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_4330356
_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 H58 N4 Ni'
_chemical_formula_sum            'C41 H58 N4 Ni'
_chemical_formula_weight         665.62
_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                95.819(8)
_cell_angle_beta                 96.008(8)
_cell_angle_gamma                110.731(8)
_cell_formula_units_Z            2
_cell_length_a                   9.8640(10)
_cell_length_b                   12.3300(13)
_cell_length_c                   16.8483(16)
_cell_measurement_reflns_used    30048
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      3.25
_cell_volume                     1884.7(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1298
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27108
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         3.34
_diffrn_standards_decay_%        'No decay'
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.419
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6806
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0899
_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^)+(0.1094P)^2^+4.3258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2214
_refine_ls_wR_factor_ref         0.2380
_reflns_number_gt                5399
_reflns_number_total             6806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301066x_si_001_1.cif
_cod_data_source_block           c:\stoe\1\moni59a_complex3
_cod_original_cell_volume        1884.7(3)
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4330356