Metal centered oxidation or ligand centered oxidation of metal dithiolene? Spectral, electrochemical and structural studies on a nickel-4-pyridine-1,2-dithiolate system.
Li, Xin-Yu; Sun, Yong-Gang; Huo, Peng; Shao, Ming-Yan; Ji, Shu-Fang; Zhu, Qin-Yu; Dai, Jie; Physical chemistry chemical physics : PCCP 15 (2013) 4016–4023; doi:10.1039/c3cp44054k

data_7211280
_publ_section_title
;
 Metal centered oxidation or ligand centered oxidation of metal
 dithiolene? Spectral, electrochemical and structural studies on a
 nickel-4-pyridine-1,2-dithiolate system.
;
_journal_issue                   11
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              4016
_journal_page_last               4023
_journal_paper_doi               10.1039/c3cp44054k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C27 H33 N4 Ni O5 S5'
_chemical_formula_weight         712.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 96.088(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.049(4)
_cell_length_b                   11.691(6)
_cell_length_c                   14.982(7)
_cell_measurement_reflns_used    5486
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1576.0(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.1082
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10855
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.6928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5700
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0215P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                4296
_reflns_number_total             5700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cp44054k.txt
_cod_data_source_block           3
_cod_original_cell_volume        1576.1(13)
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               7211280