#------------------------------------------------------------------------------ #$Date: 2023-05-06 12:48:58 +0200 (Sat, 06 May 2023) $ #$Revision: 283596 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022699.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_2022699 loop_ _publ_author_name 'Naghiyev, Farid N.' 'Khrustalev, Victor N.' 'Novikov, Anton P.' 'Akkurt, Mehmet' 'Khalilov, Ali N.' 'Bhattarai, Ajaya' 'Mamedov, İbrahim G' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of 2,5-di-imino-8a-methyl-4,9-bis-(4-methyl-phen-yl)-7-oxo-6-phenyl-deca-hydro-2H-3,8-methano-pyrano[3,2-c]pyridine-3,4a-dicarbo-nitrile N,N-di-methyl-formamide monosolvate. ; _journal_coeditor_code WM5672 _journal_issue 'Pt 4' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 254 _journal_page_last 258 _journal_paper_doi 10.1107/S2056989023001718 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'C32 H27 N5 O2, C3 H7 N O' _chemical_formula_moiety 'C32 H27 N5 O2, C3 H7 N O' _chemical_formula_sum 'C35 H34 N6 O3' _chemical_formula_weight 586.68 _chemical_name_common ;2,5-Diimino-8a-methyl-4,9-bis(4-methylphenyl)-7-oxo-6-phenyl-decahydro-2H-3,8-methanopyrano[3,2-c]pyridine-3,4a-dicarbonitrile N,N-dimethylformamide monosolvate ; _chemical_name_systematic ;4,10-Diimino-8-methyl-2,11-bis(4-methylphenyl)-6-oxo-5-phenyl-9-oxa-5-azatricyclo[5.3.1.0^3,8^]undecane-1,3-dicarbonitrile N,N-dimethylformamide monosolvate ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 105.666(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.6747(3) _cell_length_b 15.7656(2) _cell_length_c 10.9086(2) _cell_measurement_reflns_used 19771 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 79.0 _cell_measurement_theta_min 3.8 _cell_volume 2926.79(9) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2021) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2021) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2021) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.965 _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 0.0507 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 31226 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.491 _diffrn_reflns_theta_min 3.822 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2021) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.331 _exptl_crystal_description prism _exptl_crystal_F_000 1240 _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.339 _refine_diff_density_min -0.364 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 408 _refine_ls_number_reflns 6140 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0587 _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^)+(0.0745P)^2^+3.3477P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1600 _refine_ls_wR_factor_ref 0.1656 _reflns_number_gt 5275 _reflns_number_total 6140 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5672sup1.cif _cod_data_source_block I _cod_depositor_comments 'Adding full bibliography for 2022699.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2022699 _cod_database_fobs_code 2022699 _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 0.908 _shelx_estimated_absorpt_t_max 0.946 _shelx_hkl_file ; 0 0 1 0.80 0.64 0 0 1 0.79 0.56 0 0 2 8626.00 431.33 0 0 2 8885.90 431.57 0 0 3 0.50 1.79 0 0 4 2901.06 144.80 0 0 5 -0.23 2.54 0 0 5 -2.06 2.61 0 0 -5 -1.71 2.62 0 0 6 85.34 7.39 0 0 -6 107.13 7.75 0 0 6 98.23 7.64 0 0 7 3.50 3.24 0 0 7 -1.09 3.02 0 0 7 -0.72 3.14 0 0 -7 -1.33 2.99 0 0 8 947.26 53.96 0 0 8 1121.84 56.03 0 0 -8 1083.74 55.62 0 0 8 1076.58 55.92 0 0 8 1114.03 56.10 0 0 -9 -4.76 4.23 0 0 9 -3.19 4.27 0 0 9 -0.46 4.03 0 0 9 1.13 2.67 0 0 9 1.43 3.86 0 0 10 104.55 9.00 0 0 10 98.98 8.98 0 0 -10 93.85 8.53 0 0 10 82.77 7.16 0 0 10 87.43 8.39 0 0 11 -1.17 3.74 0 0 11 -3.80 3.07 0 0 11 -3.74 3.69 0 0 12 171.40 10.51 0 0 12 134.52 9.62 0 1 0 0.54 0.38 0 -1 -1 798.20 42.09 0 -1 1 880.37 42.22 0 -1 1 863.33 41.95 0 1 1 842.46 42.19 0 -1 2 367.43 18.61 0 -1 2 356.93 18.22 0 1 2 357.04 18.43 0 1 3 2444.80 123.14 0 -1 3 2588.74 123.51 0 -1 -3 2426.24 123.26 0 -1 4 1004.84 50.13 0 -1 -4 960.02 49.83 0 -1 5 206.62 13.17 0 -1 -5 234.90 13.16 0 1 -5 227.40 13.29 0 1 5 222.61 13.34 0 -1 5 228.47 13.39 0 -1 5 217.56 13.29 0 -1 -6 8.55 3.03 0 1 -6 13.89 3.34 0 -1 6 10.54 3.23 0 -1 6 12.87 3.38 0 -1 6 10.88 3.24 0 -1 -7 16.55 4.14 0 1 -7 20.05 4.29 0 -1 7 30.43 4.66 0 -1 7 16.78 4.43 0 -1 7 23.73 4.53 0 -1 8 10.70 4.40 0 1 8 5.07 2.80 0 -1 8 10.51 2.86 0 1 -8 10.94 3.93 0 -1 -8 12.80 3.85 0 -1 8 12.10 3.56 0 -1 8 9.46 3.67 0 -1 8 12.20 4.31 0 -1 9 54.64 6.43 0 -1 9 50.78 6.43 0 -1 9 30.88 4.34 0 1 9 34.41 4.51 0 -1 -9 37.16 5.57 0 1 -9 42.93 6.06 0 -1 9 29.56 5.75 0 1 9 41.30 5.92 0 -1 10 78.83 6.84 0 1 10 73.59 7.82 0 1 10 67.21 6.43 0 -1 10 85.45 8.23 0 -1 10 98.39 8.87 0 1 10 79.07 8.27 0 -1 10 83.27 8.57 0 -1 10 103.04 8.96 0 -1 -10 77.67 7.77 0 1 -10 72.57 7.94 0 -1 11 130.38 9.61 0 -1 11 102.55 9.01 0 1 11 110.32 8.79 0 -1 11 113.49 8.77 0 -1 11 98.52 7.59 0 -1 12 64.34 5.58 0 1 12 62.61 5.70 0 1 12 52.90 5.66 0 -1 12 65.56 5.92 0 1 13 250.88 13.50 0 2 0 3605.01 178.23 0 -2 1 2153.62 106.27 0 -2 -1 2157.49 106.40 0 2 -1 2358.17 106.67 0 -2 1 2031.45 106.52 0 2 1 2114.12 106.51 0 2 -2 6.48 2.08 0 2 2 6.19 2.17 0 -2 2 5.16 1.32 0 2 2 4.46 1.85 0 -2 2 4.74 1.99 0 -2 -2 3.46 1.61 0 -2 3 168.45 9.62 0 2 3 171.28 9.61 0 -2 3 172.85 8.97 0 2 3 165.66 9.43 0 -2 -3 158.94 9.30 0 -2 -4 5276.41 263.01 0 2 4 5252.41 262.98 0 2 4 5234.97 263.30 0 -2 4 5478.10 263.39 0 -2 -5 170.30 10.18 0 -2 5 178.45 10.62 0 2 5 163.62 10.45 0 -2 5 175.90 10.57 0 2 5 166.56 10.51 0 2 5 153.09 10.29 0 -2 5 154.82 10.33 0 2 -6 159.69 10.58 0 -2 -6 160.17 10.06 0 2 -6 143.33 9.84 0 -2 6 150.31 10.36 0 2 6 144.63 10.32 0 -2 6 164.83 10.55 0 2 6 152.68 10.39 0 2 6 151.64 10.42 0 -2 6 164.03 10.60 0 -2 -7 26.19 4.06 0 2 -7 31.96 4.79 0 2 7 29.47 4.49 0 -2 7 28.22 4.47 0 2 -7 22.92 3.94 0 2 7 24.52 4.43 0 -2 7 22.89 4.41 0 -2 7 21.95 4.24 0 2 7 18.85 4.11 0 2 -8 130.23 9.29 0 -2 -8 100.68 8.48 0 -2 8 80.45 7.67 0 2 -8 92.26 8.29 0 -2 8 113.21 9.04 0 2 8 121.05 9.24 0 -2 8 118.79 9.21 0 -2 8 116.19 9.10 0 2 8 108.10 8.87 0 2 8 102.98 8.79 0 2 8 87.33 7.31 0 -2 8 90.97 7.39 0 2 9 286.19 18.36 0 -2 9 293.36 18.34 0 -2 9 304.36 18.56 0 2 9 306.53 18.52 0 -2 9 259.26 16.65 0 2 9 249.50 16.53 0 2 9 287.68 18.28 0 -2 9 312.41 18.58 0 2 -9 310.27 18.60 0 -2 -9 286.06 17.80 0 -2 10 12.57 4.58 0 2 -10 14.43 4.55 0 -2 -10 15.21 4.18 0 -2 10 12.70 3.48 0 2 10 13.14 4.76 0 -2 10 9.22 4.58 0 -2 10 9.33 4.39 0 2 10 9.23 4.13 0 -2 10 16.08 4.68 0 2 10 20.76 4.82 0 -2 11 180.72 11.95 0 2 11 177.99 11.83 0 2 11 170.69 11.71 0 -2 11 175.51 11.92 0 -2 11 160.89 11.21 0 -2 11 141.03 10.28 0 2 12 3.04 2.93 0 -2 12 2.97 2.77 0 2 12 5.03 2.80 0 2 13 10.56 2.02 0 3 0 2.98 1.68 0 -3 -1 1809.04 78.72 0 -3 1 1349.86 78.76 0 3 1 1401.78 78.74 0 3 1 1824.10 79.29 0 3 -1 1862.62 79.27 0 -3 2 94.55 5.32 0 3 2 93.54 5.95 0 -3 2 90.49 5.97 0 -3 -3 492.65 25.25 0 -3 3 474.79 24.78 0 3 3 505.92 25.66 0 3 -3 519.83 25.55 0 3 3 514.58 25.61 0 -3 3 487.82 25.62 0 3 4 17.64 2.95 0 3 -4 15.99 2.73 0 -3 4 18.51 2.84 0 3 4 16.42 2.80 0 -3 -4 21.53 2.62 0 3 -5 189.45 11.96 0 3 5 192.51 12.15 0 -3 5 187.30 12.16 0 -3 5 209.23 12.41 0 3 5 216.18 12.44 0 3 5 213.62 12.43 0 -3 5 212.61 12.47 0 -3 -5 212.95 11.91 0 3 -6 50.05 4.92 0 -3 6 30.97 4.65 0 3 6 35.50 4.73 0 3 6 29.86 4.52 0 -3 6 41.63 4.97 0 -3 6 42.89 4.92 0 3 6 46.53 5.01 0 -3 -6 34.38 4.38 0 -3 -7 58.56 5.95 0 -3 7 66.61 6.50 0 3 7 57.94 6.26 0 3 -7 69.58 6.34 0 -3 7 60.83 5.45 0 -3 7 70.18 6.70 0 3 7 70.30 6.61 0 -3 7 74.54 6.72 0 3 7 73.86 6.59 0 3 8 271.26 16.43 0 -3 8 240.94 16.18 0 -3 8 292.76 16.76 0 3 8 278.47 16.57 0 3 8 240.84 15.85 0 -3 8 247.40 15.05 0 3 8 259.81 16.40 0 -3 8 260.70 16.34 0 -3 8 194.44 15.02 0 3 -8 265.81 16.09 0 3 8 219.40 15.57 0 -3 -8 260.42 15.70 0 3 -8 284.80 16.82 0 3 -9 188.55 13.22 0 -3 -9 155.46 11.91 0 3 -9 145.44 12.20 0 3 9 186.58 12.97 0 -3 9 215.06 13.44 0 3 9 193.91 12.93 0 -3 9 186.10 12.98 0 3 9 201.81 13.11 0 -3 9 185.97 12.93 0 -3 9 134.55 11.62 0 -3 9 158.11 11.39 0 -3 10 445.16 24.62 0 3 10 404.65 24.58 0 3 10 416.52 24.29 0 -3 10 424.86 24.71 0 -3 10 440.00 24.52 0 3 10 450.84 24.58 0 -3 10 380.16 22.94 0 -3 10 392.98 23.68 0 3 -10 377.12 24.43 0 3 11 1.05 3.53 0 -3 11 7.03 3.67 0 -3 11 3.19 3.18 0 -3 11 6.66 2.85 0 -3 11 5.02 3.53 0 3 11 3.50 3.12 0 3 12 4.54 2.59 0 -3 12 5.20 2.75 0 3 -12 5.41 2.79 0 3 13 33.73 2.90 0 4 0 470.29 24.13 0 4 1 8687.57 445.67 0 -4 1 8808.11 445.73 0 4 1 9190.76 446.29 0 4 1 9785.32 446.43 0 4 -1 9999.00 446.37 0 -4 -1 9522.93 446.26 0 -4 -1 8875.59 445.68 0 4 2 1215.62 58.61 0 -4 2 1173.38 58.65 0 4 -2 1318.75 59.06 0 -4 2 1084.57 58.03 0 -4 -2 1292.45 58.96 0 -4 -2 1272.91 58.38 0 -4 2 1149.24 58.84 0 4 -3 267.23 14.79 0 -4 -3 271.16 14.27 0 4 3 270.96 14.65 0 -4 3 279.27 14.76 0 -4 -4 681.32 34.78 0 4 -4 664.86 35.20 0 4 4 685.38 35.37 0 4 4 665.18 35.20 0 -4 4 704.25 35.36 0 -4 -5 202.37 11.82 0 4 -5 215.35 12.44 0 -4 5 194.01 12.28 0 4 5 195.24 12.31 0 4 5 202.63 12.37 0 -4 5 215.25 12.48 0 -4 5 210.95 12.49 0 4 5 190.93 12.25 0 4 5 221.95 12.46 0 4 -6 137.67 9.60 0 -4 -6 136.14 8.68 0 -4 6 137.48 9.38 0 4 6 104.49 8.84 0 -4 6 143.56 9.42 0 4 6 125.02 9.10 0 4 -6 131.94 9.09 0 -4 6 135.55 9.24 0 4 6 111.31 8.97 0 -4 7 7.50 2.68 0 4 7 7.61 3.32 0 -4 7 8.21 3.41 0 4 7 6.96 3.17 0 4 7 9.91 3.56 0 -4 7 10.22 3.53 0 4 7 6.09 3.32 0 4 -7 11.02 3.72 0 4 7 5.47 3.42 0 -4 7 12.31 3.67 0 -4 -7 4.30 2.81 0 -4 7 5.44 2.71 0 4 8 30.50 5.18 0 -4 8 51.38 6.04 0 4 8 41.77 5.57 0 4 8 37.72 5.65 0 -4 8 40.37 5.76 0 -4 8 43.48 4.84 0 -4 8 42.21 5.74 0 4 8 41.93 5.61 0 4 -8 33.86 5.64 0 -4 8 33.29 4.89 0 -4 -8 35.45 4.92 0 4 9 252.86 16.24 0 -4 9 275.70 16.60 0 4 9 255.40 16.06 0 -4 9 251.16 15.32 0 -4 9 273.43 16.61 0 -4 9 259.57 16.57 0 4 9 242.87 16.33 0 4 9 267.90 16.38 0 4 -9 222.66 16.09 0 -4 9 211.92 15.39 0 -4 10 298.16 17.80 0 -4 10 284.77 18.13 0 4 10 303.32 18.54 0 -4 10 324.10 19.00 0 4 10 292.28 18.51 0 4 10 308.34 18.68 0 -4 10 321.45 18.91 0 -4 11 16.03 3.26 0 4 11 13.95 4.02 0 4 11 17.33 3.72 0 -4 11 16.39 3.77 0 4 11 13.91 3.73 0 -4 11 13.78 3.80 0 -4 12 2.16 2.27 0 -5 0 -0.61 1.76 0 5 0 1.28 1.82 0 5 1 254.51 12.46 0 5 -1 252.00 12.38 0 -5 1 219.20 12.14 0 -5 -1 247.67 12.22 0 5 1 234.84 12.20 0 -5 1 208.78 11.22 0 5 -2 505.29 23.25 0 5 2 452.94 23.22 0 -5 2 404.51 22.02 0 5 2 453.68 22.47 0 -5 2 437.12 22.56 0 -5 -2 494.88 23.19 0 -5 -2 460.32 22.24 0 -5 2 451.53 23.08 0 5 -3 959.05 48.75 0 -5 3 935.05 48.46 0 5 3 966.98 48.38 0 -5 -3 963.62 47.98 0 -5 -3 957.00 48.69 0 -5 -4 9.05 2.86 0 5 4 7.06 2.95 0 5 -4 5.11 2.73 0 5 4 9.62 2.21 0 -5 4 7.93 2.42 0 -5 -4 5.72 1.86 0 5 5 11.48 2.82 0 -5 5 14.88 3.02 0 5 -5 19.24 3.46 0 5 5 12.31 3.38 0 -5 5 14.99 2.96 0 5 5 17.30 3.06 0 5 5 16.92 3.02 0 -5 5 14.11 2.94 0 -5 -5 13.64 2.50 0 5 6 189.13 12.15 0 5 6 192.49 12.13 0 -5 6 200.07 12.35 0 -5 6 196.08 12.30 0 5 -6 186.51 12.22 0 5 -6 192.11 12.60 0 -5 -6 194.29 11.47 0 -5 6 199.51 12.30 0 5 6 182.25 12.05 0 5 -7 248.78 14.91 0 -5 -7 226.30 13.46 0 -5 7 240.68 14.48 0 5 7 218.90 14.06 0 -5 7 252.90 14.61 0 5 7 224.90 14.21 0 5 7 225.13 14.20 0 -5 7 232.57 14.37 0 -5 7 224.33 13.75 0 5 7 196.41 13.83 0 5 -7 231.08 14.48 0 -5 7 192.96 13.53 0 -5 -8 173.16 12.60 0 5 -8 196.36 13.53 0 5 8 183.19 12.81 0 -5 8 199.16 13.15 0 -5 8 188.69 13.01 0 5 8 190.21 12.74 0 -5 8 199.05 12.93 0 5 8 177.12 12.65 0 5 8 172.79 12.57 0 -5 8 194.49 12.31 0 5 -8 190.13 13.19 0 -5 8 180.11 12.38 0 5 -9 24.49 5.28 0 -5 9 20.58 4.59 0 5 9 16.50 4.52 0 -5 9 17.98 4.80 0 -5 -9 17.59 4.77 0 5 9 23.28 5.04 0 -5 9 9.61 4.50 0 5 9 18.79 4.52 0 5 -9 22.31 5.47 0 -5 9 25.67 4.24 0 -5 9 15.84 4.71 0 5 9 18.71 4.52 0 -5 10 146.75 10.11 0 5 10 144.17 10.63 0 5 10 148.66 10.71 0 -5 10 155.67 10.86 0 -5 10 146.85 10.84 0 5 10 150.34 10.63 0 5 10 129.67 10.41 0 -5 11 11.01 2.89 0 -5 11 16.28 3.57 0 5 11 12.36 3.81 0 5 11 19.20 3.49 0 -5 11 13.82 3.52 0 5 12 2.01 2.58 0 -5 12 1.23 1.58 0 6 0 2017.64 97.61 0 -6 0 1892.97 97.34 0 6 1 204.19 11.71 0 6 -1 216.92 11.92 0 6 1 224.97 12.02 0 -6 -1 216.09 11.76 0 -6 1 190.49 11.69 0 6 -2 1037.44 47.00 0 6 2 982.37 46.97 0 -6 2 941.75 46.78 0 6 2 943.06 45.79 0 -6 2 960.98 45.95 0 -6 -2 1028.07 46.88 0 -6 2 826.21 45.56 0 -6 3 776.65 40.55 0 6 3 825.30 40.45 0 6 -3 781.77 41.13 0 -6 -3 794.47 40.01 0 -6 -3 818.09 41.12 0 6 3 793.21 41.30 0 -6 -4 21.15 3.63 0 6 -4 27.22 3.80 0 -6 4 22.40 2.94 0 6 4 20.21 2.82 0 -6 -4 21.70 2.32 0 6 -5 132.10 8.88 0 -6 5 149.43 8.64 0 6 5 112.60 8.26 0 6 5 134.43 8.33 0 -6 5 124.64 8.54 0 -6 -5 125.43 8.63 0 -6 -5 123.15 7.61 0 6 5 134.93 8.98 0 6 5 103.82 8.12 0 -6 5 123.13 8.39 0 6 -6 246.28 14.40 0 -6 -6 214.85 13.58 0 6 6 202.60 13.31 0 6 6 214.31 13.42 0 -6 6 254.02 13.96 0 -6 6 220.16 13.67 0 6 6 203.27 13.57 0 6 -6 237.83 14.12 0 -6 6 229.29 13.69 0 6 6 209.48 13.41 0 -6 -7 273.66 17.03 0 6 -7 308.46 18.04 0 6 7 287.24 17.03 0 -6 7 324.57 17.56 0 -6 7 294.96 17.26 0 6 7 290.04 17.08 0 6 7 269.95 16.96 0 -6 7 307.48 17.36 0 6 7 256.11 16.87 0 6 -7 288.50 17.55 0 -6 7 253.82 16.78 0 6 -8 29.96 5.19 0 -6 8 33.45 4.87 0 -6 8 23.74 4.57 0 6 8 23.61 4.54 0 6 8 30.44 4.99 0 -6 -8 24.36 4.84 0 -6 8 27.67 4.87 0 6 8 26.57 4.51 0 -6 8 33.15 4.40 0 6 -8 23.78 5.45 0 -6 8 28.62 4.74 0 6 8 24.65 4.35 0 -6 9 180.74 13.24 0 6 9 180.51 13.04 0 -6 -9 170.91 13.05 0 6 -9 181.55 13.76 0 6 9 196.46 12.98 0 -6 9 220.97 13.40 0 -6 9 212.87 12.95 0 6 9 205.27 13.14 0 -6 9 207.11 13.29 0 6 9 192.74 12.85 0 6 -9 192.49 13.76 0 -6 9 186.02 13.00 0 -6 10 23.18 3.89 0 6 10 20.77 4.27 0 6 10 20.00 4.36 0 -6 10 14.42 3.78 0 6 10 29.78 4.46 0 -6 10 23.01 4.21 0 6 10 21.94 3.90 0 -6 11 64.92 5.57 0 6 11 65.28 5.98 0 -6 11 64.30 5.65 0 -6 12 16.23 2.04 0 6 12 15.79 2.85 0 7 0 0.39 2.00 0 7 0 -0.17 2.48 0 -7 0 0.60 2.36 0 7 1 566.52 30.62 0 7 -1 590.92 30.95 0 7 1 645.81 31.14 0 -7 -1 623.02 30.73 0 -7 1 534.48 30.67 0 -7 2 273.28 14.26 0 -7 2 231.70 12.69 0 -7 -2 267.29 14.16 0 7 2 273.17 14.33 0 7 -2 283.50 14.46 0 -7 -3 148.43 9.38 0 7 3 151.79 8.30 0 -7 3 151.81 8.47 0 7 3 154.98 9.68 0 7 -3 137.70 9.38 0 7 -4 200.33 12.10 0 -7 -4 185.17 11.92 0 -7 4 204.49 11.33 0 7 4 192.98 11.04 0 7 -5 760.05 41.59 0 7 5 791.74 40.86 0 -7 5 798.80 41.12 0 7 -5 795.15 41.83 0 -7 -5 804.90 41.56 0 7 6 15.41 3.62 0 -7 -6 23.94 4.36 0 7 -6 31.37 4.86 0 -7 6 20.96 3.96 0 7 6 14.82 3.43 0 7 6 12.65 3.11 0 -7 6 20.74 4.01 0 7 -6 27.57 4.61 0 -7 6 19.93 3.66 0 7 6 10.88 3.23 0 7 7 16.18 4.17 0 -7 -7 24.34 4.89 0 7 -7 25.82 5.01 0 7 7 23.25 3.68 0 -7 7 22.75 4.03 0 7 7 20.95 3.69 0 -7 7 23.93 3.93 0 -7 7 18.95 4.14 0 7 -7 29.65 4.99 0 -7 7 26.96 4.21 0 7 7 21.22 3.85 0 -7 8 124.06 9.19 0 7 8 94.91 8.58 0 -7 -8 111.50 9.42 0 7 -8 119.11 9.81 0 7 -8 124.10 10.05 0 7 8 95.50 8.38 0 -7 8 124.17 9.11 0 7 8 102.61 8.56 0 -7 8 140.64 9.45 0 7 8 132.60 9.33 0 -7 8 109.51 8.97 0 7 9 23.23 4.51 0 7 9 16.92 4.73 0 -7 -9 18.40 4.59 0 7 -9 20.22 4.57 0 -7 9 20.93 4.44 0 7 9 10.19 3.25 0 -7 9 24.00 4.11 0 7 -9 23.81 5.14 0 -7 9 12.05 4.08 0 7 9 12.11 3.78 0 -7 9 27.35 4.33 0 -7 10 4.53 2.79 0 -7 10 11.53 3.37 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83.47 8.65 0 11 4 103.50 8.38 0 -11 -4 113.16 8.19 0 11 -4 80.84 8.55 0 -11 4 94.51 8.04 0 11 5 434.49 25.59 0 11 -5 434.94 25.46 0 11 5 435.23 25.44 0 11 5 452.69 25.54 0 -11 -5 440.23 25.02 0 11 -5 479.29 26.14 0 -11 5 423.39 25.04 0 11 6 2.01 3.90 0 -11 -6 -0.69 3.88 0 -11 6 0.55 2.55 0 11 6 3.16 2.75 0 11 -6 -0.38 3.69 0 11 -6 -0.41 3.91 0 -11 6 1.38 3.34 0 -11 7 17.61 3.97 0 11 -7 21.63 4.28 0 11 -7 21.37 4.67 0 11 7 14.23 4.78 0 11 7 15.51 3.47 0 -11 -7 18.01 4.30 0 -11 8 24.01 4.27 0 11 8 25.77 3.59 0 -11 8 22.16 4.18 0 11 9 46.71 4.44 0 -11 9 56.27 5.20 0 11 9 48.87 5.56 0 -11 10 29.24 3.30 0 11 10 30.24 3.60 0 11 -11 0.99 1.89 0 -12 0 64.25 6.79 0 -12 0 86.42 6.76 0 12 0 61.16 5.62 0 12 0 82.33 7.94 0 12 0 58.93 6.86 0 12 0 72.44 6.92 0 -12 -1 14.49 3.93 0 -12 1 9.03 4.13 0 12 1 14.17 3.19 0 12 -1 5.34 3.83 0 -12 -1 9.91 3.93 0 -12 1 8.18 4.21 0 12 -1 -3.25 4.37 0 12 -1 5.93 4.23 0 12 1 4.18 3.84 0 12 1 16.22 3.35 0 12 2 248.52 14.63 0 12 -2 243.23 15.05 0 12 2 228.71 14.32 0 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176.36 12.96 0 -15 1 185.57 13.13 0 -15 -1 192.53 13.13 0 15 -1 242.83 14.64 0 -15 1 220.32 13.82 0 -15 -1 211.99 13.40 0 -15 -2 103.50 8.61 0 15 -2 112.72 9.30 0 -15 2 125.18 9.38 0 15 2 117.70 9.43 0 -15 2 95.89 8.64 0 15 -2 88.68 8.51 0 15 -2 109.20 9.23 0 15 3 392.76 21.87 0 -15 3 335.86 20.84 0 15 4 47.22 6.17 0 15 -4 55.36 6.50 0 -15 4 55.42 6.00 0 15 -5 30.30 5.10 0 -15 5 38.45 4.94 0 -15 6 41.13 4.64 0 15 -6 36.84 4.76 0 15 7 6.12 3.21 0 15 -7 14.75 2.98 0 15 8 15.68 2.58 0 -15 8 13.64 2.38 0 16 0 0.40 4.34 0 16 0 -2.33 3.79 0 -16 0 1.52 3.52 0 16 1 16.52 4.01 0 16 -1 21.01 4.77 0 16 -1 23.02 5.09 0 -16 -1 25.28 4.32 0 -16 1 22.49 4.60 0 -16 1 19.14 4.59 0 -16 2 -0.93 3.42 0 16 2 6.83 3.97 0 16 -2 3.96 3.84 0 -16 3 102.61 8.63 0 16 3 133.52 9.46 0 -16 4 46.48 5.27 0 16 4 53.55 5.71 0 16 -4 60.15 6.17 0 -16 5 7.99 2.93 0 16 -5 7.49 3.49 0 -16 5 10.07 2.17 0 16 -6 14.58 3.18 0 16 6 11.57 3.55 0 16 -7 32.53 2.99 0 -16 8 1.38 1.05 0 17 0 -6.06 3.19 0 -17 1 10.34 3.66 0 17 -1 7.74 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3 5 217.56 15.78 10 -3 6 183.08 12.77 -10 -3 -6 157.76 13.11 -10 -3 -6 167.15 12.29 -10 3 -6 173.63 13.08 10 -3 6 150.01 12.27 10 -3 6 184.35 13.70 10 3 6 156.76 13.14 10 -3 6 212.93 14.02 10 3 6 221.72 14.05 -10 3 -6 197.51 13.73 -10 3 -7 58.04 7.56 10 -3 7 53.73 7.07 10 3 7 45.92 6.75 10 -3 7 59.74 7.26 10 3 7 46.40 6.62 10 -3 8 1.74 3.28 10 3 8 -7.25 3.53 10 3 8 0.25 2.89 -10 3 -8 -3.11 4.27 10 -3 8 -2.89 3.50 10 3 8 0.70 3.14 10 -3 9 18.62 3.34 10 3 9 16.38 3.15 10 -3 9 9.33 2.82 10 3 9 17.43 3.05 -10 3 -9 15.70 3.50 10 3 9 15.34 2.91 -10 -4 13 34.46 3.37 -10 -4 12 340.05 19.45 -10 -4 12 339.84 19.20 -10 -4 11 19.94 4.59 -10 4 11 9.83 3.41 -10 4 11 10.60 4.13 -10 -4 11 14.20 3.87 -10 -4 10 57.46 6.39 -10 4 10 59.47 6.03 -10 -4 10 49.00 6.74 -10 -4 10 58.48 7.06 -10 4 10 45.58 6.75 -10 -4 10 46.15 6.69 -10 4 9 405.12 24.14 -10 -4 9 457.10 25.00 -10 4 9 445.61 24.52 -10 -4 9 419.11 25.93 -10 4 9 429.70 25.53 -10 -4 9 448.40 26.01 -10 4 9 437.24 25.86 -10 4 8 348.45 20.02 -10 -4 8 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5.86 -20 -6 5 70.99 5.28 -20 -6 4 3.96 2.76 -20 -6 4 8.22 3.02 -20 -6 4 0.72 2.32 -20 -6 3 41.45 4.14 20 6 -3 53.21 4.74 -20 -6 3 55.12 4.58 -20 -6 3 61.11 5.31 -20 -6 2 43.20 3.98 20 6 -2 60.96 5.37 -20 -6 2 65.11 5.23 -20 -6 2 48.43 4.38 -20 -6 1 162.25 9.99 20 6 -1 164.41 10.63 -20 6 0 82.93 6.17 20 6 0 86.73 6.63 -20 6 -1 -0.62 1.85 20 6 1 0.75 1.88 -20 -7 7 7.70 1.85 -20 -7 6 44.44 4.11 -20 -7 5 103.09 7.22 20 7 -3 5.11 1.90 20 7 -2 1.03 2.34 -20 -7 2 1.34 2.33 20 7 -1 -4.90 2.64 -20 -7 1 1.14 2.04 20 7 0 1.09 2.23 -20 -8 6 11.96 1.96 -20 -8 5 -1.08 1.90 -20 -8 4 -1.88 2.13 20 8 -1 0.35 1.70 -20 -8 1 1.27 1.58 -20 -9 4 2.18 1.48 -20 -9 3 -0.96 1.54 -21 0 8 2.15 1.72 -21 0 7 3.96 2.94 -21 0 7 0.19 2.26 -21 0 6 31.86 4.51 -21 0 6 28.96 4.09 -21 0 5 1.30 3.55 -21 0 5 -1.04 3.04 -21 0 4 8.68 3.83 -21 0 4 7.98 3.45 -21 0 3 1.35 3.50 21 0 -3 -7.30 3.78 -21 0 3 -1.87 3.74 -21 0 3 -4.14 3.38 -21 0 2 14.75 3.97 -21 0 2 12.90 3.54 -21 0 2 13.22 3.92 -21 0 1 -0.45 3.13 -21 0 1 0.24 2.75 -21 0 1 1.78 3.01 -21 0 0 0.35 2.65 21 0 0 -0.67 3.15 -21 0 0 2.27 2.80 -21 0 0 -0.39 2.46 -21 0 -1 -1.87 1.94 -21 0 -1 1.51 1.68 -21 -1 8 5.30 1.76 -21 -1 7 -0.19 2.75 -21 -1 7 2.04 2.37 -21 -1 6 13.41 3.65 -21 -1 6 11.34 3.23 -21 -1 5 21.18 4.26 -21 -1 5 17.04 3.69 -21 -1 4 0.26 3.63 -21 -1 4 2.95 3.17 -21 -1 3 155.41 10.98 21 1 -3 151.95 10.42 -21 -1 3 170.15 11.05 -21 -1 2 3.47 3.50 21 -1 -2 -0.26 2.74 21 1 -2 1.03 2.67 -21 -1 2 0.98 3.30 -21 1 2 4.06 3.39 -21 -1 2 2.31 3.03 21 1 -2 1.47 3.15 -21 -1 1 -0.22 3.03 21 -1 -1 3.59 2.63 21 1 -1 1.48 3.44 -21 -1 1 -2.77 2.80 -21 -1 1 0.84 3.00 -21 1 1 0.23 3.10 -21 -1 0 58.57 5.07 -21 1 0 70.89 5.56 21 1 0 69.13 5.81 -21 -1 0 74.27 5.59 -21 -1 0 57.43 5.18 -21 1 -1 18.74 2.39 21 1 1 16.02 2.74 -21 -1 -1 21.34 2.61 -21 -1 -1 12.42 2.13 -21 2 8 86.79 5.45 -21 -2 7 -1.55 2.56 -21 2 7 2.81 2.60 -21 -2 7 1.33 2.10 -21 2 7 0.51 2.04 -21 2 6 0.65 3.04 -21 -2 6 -0.21 3.01 -21 -2 6 1.88 2.55 -21 2 6 0.64 2.52 -21 -2 5 -0.24 3.30 -21 2 5 3.63 3.40 -21 -2 5 0.24 2.62 -21 2 5 -0.72 2.72 -21 -2 4 21.65 4.23 -21 2 4 17.66 4.08 -21 -2 4 14.05 3.61 -21 2 4 18.38 3.60 -21 2 4 12.06 3.78 21 2 -3 -3.25 3.06 -21 -2 3 -0.76 2.97 -21 2 3 0.51 2.87 -21 -2 3 -2.21 3.41 -21 2 3 0.25 3.30 -21 -2 2 1.62 3.23 -21 2 2 3.07 3.23 21 -2 -2 3.78 2.78 21 2 -2 -1.21 2.48 -21 -2 2 2.15 2.76 -21 2 2 -0.73 2.71 21 2 -2 -2.08 3.36 -21 -2 2 -4.99 3.29 -21 -2 1 8.80 3.16 -21 2 1 9.88 3.34 -21 -2 1 7.03 2.87 -21 2 1 9.34 2.95 21 2 -1 4.45 3.29 -21 2 1 7.23 3.22 -21 -2 1 9.54 3.11 -21 -2 0 6.42 2.66 -21 2 0 6.12 2.66 -21 -2 0 4.11 2.24 -21 2 0 4.20 2.29 21 2 0 3.90 3.00 -21 2 0 7.12 2.83 -21 2 -1 9.50 1.99 -21 2 -1 8.54 1.71 21 2 1 11.75 2.24 -21 2 -1 9.53 1.95 -21 -3 7 14.43 2.27 -21 -3 7 15.51 2.46 -21 -3 6 3.31 2.70 -21 3 6 5.08 2.86 -21 -3 6 3.91 2.42 -21 3 6 1.84 2.31 -21 -3 5 7.11 3.27 -21 3 5 11.39 3.47 -21 -3 5 5.17 2.74 -21 3 5 6.17 2.72 -21 -3 4 285.20 17.31 -21 3 4 289.25 17.36 -21 -3 4 331.24 17.71 -21 3 4 335.25 17.73 -21 3 4 311.06 17.63 -21 -3 3 -0.44 3.19 -21 3 3 0.90 3.16 -21 -3 3 5.12 2.72 -21 3 3 6.86 2.70 21 3 -3 -0.33 2.37 -21 3 3 0.47 3.28 -21 -3 2 31.30 4.21 -21 3 2 33.16 4.30 21 3 -2 30.64 4.06 -21 -3 2 25.60 3.76 -21 3 2 28.49 3.88 -21 3 1 129.23 8.39 21 3 -1 129.79 8.67 -21 -3 1 117.05 8.09 -21 3 1 111.04 8.10 -21 -3 0 32.03 3.14 -21 -3 0 19.22 2.67 21 3 0 23.64 3.34 -21 3 0 24.26 3.24 -21 -4 7 -0.39 1.59 -21 -4 6 18.12 2.88 -21 -4 6 15.72 2.41 -21 -4 6 19.82 2.90 -21 -4 5 1.50 2.78 -21 -4 5 2.27 2.14 -21 -4 5 7.87 2.64 -21 -4 4 3.77 3.30 -21 -4 4 4.99 2.52 -21 -4 3 252.87 12.71 -21 -4 3 221.05 12.36 -21 4 3 236.46 12.82 -21 -4 2 31.40 3.67 -21 -4 2 26.22 3.32 21 4 -2 28.08 3.67 -21 4 2 29.55 4.12 -21 -4 1 2.87 2.19 -21 -4 1 0.53 1.80 21 4 -1 0.19 2.53 -21 4 1 -1.08 2.56 21 4 0 73.11 5.36 -21 -5 7 3.75 1.40 -21 -5 6 8.77 2.07 -21 -5 5 127.08 8.04 -21 -5 4 1.37 2.10 -21 -5 3 54.35 4.02 21 5 -2 180.22 10.45 21 5 -1 47.65 3.99 -21 5 1 44.06 3.96 -21 -6 5 1.55 1.72 -21 -6 4 61.01 4.66 -21 -6 3 62.47 4.62 -21 -7 4 9.77 1.80 -21 -7 3 7.62 1.63 -22 0 6 6.40 2.14 -22 0 6 10.89 1.98 -22 0 5 3.11 2.48 -22 0 5 0.96 1.93 -22 0 4 2.09 2.49 -22 0 4 -0.69 2.01 -22 0 3 -1.19 2.44 -22 0 3 -3.24 2.22 -22 0 2 96.69 6.50 -22 0 2 95.66 6.41 -22 0 1 -1.80 1.83 -22 0 1 0.48 1.38 -22 -1 6 7.43 2.12 -22 -1 6 6.40 1.77 -22 -1 5 0.16 2.35 -22 -1 5 2.43 1.94 -22 -1 4 13.17 2.95 -22 -1 4 15.85 2.67 -22 -1 3 10.94 2.75 -22 -1 3 4.74 2.14 -22 -1 2 44.01 3.88 -22 -1 2 39.33 3.59 -22 1 2 37.10 3.78 -22 -1 1 -0.66 1.60 -22 -1 1 -0.99 1.31 -22 1 1 1.57 1.64 -22 2 6 27.71 2.74 -22 2 6 27.37 2.54 -22 -2 5 117.85 7.25 -22 2 5 116.79 7.29 -22 -2 5 117.53 7.09 -22 2 5 107.16 7.05 -22 -2 4 -2.94 2.68 -22 2 4 -3.51 2.57 -22 -2 4 -1.01 2.01 -22 2 4 -1.64 2.01 -22 -2 3 53.93 4.37 -22 2 3 44.74 4.24 -22 -2 3 49.29 4.02 -22 2 3 47.26 4.06 -22 -2 2 -0.12 2.06 -22 2 2 -3.40 2.17 -22 -2 2 2.73 1.66 -22 2 2 0.52 1.58 -22 -3 4 40.13 3.46 -22 -3 4 39.51 3.24 -22 3 2 25.36 2.70 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 31524 _shelx_res_file ; TITL wm5672 in P2(1)/c shelx.res created by SHELXL-2018/3 at 15:12:07 on 20-Feb-2023 CELL 1.54184 17.6747 15.7656 10.9086 90.000 105.666 90.000 ZERR 4.00 0.0003 0.0002 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 140 136 24 12 MERG 2 OMIT -2 5 1 OMIT -3 8 1 OMIT -1 8 9 OMIT -12 2 8 OMIT -1 8 1 OMIT 4 0 8 OMIT -2 1 1 OMIT -4 12 10 OMIT 4 2 7 OMIT -5 12 8 OMIT 1 1 7 OMIT -3 6 8 OMIT -6 3 9 OMIT -1 9 9 OMIT 12 11 1 OMIT -2 9 9 OMIT -1 9 7 OMIT -5 3 9 OMIT -5 14 7 OMIT 3 6 1 OMIT 0 1 7 OMIT -12 2 7 OMIT 1 11 8 FMAP 2 PLAN 5 SIZE 0.080 0.110 0.140 ACTA BOND $H CONF L.S. 13 TEMP -173.00 WGHT 0.074500 3.347700 FVAR 0.58873 C1 1 0.846879 0.495234 0.846062 11.00000 0.02371 0.01509 = 0.01918 -0.00029 0.00637 -0.00167 C2 1 0.900390 0.467143 0.765670 11.00000 0.02344 0.01720 = 0.01897 0.00014 0.00632 0.00053 C4 1 0.816292 0.338848 0.708345 11.00000 0.02346 0.01706 = 0.02182 0.00067 0.00690 0.00079 C5 1 0.774853 0.359579 0.810000 11.00000 0.02395 0.01463 = 0.02088 -0.00123 0.00800 -0.00155 AFIX 13 H5 2 0.766607 0.305061 0.851447 11.00000 -1.20000 AFIX 0 C6 1 0.692404 0.397817 0.745902 11.00000 0.02451 0.01622 = 0.01981 -0.00167 0.00517 0.00015 AFIX 13 H6 2 0.682604 0.393814 0.651413 11.00000 -1.20000 AFIX 0 C7 1 0.697687 0.495046 0.784962 11.00000 0.02189 0.01678 = 0.02099 -0.00002 0.00521 0.00029 C8 1 0.770280 0.536231 0.753581 11.00000 0.02477 0.01776 = 0.01658 -0.00028 0.00640 -0.00043 AFIX 13 H8 2 0.769058 0.518255 0.665155 11.00000 -1.20000 AFIX 0 C9 1 0.822233 0.418527 0.914337 11.00000 0.02310 0.01722 = 0.02068 -0.00101 0.00858 0.00003 C10 1 0.706805 0.495261 0.926407 11.00000 0.02395 0.01482 = 0.02351 -0.00023 0.00658 -0.00178 C11 1 0.889647 0.556270 0.942552 11.00000 0.02420 0.01636 = 0.02089 -0.00003 0.00799 0.00075 C12 1 0.913674 0.371534 0.595683 11.00000 0.02727 0.01759 = 0.02097 -0.00307 0.00918 -0.00342 C13 1 0.877747 0.398974 0.472887 11.00000 0.02843 0.02439 = 0.02597 -0.00003 0.00806 0.00211 AFIX 43 H13 2 0.829930 0.429983 0.455287 11.00000 -1.20000 AFIX 0 C14 1 0.912457 0.380603 0.376127 11.00000 0.03837 0.03136 = 0.02327 0.00153 0.01100 -0.00033 AFIX 43 H14 2 0.888170 0.398723 0.291590 11.00000 -1.20000 AFIX 0 C15 1 0.982549 0.335835 0.402578 11.00000 0.03635 0.02556 = 0.02819 -0.00690 0.01790 -0.00505 AFIX 43 H15 2 1.006297 0.323451 0.336214 11.00000 -1.20000 AFIX 0 C16 1 1.018120 0.309038 0.526304 11.00000 0.02776 0.02134 = 0.03464 -0.00393 0.01264 -0.00101 AFIX 43 H16 2 1.066067 0.278253 0.544171 11.00000 -1.20000 AFIX 0 C17 1 0.983797 0.327133 0.623597 11.00000 0.02823 0.01844 = 0.02621 -0.00093 0.00820 -0.00067 AFIX 43 H17 2 1.008099 0.309285 0.708266 11.00000 -1.20000 AFIX 0 C18 1 0.624854 0.355391 0.783221 11.00000 0.02422 0.01512 = 0.02368 -0.00373 0.00781 -0.00007 C19 1 0.634653 0.314427 0.900490 11.00000 0.02435 0.01962 = 0.02241 -0.00123 0.00457 -0.00047 AFIX 43 H19 2 0.685990 0.306811 0.955333 11.00000 -1.20000 AFIX 0 C20 1 0.570095 0.284843 0.937383 11.00000 0.03029 0.02120 = 0.02155 -0.00128 0.00829 -0.00294 AFIX 43 H20 2 0.578280 0.256282 1.016577 11.00000 -1.20000 AFIX 0 C21 1 0.493702 0.295985 0.861247 11.00000 0.02821 0.01912 = 0.02853 -0.00488 0.01002 -0.00303 C22 1 0.484558 0.332045 0.741236 11.00000 0.02377 0.02156 = 0.02741 -0.00259 0.00351 -0.00059 AFIX 43 H22 2 0.433380 0.336973 0.684802 11.00000 -1.20000 AFIX 0 C23 1 0.548923 0.360934 0.702576 11.00000 0.02984 0.01784 = 0.02134 -0.00033 0.00619 -0.00092 AFIX 43 H23 2 0.541005 0.384761 0.620081 11.00000 -1.20000 AFIX 0 C24 1 0.424320 0.273187 0.909647 11.00000 0.02743 0.02758 = 0.03276 -0.00256 0.01026 -0.00316 AFIX 137 H24A 2 0.408264 0.322797 0.950610 11.00000 -1.50000 H24B 2 0.438846 0.226951 0.971608 11.00000 -1.50000 H24C 2 0.380636 0.254957 0.838265 11.00000 -1.50000 AFIX 0 C25 1 0.625641 0.538263 0.711746 11.00000 0.02648 0.01884 = 0.02539 -0.00209 0.00932 -0.00180 C26 1 0.773310 0.632706 0.755727 11.00000 0.02411 0.01808 = 0.02034 0.00179 0.00366 0.00022 C27 1 0.746162 0.682679 0.840809 11.00000 0.02868 0.01837 = 0.02284 0.00117 0.00877 0.00014 AFIX 43 H27 2 0.721083 0.656657 0.897947 11.00000 -1.20000 AFIX 0 C28 1 0.755613 0.770049 0.842330 11.00000 0.03071 0.01940 = 0.02229 -0.00160 0.00595 0.00196 AFIX 43 H28 2 0.736015 0.802987 0.899962 11.00000 -1.20000 AFIX 0 C29 1 0.793074 0.810811 0.761614 11.00000 0.02824 0.01893 = 0.02237 0.00186 0.00175 -0.00043 C30 1 0.819454 0.760765 0.676557 11.00000 0.03238 0.01988 = 0.02299 0.00336 0.00727 -0.00282 AFIX 43 H30 2 0.844772 0.786878 0.619812 11.00000 -1.20000 AFIX 0 C31 1 0.809460 0.673177 0.673013 11.00000 0.02996 0.02100 = 0.02133 0.00027 0.00838 0.00044 AFIX 43 H31 2 0.827533 0.640525 0.613376 11.00000 -1.20000 AFIX 0 C32 1 0.805746 0.905350 0.768855 11.00000 0.03916 0.01849 = 0.03165 0.00206 0.00762 -0.00090 AFIX 137 H32A 2 0.852432 0.918575 0.838280 11.00000 -1.50000 H32B 2 0.759739 0.933163 0.784828 11.00000 -1.50000 H32C 2 0.813314 0.925827 0.688169 11.00000 -1.50000 AFIX 0 C33 1 0.890038 0.374039 1.006325 11.00000 0.02590 0.01735 = 0.02201 0.00136 0.00598 -0.00057 AFIX 137 H33A 2 0.919202 0.414849 1.069304 11.00000 -1.50000 H33B 2 0.925089 0.349923 0.959485 11.00000 -1.50000 H33C 2 0.869776 0.328506 1.049816 11.00000 -1.50000 AFIX 0 C34 1 0.635791 0.471726 0.376972 11.00000 0.03140 0.02792 = 0.02427 -0.00099 0.00943 0.00103 AFIX 43 H34 2 0.593630 0.505419 0.388302 11.00000 -1.20000 AFIX 0 C35 1 0.683569 0.370627 0.248870 11.00000 0.03757 0.02537 = 0.02768 -0.00092 0.00999 0.00273 AFIX 137 H35A 2 0.709455 0.394672 0.187861 11.00000 -1.50000 H35B 2 0.658547 0.316752 0.215915 11.00000 -1.50000 H35C 2 0.722664 0.360780 0.330382 11.00000 -1.50000 AFIX 0 C36 1 0.549321 0.432539 0.170188 11.00000 0.02953 0.04340 = 0.02765 -0.00462 0.00633 0.00007 AFIX 137 H36A 2 0.521478 0.378714 0.169526 11.00000 -1.50000 H36B 2 0.558662 0.441861 0.086657 11.00000 -1.50000 H36C 2 0.517414 0.479056 0.188991 11.00000 -1.50000 AFIX 0 N2 3 0.957801 0.513081 0.759945 11.00000 0.02803 0.02214 = 0.02446 -0.00207 0.01051 -0.00271 H2N 2 0.983986 0.492325 0.701727 11.00000 -1.20000 N3 3 0.876584 0.391559 0.695470 11.00000 0.02553 0.01631 = 0.02174 -0.00273 0.00976 -0.00203 N10 3 0.659997 0.529022 0.980865 11.00000 0.03113 0.02156 = 0.02595 0.00015 0.01314 -0.00013 H10N 2 0.675126 0.520550 1.070519 11.00000 -1.20000 N11 3 0.920835 0.601552 1.022871 11.00000 0.02834 0.02118 = 0.02549 -0.00102 0.00733 -0.00040 N25 3 0.570377 0.568060 0.646542 11.00000 0.02908 0.02443 = 0.03455 0.00296 0.00610 0.00112 N34 3 0.624230 0.429547 0.267362 11.00000 0.02883 0.02626 = 0.02406 -0.00182 0.00640 0.00101 O4 4 0.796214 0.277590 0.639515 11.00000 0.03219 0.02047 = 0.03070 -0.00730 0.01259 -0.00344 O9 4 0.772256 0.450541 0.990819 11.00000 0.02408 0.01870 = 0.01914 0.00030 0.00810 0.00136 O34 4 0.696534 0.470514 0.464404 11.00000 0.03576 0.03652 = 0.02527 -0.00421 0.00492 0.00324 HKLF 4 REM wm5672 in P2(1)/c REM wR2 = 0.1656, GooF = S = 1.078, Restrained GooF = 1.078 for all data REM R1 = 0.0587 for 5275 Fo > 4sig(Fo) and 0.0666 for all 6140 data REM 408 parameters refined using 0 restraints END WGHT 0.0745 3.3477 REM Highest difference peak 0.339, deepest hole -0.364, 1-sigma level 0.067 Q1 1 0.7009 0.4958 0.8485 11.00000 0.05 0.34 Q2 1 0.7367 0.5076 0.7792 11.00000 0.05 0.30 Q3 1 0.7936 0.3522 0.7555 11.00000 0.05 0.28 Q4 1 0.6700 0.5207 0.7592 11.00000 0.05 0.28 Q5 1 0.6022 0.5388 0.9399 11.00000 0.05 0.27 ; _shelx_res_checksum 91053 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.84688(12) 0.49523(12) 0.84606(19) 0.0192(4) Uani d 1 . . C C2 0.90039(12) 0.46714(13) 0.76567(19) 0.0198(4) Uani d 1 . . C C4 0.81629(12) 0.33885(13) 0.70834(19) 0.0206(4) Uani d 1 . . C C5 0.77485(12) 0.35958(13) 0.81000(19) 0.0194(4) Uani d 1 . . H H5 0.766607 0.305061 0.851447 0.023 Uiso calc 1 . . C C6 0.69240(12) 0.39782(13) 0.74590(19) 0.0203(4) Uani d 1 . . H H6 0.682604 0.393814 0.651413 0.024 Uiso calc 1 . . C C7 0.69769(12) 0.49505(13) 0.78496(19) 0.0200(4) Uani d 1 . . C C8 0.77028(12) 0.53623(13) 0.75358(19) 0.0195(4) Uani d 1 . . H H8 0.769058 0.518255 0.665155 0.023 Uiso calc 1 . . C C9 0.82223(12) 0.41853(13) 0.91434(19) 0.0198(4) Uani d 1 . . C C10 0.70680(12) 0.49526(13) 0.9264(2) 0.0207(4) Uani d 1 . . C C11 0.88965(12) 0.55627(13) 0.94255(19) 0.0201(4) Uani d 1 . . C C12 0.91367(12) 0.37153(13) 0.5957(2) 0.0214(4) Uani d 1 . . C C13 0.87775(13) 0.39897(14) 0.4729(2) 0.0261(5) Uani d 1 . . H H13 0.829930 0.429983 0.455287 0.031 Uiso calc 1 . . C C14 0.91246(15) 0.38060(16) 0.3761(2) 0.0305(5) Uani d 1 . . H H14 0.888170 0.398723 0.291590 0.037 Uiso calc 1 . . C C15 0.98255(14) 0.33583(15) 0.4026(2) 0.0283(5) Uani d 1 . . H H15 1.006297 0.323451 0.336214 0.034 Uiso calc 1 . . C C16 1.01812(13) 0.30904(14) 0.5263(2) 0.0271(5) Uani d 1 . . H H16 1.066067 0.278253 0.544171 0.033 Uiso calc 1 . . C C17 0.98380(13) 0.32713(13) 0.6236(2) 0.0241(4) Uani d 1 . . H H17 1.008099 0.309285 0.708266 0.029 Uiso calc 1 . . C C18 0.62485(12) 0.35539(13) 0.7832(2) 0.0208(4) Uani d 1 . . C C19 0.63465(13) 0.31443(13) 0.9005(2) 0.0225(4) Uani d 1 . . H H19 0.685990 0.306811 0.955333 0.027 Uiso calc 1 . . C C20 0.57009(13) 0.28484(14) 0.9374(2) 0.0241(4) Uani d 1 . . H H20 0.578280 0.256282 1.016577 0.029 Uiso calc 1 . . C C21 0.49370(13) 0.29599(14) 0.8612(2) 0.0248(5) Uani d 1 . . C C22 0.48456(13) 0.33204(14) 0.7412(2) 0.0249(5) Uani d 1 . . H H22 0.433380 0.336973 0.684802 0.030 Uiso calc 1 . . C C23 0.54892(13) 0.36093(13) 0.7026(2) 0.0231(4) Uani d 1 . . H H23 0.541005 0.384761 0.620081 0.028 Uiso calc 1 . . C C24 0.42432(13) 0.27319(15) 0.9096(2) 0.0288(5) Uani d 1 . . H H24A 0.408264 0.322797 0.950610 0.043 Uiso calc 1 . . H H24B 0.438846 0.226951 0.971608 0.043 Uiso calc 1 . . H H24C 0.380636 0.254957 0.838265 0.043 Uiso calc 1 . . C C25 0.62564(13) 0.53826(13) 0.7117(2) 0.0231(4) Uani d 1 . . C C26 0.77331(12) 0.63271(13) 0.75573(19) 0.0213(4) Uani d 1 . . C C27 0.74616(13) 0.68268(13) 0.8408(2) 0.0229(4) Uani d 1 . . H H27 0.721083 0.656657 0.897947 0.028 Uiso calc 1 . . C C28 0.75561(13) 0.77005(14) 0.8423(2) 0.0244(4) Uani d 1 . . H H28 0.736015 0.802987 0.899962 0.029 Uiso calc 1 . . C C29 0.79307(13) 0.81081(14) 0.7616(2) 0.0242(4) Uani d 1 . . C C30 0.81945(13) 0.76077(14) 0.6766(2) 0.0251(5) Uani d 1 . . H H30 0.844772 0.786878 0.619812 0.030 Uiso calc 1 . . C C31 0.80946(13) 0.67318(14) 0.6730(2) 0.0238(4) Uani d 1 . . H H31 0.827533 0.640525 0.613376 0.029 Uiso calc 1 . . C C32 0.80575(15) 0.90535(14) 0.7689(2) 0.0301(5) Uani d 1 . . H H32A 0.852432 0.918575 0.838280 0.045 Uiso calc 1 . . H H32B 0.759739 0.933163 0.784828 0.045 Uiso calc 1 . . H H32C 0.813314 0.925827 0.688169 0.045 Uiso calc 1 . . C C33 0.89004(12) 0.37404(13) 1.0063(2) 0.0218(4) Uani d 1 . . H H33A 0.919202 0.414849 1.069304 0.033 Uiso calc 1 . . H H33B 0.925089 0.349923 0.959485 0.033 Uiso calc 1 . . H H33C 0.869776 0.328506 1.049816 0.033 Uiso calc 1 . . C C34 0.63579(14) 0.47173(15) 0.3770(2) 0.0275(5) Uani d 1 . . H H34 0.593630 0.505419 0.388302 0.033 Uiso calc 1 . . C C35 0.68357(15) 0.37063(15) 0.2489(2) 0.0300(5) Uani d 1 . . H H35A 0.709455 0.394672 0.187861 0.045 Uiso calc 1 . . H H35B 0.658547 0.316752 0.215915 0.045 Uiso calc 1 . . H H35C 0.722664 0.360780 0.330382 0.045 Uiso calc 1 . . C C36 0.54932(14) 0.43254(18) 0.1702(2) 0.0338(5) Uani d 1 . . H H36A 0.521478 0.378714 0.169526 0.051 Uiso calc 1 . . H H36B 0.558662 0.441861 0.086657 0.051 Uiso calc 1 . . H H36C 0.517414 0.479056 0.188991 0.051 Uiso calc 1 . . N N2 0.95780(11) 0.51308(12) 0.75995(18) 0.0242(4) Uani d 1 . . H H2N 0.9840(16) 0.4923(18) 0.702(3) 0.029 Uiso d 1 . . N N3 0.87658(10) 0.39156(11) 0.69547(16) 0.0205(4) Uani d 1 . . N N10 0.66000(11) 0.52902(12) 0.98087(19) 0.0252(4) Uani d 1 . . H H10N 0.6751(16) 0.5206(18) 1.071(3) 0.030 Uiso d 1 . . N N11 0.92084(11) 0.60155(12) 1.02287(17) 0.0250(4) Uani d 1 . . N N25 0.57038(11) 0.56806(13) 0.64654(19) 0.0298(4) Uani d 1 . . N N34 0.62423(11) 0.42955(12) 0.26736(18) 0.0265(4) Uani d 1 . . O O4 0.79621(9) 0.27759(10) 0.63952(15) 0.0270(4) Uani d 1 . . O O9 0.77226(8) 0.45054(9) 0.99082(13) 0.0202(3) Uani d 1 . . O O34 0.69653(10) 0.47051(11) 0.46440(15) 0.0332(4) Uani 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 0.0237(10) 0.0151(9) 0.0192(9) -0.0017(7) 0.0064(8) -0.0003(7) C2 0.0234(10) 0.0172(9) 0.0190(9) 0.0005(8) 0.0063(8) 0.0001(8) C4 0.0235(10) 0.0171(9) 0.0218(10) 0.0008(8) 0.0069(8) 0.0007(8) C5 0.0240(10) 0.0146(9) 0.0209(10) -0.0016(7) 0.0080(8) -0.0012(7) C6 0.0245(10) 0.0162(9) 0.0198(10) 0.0002(8) 0.0052(8) -0.0017(7) C7 0.0219(10) 0.0168(9) 0.0210(10) 0.0003(8) 0.0052(8) 0.0000(8) C8 0.0248(10) 0.0178(9) 0.0166(9) -0.0004(8) 0.0064(8) -0.0003(7) C9 0.0231(10) 0.0172(9) 0.0207(10) 0.0000(8) 0.0086(8) -0.0010(8) C10 0.0239(10) 0.0148(9) 0.0235(10) -0.0018(7) 0.0066(8) -0.0002(8) C11 0.0242(10) 0.0164(9) 0.0209(10) 0.0007(8) 0.0080(8) 0.0000(8) C12 0.0273(10) 0.0176(9) 0.0210(10) -0.0034(8) 0.0092(8) -0.0031(8) C13 0.0284(11) 0.0244(11) 0.0260(11) 0.0021(9) 0.0081(9) 0.0000(9) C14 0.0384(13) 0.0314(12) 0.0233(11) -0.0003(10) 0.0110(9) 0.0015(9) C15 0.0363(12) 0.0256(11) 0.0282(11) -0.0051(9) 0.0179(9) -0.0069(9) C16 0.0278(11) 0.0213(10) 0.0346(12) -0.0010(9) 0.0126(9) -0.0039(9) C17 0.0282(11) 0.0184(10) 0.0262(11) -0.0007(8) 0.0082(8) -0.0009(8) C18 0.0242(10) 0.0151(9) 0.0237(10) -0.0001(8) 0.0078(8) -0.0037(8) C19 0.0243(10) 0.0196(10) 0.0224(10) -0.0005(8) 0.0046(8) -0.0012(8) C20 0.0303(11) 0.0212(10) 0.0216(10) -0.0029(8) 0.0083(9) -0.0013(8) C21 0.0282(11) 0.0191(10) 0.0285(11) -0.0030(8) 0.0100(9) -0.0049(8) C22 0.0238(10) 0.0216(10) 0.0274(11) -0.0006(8) 0.0035(8) -0.0026(8) C23 0.0298(11) 0.0178(10) 0.0213(10) -0.0009(8) 0.0062(8) -0.0003(8) C24 0.0274(11) 0.0276(12) 0.0328(12) -0.0032(9) 0.0103(9) -0.0026(9) C25 0.0265(11) 0.0188(10) 0.0254(11) -0.0018(8) 0.0093(9) -0.0021(8) C26 0.0241(10) 0.0181(10) 0.0203(10) 0.0002(8) 0.0037(8) 0.0018(8) C27 0.0287(11) 0.0184(10) 0.0228(10) 0.0001(8) 0.0088(8) 0.0012(8) C28 0.0307(11) 0.0194(10) 0.0223(10) 0.0020(8) 0.0059(9) -0.0016(8) C29 0.0282(11) 0.0189(10) 0.0224(10) -0.0004(8) 0.0018(8) 0.0019(8) C30 0.0324(11) 0.0199(10) 0.0230(10) -0.0028(9) 0.0073(9) 0.0034(8) C31 0.0300(11) 0.0210(10) 0.0213(10) 0.0004(8) 0.0084(8) 0.0003(8) C32 0.0392(13) 0.0185(10) 0.0317(12) -0.0009(9) 0.0076(10) 0.0021(9) C33 0.0259(10) 0.0173(9) 0.0220(10) -0.0006(8) 0.0060(8) 0.0014(8) C34 0.0314(11) 0.0279(11) 0.0243(11) 0.0010(9) 0.0094(9) -0.0010(9) C35 0.0376(13) 0.0254(11) 0.0277(11) 0.0027(9) 0.0100(10) -0.0009(9) C36 0.0295(12) 0.0434(14) 0.0277(12) 0.0001(10) 0.0063(9) -0.0046(10) N2 0.0280(9) 0.0221(9) 0.0245(9) -0.0027(7) 0.0105(8) -0.0021(7) N3 0.0255(9) 0.0163(8) 0.0217(8) -0.0020(7) 0.0098(7) -0.0027(7) N10 0.0311(10) 0.0216(9) 0.0260(10) -0.0001(7) 0.0131(8) 0.0001(7) N11 0.0283(9) 0.0212(9) 0.0255(9) -0.0004(7) 0.0073(7) -0.0010(7) N25 0.0291(10) 0.0244(10) 0.0346(11) 0.0011(8) 0.0061(8) 0.0030(8) N34 0.0288(10) 0.0263(10) 0.0241(9) 0.0010(8) 0.0064(8) -0.0018(7) O4 0.0322(8) 0.0205(7) 0.0307(8) -0.0034(6) 0.0126(7) -0.0073(6) O9 0.0241(7) 0.0187(7) 0.0191(7) 0.0014(5) 0.0081(6) 0.0003(5) O34 0.0358(9) 0.0365(9) 0.0253(8) 0.0032(7) 0.0049(7) -0.0042(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' N N 0.0311 0.0180 '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 C11 C1 C2 . . 108.85(17) ? C11 C1 C9 . . 108.90(17) ? C2 C1 C9 . . 110.55(16) ? C11 C1 C8 . . 111.83(16) ? C2 C1 C8 . . 107.95(16) ? C9 C1 C8 . . 108.76(16) ? N2 C2 N3 . . 125.53(19) ? N2 C2 C1 . . 119.71(19) ? N3 C2 C1 . . 114.63(17) ? O4 C4 N3 . . 121.14(19) ? O4 C4 C5 . . 120.22(18) ? N3 C4 C5 . . 118.64(17) ? C4 C5 C9 . . 113.46(17) ? C4 C5 C6 . . 109.41(16) ? C9 C5 C6 . . 110.87(16) ? C4 C5 H5 . . 107.6 ? C9 C5 H5 . . 107.6 ? C6 C5 H5 . . 107.6 ? C18 C6 C5 . . 114.69(17) ? C18 C6 C7 . . 110.33(16) ? C5 C6 C7 . . 105.86(16) ? C18 C6 H6 . . 108.6 ? C5 C6 H6 . . 108.6 ? C7 C6 H6 . . 108.6 ? C25 C7 C10 . . 113.04(18) ? C25 C7 C8 . . 109.31(17) ? C10 C7 C8 . . 110.95(17) ? C25 C7 C6 . . 108.74(16) ? C10 C7 C6 . . 105.03(16) ? C8 C7 C6 . . 109.64(16) ? C26 C8 C7 . . 116.18(17) ? C26 C8 C1 . . 112.08(16) ? C7 C8 C1 . . 107.58(16) ? C26 C8 H8 . . 106.8 ? C7 C8 H8 . . 106.8 ? C1 C8 H8 . . 106.8 ? O9 C9 C33 . . 105.95(16) ? O9 C9 C5 . . 109.93(16) ? C33 C9 C5 . . 112.84(17) ? O9 C9 C1 . . 107.35(16) ? C33 C9 C1 . . 114.04(17) ? C5 C9 C1 . . 106.61(16) ? N10 C10 O9 . . 123.02(19) ? N10 C10 C7 . . 125.6(2) ? O9 C10 C7 . . 111.38(17) ? N11 C11 C1 . . 175.8(2) ? C17 C12 C13 . . 121.3(2) ? C17 C12 N3 . . 120.32(19) ? C13 C12 N3 . . 118.38(19) ? C14 C13 C12 . . 119.2(2) ? C14 C13 H13 . . 120.4 ? C12 C13 H13 . . 120.4 ? C15 C14 C13 . . 120.1(2) ? C15 C14 H14 . . 119.9 ? C13 C14 H14 . . 119.9 ? C14 C15 C16 . . 120.0(2) ? C14 C15 H15 . . 120.0 ? C16 C15 H15 . . 120.0 ? C17 C16 C15 . . 120.2(2) ? C17 C16 H16 . . 119.9 ? C15 C16 H16 . . 119.9 ? C12 C17 C16 . . 119.1(2) ? C12 C17 H17 . . 120.4 ? C16 C17 H17 . . 120.4 ? C23 C18 C19 . . 117.73(19) ? C23 C18 C6 . . 119.75(19) ? C19 C18 C6 . . 122.41(18) ? C20 C19 C18 . . 120.7(2) ? C20 C19 H19 . . 119.7 ? C18 C19 H19 . . 119.7 ? C19 C20 C21 . . 121.7(2) ? C19 C20 H20 . . 119.2 ? C21 C20 H20 . . 119.2 ? C20 C21 C22 . . 117.3(2) ? C20 C21 C24 . . 120.8(2) ? C22 C21 C24 . . 121.8(2) ? C23 C22 C21 . . 121.3(2) ? C23 C22 H22 . . 119.3 ? C21 C22 H22 . . 119.3 ? C22 C23 C18 . . 120.9(2) ? C22 C23 H23 . . 119.5 ? C18 C23 H23 . . 119.5 ? C21 C24 H24A . . 109.5 ? C21 C24 H24B . . 109.5 ? H24A C24 H24B . . 109.5 ? C21 C24 H24C . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? N25 C25 C7 . . 174.4(2) ? C31 C26 C27 . . 118.15(19) ? C31 C26 C8 . . 117.91(19) ? C27 C26 C8 . . 123.83(19) ? C28 C27 C26 . . 120.4(2) ? C28 C27 H27 . . 119.8 ? C26 C27 H27 . . 119.8 ? C27 C28 C29 . . 121.8(2) ? C27 C28 H28 . . 119.1 ? C29 C28 H28 . . 119.1 ? C30 C29 C28 . . 117.5(2) ? C30 C29 C32 . . 121.6(2) ? C28 C29 C32 . . 120.8(2) ? C29 C30 C31 . . 121.2(2) ? C29 C30 H30 . . 119.4 ? C31 C30 H30 . . 119.4 ? C30 C31 C26 . . 120.9(2) ? C30 C31 H31 . . 119.6 ? C26 C31 H31 . . 119.6 ? C29 C32 H32A . . 109.5 ? C29 C32 H32B . . 109.5 ? H32A C32 H32B . . 109.5 ? C29 C32 H32C . . 109.5 ? H32A C32 H32C . . 109.5 ? H32B C32 H32C . . 109.5 ? C9 C33 H33A . . 109.5 ? C9 C33 H33B . . 109.5 ? H33A C33 H33B . . 109.5 ? C9 C33 H33C . . 109.5 ? H33A C33 H33C . . 109.5 ? H33B C33 H33C . . 109.5 ? O34 C34 N34 . . 125.3(2) ? O34 C34 H34 . . 117.3 ? N34 C34 H34 . . 117.3 ? N34 C35 H35A . . 109.5 ? N34 C35 H35B . . 109.5 ? H35A C35 H35B . . 109.5 ? N34 C35 H35C . . 109.5 ? H35A C35 H35C . . 109.5 ? H35B C35 H35C . . 109.5 ? N34 C36 H36A . . 109.5 ? N34 C36 H36B . . 109.5 ? H36A C36 H36B . . 109.5 ? N34 C36 H36C . . 109.5 ? H36A C36 H36C . . 109.5 ? H36B C36 H36C . . 109.5 ? C2 N2 H2N . . 112.5(17) ? C4 N3 C2 . . 124.93(17) ? C4 N3 C12 . . 117.45(17) ? C2 N3 C12 . . 117.42(17) ? C10 N10 H10N . . 112.8(17) ? C34 N34 C35 . . 120.03(19) ? C34 N34 C36 . . 121.7(2) ? C35 N34 C36 . . 117.86(19) ? C10 O9 C9 . . 116.16(15) ? 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 C1 C11 . 1.475(3) ? C1 C2 . 1.519(3) ? C1 C9 . 1.543(3) ? C1 C8 . 1.591(3) ? C2 N2 . 1.262(3) ? C2 N3 . 1.418(3) ? C4 O4 . 1.216(3) ? C4 N3 . 1.388(3) ? C4 C5 . 1.520(3) ? C5 C9 . 1.532(3) ? C5 C6 . 1.557(3) ? C5 H5 . 1.0000 ? C6 C18 . 1.517(3) ? C6 C7 . 1.587(3) ? C6 H6 . 1.0000 ? C7 C25 . 1.475(3) ? C7 C10 . 1.507(3) ? C7 C8 . 1.556(3) ? C8 C26 . 1.522(3) ? C8 H8 . 1.0000 ? C9 O9 . 1.459(2) ? C9 C33 . 1.512(3) ? C10 N10 . 1.259(3) ? C10 O9 . 1.375(2) ? C11 N11 . 1.149(3) ? C12 C17 . 1.384(3) ? C12 C13 . 1.388(3) ? C12 N3 . 1.449(3) ? C13 C14 . 1.387(3) ? C13 H13 . 0.9500 ? C14 C15 . 1.387(3) ? C14 H14 . 0.9500 ? C15 C16 . 1.392(3) ? C15 H15 . 0.9500 ? C16 C17 . 1.387(3) ? C16 H16 . 0.9500 ? C17 H17 . 0.9500 ? C18 C23 . 1.395(3) ? C18 C19 . 1.401(3) ? C19 C20 . 1.389(3) ? C19 H19 . 0.9500 ? C20 C21 . 1.392(3) ? C20 H20 . 0.9500 ? C21 C22 . 1.396(3) ? C21 C24 . 1.504(3) ? C22 C23 . 1.392(3) ? C22 H22 . 0.9500 ? C23 H23 . 0.9500 ? C24 H24A . 0.9800 ? C24 H24B . 0.9800 ? C24 H24C . 0.9800 ? C25 N25 . 1.143(3) ? C26 C31 . 1.393(3) ? C26 C27 . 1.397(3) ? C27 C28 . 1.387(3) ? C27 H27 . 0.9500 ? C28 C29 . 1.393(3) ? C28 H28 . 0.9500 ? C29 C30 . 1.391(3) ? C29 C32 . 1.506(3) ? C30 C31 . 1.391(3) ? C30 H30 . 0.9500 ? C31 H31 . 0.9500 ? C32 H32A . 0.9800 ? C32 H32B . 0.9800 ? C32 H32C . 0.9800 ? C33 H33A . 0.9800 ? C33 H33B . 0.9800 ? C33 H33C . 0.9800 ? C34 O34 . 1.229(3) ? C34 N34 . 1.335(3) ? C34 H34 . 0.9500 ? C35 N34 . 1.455(3) ? C35 H35A . 0.9800 ? C35 H35B . 0.9800 ? C35 H35C . 0.9800 ? C36 N34 . 1.456(3) ? C36 H36A . 0.9800 ? C36 H36B . 0.9800 ? C36 H36C . 0.9800 ? N2 H2N . 0.94(3) ? N10 H10N . 0.95(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C6 H6 O34 . 1.00 2.44 3.297(3) 143 yes C8 H8 O34 . 1.00 2.34 3.241(3) 149 yes C13 H13 O34 . 0.95 2.47 3.373(3) 159 yes C27 H27 N10 . 0.95 2.56 3.432(3) 152 yes C30 H30 N11 4_575 0.95 2.61 3.515(3) 160 yes C33 H33C O4 4_566 0.98 2.48 3.447(3) 170 yes C35 H35C O34 . 0.98 2.39 2.787(3) 104 no C24 H24C Cg7 2_646 0.98 2.84 3.715(2) 148 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 C11 C1 C2 N2 . . . . -21.8(3) ? C9 C1 C2 N2 . . . . -141.3(2) ? C8 C1 C2 N2 . . . . 99.8(2) ? C11 C1 C2 N3 . . . . 162.27(17) ? C9 C1 C2 N3 . . . . 42.7(2) ? C8 C1 C2 N3 . . . . -76.1(2) ? O4 C4 C5 C9 . . . . 161.19(19) ? N3 C4 C5 C9 . . . . -19.4(3) ? O4 C4 C5 C6 . . . . -74.4(2) ? N3 C4 C5 C6 . . . . 105.0(2) ? C4 C5 C6 C18 . . . . 128.31(18) ? C9 C5 C6 C18 . . . . -105.81(19) ? C4 C5 C6 C7 . . . . -109.82(18) ? C9 C5 C6 C7 . . . . 16.1(2) ? C18 C6 C7 C25 . . . . -64.0(2) ? C5 C6 C7 C25 . . . . 171.40(16) ? C18 C6 C7 C10 . . . . 57.3(2) ? C5 C6 C7 C10 . . . . -67.34(19) ? C18 C6 C7 C8 . . . . 176.56(16) ? C5 C6 C7 C8 . . . . 51.9(2) ? C25 C7 C8 C26 . . . . 47.0(2) ? C10 C7 C8 C26 . . . . -78.3(2) ? C6 C7 C8 C26 . . . . 166.10(16) ? C25 C7 C8 C1 . . . . 173.51(16) ? C10 C7 C8 C1 . . . . 48.2(2) ? C6 C7 C8 C1 . . . . -67.4(2) ? C11 C1 C8 C26 . . . . 19.3(2) ? C2 C1 C8 C26 . . . . -100.43(19) ? C9 C1 C8 C26 . . . . 139.59(17) ? C11 C1 C8 C7 . . . . -109.61(19) ? C2 C1 C8 C7 . . . . 130.67(17) ? C9 C1 C8 C7 . . . . 10.7(2) ? C4 C5 C9 O9 . . . . 167.19(16) ? C6 C5 C9 O9 . . . . 43.6(2) ? C4 C5 C9 C33 . . . . -74.8(2) ? C6 C5 C9 C33 . . . . 161.62(17) ? C4 C5 C9 C1 . . . . 51.1(2) ? C6 C5 C9 C1 . . . . -72.5(2) ? C11 C1 C9 O9 . . . . 59.6(2) ? C2 C1 C9 O9 . . . . 179.10(15) ? C8 C1 C9 O9 . . . . -62.54(19) ? C11 C1 C9 C33 . . . . -57.5(2) ? C2 C1 C9 C33 . . . . 62.1(2) ? C8 C1 C9 C33 . . . . -179.57(16) ? C11 C1 C9 C5 . . . . 177.32(16) ? C2 C1 C9 C5 . . . . -63.1(2) ? C8 C1 C9 C5 . . . . 55.2(2) ? C25 C7 C10 N10 . . . . -1.0(3) ? C8 C7 C10 N10 . . . . 122.2(2) ? C6 C7 C10 N10 . . . . -119.4(2) ? C25 C7 C10 O9 . . . . 176.72(16) ? C8 C7 C10 O9 . . . . -60.1(2) ? C6 C7 C10 O9 . . . . 58.3(2) ? C17 C12 C13 C14 . . . . 0.8(3) ? N3 C12 C13 C14 . . . . 179.8(2) ? C12 C13 C14 C15 . . . . -0.5(3) ? C13 C14 C15 C16 . . . . 0.2(4) ? C14 C15 C16 C17 . . . . -0.2(3) ? C13 C12 C17 C16 . . . . -0.7(3) ? N3 C12 C17 C16 . . . . -179.82(19) ? C15 C16 C17 C12 . . . . 0.4(3) ? C5 C6 C18 C23 . . . . -156.70(18) ? C7 C6 C18 C23 . . . . 83.9(2) ? C5 C6 C18 C19 . . . . 27.2(3) ? C7 C6 C18 C19 . . . . -92.2(2) ? C23 C18 C19 C20 . . . . -3.6(3) ? C6 C18 C19 C20 . . . . 172.57(19) ? C18 C19 C20 C21 . . . . -1.2(3) ? C19 C20 C21 C22 . . . . 5.1(3) ? C19 C20 C21 C24 . . . . -172.4(2) ? C20 C21 C22 C23 . . . . -4.2(3) ? C24 C21 C22 C23 . . . . 173.3(2) ? C21 C22 C23 C18 . . . . -0.5(3) ? C19 C18 C23 C22 . . . . 4.4(3) ? C6 C18 C23 C22 . . . . -171.82(19) ? C7 C8 C26 C31 . . . . -148.55(19) ? C1 C8 C26 C31 . . . . 87.2(2) ? C7 C8 C26 C27 . . . . 35.4(3) ? C1 C8 C26 C27 . . . . -88.9(2) ? C31 C26 C27 C28 . . . . -0.3(3) ? C8 C26 C27 C28 . . . . 175.78(19) ? C26 C27 C28 C29 . . . . -1.0(3) ? C27 C28 C29 C30 . . . . 1.4(3) ? C27 C28 C29 C32 . . . . -177.4(2) ? C28 C29 C30 C31 . . . . -0.6(3) ? C32 C29 C30 C31 . . . . 178.2(2) ? C29 C30 C31 C26 . . . . -0.7(3) ? C27 C26 C31 C30 . . . . 1.1(3) ? C8 C26 C31 C30 . . . . -175.21(19) ? O4 C4 N3 C2 . . . . 175.69(19) ? C5 C4 N3 C2 . . . . -3.7(3) ? O4 C4 N3 C12 . . . . 1.0(3) ? C5 C4 N3 C12 . . . . -178.45(17) ? N2 C2 N3 C4 . . . . 175.9(2) ? C1 C2 N3 C4 . . . . -8.5(3) ? N2 C2 N3 C12 . . . . -9.4(3) ? C1 C2 N3 C12 . . . . 166.25(17) ? C17 C12 N3 C4 . . . . -98.1(2) ? C13 C12 N3 C4 . . . . 82.8(2) ? C17 C12 N3 C2 . . . . 86.7(2) ? C13 C12 N3 C2 . . . . -92.4(2) ? O34 C34 N34 C35 . . . . 5.8(4) ? O34 C34 N34 C36 . . . . 178.1(2) ? N10 C10 O9 C9 . . . . -177.47(19) ? C7 C10 O9 C9 . . . . 4.7(2) ? C33 C9 O9 C10 . . . . 178.80(16) ? C5 C9 O9 C10 . . . . -59.0(2) ? C1 C9 O9 C10 . . . . 56.6(2) ?