Nickel Complexes of o-Amidochalcogenophenolate(2-)/o-Iminochalcogenobenzosemiquinonate(1-) π-Radical: Synthesis, Structures, Electron Spin Resonance, and X-ray Absorption Spectroscopic Evidence
Chung-Hung Hsieh; I-Jui Hsu; Chien-Ming Lee; Shyue-Chu Ke; Tze-Yuan Wang; Gene-Hsiang Lee; Yu Wang; Jin-Ming Chen; Jyh-Fu Lee; Wen-Feng Liaw; Inorganic Chemistry 42 (2003) 3925–3933; doi:10.1021/ic034211r

data_4313783
_publ_section_title
;
 Nickel Complexes of
 o-Amidochalcogenophenolate(2-)/o-Iminochalcogenobenzosemiquinonate(1-)
 \p-Radical: Synthesis, Structures, Electron Spin Resonance, and X-ray
 Absorption Spectroscopic Evidence
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3925
_journal_page_last               3933
_journal_paper_doi               10.1021/ic034211r
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C48 H40 N3 Ni P2 Se2'
_chemical_formula_weight         937.40
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 99.485(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1779(12)
_cell_length_b                   11.3673(8)
_cell_length_c                   20.4646(14)
_cell_measurement_temperature    293(2)
_cell_volume                     4170.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0748
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12999
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    2.325
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunky
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0010P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0472
_reflns_number_gt                2329
_reflns_number_total             4747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034211rsi20030225_095102.cif
_cod_data_source_block           liaw085m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313783