Palladium-catalyzed intermolecular [4 + 2] formal cycloaddition with (Z)-3-iodo allylic nucleophiles and allenamides.
Yan, Fachao; Liang, Hanbing; Ai, Bing; Liang, Wenjing; Jiao, Luyang; Yao, Shuzhi; Zhao, Pingping; Liu, Qing; Dong, Yunhui; Liu, Hui; Organic & biomolecular chemistry 17 (2019) 2651–2656; doi:10.1039/c8ob03072c

data_7156693
_publ_section_title
;
 Palladium-catalyzed intermolecular [4 + 2] formal cycloaddition with
 (Z)-3-iodo allylic nucleophiles and allenamides.
;
_journal_issue                   10
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2651
_journal_page_last               2656
_journal_paper_doi               10.1039/c8ob03072c
_journal_volume                  17
_journal_year                    2019
_chemical_formula_sum            'C24 H27 N O3 S'
_chemical_formula_weight         409.53
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-04-17 deposited with the CCDC.
2019-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                92.060(5)
_cell_angle_beta                 111.910(5)
_cell_angle_gamma                102.119(5)
_cell_formula_units_Z            2
_cell_length_a                   8.9412(15)
_cell_length_b                   11.6147(19)
_cell_length_c                   11.727(2)
_cell_measurement_temperature    296(2)
_cell_volume                     1095.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8204
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.172
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             436
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.2406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                2442
_reflns_number_total             3840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ob03072c2.cif
_cod_data_source_block           mo_ww1_0m
_cod_depositor_comments          'Adding full bibliography for 7156693.cif.'
_cod_database_code               7156693