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_7125251
_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_formula_moiety         'C20 H30 N2 O Si2'
_chemical_formula_sum            'C20 H30 N2 O Si2'
_chemical_formula_weight         370.64
_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'
_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                 100.934(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5738(8)
_cell_length_b                   10.3894(4)
_cell_length_c                   12.0069(5)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      2.56
_cell_volume                     2152.44(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.971
_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  0.0406
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
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_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.282
_diffrn_reflns_theta_min         2.561
_exptl_absorpt_coefficient_mu    1.562
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0495
_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^)+(0.0906P)^2^+0.6209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3350
_reflns_number_total             3834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07885k2.cif
_cod_data_source_block           t_0ma
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7125251
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.696
_shelx_estimated_absorpt_t_max   0.745
_shelx_res_checksum              66405