Unusual κ1 coordination of a β-diketiminate ligand in niobium complexes.
Ziegler, Jessica A.; Bergman, Robert G.; Arnold, John; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12661–12668; doi:10.1039/c6dt02373h

data_7040065
_publ_section_title
;
 Unusual \k1 coordination of a \b-diketiminate ligand in niobium
 complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12661
_journal_page_last               12668
_journal_paper_doi               10.1039/c6dt02373h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C38 H55 N3 Nb 1+, C24 H20 B 1-, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C62.5 H76 B Cl N3 Nb'
_chemical_formula_weight         1008.43
_chemical_name_common            '[(BDI)CpNb(NtBu)][BPh4]'
_chemical_properties_physical    ', Air-sensitive,Moisture-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'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   '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
;
2016-07-14 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                66.416(5)
_cell_angle_beta                 83.348(5)
_cell_angle_gamma                88.954(5)
_cell_formula_units_Z            4
_cell_length_a                   17.283(5)
_cell_length_b                   17.704(5)
_cell_length_c                   19.633(5)
_cell_measurement_reflns_used    9506
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.31
_cell_volume                     5466(3)
_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    SIR-2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.8366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            87658
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_min         1.140
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             2140
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/hexane'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1249
_refine_ls_number_reflns         20049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0279P)^2^+5.7779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16728
_reflns_number_total             20049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02373h2.cif
_cod_data_source_block           Compound3
_cod_depositor_comments
'Adding full bibliography for 7040063--7040066.cif.'
_cod_original_formula_sum        'C62.50 H76 B Cl N3 Nb'
_cod_database_code               7040065
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.982
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              19907
_shelx_hkl_checksum              25617
_shelx_fab_checksum              61973