Terminal Thiolate-Dominated H/D Exchanges and H<sub>2</sub> Release: Diiron Thiol-Hydride.
Yu, Xin; Pang, Maofu; Zhang, Shengnan; Hu, Xinlong; Tung, Chen-Ho; Wang, Wenguang; Journal of the American Chemical Society 140 (2018) 11454–11463; doi:10.1021/jacs.8b06996

data_4132855
_publ_section_title
;
 Terminal Thiolate-Dominated H/D Exchanges and H<sub>2</sub> Release:
 Diiron Thiol-Hydride.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11454
_journal_page_last               11463
_journal_paper_doi               10.1021/jacs.8b06996
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C53 H58 Fe2 O2 P3 S3, C32 H12 B F24'
_chemical_formula_sum            'C85 H70 B F24 Fe2 O2 P3 S3'
_chemical_formula_weight         1891.01
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                87.191(3)
_cell_angle_beta                 75.218(3)
_cell_angle_gamma                72.693(3)
_cell_formula_units_Z            2
_cell_length_a                   17.9369(5)
_cell_length_b                   18.5508(6)
_cell_length_c                   18.5978(6)
_cell_measurement_reflns_used    10481
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.1750
_cell_measurement_theta_min      4.2820
_cell_volume                     5710.2(3)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     16.00  43.00   1.00    0.60    --   48.20 -29.00-115.00   27
  2  \w    -23.00   3.00   1.00    0.60    --   48.20 -29.00-115.00   26
  3  \w     37.00 115.00   1.00    4.00    --  107.75 -29.00-115.00   78
  4  \w     97.00 178.00   1.00    4.00    --  107.75  19.00   0.00   81
  5  \w    100.00 167.00   1.00    4.00    --  107.75  29.00  45.00   67
  6  \w     79.00 119.00   1.00    4.00    --  107.75 -19.00   0.00   40
  7  \w     50.00 124.00   1.00    4.00    --  107.75 -77.00 -30.00   74
  8  \w     47.00  94.00   1.00    4.00    --  107.75 -99.00 -90.00   47
  9  \w     35.00 109.00   1.00    4.00    --  107.75 -99.00 -30.00   74
 10  \w     48.00 108.00   1.00    4.00    --  107.75 -99.00  90.00   60
 11  \w     45.00 120.00   1.00    4.00    --  107.75 -19.00 150.00   75
 12  \w     39.00 114.00   1.00    4.00    --  107.75 -37.00  30.00   75
 13  \w     36.00 123.00   1.00    0.60    --   48.20  29.00  45.00   87
 14  \w     36.00  62.00   1.00    4.00    --  107.75 -19.00   0.00   26
 15  \w     35.00 109.00   1.00    4.00    --  107.75 -99.00-150.00   74
 16  \w     35.00 117.00   1.00    4.00    --  107.75-125.00-150.00   82
 17  \w    -23.00  61.00   1.00    0.60    --   48.20 -37.00  90.00   84
 18  \w    -55.00  26.00   1.00    0.60    --  -48.20  29.00  45.00   81
 19  \w    -38.00 -13.00   1.00    4.00    --  -86.25  29.00  45.00   25
 20  \w    -96.00 -70.00   1.00    4.00    --  -86.25  29.00  45.00   26
 21  \w   -119.00 -36.00   1.00    0.60    --  -48.20 -29.00-115.00   83
 22  \w    -52.00 -18.00   1.00    4.00    --  -86.25 125.00-120.00   34
 23  \w    -91.00 -55.00   1.00    4.00    --  -86.25 125.00-120.00   36
 24  \w   -137.00 -79.00   1.00    4.00    --  -86.25 -29.00-115.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0778357000
_diffrn_orient_matrix_UB_12      -0.0306330000
_diffrn_orient_matrix_UB_13      0.0267192000
_diffrn_orient_matrix_UB_21      0.0030294000
_diffrn_orient_matrix_UB_22      -0.0813093000
_diffrn_orient_matrix_UB_23      -0.0174285000
_diffrn_orient_matrix_UB_31      0.0507493000
_diffrn_orient_matrix_UB_32      0.0047931000
_diffrn_orient_matrix_UB_33      -0.0795494000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53493
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         4.059
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1924
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1116
_refine_ls_number_reflns         20135
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1419P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13970
_reflns_number_total             20135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06996_si_002.cif
_cod_data_source_block           1852518
_cod_database_code               4132855
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         FeSPCOBF
_reflns_odcompleteness_completeness 98.79
_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
2. Rigid bond restraints
 C54, C55
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
 C56, C60
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
3. Others
 Fixed Sof: F16(0.5) F17(0.5) F18(0.5) F93(0.5) F94(0.5) F96(0.5)
4.a Ternary CH refined with riding coordinates:
 C41(H41), C47(H47)
4.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C48(H48A,H48B),
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
  C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C36(H36), C37(H37), C38(H38), C39(H39), C55(H55), C57(H57), C59(H59),
 C63(H63), C65(H65), C67(H67), C71(H71), C73(H73), C75(H75), C79(H79), C81(H81),
  C83(H83)
;
_shelx_res_checksum              48546
_shelx_hkl_checksum              74634
_shelx_fab_checksum              3211
_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 1.461
_oxdiff_exptl_absorpt_empirical_full_min 0.593