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_4132856
_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         'C54 H60 Fe2 O2 P3 S3, 2(C H2 Cl2), B F4'
_chemical_formula_sum            'C56 H64 B Cl4 F4 Fe2 O2 P3 S3'
_chemical_formula_weight         1298.47
_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             2018-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                97.274(3)
_cell_angle_beta                 107.312(3)
_cell_angle_gamma                109.106(4)
_cell_formula_units_Z            2
_cell_length_a                   12.9031(5)
_cell_length_b                   14.8618(6)
_cell_length_c                   17.6715(7)
_cell_measurement_reflns_used    11691
_cell_measurement_temperature    172.9(5)
_cell_measurement_theta_max      30.4800
_cell_measurement_theta_min      3.4770
_cell_volume                     2961.3(2)
_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      172.9(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_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    -56.00 -21.00   1.00    8.00    --   -4.48 -83.00   4.00   35
  2  \w    -24.00  66.00   1.00    8.00    --   -4.48  83.00 125.00   90
  3  \w    -26.00  28.00   1.00    8.00    --   -4.48 -99.00-150.00   54
  4  \w    -26.00  25.00   1.00    8.00    --   -4.48 -99.00 -30.00   51
  5  \w    -26.00   6.00   1.00    8.00    --   -4.48 -99.00  90.00   32
  6  \w    -18.00  68.00   1.00    8.00    --   -4.48  57.00  30.00   86
  7  \w    -12.00  20.00   1.00    8.00    --   -4.48 -83.00   4.00   32
;
_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      0.0201316000
_diffrn_orient_matrix_UB_12      -0.0351430000
_diffrn_orient_matrix_UB_13      0.0160421000
_diffrn_orient_matrix_UB_21      -0.0155921000
_diffrn_orient_matrix_UB_22      0.0100565000
_diffrn_orient_matrix_UB_23      0.0344561000
_diffrn_orient_matrix_UB_31      -0.0569690000
_diffrn_orient_matrix_UB_32      -0.0371837000
_diffrn_orient_matrix_UB_33      -0.0209565000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33415
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.314
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09135
_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    1.456
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1340
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         12012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0677P)^2^+0.3060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9154
_reflns_number_total             12012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06996_si_002.cif
_cod_data_source_block           1852519
_cod_database_code               4132856
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         FePSCO
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C47(H47), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C49(H49A,H49B), C42(H42A,H42B), C50(H50A,H50B), C33(H33A,
 H33B), C32(H32A,H32B), C45(H45A,H45B), C46(H46A,H46B), C34(H34A,H34B),
 C52(H52A,H52B), C51(H51A,H51B), C44(H44A,H44B), C48(H48A,H48B), C55(H55A,H55B),
  C56(H56A,H56B)
2.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C20(H20), C23(H23), C22(H22), C10(H10), C8(H8), C27(H27), C21(H21),
 C5(H5), C11(H11), C17(H17), C9(H9), C6(H6), C3(H3), C26(H26), C12(H12),
 C29(H29), C39(H39), C14(H14), C16(H16), C37(H37), C15(H15), C38(H38), C28(H28),
  C4(H4), C18(H18), C24(H24), C30(H30)
2.d Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C)
;
_shelx_res_checksum              80650
_shelx_hkl_checksum              97624
_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 4.163
_oxdiff_exptl_absorpt_empirical_full_min 0.264