#------------------------------------------------------------------------------ #$Date: 2021-07-21 08:22:48 +0300 (Wed, 21 Jul 2021) $ #$Revision: 267666 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243872.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_2243872 loop_ _publ_author_name 'Okmanov, R. Ya.' 'Makhmudova, M. M.' 'Bobaev, I. D.' 'Tashkhodjaev, B.' _publ_section_title ; Withanolides from Physalis angulata L. ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 804 _journal_page_last 808 _journal_paper_doi 10.1107/S205698902100709X _journal_volume 77 _journal_year 2021 _chemical_absolute_configuration rm _chemical_formula_iupac 'C28 H40 O7' _chemical_formula_moiety 'C28 H40 O7' _chemical_formula_sum 'C28 H40 O7' _chemical_formula_weight 488.60 _chemical_melting_point 528(3) _chemical_name_common ; 14a-hydroxyixocarpanolide ; _chemical_name_systematic (20R,22R)-5\a,14\a,20-Trihydroxy-1-oxo-6\a,7\a-epoxywitha-2-enolide _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_Hall 'P 1' _space_group_name_H-M_alt 'P 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method SHELXL-2014/8 _cell_angle_alpha 112.81(3) _cell_angle_beta 96.49(3) _cell_angle_gamma 93.13(3) _cell_formula_units_Z 1 _cell_length_a 6.2374(12) _cell_length_b 9.5938(19) _cell_length_c 11.351(2) _cell_measurement_reflns_used 1941 _cell_measurement_temperature 290(2) _cell_measurement_theta_max 75.4630 _cell_measurement_theta_min 4.2650 _cell_volume 618.5(3) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2018) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2018) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2018) ; _computing_molecular_graphics ; XP (Sheldrick, 1998) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008), PLATON (Spek, 2020) and publCIF (Westrip, 2010)' ; _computing_structure_refinement ; SHELXL2014/8 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS7 (Sheldrick, 2008) ; _diffrn_ambient_temperature 290.0(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.2576 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_unetI/netI 0.0320 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4169 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.647 _diffrn_reflns_theta_min 4.271 _diffrn_source 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.755 _exptl_absorpt_correction_T_max 0.85279 _exptl_absorpt_correction_T_min 0.77644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Sheldrick, 2003) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.312 _exptl_crystal_description prizmatic _exptl_crystal_F_000 264 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _refine_diff_density_max 0.170 _refine_diff_density_min -0.193 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack -0.1(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 333 _refine_ls_number_reflns 2812 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0405 _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^)+(0.0647P)^2^+0.0383P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1035 _refine_ls_wR_factor_ref 0.1097 _reflns_number_gt 2545 _reflns_number_total 2812 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file dj2029sup1.cif _cod_data_source_block II _cod_original_cell_volume 618.5(2) _cod_database_code 2243872 _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_hkl_file ; 0 0 -1 9623.30 206.061 21 0 0 -1 9729.92 212.639 19 0 0 -2 33195.7 586.480 21 0 0 -2 33764.4 597.291 19 0 0 -3 156500. 2102.48 21 0 0 -3 158048. 2100.39 19 0 0 -4 284224. 3626.16 19 0 0 -5 83518.4 1531.63 19 0 0 -6 36466.9 1007.13 19 0 0 -7 23788.1 875.581 19 0 0 -8 2168.56 336.270 8 0 0 -8 2205.62 282.637 19 0 0 -9 742.476 238.827 8 0 0 -10 316.298 184.325 8 0 0 -11 1121.99 253.962 7 0 0 -11 977.014 252.524 8 0 0 -12 42.0739 102.086 7 0 0 -12 587.609 180.822 8 0 1 -13 4119.15 341.813 7 0 1 -12 2315.06 331.147 7 0 1 -11 6237.30 560.287 8 0 1 -11 5859.09 583.811 7 0 1 -10 12654.1 830.191 8 0 1 -9 22915.1 931.053 19 0 1 -9 21841.4 1088.28 8 0 1 -8 707.839 167.430 19 0 1 -8 887.098 249.210 8 0 1 -7 10676.2 549.086 19 0 1 -6 121478. 2061.61 19 0 1 -5 33006.2 826.287 19 0 1 -4 146453. 2058.62 19 0 1 -4 145754. 1987.63 21 0 1 -3 125003. 1699.27 19 0 1 -3 125508. 1632.86 21 0 1 -2 109905. 1406.43 19 0 -1 1 188613. 2184.41 1 0 -1 0 366570. 4080.18 1 0 -1 -1 557649. 6153.76 19 0 -1 -1 543199. 6123.38 1 0 -1 -2 89720.1 1364.60 19 0 -1 -3 83283.5 1403.53 19 0 -1 -4 180151. 2650.28 19 0 -1 -5 21893.5 751.348 19 0 -1 -6 8188.92 495.393 19 0 -1 -7 6512.52 477.920 19 0 -1 -8 7524.96 651.884 13 0 -1 -8 7886.76 560.216 19 0 -1 -8 6153.52 576.260 8 0 -1 -9 8087.36 663.509 8 0 -1 -10 2206.79 353.408 7 0 -1 -10 2601.60 375.094 8 0 -1 -11 1789.91 292.553 7 0 -1 -11 1734.94 285.550 8 0 -1 -12 2038.33 217.093 7 0 -1 -12 2522.58 269.566 8 0 2 -13 1870.96 277.396 7 0 2 -12 3471.29 433.634 7 0 2 -11 2708.76 388.553 8 0 2 -11 3084.76 435.579 7 0 2 -10 10498.5 760.975 8 0 2 -9 22270.8 1095.57 8 0 2 -8 1021.23 189.875 19 0 2 -7 26916.3 856.154 19 0 2 -6 31719.5 858.560 19 0 2 -5 177938. 2510.68 19 0 2 -5 176586. 2364.07 21 0 2 -4 33351.6 727.620 19 0 2 -4 33714.9 633.506 21 0 2 -3 54471.4 916.282 19 0 -2 2 19428.5 459.724 1 0 -2 1 125703. 1653.89 1 0 -2 0 55423.8 922.562 1 0 -2 -1 186306. 2441.26 1 0 -2 -2 217951. 2937.35 19 0 -2 -3 6677.23 376.610 19 0 -2 -4 39723.4 1062.24 19 0 -2 -5 18558.0 758.032 19 0 -2 -6 3732.69 375.151 19 0 -2 -7 13449.8 739.218 19 0 -2 -7 13440.9 860.620 13 0 -2 -8 9543.60 745.479 13 0 -2 -9 1772.22 328.752 8 0 -2 -10 1639.81 297.398 8 0 -2 -10 1940.97 288.171 7 0 -2 -11 2222.62 283.177 8 0 3 -14 576.494 126.834 7 0 3 -13 108.900 141.326 7 0 3 -12 1765.41 338.182 7 0 3 -11 8253.48 710.161 7 0 3 -10 3765.02 460.263 8 0 3 -9 1907.63 326.585 8 0 3 -8 11692.4 604.537 19 0 3 -7 2367.92 255.068 19 0 3 -6 42777.7 1034.59 19 0 3 -5 55073.4 1130.18 19 0 3 -5 57625.6 927.212 21 0 -3 4 203950. 2805.33 1 0 -3 3 12539.9 438.313 1 0 -3 2 34091.3 740.228 1 0 -3 1 18446.4 539.746 1 0 -3 0 84589.8 1413.95 1 0 -3 -1 7689.96 363.052 1 0 -3 -2 34214.5 913.855 19 0 -3 -2 33628.7 894.313 1 0 -3 -3 18044.1 705.752 19 0 -3 -4 20746.7 822.985 19 0 -3 -5 8255.93 549.997 19 0 -3 -6 5056.12 465.047 19 0 -3 -6 5547.07 553.613 13 0 -3 -7 8264.37 695.591 13 0 -3 -8 6714.70 627.929 13 0 -3 -9 693.182 228.324 8 0 -3 -10 1532.94 261.768 8 0 -3 -11 2293.71 226.757 8 0 4 -14 1302.89 169.584 7 0 4 -13 574.198 173.763 7 0 4 -12 5419.99 541.323 7 0 4 -11 6891.06 634.943 7 0 4 -10 936.362 261.631 7 0 4 -10 748.350 227.758 12 0 4 -9 41173.2 1509.26 12 0 -4 9 37763.8 1259.09 1 0 -4 8 8866.02 558.295 1 0 -4 7 2774.10 306.644 1 0 -4 6 12027.6 575.528 1 0 -4 5 69021.5 1425.41 1 0 -4 4 267158. 3585.07 1 0 -4 3 20601.2 643.464 1 0 -4 2 12250.2 500.529 1 0 -4 1 20324.2 656.980 1 0 -4 0 3667.89 281.311 1 0 -4 -1 26814.9 827.515 19 0 -4 -1 27354.8 832.794 1 0 -4 -2 20036.4 762.389 19 0 -4 -3 1822.96 252.861 19 0 -4 -4 42340.1 1321.46 19 0 -4 -5 12735.1 766.329 11 0 -4 -5 11402.4 693.962 19 0 -4 -5 11027.5 780.598 14 0 -4 -6 8876.41 726.281 13 0 -4 -7 73.6065 165.558 13 0 -4 -8 3568.47 445.821 13 0 -4 -9 1072.81 235.808 8 0 -4 -10 178.066 113.469 8 0 5 -13 308.883 148.438 7 0 5 -12 424.613 199.371 7 0 5 -11 5906.28 548.503 12 0 5 -11 6007.69 582.695 7 0 5 -10 16956.4 985.936 12 0 5 -10 17459.1 993.373 7 0 5 -9 22001.9 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0 -9 -1 596.979 210.483 14 0 -9 -2 10609.5 628.177 11 0 -9 -3 204.367 108.508 11 0 -9 -3 118.350 118.482 13 0 -9 -4 141.670 95.5919 13 0 10 -11 984.708 189.676 9 0 10 -11 1259.08 196.043 17 0 10 -10 2121.04 277.317 17 0 10 -10 2232.49 294.557 9 0 10 -9 2670.80 345.132 9 0 10 -9 3006.88 338.008 17 0 10 -8 1829.04 319.685 9 0 10 -7 3622.13 441.273 9 0 10 -6 1343.56 315.259 9 0 -10 5 4346.86 480.420 11 0 -10 4 10021.1 710.185 11 0 -10 3 4520.59 470.599 11 0 -10 2 1890.12 321.740 11 0 -10 1 514.678 190.394 11 0 -10 1 987.047 208.226 14 0 -10 0 2800.63 325.384 11 0 -10 0 3133.96 333.398 14 0 -10 -1 5997.46 433.956 13 0 -10 -1 7315.43 450.459 11 0 -10 -2 1858.04 212.099 13 0 -11 9 8286.31 458.044 11 0 -11 8 1552.02 234.188 11 0 -11 7 31.1667 122.820 11 0 -11 6 2638.01 323.129 11 0 -11 5 1300.93 247.292 11 0 -11 4 1513.27 248.493 11 0 -11 3 778.612 192.280 11 0 -11 2 58.2844 108.846 11 0 -11 1 76.0479 101.247 11 0 -11 1-254.811 102.299 13 0 -12 6 312.743 101.199 11 0 -12 5 2527.80 216.585 11 1 -12 6 180.121 81.1523 11 1 -11 1 3504.03 273.475 14 1 -11 1 3604.33 269.005 11 1 -11 2 747.385 160.815 11 1 -11 2 604.481 141.488 14 1 -11 3 1456.70 216.074 14 1 -11 3 1421.78 224.866 11 1 -11 4 1061.71 222.667 11 1 -11 5 1640.41 252.433 11 1 -11 6 2730.15 322.635 11 1 -11 7-37.2988 106.551 11 1 -11 8 98.0500 118.613 11 1 -11 9 7773.09 438.691 11 1 -11 10 13.9768 72.1443 11 1 -10 -2 4086.59 341.461 13 1 -10 -1 5742.51 441.131 14 1 -10 0 3180.53 363.345 14 1 -10 0 3185.87 331.166 11 1 -10 1-3.61604 132.419 11 1 -10 1-67.0091 136.136 14 1 -10 2 1995.76 310.445 11 1 -10 2 1913.91 311.336 14 1 -10 3 1121.36 244.608 11 1 -10 4 500.665 198.417 11 -1 10 -5 1878.30 317.955 9 -1 10 -6 1344.93 290.455 9 -1 10 -7 2033.25 348.426 9 -1 10 -8 851.734 245.807 9 -1 10 -9 174.693 186.771 9 -1 10 -10 2305.52 295.778 9 -1 10 -10 1775.90 243.370 17 -1 10 -11 5168.21 361.880 9 -1 10 -11 4077.97 305.856 17 1 -9 -4 571.680 145.083 13 1 -9 -3 4433.23 412.463 13 1 -9 -2 1458.38 281.092 14 1 -9 -1 9927.82 638.217 11 1 -9 -1 8906.69 670.189 14 1 -9 0 4721.38 481.066 11 1 -9 0 5093.39 531.635 14 1 -9 1 11956.4 788.388 11 1 -9 2 3111.03 416.374 15 1 -9 2 2412.88 372.731 11 1 -9 3 21675.9 1042.07 15 -1 9 -4 17224.9 955.853 9 1 -9 4 17007.9 901.262 15 -1 9 -5 2535.69 413.328 9 -1 9 -6 4392.39 504.612 9 -1 9 -6 5364.63 531.669 12 -1 9 -7-22.7634 168.128 9 -1 9 -7-129.699 156.628 12 -1 9 -8 2799.05 387.995 12 -1 9 -8 2720.35 405.702 9 -1 9 -9 130.432 198.015 9 -1 9 -9 51.9727 146.304 12 -1 9 -10 4452.01 453.476 9 -1 9 -10 3920.85 421.834 12 -1 9 -11 408.304 160.654 12 -1 9 -11 611.048 195.960 9 -1 9 -12 3137.33 293.684 17 -1 9 -12 3461.13 290.190 9 1 -8 -6-2.36527 73.2750 13 1 -8 -5 2372.80 301.583 13 1 -8 -4 1557.47 294.834 14 1 -8 -4 1572.24 300.274 13 1 -8 -3 10806.4 749.075 14 1 -8 -2 3356.12 402.262 11 1 -8 -2 2738.62 406.539 14 1 -8 -1 4043.13 458.891 11 1 -8 -1 4051.89 493.372 14 1 -8 0 8824.98 681.038 11 1 -8 0 7224.02 628.427 15 1 -8 1 11607.4 811.132 11 1 -8 1 11240.6 781.456 15 1 -8 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100.626 111.254 18 5 3 -9 148.925 174.839 7 5 3 -9 165.326 180.620 5 5 3 -8 1985.49 328.935 18 5 3 -8 2431.92 415.123 7 5 3 -8 2482.28 384.459 5 5 3 -7 7598.42 652.790 18 5 3 -7 8032.74 732.837 7 5 3 -7 7667.73 650.986 5 5 3 -6 13135.1 865.677 18 5 3 -6 12998.2 938.908 7 5 3 -6 15263.1 844.142 3 5 3 -6 14038.4 857.180 5 5 3 -5 4820.48 584.143 18 5 3 -5 4658.18 567.751 7 5 3 -5 5187.53 528.776 3 5 3 -4 8858.72 728.012 18 5 3 -4 8716.92 765.802 7 5 3 -4 9240.23 710.467 3 5 3 -3 6392.26 617.350 18 5 3 -3 5930.91 576.508 3 5 3 -2 2195.65 364.189 3 5 3 -2 2655.03 401.457 18 5 3 -2 2743.27 372.995 2 5 3 -1 12598.8 818.477 18 5 3 -1 13411.9 849.838 2 5 3 -1 10982.2 808.668 3 5 3 0 39233.2 1492.74 2 5 3 0 38160.0 1501.59 3 5 3 1 3347.65 467.251 2 5 3 1 3729.74 459.598 3 5 3 2 4065.39 481.803 10 -5 -3 -2 3406.46 505.761 4 5 3 2 4388.13 462.096 3 5 3 3 1452.59 300.922 10 -5 -3 -3 1423.87 285.571 4 5 3 4 540.889 213.280 10 -5 -3 -4 1030.04 249.705 4 5 3 5 1240.65 243.435 10 -5 -3 -5 1210.52 231.541 4 -5 -3 -5 1120.11 221.452 12 -5 -3 -6 1220.73 192.803 4 5 4 -11 818.883 212.046 7 5 4 -10 1367.74 221.585 18 5 4 -10 1355.62 283.252 7 5 4 -9 2178.32 379.121 7 5 4 -9 1697.80 275.937 18 5 4 -8 179.464 161.743 18 5 4 -8 71.7299 182.310 7 5 4 -7 5792.65 565.761 18 5 4 -7 5899.20 630.866 7 5 4 -7 7304.35 571.868 3 5 4 -6 6980.07 644.500 18 5 4 -6 6932.05 697.735 7 5 4 -6 7286.13 595.342 3 5 4 -5 2710.67 408.635 18 5 4 -5 2695.53 448.138 7 5 4 -5 2512.09 382.804 3 5 4 -4 5615.48 586.134 18 5 4 -4 5588.13 562.923 3 5 4 -3 5003.73 554.857 18 5 4 -3 5302.96 562.268 3 5 4 -2 7679.54 638.296 18 5 4 -2 8574.10 682.131 2 5 4 -1 428.337 222.777 2 5 4 0 6353.70 602.049 2 5 4 0 6985.96 631.824 3 5 4 1 836.808 272.327 3 5 4 1 993.243 259.021 2 5 4 2 3047.55 410.145 10 -5 -4 -2 3324.47 414.947 4 5 4 2 3192.14 389.248 3 5 4 3 1096.98 249.288 10 -5 -4 -3 920.302 245.150 4 5 4 4 185.147 155.316 10 -5 -4 -4 264.663 150.276 4 -5 -4 -4 44.8981 96.1010 12 5 4 5 2094.12 228.666 10 -5 -4 -5 1853.51 225.560 4 5 5 -11 422.284 159.981 7 5 5 -10 92.8964 103.100 18 5 5 -10 266.137 171.745 7 5 5 -9 2510.48 330.968 18 5 5 -9 2710.77 396.089 7 5 5 -8 2277.93 335.922 18 5 5 -8 2437.65 401.893 7 5 5 -7 371.997 163.874 3 5 5 -7 264.876 164.905 18 5 5 -7 667.839 248.279 7 5 5 -6 510.587 178.891 3 5 5 -6 359.586 203.609 18 5 5 -6 163.247 194.470 7 5 5 -5 458.198 184.136 3 5 5 -5 442.424 205.714 18 5 5 -4 1070.36 285.486 3 5 5 -4 1081.12 281.496 18 5 5 -3 330.319 177.274 18 5 5 -3 803.852 258.062 2 5 5 -2 635.156 260.034 2 5 5 -1 3070.19 413.676 2 5 5 0 1763.09 329.402 2 5 5 1 4204.55 454.186 2 5 5 1 4369.12 447.548 3 5 5 2 293.506 178.121 10 5 5 2 403.441 147.269 3 -5 -5 -2 472.899 178.097 4 5 5 3 159.881 124.713 10 -5 -5 -3 223.970 128.046 4 5 5 4 1283.92 190.290 10 -5 -5 -4 863.696 166.070 4 5 6 -10 914.862 221.241 7 5 6 -10 638.045 158.231 18 5 6 -9 571.774 217.596 7 5 6 -9 135.067 116.588 18 5 6 -8 1354.66 264.822 18 5 6 -7 1869.56 279.972 3 5 6 -7 2366.16 357.106 18 5 6 -6 1741.84 289.400 3 5 6 -6 2601.01 376.710 18 5 6 -5 186.147 154.698 3 5 6 -5 598.832 215.236 18 5 6 -4 3078.20 395.949 18 5 6 -4 2299.78 362.261 3 5 6 -3 91.1685 120.943 18 5 6 -3 104.654 151.951 2 5 6 -2 1080.22 257.121 2 5 6 -1 2273.02 342.897 2 5 6 0 823.405 227.551 3 5 6 0 843.065 235.520 2 5 6 1 2089.20 287.033 10 5 6 1 1746.97 244.255 3 5 6 1 1771.07 268.105 2 5 6 2 504.999 162.972 10 -5 -6 -2 584.972 155.661 4 5 6 3 2305.67 215.009 10 5 7 -10 2059.88 222.169 18 5 7 -9 1319.91 217.967 18 5 7 -8 170.465 124.385 18 5 7 -7-19.9145 109.118 3 5 7 -7-183.725 137.420 18 5 7 -6 493.700 166.725 3 5 7 -6 559.787 180.830 18 5 7 -5 2879.77 339.748 18 5 7 -5 1843.92 294.921 3 5 7 -4 907.335 224.438 3 5 7 -4 809.912 190.964 18 5 7 -4 1147.60 247.319 2 5 7 -3 1098.42 245.636 2 5 7 -2 2482.56 319.671 2 5 7 -2 2679.95 336.315 3 5 7 -1 3033.19 334.182 2 5 7 -1 2338.89 298.100 3 5 7 0 3282.83 307.315 10 5 7 0 3031.34 306.151 2 5 7 0 2756.87 277.557 3 5 7 1 4844.05 323.303 10 5 8 -9 4446.03 297.284 18 5 8 -8 2029.82 230.776 18 5 8 -7 508.923 153.508 18 5 8 -6 476.050 151.133 3 5 8 -6 408.486 129.231 18 5 8 -5 977.239 191.767 3 5 8 -4 566.524 157.582 3 5 8 -4 435.275 155.806 2 5 8 -3 436.573 155.408 3 5 8 -3 354.416 119.040 2 5 8 -2 304.152 122.924 3 5 8 -2 236.613 126.667 2 5 8 -1 406.109 100.237 3 6 -8 2 654.398 125.953 15 6 -8 3 885.285 140.253 15 6 -8 4 312.412 100.319 15 6 -7 -2 996.418 158.264 6 6 -7 -1 2150.96 246.103 6 6 -7 0 908.636 155.907 15 6 -7 1 603.703 157.219 15 6 -7 2 711.962 164.239 15 6 -7 3 422.505 171.316 16 6 -7 3 378.461 143.633 15 6 -7 4 2613.57 293.640 16 6 -7 4 2463.96 274.479 15 6 -7 5 357.512 136.056 16 6 -7 6 280.306 105.753 16 6 -6 -4 137.136 93.5997 6 6 -6 -3 208.613 110.785 6 6 -6 -2 2948.25 356.641 3 6 -6 -2 2129.30 278.342 6 6 -6 -1 155.337 151.833 3 6 -6 0 2008.20 313.779 3 6 -6 0 2413.04 283.724 15 6 -6 1 356.771 181.569 16 6 -6 1 438.070 178.082 15 6 -6 1 595.914 189.713 3 6 -6 2 116.391 146.364 16 6 -6 2-61.2447 124.532 15 6 -6 2 326.476 179.371 3 6 -6 3 2433.92 309.259 3 6 -6 3 2370.31 321.430 16 6 -6 4 404.762 161.435 16 6 -6 5 1459.00 235.740 16 6 -6 6 161.876 132.251 16 -6 6 -6-1.40697 80.2167 12 6 -6 7 400.604 124.044 16 6 -5 -5 82.5667 92.2544 6 6 -5 -4 1079.56 229.591 3 6 -5 -4 830.661 178.932 6 6 -5 -3 1234.29 254.651 3 6 -5 -3 1174.27 222.641 6 6 -5 -2 85.9606 126.876 3 6 -5 -2 193.318 131.559 6 6 -5 -1 3545.28 434.520 3 6 -5 0 651.640 184.048 16 6 -5 0 382.305 171.495 15 6 -5 0 417.827 196.327 3 6 -5 1 579.534 205.264 16 6 -5 1 1097.16 263.521 3 6 -5 2 1776.82 304.173 16 6 -5 2 1623.17 298.671 3 6 -5 3 2052.93 324.317 16 6 -5 3 2346.06 323.920 3 6 -5 4 2577.28 331.046 16 -6 5 -4 2575.95 302.994 12 6 -5 5 3834.15 379.242 16 -6 5 -5 3447.61 343.792 12 6 -5 6 2571.23 289.482 16 -6 5 -6 2193.11 261.850 12 6 -5 7 864.604 171.079 16 -6 5 -7 602.126 146.470 12 6 -4 -6 349.783 130.741 6 6 -4 -5 1284.23 240.829 3 6 -4 -5 1197.17 214.618 6 6 -4 -4 166.630 118.003 6 6 -4 -4 125.671 152.786 3 6 -4 -3 188.734 141.793 6 6 -4 -3 16.8791 135.572 3 6 -4 -2 582.740 191.038 6 6 -4 -2 403.433 198.498 3 6 -4 -1 2004.23 359.443 3 6 -4 0 7132.67 570.634 16 6 -4 0 5438.39 547.757 3 6 -4 1 5389.60 506.604 16 6 -4 1 4342.43 478.248 3 6 -4 2 52.5823 158.284 3 -6 4 -3-9.05928 152.228 12 6 -4 3 318.929 184.903 3 -6 4 -4 2162.73 319.900 12 -6 4 -5 4117.05 414.042 12 -6 4 -6 1393.52 240.216 12 -6 4 -7 1041.87 196.261 12 6 -3 -7 1287.09 214.037 6 6 -3 -6 72.2299 93.3797 6 6 -3 -6 440.749 161.693 3 6 -3 -5 163.140 120.609 6 6 -3 -5-240.521 151.665 3 6 -3 -4 33.8012 131.312 6 6 -3 -4 458.301 198.727 3 6 -3 -3 623.708 224.904 3 6 -3 -2 4365.61 501.283 3 6 -3 -1 827.044 254.207 3 6 -3 0 1622.55 290.260 16 6 -3 0 1441.27 302.362 3 6 -3 1 4614.31 484.238 3 6 -3 2 4384.39 469.515 3 -6 3 -2 4029.51 443.871 12 -6 3 -3 3007.22 395.543 12 -6 3 -4 6425.99 548.467 12 -6 3 -5 3136.47 372.914 12 -6 3 -6 2467.03 319.755 12 -6 3 -7 693.144 188.460 12 6 -2 -8 82.0774 99.0800 6 6 -2 -7 2209.54 293.283 6 6 -2 -6 1682.58 272.991 6 6 -2 -6 1640.29 273.740 3 6 -2 -5 46.1901 110.409 6 6 -2 -5-34.6783 158.173 3 6 -2 -4 1888.55 325.196 3 6 -2 -3 2735.30 401.905 3 6 -2 -2 3689.44 469.320 3 6 -2 -1 487.687 195.966 3 6 -2 0 29227.5 1252.20 3 6 -2 1 9779.17 698.078 3 -6 2 -1 9813.27 688.724 12 6 -2 2 8291.24 626.969 3 -6 2 -2 7273.91 603.480 12 -6 2 -3 5721.15 537.156 12 -6 2 -4 7441.26 606.724 12 -6 2 -5 15521.0 820.720 12 -6 2 -6 71.4182 161.355 12 -6 2 -7 1462.59 213.486 12 6 -1 -8 2106.90 259.766 6 6 -1 -8 2921.33 277.975 5 6 -1 -7 695.197 177.682 6 6 -1 -7 1025.61 211.014 5 6 -1 -6 3241.89 381.855 3 6 -1 -6 2848.10 364.164 6 6 -1 -5 168.169 159.231 3 6 -1 -4 2298.00 367.764 3 6 -1 -3 186.192 178.386 3 6 -1 -2 4314.07 493.730 3 6 -1 -1 5252.76 529.493 3 6 -1 0-66.1174 148.420 3 6 -1 1 14883.3 866.401 3 -6 1 -2 1328.57 285.447 12 6 -1 2 1222.11 266.432 3 -6 1 -3 3966.04 464.302 12 -6 1 -4 5062.24 506.548 12 -6 1 -5 10335.2 656.051 12 -6 1 -6 265.779 145.207 12 -6 1 -7 292.480 100.115 12 6 0 -9 2982.07 269.084 5 6 0 -8 2719.02 291.989 6 6 0 -8 3535.13 345.277 5 6 0 -7 85.2328 167.763 7 6 0 -7 1024.52 231.483 5 6 0 -6 4981.54 556.263 7 6 0 -6 5241.61 485.001 3 6 0 -5 394.091 192.342 3 6 0 -4 365.376 179.282 3 6 0 -3 3245.42 427.358 3 6 0 -2 1414.76 284.263 3 6 0 -1 3823.38 456.269 3 6 0 0 5046.75 518.291 3 6 0 1 575.575 193.057 3 6 0 2 7098.04 562.379 3 -6 0 -3 4684.56 499.743 12 -6 0 -4 661.321 216.735 12 -6 0 -5 47.8901 134.143 12 -6 0 -6 24.1180 109.201 12 6 1 -9 1104.90 207.123 5 6 1 -8 1082.24 259.080 7 6 1 -8 1858.79 286.393 5 6 1 -7 3388.72 455.493 7 6 1 -7 3683.61 393.740 5 6 1 -6 4732.39 498.951 18 6 1 -6 4557.23 560.128 7 6 1 -6 4999.04 474.455 3 6 1 -6 5819.08 488.635 5 6 1 -5 6564.26 610.471 18 6 1 -5 6352.86 558.799 3 6 1 -4 3034.74 443.538 18 6 1 -4 2565.64 384.888 3 6 1 -3 8535.10 715.274 18 6 1 -3 8640.91 667.377 3 6 1 -2 5859.68 598.953 18 6 1 -2 6178.90 574.062 3 6 1 -1 5113.41 514.048 3 6 1 0 4631.03 464.121 10 6 1 0 5163.38 509.692 3 6 1 1 503.071 199.214 10 6 1 1 342.721 185.200 3 6 1 2 3999.04 459.513 10 6 1 2 3542.26 399.397 3 6 1 3 930.653 242.712 10 -6 -1 -4 2527.89 336.804 12 -6 -1 -5-67.7883 126.055 12 6 2 -9 451.878 170.597 7 6 2 -8 2053.34 355.256 7 6 2 -7-167.878 142.216 18 6 2 -7-177.535 137.237 3 6 2 -6 697.099 213.082 3 6 2 -6 347.317 233.563 7 6 2 -6 597.385 214.118 18 6 2 -5 1057.87 251.475 3 6 2 -5 1182.01 280.165 18 6 2 -4 7931.43 681.962 18 6 2 -4 8039.05 627.255 3 6 2 -3 5964.71 600.597 18 6 2 -3 5618.39 536.473 3 6 2 -2 487.595 186.063 3 6 2 -2 573.990 234.420 18 6 2 -1 9245.08 627.465 10 6 2 -1 9773.19 712.715 3 6 2 0 8919.20 644.582 10 6 2 0 7933.17 629.223 3 6 2 1 6347.16 548.627 10 6 2 1 6473.50 561.288 3 6 2 2 611.342 193.715 10 6 2 2 968.894 200.801 3 6 2 3 1780.42 282.341 10 -6 -2 -4 3959.01 373.389 12 -6 -2 -5 2201.88 228.179 12 6 3 -9 753.396 214.963 7 6 3 -8 134.604 118.354 18 6 3 -8 184.904 198.165 7 6 3 -7 330.414 182.447 3 6 3 -7 420.561 220.403 7 6 3 -7 266.055 158.082 18 6 3 -6-67.1577 137.193 3 6 3 -6 291.756 168.216 18 6 3 -5 5289.36 539.201 18 6 3 -5 5007.39 482.760 3 6 3 -4 505.566 190.433 3 6 3 -4 568.808 244.707 18 6 3 -3 4038.27 480.713 18 6 3 -3 3821.17 452.567 3 6 3 -2 1252.29 287.444 3 6 3 -2 1264.61 283.466 18 6 3 -1 3260.88 384.694 10 6 3 -1 2396.08 364.124 3 6 3 0 2155.48 324.029 10 6 3 0 2156.24 346.841 3 6 3 1-219.456 160.305 10 6 3 1 364.777 147.148 3 6 3 2 1287.64 275.354 10 6 3 3 741.493 188.921 10 -6 -3 -3 1065.40 215.116 12 -6 -3 -4 867.520 153.793 12 6 4 -9 1460.17 206.727 18 6 4 -8 2403.98 299.282 18 6 4 -7 240.081 137.467 3 6 4 -7 457.922 183.626 18 6 4 -6 1533.38 260.473 3 6 4 -6 1758.90 308.074 18 6 4 -5 599.728 188.586 3 6 4 -5 398.797 195.075 18 6 4 -4 567.777 180.350 3 6 4 -4 612.236 209.210 18 6 4 -3 1111.00 257.179 3 6 4 -3 730.587 225.055 18 6 4 -2 1358.77 283.443 3 6 4 -2 1686.60 282.468 18 6 4 -1 3023.84 346.942 10 6 4 -1 2869.32 375.272 3 6 4 0 1345.71 251.442 10 6 4 0 1271.95 249.564 3 6 4 1 1944.67 275.927 10 6 4 1 1587.80 233.859 3 6 4 2 357.794 151.905 10 6 4 3 143.710 103.441 10 6 5 -9-102.833 96.6464 18 6 5 -8 1376.46 230.097 18 6 5 -7 326.997 129.922 3 6 5 -7 720.797 192.848 18 6 5 -6 1057.65 200.880 3 6 5 -6 706.078 193.579 18 6 5 -5 1049.07 222.700 3 6 5 -5 1145.93 243.559 18 6 5 -4 158.804 144.153 3 6 5 -4 193.017 134.089 18 6 5 -3 33.9054 134.751 3 6 5 -3 23.0335 116.159 18 6 5 -2 69.5635 124.489 3 6 5 -1 3997.16 356.474 10 6 5 -1 3649.89 374.861 3 6 5 0 6208.23 421.737 10 6 5 0 5742.11 413.440 3 6 5 1 796.739 168.673 10 6 5 2 331.891 101.373 10 6 6 -8 374.921 122.160 18 6 6 -7 1524.14 221.953 18 6 6 -6 214.083 111.433 3 6 6 -6 49.0742 117.699 18 6 6 -5 1950.45 258.081 18 6 6 -5 1924.59 258.609 3 6 6 -4 1573.81 210.635 18 6 6 -4 1817.15 254.380 3 6 6 -3 460.813 152.899 3 6 6 -2 1964.93 260.614 3 6 6 -1 958.284 170.206 3 6 7 -5 624.655 133.948 3 6 7 -4 270.140 107.103 3 6 7 -3 13.5893 70.9329 3 7 -5 -2 5560.14 371.222 3 7 -5 -1 264.749 126.111 3 7 -5 0 1178.84 210.071 3 7 -5 1-107.523 139.907 3 7 -5 3-32.2870 72.6801 16 7 -4 -3 1133.46 199.744 3 7 -4 -2 560.156 175.144 3 7 -4 -1 1070.69 209.089 3 7 -4 0 1163.18 222.267 3 7 -4 1 1005.00 202.653 3 7 -4 2 1214.38 185.502 16 7 -4 2 1259.30 196.259 3 7 -4 3 684.738 157.583 16 7 -4 4 516.465 130.299 16 7 -3 -4-75.5790 121.034 3 7 -3 -3 195.350 137.948 3 7 -3 -2 750.710 201.225 3 7 -3 -1 267.253 152.000 3 7 -3 0 9059.36 582.358 3 7 -3 1 889.783 202.682 3 7 -3 2 3621.85 312.443 16 7 -3 2 3301.59 309.338 3 7 -3 3 1621.43 212.788 16 -7 3 -3 1266.03 182.783 12 7 -3 4 1903.47 214.762 16 -7 3 -4 876.542 145.097 12 7 -2 -5 176.653 130.735 3 7 -2 -4 19.4716 116.454 3 7 -2 -3 580.681 186.310 3 7 -2 -2 2.94172 125.750 3 7 -2 -1 1069.98 228.484 3 7 -2 0 3399.56 377.142 3 7 -2 1 5373.94 447.767 3 7 -2 2 706.490 158.748 16 -7 2 -2 320.838 138.644 12 7 -2 2 911.788 193.712 3 -7 2 -3 1234.52 202.765 12 -7 2 -4 5236.69 354.088 12 7 -1 -6 3615.47 273.131 3 7 -1 -5 27.9010 132.117 3 7 -1 -4 1752.80 268.434 3 7 -1 -3 515.327 176.721 3 7 -1 -2 312.411 166.565 3 7 -1 -1 1447.26 268.578 3 7 -1 0 2418.86 325.688 3 -7 1 0 2028.31 264.877 12 -7 1 -1 1087.40 227.791 12 7 -1 1 1576.33 248.800 3 -7 1 -2 2876.52 320.113 12 -7 1 -3 355.995 150.422 12 -7 1 -4 1810.06 222.137 12 7 0 -6 2735.41 265.928 3 7 0 -5 2706.48 306.427 3 7 0 -4 307.518 149.574 3 7 0 -3 774.650 206.462 3 7 0 -2 1349.89 264.636 3 -7 0 1 1144.91 226.531 12 7 0 -1 1070.45 242.297 3 -7 0 0 1155.14 227.441 12 7 0 0 1553.67 262.092 3 -7 0 -1 203.852 151.063 12 7 0 1 258.710 151.248 3 -7 0 -2 1569.67 254.889 12 -7 0 -3 657.044 168.541 12 -7 0 -4 97.9825 89.4905 12 7 1 -6 328.368 121.394 3 7 1 -5 271.142 128.768 3 7 1 -4 1505.02 243.927 3 7 1 -3 349.486 163.205 3 7 1 -2 2563.10 338.225 3 7 1 -1 832.499 216.250 3 -7 -1 0 1038.17 231.266 12 7 1 0 1759.05 265.811 3 -7 -1 -1 595.508 189.416 12 7 1 1 633.376 157.501 3 -7 -1 -2 254.498 144.325 12 -7 -1 -3 2532.55 252.775 12 7 2 -6 2643.05 260.393 3 7 2 -5 185.817 119.370 3 7 2 -4 1103.79 214.074 3 7 2 -3 57.9041 104.315 3 7 2 -2 1962.30 288.018 3 7 2 -1 253.756 157.047 3 7 2 0 232.017 128.038 3 -7 -2 -1 259.221 147.780 12 7 2 1 367.555 121.269 3 -7 -2 -2 207.974 114.084 12 7 3 -6 378.721 124.053 3 7 3 -5 97.2477 121.801 3 7 3 -4 455.281 152.267 3 7 3 -3 1652.46 245.943 3 7 3 -2 40.5231 117.981 3 7 3 -1 779.494 182.557 3 7 3 0 270.803 113.499 3 -7 -3 -1-39.7844 89.0996 12 7 4 -5 2006.49 217.287 3 7 4 -4 90.5077 89.9142 3 7 4 -3 527.490 149.613 3 7 4 -2 1829.15 219.851 3 7 4 -1 1220.40 162.533 3 0 0 0 0.00 0.00 0 TITL II-Pha_ang_An in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 6.237407 9.593755 11.350997 112.8119 96.4936 93.1259 ZERR 3.00 0.000402 0.000696 0.000729 0.0064 0.0053 0.0056 LATT 1 SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END ; _shelx_hkl_checksum 22691 _shelx_res_file ; II.res created by SHELXL-2014/8 TITL II in P1 CELL 1.54184 6.2374 9.5938 11.3510 112.812 96.494 93.126 ZERR 1.00 0.0012 0.0019 0.0023 0.030 0.030 0.030 LATT -1 SFAC C H O UNIT 28 40 7 ACTA CONF MPLA 4 C1 C2 C3 C4 C5 C10 MPLA 5 C5 C6 C7 C8 C9 C10 EQIV $1 +x, +y, +z EQIV $2 +x, +y, +z+1 EQIV $3 +x-1, +y, +z-1 RTAB O2H2 O20 H20_$1 RTAB H2O5 H20 O5_$2 RTAB O2O5 O20 O5_$2 RTAB O2O5 O20 H20 O5_$2 RTAB C7H7 C7 H7A_$1 RTAB H7O2 H7A O26_$3 RTAB C7O2 C7 O26_$3 RTAB C7O2 C7 H7A O26_$3 L.S. 4 BOND $H FMAP 2 PLAN 20 WGHT 0.064700 0.038300 FVAR 14.88387 O1 3 1.073399 1.221576 0.384484 11.00000 0.05660 0.07984 = 0.07614 0.05061 -0.01013 -0.01574 O2 3 1.006987 0.604003 0.911991 11.00000 0.05753 0.04574 = 0.03720 0.02141 0.01567 0.01718 O5 3 0.857546 0.879086 0.096923 11.00000 0.06748 0.05705 = 0.03875 0.01972 0.02050 0.02612 O14 3 0.905003 0.658489 0.367115 11.00000 0.05715 0.05043 = 0.03461 0.01526 0.01226 0.02072 O20 3 0.730621 0.737833 0.811831 11.00000 0.04455 0.05732 = 0.03706 0.02178 0.01249 0.01694 O26 3 1.041155 0.528127 1.070640 11.00000 0.07184 0.07311 = 0.04559 0.03351 0.01868 0.02103 O67 3 0.604511 0.670905 0.131909 11.00000 0.08008 0.04008 = 0.03519 0.00575 -0.00373 0.01082 C1 1 0.915722 1.168880 0.301733 11.00000 0.04277 0.04566 = 0.04564 0.02221 0.00780 0.00925 C2 1 0.877485 1.231187 0.201714 11.00000 0.05888 0.05850 = 0.06251 0.03949 0.01016 0.00672 AFIX 43 H2A 2 0.962429 1.318472 0.210794 11.00000 -1.20000 AFIX 0 C3 1 0.725632 1.166373 0.099342 11.00000 0.06965 0.07054 = 0.05916 0.04407 0.00739 0.01974 AFIX 43 H3A 2 0.710321 1.209496 0.038671 11.00000 -1.20000 AFIX 0 C4 1 0.579423 1.028985 0.076803 11.00000 0.06476 0.05879 = 0.04084 0.02530 -0.00077 0.01638 AFIX 23 H4A 2 0.557007 0.963883 -0.014579 11.00000 -1.20000 H4B 2 0.439613 1.058888 0.101386 11.00000 -1.20000 AFIX 0 C5 1 0.671326 0.939482 0.153657 11.00000 0.05008 0.04620 = 0.03007 0.01478 0.00636 0.01656 C6 1 0.507726 0.807749 0.138407 11.00000 0.05448 0.04237 = 0.03663 0.01119 -0.00931 0.00538 AFIX 13 H6A 2 0.372547 0.792810 0.079768 11.00000 -1.20000 AFIX 0 C7 1 0.497014 0.753125 0.241154 11.00000 0.04490 0.04144 = 0.03971 0.01213 -0.00630 0.00135 AFIX 13 H7A 2 0.355003 0.705369 0.242715 11.00000 -1.20000 AFIX 0 C8 1 0.636611 0.833946 0.370404 11.00000 0.03544 0.03609 = 0.02930 0.01105 0.00025 0.00298 AFIX 13 H8A 2 0.541418 0.894617 0.428986 11.00000 -1.20000 AFIX 0 C9 1 0.823576 0.947942 0.371346 11.00000 0.03773 0.03929 = 0.02999 0.01418 0.00308 0.00420 AFIX 13 H9A 2 0.931527 0.887818 0.323815 11.00000 -1.20000 AFIX 0 C10 1 0.742630 1.045997 0.298762 11.00000 0.03873 0.03821 = 0.03152 0.01450 0.00574 0.00737 C11 1 0.933020 1.035298 0.512746 11.00000 0.07017 0.04654 = 0.03950 0.02234 -0.01595 -0.01963 AFIX 23 H11A 2 1.057734 1.101107 0.514000 11.00000 -1.20000 H11B 2 0.831562 1.099431 0.561264 11.00000 -1.20000 AFIX 0 C12 1 1.007375 0.931552 0.579927 11.00000 0.05410 0.05275 = 0.03837 0.02380 -0.01057 -0.01580 AFIX 23 H12A 2 1.065265 0.993403 0.669434 11.00000 -1.20000 H12B 2 1.122919 0.876879 0.538675 11.00000 -1.20000 AFIX 0 C13 1 0.820608 0.816305 0.574757 11.00000 0.04054 0.03272 = 0.02989 0.01410 0.00138 0.00172 C14 1 0.726245 0.726807 0.429939 11.00000 0.03808 0.03510 = 0.03050 0.00902 0.00304 0.00321 C15 1 0.573785 0.598510 0.431431 11.00000 0.05003 0.03866 = 0.04656 0.01609 -0.00779 -0.00776 AFIX 23 H15A 2 0.550683 0.513220 0.348119 11.00000 -1.20000 H15B 2 0.434664 0.632871 0.453529 11.00000 -1.20000 AFIX 0 C16 1 0.692973 0.554586 0.536096 11.00000 0.05366 0.03771 = 0.04100 0.01528 0.00066 -0.00372 AFIX 23 H16A 2 0.749953 0.457647 0.496643 11.00000 -1.20000 H16B 2 0.594087 0.545666 0.593510 11.00000 -1.20000 AFIX 0 C17 1 0.882195 0.682310 0.613121 11.00000 0.03818 0.03535 = 0.03208 0.01278 0.00667 0.00304 AFIX 13 H17A 2 1.013381 0.647597 0.575603 11.00000 -1.20000 AFIX 0 C18 1 0.647971 0.901866 0.652032 11.00000 0.06480 0.04578 = 0.03714 0.01795 0.01263 0.02017 AFIX 137 H18A 2 0.530616 0.830303 0.647867 11.00000 -1.50000 H18B 2 0.593968 0.970926 0.616099 11.00000 -1.50000 H18C 2 0.711318 0.957899 0.740476 11.00000 -1.50000 AFIX 0 C19 1 0.552866 1.131457 0.355020 11.00000 0.04969 0.04226 = 0.04762 0.01670 0.01457 0.01346 AFIX 137 H19A 2 0.589115 1.182088 0.447163 11.00000 -1.50000 H19B 2 0.425731 1.060549 0.334211 11.00000 -1.50000 H19C 2 0.524962 1.205230 0.318902 11.00000 -1.50000 AFIX 0 C20 1 0.928673 0.710161 0.757658 11.00000 0.03902 0.03924 = 0.03135 0.01301 0.00662 0.00463 C21 1 1.099710 0.845502 0.833515 11.00000 0.05556 0.04437 = 0.03558 0.01710 -0.00201 -0.00265 AFIX 137 H21A 2 1.043043 0.937522 0.836077 11.00000 -1.50000 H21B 2 1.227449 0.832269 0.792085 11.00000 -1.50000 H21C 2 1.135983 0.851658 0.919994 11.00000 -1.50000 AFIX 0 C22 1 1.000648 0.565113 0.773066 11.00000 0.04163 0.04077 = 0.03113 0.01451 0.00539 0.00431 AFIX 13 H22A 2 0.885404 0.481657 0.726459 11.00000 -1.20000 AFIX 0 C23 1 1.214694 0.511051 0.729644 11.00000 0.04907 0.05101 = 0.04412 0.02231 0.01383 0.01332 AFIX 23 H23A 2 1.311106 0.598002 0.737504 11.00000 -1.20000 H23B 2 1.187738 0.442337 0.639200 11.00000 -1.20000 AFIX 0 C24 1 1.327047 0.430037 0.807621 11.00000 0.04287 0.03654 = 0.04045 0.01406 0.00438 0.00569 AFIX 13 H24A 2 1.431571 0.506152 0.876578 11.00000 -1.20000 AFIX 0 C25 1 1.165367 0.368260 0.873127 11.00000 0.04428 0.04145 = 0.04603 0.02075 0.00474 0.00569 AFIX 13 H25A 2 1.050802 0.300310 0.805657 11.00000 -1.20000 AFIX 0 C26 1 1.063161 0.501545 0.960193 11.00000 0.04211 0.04643 = 0.04192 0.02350 0.00910 0.00524 C27 1 1.261692 0.280036 0.948222 11.00000 0.07477 0.05455 = 0.06840 0.03740 0.01578 0.01814 AFIX 137 H27A 2 1.150264 0.246254 0.985931 11.00000 -1.50000 H27B 2 1.374177 0.344512 1.015336 11.00000 -1.50000 H27C 2 1.321569 0.193533 0.890904 11.00000 -1.50000 AFIX 0 C28 1 1.455834 0.307375 0.724916 11.00000 0.04806 0.04750 = 0.06321 0.02109 0.01250 0.01236 AFIX 137 H28A 2 1.552523 0.275999 0.779730 11.00000 -1.50000 H28B 2 1.538364 0.347358 0.676412 11.00000 -1.50000 H28C 2 1.357638 0.221599 0.666575 11.00000 -1.50000 AFIX 0 H5 2 0.857852 0.792564 0.113306 11.00000 0.06934 H14 2 0.883946 0.628232 0.288719 11.00000 0.06883 H20 2 0.767768 0.766791 0.883795 11.00000 0.09322 HKLF 4 REM II in P1 REM R1 = 0.0405 for 2545 Fo > 4sig(Fo) and 0.0454 for all 2812 data REM 333 parameters refined using 3 restraints END WGHT 0.0647 0.0383 REM Highest difference peak 0.170, deepest hole -0.193, 1-sigma level 0.040 Q1 1 0.6880 0.7719 0.4064 11.00000 0.05 0.17 Q2 1 0.8613 0.7639 0.5991 11.00000 0.05 0.16 Q3 1 0.6158 0.9856 0.1175 11.00000 0.05 0.16 Q4 1 0.7712 1.0029 0.3347 11.00000 0.05 0.14 Q5 1 1.5642 0.5962 0.8248 11.00000 0.05 0.14 Q6 1 1.0552 0.1933 0.9406 11.00000 0.05 0.13 Q7 1 0.7790 0.7741 0.4966 11.00000 0.05 0.12 Q8 1 0.8316 1.0794 0.2868 11.00000 0.05 0.12 Q9 1 0.5115 0.7215 0.6735 11.00000 0.05 0.12 Q10 1 0.6517 0.6756 0.4378 11.00000 0.05 0.12 Q11 1 0.4209 0.7069 0.6373 11.00000 0.05 0.11 Q12 1 0.7094 0.9921 0.2392 11.00000 0.05 0.11 Q13 1 0.7119 0.7083 0.1159 11.00000 0.05 0.11 Q14 1 0.3342 1.3445 0.3653 11.00000 0.05 0.11 Q15 1 0.8905 1.1753 0.2258 11.00000 0.05 0.11 Q16 1 0.3323 1.1025 -0.0042 11.00000 0.05 0.11 Q17 1 1.1341 1.4140 0.2891 11.00000 0.05 0.11 Q18 1 0.2696 0.5942 0.2240 11.00000 0.05 0.11 Q19 1 0.9610 0.9421 0.8799 11.00000 0.05 0.11 Q20 1 0.9115 0.8821 0.5946 11.00000 0.05 0.10 ; _shelx_res_checksum 77263 loop_ _space_group_symop_operation_xyz 'x, y, z' 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 1.0734(4) 1.2216(4) 0.3845(3) 0.0674(8) Uani d 1 . . O O2 1.0070(4) 0.6040(2) 0.9120(2) 0.0441(5) Uani d 1 . . O O5 0.8575(4) 0.8791(3) 0.0969(2) 0.0524(6) Uani d 1 . . O O14 0.9050(4) 0.6585(3) 0.3671(2) 0.0468(5) Uani d 1 . . O O20 0.7306(4) 0.7378(3) 0.8118(2) 0.0444(5) Uani d 1 . . O O26 1.0412(5) 0.5281(3) 1.0706(2) 0.0591(7) Uani d 1 . . O O67 0.6045(4) 0.6709(3) 0.1319(2) 0.0555(6) Uani d 1 . . C C1 0.9157(5) 1.1689(4) 0.3017(3) 0.0431(7) Uani d 1 . . C C2 0.8775(6) 1.2312(5) 0.2017(4) 0.0551(9) Uani d 1 . . H H2A 0.9624 1.3185 0.2108 0.066 Uiso calc 1 . . C C3 0.7256(6) 1.1664(5) 0.0993(4) 0.0605(10) Uani d 1 . . H H3A 0.7103 1.2095 0.0387 0.073 Uiso calc 1 . . C C4 0.5794(6) 1.0290(4) 0.0768(3) 0.0534(8) Uani d 1 . . H H4A 0.5570 0.9639 -0.0146 0.064 Uiso calc 1 . . H H4B 0.4396 1.0589 0.1014 0.064 Uiso calc 1 . . C C5 0.6713(5) 0.9395(4) 0.1537(3) 0.0417(7) Uani d 1 . . C C6 0.5077(6) 0.8077(4) 0.1384(3) 0.0472(7) Uani d 1 . . H H6A 0.3725 0.7928 0.0798 0.057 Uiso calc 1 . . C C7 0.4970(5) 0.7531(4) 0.2412(3) 0.0444(7) Uani d 1 . . H H7A 0.3550 0.7054 0.2427 0.053 Uiso calc 1 . . C C8 0.6366(4) 0.8339(3) 0.3704(3) 0.0346(6) Uani d 1 . . H H8A 0.5414 0.8946 0.4290 0.042 Uiso calc 1 . . C C9 0.8236(5) 0.9479(3) 0.3713(3) 0.0357(6) Uani d 1 . . H H9A 0.9315 0.8878 0.3238 0.043 Uiso calc 1 . . C C10 0.7426(5) 1.0460(3) 0.2988(3) 0.0358(6) Uani d 1 . . C C11 0.9330(6) 1.0353(4) 0.5127(3) 0.0535(9) Uani d 1 . . H H11A 1.0577 1.1011 0.5140 0.064 Uiso calc 1 . . H H11B 0.8316 1.0994 0.5613 0.064 Uiso calc 1 . . C C12 1.0074(5) 0.9316(4) 0.5799(3) 0.0490(8) Uani d 1 . . H H12A 1.0653 0.9934 0.6694 0.059 Uiso calc 1 . . H H12B 1.1229 0.8769 0.5387 0.059 Uiso calc 1 . . C C13 0.8206(4) 0.8163(3) 0.5748(3) 0.0343(6) Uani d 1 . . C C14 0.7262(4) 0.7268(3) 0.4299(3) 0.0360(6) Uani d 1 . . C C15 0.5738(5) 0.5985(4) 0.4314(3) 0.0471(7) Uani d 1 . . H H15A 0.5507 0.5132 0.3481 0.056 Uiso calc 1 . . H H15B 0.4347 0.6329 0.4535 0.056 Uiso calc 1 . . C C16 0.6930(5) 0.5546(4) 0.5361(3) 0.0451(7) Uani d 1 . . H H16A 0.7500 0.4576 0.4966 0.054 Uiso calc 1 . . H H16B 0.5941 0.5457 0.5935 0.054 Uiso calc 1 . . C C17 0.8822(4) 0.6823(3) 0.6131(3) 0.0353(6) Uani d 1 . . H H17A 1.0134 0.6476 0.5756 0.042 Uiso calc 1 . . C C18 0.6480(6) 0.9019(4) 0.6520(3) 0.0478(7) Uani d 1 . . H H18A 0.5306 0.8303 0.6479 0.072 Uiso calc 1 . . H H18B 0.5940 0.9709 0.6161 0.072 Uiso calc 1 . . H H18C 0.7113 0.9579 0.7405 0.072 Uiso calc 1 . . C C19 0.5529(5) 1.1315(4) 0.3550(3) 0.0459(7) Uani d 1 . . H H19A 0.5891 1.1821 0.4472 0.069 Uiso calc 1 . . H H19B 0.4257 1.0605 0.3342 0.069 Uiso calc 1 . . H H19C 0.5250 1.2052 0.3189 0.069 Uiso calc 1 . . C C20 0.9287(5) 0.7102(3) 0.7577(3) 0.0367(6) Uani d 1 . . C C21 1.0997(5) 0.8455(4) 0.8335(3) 0.0458(7) Uani d 1 . . H H21A 1.0430 0.9375 0.8361 0.069 Uiso calc 1 . . H H21B 1.2274 0.8323 0.7921 0.069 Uiso calc 1 . . H H21C 1.1360 0.8517 0.9200 0.069 Uiso calc 1 . . C C22 1.0006(5) 0.5651(3) 0.7731(3) 0.0378(6) Uani d 1 . . H H22A 0.8854 0.4817 0.7265 0.045 Uiso calc 1 . . C C23 1.2147(6) 0.5111(4) 0.7296(3) 0.0461(7) Uani d 1 . . H H23A 1.3111 0.5980 0.7375 0.055 Uiso calc 1 . . H H23B 1.1877 0.4423 0.6392 0.055 Uiso calc 1 . . C C24 1.3270(5) 0.4300(3) 0.8076(3) 0.0404(6) Uani d 1 . . H H24A 1.4316 0.5062 0.8766 0.048 Uiso calc 1 . . C C25 1.1654(5) 0.3683(4) 0.8731(3) 0.0430(7) Uani d 1 . . H H25A 1.0508 0.3003 0.8057 0.052 Uiso calc 1 . . C C26 1.0632(5) 0.5015(4) 0.9602(3) 0.0414(7) Uani d 1 . . C C27 1.2617(7) 0.2800(5) 0.9482(4) 0.0610(9) Uani d 1 . . H H27A 1.1503 0.2463 0.9859 0.091 Uiso calc 1 . . H H27B 1.3742 0.3445 1.0153 0.091 Uiso calc 1 . . H H27C 1.3216 0.1935 0.8909 0.091 Uiso calc 1 . . C C28 1.4558(6) 0.3074(4) 0.7249(4) 0.0525(8) Uani d 1 . . H H28A 1.5525 0.2760 0.7797 0.079 Uiso calc 1 . . H H28B 1.5384 0.3474 0.6764 0.079 Uiso calc 1 . . H H28C 1.3576 0.2216 0.6666 0.079 Uiso calc 1 . . H H5 0.858(7) 0.793(6) 0.113(4) 0.069(13) Uiso d 1 . . H H14 0.884(8) 0.628(6) 0.289(5) 0.069(14) Uiso d 1 . . H H20 0.768(9) 0.767(7) 0.884(6) 0.09(2) Uiso 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 O1 0.0566(14) 0.0798(18) 0.0761(19) -0.0157(13) -0.0101(13) 0.0506(16) O2 0.0575(13) 0.0457(12) 0.0372(11) 0.0172(10) 0.0157(9) 0.0214(10) O5 0.0675(15) 0.0570(15) 0.0387(12) 0.0261(12) 0.0205(10) 0.0197(11) O14 0.0572(14) 0.0504(13) 0.0346(12) 0.0207(11) 0.0123(10) 0.0153(10) O20 0.0445(12) 0.0573(14) 0.0371(12) 0.0169(10) 0.0125(9) 0.0218(11) O26 0.0718(17) 0.0731(17) 0.0456(14) 0.0210(13) 0.0187(12) 0.0335(13) O67 0.0801(17) 0.0401(12) 0.0352(12) 0.0108(11) -0.0037(11) 0.0057(9) C1 0.0428(16) 0.0457(17) 0.0456(17) 0.0093(13) 0.0078(13) 0.0222(14) C2 0.059(2) 0.058(2) 0.063(2) 0.0067(16) 0.0102(17) 0.0395(19) C3 0.070(2) 0.071(2) 0.059(2) 0.0197(19) 0.0074(18) 0.044(2) C4 0.065(2) 0.059(2) 0.0408(17) 0.0164(17) -0.0008(15) 0.0253(16) C5 0.0501(17) 0.0462(17) 0.0301(14) 0.0166(14) 0.0064(12) 0.0148(13) C6 0.0545(18) 0.0424(17) 0.0366(15) 0.0054(13) -0.0093(13) 0.0112(13) C7 0.0449(16) 0.0414(17) 0.0397(16) 0.0014(13) -0.0063(13) 0.0121(13) C8 0.0354(14) 0.0361(14) 0.0293(14) 0.0030(11) 0.0002(11) 0.0110(11) C9 0.0377(14) 0.0393(15) 0.0300(13) 0.0042(11) 0.0031(10) 0.0142(12) C10 0.0387(14) 0.0382(14) 0.0315(13) 0.0074(11) 0.0057(10) 0.0145(11) C11 0.070(2) 0.0465(18) 0.0395(17) -0.0196(16) -0.0160(16) 0.0223(15) C12 0.0541(19) 0.0528(19) 0.0384(16) -0.0158(15) -0.0106(13) 0.0238(15) C13 0.0405(15) 0.0327(13) 0.0299(13) 0.0017(11) 0.0014(11) 0.0141(11) C14 0.0381(14) 0.0351(14) 0.0305(14) 0.0032(11) 0.0030(11) 0.0090(11) C15 0.0500(18) 0.0387(15) 0.0466(17) -0.0078(13) -0.0078(13) 0.0161(14) C16 0.0537(18) 0.0377(16) 0.0410(16) -0.0037(13) 0.0007(13) 0.0153(13) C17 0.0382(14) 0.0354(14) 0.0321(14) 0.0030(11) 0.0067(11) 0.0128(12) C18 0.065(2) 0.0458(17) 0.0371(16) 0.0202(15) 0.0126(14) 0.0179(14) C19 0.0497(18) 0.0423(16) 0.0476(18) 0.0135(14) 0.0146(14) 0.0167(14) C20 0.0390(14) 0.0392(14) 0.0313(14) 0.0046(11) 0.0066(11) 0.0130(12) C21 0.0556(19) 0.0444(16) 0.0356(15) -0.0026(14) -0.0020(13) 0.0171(13) C22 0.0416(15) 0.0408(15) 0.0311(14) 0.0043(12) 0.0054(11) 0.0145(12) C23 0.0491(17) 0.0510(18) 0.0441(17) 0.0133(14) 0.0138(13) 0.0223(15) C24 0.0429(15) 0.0365(14) 0.0404(15) 0.0057(12) 0.0044(12) 0.0141(12) C25 0.0443(15) 0.0414(16) 0.0460(17) 0.0057(12) 0.0047(13) 0.0207(14) C26 0.0421(15) 0.0464(17) 0.0419(16) 0.0052(13) 0.0091(12) 0.0235(14) C27 0.075(2) 0.055(2) 0.068(2) 0.0181(19) 0.0158(19) 0.0374(19) C28 0.0481(17) 0.0475(18) 0.063(2) 0.0124(14) 0.0125(15) 0.0211(16) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C26 O2 C22 . . 119.2(2) ? C5 O5 H5 . . 100(3) ? C14 O14 H14 . . 114(3) ? C20 O20 H20 . . 103(4) ? C7 O67 C6 . . 60.3(2) ? O1 C1 C2 . . 118.9(3) ? O1 C1 C10 . . 123.8(3) ? C2 C1 C10 . . 117.1(3) ? C3 C2 C1 . . 122.0(3) ? C3 C2 H2A . . 119.0 ? C1 C2 H2A . . 119.0 ? C2 C3 C4 . . 123.3(3) ? C2 C3 H3A . . 118.3 ? C4 C3 H3A . . 118.3 ? C3 C4 C5 . . 112.1(3) ? C3 C4 H4A . . 109.2 ? C5 C4 H4A . . 109.2 ? C3 C4 H4B . . 109.2 ? C5 C4 H4B . . 109.2 ? H4A C4 H4B . . 107.9 ? O5 C5 C6 . . 108.7(3) ? O5 C5 C4 . . 105.4(3) ? C6 C5 C4 . . 110.6(3) ? O5 C5 C10 . . 109.5(2) ? C6 C5 C10 . . 111.4(2) ? C4 C5 C10 . . 111.0(3) ? O67 C6 C7 . . 59.6(2) ? O67 C6 C5 . . 114.1(3) ? C7 C6 C5 . . 121.6(3) ? O67 C6 H6A . . 116.3 ? C7 C6 H6A . . 116.3 ? C5 C6 H6A . . 116.3 ? O67 C7 C6 . . 60.0(2) ? O67 C7 C8 . . 117.5(3) ? C6 C7 C8 . . 120.6(3) ? O67 C7 H7A . . 115.7 ? C6 C7 H7A . . 115.7 ? C8 C7 H7A . . 115.7 ? C7 C8 C14 . . 113.8(2) ? C7 C8 C9 . . 114.2(2) ? C14 C8 C9 . . 109.8(2) ? C7 C8 H8A . . 106.1 ? C14 C8 H8A . . 106.1 ? C9 C8 H8A . . 106.1 ? C10 C9 C11 . . 116.2(2) ? C10 C9 C8 . . 111.0(2) ? C11 C9 C8 . . 108.0(2) ? C10 C9 H9A . . 107.1 ? C11 C9 H9A . . 107.1 ? C8 C9 H9A . . 107.1 ? C19 C10 C9 . . 111.9(2) ? C19 C10 C1 . . 105.6(2) ? C9 C10 C1 . . 114.3(2) ? C19 C10 C5 . . 110.1(2) ? C9 C10 C5 . . 108.3(2) ? C1 C10 C5 . . 106.5(2) ? C12 C11 C9 . . 113.7(3) ? C12 C11 H11A . . 108.8 ? C9 C11 H11A . . 108.8 ? C12 C11 H11B . . 108.8 ? C9 C11 H11B . . 108.8 ? H11A C11 H11B . . 107.7 ? C11 C12 C13 . . 112.1(3) ? C11 C12 H12A . . 109.2 ? C13 C12 H12A . . 109.2 ? C11 C12 H12B . . 109.2 ? C13 C12 H12B . . 109.2 ? H12A C12 H12B . . 107.9 ? C18 C13 C12 . . 109.4(3) ? C18 C13 C14 . . 111.2(2) ? C12 C13 C14 . . 106.9(2) ? C18 C13 C17 . . 111.2(2) ? C12 C13 C17 . . 117.4(2) ? C14 C13 C17 . . 100.3(2) ? O14 C14 C15 . . 107.0(2) ? O14 C14 C8 . . 109.7(2) ? C15 C14 C8 . . 119.1(2) ? O14 C14 C13 . . 105.9(2) ? C15 C14 C13 . . 103.5(2) ? C8 C14 C13 . . 110.8(2) ? C14 C15 C16 . . 103.8(2) ? C14 C15 H15A . . 111.0 ? C16 C15 H15A . . 111.0 ? C14 C15 H15B . . 111.0 ? C16 C15 H15B . . 111.0 ? H15A C15 H15B . . 109.0 ? C15 C16 C17 . . 107.5(2) ? C15 C16 H16A . . 110.2 ? C17 C16 H16A . . 110.2 ? C15 C16 H16B . . 110.2 ? C17 C16 H16B . . 110.2 ? H16A C16 H16B . . 108.5 ? C20 C17 C16 . . 113.2(2) ? C20 C17 C13 . . 119.4(2) ? C16 C17 C13 . . 103.1(2) ? C20 C17 H17A . . 106.8 ? C16 C17 H17A . . 106.8 ? C13 C17 H17A . . 106.8 ? C13 C18 H18A . . 109.5 ? C13 C18 H18B . . 109.5 ? H18A C18 H18B . . 109.5 ? C13 C18 H18C . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? C10 C19 H19A . . 109.5 ? C10 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? C10 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? O20 C20 C21 . . 109.3(3) ? O20 C20 C17 . . 108.7(2) ? C21 C20 C17 . . 112.1(2) ? O20 C20 C22 . . 105.9(2) ? C21 C20 C22 . . 110.1(2) ? C17 C20 C22 . . 110.5(2) ? C20 C21 H21A . . 109.5 ? C20 C21 H21B . . 109.5 ? H21A C21 H21B . . 109.5 ? C20 C21 H21C . . 109.5 ? H21A C21 H21C . . 109.5 ? H21B C21 H21C . . 109.5 ? O2 C22 C23 . . 110.7(2) ? O2 C22 C20 . . 103.0(2) ? C23 C22 C20 . . 118.2(2) ? O2 C22 H22A . . 108.2 ? C23 C22 H22A . . 108.2 ? C20 C22 H22A . . 108.2 ? C22 C23 C24 . . 113.1(3) ? C22 C23 H23A . . 109.0 ? C24 C23 H23A . . 109.0 ? C22 C23 H23B . . 109.0 ? C24 C23 H23B . . 109.0 ? H23A C23 H23B . . 107.8 ? C28 C24 C23 . . 111.1(3) ? C28 C24 C25 . . 112.6(3) ? C23 C24 C25 . . 111.5(3) ? C28 C24 H24A . . 107.1 ? C23 C24 H24A . . 107.1 ? C25 C24 H24A . . 107.1 ? C26 C25 C27 . . 110.4(3) ? C26 C25 C24 . . 107.4(2) ? C27 C25 C24 . . 115.1(3) ? C26 C25 H25A . . 107.9 ? C27 C25 H25A . . 107.9 ? C24 C25 H25A . . 107.9 ? O26 C26 O2 . . 118.0(3) ? O26 C26 C25 . . 125.7(3) ? O2 C26 C25 . . 116.2(3) ? C25 C27 H27A . . 109.5 ? C25 C27 H27B . . 109.5 ? H27A C27 H27B . . 109.5 ? C25 C27 H27C . . 109.5 ? H27A C27 H27C . . 109.5 ? H27B C27 H27C . . 109.5 ? C24 C28 H28A . . 109.5 ? C24 C28 H28B . . 109.5 ? H28A C28 H28B . . 109.5 ? C24 C28 H28C . . 109.5 ? H28A C28 H28C . . 109.5 ? H28B C28 H28C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C1 . 1.214(4) ? O2 C26 . 1.341(4) ? O2 C22 . 1.468(3) ? O5 C5 . 1.433(4) ? O5 H5 . 0.92(5) ? O14 C14 . 1.442(4) ? O14 H14 . 0.81(5) ? O20 C20 . 1.434(4) ? O20 H20 . 0.76(6) ? O26 C26 . 1.204(4) ? O67 C7 . 1.448(4) ? O67 C6 . 1.454(4) ? C1 C2 . 1.478(5) ? C1 C10 . 1.542(4) ? C2 C3 . 1.327(6) ? C2 H2A . 0.9300 ? C3 C4 . 1.480(6) ? C3 H3A . 0.9300 ? C4 C5 . 1.532(4) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 C6 . 1.523(5) ? C5 C10 . 1.560(4) ? C6 C7 . 1.458(5) ? C6 H6A . 0.9800 ? C7 C8 . 1.506(4) ? C7 H7A . 0.9800 ? C8 C14 . 1.530(4) ? C8 C9 . 1.551(4) ? C8 H8A . 0.9800 ? C9 C10 . 1.542(4) ? C9 C11 . 1.546(4) ? C9 H9A . 0.9800 ? C10 C19 . 1.534(4) ? C11 C12 . 1.532(5) ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C12 C13 . 1.542(4) ? C12 H12A . 0.9700 ? C12 H12B . 0.9700 ? C13 C18 . 1.534(4) ? C13 C14 . 1.555(4) ? C13 C17 . 1.562(4) ? C14 C15 . 1.520(4) ? C15 C16 . 1.538(5) ? C15 H15A . 0.9700 ? C15 H15B . 0.9700 ? C16 C17 . 1.561(4) ? C16 H16A . 0.9700 ? C16 H16B . 0.9700 ? C17 C20 . 1.546(4) ? C17 H17A . 0.9800 ? C18 H18A . 0.9600 ? C18 H18B . 0.9600 ? C18 H18C . 0.9600 ? C19 H19A . 0.9600 ? C19 H19B . 0.9600 ? C19 H19C . 0.9600 ? C20 C21 . 1.530(4) ? C20 C22 . 1.552(4) ? C21 H21A . 0.9600 ? C21 H21B . 0.9600 ? C21 H21C . 0.9600 ? C22 C23 . 1.523(4) ? C22 H22A . 0.9800 ? C23 C24 . 1.527(5) ? C23 H23A . 0.9700 ? C23 H23B . 0.9700 ? C24 C28 . 1.526(5) ? C24 C25 . 1.539(4) ? C24 H24A . 0.9800 ? C25 C26 . 1.507(5) ? C25 C27 . 1.518(5) ? C25 H25A . 0.9800 ? C27 H27A . 0.9600 ? C27 H27B . 0.9600 ? C27 H27C . 0.9600 ? C28 H28A . 0.9600 ? C28 H28B . 0.9600 ? C28 H28C . 0.9600 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O20 H20 O5 1_556 0.76(6) 2.22(6) 2.973(4) 173 y C7 H7A O26 1_454 0.98 2.59 3.367(5) 136 y 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 C1 C2 C3 . . . . 171.0(4) ? C10 C1 C2 C3 . . . . -12.6(5) ? C1 C2 C3 C4 . . . . 1.1(6) ? C2 C3 C4 C5 . . . . -20.5(6) ? C3 C4 C5 O5 . . . . -68.1(4) ? C3 C4 C5 C6 . . . . 174.6(3) ? C3 C4 C5 C10 . . . . 50.3(4) ? C7 O67 C6 C5 . . . . 113.8(3) ? O5 C5 C6 O67 . . . . 27.8(3) ? C4 C5 C6 O67 . . . . 143.1(3) ? C10 C5 C6 O67 . . . . -92.9(3) ? O5 C5 C6 C7 . . . . 95.8(4) ? C4 C5 C6 C7 . . . . -148.9(3) ? C10 C5 C6 C7 . . . . -25.0(4) ? C6 O67 C7 C8 . . . . -111.3(3) ? C5 C6 C7 O67 . . . . -101.2(3) ? O67 C6 C7 C8 . . . . 106.1(3) ? C5 C6 C7 C8 . . . . 4.9(5) ? O67 C7 C8 C14 . . . . -71.8(3) ? C6 C7 C8 C14 . . . . -141.6(3) ? O67 C7 C8 C9 . . . . 55.4(4) ? C6 C7 C8 C9 . . . . -14.4(4) ? C7 C8 C9 C10 . . . . 44.7(3) ? C14 C8 C9 C10 . . . . 173.9(2) ? C7 C8 C9 C11 . . . . 173.1(3) ? C14 C8 C9 C11 . . . . -57.7(3) ? C11 C9 C10 C19 . . . . -67.2(3) ? C8 C9 C10 C19 . . . . 56.7(3) ? C11 C9 C10 C1 . . . . 52.9(4) ? C8 C9 C10 C1 . . . . 176.7(2) ? C11 C9 C10 C5 . . . . 171.4(3) ? C8 C9 C10 C5 . . . . -64.8(3) ? O1 C1 C10 C19 . . . . 99.7(4) ? C2 C1 C10 C19 . . . . -76.5(4) ? O1 C1 C10 C9 . . . . -23.8(5) ? C2 C1 C10 C9 . . . . 160.0(3) ? O1 C1 C10 C5 . . . . -143.3(4) ? C2 C1 C10 C5 . . . . 40.5(4) ? O5 C5 C10 C19 . . . . 170.9(3) ? C6 C5 C10 C19 . . . . -68.9(3) ? C4 C5 C10 C19 . . . . 54.9(3) ? O5 C5 C10 C9 . . . . -66.6(3) ? C6 C5 C10 C9 . . . . 53.7(3) ? C4 C5 C10 C9 . . . . 177.5(3) ? O5 C5 C10 C1 . . . . 56.8(3) ? C6 C5 C10 C1 . . . . 177.1(3) ? C4 C5 C10 C1 . . . . -59.1(3) ? C10 C9 C11 C12 . . . . 179.3(3) ? C8 C9 C11 C12 . . . . 53.9(4) ? C9 C11 C12 C13 . . . . -55.1(4) ? C11 C12 C13 C18 . . . . -64.7(3) ? C11 C12 C13 C14 . . . . 55.8(3) ? C11 C12 C13 C17 . . . . 167.4(3) ? C7 C8 C14 O14 . . . . 76.9(3) ? C9 C8 C14 O14 . . . . -52.5(3) ? C7 C8 C14 C15 . . . . -46.7(4) ? C9 C8 C14 C15 . . . . -176.2(3) ? C7 C8 C14 C13 . . . . -166.4(3) ? C9 C8 C14 C13 . . . . 64.1(3) ? C18 C13 C14 O14 . . . . 177.1(2) ? C12 C13 C14 O14 . . . . 57.8(3) ? C17 C13 C14 O14 . . . . -65.2(3) ? C18 C13 C14 C15 . . . . -70.5(3) ? C12 C13 C14 C15 . . . . 170.1(3) ? C17 C13 C14 C15 . . . . 47.2(3) ? C18 C13 C14 C8 . . . . 58.2(3) ? C12 C13 C14 C8 . . . . -61.2(3) ? C17 C13 C14 C8 . . . . 175.9(2) ? O14 C14 C15 C16 . . . . 74.2(3) ? C8 C14 C15 C16 . . . . -160.8(3) ? C13 C14 C15 C16 . . . . -37.3(3) ? C14 C15 C16 C17 . . . . 13.0(3) ? C15 C16 C17 C20 . . . . 146.3(3) ? C15 C16 C17 C13 . . . . 16.0(3) ? C18 C13 C17 C20 . . . . -46.5(3) ? C12 C13 C17 C20 . . . . 80.5(3) ? C14 C13 C17 C20 . . . . -164.2(2) ? C18 C13 C17 C16 . . . . 79.9(3) ? C12 C13 C17 C16 . . . . -153.1(3) ? C14 C13 C17 C16 . . . . -37.8(3) ? C16 C17 C20 O20 . . . . -53.7(3) ? C13 C17 C20 O20 . . . . 67.9(3) ? C16 C17 C20 C21 . . . . -174.6(3) ? C13 C17 C20 C21 . . . . -53.1(3) ? C16 C17 C20 C22 . . . . 62.1(3) ? C13 C17 C20 C22 . . . . -176.3(2) ? C26 O2 C22 C23 . . . . -53.1(3) ? C26 O2 C22 C20 . . . . 179.6(2) ? O20 C20 C22 O2 . . . . -54.7(3) ? C21 C20 C22 O2 . . . . 63.4(3) ? C17 C20 C22 O2 . . . . -172.2(2) ? O20 C20 C22 C23 . . . . -177.1(3) ? C21 C20 C22 C23 . . . . -59.1(3) ? C17 C20 C22 C23 . . . . 65.4(3) ? O2 C22 C23 C24 . . . . 31.1(4) ? C20 C22 C23 C24 . . . . 149.5(3) ? C22 C23 C24 C28 . . . . 148.4(3) ? C22 C23 C24 C25 . . . . 21.9(4) ? C28 C24 C25 C26 . . . . 175.2(3) ? C23 C24 C25 C26 . . . . -59.1(3) ? C28 C24 C25 C27 . . . . 51.8(4) ? C23 C24 C25 C27 . . . . 177.5(3) ? C22 O2 C26 O26 . . . . -170.9(3) ? C22 O2 C26 C25 . . . . 13.8(4) ? C27 C25 C26 O26 . . . . -6.5(5) ? C24 C25 C26 O26 . . . . -132.7(3) ? C27 C25 C26 O2 . . . . 168.4(3) ? C24 C25 C26 O2 . . . . 42.2(4) ? _cod_database_fobs_code 2243872