Rapid Assembly of Tetrasubstituted Furans via Pummerer-Type Rearrangement.
Haut, Franz-Lucas; Habiger, Christoph; Wein, Lukas A.; Wurst, Klaus; Podewitz, Maren; Magauer, Thomas; Journal of the American Chemical Society 143 (2021) 1216–1223; doi:10.1021/jacs.0c12194

data_4135576
_publ_section_title
;
 Rapid Assembly of Tetrasubstituted Furans via Pummerer-Type
 Rearrangement.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1216
_journal_page_last               1223
_journal_paper_doi               10.1021/jacs.0c12194
_journal_volume                  143
_journal_year                    2021
_chemical_formula_sum            'C12 H18 O2 S'
_chemical_formula_weight         226.32
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                108.4650(10)
_cell_angle_beta                 102.6140(10)
_cell_angle_gamma                98.5840(10)
_cell_formula_units_Z            8
_cell_length_a                   9.1402(4)
_cell_length_b                   15.4595(7)
_cell_length_c                   19.9824(9)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      23.8
_cell_measurement_theta_min      2.2
_cell_volume                     2539.8(2)
_computing_cell_refinement       'Bruker SAINT-V 8.34A'
_computing_data_collection       'Bruker Apex III'
_computing_data_reduction        'Bruker SAINT-V 8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL-XT-2014/4 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi layered optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39037
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        22.998
_diffrn_reflns_theta_max         22.998
_diffrn_reflns_theta_min         2.241
_diffrn_source                   'Incoatec Microfocus'
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS-2014/5)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         7034
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0407P)^2^+2.7899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5246
_reflns_number_total             7034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c12194_si_002.cif
_cod_data_source_block           11d
_cod_database_code               4135576
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              81842
_shelx_hkl_checksum              58285