#------------------------------------------------------------------------------ #$Date: 2024-12-06 19:30:00 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296460 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/94/7249421.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_7249421 loop_ _publ_author_name 'Islam, Md Faizul' 'Wijesekera, Gamage Isuri P.' 'Sindt, Ammon J.' 'Smith, Mark D.' 'Shimizu, Linda S.' _publ_section_title ; Examination of photoinduced radicals in two crystal forms of triphenylamine bis-urea macrocycles ; _journal_issue 42 _journal_name_full CrystEngComm _journal_page_first 6025 _journal_page_last 6033 _journal_paper_doi 10.1039/D4CE00839A _journal_volume 26 _journal_year 2024 _chemical_formula_moiety 'C42 H38 N6 O2, 0.451(C4 H10 O2)' _chemical_formula_sum 'C43.81 H42.51 N6 O2.9' _chemical_formula_weight 699.40 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2023-05-04 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-03-31 deposited with the CCDC. 2024-10-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.800(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 15.7922(12) _cell_length_b 4.7118(4) _cell_length_c 26.096(2) _cell_measurement_reflns_used 3214 _cell_measurement_temperature 301(2) _cell_measurement_theta_max 24.724 _cell_measurement_theta_min 2.342 _cell_volume 1877.4(3) _computing_cell_refinement 'SAINT V8.40B (Bruker, 2016)' _computing_data_collection 'Bruker APEX3 v2019.1-0 (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40B (Bruker, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 301(2) _diffrn_detector PHOTON-II _diffrn_detector_area_resol_mean 7.39 _diffrn_detector_type 'area detector' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 QUEST' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_unetI/netI 0.0479 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 22436 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 23.256 _diffrn_reflns_theta_max 23.256 _diffrn_reflns_theta_min 2.342 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_type 'Incoatec I\ms' _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_T_max 0.4899 _exptl_absorpt_correction_T_min 0.4501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0971 before and 0.0607 after correction. The Ratio of minimum to maximum transmission is 0.9188. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.237 _exptl_crystal_description needle _exptl_crystal_F_000 741 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.705 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef 0.029(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 256 _refine_ls_number_reflns 2697 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.1235 _refine_ls_R_factor_gt 0.0834 _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^)+(0.1086P)^2^+1.4389P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2040 _refine_ls_wR_factor_ref 0.2310 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1750 _reflns_number_total 2697 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00839a2.cif _cod_data_source_block tpah_dme _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' 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 8170 2020-07-09 18:12:32Z antanas Adding full bibliography for 7249420--7249422.cif. ; _cod_original_formula_sum 'C43.81 H42.51 N6 O2.90' _cod_database_code 7249421 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.998 _shelx_estimated_absorpt_t_min 0.991 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O2S-C4S = O2S-C3S = O1S-C2S = O1S-C1S 1.45 with sigma of 0.015 C3S-C2S 1.54 with sigma of 0.015 O2S-C2S = O1S-C3S = C4S-C3S = C2S-C1S 2.36 with sigma of 0.02 H7-H1SB -2 with sigma of 0.02 3. Restrained planarity O1S, O2S, C1S, C2S, C3S, C4S with sigma of 0.1 4. Others Sof(O1S)=Sof(O2S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(H2SA)= Sof(H2SB)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)= FVAR(1) Uiso(O1S)=Uiso(O2S)=Uiso(C1S)=Uiso(C2S)=Uiso(C3S)=Uiso(C4S)=FVAR(2) 5.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C21(H21A,H21B), C2S(H2SA,H2SB), C3S(H3SA,H3SB) 5.b Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20) 5.c Idealised Me refined with riding coordinates: C1S(H1SA,H1SB,H1SC) 5.d Idealised Me refined as rotating group: C4S(H4SA,H4SB,H4SC) ; _shelx_res_file ; TITL tpah_dme_a.res in P2(1)/c tpah_dme.res created by SHELXL-2018/3 at 21:01:26 on 04-May-2023 REM Old TITL tpah_dme in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.236, Rweak 0.030, Alpha 0.062 REM 0.546 for 383 systematic absences, Orientation as input REM Formula found by SHELXT: C19 N5 O CELL 0.71073 15.7922 4.7118 26.0964 90 104.8 90 ZERR 2 0.0012 0.0004 0.002 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 87.61 85.01 12 5.8 DFIX 1.45 0.015 O2S C4S O2S C3S O1S C2S O1S C1S DFIX 1.54 0.015 C3S C2S DFIX 2.36 O2S C2S O1S C3S C4S C3S C2S C1S FLAT O1S O2S C1S C2S C3S C4S DFIX -2 H7 H1Sb L.S. 15 PLAN 9 SIZE 0.03 0.06 0.12 TEMP 28(2) CONF list 4 MORE -1 BOND $H fmap 2 53 acta OMIT -2 0 2 REM REM REM WGHT 0.108600 1.438900 EXTI 0.028506 FVAR 0.71237 0.22533 0.18908 O1 4 0.581214 0.902919 0.334540 11.00000 0.07451 0.04491 = 0.07624 0.00066 0.00747 -0.00602 N1 3 0.507119 0.487927 0.316470 11.00000 0.05743 0.04936 = 0.07880 -0.00309 0.01304 -0.00529 H1 2 0.510420 0.294203 0.314467 11.00000 0.06849 N2 3 0.654043 0.485558 0.351776 11.00000 0.05319 0.04852 = 0.06407 -0.00324 0.00782 -0.00184 H2 2 0.648944 0.303057 0.354812 11.00000 0.06064 N3 3 0.840445 0.648478 0.600022 11.00000 0.06230 0.10079 = 0.05433 0.00692 0.01315 -0.00629 C1 1 0.581039 0.641236 0.334319 11.00000 0.05844 0.04463 = 0.04400 -0.00269 0.01318 -0.00904 C2 1 0.739343 0.614317 0.372907 11.00000 0.05492 0.07676 = 0.05875 -0.00253 0.01688 -0.00245 AFIX 23 H2A 2 0.738267 0.805681 0.359052 11.00000 -1.20000 H2B 2 0.782618 0.507641 0.360373 11.00000 -1.20000 AFIX 0 C3 1 0.767501 0.626918 0.432372 11.00000 0.04987 0.05777 = 0.05462 0.00180 0.01445 -0.00476 C4 1 0.845526 0.514455 0.461360 11.00000 0.06015 0.10679 = 0.06110 0.01114 0.02329 0.02037 AFIX 43 H4 2 0.882853 0.430151 0.443437 11.00000 -1.20000 AFIX 0 C5 1 0.870311 0.522122 0.515796 11.00000 0.05602 0.11077 = 0.05838 0.02046 0.01649 0.02171 AFIX 43 H5 2 0.923475 0.442647 0.533842 11.00000 -1.20000 AFIX 0 C6 1 0.817784 0.645002 0.543617 11.00000 0.05411 0.07335 = 0.05277 0.00521 0.00943 -0.00134 C7 1 0.739870 0.762283 0.515732 11.00000 0.06959 0.09355 = 0.05781 -0.01846 0.01314 0.01749 AFIX 43 H7 2 0.703454 0.849688 0.533915 11.00000 -1.20000 AFIX 0 C8 1 0.715148 0.751787 0.461183 11.00000 0.06162 0.08857 = 0.06636 -0.00907 0.00469 0.01743 AFIX 43 H8 2 0.661838 0.830761 0.443253 11.00000 -1.20000 AFIX 0 C9 1 0.928023 0.701153 0.628692 11.00000 0.05271 0.06582 = 0.06409 -0.00412 0.00734 0.00465 C10 1 0.977872 0.895258 0.610744 11.00000 0.08621 0.08081 = 0.11828 0.01319 0.00089 -0.02092 AFIX 43 H10 2 0.954448 0.991353 0.579174 11.00000 -1.20000 AFIX 0 C11 1 1.062055 0.949457 0.638870 11.00000 0.08534 0.11855 = 0.16270 -0.02189 0.00946 -0.03559 AFIX 43 H11 2 1.095337 1.081800 0.626131 11.00000 -1.20000 AFIX 0 C12 1 1.097577 0.812544 0.685110 11.00000 0.05921 0.15808 = 0.12945 -0.07069 -0.00195 0.00304 AFIX 43 H12 2 1.154753 0.850441 0.704155 11.00000 -1.20000 AFIX 0 C13 1 1.048637 0.620794 0.702971 11.00000 0.07435 0.18036 = 0.08276 -0.01392 -0.00228 0.03941 AFIX 43 H13 2 1.072476 0.527196 0.734761 11.00000 -1.20000 AFIX 0 C14 1 0.964229 0.560555 0.675212 11.00000 0.06641 0.13015 = 0.07127 0.01759 0.00979 0.01364 AFIX 43 H14 2 0.931793 0.425204 0.687879 11.00000 -1.20000 AFIX 0 C15 1 0.775710 0.586487 0.627245 11.00000 0.05146 0.06941 = 0.05217 -0.00327 0.00558 -0.00125 C16 1 0.772483 0.725305 0.673179 11.00000 0.05401 0.09260 = 0.06903 -0.02115 0.00868 -0.01982 AFIX 43 H16 2 0.813352 0.866099 0.686711 11.00000 -1.20000 AFIX 0 C17 1 0.709427 0.658409 0.699429 11.00000 0.05634 0.09240 = 0.05535 -0.01917 0.00997 -0.00975 AFIX 43 H17 2 0.710197 0.751117 0.731006 11.00000 -1.20000 AFIX 0 C18 1 0.645945 0.460254 0.680451 11.00000 0.04953 0.06795 = 0.05597 0.00011 0.00767 -0.00121 C19 1 0.648842 0.325033 0.634353 11.00000 0.09702 0.08360 = 0.06842 -0.01706 0.02616 -0.04002 AFIX 43 H19 2 0.606632 0.189060 0.620252 11.00000 -1.20000 AFIX 0 C20 1 0.712797 0.385234 0.608242 11.00000 0.11392 0.08236 = 0.06792 -0.02729 0.03921 -0.02870 AFIX 43 H20 2 0.713099 0.287620 0.577315 11.00000 -1.20000 AFIX 0 C21 1 0.577553 0.389816 0.708680 11.00000 0.06370 0.07968 = 0.06346 0.00609 0.00848 -0.00164 AFIX 23 H21A 2 0.571712 0.185188 0.709988 11.00000 -1.20000 H21B 2 0.596374 0.458498 0.744855 11.00000 -1.20000 AFIX 0 PART -1 O1S 4 0.491215 0.519289 0.538357 21.00000 31.00000 O2S 4 0.513286 1.175725 0.470832 21.00000 31.00000 C1S 1 0.479763 0.223556 0.517600 21.00000 31.00000 AFIX 133 H1SA 2 0.509004 0.094337 0.544841 21.00000 -1.50000 H1SB 2 0.504410 0.207352 0.487694 21.00000 -1.50000 H1SC 2 0.418492 0.178339 0.506884 21.00000 -1.50000 AFIX 0 C2S 1 0.494403 0.703252 0.496351 21.00000 31.00000 AFIX 23 H2SA 2 0.440167 0.689421 0.468772 21.00000 -1.20000 H2SB 2 0.542106 0.647966 0.481298 21.00000 -1.20000 AFIX 0 C3S 1 0.507567 1.001530 0.515789 21.00000 31.00000 AFIX 23 H3SA 2 0.458790 1.062235 0.529393 21.00000 -1.20000 H3SB 2 0.560996 1.017072 0.543962 21.00000 -1.20000 AFIX 0 C4S 1 0.525463 1.464451 0.488598 21.00000 31.00000 AFIX 137 H4SA 2 0.544347 1.576146 0.462804 21.00000 -1.50000 H4SB 2 0.569037 1.472060 0.521819 21.00000 -1.50000 H4SC 2 0.471155 1.538399 0.493064 21.00000 -1.50000 AFIX 0 HKLF 4 REM tpah_dme_a.res in P2(1)/c REM wR2 = 0.230974, GooF = S = 1.05379, Restrained GooF = 1.05744 for all data REM R1 = 0.083443 for 1750 Fo > 4sig(Fo) and 0.123469 for all 2697 data REM 256 parameters refined using 12 restraints END WGHT 0.1087 1.4367 REM Highest difference peak 0.705, deepest hole -0.249, 1-sigma level 0.055 Q1 1 1.1882 0.8413 0.7224 11.00000 0.05 0.71 Q2 1 0.5231 1.2437 0.4625 11.00000 0.05 0.31 Q3 1 0.5392 0.9820 0.5083 11.00000 0.05 0.26 Q4 1 0.5004 1.1247 0.4803 11.00000 0.05 0.24 Q5 1 0.8681 0.2810 0.4369 11.00000 0.05 0.18 Q6 1 0.6949 0.7005 0.5577 11.00000 0.05 0.15 Q7 1 0.6446 0.5617 0.4195 11.00000 0.05 0.14 Q8 1 0.7740 0.8423 0.4600 11.00000 0.05 0.14 Q9 1 0.6459 0.6602 0.4816 11.00000 0.05 0.14 ; _shelx_res_checksum 99538 _shelx_hkl_file ; -2 0 0 289.97 11.40 2 0 0 303.27 10.70 2 0 0 305.37 9.10 2 0 0 310.57 11.90 -3 0 0 4.60 3.60 -3 0 0 5.30 6.40 3 0 0 14.60 4.80 3 0 0 13.50 4.00 3 0 0 5.50 5.60 -3 0 0 5.40 3.50 -4 0 0 933.31 24.10 4 0 0 944.41 27.90 -4 0 0 901.91 27.50 4 0 0 931.91 24.20 -4 0 0 929.11 30.00 4 0 0 924.61 30.10 -5 0 0 197.58 14.40 5 0 0 216.58 15.90 -5 0 0 201.18 12.80 5 0 0 194.88 10.20 -5 0 0 201.88 10.30 6 0 0 290.37 19.40 -6 0 0 289.87 13.00 -6 0 0 297.67 16.70 6 0 0 309.27 17.30 6 0 0 288.17 13.30 -6 0 0 309.97 18.80 -7 0 0 33.30 11.80 -7 0 0 32.10 8.50 -7 0 0 44.50 7.60 7 0 0 33.10 10.80 7 0 0 46.20 10.80 7 0 0 42.90 8.00 8 0 0 0.70 9.50 8 0 0 6.10 5.40 8 0 0 -1.60 6.40 9 0 0 346.97 21.80 -9 0 0 356.76 22.10 9 0 0 348.37 25.80 9 0 0 334.27 16.50 -9 0 0 339.37 17.00 -9 0 0 345.27 23.40 10 0 0 186.58 13.40 10 0 0 208.48 21.80 -10 0 0 186.18 13.30 -10 0 0 175.98 17.20 10 0 0 206.38 18.30 -10 0 0 210.78 20.30 -11 0 0 147.39 23.00 -11 0 0 98.19 12.90 -11 0 0 112.79 15.20 11 0 0 112.79 15.30 -11 0 0 111.49 10.90 11 0 0 99.79 11.00 11 0 0 100.19 20.40 -12 0 0 149.99 13.40 -12 0 0 160.48 19.50 -12 0 0 181.08 19.50 -12 0 0 169.68 17.00 12 0 0 172.28 23.10 -13 0 0 133.49 13.50 -13 0 0 143.59 19.00 -13 0 0 132.09 16.50 13 0 0 160.88 19.50 -13 0 0 126.99 23.00 13 0 0 214.68 32.30 14 0 0 196.58 25.20 14 0 0 145.29 24.50 -14 0 0 191.18 15.70 -14 0 0 165.78 20.90 -14 0 0 200.78 19.40 -15 0 0 68.49 15.80 -15 0 0 67.69 13.10 15 0 0 37.50 20.70 15 0 0 44.20 14.60 -15 0 0 53.49 18.50 16 0 0 69.09 16.70 -16 0 0 33.70 14.00 -16 0 0 67.29 13.20 16 0 0 38.20 19.50 -16 0 0 56.99 15.60 0 -1 0 7.20 5.70 0 -1 0 0.60 2.60 0 -1 0 1.00 2.60 0 1 0 1.40 5.60 1 -1 0 4720.33 100.59 1 -1 0 4812.22 96.39 -1 -1 0 4622.34 102.49 1 -1 0 4836.52 95.49 -1 -1 0 4752.72 96.79 -1 1 0 4682.73 100.89 1 1 0 4800.82 96.59 -1 1 0 4818.02 95.39 1 1 0 4674.03 102.99 -1 1 0 4795.52 96.09 -2 -1 0 282.47 15.00 2 -1 0 317.87 11.80 2 -1 0 300.57 11.80 -2 -1 0 310.57 13.90 2 -1 0 300.87 12.80 -2 -1 0 308.17 12.30 -2 1 0 311.37 11.70 -2 1 0 294.67 13.30 2 1 0 318.57 16.70 2 1 0 288.67 11.90 -2 1 0 299.37 11.20 3 -1 0 2680.43 58.99 -3 -1 0 2639.94 60.19 3 -1 0 2672.33 59.79 -3 -1 0 2564.54 62.79 3 -1 0 2634.74 59.89 -3 -1 0 2651.03 64.79 -3 1 0 2550.44 58.89 3 1 0 2661.13 65.39 3 1 0 2616.94 63.29 -3 1 0 2629.64 59.19 -3 1 0 2610.14 59.59 3 1 0 2603.34 60.09 -4 -1 0 391.16 17.20 -4 -1 0 389.06 19.30 4 -1 0 401.86 14.90 -4 -1 0 412.26 19.80 4 -1 0 406.96 18.10 4 -1 0 403.76 16.90 -4 1 0 401.96 15.40 4 1 0 395.86 17.00 4 1 0 404.96 20.70 4 1 0 405.46 20.00 -4 1 0 399.86 17.50 5 -1 0 1239.18 36.20 -5 -1 0 1197.88 35.60 -5 -1 0 1143.89 38.30 -5 -1 0 1169.58 36.30 5 -1 0 1255.97 31.80 5 -1 0 1202.48 37.70 -5 -1 0 1271.37 40.20 -5 1 0 1217.88 36.90 5 1 0 1217.68 39.60 -5 1 0 1197.48 32.30 5 1 0 1166.68 39.50 5 1 0 1209.78 36.30 -6 -1 0 -1.20 5.50 -6 -1 0 -0.20 6.00 -6 -1 0 -0.90 7.50 6 -1 0 4.30 4.40 6 -1 0 2.90 7.60 -6 -1 0 -0.30 8.10 6 -1 0 3.40 5.50 6 1 0 0.70 4.90 -6 1 0 0.60 4.30 6 1 0 9.00 8.30 -6 1 0 1.20 6.60 -6 1 0 9.70 5.80 7 -1 0 80.69 13.00 -7 -1 0 66.19 11.10 -7 -1 0 72.69 14.00 7 -1 0 62.89 13.90 -7 -1 0 65.89 13.60 7 -1 0 62.79 7.50 -7 -1 0 65.39 12.30 -7 1 0 65.19 11.70 -7 1 0 63.09 7.50 -7 1 0 54.29 12.20 7 1 0 72.99 15.60 7 1 0 70.49 11.70 -8 -1 0 509.25 28.80 8 -1 0 493.65 24.90 8 -1 0 517.45 18.90 -8 -1 0 407.46 24.50 -8 -1 0 524.35 23.70 -8 -1 0 494.55 25.50 8 -1 0 545.05 28.60 -8 1 0 533.05 19.90 -8 1 0 493.15 26.20 -8 1 0 501.55 25.00 8 1 0 539.25 25.70 8 1 0 530.75 30.10 -9 -1 0 3.60 9.70 9 -1 0 -2.10 6.10 9 -1 0 2.10 4.70 -9 -1 0 -10.80 5.20 -9 -1 0 -6.20 4.70 9 -1 0 -4.40 8.00 -9 -1 0 -0.60 7.30 9 1 0 -1.40 9.60 -9 1 0 -1.90 8.20 -9 1 0 -4.40 3.90 9 1 0 -3.20 6.00 -9 1 0 -2.60 4.50 -10 -1 0 17.60 11.50 10 -1 0 -1.60 6.10 -10 -1 0 3.60 8.50 -10 -1 0 27.40 8.70 -10 -1 0 5.00 7.30 10 -1 0 4.40 8.60 10 -1 0 3.20 5.50 -10 1 0 1.40 7.80 -10 1 0 2.70 5.00 10 1 0 10.80 9.10 10 1 0 -0.40 10.00 -10 1 0 6.30 6.40 -11 -1 0 8.00 8.30 11 -1 0 23.10 7.30 -11 -1 0 21.60 9.90 11 -1 0 16.30 9.80 -11 -1 0 8.50 9.80 11 -1 0 1.10 10.40 -11 -1 0 -4.90 9.00 11 1 0 15.00 8.90 -11 1 0 5.30 5.80 -11 1 0 8.50 7.90 -11 1 0 8.10 9.40 11 1 0 0.60 11.00 -12 -1 0 39.10 12.20 -12 -1 0 15.70 12.10 -12 -1 0 21.50 11.10 12 -1 0 28.90 13.00 12 -1 0 20.40 8.10 12 -1 0 31.90 16.20 -12 -1 0 30.90 10.60 -12 1 0 21.20 10.60 12 1 0 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10.10 2 2 -26 -2.60 11.00 -2 2 26 -10.30 6.50 2 2 -26 10.10 10.50 1 -2 -26 -0.70 10.70 -1 -2 26 5.60 11.10 1 -2 -26 21.50 14.70 1 -2 -26 9.10 7.40 1 2 -26 -5.90 10.10 1 2 -26 17.00 10.30 -1 2 26 -1.50 7.30 10 0 -27 2.20 8.00 -10 0 27 6.70 10.40 10 0 -27 -2.90 8.80 10 0 -27 -6.20 11.10 -10 0 27 -5.00 9.40 -9 0 27 -0.90 7.80 9 0 -27 5.70 9.80 9 0 -27 1.40 11.20 9 0 -27 23.00 9.20 -9 0 27 22.40 11.40 -8 0 27 6.50 9.00 8 0 -27 1.10 8.70 8 0 -27 2.40 12.20 7 0 -27 0.20 8.50 7 0 -27 -0.60 8.70 -7 0 27 8.80 8.80 -7 0 27 36.90 12.80 6 0 -27 -4.10 10.10 -6 0 27 -9.80 8.80 -6 0 27 22.40 8.80 6 0 -27 2.20 12.10 5 0 -27 1.30 8.00 -5 0 27 5.90 8.30 5 0 -27 -9.60 7.30 4 0 -27 6.50 11.50 4 0 -27 33.90 11.70 -4 0 27 13.60 8.50 -3 0 27 70.09 17.60 3 0 -27 4.80 10.70 2 0 -27 0.50 10.40 2 0 -27 -0.70 9.80 -2 0 27 -6.60 5.50 1 0 -27 21.10 10.60 1 0 -27 -4.30 7.80 0 0 27 2.50 8.60 0 0 -27 -8.60 9.20 0 0 -27 14.40 12.70 0 0 -27 44.80 15.90 2 0 27 4.80 10.30 -2 0 -27 1.40 9.40 -2 0 -27 -5.70 11.00 -9 -1 27 4.20 9.10 9 -1 -27 7.80 12.70 9 -1 -27 -5.30 8.30 -9 1 27 -13.40 9.00 -9 1 27 3.80 9.10 9 1 -27 -0.90 9.70 9 1 -27 -7.50 6.80 9 1 -27 27.50 13.20 -8 -1 27 7.50 8.80 8 -1 -27 20.60 14.00 8 -1 -27 15.60 10.40 -8 1 27 8.80 10.70 -8 1 27 20.60 10.70 8 1 -27 3.30 11.70 8 1 -27 9.80 11.30 7 -1 -27 7.10 10.30 7 -1 -27 0.30 8.80 -7 -1 27 26.70 10.80 -7 1 27 3.50 7.90 7 1 -27 11.70 11.40 -7 1 27 15.30 13.50 7 1 -27 -12.70 9.90 6 -1 -27 9.40 12.50 6 -1 -27 25.80 11.80 -6 -1 27 24.00 13.70 -6 1 27 16.80 9.90 6 1 -27 10.20 12.90 -6 1 27 11.20 11.80 6 1 -27 36.40 16.00 -5 -1 27 16.40 10.20 5 -1 -27 -1.80 9.00 5 -1 -27 16.50 13.70 5 1 -27 19.60 12.80 5 1 -27 7.90 12.30 4 -1 -27 -14.00 8.90 -4 -1 27 -4.00 7.90 4 -1 -27 2.80 13.00 4 1 -27 -11.60 8.60 4 1 -27 0.80 10.60 -4 1 27 -2.90 7.60 -3 -1 27 0.20 8.80 3 -1 -27 6.60 11.00 3 -1 -27 -14.80 9.60 3 1 -27 20.40 14.10 3 1 -27 6.80 10.80 -3 1 27 17.20 10.20 2 -1 -27 5.80 10.20 -2 -1 27 -1.70 8.50 2 -1 -27 -1.30 10.60 2 1 -27 -8.60 8.60 -2 1 27 -13.90 7.20 2 1 -27 -4.20 9.90 -1 -1 27 5.90 10.50 1 -1 -27 4.70 10.90 1 -1 -27 0.00 8.70 1 -1 -27 -3.80 6.20 -1 1 27 -1.10 8.30 1 1 -27 8.00 10.30 1 1 -27 2.30 9.00 1 1 -27 0.30 11.10 0 1 27 55.09 11.80 0 1 -27 21.40 13.80 1 -1 27 30.00 13.90 -1 -1 -27 8.00 8.90 -1 -1 -27 3.20 11.10 1 1 27 -0.20 10.20 -1 1 -27 7.30 13.50 -1 1 -27 -2.70 9.40 -1 1 -27 24.60 12.00 -8 0 28 1.40 9.20 8 0 -28 11.40 11.20 8 0 -28 33.70 13.90 -8 0 28 10.90 11.20 -7 0 28 17.90 8.80 7 0 -28 -3.70 9.90 7 0 -28 17.20 13.20 -6 0 28 43.70 13.20 6 0 -28 18.70 14.80 6 0 -28 41.20 16.30 -5 0 28 18.40 9.40 5 0 -28 15.90 12.80 5 0 -28 15.50 12.10 -4 0 28 12.40 8.20 4 0 -28 11.60 12.40 4 0 -28 3.00 10.70 -3 0 28 -2.70 9.20 3 0 -28 0.40 9.90 3 0 -28 0.20 11.00 -2 0 28 -5.70 6.30 2 0 -28 18.00 12.10 2 0 -28 -4.20 10.20 1 0 -28 -2.60 9.00 1 0 -28 6.20 9.10 -1 0 28 -2.30 5.40 1 0 -28 -6.80 9.60 0 0 -28 -16.90 8.80 0 0 -28 -3.00 9.00 0 0 28 11.90 10.10 0 0 -28 1.00 10.30 7 -1 -28 -1.90 9.40 7 -1 -28 9.20 10.10 -7 -1 28 47.20 15.40 -7 1 28 4.00 8.50 7 1 -28 10.90 11.90 -7 1 28 8.60 12.60 7 1 -28 24.70 13.60 -6 -1 28 16.10 11.10 6 -1 -28 1.40 8.70 6 -1 -28 4.10 13.10 6 1 -28 1.10 12.00 -6 1 28 6.40 9.40 6 1 -28 14.30 11.90 5 -1 -28 -15.80 9.70 5 -1 -28 -4.30 9.50 -5 -1 28 8.30 10.10 5 1 -28 -1.10 10.10 5 1 -28 3.50 10.80 4 -1 -28 -12.20 10.40 -4 -1 28 4.20 10.10 -4 1 28 12.00 9.10 4 1 -28 1.70 10.70 3 -1 -28 8.60 11.50 -3 -1 28 -2.50 8.70 3 -1 -28 -14.10 7.90 3 1 -28 -7.60 10.70 3 1 -28 -4.40 10.60 -3 1 28 -7.80 7.10 -2 -1 28 42.50 15.40 2 -1 -28 18.00 14.50 2 -1 -28 8.20 11.80 -2 1 28 9.90 10.90 2 1 -28 13.50 14.60 2 1 -28 3.20 11.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 50734 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_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 0.58121(19) 0.9029(6) 0.33454(12) 0.0674(9) Uani 1 1 d . . . . . N1 N 0.5071(2) 0.4879(9) 0.31647(15) 0.0627(10) Uani 1 1 d . . . . . H1 H 0.510(3) 0.294(11) 0.3145(16) 0.068(14) Uiso 1 1 d . . . . . N2 N 0.6540(2) 0.4856(9) 0.35178(14) 0.0566(10) Uani 1 1 d . . . . . H2 H 0.649(3) 0.303(10) 0.3548(16) 0.061(13) Uiso 1 1 d . . . . . N3 N 0.8404(2) 0.6485(9) 0.60002(14) 0.0728(12) Uani 1 1 d . . . . . C1 C 0.5810(3) 0.6412(9) 0.33432(14) 0.0490(10) Uani 1 1 d . . . . . C2 C 0.7393(3) 0.6143(10) 0.37291(16) 0.0630(12) Uani 1 1 d . . . . . H2A H 0.738267 0.805681 0.359052 0.076 Uiso 1 1 calc R U . . . H2B H 0.782618 0.507641 0.360373 0.076 Uiso 1 1 calc R U . . . C3 C 0.7675(3) 0.6269(9) 0.43237(16) 0.0539(11) Uani 1 1 d . . . . . C4 C 0.8455(3) 0.5145(12) 0.46136(18) 0.0746(14) Uani 1 1 d . . . . . H4 H 0.882853 0.430151 0.443437 0.090 Uiso 1 1 calc R U . . . C5 C 0.8703(3) 0.5221(11) 0.51580(18) 0.0747(15) Uani 1 1 d . . . . . H5 H 0.923475 0.442647 0.533842 0.090 Uiso 1 1 calc R U . . . C6 C 0.8178(3) 0.6450(10) 0.54362(16) 0.0608(12) Uani 1 1 d . . . . . C7 C 0.7399(3) 0.7623(11) 0.51573(18) 0.0742(14) Uani 1 1 d . . . . . H7 H 0.703454 0.849688 0.533915 0.089 Uiso 1 1 calc DR U . . . C8 C 0.7151(3) 0.7518(11) 0.46118(18) 0.0743(14) Uani 1 1 d . . . . . H8 H 0.661838 0.830761 0.443253 0.089 Uiso 1 1 calc R U . . . C9 C 0.9280(3) 0.7012(10) 0.62869(17) 0.0623(12) Uani 1 1 d . . . . . C10 C 0.9779(4) 0.8953(12) 0.6107(3) 0.0997(19) Uani 1 1 d . . . . . H10 H 0.954448 0.991353 0.579174 0.120 Uiso 1 1 calc R U . . . C11 C 1.0621(4) 0.9495(16) 0.6389(4) 0.126(3) Uani 1 1 d . . . . . H11 H 1.095337 1.081800 0.626131 0.151 Uiso 1 1 calc R U . . . C12 C 1.0976(4) 0.813(2) 0.6851(4) 0.120(3) Uani 1 1 d . . . . . H12 H 1.154753 0.850441 0.704155 0.144 Uiso 1 1 calc R U . . . C13 C 1.0486(4) 0.6208(19) 0.7030(2) 0.117(3) Uani 1 1 d . . . . . H13 H 1.072476 0.527196 0.734761 0.140 Uiso 1 1 calc R U . . . C14 C 0.9642(3) 0.5606(14) 0.6752(2) 0.0907(17) Uani 1 1 d . . . . . H14 H 0.931793 0.425204 0.687879 0.109 Uiso 1 1 calc R U . . . C15 C 0.7757(3) 0.5865(10) 0.62724(16) 0.0591(11) Uani 1 1 d . . . . . C16 C 0.7725(3) 0.7253(11) 0.67318(18) 0.0732(14) Uani 1 1 d . . . . . H16 H 0.813352 0.866099 0.686711 0.088 Uiso 1 1 calc R U . . . C17 C 0.7094(3) 0.6584(11) 0.69943(17) 0.0688(13) Uani 1 1 d . . . . . H17 H 0.710197 0.751117 0.731006 0.083 Uiso 1 1 calc R U . . . C18 C 0.6459(3) 0.4603(10) 0.68045(17) 0.0589(11) Uani 1 1 d . . . . . C19 C 0.6488(3) 0.3250(11) 0.63435(19) 0.0821(15) Uani 1 1 d . . . . . H19 H 0.606632 0.189060 0.620252 0.099 Uiso 1 1 calc R U . . . C20 C 0.7128(4) 0.3852(11) 0.60824(19) 0.0852(16) Uani 1 1 d . . . . . H20 H 0.713099 0.287620 0.577315 0.102 Uiso 1 1 calc R U . . . C21 C 0.5776(3) 0.3898(11) 0.70868(18) 0.0704(13) Uani 1 1 d . . . . . H21A H 0.571712 0.185188 0.709988 0.084 Uiso 1 1 calc R U . . . H21B H 0.596374 0.458498 0.744855 0.084 Uiso 1 1 calc R U . . . O1S O 0.491(2) 0.519(5) 0.5384(11) 0.189(9) Uiso 0.225(4) 1 d D U P A -1 O2S O 0.513(2) 1.176(5) 0.4708(11) 0.189(9) Uiso 0.225(4) 1 d D U P A -1 C1S C 0.480(3) 0.224(5) 0.5176(17) 0.189(9) Uiso 0.225(4) 1 d D U P A -1 H1SA H 0.509004 0.094337 0.544841 0.284 Uiso 0.225(4) 1 calc R U P A -1 H1SB H 0.504410 0.207352 0.487694 0.284 Uiso 0.225(4) 1 calc DR U P A -1 H1SC H 0.418492 0.178339 0.506884 0.284 Uiso 0.225(4) 1 calc R U P A -1 C2S C 0.494(2) 0.703(5) 0.4964(13) 0.189(9) Uiso 0.225(4) 1 d D U P A -1 H2SA H 0.440167 0.689421 0.468772 0.227 Uiso 0.225(4) 1 calc R U P A -1 H2SB H 0.542106 0.647966 0.481298 0.227 Uiso 0.225(4) 1 calc R U P A -1 C3S C 0.508(3) 1.002(5) 0.5158(12) 0.189(9) Uiso 0.225(4) 1 d D U P A -1 H3SA H 0.458790 1.062235 0.529393 0.227 Uiso 0.225(4) 1 calc R U P A -1 H3SB H 0.560996 1.017072 0.543962 0.227 Uiso 0.225(4) 1 calc R U P A -1 C4S C 0.525(3) 1.464(5) 0.4886(17) 0.189(9) Uiso 0.225(4) 1 d D U P A -1 H4SA H 0.544347 1.576146 0.462804 0.284 Uiso 0.225(4) 1 calc R U P A -1 H4SB H 0.569037 1.472060 0.521819 0.284 Uiso 0.225(4) 1 calc R U P A -1 H4SC H 0.471155 1.538399 0.493064 0.284 Uiso 0.225(4) 1 calc R U P A -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.075(2) 0.0449(19) 0.076(2) 0.0007(15) 0.0075(16) -0.0060(14) N1 0.057(2) 0.049(2) 0.079(3) -0.003(2) 0.0130(19) -0.0053(19) N2 0.053(2) 0.049(2) 0.064(2) -0.0032(19) 0.0078(17) -0.0018(19) N3 0.062(2) 0.101(3) 0.054(2) 0.007(2) 0.0131(19) -0.006(2) C1 0.058(3) 0.045(2) 0.044(2) -0.0027(19) 0.0132(19) -0.009(2) C2 0.055(3) 0.077(3) 0.059(3) -0.003(2) 0.017(2) -0.002(2) C3 0.050(2) 0.058(3) 0.055(3) 0.002(2) 0.014(2) -0.005(2) C4 0.060(3) 0.107(4) 0.061(3) 0.011(3) 0.023(2) 0.020(3) C5 0.056(3) 0.111(4) 0.058(3) 0.020(3) 0.016(2) 0.022(3) C6 0.054(3) 0.073(3) 0.053(3) 0.005(2) 0.009(2) -0.001(2) C7 0.070(3) 0.094(4) 0.058(3) -0.018(3) 0.013(2) 0.017(3) C8 0.062(3) 0.089(4) 0.066(3) -0.009(3) 0.005(2) 0.017(3) C9 0.053(3) 0.066(3) 0.064(3) -0.004(2) 0.007(2) 0.005(2) C10 0.086(4) 0.081(4) 0.118(5) 0.013(3) 0.001(4) -0.021(3) C11 0.085(5) 0.119(6) 0.163(7) -0.022(5) 0.009(5) -0.036(4) C12 0.059(4) 0.158(7) 0.129(6) -0.071(6) -0.002(4) 0.003(4) C13 0.074(4) 0.180(8) 0.083(4) -0.014(4) -0.002(3) 0.039(5) C14 0.066(3) 0.130(5) 0.071(3) 0.018(3) 0.010(3) 0.014(3) C15 0.051(2) 0.069(3) 0.052(3) -0.003(2) 0.006(2) -0.001(2) C16 0.054(3) 0.093(4) 0.069(3) -0.021(3) 0.009(2) -0.020(3) C17 0.056(3) 0.092(4) 0.055(3) -0.019(3) 0.010(2) -0.010(3) C18 0.050(2) 0.068(3) 0.056(3) 0.000(2) 0.008(2) -0.001(2) C19 0.097(4) 0.084(4) 0.068(3) -0.017(3) 0.026(3) -0.040(3) C20 0.114(4) 0.082(4) 0.068(3) -0.027(3) 0.039(3) -0.029(3) C21 0.064(3) 0.080(3) 0.063(3) 0.006(2) 0.008(2) -0.002(2) 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 _geom_angle_publ_flag C1 N1 H1 120(3) . . ? C1 N1 C21 124.0(4) . 3_666 ? C21 N1 H1 115(3) 3_666 . ? C1 N2 H2 119(3) . . ? C1 N2 C2 122.2(4) . . ? C2 N2 H2 119(3) . . ? C9 N3 C6 120.1(4) . . ? C9 N3 C15 120.2(4) . . ? C15 N3 C6 119.6(3) . . ? O1 C1 N1 122.5(4) . . ? O1 C1 N2 122.9(4) . . ? N2 C1 N1 114.6(4) . . ? N2 C2 H2A 108.7 . . ? N2 C2 H2B 108.7 . . ? N2 C2 C3 114.2(3) . . ? H2A C2 H2B 107.6 . . ? C3 C2 H2A 108.7 . . ? C3 C2 H2B 108.7 . . ? C4 C3 C2 122.7(4) . . ? C4 C3 C8 116.1(4) . . ? C8 C3 C2 121.2(4) . . ? C3 C4 H4 118.8 . . ? C5 C4 C3 122.4(4) . . ? C5 C4 H4 118.8 . . ? C4 C5 H5 119.7 . . ? C6 C5 C4 120.7(4) . . ? C6 C5 H5 119.7 . . ? C5 C6 N3 122.0(4) . . ? C5 C6 C7 118.2(4) . . ? C7 C6 N3 119.8(4) . . ? C6 C7 H7 119.6 . . ? C6 C7 C8 120.8(4) . . ? C8 C7 H7 119.6 . . ? C3 C8 H8 119.1 . . ? C7 C8 C3 121.7(4) . . ? C7 C8 H8 119.1 . . ? C10 C9 N3 120.5(4) . . ? C10 C9 C14 118.7(5) . . ? C14 C9 N3 120.8(4) . . ? C9 C10 H10 119.8 . . ? C9 C10 C11 120.5(6) . . ? C11 C10 H10 119.8 . . ? C10 C11 H11 119.6 . . ? C12 C11 C10 120.8(7) . . ? C12 C11 H11 119.6 . . ? C11 C12 H12 120.6 . . ? C13 C12 C11 118.9(6) . . ? C13 C12 H12 120.6 . . ? C12 C13 H13 119.3 . . ? C12 C13 C14 121.4(7) . . ? C14 C13 H13 119.3 . . ? C9 C14 C13 119.7(6) . . ? C9 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 N3 122.0(4) . . ? C20 C15 N3 120.7(4) . . ? C20 C15 C16 117.3(4) . . ? C15 C16 H16 119.5 . . ? C15 C16 C17 121.0(4) . . ? C17 C16 H16 119.5 . . ? C16 C17 H17 119.0 . . ? C18 C17 C16 122.1(4) . . ? C18 C17 H17 119.0 . . ? C17 C18 C19 116.7(4) . . ? C17 C18 C21 122.0(4) . . ? C19 C18 C21 121.3(4) . . ? C18 C19 H19 119.1 . . ? C18 C19 C20 121.9(4) . . ? C20 C19 H19 119.1 . . ? C15 C20 C19 121.1(4) . . ? C15 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? N1 C21 C18 112.9(4) 3_666 . ? N1 C21 H21A 109.0 3_666 . ? N1 C21 H21B 109.0 3_666 . ? C18 C21 H21A 109.0 . . ? C18 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C2S O1S C1S 108.5(16) . . ? C4S O2S C3S 107.8(16) . . ? O1S C1S H1SA 109.5 . . ? O1S C1S H1SB 109.5 . . ? O1S C1S H1SC 109.5 . . ? H1SA C1S H1SB 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? O1S C2S H2SA 109.6 . . ? O1S C2S H2SB 109.6 . . ? O1S C2S C3S 110.2(17) . . ? H2SA C2S H2SB 108.1 . . ? C3S C2S H2SA 109.6 . . ? C3S C2S H2SB 109.6 . . ? O2S C3S C2S 106.8(16) . . ? O2S C3S H3SA 110.4 . . ? O2S C3S H3SB 110.4 . . ? C2S C3S H3SA 110.4 . . ? C2S C3S H3SB 110.4 . . ? H3SA C3S H3SB 108.6 . . ? O2S C4S H4SA 109.5 . . ? O2S C4S H4SB 109.5 . . ? O2S C4S H4SC 109.5 . . ? H4SA C4S H4SB 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? 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 O1 C1 1.233(5) . ? N1 H1 0.92(5) . ? N1 C1 1.350(5) . ? N1 C21 1.450(6) 3_666 ? N2 H2 0.87(5) . ? N2 C1 1.344(5) . ? N2 C2 1.452(5) . ? N3 C6 1.423(5) . ? N3 C9 1.416(5) . ? N3 C15 1.416(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C3 1.502(6) . ? C3 C4 1.377(6) . ? C3 C8 1.383(6) . ? C4 H4 0.9300 . ? C4 C5 1.374(6) . ? C5 H5 0.9300 . ? C5 C6 1.363(6) . ? C6 C7 1.375(6) . ? C7 H7 0.9300 . ? C7 C8 1.377(6) . ? C8 H8 0.9300 . ? C9 C10 1.365(7) . ? C9 C14 1.373(6) . ? C10 H10 0.9300 . ? C10 C11 1.369(8) . ? C11 H11 0.9300 . ? C11 C12 1.357(10) . ? C12 H12 0.9300 . ? C12 C13 1.347(10) . ? C13 H13 0.9300 . ? C13 C14 1.374(8) . ? C14 H14 0.9300 . ? C15 C16 1.378(6) . ? C15 C20 1.371(6) . ? C16 H16 0.9300 . ? C16 C17 1.382(6) . ? C17 H17 0.9300 . ? C17 C18 1.367(6) . ? C18 C19 1.372(6) . ? C18 C21 1.492(6) . ? C19 H19 0.9300 . ? C19 C20 1.384(6) . ? C20 H20 0.9300 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? O1S C1S 1.489(15) . ? O1S C2S 1.408(15) . ? O2S C3S 1.453(15) . ? O2S C4S 1.434(15) . ? C1S H1SA 0.9600 . ? C1S H1SB 0.9600 . ? C1S H1SC 0.9600 . ? C2S H2SA 0.9700 . ? C2S H2SB 0.9700 . ? C2S C3S 1.491(15) . ? C3S H3SA 0.9700 . ? C3S H3SB 0.9700 . ? C4S H4SA 0.9600 . ? C4S H4SB 0.9600 . ? C4S H4SC 0.9600 . ? 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 _geom_torsion_publ_flag N2 C2 C3 C4 125.0(5) . . . . ? N2 C2 C3 C8 -54.4(6) . . . . ? N3 C6 C7 C8 -177.6(4) . . . . ? N3 C9 C10 C11 179.0(5) . . . . ? N3 C9 C14 C13 -178.4(5) . . . . ? N3 C15 C16 C17 -179.1(4) . . . . ? N3 C15 C20 C19 -179.4(5) . . . . ? C1 N2 C2 C3 98.3(5) . . . . ? C2 N2 C1 O1 0.6(6) . . . . ? C2 N2 C1 N1 -179.3(3) . . . . ? C2 C3 C4 C5 -178.8(5) . . . . ? C2 C3 C8 C7 179.4(4) . . . . ? C3 C4 C5 C6 -0.4(8) . . . . ? C4 C3 C8 C7 -0.1(7) . . . . ? C4 C5 C6 N3 178.0(5) . . . . ? C4 C5 C6 C7 -0.4(8) . . . . ? C5 C6 C7 C8 1.0(8) . . . . ? C6 N3 C9 C10 38.1(7) . . . . ? C6 N3 C9 C14 -142.5(5) . . . . ? C6 N3 C15 C16 -142.9(5) . . . . ? C6 N3 C15 C20 36.5(7) . . . . ? C6 C7 C8 C3 -0.7(8) . . . . ? C8 C3 C4 C5 0.6(7) . . . . ? C9 N3 C6 C5 40.9(7) . . . . ? C9 N3 C6 C7 -140.7(5) . . . . ? C9 N3 C15 C16 39.9(6) . . . . ? C9 N3 C15 C20 -140.7(5) . . . . ? C9 C10 C11 C12 -0.2(11) . . . . ? C10 C9 C14 C13 1.1(8) . . . . ? C10 C11 C12 C13 0.2(11) . . . . ? C11 C12 C13 C14 0.4(11) . . . . ? C12 C13 C14 C9 -1.1(10) . . . . ? C14 C9 C10 C11 -0.4(9) . . . . ? C15 N3 C6 C5 -136.3(5) . . . . ? C15 N3 C6 C7 42.1(6) . . . . ? C15 N3 C9 C10 -144.8(5) . . . . ? C15 N3 C9 C14 34.6(7) . . . . ? C15 C16 C17 C18 -2.2(8) . . . . ? C16 C15 C20 C19 0.0(8) . . . . ? C16 C17 C18 C19 1.4(7) . . . . ? C16 C17 C18 C21 -179.6(4) . . . . ? C17 C18 C19 C20 0.1(8) . . . . ? C17 C18 C21 N1 104.3(5) . . . 3_666 ? C18 C19 C20 C15 -0.8(9) . . . . ? C19 C18 C21 N1 -76.7(6) . . . 3_666 ? C20 C15 C16 C17 1.5(7) . . . . ? C21 N1 C1 O1 6.1(6) 3_666 . . . ? C21 N1 C1 N2 -174.0(4) 3_666 . . . ? C21 C18 C19 C20 -178.9(5) . . . . ? O1S C2S C3S O2S 178.0(14) . . . . ? C1S O1S C2S C3S -178.9(14) . . . . ? C4S O2S C3S C2S 179.7(17) . . . . ?