Cu-catalyzed one-pot synthesis of fused oxazepinone derivatives via sp2 C–H and O–H cross-dehydrogenative coupling
Zhang, Zeyuan; Dai, Zhen; Ma, Xinkun; Liu, Yihan; Ma, Xiaojun; Li, Wanli; Ma, Chen; Organic Chemistry Frontiers 3 (2016) 799–; doi:10.1039/C6QO00040A

data_1553432
_publ_section_title
;
 Cu-catalyzed one-pot synthesis of fused oxazepinone derivatives via sp2
 C--H and O--H cross-dehydrogenative coupling
;
_journal_issue                   7
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              799
_journal_paper_doi               10.1039/C6QO00040A
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C22 H13 Cl N2 O2, C H2 Cl2'
_chemical_formula_sum            'C23 H15 Cl3 N2 O2'
_chemical_formula_weight         457.72
_chemical_name_common            4a
_chemical_name_systematic        4a
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-22 deposited with the CCDC.
2016-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7032(10)
_cell_length_b                   16.441(2)
_cell_length_c                   14.9629(18)
_cell_measurement_reflns_used    2674
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.108
_cell_measurement_theta_min      2.743
_cell_volume                     1895.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.1332
_diffrn_reflns_av_sigmaI/netI    0.1707
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9190
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.509
_exptl_crystal_colour            clolorless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3058
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1592
_reflns_number_gt                2069
_reflns_number_total             3058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qo00040a2.cif
_cod_data_source_block           p
_cod_database_code               1553432