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_4132248
_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         'C38 H47 Fe N P2 S Si'
_chemical_formula_sum            'C38 H47 Fe N P2 S Si'
_chemical_formula_weight         695.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.320(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1224(9)
_cell_length_b                   16.4372(14)
_cell_length_c                   21.1981(18)
_cell_measurement_reflns_used    9003
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.240
_cell_measurement_theta_min      2.386
_cell_volume                     3480.5(5)
_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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0822
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            226016
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.249
_diffrn_reflns_theta_min         2.112
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.597
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         21893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+1.0360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17770
_reflns_number_total             21893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02603_si_002.cif
_cod_data_source_block           compound11
_cod_database_code               4132248
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.865
_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. Others
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C36)=Sof(H36)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(H41C)=1-FVAR(1)
 Sof(C40)=Sof(H40)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=Sof(H39C)=FVAR(1)
 Sof(H31A)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=1-FVAR(2)
 Sof(H31)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C33)=Sof(H33A)=Sof(H33B)=
 Sof(H33C)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C19(H19), C31(H31), C31(H31A), C22(H22), C40(H40), C36(H36)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C1(H1), C8(H8), C27(H27), C29(H29), C28(H28), C4(H4),
 C5(H5), C17(H17), C26(H26), C2(H2), C3(H3), C18(H18), C16(H16), C15(H15)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C43(H43A,H43B,H43C), C34(H34A,H34B,
 H34C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C33(H33A,H33B,H33C), C37(H37A,
 H37B,H37C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C35(H35A,H35B,H35C),
 C32(H32A,H32B,H32C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              95217
_shelx_hkl_checksum              2546
_olex2_submission_special_instructions 'No special instructions were received'