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_4338236
_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         'Al3 H7 O62 P2 W15, 7(C4 H12 N), Na'
_chemical_formula_sum            'C28 H91 Al3 N7 Na O62 P2 W15'
_chemical_formula_weight         4441.67
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 114.237(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   58.56(3)
_cell_length_b                   14.871(7)
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_cell_measurement_reflns_used    16654
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.20
_cell_measurement_theta_min      6.78
_cell_volume                     20439(18)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
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_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       76
_diffrn_reflns_limit_h_min       -76
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            200732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.421
_exptl_absorpt_coefficient_mu    16.974
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.625
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_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             15952.00
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_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
;
_refine_diff_density_max         4.190
_refine_diff_density_min         -3.020
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_refine_ls_number_reflns         23451
_refine_ls_number_restraints     2010
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0921
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0504P)^2^+1915.5951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic402650g_si_003.cif
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_cod_depositor_comments
'Adding full bibliography for 4338236--4338237.cif.'
_cod_original_cell_volume        20439(17)
_cod_database_code               4338236
_shelxl_version_number           2013-2
_shelx_res_checksum              95900