#------------------------------------------------------------------------------ #$Date: 2025-06-26 03:31:50 +0100 (Thu, 26 Jun 2025) $ #$Revision: 300210 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023521.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_2023521 loop_ _publ_author_name 'El Moutaouakil Ala Allah, Abderrazzak' 'Kariuki, Benson M.' 'Al-Sulami, Ahlam I.' 'Basha, Maram T.' 'Allehyani, Basmah H.' 'Alsubari, Abdulsalam' 'Mague, Joel T.' 'Ramli, Youssef' _publ_section_title ; Synthesis, crystal structure and Hirshfeld surface analysis of 2-azido-N-(2,6-dimethylphenyl)acetamide ; _journal_coeditor_code ZN2043 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989025004530 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac 'C10 H12 N4 O' _chemical_formula_moiety 'C10 H12 N4 O' _chemical_formula_sum 'C10 H12 N4 O' _chemical_formula_weight 204.24 _chemical_name_systematic ; 2-Azido-N-(2,6-dimethylphenyl)acetamide ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 93.584(6) _cell_angle_beta 90.385(5) _cell_angle_gamma 99.905(5) _cell_formula_units_Z 4 _cell_length_a 4.8530(3) _cell_length_b 7.3504(5) _cell_length_c 29.862(3) _cell_measurement_reflns_used 2419 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 72.6110 _cell_measurement_theta_min 5.9210 _cell_volume 1047.13(14) _computing_cell_refinement ; CrysAlisPro 1.171.43.90 (Rigaku OD, 2023) ; _computing_data_collection ; CrysAlisPro CCD 43.120a (Rigaku OD, 2024) ; _computing_data_reduction ; CrysAlisPro 1.171.43.90 (Rigaku OD, 2023) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2019/2 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 10.5082 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.965 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_unetI/netI 0.0627 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 4441 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.685 _diffrn_reflns_theta_min 4.451 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.24455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2023) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.295 _exptl_crystal_description plate _exptl_crystal_F_000 432 _exptl_crystal_size_max 0.810 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.262 _refine_diff_density_min -0.281 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 284 _refine_ls_number_reflns 4441 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0757 _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^)+(0.1273P)^2^+0.4349P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2208 _refine_ls_wR_factor_ref 0.2441 _reflns_number_gt 2956 _reflns_number_total 4441 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zn2043.cif _cod_data_source_block I _cod_original_cell_volume 1047.14(13) _cod_database_code 2023521 _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 0.591 _shelx_estimated_absorpt_t_max 0.972 _shelx_hkl_file ; 0 0 -3 23.0031 102.322 -2 0 0 -3 23.0031 102.322 1 0 0 -4 161618. 10804.4 -2 0 0 -4 161618. 10804.4 1 0 0 -5 166.739 170.995 -2 0 0 -5 166.739 170.995 1 0 0 -6 397605. 12864.6 -2 0 0 -6 397605. 12864.6 1 0 0 -7 94.2244 229.443 -2 0 0 -7 94.2244 229.443 1 0 0 -8 151.466 449.495 -2 0 0 -8 151.466 449.495 1 0 0 -9 70.2505 455.620 -2 0 0 -9 70.2505 455.620 1 0 0 -10 999999. 4515.74 -2 0 0 -10 999999. 4515.74 1 0 0 -11 105.764 416.073 -2 0 0 -11 105.764 416.073 1 0 0 -12 244933. 2551.54 -2 0 0 -12 244933. 2551.54 1 0 0 -13 119.292 480.008 -2 0 0 -13 119.292 480.008 1 0 0 -14 90425.2 1834.03 -2 0 0 -14 90425.2 1834.03 1 0 0 -15 53.4035 536.094 -2 0 0 -15 53.4035 536.094 1 0 0 -16 49232.9 1520.22 -2 0 0 -16 49232.9 1520.22 1 0 0 -17 102.750 469.676 -2 0 0 -17 102.750 469.676 1 0 0 -18 671.476 655.688 -2 0 0 -18 671.476 655.688 1 0 0 -19 581.894 510.892 -2 0 0 -19 581.894 510.892 1 0 0 -20 73631.4 1626.01 -2 0 0 -20 73631.4 1626.01 1 0 0 -21 226.092 321.382 -2 0 0 -21 226.092 321.382 1 0 0 -22 49879.1 4513.58 -2 0 0 -22 49879.1 4513.58 1 0 0 -23 65.7242 471.755 -2 0 0 -23 65.7242 471.755 1 0 0 24 12235.6 1830.69 -2 0 0 24 12235.6 1830.69 1 0 0 -25 48.9591 527.277 -2 0 0 -25 48.9591 527.277 1 0 0 -26 32.9852 419.482 -2 0 0 -26 32.9852 419.482 1 0 0 -27-46.9642 433.323 -2 0 0 -27-46.9642 433.323 1 0 0 -28 559.492 471.517 -2 0 0 -28 559.492 471.517 1 0 0 -29 159.194 402.102 -2 0 0 -29 159.194 402.102 1 0 0 -30-61.8543 669.279 -2 0 0 -30-61.8543 669.279 1 0 0 -31 927.212 505.306 -2 0 0 -31 927.212 505.306 1 0 0 -32 10710.9 749.536 -2 0 0 -32 10710.9 749.536 1 0 0 -33 135.861 482.113 -2 0 0 -33 135.861 482.113 1 0 0 -34 2501.81 575.109 -2 0 0 -34 2501.81 575.109 1 0 0 -35 19.8893 405.060 -2 0 0 -35 19.8893 405.060 1 0 0 -36 6196.55 521.335 -2 0 0 -36 6196.55 521.335 1 0 1 -36 922.865 331.933 1 0 1 -35-222.454 367.135 1 0 1 -34 2993.24 433.041 1 0 1 -33 749.232 436.395 1 0 1 -32 2110.40 472.039 1 0 1 -31 5826.91 1403.27 1 0 1 -30 13936.7 3919.68 1 0 1 -29 480.468 341.042 1 0 1 -28 4460.72 817.560 1 0 1 -27 7660.40 1467.91 1 0 1 -26 3004.20 385.439 1 0 1 -25-25.1998 495.873 1 0 -1 -24 12.1211 417.499 -2 0 1 -25 12.1211 417.499 1 0 1 -24 1776.78 494.248 1 0 -1 -23 937.485 365.226 -2 0 1 -24 937.485 365.226 1 0 -1 23 15.9095 463.657 1 0 -1 -22 10569.0 402.057 -2 0 1 -23 10569.0 402.057 1 0 -1 22 12147.4 1716.34 1 0 -1 -21 11373.7 377.920 -2 0 1 -22 11373.7 377.920 1 0 -1 21-56.6787 626.179 1 0 -1 -20 3554.92 519.153 -2 0 1 -21 3554.92 519.153 1 0 1 -20 10903.7 828.758 1 0 -1 19 2299.43 704.805 1 0 -1 18 156.056 599.849 1 0 -1 17 12058.2 839.953 1 0 -1 16 2962.80 637.071 1 0 -1 15 4085.00 631.617 1 0 -1 14 2966.33 621.575 1 0 -1 13-130.696 526.795 1 0 1 11 79832.4 1153.91 -2 0 -1 12 79832.4 1153.91 1 0 1 10 92931.1 1164.19 -2 0 -1 11 92931.1 1164.19 1 0 1 9 25380.4 735.588 -2 0 -1 10 25380.4 735.588 1 0 1 8 13939.1 612.674 -2 0 -1 9 13939.1 612.674 1 0 1 7 44774.1 784.445 -2 0 -1 8 44774.1 784.445 1 0 1 6 80595.2 893.227 -2 0 -1 7 80595.2 893.227 1 0 1 5 194951. 1196.30 -2 0 -1 6 194951. 1196.30 1 0 -1 5 195701. 1238.07 1 0 -1 4 6593.45 381.224 1 0 -1 3 5235.42 342.851 1 0 -1 2 95975.8 737.873 1 0 -1 1 134641. 876.387 1 0 -1 0 105629. 747.899 1 0 -1 -1 246514. 1181.39 1 0 -1 -2 69421.1 627.702 1 0 -1 -3 27888.1 463.608 1 0 -1 -4 42800.6 591.087 1 0 -1 -5 128318. 962.675 1 0 -1 -6 102927. 930.372 1 0 -1 -7 7831.54 418.684 1 0 -1 -8 15483.5 2614.26 1 0 -1 -9 16968.0 2865.43 1 0 -1 -10 26954.5 1870.16 1 0 -1 -11 44496.3 1135.01 1 0 -1 -12 28427.0 536.634 1 0 -1 -13 1744.63 285.067 1 0 -1 -14 9268.62 375.186 1 0 -1 -15 15221.3 780.621 1 0 -1 -16 9050.61 743.732 1 0 -1 -17 7012.21 693.305 1 0 -1 -18 2585.13 589.592 1 0 -1 -19 1896.43 647.218 1 0 -1 -20 6845.19 792.831 1 0 -1 -21-583.438 622.288 1 0 1 -22 7455.65 396.770 -2 0 -1 -21 7455.65 396.770 1 0 -1 -22 19321.8 1100.89 1 0 1 -23 10451.7 436.445 -2 0 -1 -22 10451.7 436.445 1 0 -1 -23-1381.91 647.376 1 0 1 -24 993.360 377.834 -2 0 -1 -23 993.360 377.834 1 0 -1 -24 241.437 715.930 1 0 1 -25 83.6804 426.663 -2 0 -1 -24 83.6804 426.663 1 0 1 -26 3208.15 1397.57 -2 0 -1 -25 3208.15 1397.57 1 0 -1 -26 8087.63 3517.49 1 0 -1 -27 9122.17 3261.40 1 0 -1 -28 655.715 538.312 1 0 -1 -29 1526.96 544.567 1 0 -1 -30 26686.7 721.013 1 0 -1 -31 2022.80 544.968 1 0 -1 -32-206.293 462.886 1 0 -1 -33 929.068 381.928 1 0 -1 -34 2098.36 411.958 1 0 -1 -35 632.693 351.504 1 0 -1 -36 898.674 304.059 1 0 -2 -34 739.097 375.585 -2 0 2 -35 739.097 375.585 1 0 -2 -33 1399.74 443.296 -2 0 2 -34 1399.74 443.296 1 0 -2 -32 1364.88 455.507 -2 0 2 -33 1364.88 455.507 1 0 -2 -31 455.849 496.242 -2 0 2 -32 455.849 496.242 1 0 -2 -30 26.0724 431.831 -2 0 2 -31 26.0724 431.831 1 0 -2 -29 5079.13 968.378 -2 0 2 -30 5079.13 968.378 1 0 -2 -28 5159.50 593.509 -2 0 2 -29 5159.50 593.509 1 0 -2 -27 2499.69 493.406 -2 0 2 -28 2499.69 493.406 1 0 -2 -26 11039.4 2306.62 -2 0 2 -27 11039.4 2306.62 1 0 2 25 15301.9 1368.43 -2 0 -2 26 15301.9 1368.43 1 0 -2 -24 10978.9 2090.98 -2 0 2 -25 10978.9 2090.98 1 0 2 23 6092.70 578.979 -2 0 -2 24 6092.70 578.979 1 0 -2 -22 8731.14 591.745 -2 0 2 -23 8731.14 591.745 1 0 -2 -21 8560.64 549.563 -2 0 2 -22 8560.64 549.563 1 0 2 20 6340.92 537.554 -2 0 -2 21 6340.92 537.554 1 0 -2 -19 18413.9 594.831 -2 0 2 -20 18413.9 594.831 1 0 2 18 16103.5 926.398 -2 0 -2 19 16103.5 926.398 1 0 2 17 18846.8 1207.19 -2 0 -2 18 18846.8 1207.19 1 0 2 16 53432.2 1739.52 -2 0 -2 17 53432.2 1739.52 1 0 2 15 83104.7 1996.92 -2 0 -2 16 83104.7 1996.92 1 0 2 14 57303.7 1658.67 -2 0 -2 15 57303.7 1658.67 1 0 2 13 57550.9 1581.67 -2 0 -2 14 57550.9 1581.67 1 0 2 12 736.397 748.501 -2 0 -2 13 736.397 748.501 1 0 2 11 73649.6 1646.58 -2 0 -2 12 73649.6 1646.58 1 0 2 10 69649.0 1540.02 -2 0 -2 11 69649.0 1540.02 1 0 2 9 4504.42 701.367 -2 0 -2 10 4504.42 701.367 1 0 2 8 41205.4 1163.80 -2 0 -2 9 41205.4 1163.80 1 0 2 7 206613. 2220.04 -2 0 -2 8 206613. 2220.04 1 0 2 6 194711. 2069.09 -2 0 -2 7 194711. 2069.09 1 0 2 5 340647. 2644.89 -2 0 -2 6 340647. 2644.89 1 0 2 4 317246. 2449.50 -2 0 -2 5 317246. 2449.50 1 0 2 3 438595. 2811.70 -2 0 -2 4 438595. 2811.70 1 0 2 2 187790. 1902.60 -2 0 -2 3 187790. 1902.60 1 0 2 1 45491.8 1047.88 -2 0 -2 2 45491.8 1047.88 1 0 2 0 50864.0 1096.69 -2 0 -2 1 50864.0 1096.69 1 0 2 -1 71976.9 1268.36 -2 0 -2 0 71976.9 1268.36 1 0 2 -2 80660.6 1323.95 -2 0 -2 -1 80660.6 1323.95 1 0 2 -3 270446. 2310.13 -2 0 -2 -2 270446. 2310.13 1 0 2 -4 254426. 2151.00 -2 0 -2 -3 254426. 2151.00 1 0 2 -5 439852. 2849.62 -2 0 -2 -4 439852. 2849.62 1 0 2 -6 268247. 2314.72 -2 0 -2 -5 268247. 2314.72 1 0 2 -7 262969. 2351.02 -2 0 -2 -6 262969. 2351.02 1 0 2 -8 101588. 1501.73 -2 0 -2 -7 101588. 1501.73 1 0 2 -9 53744.3 1214.01 -2 0 -2 -8 53744.3 1214.01 1 0 2 -10 2377.70 436.267 -2 0 -2 -9 2377.70 436.267 1 0 2 -11 85707.3 1799.11 -2 0 -2 -10 85707.3 1799.11 1 0 2 -12 43744.3 6689.97 -2 0 -2 -11 43744.3 6689.97 1 0 2 -13 765.693 367.269 -2 0 -2 -12 765.693 367.269 1 0 2 -14 26292.5 3445.78 -2 0 -2 -13 26292.5 3445.78 1 0 2 -15 90150.0 1913.32 -2 0 -2 -14 90150.0 1913.32 1 0 2 -16 79637.0 1904.58 -2 0 -2 -15 79637.0 1904.58 1 0 2 -17 50082.3 1641.92 -2 0 -2 -16 50082.3 1641.92 1 0 2 -18 15471.2 1181.80 -2 0 -2 -17 15471.2 1181.80 1 0 2 -19 25563.6 1455.50 -2 0 -2 -18 25563.6 1455.50 1 0 2 -20 18623.6 722.418 -2 0 -2 -19 18623.6 722.418 1 0 2 -21 10111.4 1540.81 -2 0 -2 -20 10111.4 1540.81 1 0 2 -22 10092.1 823.330 -2 0 -2 -21 10092.1 823.330 1 0 2 -23 8838.88 994.613 -2 0 -2 -22 8838.88 994.613 1 0 2 -24 10245.2 1996.88 -2 0 -2 -23 10245.2 1996.88 1 0 2 -25 10737.5 1414.05 -2 0 -2 -24 10737.5 1414.05 1 0 2 -26 23058.5 3080.25 -2 0 -2 -25 23058.5 3080.25 1 0 2 -27 11013.8 766.370 -2 0 -2 -26 11013.8 766.370 1 0 2 -28 2914.17 696.154 -2 0 -2 -27 2914.17 696.154 1 0 2 -29 6887.83 737.761 -2 0 -2 -28 6887.83 737.761 1 0 2 -30 4636.75 694.726 -2 0 -2 -29 4636.75 694.726 1 0 2 -31 24.9908 579.455 -2 0 -2 -30 24.9908 579.455 1 0 2 -32 490.236 469.916 -2 0 -2 -31 490.236 469.916 1 0 2 -33 1708.15 455.726 -2 0 -2 -32 1708.15 455.726 1 0 2 -34 1171.32 404.540 -2 0 -2 -33 1171.32 404.540 1 0 2 -35 306.030 328.804 -2 0 -2 -34 306.030 328.804 1 0 3 -33 885.977 264.204 1 0 3 -32-8.08396 322.292 1 0 3 -31 199.976 318.784 1 0 3 -30 1152.71 350.277 1 0 -3 -28 828.590 400.160 -2 0 3 -30 828.590 400.160 1 0 -3 -27 2033.39 903.023 -2 0 3 -29 2033.39 903.023 1 0 -3 28 284.591 575.170 1 0 -3 -26 550.467 420.251 -2 0 3 -28 550.467 420.251 1 0 -3 -25 3046.95 531.235 -2 0 3 -27 3046.95 531.235 1 0 -3 -24 2734.49 442.147 -2 0 3 -26 2734.49 442.147 1 0 -3 -23 505.326 414.912 -2 0 3 -25 505.326 414.912 1 0 -3 -22 145.776 402.241 -2 0 3 -24 145.776 402.241 1 0 3 21 2584.03 760.196 -2 0 -3 23 2584.03 760.196 1 0 -3 -20 5651.15 1363.43 -2 0 3 -22 5651.15 1363.43 1 0 3 19 7091.69 491.059 -2 0 -3 21 7091.69 491.059 1 0 3 18 25191.2 2065.41 -2 0 -3 20 25191.2 2065.41 1 0 3 17 1223.65 436.902 -2 0 -3 19 1223.65 436.902 1 0 -3 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311.752 1 5 3 4 1913.39 203.693 -2 -5 -3 7 1913.39 203.693 1 5 3 3 207.602 188.442 -2 -5 -3 6 207.602 188.442 1 5 3 2 515.742 203.523 -2 -5 -3 5 515.742 203.523 1 5 3 1 1573.50 217.739 -2 -5 -3 4 1573.50 217.739 1 5 3 0 1405.78 219.999 -2 -5 -3 3 1405.78 219.999 1 5 3 -1 26.9265 192.640 -2 -5 -3 2 26.9265 192.640 1 5 3 -2-52.1681 195.645 -2 -5 -3 1-52.1681 195.645 1 5 3 -3 888.596 208.488 -2 -5 -3 0 888.596 208.488 1 5 3 -4 2310.63 222.997 -2 -5 -3 -1 2310.63 222.997 1 5 3 -5 719.887 197.139 -2 -5 -3 -2 719.887 197.139 1 5 3 -6 89.3596 179.940 -2 -5 -3 -3 89.3596 179.940 1 5 3 -7 1893.54 190.292 -2 -5 -3 -4 1893.54 190.292 1 5 3 -8 2671.00 192.071 -2 -5 -3 -5 2671.00 192.071 1 5 3 -9 710.909 154.030 -2 -5 -3 -6 710.909 154.030 1 0 1 -36 497.045 327.486 2 0 1 -35 173.420 376.267 2 0 1 -34 2470.79 625.140 2 0 1 -33 323.660 344.450 2 0 1 -32 1816.40 511.040 2 0 1 -31 6963.62 585.782 2 0 1 -30 13870.8 663.941 2 0 1 -29 951.950 553.255 2 0 1 -28 5163.88 609.667 2 0 1 -27 6202.35 1991.83 2 0 1 -25 100.751 874.467 2 0 1 -24 1101.60 779.338 2 0 1 -23 348.144 710.407 2 0 1 -22 10977.9 982.708 2 0 1 -21-786.705 636.301 2 0 1 -20 8292.42 925.516 2 0 1 -19 2364.38 676.611 2 0 1 -18 117.702 584.521 2 0 1 -17 9850.45 845.771 2 0 1 -16 3169.81 638.490 2 0 1 -15 2015.19 647.572 2 0 1 -14 1880.92 325.443 2 0 1 -13-8.10938 301.901 2 0 1 -12 20444.2 7303.81 2 0 1 -11 28905.1 12360.4 2 0 1 -10 3372.29 1716.03 2 0 1 -9 447.162 423.255 2 0 1 -8 23325.4 614.344 2 0 1 -7 9342.66 443.715 2 0 1 -6 63553.3 825.982 2 0 1 -5 134712. 1016.05 2 0 1 -4 5365.99 358.297 2 0 1 -3 2485.52 326.804 2 0 1 -2 60276.9 631.816 2 0 1 -1 67146.2 609.956 2 0 1 0 56036.5 537.402 2 0 1 1 115612. 772.004 2 0 1 2 38119.2 507.432 2 0 1 3 15422.9 434.885 2 0 1 4 24319.3 511.582 2 0 1 12 15604.5 733.996 2 0 1 13 784.939 582.712 2 0 1 14 5545.03 658.067 2 0 1 15 7084.40 748.311 2 0 1 16 3820.91 668.731 2 0 1 17 3526.05 642.575 2 0 1 18 1028.93 607.051 2 0 1 19 1117.83 604.865 2 0 1 20 2835.84 727.812 2 0 -1 -21-104.684 423.466 2 0 -1 -22 10530.3 1062.24 2 0 -1 -23 172.301 462.522 2 0 -1 -24 95.9698 486.055 2 0 -1 -25 719.019 515.216 2 0 -1 -26 6330.30 625.077 2 0 -1 -27 7550.73 1247.21 2 0 -1 -28 135.100 340.429 2 0 -1 -29 821.739 570.665 2 0 -1 -30 14415.8 4215.17 2 0 -1 -31 1881.79 496.774 2 0 -1 -32-157.756 429.123 2 0 -1 -33 1223.23 410.839 2 0 -1 -34 1991.40 398.573 2 0 -1 -35 333.573 333.407 2 0 -1 -36 462.512 289.410 2 0 3 -35 190.491 207.609 2 0 3 -34 318.667 265.775 2 0 3 -33 583.062 314.442 2 0 3 -32 66.1879 321.542 2 0 3 -31-84.7637 358.337 2 0 3 -30 994.849 323.828 2 0 3 -29 1295.15 310.798 2 0 3 -28 285.945 309.907 2 0 3 -27 1515.96 366.242 2 0 3 -23 925.593 877.486 2 0 3 -22 2519.14 796.764 2 0 3 -21 3995.20 764.038 2 0 3 -20 9456.26 914.488 2 0 3 -19 327.559 616.383 2 0 3 -18 12565.4 883.227 2 0 3 -17 7880.77 739.114 2 0 3 -14 33.3610 286.755 2 0 3 -13 1302.56 315.511 2 0 3 -12 1573.25 373.457 2 0 3 -6 68997.6 1351.69 2 0 -3 -28 639.688 363.916 2 0 -3 -29 26.1106 338.774 2 0 -3 -30 105.825 314.736 2 0 -3 -31-322.386 302.510 2 0 4 -34 9.88707 199.924 2 0 5 -31 124.188 223.356 2 0 5 -30-112.217 274.904 2 0 5 -12 152.018 554.388 2 0 -5 -27-73.3114 239.849 2 0 -5 -28 50.6298 209.840 2 0 -5 -29 314.681 185.073 2 0 7 19 744.276 190.186 2 1 -7 -21 518.968 182.309 2 1 -7 -20 326.666 193.505 2 -1 7 17 318.020 236.463 2 -1 7 16 233.142 261.542 2 1 -7 19 137.495 254.190 2 1 -7 20 323.323 229.022 2 -1 7 -22-140.649 242.584 2 -1 7 -23 263.525 226.346 2 1 -5 -28 2649.18 259.187 2 1 -5 -27 364.783 258.633 2 1 -5 -26 407.398 201.444 2 1 -5 -25 1270.41 806.361 2 1 -5 -21 1255.73 311.131 2 1 -5 -20 348.778 317.643 2 1 -5 -19-60.3014 324.638 2 -1 5 -26 277.005 324.570 2 -1 5 -27 2650.85 351.742 2 -1 5 -28 399.264 286.807 2 -1 5 -29 363.169 502.295 2 -1 5 -30 2249.73 717.267 2 -1 5 -31-3.48964 315.920 2 1 -3 -32-153.898 210.524 2 1 -3 -31-184.119 226.067 2 1 -3 -30 109.631 237.269 2 1 -3 -3 5009.66 186.103 2 1 -3 27-92.6785 513.376 2 -1 3 -28 70.7715 389.112 2 -1 3 -29 1559.16 336.710 2 -1 3 -30-14.2030 293.942 2 -1 3 -31 72.2746 271.888 2 -1 3 -32 136.328 221.514 2 -1 3 -33 177.338 279.439 2 -1 3 -34-276.073 228.760 2 -1 3 -35 276.372 186.743 2 1 -1 -5 61791.2 600.121 2 1 -1 -3 261211. 1264.48 2 1 -1 -2 170384. 1630.58 2 1 -1 -1 1124.19 301.236 2 -1 1 -1 20169.5 447.139 2 -1 1 -35-18.5817 310.845 2 -1 1 -36-100.126 262.380 2 -1 0 2 234190. 571.008 2 1 0 -1 2943.20 278.342 2 1 1 -12 424.368 349.974 2 1 2 -35 419.046 306.963 2 1 2 -34 53.5845 274.972 2 1 2 -33-96.9366 271.248 2 1 2 -32 172.366 297.132 2 1 2 -31 1860.99 351.025 2 1 2 -30 1444.02 394.778 2 1 2 -7 16944.5 405.072 2 1 2 -6 81.6138 216.222 2 1 2 -5 23676.9 462.210 2 -1 -2 -34 357.939 237.953 2 1 4 -32 323.915 238.491 2 1 4 -31 72.4450 275.693 2 1 4 -30 2042.76 357.524 2 1 4 -29 585.113 350.958 2 1 4 -28 446.528 357.301 2 1 4 28 1936.75 315.837 2 1 4 29-696.368 399.899 2 1 6 -27 94.1667 219.266 2 1 6 -26 885.764 258.460 2 1 6 20 805.772 234.260 2 1 6 21 96.4617 193.474 2 -1 -6 -22 1010.17 203.134 2 -1 -6 -23 158.475 176.589 2 -1 -8 15-12.5757 160.362 2 -2 7 -23 21.4697 174.301 2 -2 4 -31 96.5939 209.972 2 -2 4 -32-41.2176 178.934 2 2 -2 -33 227.076 175.875 2 2 -2 -32-94.1866 209.590 2 2 -2 -30 2776.13 394.082 2 -2 2 -15 5918.61 315.915 2 2 -2 29-30.3940 498.179 2 2 -2 30 3511.80 503.094 2 2 -2 31 1451.54 369.877 2 -2 2 -32 88.4144 282.772 2 2 -2 33 125.730 280.677 2 2 0 -34-90.1192 350.256 2 2 0 -33 199.730 398.741 2 2 0 -32 275.009 416.836 2 2 0 -31-18.2240 284.758 2 2 0 -30 20.4542 290.054 2 2 0 -29 196.466 376.160 2 2 0 -28 1063.77 343.814 2 2 0 -27-3.94441 455.873 2 2 0 -26 777.357 552.331 2 2 0 -19 116.334 175.232 2 2 0 -17 7197.94 549.457 2 2 0 -16-108.384 354.450 2 2 0 -15 816.797 370.486 2 2 0 -14 392.455 348.141 2 2 0 -13 7123.40 521.655 2 2 0 -12 849.687 368.955 2 2 0 -11 3718.78 477.263 2 2 0 -10 5110.59 501.658 2 2 0 -9 19921.7 691.465 2 2 0 -8 8320.40 521.220 2 2 0 -7 21467.7 633.005 2 2 0 -6 1606.53 390.956 2 2 0 -5 346.856 358.655 2 2 0 -3 30558.9 709.831 2 2 0 3 45603.3 674.984 2 2 0 4 55721.6 708.999 2 2 0 5 11830.4 402.227 2 2 0 6 1684.26 280.852 2 2 0 7 9232.64 348.565 2 2 0 14 48.3170 355.714 2 2 0 15 3667.45 436.523 2 2 0 18 99.9521 312.361 2 2 0 19 182.481 339.191 2 2 0 20 942.777 361.869 2 2 0 21 494.090 358.025 2 2 0 22 671.268 575.646 2 2 0 23-283.703 776.020 2 2 0 24 644.530 762.289 2 2 0 25 985.422 763.789 2 2 0 26 2692.96 741.552 2 2 0 27-167.440 660.195 2 2 0 28 317.046 618.660 2 2 0 29-693.186 564.755 2 2 0 30 167.203 511.658 2 2 0 31-497.904 448.640 2 2 0 32-465.629 397.313 2 2 0 33 657.752 315.338 2 -2 0 -34-156.741 225.638 2 2 2 -33 374.746 340.328 2 2 2 -32 643.751 390.617 2 2 2 -31-424.490 440.210 2 2 2 -30 548.670 348.808 2 2 2 -29 1194.95 465.048 2 2 2 -20 362.216 662.581 2 2 2 -19 1053.33 555.292 2 2 2 -18-164.894 477.089 2 2 2 -17 222.076 444.623 2 2 2 -16 44.6997 424.330 2 2 2 -15 1080.87 419.755 2 2 2 -14-16.7832 367.735 2 2 2 -13 14.7783 370.971 2 2 2 -12 37.1323 362.866 2 2 2 -11 553.317 345.188 2 2 2 -10 334.727 307.491 2 2 2 -9 73.0082 279.511 2 2 2 -8 2272.09 417.272 2 2 2 -7 184.993 352.998 2 2 2 -6 489.643 399.301 2 2 2 -3 223.469 412.063 2 2 2 4 5813.23 503.006 2 2 2 5 899.823 390.509 2 2 2 6 4558.65 2522.92 2 2 2 7 264.087 694.079 2 2 2 8 757.752 853.860 2 2 2 10 86.7922 426.310 2 2 2 11-21.2412 388.688 2 2 2 12-219.278 404.372 2 2 2 13 643.184 420.576 2 2 2 14-65.9872 392.910 2 2 2 15 821.327 442.037 2 2 2 16 199.263 418.094 2 2 2 17-352.954 494.690 2 2 2 18 645.907 296.890 2 2 2 19 146.362 254.568 2 2 2 20 3085.14 283.000 2 2 2 21 7532.89 405.723 2 2 2 22 1489.47 823.401 2 2 2 23 1055.30 774.108 2 2 2 24 63.8712 751.112 2 2 2 25 100.001 682.981 2 2 2 26 237.754 635.516 2 2 2 27 1391.69 610.966 2 2 2 28 341.261 547.474 2 2 2 29 43.3570 482.950 2 2 2 30 865.325 441.749 2 2 2 31-100.560 366.533 2 2 2 32 303.004 269.594 2 2 4 -30 299.310 234.134 2 2 4 -29 93.6168 272.717 2 2 4 -13-280.903 444.018 2 2 4 -12 2059.33 684.964 2 2 4 4 137.446 487.737 2 2 4 5-111.523 510.386 2 2 4 6-133.177 509.660 2 2 4 7-357.440 694.452 2 2 4 20-139.291 280.257 2 2 4 21 365.225 265.789 2 2 4 22 969.608 256.113 2 2 4 25-246.444 494.646 2 2 4 26 295.502 439.233 2 2 4 27 333.269 369.041 2 2 4 28-148.397 310.258 2 2 6 20 441.604 334.985 2 3 -6 -19 167.333 124.074 2 3 -6 -16 262.904 209.039 2 3 -6 -15 782.579 224.203 2 3 -6 18-65.7107 170.492 2 -3 6 -21-80.4839 222.184 2 -3 6 -22 427.375 215.075 2 -3 6 -23-17.6492 196.745 2 -3 6 -24 267.727 169.723 2 3 -4 -28 15.1807 149.750 2 3 -4 -27 195.173 164.145 2 3 -4 -26 1.69405 194.538 2 3 -4 -25 519.072 190.750 2 3 -4 -24 334.892 188.234 2 3 -4 -23 2419.00 227.889 2 3 -4 19 428.498 303.474 2 3 -4 20 766.159 295.637 2 3 -4 21 221.826 261.711 2 3 -4 22 491.854 235.993 2 3 -4 23 411.420 223.638 2 -3 4 -25 2672.40 309.802 2 -3 4 -26 49.8172 267.568 2 -3 4 -27 325.738 236.864 2 -3 4 -28 199.837 214.244 2 -3 4 -29-142.339 184.153 2 3 -2 -30 145.808 182.472 2 3 -2 -29 318.688 193.069 2 3 -2 -28 527.436 208.087 2 3 -2 -27-67.1625 210.174 2 3 -2 28 161.213 246.069 2 3 -2 29-55.1836 372.318 2 3 -2 30 34.4965 221.582 2 3 -2 31 1221.05 191.801 2 3 0 31 738.969 284.870 2 3 3 -27-26.7232 229.393 2 3 3 -26 507.641 270.989 2 4 -6 18 1288.95 134.602 2 -4 4 -25 694.699 168.211 2 4 -3 -25 44.6784 245.715 2 4 -1 -27 188.163 594.196 2 4 -1 -26 2416.92 323.888 2 4 -1 26 636.343 303.049 2 4 1 -26 334.502 296.445 2 4 1 -25-94.2436 340.876 2 4 1 -20 1156.35 195.834 2 4 1 -19 312.891 183.187 2 -4 -1 -18 546.161 209.888 2 -4 -1 -19-21.5243 193.006 2 -4 -1 -20 751.706 181.618 2 -4 -1 -21 120.416 159.856 2 4 1 22 457.360 389.318 2 4 1 23 243.002 343.148 2 4 1 24 347.562 292.016 2 -4 -3 -16 15.2045 142.278 2 -4 -3 -17 88.2426 133.253 2 4 3 18 427.036 370.645 2 -4 -3 -19 164.575 103.903 2 5 -3 -18 105.102 116.546 2 5 -3 18 68.7712 152.438 2 5 -3 19 470.691 144.301 2 5 2 -15 482.861 112.083 2 0 0 0 0.00000 0.00000 0 TITL bmk2469b_twin1_hklf4 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 4.853023 7.350373 29.862393 93.5837 90.3846 99.9053 ZERR 4.00 0.000259 0.000532 0.002504 0.0064 0.0054 0.0052 LATT 1 SFAC C H N O UNIT 44.00 40.00 4.00 4.00 TREF HKLF 5 BASF 0.40363 END ; _shelx_hkl_checksum 13069 _shelx_res_file ; TITL bmk2469b in P-1 shelx.res created by SHELXL-2019/3 at 17:20:22 on 06-May-2025 REM P-1 (#2 in standard setting) CELL 1.54184 4.8530 7.3504 29.8624 93.584 90.385 99.905 ZERR 4.00 0.0003 0.0005 0.0025 0.006 0.005 0.005 LATT 1 SFAC C H N O UNIT 40 48 16 4 MERG 2 FMAP 2 PLAN 10 SIZE 0.040 0.130 0.810 ACTA BOND $H LIST 4 L.S. 4 TEMP 23.00 WGHT 0.127300 0.434900 BASF 0.40254 FVAR 10.80734 C1 1 0.391393 0.729648 0.142370 11.00000 0.03959 0.05780 = 0.03920 -0.00742 -0.00913 0.01589 C2 1 0.530806 0.910923 0.136280 11.00000 0.04471 0.05248 = 0.04928 -0.00260 -0.01028 0.00907 C3 1 0.465020 1.052501 0.165431 11.00000 0.07428 0.05231 = 0.06343 -0.00938 -0.00903 0.01751 AFIX 43 H3 2 0.551146 1.173825 0.161931 11.00000 -1.20000 AFIX 0 C4 1 0.277512 1.017217 0.198918 11.00000 0.08586 0.06775 = 0.05103 -0.00992 -0.00205 0.02649 AFIX 43 H4 2 0.236213 1.113937 0.217831 11.00000 -1.20000 AFIX 0 C5 1 0.149061 0.837827 0.204721 11.00000 0.06804 0.08559 = 0.04191 0.00065 0.00653 0.02563 AFIX 43 H5 2 0.021724 0.814386 0.227667 11.00000 -1.20000 AFIX 0 C6 1 0.207791 0.691926 0.176687 11.00000 0.05092 0.05656 = 0.04201 -0.00069 -0.00526 0.01262 C7 1 0.737314 0.954146 0.099414 11.00000 0.05547 0.07480 = 0.06335 0.00176 0.00042 0.01273 AFIX 137 H7A 2 0.806593 1.084855 0.100752 11.00000 -1.50000 H7B 2 0.646671 0.916193 0.070856 11.00000 -1.50000 H7C 2 0.890367 0.888951 0.103125 11.00000 -1.50000 AFIX 0 C8 1 0.071613 0.498428 0.186005 11.00000 0.07630 0.08089 = 0.05929 0.01649 0.00822 0.00398 AFIX 137 H8A 2 0.206330 0.417190 0.182689 11.00000 -1.50000 H8B 2 -0.081267 0.457138 0.165192 11.00000 -1.50000 H8C 2 0.002923 0.497548 0.216077 11.00000 -1.50000 AFIX 0 C9 1 0.252031 0.484942 0.083585 11.00000 0.03376 0.06799 = 0.03721 -0.00320 -0.00426 0.00824 C10 1 0.356454 0.343630 0.051934 11.00000 0.04407 0.06745 = 0.04310 -0.01294 -0.00803 0.00999 AFIX 23 H10A 2 0.558968 0.371779 0.050904 11.00000 -1.20000 H10B 2 0.304729 0.221644 0.063171 11.00000 -1.20000 AFIX 0 C11 1 0.858829 0.660051 0.358268 11.00000 0.02320 0.02980 = 0.05352 0.00631 0.00136 0.01149 C12 1 0.993785 0.844317 0.365112 11.00000 0.02905 0.02770 = 0.05681 0.00514 0.00474 0.00957 C13 1 0.922907 0.972455 0.336560 11.00000 0.05440 0.03343 = 0.06735 0.01107 0.00857 0.01197 AFIX 43 H13 2 1.012905 1.094993 0.339935 11.00000 -1.20000 AFIX 0 C14 1 0.721535 0.920054 0.303446 11.00000 0.07210 0.04824 = 0.05530 0.01218 -0.00094 0.02439 AFIX 43 H14 2 0.669115 1.008470 0.285733 11.00000 -1.20000 AFIX 0 C15 1 0.596877 0.737057 0.296360 11.00000 0.05636 0.05607 = 0.05107 0.00716 -0.00948 0.02131 AFIX 43 H15 2 0.465969 0.703164 0.273131 11.00000 -1.20000 AFIX 0 C16 1 0.662798 0.602270 0.323207 11.00000 0.03702 0.03838 = 0.05327 0.00056 -0.00498 0.01069 C17 1 1.209282 0.900975 0.401535 11.00000 0.03735 0.04752 = 0.06992 0.00435 -0.00300 -0.00181 AFIX 137 H17A 2 1.372137 0.847494 0.394543 11.00000 -1.50000 H17B 2 1.134856 0.858455 0.429465 11.00000 -1.50000 H17C 2 1.259438 1.033412 0.404019 11.00000 -1.50000 AFIX 0 C18 1 0.536119 0.403873 0.313324 11.00000 0.07293 0.04637 = 0.07256 -0.00334 -0.01765 0.00274 AFIX 137 H18A 2 0.344075 0.384169 0.322205 11.00000 -1.50000 H18B 2 0.636947 0.327169 0.329667 11.00000 -1.50000 H18C 2 0.545843 0.372652 0.281742 11.00000 -1.50000 AFIX 0 C19 1 0.732234 0.441560 0.416010 11.00000 0.02504 0.02477 = 0.05837 0.00675 -0.00362 0.00703 C20 1 0.843696 0.318404 0.447978 11.00000 0.02979 0.03180 = 0.06075 0.01609 0.00325 0.01216 AFIX 23 H20A 2 0.789956 0.190184 0.436906 11.00000 -1.20000 H20B 2 1.046425 0.347350 0.448974 11.00000 -1.20000 AFIX 0 N1 3 0.449710 0.584979 0.111488 11.00000 0.03275 0.05730 = 0.04586 -0.00775 -0.00360 0.01261 N2 3 0.238933 0.342659 0.006388 11.00000 0.04626 0.07979 = 0.04296 -0.00286 -0.00141 0.00360 N3 3 0.010324 0.243673 -0.000516 11.00000 0.04740 0.07713 = 0.04087 -0.00847 -0.00197 0.01433 N4 3 -0.193781 0.156158 -0.012785 11.00000 0.04992 0.10048 = 0.06700 -0.01734 -0.01624 0.00754 N5 3 0.923334 0.527967 0.388263 11.00000 0.01707 0.03173 = 0.06010 0.01015 -0.00029 0.00725 N6 3 0.738158 0.341789 0.493045 11.00000 0.04450 0.04367 = 0.06158 0.00755 -0.00228 -0.00196 N7 3 0.510308 0.245539 0.500538 11.00000 0.03359 0.03717 = 0.05828 0.00841 -0.00122 0.01166 N8 3 0.308763 0.165657 0.512999 11.00000 0.03653 0.07056 = 0.08915 0.01397 0.00578 0.00928 O1 4 0.002971 0.496978 0.084496 11.00000 0.03110 0.08531 = 0.06240 -0.01619 -0.00704 0.01766 O2 4 0.486397 0.453849 0.415606 11.00000 0.02106 0.05820 = 0.07339 0.01879 0.00316 0.01460 H5A 2 1.108021 0.534138 0.394592 11.00000 0.04042 H1 2 0.630064 0.582564 0.105289 11.00000 0.07285 HKLF 5 REM bmk2469b in P-1 REM wR2 = 0.2441, GooF = S = 1.084, Restrained GooF = 1.084 for all data REM R1 = 0.0757 for 2956 Fo > 4sig(Fo) and 0.1040 for all 4441 data REM 284 parameters refined using 0 restraints END WGHT 0.1273 0.4349 REM Highest difference peak 0.262, deepest hole -0.281, 1-sigma level 0.065 Q1 1 0.8290 0.9839 0.4001 11.00000 0.05 0.26 Q2 1 0.6910 0.6140 0.0726 11.00000 0.05 0.24 Q3 1 -0.3953 0.1615 -0.0217 11.00000 0.05 0.23 Q4 1 1.1281 1.1061 0.1099 11.00000 0.05 0.22 Q5 1 0.8865 0.7976 0.3679 11.00000 0.05 0.22 Q6 1 -0.0884 0.5232 0.0929 11.00000 0.05 0.21 Q7 1 1.2938 1.1044 0.3012 11.00000 0.05 0.21 Q8 1 0.3449 0.3938 0.2821 11.00000 0.05 0.21 Q9 1 1.1536 0.5142 0.4503 11.00000 0.05 0.21 Q10 1 0.4009 1.0382 0.1813 11.00000 0.05 0.21 ; _shelx_res_checksum 50701 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.3914(11) 0.7296(8) 0.14237(17) 0.0451(13) Uani d 1 . . C C2 0.5308(11) 0.9109(9) 0.13628(19) 0.0490(13) Uani d 1 . . C C3 0.4650(15) 1.0525(10) 0.1654(2) 0.0632(17) Uani d 1 . . H H3 0.551146 1.173825 0.161931 0.076 Uiso calc 1 . . C C4 0.2775(16) 1.0172(10) 0.1989(2) 0.0672(18) Uani d 1 . . H H4 0.236213 1.113937 0.217831 0.081 Uiso calc 1 . . C C5 0.1491(14) 0.8378(11) 0.2047(2) 0.0638(18) Uani d 1 . . H H5 0.021724 0.814386 0.227667 0.077 Uiso calc 1 . . C C6 0.2078(12) 0.6919(9) 0.17669(18) 0.0496(13) Uani d 1 . . C C7 0.7373(14) 0.9541(11) 0.0994(2) 0.0645(17) Uani d 1 . . H H7A 0.806593 1.084855 0.100752 0.097 Uiso calc 1 . . H H7B 0.646671 0.916193 0.070856 0.097 Uiso calc 1 . . H H7C 0.890367 0.888951 0.103125 0.097 Uiso calc 1 . . C C8 0.0716(16) 0.4984(12) 0.1860(3) 0.073(2) Uani d 1 . . H H8A 0.206330 0.417190 0.182689 0.109 Uiso calc 1 . . H H8B -0.081267 0.457138 0.165192 0.109 Uiso calc 1 . . H H8C 0.002923 0.497548 0.216077 0.109 Uiso calc 1 . . C C9 0.2520(10) 0.4849(8) 0.08358(17) 0.0467(13) Uani d 1 . . C C10 0.3565(11) 0.3436(9) 0.05193(18) 0.0522(14) Uani d 1 . . H H10A 0.558968 0.371779 0.050904 0.063 Uiso calc 1 . . H H10B 0.304729 0.221644 0.063171 0.063 Uiso calc 1 . . C C11 0.8588(9) 0.6601(6) 0.35827(17) 0.0345(10) Uani d 1 . . C C12 0.9938(9) 0.8443(7) 0.36511(18) 0.0372(11) Uani d 1 . . C C13 0.9229(12) 0.9725(8) 0.3366(2) 0.0508(13) Uani d 1 . . H H13 1.012905 1.094993 0.339935 0.061 Uiso calc 1 . . C C14 0.7215(14) 0.9201(9) 0.3034(2) 0.0565(15) Uani d 1 . . H H14 0.669115 1.008470 0.285733 0.068 Uiso calc 1 . . C C15 0.5969(12) 0.7371(9) 0.2964(2) 0.0530(14) Uani d 1 . . H H15 0.465969 0.703164 0.273131 0.064 Uiso calc 1 . . C C16 0.6628(10) 0.6023(7) 0.32321(19) 0.0425(12) Uani d 1 . . C C17 1.2093(11) 0.9010(8) 0.4015(2) 0.0527(14) Uani d 1 . . H H17A 1.372137 0.847494 0.394543 0.079 Uiso calc 1 . . H H17B 1.134856 0.858455 0.429465 0.079 Uiso calc 1 . . H H17C 1.259438 1.033412 0.404019 0.079 Uiso calc 1 . . C C18 0.5361(15) 0.4039(9) 0.3133(3) 0.0652(17) Uani d 1 . . H H18A 0.344075 0.384169 0.322205 0.098 Uiso calc 1 . . H H18B 0.636947 0.327169 0.329667 0.098 Uiso calc 1 . . H H18C 0.545843 0.372652 0.281742 0.098 Uiso calc 1 . . C C19 0.7322(9) 0.4416(6) 0.41601(17) 0.0356(10) Uani d 1 . . C C20 0.8437(9) 0.3184(7) 0.44798(17) 0.0394(11) Uani d 1 . . H H20A 0.789956 0.190184 0.436906 0.047 Uiso calc 1 . . H H20B 1.046425 0.347350 0.448974 0.047 Uiso calc 1 . . N N1 0.4497(9) 0.5850(7) 0.11149(15) 0.0452(11) Uani d 1 . . N N2 0.2389(11) 0.3427(8) 0.00639(16) 0.0575(13) Uani d 1 . . N N3 0.0103(11) 0.2437(8) -0.00052(15) 0.0552(13) Uani d 1 . . N N4 -0.1938(12) 0.1562(10) -0.0128(2) 0.0742(17) Uani d 1 . . N N5 0.9233(7) 0.5280(5) 0.38826(15) 0.0356(9) Uani d 1 . . N N6 0.7382(9) 0.3418(6) 0.49305(17) 0.0509(11) Uani d 1 . . N N7 0.5103(9) 0.2455(6) 0.50054(15) 0.0421(10) Uani d 1 . . N N8 0.3088(10) 0.1657(8) 0.5130(2) 0.0650(15) Uani d 1 . . O O1 0.0030(8) 0.4970(7) 0.08450(15) 0.0596(12) Uani d 1 . . O O2 0.4864(7) 0.4538(6) 0.41561(14) 0.0493(10) Uani d 1 . . H H5A 1.108(12) 0.534(8) 0.3946(18) 0.040(14) Uiso d 1 . . H H1 0.630(16) 0.583(11) 0.105(2) 0.07(2) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.040(3) 0.058(4) 0.039(3) 0.016(2) -0.009(2) -0.007(2) C2 0.045(3) 0.052(3) 0.049(3) 0.009(2) -0.010(2) -0.003(2) C3 0.074(4) 0.052(4) 0.063(4) 0.018(3) -0.009(3) -0.009(3) C4 0.086(5) 0.068(5) 0.051(4) 0.026(4) -0.002(3) -0.010(3) C5 0.068(4) 0.086(5) 0.042(3) 0.026(4) 0.007(3) 0.001(3) C6 0.051(3) 0.057(4) 0.042(3) 0.013(3) -0.005(2) -0.001(2) C7 0.055(4) 0.075(5) 0.063(4) 0.013(3) 0.000(3) 0.002(3) C8 0.076(5) 0.081(5) 0.059(4) 0.004(4) 0.008(3) 0.016(4) C9 0.034(3) 0.068(4) 0.037(3) 0.008(2) -0.0043(19) -0.003(2) C10 0.044(3) 0.067(4) 0.043(3) 0.010(3) -0.008(2) -0.013(3) C11 0.0232(19) 0.030(2) 0.054(3) 0.0115(16) 0.0014(18) 0.006(2) C12 0.029(2) 0.028(2) 0.057(3) 0.0096(17) 0.0047(18) 0.005(2) C13 0.054(3) 0.033(3) 0.067(4) 0.012(2) 0.009(3) 0.011(2) C14 0.072(4) 0.048(3) 0.055(4) 0.024(3) -0.001(3) 0.012(3) C15 0.056(3) 0.056(4) 0.051(3) 0.021(3) -0.009(2) 0.007(3) C16 0.037(3) 0.038(3) 0.053(3) 0.011(2) -0.005(2) 0.001(2) C17 0.037(3) 0.048(3) 0.070(4) -0.002(2) -0.003(3) 0.004(3) C18 0.073(4) 0.046(4) 0.073(4) 0.003(3) -0.018(3) -0.003(3) C19 0.025(2) 0.025(2) 0.058(3) 0.0070(16) -0.0036(18) 0.0067(19) C20 0.030(2) 0.032(2) 0.061(3) 0.0122(17) 0.003(2) 0.016(2) N1 0.033(2) 0.057(3) 0.046(2) 0.0126(19) -0.0036(18) -0.008(2) N2 0.046(3) 0.080(4) 0.043(3) 0.004(2) -0.001(2) -0.003(2) N3 0.047(3) 0.077(4) 0.041(3) 0.014(2) -0.0020(19) -0.008(2) N4 0.050(3) 0.100(5) 0.067(4) 0.008(3) -0.016(3) -0.017(3) N5 0.0171(16) 0.032(2) 0.060(3) 0.0073(13) -0.0003(16) 0.0102(17) N6 0.044(3) 0.044(3) 0.062(3) -0.0020(19) -0.002(2) 0.008(2) N7 0.034(2) 0.037(2) 0.058(3) 0.0117(16) -0.0012(17) 0.0084(19) N8 0.037(3) 0.071(4) 0.089(4) 0.009(2) 0.006(2) 0.014(3) O1 0.031(2) 0.085(3) 0.062(3) 0.0177(19) -0.0070(16) -0.016(2) O2 0.0211(17) 0.058(2) 0.073(3) 0.0146(15) 0.0032(15) 0.0188(19) 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 C6 C1 C2 . . 121.7(6) ? C6 C1 N1 . . 120.9(6) ? C2 C1 N1 . . 117.4(5) ? C3 C2 C1 . . 117.2(6) ? C3 C2 C7 . . 120.4(6) ? C1 C2 C7 . . 122.4(6) ? C4 C3 C2 . . 121.6(7) ? C4 C3 H3 . . 119.2 ? C2 C3 H3 . . 119.2 ? C3 C4 C5 . . 119.9(7) ? C3 C4 H4 . . 120.0 ? C5 C4 H4 . . 120.0 ? C4 C5 C6 . . 120.7(6) ? C4 C5 H5 . . 119.6 ? C6 C5 H5 . . 119.6 ? C1 C6 C5 . . 118.8(6) ? C1 C6 C8 . . 122.9(6) ? C5 C6 C8 . . 118.3(6) ? C2 C7 H7A . . 109.5 ? C2 C7 H7B . . 109.5 ? H7A C7 H7B . . 109.5 ? C2 C7 H7C . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? C6 C8 H8A . . 109.5 ? C6 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C6 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? O1 C9 N1 . . 124.2(5) ? O1 C9 C10 . . 120.9(5) ? N1 C9 C10 . . 114.8(4) ? N2 C10 C9 . . 111.5(5) ? N2 C10 H10A . . 109.3 ? C9 C10 H10A . . 109.3 ? N2 C10 H10B . . 109.3 ? C9 C10 H10B . . 109.3 ? H10A C10 H10B . . 108.0 ? C12 C11 C16 . . 122.0(5) ? C12 C11 N5 . . 118.5(4) ? C16 C11 N5 . . 119.5(4) ? C13 C12 C11 . . 117.9(5) ? C13 C12 C17 . . 121.1(5) ? C11 C12 C17 . . 121.0(5) ? C14 C13 C12 . . 120.8(5) ? C14 C13 H13 . . 119.6 ? C12 C13 H13 . . 119.6 ? C13 C14 C15 . . 120.4(6) ? C13 C14 H14 . . 119.8 ? C15 C14 H14 . . 119.8 ? C14 C15 C16 . . 121.4(5) ? C14 C15 H15 . . 119.3 ? C16 C15 H15 . . 119.3 ? C15 C16 C11 . . 117.4(5) ? C15 C16 C18 . . 120.3(5) ? C11 C16 C18 . . 122.3(5) ? C12 C17 H17A . . 109.5 ? C12 C17 H17B . . 109.5 ? H17A C17 H17B . . 109.5 ? C12 C17 H17C . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? C16 C18 H18A . . 109.5 ? C16 C18 H18B . . 109.5 ? H18A C18 H18B . . 109.5 ? C16 C18 H18C . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? O2 C19 N5 . . 124.4(4) ? O2 C19 C20 . . 120.5(4) ? N5 C19 C20 . . 115.1(4) ? N6 C20 C19 . . 111.9(4) ? N6 C20 H20A . . 109.2 ? C19 C20 H20A . . 109.2 ? N6 C20 H20B . . 109.2 ? C19 C20 H20B . . 109.2 ? H20A C20 H20B . . 107.9 ? C9 N1 C1 . . 122.5(4) ? C9 N1 H1 . . 118(5) ? C1 N1 H1 . . 117(5) ? N3 N2 C10 . . 115.4(5) ? N4 N3 N2 . . 170.7(6) ? C19 N5 C11 . . 122.4(3) ? C19 N5 H5A . . 119(4) ? C11 N5 H5A . . 115(4) ? N7 N6 C20 . . 115.9(5) ? N8 N7 N6 . . 171.1(6) ? 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 C6 . 1.373(8) ? C1 C2 . 1.410(9) ? C1 N1 . 1.430(7) ? C2 C3 . 1.396(8) ? C2 C7 . 1.505(9) ? C3 C4 . 1.363(10) ? C3 H3 . 0.9300 ? C4 C5 . 1.380(10) ? C4 H4 . 0.9300 ? C5 C6 . 1.389(9) ? C5 H5 . 0.9300 ? C6 C8 . 1.505(10) ? C7 H7A . 0.9600 ? C7 H7B . 0.9600 ? C7 H7C . 0.9600 ? C8 H8A . 0.9600 ? C8 H8B . 0.9600 ? C8 H8C . 0.9600 ? C9 O1 . 1.227(6) ? C9 N1 . 1.351(7) ? C9 C10 . 1.515(7) ? C10 N2 . 1.470(7) ? C10 H10A . 0.9700 ? C10 H10B . 0.9700 ? C11 C12 . 1.401(7) ? C11 C16 . 1.405(7) ? C11 N5 . 1.433(6) ? C12 C13 . 1.393(7) ? C12 C17 . 1.493(7) ? C13 C14 . 1.375(9) ? C13 H13 . 0.9300 ? C14 C15 . 1.379(9) ? C14 H14 . 0.9300 ? C15 C16 . 1.390(8) ? C15 H15 . 0.9300 ? C16 C18 . 1.492(8) ? C17 H17A . 0.9600 ? C17 H17B . 0.9600 ? C17 H17C . 0.9600 ? C18 H18A . 0.9600 ? C18 H18B . 0.9600 ? C18 H18C . 0.9600 ? C19 O2 . 1.212(5) ? C19 N5 . 1.350(6) ? C19 C20 . 1.514(6) ? C20 N6 . 1.454(7) ? C20 H20A . 0.9700 ? C20 H20B . 0.9700 ? N1 H1 . 0.90(8) ? N2 N3 . 1.226(7) ? N3 N4 . 1.129(7) ? N5 H5A . 0.91(6) ? N6 N7 . 1.236(6) ? N7 N8 . 1.129(7) ? 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 N1 H1 O1 1_655 0.90(8) 2.10(8) 2.973(6) 163(7) N5 H5A O2 1_655 0.91(6) 2.13(6) 2.995(5) 160(5) C8 H8B O1 . 0.96 2.47 3.046(10) 118 C10 H10A O1 1_655 0.97 2.38 3.266(7) 151 C18 H18B N5 . 0.96 2.47 2.911(9) 108 C20 H20B O2 1_655 0.97 2.39 3.278(6) 152 C7 H7C Cg1 1_655 0.96 2.97 3.745(7) 138 C17 H17A Cg2 1_655 0.96 2.87 3.722(6) 148