Palladium-catalyzed direct intermolecular silylation of remote unactivated C(sp<sup>3</sup>)-H bonds.
Pan, Jin-Long; Li, Quan-Zhe; Zhang, Ting-Yu; Hou, Si-Hua; Kang, Jun-Cheng; Zhang, Shu-Yu; Chemical communications (Cambridge, England) 52 (2016) 13151–13154; doi:10.1039/c6cc07885k

data_7125252
_publ_section_title
;
 Palladium-catalyzed direct intermolecular silylation of remote
 unactivated C(sp<sup>3</sup>)-H bonds.
;
_journal_issue                   89
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13151
_journal_page_last               13154
_journal_paper_doi               10.1039/c6cc07885k
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H29 N3 O3 Si'
_chemical_formula_sum            'C26 H29 N3 O3 Si'
_chemical_formula_weight         459.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-06 deposited with the CCDC.
2016-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.8407(9)
_cell_length_b                   11.7200(3)
_cell_length_c                   10.6590(2)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.28
_cell_measurement_theta_min      3.93
_cell_volume                     4976.53(19)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25688
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.366
_diffrn_reflns_theta_min         3.931
_exptl_absorpt_coefficient_mu    1.086
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 3233 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.044(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8653
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+6.8189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                7696
_reflns_number_total             8653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07885k2.cif
_cod_data_source_block           t_0m
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7125252
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.812
_shelx_estimated_absorpt_t_max   0.812
_shelx_res_checksum              50665