Photocatalyzed, β-Selective Hydrocarboxylation of α,β-Unsaturated Esters with CO2 under Flow for β-Lactone Synthesis
Kang, Guowei; Romo, Daniel; ACS Catalysis  (2021) 1309–1315; doi:10.1021/acscatal.0c05050

data_4518474
_publ_section_title
;
 Photocatalyzed, \b-Selective Hydrocarboxylation of \a,\b-Unsaturated
 Esters with CO2 under Flow for \b-Lactone Synthesis
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              1309
_journal_page_last               1315
_journal_paper_doi               10.1021/acscatal.0c05050
_journal_year                    2021
_chemical_formula_sum            'C13 H19 N O4'
_chemical_formula_weight         253.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.116(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.6772(10)
_cell_length_b                   13.7805(9)
_cell_length_c                   16.5498(12)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.46
_cell_volume                     2663.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19811
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         1.923
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.6098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4963
_reflns_number_total             5425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05050_si_004.cif
_cod_data_source_block           DR54AB
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4518474
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2013-4
_shelx_res_checksum              67904
_shelx_hkl_checksum              94000