data_schreiner14004 _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H8 O4' _chemical_formula_weight 204.17 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 0.0016 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.629(2) _cell_length_b 6.5940(13) _cell_length_c 11.819(2) _cell_angle_alpha 90 _cell_angle_beta 92.98(3) _cell_angle_gamma 90 _cell_volume 905.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 596 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 23.28 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.498 _exptl_crystal_F_000 424 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 0.116 _shelx_estimated_absorpt_T_min 0.947 _shelx_estimated_absorpt_T_max 0.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6476 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details 'SADABS-2008/1' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Bruker Nonius FR591 rotating anode' _diffrn_measurement_device_type 'Bruker Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9657 _diffrn_reflns_av_unetI/netI 0.1061 _diffrn_reflns_av_R_equivalents 0.1407 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.452 _diffrn_reflns_theta_max 27.149 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 2003 _reflns_number_gt 1115 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker AXS Collect (2009)' _computing_cell_refinement ; Denzo/Scalepack (HKL Research, Inc., 1997) ; _computing_data_reduction ; Denzo/Scalepack (HKL Research, Inc., 1997) ; _computing_structure_solution 'SHELXT-2015 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Denzo/Scalepack (HKL Research, Inc., 1997) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2003 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.35820(18) 0.0870(4) 0.22783(16) 0.0297(5) Uani 1 1 d . . . . . H1 H 0.354073 -0.013206 0.169995 0.036 Uiso 1 1 calc R U . . . O1 O -0.05010(13) 0.4257(3) 0.22184(12) 0.0372(4) Uani 1 1 d . . . . . C2 C 0.43903(18) 0.0717(4) 0.31829(16) 0.0335(5) Uani 1 1 d . . . . . H2 H 0.491003 -0.039505 0.322081 0.040 Uiso 1 1 calc R U . . . O2 O 0.25941(15) 0.7199(3) 0.04792(12) 0.0499(5) Uani 1 1 d . . . . . C3 C 0.44452(18) 0.2165(4) 0.40260(16) 0.0329(6) Uani 1 1 d . . . . . H3 H 0.499724 0.203708 0.464305 0.040 Uiso 1 1 calc R U . . . O3 O -0.02636(13) 0.6546(3) 0.09011(11) 0.0376(4) Uani 1 1 d . . . . . C4 C 0.37018(17) 0.3802(3) 0.39782(15) 0.0276(5) Uani 1 1 d . . . . . H4 H 0.374246 0.480607 0.455527 0.033 Uiso 1 1 calc R U . . . O4 O 0.07117(14) 0.7516(3) 0.03793(11) 0.0393(4) Uani 1 1 d . . . . . C5 C 0.28969(17) 0.3956(3) 0.30772(14) 0.0242(5) Uani 1 1 d . . . . . C6 C 0.28403(17) 0.2506(3) 0.22373(15) 0.0254(5) Uani 1 1 d . . . . . C7 C 0.18988(18) 0.2952(3) 0.13529(15) 0.0284(5) Uani 1 1 d . . . . . H7A H 0.128005 0.192273 0.136797 0.034 Uiso 1 1 calc R U . . . H7B H 0.220387 0.298024 0.058649 0.034 Uiso 1 1 calc R U . . . C8 C 0.14441(17) 0.5085(3) 0.16875(15) 0.0246(5) Uani 1 1 d . . . . . C9 C 0.20171(17) 0.5589(3) 0.28772(14) 0.0270(5) Uani 1 1 d . . . . . H9A H 0.238519 0.694323 0.287753 0.032 Uiso 1 1 calc R U . . . H9B H 0.144203 0.556118 0.346586 0.032 Uiso 1 1 calc R U . . . C10 C 0.01682(19) 0.5160(3) 0.16819(16) 0.0282(5) Uani 1 1 d . . . . . C11 C 0.1710(2) 0.6644(4) 0.08241(15) 0.0322(5) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0343(13) 0.0260(13) 0.0290(9) -0.0036(10) 0.0036(8) 0.0004(10) O1 0.0306(9) 0.0359(10) 0.0456(8) -0.0028(8) 0.0063(7) -0.0066(8) C2 0.0285(12) 0.0340(14) 0.0380(11) 0.0059(11) 0.0009(9) 0.0071(11) O2 0.0486(11) 0.0601(14) 0.0414(9) 0.0027(9) 0.0065(8) -0.0246(10) C3 0.0303(13) 0.0402(15) 0.0278(10) 0.0043(11) -0.0036(9) 0.0028(11) O3 0.0339(9) 0.0409(11) 0.0373(8) 0.0040(8) -0.0059(7) 0.0057(8) C4 0.0293(12) 0.0307(14) 0.0227(9) -0.0005(10) 0.0008(8) -0.0002(10) O4 0.0496(11) 0.0352(11) 0.0326(8) 0.0085(7) -0.0018(7) 0.0013(8) C5 0.0238(11) 0.0263(13) 0.0226(9) 0.0016(9) 0.0025(8) -0.0018(9) C6 0.0241(11) 0.0293(13) 0.0229(9) 0.0015(9) 0.0014(8) -0.0027(10) C7 0.0282(11) 0.0305(14) 0.0262(10) -0.0034(10) -0.0013(8) 0.0024(10) C8 0.0244(11) 0.0265(13) 0.0224(9) 0.0012(9) -0.0023(7) -0.0017(10) C9 0.0289(12) 0.0283(14) 0.0234(9) -0.0026(10) -0.0032(8) 0.0014(10) C10 0.0327(12) 0.0267(13) 0.0245(9) -0.0054(10) -0.0038(8) 0.0025(10) C11 0.0379(14) 0.0338(14) 0.0243(9) -0.0030(10) -0.0036(9) -0.0067(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.381(3) . ? C1 C2 1.390(3) . ? C1 H1 0.9500 . ? O1 C10 1.189(2) . ? C2 C3 1.379(3) . ? C2 H2 0.9500 . ? O2 C11 1.183(2) . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? O3 C10 1.375(2) . ? O3 O4 1.466(2) . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? O4 C11 1.375(3) . ? C5 C6 1.378(3) . ? C5 C9 1.496(3) . ? C6 C7 1.503(3) . ? C7 C8 1.561(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.484(3) . ? C8 C11 1.492(3) . ? C8 C9 1.560(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.7(2) . . ? C6 C1 H1 120.7 . . ? C2 C1 H1 120.7 . . ? C3 C2 C1 120.6(2) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.38(19) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C10 O3 O4 107.98(15) . . ? C3 C4 C5 119.03(19) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C11 O4 O3 108.25(15) . . ? C6 C5 C4 120.5(2) . . ? C6 C5 C9 112.29(17) . . ? C4 C5 C9 127.17(18) . . ? C5 C6 C1 120.73(19) . . ? C5 C6 C7 111.78(18) . . ? C1 C6 C7 127.48(18) . . ? C6 C7 C8 104.14(16) . . ? C6 C7 H7A 110.9 . . ? C8 C7 H7A 110.9 . . ? C6 C7 H7B 110.9 . . ? C8 C7 H7B 110.9 . . ? H7A C7 H7B 108.9 . . ? C10 C8 C11 102.51(17) . . ? C10 C8 C9 112.15(15) . . ? C11 C8 C9 112.06(17) . . ? C10 C8 C7 112.37(17) . . ? C11 C8 C7 111.26(16) . . ? C9 C8 C7 106.61(16) . . ? C5 C9 C8 104.22(16) . . ? C5 C9 H9A 110.9 . . ? C8 C9 H9A 110.9 . . ? C5 C9 H9B 110.9 . . ? C8 C9 H9B 110.9 . . ? H9A C9 H9B 108.9 . . ? O1 C10 O3 117.7(2) . . ? O1 C10 C8 131.5(2) . . ? O3 C10 C8 110.81(17) . . ? O2 C11 O4 118.1(2) . . ? O2 C11 C8 131.5(2) . . ? O4 C11 C8 110.40(18) . . ? _refine_diff_density_max 0.171 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.050 _shelx_res_file ; TITL schreiner14004 in P2(1)/c schreiner14004.res created by SHELXL-2018/3 at 11:42:04 on 05-Jun-2019 CELL 0.71073 11.6290 6.5940 11.8190 90.000 92.981 90.000 ZERR 4.00 0.0023 0.0013 0.0024 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O UNIT 44 32 16 LIST 4 TEMP -123 SIZE 0.05 0.27 0.48 OMIT 1 0 0 ! partly behind beamstop shadow ACTA L.S. 10 BOND $H FMAP 2 PLAN 20 ACTA WGHT 0.031700 FVAR 1.16099 C1 1 0.358201 0.086969 0.227832 11.00000 0.03426 0.02598 = 0.02900 -0.00362 0.00363 0.00042 AFIX 43 H1 2 0.354073 -0.013206 0.169995 11.00000 -1.20000 AFIX 0 O1 3 -0.050097 0.425679 0.221845 11.00000 0.03064 0.03594 = 0.04559 -0.00278 0.00635 -0.00664 C2 1 0.439033 0.071737 0.318294 11.00000 0.02851 0.03395 = 0.03800 0.00591 0.00089 0.00712 AFIX 43 H2 2 0.491003 -0.039505 0.322081 11.00000 -1.20000 AFIX 0 O2 3 0.259407 0.719861 0.047919 11.00000 0.04864 0.06010 = 0.04143 0.00268 0.00653 -0.02464 C3 1 0.444522 0.216530 0.402595 11.00000 0.03033 0.04020 = 0.02777 0.00431 -0.00355 0.00283 AFIX 43 H3 2 0.499724 0.203708 0.464305 11.00000 -1.20000 AFIX 0 O3 3 -0.026361 0.654617 0.090106 11.00000 0.03385 0.04089 = 0.03726 0.00401 -0.00588 0.00568 C4 1 0.370180 0.380185 0.397823 11.00000 0.02927 0.03070 = 0.02266 -0.00052 0.00082 -0.00024 AFIX 43 H4 2 0.374246 0.480607 0.455527 11.00000 -1.20000 AFIX 0 O4 3 0.071167 0.751571 0.037927 11.00000 0.04959 0.03524 = 0.03257 0.00851 -0.00182 0.00125 C5 1 0.289694 0.395642 0.307719 11.00000 0.02379 0.02634 = 0.02262 0.00163 0.00255 -0.00178 C6 1 0.284035 0.250612 0.223727 11.00000 0.02405 0.02934 = 0.02290 0.00147 0.00142 -0.00272 C7 1 0.189879 0.295210 0.135287 11.00000 0.02822 0.03048 = 0.02623 -0.00340 -0.00135 0.00243 AFIX 23 H7A 2 0.128005 0.192273 0.136797 11.00000 -1.20000 H7B 2 0.220387 0.298024 0.058649 11.00000 -1.20000 AFIX 0 C8 1 0.144408 0.508539 0.168755 11.00000 0.02442 0.02646 = 0.02241 0.00125 -0.00234 -0.00171 C9 1 0.201710 0.558944 0.287716 11.00000 0.02891 0.02830 = 0.02341 -0.00255 -0.00316 0.00138 AFIX 23 H9A 2 0.238519 0.694323 0.287753 11.00000 -1.20000 H9B 2 0.144203 0.556118 0.346586 11.00000 -1.20000 AFIX 0 C10 1 0.016819 0.516033 0.168194 11.00000 0.03271 0.02674 = 0.02448 -0.00544 -0.00384 0.00252 C11 1 0.170991 0.664424 0.082413 11.00000 0.03785 0.03381 = 0.02430 -0.00303 -0.00360 -0.00667 HKLF 4 REM schreiner14004 in P2(1)/c REM wR2 = 0.100540, GooF = S = 0.94832, Restrained GooF = 0.94832 for all data REM R1 = 0.048501 for 1115 Fo > 4sig(Fo) and 0.117421 for all 2003 data REM 136 parameters refined using 0 restraints END WGHT 0.0317 0.0000 REM Highest difference peak 0.171, deepest hole -0.242, 1-sigma level 0.050 Q1 1 0.2593 0.3919 -0.0411 11.00000 0.05 0.17 Q2 1 0.0482 0.0903 0.1889 11.00000 0.05 0.16 Q3 1 0.1987 0.7400 0.2846 11.00000 0.05 0.16 Q4 1 0.0415 0.3976 0.3372 11.00000 0.05 0.16 Q5 1 0.0798 0.0583 0.0619 11.00000 0.05 0.16 Q6 1 0.0952 0.2400 0.0714 11.00000 0.05 0.15 Q7 1 -0.1562 0.4508 0.1172 11.00000 0.05 0.15 Q8 1 -0.0994 0.7486 0.1442 11.00000 0.05 0.15 Q9 1 0.0901 0.5255 0.1918 11.00000 0.05 0.14 Q10 1 0.1179 0.4268 0.4748 11.00000 0.05 0.14 Q11 1 -0.1438 0.3492 0.1751 11.00000 0.05 0.14 Q12 1 0.1871 0.2482 0.0598 11.00000 0.05 0.14 Q13 1 -0.0289 0.3033 0.2130 11.00000 0.05 0.14 Q14 1 0.1855 0.5020 -0.0305 11.00000 0.05 0.14 Q15 1 0.1110 0.5585 -0.0005 11.00000 0.05 0.14 Q16 1 0.0834 0.4684 0.4057 11.00000 0.05 0.14 Q17 1 0.0559 0.3474 0.2857 11.00000 0.05 0.14 Q18 1 -0.0046 0.4940 0.3610 11.00000 0.05 0.14 Q19 1 0.1999 0.3943 0.1005 11.00000 0.05 0.13 Q20 1 -0.0935 0.3461 0.1091 11.00000 0.05 0.13 ; _shelx_res_checksum 97497 _shelx_hkl_file ; 1 0 0 368.00 22.24 1 0 0 92.45 20.51 2 0 0 29.62 8.34 -2 0 0 15.91 15.39 2 0 0 -10.29 18.49 -2 0 0 -10.25 16.71 3 0 0 1184.03 63.63 -3 0 0 1144.36 62.16 -3 0 0 1219.66 236.55 3 0 0 1167.18 222.11 -4 0 0 1488.92 76.06 4 0 0 1594.86 87.58 -4 0 0 1401.78 283.45 4 0 0 1615.87 284.14 -5 0 0 1066.55 58.63 5 0 0 1073.77 61.00 -5 0 0 975.98 192.49 5 0 0 923.59 186.33 6 0 0 75.70 14.25 -6 0 0 18.94 13.05 6 0 0 -17.50 66.61 -6 0 0 124.73 59.49 7 0 0 127.40 17.46 -7 0 0 87.24 49.31 -7 0 0 62.90 61.55 7 0 0 101.25 60.00 -8 0 0 265.30 26.28 8 0 0 377.10 27.81 8 0 0 304.34 85.02 -8 0 0 185.15 84.03 9 0 0 523.83 35.42 -9 0 0 602.85 45.45 -9 0 0 690.93 165.01 9 0 0 696.33 158.48 -10 0 0 368.85 29.70 10 0 0 317.71 30.09 10 0 0 136.76 87.59 -10 0 0 166.46 87.42 -11 0 0 491.06 36.75 11 0 0 521.50 55.44 11 0 0 471.97 129.73 -11 0 0 296.53 118.31 12 0 0 331.95 51.27 13 0 0 47.69 9.04 13 0 0 35.19 34.81 14 0 0 176.82 11.41 14 0 0 115.44 40.10 0 -1 0 5.00 8.61 0 1 0 19.33 7.16 0 -1 0 -26.70 16.18 -1 -1 0 384.55 20.94 1 -1 0 368.41 17.39 -1 -1 0 378.12 17.67 -1 1 0 398.59 19.48 1 -1 0 297.18 64.48 -1 -1 0 351.00 68.74 -1 1 0 330.94 66.12 1 1 0 315.62 69.80 2 -1 0 7002.14 482.23 -2 -1 0 7220.27 274.72 -2 -1 0 7250.64 339.43 2 1 0 7093.60 374.32 -2 1 0 7116.21 328.79 2 1 0 6881.98 315.03 -2 -1 0 7310.53 1276.79 2 -1 0 6724.65 1279.16 -2 1 0 6969.61 1273.03 2 1 0 6796.01 1270.36 -3 -1 0 124.81 6.12 -3 -1 0 95.76 13.42 3 -1 0 112.66 11.92 3 1 0 120.15 6.60 -3 1 0 139.55 12.75 3 1 0 123.51 12.38 -3 -1 0 123.70 40.77 3 -1 0 162.19 42.96 -3 1 0 91.87 49.38 3 1 0 137.22 39.94 4 -1 0 478.74 24.81 -4 -1 0 570.26 34.44 4 1 0 427.62 31.85 4 1 0 532.45 45.96 -4 1 0 498.92 25.51 -4 -1 0 342.37 95.51 4 -1 0 391.58 106.37 4 1 0 607.56 99.87 -4 1 0 539.70 99.62 -5 -1 0 209.51 16.98 5 -1 0 219.65 18.85 -5 1 0 186.91 17.84 5 1 0 229.02 10.83 5 1 0 239.33 21.90 5 -1 0 178.26 60.42 -5 -1 0 174.40 59.48 -5 1 0 274.54 63.54 5 1 0 100.74 56.15 -6 -1 0 158.55 17.13 6 -1 0 210.18 19.96 6 1 0 215.35 19.60 6 1 0 207.29 10.83 -6 1 0 187.57 18.58 6 -1 0 94.18 82.79 -6 -1 0 202.42 68.44 6 1 0 225.63 67.97 -6 1 0 260.12 73.65 7 -1 0 345.57 25.66 -7 -1 0 348.66 34.52 -7 1 0 389.66 33.01 7 1 0 370.83 17.87 7 1 0 367.46 32.08 7 -1 0 251.42 85.17 -7 -1 0 173.69 80.70 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