Diastereoselective Synthesis of Dibenzo[b,d]azepines by Pd(II)-Catalyzed [5 + 2] Annulation of o-Arylanilines with Dienes.
Bai, Lu; Wang, Yan; Ge, Yicong; Liu, Jingjing; Luan, Xinjun; Organic letters 19 (2017) 1734–1737; doi:10.1021/acs.orglett.7b00503

data_1545940
_publ_section_title
;
 Diastereoselective Synthesis of Dibenzo[b,d]azepines by Pd(II)-Catalyzed
 [5 + 2] Annulation of o-Arylanilines with Dienes.
;
_journal_issue                   7
_journal_name_full               'Organic letters'
_journal_page_first              1734
_journal_page_last               1737
_journal_paper_doi               10.1021/acs.orglett.7b00503
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C26 H26 N2 O3 S'
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_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
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_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   19.790(10)
_cell_length_c                   13.725(8)
_cell_measurement_reflns_used    1010
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      37.416
_cell_measurement_theta_min      5.220
_cell_volume                     4560(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
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_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12244
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.904
_exptl_absorpt_coefficient_mu    0.173
_exptl_crystal_colour            colorless
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_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1219
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_number_gt                2331
_reflns_number_total             4480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b00503_si_004.cif
_cod_data_source_block           1
_cod_database_code               1545940
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              88220
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