#------------------------------------------------------------------------------ #$Date: 2023-07-15 03:48:23 +0200 (Sat, 15 Jul 2023) $ #$Revision: 285220 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022821.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_2022821 loop_ _publ_author_name 'Khalilov, Ali N.' 'Khrustalev, Victor N.' 'Samigullina, Aida I.' 'Akkurt, Mehmet' 'Rzayev, Rovnag M.' 'Bhattarai, Ajaya' 'Mamedov, \.Ibrahim G.' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of (E)-1-(2,4-dimethylfuran-3-yl)-3-phenylprop-2-en-1-one ; _journal_coeditor_code VM2287 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989023006084 _journal_volume 79 _journal_year 2023 _chemical_absolute_configuration ad _chemical_formula_iupac 'C15 H14 O2' _chemical_formula_moiety 'C15 H14 O2' _chemical_formula_sum 'C15 H14 O2' _chemical_formula_weight 226.26 _chemical_name_systematic ; (E)-1-(2,4-Dimethylfuran-3-yl)-3-phenylprop-2-en-1-one ; _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.84787(5) _cell_length_b 12.18109(9) _cell_length_c 16.24568(15) _cell_measurement_reflns_used 10780 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 77.685 _cell_measurement_theta_min 4.505 _cell_volume 1157.236(17) _computing_cell_refinement ; CrysAlisPro 1.171.41.117a (Rigaku OD, 2021) ; _computing_data_collection ; CrysAlisPro 1.171.41.117a (Rigaku OD, 2021) ; _computing_data_reduction ; CrysAlisPro 1.171.41.117a (Rigaku OD, 2021) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\f and \w' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_unetI/netI 0.0217 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 12000 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.774 _diffrn_reflns_theta_min 4.537 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2021) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.299 _exptl_crystal_description prism _exptl_crystal_F_000 480 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.177 _refine_diff_density_min -0.241 _refine_ls_abs_structure_details ; Flack x determined using 940 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.16(7) _refine_ls_extinction_coef 0.0046(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 157 _refine_ls_number_reflns 2410 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0299 _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^)+(0.0426P)^2^+0.3199P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.0806 _reflns_number_gt 2382 _reflns_number_total 2410 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file vm2287sup1.cif _cod_data_source_block I _cod_database_code 2022821 _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 0.854 _shelx_estimated_absorpt_t_max 0.887 _shelx_hkl_file ; 0 0 -1 0.06 0.10 0 0 -2 3277.60 86.97 0 0 -2 3255.78 87.55 0 0 -3 0.49 0.35 0 0 -3 0.09 0.32 0 0 -3 0.30 0.23 0 0 -4 3247.39 87.12 0 0 -4 3148.85 87.73 0 0 -4 3310.48 88.41 0 0 -5 -0.17 0.38 0 0 -5 0.77 0.48 0 0 -5 0.15 0.49 0 0 -6 1087.73 32.41 0 0 -6 1153.21 33.63 0 0 -6 1093.16 34.02 0 0 -7 0.34 0.35 0 0 -7 0.52 0.58 0 0 -7 0.23 0.57 0 0 -7 1.86 0.90 0 0 -8 168.29 9.61 0 0 -8 168.25 8.10 0 0 -8 171.15 9.07 0 0 -9 -0.33 0.52 0 0 -9 -0.39 0.75 0 0 -10 11.81 2.81 0 0 -10 11.42 2.59 0 0 -11 1.89 0.60 0 0 -11 2.32 1.47 0 0 -11 0.53 0.59 0 0 -12 73.18 7.91 0 0 -12 72.16 3.84 0 0 -12 87.82 8.26 0 0 -13 0.73 0.54 0 0 -13 0.60 0.95 0 0 -13 1.32 1.48 0 0 -14 2374.28 77.86 0 0 -14 2285.10 63.64 0 0 -14 2343.05 75.22 0 0 -15 -0.13 0.54 0 0 -15 0.18 0.67 0 0 -15 1.60 2.00 0 0 -16 254.16 10.15 0 0 -17 0.47 0.68 0 0 -18 1707.35 46.70 0 0 -18 1599.34 46.51 0 0 -19 0.72 0.58 0 0 -19 0.29 0.51 0 0 -20 174.93 6.07 0 0 -20 197.64 6.49 0 0 -20 191.90 6.49 0 1 0 0.50 0.15 0 1 -1 116.54 4.01 0 1 -2 1149.15 32.82 0 1 -2 1247.11 33.18 0 -1 -3 74.24 3.23 0 1 -3 75.69 3.60 0 1 -3 78.68 3.81 0 1 -3 72.77 3.62 0 1 -3 79.34 2.86 0 1 3 82.31 2.90 0 1 -4 518.29 16.18 0 -1 -4 496.80 15.70 0 1 -4 519.92 16.51 0 1 -4 519.63 14.54 0 1 4 523.01 14.55 0 -1 -5 0.37 0.47 0 1 -5 0.34 0.46 0 1 -6 644.17 21.66 0 -1 -6 636.34 22.15 0 -1 -6 663.89 20.86 0 1 -6 674.56 21.08 0 1 -6 622.54 21.46 0 1 -7 1.01 0.75 0 1 -7 0.77 0.82 0 -1 -7 0.20 0.51 0 1 -7 0.42 0.53 0 -1 -7 0.28 0.63 0 -1 -7 0.22 0.40 0 -1 -8 26.90 1.92 0 -1 -8 24.87 3.02 0 1 -8 26.50 3.20 0 1 -8 35.11 3.88 0 1 -8 32.18 3.74 0 -1 -8 31.23 3.86 0 -1 -9 319.76 10.98 0 1 -9 364.05 15.94 0 1 -9 323.35 14.30 0 -1 -9 390.56 15.33 0 -1 -9 372.34 16.77 0 1 -9 342.83 15.75 0 -1 -10 20.83 1.93 0 -1 -10 17.24 3.44 0 -1 -10 20.84 3.30 0 1 -10 24.50 3.95 0 1 -10 22.62 3.75 0 -1 -11 477.83 15.05 0 1 -11 486.67 21.83 0 -1 -11 496.68 21.00 0 1 -11 452.91 21.28 0 -1 -11 513.10 23.09 0 1 -12 272.64 15.65 0 -1 -12 256.76 14.54 0 -1 -12 248.79 8.45 0 -1 -12 248.65 8.97 0 1 -12 240.10 8.70 0 -1 -12 236.59 8.33 0 -1 -12 270.96 16.35 0 -1 -13 0.65 0.68 0 -1 -13 1.67 1.53 0 1 -13 0.64 1.61 0 -1 -13 -0.69 1.34 0 -1 -13 0.70 1.35 0 1 -13 0.34 0.44 0 -1 -13 0.52 0.60 0 -1 -13 0.19 0.41 0 -1 -13 -0.10 0.43 0 1 -14 419.48 23.32 0 -1 -14 427.67 23.57 0 -1 -14 458.43 23.83 0 -1 -14 440.53 14.97 0 1 -14 402.91 22.35 0 1 -14 405.09 13.65 0 -1 -14 433.08 14.16 0 1 -15 54.70 7.95 0 -1 -15 57.33 8.13 0 1 -15 57.97 7.76 0 -1 -15 63.42 4.15 0 -1 -15 53.52 3.50 0 1 -15 61.44 3.47 0 1 -16 582.28 18.72 0 -1 -16 583.78 18.55 0 -1 -16 527.31 17.39 0 -1 -17 154.16 6.94 0 1 -17 159.44 7.11 0 1 -18 18.86 1.97 0 -1 -18 19.30 1.93 0 -1 -18 18.08 1.95 0 1 -19 1.10 0.60 0 -1 -19 1.34 0.58 0 -1 -19 0.51 0.53 0 1 -20 0.36 0.34 0 1 -20 1.15 0.44 0 -1 -20 0.53 0.41 0 2 0 3691.44 98.14 0 2 -1 4102.47 109.57 0 2 -2 4106.22 110.07 0 2 -2 4083.74 110.21 0 2 -3 4676.23 127.35 0 -2 -3 4745.28 125.51 0 2 -4 1042.73 28.54 0 2 4 1014.53 28.49 0 2 -4 977.20 29.84 0 -2 -4 991.46 28.28 0 2 -4 998.87 30.22 0 2 -5 807.94 23.18 0 2 5 833.49 23.23 0 2 -5 834.11 25.73 0 -2 -5 748.89 23.57 0 2 -5 814.50 25.20 0 2 -6 8.35 0.99 0 2 6 8.52 1.02 0 2 -6 9.02 1.66 0 2 -6 8.66 1.74 0 -2 -6 7.38 1.70 0 -2 -6 8.93 1.41 0 2 -7 122.77 7.06 0 -2 -7 121.03 6.27 0 2 -7 133.27 7.36 0 -2 -7 114.89 4.75 0 -2 -7 134.12 8.02 0 -2 -8 17.76 2.41 0 2 -8 15.90 2.74 0 -2 -8 18.93 3.14 0 -2 -8 17.23 1.59 0 -2 -9 108.24 6.94 0 2 -9 103.70 8.04 0 2 -9 107.80 7.58 0 -2 -9 106.71 4.82 0 -2 -9 120.19 8.75 0 -2 -10 7.73 1.97 0 2 -10 5.93 1.89 0 -2 -10 7.09 2.35 0 2 -10 6.52 2.16 0 -2 -10 6.59 1.15 0 -2 -11 450.64 13.87 0 -2 -11 441.02 21.14 0 2 -11 450.55 20.73 0 -2 -11 411.79 18.08 0 2 -11 399.18 18.55 0 -2 -11 388.47 12.73 0 -2 -11 406.74 13.22 0 -2 -11 395.18 12.72 0 -2 -11 390.82 13.53 0 -2 -12 95.92 8.08 0 2 -12 103.83 9.61 0 -2 -12 99.58 4.50 0 -2 -12 99.62 4.54 0 2 -12 103.82 4.60 0 -2 -12 95.37 4.82 0 -2 -12 97.12 9.65 0 -2 -12 104.50 5.25 0 -2 -13 276.56 10.30 0 -2 -13 264.69 17.39 0 2 -13 284.18 17.48 0 2 -13 275.61 17.48 0 -2 -13 278.08 17.50 0 -2 -13 260.25 9.24 0 -2 -13 263.64 9.79 0 2 -13 263.72 9.25 0 -2 -13 250.98 9.12 0 -2 -14 294.69 10.90 0 -2 -14 261.35 17.92 0 2 -14 278.51 18.00 0 -2 -14 318.68 19.33 0 2 -14 293.19 18.71 0 -2 -14 279.67 9.71 0 -2 -14 265.87 10.22 0 2 -14 282.92 9.74 0 -2 -14 272.48 9.67 0 -2 -15 1624.19 44.69 0 -2 -15 1546.46 56.69 0 2 -15 1581.25 56.57 0 -2 -15 1551.87 56.95 0 2 -15 1535.15 56.76 0 -2 -15 1461.20 42.86 0 -2 -15 1591.97 43.98 0 -2 -15 1521.52 42.95 0 -2 -16 315.53 11.22 0 -2 -16 327.34 11.84 0 -2 -17 9.34 1.48 0 2 -17 9.91 1.58 0 -2 -18 86.55 4.27 0 2 -18 87.34 4.53 0 -2 -18 85.08 4.40 0 2 -18 91.57 4.50 0 2 -19 18.66 1.70 0 -2 -19 20.50 1.84 0 2 -19 19.17 1.70 0 -2 -19 24.64 1.86 0 2 -20 44.90 2.27 0 -2 -20 53.97 2.50 0 2 20 57.22 2.59 0 2 -20 44.67 2.24 0 -2 -20 42.27 2.19 0 3 0 0.09 0.39 0 3 0 0.06 0.28 0 3 1 319.82 10.09 0 3 -1 323.72 10.38 0 3 -1 325.40 10.89 0 3 -1 305.15 9.01 0 -3 -1 328.96 9.00 0 3 -2 2251.91 59.18 0 3 -2 2136.96 59.56 0 3 2 2087.54 57.57 0 3 -3 1.18 0.64 0 3 -3 0.95 0.54 0 3 -4 263.36 9.27 0 3 4 266.82 9.25 0 -3 -4 230.37 7.44 0 3 -4 255.05 10.10 0 3 -5 3364.62 87.14 0 3 5 3263.80 87.07 0 3 -5 3321.98 89.26 0 -3 -5 3064.03 85.65 0 3 -5 2986.02 88.64 0 3 -6 6.72 1.18 0 3 6 6.09 1.13 0 -3 -6 4.96 0.98 0 3 -6 7.43 1.72 0 3 -6 7.58 1.73 0 -3 -6 8.48 1.00 0 3 7 240.65 8.89 0 3 -7 222.41 8.68 0 -3 -7 248.62 12.24 0 -3 -7 230.49 8.10 0 -3 -7 242.04 9.34 0 3 -7 242.33 11.54 0 3 -7 234.55 11.70 0 -3 -8 9.23 1.25 0 3 -8 12.73 2.60 0 -3 -8 11.26 1.81 0 -3 -8 8.35 2.25 0 3 -8 14.40 2.62 0 -3 -9 582.65 23.70 0 3 -9 567.53 22.36 0 -3 -9 566.60 19.76 0 -3 -9 532.01 17.13 0 -3 -10 14.01 3.33 0 3 -10 11.31 2.71 0 -3 -10 15.51 2.61 0 -3 -10 14.78 1.47 0 -3 -10 15.66 1.64 0 -3 -10 13.63 1.40 0 -3 -10 13.16 1.65 0 -3 -11 29.49 2.46 0 3 -11 36.30 5.14 0 -3 -11 32.79 5.38 0 -3 -11 28.03 2.16 0 -3 -11 27.61 2.30 0 3 -11 26.91 1.99 0 -3 -11 25.91 2.44 0 -3 -11 26.25 2.08 0 3 -12 16.29 3.93 0 -3 -12 15.16 3.77 0 -3 -12 16.10 1.91 0 -3 -12 13.94 3.77 0 3 -12 13.96 3.68 0 -3 -12 17.21 1.75 0 -3 -12 15.47 1.83 0 3 -12 16.06 1.59 0 -3 -12 15.50 1.91 0 -3 -12 18.80 1.79 0 -3 -13 16.82 2.02 0 3 -13 12.41 3.77 0 -3 -13 21.40 4.79 0 -3 -13 20.34 4.47 0 3 -13 15.91 4.12 0 -3 -13 16.14 1.75 0 3 -13 15.30 1.56 0 -3 -13 15.22 1.85 0 -3 -13 14.73 1.66 0 -3 -14 255.29 9.90 0 -3 -14 252.68 17.62 0 3 -14 254.77 17.49 0 -3 -14 251.02 17.27 0 3 -14 256.28 17.16 0 -3 -14 237.89 9.04 0 -3 -14 253.35 9.74 0 -3 -14 258.60 9.22 0 -3 -15 66.96 8.80 0 -3 -15 80.19 4.60 0 3 -15 61.13 8.39 0 -3 -15 70.63 8.93 0 3 -15 68.50 8.80 0 -3 -15 80.91 4.09 0 -3 -15 77.68 4.43 0 -3 -15 74.53 3.95 0 -3 -16 30.17 2.50 0 -3 -16 25.64 2.42 0 -3 -17 0.76 0.65 0 3 -17 1.52 0.82 0 -3 -18 47.39 2.92 0 3 -18 41.83 2.76 0 -3 -18 47.95 3.12 0 3 -18 47.47 3.08 0 3 -19 106.57 4.46 0 -3 -19 113.69 4.52 0 -3 -19 110.97 4.76 0 3 -19 120.95 4.83 0 3 20 83.17 3.35 0 3 -20 78.41 3.20 0 -3 -20 90.00 3.35 0 4 0 4672.58 126.34 0 4 0 4785.56 127.38 0 4 -1 581.96 17.95 0 4 -1 577.16 18.62 0 4 1 576.52 17.74 0 4 -2 1344.09 37.81 0 4 2 1286.39 36.31 0 4 -2 1250.64 35.57 0 -4 -2 1302.67 35.56 0 4 3 762.45 21.98 0 4 -3 811.91 25.12 0 4 -3 788.83 24.53 0 4 -4 889.89 29.04 0 4 -4 912.85 28.80 0 4 4 921.45 27.97 0 4 -4 908.80 28.08 0 4 -5 247.99 10.99 0 4 5 251.87 9.87 0 4 -5 246.30 9.87 0 -4 -5 217.34 7.78 0 4 -6 118.07 7.51 0 4 -6 127.11 6.46 0 4 6 132.81 6.57 0 -4 -6 109.22 4.76 0 4 -7 272.26 13.33 0 4 -7 264.09 13.20 0 4 -7 267.95 10.82 0 4 7 275.67 10.92 0 -4 -7 263.29 9.22 0 4 -8 383.54 17.26 0 4 -8 367.30 16.82 0 -4 -8 327.15 16.85 0 -4 -8 357.52 11.95 0 -4 -9 1951.40 61.20 0 -4 -9 1844.01 52.54 0 4 -9 1928.92 59.97 0 4 -9 2002.80 60.97 0 -4 -9 1857.61 52.13 0 -4 -10 774.77 30.79 0 -4 -10 735.28 21.99 0 4 -10 745.61 30.22 0 4 -10 727.04 29.15 0 -4 -10 718.29 21.90 0 -4 -10 692.16 21.44 0 -4 -10 741.13 21.54 0 -4 -10 715.17 22.32 0 -4 -11 762.78 24.06 0 -4 -11 806.26 32.04 0 4 -11 845.85 32.61 0 -4 -11 801.10 24.58 0 4 -11 831.37 33.81 0 4 -11 763.33 31.68 0 -4 -11 791.14 23.74 0 -4 -11 797.37 23.73 0 -4 -11 819.86 24.28 0 -4 -11 842.30 34.20 0 4 -12 1.24 1.21 0 -4 -12 3.78 2.00 0 -4 -12 1.50 0.72 0 4 -12 1.22 1.53 0 -4 -12 0.74 1.43 0 -4 -12 1.90 0.77 0 -4 -12 2.77 0.86 0 -4 -12 1.31 0.78 0 -4 -12 3.72 1.06 0 -4 -13 18.04 4.21 0 4 -13 17.62 4.25 0 -4 -13 16.29 1.98 0 -4 -13 14.31 4.01 0 -4 -13 14.97 1.76 0 -4 -13 16.34 1.85 0 -4 -13 14.44 1.88 0 -4 -13 16.27 2.03 0 -4 -14 76.63 4.48 0 -4 -14 90.55 10.43 0 4 -14 65.79 8.81 0 -4 -14 71.68 4.40 0 4 -14 67.85 8.45 0 -4 -14 74.09 8.93 0 -4 -14 86.58 4.44 0 -4 -14 74.54 4.16 0 -4 -15 17.28 1.83 0 -4 -15 15.56 1.90 0 -4 -15 17.05 1.84 0 -4 -15 17.23 2.03 0 -4 -16 148.16 6.54 0 -4 -16 153.58 6.53 0 4 -17 0.86 0.72 0 -4 -17 1.70 0.76 0 -4 -17 0.23 0.50 0 4 -17 0.69 0.56 0 -4 -17 0.91 0.58 0 -4 -18 8.07 1.19 0 4 -18 10.28 1.38 0 -4 -18 11.40 1.26 0 -4 -19 3.76 0.59 0 4 19 4.16 0.80 0 4 -19 5.24 0.85 0 -4 -19 4.60 0.83 0 5 0 0.17 0.43 0 5 -1 17.38 2.21 0 5 -1 17.42 1.97 0 5 1 19.12 2.04 0 -5 -2 196.97 6.74 0 5 -2 185.35 8.97 0 5 2 190.55 8.93 0 5 -2 189.74 8.94 0 5 -2 171.87 8.11 0 5 2 193.30 7.54 0 5 -3 419.35 15.03 0 5 3 387.04 14.70 0 5 -3 415.09 15.37 0 5 3 388.22 12.27 0 5 -3 398.50 14.53 0 -5 -3 401.26 11.95 0 -5 -3 367.87 11.72 0 5 4 103.25 6.30 0 5 -4 104.27 6.31 0 5 -4 92.29 6.18 0 5 -4 108.07 6.88 0 -5 -4 114.23 4.53 0 5 -4 85.51 4.75 0 -5 -4 95.38 4.88 0 5 -5 1071.11 32.40 0 5 5 1019.10 32.07 0 5 -5 1022.53 33.68 0 5 -5 1032.15 33.23 0 -5 -5 982.35 28.81 0 5 -5 969.48 30.67 0 -5 -5 1026.57 30.79 0 5 -6 176.05 9.04 0 5 6 179.05 9.03 0 5 -6 201.31 10.65 0 -5 -6 173.81 6.82 0 -5 -6 177.05 8.71 0 5 -6 186.06 8.94 0 -5 -7 203.40 10.16 0 5 -7 208.41 10.31 0 -5 -7 191.19 7.56 0 5 -7 193.21 9.61 0 5 7 208.15 9.93 0 -5 -7 184.09 11.41 0 5 -7 214.22 11.85 0 -5 -8 90.97 4.19 0 5 -8 99.08 8.31 0 5 -8 102.93 8.38 0 -5 -8 86.45 4.10 0 5 -8 88.23 5.90 0 -5 -8 93.78 4.73 0 -5 -8 83.44 6.66 0 5 -8 87.02 6.79 0 5 -9 127.70 9.08 0 -5 -9 150.14 9.68 0 -5 -9 143.40 6.23 0 5 -9 153.86 10.98 0 5 -9 134.04 10.35 0 -5 -9 131.83 5.52 0 -5 -9 126.09 5.49 0 5 -9 125.01 5.02 0 -5 -9 119.55 5.63 0 -5 -10 19.19 3.63 0 5 -10 20.18 3.76 0 -5 -10 16.90 1.85 0 5 -10 15.27 3.57 0 5 -10 18.63 4.08 0 -5 -10 14.67 1.66 0 -5 -10 18.01 1.80 0 -5 -10 17.38 1.93 0 -5 -10 17.39 2.08 0 -5 -11 456.24 21.91 0 5 -11 483.64 22.47 0 -5 -11 506.14 15.79 0 -5 -11 499.00 24.83 0 5 -11 485.80 23.74 0 5 -11 492.42 24.56 0 -5 -11 459.11 15.37 0 -5 -11 462.06 15.35 0 -5 -11 458.75 15.72 0 -5 -11 483.65 16.24 0 -5 -12 124.13 10.72 0 5 -12 125.63 10.69 0 -5 -12 127.99 6.10 0 -5 -12 126.64 12.00 0 5 -12 129.55 11.94 0 5 -12 128.23 11.37 0 -5 -12 135.35 6.11 0 -5 -12 132.54 6.09 0 -5 -12 136.35 6.62 0 -5 -12 134.81 6.39 0 -5 -13 40.35 6.20 0 5 -13 42.76 6.29 0 -5 -13 32.09 2.96 0 -5 -13 43.63 7.28 0 5 -13 41.67 6.92 0 -5 -13 41.55 3.11 0 -5 -13 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22.88 2.46 -5 -4 -7 22.91 2.21 -5 4 7 23.14 2.21 -5 4 7 27.15 1.99 5 4 -7 20.88 1.92 -5 -4 -6 101.79 5.15 5 4 -6 93.98 4.69 -5 4 6 116.94 4.79 -5 -4 -6 109.60 5.27 -5 4 6 116.05 4.98 -5 -4 -6 115.18 5.46 -5 4 6 103.10 5.26 -5 4 5 103.91 4.73 -5 4 5 108.23 4.99 -5 -4 -5 109.41 5.45 -5 -4 -5 106.28 5.40 -5 -4 -5 107.96 5.37 -5 4 5 97.83 5.19 -5 -4 -4 21.29 2.32 -5 -4 -4 24.29 2.46 -5 -4 -4 23.87 2.42 -5 4 4 20.99 2.05 -5 4 4 20.93 2.27 -5 4 4 19.63 1.89 -5 4 4 21.28 2.21 -5 -4 -4 20.57 2.17 -5 4 3 25.17 2.41 -5 4 3 23.90 5.45 -5 -4 -3 24.06 2.58 -5 -4 -3 23.19 2.50 -5 -4 -3 23.57 2.18 -5 4 3 24.25 2.25 -5 4 3 26.54 2.54 -5 4 3 29.57 2.33 -5 -4 -3 27.90 2.70 -5 4 2 371.58 12.91 -5 -4 -2 368.84 12.86 -5 4 2 333.00 12.46 -5 4 2 347.49 22.46 -5 -4 -2 370.81 13.52 -5 -4 -2 363.23 13.35 -5 4 2 384.22 12.84 -5 4 2 370.84 13.02 -5 4 2 383.24 12.59 -5 -4 -2 379.38 13.52 -5 4 1 336.86 11.79 -5 4 1 336.81 11.65 -5 4 1 312.26 21.08 -5 -4 -1 303.08 12.15 -5 4 1 330.96 11.77 -5 -4 -1 306.02 11.75 -5 4 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1.39 -5 6 5 5.92 0.99 -5 -6 -5 8.38 1.44 -5 6 5 6.49 1.29 -5 6 4 51.47 3.61 -5 6 4 56.71 3.11 -5 -6 -4 53.25 3.65 -5 6 4 55.81 3.08 -5 6 4 54.85 3.53 -5 -6 -4 55.19 3.74 -5 -6 -4 49.33 3.54 -5 6 4 54.11 3.48 -5 6 3 122.24 5.22 -5 6 3 119.30 5.18 -5 -6 -3 123.15 6.11 -5 -6 -3 110.79 5.82 -5 -6 -3 114.42 5.93 -5 6 3 111.69 5.75 -5 6 3 122.51 5.64 -5 6 2 10.50 1.40 -5 -6 -2 10.48 1.73 -5 6 2 9.67 1.59 -5 -6 -2 10.99 1.74 -5 6 2 11.17 1.54 -5 6 2 11.89 1.50 -5 -6 -1 96.63 5.48 -5 6 1 98.62 5.26 -5 6 1 101.73 4.78 -5 6 1 101.06 4.94 -5 6 1 102.54 4.80 -5 6 0 1.44 0.71 -5 -6 0 1.77 0.93 -5 6 0 0.87 0.68 -5 6 0 1.48 0.73 -5 6 0 1.41 0.69 -5 6 0 0.77 0.75 -5 6 -1 108.29 4.95 -5 6 -1 101.95 4.80 -5 -6 1 99.49 5.59 -5 6 -1 107.31 5.11 -5 -6 1 95.15 5.43 -5 6 -1 97.78 5.16 -5 6 -2 12.30 1.54 -5 6 -2 13.95 1.62 -5 -6 2 13.03 1.93 -5 -6 2 11.21 1.71 -5 6 -2 10.58 1.40 -5 6 -2 12.57 1.72 -5 6 -2 10.59 1.47 -5 6 -3 128.71 5.37 -5 -6 3 130.79 6.38 -5 6 -3 121.51 5.42 -5 -6 3 122.57 6.06 -5 -6 3 111.97 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4.81 -6 -4 -3 115.54 5.23 -6 4 3 106.64 4.57 -6 -4 -3 100.70 4.90 -6 4 2 74.06 3.69 -6 4 2 70.73 3.68 -6 -4 -2 65.61 3.89 -6 4 2 69.06 3.51 -6 -4 -2 65.67 3.81 -6 -4 -1 186.34 7.18 -6 4 1 181.53 7.08 -6 4 1 195.13 7.18 -6 -4 -1 195.44 7.35 -6 4 1 188.01 7.04 -6 -4 0 116.13 5.24 -6 4 0 115.29 5.04 -6 4 0 118.31 4.94 -6 -4 0 100.19 5.02 -6 -4 0 114.44 5.45 -6 -4 0 113.73 5.35 -6 4 0 118.73 4.98 -6 4 -1 167.21 6.74 -6 -4 1 179.60 7.24 -6 4 -1 189.35 6.68 -6 -4 1 174.30 7.11 -6 -4 1 180.20 7.34 -6 -4 1 178.27 7.21 -6 -4 2 62.83 3.77 -6 -4 2 58.23 3.58 -6 -4 2 63.37 3.75 -6 4 -2 69.59 3.45 -6 -4 2 64.89 3.67 -6 4 -3 107.88 4.61 -6 -4 3 97.06 4.97 -6 -4 3 90.76 4.75 -6 -4 3 99.00 4.85 -6 4 -3 115.34 4.61 -6 -4 3 102.54 4.78 -6 4 -4 253.81 8.69 -6 -4 4 257.71 9.12 -6 -4 4 251.68 8.89 -6 4 -4 259.82 8.59 -6 4 -5 57.37 2.91 -6 -4 5 51.76 3.18 -6 4 -5 58.45 2.82 -6 -4 5 59.64 3.02 -6 -4 6 195.23 7.59 -6 4 -6 201.83 6.84 -6 -4 6 202.92 7.46 -6 -4 6 206.40 6.86 -6 -4 7 21.28 1.82 -6 -4 7 19.81 1.66 -6 -4 8 38.54 2.36 -6 -4 8 42.32 2.29 -6 -4 9 42.71 2.22 -6 -4 9 42.86 2.10 -6 -4 10 42.05 1.86 -6 5 10 6.34 0.62 -6 5 10 7.40 0.64 -6 5 9 38.62 1.91 -6 5 9 38.06 1.92 -6 5 8 24.79 1.61 -6 5 8 25.26 1.68 -6 5 7 29.91 1.90 -6 5 6 113.35 4.09 -6 5 6 124.53 4.76 -6 5 6 120.01 4.17 -6 5 5 67.09 2.99 -6 5 5 66.59 3.27 -6 5 5 68.88 3.45 -6 5 5 74.00 3.08 -6 5 4 13.68 1.47 -6 5 4 13.75 1.28 -6 -5 -4 16.75 1.64 -6 5 4 14.94 1.43 -6 5 4 16.24 1.36 -6 -5 -4 14.06 1.48 -6 5 3 73.83 3.48 -6 5 3 76.05 3.77 -6 -5 -3 77.07 3.98 -6 5 3 79.31 3.54 -6 -5 -3 76.66 3.94 -6 5 2 73.88 3.55 -6 5 2 79.43 3.78 -6 -5 -2 70.36 3.95 -6 -5 -2 71.38 3.89 -6 5 2 77.11 3.57 -6 5 1 48.53 2.79 -6 5 1 48.97 2.84 -6 -5 -1 52.07 3.00 -6 5 1 50.03 2.80 -6 5 0 18.47 1.64 -6 -5 0 15.85 1.62 -6 5 0 14.78 1.47 -6 -5 0 15.76 1.66 -6 -5 0 13.28 1.66 -6 5 0 17.15 1.57 -6 -5 0 12.21 1.62 -6 -5 1 49.11 3.03 -6 5 -1 48.77 2.81 -6 5 -1 44.67 2.62 -6 -5 1 48.39 3.06 -6 -5 1 48.28 3.10 -6 -5 1 52.31 3.18 -6 -5 2 69.36 3.82 -6 -5 2 76.97 3.95 -6 -5 2 74.71 3.97 -6 -5 2 69.64 3.77 -6 5 -2 74.02 3.50 -6 -5 3 75.05 4.02 -6 -5 3 72.73 3.88 -6 5 -3 84.66 3.64 -6 -5 3 79.17 3.91 -6 5 -4 16.88 1.47 -6 -5 4 14.57 1.65 -6 -5 4 17.15 1.64 -6 5 -4 15.76 1.39 -6 -5 4 15.91 1.54 -6 5 -5 69.66 3.18 -6 -5 5 63.93 3.46 -6 -5 5 68.82 3.21 -6 5 -6 124.54 4.49 -6 -5 6 113.26 5.04 -6 -5 6 117.35 4.90 -6 -5 6 121.32 4.37 -6 -5 7 29.20 2.07 -6 -5 7 33.49 2.04 -6 -5 8 24.32 1.71 -6 -5 8 24.23 1.59 -6 -5 9 39.20 1.94 -6 -5 9 35.03 1.67 -6 6 9 90.85 3.12 -6 6 8 3.93 0.58 -6 6 8 4.02 0.57 -6 6 7 66.80 2.89 -6 6 7 70.41 2.98 -6 6 6 15.50 1.25 -6 6 6 14.53 1.25 -6 6 6 12.06 0.88 -6 6 5 54.22 2.70 -6 6 5 53.43 2.27 -6 6 5 59.47 2.48 -6 6 4 49.65 2.33 -6 -6 -4 54.37 2.86 -6 6 4 48.87 2.58 -6 6 4 51.50 2.44 -6 -6 -4 48.70 2.72 -6 6 3 60.86 2.79 -6 6 3 55.17 2.99 -6 -6 -3 65.15 3.34 -6 -6 -3 62.29 3.24 -6 6 3 59.53 2.84 -6 6 2 18.50 1.50 -6 6 2 20.52 1.67 -6 -6 -2 22.36 1.92 -6 6 2 20.77 1.58 -6 -6 -2 19.88 1.79 -6 6 1 38.18 2.24 -6 6 1 40.47 2.40 -6 6 1 38.99 2.28 -6 6 0 3.12 0.76 -6 -6 0 1.66 0.63 -6 -6 0 1.50 0.70 -6 -6 0 1.89 0.73 -6 6 0 2.56 0.69 -6 6 0 3.17 0.72 -6 6 -1 44.34 2.45 -6 6 -1 41.47 2.37 -6 -6 1 39.27 2.68 -6 -6 1 37.91 2.54 -6 -6 1 43.04 2.72 -6 6 -2 21.86 1.66 -6 -6 2 19.69 1.75 -6 6 -2 20.40 1.56 -6 -6 2 19.84 1.83 -6 -6 2 22.15 1.92 -6 6 -2 25.31 1.73 -6 -6 2 19.06 1.75 -6 -6 3 60.65 3.30 -6 -6 3 63.06 3.32 -6 6 -3 63.33 2.95 -6 -6 3 64.13 3.25 -6 6 -4 52.37 2.61 -6 -6 4 50.10 2.94 -6 -6 4 53.48 2.85 -6 6 -4 53.49 2.51 -6 -6 4 50.39 2.70 -6 -6 5 48.72 2.86 -6 6 -5 57.01 2.61 -6 -6 5 57.36 2.98 -6 -6 5 54.28 2.59 -6 -6 6 13.74 1.31 -6 -6 6 12.84 0.95 -6 -6 7 67.46 3.17 -6 -6 7 72.07 3.04 -6 -6 8 4.01 0.56 -6 -6 8 3.39 0.61 -6 7 7 29.09 1.49 -6 7 7 32.16 1.52 -6 7 6 57.64 2.45 -6 7 6 58.28 2.48 -6 7 5 71.11 2.89 -6 7 5 66.90 2.91 -6 7 5 67.90 2.55 -6 7 4 2.40 0.52 -6 7 4 2.62 0.50 -6 -7 -4 2.63 0.59 -6 7 4 2.03 0.38 -6 7 3 5.62 0.67 -6 7 3 5.64 0.75 -6 -7 -3 5.52 0.90 -6 -7 -3 6.13 0.94 -6 7 2 1.58 0.51 -6 -7 -2 1.45 0.59 -6 -7 -2 2.10 0.61 -6 7 2 1.18 0.51 -6 7 2 1.29 0.45 -6 7 1 97.66 4.02 -6 7 1 101.54 3.86 -6 7 1 101.78 3.95 -6 7 0 82.70 3.47 -6 7 0 89.12 3.64 -6 -7 0 84.09 3.97 -6 -7 0 84.14 3.74 -6 -7 0 86.47 3.97 -6 7 0 90.63 3.61 -6 7 -1 100.78 3.91 -6 -7 1 98.84 4.35 -6 -7 1 96.86 4.20 -6 7 -1 102.40 3.97 -6 -7 1 95.64 4.25 -6 7 -2 1.10 0.46 -6 -7 2 1.86 0.61 -6 -7 2 1.64 0.61 -6 -7 2 2.25 0.68 -6 7 -2 1.78 0.50 -6 7 -2 1.94 0.55 -6 -7 3 5.88 0.91 -6 7 -3 5.23 0.75 -6 -7 3 5.19 0.84 -6 7 -3 4.40 0.77 -6 -7 3 4.85 0.82 -6 -7 4 3.00 0.64 -6 -7 4 2.41 0.57 -6 -7 4 2.29 0.63 -6 -7 5 71.80 3.11 -6 -7 5 68.85 3.05 -6 -7 5 62.19 2.56 -6 -7 6 57.91 2.66 -6 -7 6 58.22 2.61 -6 -7 7 31.14 1.54 -6 8 5 8.97 0.73 -6 8 4 19.03 1.18 -6 8 4 17.72 1.00 -6 -8 -3 62.62 2.71 -6 8 3 64.19 2.62 -6 -8 -3 61.01 2.67 -6 8 3 65.48 2.50 -6 -8 -2 43.70 2.28 -6 -8 -2 45.20 2.27 -6 8 2 45.40 2.05 -6 8 1 10.97 0.95 -6 -8 0 17.08 1.40 -6 8 0 16.89 1.22 -6 -8 0 18.67 1.42 -6 8 0 18.96 1.25 -6 8 -1 10.68 0.95 -6 -8 1 9.44 0.98 -6 -8 1 10.76 1.10 -6 -8 1 10.60 1.06 -6 8 -2 43.75 2.02 -6 8 -2 43.25 2.02 -6 -8 2 45.31 2.22 -6 -8 2 41.25 2.19 -6 -8 2 45.86 2.29 -6 -8 3 57.68 2.51 -6 8 -3 61.63 2.40 -6 -8 3 56.28 2.63 -6 -8 3 62.59 2.66 -6 -8 5 8.99 0.81 -6 9 1 24.77 1.19 -6 -9 -1 22.79 1.28 -6 -9 0 80.83 3.05 -6 9 0 90.14 2.98 -6 -9 0 86.72 3.14 -6 -9 1 26.37 1.38 -7 0 0 -0.13 0.37 -7 0 0 0.06 0.51 -7 0 1 57.33 2.67 -7 0 -1 57.84 2.63 -7 0 1 58.01 2.73 -7 0 2 1.14 0.50 -7 0 -2 0.65 0.46 -7 0 3 64.60 2.66 -7 0 -3 63.61 2.71 -7 0 3 59.53 2.77 -7 0 4 75.54 2.85 -7 0 4 80.71 3.17 -7 0 5 145.91 4.85 -7 0 6 19.39 1.07 -7 1 5 4.95 0.60 -7 1 4 91.37 3.24 -7 1 4 94.12 3.50 -7 1 3 7.02 0.79 -7 -1 -3 6.80 0.86 -7 1 3 8.34 0.88 -7 1 2 28.96 1.72 -7 -1 -2 30.75 1.79 -7 1 2 31.65 1.82 -7 1 1 177.12 5.99 -7 1 0 47.54 2.35 -7 -1 0 46.68 2.39 -7 1 0 46.69 2.36 -7 -1 0 48.30 2.36 -7 -1 1 182.82 6.19 -7 -1 1 187.61 6.26 -7 1 -1 180.24 6.13 -7 1 -2 29.78 1.73 -7 -1 2 28.46 1.69 -7 -1 2 29.47 1.73 -7 1 -2 26.46 1.59 -7 1 -3 8.33 0.89 -7 -1 3 9.31 0.92 -7 -1 3 8.86 0.93 -7 -1 4 89.95 3.24 -7 -1 4 95.35 3.59 -7 -1 5 4.29 0.60 -7 -1 6 43.04 1.82 -7 2 5 28.78 1.38 -7 2 4 1.23 0.38 -7 2 4 0.84 0.31 -7 2 3 139.64 4.69 -7 -2 -3 140.44 4.83 -7 2 3 147.00 4.89 -7 -2 -2 83.51 3.38 -7 2 2 86.95 3.30 -7 2 2 85.77 3.39 -7 2 1 67.70 2.84 -7 2 1 64.45 2.86 -7 -2 0 46.00 2.27 -7 2 0 43.51 2.18 -7 -2 0 41.57 2.11 -7 -2 1 63.50 2.89 -7 -2 1 65.03 2.89 -7 -2 2 88.56 3.38 -7 2 -2 88.16 3.33 -7 -2 2 79.75 3.29 -7 -2 2 84.30 3.44 -7 2 -2 84.74 3.29 -7 2 -3 146.19 4.68 -7 -2 3 135.00 4.62 -7 -2 3 131.50 4.75 -7 -2 4 0.84 0.37 -7 -2 4 1.23 0.39 -7 -2 4 0.92 0.32 -7 -2 5 32.39 1.65 -7 -2 6 11.37 0.80 -7 3 4 216.91 6.50 -7 -3 -3 31.26 1.58 -7 3 3 28.08 1.43 -7 3 3 28.23 1.50 -7 -3 -2 83.75 3.24 -7 3 2 86.59 3.13 -7 3 2 79.18 3.16 -7 3 1 135.68 4.54 -7 3 1 126.75 4.53 -7 -3 0 73.74 3.11 -7 3 0 79.63 3.06 -7 -3 1 125.87 4.46 -7 3 -1 124.59 4.37 -7 -3 2 82.86 3.14 -7 3 -2 86.00 3.10 -7 -3 2 77.56 3.08 -7 3 -2 80.67 3.08 -7 -3 2 75.69 3.12 -7 3 -3 27.92 1.44 -7 -3 3 28.74 1.47 -7 -3 3 28.07 1.55 -7 3 -3 28.02 1.44 -7 -3 3 29.63 1.61 -7 -3 4 225.33 6.96 -7 -3 5 5.68 0.60 -7 -4 -3 17.51 1.03 -7 4 3 19.20 1.01 -7 4 2 139.86 4.44 -7 -4 -2 135.89 4.56 -7 4 2 138.87 4.47 -7 4 1 329.62 9.34 -7 4 1 307.34 9.31 -7 4 0 5.28 0.64 -7 -4 0 5.76 0.70 -7 4 0 5.81 0.66 -7 -4 1 299.67 8.93 -7 4 -2 144.73 4.46 -7 -4 2 129.72 4.44 -7 4 -2 136.49 4.46 -7 -4 3 18.10 1.09 -7 4 -3 17.14 1.00 -7 -4 3 18.82 1.10 -7 -4 4 21.28 1.15 -7 -5 0 24.14 1.25 -7 5 0 25.01 1.20 -7 5 0 24.73 1.19 -7 5 -1 91.27 3.05 0 0 0 0.00 0.00 TITL 23VKh_R078a_auto in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 5.847867 12.181018 16.245681 90.0000 90.0000 90.0000 ZERR 4.00 0.000046 0.000088 0.000147 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H O UNIT 60.00 56.00 8.00 REM CrysAlisPro recorded range (K): Min=99.8; max=100.1; aver:99.9 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 44678 _shelx_res_file ; TITL AN27 in P2(1)2(1)2(1) CELL 1.54184 5.84787 12.18109 16.24568 90.0000 90.0000 90.0000 ZERR 4.00 0.00005 0.00009 0.00015 0.0000 0.0000 0.0000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H O UNIT 60 56 8 TEMP -173.0 SIZE 0.18 0.20 0.24 L.S. 12 BOND $H ACTA CONF WGHT 0.042600 0.319900 EXTI 0.004626 FVAR 1.08802 O1 3 -0.124952 0.421589 0.523341 11.00000 0.01891 0.02437 = 0.02422 0.00255 0.00206 -0.00166 O2 3 0.421825 0.639772 0.514857 11.00000 0.01947 0.02226 = 0.02066 -0.00484 0.00294 -0.00317 C1 1 -0.032705 0.596063 0.585478 11.00000 0.01861 0.02347 = 0.02113 0.00012 0.00388 0.00273 AFIX 137 H1A 2 -0.193579 0.590298 0.601812 11.00000 -1.50000 H1B 2 -0.006354 0.667211 0.558963 11.00000 -1.50000 H1C 2 0.064739 0.589804 0.634331 11.00000 -1.50000 AFIX 0 C2 1 0.023389 0.506624 0.526978 11.00000 0.01609 0.01750 = 0.01867 0.00337 -0.00192 0.00095 C3 1 0.199144 0.490662 0.471376 11.00000 0.01546 0.01711 = 0.01608 0.00171 -0.00127 0.00052 C4 1 0.151752 0.388008 0.430279 11.00000 0.01899 0.01752 = 0.01844 0.00086 -0.00158 0.00145 C5 1 -0.043142 0.349811 0.463793 11.00000 0.01902 0.01599 = 0.02411 -0.00054 -0.00084 -0.00303 AFIX 43 H5 2 -0.115023 0.282810 0.448751 11.00000 -1.20000 AFIX 0 C6 1 0.389731 0.569014 0.462088 11.00000 0.01549 0.01671 = 0.01721 0.00108 -0.00137 0.00201 C7 1 0.538176 0.561930 0.388639 11.00000 0.01893 0.01848 = 0.01775 -0.00250 0.00085 -0.00062 AFIX 43 H7 2 0.501203 0.512201 0.345603 11.00000 -1.20000 AFIX 0 C8 1 0.724679 0.625334 0.382472 11.00000 0.01809 0.01544 = 0.01717 -0.00108 -0.00074 0.00207 AFIX 43 H8 2 0.752796 0.674188 0.426916 11.00000 -1.20000 AFIX 0 C9 1 0.889551 0.627581 0.314894 11.00000 0.01552 0.01700 = 0.01605 0.00102 0.00018 0.00094 C10 1 1.058515 0.708878 0.315320 11.00000 0.01918 0.01823 = 0.02038 -0.00347 0.00025 -0.00165 AFIX 43 H10 2 1.061063 0.761533 0.358447 11.00000 -1.20000 AFIX 0 C11 1 1.222507 0.713738 0.253650 11.00000 0.01917 0.02079 = 0.02505 -0.00115 0.00365 -0.00562 AFIX 43 H11 2 1.336008 0.769516 0.254740 11.00000 -1.20000 AFIX 0 C12 1 1.220736 0.636901 0.190190 11.00000 0.01927 0.02239 = 0.02003 0.00057 0.00436 0.00085 AFIX 43 H12 2 1.333067 0.639955 0.148008 11.00000 -1.20000 AFIX 0 C13 1 1.053758 0.555707 0.188882 11.00000 0.02247 0.02185 = 0.01993 -0.00471 0.00239 -0.00184 AFIX 43 H13 2 1.051825 0.503330 0.145560 11.00000 -1.20000 AFIX 0 C14 1 0.890140 0.550788 0.250443 11.00000 0.01932 0.02007 = 0.02264 -0.00416 0.00233 -0.00545 AFIX 43 H14 2 0.777064 0.494824 0.249033 11.00000 -1.20000 AFIX 0 C15 1 0.281984 0.328376 0.364800 11.00000 0.02216 0.01868 = 0.02583 -0.00603 0.00139 -0.00091 AFIX 137 H15A 2 0.263738 0.366723 0.312178 11.00000 -1.50000 H15B 2 0.223123 0.253350 0.359758 11.00000 -1.50000 H15C 2 0.444382 0.326002 0.379582 11.00000 -1.50000 AFIX 0 HKLF 4 REM AN27 in P2(1)2(1)2(1) REM R1 = 0.0299 for 2382 Fo > 4sig(Fo) and 0.0302 for all 2410 data REM 157 parameters refined using 0 restraints END WGHT 0.0426 0.3199 REM Highest difference peak 0.177, deepest hole -0.241, 1-sigma level 0.038 Q1 1 0.0291 0.3745 0.4393 11.00000 0.05 0.18 Q2 1 1.1460 0.5918 0.1978 11.00000 0.05 0.17 Q3 1 -0.0663 0.3654 0.4237 11.00000 0.05 0.16 Q4 1 0.9370 0.6823 0.2999 11.00000 0.05 0.16 Q5 1 -0.2720 0.4405 0.4862 11.00000 0.05 0.15 Q6 1 0.2681 0.5325 0.4604 11.00000 0.05 0.14 Q7 1 0.8673 0.5979 0.2809 11.00000 0.05 0.14 Q8 1 0.9159 0.5755 0.2926 11.00000 0.05 0.14 Q9 1 -0.1809 0.3019 0.4649 11.00000 0.05 0.14 Q10 1 0.4507 0.5549 0.4281 11.00000 0.05 0.14 Q11 1 0.2146 0.3641 0.4021 11.00000 0.05 0.13 Q12 1 0.5795 0.6151 0.3777 11.00000 0.05 0.13 Q13 1 0.9983 0.5571 0.2209 11.00000 0.05 0.13 Q14 1 0.3271 0.5098 0.4756 11.00000 0.05 0.12 Q15 1 0.7939 0.6302 0.3376 11.00000 0.05 0.12 Q16 1 0.1847 0.4391 0.4427 11.00000 0.05 0.12 Q17 1 -0.2314 0.4992 0.5160 11.00000 0.05 0.11 Q18 1 0.2091 0.4288 0.4601 11.00000 0.05 0.11 Q19 1 0.1390 0.4797 0.6035 11.00000 0.05 0.11 Q20 1 -0.0027 0.5553 0.5577 11.00000 0.05 0.11 ; _shelx_res_checksum 90211 _shelxl_version_number .2013 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 O O1 -0.1250(2) 0.42159(10) 0.52334(8) 0.0225(3) Uani d 1 . . O O2 0.4218(2) 0.63977(10) 0.51486(7) 0.0208(3) Uani d 1 . . C C1 -0.0327(3) 0.59606(14) 0.58548(11) 0.0211(4) Uani d 1 . . H H1A -0.1936 0.5903 0.6018 0.032 Uiso calc 1 . . H H1B -0.0064 0.6672 0.5590 0.032 Uiso calc 1 . . H H1C 0.0647 0.5898 0.6343 0.032 Uiso calc 1 . . C C2 0.0234(3) 0.50662(13) 0.52698(10) 0.0174(3) Uani d 1 . . C C3 0.1991(3) 0.49066(13) 0.47138(10) 0.0162(3) Uani d 1 . . C C4 0.1518(3) 0.38801(13) 0.43028(10) 0.0183(4) Uani d 1 . . C C5 -0.0431(3) 0.34981(13) 0.46379(11) 0.0197(3) Uani d 1 . . H H5 -0.1150 0.2828 0.4488 0.024 Uiso calc 1 . . C C6 0.3897(3) 0.56901(13) 0.46209(10) 0.0165(3) Uani d 1 . . C C7 0.5382(3) 0.56193(14) 0.38864(10) 0.0184(3) Uani d 1 . . H H7 0.5012 0.5122 0.3456 0.022 Uiso calc 1 . . C C8 0.7247(3) 0.62533(13) 0.38247(10) 0.0169(3) Uani d 1 . . H H8 0.7528 0.6742 0.4269 0.020 Uiso calc 1 . . C C9 0.8896(3) 0.62758(13) 0.31489(10) 0.0162(3) Uani d 1 . . C C10 1.0585(3) 0.70888(13) 0.31532(11) 0.0193(3) Uani d 1 . . H H10 1.0611 0.7615 0.3584 0.023 Uiso calc 1 . . C C11 1.2225(3) 0.71374(14) 0.25365(11) 0.0217(4) Uani d 1 . . H H11 1.3360 0.7695 0.2547 0.026 Uiso calc 1 . . C C12 1.2207(3) 0.63690(14) 0.19019(11) 0.0206(4) Uani d 1 . . H H12 1.3331 0.6400 0.1480 0.025 Uiso calc 1 . . C C13 1.0538(3) 0.55571(14) 0.18888(11) 0.0214(4) Uani d 1 . . H H13 1.0518 0.5033 0.1456 0.026 Uiso calc 1 . . C C14 0.8901(3) 0.55079(14) 0.25044(11) 0.0207(3) Uani d 1 . . H H14 0.7771 0.4948 0.2490 0.025 Uiso calc 1 . . C C15 0.2820(3) 0.32838(14) 0.36480(11) 0.0222(4) Uani d 1 . . H H15A 0.2637 0.3667 0.3122 0.033 Uiso calc 1 . . H H15B 0.2231 0.2534 0.3598 0.033 Uiso calc 1 . . H H15C 0.4444 0.3260 0.3796 0.033 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 O1 0.0189(6) 0.0244(6) 0.0242(6) -0.0017(5) 0.0021(5) 0.0025(5) O2 0.0195(6) 0.0223(6) 0.0207(6) -0.0032(5) 0.0029(5) -0.0048(5) C1 0.0186(7) 0.0235(8) 0.0211(8) 0.0027(7) 0.0039(7) 0.0001(6) C2 0.0161(7) 0.0175(7) 0.0187(8) 0.0009(6) -0.0019(6) 0.0034(6) C3 0.0155(7) 0.0171(7) 0.0161(7) 0.0005(6) -0.0013(6) 0.0017(6) C4 0.0190(8) 0.0175(8) 0.0184(7) 0.0015(6) -0.0016(6) 0.0009(6) C5 0.0190(7) 0.0160(7) 0.0241(8) -0.0030(6) -0.0008(7) -0.0005(6) C6 0.0155(7) 0.0167(7) 0.0172(7) 0.0020(6) -0.0014(6) 0.0011(6) C7 0.0189(7) 0.0185(7) 0.0177(7) -0.0006(6) 0.0009(6) -0.0025(6) C8 0.0181(7) 0.0154(7) 0.0172(7) 0.0021(6) -0.0007(6) -0.0011(6) C9 0.0155(7) 0.0170(7) 0.0160(7) 0.0009(6) 0.0002(6) 0.0010(6) C10 0.0192(8) 0.0182(7) 0.0204(8) -0.0017(7) 0.0003(7) -0.0035(6) C11 0.0192(8) 0.0208(8) 0.0250(8) -0.0056(7) 0.0037(7) -0.0011(7) C12 0.0193(8) 0.0224(8) 0.0200(8) 0.0008(7) 0.0044(7) 0.0006(7) C13 0.0225(8) 0.0218(8) 0.0199(8) -0.0018(7) 0.0024(7) -0.0047(7) C14 0.0193(7) 0.0201(8) 0.0226(8) -0.0055(7) 0.0023(7) -0.0042(6) C15 0.0222(8) 0.0187(8) 0.0258(9) -0.0009(7) 0.0014(7) -0.0060(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 O1 C5 . . 106.96(13) ? C2 C1 H1A . . 109.5 ? C2 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? C2 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? O1 C2 C3 . . 109.92(14) ? O1 C2 C1 . . 116.68(14) ? C3 C2 C1 . . 133.39(16) ? C2 C3 C4 . . 106.33(14) ? C2 C3 C6 . . 122.53(15) ? C4 C3 C6 . . 131.14(15) ? C5 C4 C3 . . 105.95(15) ? C5 C4 C15 . . 123.41(16) ? C3 C4 C15 . . 130.63(15) ? C4 C5 O1 . . 110.84(14) ? C4 C5 H5 . . 124.6 ? O1 C5 H5 . . 124.6 ? O2 C6 C3 . . 119.83(15) ? O2 C6 C7 . . 120.92(15) ? C3 C6 C7 . . 119.25(14) ? C8 C7 C6 . . 120.31(15) ? C8 C7 H7 . . 119.8 ? C6 C7 H7 . . 119.8 ? C7 C8 C9 . . 127.15(15) ? C7 C8 H8 . . 116.4 ? C9 C8 H8 . . 116.4 ? C10 C9 C14 . . 118.27(15) ? C10 C9 C8 . . 118.39(14) ? C14 C9 C8 . . 123.32(15) ? C11 C10 C9 . . 120.97(15) ? C11 C10 H10 . . 119.5 ? C9 C10 H10 . . 119.5 ? C10 C11 C12 . . 120.04(16) ? C10 C11 H11 . . 120.0 ? C12 C11 H11 . . 120.0 ? C13 C12 C11 . . 119.66(16) ? C13 C12 H12 . . 120.2 ? C11 C12 H12 . . 120.2 ? C14 C13 C12 . . 120.33(15) ? C14 C13 H13 . . 119.8 ? C12 C13 H13 . . 119.8 ? C13 C14 C9 . . 120.75(16) ? C13 C14 H14 . . 119.6 ? C9 C14 H14 . . 119.6 ? C4 C15 H15A . . 109.5 ? C4 C15 H15B . . 109.5 ? H15A C15 H15B . . 109.5 ? C4 C15 H15C . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 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 O1 C2 . 1.352(2) ? O1 C5 . 1.389(2) ? O2 C6 . 1.230(2) ? C1 C2 . 1.482(2) ? C1 H1A . 0.9800 ? C1 H1B . 0.9800 ? C1 H1C . 0.9800 ? C2 C3 . 1.382(2) ? C3 C4 . 1.444(2) ? C3 C6 . 1.475(2) ? C4 C5 . 1.346(2) ? C4 C15 . 1.496(2) ? C5 H5 . 0.9500 ? C6 C7 . 1.478(2) ? C7 C8 . 1.340(2) ? C7 H7 . 0.9500 ? C8 C9 . 1.461(2) ? C8 H8 . 0.9500 ? C9 C10 . 1.399(2) ? C9 C14 . 1.404(2) ? C10 C11 . 1.388(2) ? C10 H10 . 0.9500 ? C11 C12 . 1.392(2) ? C11 H11 . 0.9500 ? C12 C13 . 1.390(2) ? C12 H12 . 0.9500 ? C13 C14 . 1.385(2) ? C13 H13 . 0.9500 ? C14 H14 . 0.9500 ? C15 H15A . 0.9800 ? C15 H15B . 0.9800 ? C15 H15C . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C8 H8 O2 . 0.95 2.44 2.792(2) 102 no C10 H10 O2 4_566 0.95 2.52 3.413(2) 157 yes C12 H12 Cg1 2_664 0.95 2.91 3.7339(19) 146 yes C15 H15B Cg2 3_645 0.98 2.85 3.6366(19) 137 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 C5 O1 C2 C3 . . . . -0.31(17) ? C5 O1 C2 C1 . . . . 178.43(14) ? O1 C2 C3 C4 . . . . 0.56(18) ? C1 C2 C3 C4 . . . . -177.90(17) ? O1 C2 C3 C6 . . . . -179.00(14) ? C1 C2 C3 C6 . . . . 2.5(3) ? C2 C3 C4 C5 . . . . -0.59(18) ? C6 C3 C4 C5 . . . . 178.92(17) ? C2 C3 C4 C15 . . . . -179.55(17) ? C6 C3 C4 C15 . . . . 0.0(3) ? C3 C4 C5 O1 . . . . 0.42(18) ? C15 C4 C5 O1 . . . . 179.47(15) ? C2 O1 C5 C4 . . . . -0.08(18) ? C2 C3 C6 O2 . . . . 14.5(2) ? C4 C3 C6 O2 . . . . -164.92(16) ? C2 C3 C6 C7 . . . . -164.79(15) ? C4 C3 C6 C7 . . . . 15.8(3) ? O2 C6 C7 C8 . . . . 6.9(2) ? C3 C6 C7 C8 . . . . -173.80(15) ? C6 C7 C8 C9 . . . . 179.30(15) ? C7 C8 C9 C10 . . . . 172.52(16) ? C7 C8 C9 C14 . . . . -8.9(3) ? C14 C9 C10 C11 . . . . 0.1(3) ? C8 C9 C10 C11 . . . . 178.70(16) ? C9 C10 C11 C12 . . . . -0.1(3) ? C10 C11 C12 C13 . . . . 0.2(3) ? C11 C12 C13 C14 . . . . -0.2(3) ? C12 C13 C14 C9 . . . . 0.2(3) ? C10 C9 C14 C13 . . . . -0.1(3) ? C8 C9 C14 C13 . . . . -178.66(16) ? _cod_database_fobs_code 2022821