Mono-substituted silicotungstates as active catalysts for sustainable oxidations: homo- and heterogeneous performance
Balula, Salete S.; Cunha-Silva, Luís; Santos, Isabel C. M. S.; Estrada, Ana C.; Fernandes, A. C.; Cavaleiro, José A. S.; Pires, João; Freire, Cristina; Cavaleiro, Ana M. V.; New Journal of Chemistry 37 (2013) 2341–; doi:10.1039/c3nj00243h

data_7053083
_publ_section_title
;
 Mono-substituted silicotungstates as active catalysts for sustainable
 oxidations: homo- and heterogeneous performance
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2341
_journal_paper_doi               10.1039/c3nj00243h
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'K4, H2, Si W11 Co H2 O40, 22(H20)'
_chemical_formula_sum            'Co H48 K4 O62 Si W11'
_chemical_formula_weight         3306.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           128
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2n'
_symmetry_space_group_name_H-M   'P 4/m n c'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '12 January 2012'
_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.1182(7)
_cell_length_b                   14.1182(7)
_cell_length_c                   12.4604(11)
_cell_measurement_reflns_used    3245
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.54
_cell_volume                     2483.7(3)
_computing_cell_refinement       'APEX2 '
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT+ (Bruker, 1997-2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL '
_computing_structure_refinement  'SHELXTL '
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11494
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         4.36
_exptl_absorpt_coefficient_mu    26.184
_exptl_absorpt_correction_T_max  0.0120
_exptl_absorpt_correction_T_min  0.0030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    4.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2950
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.557
_refine_diff_density_min         -3.960
_refine_diff_density_rms         0.368
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+97.3676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                1247
_reflns_number_total             1333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj00243h.txt
_cod_data_source_block           sb0310
_cod_database_code               7053083