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_4319093
_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-Cs4.5K0.5[AlW12O40]
_chemical_formula_sum            'Al Cs4.5 K0.5 O47.5 W12'
_chemical_formula_weight         3610.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           26
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2'
_symmetry_space_group_name_H-M   'P m c 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0441(10)
_cell_length_b                   13.2270(8)
_cell_length_c                   20.5919(13)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.74
_cell_measurement_theta_min      2.23
_cell_volume                     4369.9(5)
_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 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            76106
_diffrn_reflns_theta_full        33.03
_diffrn_reflns_theta_max         33.03
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    35.324
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.482561
_exptl_absorpt_correction_type   'multi-scan and face-indexing'
_exptl_absorpt_process_details   'SADABS, Sheldrick; XPREP'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6152
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         11.063
_refine_diff_density_min         -11.458
_refine_diff_density_rms         0.658
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.193(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         16190
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+403.5270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                15546
_reflns_number_total             16190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026023r_s2_1.cif
_cod_data_source_block           beta-Cs4.5K0.5[AlW12O40]7.5H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_formula_sum        'Al Cs4.50 K0.50 O47.50 W12'
_cod_database_code               4319093