2,3-Diethylthiazolium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
Tomiyama, Etsuko; Tomono, Kazuaki; Miyamura, Kazuo; Acta Crystallographica Section E 63 (2007) m2741–m2741; doi:10.1107/S1600536807049070

data_2215845
_publ_section_title
;
 2,3-Diethylthiazolium
 bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
;
_journal_coeditor_code           CI2476
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2741
_journal_page_last               m2741
_journal_paper_doi               10.1107/S1600536807049070
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C7 H12 N S) [Ni (C3 S5)2]'
_chemical_formula_moiety         'C7 H12 N S + ,  C6 Ni1 S10 -'
_chemical_formula_sum            'C13 H12 N Ni S11'
_chemical_formula_weight         593.61
_chemical_name_systematic
;
2,3-Diethylthiazolium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.344(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2465(9)
_cell_length_b                   10.4325(12)
_cell_length_c                   25.382(3)
_cell_measurement_reflns_used    4004
_cell_measurement_temperature    300.0(10)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.53
_cell_volume                     2179.9(4)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and Mercury (Bruno <i>et al.</i>,
2002)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 1997) and KENX (Sakai, 2002)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      300.0(10)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13052
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        'no decay, variation 0.115'
_diffrn_standards_interval_time  330
_diffrn_standards_number         134
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_T_max  0.93343
_exptl_absorpt_correction_T_min  0.71869
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(XPREP; Bruker, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.332
_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     237
_refine_ls_number_reflns         4945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0377P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                3804
_reflns_number_total             4945
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2476.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2215845
_cod_database_fobs_code          2215845