Bis(tetra-<i>n</i>-butylammonium) bis(2-dicyanomethylene-4,5-dimercapto-1,3-dithiole)nickel(II)
Tomura, Masaaki; Yamashita, Yoshiro; Acta Crystallographica Section E 58 (2002) m133–m135; doi:10.1107/S1600536802004816

data_2201156
_publ_section_title
;
 Bis(tetra-<i>n</i>-butylammonium)
 bis(2-dicyanomethylene-4,5-dimercapto-1,3-dithiole)nickel(II)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m133
_journal_page_last               m135
_journal_paper_doi               10.1107/S1600536802004816
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C16 H36 N1)2 [Ni (C6 N2 S4)2]'
_chemical_formula_moiety         '2C16 H36 N1 1+, C12 N4 Ni S8 2-'
_chemical_formula_sum            'C44 H72 N6 Ni S8'
_chemical_formula_weight         1000.33
_chemical_melting_point          521
_chemical_name_systematic
;
bis(tetra-n-butylammonium) bis(2-dicyanomethylene-4,5-dimercapto-
1,3-dithiole)nickel(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                76.26(3)
_cell_angle_beta                 80.99(3)
_cell_angle_gamma                89.69(4)
_cell_formula_units_Z            1
_cell_length_a                   8.252(4)
_cell_length_b                   12.012(6)
_cell_length_c                   13.867(6)
_cell_measurement_reflns_used    4920
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1318.0(11)
_computing_cell_refinement
;
CrystalClear
;
_computing_data_collection
;
CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation & Rigaku Corporation, 2000)
;
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'Graphite monochromator'
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12833
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.9649
_exptl_absorpt_correction_T_min  0.6718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            green--black
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.966
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5808
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0934
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w = 1/[\s^2^(Fo^2^)+(0.1389P)^2^+1.6175P] where P = (Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2393
_refine_ls_wR_factor_ref         0.2711
_reflns_number_gt                4177
_reflns_number_total             5808
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6113.cif
_cod_data_source_block           I
_cod_original_cell_volume        1317.9(10)
_cod_database_code               2201156
_cod_database_fobs_code          2201156