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_7110251
_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            'C8 H9 Br O2'
_chemical_formula_weight         217.06
_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                 103.620(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.8136(2)
_cell_length_b                   20.7534(8)
_cell_length_c                   7.4685(3)
_cell_measurement_temperature    293(2)
_cell_volume                     875.75(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.863
_diffrn_measured_fraction_theta_max 0.863
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5739
_diffrn_reflns_theta_full        29.46
_diffrn_reflns_theta_max         29.46
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    4.642
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             432
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.269
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.3137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                1776
_reflns_number_total             2097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47310d.txt
_cod_data_source_block           1
_cod_depositor_comments
;

2018-02-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C32 H36 Br4 O8'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     868.25
_cod_database_code               7110251