3-Methoxycarbonyl-1-methylpyridinium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(II)
Tomono, Kazuaki; Sasaki, Yuka; Miyamura, Kazuo; Acta Crystallographica Section E 61 (2005) m18–m20; doi:10.1107/S1600536804031034

data_2204917
_publ_section_title
;
 3-Methoxycarbonyl-1-methylpyridinium
 bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(II)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m18
_journal_page_last               m20
_journal_paper_doi               10.1107/S1600536804031034
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '(C8 H10 N O2) [Ni (C3 S5)2]'
_chemical_formula_moiety         'C8 H10 N O2 +, C6 Ni S10 -'
_chemical_formula_sum            'C14 H10 N Ni O2 S10'
_chemical_formula_weight         603.54
_chemical_name_systematic
;
3-Methoxycarbonyl-1-methylpyridinium
bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(II)
;
_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                84.319(5)
_cell_angle_beta                 82.170(5)
_cell_angle_gamma                80.583(5)
_cell_formula_units_Z            2
_cell_length_a                   7.2051(19)
_cell_length_b                   12.139(3)
_cell_length_c                   12.732(3)
_cell_measurement_reflns_used    2889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      1.62
_cell_volume                     1085.0(5)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and MERCURY (CCDC, 2002)'
_computing_publication_material
;
SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX (Sakai, 2002),
ORTEPIII and MERCURY
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7209
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        'no decay, variation 0.34'
_diffrn_standards_interval_time  330
_diffrn_standards_number         92
_exptl_absorpt_coefficient_mu    1.869
_exptl_absorpt_correction_T_max  0.96688
_exptl_absorpt_correction_T_min  0.69296
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(XPREP in SAINT; Bruker, 2001)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.676
_refine_diff_density_min         -0.674
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_expression not_defined
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0961P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1847
_reflns_number_gt                3426
_reflns_number_total             4870
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6312.cif
_cod_data_source_block           I
_cod_database_code               2204917