Base-Free Iron Hydrosilylene Complexes via an α-Hydride Migration that Induces Spin Pairing.
Smith, Patrick W.; Tilley, T. Don; Journal of the American Chemical Society 140 (2018) 3880–3883; doi:10.1021/jacs.8b01185

data_4132069
_publ_section_title
;
 Base-Free Iron Hydrosilylene Complexes via an \a-Hydride Migration that
 Induces Spin Pairing.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3880
_journal_page_last               3883
_journal_paper_doi               10.1021/jacs.8b01185
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '2(C41 H59 Fe P Si)'
_chemical_formula_sum            'C82 H118 Fe2 P2 Si2'
_chemical_formula_weight         1333.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0318(3)
_cell_length_b                   15.6740(3)
_cell_length_c                   33.3126(6)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.30
_cell_volume                     7326.6(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 1.000
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            66365
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.438
_diffrn_reflns_theta_min         1.223
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0796 before and 0.0542 after correction.
The Ratio of minimum to maximum transmission is 0.9408.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0380P)^2^+6.4219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5474
_reflns_number_total             6763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01185_si_007.cif
_cod_data_source_block           ps4_94_0m
_cod_database_code               4132069
_shelx_shelxl_version_number     2017/1
_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, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=1-FVAR(1)
 Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11)=Sof(H11)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(H13C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C17(H17), C14(H14), C11(H11)
3.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B)
3.c Me refined with riding coordinates:
 C12(H12D,H12E,H12F), C12(H12A,H12B,H12C)
3.d Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C28(H28), C30(H30), C37(H37), C39(H39)
3.e Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
  C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              91861
_shelx_hkl_checksum              19800
_olex2_submission_special_instructions 'No special instructions were received'