Direct Method to Access Various Functional Arylalkoxysilanes by Rh-catalysed Intermolecular C–H Silylation of Alkoxysilane
Som, Salina; Choi, Jongwook; Katsoulis, Dimitris; Lee, Kangsang L.; Chemical Science  (2022) –; doi:10.1039/D2SC03727K

data_1567523
_publ_section_title
;
 Direct Method to Access Various Functional Arylalkoxysilanes by
 Rh-catalysed Intermolecular C--H Silylation of Alkoxysilane
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03727K
_journal_year                    2022
_chemical_formula_sum            'C68 H72 P4 Rh2'
_chemical_formula_weight         1218.95
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-04-13 deposited with the CCDC.	2022-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1998(4)
_cell_length_b                   18.0969(5)
_cell_length_c                   24.5076(8)
_cell_measurement_reflns_used    4346
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.27
_cell_volume                     5854.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.1429
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27044
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.380
_diffrn_reflns_theta_min         1.399
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       plate
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
; 
 Flack x determined using 2550 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.701
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         11938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.701
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0483P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                7779
_reflns_number_total             11938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03727k2.cif
_cod_data_source_block           bv091616
_cod_database_code               1567523
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              67982