Synthesis, X-ray Structures, Electronic Properties, and O<sub>2</sub>/NO Reactivities of Thiol Dioxygenase Active-Site Models.
Fischer, Anne A.; Stracey, Nuru; Lindeman, Sergey V.; Brunold, Thomas C.; Fiedler, Adam T.; Inorganic chemistry 55 (2016) 11839–11853; doi:10.1021/acs.inorgchem.6b01931

data_4349131
_publ_section_title
;
 Synthesis, X-ray Structures, Electronic Properties, and O<sub>2</sub>/NO
 Reactivities of Thiol Dioxygenase Active-Site Models.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11839
_journal_page_last               11853
_journal_paper_doi               10.1021/acs.inorgchem.6b01931
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C50 H45 Fe N7 P S, C24 H20 B, C H2 Cl, C H4 O'
_chemical_formula_sum            'C76 H71 B Cl Fe N7 O P S'
_chemical_formula_weight         1263.54
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.0967(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.2143(3)
_cell_length_b                   21.0046(2)
_cell_length_c                   17.0445(2)
_cell_measurement_reflns_used    16474
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0790
_cell_measurement_theta_min      3.1650
_cell_volume                     6538.69(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.975
_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   -124.00 -79.00   1.00   10.00    --  -41.40 -99.00-180.00   45
  2  \w   -124.00 -79.00   1.00   10.00    --  -41.40 -99.00 150.00   45
  3  \w   -120.00  -8.00   1.00   10.00    --  -41.40 -77.00  90.00  112
  4  \w    -96.00  -2.00   1.00   10.00    --  -41.40 125.00-180.00   94
  5  \w     81.00 178.00   1.00   30.00    --  108.29  45.00 120.00   97
  6  \w     94.00 178.00   1.00   30.00    --  108.29 125.00  30.00   84
  7  \w     34.00 139.00   1.00   30.00    --  108.29 -61.00  60.00  105
  8  \w     33.00 103.00   1.00   30.00    --  108.29-125.00   0.00   70
  9  \w     75.00 178.00   1.00   30.00    --  108.29  77.00-180.00  103
 10  \w     78.00 178.00   1.00   30.00    --  108.29  30.00 -60.00  100
 11  \w    -36.00 -12.00   1.00   10.00    --  -41.40 -57.00-180.00   24
 12  \w   -115.00 -12.00   1.00   10.00    --  -41.40 -57.00 -30.00  103
 13  \w    -46.00  -8.00   1.00   10.00    --  -41.40 -77.00 -90.00   38
 14  \w     75.00 178.00   1.00   30.00    --  108.29  77.00 150.00  103
 15  \w     81.00 178.00   1.00   30.00    --  108.29  45.00-120.00   97
 16  \w     94.00 178.00   1.00   30.00    --  108.29 125.00 -30.00   84
 17  \w     78.00 145.00   1.00   30.00    --  108.29  61.00  60.00   67
 18  \w     78.00 108.00   1.00   30.00    --  108.29  30.00  30.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0627732000
_diffrn_orient_matrix_UB_12      -0.0462991000
_diffrn_orient_matrix_UB_13      -0.0022144000
_diffrn_orient_matrix_UB_21      -0.0551318000
_diffrn_orient_matrix_UB_22      0.0454645000
_diffrn_orient_matrix_UB_23      -0.0585850000
_diffrn_orient_matrix_UB_31      0.0117772000
_diffrn_orient_matrix_UB_32      -0.0341770000
_diffrn_orient_matrix_UB_33      -0.0748225000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53840
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.77
_diffrn_reflns_theta_min         3.21
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.30a (Agilent, 2015)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         13090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0493P)^2^+1.6871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                10899
_reflns_number_total             13090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01931_si_002.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        6538.68(14)
_cod_database_code               4349131
_chemical_oxdiff_formula
'Fe C50 H45 N7 O2 S P B C24 H20 C2 H4 O C H2 Cl'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 N7(H7A,H7B), C49(H49A,H49B), C50(H50A,H50B), C76(H76A,H76B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45),
  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59),
 C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68),
  C70(H70), C71(H71), C72(H72), C73(H73), C74(H74)
2.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C75(H75A,H75B,
 H75C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_date_sample_submission    2015-04-16
_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 1.487
_oxdiff_exptl_absorpt_empirical_full_min 0.582