A silver-catalyzed domino inverse electron-demand oxo-Diels-Alder reaction of 3-cyclopropylideneprop-2-en-1-ones with 2,3-dioxopyrrolidines via cyclobutane-fused furan.
Zhang, Yanshun; Wei, Yin; Shi, Min; Chemical communications (Cambridge, England) 57 (2021) 3599–3602; doi:10.1039/d1cc00707f

data_7128010
_publ_section_title
;
 A silver-catalyzed domino inverse electron-demand oxo-Diels-Alder
 reaction of 3-cyclopropylideneprop-2-en-1-ones with 2,3-dioxopyrrolidines
 via cyclobutane-fused furan.
;
_journal_issue                   29
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3599
_journal_page_last               3602
_journal_paper_doi               10.1039/d1cc00707f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_sum            'C34 H27 N O3 S'
_chemical_formula_weight         529.62
_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-2013
_audit_update_record
;
2020-12-25 deposited with the CCDC.	2021-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                69.3010(10)
_cell_angle_beta                 88.1310(10)
_cell_angle_gamma                67.2510(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5667(4)
_cell_length_b                   10.7003(5)
_cell_length_c                   13.9406(6)
_cell_measurement_reflns_used    9003
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.289
_cell_measurement_theta_min      4.393
_cell_volume                     1349.84(10)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_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  0.0758
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23056
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.105
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.025(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5000
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0970P)^2^+0.8710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3913
_reflns_number_total             5000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00707f2.cif
_cod_data_source_block           mo_d8v20824_0m
_cod_depositor_comments          'Adding full bibliography for 7128010.cif.'
_cod_database_code               7128010
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2013-4
_shelx_res_checksum              16180
_shelx_hkl_checksum              45092