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_4132245
_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
'C36 H44 Fe N2 P2 S Si, C12 H23.35 Li O5.02, 0.99(C4 H8 O)'
_chemical_formula_sum            'C51.96 H75.25 Fe Li N2 O6 P2 S Si'
_chemical_formula_weight         1008.89
_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             2016-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.629(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.739(3)
_cell_length_b                   19.956(4)
_cell_length_c                   21.496(4)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      2.21
_cell_volume                     5262.7(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0826
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            90571
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.575
_diffrn_reflns_theta_min         1.949
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.7947.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.739
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         10921
_refine_ls_number_restraints     1362
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.0943
_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^)+(0.0920P)^2^+19.5630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7731
_reflns_number_total             10921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02603_si_002.cif
_cod_data_source_block           compound7Hcrown
_cod_original_cell_volume        5262.8(18)
_cod_database_code               4132245
_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. Uiso/Uaniso restraints and constraints
C82 \\sim C81 \\sim C80 \\sim C83: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
P2 \\sim C38 \\sim C36: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
P3 \\sim C41 \\sim C39 \\sim C40 \\sim C46 \\sim C47 \\sim C45 \\sim P2 \\sim
C38 \\sim C36 \\sim C37 \\sim C42 \\sim C43 \\sim C44: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C57 \\sim O3 \\sim C56 \\sim C59 \\sim C58 \\sim C54 \\sim C55 \\sim O2 \\sim
C53 \\sim O1 \\sim C48 \\sim C50 \\sim C51 \\sim C49 \\sim C52: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C63 \\sim O6 \\sim C64 \\sim C65: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C70 \\sim O8 \\sim O9 \\sim O11 \\sim C73 \\sim H73A \\sim H73B \\sim C74 \\sim
H74A \\sim H74B \\sim C69 \\sim C71 \\sim C72 \\sim C68 \\sim C75 \\sim O5
\\sim C61 \\sim C67 \\sim C62 \\sim O4 \\sim C60 \\sim C66 \\sim C65 \\sim O7
\\sim O10 \\sim C63 \\sim O6 \\sim C64 \\sim H2AA: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C10 \\sim C4 \\sim C9 \\sim C8 \\sim C3 \\sim C7 \\sim C2 \\sim C1 \\sim C11
\\sim C6 \\sim C5: within 1.7A with sigma of 0.04 and sigma for terminal atoms
of 0.08
Uanis(P3) = Uanis(P2)
3. Rigid body (RIGU) restrains
 C66, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C3, C6, C4, C5, C9, C7, C8, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0AA, C82, C81, C80, C83, O1SB, C79, C78, C77, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, C47, C45, C37, C42, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C39, C40, P2, C38, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P3, C41, C39, C40, C46, C47, C45, P2, C38, C36, C37, C42, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C57, O3, C56, C59, C58, C54, C55, O2, C53, O1, C48, C50, C51, C49, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, O9, O11, C73, C74, C69, C71, C72, C68, C75, C70, Li1, O5, C61, C67, C62,
 O4, C60, C66, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C63, C64, C65, O7, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 1*[Sof(C57)+Sof(H1A)+Sof(H1C)+Sof(O3)+Sof(C56)+Sof(H7A)+Sof(H7B)+Sof(C59)+
 Sof(H5AA)+Sof(H5AB)+Sof(C58)+Sof(H15A)+Sof(H15B)]+1*[Sof(C54)+Sof(H54A)+
 Sof(H54B)+Sof(C55)+Sof(H55A)+Sof(H55B)+Sof(O2)+Sof(C53)+Sof(H53A)+Sof(H53B)+
 Sof(C52)+Sof(H52A)+Sof(H52B)]+1*[Sof(O1)+Sof(C48)+Sof(H9AA)+Sof(H9AB)+Sof(C50)+
 Sof(H1BA)+Sof(H1BB)+Sof(C51)+Sof(H11A)+Sof(H11B)+Sof(C49)+Sof(H16A)+Sof(H16B)]=
 1 with esd of 0.01
 Sof(O1SB)=Sof(C79)=Sof(H1SC)=Sof(C78)=Sof(H2SC)=Sof(H2SD)=Sof(C77)=Sof(H3SC)=
 Sof(H3SD)=Sof(C76)=Sof(H4SC)=Sof(H4SD)=1-FVAR(1)
 Sof(O0AA)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C80)=
 Sof(H80A)=Sof(H80B)=Sof(C83)=Sof(H83A)=Sof(H83B)=FVAR(1)
 Sof(O5)=Sof(C61)=Sof(H3AA)=Sof(H3AB)=Sof(C67)=Sof(H10A)=Sof(H10B)=Sof(C62)=
 Sof(H2XA)=Sof(H2XB)=Sof(O4)=Sof(C60)=Sof(H22A)=Sof(H22B)=Sof(C66)=Sof(H25A)=
 Sof(H25B)=Sof(C65)=Sof(H4AA)=Sof(H4AB)=Sof(O7)=Sof(O10)=Sof(C63)=Sof(H8AA)=
 Sof(H8AB)=Sof(O6)=Sof(C64)=Sof(H2AA)=Sof(H2AB)=1-FVAR(2)
 Sof(O8)=Sof(O9)=Sof(O11)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=
 Sof(H74B)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=
 Sof(H72A)=Sof(H72B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C75)=Sof(H75A)=Sof(H75B)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=FVAR(2)
 Sof(C9)=Sof(H3B)=Sof(C7)=Sof(H1B)=Sof(C8)=Sof(H2B)=Sof(C10)=Sof(H4B)=Sof(C11)=
 Sof(H5B)=1-FVAR(3)
 Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C6)=Sof(H6)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5)=FVAR(3)
 Sof(P3)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C36)=Sof(H36)=Sof(C37)=
 Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=1-FVAR(4)
 Sof(C41)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C39)=Sof(H3BA)=Sof(C40)=Sof(H1AA)=
 Sof(H1AB)=Sof(H1AC)=Sof(C46)=Sof(H1MA)=Sof(H1MB)=Sof(H1MC)=Sof(C47)=Sof(H3MA)=
 Sof(H3MB)=Sof(H3MC)=Sof(C45)=Sof(H2M)=Sof(P2)=FVAR(4)
 Sof(C57)=Sof(H1A)=Sof(H1C)=Sof(O3)=Sof(C56)=Sof(H7A)=Sof(H7B)=Sof(C59)=
 Sof(H5AA)=Sof(H5AB)=Sof(C58)=Sof(H15A)=Sof(H15B)=FVAR(5)
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(O2)=Sof(C53)=
 Sof(H53A)=Sof(H53B)=Sof(C52)=Sof(H52A)=Sof(H52B)=FVAR(6)
 Sof(O1)=Sof(C48)=Sof(H9AA)=Sof(H9AB)=Sof(C50)=Sof(H1BA)=Sof(H1BB)=Sof(C51)=
 Sof(H11A)=Sof(H11B)=Sof(C49)=Sof(H16A)=Sof(H16B)=FVAR(7)
5.a Ternary CH refined with riding coordinates:
 C24(H24), C27(H27), C39(H3BA), C45(H2M), C36(H36), C42(H42)
5.b Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B), C69(H69A,H69B), C71(H71A,H71B), C72(H72A,
 H72B), C68(H68A,H68B), C75(H75A,H75B), C70(H70A,H70B), C61(H3AA,H3AB),
 C67(H10A,H10B), C62(H2XA,H2XB), C60(H22A,H22B), C66(H25A,H25B), C65(H4AA,H4AB),
  C82(H82A,H82B), C81(H81A,H81B), C80(H80A,H80B), C83(H83A,H83B), C78(H2SC,
 H2SD), C77(H3SC,H3SD), C76(H4SC,H4SD), C57(H1A,H1C), C56(H7A,H7B), C59(H5AA,
 H5AB), C58(H15A,H15B), C54(H54A,H54B), C55(H55A,H55B), C53(H53A,H53B),
 C48(H9AA,H9AB), C50(H1BA,H1BB), C51(H11A,H11B), C49(H16A,H16B), C52(H52A,H52B),
  C63(H8AA,H8AB), C64(H2AA,H2AB)
5.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C15(H15), C34(H34), C19(H19), C22(H22), C33(H33),
 C14(H14), C20(H20), C13(H13), C2(H2), C3(H3), C21(H21), C6(H6), C4(H4), C5(H5),
  C79(H1SC), C9(H3B), C7(H1B), C8(H2B), C10(H4B), C11(H5B)
5.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25C,H25D,H25E), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C41(H0AA,H0AB,H0AC), C40(H1AA,H1AB,H1AC), C46(H1MA,H1MB,H1MC), C47(H3MA,
 H3MB,H3MC), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C)
;
_shelx_res_checksum              49351
_shelx_hkl_checksum              65137
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'