Hexakis(dimethyl sulfoxide-κ<i>O</i>)calcium μ~6~-oxido-dodecakis-μ~2~-oxido-hexaoxidohexatungstate(VI)
Zhang, Jinfang; Acta Crystallographica Section E 68 (2012) m702–; doi:10.1107/S1600536812018338

data_2234797
_publ_section_title
;
 Hexakis(dimethyl sulfoxide-\k<i>O</i>)calcium
 \m~6~-oxido-dodecakis-\m~2~-oxido-hexaoxidohexatungstate(VI)
;
_journal_coeditor_code           RZ2743
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m702
_journal_paper_doi               10.1107/S1600536812018338
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ca (C2 H6 O S)6] [W6 O19]'
_chemical_formula_moiety         'C12 H36 Ca O6 S6 2+, O19 W6 2-'
_chemical_formula_sum            'C12 H36 Ca O25 S6 W6'
_chemical_formula_weight         1915.95
_chemical_name_systematic
;
Hexakis(dimethyl sulfoxide-\k<i>O</i>)calcium
\m~6~-oxido-dodecakis-\m~2~-oxido-hexaoxidohexatungstate(VI)
;
_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           'SHELXTL (Sheldrick, 2008)'
_cell_angle_alpha                84.53(3)
_cell_angle_beta                 73.15(3)
_cell_angle_gamma                74.02(3)
_cell_formula_units_Z            1
_cell_length_a                   8.1871(16)
_cell_length_b                   11.352(2)
_cell_length_c                   11.378(2)
_cell_measurement_reflns_used    4353
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9488
_cell_measurement_theta_min      3.6542
_cell_volume                     972.8(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8635
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.200
_exptl_absorpt_correction_T_max  0.094
_exptl_absorpt_correction_T_min  0.047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0465
_reflns_number_gt                3072
_reflns_number_total             3507
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rz2743.cif
_cod_data_source_block           I
_cod_original_cell_volume        972.8(3)
_cod_database_code               2234797
_cod_database_fobs_code          2234797