1-(2-Methoxy-2-oxoethyl)pyridinium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
Koori, Takahiro; Tomono, Kazuaki; Miyamura, Kazuo; Acta Crystallographica Section E 62 (2006) m256–m258; doi:10.1107/S160053680600016X

data_2208031
_publ_section_title
;
 1-(2-Methoxy-2-oxoethyl)pyridinium
 bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
;
_journal_coeditor_code           CV6628
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m256
_journal_page_last               m258
_journal_paper_doi               10.1107/S160053680600016X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C8 H10 N O2) [Ni (C3 H2 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
;
1-(2-Methoxy-2-oxoethyl)pyridinium
bis(2-thioxo-1,3-dithiole-4,5-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
_cell_angle_alpha                69.190(2)
_cell_angle_beta                 80.777(2)
_cell_angle_gamma                89.274(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1870(9)
_cell_length_b                   11.2783(12)
_cell_length_c                   13.0752(14)
_cell_measurement_reflns_used    2126
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.79
_cell_volume                     1112.7(2)
_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 (Bruno <i>et al.</i>,
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 0.983
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device       'Bruker SMART APEX CCD-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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6648
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time  330
_diffrn_standards_number         62
_exptl_absorpt_coefficient_mu    1.823
_exptl_absorpt_correction_T_max  0.93439
_exptl_absorpt_correction_T_min  0.75628
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(XPREP in SAINT; Bruker, 2001)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.269
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_expression not_defined
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0263P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                3072
_reflns_number_total             4674
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6628.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2208031
_cod_database_fobs_code          2208031