Palladium-Catalyzed Intermolecular Alkynylcarbonylation of Unactivated Alkenes: Easy Access to β-Alkynylcarboxylic Esters
Li, Xiang; Chen, Pinhong; Liu, Guosheng; Chemical Communications  (2022) –; doi:10.1039/D1CC07092D

data_7129605
_publ_section_title
;
 Palladium-Catalyzed Intermolecular Alkynylcarbonylation of Unactivated
 Alkenes: Easy Access to \b-Alkynylcarboxylic Esters
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC07092D
_journal_year                    2022
_chemical_formula_sum            'C27 H38 O5 Si'
_chemical_formula_weight         470.66
_chemical_name_systematic
'methyl 6-((2-oxo-2H-chromen-4-yl)oxy)-3-((triisopropylsilyl)ethynyl)hexanoate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc29ghx6
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-12-16 deposited with the CCDC.	2022-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                109.976(2)
_cell_angle_beta                 113.932(2)
_cell_angle_gamma                98.587(2)
_cell_formula_units_Z            4
_cell_length_a                   13.9071(10)
_cell_length_b                   14.9140(12)
_cell_length_c                   16.1401(13)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      54.925
_cell_measurement_theta_min      5.348
_cell_volume                     2709.4(4)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37764
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.700
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0076(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         10067
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0727
_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^)+(0.0729P)^2^+2.5746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6856
_reflns_number_total             10067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc07092d2.cif
_cod_data_source_block           mo_d8v19162_0m
_cod_database_code               7129605
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2013-4
_shelx_res_checksum              50975
_shelx_hkl_checksum              34149