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_4025247
_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            'C4 H14 Cl2 N2 Pd'
_chemical_formula_weight         267.47
_chemical_name_systematic
; 
 ? 
;
_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                 98.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.7022(15)
_cell_length_b                   6.0157(12)
_cell_length_c                   10.457(2)
_cell_measurement_temperature    293(2)
_cell_volume                     479.22(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3580
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         3.92
_exptl_absorpt_coefficient_mu    2.425
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             264
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0618P)^2^+0.0577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                833
_reflns_number_total             859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo902636g_si_001.cif
_cod_data_source_block           3
_cod_original_cell_volume        479.22(16)
_cod_database_code               4025247