Synthesis of oxazolidine-2,4-diones by a tandem phosphorus-mediated carboxylative condensation-cyclization reaction using atmospheric carbon dioxide
Wen-Zhen Zhang; Tian Xia; Xu-Tong Yang; Xiao-Bing Lu; Chem.Commun. 51 (2015) 6175–; doi:10.1039/C5cc01530H

data_7116887
_publ_section_title
;
 Synthesis of oxazolidine-2,4-diones by a tandem phosphorus-mediated
 carboxylative condensation-cyclization reaction using atmospheric carbon
 dioxide
;
_journal_name_full               Chem.Commun.
_journal_page_first              6175
_journal_paper_doi               10.1039/C5cc01530H
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C16 H12 Cl N O3'
_chemical_formula_weight         301.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-17 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                78.123(5)
_cell_angle_beta                 81.589(5)
_cell_angle_gamma                61.978(5)
_cell_formula_units_Z            4
_cell_length_a                   10.3981(8)
_cell_length_b                   10.4368(8)
_cell_length_c                   15.4169(12)
_cell_measurement_temperature    296(2)
_cell_volume                     1442.9(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13130
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.273
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0693P)^2^+0.0896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1528
_reflns_number_gt                3608
_reflns_number_total             6559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01530h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1442.95(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7116887