Synthesis, Structure, and Cooperative Proton-Electron Transfer Reaction of Bis(5,6-diethylpyrazinedithiolato)metal Complexes (M = Ni, Pd, Pt)
Takashi Kubo; Misako Ohsahi; Katsuaki Miyazaki; Akio Ichimura; Kazuhiro Nakasuji; Inorganic Chemistry 43 (2004) 7301–7307; doi:10.1021/ic049621+

data_4327431
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science, Osaka University 
Machikaneyama 1-1, Toyonaka, Osaka, 560-0043, Japan
;
_publ_contact_author_email       kubo@chem.sci.osaka-u.ac.jp
_publ_contact_author_fax         '+81 6 6850 5395'
_publ_contact_author_name        'Takashi Kubo'
_publ_contact_author_phone       '+81 6 6850 5394'
_publ_section_title
;
 Synthesis, Structure, and Cooperative Proton-Electron Transfer Reaction
 of Bis(5,6-diethylpyrazinedithiolato)metal Complexes (M = Ni, Pd, Pt)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7301
_journal_page_last               7307
_journal_paper_doi               10.1021/ic049621+
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C22 H36 N6 Ni O2 S4'
_chemical_formula_weight         603.52
_chemical_name_common            Ni(Hdepdt)2-DMF
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                72.092(2)
_cell_angle_beta                 68.350(2)
_cell_angle_gamma                88.225(4)
_cell_formula_units_Z            1
_cell_length_a                   8.1157(5)
_cell_length_b                   9.1057(8)
_cell_length_c                   10.7936(11)
_cell_measurement_reflns_used    3287
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     702.38(10)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6074
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             318
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0817
_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^)+(0.1181P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.1746
_reflns_number_gt                2446
_reflns_number_total             3113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0496212Bsi20040322_012110_1.cif
_cod_data_source_block           NiDMF
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4327431