Palladium-catalyzed selective C-C bond cleavage of keto-vinylidenecyclopropanes: construction of structurally rich dihydrofurans and tetrahydrofurans.
Ning, Chao; Yu, Ziqi; Shi, Min; Wei, Yin; Chemical science 15 (2024) 9192–9200; doi:10.1039/d4sc02536a

data_1571631
_publ_section_title
;
 Palladium-catalyzed selective C-C bond cleavage of
 keto-vinylidenecyclopropanes: construction of structurally rich
 dihydrofurans and tetrahydrofurans.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              9192
_journal_page_last               9200
_journal_paper_doi               10.1039/d4sc02536a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C17 H21 N O3 S'
_chemical_formula_weight         319.41
_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   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2022-09-13 deposited with the CCDC.	2024-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.9460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3144(3)
_cell_length_b                   12.2204(4)
_cell_length_c                   13.0932(4)
_cell_measurement_reflns_used    6946
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      54.664
_cell_measurement_theta_min      4.562
_cell_volume                     1648.17(9)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0695
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19731
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.586
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3222
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0474P)^2^+0.7903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2702
_reflns_number_total             3222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02536a2.cif
_cod_data_source_block           mo_d8v22340_0m
_cod_depositor_comments
'Adding full bibliography for 1571631--1571632.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1571631
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-4
_shelx_res_checksum              19470