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_4132857
_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         'B F4, C54 H56 Fe2 O3 P3 S3, 3(C H2 Cl2)'
_chemical_formula_sum            'C57 H62 B Cl6 F4 Fe2 O3 P3 S3'
_chemical_formula_weight         1395.36
_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     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                90
_cell_angle_beta                 97.296(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6592(2)
_cell_length_b                   21.1825(4)
_cell_length_c                   23.4254(4)
_cell_measurement_reflns_used    12243
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.6660
_cell_measurement_theta_min      4.0350
_cell_volume                     6230.74(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.936
_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    119.00 146.00   1.00    1.69    --  107.75 108.00 -98.00   27
  2  \w     94.00 178.00   1.00    1.69    --  107.75 125.00-120.00   84
  3  \w     95.00 178.00   1.00    1.69    --  107.75 125.00  90.00   83
  4  \w    -85.00   3.00   1.00    0.42    --  -48.45 108.00 -98.00   88
  5  \w    -88.00 -30.00   1.00    1.69    --  -86.25 108.00 -98.00   58
  6  \w   -159.00 -75.00   1.00    1.69    --  -86.25 -37.00-150.00   84
  7  \w    -61.00  14.00   1.00    0.42    --  -48.45  37.00-180.00   75
  8  \w    104.00 178.00   1.00    1.69    --  107.75  37.00   0.00   74
  9  \w   -119.00 -81.00   1.00    1.69    --  -86.25-108.00 163.00   38
 10  \w     28.00  56.00   1.00    0.42    --   48.45-108.00 163.00   28
 11  \w     81.00 108.00   1.00    1.69    --  107.75-108.00 163.00   27
 12  \w     84.00 109.00   1.00    1.69    --  107.75-125.00  30.00   25
 13  \w     35.00  82.00   1.00    1.69    --  107.75-125.00  30.00   47
 14  \w     43.00 112.00   1.00    1.69    --  107.75-125.00-120.00   69
 15  \w   -118.00 -77.00   1.00    0.42    --  -48.45-125.00 -30.00   41
;
_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      -0.0037595000
_diffrn_orient_matrix_UB_12      -0.0598366000
_diffrn_orient_matrix_UB_13      -0.0375886000
_diffrn_orient_matrix_UB_21      0.0544663000
_diffrn_orient_matrix_UB_22      -0.0378254000
_diffrn_orient_matrix_UB_23      0.0517621000
_diffrn_orient_matrix_UB_31      -0.1097908000
_diffrn_orient_matrix_UB_32      -0.0168171000
_diffrn_orient_matrix_UB_33      0.0174946000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38081
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.187
_diffrn_reflns_theta_min         3.520
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.224
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       ROD
_exptl_crystal_F_000             2864
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         12349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+21.5391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10015
_reflns_number_total             12349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06996_si_002.cif
_cod_data_source_block           1852520
_cod_database_code               4132857
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         FeSPCO
_reflns_odcompleteness_completeness 98.98
_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.a Ternary CH refined with riding coordinates:
 C43(H43), C49(H49)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C44(H44A,H44B), C45(H45A,
 H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B),
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B),
  C56(H56A,H56B), C57(H57A,H57B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C39(H39), C40(H40), C41(H41), C42(H42)
;
_shelx_res_checksum              83962
_shelx_hkl_checksum              46821
_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 1.850
_oxdiff_exptl_absorpt_empirical_full_min 0.486