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_4132065
_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         'C32 H57 Fe N2 P Si'
_chemical_formula_sum            'C32 H57 Fe N2 P Si'
_chemical_formula_weight         584.70
_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     direct
_audit_creation_date             2017-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.6114(11)
_cell_length_b                   26.303(2)
_cell_length_c                   16.3706(12)
_cell_measurement_reflns_used    7076
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.319
_cell_measurement_theta_min      2.377
_cell_volume                     6722.2(9)
_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
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.980
_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  0.0595
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24471
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.374
_diffrn_reflns_theta_min         1.244
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0467 before and 0.0386 after correction. The Ratio of minimum to maximum transmission is 0.8739. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         11475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0572P)^2^+4.8385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8757
_reflns_number_total             11475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01185_si_004.cif
_cod_data_source_block           ps5_28
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C64 H114 Fe2 N4 P2 Si2'
_cod_original_formula_weight         1169.41
_cod_original_formula_moiety         '2(C32 H57 Fe N2 P Si)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        6722.1(9)
_cod_database_code               4132065
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5658(10)
 0.4342(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Si(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C11(H11), C15(H15), C24(H24), C27(H27), C30(H30), C43(H43), C47(H47),
 C56(H56), C59(H59), C62(H62)
3.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C22(H22), C52(H52), C54(H54)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              15443
_shelx_hkl_checksum              35300
_olex2_submission_special_instructions 'No special instructions were received'