Bis(tetrabutylammonium) bis(3,4,5-trioxocyclopent-1-ene-1,2-dithiolato-κ^2^<i>S</i>,<i>S</i>')cadmate(II) 0.25-hydrate
Chen, Hong-Yu; Xia, Guang-Ming; Zhang, Zhen-Wei; Li, Ping; Acta Crystallographica Section E 67 (2011) m12–m13; doi:10.1107/S1600536810049913

data_2228790
_publ_section_title
;
 Bis(tetrabutylammonium)
 bis(3,4,5-trioxocyclopent-1-ene-1,2-dithiolato-\k^2^<i>S</i>,<i>S</i>')cadmate(II)
 0.25-hydrate
;
_journal_coeditor_code           JJ2066
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m12
_journal_page_last               m13
_journal_paper_doi               10.1107/S1600536810049913
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C16 H36 N)2 [Cd (C5 O3 S2)2], 0.25H2 O'
_chemical_formula_moiety         '2(C16 H36 N +), C10 Cd O6 S4 2-, 0.25(H2 O)'
_chemical_formula_sum            'C42 H72.5 Cd N2 O6.25 S4'
_chemical_formula_weight         946.16
_chemical_name_systematic
;
Bis(tetrabutylammonium)
bis(3,4,5-trioxocyclopent-1-ene-1,2-dithiolato-
\k^2^<i>S</i>,<i>S</i>')cadmate(II) 0.25-hydrate
;
_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                74.853(5)
_cell_angle_beta                 86.898(5)
_cell_angle_gamma                87.705(5)
_cell_formula_units_Z            2
_cell_length_a                   9.820(5)
_cell_length_b                   15.002(5)
_cell_length_c                   17.406(5)
_cell_measurement_reflns_used    6268
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.49
_cell_volume                     2470.6(17)
_computing_cell_refinement
'<i>CrysAlis PRO</i> (Oxford Diffraction, 2007)'
_computing_data_collection
'<i>CrysAlis PRO</i> (Oxford Diffraction, 2007)'
_computing_data_reduction
'<i>CrysAlis RED</i> (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction 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     0.71069
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30150
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1001
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.419
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         10069
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.4766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1436
_reflns_number_gt                6510
_reflns_number_total             10069
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jj2066.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C42 H72.50 Cd N2 O6.25 S4'
_cod_database_code               2228790
_cod_database_fobs_code          2228790