Heterolytic cleavage of a Si-H bond by a metal-ligand cooperation of a cationic iridium amido complex and hydrosilylation of aldehydes.
Iizuka, Kosuke; Nakajima, Yumiko; Sato, Kazuhiko; Dalton transactions (Cambridge, England : 2003) 51 (2022) 12781–12785; doi:10.1039/d2dt01733d

data_7711430
_publ_section_title
;
 Heterolytic cleavage of a Si-H bond by a metal-ligand cooperation of a
 cationic iridium amido complex and hydrosilylation of aldehydes.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12781
_journal_page_last               12785
_journal_paper_doi               10.1039/d2dt01733d
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C30 H44 Ir N3 O Si, C F3 O3 S'
_chemical_formula_sum            'C31 H45 F3 Ir N3 O4 S Si'
_chemical_formula_weight         833.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-09 deposited with the CCDC.	2022-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.143(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1347(2)
_cell_length_b                   15.7212(3)
_cell_length_c                   22.1257(4)
_cell_measurement_reflns_used    14602
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      28.8720
_cell_measurement_theta_min      2.4000
_cell_volume                     3470.18(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ORTEP3 for windows'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -16.00   9.00   0.50    8.00    --  -10.90  46.00 -60.00   50
  2  \w   -100.00  79.00   0.50    8.00    --  -10.90  46.00 150.00  358
  3  \w      8.00  73.00   0.50    8.00    --  -10.90  55.00 -30.00  130
  4  \w    -99.00 -74.00   0.50    8.00    --  -10.90  28.00 -90.00   50
  5  \w    -42.00 -17.00   0.50    8.00    --  -10.90  28.00 -90.00   50
  6  \w   -100.00 -55.00   0.50    8.00    --  -10.90  46.00 -60.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0023021000
_diffrn_orient_matrix_UB_12      0.0445500000
_diffrn_orient_matrix_UB_13      -0.0052279000
_diffrn_orient_matrix_UB_21      -0.0335482000
_diffrn_orient_matrix_UB_22      0.0055452000
_diffrn_orient_matrix_UB_23      0.0252754000
_diffrn_orient_matrix_UB_31      0.0626280000
_diffrn_orient_matrix_UB_32      0.0046127000
_diffrn_orient_matrix_UB_33      0.0198550000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25841
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         2.275
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.025
_refine_diff_density_max         3.446
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0447P)^2^+1.7811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5073
_reflns_number_total             6156
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 8.8710\% 
around [-0.33 -0.04 -0.94] (reciprocal) or [-0.88 -0.03 -0.48] (direct)
;
_cod_data_source_file            d2dt01733d2.cif
_cod_data_source_block           2b
_cod_database_code               7711430
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H44 F3 Ir N2 O4 S Si'
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.560
_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
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C18(H18A,H18B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C4(H4), C13(H13), C10(H10), C5(H5), C12(H12), C6(H6)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C15(H15A,H15B,H15C), C19(H19A,H19B,
 H19C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C14(H14A,
 H14B,H14C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              74639
_shelx_hkl_checksum              61274
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.912
_oxdiff_exptl_absorpt_empirical_full_min 0.629
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2