1-(4-Cyanobenzyl)-4-methylpyridinium bis(benzene-1,2-dithiolato)nickelate(III)
Liu, Guang-Xiang; Acta Crystallographica Section E 63 (2007) m1707–; doi:10.1107/S1600536807023847

data_2213831
_publ_section_title
;
 1-(4-Cyanobenzyl)-4-methylpyridinium
 bis(benzene-1,2-dithiolato)nickelate(III)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1707
_journal_paper_doi               10.1107/S1600536807023847
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C14 H13 N2) [Ni (C6 H4 S2)2]'
_chemical_formula_moiety         'C14 H13 N2 + , C12 H8 Ni S4 -'
_chemical_formula_sum            'C26 H21 N2 Ni S4'
_chemical_formula_weight         548.40
_chemical_name_systematic
;1-(4-Cyanobenzyl)-4-methylpyridinium
 bis(benzene-1,2-dithiolato)nickelate(III)
;
_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                 96.480(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   42.344(3)
_cell_length_b                   7.2455(6)
_cell_length_c                   32.768(2)
_cell_measurement_reflns_used    1320
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      16.47
_cell_measurement_theta_min      2.85
_cell_volume                     9989.1(13)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type
'Bruker SMART APEX CCD area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1131
_diffrn_reflns_av_sigmaI/netI    0.1500
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            27982
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  0.8955
_exptl_absorpt_correction_T_min  0.8057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.1923
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                3392
_reflns_number_total             8530
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2244.cif
_cod_data_source_block           I
_cod_original_cell_volume        9988.9(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2213831
_cod_database_fobs_code          2213831