#------------------------------------------------------------------------------ #$Date: 2022-11-24 12:09:55 +0200 (Thu, 24 Nov 2022) $ #$Revision: 279545 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/62/8106246.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_8106246 loop_ _publ_author_name 'Alotaibi, Mohammad Hayal' _publ_section_title ; Crystal structure of (E)-N′-(4-methoxybenzylidene)-5-methyl-1-(4-tolyl)-1H-1,2,3-triazole-4-carbohydrazide, C19H19N5O2 ; _journal_issue 4 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 649 _journal_page_last 650 _journal_paper_doi 10.1515/ncrs-2017-0421 _journal_volume 233 _journal_year 2018 _chemical_formula_sum 'C19 H19 N5 O2' _chemical_formula_weight 349.39 _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 _cell_angle_alpha 102.751(2) _cell_angle_beta 96.130(2) _cell_angle_gamma 103.079(2) _cell_formula_units_Z 2 _cell_length_a 6.6320(3) _cell_length_b 10.3272(5) _cell_length_c 13.0832(6) _cell_measurement_reflns_used 5998 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 33.08 _cell_measurement_theta_min 2.30 _cell_volume 839.63(7) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_unetI/netI 0.0845 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 10420 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 24.995 _diffrn_reflns_theta_max 24.995 _diffrn_reflns_theta_min 2.093 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS_Bruker_2014 _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.382 _exptl_crystal_description block _exptl_crystal_F_000 368 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.312 _exptl_crystal_size_min 0.183 _refine_diff_density_max 0.256 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.067 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 242 _refine_ls_number_reflns 2930 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0553 _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^)+(0.0757P)^2^+0.2060P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1384 _refine_ls_wR_factor_ref 0.1521 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2273 _reflns_number_total 2930 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file suppl_ncrs-2017-0421_suppl.cif _cod_data_source_block a_a _cod_database_code 8106246 _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_res_file ; a_a.res created by SHELXL-2014/7 TITL a_a.res in P-1 REM Old TITL mo_ot3_0m in P-1 REM SHELXT solution in P-1 REM R1 0.138, Rweak 0.007, Alpha 0.036, Orientation as input REM Formula found by SHELXT: C19 N5 O2 CELL 0.71073 6.6320 10.3272 13.0832 102.751 96.130 103.079 ZERR 2.000 0.0003 0.0005 0.0006 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 38 38 10 4 TEMP -173.15 L.S. 15 BOND $H LIST 4 ACTA CONF FMAP 2 OMIT -4 50 PLAN 20 WGHT 0.075700 0.206000 FVAR 1.27340 O1 4 0.656250 0.384239 0.310373 11.00000 0.02781 0.03193 = 0.03040 0.01805 0.01327 0.01495 O2 4 -0.182023 0.016138 0.679799 11.00000 0.02138 0.02953 = 0.02003 0.01507 0.00764 0.00816 N1 3 0.715735 0.674252 0.123650 11.00000 0.01749 0.01957 = 0.01576 0.00639 0.00673 0.00665 N2 3 0.542682 0.715768 0.150811 11.00000 0.02153 0.02984 = 0.02680 0.01468 0.01059 0.01116 N3 3 0.465865 0.643574 0.214526 11.00000 0.02120 0.02618 = 0.02353 0.01144 0.00811 0.00867 N4 3 0.369213 0.463329 0.341379 11.00000 0.02014 0.02445 = 0.02029 0.01142 0.00821 0.00782 N5 3 0.308704 0.376623 0.405175 11.00000 0.02190 0.02103 = 0.01645 0.00669 0.00602 0.00407 C1 1 0.833309 0.734904 0.052776 11.00000 0.02193 0.01601 = 0.01457 0.00410 0.00686 0.00641 C2 1 1.049360 0.782267 0.078048 11.00000 0.02274 0.02104 = 0.01462 0.00563 0.00199 0.00719 AFIX 43 H2A 2 1.120417 0.776081 0.143101 11.00000 -1.20000 AFIX 0 C3 1 1.161326 0.838586 0.008304 11.00000 0.01960 0.02133 = 0.02269 0.00674 0.00659 0.00541 AFIX 43 H3A 2 1.309700 0.871195 0.026189 11.00000 -1.20000 AFIX 0 C4 1 1.060834 0.848644 -0.088182 11.00000 0.03010 0.01483 = 0.01892 0.00568 0.01077 0.01035 C5 1 0.842772 0.801767 -0.110913 11.00000 0.02948 0.02307 = 0.01613 0.00878 0.00405 0.01100 AFIX 43 H5A 2 0.770862 0.809362 -0.175252 11.00000 -1.20000 AFIX 0 C6 1 0.728467 0.744468 -0.042132 11.00000 0.02137 0.02132 = 0.01977 0.00587 0.00374 0.00671 AFIX 43 H6A 2 0.580018 0.711999 -0.059489 11.00000 -1.20000 AFIX 0 C7 1 1.183470 0.904545 -0.165569 11.00000 0.03499 0.02821 = 0.02695 0.01250 0.01244 0.01057 AFIX 137 H7A 2 1.299941 0.982899 -0.126886 11.00000 -1.50000 H7B 2 1.091621 0.934502 -0.214165 11.00000 -1.50000 H7C 2 1.239126 0.832828 -0.206312 11.00000 -1.50000 AFIX 0 C8 1 0.920391 0.505452 0.155241 11.00000 0.03083 0.02916 = 0.03121 0.01515 0.01703 0.01625 AFIX 137 H8A 2 0.892706 0.423327 0.182713 11.00000 -1.50000 H8B 2 1.054714 0.568103 0.193015 11.00000 -1.50000 H8C 2 0.926438 0.478722 0.079178 11.00000 -1.50000 AFIX 0 C9 1 0.749260 0.575621 0.171668 11.00000 0.01786 0.01857 = 0.01320 0.00357 0.00220 0.00373 C10 1 0.588400 0.557074 0.229328 11.00000 0.01733 0.01829 = 0.01428 0.00326 0.00282 0.00538 C11 1 0.544127 0.460648 0.297130 11.00000 0.01866 0.02170 = 0.01566 0.00326 0.00434 0.00427 C12 1 0.124609 0.368776 0.429215 11.00000 0.02217 0.02256 = 0.01905 0.00681 0.00413 0.00754 AFIX 43 H12A 2 0.039181 0.419868 0.401889 11.00000 -1.20000 AFIX 0 C13 1 0.044793 0.282524 0.497888 11.00000 0.02061 0.01923 = 0.01454 0.00369 0.00465 0.00466 C14 1 0.171407 0.212414 0.545758 11.00000 0.01647 0.02436 = 0.01658 0.00308 0.00404 0.00617 AFIX 43 H14A 2 0.313464 0.224385 0.535500 11.00000 -1.20000 AFIX 0 C15 1 0.093285 0.127740 0.606512 11.00000 0.01986 0.02626 = 0.01663 0.00698 0.00288 0.01029 AFIX 43 H15A 2 0.181307 0.081461 0.638148 11.00000 -1.20000 AFIX 0 C16 1 -0.115336 0.108299 0.622750 11.00000 0.02318 0.02012 = 0.01039 0.00346 0.00415 0.00556 C17 1 -0.241372 0.180176 0.579187 11.00000 0.01829 0.02431 = 0.01923 0.00721 0.00699 0.00940 AFIX 43 H17A 2 -0.381459 0.171108 0.592221 11.00000 -1.20000 AFIX 0 C18 1 -0.160421 0.265326 0.516454 11.00000 0.02181 0.02476 = 0.02023 0.00832 0.00480 0.00987 AFIX 43 H18A 2 -0.247628 0.312755 0.485641 11.00000 -1.20000 AFIX 0 C19 1 -0.400273 -0.018611 0.686689 11.00000 0.02182 0.03033 = 0.02714 0.01631 0.00959 0.00511 AFIX 137 H19A 2 -0.432945 -0.098646 0.716427 11.00000 -1.50000 H19B 2 -0.483151 -0.040348 0.615597 11.00000 -1.50000 H19C 2 -0.434509 0.059313 0.732770 11.00000 -1.50000 AFIX 0 H1N4 2 0.286751 0.516720 0.324289 11.00000 0.04105 HKLF 4 REM a_a.res in P-1 REM R1 = 0.0553 for 2273 Fo > 4sig(Fo) and 0.0736 for all 2930 data REM 242 parameters refined using 0 restraints END WGHT 0.0750 0.2095 REM Highest difference peak 0.256, deepest hole -0.341, 1-sigma level 0.067 Q1 1 0.6442 0.5227 0.1813 11.00000 0.05 0.26 Q2 1 0.7842 0.8335 -0.0621 11.00000 0.05 0.25 Q3 1 0.5462 0.2996 0.3222 11.00000 0.05 0.23 Q4 1 -0.3432 0.3102 0.6453 11.00000 0.05 0.22 Q5 1 -0.0432 0.0978 0.5857 11.00000 0.05 0.21 Q6 1 0.1716 0.1571 0.4341 11.00000 0.05 0.21 Q7 1 1.2164 1.0794 -0.1786 11.00000 0.05 0.21 Q8 1 0.5449 0.7838 0.1262 11.00000 0.05 0.21 Q9 1 1.1246 0.7601 0.0317 11.00000 0.05 0.21 Q10 1 -0.3677 0.1946 0.6594 11.00000 0.05 0.20 Q11 1 1.0161 0.5011 0.0985 11.00000 0.05 0.20 Q12 1 0.9679 0.6864 0.1003 11.00000 0.05 0.19 Q13 1 0.7526 0.7801 -0.3036 11.00000 0.05 0.19 Q14 1 1.0730 0.5777 0.1533 11.00000 0.05 0.19 Q15 1 1.3758 0.9379 -0.1385 11.00000 0.05 0.19 Q16 1 0.7680 0.3820 0.2438 11.00000 0.05 0.19 Q17 1 0.8166 0.5440 0.1606 11.00000 0.05 0.19 Q18 1 0.5719 0.5211 0.2593 11.00000 0.05 0.18 Q19 1 0.2701 -0.0384 0.6732 11.00000 0.05 0.18 Q20 1 0.9160 0.7936 0.0636 11.00000 0.05 0.18 ; _shelx_res_checksum 21413 _shelx_hkl_file ; -1 0 0 860.51 102.99 -1 0 0 815.32 102.49 -1 0 0 869.31 102.79 1 0 0 838.82 102.99 1 0 0 690.73 102.49 1 0 0 856.11 102.79 -2 0 0 707.43 85.49 -2 0 0 678.83 85.99 -2 0 0 689.03 86.49 2 0 0 658.03 86.49 2 0 0 676.33 86.09 -3 0 0 1171.98 149.19 -3 0 0 1214.48 147.59 -3 0 0 1208.18 148.39 3 0 0 1161.78 148.49 3 0 0 1130.19 149.19 -4 0 0 345.97 44.20 -4 0 0 333.27 42.40 -4 0 0 330.67 45.20 4 0 0 336.07 45.90 -5 0 0 11.80 7.30 -5 0 0 5.80 9.60 -5 0 0 16.30 3.20 5 0 0 37.90 13.30 -6 0 0 -1.20 9.10 -6 0 0 7.10 9.90 -6 0 0 5.80 4.90 6 0 0 23.60 12.80 -7 0 0 34.40 5.30 -7 0 0 8.00 16.60 7 0 0 49.50 22.00 -8 0 0 52.99 26.20 8 0 0 39.90 29.90 -9 0 0 127.79 42.00 9 0 0 248.78 48.50 -10 1 0 38.20 47.20 9 -1 0 121.79 33.70 -9 1 0 77.49 36.00 8 -1 0 52.59 28.40 7 -1 0 25.00 15.30 -7 1 0 1.50 3.80 -7 1 0 9.90 15.20 -7 1 0 4.50 12.00 6 -1 0 47.40 17.70 -6 1 0 57.99 8.20 -6 1 0 36.00 15.10 -6 1 0 43.70 14.80 -6 1 0 31.20 15.90 5 -1 0 318.67 43.70 -5 1 0 296.97 42.60 -5 1 0 337.97 40.20 -5 1 0 301.77 45.60 -5 1 0 296.17 43.10 4 -1 0 24.20 8.30 4 -1 0 29.80 7.90 -4 1 0 27.20 7.80 -4 1 0 37.30 5.20 -4 1 0 17.40 7.90 -4 1 0 29.60 11.50 3 -1 0 2483.85 305.77 -3 1 0 2563.34 305.77 -3 1 0 2237.08 304.67 -3 1 0 2415.06 305.27 -3 1 0 2504.45 305.97 2 -1 0 674.63 86.69 2 -1 0 696.33 87.19 2 -1 0 684.13 87.19 -2 1 0 658.13 86.69 -2 1 0 730.53 87.19 -2 1 0 693.93 87.09 1 -1 0 6961.50 876.21 1 -1 0 7074.79 876.51 1 -1 0 7052.29 876.21 -1 1 0 7254.67 876.51 -1 1 0 6877.31 876.21 -1 1 0 6892.31 876.21 0 -1 0 595.44 75.09 -1 -1 0 786.92 108.39 -1 -1 0 921.71 108.99 1 1 0 861.01 108.89 1 1 0 903.81 108.39 -2 -1 0 20.80 6.80 -2 -1 0 24.90 3.70 -2 -1 0 26.00 4.00 2 1 0 20.80 5.60 2 1 0 25.10 3.70 -3 -1 0 736.63 87.49 -3 -1 0 732.63 87.19 -3 -1 0 694.53 88.89 3 1 0 637.44 87.19 3 1 0 668.83 89.09 -4 -1 0 66.79 9.90 -4 -1 0 115.49 16.10 -4 -1 0 83.29 11.50 4 1 0 65.19 14.20 -5 -1 0 102.29 13.70 5 1 0 123.69 20.70 -6 -1 0 151.38 27.30 6 1 0 193.98 29.50 -7 -1 0 -4.60 12.10 7 1 0 -18.10 19.30 -8 -1 0 56.59 28.60 8 1 0 158.38 35.60 -9 -1 0 28.50 35.10 9 1 0 -20.20 37.80 -10 2 0 -11.60 39.50 -9 2 0 97.79 33.70 8 -2 0 35.60 25.90 -8 2 0 71.79 23.30 7 -2 0 8.10 18.20 -7 2 0 9.70 15.80 -7 2 0 19.50 18.90 -7 2 0 13.40 6.50 6 -2 0 95.09 21.10 -6 2 0 73.19 16.20 -6 2 0 77.79 18.90 -6 2 0 90.09 18.90 5 -2 0 -10.60 9.90 5 -2 0 6.30 9.00 -5 2 0 -6.00 13.40 -5 2 0 -1.20 8.40 -5 2 0 17.00 10.80 -5 2 0 8.10 4.30 -5 2 0 3.10 9.30 4 -2 0 764.02 96.79 4 -2 0 767.22 96.89 -4 2 0 754.52 96.09 -4 2 0 808.22 96.89 -4 2 0 678.03 94.99 -4 2 0 780.12 96.79 3 -2 0 704.53 89.69 3 -2 0 688.63 90.29 3 -2 0 675.43 90.39 -3 2 0 716.03 89.89 -3 2 0 780.02 90.69 -3 2 0 688.93 90.09 2 -2 0 43.10 6.60 2 -2 0 43.30 7.00 2 -2 0 43.50 7.60 -2 2 0 32.80 5.30 -2 2 0 41.90 7.00 -2 2 0 43.20 7.70 -2 2 0 44.40 6.50 1 -2 0 9639.64 1191.88 1 -2 0 9999.00 1192.28 -1 2 0 9001.60 1192.08 0 -2 0 874.51 110.89 0 -2 0 866.91 110.49 0 2 0 907.81 110.89 -1 -2 0 239.08 32.40 1 2 0 240.58 32.10 1 2 0 249.97 32.60 1 2 0 278.27 32.00 -2 -2 0 915.21 132.49 -2 -2 0 1146.69 133.69 2 2 0 1159.78 132.09 2 2 0 999.20 133.19 -3 -2 0 23.40 7.60 3 2 0 26.20 8.30 -4 -2 0 29.60 14.00 4 2 0 32.50 5.80 4 2 0 28.70 11.50 5 2 0 166.68 28.40 -6 -2 0 43.90 18.00 6 2 0 113.79 19.90 -7 -2 0 135.09 28.50 7 2 0 117.19 28.20 -8 -2 0 128.09 32.10 8 2 0 202.78 35.70 -9 -2 0 55.59 39.60 9 2 0 34.70 32.00 -10 3 0 127.49 24.20 -10 3 0 67.99 45.50 -9 3 0 48.30 29.30 -8 3 0 18.50 15.30 -8 3 0 -8.00 7.50 7 -3 0 87.99 20.10 -7 3 0 99.59 13.90 -7 3 0 44.10 20.00 6 -3 0 345.57 47.60 -6 3 0 340.27 47.90 -6 3 0 327.47 42.20 -6 3 0 304.87 47.90 -6 3 0 306.37 46.10 5 -3 0 -0.10 7.70 5 -3 0 -8.10 9.70 -5 3 0 -7.60 12.00 -5 3 0 -3.50 10.20 -5 3 0 0.60 8.60 -5 3 0 20.40 8.60 -5 3 0 0.70 4.90 4 -3 0 712.83 89.59 4 -3 0 733.03 90.49 4 -3 0 701.73 90.89 -4 3 0 615.14 89.79 -4 3 0 685.03 90.49 -4 3 0 754.82 90.79 -4 3 0 730.53 89.79 3 -3 0 59.79 10.90 -3 3 0 45.30 9.60 -3 3 0 45.50 8.20 -3 3 0 38.20 6.10 -3 3 0 49.90 9.40 2 -3 0 551.14 80.69 2 -3 0 662.93 82.49 2 -3 0 604.54 81.59 -2 3 0 719.23 80.79 -2 3 0 649.24 81.49 -2 3 0 624.34 81.69 -2 3 0 720.43 82.59 1 -3 0 5130.89 676.33 1 -3 0 6223.18 675.63 1 -3 0 5136.99 676.53 -1 3 0 5417.66 676.63 -1 3 0 5137.79 675.53 0 -3 0 117.39 13.50 0 -3 0 108.09 14.20 0 3 0 105.79 14.30 0 3 0 84.59 13.20 -1 -3 0 565.64 65.29 1 3 0 494.15 64.99 1 3 0 536.25 65.49 1 3 0 426.96 64.99 1 3 0 558.44 64.99 -2 -3 0 21.10 5.60 -2 -3 0 26.30 6.10 2 3 0 16.90 3.70 -3 -3 0 36.60 8.80 -3 -3 0 34.00 11.20 3 3 0 33.20 9.90 3 3 0 38.70 5.90 -4 -3 0 -7.80 8.60 -4 -3 0 18.70 10.20 4 3 0 5.30 10.20 4 3 0 6.20 3.70 -5 -3 0 12.80 9.80 5 3 0 20.90 11.10 5 3 0 19.90 5.50 -6 -3 0 1.70 14.20 6 3 0 -2.50 15.90 -7 -3 0 412.06 67.99 7 3 0 526.15 69.09 -8 -3 0 -23.60 26.20 8 3 0 36.20 32.40 -9 -3 0 2.20 29.40 9 3 0 -5.60 42.30 -10 4 0 27.20 37.20 -10 4 0 25.50 18.20 -9 4 0 135.09 30.40 -9 4 0 147.99 35.50 -8 4 0 67.59 23.70 -8 4 0 78.29 15.10 -8 4 0 82.19 15.00 -7 4 0 49.60 17.60 -7 4 0 50.99 9.90 -7 4 0 49.30 11.00 -6 4 0 8.20 10.20 -6 4 0 15.60 7.60 -6 4 0 9.80 4.80 5 -4 0 2117.99 253.87 5 -4 0 2166.28 252.27 -5 4 0 1987.10 252.27 -5 4 0 2121.69 253.57 -5 4 0 1826.32 252.07 -5 4 0 1906.91 252.87 -5 4 0 1916.21 250.57 4 -4 0 531.25 66.69 4 -4 0 521.65 64.89 -4 4 0 553.64 66.59 -4 4 0 512.65 65.59 -4 4 0 446.66 64.29 -4 4 0 485.25 63.09 -4 4 0 495.05 64.89 3 -4 0 111.99 17.90 3 -4 0 132.89 19.00 -3 4 0 130.89 15.80 -3 4 0 126.09 18.20 -3 4 0 130.89 19.90 -3 4 0 101.39 16.40 -3 4 0 137.29 18.90 2 -4 0 -4.30 6.40 2 -4 0 2.30 2.00 -2 4 0 11.40 6.30 -2 4 0 4.50 3.80 -2 4 0 7.80 4.00 -2 4 0 10.20 1.90 -2 4 0 4.10 1.10 1 -4 0 4.90 2.20 1 -4 0 2.10 4.80 1 -4 0 1.30 3.80 -1 4 0 8.20 5.90 -1 4 0 1.60 1.60 0 -4 0 56.69 9.30 0 -4 0 72.19 8.60 0 4 0 44.50 7.90 0 4 0 61.49 9.90 -1 -4 0 36.20 5.80 1 4 0 29.00 5.40 1 4 0 18.70 4.60 1 4 0 29.20 5.50 -2 -4 0 67.99 11.30 2 4 0 67.99 9.80 2 4 0 60.79 11.70 -3 -4 0 197.78 28.00 3 4 0 184.68 28.80 3 4 0 205.88 25.80 4 4 0 93.79 18.60 4 4 0 116.79 15.50 -5 -4 0 -2.40 9.30 5 4 0 16.10 13.30 -6 -4 0 8.80 17.00 6 4 0 29.20 13.60 -7 -4 0 19.00 17.20 7 4 0 8.60 21.10 -8 -4 0 85.99 33.10 8 4 0 -15.40 32.70 -10 5 0 -37.90 36.10 -10 5 0 43.50 20.80 -9 5 0 43.30 15.50 -8 5 0 21.60 11.40 -8 5 0 25.70 18.70 -8 5 0 13.50 9.30 -7 5 0 5.70 13.10 -7 5 0 6.10 6.60 -7 5 0 5.50 9.00 6 -5 0 413.86 49.70 -6 5 0 385.66 47.30 -6 5 0 351.36 48.40 -6 5 0 319.37 49.70 5 -5 0 353.86 49.50 5 -5 0 425.36 52.99 -5 5 0 371.06 51.79 -5 5 0 433.76 57.59 -5 5 0 365.86 50.09 -5 5 0 321.17 48.70 -5 5 0 382.36 47.10 4 -5 0 115.89 19.40 4 -5 0 148.79 21.20 -4 5 0 134.99 16.10 -4 5 0 88.79 16.80 -4 5 0 116.19 19.60 -4 5 0 152.08 23.00 -4 5 0 144.59 21.10 3 -5 0 150.88 23.30 3 -5 0 169.48 24.90 -3 5 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-19 14.80 24.50 -3 -5 19 28.00 22.40 -3 -5 19 37.90 31.70 2 5 -19 19.20 22.70 -2 -5 19 17.10 21.70 1 5 -19 12.20 22.60 0 5 -19 13.70 23.40 -1 5 -19 1.40 24.70 -2 5 -19 5.40 27.80 2 -5 19 14.10 33.90 -4 -4 19 -20.70 22.70 -4 -4 19 36.20 22.90 3 4 -19 47.70 24.40 -3 -4 19 -35.70 26.30 -3 -4 19 18.50 19.60 2 4 -19 50.19 23.00 -2 -4 19 22.70 19.60 -2 -4 19 38.70 27.70 1 4 -19 1.70 20.30 0 4 -19 -2.60 16.60 -1 4 -19 35.30 24.80 -2 4 -19 17.20 27.70 2 -4 19 -31.80 35.60 -4 -3 19 108.29 29.00 -4 -3 19 154.58 32.80 3 3 -19 -17.80 22.00 -3 -3 19 3.40 20.20 -3 -3 19 -28.30 24.60 2 3 -19 -27.20 22.50 -2 -3 19 7.30 17.40 -2 -3 19 10.80 24.00 1 3 -19 -12.30 19.80 0 3 -19 -4.60 21.40 -1 3 -19 11.20 24.00 -2 3 -19 26.20 20.30 2 -3 19 -25.60 36.30 4 2 -19 35.00 25.20 4 2 -19 20.40 40.40 -4 -2 19 73.09 25.10 -4 -2 19 31.10 21.60 3 2 -19 -12.10 23.60 -3 -2 19 -16.90 18.80 -3 -2 19 7.30 27.00 2 2 -19 12.80 22.00 -2 -2 19 1.70 19.30 1 2 -19 5.40 22.30 -1 -2 19 2.10 17.30 0 2 -19 11.70 23.50 -1 2 -19 -0.70 21.20 -2 2 -19 37.20 21.70 4 1 -19 7.50 26.90 4 1 -19 -8.20 30.40 -4 -1 19 -3.30 21.90 -4 -1 19 6.10 28.90 3 1 -19 84.89 28.40 3 1 -19 127.79 34.90 -3 -1 19 94.59 32.30 -3 -1 19 134.59 26.00 2 1 -19 3.70 20.10 -2 -1 19 -15.20 18.50 1 1 -19 19.00 23.20 -1 -1 19 24.50 20.40 0 1 -19 17.20 24.00 -1 1 -19 96.89 25.00 4 0 -19 142.79 48.80 -4 0 19 114.49 26.80 -4 0 19 98.79 35.40 3 0 -19 -2.90 38.40 3 0 -19 22.70 24.00 -3 0 19 36.30 19.80 2 0 -19 -19.80 26.70 2 0 -19 19.40 22.70 -2 0 19 6.30 19.70 1 0 -19 0.40 24.50 -1 0 19 14.80 19.40 0 0 -19 -3.40 25.60 -1 0 -19 7.80 20.70 4 -1 -19 -0.70 43.30 -4 1 19 -6.40 21.30 3 -1 -19 47.70 31.00 3 -1 -19 -23.90 25.80 -3 1 19 -26.70 20.80 2 -1 -19 35.60 26.10 2 -1 -19 -35.80 40.10 -2 1 19 34.50 23.80 1 -1 -19 -23.00 39.80 1 -1 -19 18.20 26.70 -1 1 19 13.60 22.00 0 -1 -19 95.69 34.20 0 1 19 129.39 30.10 3 -2 -19 -2.10 42.60 -3 2 19 16.90 22.60 2 -2 -19 2.80 28.30 2 -2 -19 20.30 44.60 -2 2 19 -2.20 22.80 1 -2 -19 81.09 30.00 1 -2 -19 -35.20 43.90 -1 2 19 111.49 28.20 -2 -6 20 250.17 59.29 1 6 -20 53.89 30.40 0 6 -20 -25.10 26.30 2 5 -20 96.29 31.10 -2 -5 20 36.60 34.50 1 5 -20 -36.80 25.20 0 5 -20 51.49 28.80 -1 5 -20 30.10 22.80 3 4 -20 118.39 34.50 2 4 -20 12.90 25.60 -2 -4 20 21.70 23.60 1 4 -20 10.60 26.30 0 4 -20 48.80 29.00 -1 4 -20 76.49 31.20 3 3 -20 63.49 33.00 -3 -3 20 102.49 37.80 -3 -3 20 121.49 37.50 2 3 -20 55.09 29.50 1 3 -20 -21.80 23.80 0 3 -20 -29.80 19.60 3 2 -20 7.60 28.50 -3 -2 20 -18.00 23.20 -3 -2 20 3.10 30.90 2 2 -20 2.40 26.90 1 2 -20 18.10 25.60 0 2 -20 18.60 27.30 2 1 -20 47.40 21.30 -2 -1 20 2.50 36.20 1 1 -20 18.70 28.50 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 14930 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.6563(2) 0.38424(16) 0.31037(12) 0.0265(4) Uani 1 1 d . . . . . O2 O -0.1820(2) 0.01614(16) 0.67980(11) 0.0216(4) Uani 1 1 d . . . . . N1 N 0.7157(3) 0.67425(18) 0.12365(13) 0.0167(4) Uani 1 1 d . . . . . N2 N 0.5427(3) 0.7158(2) 0.15081(14) 0.0236(5) Uani 1 1 d . . . . . N3 N 0.4659(3) 0.64357(19) 0.21453(14) 0.0220(5) Uani 1 1 d . . . . . N4 N 0.3692(3) 0.46333(19) 0.34138(14) 0.0200(4) Uani 1 1 d . . . . . N5 N 0.3087(3) 0.37662(18) 0.40517(13) 0.0195(4) Uani 1 1 d . . . . . C1 C 0.8333(3) 0.7349(2) 0.05278(15) 0.0169(5) Uani 1 1 d . . . . . C2 C 1.0494(3) 0.7823(2) 0.07805(16) 0.0191(5) Uani 1 1 d . . . . . H2A H 1.1204 0.7761 0.1431 0.023 Uiso 1 1 calc R U . . . C3 C 1.1613(3) 0.8386(2) 0.00830(17) 0.0208(5) Uani 1 1 d . . . . . H3A H 1.3097 0.8712 0.0262 0.025 Uiso 1 1 calc R U . . . C4 C 1.0608(3) 0.8486(2) -0.08818(16) 0.0198(5) Uani 1 1 d . . . . . C5 C 0.8428(4) 0.8018(2) -0.11091(16) 0.0215(5) Uani 1 1 d . . . . . H5A H 0.7709 0.8094 -0.1753 0.026 Uiso 1 1 calc R U . . . C6 C 0.7285(3) 0.7445(2) -0.04213(16) 0.0205(5) Uani 1 1 d . . . . . H6A H 0.5800 0.7120 -0.0595 0.025 Uiso 1 1 calc R U . . . C7 C 1.1835(4) 0.9045(3) -0.16557(18) 0.0282(6) Uani 1 1 d . . . . . H7A H 1.2999 0.9829 -0.1269 0.042 Uiso 1 1 calc R U . . . H7B H 1.0916 0.9345 -0.2142 0.042 Uiso 1 1 calc R U . . . H7C H 1.2391 0.8328 -0.2063 0.042 Uiso 1 1 calc R U . . . C8 C 0.9204(4) 0.5055(2) 0.15524(18) 0.0268(6) Uani 1 1 d . . . . . H8A H 0.8927 0.4233 0.1827 0.040 Uiso 1 1 calc R U . . . H8B H 1.0547 0.5681 0.1930 0.040 Uiso 1 1 calc R U . . . H8C H 0.9264 0.4787 0.0792 0.040 Uiso 1 1 calc R U . . . C9 C 0.7493(3) 0.5756(2) 0.17167(15) 0.0168(5) Uani 1 1 d . . . . . C10 C 0.5884(3) 0.5571(2) 0.22933(15) 0.0166(5) Uani 1 1 d . . . . . C11 C 0.5441(3) 0.4606(2) 0.29713(16) 0.0190(5) Uani 1 1 d . . . . . C12 C 0.1246(3) 0.3688(2) 0.42921(16) 0.0207(5) Uani 1 1 d . . . . . H12A H 0.0392 0.4199 0.4019 0.025 Uiso 1 1 calc R U . . . C13 C 0.0448(3) 0.2825(2) 0.49789(16) 0.0182(5) Uani 1 1 d . . . . . C14 C 0.1714(3) 0.2124(2) 0.54576(16) 0.0192(5) Uani 1 1 d . . . . . H14A H 0.3135 0.2244 0.5355 0.023 Uiso 1 1 calc R U . . . C15 C 0.0933(3) 0.1277(2) 0.60651(16) 0.0199(5) Uani 1 1 d . . . . . H15A H 0.1813 0.0815 0.6381 0.024 Uiso 1 1 calc R U . . . C16 C -0.1153(3) 0.1083(2) 0.62275(15) 0.0179(5) Uani 1 1 d . . . . . C17 C -0.2414(3) 0.1802(2) 0.57919(16) 0.0194(5) Uani 1 1 d . . . . . H17A H -0.3815 0.1711 0.5922 0.023 Uiso 1 1 calc R U . . . C18 C -0.1604(3) 0.2653(2) 0.51645(16) 0.0211(5) Uani 1 1 d . . . . . H18A H -0.2476 0.3128 0.4856 0.025 Uiso 1 1 calc R U . . . C19 C -0.4003(3) -0.0186(2) 0.68669(18) 0.0248(5) Uani 1 1 d . . . . . H19A H -0.4329 -0.0986 0.7164 0.037 Uiso 1 1 calc R U . . . H19B H -0.4832 -0.0403 0.6156 0.037 Uiso 1 1 calc R U . . . H19C H -0.4345 0.0593 0.7328 0.037 Uiso 1 1 calc R U . . . H1N4 H 0.287(4) 0.517(3) 0.324(2) 0.041(8) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0278(9) 0.0319(10) 0.0304(9) 0.0181(8) 0.0133(7) 0.0149(8) O2 0.0214(8) 0.0295(9) 0.0200(8) 0.0151(7) 0.0076(6) 0.0082(7) N1 0.0175(9) 0.0196(10) 0.0158(9) 0.0064(8) 0.0067(7) 0.0067(8) N2 0.0215(10) 0.0298(11) 0.0268(10) 0.0147(9) 0.0106(8) 0.0112(9) N3 0.0212(10) 0.0262(11) 0.0235(10) 0.0114(9) 0.0081(8) 0.0087(8) N4 0.0201(10) 0.0245(11) 0.0203(10) 0.0114(8) 0.0082(8) 0.0078(9) N5 0.0219(10) 0.0210(10) 0.0164(9) 0.0067(8) 0.0060(8) 0.0041(8) C1 0.0219(12) 0.0160(11) 0.0146(10) 0.0041(9) 0.0069(9) 0.0064(9) C2 0.0227(12) 0.0210(12) 0.0146(10) 0.0056(9) 0.0020(9) 0.0072(9) C3 0.0196(12) 0.0213(12) 0.0227(11) 0.0067(10) 0.0066(9) 0.0054(9) C4 0.0301(13) 0.0148(11) 0.0189(11) 0.0057(9) 0.0108(9) 0.0104(10) C5 0.0295(13) 0.0231(12) 0.0161(11) 0.0088(9) 0.0040(9) 0.0110(10) C6 0.0214(12) 0.0213(12) 0.0198(11) 0.0059(9) 0.0037(9) 0.0067(9) C7 0.0350(14) 0.0282(14) 0.0269(12) 0.0125(11) 0.0124(11) 0.0106(11) C8 0.0308(13) 0.0292(13) 0.0312(13) 0.0151(11) 0.0170(11) 0.0163(11) C9 0.0179(11) 0.0186(11) 0.0132(10) 0.0036(9) 0.0022(8) 0.0037(9) C10 0.0173(11) 0.0183(11) 0.0143(10) 0.0033(9) 0.0028(9) 0.0054(9) C11 0.0187(11) 0.0217(12) 0.0157(11) 0.0033(9) 0.0043(9) 0.0043(9) C12 0.0222(12) 0.0226(12) 0.0191(11) 0.0068(9) 0.0041(9) 0.0075(10) C13 0.0206(12) 0.0192(12) 0.0145(10) 0.0037(9) 0.0047(9) 0.0047(9) C14 0.0165(11) 0.0244(12) 0.0166(11) 0.0031(9) 0.0040(9) 0.0062(9) C15 0.0199(12) 0.0263(13) 0.0166(11) 0.0070(10) 0.0029(9) 0.0103(10) C16 0.0232(12) 0.0201(12) 0.0104(10) 0.0035(9) 0.0041(9) 0.0056(9) C17 0.0183(12) 0.0243(12) 0.0192(11) 0.0072(9) 0.0070(9) 0.0094(10) C18 0.0218(12) 0.0248(12) 0.0202(11) 0.0083(10) 0.0048(9) 0.0099(10) C19 0.0218(12) 0.0303(13) 0.0271(12) 0.0163(11) 0.0096(10) 0.0051(10) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C16 O2 C19 117.55(16) . . C9 N1 N2 111.05(16) . . C9 N1 C1 129.13(17) . . N2 N1 C1 119.82(16) . . N3 N2 N1 106.88(16) . . N2 N3 C10 109.05(16) . . C11 N4 N5 119.87(18) . . C11 N4 H1N4 119.6(16) . . N5 N4 H1N4 120.3(16) . . C12 N5 N4 115.82(18) . . C2 C1 C6 120.35(19) . . C2 C1 N1 120.22(18) . . C6 C1 N1 119.42(19) . . C3 C2 C1 119.69(19) . . C3 C2 H2A 120.2 . . C1 C2 H2A 120.2 . . C2 C3 C4 121.4(2) . . C2 C3 H3A 119.3 . . C4 C3 H3A 119.3 . . C5 C4 C3 117.68(19) . . C5 C4 C7 121.09(19) . . C3 C4 C7 121.2(2) . . C6 C5 C4 121.63(19) . . C6 C5 H5A 119.2 . . C4 C5 H5A 119.2 . . C5 C6 C1 119.3(2) . . C5 C6 H6A 120.4 . . C1 C6 H6A 120.4 . . C4 C7 H7A 109.5 . . C4 C7 H7B 109.5 . . H7A C7 H7B 109.5 . . C4 C7 H7C 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . C9 C8 H8A 109.5 . . C9 C8 H8B 109.5 . . H8A C8 H8B 109.5 . . C9 C8 H8C 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . N1 C9 C10 103.84(18) . . N1 C9 C8 124.23(18) . . C10 C9 C8 131.9(2) . . N3 C10 C9 109.18(18) . . N3 C10 C11 122.82(18) . . C9 C10 C11 128.00(18) . . O1 C11 N4 123.7(2) . . O1 C11 C10 122.18(18) . . N4 C11 C10 114.14(18) . . N5 C12 C13 120.9(2) . . N5 C12 H12A 119.6 . . C13 C12 H12A 119.6 . . C18 C13 C14 118.1(2) . . C18 C13 C12 120.60(19) . . C14 C13 C12 121.33(19) . . C15 C14 C13 121.01(19) . . C15 C14 H14A 119.5 . . C13 C14 H14A 119.5 . . C14 C15 C16 120.6(2) . . C14 C15 H15A 119.7 . . C16 C15 H15A 119.7 . . O2 C16 C17 124.37(19) . . O2 C16 C15 116.24(18) . . C17 C16 C15 119.4(2) . . C18 C17 C16 119.45(19) . . C18 C17 H17A 120.3 . . C16 C17 H17A 120.3 . . C13 C18 C17 121.5(2) . . C13 C18 H18A 119.3 . . C17 C18 H18A 119.3 . . O2 C19 H19A 109.5 . . O2 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . O2 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 C11 1.226(2) . O2 C16 1.361(2) . O2 C19 1.428(3) . N1 C9 1.355(3) . N1 N2 1.367(2) . N1 C1 1.432(3) . N2 N3 1.305(2) . N3 C10 1.366(3) . N4 C11 1.354(3) . N4 N5 1.378(2) . N4 H1N4 0.90(3) . N5 C12 1.282(3) . C1 C2 1.383(3) . C1 C6 1.391(3) . C2 C3 1.381(3) . C2 H2A 0.9500 . C3 C4 1.399(3) . C3 H3A 0.9500 . C4 C5 1.394(3) . C4 C7 1.497(3) . C5 C6 1.383(3) . C5 H5A 0.9500 . C6 H6A 0.9500 . C7 H7A 0.9800 . C7 H7B 0.9800 . C7 H7C 0.9800 . C8 C9 1.488(3) . C8 H8A 0.9800 . C8 H8B 0.9800 . C8 H8C 0.9800 . C9 C10 1.374(3) . C10 C11 1.476(3) . C12 C13 1.457(3) . C12 H12A 0.9500 . C13 C18 1.387(3) . C13 C14 1.409(3) . C14 C15 1.362(3) . C14 H14A 0.9500 . C15 C16 1.398(3) . C15 H15A 0.9500 . C16 C17 1.393(3) . C17 C18 1.391(3) . C17 H17A 0.9500 . C18 H18A 0.9500 . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C9 N1 N2 N3 -0.6(2) . . . . C1 N1 N2 N3 179.37(17) . . . . N1 N2 N3 C10 0.5(2) . . . . C11 N4 N5 C12 -168.70(19) . . . . C9 N1 C1 C2 -48.6(3) . . . . N2 N1 C1 C2 131.5(2) . . . . C9 N1 C1 C6 130.8(2) . . . . N2 N1 C1 C6 -49.1(3) . . . . C6 C1 C2 C3 -0.4(3) . . . . N1 C1 C2 C3 178.98(18) . . . . C1 C2 C3 C4 -0.2(3) . . . . C2 C3 C4 C5 1.0(3) . . . . C2 C3 C4 C7 -177.50(19) . . . . C3 C4 C5 C6 -1.3(3) . . . . C7 C4 C5 C6 177.17(19) . . . . C4 C5 C6 C1 0.8(3) . . . . C2 C1 C6 C5 0.0(3) . . . . N1 C1 C6 C5 -179.31(18) . . . . N2 N1 C9 C10 0.4(2) . . . . C1 N1 C9 C10 -179.55(19) . . . . N2 N1 C9 C8 177.6(2) . . . . C1 N1 C9 C8 -2.3(3) . . . . N2 N3 C10 C9 -0.3(2) . . . . N2 N3 C10 C11 -179.80(19) . . . . N1 C9 C10 N3 -0.1(2) . . . . C8 C9 C10 N3 -177.0(2) . . . . N1 C9 C10 C11 179.4(2) . . . . C8 C9 C10 C11 2.5(4) . . . . N5 N4 C11 O1 -0.1(3) . . . . N5 N4 C11 C10 179.03(17) . . . . N3 C10 C11 O1 -179.5(2) . . . . C9 C10 C11 O1 1.1(4) . . . . N3 C10 C11 N4 1.4(3) . . . . C9 C10 C11 N4 -178.0(2) . . . . N4 N5 C12 C13 -178.80(17) . . . . N5 C12 C13 C18 -174.6(2) . . . . N5 C12 C13 C14 4.3(3) . . . . C18 C13 C14 C15 1.5(3) . . . . C12 C13 C14 C15 -177.4(2) . . . . C13 C14 C15 C16 0.1(3) . . . . C19 O2 C16 C17 6.2(3) . . . . C19 O2 C16 C15 -172.48(18) . . . . C14 C15 C16 O2 176.56(18) . . . . C14 C15 C16 C17 -2.2(3) . . . . O2 C16 C17 C18 -175.86(18) . . . . C15 C16 C17 C18 2.8(3) . . . . C14 C13 C18 C17 -0.9(3) . . . . C12 C13 C18 C17 178.05(19) . . . . C16 C17 C18 C13 -1.3(3) . . . .