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_4349130
_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         'C52 H47 Fe N7 O2 P S, C24 H20 B, C H4 O'
_chemical_formula_sum            'C77 H71 B Fe N7 O3 P S'
_chemical_formula_weight         1272.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                101.548(2)
_cell_angle_beta                 105.060(2)
_cell_angle_gamma                102.362(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7590(4)
_cell_length_b                   15.7112(4)
_cell_length_c                   16.5846(5)
_cell_measurement_reflns_used    25704
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.9260
_cell_measurement_theta_min      3.7090
_cell_volume                     3254.96(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'XS (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 0.995
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -96.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5237  125.0000   60.0000 94

  2 omega -131.00   48.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5237    0.0000  -60.0000 179

  3 omega  -49.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5237   37.0000  -30.0000 84

  4 omega   23.00   99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5237 -125.0000 -120.0000 76

  5 omega   23.00   99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5237 -125.0000   60.0000 76

  6 omega   34.00   98.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000  120.0000 64

  7 omega   78.00  178.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878   30.0000  -90.0000 100

  8 omega   34.00  139.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -61.0000  -30.0000 105

  9 omega   24.00  109.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000  -30.0000 85

 10 omega   94.00  178.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  125.0000  -90.0000 84

 11 omega   30.00   90.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000   90.0000 60

 12 omega   24.00  109.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000   60.0000 85

 13 omega   78.00  178.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878   30.0000    0.0000 100

 14 omega   94.00  178.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  125.0000 -180.0000 84

 15 omega   30.00   90.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000  -60.0000 60

 16 omega   30.00   90.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000 -150.0000 60

 17 omega   34.00   98.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000   30.0000 64

 18 omega   24.00  109.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000 -120.0000 85

 19 omega   34.00   98.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000 -150.0000 64

 20 omega   33.00  122.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878 -125.0000 -150.0000 89

 21 omega -120.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5237  -77.0000   90.0000 112

 22 omega -124.00  -79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5237  -99.0000  -60.0000 45

 23 omega -120.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5237  -77.0000 -150.0000 112

 24 omega -115.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5237  -57.0000    0.0000 103

 25 omega -115.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5237  -57.0000  150.0000 103

 26 omega -117.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5237  -69.0000  -42.0000 107

 27 omega   47.00  168.00   1.0000    2.9650
omega____ theta____ kappa____ phi______ frames
    -      108.2878   15.0000  150.0000 121
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0430070000
_diffrn_orient_matrix_UB_12      0.0274244000
_diffrn_orient_matrix_UB_13      -0.0708930000
_diffrn_orient_matrix_UB_21      -0.0950997000
_diffrn_orient_matrix_UB_22      0.0354200000
_diffrn_orient_matrix_UB_23      -0.0320725000
_diffrn_orient_matrix_UB_31      0.0608741000
_diffrn_orient_matrix_UB_32      0.0941802000
_diffrn_orient_matrix_UB_33      0.0627189000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45798
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.19
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.825
_exptl_absorpt_correction_T_max  0.715
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.3144
_exptl_crystal_size_mid          0.2203
_exptl_crystal_size_min          0.1609
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         13004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0332P)^2^+3.0878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                12076
_reflns_number_total             13004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01931_si_002.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        3254.96(14)
_cod_database_code               4349130
_chemical_oxdiff_formula         'Fe C53 H47 N7 S O2 P B C24 H20 C H4 O '
_reflns_odcompleteness_completeness 99.99
_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,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C73A) = Uanis(C73)
Uanis(C74A) = Uanis(C74)
Uanis(O2A) = Uanis(O2)
Uanis(O1) = Uanis(O1A)
3. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C73A)=Sof(H73C)=Sof(H73D)=Sof(C74A)=Sof(H74A)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74)=FVAR(1)
 Sof(O1A)=1-FVAR(2)
 Sof(O1)=FVAR(2)
 Sof(O2A)=Sof(H76D)=Sof(H76E)=Sof(H76F)=1-FVAR(3)
 Sof(O2)=Sof(H76A)=Sof(H76B)=Sof(H76C)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C74(H74), C74A(H74A)
4.b Secondary CH2 refined with riding coordinates:
 N7(H7AA,H7AB), N7(H7BC,H7BD), C73(H73A,H73B), C73A(H73C,H73D)
4.c Me refined with riding coordinates:
 C76(H76A,H76B,H76C), C76(H76D,H76E,H76F)
4.d Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
  C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
 C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
  C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
4.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C23(H23A,H23B,H23C), C36(H36A,H36B,H36C), C77(H77A,H77B,
 H77C)
4.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_date_sample_data_collection 2015-08-25
_olex2_date_sample_submission    2015-08-25
_olex2_submission_special_instructions 'No special instructions were received'