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_4117733
_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         'C59 H56 B Fe N7 O, C H2 Cl, C2 H3 N'
_chemical_formula_sum            'C62 H61 B Cl Fe N8 O'
_chemical_formula_weight         1036.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-09-21
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  Olex2 1.1
  (compiled 2011.09.07 svn.r1971, GUI svn.r3853)
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_cell_angle_alpha                90.00
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_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0304(2)
_cell_length_b                   32.0673(6)
_cell_length_c                   17.1467(3)
_cell_measurement_reflns_used    19866
_cell_measurement_temperature    100.9
_cell_measurement_theta_max      29.5188
_cell_measurement_theta_min      3.3753
_cell_volume                     5465.73(18)
_computing_cell_refinement
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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)
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_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)
;
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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)
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      374.05
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_details
;
  1 omega  -83.00   11.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  -37.0000   60.0000 188

  2 omega  -48.00   64.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8259    0.0000  -90.0000 224

  3 omega  -67.00  -40.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -77.0000  -30.0000 54

  4 omega  -88.00   14.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  -37.0000 -120.0000 204

  5 omega  -28.00   64.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8259   37.0000   60.0000 184
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0231799000
_diffrn_orient_matrix_UB_12      0.0003444000
_diffrn_orient_matrix_UB_13      -0.0372948000
_diffrn_orient_matrix_UB_21      0.0370959000
_diffrn_orient_matrix_UB_22      0.0184163000
_diffrn_orient_matrix_UB_23      0.0108466000
_diffrn_orient_matrix_UB_31      0.0563786000
_diffrn_orient_matrix_UB_32      -0.0122545000
_diffrn_orient_matrix_UB_33      0.0152637000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60411
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.58
_diffrn_reflns_theta_min         3.38
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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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)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.4241
_exptl_crystal_size_mid          0.2992
_exptl_crystal_size_min          0.1894
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         13966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+3.9221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                11810
_reflns_number_total             13966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja212163t_si_001_1.cif
_cod_data_source_block           Complex1
_cod_original_cell_volume        5465.76(19)
_cod_database_code               4117733
_chemical_oxdiff_formula         'C61 H59 N7 O B Fe Cl2'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32