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_4110846
_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            'Cl0.5 Fe4 H47 O99 Rb11.5 Si2 W20'
_chemical_formula_weight         6588.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.7770(10)
_cell_angle_beta                 101.797(2)
_cell_angle_gamma                94.181(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4883(8)
_cell_length_b                   18.7832(12)
_cell_length_c                   20.8326(13)
_cell_measurement_reflns_used    7495
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.21
_cell_volume                     4700.0(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      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49364
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    31.035
_exptl_absorpt_correction_T_max  0.3060
_exptl_absorpt_correction_T_min  0.0898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10, Sheldrick 2003'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    4.656
_exptl_crystal_description       plate
_exptl_crystal_F_000             5770
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.113
_refine_diff_density_min         -4.431
_refine_diff_density_rms         0.449
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1122
_refine_ls_number_reflns         23280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0368P)^2^+112.0488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                19077
_reflns_number_total             23280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063157lsi20060511_053904.cif
_cod_data_source_block           dimer
_cod_original_formula_sum        'H47 Cl0.50 Fe4 O99 Rb11.50 Si2 W20'
_cod_database_code               4110846