Palladium-catalyzed intermolecular [3 + 2] carbocyclization of alkynols and propiolates: an efficient entry to halo-cyclopentadienes
Yang Gao; Wanqing Wu; Huawen Huang; Yubing Huang; Huanfeng Jiang; Chem.Commun. 50 (2014) 846–; doi:10.1039/c3cc47310d

data_7110252
_publ_section_title
;
 Palladium-catalyzed intermolecular [3 + 2] carbocyclization of alkynols
 and propiolates: an efficient entry to halo-cyclopentadienes
;
_journal_name_full               Chem.Commun.
_journal_page_first              846
_journal_paper_doi               10.1039/c3cc47310d
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C15 H20 Br O4'
_chemical_formula_weight         344.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.966(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.76610(10)
_cell_length_b                   11.1691(2)
_cell_length_c                   22.7520(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1464.42(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            21381
_diffrn_reflns_theta_full        29.46
_diffrn_reflns_theta_max         29.46
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    2.818
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             708
_refine_diff_density_max         1.891
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0403P)^2^+4.5624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                3152
_reflns_number_total             3762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47310d.txt
_cod_data_source_block           1a
_cod_database_code               7110252