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_4117891
_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         'C18 H24 Cl3 N2 Nb O4, 0.5(C7 H8)'
_chemical_formula_sum            'C21.5 H28 Cl3 N2 Nb O4'
_chemical_formula_weight         577.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.7650(10)
_cell_angle_beta                 95.120(2)
_cell_angle_gamma                99.874(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4401(3)
_cell_length_b                   10.5793(5)
_cell_length_c                   16.3555(7)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.51
_cell_volume                     1248.30(9)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans; 9 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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35718
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2009/1, Bruker-AXS, Madison'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       Plate
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.19
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_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.445
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     309
_refine_ls_number_reflns         7617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.445
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_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          0.0624
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                6672
_reflns_number_total             7617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja302275j_si_002_11.cif
_cod_data_source_block           2f
_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_original_formula_sum        'C21.50 H28 Cl3 N2 Nb O4'
_cod_database_code               4117891