Reductive Deprotonation and Dehydrogenation of Phenylhydrazine at a Nickel Center To Give a Nickel Diazenido Complex
Claudia Köthe; Ramona Metzinger; Christian Herwig; Christian Limberg; Inorganic Chemistry 51 (2012) 9740–9747; doi:10.1021/ic301066x

data_4330357
_publ_contact_author_address
;
      Institut fuer Chemie
      Humboldt Universitaet zu Berlin
      Brook-Taylor-Str. 2
      12489 Berlin
      Germany
;
_publ_contact_author_email       ramona.metzinger@chemie.hu-berlin.de
_publ_contact_author_fax         0049-30-20936966
_publ_contact_author_name        'Ramona Metzinger'
_publ_contact_author_phone       0049-30-20937391
_publ_section_title
;
 Reductive Deprotonation and Dehydrogenation of Phenylhydrazine at a
 Nickel Center To Give a Nickel Diazenido Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9740
_journal_page_last               9747
_journal_paper_doi               10.1021/ic301066x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C41 H60 N4 Ni'
_chemical_formula_sum            'C41 H60 N4 Ni'
_chemical_formula_weight         667.64
_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                 113.932(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6151(6)
_cell_length_b                   12.2221(3)
_cell_length_c                   19.5038(7)
_cell_measurement_reflns_used    30862
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.02
_cell_volume                     4055.9(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'STOE IPDS 2 Theta'
_diffrn_measurement_method       'Rotation Method'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9657
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        'No decay'
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       needle
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         9657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                6436
_reflns_number_total             9657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301066x_si_001_2.cif
_cod_data_source_block           c:\stoe\1\moni33_complex1
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4330357