New Ionic Crystals of Oppositely Charged Cluster Ions and Their Characterization
Jung Ho Son; Young-Uk Kwon; Oc Hee Han; Inorganic Chemistry 42 (2003) 4153–4159; doi:10.1021/ic0340377

data_4313825
_publ_section_title
;
 New Ionic Crystals of Oppositely Charged Cluster Ions and Their
 Characterization
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4153
_journal_page_last               4159
_journal_paper_doi               10.1021/ic0340377
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '[W2Al28O18(OH)48(H2O)24][H2W12O40]2.55H2O'
_chemical_formula_sum            'Al14 O112.83 W13'
_chemical_formula_weight         4573.01
_chemical_name_common            W2Al28-2W12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.019(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9154(13)
_cell_length_b                   16.2032(12)
_cell_length_c                   44.491(4)
_cell_measurement_temperature    293(2)
_cell_volume                     11361.2(16)
_computing_cell_refinement       'SMART (Bruker AXS, Inc., 1998)'
_computing_data_collection       'SMART (Bruker AXS, Inc., 1998)'
_computing_data_reduction        'SAINT (Bruker AXS, Inc., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Siemens 1K CCD'
_diffrn_measurement_method       'Omega scan'
_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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.1274
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            72425
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    13.332
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, G. M. 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             8186
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.421
_refine_diff_density_min         -3.781
_refine_diff_density_rms         0.401
_refine_ls_extinction_coef       0.000108(7)
_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_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         26316
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          13.222
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                14038
_reflns_number_total             26316
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0340377si20030115_032525_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_original_cell_volume        11361.1(16)
_cod_database_code               4313825