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_4330494
_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         'C58 H49 B Fe N6 O4, C2 H3 N'
_chemical_formula_sum            'C60 H52 B Fe N7 O4'
_chemical_formula_weight         1001.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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_date             2012-06-08
_audit_creation_method
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  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
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_cell_angle_alpha                90.00
_cell_angle_beta                 104.121(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.1369(8)
_cell_length_b                   13.5597(3)
_cell_length_c                   20.5303(4)
_cell_measurement_reflns_used    25638
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8989
_cell_measurement_theta_min      3.2569
_cell_volume                     10295.9(4)
_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)
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_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)
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_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)
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_computing_molecular_graphics
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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
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olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_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 0.991
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega  -28.00   24.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737   37.0000  120.0000 52

  2 omega  -44.00   29.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737   37.0000    0.0000 73

  3 omega  -38.00   33.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737   37.0000   60.0000 71

  4 omega   62.00   98.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7737 -125.0000   30.0000 36

  5 omega   73.00  108.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -94.0000  -30.0000 35

  6 omega   39.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000   60.0000 51

  7 omega  132.00  171.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000 -120.0000 39

  8 omega   95.00  177.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000   60.0000 82

  9 omega   54.00   95.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -90.0000 41

 10 omega   32.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000  120.0000 58

 11 omega  140.00  165.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  159.0000 -174.0000 25

 12 omega   37.00   71.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000   30.0000 34

 13 omega   29.00   88.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000 -180.0000 59

 14 omega   42.00   97.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -94.0000 -180.0000 55

 15 omega -115.00  -11.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737  -57.0000  -30.0000 104

 16 omega -115.00  -11.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737  -57.0000 -150.0000 104

 17 omega -117.00  -55.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737 -152.0000   79.0000 62

 18 omega -115.00  -11.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737  -57.0000   90.0000 104

 19 omega   46.00  119.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   15.0000  120.0000 73

 20 omega   77.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   30.0000 -150.0000 101
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0080355000
_diffrn_orient_matrix_UB_12      0.1107211000
_diffrn_orient_matrix_UB_13      0.0124392000
_diffrn_orient_matrix_UB_21      -0.0406003000
_diffrn_orient_matrix_UB_22      0.0201670000
_diffrn_orient_matrix_UB_23      -0.0082717000
_diffrn_orient_matrix_UB_31      0.0045779000
_diffrn_orient_matrix_UB_32      -0.0160970000
_diffrn_orient_matrix_UB_33      0.0758807000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            72082
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.06
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    2.789
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.456
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.5011
_exptl_crystal_size_mid          0.2887
_exptl_crystal_size_min          0.0559
_refine_diff_density_max         1.007
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1321
_refine_ls_number_reflns         20374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+10.0109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1430
_reflns_number_gt                18607
_reflns_number_total             20374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3012712_si_002_3.cif
_cod_data_source_block           2acacPhmal
_cod_database_code               4330494
_chemical_oxdiff_formula         'Fe C58 H49 B N6 O4'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97