Formation, Isomerization, and Derivatization of Keggin Tungstoaluminates
Jennifer J. Cowan; Alan J. Bailey; Robert A. Heintz; Bao T. Do; Kenneth I. Hardcastle; Craig L. Hill; Ira A. Weinstock; Inorganic Chemistry 40 (2001) 6666–6675; doi:10.1021/ic0106120

data_4320707
_publ_contact_author_address
;
Emory University
Department of Chemistry
X-ray Crystallography Laboratory
Atlanta GA 30322-2210
USA
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_publ_contact_author_email       khardca@emory.edu
_publ_contact_author_fax         404-727-6586
_publ_contact_author_phone       404-727-6140
_publ_section_title
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 Formation, Isomerization, and Derivatization of Keggin Tungstoaluminates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6666
_journal_page_last               6675
_journal_paper_doi               10.1021/ic0106120
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'Al2 Co3 H54 K12 O108 W22'
_chemical_formula_weight         6527.08
_chemical_name_systematic
;
  ?
;
_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                90.024(2)
_cell_angle_beta                 60.011(2)
_cell_angle_gamma                60.039(2)
_cell_formula_units_Z            1
_cell_length_a                   15.6315(16)
_cell_length_b                   15.6328(16)
_cell_length_c                   15.6522(16)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.224
_cell_measurement_theta_min      2.603
_cell_volume                     2706.0(5)
_computing_cell_refinement       'Bruker SAINT'
_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 0.884
_diffrn_measured_fraction_theta_max 0.884
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.1050
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24877
_diffrn_reflns_theta_full        32.58
_diffrn_reflns_theta_max         32.58
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    24.310
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.381837
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2881
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.448
_refine_diff_density_min         -4.573
_refine_diff_density_rms         0.568
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         17419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                10628
_reflns_number_total             17419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0106120_1.cif
_cod_data_source_block           jc5247s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        'H54 Al2 Co3 K12 O108 W22'
_cod_database_code               4320707