A synthetic model of the nonheme iron-superoxo intermediate of cysteine dioxygenase.
Fischer, Anne A.; Lindeman, Sergey V.; Fiedler, Adam T.; Chemical communications (Cambridge, England) 54 (2018) 11344–11347; doi:10.1039/c8cc06247a

data_7122370
_publ_section_title
;
 A synthetic model of the nonheme iron-superoxo intermediate of cysteine
 dioxygenase.
;
_journal_issue                   80
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11344
_journal_page_last               11347
_journal_paper_doi               10.1039/c8cc06247a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C21 H28 B Fe N7 S'
_chemical_formula_sum            'C21 H28 B Fe N7 S'
_chemical_formula_weight         477.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2018-06-26 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.19917(12)
_cell_length_b                   13.84434(12)
_cell_length_c                   21.58924(15)
_cell_measurement_reflns_used    18232
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.6710
_cell_measurement_theta_min      4.7490
_cell_volume                     4542.86(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -67.00  32.00   1.00    7.50    --  -42.33  37.00-120.00   99
  2  \w   -117.00 -18.00   1.00    7.50    --  -42.33 -37.00  60.00   99
  3  \w     23.00  98.00   1.00    7.50    --   42.33-125.00 -90.00   75
  4  \w     24.00 133.00   1.00   30.00    --  100.00 -77.00 -30.00  109
  5  \w     94.00 173.00   1.00   30.00    --  100.00 125.00   0.00   79
  6  \w     24.00 133.00   1.00   30.00    --  100.00 -77.00-180.00  109
  7  \w     94.00 173.00   1.00   30.00    --  100.00 125.00-120.00   79
  8  \w     74.00 173.00   1.00   30.00    --  100.00  45.00 -60.00   99
  9  \w     18.00 153.00   1.00   30.00    --  100.00 -15.00  90.00  135
 10  \w     18.00 153.00   1.00   30.00    --  100.00 -15.00 -90.00  135
 11  \w   -118.00 -10.00   1.00    7.50    --  -42.33 -77.00-150.00  108
 12  \w   -118.00 -10.00   1.00    7.50    --  -42.33 -77.00 -30.00  108
 13  \w      1.00  83.00   1.00    7.50    --   42.33 -99.00  60.00   82
 14  \w     71.00 105.00   1.00   30.00    --  100.00  61.00-180.00   34
 15  \w     71.00 172.00   1.00   30.00    --  100.00  61.00  90.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0450152000
_diffrn_orient_matrix_UB_12      0.0996874000
_diffrn_orient_matrix_UB_13      -0.0007597000
_diffrn_orient_matrix_UB_21      -0.0548664000
_diffrn_orient_matrix_UB_22      0.0287951000
_diffrn_orient_matrix_UB_23      -0.0570858000
_diffrn_orient_matrix_UB_31      -0.0723773000
_diffrn_orient_matrix_UB_32      0.0401548000
_diffrn_orient_matrix_UB_33      0.0428160000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39263
_diffrn_reflns_theta_full        70.49
_diffrn_reflns_theta_max         70.49
_diffrn_reflns_theta_min         4.10
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.362
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.040
_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     294
_refine_ls_number_reflns         4345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+2.0467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0643
_reflns_number_gt                4121
_reflns_number_total             4345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc06247a2.cif
_cod_data_source_block           complex1
_cod_depositor_comments          'Adding full bibliography for 7122370.cif.'
_cod_database_code               7122370
_chemical_oxdiff_formula         'C21 H28 B Fe N7 S'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C18(H18), C19(H19), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_olex2_date_sample_submission    2017-07-27
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.327
_oxdiff_exptl_absorpt_empirical_full_min 0.702