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_7115732
_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_absolute_configuration unk
_chemical_formula_sum            'C18 H24 N O4'
_chemical_formula_weight         318.38
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.347(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7071(2)
_cell_length_b                   4.847
_cell_length_c                   14.6978(10)
_cell_measurement_reflns_used    10447
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.10
_cell_measurement_theta_min      6.60
_cell_volume                     895.67(6)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0314
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10812
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.144
_diffrn_reflns_theta_min         6.576
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       block
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 1284 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.52(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3101
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0949P)^2^+0.0398P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.916
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                2870
_reflns_number_total             3101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc05485g2.cif
_cod_data_source_block           shelx_2
_cod_database_code               7115732
_shelxl_version_number           2013-2
_shelx_res_checksum              95269
_shelx_hkl_checksum              23291