1-(4-Iodobenzyl)-3-methylpyridinium bis(benzene-1,2-dithiolato)nickelate(III)
Liu, Guang-Xiang; Acta Crystallographica Section E 67 (2011) m1607–; doi:10.1107/S1600536811043522

data_2232456
_publ_section_title
;
 1-(4-Iodobenzyl)-3-methylpyridinium
 bis(benzene-1,2-dithiolato)nickelate(III)
;
_journal_coeditor_code           RZ2652
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1607
_journal_paper_doi               10.1107/S1600536811043522
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C13 H13 I N) [Ni (C6 H4 S2)2]'
_chemical_formula_moiety         'C13 H13 I N +, C12 H8 Ni S4 -'
_chemical_formula_sum            'C25 H21 I N Ni S4'
_chemical_formula_weight         649.28
_chemical_name_systematic
;
1-(4-Iodobenzyl)-3-methylpyridinium bis(benzene-1,2-dithiolato)nickelate(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                98.425(2)
_cell_angle_beta                 98.466(2)
_cell_angle_gamma                96.216(3)
_cell_formula_units_Z            2
_cell_length_a                   7.3222(14)
_cell_length_b                   12.267(2)
_cell_length_c                   14.628(3)
_cell_measurement_reflns_used    2848
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.39
_cell_volume                     1274.2(4)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6282
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    2.315
_exptl_absorpt_correction_T_max  0.7686
_exptl_absorpt_correction_T_min  0.5844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.524
_refine_diff_density_min         -1.913
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0559
_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^)+(0.1231P)^2^+0.2746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1957
_reflns_number_gt                3397
_reflns_number_total             4392
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2652.cif
_cod_data_source_block           I
_cod_database_code               2232456
_cod_database_fobs_code          2232456