A sandwich-type aluminium complex composed of tri-lacunary Keggin-type polyoxotungstate: synthesis and X-ray crystal structure of [(A-PW9O34)2{W(OH)(OH2)}{Al(OH)(OH2)}{Al(μ-OH)(OH2)2}2]7-.
Kato, Chika Nozaki; Katayama, Yurika; Nagami, Masaru; Kato, Masao; Yamasaki, Mikio; Dalton transactions (Cambridge, England : 2003) 39 (2010) 11469–11474; doi:10.1039/c0dt00722f

data_7026808
_publ_section_title
;
 A sandwich-type aluminium complex composed of tri-lacunary Keggin-type
 polyoxotungstate: synthesis and X-ray crystal structure of
 [(A-PW9O34)2{W(OH)(OH2)}{Al(OH)(OH2)}{Al(\m-OH)(OH2)2}2]7-.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11469
_journal_page_last               11474
_journal_paper_doi               10.1039/c0dt00722f
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         '(H16 Al3 K6 Na O78 P2 W19), 18.75(H2 O)'
_chemical_formula_sum            'Al3 H53.5 K6 Na O96.75 P2 W19'
_chemical_formula_weight         5495.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                65.975(10)
_cell_angle_beta                 81.948(19)
_cell_angle_gamma                73.966(16)
_cell_formula_units_Z            2
_cell_length_a                   13.300(5)
_cell_length_b                   19.135(7)
_cell_length_c                   20.684(8)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     4619(3)
_computing_cell_refinement       'CrystalClear (Rigaku & RAC 2007)'
_computing_data_collection       'CrystalClear (Rigaku & RAC 2007)'
_computing_data_reduction        'CrystalStructure (Rigaku & RAC 2007)'
_computing_publication_material  'CrystalStructure (Rigaku & RAC 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      93.1
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55017
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.43
_exptl_absorpt_coefficient_mu    24.041
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.951
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4855.00
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         6.28
_refine_diff_density_min         -3.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     1223
_refine_ls_number_reflns         20298
_refine_ls_number_restraints     269
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0620P)^2^+94.2061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                15681
_reflns_number_total             20298
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c0dt00722f.txt
_cod_data_source_block           sc0410e
_cod_original_cell_volume        4618(3)
_cod_original_formula_sum        'H53.50 Al3 K6 Na O96.75 P2 W19 '
_cod_database_code               7026808