N-N Bond Cleavage of 1,2-Diarylhydrazines and N-H Bond Formation via H-Atom Transfer in Vanadium Complexes Supported by a Redox-Active Ligand.
Milsmann, Carsten; Semproni, Scott P.; Chirik, Paul J.; Journal of the American Chemical Society 136 (2014) 12099–; doi:10.1021/ja5062196

data_4122429
_publ_section_title
;
 N-N Bond Cleavage of 1,2-Diarylhydrazines and N-H Bond Formation via
 H-Atom Transfer in Vanadium Complexes Supported by a Redox-Active Ligand.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12099
_journal_paper_doi               10.1021/ja5062196
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C121 H133 N10 V2'
_chemical_formula_weight         1829.25
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.568(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.567(5)
_cell_length_b                   24.266(5)
_cell_length_c                   18.216(5)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.51
_cell_measurement_theta_min      3.04
_cell_volume                     5089(3)
_computing_cell_refinement       'BRUKER, APEX II SOFTWARE SUITE'
_computing_data_collection       'BRUKER, APEX II SOFTWARE SUITE'
_computing_data_reduction        'BRUKER, APEX II SOFTWARE SUITE'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
'SUPERFLIP (Palatinus, L. and Chapuis, G., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25544
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         65.93
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.953
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.6642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1950
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         8561
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+1.5703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                6924
_reflns_number_total             8561
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja5062196_si_002.cif
_cod_data_source_block           cm51_relabel
_cod_depositor_comments
'Adding full bibliography for 4122429--4122430.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4122429