Crystal Structure of Benzyldimethyl(ω-cyclohexylethyl)ammonium Bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
KAKIHARA, Shunta; SAEKI, Masahiro; ICHIMURA, Shuhei; TAMAKI, Yoshinori; MIYAMURA, Kazuo; X-ray Structure Analysis Online 33 (2017) 15–; doi:10.2116/xraystruct.33.15

data_1551596
_publ_section_title
;
 Crystal Structure of Benzyldimethyl(\w-cyclohexylethyl)ammonium
 Bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              15
_journal_paper_doi               10.2116/xraystruct.33.15
_journal_volume                  33
_journal_year                    2017
_chemical_formula_moiety         'C17 H28 N +, C6 Ni S10 -'
_chemical_formula_sum            'C23 H28 N Ni S10'
_chemical_formula_weight         697.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9129(11)
_cell_length_b                   17.270(3)
_cell_length_c                   21.673(3)
_cell_measurement_reflns_used    2695
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      22.53
_cell_measurement_theta_min      2.74
_cell_volume                     2961.7(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'BrukerAXS CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.1300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18100
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.258
_diffrn_reflns_theta_min         1.508
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  0.9098
_exptl_absorpt_correction_T_min  0.6090
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
XPREP; Bruker AXS 2000
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 1364 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.821
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0097P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.717
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                4649
_reflns_number_total             6708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            33_15_1.txt
_cod_data_source_block           BnC2cHx
_cod_original_cell_volume        2961.8(7)
_cod_database_code               1551596
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.609
_shelx_estimated_absorpt_t_max   0.910
_shelx_res_checksum              29095
_shelx_hkl_checksum              74617
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n