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_4122430
_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            'C55 H58 N5 V'
_chemical_formula_weight         840.00
_chemical_name_systematic
;
 ?
;
_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                90.000
_cell_angle_beta                 98.202(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   9.095(5)
_cell_length_b                   25.897(5)
_cell_length_c                   19.745(5)
_cell_measurement_reflns_used    9481
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.64
_cell_measurement_theta_min      2.83
_cell_volume                     4603(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP 3 (Farraguia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR 92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.963
_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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21855
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         65.98
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    2.116
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+1.3342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                6340
_reflns_number_total             7729
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja5062196_si_002.cif
_cod_data_source_block           cm74_relabel
_cod_depositor_comments
'Adding full bibliography for 4122429--4122430.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4122430