#------------------------------------------------------------------------------ #$Date: 2019-02-21 05:37:17 +0200 (Thu, 21 Feb 2019) $ #$Revision: 213743 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/28/2242853.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_2242853 loop_ _publ_author_name 'Azzam, Rasha A.' 'Elgemeie, Galal H.' 'Osman, Rokia R.' 'Jones, Peter G.' _publ_section_title ; Crystal structure of potassium [4-amino-5-(benzo[d]thiazol-2-yl)-6-(methylsulfanyl)pyrimidin-2-yl](phenylsulfonyl)azanide dimethylformamide monosolvate hemihydrate ; _journal_coeditor_code SU5477 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 367 _journal_page_last 371 _journal_paper_doi 10.1107/S2056989019002275 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'K +, C18 H14 N5 O2 S3 -, C3 H7 N O, 0.5H2 O' _chemical_formula_moiety '(C18 H14 N5 O2 S3 1-), (K 1+), (C3 H7 N O), 0.5(H2 O)' _chemical_formula_sum 'C21 H22 K N6 O3.5 S3' _chemical_formula_weight 549.72 _chemical_name_systematic ;Potassium [4-amino-5-(benzo[d]thiazol-2-yl)-6-(methylsulfanyl)pyrimidin-2-yl](phenylsulfonyl)azanide dimethylformamide monosolvate hemihydrate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _cell_angle_alpha 90.160(2) _cell_angle_beta 102.361(2) _cell_angle_gamma 117.933(3) _cell_formula_units_Z 4 _cell_length_a 11.8407(2) _cell_length_b 12.6001(4) _cell_length_c 18.8671(5) _cell_measurement_reflns_used 60104 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.6140 _cell_measurement_theta_min 2.3830 _cell_volume 2411.88(13) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_molecular_graphics ; XP (Siemens, 1994) ; _computing_publication_material ; SHELXL2017 (Sheldrick, 2015) ; _computing_structure_refinement ; SHELXL2017 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 16.1419 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur Eos' _diffrn_measurement_method \w-scan _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_unetI/netI 0.0224 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 256622 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.032 _diffrn_reflns_theta_min 2.226 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.99436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1140 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.492 _refine_diff_density_min -0.396 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 652 _refine_ls_number_reflns 13912 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0304 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+1.3600P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.0766 _reflns_number_gt 11954 _reflns_number_total 13912 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file su5477sup1.cif _cod_data_source_block I _cod_original_formula_sum 'C21 H22 K N6 O3.50 S3' _cod_database_code 2242853 _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 0.839 _shelx_estimated_absorpt_t_max 0.881 _shelx_hkl_file ; 0 0 2 263.451 56.5060 0 0 3 32381.3 878.856 0 0 3 31525.4 889.070 0 0 3 31227.0 787.467 0 0 -3 31829.6 876.962 0 0 3 30587.4 873.630 0 0 3 30751.5 875.997 0 0 3 32239.8 888.640 0 0 3 31215.2 854.523 0 0 3 32757.7 893.751 0 0 3 31524.5 883.238 0 0 -3 31913.7 837.733 0 0 3 29714.6 869.299 0 0 3 31422.8 881.079 0 0 3 32820.7 876.954 0 0 3 31249.2 887.517 0 0 -3 31392.1 874.086 0 0 -3 31684.2 888.095 0 0 -3 31647.3 887.096 0 0 -3 32288.6 797.987 0 0 3 31230.9 880.716 0 0 3 31895.2 891.106 0 0 -3 31150.2 885.273 0 0 3 32452.2 891.042 0 0 -3 30478.9 871.517 0 0 -3 30139.5 875.978 0 0 -3 32204.0 890.742 0 0 -3 29752.9 877.011 0 0 3 32030.4 887.781 0 0 -3 31020.7 884.968 0 0 3 32542.3 889.499 0 0 -3 32017.8 884.670 0 0 -3 32135.4 882.045 0 0 -3 33097.5 894.388 0 0 3 32186.6 890.122 0 0 3 30637.1 873.609 0 0 3 31328.7 887.464 0 0 3 32428.2 888.287 0 0 -3 31022.6 884.160 0 0 -3 32269.5 887.600 0 0 3 31553.5 881.569 0 0 -3 31620.2 884.003 0 0 -3 31993.2 865.157 0 0 -3 30578.9 869.410 0 0 3 32410.1 846.985 0 0 -3 30825.1 870.045 0 0 -3 31642.1 885.621 0 0 -3 31198.2 880.126 0 0 3 31084.2 817.946 0 0 -3 31432.2 883.214 0 0 4 2341.93 224.160 0 0 -4 2302.77 212.191 0 0 -4 2082.44 188.876 0 0 -4 2033.06 210.838 0 0 4 2251.04 227.252 0 0 4 1982.73 201.839 0 0 -4 2080.37 216.836 0 0 4 1984.50 163.601 0 0 -4 2082.71 221.408 0 0 4 2068.01 174.024 0 0 -4 1901.57 203.454 0 0 -4 1842.87 195.794 0 0 4 2099.91 213.137 0 0 4 2085.10 206.857 0 0 -4 2137.90 212.822 0 0 4 1879.10 211.668 0 0 -4 1962.88 202.331 0 0 4 1910.47 215.242 0 0 4 1828.02 198.241 0 0 -4 2001.48 211.521 0 0 4 2042.35 207.361 0 0 4 2002.73 204.400 0 0 4 2000.36 200.451 0 0 -4 1927.16 200.048 0 0 -4 2070.23 168.554 0 0 4 2005.19 208.271 0 0 4 2168.76 192.756 0 0 4 2202.87 211.741 0 0 -4 2293.01 223.759 0 0 4 1780.39 200.060 0 0 4 1908.65 204.778 0 0 4 2549.53 230.175 0 0 -4 2304.74 215.530 0 0 4 1947.08 203.690 0 0 -4 1984.86 193.074 0 0 -4 1954.48 199.856 0 0 -4 1941.00 213.739 0 0 -4 2285.48 221.486 0 0 -4 2205.52 213.208 0 0 4 2309.11 216.370 0 0 -4 1968.29 205.901 0 0 -4 2165.95 216.271 0 0 -4 1882.84 197.262 0 0 4 1991.26 208.083 0 0 4 2040.62 206.029 0 0 4 2212.54 214.191 0 0 -4 2041.30 212.609 0 0 -5 15016.0 652.548 0 0 5 15085.1 655.651 0 0 -5 14955.0 659.403 0 0 5 16278.6 624.812 0 0 5 15370.2 657.236 0 0 -5 15476.3 659.568 0 0 5 16040.4 598.399 0 0 5 16817.6 687.667 0 0 -5 15083.0 663.955 0 0 -5 16049.1 668.055 0 0 5 15562.5 556.205 0 0 -5 15888.9 664.386 0 0 -5 15337.8 655.801 0 0 5 16069.8 671.323 0 0 -5 15826.9 675.912 0 0 -5 15254.1 657.889 0 0 5 16249.0 678.779 0 0 5 15121.8 648.805 0 0 5 15274.2 634.851 0 0 5 16758.7 681.555 0 0 -5 15051.8 654.666 0 0 5 14642.2 651.901 0 0 5 16415.2 667.146 0 0 -5 15567.3 669.639 0 0 5 14914.7 656.034 0 0 -5 16084.6 665.417 0 0 -5 16209.2 647.824 0 0 -5 16011.2 566.623 0 0 -5 15814.7 665.906 0 0 -5 16376.3 674.343 0 0 5 16358.6 674.460 0 0 5 15747.3 668.408 0 0 -5 15633.8 663.574 0 0 -5 15865.1 668.527 0 0 -5 15191.0 654.372 0 0 5 16037.7 669.354 0 0 5 15868.5 676.501 0 0 -5 15877.1 655.154 0 0 5 14401.6 649.412 0 0 5 15686.1 662.625 0 0 5 16319.6 678.342 0 0 5 16491.0 673.724 0 0 5 15255.4 659.789 0 0 -5 15351.2 649.727 0 0 -5 14845.4 604.602 0 0 5 15010.0 657.610 0 0 -6 41556.0 1306.98 0 0 6 43025.5 1310.40 0 0 6 41122.9 1320.11 0 0 6 40158.7 1305.68 0 0 -6 40532.8 1282.14 0 0 -6 40086.5 1314.55 0 0 -6 41073.1 1289.23 0 0 6 41267.9 1288.61 0 0 6 42697.1 1317.80 0 0 6 40918.9 1307.05 0 0 6 39800.1 1303.89 0 0 -6 38166.3 1271.17 0 0 6 40271.6 1300.34 0 0 -6 38328.0 1277.94 0 0 6 39818.6 1132.67 0 0 6 38787.1 1293.75 0 0 -6 42323.8 1153.25 0 0 -6 40566.1 1316.40 0 0 6 41490.7 1316.30 0 0 6 40858.4 1301.00 0 0 -6 41706.1 1310.76 0 0 6 38631.2 1290.90 0 0 6 43610.9 1331.57 0 0 6 42859.9 1312.43 0 0 6 41815.4 1316.88 0 0 6 41010.6 1189.01 0 0 -6 41102.7 1308.75 0 0 6 42526.6 1324.97 0 0 -6 43194.0 1324.80 0 0 6 41562.5 1309.77 0 0 -6 39481.1 1287.99 0 0 -6 40026.0 1289.47 0 0 -6 40775.9 1304.89 0 0 -6 40640.5 1223.80 0 0 -6 38863.4 1303.56 0 0 6 44356.1 1337.56 0 0 -6 41216.9 1305.00 0 0 6 41465.6 1316.89 0 0 -6 42695.7 1275.18 0 0 -6 39571.7 1292.44 0 0 -6 39942.0 1311.04 0 0 6 38150.0 1249.85 0 0 6 42355.0 1239.33 0 0 6 41261.0 1306.53 0 0 -6 39595.3 1283.55 0 0 -6 39522.5 1292.23 0 0 -7 2403.05 305.142 0 0 -7 2053.57 294.178 0 0 7 2819.67 325.941 0 0 7 2320.45 291.339 0 0 7 2309.28 256.742 0 0 -7 2204.83 223.831 0 0 7 2348.51 228.633 0 0 7 2275.96 300.121 0 0 -7 2232.48 290.345 0 0 -7 2278.13 300.124 0 0 -7 2706.68 318.299 0 0 7 2271.88 299.962 0 0 -7 1817.50 266.899 0 0 7 2350.47 244.368 0 0 7 1930.73 282.387 0 0 -7 2181.14 262.913 0 0 -7 2115.40 253.125 0 0 7 2662.80 327.495 0 0 -7 2324.32 304.696 0 0 -7 2164.20 288.224 0 0 7 2319.37 294.188 0 0 -7 2211.51 300.903 0 0 7 2483.13 312.378 0 0 7 2933.14 338.724 0 0 7 1990.63 270.326 0 0 -7 2469.33 309.224 0 0 7 2643.54 311.051 0 0 8 37679.4 1383.56 0 0 -8 35865.7 1361.20 0 0 -8 42315.6 1232.13 0 0 -8 37608.7 1373.68 0 0 -8 37758.1 1384.24 0 0 8 38269.5 1396.95 0 0 8 38306.2 1243.48 0 0 8 37987.2 1365.57 0 0 -8 35836.6 1358.69 0 0 8 40341.4 1418.03 0 0 8 37657.5 1387.82 0 0 -8 39708.7 1424.68 0 0 -8 38005.7 1382.78 0 0 8 37471.6 1332.23 0 0 -8 37588.1 1395.68 0 0 8 38138.2 1388.78 0 0 -8 38256.7 1407.44 0 0 -8 37785.6 1380.60 0 0 -8 39731.3 1425.82 0 0 8 40407.7 1418.94 0 0 8 37410.5 1175.18 0 0 8 38472.0 1399.15 0 0 -8 37977.1 1287.58 0 0 8 38841.4 1399.81 0 0 8 39146.0 1404.13 0 0 9 298.269 204.712 0 0 -9 546.552 221.171 0 0 -9 644.412 235.061 0 0 -9 412.497 222.744 0 0 9 329.133 194.184 0 0 -9 383.900 201.009 0 0 -9 866.343 250.284 0 0 9 753.262 258.812 0 0 -9 533.045 222.543 0 0 9 471.092 192.019 0 0 9 538.732 209.408 0 0 -9 640.487 240.460 0 0 9 532.082 155.910 0 0 -9 602.141 195.011 0 0 9 540.485 226.471 0 0 -9 505.772 206.599 0 0 9 832.897 265.938 0 0 9 828.040 225.075 0 0 -9 750.357 153.142 0 0 -9 820.472 242.838 0 0 9 538.103 203.042 0 0 9 523.539 231.355 0 0 9 518.234 243.890 0 0 -9 492.093 200.608 0 0 -10 13103.2 831.515 0 0 -10 14947.2 893.834 0 0 -10 13888.8 862.302 0 0 -10 14703.8 885.021 0 0 10 12363.8 659.741 0 0 10 14256.6 865.290 0 0 10 14037.1 844.281 0 0 10 15656.6 900.363 0 0 -10 14557.0 884.222 0 0 10 12895.1 837.697 0 0 -10 14641.5 868.808 0 0 -10 13725.2 850.947 0 0 10 15554.8 869.341 0 0 10 14637.5 875.636 0 0 10 13457.3 844.834 0 0 10 13147.4 845.793 0 0 10 13280.0 846.798 0 0 -10 13274.1 836.460 0 0 -10 14425.0 868.812 0 0 -10 13219.5 761.738 0 0 10 14327.7 866.648 0 0 10 15289.8 886.157 0 0 -10 13587.3 849.463 0 0 11 15144.1 940.977 0 0 11 13905.5 885.034 0 0 -11 15422.8 951.669 0 0 -11 15227.2 849.567 0 0 -11 13583.5 894.106 0 0 -11 13261.6 894.199 0 0 -11 14862.2 938.531 0 0 11 14276.8 731.337 0 0 11 14614.0 923.678 0 0 11 14730.3 932.052 0 0 -11 13446.9 904.873 0 0 11 14644.0 924.846 0 0 11 14169.3 907.698 0 0 -11 14632.3 924.034 0 0 11 13903.4 858.658 0 0 11 12665.2 866.800 0 0 11 13408.1 892.479 0 0 11 13032.5 880.667 0 0 -11 14058.2 911.309 0 0 -11 13906.2 890.514 0 0 11 13564.8 892.488 0 0 -11 13258.2 886.963 0 0 -11 14878.8 917.733 0 0 12 218.704 232.185 0 0 -12 616.294 302.856 0 0 -12 183.630 207.969 0 0 12 136.939 184.938 0 0 12 166.445 203.352 0 0 12 828.994 308.005 0 0 12 127.013 224.863 0 0 12 507.976 244.406 0 0 -12 365.355 264.055 0 0 12 365.658 149.312 0 0 -12 800.581 275.807 0 0 -12 242.432 194.136 0 0 12 416.210 225.978 0 0 -12 500.362 248.137 0 0 12 312.091 242.445 0 0 -12 265.049 225.169 0 0 -12 971.056 304.826 0 0 -12 185.429 187.097 0 0 -12 400.896 241.688 0 0 12 331.653 238.562 0 0 12 389.025 203.777 0 0 -12 282.462 195.724 0 0 12 435.894 242.032 0 0 -13 969.739 310.288 0 0 -13 440.214 250.643 0 0 13 711.727 281.310 0 0 13 526.585 235.430 0 0 -13 876.511 266.052 0 0 -13 682.122 274.154 0 0 13 875.016 291.298 0 0 13 465.328 213.346 0 0 -13 267.902 222.462 0 0 -13 606.957 238.738 0 0 13 655.438 226.678 0 0 -13 877.089 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6053.09 704.936 0 0 15 5006.25 636.312 0 0 15 6083.26 713.972 0 0 -15 5913.90 696.613 0 0 -15 5489.48 674.173 0 0 -15 5926.44 723.278 0 0 -15 6040.21 695.704 0 0 15 5365.68 655.364 0 0 15 5858.36 536.959 0 0 -15 5021.60 642.451 0 0 15 6178.61 693.671 0 0 15 5449.96 681.567 0 0 15 5320.48 655.189 0 0 16 57946.0 2299.16 0 0 -16 51710.1 2289.26 0 0 -16 55681.9 2367.62 0 0 16 60667.3 2427.99 0 0 16 54229.3 1922.36 0 0 -16 52035.8 2288.08 0 0 16 50775.8 2268.83 0 0 16 51501.8 2243.31 0 0 16 55213.8 2351.66 0 0 -16 56405.5 2385.94 0 0 16 59204.5 2406.62 0 0 -16 53865.1 2339.87 0 0 16 56986.1 2373.54 0 0 16 52331.4 2303.21 0 0 -16 50536.9 2263.03 0 0 16 50109.3 2254.96 0 0 -16 56525.0 2180.93 0 0 16 57519.9 2382.95 0 0 -16 55739.9 2319.54 0 0 -16 54176.5 2322.56 0 0 17 2211.99 518.045 0 0 17 1246.56 400.985 0 0 -17 2912.39 490.903 0 0 17 2365.07 514.760 0 0 17 1722.92 456.009 0 0 -17 1203.50 390.032 0 0 17 1911.92 463.325 0 0 -17 2242.76 508.520 0 0 -17 1074.69 349.619 0 0 17 2672.74 527.027 0 0 -17 1927.17 459.448 0 0 -17 1350.94 432.752 0 0 17 1777.36 430.056 0 0 17 2378.05 530.118 0 0 -17 1688.12 424.080 0 0 17 1793.54 345.866 0 0 -17 2098.10 503.012 0 0 17 2304.41 495.839 0 0 17 2242.88 490.939 0 0 18 1106.53 316.308 0 0 18 2370.85 526.640 0 0 -18 1723.04 476.506 0 0 18 890.887 364.987 0 0 18 952.508 249.876 0 0 18 1210.97 391.115 0 0 -18 1519.88 436.459 0 0 18 1849.13 479.302 0 0 -18 946.875 402.105 0 0 18 1276.38 384.018 0 0 18 566.087 198.138 0 0 18 1250.52 388.370 0 0 18 737.909 336.645 0 0 18 1550.90 431.186 0 0 -18 651.304 294.722 0 0 -18 1455.46 358.914 0 0 -18 1391.12 421.646 0 0 -18 1059.79 386.698 0 0 -18 1681.94 416.036 0 0 -19 2521.75 569.600 0 0 19 2257.24 534.121 0 0 19 2417.26 518.128 0 0 19 2229.03 524.185 0 0 19 3972.23 657.526 0 0 -19 1747.13 462.086 0 0 -19 2392.82 566.385 0 0 -19 2812.52 599.794 0 0 19 3418.59 618.189 0 0 19 2765.24 541.056 0 0 19 2636.57 410.083 0 0 -19 2388.37 559.905 0 0 19 2014.01 499.967 0 0 19 3167.16 613.551 0 0 -19 3369.88 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1236.07 10 -10 -18 11289.4 1200.40 10 -10 -18 8652.10 1087.96 -10 10 18 8817.99 1068.11 -10 10 18 9547.94 1125.15 -10 10 18 9666.39 1110.08 10 -10 -18 11356.8 1209.25 -10 10 18 10291.8 1132.48 10 -10 -18 8738.30 1058.51 10 -10 -18 12497.9 1254.78 -10 10 18 11505.6 1119.33 10 -10 -18 10602.4 1209.19 10 -10 -17-209.215 341.393 -10 10 17 168.849 215.875 -10 10 17 695.748 389.489 10 -10 -17 1057.05 433.772 10 -10 -17 289.447 294.148 -10 10 17-220.803 260.386 -10 10 17 7.07628 268.140 -10 10 17-60.6838 229.739 -10 10 17 84.9610 262.338 10 -10 -17 731.081 409.600 -10 10 17 212.307 254.951 -10 10 17 215.464 324.028 -10 10 17 74.1837 201.696 10 -10 -17 602.054 265.738 10 -10 -17 657.489 370.764 10 -10 -17 489.958 333.056 -10 10 17-111.473 276.537 -10 10 17 198.955 265.659 -10 10 17 311.050 333.993 10 -10 -17 37.6357 252.690 -10 10 17-25.1238 314.248 -10 10 17 44.9466 276.371 10 -10 -17 182.856 196.512 10 -10 -17 144.294 241.117 -10 10 16 6005.33 800.124 10 -10 -16 3415.86 686.413 -10 10 16 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1276.00 366.253 12 -11 -11 817.632 338.466 12 -11 -11 2393.07 506.954 -12 11 11 1047.85 370.252 -12 11 11 1877.07 482.663 -12 11 11 853.206 343.430 12 -11 -11 1108.06 372.168 -12 11 11 1035.16 357.521 -12 11 11 1565.34 442.360 -12 11 11 1282.90 367.856 -12 11 11 1521.82 441.428 12 -11 -11 1773.61 445.996 12 -11 -11 1451.15 437.745 -12 11 11 1706.82 451.822 -12 11 11 1846.06 432.948 -12 11 11 1352.14 352.869 12 -11 -11 1353.86 398.240 -12 11 11 1168.70 385.533 12 -11 -11 1442.95 430.629 12 -11 -11 1637.03 418.168 12 -11 -11 1389.54 380.777 -12 11 11 1487.54 385.943 -12 11 10 743.918 387.959 12 -11 -10 479.221 276.861 12 -11 -10 425.201 211.796 12 -11 -10 441.661 291.980 -12 11 10-158.355 230.414 -12 11 10 493.696 322.921 -12 11 10 462.862 262.392 12 -11 -10 293.058 265.214 -12 11 10 1034.21 370.590 -12 11 10 594.224 309.510 -12 11 10 95.7481 202.144 -12 11 10 301.088 201.998 12 -11 -10 110.237 174.509 12 -11 -10 438.775 226.054 -12 11 10-23.3599 184.575 -12 11 10 320.271 198.144 -12 11 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565.021 12 -11 -4 3565.74 564.176 12 -11 -4 4135.27 586.027 -12 11 4 3719.80 563.512 -12 11 4 3405.13 530.667 -12 11 4 3516.71 559.805 12 -11 -4 3477.26 544.583 -12 11 4 4580.19 619.122 -12 11 4 3529.62 552.897 12 -11 -4 4567.80 728.531 12 -11 -4 4200.66 596.128 -12 11 4 4505.72 703.993 -12 11 3 2303.30 558.913 12 -11 -3 1528.38 393.189 -12 11 3 1225.20 327.618 12 -11 -3 2117.82 448.878 12 -11 -3 1780.17 457.498 -12 11 3 1043.91 336.527 -12 11 3 1159.46 324.292 -12 11 3 829.760 278.294 -12 11 3 1481.62 364.522 12 -11 -3 1507.40 372.768 -12 11 3 1515.81 366.969 12 -11 -3 1499.41 361.725 -12 11 3 1632.08 397.759 12 -11 -3 2142.61 461.915 -12 11 3 1221.14 337.780 12 -11 -3 1315.28 345.666 -12 11 3 1299.24 339.085 -12 11 3 978.154 304.900 12 -11 -3 821.487 400.126 12 -11 -3 1299.44 369.634 -12 11 3 2118.92 474.436 12 -11 -3 1827.46 412.483 -12 11 2 187.737 302.010 12 -11 -2 314.544 224.647 -12 11 2-102.172 206.678 12 -11 -2 452.609 271.850 -12 11 2 52.8157 186.592 12 -11 -2 122.178 188.834 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260.760 -15 2 0 8009.49 1022.64 -15 2 -1 3265.73 665.571 -15 1 12 5090.65 847.100 -15 1 11 3192.90 691.912 -15 1 11 4224.91 750.147 -15 1 10 2575.78 578.186 -15 1 10 3112.70 630.363 -15 1 9 405.270 306.201 -15 1 9 105.176 289.267 -15 1 8 823.205 413.813 -15 1 8 548.166 267.410 -15 1 7 3161.65 672.920 -15 1 7 3774.99 709.932 -15 1 6-141.376 204.386 -15 1 6-157.985 294.543 -15 1 5 311.094 294.320 -15 1 5 68.1303 203.310 -15 0 9 232.481 286.205 -15 0 8 510.466 272.851 -15 0 8 1509.39 492.910 -15 0 7 335.696 229.466 16 -13 -9 894.112 359.193 -16 13 6 29691.1 2020.72 -16 13 5 205.510 270.385 -16 13 4 1327.98 460.625 -16 13 3 518.883 308.320 16 -12 -9 290.317 236.523 16 -12 -8 2094.62 550.551 16 -12 -7 178.716 241.155 16 -12 -6 8554.34 1033.96 -16 12 4-207.660 252.520 -16 12 3 358.815 203.880 -16 12 2 1078.19 433.406 -16 12 1-397.440 329.200 -16 12 0-178.373 269.622 16 -11 -10 8118.31 1067.72 16 -11 -9 22748.4 1782.41 16 -11 -8 1172.60 460.362 16 -11 -7 399.237 250.303 16 -11 -6 720.622 349.086 16 -11 -5 12718.4 1266.36 16 -11 -4 1320.43 421.806 -16 11 2 4063.99 726.811 -16 11 1 1393.70 494.432 -16 11 0-488.344 326.272 -16 11 -1 4489.88 792.620 -16 11 -2 4173.15 788.732 16 -10 -10 534.614 416.812 16 -10 -9 145.644 273.187 16 -10 -8 802.359 324.710 16 -10 -7-149.673 333.091 16 -10 -6 1389.97 449.403 16 -10 -5 748.708 382.428 16 -10 -4 9608.40 1107.78 16 -10 -3 2185.21 530.281 16 -10 -2 4776.41 772.831 16 -10 -1 897.525 366.620 -16 10 -1 4565.14 771.055 -16 10 -2 5022.38 819.808 -16 10 -3 436.128 335.189 16 -9 -9 3813.02 720.574 16 -9 -8 4979.87 851.796 16 -9 -7 6080.05 908.494 16 -9 -6 2953.85 649.330 16 -9 -5 1142.39 437.437 16 -9 -4 813.590 411.330 16 -9 -3 192.459 246.465 16 -9 -2 1703.33 474.172 16 -9 -1 31.4742 203.349 16 -8 -9 2494.95 598.834 16 -8 -8 1026.40 452.177 16 -8 -7 1858.71 552.831 -16 8 6 2126.99 587.865 16 -8 -6 2276.21 607.243 -16 8 5 1083.61 460.211 16 -8 -5 2535.21 601.884 16 -8 -4 16158.1 1468.32 -16 8 4 13600.3 1403.83 -16 8 3 243.217 275.628 16 -8 -3-152.956 248.377 -16 8 2 2019.86 588.426 16 -8 -2 1859.82 532.828 -16 8 1 1619.98 530.040 16 -8 -1 2343.79 580.151 -16 8 0 317.962 298.059 -16 8 -1 623.478 400.996 16 -7 -8 6639.93 972.805 16 -7 -7 3755.61 765.419 -16 7 6-215.974 376.781 16 -7 -6-347.915 378.638 -16 7 5 171.541 274.484 16 -7 -5 1307.42 457.419 -16 7 4 965.332 469.584 16 -7 -4 2249.86 584.325 -16 7 3 4805.71 839.127 16 -7 -3 4760.63 810.909 -16 7 2 5888.53 931.336 16 -7 -2 6316.39 936.471 -16 7 1 1424.78 463.035 -16 7 0 622.936 371.245 -16 7 -1 304.737 281.780 -16 7 -2 798.375 382.048 -16 7 -3-78.2798 264.161 -16 7 -4 4173.94 754.621 -16 6 7 1878.99 578.465 -16 6 6 719.505 341.468 16 -6 -6 1097.46 446.120 -16 6 5-799.667 412.153 16 -6 -5 116.346 250.415 -16 6 4 397.356 300.994 16 -6 -4 776.276 421.002 -16 6 3 6977.48 1017.53 16 -6 -3 7155.23 1006.78 -16 6 2 8314.93 1067.90 16 -6 -2 7475.98 1034.89 -16 6 1 779.171 439.281 -16 6 0 1489.23 515.263 -16 6 -1 7820.74 1026.70 -16 6 -2-205.924 214.896 -16 5 7 2415.27 603.538 -16 5 6-222.198 319.089 -16 5 5 83.0448 267.639 -16 5 4 1826.71 554.882 -16 5 3 452.230 291.596 -16 5 2 266.867 242.961 -16 5 1 228.408 259.743 -16 5 0 4576.09 799.621 -16 5 0 3533.12 697.997 -16 5 -1 225.073 247.183 -16 4 6 895.848 422.887 -16 4 5 316.540 341.727 -16 4 4-177.192 233.389 -16 4 3 282.811 302.631 -16 4 2-1.11879 293.997 -16 4 1 380.095 306.466 -16 3 6 3699.51 746.438 -16 3 5 919.531 405.594 -16 3 4 789.114 425.415 -16 3 3 15622.7 1442.28 17 -10 -3-46.7700 295.444 0 0 0 0.00 0.00 TITL ELG_GRR1 in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 11.840695 12.600138 18.867076 90.1595 102.3609 117.9332 ZERR 5.00 0.000117 0.000203 0.000259 0.0012 0.0011 0.0013 LATT 1 SFAC C H N O S UNIT 90.00 75.00 25.00 10.00 15.00 TREF HKLF 4 END ; _shelx_hkl_checksum 56662 _shelx_res_file ; TITL ELG_GRR1 in P-1 shelx.res created by SHELXL-2017/1 at 09:35:14 on 12-Dec-2018 CELL 0.71073 11.840695 12.600138 18.867076 90.1595 102.3609 117.9332 ZERR 4.00 0.00024 0.00041 0.00052 0.0024 0.0022 0.0026 LATT 1 SFAC C H N O S K UNIT 84 88 24 14 12 4 TEMP -173 SIZE 0.35 0.25 0.25 FMAP 2 PLAN 10 CONN $K 6 CONN S3 S3' 4 CONN N1 2 CONN C10 C10' 3 CONN O2' 1 CONN C91 2 SHEL 999 0.71 ACTA BOND $H HTAB N4 O1' HTAB N4 N3 HTAB N4' O91 HTAB N4' N3' EQIV $1 -x+1, -y+1, -z+1 HTAB O1W O2'_$1 EQIV $2 -x+1, -y+2, -z+1 HTAB O1W O1_$2 EQIV $3 2-x,2-y,-z RTAB CONT C6 C6_$3 CONF L.S. 4 WGHT 0.033100 1.360000 FVAR 3.22245 S1 5 0.679770 1.028284 0.098017 11.00000 0.02517 0.01570 = 0.01810 0.00747 0.01195 0.01219 S2 5 0.471624 1.042451 0.154766 11.00000 0.01847 0.01588 = 0.01479 0.00621 0.00581 0.01093 S3 5 0.316762 0.909400 0.395537 11.00000 0.01119 0.01133 = 0.01105 0.00208 0.00318 0.00464 C2 1 0.636922 0.905517 0.150965 11.00000 0.01269 0.01213 = 0.01264 0.00324 0.00285 0.00520 C3A 1 0.730991 0.856587 0.074772 11.00000 0.01336 0.01585 = 0.01331 0.00188 0.00309 0.00708 C4 1 0.773889 0.787167 0.041547 11.00000 0.02135 0.02009 = 0.01926 0.00332 0.00738 0.01178 AFIX 43 H4 2 0.762989 0.712529 0.057998 11.00000 -1.20000 AFIX 0 C5 1 0.832410 0.829844 -0.015701 11.00000 0.02007 0.02503 = 0.01806 0.00039 0.00654 0.01213 AFIX 43 H5 2 0.862215 0.784025 -0.038767 11.00000 -1.20000 AFIX 0 C6 1 0.848385 0.939912 -0.040202 11.00000 0.01670 0.02796 = 0.01411 0.00317 0.00503 0.00962 AFIX 43 H6 2 0.889986 0.967721 -0.079226 11.00000 -1.20000 AFIX 0 C7 1 0.805071 1.008854 -0.008946 11.00000 0.01975 0.02185 = 0.01560 0.00573 0.00650 0.00952 AFIX 43 H7 2 0.814762 1.082683 -0.026224 11.00000 -1.20000 AFIX 0 C7A 1 0.746475 0.965627 0.049065 11.00000 0.01553 0.01706 = 0.01332 0.00261 0.00461 0.00828 C8 1 0.574835 0.895694 0.211277 11.00000 0.01331 0.01119 = 0.01197 0.00299 0.00409 0.00554 C9 1 0.502588 0.954991 0.220935 11.00000 0.01148 0.01098 = 0.01263 0.00291 0.00226 0.00471 C10 1 0.464765 0.874550 0.327338 11.00000 0.01014 0.01250 = 0.01228 0.00241 0.00226 0.00395 C11 1 0.576095 0.814968 0.264595 11.00000 0.01144 0.01177 = 0.01295 0.00235 0.00190 0.00468 C12 1 0.374160 1.089050 0.194055 11.00000 0.01827 0.01888 = 0.01802 0.00277 0.00383 0.01199 AFIX 137 H12A 2 0.417727 1.120507 0.245597 11.00000 -1.50000 H12B 2 0.286843 1.019598 0.190301 11.00000 -1.50000 H12C 2 0.364720 1.152476 0.167707 11.00000 -1.50000 AFIX 0 C13 1 0.170105 0.820288 0.326874 11.00000 0.01166 0.01464 = 0.01242 0.00132 0.00403 0.00480 C14 1 0.115723 0.694786 0.322205 11.00000 0.02130 0.01543 = 0.02235 0.00366 0.00148 0.00567 AFIX 43 H14 2 0.159533 0.658842 0.352897 11.00000 -1.20000 AFIX 0 C15 1 -0.003685 0.622785 0.271953 11.00000 0.02299 0.01607 = 0.02595 0.00031 0.00171 0.00085 AFIX 43 H15 2 -0.041467 0.537174 0.268056 11.00000 -1.20000 AFIX 0 C16 1 -0.067655 0.675902 0.227513 11.00000 0.01429 0.02684 = 0.01907 -0.00389 0.00095 0.00360 AFIX 43 H16 2 -0.149850 0.626424 0.193940 11.00000 -1.20000 AFIX 0 C17 1 -0.012099 0.800645 0.231960 11.00000 0.01838 0.02741 = 0.02001 -0.00081 -0.00019 0.01301 AFIX 43 H17 2 -0.055603 0.836490 0.200925 11.00000 -1.20000 AFIX 0 C18 1 0.107503 0.873744 0.281862 11.00000 0.01650 0.01764 = 0.01841 0.00052 0.00299 0.00955 AFIX 43 H18 2 0.145806 0.959352 0.285031 11.00000 -1.20000 AFIX 0 N1 3 0.447907 0.945439 0.277169 11.00000 0.01355 0.01406 = 0.01298 0.00380 0.00395 0.00718 N2 3 0.523772 0.807179 0.322394 11.00000 0.01429 0.01425 = 0.01373 0.00391 0.00470 0.00761 N3 3 0.670401 0.825707 0.132348 11.00000 0.01694 0.01566 = 0.01432 0.00359 0.00613 0.00879 N4 3 0.630033 0.742641 0.260542 11.00000 0.02608 0.01833 = 0.01741 0.00865 0.01091 0.01544 H02 2 0.613469 0.687041 0.289959 11.00000 0.03276 H01 2 0.650580 0.736462 0.220837 11.00000 0.03389 N5 3 0.419161 0.865210 0.389308 11.00000 0.01329 0.01661 = 0.01314 0.00406 0.00463 0.00819 O1 4 0.355837 1.035383 0.384277 11.00000 0.01513 0.01089 = 0.01759 0.00149 0.00389 0.00435 O2 4 0.282690 0.879204 0.464847 11.00000 0.01704 0.01828 = 0.01244 0.00334 0.00589 0.00813 S1' 5 0.614367 0.295112 0.016761 11.00000 0.01307 0.02409 = 0.01137 -0.00157 0.00081 0.00726 S2' 5 0.543762 0.469458 0.094281 11.00000 0.02224 0.02347 = 0.01330 0.00867 0.00615 0.01611 S3' 5 0.461925 0.426918 0.358464 11.00000 0.01608 0.01188 = 0.01004 0.00284 0.00399 0.00854 C2' 1 0.724635 0.348468 0.103699 11.00000 0.01354 0.01164 = 0.00987 0.00225 0.00157 0.00526 C3A' 1 0.856177 0.344671 0.036471 11.00000 0.01744 0.01493 = 0.01256 0.00365 0.00466 0.00840 C4' 1 0.972338 0.362911 0.018808 11.00000 0.01931 0.02496 = 0.01708 0.00544 0.00603 0.01271 AFIX 43 H4' 2 1.051620 0.390641 0.055865 11.00000 -1.20000 AFIX 0 C5' 1 0.970227 0.340014 -0.053402 11.00000 0.02489 0.02521 = 0.02068 0.00750 0.01223 0.01561 AFIX 43 H5' 2 1.048490 0.351042 -0.065639 11.00000 -1.20000 AFIX 0 C6' 1 0.854441 0.300827 -0.108705 11.00000 0.02903 0.02181 = 0.01502 0.00296 0.00935 0.01314 AFIX 43 H6' 2 0.855166 0.285520 -0.157894 11.00000 -1.20000 AFIX 0 C7' 1 0.739408 0.284210 -0.092576 11.00000 0.02240 0.02136 = 0.01276 -0.00110 0.00309 0.00877 AFIX 43 H7' 2 0.661289 0.259304 -0.130140 11.00000 -1.20000 AFIX 0 C7A' 1 0.740803 0.304962 -0.019572 11.00000 0.01645 0.01409 = 0.01394 0.00087 0.00455 0.00652 C8' 1 0.680454 0.361292 0.168699 11.00000 0.01050 0.01162 = 0.01076 0.00212 0.00196 0.00424 C9' 1 0.595099 0.408798 0.170953 11.00000 0.01193 0.00993 = 0.01208 0.00298 0.00161 0.00421 C10' 1 0.588051 0.366218 0.287888 11.00000 0.01129 0.00963 = 0.01179 0.00127 0.00137 0.00435 C11' 1 0.720359 0.320862 0.235201 11.00000 0.01020 0.01116 = 0.01183 0.00078 0.00115 0.00412 C12' 1 0.414387 0.487948 0.118412 11.00000 0.02364 0.02844 = 0.01792 0.00583 0.00414 0.01942 AFIX 137 H12D 2 0.348305 0.410299 0.129017 11.00000 -1.50000 H12E 2 0.372818 0.515917 0.077628 11.00000 -1.50000 H12F 2 0.451606 0.547696 0.161728 11.00000 -1.50000 AFIX 0 C13' 1 0.314568 0.373368 0.288154 11.00000 0.01612 0.02133 = 0.01101 0.00389 0.00529 0.01233 C14' 1 0.246433 0.251326 0.261691 11.00000 0.01640 0.02112 = 0.01409 0.00299 0.00582 0.01024 AFIX 43 H14' 2 0.280816 0.199034 0.279043 11.00000 -1.20000 AFIX 0 C15' 1 0.127407 0.206420 0.209554 11.00000 0.01650 0.02720 = 0.01524 0.00139 0.00643 0.00751 AFIX 43 H15' 2 0.081078 0.123450 0.190146 11.00000 -1.20000 AFIX 0 C16' 1 0.076203 0.282715 0.185832 11.00000 0.01605 0.04214 = 0.01499 0.00611 0.00483 0.01586 AFIX 43 H16' 2 -0.006040 0.251404 0.150880 11.00000 -1.20000 AFIX 0 C17' 1 0.144368 0.404401 0.212840 11.00000 0.02674 0.04005 = 0.01858 0.00918 0.00686 0.02563 AFIX 43 H17' 2 0.108590 0.456059 0.196406 11.00000 -1.20000 AFIX 0 C18' 1 0.264921 0.451073 0.263900 11.00000 0.02544 0.02595 = 0.01611 0.00431 0.00547 0.01850 AFIX 43 H18' 2 0.312684 0.534651 0.281964 11.00000 -1.20000 AFIX 0 N1' 3 0.550025 0.413848 0.229325 11.00000 0.01362 0.01372 = 0.01169 0.00348 0.00313 0.00736 N2' 3 0.673010 0.322321 0.293743 11.00000 0.01216 0.01349 = 0.01120 0.00224 0.00188 0.00688 N3' 3 0.843679 0.367515 0.105798 11.00000 0.01453 0.01788 = 0.01184 0.00335 0.00388 0.00799 N4' 3 0.806639 0.277839 0.243744 11.00000 0.01695 0.02171 = 0.01257 0.00484 0.00417 0.01314 H02' 2 0.806762 0.236111 0.278823 11.00000 0.02565 H01' 2 0.838122 0.272405 0.207278 11.00000 0.03224 N5' 3 0.537034 0.355816 0.347809 11.00000 0.01541 0.01397 = 0.01139 0.00346 0.00351 0.00972 O1' 4 0.536533 0.556954 0.357744 11.00000 0.02550 0.01191 = 0.01706 0.00317 0.00648 0.00944 O2' 4 0.416878 0.394209 0.425150 11.00000 0.02120 0.01962 = 0.01167 0.00400 0.00674 0.01181 O1W 4 0.749449 0.843594 0.548103 11.00000 0.03392 0.02093 = 0.03059 0.00489 0.01766 0.01096 H03 2 0.721173 0.779100 0.564064 11.00000 0.04277 H04 2 0.722306 0.880965 0.569055 11.00000 0.05868 K1 6 0.494062 0.689515 0.450397 11.00000 0.02118 0.01917 = 0.01416 0.00500 0.00636 0.01203 K2 6 0.616754 0.183865 0.411841 11.00000 0.01341 0.01430 = 0.01346 0.00372 0.00394 0.00694 C91 1 0.803250 0.044417 0.395445 11.00000 0.01552 0.01756 = 0.01552 0.00190 0.00470 0.00758 AFIX 43 H91 2 0.767210 0.011982 0.435682 11.00000 -1.20000 AFIX 0 C92 1 0.901276 -0.089014 0.408944 11.00000 0.02726 0.02190 = 0.02386 0.00790 0.00814 0.01666 AFIX 137 H92A 2 0.859007 -0.110674 0.449887 11.00000 -1.50000 H92B 2 0.996418 -0.057876 0.427120 11.00000 -1.50000 H92C 2 0.864741 -0.160831 0.373445 11.00000 -1.50000 AFIX 0 C93 1 0.934157 0.047185 0.312302 11.00000 0.02953 0.03117 = 0.02572 0.01280 0.01654 0.02076 AFIX 137 H93A 2 0.914558 0.111216 0.294568 11.00000 -1.50000 H93B 2 0.896673 -0.019652 0.273044 11.00000 -1.50000 H93C 2 1.029863 0.079505 0.327664 11.00000 -1.50000 AFIX 0 N91 3 0.877023 0.003526 0.373884 11.00000 0.01926 0.01884 = 0.01822 0.00640 0.00770 0.01180 O91 4 0.778076 0.121688 0.366917 11.00000 0.02057 0.02081 = 0.01899 0.00385 0.00624 0.01304 C94 1 0.801066 0.478118 0.483718 11.00000 0.01959 0.02295 = 0.01790 0.00359 0.00116 0.00542 AFIX 43 H94 2 0.776435 0.467817 0.431813 11.00000 -1.20000 AFIX 0 C95 1 0.969543 0.680870 0.475269 11.00000 0.03586 0.03045 = 0.03245 0.01627 0.00137 -0.00414 AFIX 137 H95A 2 0.931121 0.654844 0.422790 11.00000 -1.50000 H95B 2 1.062670 0.701335 0.486721 11.00000 -1.50000 H95C 2 0.962128 0.752100 0.488784 11.00000 -1.50000 AFIX 0 C96 1 0.942661 0.606691 0.594441 11.00000 0.09719 0.02947 = 0.02239 -0.00153 0.00303 -0.02152 AFIX 137 H96A 2 1.030708 0.614032 0.610117 11.00000 -1.50000 H96B 2 0.880906 0.539661 0.615825 11.00000 -1.50000 H96C 2 0.945776 0.682111 0.610803 11.00000 -1.50000 AFIX 0 N92 3 0.899493 0.583597 0.516019 11.00000 0.02243 0.01634 = 0.01930 0.00502 0.00229 0.00289 O92 4 0.738092 0.391586 0.514912 11.00000 0.02091 0.01626 = 0.02186 0.00333 0.00366 0.00358 HKLF 4 REM ELG_GRR1 in P-1 REM R1 = 0.0304 for 11954 Fo > 4sig(Fo) and 0.0394 for all 13912 data REM 652 parameters refined using 0 restraints END WGHT 0.0331 1.3600 REM Highest difference peak 0.492, deepest hole -0.396, 1-sigma level 0.061 Q1 1 0.6979 0.3301 0.1989 11.00000 0.05 0.49 Q2 1 0.3772 0.8905 0.3926 11.00000 0.05 0.46 Q3 1 0.4568 0.9094 0.3015 11.00000 0.05 0.43 Q4 1 0.5770 0.8536 0.2357 11.00000 0.05 0.41 Q5 1 0.3829 0.3985 0.3177 11.00000 0.05 0.41 Q6 1 0.5792 0.4006 0.2601 11.00000 0.05 0.40 Q7 1 0.7551 0.8235 0.0623 11.00000 0.05 0.39 Q8 1 0.2291 0.8564 0.3609 11.00000 0.05 0.39 Q9 1 0.2791 0.4026 0.2776 11.00000 0.05 0.38 Q10 1 0.4992 0.5027 0.3591 11.00000 0.05 0.38 ; _shelx_res_checksum 69818 loop_ _space_group_symop_operation_xyz 'x, y, z' '-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 S S1 0.67977(4) 1.02828(3) 0.09802(2) 0.01751(7) Uani d 1 S S2 0.47162(3) 1.04245(3) 0.15477(2) 0.01496(6) Uani d 1 S S3 0.31676(3) 0.90940(3) 0.39554(2) 0.01143(6) Uani d 1 C C2 0.63692(12) 0.90552(11) 0.15096(6) 0.0128(2) Uani d 1 C C3A 0.73099(13) 0.85659(11) 0.07477(7) 0.0142(2) Uani d 1 C C4 0.77389(14) 0.78717(12) 0.04155(7) 0.0191(3) Uani d 1 H H4 0.762989 0.712529 0.057998 0.023 Uiso calc 1 C C5 0.83241(14) 0.82984(13) -0.01570(7) 0.0202(3) Uani d 1 H H5 0.862215 0.784025 -0.038767 0.024 Uiso calc 1 C C6 0.84838(14) 0.93991(13) -0.04020(7) 0.0198(3) Uani d 1 H H6 0.889986 0.967721 -0.079226 0.024 Uiso calc 1 C C7 0.80507(14) 1.00885(12) -0.00895(7) 0.0189(3) Uani d 1 H H7 0.814762 1.082683 -0.026224 0.023 Uiso calc 1 C C7A 0.74648(13) 0.96563(11) 0.04907(7) 0.0149(2) Uani d 1 C C8 0.57484(12) 0.89569(10) 0.21128(6) 0.0121(2) Uani d 1 C C9 0.50259(12) 0.95499(10) 0.22093(6) 0.0121(2) Uani d 1 C C10 0.46477(12) 0.87455(11) 0.32734(6) 0.0123(2) Uani d 1 C C11 0.57609(12) 0.81497(11) 0.26460(6) 0.0126(2) Uani d 1 C C12 0.37416(14) 1.08905(12) 0.19405(7) 0.0172(2) Uani d 1 H H12A 0.417727 1.120507 0.245597 0.026 Uiso calc 1 H H12B 0.286843 1.019598 0.190301 0.026 Uiso calc 1 H H12C 0.364720 1.152476 0.167707 0.026 Uiso calc 1 C C13 0.17010(12) 0.82029(11) 0.32687(6) 0.0134(2) Uani d 1 C C14 0.11572(15) 0.69479(12) 0.32221(8) 0.0217(3) Uani d 1 H H14 0.159533 0.658842 0.352897 0.026 Uiso calc 1 C C15 -0.00368(15) 0.62278(13) 0.27195(8) 0.0260(3) Uani d 1 H H15 -0.041467 0.537174 0.268056 0.031 Uiso calc 1 C C16 -0.06766(14) 0.67590(14) 0.22751(8) 0.0232(3) Uani d 1 H H16 -0.149850 0.626424 0.193940 0.028 Uiso calc 1 C C17 -0.01210(14) 0.80064(13) 0.23196(8) 0.0219(3) Uani d 1 H H17 -0.055603 0.836490 0.200925 0.026 Uiso calc 1 C C18 0.10750(13) 0.87374(12) 0.28186(7) 0.0172(2) Uani d 1 H H18 0.145806 0.959352 0.285031 0.021 Uiso calc 1 N N1 0.44791(11) 0.94544(9) 0.27717(6) 0.0132(2) Uani d 1 N N2 0.52377(11) 0.80718(9) 0.32239(6) 0.0135(2) Uani d 1 N N3 0.67040(11) 0.82571(10) 0.13235(6) 0.0148(2) Uani d 1 N N4 0.63003(12) 0.74264(10) 0.26054(6) 0.0176(2) Uani d 1 H H02 0.6135(19) 0.6870(18) 0.2900(11) 0.033(5) Uiso d 1 H H01 0.651(2) 0.7365(18) 0.2208(11) 0.034(5) Uiso d 1 N N5 0.41916(11) 0.86521(10) 0.38931(6) 0.0137(2) Uani d 1 O O1 0.35584(9) 1.03538(8) 0.38428(5) 0.01534(17) Uani d 1 O O2 0.28269(9) 0.87920(8) 0.46485(5) 0.01566(18) Uani d 1 S S1' 0.61437(3) 0.29511(3) 0.01676(2) 0.01725(7) Uani d 1 S S2' 0.54376(3) 0.46946(3) 0.09428(2) 0.01721(7) Uani d 1 S S3' 0.46192(3) 0.42692(3) 0.35846(2) 0.01176(6) Uani d 1 C C2' 0.72463(12) 0.34847(11) 0.10370(6) 0.0122(2) Uani d 1 C C3A' 0.85618(13) 0.34467(11) 0.03647(7) 0.0145(2) Uani d 1 C C4' 0.97234(14) 0.36291(13) 0.01881(7) 0.0193(3) Uani d 1 H H4' 1.051620 0.390641 0.055865 0.023 Uiso calc 1 C C5' 0.97023(15) 0.34001(13) -0.05340(8) 0.0209(3) Uani d 1 H H5' 1.048490 0.351042 -0.065639 0.025 Uiso calc 1 C C6' 0.85444(15) 0.30083(12) -0.10871(7) 0.0209(3) Uani d 1 H H6' 0.855166 0.285520 -0.157894 0.025 Uiso calc 1 C C7' 0.73941(15) 0.28421(12) -0.09258(7) 0.0198(3) Uani d 1 H H7' 0.661289 0.259304 -0.130140 0.024 Uiso calc 1 C C7A' 0.74080(13) 0.30496(11) -0.01957(7) 0.0150(2) Uani d 1 C C8' 0.68045(12) 0.36129(10) 0.16870(6) 0.0115(2) Uani d 1 C C9' 0.59510(12) 0.40880(10) 0.17095(6) 0.0120(2) Uani d 1 C C10' 0.58805(12) 0.36622(10) 0.28789(6) 0.0114(2) Uani d 1 C C11' 0.72036(12) 0.32086(10) 0.23520(6) 0.0117(2) Uani d 1 C C12' 0.41439(15) 0.48795(13) 0.11841(7) 0.0206(3) Uani d 1 H H12D 0.348305 0.410299 0.129017 0.031 Uiso calc 1 H H12E 0.372818 0.515917 0.077628 0.031 Uiso calc 1 H H12F 0.451606 0.547696 0.161728 0.031 Uiso calc 1 C C13' 0.31457(13) 0.37337(12) 0.28815(6) 0.0144(2) Uani d 1 C C14' 0.24643(13) 0.25133(12) 0.26169(7) 0.0163(2) Uani d 1 H H14' 0.280816 0.199034 0.279043 0.020 Uiso calc 1 C C15' 0.12741(14) 0.20642(13) 0.20955(7) 0.0205(3) Uani d 1 H H15' 0.081078 0.123450 0.190146 0.025 Uiso calc 1 C C16' 0.07620(15) 0.28272(15) 0.18583(7) 0.0234(3) Uani d 1 H H16' -0.006040 0.251404 0.150880 0.028 Uiso calc 1 C C17' 0.14437(15) 0.40440(15) 0.21284(8) 0.0242(3) Uani d 1 H H17' 0.108590 0.456059 0.196406 0.029 Uiso calc 1 C C18' 0.26492(15) 0.45107(13) 0.26390(7) 0.0199(3) Uani d 1 H H18' 0.312684 0.534651 0.281964 0.024 Uiso calc 1 N N1' 0.55003(11) 0.41385(9) 0.22932(5) 0.01266(19) Uani d 1 N N2' 0.67301(10) 0.32232(9) 0.29374(5) 0.01215(19) Uani d 1 N N3' 0.84368(11) 0.36751(10) 0.10580(6) 0.0146(2) Uani d 1 N N4' 0.80664(11) 0.27784(10) 0.24374(6) 0.0154(2) Uani d 1 H H02' 0.8068(18) 0.2361(17) 0.2788(10) 0.026(5) Uiso d 1 H H01' 0.8381(19) 0.2724(17) 0.2073(11) 0.032(5) Uiso d 1 N N5' 0.53703(11) 0.35582(9) 0.34781(5) 0.01244(19) Uani d 1 O O1' 0.53653(10) 0.55695(8) 0.35774(5) 0.01774(19) Uani d 1 O O2' 0.41688(10) 0.39421(8) 0.42515(5) 0.01618(18) Uani d 1 O O1W 0.74945(12) 0.84359(11) 0.54810(6) 0.0277(2) Uani d 1 H H03 0.721(2) 0.779(2) 0.5641(12) 0.043(6) Uiso d 1 H H04 0.722(3) 0.881(2) 0.5691(14) 0.059(7) Uiso d 1 K K1 0.49406(3) 0.68951(3) 0.45040(2) 0.01683(6) Uani d 1 K K2 0.61675(3) 0.18387(2) 0.41184(2) 0.01349(6) Uani d 1 C C91 0.80325(13) 0.04442(12) 0.39544(7) 0.0162(2) Uani d 1 H H91 0.767210 0.011982 0.435682 0.019 Uiso calc 1 C C92 0.90128(15) -0.08901(13) 0.40894(8) 0.0220(3) Uani d 1 H H92A 0.859007 -0.110674 0.449887 0.033 Uiso calc 1 H H92B 0.996418 -0.057876 0.427120 0.033 Uiso calc 1 H H92C 0.864741 -0.160831 0.373445 0.033 Uiso calc 1 C C93 0.93416(16) 0.04719(14) 0.31230(8) 0.0245(3) Uani d 1 H H93A 0.914558 0.111216 0.294568 0.037 Uiso calc 1 H H93B 0.896673 -0.019652 0.273044 0.037 Uiso calc 1 H H93C 1.029863 0.079505 0.327664 0.037 Uiso calc 1 N N91 0.87702(12) 0.00353(10) 0.37388(6) 0.0171(2) Uani d 1 O O91 0.77808(10) 0.12169(9) 0.36692(5) 0.01859(19) Uani d 1 C C94 0.80107(14) 0.47812(13) 0.48372(8) 0.0227(3) Uani d 1 H H94 0.776435 0.467817 0.431813 0.027 Uiso calc 1 C C95 0.96954(19) 0.68087(16) 0.47527(10) 0.0424(5) Uani d 1 H H95A 0.931121 0.654844 0.422790 0.064 Uiso calc 1 H H95B 1.062670 0.701335 0.486721 0.064 Uiso calc 1 H H95C 0.962128 0.752100 0.488784 0.064 Uiso calc 1 C C96 0.9427(3) 0.60669(19) 0.59444(10) 0.0733(9) Uani d 1 H H96A 1.030708 0.614032 0.610117 0.110 Uiso calc 1 H H96B 0.880906 0.539661 0.615825 0.110 Uiso calc 1 H H96C 0.945776 0.682111 0.610803 0.110 Uiso calc 1 N N92 0.89949(12) 0.58360(10) 0.51602(6) 0.0225(2) Uani d 1 O O92 0.73809(10) 0.39159(9) 0.51491(5) 0.0222(2) Uani d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.02517(18) 0.01570(14) 0.01810(14) 0.01219(13) 0.01195(12) 0.00747(11) S2 0.01847(16) 0.01588(14) 0.01479(13) 0.01093(12) 0.00581(11) 0.00621(11) S3 0.01119(14) 0.01133(12) 0.01105(12) 0.00464(11) 0.00318(10) 0.00208(9) C2 0.0127(6) 0.0121(5) 0.0126(5) 0.0052(5) 0.0028(4) 0.0032(4) C3A 0.0134(6) 0.0159(5) 0.0133(5) 0.0071(5) 0.0031(4) 0.0019(4) C4 0.0214(7) 0.0201(6) 0.0193(6) 0.0118(5) 0.0074(5) 0.0033(5) C5 0.0201(7) 0.0250(7) 0.0181(6) 0.0121(6) 0.0065(5) 0.0004(5) C6 0.0167(7) 0.0280(7) 0.0141(6) 0.0096(6) 0.0050(5) 0.0032(5) C7 0.0198(7) 0.0219(6) 0.0156(6) 0.0095(5) 0.0065(5) 0.0057(5) C7A 0.0155(6) 0.0171(6) 0.0133(5) 0.0083(5) 0.0046(4) 0.0026(4) C8 0.0133(6) 0.0112(5) 0.0120(5) 0.0055(5) 0.0041(4) 0.0030(4) C9 0.0115(6) 0.0110(5) 0.0126(5) 0.0047(4) 0.0023(4) 0.0029(4) C10 0.0101(6) 0.0125(5) 0.0123(5) 0.0040(5) 0.0023(4) 0.0024(4) C11 0.0114(6) 0.0118(5) 0.0129(5) 0.0047(5) 0.0019(4) 0.0024(4) C12 0.0183(7) 0.0189(6) 0.0180(6) 0.0120(5) 0.0038(5) 0.0028(5) C13 0.0117(6) 0.0146(5) 0.0124(5) 0.0048(5) 0.0040(4) 0.0013(4) C14 0.0213(7) 0.0154(6) 0.0223(6) 0.0057(5) 0.0015(5) 0.0037(5) C15 0.0230(8) 0.0161(6) 0.0260(7) 0.0008(6) 0.0017(6) 0.0003(5) C16 0.0143(7) 0.0268(7) 0.0191(6) 0.0036(6) 0.0009(5) -0.0039(5) C17 0.0184(7) 0.0274(7) 0.0200(6) 0.0130(6) -0.0002(5) -0.0008(5) C18 0.0165(7) 0.0176(6) 0.0184(6) 0.0095(5) 0.0030(5) 0.0005(5) N1 0.0135(5) 0.0141(5) 0.0130(5) 0.0072(4) 0.0040(4) 0.0038(4) N2 0.0143(5) 0.0143(5) 0.0137(5) 0.0076(4) 0.0047(4) 0.0039(4) N3 0.0169(6) 0.0157(5) 0.0143(5) 0.0088(4) 0.0061(4) 0.0036(4) N4 0.0261(7) 0.0183(5) 0.0174(5) 0.0154(5) 0.0109(5) 0.0087(4) N5 0.0133(5) 0.0166(5) 0.0131(5) 0.0082(4) 0.0046(4) 0.0041(4) O1 0.0151(5) 0.0109(4) 0.0176(4) 0.0043(3) 0.0039(3) 0.0015(3) O2 0.0170(5) 0.0183(4) 0.0124(4) 0.0081(4) 0.0059(3) 0.0033(3) S1' 0.01307(16) 0.02409(16) 0.01137(13) 0.00726(13) 0.00081(11) -0.00157(11) S2' 0.02224(17) 0.02347(15) 0.01330(14) 0.01611(14) 0.00615(12) 0.00867(11) S3' 0.01608(15) 0.01188(13) 0.01004(12) 0.00854(11) 0.00399(10) 0.00284(9) C2' 0.0135(6) 0.0116(5) 0.0099(5) 0.0053(5) 0.0016(4) 0.0022(4) C3A' 0.0174(6) 0.0149(5) 0.0126(5) 0.0084(5) 0.0047(5) 0.0037(4) C4' 0.0193(7) 0.0250(6) 0.0171(6) 0.0127(6) 0.0060(5) 0.0054(5) C5' 0.0249(8) 0.0252(7) 0.0207(6) 0.0156(6) 0.0122(5) 0.0075(5) C6' 0.0290(8) 0.0218(6) 0.0150(6) 0.0131(6) 0.0093(5) 0.0030(5) C7' 0.0224(7) 0.0214(6) 0.0128(6) 0.0088(6) 0.0031(5) -0.0011(5) C7A' 0.0165(6) 0.0141(5) 0.0139(5) 0.0065(5) 0.0045(5) 0.0009(4) C8' 0.0105(6) 0.0116(5) 0.0108(5) 0.0042(4) 0.0020(4) 0.0021(4) C9' 0.0119(6) 0.0099(5) 0.0121(5) 0.0042(4) 0.0016(4) 0.0030(4) C10' 0.0113(6) 0.0096(5) 0.0118(5) 0.0043(4) 0.0014(4) 0.0013(4) C11' 0.0102(6) 0.0112(5) 0.0118(5) 0.0041(4) 0.0011(4) 0.0008(4) C12' 0.0236(7) 0.0284(7) 0.0179(6) 0.0194(6) 0.0041(5) 0.0058(5) C13' 0.0161(6) 0.0213(6) 0.0110(5) 0.0123(5) 0.0053(4) 0.0039(4) C14' 0.0164(7) 0.0211(6) 0.0141(5) 0.0102(5) 0.0058(5) 0.0030(5) C15' 0.0165(7) 0.0272(7) 0.0152(6) 0.0075(6) 0.0064(5) 0.0014(5) C16' 0.0161(7) 0.0421(8) 0.0150(6) 0.0159(6) 0.0048(5) 0.0061(5) C17' 0.0267(8) 0.0400(8) 0.0186(6) 0.0256(7) 0.0069(5) 0.0092(6) C18' 0.0254(8) 0.0259(7) 0.0161(6) 0.0185(6) 0.0055(5) 0.0043(5) N1' 0.0136(5) 0.0137(5) 0.0117(4) 0.0074(4) 0.0031(4) 0.0035(4) N2' 0.0122(5) 0.0135(5) 0.0112(4) 0.0069(4) 0.0019(4) 0.0022(4) N3' 0.0145(5) 0.0179(5) 0.0118(5) 0.0080(4) 0.0039(4) 0.0034(4) N4' 0.0169(6) 0.0217(5) 0.0126(5) 0.0131(5) 0.0042(4) 0.0048(4) N5' 0.0154(5) 0.0140(5) 0.0114(4) 0.0097(4) 0.0035(4) 0.0035(4) O1' 0.0255(5) 0.0119(4) 0.0171(4) 0.0094(4) 0.0065(4) 0.0032(3) O2' 0.0212(5) 0.0196(4) 0.0117(4) 0.0118(4) 0.0067(3) 0.0040(3) O1W 0.0339(7) 0.0209(5) 0.0306(6) 0.0110(5) 0.0177(5) 0.0049(4) K1 0.02118(15) 0.01917(13) 0.01416(12) 0.01203(11) 0.00636(10) 0.00500(9) K2 0.01341(13) 0.01430(12) 0.01346(11) 0.00694(10) 0.00394(9) 0.00372(9) C91 0.0155(6) 0.0176(6) 0.0155(5) 0.0076(5) 0.0047(5) 0.0019(4) C92 0.0273(8) 0.0219(6) 0.0239(7) 0.0167(6) 0.0081(6) 0.0079(5) C93 0.0295(8) 0.0312(7) 0.0257(7) 0.0208(7) 0.0165(6) 0.0128(6) N91 0.0193(6) 0.0188(5) 0.0182(5) 0.0118(5) 0.0077(4) 0.0064(4) O91 0.0206(5) 0.0208(5) 0.0190(4) 0.0130(4) 0.0062(4) 0.0039(4) C94 0.0196(7) 0.0230(7) 0.0179(6) 0.0054(6) 0.0012(5) 0.0036(5) C95 0.0359(10) 0.0305(9) 0.0324(9) -0.0041(8) 0.0014(7) 0.0163(7) C96 0.097(2) 0.0295(9) 0.0224(9) -0.0215(11) 0.0030(10) -0.0015(7) N92 0.0224(6) 0.0163(5) 0.0193(5) 0.0029(5) 0.0023(5) 0.0050(4) O92 0.0209(5) 0.0163(4) 0.0219(5) 0.0036(4) 0.0037(4) 0.0033(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 C7A S1 C2 . . 89.78(6) ? C9 S2 C12 . . 100.78(6) ? O2 S3 O1 . . 113.35(5) ? O2 S3 N5 . . 106.98(5) ? O1 S3 N5 . . 116.05(6) ? O2 S3 C13 . . 106.02(6) ? O1 S3 C13 . . 106.14(6) ? N5 S3 C13 . . 107.73(6) ? N3 C2 C8 . . 122.89(11) ? N3 C2 S1 . . 113.58(9) ? C8 C2 S1 . . 123.50(9) ? N3 C3A C7A . . 114.97(11) ? N3 C3A C4 . . 125.16(11) ? C7A C3A C4 . . 119.86(12) ? C5 C4 C3A . . 118.46(12) ? C5 C4 H4 . . 120.8 ? C3A C4 H4 . . 120.8 ? C4 C5 C6 . . 120.89(13) ? C4 C5 H5 . . 119.6 ? C6 C5 H5 . . 119.6 ? C7 C6 C5 . . 121.59(12) ? C7 C6 H6 . . 119.2 ? C5 C6 H6 . . 119.2 ? C6 C7 C7A . . 117.32(12) ? C6 C7 H7 . . 121.3 ? C7A C7 H7 . . 121.3 ? C7 C7A C3A . . 121.87(12) ? C7 C7A S1 . . 128.54(10) ? C3A C7A S1 . . 109.57(9) ? C9 C8 C11 . . 113.91(11) ? C9 C8 C2 . . 125.26(10) ? C11 C8 C2 . . 120.71(11) ? N1 C9 C8 . . 124.03(11) ? N1 C9 S2 . . 115.19(9) ? C8 C9 S2 . . 120.71(9) ? N2 C10 N1 . . 125.23(11) ? N2 C10 N5 . . 113.88(10) ? N1 C10 N5 . . 120.89(11) ? N4 C11 N2 . . 115.53(11) ? N4 C11 C8 . . 122.42(11) ? N2 C11 C8 . . 122.05(11) ? S2 C12 H12A . . 109.5 ? S2 C12 H12B . . 109.5 ? H12A C12 H12B . . 109.5 ? S2 C12 H12C . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? C18 C13 C14 . . 120.90(12) ? C18 C13 S3 . . 120.94(10) ? C14 C13 S3 . . 118.07(10) ? C15 C14 C13 . . 119.14(13) ? C15 C14 H14 . . 120.4 ? C13 C14 H14 . . 120.4 ? C16 C15 C14 . . 120.15(13) ? C16 C15 H15 . . 119.9 ? C14 C15 H15 . . 119.9 ? C17 C16 C15 . . 120.28(13) ? C17 C16 H16 . . 119.9 ? C15 C16 H16 . . 119.9 ? C16 C17 C18 . . 120.15(13) ? C16 C17 H17 . . 119.9 ? C18 C17 H17 . . 119.9 ? C13 C18 C17 . . 119.37(12) ? C13 C18 H18 . . 120.3 ? C17 C18 H18 . . 120.3 ? C9 N1 C10 . . 116.76(10) ? C10 N2 C11 . . 117.63(10) ? C10 N2 K1 . . 101.67(7) ? C11 N2 K1 . . 140.70(8) ? C2 N3 C3A . . 112.08(10) ? C11 N4 H02 . . 116.3(13) ? C11 N4 H01 . . 116.8(13) ? H02 N4 H01 . . 122.6(18) ? C10 N5 S3 . . 121.03(9) ? C10 N5 K1 . . 97.74(7) ? S3 N5 K1 . . 137.67(6) ? S3 O1 K2 . 1_565 115.26(5) ? S3 O2 K2 . 2_666 136.13(5) ? C7A' S1' C2' . . 89.38(6) ? C9' S2' C12' . . 101.82(6) ? O1' S3' O2' . . 113.04(5) ? O1' S3' N5' . . 114.63(6) ? O2' S3' N5' . . 107.06(5) ? O1' S3' C13' . . 107.07(6) ? O2' S3' C13' . . 104.46(6) ? N5' S3' C13' . . 110.11(6) ? N3' C2' C8' . . 123.71(11) ? N3' C2' S1' . . 114.91(9) ? C8' C2' S1' . . 121.23(9) ? N3' C3A' C4' . . 125.82(12) ? N3' C3A' C7A' . . 114.92(11) ? C4' C3A' C7A' . . 119.19(11) ? C5' C4' C3A' . . 119.11(13) ? C5' C4' H4' . . 120.4 ? C3A' C4' H4' . . 120.4 ? C4' C5' C6' . . 121.01(13) ? C4' C5' H5' . . 119.5 ? C6' C5' H5' . . 119.5 ? C7' C6' C5' . . 120.77(12) ? C7' C6' H6' . . 119.6 ? C5' C6' H6' . . 119.6 ? C6' C7' C7A' . . 118.25(13) ? C6' C7' H7' . . 120.9 ? C7A' C7' H7' . . 120.9 ? C7' C7A' C3A' . . 121.65(12) ? C7' C7A' S1' . . 128.70(11) ? C3A' C7A' S1' . . 109.58(9) ? C9' C8' C11' . . 114.77(11) ? C9' C8' C2' . . 124.58(10) ? C11' C8' C2' . . 120.62(11) ? N1' C9' C8' . . 123.92(11) ? N1' C9' S2' . . 116.05(9) ? C8' C9' S2' . . 120.02(9) ? N2' C10' N1' . . 125.70(11) ? N2' C10' N5' . . 113.44(10) ? N1' C10' N5' . . 120.83(11) ? N2' C11' N4' . . 115.39(10) ? N2' C11' C8' . . 121.93(11) ? N4' C11' C8' . . 122.68(11) ? S2' C12' H12D . . 109.5 ? S2' C12' H12E . . 109.5 ? H12D C12' H12E . . 109.5 ? S2' C12' H12F . . 109.5 ? H12D C12' H12F . . 109.5 ? H12E C12' H12F . . 109.5 ? C14' C13' C18' . . 121.11(12) ? C14' C13' S3' . . 118.40(9) ? C18' C13' S3' . . 120.36(10) ? C13' C14' C15' . . 119.30(12) ? C13' C14' H14' . . 120.3 ? C15' C14' H14' . . 120.3 ? C16' C15' C14' . . 120.01(13) ? C16' C15' H15' . . 120.0 ? C14' C15' H15' . . 120.0 ? C17' C16' C15' . . 120.38(13) ? C17' C16' H16' . . 119.8 ? C15' C16' H16' . . 119.8 ? C16' C17' C18' . . 120.21(13) ? C16' C17' H17' . . 119.9 ? C18' C17' H17' . . 119.9 ? C17' C18' C13' . . 118.96(13) ? C17' C18' H18' . . 120.5 ? C13' C18' H18' . . 120.5 ? C9' N1' C10' . . 116.17(10) ? C10' N2' C11' . . 117.31(10) ? C10' N2' K2 . . 101.07(7) ? C11' N2' K2 . . 136.87(8) ? C2' N3' C3A' . . 111.15(10) ? C11' N4' H02' . . 116.1(13) ? C11' N4' H01' . . 119.3(13) ? H02' N4' H01' . . 121.2(18) ? C10' N5' S3' . . 120.32(8) ? C10' N5' K2 . . 96.61(7) ? S3' N5' K2 . . 143.06(5) ? S3' O1' K1 . . 114.51(5) ? K1 O1W H03 . . 74.2(16) ? K1 O1W H04 . . 93.9(18) ? H03 O1W H04 . . 103(2) ? O92 K1 O1' 2_666 . 122.10(3) y O92 K1 O2' 2_666 2_666 89.19(3) y O1' K1 O2' . 2_666 94.53(3) y O92 K1 N2 2_666 . 117.13(3) y O1' K1 N2 . . 72.98(3) y O2' K1 N2 2_666 . 153.65(3) y O92 K1 O1W 2_666 . 125.24(3) y O1' K1 O1W . . 105.49(3) y O2' K1 O1W 2_666 . 59.75(3) y N2 K1 O1W . . 100.51(3) y O92 K1 N5 2_666 . 80.48(3) y O1' K1 N5 . . 116.98(3) y O2' K1 N5 2_666 . 147.63(3) y N2 K1 N5 . . 46.67(3) y O1W K1 N5 . . 101.98(3) y O91 K2 O2 . 2_666 79.15(3) y O91 K2 O1 . 1_545 122.24(3) y O2 K2 O1 2_666 1_545 104.71(3) y O91 K2 O92 . . 116.05(3) y O2 K2 O92 2_666 . 74.59(3) y O1 K2 O92 1_545 . 120.48(3) y O91 K2 N2' . . 78.44(3) y O2 K2 N2' 2_666 . 145.92(3) y O1 K2 N2' 1_545 . 108.90(3) y O92 K2 N2' . . 92.77(3) y O91 K2 N5' . . 124.93(3) y O2 K2 N5' 2_666 . 145.82(3) y O1 K2 N5' 1_545 . 83.45(3) y O92 K2 N5' . . 72.82(3) y N2' K2 N5' . . 46.50(3) y O91 C91 N91 . . 124.77(12) ? O91 C91 H91 . . 117.6 ? N91 C91 H91 . . 117.6 ? N91 C92 H92A . . 109.5 ? N91 C92 H92B . . 109.5 ? H92A C92 H92B . . 109.5 ? N91 C92 H92C . . 109.5 ? H92A C92 H92C . . 109.5 ? H92B C92 H92C . . 109.5 ? N91 C93 H93A . . 109.5 ? N91 C93 H93B . . 109.5 ? H93A C93 H93B . . 109.5 ? N91 C93 H93C . . 109.5 ? H93A C93 H93C . . 109.5 ? H93B C93 H93C . . 109.5 ? C91 N91 C93 . . 121.04(11) ? C91 N91 C92 . . 122.18(11) ? C93 N91 C92 . . 116.75(11) ? C91 O91 K2 . . 120.87(8) ? O92 C94 N92 . . 125.77(13) ? O92 C94 K2 . . 52.85(7) ? N92 C94 K2 . . 163.54(11) ? O92 C94 H94 . . 117.1 ? N92 C94 H94 . . 117.1 ? K2 C94 H94 . . 67.1 ? N92 C95 H95A . . 109.5 ? N92 C95 H95B . . 109.5 ? H95A C95 H95B . . 109.5 ? N92 C95 H95C . . 109.5 ? H95A C95 H95C . . 109.5 ? H95B C95 H95C . . 109.5 ? N92 C96 H96A . . 109.5 ? N92 C96 H96B . . 109.5 ? H96A C96 H96B . . 109.5 ? N92 C96 H96C . . 109.5 ? H96A C96 H96C . . 109.5 ? H96B C96 H96C . . 109.5 ? C94 N92 C96 . . 120.61(13) ? C94 N92 C95 . . 122.44(13) ? C96 N92 C95 . . 116.95(14) ? C94 O92 K1 . 2_666 132.77(10) ? C94 O92 K2 . . 106.74(9) ? K1 O92 K2 2_666 . 87.35(3) y 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 S1 C7A . 1.7299(13) ? S1 C2 . 1.7716(12) ? S2 C9 . 1.7600(12) ? S2 C12 . 1.7957(13) ? S3 O2 . 1.4500(9) ? S3 O1 . 1.4611(9) ? S3 N5 . 1.5770(11) ? S3 C13 . 1.7767(13) ? C2 N3 . 1.3126(16) ? C2 C8 . 1.4575(16) ? C3A N3 . 1.3859(16) ? C3A C7A . 1.4008(17) ? C3A C4 . 1.4020(18) ? C4 C5 . 1.3822(19) ? C4 H4 . 0.9500 ? C5 C6 . 1.403(2) ? C5 H5 . 0.9500 ? C6 C7 . 1.3818(19) ? C6 H6 . 0.9500 ? C7 C7A . 1.3966(17) ? C7 H7 . 0.9500 ? C8 C9 . 1.4100(17) ? C8 C11 . 1.4354(16) ? C9 N1 . 1.3346(15) ? C10 N2 . 1.3419(16) ? C10 N1 . 1.3507(15) ? C10 N5 . 1.3726(15) ? C11 N4 . 1.3454(16) ? C11 N2 . 1.3474(15) ? C12 H12A . 0.9800 ? C12 H12B . 0.9800 ? C12 H12C . 0.9800 ? C13 C18 . 1.3877(17) ? C13 C14 . 1.3943(18) ? C14 C15 . 1.393(2) ? C14 H14 . 0.9500 ? C15 C16 . 1.390(2) ? C15 H15 . 0.9500 ? C16 C17 . 1.385(2) ? C16 H16 . 0.9500 ? C17 C18 . 1.3938(19) ? C17 H17 . 0.9500 ? C18 H18 . 0.9500 ? K1 N2 . 2.8371(10) y K1 N5 . 2.9038(11) y K1 O1' . 2.6918(9) y K1 O2' 2_666 2.7811(9) y K1 O1W . 2.8991(13) y K1 O92 2_666 2.6779(11) y K2 N2' . 2.8320(10) y K2 N5' . 2.9133(10) y K2 O1 1_545 2.6846(10) y K2 O2 2_666 2.6782(9) y K2 O91 . 2.6594(10) y K2 O92 . 2.8193(10) y N4 H02 . 0.87(2) ? N4 H01 . 0.85(2) ? S1' C7A' . 1.7299(13) ? S1' C2' . 1.7612(12) ? S2' C9' . 1.7639(12) ? S2' C12' . 1.8002(14) ? S3' O1' . 1.4541(9) ? S3' O2' . 1.4566(9) ? S3' N5' . 1.5672(10) ? S3' C13' . 1.7778(13) ? C2' N3' . 1.3058(17) ? C2' C8' . 1.4685(16) ? C3A' N3' . 1.3915(15) ? C3A' C4' . 1.3986(19) ? C3A' C7A' . 1.4046(18) ? C4' C5' . 1.3843(18) ? C4' H4' . 0.9500 ? C5' C6' . 1.401(2) ? C5' H5' . 0.9500 ? C6' C7' . 1.379(2) ? C6' H6' . 0.9500 ? C7' C7A' . 1.3964(17) ? C7' H7' . 0.9500 ? C8' C9' . 1.4024(17) ? C8' C11' . 1.4256(16) ? C9' N1' . 1.3360(15) ? C10' N2' . 1.3432(15) ? C10' N1' . 1.3519(15) ? C10' N5' . 1.3708(15) ? C11' N2' . 1.3451(15) ? C11' N4' . 1.3462(16) ? C12' H12D . 0.9800 ? C12' H12E . 0.9800 ? C12' H12F . 0.9800 ? C13' C14' . 1.3877(18) ? C13' C18' . 1.3929(17) ? C14' C15' . 1.3893(19) ? C14' H14' . 0.9500 ? C15' C16' . 1.387(2) ? C15' H15' . 0.9500 ? C16' C17' . 1.386(2) ? C16' H16' . 0.9500 ? C17' C18' . 1.390(2) ? C17' H17' . 0.9500 ? C18' H18' . 0.9500 ? N4' H02' . 0.847(19) ? N4' H01' . 0.87(2) ? O1W H03 . 0.81(2) ? O1W H04 . 0.82(3) ? C91 O91 . 1.2380(15) ? C91 N91 . 1.3291(17) ? C91 H91 . 0.9500 ? C92 N91 . 1.4548(16) ? C92 H92A . 0.9800 ? C92 H92B . 0.9800 ? C92 H92C . 0.9800 ? C93 N91 . 1.4497(17) ? C93 H93A . 0.9800 ? C93 H93B . 0.9800 ? C93 H93C . 0.9800 ? C94 O92 . 1.2333(17) ? C94 N92 . 1.3177(18) ? C94 H94 . 0.9500 ? C95 N92 . 1.4516(19) ? C95 H95A . 0.9800 ? C95 H95B . 0.9800 ? C95 H95C . 0.9800 ? C96 N92 . 1.439(2) ? C96 H96A . 0.9800 ? C96 H96B . 0.9800 ? C96 H96C . 0.9800 ? 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 N4 H01 N3 . 0.85(2) 2.01(2) 2.6859(15) 136.0(18) yes N4' H01' N3' . 0.87(2) 2.26(2) 2.8781(15) 128.5(16) yes N4 H02 O1' . 0.87(2) 2.06(2) 2.9205(14) 167.5(18) yes N4' H02' O91 . 0.847(19) 2.180(19) 3.0207(14) 172.0(17) yes O1W H03 O2' 2_666 0.81(2) 2.07(2) 2.8314(15) 157(2) yes O1W H04 O1 2_676 0.82(3) 2.00(3) 2.8211(15) 176(3) yes 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_4 _geom_torsion _geom_torsion_publ_flag C7A S1 C2 N3 . -0.17(11) ? C7A S1 C2 C8 . 177.68(11) ? N3 C3A C4 C5 . 179.77(13) ? C7A C3A C4 C5 . 0.8(2) ? C3A C4 C5 C6 . -0.1(2) ? C4 C5 C6 C7 . -0.8(2) ? C5 C6 C7 C7A . 1.1(2) ? C6 C7 C7A C3A . -0.3(2) ? C6 C7 C7A S1 . -178.52(11) ? N3 C3A C7A C7 . -179.64(12) ? C4 C3A C7A C7 . -0.6(2) ? N3 C3A C7A S1 . -1.16(14) ? C4 C3A C7A S1 . 177.90(11) ? C2 S1 C7A C7 . 179.08(13) ? C2 S1 C7A C3A . 0.73(10) ? N3 C2 C8 C9 . -160.28(13) ? S1 C2 C8 C9 . 22.06(18) y N3 C2 C8 C11 . 15.40(19) ? S1 C2 C8 C11 . -162.25(10) ? C11 C8 C9 N1 . 4.82(18) ? C2 C8 C9 N1 . -179.23(12) ? C11 C8 C9 S2 . -171.83(9) ? C2 C8 C9 S2 . 4.12(18) ? C12 S2 C9 N1 . 1.16(11) ? C12 S2 C9 C8 . 178.09(10) ? C9 C8 C11 N4 . 174.05(12) ? C2 C8 C11 N4 . -2.09(19) ? C9 C8 C11 N2 . -6.32(17) ? C2 C8 C11 N2 . 177.53(11) ? O2 S3 C13 C18 . 113.30(11) ? O1 S3 C13 C18 . -7.52(12) ? N5 S3 C13 C18 . -132.44(11) ? O2 S3 C13 C14 . -63.18(12) ? O1 S3 C13 C14 . 175.99(10) ? N5 S3 C13 C14 . 51.07(12) ? C18 C13 C14 C15 . -0.6(2) ? S3 C13 C14 C15 . 175.93(11) ? C13 C14 C15 C16 . -0.4(2) ? C14 C15 C16 C17 . 1.1(2) ? C15 C16 C17 C18 . -1.0(2) ? C14 C13 C18 C17 . 0.7(2) ? S3 C13 C18 C17 . -175.65(10) ? C16 C17 C18 C13 . 0.0(2) ? C8 C9 N1 C10 . 0.33(18) ? S2 C9 N1 C10 . 177.15(9) ? N2 C10 N1 C9 . -4.84(18) ? N5 C10 N1 C9 . 175.93(11) ? N1 C10 N2 C11 . 3.35(19) ? N5 C10 N2 C11 . -177.38(11) ? N1 C10 N2 K1 . -177.35(11) ? N5 C10 N2 K1 . 1.93(12) ? N4 C11 N2 C10 . -177.73(11) ? C8 C11 N2 C10 . 2.63(18) ? N4 C11 N2 K1 . 3.35(19) ? C8 C11 N2 K1 . -176.30(9) ? C8 C2 N3 C3A . -178.31(11) ? S1 C2 N3 C3A . -0.45(14) ? C7A C3A N3 C2 . 1.06(16) ? C4 C3A N3 C2 . -177.94(13) ? N2 C10 N5 S3 . -164.13(9) ? N1 C10 N5 S3 . 15.18(17) y N2 C10 N5 K1 . -1.86(11) ? N1 C10 N5 K1 . 177.45(10) ? O2 S3 N5 C10 . 176.11(10) ? O1 S3 N5 C10 . -56.26(12) ? C13 S3 N5 C10 . 62.49(11) y O2 S3 N5 K1 . 22.74(10) ? O1 S3 N5 K1 . 150.37(7) ? C13 S3 N5 K1 . -90.88(9) ? O2 S3 O1 K2 1_565 99.65(6) ? N5 S3 O1 K2 1_565 -24.76(7) ? C13 S3 O1 K2 1_565 -144.38(5) ? O1 S3 O2 K2 2_666 -113.35(8) ? N5 S3 O2 K2 2_666 15.85(9) ? C13 S3 O2 K2 2_666 130.61(7) ? C7A' S1' C2' N3' . -2.26(10) ? C7A' S1' C2' C8' . -178.12(10) ? N3' C3A' C4' C5' . -177.66(12) ? C7A' C3A' C4' C5' . -0.73(19) ? C3A' C4' C5' C6' . 1.0(2) ? C4' C5' C6' C7' . 0.1(2) ? C5' C6' C7' C7A' . -1.4(2) ? C6' C7' C7A' C3A' . 1.59(19) ? C6' C7' C7A' S1' . 178.38(11) ? N3' C3A' C7A' C7' . 176.71(12) ? C4' C3A' C7A' C7' . -0.55(19) ? N3' C3A' C7A' S1' . -0.63(14) ? C4' C3A' C7A' S1' . -177.89(10) ? C2' S1' C7A' C7' . -175.59(13) ? C2' S1' C7A' C3A' . 1.51(9) ? N3' C2' C8' C9' . 142.01(13) ? S1' C2' C8' C9' . -42.51(16) y N3' C2' C8' C11' . -40.08(17) ? S1' C2' C8' C11' . 135.40(10) ? C11' C8' C9' N1' . -1.83(17) ? C2' C8' C9' N1' . 176.19(11) ? C11' C8' C9' S2' . 176.82(9) ? C2' C8' C9' S2' . -5.15(17) ? C12' S2' C9' N1' . -12.29(11) ? C12' S2' C9' C8' . 168.96(10) ? C9' C8' C11' N2' . 3.63(17) ? C2' C8' C11' N2' . -174.47(11) ? C9' C8' C11' N4' . -176.93(11) ? C2' C8' C11' N4' . 4.96(18) ? O1' S3' C13' C14' . 159.94(10) ? O2' S3' C13' C14' . -79.93(11) ? N5' S3' C13' C14' . 34.72(12) ? O1' S3' C13' C18' . -24.15(12) ? O2' S3' C13' C18' . 95.97(11) ? N5' S3' C13' C18' . -149.37(10) ? C18' C13' C14' C15' . 0.69(19) ? S3' C13' C14' C15' . 176.57(10) ? C13' C14' C15' C16' . -1.62(19) ? C14' C15' C16' C17' . 1.2(2) ? C15' C16' C17' C18' . 0.1(2) ? C16' C17' C18' C13' . -1.0(2) ? C14' C13' C18' C17' . 0.6(2) ? S3' C13' C18' C17' . -175.16(10) ? C8' C9' N1' C10' . -2.00(18) ? S2' C9' N1' C10' . 179.30(9) ? N2' C10' N1' C9' . 4.65(18) ? N5' C10' N1' C9' . -173.44(11) ? N1' C10' N2' C11' . -2.95(18) ? N5' C10' N2' C11' . 175.27(10) ? N1' C10' N2' K2 . -162.67(10) ? N5' C10' N2' K2 . 15.55(11) ? N4' C11' N2' C10' . 179.06(11) ? C8' C11' N2' C10' . -1.46(17) ? N4' C11' N2' K2 . -30.78(17) ? C8' C11' N2' K2 . 148.69(9) ? C8' C2' N3' C3A' . 178.01(11) ? S1' C2' N3' C3A' . 2.26(13) ? C4' C3A' N3' C2' . 176.01(12) ? C7A' C3A' N3' C2' . -1.04(15) ? N2' C10' N5' S3' . 166.36(9) ? N1' C10' N5' S3' . -15.33(16) y N2' C10' N5' K2 . -14.92(10) ? N1' C10' N5' K2 . 163.39(10) ? O1' S3' N5' C10' . -55.50(11) ? O2' S3' N5' C10' . 178.27(9) ? C13' S3' N5' C10' . 65.28(11) y O1' S3' N5' K2 . 126.62(9) ? O2' S3' N5' K2 . 0.38(11) ? C13' S3' N5' K2 . -112.60(9) ? O2' S3' O1' K1 . -20.89(7) ? N5' S3' O1' K1 . -143.97(5) ? C13' S3' O1' K1 . 93.58(6) ? O91 C91 N91 C93 . -0.8(2) ? O91 C91 N91 C92 . -178.96(13) ? N91 C91 O91 K2 . 176.30(10) ? O92 C94 N92 C96 . -0.2(3) ? K2 C94 N92 C96 . -79.3(4) ? O92 C94 N92 C95 . 179.47(17) ? K2 C94 N92 C95 . 100.3(4) ? N92 C94 O92 K1 2_666 98.16(17) ? K2 C94 O92 K1 2_666 -102.27(11) ? N92 C94 O92 K2 . -159.57(14) ? _cod_database_fobs_code 2242853