Palladium-catalyzed cascade cyclization of allylamine-tethered alkylidenecyclopropanes: facile access to iodine/difluoromethylene- and perfluoroalkyl-containing 1-benzazepine scaffolds.
Yu, Liu-Zhu; Zhu, Zi-Zhong; Hu, Xu-Bo; Tang, Xiang-Ying; Shi, Min; Chemical communications (Cambridge, England) 52 (2016) 6581–6584; doi:10.1039/c6cc02496c

data_7124629
_publ_section_title
;
 Palladium-catalyzed cascade cyclization of allylamine-tethered
 alkylidenecyclopropanes: facile access to iodine/difluoromethylene- and
 perfluoroalkyl-containing 1-benzazepine scaffolds.
;
_journal_issue                   39
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6581
_journal_page_last               6584
_journal_paper_doi               10.1039/c6cc02496c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C31 H32 F2 I N O4 S'
_chemical_formula_weight         679.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-12-04 deposited with the CCDC.
2016-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.072(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4081(9)
_cell_length_b                   22.6704(15)
_cell_length_c                   19.5045(14)
_cell_measurement_reflns_used    5965
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.301
_cell_measurement_theta_min      4.624
_cell_volume                     6021.2(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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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^)+(0.0747P)^2^+2.6432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_data_source_file            c6cc02496c2.cif
_cod_data_source_block           cd15301
_cod_original_sg_symbol_H-M      'P 21/c'
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_shelx_estimated_absorpt_t_max   0.862
_shelxl_version_number           2013-4
_shelx_res_checksum              83528