#------------------------------------------------------------------------------ #$Date: 2021-11-10 01:16:51 +0200 (Wed, 10 Nov 2021) $ #$Revision: 270546 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/51/1565152.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_1565152 loop_ _publ_author_name 'Wang, Lele' 'Han, Hua-Bin' 'Gu, Lijie' 'Zhang, Wenjing' 'Zhao, Junwei' 'Wang, Qi-Lin' _publ_section_title ; Skeletal remodeling of chalcone-based pyridinium salts to access isoindoline polycycles and their bridged derivatives ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC05741C _journal_year 2021 _chemical_formula_moiety 'C26 H24 N2 O3' _chemical_formula_sum 'C26 H24 N2 O3' _chemical_formula_weight 412.47 _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_update_record ; 2021-05-28 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.064(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.8952(8) _cell_length_b 8.6715(6) _cell_length_c 21.1913(13) _cell_measurement_reflns_used 9896 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 72.4441 _cell_measurement_theta_min 4.1415 _cell_volume 2180.4(2) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_collection 'Bruker Instrument Service vV6.2.9' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 882)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON II' _diffrn_radiation_monochromator 'Helixos MX multilayer Optic' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_unetI/netI 0.0615 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 21965 _diffrn_reflns_theta_full 72.52 _diffrn_reflns_theta_max 72.52 _diffrn_reflns_theta_min 4.14 _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 872 _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.430 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.415 _refine_diff_density_min -0.384 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 281 _refine_ls_number_reflns 4310 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0738 _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^)+(0.1537P)^2^+0.3407P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2043 _refine_ls_wR_factor_ref 0.2161 _reflns_number_gt 3685 _reflns_number_total 4310 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc05741c2.cif _cod_data_source_block hd_wql34 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 1565152 _shelx_res_file ; TITL hd_wql34_0m_a.res in P2(1)/n hd_wql34_0m.res created by SHELXL-2017/1 at 22:21:16 on 14-Oct-2020 CELL 1.54178 11.8952 8.6715 21.1913 90.000 94.064 90.000 ZERR 4.00 0.0008 0.0006 0.0013 0.000 0.002 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N O UNIT 104 96 8 12 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.130 SIZE 0.100 0.430 0.600 ACTA EQIV $1 -x+1, -y+1, -z+1 HTAB C21 N2_$1 HTAB C22 O3_$1 L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.153700 0.340700 FVAR 0.59847 O1 4 0.676483 0.622784 0.764818 11.00000 0.05686 0.05234 = 0.02666 -0.01046 -0.00792 0.01639 O2 4 0.078227 0.824412 0.610409 11.00000 0.05109 0.03594 = 0.02541 0.00097 0.00288 0.00714 O3 4 0.668195 0.518223 0.668410 11.00000 0.07193 0.07503 = 0.03353 -0.02017 -0.00902 0.03088 N1 3 0.229009 0.494220 0.499271 11.00000 0.04909 0.03591 = 0.02114 -0.00544 0.00481 0.00082 N2 3 0.540345 0.820814 0.469633 11.00000 0.05295 0.05030 = 0.03149 0.00709 0.01015 0.00057 C1 1 0.177922 0.721699 0.838786 11.00000 0.05976 0.03956 = 0.01933 -0.00148 0.00664 -0.00939 AFIX 43 H1 2 0.183817 0.719476 0.883720 11.00000 -1.20000 AFIX 0 C2 1 0.260582 0.653471 0.805501 11.00000 0.05158 0.04361 = 0.02078 0.00223 0.00185 -0.00264 AFIX 43 H18 2 0.323487 0.605537 0.827611 11.00000 -1.20000 AFIX 0 C3 1 0.251745 0.654929 0.739629 11.00000 0.04650 0.03865 = 0.02100 0.00012 0.00495 -0.00068 AFIX 43 H15 2 0.307497 0.605325 0.716881 11.00000 -1.20000 AFIX 0 C4 1 0.161253 0.729025 0.706963 11.00000 0.04472 0.02898 = 0.02200 -0.00146 0.00532 -0.00445 C5 1 0.150775 0.741963 0.636511 11.00000 0.04289 0.02763 = 0.02158 -0.00052 0.00443 -0.00046 C6 1 0.229422 0.655911 0.595131 11.00000 0.04265 0.03191 = 0.01579 -0.00037 0.00273 0.00103 AFIX 13 H6 2 0.276059 0.580154 0.621151 11.00000 -1.20000 AFIX 0 C7 1 0.306844 0.774121 0.564159 11.00000 0.04309 0.03404 = 0.01859 0.00202 0.00333 0.00230 AFIX 13 H19 2 0.258963 0.861792 0.547386 11.00000 -1.20000 AFIX 0 C8 1 0.397441 0.839426 0.613191 11.00000 0.04386 0.03261 = 0.02396 0.00011 0.00424 -0.00139 AFIX 23 H5 2 0.433215 0.930117 0.594513 11.00000 -1.20000 H20 2 0.359757 0.875399 0.650688 11.00000 -1.20000 AFIX 0 C9 1 0.487372 0.726855 0.634361 11.00000 0.04572 0.03756 = 0.02294 -0.00306 0.00464 0.00070 AFIX 43 H21 2 0.513121 0.659726 0.603023 11.00000 -1.20000 AFIX 0 C10 1 0.534941 0.711225 0.692624 11.00000 0.04585 0.03672 = 0.02397 -0.00358 0.00343 0.00086 AFIX 43 H22 2 0.506551 0.768102 0.726356 11.00000 -1.20000 AFIX 0 C11 1 0.631751 0.606008 0.705436 11.00000 0.05030 0.04035 = 0.02460 -0.00661 -0.00092 0.00310 C12 1 0.778246 0.535925 0.781812 11.00000 0.06533 0.06308 = 0.04257 -0.01893 -0.01463 0.02697 AFIX 23 H23 2 0.836997 0.560916 0.752592 11.00000 -1.20000 H24 2 0.762575 0.423905 0.779109 11.00000 -1.20000 AFIX 0 C13 1 0.817560 0.579174 0.848154 11.00000 0.06832 0.07344 = 0.04299 -0.01508 -0.01806 0.02581 AFIX 137 H3 2 0.823415 0.691644 0.851516 11.00000 -1.50000 H4 2 0.891536 0.532794 0.859023 11.00000 -1.50000 H2 2 0.763458 0.541387 0.877336 11.00000 -1.50000 AFIX 0 C14 1 0.156564 0.571070 0.542834 11.00000 0.04376 0.03319 = 0.01816 -0.00145 0.00180 0.00218 AFIX 13 H14 2 0.106737 0.646999 0.518871 11.00000 -1.20000 AFIX 0 C15 1 0.086675 0.439232 0.564132 11.00000 0.04424 0.03299 = 0.02202 0.00082 -0.00322 0.00054 C16 1 0.004000 0.439168 0.607458 11.00000 0.04797 0.03593 = 0.02194 0.00193 0.00048 -0.00154 AFIX 43 H13 2 -0.014395 0.531501 0.628546 11.00000 -1.20000 AFIX 0 C17 1 -0.051209 0.302263 0.619425 11.00000 0.05135 0.04350 = 0.02618 0.00703 -0.00184 -0.00521 AFIX 43 H12 2 -0.108570 0.301241 0.648416 11.00000 -1.20000 AFIX 0 C18 1 -0.022975 0.166124 0.589132 11.00000 0.05610 0.03461 = 0.03814 0.00857 -0.00854 -0.00682 AFIX 43 H7 2 -0.060037 0.072651 0.598431 11.00000 -1.20000 AFIX 0 C19 1 0.058820 0.166193 0.545527 11.00000 0.05283 0.03234 = 0.03686 -0.00134 -0.00846 0.00251 AFIX 43 H8 2 0.077937 0.073683 0.524791 11.00000 -1.20000 AFIX 0 C20 1 0.112121 0.303969 0.532810 11.00000 0.04639 0.03522 = 0.02517 -0.00082 -0.00575 0.00348 C21 1 0.198605 0.332855 0.485848 11.00000 0.05095 0.03626 = 0.02546 -0.00808 -0.00111 0.00180 AFIX 23 H10 2 0.264440 0.263688 0.493221 11.00000 -1.20000 H9 2 0.166187 0.319805 0.441844 11.00000 -1.20000 AFIX 0 C22 1 0.322708 0.563615 0.482585 11.00000 0.04679 0.04221 = 0.01861 -0.00081 0.00355 0.00428 AFIX 43 H11 2 0.364484 0.516714 0.451168 11.00000 -1.20000 AFIX 0 C23 1 0.360740 0.699100 0.508870 11.00000 0.04480 0.03939 = 0.01877 0.00242 0.00523 0.00317 C24 1 0.459490 0.766146 0.486315 11.00000 0.04938 0.04159 = 0.02178 0.00441 0.00563 0.00348 C25 1 0.086471 0.793340 0.806851 11.00000 0.05493 0.04210 = 0.02778 -0.00306 0.01396 -0.00162 AFIX 43 H16 2 0.029480 0.839232 0.829858 11.00000 -1.20000 AFIX 0 C26 1 0.078318 0.797899 0.741032 11.00000 0.04977 0.03677 = 0.02595 -0.00047 0.00756 0.00043 AFIX 43 H17 2 0.016109 0.848046 0.719183 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM hd_wql34_0m_a.res in P2(1)/n REM R1 = 0.0738 for 3685 Fo > 4sig(Fo) and 0.0817 for all 4310 data REM 281 parameters refined using 0 restraints END WGHT 0.1537 0.3407 REM Instructions for potential hydrogen bonds HTAB C21 N2_$1 HTAB C22 O3_$1 REM Highest difference peak 0.415, deepest hole -0.384, 1-sigma level 0.079 Q1 1 0.7094 0.5896 0.6573 11.00000 0.05 0.42 Q2 1 0.3343 0.7236 0.5360 11.00000 0.05 0.40 Q3 1 0.1984 0.6975 0.6212 11.00000 0.05 0.35 Q4 1 0.8075 0.4547 0.7610 11.00000 0.05 0.34 Q5 1 0.2672 0.7132 0.5800 11.00000 0.05 0.32 ; _shelx_res_checksum 37285 _shelx_hkl_file ; -1 0 0 1.70 0.60 -1 0 0 3.20 1.20 -2 0 0 518.95 54.89 -2 0 0 672.93 54.29 -3 0 0 8.50 3.40 -4 0 0 58.89 8.90 -4 0 0 57.29 7.40 -5 0 0 1.90 1.70 -5 0 0 0.20 3.70 -6 0 0 210.78 22.70 -6 0 0 205.38 25.30 -6 0 0 223.78 25.50 -7 0 0 12.30 8.40 -7 0 0 1.90 3.50 -7 0 0 3.80 4.60 8 0 0 89.79 9.70 -8 0 0 116.39 20.60 -9 0 0 -15.60 14.20 -9 0 0 3.60 6.10 -9 0 0 6.70 7.70 -9 0 0 -0.10 1.30 9 0 0 0.60 0.80 -10 0 0 19.70 3.80 -10 0 0 30.00 10.40 -10 0 0 7.80 26.80 -11 0 0 -28.90 35.30 11 0 0 -0.30 0.60 11 0 0 -0.40 0.50 -11 0 0 10.90 10.90 -11 0 0 0.60 1.10 12 0 0 77.89 7.90 12 0 0 77.89 8.50 13 0 0 -0.70 0.50 13 0 0 0.50 0.60 14 0 0 11.10 1.60 -14 0 0 11.80 1.60 14 0 0 7.40 1.50 0 1 0 0.40 0.80 0 1 0 2.90 1.20 -1 -1 0 15.10 2.70 -1 -1 0 16.20 2.50 1 -1 0 15.90 2.70 -2 -1 0 1325.97 106.29 2 1 0 1019.80 104.29 -3 -1 0 25.70 4.70 -3 -1 0 26.30 5.00 -3 -1 0 23.00 4.20 -3 1 0 26.50 6.70 3 1 0 21.40 2.50 -4 -1 0 538.65 56.19 -4 -1 0 566.14 55.89 -4 -1 0 667.83 59.19 -4 1 0 621.44 58.09 -4 1 0 581.94 54.49 -5 -1 0 94.39 12.80 -5 -1 0 103.29 14.40 -5 -1 0 88.99 12.10 -5 1 0 106.19 15.40 -5 1 0 95.79 11.00 -6 -1 0 93.79 14.30 -6 -1 0 71.39 12.40 -6 -1 0 86.59 12.10 -6 1 0 83.39 16.00 -7 -1 0 124.99 20.20 -7 -1 0 112.59 18.40 -7 -1 0 119.59 16.50 -7 1 0 140.09 16.10 -7 1 0 152.08 29.70 8 -1 0 131.59 13.70 8 -1 0 152.48 13.80 -8 1 0 116.79 14.10 8 1 0 145.89 13.60 -9 -1 0 217.28 25.20 -9 -1 0 183.48 26.60 9 -1 0 182.38 17.60 9 -1 0 170.68 16.90 -9 -1 0 185.48 27.80 9 1 0 177.68 17.40 -9 1 0 205.78 40.30 9 1 0 161.98 17.10 -10 -1 0 23.60 18.70 10 -1 0 53.69 5.80 -10 -1 0 25.20 10.60 -10 -1 0 42.60 13.30 10 -1 0 45.30 4.90 -10 1 0 35.00 5.90 10 1 0 37.70 5.20 10 1 0 51.49 5.60 -10 1 0 73.19 16.50 -10 1 0 -12.90 34.70 -11 -1 0 8.10 8.90 11 -1 0 4.70 1.40 -11 -1 0 2.00 1.50 -11 -1 0 1.20 26.70 11 -1 0 5.40 1.40 11 1 0 4.60 1.40 11 1 0 4.50 1.20 -11 1 0 5.40 10.60 12 -1 0 38.50 4.80 12 1 0 36.80 4.70 12 1 0 34.20 4.30 -13 -1 0 4.60 1.20 13 -1 0 4.40 1.30 13 -1 0 2.20 1.00 13 1 0 4.40 1.20 13 1 0 3.70 1.30 14 -1 0 36.20 4.10 14 -1 0 34.60 3.90 -14 -1 0 40.30 4.00 14 1 0 33.40 4.00 0 -2 0 8920.61 796.62 -1 -2 0 290.07 26.10 -1 -2 0 276.87 26.00 1 -2 0 238.98 25.20 -2 -2 0 3879.11 311.37 -2 -2 0 3514.85 310.87 -2 -2 0 2983.90 309.17 -3 -2 0 1894.81 184.78 -3 -2 0 1953.60 185.28 -3 -2 0 1981.00 183.78 -3 2 0 2319.77 187.38 -4 -2 0 20.60 4.80 -4 -2 0 23.10 5.70 -4 -2 0 20.40 6.10 -4 2 0 26.20 9.10 -5 -2 0 190.58 22.20 -5 -2 0 195.98 24.00 -5 -2 0 163.08 21.50 -5 2 0 225.08 19.90 -5 2 0 223.28 28.00 -6 -2 0 22.80 8.00 -6 -2 0 14.80 6.00 -6 -2 0 14.30 5.90 -6 2 0 -1.20 13.20 -6 2 0 17.00 4.60 7 -2 0 3.60 0.80 -7 -2 0 7.80 6.20 -7 -2 0 7.80 6.40 -7 2 0 -0.70 1.30 -7 2 0 -8.70 14.70 -8 -2 0 57.39 12.80 -8 -2 0 39.00 9.80 8 -2 0 35.40 4.00 8 -2 0 37.60 4.60 -8 2 0 28.40 4.90 8 2 0 34.20 4.30 -8 2 0 37.90 26.00 -9 -2 0 325.77 36.70 9 -2 0 266.77 25.30 9 -2 0 245.48 24.50 -9 -2 0 315.37 35.20 9 2 0 236.58 24.90 -10 -2 0 21.10 3.20 10 -2 0 20.60 3.30 -10 -2 0 47.00 25.60 10 -2 0 18.10 2.80 -10 -2 0 27.80 12.00 -10 -2 0 21.40 11.90 -10 2 0 30.60 12.10 -10 2 0 15.20 3.90 10 2 0 22.20 3.20 11 -2 0 96.79 10.50 -11 -2 0 148.09 28.00 11 -2 0 109.99 11.20 11 2 0 108.79 11.10 12 -2 0 8.50 1.70 -12 -2 0 14.10 2.00 12 2 0 9.40 1.90 -12 2 0 6.50 2.40 13 -2 0 9.60 1.80 13 -2 0 6.90 1.50 -13 -2 0 6.00 1.30 13 2 0 7.20 1.60 -13 2 0 4.10 1.60 14 -2 0 6.50 1.20 -14 -2 0 8.60 1.40 14 2 0 8.30 1.50 0 -3 0 1.90 1.70 0 -3 0 0.10 1.00 1 -3 0 534.45 49.50 -1 -3 0 573.94 50.59 -1 -3 0 557.04 50.59 1 -3 0 465.75 49.00 -2 -3 0 501.75 49.20 -2 -3 0 520.05 49.30 -3 -3 0 870.61 81.99 -3 -3 0 942.41 82.39 -3 -3 0 798.72 78.99 -4 -3 0 71.39 10.60 -4 -3 0 62.69 10.30 -4 -3 0 60.79 8.40 -5 -3 0 14.30 5.50 -5 -3 0 8.00 3.70 -5 -3 0 13.60 7.00 -5 -3 0 15.30 5.80 -5 3 0 15.80 3.30 -6 -3 0 134.79 20.00 -6 -3 0 112.69 15.50 -6 -3 0 102.19 17.80 -7 -3 0 28.80 4.10 -7 -3 0 46.00 10.10 7 -3 0 31.80 3.80 -7 -3 0 35.40 4.20 -7 -3 0 47.70 16.90 -7 -3 0 42.80 11.20 7 -3 0 26.50 3.90 -7 3 0 34.00 5.30 -8 -3 0 26.30 8.90 8 -3 0 13.30 3.00 -8 -3 0 16.90 2.90 -8 -3 0 21.20 9.50 8 -3 0 24.40 2.80 -8 -3 0 22.30 4.70 8 -3 0 15.30 3.00 -8 -3 0 17.90 8.90 -8 3 0 19.80 4.40 8 3 0 21.20 3.10 -9 -3 0 18.40 3.00 -9 -3 0 36.60 11.60 -9 -3 0 24.10 8.40 -9 -3 0 23.10 13.10 9 -3 0 20.50 2.80 9 -3 0 18.60 3.20 9 3 0 19.30 3.20 -9 3 0 17.80 3.90 10 -3 0 57.59 6.20 10 -3 0 54.29 6.50 -10 -3 0 45.40 15.40 -10 -3 0 62.29 6.50 -10 -3 0 35.20 16.50 -10 -3 0 67.69 6.40 -10 3 0 70.19 20.20 10 3 0 52.69 6.60 -11 -3 0 -1.00 16.90 -11 -3 0 1.70 0.80 -11 -3 0 -1.90 1.40 11 -3 0 1.90 0.80 11 -3 0 1.40 1.00 -11 3 0 0.50 1.00 11 3 0 0.00 0.60 12 -3 0 0.60 0.50 -12 -3 0 1.50 0.70 12 -3 0 1.20 1.00 -12 3 0 1.40 1.30 12 3 0 2.50 1.10 -13 -3 0 112.29 10.30 13 -3 0 103.39 10.10 13 3 0 103.19 10.50 14 -3 0 20.50 2.30 -14 -3 0 24.20 2.50 14 3 0 20.10 2.60 0 -4 0 219.98 22.30 0 -4 0 206.58 22.20 -1 -4 0 109.19 13.60 1 -4 0 107.79 12.30 -1 -4 0 117.09 13.50 -2 -4 0 32.90 6.70 -2 -4 0 30.40 6.60 2 4 0 27.60 3.80 -3 -4 0 379.06 37.50 -3 -4 0 336.47 36.80 -4 -4 0 3.60 4.00 -4 -4 0 2.70 2.10 -4 -4 0 1.40 1.50 -4 -4 0 1.10 3.20 -5 -4 0 34.20 8.60 -5 -4 0 42.40 9.50 -5 -4 0 33.70 6.00 -5 -4 0 44.60 8.00 -5 -4 0 26.80 4.00 -6 -4 0 125.29 12.30 -6 -4 0 140.69 13.80 -6 -4 0 161.88 20.40 -6 -4 0 121.99 12.50 -6 -4 0 140.19 19.80 6 -4 0 108.19 12.00 -6 4 0 124.49 14.20 7 -4 0 1.10 0.80 -7 -4 0 -4.20 4.50 -7 -4 0 0.40 0.90 -7 -4 0 -8.30 12.10 7 -4 0 2.60 1.30 -7 -4 0 -0.60 4.70 -7 -4 0 2.00 1.50 -7 -4 0 1.30 1.90 -7 -4 0 -3.20 4.40 7 4 0 1.30 1.60 -7 4 0 3.70 2.40 8 -4 0 4.10 1.10 8 -4 0 6.40 1.90 -8 -4 0 9.20 2.30 -8 -4 0 2.80 7.60 -8 -4 0 3.40 6.70 -8 -4 0 2.90 1.30 -8 -4 0 8.10 2.10 -8 -4 0 -2.10 5.50 -8 4 0 5.10 2.30 8 4 0 4.00 1.50 -9 -4 0 128.89 21.60 -9 -4 0 122.79 12.00 -9 -4 0 111.69 11.20 -9 -4 0 90.49 19.60 9 -4 0 111.59 10.90 9 -4 0 105.89 10.80 -9 -4 0 102.69 18.20 9 4 0 106.09 11.40 -9 4 0 102.69 12.90 10 -4 0 4.00 1.20 -10 -4 0 -3.60 10.90 -10 -4 0 1.10 0.80 -10 -4 0 5.10 2.50 -10 4 0 2.00 1.70 10 4 0 2.50 1.50 -11 -4 0 24.10 3.50 -11 -4 0 20.40 3.10 11 -4 0 27.30 3.10 11 4 0 23.10 3.50 -11 4 0 19.40 4.20 12 -4 0 0.30 0.50 -12 -4 0 0.00 0.40 12 4 0 0.60 0.70 -12 4 0 1.30 1.20 -13 -4 0 13.40 1.70 13 -4 0 12.20 1.70 13 4 0 12.30 1.90 0 -5 0 -0.10 1.90 0 -5 0 0.10 2.40 -1 -5 0 31.40 7.40 -1 -5 0 45.70 7.90 -2 -5 0 4.70 3.30 -2 -5 0 4.40 3.50 2 5 0 1.30 2.20 -3 -5 0 337.37 36.70 -3 -5 0 262.57 38.80 -3 -5 0 388.86 32.60 3 -5 0 310.07 30.70 -3 -5 0 335.07 31.00 3 -5 0 343.27 30.70 3 -5 0 347.57 30.80 -4 -5 0 85.39 10.10 -4 -5 0 96.99 15.30 4 -5 0 95.79 9.60 -4 -5 0 98.99 15.00 -4 -5 0 111.79 10.00 5 -5 0 124.09 13.40 -5 -5 0 132.79 13.70 -5 -5 0 144.89 20.40 -5 -5 0 138.09 13.70 -5 -5 0 138.49 20.40 -5 -5 0 150.08 13.40 -5 -5 0 164.68 15.40 -5 5 0 133.49 16.10 -6 -5 0 253.57 25.20 -6 -5 0 276.97 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23 37.60 4.70 3 3 -23 57.49 5.60 -2 -3 23 22.90 2.90 -2 -3 23 21.10 2.70 2 -3 -23 27.80 2.80 -2 -3 23 18.00 2.70 2 3 -23 26.00 3.30 -1 -3 23 3.20 0.90 -1 -3 23 2.40 1.30 -1 -3 23 3.10 1.00 1 -3 -23 2.50 0.80 1 3 -23 1.40 1.00 -1 3 23 2.50 1.00 0 -3 23 13.10 2.00 0 -3 -23 17.80 2.20 0 -3 23 14.70 2.20 0 3 23 17.40 2.50 0 3 -23 11.00 3.20 -1 -3 -23 1.40 0.70 -1 -3 -23 2.40 1.60 1 -3 23 1.50 0.80 1 -3 23 2.70 0.90 1 3 23 2.00 0.80 -1 3 -23 -0.10 0.80 2 -3 23 36.50 3.60 -2 -3 -23 27.20 3.40 -2 -3 -23 30.90 4.00 2 3 23 36.80 3.90 -2 3 -23 26.20 4.10 -3 -3 -23 7.60 1.60 -3 3 -23 5.10 2.30 -3 3 -23 8.00 1.70 -4 -3 -23 7.30 1.70 4 -3 23 9.80 1.40 4 3 23 11.10 1.50 -5 -4 23 0.80 0.40 5 -4 -23 0.40 0.40 -5 -4 23 0.80 0.40 -5 -4 23 1.40 0.60 -5 4 23 0.20 0.70 5 4 -23 -0.40 0.50 -4 -4 23 12.20 2.00 4 -4 -23 15.10 1.90 -4 -4 23 11.70 2.30 4 4 -23 15.50 2.30 -4 4 23 17.20 2.40 -3 -4 23 14.70 1.80 3 -4 -23 14.90 1.70 -3 -4 23 10.70 1.90 -3 4 23 18.20 2.70 3 4 -23 12.80 2.60 2 -4 -23 30.50 3.10 -2 -4 23 28.70 3.10 -2 -4 23 23.80 2.90 -2 -4 23 25.50 3.50 2 4 -23 30.30 3.60 -1 -4 23 5.40 1.00 -1 -4 23 4.30 0.90 1 -4 -23 4.00 1.10 -1 4 23 6.60 1.40 0 -4 23 169.38 14.20 0 -4 23 163.58 13.70 0 -4 -23 132.69 13.50 0 4 -23 126.59 14.20 1 -4 23 0.10 0.80 1 -4 23 0.70 0.60 -1 -4 -23 0.10 0.60 1 4 23 0.50 0.60 -1 4 -23 0.00 0.70 -2 -4 -23 11.70 2.60 2 -4 23 12.80 1.70 2 4 23 14.80 1.90 3 -4 23 29.20 3.10 -3 -4 -23 25.00 3.60 3 4 23 29.60 3.20 -2 -5 23 62.39 5.80 2 5 -23 57.09 6.20 -1 -5 23 1.40 0.50 -1 5 23 2.10 0.70 1 5 -23 1.20 0.80 0 -5 23 27.60 3.40 0 5 23 35.80 3.60 -6 0 24 75.69 6.80 -6 0 24 58.29 7.10 -5 0 24 -0.60 0.70 5 0 -24 0.90 0.70 -5 0 24 1.00 0.80 5 0 -24 0.20 0.40 4 0 -24 87.49 9.20 4 0 -24 108.89 9.60 -4 0 24 97.49 9.30 3 0 -24 0.30 0.50 3 0 -24 -0.50 0.80 -3 0 24 -0.40 0.60 -3 0 24 -0.30 0.40 -2 0 24 0.90 0.60 -2 0 24 2.30 0.90 2 0 -24 0.70 0.60 2 0 -24 -0.30 0.80 -2 0 24 1.60 0.90 -1 0 24 -1.50 0.90 1 0 -24 1.60 0.80 -1 0 24 -0.20 0.30 1 0 -24 -0.10 1.60 -1 0 24 -0.20 0.70 1 0 -24 0.30 0.80 0 0 24 5.00 1.00 0 0 -24 4.20 0.90 0 0 24 2.70 0.90 0 0 -24 0.30 1.20 -1 0 -24 0.10 0.60 1 0 24 0.60 0.40 1 0 24 0.40 0.50 2 0 24 15.30 2.60 -2 0 -24 15.50 2.30 2 0 24 19.80 2.20 3 0 24 1.70 0.80 -3 0 -24 -0.80 0.50 3 0 24 -0.40 0.30 -4 0 -24 0.40 0.50 -4 0 -24 0.20 0.70 4 0 24 -0.40 0.30 4 0 24 0.00 0.40 -6 -1 24 19.30 2.60 6 1 -24 24.90 2.70 -6 1 24 25.60 2.60 -6 1 24 20.30 2.90 5 -1 -24 30.40 3.70 -5 -1 24 25.20 3.90 5 1 -24 37.40 3.70 -5 1 24 30.40 3.70 4 -1 -24 63.59 6.50 -4 1 24 68.79 6.70 4 1 -24 69.09 6.50 4 1 -24 63.59 6.80 3 -1 -24 1.70 0.50 -3 -1 24 0.80 0.90 -3 -1 24 1.40 0.70 -3 1 24 0.60 1.00 -3 1 24 1.40 0.70 3 1 -24 2.00 0.90 3 1 -24 1.00 0.70 2 -1 -24 137.09 12.40 -2 -1 24 118.99 12.10 2 1 -24 143.09 12.50 2 1 -24 130.09 12.80 1 -1 -24 2.80 0.80 -1 -1 24 2.10 0.90 -1 -1 24 3.20 0.80 -1 -1 24 2.70 1.30 -1 -1 24 2.50 0.90 -1 1 24 4.40 1.20 -1 1 24 4.50 1.20 1 1 -24 1.60 1.10 -1 1 24 2.20 1.00 0 -1 -24 58.89 5.40 0 -1 24 47.00 5.20 0 -1 24 49.40 5.50 0 -1 -24 38.30 6.20 0 1 24 55.39 5.70 0 1 -24 55.79 5.50 0 1 24 60.89 5.70 -1 -1 -24 8.10 2.50 -1 -1 -24 14.10 1.90 1 -1 24 9.30 1.60 1 -1 24 12.50 2.00 1 1 24 15.10 1.90 1 1 24 12.60 2.20 -1 1 -24 13.20 2.00 -2 -1 -24 0.60 0.60 2 -1 24 0.50 0.50 2 -1 24 0.20 0.50 -2 1 -24 -0.40 0.50 -2 1 -24 0.00 0.70 2 1 24 0.60 0.50 2 1 24 2.20 0.90 -3 -1 -24 18.70 2.50 -3 -1 -24 25.40 3.10 3 1 24 20.30 2.60 -3 1 -24 17.00 2.40 -4 -1 -24 45.10 4.60 -4 1 -24 44.80 4.60 -6 -2 24 33.90 4.10 6 -2 -24 44.00 4.10 -6 -2 24 36.90 4.10 6 2 -24 45.30 4.40 -6 2 24 45.90 4.30 -5 -2 24 3.50 0.80 5 -2 -24 4.60 0.90 -5 -2 24 4.50 0.90 -5 -2 24 4.30 1.10 5 2 -24 4.60 1.20 -5 2 24 6.70 1.20 -4 -2 24 3.20 0.80 -4 -2 24 2.90 0.90 -4 -2 24 4.50 1.10 -4 2 24 6.00 1.80 -4 2 24 5.30 1.20 4 2 -24 3.00 1.10 -3 -2 24 7.30 1.50 3 -2 -24 12.60 1.60 -3 -2 24 9.70 1.80 -3 2 24 9.50 2.00 3 2 -24 10.70 1.90 3 2 -24 11.50 1.80 -3 2 24 12.10 1.90 -2 -2 24 14.30 2.20 -2 -2 24 12.00 1.90 -2 -2 24 14.50 2.20 2 2 -24 17.40 2.20 -2 2 24 12.80 2.30 2 2 -24 14.80 2.40 -1 -2 24 5.40 1.40 -1 -2 24 4.80 1.30 1 -2 -24 9.30 1.50 -1 2 24 8.40 1.60 1 2 -24 7.50 2.00 0 -2 24 4.20 1.10 0 -2 -24 6.90 1.40 0 -2 24 6.30 1.20 0 2 -24 6.70 2.20 0 2 24 9.20 1.60 -1 -2 -24 87.99 10.30 -1 -2 -24 101.39 9.90 1 -2 24 109.89 10.00 1 2 24 116.89 10.20 -2 -2 -24 22.90 3.80 2 -2 24 25.70 2.90 2 2 24 23.50 2.90 -3 -2 -24 24.20 2.70 -3 2 -24 20.50 2.70 -4 -2 -24 3.90 1.20 -4 -2 -24 2.80 0.80 -4 2 -24 2.40 0.80 4 2 24 2.80 0.80 -5 -3 24 2.10 0.50 -5 -3 24 3.40 0.80 -5 -3 24 3.10 0.70 -5 3 24 3.60 0.90 5 3 -24 3.00 0.90 -4 -3 24 0.80 0.50 4 -3 -24 3.40 0.70 -4 -3 24 1.90 0.60 -4 -3 24 1.30 0.60 -4 3 24 2.30 0.90 4 3 -24 0.80 0.80 -3 -3 24 51.39 5.50 -3 -3 24 50.59 5.00 3 -3 -24 49.50 5.30 -3 -3 24 52.69 5.10 3 3 -24 46.10 6.00 -2 -3 24 3.90 0.80 -2 -3 24 2.50 0.90 2 -3 -24 3.60 0.80 -2 -3 24 4.30 0.80 2 3 -24 2.00 1.00 -2 3 24 3.00 1.00 -1 -3 24 45.00 4.70 -1 -3 24 42.60 4.90 1 -3 -24 49.10 4.60 0 -3 -24 15.40 2.00 0 -3 24 12.10 1.80 0 -3 24 14.70 1.90 0 3 24 16.90 2.20 -1 -3 -24 5.30 1.10 1 -3 24 4.20 1.10 1 3 24 4.30 1.20 -2 -3 -24 25.30 2.90 -2 -3 -24 31.60 4.00 -3 -3 -24 23.90 3.10 -3 -3 -24 18.30 2.10 3 4 -24 0.50 0.70 -3 4 24 0.10 0.60 2 -4 -24 19.90 2.30 -2 -4 24 20.80 2.30 -2 -4 24 23.80 2.30 -1 -4 24 1.50 0.60 -1 -4 24 1.00 0.40 -1 4 24 0.40 0.50 1 4 -24 0.30 0.70 0 -4 24 18.00 2.00 1 -4 24 41.90 4.40 1 4 24 51.19 4.80 -5 0 25 9.30 1.40 -5 0 25 9.10 1.60 5 0 -25 10.30 1.40 -4 0 25 0.50 0.50 4 0 -25 0.20 0.40 -4 0 25 1.60 0.70 -3 0 25 31.90 2.90 -3 0 25 22.40 3.10 3 0 -25 33.50 3.10 -3 0 25 22.40 2.90 -2 0 25 0.20 0.60 -2 0 25 -0.30 0.40 -2 0 25 0.00 1.20 -2 0 25 0.50 0.60 2 0 -25 -0.70 0.40 -1 0 25 1.20 0.60 0 0 25 0.40 0.50 0 0 -25 -2.10 1.40 0 0 -25 -0.50 0.70 0 0 25 -0.10 0.30 -1 0 -25 37.60 4.70 1 0 25 45.00 4.30 -1 0 -25 43.90 4.40 2 0 25 -0.30 0.40 -2 0 -25 -0.10 0.50 -2 0 -25 1.00 0.80 -3 0 -25 19.30 2.30 -3 0 -25 21.50 2.60 -5 -1 25 13.10 2.00 5 -1 -25 19.90 2.00 -5 -1 25 14.90 2.00 5 1 -25 16.40 2.50 -5 1 25 15.70 2.10 -5 1 25 20.80 2.50 -4 -1 25 5.10 1.00 -4 -1 25 5.00 1.10 4 1 -25 6.90 1.20 -4 1 25 4.70 1.00 -4 1 25 6.10 1.30 3 -1 -25 85.99 7.60 -3 -1 25 66.19 7.60 -3 1 25 70.19 7.80 3 1 -25 89.39 7.90 -3 1 25 83.19 7.80 -2 -1 25 1.90 0.70 -2 -1 25 0.60 0.80 -2 1 25 2.40 0.90 2 1 -25 3.30 0.80 2 1 -25 1.60 1.00 -1 -1 25 9.70 2.20 1 -1 -25 12.60 1.70 -1 1 25 15.10 1.90 1 1 -25 14.30 2.30 -1 1 25 11.00 2.10 0 -1 25 0.40 0.50 0 -1 -25 -0.10 0.50 0 1 -25 0.70 0.70 0 1 25 0.70 0.40 0 1 -25 -0.10 0.60 0 1 25 0.40 0.80 -1 -1 -25 5.80 1.70 -1 -1 -25 4.50 1.20 -1 1 -25 3.70 0.80 1 1 25 4.80 1.30 -2 -1 -25 16.40 2.30 -2 -1 -25 15.40 1.90 2 1 25 13.90 2.00 -2 1 -25 11.20 1.80 -3 -1 -25 22.00 2.70 -3 -1 -25 16.70 2.30 3 1 25 20.80 2.20 -3 1 -25 22.00 2.70 -4 -2 25 46.30 4.90 4 -2 -25 47.70 4.80 4 2 -25 47.60 4.90 -3 -2 25 28.30 3.30 -3 -2 25 35.40 3.50 3 -2 -25 38.80 3.40 -3 -2 25 25.50 3.30 3 2 -25 33.20 3.90 2 -2 -25 0.20 0.40 -2 -2 25 0.10 0.40 -2 -2 25 -0.40 0.50 2 2 -25 -0.30 0.50 2 2 -25 1.20 1.20 -2 2 25 -0.10 0.30 1 -2 -25 24.00 2.90 -1 -2 25 23.50 2.80 -1 2 25 23.40 2.80 0 -2 25 115.99 10.30 0 -2 -25 99.49 10.10 0 2 25 120.39 10.40 0 2 -25 96.89 10.50 1 -2 25 0.70 0.40 -1 -2 -25 0.50 0.40 -1 2 -25 -0.20 0.50 -1 2 -25 2.90 1.10 1 2 25 0.90 0.50 -2 -2 -25 57.59 6.20 2 2 25 67.19 6.20 -2 -3 25 0.80 0.40 -2 -3 25 0.30 0.50 2 -3 -25 0.40 0.40 2 3 -25 -0.50 0.40 -2 3 25 0.20 0.40 1 -3 -25 6.00 1.10 0 -3 25 32.50 3.30 0 3 25 31.00 3.40 2 0 -26 5.50 1.10 -2 0 26 4.70 1.00 1 0 -26 0.50 0.40 -1 0 26 0.60 0.60 0 0 26 9.60 1.50 0 0 -26 9.30 1.40 -2 1 26 9.00 1.30 -1 -1 26 -0.10 0.30 1 -1 -26 -0.40 0.30 -1 1 26 0.00 0.40 1 1 -26 0.20 0.80 0 1 26 4.20 0.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 87990 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_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_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.67648(14) 0.62278(19) 0.76482(7) 0.0458(4) Uani d . . . 1 . . O O2 0.07823(13) 0.82441(16) 0.61041(6) 0.0375(4) Uani d . . . 1 . . O O3 0.66820(17) 0.5182(2) 0.66841(8) 0.0608(5) Uani d . . . 1 . . N N1 0.22901(15) 0.49422(19) 0.49927(7) 0.0353(4) Uani d . . . 1 . . N N2 0.54035(17) 0.8208(2) 0.46963(8) 0.0446(4) Uani d . . . 1 . . C C1 0.17792(19) 0.7217(2) 0.83879(8) 0.0394(5) Uani d . . . 1 . . H H1 0.183817 0.719476 0.88372 0.047 Uiso calc U . R 1 . . C C2 0.26058(19) 0.6535(2) 0.80550(8) 0.0387(5) Uani d . . . 1 . . H H18 0.323487 0.605537 0.827611 0.046 Uiso calc U . R 1 . . C C3 0.25174(17) 0.6549(2) 0.73963(8) 0.0353(4) Uani d . . . 1 . . H H15 0.307497 0.605325 0.716881 0.042 Uiso calc U . R 1 . . C C4 0.16125(16) 0.7290(2) 0.70696(8) 0.0318(4) Uani d . . . 1 . . C C5 0.15078(16) 0.7420(2) 0.63651(8) 0.0306(4) Uani d . . . 1 . . C C6 0.22942(16) 0.6559(2) 0.59513(8) 0.0301(4) Uani d . . . 1 . . H H6 0.276059 0.580154 0.621151 0.036 Uiso calc U . R 1 . . C C7 0.30684(16) 0.7741(2) 0.56416(8) 0.0319(4) Uani d . . . 1 . . H H19 0.258963 0.861792 0.547386 0.038 Uiso calc U . R 1 . . C C8 0.39744(17) 0.8394(2) 0.61319(8) 0.0334(4) Uani d . . . 1 . . H H5 0.433215 0.930117 0.594513 0.04 Uiso calc U . R 1 . . H H20 0.359757 0.875399 0.650688 0.04 Uiso calc U . R 1 . . C C9 0.48737(17) 0.7269(2) 0.63436(8) 0.0353(4) Uani d . . . 1 . . H H21 0.513121 0.659726 0.603023 0.042 Uiso calc U . R 1 . . C C10 0.53494(17) 0.7112(2) 0.69262(9) 0.0355(4) Uani d . . . 1 . . H H22 0.506551 0.768102 0.726356 0.043 Uiso calc U . R 1 . . C C11 0.63175(18) 0.6060(2) 0.70544(9) 0.0386(5) Uani d . . . 1 . . C C12 0.7782(2) 0.5359(3) 0.78181(12) 0.0579(7) Uani d . . . 1 . . H H23 0.836997 0.560916 0.752592 0.069 Uiso calc U . R 1 . . H H24 0.762575 0.423905 0.779109 0.069 Uiso calc U . R 1 . . C C13 0.8176(3) 0.5792(4) 0.84815(12) 0.0626(7) Uani d . . . 1 . . H H3 0.823415 0.691644 0.851516 0.094 Uiso calc U . R 1 . . H H4 0.891536 0.532794 0.859023 0.094 Uiso calc U . R 1 . . H H2 0.763458 0.541387 0.877336 0.094 Uiso calc U . R 1 . . C C14 0.15656(16) 0.5711(2) 0.54283(8) 0.0317(4) Uani d . . . 1 . . H H14 0.106737 0.646999 0.518871 0.038 Uiso calc U . R 1 . . C C15 0.08668(16) 0.4392(2) 0.56413(8) 0.0333(4) Uani d . . . 1 . . C C16 0.00400(17) 0.4392(2) 0.60746(8) 0.0354(4) Uani d . . . 1 . . H H13 -0.014395 0.531501 0.628546 0.042 Uiso calc U . R 1 . . C C17 -0.05121(19) 0.3023(2) 0.61942(9) 0.0406(5) Uani d . . . 1 . . H H12 -0.10857 0.301241 0.648416 0.049 Uiso calc U . R 1 . . C C18 -0.0230(2) 0.1661(2) 0.58913(10) 0.0435(5) Uani d . . . 1 . . H H7 -0.060037 0.072651 0.598431 0.052 Uiso calc U . R 1 . . C C19 0.05882(19) 0.1662(2) 0.54553(10) 0.0412(5) Uani d . . . 1 . . H H8 0.077937 0.073683 0.524791 0.049 Uiso calc U . R 1 . . C C20 0.11212(17) 0.3040(2) 0.53281(8) 0.0360(4) Uani d . . . 1 . . C C21 0.19860(18) 0.3329(2) 0.48585(9) 0.0377(5) Uani d . . . 1 . . H H10 0.26444 0.263688 0.493221 0.045 Uiso calc U . R 1 . . H H9 0.166187 0.319805 0.441844 0.045 Uiso calc U . R 1 . . C C22 0.32271(17) 0.5636(2) 0.48259(8) 0.0358(4) Uani d . . . 1 . . H H11 0.364484 0.516714 0.451168 0.043 Uiso calc U . R 1 . . C C23 0.36074(17) 0.6991(2) 0.50887(8) 0.0342(4) Uani d . . . 1 . . C C24 0.45949(18) 0.7661(2) 0.48632(8) 0.0374(5) Uani d . . . 1 . . C C25 0.08647(19) 0.7933(2) 0.80685(9) 0.0411(5) Uani d . . . 1 . . H H16 0.02948 0.839232 0.829858 0.049 Uiso calc U . R 1 . . C C26 0.07832(18) 0.7979(2) 0.74103(9) 0.0373(4) Uani d . . . 1 . . H H17 0.016109 0.848046 0.719183 0.045 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0569(9) 0.0523(9) 0.0267(7) 0.0164(7) -0.0079(6) -0.0105(6) O2 0.0511(8) 0.0359(7) 0.0254(6) 0.0071(6) 0.0029(5) 0.0010(5) O3 0.0719(11) 0.0750(12) 0.0335(8) 0.0309(9) -0.0090(7) -0.0202(8) N1 0.0491(9) 0.0359(8) 0.0211(7) 0.0008(7) 0.0048(6) -0.0054(6) N2 0.0529(11) 0.0503(10) 0.0315(8) 0.0006(8) 0.0102(7) 0.0071(7) C1 0.0598(12) 0.0396(10) 0.0193(8) -0.0094(8) 0.0066(8) -0.0015(7) C2 0.0516(11) 0.0436(10) 0.0208(9) -0.0026(8) 0.0018(7) 0.0022(7) C3 0.0465(10) 0.0386(10) 0.0210(8) -0.0007(7) 0.0050(7) 0.0001(7) C4 0.0447(10) 0.0290(8) 0.0220(8) -0.0045(7) 0.0053(7) -0.0015(6) C5 0.0429(10) 0.0276(8) 0.0216(8) -0.0005(7) 0.0044(7) -0.0005(6) C6 0.0426(9) 0.0319(9) 0.0158(7) 0.0010(7) 0.0027(6) -0.0004(6) C7 0.0431(10) 0.0340(9) 0.0186(7) 0.0023(7) 0.0033(7) 0.0020(6) C8 0.0439(10) 0.0326(9) 0.0240(8) -0.0014(7) 0.0042(7) 0.0001(7) C9 0.0457(10) 0.0376(10) 0.0229(8) 0.0007(7) 0.0046(7) -0.0031(7) C10 0.0458(10) 0.0367(9) 0.0240(8) 0.0009(7) 0.0034(7) -0.0036(7) C11 0.0503(11) 0.0403(10) 0.0246(8) 0.0031(8) -0.0009(7) -0.0066(7) C12 0.0653(15) 0.0631(15) 0.0426(12) 0.0270(12) -0.0146(11) -0.0189(11) C13 0.0683(16) 0.0734(17) 0.0430(13) 0.0258(13) -0.0181(11) -0.0151(12) C14 0.0438(10) 0.0332(9) 0.0182(7) 0.0022(7) 0.0018(7) -0.0014(6) C15 0.0442(10) 0.0330(9) 0.0220(8) 0.0005(7) -0.0032(7) 0.0008(7) C16 0.0480(10) 0.0359(10) 0.0219(8) -0.0015(7) 0.0005(7) 0.0019(7) C17 0.0513(11) 0.0435(11) 0.0262(8) -0.0052(8) -0.0018(8) 0.0070(8) C18 0.0561(12) 0.0346(10) 0.0381(10) -0.0068(8) -0.0085(9) 0.0086(8) C19 0.0528(12) 0.0323(9) 0.0369(10) 0.0025(8) -0.0085(8) -0.0013(7) C20 0.0464(10) 0.0352(9) 0.0252(8) 0.0035(7) -0.0057(7) -0.0008(7) C21 0.0509(11) 0.0363(10) 0.0255(8) 0.0018(8) -0.0011(8) -0.0081(7) C22 0.0468(10) 0.0422(10) 0.0186(7) 0.0043(8) 0.0035(7) -0.0008(7) C23 0.0448(10) 0.0394(10) 0.0188(8) 0.0032(7) 0.0052(7) 0.0024(7) C24 0.0494(11) 0.0416(10) 0.0218(8) 0.0035(8) 0.0056(7) 0.0044(7) C25 0.0549(12) 0.0421(11) 0.0278(9) -0.0016(9) 0.0140(8) -0.0031(8) C26 0.0498(11) 0.0368(10) 0.0260(9) 0.0004(8) 0.0076(7) -0.0005(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 O1 C12 . . 116.51(16) ? C22 N1 C14 . . 120.02(16) ? C22 N1 C21 . . 125.22(16) ? C14 N1 C21 . . 114.04(16) ? C2 C1 C25 . . 120.28(17) ? C2 C1 H1 . . 119.9 ? C25 C1 H1 . . 119.9 ? C1 C2 C3 . . 120.10(19) ? C1 C2 H18 . . 120.0 ? C3 C2 H18 . . 120.0 ? C2 C3 C4 . . 120.17(18) ? C2 C3 H15 . . 119.9 ? C4 C3 H15 . . 119.9 ? C3 C4 C26 . . 119.26(16) ? C3 C4 C5 . . 122.52(17) ? C26 C4 C5 . . 118.19(17) ? O2 C5 C4 . . 120.17(16) ? O2 C5 C6 . . 117.97(15) ? C4 C5 C6 . . 121.86(16) ? C5 C6 C14 . . 108.08(15) ? C5 C6 C7 . . 109.07(14) ? C14 C6 C7 . . 109.29(13) ? C5 C6 H6 . . 110.1 ? C14 C6 H6 . . 110.1 ? C7 C6 H6 . . 110.1 ? C23 C7 C8 . . 111.20(16) ? C23 C7 C6 . . 109.75(15) ? C8 C7 C6 . . 111.25(14) ? C23 C7 H19 . . 108.2 ? C8 C7 H19 . . 108.2 ? C6 C7 H19 . . 108.2 ? C9 C8 C7 . . 114.31(15) ? C9 C8 H5 . . 108.7 ? C7 C8 H5 . . 108.7 ? C9 C8 H20 . . 108.7 ? C7 C8 H20 . . 108.7 ? H5 C8 H20 . . 107.6 ? C10 C9 C8 . . 126.50(17) ? C10 C9 H21 . . 116.7 ? C8 C9 H21 . . 116.7 ? C9 C10 C11 . . 120.56(17) ? C9 C10 H22 . . 119.7 ? C11 C10 H22 . . 119.7 ? O3 C11 O1 . . 123.17(19) ? O3 C11 C10 . . 125.85(18) ? O1 C11 C10 . . 110.97(16) ? O1 C12 C13 . . 107.63(18) ? O1 C12 H23 . . 110.2 ? C13 C12 H23 . . 110.2 ? O1 C12 H24 . . 110.2 ? C13 C12 H24 . . 110.2 ? H23 C12 H24 . . 108.5 ? C12 C13 H3 . . 109.5 ? C12 C13 H4 . . 109.5 ? H3 C13 H4 . . 109.5 ? C12 C13 H2 . . 109.5 ? H3 C13 H2 . . 109.5 ? H4 C13 H2 . . 109.5 ? N1 C14 C15 . . 101.87(15) ? N1 C14 C6 . . 110.08(15) ? C15 C14 C6 . . 116.20(14) ? N1 C14 H14 . . 109.5 ? C15 C14 H14 . . 109.5 ? C6 C14 H14 . . 109.5 ? C20 C15 C16 . . 120.13(18) ? C20 C15 C14 . . 110.77(17) ? C16 C15 C14 . . 129.09(17) ? C17 C16 C15 . . 119.08(19) ? C17 C16 H13 . . 120.5 ? C15 C16 H13 . . 120.5 ? C16 C17 C18 . . 120.4(2) ? C16 C17 H12 . . 119.8 ? C18 C17 H12 . . 119.8 ? C19 C18 C17 . . 120.56(19) ? C19 C18 H7 . . 119.7 ? C17 C18 H7 . . 119.7 ? C20 C19 C18 . . 118.74(19) ? C20 C19 H8 . . 120.6 ? C18 C19 H8 . . 120.6 ? C19 C20 C15 . . 121.0(2) ? C19 C20 C21 . . 128.02(19) ? C15 C20 C21 . . 110.96(17) ? N1 C21 C20 . . 101.62(15) ? N1 C21 H10 . . 111.4 ? C20 C21 H10 . . 111.4 ? N1 C21 H9 . . 111.4 ? C20 C21 H9 . . 111.4 ? H10 C21 H9 . . 109.3 ? N1 C22 C23 . . 122.60(17) ? N1 C22 H11 . . 118.7 ? C23 C22 H11 . . 118.7 ? C22 C23 C24 . . 118.20(17) ? C22 C23 C7 . . 122.51(18) ? C24 C23 C7 . . 119.14(17) ? N2 C24 C23 . . 178.3(2) ? C1 C25 C26 . . 119.89(19) ? C1 C25 H16 . . 120.1 ? C26 C25 H16 . . 120.1 ? C25 C26 C4 . . 120.3(2) ? C25 C26 H17 . . 119.9 ? C4 C26 H17 . . 119.9 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C11 . 1.339(2) ? O1 C12 . 1.449(3) ? O2 C5 . 1.222(2) ? O3 C11 . 1.196(3) ? N1 C22 . 1.336(3) ? N1 C14 . 1.467(2) ? N1 C21 . 1.468(3) ? N2 C24 . 1.150(3) ? C1 C2 . 1.383(3) ? C1 C25 . 1.387(3) ? C1 H1 . 0.95 ? C2 C3 . 1.392(2) ? C2 H18 . 0.95 ? C3 C4 . 1.395(3) ? C3 H15 . 0.95 ? C4 C26 . 1.397(3) ? C4 C5 . 1.494(2) ? C5 C6 . 1.522(2) ? C6 C14 . 1.544(2) ? C6 C7 . 1.554(2) ? C6 H6 . 1.0 ? C7 C23 . 1.521(2) ? C7 C8 . 1.550(3) ? C7 H19 . 1.0 ? C8 C9 . 1.493(3) ? C8 H5 . 0.99 ? C8 H20 . 0.99 ? C9 C10 . 1.328(3) ? C9 H21 . 0.95 ? C10 C11 . 1.479(3) ? C10 H22 . 0.95 ? C12 C13 . 1.498(3) ? C12 H23 . 0.99 ? C12 H24 . 0.99 ? C13 H3 . 0.98 ? C13 H4 . 0.98 ? C13 H2 . 0.98 ? C14 C15 . 1.502(3) ? C14 H14 . 1.0 ? C15 C20 . 1.392(3) ? C15 C16 . 1.392(3) ? C16 C17 . 1.389(3) ? C16 H13 . 0.95 ? C17 C18 . 1.396(3) ? C17 H12 . 0.95 ? C18 C19 . 1.389(3) ? C18 H7 . 0.95 ? C19 C20 . 1.388(3) ? C19 H8 . 0.95 ? C20 C21 . 1.502(3) ? C21 H10 . 0.99 ? C21 H9 . 0.99 ? C22 C23 . 1.364(3) ? C22 H11 . 0.95 ? C23 C24 . 1.423(3) ? C25 C26 . 1.392(3) ? C25 H16 . 0.95 ? C26 H17 . 0.95 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C21 H10 N2 3_666 0.99 2.51 3.449(3) 158.6 ? C22 H11 O3 3_666 0.95 2.55 3.287(2) 134.1 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C25 C1 C2 C3 . . . . -0.7(3) ? C1 C2 C3 C4 . . . . 1.9(3) ? C2 C3 C4 C26 . . . . -1.7(3) ? C2 C3 C4 C5 . . . . 176.48(18) ? C3 C4 C5 O2 . . . . -170.60(18) ? C26 C4 C5 O2 . . . . 7.6(3) ? C3 C4 C5 C6 . . . . 8.7(3) ? C26 C4 C5 C6 . . . . -173.06(17) ? O2 C5 C6 C14 . . . . -50.5(2) ? C4 C5 C6 C14 . . . . 130.15(17) ? O2 C5 C6 C7 . . . . 68.2(2) ? C4 C5 C6 C7 . . . . -111.12(18) ? C5 C6 C7 C23 . . . . -163.48(14) ? C14 C6 C7 C23 . . . . -45.51(19) ? C5 C6 C7 C8 . . . . 73.02(18) ? C14 C6 C7 C8 . . . . -169.01(15) ? C23 C7 C8 C9 . . . . -51.5(2) ? C6 C7 C8 C9 . . . . 71.2(2) ? C7 C8 C9 C10 . . . . -141.2(2) ? C8 C9 C10 C11 . . . . -173.40(19) ? C12 O1 C11 O3 . . . . 4.2(4) ? C12 O1 C11 C10 . . . . -174.8(2) ? C9 C10 C11 O3 . . . . -7.3(4) ? C9 C10 C11 O1 . . . . 171.57(19) ? C11 O1 C12 C13 . . . . 176.4(2) ? C22 N1 C14 C15 . . . . -162.80(16) ? C21 N1 C14 C15 . . . . 7.91(19) ? C22 N1 C14 C6 . . . . -38.9(2) ? C21 N1 C14 C6 . . . . 131.77(16) ? C5 C6 C14 N1 . . . . 176.44(14) ? C7 C6 C14 N1 . . . . 57.85(19) ? C5 C6 C14 C15 . . . . -68.48(19) ? C7 C6 C14 C15 . . . . 172.94(15) ? N1 C14 C15 C20 . . . . -3.41(19) ? C6 C14 C15 C20 . . . . -123.04(17) ? N1 C14 C15 C16 . . . . 178.04(18) ? C6 C14 C15 C16 . . . . 58.4(3) ? C20 C15 C16 C17 . . . . 0.8(3) ? C14 C15 C16 C17 . . . . 179.28(18) ? C15 C16 C17 C18 . . . . 1.0(3) ? C16 C17 C18 C19 . . . . -1.5(3) ? C17 C18 C19 C20 . . . . 0.2(3) ? C18 C19 C20 C15 . . . . 1.6(3) ? C18 C19 C20 C21 . . . . -177.08(18) ? C16 C15 C20 C19 . . . . -2.2(3) ? C14 C15 C20 C19 . . . . 179.13(17) ? C16 C15 C20 C21 . . . . 176.75(16) ? C14 C15 C20 C21 . . . . -2.0(2) ? C22 N1 C21 C20 . . . . 161.20(17) ? C14 N1 C21 C20 . . . . -8.9(2) ? C19 C20 C21 N1 . . . . -174.79(19) ? C15 C20 C21 N1 . . . . 6.4(2) ? C14 N1 C22 C23 . . . . 6.2(3) ? C21 N1 C22 C23 . . . . -163.44(18) ? N1 C22 C23 C24 . . . . -177.98(17) ? N1 C22 C23 C7 . . . . 6.6(3) ? C8 C7 C23 C22 . . . . 138.51(18) ? C6 C7 C23 C22 . . . . 15.0(2) ? C8 C7 C23 C24 . . . . -36.9(2) ? C6 C7 C23 C24 . . . . -160.42(16) ? C2 C1 C25 C26 . . . . -0.6(3) ? C1 C25 C26 C4 . . . . 0.7(3) ? C3 C4 C26 C25 . . . . 0.4(3) ? C5 C4 C26 C25 . . . . -177.85(18) ?