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_4132854
_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, B F4, C H2 Cl2'
_chemical_formula_sum            'C54 H60 B Cl2 F4 Fe2 O2 P3 S3'
_chemical_formula_weight         1199.52
_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   mixed
_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                 102.738(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.971(2)
_cell_length_b                   25.090(4)
_cell_length_c                   18.274(3)
_cell_measurement_reflns_used    6139
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.109
_cell_measurement_theta_min      2.225
_cell_volume                     6248.0(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'BRuker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36241
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.699
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1159 before and 0.0596 after correction.
The Ratio of minimum to maximum transmission is 0.5916.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       rod
_exptl_crystal_F_000             2480
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         10915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0715P)^2^+9.4759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6622
_reflns_number_total             10915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06996_si_002.cif
_cod_data_source_block           1852517
_cod_original_cell_volume        6248.3(18)
_cod_database_code               4132854
_shelx_shelxl_version_number     2014/7
_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:
 C35(H35), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C42(H42A,H42B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C54(H54A,H54B)
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),
 C48(H48), C49(H49), C50(H50), C51(H51)
;
_shelx_res_checksum              64740
_shelx_hkl_checksum              91697
_shelx_fab_checksum              49974
_olex2_submission_special_instructions 'No special instructions were received'