Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global # *** Added by check_cif _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Nikonov, Georgii I.' 'Howard, Judith A. K.' 'Kuzmina, Lyudmila G.' _publ_contact_author_name 'Dr Georgii I. Nikonov' _publ_contact_author_address ; Chemistry Moscow State University Vorob'evy Gory Moscow 119899 RUSSIAN FEDERATION ; _publ_contact_author_phone '+7 095 9391976' _publ_contact_author_fax '+7 095 9328846' _publ_contact_author_email nikonov@org.chem.msu.su _publ_section_title ; Niobocene hydrides with functionalized silyl ligands. Tuning of interligand hypervalent interactions (IHI) M...Si...X. ; data_compound16 _database_code_CSD 175461 # Cp2Nb(SiMe2I)2H (Compound 16) _audit_creation_method SHELXL _chemical_name_systematic ; bis(cyclopentadienyl)bis(iododimethylsilyl)hydrido niobium(V) ; _chemical_name_common ? _chemical_formula_moiety 'Cp2Nb(SiMe2I)2H' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H23 I2 Nb Si2' _chemical_formula_weight 594.21 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 18.996(3) _cell_length_b 18.996(3) _cell_length_c 13.031(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4702.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour dark-violet _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method ? _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 3.230 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.708 _exptl_absorpt_correction_T_max 0.977 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1417 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max -6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 6.44 _diffrn_reflns_theta_max 25.97 _reflns_number_total 1417 _reflns_number_observed 1122 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+52.3760P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1417 _refine_ls_number_parameters 99 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_obs 0.0560 _refine_ls_wR_factor_all 0.1758 _refine_ls_wR_factor_obs 0.1658 _refine_ls_goodness_of_fit_all 1.115 _refine_ls_goodness_of_fit_obs 1.190 _refine_ls_restrained_S_all 1.115 _refine_ls_restrained_S_obs 1.190 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nb1 Nb 0.15879(6) 0.37960(6) 0.0000 0.0249(4) Uani 1 d S . I1 I 0.17663(4) 0.38358(4) 0.33153(6) 0.0407(4) Uani 1 d . . Si1 Si 0.23861(14) 0.40498(14) 0.1575(3) 0.0307(7) Uani 1 d . . C1 C 0.0517(5) 0.4324(6) -0.0533(12) 0.043(3) Uani 1 d . . C2 C 0.1390(7) 0.5031(7) 0.0000 0.034(3) Uani 1 d S . C3 C 0.1049(5) 0.4769(5) -0.0869(11) 0.035(2) Uani 1 d . . C4 C 0.2154(8) 0.2669(7) 0.0000 0.036(4) Uani 1 d S . C5 C 0.1713(6) 0.2693(5) 0.0900(11) 0.040(3) Uani 1 d . . C6 C 0.1005(6) 0.2750(5) 0.0546(11) 0.039(3) Uani 1 d . . C7 C 0.2786(5) 0.5058(4) 0.1764(8) 0.026(2) Uani 1 d . . C8 C 0.3278(7) 0.3497(6) 0.1722(9) 0.041(3) Uani 1 d . . C1' C 0.5000 0.5000 0.5000 0.077(14) Uiso 1 d S . C2' C 0.4039(23) 0.5335(21) 0.5000 0.110(11) Uiso 1 d S . C3' C 0.4251(35) 0.6286(33) 0.5000 0.158(21) Uiso 1 d S . H1A H 0.0166 0.4106 -0.0948 0.050 Uiso 1 d . . H2A H 0.1754 0.5388 0.0000 0.050 Uiso 1 d S . H3A H 0.1131 0.4905 -0.1569 0.050 Uiso 1 d . . H4A H 0.2665 0.2604 0.0000 0.050 Uiso 1 d S . H5A H 0.1868 0.2627 0.1607 0.050 Uiso 1 d . . H6A H 0.0584 0.2734 0.0955 0.050 Uiso 1 d . . H7A H 0.3075 0.5074 0.2374 0.050 Uiso 1 d . . H7B H 0.3077 0.5178 0.1181 0.050 Uiso 1 d . . H7C H 0.2412 0.5389 0.1824 0.050 Uiso 1 d . . H8A H 0.3535 0.3651 0.2332 0.050 Uiso 1 d . . H8B H 0.3193 0.3010 0.1760 0.050 Uiso 1 d . . H8C H 0.3590 0.3593 0.1134 0.050 Uiso 1 d . . H1 H 0.2511 0.4155 0.0000 0.035 Uiso 1 d S . 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 0.0265(7) 0.0221(6) 0.0261(8) 0.000 0.000 0.0033(4) I1 0.0492(6) 0.0428(5) 0.0300(6) -0.0001(3) 0.0076(3) 0.0051(3) Si1 0.0306(14) 0.0306(14) 0.031(2) -0.0024(10) 0.0008(10) 0.0038(9) C1 0.024(5) 0.044(6) 0.060(8) -0.009(5) -0.007(5) 0.003(4) C2 0.034(7) 0.023(6) 0.046(10) 0.000 0.000 0.010(5) C3 0.034(5) 0.029(5) 0.041(8) 0.004(4) -0.003(4) 0.009(3) C4 0.054(9) 0.023(7) 0.031(10) 0.000 0.000 0.017(6) C5 0.059(7) 0.026(5) 0.035(8) 0.002(4) 0.002(5) 0.003(4) C6 0.049(6) 0.026(5) 0.044(8) 0.009(5) 0.011(5) -0.002(4) C7 0.044(5) 0.015(4) 0.018(5) -0.007(3) -0.003(4) 0.015(3) C8 0.067(8) 0.032(5) 0.025(7) 0.005(4) -0.013(5) 0.022(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 C1 2.371(10) 10 ? Nb1 C1 2.371(10) . ? Nb1 C2 2.376(13) . ? Nb1 C6 2.383(9) 10 ? Nb1 C6 2.383(9) . ? Nb1 C3 2.397(10) 10 ? Nb1 C3 2.397(10) . ? Nb1 C4 2.396(13) . ? Nb1 C5 2.414(11) . ? Nb1 C5 2.414(11) 10 ? Nb1 Si1 2.597(3) . ? Nb1 Si1 2.597(3) 10 ? I1 Si1 2.587(3) . ? Si1 C8 2.002(11) . ? Si1 C7 2.075(10) . ? C1 C1 1.39(3) 10 ? C1 C3 1.39(2) . ? C2 C3 1.40(2) . ? C2 C3 1.40(2) 10 ? C4 C5 1.44(2) 10 ? C4 C5 1.44(2) . ? C5 C6 1.43(2) . ? C6 C6 1.42(3) 10 ? C1' C2' 1.93(4) 11_566 ? C1' C2' 1.93(4) . ? C1' C2' 1.93(4) 9_666 ? C1' C2' 1.93(4) 3_655 ? C2' C3' 1.85(8) . ? 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 Nb1 C1 34.1(7) 10 . ? C1 Nb1 C2 56.4(4) 10 . ? C1 Nb1 C2 56.4(4) . . ? C1 Nb1 C6 92.4(4) 10 10 ? C1 Nb1 C6 82.3(4) . 10 ? C2 Nb1 C6 138.6(4) . 10 ? C1 Nb1 C6 82.3(4) 10 . ? C1 Nb1 C6 92.4(4) . . ? C2 Nb1 C6 138.6(4) . . ? C6 Nb1 C6 34.7(7) 10 . ? C1 Nb1 C3 33.8(4) 10 10 ? C1 Nb1 C3 56.4(4) . 10 ? C2 Nb1 C3 34.0(3) . 10 ? C6 Nb1 C3 125.8(4) 10 10 ? C6 Nb1 C3 107.7(4) . 10 ? C1 Nb1 C3 56.4(4) 10 . ? C1 Nb1 C3 33.8(4) . . ? C2 Nb1 C3 34.0(3) . . ? C6 Nb1 C3 107.7(4) 10 . ? C6 Nb1 C3 125.8(4) . . ? C3 Nb1 C3 56.4(6) 10 . ? C1 Nb1 C4 139.7(5) 10 . ? C1 Nb1 C4 139.7(5) . . ? C2 Nb1 C4 162.4(5) . . ? C6 Nb1 C4 57.6(5) 10 . ? C6 Nb1 C4 57.6(5) . . ? C3 Nb1 C4 151.7(3) 10 . ? C3 Nb1 C4 151.7(3) . . ? C1 Nb1 C5 108.0(4) 10 . ? C1 Nb1 C5 126.4(4) . . ? C2 Nb1 C5 150.8(3) . . ? C6 Nb1 C5 57.8(5) 10 . ? C6 Nb1 C5 34.6(4) . . ? C3 Nb1 C5 118.8(4) 10 . ? C3 Nb1 C5 160.3(4) . . ? C4 Nb1 C5 34.9(4) . . ? C1 Nb1 C5 126.4(4) 10 10 ? C1 Nb1 C5 108.0(4) . 10 ? C2 Nb1 C5 150.8(3) . 10 ? C6 Nb1 C5 34.6(4) 10 10 ? C6 Nb1 C5 57.8(5) . 10 ? C3 Nb1 C5 160.3(4) 10 10 ? C3 Nb1 C5 118.8(5) . 10 ? C4 Nb1 C5 34.9(4) . 10 ? C5 Nb1 C5 58.2(7) . 10 ? C1 Nb1 Si1 101.0(4) 10 . ? C1 Nb1 Si1 130.8(3) . . ? C2 Nb1 Si1 84.8(2) . . ? C6 Nb1 Si1 131.4(3) 10 . ? C6 Nb1 Si1 101.0(3) . . ? C3 Nb1 Si1 74.5(3) 10 . ? C3 Nb1 Si1 118.7(3) . . ? C4 Nb1 Si1 84.5(3) . . ? C5 Nb1 Si1 73.7(3) . . ? C5 Nb1 Si1 119.2(3) 10 . ? C1 Nb1 Si1 130.8(3) 10 10 ? C1 Nb1 Si1 101.0(4) . 10 ? C2 Nb1 Si1 84.8(2) . 10 ? C6 Nb1 Si1 101.0(3) 10 10 ? C6 Nb1 Si1 131.4(3) . 10 ? C3 Nb1 Si1 118.7(3) 10 10 ? C3 Nb1 Si1 74.5(3) . 10 ? C4 Nb1 Si1 84.5(3) . 10 ? C5 Nb1 Si1 119.2(3) . 10 ? C5 Nb1 Si1 73.7(3) 10 10 ? Si1 Nb1 Si1 104.43(14) . 10 ? C8 Si1 C7 99.4(5) . . ? C8 Si1 I1 102.6(4) . . ? C7 Si1 I1 102.0(3) . . ? C8 Si1 Nb1 118.2(4) . . ? C7 Si1 Nb1 118.6(3) . . ? I1 Si1 Nb1 113.45(11) . . ? C1 C1 C3 108.4(8) 10 . ? C1 C1 Nb1 73.0(4) 10 . ? C3 C1 Nb1 74.1(6) . . ? C3 C2 C3 108.4(14) . 10 ? C3 C2 Nb1 73.8(7) . . ? C3 C2 Nb1 73.8(7) 10 . ? C1 C3 C2 107.4(12) . . ? C1 C3 Nb1 72.1(6) . . ? C2 C3 Nb1 72.2(7) . . ? C5 C4 C5 108.8(14) 10 . ? C5 C4 Nb1 73.2(6) 10 . ? C5 C4 Nb1 73.2(6) . . ? C4 C5 C6 106.6(12) . . ? C4 C5 Nb1 71.9(7) . . ? C6 C5 Nb1 71.5(7) . . ? C6 C6 C5 108.9(8) 10 . ? C6 C6 Nb1 72.6(3) 10 . ? C5 C6 Nb1 73.9(6) . . ? C2' C1' C2' 90.000(6) 11_566 . ? C2' C1' C2' 90.000(9) 11_566 9_666 ? C2' C1' C2' 180.000(4) . 9_666 ? C2' C1' C2' 180.000(4) 11_566 3_655 ? C2' C1' C2' 90.000(10) . 3_655 ? C2' C1' C2' 90.000(1) 9_666 3_655 ? C3' C2' C1' 96.7(34) . . ? _refine_diff_density_max 1.086 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.148 #==end data_compound19 _database_code_CSD 175462 # [Cp2Nb(mu-H2)AlH(mu-H))]2 (Compound 19) _audit_creation_method SHELXL _chemical_name_systematic ; bis[bis(cyclopentadienyl)tetrahydraaluminate niobium(III)] ; _chemical_name_common 'tetrahydraaluminate niobocene dimer' _chemical_formula_moiety '[Cp2Nb(AlH4)]2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H14 Al Nb' _chemical_formula_weight 254.10 _chemical_melting_point ? _chemical_comapound_source ? 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' 'Al' 'Al' 0.0645 0.0514 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.894(2) _cell_length_b 12.499(2) _cell_length_c 14.256(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.01(2) _cell_angle_gamma 90.00 _cell_volume 1031.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method ? _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.80736 _exptl_absorpt_correction_T_max 0.91377 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6705 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.50 _reflns_number_total 2138 _reflns_number_observed 1823 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 107 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+1.1138P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2031 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_obs 0.0251 _refine_ls_wR_factor_all 0.0541 _refine_ls_wR_factor_obs 0.0491 _refine_ls_goodness_of_fit_all 1.124 _refine_ls_goodness_of_fit_obs 1.152 _refine_ls_restrained_S_all 1.164 _refine_ls_restrained_S_obs 1.152 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nb1 Nb 0.23589(4) 0.74113(2) 0.12518(2) 0.01678(8) Uani 1 d . . Al1 Al 0.05264(15) 0.60381(6) -0.00667(6) 0.0249(2) Uani 1 d . . C1 C 0.3887(5) 0.7282(2) 0.2917(2) 0.0309(6) Uani 1 d . . C2 C 0.2365(5) 0.6418(2) 0.2656(2) 0.0288(6) Uani 1 d . . C3 C 0.3334(5) 0.5760(2) 0.2021(2) 0.0274(6) Uani 1 d . . C4 C 0.5464(5) 0.6218(2) 0.1918(2) 0.0287(6) Uani 1 d . . C5 C 0.5791(5) 0.7157(2) 0.2457(2) 0.0304(7) Uani 1 d . . C6 C 0.1151(6) 0.9184(2) 0.1558(2) 0.0320(7) Uani 1 d . . C7 C -0.0583(5) 0.8730(2) 0.0875(2) 0.0346(7) Uani 1 d . . C8 C 0.0346(5) 0.8528(2) 0.0045(2) 0.0294(6) Uani 1 d . . C9 C 0.2663(5) 0.8896(2) 0.0220(2) 0.0252(6) Uani 1 d . . C10 C 0.3159(5) 0.9288(2) 0.1159(2) 0.0281(6) Uani 1 d . . H1A H 0.3674(49) 0.7827(23) 0.3311(21) 0.028(8) Uiso 1 d . . H2A H 0.1070(55) 0.6324(25) 0.2859(23) 0.039(9) Uiso 1 d . . H3A H 0.2842(48) 0.5146(24) 0.1816(20) 0.026(8) Uiso 1 d . . H4A H 0.6401(59) 0.5974(27) 0.1551(24) 0.045(10) Uiso 1 d . . H5A H 0.6955(52) 0.7614(23) 0.2543(21) 0.028(8) Uiso 1 d . . H6A H 0.1059(54) 0.9333(26) 0.2143(24) 0.040(10) Uiso 1 d . . H7A H -0.2003(58) 0.8595(25) 0.0903(24) 0.039(9) Uiso 1 d . . H8A H -0.0309(52) 0.8265(24) -0.0475(22) 0.029(9) Uiso 1 d . . H9A H 0.3663(48) 0.8893(22) -0.0187(21) 0.025(8) Uiso 1 d . . H10A H 0.4473(51) 0.9544(24) 0.1457(22) 0.032(9) Uiso 1 d . . H1 H 0.1725(41) 0.4854(20) -0.0072(18) 0.016(6) Uiso 1 d . . H2 H -0.0473(50) 0.6245(23) -0.1087(21) 0.037(8) Uiso 1 d . . H3 H -0.0079(57) 0.6825(27) 0.1067(24) 0.053(10) Uiso 1 d . . H4 H 0.3447(58) 0.6851(28) 0.0357(24) 0.056(10) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.01859(12) 0.01658(12) 0.01483(12) 0.00121(9) 0.00231(8) -0.00016(9) Al1 0.0344(5) 0.0202(4) 0.0187(4) 0.0003(3) 0.0014(3) -0.0045(3) C1 0.041(2) 0.033(2) 0.0163(14) 0.0006(12) -0.0007(12) 0.0057(13) C2 0.0288(15) 0.039(2) 0.0197(15) 0.0105(12) 0.0069(12) 0.0004(13) C3 0.036(2) 0.0187(13) 0.0238(15) 0.0055(12) -0.0025(12) -0.0002(12) C4 0.0275(14) 0.034(2) 0.024(2) 0.0092(12) 0.0026(12) 0.0109(12) C5 0.0241(14) 0.035(2) 0.027(2) 0.0101(13) -0.0084(12) -0.0046(12) C6 0.047(2) 0.0211(14) 0.030(2) -0.0010(12) 0.0128(14) 0.0112(13) C7 0.0246(15) 0.0254(14) 0.054(2) 0.0111(14) 0.0088(14) 0.0086(12) C8 0.036(2) 0.0214(13) 0.026(2) 0.0038(12) -0.0064(13) 0.0010(11) C9 0.036(2) 0.0150(12) 0.026(2) 0.0032(11) 0.0089(12) -0.0007(11) C10 0.036(2) 0.0154(13) 0.031(2) -0.0015(11) 0.0019(13) -0.0037(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 C8 2.353(3) . ? Nb1 C2 2.355(3) . ? Nb1 C3 2.356(3) . ? Nb1 C1 2.378(3) . ? Nb1 C7 2.379(3) . ? Nb1 C6 2.393(3) . ? Nb1 C9 2.396(3) . ? Nb1 C10 2.402(3) . ? Nb1 C4 2.411(3) . ? Nb1 C5 2.412(3) . ? Nb1 Al1 2.6212(10) . ? Nb1 H3 1.59(3) . ? Nb1 H4 1.69(3) . ? Al1 Al1 2.683(2) 3_565 ? Al1 H1 1.64(2) . ? Al1 H2 1.48(3) . ? Al1 H3 1.98(3) . ? Al1 H4 1.99(3) . ? C1 C2 1.408(4) . ? C1 C5 1.413(4) . ? C1 H1A 0.91(3) . ? C2 C3 1.422(4) . ? C2 H2A 0.87(3) . ? C3 C4 1.412(4) . ? C3 H3A 0.85(3) . ? C4 C5 1.396(4) . ? C4 H4A 0.88(3) . ? C5 H5A 0.88(3) . ? C6 C7 1.391(5) . ? C6 C10 1.414(4) . ? C6 H6A 0.87(3) . ? C7 C8 1.418(5) . ? C7 H7A 0.86(3) . ? C8 C9 1.417(4) . ? C8 H8A 0.84(3) . ? C9 C10 1.402(4) . ? C9 H9A 0.90(3) . ? C10 H10A 0.87(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 Nb1 C2 148.54(11) . . ? C8 Nb1 C3 154.71(10) . . ? C2 Nb1 C3 35.13(10) . . ? C8 Nb1 C1 144.29(11) . . ? C2 Nb1 C1 34.60(10) . . ? C3 Nb1 C1 57.58(10) . . ? C8 Nb1 C7 34.88(11) . . ? C2 Nb1 C7 116.10(11) . . ? C3 Nb1 C7 144.58(11) . . ? C1 Nb1 C7 113.15(11) . . ? C8 Nb1 C6 57.18(11) . . ? C2 Nb1 C6 106.56(11) . . ? C3 Nb1 C6 141.34(11) . . ? C1 Nb1 C6 87.12(11) . . ? C7 Nb1 C6 33.89(11) . . ? C8 Nb1 C9 34.71(10) . . ? C2 Nb1 C9 160.38(10) . . ? C3 Nb1 C9 157.51(10) . . ? C1 Nb1 C9 127.35(10) . . ? C7 Nb1 C9 57.40(10) . . ? C6 Nb1 C9 56.94(10) . . ? C8 Nb1 C10 57.11(10) . . ? C2 Nb1 C10 126.39(10) . . ? C3 Nb1 C10 148.03(10) . . ? C1 Nb1 C10 94.61(10) . . ? C7 Nb1 C10 56.82(11) . . ? C6 Nb1 C10 34.31(10) . . ? C9 Nb1 C10 33.99(9) . . ? C8 Nb1 C4 153.36(11) . . ? C2 Nb1 C4 57.41(10) . . ? C3 Nb1 C4 34.45(10) . . ? C1 Nb1 C4 56.67(10) . . ? C7 Nb1 C4 169.61(11) . . ? C6 Nb1 C4 136.96(11) . . ? C9 Nb1 C4 125.50(10) . . ? C10 Nb1 C4 118.93(11) . . ? C8 Nb1 C5 146.71(10) . . ? C2 Nb1 C5 57.34(10) . . ? C3 Nb1 C5 57.07(10) . . ? C1 Nb1 C5 34.30(10) . . ? C7 Nb1 C5 136.73(11) . . ? C6 Nb1 C5 103.31(11) . . ? C9 Nb1 C5 112.83(10) . . ? C10 Nb1 C5 91.20(10) . . ? C4 Nb1 C5 33.65(10) . . ? C8 Nb1 Al1 77.47(8) . . ? C2 Nb1 Al1 101.42(8) . . ? C3 Nb1 Al1 77.91(7) . . ? C1 Nb1 Al1 134.19(8) . . ? C7 Nb1 Al1 96.28(9) . . ? C6 Nb1 Al1 129.87(8) . . ? C9 Nb1 Al1 97.82(7) . . ? C10 Nb1 Al1 131.18(7) . . ? C4 Nb1 Al1 93.16(8) . . ? C5 Nb1 Al1 126.82(8) . . ? C8 Nb1 H3 80.7(12) . . ? C2 Nb1 H3 75.7(12) . . ? C3 Nb1 H3 78.8(12) . . ? C1 Nb1 H3 107.0(12) . . ? C7 Nb1 H3 71.7(12) . . ? C6 Nb1 H3 99.6(12) . . ? C9 Nb1 H3 115.3(12) . . ? C10 Nb1 H3 128.5(12) . . ? C4 Nb1 H3 112.0(12) . . ? C5 Nb1 H3 131.8(12) . . ? Al1 Nb1 H3 49.0(12) . . ? C8 Nb1 H4 84.5(12) . . ? C2 Nb1 H4 119.0(12) . . ? C3 Nb1 H4 83.9(12) . . ? C1 Nb1 H4 126.9(12) . . ? C7 Nb1 H4 118.9(12) . . ? C6 Nb1 H4 133.8(12) . . ? C9 Nb1 H4 76.9(12) . . ? C10 Nb1 H4 104.9(12) . . ? C4 Nb1 H4 70.8(12) . . ? C5 Nb1 H4 95.5(12) . . ? Al1 Nb1 H4 49.4(12) . . ? H3 Nb1 H4 98.4(17) . . ? Nb1 Al1 Al1 130.66(5) . 3_565 ? Nb1 Al1 H1 118.4(9) . . ? Al1 Al1 H1 40.0(8) 3_565 . ? Nb1 Al1 H2 128.4(11) . . ? Al1 Al1 H2 100.6(11) 3_565 . ? H1 Al1 H2 104.0(14) . . ? Nb1 Al1 H3 37.2(10) . . ? Al1 Al1 H3 110.0(10) 3_565 . ? H1 Al1 H3 126.6(13) . . ? H2 Al1 H3 127.9(15) . . ? Nb1 Al1 H4 40.0(10) . . ? Al1 Al1 H4 132.1(10) 3_565 . ? H1 Al1 H4 96.5(13) . . ? H2 Al1 H4 111.5(15) . . ? H3 Al1 H4 77.2(14) . . ? C2 C1 C5 108.4(3) . . ? C2 C1 Nb1 71.8(2) . . ? C5 C1 Nb1 74.2(2) . . ? C2 C1 H1A 125.7(19) . . ? C5 C1 H1A 125.9(19) . . ? Nb1 C1 H1A 119.8(19) . . ? C1 C2 C3 107.4(3) . . ? C1 C2 Nb1 73.6(2) . . ? C3 C2 Nb1 72.5(2) . . ? C1 C2 H2A 124.7(22) . . ? C3 C2 H2A 128.0(22) . . ? Nb1 C2 H2A 119.5(21) . . ? C4 C3 C2 107.8(3) . . ? C4 C3 Nb1 74.9(2) . . ? C2 C3 Nb1 72.4(2) . . ? C4 C3 H3A 125.5(19) . . ? C2 C3 H3A 126.0(19) . . ? Nb1 C3 H3A 126.4(20) . . ? C5 C4 C3 108.4(3) . . ? C5 C4 Nb1 73.2(2) . . ? C3 C4 Nb1 70.6(2) . . ? C5 C4 H4A 125.4(23) . . ? C3 C4 H4A 126.2(23) . . ? Nb1 C4 H4A 119.6(22) . . ? C4 C5 C1 108.0(3) . . ? C4 C5 Nb1 73.1(2) . . ? C1 C5 Nb1 71.5(2) . . ? C4 C5 H5A 130.0(19) . . ? C1 C5 H5A 121.9(19) . . ? Nb1 C5 H5A 122.6(19) . . ? C7 C6 C10 108.4(3) . . ? C7 C6 Nb1 72.5(2) . . ? C10 C6 Nb1 73.2(2) . . ? C7 C6 H6A 126.1(22) . . ? C10 C6 H6A 125.4(22) . . ? Nb1 C6 H6A 116.8(22) . . ? C6 C7 C8 107.9(3) . . ? C6 C7 Nb1 73.6(2) . . ? C8 C7 Nb1 71.6(2) . . ? C6 C7 H7A 129.7(23) . . ? C8 C7 H7A 122.4(23) . . ? Nb1 C7 H7A 121.7(22) . . ? C9 C8 C7 107.9(3) . . ? C9 C8 Nb1 74.3(2) . . ? C7 C8 Nb1 73.6(2) . . ? C9 C8 H8A 123.4(21) . . ? C7 C8 H8A 128.6(21) . . ? Nb1 C8 H8A 119.9(21) . . ? C10 C9 C8 107.5(3) . . ? C10 C9 Nb1 73.2(2) . . ? C8 C9 Nb1 71.0(2) . . ? C10 C9 H9A 124.9(19) . . ? C8 C9 H9A 127.6(19) . . ? Nb1 C9 H9A 121.7(18) . . ? C9 C10 C6 108.3(3) . . ? C9 C10 Nb1 72.77(15) . . ? C6 C10 Nb1 72.5(2) . . ? C9 C10 H10A 126.8(20) . . ? C6 C10 H10A 124.9(20) . . ? Nb1 C10 H10A 119.8(20) . . ? _refine_diff_density_max 0.485 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.072 #==end data_compound21 _database_code_CSD 175463 # Cp2NbH2SiMe2PPh2 (Compound 21) _audit_creation_method SHELXL _chemical_name_systematic ; bis(cyclopentadienyl)(dimethyl(diphenylphosphido)silyl)dihydride niobium(V) ; _chemical_name_common ; dimethyl(diphenylphosphido)silyl niobocen dihydride ; _chemical_formula_moiety 'Cp2NbH2SiMe2PPh2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H28 Nb P Si' _chemical_formula_weight 468.43 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3692(2) _cell_length_b 12.83310(10) _cell_length_c 12.6511(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.8480(10) _cell_angle_gamma 90.00 _cell_volume 2167.85(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'light-yellow' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method ? _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15272 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.58 _reflns_number_total 5007 _reflns_number_observed 4526 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 16 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+1.1705P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4991 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_obs 0.0209 _refine_ls_wR_factor_all 0.0552 _refine_ls_wR_factor_obs 0.0497 _refine_ls_goodness_of_fit_all 1.117 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_restrained_S_all 1.147 _refine_ls_restrained_S_obs 1.091 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nb1 Nb 0.269125(10) 0.016816(10) 0.473838(10) 0.01914(5) Uani 1 d . . P1 P 0.26411(3) -0.29321(3) 0.39864(3) 0.01837(8) Uani 1 d . . Si1 Si 0.17435(3) -0.16428(3) 0.47856(3) 0.01787(9) Uani 1 d . . C1 C 0.3250(2) 0.11893(14) 0.33009(14) 0.0352(4) Uani 1 d . . C2 C 0.2258(2) 0.15039(15) 0.3473(2) 0.0391(4) Uani 1 d . . C3 C 0.16146(15) 0.0656(2) 0.32373(14) 0.0341(4) Uani 1 d . . C4 C 0.22157(14) -0.01965(14) 0.29374(13) 0.0279(3) Uani 1 d . . C5 C 0.32293(14) 0.01438(14) 0.29598(13) 0.0295(4) Uani 1 d . . C6 C 0.39862(14) 0.10543(15) 0.57742(14) 0.0321(4) Uani 1 d . . C7 C 0.30615(15) 0.15299(14) 0.59951(14) 0.0325(4) Uani 1 d . . C8 C 0.24712(14) 0.07930(15) 0.65049(14) 0.0316(4) Uani 1 d . . C9 C 0.30239(14) -0.01515(14) 0.65877(13) 0.0295(4) Uani 1 d . . C10 C 0.39646(14) 0.00229(14) 0.61467(14) 0.0313(4) Uani 1 d . . C11 C 0.38131(11) -0.31297(12) 0.47893(13) 0.0229(3) Uani 1 d . . C12 C 0.46187(13) -0.35459(13) 0.4259(2) 0.0304(4) Uani 1 d . . C13 C 0.55158(14) -0.37953(14) 0.4802(2) 0.0415(5) Uani 1 d . . C14 C 0.56287(14) -0.36342(14) 0.5881(2) 0.0449(5) Uani 1 d . . C15 C 0.4849(2) -0.32067(14) 0.6418(2) 0.0386(5) Uani 1 d . . C16 C 0.39464(13) -0.29480(13) 0.58792(14) 0.0283(3) Uani 1 d . . C17 C 0.19623(11) -0.41444(11) 0.42844(11) 0.0187(3) Uani 1 d . . C18 C 0.21844(12) -0.47722(12) 0.51682(13) 0.0226(3) Uani 1 d . . C19 C 0.16747(13) -0.57018(13) 0.53260(14) 0.0265(3) Uani 1 d . . C20 C 0.09223(13) -0.60197(13) 0.46035(14) 0.0286(3) Uani 1 d . . C21 C 0.06674(13) -0.53940(15) 0.37379(14) 0.0311(4) Uani 1 d . . C22 C 0.11838(13) -0.44686(14) 0.35787(13) 0.0268(3) Uani 1 d . . C23 C 0.05241(12) -0.17280(14) 0.39447(14) 0.0265(3) Uani 1 d . . C24 C 0.13129(12) -0.21661(13) 0.60911(12) 0.0239(3) Uani 1 d . . H1' H 0.1507(18) -0.0005(16) 0.5018(18) 0.043(6) Uiso 1 d . . H2' H 0.3402(15) -0.0903(16) 0.4544(16) 0.037(5) Uiso 1 d . . H1 H 0.3812(17) 0.1596(17) 0.3416(17) 0.040(6) Uiso 1 d . . H2 H 0.2037(18) 0.2140(20) 0.3714(19) 0.053(7) Uiso 1 d . . H3 H 0.0914(15) 0.0633(16) 0.3284(15) 0.031(5) Uiso 1 d . . H4 H 0.1993(14) -0.0848(16) 0.2682(15) 0.027(5) Uiso 1 d . . H5 H 0.3785(17) -0.0242(16) 0.2781(17) 0.037(6) Uiso 1 d . . H6 H 0.4498(17) 0.1369(17) 0.5457(17) 0.040(6) Uiso 1 d . . H7 H 0.2868(17) 0.2184(19) 0.5823(18) 0.048(6) Uiso 1 d . . H8 H 0.1832(16) 0.0912(17) 0.6730(16) 0.039(6) Uiso 1 d . . H9 H 0.2828(15) -0.0747(17) 0.6926(16) 0.033(5) Uiso 1 d . . H10 H 0.4471(17) -0.0459(17) 0.6129(17) 0.039(6) Uiso 1 d . . H12 H 0.4562(16) -0.3660(16) 0.3479(17) 0.039(6) Uiso 1 d . . H13 H 0.6026(18) -0.4086(19) 0.4426(18) 0.052(7) Uiso 1 d . . H14 H 0.6202(19) -0.3804(19) 0.6218(19) 0.053(7) Uiso 1 d . . H15 H 0.4885(16) -0.3090(16) 0.7130(17) 0.035(5) Uiso 1 d . . H16 H 0.3447(16) -0.2684(16) 0.6241(16) 0.035(5) Uiso 1 d . . H18 H 0.2681(14) -0.4562(14) 0.5672(14) 0.022(4) Uiso 1 d . . H19 H 0.1828(15) -0.6107(16) 0.5921(16) 0.031(5) Uiso 1 d . . H20 H 0.0590(15) -0.6634(16) 0.4696(16) 0.033(5) Uiso 1 d . . H21 H 0.0149(17) -0.5580(18) 0.3256(18) 0.045(6) Uiso 1 d . . H22 H 0.1006(15) -0.4071(16) 0.2972(16) 0.037(5) Uiso 1 d . . H23A H 0.0064(19) -0.1238(20) 0.4203(20) 0.060(7) Uiso 1 d . . H23B H 0.0599(17) -0.1584(18) 0.3212(19) 0.050(6) Uiso 1 d . . H23C H 0.0233(16) -0.2415(18) 0.3956(16) 0.042(6) Uiso 1 d . . H24A H 0.0741(17) -0.1776(17) 0.6289(17) 0.041(6) Uiso 1 d . . H24B H 0.1096(15) -0.2879(17) 0.6014(15) 0.033(5) Uiso 1 d . . H24C H 0.1794(15) -0.2146(15) 0.6667(15) 0.031(5) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.02143(8) 0.01564(8) 0.02022(8) -0.00090(5) -0.00018(5) -0.00099(5) P1 0.0188(2) 0.0185(2) 0.0177(2) -0.00035(14) -0.00019(14) -0.00205(14) Si1 0.0175(2) 0.0188(2) 0.0170(2) -0.00047(15) -0.00160(15) -0.00122(15) C1 0.0504(11) 0.0273(9) 0.0280(8) 0.0041(7) 0.0043(8) -0.0139(8) C2 0.0625(13) 0.0235(9) 0.0309(9) 0.0062(7) -0.0013(9) 0.0090(9) C3 0.0364(10) 0.0384(10) 0.0271(8) 0.0081(7) -0.0039(7) 0.0077(8) C4 0.0366(9) 0.0266(8) 0.0199(7) 0.0024(6) -0.0033(6) -0.0047(7) C5 0.0361(9) 0.0297(9) 0.0231(8) -0.0002(7) 0.0057(7) -0.0041(7) C6 0.0323(9) 0.0338(9) 0.0300(9) -0.0074(7) -0.0004(7) -0.0139(7) C7 0.0452(10) 0.0216(8) 0.0304(9) -0.0076(7) -0.0013(8) -0.0032(7) C8 0.0337(9) 0.0366(10) 0.0246(8) -0.0091(7) 0.0024(7) -0.0028(8) C9 0.0361(9) 0.0297(9) 0.0221(8) 0.0001(7) -0.0067(7) -0.0096(7) C10 0.0295(9) 0.0320(9) 0.0313(9) -0.0064(7) -0.0092(7) -0.0005(7) C11 0.0202(7) 0.0161(7) 0.0318(8) 0.0029(6) -0.0030(6) -0.0041(5) C12 0.0241(8) 0.0195(8) 0.0477(11) 0.0014(7) 0.0022(7) -0.0026(6) C13 0.0220(8) 0.0230(9) 0.079(2) 0.0016(9) -0.0021(9) 0.0016(7) C14 0.0266(9) 0.0225(9) 0.083(2) 0.0102(10) -0.0229(10) -0.0036(7) C15 0.0404(10) 0.0271(9) 0.0461(11) 0.0080(8) -0.0213(9) -0.0106(8) C16 0.0263(8) 0.0246(8) 0.0330(9) 0.0026(7) -0.0065(7) -0.0052(7) C17 0.0181(6) 0.0187(7) 0.0194(7) -0.0035(5) 0.0023(5) -0.0007(5) C18 0.0213(7) 0.0206(7) 0.0254(8) -0.0019(6) -0.0026(6) 0.0004(6) C19 0.0290(8) 0.0208(8) 0.0298(8) 0.0026(6) 0.0017(7) 0.0003(6) C20 0.0295(8) 0.0233(8) 0.0335(9) -0.0041(7) 0.0069(7) -0.0089(7) C21 0.0299(8) 0.0385(10) 0.0246(8) -0.0064(7) -0.0010(7) -0.0141(8) C22 0.0279(8) 0.0321(9) 0.0200(7) 0.0003(6) -0.0015(6) -0.0078(7) C23 0.0208(7) 0.0297(9) 0.0285(8) 0.0009(7) -0.0046(6) -0.0025(7) C24 0.0254(8) 0.0266(8) 0.0197(7) -0.0025(6) 0.0020(6) -0.0043(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 C4 2.381(2) . ? Nb1 C1 2.391(2) . ? Nb1 C9 2.395(2) . ? Nb1 C5 2.396(2) . ? Nb1 C2 2.397(2) . ? Nb1 C7 2.398(2) . ? Nb1 C6 2.405(2) . ? Nb1 C8 2.406(2) . ? Nb1 C3 2.408(2) . ? Nb1 C10 2.410(2) . ? Nb1 Si1 2.6491(4) . ? P1 C11 1.842(2) . ? P1 C17 1.849(2) . ? P1 Si1 2.3065(5) . ? Si1 C24 1.899(2) . ? Si1 C23 1.905(2) . ? C1 C5 1.409(3) . ? C1 C2 1.413(3) . ? C2 C3 1.410(3) . ? C3 C4 1.420(3) . ? C4 C5 1.423(3) . ? C6 C10 1.406(3) . ? C6 C7 1.419(3) . ? C7 C8 1.408(3) . ? C8 C9 1.421(3) . ? C9 C10 1.419(3) . ? C11 C16 1.401(2) . ? C11 C12 1.402(2) . ? C12 C13 1.389(3) . ? C13 C14 1.381(3) . ? C14 C15 1.386(3) . ? C15 C16 1.396(2) . ? C17 C18 1.398(2) . ? C17 C22 1.400(2) . ? C18 C19 1.393(2) . ? C19 C20 1.387(2) . ? C20 C21 1.387(3) . ? C21 C22 1.393(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Nb1 C1 57.22(6) . . ? C4 Nb1 C9 158.24(6) . . ? C1 Nb1 C9 141.91(6) . . ? C4 Nb1 C5 34.65(6) . . ? C1 Nb1 C5 34.24(6) . . ? C9 Nb1 C5 149.90(7) . . ? C4 Nb1 C2 57.12(6) . . ? C1 Nb1 C2 34.33(7) . . ? C9 Nb1 C2 143.33(7) . . ? C5 Nb1 C2 57.03(7) . . ? C4 Nb1 C7 144.51(6) . . ? C1 Nb1 C7 92.46(6) . . ? C9 Nb1 C7 56.97(6) . . ? C5 Nb1 C7 124.78(6) . . ? C2 Nb1 C7 87.53(7) . . ? C4 Nb1 C6 139.92(6) . . ? C1 Nb1 C6 84.94(6) . . ? C9 Nb1 C6 56.97(6) . . ? C5 Nb1 C6 106.04(6) . . ? C2 Nb1 C6 99.75(7) . . ? C7 Nb1 C6 34.37(7) . . ? C4 Nb1 C8 156.21(6) . . ? C1 Nb1 C8 125.52(6) . . ? C9 Nb1 C8 34.42(6) . . ? C5 Nb1 C8 158.87(6) . . ? C2 Nb1 C8 110.22(7) . . ? C7 Nb1 C8 34.10(6) . . ? C6 Nb1 C8 56.92(6) . . ? C4 Nb1 C3 34.50(6) . . ? C1 Nb1 C3 56.95(7) . . ? C9 Nb1 C3 152.82(7) . . ? C5 Nb1 C3 57.21(7) . . ? C2 Nb1 C3 34.11(7) . . ? C7 Nb1 C3 115.41(7) . . ? C6 Nb1 C3 133.85(7) . . ? C8 Nb1 C3 123.36(7) . . ? C4 Nb1 C10 146.88(7) . . ? C1 Nb1 C10 111.65(7) . . ? C9 Nb1 C10 34.35(6) . . ? C5 Nb1 C10 117.34(7) . . ? C2 Nb1 C10 133.45(7) . . ? C7 Nb1 C10 56.70(6) . . ? C6 Nb1 C10 33.96(6) . . ? C8 Nb1 C10 56.87(6) . . ? C3 Nb1 C10 167.40(7) . . ? C4 Nb1 Si1 75.16(4) . . ? C1 Nb1 Si1 131.74(5) . . ? C9 Nb1 Si1 83.89(4) . . ? C5 Nb1 Si1 100.13(4) . . ? C2 Nb1 Si1 122.85(5) . . ? C7 Nb1 Si1 135.05(5) . . ? C6 Nb1 Si1 137.29(5) . . ? C8 Nb1 Si1 101.00(5) . . ? C3 Nb1 Si1 88.74(5) . . ? C10 Nb1 Si1 103.69(5) . . ? C11 P1 C17 100.62(7) . . ? C11 P1 Si1 107.69(5) . . ? C17 P1 Si1 104.05(5) . . ? C24 Si1 C23 100.22(8) . . ? C24 Si1 P1 108.33(6) . . ? C23 Si1 P1 99.41(6) . . ? C24 Si1 Nb1 119.73(5) . . ? C23 Si1 Nb1 115.77(6) . . ? P1 Si1 Nb1 111.08(2) . . ? C5 C1 C2 108.4(2) . . ? C5 C1 Nb1 73.09(10) . . ? C2 C1 Nb1 73.08(10) . . ? C3 C2 C1 108.3(2) . . ? C3 C2 Nb1 73.37(10) . . ? C1 C2 Nb1 72.60(10) . . ? C2 C3 C4 107.7(2) . . ? C2 C3 Nb1 72.52(10) . . ? C4 C3 Nb1 71.72(9) . . ? C3 C4 C5 108.0(2) . . ? C3 C4 Nb1 73.78(10) . . ? C5 C4 Nb1 73.25(9) . . ? C1 C5 C4 107.6(2) . . ? C1 C5 Nb1 72.67(10) . . ? C4 C5 Nb1 72.10(10) . . ? C10 C6 C7 107.8(2) . . ? C10 C6 Nb1 73.21(10) . . ? C7 C6 Nb1 72.55(10) . . ? C8 C7 C6 108.4(2) . . ? C8 C7 Nb1 73.28(10) . . ? C6 C7 Nb1 73.09(10) . . ? C7 C8 C9 107.8(2) . . ? C7 C8 Nb1 72.62(10) . . ? C9 C8 Nb1 72.36(10) . . ? C10 C9 C8 107.7(2) . . ? C10 C9 Nb1 73.38(10) . . ? C8 C9 Nb1 73.21(10) . . ? C6 C10 C9 108.3(2) . . ? C6 C10 Nb1 72.83(10) . . ? C9 C10 Nb1 72.27(10) . . ? C16 C11 C12 118.1(2) . . ? C16 C11 P1 125.65(13) . . ? C12 C11 P1 116.18(13) . . ? C13 C12 C11 121.1(2) . . ? C14 C13 C12 120.2(2) . . ? C13 C14 C15 119.8(2) . . ? C14 C15 C16 120.5(2) . . ? C15 C16 C11 120.4(2) . . ? C18 C17 C22 117.41(14) . . ? C18 C17 P1 124.12(11) . . ? C22 C17 P1 118.46(12) . . ? C19 C18 C17 121.48(14) . . ? C20 C19 C18 120.1(2) . . ? C19 C20 C21 119.5(2) . . ? C20 C21 C22 120.2(2) . . ? C21 C22 C17 121.3(2) . . ? _refine_diff_density_max 0.375 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.058 #==end data_compound24 _database_code_CSD 175464 # Cp2Nb(SiMe2OMe)2H (Compound 24) _audit_creation_method SHELXL _chemical_name_systematic ; bis(cyclopentadienyl)bis(dimethylmethoxysilyl)hydride niobium(V) ; _chemical_name_common ; bis(dimethylmethoxysilyl)niobocen monohydride ; _chemical_formula_moiety 'Cp2Nb(SiMe2OMe)2H' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H29 Nb O2 Si2' _chemical_formula_weight 402.48 _chemical_melting_point ? _chemical_compound_source ? 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' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.77290(10) _cell_length_b 10.5018(2) _cell_length_c 13.0324(2) _cell_angle_alpha 70.1000(10) _cell_angle_beta 72.7390(10) _cell_angle_gamma 73.9360(10) _cell_volume 936.79(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method ? _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6066 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3648 _reflns_number_observed 3287 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 152 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.7843P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0041(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3496 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_obs 0.0361 _refine_ls_wR_factor_all 0.0959 _refine_ls_wR_factor_obs 0.0843 _refine_ls_goodness_of_fit_all 1.109 _refine_ls_goodness_of_fit_obs 1.111 _refine_ls_restrained_S_all 1.193 _refine_ls_restrained_S_obs 1.111 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nb1 Nb 0.34173(4) 0.70585(3) 0.66717(2) 0.01450(12) Uani 1 d . . Si1 Si 0.30376(12) 0.45993(9) 0.80271(7) 0.0173(2) Uani 1 d . . Si2 Si 0.15753(12) 0.88968(9) 0.77579(7) 0.0184(2) Uani 1 d . . O1 O 0.4165(4) 0.3381(2) 0.7350(2) 0.0277(6) Uani 1 d . . O2 O 0.1773(4) 1.0491(2) 0.6887(2) 0.0269(6) Uani 1 d . . C1 C 0.0474(5) 0.7126(4) 0.6414(3) 0.0232(7) Uani 1 d . . C2 C 0.1733(5) 0.6124(4) 0.5915(3) 0.0234(7) Uani 1 d . . C3 C 0.3003(5) 0.6803(4) 0.5011(3) 0.0259(7) Uani 1 d . . C4 C 0.2501(5) 0.8236(4) 0.4943(3) 0.0265(8) Uani 1 d . . C5 C 0.0943(5) 0.8439(4) 0.5801(3) 0.0267(8) Uani 1 d . . C6 C 0.5772(5) 0.6803(4) 0.7596(3) 0.0236(7) Uani 1 d . . C7 C 0.6412(5) 0.5830(4) 0.6965(3) 0.0255(8) Uani 1 d . . C8 C 0.6619(5) 0.6569(4) 0.5828(3) 0.0258(8) Uani 1 d . . C9 C 0.6145(5) 0.8007(4) 0.5739(3) 0.0234(7) Uani 1 d . . C10 C 0.5618(4) 0.8156(4) 0.6829(3) 0.0213(7) Uani 1 d . . C11 C 0.0601(5) 0.4289(4) 0.8604(3) 0.0250(7) Uani 1 d . . C12 C 0.3959(5) 0.4081(4) 0.9331(3) 0.0279(8) Uani 1 d . . C13 C 0.2326(6) 0.8773(4) 0.9048(3) 0.0279(8) Uani 1 d . . C14 C -0.0983(5) 0.8916(4) 0.8310(4) 0.0296(8) Uani 1 d . . C15 C 0.4513(8) 0.1954(4) 0.7919(4) 0.0444(11) Uani 1 d . . C16 C 0.0584(7) 1.1719(4) 0.7091(4) 0.0402(10) Uani 1 d . . H1A H -0.0491(58) 0.6945(42) 0.7039(36) 0.029(11) Uiso 1 d . . H2A H 0.1612(58) 0.5218(47) 0.6078(37) 0.033(11) Uiso 1 d . . H3A H 0.3916(50) 0.6411(37) 0.4550(32) 0.014(9) Uiso 1 d . . H4A H 0.3156(66) 0.8960(50) 0.4381(42) 0.047(13) Uiso 1 d . . H5A H 0.0328(60) 0.9194(47) 0.5876(37) 0.033(12) Uiso 1 d . . H6A H 0.5581(61) 0.6565(46) 0.8346(41) 0.037(12) Uiso 1 d . . H7A H 0.6621(59) 0.4931(49) 0.7236(38) 0.035(12) Uiso 1 d . . H8A H 0.6948(56) 0.6191(42) 0.5215(36) 0.028(10) Uiso 1 d . . H9A H 0.6279(57) 0.8678(45) 0.5091(37) 0.030(11) Uiso 1 d . . H10A H 0.5357(50) 0.8925(41) 0.6987(31) 0.018(9) Uiso 1 d . . H11A H 0.0599(62) 0.3343(50) 0.9088(40) 0.041(12) Uiso 1 d . . H11B H -0.0040(59) 0.4440(43) 0.8070(38) 0.031(11) Uiso 1 d . . H11C H -0.0078(64) 0.4904(49) 0.9001(40) 0.040(12) Uiso 1 d . . H12A H 0.3695(67) 0.3223(54) 0.9787(43) 0.048(14) Uiso 1 d . . H12B H 0.3317(73) 0.4766(56) 0.9810(46) 0.059(15) Uiso 1 d . . H12C H 0.5265(63) 0.4019(43) 0.9168(36) 0.034(11) Uiso 1 d . . H13A H 0.1617(67) 0.9508(52) 0.9438(42) 0.049(14) Uiso 1 d . . H13B H 0.3509(65) 0.8806(45) 0.8908(37) 0.034(12) Uiso 1 d . . H13C H 0.2158(63) 0.7912(50) 0.9624(41) 0.042(12) Uiso 1 d . . H14A H -0.1609(76) 0.9571(60) 0.8728(49) 0.064(17) Uiso 1 d . . H14B H -0.1126(63) 0.8034(53) 0.8702(40) 0.041(13) Uiso 1 d . . H14C H -0.1621(65) 0.9204(48) 0.7708(42) 0.043(13) Uiso 1 d . . H15A H 0.4862(84) 0.1417(65) 0.7398(55) 0.077(19) Uiso 1 d . . H15B H 0.3379(78) 0.1711(56) 0.8484(48) 0.060(16) Uiso 1 d . . H15C H 0.5433(80) 0.1735(58) 0.8299(49) 0.060(17) Uiso 1 d . . H16A H 0.1164(100) 1.2422(77) 0.6813(63) 0.098(24) Uiso 1 d . . H16B H 0.0212(65) 1.1653(49) 0.7899(45) 0.045(13) Uiso 1 d . . H16C H -0.0483(81) 1.1934(57) 0.6830(49) 0.062(17) Uiso 1 d . . H1 H 0.2088(65) 0.6720(49) 0.8156(42) 0.050(14) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0153(2) 0.0128(2) 0.0126(2) -0.00062(10) -0.00127(10) -0.00412(10) Si1 0.0180(4) 0.0151(4) 0.0155(4) -0.0006(3) -0.0010(3) -0.0058(3) Si2 0.0214(4) 0.0148(4) 0.0157(4) -0.0026(3) -0.0009(3) -0.0043(3) O1 0.0328(14) 0.0153(11) 0.0261(13) -0.0041(10) 0.0049(11) -0.0052(10) O2 0.0363(14) 0.0134(11) 0.0241(13) -0.0006(9) -0.0011(11) -0.0059(10) C1 0.020(2) 0.028(2) 0.024(2) -0.0062(14) -0.0071(14) -0.0063(14) C2 0.030(2) 0.022(2) 0.023(2) -0.0067(14) -0.0096(14) -0.0072(14) C3 0.031(2) 0.028(2) 0.017(2) -0.0072(14) -0.0045(15) -0.0034(15) C4 0.035(2) 0.026(2) 0.014(2) 0.0036(14) -0.0086(14) -0.008(2) C5 0.030(2) 0.023(2) 0.026(2) -0.0050(15) -0.014(2) 0.0026(15) C6 0.018(2) 0.027(2) 0.023(2) -0.0005(14) -0.0060(14) -0.0081(14) C7 0.017(2) 0.019(2) 0.035(2) -0.0017(15) -0.0034(14) -0.0049(13) C8 0.017(2) 0.027(2) 0.030(2) -0.010(2) 0.0054(14) -0.0081(14) C9 0.022(2) 0.022(2) 0.021(2) -0.0004(14) 0.0017(14) -0.0111(14) C10 0.017(2) 0.018(2) 0.029(2) -0.0061(14) -0.0014(13) -0.0078(13) C11 0.025(2) 0.025(2) 0.024(2) -0.005(2) -0.0002(15) -0.0106(14) C12 0.031(2) 0.027(2) 0.022(2) 0.0054(15) -0.008(2) -0.012(2) C13 0.034(2) 0.028(2) 0.022(2) -0.006(2) -0.003(2) -0.011(2) C14 0.023(2) 0.028(2) 0.031(2) -0.011(2) 0.004(2) -0.003(2) C15 0.054(3) 0.017(2) 0.048(3) -0.005(2) 0.002(2) -0.005(2) C16 0.054(3) 0.019(2) 0.042(3) -0.007(2) -0.009(2) -0.002(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 Nb1 C4 2.383(3) . ? Nb1 C6 2.386(3) . ? Nb1 C1 2.388(3) . ? Nb1 C3 2.391(4) . ? Nb1 C5 2.392(4) . ? Nb1 C8 2.392(3) . ? Nb1 C10 2.399(3) . ? Nb1 C7 2.400(3) . ? Nb1 C9 2.404(3) . ? Nb1 C2 2.405(3) . ? Nb1 Si1 2.6238(9) . ? Nb1 Si2 2.6284(9) . ? Si1 O1 1.695(3) . ? Si1 C12 1.890(4) . ? Si1 C11 1.894(4) . ? Si2 O2 1.691(2) . ? Si2 C13 1.892(4) . ? Si2 C14 1.900(4) . ? O1 C15 1.416(5) . ? O2 C16 1.420(5) . ? C1 C2 1.416(5) . ? C1 C5 1.424(5) . ? C2 C3 1.414(5) . ? C3 C4 1.426(5) . ? C4 C5 1.405(5) . ? C6 C7 1.421(5) . ? C6 C10 1.429(5) . ? C7 C8 1.404(5) . ? C8 C9 1.424(5) . ? C9 C10 1.407(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Nb1 C6 141.28(13) . . ? C4 Nb1 C1 57.21(13) . . ? C6 Nb1 C1 159.80(13) . . ? C4 Nb1 C3 34.75(13) . . ? C6 Nb1 C3 141.12(13) . . ? C1 Nb1 C3 57.26(13) . . ? C4 Nb1 C5 34.24(13) . . ? C6 Nb1 C5 151.32(13) . . ? C1 Nb1 C5 34.66(12) . . ? C3 Nb1 C5 57.42(13) . . ? C4 Nb1 C8 94.81(13) . . ? C6 Nb1 C8 57.03(13) . . ? C1 Nb1 C8 141.28(13) . . ? C3 Nb1 C8 84.34(13) . . ? C5 Nb1 C8 128.56(13) . . ? C4 Nb1 C10 109.20(12) . . ? C6 Nb1 C10 34.75(12) . . ? C1 Nb1 C10 151.47(12) . . ? C3 Nb1 C10 127.85(13) . . ? C5 Nb1 C10 119.40(12) . . ? C8 Nb1 C10 57.11(12) . . ? C4 Nb1 C7 128.38(13) . . ? C6 Nb1 C7 34.53(13) . . ? C1 Nb1 C7 151.11(13) . . ? C3 Nb1 C7 109.37(13) . . ? C5 Nb1 C7 162.54(13) . . ? C8 Nb1 C7 34.06(13) . . ? C10 Nb1 C7 57.43(12) . . ? C4 Nb1 C9 84.46(13) . . ? C6 Nb1 C9 57.13(12) . . ? C1 Nb1 C9 141.45(12) . . ? C3 Nb1 C9 94.33(13) . . ? C5 Nb1 C9 109.70(13) . . ? C8 Nb1 C9 34.54(12) . . ? C10 Nb1 C9 34.08(12) . . ? C7 Nb1 C9 57.10(12) . . ? C4 Nb1 C2 57.19(12) . . ? C6 Nb1 C2 151.39(12) . . ? C1 Nb1 C2 34.36(12) . . ? C3 Nb1 C2 34.28(12) . . ? C5 Nb1 C2 57.29(12) . . ? C8 Nb1 C2 109.51(13) . . ? C10 Nb1 C2 162.06(12) . . ? C7 Nb1 C2 119.56(13) . . ? C9 Nb1 C2 128.10(12) . . ? C4 Nb1 Si1 129.86(10) . . ? C6 Nb1 Si1 84.24(9) . . ? C1 Nb1 Si1 83.62(9) . . ? C3 Nb1 Si1 99.36(9) . . ? C5 Nb1 Si1 118.18(10) . . ? C8 Nb1 Si1 99.43(9) . . ? C10 Nb1 Si1 118.92(9) . . ? C7 Nb1 Si1 73.03(9) . . ? C9 Nb1 Si1 130.03(9) . . ? C2 Nb1 Si1 72.75(9) . . ? C4 Nb1 Si2 98.05(10) . . ? C6 Nb1 Si2 84.78(9) . . ? C1 Nb1 Si2 83.76(9) . . ? C3 Nb1 Si2 128.99(9) . . ? C5 Nb1 Si2 71.74(10) . . ? C8 Nb1 Si2 129.96(9) . . ? C10 Nb1 Si2 73.00(9) . . ? C7 Nb1 Si2 119.27(10) . . ? C9 Nb1 Si2 99.18(9) . . ? C2 Nb1 Si2 118.09(9) . . ? Si1 Nb1 Si2 108.21(3) . . ? O1 Si1 C12 106.0(2) . . ? O1 Si1 C11 105.4(2) . . ? C12 Si1 C11 103.0(2) . . ? O1 Si1 Nb1 109.84(9) . . ? C12 Si1 Nb1 115.47(12) . . ? C11 Si1 Nb1 116.20(12) . . ? O2 Si2 C13 106.0(2) . . ? O2 Si2 C14 106.3(2) . . ? C13 Si2 C14 102.3(2) . . ? O2 Si2 Nb1 108.80(9) . . ? C13 Si2 Nb1 116.67(13) . . ? C14 Si2 Nb1 115.84(13) . . ? C15 O1 Si1 122.5(3) . . ? C16 O2 Si2 123.3(3) . . ? C2 C1 C5 108.1(3) . . ? C2 C1 Nb1 73.5(2) . . ? C5 C1 Nb1 72.8(2) . . ? C3 C2 C1 108.1(3) . . ? C3 C2 Nb1 72.3(2) . . ? C1 C2 Nb1 72.2(2) . . ? C2 C3 C4 107.6(3) . . ? C2 C3 Nb1 73.4(2) . . ? C4 C3 Nb1 72.3(2) . . ? C5 C4 C3 108.5(3) . . ? C5 C4 Nb1 73.2(2) . . ? C3 C4 Nb1 72.9(2) . . ? C4 C5 C1 107.7(3) . . ? C4 C5 Nb1 72.5(2) . . ? C1 C5 Nb1 72.5(2) . . ? C7 C6 C10 108.0(3) . . ? C7 C6 Nb1 73.3(2) . . ? C10 C6 Nb1 73.1(2) . . ? C8 C7 C6 107.7(3) . . ? C8 C7 Nb1 72.6(2) . . ? C6 C7 Nb1 72.2(2) . . ? C7 C8 C9 108.6(3) . . ? C7 C8 Nb1 73.3(2) . . ? C9 C8 Nb1 73.2(2) . . ? C10 C9 C8 108.0(3) . . ? C10 C9 Nb1 72.8(2) . . ? C8 C9 Nb1 72.3(2) . . ? C9 C10 C6 107.7(3) . . ? C9 C10 Nb1 73.2(2) . . ? C6 C10 Nb1 72.1(2) . . ? _refine_diff_density_max 0.550 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.104 #==end