Palladium-Catalyzed Oxidative Annulation of ortho-Alkenylanilines and Allenes: an Access to Benzo[b]azepines.
Wu, Lisha; Meng, Yinfeng; Ferguson, Jamie; Wang, Lijie; Zeng, Fanlong; The Journal of organic chemistry  (2017) –; doi:10.1021/acs.joc.7b00012

data_4032675
_publ_section_title
;
 Palladium-Catalyzed Oxidative Annulation of ortho-Alkenylanilines and
 Allenes: an Access to Benzo[b]azepines.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.7b00012
_journal_year                    2017
_chemical_formula_moiety         'C31 H27 N O2 S'
_chemical_formula_sum            'C31 H27 N O2 S'
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_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.032
_cell_measurement_theta_min      2.424
_cell_volume                     1240.4(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  \w
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_diffrn_reflns_av_R_equivalents  0.0207
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_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_l_max       13
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_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.097
_diffrn_reflns_theta_max         25.097
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_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.298
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_exptl_transmission_factor_min   0.945
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_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.1398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3425
_reflns_number_total             4376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b00012_si_002.cif
_cod_data_source_block           xb9832_0m
_cod_original_cell_volume        1240.5(7)
_cod_database_code               4032675
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              57677
_shelx_hkl_checksum              53566