Copper-catalyzed oxidative phosphonation of 3,4-dihydro-1,4-benzoxazin-2-ones
Wang, Jie; Li, Jun; Wei, Yuanyuan; Yang, Jingya; Huo, Congde; Organic Chemistry Frontiers 5 (2018) 3534–; doi:10.1039/C8QO01049H

data_1554488
_publ_section_title
;
 Copper-catalyzed oxidative phosphonation of
 3,4-dihydro-1,4-benzoxazin-2-ones
;
_journal_issue                   24
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              3534
_journal_paper_doi               10.1039/C8QO01049H
_journal_volume                  5
_journal_year                    2018
_chemical_formula_sum            'C17 H18 N O5 P'
_chemical_formula_weight         347.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-09-26 deposited with the CCDC.
2018-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                64.045(2)
_cell_angle_beta                 69.351(2)
_cell_angle_gamma                83.294(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5039(7)
_cell_length_b                   10.0075(8)
_cell_length_c                   10.6869(8)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      70.3998
_cell_measurement_theta_min      4.8896
_cell_volume                     854.35(11)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.982
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19530
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.393
_diffrn_reflns_theta_min         4.889
_exptl_absorpt_coefficient_mu    1.665
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       1.10(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3207
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0820
_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^)+(0.1324P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1885
_refine_ls_wR_factor_ref         0.1899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3094
_reflns_number_total             3207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qo01049h2.cif
_cod_data_source_block           HCD4
_cod_database_code               1554488
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.653
_shelx_estimated_absorpt_t_max   0.653
_shelx_res_checksum              22050
_shelx_hkl_checksum              34833