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_1559324
_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         'C64 H67 B F15 N4 Nb O2, C4 H10 O'
_chemical_formula_sum            'C68 H77 B F15 N4 Nb O3'
_chemical_formula_weight         1387.05
_chemical_melting_point          458
_chemical_name_common            (BDI)Nb(NAr)(N(tBu)CO2B(C6F5)3)
_chemical_name_systematic
'(tris(pentafluorophenyl)borate-N-tert-butylcarbamidato-N,O)-(2,6-diisopropylphenyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V) diethyl ether solvate'
_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
;
2020-05-14 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.576(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.2228(19)
_cell_length_b                   24.338(2)
_cell_length_c                   24.561(2)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.36
_cell_volume                     13279.0(19)
_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 0.994
_diffrn_measured_fraction_theta_max 0.988
_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  0.1107
_diffrn_reflns_av_unetI/netI     0.1368
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            63281
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.427
_diffrn_reflns_theta_min         1.659
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       plate
_exptl_crystal_F_000             5744
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.938
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1695
_refine_ls_number_reflns         24250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0688
_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/[\s^2^(Fo^2^)+(0.0905P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14154
_reflns_number_total             24250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03489d2.cif
_cod_data_source_block           bmkxr69
_cod_original_cell_volume        13279(2)
_cod_database_code               1559324
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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), C76(H76),
 C79(H79), C88(H88), C91(H91), C100(H100), C103(H103)
2.b Secondary CH2 refined with riding coordinates:
 C130(H13D,H13E), C131(H13F,H13G), C134(H13N,H13O), C135(H13P,H13Q)
2.c 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), C66(H66), C72(H72), C73(H73), C74(H74), C84(H84), C85(H85),
  C86(H86), C96(H96), C97(H97), C98(H98)
2.d 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), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C81(H81A,
 H81B,H81C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C),
 C93(H93A,H93B,H93C), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C104(H10G,
 H10H,H10I), C105(H10J,H10K,H10L), C107(H10M,H10N,H10O), C108(H10P,H10Q,H10R),
 C109(H10S,H10T,H10U), C129(H12A,H12B,H12C), C132(H13H,H13I,H13J), C133(H13K,
 H13L,H13M), C136(H13R,H13S,H13T)
;
_olex2_submission_special_instructions 'No special instructions were received'