Groups 5 and 6 Terminal Hydrazido(2-) Complexes: Nβ Substituent Effects on Ligand-to-Metal Charge-Transfer Energies and Oxidation States
Ian A. Tonks; Alec C. Durrell; Harry B. Gray; John E. Bercaw; Journal of the American Chemical Society 134 (2012) 7301–7304; doi:10.1021/ja302275j

data_4117888
_publ_contact_author
;       Michael W. Day
        Beckman Institute
        California Institute of Technology
        Pasadena, CA  91125
        USA
;
_publ_contact_author_email       mikeday@caltech.edu
_publ_contact_author_fax         '(818) 449 4159'
_publ_contact_author_phone       '(818) 395 2734'
_publ_section_title
;
 Groups 5 and 6 Terminal Hydrazido(2-) Complexes: N\b Substituent Effects
 on Ligand-to-Metal Charge-Transfer Energies and Oxidation States
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7301
_journal_page_last               7304
_journal_paper_doi               10.1021/ja302275j
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C16 H18 Br2 Cl3 N2 Nb O2'
_chemical_formula_sum            'C16 H18 Br2 Cl3 N2 Nb O2'
_chemical_formula_weight         629.40
_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                 99.838(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8532(4)
_cell_length_b                   26.6360(13)
_cell_length_c                   9.4480(5)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.49
_cell_measurement_theta_min      2.32
_cell_volume                     2195.21(19)
_computing_cell_refinement       'Bruker SAINT-Plus v7.68A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.68A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 18 settings'
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            145626
_diffrn_reflns_theta_full        45.45
_diffrn_reflns_theta_max         45.45
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    4.567
_exptl_absorpt_correction_T_max  0.5107
_exptl_absorpt_correction_T_min  0.4198
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       Block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.553
_refine_diff_density_min         -1.521
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.445
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     237
_refine_ls_number_reflns         18408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.445
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0247
_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^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0401
_refine_ls_wR_factor_ref         0.0408
_reflns_number_gt                13363
_reflns_number_total             18408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja302275j_si_002_08.cif
_cod_data_source_block           2c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4117888