Ionic Crystals [M3O(OOCC6H5)6(H2O)3]4[α-SiW12O40] (M = Cr, Fe) as Heterogeneous Catalysts for Pinacol Rearrangement
Sayaka Uchida; Aldes Lesbani; Yoshiyuki Ogasawara; Noritaka Mizuno; Inorganic Chemistry 51 (2012) 775–777; doi:10.1021/ic2025186

data_4328074
_publ_section_title
;
 Ionic Crystals [M3O(OOCC6H5)6(H2O)3]4[\a-SiW12O40] (M = Cr, Fe) as
 Heterogeneous Catalysts for Pinacol Rearrangement
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              775
_journal_page_last               777
_journal_paper_doi               10.1021/ic2025186
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C168 Fe12 O104 Si W12'
_chemical_formula_sum            'C168 Fe12 O104 Si W12'
_chemical_formula_weight         6586.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 116.7664(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   22.4142(2)
_cell_length_b                   33.2833(4)
_cell_length_c                   22.9409(3)
_cell_measurement_temperature    183(1)
_cell_volume                     15280.5(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_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      183(1)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41533
_diffrn_reflns_theta_full        29.64
_diffrn_reflns_theta_max         29.64
_exptl_absorpt_coefficient_mu    5.118
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       plate
_exptl_crystal_F_000             6108.00
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         4.380
_refine_diff_density_min         -5.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_number_parameters     667
_refine_ls_number_reflns         41533
_refine_ls_number_restraints     11
_refine_ls_R_factor_gt           0.1191
_refine_ls_shift/su_max          0.001
_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         0.3733
_reflns_number_gt                20891
_reflns_number_total             41533
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic2025186_si_001_2.cif
_cod_data_source_block           2a.inf
_cod_database_code               4328074