#------------------------------------------------------------------------------ #$Date: 2022-03-03 22:09:58 +0000 (Thu, 03 Mar 2022) $ #$Revision: 273274 $ #$URL: svn://www.crystallography.net/cod/cif/4/51/93/4519367.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4519367 loop_ _publ_author_name 'Hipwell, Vince M.' 'Zee, Chih-Te' 'Rodriguez, Jose' 'Garcia-Garibay, Miguel A.' _publ_section_title ; Scale-Dependent Photosalience and Topotactic Reaction of Microcrystalline Benzylidenebutyrolactone Determined by Electron Microscopy and Electron Diffraction ; _journal_issue 3 _journal_name_full 'Crystal Growth & Design' _journal_page_first 1533 _journal_page_last 1537 _journal_paper_doi 10.1021/acs.cgd.1c01378 _journal_volume 22 _journal_year 2022 _chemical_formula_sum 'C48 H40 O8' _chemical_formula_weight 744.84 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 108.06(2) _cell_angle_gamma 90 _cell_formula_units_Z 1 _cell_length_a 11.440(2) _cell_length_b 5.9800(12) _cell_length_c 12.430(3) _cell_measurement_temperature 293(2) _cell_volume 808.5(3) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.820 _diffrn_measured_fraction_theta_max 0.820 _diffrn_radiation_wavelength 0.97918 _diffrn_reflns_av_unetI/netI 0.0709 _diffrn_reflns_Laue_measured_fraction_full 0.820 _diffrn_reflns_Laue_measured_fraction_max 0.820 _diffrn_reflns_number 804 _diffrn_reflns_point_group_measured_fraction_full 0.820 _diffrn_reflns_point_group_measured_fraction_max 0.820 _diffrn_reflns_theta_full 30.920 _diffrn_reflns_theta_max 30.920 _diffrn_reflns_theta_min 6.183 _exptl_absorpt_coefficient_mu 0.000 _exptl_crystal_density_diffrn 1.530 _exptl_crystal_F_000 157 _refine_diff_density_max 0.143 _refine_diff_density_min -0.136 _refine_diff_density_rms 0.039 _refine_ls_extinction_coef 0.5(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.752 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 119 _refine_ls_number_reflns 804 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.752 _refine_ls_R_factor_all 0.1971 _refine_ls_R_factor_gt 0.1638 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4169 _refine_ls_wR_factor_ref 0.4444 _reflns_Friedel_coverage 0.000 _reflns_number_gt 576 _reflns_number_total 804 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cg1c01378_si_003.cif _cod_data_source_block SG14 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 4519367 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_res_file ; TITL VH2_101_powder_hv_final_SG14_a.res in P2(1)/n SG14.res created by SHELXL-2018/3 at 18:28:54 on 18-May-2021 REM Old TITL cg in space group P 1 21/c 1 . REM SHELXT solution in P2(1)/n: R1 0.297, Rweak 0.367, Alpha 0.128 REM 1.856 for 20 systematic absences, Orientation as input REM Formula found by SHELXT: C13 CELL 0.97918 11.4400 5.9800 12.4300 90.000 108.060 90.000 ZERR 1.000 0.0023 0.0012 0.0025 0.000 0.022 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C 0.1361 0.3731 0.5482 3.2814 1.2266 13.04 0.5971 41.02 0 0 0 0 0.68 12.011 SFAC O 0.1433 0.3055 0.5103 2.2683 0.9370 8.26 0.3923 25.66 0 0 0 0 0.68 15.999 SFAC H 0.0367 0.5608 0.1269 3.7913 0.2360 13.55 0.1290 37.72 0 0 0 0 0.23 1.008 UNIT 48 8 40 L.S. 100 LIST 6 FMAP 2 PLAN 20 ACTA WGHT 0.200000 EXTI 0.516127 FVAR 45.92828 C1 1 0.319295 0.676880 0.467621 11.00000 0.06124 0.03094 = 0.10403 0.00903 0.04205 0.01636 O1 2 0.346688 0.860179 0.505576 11.00000 0.09818 0.04831 = 0.12524 -0.00235 0.07259 0.01738 C3 1 0.317557 0.365602 0.368838 11.00000 0.06314 0.04298 = 0.09756 0.00519 0.03208 0.00309 AFIX 23 H3A 3 0.349527 0.214766 0.371528 11.00000 -1.20000 H3B 3 0.295322 0.422201 0.291997 11.00000 -1.20000 AFIX 0 O2 2 0.217737 0.594340 0.454845 11.00000 0.05700 0.07976 = 0.16506 -0.00328 0.04808 0.01080 C2 1 0.215608 0.379617 0.416296 11.00000 0.05447 0.09166 = 0.07749 0.01076 0.01310 -0.00860 AFIX 23 H2A 3 0.138034 0.348191 0.358755 11.00000 -1.20000 H2B 3 0.226832 0.273740 0.477797 11.00000 -1.20000 AFIX 0 C5 1 0.517468 0.605578 0.435883 11.00000 0.08162 0.02118 = 0.13546 -0.02367 0.05850 -0.00365 AFIX 13 H5 3 0.517383 0.766267 0.451341 11.00000 -1.20000 AFIX 0 C4 1 0.401581 0.512567 0.448518 11.00000 0.06117 0.03306 = 0.10363 -0.00287 0.04669 -0.00921 C7 1 0.524551 0.392799 0.259973 11.00000 0.07944 0.04443 = 0.13296 -0.02334 0.07273 -0.01722 AFIX 43 H7 3 0.488104 0.269101 0.281812 11.00000 -1.20000 AFIX 0 C6 1 0.544959 0.580551 0.327280 11.00000 0.05821 0.02207 = 0.09731 -0.01632 0.04838 -0.00502 C8 1 0.554421 0.380714 0.165912 11.00000 0.08099 0.06088 = 0.08941 -0.03028 0.03838 -0.01216 AFIX 43 H8 3 0.536220 0.250351 0.123158 11.00000 -1.20000 AFIX 0 C9 1 0.610650 0.550640 0.128840 11.00000 0.07206 0.06757 = 0.07365 0.00023 0.04291 -0.01111 AFIX 43 H9 3 0.630838 0.543778 0.061972 11.00000 -1.20000 AFIX 0 C10 1 0.635113 0.734346 0.199344 11.00000 0.07139 0.05126 = 0.09155 0.00918 0.02966 -0.01738 AFIX 43 H10 3 0.681112 0.850947 0.183640 11.00000 -1.20000 AFIX 0 C11 1 0.595808 0.751158 0.288212 11.00000 0.07358 0.03236 = 0.08938 0.01556 0.04406 0.00118 AFIX 43 H11 3 0.603814 0.887917 0.325425 11.00000 -1.20000 AFIX 0 HKLF 4 REM VH2_101_powder_hv_final_SG14_a.res in P2(1)/n REM wR2 = 0.4444, GooF = S = 1.752, Restrained GooF = 1.752 for all data REM R1 = 0.1638 for 576 Fo > 4sig(Fo) and 0.1971 for all 804 data REM 119 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.143, deepest hole -0.136, 1-sigma level 0.039 Q1 1 0.2541 0.7450 0.4226 11.00000 0.05 0.14 Q2 1 0.4886 0.5543 0.2133 11.00000 0.05 0.13 Q3 1 0.1807 0.2910 0.1853 11.00000 0.05 0.12 Q4 1 0.1409 0.3804 0.2726 11.00000 0.05 0.12 Q5 1 0.3670 0.6132 0.3681 11.00000 0.05 0.12 Q6 1 0.4257 0.7098 0.3532 11.00000 0.05 0.11 Q7 1 0.4207 0.0953 0.4561 11.00000 0.05 0.11 Q8 1 0.2895 0.2327 0.5794 11.00000 0.05 0.10 Q9 1 0.5140 0.5093 0.3564 11.00000 0.05 0.10 Q10 1 0.6469 1.1603 0.2939 11.00000 0.05 0.10 Q11 1 0.6816 0.2123 0.1993 11.00000 0.05 0.10 Q12 1 0.6372 0.8822 0.0644 11.00000 0.05 0.09 Q13 1 0.5536 1.0395 0.3409 11.00000 0.05 0.08 Q14 1 0.4387 0.9855 0.5755 11.00000 0.05 0.08 Q15 1 0.6732 0.8565 0.3814 11.00000 0.05 0.08 Q16 1 0.2592 0.5579 0.4980 11.00000 0.05 0.08 Q17 1 0.5834 0.6600 0.1350 11.00000 0.05 0.07 Q18 1 0.5043 0.9529 0.2367 11.00000 0.05 0.07 Q19 1 0.5640 0.6239 0.0434 11.00000 0.05 0.07 Q20 1 0.0649 0.4650 0.3301 11.00000 0.05 0.07 ; _shelx_res_checksum 74592 _shelx_hkl_file ; 0 1 2 1076.11 391.730 -1 0 1 3 84259. 3441.87 1 0 1 4 29724. 1468.44 1 0 1 5 3274.07 670.595 1 0 1 6 41630. 1901.72 -1 0 1 8 8162.20 1201.56 1 0 1 9 2095.48 1102.68 1 0 1 10 724.33 1199.76 1 0 1 11 -56.71 1682.38 1 0 1 12 117.06 1146.22 1 0 2 1 118997. 4820.21 1 0 2 3 189133. 7550.93 1 0 2 4 50959. 2201.36 1 0 2 5 48302. 2289.25 1 0 2 6 7584.89 855.373 1 0 2 7 44886. 2213.34 1 0 2 8 201.16 641.030 1 0 2 9 1537.95 745.505 1 0 2 10 8987.21 1101.08 1 0 2 11 -187.06 727.326 1 0 3 1 18811. 1222.13 1 0 3 2 22753. 1354.57 1 0 3 3 10571. 968.637 1 0 3 4 1837.19 828.605 1 0 3 5 45046. 2289.25 1 0 3 6 12239. 930.482 1 0 3 7 -11.41 696.963 1 0 3 9 2439.07 794.246 1 0 3 10 5261.68 865.361 1 0 4 1 10953. 1054.53 1 0 4 2 15222. 1169.60 1 0 4 3 20455. 1371.35 1 0 4 4 3943.26 799.440 1 0 4 5 6466.23 995.404 1 0 4 6 323.01 830.802 1 0 4 7 1087.09 868.157 1 0 4 8 2205.35 685.177 -1 0 5 1 1485.62 751.697 1 0 5 2 2754.69 847.782 1 0 5 3 10070. 1101.08 1 0 5 4 4121.05 1285.06 1 0 5 5 1957.65 823.211 1 0 5 6 504.39 1178.58 1 0 5 7 5111.86 1046.94 1 0 6 0 16025. 1889.53 -1 0 6 1 8389.92 1183.78 1 0 6 2 13390. 1316.02 1 0 6 3 458.45 789.052 1 1 1 -12 68.10 1596.08 1 1 1 -11 -861.37 1472.03 -1 1 1 -9 4518.57 1440.47 1 1 1 -8 923.89 1252.90 1 1 1 -7 2972.43 915.900 1 1 1 -6 3797.44 704.354 1 1 1 -5 64882. 2772.67 1 1 1 -3 252097. 13851. 1 1 1 1 390930. 15124. 1 1 1 2 999999. 38414. 1 1 1 3 408709. 15851. 1 1 1 4 230923. 9139.02 1 1 1 5 132761. 5419.49 1 1 1 6 -220.93 822.213 1 1 1 8 2321.21 1019.97 1 1 1 9 1086.49 1144.03 1 1 1 10 5679.18 1313.82 1 1 1 11 841.79 1146.62 -1 1 2 -12 -471.63 957.650 1 1 2 -11 1056.33 815.620 -1 1 2 -10 3320.01 860.367 1 1 2 -9 25270. 1604.47 -1 1 2 -8 40032. 2043.55 1 1 2 -7 424.89 589.292 1 1 2 -6 19243. 1188.77 1 1 2 -5 36556. 1797.84 1 1 2 -4 72493. 3122.25 1 1 2 -3 45865. 2079.50 1 1 2 -2 108270. 4402.71 1 1 2 -1 44966. 2003.59 1 1 2 0 96564. 3989.21 1 1 2 1 32341. 1601.28 -1 1 2 2 169017. 6779.86 1 1 2 3 81023. 3515.78 1 1 2 4 79904. 3465.84 1 1 2 5 17946. 1227.93 1 1 2 7 10044. 1011.98 -1 1 2 8 -86.36 696.563 1 1 2 9 676.79 778.066 1 1 2 10 7311.22 1069.72 1 1 2 11 583.90 802.636 1 1 3 -11 347.58 746.104 1 1 3 -10 2447.06 1108.07 1 1 3 -9 4266.88 891.529 1 1 3 -8 435.68 658.209 1 1 3 -7 566.32 645.225 1 1 3 -6 -359.57 682.980 1 1 3 -5 21374. 1368.76 1 1 3 -4 1548.74 650.019 1 1 3 -3 26328. 1492.41 1 1 3 -2 2101.48 674.989 1 1 3 -1 47044. 2197.36 1 1 3 0 1621.65 713.143 1 1 3 1 6044.74 854.973 1 1 3 2 154015. 6304.43 1 1 3 3 347982. 13741. 1 1 3 4 2594.88 857.970 1 1 3 5 1348.78 797.043 1 1 3 6 1556.93 734.318 1 1 3 7 1314.22 716.539 1 1 3 8 899.72 776.667 -1 1 3 9 1731.72 700.758 1 1 3 10 642.63 1049.54 1 1 4 -9 1152.62 638.034 -1 1 4 -8 -737.11 771.274 1 1 4 -7 3024.37 1333.20 1 1 4 -6 3851.37 884.338 1 1 4 -5 1799.24 683.579 1 1 4 -3 4172.99 694.166 1 1 4 -2 4608.47 788.453 1 1 4 0 1995.60 740.111 1 1 4 1 6987.61 967.438 1 1 4 2 5803.03 894.326 1 1 4 3 2698.76 787.055 1 1 4 4 1118.86 719.736 -1 1 4 5 946.26 830.003 1 1 4 6 1425.09 882.141 1 1 4 7 670.79 729.524 1 1 4 8 917.30 758.889 1 1 4 9 1735.92 841.389 -1 1 5 -7 927.29 853.575 -1 1 5 -6 4500.59 1155.01 1 1 5 -5 2896.52 767.079 1 1 5 -4 3967.24 897.922 1 1 5 -3 5329.60 1365.56 1 1 5 -2 10697. 1084.50 1 1 5 0 12523. 1270.67 1 1 5 1 22893. 1661.40 1 1 5 3 14271. 1900.92 1 1 5 4 858.97 772.272 1 1 5 5 12026. 1252.70 1 1 5 6 1785.86 979.823 1 1 6 -3 3116.26 903.715 1 1 6 -2 7231.32 1046.94 1 1 6 -1 1619.06 636.436 1 1 6 0 1798.44 1414.70 1 1 6 1 3845.38 1005.59 1 1 6 2 1467.04 1198.96 1 1 6 3 2415.10 973.431 1 2 1 -12 3076.31 1184.98 1 2 1 -11 2998.40 1648.62 1 2 1 -10 410.31 988.613 1 2 1 -9 3987.21 1342.19 -1 2 1 -8 10801. 1122.05 1 2 1 -7 3413.90 572.313 1 2 1 -6 22912. 1737.51 1 2 1 -5 148522. 8322.00 1 2 1 -4 201758. 11119. 1 2 1 -3 6478.22 738.713 1 2 1 -1 407111. 15717. 1 2 1 0 154934. 6102.67 1 2 1 1 7479.02 676.987 1 2 1 2 785656. 30244. 1 2 1 3 2606.87 670.595 1 2 1 4 930.28 730.523 1 2 1 5 2852.57 644.426 1 2 1 6 991.21 1000.60 1 2 1 7 5273.67 1185.18 1 2 1 8 343.39 1047.34 1 2 1 9 481.02 1633.84 1 2 1 10 2644.82 1203.95 -1 2 1 11 -2417.1 1729.92 1 2 2 -12 614.06 762.484 1 2 2 -11 -109.99 722.932 1 2 2 -10 293.45 683.979 1 2 2 -9 9490.60 980.622 1 2 2 -8 1203.55 503.196 1 2 2 -7 3182.18 616.460 1 2 2 -6 3969.23 623.451 1 2 2 -3 153655. 6124.64 1 2 2 -2 47024. 2079.50 1 2 2 -1 39213. 1859.77 1 2 2 0 271074. 10653. 1 2 2 1 1812.42 692.169 1 2 2 3 117399. 4898.12 1 2 2 4 124131. 5183.77 1 2 2 5 65961. 3020.37 1 2 2 6 4174.99 874.150 1 2 2 7 7259.28 949.659 1 2 2 8 412.30 709.548 1 2 2 9 -520.38 772.472 1 2 2 10 2942.47 976.028 1 2 3 -11 1010.19 1127.05 1 2 3 -10 20196. 1441.67 1 2 3 -9 19996. 1330.60 1 2 3 -8 7361.16 873.751 1 2 3 -7 5291.64 831.401 1 2 3 -6 1582.90 1103.27 1 2 3 -5 4117.06 682.580 1 2 3 -3 8623.64 871.953 1 2 3 -2 210148. 8381.93 1 2 3 -1 65421. 2934.48 1 2 3 1 39193. 1983.42 -1 2 3 2 2283.26 709.947 1 2 3 3 4330.80 1311.62 1 2 3 4 20236. 1466.24 1 2 3 5 12563. 1165.80 1 2 3 6 1695.96 699.959 1 2 3 7 1444.07 737.714 1 2 3 8 504.99 784.857 1 2 3 9 819.02 802.436 1 2 4 -9 3615.66 857.770 1 2 4 -8 1980.02 837.994 1 2 4 -7 5365.56 935.477 1 2 4 -6 7113.46 928.485 -1 2 4 -5 6979.62 893.327 1 2 4 -4 5920.89 833.599 1 2 4 -3 3837.39 736.116 1 2 4 -2 40971. 2069.51 1 2 4 -1 10887. 1090.69 1 2 4 0 2562.92 801.438 1 2 4 1 2339.19 775.069 1 2 4 2 11982. 1129.24 1 2 4 3 1206.35 700.359 1 2 4 4 18186. 1494.21 1 2 4 5 3224.13 969.236 1 2 4 6 5041.94 1057.93 1 2 4 7 4420.69 923.691 1 2 4 8 686.58 879.144 1 2 5 -7 8395.92 1070.71 1 2 5 -6 13989. 1226.13 1 2 5 -5 1843.59 781.661 1 2 5 -4 2896.52 792.049 1 2 5 -3 2415.10 758.889 1 2 5 -2 4890.13 859.168 1 2 5 -1 1896.92 882.940 -1 2 5 0 50979. 2656.81 1 2 5 1 6925.68 952.256 1 2 5 2 1634.24 847.183 1 2 5 3 6110.66 998.201 1 2 5 4 4536.55 977.027 1 2 5 5 10555. 1309.03 -1 2 5 6 2117.46 1271.27 1 2 6 -3 3601.67 891.529 1 2 6 -2 6216.53 945.664 1 2 6 -1 6855.77 1132.84 1 2 6 0 8515.77 1202.56 1 2 6 1 6955.65 1159.21 1 2 6 2 570.91 1518.78 1 3 0 0 202.36 544.146 1 3 1 -12 1025.37 1009.79 1 3 1 -11 1192.37 1000.60 1 3 1 -10 2251.30 929.683 1 3 1 -9 2033.56 1029.56 1 3 1 -8 2411.10 1174.39 1 3 1 -7 10813. 1011.19 1 3 1 -6 18923. 1418.30 1 3 1 -5 19594. 1339.19 1 3 1 -4 30483. 1884.74 -1 3 1 -3 32441. 1939.47 1 3 1 -2 2213.34 425.888 -1 3 1 -1 129345. 5133.83 1 3 1 0 362964. 14061. 1 3 1 1 215941. 8495.80 1 3 1 2 21774. 1268.48 1 3 1 3 70915. 3112.26 1 3 1 4 47603. 2321.21 1 3 1 6 2187.37 1060.93 1 3 1 7 1923.49 1078.70 1 3 1 8 7471.03 1378.54 1 3 1 9 10240. 1962.44 1 3 1 10 856.77 1199.36 1 3 2 -12 803.24 703.555 1 3 2 -11 318.02 661.605 1 3 2 -10 5147.82 806.831 1 3 2 -9 5247.70 778.465 1 3 2 -8 4826.20 644.826 -1 3 2 -7 48562. 3086.29 1 3 2 -6 1623.65 751.497 1 3 2 -5 50999. 3182.18 1 3 2 -4 17079. 1386.53 1 3 2 -3 938.07 753.495 1 3 2 -2 414302. 16095. -1 3 2 -1 208150. 8246.10 1 3 2 0 4322.81 632.041 1 3 2 1 19373. 1257.09 -1 3 2 2 13971. 1060.33 1 3 2 3 42069. 2105.47 1 3 2 4 35897. 1965.44 1 3 2 5 40931. 2183.38 1 3 2 6 7269.27 980.622 1 3 2 7 250.30 834.997 1 3 2 8 2840.59 871.154 1 3 2 9 1094.09 858.968 1 3 2 10 709.55 848.181 1 3 3 -11 1417.30 735.716 1 3 3 -10 1794.05 707.350 1 3 3 -9 36596. 1930.08 1 3 3 -8 406.71 663.004 1 3 3 -7 49301. 2361.16 1 3 3 -6 5297.64 802.636 1 3 3 -5 19047. 1177.59 1 3 3 -3 2423.09 636.436 1 3 3 -2 26948. 1524.17 1 3 3 -1 30164. 1657.21 1 3 3 0 66620. 2996.40 -1 3 3 1 5832.99 837.394 1 3 3 2 32761. 1844.58 -1 3 3 3 3499.80 947.262 1 3 3 4 57091. 2800.64 1 3 3 5 1067.32 811.226 1 3 3 6 3447.86 912.504 1 3 3 7 4436.67 956.851 1 3 3 8 -201.76 909.108 1 3 3 9 2351.18 1288.45 -1 3 4 -10 831.00 721.134 1 3 4 -9 4654.41 1148.22 1 3 4 -8 4226.92 915.101 -1 3 4 -7 42129. 2113.46 1 3 4 -6 14285. 1145.42 1 3 4 -5 25629. 1525.77 1 3 4 -4 495.01 689.772 1 3 4 -3 30983. 1671.59 1 3 4 -2 20715. 1379.54 1 3 4 -1 20076. 1407.71 1 3 4 0 13228. 1208.15 1 3 4 1 2169.39 841.190 1 3 4 2 11838. 1165.00 1 3 4 3 32781. 2001.60 1 3 4 4 8893.32 1217.94 1 3 4 5 187.24 1015.58 1 3 4 6 1653.41 807.230 1 3 4 7 3343.98 873.551 1 3 5 -7 683.98 741.509 1 3 5 -6 4802.23 883.339 1 3 5 -5 4826.20 797.642 1 3 5 -4 1044.55 702.756 1 3 5 -3 1604.07 722.932 -1 3 5 -2 3334.00 895.724 1 3 5 -1 2251.30 949.659 -1 3 5 1 1602.68 937.474 1 3 5 2 18390. 1512.78 1 3 5 3 2714.74 1061.92 -1 3 5 4 8034.35 1268.08 1 3 5 5 567.12 1232.12 1 3 6 -2 5047.94 1041.95 1 3 6 -1 1911.50 963.842 1 3 6 0 918.30 1409.11 1 4 0 -2 4538.55 549.340 1 4 0 0 23452. 1231.72 1 4 1 -12 1185.38 1404.91 1 4 1 -11 1986.01 1413.90 1 4 1 -10 314.22 1206.15 1 4 1 -9 868.16 1086.30 1 4 1 -8 2840.59 692.169 1 4 1 -6 1440.67 384.738 1 4 1 -5 145126. 5629.24 1 4 1 -4 197603. 7662.80 1 4 1 -3 15771. 865.560 1 4 1 0 56512. 2449.06 1 4 1 1 522373. 20256. 1 4 1 2 4188.97 749.100 -1 4 1 3 31802. 1738.31 1 4 1 5 22433. 1690.17 -1 4 1 6 2197.36 1491.01 1 4 1 7 3389.93 1238.71 1 4 1 8 3721.53 1348.18 -1 4 1 10 5365.56 1960.45 1 4 2 -12 1239.91 655.013 -1 4 2 -10 17267. 1637.03 1 4 2 -9 25949. 1858.37 1 4 2 -8 2916.50 744.706 1 4 2 -7 1801.04 616.659 1 4 2 -6 44706. 2814.62 1 4 2 -5 1355.17 627.846 1 4 2 -4 121035. 6831.79 1 4 2 -3 14.96 594.885 -1 4 2 -2 76248. 3252.09 1 4 2 -1 4143.02 694.766 1 4 2 0 16926. 1173.39 1 4 2 1 24551. 1388.93 -1 4 2 2 181582. 7371.15 -1 4 2 3 16390. 1222.53 -1 4 2 5 1480.82 792.448 1 4 2 6 1588.09 829.604 -1 4 2 7 5271.67 1052.34 1 4 2 8 -105.29 1287.05 1 4 2 9 1836.59 928.685 1 4 3 -11 1829.60 667.798 1 4 3 -10 280.06 603.275 1 4 3 -9 4934.07 667.598 1 4 3 -8 1642.83 672.992 1 4 3 -7 48142. 3130.24 1 4 3 -6 5834.99 676.188 1 4 3 -5 462.05 437.075 1 4 3 -4 2159.41 580.303 1 4 3 -3 1992.01 617.259 1 4 3 -2 58889. 2726.73 1 4 3 -1 2373.15 729.524 1 4 3 0 11892. 1040.55 1 4 3 1 79445. 3567.72 1 4 3 2 2415.10 855.173 1 4 3 3 19944. 1392.73 1 4 3 4 14263. 1248.90 1 4 3 5 8781.45 1071.71 1 4 3 6 1589.89 872.952 1 4 3 7 442.27 651.218 1 4 3 8 3993.20 1039.95 1 4 4 -9 1905.11 773.871 1 4 4 -7 13100. 1069.52 1 4 4 -6 7371.15 888.333 1 4 4 -4 2752.69 676.188 1 4 4 -3 9832.19 1035.76 1 4 4 -2 15326. 1245.50 1 4 4 -1 1851.78 739.712 1 4 4 0 47123. 2429.08 1 4 4 1 1601.68 831.601 1 4 4 2 1467.04 937.874 1 4 4 4 3793.44 1085.50 1 4 4 5 2305.23 854.773 1 4 4 6 2970.43 828.605 1 4 4 7 1262.28 812.224 1 4 5 -7 2706.75 1197.36 1 4 5 -6 -396.52 678.385 -1 4 5 -5 1649.82 732.920 -1 4 5 -4 8242.10 964.242 1 4 5 -3 9584.49 1113.86 -1 4 5 -2 14872. 1416.10 1 4 5 0 833.40 921.493 1 4 5 1 38893. 2261.28 1 4 5 2 14854. 1401.72 1 4 5 3 4934.07 1161.01 1 4 5 4 1323.61 1016.38 1 5 0 -4 4438.67 277.866 1 5 0 -2 874.15 416.700 1 5 0 0 651.02 625.049 1 5 0 2 -354.97 940.670 1 5 1 -12 -136.68 1307.43 1 5 1 -11 7207.34 1376.95 1 5 1 -10 1083.50 1170.39 1 5 1 -9 1597.48 593.287 1 5 1 -8 1923.29 454.454 1 5 1 -7 5771.07 523.172 -1 5 1 -6 2485.02 354.974 -1 5 1 -5 264682. 10238. 1 5 1 -4 81242. 3296.04 1 5 1 -2 315022. 12289. 1 5 1 -1 2504.99 517.978 1 5 1 0 18202. 994.605 1 5 1 1 348182. 13646. 1 5 1 2 16065. 1178.98 1 5 1 3 35557. 1937.47 1 5 1 4 290.05 987.814 1 5 1 5 2912.50 1175.59 -1 5 1 6 -649.42 1130.04 1 5 1 7 1092.29 1741.51 1 5 1 8 2876.55 1278.66 1 5 1 9 962.64 1313.62 1 5 2 -12 133.58 815.421 1 5 2 -11 839.59 846.783 1 5 2 -10 4027.16 883.938 1 5 2 -9 17347. 1510.19 1 5 2 -5 1215.34 547.343 1 5 2 -3 7035.55 683.579 1 5 2 -2 37475. 1808.83 1 5 2 -1 106912. 4460.64 1 5 2 0 47663. 2281.26 1 5 2 1 4328.80 780.063 1 5 2 2 3553.73 782.660 1 5 2 4 43508. 2279.26 1 5 2 5 6164.60 959.248 1 5 2 6 2992.41 908.908 1 5 2 7 3363.96 905.512 1 5 3 -11 1472.83 781.661 1 5 3 -10 7231.32 1070.51 1 5 3 -9 36236. 2602.87 1 5 3 -8 468.64 759.088 1 5 3 -7 14067. 1289.65 1 5 3 -6 9524.56 1074.71 -1 5 3 -5 1203.15 654.214 -1 5 3 -4 1986.61 635.437 1 5 3 -3 26528. 1523.17 1 5 3 -2 13841. 1062.72 1 5 3 -1 17299. 1219.74 1 5 3 0 59369. 2818.61 -1 5 3 1 3621.65 826.807 1 5 3 2 1708.55 1269.08 1 5 3 3 3535.75 849.580 1 5 3 4 1606.27 840.191 1 5 3 5 3330.00 908.709 1 5 3 6 1765.48 917.099 1 5 3 7 1453.65 840.990 1 5 4 -9 1548.54 854.574 1 5 4 -8 8743.50 915.900 1 5 4 -7 7239.31 845.185 1 5 4 -6 1934.08 630.243 1 5 4 -5 6857.76 800.439 1 5 4 -4 8138.23 947.063 1 5 4 -3 2528.96 1183.38 1 5 4 -2 1518.58 817.418 1 5 4 -1 4812.22 906.911 1 5 4 0 2467.04 867.958 1 5 4 1 43967. 2377.15 1 5 4 2 5691.17 1129.24 1 5 4 3 -503.40 934.078 1 5 4 4 1152.22 872.153 1 5 4 5 -387.14 819.016 1 5 4 6 3493.80 934.877 1 5 5 -7 2005.59 721.533 1 5 5 -6 826.01 750.898 1 5 5 -5 4508.58 1304.83 1 5 5 -4 2207.35 1234.72 1 5 5 -3 13726. 1240.51 1 5 5 -2 1125.05 864.362 1 5 5 -1 9546.54 1205.95 -1 5 5 0 2538.95 918.497 1 5 5 1 2409.11 888.133 1 5 5 2 837.59 838.393 1 5 5 3 5423.49 1177.19 1 6 0 -4 8353.97 440.471 1 6 0 -2 180104. 7079.50 1 6 0 0 20895. 1274.07 1 6 0 2 45865. 3270.07 1 6 1 -12 851.38 1141.63 1 6 1 -11 1557.13 824.809 1 6 1 -10 3581.70 795.445 1 6 1 -9 1933.88 463.843 1 6 1 -8 7155.41 556.731 1 6 1 -7 20635. 958.449 -1 6 1 -5 138094. 5465.44 1 6 1 -3 161886. 6406.31 1 6 1 -2 11101. 786.056 1 6 1 -1 33799. 1654.21 1 6 1 0 51019. 2351.18 1 6 1 1 22793. 1370.15 1 6 1 2 45326. 2233.32 1 6 1 3 2057.53 631.442 1 6 1 4 15134. 1379.74 1 6 1 5 553.73 1181.98 1 6 1 6 2049.54 1767.68 1 6 1 7 4186.97 1336.59 1 6 1 8 1853.77 1834.60 1 6 2 -12 531.16 733.120 1 6 2 -11 325.21 721.334 1 6 2 -10 413.10 510.187 1 6 2 -9 37675. 1757.69 1 6 2 -8 5459.44 621.653 1 6 2 -7 39273. 1742.11 1 6 2 -5 13136. 894.126 1 6 2 -4 3993.20 592.488 1 6 2 -3 51838. 2349.18 1 6 2 -2 183080. 7341.18 1 6 2 0 28706. 1587.29 1 6 2 1 27107. 1558.73 -1 6 2 2 1828.40 717.938 1 6 2 3 29125. 1771.87 1 6 2 4 3861.36 886.935 1 6 2 5 2574.91 835.996 1 6 2 6 1628.84 922.892 1 6 2 7 645.42 888.133 1 6 3 -10 1996.00 916.899 1 6 3 -9 1046.54 785.057 1 6 3 -8 32761. 2303.23 1 6 3 -7 -46.02 672.392 1 6 3 -6 21474. 1613.26 1 6 3 -5 2900.52 669.196 1 6 3 -4 3184.18 685.776 1 6 3 -3 1257.09 661.006 1 6 3 -2 3673.59 761.485 1 6 3 0 36796. 2001.60 1 6 3 1 13102. 1286.06 1 6 3 2 1747.50 1168.60 1 6 3 3 1266.48 780.463 -1 6 3 4 2325.21 856.172 -1 6 3 5 770.67 819.815 1 6 3 6 3264.08 1147.42 1 6 4 -9 3607.67 969.236 -1 6 4 -8 4808.23 984.418 1 6 4 -7 1023.17 650.019 1 6 4 -6 5719.13 730.123 1 6 4 -5 1088.89 547.542 1 6 4 -4 3184.18 808.030 1 6 4 -3 424.89 702.956 1 6 4 -2 7598.87 1039.15 1 6 4 -1 5834.99 966.639 1 6 4 0 23871. 1525.57 1 6 4 1 26748. 1795.24 1 6 4 2 2041.55 1016.58 1 6 4 3 797.64 930.882 1 6 4 4 3136.23 900.518 1 6 4 5 1630.64 895.724 1 6 5 -6 4608.47 875.948 1 6 5 -5 2882.54 611.865 1 6 5 -4 -706.35 762.085 1 6 5 -3 6030.76 1242.31 1 6 5 -2 478.43 800.239 1 6 5 -1 2075.51 900.518 1 6 5 0 2197.36 901.517 1 6 5 1 5848.98 978.225 1 7 0 -6 3108.27 385.137 1 7 0 -4 39.33 322.013 1 7 0 -2 -429.08 504.794 1 7 0 0 422.89 700.159 1 7 0 2 738.91 1149.62 1 7 1 -12 -190.83 1029.76 1 7 1 -11 1946.26 762.884 1 7 1 -10 -66.82 498.801 1 7 1 -8 4434.67 418.497 -1 7 1 -7 17845. 1117.86 1 7 1 -5 51498. 2191.37 1 7 1 -4 697.36 471.034 1 7 1 -3 40591. 1821.41 1 7 1 -2 7640.82 734.118 -1 7 1 -1 5379.54 700.159 1 7 1 0 5781.06 791.849 1 7 1 1 436.48 654.614 1 7 1 2 13767. 1184.98 1 7 1 3 6274.46 867.358 1 7 1 4 1540.95 957.051 1 7 1 5 4422.69 1602.28 1 7 1 6 6703.95 1869.55 1 7 2 -11 2614.86 760.287 1 7 2 -10 3663.60 524.969 1 7 2 -9 1589.29 430.483 1 7 2 -8 1246.70 688.973 1 7 2 -7 33220. 1466.44 -1 7 2 -6 29405. 1409.31 1 7 2 -5 11242. 898.721 1 7 2 -2 1750.90 677.386 1 7 2 -1 22054. 1344.59 1 7 2 0 2622.85 720.335 1 7 2 1 10074. 1038.55 -1 7 2 2 2255.29 711.545 1 7 2 3 2918.49 853.375 -1 7 2 4 7558.92 1043.35 1 7 2 5 4908.11 1193.57 1 7 2 6 -66.18 812.025 1 7 3 -10 2003.59 953.655 1 7 3 -9 1369.36 576.707 -1 7 3 -8 1706.35 541.350 1 7 3 -7 1039.35 627.047 1 7 3 -6 16039. 1007.19 -1 7 3 -5 2475.03 689.172 1 7 3 -4 3887.33 759.088 1 7 3 -3 1407.31 634.039 1 7 3 -2 12277. 920.095 1 7 3 -1 19866. 1383.94 1 7 3 0 826.81 830.602 1 7 3 1 10681. 1115.86 1 7 3 2 4324.81 963.842 1 7 3 3 8931.27 1126.85 1 7 3 4 -47.36 746.903 1 7 4 -8 4646.42 895.924 1 7 4 -7 -706.75 728.725 1 7 4 -6 1002.60 695.365 1 7 4 -5 2003.59 1062.32 1 7 4 -4 4868.15 921.693 1 7 4 -3 11764. 1166.20 -1 7 4 -2 604.87 810.826 1 7 4 -1 1222.73 708.150 1 7 4 0 3945.26 1037.35 1 7 4 1 30384. 1900.72 1 7 4 2 1615.66 888.333 1 7 4 3 2530.96 917.898 1 7 5 -4 861.57 1311.23 1 7 5 -3 1869.35 759.488 1 7 5 -2 1093.49 972.033 1 7 5 -1 1109.47 864.362 1 8 0 -4 3985.21 656.012 1 8 0 -2 3076.31 660.407 -1 8 0 0 4182.98 824.210 1 8 0 2 4562.52 952.256 1 8 1 -11 1883.14 535.757 1 8 1 -10 232.92 408.909 1 8 1 -9 595.09 304.834 -1 8 1 -8 17887. 775.868 1 8 1 -6 20376. 1036.36 1 8 1 -4 6731.92 955.652 1 8 1 -3 23991. 1281.06 1 8 1 -1 19604. 1240.51 1 8 1 0 4872.15 780.063 1 8 1 1 393.93 834.797 1 8 1 2 1279.86 629.444 1 8 1 3 91.33 889.132 1 8 1 4 5461.44 1104.87 1 8 1 5 1056.53 1346.78 1 8 1 6 -420.69 1743.31 1 8 2 -11 1874.55 651.817 1 8 2 -9 2269.27 588.094 1 8 2 -8 5401.51 479.624 1 8 2 -7 2746.70 461.046 1 8 2 -6 23132. 1353.57 1 8 2 -5 15186. 1037.35 1 8 2 -4 2678.78 524.770 1 8 2 -2 2363.16 832.600 -1 8 2 -1 37355. 1931.28 1 8 2 0 335.60 678.785 1 8 2 1 537.95 657.410 1 8 2 2 10621. 1178.98 1 8 2 3 3811.42 920.095 -1 8 2 4 -57.17 791.449 1 8 2 5 1079.90 856.971 1 8 3 -9 178.11 684.178 1 8 3 -8 14521. 917.298 1 8 3 -7 2019.57 520.974 1 8 3 -6 3208.15 771.673 1 8 3 -5 4394.72 769.676 1 8 3 -3 4214.94 713.943 -1 8 3 -2 -87.40 772.872 1 8 3 -1 3897.32 1317.82 -1 8 3 0 -460.85 934.278 1 8 3 1 1245.30 811.425 1 8 3 2 1562.52 821.413 1 8 3 3 4105.07 888.932 1 8 3 4 267.68 1099.68 -1 8 4 -7 584.30 549.340 1 8 4 -6 11049. 1062.12 1 8 4 -5 1511.78 1174.79 1 8 4 -4 17980. 1385.34 1 8 4 -3 -269.08 1078.50 1 8 4 -2 2393.13 835.796 1 8 4 -1 1153.81 1128.64 1 8 4 0 5083.89 955.053 1 8 4 1 28.83 805.832 1 8 4 2 685.98 1118.26 1 9 0 -6 1216.14 342.389 1 9 0 -4 529.36 661.406 1 9 0 -2 -1206.0 1019.78 1 9 0 0 -496.20 1099.68 1 9 0 2 515.78 837.394 1 9 0 4 116.70 1217.14 1 9 1 -11 515.98 657.410 1 9 1 -10 389.33 279.864 1 9 1 -9 12040. 563.923 1 9 1 -8 2243.31 228.725 1 9 1 -7 2748.70 475.629 1 9 1 -6 14569. 824.210 1 9 1 -5 14357. 1378.74 -1 9 1 -4 3070.31 706.352 1 9 1 -3 14039. 992.408 -1 9 1 -2 11894. 964.641 1 9 1 -1 7143.42 848.381 1 9 1 0 942.07 697.163 1 9 1 1 3010.38 821.613 1 9 1 2 5385.53 865.560 1 9 1 4 1715.54 994.605 1 9 2 -9 1930.28 418.897 1 9 2 -8 42789. 1834.40 1 9 2 -7 161.89 925.289 1 9 2 -5 2932.48 582.301 1 9 2 -4 18382. 1235.92 1 9 2 -3 6218.53 1283.46 1 9 2 -2 2221.33 713.943 1 9 2 -1 1474.03 670.595 1 9 2 0 3252.09 819.016 1 9 2 1 1803.83 742.908 1 9 2 2 4202.95 944.665 1 9 2 3 2746.70 870.155 1 9 2 4 1626.45 868.157 1 9 3 -8 1412.10 407.311 1 9 3 -7 25110. 1511.19 -1 9 3 -6 1386.34 640.431 1 9 3 -4 1352.78 740.511 1 9 3 -3 3399.92 832.800 1 9 3 -2 2818.61 815.021 1 9 3 -1 1913.90 1129.64 -1 9 3 0 8481.81 1023.37 1 9 3 1 1972.43 744.506 1 9 3 2 1848.38 1052.94 1 9 4 -5 2590.89 864.761 1 9 4 -4 1354.77 746.903 1 9 4 -3 919.50 767.678 1 9 4 -2 -724.53 960.646 1 9 4 -1 3835.39 1579.50 1 10 0 -8 6196.56 375.948 1 10 0 -6 43488. 1889.33 -1 10 0 -4 12709. 968.037 1 10 0 -2 2858.57 778.265 1 10 0 0 5367.55 1019.18 1 10 0 2 4878.14 1018.98 1 10 1 -9 5507.39 454.254 1 10 1 -8 19766. 1055.13 1 10 1 -7 2994.40 469.236 1 10 1 -6 31262. 1526.17 1 10 1 -5 3923.29 582.900 1 10 1 -4 5203.75 704.953 1 10 1 -3 1559.53 588.293 1 10 1 -2 3296.04 713.143 1 10 1 -1 1597.48 727.726 1 10 1 0 2572.91 816.220 1 10 1 2 2179.38 878.944 1 10 1 3 4794.24 1101.88 1 10 2 -8 1186.38 626.248 1 10 2 -7 2866.56 615.061 -1 10 2 -6 4972.03 698.361 1 10 2 -5 4696.36 831.601 1 10 2 -4 441.67 664.402 1 10 2 -2 4478.62 787.454 1 10 2 -1 420.69 715.940 1 10 2 0 871.15 766.879 1 10 2 1 -504.19 734.318 1 10 2 2 1730.72 1098.48 1 10 3 -6 3431.88 764.082 1 10 3 -5 1064.12 926.487 1 10 3 -4 4704.35 849.779 1 10 3 -3 2221.33 789.652 -1 10 3 -2 791.25 744.506 1 10 3 -1 711.75 631.841 1 10 3 0 -76.97 896.523 -1 11 0 -6 609.47 657.610 1 11 0 -4 228.93 669.995 1 11 0 -2 1099.88 1229.92 1 11 0 0 1117.46 1165.20 1 11 1 -8 1576.91 482.421 1 11 1 -7 767.48 506.991 -1 11 1 -6 3937.27 709.748 1 11 1 -5 4814.22 672.193 1 11 1 -4 2914.50 752.696 1 11 1 -3 2279.26 959.847 1 11 1 -1 724.73 672.592 1 11 1 0 1451.66 753.695 -1 11 2 -5 409.31 626.647 1 11 2 -4 803.44 743.907 1 11 2 -3 2648.82 896.723 1 11 2 -2 2033.56 935.876 1 11 2 -1 49.56 588.693 -1 0 0 0 0. 0.00 0 ; _shelx_hkl_checksum 85736 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 0.3193(10) 0.6769(17) 0.4676(11) 0.062(4) Uani 1 1 d . . . . . O1 O 0.3467(11) 0.8602(17) 0.5056(11) 0.082(4) Uani 1 1 d . . . . . C3 C 0.3176(10) 0.3656(16) 0.3688(12) 0.066(4) Uani 1 1 d . . . . . H3A H 0.349527 0.214766 0.371528 0.080 Uiso 1 1 calc R U . . . H3B H 0.295322 0.422201 0.291997 0.080 Uiso 1 1 calc R U . . . O2 O 0.2177(10) 0.594(2) 0.4548(13) 0.097(5) Uani 1 1 d . . . . . C2 C 0.2156(10) 0.380(2) 0.4163(11) 0.076(4) Uani 1 1 d . . . . . H2A H 0.138034 0.348191 0.358755 0.091 Uiso 1 1 calc R U . . . H2B H 0.226832 0.273740 0.477797 0.091 Uiso 1 1 calc R U . . . C5 C 0.5175(10) 0.6056(15) 0.4359(12) 0.074(4) Uani 1 1 d . . . . . H5 H 0.517383 0.766267 0.451341 0.088 Uiso 1 1 calc R U . . . C4 C 0.4016(9) 0.5126(15) 0.4485(10) 0.061(4) Uani 1 1 d . . . . . C7 C 0.5246(11) 0.3928(17) 0.2600(12) 0.077(5) Uani 1 1 d . . . . . H7 H 0.488104 0.269101 0.281812 0.092 Uiso 1 1 calc R U . . . C6 C 0.5450(9) 0.5806(13) 0.3273(9) 0.054(3) Uani 1 1 d . . . . . C8 C 0.5544(10) 0.381(2) 0.1659(12) 0.074(4) Uani 1 1 d . . . . . H8 H 0.536220 0.250351 0.123158 0.089 Uiso 1 1 calc R U . . . C9 C 0.6107(10) 0.5506(18) 0.1288(10) 0.066(4) Uani 1 1 d . . . . . H9 H 0.630838 0.543778 0.061972 0.080 Uiso 1 1 calc R U . . . C10 C 0.6351(10) 0.7343(18) 0.1993(12) 0.070(4) Uani 1 1 d . . . . . H10 H 0.681112 0.850947 0.183640 0.084 Uiso 1 1 calc R U . . . C11 C 0.5958(9) 0.7512(15) 0.2882(11) 0.061(4) Uani 1 1 d . . . . . H11 H 0.603814 0.887917 0.325425 0.073 Uiso 1 1 calc R U . . . 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 0.061(8) 0.031(6) 0.104(11) 0.009(6) 0.042(7) 0.016(5) O1 0.098(8) 0.048(6) 0.125(10) -0.002(6) 0.073(8) 0.017(5) C3 0.063(7) 0.043(6) 0.098(10) 0.005(6) 0.032(7) 0.003(6) O2 0.057(7) 0.080(8) 0.165(14) -0.003(8) 0.048(8) 0.011(6) C2 0.054(7) 0.092(10) 0.077(10) 0.011(7) 0.013(7) -0.009(6) C5 0.082(8) 0.021(5) 0.135(13) -0.024(6) 0.058(9) -0.004(5) C4 0.061(7) 0.033(5) 0.104(10) -0.003(6) 0.047(7) -0.009(5) C7 0.079(9) 0.044(6) 0.133(14) -0.023(7) 0.073(9) -0.017(5) C6 0.058(6) 0.022(5) 0.097(9) -0.016(5) 0.048(6) -0.005(4) C8 0.081(9) 0.061(7) 0.089(10) -0.030(7) 0.038(8) -0.012(6) C9 0.072(8) 0.068(8) 0.074(9) 0.000(7) 0.043(7) -0.011(6) C10 0.071(8) 0.051(7) 0.092(11) 0.009(6) 0.030(8) -0.017(6) C11 0.074(8) 0.032(6) 0.089(9) 0.016(5) 0.044(8) 0.001(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0000 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' 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 O1 C1 O2 122.8(10) . . ? O1 C1 C4 126.1(11) . . ? O2 C1 C4 110.3(10) . . ? C4 C3 C2 97.6(9) . . ? C1 O2 C2 109.7(10) . . ? O2 C2 C3 105.4(10) . . ? C6 C5 C4 120.3(10) . . ? C6 C5 C4 122.8(8) . 3_666 ? C4 C5 C4 91.5(9) . 3_666 ? C1 C4 C3 101.5(9) . . ? C1 C4 C5 114.4(8) . . ? C3 C4 C5 125.4(10) . . ? C1 C4 C5 112.3(10) . 3_666 ? C3 C4 C5 114.9(8) . 3_666 ? C5 C4 C5 88.5(9) . 3_666 ? C8 C7 C6 122.8(10) . . ? C11 C6 C7 114.4(11) . . ? C11 C6 C5 119.4(9) . . ? C7 C6 C5 126.2(9) . . ? C7 C8 C9 122.7(11) . . ? C8 C9 C10 113.9(12) . . ? C11 C10 C9 122.6(10) . . ? C10 C11 C6 123.0(10) . . ? 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 O1 1.196(14) . ? C1 O2 1.226(14) . ? C1 C4 1.431(13) . ? C3 C4 1.445(15) . ? C3 C2 1.463(14) . ? O2 C2 1.368(16) . ? C5 C6 1.486(16) . ? C5 C4 1.490(13) . ? C5 C4 1.611(16) 3_666 ? C7 C8 1.318(17) . ? C7 C6 1.376(14) . ? C6 C11 1.338(13) . ? C8 C9 1.357(15) . ? C9 C10 1.379(15) . ? C10 C11 1.319(16) . ?