Voltammetric and Spectroscopic Studies of α- and β-[PW12O40](3-) Polyoxometalates in Neutral and Acidic Media: Structural Characterization as Their [(n-Bu4N)3][PW12O40] Salts.
Ueda, Tadaharu; Kodani, Keisuke; Ota, Hiromi; Shiro, Motoo; Guo, Si-Xuan; Boas, John F.; Bond, Alan M.; Inorganic chemistry 56 (2017) 3990–4001; doi:10.1021/acs.inorgchem.6b03046

data_4345619
_publ_section_title
;
 Voltammetric and Spectroscopic Studies of \a- and \b-[PW12O40](3-)
 Polyoxometalates in Neutral and Acidic Media: Structural Characterization
 as Their [(n-Bu4N)3][PW12O40] Salts.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3990
_journal_page_last               4001
_journal_paper_doi               10.1021/acs.inorgchem.6b03046
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'O40 P W12, 3(C16 H36 N)'
_chemical_formula_sum            'C48 H108 N3 O40 P W12'
_chemical_formula_weight         3604.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                95.385(3)
_cell_angle_beta                 93.074(3)
_cell_angle_gamma                90.727(3)
_cell_formula_units_Z            2
_cell_length_a                   13.7108(19)
_cell_length_b                   15.384(2)
_cell_length_c                   19.356(3)
_cell_measurement_reflns_used    12427
_cell_measurement_temperature    173
_cell_measurement_theta_max      31.20
_cell_measurement_theta_min      1.80
_cell_volume                     4058.2(10)
_computing_cell_refinement       'CrystalClear (Rigaku, 2010)'
_computing_data_collection       'CrystalClear (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear (Rigaku, 2010)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku, 2000-2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 28.626
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53421
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        25.680
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.520
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.052
_exptl_absorpt_correction_T_max  0.188
_exptl_absorpt_correction_T_min  0.126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3280.00
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.098
_refine_diff_density_max         7.66
_refine_diff_density_min         -3.91
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     961
_refine_ls_number_reflns         15263
_refine_ls_number_restraints     3237
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0922P)^2^+198.7023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1970
_refine_ls_wR_factor_ref         0.2078
_reflns_number_gt                12039
_reflns_number_total             15263
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic6b03046_si_002.cif
_cod_data_source_block           RGK1875ccdlt
_cod_database_code               4345619
_verf_plat201_alert_2_a
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s)   .......   16 Report
RESPONSE: Disordered C atoms of tetrabutylammonium ion are heavily
          superimposed. See _publ_section_exptl_refinement.
;