1-Butylpyridinium bis(1,2-dicyanoethene-1,2-dithiolato)nickelate(III)
Duan, Hai-Bao; Acta Crystallographica Section E 67 (2011) m1567–; doi:10.1107/S1600536811042103

data_2232476
_publ_section_title
;
 1-Butylpyridinium bis(1,2-dicyanoethene-1,2-dithiolato)nickelate(III)
;
_journal_coeditor_code           TK2798
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1567
_journal_paper_doi               10.1107/S1600536811042103
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C9 H14 N) [Ni (C4 N2 S2)2]'
_chemical_formula_moiety         'C9 H14 N +, C8 N4 Ni S4 -'
_chemical_formula_sum            'C17 H14 N5 Ni S4'
_chemical_formula_weight         475.30
_chemical_name_systematic
;
1-Butylpyridinium bis(1,2-dicyanoethene-1,2-dithiolato)nicklate(III)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.695(9)
_cell_angle_beta                 75.882(10)
_cell_angle_gamma                64.480(11)
_cell_formula_units_Z            2
_cell_length_a                   9.2764(11)
_cell_length_b                   9.9863(11)
_cell_length_c                   12.7115(15)
_cell_measurement_temperature    293(2)
_cell_volume                     1029.5(2)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7461
_diffrn_reflns_theta_full        62.62
_diffrn_reflns_theta_max         62.62
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    5.254
_exptl_absorpt_correction_T_max  0.591
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.328
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3196
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                2499
_reflns_number_total             3196
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2798.cif
_cod_data_source_block           I
_cod_database_code               2232476
_cod_database_fobs_code          2232476