Nonheme iron-thiolate complexes as structural models of sulfoxide synthase active sites.
Ekanayake, Danushka M.; Fischer, Anne A.; Elwood, Maya E.; Guzek, Alexandra M.; Lindeman, Sergey V.; Popescu, Codrina V.; Fiedler, Adam T.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17745–17757; doi:10.1039/d0dt03403g

data_7705786
_publ_section_title
;
 Nonheme iron-thiolate complexes as structural models of sulfoxide
 synthase active sites.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17745
_journal_page_last               17757
_journal_paper_doi               10.1039/d0dt03403g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C22 H31 Fe N6 S, C24 H20 B, C H2 Cl'
_chemical_formula_sum            'C47 H53 B Cl Fe N6 S'
_chemical_formula_weight         836.12
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-30 deposited with the CCDC.	2020-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                78.014(2)
_cell_angle_beta                 89.101(2)
_cell_angle_gamma                86.0173(19)
_cell_formula_units_Z            2
_cell_length_a                   10.5475(2)
_cell_length_b                   14.1880(3)
_cell_length_c                   14.5112(4)
_cell_measurement_reflns_used    14375
_cell_measurement_temperature    100.05(10)
_cell_measurement_theta_max      70.5570
_cell_measurement_theta_min      4.1710
_cell_volume                     2119.10(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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    3.50    --  -42.33  37.00 -90.00   99
  2  \w   -117.00 -18.00   1.00    3.50    --  -42.33 -37.00  90.00   99
  3  \w    -67.00  32.00   1.00    3.50    --  -42.33  37.00  30.00   99
  4  \w      1.00  83.00   1.00    3.50    --   42.33 -99.00   0.00   82
  5  \w     94.00 173.00   1.00   15.00    --  100.00 125.00 -30.00   79
  6  \w     28.00 129.00   1.00   15.00    --  100.00 -61.00 -30.00  101
  7  \w     67.00 176.00   1.00   15.00    --  100.00  77.00  30.00  109
  8  \w     27.00 118.00   1.00   15.00    --  100.00-125.00 -60.00   91
  9  \w     74.00 173.00   1.00   15.00    --  100.00  45.00  90.00   99
 10  \w     27.00 118.00   1.00   15.00    --  100.00-125.00  60.00   91
 11  \w     27.00 118.00   1.00   15.00    --  100.00-125.00 -90.00   91
 12  \w     74.00 173.00   1.00   15.00    --  100.00  45.00 150.00   99
 13  \w     94.00 173.00   1.00   15.00    --  100.00 125.00 -60.00   79
 14  \w     94.00 173.00   1.00   15.00    --  100.00 125.00 -90.00   79
 15  \w     24.00 133.00   1.00   15.00    --  100.00 -77.00 -90.00  109
 16  \w     27.00 118.00   1.00   15.00    --  100.00-125.00 150.00   91
 17  \w     74.00 173.00   1.00   15.00    --  100.00  45.00 -30.00   99
 18  \w   -118.00 -10.00   1.00    3.50    --  -42.33 -77.00-180.00  108
 19  \w   -114.00 -14.00   1.00    3.50    --  -42.33 -57.00-120.00  100
 20  \w   -118.00 -10.00   1.00    3.50    --  -42.33 -77.00   0.00  108
 21  \w    -32.00  67.00   1.00    3.50    --   42.33 -37.00  90.00   99
 22  \w     67.00 137.00   1.00   15.00    --  100.00  77.00 -90.00   70
 23  \w     71.00 172.00   1.00   15.00    --  100.00  61.00-180.00  101
 24  \w     71.00 172.00   1.00   15.00    --  100.00  61.00 -90.00  101
 25  \w     67.00 176.00   1.00   15.00    --  100.00  77.00-150.00  109
 26  \w     72.00 176.00   1.00   15.00    --  100.00  30.00-120.00  104
 27  \w     71.00 172.00   1.00   15.00    --  100.00  61.00 150.00  101
 28  \w     67.00 176.00   1.00   15.00    --  100.00  77.00  90.00  109
 29  \w     71.00  73.00   1.00   15.00    --  100.00  61.00   0.00    2
;
_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      -0.0374940000
_diffrn_orient_matrix_UB_12      -0.0582801000
_diffrn_orient_matrix_UB_13      0.0972074000
_diffrn_orient_matrix_UB_21      -0.0319962000
_diffrn_orient_matrix_UB_22      0.0947535000
_diffrn_orient_matrix_UB_23      0.0340655000
_diffrn_orient_matrix_UB_31      -0.1378667000
_diffrn_orient_matrix_UB_32      0.0018559000
_diffrn_orient_matrix_UB_33      -0.0341919000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37008
_diffrn_reflns_theta_full        70.58
_diffrn_reflns_theta_max         70.58
_diffrn_reflns_theta_min         3.97
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.205
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         8011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0789P)^2^+1.1178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                7336
_reflns_number_total             8011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt03403g2.cif
_cod_data_source_block           complex2
_cod_depositor_comments
'Adding full bibliography for 7705784--7705787.cif.'
_cod_original_cell_volume        2119.09(9)
_cod_database_code               7705786
_chemical_oxdiff_formula         'C46 H51 B Fe N6 S C H2 Cl'
_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 C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C15, C6A}
3. Uiso/Uaniso restraints and constraints
Uanis(C17A) = Uanis(C17)
Uanis(C22) = Uanis(C22A)
Uanis(C21) = Uanis(C21A)
Uanis(C19) = Uanis(C46)
Uanis(C20A) = Uanis(C20)
Uanis(C18) = Uanis(C18A)
Uanis(N5A) = Uanis(N5)
Uanis(C3A) = Uanis(C3)
Uanis(C4) = Uanis(C4A)
Uanis(C5A) = Uanis(C5)
Uanis(C16A) = Uanis(C16)
Uanis(C15) = Uanis(C6A)
4. Others
 Sof(N5A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=
 Sof(H6A)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17A)=Sof(C18A)=
 Sof(H18C)=Sof(H18D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21C)=
 Sof(H21D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C46)=Sof(H46A)=Sof(H46B)=1-FVAR(1)
 Sof(N5)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18A)=
 Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=
 Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=FVAR(1)
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5)
5.a Ternary CH refined with riding coordinates:
 C17(H17), C17A(H17A)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C12(H12A,H12B), C18(H18A,H18B), C18A(H18C,H18D),
 C19(H19A,H19B), C20(H20A,H20B), C20A(H20C,H20D), C21(H21A,H21B), C21A(H21C,
 H21D), C22(H22A,H22B), C22A(H22C,H22D), C46(H46A,H46B), C1S(H1SA,H1SB),
 C2S(H2SA,H2SB)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C3A(H3A), C4(H4), C4A(H4A), C5(H5), C5A(H5A), C6(H6), C9(H9),
 C10(H10), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F)
;
_olex2_date_sample_data_collection 2019-06-19
_olex2_date_sample_submission    2019-06-18
_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 1.219
_oxdiff_exptl_absorpt_empirical_full_min 0.874