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_1559315
_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         'C48 H68 N5 Nb O, 0.5(C6 H6)'
_chemical_formula_sum            'C51 H71 N5 Nb O'
_chemical_formula_weight         863.03
_chemical_melting_point          492
_chemical_name_common            (BDI)Nb(NAr)(O)(DMAP)
_chemical_name_systematic
'(2,6-diisopropylphenyl)imino-oxido-4-dimethylaminopyridine-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V) benzene solvate'
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-05-14 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                81.664(2)
_cell_angle_beta                 85.819(3)
_cell_angle_gamma                68.744(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6646(8)
_cell_length_b                   12.6365(7)
_cell_length_c                   17.2467(10)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.77
_cell_volume                     2343.6(2)
_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    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31429
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.469
_diffrn_reflns_theta_min         1.194
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       block
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         8583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0288
_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/[\s^2^(Fo^2^)+(0.0211P)^2^+1.8827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7993
_reflns_number_total             8583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03489d2.cif
_cod_data_source_block           shelx_CCDC1
_cod_database_code               1559315
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.965