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_4132853
_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 H57 Fe2 O2 P3 S3, C H2 Cl2'
_chemical_formula_sum            'C54 H59 Cl2 Fe2 O2 P3 S3'
_chemical_formula_weight         1111.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/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                 90.251(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9127(5)
_cell_length_b                   15.2090(6)
_cell_length_c                   27.6092(9)
_cell_measurement_reflns_used    12243
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.6660
_cell_measurement_theta_min      4.0350
_cell_volume                     5422.1(3)
_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 0.983
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32922
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.445
_exptl_absorpt_coefficient_mu    0.877
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       rod
_exptl_crystal_F_000             2312
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         10853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0473P)^2^+8.9507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7982
_reflns_number_total             10853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06996_si_002.cif
_cod_data_source_block           1852516
_cod_database_code               4132853
_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, All Fe(H) groups
2.a Riding coordinates:
 Fe1(H)
2.b Ternary CH refined with riding coordinates:
 C41(H41), C47(H47)
2.c Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C46(H46A,H46B), C45(H45A,H45B), C48(H48A,H48B), C50(H50A,
 H50B), C33(H33A,H33B), C52(H52A,H52B), C44(H44A,H44B), C42(H42A,H42B),
 C43(H43A,H43B), C34(H34A,H34B), C51(H51A,H51B), C32(H32A,H32B), C54(H54A,H54B)
2.d Aromatic/amide H refined with riding coordinates:
 C22(H22), C20(H20), C16(H16), C29(H29), C21(H21), C17(H17), C6(H6), C27(H27),
 C9(H9), C10(H10), C3(H3), C11(H11), C14(H14), C39(H39), C8(H8), C37(H37),
 C5(H5), C26(H26), C36(H36), C15(H15), C38(H38), C30(H30), C12(H12), C18(H18),
 C24(H24), C4(H4), C28(H28), C23(H23)
;
_shelx_res_checksum              47163
_shelx_hkl_checksum              29106
_shelx_fab_checksum              10998
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'