Iron complexes supported by silyl-NHC chelate ligands: synthesis and use for double hydroboration of nitriles.
Komuro, Takashi; Hayasaka, Kohei; Takahashi, Kasumi; Ishiwata, Nozomu; Yamauchi, Kota; Tobita, Hiromi; Hashimoto, Hisako; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4041–4047; doi:10.1039/d3dt03605g

data_7715385
_publ_section_title
;
 Iron complexes supported by silyl-NHC chelate ligands: synthesis and use
 for double hydroboration of nitriles.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4041
_journal_page_last               4047
_journal_paper_doi               10.1039/d3dt03605g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C37 H51 Fe N3 O3 Si, C4 H8 O'
_chemical_formula_sum            'C41 H59 Fe N3 O4 Si'
_chemical_formula_weight         741.85
_chemical_properties_physical    Air-sensitive
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.728(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5838(5)
_cell_length_b                   8.8169(4)
_cell_length_c                   33.9397(11)
_cell_measurement_reflns_used    7612
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.3410
_cell_measurement_theta_min      2.0740
_cell_volume                     4017.8(3)
_computing_cell_refinement
;
'CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)'
;
_computing_data_collection
;
'CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)'
;
_computing_data_reduction
;
'CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)'
;
_computing_molecular_graphics
;
'ORTEP-3', 'Yadokari-XG (Wakita, Nemoto et al., 2009)'
;
_computing_publication_material
;
'Yadokari-XG (Wakita, Nemoto et al., 2009)'
;
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'DIRDIF-2008 (PATTY)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            34543
_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         27.484
_diffrn_reflns_theta_min         2.082
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0482P)^2^+3.6685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6234
_reflns_number_total             9223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03605g2.cif
_cod_data_source_block           complex-5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7715385
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.974
_oxdiff_exptl_absorpt_empirical_full_min 0.932
_oxdiff_exptl_absorpt_empirical_full_max 1.106
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              38923