Synthesis, Characterization, and Reactions of Isolable (β-Diketiminato)Nb(III) Imido Complexes.
Tomson, Neil C.; Arnold, John; Bergman, Robert G.; Organometallics 29 (2010) 5010–5025; doi:10.1021/om1002528

data_4066026
_publ_section_title
;
 Synthesis, Characterization, and Reactions of Isolable
 (\b-Diketiminato)Nb(III) Imido Complexes.
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5010
_journal_page_last               5025
_journal_paper_doi               10.1021/om1002528
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C47 H66 N5 Nb'
_chemical_formula_sum            'C47 H66 N5 Nb'
_chemical_formula_weight         793.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.922(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.471(3)
_cell_length_b                   17.964(4)
_cell_length_c                   19.609(4)
_cell_measurement_reflns_used    1996
_cell_measurement_temperature    137(2)
_cell_measurement_theta_max      38.215
_cell_measurement_theta_min      4.535
_cell_volume                     4361.0(17)
_computing_cell_refinement       'Bruker SAINT v7.07'
_computing_data_collection       'Bruker SMART v5.631'
_computing_data_reduction        'Bruker SAINT v7.07'
_computing_molecular_graphics    'Bruker-AXS XP v.6'
_computing_publication_material  'Bruker-AXS XP v.6'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      137(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14628
_diffrn_reflns_theta_full        20.60
_diffrn_reflns_theta_max         20.60
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.874393
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         4437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                3409
_reflns_number_total             4437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1002528_si_001.cif
_cod_data_source_block           (BDI)pyNb(NtBu)(NMes)
_cod_original_cell_volume        4361.3(15)
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               4066026