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_4132243
_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         'C72 H88 Fe2 N2 P4 S2 Si2, C4 H9.66 O'
_chemical_formula_sum            'C76 H98 Fe2 N2 O P4 S2 Si2'
_chemical_formula_weight         1411.44
_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             2017-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.650(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0710(9)
_cell_length_b                   17.5234(8)
_cell_length_c                   21.7136(9)
_cell_measurement_reflns_used    9326
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.73
_cell_measurement_theta_min      2.32
_cell_volume                     7316.7(6)
_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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0457
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            195818
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.039
_diffrn_reflns_theta_min         2.324
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0617 before and 0.0429 after correction. The Ratio of minimum to maximum transmission is 0.9350. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         21395
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+6.7690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17093
_reflns_number_total             21395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02603_si_002.cif
_cod_data_source_block           compound6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132243
_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. Rigid body (RIGU) restrains
 C41A, C41, C40, C40A, C39, C39A, C38, C38A, C37, C37A, C42A, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18A, C17A, C16A, C15A, C14A, C13A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15A, C16A, C17A, C18A, C13A, C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25A, C26A, C27A, C28A, C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C30, C29, C28, C27, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H29A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C25A)=Sof(C28A)=
 Sof(H28A)=1-FVAR(1)
 Sof(H29)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=FVAR(1)
 Sof(C42)=Sof(C40)=Sof(H40)=Sof(C38)=Sof(H38)=Sof(C37)=Sof(H37)=Sof(C39)=
 Sof(H39)=Sof(C41)=Sof(H41)=1-FVAR(2)
 Sof(C41A)=Sof(H41A)=Sof(C40A)=Sof(H40A)=Sof(C39A)=Sof(H39A)=Sof(C38A)=
 Sof(H38A)=Sof(C37A)=Sof(H37A)=Sof(C42A)=FVAR(2)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=
 Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=Sof(H3S)=1-FVAR(3)
 Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(H5SC)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(C8S)=
 Sof(H8SA)=Sof(H8SB)=Sof(H8SC)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=FVAR(3)
 Sof(C13)=Sof(C18)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C17)=Sof(H17)=
 Sof(C16)=Sof(H16)=1-FVAR(4)
 Sof(C16A)=Sof(H16A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C13A)=
 Sof(C18A)=Sof(C17A)=Sof(H17A)=FVAR(4)
 Sof(Si1)=1-FVAR(5)
 Sof(Si1A)=FVAR(5)
4.a Ternary CH refined with riding coordinates:
 C55(H55), C58(H58), C33(H33), C31(H31), C70(H70), C22(H22), C67(H67), C19(H19)
4.b Secondary CH2 refined with riding coordinates:
 C6S(H6SA,H6SB), C7S(H7SA,H7SB), C2S(H2SA,H2SB)
4.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C45(H45), C44(H44), C52(H52), C46(H46), C51(H51), C50(H50),
 C65(H65), C64(H64), C1(H1), C29(H29), C29(H29A), C5(H5), C62(H62), C2(H2),
 C63(H63), C4(H4), C3(H3), C26(H26), C27(H27), C28(H28), C26A(H26A), C27A(H27A),
  C28A(H28A), C41A(H41A), C40A(H40A), C39A(H39A), C38A(H38A), C37A(H37A),
 C40(H40), C38(H38), C37(H37), C39(H39), C41(H41), C3S(H3S), C16A(H16A),
 C14A(H14A), C15A(H15A), C17A(H17A), C14(H14), C15(H15), C17(H17), C16(H16),
 C10(H10), C8(H8), C9(H9)
4.d Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C56(H56A,H56B,
 H56C), C35(H35A,H35B,H35C), C72(H72A,H72B,H72C), C34(H34A,H34B,H34C), C32(H32A,
 H32B,H32C), C69(H69A,H69B,H69C), C68(H68A,H68B,H68C), C71(H71A,H71B,H71C),
 C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C23(H23A,H23B,H23C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C5S(H5SA,H5SB,H5SC), C8S(H8SA,H8SB,H8SC), C1S(H1SA,
 H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'