# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2013 #============================================================================ # 1. TITLE AND AUTHOR LIST data_first_block _publ_section_title ; Synthesis and Structural Characterization of New Organo-Diimido and Organo-Imido Niobium and Titanium Complexes. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Dorado, I' ; Departamento de Quimica Inorganica Campus Universitario Universidad de Alcala 28871 Alcala de Henares Madrid Spain ; 'Garces, A' ; Departamento de Quimica Inorganica Campus Universitario Universidad de Alcala 28871 Alcala de Henares Madrid Spain ; 'Lopez-Mardomingo, C' ; Departamento de Quimica Organica Campus Universitario Universidad de Alcala 28871 Alcala de Henares Madrid Spain ; 'Fajardo, M' ; Departamento de Ciencias Experimentales e Ingenieria E.S.C.E.T. Universidad Rey Juan Carlos 28993 Mostoles Madrid Spain ; 'Rodriguez, A' ; Departamento de Quimica Inorganica, Organica y Bioquimica Facultad de Quimica Universidad Castilla-La Mancha 13071 Ciudad Real Spain ; 'Antinolo, A' ; Departamento de Quimica Inorganica, Organica y Bioquimica Facultad de Quimica Universidad Castilla-La Mancha 13071 Ciudad Real Spain ; 'Otero, A' ; Departamento de Quimica Inorganica, Organica y Bioquimica Facultad de Quimica Universidad Castilla-La Mancha 13071 Ciudad Real Spain ; #============================================================================ # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================ data_3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H38 N2 Nb Si3' _chemical_formula_weight 447.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.306(8) _cell_length_b 16.0717(7) _cell_length_c 19.428(4) _cell_angle_alpha 90.00 _cell_angle_beta 117.19(2) _cell_angle_gamma 90.00 _cell_volume 5362(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour maroon _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'four circle diffractometer Nonius-Mach3' _diffrn_measurement_method '\w/2\2q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 6471 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1365 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.99 _reflns_number_total 6471 _reflns_number_gt 2039 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (control program)' _computing_cell_refinement 'Nonius (control program)' _computing_data_reduction 'XRAY80 (Stewart, 1976)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6471 _refine_ls_number_parameters 196 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.2174 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2417 _refine_ls_wR_factor_gt 0.1545 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.77927(5) 0.07075(5) 0.19330(4) 0.0694(3) Uani 1 1 d . . . Si1 Si 0.89960(19) 0.1968(2) 0.35144(17) 0.1143(12) Uani 1 1 d D . . Si2 Si 0.58747(18) 0.0510(3) 0.16323(18) 0.1218(14) Uani 1 1 d D . . Si3 Si 0.85777(18) -0.08142(19) 0.11963(18) 0.0944(9) Uani 1 1 d D . . N1 N 0.7651(4) 0.1439(4) 0.1205(4) 0.078(2) Uani 1 1 d . . . N2 N 0.8037(5) -0.0317(6) 0.2917(5) 0.099(3) Uani 1 1 d . . . C20 C 0.8039(5) 0.1552(6) 0.2889(5) 0.080(3) Uani 1 1 d . A . H20A H 0.7699 0.2027 0.2672 0.096 Uiso 1 1 calc . . . H20B H 0.7864 0.1273 0.3225 0.096 Uiso 1 1 calc . . . C30 C 0.6658(5) 0.0143(6) 0.1409(5) 0.085(3) Uani 1 1 d . T . H30A H 0.6462 0.0187 0.0853 0.102 Uiso 1 1 calc . . . H30B H 0.6732 -0.0445 0.1534 0.102 Uiso 1 1 calc . . . C40 C 0.8755(5) 0.0039(6) 0.1869(5) 0.082(3) Uani 1 1 d . M . H40A H 0.9060 0.0450 0.1760 0.099 Uiso 1 1 calc . . . H40B H 0.9085 -0.0176 0.2383 0.099 Uiso 1 1 calc . . . C12 C 0.7568(5) 0.1963(5) 0.0595(4) 0.065(2) Uani 1 1 d . . . C13 C 0.6907(5) 0.1983(6) -0.0094(5) 0.075(3) Uani 1 1 d . . . H13 H 0.6496 0.1632 -0.0168 0.090 Uiso 1 1 calc . . . C14 C 0.8165(5) 0.2488(6) 0.0683(5) 0.080(3) Uani 1 1 d . . . H14 H 0.8624 0.2487 0.1145 0.096 Uiso 1 1 calc . . . C15 C 0.8167(6) -0.0786(8) 0.3387(6) 0.112(4) Uani 1 1 d . . . C16 C 0.8334(9) -0.1405(9) 0.3989(7) 0.173(6) Uani 1 1 d . . . H16A H 0.8845 -0.1629 0.4149 0.260 Uiso 1 1 calc . . . H16B H 0.7956 -0.1844 0.3792 0.260 Uiso 1 1 calc . . . H16C H 0.8309 -0.1149 0.4424 0.260 Uiso 1 1 calc . . . C1 C 0.9160(13) 0.2710(12) 0.4301(11) 0.093(7) Uiso 0.50 1 d PDU A 1 H1A H 0.9702 0.2853 0.4569 0.140 Uiso 0.50 1 calc P B 1 H1B H 0.9004 0.2460 0.4658 0.140 Uiso 0.50 1 calc P C 1 H1C H 0.8858 0.3204 0.4086 0.140 Uiso 0.50 1 calc P D 1 C2 C 0.9833(13) 0.1269(15) 0.3830(15) 0.141(10) Uiso 0.50 1 d PD A 1 H2A H 1.0302 0.1575 0.4132 0.212 Uiso 0.50 1 calc P E 1 H2B H 0.9854 0.1036 0.3385 0.212 Uiso 0.50 1 calc P F 1 H2C H 0.9781 0.0829 0.4137 0.212 Uiso 0.50 1 calc P G 1 C3 C 0.9146(15) 0.2850(14) 0.2929(12) 0.131(9) Uiso 0.50 1 d PD A 1 H3A H 0.9667 0.3063 0.3206 0.197 Uiso 0.50 1 calc P H 1 H3B H 0.8780 0.3289 0.2853 0.197 Uiso 0.50 1 calc P I 1 H3C H 0.9067 0.2641 0.2435 0.197 Uiso 0.50 1 calc P J 1 C11 C 0.8878(15) 0.2505(13) 0.4310(11) 0.105(9) Uiso 0.50 1 d PDU A 2 H11A H 0.9364 0.2751 0.4665 0.157 Uiso 0.50 1 calc P K 2 H11B H 0.8719 0.2108 0.4580 0.157 Uiso 0.50 1 calc P L 2 H11C H 0.8489 0.2931 0.4094 0.157 Uiso 0.50 1 calc P M 2 C21 C 0.9584(15) 0.1015(13) 0.4076(14) 0.138(10) Uiso 0.50 1 d PD A 2 H21A H 1.0114 0.1176 0.4400 0.207 Uiso 0.50 1 calc P N 2 H21B H 0.9570 0.0596 0.3717 0.207 Uiso 0.50 1 calc P O 2 H21C H 0.9362 0.0797 0.4391 0.207 Uiso 0.50 1 calc P P 2 C31 C 0.9509(14) 0.2346(16) 0.2982(14) 0.139(10) Uiso 0.50 1 d PD A 2 H31A H 0.9984 0.2615 0.3335 0.208 Uiso 0.50 1 calc P Q 2 H31B H 0.9185 0.2736 0.2594 0.208 Uiso 0.50 1 calc P R 2 H31C H 0.9628 0.1886 0.2740 0.208 Uiso 0.50 1 calc P S 2 C4 C 0.5021(11) -0.0252(14) 0.1035(10) 0.096(7) Uiso 0.50 1 d PDU T 1 H4A H 0.4574 -0.0107 0.1104 0.145 Uiso 0.50 1 calc P U 1 H4B H 0.5177 -0.0811 0.1212 0.145 Uiso 0.50 1 calc P V 1 H4C H 0.4892 -0.0213 0.0497 0.145 Uiso 0.50 1 calc P W 1 C5 C 0.6146(14) 0.0111(16) 0.2652(9) 0.113(9) Uiso 0.50 1 d PDU T 1 H5A H 0.5764 0.0293 0.2806 0.169 Uiso 0.50 1 calc P X 1 H5B H 0.6648 0.0326 0.3008 0.169 Uiso 0.50 1 calc P Y 1 H5C H 0.6164 -0.0486 0.2655 0.169 Uiso 0.50 1 calc P Z 1 C6 C 0.5826(19) 0.1676(10) 0.157(2) 0.140(12) Uiso 0.50 1 d PDU T 1 H6A H 0.5425 0.1872 0.1692 0.211 Uiso 0.50 1 calc P A 1 H6B H 0.5710 0.1847 0.1056 0.211 Uiso 0.50 1 calc P B 1 H6C H 0.6318 0.1906 0.1932 0.211 Uiso 0.50 1 calc P C 1 C41 C 0.4852(10) 0.0190(15) 0.0987(12) 0.110(8) Uiso 0.50 1 d PDU T 2 H41A H 0.4510 0.0444 0.1161 0.165 Uiso 0.50 1 calc P D 2 H41B H 0.4810 -0.0405 0.1001 0.165 Uiso 0.50 1 calc P E 2 H41C H 0.4709 0.0364 0.0467 0.165 Uiso 0.50 1 calc P F 2 C51 C 0.6130(16) 0.0541(16) 0.2669(9) 0.120(9) Uiso 0.50 1 d PDU T 2 H51A H 0.5705 0.0773 0.2733 0.180 Uiso 0.50 1 calc P G 2 H51B H 0.6585 0.0879 0.2939 0.180 Uiso 0.50 1 calc P H 2 H51C H 0.6234 -0.0014 0.2876 0.180 Uiso 0.50 1 calc P I 2 C61 C 0.568(2) 0.1612(13) 0.1295(18) 0.168(16) Uiso 0.50 1 d PDU T 2 H61A H 0.5293 0.1843 0.1425 0.253 Uiso 0.50 1 calc P J 2 H61B H 0.5487 0.1630 0.0744 0.253 Uiso 0.50 1 calc P K 2 H61C H 0.6149 0.1929 0.1542 0.253 Uiso 0.50 1 calc P L 2 C7 C 0.7987(13) -0.1663(14) 0.1262(16) 0.167(11) Uiso 0.50 1 d PDU M 1 H7A H 0.7996 -0.2119 0.0947 0.250 Uiso 0.50 1 calc P N 1 H7B H 0.7461 -0.1476 0.1083 0.250 Uiso 0.50 1 calc P O 1 H7C H 0.8193 -0.1842 0.1790 0.250 Uiso 0.50 1 calc P P 1 C8 C 0.9521(10) -0.1261(16) 0.1350(16) 0.113(10) Uiso 0.50 1 d PDU M 1 H8A H 0.9432 -0.1685 0.0970 0.169 Uiso 0.50 1 calc P Q 1 H8B H 0.9781 -0.1499 0.1858 0.169 Uiso 0.50 1 calc P R 1 H8C H 0.9840 -0.0830 0.1300 0.169 Uiso 0.50 1 calc P S 1 C9 C 0.7759(13) -0.0693(16) 0.0239(10) 0.119(9) Uiso 0.50 1 d PDU M 1 H9A H 0.7710 -0.1183 -0.0062 0.178 Uiso 0.50 1 calc P T 1 H9B H 0.7846 -0.0219 -0.0013 0.178 Uiso 0.50 1 calc P U 1 H9C H 0.7290 -0.0612 0.0286 0.178 Uiso 0.50 1 calc P V 1 C71 C 0.8347 -0.1752 0.1654 0.107 Uiso 0.50 1 d PDU M 2 H71A H 0.8239 -0.2225 0.1319 0.161 Uiso 0.50 1 calc P W 2 H71B H 0.7900 -0.1633 0.1731 0.161 Uiso 0.50 1 calc P X 2 H71C H 0.8785 -0.1872 0.2144 0.161 Uiso 0.50 1 calc P Y 2 C81 C 0.9484(11) -0.1052(18) 0.1094(15) 0.113(10) Uiso 0.50 1 d PDU M 2 H81A H 0.9392 -0.1528 0.0765 0.169 Uiso 0.50 1 calc P Z 2 H81B H 0.9907 -0.1167 0.1595 0.169 Uiso 0.50 1 calc P A 2 H81C H 0.9613 -0.0581 0.0870 0.169 Uiso 0.50 1 calc P B 2 C91 C 0.7939(15) -0.033(2) 0.0216(13) 0.176(14) Uiso 0.50 1 d PDU M 2 H91A H 0.7840 -0.0732 -0.0184 0.265 Uiso 0.50 1 calc P C 2 H91B H 0.8199 0.0144 0.0140 0.265 Uiso 0.50 1 calc P D 2 H91C H 0.7454 -0.0157 0.0196 0.265 Uiso 0.50 1 calc P E 2 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 Nb1 0.0695(5) 0.0836(6) 0.0561(4) 0.0102(5) 0.0296(4) 0.0074(5) Si1 0.092(2) 0.158(3) 0.0744(19) -0.024(2) 0.0227(17) 0.010(2) Si2 0.0710(19) 0.207(4) 0.086(2) -0.006(2) 0.0342(16) 0.009(2) Si3 0.097(2) 0.085(2) 0.102(2) -0.0104(18) 0.0457(18) -0.0025(18) N1 0.076(5) 0.087(5) 0.059(4) 0.018(4) 0.022(4) 0.010(4) N2 0.097(6) 0.117(7) 0.082(6) 0.032(5) 0.040(5) 0.006(5) C20 0.069(6) 0.105(7) 0.066(5) 0.013(5) 0.030(5) 0.013(5) C30 0.064(6) 0.109(8) 0.078(6) 0.001(6) 0.028(5) 0.006(5) C40 0.081(6) 0.081(6) 0.081(6) 0.002(5) 0.033(5) 0.005(5) C12 0.083(6) 0.067(6) 0.046(4) -0.005(4) 0.031(4) 0.014(5) C13 0.063(5) 0.101(7) 0.047(5) 0.000(5) 0.014(4) -0.007(5) C14 0.075(6) 0.095(7) 0.048(5) 0.017(5) 0.010(4) -0.002(5) C15 0.103(9) 0.135(10) 0.081(7) 0.030(7) 0.029(6) -0.024(8) C16 0.248(18) 0.152(12) 0.131(11) 0.072(10) 0.096(12) -0.017(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N1 1.762(7) . ? Nb1 C30 2.149(9) . ? Nb1 C20 2.170(9) . ? Nb1 C40 2.198(9) . ? Nb1 N2 2.402(8) . ? Si1 C20 1.813(9) . ? Si1 C2 1.828(16) . ? Si1 C31 1.832(16) . ? Si1 C1 1.849(14) . ? Si1 C11 1.874(15) . ? Si1 C3 1.921(16) . ? Si1 C21 1.922(16) . ? Si2 C51 1.843(16) . ? Si2 C30 1.851(9) . ? Si2 C41 1.864(15) . ? Si2 C61 1.867(17) . ? Si2 C6 1.878(16) . ? Si2 C5 1.914(15) . ? Si2 C4 1.953(15) . ? Si3 C40 1.815(10) . ? Si3 C9 1.819(15) . ? Si3 C7 1.819(16) . ? Si3 C8 1.851(15) . ? Si3 C81 1.887(16) . ? Si3 C91 1.900(17) . ? Si3 C71 1.905(3) . ? N1 C12 1.402(10) . ? N2 C15 1.120(11) . ? C12 C13 1.363(10) . ? C12 C14 1.375(11) . ? C13 C14 1.380(11) 7_655 ? C14 C13 1.380(11) 7_655 ? C15 C16 1.454(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Nb1 C30 98.7(3) . . ? N1 Nb1 C20 99.3(3) . . ? C30 Nb1 C20 116.5(3) . . ? N1 Nb1 C40 96.1(3) . . ? C30 Nb1 C40 118.1(4) . . ? C20 Nb1 C40 119.6(3) . . ? N1 Nb1 N2 177.2(3) . . ? C30 Nb1 N2 82.8(3) . . ? C20 Nb1 N2 82.0(3) . . ? C40 Nb1 N2 81.1(3) . . ? C20 Si1 C2 118.1(9) . . ? C20 Si1 C31 113.1(9) . . ? C2 Si1 C31 76.7(12) . . ? C20 Si1 C1 122.0(8) . . ? C2 Si1 C1 109.2(9) . . ? C31 Si1 C1 108.7(12) . . ? C20 Si1 C11 104.6(8) . . ? C2 Si1 C11 115.4(11) . . ? C31 Si1 C11 127.9(12) . . ? C1 Si1 C11 19.9(10) . . ? C20 Si1 C3 105.0(8) . . ? C2 Si1 C3 107.6(12) . . ? C31 Si1 C3 32.2(9) . . ? C1 Si1 C3 89.9(10) . . ? C11 Si1 C3 104.9(9) . . ? C20 Si1 C21 104.1(9) . . ? C2 Si1 C21 28.1(10) . . ? C31 Si1 C21 104.7(9) . . ? C1 Si1 C21 102.2(11) . . ? C11 Si1 C21 99.3(11) . . ? C3 Si1 C21 135.6(11) . . ? C51 Si2 C30 115.2(9) . . ? C51 Si2 C41 114.5(11) . . ? C30 Si2 C41 118.9(8) . . ? C51 Si2 C61 105.6(11) . . ? C30 Si2 C61 106.1(13) . . ? C41 Si2 C61 92.4(15) . . ? C51 Si2 C6 91.4(14) . . ? C30 Si2 C6 109.0(12) . . ? C41 Si2 C6 103.1(10) . . ? C61 Si2 C6 15.0(16) . . ? C51 Si2 C5 21.1(10) . . ? C30 Si2 C5 105.6(9) . . ? C41 Si2 C5 108.0(11) . . ? C61 Si2 C5 126.6(13) . . ? C6 Si2 C5 112.5(14) . . ? C51 Si2 C4 113.4(11) . . ? C30 Si2 C4 102.7(8) . . ? C41 Si2 C4 23.1(9) . . ? C61 Si2 C4 113.9(14) . . ? C6 Si2 C4 125.7(11) . . ? C5 Si2 C4 99.4(8) . . ? C40 Si3 C9 116.4(9) . . ? C40 Si3 C7 115.7(9) . . ? C9 Si3 C7 82.7(11) . . ? C40 Si3 C8 109.2(9) . . ? C9 Si3 C8 122.5(12) . . ? C7 Si3 C8 107.5(10) . . ? C40 Si3 C81 110.5(9) . . ? C9 Si3 C81 109.1(12) . . ? C7 Si3 C81 119.8(13) . . ? C8 Si3 C81 17.7(12) . . ? C40 Si3 C91 103.6(11) . . ? C9 Si3 C91 21.2(13) . . ? C7 Si3 C91 103.7(13) . . ? C8 Si3 C91 117.5(13) . . ? C81 Si3 C91 100.7(10) . . ? C40 Si3 C71 105.6(3) . . ? C9 Si3 C71 106.5(8) . . ? C7 Si3 C71 23.9(9) . . ? C8 Si3 C71 92.4(8) . . ? C81 Si3 C71 108.4(9) . . ? C91 Si3 C71 127.6(11) . . ? C12 N1 Nb1 174.4(6) . . ? C15 N2 Nb1 178.3(10) . . ? Si1 C20 Nb1 124.2(4) . . ? Si2 C30 Nb1 121.3(5) . . ? Si3 C40 Nb1 121.6(5) . . ? C13 C12 C14 117.5(8) . . ? C13 C12 N1 122.6(9) . . ? C14 C12 N1 119.9(8) . . ? C12 C13 C14 121.5(8) . 7_655 ? C12 C14 C13 120.9(8) . 7_655 ? N2 C15 C16 179.2(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.666 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.095