Collective synthesis of aspulvinone and its analogues by vinylogous aldol condensation of substituted tetronic acids with aldehydes.
Yu, Xiaotan; Gu, Xiaoxia; Zhao, Yunpeng; Wang, Fengqing; Sun, Weiguang; Qi, Changxing; Gu, Lianghu; Zhang, Yonghui; RSC advances 13 (2023) 4859–4864; doi:10.1039/d2ra08133d

data_7246391
_publ_section_title
;
 Collective synthesis of aspulvinone and its analogues by vinylogous aldol
 condensation of substituted tetronic acids with aldehydes.
;
_journal_issue                   7
_journal_name_full               'RSC advances'
_journal_page_first              4859
_journal_page_last               4864
_journal_paper_doi               10.1039/d2ra08133d
_journal_volume                  13
_journal_year                    2023
_chemical_formula_sum            'C40 H34 O7'
_chemical_formula_weight         626.67
_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-2014/7
_audit_update_record
;
2022-09-01 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                70.624(2)
_cell_angle_beta                 84.081(2)
_cell_angle_gamma                82.783(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5414(2)
_cell_length_b                   13.4295(3)
_cell_length_c                   13.5307(3)
_cell_measurement_reflns_used    19990
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.506
_cell_measurement_theta_min      3.475
_cell_volume                     1619.12(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  ccd
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36514
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.590
_diffrn_reflns_theta_max         66.590
_diffrn_reflns_theta_min         3.470
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       Block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   0.864
_exptl_transmission_factor_min   0.864
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0599P)^2^+0.8740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5220
_reflns_number_total             5700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra08133d2.cif
_cod_data_source_block           1_a_CCDC2
_cod_database_code               7246391
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.871
_shelx_estimated_absorpt_t_max   0.871
_shelx_res_checksum              57182