#------------------------------------------------------------------------------
#$Date: 2020-10-10 04:31:56 +0300 (Sat, 10 Oct 2020) $
#$Revision: 258285 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/93/1559322.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_1559322
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 H72 B N4 Nb O2'
_chemical_formula_sum            'C43 H72 B N4 Nb O2'
_chemical_formula_weight         780.76
_chemical_melting_point          415
_chemical_name_common            (BDI)NbH(N[BO2C6H12]tBu)(NtBu)
_chemical_name_systematic
hydrido-(N-(tert-butyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-amino)-(tert-butyl)imino-(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      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
_audit_creation_date             2020-05-16
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-17 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.045(6)
_cell_angle_beta                 101.926(5)
_cell_angle_gamma                113.572(6)
_cell_formula_units_Z            2
_cell_length_a                   9.897(2)
_cell_length_b                   11.357(2)
_cell_length_c                   21.303(4)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.23
_cell_volume                     2138.0(7)
_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 0.968
_diffrn_measured_fraction_theta_max 0.964
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18471
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.379
_diffrn_reflns_theta_min         0.981
_exptl_absorpt_coefficient_mu    0.320
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       needle
_exptl_crystal_F_000             840
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexamethyldisiloxane'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.798
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         7562
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1348P)²+10.6428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6937
_reflns_number_total             7562
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03489d2.cif
_cod_data_source_block           bmkxr49
_cod_original_cell_volume        2138.1(8)
_cod_database_code               1559322
_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   0.984
_shelx_estimated_absorpt_t_min   0.975
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.706(2)
 0.294(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(C36) = Uanis(C34)
4.a Ternary CH refined with riding coordinates:
 C24(H24), C15(H15), C27(H27), C12(H12)
4.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C10(H10), C2(H2), C8(H8), C9(H9), C20(H20)
4.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C29(H29A,H29B,
 H29C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C14(H14A,H14B,H14C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C42(H42A,H42B,H42C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C13(H13A,H13B,
 H13C), C40(H40A,H40B,H40C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
Nb Nb 0.07584(8) 0.25224(7) 0.27075(3) 0.01419(19) Uani 1 1 d . . . . .
C1 C 0.2604(8) 0.0852(7) 0.2647(4) 0.0170(15) Uani 1 1 d . . . . .
O1 O 0.2239(6) 0.2905(5) 0.1600(3) 0.0202(12) Uani 1 1 d . . . . .
C34 C 0.0816(11) 0.5222(8) 0.2206(4) 0.0275(13) Uani 1 1 d . . . . .
N4 N 0.1129(7) 0.4050(6) 0.2139(3) 0.0173(13) Uani 1 1 d . . . . .
O2 O 0.3062(7) 0.5064(6) 0.1480(3) 0.0309(14) Uani 1 1 d . . . . .
C36 C 0.1933(10) 0.6236(7) 0.2693(4) 0.0275(13) Uani 1 1 d . U . . .
H36A H 0.206733 0.587150 0.310666 0.041 Uiso 1 1 calc GR . . . .
H36B H 0.158141 0.691784 0.273857 0.041 Uiso 1 1 calc GR . . . .
H36C H 0.290045 0.659773 0.256172 0.041 Uiso 1 1 calc GR . . . .
N2 N -0.0481(7) 0.0703(6) 0.1999(3) 0.0165(13) Uani 1 1 d . . . . .
C3 C 0.0149(9) -0.0013(8) 0.1804(4) 0.0188(16) Uani 1 1 d . . . . .
C25 C -0.3420(9) -0.0969(8) 0.3221(4) 0.0237(17) Uani 1 1 d . . . . .
H25A H -0.337961 -0.009547 0.326461 0.036 Uiso 1 1 calc GR . . . .
H25B H -0.298261 -0.117809 0.363910 0.036 Uiso 1 1 calc GR . . . .
H25C H -0.447577 -0.158809 0.307462 0.036 Uiso 1 1 calc GR . . . .
C24 C -0.2517(8) -0.1039(7) 0.2727(4) 0.0187(14) Uani 1 1 d . . . . .
H24 H -0.143913 -0.041950 0.289155 0.022 Uiso 1 1 calc R . . . .
N1 N 0.2277(7) 0.1589(6) 0.3027(3) 0.0153(13) Uani 1 1 d . . . . .
C18 C -0.2110(9) 0.0244(7) 0.1754(3) 0.0163(15) Uani 1 1 d . . . . .
C33 C -0.1099(9) 0.2539(8) 0.4088(4) 0.0221(17) Uani 1 1 d . . . . .
H33A H -0.176575 0.270788 0.372537 0.033 Uiso 1 1 calc GR . . . .
H33B H -0.135011 0.270209 0.449202 0.033 Uiso 1 1 calc GR . . . .
H33C H -0.123754 0.163725 0.403796 0.033 Uiso 1 1 calc GR . . . .
C15 C 0.1411(10) -0.0485(8) 0.3875(4) 0.0246(18) Uani 1 1 d . . . . .
H15 H 0.099382 -0.050504 0.340334 0.030 Uiso 1 1 calc R . . . .
C29 C -0.2299(12) 0.2660(10) 0.0586(5) 0.035(2) Uani 1 1 d . . . . .
H29A H -0.324856 0.223809 0.026197 0.053 Uiso 1 1 calc GR . . . .
H29B H -0.156170 0.333607 0.039627 0.053 Uiso 1 1 calc GR . . . .
H29C H -0.248633 0.304394 0.095310 0.053 Uiso 1 1 calc GR . . . .
C22 C -0.4249(9) 0.0129(9) 0.0938(4) 0.0264(19) Uani 1 1 d . . . . .
H22 H -0.465076 0.041671 0.055388 0.032 Uiso 1 1 calc R . . . .
C21 C -0.5230(10) -0.0809(9) 0.1234(4) 0.0272(18) Uani 1 1 d . . . . .
H21 H -0.628491 -0.119191 0.104741 0.033 Uiso 1 1 calc R . . . .
N3 N 0.0889(7) 0.3191(6) 0.3486(3) 0.0169(13) Uani 1 1 d . . . . .
C41 C 0.3029(11) 0.2124(10) 0.0750(5) 0.033(2) Uani 1 1 d . . . . .
H41A H 0.294352 0.133800 0.095967 0.050 Uiso 1 1 calc GR . . . .
H41B H 0.381004 0.234083 0.049962 0.050 Uiso 1 1 calc GR . . . .
H41C H 0.205656 0.198229 0.046181 0.050 Uiso 1 1 calc GR . . . .
C43 C 0.5088(12) 0.5464(12) 0.0935(5) 0.047(3) Uani 1 1 d . . . . .
H43A H 0.504898 0.629145 0.082920 0.071 Uiso 1 1 calc GR . . . .
H43B H 0.539850 0.512638 0.059285 0.071 Uiso 1 1 calc GR . . . .
H43C H 0.581864 0.558972 0.134432 0.071 Uiso 1 1 calc GR . . . .
C11 C 0.2743(9) 0.0794(8) 0.4097(4) 0.0210(17) Uani 1 1 d . . . . .
C14 C 0.4863(10) 0.5334(8) 0.3776(4) 0.0251(18) Uani 1 1 d . . . . .
H14A H 0.563034 0.566027 0.418069 0.038 Uiso 1 1 calc GR . . . .
H14B H 0.385943 0.512735 0.385997 0.038 Uiso 1 1 calc GR . . . .
H14C H 0.507024 0.599276 0.347041 0.038 Uiso 1 1 calc GR . . . .
C31 C 0.0785(10) 0.4843(8) 0.4182(4) 0.0239(18) Uani 1 1 d . . . . .
H31A H 0.177920 0.540222 0.410753 0.036 Uiso 1 1 calc GR . . . .
H31B H 0.073040 0.505573 0.461901 0.036 Uiso 1 1 calc GR . . . .
H31C H -0.000675 0.497567 0.386855 0.036 Uiso 1 1 calc GR . . . .
C27 C -0.1676(9) 0.1661(8) 0.0815(4) 0.0216(17) Uani 1 1 d . . . . .
H27 H -0.066081 0.212138 0.111258 0.026 Uiso 1 1 calc R . . . .
C38 C 0.3455(9) 0.3219(9) 0.1255(4) 0.0234(17) Uani 1 1 d . . . . .
C32 C 0.1627(10) 0.3184(8) 0.4656(4) 0.0241(18) Uani 1 1 d . . . . .
H32A H 0.145811 0.227362 0.461777 0.036 Uiso 1 1 calc GR . . . .
H32B H 0.143660 0.339346 0.506677 0.036 Uiso 1 1 calc GR . . . .
H32C H 0.267495 0.372609 0.464022 0.036 Uiso 1 1 calc GR . . . .
C10 C 0.3611(10) 0.1012(9) 0.4726(4) 0.0250(18) Uani 1 1 d . . . . .
H10 H 0.336419 0.034103 0.500368 0.030 Uiso 1 1 calc R . . . .
C7 C 0.4379(9) 0.2999(8) 0.3915(4) 0.0188(16) Uani 1 1 d . . . . .
C28 C -0.1465(11) 0.1027(9) 0.0221(4) 0.030(2) Uani 1 1 d . . . . .
H28A H -0.100164 0.042561 0.036187 0.045 Uiso 1 1 calc GR . . . .
H28B H -0.080831 0.169588 -0.000200 0.045 Uiso 1 1 calc GR . . . .
H28C H -0.245288 0.055646 -0.007179 0.045 Uiso 1 1 calc GR . . . .
C26 C -0.2567(11) -0.2424(8) 0.2672(5) 0.0321(19) Uani 1 1 d . . . . .
H26A H -0.361242 -0.304426 0.250143 0.048 Uiso 1 1 calc GR . . . .
H26B H -0.218767 -0.263816 0.309957 0.048 Uiso 1 1 calc GR . . . .
H26C H -0.193301 -0.246055 0.238184 0.048 Uiso 1 1 calc GR . . . .
C16 C 0.0187(10) -0.0638(8) 0.4233(4) 0.0270(18) Uani 1 1 d . . . . .
H16A H 0.061703 -0.051518 0.469846 0.041 Uiso 1 1 calc GR . . . .
H16B H -0.062591 -0.150485 0.411989 0.041 Uiso 1 1 calc GR . . . .
H16C H -0.022238 0.000681 0.411364 0.041 Uiso 1 1 calc GR . . . .
C2 C 0.1646(9) 0.0162(8) 0.2057(4) 0.0199(16) Uani 1 1 d . . . . .
H2 H 0.206802 -0.022824 0.180389 0.024 Uiso 1 1 calc R . . . .
C8 C 0.5199(10) 0.3162(9) 0.4552(4) 0.0237(17) Uani 1 1 d . . . . .
H8 H 0.603105 0.395981 0.471186 0.028 Uiso 1 1 calc R . . . .
C30 C 0.0556(9) 0.3432(8) 0.4103(4) 0.0196(16) Uani 1 1 d . . . . .
C12 C 0.4908(9) 0.4111(8) 0.3491(4) 0.0224(17) Uani 1 1 d . . . . .
H12 H 0.421084 0.385044 0.305404 0.027 Uiso 1 1 calc R . . . .
C17 C 0.1894(11) -0.1622(9) 0.3987(4) 0.033(2) Uani 1 1 d . . . . .
H17A H 0.265701 -0.154284 0.374145 0.049 Uiso 1 1 calc GR . . . .
H17B H 0.100958 -0.243940 0.384329 0.049 Uiso 1 1 calc GR . . . .
H17C H 0.232076 -0.160335 0.444668 0.049 Uiso 1 1 calc GR . . . .
C42 C 0.2352(12) 0.4316(11) 0.0359(4) 0.040(2) Uani 1 1 d . . . . .
H42A H 0.136649 0.366521 0.039736 0.061 Uiso 1 1 calc GR . . . .
H42B H 0.267295 0.402523 0.000522 0.061 Uiso 1 1 calc GR . . . .
H42C H 0.226814 0.513378 0.027057 0.061 Uiso 1 1 calc GR . . . .
C9 C 0.4810(10) 0.2167(9) 0.4955(4) 0.0252(18) Uani 1 1 d . . . . .
H9 H 0.537544 0.228977 0.538678 0.030 Uiso 1 1 calc R . . . .
C23 C -0.2703(9) 0.0664(8) 0.1181(4) 0.0183(16) Uani 1 1 d . . . . .
C39 C 0.3531(11) 0.4511(9) 0.0996(4) 0.029(2) Uani 1 1 d . . . . .
C35 C 0.0609(13) 0.5790(10) 0.1557(4) 0.036(2) Uani 1 1 d . . . . .
H35A H 0.016805 0.641546 0.159006 0.055 Uiso 1 1 calc GR . . . .
H35B H -0.006718 0.509526 0.122187 0.055 Uiso 1 1 calc GR . . . .
H35C H 0.159421 0.622198 0.144628 0.055 Uiso 1 1 calc GR . . . .
C37 C -0.0693(10) 0.4790(9) 0.2404(4) 0.0263(18) Uani 1 1 d . . . . .
H37A H -0.063532 0.437716 0.280625 0.039 Uiso 1 1 calc GR . . . .
H37B H -0.149577 0.417275 0.206451 0.039 Uiso 1 1 calc GR . . . .
H37C H -0.091846 0.554074 0.246704 0.039 Uiso 1 1 calc GR . . . .
C5 C -0.0720(10) -0.1155(8) 0.1292(4) 0.0246(18) Uani 1 1 d . . . . .
H5A H -0.106363 -0.195648 0.150156 0.037 Uiso 1 1 calc GR . . . .
H5B H -0.005755 -0.118918 0.101466 0.037 Uiso 1 1 calc GR . . . .
H5C H -0.159811 -0.105184 0.103006 0.037 Uiso 1 1 calc GR . . . .
C20 C -0.4650(10) -0.1183(9) 0.1808(4) 0.0270(18) Uani 1 1 d . . . . .
H20 H -0.532156 -0.181209 0.202091 0.032 Uiso 1 1 calc R . . . .
C4 C 0.4067(10) 0.0666(9) 0.2847(4) 0.0270(19) Uani 1 1 d . . . . .
H4A H 0.490257 0.149612 0.302190 0.041 Uiso 1 1 calc GR . . . .
H4B H 0.427260 0.032802 0.247066 0.041 Uiso 1 1 calc GR . . . .
H4C H 0.396756 0.005420 0.317635 0.041 Uiso 1 1 calc GR . . . .
C13 C 0.6513(10) 0.4395(9) 0.3418(4) 0.0266(18) Uani 1 1 d . . . . .
H13A H 0.680595 0.506584 0.312199 0.040 Uiso 1 1 calc GR . . . .
H13B H 0.654178 0.360805 0.324506 0.040 Uiso 1 1 calc GR . . . .
H13C H 0.721782 0.469464 0.383948 0.040 Uiso 1 1 calc GR . . . .
C6 C 0.3152(8) 0.1821(7) 0.3692(3) 0.0146(15) Uani 1 1 d . . . . .
C19 C -0.3106(9) -0.0658(7) 0.2082(4) 0.0192(16) Uani 1 1 d . . . . .
C40 C 0.4866(11) 0.3340(12) 0.1743(4) 0.039(2) Uani 1 1 d . . . . .
H40A H 0.528907 0.416720 0.200611 0.059 Uiso 1 1 calc GR . . . .
H40B H 0.561555 0.329606 0.151724 0.059 Uiso 1 1 calc GR . . . .
H40C H 0.460659 0.263307 0.202145 0.059 Uiso 1 1 calc GR . . . .
B B 0.2150(10) 0.4058(9) 0.1752(4) 0.0184(18) Uani 1 1 d . . . . .
H H -0.143(8) 0.183(7) 0.268(4) 0.006(16) 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'
B B 0.0013 0.0007 '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'
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
N4 Nb N2 105.2(2) . . ?
N4 Nb N1 126.6(2) . . ?
N4 Nb H 104(2) . . ?
N2 Nb H 70(2) . . ?
N1 Nb N2 82.1(2) . . ?
N1 Nb H 127(2) . . ?
N3 Nb N4 104.8(3) . . ?
N3 Nb N2 143.6(3) . . ?
N3 Nb N1 96.2(3) . . ?
N3 Nb H 83(2) . . ?
N1 C1 C2 124.6(7) . . ?
N1 C1 C4 120.4(7) . . ?
C2 C1 C4 115.0(6) . . ?
B O1 C38 106.8(6) . . ?
N4 C34 C35 111.3(7) . . ?
N4 C34 C37 107.2(6) . . ?
C36 C34 N4 115.0(8) . . ?
C36 C34 C35 109.5(7) . . ?
C36 C34 C37 107.0(7) . . ?
C37 C34 C35 106.3(8) . . ?
C34 N4 Nb 129.2(5) . . ?
B N4 Nb 109.8(5) . . ?
B N4 C34 119.0(6) . . ?
B O2 C39 106.6(7) . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C3 N2 Nb 125.4(5) . . ?
C3 N2 C18 115.6(7) . . ?
C18 N2 Nb 119.0(4) . . ?
N2 C3 C2 123.8(7) . . ?
N2 C3 C5 122.5(7) . . ?
C2 C3 C5 113.6(7) . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
C25 C24 H24 108.2 . . ?
C25 C24 C26 108.9(7) . . ?
C26 C24 H24 108.2 . . ?
C19 C24 C25 111.3(6) . . ?
C19 C24 H24 108.2 . . ?
C19 C24 C26 111.9(7) . . ?
C1 N1 Nb 125.2(5) . . ?
C1 N1 C6 113.6(6) . . ?
C6 N1 Nb 121.0(4) . . ?
C23 C18 N2 120.7(7) . . ?
C19 C18 N2 119.7(7) . . ?
C19 C18 C23 119.6(7) . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
C11 C15 H15 108.8 . . ?
C11 C15 C16 109.9(7) . . ?
C11 C15 C17 111.1(7) . . ?
C16 C15 H15 108.8 . . ?
C16 C15 C17 109.4(7) . . ?
C17 C15 H15 108.8 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
C21 C22 H22 119.0 . . ?
C21 C22 C23 122.1(8) . . ?
C23 C22 H22 119.0 . . ?
C22 C21 H21 120.6 . . ?
C22 C21 C20 118.8(8) . . ?
C20 C21 H21 120.6 . . ?
C30 N3 Nb 163.2(6) . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
C10 C11 C15 119.8(8) . . ?
C10 C11 C6 117.5(8) . . ?
C6 C11 C15 122.7(7) . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
C29 C27 H27 108.3 . . ?
C29 C27 C28 108.2(7) . . ?
C28 C27 H27 108.3 . . ?
C23 C27 C29 111.6(7) . . ?
C23 C27 H27 108.3 . . ?
C23 C27 C28 111.9(7) . . ?
O1 C38 C41 108.5(7) . . ?
O1 C38 C39 101.5(6) . . ?
O1 C38 C40 107.1(6) . . ?
C41 C38 C39 115.6(7) . . ?
C41 C38 C40 109.4(8) . . ?
C40 C38 C39 113.9(8) . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
C11 C10 H10 119.0 . . ?
C9 C10 C11 122.0(8) . . ?
C9 C10 H10 119.0 . . ?
C8 C7 C12 118.1(7) . . ?
C6 C7 C8 118.5(7) . . ?
C6 C7 C12 123.3(7) . . ?
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 . . ?
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 . . ?
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 . . ?
C1 C2 H2 116.2 . . ?
C3 C2 C1 127.6(7) . . ?
C3 C2 H2 116.2 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.9(8) . . ?
C9 C8 H8 119.6 . . ?
N3 C30 C33 108.3(6) . . ?
N3 C30 C31 108.6(6) . . ?
N3 C30 C32 109.9(6) . . ?
C31 C30 C33 109.9(7) . . ?
C32 C30 C33 111.0(7) . . ?
C32 C30 C31 109.1(7) . . ?
C14 C12 H12 108.6 . . ?
C7 C12 C14 110.8(6) . . ?
C7 C12 H12 108.6 . . ?
C13 C12 C14 109.8(7) . . ?
C13 C12 C7 110.6(6) . . ?
C13 C12 H12 108.6 . . ?
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 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
C10 C9 C8 119.8(7) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C18 C23 C27 121.7(7) . . ?
C22 C23 C18 118.9(8) . . ?
C22 C23 C27 119.4(7) . . ?
O2 C39 C43 108.4(8) . . ?
O2 C39 C38 102.9(6) . . ?
O2 C39 C42 106.2(7) . . ?
C43 C39 C38 115.6(8) . . ?
C43 C39 C42 110.4(8) . . ?
C42 C39 C38 112.6(8) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 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 . . ?
C21 C20 H20 119.2 . . ?
C21 C20 C19 121.5(8) . . ?
C19 C20 H20 119.3 . . ?
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 . . ?
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 . . ?
C11 C6 N1 117.9(7) . . ?
C7 C6 N1 120.7(7) . . ?
C7 C6 C11 121.3(7) . . ?
C18 C19 C24 120.9(7) . . ?
C20 C19 C24 120.1(7) . . ?
C20 C19 C18 119.0(7) . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O1 B N4 118.7(7) . . ?
O2 B O1 112.6(7) . . ?
O2 B N4 128.7(7) . . ?
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
Nb N4 2.071(6) . ?
Nb N2 2.292(7) . ?
Nb N1 2.168(6) . ?
Nb N3 1.782(6) . ?
Nb H 1.97(7) . ?
C1 N1 1.335(10) . ?
C1 C2 1.416(12) . ?
C1 C4 1.520(10) . ?
O1 C38 1.463(9) . ?
O1 B 1.390(10) . ?
C34 N4 1.495(11) . ?
C34 C36 1.460(12) . ?
C34 C35 1.535(11) . ?
C34 C37 1.524(13) . ?
N4 B 1.428(11) . ?
O2 C39 1.451(10) . ?
O2 B 1.359(11) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N2 C3 1.318(10) . ?
N2 C18 1.458(10) . ?
C3 C2 1.399(11) . ?
C3 C5 1.526(11) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25 C24 1.536(11) . ?
C24 H24 1.0000 . ?
C24 C26 1.557(10) . ?
C24 C19 1.513(11) . ?
N1 C6 1.462(9) . ?
C18 C23 1.410(11) . ?
C18 C19 1.410(11) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 C30 1.537(11) . ?
C15 H15 1.0000 . ?
C15 C11 1.510(13) . ?
C15 C16 1.516(12) . ?
C15 C17 1.549(12) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C29 C27 1.530(12) . ?
C22 H22 0.9500 . ?
C22 C21 1.380(13) . ?
C22 C23 1.382(11) . ?
C21 H21 0.9500 . ?
C21 C20 1.382(12) . ?
N3 C30 1.470(9) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C41 C38 1.508(12) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43 C39 1.520(13) . ?
C11 C10 1.396(11) . ?
C11 C6 1.427(11) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 C12 1.536(11) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31 C30 1.530(11) . ?
C27 H27 1.0000 . ?
C27 C28 1.546(11) . ?
C27 C23 1.527(11) . ?
C38 C39 1.547(13) . ?
C38 C40 1.516(12) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C32 C30 1.520(11) . ?
C10 H10 0.9500 . ?
C10 C9 1.371(13) . ?
C7 C8 1.398(11) . ?
C7 C12 1.536(12) . ?
C7 C6 1.397(11) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C2 H2 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.398(12) . ?
C12 H12 1.0000 . ?
C12 C13 1.530(11) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C42 C39 1.546(13) . ?
C9 H9 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C20 H20 0.9500 . ?
C20 C19 1.390(12) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.706(2)
2 0.294(2)
