Silyl‒pyridine‒amine pincer-ligated iridium complexes for catalytic silane deuteration via room temperature C‒D bond activation of benzene-d6
Komuro, Takashi; Osawa, Tomohiro; Suzuki, Ryuju; Mochizuki, Daiki; Higashi, Hironori; Tobita, Hiromi; Chemical Communications  (2018) –; doi:10.1039/C8CC09178A

data_7122755
_publ_section_title
;
 Silyl--pyridine--amine pincer-ligated iridium complexes for catalytic
 silane deuteration via room temperature C--D bond activation of
 benzene-d6
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09178A
_journal_year                    2018
_chemical_formula_moiety         'C26 H46 Cl Ir N4 Si, C7 H8, 0.5(C7 H8)'
_chemical_formula_sum            'C36.5 H58 Cl Ir N4 Si'
_chemical_formula_weight         808.61
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-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'
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-12-08 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.7314(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4572(4)
_cell_length_b                   10.2996(3)
_cell_length_c                   25.5865(9)
_cell_measurement_reflns_used    63749
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     3765.8(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'DIRDIF-2008 (PATTY)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            42766
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         1.982
_exptl_absorpt_coefficient_mu    3.678
_exptl_absorpt_correction_T_max  0.743431
_exptl_absorpt_correction_T_min  0.539177
_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            orange
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             1652
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.694
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         8619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0181P)^2^+12.7936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7860
_reflns_number_total             8619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09178a2.cif
_cod_data_source_block           complex-2
_cod_original_formula_sum        'C36.50 H58 Cl Ir N4 Si'
_cod_database_code               7122755
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.542
_shelx_estimated_absorpt_t_max   0.783
_shelx_res_checksum              59375
_shelx_hkl_checksum              52668