PdCl2(HNMe2)2-Catalyzed Highly Selective Cross [2 + 2 + 2] Cyclization of Alkynoates and Alkenes under Molecular Oxygen
Yanxia Shen; Huanfeng Jiang; Zhengwang Chen; Journal of Organic Chemistry 75 (2010) 1321–1324; doi:10.1021/jo902636g

data_4025248
_publ_section_title
;
 PdCl2(HNMe2)2-Catalyzed Highly Selective Cross [2 + 2 + 2] Cyclization of
 Alkynoates and Alkenes under Molecular Oxygen
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1321
_journal_page_last               1324
_journal_paper_doi               10.1021/jo902636g
_journal_volume                  75
_journal_year                    2010
_chemical_formula_sum            'C21 H18 O10'
_chemical_formula_weight         430.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 104.32(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.620(3)
_cell_length_b                   19.411(4)
_cell_length_c                   8.0165(16)
_cell_measurement_temperature    293(2)
_cell_volume                     2053.5(8)
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16049
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.9768
_exptl_absorpt_correction_T_min  0.9659
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+0.2974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                2458
_reflns_number_total             3695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo902636g_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        2053.6(7)
_cod_database_code               4025248