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_1559328
_publ_section_title
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 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         'C51 H69 N4 Nb O'
_chemical_formula_sum            'C51 H69 N4 Nb O'
_chemical_formula_weight         847.01
_chemical_melting_point          423
_chemical_name_common            (BDI)Nb(NAr)(N(tBu)C(CPh2)O)
_chemical_name_systematic
(N-tert-butylamino-2,2-diphenylethenolato-N,O)-(2,6-diisopropylphenyl)imino-(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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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
;
2020-05-15 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.813(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1485(11)
_cell_length_b                   15.8759(7)
_cell_length_c                   24.2007(11)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.18
_cell_volume                     9081.5(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 0.995
_diffrn_measured_fraction_theta_max 0.991
_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  0.0400
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            123296
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.441
_diffrn_reflns_theta_min         1.544
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0864 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.9538.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.385
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1059
_refine_ls_number_reflns         16641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+6.4150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12840
_reflns_number_total             16641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03489d2.cif
_cod_data_source_block           bmkxr74
_cod_database_code               1559328
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.941
_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:
 C27(H27), C75(H75), C63(H63), C24(H24), C12(H12), C78(H78), C66(H66), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C2(H2), C61(H61), C92(H92), C51(H51), C93(H93), C60(H60), C10(H10),
 C72(H72), C9(H9), C41(H41), C20(H20), C73(H73), C102(H102), C59(H59), C8(H8),
 C21(H21), C22(H22), C71(H71), C42(H42), C100(H100), C96(H96), C95(H95),
 C94(H94), C49(H49), C50(H50), C43(H43), C101(H101), C98(H98), C99(H99),
 C45(H45), C48(H48), C47(H47), C44(H44)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C),
 C87(H87A,H87B,H87C), C25(H25A,H25B,H25C), C36(H36A,H36B,H36C), C88(H88A,H88B,
 H88C), C83(H83A,H83B,H83C), C37(H37A,H37B,H37C), C77(H77A,H77B,H77C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C),
 C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C79(H79A,H79B,H79C), C82(H82A,H82B,
 H82C), C32(H32A,H32B,H32C), C13(H13A,H13B,H13C), C65(H65A,H65B,H65C), C67(H67A,
 H67B,H67C), C26(H26A,H26B,H26C), C76(H76A,H76B,H76C), C68(H68A,H68B,H68C),
 C64(H64A,H64B,H64C), C80(H80A,H80B,H80C), C31(H31A,H31B,H31C), C17(H17A,H17B,
 H17C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'