Fe(II) Complexes That Mimic the Active Site Structure of Acetylacetone Dioxygenase: O2 and NO Reactivity
Heaweon Park; Michael M. Bittner; Jacob S. Baus; Sergey V. Lindeman; Adam T. Fiedler; Inorganic Chemistry 51 (2012) 10279–10289; doi:10.1021/ic3012712

data_4330496
_publ_contact_author_name
;
;
_publ_section_title
;
 Fe(II) Complexes That Mimic the Active Site Structure of Acetylacetone
 Dioxygenase: O2 and NO Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10279
_journal_page_last               10289
_journal_paper_doi               10.1021/ic3012712
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'0.5(C116 H128 B4 Fe6 N24 O20), 1.49(C4 H6 N2)'
_chemical_formula_sum            'C63.96 H72.94 B2 Fe3 N14.98 O10'
_chemical_formula_weight         1400.78
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-11
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  Olex2 1.1-beta
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8198(10)
_cell_length_b                   22.6357(16)
_cell_length_c                   19.1610(10)
_cell_measurement_reflns_used    4277
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0111
_cell_measurement_theta_min      3.4057
_cell_volume                     6861.4(7)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
  1 omega  -49.00   -7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487   37.0000  -60.0000 42

  2 omega  -81.00   40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487   19.0000 -150.0000 121

  3 omega   63.00   90.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000  150.0000 27

  4 omega   32.00   86.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  150.0000 54

  5 omega  102.00  160.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   98.0000 -145.0000 58

  6 omega   39.00   94.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -90.0000 55

  7 omega   30.00   88.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000  -30.0000 58

  8 omega   42.00   94.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000   90.0000 52

  9 omega -115.00  -62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -57.0000 -120.0000 53

 10 omega -117.00  -14.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -37.0000  120.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0426956000
_diffrn_orient_matrix_UB_12      -0.0607129000
_diffrn_orient_matrix_UB_13      -0.0089184000
_diffrn_orient_matrix_UB_21      -0.0400755000
_diffrn_orient_matrix_UB_22      0.0210446000
_diffrn_orient_matrix_UB_23      -0.0689116000
_diffrn_orient_matrix_UB_31      0.0778123000
_diffrn_orient_matrix_UB_32      -0.0224688000
_diffrn_orient_matrix_UB_33      -0.0404303000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22926
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.18
_diffrn_reflns_theta_min         3.62
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    5.568
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       plate
_exptl_crystal_F_000             2918
_exptl_crystal_size_max          0.1452
_exptl_crystal_size_mid          0.0865
_exptl_crystal_size_min          0.0374
_refine_diff_density_max         2.137
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         6955
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0781
_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^)+(0.1247P)^2^+8.1178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2255
_reflns_number_gt                5088
_reflns_number_total             6955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3012712_si_002_5.cif
_cod_data_source_block           5acacPhF3
_cod_database_code               4330496
_chemical_oxdiff_formula         'Fe3 (C7 H5 O2)4 (C15 H22 N6 B)2 O2'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97