Crystal Structure of Dimethyldodecylhexadecylammonium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
DAI, Kotaro; KUSUNOKI, Satoe; HIROTA, Mami; TOMONO, Kazuaki; MIYAMURA, Kazuo; X-ray Structure Analysis Online 27 (2011) 35–; doi:10.2116/xraystruct.27.35

data_1551723
_publ_section_title
;
 Crystal Structure of Dimethyldodecylhexadecylammonium
 bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
;
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              35
_journal_paper_doi               10.2116/xraystruct.27.35
_journal_volume                  27
_journal_year                    2011
_chemical_formula_iupac          'C36 H64 N Ni S10'
_chemical_formula_moiety         'C30 H64 N, C6 Ni S10'
_chemical_formula_sum            'C36 H64 N Ni S10'
_chemical_formula_weight         890.19
_chemical_name_systematic
;
Dimethyldodecylhexadecylammonium
bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                84.5750(10)
_cell_angle_beta                 87.9670(10)
_cell_angle_gamma                86.7670(10)
_cell_formula_units_Z            2
_cell_length_a                   7.6149(5)
_cell_length_b                   12.2245(9)
_cell_length_c                   24.2399(17)
_cell_measurement_reflns_used    3335
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.49
_cell_volume                     2241.7(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEPIII (Burnett &amp; Johnson, 1996) and MERCURY (CCDC, 2002)'
_computing_publication_material
;
SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), 
KENX, and ORTEPIII and MERCURY
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device
'Bruker SMART APEX CCD-detector diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13752
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.81
_diffrn_standards_interval_time  330
_diffrn_standards_number         58
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.94907
_exptl_absorpt_correction_T_min  0.85273
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(XPREP; Bruker AXS 2000)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             950
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.498
_refine_diff_density_min         -0.727
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_expression not_defined
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         9628
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1806
_reflns_number_gt                6574
_reflns_number_total             9628
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            27_35_1.cif
_cod_data_source_block           c1612nit173ka
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               1551723