An S = <sup>1</sup>/<sub>2</sub> Iron Complex Featuring N<sub>2</sub>, Thiolate, and Hydride Ligands: Reductive Elimination of H<sub>2</sub> and Relevant Thermochemical Fe-H Parameters.
Gu, Nina X.; Oyala, Paul H.; Peters, Jonas C.; Journal of the American Chemical Society 140 (2018) 6374–6382; doi:10.1021/jacs.8b02603

data_4132244
_publ_section_title
;
 An S = <sup>1</sup>/<sub>2</sub> Iron Complex Featuring N<sub>2</sub>,
 Thiolate, and Hydride Ligands: Reductive Elimination of H<sub>2</sub> and
 Relevant Thermochemical Fe-H Parameters.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6374
_journal_page_last               6382
_journal_paper_doi               10.1021/jacs.8b02603
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '1(C43.77 H62.33 Fe Li N2 O2 P2 S Si)'
_chemical_formula_sum            'C43.83 H62.62 Fe Li N2 O2 P2 S Si'
_chemical_formula_weight         834.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.3145(16)
_cell_length_b                   13.0291(11)
_cell_length_c                   35.412(3)
_cell_measurement_reflns_used    9722
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      2.56
_cell_volume                     8911.4(13)
_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  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.03
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            99776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.556
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0735 before and 0.0608 after correction. The Ratio of minimum to maximum transmission is 0.8455. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       block
_exptl_crystal_F_000             3557
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.295(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1093
_refine_ls_number_reflns         17886
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0630P)^2^+7.4750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.966
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                15678
_reflns_number_total             17886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02603_si_002.cif
_cod_data_source_block           compound7H
_cod_original_cell_volume        8911.4(12)
_cod_database_code               4132244
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.705(18) 0.295(18)
2. 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, All C(H,H,H,H,H,H) groups
3. Restrained distances
 C87-O4 \\sim O4-C89
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 O4, C86, C85, C84, C83, C87, C88, C89, C90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C37, C38, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, C35, C34, C37, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C93, C94
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C39, C44, C40, C41, C45, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C39, C45, C40, C41, C44, C46, C42, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=FVAR(1)
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=Sof(C89)=
 Sof(H89A)=Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=1-FVAR(2)
 Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C84)=Sof(H84A)=
 Sof(H84B)=Sof(C83)=Sof(H83A)=Sof(H83B)=FVAR(2)
 Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C35)=
 Sof(H35)=1-FVAR(3)
 Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=FVAR(3)
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=FVAR(4)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=1-FVAR(5)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C45)=Sof(H45A)=Sof(H45B)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C77(H77), C68(H68), C65(H65), C80(H80), C37(H37), C19(H19),
 C22(H22), C35(H35)
6.b Secondary CH2 refined with riding coordinates:
 C93(H93A,H93B), C91(H91A,H91B), C028(H02A,H02B), C02H(H02F,H02G), C39(H39A,
 H39B), C45(H45A,H45B), C86(H86A,H86B), C85(H85A,H85B), C84(H84A,H84B),
 C40(H40A,H40B), C41(H41A,H41B), C83(H83A,H83B), C87(H87A,H87B), C89(H89A,H89B),
  C42(H42A,H42B), C43(H43A,H43B)
6.c Me refined with riding coordinates:
 C34(H34A,H34B,H34C), C34(H34D,H34E,H34F)
6.d Aromatic/amide H refined with riding coordinates:
 C54(H54), C8(H8), C55(H55), C51(H51), C47(H47), C56(H56), C10(H10), C63(H63),
 C9(H9), C60(H60), C49(H49), C1(H1), C29(H29), C48(H48), C28(H28), C50(H50),
 C5(H5), C62(H62), C2(H2), C61(H61), C75(H75), C4(H4), C26(H26), C3(H3),
 C17(H17), C27(H27), C73(H73), C74(H74), C72(H72), C15(H15), C16(H16), C14(H14)
6.e Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C32(H32A,H32B,H32C), C70(H70A,H70B,H70C), C69(H69A,H69B,
 H69C), C78(H78A,H78B,H78C), C33(H33A,H33B,H33C), C67(H67A,H67B,H67C), C81(H81A,
 H81B,H81C), C21(H21A,H21B,H21C), C02A(H02C,H02D,H02E), C82(H82A,H82B,H82C),
 C24(H24A,H24B,H24C), C66(H66A,H66B,H66C), C02K(H02H,H02I,H02J), C92(H92A,H92B,
 H92C), C20(H20A,H20B,H20C), C38(H38A,H38B,H38C), C23(H23A,H23B,H23C), C94(H94A,
 H94B,H94C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C88(H88A,H88B,H88C),
 C90(H90A,H90B,H90C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              37605
_shelx_hkl_checksum              85882
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'