#------------------------------------------------------------------------------
#$Date: 2020-10-10 04:31:56 +0300 (Sat, 10 Oct 2020) $
#$Revision: 258285 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/93/1559326.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_1559326
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         'C54 H79 N4 Nb O2 Si'
_chemical_formula_sum            'C54 H79 N4 Nb O2 Si'
_chemical_formula_weight         937.21
_chemical_melting_point          478
_chemical_name_common            (BDI)Nb(OCHNtBu)(O[SiMe2Ph])(NAr)
_chemical_name_systematic
(2,6-diisopropylphenyl)imino-(tert-butyliminomethoxy)-dimethylphenylsilanolato-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-14
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-14 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.431(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.629(2)
_cell_length_b                   21.336(4)
_cell_length_c                   19.715(4)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.17
_cell_volume                     5307.5(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59328
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.389
_diffrn_reflns_theta_min         1.407
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6620
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0556 before and 0.0471 after correction.
The Ratio of minimum to maximum transmission is 0.8884.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0422P)²+7.8592P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8048
_reflns_number_total             9689
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03489d2.cif
_cod_data_source_block           bmkxr71
_cod_original_cell_volume        5307.4(18)
_cod_database_code               1559326
_shelx_shelxl_version_number     2018/3
_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_max   0.977
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C36(H36), C39(H39)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C33(H33), C34(H34), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C50(H50)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.6534(2) 0.68754(13) 0.26279(14) 0.0195(6) Uani 1 1 d . . . . .
C2 C 0.7180(2) 0.73107(13) 0.23221(14) 0.0204(6) Uani 1 1 d . . . . .
H2 H 0.738994 0.720922 0.187831 0.024 Uiso 1 1 calc R . . . .
C3 C 0.7557(2) 0.78780(13) 0.25874(14) 0.0188(6) Uani 1 1 d . . . . .
C4 C 0.6051(3) 0.63756(14) 0.21710(15) 0.0289(7) Uani 1 1 d . . . . .
H4A H 0.633934 0.596553 0.230573 0.043 Uiso 1 1 calc GR . . . .
H4B H 0.621993 0.646286 0.169967 0.043 Uiso 1 1 calc GR . . . .
H4C H 0.528011 0.637352 0.221060 0.043 Uiso 1 1 calc GR . . . .
C5 C 0.7987(3) 0.83330(14) 0.20776(14) 0.0274(7) Uani 1 1 d . . . . .
H5A H 0.767034 0.874715 0.214129 0.041 Uiso 1 1 calc GR . . . .
H5B H 0.780968 0.818391 0.161649 0.041 Uiso 1 1 calc GR . . . .
H5C H 0.875846 0.836249 0.214513 0.041 Uiso 1 1 calc GR . . . .
C6 C 0.5440(2) 0.64899(13) 0.34852(13) 0.0203(6) Uani 1 1 d . . . . .
C7 C 0.5653(2) 0.58773(13) 0.37090(14) 0.0224(6) Uani 1 1 d . . . . .
C8 C 0.4794(3) 0.55118(14) 0.38981(15) 0.0292(7) Uani 1 1 d . . . . .
H8 H 0.491603 0.509496 0.405147 0.035 Uiso 1 1 calc R . . . .
C9 C 0.3770(3) 0.57441(16) 0.38666(18) 0.0371(8) Uani 1 1 d . . . . .
H9 H 0.320074 0.548819 0.400175 0.044 Uiso 1 1 calc R . . . .
C10 C 0.3574(3) 0.63459(15) 0.36395(17) 0.0319(7) Uani 1 1 d . . . . .
H10 H 0.286876 0.650209 0.361960 0.038 Uiso 1 1 calc R . . . .
C11 C 0.4402(2) 0.67279(14) 0.34387(14) 0.0232(6) Uani 1 1 d . . . . .
C12 C 0.6766(2) 0.55987(13) 0.37522(14) 0.0235(6) Uani 1 1 d . . . . .
H12 H 0.725768 0.590680 0.354902 0.028 Uiso 1 1 calc R . . . .
C13 C 0.6833(3) 0.49839(14) 0.33535(17) 0.0350(8) Uani 1 1 d . . . . .
H13A H 0.638547 0.466679 0.355904 0.053 Uiso 1 1 calc GR . . . .
H13B H 0.756886 0.483772 0.336514 0.053 Uiso 1 1 calc GR . . . .
H13C H 0.658659 0.505434 0.288155 0.053 Uiso 1 1 calc GR . . . .
C14 C 0.7145(3) 0.54874(15) 0.44910(15) 0.0297(7) Uani 1 1 d . . . . .
H14A H 0.710569 0.588076 0.474538 0.044 Uiso 1 1 calc GR . . . .
H14B H 0.787878 0.533763 0.450444 0.044 Uiso 1 1 calc GR . . . .
H14C H 0.669177 0.517267 0.469566 0.044 Uiso 1 1 calc GR . . . .
C15 C 0.4148(2) 0.73779(14) 0.31523(15) 0.0241(6) Uani 1 1 d . . . . .
H15 H 0.482773 0.757926 0.302778 0.029 Uiso 1 1 calc R . . . .
C16 C 0.3422(3) 0.73379(18) 0.25123(17) 0.0441(9) Uani 1 1 d . . . . .
H16A H 0.275596 0.713334 0.262158 0.066 Uiso 1 1 calc GR . . . .
H16B H 0.377218 0.709361 0.216536 0.066 Uiso 1 1 calc GR . . . .
H16C H 0.327402 0.776111 0.234002 0.066 Uiso 1 1 calc GR . . . .
C17 C 0.3620(3) 0.78002(17) 0.36581(17) 0.0394(8) Uani 1 1 d . . . . .
H17A H 0.295402 0.760875 0.379073 0.059 Uiso 1 1 calc GR . . . .
H17B H 0.347183 0.820938 0.344905 0.059 Uiso 1 1 calc GR . . . .
H17C H 0.409226 0.785493 0.406097 0.059 Uiso 1 1 calc GR . . . .
C18 C 0.7859(2) 0.86660(12) 0.34211(13) 0.0180(6) Uani 1 1 d . . . . .
C19 C 0.7063(2) 0.91118(13) 0.35250(13) 0.0195(6) Uani 1 1 d . . . . .
C20 C 0.7387(2) 0.97212(13) 0.36881(14) 0.0246(7) Uani 1 1 d . . . . .
H20 H 0.686822 1.003694 0.374536 0.030 Uiso 1 1 calc R . . . .
C21 C 0.8456(2) 0.98749(14) 0.37684(15) 0.0264(7) Uani 1 1 d . . . . .
H21 H 0.866025 1.029191 0.388072 0.032 Uiso 1 1 calc R . . . .
C22 C 0.9212(3) 0.94261(14) 0.36856(15) 0.0272(7) Uani 1 1 d . . . . .
H22 H 0.993799 0.953477 0.375228 0.033 Uiso 1 1 calc R . . . .
C23 C 0.8942(2) 0.88111(13) 0.35053(14) 0.0217(6) Uani 1 1 d . . . . .
C24 C 0.5887(2) 0.89443(14) 0.34678(15) 0.0239(6) Uani 1 1 d . . . . .
H24 H 0.582157 0.849802 0.361514 0.029 Uiso 1 1 calc R . . . .
C25 C 0.5221(3) 0.93379(16) 0.39363(18) 0.0355(8) Uani 1 1 d . . . . .
H25A H 0.554599 0.933187 0.439664 0.053 Uiso 1 1 calc GR . . . .
H25B H 0.450349 0.916387 0.394320 0.053 Uiso 1 1 calc GR . . . .
H25C H 0.518652 0.977051 0.376991 0.053 Uiso 1 1 calc GR . . . .
C26 C 0.5449(3) 0.89817(16) 0.27354(17) 0.0365(8) Uani 1 1 d . . . . .
H26A H 0.469098 0.888130 0.271939 0.055 Uiso 1 1 calc GR . . . .
H26B H 0.582370 0.868143 0.245589 0.055 Uiso 1 1 calc GR . . . .
H26C H 0.555057 0.940652 0.256060 0.055 Uiso 1 1 calc GR . . . .
C27 C 0.9820(2) 0.83367(14) 0.34165(16) 0.0269(7) Uani 1 1 d . . . . .
H27 H 0.949541 0.795588 0.319754 0.032 Uiso 1 1 calc R . . . .
C28 C 1.0685(3) 0.85802(16) 0.29500(18) 0.0359(8) Uani 1 1 d . . . . .
H28A H 1.035182 0.873201 0.252311 0.054 Uiso 1 1 calc GR . . . .
H28B H 1.117651 0.823896 0.285476 0.054 Uiso 1 1 calc GR . . . .
H28C H 1.107453 0.892373 0.317674 0.054 Uiso 1 1 calc GR . . . .
C29 C 1.0322(2) 0.81375(16) 0.41041(17) 0.0331(8) Uani 1 1 d . . . . .
H29A H 1.068754 0.849632 0.431783 0.050 Uiso 1 1 calc GR . . . .
H29B H 1.083170 0.779930 0.403649 0.050 Uiso 1 1 calc GR . . . .
H29C H 0.976712 0.798947 0.439789 0.050 Uiso 1 1 calc GR . . . .
C30 C 0.9241(2) 0.65104(14) 0.42364(15) 0.0244(7) Uani 1 1 d . . . . .
C31 C 0.9742(2) 0.62653(14) 0.36679(16) 0.0278(7) Uani 1 1 d . . . . .
C32 C 1.0581(3) 0.58452(18) 0.37821(19) 0.0467(10) Uani 1 1 d . . . . .
H32 H 1.092952 0.567788 0.340492 0.056 Uiso 1 1 calc R . . . .
C33 C 1.0910(3) 0.5669(2) 0.4424(2) 0.0635(13) Uani 1 1 d . . . . .
H33 H 1.147481 0.537839 0.448753 0.076 Uiso 1 1 calc R . . . .
C34 C 1.0424(3) 0.5913(2) 0.4978(2) 0.0590(13) Uani 1 1 d . . . . .
H34 H 1.066483 0.578973 0.542135 0.071 Uiso 1 1 calc R . . . .
C35 C 0.9589(3) 0.63366(17) 0.49026(17) 0.0358(8) Uani 1 1 d . . . . .
C36 C 0.9420(2) 0.64567(14) 0.29479(15) 0.0266(7) Uani 1 1 d . . . . .
H36 H 0.881165 0.675467 0.297099 0.032 Uiso 1 1 calc R . . . .
C37 C 0.9061(3) 0.59065(17) 0.24996(18) 0.0445(9) Uani 1 1 d . . . . .
H37A H 0.965812 0.562099 0.244212 0.067 Uiso 1 1 calc GR . . . .
H37B H 0.880682 0.606352 0.205468 0.067 Uiso 1 1 calc GR . . . .
H37C H 0.848648 0.568199 0.271411 0.067 Uiso 1 1 calc GR . . . .
C38 C 1.0322(3) 0.67986(15) 0.26122(17) 0.0364(8) Uani 1 1 d . . . . .
H38A H 1.056409 0.714893 0.290038 0.055 Uiso 1 1 calc GR . . . .
H38B H 1.006918 0.695887 0.216840 0.055 Uiso 1 1 calc GR . . . .
H38C H 1.091078 0.650756 0.255219 0.055 Uiso 1 1 calc GR . . . .
C39 C 0.9083(3) 0.66060(18) 0.55232(16) 0.0373(8) Uani 1 1 d . . . . .
H39 H 0.839127 0.679635 0.536788 0.045 Uiso 1 1 calc R . . . .
C40 C 0.8848(3) 0.61073(18) 0.60515(17) 0.0417(9) Uani 1 1 d . . . . .
H40A H 0.839661 0.578123 0.584166 0.063 Uiso 1 1 calc GR . . . .
H40B H 0.848287 0.630062 0.642702 0.063 Uiso 1 1 calc GR . . . .
H40C H 0.951466 0.591982 0.622477 0.063 Uiso 1 1 calc GR . . . .
C41 C 0.9762(3) 0.7126(2) 0.5839(2) 0.0586(11) Uani 1 1 d . . . . .
H41A H 1.045011 0.695452 0.599388 0.088 Uiso 1 1 calc GR . . . .
H41B H 0.940465 0.730431 0.622613 0.088 Uiso 1 1 calc GR . . . .
H41C H 0.986750 0.745362 0.550041 0.088 Uiso 1 1 calc GR . . . .
C42 C 0.4456(2) 0.75861(15) 0.54177(14) 0.0246(6) Uani 1 1 d . . . . .
C43 C 0.4634(3) 0.82416(15) 0.54578(15) 0.0327(8) Uani 1 1 d . . . . .
H43 H 0.533846 0.839711 0.549732 0.039 Uiso 1 1 calc R . . . .
C44 C 0.3788(3) 0.86591(19) 0.54400(17) 0.0455(10) Uani 1 1 d . . . . .
H44 H 0.392127 0.909705 0.546094 0.055 Uiso 1 1 calc R . . . .
C45 C 0.2764(3) 0.8446(2) 0.53925(18) 0.0525(11) Uani 1 1 d . . . . .
H45 H 0.219282 0.873599 0.538290 0.063 Uiso 1 1 calc R . . . .
C46 C 0.2560(3) 0.7817(2) 0.53588(17) 0.0519(12) Uani 1 1 d . . . . .
H46 H 0.184927 0.767117 0.532999 0.062 Uiso 1 1 calc R . . . .
C47 C 0.3407(3) 0.73846(18) 0.53669(15) 0.0363(8) Uani 1 1 d . . . . .
H47 H 0.325864 0.694880 0.533707 0.044 Uiso 1 1 calc R . . . .
C48 C 0.5170(3) 0.62399(15) 0.56214(18) 0.0402(9) Uani 1 1 d . . . . .
H48A H 0.470531 0.609267 0.524368 0.060 Uiso 1 1 calc GR . . . .
H48B H 0.477914 0.623910 0.604041 0.060 Uiso 1 1 calc GR . . . .
H48C H 0.578477 0.596136 0.567484 0.060 Uiso 1 1 calc GR . . . .
C49 C 0.6560(3) 0.73128(16) 0.61402(15) 0.0308(7) Uani 1 1 d . . . . .
H49A H 0.718680 0.704196 0.615920 0.046 Uiso 1 1 calc GR . . . .
H49B H 0.620935 0.729163 0.657377 0.046 Uiso 1 1 calc GR . . . .
H49C H 0.677444 0.774593 0.605396 0.046 Uiso 1 1 calc GR . . . .
C50 C 0.7844(2) 0.85459(13) 0.50874(14) 0.0231(6) Uani 1 1 d . . . . .
H50 H 0.859196 0.857759 0.515199 0.028 Uiso 1 1 calc R . . . .
C51 C 0.7744(2) 0.93526(13) 0.59042(15) 0.0250(6) Uani 1 1 d . . . . .
C52 C 0.8919(3) 0.92505(16) 0.60858(19) 0.0409(9) Uani 1 1 d . . . . .
H52A H 0.903306 0.881544 0.623057 0.061 Uiso 1 1 calc GR . . . .
H52B H 0.914269 0.953392 0.645576 0.061 Uiso 1 1 calc GR . . . .
H52C H 0.933428 0.933643 0.568753 0.061 Uiso 1 1 calc GR . . . .
C53 C 0.7102(3) 0.92804(17) 0.65428(17) 0.0454(10) Uani 1 1 d . . . . .
H53A H 0.634814 0.934220 0.642440 0.068 Uiso 1 1 calc GR . . . .
H53B H 0.733749 0.959353 0.688027 0.068 Uiso 1 1 calc GR . . . .
H53C H 0.721150 0.885934 0.673166 0.068 Uiso 1 1 calc GR . . . .
C54 C 0.7576(3) 1.00046(14) 0.56069(17) 0.0361(8) Uani 1 1 d . . . . .
H54A H 0.799889 1.005164 0.520455 0.054 Uiso 1 1 calc GR . . . .
H54B H 0.779631 1.031963 0.594604 0.054 Uiso 1 1 calc GR . . . .
H54C H 0.682419 1.006272 0.547854 0.054 Uiso 1 1 calc GR . . . .
N1 N 0.63063(17) 0.68902(10) 0.32874(11) 0.0163(5) Uani 1 1 d . . . . .
N2 N 0.75280(18) 0.80316(10) 0.32429(11) 0.0163(5) Uani 1 1 d . . . . .
N3 N 0.83775(18) 0.69208(10) 0.41376(11) 0.0189(5) Uani 1 1 d . . . . .
N4 N 0.72737(19) 0.89018(11) 0.54096(12) 0.0255(6) Uani 1 1 d . . . . .
O1 O 0.62280(15) 0.70575(9) 0.47208(9) 0.0204(4) Uani 1 1 d . . . . .
O2 O 0.74438(17) 0.81215(9) 0.46549(10) 0.0268(5) Uani 1 1 d . . . . .
Si Si 0.56232(6) 0.70444(4) 0.54429(4) 0.02088(18) Uani 1 1 d . . . . .
Nb Nb 0.72142(2) 0.73856(2) 0.40928(2) 0.01535(8) Uani 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'
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'
Si Si 0.0817 0.0704 '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
C2 C1 C4 116.3(2) . . ?
N1 C1 C2 123.9(3) . . ?
N1 C1 C4 119.8(2) . . ?
C1 C2 H2 116.0 . . ?
C1 C2 C3 127.9(3) . . ?
C3 C2 H2 116.0 . . ?
C2 C3 C5 115.7(2) . . ?
N2 C3 C2 123.6(2) . . ?
N2 C3 C5 120.7(2) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 121.5(3) . . ?
C7 C6 N1 119.7(3) . . ?
C11 C6 N1 118.7(2) . . ?
C6 C7 C12 123.0(2) . . ?
C8 C7 C6 117.6(3) . . ?
C8 C7 C12 119.4(3) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.5(3) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.2(3) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.6(3) . . ?
C11 C10 H10 119.7 . . ?
C6 C11 C15 122.2(2) . . ?
C10 C11 C6 118.6(3) . . ?
C10 C11 C15 119.1(3) . . ?
C7 C12 H12 108.0 . . ?
C7 C12 C13 112.1(3) . . ?
C7 C12 C14 111.3(2) . . ?
C13 C12 H12 108.0 . . ?
C14 C12 H12 108.0 . . ?
C14 C12 C13 109.4(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15 108.2 . . ?
C11 C15 C16 111.3(3) . . ?
C16 C15 H15 108.2 . . ?
C17 C15 C11 112.8(2) . . ?
C17 C15 H15 108.2 . . ?
C17 C15 C16 108.1(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 122.2(3) . . ?
C19 C18 N2 117.7(2) . . ?
C23 C18 N2 120.1(2) . . ?
C18 C19 C24 122.0(2) . . ?
C20 C19 C18 117.3(3) . . ?
C20 C19 C24 120.7(3) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.3(3) . . ?
C21 C20 H20 119.4 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.0(3) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 119.2 . . ?
C21 C22 C23 121.6(3) . . ?
C23 C22 H22 119.2 . . ?
C18 C23 C27 123.5(2) . . ?
C22 C23 C18 117.5(3) . . ?
C22 C23 C27 118.9(3) . . ?
C19 C24 H24 107.1 . . ?
C19 C24 C25 112.7(2) . . ?
C25 C24 H24 107.1 . . ?
C26 C24 C19 111.7(2) . . ?
C26 C24 H24 107.1 . . ?
C26 C24 C25 110.9(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27 107.7 . . ?
C23 C27 C28 112.5(3) . . ?
C23 C27 C29 111.1(2) . . ?
C28 C27 H27 107.7 . . ?
C29 C27 H27 107.7 . . ?
C29 C27 C28 110.1(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C35 120.5(3) . . ?
N3 C30 C31 119.5(3) . . ?
N3 C30 C35 120.0(3) . . ?
C30 C31 C36 122.2(3) . . ?
C32 C31 C30 118.2(3) . . ?
C32 C31 C36 119.6(3) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.6(3) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 H33 119.9 . . ?
C32 C33 C34 120.1(3) . . ?
C34 C33 H33 119.9 . . ?
C33 C34 H34 119.3 . . ?
C33 C34 C35 121.4(3) . . ?
C35 C34 H34 119.3 . . ?
C30 C35 C39 121.6(3) . . ?
C34 C35 C30 118.2(3) . . ?
C34 C35 C39 120.2(3) . . ?
C31 C36 H36 107.7 . . ?
C31 C36 C37 113.3(3) . . ?
C31 C36 C38 111.1(3) . . ?
C37 C36 H36 107.7 . . ?
C38 C36 H36 107.7 . . ?
C38 C36 C37 109.0(3) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C39 H39 107.4 . . ?
C35 C39 C40 112.8(3) . . ?
C35 C39 C41 111.0(3) . . ?
C40 C39 H39 107.4 . . ?
C41 C39 H39 107.4 . . ?
C41 C39 C40 110.6(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 Si 119.0(2) . . ?
C47 C42 C43 117.1(3) . . ?
C47 C42 Si 123.8(3) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 C42 120.7(3) . . ?
C44 C43 H43 119.6 . . ?
C43 C44 H44 119.6 . . ?
C45 C44 C43 120.7(4) . . ?
C45 C44 H44 119.6 . . ?
C44 C45 H45 119.9 . . ?
C46 C45 C44 120.3(4) . . ?
C46 C45 H45 119.9 . . ?
C45 C46 H46 120.0 . . ?
C45 C46 C47 120.0(4) . . ?
C47 C46 H46 120.0 . . ?
C42 C47 C46 121.1(4) . . ?
C42 C47 H47 119.4 . . ?
C46 C47 H47 119.4 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Si C48 H48A 109.5 . . ?
Si C48 H48B 109.5 . . ?
Si C48 H48C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
Si C49 H49A 109.5 . . ?
Si C49 H49B 109.5 . . ?
Si C49 H49C 109.5 . . ?
N4 C50 H50 118.9 . . ?
N4 C50 O2 122.2(3) . . ?
O2 C50 H50 118.9 . . ?
C52 C51 C53 109.6(3) . . ?
C54 C51 C52 109.9(3) . . ?
C54 C51 C53 109.8(3) . . ?
N4 C51 C52 115.0(3) . . ?
N4 C51 C53 105.3(2) . . ?
N4 C51 C54 107.2(2) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C1 N1 C6 116.1(2) . . ?
C1 N1 Nb 125.87(18) . . ?
C6 N1 Nb 117.75(16) . . ?
C3 N2 C18 116.3(2) . . ?
C3 N2 Nb 126.27(18) . . ?
C18 N2 Nb 117.02(16) . . ?
C30 N3 Nb 172.9(2) . . ?
C50 N4 C51 120.7(3) . . ?
Si O1 Nb 154.18(12) . . ?
C50 O2 Nb 164.4(2) . . ?
C48 Si C42 109.19(16) . . ?
C48 Si C49 109.68(16) . . ?
C49 Si C42 107.68(14) . . ?
O1 Si C42 111.14(11) . . ?
O1 Si C48 109.86(13) . . ?
O1 Si C49 109.25(13) . . ?
N1 Nb N2 81.79(8) . . ?
N3 Nb N1 99.99(9) . . ?
N3 Nb N2 102.19(9) . . ?
N3 Nb O1 108.80(9) . . ?
N3 Nb O2 108.76(10) . . ?
O1 Nb N1 87.57(8) . . ?
O1 Nb N2 148.55(8) . . ?
O1 Nb O2 90.69(8) . . ?
O2 Nb N1 150.12(9) . . ?
O2 Nb N2 84.33(8) . . ?
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 C2 1.391(4) . ?
C1 C4 1.508(4) . ?
C1 N1 1.344(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.394(4) . ?
C3 C5 1.514(4) . ?
C3 N2 1.335(3) . ?
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 C7 1.402(4) . ?
C6 C11 1.405(4) . ?
C6 N1 1.454(3) . ?
C7 C8 1.400(4) . ?
C7 C12 1.525(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.379(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.396(4) . ?
C11 C15 1.526(4) . ?
C12 H12 1.0000 . ?
C12 C13 1.533(4) . ?
C12 C14 1.532(4) . ?
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 H15 1.0000 . ?
C15 C16 1.530(4) . ?
C15 C17 1.519(4) . ?
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 C19 1.405(4) . ?
C18 C23 1.405(4) . ?
C18 N2 1.455(3) . ?
C19 C20 1.397(4) . ?
C19 C24 1.527(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.391(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.366(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.398(4) . ?
C23 C27 1.517(4) . ?
C24 H24 1.0000 . ?
C24 C25 1.527(4) . ?
C24 C26 1.526(4) . ?
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 H27 1.0000 . ?
C27 C28 1.547(4) . ?
C27 C29 1.532(4) . ?
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 C31 1.411(4) . ?
C30 C35 1.417(4) . ?
C30 N3 1.405(4) . ?
C31 C32 1.398(4) . ?
C31 C36 1.516(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.367(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.378(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.392(5) . ?
C35 C39 1.517(5) . ?
C36 H36 1.0000 . ?
C36 C37 1.527(4) . ?
C36 C38 1.527(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39 1.0000 . ?
C39 C40 1.527(5) . ?
C39 C41 1.518(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.418(4) . ?
C42 C47 1.392(4) . ?
C42 Si 1.872(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.390(5) . ?
C44 H44 0.9500 . ?
C44 C45 1.371(6) . ?
C45 H45 0.9500 . ?
C45 C46 1.367(6) . ?
C46 H46 0.9500 . ?
C46 C47 1.412(5) . ?
C47 H47 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 Si 1.848(3) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C49 Si 1.865(3) . ?
C50 H50 0.9500 . ?
C50 N4 1.240(4) . ?
C50 O2 1.329(3) . ?
C51 C52 1.526(4) . ?
C51 C53 1.534(4) . ?
C51 C54 1.521(4) . ?
C51 N4 1.476(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
N1 Nb 2.191(2) . ?
N2 Nb 2.218(2) . ?
N3 Nb 1.772(2) . ?
O1 Si 1.6441(19) . ?
O1 Nb 1.9247(18) . ?
O2 Nb 1.9366(19) . ?
