Synthesis, Characterization, and Reactivity of Ferrous and Ferric Oxo/Peroxo Pivalate Complexes in Relation to Gif-Type Oxygenation of Substrates
Remle Çelenligil-Çetin; Richard J. Staples; Pericles Stavropoulos; Inorganic Chemistry 39 (2000) 5838–5846; doi:10.1021/ic000261+

data_4327615
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of Ferrous and Ferric
 Oxo/Peroxo Pivalate Complexes in Relation to Gif-Type Oxygenation of
 Substrates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5838
_journal_page_last               5846
_journal_paper_doi               10.1021/ic000261+
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C38 H40 F30 Fe6 O33'
_chemical_formula_weight         1929.80
_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                75.731(2)
_cell_angle_beta                 87.745(2)
_cell_angle_gamma                61.218(1)
_cell_formula_units_Z            2
_cell_length_a                   13.1278(5)
_cell_length_b                   13.1794(5)
_cell_length_c                   25.0769(6)
_cell_measurement_reflns_used    143
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      19.47
_cell_measurement_theta_min      2.27
_cell_volume                     3669.3(2)
_computing_cell_refinement       'SMART (Bruker, V4.050, 1995)'
_computing_data_collection       'ASTRO (Bruker, V4.050, 1995)'
_computing_data_reduction        'SAINT (Bruker, V5.A06, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998, ver 5.10)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_method       '\w, 0.3 deg'
_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  0.1187
_diffrn_reflns_av_sigmaI/netI    0.2073
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15816
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  0.942203
_exptl_absorpt_correction_T_min  0.619958
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       plate
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         9574
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.2325
_refine_ls_R_factor_gt           0.1015
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1519P)^2^+9.3731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2435
_refine_ls_wR_factor_ref         0.3251
_reflns_number_gt                3942
_reflns_number_total             9574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0002612B_5.cif
_cod_data_source_block           compound_6
_cod_database_code               4327615