Bis[1-(ethoxycarbonylmethyl)pyridinium] bis(1,2-dicyanoethene-1,2-dithiolato-κ^2^<i>S</i>,<i>S</i>')nickelate(II)
Ren, Tian-li; Yang, Cheng-jian; Fang, De-yu; Shi, Guo-xun; Zhu, Xue; Acta Crystallographica Section E 68 (2012) m1151–; doi:10.1107/S1600536812033831

data_2236144
_publ_section_title
;
 Bis[1-(ethoxycarbonylmethyl)pyridinium]
 bis(1,2-dicyanoethene-1,2-dithiolato-\k^2^<i>S</i>,<i>S</i>')nickelate(II)
;
_journal_coeditor_code           BX2420
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1151
_journal_paper_doi               10.1107/S1600536812033831
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C9 H12 N O2)2 [Ni (C4 N2 S2)2 ]'
_chemical_formula_moiety         '2(C9 H12 N O2 +), C8 N4 Ni S4 2-'
_chemical_formula_sum            'C26 H24 N6 Ni O4 S4'
_chemical_formula_weight         671.46
_chemical_name_systematic
;
Bis[1-(ethoxycarbonylmethyl)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 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                 104.803(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.486(2)
_cell_length_b                   19.542(5)
_cell_length_c                   17.635(4)
_cell_measurement_reflns_used    1842
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      19.95
_cell_measurement_theta_min      2.39
_cell_volume                     3160.6(13)
_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  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(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       '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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16888
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.9137
_exptl_absorpt_correction_T_min  0.7701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0432
_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^)+(0.06P)^2^+1.22P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                5024
_reflns_number_total             6200
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bx2420.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2236144
_cod_database_fobs_code          2236144