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_2012535
_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(C24 H20 As +)'
_chemical_formula_sum            'C54 H40 As2 S10 Zn'
_chemical_formula_weight         1224.67
_chemical_melting_point          .478E-305
_chemical_name_systematic
;
 Bis(tetraphenylarsonium) bis(1,3-dithiole-2-thione-4,5-dithiolato)zinc(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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.0720(10)
_cell_angle_beta                 85.8670(10)
_cell_angle_gamma                72.2590(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3451(5)
_cell_length_b                   15.0563(7)
_cell_length_c                   18.8083(8)
_cell_measurement_reflns_used    4866
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.26
_cell_volume                     2668.9(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_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      300(2)
_diffrn_measured_fraction_theta_full .995
_diffrn_measured_fraction_theta_max .995
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0282
_diffrn_reflns_av_sigmaI/netI    .0597
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16003
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.118
_exptl_absorpt_correction_T_max  .8620
_exptl_absorpt_correction_T_min  .7382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          .33
_exptl_crystal_size_mid          .21
_exptl_crystal_size_min          .15
_refine_diff_density_max         .357
_refine_diff_density_min         -.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .858
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         9377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .858
_refine_ls_R_factor_all          .0640
_refine_ls_R_factor_gt           .0335
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .0613
_refine_ls_wR_factor_ref         .0671
_reflns_number_gt                6069
_reflns_number_total             9377
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tr1005.cif
_cod_data_source_block           IX
_cod_database_code               2012535
_cod_database_fobs_code          2012535