Bis(tetra-<i>n</i>-butylammonium) (a redetermination at 150K) and bis(tetraphenylarsonium) bis(1,3-dithiole-2-thione-4,5-dithiolato)zinc(II) (at 300K)
Comerlato, Nadia M.; Harrison, William T.A.; Howie, R. Alan; Low, John Nicolson; Silvino, Alexandre C.; Wardell, James L.; Wardell, Solange M.S.V.; Acta Crystallographica Section C 58 (2002) m105–m108; doi:10.1107/S0108270101018534

data_2012534
_publ_section_title
;
 Bis(tetra-<i>n</i>-butylammonium) (a redetermination at 150K) and
 bis(tetraphenylarsonium)
 bis(1,3-dithiole-2-thione-4,5-dithiolato)zinc(II) (at 300K)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m105
_journal_page_last               m108
_journal_paper_doi               10.1107/S0108270101018534
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         '(C6 S10 Zn 2-), 2(C16 H36 N +)'
_chemical_formula_sum            'C38 H72 N2 S10 Zn'
_chemical_formula_weight         942.95
_chemical_melting_point          .436E-305
_chemical_name_systematic
;
 Bis(tetra-n-butylammonium)
bis(1,3-dithiole-2-thione-4,5-dithiolato)zinc(II)
 at 150K
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.9544(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.2564(3)
_cell_length_b                   8.9478(2)
_cell_length_c                   29.2379(5)
_cell_measurement_reflns_used    22851
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      3.23
_cell_volume                     5031.06(16)
_computing_cell_refinement       'DENZO and COLLECT'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full .493
_diffrn_measured_fraction_theta_max .428
_diffrn_measurement_device_type  'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0612
_diffrn_reflns_av_sigmaI/netI    .0791
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            22851
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .930
_exptl_absorpt_correction_T_max  .859
_exptl_absorpt_correction_T_min  .770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .10
_refine_diff_density_max         .229
_refine_diff_density_min         -.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5525
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          .1461
_refine_ls_R_factor_gt           .0489
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1084
_refine_ls_wR_factor_ref         .1322
_reflns_number_gt                2563
_reflns_number_total             5525
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tr1005.cif
_cod_data_source_block           IV150
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2012534
_cod_database_fobs_code          2012534