Pd(II)-Catalyzed Highly Regio- and Stereoselective Assembly of C-C Double Bonds: An Efficient Method for the Synthesis of 2,4-Dihalo-1,3,5-trienes from Alkynols.
Jiang, Huanfeng; Gao, Yang; Wu, Wanqing; Huang, Yubing; Organic letters 15 (2013) 238–241; doi:10.1021/ol302730x

data_1508841
_publ_section_title
;
 Pd(II)-Catalyzed Highly Regio- and Stereoselective Assembly of C-C Double
 Bonds: An Efficient Method for the Synthesis of 2,4-Dihalo-1,3,5-trienes
 from Alkynols.
;
_journal_issue                   2
_journal_name_full               'Organic letters'
_journal_page_first              238
_journal_page_last               241
_journal_paper_doi               10.1021/ol302730x
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C26 H24'
_chemical_formula_weight         336.45
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 95.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.406(2)
_cell_length_b                   5.8201(12)
_cell_length_c                   15.187(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1003.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9091
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.9938
_exptl_absorpt_correction_T_min  0.9876
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0978P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1767
_reflns_number_gt                946
_reflns_number_total             2287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol302730x_si_002.cif
_cod_data_source_block           gy
_cod_original_cell_volume        1003.5(4)
_cod_database_code               1508841