1-Methyl-<i>N</i>-(4-nitrobenzyl)pyridinium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
Tong, Wen-Jun; Liu, Ling; Meng, Qing-Jin; Li, Yi-Zhi; Yao, Yuan-Gen; Acta Crystallographica Section E 59 (2003) m3–m5; doi:10.1107/S1600536802022006

data_2202098
_publ_section_title
;
 1-Methyl-<i>N</i>-(4-nitrobenzyl)pyridinium
 bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3
_journal_page_last               m5
_journal_paper_doi               10.1107/S1600536802022006
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(C13 H13 N2 O2) [Ni (C3 S5)2]'
_chemical_formula_moiety         'C13 H13 N2 O2 +, C6 Ni S10 -'
_chemical_formula_sum            'C19 H13 N2 Ni O2 S10'
_chemical_formula_weight         680.70
_chemical_name_systematic        ?
_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
_cell_angle_alpha                105.430(10)
_cell_angle_beta                 92.450(10)
_cell_angle_gamma                108.340(10)
_cell_formula_units_Z            2
_cell_length_a                   7.9820(10)
_cell_length_b                   12.364(2)
_cell_length_c                   13.978(2)
_cell_measurement_reflns_used    885
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.19
_cell_volume                     1250.1(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0877
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6270
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.324
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.60(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0558
_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^)+(0.02P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                2588
_reflns_number_total             4322
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6200.cif
_cod_data_source_block           I
_cod_database_code               2202098
_cod_database_fobs_code          2202098