One-Pot CuI/DBU-Catalyzed Carboxylative Cyclization toward Oxazolidinones Using Recyclable Molecular Sieves as Efficient Promoters for Fixation of CO2 in Water Medium
Liu, Yu-Te; Cheng, Chi-Wei; Lu, Huan-Chang; Chang, Ting-Yu; Chen, Chun-Ying; Yang, Hao-Chun; Yu, Shih-Hsien; Zehra, Syeda; Liu, Shu-Hui; Leung, Man-Kit; Lee, Kwang-Ming; Chen, Hsiu-Hui; The Journal of Organic Chemistry  (2020) –; doi:10.1021/acs.joc.0c01833

data_4038890
_publ_section_title
;
 One-Pot CuI/DBU-Catalyzed Carboxylative Cyclization toward Oxazolidinones
 Using Recyclable Molecular Sieves as Efficient Promoters for Fixation of
 CO2 in Water Medium
;
_journal_name_full               'The Journal of Organic Chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01833
_journal_year                    2020
_chemical_formula_sum            'C29 H23 N O2'
_chemical_formula_weight         417.48
_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-2017/1
_cell_angle_alpha                88.042(6)
_cell_angle_beta                 84.239(7)
_cell_angle_gamma                78.625(6)
_cell_formula_units_Z            2
_cell_length_a                   6.1618(5)
_cell_length_b                   8.7522(6)
_cell_length_c                   20.3805(17)
_cell_measurement_reflns_used    1274
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.2580
_cell_measurement_theta_min      3.6150
_cell_volume                     1071.96(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.2496
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.1444
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            5180
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.014
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0575P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2509
_reflns_number_total             5180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01833_si_002.cif
_cod_data_source_block           ic19786
_cod_database_code               4038890
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              43988
_shelx_hkl_checksum              89836