Kinetic Analysis and Sequencing of Si-H and C-H Bond Activation Reactions: Direct Silylation of Arenes Catalyzed by an Iridium-Polyhydride.
Esteruelas, Miguel A.; Martínez, Antonio; Oliván, Montserrat; Oñate, Enrique; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c07578

data_4135329
_publ_section_title
;
 Kinetic Analysis and Sequencing of Si-H and C-H Bond Activation
 Reactions: Direct Silylation of Arenes Catalyzed by an
 Iridium-Polyhydride.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c07578
_journal_year                    2020
_chemical_formula_sum            'C34 H63 Ir O3 P2 Si3'
_chemical_formula_weight         858.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 96.485(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.509(2)
_cell_length_b                   18.340(3)
_cell_length_c                   15.539(3)
_cell_measurement_reflns_used    4973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     4108.4(12)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1015
_diffrn_reflns_av_unetI/netI     0.1751
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47825
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         29.702
_diffrn_reflns_theta_min         1.319
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.444
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       'irregilar block'
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.119
_refine_diff_density_max         3.036
_refine_diff_density_min         -3.230
_refine_diff_density_rms         0.227
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.021(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         21062
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0427P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                12877
_reflns_number_total             21062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c07578_si_003.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        4108.6(12)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4135329
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.587
_shelx_estimated_absorpt_t_max   0.685
_shelx_res_checksum              54400
_shelx_hkl_checksum              76843