#------------------------------------------------------------------------------ #$Date: 2022-07-23 05:08:35 +0100 (Sat, 23 Jul 2022) $ #$Revision: 276899 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244129.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_2244129 loop_ _publ_author_name 'Mahmudov, Ibadulla' 'Atio\(glu, Zeliha' 'Akkurt, Mehmet' 'Abdullayev, Yusif' 'Sujayev, Afsun' 'Bhattarai, Ajaya' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of 2-(4-amino-6-phenyl-1,2,5,6-tetrahydro-1,3,5-triazin-2-ylidene)malononitrile dimethylformamide hemisolvate ; _journal_coeditor_code ZL5032 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989022006910 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac '2C12 H10 N6, C3 H7 N O' _chemical_formula_moiety '2(C12 H10 N6), C3 H7 N O' _chemical_formula_sum 'C27 H27 N13 O' _chemical_formula_weight 549.61 _chemical_name_common ; 2-(4-Amino-6-phenyl-1,2,5,6-tetrahydro-1,3,5-triazin-2-ylidene)malononitrile dimethylformamide hemisolvate ; _chemical_name_systematic ; 2-(4-Amino-6-phenyl-1,2,5,6-tetrahydro-1,3,5-triazin-2-ylidene)propanedinitrile dimethylformamide hemisolvate ; _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 _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 98.024(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.9102(4) _cell_length_b 13.5595(7) _cell_length_c 22.0520(12) _cell_measurement_reflns_used 7300 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.37 _cell_measurement_theta_min 2.40 _cell_volume 2638.2(2) _computing_cell_refinement ; SAINT (Bruker, 2018) ; _computing_data_collection ; APEX3 (Bruker, 2018) ; _computing_data_reduction ; SAINT (Bruker, 2018) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker D8 Quest PHOTON 100 detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_unetI/netI 0.0393 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 19167 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.386 _diffrn_reflns_theta_min 2.395 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_correction_T_min 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2018) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.384 _exptl_crystal_description block _exptl_crystal_F_000 1152 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.260 _refine_diff_density_max 0.243 _refine_diff_density_min -0.233 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 422 _refine_ls_number_reflns 5368 _refine_ls_number_restraints 219 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0453 _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^)+(0.0406P)^2^+1.7380P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1015 _refine_ls_wR_factor_ref 0.1107 _reflns_number_gt 4215 _reflns_number_total 5368 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zl5032sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2244129 _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 0.973 _shelx_estimated_absorpt_t_max 0.976 _shelx_hkl_file ; -1 0 0 274.67 7.80 2 0 0 601.64 17.30 -2 0 0 638.74 17.40 -3 0 0 3365.06 81.29 3 0 0 3118.29 80.79 -4 0 0 1043.60 28.90 4 0 0 990.80 28.60 5 0 0 958.40 28.00 -5 0 0 860.71 27.10 -6 0 0 3329.37 82.99 6 0 0 3000.50 81.69 7 0 0 126.89 14.30 -7 0 0 105.49 9.80 8 0 0 2.20 7.40 -8 0 0 4.40 5.20 9 0 0 732.03 30.40 -9 0 0 702.03 26.80 10 0 0 56.69 10.00 -10 0 0 32.20 7.60 -11 0 0 10.80 7.10 11 0 0 15.20 8.60 1 -1 0 825.12 21.90 -1 -1 0 851.61 20.90 -1 -1 0 831.22 21.10 1 1 0 839.52 20.90 -1 1 0 863.51 21.90 -2 -1 0 575.14 15.80 2 -1 0 582.84 16.80 -2 1 0 583.54 16.60 2 1 0 539.55 16.20 -3 -1 0 45.70 5.10 3 -1 0 38.00 4.60 -3 1 0 44.30 5.50 3 1 0 46.50 4.50 -4 -1 0 88.09 6.80 4 -1 0 84.59 7.80 -4 1 0 97.79 7.40 5 -1 0 473.05 17.50 -5 -1 0 485.65 16.60 -5 1 0 469.05 17.20 -6 -1 0 260.87 12.20 6 -1 0 232.68 13.00 6 1 0 231.58 13.90 -6 1 0 244.28 12.50 -7 -1 0 96.29 9.20 -7 1 0 100.59 9.90 -8 -1 0 217.38 13.20 8 -1 0 210.58 16.30 -8 1 0 221.68 14.40 8 1 0 242.68 18.20 -9 -1 0 -4.20 4.80 9 -1 0 1.80 8.80 9 1 0 15.10 8.40 -9 1 0 5.60 5.60 9 1 0 4.00 6.10 10 -1 0 113.39 15.20 -10 -1 0 76.19 9.60 10 1 0 75.09 10.60 -10 1 0 79.59 10.30 11 -1 0 267.37 18.90 -11 -1 0 216.88 15.80 -11 1 0 218.48 16.80 11 1 0 241.88 18.40 0 -2 0 682.33 17.90 -1 -2 0 187.28 5.40 1 -2 0 177.78 7.40 1 2 0 174.48 5.50 -1 2 0 178.38 7.10 2 -2 0 6495.45 160.58 -2 2 0 6578.84 160.68 2 2 0 6570.84 158.58 3 -2 0 1527.45 40.80 -3 -2 0 1543.65 39.20 3 2 0 1494.15 38.60 3 2 0 1481.55 39.10 -3 2 0 1546.15 40.90 -4 -2 0 43.80 5.80 4 -2 0 28.10 4.80 -4 2 0 31.50 5.00 5 -2 0 259.77 13.00 -5 -2 0 297.47 11.80 5 2 0 285.57 11.20 -5 2 0 285.47 13.10 6 -2 0 207.78 12.80 -6 -2 0 199.48 10.50 -6 2 0 205.58 11.90 6 2 0 202.28 10.40 6 2 0 224.98 13.80 -7 -2 0 975.80 29.70 7 2 0 911.31 31.00 -7 2 0 961.70 31.40 7 2 0 909.91 28.80 -8 -2 0 18.40 5.60 8 -2 0 27.80 8.00 8 2 0 38.50 9.00 -8 2 0 30.20 6.90 8 2 0 21.50 6.60 9 -2 0 8.60 8.20 -9 -2 0 14.00 5.50 -9 2 0 19.90 6.90 9 2 0 33.50 8.80 9 2 0 13.10 6.70 -10 -2 0 62.99 8.60 10 -2 0 50.99 13.30 10 2 0 79.69 12.60 10 2 0 62.49 9.90 -10 2 0 69.99 10.10 0 -3 0 1.60 2.10 2 -3 0 1099.19 29.50 -2 3 0 1010.10 29.20 -3 -3 0 1140.59 30.30 3 -3 0 1151.28 32.60 3 3 0 1143.09 29.50 -3 3 0 1173.58 32.60 4 -3 0 197.28 11.10 -4 3 0 197.78 10.50 5 -3 0 433.56 17.40 -5 -3 0 448.16 15.20 5 3 0 429.26 14.20 -5 3 0 465.55 17.50 6 -3 0 533.75 20.80 -6 -3 0 541.45 18.20 -6 3 0 538.55 20.50 6 3 0 505.25 19.60 6 3 0 510.15 17.00 -7 -3 0 17.60 4.80 7 3 0 17.30 4.90 -7 3 0 16.40 5.50 7 3 0 19.60 6.50 8 -3 0 731.03 28.50 -8 -3 0 664.63 23.40 8 3 0 594.94 28.90 -8 3 0 675.73 26.40 8 3 0 669.53 23.10 9 -3 0 10.10 8.60 -9 -3 0 27.40 6.30 -9 3 0 19.10 6.90 9 3 0 15.60 6.90 10 -3 0 -2.20 9.60 -10 -3 0 17.70 6.20 10 3 0 5.90 7.90 -10 3 0 11.40 6.90 0 -4 0 761.82 21.30 1 -4 0 5870.41 144.89 -1 -4 0 5767.82 143.19 -1 4 0 5992.20 145.09 -2 -4 0 1523.95 38.60 2 -4 0 1540.15 41.60 -2 4 0 1560.94 41.60 2 4 0 1536.85 38.70 -3 -4 0 454.55 14.20 3 -4 0 484.45 17.20 -3 4 0 481.05 16.90 4 -4 0 318.77 14.30 -4 -4 0 311.07 11.50 -4 4 0 328.37 14.00 4 4 0 339.37 10.90 5 -4 0 101.99 10.00 -5 -4 0 117.99 7.30 5 4 0 116.89 6.50 -5 4 0 103.79 9.20 6 -4 0 25.80 6.20 -6 -4 0 23.80 4.50 -6 4 0 24.10 6.00 6 4 0 26.50 4.40 7 -4 0 109.69 13.00 -7 -4 0 124.89 9.00 -7 4 0 114.79 11.50 -8 -4 0 50.29 6.80 8 -4 0 60.19 10.20 -8 4 0 59.69 8.80 -9 -4 0 102.79 9.90 9 -4 0 82.99 11.90 -9 4 0 98.29 12.80 9 4 0 101.39 10.10 -10 -4 0 240.08 14.00 10 -4 0 191.08 21.30 -10 4 0 233.58 17.80 10 4 0 213.18 13.50 0 -5 0 0.60 2.20 1 -5 0 829.82 24.20 -1 -5 0 804.72 22.50 -1 5 0 839.22 24.50 2 -5 0 11.40 4.00 -2 -5 0 17.00 2.70 -2 5 0 11.80 4.00 3 -5 0 235.78 11.70 -3 5 0 212.48 11.20 4 -5 0 16.20 4.80 -4 -5 0 17.20 4.00 -4 5 0 21.40 4.90 5 -5 0 97.09 10.10 -5 -5 0 79.69 6.90 -5 5 0 75.99 8.80 -6 -5 0 77.29 7.20 6 -5 0 84.99 10.60 -6 5 0 84.29 9.90 7 -5 0 51.89 8.60 -7 -5 0 56.59 7.20 -7 5 0 46.50 7.60 -8 -5 0 202.28 11.40 8 -5 0 188.48 16.90 -8 5 0 199.78 15.10 -9 -5 0 27.90 5.90 9 -5 0 6.40 8.90 -9 5 0 25.10 7.60 10 -5 0 34.50 11.50 -10 -5 0 57.49 7.40 -10 5 0 75.49 11.90 0 -6 0 6490.05 160.38 -1 -6 0 274.07 10.60 -1 -6 0 266.87 10.00 1 -6 0 274.47 11.60 2 -6 0 78.09 7.70 -2 -6 0 63.49 5.40 -2 6 0 84.29 7.80 3 -6 0 1436.26 41.20 -3 6 0 1431.16 41.20 4 -6 0 8.80 4.50 -4 6 0 7.40 4.30 5 -6 0 191.18 12.80 -5 -6 0 180.28 9.40 -5 6 0 199.58 12.40 -6 -6 0 184.08 9.70 6 -6 0 161.08 13.40 -6 6 0 172.58 12.90 -7 -6 0 0.60 3.90 7 -6 0 -3.70 5.80 -7 6 0 4.10 4.80 8 -6 0 85.69 11.80 -8 -6 0 91.19 8.70 -8 6 0 84.89 12.30 9 -6 0 12.50 9.00 -9 -6 0 13.70 4.90 -9 6 0 12.20 6.70 10 -6 0 56.79 13.30 -10 -6 0 85.19 9.30 -10 6 0 81.39 11.70 0 -7 0 1.60 2.90 1 -7 0 1428.86 40.10 -1 -7 0 1437.86 38.90 2 -7 0 12.10 4.20 -2 -7 0 20.00 3.40 -2 7 0 14.80 4.30 3 -7 0 64.99 8.20 -3 -7 0 64.29 4.60 -3 7 0 60.79 7.90 4 -7 0 12.50 5.10 -4 7 0 3.90 4.20 -5 -7 0 -4.30 3.10 5 -7 0 1.30 5.00 -5 7 0 4.60 4.90 6 -7 0 386.66 19.60 -6 -7 0 375.16 14.20 -6 7 0 382.86 18.90 -7 -7 0 159.58 9.70 7 -7 0 159.58 14.90 -7 7 0 168.68 14.10 -8 -7 0 36.30 5.50 8 -7 0 26.60 9.00 -8 7 0 30.90 7.30 -9 -7 0 147.49 9.70 9 -7 0 115.29 14.00 -9 7 0 148.59 15.60 10 -7 0 -14.70 10.90 -10 -7 0 5.40 4.30 -10 7 0 2.60 7.00 0 -8 0 47.90 5.90 0 -8 0 56.19 6.20 -1 -8 0 2119.99 55.59 1 -8 0 2121.49 56.89 -1 -8 0 2056.59 54.79 -2 -8 0 75.69 6.00 -2 -8 0 49.99 6.20 2 -8 0 58.19 8.00 3 -8 0 658.03 23.70 -3 -8 0 668.03 19.10 -3 8 0 651.83 23.70 4 -8 0 315.87 16.00 -4 8 0 306.77 15.60 5 -8 0 -0.70 5.10 -5 -8 0 5.50 4.50 -5 8 0 -2.90 3.70 -6 -8 0 1.00 3.70 6 -8 0 10.30 6.30 -6 8 0 2.60 5.40 -7 -8 0 97.99 8.30 7 -8 0 111.59 14.00 -7 8 0 116.19 13.00 8 -8 0 106.19 15.40 -8 -8 0 115.49 8.60 -8 8 0 119.19 14.10 -9 -8 0 3.00 3.80 9 -8 0 -17.80 7.80 -9 8 0 -1.70 6.10 0 -9 0 1.20 3.50 0 -9 0 2.40 3.30 -1 -9 0 91.59 7.30 -1 -9 0 97.19 7.20 1 -9 0 96.69 8.40 2 -9 0 252.27 13.30 -2 -9 0 242.88 11.20 -2 -9 0 256.97 10.60 -3 -9 0 60.59 5.40 3 -9 0 69.79 9.20 -3 9 0 54.79 7.70 4 -9 0 571.14 23.20 -4 9 0 598.54 23.60 -5 -9 0 118.09 8.80 5 -9 0 136.09 12.90 -5 9 0 125.39 12.40 -6 -9 0 855.01 25.90 6 -9 0 845.12 32.10 -6 9 0 854.91 32.00 -7 -9 0 141.69 9.10 7 -9 0 156.58 15.50 -7 9 0 178.38 15.10 8 -9 0 -10.80 6.60 -8 -9 0 -2.10 3.50 -8 9 0 7.80 7.50 -9 -9 0 6.30 4.00 -9 9 0 4.70 6.70 0 -10 0 809.62 25.90 0 -10 0 770.42 25.10 1 -10 0 32.80 5.30 -1 -10 0 36.10 5.40 -1 -10 0 26.20 4.60 2 -10 0 708.33 25.20 -2 -10 0 700.23 22.80 -2 -10 0 701.33 21.90 3 -10 0 1132.69 36.40 -3 -10 0 1097.89 32.40 -3 -10 0 1116.89 31.00 4 -10 0 641.54 25.40 -4 10 0 635.74 25.50 5 -10 0 266.77 16.70 -5 -10 0 256.07 11.70 -5 10 0 263.07 16.60 6 -10 0 5.70 6.40 -6 10 0 13.30 7.00 -7 -10 0 60.39 7.10 7 -10 0 66.49 10.70 -7 10 0 93.79 13.40 8 -10 0 -3.50 8.00 -8 -10 0 -3.70 3.70 -8 10 0 2.10 6.70 0 -11 0 3.80 4.50 0 -11 0 0.10 3.50 -1 -11 0 77.39 7.90 -1 -11 0 89.89 8.30 1 -11 0 94.49 9.70 1 -11 0 75.89 9.20 -2 -11 0 106.59 8.30 -2 -11 0 87.99 8.40 2 -11 0 95.59 10.40 -3 -11 0 42.20 5.80 -3 -11 0 53.59 6.00 3 -11 0 38.60 7.60 -4 -11 0 37.80 5.60 4 -11 0 30.50 6.70 5 -11 0 29.00 7.80 -5 11 0 29.30 6.60 6 -11 0 74.59 10.70 -6 -11 0 60.09 7.10 -6 11 0 57.59 8.40 -7 -11 0 41.40 5.70 7 -11 0 35.80 9.10 -7 11 0 44.30 8.20 8 -11 0 101.89 13.30 -8 -11 0 129.39 8.40 -8 11 0 143.39 16.50 0 -12 0 6.60 4.40 0 -12 0 6.10 5.10 1 -12 0 237.58 14.00 1 -12 0 264.37 14.50 -1 -12 0 235.18 12.70 -1 -12 0 251.27 12.70 2 -12 0 106.49 11.20 2 -12 0 116.09 11.50 -2 -12 0 125.49 9.50 -2 -12 0 133.19 8.80 3 -12 0 22.90 6.50 -3 -12 0 26.30 5.50 4 -12 0 750.72 29.30 -4 -12 0 720.73 23.90 -5 -12 0 14.70 4.40 5 -12 0 10.80 6.70 -6 -12 0 15.50 4.20 6 -12 0 14.40 7.60 -6 -12 0 5.50 4.10 -7 -12 0 5.00 3.50 7 -12 0 -4.20 6.80 0 -13 0 1.30 3.90 0 -13 0 5.10 5.10 -1 -13 0 86.39 8.90 -1 -13 0 85.39 8.90 1 -13 0 91.29 10.30 1 -13 0 96.59 10.50 -2 -13 0 0.40 4.00 2 -13 0 5.50 5.60 2 -13 0 1.20 6.20 -3 -13 0 18.50 5.40 3 -13 0 26.90 7.10 -4 -13 0 5.70 4.20 4 -13 0 7.20 6.40 5 -13 0 47.90 9.60 -5 -13 0 46.70 6.10 6 -13 0 63.49 11.20 -6 -13 0 64.79 7.20 -6 -13 0 77.29 7.50 -7 -13 0 49.90 5.80 7 -13 0 64.39 11.30 0 -14 0 32.80 6.90 0 -14 0 34.40 7.10 1 -14 0 79.69 10.80 -1 -14 0 83.79 9.00 1 -14 0 105.59 11.20 -1 -14 0 97.99 9.60 2 -14 0 2.10 5.30 -2 -14 0 1.10 4.20 2 -14 0 2.80 6.10 3 -14 0 9.40 7.40 -3 -14 0 4.80 4.30 3 -14 0 11.80 6.50 4 -14 0 6.90 7.20 -4 -14 0 10.50 4.80 4 -14 0 7.80 7.10 -5 -14 0 0.10 3.80 5 -14 0 3.80 7.10 -6 -14 0 317.67 13.60 6 -14 0 334.07 21.80 -6 -14 0 281.07 12.90 0 -15 0 0.00 5.40 0 -15 0 -2.30 4.30 -1 -15 0 -3.10 3.90 -1 -15 0 9.50 5.00 1 -15 0 9.50 6.00 1 -15 0 -0.10 5.00 2 -15 0 17.80 7.30 2 -15 0 28.40 7.30 -2 -15 0 16.00 5.20 3 -15 0 7.00 6.00 -3 -15 0 11.70 3.50 3 -15 0 6.20 7.30 -3 -15 0 2.30 4.50 4 -15 0 17.20 7.50 4 -15 0 24.00 7.90 -4 -15 0 9.00 4.90 5 -15 0 90.09 12.40 -5 -15 0 88.79 8.70 5 -15 0 110.89 14.30 0 -16 0 9.20 6.20 0 -16 0 -0.70 4.40 1 -16 0 3.90 6.30 -1 -16 0 9.30 5.10 1 -16 0 20.50 7.10 2 -16 0 26.80 7.70 2 -16 0 10.40 6.30 -2 -16 0 7.50 4.90 3 -16 0 22.10 8.00 -3 -16 0 29.00 6.50 3 -16 0 49.60 9.90 -11 0 1 -2.00 6.20 11 0 -1 -14.30 7.90 10 0 -1 -0.20 7.40 10 0 -1 38.00 12.40 -10 0 1 5.40 5.50 9 0 -1 -7.70 6.30 -9 0 1 2.70 5.50 9 0 -1 15.80 8.90 -8 0 1 -1.20 4.30 8 0 -1 -0.90 6.40 7 0 -1 17.10 6.50 -6 0 1 1.60 3.60 6 0 -1 10.10 5.00 -5 0 1 1.00 3.30 -4 0 1 0.20 2.80 4 0 -1 3.10 3.40 3 0 -1 2.80 2.90 -3 0 1 1.70 2.70 2 0 -1 2.20 2.50 -2 0 1 -0.50 2.10 -1 0 1 0.00 1.00 -1 0 -1 1.80 1.50 1 0 1 1.10 1.80 2 0 1 -1.60 3.10 -2 0 -1 -0.30 2.70 -3 0 -1 -1.40 2.80 3 0 1 -3.50 3.30 4 0 1 8.00 4.10 -4 0 -1 1.80 3.40 -5 0 -1 1.40 3.50 -6 0 -1 3.80 4.10 6 0 1 8.90 5.10 -7 0 -1 1.70 4.40 -8 0 -1 0.40 5.10 8 0 1 5.50 8.40 -9 0 -1 5.10 5.70 9 0 1 12.00 9.10 10 0 1 14.80 10.40 -11 -1 1 141.09 13.20 11 -1 -1 166.18 17.30 -11 1 1 146.79 15.00 11 1 -1 134.59 16.70 -10 -1 1 7.90 6.10 10 -1 -1 30.10 12.00 10 1 -1 29.30 10.90 -10 1 1 0.90 5.30 10 1 -1 -5.60 7.40 9 -1 -1 26.60 8.60 -9 -1 1 22.40 6.20 -9 1 1 24.40 6.80 9 1 -1 15.80 7.20 9 1 -1 24.10 9.20 -8 -1 1 403.56 17.50 8 -1 -1 392.16 20.30 8 1 -1 400.86 20.50 -8 1 1 416.46 18.60 8 1 -1 413.96 18.20 7 -1 -1 2004.50 55.99 -7 -1 1 2039.40 55.09 7 1 -1 2001.70 55.39 -7 1 1 2009.30 55.99 7 1 -1 1931.31 55.29 -6 -1 1 30.60 4.90 6 -1 -1 25.40 5.40 -6 1 1 33.50 5.40 6 1 -1 31.00 5.80 -5 -1 1 604.84 19.00 5 -1 -1 580.84 19.80 -5 1 1 579.64 19.70 4 -1 -1 972.30 28.10 -4 -1 1 998.70 27.30 4 1 -1 932.01 27.10 -4 1 1 1013.70 28.30 3 -1 -1 846.32 23.80 -3 -1 1 854.41 22.70 -3 1 1 846.42 23.70 3 1 -1 791.72 22.60 -2 -1 1 1064.29 26.70 2 -1 -1 1024.10 27.70 2 1 -1 1013.70 26.70 -2 1 1 1071.09 27.80 2 1 -1 1062.09 27.20 1 -1 -1 1392.56 35.60 -1 -1 1 1440.26 35.20 -1 1 1 1414.86 35.60 1 1 -1 1419.56 35.20 1 -1 1 791.12 21.80 -1 1 -1 805.42 21.70 -2 -1 -1 606.84 17.50 2 -1 1 607.24 18.00 2 1 1 607.34 17.90 -2 1 -1 642.14 18.10 3 -1 1 1196.48 33.50 -3 -1 -1 1227.18 32.90 -3 1 -1 1335.07 34.00 3 1 1 1179.38 33.10 -4 -1 -1 1901.41 50.19 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1019.20 29.40 1 -7 4 403.06 15.20 1 -7 4 365.76 15.30 -1 7 -4 398.66 15.10 2 -7 4 12.80 5.20 2 -7 4 14.00 4.60 -2 7 -4 11.10 4.40 3 -7 4 228.78 12.50 3 -7 4 215.78 12.80 -3 7 -4 216.08 12.30 4 -7 4 139.19 11.50 -4 7 -4 141.89 10.80 -5 -7 -4 15.80 6.20 5 -7 4 2.90 5.20 -5 7 -4 5.80 5.30 -6 -7 -4 -1.10 4.60 6 -7 4 -5.70 5.70 -6 7 -4 -6.30 4.90 -7 -7 -4 50.59 7.50 7 -7 4 44.80 8.70 -7 7 -4 51.89 9.20 -8 -7 -4 7.10 5.80 8 -7 4 11.40 8.40 -8 7 -4 20.00 7.50 -9 -7 -4 0.80 5.20 9 -7 4 -20.60 8.80 -9 7 -4 5.90 7.10 9 -8 -4 130.49 16.30 8 -8 -4 18.60 7.90 8 8 -4 24.90 5.10 7 -8 -4 27.00 7.60 7 8 -4 22.10 5.20 6 -8 -4 257.17 16.30 6 8 -4 233.68 11.00 5 -8 -4 334.77 17.30 -5 -8 4 302.47 12.70 5 8 -4 316.87 12.70 -4 -8 4 -0.30 3.60 4 -8 -4 3.30 4.70 4 8 -4 4.40 4.00 -3 -8 4 687.93 19.40 -3 -8 4 694.53 21.70 3 -8 -4 645.74 24.00 3 8 -4 687.13 21.70 2 -8 -4 2.70 4.40 -2 -8 4 3.80 2.90 -2 -8 4 5.90 3.80 -1 -8 4 274.17 12.30 -1 -8 4 266.77 11.10 1 -8 -4 266.37 13.10 0 -8 4 181.58 10.70 0 -8 4 195.18 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11.40 -2 -10 -4 147.29 8.10 2 -10 4 152.28 11.60 -2 10 -4 139.39 11.30 3 -10 4 136.39 12.20 3 -10 4 123.59 11.70 -3 10 -4 122.09 11.40 4 -10 4 565.94 23.80 4 -10 4 519.25 23.00 -4 10 -4 535.55 23.10 -5 -10 -4 6.60 4.70 5 -10 4 -1.20 6.40 5 -10 4 -5.60 6.30 -5 10 -4 7.50 6.30 6 -10 4 19.70 8.20 -6 -10 -4 15.00 5.40 6 -10 4 6.30 7.00 -6 10 -4 19.40 6.70 7 -10 4 0.00 7.20 7 -10 4 -2.10 8.00 -7 -10 -4 -6.30 4.90 -7 10 -4 0.00 6.00 8 -10 4 28.10 9.70 -8 10 -4 38.40 10.40 8 -11 -4 48.30 10.30 7 -11 -4 55.89 9.80 -6 -11 4 48.30 6.50 6 -11 -4 36.90 8.20 -5 -11 4 -10.00 3.90 5 -11 -4 -2.00 5.60 -4 -11 4 0.50 4.30 4 -11 -4 7.80 6.10 -4 -11 4 4.60 3.10 -3 -11 4 133.89 9.70 -3 -11 4 145.89 8.60 3 -11 -4 157.08 12.70 -2 -11 4 10.70 4.10 -2 -11 4 17.80 5.30 2 -11 -4 19.80 6.10 -1 -11 4 433.06 16.50 -1 -11 4 397.46 17.20 1 -11 -4 419.76 18.70 0 -11 4 20.00 5.90 0 -11 4 12.80 4.40 0 -11 -4 12.80 4.70 1 -11 4 11.30 4.90 -1 -11 -4 10.30 4.50 -1 -11 -4 18.50 4.70 1 -11 4 13.70 6.40 -2 -11 -4 16.90 4.30 2 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748.73 29.10 4 -12 4 -1.40 5.80 4 -12 4 -0.50 6.20 -4 12 -4 0.90 6.10 5 -12 4 117.19 13.90 5 -12 4 119.29 14.20 -5 12 -4 136.39 14.40 -6 -12 -4 52.19 7.30 6 -12 4 64.39 11.20 6 -12 4 51.99 10.60 -6 12 -4 69.69 11.30 7 -12 4 -10.30 7.50 -7 -12 -4 -1.80 5.30 7 -12 4 15.10 7.80 -7 12 -4 14.50 8.80 7 -13 -4 2.60 6.80 6 -13 -4 29.10 8.20 -5 -13 4 72.99 8.10 -4 -13 4 1.00 4.60 -4 -13 4 12.10 3.80 4 -13 -4 10.10 6.60 -3 -13 4 5.40 4.60 -3 -13 4 -0.50 3.60 3 -13 -4 -3.40 5.40 -2 -13 4 9.50 4.60 -2 -13 4 2.70 3.90 2 -13 -4 9.00 5.40 -1 -13 4 46.40 6.40 1 -13 -4 46.50 8.00 -1 -13 4 50.29 7.50 0 -13 4 204.28 12.30 0 -13 -4 180.48 11.40 0 -13 -4 187.88 13.00 0 -13 4 182.68 13.60 -1 -13 -4 8.00 4.40 -1 -13 -4 1.40 4.10 1 -13 4 4.90 4.60 1 -13 4 0.70 6.10 -2 -13 -4 77.29 7.70 2 -13 4 58.89 9.10 -2 -13 -4 61.19 8.50 2 -13 4 62.89 10.40 -3 -13 -4 129.59 10.50 3 -13 4 131.99 13.30 3 -13 4 120.29 13.00 4 -13 4 36.00 9.10 4 -13 4 33.10 8.20 -4 13 -4 26.40 7.30 5 -13 4 51.59 9.70 -5 13 -4 65.79 11.20 -6 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29.10 8.40 0 3 25 10.10 6.80 0 3 -25 7.40 8.30 0 3 -25 5.00 9.30 1 -3 25 74.09 14.70 -1 -3 -25 67.89 14.00 -1 3 -25 71.09 12.80 1 3 25 83.19 12.00 2 -3 25 -9.30 12.30 -2 -3 -25 26.30 8.50 -2 3 -25 14.10 8.80 2 3 25 23.00 9.00 -2 3 -25 54.69 14.50 -5 -4 25 18.30 9.80 5 -4 -25 17.30 10.60 5 4 -25 7.50 10.50 -4 -4 25 2.70 9.10 4 -4 -25 6.80 8.10 4 4 -25 20.90 9.30 4 4 -25 4.30 8.10 3 -4 -25 10.40 8.60 -3 -4 25 1.30 9.20 3 4 -25 -2.30 7.70 3 4 -25 16.20 8.90 -2 -4 25 5.40 9.80 2 -4 -25 24.80 8.30 2 4 -25 12.30 8.60 2 4 -25 29.90 10.50 1 -4 -25 15.80 6.80 -1 -4 25 -2.40 8.20 1 -4 -25 -14.70 7.60 -1 4 25 8.30 6.20 1 4 -25 12.20 8.80 1 4 -25 -3.70 8.20 0 -4 25 -0.80 9.70 0 4 -25 5.60 9.00 0 4 -25 20.70 10.20 0 4 25 5.70 5.80 1 -4 25 -3.60 9.00 -1 -4 -25 -12.40 9.40 -1 4 -25 9.30 9.70 -1 4 -25 12.20 9.30 1 4 25 3.10 5.80 2 -4 25 3.90 12.60 -2 -4 -25 47.20 10.40 -2 -4 -25 5.90 14.70 2 4 25 21.10 7.20 -2 4 -25 33.40 11.10 -4 -5 25 35.90 12.50 4 -5 -25 48.90 13.70 4 5 -25 55.29 9.40 4 5 -25 52.79 12.30 3 -5 -25 49.80 11.10 3 5 -25 46.30 9.10 3 5 -25 37.40 10.00 -2 -5 25 -0.40 8.50 2 -5 -25 13.80 8.20 2 5 -25 12.80 8.00 2 5 -25 31.40 10.70 -1 -5 25 6.00 9.60 1 -5 -25 33.00 8.60 1 5 -25 15.40 8.50 1 5 -25 30.10 9.80 0 -5 25 -6.70 8.20 0 -5 -25 -2.50 9.10 0 5 -25 18.60 8.90 0 5 -25 9.70 8.60 -1 5 -25 50.39 11.80 -1 5 -25 28.20 11.20 -3 -6 25 62.69 14.30 3 -6 -25 96.49 14.40 3 6 -25 75.79 13.70 3 6 -25 60.09 8.90 2 -6 -25 9.90 7.30 -2 -6 25 -7.60 10.10 2 6 -25 4.60 7.40 2 6 -25 12.40 10.00 1 -6 -25 73.99 11.60 -1 -6 25 42.70 13.10 1 6 -25 63.19 12.90 1 6 -25 73.89 11.40 0 -6 -25 28.00 7.50 0 6 -25 15.40 8.40 0 6 -25 6.70 10.10 -1 6 -25 5.70 9.60 -1 6 -25 8.50 8.10 -2 -7 25 -11.90 9.50 2 -7 -25 4.20 6.90 2 7 -25 1.70 5.70 2 7 -25 4.30 8.90 1 -7 -25 58.89 10.30 -1 -7 25 36.10 12.00 1 7 -25 50.79 9.10 1 7 -25 68.79 13.10 -5 0 26 32.10 9.20 5 0 -26 46.10 11.90 4 0 -26 -22.60 11.50 4 0 -26 20.30 9.50 -4 0 26 -0.10 7.50 3 0 -26 35.00 9.00 3 0 -26 -2.70 9.90 -3 0 26 14.30 8.60 2 0 -26 25.30 9.60 2 0 -26 -8.20 10.10 -2 0 26 -5.90 7.20 -1 0 26 -2.80 8.20 1 0 -26 -8.30 10.00 1 0 -26 16.00 9.00 0 0 -26 94.89 13.50 0 0 -26 53.59 14.20 0 0 26 73.69 14.10 1 0 26 231.58 23.80 -1 0 -26 252.07 19.30 -1 0 -26 175.98 20.40 -2 0 -26 516.75 26.00 2 0 26 495.65 29.60 -2 0 -26 476.95 35.20 -5 -1 26 75.49 12.70 5 -1 -26 48.70 14.30 5 1 -26 51.49 15.00 -4 -1 26 -4.90 7.70 4 -1 -26 30.90 11.60 -4 1 26 -5.10 6.90 4 1 -26 -15.40 13.20 4 1 -26 8.80 10.00 3 -1 -26 -10.60 9.00 -3 -1 26 10.30 8.70 3 -1 -26 28.00 10.10 -3 1 26 4.60 7.10 3 1 -26 -10.10 10.00 3 1 -26 13.50 8.60 2 -1 -26 4.60 10.10 -2 -1 26 7.20 8.80 2 1 -26 -2.60 10.60 -2 1 26 -0.30 7.20 1 -1 -26 52.29 13.50 -1 -1 26 55.09 12.60 1 1 -26 55.49 13.40 -1 1 26 58.39 10.80 1 1 -26 69.59 11.00 0 -1 26 154.48 19.30 0 -1 -26 222.58 17.50 0 -1 -26 164.18 18.00 0 1 -26 189.58 19.00 0 1 26 135.79 16.90 1 -1 26 194.18 23.00 -1 -1 -26 199.78 21.60 -1 -1 -26 240.58 19.10 1 1 26 220.38 21.40 -1 1 -26 226.48 20.20 -1 1 -26 222.88 28.40 2 -1 26 79.69 14.40 -2 -1 -26 120.99 16.90 -2 -1 -26 97.09 18.80 2 1 26 94.49 14.30 -2 1 -26 84.49 15.80 4 -2 -26 26.70 11.50 -4 -2 26 25.30 10.70 4 2 -26 59.59 15.80 4 2 -26 39.40 12.40 -3 -2 26 -1.50 8.60 3 -2 -26 30.20 10.90 3 -2 -26 -13.60 8.80 3 2 -26 2.80 11.00 -3 2 26 4.70 6.60 3 2 -26 26.30 10.60 -2 -2 26 21.00 11.00 2 -2 -26 34.70 8.30 2 2 -26 13.90 10.70 2 2 -26 35.70 9.70 -2 2 26 13.40 6.90 1 -2 -26 10.10 10.90 -1 -2 26 4.20 9.80 -1 2 26 24.80 8.40 1 2 -26 51.19 12.10 1 2 -26 14.90 11.20 0 -2 -26 -9.40 10.60 0 -2 26 4.60 10.60 0 2 26 18.50 8.60 0 2 -26 20.80 11.10 0 2 -26 20.60 9.90 1 -2 26 55.59 14.80 -1 2 -26 69.39 12.20 -4 -3 26 -1.30 8.60 4 -3 -26 -2.80 10.30 4 3 -26 8.20 10.70 -3 -3 26 287.17 22.80 3 -3 -26 284.07 20.70 3 3 -26 318.07 21.80 3 3 -26 313.07 24.60 2 -3 -26 3.30 7.00 -2 -3 26 -10.60 9.60 2 -3 -26 -12.50 8.30 -2 3 26 -0.40 6.20 2 3 -26 6.50 10.00 2 3 -26 12.60 8.70 -1 -3 26 10.80 11.10 -1 3 26 14.60 7.90 1 3 -26 18.80 10.60 1 3 -26 22.80 9.50 0 -3 26 9.80 11.90 0 3 26 5.00 7.30 0 3 -26 24.60 10.40 0 3 -26 28.50 12.50 1 -3 26 7.50 13.70 -1 -3 -26 25.90 8.80 1 3 26 -4.90 6.20 -1 3 -26 34.70 13.00 -1 3 -26 10.90 8.70 4 -4 -26 69.39 14.20 -4 -4 26 72.49 14.20 4 4 -26 79.49 13.90 -3 -4 26 3.80 10.80 3 -4 -26 1.00 8.80 3 4 -26 9.60 9.70 -2 -4 26 30.10 12.90 2 -4 -26 41.80 10.50 2 4 -26 18.40 9.30 2 4 -26 51.99 12.20 -1 -4 26 50.89 14.20 1 4 -26 73.09 13.00 1 4 -26 92.49 14.90 0 -4 26 21.10 14.20 0 4 -26 55.89 13.80 0 4 -26 39.10 11.70 1 -4 26 -8.20 9.20 1 4 26 -3.30 6.20 -1 4 -26 4.40 8.60 -1 4 -26 26.90 11.70 3 -5 -26 144.09 16.10 3 5 -26 159.18 17.10 3 5 -26 150.18 17.80 2 -5 -26 17.50 7.70 -2 -5 26 -6.00 11.00 2 5 -26 7.60 8.40 2 5 -26 4.40 8.60 1 -5 -26 17.10 6.90 -1 -5 26 8.10 12.80 1 5 -26 28.30 10.10 1 5 -26 22.10 9.80 0 -5 26 -7.70 11.90 0 5 -26 3.90 9.20 0 5 -26 21.20 10.20 3 0 -27 -10.00 14.50 3 0 -27 20.40 9.70 -3 0 27 -3.50 7.70 2 0 -27 21.70 9.00 2 0 -27 0.60 16.30 -2 0 27 2.50 10.20 1 0 -27 -3.70 16.20 -1 0 27 7.80 10.30 1 0 -27 22.90 8.40 0 0 -27 9.20 15.00 0 0 27 17.40 11.80 0 0 -27 24.50 9.40 3 -1 -27 22.10 11.00 -3 -1 27 14.90 10.80 3 1 -27 20.00 14.50 -3 1 27 15.00 8.60 3 1 -27 18.90 8.80 -2 -1 27 23.60 11.00 2 -1 -27 14.40 8.10 2 1 -27 33.10 16.40 2 1 -27 18.70 9.30 -1 -1 27 40.80 13.70 1 -1 -27 50.89 10.10 1 1 -27 71.99 12.20 1 1 -27 56.39 17.80 -1 1 27 40.30 10.90 0 -1 -27 159.08 20.70 0 -1 27 198.98 24.50 0 1 -27 194.08 19.30 0 1 -27 250.57 32.50 0 1 27 162.68 18.20 -3 -2 27 45.60 12.60 3 -2 -27 -0.10 12.70 3 -2 -27 68.29 13.70 3 2 -27 71.89 15.60 -3 2 27 30.20 9.40 2 -2 -27 155.18 16.20 -2 -2 27 124.59 17.00 2 2 -27 132.49 17.40 1 -2 -27 101.69 14.20 -1 -2 27 65.59 15.40 1 2 -27 68.29 13.40 1 2 -27 71.59 15.00 0 -2 27 200.38 23.20 0 -2 -27 162.88 21.00 0 2 27 167.58 16.70 0 2 -27 247.88 20.10 0 2 -27 251.27 26.70 2 -3 -27 49.10 9.80 -2 -3 27 40.50 13.30 2 3 -27 51.19 11.10 -2 3 27 29.40 9.30 2 3 -27 67.49 13.10 -1 -3 27 37.70 13.20 1 3 -27 38.10 11.90 1 3 -27 52.69 13.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 90263 _shelx_res_file ; TITL zl5032 in P2(1)/c shelx.res created by SHELXL-2018/3 at 14:49:25 on 04-Jul-2022 CELL 0.71073 8.9102 13.5595 22.0520 90.000 98.024 90.000 ZERR 4.00 0.0004 0.0007 0.0012 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 108 108 52 4 MERG 2 OMIT 0 0 2 OMIT 1 0 0 OMIT 2 1 9 SIMU 0.02 C4 > C9A EADP C4 C4A SADI C1 C4 C1 C4A C13 C16 EQIV $1 x-1, y, z HTAB N1 N5_$1 EQIV $2 x+1, y-1, z HTAB N3 N12_$2 HTAB N4 O1 EQIV $3 x+1, y, z HTAB N4 N11_$3 HTAB N4 N8_$3 HTAB N7 O1 HTAB N7 N11_$3 EQIV $4 x-1, y+1, z HTAB N9 N6_$4 HTAB N10 O1 HTAB N10 N5_$1 HTAB N10 N2_$1 EQIV $5 -x, -y+1, -z+1 HTAB C1 N11_$5 EQIV $6 -x, -y+2, -z+1 HTAB C13 N12_$6 FMAP 2 PLAN 5 SIZE 0.260 0.260 0.300 ACTA HTAB 2.00000 BOND $H CONF LIST 6 L.S. 13 TEMP -123.00 WGHT 0.040600 1.738000 FVAR 0.67205 0.67238 0.66244 O1 4 0.305494 0.599881 0.361403 11.00000 0.02233 0.04204 = 0.02548 -0.00198 0.00399 0.00134 N1 3 0.525743 0.428283 0.432929 11.00000 0.01421 0.02162 = 0.03105 -0.00149 0.00507 0.00160 AFIX 3 H1N 2 0.431602 0.454984 0.432599 11.00000 -1.20000 AFIX 0 N2 3 0.785714 0.453800 0.426543 11.00000 0.01443 0.01856 = 0.01832 -0.00118 0.00263 0.00081 N3 3 0.691168 0.293692 0.440160 11.00000 0.01670 0.01658 = 0.03102 0.00368 0.00273 0.00051 AFIX 3 H3N 2 0.703754 0.227992 0.443812 11.00000 -1.20000 AFIX 0 N4 3 0.618988 0.583803 0.424436 11.00000 0.01553 0.01953 = 0.03264 -0.00056 0.00155 0.00127 AFIX 3 H4A 2 0.524426 0.608445 0.416945 11.00000 -1.20000 H4B 2 0.696850 0.625464 0.422575 11.00000 -1.20000 AFIX 0 N5 3 1.191751 0.421917 0.436449 11.00000 0.01826 0.02610 = 0.03969 0.00084 0.00459 0.00091 N6 3 0.995502 0.129112 0.421913 11.00000 0.02914 0.02053 = 0.04094 -0.00114 0.00499 0.00157 N7 3 0.118624 0.774583 0.417602 11.00000 0.01368 0.02112 = 0.02722 0.00331 0.00398 0.00274 AFIX 3 H7N 2 0.210064 0.747167 0.414922 11.00000 -1.20000 AFIX 0 N8 3 -0.142615 0.749130 0.421227 11.00000 0.01609 0.01784 = 0.01911 0.00034 0.00323 0.00084 N9 3 -0.038483 0.909697 0.429202 11.00000 0.01950 0.01618 = 0.02431 -0.00010 0.00586 -0.00035 AFIX 3 H9N 2 -0.052583 0.976797 0.430802 11.00000 -1.20000 AFIX 0 N10 3 0.019963 0.618590 0.414531 11.00000 0.01905 0.01843 = 0.03238 0.00015 0.00918 0.00250 AFIX 3 H10A 2 0.110823 0.595869 0.407432 11.00000 -1.20000 H10B 2 -0.055088 0.577908 0.422065 11.00000 -1.20000 AFIX 0 N11 3 -0.539590 0.781210 0.432755 11.00000 0.02062 0.02502 = 0.04714 -0.00416 0.00753 0.00116 N12 3 -0.333071 1.072378 0.454729 11.00000 0.03074 0.02168 = 0.03854 -0.00350 0.01049 0.00106 N13 3 0.271782 0.595111 0.257186 11.00000 0.02422 0.02966 = 0.02537 -0.00006 0.00268 0.00198 C1 1 0.533784 0.322078 0.423611 11.00000 0.01660 0.02003 = 0.03113 0.00289 0.00522 -0.00106 AFIX 13 H1A 2 0.471224 0.288129 0.451612 11.00000 -1.20000 AFIX 0 C2 1 0.644067 0.487669 0.427912 11.00000 0.01703 0.02046 = 0.01540 -0.00142 0.00144 -0.00085 C3 1 0.806004 0.355214 0.432957 11.00000 0.01666 0.02005 = 0.01331 -0.00002 0.00099 -0.00173 PART 1 SAME C16 > C21 C4 1 0.475268 0.293214 0.357592 21.00000 0.01761 0.01860 = 0.03507 -0.00157 -0.00044 0.00253 C5 1 0.556344 0.317665 0.310113 21.00000 0.01949 0.02902 = 0.02352 -0.00019 -0.00329 -0.00116 AFIX 43 H5 2 0.650282 0.351418 0.318958 21.00000 -1.20000 AFIX 0 C6 1 0.501161 0.293164 0.249869 21.00000 0.02606 0.02930 = 0.03382 -0.00166 -0.00398 0.00064 AFIX 43 H6 2 0.557368 0.310779 0.217927 21.00000 -1.20000 AFIX 0 C7 1 0.364912 0.243281 0.236017 21.00000 0.02620 0.03483 = 0.03621 -0.00974 -0.00849 0.00143 AFIX 43 H7 2 0.327883 0.226416 0.194827 21.00000 -1.20000 AFIX 0 C8 1 0.283526 0.218337 0.282654 21.00000 0.02113 0.04288 = 0.05073 -0.01112 -0.00016 -0.00642 AFIX 43 H8 2 0.189913 0.184280 0.273567 21.00000 -1.20000 AFIX 0 C9 1 0.338602 0.243099 0.343237 21.00000 0.02284 0.03336 = 0.04281 -0.00525 0.00710 -0.00217 AFIX 43 H9 2 0.281954 0.225472 0.375038 21.00000 -1.20000 AFIX 0 PART 2 SAME C16 > C21 C4A 1 0.462875 0.289729 0.360784 -21.00000 0.01761 0.01860 = 0.03507 -0.00157 -0.00044 0.00253 C5A 1 0.524609 0.316543 0.309253 -21.00000 0.01971 0.03031 = 0.04899 -0.00425 -0.00889 -0.00627 AFIX 43 H5A 2 0.611348 0.358019 0.313107 -21.00000 -1.20000 AFIX 0 C6A 1 0.460720 0.283249 0.251404 -21.00000 0.03617 0.03776 = 0.03471 -0.00299 -0.00842 0.00086 AFIX 43 H6A 2 0.504516 0.299588 0.215823 -21.00000 -1.20000 AFIX 0 C7A 1 0.332899 0.226296 0.247716 -21.00000 0.02390 0.03595 = 0.04772 -0.00945 -0.00632 -0.00459 AFIX 43 H7A 2 0.286987 0.203583 0.208748 -21.00000 -1.20000 AFIX 0 C8A 1 0.269226 0.201095 0.298792 -21.00000 0.02603 0.03998 = 0.04890 -0.01222 -0.00344 -0.00044 AFIX 43 H8A 2 0.179205 0.162676 0.294487 -21.00000 -1.20000 AFIX 0 C9A 1 0.335050 0.231186 0.356790 -21.00000 0.01789 0.02683 = 0.04742 -0.00901 0.00357 -0.00337 AFIX 43 H9A 2 0.293473 0.212108 0.392413 -21.00000 -1.20000 AFIX 0 PART 0 C10 1 0.952642 0.315413 0.432286 11.00000 0.01774 0.01835 = 0.01874 -0.00043 0.00273 0.00059 C11 1 1.081728 0.376320 0.434625 11.00000 0.01811 0.01944 = 0.01953 0.00115 0.00326 0.00543 C12 1 0.976193 0.212424 0.427224 11.00000 0.01649 0.02341 = 0.02020 0.00127 0.00233 -0.00092 C13 1 0.101640 0.880248 0.407545 11.00000 0.01565 0.02138 = 0.02172 0.00135 0.00265 -0.00063 AFIX 13 H13A 2 0.187900 0.914501 0.432945 11.00000 -1.20000 AFIX 0 C14 1 -0.001739 0.715150 0.417383 11.00000 0.01734 0.02074 = 0.01520 0.00116 0.00209 -0.00017 C15 1 -0.155957 0.847473 0.429328 11.00000 0.01780 0.01952 = 0.01289 0.00090 0.00130 -0.00028 C16 1 0.103435 0.907868 0.340771 11.00000 0.02444 0.01838 = 0.02392 0.00145 0.00738 0.00417 C17 1 -0.019967 0.886096 0.296771 11.00000 0.03320 0.02906 = 0.02501 0.00064 0.00303 0.00207 AFIX 43 H17A 2 -0.106544 0.854486 0.308568 11.00000 -1.20000 AFIX 0 C18 1 -0.017173 0.910341 0.235725 11.00000 0.04779 0.03618 = 0.02263 0.00145 0.00280 0.01119 AFIX 43 H18A 2 -0.101889 0.895731 0.205920 11.00000 -1.20000 AFIX 0 C19 1 0.108594 0.955573 0.218518 11.00000 0.06160 0.03462 = 0.02656 0.00703 0.01815 0.01441 AFIX 43 H19A 2 0.110939 0.971849 0.176760 11.00000 -1.20000 AFIX 0 C20 1 0.230884 0.977227 0.261741 11.00000 0.04821 0.04045 = 0.04471 0.00814 0.02802 -0.00003 AFIX 43 H20A 2 0.317372 1.008472 0.249608 11.00000 -1.20000 AFIX 0 C21 1 0.229092 0.953697 0.323328 11.00000 0.03085 0.03617 = 0.03648 0.00375 0.01295 -0.00158 AFIX 43 H21A 2 0.313711 0.969113 0.352997 11.00000 -1.20000 AFIX 0 C22 1 -0.298930 0.886569 0.438179 11.00000 0.01895 0.01758 = 0.02159 -0.00057 0.00399 0.00073 C23 1 -0.428603 0.826372 0.435602 11.00000 0.01908 0.01887 = 0.02343 -0.00056 0.00427 0.00463 C24 1 -0.318972 0.988760 0.447569 11.00000 0.01750 0.02518 = 0.02023 0.00133 0.00480 0.00032 C25 1 0.338718 0.569688 0.312144 11.00000 0.02230 0.02972 = 0.02852 -0.00017 0.00240 0.00234 AFIX 43 H25A 2 0.419969 0.523933 0.313982 11.00000 -1.20000 AFIX 0 C26 1 0.146818 0.664180 0.249898 11.00000 0.03813 0.05157 = 0.04416 0.00999 0.00349 0.01624 AFIX 127 H26A 2 0.109491 0.673180 0.289282 31.00000 -1.50000 H26B 2 0.064973 0.638462 0.219737 31.00000 -1.50000 H26C 2 0.181335 0.727686 0.235740 31.00000 -1.50000 H26D 2 0.127708 0.686372 0.207224 -31.00000 -1.50000 H26E 2 0.172226 0.721090 0.276769 -31.00000 -1.50000 H26F 2 0.055864 0.631866 0.260765 -31.00000 -1.50000 AFIX 0 C27 1 0.322200 0.557314 0.201441 11.00000 0.04194 0.04146 = 0.02730 -0.00512 0.00617 -0.00097 AFIX 137 H27A 2 0.397900 0.505441 0.212058 11.00000 -1.50000 H27B 2 0.367225 0.611049 0.180343 11.00000 -1.50000 H27C 2 0.235333 0.530070 0.174488 11.00000 -1.50000 AFIX 0 HKLF 4 REM zl5032 in P2(1)/c REM wR2 = 0.1107, GooF = S = 1.021, Restrained GooF = 1.002 for all data REM R1 = 0.0453 for 4215 Fo > 4sig(Fo) and 0.0639 for all 5368 data REM 422 parameters refined using 219 restraints END WGHT 0.0406 1.7380 REM Instructions for potential hydrogen bonds HTAB N1 N5_$1 HTAB N3 N12_$2 HTAB N4 O1 HTAB N4 N11_$3 HTAB N4 N8_$3 HTAB N7 O1 HTAB N7 N11_$3 HTAB N9 N6_$4 HTAB N10 O1 HTAB N10 N5_$1 HTAB N10 N2_$1 HTAB C13 N12_$6 REM Highest difference peak 0.243, deepest hole -0.233, 1-sigma level 0.046 Q1 1 0.0975 0.8937 0.3717 11.00000 0.05 0.24 Q2 1 -0.2367 0.7248 0.4127 11.00000 0.05 0.20 Q3 1 0.7065 0.3014 0.3993 11.00000 0.05 0.20 Q4 1 0.8784 0.3358 0.4226 11.00000 0.05 0.19 Q5 1 0.5321 0.3752 0.4188 11.00000 0.05 0.19 ; _shelx_res_checksum 6903 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 O O1 0.30549(14) 0.59988(10) 0.36140(6) 0.0299(3) Uani d 1 . . N N1 0.52574(16) 0.42828(11) 0.43293(7) 0.0221(3) Uani d 1 . . H H1N 0.431602 0.454984 0.432599 0.027 Uiso d 1 . . N N2 0.78571(15) 0.45380(10) 0.42654(6) 0.0171(3) Uani d 1 . . N N3 0.69117(16) 0.29369(11) 0.44016(7) 0.0215(3) Uani d 1 . . H H3N 0.703754 0.227992 0.443812 0.026 Uiso d 1 . . N N4 0.61899(16) 0.58380(11) 0.42444(7) 0.0227(3) Uani d 1 . . H H4A 0.524426 0.608445 0.416945 0.027 Uiso d 1 . . H H4B 0.696850 0.625464 0.422575 0.027 Uiso d 1 . . N N5 1.19175(17) 0.42192(12) 0.43645(8) 0.0280(4) Uani d 1 . . N N6 0.99550(18) 0.12911(12) 0.42191(8) 0.0302(4) Uani d 1 . . N N7 0.11862(16) 0.77458(11) 0.41760(7) 0.0206(3) Uani d 1 . . H H7N 0.210064 0.747167 0.414922 0.025 Uiso d 1 . . N N8 -0.14262(15) 0.74913(10) 0.42123(6) 0.0176(3) Uani d 1 . . N N9 -0.03848(16) 0.90970(10) 0.42920(7) 0.0197(3) Uani d 1 . . H H9N -0.052583 0.976797 0.430802 0.024 Uiso d 1 . . N N10 0.01996(17) 0.61859(11) 0.41453(7) 0.0228(3) Uani d 1 . . H H10A 0.110823 0.595869 0.407432 0.027 Uiso d 1 . . H H10B -0.055088 0.577908 0.422065 0.027 Uiso d 1 . . N N11 -0.53959(18) 0.78121(12) 0.43275(8) 0.0307(4) Uani d 1 . . N N12 -0.33307(19) 1.07238(11) 0.45473(8) 0.0298(4) Uani d 1 . . N N13 0.27178(17) 0.59511(12) 0.25719(7) 0.0265(3) Uani d 1 . . C C1 0.53378(19) 0.32208(13) 0.42361(8) 0.0224(4) Uani d 1 . . H H1A 0.471224 0.288129 0.451612 0.027 Uiso calc 1 A 1 C C2 0.64407(18) 0.48767(12) 0.42791(7) 0.0177(3) Uani d 1 . . C C3 0.80600(18) 0.35521(12) 0.43296(7) 0.0168(3) Uani d 1 . . C C4 0.475(3) 0.293(2) 0.3576(4) 0.0241(10) Uani d 0.67(3) B 1 C C5 0.5563(13) 0.3177(10) 0.3101(4) 0.0246(14) Uani d 0.67(3) B 1 H H5 0.650282 0.351418 0.318958 0.030 Uiso calc 0.67(3) B 1 C C6 0.5012(13) 0.2932(9) 0.2499(4) 0.0305(15) Uani d 0.67(3) B 1 H H6 0.557368 0.310779 0.217927 0.037 Uiso calc 0.67(3) B 1 C C7 0.3649(13) 0.2433(8) 0.2360(5) 0.0336(18) Uani d 0.67(3) B 1 H H7 0.327883 0.226416 0.194827 0.040 Uiso calc 0.67(3) B 1 C C8 0.2835(11) 0.2183(9) 0.2827(6) 0.0387(19) Uani d 0.67(3) B 1 H H8 0.189913 0.184280 0.273567 0.046 Uiso calc 0.67(3) B 1 C C9 0.3386(15) 0.2431(11) 0.3432(5) 0.0328(18) Uani d 0.67(3) B 1 H H9 0.281954 0.225472 0.375038 0.039 Uiso calc 0.67(3) B 1 C C4A 0.463(6) 0.290(5) 0.3608(8) 0.0241(10) Uani d 0.33(3) B 2 C C5A 0.525(3) 0.317(2) 0.3093(10) 0.034(4) Uani d 0.33(3) B 2 H H5A 0.611348 0.358019 0.313107 0.041 Uiso calc 0.33(3) B 2 C C6A 0.461(3) 0.2832(19) 0.2514(9) 0.037(3) Uani d 0.33(3) B 2 H H6A 0.504516 0.299588 0.215823 0.045 Uiso calc 0.33(3) B 2 C C7A 0.333(3) 0.2263(16) 0.2477(10) 0.037(3) Uani d 0.33(3) B 2 H H7A 0.286987 0.203583 0.208748 0.044 Uiso calc 0.33(3) B 2 C C8A 0.269(2) 0.2011(17) 0.2988(11) 0.039(3) Uani d 0.33(3) B 2 H H8A 0.179205 0.162676 0.294487 0.047 Uiso calc 0.33(3) B 2 C C9A 0.335(3) 0.231(2) 0.3568(10) 0.031(3) Uani d 0.33(3) B 2 H H9A 0.293473 0.212108 0.392413 0.037 Uiso calc 0.33(3) B 2 C C10 0.95264(19) 0.31541(12) 0.43229(8) 0.0183(3) Uani d 1 . . C C11 1.08173(19) 0.37632(12) 0.43463(8) 0.0190(4) Uani d 1 . . C C12 0.97619(19) 0.21242(13) 0.42722(8) 0.0201(4) Uani d 1 . . C C13 0.10164(19) 0.88025(13) 0.40755(8) 0.0196(4) Uani d 1 . . H H13A 0.187900 0.914501 0.432945 0.023 Uiso calc 1 . . C C14 -0.00174(18) 0.71515(12) 0.41738(7) 0.0178(3) Uani d 1 . . C C15 -0.15596(18) 0.84747(12) 0.42933(7) 0.0168(3) Uani d 1 . . C C16 0.1034(2) 0.90787(13) 0.34077(8) 0.0219(4) Uani d 1 . . C C17 -0.0200(2) 0.88610(15) 0.29677(8) 0.0292(4) Uani d 1 . . H H17A -0.106544 0.854486 0.308568 0.035 Uiso calc 1 . . C C18 -0.0172(3) 0.91034(16) 0.23572(9) 0.0357(5) Uani d 1 . . H H18A -0.101889 0.895731 0.205920 0.043 Uiso calc 1 . . C C19 0.1086(3) 0.95557(16) 0.21852(10) 0.0398(5) Uani d 1 . . H H19A 0.110939 0.971849 0.176760 0.048 Uiso calc 1 . . C C20 0.2309(3) 0.97723(17) 0.26174(11) 0.0424(6) Uani d 1 . . H H20A 0.317372 1.008472 0.249608 0.051 Uiso calc 1 . . C C21 0.2291(2) 0.95370(15) 0.32333(10) 0.0337(5) Uani d 1 . . H H21A 0.313711 0.969113 0.352997 0.040 Uiso calc 1 . . C C22 -0.29893(19) 0.88657(12) 0.43818(8) 0.0193(3) Uani d 1 . . C C23 -0.42860(19) 0.82637(13) 0.43560(8) 0.0203(4) Uani d 1 . . C C24 -0.31897(19) 0.98876(13) 0.44757(8) 0.0208(4) Uani d 1 . . C C25 0.3387(2) 0.56969(14) 0.31214(9) 0.0270(4) Uani d 1 . . H H25A 0.419969 0.523933 0.313982 0.032 Uiso calc 1 . . C C26 0.1468(3) 0.66418(18) 0.24990(11) 0.0448(6) Uani d 1 . . H H26A 0.109491 0.673180 0.289282 0.067 Uiso calc 0.66(3) . . H H26B 0.064973 0.638462 0.219737 0.067 Uiso calc 0.66(3) . . H H26C 0.181335 0.727686 0.235740 0.067 Uiso calc 0.66(3) . . H H26D 0.127708 0.686372 0.207224 0.067 Uiso calc 0.34(3) . . H H26E 0.172226 0.721090 0.276769 0.067 Uiso calc 0.34(3) . . H H26F 0.055864 0.631866 0.260765 0.067 Uiso calc 0.34(3) . . C C27 0.3222(3) 0.55731(17) 0.20144(9) 0.0368(5) Uani d 1 . . H H27A 0.397900 0.505441 0.212058 0.055 Uiso calc 1 . . H H27B 0.367225 0.611049 0.180343 0.055 Uiso calc 1 . . H H27C 0.235333 0.530070 0.174488 0.055 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 0.0223(7) 0.0420(8) 0.0255(7) 0.0013(6) 0.0040(5) -0.0020(6) N1 0.0142(7) 0.0216(8) 0.0311(8) 0.0016(6) 0.0051(6) -0.0015(6) N2 0.0144(7) 0.0186(7) 0.0183(7) 0.0008(5) 0.0026(5) -0.0012(6) N3 0.0167(7) 0.0166(7) 0.0310(8) 0.0005(6) 0.0027(6) 0.0037(6) N4 0.0155(7) 0.0195(7) 0.0326(8) 0.0013(6) 0.0015(6) -0.0006(6) N5 0.0183(8) 0.0261(8) 0.0397(9) 0.0009(7) 0.0046(7) 0.0008(7) N6 0.0291(9) 0.0205(9) 0.0409(10) 0.0016(7) 0.0050(7) -0.0011(7) N7 0.0137(7) 0.0211(7) 0.0272(8) 0.0027(6) 0.0040(6) 0.0033(6) N8 0.0161(7) 0.0178(7) 0.0191(7) 0.0008(6) 0.0032(5) 0.0003(6) N9 0.0195(7) 0.0162(7) 0.0243(7) -0.0003(6) 0.0059(6) -0.0001(6) N10 0.0190(7) 0.0184(7) 0.0324(8) 0.0025(6) 0.0092(6) 0.0001(6) N11 0.0206(8) 0.0250(8) 0.0471(10) 0.0012(7) 0.0075(7) -0.0042(7) N12 0.0307(9) 0.0217(9) 0.0385(10) 0.0011(7) 0.0105(7) -0.0035(7) N13 0.0242(8) 0.0297(9) 0.0254(8) 0.0020(7) 0.0027(6) -0.0001(7) C1 0.0166(8) 0.0200(9) 0.0311(10) -0.0011(7) 0.0052(7) 0.0029(7) C2 0.0170(8) 0.0205(9) 0.0154(8) -0.0008(7) 0.0014(6) -0.0014(6) C3 0.0167(8) 0.0201(8) 0.0133(8) -0.0017(6) 0.0010(6) 0.0000(6) C4 0.018(4) 0.019(2) 0.0351(13) 0.003(2) -0.0004(14) -0.0016(19) C5 0.019(3) 0.029(2) 0.024(2) -0.001(3) -0.0033(18) -0.0002(17) C6 0.026(4) 0.029(3) 0.034(2) 0.001(2) -0.004(2) -0.0017(17) C7 0.026(4) 0.035(3) 0.036(3) 0.001(3) -0.008(3) -0.010(2) C8 0.021(3) 0.043(4) 0.051(5) -0.006(2) 0.000(3) -0.011(3) C9 0.023(2) 0.033(4) 0.043(3) -0.002(2) 0.007(3) -0.005(3) C4A 0.018(4) 0.019(2) 0.0351(13) 0.003(2) -0.0004(14) -0.0016(19) C5A 0.020(7) 0.030(5) 0.049(6) -0.006(5) -0.009(4) -0.004(4) C6A 0.036(8) 0.038(6) 0.035(5) 0.001(6) -0.008(5) -0.003(4) C7A 0.024(7) 0.036(6) 0.048(7) -0.005(5) -0.006(5) -0.009(5) C8A 0.026(5) 0.040(7) 0.049(7) 0.000(4) -0.003(5) -0.012(5) C9A 0.018(4) 0.027(6) 0.047(6) -0.003(4) 0.004(5) -0.009(6) C10 0.0177(8) 0.0184(8) 0.0187(8) 0.0006(7) 0.0027(6) -0.0004(6) C11 0.0181(8) 0.0194(8) 0.0195(8) 0.0054(7) 0.0033(6) 0.0011(7) C12 0.0165(8) 0.0234(10) 0.0202(9) -0.0009(7) 0.0023(7) 0.0013(7) C13 0.0156(8) 0.0214(9) 0.0217(9) -0.0006(7) 0.0027(6) 0.0014(7) C14 0.0173(8) 0.0207(8) 0.0152(8) -0.0002(7) 0.0021(6) 0.0012(6) C15 0.0178(8) 0.0195(8) 0.0129(8) -0.0003(7) 0.0013(6) 0.0009(6) C16 0.0244(9) 0.0184(9) 0.0239(9) 0.0042(7) 0.0074(7) 0.0014(7) C17 0.0332(10) 0.0291(10) 0.0250(9) 0.0021(8) 0.0030(8) 0.0006(8) C18 0.0478(13) 0.0362(11) 0.0226(10) 0.0112(10) 0.0028(9) 0.0014(8) C19 0.0616(15) 0.0346(12) 0.0266(11) 0.0144(11) 0.0181(10) 0.0070(9) C20 0.0482(14) 0.0404(13) 0.0447(13) 0.0000(11) 0.0280(11) 0.0081(10) C21 0.0309(11) 0.0362(11) 0.0365(11) -0.0016(9) 0.0129(9) 0.0037(9) C22 0.0190(8) 0.0176(8) 0.0216(8) 0.0007(7) 0.0040(7) -0.0006(7) C23 0.0191(9) 0.0189(9) 0.0234(9) 0.0046(7) 0.0043(7) -0.0006(7) C24 0.0175(8) 0.0252(10) 0.0202(9) 0.0003(7) 0.0048(7) 0.0013(7) C25 0.0223(9) 0.0297(10) 0.0285(10) 0.0023(8) 0.0024(8) -0.0002(8) C26 0.0381(12) 0.0516(14) 0.0442(13) 0.0162(11) 0.0035(10) 0.0100(11) C27 0.0419(12) 0.0415(12) 0.0273(10) -0.0010(10) 0.0062(9) -0.0051(9) 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' 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 N1 C1 . . 121.73(14) ? C2 N1 H1N . . 119.5 ? C1 N1 H1N . . 117.0 ? C2 N2 C3 . . 116.49(14) ? C3 N3 C1 . . 121.98(14) ? C3 N3 H3N . . 122.4 ? C1 N3 H3N . . 112.9 ? C2 N4 H4A . . 121.5 ? C2 N4 H4B . . 119.7 ? H4A N4 H4B . . 117.8 ? C14 N7 C13 . . 121.69(14) ? C14 N7 H7N . . 118.7 ? C13 N7 H7N . . 118.0 ? C14 N8 C15 . . 116.36(14) ? C15 N9 C13 . . 122.20(14) ? C15 N9 H9N . . 120.7 ? C13 N9 H9N . . 114.4 ? C14 N10 H10A . . 119.1 ? C14 N10 H10B . . 118.6 ? H10A N10 H10B . . 122.1 ? C25 N13 C26 . . 120.88(17) ? C25 N13 C27 . . 121.94(17) ? C26 N13 C27 . . 117.16(17) ? N3 C1 N1 . . 106.94(14) ? N3 C1 C4A . . 115(3) ? N1 C1 C4A . . 113(3) ? N3 C1 C4 . . 111.2(12) ? N1 C1 C4 . . 111.7(14) ? N3 C1 H1A . . 109.0 ? N1 C1 H1A . . 109.0 ? C4 C1 H1A . . 109.0 ? N4 C2 N1 . . 117.85(15) ? N4 C2 N2 . . 119.06(15) ? N1 C2 N2 . . 123.09(15) ? N3 C3 N2 . . 122.10(15) ? N3 C3 C10 . . 118.86(15) ? N2 C3 C10 . . 119.04(15) ? C9 C4 C5 . . 118.3(6) ? C9 C4 C1 . . 120.9(8) ? C5 C4 C1 . . 120.8(7) ? C6 C5 C4 . . 120.7(6) ? C6 C5 H5 . . 119.7 ? C4 C5 H5 . . 119.7 ? C7 C6 C5 . . 120.6(7) ? C7 C6 H6 . . 119.7 ? C5 C6 H6 . . 119.7 ? C8 C7 C6 . . 119.4(6) ? C8 C7 H7 . . 120.3 ? C6 C7 H7 . . 120.3 ? C7 C8 C9 . . 120.1(6) ? C7 C8 H8 . . 119.9 ? C9 C8 H8 . . 119.9 ? C4 C9 C8 . . 120.9(7) ? C4 C9 H9 . . 119.5 ? C8 C9 H9 . . 119.5 ? C5A C4A C9A . . 121.3(12) ? C5A C4A C1 . . 121.1(17) ? C9A C4A C1 . . 117.6(16) ? C4A C5A C6A . . 120.6(14) ? C4A C5A H5A . . 119.7 ? C6A C5A H5A . . 119.7 ? C7A C6A C5A . . 117.8(13) ? C7A C6A H6A . . 121.1 ? C5A C6A H6A . . 121.1 ? C6A C7A C8A . . 121.8(13) ? C6A C7A H7A . . 119.1 ? C8A C7A H7A . . 119.1 ? C7A C8A C9A . . 120.8(13) ? C7A C8A H8A . . 119.6 ? C9A C8A H8A . . 119.6 ? C4A C9A C8A . . 117.7(13) ? C4A C9A H9A . . 121.1 ? C8A C9A H9A . . 121.1 ? C11 C10 C3 . . 121.69(15) ? C11 C10 C12 . . 116.75(15) ? C3 C10 C12 . . 121.53(15) ? N5 C11 C10 . . 176.54(18) ? N6 C12 C10 . . 178.65(19) ? N9 C13 N7 . . 107.24(13) ? N9 C13 C16 . . 112.08(14) ? N7 C13 C16 . . 112.03(14) ? N9 C13 H13A . . 108.5 ? N7 C13 H13A . . 108.5 ? C16 C13 H13A . . 108.5 ? N10 C14 N7 . . 118.14(15) ? N10 C14 N8 . . 118.86(15) ? N7 C14 N8 . . 122.99(15) ? N9 C15 N8 . . 122.37(15) ? N9 C15 C22 . . 118.69(15) ? N8 C15 C22 . . 118.93(15) ? C21 C16 C17 . . 119.55(17) ? C21 C16 C13 . . 119.91(17) ? C17 C16 C13 . . 120.54(16) ? C18 C17 C16 . . 120.38(19) ? C18 C17 H17A . . 119.8 ? C16 C17 H17A . . 119.8 ? C19 C18 C17 . . 119.9(2) ? C19 C18 H18A . . 120.1 ? C17 C18 H18A . . 120.1 ? C20 C19 C18 . . 120.05(19) ? C20 C19 H19A . . 120.0 ? C18 C19 H19A . . 120.0 ? C19 C20 C21 . . 120.6(2) ? C19 C20 H20A . . 119.7 ? C21 C20 H20A . . 119.7 ? C16 C21 C20 . . 119.5(2) ? C16 C21 H21A . . 120.2 ? C20 C21 H21A . . 120.2 ? C23 C22 C24 . . 116.95(15) ? C23 C22 C15 . . 121.67(15) ? C24 C22 C15 . . 121.33(15) ? N11 C23 C22 . . 176.48(19) ? N12 C24 C22 . . 178.8(2) ? O1 C25 N13 . . 126.02(18) ? O1 C25 H25A . . 117.0 ? N13 C25 H25A . . 117.0 ? N13 C26 H26A . . 109.5 ? N13 C26 H26B . . 109.5 ? H26A C26 H26B . . 109.5 ? N13 C26 H26C . . 109.5 ? H26A C26 H26C . . 109.5 ? H26B C26 H26C . . 109.5 ? N13 C26 H26D . . 109.5 ? H26A C26 H26D . . 141.1 ? H26B C26 H26D . . 56.3 ? H26C C26 H26D . . 56.3 ? N13 C26 H26E . . 109.5 ? H26A C26 H26E . . 56.3 ? H26B C26 H26E . . 141.1 ? H26C C26 H26E . . 56.3 ? H26D C26 H26E . . 109.5 ? N13 C26 H26F . . 109.5 ? H26A C26 H26F . . 56.3 ? H26B C26 H26F . . 56.3 ? H26C C26 H26F . . 141.1 ? H26D C26 H26F . . 109.5 ? H26E C26 H26F . . 109.5 ? N13 C27 H27A . . 109.5 ? N13 C27 H27B . . 109.5 ? H27A C27 H27B . . 109.5 ? N13 C27 H27C . . 109.5 ? H27A C27 H27C . . 109.5 ? H27B C27 H27C . . 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 C25 . 1.235(2) ? N1 C2 . 1.343(2) ? N1 C1 . 1.458(2) ? N1 H1N . 0.9127 ? N2 C2 . 1.347(2) ? N2 C3 . 1.354(2) ? N3 C3 . 1.347(2) ? N3 C1 . 1.451(2) ? N3 H3N . 0.9001 ? N4 C2 . 1.323(2) ? N4 H4A . 0.9000 ? N4 H4B . 0.9000 ? N5 C11 . 1.155(2) ? N6 C12 . 1.151(2) ? N7 C14 . 1.341(2) ? N7 C13 . 1.454(2) ? N7 H7N . 0.9050 ? N8 C14 . 1.351(2) ? N8 C15 . 1.353(2) ? N9 C15 . 1.345(2) ? N9 C13 . 1.454(2) ? N9 H9N . 0.9198 ? N10 C14 . 1.326(2) ? N10 H10A . 0.9001 ? N10 H10B . 0.9000 ? N11 C23 . 1.157(2) ? N12 C24 . 1.154(2) ? N13 C25 . 1.320(2) ? N13 C26 . 1.447(3) ? N13 C27 . 1.459(2) ? C1 C4A . 1.506(12) ? C1 C4 . 1.527(6) ? C1 H1A . 1.0000 ? C3 C10 . 1.416(2) ? C4 C9 . 1.392(7) ? C4 C5 . 1.393(7) ? C5 C6 . 1.391(7) ? C5 H5 . 0.9500 ? C6 C7 . 1.386(7) ? C6 H6 . 0.9500 ? C7 C8 . 1.381(7) ? C7 H7 . 0.9500 ? C8 C9 . 1.398(7) ? C8 H8 . 0.9500 ? C9 H9 . 0.9500 ? C4A C5A . 1.379(13) ? C4A C9A . 1.381(13) ? C5A C6A . 1.397(13) ? C5A H5A . 0.9500 ? C6A C7A . 1.369(12) ? C6A H6A . 0.9500 ? C7A C8A . 1.373(12) ? C7A H7A . 0.9500 ? C8A C9A . 1.392(13) ? C8A H8A . 0.9500 ? C9A H9A . 0.9500 ? C10 C11 . 1.411(2) ? C10 C12 . 1.419(2) ? C13 C16 . 1.522(2) ? C13 H13A . 1.0000 ? C15 C22 . 1.418(2) ? C16 C21 . 1.381(3) ? C16 C17 . 1.393(3) ? C17 C18 . 1.389(3) ? C17 H17A . 0.9500 ? C18 C19 . 1.376(3) ? C18 H18A . 0.9500 ? C19 C20 . 1.376(3) ? C19 H19A . 0.9500 ? C20 C21 . 1.397(3) ? C20 H20A . 0.9500 ? C21 H21A . 0.9500 ? C22 C23 . 1.409(2) ? C22 C24 . 1.416(2) ? C25 H25A . 0.9500 ? C26 H26A . 0.9800 ? C26 H26B . 0.9800 ? C26 H26C . 0.9800 ? C26 H26D . 0.9800 ? C26 H26E . 0.9800 ? C26 H26F . 0.9800 ? C27 H27A . 0.9800 ? C27 H27B . 0.9800 ? C27 H27C . 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 N1 H1N N5 1_455 0.91 2.20 2.989(2) 144.8 yes N3 H3N N12 1_645 0.90 2.15 3.029(2) 163.8 yes N4 H4A O1 . 0.90 2.16 2.9493(19) 146.5 yes N4 H4A N11 1_655 0.90 2.45 3.044(2) 124.1 yes N4 H4B N8 1_655 0.90 2.21 3.096(2) 169.3 yes N7 H7N O1 . 0.90 2.53 3.240(2) 136.0 yes N7 H7N N11 1_655 0.90 2.26 3.018(2) 141.4 yes N9 H9N N6 1_465 0.92 2.12 2.997(2) 158.1 yes N10 H10A O1 . 0.90 2.13 2.9566(19) 152.4 yes N10 H10A N5 1_455 0.90 2.52 3.079(2) 120.5 yes N10 H10B N2 1_455 0.90 2.21 3.094(2) 166.4 yes C1 H1A N11 3_566 1.00 2.71 3.457(3) 132.1 yes C13 H13A N12 3_576 1.00 2.64 3.484(2) 142.7 yes C27 H27B Cg2 2_655 0.98 2.85 3.664(7) 141 yes C27 H27B Cg3 2_655 0.98 2.88 3.707(14) 143 no C26 H26E Cg5 1_555 0.98 2.92 3.714(3) 139 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 C3 N3 C1 N1 . . . . -30.9(2) ? C3 N3 C1 C4A . . . . 96(2) ? C3 N3 C1 C4 . . . . 91.4(10) ? C2 N1 C1 N3 . . . . 28.4(2) ? C2 N1 C1 C4A . . . . -99.2(16) ? C2 N1 C1 C4 . . . . -93.5(8) ? C1 N1 C2 N4 . . . . 166.32(16) ? C1 N1 C2 N2 . . . . -14.0(3) ? C3 N2 C2 N4 . . . . 177.19(15) ? C3 N2 C2 N1 . . . . -2.5(2) ? C1 N3 C3 N2 . . . . 18.8(2) ? C1 N3 C3 C10 . . . . -161.37(16) ? C2 N2 C3 N3 . . . . 0.2(2) ? C2 N2 C3 C10 . . . . -179.59(14) ? N3 C1 C4 C9 . . . . 131(2) ? N1 C1 C4 C9 . . . . -109(3) ? N3 C1 C4 C5 . . . . -50(3) ? N1 C1 C4 C5 . . . . 70(3) ? C9 C4 C5 C6 . . . . 0(4) ? C1 C4 C5 C6 . . . . -178.6(19) ? C4 C5 C6 C7 . . . . 0(2) ? C5 C6 C7 C8 . . . . 0.3(14) ? C6 C7 C8 C9 . . . . -0.1(14) ? C5 C4 C9 C8 . . . . 0(4) ? C1 C4 C9 C8 . . . . 178.7(19) ? C7 C8 C9 C4 . . . . 0(2) ? N3 C1 C4A C5A . . . . -57(7) ? N1 C1 C4A C5A . . . . 66(6) ? N3 C1 C4A C9A . . . . 122(5) ? N1 C1 C4A C9A . . . . -115(5) ? C9A C4A C5A C6A . . . . -1(8) ? C1 C4A C5A C6A . . . . 178(4) ? C4A C5A C6A C7A . . . . 2(5) ? C5A C6A C7A C8A . . . . -1(3) ? C6A C7A C8A C9A . . . . -1(3) ? C5A C4A C9A C8A . . . . -1(8) ? C1 C4A C9A C8A . . . . -180(4) ? C7A C8A C9A C4A . . . . 2(5) ? N3 C3 C10 C11 . . . . -169.86(15) ? N2 C3 C10 C11 . . . . 9.9(2) ? N3 C3 C10 C12 . . . . 12.2(2) ? N2 C3 C10 C12 . . . . -167.99(15) ? C15 N9 C13 N7 . . . . -28.3(2) ? C15 N9 C13 C16 . . . . 95.08(18) ? C14 N7 C13 N9 . . . . 28.7(2) ? C14 N7 C13 C16 . . . . -94.64(19) ? C13 N7 C14 N10 . . . . 166.71(15) ? C13 N7 C14 N8 . . . . -14.7(2) ? C15 N8 C14 N10 . . . . 174.49(15) ? C15 N8 C14 N7 . . . . -4.1(2) ? C13 N9 C15 N8 . . . . 13.6(2) ? C13 N9 C15 C22 . . . . -166.34(15) ? C14 N8 C15 N9 . . . . 4.7(2) ? C14 N8 C15 C22 . . . . -175.44(14) ? N9 C13 C16 C21 . . . . 132.95(17) ? N7 C13 C16 C21 . . . . -106.44(19) ? N9 C13 C16 C17 . . . . -47.9(2) ? N7 C13 C16 C17 . . . . 72.7(2) ? C21 C16 C17 C18 . . . . -0.1(3) ? C13 C16 C17 C18 . . . . -179.21(17) ? C16 C17 C18 C19 . . . . 0.4(3) ? C17 C18 C19 C20 . . . . -0.4(3) ? C18 C19 C20 C21 . . . . 0.0(3) ? C17 C16 C21 C20 . . . . -0.2(3) ? C13 C16 C21 C20 . . . . 178.87(18) ? C19 C20 C21 C16 . . . . 0.3(3) ? N9 C15 C22 C23 . . . . 176.58(15) ? N8 C15 C22 C23 . . . . -3.3(2) ? N9 C15 C22 C24 . . . . -0.8(2) ? N8 C15 C22 C24 . . . . 179.27(15) ? C26 N13 C25 O1 . . . . -0.1(3) ? C27 N13 C25 O1 . . . . 178.26(19) ? _cod_database_fobs_code 2244129