Halo, Alkyl, Aryl, and Bis(imido) Complexes of Niobium Supported by the beta-Diketiminato Ligand.
Tomson, Neil C.; Arnold, John; Bergman, Robert G.; Organometallics 29 (2010) 2926–2942; doi:10.1021/om1001827

data_4065891
_publ_section_title
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 Halo, Alkyl, Aryl, and Bis(imido) Complexes of Niobium Supported by the
 beta-Diketiminato Ligand.
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2926
_journal_page_last               2942
_journal_paper_doi               10.1021/om1001827
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C42 H64 N5 Nb'
_chemical_formula_sum            'C42 H64 N5 Nb'
_chemical_formula_weight         731.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.6487(12)
_cell_length_b                   18.8868(12)
_cell_length_c                   22.3644(14)
_cell_measurement_reflns_used    4710
_cell_measurement_temperature    457(2)
_cell_measurement_theta_max      42.741
_cell_measurement_theta_min      4.674
_cell_volume                     8299.5(9)
_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      153(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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33520
_diffrn_reflns_theta_full        22.73
_diffrn_reflns_theta_max         22.73
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.887106
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.382
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.382
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                4337
_reflns_number_total             5593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1001827_si_002.cif
_cod_data_source_block           (BDI)pyNb(NtBu)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '-120(2)' was changed to '153(2)'
- it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4065891