Stability and Structure in α- and β-Keggin Heteropolytungstates, [Xn+W12O40](8-n)-, X = p-Block Cation
Wade A. Neiwert; Jennifer J. Cowan; Kenneth I. Hardcastle; Craig L. Hill; Ira A. Weinstock; Inorganic Chemistry 41 (2002) 6950–6952; doi:10.1021/ic026023r

data_4319094
_publ_contact_author_address
;
Emory University
Department of Chemistry
X-ray Crystallography Laboratory
Atlanta GA 30322-2210
USA
;
_publ_contact_author_email       khardca@emory.edu
_publ_contact_author_fax         404-727-6586
_publ_contact_author_name        'Kenneth I. Hardcastle'
_publ_contact_author_phone       404-727-6140
_publ_section_title
;
 Stability and Structure in \a- and \b-Keggin Heteropolytungstates,
 [Xn+W12O40](8-n)-, X = p-Block Cation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6950
_journal_page_last               6952
_journal_paper_doi               10.1021/ic026023r
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         beta-Cs3.5K1.5[AlW12O40]
_chemical_formula_sum            'Al Cs3.5 K1.5 O44.95 W12'
_chemical_formula_weight         3476.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   17.4163(8)
_cell_length_b                   17.4163(8)
_cell_length_c                   47.663(5)
_cell_measurement_reflns_used    7765
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.70
_cell_measurement_theta_min      2.34
_cell_volume                     12520.6(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1047
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            63716
_diffrn_reflns_theta_full        33.08
_diffrn_reflns_theta_max         33.08
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    36.219
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.346362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             17779
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_refine_diff_density_max         8.302
_refine_diff_density_min         -9.085
_refine_diff_density_rms         0.928
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         4999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0865
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+7000.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2202
_refine_ls_wR_factor_ref         0.2269
_reflns_number_gt                4222
_reflns_number_total             4999
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026023r_s2_2.cif
_cod_data_source_block           beta-Cs3.5K1.5[AlW12O40].5H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        12520.5(14)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'Al Cs3.50 K1.50 O44.95 W12'
_cod_database_code               4319094