#------------------------------------------------------------------------------ #$Date: 2024-09-25 04:06:52 +0200 (Wed, 25 Sep 2024) $ #$Revision: 294885 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023259.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_2023259 loop_ _publ_author_name 'Moroni, Aldana B.' 'Bottoso, Tiago' 'Lionello, Diego F.' 'Vega, Daniel R.' 'Kaufman, Teodoro S.' 'Calvo, Natalia L.' _publ_section_title ; Synthesis, crystal structure and Hirshfeld surface analysis of sulfamethoxazolium methylsulfate monohydrate ; _journal_coeditor_code EX2088 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024009204 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C10 H12 N3 O3 S +, C H3 O4 S -, H2 O' _chemical_formula_moiety 'C10 H12 N3 O3 S +, C H3 O4 S -, H2 O' _chemical_formula_sum 'C11 H17 N3 O8 S2' _chemical_formula_weight 383.39 _chemical_name_common ; Sulfamethoxazolium methyl sulfate monohydrate ; _chemical_name_systematic ; 4-[(5-Methyl-1,2-oxazol-3-yl)sulfamoyl]anilinium methyl sulfate monohydrate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2019/1 _cell_angle_alpha 84.722(6) _cell_angle_beta 78.442(5) _cell_angle_gamma 81.940(5) _cell_formula_units_Z 2 _cell_length_a 5.8838(8) _cell_length_b 11.6532(15) _cell_length_c 12.3276(16) _cell_measurement_reflns_used 1942 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 26.1537 _cell_measurement_theta_min 2.2773 _cell_volume 818.14(19) _computing_cell_refinement ; SAINT (Bruker, 2019) ; _computing_data_collection ; APEX4 (Bruker, 2019) ; _computing_data_reduction ; SAINT (Bruker, 2019) ; _computing_molecular_graphics ; POV-RAY (Cason, 2004), Mercury (Macrae et al., 2020), PLATON (Spek, 2020) ; _computing_publication_material ; publCIF (Westrip, 2010), WinGX (Farrugia, 2012), PLATON (Spek, 2020), SHELXS97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2019/1 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker D8 Quest ECO' _diffrn_measurement_method '\w scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_unetI/netI 0.0301 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 18938 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.365 _diffrn_reflns_theta_min 3.381 _diffrn_source 'Sealed tube' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.372 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.556 _exptl_crystal_description needle _exptl_crystal_F_000 400 _exptl_crystal_size_max 1.000 _exptl_crystal_size_mid 0.354 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.330 _refine_diff_density_min -0.321 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 226 _refine_ls_number_reflns 3318 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0430 _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^)+(0.0142P)^2^+1.0486P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.1000 _reflns_number_gt 2716 _reflns_number_total 3318 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ex2088.cif _cod_data_source_block I _cod_database_code 2023259 _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 0.661 _shelx_estimated_absorpt_t_max 0.957 _shelx_hkl_file ; -1 0 0 289.37 14.20 -1 0 0 275.97 14.10 -1 0 0 280.37 15.00 -1 0 0 289.97 14.90 -1 0 0 263.97 13.80 1 0 0 274.57 14.10 1 0 0 281.27 14.20 1 0 0 276.27 15.60 1 0 0 294.87 14.90 -3 0 0 958.60 45.80 -3 0 0 890.51 45.40 -3 0 0 916.31 48.00 -3 0 0 900.31 45.00 -3 0 0 950.30 47.70 3 0 0 926.71 45.80 3 0 0 937.31 45.00 3 0 0 934.41 47.70 3 0 0 897.11 45.40 -4 0 0 703.73 40.10 -4 0 0 744.63 41.40 -4 0 0 772.62 38.20 -4 0 0 669.43 36.90 4 0 0 710.33 37.50 4 0 0 736.53 37.20 4 0 0 706.83 37.90 4 0 0 718.73 40.40 -5 0 0 452.95 28.20 -5 0 0 530.15 29.50 -5 0 0 461.05 31.00 -5 0 0 495.05 33.80 5 0 0 489.75 28.60 5 0 0 519.15 28.80 5 0 0 523.95 32.70 5 0 0 464.75 28.80 -6 0 0 54.89 9.10 -6 0 0 43.10 12.70 -6 0 0 46.40 8.80 6 0 0 64.59 10.00 6 0 0 40.30 9.70 6 0 0 36.10 7.80 -7 0 0 123.19 19.50 -7 0 0 141.29 20.80 7 0 0 153.28 23.50 7 0 0 80.59 14.50 7 0 0 92.09 15.30 7 0 0 115.99 14.20 7 -1 0 -6.00 7.10 7 -1 0 2.60 6.20 7 -1 0 -8.20 8.10 7 -1 0 -1.40 13.30 -7 1 0 1.60 9.90 -7 1 0 -9.30 12.20 6 -1 0 2.70 6.60 6 -1 0 3.10 8.10 6 -1 0 1.40 5.80 -6 1 0 -12.30 8.00 -6 1 0 -0.10 6.30 5 -1 0 45.00 9.20 5 -1 0 52.79 8.90 5 -1 0 46.90 6.90 5 -1 0 47.80 7.90 -5 1 0 61.79 13.20 -5 1 0 69.49 9.70 -5 1 0 46.30 8.30 -5 1 0 47.80 8.10 4 -1 0 45.20 6.90 4 -1 0 40.80 7.70 4 -1 0 43.10 6.80 4 -1 0 52.49 7.60 -4 1 0 40.30 7.70 -4 1 0 46.60 9.80 -4 1 0 58.69 7.90 -4 1 0 50.89 8.30 3 -1 0 1091.39 53.69 3 -1 0 1035.10 51.49 3 -1 0 1062.79 50.99 3 -1 0 1069.29 50.79 -3 1 0 1087.79 50.89 -3 1 0 995.20 53.29 -3 1 0 1055.49 54.79 -3 1 0 1019.20 50.89 2 -1 0 327.97 17.60 2 -1 0 360.96 19.50 2 -1 0 342.47 17.80 2 -1 0 353.26 18.50 -2 1 0 354.46 17.60 -2 1 0 328.37 18.30 -2 1 0 326.27 17.80 -2 1 0 348.17 20.60 -2 1 0 341.27 19.60 1 -1 0 24.30 2.60 1 -1 0 29.60 4.30 1 -1 0 22.70 3.80 1 -1 0 21.30 3.30 -1 1 0 15.40 2.90 -1 1 0 16.50 4.10 -1 1 0 23.30 3.30 -1 1 0 24.70 3.30 -1 1 0 23.20 2.50 0 -1 0 0.10 0.50 -1 -1 0 741.63 35.30 -1 -1 0 765.22 34.70 -1 -1 0 707.13 34.50 -1 -1 0 767.22 35.50 1 1 0 742.33 35.50 1 1 0 729.03 34.70 1 1 0 709.63 34.60 1 1 0 730.03 35.30 -2 -1 0 823.72 41.80 -2 -1 0 883.71 43.20 -2 -1 0 906.91 43.90 -2 -1 0 907.11 43.20 -2 -1 0 888.61 42.30 2 1 0 851.91 43.10 2 1 0 933.11 44.10 2 1 0 890.01 43.20 2 1 0 859.71 42.40 2 1 0 886.11 42.00 -3 -1 0 655.03 34.00 -3 -1 0 665.63 36.20 -3 -1 0 691.03 35.40 -3 -1 0 652.23 35.80 -3 -1 0 674.73 33.60 3 1 0 711.63 33.90 3 1 0 664.43 35.00 3 1 0 692.63 36.30 3 1 0 649.24 34.20 -4 -1 0 0.80 5.20 -4 -1 0 0.40 4.10 -4 -1 0 2.30 3.40 -4 -1 0 -2.40 3.70 4 1 0 -1.20 3.00 4 1 0 0.50 4.60 4 1 0 -4.60 3.50 4 1 0 -3.70 4.10 -5 -1 0 -0.30 5.10 -5 -1 0 4.20 4.60 -5 -1 0 5.60 4.80 -5 -1 0 2.90 8.30 5 1 0 1.90 5.90 5 1 0 -1.70 5.00 5 1 0 5.00 5.00 5 1 0 -1.70 5.50 -6 -1 0 270.07 20.30 -6 -1 0 280.87 23.50 6 1 0 212.28 18.60 6 1 0 239.38 18.30 6 1 0 215.08 20.60 6 1 0 239.88 20.10 -7 -1 0 15.10 10.90 -7 -1 0 27.30 9.90 -7 -1 0 17.00 8.80 -7 -1 0 21.50 9.70 7 1 0 11.20 7.80 7 1 0 22.70 10.20 6 -2 0 -7.10 3.80 6 -2 0 1.40 4.90 6 -2 0 -10.80 6.00 6 -2 0 -12.80 5.90 6 -2 0 -5.90 9.10 -6 2 0 -12.70 9.30 -6 2 0 -2.60 6.50 5 -2 0 612.24 33.60 5 -2 0 652.53 37.70 5 -2 0 663.23 34.60 5 -2 0 544.85 31.50 -5 2 0 533.65 33.00 -5 2 0 560.14 36.50 -5 2 0 564.44 38.70 4 -2 0 308.77 19.40 4 -2 0 326.17 19.70 4 -2 0 306.27 21.90 4 -2 0 268.87 17.20 -4 2 0 295.47 23.60 -4 2 0 270.47 18.40 -4 2 0 290.37 21.50 3 -2 0 512.15 29.10 3 -2 0 522.95 26.50 3 -2 0 511.15 25.70 3 -2 0 502.35 27.20 -3 2 0 501.55 30.70 -3 2 0 476.15 28.80 -3 2 0 502.35 26.50 2 -2 0 24.40 4.00 2 -2 0 15.80 2.30 2 -2 0 16.60 3.90 2 -2 0 13.30 2.00 2 -2 0 18.40 3.80 -2 2 0 21.40 3.80 -2 2 0 17.40 3.80 -2 2 0 26.40 6.10 -2 2 0 14.60 3.00 1 -2 0 4296.67 210.18 1 -2 0 4864.91 209.28 -1 2 0 4593.64 209.18 -1 -2 0 2184.58 101.19 -1 -2 0 2045.10 98.79 -1 -2 0 2258.17 100.39 1 2 0 2430.96 101.49 1 2 0 2097.29 98.89 1 2 0 2196.38 100.39 1 2 0 2157.88 100.69 1 2 0 2158.08 101.09 1 2 0 2139.59 99.59 -2 -2 0 6512.15 293.37 -2 -2 0 6910.81 295.17 2 2 0 6459.85 294.97 2 2 0 6034.40 292.67 2 2 0 6536.05 294.67 2 2 0 6237.28 293.17 -3 -2 0 376.16 21.10 -3 -2 0 383.26 22.20 -3 -2 0 419.46 23.70 -3 -2 0 396.46 23.10 3 2 0 373.06 21.90 3 2 0 391.86 22.80 3 2 0 372.66 21.50 3 2 0 383.56 23.50 3 2 0 367.36 20.90 -4 -2 0 1033.00 51.49 -4 -2 0 998.90 51.09 -4 -2 0 948.21 51.89 4 2 0 966.10 50.99 4 2 0 949.90 49.40 4 2 0 996.30 52.59 4 2 0 983.10 48.90 -5 -2 0 426.06 27.90 -5 -2 0 459.55 27.90 -5 -2 0 400.36 28.40 -5 -2 0 409.86 25.20 5 2 0 432.96 29.40 5 2 0 423.76 27.60 5 2 0 403.96 25.30 5 2 0 408.86 25.30 -6 -2 0 21.40 8.90 -6 -2 0 9.50 6.30 -6 -2 0 6.50 6.20 -6 -2 0 13.10 6.50 6 2 0 7.50 6.60 6 2 0 7.80 6.70 6 2 0 5.50 6.00 6 2 0 12.00 7.10 -7 -2 0 90.69 12.80 -7 -2 0 94.39 17.10 7 2 0 88.09 12.80 7 2 0 81.39 12.60 7 2 0 76.19 14.30 6 -3 0 20.40 7.60 6 -3 0 14.80 4.60 6 -3 0 11.10 4.30 6 -3 0 15.30 7.30 -6 3 0 7.60 11.70 -6 3 0 12.10 7.80 5 -3 0 269.47 16.30 5 -3 0 241.18 16.50 5 -3 0 329.67 23.40 5 -3 0 289.47 23.20 5 -3 0 309.67 20.20 -5 3 0 252.97 22.40 -5 3 0 261.47 20.00 -5 3 0 273.17 26.80 4 -3 0 101.39 11.80 4 -3 0 108.69 13.30 4 -3 0 81.59 8.10 4 -3 0 97.59 7.90 -4 3 0 94.69 14.90 -4 3 0 87.29 12.80 -4 3 0 96.59 11.10 3 -3 0 736.63 33.10 3 -3 0 683.93 36.20 3 -3 0 685.23 37.40 3 -3 0 746.43 35.50 3 -3 0 680.13 33.40 -3 3 0 700.53 40.20 -3 3 0 664.13 37.60 -3 3 0 628.44 34.80 2 -3 0 1385.06 63.09 2 -3 0 1415.56 62.89 2 -3 0 1405.36 66.79 2 -3 0 1438.16 66.19 -2 3 0 1330.97 68.39 -2 3 0 1243.78 64.19 -2 3 0 1387.96 66.99 0 -3 0 277.57 13.60 0 -3 0 255.07 14.70 0 -3 0 263.37 14.60 0 -3 0 291.17 15.20 0 3 0 307.77 15.10 0 3 0 271.17 14.50 0 3 0 287.87 15.20 0 3 0 258.97 13.20 0 3 0 264.37 14.80 -1 -3 0 419.06 21.00 -1 -3 0 399.26 21.90 -1 -3 0 389.16 21.10 1 3 0 413.76 21.20 1 3 0 415.46 21.90 1 3 0 429.36 21.50 1 3 0 393.26 19.80 -2 -3 0 2158.88 104.59 -2 -3 0 2343.37 104.19 -2 -3 0 2330.57 107.49 -2 -3 0 2435.06 105.89 2 3 0 2415.96 107.79 2 3 0 2185.28 105.89 2 3 0 2166.58 104.19 2 3 0 2347.36 107.29 2 3 0 2114.89 104.69 -3 -3 0 128.89 10.10 -3 -3 0 145.09 12.40 -3 -3 0 154.08 13.00 3 3 0 134.29 10.90 3 3 0 144.79 10.20 3 3 0 144.29 12.10 3 3 0 142.69 11.90 3 3 0 128.19 9.80 -4 -3 0 42.40 7.50 -4 -3 0 37.30 7.70 -4 -3 0 51.59 8.00 4 3 0 59.89 8.60 4 3 0 47.60 7.30 4 3 0 40.70 7.90 4 3 0 45.40 7.30 -5 -3 0 -6.40 5.70 -5 -3 0 -5.20 4.80 -5 -3 0 -0.20 5.40 5 3 0 7.20 5.70 5 3 0 -2.80 5.00 5 3 0 0.60 5.30 5 3 0 -0.10 5.40 -6 -3 0 6.70 7.40 -6 -3 0 21.50 8.60 6 3 0 13.90 7.70 6 3 0 7.00 6.90 6 3 0 1.80 7.00 -7 -3 0 -9.80 8.00 -7 -3 0 3.60 8.60 7 3 0 -16.50 8.60 7 3 0 -3.90 6.80 7 3 0 14.50 9.90 6 -4 0 18.10 8.50 6 -4 0 17.40 8.20 6 -4 0 11.20 3.70 -6 4 0 16.60 11.30 -6 4 0 18.50 8.40 5 -4 0 444.66 21.50 5 -4 0 439.66 27.40 5 -4 0 386.96 21.70 5 -4 0 429.76 28.80 -5 4 0 389.66 26.30 -5 4 0 366.46 31.40 4 -4 0 455.45 22.10 4 -4 0 480.15 27.50 4 -4 0 467.25 29.40 4 -4 0 400.26 22.30 -4 4 0 419.16 25.70 -4 4 0 444.96 31.60 -4 4 0 437.76 29.30 3 -4 0 981.70 50.59 3 -4 0 1031.40 49.70 3 -4 0 927.11 44.90 3 -4 0 1023.80 44.80 -3 4 0 917.61 50.49 -3 4 0 896.41 47.30 -3 4 0 963.30 53.19 2 -4 0 3.20 1.20 2 -4 0 3.80 2.80 2 -4 0 5.50 3.70 2 -4 0 3.00 1.10 -2 4 0 0.90 3.00 -2 4 0 2.60 5.50 -2 4 0 1.80 3.00 1 -4 0 2459.85 116.89 1 -4 0 2693.13 119.59 -1 4 0 2648.44 119.69 -1 4 0 2488.95 120.69 -1 4 0 2502.95 116.69 0 -4 0 2348.57 117.99 0 -4 0 2460.45 119.69 0 -4 0 2544.15 120.29 0 -4 0 2764.42 120.59 0 4 0 2536.65 120.19 0 4 0 2806.42 120.59 0 4 0 2754.42 120.69 0 4 0 2563.04 119.69 -1 -4 0 7561.04 342.17 1 4 0 7468.95 342.67 -2 -4 0 153.48 12.40 2 4 0 129.49 11.40 2 4 0 141.29 11.20 2 4 0 144.39 10.40 2 4 0 135.69 10.40 -3 -4 0 35.70 4.50 -3 -4 0 34.80 5.50 -3 -4 0 34.00 6.50 3 4 0 24.60 4.50 3 4 0 23.50 5.50 3 4 0 31.20 5.60 3 4 0 20.50 5.40 3 4 0 33.30 4.40 -4 -4 0 825.02 46.10 -4 -4 0 858.11 46.30 -4 -4 0 841.62 42.40 4 4 0 822.32 42.40 4 4 0 818.72 43.60 4 4 0 840.52 45.70 4 4 0 836.82 46.60 -5 -4 0 987.30 54.49 -5 -4 0 1011.80 54.89 -5 -4 0 1040.30 51.39 5 4 0 944.51 53.69 5 4 0 953.70 51.09 5 4 0 997.40 50.69 5 4 0 919.71 54.69 -6 -4 0 16.90 8.40 -6 -4 0 35.20 9.50 -6 -4 0 23.80 7.50 -6 -4 0 13.20 8.10 6 4 0 14.10 7.70 6 4 0 15.00 7.70 6 4 0 8.90 7.00 -7 -4 0 42.80 11.30 -7 -4 0 32.70 10.60 7 4 0 23.20 8.60 7 4 0 31.30 10.60 7 4 0 32.80 11.00 6 -5 0 276.57 25.00 6 -5 0 287.07 23.10 -6 5 0 250.67 29.90 -6 5 0 226.78 24.10 5 -5 0 292.97 21.00 5 -5 0 283.97 23.00 -5 5 0 230.78 26.60 -5 5 0 231.08 20.50 4 -5 0 999.00 52.09 4 -5 0 1014.50 50.79 -4 5 0 927.51 55.69 -4 5 0 859.31 47.70 -4 5 0 854.51 51.59 3 -5 0 9.80 4.20 3 -5 0 11.80 6.30 -3 5 0 1.40 7.60 -3 5 0 5.30 3.70 -3 5 0 0.80 3.60 2 -5 0 102.39 10.40 2 -5 0 99.99 6.00 2 -5 0 104.69 10.70 -2 5 0 102.79 11.70 -2 5 0 99.69 10.40 1 -5 0 404.06 20.90 1 -5 0 421.46 23.60 -1 5 0 401.26 20.50 -1 5 0 450.75 23.90 -1 5 0 399.76 20.20 -1 5 0 420.46 21.40 -1 5 0 402.96 23.30 -1 5 0 389.36 24.50 0 -5 0 1102.69 54.89 0 -5 0 1068.59 54.29 0 -5 0 1199.28 55.39 0 -5 0 1109.59 52.19 0 5 0 1211.78 55.69 0 5 0 1176.38 55.19 0 5 0 1054.79 54.69 0 5 0 1125.79 52.29 0 5 0 1116.29 54.29 -1 -5 0 83.39 8.90 -1 -5 0 106.99 6.30 -1 -5 0 84.69 9.60 1 5 0 101.19 6.60 1 5 0 88.29 9.00 1 5 0 103.19 6.30 1 5 0 113.89 8.60 1 5 0 105.99 9.10 -2 -5 0 66.29 10.00 -2 -5 0 96.69 7.80 2 5 0 70.09 9.60 2 5 0 84.59 8.70 2 5 0 98.69 9.20 2 5 0 79.49 8.20 2 5 0 91.89 9.20 -3 -5 0 194.68 8.90 -3 -5 0 181.48 15.60 -3 -5 0 169.58 11.80 3 5 0 176.88 12.20 3 5 0 152.58 14.30 3 5 0 159.88 13.20 3 5 0 189.58 14.30 3 5 0 169.28 14.40 -4 -5 0 43.80 6.10 -4 -5 0 29.60 7.70 -4 -5 0 48.50 7.50 4 5 0 61.09 9.00 4 5 0 40.50 8.10 4 5 0 43.20 7.60 4 5 0 43.40 8.00 4 5 0 47.10 8.50 -5 -5 0 229.78 21.90 -5 -5 0 229.88 16.70 -5 -5 0 250.07 19.50 5 5 0 209.58 20.80 5 5 0 244.18 18.50 5 5 0 251.17 22.00 5 5 0 245.58 18.40 -6 -5 0 25.30 9.00 -6 -5 0 23.50 9.90 -6 -5 0 15.20 7.20 6 5 0 18.80 8.00 6 5 0 19.60 7.60 6 5 0 35.80 9.10 -7 -5 0 -5.90 7.80 -7 -5 0 -12.00 12.50 7 5 0 -11.40 8.00 7 5 0 -6.40 7.30 6 -6 0 -8.50 19.70 6 -6 0 -6.80 20.90 6 -6 0 9.10 8.50 6 -6 0 -5.60 20.50 -6 6 0 -6.30 10.40 -6 6 0 -16.60 11.30 5 -6 0 -22.00 13.90 5 -6 0 0.50 6.30 5 -6 0 -23.10 14.50 5 -6 0 -27.90 14.30 5 -6 0 2.60 7.00 -5 6 0 -17.50 10.00 -5 6 0 1.40 7.10 4 -6 0 671.23 39.10 4 -6 0 724.63 38.70 -4 6 0 573.84 38.90 -4 6 0 588.04 35.00 -4 6 0 637.34 43.80 3 -6 0 122.99 12.70 3 -6 0 148.79 14.90 -3 6 0 131.59 17.70 -3 6 0 106.39 11.30 -3 6 0 114.19 14.10 2 -6 0 71.59 9.90 2 -6 0 69.69 4.90 -2 6 0 55.99 8.50 -2 6 0 61.69 8.40 -2 6 0 65.09 4.40 -2 6 0 62.39 11.40 1 -6 0 2181.18 105.59 1 -6 0 2325.97 108.59 -1 6 0 2105.59 109.49 -1 6 0 2326.57 104.69 -1 6 0 2364.66 109.09 -1 6 0 2393.66 108.99 -1 6 0 2266.37 105.29 0 -6 0 1026.30 53.79 0 -6 0 1101.59 52.69 0 -6 0 989.10 51.29 0 6 0 969.30 51.79 0 6 0 1096.29 52.49 0 6 0 1090.39 52.89 0 6 0 1025.80 51.19 0 6 0 1086.59 49.00 -1 -6 0 287.17 18.50 -1 -6 0 282.67 18.60 -1 -6 0 310.97 14.90 1 6 0 298.77 18.50 1 6 0 298.07 15.20 1 6 0 308.27 18.30 1 6 0 272.57 15.40 1 6 0 258.77 17.90 -2 -6 0 464.35 28.40 -2 -6 0 507.75 23.90 2 6 0 464.15 28.00 2 6 0 510.45 27.70 2 6 0 456.35 27.10 -3 -6 0 44.10 7.70 3 6 0 45.30 7.60 3 6 0 41.10 6.50 3 6 0 64.79 10.20 3 6 0 34.10 6.50 -4 -6 0 168.38 14.50 -4 -6 0 204.38 9.50 -4 -6 0 172.78 19.10 4 6 0 157.28 14.80 4 6 0 199.08 15.60 4 6 0 205.28 17.10 4 6 0 177.98 18.20 4 6 0 175.68 17.20 -5 -6 0 468.05 33.10 -5 -6 0 495.25 28.50 -5 -6 0 499.95 25.10 5 6 0 432.66 32.80 5 6 0 473.65 29.50 5 6 0 483.75 28.60 5 6 0 462.65 32.90 -6 -6 0 34.80 9.70 -6 -6 0 23.60 6.90 -6 -6 0 37.60 10.60 6 6 0 23.80 9.50 6 6 0 36.90 9.40 6 6 0 40.00 9.60 5 -7 0 13.20 8.10 5 -7 0 1.50 11.20 -5 7 0 26.70 9.10 -5 7 0 25.20 12.20 4 -7 0 52.39 10.00 -4 7 0 43.50 14.50 -4 7 0 54.69 8.40 3 -7 0 1113.39 57.59 -3 7 0 1044.90 61.19 -3 7 0 1027.00 57.59 -3 7 0 1065.49 53.19 -3 7 0 1070.19 56.29 2 -7 0 209.48 11.70 2 -7 0 196.18 17.00 -2 7 0 208.68 16.80 -2 7 0 214.98 11.30 -2 7 0 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1 0 -14 -6.90 7.60 1 0 -14 -9.80 6.70 -1 0 14 -0.40 10.30 -1 0 14 -5.00 5.80 0 0 -14 -0.70 6.20 0 0 14 -6.00 9.10 0 0 14 -7.10 6.90 -1 0 -14 -11.60 6.20 -1 0 -14 -7.30 4.00 -1 0 -14 -6.20 2.80 1 0 14 -12.60 7.40 1 0 14 -13.40 8.90 -2 0 -14 14.20 7.50 2 0 14 19.00 12.90 2 0 14 24.40 10.30 -3 0 -14 11.20 7.40 3 0 14 16.30 12.40 3 0 14 38.00 12.80 -4 0 -14 2.80 6.80 4 0 14 -12.30 9.50 4 0 14 -12.00 9.20 1 -1 -14 -7.90 4.90 1 -1 -14 -12.80 6.80 -1 1 14 -4.00 5.90 -1 1 14 -5.70 7.20 0 -1 -14 -4.30 5.30 0 1 14 -8.30 7.00 0 1 14 5.10 10.70 0 1 14 2.10 7.80 -1 -1 -14 59.29 7.90 -1 -1 -14 52.59 10.70 -1 -1 -14 71.99 9.60 1 1 14 67.29 13.20 1 1 14 63.39 16.30 -2 -1 -14 57.29 10.70 2 1 14 61.49 14.80 2 1 14 61.49 14.80 -3 -1 -14 216.38 22.10 3 1 14 254.17 26.30 3 1 14 205.78 24.00 -4 -1 -14 64.29 12.50 4 1 14 88.19 17.80 4 1 14 66.49 16.30 1 -2 -14 74.49 12.80 -1 2 14 63.79 15.80 -1 2 14 78.59 12.50 0 -2 -14 293.97 24.60 0 -2 -14 252.47 19.80 0 2 14 231.18 21.30 0 2 14 284.97 27.80 0 2 14 202.38 20.60 -1 -2 -14 4.70 4.30 -1 -2 -14 -0.20 6.30 1 2 14 -0.60 9.40 1 2 14 2.30 10.50 -2 -2 -14 289.17 25.60 2 2 14 303.07 27.40 2 2 14 304.77 30.20 -3 -2 -14 6.90 7.10 3 2 14 -6.70 10.40 3 2 14 3.30 10.10 -4 -2 -14 -10.80 6.50 4 2 14 11.30 10.10 4 2 14 -5.80 10.30 1 -3 -14 9.70 7.30 -1 3 14 9.00 11.40 -1 3 14 0.70 6.30 -1 3 14 6.10 11.80 0 -3 -14 3.40 6.70 0 -3 -14 -6.10 5.30 0 3 14 -4.60 10.80 0 3 14 2.10 7.80 0 3 14 -0.10 10.70 0 3 14 -8.90 10.70 -1 -3 -14 272.07 24.80 -1 -3 -14 275.67 17.70 1 3 14 231.28 18.70 1 3 14 271.77 28.10 1 3 14 315.77 26.90 -2 -3 -14 237.48 21.70 2 3 14 288.97 27.00 2 3 14 216.38 25.90 -3 -3 -14 259.27 23.50 3 3 14 201.58 26.00 3 3 14 203.08 25.60 -4 -3 -14 93.59 15.00 4 3 14 113.49 20.40 4 3 14 96.49 19.10 1 -4 -14 163.78 19.80 -1 4 14 204.58 25.90 -1 4 14 181.88 17.50 0 -4 -14 8.80 5.50 0 -4 -14 13.40 8.50 0 4 14 28.00 12.40 0 4 14 3.50 8.70 0 4 14 21.60 13.40 0 4 14 11.70 8.40 -1 -4 -14 73.69 10.00 -1 -4 -14 58.59 11.80 1 4 14 73.89 14.40 1 4 14 57.89 16.10 1 4 14 78.09 11.70 -2 -4 -14 18.60 8.50 2 4 14 33.20 10.90 2 4 14 33.30 13.00 -3 -4 -14 -8.10 7.40 3 4 14 -8.70 8.90 3 4 14 3.70 11.10 4 4 14 -3.40 11.40 4 4 14 3.80 11.10 0 -5 -14 17.30 10.10 0 -5 -14 2.10 6.00 0 5 14 20.40 12.90 0 5 14 2.40 8.60 0 5 14 -17.60 11.70 0 5 14 3.70 8.80 -1 -5 -14 226.98 16.90 -1 -5 -14 214.48 23.90 1 5 14 250.37 24.50 1 5 14 227.38 25.20 1 5 14 207.08 18.90 -2 -5 -14 -7.50 7.40 -2 -5 -14 -4.20 2.50 2 5 14 -0.60 3.30 2 5 14 -15.90 8.80 2 5 14 -8.30 8.80 -3 -5 -14 70.79 14.10 3 5 14 86.79 18.00 0 -6 -14 -2.50 6.20 0 -6 -14 12.20 9.90 0 6 14 3.60 11.00 0 6 14 11.90 9.90 0 6 14 -5.00 10.60 -1 -6 -14 11.60 5.10 -1 -6 -14 9.80 9.30 1 6 14 15.30 12.10 1 6 14 22.10 12.30 -2 -6 -14 27.00 10.00 -2 -6 -14 25.10 4.60 2 6 14 28.90 12.50 2 6 14 45.60 13.60 2 6 14 27.50 6.20 -3 -6 -14 33.40 11.60 3 6 14 45.30 13.40 3 6 14 28.60 13.60 -1 -7 -14 97.59 15.90 -1 -7 -14 121.29 13.80 1 7 14 153.08 22.60 1 7 14 137.19 21.50 -2 -7 -14 29.20 5.70 -2 -7 -14 34.00 11.20 2 7 14 48.30 13.20 2 7 14 21.10 8.00 2 7 14 54.99 14.50 -1 1 -15 32.20 9.70 -1 1 -15 17.80 5.70 -1 1 -15 12.30 4.40 1 -1 15 15.50 10.30 1 -1 15 21.90 12.90 2 -1 15 2.70 9.00 2 -1 15 10.40 11.70 0 0 -15 8.10 8.80 0 0 -15 4.20 7.20 0 0 15 32.40 13.30 0 0 15 8.40 7.70 -1 0 -15 3.60 7.60 1 0 15 4.10 8.80 1 0 15 3.60 12.00 -2 0 -15 185.58 20.00 2 0 15 130.89 23.40 2 0 15 146.49 20.40 0 -1 -15 11.30 7.00 0 -1 -15 -2.40 6.60 0 1 15 7.30 8.50 0 1 15 24.70 13.30 -1 -1 -15 69.19 13.00 -1 -1 -15 73.49 8.70 -1 -1 -15 72.99 9.80 1 1 15 111.09 18.50 -2 -1 -15 12.90 8.60 2 1 15 2.40 9.40 2 1 15 14.60 13.30 0 -2 -15 18.10 7.90 0 -2 -15 27.90 10.00 0 2 15 29.50 10.20 0 2 15 48.10 15.40 0 2 15 20.10 10.40 -1 -2 -15 30.80 9.90 1 2 15 39.50 11.10 1 2 15 37.50 14.50 -2 -2 -15 54.89 10.10 2 2 15 73.79 18.50 2 2 15 54.89 14.20 -3 -2 -15 24.10 10.00 3 2 15 43.00 15.00 3 2 15 22.30 11.60 -1 -3 -15 0.40 7.70 -1 -3 -15 1.80 4.30 1 3 15 -11.60 5.70 1 3 15 -2.90 12.00 -2 -3 -15 -0.60 7.30 2 3 15 -1.00 8.10 2 3 15 7.50 9.60 -1 -4 -15 0.50 4.50 -1 -4 -15 -3.10 8.60 1 4 15 3.20 6.90 1 4 15 18.90 9.70 1 4 15 4.90 11.90 -2 -4 -15 293.77 28.00 2 4 15 312.57 29.00 2 4 15 279.67 27.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 7857 _shelx_res_file ; TITL SCABM_016_A_0m_a.res in P-1 SCABM_016_A_0m_a.res created by SHELXL-2019/1 at 14:02:12 on 30-Aug-2024 REM Old TITL SCABM_016_A_0m in P-1 REM SHELXT solution in P-1: R1 0.141, Rweak 0.003, Alpha 0.036 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C12 N4 O6 S2 CELL 0.71073 5.8838 11.6532 12.3276 84.722 78.442 81.940 ZERR 2.000 0.0008 0.0015 0.0016 0.006 0.005 0.005 LATT 1 SFAC C H N O S UNIT 22 34 6 16 4 TEMP 25 SIZE 0.12 0.354 1.213 L.S. 10 BOND $H ACTA CONF OMIT 0 1 0 HTAB C3 O24 EQIV $1 -x, -y+1, -z+1 HTAB C4 O24_$1 HTAB C13 O10 EQIV $2 -x+1, -y, -z+1 HTAB N1 O19_$2 HTAB N1 S21_$2 HTAB N1 O18 HTAB N1 O24 EQIV $3 -x+1, -y+1, -z HTAB N11 N16_$3 EQIV $4 x+1, y, z HTAB C23 O20_$4 EQIV $5 -x+1, -y+1, -z+1 HTAB O24 O10_$5 EQIV $6 x-1, y, z+1 HTAB O24 O15_$6 EQIV $7 -x, -y, -z+1 HTAB O24 O19_$7 HTAB O24 S21_$7 LIST 4 FMAP 2 PLAN 20 WGHT 0.014200 1.048600 FVAR 1.41212 C3 1 0.307493 0.367267 0.465489 11.00000 0.02973 0.03534 = 0.04076 0.00090 -0.00580 -0.00107 AFIX 43 H3 2 0.152494 0.384591 0.500421 11.00000 -1.20000 REM ##### REM ##### AFIX 0 C4 1 0.413152 0.445127 0.385617 11.00000 0.03787 0.03185 = 0.04156 0.00373 -0.01013 -0.00053 AFIX 43 H4 2 0.330192 0.515477 0.366393 11.00000 -1.20000 AFIX 0 C6 1 0.771497 0.312741 0.363279 11.00000 0.03027 0.04142 = 0.03538 -0.00005 -0.00072 -0.00261 AFIX 43 H6 2 0.926915 0.295236 0.329032 11.00000 -1.20000 AFIX 0 C7 1 0.665265 0.235400 0.443044 11.00000 0.03480 0.03197 = 0.03900 0.00209 -0.00312 0.00260 AFIX 43 H7 2 0.748077 0.165273 0.462965 11.00000 -1.20000 AFIX 0 C13 1 0.986914 0.313960 0.057801 11.00000 0.05028 0.05254 = 0.03806 -0.00127 -0.01209 0.00324 AFIX 43 H13 2 1.096502 0.312564 0.102944 11.00000 -1.20000 AFIX 0 REM ##### N1 3 0.321417 0.180496 0.573828 11.00000 0.03239 0.02980 = 0.03614 0.00047 -0.00293 -0.00433 AFIX 137 H1A 2 0.418354 0.149870 0.618726 11.00000 -1.50000 H1B 2 0.284132 0.124328 0.538887 11.00000 -1.50000 H1C 2 0.192294 0.216536 0.613491 11.00000 -1.50000 AFIX 0 C2 1 0.435639 0.263945 0.492249 11.00000 0.03314 0.02844 = 0.02769 -0.00206 -0.00622 -0.00753 C5 1 0.643822 0.416398 0.335074 11.00000 0.03591 0.03090 = 0.02620 -0.00029 -0.01012 -0.00892 S8 5 0.773274 0.514946 0.231735 11.00000 0.04239 0.03746 = 0.03092 0.00195 -0.00954 -0.01509 O9 4 0.665145 0.630108 0.254155 11.00000 0.06931 0.03060 = 0.04612 -0.00141 -0.01059 -0.01435 O10 4 1.020494 0.487695 0.219784 11.00000 0.04101 0.06541 = 0.04411 0.00699 -0.01055 -0.02328 N11 3 0.697225 0.489747 0.117230 11.00000 0.04718 0.03939 = 0.03146 -0.00116 -0.01422 -0.00082 AFIX 43 H11 2 0.595794 0.540280 0.092239 11.00000 -1.20000 AFIX 0 C12 1 0.783477 0.392815 0.056564 11.00000 0.04313 0.03855 = 0.02443 0.00586 -0.00445 -0.00969 C14 1 0.988118 0.241217 -0.020442 11.00000 0.06043 0.04711 = 0.03423 0.00150 -0.00391 -0.00070 O15 4 0.797788 0.271606 -0.067339 11.00000 0.06985 0.05048 = 0.03985 -0.01146 -0.01379 -0.00092 N16 3 0.664092 0.369264 -0.016092 11.00000 0.05291 0.04696 = 0.03662 -0.00704 -0.01161 -0.00162 C17 1 1.150778 0.140617 -0.065629 11.00000 0.08750 0.06283 = 0.05482 -0.01100 -0.00096 0.01575 AFIX 137 H17A 2 1.196861 0.090255 -0.005591 11.00000 -1.50000 H17B 2 1.286665 0.167607 -0.112248 11.00000 -1.50000 H17C 2 1.074268 0.098765 -0.108343 11.00000 -1.50000 REM ##### REM ##### REM ##### REM ##### REM ##### REM ##### REM ##### REM ##### REM ##### REM ##### REM ##### REM ##### AFIX 0 O18 4 0.231333 0.062153 0.406141 11.00000 0.09747 0.10113 = 0.04855 -0.02840 -0.00096 -0.05231 O19 4 0.356802 -0.095083 0.289794 11.00000 0.03999 0.03334 = 0.08010 0.00107 -0.01345 0.00016 O20 4 -0.040266 -0.003296 0.309848 11.00000 0.03231 0.05136 = 0.08008 0.00180 -0.01055 -0.00737 S21 5 0.196893 0.010133 0.311111 11.00000 0.03551 0.03171 = 0.03601 0.00050 -0.00723 -0.00727 O22 4 0.262049 0.097833 0.208788 11.00000 0.05300 0.06127 = 0.06285 0.03020 -0.01887 -0.01489 C23 1 0.491295 0.134773 0.190549 11.00000 0.06031 0.06624 = 0.06887 0.01934 -0.00695 -0.02637 AFIX 137 H23A 2 0.538503 0.158159 0.113494 11.00000 -1.50000 H23B 2 0.600925 0.071669 0.211404 11.00000 -1.50000 H23C 2 0.487101 0.199088 0.234604 11.00000 -1.50000 AFIX 0 O24 4 -0.106347 0.288809 0.677801 11.00000 0.04244 0.04251 = 0.04514 -0.00795 -0.00411 -0.01084 H24A 2 -0.102121 0.317375 0.730223 11.00000 -1.20000 H24B 2 -0.199378 0.241914 0.696120 11.00000 -1.20000 HKLF 4 REM SCABM_016_A_0m_a.res in P-1 REM wR2 = 0.1000, GooF = S = 1.058, Restrained GooF = 1.058 for all data REM R1 = 0.0430 for 2716 Fo > 4sig(Fo) and 0.0568 for all 3318 data REM 226 parameters refined using 0 restraints END WGHT 0.0135 1.0552 REM Highest difference peak 0.330, deepest hole -0.321, 1-sigma level 0.054 Q1 1 0.6878 0.4601 0.2916 11.00000 0.05 0.33 Q2 1 0.7743 0.6104 0.2125 11.00000 0.05 0.30 Q3 1 0.9074 0.4754 0.2042 11.00000 0.05 0.30 Q4 1 0.6965 0.1266 0.1790 11.00000 0.05 0.23 Q5 1 0.3069 -0.0712 0.3494 11.00000 0.05 0.23 Q6 1 0.5059 0.4098 0.3367 11.00000 0.05 0.23 Q7 1 0.2011 0.1049 0.3794 11.00000 0.05 0.22 Q8 1 1.1688 0.1430 -0.1363 11.00000 0.05 0.21 Q9 1 0.3732 0.0407 0.4004 11.00000 0.05 0.20 Q10 1 0.5583 0.4383 0.3718 11.00000 0.05 0.20 Q11 1 1.0926 0.4206 0.2108 11.00000 0.05 0.20 Q12 1 0.7996 0.4674 0.1405 11.00000 0.05 0.20 Q13 1 0.2241 0.1215 0.1786 11.00000 0.05 0.19 Q14 1 0.3470 0.0282 0.1554 11.00000 0.05 0.19 Q15 1 0.4001 0.3226 0.5016 11.00000 0.05 0.19 Q16 1 0.0858 0.1207 0.3353 11.00000 0.05 0.19 Q17 1 1.0796 0.6029 0.1363 11.00000 0.05 0.19 Q18 1 0.4012 0.2328 0.5267 11.00000 0.05 0.19 Q19 1 0.0319 0.0597 0.2605 11.00000 0.05 0.19 Q20 1 0.4554 0.2207 0.1547 11.00000 0.05 0.18 ; _shelx_res_checksum 40464 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 _atom_site_disorder_assembly _atom_site_disorder_group C C3 0.3075(4) 0.3673(2) 0.4655(2) 0.0359(5) Uani d 1 . . H H3 0.152494 0.384591 0.500421 0.043 Uiso calc 1 . . C C4 0.4132(4) 0.4451(2) 0.3856(2) 0.0375(5) Uani d 1 . . H H4 0.330192 0.515477 0.366393 0.045 Uiso calc 1 . . C C6 0.7715(4) 0.3127(2) 0.3633(2) 0.0368(5) Uani d 1 . . H H6 0.926915 0.295236 0.329032 0.044 Uiso calc 1 . . C C7 0.6653(4) 0.2354(2) 0.4430(2) 0.0367(5) Uani d 1 . . H H7 0.748077 0.165273 0.462965 0.044 Uiso calc 1 . . C C13 0.9869(5) 0.3140(2) 0.0578(2) 0.0475(6) Uani d 1 . . H H13 1.096502 0.312564 0.102944 0.057 Uiso calc 1 . . N N1 0.3214(3) 0.18050(16) 0.57383(16) 0.0334(4) Uani d 1 . . H H1A 0.418354 0.149870 0.618726 0.050 Uiso calc 1 . . H H1B 0.284132 0.124328 0.538887 0.050 Uiso calc 1 . . H H1C 0.192294 0.216536 0.613491 0.050 Uiso calc 1 . . C C2 0.4356(4) 0.26394(19) 0.49225(18) 0.0293(5) Uani d 1 . . C C5 0.6438(4) 0.41640(19) 0.33507(18) 0.0301(5) Uani d 1 . . S S8 0.77327(11) 0.51495(5) 0.23174(5) 0.03585(16) Uani d 1 . . O O9 0.6651(4) 0.63011(15) 0.25416(15) 0.0480(5) Uani d 1 . . O O10 1.0205(3) 0.48770(17) 0.21978(15) 0.0489(5) Uani d 1 . . N N11 0.6972(4) 0.48975(18) 0.11723(16) 0.0389(5) Uani d 1 . . H H11 0.595794 0.540280 0.092239 0.047 Uiso calc 1 . . C C12 0.7835(4) 0.3928(2) 0.05656(18) 0.0357(5) Uani d 1 . . C C14 0.9881(5) 0.2412(2) -0.0204(2) 0.0488(7) Uani d 1 . . O O15 0.7978(4) 0.27161(17) -0.06734(15) 0.0530(5) Uani d 1 . . N N16 0.6641(4) 0.36926(19) -0.01609(18) 0.0452(5) Uani d 1 . . C C17 1.1508(7) 0.1406(3) -0.0656(3) 0.0721(10) Uani d 1 . . H H17A 1.196861 0.090255 -0.005591 0.108 Uiso calc 1 . . H H17B 1.286665 0.167607 -0.112248 0.108 Uiso calc 1 . . H H17C 1.074268 0.098765 -0.108343 0.108 Uiso calc 1 . . O O18 0.2313(5) 0.0622(2) 0.40614(18) 0.0788(8) Uani d 1 . . O O19 0.3568(3) -0.09508(15) 0.28979(18) 0.0516(5) Uani d 1 . . O O20 -0.0403(3) -0.00330(17) 0.30985(18) 0.0548(5) Uani d 1 . . S S21 0.19689(10) 0.01013(5) 0.31111(5) 0.03422(16) Uani d 1 . . O O22 0.2620(4) 0.09783(18) 0.20879(18) 0.0594(6) Uani d 1 . . C C23 0.4913(6) 0.1348(3) 0.1905(3) 0.0656(9) Uani d 1 . . H H23A 0.538503 0.158159 0.113494 0.098 Uiso calc 1 . . H H23B 0.600925 0.071669 0.211404 0.098 Uiso calc 1 . . H H23C 0.487101 0.199088 0.234604 0.098 Uiso calc 1 . . O O24 -0.1063(3) 0.28881(17) 0.67780(16) 0.0431(4) Uani d 1 . . H H24A -0.102(5) 0.317(3) 0.730(3) 0.052 Uiso d 1 . . H H24B -0.199(5) 0.242(3) 0.696(2) 0.052 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 C3 0.0297(11) 0.0353(12) 0.0408(13) -0.0011(9) -0.0058(10) 0.0009(10) C4 0.0379(13) 0.0318(12) 0.0416(13) -0.0005(10) -0.0101(11) 0.0037(10) C6 0.0303(12) 0.0414(13) 0.0354(12) -0.0026(10) -0.0007(10) 0.0000(10) C7 0.0348(12) 0.0320(12) 0.0390(13) 0.0026(10) -0.0031(10) 0.0021(10) C13 0.0503(16) 0.0525(16) 0.0381(14) 0.0032(13) -0.0121(12) -0.0013(12) N1 0.0324(10) 0.0298(10) 0.0361(10) -0.0043(8) -0.0029(8) 0.0005(8) C2 0.0331(11) 0.0284(11) 0.0277(11) -0.0075(9) -0.0062(9) -0.0021(8) C5 0.0359(12) 0.0309(11) 0.0262(11) -0.0089(9) -0.0101(9) -0.0003(9) S8 0.0424(3) 0.0375(3) 0.0309(3) -0.0151(3) -0.0095(2) 0.0020(2) O9 0.0693(13) 0.0306(9) 0.0461(10) -0.0144(8) -0.0106(9) -0.0014(8) O10 0.0410(10) 0.0654(12) 0.0441(10) -0.0233(9) -0.0105(8) 0.0070(9) N11 0.0472(12) 0.0394(11) 0.0315(10) -0.0008(9) -0.0142(9) -0.0012(8) C12 0.0431(13) 0.0385(13) 0.0244(11) -0.0097(10) -0.0045(10) 0.0059(9) C14 0.0604(17) 0.0471(15) 0.0342(13) -0.0007(13) -0.0039(12) 0.0015(11) O15 0.0699(13) 0.0505(11) 0.0399(10) -0.0009(10) -0.0138(9) -0.0115(9) N16 0.0529(13) 0.0470(13) 0.0366(11) -0.0016(10) -0.0116(10) -0.0070(10) C17 0.087(3) 0.063(2) 0.0548(19) 0.0158(18) -0.0010(17) -0.0110(16) O18 0.0975(18) 0.1011(19) 0.0486(12) -0.0523(15) -0.0010(12) -0.0284(12) O19 0.0400(10) 0.0333(9) 0.0801(14) 0.0002(8) -0.0135(10) 0.0011(9) O20 0.0323(10) 0.0514(11) 0.0801(15) -0.0074(8) -0.0105(9) 0.0018(10) S21 0.0355(3) 0.0317(3) 0.0360(3) -0.0073(2) -0.0072(2) 0.0005(2) O22 0.0530(12) 0.0613(13) 0.0628(13) -0.0149(10) -0.0189(10) 0.0302(10) C23 0.0603(19) 0.066(2) 0.069(2) -0.0264(16) -0.0070(16) 0.0193(16) O24 0.0424(10) 0.0425(11) 0.0451(11) -0.0108(8) -0.0041(9) -0.0080(8) 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' 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 C2 C3 C4 . . 119.0(2) ? C2 C3 H3 . . 120.5 ? C4 C3 H3 . . 120.5 ? C5 C4 C3 . . 119.0(2) ? C5 C4 H4 . . 120.5 ? C3 C4 H4 . . 120.5 ? C5 C6 C7 . . 119.3(2) ? C5 C6 H6 . . 120.4 ? C7 C6 H6 . . 120.4 ? C2 C7 C6 . . 118.9(2) ? C2 C7 H7 . . 120.5 ? C6 C7 H7 . . 120.5 ? C14 C13 C12 . . 104.7(2) ? C14 C13 H13 . . 127.6 ? C12 C13 H13 . . 127.6 ? C2 N1 H1A . . 109.5 ? C2 N1 H1B . . 109.5 ? H1A N1 H1B . . 109.5 ? C2 N1 H1C . . 109.5 ? H1A N1 H1C . . 109.5 ? H1B N1 H1C . . 109.5 ? C7 C2 C3 . . 122.3(2) ? C7 C2 N1 . . 118.9(2) ? C3 C2 N1 . . 118.9(2) ? C4 C5 C6 . . 121.5(2) ? C4 C5 S8 . . 118.33(17) ? C6 C5 S8 . . 120.15(18) ? O10 S8 O9 . . 119.97(12) ? O10 S8 N11 . . 108.68(11) ? O9 S8 N11 . . 104.56(11) ? O10 S8 C5 . . 107.58(11) ? O9 S8 C5 . . 109.04(11) ? N11 S8 C5 . . 106.22(10) ? C12 N11 S8 . . 125.09(17) ? C12 N11 H11 . . 117.5 ? S8 N11 H11 . . 117.5 ? N16 C12 N11 . . 117.4(2) ? N16 C12 C13 . . 112.3(2) ? N11 C12 C13 . . 130.3(2) ? C13 C14 O15 . . 109.8(2) ? C13 C14 C17 . . 134.3(3) ? O15 C14 C17 . . 115.9(3) ? C14 O15 N16 . . 108.66(19) ? C12 N16 O15 . . 104.5(2) ? C14 C17 H17A . . 109.5 ? C14 C17 H17B . . 109.5 ? H17A C17 H17B . . 109.5 ? C14 C17 H17C . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? O18 S21 O20 . . 115.06(14) ? O18 S21 O19 . . 111.33(15) ? O20 S21 O19 . . 113.41(11) ? O18 S21 O22 . . 106.60(14) ? O20 S21 O22 . . 103.29(12) ? O19 S21 O22 . . 106.17(12) ? C23 O22 S21 . . 117.03(18) ? O22 C23 H23A . . 109.5 ? O22 C23 H23B . . 109.5 ? H23A C23 H23B . . 109.5 ? O22 C23 H23C . . 109.5 ? H23A C23 H23C . . 109.5 ? H23B C23 H23C . . 109.5 ? H24A O24 H24B . . 106(3) ? 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 C3 C2 . 1.378(3) ? C3 C4 . 1.388(3) ? C3 H3 . 0.9300 ? C4 C5 . 1.384(3) ? C4 H4 . 0.9300 ? C6 C5 . 1.385(3) ? C6 C7 . 1.385(3) ? C6 H6 . 0.9300 ? C7 C2 . 1.374(3) ? C7 H7 . 0.9300 ? C13 C14 . 1.340(4) ? C13 C12 . 1.405(4) ? C13 H13 . 0.9300 ? N1 C2 . 1.463(3) ? N1 H1A . 0.8900 ? N1 H1B . 0.8900 ? N1 H1C . 0.8900 ? C5 S8 . 1.763(2) ? S8 O10 . 1.4253(19) ? S8 O9 . 1.4285(19) ? S8 N11 . 1.626(2) ? N11 C12 . 1.391(3) ? N11 H11 . 0.8600 ? C12 N16 . 1.312(3) ? C14 O15 . 1.351(3) ? C14 C17 . 1.481(4) ? O15 N16 . 1.412(3) ? C17 H17A . 0.9600 ? C17 H17B . 0.9600 ? C17 H17C . 0.9600 ? O18 S21 . 1.429(2) ? O19 S21 . 1.4472(18) ? O20 S21 . 1.4291(18) ? S21 O22 . 1.5689(19) ? O22 C23 . 1.442(3) ? C23 H23A . 0.9600 ? C23 H23B . 0.9600 ? C23 H23C . 0.9600 ? O24 H24A . 0.76(3) ? O24 H24B . 0.81(3) ? 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 C3 H3 O24 . 0.93 2.65 3.353(3) 132.6 yes C4 H4 O24 2_566 0.93 2.54 3.469(3) 177.3 yes C13 H13 O10 . 0.93 2.54 3.023(3) 112.5 yes N1 H1A O19 2_656 0.89 1.91 2.800(3) 174.9 yes N1 H1A S21 2_656 0.89 2.94 3.774(2) 156.4 yes N1 H1B O18 . 0.89 1.95 2.761(3) 151.7 yes N1 H1C O24 . 0.89 1.89 2.772(3) 170.3 yes N11 H11 N16 2_665 0.86 2.07 2.912(3) 167.3 yes C23 H23B O20 1_655 0.96 2.65 3.506(4) 149.2 yes O24 H24A O10 2_666 0.76(3) 2.54(3) 3.140(3) 137(3) yes O24 H24A O15 1_456 0.76(3) 2.47(3) 3.072(3) 137(3) yes O24 H24B O19 2_556 0.81(3) 2.03(3) 2.821(3) 163(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 C2 C3 C4 C5 . . . . 0.2(4) ? C5 C6 C7 C2 . . . . -0.1(4) ? C6 C7 C2 C3 . . . . -0.4(4) ? C6 C7 C2 N1 . . . . 178.0(2) ? C4 C3 C2 C7 . . . . 0.4(4) ? C4 C3 C2 N1 . . . . -178.0(2) ? C3 C4 C5 C6 . . . . -0.7(4) ? C3 C4 C5 S8 . . . . 178.67(18) ? C7 C6 C5 C4 . . . . 0.7(4) ? C7 C6 C5 S8 . . . . -178.69(18) ? C4 C5 S8 O10 . . . . 160.72(18) ? C6 C5 S8 O10 . . . . -19.9(2) ? C4 C5 S8 O9 . . . . 29.1(2) ? C6 C5 S8 O9 . . . . -151.45(19) ? C4 C5 S8 N11 . . . . -83.0(2) ? C6 C5 S8 N11 . . . . 96.4(2) ? O10 S8 N11 C12 . . . . 43.0(2) ? O9 S8 N11 C12 . . . . 172.3(2) ? C5 S8 N11 C12 . . . . -72.5(2) ? S8 N11 C12 N16 . . . . 162.55(18) ? S8 N11 C12 C13 . . . . -19.1(4) ? C14 C13 C12 N16 . . . . 1.1(3) ? C14 C13 C12 N11 . . . . -177.3(2) ? C12 C13 C14 O15 . . . . -0.4(3) ? C12 C13 C14 C17 . . . . 178.0(3) ? C13 C14 O15 N16 . . . . -0.4(3) ? C17 C14 O15 N16 . . . . -179.2(2) ? N11 C12 N16 O15 . . . . 177.28(19) ? C13 C12 N16 O15 . . . . -1.4(3) ? C14 O15 N16 C12 . . . . 1.1(3) ? O18 S21 O22 C23 . . . . 55.1(3) ? O20 S21 O22 C23 . . . . 176.7(2) ? O19 S21 O22 C23 . . . . -63.7(3) ?