Equilibria between α and β Isomers of Keggin Heteropolytungstates
Ira A. Weinstock; Jennifer J. Cowan; Elena M. G. Barbuzzi; Huadong Zeng; Craig L. Hill; Journal of the American Chemical Society 121 (1999) 4608–4617; doi:10.1021/ja982908j

data_4116390
_publ_contact_author
;
    Ira A. Weinstock
    Department of Chemistry
    Emory University
    Atlanta, GA 30033
    Permanent address: 
    US Forest Service
    Forest Products Laboratory
    Madison, WI 53705
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_publ_contact_author_email       iaweinst@facstaff.wisc.edu
_publ_contact_author_fax         '404 727 6076'
_publ_contact_author_phone       '404 727 7699'
_publ_section_title
;
 Equilibria between \a and \b Isomers of Keggin Heteropolytungstates
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4608
_journal_page_last               4617
_journal_paper_doi               10.1021/ja982908j
_journal_volume                  121
_journal_year                    1999
_chemical_formula_analytical     K5AlW12O40.17H2O
_chemical_formula_structural     K5AlW12O40.17H2O
_chemical_formula_sum            'Al K5 O57 W12'
_chemical_formula_weight         3373.94
_chemical_name_common            keggin
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           180
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 62 2 (0 0 4)'
_symmetry_space_group_name_H-M   'P 62 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   19.07200(10)
_cell_length_b                   19.07200(10)
_cell_length_c                   12.5658(2)
_cell_measurement_reflns_used    45
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68
_cell_measurement_theta_min      4
_cell_volume                     3958.34(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_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  0.1022
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25389
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    26.568
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.246
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       rod
_exptl_crystal_F_000             4455
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.849
_refine_diff_density_min         -2.427
_refine_diff_density_rms         0.450
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       0.00046(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         3272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/esd_mean        0.104
_refine_ls_shift/su_max          2.608
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0745
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                2753
_reflns_number_total             3274
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982908j.cif
_cod_data_source_block           hill16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116390