#------------------------------------------------------------------------------ #$Date: 2020-10-06 12:20:44 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257606 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/04/7240411.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_7240411 loop_ _publ_author_name 'Charpe, Vaibhav Pramod' 'Sagadevan, Arunachalam' 'Hwang, Kuo Chu' _publ_section_title ; Visible light-induced aerobic oxidation of diarylalkynes to \a-diketones catalyzed by copper-superoxo at room temperature ; _journal_issue 14 _journal_name_full 'Green Chemistry' _journal_page_first 4426 _journal_page_last 4432 _journal_paper_doi 10.1039/D0GC00975J _journal_volume 22 _journal_year 2020 _chemical_formula_sum 'C20 H14 N2' _chemical_formula_weight 282.33 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _audit_update_record ; 2018-07-30 deposited with the CCDC. 2020-04-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.035(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.0178(13) _cell_length_b 10.934(2) _cell_length_c 22.509(5) _cell_measurement_reflns_used 3876 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.5996 _cell_measurement_theta_min 2.6021 _cell_volume 1475.3(5) _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.990 _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 0.0501 _diffrn_reflns_av_unetI/netI 0.0512 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 11963 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.698 _diffrn_reflns_theta_min 1.816 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.6897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Lump _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.304 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.064 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 3101 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0452 _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^)+(0.0654P)^2^+0.2648P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1197 _refine_ls_wR_factor_ref 0.1278 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2486 _reflns_number_total 3101 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0gc00975j2.cif _cod_data_source_block mo_170751LT_0m _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 7240411--7240415.cif. Adding full bibliography for 7240411--7240415.cif. ; _cod_original_cell_volume 1475.3(6) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7240411 _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. ; _shelxl_version_number 2014/6 _shelx_res_file ; TITL mo_170751LT_0m in P2(1)/n CELL 0.71073 6.0178 10.9336 22.5092 90.000 95.035 90.000 ZERR 4.00 0.0013 0.0024 0.0050 0.000 0.004 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N UNIT 80 56 8 TEMP -173 ACTA L.S. 4 FMAP 2 PLAN 5 BOND $H WGHT 0.065400 0.264800 FVAR 0.78749 N1 3 0.509649 0.013151 0.241139 11.00000 0.01718 0.02015 = 0.01674 -0.00066 0.00300 0.00031 N2 3 0.734698 0.207011 0.189763 11.00000 0.01775 0.01929 = 0.01906 -0.00032 0.00199 0.00075 C1 1 1.092667 0.156047 0.326849 11.00000 0.01979 0.02356 = 0.02385 -0.00608 -0.00210 0.00246 AFIX 43 H1 2 1.227694 0.186159 0.346576 11.00000 -1.20000 AFIX 0 C2 1 0.973245 0.062751 0.353725 11.00000 0.02691 0.02557 = 0.01737 -0.00156 -0.00039 0.00573 AFIX 43 H3 2 1.029400 0.030857 0.391341 11.00000 -1.20000 AFIX 0 C3 1 0.778198 0.017661 0.326457 11.00000 0.02564 0.02197 = 0.01860 0.00054 0.00389 0.00107 AFIX 43 H14 2 0.698777 -0.044448 0.345178 11.00000 -1.20000 AFIX 0 C4 1 0.695624 0.064255 0.270134 11.00000 0.01723 0.01929 = 0.01788 -0.00242 0.00301 0.00262 C5 1 0.440652 0.057091 0.188127 11.00000 0.01587 0.01877 = 0.01680 -0.00159 0.00493 0.00163 C6 1 0.251319 -0.009594 0.155566 11.00000 0.01666 0.01628 = 0.02031 0.00065 0.00151 0.00164 C7 1 0.240492 -0.029736 0.094004 11.00000 0.02550 0.02401 = 0.02036 0.00127 0.00344 -0.00296 AFIX 43 H10 2 0.354630 0.001033 0.071504 11.00000 -1.20000 AFIX 0 C8 1 0.063047 -0.094677 0.065725 11.00000 0.03305 0.02831 = 0.02029 -0.00138 -0.00379 -0.00191 AFIX 43 H11 2 0.057099 -0.108829 0.023974 11.00000 -1.20000 AFIX 0 C9 1 -0.104901 -0.138815 0.097998 11.00000 0.02232 0.02353 = 0.03320 -0.00295 -0.00529 -0.00447 AFIX 43 H2 2 -0.228160 -0.181032 0.078278 11.00000 -1.20000 AFIX 0 C10 1 0.548528 0.160687 0.163577 11.00000 0.01701 0.01837 = 0.01805 -0.00103 0.00392 0.00027 C11 1 0.814343 0.157929 0.243298 11.00000 0.01849 0.01776 = 0.01683 -0.00212 0.00305 0.00345 C12 1 1.015207 0.203362 0.272588 11.00000 0.01920 0.01977 = 0.02195 -0.00269 0.00398 -0.00013 AFIX 43 H4 2 1.095746 0.266216 0.254752 11.00000 -1.20000 AFIX 0 C13 1 0.457429 0.226164 0.108640 11.00000 0.01905 0.01775 = 0.01838 -0.00005 0.00015 -0.00437 C14 1 0.595092 0.247379 0.063217 11.00000 0.01887 0.02736 = 0.02202 0.00072 0.00243 -0.00251 AFIX 43 H9 2 0.742525 0.215515 0.066437 11.00000 -1.20000 AFIX 0 C15 1 0.519077 0.314683 0.013214 11.00000 0.02717 0.03301 = 0.01852 0.00291 0.00412 -0.00650 AFIX 43 H8 2 0.613479 0.327678 -0.017879 11.00000 -1.20000 AFIX 0 C16 1 0.305611 0.362810 0.008729 11.00000 0.02952 0.02598 = 0.01862 0.00410 -0.00471 -0.00559 AFIX 43 H7 2 0.253780 0.410026 -0.025117 11.00000 -1.20000 AFIX 0 C17 1 0.167720 0.341773 0.053889 11.00000 0.02060 0.02651 = 0.02674 0.00133 -0.00351 -0.00140 AFIX 43 H6 2 0.021127 0.374778 0.050814 11.00000 -1.20000 AFIX 0 C18 1 0.241701 0.273063 0.103467 11.00000 0.01935 0.02562 = 0.02171 0.00129 0.00331 -0.00328 AFIX 43 H5 2 0.145225 0.258011 0.133879 11.00000 -1.20000 AFIX 0 C19 1 0.085294 -0.058541 0.187865 11.00000 0.01922 0.01839 = 0.02056 0.00064 0.00333 0.00291 AFIX 43 H13 2 0.094561 -0.048739 0.229945 11.00000 -1.20000 AFIX 0 C20 1 -0.093104 -0.121338 0.159251 11.00000 0.01795 0.02247 = 0.03225 0.00113 0.00476 -0.00145 AFIX 43 H12 2 -0.207470 -0.152468 0.181566 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM mo_170751LT_0m in P2(1)/n REM R1 = 0.0452 for 2486 Fo > 4sig(Fo) and 0.0571 for all 3101 data REM 199 parameters refined using 0 restraints END WGHT 0.0654 0.2671 REM Highest difference peak 0.304, deepest hole -0.275, 1-sigma level 0.064 Q1 1 0.2446 0.3668 0.0325 11.00000 0.05 0.30 Q2 1 0.3540 0.0132 0.1671 11.00000 0.05 0.28 Q3 1 0.4879 0.1953 0.1369 11.00000 0.05 0.27 Q4 1 0.3864 0.3175 0.0023 11.00000 0.05 0.25 Q5 1 0.5321 0.0921 0.1632 11.00000 0.05 0.24 ; _shelx_res_checksum 32452 _shelx_hkl_file ; -1 0 0 0.49883 0.73876 4 -2 0 0 96.9988 6.59312 4 -4 0 0 1379.81 75.4104 4 -5 0 0 -0.5334 1.67864 1 -5 0 0 1.04813 1.40713 1 -6 0 0 274.434 16.6057 1 -7 0 0 0.48348 2.11977 1 0 -1 0 -0.0881 0.39827 1 0 1 0 0.13307 0.39694 1 -1 -1 0 1156.46 62.8754 1 -1 -1 0 1203.56 62.7611 4 -2 -1 0 1345.77 68.0980 1 -2 -1 0 1241.60 67.1322 3 -2 -1 0 1236.09 67.9026 4 -2 -1 0 1240.37 67.6003 1 -3 -1 0 67.2000 5.61493 1 -3 -1 0 79.2949 5.93302 4 -3 -1 0 75.0904 5.24885 1 -4 -1 0 49.5244 5.08676 4 -4 -1 0 55.8295 4.44494 1 -4 -1 0 38.3700 4.51405 1 -5 -1 0 113.673 8.80762 1 -5 -1 0 114.869 9.27219 4 -5 -1 0 108.810 8.18472 1 -6 -1 0 22.6389 4.01717 1 -7 -1 0 44.9974 5.99834 1 0 -2 0 4.14916 1.37097 1 0 2 0 6.68263 1.55361 1 -1 -2 0 2808.54 149.922 4 -1 -2 0 2712.58 150.629 1 -1 2 0 2739.08 149.967 1 1 2 0 3033.67 150.980 1 -1 2 0 2885.53 150.045 1 -2 -2 0 30.1278 3.15176 4 -2 -2 0 27.1188 3.31878 1 -3 -2 0 964.046 51.8144 4 -3 -2 0 943.160 50.7024 3 -3 -2 0 932.027 51.7970 1 -4 -2 0 66.7811 6.13187 1 -4 -2 0 64.0944 6.13576 4 -4 -2 0 73.8018 4.57190 3 -5 -2 0 13.2593 3.19454 1 -5 -2 0 12.8233 3.45939 4 -6 -2 0 2.46957 2.49639 1 -7 -2 0 123.233 10.6764 1 0 -3 0 -1.7774 1.50648 1 -1 -3 0 1819.38 95.6582 1 -1 3 0 1753.59 93.7982 2 -1 3 0 1792.31 95.1058 1 1 3 0 1737.67 95.8362 1 -2 -3 0 458.747 26.3004 1 -2 -3 0 460.398 25.2704 4 2 3 0 407.963 26.3035 1 -2 3 0 463.230 25.0287 1 -2 3 0 468.862 24.9458 1 -3 -3 0 23.4990 3.43057 4 -3 -3 0 32.0179 4.30510 1 -4 -3 0 89.5524 7.97223 1 -4 -3 0 90.4840 7.51933 4 -4 -3 0 101.852 6.45369 3 -5 -3 0 2.18928 2.40477 1 -5 -3 0 0.29275 2.00840 4 -6 -3 0 68.8888 7.71100 1 -6 -3 0 77.0149 7.86259 4 -7 -3 0 18.0396 4.91583 1 0 -4 0 277.299 17.0685 1 1 -4 0 39.0197 4.02490 1 -1 -4 0 39.9167 4.68588 1 -1 4 0 33.5834 2.76251 2 -2 -4 0 179.034 11.2842 4 -2 -4 0 178.727 12.7350 1 -2 4 0 192.955 11.6908 1 -2 4 0 188.948 11.8583 1 2 4 0 185.794 13.3255 1 -3 -4 0 280.642 18.3878 1 -3 -4 0 290.796 17.1426 4 3 4 0 240.337 18.4219 1 -3 4 0 301.758 16.6130 1 -3 4 0 304.451 16.8354 1 -4 -4 0 983.133 53.8385 4 -4 -4 0 987.872 52.9637 3 -4 -4 0 943.405 54.8581 1 -5 -4 0 74.1369 7.99288 1 -5 -4 0 81.8997 7.36860 4 -6 -4 0 38.6459 5.77751 4 -6 -4 0 37.3605 6.47935 1 -7 -4 0 -2.3006 2.74148 1 0 -5 0 4.42781 2.27943 1 0 5 0 -0.6487 1.72428 1 -1 -5 0 463.172 26.4572 1 1 -5 0 422.340 25.2397 1 -1 5 0 406.092 25.6996 1 1 5 0 428.861 26.5951 1 -1 5 0 439.118 23.6688 2 -2 -5 0 645.340 35.6583 4 -2 -5 0 650.723 37.9416 1 -2 5 0 677.173 37.1691 1 2 5 0 611.336 38.3847 1 -3 -5 0 6.86409 2.28429 4 -3 -5 0 6.18414 3.26782 1 -3 5 0 2.36176 1.86779 1 -3 5 0 8.88086 2.54604 1 3 5 0 6.03330 3.50980 1 -4 -5 0 872.430 51.0097 1 -4 -5 0 841.129 48.9370 4 -4 5 0 926.670 48.9865 1 -4 5 0 877.568 48.3324 1 -5 -5 0 35.1973 5.30867 4 -5 -5 0 31.8986 6.03577 1 -5 -5 0 43.3342 5.25234 3 -5 5 0 38.5556 4.41325 1 -6 -5 0 -0.6469 3.16385 1 -6 -5 0 1.82908 2.63110 4 -7 -5 0 10.0732 4.69331 1 0 -6 0 640.478 35.7639 1 0 6 0 569.665 36.0654 1 -1 -6 0 919.774 51.6257 1 1 -6 0 841.681 50.2823 1 -1 6 0 884.137 48.4470 2 -1 6 0 914.473 51.5375 1 1 6 0 942.922 52.3411 1 -2 -6 0 179.639 11.4779 4 -2 -6 0 172.942 13.8917 1 -2 6 0 187.591 13.5565 1 2 6 0 196.076 14.7666 1 -3 -6 0 139.547 9.29812 4 -3 -6 0 136.246 11.7057 1 -3 6 0 123.023 10.3541 1 -4 -6 0 85.8971 7.47552 4 -4 -6 0 89.4652 9.60604 1 -4 6 0 92.9072 8.32691 1 -5 -6 0 35.3134 6.71648 1 -5 -6 0 51.2920 5.66717 3 -5 -6 0 36.9717 5.46686 4 -5 6 0 41.3944 5.70135 1 -6 -6 0 62.8087 9.32125 1 -6 -6 0 65.1628 7.66262 4 -6 6 0 55.6721 6.33040 1 0 -7 0 -2.5403 2.17488 1 0 7 0 0.52126 2.20270 1 -1 -7 0 10.6782 3.95392 1 1 -7 0 8.59195 3.17230 1 -1 7 0 9.04079 3.49315 1 -1 7 0 6.03495 1.75723 2 1 7 0 10.4145 3.86445 1 -2 -7 0 12.1709 2.89108 4 -2 -7 0 12.7516 4.49637 1 2 7 0 25.1339 5.81377 1 -2 7 0 21.1122 4.91169 1 -3 -7 0 705.647 37.3589 4 -3 -7 0 699.245 40.9893 1 3 7 0 574.399 40.8681 1 -3 7 0 670.211 39.6899 1 -4 -7 0 1.51819 2.13789 4 -4 -7 0 2.99035 3.54503 1 -4 7 0 0.09846 2.75670 1 -5 -7 0 4.56327 2.80130 3 -5 -7 0 9.16170 3.03567 4 -5 -7 0 0.11128 3.11433 1 -5 7 0 1.32119 2.70603 1 -6 -7 0 33.5361 7.35969 1 -6 -7 0 37.6411 5.95283 4 -6 7 0 28.9333 5.55592 1 0 -8 0 0.18124 3.07719 1 0 8 0 2.27158 1.58622 2 0 8 0 -1.0053 2.52865 1 -1 -8 0 65.2814 8.40248 1 1 -8 0 62.1607 7.57470 1 -1 8 0 64.9093 8.65593 1 -1 8 0 62.1426 5.09890 2 1 8 0 71.8376 9.02769 1 -2 -8 0 123.128 12.0860 1 -2 -8 0 127.428 8.76305 4 2 8 0 116.360 12.3910 1 -2 8 0 114.553 11.6585 1 -3 -8 0 26.6831 3.95183 4 -3 -8 0 20.6570 5.99656 1 -4 -8 0 29.5004 6.68870 1 -4 -8 0 37.9309 4.91355 4 -4 8 0 25.6076 5.90049 1 -5 -8 0 0.35609 3.46340 1 -5 -8 0 2.71420 2.74951 3 -5 -8 0 2.03173 2.42160 4 -5 8 0 -4.1292 2.36910 1 -6 -8 0 55.0723 7.14781 4 -6 -8 0 51.6469 9.43646 1 -6 8 0 46.5775 7.65929 1 0 -9 0 1.26664 3.56225 1 0 9 0 0.20120 3.11727 1 -1 -9 0 27.4657 6.40053 1 1 -9 0 25.6582 8.54034 1 1 9 0 17.4872 5.80300 1 -1 9 0 28.9732 3.49292 2 -1 9 0 19.6442 5.69385 1 -2 -9 0 74.3061 6.43039 4 -2 -9 0 70.8678 10.2349 1 -2 9 0 46.9310 8.76857 1 -2 9 0 83.3611 4.95828 2 -3 -9 0 57.0480 9.19147 1 -3 -9 0 42.6359 4.86936 4 3 9 0 11.7943 6.21767 1 -3 9 0 25.7197 6.52055 1 -4 -9 0 279.939 17.2560 4 -4 -9 0 290.926 21.8681 1 -4 9 0 242.782 20.5159 1 -5 -9 0 2.23814 2.92918 3 -5 -9 0 -0.4281 3.91341 1 -5 -9 0 4.68330 2.64508 4 -5 9 0 1.86833 3.32716 1 0 -10 0 223.964 16.8061 1 0 10 0 151.357 16.1657 1 -1 -10 0 61.6704 9.43524 1 1 10 0 23.3199 7.26829 1 -1 10 0 45.0372 4.55886 2 -1 10 0 26.4846 6.98899 1 -2 -10 0 3.90148 2.68338 4 -2 -10 0 -0.9728 3.76801 1 2 10 0 9.32279 5.97610 1 -2 10 0 7.66699 4.70828 1 -3 -10 0 420.861 29.4083 1 -3 -10 0 441.788 24.2953 4 -3 10 0 353.672 28.3932 1 -4 -10 0 319.738 18.1459 4 -4 -10 0 297.951 22.9801 1 -4 10 0 222.429 21.1843 1 -5 -10 0 44.9713 7.26630 3 -5 -10 0 36.5047 8.77735 1 -5 -10 0 35.9835 5.32480 4 -5 10 0 24.6756 7.08698 1 0 11 0 0.71378 4.11808 1 -1 -11 0 -1.2767 3.94802 1 -1 11 0 -3.1768 3.31945 1 1 11 0 -4.2290 3.44953 1 -2 -11 0 13.3020 4.64403 4 -2 -11 0 10.6684 5.99514 1 -2 11 0 0.93367 3.91034 1 2 11 0 -3.2309 4.70824 1 -3 -11 0 16.0580 6.63361 1 -3 11 0 9.69285 5.53423 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-1 24 4.35475 4.29033 1 0 1 -24 7.17615 5.37915 1 0 1 24 1.47873 4.12838 1 0 1 24 7.68660 3.05213 2 -1 -1 -24 27.4344 7.83541 1 -1 1 -24 26.5417 5.52581 4 -1 1 -24 17.8892 7.06463 1 -2 -1 -24 1.48580 3.47254 4 -2 -1 -24 0.68013 4.30420 1 -2 1 -24 1.55058 4.48662 1 -2 1 -24 0.62302 2.87839 4 -3 -1 -24 53.1961 10.3092 1 -3 -1 -24 44.8983 7.10543 4 -3 1 -24 45.3384 6.84217 4 -3 1 -24 36.8645 9.23192 1 -4 -2 24 12.5416 6.01211 1 -4 2 24 17.2741 6.73492 1 -3 -2 24 76.0109 7.02670 2 -3 -2 24 68.9502 11.7308 1 -3 2 24 75.4651 11.6911 1 -3 2 24 71.4405 6.30892 2 -2 -2 24 29.0273 4.65667 2 -2 -2 24 21.6692 6.81464 1 -2 2 24 29.7241 4.68087 2 -2 2 24 22.9918 6.94038 1 -1 -2 24 -2.9560 3.55543 1 -1 -2 24 1.84835 2.26464 2 1 2 -24 4.97296 4.99140 1 -1 2 24 1.79650 4.08622 1 -1 2 24 1.13426 2.25565 2 0 -2 24 20.5911 6.31321 1 0 -2 -24 25.3751 7.63531 1 0 2 24 21.5566 4.39603 2 0 2 24 30.8783 7.31583 1 0 2 -24 22.3799 7.36470 1 -1 -2 -24 39.8966 9.27741 1 -1 2 -24 40.4991 6.10297 4 -1 2 -24 34.6131 8.60960 1 -2 -2 -24 15.9554 6.57430 1 -2 -2 -24 15.2565 5.24527 4 -2 2 -24 18.5807 4.17304 4 -2 2 -24 14.5709 6.51138 1 -3 -2 -24 40.5962 9.61519 1 -3 -2 -24 41.2215 6.93086 4 -3 2 -24 38.7670 6.06620 4 -3 2 -24 36.6305 9.21919 1 -4 -3 24 200.873 19.4060 1 -4 3 24 222.096 19.9340 1 -3 -3 24 38.3858 8.91549 1 -3 3 24 34.2928 4.28388 2 -3 3 24 28.9858 7.84482 1 -2 -3 24 45.0911 6.06569 2 -2 -3 24 57.6547 10.1707 1 -2 3 24 47.8874 9.50524 1 -2 3 24 52.8652 6.21074 2 -1 -3 24 37.9221 8.12983 1 -1 -3 24 38.0742 5.68810 2 1 3 -24 39.3548 9.32746 1 -1 3 24 35.5803 5.49236 2 -1 3 24 44.3271 8.93043 1 0 -3 24 4.47614 4.56317 1 0 -3 -24 4.39284 5.04100 1 0 3 -24 9.55963 5.80700 1 0 3 24 7.13624 3.10554 2 0 3 24 5.97777 4.73905 1 -1 -3 -24 5.67481 5.37087 1 -1 3 -24 6.62172 5.68337 1 1 3 24 11.9537 7.68546 1 -1 3 -24 10.8986 3.46423 4 -2 -3 -24 76.2226 12.9690 1 -2 3 -24 83.6687 7.61638 4 -2 3 -24 69.9299 12.4754 1 -3 -3 -24 15.7292 6.90099 1 -3 3 -24 14.0020 3.77117 4 -3 3 -24 13.8583 6.50571 1 -3 -4 24 152.475 16.0531 1 -3 4 24 142.631 9.93540 2 -3 4 24 147.257 15.7275 1 -2 -4 24 5.59614 2.87233 2 -2 -4 24 5.37903 4.90895 1 2 -4 -24 8.30989 4.02143 3 -2 4 24 4.84321 2.50347 2 -2 4 24 8.30670 5.14153 1 1 -4 -24 -2.1902 3.01812 3 -1 -4 24 -1.7381 4.01059 1 -1 -4 24 1.07101 2.34742 2 -1 4 24 -1.1365 3.69690 1 -1 4 24 0.17545 2.00985 2 1 4 -24 2.44723 4.41566 1 0 -4 -24 122.046 12.1882 3 0 -4 -24 121.575 14.6388 1 0 4 24 135.738 14.3785 1 0 4 -24 129.181 14.8039 1 0 4 24 125.553 10.4631 2 -1 -4 -24 12.5509 4.86587 3 -1 -4 -24 15.6601 6.71704 1 1 4 24 13.9228 8.87721 1 -1 4 -24 14.8243 6.57590 1 -2 -4 -24 17.1599 6.85312 1 -2 4 -24 15.0292 6.55012 1 3 -5 -24 32.7020 6.91628 3 -3 -5 24 25.3401 8.15856 1 -3 5 24 37.5362 9.46042 1 -3 5 24 26.1143 3.64303 2 2 -5 -24 2.17983 3.48381 3 -2 -5 24 0.26164 2.56347 2 -2 -5 24 -0.7300 4.48828 1 -2 5 24 1.27109 1.97187 2 -2 5 24 -0.6864 3.98314 1 -1 -5 24 11.5406 5.61837 1 -1 -5 24 5.43146 2.94030 2 1 -5 -24 7.65031 4.37497 3 -1 5 24 9.43136 5.65401 1 1 5 -24 7.35843 5.68884 1 -1 5 24 14.6085 3.56181 2 0 -5 -24 18.0367 5.68941 3 0 -5 -24 17.7097 7.78537 1 0 5 24 26.7477 4.79394 2 0 5 24 28.4924 7.69496 1 0 5 -24 26.4412 7.84239 1 -1 -5 -24 16.3941 5.32146 3 -1 -5 -24 15.3216 6.96320 1 -1 5 -24 15.5256 6.61639 1 -2 -5 -24 8.33027 6.13338 1 -2 -5 -24 17.1972 5.48464 3 -2 5 -24 11.1234 6.20052 1 -2 -6 24 15.5865 6.49084 1 2 -6 -24 22.6467 6.19016 3 -2 6 24 13.6150 3.23109 2 -2 6 24 20.3141 7.33245 1 -1 -6 24 10.2612 6.00052 1 1 -6 -24 9.71953 4.78268 3 -1 6 24 15.5730 3.81883 2 -1 6 24 10.9498 6.36592 1 1 6 -24 8.79064 6.04102 1 0 -6 -24 422.892 29.3537 3 0 6 24 424.912 26.5485 2 0 6 -24 404.705 32.5122 1 0 6 24 473.389 32.7328 1 -1 -6 -24 89.4548 13.7079 1 -1 -6 -24 83.3595 11.3704 3 -1 6 -24 68.6327 12.4834 1 1 -7 -24 2.97800 3.86057 3 -1 7 24 3.23447 2.65493 2 -1 7 24 6.03568 5.26606 1 1 7 -24 -0.3237 4.89690 1 0 -7 -24 46.0270 8.69631 3 0 7 24 58.8814 11.5469 1 0 7 -24 65.7660 12.5679 1 0 7 24 45.9490 6.64790 2 -4 0 25 2.82000 4.34760 1 -3 0 25 184.701 17.7158 1 -3 0 25 170.549 12.1456 2 -2 0 25 -1.0376 1.91206 2 -2 0 25 -0.3886 3.99566 1 1 0 -25 11.9224 6.42847 1 -1 0 25 17.5568 4.08035 2 -1 0 25 18.8725 6.15458 1 0 0 25 3.17175 2.87114 2 0 0 -25 7.54408 5.25543 1 0 0 25 2.38576 3.87852 1 -1 0 -25 4.87033 4.73912 1 -2 0 -25 -0.6183 4.36506 1 -2 0 -25 -2.2948 2.86344 4 -4 -1 25 145.090 16.3590 1 -4 1 25 154.863 16.6185 1 -3 -1 25 157.045 16.3657 1 -3 -1 25 145.891 11.0999 2 -3 1 25 158.688 16.3198 1 -3 1 25 153.371 10.8375 2 -2 -1 25 0.31506 2.11312 2 -2 -1 25 5.13582 4.90253 1 -2 1 25 1.10101 4.08776 1 -2 1 25 2.37838 2.13567 2 -1 -1 25 38.6761 5.68134 2 -1 -1 25 32.7931 8.06277 1 -1 1 25 39.9785 5.67771 2 1 1 -25 25.9126 7.88700 1 -1 1 25 34.2352 8.02520 1 0 -1 -25 88.8943 13.3162 1 0 -1 25 88.6439 11.6159 1 0 1 25 101.509 12.0915 1 0 1 -25 96.8809 13.9748 1 0 1 25 89.4731 8.74542 2 -1 -1 -25 -0.4570 4.34647 1 -1 1 -25 -3.9763 3.17790 4 -1 1 -25 0.11703 4.25293 1 -2 -1 -25 10.0262 4.41501 4 -2 -1 -25 17.4983 7.23815 1 -2 1 -25 10.8165 6.33557 1 -2 1 -25 16.3650 4.19831 4 -3 -2 25 14.4306 3.60388 2 -3 -2 25 8.23287 5.72070 1 -3 2 25 11.1191 5.98558 1 -3 2 25 15.8451 3.14261 2 -2 -2 25 7.36961 5.17710 1 -2 -2 25 12.0972 3.24703 2 -2 2 25 2.26235 4.42403 1 -2 2 25 3.98528 2.54391 2 -1 -2 25 105.592 12.6882 1 -1 -2 25 103.841 9.30115 2 1 2 -25 88.4666 13.4886 1 -1 2 25 106.463 9.14051 2 -1 2 25 104.632 12.6429 1 0 -2 25 71.3926 11.0409 1 0 -2 -25 66.7727 11.7797 1 0 2 25 69.5225 10.9205 1 0 2 25 78.0158 8.18886 2 0 2 -25 54.2411 11.0206 1 -1 -2 -25 1.44573 4.91804 1 -1 2 -25 1.30375 4.70374 1 -1 2 -25 -0.2754 2.79423 4 -2 -2 -25 60.6368 11.6789 1 -2 -2 -25 37.6273 7.32997 4 -2 2 -25 49.6930 10.3795 1 -2 2 -25 52.6628 6.90791 4 -3 -3 25 11.6146 5.97029 1 -3 3 25 6.68045 2.25766 2 -3 3 25 5.49961 5.01471 1 -2 -3 25 4.82614 2.67634 2 -2 -3 25 -1.2763 4.24927 1 -2 3 25 1.19225 3.88329 1 -2 3 25 3.62909 2.38736 2 -1 -3 25 11.2686 3.79029 2 -1 -3 25 5.33401 4.83733 1 1 3 -25 11.3535 6.25321 1 -1 3 25 17.7737 6.34313 1 -1 3 25 10.2072 3.31328 2 0 -3 -25 6.65289 5.54932 1 0 3 25 12.1729 5.71213 1 0 3 25 6.97809 3.27964 2 0 3 -25 9.41631 6.15932 1 -1 -3 -25 14.6837 6.77283 1 -1 3 -25 21.9088 7.52996 1 -2 -3 -25 -2.2433 4.08090 1 -2 -3 -25 -3.2950 3.61287 4 -2 3 -25 0.30480 4.68731 1 -3 -4 25 -0.9166 4.52734 1 -3 4 25 -0.9568 1.54038 2 -3 4 25 -0.0191 4.28567 1 -2 -4 25 5.00523 5.00104 1 -2 -4 25 4.28946 2.89347 2 -2 4 25 4.73249 2.56311 2 -2 4 25 7.38229 5.26414 1 -1 -4 25 15.6735 6.12559 1 -1 -4 25 12.3047 3.64769 2 1 -4 -25 12.4123 5.39636 3 -1 4 25 17.4057 6.77448 1 1 4 -25 20.3439 7.77092 1 -1 4 25 11.4821 3.51531 2 0 -4 -25 8.26943 4.88369 3 0 -4 -25 9.37337 6.20317 1 0 4 -25 7.53411 5.45702 1 0 4 25 10.7545 5.69290 1 0 4 25 6.64798 3.18155 2 -1 -4 -25 40.1087 9.30053 1 -1 4 -25 31.4823 8.89349 1 -2 -4 -25 8.56491 5.94449 1 -2 4 -25 1.47043 4.70266 1 2 -5 -25 6.43625 4.26586 3 -2 -5 25 3.41694 2.79615 2 -2 -5 25 -0.3023 4.73788 1 -2 5 25 7.11670 5.53046 1 -2 5 25 3.20092 2.37879 2 -1 -5 25 19.9137 6.08055 2 1 -5 -25 19.1408 5.57134 3 -1 -5 25 14.3147 6.22529 1 1 5 -25 24.9288 8.12055 1 -1 5 25 15.4162 3.77906 2 -1 5 25 18.6709 6.92935 1 0 -5 -25 109.858 13.1365 3 0 5 25 96.2160 9.16930 2 0 5 25 117.013 13.9032 1 0 5 -25 95.3667 14.6094 1 -1 -5 -25 82.8318 11.0901 3 -1 -5 -25 79.9964 13.1565 1 -1 5 -25 81.1394 13.3939 1 1 -6 -25 39.6032 7.80270 3 1 6 -25 34.1471 9.59663 1 -1 6 25 38.1710 9.50679 1 -1 6 25 36.0080 5.40296 2 0 -6 -25 129.945 13.1830 3 0 6 25 122.048 10.6487 2 0 6 -25 127.933 16.1617 1 0 6 25 131.124 15.4762 1 -3 0 26 -1.0560 2.01634 2 -3 0 26 2.78311 4.77590 1 -2 0 26 2.98407 2.51052 2 -2 0 26 -2.4555 3.61493 1 -1 0 26 2.63959 4.38505 1 -1 0 26 -1.5578 2.21470 2 0 0 26 0.42640 3.78403 1 0 0 -26 2.38443 5.13429 1 -1 0 -26 -2.2206 4.24175 1 -2 0 -26 42.7367 6.93767 4 -2 0 -26 36.7755 9.71292 1 -3 -1 26 29.9920 8.18355 1 -3 -1 26 36.1100 5.11400 2 -3 1 26 34.9795 8.64555 1 -3 1 26 30.4115 4.53945 2 -2 -1 26 117.657 13.9397 1 -2 -1 26 111.132 9.54507 2 -2 1 26 114.074 13.7710 1 -2 1 26 104.494 9.18954 2 -1 -1 26 72.4514 11.8893 1 -1 -1 26 64.9013 7.79741 2 -1 1 26 66.9467 7.84634 2 -1 1 26 62.9017 11.1148 1 0 -1 -26 26.1142 8.21844 1 0 -1 26 20.5659 6.80376 1 0 1 -26 20.5157 7.61177 1 0 1 26 16.1575 6.30187 1 0 1 26 31.1297 6.02327 2 -1 -1 -26 6.77520 5.60568 1 -1 1 -26 1.27360 3.71006 4 -1 1 -26 -0.6558 4.71450 1 -2 -1 -26 1.49549 4.87019 1 -2 -1 -26 -1.1275 3.13087 4 -2 1 -26 1.05120 4.74610 1 -2 1 -26 1.67758 2.93476 4 -3 -2 26 3.77673 5.33842 1 -3 -2 26 -1.3908 1.96508 2 -3 2 26 -2.2620 1.61328 2 -3 2 26 5.00016 5.35458 1 -2 -2 26 0.76360 4.76360 1 -2 -2 26 4.48954 2.92373 2 -2 2 26 7.14583 5.08644 1 -2 2 26 3.26889 2.49798 2 -1 -2 26 75.5059 11.6555 1 -1 -2 26 66.4059 7.89577 2 -1 2 26 61.9891 7.50176 2 1 2 -26 69.8790 12.6492 1 -1 2 26 65.7838 11.3043 1 0 -2 -26 8.22927 5.79030 1 0 2 26 10.4826 3.55781 2 0 2 26 4.39574 4.82841 1 0 2 -26 14.8424 6.86810 1 -1 -2 -26 27.6067 8.45245 1 -1 2 -26 31.6523 8.98924 1 -1 2 -26 25.3847 5.21288 4 -2 -2 -26 7.29682 5.71293 1 -2 -2 -26 5.76634 4.63142 4 -2 2 -26 13.8484 3.83920 4 -2 2 -26 8.61944 5.95998 1 -3 -3 26 5.51312 5.40932 1 -3 3 26 6.99565 5.65737 1 -3 3 26 3.42758 2.14917 2 -2 -3 26 -1.0414 2.23966 2 -2 -3 26 5.78936 5.21796 1 -2 3 26 2.85059 4.63411 1 -2 3 26 1.37645 2.17211 2 -1 -3 26 63.2267 10.7800 1 -1 -3 26 70.6915 8.09926 2 -1 3 26 64.2459 7.42408 2 -1 3 26 56.7563 10.5939 1 1 3 -26 44.3560 10.3899 1 0 -3 -26 166.435 18.0963 1 0 3 -26 179.710 18.6453 1 0 3 26 193.190 17.9638 1 0 3 26 182.971 13.6083 2 -1 -3 -26 17.4052 7.37515 1 -1 3 -26 16.5319 7.40427 1 -2 -4 26 33.2236 8.62583 1 -2 -4 26 33.8490 5.80102 2 -2 4 26 33.6053 5.22972 2 -2 4 26 40.6258 9.36197 1 -1 -4 26 4.38341 3.07913 2 -1 -4 26 2.06604 4.64810 1 -1 4 26 -1.3524 2.05385 2 -1 4 26 -0.1447 4.17795 1 1 4 -26 5.63874 5.71886 1 0 4 26 13.0894 4.30469 2 0 4 26 32.3012 8.25554 1 0 4 -26 20.2997 7.57668 1 -1 -4 -26 14.1560 6.63697 1 -1 4 -26 11.4530 6.86331 1 1 -5 -26 54.3986 8.90695 3 -1 -5 26 38.3341 9.28909 1 -1 5 26 48.2396 6.18825 2 -1 5 26 47.7883 10.3365 1 1 5 -26 31.6378 9.37531 1 0 -5 -26 118.844 13.6659 3 0 5 -26 136.556 16.8967 1 0 5 26 162.470 12.1916 2 0 5 26 180.211 17.3842 1 -2 0 27 -0.6194 2.14497 2 -2 0 27 -1.0294 4.09886 1 -1 0 27 0.84903 2.39511 2 -1 0 27 0.32315 4.28489 1 0 0 -27 0.12188 4.98783 1 0 0 27 4.53076 5.33656 1 -1 0 -27 9.68889 6.25067 1 -2 -1 27 1.31628 2.43699 2 -2 -1 27 2.04561 4.63635 1 -2 1 27 -2.7192 1.90604 2 -2 1 27 4.12630 5.12026 1 -1 -1 27 6.56550 5.28268 1 -1 -1 27 11.8336 3.73388 2 -1 1 27 8.35976 3.37005 2 -1 1 27 10.6389 6.04863 1 0 -1 -27 8.12036 6.25906 1 0 1 -27 12.8511 6.90536 1 0 1 27 24.6423 7.27516 1 -1 -1 -27 1.06215 4.97252 1 -1 1 -27 0.84877 4.44428 1 -1 1 -27 -2.9134 3.17039 4 -2 -2 27 7.51236 3.33594 2 -2 -2 27 2.43145 5.06570 1 -2 2 27 1.19130 2.36867 2 -2 2 27 1.38206 4.68624 1 -1 -2 27 71.9044 8.97996 2 -1 -2 27 104.243 12.9034 1 -1 2 27 91.8769 8.77217 2 -1 2 27 93.2328 13.9081 1 0 -2 -27 1.08774 4.77967 1 0 2 27 1.19809 3.22060 2 0 2 27 5.46704 5.31156 1 0 2 -27 -4.2526 4.29815 1 -1 -2 -27 9.55019 6.37923 1 -1 2 -27 6.37389 5.52715 1 -2 -3 27 -0.6983 2.24054 2 -2 -3 27 -1.0454 4.76519 1 -2 3 27 3.98350 5.07517 1 -2 3 27 -0.9912 2.00553 2 -1 -3 27 55.2241 7.67871 2 -1 -3 27 64.7423 11.5903 1 -1 3 27 77.0697 8.26510 2 -1 3 27 67.9762 11.9626 1 0 3 -27 2.79656 5.57373 1 0 3 27 5.07084 4.78436 1 0 3 27 2.45051 2.61002 2 -1 -4 27 9.97003 6.30795 1 -1 4 27 4.72356 5.31977 1 0 4 -27 11.2487 6.60482 1 -1 0 28 -0.0027 4.42811 1 -1 0 28 1.25725 2.85022 2 0 0 -28 27.3706 8.96539 1 -1 -1 28 32.5787 8.70874 1 -1 -1 28 28.5713 5.38095 2 -1 1 28 34.6446 8.79493 1 -1 1 28 33.0651 5.69759 2 0 -1 -28 -0.0244 4.77261 1 0 1 -28 5.59486 6.05339 1 -1 -2 28 -2.3224 4.19045 1 -1 2 28 1.65328 4.54159 1 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/4' _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.6897 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71050 6.051 11.019 22.605 90.241 95.203 90.249 ) ; _shelx_hkl_checksum 83379 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 N1 N 0.5096(2) 0.01315(11) 0.24114(5) 0.0179(3) Uani 1 1 d . . . . . N2 N 0.73470(19) 0.20701(11) 0.18976(5) 0.0187(3) Uani 1 1 d . . . . . C1 C 1.0927(3) 0.15605(14) 0.32685(6) 0.0226(3) Uani 1 1 d . . . . . H1 H 1.2277 0.1862 0.3466 0.027 Uiso 1 1 calc R U . . . C2 C 0.9732(3) 0.06275(14) 0.35372(6) 0.0234(3) Uani 1 1 d . . . . . H3 H 1.0294 0.0309 0.3913 0.028 Uiso 1 1 calc R U . . . C3 C 0.7782(3) 0.01766(14) 0.32646(6) 0.0220(3) Uani 1 1 d . . . . . H14 H 0.6988 -0.0444 0.3452 0.026 Uiso 1 1 calc R U . . . C4 C 0.6956(2) 0.06426(13) 0.27013(6) 0.0180(3) Uani 1 1 d . . . . . C5 C 0.4407(2) 0.05709(13) 0.18813(6) 0.0169(3) Uani 1 1 d . . . . . C6 C 0.2513(2) -0.00959(13) 0.15557(6) 0.0178(3) Uani 1 1 d . . . . . C7 C 0.2405(3) -0.02974(14) 0.09400(6) 0.0232(3) Uani 1 1 d . . . . . H10 H 0.3546 0.0010 0.0715 0.028 Uiso 1 1 calc R U . . . C8 C 0.0630(3) -0.09468(15) 0.06572(7) 0.0276(4) Uani 1 1 d . . . . . H11 H 0.0571 -0.1088 0.0240 0.033 Uiso 1 1 calc R U . . . C9 C -0.1049(3) -0.13881(14) 0.09800(7) 0.0268(4) Uani 1 1 d . . . . . H2 H -0.2282 -0.1810 0.0783 0.032 Uiso 1 1 calc R U . . . C10 C 0.5485(2) 0.16069(13) 0.16358(6) 0.0177(3) Uani 1 1 d . . . . . C11 C 0.8143(2) 0.15793(13) 0.24330(6) 0.0176(3) Uani 1 1 d . . . . . C12 C 1.0152(2) 0.20336(14) 0.27259(6) 0.0202(3) Uani 1 1 d . . . . . H4 H 1.0957 0.2662 0.2548 0.024 Uiso 1 1 calc R U . . . C13 C 0.4574(2) 0.22616(13) 0.10864(6) 0.0185(3) Uani 1 1 d . . . . . C14 C 0.5951(2) 0.24738(14) 0.06322(6) 0.0227(3) Uani 1 1 d . . . . . H9 H 0.7425 0.2155 0.0664 0.027 Uiso 1 1 calc R U . . . C15 C 0.5191(3) 0.31468(15) 0.01321(6) 0.0261(4) Uani 1 1 d . . . . . H8 H 0.6135 0.3277 -0.0179 0.031 Uiso 1 1 calc R U . . . C16 C 0.3056(3) 0.36281(14) 0.00873(6) 0.0251(4) Uani 1 1 d . . . . . H7 H 0.2538 0.4100 -0.0251 0.030 Uiso 1 1 calc R U . . . C17 C 0.1677(3) 0.34177(14) 0.05389(6) 0.0249(4) Uani 1 1 d . . . . . H6 H 0.0211 0.3748 0.0508 0.030 Uiso 1 1 calc R U . . . C18 C 0.2417(2) 0.27306(14) 0.10347(6) 0.0221(3) Uani 1 1 d . . . . . H5 H 0.1452 0.2580 0.1339 0.027 Uiso 1 1 calc R U . . . C19 C 0.0853(2) -0.05854(13) 0.18787(6) 0.0193(3) Uani 1 1 d . . . . . H13 H 0.0946 -0.0487 0.2299 0.023 Uiso 1 1 calc R U . . . C20 C -0.0931(3) -0.12134(14) 0.15925(7) 0.0241(3) Uani 1 1 d . . . . . H12 H -0.2075 -0.1525 0.1816 0.029 Uiso 1 1 calc R U . . . 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 N1 0.0172(6) 0.0201(7) 0.0167(6) -0.0007(4) 0.0030(5) 0.0003(5) N2 0.0177(6) 0.0193(7) 0.0191(6) -0.0003(5) 0.0020(5) 0.0007(5) C1 0.0198(7) 0.0236(8) 0.0238(7) -0.0061(6) -0.0021(6) 0.0025(6) C2 0.0269(8) 0.0256(8) 0.0174(7) -0.0016(6) -0.0004(6) 0.0057(6) C3 0.0256(8) 0.0220(8) 0.0186(7) 0.0005(5) 0.0039(6) 0.0011(6) C4 0.0172(7) 0.0193(8) 0.0179(6) -0.0024(5) 0.0030(5) 0.0026(6) C5 0.0159(7) 0.0188(7) 0.0168(6) -0.0016(5) 0.0049(5) 0.0016(6) C6 0.0167(7) 0.0163(7) 0.0203(7) 0.0006(5) 0.0015(5) 0.0016(6) C7 0.0255(8) 0.0240(8) 0.0204(7) 0.0013(6) 0.0034(6) -0.0030(6) C8 0.0331(9) 0.0283(9) 0.0203(7) -0.0014(6) -0.0038(6) -0.0019(7) C9 0.0223(8) 0.0235(9) 0.0332(8) -0.0029(6) -0.0053(6) -0.0045(6) C10 0.0170(7) 0.0184(7) 0.0180(6) -0.0010(5) 0.0039(5) 0.0003(6) C11 0.0185(7) 0.0178(7) 0.0168(6) -0.0021(5) 0.0031(5) 0.0034(6) C12 0.0192(7) 0.0198(8) 0.0220(7) -0.0027(5) 0.0040(6) -0.0001(6) C13 0.0190(7) 0.0177(7) 0.0184(7) 0.0000(5) 0.0001(5) -0.0044(6) C14 0.0189(7) 0.0274(9) 0.0220(7) 0.0007(6) 0.0024(6) -0.0025(6) C15 0.0272(8) 0.0330(9) 0.0185(7) 0.0029(6) 0.0041(6) -0.0065(7) C16 0.0295(9) 0.0260(9) 0.0186(7) 0.0041(6) -0.0047(6) -0.0056(7) C17 0.0206(8) 0.0265(9) 0.0267(7) 0.0013(6) -0.0035(6) -0.0014(6) C18 0.0194(7) 0.0256(8) 0.0217(7) 0.0013(6) 0.0033(6) -0.0033(6) C19 0.0192(7) 0.0184(8) 0.0206(7) 0.0006(5) 0.0033(6) 0.0029(6) C20 0.0179(7) 0.0225(8) 0.0323(8) 0.0011(6) 0.0048(6) -0.0015(6) 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' 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 _geom_angle_publ_flag C5 N1 C4 117.60(12) . . ? C10 N2 C11 117.46(12) . . ? C12 C1 C2 120.53(13) . . ? C12 C1 H1 119.7 . . ? C2 C1 H1 119.7 . . ? C3 C2 C1 121.09(13) . . ? C3 C2 H3 119.5 . . ? C1 C2 H3 119.5 . . ? C2 C3 C4 119.49(14) . . ? C2 C3 H14 120.3 . . ? C4 C3 H14 120.3 . . ? N1 C4 C11 121.07(12) . . ? N1 C4 C3 119.32(13) . . ? C11 C4 C3 119.50(13) . . ? N1 C5 C10 121.13(12) . . ? N1 C5 C6 115.66(13) . . ? C10 C5 C6 123.18(12) . . ? C19 C6 C7 118.90(13) . . ? C19 C6 C5 118.93(12) . . ? C7 C6 C5 122.10(13) . . ? C8 C7 C6 120.09(14) . . ? C8 C7 H10 120.0 . . ? C6 C7 H10 120.0 . . ? C9 C8 C7 120.37(14) . . ? C9 C8 H11 119.8 . . ? C7 C8 H11 119.8 . . ? C8 C9 C20 119.87(14) . . ? C8 C9 H2 120.1 . . ? C20 C9 H2 120.1 . . ? N2 C10 C5 121.60(12) . . ? N2 C10 C13 114.95(12) . . ? C5 C10 C13 123.42(12) . . ? N2 C11 C4 120.64(12) . . ? N2 C11 C12 119.47(13) . . ? C4 C11 C12 119.87(12) . . ? C1 C12 C11 119.52(14) . . ? C1 C12 H4 120.2 . . ? C11 C12 H4 120.2 . . ? C14 C13 C18 119.26(13) . . ? C14 C13 C10 119.37(13) . . ? C18 C13 C10 121.26(13) . . ? C15 C14 C13 120.62(14) . . ? C15 C14 H9 119.7 . . ? C13 C14 H9 119.7 . . ? C16 C15 C14 119.90(14) . . ? C16 C15 H8 120.1 . . ? C14 C15 H8 120.1 . . ? C15 C16 C17 119.66(13) . . ? C15 C16 H7 120.2 . . ? C17 C16 H7 120.2 . . ? C18 C17 C16 120.64(14) . . ? C18 C17 H6 119.7 . . ? C16 C17 H6 119.7 . . ? C17 C18 C13 119.91(14) . . ? C17 C18 H5 120.0 . . ? C13 C18 H5 120.0 . . ? C20 C19 C6 120.66(13) . . ? C20 C19 H13 119.7 . . ? C6 C19 H13 119.7 . . ? C19 C20 C9 120.03(14) . . ? C19 C20 H12 120.0 . . ? C9 C20 H12 120.0 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C5 1.3191(18) . ? N1 C4 1.3647(18) . ? N2 C10 1.3203(18) . ? N2 C11 1.3669(17) . ? C1 C12 1.370(2) . ? C1 C2 1.414(2) . ? C1 H1 0.9500 . ? C2 C3 1.368(2) . ? C2 H3 0.9500 . ? C3 C4 1.4153(19) . ? C3 H14 0.9500 . ? C4 C11 1.414(2) . ? C5 C10 1.440(2) . ? C5 C6 1.4901(18) . ? C6 C19 1.393(2) . ? C6 C7 1.3990(19) . ? C7 C8 1.389(2) . ? C7 H10 0.9500 . ? C8 C9 1.382(2) . ? C8 H11 0.9500 . ? C9 C20 1.388(2) . ? C9 H2 0.9500 . ? C10 C13 1.4910(19) . ? C11 C12 1.4151(19) . ? C12 H4 0.9500 . ? C13 C14 1.391(2) . ? C13 C18 1.391(2) . ? C14 C15 1.388(2) . ? C14 H9 0.9500 . ? C15 C16 1.384(2) . ? C15 H8 0.9500 . ? C16 C17 1.387(2) . ? C16 H7 0.9500 . ? C17 C18 1.386(2) . ? C17 H6 0.9500 . ? C18 H5 0.9500 . ? C19 C20 1.385(2) . ? C19 H13 0.9500 . ? C20 H12 0.9500 . ?