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_4327614
_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            'C71.5 H121 Fe6 N2 O28.5'
_chemical_formula_weight         1799.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.235(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.9379(5)
_cell_length_b                   18.7231(7)
_cell_length_c                   23.721(1)
_cell_measurement_reflns_used    122
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      15.12
_cell_measurement_theta_min      2.38
_cell_volume                     9617.0(6)
_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, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1360
_diffrn_reflns_av_sigmaI/netI    0.1527
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45592
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.39
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.9444
_exptl_absorpt_correction_T_min  0.8231
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       needle
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.171
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         12566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.1783
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2426
_reflns_number_gt                6107
_reflns_number_total             12566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0002612B_4.cif
_cod_data_source_block           compound_5
_cod_original_cell_volume        9617.1(6)
_cod_original_formula_sum        'C71.50 H121 Fe6 N2 O28.50'
_cod_database_code               4327614