#------------------------------------------------------------------------------ #$Date: 2019-11-10 19:00:09 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225975 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515883.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_4515883 loop_ _publ_author_name 'Nomura, Eisaku' 'Noda, Takumi' 'Gomi, Daiki' 'Mori, Hajime' _publ_section_title ; Substituent Effect on the Formation of Arylindanes by Dimerization of Ferulic Acid and its Related Compounds. ; _journal_issue 10 _journal_name_full 'ACS omega' _journal_page_first 12746 _journal_page_last 12753 _journal_paper_doi 10.1021/acsomega.8b01953 _journal_volume 3 _journal_year 2018 _chemical_formula_moiety 'C26 H32 O10' _chemical_formula_sum 'C26 H32 O10' _chemical_formula_weight 504.51 _chemical_name_common 5b _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 _cell_angle_alpha 89.7450(10) _cell_angle_beta 76.6900(10) _cell_angle_gamma 79.1410(10) _cell_formula_units_Z 2 _cell_length_a 8.79880(16) _cell_length_b 10.50228(19) _cell_length_c 13.8851(3) _cell_measurement_reflns_used 8438 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 68.23 _cell_measurement_theta_min 3.27 _cell_volume 1225.25(4) _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 5.000 _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54187 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_unetI/netI 0.0432 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 12901 _diffrn_reflns_point_group_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.970 _diffrn_reflns_theta_full 67.687 _diffrn_reflns_theta_max 68.230 _diffrn_reflns_theta_min 3.274 _exptl_absorpt_coefficient_mu 0.881 _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.368 _exptl_crystal_description prism _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.259 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 325 _refine_ls_number_reflns 4357 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0435 _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^)+(0.0725P)^2^+0.2391P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1183 _refine_ls_wR_factor_ref 0.1270 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3640 _reflns_number_total 4357 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ao8b01953_si_002.cif _cod_data_source_block shelxl _cod_original_cell_volume 1225.24(4) _cod_database_code 4515883 _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_estimated_absorpt_t_min 0.778 _shelx_estimated_absorpt_t_max 0.843 _shelxl_version_number 2013-4 _shelx_res_file ; TITL indane-dime20150309-2 CELL 1.54187 8.79880 10.50228 13.88508 89.745 76.690 79.141 ZERR 2 0.00016 0.00019 0.00025 0.001 0.001 0.001 LATT 1 SFAC C H O UNIT 52 64 20 SHEL 99999.000000 0.000000 L.S. 5 FMAP 2 PLAN -45 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP 23.0 ACTA SIZE 0.200 0.250 0.300 WGHT 0.072500 0.239100 FVAR 1.10731 O1 3 -0.206402 1.049273 0.375582 11.00000 0.02539 0.02088 = 0.01458 0.00050 0.00005 -0.00652 O2 3 -0.483293 0.785940 0.048351 11.00000 0.02378 0.03567 = 0.03230 0.00722 -0.00806 -0.01661 O3 3 0.086042 1.278002 0.129886 11.00000 0.03128 0.02361 = 0.02193 0.00147 -0.00400 -0.01416 O4 3 0.551071 0.241191 0.490972 11.00000 0.01993 0.02931 = 0.02132 0.00019 -0.00280 0.00245 AFIX 83 H4 2 0.618841 0.215411 0.440249 11.00000 -1.20000 AFIX 0 O5 3 0.079871 0.750877 0.473767 11.00000 0.04160 0.03514 = 0.01833 0.00062 -0.00457 -0.01982 O6 3 0.303093 0.356988 0.639077 11.00000 0.02304 0.02293 = 0.01676 0.00170 -0.00607 -0.00684 O7 3 0.174709 0.811812 0.320459 11.00000 0.03639 0.02758 = 0.02144 0.00564 -0.00829 -0.01720 O8 3 0.530087 0.242314 0.301337 11.00000 0.02034 0.02727 = 0.01817 -0.00131 0.00014 0.00151 O9 3 -0.269481 0.691966 0.103048 11.00000 0.03086 0.03844 = 0.04761 0.01853 -0.01378 -0.01652 O10 3 -0.057866 1.249319 0.321688 11.00000 0.04459 0.02546 = 0.01494 -0.00072 -0.00470 -0.01593 AFIX 83 H10 2 -0.084725 1.221544 0.377061 11.00000 -1.20000 AFIX 0 C11 1 0.262439 0.378022 0.346945 11.00000 0.02219 0.02000 = 0.01562 0.00095 -0.00371 -0.00553 AFIX 43 H11 2 0.253583 0.382681 0.281504 11.00000 -1.20000 AFIX 0 C12 1 0.146158 0.429996 0.521330 11.00000 0.01891 0.01499 = 0.01838 0.00039 -0.00227 -0.00588 C13 1 0.136337 0.440326 0.423058 11.00000 0.01773 0.01656 = 0.01772 0.00101 -0.00244 -0.00610 C14 1 0.004046 1.088545 0.077932 11.00000 0.01788 0.02185 = 0.01596 0.00098 -0.00317 -0.00451 C15 1 -0.064571 1.160828 0.252196 11.00000 0.02141 0.02015 = 0.01739 -0.00141 -0.00416 -0.00487 C16 1 -0.147435 0.969666 0.202500 11.00000 0.01781 0.01904 = 0.02086 0.00095 -0.00319 -0.00519 AFIX 43 H16 2 -0.199268 0.900401 0.218951 11.00000 -1.20000 AFIX 0 C17 1 -0.075808 0.986404 0.103047 11.00000 0.01720 0.01835 = 0.01756 -0.00162 -0.00293 -0.00315 C18 1 0.289185 0.365631 0.541646 11.00000 0.02251 0.01665 = 0.01747 0.00184 -0.00442 -0.00838 C19 1 -0.336857 0.780418 0.063834 11.00000 0.02170 0.03081 = 0.01927 -0.00078 -0.00331 -0.01044 C20 1 -0.141329 1.055454 0.275966 11.00000 0.01654 0.02172 = 0.01641 0.00085 -0.00202 -0.00072 C21 1 0.399622 0.309825 0.368975 11.00000 0.02019 0.01785 = 0.01938 -0.00005 0.00074 -0.00427 C22 1 -0.005781 0.521218 0.393003 11.00000 0.02113 0.01802 = 0.01455 -0.00009 -0.00348 -0.00573 AFIX 13 H22 2 -0.041588 0.465822 0.349607 11.00000 -1.20000 AFIX 0 C23 1 0.047432 0.634947 0.331096 11.00000 0.01830 0.02236 = 0.01445 0.00147 -0.00174 -0.00306 AFIX 23 H23A 2 0.134072 0.599081 0.275590 11.00000 -1.20000 H23B 2 -0.040493 0.677813 0.304204 11.00000 -1.20000 AFIX 0 C24 1 0.415413 0.305059 0.466656 11.00000 0.01765 0.01729 = 0.02125 0.00224 -0.00357 -0.00330 C25 1 0.005444 1.176656 0.154011 11.00000 0.02112 0.02039 = 0.01979 0.00177 -0.00457 -0.00756 C26 1 -0.095545 0.892425 0.025805 11.00000 0.01839 0.02057 = 0.01664 0.00030 -0.00205 -0.00775 AFIX 13 H26 2 -0.053862 0.804550 0.043706 11.00000 -1.20000 AFIX 0 C27 1 0.401053 0.441381 0.663435 11.00000 0.03073 0.03423 = 0.02642 -0.00141 -0.01112 -0.01165 AFIX 33 H27A 2 0.508875 0.412931 0.626656 11.00000 -1.20000 H27B 2 0.397203 0.439109 0.733070 11.00000 -1.20000 H27C 2 0.362480 0.528448 0.646842 11.00000 -1.20000 AFIX 0 C28 1 -0.274951 0.900460 0.028149 11.00000 0.02137 0.02248 = 0.02010 -0.00056 -0.00345 -0.00700 AFIX 23 H28A 2 -0.336807 0.973862 0.070963 11.00000 -1.20000 H28B 2 -0.290867 0.916385 -0.038025 11.00000 -1.20000 AFIX 0 C29 1 0.533480 0.257847 0.199197 11.00000 0.03253 0.02967 = 0.01780 0.00054 0.00109 0.00139 AFIX 33 H29A 2 0.531780 0.347286 0.183975 11.00000 -1.20000 H29B 2 0.442230 0.231495 0.184587 11.00000 -1.20000 H29C 2 0.628722 0.205255 0.160024 11.00000 -1.20000 AFIX 0 C30 1 0.100880 0.735663 0.385282 11.00000 0.01830 0.02241 = 0.01860 0.00391 -0.00259 -0.00321 C31 1 -0.561180 0.679905 0.086213 11.00000 0.03013 0.04139 = 0.04597 0.00960 -0.00850 -0.02265 AFIX 23 H31A 2 -0.566067 0.672308 0.156461 11.00000 -1.20000 H31B 2 -0.502568 0.598770 0.052206 11.00000 -1.20000 AFIX 0 C32 1 0.223404 0.920064 0.362367 11.00000 0.03575 0.02705 = 0.02951 0.00445 -0.01361 -0.01499 AFIX 23 H32A 2 0.285638 0.889478 0.410084 11.00000 -1.20000 H32B 2 0.130633 0.982749 0.395791 11.00000 -1.20000 AFIX 0 C33 1 -0.291272 0.946565 0.405147 11.00000 0.03361 0.02409 = 0.02029 0.00108 0.00170 -0.01046 AFIX 33 H33A 2 -0.381027 0.956076 0.375569 11.00000 -1.20000 H33B 2 -0.327632 0.950134 0.475964 11.00000 -1.20000 H33C 2 -0.222087 0.864590 0.383742 11.00000 -1.20000 AFIX 0 C34 1 -0.018568 1.400113 0.125195 11.00000 0.04780 0.02380 = 0.02771 0.00403 -0.00973 -0.01334 AFIX 33 H34A 2 -0.067903 1.396221 0.070668 11.00000 -1.20000 H34B 2 0.041668 1.468331 0.115986 11.00000 -1.20000 H34C 2 -0.099131 1.417102 0.185806 11.00000 -1.20000 AFIX 0 C35 1 0.321140 0.981292 0.278828 11.00000 0.04990 0.04006 = 0.04093 0.01107 -0.01457 -0.02725 AFIX 33 H35A 2 0.257022 1.014583 0.233607 11.00000 -1.20000 H35B 2 0.410301 0.917563 0.244722 11.00000 -1.20000 H35C 2 0.358775 1.050995 0.304581 11.00000 -1.20000 AFIX 0 C36 1 -0.726513 0.709335 0.068541 11.00000 0.03784 0.07322 = 0.02877 0.01317 -0.01029 -0.03535 AFIX 33 H36A 2 -0.779402 0.638482 0.089589 11.00000 -1.20000 H36B 2 -0.720290 0.721118 -0.000765 11.00000 -1.20000 H36C 2 -0.785280 0.787173 0.105530 11.00000 -1.20000 AFIX 0 HKLF 4 REM indane-dime20150309-2 REM R1 = 0.0435 for 3640 Fo > 4sig(Fo) and 0.0527 for all 4357 data REM 325 parameters refined using 0 restraints END WGHT 0.0725 0.2391 REM Instructions for potential hydrogen bonds EQIV $1 x+1, y-1, z HTAB O4 O1_$1 HTAB O4 O8 HTAB O10 O1 EQIV $2 -x, -y+2, -z+1 HTAB O10 O5_$2 EQIV $3 -x, -y+1, -z+1 HTAB C23 O6_$3 HTAB C27 O4 EQIV $4 -x+1, -y+1, -z+1 HTAB C32 O4_$4 HTAB C33 O6_$3 HTAB C34 O10 REM Highest difference peak 0.259, deepest hole -0.300, 1-sigma level 0.072 Q1 1 0.1617 0.4755 0.4761 11.00000 0.05 0.26 Q2 1 0.0834 1.0582 -0.0665 11.00000 0.05 0.23 Q3 1 -0.0191 0.4225 0.6357 11.00000 0.05 0.22 Q4 1 0.2461 0.3423 0.2774 11.00000 0.05 0.21 Q5 1 -0.7724 0.8006 -0.0037 11.00000 0.05 0.20 Q6 1 -0.1392 1.3803 0.1048 11.00000 0.05 0.19 Q7 1 -0.0630 1.0659 0.0847 11.00000 0.05 0.19 Q8 1 -0.4619 0.9840 0.3471 11.00000 0.05 0.19 Q9 1 0.6940 0.2425 0.1698 11.00000 0.05 0.19 Q10 1 -0.0629 0.6462 0.2314 11.00000 0.05 0.19 Q11 1 -0.4734 0.8795 0.2992 11.00000 0.05 0.18 Q12 1 -0.0269 0.6584 0.1226 11.00000 0.05 0.18 Q13 1 0.6942 0.2646 0.4962 11.00000 0.05 0.18 Q14 1 -0.0733 0.6005 0.1848 11.00000 0.05 0.17 Q15 1 0.0532 0.9992 0.3010 11.00000 0.05 0.17 Q16 1 -0.3902 0.9361 0.1874 11.00000 0.05 0.17 Q17 1 -0.3518 0.9671 0.1199 11.00000 0.05 0.17 Q18 1 0.2183 0.1929 0.3462 11.00000 0.05 0.17 Q19 1 0.4768 0.2064 0.1607 11.00000 0.05 0.17 Q20 1 0.1441 1.0750 0.3166 11.00000 0.05 0.17 Q21 1 0.0295 1.1005 0.0329 11.00000 0.05 0.17 Q22 1 -0.7793 0.9267 0.1181 11.00000 0.05 0.17 Q23 1 -0.1122 1.2229 0.0351 11.00000 0.05 0.17 Q24 1 0.0000 1.5000 0.0000 10.50000 0.05 0.17 Q25 1 -0.0928 0.7364 0.2575 11.00000 0.05 0.17 Q26 1 -0.0829 1.2020 0.1983 11.00000 0.05 0.17 Q27 1 0.0280 0.7636 0.0512 11.00000 0.05 0.17 Q28 1 0.5321 0.8622 0.2192 11.00000 0.05 0.17 Q29 1 0.6564 0.4205 0.6014 11.00000 0.05 0.16 Q30 1 -0.3825 0.9074 0.2025 11.00000 0.05 0.16 Q31 1 0.2620 1.1089 0.3212 11.00000 0.05 0.16 Q32 1 -0.8643 0.7358 -0.0214 11.00000 0.05 0.16 Q33 1 -0.3944 0.9778 0.3027 11.00000 0.05 0.16 Q34 1 0.2518 0.4362 0.5268 11.00000 0.05 0.16 Q35 1 0.4117 0.9125 0.2838 11.00000 0.05 0.16 Q36 1 0.0813 0.9980 0.3745 11.00000 0.05 0.16 Q37 1 -0.5523 0.5842 -0.0158 11.00000 0.05 0.16 Q38 1 0.2465 0.5375 0.4964 11.00000 0.05 0.16 Q39 1 -0.4435 0.5292 -0.0141 11.00000 0.05 0.16 Q40 1 -0.0035 0.7025 0.1951 11.00000 0.05 0.16 Q41 1 0.6404 0.3247 0.5787 11.00000 0.05 0.16 Q42 1 0.0422 1.1363 0.1992 11.00000 0.05 0.16 Q43 1 -0.0074 0.9702 0.3770 11.00000 0.05 0.16 Q44 1 -0.4790 0.6112 0.0007 11.00000 0.05 0.15 Q45 1 0.2199 0.5559 0.6973 11.00000 0.05 0.15 ; _shelx_res_checksum 94682 _shelx_hkl_file ; 0 0 1 1846.73 70.68 0 0 1 1980.48 77.83 0 0 1 1893.53 74.77 0 0 1 1832.15 72.73 0 0 1 1912.59 73.50 0 0 -1 1846.36 73.52 0 0 -1 1903.69 73.15 0 0 -1 1958.79 77.61 0 0 -1 1946.97 76.58 0 0 -1 1837.17 70.11 0 0 2 990.86 35.76 0 0 2 1021.21 39.95 0 0 2 1011.64 39.30 0 0 2 1021.32 39.56 0 0 -2 990.68 43.33 0 0 -2 1025.62 37.67 0 0 -2 1005.10 38.76 0 0 -2 1045.81 40.95 0 0 3 4044.23 209.40 0 0 3 4099.73 213.62 0 0 3 4132.81 213.61 0 0 3 3963.42 197.22 0 0 -3 4123.72 212.93 0 0 -3 4201.79 210.41 0 0 -3 3940.24 206.35 0 0 -3 4115.64 215.22 0 0 4 3502.83 180.45 0 0 4 3469.69 179.18 0 0 4 3566.57 184.95 0 0 4 3484.71 170.66 0 0 -4 3350.97 175.61 0 0 -4 3478.17 172.88 0 0 -4 3480.19 179.63 0 0 -4 3471.03 181.93 0 0 5 3379.22 176.79 0 0 5 3273.28 170.58 0 0 5 3300.03 171.94 0 0 5 3232.71 158.67 0 0 -5 3202.41 170.05 0 0 -5 3291.82 164.37 0 0 -5 3178.20 168.05 0 0 -5 3291.74 171.72 0 0 6 460.06 19.13 0 0 6 478.89 18.54 0 0 6 476.11 23.42 0 0 6 525.56 25.58 0 0 -6 479.88 19.59 0 0 -6 475.15 24.44 0 0 -6 480.71 24.02 0 0 -6 494.69 24.31 0 0 7 2168.48 101.99 0 0 7 2198.54 112.93 0 0 7 2274.49 115.98 0 0 7 2109.07 102.43 0 0 -7 2182.56 113.39 0 0 -7 2165.83 103.33 0 0 -7 2282.61 116.44 0 0 -7 2140.42 112.71 0 0 8 83.35 4.63 0 0 8 83.16 4.23 0 0 8 94.31 5.35 0 0 8 100.91 8.67 0 0 -8 85.53 4.86 0 0 -8 103.24 8.59 0 0 -8 102.19 8.79 0 0 -8 99.88 8.83 0 0 9 109.80 13.32 0 0 -9 114.78 10.47 0 0 -9 109.23 10.10 0 0 10 9.68 4.46 0 0 -10 16.64 5.10 0 0 -10 9.31 4.39 0 0 11 -0.60 2.96 0 0 -11 3.99 3.39 0 0 -11 -0.71 2.74 0 0 12 162.06 12.88 0 0 -12 169.11 14.51 0 0 -12 164.01 12.70 0 0 13 1.74 3.24 0 0 -13 5.05 4.03 0 0 -13 -0.00 2.92 0 0 14 55.33 6.53 0 0 -14 53.20 8.36 0 0 -14 46.11 6.04 0 0 15 127.80 9.03 0 0 -15 133.19 11.67 0 0 -16 6.80 3.85 0 1 -16 4.97 3.74 0 1 -15 45.76 7.32 0 1 -14 5.03 3.59 0 -1 14 -0.75 2.10 0 1 -13 41.73 5.38 0 1 -13 50.01 8.08 0 -1 13 43.74 5.77 0 1 -12 33.28 7.96 0 1 -12 34.16 5.30 0 -1 12 34.12 5.75 0 1 -11 21.38 4.51 0 1 -11 27.15 6.39 0 -1 11 23.78 5.06 0 1 -10 375.01 23.06 0 1 -10 357.81 19.96 0 -1 10 381.24 20.94 0 1 -9 532.08 30.27 0 1 -9 582.53 29.38 0 1 -9 543.54 25.46 0 1 -9 632.69 32.81 0 -1 9 637.02 31.34 0 1 -8 282.89 17.57 0 1 -8 309.65 17.64 0 1 -8 288.63 13.17 0 1 -8 293.35 15.74 0 1 -8 303.54 17.95 0 1 -8 305.65 17.13 0 -1 8 276.15 13.23 0 -1 8 311.57 16.19 0 -1 8 295.24 12.79 0 1 -7 19.46 3.83 0 1 -7 5.46 3.37 0 1 -7 0.11 2.00 0 1 -7 8.01 3.52 0 1 -7 5.28 3.17 0 -1 7 6.07 3.03 0 -1 7 6.13 2.68 0 -1 7 10.30 3.03 0 -1 7 -0.06 2.25 0 -1 7 6.42 2.11 0 1 -6 3615.50 197.58 0 1 -6 3614.32 197.09 0 1 -6 3662.10 193.67 0 1 -6 3659.25 198.55 0 1 -6 3620.47 197.25 0 -1 6 3661.73 191.05 0 -1 6 3857.65 206.82 0 -1 6 3463.93 183.51 0 -1 6 3435.00 183.21 0 1 -5 618.07 28.85 0 1 -5 630.96 28.34 0 1 -5 624.19 28.56 0 1 -5 604.63 26.14 0 1 -5 627.75 29.34 0 -1 5 644.16 28.29 0 -1 5 653.57 28.93 0 -1 5 621.19 25.53 0 -1 5 584.57 25.50 0 1 -4 201.22 10.86 0 1 -4 181.17 10.15 0 1 -4 151.36 8.26 0 1 -4 181.04 10.90 0 1 -4 179.76 10.77 0 1 -4 169.64 9.34 0 -1 4 198.85 10.51 0 -1 4 166.07 9.53 0 -1 4 186.83 9.00 0 -1 4 196.10 10.16 0 1 -3 2654.17 122.88 0 1 -3 2651.39 125.97 0 1 -3 2296.80 109.01 0 1 -3 2638.34 125.23 0 -1 3 2704.94 125.46 0 -1 3 2436.82 115.29 0 -1 3 2562.63 119.02 0 1 -2 419.21 17.41 0 1 -2 545.79 20.95 0 1 -2 556.19 19.56 0 -1 2 558.64 21.16 0 -1 2 527.73 20.29 0 -1 2 442.74 17.99 0 -1 2 511.89 19.22 0 -1 2 541.66 19.29 0 1 -1 3896.32 199.56 0 1 -1 3977.81 188.23 0 1 -1 3995.32 195.48 0 -1 1 3864.63 190.18 0 -1 1 3988.41 194.94 0 -1 1 4061.27 191.72 0 1 0 543.79 18.22 0 1 0 509.64 16.15 0 1 0 541.61 16.94 0 1 0 485.18 17.22 0 1 0 554.05 18.50 0 -1 0 452.02 14.69 0 -1 0 592.85 21.71 0 -1 0 552.83 18.39 0 -1 0 518.46 17.30 0 -1 0 552.10 17.14 0 1 1 1403.21 56.04 0 1 1 1546.98 60.94 0 1 1 1516.13 57.27 0 1 1 1500.88 57.03 0 1 1 1321.74 53.03 0 1 1 1441.76 58.24 0 -1 -1 1455.80 57.89 0 -1 -1 1504.84 59.39 0 -1 -1 1629.27 62.38 0 1 2 640.62 24.87 0 1 2 594.96 20.10 0 1 2 620.44 25.78 0 -1 -2 657.87 26.39 0 -1 -2 633.49 21.93 0 -1 -2 643.48 24.85 0 -1 -2 578.98 23.40 0 1 3 8084.07 493.77 0 1 3 7791.95 452.48 0 1 3 7903.23 477.16 0 -1 -3 8149.64 477.67 0 -1 -3 6968.84 425.44 0 -1 -3 8221.89 495.10 0 -1 -3 7455.46 457.94 0 -1 -3 7817.57 478.01 0 1 4 5938.88 319.49 0 1 4 6169.08 348.19 0 1 4 5879.24 344.02 0 -1 -4 4672.80 258.95 0 -1 -4 5850.24 336.36 0 -1 -4 4958.31 286.02 0 -1 -4 6210.69 350.33 0 -1 -4 5738.99 331.88 0 1 5 3690.16 181.93 0 1 5 3761.10 200.64 0 1 5 3806.70 201.34 0 -1 -5 3727.05 201.49 0 -1 -5 3873.14 204.19 0 -1 -5 3666.92 199.18 0 -1 -5 3049.34 165.82 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4 14.55 3.37 0 -2 4 19.99 4.54 0 -2 4 -0.04 3.59 0 2 -3 209.09 16.63 0 2 -3 197.72 15.91 0 2 -3 157.46 11.02 0 2 -3 231.36 9.54 0 -2 3 232.69 12.14 0 -2 3 222.69 9.57 0 -2 3 228.77 12.37 0 -2 3 212.27 11.62 0 2 -2 712.70 37.57 0 2 -2 782.89 28.84 0 2 -2 774.53 33.11 0 -2 2 750.10 31.99 0 -2 2 759.32 27.93 0 -2 2 813.00 34.27 0 -2 2 773.72 33.52 0 2 -1 49.68 5.52 0 2 -1 50.69 3.22 0 2 -1 51.23 5.10 0 2 -1 49.95 7.85 0 -2 1 57.82 3.07 0 -2 1 50.28 5.50 0 -2 1 52.79 7.69 0 2 0 4572.97 233.34 0 2 0 4662.31 244.08 0 2 0 4590.09 240.26 0 2 0 4428.66 234.68 0 -2 0 4794.62 243.31 0 -2 0 4670.29 255.27 0 -2 0 4408.36 230.03 0 -2 0 4784.72 249.86 0 2 1 1179.68 48.71 0 2 1 1129.87 48.94 0 2 1 1102.48 45.14 0 -2 -1 1216.49 53.34 0 -2 -1 1225.96 50.43 0 -2 -1 1060.87 44.45 0 2 2 704.69 26.62 0 2 2 662.44 29.90 0 2 2 705.05 30.11 0 2 2 697.62 30.22 0 -2 -2 713.26 30.29 0 -2 -2 735.86 31.28 0 -2 -2 726.32 31.66 0 -2 -2 746.74 29.55 0 2 3 803.34 37.38 0 2 3 797.89 35.24 0 2 3 772.66 35.19 0 2 3 821.36 30.99 0 -2 -3 835.65 36.69 0 -2 -3 803.58 36.99 0 -2 -3 924.45 36.14 0 -2 -3 772.46 35.09 0 2 4 483.19 24.37 0 2 4 469.26 21.87 0 2 4 485.02 17.46 0 2 4 454.43 22.27 0 -2 -4 474.45 18.05 0 -2 -4 465.97 23.68 0 -2 -4 496.56 22.87 0 -2 -4 435.02 21.42 0 2 5 3561.51 190.33 0 2 5 3588.62 189.95 0 2 5 3409.90 168.47 0 -2 -5 3616.20 192.00 0 -2 -5 3159.26 171.30 0 -2 -5 3448.48 188.39 0 -2 -5 3476.05 173.77 0 2 6 444.93 22.92 0 2 6 463.10 22.72 0 2 6 444.33 23.57 0 2 6 414.57 16.15 0 -2 -6 406.31 21.41 0 -2 -6 472.29 23.14 0 -2 -6 422.07 16.67 0 -2 -6 435.82 23.71 0 2 7 833.07 41.87 0 2 7 858.49 40.95 0 2 7 838.04 41.62 0 -2 -7 693.09 36.65 0 -2 -7 806.20 42.32 0 -2 -7 768.50 31.41 0 -2 -7 863.83 41.59 0 2 8 1583.03 83.15 0 2 8 1603.85 81.68 0 2 8 1601.62 83.43 0 -2 -8 1644.49 83.57 0 -2 -8 1278.34 69.60 0 -2 -8 1566.77 84.00 0 2 9 2.88 4.30 0 2 9 2.17 3.62 0 -2 -9 3.86 4.44 0 2 10 1205.91 66.62 0 2 10 1279.46 72.47 0 2 11 887.48 59.93 0 -2 -11 858.87 48.87 0 -2 -11 851.74 52.44 0 2 12 69.75 10.40 0 -2 -12 68.97 9.66 0 -2 -12 69.87 9.75 0 -2 -13 321.39 21.36 0 -2 -13 305.84 21.13 0 -2 -14 3.77 4.35 0 -2 -14 4.41 4.07 0 -2 -15 4.31 3.71 0 -2 -15 7.76 4.01 0 3 -15 2.46 3.51 0 3 -14 58.35 8.68 0 3 -13 187.58 15.33 0 3 -12 351.06 23.88 0 3 -11 161.53 14.34 0 3 -10 118.29 11.54 0 3 -10 110.96 12.15 0 -3 10 98.41 7.40 0 -3 10 106.47 7.40 0 3 -9 20.71 3.58 0 3 -9 35.80 6.54 0 3 -9 22.13 5.21 0 -3 9 20.09 3.91 0 -3 9 6.52 2.91 0 3 -8 449.17 22.11 0 3 -8 424.56 20.15 0 3 -8 442.04 21.64 0 3 -8 444.37 29.31 0 3 -8 454.27 25.47 0 -3 8 462.65 22.67 0 -3 8 460.46 23.35 0 -3 8 455.17 21.09 0 -3 8 443.41 20.76 0 3 -7 2745.74 142.43 0 3 -7 2827.20 153.46 0 3 -7 2785.24 151.68 0 3 -7 2501.04 135.37 0 3 -7 2824.70 148.61 0 3 -7 2655.82 156.49 0 -3 7 2729.43 142.06 0 -3 7 2880.02 147.83 0 -3 7 2853.84 149.80 0 -3 7 2870.49 152.96 0 3 -6 23.20 5.39 0 3 -6 29.95 5.29 0 3 -6 28.01 7.27 0 3 -6 25.97 2.82 0 3 -6 42.91 3.57 0 3 -6 23.86 4.32 0 -3 6 34.81 4.30 0 -3 6 17.07 2.98 0 -3 6 23.29 2.96 0 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24.99 0 -3 -1 541.71 22.25 0 -3 -1 523.55 22.06 0 -3 -1 553.56 28.28 0 3 2 1728.11 81.14 0 3 2 1713.37 76.98 0 3 2 1805.49 80.39 0 3 2 1641.39 78.32 0 3 2 1698.63 79.17 0 -3 -2 2165.66 109.41 0 -3 -2 1766.92 80.80 0 -3 -2 1810.82 84.71 0 -3 -2 1807.36 84.51 0 3 3 1384.14 66.06 0 3 3 1425.59 66.23 0 3 3 1403.60 59.51 0 3 3 1429.37 66.09 0 -3 -3 1448.47 68.36 0 -3 -3 1474.71 67.76 0 -3 -3 1364.61 60.77 0 -3 -3 1547.70 70.94 0 3 4 2876.33 139.38 0 3 4 2952.64 154.22 0 3 4 2960.15 153.74 0 3 4 3040.90 160.44 0 -3 -4 2981.08 148.69 0 -3 -4 3001.56 158.78 0 -3 -4 3112.40 160.96 0 -3 -4 2990.90 155.92 0 3 5 1862.85 95.06 0 3 5 1814.17 91.05 0 3 5 1810.90 89.14 0 3 5 1760.35 77.33 0 -3 -5 1831.49 84.15 0 -3 -5 1736.34 87.49 0 -3 -5 1757.82 90.53 0 -3 -5 1888.76 92.74 0 3 6 329.20 17.68 0 3 6 294.17 11.03 0 -3 -6 311.00 19.48 0 -3 -6 309.69 17.68 0 -3 -6 333.07 17.87 0 -3 -6 329.57 13.73 0 3 7 117.30 9.59 0 -3 -7 98.30 10.05 0 -3 -7 113.45 11.38 0 -3 -7 118.33 9.80 0 3 8 213.85 14.38 0 -3 -8 208.88 16.94 0 3 9 388.32 23.57 0 3 9 526.37 31.41 0 -3 -9 381.95 26.78 0 3 10 677.29 38.86 0 3 10 694.31 41.75 0 -3 -10 673.50 42.51 0 3 11 2243.65 130.10 0 3 11 2369.93 139.63 0 -3 -11 2317.14 140.97 0 3 12 243.82 18.78 0 -3 -12 236.06 17.83 0 3 13 33.20 7.65 0 -3 -13 34.39 7.42 0 -3 -13 34.67 7.77 0 3 14 37.03 7.47 0 -3 -14 32.07 6.93 0 -3 -14 35.99 7.07 0 3 15 11.35 5.98 0 -3 -15 22.30 5.07 0 -3 -15 20.82 5.08 0 4 -15 3.03 3.67 0 4 -14 81.43 9.12 0 4 -13 -0.23 3.21 0 4 -12 594.56 35.30 0 4 -11 90.91 10.82 0 4 -11 78.10 8.49 0 4 -10 433.06 25.82 0 4 -10 294.72 25.31 0 -4 10 388.01 21.19 0 4 -9 71.04 11.22 0 4 -9 68.02 8.88 0 -4 9 59.48 6.80 0 4 -8 228.43 19.61 0 4 -8 206.35 15.06 0 -4 8 215.50 13.87 0 4 -7 320.36 18.22 0 4 -7 333.72 15.81 0 4 -7 367.69 21.02 0 4 -7 385.53 26.82 0 4 -7 358.63 20.76 0 -4 7 335.31 15.40 0 -4 7 393.80 19.98 0 -4 7 394.03 21.63 0 4 -6 1.21 3.39 0 4 -6 5.32 2.99 0 4 -6 -0.04 1.64 0 4 -6 6.06 5.12 0 4 -6 7.95 3.28 0 -4 6 2.34 1.35 0 -4 6 3.16 1.36 0 4 -5 530.92 32.78 0 4 -5 419.79 23.41 0 4 -5 501.09 25.64 0 4 -5 497.17 20.06 0 4 -5 507.48 25.74 0 -4 5 558.19 23.19 0 -4 5 519.73 25.50 0 4 -4 744.26 42.84 0 4 -4 693.94 33.30 0 4 -4 531.93 28.65 0 4 -4 693.38 27.75 0 -4 4 699.08 27.62 0 -4 4 733.16 34.74 0 -4 4 719.37 35.16 0 -4 4 701.59 33.34 0 4 -3 1285.12 67.53 0 4 -3 868.56 44.64 0 4 -3 1147.57 46.53 0 4 -3 1124.76 52.88 0 -4 3 1134.71 53.02 0 -4 3 1243.12 51.81 0 -4 3 1159.36 54.95 0 -4 3 1190.49 54.90 0 4 -2 713.68 35.98 0 4 -2 804.56 40.63 0 4 -2 964.25 37.28 0 4 -2 904.05 41.61 0 -4 2 891.04 41.26 0 -4 2 896.09 41.04 0 -4 2 989.30 38.24 0 -4 2 973.23 43.91 0 4 -1 895.69 35.25 0 4 -1 800.48 39.92 0 4 -1 840.09 39.73 0 -4 1 881.16 47.66 0 -4 1 820.88 38.21 0 -4 1 903.76 35.38 0 4 0 2674.36 137.94 0 4 0 2650.89 127.56 0 4 0 2603.16 132.15 0 -4 0 2565.92 141.20 0 -4 0 2771.92 132.07 0 -4 0 2524.61 127.08 0 4 1 73.20 6.68 0 4 1 64.26 4.88 0 4 1 67.07 5.95 0 4 1 70.40 6.60 0 4 1 69.66 5.05 0 -4 -1 64.82 8.57 0 -4 -1 68.65 4.85 0 -4 -1 66.48 5.65 0 4 2 730.26 33.59 0 4 2 742.06 32.29 0 4 2 735.14 31.56 0 4 2 705.50 30.51 0 4 2 671.48 31.21 0 -4 -2 683.65 28.78 0 -4 -2 728.77 32.97 0 -4 -2 751.89 32.24 0 -4 -2 770.24 35.22 0 -4 -2 756.78 37.23 0 4 3 254.64 11.34 0 4 3 247.50 13.89 0 4 3 244.50 13.94 0 4 3 256.36 13.27 0 4 3 257.12 11.30 0 -4 -3 269.59 14.43 0 -4 -3 259.69 13.11 0 -4 -3 282.88 15.04 0 -4 -3 255.39 14.09 0 -4 -3 239.83 10.36 0 4 4 232.86 10.05 0 4 4 241.85 14.79 0 4 4 227.30 10.01 0 4 4 238.72 13.67 0 4 4 243.25 13.62 0 -4 -4 273.46 13.85 0 -4 -4 248.06 14.34 0 -4 -4 248.49 15.02 0 -4 -4 236.12 13.03 0 4 5 483.22 25.84 0 4 5 415.33 17.43 0 4 5 463.55 24.07 0 4 5 447.79 22.67 0 4 5 437.92 17.43 0 -4 -5 485.67 24.12 0 -4 -5 454.46 23.23 0 -4 -5 375.48 18.80 0 -4 -5 442.46 24.20 0 4 6 11.28 4.74 0 4 6 29.47 4.41 0 4 6 11.93 4.92 0 -4 -6 7.34 1.89 0 -4 -6 10.07 4.58 0 -4 -6 9.80 4.48 0 -4 -6 15.25 5.32 0 4 7 400.71 28.33 0 4 7 406.29 23.81 0 -4 -7 391.79 24.61 0 4 8 6.98 4.95 0 4 8 4.43 4.07 0 -4 -8 5.19 5.47 0 4 9 788.76 43.73 0 -4 -9 782.39 47.42 0 4 10 2003.45 116.50 0 4 10 1953.20 110.54 0 -4 -10 1943.76 117.26 0 4 11 376.55 24.44 0 4 11 373.80 26.98 0 -4 -11 361.48 28.00 0 -4 -12 19.25 8.37 0 -4 -12 16.19 5.94 0 4 13 163.03 15.12 0 -4 -13 157.84 12.99 0 -4 -13 156.99 14.45 0 4 14 2.13 4.26 0 -4 -14 5.56 4.10 0 -4 -14 2.07 3.75 0 4 15 183.49 12.57 0 -4 -15 189.48 13.40 0 -4 -15 173.98 11.81 0 5 -15 0.09 2.13 0 5 -14 96.73 9.78 0 5 -13 242.62 17.25 0 5 -12 195.03 15.61 0 5 -12 150.41 11.72 0 5 -11 82.48 9.77 0 5 -11 95.06 10.96 0 -5 11 85.55 7.62 0 5 -10 19.70 6.73 0 5 -10 16.44 5.92 0 -5 10 18.76 4.63 0 5 -9 104.94 11.76 0 5 -9 126.58 11.89 0 -5 9 121.08 10.14 0 5 -8 553.23 46.53 0 5 -8 454.17 27.12 0 -5 8 442.34 25.46 0 5 -7 121.75 18.18 0 5 -7 194.73 13.56 0 -5 7 198.86 13.44 0 5 -6 1.87 2.81 0 5 -6 1.67 3.05 0 5 -6 2.07 3.10 0 5 -6 0.75 5.18 0 -5 6 -0.02 3.08 0 -5 6 -0.25 2.94 0 5 -5 1393.76 70.88 0 5 -5 1210.78 65.22 0 -5 5 1431.12 72.05 0 -5 5 1512.39 75.28 0 -5 5 1386.74 70.29 0 5 -4 1321.11 57.54 0 5 -4 1207.36 63.58 0 5 -4 1248.34 67.46 0 5 -4 1402.89 69.47 0 -5 4 1402.70 70.06 0 -5 4 1458.35 71.89 0 -5 4 1513.62 73.94 0 -5 4 1352.87 58.16 0 5 -3 30.63 5.16 0 5 -3 26.11 5.67 0 5 -3 30.53 2.16 0 -5 3 40.99 5.81 0 -5 3 30.51 5.69 0 -5 3 41.31 5.82 0 -5 3 28.81 2.92 0 5 -2 1359.60 70.07 0 5 -2 1528.76 78.74 0 5 -2 1566.70 69.57 0 5 -2 1622.06 79.56 0 -5 2 1703.07 82.62 0 -5 2 1588.92 77.52 0 -5 2 1674.79 72.23 0 -5 2 1587.86 77.83 0 5 -1 54.30 3.34 0 5 -1 53.23 7.21 0 -5 1 51.91 3.20 0 -5 1 52.49 6.27 0 5 0 61.97 4.29 0 5 0 67.36 6.86 0 5 0 98.65 8.61 0 -5 0 74.55 9.93 0 -5 0 71.62 4.16 0 -5 0 72.61 6.36 0 5 1 1280.74 61.85 0 5 1 1155.87 54.38 0 5 1 1342.17 58.95 0 5 1 983.80 51.24 0 5 1 1262.08 59.20 0 -5 -1 1339.35 58.56 0 -5 -1 1278.28 58.93 0 -5 -1 1263.69 57.78 0 -5 -1 1417.85 68.00 0 -5 -1 1225.26 65.10 0 5 2 115.39 7.33 0 5 2 112.68 7.03 0 5 2 119.59 8.99 0 5 2 107.75 7.78 0 5 2 120.94 7.10 0 -5 -2 131.09 9.50 0 -5 -2 119.38 8.11 0 -5 -2 119.04 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2.86 -1 9 9 3.17 3.26 1 -9 -8 -0.03 2.40 -1 9 8 -0.27 2.91 1 -9 -7 284.78 18.15 -1 9 7 313.92 20.61 1 -9 -6 6.78 4.00 1 -9 -5 210.84 15.20 -1 9 5 337.22 22.90 1 -9 -4 132.15 10.75 -1 9 4 164.18 14.30 -1 9 3 5.91 2.80 -1 9 2 22.17 4.54 -1 9 2 25.17 6.70 -1 9 1 31.76 6.17 -1 9 1 35.92 8.22 1 -9 0 391.60 21.41 -1 9 0 445.68 26.18 1 -9 1 135.07 10.25 -1 9 -1 154.89 12.93 1 -9 2 14.02 4.38 -1 9 -2 12.81 5.88 1 -9 3 2.27 5.35 -1 9 -3 2.41 4.29 -1 9 -3 -10.63 4.87 1 -9 4 130.67 12.75 -1 9 -4 131.38 12.72 -1 9 -4 134.03 13.36 1 -9 5 53.28 8.89 -1 9 -5 45.74 8.88 -1 9 -5 54.10 9.09 1 -9 6 -0.75 4.16 -1 9 -6 -1.66 3.72 -1 9 -6 -1.21 3.96 -1 9 -7 79.87 15.56 1 -9 8 416.99 27.32 -1 9 -8 411.10 25.88 -1 9 -8 390.86 25.11 1 -9 9 922.24 53.50 -1 9 -9 888.43 49.94 -1 9 -9 872.45 48.67 -1 9 -10 40.72 7.18 -1 9 -10 42.55 6.44 1 -9 11 -0.06 3.06 -1 9 -11 6.10 5.40 -1 9 -11 5.22 2.79 1 -8 -11 17.36 4.56 -1 8 11 16.72 4.65 1 -8 -10 92.15 10.03 -1 8 10 69.63 6.16 -1 8 10 95.45 9.03 1 -8 -9 86.19 10.28 -1 8 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5 11.11 3.69 -9 -6 -5 12.55 3.75 -9 -6 -6 0.34 2.27 -9 -6 -7 207.83 14.01 -9 -6 -8 0.38 2.68 -9 -7 2 21.12 5.02 -9 -7 1 104.80 9.16 -9 -7 0 132.52 10.58 -9 -7 -1 139.78 10.94 -9 -7 -2 1.77 1.40 -9 -7 -3 29.15 3.73 -9 -7 -3 36.15 5.55 9 7 4 17.89 4.95 -9 -7 -4 19.17 3.60 9 7 5 7.50 3.06 -9 -7 -5 -0.19 2.88 9 7 6 8.79 2.94 -9 -7 -6 -0.18 3.32 -9 -7 -7 -0.21 2.30 -9 -7 -8 94.17 8.30 -9 -8 0 9.54 4.15 -9 -8 -1 23.23 5.30 -9 -8 -2 6.00 3.72 9 8 3 129.75 10.59 -9 -8 -3 129.34 7.57 9 8 4 27.31 5.32 -9 -8 -4 25.43 3.92 9 8 5 -0.05 1.78 -9 -8 -5 0.03 1.53 -9 -8 -6 87.08 7.20 -10 -3 -7 20.89 2.65 -10 -3 -8 360.80 16.89 -10 -4 -6 49.96 3.45 -10 -4 -7 159.40 8.58 -10 -4 -8 350.72 16.59 -10 -5 -7 113.45 5.50 ; _shelx_hkl_checksum 76927 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 O1 O -0.20640(14) 1.04927(11) 0.37558(8) 0.0208(3) Uani 1 1 d . . O2 O -0.48329(15) 0.78594(12) 0.04835(9) 0.0289(3) Uani 1 1 d . . O3 O 0.08604(15) 1.27800(11) 0.12989(8) 0.0248(3) Uani 1 1 d . . O4 O 0.55107(14) 0.24119(11) 0.49097(8) 0.0248(3) Uani 1 1 d . . H4 H 0.6188 0.2154 0.4402 0.030 Uiso 1 1 calc R U O5 O 0.07987(16) 0.75088(12) 0.47377(9) 0.0304(3) Uani 1 1 d . . O6 O 0.30309(14) 0.35699(11) 0.63908(8) 0.0204(3) Uani 1 1 d . . O7 O 0.17471(15) 0.81181(12) 0.32046(9) 0.0267(3) Uani 1 1 d . . O8 O 0.53009(14) 0.24231(11) 0.30134(8) 0.0235(3) Uani 1 1 d . . O9 O -0.26948(16) 0.69197(13) 0.10305(11) 0.0369(3) Uani 1 1 d . . O10 O -0.05787(16) 1.24932(11) 0.32169(8) 0.0275(3) Uani 1 1 d . . H10 H -0.0847 1.2215 0.3771 0.033 Uiso 1 1 calc R U C11 C 0.2624(2) 0.37802(15) 0.34695(12) 0.0192(4) Uani 1 1 d . . H11 H 0.2536 0.3827 0.2815 0.023 Uiso 1 1 calc R U C12 C 0.14616(19) 0.43000(15) 0.52133(11) 0.0174(3) Uani 1 1 d . . C13 C 0.13634(19) 0.44033(15) 0.42306(11) 0.0172(3) Uani 1 1 d . . C14 C 0.00405(19) 1.08855(16) 0.07793(11) 0.0186(4) Uani 1 1 d . . C15 C -0.0646(2) 1.16083(16) 0.25220(12) 0.0196(4) Uani 1 1 d . . C16 C -0.1474(2) 0.96967(16) 0.20250(12) 0.0192(4) Uani 1 1 d . . H16 H -0.1993 0.9004 0.2190 0.023 Uiso 1 1 calc R U C17 C -0.07581(19) 0.98640(15) 0.10305(11) 0.0179(4) Uani 1 1 d . . C18 C 0.2892(2) 0.36563(15) 0.54165(12) 0.0183(4) Uani 1 1 d . . C19 C -0.3369(2) 0.78042(17) 0.06383(12) 0.0234(4) Uani 1 1 d . . C20 C -0.14133(19) 1.05545(16) 0.27597(11) 0.0189(4) Uani 1 1 d . . C21 C 0.3996(2) 0.30983(15) 0.36897(12) 0.0199(4) Uani 1 1 d . . C22 C -0.00578(19) 0.52122(15) 0.39300(11) 0.0177(4) Uani 1 1 d . . H22 H -0.0416 0.4658 0.3496 0.021 Uiso 1 1 calc R U C23 C 0.0474(2) 0.63495(16) 0.33110(11) 0.0188(4) Uani 1 1 d . . H23A H 0.1341 0.5991 0.2756 0.023 Uiso 1 1 calc R U H23B H -0.0405 0.6778 0.3042 0.023 Uiso 1 1 calc R U C24 C 0.41541(19) 0.30506(15) 0.46666(12) 0.0189(4) Uani 1 1 d . . C25 C 0.0054(2) 1.17666(16) 0.15401(12) 0.0200(4) Uani 1 1 d . . C26 C -0.09555(19) 0.89242(16) 0.02581(11) 0.0183(4) Uani 1 1 d . . H26 H -0.0539 0.8046 0.0437 0.022 Uiso 1 1 calc R U C27 C 0.4011(2) 0.44138(19) 0.66344(13) 0.0290(4) Uani 1 1 d . . H27A H 0.5089 0.4129 0.6267 0.035 Uiso 1 1 calc R U H27B H 0.3972 0.4391 0.7331 0.035 Uiso 1 1 calc R U H27C H 0.3625 0.5284 0.6468 0.035 Uiso 1 1 calc R U C28 C -0.2750(2) 0.90046(16) 0.02815(12) 0.0212(4) Uani 1 1 d . . H28A H -0.3368 0.9739 0.0710 0.025 Uiso 1 1 calc R U H28B H -0.2909 0.9164 -0.0380 0.025 Uiso 1 1 calc R U C29 C 0.5335(2) 0.25785(18) 0.19920(12) 0.0288(4) Uani 1 1 d . . H29A H 0.5318 0.3473 0.1840 0.035 Uiso 1 1 calc R U H29B H 0.4422 0.2315 0.1846 0.035 Uiso 1 1 calc R U H29C H 0.6287 0.2053 0.1600 0.035 Uiso 1 1 calc R U C30 C 0.1009(2) 0.73566(16) 0.38528(12) 0.0202(4) Uani 1 1 d . . C31 C -0.5612(2) 0.6799(2) 0.08621(16) 0.0371(5) Uani 1 1 d . . H31A H -0.5661 0.6723 0.1565 0.045 Uiso 1 1 calc R U H31B H -0.5026 0.5988 0.0522 0.045 Uiso 1 1 calc R U C32 C 0.2234(2) 0.92006(18) 0.36237(14) 0.0286(4) Uani 1 1 d . . H32A H 0.2856 0.8895 0.4101 0.034 Uiso 1 1 calc R U H32B H 0.1306 0.9827 0.3958 0.034 Uiso 1 1 calc R U C33 C -0.2913(2) 0.94657(17) 0.40515(13) 0.0267(4) Uani 1 1 d . . H33A H -0.3810 0.9561 0.3756 0.032 Uiso 1 1 calc R U H33B H -0.3276 0.9501 0.4760 0.032 Uiso 1 1 calc R U H33C H -0.2221 0.8646 0.3837 0.032 Uiso 1 1 calc R U C34 C -0.0186(3) 1.40011(17) 0.12519(14) 0.0321(4) Uani 1 1 d . . H34A H -0.0679 1.3962 0.0707 0.039 Uiso 1 1 calc R U H34B H 0.0417 1.4683 0.1160 0.039 Uiso 1 1 calc R U H34C H -0.0991 1.4171 0.1858 0.039 Uiso 1 1 calc R U C35 C 0.3211(3) 0.9813(2) 0.27883(16) 0.0405(5) Uani 1 1 d . . H35A H 0.2570 1.0146 0.2336 0.049 Uiso 1 1 calc R U H35B H 0.4103 0.9176 0.2447 0.049 Uiso 1 1 calc R U H35C H 0.3588 1.0510 0.3046 0.049 Uiso 1 1 calc R U C36 C -0.7265(3) 0.7093(2) 0.06854(15) 0.0429(6) Uani 1 1 d . . H36A H -0.7794 0.6385 0.0896 0.052 Uiso 1 1 calc R U H36B H -0.7203 0.7211 -0.0008 0.052 Uiso 1 1 calc R U H36C H -0.7853 0.7872 0.1055 0.052 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 O1 0.0254(7) 0.0209(6) 0.0146(5) 0.0005(4) 0.0001(5) -0.0065(5) O2 0.0238(7) 0.0357(7) 0.0323(7) 0.0072(5) -0.0081(5) -0.0166(6) O3 0.0313(7) 0.0236(6) 0.0219(6) 0.0015(5) -0.0040(5) -0.0142(5) O4 0.0199(6) 0.0293(7) 0.0213(6) 0.0002(5) -0.0028(5) 0.0025(5) O5 0.0416(8) 0.0351(7) 0.0183(6) 0.0006(5) -0.0046(5) -0.0198(6) O6 0.0230(6) 0.0229(6) 0.0168(6) 0.0017(4) -0.0061(5) -0.0068(5) O7 0.0364(8) 0.0276(7) 0.0214(6) 0.0056(5) -0.0083(5) -0.0172(6) O8 0.0203(7) 0.0273(6) 0.0182(6) -0.0013(5) 0.0001(5) 0.0015(5) O9 0.0309(8) 0.0384(8) 0.0476(8) 0.0185(7) -0.0138(7) -0.0165(6) O10 0.0446(8) 0.0255(6) 0.0149(6) -0.0007(5) -0.0047(5) -0.0159(6) C11 0.0222(9) 0.0200(8) 0.0156(8) 0.0009(6) -0.0037(7) -0.0055(7) C12 0.0189(9) 0.0150(8) 0.0184(8) 0.0004(6) -0.0023(7) -0.0059(6) C13 0.0177(9) 0.0166(8) 0.0177(8) 0.0010(6) -0.0024(6) -0.0061(6) C14 0.0179(9) 0.0219(8) 0.0160(8) 0.0010(6) -0.0032(6) -0.0045(7) C15 0.0214(9) 0.0201(8) 0.0174(8) -0.0014(6) -0.0042(7) -0.0049(7) C16 0.0178(9) 0.0190(8) 0.0209(8) 0.0009(6) -0.0032(6) -0.0052(6) C17 0.0172(9) 0.0183(8) 0.0176(8) -0.0016(6) -0.0029(6) -0.0032(7) C18 0.0225(9) 0.0166(8) 0.0175(8) 0.0018(6) -0.0044(7) -0.0084(7) C19 0.0217(9) 0.0308(10) 0.0193(8) -0.0008(7) -0.0033(7) -0.0104(7) C20 0.0165(9) 0.0217(8) 0.0164(8) 0.0009(6) -0.0020(6) -0.0007(7) C21 0.0202(9) 0.0178(8) 0.0194(8) 0.0000(6) 0.0007(7) -0.0043(7) C22 0.0211(9) 0.0180(8) 0.0145(7) -0.0001(6) -0.0035(6) -0.0057(7) C23 0.0183(9) 0.0224(8) 0.0144(7) 0.0015(6) -0.0017(6) -0.0031(7) C24 0.0177(9) 0.0173(8) 0.0213(8) 0.0022(6) -0.0036(7) -0.0033(7) C25 0.0211(9) 0.0204(8) 0.0198(8) 0.0018(6) -0.0046(7) -0.0076(7) C26 0.0184(9) 0.0206(8) 0.0166(8) 0.0003(6) -0.0020(6) -0.0077(7) C27 0.0307(11) 0.0342(10) 0.0264(9) -0.0014(8) -0.0111(8) -0.0117(8) C28 0.0214(9) 0.0225(9) 0.0201(8) -0.0006(6) -0.0034(7) -0.0070(7) C29 0.0325(11) 0.0297(10) 0.0178(9) 0.0005(7) 0.0011(7) 0.0014(8) C30 0.0183(9) 0.0224(8) 0.0186(8) 0.0039(6) -0.0026(6) -0.0032(7) C31 0.0301(11) 0.0414(12) 0.0460(12) 0.0096(9) -0.0085(9) -0.0227(9) C32 0.0358(11) 0.0270(9) 0.0295(9) 0.0045(7) -0.0136(8) -0.0150(8) C33 0.0336(11) 0.0241(9) 0.0203(8) 0.0011(7) 0.0017(7) -0.0105(8) C34 0.0478(13) 0.0238(9) 0.0277(10) 0.0040(7) -0.0097(9) -0.0133(8) C35 0.0499(14) 0.0401(12) 0.0409(12) 0.0111(9) -0.0146(10) -0.0273(10) C36 0.0378(12) 0.0732(16) 0.0288(10) 0.0132(10) -0.0103(9) -0.0354(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 '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 C20 O1 C33 116.94(12) . . C19 O2 C31 115.75(14) . . C25 O3 C34 112.95(13) . . C24 O4 H4 109.5 . . C18 O6 C27 112.75(12) . . C30 O7 C32 116.30(13) . . C21 O8 C29 117.46(13) . . C15 O10 H10 109.5 . . C21 C11 C13 120.16(14) . . C21 C11 H11 119.9 . . C13 C11 H11 119.9 . . C13 C12 C18 118.45(15) . . C13 C12 C22 122.56(14) . 2_566 C18 C12 C22 118.90(14) . 2_566 C12 C13 C11 120.33(15) . . C12 C13 C22 122.33(14) . . C11 C13 C22 117.31(14) . . C17 C14 C25 118.33(14) . . C17 C14 C26 123.70(14) . 2_575 C25 C14 C26 117.92(15) . 2_575 O10 C15 C25 118.59(15) . . O10 C15 C20 122.64(14) . . C25 C15 C20 118.77(15) . . C20 C16 C17 120.39(15) . . C20 C16 H16 119.8 . . C17 C16 H16 119.8 . . C14 C17 C16 120.20(14) . . C14 C17 C26 122.47(14) . . C16 C17 C26 117.29(14) . . O6 C18 C24 119.04(14) . . O6 C18 C12 119.46(14) . . C24 C18 C12 121.43(14) . . O9 C19 O2 123.48(16) . . O9 C19 C28 126.14(16) . . O2 C19 C28 110.36(14) . . O1 C20 C16 125.81(15) . . O1 C20 C15 113.76(14) . . C16 C20 C15 120.44(15) . . O8 C21 C11 125.70(14) . . O8 C21 C24 114.03(14) . . C11 C21 C24 120.27(15) . . C12 C22 C13 114.31(13) 2_566 . C12 C22 C23 111.09(13) 2_566 . C13 C22 C23 109.36(13) . . C12 C22 H22 107.2 2_566 . C13 C22 H22 107.2 . . C23 C22 H22 107.2 . . C30 C23 C22 116.06(13) . . C30 C23 H23A 108.3 . . C22 C23 H23A 108.3 . . C30 C23 H23B 108.3 . . C22 C23 H23B 108.3 . . H23A C23 H23B 107.4 . . O4 C24 C18 118.96(14) . . O4 C24 C21 121.90(14) . . C18 C24 C21 119.14(15) . . C15 C25 O3 119.33(14) . . C15 C25 C14 121.82(15) . . O3 C25 C14 118.77(14) . . C14 C26 C17 113.45(14) 2_575 . C14 C26 C28 110.33(13) 2_575 . C17 C26 C28 110.62(13) . . C14 C26 H26 107.4 2_575 . C17 C26 H26 107.4 . . C28 C26 H26 107.4 . . O6 C27 H27A 109.5 . . O6 C27 H27B 109.5 . . H27A C27 H27B 109.5 . . O6 C27 H27C 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . C19 C28 C26 113.98(14) . . C19 C28 H28A 108.8 . . C26 C28 H28A 108.8 . . C19 C28 H28B 108.8 . . C26 C28 H28B 108.8 . . H28A C28 H28B 107.7 . . O8 C29 H29A 109.5 . . O8 C29 H29B 109.5 . . H29A C29 H29B 109.5 . . O8 C29 H29C 109.5 . . H29A C29 H29C 109.5 . . H29B C29 H29C 109.5 . . O5 C30 O7 123.05(16) . . O5 C30 C23 126.95(15) . . O7 C30 C23 109.98(13) . . O2 C31 C36 107.42(17) . . O2 C31 H31A 110.2 . . C36 C31 H31A 110.2 . . O2 C31 H31B 110.2 . . C36 C31 H31B 110.2 . . H31A C31 H31B 108.5 . . O7 C32 C35 107.55(15) . . O7 C32 H32A 110.2 . . C35 C32 H32A 110.2 . . O7 C32 H32B 110.2 . . C35 C32 H32B 110.2 . . H32A C32 H32B 108.5 . . O1 C33 H33A 109.5 . . O1 C33 H33B 109.5 . . H33A C33 H33B 109.5 . . O1 C33 H33C 109.5 . . H33A C33 H33C 109.5 . . H33B C33 H33C 109.5 . . O3 C34 H34A 109.5 . . O3 C34 H34B 109.5 . . H34A C34 H34B 109.5 . . O3 C34 H34C 109.5 . . H34A C34 H34C 109.5 . . H34B C34 H34C 109.5 . . C32 C35 H35A 109.5 . . C32 C35 H35B 109.5 . . H35A C35 H35B 109.5 . . C32 C35 H35C 109.5 . . H35A C35 H35C 109.5 . . H35B C35 H35C 109.5 . . C31 C36 H36A 109.5 . . C31 C36 H36B 109.5 . . H36A C36 H36B 109.5 . . C31 C36 H36C 109.5 . . H36A C36 H36C 109.5 . . H36B C36 H36C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 C20 1.3761(19) . O1 C33 1.431(2) . O2 C19 1.345(2) . O2 C31 1.450(2) . O3 C25 1.3856(19) . O3 C34 1.442(2) . O4 C24 1.3677(19) . O4 H4 0.8200 . O5 C30 1.206(2) . O6 C18 1.3872(19) . O6 C27 1.438(2) . O7 C30 1.339(2) . O7 C32 1.456(2) . O8 C21 1.3803(19) . O8 C29 1.421(2) . O9 C19 1.203(2) . O10 C15 1.3613(19) . O10 H10 0.8200 . C11 C21 1.381(2) . C11 C13 1.403(2) . C11 H11 0.9300 . C12 C13 1.389(2) . C12 C18 1.401(2) . C12 C22 1.514(2) 2_566 C13 C22 1.515(2) . C14 C17 1.391(2) . C14 C25 1.411(2) . C14 C26 1.512(2) 2_575 C15 C25 1.384(2) . C15 C20 1.402(2) . C16 C20 1.381(2) . C16 C17 1.405(2) . C16 H16 0.9300 . C17 C26 1.521(2) . C18 C24 1.389(2) . C19 C28 1.503(2) . C21 C24 1.395(2) . C22 C12 1.514(2) 2_566 C22 C23 1.550(2) . C22 H22 0.9800 . C23 C30 1.504(2) . C23 H23A 0.9700 . C23 H23B 0.9700 . C26 C14 1.512(2) 2_575 C26 C28 1.558(2) . C26 H26 0.9800 . C27 H27A 0.9600 . C27 H27B 0.9600 . C27 H27C 0.9600 . C28 H28A 0.9700 . C28 H28B 0.9700 . C29 H29A 0.9600 . C29 H29B 0.9600 . C29 H29C 0.9600 . C31 C36 1.505(3) . C31 H31A 0.9700 . C31 H31B 0.9700 . C32 C35 1.497(3) . C32 H32A 0.9700 . C32 H32B 0.9700 . C33 H33A 0.9600 . C33 H33B 0.9600 . C33 H33C 0.9600 . C34 H34A 0.9600 . C34 H34B 0.9600 . C34 H34C 0.9600 . C35 H35A 0.9600 . C35 H35B 0.9600 . C35 H35C 0.9600 . C36 H36A 0.9600 . C36 H36B 0.9600 . C36 H36C 0.9600 . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 C18 C12 C13 C11 5.3(2) . . C22 C12 C13 C11 -171.15(15) 2_566 . C18 C12 C13 C22 -172.73(14) . . C22 C12 C13 C22 10.8(3) 2_566 . C21 C11 C13 C12 -2.3(2) . . C21 C11 C13 C22 175.79(15) . . C25 C14 C17 C16 -2.4(2) . . C26 C14 C17 C16 174.91(15) 2_575 . C25 C14 C17 C26 175.08(15) . . C26 C14 C17 C26 -7.6(3) 2_575 . C20 C16 C17 C14 1.0(2) . . C20 C16 C17 C26 -176.65(15) . . C27 O6 C18 C24 76.60(18) . . C27 O6 C18 C12 -106.24(17) . . C13 C12 C18 O6 178.38(13) . . C22 C12 C18 O6 -5.0(2) 2_566 . C13 C12 C18 C24 -4.5(2) . . C22 C12 C18 C24 172.06(14) 2_566 . C31 O2 C19 O9 2.7(2) . . C31 O2 C19 C28 -175.68(14) . . C33 O1 C20 C16 -1.7(2) . . C33 O1 C20 C15 178.03(14) . . C17 C16 C20 O1 -179.89(14) . . C17 C16 C20 C15 0.4(2) . . O10 C15 C20 O1 -0.9(2) . . C25 C15 C20 O1 179.95(14) . . O10 C15 C20 C16 178.77(15) . . C25 C15 C20 C16 -0.3(2) . . C29 O8 C21 C11 8.9(2) . . C29 O8 C21 C24 -170.99(15) . . C13 C11 C21 O8 178.51(15) . . C13 C11 C21 C24 -1.6(2) . . C12 C13 C22 C12 -10.0(2) . 2_566 C11 C13 C22 C12 171.92(14) . 2_566 C12 C13 C22 C23 115.27(16) . . C11 C13 C22 C23 -62.82(18) . . C12 C22 C23 C30 60.60(18) 2_566 . C13 C22 C23 C30 -66.51(17) . . O6 C18 C24 O4 -1.5(2) . . C12 C18 C24 O4 -178.58(14) . . O6 C18 C24 C21 177.81(14) . . C12 C18 C24 C21 0.7(2) . . O8 C21 C24 O4 1.6(2) . . C11 C21 C24 O4 -178.34(15) . . O8 C21 C24 C18 -177.70(14) . . C11 C21 C24 C18 2.4(2) . . O10 C15 C25 O3 2.9(2) . . C20 C15 C25 O3 -177.96(14) . . O10 C15 C25 C14 179.66(15) . . C20 C15 C25 C14 -1.2(3) . . C34 O3 C25 C15 -80.86(19) . . C34 O3 C25 C14 102.27(17) . . C17 C14 C25 C15 2.6(2) . . C26 C14 C25 C15 -174.93(15) 2_575 . C17 C14 C25 O3 179.36(14) . . C26 C14 C25 O3 1.9(2) 2_575 . C14 C17 C26 C14 6.9(2) . 2_575 C16 C17 C26 C14 -175.55(14) . 2_575 C14 C17 C26 C28 -117.74(16) . . C16 C17 C26 C28 59.84(18) . . O9 C19 C28 C26 11.9(2) . . O2 C19 C28 C26 -169.80(13) . . C14 C26 C28 C19 121.36(15) 2_575 . C17 C26 C28 C19 -112.27(15) . . C32 O7 C30 O5 -2.8(2) . . C32 O7 C30 C23 175.78(14) . . C22 C23 C30 O5 -14.7(2) . . C22 C23 C30 O7 166.82(13) . . C19 O2 C31 C36 175.72(15) . . C30 O7 C32 C35 172.74(16) . .