Si1 C10 H10 109.5 . . ? Si1 C10 H11 109.5 . . ? H10 C10 H11 109.5 . . ? Si1 C10 H12 109.5 . . ? H10 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C12 C11 C16 117.0(4) . . ? C12 C11 Si1 121.3(4) . . ? C16 C11 Si1 121.3(3) . . ? C11 C12 C13 121.0(5) . . ? C11 C12 H13 119.5 . . ? C13 C12 H13 119.5 . . ? C14 C13 C12 120.9(5) . . ? C14 C13 H14 119.6 . . ? C12 C13 H14 119.6 . . ? C13 C14 C15 121.0(5) . . ? C13 C14 H15 119.5 . . ? C15 C14 H15 119.5 . . ? C14 C15 C16 117.0(4) . . ? C14 C15 C17 121.9(4) . . ? C16 C15 C17 121.0(4) . . ? O2 C16 C15 121.9(4) . . ? O2 C16 C11 115.3(4) . . ? C15 C16 C11 122.8(4) . . ? C21 C17 C15 110.1(4) . . ? C21 C17 C18 109.7(4) . . ? C15 C17 C18 109.3(4) . . ? C21 C17 C19 109.0(4) . . ? C15 C17 C19 109.6(4) . . ? C18 C17 C19 109.1(4) . . ? C17 C18 H16 109.5 . . ? C17 C18 H17 109.5 . . ? H16 C18 H17 109.5 . . ? C17 C18 H18 109.5 . . ? H16 C18 H18 109.5 . . ? H17 C18 H18 109.5 . . ? C17 C19 H19 109.5 . . ? C17 C19 H20 109.5 . . ? H19 C19 H20 109.5 . . ? C17 C19 H21 109.5 . . ? H19 C19 H21 109.5 . . ? H20 C19 H21 109.5 . . ? O2 C20 C21 120.8(4) . . ? O2 C20 C25 114.3(4) . . ? C21 C20 C25 124.8(4) . . ? C22 C21 C20 116.7(4) . . ? C22 C21 C17 121.3(4) . . ? C20 C21 C17 121.9(4) . . ? C21 C22 C23 121.7(5) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C22 C23 C24 119.4(4) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C23 C24 C25 122.1(5) . . ? C23 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C24 C25 C20 115.2(4) . . ? C24 C25 Si2 121.4(3) . . ? C20 C25 Si2 123.4(3) . . ? Si2 C26 H25 109.5 . . ? Si2 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? Si2 C26 H27 109.5 . . ? H25 C26 H27 109.5 . . ? H26 C26 H27 109.5 . . ? Si2 C27 H28 109.5 . . ? Si2 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? Si2 C27 H30 109.5 . . ? H28 C27 H30 109.5 . . ? H29 C27 H30 109.5 . . ? C29 C28 C32 108.2(4) . . ? C29 C28 C33 124.8(5) . . ? C32 C28 C33 126.8(4) . . ? C29 C28 W1 72.9(3) . . ? C32 C28 W1 70.7(3) . . ? C33 C28 W1 126.9(3) . . ? C28 C29 C30 107.9(4) . . ? C28 C29 C34 122.6(4) . . ? C30 C29 C34 127.6(5) . . ? C28 C29 W1 72.5(3) . . ? C30 C29 W1 70.8(3) . . ? C34 C29 W1 134.5(3) . . ? C31 C30 C29 107.9(4) . . ? C31 C30 C35 123.6(5) . . ? C29 C30 C35 126.8(5) . . ? C31 C30 W1 71.1(3) . . ? C29 C30 W1 74.0(3) . . ? C35 C30 W1 131.8(4) . . ? C32 C31 C30 107.7(4) . . ? C32 C31 C36 124.9(5) . . ? C30 C31 C36 126.7(5) . . ? C32 C31 W1 72.9(3) . . ? C30 C31 W1 73.1(3) . . ? C36 C31 W1 127.2(4) . . ? C31 C32 C28 108.3(4) . . ? C31 C32 C37 126.0(5) . . ? C28 C32 C37 125.3(4) . . ? C31 C32 W1 71.5(3) . . ? C28 C32 W1 74.1(3) . . ? C37 C32 W1 126.1(3) . . ? C28 C33 H31 109.5 . . ? C28 C33 H32 109.5 . . ? H31 C33 H32 109.5 . . ? C28 C33 H33 109.5 . . ? H31 C33 H33 109.5 . . ? H32 C33 H33 109.5 . . ? C29 C34 H34 109.5 . . ? C29 C34 H35 109.5 . . ? H34 C34 H35 109.5 . . ? C29 C34 H36 109.5 . . ? H34 C34 H36 109.5 . . ? H35 C34 H36 109.5 . . ? C30 C35 H37 109.5 . . ? C30 C35 H38 109.5 . . ? H37 C35 H38 109.5 . . ? C30 C35 H39 109.5 . . ? H37 C35 H39 109.5 . . ? H38 C35 H39 109.5 . . ? C31 C36 H40 109.5 . . ? C31 C36 H41 109.5 . . ? H40 C36 H41 109.5 . . ? C31 C36 H42 109.5 . . ? H40 C36 H42 109.5 . . ? H41 C36 H42 109.5 . . ? C32 C37 H43 109.5 . . ? C32 C37 H44 109.5 . . ? H43 C37 H44 109.5 . . ? C32 C37 H45 109.5 . . ? H43 C37 H45 109.5 . . ? H44 C37 H45 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 N1 W1 Si2 C26 -54.6(2) . . . . ? C1 W1 Si2 C26 35.7(2) . . . . ? C2 W1 Si2 C26 -94.5(2) . . . . ? C31 W1 Si2 C26 107.1(2) . . . . ? C32 W1 Si2 C26 151.9(3) . . . . ? C30 W1 Si2 C26 117.0(2) . . . . ? C28 W1 Si2 C26 173.3(2) . . . . ? C29 W1 Si2 C26 151.6(2) . . . . ? N1 W1 Si2 C27 -170.6(3) . . . . ? C1 W1 Si2 C27 -80.3(3) . . . . ? C2 W1 Si2 C27 149.5(3) . . . . ? C31 W1 Si2 C27 -8.9(3) . . . . ? C32 W1 Si2 C27 35.9(3) . . . . ? C30 W1 Si2 C27 1.0(3) . . . . ? C28 W1 Si2 C27 57.3(3) . . . . ? C29 W1 Si2 C27 35.6(3) . . . . ? N1 W1 Si2 C25 63.7(2) . . . . ? C1 W1 Si2 C25 153.9(2) . . . . ? C2 W1 Si2 C25 23.7(2) . . . . ? C31 W1 Si2 C25 -134.7(2) . . . . ? C32 W1 Si2 C25 -89.9(3) . . . . ? C30 W1 Si2 C25 -124.8(2) . . . . ? C28 W1 Si2 C25 -68.5(2) . . . . ? C29 W1 Si2 C25 -90.1(2) . . . . ? C10 Si1 N1 C2 160.4(4) . . . . ? C9 Si1 N1 C2 -82.4(4) . . . . ? C11 Si1 N1 C2 32.6(4) . . . . ? C10 Si1 N1 W1 -14.3(6) . . . . ? C9 Si1 N1 W1 102.9(6) . . . . ? C11 Si1 N1 W1 -142.1(5) . . . . ? C1 W1 N1 C2 -178.4(3) . . . . ? C31 W1 N1 C2 108.1(3) . . . . ? C32 W1 N1 C2 64.6(3) . . . . ? C28 W1 N1 C2 20.7(3) . . . . ? C29 W1 N1 C2 -21.7(5) . . . . ? Si2 W1 N1 C2 -96.2(2) . . . . ? C1 W1 N1 Si1 -2.7(6) . . . . ? C2 W1 N1 Si1 175.6(7) . . . . ? C31 W1 N1 Si1 -76.3(6) . . . . ? C32 W1 N1 Si1 -119.7(5) . . . . ? C28 W1 N1 Si1 -163.6(5) . . . . ? C29 W1 N1 Si1 154.0(4) . . . . ? Si2 W1 N1 Si1 79.5(5) . . . . ? Si1 N1 C2 C3 68.3(5) . . . . ? W1 N1 C2 C3 -113.9(4) . . . . ? Si1 N1 C2 W1 -177.7(4) . . . . ? C1 W1 C2 N1 2.1(3) . . . . ? C31 W1 C2 N1 -121.1(3) . . . . ? C32 W1 C2 N1 -130.2(2) . . . . ? C30 W1 C2 N1 -178.3(3) . . . . ? C28 W1 C2 N1 -164.1(2) . . . . ? C29 W1 C2 N1 169.4(2) . . . . ? Si2 W1 C2 N1 84.7(2) . . . . ? N1 W1 C2 C3 107.8(4) . . . . ? C1 W1 C2 C3 109.9(4) . . . . ? C31 W1 C2 C3 -13.3(5) . . . . ? C32 W1 C2 C3 -22.4(4) . . . . ? C30 W1 C2 C3 -70.5(5) . . . . ? C28 W1 C2 C3 -56.3(4) . . . . ? C29 W1 C2 C3 -82.8(4) . . . . ? Si2 W1 C2 C3 -167.5(3) . . . . ? N1 C2 C3 C4 -159.6(4) . . . . ? W1 C2 C3 C4 127.4(4) . . . . ? N1 C2 C3 C8 18.6(6) . . . . ? W1 C2 C3 C8 -54.4(5) . . . . ? C8 C3 C4 C5 0.6(6) . . . . ? C2 C3 C4 C5 178.9(4) . . . . ? C3 C4 C5 C6 -0.2(7) . . . . ? C4 C5 C6 C7 0.1(7) . . . . ? C5 C6 C7 C8 -0.4(8) . . . . ? C6 C7 C8 C3 0.8(7) . . . . ? C4 C3 C8 C7 -0.9(7) . . . . ? C2 C3 C8 C7 -179.1(4) . . . . ? N1 Si1 C11 C12 -133.8(4) . . . . ? C10 Si1 C11 C12 100.6(5) . . . . ? C9 Si1 C11 C12 -15.2(5) . . . . ? N1 Si1 C11 C16 38.8(4) . . . . ? C10 Si1 C11 C16 -86.8(4) . . . . ? C9 Si1 C11 C16 157.4(4) . . . . ? C16 C11 C12 C13 -0.3(7) . . . . ? Si1 C11 C12 C13 172.7(4) . . . . ? C11 C12 C13 C14 -2.4(9) . . . . ? C12 C13 C14 C15 1.6(9) . . . . ? C13 C14 C15 C16 1.8(8) . . . . ? C13 C14 C15 C17 -179.1(5) . . . . ? C20 O2 C16 C15 22.0(6) . . . . ? C20 O2 C16 C11 -157.7(4) . . . . ? C14 C15 C16 O2 175.6(4) . . . . ? C17 C15 C16 O2 -3.4(7) . . . . ? C14 C15 C16 C11 -4.6(7) . . . . ? C17 C15 C16 C11 176.3(4) . . . . ? C12 C11 C16 O2 -176.4(4) . . . . ? Si1 C11 C16 O2 10.7(6) . . . . ? C12 C11 C16 C15 3.9(7) . . . . ? Si1 C11 C16 C15 -169.1(4) . . . . ? C14 C15 C17 C21 166.5(4) . . . . ? C16 C15 C17 C21 -14.5(6) . . . . ? C14 C15 C17 C18 45.9(6) . . . . ? C16 C15 C17 C18 -135.0(5) . . . . ? C14 C15 C17 C19 -73.6(6) . . . . ? C16 C15 C17 C19 105.4(5) . . . . ? C16 O2 C20 C21 -20.5(6) . . . . ? C16 O2 C20 C25 160.8(4) . . . . ? O2 C20 C21 C22 -177.2(4) . . . . ? C25 C20 C21 C22 1.3(7) . . . . ? O2 C20 C21 C17 0.6(6) . . . . ? C25 C20 C21 C17 179.0(4) . . . . ? C15 C17 C21 C22 -166.5(4) . . . . ? C18 C17 C21 C22 -46.2(6) . . . . ? C19 C17 C21 C22 73.2(6) . . . . ? C15 C17 C21 C20 15.8(6) . . . . ? C18 C17 C21 C20 136.2(5) . . . . ? C19 C17 C21 C20 -104.5(5) . . . . ? C20 C21 C22 C23 -1.1(7) . . . . ? C17 C21 C22 C23 -178.9(5) . . . . ? C21 C22 C23 C24 0.1(8) . . . . ? C22 C23 C24 C25 0.8(8) . . . . ? C23 C24 C25 C20 -0.6(7) . . . . ? C23 C24 C25 Si2 177.5(4) . . . . ? O2 C20 C25 C24 178.1(4) . . . . ? C21 C20 C25 C24 -0.5(7) . . . . ? O2 C20 C25 Si2 0.0(5) . . . . ? C21 C20 C25 Si2 -178.6(3) . . . . ? C26 Si2 C25 C24 -124.1(4) . . . . ? C27 Si2 C25 C24 -22.2(4) . . . . ? W1 Si2 C25 C24 112.9(4) . . . . ? C26 Si2 C25 C20 53.9(4) . . . . ? C27 Si2 C25 C20 155.8(4) . . . . ? W1 Si2 C25 C20 -69.1(4) . . . . ? N1 W1 C28 C29 -147.2(3) . . . . ? C1 W1 C28 C29 61.5(4) . . . . ? C2 W1 C28 C29 -134.0(3) . . . . ? C31 W1 C28 C29 79.3(3) . . . . ? C32 W1 C28 C29 117.0(4) . . . . ? C30 W1 C28 C29 37.2(3) . . . . ? Si2 W1 C28 C29 -40.2(3) . . . . ? N1 W1 C28 C32 95.7(3) . . . . ? C1 W1 C28 C32 -55.6(4) . . . . ? C2 W1 C28 C32 108.9(3) . . . . ? C31 W1 C28 C32 -37.7(3) . . . . ? C30 W1 C28 C32 -79.8(3) . . . . ? C29 W1 C28 C32 -117.0(4) . . . . ? Si2 W1 C28 C32 -157.2(2) . . . . ? N1 W1 C28 C33 -26.2(5) . . . . ? C1 W1 C28 C33 -177.6(4) . . . . ? C2 W1 C28 C33 -13.0(4) . . . . ? C31 W1 C28 C33 -159.7(5) . . . . ? C32 W1 C28 C33 -122.0(6) . . . . ? C30 W1 C28 C33 158.2(5) . . . . ? C29 W1 C28 C33 121.0(6) . . . . ? Si2 W1 C28 C33 80.8(4) . . . . ? C32 C28 C29 C30 0.0(5) . . . . ? C33 C28 C29 C30 174.2(5) . . . . ? W1 C28 C29 C30 -62.3(3) . . . . ? C32 C28 C29 C34 -165.6(4) . . . . ? C33 C28 C29 C34 8.7(7) . . . . ? W1 C28 C29 C34 132.2(4) . . . . ? C32 C28 C29 W1 62.2(3) . . . . ? C33 C28 C29 W1 -123.5(5) . . . . ? N1 W1 C29 C28 67.0(5) . . . . ? C1 W1 C29 C28 -138.7(3) . . . . ? C2 W1 C29 C28 51.9(3) . . . . ? C31 W1 C29 C28 -79.0(3) . . . . ? C32 W1 C29 C28 -37.1(3) . . . . ? C30 W1 C29 C28 -116.9(4) . . . . ? Si2 W1 C29 C28 142.7(3) . . . . ? N1 W1 C29 C30 -176.1(3) . . . . ? C1 W1 C29 C30 -21.9(3) . . . . ? C2 W1 C29 C30 168.8(3) . . . . ? C31 W1 C29 C30 37.8(3) . . . . ? C32 W1 C29 C30 79.8(3) . . . . ? C28 W1 C29 C30 116.9(4) . . . . ? Si2 W1 C29 C30 -100.4(3) . . . . ? N1 W1 C29 C34 -51.8(7) . . . . ? C1 W1 C29 C34 102.4(5) . . . . ? C2 W1 C29 C34 -66.9(5) . . . . ? C31 W1 C29 C34 162.1(6) . . . . ? C32 W1 C29 C34 -155.9(6) . . . . ? C30 W1 C29 C34 124.3(6) . . . . ? C28 W1 C29 C34 -118.9(6) . . . . ? Si2 W1 C29 C34 23.9(5) . . . . ? C28 C29 C30 C31 -0.1(5) . . . . ? C34 C29 C30 C31 164.5(5) . . . . ? W1 C29 C30 C31 -63.5(3) . . . . ? C28 C29 C30 C35 -165.9(5) . . . . ? C34 C29 C30 C35 -1.3(8) . . . . ? W1 C29 C30 C35 130.7(5) . . . . ? C28 C29 C30 W1 63.4(3) . . . . ? C34 C29 C30 W1 -132.0(5) . . . . ? C1 W1 C30 C31 -84.2(3) . . . . ? C2 W1 C30 C31 96.2(4) . . . . ? C32 W1 C30 C31 37.9(3) . . . . ? C28 W1 C30 C31 79.4(3) . . . . ? C29 W1 C30 C31 115.9(4) . . . . ? Si2 W1 C30 C31 -166.1(3) . . . . ? C1 W1 C30 C29 160.0(3) . . . . ? C2 W1 C30 C29 -19.7(5) . . . . ? C31 W1 C30 C29 -115.9(4) . . . . ? C32 W1 C30 C29 -77.9(3) . . . . ? C28 W1 C30 C29 -36.5(3) . . . . ? Si2 W1 C30 C29 78.0(3) . . . . ? C1 W1 C30 C35 34.5(5) . . . . ? C2 W1 C30 C35 -145.1(5) . . . . ? C31 W1 C30 C35 118.7(7) . . . . ? C32 W1 C30 C35 156.6(6) . . . . ? C28 W1 C30 C35 -161.9(6) . . . . ? C29 W1 C30 C35 -125.4(7) . . . . ? Si2 W1 C30 C35 -47.5(5) . . . . ? C29 C30 C31 C32 0.2(5) . . . . ? C35 C30 C31 C32 166.6(5) . . . . ? W1 C30 C31 C32 -65.2(3) . . . . ? C29 C30 C31 C36 -170.5(5) . . . . ? C35 C30 C31 C36 -4.1(8) . . . . ? W1 C30 C31 C36 124.2(5) . . . . ? C29 C30 C31 W1 65.3(3) . . . . ? C35 C30 C31 W1 -128.3(5) . . . . ? N1 W1 C31 C32 -78.0(4) . . . . ? C1 W1 C31 C32 -155.1(3) . . . . ? C2 W1 C31 C32 -15.6(4) . . . . ? C30 W1 C31 C32 115.2(4) . . . . ? C28 W1 C31 C32 37.2(3) . . . . ? C29 W1 C31 C32 77.9(3) . . . . ? Si2 W1 C31 C32 132.3(3) . . . . ? N1 W1 C31 C30 166.8(3) . . . . ? C1 W1 C31 C30 89.7(3) . . . . ? C2 W1 C31 C30 -130.8(3) . . . . ? C32 W1 C31 C30 -115.2(4) . . . . ? C28 W1 C31 C30 -78.0(3) . . . . ? C29 W1 C31 C30 -37.3(3) . . . . ? Si2 W1 C31 C30 17.1(3) . . . . ? N1 W1 C31 C36 43.2(6) . . . . ? C1 W1 C31 C36 -33.9(5) . . . . ? C2 W1 C31 C36 105.6(5) . . . . ? C32 W1 C31 C36 121.2(6) . . . . ? C30 W1 C31 C36 -123.6(6) . . . . ? C28 W1 C31 C36 158.4(6) . . . . ? C29 W1 C31 C36 -160.9(6) . . . . ? Si2 W1 C31 C36 -106.5(5) . . . . ? C30 C31 C32 C28 -0.2(5) . . . . ? C36 C31 C32 C28 170.7(5) . . . . ? W1 C31 C32 C28 -65.5(3) . . . . ? C30 C31 C32 C37 -173.0(4) . . . . ? C36 C31 C32 C37 -2.2(8) . . . . ? W1 C31 C32 C37 121.7(5) . . . . ? C30 C31 C32 W1 65.3(3) . . . . ? C36 C31 C32 W1 -123.8(5) . . . . ? C29 C28 C32 C31 0.1(5) . . . . ? C33 C28 C32 C31 -174.0(5) . . . . ? W1 C28 C32 C31 63.8(3) . . . . ? C29 C28 C32 C37 173.0(4) . . . . ? C33 C28 C32 C37 -1.1(7) . . . . ? W1 C28 C32 C37 -123.3(4) . . . . ? C29 C28 C32 W1 -63.7(3) . . . . ? C33 C28 C32 W1 122.2(5) . . . . ? N1 W1 C32 C31 132.6(3) . . . . ? C1 W1 C32 C31 26.6(3) . . . . ? C2 W1 C32 C31 169.1(3) . . . . ? C30 W1 C32 C31 -38.1(3) . . . . ? C28 W1 C32 C31 -116.0(4) . . . . ? C29 W1 C32 C31 -79.6(3) . . . . ? Si2 W1 C32 C31 -79.9(3) . . . . ? N1 W1 C32 C28 -111.3(3) . . . . ? C1 W1 C32 C28 142.6(3) . . . . ? C2 W1 C32 C28 -74.9(3) . . . . ? C31 W1 C32 C28 116.0(4) . . . . ? C30 W1 C32 C28 78.0(3) . . . . ? C29 W1 C32 C28 36.4(3) . . . . ? Si2 W1 C32 C28 36.2(4) . . . . ? N1 W1 C32 C37 11.1(5) . . . . ? C1 W1 C32 C37 -94.9(4) . . . . ? C2 W1 C32 C37 47.6(4) . . . . ? C31 W1 C32 C37 -121.5(6) . . . . ? C30 W1 C32 C37 -159.6(5) . . . . ? C28 W1 C32 C37 122.4(5) . . . . ? C29 W1 C32 C37 158.9(5) . . . . ? Si2 W1 C32 C37 158.6(3) . . . . ? #===END