Bis[1-(4-cyanobenzyl)pyrazinium] bis(1,2-dicyanoethene-1,2-dithiolato)nickelate(II)
Zhang, Hui; Pei, Wen-Bo; Yu, Shan-Shan; Ren, Xiao-Ming; Acta Crystallographica Section E 67 (2011) m943–; doi:10.1107/S1600536811022550

data_2230721
_publ_section_title
;
 Bis[1-(4-cyanobenzyl)pyrazinium]
 bis(1,2-dicyanoethene-1,2-dithiolato)nickelate(II)
;
_journal_coeditor_code           IM2295
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m943
_journal_paper_doi               10.1107/S1600536811022550
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C12 H10 N3)2 [Ni (C4 N2 S2)2]'
_chemical_formula_moiety         '2(C12 H10 N3 +), C8 N4 Ni S4 2-'
_chemical_formula_sum            'C32 H20 N10 Ni S4'
_chemical_formula_weight         731.53
_chemical_melting_point          456
_chemical_name_systematic
;
Bis[1-(4-cyanobenzyl)pyrazinium]
bis(1,2-dicyanoethene-1,2-dithiolato)nickelate(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.671(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.115(3)
_cell_length_b                   13.623(6)
_cell_length_c                   17.186(8)
_cell_measurement_reflns_used    8060
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.42
_cell_volume                     1631.4(13)
_computing_cell_refinement       'SMART (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8060
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0431P)^2^+0.3009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                2586
_reflns_number_total             2871
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            im2295.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2230721
_cod_database_fobs_code          2230721