The True Nature of the Di-iron(III) γ-Keggin Structure in Water: Catalytic Aerobic Oxidation and Chemistry of an Unsymmetrical Trimer
Bogdan Botar; Yurii V. Geletii; Paul Kögerler; Djamaladdin G. Musaev; Keiji Morokuma; Ira A. Weinstock; Craig L. Hill; Journal of the American Chemical Society 128 (2006) 11268–11277; doi:10.1021/ja063157l

data_4110845
_publ_contact_author_address
;
Emory University
Department of Chemistry
Atlanta GA 30322-2210
USA
;
_publ_contact_author_email       bbotar@emory.edu
_publ_contact_author_fax         404-727-6076
_publ_contact_author_name        'Bogdan Botar'
_publ_contact_author_phone       404-727-4419
_publ_section_title
;
 The True Nature of the Di-iron(III) \g-Keggin Structure in Water:
 Catalytic Aerobic Oxidation and Chemistry of an Unsymmetrical Trimer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11268
_journal_page_last               11277
_journal_paper_doi               10.1021/ja063157l
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C16 H147 Fe6 K7 N8 O154 Si3 W30'
_chemical_formula_weight         9124.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 105.372(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   32.062(2)
_cell_length_b                   20.3625(14)
_cell_length_c                   12.7065(9)
_cell_measurement_reflns_used    7387
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.40
_cell_measurement_theta_min      2.22
_cell_volume                     7998.8(9)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0689
_diffrn_reflns_av_sigmaI/netI    0.1019
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            72436
_diffrn_reflns_theta_full        33.04
_diffrn_reflns_theta_max         33.04
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    22.320
_exptl_absorpt_correction_T_max  0.3478
_exptl_absorpt_correction_T_min  0.0890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10, Sheldrick 2003'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    3.789
_exptl_crystal_description       prism
_exptl_crystal_F_000             8164
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.602
_refine_diff_density_min         -2.983
_refine_diff_density_rms         0.440
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         28511
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0674
_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^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                22614
_reflns_number_total             28511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063157lsi20060511_053812.cif
_cod_data_source_block
K7[(CH3)2(NH2)]8[{Fe2(OH)3(H2O)2}3(SiW10O36)3]31H2O
_cod_original_cell_volume        7998.9(10)
_cod_database_code               4110845