Crystal structure of bis[1-(4-bromobenzyl)pyridinium] bis(1,2-dicyanoethene-1,2-dithiolato-κ^2^<i>S</i>,<i>S</i>')nickelate(II)
Zeng, Dong; Yang, Shui-Bin; Tian, Zheng-Fang; Acta Crystallographica Section E 70 (2014) m395–m396; doi:10.1107/S1600536814024222

data_2240184
_publ_section_title
;
 Crystal structure of bis[1-(4-bromobenzyl)pyridinium]
 bis(1,2-dicyanoethene-1,2-dithiolato-\k^2^<i>S</i>,<i>S</i>')nickelate(II)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m395
_journal_page_last               m396
_journal_paper_doi               10.1107/S1600536814024222
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C12 H11 Br N)2 [Ni (C4 N2 S2)2]'
_chemical_formula_moiety         '2(C12 H11 Br N +), C8 N4 Ni S4 2-'
_chemical_formula_sum            'C32 H22 Br2 N6 Ni S4'
_chemical_formula_weight         837.29
_chemical_melting_point          473
_chemical_name_systematic
;
Bis[1-(4-bromobenzyl)pyridinium]
bis(1,2-dicyanoethene-1,2-dithiolato-\k^2^<i>S</i>,<i>S</i>')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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.385(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.783(2)
_cell_length_b                   11.962(3)
_cell_length_c                   14.858(3)
_cell_measurement_reflns_used    14683
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.19
_cell_volume                     1724.3(7)
_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
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14683
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    3.155
_exptl_absorpt_correction_T_max  0.6490
_exptl_absorpt_correction_T_min  0.5711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2000)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.908
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0517P)^2^+0.2393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                2204
_reflns_number_total             3040
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm5078sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1724.3(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2240184
_cod_database_fobs_code          2240184