One-Pot Reaction of Carboxylic Acids and Ynol Ethers for The Synthesis of β-Keto Esters.
Zeng, Linwei; Lai, Zhencheng; Cui, Sunliang; The Journal of organic chemistry 83 (2018) 14834–14841; doi:10.1021/acs.joc.8b02715

data_4035706
_publ_section_title
;
 One-Pot Reaction of Carboxylic Acids and Ynol Ethers for The Synthesis of
 \b-Keto Esters.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              14834
_journal_page_last               14841
_journal_paper_doi               10.1021/acs.joc.8b02715
_journal_volume                  83
_journal_year                    2018
_chemical_formula_sum            'C17 H16 O3'
_chemical_formula_weight         268.30
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           Orthorhombic'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   18.775(7)
_cell_length_b                   10.002(4)
_cell_length_c                   31.332(12)
_cell_measurement_reflns_used    953
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.11
_cell_measurement_theta_min      2.53
_cell_volume                     5884(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL(Sheldrick, 2008)'
_computing_publication_material  'WINGX (Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare,1999)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX2 CCD area-detector diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.2792
_diffrn_reflns_av_sigmaI/netI    0.1746
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            40045
_diffrn_reflns_theta_full        27.72
_diffrn_reflns_theta_max         27.72
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9797
_exptl_absorpt_correction_T_min  0.9741
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.3378
_refine_ls_R_factor_gt           0.0896
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0983P)^2^+4.4400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.3219
_reflns_number_gt                1573
_reflns_number_total             6809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo8b02715_si_002.cif
_cod_data_source_block           1_a
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4035706