A low-temperature phase of bis(tetrabutylammonium) octa-μ~3~-chlorido-hexachlorido-<i>octahedro</i>-hexatungstate
Johnston, Dean H.; Brown, Chris M.; Yu, Andrew S.; Gallucci, Judith C.; Acta Crystallographica Section C 66 (2010) m303–m306; doi:10.1107/S0108270110037017

data_2017853
_publ_section_title
;
 A low-temperature phase of bis(tetrabutylammonium)
 octa-\m~3~-chlorido-hexachlorido-<i>octahedro</i>-hexatungstate
;
_journal_coeditor_code           MX3029
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m303
_journal_page_last               m306
_journal_paper_doi               10.1107/S0108270110037017
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C16 H36 N)2 [W6 Cl14]'
_chemical_formula_moiety         '2(C16 H36 N +), Cl14 W6 2-'
_chemical_formula_sum            'C32 H72 Cl14 N2 W6'
_chemical_formula_weight         2084.32
_chemical_name_common            'tungsten chloride cluster'
_chemical_name_systematic
;
bis(tetrabutylammonium)
octa-\m~3~-chlorido-hexachlorido-<i>octahedro</i>-hexatungstate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 112.4150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3152(2)
_cell_length_b                   11.72200(10)
_cell_length_c                   22.27860(10)
_cell_measurement_reflns_used    12939
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_volume                     5387.31(8)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997),
Mercury (Macrae <i>et al.</i>, 2008), POV-RAY (Cason, 2004)
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            137050
_diffrn_reflns_reduction_process
;
Scaled and merged with SADABS and XPREP (Bruker, 2008)
;
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    13.479
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.57
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.198
_refine_diff_density_min         -1.691
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         12352
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.5516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                9499
_reflns_number_total             12352
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            mx3029.cif
_cod_data_source_block           I_150K
_cod_original_cell_volume        5387.31(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017853
_cod_database_fobs_code          2017853