<i>N</i>-Ethylpyridinium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate
Xue, Gang; Xu, Wen; Yu, Wentao; Fang, Qi; Acta Crystallographica Section C 59 (2003) m27–m29; doi:10.1107/S0108270102020115

data_2013164
_publ_section_title
;
 <i>N</i>-Ethylpyridinium
 bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m27
_journal_page_last               m29
_journal_paper_doi               10.1107/S0108270102020115
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[C7 H10 N] [Ni (C3 S5)2]'
_chemical_formula_moiety         'C7 H10 N + , C6 Ni1 S10 -'
_chemical_formula_sum            'C13 H10 N Ni S10'
_chemical_formula_weight         559.61
_chemical_melting_point          470
_chemical_name_systematic
;
N-ethylpyridinium 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
_audit_creation_method           SHELXL97
_cell_angle_alpha                112.555(9)
_cell_angle_beta                 104.477(7)
_cell_angle_gamma                95.876(10)
_cell_formula_units_Z            4
_cell_length_a                   8.7825(8)
_cell_length_b                   16.209(2)
_cell_length_c                   16.7077(16)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.41
_cell_measurement_theta_min      5.30
_cell_volume                     2073.8(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.97
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \q/2\q
_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  0.024
_diffrn_reflns_av_sigmaI/netI    0.043
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8565
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.941
_exptl_absorpt_correction_T_max  0.678
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(XSCANS; Siemens, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.40
_refine_ls_extinction_coef       0.00173(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Bruker, 1997)'
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         7056
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.076
_refine_ls_R_factor_gt           0.043
_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^)+(0.0509P)^2^+2.0853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.099
_refine_ls_wR_factor_ref         0.118
_reflns_number_gt                4722
_reflns_number_total             7056
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg1142.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C13 H10 N Ni1 S10'
_cod_database_code               2013164
_cod_database_fobs_code          2013164