Palladium-Catalyzed Intermolecular Trans-Selective Carbofunctionalization of Internal Alkynes to Highly Functionalized Alkenes
Lv, Weiwei; Liu, Shihan; Chen, Yanhui; Wen, Si; Lan, Yu; Cheng, Guolin; ACS Catalysis  (2020) 10516–; doi:10.1021/acscatal.0c02522

data_4517994
_publ_section_title
;
 Palladium-Catalyzed Intermolecular Trans-Selective Carbofunctionalization
 of Internal Alkynes to Highly Functionalized Alkenes
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              10516
_journal_paper_doi               10.1021/acscatal.0c02522
_journal_year                    2020
_chemical_formula_moiety         'C27 H34 Si2'
_chemical_formula_sum            'C27 H34 Si2'
_chemical_formula_weight         414.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.06
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.963(3)
_cell_length_b                   12.0779(15)
_cell_length_c                   28.792(5)
_cell_measurement_reflns_used    2356
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.43
_cell_volume                     5024.6(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.783
_diffrn_measured_fraction_theta_max 0.783
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.1116
_diffrn_reflns_av_sigmaI/netI    0.1477
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            12399
_diffrn_reflns_theta_full        25.56
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Colorless
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0072P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                2090
_reflns_number_total             4721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs0c02522_si_003.cif
_cod_data_source_block           lvvv_0ma
_cod_original_cell_volume        5024.8(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4517994