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_4117734
_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 H55 B Fe N7 O, C0.94 Cl1.24, 0.57(C H2 Cl2), 0.26(C)'
_chemical_formula_sum            'C60.77 H56.15 B Cl2.39 Fe N7 O'
_chemical_formula_weight         1051.86
_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                 92.617(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9365(6)
_cell_length_b                   9.9321(5)
_cell_length_c                   37.6317(14)
_cell_measurement_reflns_used    8058
_cell_measurement_temperature    100.6
_cell_measurement_theta_max      73.8617
_cell_measurement_theta_min      3.2324
_cell_volume                     5576.9(4)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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
;
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      100.6
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega  -67.00  -39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487   37.0000  120.0000 28

  2 omega -112.00  -11.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -55.0000  -63.0000 101

  3 omega    6.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487   37.0000  120.0000 25

  4 omega  -67.00   29.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487   37.0000 -120.0000 96

  5 omega  119.00  164.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000  -30.0000 45

  6 omega   44.00   73.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000 -180.0000 29

  7 omega   44.00   76.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  120.0000 32

  8 omega   32.00   71.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -30.0000 39

  9 omega   39.00   65.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000   30.0000 26

 10 omega  112.00  170.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000 -180.0000 58

 11 omega   73.00  177.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   77.0000  -90.0000 104

 12 omega   74.00  176.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   15.0000 -150.0000 102

 13 omega   14.00  117.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6487   37.0000  150.0000 103

 14 omega    7.00  119.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6487   77.0000 -150.0000 112

 15 omega   23.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6487 -125.0000    0.0000 75

 16 omega   76.00  152.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   67.0000   77.0000 76
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0015121000
_diffrn_orient_matrix_UB_12      0.1164039000
_diffrn_orient_matrix_UB_13      -0.0269924000
_diffrn_orient_matrix_UB_21      -0.1011416000
_diffrn_orient_matrix_UB_22      0.0222879000
_diffrn_orient_matrix_UB_23      0.0040182000
_diffrn_orient_matrix_UB_31      0.0208673000
_diffrn_orient_matrix_UB_32      0.0999631000
_diffrn_orient_matrix_UB_33      0.0305678000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            30976
_diffrn_reflns_theta_full        74.03
_diffrn_reflns_theta_max         74.03
_diffrn_reflns_theta_min         3.70
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.583
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.255
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       plate
_exptl_crystal_F_000             2198
_exptl_crystal_size_max          0.5621
_exptl_crystal_size_mid          0.1825
_exptl_crystal_size_min          0.0604
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         11016
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0662P)^2^+2.1017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1382
_reflns_number_gt                9021
_reflns_number_total             11016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja212163t_si_001_2.cif
_cod_data_source_block           Complex2
_cod_database_code               4117734
_chemical_oxdiff_formula         'Fe C60 H58 N7 O B Cl2'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97