Rhodium(III)-catalyzed C-H activation/[4+3] annulation of N-phenoxyacetamides and alpha,beta-unsaturated aldehydes: an efficient route to 1,2-oxazepines at room temperature
Pingping Duan; Xia Lan; Ying Chen; Shao-Song Qian; Jie Jack Li; Liang Lu; Yanbo Lu; Bo Chen,; Mei Hong; Jing Zhao; Chem.Commun. 50 (2014) 12135–; doi:10.1039/C4cc05485G

data_7115731
_publ_section_title
;
 Rhodium(III)-catalyzed C-H activation/[4+3] annulation of
 N-phenoxyacetamides and alpha,beta-unsaturated aldehydes: an efficient
 route to 1,2-oxazepines at room temperature
;
_journal_name_full               Chem.Commun.
_journal_page_first              12135
_journal_paper_doi               10.1039/C4cc05485G
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C11 H17 N O3'
_chemical_formula_weight         211.25
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.070(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9758(10)
_cell_length_b                   6.7000(5)
_cell_length_c                   14.3713(11)
_cell_measurement_reflns_used    4417
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.10
_cell_measurement_theta_min      6.60
_cell_volume                     1083.10(16)
_computing_cell_refinement       'CrystalClear-SM Auto 2.0 r4'
_computing_data_collection       'CrystalClear-SM 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Auto 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.777
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Rigaku Saturn944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.777
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5306
_diffrn_reflns_point_group_measured_fraction_full 0.777
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         59.966
_diffrn_reflns_theta_min         6.559
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       prism
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.029(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0996
_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^)+(0.1000P)^2^+3.3000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2607
_refine_ls_wR_factor_ref         0.2680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1187
_reflns_number_total             1519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc05485g2.cif
_cod_data_source_block           shelx_1
_cod_database_code               7115731
_shelx_estimated_absorpt_t_min   0.791
_shelx_estimated_absorpt_t_max   0.927
_shelxl_version_number           2013-2
_shelx_res_checksum              85073
_shelx_hkl_checksum              89522