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_7122753
_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         'C19 H36 Cl Ir N2 Si'
_chemical_formula_sum            'C19 H36 Cl Ir N2 Si'
_chemical_formula_weight         548.24
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.3885(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.6082(5)
_cell_length_b                   18.4684(6)
_cell_length_c                   17.6685(5)
_cell_measurement_reflns_used    53726
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.1
_cell_volume                     4407.5(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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0700
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52087
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.868
_exptl_absorpt_coefficient_mu    6.238
_exptl_absorpt_correction_T_max  0.602455
_exptl_absorpt_correction_T_min  0.458390
_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            red
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether'
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.905
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         10066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+12.9967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8923
_reflns_number_total             10066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09178a2.cif
_cod_data_source_block           complex-1
_cod_database_code               7122753
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.417
_shelx_estimated_absorpt_t_max   0.669
_shelx_res_checksum              55441
_shelx_hkl_checksum              40620