1,2-Addition and cycloaddition reactions of niobium bis(imido) and oxo imido complexes
Fostvedt, Jade I.; Grant, Lauren N.; Kriegel, Benjamin M.; Obenhuber, Andreas H.; Lohrey, Trevor D.; Bergman, Robert G.; Arnold, John; Chemical Science  (2020) –; doi:10.1039/D0SC03489D

data_1559322
_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       '\f and \w 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/[\s^2^(Fo^2^)+(0.1348P)^2^+10.6428P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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'