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_4132247
_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, C16 H32 Na O8, 0.45(C4 H8 O1), 0.55(C5 H12)'
_chemical_formula_sum            'C56.55 H86.19 Fe N2 Na O8.45 P2 S Si'
_chemical_formula_weight         1130.20
_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
_audit_creation_date             2017-06-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.234(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4040(17)
_cell_length_b                   20.067(2)
_cell_length_c                   21.317(3)
_cell_measurement_reflns_used    9001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.260
_cell_volume                     5817.6(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      99.98
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0652
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            79498
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.264
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.7290
_exptl_absorpt_correction_T_min  0.6724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1698 before and 0.0891 after correction. The Ratio of minimum to maximum transmission is 0.9224. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         10269
_refine_ls_number_restraints     582
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0634P)^2^+13.6687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7954
_reflns_number_total             10269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02603_si_002.cif
_cod_data_source_block           compound9
_cod_original_cell_volume        5817.5(12)
_cod_database_code               4132247
_shelx_shelxl_version_number     2016/6
_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
C55 \\sim C53 \\sim C56 \\sim C57 \\sim O12 \\sim O11 \\sim O10 \\sim O9 \\sim
C59 \\sim C58 \\sim C60 \\sim C54: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O7 \\sim O5 \\sim O6 \\sim C51 \\sim C52 \\sim O8 \\sim C47 \\sim C45 \\sim C48
\\sim C50 \\sim C46 \\sim C49: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C31 \\sim C33 \\sim C32: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C31 \\sim C33 \\sim C016: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O3 \\sim O1 \\sim O4 \\sim C41 \\sim C38 \\sim C40 \\sim C44 \\sim C43 \\sim
C42: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O3 \\sim O1 \\sim O2 \\sim O4 \\sim C41 \\sim C38 \\sim C40 \\sim C37 \\sim C44
\\sim C43 \\sim C42 \\sim C39: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C32 \\sim C31 \\sim C33: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C016 \\sim C31 \\sim C33: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C69 \\sim O13 \\sim C61 \\sim C65 \\sim C62: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C65 \\sim O13 \\sim C61 \\sim C62 \\sim C69: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C65 \\sim C64 \\sim C63 \\sim C62 \\sim C61: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O13 \\sim C69 \\sim C68 \\sim C67 \\sim C66: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C55, C53, C56, C57, O12, O11, O10, O9, C59, C58, C60, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, O5, O6, C51, C52, O8, C47, C45, C48, C50, C46, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C33, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C33, C016
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, O1, O4, C41, C38, C40, C44, C43, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, O1, O2, O4, C41, C38, C40, C37, C44, C43, C42, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C31, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C016, C31, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, C69, C65, C61, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61, C62, C63, C64, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, C69, C68, C67, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H34A)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=1-FVAR(1)
 Sof(H34)=Sof(C01Q)=Sof(H01D)=Sof(H01E)=Sof(H01F)=FVAR(1)
 Sof(H22A)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(2)
 Sof(H22)=Sof(C8AA)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=FVAR(2)
 Sof(H31A)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=1-FVAR(3)
 Sof(H31)=Sof(C016)=Sof(H01A)=Sof(H01B)=Sof(H01C)=FVAR(3)
 Sof(C55)=Sof(HF)=Sof(HG)=Sof(C53)=Sof(H3AA)=Sof(H4AA)=Sof(C56)=Sof(H5AA)=
 Sof(H6AA)=Sof(C57)=Sof(H7AA)=Sof(H9AA)=Sof(O12)=Sof(O11)=Sof(O10)=Sof(O9)=
 Sof(C59)=Sof(H0BA)=Sof(H1BA)=Sof(C58)=Sof(H2BA)=Sof(H3BA)=Sof(C60)=Sof(H6BA)=
 Sof(H7BA)=Sof(C54)=Sof(H8BA)=Sof(H9BA)=1-FVAR(4)
 Sof(O7)=Sof(O5)=Sof(O6)=Sof(C51)=Sof(HH)=Sof(HI)=Sof(C52)=Sof(HJ)=Sof(HK)=
 Sof(O8)=Sof(C47)=Sof(HN)=Sof(HO)=Sof(C45)=Sof(HP)=Sof(HQ)=Sof(C48)=Sof(HV)=
 Sof(HW)=Sof(C50)=Sof(HX)=Sof(HY)=Sof(C46)=Sof(H1AA)=Sof(H2AA)=Sof(C49)=
 Sof(H4BA)=Sof(H5BA)=FVAR(4)
 Sof(O13)=Sof(C69)=Sof(H2CA)=Sof(H3CA)=Sof(C68)=Sof(H2DA)=Sof(H3DA)=Sof(C67)=
 Sof(H8DA)=Sof(H9DA)=Sof(C66)=Sof(H0EA)=Sof(H1EA)=1-FVAR(5)
 Sof(C61)=Sof(H4CA)=Sof(H5CA)=Sof(H6CA)=Sof(C62)=Sof(H7CA)=Sof(H8CA)=Sof(C65)=
 Sof(H9CA)=Sof(H0DA)=Sof(H1DA)=Sof(C63)=Sof(H4DA)=Sof(H5DA)=Sof(C64)=Sof(H6DA)=
 Sof(H7DA)=FVAR(5)
5.a Ternary CH refined with riding coordinates:
 C19(H19), C31(H31), C31(H31A), C22(H22), C22(H22A), C34(H34), C34(H34A)
5.b Secondary CH2 refined with riding coordinates:
 C41(H,HA), C38(HB,HC), C40(HD,HE), C55(HF,HG), C51(HH,HI), C52(HJ,HK), C37(HL,
 HM), C47(HN,HO), C45(HP,HQ), C44(HR,HS), C43(HT,HU), C48(HV,HW), C50(HX,HY),
 C42(HZ,H0AA), C46(H1AA,H2AA), C53(H3AA,H4AA), C56(H5AA,H6AA), C57(H7AA,H9AA),
 C59(H0BA,H1BA), C58(H2BA,H3BA), C49(H4BA,H5BA), C60(H6BA,H7BA), C54(H8BA,H9BA),
  C39(H0CA,H1CA), C69(H2CA,H3CA), C62(H7CA,H8CA), C68(H2DA,H3DA), C63(H4DA,
 H5DA), C64(H6DA,H7DA), C67(H8DA,H9DA), C66(H0EA,H1EA)
5.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C14(H14), C26(H26), C27(H27), C5(H5), C16(H16), C9(H9), C17(H17),
 C10(H10), C4(H4), C15(H15), C3(H3), C28(H28), C8(H8), C2(H2), C1(H1)
5.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C016(H01A,H01B,
 H01C), C23(H23A,H23B,H23C), C01Q(H01D,H01E,H01F), C35(H35A,H35B,H35C),
 C8AA(H8AA,H8AB,H8AC), C36(H36A,H36B,H36C), C24(H24A,H24B,H24C), C32(H32A,H32B,
 H32C), C61(H4CA,H5CA,H6CA), C65(H9CA,H0DA,H1DA)
;
_shelx_res_checksum              37108
_shelx_hkl_checksum              69127
_olex2_submission_special_instructions 'No special instructions were received'