1-(2,4-Dichlorobenzyl)pyridinium bis(2-sulfanylidene-1,3-dithiole-4,5-dithiolato-κ^2^<i>S</i>,<i>S</i>')nickelate(III)
Liu, Guang-Xiang; Acta Crystallographica Section E 67 (2011) m1654–; doi:10.1107/S1600536811045004

data_2232679
_publ_section_title
;
 1-(2,4-Dichlorobenzyl)pyridinium
 bis(2-sulfanylidene-1,3-dithiole-4,5-dithiolato-\k^2^<i>S</i>,<i>S</i>')nickelate(III)
;
_journal_coeditor_code           GK2414
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1654
_journal_paper_doi               10.1107/S1600536811045004
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C12 H10 Cl2 N) [Ni (C3 S5)2]'
_chemical_formula_moiety         'C12 H10 Cl2 N +, C6 Ni S10 -'
_chemical_formula_sum            'C18 H10 Cl2 N Ni S10'
_chemical_formula_weight         690.48
_chemical_name_systematic
;
1-(2,4-Dichlorobenzyl)pyridinium bis(2-sulfanylidene-1,3-dithiole-
4,5-dithiolato-\k^2^<i>S</i>,<i>S</i>')nickelate(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.2310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4614(5)
_cell_length_b                   8.2158(3)
_cell_length_c                   21.8894(8)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.66
_cell_volume                     2484.00(16)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18903
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_T_max  0.8367
_exptl_absorpt_correction_T_min  0.6450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.694
_refine_ls_extinction_coef       0.0070(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0486P)^2^+0.8363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                3992
_reflns_number_total             4615
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gk2414.cif
_cod_data_source_block           I
_cod_original_cell_volume        2484.00(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2232679
_cod_database_fobs_code          2232679