#------------------------------------------------------------------------------ #$Date: 2021-10-14 05:24:17 +0300 (Thu, 14 Oct 2021) $ #$Revision: 269933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243929.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_2243929 loop_ _publ_author_name 'Mambourg, Kalina' 'Tumanov, Nikolay' 'Henon, Gilles' 'Lanners, Steve' 'Garcia-Ladona, Javier' 'Wouters, Johan' _publ_section_title ; Crystal structures of two alanylpiperidine analogues ; _journal_coeditor_code VM2254 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989021010392 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C19 H28 N2 O5 S' _chemical_formula_moiety 'C19 H28 N2 O5 S' _chemical_formula_sum 'C19 H28 N2 O5 S' _chemical_formula_weight 396.49 _chemical_name_systematic 'Ethyl 1-[N-(4-methylphenyl)-N-(methylsulfonyl)alanyl]piperidine-4-carboxylate' _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 _atom_sites_solution_primary dual _atom_sites_solution_secondary dual _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 75.947(6) _cell_angle_beta 79.302(6) _cell_angle_gamma 74.554(5) _cell_formula_units_Z 2 _cell_length_a 8.5368(6) _cell_length_b 9.6594(6) _cell_length_c 13.5173(12) _cell_measurement_reflns_used 3246 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 30.5 _cell_measurement_theta_min 2.4 _cell_volume 1033.47(14) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2018) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2018) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2018) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2016 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 295(2) _diffrn_detector_area_resol_mean 10.3712 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.900 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur, Gemini Ultra R ; _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_unetI/netI 0.045 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 13200 _diffrn_reflns_theta_full 25.2 _diffrn_reflns_theta_max 32.8 _diffrn_reflns_theta_min 2.234 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.188 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_correction_T_min 0.923 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; [CrysAlisPro (Rigaku OD, 2018), based on expressions derived by Clark & Reid (1995)] ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 424 _exptl_crystal_size_max 0.790 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.336 _refine_diff_density_min -0.375 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 248 _refine_ls_number_reflns 6870 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.02 _refine_ls_R_factor_all 0.093 _refine_ls_R_factor_gt 0.054 _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^)+(0.0633P)^2^+0.1206P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.130 _refine_ls_wR_factor_ref 0.158 _reflns_number_gt 4304 _reflns_number_total 6870 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file vm2254sup1.cif _cod_data_source_block I _cod_database_code 2243929 _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 0.866 _shelx_estimated_absorpt_t_max 0.991 _shelx_hkl_file ; 0 0 2 1279.76 5.75 0 0 2 1288.72 7.60 0 0 3 1248.85 9.15 0 0 3 1212.70 6.98 0 0 -3 1223.12 7.48 0 0 4 571.18 7.24 0 0 4 561.61 5.55 0 0 -4 582.14 5.96 0 0 5 53.95 1.92 0 0 -5 55.85 2.05 0 0 5 55.15 2.53 0 0 -6 57.61 2.30 0 0 6 56.46 2.20 0 0 6 59.13 2.94 0 0 -7 20.04 1.45 0 0 7 19.79 1.84 0 0 7 20.54 1.43 0 0 -8 20.26 1.57 0 0 8 21.41 2.04 0 0 8 19.90 1.50 0 0 9 97.15 4.65 0 0 -9 101.61 3.72 0 0 9 91.88 3.43 0 0 10 1.30 0.50 0 0 10 2.51 0.98 0 0 -11 23.12 1.67 0 0 11 19.36 1.74 0 0 11 19.87 2.40 0 0 -11 22.74 2.88 0 0 12 81.05 5.10 0 0 -12 85.04 3.93 0 0 -12 93.55 6.18 0 0 12 76.79 3.58 0 0 -12 89.63 3.28 0 0 -13 0.52 0.75 0 0 13 -0.69 0.82 0 0 -13 0.41 0.39 0 0 -14 1.67 0.71 0 0 -14 3.48 1.39 0 0 14 2.65 0.93 0 0 -15 0.89 0.68 0 0 -15 0.79 0.65 0 0 -16 1.47 0.80 0 0 -17 -0.85 1.06 0 0 -18 3.68 1.84 0 0 -18 -0.43 1.16 0 0 -19 -1.72 1.89 0 1 -19 -0.19 1.45 0 1 -18 5.32 2.09 0 1 -18 4.23 1.82 0 1 -17 8.91 2.39 0 1 -17 4.87 1.94 0 1 -16 8.28 2.28 0 1 -15 -0.34 0.55 0 1 -15 0.02 0.80 0 1 -14 1.94 0.75 0 1 -14 6.31 1.82 0 1 -13 36.31 4.13 0 1 -13 29.82 2.67 0 1 -12 55.87 3.51 0 -1 12 51.20 4.07 0 -1 11 5.07 1.32 0 1 -11 5.61 0.99 0 1 -11 5.67 1.08 0 1 -10 44.24 2.86 0 -1 10 56.59 3.80 0 -1 9 6.81 1.32 0 -1 8 1.68 0.36 0 -1 8 2.35 0.77 0 -1 7 97.17 2.43 0 1 -7 104.19 3.85 0 -1 7 102.34 4.24 0 -1 6 134.61 4.44 0 -1 6 130.58 2.51 0 1 -6 134.64 4.13 0 1 -6 140.51 4.56 0 -1 5 8.41 0.56 0 -1 5 9.02 1.07 0 1 -5 10.00 1.11 0 1 -4 66.22 2.54 0 -1 4 64.42 2.51 0 1 -3 180.42 3.68 0 -1 3 182.71 3.66 0 -1 2 1847.68 9.68 0 1 -2 1876.61 9.85 0 1 -1 26.53 0.87 0 -1 1 26.77 0.88 0 -1 0 250.07 2.97 0 1 0 251.26 3.12 0 1 1 38.57 1.05 0 -1 -1 39.84 1.29 0 1 1 39.74 1.17 0 1 2 1886.80 7.81 0 -1 -2 1852.85 6.46 0 -1 -2 1825.47 10.99 0 1 2 1838.67 8.76 0 -1 -3 97.87 3.01 0 1 3 101.82 2.59 0 1 3 100.47 2.55 0 1 3 99.72 1.50 0 1 4 363.74 5.63 0 1 4 348.31 5.32 0 -1 -4 332.82 3.45 0 1 4 358.06 3.58 0 -1 -4 354.50 6.63 0 -1 -5 19.45 0.97 0 1 5 19.05 1.42 0 -1 -5 17.75 1.69 0 1 5 18.71 1.46 0 -1 -6 28.05 2.32 0 1 6 26.86 1.91 0 -1 -6 26.27 1.28 0 1 6 26.64 1.75 0 -1 -7 57.70 2.12 0 1 7 54.03 2.64 0 1 7 53.66 2.98 0 -1 -7 61.03 3.66 0 1 8 124.37 4.81 0 -1 -8 119.97 3.32 0 1 8 121.24 4.21 0 -1 -8 131.98 5.74 0 -1 -9 86.17 4.97 0 -1 -9 77.61 2.84 0 1 9 75.43 3.51 0 1 9 77.73 4.06 0 -1 -10 250.17 5.43 0 1 10 254.21 7.92 0 1 10 259.67 6.82 0 -1 -11 24.27 1.78 0 1 11 27.09 1.36 0 1 11 25.50 2.74 0 -1 -11 26.78 3.13 0 1 12 0.68 0.26 0 1 12 0.56 0.67 0 -1 -12 0.91 0.26 0 -1 -12 1.94 1.07 0 -1 -13 2.13 1.24 0 1 13 1.01 0.46 0 1 13 2.78 0.98 0 1 14 10.01 2.11 0 1 14 10.22 1.68 0 -1 -14 13.20 2.55 0 1 15 -0.17 0.80 0 -1 -15 1.09 1.32 0 -1 -16 2.93 1.69 0 -1 -17 0.95 0.70 0 -1 -18 -0.51 1.16 0 -1 -19 2.03 1.03 0 2 -18 -0.05 0.97 0 2 -18 1.28 0.92 0 2 -17 0.67 0.97 0 2 -17 1.76 1.17 0 2 -16 0.15 0.55 0 2 -16 1.52 1.25 0 2 -16 -0.57 1.11 0 2 -15 7.61 2.12 0 2 -15 5.17 1.33 0 2 -14 0.68 0.45 0 2 -14 1.83 1.18 0 2 -13 16.30 2.19 0 -2 12 -0.13 0.23 0 2 -12 -0.35 0.58 0 -2 11 44.07 2.31 0 2 -11 49.43 3.42 0 2 -10 60.57 3.54 0 -2 10 59.82 4.04 0 2 -10 64.30 3.77 0 -2 9 4.79 1.13 0 2 -9 4.77 1.02 0 2 -8 40.31 2.79 0 -2 8 61.69 3.58 0 -2 7 16.37 1.70 0 -2 6 6.87 1.07 0 2 -6 5.43 0.87 0 -2 5 1891.49 15.70 0 2 -5 2031.68 16.20 0 -2 4 82.37 2.94 0 2 -4 85.57 2.99 0 2 -3 468.32 6.12 0 -2 3 447.98 6.08 0 2 -2 53.34 1.74 0 2 -2 51.62 1.25 0 2 -1 970.84 5.96 0 -2 1 991.97 8.42 0 2 -1 919.57 6.46 0 -2 1 951.38 8.62 0 2 -1 973.07 5.81 0 2 0 22.76 1.34 0 -2 0 23.02 1.29 0 2 0 23.10 1.14 0 2 0 22.55 1.33 0 2 1 44.46 1.71 0 -2 -1 45.25 1.07 0 2 1 45.35 1.77 0 2 1 45.78 1.86 0 2 1 44.97 1.02 0 -2 -2 8.13 0.84 0 2 2 8.29 0.83 0 2 2 8.23 0.70 0 2 2 9.39 0.85 0 2 2 9.27 0.64 0 -2 -2 8.77 0.73 0 -2 -2 9.26 0.64 0 2 3 157.19 3.33 0 -2 -3 152.35 4.03 0 2 3 151.66 2.65 0 -2 -3 139.81 3.13 0 2 3 156.00 3.10 0 -2 -3 159.80 3.13 0 -2 -3 150.49 2.81 0 -2 -4 176.76 2.85 0 -2 -4 168.26 4.78 0 2 4 175.66 3.85 0 2 4 181.29 3.57 0 -2 -4 175.30 3.91 0 -2 -5 349.42 3.87 0 -2 -5 361.35 6.41 0 2 5 348.59 6.64 0 2 5 362.50 3.48 0 2 5 362.11 5.11 0 2 5 353.10 6.17 0 -2 -5 368.13 7.78 0 2 6 28.73 1.13 0 -2 -6 29.23 2.01 0 2 6 29.49 1.97 0 2 6 29.48 1.51 0 -2 -6 29.05 1.09 0 -2 -6 28.36 2.39 0 2 6 30.85 2.10 0 2 7 257.35 4.50 0 2 7 242.33 6.25 0 2 7 251.38 6.36 0 -2 -7 272.35 7.84 0 -2 -7 248.38 3.16 0 2 8 12.92 1.06 0 -2 -8 12.80 0.72 0 -2 -8 13.15 1.99 0 2 8 13.07 1.58 0 -2 -9 49.31 3.80 0 2 9 46.49 3.14 0 -2 -9 45.14 1.31 0 2 9 42.97 1.95 0 -2 -10 14.39 0.71 0 2 10 14.89 1.18 0 -2 -10 14.76 2.28 0 2 10 16.11 1.97 0 2 11 53.41 3.56 0 2 11 53.00 2.27 0 2 11 57.01 3.97 0 -2 -11 65.82 4.92 0 2 12 189.40 4.32 0 2 12 195.84 7.82 0 2 12 222.04 7.48 0 -2 -12 233.59 9.80 0 2 13 3.39 0.97 0 2 13 3.59 1.16 0 -2 -13 4.41 1.32 0 2 14 6.33 1.46 0 2 14 6.09 1.57 0 -2 -14 5.79 1.70 0 2 15 2.52 0.96 0 2 15 1.41 0.76 0 2 16 3.45 1.46 0 -2 -16 1.15 1.29 0 -2 -17 0.76 1.08 0 -2 -18 3.12 1.87 0 -2 -19 -0.68 1.14 0 3 -18 1.98 1.04 0 3 -17 1.91 1.11 0 3 -17 3.32 1.76 0 3 -16 0.02 1.02 0 3 -16 -0.10 0.73 0 3 -16 0.01 0.52 0 3 -15 2.40 1.00 0 3 -15 7.13 2.02 0 3 -15 5.19 1.73 0 3 -14 1.17 0.74 0 3 -14 2.22 1.07 0 3 -13 7.06 1.54 0 -3 12 9.04 1.12 0 3 -12 12.93 1.99 0 3 -11 0.07 0.53 0 -3 11 0.64 0.49 0 3 -10 0.62 0.47 0 -3 10 0.46 0.41 0 -3 9 8.54 1.13 0 3 -9 11.99 1.75 0 3 -8 11.40 1.64 0 -3 8 12.08 1.36 0 -3 7 224.35 5.66 0 3 -6 53.49 2.96 0 -3 6 51.29 2.67 0 3 -5 5.73 0.90 0 -3 5 5.09 0.85 0 -3 4 149.00 4.38 0 3 -4 159.66 4.19 0 3 -3 193.46 4.07 0 -3 3 179.45 4.72 0 3 -3 186.94 2.91 0 3 -3 196.60 4.04 0 -3 2 6.31 0.86 0 3 -2 8.51 0.76 0 -3 2 7.97 0.98 0 3 -2 8.06 0.75 0 3 -2 8.46 0.74 0 3 -1 500.38 8.18 0 -3 1 476.26 7.31 0 3 -1 467.75 5.89 0 3 -1 476.65 4.63 0 -3 1 470.60 7.12 0 3 -1 478.72 4.61 0 3 0 0.25 0.31 0 3 0 0.80 0.39 0 3 0 0.66 0.26 0 3 0 0.30 0.18 0 -3 0 0.34 0.13 0 3 1 12.26 1.19 0 3 1 11.12 1.15 0 3 1 11.42 1.03 0 3 1 10.72 1.09 0 -3 -1 10.74 0.60 0 3 1 10.41 0.55 0 3 2 39.88 1.27 0 -3 -2 37.56 1.35 0 3 2 39.75 2.08 0 3 2 37.58 2.06 0 3 2 38.41 1.90 0 -3 -3 131.14 3.56 0 3 3 136.86 3.39 0 -3 -3 133.61 4.15 0 3 3 133.72 2.81 0 3 3 133.12 3.81 0 -3 -3 126.02 2.93 0 -3 -3 132.51 3.52 0 3 3 132.08 4.07 0 3 4 961.45 12.08 0 3 4 986.44 9.07 0 3 4 990.48 8.54 0 -3 -4 968.65 9.12 0 -3 -4 983.40 9.66 0 3 4 985.68 10.31 0 -3 -4 985.41 9.41 0 -3 -4 956.33 12.12 0 3 5 1401.39 16.02 0 3 5 1489.47 12.75 0 -3 -5 1412.70 10.72 0 -3 -5 1486.08 16.15 0 3 5 1460.84 12.34 0 -3 -5 1512.81 12.95 0 -3 -6 221.45 6.75 0 -3 -6 217.42 4.02 0 3 6 230.79 5.09 0 -3 -6 233.44 5.64 0 3 6 226.10 5.38 0 3 6 219.89 2.99 0 3 7 163.86 5.10 0 -3 -7 180.09 6.49 0 3 7 174.56 4.49 0 3 7 179.42 2.69 0 -3 -7 173.17 3.41 0 3 8 1.31 0.61 0 -3 -8 0.61 0.22 0 -3 -8 0.02 0.58 0 3 8 0.35 0.40 0 3 9 1.72 0.59 0 -3 -9 2.39 1.03 0 3 9 2.20 0.58 0 -3 -9 2.73 0.39 0 3 9 2.19 0.91 0 3 10 29.25 2.70 0 3 10 29.09 1.93 0 -3 -10 30.19 1.11 0 -3 -10 34.12 3.45 0 3 10 27.53 2.63 0 -3 -11 0.55 0.54 0 3 11 0.85 0.62 0 3 11 1.96 0.92 0 3 11 1.05 0.47 0 3 12 -0.15 0.28 0 3 12 0.13 0.60 0 -3 -12 -0.86 0.90 0 3 12 -0.39 0.53 0 -3 -13 6.54 1.65 0 3 13 6.54 1.56 0 3 13 3.86 1.20 0 -3 -14 0.13 0.82 0 3 14 1.03 0.73 0 3 14 0.59 0.63 0 -3 -15 0.63 1.16 0 3 15 0.50 0.80 0 3 15 0.73 0.67 0 3 16 0.93 0.65 0 3 16 0.02 0.63 0 -3 -17 3.41 1.83 0 -3 -18 -0.57 0.69 0 -3 -19 1.10 1.37 0 4 -17 1.69 1.20 0 4 -17 1.81 1.36 0 4 -16 8.67 2.14 0 4 -16 15.68 3.23 0 4 -16 20.48 3.55 0 4 -15 8.36 2.01 0 4 -15 7.08 2.09 0 4 -15 6.92 2.02 0 4 -14 2.75 1.16 0 4 -14 3.00 1.31 0 4 -13 4.45 1.51 0 4 -13 4.23 1.39 0 4 -12 0.57 0.84 0 4 -12 0.24 0.68 0 -4 12 0.61 0.45 0 4 -11 1.34 0.66 0 -4 11 0.67 0.39 0 4 -11 2.23 0.93 0 4 -10 29.78 3.07 0 4 -10 25.68 2.71 0 -4 10 23.40 2.05 0 4 -9 66.64 4.44 0 4 -9 68.87 4.17 0 -4 9 60.38 3.28 0 4 -8 32.37 3.03 0 -4 8 28.77 2.29 0 4 -8 33.40 2.71 0 4 -7 25.55 2.29 0 -4 7 21.03 1.94 0 4 -6 110.13 4.32 0 4 -6 111.48 4.32 0 -4 6 100.97 4.18 0 4 -5 261.18 6.15 0 -4 5 252.07 6.52 0 4 -5 251.62 5.90 0 4 -4 63.72 3.73 0 4 -4 60.47 1.81 0 -4 4 59.13 3.11 0 4 -4 59.13 2.65 0 4 -4 62.72 2.70 0 4 -3 43.98 1.83 0 4 -3 43.19 2.01 0 4 -3 45.30 3.03 0 -4 3 41.25 2.61 0 4 -3 43.49 2.01 0 -4 3 45.11 2.71 0 4 -2 35.90 1.82 0 4 -2 38.23 2.66 0 4 -2 34.43 1.62 0 -4 2 34.15 2.25 0 4 -2 36.42 1.60 0 -4 2 32.96 2.24 0 4 -1 18.73 1.43 0 -4 1 16.52 1.61 0 -4 1 16.37 1.63 0 4 -1 18.58 0.97 0 4 -1 19.22 1.83 0 4 -1 17.11 0.98 0 4 0 7.85 1.18 0 4 0 9.51 0.65 0 4 0 9.83 1.08 0 4 0 11.07 1.35 0 4 1 113.80 3.80 0 4 1 112.71 4.29 0 4 1 108.96 1.87 0 -4 -1 108.90 1.87 0 4 1 113.12 4.12 0 4 1 114.11 4.10 0 -4 -2 13.30 0.84 0 4 2 13.83 1.35 0 4 2 15.88 1.59 0 4 2 13.88 1.40 0 4 2 13.99 0.76 0 4 2 13.92 1.45 0 4 3 37.04 2.38 0 4 3 40.14 1.52 0 4 3 38.03 2.14 0 4 3 37.46 2.38 0 -4 -3 37.28 1.63 0 -4 -3 35.83 2.29 0 4 4 38.77 2.07 0 4 4 36.48 2.52 0 -4 -4 41.09 2.69 0 -4 -4 37.34 1.88 0 -4 -4 37.33 2.21 0 4 4 40.36 2.47 0 4 4 36.09 1.73 0 -4 -5 52.00 3.23 0 4 5 51.95 2.29 0 4 5 51.62 3.18 0 4 5 53.88 2.85 0 -4 -5 53.95 2.55 0 -4 -5 51.23 2.42 0 -4 -5 51.49 2.62 0 4 5 50.90 2.29 0 4 6 75.50 4.19 0 4 6 75.40 3.08 0 4 6 76.56 3.39 0 -4 -6 81.63 4.32 0 -4 -6 76.88 2.98 0 -4 -6 79.15 3.33 0 4 7 443.97 8.26 0 4 7 447.44 10.01 0 -4 -7 457.50 7.01 0 -4 -7 460.30 10.79 0 4 7 451.52 8.35 0 -4 -8 8.93 0.93 0 4 8 7.85 1.14 0 -4 -8 6.91 1.39 0 4 8 9.33 0.64 0 4 8 8.54 1.24 0 4 8 8.03 1.43 0 -4 -9 17.53 2.39 0 4 9 18.59 1.96 0 4 9 18.52 2.21 0 4 9 16.91 1.68 0 4 10 35.08 3.20 0 4 10 31.25 2.27 0 -4 -10 41.49 3.85 0 4 10 35.62 2.93 0 4 11 88.20 4.83 0 4 11 86.77 5.14 0 -4 -11 95.38 6.05 0 -4 -12 85.73 6.12 0 4 12 81.39 5.19 0 4 12 78.24 4.82 0 -4 -13 0.32 0.73 0 4 13 0.92 0.81 0 4 13 1.01 0.87 0 4 14 5.07 1.57 0 4 14 2.63 1.19 0 -4 -14 4.47 1.64 0 -4 -15 10.58 2.58 0 4 15 7.51 1.86 0 4 15 10.03 2.18 0 -4 -16 -0.45 0.91 0 4 16 -0.76 0.75 0 4 16 -1.07 1.07 0 4 17 0.34 1.03 0 -4 -17 -0.27 0.78 0 -4 -18 -0.23 0.77 0 -4 -19 6.43 2.21 0 5 -16 0.88 1.20 0 5 -16 3.12 1.76 0 5 -16 -0.76 1.02 0 5 -15 1.12 0.91 0 5 -15 2.90 1.35 0 5 -14 1.82 0.97 0 5 -14 2.18 1.28 0 5 -13 1.20 1.00 0 5 -13 0.15 0.83 0 5 -12 2.59 1.24 0 5 -12 1.82 0.80 0 5 -11 1.36 0.77 0 5 -11 1.50 0.85 0 -5 11 1.43 0.62 0 5 -10 1.02 0.57 0 -5 10 1.37 0.59 0 5 -10 1.61 0.80 0 5 -9 17.24 2.43 0 5 -9 15.51 2.12 0 -5 9 12.71 1.69 0 5 -8 34.97 2.86 0 -5 8 29.35 2.50 0 -5 7 0.15 0.46 0 5 -7 -0.05 0.37 0 5 -6 596.92 10.19 0 -5 6 535.88 10.52 0 -5 5 1.23 0.64 0 5 -5 1.44 0.53 0 -5 5 0.08 0.49 0 5 -5 1.15 0.53 0 5 -4 0.13 0.34 0 -5 4 0.59 0.56 0 5 -4 0.26 0.30 0 5 -4 -0.03 0.26 0 -5 4 0.43 0.53 0 -5 3 30.52 2.51 0 5 -3 33.00 1.80 0 -5 3 31.27 2.46 0 5 -3 29.76 1.76 0 5 -3 31.04 1.84 0 5 -2 23.06 1.33 0 -5 2 21.56 2.05 0 5 -2 21.83 1.34 0 5 -2 23.24 1.70 0 -5 2 22.61 2.06 0 -5 1 19.08 1.95 0 5 -1 20.53 1.05 0 -5 1 17.10 1.77 0 5 -1 21.87 1.72 0 5 -1 18.31 1.10 0 5 0 72.24 3.32 0 5 0 77.94 3.96 0 5 0 76.72 1.68 0 5 0 67.37 1.78 0 5 1 -0.26 0.47 0 5 1 0.14 0.26 0 -5 -1 0.19 0.12 0 5 1 0.30 0.46 0 5 1 0.06 0.14 0 5 2 40.80 1.26 0 5 2 38.82 2.49 0 5 2 38.77 2.83 0 5 2 43.40 2.78 0 5 2 39.98 2.67 0 -5 -2 36.69 1.35 0 5 3 109.91 4.18 0 -5 -3 106.99 2.75 0 5 3 110.83 4.42 0 5 3 110.80 2.50 0 5 3 114.70 4.80 0 5 3 107.88 4.59 0 5 4 14.48 1.72 0 5 4 15.08 1.50 0 5 4 15.09 1.72 0 -5 -4 14.54 1.18 0 5 4 15.90 1.11 0 5 5 338.78 5.82 0 5 5 330.95 8.56 0 -5 -5 353.29 6.33 0 -5 -5 349.93 8.77 0 5 5 346.82 6.91 0 -5 -6 392.72 9.81 0 -5 -6 367.64 7.24 0 5 6 373.86 9.55 0 5 6 389.91 7.04 0 5 6 365.50 6.71 0 -5 -7 44.53 3.49 0 -5 -7 31.14 2.23 0 5 7 43.98 3.41 0 5 7 39.09 2.42 0 5 8 93.43 4.09 0 5 8 97.43 5.21 0 -5 -8 106.60 5.68 0 5 9 129.11 5.13 0 5 9 136.30 6.41 0 -5 -9 145.19 7.05 0 -5 -10 43.20 4.05 0 5 10 36.20 2.90 0 5 10 40.81 3.70 0 5 11 11.29 2.07 0 -5 -11 13.17 2.43 0 5 11 12.58 1.88 0 5 12 19.31 2.43 0 -5 -12 24.19 3.33 0 5 12 20.20 2.75 0 5 13 4.92 1.59 0 5 13 3.02 1.19 0 -5 -13 2.81 1.55 0 5 14 10.54 2.29 0 -5 -14 10.33 2.40 0 5 14 5.93 1.58 0 -5 -15 5.44 1.76 0 5 15 2.57 1.27 0 5 15 4.61 1.49 0 5 16 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2.06 0 6 -1 16.93 1.09 0 6 -1 21.09 1.96 0 6 0 1.45 0.30 0 -6 0 2.17 0.81 0 6 0 2.00 0.55 0 6 0 1.80 0.27 0 6 1 64.69 3.39 0 -6 -1 60.15 3.53 0 6 1 70.31 3.78 0 6 2 77.02 4.13 0 6 2 76.37 3.84 0 -6 -2 73.06 1.62 0 6 2 82.24 1.59 0 6 3 67.67 3.98 0 -6 -3 71.84 3.88 0 6 3 71.38 1.90 0 -6 -3 67.67 2.12 0 6 3 69.30 3.79 0 6 4 63.65 3.78 0 6 4 65.13 2.17 0 -6 -4 65.22 3.57 0 -6 -4 62.83 2.40 0 6 4 64.17 4.00 0 -6 -5 10.74 1.15 0 -6 -5 8.94 1.33 0 6 5 11.18 1.05 0 6 5 10.00 1.62 0 -6 -6 1.94 0.64 0 -6 -6 2.39 0.62 0 6 6 2.02 0.55 0 6 6 2.48 0.98 0 6 6 2.66 0.72 0 6 7 0.09 0.51 0 6 7 0.02 0.38 0 -6 -7 0.41 0.69 0 -6 -7 0.33 0.41 0 -6 -8 80.10 5.15 0 6 8 71.28 3.50 0 6 8 75.68 4.87 0 -6 -9 15.86 2.45 0 6 9 11.94 1.64 0 6 9 12.25 2.13 0 6 10 28.65 3.26 0 6 10 22.57 2.32 0 -6 -10 31.88 3.58 0 6 10 20.39 0.83 0 6 11 3.39 1.30 0 6 11 2.83 0.91 0 -6 -11 3.19 1.23 0 -6 -12 3.00 1.46 0 6 12 4.25 1.28 0 6 12 2.05 0.90 0 6 13 27.72 3.54 0 6 13 24.05 2.98 0 -6 -13 31.41 4.10 0 6 14 8.26 1.81 0 6 14 8.23 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5.34 1.71 0 7 16 7.05 2.13 0 -7 -16 12.08 2.95 0 7 16 11.85 2.44 0 7 17 0.74 1.13 0 -7 -17 1.72 1.24 0 7 18 4.57 2.00 0 7 19 -3.53 1.71 0 8 -13 -0.34 0.83 0 -8 13 -0.23 0.81 0 8 -12 -0.20 0.91 0 -8 12 0.39 0.78 0 -8 11 0.58 0.75 0 8 -11 -0.48 0.72 0 -8 10 2.46 1.22 0 -8 10 1.55 0.91 0 8 -10 1.88 1.19 0 8 -10 1.44 0.93 0 8 -9 7.32 1.50 0 8 -9 11.57 2.54 0 -8 9 9.02 1.96 0 -8 9 5.25 1.36 0 8 -8 6.69 1.88 0 -8 8 3.65 1.08 0 -8 8 8.40 1.88 0 8 -8 6.83 1.31 0 -8 7 11.19 2.18 0 -8 7 7.63 1.60 0 8 -7 9.32 1.51 0 -8 6 8.94 1.80 0 -8 6 5.70 1.41 0 8 -6 8.87 1.41 0 -8 5 9.25 1.73 0 8 -5 7.24 1.08 0 -8 5 9.88 1.98 0 8 -4 72.90 3.66 0 -8 4 72.29 4.96 0 8 -4 65.24 3.04 0 -8 4 68.13 4.66 0 8 -3 82.10 4.17 0 8 -3 68.08 2.75 0 -8 3 71.94 4.73 0 8 -2 12.27 0.91 0 8 -2 8.63 0.89 0 -8 2 14.27 2.11 0 8 -2 14.79 1.88 0 -8 1 31.98 3.10 0 8 -1 32.10 2.88 0 8 0 11.06 1.77 0 -8 0 11.93 1.87 0 -8 -1 25.33 2.71 0 8 1 26.43 2.70 0 8 2 27.27 2.86 0 -8 -2 24.93 2.72 0 8 3 73.15 4.79 0 -8 -3 66.91 4.30 0 8 4 40.28 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1.17 -11 -9 -3 -1.20 1.05 -11 -9 -4 -0.76 0.97 -11 -9 -5 -0.30 1.03 -11 -9 -6 3.36 1.58 -12 -1 -3 1.33 1.02 -12 -2 0 12.49 3.00 -12 -2 -1 3.77 1.68 -12 -2 -2 2.87 1.62 -12 -2 -3 1.79 1.44 -12 -2 -4 0.11 1.03 -12 -2 -5 -0.87 1.13 -12 -2 -6 1.82 1.30 -12 -3 1 4.91 1.98 -12 -3 0 4.08 1.69 -12 -3 -1 3.95 1.61 -12 -3 -2 0.46 0.85 -12 -3 -3 -0.43 0.82 -12 -3 -4 1.41 1.11 -12 -3 -5 1.68 1.36 -12 -3 -6 0.41 0.77 -12 -3 -7 -0.03 0.89 -12 -4 1 10.78 2.76 -12 -4 0 10.55 2.79 -12 -4 -1 12.14 2.81 -12 -4 -2 2.02 1.74 -12 -4 -3 5.28 2.11 -12 -4 -4 2.83 1.53 -12 -4 -5 0.48 1.03 -12 -4 -6 4.77 1.88 -12 -4 -7 3.90 1.49 -12 -4 -8 2.80 1.61 -12 -5 2 -3.56 1.46 -12 -5 1 0.56 0.87 -12 -5 1 1.10 1.20 -12 -5 0 0.28 1.29 -12 -5 -1 0.75 0.84 -12 -5 -2 1.59 1.20 -12 -5 -3 4.40 1.82 -12 -5 -4 2.62 1.16 -12 -5 -5 2.73 1.44 -12 -5 -6 1.09 1.10 -12 -5 -7 1.55 1.34 -12 -5 -8 2.14 1.47 -12 -5 -9 2.43 1.26 -12 -6 2 0.14 0.61 -12 -6 1 1.37 1.09 -12 -6 1 0.06 0.79 -12 -6 0 2.47 1.51 -12 -6 0 -0.50 1.21 -12 -6 -1 2.20 1.34 -12 -6 -2 1.67 1.48 -12 -6 -3 2.28 1.11 -12 -6 -4 0.03 0.80 -12 -6 -5 -0.17 0.89 -12 -6 -6 0.38 0.79 -12 -6 -7 1.22 1.18 -12 -6 -8 1.19 1.12 -12 -6 -9 -2.31 1.79 -12 -7 1 -0.98 1.16 -12 -7 0 -2.06 1.08 -12 -7 0 1.65 1.16 -12 -7 -1 -1.17 1.57 -12 -7 -1 2.58 1.46 -12 -7 -2 -0.07 0.71 -12 -7 -2 1.12 1.01 -12 -7 -3 -2.30 1.40 -12 -7 -3 1.21 1.25 -12 -7 -4 -1.45 1.20 -12 -7 -5 -1.11 1.29 -12 -7 -6 1.32 1.05 -12 -7 -7 0.84 0.94 -12 -7 -8 -0.84 1.18 -12 -7 -9 1.93 1.49 -12 -8 -5 4.27 1.81 -12 -8 -6 4.41 1.56 -12 -8 -7 2.35 1.10 0 0 0 0.00 0.00 TITL nt0963_KAMA_A1_EtoAC in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 8.536812 9.659386 13.517300 75.9470 79.3016 74.5541 ZERR 2.00 0.000569 0.000565 0.001155 0.0062 0.0064 0.0054 LATT 1 SFAC C H N O S UNIT 38.00 56.00 4.00 10.00 2.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 78714 _shelx_res_file ; TITL nt0963_kama_a1_etoac_a.res in P-1 nt0963_KAMA_A1_EtoAC.res created by SHELXL-2016/6 at 13:31:49 on 01-Sep-2021 REM Old TITL nt0963_KAMA_A1_EtoAC in P-1 REM SHELXT solution in P-1 REM R1 0.185, Rweak 0.014, Alpha 0.046, Orientation as input REM Formula found by SHELXT: C19 N3 O4 S CELL 0.71073 8.5368 9.6594 13.5173 75.947 79.302 74.554 ZERR 2 0.0006 0.0006 0.0012 0.006 0.006 0.005 LATT 1 SFAC C H N O S UNIT 38 56 4 10 2 L.S. 10 PLAN 4 CONF BOND $H list 4 fmap 2 53 MORE -1 ACTA TEMP 22 CONF HTAB SIZE 0.79 0.18 0.05 WGHT 0.063300 0.120600 FVAR 0.70028 S1 5 0.210063 0.112264 0.499705 11.00000 0.03807 0.03617 = 0.06359 -0.01207 -0.00197 -0.00995 O1 4 0.205456 0.425924 0.580100 11.00000 0.04439 0.04913 = 0.06446 -0.01944 -0.00787 0.00480 O2 4 0.268804 -0.043782 1.006833 11.00000 0.15667 0.06895 = 0.10717 -0.01311 0.00152 -0.02258 O3 4 0.155121 0.162589 1.061934 11.00000 0.10496 0.07996 = 0.06946 -0.01331 0.01438 -0.01741 O4 4 0.211362 0.034805 0.421857 11.00000 0.05979 0.05315 = 0.08286 -0.02799 -0.00431 -0.02125 O5 4 0.256638 0.029434 0.596970 11.00000 0.06291 0.05201 = 0.06694 0.00393 -0.00532 -0.02107 N1 3 0.334610 0.221209 0.455492 11.00000 0.03524 0.03672 = 0.04918 -0.00891 -0.00536 -0.00823 N2 3 0.388209 0.319326 0.692428 11.00000 0.05414 0.05338 = 0.05169 -0.01909 -0.00760 0.00166 C1 1 0.435206 0.242221 0.526067 11.00000 0.03330 0.03756 = 0.05067 -0.01194 -0.00510 -0.00469 AFIX 13 H1 2 0.484975 0.145601 0.564865 11.00000 -1.20000 AFIX 0 C2 1 0.330922 0.335012 0.603071 11.00000 0.03892 0.03816 = 0.05274 -0.01142 -0.00362 -0.00753 C3 1 0.294225 0.408132 0.766762 11.00000 0.07605 0.05381 = 0.05569 -0.02259 -0.00486 -0.00525 AFIX 23 H3A 2 0.212739 0.487753 0.733487 11.00000 -1.20000 H3B 2 0.367076 0.450568 0.791143 11.00000 -1.20000 AFIX 0 C4 1 0.209914 0.315490 0.857230 11.00000 0.05975 0.05997 = 0.05678 -0.02143 -0.00723 -0.00072 AFIX 23 H4A 2 0.126979 0.283509 0.834039 11.00000 -1.20000 H4B 2 0.155721 0.374364 0.908049 11.00000 -1.20000 AFIX 0 C5 1 0.333021 0.180855 0.906795 11.00000 0.06003 0.06469 = 0.05420 -0.01703 -0.01454 -0.00598 AFIX 13 H5 2 0.409068 0.216659 0.934903 11.00000 -1.20000 AFIX 0 C6 1 0.433383 0.096037 0.825465 11.00000 0.06350 0.05873 = 0.06196 -0.01673 -0.02408 0.00941 AFIX 23 H6A 2 0.517049 0.016237 0.856466 11.00000 -1.20000 H6B 2 0.362540 0.054116 0.798864 11.00000 -1.20000 AFIX 0 C7 1 0.513946 0.196349 0.737717 11.00000 0.04899 0.07489 = 0.05978 -0.02472 -0.01523 0.00382 AFIX 23 H7A 2 0.590425 0.233317 0.763271 11.00000 -1.20000 H7B 2 0.574515 0.141684 0.685678 11.00000 -1.20000 AFIX 0 C8 1 0.249374 0.085231 0.995381 11.00000 0.07836 0.06628 = 0.06682 -0.01221 -0.01866 -0.00707 C9 1 0.065039 0.087945 1.152880 11.00000 0.11391 0.09481 = 0.08588 0.00527 0.01355 -0.01943 AFIX 23 H9A 2 0.004626 0.029494 1.132728 11.00000 -1.20000 H9B 2 0.140898 0.023064 1.198758 11.00000 -1.20000 AFIX 0 C10 1 -0.045626 0.195842 1.204021 11.00000 0.12458 0.14344 = 0.09164 0.00851 0.03330 -0.01268 AFIX 137 H10A 2 0.012297 0.263307 1.213528 11.00000 -1.50000 H10B 2 -0.091589 0.148539 1.269779 11.00000 -1.50000 H10C 2 -0.131975 0.248210 1.163132 11.00000 -1.50000 AFIX 0 C11 1 0.571888 0.314221 0.466297 11.00000 0.03635 0.05386 = 0.06442 -0.01998 -0.00007 -0.01394 AFIX 137 H11A 2 0.636931 0.256036 0.418334 11.00000 -1.50000 H11B 2 0.639730 0.321567 0.513158 11.00000 -1.50000 H11C 2 0.525388 0.410564 0.429625 11.00000 -1.50000 AFIX 0 C12 1 0.011817 0.221661 0.519966 11.00000 0.03320 0.05707 = 0.12020 -0.02881 0.00353 -0.01100 AFIX 137 H12A 2 -0.017746 0.283965 0.455966 11.00000 -1.50000 H12B 2 0.008836 0.280954 0.568219 11.00000 -1.50000 H12C 2 -0.064229 0.159986 0.546811 11.00000 -1.50000 AFIX 0 C13 1 0.320556 0.311430 0.353807 11.00000 0.03958 0.04104 = 0.04933 -0.01049 -0.00586 -0.00944 C14 1 0.223082 0.451970 0.339659 11.00000 0.05278 0.04844 = 0.05543 -0.01087 -0.01053 0.00158 AFIX 43 H14 2 0.166814 0.491483 0.396039 11.00000 -1.20000 AFIX 0 C15 1 0.209719 0.533584 0.241014 11.00000 0.05675 0.05682 = 0.06950 -0.00299 -0.01877 0.00067 AFIX 43 H15 2 0.144679 0.628604 0.232086 11.00000 -1.20000 AFIX 0 C16 1 0.289877 0.478424 0.155435 11.00000 0.06074 0.07126 = 0.05403 -0.00238 -0.01122 -0.02355 C17 1 0.389840 0.338509 0.171726 11.00000 0.07911 0.06934 = 0.05338 -0.01682 0.00624 -0.02231 AFIX 43 H17 2 0.447572 0.299605 0.115395 11.00000 -1.20000 AFIX 0 C18 1 0.406028 0.255189 0.269534 11.00000 0.06271 0.04707 = 0.05731 -0.01427 0.00350 -0.01094 AFIX 43 H18 2 0.474265 0.161520 0.278607 11.00000 -1.20000 AFIX 0 C19 1 0.267396 0.568839 0.048390 11.00000 0.09250 0.10597 = 0.06242 0.00848 -0.01671 -0.02241 AFIX 137 H19A 2 0.162225 0.569619 0.032294 11.00000 -1.50000 H19B 2 0.351973 0.526722 -0.000565 11.00000 -1.50000 H19C 2 0.273737 0.667492 0.045582 11.00000 -1.50000 AFIX 0 HKLF 4 REM nt0963_kama_a1_etoac_a.res in P-1 REM R1 = 0.0540 for 4304 Fo > 4sig(Fo) and 0.0932 for all 6870 data REM 248 parameters refined using 0 restraints END WGHT 0.0633 0.1206 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y, -z+1 HTAB C7 O4_$1 EQIV $2 -x, -y, -z+2 HTAB C10 O5_$2 HTAB C12 O1 EQIV $3 -x, -y, -z+1 HTAB C12 O4_$3 HTAB C14 O1 REM Highest difference peak 0.336, deepest hole -0.375, 1-sigma level 0.043 Q1 1 0.1040 0.1747 0.5144 11.00000 0.05 0.34 Q2 1 0.1187 -0.0159 1.1626 11.00000 0.05 0.24 Q3 1 0.1472 0.0975 0.4366 11.00000 0.05 0.23 Q4 1 0.3858 0.2844 0.5646 11.00000 0.05 0.23 ; _shelx_res_checksum 36550 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 S S1 0.21006(5) 0.11226(4) 0.49970(3) 0.04597(14) Uani d 1 . . O O1 0.20546(16) 0.42592(12) 0.58010(10) 0.0542(3) Uani d 1 . . O O2 0.2688(3) -0.0438(2) 1.00683(16) 0.1150(8) Uani d 1 . . O O3 0.1551(3) 0.16259(18) 1.06193(12) 0.0894(5) Uani d 1 . . O O4 0.21136(17) 0.03480(13) 0.42186(11) 0.0618(4) Uani d 1 . . O O5 0.25664(18) 0.02943(13) 0.59697(11) 0.0624(4) Uani d 1 . . N N1 0.33461(16) 0.22121(13) 0.45549(10) 0.0404(3) Uani d 1 . . N N2 0.3882(2) 0.31933(16) 0.69243(11) 0.0543(4) Uani d 1 . . C C1 0.4352(2) 0.24222(16) 0.52607(12) 0.0407(3) Uani d 1 . . H H1 0.484975 0.145601 0.564865 0.049 Uiso calc 1 . . C C2 0.3309(2) 0.33501(16) 0.60307(13) 0.0435(4) Uani d 1 . . C C3 0.2942(3) 0.4081(2) 0.76676(14) 0.0622(5) Uani d 1 . . H H3A 0.212739 0.487753 0.733487 0.075 Uiso calc 1 . . H H3B 0.367076 0.450568 0.791143 0.075 Uiso calc 1 . . C C4 0.2099(3) 0.3155(2) 0.85723(15) 0.0598(5) Uani d 1 . . H H4A 0.126979 0.283509 0.834039 0.072 Uiso calc 1 . . H H4B 0.155721 0.374364 0.908049 0.072 Uiso calc 1 . . C C5 0.3330(3) 0.1809(2) 0.90679(14) 0.0595(5) Uani d 1 . . H H5 0.409068 0.216659 0.934903 0.071 Uiso calc 1 . . C C6 0.4334(3) 0.0960(2) 0.82547(15) 0.0631(5) Uani d 1 . . H H6A 0.517049 0.016237 0.856466 0.076 Uiso calc 1 . . H H6B 0.362540 0.054116 0.798864 0.076 Uiso calc 1 . . C C7 0.5139(3) 0.1963(2) 0.73772(15) 0.0617(5) Uani d 1 . . H H7A 0.590425 0.233317 0.763271 0.074 Uiso calc 1 . . H H7B 0.574515 0.141684 0.685678 0.074 Uiso calc 1 . . C C8 0.2494(3) 0.0852(2) 0.99538(17) 0.0714(6) Uani d 1 . . C C9 0.0650(4) 0.0879(3) 1.1529(2) 0.1069(10) Uani d 1 . . H H9A 0.004626 0.029494 1.132728 0.128 Uiso calc 1 . . H H9B 0.140898 0.023064 1.198758 0.128 Uiso calc 1 . . C C10 -0.0456(5) 0.1958(4) 1.2040(2) 0.1357(14) Uani d 1 . . H H10A 0.012297 0.263307 1.213528 0.204 Uiso calc 1 . . H H10B -0.091589 0.148539 1.269779 0.204 Uiso calc 1 . . H H10C -0.131975 0.248210 1.163132 0.204 Uiso calc 1 . . C C11 0.5719(2) 0.31422(19) 0.46630(14) 0.0503(4) Uani d 1 . . H H11A 0.636931 0.256036 0.418334 0.075 Uiso calc 1 . . H H11B 0.639730 0.321567 0.513158 0.075 Uiso calc 1 . . H H11C 0.525388 0.410564 0.429625 0.075 Uiso calc 1 . . C C12 0.0118(2) 0.2217(2) 0.5200(2) 0.0700(6) Uani d 1 . . H H12A -0.017746 0.283965 0.455966 0.105 Uiso calc 1 . . H H12B 0.008836 0.280954 0.568219 0.105 Uiso calc 1 . . H H12C -0.064229 0.159986 0.546811 0.105 Uiso calc 1 . . C C13 0.3206(2) 0.31143(16) 0.35381(13) 0.0431(4) Uani d 1 . . C C14 0.2231(2) 0.45197(18) 0.33966(14) 0.0543(4) Uani d 1 . . H H14 0.166814 0.491483 0.396039 0.065 Uiso calc 1 . . C C15 0.2097(3) 0.5336(2) 0.24101(16) 0.0641(5) Uani d 1 . . H H15 0.144679 0.628604 0.232086 0.077 Uiso calc 1 . . C C16 0.2899(3) 0.4784(2) 0.15543(15) 0.0617(5) Uani d 1 . . C C17 0.3898(3) 0.3385(2) 0.17173(16) 0.0675(6) Uani d 1 . . H H17 0.447572 0.299605 0.115395 0.081 Uiso calc 1 . . C C18 0.4060(3) 0.25519(19) 0.26953(14) 0.0569(5) Uani d 1 . . H H18 0.474265 0.161520 0.278607 0.068 Uiso calc 1 . . C C19 0.2674(4) 0.5688(3) 0.04839(17) 0.0908(8) Uani d 1 . . H H19A 0.162225 0.569619 0.032294 0.136 Uiso calc 1 . . H H19B 0.351973 0.526722 -0.000565 0.136 Uiso calc 1 . . H H19C 0.273737 0.667492 0.045582 0.136 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 S1 0.0381(2) 0.0362(2) 0.0636(3) -0.00995(16) -0.00197(19) -0.01207(17) O1 0.0444(7) 0.0491(6) 0.0645(8) 0.0048(5) -0.0079(6) -0.0194(5) O2 0.157(2) 0.0689(11) 0.1072(15) -0.0226(12) 0.0015(14) -0.0131(10) O3 0.1050(15) 0.0800(10) 0.0695(10) -0.0174(10) 0.0144(9) -0.0133(8) O4 0.0598(9) 0.0532(7) 0.0829(9) -0.0212(6) -0.0043(7) -0.0280(6) O5 0.0629(9) 0.0520(7) 0.0669(8) -0.0211(6) -0.0053(7) 0.0039(6) N1 0.0352(7) 0.0367(6) 0.0492(7) -0.0082(5) -0.0054(6) -0.0089(5) N2 0.0541(10) 0.0534(8) 0.0517(8) 0.0017(7) -0.0076(7) -0.0191(6) C1 0.0333(8) 0.0376(7) 0.0507(9) -0.0047(6) -0.0051(7) -0.0119(6) C2 0.0389(9) 0.0382(7) 0.0527(9) -0.0075(6) -0.0036(7) -0.0114(6) C3 0.0761(15) 0.0538(10) 0.0557(11) -0.0053(10) -0.0049(10) -0.0226(8) C4 0.0598(13) 0.0600(11) 0.0568(11) -0.0007(9) -0.0072(9) -0.0214(9) C5 0.0600(13) 0.0647(11) 0.0542(11) -0.0060(9) -0.0145(9) -0.0170(8) C6 0.0635(14) 0.0587(10) 0.0620(12) 0.0094(9) -0.0241(10) -0.0167(9) C7 0.0490(12) 0.0749(12) 0.0598(11) 0.0038(9) -0.0152(9) -0.0247(9) C8 0.0784(17) 0.0663(13) 0.0668(13) -0.0071(11) -0.0187(12) -0.0122(10) C9 0.114(3) 0.0948(18) 0.0859(19) -0.0194(18) 0.0136(18) 0.0053(15) C10 0.125(3) 0.143(3) 0.092(2) -0.013(2) 0.033(2) 0.009(2) C11 0.0363(9) 0.0539(9) 0.0644(11) -0.0139(7) -0.0001(8) -0.0200(8) C12 0.0332(10) 0.0571(11) 0.1202(19) -0.0110(8) 0.0035(11) -0.0288(11) C13 0.0396(9) 0.0410(8) 0.0493(9) -0.0094(7) -0.0059(7) -0.0105(6) C14 0.0528(11) 0.0484(9) 0.0554(10) 0.0016(8) -0.0105(9) -0.0109(8) C15 0.0567(13) 0.0568(11) 0.0695(13) 0.0007(9) -0.0188(10) -0.0030(9) C16 0.0607(13) 0.0713(12) 0.0540(11) -0.0235(10) -0.0112(10) -0.0024(9) C17 0.0791(16) 0.0693(12) 0.0534(11) -0.0223(11) 0.0062(10) -0.0168(9) C18 0.0627(13) 0.0471(9) 0.0573(11) -0.0109(8) 0.0035(9) -0.0143(8) C19 0.092(2) 0.1060(19) 0.0624(14) -0.0224(16) -0.0167(14) 0.0085(13) 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 O5 S1 O4 . . 118.43(8) ? O5 S1 N1 . . 106.30(8) ? O4 S1 N1 . . 108.16(8) ? O5 S1 C12 . . 108.50(11) ? O4 S1 C12 . . 107.33(10) ? N1 S1 C12 . . 107.71(8) ? C8 O3 C9 . . 119.1(2) ? C13 N1 C1 . . 122.65(12) ? C13 N1 S1 . . 117.57(11) ? C1 N1 S1 . . 118.92(10) ? C2 N2 C3 . . 119.21(16) ? C2 N2 C7 . . 126.42(15) ? C3 N2 C7 . . 112.45(15) ? N1 C1 C11 . . 110.73(13) ? N1 C1 C2 . . 111.57(13) ? C11 C1 C2 . . 109.61(12) ? N1 C1 H1 . . 108.3 ? C11 C1 H1 . . 108.3 ? C2 C1 H1 . . 108.3 ? O1 C2 N2 . . 121.94(15) ? O1 C2 C1 . . 120.33(15) ? N2 C2 C1 . . 117.58(15) ? N2 C3 C4 . . 110.73(15) ? N2 C3 H3A . . 109.5 ? C4 C3 H3A . . 109.5 ? N2 C3 H3B . . 109.5 ? C4 C3 H3B . . 109.5 ? H3A C3 H3B . . 108.1 ? C3 C4 C5 . . 111.24(18) ? C3 C4 H4A . . 109.4 ? C5 C4 H4A . . 109.4 ? C3 C4 H4B . . 109.4 ? C5 C4 H4B . . 109.4 ? H4A C4 H4B . . 108.0 ? C8 C5 C6 . . 112.44(17) ? C8 C5 C4 . . 111.67(19) ? C6 C5 C4 . . 110.22(16) ? C8 C5 H5 . . 107.4 ? C6 C5 H5 . . 107.4 ? C4 C5 H5 . . 107.4 ? C7 C6 C5 . . 110.66(16) ? C7 C6 H6A . . 109.5 ? C5 C6 H6A . . 109.5 ? C7 C6 H6B . . 109.5 ? C5 C6 H6B . . 109.5 ? H6A C6 H6B . . 108.1 ? N2 C7 C6 . . 109.70(17) ? N2 C7 H7A . . 109.7 ? C6 C7 H7A . . 109.7 ? N2 C7 H7B . . 109.7 ? C6 C7 H7B . . 109.7 ? H7A C7 H7B . . 108.2 ? O2 C8 O3 . . 123.4(2) ? O2 C8 C5 . . 125.1(2) ? O3 C8 C5 . . 111.50(18) ? C10 C9 O3 . . 108.7(2) ? C10 C9 H9A . . 110.0 ? O3 C9 H9A . . 110.0 ? C10 C9 H9B . . 110.0 ? O3 C9 H9B . . 110.0 ? H9A C9 H9B . . 108.3 ? C9 C10 H10A . . 109.5 ? C9 C10 H10B . . 109.5 ? H10A C10 H10B . . 109.5 ? C9 C10 H10C . . 109.5 ? H10A C10 H10C . . 109.5 ? H10B C10 H10C . . 109.5 ? C1 C11 H11A . . 109.5 ? C1 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C1 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? S1 C12 H12A . . 109.5 ? S1 C12 H12B . . 109.5 ? H12A C12 H12B . . 109.5 ? S1 C12 H12C . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? C14 C13 C18 . . 119.67(16) ? C14 C13 N1 . . 121.20(15) ? C18 C13 N1 . . 119.13(14) ? C13 C14 C15 . . 119.47(17) ? C13 C14 H14 . . 120.3 ? C15 C14 H14 . . 120.3 ? C16 C15 C14 . . 122.01(18) ? C16 C15 H15 . . 119.0 ? C14 C15 H15 . . 119.0 ? C15 C16 C17 . . 117.39(18) ? C15 C16 C19 . . 120.6(2) ? C17 C16 C19 . . 122.0(2) ? C18 C17 C16 . . 121.65(19) ? C18 C17 H17 . . 119.2 ? C16 C17 H17 . . 119.2 ? C13 C18 C17 . . 119.76(17) ? C13 C18 H18 . . 120.1 ? C17 C18 H18 . . 120.1 ? C16 C19 H19A . . 109.5 ? C16 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? C16 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 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 S1 O5 . 1.4285(14) y S1 O4 . 1.4286(13) y S1 N1 . 1.6278(13) y S1 C12 . 1.7526(19) y O1 C2 . 1.227(2) y O2 C8 . 1.188(3) y O3 C8 . 1.324(3) y O3 C9 . 1.462(3) y N1 C13 . 1.445(2) y N1 C1 . 1.476(2) y N2 C2 . 1.346(2) y N2 C3 . 1.464(2) y N2 C7 . 1.466(2) y C1 C11 . 1.519(2) y C1 C2 . 1.537(2) y C1 H1 . 0.9800 ? C3 C4 . 1.516(3) y C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 C5 . 1.535(3) y C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 C8 . 1.514(3) y C5 C6 . 1.526(3) y C5 H5 . 0.9800 ? C6 C7 . 1.521(3) y C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? C7 H7A . 0.9700 ? C7 H7B . 0.9700 ? C9 C10 . 1.428(4) y C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C10 H10A . 0.9600 ? C10 H10B . 0.9600 ? C10 H10C . 0.9600 ? C11 H11A . 0.9600 ? C11 H11B . 0.9600 ? C11 H11C . 0.9600 ? C12 H12A . 0.9600 ? C12 H12B . 0.9600 ? C12 H12C . 0.9600 ? C13 C14 . 1.380(2) y C13 C18 . 1.381(2) y C14 C15 . 1.382(3) y C14 H14 . 0.9300 ? C15 C16 . 1.379(3) y C15 H15 . 0.9300 ? C16 C17 . 1.384(3) y C16 C19 . 1.514(3) y C17 C18 . 1.381(3) y C17 H17 . 0.9300 ? C18 H18 . 0.9300 ? C19 H19A . 0.9600 ? C19 H19B . 0.9600 ? C19 H19C . 0.9600 ? 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 C12 H12B O1 . 0.96 2.50 3.210(2) 130.4 C12 H12C O4 2_556 0.96 2.44 3.376(2) 163.7 C14 H14 O1 . 0.93 2.48 3.177(2) 132.3 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 O5 S1 N1 C13 . . . . 176.09(11) ? O4 S1 N1 C13 . . . . 47.92(13) ? C12 S1 N1 C13 . . . . -67.78(14) ? O5 S1 N1 C1 . . . . -14.24(14) ? O4 S1 N1 C1 . . . . -142.40(12) ? C12 S1 N1 C1 . . . . 101.89(14) ? C13 N1 C1 C11 . . . . -25.36(19) ? S1 N1 C1 C11 . . . . 165.51(11) ? C13 N1 C1 C2 . . . . 97.02(16) ? S1 N1 C1 C2 . . . . -72.11(15) ? C3 N2 C2 O1 . . . . 3.0(3) ? C7 N2 C2 O1 . . . . 165.98(18) ? C3 N2 C2 C1 . . . . 178.66(15) ? C7 N2 C2 C1 . . . . -18.4(3) ? N1 C1 C2 O1 . . . . -28.1(2) ? C11 C1 C2 O1 . . . . 94.89(19) ? N1 C1 C2 N2 . . . . 156.17(14) ? C11 C1 C2 N2 . . . . -80.81(18) ? C2 N2 C3 C4 . . . . 106.1(2) ? C7 N2 C3 C4 . . . . -59.1(2) ? N2 C3 C4 C5 . . . . 54.5(2) ? C3 C4 C5 C8 . . . . -178.38(17) ? C3 C4 C5 C6 . . . . -52.6(2) ? C8 C5 C6 C7 . . . . 179.54(18) ? C4 C5 C6 C7 . . . . 54.2(2) ? C2 N2 C7 C6 . . . . -103.4(2) ? C3 N2 C7 C6 . . . . 60.5(2) ? C5 C6 C7 N2 . . . . -57.7(2) ? C9 O3 C8 O2 . . . . -2.2(4) ? C9 O3 C8 C5 . . . . -179.8(2) ? C6 C5 C8 O2 . . . . 6.3(4) ? C4 C5 C8 O2 . . . . 130.8(3) ? C6 C5 C8 O3 . . . . -176.2(2) ? C4 C5 C8 O3 . . . . -51.7(3) ? C8 O3 C9 C10 . . . . -171.3(3) ? C1 N1 C13 C14 . . . . -76.6(2) ? S1 N1 C13 C14 . . . . 92.68(17) ? C1 N1 C13 C18 . . . . 103.66(19) ? S1 N1 C13 C18 . . . . -87.07(18) ? C18 C13 C14 C15 . . . . 1.3(3) ? N1 C13 C14 C15 . . . . -178.45(17) ? C13 C14 C15 C16 . . . . 0.7(3) ? C14 C15 C16 C17 . . . . -2.1(3) ? C14 C15 C16 C19 . . . . 177.7(2) ? C15 C16 C17 C18 . . . . 1.7(3) ? C19 C16 C17 C18 . . . . -178.1(2) ? C14 C13 C18 C17 . . . . -1.7(3) ? N1 C13 C18 C17 . . . . 178.02(17) ? C16 C17 C18 C13 . . . . 0.2(3) ? _cod_database_fobs_code 2243929