#------------------------------------------------------------------------------ #$Date: 2018-01-13 08:34:18 +0200 (Sat, 13 Jan 2018) $ #$Revision: 205186 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/86/1548678.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_1548678 loop_ _publ_author_name 'Prabu, P.' 'Thiruvalluvar, A.' 'Ramachandra Raja, C.' _publ_section_title ; 1-Carboxy-2-hydroxypropan-1-aminium 4-methylbenzenesulfonate monohydrate ; _journal_coeditor_code TK4043 _journal_issue 1 _journal_name_full IUCrData _journal_page_first x171848 _journal_paper_doi 10.1107/S241431461701848X _journal_volume 3 _journal_year 2018 _chemical_formula_iupac 'C4 H10 N O3 +, C7 H7 O3 S -, H2 O' _chemical_formula_moiety 'C4 H10 N O3 +, C7 H7 O3 S -, H2 O' _chemical_formula_sum 'C11 H19 N O7 S' _chemical_formula_weight 309.33 _chemical_melting_point 356 _chemical_name_systematic ; 1-Carboxy-2-hydroxypropan-1-aminium 4-methylbenzenesulfonate monohydrate ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/1 _cell_angle_alpha 90 _cell_angle_beta 92.161(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.0762(4) _cell_length_b 6.2486(4) _cell_length_c 14.5096(10) _cell_measurement_reflns_used 3667 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.25 _cell_measurement_theta_min 2.80 _cell_volume 731.71(8) _computing_cell_refinement ; APEX2 and SAINT (Bruker, 2004) ; _computing_data_collection ; APEX2 (Bruker, 2004) ; _computing_data_reduction ; SAINT and XPREP (Bruker, 2004) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2008) ; _computing_publication_material ; SHELXL2018/1 (Sheldrick, 2015b), PLATON (Spek, 2009), and publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018/1 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measurement_device_type 'Bruker Kappa APEXII CCD' _diffrn_measurement_method '\w and \f scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 8712 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.891 _diffrn_reflns_theta_min 2.524 _exptl_absorpt_coefficient_mu 0.251 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2004) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.404 _exptl_crystal_description block _exptl_crystal_F_000 328 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.185 _refine_diff_density_min -0.193 _refine_ls_abs_structure_details ; Flack x determined using 1035 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013). ; _refine_ls_abs_structure_Flack 0.06(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 203 _refine_ls_number_reflns 3347 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0371 _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^)+(0.0332P)^2^+0.1196P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.0811 _reflns_number_gt 2705 _reflns_number_total 3347 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file tk4043sup1.cif _cod_data_source_block I _cod_database_code 1548678 _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 0.963 _shelx_estimated_absorpt_t_max 0.975 _shelx_hkl_file ; -1 0 0 184.38 5.60 1 0 0 217.98 5.70 -1 0 0 253.87 5.80 2 0 0 8061.69 175.88 -2 0 0 8205.08 174.88 -2 0 0 8371.66 176.48 -2 0 0 8362.96 174.78 -3 0 0 1641.64 36.40 -3 0 0 1632.14 36.30 -3 0 0 1616.84 36.10 3 0 0 1543.85 36.20 -3 0 0 1604.84 36.60 4 0 0 7.30 1.90 -4 0 0 14.70 2.50 -4 0 0 17.70 2.60 -4 0 0 12.90 2.50 4 0 0 17.30 3.00 -4 0 0 12.80 2.70 -5 0 0 92.89 5.30 5 0 0 87.39 6.30 -5 0 0 82.79 5.20 -5 0 0 90.69 5.80 -6 0 0 213.58 8.40 -6 0 0 201.58 8.70 6 0 0 216.38 9.60 -6 0 0 186.48 9.10 7 0 0 618.14 19.10 -7 0 0 587.14 18.80 -8 0 0 2.70 3.70 8 0 0 -2.60 4.00 9 0 0 36.50 6.50 -9 0 0 49.10 6.80 -10 0 0 6.30 4.90 0 -1 0 -0.80 1.40 0 -1 0 3.20 1.60 0 -1 0 -1.80 1.10 0 -1 0 -1.60 1.20 0 1 0 -3.40 1.00 0 1 0 -0.80 1.30 0 1 0 -2.10 1.10 -1 -1 0 2618.74 57.89 -1 -1 0 2577.64 57.79 -1 -1 0 2654.53 57.79 -1 -1 0 2555.74 57.59 1 -1 0 2625.34 55.99 1 -1 0 2664.23 55.79 -1 1 0 2642.74 55.99 1 1 0 2571.14 57.79 1 1 0 2626.64 57.89 -1 1 0 2619.64 55.99 1 1 0 2682.03 57.79 -1 1 0 2679.73 55.99 -2 -1 0 4959.90 106.39 -2 -1 0 5003.40 106.29 -2 -1 0 4825.82 106.49 -2 -1 0 4819.72 106.39 2 1 0 4914.01 106.39 2 1 0 4944.31 106.39 -3 -1 0 111.29 6.30 -3 -1 0 108.79 6.00 -3 -1 0 104.49 5.90 -3 -1 0 107.49 6.40 3 1 0 101.09 6.10 3 1 0 102.39 6.30 -3 1 0 99.09 3.00 -4 -1 0 200.58 8.70 -4 -1 0 204.08 8.70 4 -1 0 181.18 5.60 -4 -1 0 195.48 9.10 -4 1 0 192.98 5.80 4 1 0 204.88 9.30 4 1 0 205.48 9.20 -4 1 0 194.38 6.00 -5 -1 0 776.22 21.90 5 -1 0 753.12 18.00 -5 -1 0 722.23 21.40 -5 -1 0 728.13 22.20 -5 1 0 776.22 16.90 -5 1 0 758.92 18.50 -5 1 0 737.63 16.80 -5 1 0 739.73 18.20 5 1 0 762.72 22.30 5 1 0 760.92 22.10 -6 -1 0 13.70 4.20 6 -1 0 9.20 2.70 -6 -1 0 9.00 3.50 -6 -1 0 20.20 4.20 6 1 0 10.00 4.20 -6 1 0 9.40 1.50 -6 1 0 4.80 2.00 6 1 0 13.30 4.60 -6 1 0 9.10 1.50 -6 1 0 12.40 2.70 7 -1 0 172.48 7.30 7 -1 0 157.78 6.80 -7 -1 0 171.08 9.70 -7 -1 0 178.08 11.00 -7 1 0 163.68 7.20 7 1 0 155.98 9.80 7 1 0 177.08 11.60 -8 -1 0 85.99 9.40 8 -1 0 68.19 5.40 8 1 0 88.29 9.70 -8 1 0 80.59 5.60 -9 -1 0 3.50 5.20 9 1 0 7.60 6.60 -10 -1 0 28.40 7.20 10 1 0 -2.00 6.10 0 -2 0 1837.12 42.00 0 -2 0 1810.52 42.20 0 -2 0 1774.62 41.90 0 -2 0 1825.82 42.20 0 2 0 1894.71 42.40 0 2 0 1832.82 42.20 0 2 0 1821.82 42.30 -1 -2 0 875.31 22.80 -1 -2 0 852.51 23.00 1 -2 0 892.61 21.10 -1 -2 0 855.41 22.70 1 -2 0 881.11 21.20 1 -2 0 858.31 21.30 1 -2 0 880.11 21.10 -1 -2 0 843.22 22.90 1 2 0 846.62 23.00 -1 2 0 882.41 21.40 -1 2 0 894.61 21.40 1 2 0 869.61 23.00 -1 2 0 898.91 21.50 1 2 0 883.61 23.20 2 -2 0 1414.26 30.30 -2 -2 0 1425.76 34.70 -2 -2 0 1305.07 33.90 -2 -2 0 1437.56 34.50 2 -2 0 1367.26 30.80 -2 -2 0 1372.56 34.70 2 -2 0 1390.76 30.30 -2 2 0 1359.56 31.00 2 2 0 1345.07 34.40 -2 2 0 1372.46 31.20 2 2 0 1352.66 34.60 -2 2 0 1370.56 30.80 -3 -2 0 1114.79 30.40 -3 -2 0 1139.99 29.90 3 -2 0 1112.39 24.40 -3 -2 0 1127.49 30.10 3 -2 0 1118.09 24.50 3 2 0 1160.28 30.40 -3 2 0 1109.49 24.90 -3 2 0 1209.78 25.30 3 2 0 1072.89 29.80 -4 -2 0 911.81 26.40 -4 -2 0 927.81 27.10 -4 -2 0 948.31 26.50 4 2 0 930.31 27.00 4 2 0 915.81 26.70 -5 -2 0 360.06 14.60 -5 -2 0 348.87 15.20 -5 -2 0 390.36 16.20 5 2 0 368.86 15.40 5 2 0 370.56 15.50 -6 -2 0 139.99 10.70 -6 -2 0 148.99 10.00 6 2 0 148.99 11.20 6 2 0 152.08 10.60 -7 -2 0 361.26 15.80 -7 -2 0 358.66 17.20 7 2 0 337.37 16.90 7 2 0 354.66 16.30 -8 -2 0 91.59 11.30 8 2 0 67.39 10.10 -9 -2 0 11.00 6.50 9 2 0 5.90 7.50 -10 -2 0 74.39 11.10 10 2 0 41.90 10.40 0 -3 0 -7.10 2.50 0 -3 0 -1.10 2.70 0 -3 0 -4.20 2.40 0 3 0 2.10 2.70 0 3 0 0.30 2.90 0 3 0 -0.20 2.20 -1 -3 0 462.15 15.80 -1 -3 0 439.86 15.50 1 -3 0 444.86 13.70 1 -3 0 452.05 14.10 -1 -3 0 426.46 15.00 1 -3 0 426.36 13.60 1 3 0 458.45 15.80 -1 3 0 454.65 14.10 -1 3 0 437.46 13.90 1 3 0 424.86 15.30 1 3 0 444.86 15.50 -1 3 0 445.96 14.20 2 -3 0 250.97 8.70 -2 -3 0 263.57 12.20 -2 -3 0 269.67 12.40 2 -3 0 267.97 9.30 2 -3 0 269.17 8.80 2 -3 0 257.27 9.40 2 3 0 285.97 12.50 -2 3 0 292.97 10.10 2 3 0 281.27 12.50 -2 3 0 289.07 9.70 -2 3 0 281.57 9.60 -3 -3 0 185.28 11.20 3 -3 0 189.18 7.00 3 -3 0 203.38 5.60 3 -3 0 185.98 5.50 -3 -3 0 205.28 11.10 -3 3 0 187.48 7.00 3 3 0 173.58 10.40 3 3 0 190.68 11.30 -3 3 0 190.78 6.70 -3 3 0 190.98 7.40 4 -3 0 263.97 6.80 4 -3 0 248.78 6.70 -4 -3 0 284.47 13.50 -4 -3 0 262.37 13.60 4 3 0 262.27 13.50 -4 3 0 257.17 8.00 4 3 0 255.87 13.40 -5 -3 0 140.49 11.40 -5 -3 0 138.59 10.60 5 3 0 148.29 11.60 5 3 0 143.69 11.10 -6 -3 0 94.79 11.00 -6 -3 0 94.09 10.00 6 3 0 84.19 10.30 6 3 0 110.99 11.40 -7 -3 0 30.70 7.40 -7 -3 0 18.10 7.70 7 3 0 10.10 7.30 7 3 0 31.60 7.30 -8 -3 0 81.79 12.00 8 3 0 80.99 11.70 -9 -3 0 11.50 7.90 9 3 0 3.50 8.40 0 -4 0 371.36 14.50 0 -4 0 356.66 13.90 0 -4 0 351.16 14.60 0 4 0 362.06 14.60 0 4 0 359.06 14.80 -1 -4 0 160.68 10.50 1 -4 0 164.08 8.60 1 -4 0 183.28 9.40 1 -4 0 186.98 9.90 -1 -4 0 178.98 10.70 -1 4 0 164.68 9.20 -1 4 0 167.98 9.60 1 4 0 171.28 10.30 -1 4 0 174.58 9.10 1 4 0 173.68 10.80 -2 -4 0 49.50 7.30 2 -4 0 40.50 5.20 2 -4 0 46.00 5.10 -2 -4 0 58.19 8.40 2 -4 0 50.59 5.30 2 4 0 52.39 7.30 -2 4 0 45.60 5.60 -2 4 0 57.69 5.90 2 4 0 48.60 7.40 -3 -4 0 599.84 22.40 3 -4 0 600.74 16.10 3 -4 0 620.24 17.40 -3 -4 0 619.84 22.90 3 -4 0 616.74 17.50 -3 4 0 595.14 18.30 -3 4 0 595.74 17.30 3 4 0 596.14 22.60 3 4 0 612.34 22.80 4 -4 0 329.27 10.20 4 -4 0 334.67 10.40 -4 -4 0 307.37 16.90 -4 -4 0 331.67 16.90 4 4 0 339.57 17.40 -4 4 0 322.27 11.40 4 4 0 326.47 17.00 -5 -4 0 62.09 10.50 -5 -4 0 69.69 10.30 5 4 0 53.99 9.60 5 4 0 60.09 10.30 -6 -4 0 139.09 13.80 -6 -4 0 104.99 12.00 6 4 0 117.29 13.40 6 4 0 142.19 13.20 -7 -4 0 31.80 7.80 -7 -4 0 61.09 10.90 7 4 0 46.30 9.70 7 4 0 44.70 10.20 -8 -4 0 11.30 8.70 8 4 0 -17.30 6.90 -9 -4 0 34.20 11.40 9 4 0 20.50 11.40 0 -5 0 -9.50 4.00 0 -5 0 -4.50 3.90 0 5 0 -5.30 4.00 0 5 0 0.90 4.60 -1 -5 0 264.97 14.70 1 -5 0 238.98 12.30 1 -5 0 251.57 12.90 1 -5 0 224.38 11.60 -1 -5 0 254.77 14.30 1 5 0 245.88 14.30 1 5 0 231.38 14.00 -1 5 0 244.18 12.90 -1 5 0 228.68 13.20 2 -5 0 204.48 10.40 -2 -5 0 201.78 13.70 2 -5 0 199.38 10.30 2 -5 0 172.68 10.70 -2 -5 0 194.98 13.80 -2 5 0 192.98 11.50 -2 5 0 201.58 11.10 2 5 0 211.28 13.90 2 5 0 186.08 13.50 3 -5 0 21.20 4.90 -3 -5 0 30.90 7.90 -3 -5 0 24.80 8.10 3 5 0 30.10 8.30 -3 5 0 27.80 5.70 3 5 0 29.40 8.20 4 -5 0 218.28 9.70 -4 -5 0 203.58 15.50 -4 -5 0 198.68 15.40 -4 5 0 199.98 10.40 4 5 0 202.98 15.20 4 5 0 238.98 16.30 -5 -5 0 32.20 8.50 5 -5 0 27.70 3.50 -5 -5 0 29.40 9.10 5 5 0 18.90 8.70 -5 5 0 29.50 4.30 5 5 0 30.70 9.00 -6 -5 0 18.40 7.90 -6 -5 0 19.80 8.70 6 5 0 17.90 9.00 6 5 0 12.90 7.90 -7 -5 0 15.80 7.50 -7 -5 0 14.10 9.40 7 5 0 1.80 9.40 7 5 0 22.80 8.80 -8 -5 0 19.60 11.90 8 5 0 5.90 10.20 0 -6 0 229.58 14.80 0 -6 0 230.78 14.40 0 6 0 197.08 14.40 0 6 0 211.38 15.10 -1 -6 0 48.50 9.10 -1 -6 0 42.80 8.60 1 -6 0 50.99 8.50 1 -6 0 37.10 7.70 1 6 0 43.20 9.20 -1 6 0 40.80 8.00 -1 6 0 28.60 7.30 1 6 0 49.90 9.80 -2 -6 0 165.88 14.60 2 -6 0 155.18 11.50 -2 -6 0 147.79 14.00 2 6 0 153.38 14.60 -2 6 0 161.98 12.20 2 6 0 144.09 14.20 -3 -6 0 146.69 14.60 -3 -6 0 168.38 15.20 3 -6 0 172.08 11.20 -3 6 0 151.68 11.40 3 6 0 145.59 15.20 3 6 0 163.58 15.00 4 -6 0 64.89 7.70 -4 -6 0 66.49 11.70 -4 -6 0 68.59 12.80 4 6 0 62.49 12.20 -4 6 0 61.19 8.30 4 6 0 54.79 11.40 -5 -6 0 12.50 7.70 -5 -6 0 -11.50 7.20 5 6 0 13.10 8.40 -5 6 0 3.40 3.70 5 6 0 -4.70 7.60 -6 -6 0 18.90 8.40 -6 -6 0 11.90 9.70 6 6 0 5.40 9.90 6 6 0 0.70 7.70 -7 -6 0 19.10 9.30 7 6 0 -4.30 10.00 0 -7 0 3.00 6.60 0 7 0 5.90 7.20 1 -7 0 34.60 8.70 -1 -7 0 47.20 9.60 -1 -7 0 40.90 9.30 1 7 0 34.70 9.90 1 7 0 30.90 9.20 -1 7 0 57.59 10.90 -2 -7 0 52.09 11.60 2 -7 0 32.40 8.10 -2 -7 0 52.39 11.40 2 7 0 38.30 10.10 -2 7 0 43.10 9.50 2 7 0 34.60 10.40 -3 -7 0 21.50 9.90 -3 -7 0 6.90 8.30 3 -7 0 2.50 5.20 3 7 0 7.10 7.50 -3 7 0 7.60 5.70 3 7 0 5.60 8.20 4 -7 0 12.50 5.10 -4 -7 0 5.40 9.40 -4 -7 0 25.20 10.50 4 7 0 -6.80 6.10 -4 7 0 6.00 5.40 4 7 0 -1.20 8.70 -5 -7 0 14.00 10.60 -5 -7 0 15.00 9.60 5 7 0 -13.90 8.30 5 7 0 19.40 9.30 0 -8 0 29.60 9.80 0 8 0 52.59 11.80 -1 -8 0 18.60 9.80 1 -8 0 11.40 8.60 -1 8 0 7.50 8.30 1 8 0 33.40 10.60 -10 0 1 -3.20 4.00 -9 0 1 135.69 9.30 9 0 -1 106.09 9.60 8 0 -1 134.39 9.50 -8 0 1 130.79 8.80 -7 0 1 81.09 7.00 7 0 -1 68.59 7.60 -6 0 1 67.19 5.30 6 0 -1 54.99 6.30 -6 0 1 60.39 5.70 -6 0 1 61.39 4.90 -5 0 1 654.53 17.30 -5 0 1 635.64 17.70 -5 0 1 628.64 17.90 5 0 -1 636.34 18.10 -4 0 1 3.30 2.20 4 0 -1 2.30 1.50 -4 0 1 2.40 1.90 -4 0 1 4.40 1.90 4 0 -1 -0.50 2.30 -4 0 1 3.50 1.90 -3 0 1 878.31 20.90 -3 0 1 855.01 21.10 -3 0 1 875.71 20.90 -3 0 1 887.61 21.20 3 0 -1 877.21 21.20 -2 0 1 9939.81 209.48 -2 0 1 9862.21 209.78 2 0 -1 9908.41 208.18 2 0 -1 9999.00 209.58 2 0 -1 9835.62 209.18 -2 0 1 9823.82 209.88 -2 0 1 9782.12 211.98 1 0 -1 524.05 12.00 -1 0 1 474.85 11.90 -1 0 1 540.05 12.30 1 0 -1 538.95 12.20 -1 0 1 543.85 12.20 1 0 -1 543.35 12.10 -1 0 1 467.15 12.00 0 0 1 -0.90 0.20 0 0 1 -1.00 0.40 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-4 3 16 -2.20 7.80 -3 -3 16 1.00 9.30 -3 -3 16 0.50 7.80 -3 3 16 12.30 8.80 3 3 -16 4.90 8.20 -2 -3 16 36.00 10.70 -2 -3 16 20.10 8.80 2 3 -16 48.10 12.50 -2 3 16 35.30 9.70 -1 -3 16 46.00 10.40 -1 -3 16 68.39 13.00 1 3 -16 32.00 10.10 -1 3 16 47.80 10.30 -1 3 16 62.49 11.70 0 -3 16 64.89 11.20 0 -3 16 58.19 10.80 0 3 -16 55.49 12.10 0 3 16 88.99 13.90 0 3 16 64.59 11.90 1 -3 16 31.70 8.90 1 -3 16 41.70 11.40 1 3 16 41.70 10.40 -1 3 -16 34.50 9.70 1 3 16 30.10 10.00 2 -3 16 19.00 8.90 2 3 16 22.20 9.90 2 3 16 9.30 8.00 3 -3 16 23.70 10.10 3 3 16 18.30 9.40 3 3 16 19.50 9.80 -2 -4 16 26.00 10.20 -2 -4 16 29.30 10.80 -2 4 16 14.40 9.60 2 4 -16 21.80 8.80 -1 -4 16 18.30 9.90 -1 -4 16 0.40 8.00 1 4 -16 -1.10 8.00 -1 4 16 -0.60 8.50 0 -4 16 3.50 9.10 0 -4 16 -8.80 6.90 0 4 -16 1.60 7.10 0 4 16 -12.00 8.50 0 4 16 0.90 7.20 1 -4 16 26.60 10.40 1 4 16 14.20 8.50 1 4 16 11.10 10.40 5 0 -17 50.19 13.90 -4 0 17 -6.60 8.40 4 0 -17 16.20 9.90 3 0 -17 87.49 13.90 -3 0 17 125.09 15.30 -3 0 17 138.89 17.10 -2 0 17 11.10 7.80 2 0 -17 7.40 9.10 -2 0 17 5.20 7.70 -1 0 17 4.00 8.00 1 0 -17 0.00 7.10 -1 0 17 -2.70 7.50 0 0 17 -0.20 8.20 0 0 -17 7.60 7.90 0 0 17 3.20 7.90 1 0 17 12.60 9.30 1 0 17 13.60 8.80 -1 0 -17 18.30 9.50 2 0 17 -1.70 8.30 -2 0 -17 -12.80 5.90 2 0 17 -10.00 6.70 3 0 17 40.40 10.30 3 0 17 36.00 10.50 4 0 17 31.10 10.80 4 -1 -17 41.30 12.20 -4 -1 17 42.00 11.60 -4 1 17 32.80 10.10 4 1 -17 36.90 12.50 -3 -1 17 2.10 8.10 3 -1 -17 5.20 8.30 -3 -1 17 10.40 8.60 3 1 -17 3.90 9.00 -3 1 17 2.80 8.10 -2 -1 17 60.49 11.60 2 -1 -17 77.79 13.70 -2 -1 17 64.59 12.60 -2 1 17 60.09 11.60 2 1 -17 68.69 12.20 -2 1 17 53.39 11.20 -1 -1 17 104.19 14.80 1 -1 -17 70.29 12.80 -1 -1 17 75.69 12.00 -1 1 17 85.99 13.40 -1 1 17 67.99 12.00 1 1 -17 57.99 11.50 0 -1 17 21.60 9.30 0 -1 17 6.80 8.20 0 -1 -17 -0.40 7.60 0 1 17 11.60 8.50 0 1 -17 0.10 7.50 0 1 17 21.70 8.80 1 -1 17 71.89 12.70 1 -1 17 47.00 10.50 1 1 17 32.00 10.10 1 1 17 35.20 9.80 -1 1 -17 60.69 12.30 2 -1 17 126.79 15.10 2 -1 17 99.19 14.90 -2 1 -17 84.19 13.30 2 1 17 94.69 13.80 2 1 17 76.39 12.50 3 -1 17 17.40 9.00 3 -1 17 22.70 10.00 -3 1 -17 27.10 9.10 3 1 17 37.10 10.60 3 1 17 33.80 9.70 4 2 -17 8.10 10.80 -3 -2 17 52.59 11.80 -3 -2 17 58.19 12.00 -3 2 17 63.69 12.40 3 2 -17 32.10 10.80 -2 -2 17 2.40 8.30 -2 -2 17 8.30 8.90 2 2 -17 8.80 9.00 -2 2 17 0.80 7.40 -1 -2 17 31.10 9.90 -1 -2 17 25.10 9.80 -1 2 17 16.80 8.20 1 2 -17 14.80 8.80 -1 2 17 5.10 7.80 0 -2 17 0.20 8.50 0 -2 17 17.70 9.00 0 2 17 -12.90 6.70 0 2 -17 7.80 7.80 0 2 17 5.40 8.20 1 -2 17 61.59 11.60 1 -2 17 48.00 10.90 -1 2 -17 34.40 9.90 1 2 17 50.39 10.30 1 2 17 39.40 9.90 2 -2 17 16.30 9.00 2 -2 17 31.80 9.70 2 2 17 40.50 10.50 2 2 17 11.30 8.80 -2 2 -17 18.70 8.40 3 -2 17 48.20 10.80 3 2 17 36.50 11.00 3 2 17 35.50 10.80 3 3 -17 13.60 9.90 -2 -3 17 80.39 13.60 -2 -3 17 72.59 12.90 2 3 -17 62.89 13.20 -2 3 17 85.19 14.00 -1 -3 17 33.70 10.80 -1 -3 17 24.20 8.90 -1 3 17 18.70 10.10 1 3 -17 10.60 8.20 0 -3 17 46.60 11.90 0 -3 17 45.90 11.20 0 3 -17 52.59 11.60 0 3 17 51.29 11.70 0 3 17 49.80 12.50 1 -3 17 10.10 8.60 1 -3 17 14.30 8.90 -1 3 -17 5.10 7.50 1 3 17 17.30 8.90 1 3 17 1.20 9.40 3 0 -18 -3.50 9.80 -3 0 18 -1.50 9.40 -3 0 18 -2.20 9.00 -2 0 18 21.00 11.00 -2 0 18 26.40 9.50 2 0 -18 21.00 10.50 -1 0 18 2.60 9.30 -1 0 18 3.50 8.80 1 0 -18 1.00 8.10 0 0 18 35.60 10.10 0 0 18 48.80 11.80 0 0 -18 31.20 10.00 -1 0 -18 -5.40 7.70 1 0 18 -5.70 7.90 1 0 18 -9.10 7.90 2 0 18 6.00 7.90 2 0 18 11.40 9.50 -3 -1 18 10.70 9.20 3 -1 -18 4.50 9.30 -3 -1 18 22.30 10.60 3 1 -18 12.20 10.80 -3 1 18 9.80 10.10 -2 -1 18 33.30 12.10 -2 -1 18 36.50 10.10 2 -1 -18 51.39 13.20 2 1 -18 22.40 11.30 -2 1 18 44.20 10.70 -2 1 18 52.79 12.00 -1 -1 18 19.80 9.80 1 -1 -18 5.10 9.20 -1 -1 18 -15.10 6.90 -1 1 18 3.00 8.10 -1 1 18 1.60 8.60 1 1 -18 -1.10 7.60 0 -1 18 32.60 9.40 0 -1 18 51.99 11.20 0 1 18 25.10 9.60 0 1 -18 25.20 9.70 0 1 18 20.10 8.90 1 -1 18 40.40 10.90 1 -1 18 25.00 10.10 1 1 18 23.40 10.20 -1 1 -18 14.40 10.30 1 1 18 26.90 9.50 2 -1 18 17.80 9.20 2 -1 18 19.30 10.60 2 1 18 11.10 7.60 2 1 18 15.10 9.30 -2 1 -18 17.40 8.20 2 2 -18 16.30 10.80 -1 -2 18 121.99 16.30 -1 -2 18 107.49 16.30 -1 2 18 147.49 18.40 -1 2 18 119.39 15.40 0 -2 18 17.80 9.20 0 -2 18 16.40 10.60 0 2 18 3.10 8.30 0 2 18 20.00 10.50 0 2 -18 12.40 8.80 1 -2 18 57.49 12.20 1 -2 18 78.39 13.90 1 2 18 101.59 14.50 1 2 18 89.59 15.20 -1 2 -18 48.90 11.60 0 0 -19 -0.80 8.70 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 69830 _shelx_res_file ; TITL P3t.res in P2(1) Z=2 shelx.res created by SHELXL-2018/1 at 19:25:02 on 22-Dec-2017 CELL 0.71073 8.0762 6.2486 14.5096 90.000 92.161 90.000 ZERR 2.00 0.0004 0.0004 0.0010 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O S UNIT 22 38 2 14 2 REM MERG 2 OMIT 0 0 1 DFIX 0.9 0.02 N1 H1A N1 H1B N1 H1C O7 H7E O7 H7D DFIX 1.47 0.02 H1A H1B H1B H1C H1C H1A H7E H7D EQIV $1 x+1, y, z HTAB C9 O1_$1 HTAB C11 O5 HTAB O5 O3 HTAB O5 S1 EQIV $2 x+1, y+1, z HTAB O6 O2_$2 HTAB O6 S1_$2 EQIV $3 -x+2, y-1/2, -z HTAB N1 O7_$3 EQIV $4 -x+1, y+1/2, -z HTAB N1 O4_$4 EQIV $5 x, y-1, z HTAB N1 O7_$5 HTAB O7 O1_$4 HTAB O7 O6 FMAP 2 PLAN 20 SIZE 0.100 0.150 0.150 ACTA BOND $H CONF L.S. 10 TEMP 23.00 WGHT 0.033200 0.119600 FVAR 1.17655 C1 1 0.190223 0.262218 0.329790 11.00000 0.02809 0.03846 = 0.02975 0.00707 -0.00128 -0.00191 C2 1 0.160924 0.190406 0.417704 11.00000 0.07156 0.04015 = 0.03289 0.00547 0.00129 -0.01491 AFIX 43 H2 2 0.116375 0.054961 0.426354 11.00000 -1.20000 AFIX 0 C3 1 0.197932 0.320200 0.492794 11.00000 0.08920 0.05895 = 0.02746 0.00547 0.00114 -0.00803 AFIX 43 H3 2 0.176111 0.271176 0.551625 11.00000 -1.20000 AFIX 0 C4 1 0.266663 0.521337 0.482633 11.00000 0.06460 0.04534 = 0.03898 -0.00455 -0.00447 -0.00056 C5 1 0.292323 0.591384 0.394240 11.00000 0.06310 0.03637 = 0.04708 -0.00093 0.00432 -0.00951 AFIX 43 H5 2 0.336603 0.726971 0.385569 11.00000 -1.20000 AFIX 0 C6 1 0.253907 0.465204 0.318124 11.00000 0.05534 0.04084 = 0.03250 0.00558 0.00489 -0.00822 AFIX 43 H6 2 0.270923 0.516931 0.259131 11.00000 -1.20000 AFIX 0 C7 1 0.310152 0.660866 0.565254 11.00000 0.11341 0.06674 = 0.04839 -0.01604 -0.00665 -0.01315 AFIX 137 H7A 2 0.299896 0.808749 0.548036 11.00000 -1.50000 H7B 2 0.422038 0.632250 0.586385 11.00000 -1.50000 H7C 2 0.236118 0.630136 0.613767 11.00000 -1.50000 AFIX 0 C8 1 0.586017 0.283036 0.114589 11.00000 0.02536 0.02365 = 0.03098 -0.00074 0.00134 0.00175 C9 1 0.731306 0.434437 0.110145 11.00000 0.01971 0.02628 = 0.02628 0.00225 -0.00047 0.00004 AFIX 13 H9 2 0.827748 0.370261 0.142508 11.00000 -1.20000 AFIX 0 C10 1 0.694147 0.652648 0.154066 11.00000 0.02948 0.02701 = 0.02955 -0.00375 0.00209 -0.00694 AFIX 13 H10 2 0.583673 0.699233 0.132162 11.00000 -1.20000 AFIX 0 C11 1 0.697749 0.643648 0.258586 11.00000 0.06433 0.05155 = 0.03351 -0.01005 0.01001 -0.02278 AFIX 137 H11A 2 0.804857 0.595975 0.281004 11.00000 -1.50000 H11B 2 0.614560 0.545714 0.278236 11.00000 -1.50000 H11C 2 0.676108 0.783559 0.282673 11.00000 -1.50000 AFIX 0 O1 4 0.106396 0.228909 0.156251 11.00000 0.05774 0.05666 = 0.02878 0.01055 -0.00490 0.00110 O2 4 0.022781 -0.053027 0.258805 11.00000 0.04224 0.07252 = 0.04045 -0.00025 0.00308 -0.03273 O3 4 0.306568 -0.020110 0.218029 11.00000 0.03708 0.03316 = 0.05128 0.00155 0.00675 -0.00434 O4 4 0.494962 0.247394 0.048803 11.00000 0.04148 0.05509 = 0.03457 0.00124 -0.00614 -0.02470 O5 4 0.571285 0.201520 0.196596 11.00000 0.04002 0.04537 = 0.03736 0.01002 -0.00145 -0.01533 AFIX 83 H5A 2 0.483804 0.135286 0.198317 11.00000 -1.50000 AFIX 0 O6 4 0.812648 0.801084 0.122635 11.00000 0.05614 0.03687 = 0.03112 -0.00119 0.00011 -0.02100 AFIX 83 H6A 2 0.877061 0.833342 0.165426 11.00000 -1.50000 AFIX 0 O7 4 0.869192 1.053413 -0.027435 11.00000 0.04975 0.02874 = 0.03997 -0.00316 0.00682 0.00143 S1 5 0.152160 0.093123 0.233718 11.00000 0.03044 0.04051 = 0.02814 0.00477 -0.00027 -0.00968 N1 3 0.768919 0.466244 0.011763 11.00000 0.02519 0.02442 = 0.03103 -0.00164 0.00357 -0.00140 H1B 2 0.864977 0.541864 0.007457 11.00000 0.03251 H1C 2 0.683441 0.534876 -0.013441 11.00000 0.06016 H1A 2 0.781753 0.338118 -0.015920 11.00000 0.05004 H7E 2 0.848486 0.980139 -0.078193 11.00000 0.04819 H7D 2 0.835521 0.983479 0.021185 11.00000 0.08815 HKLF 4 REM P3t.res in P2(1) Z=2 REM R1 = 0.0371 for 2705 Fo > 4sig(Fo) and 0.0559 for all 3347 data REM 203 parameters refined using 10 restraints END WGHT 0.0332 0.1196 REM Highest difference peak 0.185, deepest hole -0.193, 1-sigma level 0.042 Q1 1 0.0019 0.0734 0.2405 11.00000 0.05 0.19 Q2 1 0.1445 0.2199 0.2945 11.00000 0.05 0.18 Q3 1 0.2037 0.2143 0.1685 11.00000 0.05 0.18 Q4 1 0.2792 -0.1757 0.1838 11.00000 0.05 0.16 Q5 1 0.3464 -0.0303 0.1783 11.00000 0.05 0.16 Q6 1 0.7820 1.0800 -0.0595 11.00000 0.05 0.15 Q7 1 0.3552 0.5833 0.6220 11.00000 0.05 0.15 Q8 1 0.7404 0.9756 0.1249 11.00000 0.05 0.15 Q9 1 0.8165 0.8113 0.0786 11.00000 0.05 0.15 Q10 1 0.0776 -0.0629 0.2559 11.00000 0.05 0.15 Q11 1 0.0323 -0.1718 0.1990 11.00000 0.05 0.14 Q12 1 0.2835 0.0871 0.1975 11.00000 0.05 0.14 Q13 1 0.7485 0.4378 0.0721 11.00000 0.05 0.14 Q14 1 0.3757 0.4711 0.2640 11.00000 0.05 0.14 Q15 1 0.2515 0.1116 0.4226 11.00000 0.05 0.14 Q16 1 0.1966 0.7859 0.5754 11.00000 0.05 0.14 Q17 1 0.2157 -0.0227 0.1584 11.00000 0.05 0.14 Q18 1 0.9046 0.4628 0.3554 11.00000 0.05 0.14 Q19 1 0.0457 0.3582 0.1566 11.00000 0.05 0.14 Q20 1 0.0841 0.2215 0.1982 11.00000 0.05 0.14 ; _shelx_res_checksum 11537 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 C C1 0.1902(4) 0.2622(5) 0.3298(2) 0.0322(7) Uani d 1 C C2 0.1609(5) 0.1904(6) 0.4177(2) 0.0482(9) Uani d 1 H H2 0.116375 0.054961 0.426354 0.058 Uiso calc 1 C C3 0.1979(5) 0.3202(7) 0.4928(3) 0.0586(11) Uani d 1 H H3 0.176111 0.271176 0.551625 0.070 Uiso calc 1 C C4 0.2667(5) 0.5213(6) 0.4826(3) 0.0498(10) Uani d 1 C C5 0.2923(4) 0.5914(7) 0.3942(2) 0.0488(9) Uani d 1 H H5 0.336603 0.726971 0.385569 0.059 Uiso calc 1 C C6 0.2539(4) 0.4652(6) 0.3181(2) 0.0428(8) Uani d 1 H H6 0.270923 0.516931 0.259131 0.051 Uiso calc 1 C C7 0.3102(7) 0.6609(7) 0.5653(3) 0.0764(14) Uani d 1 H H7A 0.299896 0.808749 0.548036 0.115 Uiso calc 1 H H7B 0.422038 0.632250 0.586385 0.115 Uiso calc 1 H H7C 0.236118 0.630136 0.613767 0.115 Uiso calc 1 C C8 0.5860(4) 0.2830(5) 0.1146(2) 0.0267(7) Uani d 1 C C9 0.7313(3) 0.4344(5) 0.1101(2) 0.0241(6) Uani d 1 H H9 0.827748 0.370261 0.142508 0.029 Uiso calc 1 C C10 0.6941(4) 0.6526(4) 0.1541(2) 0.0287(7) Uani d 1 H H10 0.583673 0.699233 0.132162 0.034 Uiso calc 1 C C11 0.6977(5) 0.6436(6) 0.2586(2) 0.0496(10) Uani d 1 H H11A 0.804857 0.595975 0.281004 0.074 Uiso calc 1 H H11B 0.614560 0.545714 0.278236 0.074 Uiso calc 1 H H11C 0.676108 0.783559 0.282673 0.074 Uiso calc 1 O O1 0.1064(3) 0.2289(4) 0.15625(16) 0.0479(6) Uani d 1 O O2 0.0228(3) -0.0530(5) 0.25880(16) 0.0517(7) Uani d 1 O O3 0.3066(3) -0.0201(3) 0.21803(16) 0.0404(6) Uani d 1 O O4 0.4950(3) 0.2474(4) 0.04880(15) 0.0439(6) Uani d 1 O O5 0.5713(3) 0.2015(4) 0.19660(15) 0.0410(6) Uani d 1 H H5A 0.483804 0.135286 0.198317 0.061 Uiso calc 1 O O6 0.8126(3) 0.8011(3) 0.12263(15) 0.0414(6) Uani d 1 H H6A 0.877061 0.833342 0.165426 0.062 Uiso calc 1 O O7 0.8692(3) 1.0534(3) -0.02744(18) 0.0394(6) Uani d 1 S S1 0.15216(9) 0.09312(13) 0.23372(5) 0.0331(2) Uani d 1 N N1 0.7689(3) 0.4662(4) 0.01176(17) 0.0268(6) Uani d 1 H H1B 0.865(3) 0.542(4) 0.007(2) 0.033(9) Uiso d 1 H H1C 0.683(3) 0.535(5) -0.013(2) 0.060(13) Uiso d 1 H H1A 0.782(4) 0.338(4) -0.016(2) 0.050(11) Uiso d 1 H H7E 0.848(4) 0.980(5) -0.0782(17) 0.048(11) Uiso d 1 H H7D 0.836(5) 0.983(7) 0.0212(19) 0.088(17) 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 C1 0.0281(16) 0.0385(17) 0.0298(17) -0.0019(14) -0.0013(13) 0.0071(14) C2 0.072(3) 0.0402(19) 0.0329(19) -0.0149(19) 0.0013(17) 0.0055(17) C3 0.089(3) 0.059(3) 0.027(2) -0.008(2) 0.001(2) 0.0055(19) C4 0.065(2) 0.045(2) 0.039(2) -0.0006(18) -0.0045(18) -0.0046(17) C5 0.063(2) 0.0364(18) 0.047(2) -0.010(2) 0.0043(17) -0.001(2) C6 0.055(2) 0.0408(19) 0.0325(19) -0.0082(18) 0.0049(16) 0.0056(16) C7 0.113(4) 0.067(3) 0.048(3) -0.013(3) -0.007(2) -0.016(2) C8 0.0254(15) 0.0237(15) 0.0310(17) 0.0018(13) 0.0013(13) -0.0007(13) C9 0.0197(14) 0.0263(14) 0.0263(16) 0.0000(12) -0.0005(12) 0.0022(13) C10 0.0295(16) 0.0270(16) 0.0296(16) -0.0069(12) 0.0021(12) -0.0037(12) C11 0.064(2) 0.052(2) 0.0335(18) -0.0228(19) 0.0100(16) -0.0100(16) O1 0.0577(15) 0.0567(15) 0.0288(13) 0.0011(13) -0.0049(11) 0.0106(12) O2 0.0422(13) 0.0725(17) 0.0404(14) -0.0327(13) 0.0031(11) -0.0002(14) O3 0.0371(12) 0.0332(12) 0.0513(15) -0.0043(11) 0.0068(11) 0.0016(11) O4 0.0415(13) 0.0551(15) 0.0346(13) -0.0247(12) -0.0061(11) 0.0012(11) O5 0.0400(13) 0.0454(13) 0.0374(13) -0.0153(11) -0.0015(10) 0.0100(11) O6 0.0561(15) 0.0369(13) 0.0311(13) -0.0210(12) 0.0001(11) -0.0012(11) O7 0.0497(14) 0.0287(13) 0.0400(14) 0.0014(11) 0.0068(11) -0.0032(12) S1 0.0304(4) 0.0405(4) 0.0281(4) -0.0097(4) -0.0003(3) 0.0048(4) N1 0.0252(14) 0.0244(13) 0.0310(14) -0.0014(12) 0.0036(11) -0.0016(12) 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 C2 C1 C6 119.3(3) C2 C1 S1 120.2(3) C6 C1 S1 120.5(2) C1 C2 C3 119.9(3) C1 C2 H2 120.1 C3 C2 H2 120.1 C2 C3 C4 121.6(3) C2 C3 H3 119.2 C4 C3 H3 119.2 C5 C4 C3 117.5(4) C5 C4 C7 121.1(4) C3 C4 C7 121.4(4) C4 C5 C6 121.7(4) C4 C5 H5 119.2 C6 C5 H5 119.2 C1 C6 C5 119.9(3) C1 C6 H6 120.0 C5 C6 H6 120.0 C4 C7 H7A 109.5 C4 C7 H7B 109.5 H7A C7 H7B 109.5 C4 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 O4 C8 O5 125.3(3) O4 C8 C9 122.3(3) O5 C8 C9 112.4(3) N1 C9 C8 108.2(2) N1 C9 C10 109.3(2) C8 C9 C10 111.9(2) N1 C9 H9 109.1 C8 C9 H9 109.1 C10 C9 H9 109.1 O6 C10 C11 110.9(2) O6 C10 C9 107.5(2) C11 C10 C9 112.6(3) O6 C10 H10 108.6 C11 C10 H10 108.6 C9 C10 H10 108.6 C10 C11 H11A 109.5 C10 C11 H11B 109.5 H11A C11 H11B 109.5 C10 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C8 O5 H5A 109.5 C10 O6 H6A 109.5 H7E O7 H7D 111(3) O2 S1 O1 113.63(15) O2 S1 O3 111.30(15) O1 S1 O3 111.00(14) O2 S1 C1 106.57(15) O1 S1 C1 107.12(16) O3 S1 C1 106.79(14) C9 N1 H1B 109.9(19) C9 N1 H1C 106(2) H1B N1 H1C 112(2) C9 N1 H1A 110(2) H1B N1 H1A 108(2) H1C N1 H1A 110(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.381(4) C1 C6 1.381(5) C1 S1 1.767(3) C2 C3 1.382(5) C2 H2 0.9300 C3 C4 1.384(5) C3 H3 0.9300 C4 C5 1.378(5) C4 C7 1.513(5) C5 C6 1.383(5) C5 H5 0.9300 C6 H6 0.9300 C7 H7A 0.9600 C7 H7B 0.9600 C7 H7C 0.9600 C8 O4 1.204(3) C8 O5 1.304(3) C8 C9 1.511(4) C9 N1 1.484(4) C9 C10 1.539(4) C9 H9 0.9800 C10 O6 1.420(3) C10 C11 1.517(4) C10 H10 0.9800 C11 H11A 0.9600 C11 H11B 0.9600 C11 H11C 0.9600 O1 S1 1.445(2) O2 S1 1.445(2) O3 S1 1.459(2) O5 H5A 0.8200 O6 H6A 0.8200 O7 H7E 0.88(2) O7 H7D 0.88(2) N1 H1B 0.913(19) N1 H1C 0.88(2) N1 H1A 0.90(2) 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 C11 H11B O5 . 0.96 2.47 3.068(4) 120 yes O5 H5A O3 . 0.82 1.76 2.576(3) 172 yes O6 H6A O2 1_665 0.82 1.90 2.713(3) 172 yes O7 H7E O1 2_655 0.88(2) 1.98(3) 2.770(3) 149(3) yes O7 H7D O6 . 0.88(2) 1.88(3) 2.741(3) 166(4) yes N1 H1B O7 2_745 0.913(19) 2.16(2) 2.973(3) 149(2) yes N1 H1C O4 2_655 0.88(2) 2.01(2) 2.874(3) 166(3) yes N1 H1A O7 1_545 0.90(2) 1.92(2) 2.769(3) 155(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 C6 C1 C2 C3 -1.1(5) S1 C1 C2 C3 177.1(3) C1 C2 C3 C4 -1.0(6) C2 C3 C4 C5 2.0(6) C2 C3 C4 C7 -178.7(4) C3 C4 C5 C6 -1.1(6) C7 C4 C5 C6 179.7(4) C2 C1 C6 C5 2.0(5) S1 C1 C6 C5 -176.2(3) C4 C5 C6 C1 -0.9(5) O4 C8 C9 N1 -17.9(4) O5 C8 C9 N1 163.1(2) O4 C8 C9 C10 102.5(3) O5 C8 C9 C10 -76.5(3) N1 C9 C10 O6 -42.8(3) C8 C9 C10 O6 -162.6(2) N1 C9 C10 C11 -165.3(2) C8 C9 C10 C11 74.9(3) C2 C1 S1 O2 27.8(3) C6 C1 S1 O2 -154.0(3) C2 C1 S1 O1 149.7(3) C6 C1 S1 O1 -32.1(3) C2 C1 S1 O3 -91.3(3) C6 C1 S1 O3 86.9(3) _cod_database_fobs_code 1548678