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_4132246
_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 H45 Fe N2 P2 S Si'
_chemical_formula_sum            'C36 H45 Fe N2 P2 S Si'
_chemical_formula_weight         683.68
_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   mixed
_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                 91.910(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8933(7)
_cell_length_b                   12.1269(5)
_cell_length_c                   17.6931(7)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.39
_cell_measurement_theta_min      2.78
_cell_volume                     3408.2(2)
_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      99.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51712
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.898
_diffrn_reflns_theta_min         2.782
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.553
_exptl_absorpt_correction_T_max  0.7498
_exptl_absorpt_correction_T_min  0.6704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0838 before and 0.0743 after correction.
The Ratio of minimum to maximum transmission is 0.8941.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7319
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0290P)^2^+4.2710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5972
_reflns_number_total             7319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02603_si_002.cif
_cod_data_source_block           compound8H
_cod_database_code               4132246
_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
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C37, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H34A)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=1-FVAR(1)
 Sof(H34)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(1)
 Sof(H38A)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=1-FVAR(2)
 Sof(H38)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C24(H24), C21(H21), C34(H34), C34(H34A), C38(H38), C38(H38A)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C14(H14),
 C15(H15), C16(H16), C17(H17), C26(H26), C27(H27), C28(H28), C29(H29)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C19(H19A,H19B,
 H19C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C35(H35A,
 H35B,H35C), C32(H32A,H32B,H32C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              19837
_shelx_hkl_checksum              92809
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'