#------------------------------------------------------------------------------ #$Date: 2024-07-13 05:00:09 +0300 (Sat, 13 Jul 2024) $ #$Revision: 293407 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023198.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_2023198 loop_ _publ_author_name 'Vashchenko, Oleksandr V.' 'Khomenko, Dmytro M.' 'Doroshchuk, Roman O.' 'Stoica, Alexandru-Constantin' 'Vassilyeva, Olga Yu.' 'Lampeka, Rostyslav D.' _publ_section_title ; Crystal structure of catena-poly[[methanoldioxidouranium(VI)]-\m-2-[5-(2-oxidophenyl)-1H-1,2,4-triazol-3-yl]acetato-\k2 O:O′] ; _journal_coeditor_code EJ2005 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024006637 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac '[U (C10 H7 N3 O3) O2 (C H4 O)]' _chemical_formula_moiety 'C11 H11 N3 O6 U' _chemical_formula_sum 'C11 H11 N3 O6 U' _chemical_formula_weight 519.26 _chemical_name_systematic catena-Poly[[methanoldioxidouranium(VI)]-\m-2-[5-(2-oxidophenyl)-1H-1,2,4-triazol-3-yl]acetato-\k^2^O:O'] _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.9966(6) _cell_length_b 13.7147(10) _cell_length_c 17.9345(9) _cell_measurement_reflns_used 2366 _cell_measurement_temperature 200.00(10) _cell_measurement_theta_max 30.7120 _cell_measurement_theta_min 2.6210 _cell_volume 2704.8(3) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2023) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2023) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2023) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 200.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0797 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_unetI/netI 0.0496 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 6980 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 2.271 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 12.034 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.50319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2023) ; _exptl_crystal_colour 'clear light red' _exptl_crystal_density_diffrn 2.550 _exptl_crystal_description prism _exptl_crystal_F_000 1904 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.077 _refine_diff_density_min -0.816 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 194 _refine_ls_number_reflns 2380 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0331 _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^)+(0.0147P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.0561 _reflns_number_gt 1904 _reflns_number_total 2380 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ej2005.cif _cod_data_source_block I _cod_database_code 2023198 _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 0.265 _shelx_estimated_absorpt_t_max 0.379 _shelx_hkl_file ; 0 0 2 3686.90 27.47 0 0 3 1.33 1.38 0 0 4 3141.65 36.63 0 0 5 -0.71 1.74 0 0 6 14.54 3.04 0 0 7 -0.19 1.69 0 0 8 867.96 27.44 0 0 9 0.92 2.28 0 0 10 1425.66 40.38 0 0 11 1.04 3.91 0 0 12 1119.95 39.94 0 0 13 13.71 5.51 0 0 13 2.68 3.91 0 0 14 1291.43 43.94 0 0 14 1285.29 47.49 0 0 15 3.33 5.68 0 0 15 4.95 4.76 0 0 16 1041.84 44.59 0 0 16 1058.18 46.83 0 0 17 7.46 6.19 0 0 17 4.44 6.76 0 0 18 376.73 30.50 0 0 19 4.91 5.90 0 0 20 105.32 18.11 0 0 21 -8.24 7.56 0 0 22 25.25 10.69 0 0 23 13.15 9.24 0 0 24 127.22 22.26 0 0 25 23.54 12.74 0 0 26 224.15 31.38 0 0 27 8.16 9.38 0 -1 1 6.01 1.66 0 1 -1 5.18 1.51 0 1 -2 2.96 0.91 0 -1 2 4.00 1.16 0 -1 2 7.04 1.98 0 1 -2 2.47 1.46 0 -1 3 1.29 0.98 0 1 -3 1.18 0.97 0 -1 3 1.70 1.62 0 -1 4 5.07 2.57 0 -1 4 2.01 1.51 0 1 -4 3.18 1.59 0 1 -5 2.19 1.85 0 -1 5 1.77 1.43 0 -1 6 4.73 2.34 0 -1 7 5.15 2.90 0 -1 8 1.17 2.27 0 -1 9 2.40 2.80 0 1 9 0.56 2.66 0 -1 9 -4.07 2.95 0 -1 10 8.74 3.80 0 1 10 8.12 3.90 0 -1 10 13.45 5.31 0 1 11 3.89 4.15 0 -1 11 5.18 3.73 0 -1 11 3.67 4.40 0 -1 12 4.29 4.61 0 -1 12 3.70 3.74 0 1 12 8.21 4.14 0 -1 13 -2.72 3.04 0 1 13 1.27 3.80 0 -1 13 -5.38 3.90 0 1 14 13.40 7.20 0 -1 14 4.71 5.44 0 -1 14 12.22 7.24 0 1 15 6.41 5.79 0 -1 15 2.87 5.46 0 -1 15 2.09 3.79 0 1 15 3.79 4.92 0 -1 16 18.22 8.74 0 1 16 13.70 8.38 0 1 16 17.31 7.62 0 -1 16 12.23 7.56 0 -1 17 4.81 4.49 0 -1 17 5.62 6.44 0 1 17 -0.52 5.23 0 -1 18 9.51 6.54 0 -1 18 2.33 6.35 0 1 18 8.97 8.22 0 -1 19 13.03 8.14 0 1 19 6.73 5.13 0 -1 20 -1.98 6.70 0 1 20 13.37 8.46 0 1 21 1.16 6.46 0 -1 21 -9.94 7.62 0 1 22 20.19 9.75 0 -1 22 -1.00 6.28 0 -1 23 4.16 6.49 0 1 23 3.11 8.41 0 -1 24 14.23 9.99 0 1 24 8.92 9.18 0 -1 25 13.46 9.16 0 1 25 20.05 13.36 0 1 26 15.14 13.20 0 -1 26 6.94 8.14 0 -1 27 24.73 14.98 0 2 0 9999.00 83.27 0 -2 0 9990.08 80.51 0 -2 -1 8.72 2.52 0 2 -1 12.27 3.34 0 2 1 9.52 2.58 0 -2 1 8.18 2.53 0 -2 2 4138.46 52.88 0 2 2 4070.91 40.52 0 2 -2 4256.36 36.97 0 2 -2 4330.68 53.45 0 -2 3 7.68 3.19 0 -2 3 10.53 2.22 0 2 -3 11.11 3.25 0 2 -3 10.72 2.15 0 -2 4 2351.83 42.50 0 -2 4 2301.09 31.75 0 2 -4 2301.34 31.78 0 -2 5 60.35 5.65 0 -2 5 52.73 6.99 0 2 -5 64.23 5.80 0 -2 6 134.24 11.39 0 -2 6 170.70 10.33 0 -2 7 511.46 23.38 0 -2 7 482.27 18.56 0 -2 8 289.29 18.35 0 -2 8 326.73 16.39 0 -2 9 232.63 14.79 0 -2 9 213.53 16.59 0 -2 10 890.45 35.40 0 -2 10 896.39 30.84 0 -2 11 380.28 21.45 0 -2 11 414.40 25.25 0 2 12 1479.58 48.64 0 -2 12 1429.61 48.93 0 -2 12 1537.46 45.16 0 2 13 111.29 14.33 0 -2 13 128.41 14.38 0 -2 13 118.76 15.17 0 -2 14 1451.18 48.64 0 2 14 1459.04 52.42 0 -2 14 1460.57 54.60 0 -2 15 3.70 5.25 0 -2 15 5.38 5.13 0 2 15 1.67 6.49 0 2 16 1334.50 43.46 0 -2 16 1337.97 57.36 0 -2 16 1379.44 51.47 0 2 16 1340.12 54.72 0 -2 17 57.18 11.78 0 -2 17 70.33 14.06 0 2 17 67.09 14.19 0 -2 18 204.20 22.04 0 2 18 208.39 23.17 0 -2 18 194.53 24.36 0 -2 19 93.00 16.10 0 2 19 121.55 18.94 0 2 20 46.70 13.11 0 -2 20 64.37 14.56 0 -2 21 56.87 13.85 0 2 21 70.75 16.94 0 -2 22 26.24 11.43 0 2 22 1.37 8.46 0 -2 23 60.52 15.76 0 2 23 73.05 18.29 0 -2 24 99.20 20.16 0 2 24 144.33 24.32 0 2 25 18.03 11.34 0 -2 25 23.47 10.80 0 -2 26 257.99 33.17 0 2 26 257.04 34.39 0 -3 0 8.66 3.76 0 3 0 10.08 4.48 0 -3 1 4.19 3.17 0 -3 -1 1.81 2.48 0 3 1 4.37 3.52 0 3 -1 4.09 2.93 0 -3 -2 7.80 3.29 0 3 -2 3.58 2.94 0 -3 2 -1.44 2.23 0 3 2 1.89 1.63 0 3 3 0.41 1.27 0 -3 3 -0.28 3.07 0 3 -3 1.37 1.66 0 3 -3 -0.77 2.44 0 3 4 0.10 1.47 0 -3 4 2.90 2.71 0 3 -4 2.46 1.70 0 -3 5 -0.49 1.58 0 -3 5 -0.41 2.68 0 3 -5 1.68 1.83 0 -3 6 -1.22 1.64 0 -3 6 -0.61 3.36 0 -3 7 3.06 3.59 0 -3 7 3.66 1.94 0 -3 8 5.32 5.09 0 -3 8 -0.61 2.42 0 -3 9 2.37 3.20 0 -3 9 7.29 5.04 0 -3 10 6.45 3.47 0 -3 10 3.76 4.55 0 -3 11 7.29 5.93 0 -3 11 5.19 4.08 0 -3 12 12.25 5.86 0 -3 12 2.87 6.21 0 -3 13 -2.36 3.45 0 -3 13 2.68 3.87 0 -3 14 16.01 7.02 0 -3 14 16.55 9.12 0 3 14 16.44 8.76 0 -3 15 10.98 8.24 0 3 15 -4.58 5.43 0 -3 15 3.32 4.85 0 -3 16 22.59 9.95 0 -3 16 3.40 7.23 0 3 16 17.80 9.55 0 -3 17 -4.39 6.84 0 3 17 0.90 4.67 0 -3 17 8.49 7.19 0 -3 18 -4.12 6.47 0 -3 18 5.37 7.53 0 3 18 -2.00 6.38 0 -3 19 5.43 5.65 0 -3 19 2.53 5.53 0 3 19 7.96 9.06 0 3 20 -4.71 7.00 0 -3 20 0.59 4.81 0 -3 21 21.94 11.45 0 3 21 -11.78 10.64 0 -3 22 -0.08 6.42 0 3 22 9.63 11.58 0 3 23 7.98 12.61 0 -3 23 14.18 9.80 0 3 24 8.21 11.32 0 -3 24 21.27 12.33 0 3 25 -0.90 8.34 0 -3 25 15.26 10.47 0 3 26 28.57 17.13 0 4 0 894.52 34.60 0 -4 0 804.30 31.64 0 4 1 2.92 2.69 0 -4 -1 3.93 3.70 0 -4 1 -2.01 4.82 0 4 2 3078.08 58.68 0 -4 2 2931.13 63.24 0 -4 -2 2865.79 53.62 0 -4 3 641.75 29.64 0 -4 -3 686.12 24.21 0 4 3 663.92 25.22 0 -4 4 935.24 36.07 0 4 4 872.76 27.46 0 4 -4 855.90 23.76 0 -4 5 479.34 26.32 0 4 5 456.79 18.83 0 4 6 110.40 9.07 0 -4 6 106.30 13.06 0 4 7 1166.29 28.94 0 -4 7 1157.79 31.02 0 -4 7 1088.40 42.16 0 -4 8 3.68 3.10 0 -4 8 4.95 2.01 0 -4 9 1176.03 34.37 0 -4 9 1147.81 45.79 0 -4 10 585.43 25.57 0 -4 10 583.08 33.95 0 -4 11 670.52 28.83 0 -4 11 772.19 40.23 0 -4 12 1498.81 58.22 0 -4 12 1389.79 43.62 0 -4 13 126.82 14.14 0 -4 13 130.18 18.54 0 -4 14 1288.38 58.46 0 -4 14 1261.78 45.76 0 4 15 23.82 9.39 0 -4 15 25.63 8.09 0 -4 15 2.45 6.31 0 4 16 1183.47 53.91 0 -4 16 1059.78 58.31 0 -4 16 1110.48 46.51 0 -4 17 129.34 21.48 0 4 17 141.89 20.28 0 -4 17 148.08 18.24 0 -4 18 123.58 20.91 0 -4 18 116.39 17.16 0 4 18 164.64 22.10 0 -4 19 253.88 25.20 0 4 19 219.22 27.07 0 -4 19 236.09 30.81 0 -4 20 26.32 10.86 0 4 20 14.29 9.28 0 4 21 225.09 28.63 0 -4 21 233.00 26.38 0 4 22 33.62 13.15 0 -4 22 50.00 13.80 0 4 23 127.60 23.45 0 -4 23 121.56 20.58 0 4 24 62.54 18.31 0 -4 24 57.34 15.55 0 4 25 43.86 16.90 0 -5 0 1.95 4.74 0 -5 1 5.02 5.25 0 -5 -1 7.44 4.92 0 -5 -2 -2.80 2.49 0 -5 2 6.43 5.29 0 -5 -3 4.50 4.68 0 -5 3 3.28 3.27 0 -5 4 6.73 4.32 0 -5 5 0.05 4.38 0 5 5 3.05 2.74 0 -5 6 -2.52 4.94 0 5 6 1.24 3.16 0 -5 6 1.14 0.89 0 5 7 4.37 3.32 0 -5 7 -0.96 4.28 0 -5 8 -7.21 6.89 0 5 8 -0.70 2.28 0 -5 9 6.43 6.71 0 -5 9 5.89 3.80 0 5 9 5.15 3.18 0 5 10 2.20 1.91 0 -5 10 -3.71 5.80 0 -5 10 0.85 2.45 0 -5 11 -1.88 5.25 0 -5 11 3.99 4.05 0 -5 12 2.08 4.98 0 -5 12 -0.96 5.32 0 -5 13 -4.59 4.04 0 -5 13 0.32 5.67 0 -5 14 -1.38 5.28 0 -5 14 -2.96 4.01 0 -5 15 -0.73 4.00 0 -5 15 -6.15 7.30 0 -5 16 8.97 9.55 0 -5 16 6.72 6.81 0 -5 17 3.59 6.70 0 -5 17 14.89 10.01 0 5 17 -6.29 7.74 0 -5 18 1.09 6.07 0 5 18 -3.45 7.36 0 -5 18 9.10 10.24 0 5 19 7.06 8.28 0 -5 19 14.16 12.46 0 -5 19 14.21 8.45 0 -5 20 21.88 10.36 0 5 20 13.43 10.31 0 -5 20 5.17 8.72 0 5 21 1.89 9.08 0 -5 21 1.19 7.81 0 5 22 1.35 9.52 0 -5 22 21.29 10.65 0 5 23 -2.35 9.16 0 -5 23 -4.39 7.09 0 5 24 5.70 12.34 0 5 25 34.54 15.72 0 -6 0 824.33 38.16 0 -6 1 91.25 13.84 0 -6 -1 82.22 12.43 0 -6 -2 672.44 33.08 0 -6 2 681.92 36.61 0 -6 3 589.04 34.31 0 -6 -3 573.89 29.28 0 -6 4 235.20 22.36 0 -6 -4 232.59 17.86 0 -6 5 1830.27 62.40 0 -6 6 12.21 5.92 0 -6 7 1357.05 55.41 0 -6 7 1241.70 17.62 0 -6 8 1.25 1.35 0 -6 8 -7.75 6.59 0 -6 9 1569.23 62.75 0 -6 10 339.96 30.29 0 -6 11 623.04 41.27 0 -6 12 564.08 41.54 0 -6 13 143.72 15.37 0 -6 13 161.92 23.13 0 -6 14 608.91 32.89 0 -6 14 641.04 46.52 0 -6 15 66.96 16.02 0 -6 15 66.79 11.79 0 -6 16 313.59 24.93 0 -6 16 333.13 36.19 0 -6 17 180.15 20.38 0 -6 17 202.01 28.96 0 -6 18 172.73 27.84 0 6 18 147.56 22.27 0 -6 18 150.60 19.75 0 6 19 440.55 38.29 0 -6 19 432.45 32.88 0 -6 19 386.41 43.20 0 -6 20 12.77 9.70 0 -6 20 1.02 5.44 0 6 20 7.53 9.13 0 -6 21 385.14 33.06 0 6 21 443.32 41.48 0 6 22 2.99 8.79 0 -6 22 20.05 9.92 0 6 23 198.18 29.47 0 6 24 49.92 17.35 0 6 25 109.77 24.69 0 -7 0 8.60 7.04 0 -7 1 -1.06 4.93 0 -7 -1 0.23 4.15 0 -7 2 3.69 6.30 0 -7 -2 2.80 3.60 0 -7 -3 1.15 3.78 0 -7 3 4.74 4.33 0 -7 -4 2.60 4.05 0 -7 4 -3.52 4.53 0 -7 5 -0.24 5.43 0 -7 6 5.14 5.30 0 -7 7 17.99 9.46 0 -7 8 1.92 6.56 0 -7 9 2.95 7.89 0 -7 9 2.01 1.34 0 -7 10 1.50 6.30 0 -7 11 -0.48 6.50 0 -7 12 12.00 8.13 0 -7 13 -7.89 6.17 0 -7 14 -5.92 6.06 0 -7 15 13.51 14.30 0 -7 16 -10.25 8.50 0 -7 17 -10.99 7.83 0 -7 18 4.80 10.01 0 7 19 3.08 8.14 0 -7 19 11.16 7.87 0 7 20 15.02 13.91 0 -7 20 22.72 13.41 0 7 21 -8.60 9.90 0 7 22 8.46 8.68 0 7 23 36.52 16.33 0 7 24 22.46 14.25 0 -8 0 196.58 21.63 0 -8 1 300.96 26.80 0 -8 -1 297.15 25.92 0 -8 2 234.94 24.24 0 -8 -2 177.50 20.03 0 -8 -3 1240.60 50.47 0 -8 3 1393.98 59.12 0 -8 -4 37.28 9.45 0 -8 4 76.10 14.85 0 -8 5 2366.31 80.78 0 -8 6 9.19 6.58 0 -8 7 1479.93 66.15 0 -8 8 25.97 9.69 0 -8 9 812.06 50.53 0 -8 10 40.13 13.13 0 -8 11 367.97 35.69 0 -8 12 66.56 15.39 0 -8 13 134.33 23.00 0 -8 14 171.14 25.60 0 -8 15 25.96 12.35 0 -8 16 15.08 12.89 0 -8 17 154.30 27.41 0 -8 18 36.84 15.47 0 -8 19 429.66 47.64 0 8 20 3.58 8.51 0 -8 20 -0.19 9.43 0 8 21 470.88 44.45 0 -8 21 446.57 50.54 0 8 22 0.04 8.62 0 8 23 324.38 39.18 0 -9 0 6.31 5.98 0 -9 1 -3.50 4.03 0 -9 -1 5.50 6.20 0 -9 2 11.82 7.87 0 -9 -2 1.01 3.91 0 -9 -3 -2.16 3.68 0 -9 3 1.45 6.47 0 -9 4 -3.75 6.09 0 -9 -4 8.33 6.17 0 -9 5 2.44 6.43 0 -9 6 2.47 5.23 0 -9 7 1.10 6.38 0 -9 8 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2 84.00 17.50 -13 3 -2 92.85 20.48 -13 3 2 75.70 17.64 -13 3 -3 87.53 19.32 -13 -3 3 101.78 20.25 -13 3 3 84.91 19.46 -13 -3 4 396.05 36.92 -13 3 4 430.44 41.94 -13 -3 5 15.26 8.36 -13 3 5 27.59 13.84 -13 -3 6 507.82 41.65 -13 3 6 498.99 46.70 -13 -3 7 15.91 10.93 -13 3 7 22.34 12.96 -13 -3 8 447.73 39.93 -13 3 8 458.24 44.92 -13 -3 9 37.30 14.00 -13 3 9 4.50 7.66 -13 -3 10 252.47 30.53 -13 3 10 209.89 32.54 -13 3 11 28.10 11.92 -13 -3 11 70.05 17.66 -13 3 11 96.58 24.23 -13 3 12 131.99 24.74 -13 -3 12 97.96 20.91 -13 3 12 100.46 25.43 -13 3 13 109.36 23.27 -13 -3 13 91.30 19.85 -13 3 13 123.61 28.25 -13 3 14 -4.27 7.73 -13 -3 14 -7.79 7.32 -13 3 14 -0.20 13.37 -13 3 15 89.72 23.23 -13 -3 15 60.84 17.34 -13 4 0 -8.43 10.56 -13 4 -1 3.11 9.86 -13 4 1 2.01 9.03 -13 -4 2 1.53 8.68 -13 4 -2 13.85 13.06 -13 4 2 6.47 8.39 -13 -4 3 6.08 8.52 -13 4 -3 13.41 13.07 -13 4 3 12.76 11.43 -13 4 -4 4.19 10.77 -13 -4 4 2.08 6.66 -13 4 4 1.98 8.61 -13 -4 5 21.53 8.15 -13 4 5 5.96 10.05 -13 -4 6 8.10 6.27 -13 4 6 12.79 13.81 -13 -4 7 -4.25 7.17 -13 4 7 -6.96 7.96 -13 -4 8 34.43 13.28 -13 4 8 9.56 10.27 -13 4 9 8.57 9.44 -13 -4 9 17.41 10.63 -13 4 9 7.79 7.87 -13 4 10 6.43 9.74 -13 -4 10 5.78 7.95 -13 4 10 7.91 10.95 -13 4 11 9.42 7.53 -13 -4 11 1.85 6.74 -13 4 12 12.00 12.43 -13 -4 12 19.07 11.19 -13 4 12 -18.06 14.29 -13 4 13 1.53 9.09 -13 -4 13 19.56 12.99 -13 4 13 16.40 13.90 -13 4 14 10.90 11.70 -13 4 15 13.26 12.70 -13 5 0 11.15 12.69 -13 5 -1 390.96 41.26 -13 5 1 409.43 41.80 -13 5 -2 71.80 19.22 -13 5 2 60.80 18.07 -13 5 3 269.16 35.73 -13 -5 3 245.38 28.73 -13 5 -3 251.01 33.53 -13 5 -4 134.69 24.64 -13 -5 4 183.58 24.51 -13 5 4 184.27 30.58 -13 -5 5 70.70 17.78 -13 5 5 32.50 13.69 -13 -5 6 281.19 31.30 -13 5 6 279.05 37.09 -13 -5 7 -4.95 7.76 -13 5 7 5.91 11.76 -13 -5 8 311.54 32.55 -13 5 8 281.81 37.64 -13 -5 9 75.47 17.97 -13 5 9 47.79 17.65 -13 -5 10 151.16 23.37 -13 5 10 129.76 26.54 -13 5 11 176.01 27.66 -13 -5 11 143.91 23.43 -13 5 11 175.70 31.93 -13 5 12 103.86 22.02 -13 5 12 66.11 22.23 -13 5 13 202.05 30.74 -13 5 14 11.18 13.44 -13 5 15 181.97 31.71 -13 6 0 3.49 8.45 -13 6 -1 8.56 11.30 -13 6 1 11.32 9.15 -13 6 -2 13.75 12.51 -13 6 2 6.18 8.68 -13 6 -3 33.72 14.66 -13 6 3 26.70 16.02 -13 6 -4 19.36 13.60 -13 6 4 4.45 8.87 -13 -6 5 -10.26 8.51 -13 6 5 17.09 10.94 -13 -6 6 9.28 8.47 -13 6 6 -1.27 11.08 -13 -6 7 2.67 7.57 -13 6 7 -1.23 9.42 -13 -6 8 13.59 8.45 -13 6 8 9.76 10.56 -13 -6 9 -2.24 7.01 -13 6 9 2.54 9.70 -13 6 10 15.77 13.47 -13 6 11 15.13 13.99 -13 6 12 16.74 14.03 -13 6 13 24.64 15.29 -13 6 14 24.01 15.37 -13 6 15 18.71 13.91 -13 7 0 18.34 13.95 -13 7 -1 421.84 44.27 -13 7 1 502.38 47.68 -13 7 -2 74.34 20.08 -13 7 2 51.91 18.69 -13 7 -3 341.73 40.27 -13 7 3 360.05 42.03 -13 7 -4 68.48 21.34 -13 7 4 49.32 18.08 -13 7 -5 82.00 19.96 -13 7 5 55.29 16.29 -13 7 6 84.26 21.94 -13 -7 7 1.52 6.69 -13 7 7 -1.43 10.85 -13 7 8 161.78 29.70 -13 7 9 98.25 24.84 -13 7 10 25.65 15.75 -13 7 11 262.30 39.01 -13 8 0 -8.70 9.25 -13 8 -1 42.78 16.04 -13 8 1 24.05 12.61 -13 8 -2 0.71 8.52 -13 8 2 -0.51 12.24 -13 8 -3 -4.31 8.02 -13 8 3 23.71 16.05 -13 8 -4 0.29 10.98 -13 8 4 32.47 15.41 -13 8 -5 15.16 14.07 -13 8 5 -0.21 10.91 -13 8 6 -8.13 11.12 -13 8 7 7.25 12.10 -13 8 8 10.07 13.81 -13 8 9 -4.93 11.10 -13 9 0 16.93 16.07 -13 9 -1 495.10 49.42 -13 9 1 408.10 45.35 -13 9 -2 29.95 15.03 -13 9 2 11.84 11.93 -13 9 -3 234.30 35.26 -13 9 3 198.46 31.88 -13 9 -4 8.91 12.86 -13 9 4 21.76 16.37 -13 9 -5 108.61 23.44 -13 9 5 124.69 25.97 -13 9 6 29.40 18.54 -13 9 7 -14.68 12.36 -13 9 8 12.89 14.89 -13 -10 0 12.91 11.27 -13 10 0 0.77 10.21 -13 -10 1 12.93 10.13 -13 10 -1 22.48 14.53 -13 10 1 -1.44 9.82 -13 10 -2 1.17 12.88 -13 10 2 -0.25 11.28 -13 10 -3 -2.05 12.33 -13 10 3 19.57 13.46 -13 10 -4 -0.43 12.03 -13 10 4 -2.16 9.69 -13 10 -5 4.87 10.74 -13 10 5 3.33 9.98 -13 10 6 14.28 11.27 -13 10 7 27.27 14.57 -13 -11 0 16.76 12.50 -13 11 0 15.59 11.88 -13 11 -1 423.03 47.16 -13 11 1 381.36 45.15 -13 -11 1 353.72 40.86 -13 -11 2 7.89 10.09 -13 11 -2 1.13 11.73 -13 11 2 15.64 14.04 -13 -11 3 126.91 24.67 -13 11 -3 182.63 31.29 -13 11 3 190.37 33.56 -13 -11 4 28.89 15.47 -13 11 -4 -4.21 10.92 -13 11 4 9.12 9.52 -13 -11 5 77.57 22.52 -13 11 5 106.76 25.35 -13 -11 6 35.43 17.26 -13 12 0 5.09 9.81 -13 -12 1 4.73 12.78 -13 12 -1 9.56 11.68 -13 12 1 2.62 9.90 -13 -12 2 30.34 16.99 -13 12 -2 -20.18 13.64 -13 12 2 34.49 17.91 -13 -12 3 38.92 16.79 -13 12 -3 22.20 16.01 -13 -12 4 16.34 12.22 -13 12 -4 2.13 9.15 -13 13 -2 6.39 9.98 -14 0 0 67.38 18.50 -14 0 -1 11.25 11.90 -14 0 1 -9.44 8.27 -14 0 2 74.69 18.57 -14 0 3 -2.09 9.46 -14 0 4 19.33 9.45 -14 0 5 -2.32 11.39 -14 0 6 -11.19 9.74 -14 0 7 -19.52 12.76 -14 0 8 17.21 13.67 -14 0 9 -0.49 10.80 -14 0 10 40.44 17.90 -14 0 11 6.77 10.29 -14 0 12 34.89 17.90 -14 0 13 11.73 12.18 -14 -1 0 602.45 49.45 -14 1 0 476.97 44.91 -14 1 -1 3.59 7.05 -14 -1 1 -2.53 7.72 -14 1 1 -0.43 8.96 -14 1 -2 508.21 46.34 -14 -1 2 574.92 48.13 -14 1 2 543.14 47.71 -14 -1 3 -0.27 8.73 -14 1 3 -5.54 9.17 -14 -1 4 204.09 30.33 -14 1 4 221.74 30.64 -14 -1 5 25.60 12.01 -14 1 5 3.67 8.01 -14 -1 6 45.36 15.86 -14 1 6 58.26 19.09 -14 -1 7 32.82 14.55 -14 1 7 34.62 14.10 -14 -1 8 32.23 15.82 -14 1 8 34.72 14.84 -14 -1 9 14.73 12.24 -14 1 9 15.15 14.77 -14 -1 10 217.21 31.75 -14 1 10 200.40 33.01 -14 -1 11 -0.47 7.75 -14 1 11 18.75 16.64 -14 -1 12 333.03 39.84 -14 1 12 345.46 42.06 -14 -1 13 13.30 13.83 -14 2 0 42.12 15.56 -14 -2 1 5.09 6.95 -14 2 -1 21.25 15.52 -14 2 1 18.03 12.22 -14 2 -2 61.73 18.68 -14 -2 2 40.37 14.32 -14 2 2 38.41 16.57 -14 -2 3 -6.64 6.68 -14 2 3 10.69 13.61 -14 -2 4 16.92 9.41 -14 2 4 7.02 11.30 -14 -2 5 -13.90 12.38 -14 2 5 3.54 11.22 -14 -2 6 -5.34 10.41 -14 2 6 3.25 10.00 -14 -2 7 12.84 10.62 -14 2 7 30.11 14.61 -14 -2 8 1.01 9.55 -14 2 8 24.57 13.94 -14 -2 9 7.00 7.86 -14 2 9 31.15 17.50 -14 -2 10 32.08 14.92 -14 2 10 5.30 8.90 -14 -2 11 11.17 11.70 -14 2 11 32.97 15.39 -14 -2 12 31.93 16.54 -14 2 12 47.11 18.58 -14 -2 13 -11.29 11.32 -14 3 0 509.30 48.04 -14 3 -1 18.46 14.44 -14 3 1 27.96 13.80 -14 -3 2 385.36 38.85 -14 3 -2 449.36 44.24 -14 3 2 355.65 40.46 -14 3 -3 30.04 11.76 -14 -3 3 13.81 9.58 -14 3 3 55.31 17.58 -14 -3 4 224.32 29.55 -14 3 4 215.24 32.70 -14 -3 5 90.89 19.53 -14 3 5 75.35 21.06 -14 -3 6 36.03 15.51 -14 3 6 4.31 11.28 -14 -3 7 158.69 26.51 -14 3 7 153.14 27.65 -14 -3 8 37.97 14.66 -14 3 8 34.27 16.49 -14 -3 9 63.42 18.36 -14 3 9 83.80 21.27 -14 -3 10 135.31 23.47 -14 3 10 166.50 29.67 -14 -3 11 71.93 20.51 -14 3 11 36.99 18.00 -14 -3 12 236.62 31.98 -14 -3 13 23.46 13.32 -14 -3 14 255.65 33.86 -14 4 0 10.04 11.94 -14 4 -1 13.07 14.59 -14 4 1 -0.50 10.39 -14 4 -2 33.03 15.28 -14 4 2 43.96 16.10 -14 -4 3 4.89 9.49 -14 4 -3 -5.33 9.12 -14 4 3 0.25 9.03 -14 -4 4 -4.37 6.76 -14 4 4 15.34 13.17 -14 -4 5 13.78 10.91 -14 4 5 16.38 11.33 -14 -4 6 3.95 8.50 -14 4 6 17.59 12.66 -14 -4 7 18.06 9.34 -14 4 7 33.82 14.60 -14 -4 8 13.31 11.72 -14 4 8 -6.81 8.91 -14 -4 9 9.37 10.68 -14 4 9 8.58 13.38 -14 -4 10 10.30 10.89 -14 4 10 24.51 11.40 -14 -4 11 9.68 9.26 -14 -4 12 37.36 16.41 -14 5 0 268.95 36.90 -14 5 -1 37.50 16.20 -14 5 1 70.35 21.17 -14 5 -2 264.48 37.00 -14 5 2 269.54 36.32 -14 5 -3 95.90 21.75 -14 5 3 88.37 23.23 -14 5 -4 104.90 24.07 -14 -5 4 152.36 24.77 -14 5 4 90.75 23.48 -14 -5 5 196.15 28.79 -14 5 5 227.71 34.86 -14 -5 6 25.70 12.09 -14 5 6 33.56 16.87 -14 5 7 323.73 41.27 -14 -5 7 261.81 31.57 -14 -5 8 -1.91 8.28 -14 5 8 23.49 16.27 -14 -5 9 222.44 29.10 -14 5 9 213.53 34.63 -14 -5 10 78.00 18.56 -14 6 0 2.13 10.51 -14 6 -1 14.13 13.65 -14 6 1 31.29 17.81 -14 6 -2 7.68 13.93 -14 6 2 2.18 9.57 -14 6 -3 19.09 14.74 -14 6 3 10.95 11.86 -14 6 -4 3.89 10.77 -14 6 4 0.79 10.56 -14 6 5 9.00 11.93 -14 -6 6 19.51 10.75 -14 6 6 29.99 15.65 -14 -6 7 13.97 9.18 -14 6 7 31.16 17.22 -14 -6 8 -3.48 7.61 -14 6 8 24.68 16.28 -14 7 0 88.08 23.37 -14 7 -1 -2.62 10.33 -14 7 1 11.54 12.46 -14 7 -2 121.33 26.46 -14 7 2 82.94 21.72 -14 7 -3 159.96 29.71 -14 7 3 144.31 29.80 -14 7 -4 47.19 19.04 -14 7 4 49.10 19.07 -14 7 5 251.33 37.68 -14 7 6 3.16 10.25 -14 7 7 378.17 46.41 -14 8 0 36.88 14.74 -14 8 -1 18.18 15.57 -14 8 1 12.53 11.96 -14 8 -2 25.90 16.66 -14 8 2 -1.65 9.71 -14 8 -3 22.12 15.93 -14 8 3 43.14 20.65 -14 8 -4 20.82 13.88 -14 8 4 -3.89 13.46 -14 8 5 2.64 13.02 -14 9 0 7.76 8.84 -14 9 -1 -3.64 9.83 -14 9 1 -1.09 11.46 -14 9 -2 21.34 13.58 -14 9 2 21.80 17.09 -14 9 -3 78.65 22.59 -14 9 3 109.02 27.70 -14 9 -4 36.38 16.67 -14 -10 1 -24.59 13.06 -14 10 -1 19.77 14.72 -14 10 -2 20.74 15.03 -14 10 -3 37.60 18.93 -14 10 -4 -12.30 14.15 -14 -11 2 19.24 13.28 -15 0 0 9.78 11.92 -15 0 1 5.36 10.96 -15 0 2 22.28 14.35 -15 0 3 6.29 14.89 -15 0 4 47.57 17.09 -15 0 5 -8.63 12.00 -15 0 6 171.25 28.66 -15 0 7 7.25 9.07 -15 0 8 170.77 30.45 -15 0 9 15.38 13.48 -15 1 0 1.90 8.07 -15 1 -1 14.28 16.39 -15 -1 1 15.21 11.22 -15 1 1 14.47 9.64 -15 -1 2 95.53 21.62 -15 1 2 45.76 21.64 -15 -1 3 22.47 14.26 -15 1 3 6.27 9.60 -15 -1 4 249.14 34.65 -15 1 4 208.24 31.62 -15 -1 5 -13.09 10.32 -15 1 5 16.17 13.03 -15 -1 6 380.91 41.72 -15 1 6 322.99 40.45 -15 -1 7 7.05 11.03 -15 1 7 84.68 24.38 -15 -1 8 269.44 36.37 -15 1 8 222.36 33.60 -15 -1 9 14.55 15.80 -15 2 0 -8.97 8.43 -15 2 -1 27.86 15.23 -15 2 1 2.02 11.39 -15 -2 2 25.62 12.50 -15 2 2 9.90 13.18 -15 -2 3 39.60 16.89 -15 2 3 32.10 15.05 -15 -2 4 73.00 20.52 -15 2 4 98.14 21.72 -15 -2 5 -11.11 9.73 -15 2 5 6.82 13.79 -15 -2 6 135.71 23.66 -15 2 6 160.18 29.35 -15 -2 7 -5.73 11.32 -15 2 7 15.34 12.48 -15 -2 8 130.98 25.06 -15 -2 9 19.24 12.45 -15 3 0 4.98 10.06 -15 3 -1 121.66 25.47 -15 3 1 109.85 25.33 -15 3 -2 75.48 20.38 -15 3 2 97.50 23.96 -15 -3 3 69.05 18.64 -15 3 3 102.40 24.06 -15 -3 4 226.94 31.45 -15 3 4 205.42 33.70 -15 -3 5 37.33 17.42 -15 3 5 46.11 19.00 -15 -3 6 257.34 33.40 -15 3 6 279.60 37.94 -15 -3 7 -6.39 7.56 -15 -3 8 248.16 33.63 -15 -3 9 18.65 12.33 -15 -3 10 141.73 27.30 -15 4 0 14.00 13.94 -15 4 -1 60.85 19.80 -15 4 1 54.59 20.03 -15 4 -2 23.65 14.81 -15 4 2 44.59 17.31 -15 4 3 64.50 22.43 -15 -4 4 103.61 21.92 -15 4 4 48.24 16.90 -15 -4 5 26.37 14.14 -15 4 5 4.54 8.82 -15 -4 6 90.10 21.20 -15 -4 7 -0.36 8.97 -15 -4 8 63.31 18.36 -15 -4 9 21.10 12.38 -15 -4 10 82.19 21.55 -15 5 0 3.83 10.27 -15 5 -1 235.78 35.86 -15 5 1 208.79 34.26 -15 5 -2 36.21 15.06 -15 5 2 36.05 18.13 -15 5 -3 87.60 24.97 -15 5 3 59.92 19.88 -15 -5 6 124.48 24.50 -15 -5 7 22.20 12.49 -15 -5 8 182.74 28.25 -15 -5 9 14.77 11.42 -15 6 0 42.44 19.80 -15 6 -1 108.59 26.77 -15 6 -2 25.14 18.66 0 0 0 0.00 0.00 TITL shI_3654_YaLa in Pbca REM Pbca (#61 in standard setting) CELL 0.71073 10.996556 13.714678 17.934471 90.0000 90.0000 90.0000 ZERR 4.00 0.000555 0.000984 0.000896 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O U UNIT 120.00 120.00 24.00 16.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 76498 _shelx_res_file ; TITL shi_3654_yala_a.res in Pbca shi_3654_yala.res created by SHELXL-2018/3 at 15:42:42 on 01-Jul-2024 REM Old TITL shI_3654_YaLa in Pbca #61 REM SHELXT solution in Pbca REM R1 0.145, Rweak 0.010, Alpha 0.062, Orientation as input REM Formula found by SHELXT: C6 N3 O1 I CELL 0.71073 10.996556 13.714678 17.934471 90 90 90 ZERR 8 0.000555 0.000984 0.000896 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O U UNIT 88 88 24 48 8 EQIV $1 0.5+X,0.5-Y,1-Z EQIV $2 +X,0.5-Y,0.5+Z EQIV $3 -0.5+X,+Y,1.5-Z EQIV $4 1.5-X,-0.5+Y,+Z EQIV $5 +X,0.5-Y,-0.5+Z DFIX 0.85 0.01 O6 H6 L.S. 20 PLAN 5 SIZE 0.1 0.1 0.15 TEMP -73 CONF HTAB O6 O3_$1 HTAB N3 O6_$2 HTAB N3 O4_$3 HTAB C10 O2_$4 HTAB C11 N2_$5 htab BOND $H list 4 MORE -1 fmap 2 acta SHEL 99 0.84 OMIT 0 2 0 OMIT 0 2 1 OMIT 8 11 7 REM REM REM WGHT 0.014700 FVAR 0.12714 U1 5 0.693910 0.275796 0.535123 11.00000 0.01371 0.02400 = 0.01753 -0.00098 -0.00102 0.00033 O1 4 0.670590 0.161213 0.492737 11.00000 0.02974 0.02832 = 0.02968 0.00165 -0.00256 0.00034 O2 4 0.719411 0.390237 0.576342 11.00000 0.01545 0.03042 = 0.02513 -0.00218 -0.00088 0.00295 O3 4 0.517498 0.270036 0.599183 11.00000 0.01891 0.03834 = 0.01752 -0.00397 -0.00167 0.00059 O4 4 1.073356 0.148201 0.561289 11.00000 0.01411 0.03761 = 0.03061 0.01067 0.01071 0.00700 O5 4 0.900706 0.230225 0.553706 11.00000 0.01956 0.03543 = 0.02230 0.01767 0.00580 -0.00255 O6 4 0.824122 0.335522 0.432332 11.00000 0.01787 0.02588 = 0.02683 0.00161 0.00295 0.00320 H6 2 0.875390 0.290219 0.425218 11.00000 -1.50000 N1 3 0.727610 0.201111 0.660836 11.00000 0.01078 0.02719 = 0.02557 0.00191 0.00175 -0.00586 N2 3 0.816277 0.126303 0.756626 11.00000 0.02920 0.03234 = 0.02838 0.00641 -0.00145 -0.00433 N3 3 0.719471 0.179721 0.780371 11.00000 0.02696 0.03934 = 0.01719 0.00553 0.00078 0.00279 AFIX 43 H3 2 0.694586 0.183100 0.826934 11.00000 -1.20000 AFIX 0 C1 1 0.494033 0.311731 0.665399 11.00000 0.01838 0.02023 = 0.02930 0.00263 0.00441 -0.00620 C2 1 0.394357 0.373551 0.672689 11.00000 0.02178 0.02452 = 0.03913 -0.00079 0.00208 -0.00187 AFIX 43 H2 2 0.343935 0.386412 0.630816 11.00000 -1.20000 AFIX 0 C3 1 0.368578 0.416174 0.740487 11.00000 0.02357 0.02536 = 0.05917 0.00377 0.01551 -0.00212 AFIX 43 H3A 2 0.299727 0.457636 0.744780 11.00000 -1.20000 AFIX 0 C4 1 0.440067 0.400043 0.801777 11.00000 0.03033 0.03442 = 0.04171 -0.00516 0.01894 -0.01282 AFIX 43 H4 2 0.421840 0.430771 0.847916 11.00000 -1.20000 AFIX 0 C5 1 0.538276 0.338984 0.795704 11.00000 0.03164 0.03258 = 0.02429 -0.00012 0.00230 -0.01202 AFIX 43 H5 2 0.588149 0.327390 0.838037 11.00000 -1.20000 AFIX 0 C6 1 0.565799 0.293859 0.728469 11.00000 0.01921 0.02443 = 0.01969 -0.00288 0.00701 -0.00568 C7 1 0.667420 0.226308 0.723322 11.00000 0.01775 0.02855 = 0.02349 0.00709 -0.00173 -0.00760 C8 1 0.817996 0.138839 0.684871 11.00000 0.01579 0.02264 = 0.02293 0.00533 0.00219 -0.00560 C9 1 0.964784 0.162010 0.579674 11.00000 0.02427 0.01883 = 0.02012 -0.00034 -0.00103 -0.00399 C10 1 0.908987 0.093902 0.634661 11.00000 0.01544 0.02524 = 0.04441 0.00915 -0.00034 -0.00429 AFIX 23 H10A 2 0.869498 0.039972 0.607091 11.00000 -1.20000 H10B 2 0.974574 0.065223 0.665466 11.00000 -1.20000 AFIX 0 C11 1 0.862004 0.435205 0.430325 11.00000 0.05122 0.03832 = 0.03735 -0.00125 0.00644 -0.01248 AFIX 137 H11A 2 0.902753 0.448521 0.382807 11.00000 -1.50000 H11B 2 0.918432 0.447745 0.471518 11.00000 -1.50000 H11C 2 0.790796 0.477681 0.435274 11.00000 -1.50000 AFIX 0 HKLF 4 REM shi_3654_yala_a.res in Pbca REM wR2 = 0.0561, GooF = S = 1.047, Restrained GooF = 1.047 for all data REM R1 = 0.0331 for 1904 Fo > 4sig(Fo) and 0.0481 for all 2380 data REM 194 parameters refined using 1 restraints END WGHT 0.0147 0.0000 REM Instructions for potential hydrogen bonds HTAB O6 O3_$1 HTAB N3 O4_$3 HTAB N3 O6_$2 HTAB C10 O2_$4 HTAB C11 N2_$5 REM Highest difference peak 1.077, deepest hole -0.816, 1-sigma level 0.160 Q1 1 0.6910 0.2066 0.5315 11.00000 0.05 1.08 Q2 1 0.7341 0.3497 0.5261 11.00000 0.05 0.97 Q3 1 0.6291 0.2794 0.4975 11.00000 0.05 0.64 Q4 1 0.6988 0.2363 0.6003 11.00000 0.05 0.60 Q5 1 0.4569 0.2656 0.5354 11.00000 0.05 0.56 ; _shelx_res_checksum 32205 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U U1 0.69391(2) 0.27580(2) 0.53512(2) 0.01841(9) Uani d 1 . . O O1 0.6706(4) 0.1612(4) 0.4927(2) 0.0292(13) Uani d 1 . . O O2 0.7194(4) 0.3902(4) 0.5763(2) 0.0237(12) Uani d 1 . . O O3 0.5175(4) 0.2700(4) 0.5992(2) 0.0249(12) Uani d 1 . . O O4 1.0734(4) 0.1482(4) 0.5613(2) 0.0274(13) Uani d 1 . . O O5 0.9007(4) 0.2302(4) 0.5537(2) 0.0258(12) Uani d 1 . . O O6 0.8241(4) 0.3355(4) 0.4323(3) 0.0235(12) Uani d 1 . . H H6 0.875(5) 0.290(4) 0.425(4) 0.035 Uiso d 1 . . N N1 0.7276(5) 0.2011(4) 0.6608(3) 0.0212(15) Uani d 1 . . N N2 0.8163(5) 0.1263(5) 0.7566(3) 0.0300(15) Uani d 1 . . N N3 0.7195(5) 0.1797(5) 0.7804(3) 0.0278(15) Uani d 1 . . H H3 0.694586 0.183100 0.826934 0.033 Uiso calc 1 . . C C1 0.4940(6) 0.3117(5) 0.6654(4) 0.0226(17) Uani d 1 . . C C2 0.3944(6) 0.3736(5) 0.6727(4) 0.0285(19) Uani d 1 . . H H2 0.343935 0.386412 0.630816 0.034 Uiso calc 1 . . C C3 0.3686(7) 0.4162(6) 0.7405(5) 0.036(2) Uani d 1 . . H H3A 0.299727 0.457636 0.744780 0.043 Uiso calc 1 . . C C4 0.4401(6) 0.4000(6) 0.8018(4) 0.035(2) Uani d 1 . . H H4 0.421840 0.430771 0.847916 0.043 Uiso calc 1 . . C C5 0.5383(7) 0.3390(6) 0.7957(4) 0.0295(19) Uani d 1 . . H H5 0.588149 0.327390 0.838037 0.035 Uiso calc 1 . . C C6 0.5658(6) 0.2939(5) 0.7285(3) 0.0211(17) Uani d 1 . . C C7 0.6674(6) 0.2263(5) 0.7233(4) 0.0233(17) Uani d 1 . . C C8 0.8180(6) 0.1388(5) 0.6849(4) 0.0205(16) Uani d 1 . . C C9 0.9648(6) 0.1620(5) 0.5797(4) 0.0211(17) Uani d 1 . . C C10 0.9090(6) 0.0939(5) 0.6347(4) 0.0284(19) Uani d 1 . . H H10A 0.869498 0.039972 0.607091 0.034 Uiso calc 1 . . H H10B 0.974574 0.065223 0.665466 0.034 Uiso calc 1 . . C C11 0.8620(7) 0.4352(6) 0.4303(4) 0.042(2) Uani d 1 . . H H11A 0.902753 0.448521 0.382807 0.063 Uiso calc 1 . . H H11B 0.918432 0.447745 0.471518 0.063 Uiso calc 1 . . H H11C 0.790796 0.477681 0.435274 0.063 Uiso calc 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 U1 0.01371(14) 0.02400(17) 0.01753(13) 0.00033(12) -0.00102(12) -0.00098(14) O1 0.030(3) 0.028(3) 0.030(3) 0.000(2) -0.003(2) 0.002(3) O2 0.015(3) 0.030(3) 0.025(3) 0.003(2) -0.001(2) -0.002(2) O3 0.019(2) 0.038(3) 0.018(2) 0.001(2) -0.002(2) -0.004(3) O4 0.014(3) 0.038(4) 0.031(3) 0.007(2) 0.011(2) 0.011(3) O5 0.020(3) 0.035(3) 0.022(2) -0.003(2) 0.006(2) 0.018(3) O6 0.018(3) 0.026(3) 0.027(2) 0.003(2) 0.003(2) 0.002(3) N1 0.011(3) 0.027(4) 0.026(3) -0.006(2) 0.002(3) 0.002(3) N2 0.029(4) 0.032(4) 0.028(3) -0.004(3) -0.001(3) 0.006(3) N3 0.027(4) 0.039(4) 0.017(3) 0.003(3) 0.001(3) 0.006(3) C1 0.018(4) 0.020(5) 0.029(4) -0.006(3) 0.004(3) 0.003(4) C2 0.022(4) 0.025(5) 0.039(4) -0.002(3) 0.002(4) -0.001(4) C3 0.024(4) 0.025(5) 0.059(6) -0.002(4) 0.016(4) 0.004(5) C4 0.030(5) 0.034(5) 0.042(5) -0.013(4) 0.019(4) -0.005(5) C5 0.032(5) 0.033(5) 0.024(4) -0.012(4) 0.002(4) 0.000(4) C6 0.019(4) 0.024(5) 0.020(3) -0.006(3) 0.007(3) -0.003(3) C7 0.018(4) 0.029(5) 0.023(4) -0.008(3) -0.002(3) 0.007(4) C8 0.016(4) 0.023(4) 0.023(4) -0.006(3) 0.002(3) 0.005(4) C9 0.024(4) 0.019(5) 0.020(4) -0.004(3) -0.001(3) 0.000(4) C10 0.015(4) 0.025(5) 0.044(5) -0.004(3) 0.000(4) 0.009(4) C11 0.051(5) 0.038(6) 0.037(5) -0.012(5) 0.006(4) -0.001(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' U U -9.6767 9.6646 '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 O1 U1 O3 . . 93.63(19) y O1 U1 O4 . 4_456 89.78(19) y O1 U1 O5 . . 88.01(19) y O1 U1 O6 . . 93.32(19) y O1 U1 N1 . . 92.6(2) y O2 U1 O1 . . 179.0(2) y O2 U1 O3 . . 87.38(18) y O2 U1 O4 . 4_456 90.19(18) y O2 U1 O5 . . 91.33(18) y O2 U1 O6 . . 85.72(19) y O2 U1 N1 . . 87.88(19) y O3 U1 O4 . 4_456 84.70(15) y O3 U1 O5 . . 137.78(15) y O3 U1 O6 . . 152.73(16) y O3 U1 N1 . . 69.78(16) y O4 U1 O6 4_456 . 68.98(15) y O4 U1 N1 4_456 . 154.47(16) y O5 U1 O4 . 4_456 137.52(15) y O5 U1 O6 . . 68.81(14) y O5 U1 N1 . . 68.00(15) y O6 U1 N1 . . 136.12(15) y C1 O3 U1 . . 126.9(4) ? C9 O4 U1 . 4_556 130.3(4) ? C9 O5 U1 . . 141.3(4) ? U1 O6 H6 . . 105(5) ? C11 O6 U1 . . 120.3(4) ? C11 O6 H6 . . 120(5) ? C7 N1 U1 . . 124.9(4) ? C7 N1 C8 . . 104.7(6) ? C8 N1 U1 . . 129.9(4) ? C8 N2 N3 . . 104.5(6) ? N2 N3 H3 . . 124.7 ? C7 N3 N2 . . 110.7(6) ? C7 N3 H3 . . 124.7 ? O3 C1 C2 . . 119.6(7) ? O3 C1 C6 . . 122.1(6) ? C2 C1 C6 . . 118.3(7) ? C1 C2 H2 . . 119.9 ? C3 C2 C1 . . 120.2(7) ? C3 C2 H2 . . 119.9 ? C2 C3 H3A . . 119.3 ? C4 C3 C2 . . 121.4(7) ? C4 C3 H3A . . 119.3 ? C3 C4 H4 . . 120.4 ? C3 C4 C5 . . 119.2(8) ? C5 C4 H4 . . 120.4 ? C4 C5 H5 . . 119.6 ? C4 C5 C6 . . 120.9(7) ? C6 C5 H5 . . 119.6 ? C1 C6 C7 . . 119.5(6) ? C5 C6 C1 . . 120.0(6) ? C5 C6 C7 . . 120.4(6) ? N1 C7 C6 . . 126.4(6) ? N3 C7 N1 . . 107.7(6) ? N3 C7 C6 . . 125.8(6) ? N1 C8 C10 . . 123.7(6) ? N2 C8 N1 . . 112.4(6) ? N2 C8 C10 . . 123.9(7) ? O4 C9 O5 . . 123.2(6) ? O4 C9 C10 . . 118.1(6) ? O5 C9 C10 . . 118.7(6) ? C8 C10 C9 . . 114.8(6) ? C8 C10 H10A . . 108.6 ? C8 C10 H10B . . 108.6 ? C9 C10 H10A . . 108.6 ? C9 C10 H10B . . 108.6 ? H10A C10 H10B . . 107.5 ? O6 C11 H11A . . 109.5 ? O6 C11 H11B . . 109.5 ? O6 C11 H11C . . 109.5 ? H11A C11 H11B . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag U1 O1 . 1.764(5) y U1 O2 . 1.757(5) y U1 O3 . 2.256(4) y U1 O4 4_456 2.415(4) y U1 O5 . 2.382(5) y U1 O6 . 2.474(5) y U1 N1 . 2.504(5) y O3 C1 . 1.343(8) ? O4 C9 . 1.253(7) ? O5 C9 . 1.260(8) ? O6 H6 . 0.849(10) ? O6 C11 . 1.430(8) ? N1 C7 . 1.347(8) ? N1 C8 . 1.380(8) ? N2 N3 . 1.361(8) ? N2 C8 . 1.298(8) ? N3 H3 . 0.8800 ? N3 C7 . 1.335(8) ? C1 C2 . 1.392(9) ? C1 C6 . 1.401(9) ? C2 H2 . 0.9500 ? C2 C3 . 1.379(10) ? C3 H3A . 0.9500 ? C3 C4 . 1.369(10) ? C4 H4 . 0.9500 ? C4 C5 . 1.371(10) ? C5 H5 . 0.9500 ? C5 C6 . 1.389(9) ? C6 C7 . 1.454(9) ? C8 C10 . 1.481(9) ? C9 C10 . 1.490(9) ? C10 H10A . 0.9900 ? C10 H10B . 0.9900 ? C11 H11A . 0.9800 ? C11 H11B . 0.9800 ? C11 H11C . 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 O6 H6 O3 4_556 0.849(10) 1.82(3) 2.634(6) 160(7) yes N3 H3 O4 6_557 0.88 2.45 3.291(7) 159.0 yes N3 H3 O6 7_566 0.88 2.38 2.966(7) 124.2 yes C10 H10A O2 8_755 0.99 2.34 3.300(8) 163.0 yes C11 H11A N2 7_565 0.98 2.66 3.266(10) 120.3 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_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag U1 O3 C1 C2 . . . . 125.8(6) ? U1 O3 C1 C6 . . . . -55.2(9) ? U1 O4 C9 O5 4_556 . . . -8.3(10) ? U1 O4 C9 C10 4_556 . . . 171.3(4) ? U1 O5 C9 O4 . . . . 158.0(5) ? U1 O5 C9 C10 . . . . -21.7(11) ? U1 N1 C7 N3 . . . . -172.7(4) ? U1 N1 C7 C6 . . . . 5.9(10) ? U1 N1 C8 N2 . . . . 170.6(4) ? U1 N1 C8 C10 . . . . -7.6(10) ? O3 C1 C2 C3 . . . . 179.4(6) ? O3 C1 C6 C5 . . . . 179.7(6) ? O3 C1 C6 C7 . . . . -1.6(10) ? O4 C9 C10 C8 . . . . 146.7(6) ? O5 C9 C10 C8 . . . . -33.6(9) ? N1 C8 C10 C9 . . . . 45.3(9) ? N2 N3 C7 N1 . . . . 2.0(8) ? N2 N3 C7 C6 . . . . -176.6(6) ? N2 C8 C10 C9 . . . . -132.7(7) ? N3 N2 C8 N1 . . . . 1.8(8) ? N3 N2 C8 C10 . . . . 180.0(6) ? C1 C2 C3 C4 . . . . 0.7(11) ? C1 C6 C7 N1 . . . . 23.3(11) ? C1 C6 C7 N3 . . . . -158.3(7) ? C2 C1 C6 C5 . . . . -1.3(10) ? C2 C1 C6 C7 . . . . 177.4(6) ? C2 C3 C4 C5 . . . . -1.0(11) ? C3 C4 C5 C6 . . . . 0.1(11) ? C4 C5 C6 C1 . . . . 1.1(11) ? C4 C5 C6 C7 . . . . -177.6(7) ? C5 C6 C7 N1 . . . . -158.0(7) ? C5 C6 C7 N3 . . . . 20.4(11) ? C6 C1 C2 C3 . . . . 0.5(11) ? C7 N1 C8 N2 . . . . -0.6(8) ? C7 N1 C8 C10 . . . . -178.8(6) ? C8 N1 C7 N3 . . . . -0.9(8) ? C8 N1 C7 C6 . . . . 177.8(7) ? C8 N2 N3 C7 . . . . -2.3(8) ?