Gold-Catalyzed Intramolecular Regioselective 7-exo-dig Cyclization To Access 3-Methylene-3,4-dihydrobenzo[b]oxepinones.
Mangina, N. S. V. M. Rao; Kadiyala, Veerabhushanam; Guduru, Ravinder; Goutham, Kommuru; Sridhar, Balasubramanian; Karunakar, Galla V.; Organic letters 19 (2017) 282–285; doi:10.1021/acs.orglett.6b03433

data_1544943
_publ_section_title
;
 Gold-Catalyzed Intramolecular Regioselective 7-exo-dig Cyclization To
 Access 3-Methylene-3,4-dihydrobenzo[b]oxepinones.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              282
_journal_page_last               285
_journal_paper_doi               10.1021/acs.orglett.6b03433
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C28 H24 N2 O2'
_chemical_formula_sum            'C28 H24 N2 O2'
_chemical_formula_weight         420.49
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 112.2960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5420(9)
_cell_length_b                   8.1490(4)
_cell_length_c                   16.4280(10)
_cell_measurement_reflns_used    5360
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      22.77
_cell_measurement_theta_min      2.37
_cell_volume                     2296.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXL2014 (Sheldrick, 2015)'
_computing_publication_material  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25818
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.302
_diffrn_reflns_theta_min         1.187
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker,2001'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+0.2604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3358
_reflns_number_total             5523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b03433_si_002.cif
_cod_data_source_block           BB85
_cod_depositor_comments          'Adding full bibliography for 1544943.cif.'
_cod_database_code               1544943
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              5300
_shelx_hkl_checksum              86685