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_7715383
_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         'C29 H44 Fe N2 O3 Si'
_chemical_formula_sum            'C29 H44 Fe N2 O3 Si'
_chemical_formula_weight         552.60
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                105.0205(18)
_cell_angle_beta                 96.1600(10)
_cell_angle_gamma                99.7320(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5500(4)
_cell_length_b                   11.3730(6)
_cell_length_c                   16.0634(6)
_cell_measurement_reflns_used    19658
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.9
_cell_volume                     1468.06(12)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_molecular_graphics
;
'Mercury 4.0 (Macrae et al., 2020)', '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_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1276
_diffrn_reflns_av_unetI/netI     0.1041
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22916
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.441
_diffrn_reflns_theta_min         1.329
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.976550
_exptl_absorpt_correction_T_min  0.889679
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera.
Rigaku Corporation, Tokyo, Japan.
HIGASHI, T. (1999). Numabs - Numerical Absorption Correction, 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0688
_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^)+(0.0345P)^2^+1.3431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5040
_reflns_number_total             6676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03605g2.cif
_cod_data_source_block           complex-1
_cod_database_code               7715383
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              93132