A Synthetic Model of the Putative Fe(II)-Iminobenzosemiquinonate Intermediate in the Catalytic Cycle of o-Aminophenol Dioxygenases
Michael M. Bittner; Sergey V. Lindeman; Adam T. Fiedler; Journal of the American Chemical Society 134 (2012) 5460–5463; doi:10.1021/ja212163t

data_4117735
_publ_contact_author_name
;
;
_publ_section_title
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 A Synthetic Model of the Putative Fe(II)-Iminobenzosemiquinonate
 Intermediate in the Catalytic Cycle of o-Aminophenol Dioxygenases
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5460
_journal_page_last               5463
_journal_paper_doi               10.1021/ja212163t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'F6 Sb, C59 H55 B Fe N7 O, 0.5(C2 H4 Cl2)'
_chemical_formula_sum            'C60 H57 B Cl F6 Fe N7 O Sb'
_chemical_formula_weight         1229.99
_chemical_name_systematic
;
 ? 
;
_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             2011-09-21
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.218(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   39.2370(12)
_cell_length_b                   13.8346(4)
_cell_length_c                   20.7143(5)
_cell_measurement_reflns_used    11705
_cell_measurement_temperature    101.1
_cell_measurement_theta_max      73.7973
_cell_measurement_theta_min      3.3146
_cell_volume                     11155.2(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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      101.1
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
;
  1 omega -117.00  -14.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -37.0000  120.0000 206

  2 omega  -95.00  -12.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  125.0000 -150.0000 166

  3 omega  -65.00   -1.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487   37.0000   90.0000 128

  4 omega   38.00   67.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -90.0000 58

  5 omega  117.00  177.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000    0.0000 120

  6 omega   87.00  113.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -117.0000 -144.0000 52

  7 omega  101.00  165.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  117.0000  -35.0000 128

  8 omega   97.00  177.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000 -120.0000 160

  9 omega  138.00  175.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000  150.0000 74

 10 omega   32.00   66.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -60.0000 68

 11 omega   50.00   84.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -117.0000   56.0000 68

 12 omega   83.00  178.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000  -60.0000 190

 13 omega  -65.50   -7.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -77.0000  -60.0000 117

 14 omega -117.00  -14.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -37.0000   30.0000 206

 15 omega   23.00   98.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6487 -125.0000  150.0000 150

 16 omega   79.00  110.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000   60.0000 62
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0014440000
_diffrn_orient_matrix_UB_12      -0.0189098000
_diffrn_orient_matrix_UB_13      -0.0728557000
_diffrn_orient_matrix_UB_21      -0.0056687000
_diffrn_orient_matrix_UB_22      0.1083914000
_diffrn_orient_matrix_UB_23      -0.0143698000
_diffrn_orient_matrix_UB_31      0.0390800000
_diffrn_orient_matrix_UB_32      0.0164138000
_diffrn_orient_matrix_UB_33      0.0100400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.1358
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27278
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.51
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.936
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.203
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       plate
_exptl_crystal_F_000             5016
_exptl_crystal_size_max          0.4331
_exptl_crystal_size_mid          0.2883
_exptl_crystal_size_min          0.0256
_refine_diff_density_max         2.035
_refine_diff_density_min         -1.968
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1418
_refine_ls_number_reflns         27278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+40.6762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2331
_reflns_number_gt                20009
_reflns_number_total             27278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja212163t_si_001_3.cif
_cod_data_source_block           Complex3
_cod_database_code               4117735
_chemical_oxdiff_formula         'Fe C59 H55 N7 O B Sb F6 C H2 Cl'