Regioselective Tandem C–H Alkylation/Coupling Reaction of ortho-Iodophenylethylenes via C,C-Pallada(II)cycles
Zhu, Bin-Bin; Ye, Wen-Bo; He, Zhi-Tao; Zhang, Shu-Sheng; Feng, Chen-Guo; Lin, Guo-Qiang; ACS Catalysis 11 (2021) 12123–12132; doi:10.1021/acscatal.1c03386

data_4519059
_publ_section_title
;
 Regioselective Tandem C--H Alkylation/Coupling Reaction of
 ortho-Iodophenylethylenes via C,C-Pallada(II)cycles
;
_journal_issue                   19
_journal_name_full               'ACS Catalysis'
_journal_page_first              12123
_journal_page_last               12132
_journal_paper_doi               10.1021/acscatal.1c03386
_journal_volume                  11
_journal_year                    2021
_chemical_formula_sum            'C35 H56 Cl2 P2 Pd'
_chemical_formula_weight         716.03
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 100.8120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7183(4)
_cell_length_b                   14.6907(5)
_cell_length_c                   21.1331(7)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      54.966
_cell_measurement_theta_min      4.496
_cell_volume                     3573.5(2)
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45948
_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         25.997
_diffrn_reflns_theta_min         2.403
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.059
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7016
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0521P)^2^+6.5280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6175
_reflns_number_total             7016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c03386_si_002.cif
_cod_data_source_block           mo_d8v20320_0m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4519059
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.955
_shelxl_version_number           2013-4
_shelx_res_checksum              93810
_shelx_hkl_checksum              19974