#------------------------------------------------------------------------------
#$Date: 2020-10-10 04:31:56 +0300 (Sat, 10 Oct 2020) $
#$Revision: 258285 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/93/1559323.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1559323
loop_
_publ_author_name
'Fostvedt, Jade I.'
'Grant, Lauren N.'
'Kriegel, Benjamin M.'
'Obenhuber, Andreas H.'
'Lohrey, Trevor D.'
'Bergman, Robert G.'
'Arnold, John'
_publ_section_title
;
 1,2-Addition and cycloaddition reactions of niobium bis(imido) and oxo
 imido complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03489D
_journal_year                    2020
_chemical_formula_moiety         'C43 H67 N4 Nb Si, C6 H18 O Si2'
_chemical_formula_sum            'C49 H85 N4 Nb O Si3'
_chemical_formula_weight         923.38
_chemical_melting_point          393
_chemical_name_common            (BDI)NbH(N[SiH2Ph]tBu)(NtBu)
_chemical_name_systematic
'hydrido-(N-(tert-butyl)-1-phenylsilyl)amino-(tert-butyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V) hexamethyldisiloxane solvate'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-05-17 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                101.451(2)
_cell_angle_beta                 103.6950(10)
_cell_angle_gamma                103.1000(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6684(3)
_cell_length_b                   12.8523(4)
_cell_length_c                   21.1721(7)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.25
_cell_volume                     2647.70(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-2014
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46576
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.483
_diffrn_reflns_theta_min         1.688
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexamethyldisiloxane'
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         9696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0307P)²+3.5135P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7258
_reflns_number_total             9696
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03489d2.cif
_cod_data_source_block           shelx_CCDC5
_cod_original_cell_volume        2647.70(14)
_cod_database_code               1559323
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.984
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.2547(3) 0.4363(3) 0.73848(15) 0.0111(7) Uani 1 1 d . . . . .
C2 C -0.3372(3) 0.3263(3) 0.70766(15) 0.0130(7) Uani 1 1 d . . . . .
H2 H -0.4120 0.3036 0.7238 0.016 Uiso 1 1 calc R U . . .
C3 C -0.3232(3) 0.2471(3) 0.65682(16) 0.0124(7) Uani 1 1 d . . . . .
C4 C -0.3240(3) 0.5130(3) 0.77076(16) 0.0164(7) Uani 1 1 d . . . . .
H4A H -0.2565 0.5816 0.7997 0.025 Uiso 1 1 calc R U . . .
H4B H -0.3728 0.4767 0.7980 0.025 Uiso 1 1 calc R U . . .
H4C H -0.3875 0.5303 0.7355 0.025 Uiso 1 1 calc R U . . .
C5 C -0.4453(3) 0.1478(3) 0.62149(17) 0.0184(8) Uani 1 1 d . . . . .
H5A H -0.4426 0.1161 0.5759 0.028 Uiso 1 1 calc R U . . .
H5B H -0.5274 0.1710 0.6187 0.028 Uiso 1 1 calc R U . . .
H5C H -0.4450 0.0919 0.6470 0.028 Uiso 1 1 calc R U . . .
C6 C -0.0627(3) 0.5907(3) 0.76586(15) 0.0109(7) Uani 1 1 d . . . . .
C7 C -0.0023(3) 0.6354(3) 0.83578(15) 0.0129(7) Uani 1 1 d . . . . .
C8 C 0.0474(3) 0.7496(3) 0.86077(16) 0.0188(8) Uani 1 1 d . . . . .
H8 H 0.0871 0.7809 0.9080 0.023 Uiso 1 1 calc R U . . .
C9 C 0.0406(3) 0.8190(3) 0.81884(17) 0.0229(8) Uani 1 1 d . . . . .
H9 H 0.0726 0.8971 0.8372 0.027 Uiso 1 1 calc R U . . .
C10 C -0.0128(3) 0.7742(3) 0.75022(17) 0.0211(8) Uani 1 1 d . . . . .
H10 H -0.0148 0.8220 0.7213 0.025 Uiso 1 1 calc R U . . .
C11 C -0.0638(3) 0.6599(3) 0.72235(15) 0.0139(7) Uani 1 1 d . . . . .
C12 C 0.0099(3) 0.5647(3) 0.88474(16) 0.0169(7) Uani 1 1 d . . . . .
H12 H -0.0261 0.4852 0.8582 0.020 Uiso 1 1 calc R U . . .
C13 C -0.0714(3) 0.5848(3) 0.93427(17) 0.0272(9) Uani 1 1 d . . . . .
H13A H -0.0358 0.6618 0.9618 0.041 Uiso 1 1 calc R U . . .
H13B H -0.0643 0.5349 0.9636 0.041 Uiso 1 1 calc R U . . .
H13C H -0.1661 0.5705 0.9091 0.041 Uiso 1 1 calc R U . . .
C14 C 0.1578(3) 0.5857(3) 0.92443(17) 0.0243(8) Uani 1 1 d . . . . .
H14A H 0.2103 0.5738 0.8929 0.037 Uiso 1 1 calc R U . . .
H14B H 0.1638 0.5345 0.9529 0.037 Uiso 1 1 calc R U . . .
H14C H 0.1936 0.6622 0.9528 0.037 Uiso 1 1 calc R U . . .
C15 C -0.1223(3) 0.6151(3) 0.64628(15) 0.0157(7) Uani 1 1 d . . . . .
H15 H -0.1274 0.5346 0.6345 0.019 Uiso 1 1 calc R U . . .
C16 C -0.2657(3) 0.6243(3) 0.62270(18) 0.0264(9) Uani 1 1 d . . . . .
H16A H -0.3251 0.5760 0.6406 0.040 Uiso 1 1 calc R U . . .
H16B H -0.2981 0.6017 0.5733 0.040 Uiso 1 1 calc R U . . .
H16C H -0.2655 0.7012 0.6391 0.040 Uiso 1 1 calc R U . . .
C17 C -0.0323(4) 0.6725(3) 0.60973(17) 0.0237(8) Uani 1 1 d . . . . .
H17A H -0.0366 0.7489 0.6147 0.036 Uiso 1 1 calc R U . . .
H17B H -0.0632 0.6326 0.5618 0.036 Uiso 1 1 calc R U . . .
H17C H 0.0608 0.6728 0.6293 0.036 Uiso 1 1 calc R U . . .
C18 C -0.2209(3) 0.1895(2) 0.57223(15) 0.0109(7) Uani 1 1 d . . . . .
C19 C -0.2695(3) 0.2288(3) 0.51648(15) 0.0118(7) Uani 1 1 d . . . . .
C20 C -0.2846(3) 0.1654(3) 0.45211(16) 0.0175(8) Uani 1 1 d . . . . .
H20 H -0.3187 0.1906 0.4141 0.021 Uiso 1 1 calc R U . . .
C21 C -0.2517(3) 0.0673(3) 0.44208(17) 0.0197(8) Uani 1 1 d . . . . .
H21 H -0.2626 0.0253 0.3978 0.024 Uiso 1 1 calc R U . . .
C22 C -0.2022(3) 0.0306(3) 0.49758(17) 0.0179(8) Uani 1 1 d . . . . .
H22 H -0.1779 -0.0366 0.4908 0.022 Uiso 1 1 calc R U . . .
C23 C -0.1870(3) 0.0893(3) 0.56294(16) 0.0131(7) Uani 1 1 d . . . . .
C24 C -0.3088(3) 0.3362(3) 0.52332(16) 0.0149(7) Uani 1 1 d . . . . .
H24 H -0.2718 0.3792 0.5718 0.018 Uiso 1 1 calc R U . . .
C25 C -0.2475(3) 0.4069(3) 0.48185(17) 0.0232(8) Uani 1 1 d . . . . .
H25A H -0.1497 0.4198 0.4951 0.035 Uiso 1 1 calc R U . . .
H25B H -0.2680 0.4781 0.4901 0.035 Uiso 1 1 calc R U . . .
H25C H -0.2858 0.3680 0.4338 0.035 Uiso 1 1 calc R U . . .
C26 C -0.4618(3) 0.3155(3) 0.50273(19) 0.0269(9) Uani 1 1 d . . . . .
H26A H -0.5004 0.2743 0.4551 0.040 Uiso 1 1 calc R U . . .
H26B H -0.4825 0.3867 0.5095 0.040 Uiso 1 1 calc R U . . .
H26C H -0.5003 0.2724 0.5304 0.040 Uiso 1 1 calc R U . . .
C27 C -0.1386(3) 0.0402(3) 0.62030(16) 0.0157(7) Uani 1 1 d . . . . .
H27 H -0.1141 0.0985 0.6638 0.019 Uiso 1 1 calc R U . . .
C28 C -0.2511(4) -0.0584(3) 0.62069(19) 0.0272(9) Uani 1 1 d . . . . .
H28A H -0.3300 -0.0338 0.6249 0.041 Uiso 1 1 calc R U . . .
H28B H -0.2191 -0.0876 0.6589 0.041 Uiso 1 1 calc R U . . .
H28C H -0.2760 -0.1166 0.5785 0.041 Uiso 1 1 calc R U . . .
C29 C -0.0151(3) 0.0008(3) 0.61638(17) 0.0202(8) Uani 1 1 d . . . . .
H29A H -0.0399 -0.0618 0.5764 0.030 Uiso 1 1 calc R U . . .
H29B H 0.0182 -0.0226 0.6569 0.030 Uiso 1 1 calc R U . . .
H29C H 0.0557 0.0616 0.6133 0.030 Uiso 1 1 calc R U . . .
C30 C -0.0437(3) 0.2206(3) 0.83460(16) 0.0188(8) Uani 1 1 d . . . . .
C31 C -0.0995(4) 0.0965(3) 0.80028(18) 0.0281(9) Uani 1 1 d . . . . .
H31A H -0.1859 0.0819 0.7661 0.042 Uiso 1 1 calc R U . . .
H31B H -0.1127 0.0562 0.8340 0.042 Uiso 1 1 calc R U . . .
H31C H -0.0357 0.0718 0.7787 0.042 Uiso 1 1 calc R U . . .
C32 C -0.1469(4) 0.2599(3) 0.86548(18) 0.0270(9) Uani 1 1 d . . . . .
H32A H -0.1085 0.3382 0.8907 0.041 Uiso 1 1 calc R U . . .
H32B H -0.1696 0.2156 0.8960 0.041 Uiso 1 1 calc R U . . .
H32C H -0.2285 0.2512 0.8294 0.041 Uiso 1 1 calc R U . . .
C33 C 0.0897(4) 0.2454(3) 0.88933(17) 0.0293(9) Uani 1 1 d . . . . .
H33A H 0.1543 0.2188 0.8692 0.044 Uiso 1 1 calc R U . . .
H33B H 0.0748 0.2078 0.9240 0.044 Uiso 1 1 calc R U . . .
H33C H 0.1255 0.3255 0.9098 0.044 Uiso 1 1 calc R U . . .
C34 C 0.1755(3) 0.3550(3) 0.63487(15) 0.0124(7) Uani 1 1 d . . . . .
C35 C 0.0808(3) 0.4252(3) 0.61631(16) 0.0156(7) Uani 1 1 d . . . . .
H35A H -0.0125 0.3778 0.5989 0.023 Uiso 1 1 calc R U . . .
H35B H 0.1041 0.4596 0.5816 0.023 Uiso 1 1 calc R U . . .
H35C H 0.0905 0.4831 0.6565 0.023 Uiso 1 1 calc R U . . .
C36 C 0.1610(3) 0.2658(3) 0.57153(16) 0.0171(8) Uani 1 1 d . . . . .
H36A H 0.2193 0.2193 0.5833 0.026 Uiso 1 1 calc R U . . .
H36B H 0.1873 0.3013 0.5379 0.026 Uiso 1 1 calc R U . . .
H36C H 0.0671 0.2198 0.5529 0.026 Uiso 1 1 calc R U . . .
C37 C 0.3204(3) 0.4300(3) 0.66297(16) 0.0171(8) Uani 1 1 d . . . . .
H37A H 0.3293 0.4855 0.7041 0.026 Uiso 1 1 calc R U . . .
H37B H 0.3431 0.4674 0.6294 0.026 Uiso 1 1 calc R U . . .
H37C H 0.3817 0.3852 0.6734 0.026 Uiso 1 1 calc R U . . .
C38 C 0.3701(3) 0.3285(3) 0.80950(16) 0.0148(7) Uani 1 1 d . . . . .
C39 C 0.3715(3) 0.4350(3) 0.84135(16) 0.0178(8) Uani 1 1 d . . . . .
H39 H 0.3039 0.4657 0.8217 0.021 Uiso 1 1 calc R U . . .
C40 C 0.4694(3) 0.4968(3) 0.90095(17) 0.0212(8) Uani 1 1 d . . . . .
H40 H 0.4693 0.5697 0.9213 0.025 Uiso 1 1 calc R U . . .
C41 C 0.5667(3) 0.4530(3) 0.93070(17) 0.0246(9) Uani 1 1 d . . . . .
H41 H 0.6327 0.4948 0.9721 0.029 Uiso 1 1 calc R U . . .
C42 C 0.5684(3) 0.3481(3) 0.90041(17) 0.0254(9) Uani 1 1 d . . . . .
H42 H 0.6364 0.3181 0.9207 0.030 Uiso 1 1 calc R U . . .
C43 C 0.4717(3) 0.2866(3) 0.84080(17) 0.0233(8) Uani 1 1 d . . . . .
H43 H 0.4739 0.2144 0.8205 0.028 Uiso 1 1 calc R U . . .
C44 C -0.2749(5) 0.7793(4) 0.9092(2) 0.0541(13) Uani 1 1 d . . . . .
H44A H -0.3458 0.7105 0.8837 0.081 Uiso 1 1 calc R U . . .
H44B H -0.2201 0.7676 0.9500 0.081 Uiso 1 1 calc R U . . .
H44C H -0.2177 0.8010 0.8813 0.081 Uiso 1 1 calc R U . . .
C45 C -0.4599(6) 0.8453(4) 0.9858(3) 0.0716(16) Uani 1 1 d . . . . .
H45A H -0.4948 0.9058 1.0033 0.107 Uiso 1 1 calc R U . . .
H45B H -0.4064 0.8255 1.0235 0.107 Uiso 1 1 calc R U . . .
H45C H -0.5354 0.7807 0.9582 0.107 Uiso 1 1 calc R U . . .
C46 C -0.2242(6) 1.0191(4) 0.9789(3) 0.0719(16) Uani 1 1 d . . . . .
H46A H -0.1602 1.0348 0.9532 0.108 Uiso 1 1 calc R U . . .
H46B H -0.1765 1.0129 1.0231 0.108 Uiso 1 1 calc R U . . .
H46C H -0.2659 1.0794 0.9853 0.108 Uiso 1 1 calc R U . . .
C47 C -0.4387(5) 0.8061(4) 0.7339(2) 0.0553(13) Uani 1 1 d . . . . .
H47A H -0.3768 0.8731 0.7312 0.083 Uiso 1 1 calc R U . . .
H47B H -0.4985 0.7650 0.6887 0.083 Uiso 1 1 calc R U . . .
H47C H -0.3869 0.7595 0.7524 0.083 Uiso 1 1 calc R U . . .
C48 C -0.6622(4) 0.7191(3) 0.7903(2) 0.0470(12) Uani 1 1 d . . . . .
H48A H -0.6134 0.6693 0.8071 0.071 Uiso 1 1 calc R U . . .
H48B H -0.7215 0.6819 0.7444 0.071 Uiso 1 1 calc R U . . .
H48C H -0.7163 0.7387 0.8198 0.071 Uiso 1 1 calc R U . . .
C49 C -0.6308(5) 0.9424(4) 0.7591(3) 0.0637(15) Uani 1 1 d . . . . .
H49A H -0.6769 0.9682 0.7913 0.095 Uiso 1 1 calc R U . . .
H49B H -0.6970 0.9040 0.7150 0.095 Uiso 1 1 calc R U . . .
H49C H -0.5658 1.0061 0.7548 0.095 Uiso 1 1 calc R U . . .
N1 N -0.1277(2) 0.4716(2) 0.73856(12) 0.0086(6) Uani 1 1 d . . . . .
N2 N -0.2088(2) 0.2546(2) 0.63884(12) 0.0104(6) Uani 1 1 d . . . . .
N3 N -0.0215(2) 0.2796(2) 0.78368(13) 0.0135(6) Uani 1 1 d . . . . .
N4 N 0.1336(2) 0.3016(2) 0.68637(12) 0.0106(6) Uani 1 1 d . . . . .
Si1 Si 0.23748(8) 0.23727(8) 0.73082(4) 0.0134(2) Uani 1 1 d . . . . .
Si2 Si -0.35280(13) 0.89067(10) 0.93350(6) 0.0403(3) Uani 1 1 d . . . . .
Si3 Si -0.54087(12) 0.84574(9) 0.78966(6) 0.0344(3) Uani 1 1 d . . . . .
Nb Nb -0.01508(3) 0.34491(2) 0.71895(2) 0.00912(9) Uani 1 1 d . . . . .
O1 O -0.4447(3) 0.9092(2) 0.86562(14) 0.0484(8) Uani 1 1 d . . . . .
H1 H 0.105(3) 0.470(2) 0.7664(14) 0.014(8) Uiso 1 1 d . . . . .
H1A H 0.160(3) 0.150(2) 0.7458(14) 0.009(8) Uiso 1 1 d . . . . .
H1B H 0.308(3) 0.189(2) 0.6891(14) 0.015(8) Uiso 1 1 d . . . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 C1 C2 123.7(3) . . ?
N1 C1 C4 121.9(3) . . ?
C2 C1 C4 114.4(3) . . ?
C3 C2 C1 128.4(3) . . ?
C3 C2 H2 115.8 . . ?
C1 C2 H2 115.8 . . ?
N2 C3 C2 123.7(3) . . ?
N2 C3 C5 120.3(3) . . ?
C2 C3 C5 116.0(3) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 120.5(3) . . ?
C11 C6 N1 119.7(3) . . ?
C7 C6 N1 119.8(3) . . ?
C8 C7 C6 118.3(3) . . ?
C8 C7 C12 118.6(3) . . ?
C6 C7 C12 123.0(3) . . ?
C9 C8 C7 121.7(3) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 121.3(3) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 118.6(3) . . ?
C10 C11 C15 119.0(3) . . ?
C6 C11 C15 122.4(3) . . ?
C7 C12 C13 112.1(3) . . ?
C7 C12 C14 111.0(3) . . ?
C13 C12 C14 109.3(3) . . ?
C7 C12 H12 108.1 . . ?
C13 C12 H12 108.1 . . ?
C14 C12 H12 108.1 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 111.6(3) . . ?
C11 C15 C16 110.9(3) . . ?
C17 C15 C16 111.1(3) . . ?
C11 C15 H15 107.7 . . ?
C17 C15 H15 107.7 . . ?
C16 C15 H15 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 120.5(3) . . ?
C23 C18 N2 121.4(3) . . ?
C19 C18 N2 118.1(3) . . ?
C20 C19 C18 118.5(3) . . ?
C20 C19 C24 118.6(3) . . ?
C18 C19 C24 122.9(3) . . ?
C21 C20 C19 121.8(3) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C20 C21 C22 119.0(3) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
C21 C22 C23 121.9(3) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C18 118.4(3) . . ?
C22 C23 C27 118.3(3) . . ?
C18 C23 C27 123.3(3) . . ?
C19 C24 C25 111.2(3) . . ?
C19 C24 C26 112.2(3) . . ?
C25 C24 C26 109.7(3) . . ?
C19 C24 H24 107.9 . . ?
C25 C24 H24 107.9 . . ?
C26 C24 H24 107.9 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 C29 112.6(3) . . ?
C23 C27 C28 110.5(3) . . ?
C29 C27 C28 108.5(3) . . ?
C23 C27 H27 108.4 . . ?
C29 C27 H27 108.4 . . ?
C28 C27 H27 108.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C31 108.8(3) . . ?
N3 C30 C33 109.3(3) . . ?
C31 C30 C33 110.5(3) . . ?
N3 C30 C32 108.8(3) . . ?
C31 C30 C32 109.3(3) . . ?
C33 C30 C32 110.1(3) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N4 C34 C37 111.2(2) . . ?
N4 C34 C36 109.9(2) . . ?
C37 C34 C36 110.0(2) . . ?
N4 C34 C35 107.5(2) . . ?
C37 C34 C35 109.1(3) . . ?
C36 C34 C35 109.0(3) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 C43 117.1(3) . . ?
C39 C38 Si1 124.1(2) . . ?
C43 C38 Si1 118.8(3) . . ?
C40 C39 C38 121.4(3) . . ?
C40 C39 H39 119.3 . . ?
C38 C39 H39 119.3 . . ?
C41 C40 C39 120.1(3) . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 C42 120.0(3) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 120.1(3) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C42 C43 C38 121.3(3) . . ?
C42 C43 H43 119.3 . . ?
C38 C43 H43 119.3 . . ?
Si2 C44 H44A 109.5 . . ?
Si2 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
Si2 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Si2 C45 H45A 109.5 . . ?
Si2 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
Si2 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Si2 C46 H46A 109.5 . . ?
Si2 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
Si2 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
Si3 C47 H47A 109.5 . . ?
Si3 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
Si3 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
Si3 C48 H48A 109.5 . . ?
Si3 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
Si3 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Si3 C49 H49A 109.5 . . ?
Si3 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
Si3 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C1 N1 C6 116.2(2) . . ?
C1 N1 Nb 118.5(2) . . ?
C6 N1 Nb 123.88(17) . . ?
C3 N2 C18 117.1(2) . . ?
C3 N2 Nb 117.1(2) . . ?
C18 N2 Nb 125.07(17) . . ?
C30 N3 Nb 173.5(2) . . ?
C34 N4 Si1 120.09(19) . . ?
C34 N4 Nb 116.36(18) . . ?
Si1 N4 Nb 121.34(13) . . ?
N4 Si1 C38 116.21(14) . . ?
N4 Si1 H1A 109.6(11) . . ?
C38 Si1 H1A 109.5(11) . . ?
N4 Si1 H1B 110.1(11) . . ?
C38 Si1 H1B 105.7(12) . . ?
H1A Si1 H1B 105.1(16) . . ?
O1 Si2 C46 108.4(2) . . ?
O1 Si2 C45 109.9(2) . . ?
C46 Si2 C45 111.2(3) . . ?
O1 Si2 C44 109.27(19) . . ?
C46 Si2 C44 110.3(3) . . ?
C45 Si2 C44 107.7(2) . . ?
O1 Si3 C48 109.78(19) . . ?
O1 Si3 C49 107.3(2) . . ?
C48 Si3 C49 110.3(2) . . ?
O1 Si3 C47 110.4(2) . . ?
C48 Si3 C47 108.6(2) . . ?
C49 Si3 C47 110.4(2) . . ?
N3 Nb N4 102.81(11) . . ?
N3 Nb N2 103.99(11) . . ?
N4 Nb N2 107.50(9) . . ?
N3 Nb N1 103.08(10) . . ?
N4 Nb N1 149.17(9) . . ?
N2 Nb N1 82.03(9) . . ?
N3 Nb H1 98.6(9) . . ?
N4 Nb H1 87.0(9) . . ?
N2 Nb H1 149.3(9) . . ?
N1 Nb H1 72.8(9) . . ?
Si3 O1 Si2 143.37(19) . . ?
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
C1 N1 1.328(4) . ?
C1 C2 1.413(4) . ?
C1 C4 1.512(4) . ?
C2 C3 1.388(4) . ?
C2 H2 0.9500 . ?
C3 N2 1.351(4) . ?
C3 C5 1.514(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.401(4) . ?
C6 C7 1.407(4) . ?
C6 N1 1.461(4) . ?
C7 C8 1.386(5) . ?
C7 C12 1.510(4) . ?
C8 C9 1.379(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.376(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.394(5) . ?
C10 H10 0.9500 . ?
C11 C15 1.519(4) . ?
C12 C13 1.531(4) . ?
C12 C14 1.535(4) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.524(4) . ?
C15 C16 1.532(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C23 1.405(4) . ?
C18 C19 1.408(4) . ?
C18 N2 1.450(4) . ?
C19 C20 1.394(4) . ?
C19 C24 1.520(4) . ?
C20 C21 1.374(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.386(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.391(4) . ?
C22 H22 0.9500 . ?
C23 C27 1.514(4) . ?
C24 C25 1.531(4) . ?
C24 C26 1.532(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.530(4) . ?
C27 C28 1.538(4) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N3 1.468(4) . ?
C30 C31 1.527(5) . ?
C30 C33 1.529(5) . ?
C30 C32 1.535(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 N4 1.500(4) . ?
C34 C37 1.528(4) . ?
C34 C36 1.532(4) . ?
C34 C35 1.534(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.395(5) . ?
C38 C43 1.404(4) . ?
C38 Si1 1.873(3) . ?
C39 C40 1.384(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.374(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.379(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.378(5) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 Si2 1.858(4) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 Si2 1.850(5) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 Si2 1.803(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 Si3 1.861(4) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 Si3 1.840(4) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 Si3 1.857(5) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
N1 Nb 2.263(2) . ?
N2 Nb 2.228(2) . ?
N3 Nb 1.750(3) . ?
N4 Si1 1.740(3) . ?
N4 Nb 2.017(2) . ?
Si1 H1A 1.38(3) . ?
Si1 H1B 1.43(3) . ?
Si2 O1 1.630(3) . ?
Si3 O1 1.619(3) . ?
Nb H1 1.74(3) . ?
