Syntheses and Molecular Structures of Monomeric and Hydrogen-Bonded Dimeric Dawson-Type Trialuminum-Substituted Polyoxotungstates Derived under Acidic and Basic Conditions.
Kato, Chika Nozaki; Kashiwagi, Toshifumi; Unno, Wataru; Nakagawa, Miyuki; Uno, Hidemitsu; Inorganic chemistry 53 (2014) 4824–4832; doi:10.1021/ic402650g

data_4338237
_publ_section_title
;
 Syntheses and Molecular Structures of Monomeric and Hydrogen-Bonded
 Dimeric Dawson-Type Trialuminum-Substituted Polyoxotungstates Derived
 under Acidic and Basic Conditions.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4824
_journal_page_last               4832
_journal_paper_doi               10.1021/ic402650g
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'H15 Al3 Cs6 O65 P2 W15'
_chemical_formula_sum            'Al3 Cs6 H15 O65 P2 W15'
_chemical_formula_weight         4753.15
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.5841
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   12.7724(8)
_cell_length_b                   17.2403(13)
_cell_length_c                   15.1612(12)
_cell_measurement_reflns_used    8664
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      3.04
_cell_volume                     3332.0(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24848
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    29.233
_exptl_absorpt_correction_T_max  0.003
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4088.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         12.330
_refine_diff_density_min         -8.240
_refine_ls_extinction_coef       0.00020(11)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.927
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7434
_refine_ls_number_restraints     114
_refine_ls_R_factor_gt           0.1582
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.4692
_reflns_number_gt                6126
_reflns_number_total             7436
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic402650g_si_004.cif
_cod_data_source_block           MN-RT-111203a
_cod_depositor_comments
'Adding full bibliography for 4338236--4338237.cif.'
_cod_original_cell_volume        3332.0(5)
_cod_original_formula_sum        'H15 Al3 Cs6 O65 P2 W15'
_cod_database_code               4338237