#------------------------------------------------------------------------------ #$Date: 2025-08-19 12:52:15 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301804 $ #$URL: svn://www.crystallography.net/cod/cif/2/21/45/2214526.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2214526 loop_ _publ_author_name 'Zheng, Liang-Wen' 'Dong, Wen-Liang' 'Zhang, Jin-Hua' 'Zhao, Bao-Xiang' _publ_section_title (3E,4E)-3-(1,3-Benzodioxol-5-ylmethylene)-4-(1-phenylethylidene)tetrahydrofuran-2,5-dione _journal_coeditor_code BQ2028 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o3567 _journal_page_last o3567 _journal_paper_doi 10.1107/S160053680703485X _journal_volume 63 _journal_year 2007 _chemical_formula_iupac 'C20 H14 O5' _chemical_formula_moiety 'C20 H14 O5' _chemical_formula_sum 'C20 H14 O5' _chemical_formula_weight 334.31 _chemical_name_systematic ; (3E,4E)-3-(1,3-Benzodioxol-5-ylmethylene)-4-\ (1-phenylethylidene)tetrahydrofuran-2,5-dione ; _space_group_IT_number 33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _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 4 _cell_length_a 7.2201(2) _cell_length_b 18.0627(5) _cell_length_c 12.2046(4) _cell_measurement_reflns_used 3450 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.33 _cell_measurement_theta_min 3.04 _cell_volume 1591.66(8) _computing_cell_refinement APEX2 _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_data_reduction APEX2 _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEXII CCD area-detector' _diffrn_measurement_method '\f and \w' _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 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 9796 _diffrn_reflns_theta_full 27.52 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_min 2.01 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_T_max 0.9934 _exptl_absorpt_correction_T_min 0.9632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'APEX2 (Bruker, 2005)' _exptl_crystal_colour orange--yellow _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 696 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.113 _refine_diff_density_min -0.120 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 1918 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0319 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.053P)^2^+0.0276P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.0863 _reflns_number_gt 1606 _reflns_number_total 1918 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file bq2028.cif _cod_data_source_block I _cod_original_sg_symbol_Hall 'P 2c -2n ' _cod_database_code 2214526 _cod_database_fobs_code 2214526 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy C C1 0.4507(4) 1.08850(14) 0.6981(3) 0.0766(8) Uani d . 1 H H1 0.4852 1.1381 0.6987 0.092 Uiso calc R 1 C C2 0.3315(4) 1.06286(14) 0.6196(3) 0.0746(8) Uani d . 1 H H2 0.2857 1.0950 0.5666 0.090 Uiso calc R 1 C C3 0.2793(3) 0.98960(13) 0.6188(2) 0.0590(6) Uani d . 1 H H3 0.2008 0.9723 0.5641 0.071 Uiso calc R 1 C C4 0.3435(3) 0.94086(11) 0.69979(17) 0.0459(4) Uani d . 1 C C5 0.4666(3) 0.96742(11) 0.77765(19) 0.0501(5) Uani d . 1 H H5 0.5136 0.9357 0.8309 0.060 Uiso calc R 1 C C6 0.5196(4) 1.04076(13) 0.7763(3) 0.0678(7) Uani d . 1 H H6 0.6025 1.0582 0.8287 0.081 Uiso calc R 1 C C7 0.2848(3) 0.86249(11) 0.69894(19) 0.0451(4) Uani d . 1 C C8 0.2857(4) 0.82596(15) 0.5875(2) 0.0653(6) Uani d . 1 H H8A 0.3729 0.7858 0.5874 0.098 Uiso calc R 1 H H8B 0.3207 0.8616 0.5329 0.098 Uiso calc R 1 H H8C 0.1642 0.8073 0.5714 0.098 Uiso calc R 1 C C9 0.2416(3) 0.82442(11) 0.79118(19) 0.0448(4) Uani d . 1 C C10 0.2277(3) 0.74232(13) 0.7893(2) 0.0579(6) Uani d . 1 C C11 0.2485(3) 0.77359(13) 0.9690(2) 0.0578(6) Uani d . 1 C C12 0.2296(3) 0.84388(11) 0.90818(18) 0.0444(4) Uani d . 1 C C13 0.1956(3) 0.90390(11) 0.97086(17) 0.0473(5) Uani d . 1 H H13 0.2022 0.8946 1.0457 0.057 Uiso calc R 1 C C14 0.1507(3) 0.98016(11) 0.94437(16) 0.0438(4) Uani d . 1 C C15 0.0488(2) 1.00096(11) 0.85107(17) 0.0429(4) Uani d . 1 H H15 -0.0007 0.9658 0.8037 0.052 Uiso calc R 1 C C16 0.0257(2) 1.07498(12) 0.83316(17) 0.0445(4) Uani d . 1 C C17 0.1013(3) 1.12780(11) 0.9026(2) 0.0522(5) Uani d . 1 C C18 0.1941(3) 1.10943(12) 0.9952(2) 0.0618(6) Uani d . 1 H H18 0.2411 1.1453 1.0423 0.074 Uiso calc R 1 C C19 0.2157(3) 1.03414(12) 1.01647(19) 0.0544(5) Uani d . 1 H H19 0.2751 1.0195 1.0805 0.065 Uiso calc R 1 C C20 -0.0455(4) 1.18660(13) 0.7682(2) 0.0692(7) Uani d . 1 H H20A 0.0160 1.2098 0.7063 0.083 Uiso calc R 1 H H20B -0.1664 1.2092 0.7767 0.083 Uiso calc R 1 O O1 -0.0653(2) 1.10928(8) 0.74889(14) 0.0585(4) Uani d . 1 O O2 0.0608(3) 1.19719(8) 0.86474(16) 0.0709(5) Uani d . 1 O O3 0.2660(3) 0.76142(11) 1.06471(17) 0.0809(6) Uani d . 1 O O4 0.2406(3) 0.71527(9) 0.89574(18) 0.0691(5) Uani d . 1 O O5 0.2125(3) 0.69889(10) 0.71649(18) 0.0878(7) Uani d . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0858(17) 0.0437(12) 0.100(2) -0.0096(11) 0.0383(18) -0.0003(16) C2 0.0857(17) 0.0588(14) 0.0794(19) 0.0115(13) 0.0310(16) 0.0223(15) C3 0.0655(12) 0.0621(13) 0.0495(12) 0.0050(10) 0.0081(11) 0.0086(12) C4 0.0498(10) 0.0477(10) 0.0401(10) 0.0006(8) 0.0098(9) -0.0006(9) C5 0.0456(10) 0.0530(11) 0.0518(12) -0.0043(8) 0.0075(10) -0.0038(10) C6 0.0630(14) 0.0603(14) 0.0801(19) -0.0166(11) 0.0202(14) -0.0152(14) C7 0.0472(9) 0.0465(10) 0.0416(10) -0.0012(8) 0.0001(9) -0.0047(10) C8 0.0885(16) 0.0634(14) 0.0439(12) -0.0034(12) 0.0010(12) -0.0127(12) C9 0.0478(10) 0.0408(10) 0.0458(11) -0.0037(7) 0.0021(9) -0.0055(10) C10 0.0686(13) 0.0465(12) 0.0585(14) -0.0100(10) 0.0083(12) -0.0055(13) C11 0.0696(13) 0.0483(13) 0.0556(15) 0.0053(10) 0.0036(11) 0.0049(12) C12 0.0491(9) 0.0416(10) 0.0427(11) -0.0008(8) 0.0009(9) 0.0026(10) C13 0.0548(10) 0.0505(11) 0.0365(10) 0.0022(9) 0.0004(9) 0.0017(9) C14 0.0483(10) 0.0455(10) 0.0375(10) 0.0044(8) 0.0027(9) -0.0041(9) C15 0.0426(9) 0.0468(10) 0.0394(10) -0.0012(8) 0.0018(8) -0.0067(9) C16 0.0420(8) 0.0501(11) 0.0414(10) 0.0040(8) 0.0024(9) -0.0010(9) C17 0.0579(11) 0.0434(11) 0.0555(13) 0.0052(9) 0.0014(10) -0.0075(11) C18 0.0766(13) 0.0503(12) 0.0586(15) 0.0054(10) -0.0152(12) -0.0211(12) C19 0.0667(12) 0.0574(13) 0.0391(11) 0.0113(10) -0.0107(10) -0.0108(11) C20 0.0816(16) 0.0540(13) 0.0719(17) 0.0067(11) -0.0073(14) 0.0106(13) O1 0.0640(9) 0.0567(8) 0.0549(9) 0.0022(7) -0.0134(7) 0.0073(7) O2 0.0881(11) 0.0445(8) 0.0802(13) 0.0049(8) -0.0127(10) -0.0021(9) O3 0.1243(16) 0.0638(10) 0.0544(11) 0.0120(10) -0.0018(11) 0.0152(10) O4 0.1004(12) 0.0409(8) 0.0660(12) -0.0016(8) 0.0077(10) 0.0034(8) O5 0.1352(17) 0.0545(10) 0.0737(14) -0.0265(10) 0.0139(12) -0.0191(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 C1 C6 120.0(2) C2 C1 H1 120.0 C6 C1 H1 120.0 C1 C2 C3 120.2(3) C1 C2 H2 119.9 C3 C2 H2 119.9 C2 C3 C4 120.5(3) C2 C3 H3 119.7 C4 C3 H3 119.7 C5 C4 C3 118.5(2) C5 C4 C7 121.34(19) C3 C4 C7 120.1(2) C6 C5 C4 120.1(2) C6 C5 H5 119.9 C4 C5 H5 119.9 C5 C6 C1 120.6(3) C5 C6 H6 119.7 C1 C6 H6 119.7 C9 C7 C4 123.10(19) C9 C7 C8 121.79(18) C4 C7 C8 115.0(2) C7 C8 H8A 109.5 C7 C8 H8B 109.5 H8A C8 H8B 109.5 C7 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C7 C9 C12 134.23(18) C7 C9 C10 120.60(19) C12 C9 C10 104.40(18) O5 C10 O4 118.2(2) O5 C10 C9 132.4(2) O4 C10 C9 109.39(19) O3 C11 O4 119.7(2) O3 C11 C12 131.2(3) O4 C11 C12 109.0(2) C13 C12 C9 138.8(2) C13 C12 C11 115.0(2) C9 C12 C11 106.07(19) C12 C13 C14 132.6(2) C12 C13 H13 113.7 C14 C13 H13 113.7 C19 C14 C15 120.00(18) C19 C14 C13 116.60(19) C15 C14 C13 123.40(18) C16 C15 C14 117.07(18) C16 C15 H15 121.5 C14 C15 H15 121.5 C15 C16 O1 128.48(19) C15 C16 C17 121.83(19) O1 C16 C17 109.68(18) C18 C17 O2 127.7(2) C18 C17 C16 122.4(2) O2 C17 C16 109.8(2) C17 C18 C19 116.7(2) C17 C18 H18 121.6 C19 C18 H18 121.6 C18 C19 C14 121.8(2) C18 C19 H19 119.1 C14 C19 H19 119.1 O2 C20 O1 108.90(19) O2 C20 H20A 109.9 O1 C20 H20A 109.9 O2 C20 H20B 109.9 O1 C20 H20B 109.9 H20A C20 H20B 108.3 C16 O1 C20 105.74(18) C17 O2 C20 105.82(17) C11 O4 C10 109.81(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.369(4) C1 C6 1.379(4) C1 H1 0.9300 C2 C3 1.376(4) C2 H2 0.9300 C3 C4 1.403(3) C3 H3 0.9300 C4 C5 1.387(3) C4 C7 1.478(3) C5 C6 1.379(3) C5 H5 0.9300 C6 H6 0.9300 C7 C9 1.356(3) C7 C8 1.512(3) C8 H8A 0.9600 C8 H8B 0.9600 C8 H8C 0.9600 C9 C12 1.473(3) C9 C10 1.487(3) C10 O5 1.191(3) C10 O4 1.391(3) C11 O3 1.195(3) C11 O4 1.383(3) C11 C12 1.477(3) C12 C13 1.349(3) C13 C14 1.451(3) C13 H13 0.9300 C14 C19 1.395(3) C14 C15 1.407(3) C15 C16 1.365(3) C15 H15 0.9300 C16 O1 1.369(3) C16 C17 1.388(3) C19 H19 0.9300 C17 C18 1.355(3) C17 O2 1.368(3) C18 C19 1.393(3) C18 H18 0.9300 C19 H19 0.9300 C20 O2 1.419(3) C20 O1 1.424(3) C20 H20A 0.9700 C20 H20B 0.9700 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C6 C1 C2 C3 0.4(4) C1 C2 C3 C4 1.7(4) C2 C3 C4 C5 -2.7(3) C2 C3 C4 C7 179.3(2) C3 C4 C5 C6 1.8(3) C7 C4 C5 C6 179.78(19) C4 C5 C6 C1 0.2(3) C2 C1 C6 C5 -1.3(4) C5 C4 C7 C9 42.2(3) C3 C4 C7 C9 -139.8(2) C5 C4 C7 C8 -134.7(2) C3 C4 C7 C8 43.2(3) C4 C7 C9 C12 3.0(4) C8 C7 C9 C12 179.7(2) C4 C7 C9 C10 -165.19(19) C8 C7 C9 C10 11.5(3) C7 C9 C10 O5 -16.8(4) C12 C9 C10 O5 171.9(3) C7 C9 C10 O4 161.4(2) C12 C9 C10 O4 -9.9(2) C7 C9 C12 C13 27.4(4) C10 C9 C12 C13 -163.0(3) C7 C9 C12 C11 -158.1(2) C10 C9 C12 C11 11.4(2) O3 C11 C12 C13 -12.5(4) O4 C11 C12 C13 166.54(19) O3 C11 C12 C9 171.5(3) O4 C11 C12 C9 -9.4(2) C9 C12 C13 C14 1.0(4) C11 C12 C13 C14 -173.1(2) C12 C13 C14 C19 -147.5(2) C12 C13 C14 C15 31.9(3) C19 C14 C15 C16 3.0(3) C13 C14 C15 C16 -176.44(18) C14 C15 C16 O1 179.41(18) C14 C15 C16 C17 0.9(3) C15 C16 C17 C18 -3.5(3) O1 C16 C17 C18 177.8(2) C15 C16 C17 O2 178.71(18) O1 C16 C17 O2 0.0(2) O2 C17 C18 C19 179.3(2) C16 C17 C18 C19 1.9(3) C17 C18 C19 C14 2.1(4) C15 C14 C19 C18 -4.6(3) C13 C14 C19 C18 174.8(2) C15 C16 O1 C20 -179.0(2) C17 C16 O1 C20 -0.4(2) O2 C20 O1 C16 0.7(3) C18 C17 O2 C20 -177.2(2) C16 C17 O2 C20 0.4(2) O1 C20 O2 C17 -0.7(3) O3 C11 O4 C10 -177.6(3) C12 C11 O4 C10 3.2(3) O5 C10 O4 C11 -177.2(2) C9 C10 O4 C11 4.3(2) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 30655285 2 PubChem 168309240