Transfer hydrogenation of aldehydes catalyzed by silyl hydrido iron complexes bearing a [PSiP] pincer ligand
Zhang, Peng; Li, Xiaoyan; Qi, Xinghao; Sun, Hongjian; Fuhr, Olaf; Fenske, Dieter; RSC Advances 8 (2018) 14092–; doi:10.1039/C8RA02606H

data_7230486
_publ_section_title
;
 Transfer hydrogenation of aldehydes catalyzed by silyl hydrido iron
 complexes bearing a [PSiP] pincer ligand
;
_journal_issue                   25
_journal_name_full               'RSC Advances'
_journal_page_first              14092
_journal_paper_doi               10.1039/C8RA02606H
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C42 H48 Fe P4 Si'
_chemical_formula_sum            'C42 H48 Fe P4 Si'
_chemical_formula_weight         760.62
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-12-20 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.084(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.7181(7)
_cell_length_b                   18.9232(6)
_cell_length_c                   35.1134(15)
_cell_measurement_reflns_used    11366
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      62.98
_cell_measurement_theta_min      1.26
_cell_volume                     7784.8(6)
_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      200.15
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.806
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '2.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.806
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            26696
_diffrn_reflns_point_group_measured_fraction_full 0.806
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         61.169
_diffrn_reflns_theta_min         2.517
_diffrn_source                   'Cu Genix 3D'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.169
_exptl_absorpt_correction_T_max  0.7670
_exptl_absorpt_correction_T_min  0.5239
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         11341
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0980P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8763
_reflns_number_total             11341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra02606h2.cif
_cod_data_source_block           complex3
_cod_database_code               7230486
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Fe(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si2-H2SI = Si1-H1SI
 1.46 with sigma of 0.01
3.a Riding coordinates:
 Fe1(H1FE), Fe2(H2FE)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C57(H57),
 C58(H58), C59(H59), C60(H60), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68),
  C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76),
 C77(H77), C78(H78)
3.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C79(H79A,H79B,H79C), C80(H80A,
 H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C),
 C84(H84A,H84B,H84C)
;
_shelx_res_checksum              27236
_olex2_submission_special_instructions 'No special instructions were received'