#------------------------------------------------------------------------------ #$Date: 2019-07-13 12:49:48 +0300 (Sat, 13 Jul 2019) $ #$Revision: 217004 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021727.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_2021727 loop_ _publ_author_name 'Ke, Hua' 'Liao, Jian-Zhen' 'Lu, Can-Zhong' _publ_section_title ; Structural characterization and photochromic behaviour of a novel compound based on a \p-acidic naphthalene diimide derivative and a double hydroxide-bridged dinuclear Al^III^ aqua ion cluster ; _journal_coeditor_code QP3031 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619009872 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac '(C18 H12 N2 O10 S2)2 [Al2 (O H )2 (H2 O1)8], 4H2 O' _chemical_formula_moiety '2(C18 H12 N2 O10 S2 2-), Al2 H18 O10, 4(H2 O)' _chemical_formula_sum 'C36 H50 Al2 N4 O34 S4' _chemical_formula_weight 1265.00 _chemical_name_systematic ; Bis[N,N'-bis(2-sulfonatoethyl)-1,4,5,8-naphthalene diimide] di-\m-hydroxido-bis[tetraaquaaluminium(III)] tetrahydrate ; _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 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 76.525(5) _cell_angle_beta 80.080(4) _cell_angle_gamma 76.808(4) _cell_formula_units_Z 1 _cell_length_a 8.1442(4) _cell_length_b 9.2736(5) _cell_length_c 17.1777(10) _cell_measurement_reflns_used 2864 _cell_measurement_temperature 100.00(19) _cell_measurement_theta_max 76.3950 _cell_measurement_theta_min 4.9840 _cell_volume 1218.60(12) _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 ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 100.00(19) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3503 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku OD SuperNova Dual source diffractometer with an Atlas detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_unetI/netI 0.0619 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 7812 _diffrn_reflns_theta_full 66.599 _diffrn_reflns_theta_max 66.599 _diffrn_reflns_theta_min 5.001 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 3.169 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.48765 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2015) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Parallelepiped _exptl_crystal_F_000 656 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.564 _refine_diff_density_min -0.740 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 402 _refine_ls_number_reflns 4284 _refine_ls_number_restraints 17 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0516 _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^)+(0.0890P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1315 _refine_ls_wR_factor_ref 0.1473 _reflns_number_gt 3439 _reflns_number_total 4284 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file qp3031sup1.cif _cod_data_source_block I _cod_database_code 2021727 _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 -2 9570.62 354.825 2 0 0 2 9092.29 379.689 1 0 0 -3 4836.53 322.944 2 0 0 3 4555.09 342.764 1 0 0 4 9233.71 564.679 1 0 0 -4 10122.8 536.792 2 0 0 5 3332.25 404.349 1 0 0 -5 3019.84 352.918 2 0 0 6 79546.6 1984.07 1 0 0 -6 83614.7 1864.31 2 0 0 7 10455.4 810.397 1 0 0 -7 10651.0 732.738 2 0 0 8 19007.7 1187.20 1 0 0 -8 20867.8 1090.27 2 0 0 -9 4620.78 557.491 2 0 0 9 4636.97 661.344 1 0 0 10 4610.10 690.142 1 0 0 -10 4670.63 586.416 2 0 0 11 12259.9 1174.19 1 0 0 12 4095.87 727.078 1 0 0 13 376.108 281.617 1 0 0 13 396.443 323.585 14 0 0 -13 1133.18 599.990 7 0 0 -14 20519.1 1935.99 7 0 0 14 19989.3 1947.51 14 0 0 14 20596.9 1802.77 1 0 0 -15 172339. 5676.59 7 0 0 15 163464. 5606.19 14 0 0 16 66480.6 3441.11 14 0 0 -16 65654.3 3478.84 7 0 0 17 573.100 523.961 14 0 0 -17-153.937 283.582 7 0 0 -18 2776.20 713.100 7 0 0 18 4310.22 795.865 14 0 0 19 5361.97 756.966 14 0 0 -19 5009.81 789.787 7 0 0 20 9129.90 763.199 14 0 0 -20 9663.07 924.577 7 0 1 -20 5107.03 599.619 7 0 -1 19 15660.7 1213.46 14 0 1 -19 16099.0 1345.46 7 0 1 -18 41202.7 2473.68 7 0 -1 18 41085.6 2363.26 14 0 1 -17 796.895 503.510 7 0 -1 17 933.386 515.121 14 0 1 -16 2878.11 803.526 7 0 -1 16 3094.41 838.540 14 0 -1 15 5453.38 1113.89 14 0 1 -15 4809.96 1054.67 7 0 -1 14 94372.6 3985.84 1 0 1 -14 101770. 4586.63 7 0 1 -13 151884. 5424.27 7 0 -1 13 141634. 4747.65 1 0 -1 12 21195.9 2140.10 14 0 -1 12 20686.5 1739.33 1 0 -1 11 21895.6 1669.15 1 0 -1 10 18765.5 1444.42 1 0 -1 9 1984.57 483.633 1 0 1 -9 1388.87 340.295 2 0 1 -8 6844.32 631.510 2 0 -1 8 7340.96 801.189 1 0 -1 7 48301.0 1825.98 1 0 1 -7 47908.5 1544.16 2 0 -1 6 6535.69 630.962 1 0 1 -6 6062.54 522.413 2 0 1 -5 83797.4 1723.87 2 0 -1 5 88930.5 2066.29 1 0 1 -4 441839. 3680.09 2 0 -1 4 444260. 4144.96 1 0 -1 3 41225.4 1134.66 1 0 1 -3 41584.0 1034.32 2 0 -1 2 54288.9 1158.03 1 0 -1 1 106.429 100.321 1 0 1 0 33842.0 742.493 19 0 -1 -1 16962.8 396.734 3 0 1 1 16571.3 569.161 19 0 -1 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0 -2 19 288.695 212.545 14 0 2 -19 465.512 257.736 7 0 -2 18 604.734 293.691 14 0 2 -18 212.231 297.401 7 0 2 -17 7257.07 1145.68 7 0 -2 17 8180.29 1179.12 14 0 2 -16 2712.36 828.154 7 0 -2 16 2062.89 774.962 14 0 2 -15 6054.68 1203.26 7 0 -2 15 7254.78 1381.74 14 0 2 -14 1098.02 604.577 7 0 -2 14 740.490 564.716 14 0 -2 13 60588.9 3216.32 1 0 -2 13 73419.7 4358.02 14 0 -2 12 45058.7 3281.04 14 0 -2 12 35230.0 2394.70 1 0 -2 11 6500.27 1005.56 1 0 -2 11 4882.16 809.460 8 0 -2 10 42631.0 2364.73 1 0 -2 9 1196.07 460.066 1 0 2 -8 13122.5 929.083 2 0 -2 8 16304.3 1308.07 1 0 2 -7 952.606 278.677 2 0 -2 7 1041.47 395.045 1 0 2 -6 280056. 3951.09 2 0 -2 6 294375. 4737.42 1 0 2 -5 36713.4 1383.49 2 0 -2 5 36268.2 1555.39 1 0 -2 4 3980.79 522.579 1 0 -2 3 22277.3 1032.84 1 0 -2 2 22752.4 972.134 1 0 2 -1 982.558 233.541 19 0 2 0 42325.4 1185.80 19 0 2 1 193524. 2563.14 19 0 -2 -2 23687.3 683.564 3 0 2 2 22578.9 943.237 19 0 -2 -3 120279. 1422.69 3 0 2 3 121264. 2289.07 19 0 -2 -4 362626. 3830.33 2 0 -2 -4 362773. 2406.58 3 0 2 4 354505. 4255.52 19 0 -2 -5 82652.2 1190.69 3 0 -2 -5 83143.9 1988.58 2 0 -2 -6 16156.3 543.969 3 0 -2 -6 17199.2 991.945 2 0 2 6 16702.4 971.036 1 0 2 7 89428.2 2419.15 1 0 -2 -7 89397.0 2408.96 2 0 -2 -8 132645. 3138.33 2 0 2 8 129705. 3148.05 1 0 -2 -9 7909.40 835.561 2 0 2 9 6768.55 780.654 1 0 -2 -10 18388.0 1317.29 2 0 2 10 19168.9 1357.61 1 0 -2 -11 3100.58 585.636 2 0 2 11 3111.89 583.085 1 0 2 12 4244.10 728.017 1 0 -2 -13 1070.33 413.357 4 0 -2 -13 1754.97 562.657 7 0 2 13 1315.26 445.202 1 0 2 13 2461.27 749.401 14 0 -2 -14 17091.7 1691.59 7 0 2 14 16371.2 1512.77 1 0 2 14 17872.9 1731.97 14 0 -2 -14 18221.0 1566.56 4 0 -2 -15 11689.2 1444.53 7 0 2 15 12215.7 1435.58 14 0 -2 -16 9451.18 1276.43 7 0 2 16 10157.4 1281.45 14 0 -2 -17 613.721 438.154 7 0 2 17 75.0993 333.317 14 0 2 18 19052.9 1536.47 14 0 -2 -18 15712.5 1487.89 7 0 2 19 8756.67 937.705 14 0 -2 -19 7769.23 966.021 7 0 -2 -20 655.439 290.318 7 0 2 20 410.205 210.599 14 0 -2 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0 4 19 35128.5 1675.03 14 0 -4 -19 37502.2 1969.07 7 0 -4 -20 4551.60 610.940 7 0 5 -16 204.776 219.810 7 0 -5 16 250.461 272.519 14 0 5 -15 1578.28 495.161 7 0 -5 15 1468.40 529.482 14 0 5 -14 1672.45 583.454 7 0 -5 14 1645.37 675.722 14 0 -5 13 15562.3 1943.60 14 0 -5 12-572.002 575.403 14 0 -5 11 9730.57 1566.05 14 0 -5 11 7035.93 1147.97 8 0 -5 10 3096.82 883.427 8 0 -5 10 4014.88 1013.44 14 0 -5 9 3864.25 832.561 8 0 5 -9 3303.24 791.670 19 0 5 -8 5282.38 865.970 12 0 5 -8 5818.97 977.888 19 0 -5 8 5114.28 889.617 8 0 5 -7 9026.57 1078.68 12 0 5 -7 8776.20 1149.57 19 0 -5 7 9358.59 1103.56 8 0 5 -6 55573.0 2698.48 19 0 -5 6 54666.2 2520.22 8 0 5 -5 56298.3 2586.10 19 0 5 -4 3676.62 664.012 19 0 5 -3 7508.34 909.181 19 0 5 -2 13776.6 1158.59 19 0 5 -1-72.0011 226.994 19 0 5 0 45731.2 2099.19 19 0 5 1 37397.7 1921.67 19 0 5 2 9555.76 1053.09 19 0 5 3 10972.4 1153.93 19 0 5 4 102493. 3488.54 19 0 5 5 80023.8 3164.08 19 0 5 6 4589.37 846.726 19 0 5 7 10293.9 1213.01 19 0 5 8 26069.0 1729.85 1 0 5 8 25209.2 1910.52 19 0 5 9 22018.8 1633.86 1 0 5 10 42994.6 2369.38 1 0 -5 -10 46139.9 2709.21 7 0 5 11 7655.83 1052.39 1 0 -5 -11 7502.08 1129.08 7 0 5 11 5841.62 958.747 14 0 -5 -12 1657.04 587.231 7 0 5 12 875.168 380.678 1 0 5 12 1111.52 438.651 14 0 -5 -13 377.713 289.241 7 0 5 13 68.8989 403.545 14 0 -5 -14 4115.61 911.684 7 0 5 14 3843.95 824.303 14 0 5 15 3098.66 734.054 14 0 -5 -15 1739.73 622.584 7 0 -5 -16 315.624 298.253 7 0 5 16 867.073 465.623 14 0 -5 -17 3213.44 710.073 7 0 5 17 5616.07 829.032 14 0 -5 -18 65.9605 281.106 7 0 -5 -19 1908.89 462.909 7 0 -5 -20 321.515 195.134 7 0 6 -15 8996.79 782.596 7 0 -6 15 10060.5 872.583 14 0 6 -14 2218.65 504.871 7 0 -6 14 3009.47 660.390 14 0 -6 13 3681.36 885.668 14 0 -6 12 22356.5 2156.23 14 0 -6 11 9.89228 443.859 8 0 -6 11 959.069 690.985 14 0 -6 10 76029.2 4030.50 14 0 -6 10 60522.7 3175.06 8 0 -6 9 2841.39 750.167 8 0 -6 8 6162.74 1053.74 8 0 6 -8 5891.58 888.116 12 0 -6 7 1865.76 641.418 8 0 6 -7 2761.32 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1457.54 2 -1 1 -5 47930.0 1622.83 2 1 -1 5 53039.5 1650.78 1 -1 1 -6 28348.1 1338.00 2 1 -1 6 31985.6 1410.56 1 -1 1 -7 924.276 314.080 2 1 -1 7 1668.89 391.248 1 1 -1 8 24625.1 1431.87 1 -1 1 -8 21190.6 1279.76 2 -1 1 -9 2651.19 512.960 2 1 -1 9 3032.23 571.807 1 1 -1 10 9014.92 989.496 1 -1 1 -10 7877.24 871.671 2 1 -1 11 7101.71 921.566 1 -1 1 -11 5941.16 775.263 2 1 -1 12 16916.2 1881.00 14 1 -1 12 13415.6 1324.46 1 -1 1 -13 133505. 4963.01 7 1 -1 13 150971. 5751.84 14 1 -1 14-836.905 517.978 14 -1 1 -14-703.818 469.507 7 -1 1 -15 4027.95 961.398 7 1 -1 15 3447.01 881.069 14 -1 1 -16 1431.30 661.609 7 1 -1 16 1910.25 722.574 14 -1 1 -17 4700.66 1009.69 7 1 -1 17 3261.41 766.748 14 1 -1 18 6225.56 886.795 14 -1 1 -18 4612.05 869.405 7 -1 1 -19 1728.50 520.197 7 1 -1 19 2062.57 412.894 14 -1 1 -20 272.128 205.200 7 -1 0 20 455.364 210.140 14 -1 0 19 4807.32 705.360 14 1 0 -19 2523.19 515.674 7 1 0 -18 3234.84 657.626 7 -1 0 18 2927.09 687.786 14 -1 0 17 1694.40 523.691 14 1 0 -17 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2 -5 3 -2 20789.0 1570.71 9 -5 3 -3 8289.99 1235.12 2 5 -3 3 7174.98 949.059 8 -5 3 -4 16075.4 1688.21 2 5 -3 4 14196.5 1295.32 8 -5 3 -5 18483.2 1573.32 4 -5 3 -5 19888.0 1896.48 2 5 -3 5 15698.8 1350.90 8 -5 3 -6 44973.5 2454.09 4 -5 3 -6 43025.0 2812.76 2 5 -3 6 38570.7 2072.67 8 -5 3 -7 7725.53 1066.38 4 -5 3 -7 8246.97 1108.05 10 5 -3 7 6255.22 812.433 8 -5 3 -8 54974.4 2687.21 4 -5 3 -8 48847.8 2697.76 10 5 -3 8 47859.5 2288.49 8 -5 3 -9 1402.38 456.095 4 -5 3 -9 112.984 321.828 10 -5 3 -10 288.135 278.756 4 -5 3 -10-91.4422 378.544 10 -5 3 -11 63.7061 344.188 10 -5 3 -12 1256.95 545.655 10 -5 3 -13 3443.88 697.455 11 -5 3 -14 6736.01 867.047 11 -5 3 -15 9924.21 932.868 11 -5 3 -16 2929.30 421.406 11 -5 2 16 1842.11 362.911 6 -5 2 15 1420.88 350.960 14 -5 2 15 1048.27 362.926 6 -5 2 14 2360.49 522.612 14 -5 2 14 1941.81 553.737 6 -5 2 13 11315.5 1192.59 14 -5 2 12 2287.38 611.048 14 -5 2 12 1651.75 480.088 9 -5 2 11 3624.39 782.135 14 -5 2 11 3667.46 752.689 9 -5 2 10 24467.5 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16 -9 -4 -3 3434.74 605.475 6 -9 -4 -4 144.921 209.760 16 -9 -4 -4-41.7849 296.142 6 -9 -4 -5 41137.7 1707.99 16 -9 -4 -5 41108.8 2034.01 6 -9 -4 -6 4673.90 551.246 16 -9 -4 -6 5183.93 723.610 6 -9 -4 -7 7978.61 715.277 16 -9 -4 -8 207.788 142.733 16 -9 -4 -11-106.264 197.876 4 -9 -5 4 7725.80 734.067 5 -9 -5 3 2283.47 495.799 5 -9 -5 2 109.964 279.051 5 -9 -5 1 4586.80 751.433 5 -9 -5 0 3322.53 591.933 16 -9 -5 0-39.4039 296.372 5 -9 -5 -1-2.63242 208.501 16 -9 -5 -2 13128.0 1048.44 16 -9 -5 -3 10535.4 956.404 16 -9 -5 -4 3435.41 544.084 16 -9 -5 -5-83.1560 303.378 16 -9 -5 -6 20101.9 1258.81 16 -9 -5 -7 45845.8 1836.59 16 -9 -5 -8-278.613 262.015 16 -9 -5 -9 4386.34 554.553 16 -9 -5 -10 1068.09 277.402 16 -9 -5 -11 5745.04 509.333 16 -9 -6 0 7257.22 858.253 16 -9 -6 -1 1674.11 452.844 16 -9 -6 -2-338.403 308.319 16 -9 -6 -3 28561.3 1565.66 16 -9 -6 -4 22763.8 1394.12 16 -9 -6 -5 11035.3 973.527 16 -9 -6 -6-517.128 334.411 16 -9 -6 -7 2714.66 492.688 16 -9 -6 -8 974.547 305.655 16 -9 -6 -9 5264.84 613.916 16 -9 -6 -10-345.321 219.937 16 -9 -6 -11 474.457 192.013 16 -9 -7 -1 18075.2 1085.52 16 -9 -7 -2 7704.61 754.717 16 -9 -7 -3 4135.03 567.614 16 -9 -7 -4-250.923 282.023 16 -9 -7 -5 32.0076 197.890 16 -9 -7 -6 10157.3 848.767 16 -9 -7 -7 4131.54 543.922 16 -9 -7 -8 277.759 196.206 16 -9 -7 -9 1595.87 338.407 16 -10 -1 0 80.0311 126.379 6 -10 -1 -1 7.88992 155.500 6 -10 -1 -2 603.439 219.214 6 -10 -1 -3 924.028 243.527 6 -10 -1 -4-208.715 166.110 6 -10 -2 0 6038.05 591.721 6 -10 -2 -1 381.951 212.786 6 -10 -2 -2 1035.19 293.312 6 -10 -2 -3 9805.36 794.123 6 -10 -2 -4 97.6399 154.362 6 -10 -3 -1-129.357 163.357 6 -10 -3 -2 634.521 234.532 6 -10 -3 -3 768.037 263.424 6 -10 -3 -4 13601.4 946.274 6 0 0 0 0.00 0.00 0 TITL 20170104-c28-Al in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 8.144209 9.273638 17.177692 76.5251 80.0800 76.8075 ZERR 2.00 0.000367 0.000487 0.001015 0.0048 0.0044 0.0042 LATT 1 SFAC C H N O Al S UNIT 36.00 24.00 4.00 24.00 2.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 51454 _shelx_res_file ; TITL 20170104-c28-Al in P-1 #2 20170104-c28-al.res created by SHELXL-2018/3 at 16:20:52 on 13-Sep-2018 CELL 1.54184 8.1442 9.2736 17.1777 76.525 80.08 76.808 ZERR 2 0.0004 0.0005 0.001 0.005 0.004 0.004 LATT 1 SFAC C H Al N O S UNIT 36 50 2 4 34 4 EQIV $1 -X,2-Y,-Z EQIV $2 +X,1+Y,-1+Z EQIV $3 1-X,-Y,1-Z EQIV $4 -X,-Y,1-Z EQIV $5 +X,-1+Y,+Z EQIV $6 1-X,1-Y,1-Z EQIV $7 1-X,2-Y,-Z EQIV $8 -1+X,+Y,+Z DFIX 0.84 0.01 O12 H12b DFIX 0.84 0.01 O12 H12a DFIX 0.84 0.01 O13 H13b O13 H13a DFIX 0.84 0.01 O14 H14b O14 H14a DFIX 0.84 0.01 O15 H15b O15 H15a DFIX 0.84 H11 O11 DFIX 0.84 H17c O17 DFIX 0.84 H17d O17 DFIX 2.95 O2 O2_$7 DANG 1.33 0.02 H12b H12a DANG 1.33 0.02 H13b H13a DANG 1.33 0.02 H14b H14a DANG 1.33 0.02 H15b H15a DANG 1.33 0.02 H17c H17d L.S. 50 PLAN 20 TEMP -173 HTAB O13 O4 HTAB O17 O2 HTAB O12 O1_$1 HTAB O14 O16 HTAB O12 O10_$2 HTAB O14 O9_$3 HTAB O14 S2_$3 HTAB O15 O8_$4 HTAB O15 O3_$5 HTAB C1 O7_$6 HTAB O17 O1_$7 HTAB O13 O17_$8 HTAB O11 O16_$8 GRID BOND fmap 2 acta MERG 2 SHEL 999 0.84 OMIT -4 -8 8 OMIT -4 -8 7 REM REM REM WGHT 0.089000 FVAR 5.51172 S1 6 0.261521 1.012105 0.132932 11.00000 0.01642 0.01774 = 0.01049 0.00337 -0.00072 -0.00544 AL1 3 0.054356 0.566016 0.056260 11.00000 0.01794 0.01659 = 0.01049 0.00131 -0.00251 -0.00568 N1 4 0.163458 0.719017 0.341709 11.00000 0.02357 0.01993 = 0.01072 0.00432 0.00244 -0.00353 N2 4 0.270903 0.078117 0.655911 11.00000 0.01887 0.01624 = 0.01027 0.00351 -0.00303 -0.00280 O1 5 0.111911 1.020044 0.094281 11.00000 0.02003 0.02447 = 0.01778 0.00475 -0.00596 -0.00669 O2 5 0.417391 0.991211 0.077334 11.00000 0.01879 0.02693 = 0.01342 0.00326 0.00359 -0.00738 O3 5 0.243363 1.138893 0.172795 11.00000 0.03063 0.01725 = 0.01954 0.00119 -0.00543 -0.00510 O4 5 0.042260 0.592485 0.275379 11.00000 0.02435 0.02995 = 0.01094 0.00130 -0.00356 -0.00319 O5 5 0.297113 0.841828 0.404487 11.00000 0.03790 0.01697 = 0.02000 0.00306 0.00085 -0.00976 O6 5 0.180993 -0.057436 0.582740 11.00000 0.03470 0.01850 = 0.01660 0.00079 -0.00510 -0.01025 O7 5 0.353821 0.213228 0.731285 11.00000 0.02804 0.02456 = 0.01105 0.00185 -0.00573 -0.00776 O8 5 0.282100 -0.387588 0.769566 11.00000 0.02213 0.02283 = 0.01334 -0.00008 0.00039 -0.00909 O9 5 0.586631 -0.440505 0.776406 11.00000 0.02064 0.02259 = 0.01359 0.00078 0.00052 0.00051 O10 5 0.391212 -0.301495 0.870205 11.00000 0.02164 0.02387 = 0.00938 0.00174 -0.00112 -0.00568 O11 5 -0.139534 0.564754 0.013693 11.00000 0.01463 0.02111 = 0.01367 -0.00366 -0.00042 -0.00514 O12 5 0.107410 0.739322 -0.023523 11.00000 0.02084 0.01906 = 0.01080 0.00256 -0.00121 -0.00429 H12A 2 0.039494 0.815955 -0.043441 11.00000 -1.50000 H12B 2 0.187529 0.725248 -0.060792 11.00000 -1.50000 O13 5 -0.063349 0.695562 0.125261 11.00000 0.02756 0.02040 = 0.01035 -0.00024 -0.00347 -0.00113 H13A 2 -0.051418 0.673739 0.174357 11.00000 -1.50000 H13B 2 -0.131699 0.779226 0.117224 11.00000 -1.50000 O14 5 0.268188 0.554291 0.088937 11.00000 0.02058 0.02386 = 0.01325 0.00468 -0.00518 -0.01022 H14A 2 0.339965 0.608679 0.064934 11.00000 -1.50000 H14B 2 0.302097 0.515506 0.134115 11.00000 -1.50000 O15 5 0.026212 0.406229 0.147568 11.00000 0.01971 0.01783 = 0.01456 0.00427 -0.00041 -0.00634 H15A 2 -0.063188 0.388928 0.176773 11.00000 -1.50000 H15B 2 0.097491 0.324405 0.153772 11.00000 -1.50000 AFIX 6 O16 5 0.509611 0.709229 0.013764 11.00000 0.02287 0.02148 = 0.01698 -0.00250 -0.00413 -0.00542 H16A 2 0.494389 0.797988 0.022835 11.00000 -1.50000 H16B 2 0.502259 0.714810 -0.035696 11.00000 -1.50000 O17 5 0.762376 0.959621 0.081106 11.00000 0.01998 0.02660 = 0.01725 0.00086 -0.00086 -0.00529 AFIX 0 C1 1 0.282086 0.845296 0.208767 11.00000 0.02035 0.01355 = 0.01012 0.00626 -0.00025 -0.00271 AFIX 23 H1A 2 0.285652 0.757420 0.184596 11.00000 -1.20000 H1B 2 0.390434 0.829838 0.231127 11.00000 -1.20000 AFIX 0 C2 1 0.135151 0.853945 0.276598 11.00000 0.02227 0.02257 = 0.01305 0.00530 0.00263 -0.00070 AFIX 23 H2A 2 0.125485 0.946058 0.298176 11.00000 -1.20000 H2B 2 0.027509 0.860312 0.255449 11.00000 -1.20000 AFIX 0 C3 1 0.115208 0.589201 0.332029 11.00000 0.01866 0.02346 = 0.01079 0.00174 0.00271 -0.00449 C4 1 0.153777 0.451529 0.394797 11.00000 0.01864 0.02093 = 0.00909 0.00362 -0.00042 -0.00489 C5 1 0.218882 0.458922 0.464527 11.00000 0.01894 0.01893 = 0.00962 0.00196 -0.00021 -0.00700 C6 1 0.260306 0.595293 0.473155 11.00000 0.01914 0.01818 = 0.01418 0.00062 0.00175 -0.00254 C7 1 0.244825 0.728438 0.405533 11.00000 0.02375 0.02156 = 0.01347 0.00010 0.00378 -0.00555 C8 1 0.313674 0.602802 0.543555 11.00000 0.02106 0.01809 = 0.01961 -0.00399 0.00179 -0.00664 AFIX 43 H8 2 0.338679 0.694748 0.549198 11.00000 -1.20000 AFIX 0 C9 1 0.331758 0.475991 0.607408 11.00000 0.01961 0.02047 = 0.01255 -0.00458 -0.00088 -0.00427 AFIX 43 H9 2 0.367406 0.482897 0.656016 11.00000 -1.20000 AFIX 0 C10 1 0.297311 0.340819 0.599087 11.00000 0.01482 0.01947 = 0.01061 0.00214 0.00052 -0.00509 C11 1 0.241133 0.330760 0.527653 11.00000 0.01599 0.01776 = 0.01128 0.00048 -0.00094 -0.00408 C12 1 0.201913 0.195556 0.518498 11.00000 0.01785 0.01930 = 0.01107 0.00092 -0.00116 -0.00638 C13 1 0.142436 0.187755 0.449381 11.00000 0.02228 0.02440 = 0.01555 -0.00236 -0.00319 -0.00717 AFIX 43 H13 2 0.118773 0.095403 0.443560 11.00000 -1.20000 AFIX 0 C14 1 0.116898 0.317624 0.387348 11.00000 0.02385 0.02863 = 0.01057 -0.00229 -0.00327 -0.00728 AFIX 43 H14 2 0.074036 0.312842 0.340149 11.00000 -1.20000 AFIX 0 C15 1 0.217668 0.061248 0.585836 11.00000 0.02108 0.01857 = 0.01285 -0.00142 -0.00100 -0.00290 C16 1 0.312333 0.209297 0.667159 11.00000 0.01497 0.01921 = 0.01395 0.00081 -0.00121 -0.00591 C17 1 0.275419 -0.052491 0.724717 11.00000 0.01898 0.01958 = 0.01153 0.00558 -0.00009 -0.00666 AFIX 23 H17A 2 0.180420 -0.103456 0.725810 11.00000 -1.20000 H17B 2 0.259392 -0.015801 0.775735 11.00000 -1.20000 AFIX 0 C18 1 0.442863 -0.166012 0.719142 11.00000 0.01662 0.01645 = 0.01389 0.00319 -0.00109 -0.00514 H11 2 -0.237432 0.605430 0.023428 11.00000 -1.50000 H17C 2 0.658886 0.960626 0.085579 11.00000 -1.50000 H17D 2 0.793285 1.005019 0.036030 11.00000 -1.50000 S2 6 0.424249 -0.337443 0.789291 11.00000 0.01816 0.01707 = 0.00925 0.00200 -0.00127 -0.00387 H18A 2 0.532945 -0.137233 0.734131 11.00000 0.01766 H18B 2 0.474611 -0.197177 0.666643 11.00000 0.03311 HKLF 4 REM 20170104-c28-Al in P-1 #2 REM wR2 = 0.1473, GooF = S = 1.048, Restrained GooF = 1.058 for all data REM R1 = 0.0516 for 3439 Fo > 4sig(Fo) and 0.0711 for all 4284 data REM 402 parameters refined using 17 restraints END WGHT 0.0890 0.0000 REM Highest difference peak 0.564, deepest hole -0.740, 1-sigma level 0.097 Q1 1 0.4474 -0.2501 0.7460 11.00000 0.05 0.56 Q2 1 0.3803 0.8924 0.1165 11.00000 0.05 0.48 Q3 1 0.2525 0.9293 0.1788 11.00000 0.05 0.46 Q4 1 0.1025 0.6536 0.0131 11.00000 0.05 0.42 Q5 1 -0.1510 0.5245 -0.0161 11.00000 0.05 0.38 Q6 1 0.2956 0.0372 0.6674 11.00000 0.05 0.37 Q7 1 0.2619 0.5061 0.4577 11.00000 0.05 0.36 Q8 1 0.1660 1.0761 0.0735 11.00000 0.05 0.36 Q9 1 0.0480 0.4794 0.1022 11.00000 0.05 0.33 Q10 1 0.2707 -0.2318 0.8216 11.00000 0.05 0.33 Q11 1 0.2060 0.1391 0.5477 11.00000 0.05 0.33 Q12 1 0.3372 1.0857 0.0910 11.00000 0.05 0.32 Q13 1 0.1318 1.1490 0.1692 11.00000 0.05 0.31 Q14 1 -0.1201 0.7298 -0.0598 11.00000 0.05 0.31 Q15 1 0.2827 -0.4145 0.7587 11.00000 0.05 0.31 Q16 1 0.3286 -0.3716 0.7677 11.00000 0.05 0.30 Q17 1 0.3294 0.9335 0.3655 11.00000 0.05 0.30 Q18 1 0.5995 0.7990 -0.0370 11.00000 0.05 0.29 Q19 1 0.3580 -0.4227 0.8401 11.00000 0.05 0.28 Q20 1 0.2223 1.1058 0.1656 11.00000 0.05 0.28 ; _shelx_res_checksum 23254 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 0.26152(9) 1.01210(8) 0.13293(4) 0.0157(2) Uani d 1 Al Al1 0.05436(11) 0.56602(10) 0.05626(5) 0.0152(2) Uani d 1 N N1 0.1635(3) 0.7190(3) 0.34171(16) 0.0200(6) Uani d 1 N N2 0.2709(3) 0.0781(3) 0.65591(15) 0.0161(5) Uani d 1 O O1 0.1119(3) 1.0200(3) 0.09428(13) 0.0215(5) Uani d 1 O O2 0.4174(3) 0.9912(3) 0.07733(13) 0.0212(5) Uani d 1 O O3 0.2434(3) 1.1389(2) 0.17279(14) 0.0230(5) Uani d 1 O O4 0.0423(3) 0.5925(3) 0.27538(13) 0.0229(5) Uani d 1 O O5 0.2971(3) 0.8418(3) 0.40449(14) 0.0259(5) Uani d 1 O O6 0.1810(3) -0.0574(2) 0.58274(13) 0.0229(5) Uani d 1 O O7 0.3538(3) 0.2132(3) 0.73129(13) 0.0213(5) Uani d 1 O O8 0.2821(3) -0.3876(3) 0.76957(13) 0.0196(5) Uani d 1 O O9 0.5866(3) -0.4405(3) 0.77641(13) 0.0208(5) Uani d 1 O O10 0.3912(3) -0.3015(3) 0.87021(12) 0.0191(5) Uani d 1 O O11 -0.1395(3) 0.5648(2) 0.01369(13) 0.0163(4) Uani d 1 O O12 0.1074(3) 0.7393(3) -0.02352(13) 0.0179(5) Uani d 1 H H12A 0.039(4) 0.816(3) -0.043(2) 0.027 Uiso d 1 H H12B 0.188(3) 0.725(4) -0.0608(15) 0.027 Uiso d 1 O O13 -0.0633(3) 0.6956(3) 0.12526(13) 0.0204(5) Uani d 1 H H13A -0.051(5) 0.674(4) 0.1744(8) 0.031 Uiso d 1 H H13B -0.132(4) 0.779(2) 0.117(2) 0.031 Uiso d 1 O O14 0.2682(3) 0.5543(3) 0.08894(13) 0.0193(5) Uani d 1 H H14A 0.340(4) 0.609(4) 0.0649(18) 0.029 Uiso d 1 H H14B 0.302(4) 0.516(4) 0.1341(12) 0.029 Uiso d 1 O O15 0.0262(3) 0.4062(2) 0.14757(13) 0.0184(5) Uani d 1 H H15A -0.063(3) 0.389(4) 0.1768(19) 0.028 Uiso d 1 H H15B 0.097(3) 0.324(2) 0.154(2) 0.028 Uiso d 1 O O16 0.5096(3) 0.7092(2) 0.01376(13) 0.0203(5) Uani d 1 H H16A 0.494389 0.797988 0.022835 0.030 Uiso d 1 H H16B 0.502259 0.714810 -0.035696 0.030 Uiso d 1 O O17 0.7624(3) 0.9596(2) 0.08111(13) 0.0222(5) Uani d 1 C C1 0.2821(4) 0.8453(3) 0.20877(18) 0.0164(6) Uani d 1 H H1A 0.285652 0.757420 0.184596 0.020 Uiso calc 1 H H1B 0.390434 0.829838 0.231127 0.020 Uiso calc 1 C C2 0.1352(4) 0.8539(4) 0.27660(19) 0.0220(7) Uani d 1 H H2A 0.125485 0.946058 0.298176 0.026 Uiso calc 1 H H2B 0.027509 0.860312 0.255449 0.026 Uiso calc 1 C C3 0.1152(4) 0.5892(4) 0.33203(18) 0.0190(7) Uani d 1 C C4 0.1538(4) 0.4515(4) 0.39480(18) 0.0173(6) Uani d 1 C C5 0.2189(4) 0.4589(4) 0.46453(18) 0.0163(6) Uani d 1 C C6 0.2603(4) 0.5953(4) 0.47315(19) 0.0185(6) Uani d 1 C C7 0.2448(4) 0.7284(4) 0.40553(19) 0.0208(7) Uani d 1 C C8 0.3137(4) 0.6028(4) 0.54356(19) 0.0196(7) Uani d 1 H H8 0.338679 0.694748 0.549198 0.024 Uiso calc 1 C C9 0.3318(4) 0.4760(4) 0.60741(18) 0.0174(6) Uani d 1 H H9 0.367406 0.482897 0.656016 0.021 Uiso calc 1 C C10 0.2973(4) 0.3408(4) 0.59909(18) 0.0158(6) Uani d 1 C C11 0.2411(4) 0.3308(3) 0.52765(18) 0.0156(6) Uani d 1 C C12 0.2019(4) 0.1956(4) 0.51850(18) 0.0164(6) Uani d 1 C C13 0.1424(4) 0.1878(4) 0.44938(19) 0.0205(7) Uani d 1 H H13 0.118773 0.095403 0.443560 0.025 Uiso calc 1 C C14 0.1169(4) 0.3176(4) 0.38735(19) 0.0208(7) Uani d 1 H H14 0.074036 0.312842 0.340149 0.025 Uiso calc 1 C C15 0.2177(4) 0.0612(4) 0.58584(18) 0.0181(6) Uani d 1 C C16 0.3123(4) 0.2093(4) 0.66716(18) 0.0164(6) Uani d 1 C C17 0.2754(4) -0.0525(4) 0.72472(18) 0.0179(6) Uani d 1 H H17A 0.180420 -0.103456 0.725810 0.022 Uiso calc 1 H H17B 0.259392 -0.015801 0.775735 0.022 Uiso calc 1 C C18 0.4429(4) -0.1660(4) 0.71914(19) 0.0165(6) Uani d 1 H H11 -0.237(3) 0.605(4) 0.023(2) 0.025 Uiso d 1 H H17C 0.659(2) 0.961(4) 0.086(2) 0.025 Uiso d 1 H H17D 0.793(4) 1.005(4) 0.0360(14) 0.025 Uiso d 1 S S2 0.42425(9) -0.33744(8) 0.78929(4) 0.0156(2) Uani d 1 H H18A 0.533(5) -0.137(4) 0.734(2) 0.018(9) Uiso d 1 H H18B 0.475(5) -0.197(5) 0.667(3) 0.033(11) 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 S1 0.0164(4) 0.0177(4) 0.0105(4) -0.0054(3) -0.0007(3) 0.0034(3) Al1 0.0179(5) 0.0166(5) 0.0105(4) -0.0057(3) -0.0025(3) 0.0013(4) N1 0.0236(14) 0.0199(14) 0.0107(13) -0.0035(11) 0.0024(11) 0.0043(11) N2 0.0189(13) 0.0162(13) 0.0103(12) -0.0028(10) -0.0030(10) 0.0035(11) O1 0.0200(11) 0.0245(12) 0.0178(11) -0.0067(9) -0.0060(9) 0.0048(10) O2 0.0188(11) 0.0269(12) 0.0134(11) -0.0074(9) 0.0036(9) 0.0033(10) O3 0.0306(13) 0.0172(11) 0.0195(12) -0.0051(9) -0.0054(10) 0.0012(9) O4 0.0244(12) 0.0300(13) 0.0109(11) -0.0032(10) -0.0036(9) 0.0013(10) O5 0.0379(14) 0.0170(12) 0.0200(12) -0.0098(10) 0.0008(10) 0.0031(10) O6 0.0347(13) 0.0185(12) 0.0166(11) -0.0102(10) -0.0051(10) 0.0008(10) O7 0.0280(12) 0.0246(12) 0.0110(11) -0.0078(10) -0.0057(9) 0.0019(9) O8 0.0221(11) 0.0228(12) 0.0133(11) -0.0091(9) 0.0004(9) -0.0001(9) O9 0.0206(11) 0.0226(12) 0.0136(11) 0.0005(9) 0.0005(9) 0.0008(9) O10 0.0216(11) 0.0239(12) 0.0094(10) -0.0057(9) -0.0011(8) 0.0017(9) O11 0.0146(10) 0.0211(11) 0.0137(10) -0.0051(9) -0.0004(8) -0.0037(9) O12 0.0208(11) 0.0191(11) 0.0108(10) -0.0043(9) -0.0012(8) 0.0026(9) O13 0.0276(12) 0.0204(12) 0.0104(10) -0.0011(9) -0.0035(9) -0.0002(9) O14 0.0206(11) 0.0239(12) 0.0133(11) -0.0102(9) -0.0052(9) 0.0047(9) O15 0.0197(11) 0.0178(11) 0.0146(11) -0.0063(9) -0.0004(9) 0.0043(9) O16 0.0229(11) 0.0215(11) 0.0170(11) -0.0054(9) -0.0041(9) -0.0025(10) O17 0.0200(11) 0.0266(13) 0.0172(12) -0.0053(10) -0.0009(9) 0.0009(10) C1 0.0203(15) 0.0135(14) 0.0101(14) -0.0027(12) -0.0002(12) 0.0063(12) C2 0.0223(16) 0.0226(17) 0.0131(15) -0.0007(13) 0.0026(13) 0.0053(14) C3 0.0187(15) 0.0235(17) 0.0108(15) -0.0045(13) 0.0027(12) 0.0017(13) C4 0.0186(15) 0.0209(16) 0.0091(14) -0.0049(12) -0.0004(12) 0.0036(13) C5 0.0189(15) 0.0189(15) 0.0096(14) -0.0070(12) -0.0002(12) 0.0020(13) C6 0.0191(15) 0.0182(15) 0.0142(15) -0.0025(12) 0.0017(12) 0.0006(13) C7 0.0237(16) 0.0216(17) 0.0135(15) -0.0056(13) 0.0038(12) 0.0001(14) C8 0.0211(16) 0.0181(15) 0.0196(16) -0.0066(12) 0.0018(13) -0.0040(13) C9 0.0196(15) 0.0205(16) 0.0126(15) -0.0043(12) -0.0009(12) -0.0046(13) C10 0.0148(14) 0.0195(16) 0.0106(14) -0.0051(12) 0.0005(11) 0.0021(12) C11 0.0160(14) 0.0178(15) 0.0113(14) -0.0041(12) -0.0009(11) 0.0005(12) C12 0.0178(15) 0.0193(15) 0.0111(14) -0.0064(12) -0.0012(11) 0.0009(13) C13 0.0223(16) 0.0244(17) 0.0156(16) -0.0072(13) -0.0032(12) -0.0024(14) C14 0.0239(16) 0.0286(18) 0.0106(15) -0.0073(14) -0.0033(12) -0.0023(13) C15 0.0211(16) 0.0186(16) 0.0128(15) -0.0029(12) -0.0010(12) -0.0014(13) C16 0.0150(14) 0.0192(15) 0.0140(15) -0.0059(12) -0.0012(12) 0.0008(13) C17 0.0190(15) 0.0196(16) 0.0115(14) -0.0067(12) -0.0001(12) 0.0056(13) C18 0.0166(15) 0.0165(15) 0.0139(15) -0.0051(12) -0.0011(12) 0.0032(13) S2 0.0182(4) 0.0171(4) 0.0092(4) -0.0039(3) -0.0013(3) 0.0020(3) 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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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' S S 0.3331 0.5567 '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 O1 S1 C1 . . 107.48(14) O2 S1 O1 . . 110.80(13) O2 S1 O3 . . 113.80(14) O2 S1 C1 . . 104.82(14) O3 S1 O1 . . 112.33(14) O3 S1 C1 . . 107.06(14) O11 Al1 Al1 2_565 2_565 39.38(7) O11 Al1 Al1 . 2_565 39.13(7) O11 Al1 O11 2_565 . 78.51(11) O11 Al1 O12 2_565 . 92.95(10) O11 Al1 O12 . . 93.71(10) O11 Al1 O13 . . 93.43(11) O11 Al1 O13 2_565 . 171.71(11) O11 Al1 O14 2_565 . 94.18(11) O11 Al1 O14 . . 172.54(11) O11 Al1 O15 . . 96.20(10) O11 Al1 O15 2_565 . 93.42(11) O12 Al1 Al1 . 2_565 94.30(8) O13 Al1 Al1 . 2_565 132.53(9) O13 Al1 O12 . . 89.45(11) O13 Al1 O14 . . 93.93(11) O13 Al1 O15 . . 85.48(10) O14 Al1 Al1 . 2_565 133.54(9) O14 Al1 O12 . . 85.12(10) O14 Al1 O15 . . 85.63(10) O15 Al1 Al1 . 2_565 96.22(8) O15 Al1 O12 . . 169.12(11) C3 N1 C2 . . 116.8(3) C3 N1 C7 . . 125.5(3) C7 N1 C2 . . 117.6(3) C15 N2 C17 . . 116.7(3) C16 N2 C15 . . 125.5(3) C16 N2 C17 . . 117.8(2) Al1 O11 Al1 2_565 . 101.49(11) Al1 O11 H11 2_565 . 127(3) Al1 O11 H11 . . 131(3) Al1 O12 H12A . . 128(2) Al1 O12 H12B . . 118(2) H12A O12 H12B . . 105(2) Al1 O13 H13A . . 120(2) Al1 O13 H13B . . 133(2) H13A O13 H13B . . 107(2) Al1 O14 H14A . . 126(2) Al1 O14 H14B . . 129(2) H14A O14 H14B . . 104(2) Al1 O15 H15A . . 128(2) Al1 O15 H15B . . 121(2) H15A O15 H15B . . 107(2) H16A O16 H16B . . 109.3 H17C O17 H17D . . 109(3) S1 C1 H1A . . 109.3 S1 C1 H1B . . 109.3 H1A C1 H1B . . 108.0 C2 C1 S1 . . 111.6(2) C2 C1 H1A . . 109.3 C2 C1 H1B . . 109.3 N1 C2 C1 . . 110.1(3) N1 C2 H2A . . 109.6 N1 C2 H2B . . 109.6 C1 C2 H2A . . 109.6 C1 C2 H2B . . 109.6 H2A C2 H2B . . 108.1 N1 C3 C4 . . 116.6(3) O4 C3 N1 . . 120.8(3) O4 C3 C4 . . 122.5(3) C5 C4 C3 . . 120.1(3) C14 C4 C3 . . 119.9(3) C14 C4 C5 . . 120.0(3) C4 C5 C6 . . 121.1(3) C11 C5 C4 . . 120.0(3) C11 C5 C6 . . 118.9(3) C5 C6 C7 . . 119.3(3) C8 C6 C5 . . 120.1(3) C8 C6 C7 . . 120.6(3) N1 C7 C6 . . 116.5(3) O5 C7 N1 . . 120.5(3) O5 C7 C6 . . 122.9(3) C6 C8 H8 . . 119.6 C6 C8 C9 . . 120.9(3) C9 C8 H8 . . 119.6 C8 C9 H9 . . 120.1 C10 C9 C8 . . 119.8(3) C10 C9 H9 . . 120.1 C9 C10 C11 . . 120.4(3) C9 C10 C16 . . 119.4(3) C11 C10 C16 . . 120.2(3) C5 C11 C12 . . 118.8(3) C10 C11 C5 . . 119.9(3) C10 C11 C12 . . 121.4(3) C11 C12 C15 . . 119.4(3) C13 C12 C11 . . 121.1(3) C13 C12 C15 . . 119.4(3) C12 C13 H13 . . 120.2 C12 C13 C14 . . 119.7(3) C14 C13 H13 . . 120.2 C4 C14 C13 . . 120.5(3) C4 C14 H14 . . 119.7 C13 C14 H14 . . 119.7 N2 C15 C12 . . 116.9(3) O6 C15 N2 . . 120.3(3) O6 C15 C12 . . 122.7(3) N2 C16 C10 . . 116.6(3) O7 C16 N2 . . 120.3(3) O7 C16 C10 . . 123.0(3) N2 C17 H17A . . 109.2 N2 C17 H17B . . 109.2 N2 C17 C18 . . 111.8(2) H17A C17 H17B . . 107.9 C18 C17 H17A . . 109.2 C18 C17 H17B . . 109.2 C17 C18 S2 . . 109.8(2) C17 C18 H18A . . 114(2) C17 C18 H18B . . 114(2) S2 C18 H18A . . 103(2) S2 C18 H18B . . 104(2) H18A C18 H18B . . 110(3) O8 S2 O9 . . 113.01(14) O8 S2 O10 . . 112.30(13) O8 S2 C18 . . 105.80(14) O9 S2 O10 . . 112.56(13) O9 S2 C18 . . 105.65(14) O10 S2 C18 . . 106.85(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance S1 O1 . 1.465(2) S1 O2 . 1.451(2) S1 O3 . 1.461(2) S1 C1 . 1.770(3) Al1 Al1 2_565 2.8646(18) Al1 O11 . 1.855(2) Al1 O11 2_565 1.845(2) Al1 O12 . 1.932(2) Al1 O13 . 1.874(2) Al1 O14 . 1.893(2) Al1 O15 . 1.912(2) N1 C2 . 1.474(4) N1 C3 . 1.401(4) N1 C7 . 1.404(4) N2 C15 . 1.399(4) N2 C16 . 1.397(4) N2 C17 . 1.481(4) O4 C3 . 1.216(4) O5 C7 . 1.216(4) O6 C15 . 1.220(4) O7 C16 . 1.217(4) O8 S2 . 1.458(2) O9 S2 . 1.460(2) O10 S2 . 1.470(2) O11 H11 . 0.804(19) O12 H12A . 0.838(10) O12 H12B . 0.843(10) O13 H13A . 0.838(10) O13 H13B . 0.843(10) O14 H14A . 0.849(10) O14 H14B . 0.842(10) O15 H15A . 0.835(10) O15 H15B . 0.841(10) O16 H16A . 0.8506 O16 H16B . 0.8510 O17 H17C . 0.834(18) O17 H17D . 0.821(18) C1 H1A . 0.9900 C1 H1B . 0.9900 C1 C2 . 1.521(4) C2 H2A . 0.9900 C2 H2B . 0.9900 C3 C4 . 1.477(4) C4 C5 . 1.413(4) C4 C14 . 1.381(5) C5 C6 . 1.427(4) C5 C11 . 1.410(4) C6 C7 . 1.483(4) C6 C8 . 1.374(5) C8 H8 . 0.9500 C8 C9 . 1.409(5) C9 H9 . 0.9500 C9 C10 . 1.389(4) C10 C11 . 1.410(4) C10 C16 . 1.479(4) C11 C12 . 1.411(4) C12 C13 . 1.380(4) C12 C15 . 1.487(4) C13 H13 . 0.9500 C13 C14 . 1.411(5) C14 H14 . 0.9500 C17 H17A . 0.9900 C17 H17B . 0.9900 C17 C18 . 1.524(4) C18 S2 . 1.777(3) C18 H18A . 0.93(4) C18 H18B . 0.98(4) 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 O12 H12A O1 2_575 0.837(10) 1.869(11) 2.704(3) 176(4) yes O12 H12B O10 1_564 0.842(10) 1.868(12) 2.699(3) 169(4) yes O13 H13A O4 . 0.837(10) 1.935(14) 2.747(3) 163(3) yes O13 H13B O17 1_455 0.843(10) 1.72(9) 2.55(8) 167(5) yes O14 H14A O16 . 0.849(10) 1.827(11) 2.674(3) 175(4) yes O14 H14B O9 2_656 0.840(10) 1.833(13) 2.664(3) 169(3) yes O14 H14B S2 2_656 0.840(10) 2.78(2) 3.499(2) 144(3) yes O15 H15A O8 2_556 0.835(10) 1.862(12) 2.686(3) 169(3) yes O15 H15B O3 1_545 0.841(10) 1.848(11) 2.688(3) 176(3) yes C1 H1B O7 2_666 0.99 2.21 3.194(4) 173.7 yes O11 H11 O16 1_455 0.808(19) 2.08(2) 2.866(3) 163(4) yes O17 H17C O2 . 0.831(18) 1.95(2) 2.768(3) 169(3) yes O17 H17D O1 2_675 0.818(18) 2.29(3) 2.987(3) 144(4) yes _cod_database_fobs_code 2021727