[(FeIII(OH2)2)3(A-α-PW9O34)2]9- on Cationic Silica Nanoparticles, a New Type of Material and Efficient Heterogeneous Catalyst for Aerobic Oxidations
Nelya M. Okun; Travis M. Anderson; Craig L. Hill; Journal of the American Chemical Society 125 (2003) 3194–3195; doi:10.1021/ja0267223

data_4113557
_publ_section_title
;
 [(FeIII(OH2)2)3(A-\a-PW9O34)2]9- on Cationic Silica Nanoparticles, a New
 Type of Material and Efficient Heterogeneous Catalyst for Aerobic
 Oxidations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3194
_journal_page_last               3195
_journal_paper_doi               10.1021/ja0267223
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'Fe3 K9 Na0 O94.5 P2 W18'
_chemical_formula_weight         5402.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   40.376(4)
_cell_length_b                   27.904(2)
_cell_length_c                   31.186(2)
_cell_measurement_reflns_used    8973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.053
_cell_measurement_theta_min      2.613
_cell_volume                     35136(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            154772
_diffrn_reflns_theta_full        33.11
_diffrn_reflns_theta_max         33.11
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    24.527
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.32556
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light yello'
_exptl_crystal_density_diffrn    4.085
_exptl_crystal_density_meas      0
_exptl_crystal_description       irregular
_exptl_crystal_F_000             37872
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         8.618
_refine_diff_density_min         -2.432
_refine_diff_density_rms         0.486
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.372(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         31831
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+2908.7842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                30944
_reflns_number_total             31831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0267223si20030124_032045.cif
_cod_data_source_block           fdd2
_cod_original_formula_sum        'Fe3 K9 Na0 O94.50 P2 W18'
_cod_database_code               4113557