#------------------------------------------------------------------------------ #$Date: 2024-12-06 19:30:00 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296460 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/94/7249420.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_7249420 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' _chemical_formula_sum 'C42 H38 N6 O2' _chemical_formula_weight 658.78 _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 iterative _atom_sites_solution_secondary difmap _audit_creation_date 2023-06-20 _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 104.992(5) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 15.845(3) _cell_length_b 4.6481(9) _cell_length_c 26.022(5) _cell_measurement_reflns_used 2404 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 21.278 _cell_measurement_theta_min 2.348 _cell_volume 1851.3(6) _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 (Dolomanov et al., 2009)' _computing_publication_material 'OLEX2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2015)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector PHOTON-II _diffrn_detector_area_resol_mean 7.39 _diffrn_detector_type 'area detector' _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _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 0.0975 _diffrn_reflns_av_unetI/netI 0.0766 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 9991 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 21.327 _diffrn_reflns_theta_max 21.327 _diffrn_reflns_theta_min 2.661 _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 0.074 _exptl_absorpt_correction_T_max 0.6181 _exptl_absorpt_correction_T_min 0.4358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1348 before and 0.0704 after correction. The Ratio of minimum to maximum transmission is 0.7051. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.182 _exptl_crystal_description needle _exptl_crystal_F_000 696 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.910 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.067 _refine_ls_extinction_coef 0.0073(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2019/2 (Sheldrick 2019)' _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 234 _refine_ls_number_reflns 2069 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.222 _refine_ls_R_factor_all 0.1440 _refine_ls_R_factor_gt 0.1165 _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^)+(0.0412P)^2^+9.6101P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2137 _refine_ls_wR_factor_ref 0.2254 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1648 _reflns_number_total 2069 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00839a2.cif _cod_data_source_block tpa_hdme_acti _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_database_code 7249420 _shelx_shelxl_version_number 2019/2 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Restrained distances N1-H1 \\sim N2-H2 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uiso(H1) = Uiso(H2) 4.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C21(H21A,H21B) 4.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) ; _shelx_res_file ; TITL tpa_hdme_acti in P2(1)/c tpa_hdme_acti.res created by SHELXL-2019/2 at 14:59:08 on 20-Jun-2023 REM RIGU O1 C1 N1 N2 C2 C3 C4 C8 C5 C7 C6 N3 C9 C15 C10 C14 C16 C20 C11 C13 REM C17 = REM C19 C12 C18 C21 CELL 0.71073 15.8455 4.6481 26.0218 90 104.9921 90 ZERR 2 0.003 0.0009 0.0048 0 0.0051 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 84 76 12 4 EQIV $1 +X,1+Y,+Z SADI N1 H1 N2 H2 EADP H1 H2 L.S. 7 PLAN 33 TEMP -173(2) CONF HTAB N1 O1_$1 HTAB N2 O1_$1 fmap 2 53 MORE -1 ACTA BOND $H REM REM REM WGHT 0.041200 9.610101 EXTI 0.007302 FVAR 0.19845 O1 4 0.583870 0.068281 0.332836 11.00000 0.03286 0.01556 = 0.03530 -0.00012 -0.00452 0.00015 N1 3 0.657248 0.494392 0.346794 11.00000 0.02733 0.01810 = 0.02658 0.00190 -0.00053 0.00027 N2 3 0.509238 0.487581 0.314934 11.00000 0.02560 0.02112 = 0.03524 -0.00073 0.00224 0.00218 N3 3 0.162984 0.652072 0.401192 11.00000 0.02934 0.04301 = 0.02523 -0.00608 0.00151 0.00140 C1 1 0.583559 0.332338 0.331764 11.00000 0.02414 0.01901 = 0.01039 0.00186 -0.00389 0.00897 C2 1 0.424146 0.358472 0.292056 11.00000 0.02628 0.03702 = 0.04287 0.00085 0.00114 0.00328 AFIX 23 H2A 2 0.430593 0.146550 0.292766 11.00000 -1.20000 H2B 2 0.403562 0.418260 0.254364 11.00000 -1.20000 AFIX 0 C3 1 0.355482 0.439852 0.320710 11.00000 0.01970 0.02869 = 0.03388 0.00068 0.00073 -0.00518 C4 1 0.292486 0.643370 0.301148 11.00000 0.02108 0.04432 = 0.02771 0.00863 -0.00452 0.00889 AFIX 43 H4 2 0.291851 0.735903 0.268498 11.00000 -1.20000 AFIX 0 C5 1 0.230323 0.718032 0.327097 11.00000 0.02693 0.05350 = 0.02661 0.01026 0.00593 0.00714 AFIX 43 H5 2 0.188248 0.861410 0.312443 11.00000 -1.20000 AFIX 0 C6 1 0.228740 0.585697 0.374340 11.00000 0.02644 0.02248 = 0.02039 -0.00475 -0.01257 0.00141 C7 1 0.291961 0.382508 0.395200 11.00000 0.06003 0.03425 = 0.03951 0.01317 0.01705 0.00913 AFIX 43 H7 2 0.291892 0.289335 0.427683 11.00000 -1.20000 AFIX 0 C8 1 0.355984 0.312316 0.369140 11.00000 0.05127 0.03248 = 0.04584 0.01444 0.00680 0.02119 AFIX 43 H8 2 0.400118 0.176701 0.384585 11.00000 -1.20000 AFIX 0 C9 1 0.076106 0.699488 0.371510 11.00000 0.01665 0.03141 = 0.02399 0.00255 -0.00646 -0.00565 C10 1 0.040520 0.552654 0.324993 11.00000 0.02754 0.07044 = 0.03025 -0.01229 -0.00329 -0.01065 AFIX 43 H10 2 0.074166 0.412285 0.312616 11.00000 -1.20000 AFIX 0 C11 1 -0.044136 0.609591 0.296337 11.00000 0.02706 0.09519 = 0.04453 0.00036 0.00114 -0.01974 AFIX 43 H11 2 -0.066945 0.508672 0.263971 11.00000 -1.20000 AFIX 0 C12 1 -0.096430 0.804145 0.312422 11.00000 0.02696 0.08479 = 0.05391 0.04806 -0.00546 -0.00204 AFIX 43 H12 2 -0.154537 0.841263 0.292283 11.00000 -1.20000 AFIX 0 C13 1 -0.060227 0.942331 0.359212 11.00000 0.04754 0.06612 = 0.08503 0.00975 -0.00202 0.02956 AFIX 43 H13 2 -0.095006 1.077084 0.372036 11.00000 -1.20000 AFIX 0 C14 1 0.024336 0.895947 0.388777 11.00000 0.06138 0.03746 = 0.05115 -0.00195 -0.00719 0.02515 AFIX 43 H14 2 0.046841 0.999020 0.420934 11.00000 -1.20000 AFIX 0 C15 1 0.185787 0.649754 0.458369 11.00000 0.02944 0.02088 = 0.03673 -0.00654 0.00400 -0.00333 C16 1 0.130772 0.533297 0.486513 11.00000 0.02475 0.04644 = 0.03065 -0.01864 0.00677 -0.00420 AFIX 43 H16 2 0.076455 0.453097 0.467621 11.00000 -1.20000 AFIX 0 C17 1 0.153054 0.531366 0.541009 11.00000 0.02044 0.05374 = 0.02042 -0.01820 0.00268 -0.01110 AFIX 43 H17 2 0.113430 0.451879 0.559016 11.00000 -1.20000 AFIX 0 C18 1 0.232138 0.642687 0.570653 11.00000 0.02350 0.01337 = 0.02715 -0.00005 0.00459 0.00039 C19 1 0.287078 0.761708 0.542015 11.00000 0.02595 0.03856 = 0.02834 0.00389 -0.00139 -0.00035 AFIX 43 H19 2 0.341470 0.841812 0.560805 11.00000 -1.20000 AFIX 0 C20 1 0.264325 0.765640 0.487376 11.00000 0.03803 0.03233 = 0.02836 0.00985 0.00032 -0.01017 AFIX 43 H20 2 0.303045 0.849158 0.469154 11.00000 -1.20000 AFIX 0 C21 1 0.257993 0.636595 0.630580 11.00000 0.02579 0.03361 = 0.02696 -0.00245 -0.00158 0.00554 AFIX 23 H21A 2 0.258874 0.836186 0.643990 11.00000 -1.20000 H21B 2 0.213117 0.529013 0.643041 11.00000 -1.20000 AFIX 0 H2 2 0.514983 0.681407 0.315007 11.00000 0.03917 H1 2 0.656178 0.688318 0.343586 11.00000 0.03917 HKLF 4 REM tpa_hdme_acti in P2(1)/c REM wR2 = 0.2254, GooF = S = 1.222, Restrained GooF = 1.222 for all data REM R1 = 0.1165 for 1648 Fo > 4sig(Fo) and 0.1440 for all 2069 data REM 234 parameters refined using 1 restraints END WGHT 0.0413 9.6037 REM Highest difference peak 0.910, deepest hole -0.229, 1-sigma level 0.067 Q1 1 -0.1874 0.8201 0.2790 11.00000 0.05 0.91 Q2 1 0.5081 0.0369 0.3424 11.00000 0.05 0.22 Q3 1 0.2942 0.8872 0.6404 11.00000 0.05 0.21 Q4 1 0.4795 0.9044 0.5034 11.00000 0.05 0.20 Q5 1 0.6116 0.7459 0.3562 11.00000 0.05 0.20 Q6 1 0.4207 0.1503 0.3258 11.00000 0.05 0.19 Q7 1 0.2223 1.0004 0.6540 11.00000 0.05 0.19 Q8 1 0.2594 0.9690 0.3545 11.00000 0.05 0.19 Q9 1 0.2384 1.0594 0.4819 11.00000 0.05 0.19 Q10 1 0.4640 0.5296 0.5171 11.00000 0.05 0.19 Q11 1 0.2017 0.9550 0.5358 11.00000 0.05 0.19 Q12 1 0.1761 1.1630 0.3588 11.00000 0.05 0.19 Q13 1 0.2376 0.8890 0.3585 11.00000 0.05 0.18 Q14 1 0.4056 0.6957 0.4794 11.00000 0.05 0.18 Q15 1 0.5628 0.1511 0.3820 11.00000 0.05 0.18 Q16 1 0.2160 0.9016 0.5385 11.00000 0.05 0.18 Q17 1 0.4366 0.0969 0.3996 11.00000 0.05 0.18 Q18 1 0.1055 0.8833 0.3219 11.00000 0.05 0.18 Q19 1 0.4954 0.3368 0.4946 11.00000 0.05 0.17 Q20 1 0.1219 1.1361 0.3969 11.00000 0.05 0.17 Q21 1 0.6338 0.0412 0.3010 11.00000 0.05 0.17 Q22 1 0.0794 0.8223 0.4783 11.00000 0.05 0.17 Q23 1 0.7003 0.7846 0.3820 11.00000 0.05 0.17 Q24 1 -0.0399 1.2216 0.3744 11.00000 0.05 0.17 Q25 1 0.5140 0.6964 0.3556 11.00000 0.05 0.17 Q26 1 0.2988 0.3414 0.5013 11.00000 0.05 0.17 Q27 1 -0.1418 1.2751 0.3422 11.00000 0.05 0.17 Q28 1 0.6212 0.0053 0.3666 11.00000 0.05 0.17 Q29 1 -0.0411 1.1538 0.3639 11.00000 0.05 0.17 Q30 1 0.2377 0.3998 0.3190 11.00000 0.05 0.17 Q31 1 0.3026 0.8631 0.6730 11.00000 0.05 0.17 Q32 1 0.5003 0.1216 0.2774 11.00000 0.05 0.17 Q33 1 0.4758 0.5931 0.4613 11.00000 0.05 0.17 ; _shelx_res_checksum 2650 _shelx_hkl_file ; 2 0 0 125.71 6.51 2 0 0 144.64 6.33 -2 0 0 147.01 6.54 3 0 0 48.07 2.47 -3 0 0 46.77 2.83 -3 0 0 46.06 2.43 3 0 0 52.86 2.97 4 0 0 16.25 1.98 -4 0 0 12.51 1.17 4 0 0 14.47 1.23 -4 0 0 11.49 1.80 5 0 0 3.18 1.08 -5 0 0 3.84 1.83 5 0 0 2.35 1.84 -5 0 0 2.67 1.04 -6 0 0 59.17 3.94 6 0 0 67.28 3.48 -6 0 0 60.03 3.41 6 0 0 73.17 4.29 7 0 0 0.11 0.96 -7 0 0 0.46 1.58 7 0 0 0.07 1.79 -7 0 0 2.42 1.16 8 0 0 5.61 2.20 -8 0 0 8.20 1.30 8 0 0 5.55 1.33 -8 0 0 8.26 2.26 9 0 0 44.12 2.78 9 0 0 45.11 3.79 -9 0 0 37.93 3.41 -9 0 0 46.05 2.82 10 0 0 21.68 2.89 -10 0 0 19.15 1.91 -10 0 0 22.39 2.73 10 0 0 23.92 1.94 11 0 0 21.77 3.17 11 0 0 21.47 1.97 -11 0 0 25.79 2.86 -11 0 0 21.17 2.12 -12 0 0 24.03 2.35 -12 0 0 18.84 3.65 12 0 0 26.28 2.32 12 0 0 26.22 3.59 -13 0 0 20.41 3.20 13 0 0 22.29 3.59 13 0 0 20.32 2.24 -13 0 0 21.84 2.34 -14 0 0 31.98 4.00 -14 0 0 40.11 3.14 -15 0 0 24.05 3.54 -15 0 0 22.73 2.66 0 -1 0 1.20 1.25 0 1 0 0.58 1.26 -1 -1 0 441.68 20.66 1 -1 0 428.99 20.44 1 -1 0 486.83 20.52 -1 1 0 452.25 20.44 -1 1 0 473.62 20.53 1 1 0 440.06 20.64 2 -1 0 43.22 2.52 -2 -1 0 43.40 2.32 -2 -1 0 41.81 2.86 2 -1 0 42.79 2.41 -2 1 0 43.60 2.53 2 1 0 43.72 2.86 -2 1 0 38.42 2.32 2 1 0 42.17 2.37 3 -1 0 309.33 13.65 -3 -1 0 294.58 14.06 3 -1 0 292.56 13.48 -3 -1 0 294.79 13.50 -3 1 0 300.87 13.68 -3 1 0 289.19 13.41 3 1 0 302.18 13.54 3 1 0 289.75 14.03 4 -1 0 34.96 2.26 -4 -1 0 32.74 2.01 -4 -1 0 32.07 2.80 4 -1 0 35.00 2.27 4 -1 0 32.20 2.02 -4 1 0 31.90 2.24 -4 1 0 34.30 1.96 4 1 0 33.20 2.79 4 1 0 34.51 2.08 -5 -1 0 109.57 5.29 5 -1 0 105.11 5.21 -5 -1 0 113.21 6.09 5 -1 0 97.76 5.45 5 -1 0 107.90 5.39 -5 1 0 110.16 5.48 5 1 0 107.45 5.30 5 1 0 105.03 6.05 6 -1 0 1.82 1.27 -6 -1 0 2.72 1.87 6 -1 0 3.84 1.15 6 -1 0 0.69 1.66 -6 -1 0 0.80 0.89 -6 1 0 2.60 1.27 -6 1 0 2.59 1.45 6 1 0 2.25 0.93 6 1 0 2.58 2.21 -7 -1 0 9.20 2.49 7 -1 0 6.76 1.17 7 -1 0 7.28 1.57 7 -1 0 7.89 2.07 -7 -1 0 6.69 1.08 7 1 0 9.16 2.63 7 1 0 6.53 1.30 -7 1 0 8.55 1.78 -7 1 0 7.63 1.66 8 -1 0 42.39 2.68 8 -1 0 45.48 3.40 -8 -1 0 53.45 3.93 8 -1 0 46.89 2.92 -8 -1 0 44.91 2.72 -8 1 0 36.58 2.92 8 1 0 46.14 3.91 -8 1 0 43.47 2.93 8 1 0 46.15 2.84 -9 -1 0 0.25 2.00 9 -1 0 0.03 1.86 9 -1 0 0.80 1.24 -9 -1 0 1.07 1.11 9 -1 0 0.53 0.94 9 1 0 0.90 1.05 -9 1 0 1.08 1.33 -9 1 0 0.08 1.40 9 1 0 2.53 2.20 -10 -1 0 1.21 1.12 10 -1 0 0.66 0.99 10 -1 0 -1.31 1.82 -10 -1 0 -0.06 2.00 10 1 0 1.18 1.12 -10 1 0 5.48 1.86 -10 1 0 -0.14 1.20 10 1 0 -2.84 1.96 11 -1 0 1.76 2.27 11 -1 0 2.08 1.21 11 -1 0 3.44 1.69 -11 -1 0 1.54 1.33 11 1 0 2.40 1.40 -11 1 0 1.88 1.50 -11 1 0 2.26 1.77 11 1 0 -4.04 2.40 12 -1 0 6.31 1.82 12 -1 0 9.50 1.76 -12 -1 0 5.60 1.70 -12 -1 0 9.12 2.99 12 1 0 5.82 1.72 -12 1 0 3.71 2.09 -12 1 0 9.56 2.11 12 1 0 7.21 3.48 -13 -1 0 5.81 2.83 -13 -1 0 2.72 1.62 13 -1 0 -1.63 2.30 13 -1 0 2.25 1.72 13 -1 0 5.17 1.58 -13 1 0 5.01 1.83 -13 1 0 4.37 2.28 13 1 0 2.63 1.54 14 -1 0 4.71 3.23 14 -1 0 1.34 1.80 -14 -1 0 4.56 2.02 -14 -1 0 0.88 2.59 -14 1 0 5.50 1.99 14 1 0 2.91 1.61 -14 1 0 6.73 2.53 15 -1 0 3.26 1.84 15 -1 0 9.01 2.03 -15 -1 0 4.41 2.06 -15 -1 0 2.36 3.20 -15 1 0 2.81 2.25 15 1 0 1.29 1.71 -15 1 0 4.47 2.11 0 -2 0 14.84 2.02 0 -2 0 18.11 1.84 0 2 0 15.35 1.91 1 -2 0 2.17 1.63 -1 -2 0 0.78 1.69 1 -2 0 0.14 1.26 -1 2 0 2.09 1.43 1 2 0 0.27 1.68 2 -2 0 120.47 6.40 2 -2 0 126.23 6.45 -2 -2 0 132.26 6.33 -2 -2 0 112.22 6.75 -2 2 0 125.74 6.52 -2 2 0 131.80 6.47 2 2 0 126.01 6.78 -3 -2 0 1.16 1.05 -3 -2 0 4.52 2.08 3 -2 0 1.76 1.37 3 -2 0 2.85 1.36 -3 2 0 0.95 1.34 3 2 0 -0.43 1.82 -3 2 0 2.05 1.29 4 -2 0 21.99 1.99 -4 -2 0 17.86 2.56 4 -2 0 17.00 1.76 -4 -2 0 19.41 1.70 -4 2 0 17.48 1.58 4 2 0 19.28 2.50 -4 2 0 18.18 2.01 -5 -2 0 4.17 1.22 5 -2 0 2.61 1.25 5 -2 0 3.50 1.51 -5 -2 0 5.12 2.29 5 2 0 4.59 1.42 5 2 0 2.70 2.21 -5 2 0 4.43 1.18 -5 2 0 4.39 1.51 6 -2 0 62.14 3.78 -6 -2 0 63.91 4.62 -6 -2 0 61.46 3.57 6 -2 0 60.74 3.66 6 -2 0 62.43 3.70 -6 2 0 59.15 3.87 -6 2 0 62.63 3.37 6 2 0 62.61 3.68 6 2 0 61.33 4.54 7 -2 0 9.86 1.67 -7 -2 0 11.49 2.99 7 -2 0 9.87 1.39 -7 -2 0 12.42 1.45 7 -2 0 8.57 1.93 -7 2 0 12.50 2.20 7 2 0 14.29 3.20 7 2 0 9.97 1.43 -8 -2 0 5.05 2.38 -8 -2 0 3.41 1.30 8 -2 0 1.10 1.96 8 -2 0 3.87 1.52 8 -2 0 3.17 1.37 8 2 0 4.41 2.79 8 2 0 5.00 1.43 -8 2 0 5.06 1.76 -9 -2 0 1.49 2.29 9 -2 0 -0.11 1.87 -9 -2 0 -0.21 1.00 9 -2 0 1.93 1.62 9 -2 0 0.10 1.13 -9 2 0 -0.64 1.25 9 2 0 1.03 1.28 9 2 0 3.05 2.46 10 -2 0 10.21 1.70 10 -2 0 11.76 2.71 -10 -2 0 14.82 3.63 -10 -2 0 10.15 1.91 10 -2 0 12.08 2.40 10 2 0 12.21 2.28 -10 2 0 12.89 2.60 11 -2 0 35.97 2.78 11 -2 0 32.64 3.47 -11 -2 0 33.14 2.65 -11 -2 0 29.88 4.15 11 2 0 35.67 2.84 -11 2 0 33.75 3.12 12 -2 0 1.19 1.86 -12 -2 0 2.43 1.48 12 -2 0 1.26 1.52 -12 -2 0 2.20 2.93 12 -2 0 0.59 2.50 -12 2 0 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-2 -20 2.74 2.81 3 2 -20 2.76 2.01 3 2 -20 -1.77 1.63 2 -2 -20 11.44 2.44 2 -2 -20 17.62 3.94 1 -2 -20 0.25 1.49 1 -2 -20 1.77 2.53 0 -2 -20 6.95 3.32 -1 -2 -20 0.81 1.63 -1 -2 -20 1.80 2.60 -2 -2 -20 2.36 1.66 -2 -2 -20 3.88 3.03 -2 2 -20 2.44 1.64 -3 -2 -20 5.12 3.68 -3 -2 -20 3.50 1.80 -3 2 -20 6.67 2.08 -4 -2 -20 2.48 1.67 -4 -2 -20 7.31 3.47 -4 2 -20 2.92 2.02 6 -3 -20 4.00 3.31 6 -3 -20 3.83 2.45 6 -3 -20 4.57 2.20 6 3 -20 7.34 2.75 6 3 -20 3.76 2.06 5 -3 -20 3.11 2.20 5 -3 -20 7.04 2.55 5 -3 -20 10.12 4.17 -5 -3 20 5.73 2.78 5 3 -20 4.54 2.13 5 3 -20 6.25 2.28 4 -3 -20 0.12 2.86 4 -3 -20 -0.78 1.85 4 -3 -20 -0.87 1.96 4 3 -20 -1.74 1.81 4 3 -20 1.63 1.84 3 -3 -20 -0.14 2.10 3 -3 -20 4.60 3.30 3 -3 -20 3.06 2.20 2 -3 -20 1.90 3.50 2 -3 -20 7.50 2.59 1 -3 -20 0.99 2.12 1 -3 -20 1.76 3.00 12 0 -21 -1.72 2.01 11 0 -21 2.30 2.24 10 0 -21 5.08 2.48 9 0 -21 -0.23 1.90 8 0 -21 2.29 2.24 7 0 -21 0.43 2.03 6 0 -21 -0.06 1.97 -6 0 21 2.61 1.65 6 0 -21 3.34 2.62 5 0 -21 2.49 2.04 -5 0 21 1.19 1.33 5 0 -21 1.44 1.56 4 0 -21 -1.05 1.34 -4 0 21 1.50 1.40 4 0 -21 6.57 2.19 3 0 -21 0.30 1.73 -3 0 21 -0.52 1.41 -2 0 21 2.33 1.48 2 0 -21 -0.36 1.59 2 0 -21 -0.25 1.52 -1 0 21 0.94 1.38 1 0 -21 -1.42 1.70 0 0 -21 2.27 2.25 0 0 -21 0.78 1.15 0 0 21 0.58 1.36 1 0 21 0.22 1.20 -1 0 -21 1.76 1.22 -1 0 -21 1.33 2.12 2 0 21 1.00 1.33 -2 0 -21 -0.41 2.10 -2 0 -21 2.85 1.34 -3 0 -21 2.10 2.39 3 0 21 0.39 1.41 -3 0 -21 0.85 1.45 -4 0 -21 1.64 1.50 4 0 21 5.48 1.93 -4 0 -21 0.02 2.24 5 0 21 -0.27 1.32 -5 0 -21 2.58 1.72 -5 0 -21 0.69 2.31 -6 0 -21 2.43 1.94 -6 0 -21 3.29 2.76 12 -1 -21 7.52 3.08 12 1 -21 15.65 3.25 11 -1 -21 1.29 2.38 11 1 -21 2.10 2.33 10 -1 -21 3.72 2.76 10 1 -21 4.09 2.36 9 -1 -21 13.05 3.20 9 1 -21 1.87 2.17 8 -1 -21 14.87 3.53 8 1 -21 13.27 2.31 7 -1 -21 7.39 2.72 7 1 -21 13.98 3.42 7 1 -21 7.73 2.30 6 -1 -21 77.54 5.94 6 1 -21 89.24 5.80 6 1 -21 76.57 5.17 5 -1 -21 2.15 1.31 5 -1 -21 2.09 1.46 5 -1 -21 -0.61 1.74 5 1 -21 3.10 1.82 5 1 -21 6.10 2.46 4 -1 -21 3.97 2.46 4 -1 -21 2.77 1.24 4 1 -21 1.67 1.85 4 1 -21 10.20 2.64 3 -1 -21 1.13 1.16 3 -1 -21 -1.04 2.04 -3 1 21 0.46 2.08 3 1 -21 3.36 2.09 3 1 -21 0.96 1.31 2 -1 -21 -0.31 2.02 2 -1 -21 1.30 1.15 -2 1 21 1.28 1.41 2 1 -21 0.49 1.91 2 1 -21 0.49 1.42 -1 -1 21 2.53 1.21 1 -1 -21 0.69 1.12 1 -1 -21 -1.13 2.27 1 1 -21 1.16 1.51 1 1 -21 -0.27 1.82 -1 1 21 2.34 1.73 0 -1 -21 1.81 1.19 0 -1 21 2.74 1.31 0 -1 -21 1.26 2.46 0 1 -21 3.45 1.82 0 1 -21 3.74 1.97 0 1 21 2.83 1.85 -1 -1 -21 5.43 1.62 -1 -1 -21 2.96 2.96 -1 1 -21 10.36 2.25 -1 1 -21 8.77 1.77 1 1 21 8.29 2.53 -2 -1 -21 4.36 3.10 -2 -1 -21 1.18 1.29 -2 1 -21 2.26 1.50 2 1 21 1.99 1.62 -3 -1 -21 14.07 3.88 -3 -1 -21 6.53 1.83 -3 1 -21 8.91 2.08 -4 -1 -21 15.12 2.52 -4 -1 -21 22.16 4.37 -4 1 -21 11.78 1.92 -5 -1 -21 3.61 1.84 -5 -1 -21 7.48 3.45 -5 1 -21 1.36 1.72 10 -2 -21 12.19 2.48 -10 -2 21 10.89 3.67 10 -2 -21 5.91 2.90 10 2 -21 8.49 2.68 9 -2 -21 4.46 2.10 9 -2 -21 5.67 2.79 -9 -2 21 7.08 3.24 9 2 -21 7.72 2.63 8 -2 -21 7.44 2.35 -8 -2 21 7.87 3.18 8 -2 -21 10.00 3.40 8 -2 -21 10.16 2.64 8 2 -21 11.57 2.75 7 -2 -21 3.39 2.22 7 -2 -21 7.83 2.21 7 -2 -21 8.72 3.37 7 2 -21 8.10 2.38 7 2 -21 9.14 3.03 6 -2 -21 1.66 1.89 6 -2 -21 2.49 2.05 6 -2 -21 -1.24 2.21 6 2 -21 7.38 2.66 6 2 -21 0.15 1.93 5 -2 -21 8.01 2.41 5 -2 -21 10.02 2.55 5 -2 -21 9.03 3.48 5 2 -21 10.75 2.50 5 2 -21 9.27 2.77 4 -2 -21 5.49 3.20 4 -2 -21 7.97 2.39 4 -2 -21 12.57 2.43 4 2 -21 14.42 3.00 4 2 -21 6.97 2.13 3 -2 -21 5.55 2.15 3 -2 -21 7.71 3.40 3 2 -21 12.00 2.06 3 2 -21 12.13 2.60 2 -2 -21 3.22 2.87 2 -2 -21 -1.83 1.46 1 -2 -21 1.44 2.84 1 -2 -21 4.05 1.81 0 -2 -21 2.07 3.08 0 -2 -21 1.47 1.58 -1 -2 -21 -0.85 1.42 -1 -2 -21 2.84 3.19 -2 -2 -21 2.42 1.69 -2 -2 -21 3.44 3.16 -2 2 -21 3.61 1.71 -3 -2 -21 1.94 3.32 -3 -2 -21 2.73 1.64 -3 2 -21 3.50 1.98 12 0 -22 -0.44 2.10 11 0 -22 9.19 2.91 10 0 -22 -1.30 2.10 9 0 -22 3.03 2.44 8 0 -22 43.46 4.04 7 0 -22 4.36 2.39 6 0 -22 65.67 6.67 6 0 -22 66.99 4.98 5 0 -22 1.78 1.73 -5 0 22 0.75 1.51 5 0 -22 3.14 2.27 4 0 -22 3.12 2.10 4 0 -22 7.97 2.51 -4 0 22 6.23 1.98 -3 0 22 6.98 1.96 3 0 -22 4.18 2.37 3 0 -22 5.13 2.29 2 0 -22 0.75 1.75 -2 0 22 1.29 1.42 2 0 -22 -0.03 1.73 1 0 -22 6.28 2.66 0 0 -22 7.45 1.64 0 0 -22 7.30 2.56 0 0 22 8.48 2.03 -1 0 -22 9.77 1.53 1 0 22 11.45 2.31 -1 0 -22 12.54 3.28 -2 0 -22 7.56 1.90 2 0 22 6.28 1.86 -2 0 -22 6.10 2.80 -3 0 -22 14.44 1.95 3 0 22 16.76 2.74 -3 0 -22 19.91 3.93 4 0 22 15.21 2.85 -4 0 -22 12.45 1.96 -5 0 -22 12.90 2.13 11 -1 -22 -0.83 2.49 11 1 -22 10.30 3.43 10 -1 -22 9.22 3.49 10 1 -22 15.66 2.78 9 -1 -22 10.81 3.42 9 1 -22 8.31 2.58 8 -1 -22 5.24 2.56 8 1 -22 7.75 2.64 7 -1 -22 23.81 3.37 7 1 -22 21.01 2.80 7 1 -22 26.22 3.50 6 -1 -22 3.24 2.33 6 1 -22 6.84 2.83 6 1 -22 2.37 1.93 5 -1 -22 5.00 2.59 5 1 -22 9.85 2.79 5 1 -22 2.09 2.07 4 -1 -22 3.93 2.46 4 -1 -22 3.97 1.63 4 1 -22 2.17 1.80 3 -1 -22 -0.33 2.04 3 -1 -22 -0.46 1.07 3 1 -22 -1.93 1.99 3 1 -22 0.60 1.49 2 -1 -22 -0.54 1.08 2 -1 -22 0.77 2.40 2 1 -22 3.27 2.14 2 1 -22 0.97 1.52 -1 -1 22 3.29 1.35 1 -1 -22 1.07 1.19 1 -1 -22 3.38 2.65 1 1 -22 1.05 1.77 1 1 -22 5.37 2.17 0 -1 -22 9.84 1.59 0 -1 22 12.60 1.62 0 -1 -22 15.24 3.75 0 1 -22 11.27 2.63 0 1 -22 9.69 2.52 -1 -1 -22 8.18 3.41 -1 -1 -22 8.77 1.80 -1 1 -22 7.51 2.36 -1 1 -22 7.14 1.81 -2 -1 -22 0.74 2.76 -2 -1 -22 2.88 1.51 -2 1 -22 2.20 1.63 -3 -1 -22 1.96 1.43 -3 -1 -22 1.16 2.97 -3 1 -22 1.54 1.67 -4 -1 -22 0.57 2.90 -4 -1 -22 1.81 1.67 -4 1 -22 7.70 2.07 -9 -2 22 5.11 3.03 9 -2 -22 2.82 2.59 9 -2 -22 1.80 1.85 9 2 -22 0.57 1.86 8 -2 -22 2.28 2.42 8 -2 -22 -0.22 1.82 8 -2 -22 5.13 2.32 8 2 -22 1.95 2.26 7 -2 -22 5.95 2.11 7 -2 -22 3.97 2.06 7 -2 -22 2.73 2.54 7 2 -22 1.26 2.58 7 2 -22 1.42 2.16 6 -2 -22 2.07 1.76 5 -2 -22 3.85 1.95 5 -2 -22 1.37 2.65 5 -2 -22 5.26 2.09 5 2 -22 5.03 2.38 4 -2 -22 3.37 1.96 4 -2 -22 1.33 1.83 4 -2 -22 3.82 3.02 4 2 -22 2.04 2.15 4 2 -22 5.04 2.05 3 -2 -22 10.68 2.56 3 -2 -22 13.53 3.98 3 2 -22 13.89 2.37 3 2 -22 6.03 2.51 2 -2 -22 15.81 2.81 2 -2 -22 3.24 2.85 1 -2 -22 -0.20 1.59 1 -2 -22 -1.08 2.70 0 -2 -22 2.01 1.63 0 -2 -22 2.25 3.15 -1 -2 -22 23.38 5.32 -2 -2 -22 7.52 2.29 -2 -2 -22 19.93 4.87 -2 2 -22 11.15 1.85 11 0 -23 2.54 2.37 10 0 -23 0.87 2.17 9 0 -23 17.03 3.01 8 0 -23 10.08 3.17 7 0 -23 4.95 2.89 6 0 -23 1.51 1.77 5 0 -23 4.05 2.13 5 0 -23 2.76 3.73 -4 0 23 3.44 1.76 4 0 -23 -0.41 1.85 4 0 -23 0.61 1.82 3 0 -23 -0.06 1.74 3 0 -23 2.10 2.34 2 0 -23 3.82 1.94 -2 0 23 1.63 1.53 2 0 -23 1.88 2.27 1 0 -23 2.13 2.36 -1 0 23 5.63 1.65 0 0 -23 5.38 1.61 0 0 23 2.25 1.65 0 0 -23 2.39 2.47 -1 0 -23 0.12 2.43 -1 0 -23 0.89 1.45 1 0 23 1.13 1.48 -2 0 -23 1.23 1.55 -2 0 -23 3.46 2.75 2 0 23 0.12 1.32 -3 0 -23 2.96 1.74 -3 0 -23 4.38 2.75 3 0 23 2.17 1.58 -4 0 -23 7.62 2.84 -4 0 -23 -1.04 1.59 4 0 23 -0.03 1.67 10 -1 -23 3.70 2.61 10 1 -23 5.90 2.60 9 -1 -23 8.44 2.81 9 1 -23 8.31 2.70 7 -1 -23 3.04 2.46 7 1 -23 3.36 2.00 5 -1 -23 17.45 3.00 5 1 -23 18.05 2.68 4 -1 -23 7.59 2.66 4 1 -23 0.78 1.55 4 1 -23 7.99 2.52 3 -1 -23 1.78 2.56 3 -1 -23 2.57 1.38 3 1 -23 3.36 1.87 3 1 -23 1.29 2.33 2 -1 -23 1.86 1.28 2 -1 -23 5.02 2.91 2 1 -23 2.52 2.10 2 1 -23 5.88 2.11 1 -1 -23 0.86 1.35 1 -1 -23 1.43 2.61 1 1 -23 3.49 2.05 1 1 -23 6.53 2.10 0 -1 -23 1.00 1.23 0 -1 23 1.60 1.22 0 -1 -23 3.63 2.91 0 1 -23 0.01 1.86 -1 -1 -23 6.13 1.67 -1 -1 -23 10.57 3.51 1 -1 23 7.68 1.73 -2 -1 -23 8.53 3.69 -2 -1 -23 3.66 1.71 -2 1 -23 6.63 1.89 -3 -1 -23 -1.22 2.96 -3 -1 -23 0.32 1.39 -3 1 -23 0.66 1.66 7 -2 -23 3.04 2.16 7 -2 -23 5.81 2.15 7 -2 -23 6.61 3.08 7 2 -23 5.88 2.29 6 -2 -23 5.56 2.78 6 -2 -23 4.82 2.09 6 2 -23 1.69 1.98 6 2 -23 9.95 2.98 5 -2 -23 13.66 2.29 5 -2 -23 15.36 4.11 5 -2 -23 16.34 2.43 5 2 -23 7.63 3.03 5 2 -23 9.01 2.62 4 -2 -23 0.15 2.94 4 -2 -23 1.48 1.91 4 -2 -23 0.90 1.83 4 2 -23 2.41 2.31 4 2 -23 3.58 2.15 3 -2 -23 2.52 1.96 3 -2 -23 8.53 3.55 3 2 -23 3.32 2.16 3 2 -23 2.50 1.80 2 -2 -23 3.16 2.23 2 -2 -23 8.68 3.50 1 -2 -23 2.88 3.29 1 -2 -23 2.46 1.72 0 -2 -23 3.68 3.48 0 -2 -23 1.36 1.66 10 0 -24 8.37 3.20 9 0 -24 19.58 3.96 8 0 -24 8.11 2.77 7 0 -24 5.71 2.64 6 0 -24 40.15 4.00 5 0 -24 31.79 3.67 4 0 -24 0.59 1.91 3 0 -24 2.11 2.43 3 0 -24 -1.62 1.78 2 0 -24 4.99 2.40 2 0 -24 5.03 2.43 -2 0 24 2.80 1.64 1 0 -24 16.71 3.66 -1 0 24 19.60 2.23 0 0 -24 15.62 3.63 0 0 24 19.20 2.32 0 0 -24 17.33 1.86 -1 0 -24 10.64 2.16 -1 0 -24 7.07 3.14 1 0 24 12.25 2.06 -2 0 -24 4.03 2.79 -2 0 -24 1.48 1.69 2 0 24 3.01 1.70 -3 0 -24 1.80 1.83 9 -1 -24 3.23 2.72 9 1 -24 7.21 2.68 8 -1 -24 2.39 2.21 8 1 -24 7.65 2.50 7 -1 -24 2.86 2.63 7 1 -24 5.26 2.31 5 -1 -24 9.83 3.10 5 1 -24 11.28 2.63 5 1 -24 14.76 3.57 4 -1 -24 1.09 2.45 4 1 -24 0.24 1.71 4 1 -24 2.27 2.71 3 -1 -24 7.27 3.27 3 -1 -24 7.86 1.73 3 1 -24 9.41 2.64 3 1 -24 7.66 2.97 2 -1 -24 2.77 2.80 2 -1 -24 2.69 1.45 2 1 -24 3.24 2.33 2 1 -24 0.83 1.76 1 -1 -24 21.04 4.41 1 -1 -24 15.03 1.83 1 1 -24 14.52 2.42 1 1 -24 19.55 2.68 0 -1 -24 1.46 1.31 0 -1 24 2.96 1.37 0 -1 -24 4.62 2.95 0 1 -24 -0.36 1.88 0 1 -24 6.03 2.33 -1 -1 -24 5.64 2.93 -1 1 -24 1.27 1.99 -1 1 -24 8.76 2.44 -2 -1 -24 2.72 1.55 -2 -1 -24 0.31 3.07 -2 1 -24 4.52 1.82 5 -2 -24 11.71 4.28 5 -2 -24 16.72 2.44 5 -2 -24 11.28 2.74 5 2 -24 12.30 2.90 5 2 -24 10.95 3.25 4 -2 -24 13.89 3.78 4 -2 -24 3.99 2.08 4 -2 -24 1.67 1.84 4 2 -24 5.15 2.46 4 2 -24 4.30 2.47 3 -2 -24 19.74 4.73 3 2 -24 13.23 2.29 9 0 -25 4.07 2.82 8 0 -25 16.82 2.97 7 0 -25 1.60 1.98 6 0 -25 2.91 2.24 5 0 -25 2.74 1.98 4 0 -25 -1.24 1.71 3 0 -25 -0.45 1.96 2 0 -25 0.61 2.52 2 0 -25 0.02 2.13 1 0 -25 2.81 2.44 1 0 -25 -0.61 2.11 -1 0 25 3.93 1.93 0 0 -25 2.69 2.49 -1 0 -25 3.71 1.87 -1 0 -25 10.96 3.27 1 0 25 2.84 1.88 8 -1 -25 2.43 2.24 8 1 -25 4.96 2.42 7 -1 -25 1.73 2.33 7 1 -25 0.41 2.09 6 -1 -25 -0.09 2.47 6 1 -25 5.50 2.45 5 -1 -25 2.69 2.49 5 1 -25 1.22 1.69 5 1 -25 2.09 2.86 4 -1 -25 0.03 1.54 4 -1 -25 1.67 2.54 4 1 -25 0.66 1.89 3 -1 -25 1.88 2.73 3 -1 -25 2.22 1.25 3 1 -25 5.97 2.85 3 1 -25 5.31 2.22 2 -1 -25 3.47 3.22 2 1 -25 4.68 2.44 2 1 -25 3.15 1.80 1 -1 -25 1.29 1.15 1 -1 -25 2.54 2.74 1 1 -25 -0.26 2.13 0 -1 25 2.92 1.52 0 -1 -25 0.76 2.79 0 -1 -25 1.99 1.40 0 1 -25 0.20 1.98 0 1 -25 0.62 1.86 7 0 -26 7.39 2.44 6 0 -26 20.89 3.38 5 0 -26 7.97 3.09 4 0 -26 3.63 2.42 3 0 -26 3.88 2.63 2 0 -26 11.70 3.38 1 0 -26 1.54 2.53 4 1 -26 11.95 3.22 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 20208 _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 0.5839(3) 0.0683(11) 0.33284(19) 0.0304(14) Uani 1 1 d . . . . . N1 N 0.6572(4) 0.4944(14) 0.3468(2) 0.0254(15) Uani 1 1 d D . . . . N2 N 0.5092(4) 0.4876(14) 0.3149(2) 0.0284(16) Uani 1 1 d D . . . . N3 N 0.1630(4) 0.6521(14) 0.4012(2) 0.0336(17) Uani 1 1 d . . . . . C1 C 0.5836(4) 0.3323(17) 0.3318(2) 0.0194(17) Uani 1 1 d . . . . . C2 C 0.4241(4) 0.3585(18) 0.2921(3) 0.037(2) Uani 1 1 d . . . . . H2A H 0.430593 0.146550 0.292766 0.044 Uiso 1 1 calc R U . . . H2B H 0.403562 0.418260 0.254364 0.044 Uiso 1 1 calc R U . . . C3 C 0.3555(4) 0.4399(17) 0.3207(3) 0.029(2) Uani 1 1 d . . . . . C4 C 0.2925(4) 0.6434(17) 0.3011(3) 0.033(2) Uani 1 1 d . . . . . H4 H 0.291851 0.735903 0.268498 0.040 Uiso 1 1 calc R U . . . C5 C 0.2303(5) 0.7180(19) 0.3271(3) 0.036(2) Uani 1 1 d . . . . . H5 H 0.188248 0.861410 0.312443 0.043 Uiso 1 1 calc R U . . . C6 C 0.2287(4) 0.5857(16) 0.3743(3) 0.027(2) Uani 1 1 d . . . . . C7 C 0.2920(5) 0.3825(18) 0.3952(3) 0.044(2) Uani 1 1 d . . . . . H7 H 0.291892 0.289335 0.427683 0.053 Uiso 1 1 calc R U . . . C8 C 0.3560(5) 0.3123(18) 0.3691(3) 0.044(2) Uani 1 1 d . . . . . H8 H 0.400118 0.176701 0.384585 0.053 Uiso 1 1 calc R U . . . C9 C 0.0761(4) 0.6995(17) 0.3715(3) 0.0262(19) Uani 1 1 d . . . . . C10 C 0.0405(5) 0.553(2) 0.3250(3) 0.045(2) Uani 1 1 d . . . . . H10 H 0.074166 0.412285 0.312616 0.054 Uiso 1 1 calc R U . . . C11 C -0.0441(5) 0.610(2) 0.2963(3) 0.057(3) Uani 1 1 d . . . . . H11 H -0.066945 0.508672 0.263971 0.069 Uiso 1 1 calc R U . . . C12 C -0.0964(5) 0.804(2) 0.3124(4) 0.058(3) Uani 1 1 d . . . . . H12 H -0.154537 0.841263 0.292283 0.070 Uiso 1 1 calc R U . . . C13 C -0.0602(6) 0.942(2) 0.3592(4) 0.070(3) Uani 1 1 d . . . . . H13 H -0.095006 1.077084 0.372036 0.084 Uiso 1 1 calc R U . . . C14 C 0.0243(5) 0.8959(19) 0.3888(3) 0.054(3) Uani 1 1 d . . . . . H14 H 0.046841 0.999020 0.420934 0.065 Uiso 1 1 calc R U . . . C15 C 0.1858(4) 0.6498(16) 0.4584(3) 0.030(2) Uani 1 1 d . . . . . C16 C 0.1308(5) 0.5333(18) 0.4865(3) 0.034(2) Uani 1 1 d . . . . . H16 H 0.076455 0.453097 0.467621 0.041 Uiso 1 1 calc R U . . . C17 C 0.1531(4) 0.5314(18) 0.5410(3) 0.032(2) Uani 1 1 d . . . . . H17 H 0.113430 0.451879 0.559016 0.038 Uiso 1 1 calc R U . . . C18 C 0.2321(4) 0.6427(15) 0.5707(3) 0.0217(18) Uani 1 1 d . . . . . C19 C 0.2871(4) 0.7617(17) 0.5420(3) 0.033(2) Uani 1 1 d . . . . . H19 H 0.341470 0.841812 0.560805 0.039 Uiso 1 1 calc R U . . . C20 C 0.2643(5) 0.7656(17) 0.4874(3) 0.034(2) Uani 1 1 d . . . . . H20 H 0.303045 0.849158 0.469154 0.041 Uiso 1 1 calc R U . . . C21 C 0.2580(4) 0.6366(17) 0.6306(3) 0.030(2) Uani 1 1 d . . . . . H21A H 0.258874 0.836186 0.643990 0.036 Uiso 1 1 calc R U . . . H21B H 0.213117 0.529013 0.643041 0.036 Uiso 1 1 calc R U . . . H2 H 0.515(5) 0.681(13) 0.315(3) 0.039(17) Uiso 1 1 d D . . . . H1 H 0.656(5) 0.688(13) 0.344(3) 0.039(17) Uiso 1 1 d D . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.033(3) 0.016(3) 0.035(3) 0.000(3) -0.005(2) 0.000(2) N1 0.027(4) 0.018(4) 0.027(4) 0.002(3) -0.001(3) 0.000(3) N2 0.026(4) 0.021(4) 0.035(4) -0.001(3) 0.002(3) 0.002(3) N3 0.029(4) 0.043(4) 0.025(4) -0.006(3) 0.002(3) 0.001(3) C1 0.024(4) 0.019(5) 0.010(4) 0.002(4) -0.004(3) 0.009(4) C2 0.026(4) 0.037(5) 0.043(5) 0.001(4) 0.001(4) 0.003(4) C3 0.020(4) 0.029(5) 0.034(5) 0.001(4) 0.001(4) -0.005(4) C4 0.021(4) 0.044(6) 0.028(4) 0.009(4) -0.005(4) 0.009(4) C5 0.027(4) 0.054(6) 0.027(5) 0.010(5) 0.006(4) 0.007(4) C6 0.026(4) 0.022(5) 0.020(4) -0.005(4) -0.013(3) 0.001(4) C7 0.060(6) 0.034(6) 0.040(5) 0.013(5) 0.017(5) 0.009(5) C8 0.051(5) 0.032(5) 0.046(6) 0.014(5) 0.007(4) 0.021(4) C9 0.017(4) 0.031(5) 0.024(4) 0.003(4) -0.006(3) -0.006(4) C10 0.028(5) 0.070(7) 0.030(5) -0.012(5) -0.003(4) -0.011(4) C11 0.027(5) 0.095(9) 0.045(6) 0.000(6) 0.001(4) -0.020(6) C12 0.027(5) 0.085(8) 0.054(6) 0.048(6) -0.005(5) -0.002(6) C13 0.048(6) 0.066(8) 0.085(8) 0.010(7) -0.002(6) 0.030(6) C14 0.061(6) 0.037(6) 0.051(6) -0.002(5) -0.007(5) 0.025(5) C15 0.029(4) 0.021(5) 0.037(5) -0.007(4) 0.004(4) -0.003(4) C16 0.025(4) 0.046(6) 0.031(5) -0.019(4) 0.007(4) -0.004(4) C17 0.020(4) 0.054(6) 0.020(4) -0.018(4) 0.003(3) -0.011(4) C18 0.024(4) 0.013(4) 0.027(4) 0.000(4) 0.005(3) 0.000(3) C19 0.026(4) 0.039(5) 0.028(5) 0.004(4) -0.001(4) 0.000(4) C20 0.038(5) 0.032(5) 0.028(5) 0.010(4) 0.000(4) -0.010(4) C21 0.026(4) 0.034(5) 0.027(4) -0.002(4) -0.002(3) 0.006(4) 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 C21 121.3(6) . 3_666 ? C1 N1 H1 122(5) . . ? C21 N1 H1 117(5) 3_666 . ? C1 N2 C2 123.3(6) . . ? C1 N2 H2 117(5) . . ? C2 N2 H2 120(5) . . ? C6 N3 C15 119.0(5) . . ? C9 N3 C6 119.8(6) . . ? C9 N3 C15 121.1(6) . . ? O1 C1 N1 123.3(6) . . ? O1 C1 N2 122.6(7) . . ? N2 C1 N1 114.1(7) . . ? N2 C2 H2A 108.8 . . ? N2 C2 H2B 108.8 . . ? N2 C2 C3 113.7(6) . . ? H2A C2 H2B 107.7 . . ? C3 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? C4 C3 C2 122.3(7) . . ? C4 C3 C8 117.5(7) . . ? C8 C3 C2 120.1(7) . . ? C3 C4 H4 118.8 . . ? C3 C4 C5 122.4(7) . . ? C5 C4 H4 118.8 . . ? C4 C5 H5 119.8 . . ? C4 C5 C6 120.3(7) . . ? C6 C5 H5 119.8 . . ? C5 C6 N3 121.5(6) . . ? C5 C6 C7 118.4(7) . . ? C7 C6 N3 120.1(7) . . ? C6 C7 H7 119.6 . . ? C6 C7 C8 120.8(7) . . ? C8 C7 H7 119.6 . . ? C3 C8 C7 120.4(7) . . ? C3 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 N3 121.6(7) . . ? C10 C9 C14 118.2(7) . . ? C14 C9 N3 120.3(7) . . ? C9 C10 H10 120.0 . . ? C9 C10 C11 120.0(9) . . ? C11 C10 H10 120.0 . . ? C10 C11 H11 118.5 . . ? C12 C11 C10 122.9(9) . . ? C12 C11 H11 118.5 . . ? C11 C12 H12 122.0 . . ? C11 C12 C13 115.9(8) . . ? C13 C12 H12 122.0 . . ? C12 C13 H13 118.4 . . ? C12 C13 C14 123.2(9) . . ? C14 C13 H13 118.4 . . ? C9 C14 C13 119.8(8) . . ? C9 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 N3 121.7(6) . . ? C16 C15 C20 117.6(7) . . ? C20 C15 N3 120.7(7) . . ? C15 C16 H16 119.3 . . ? C17 C16 C15 121.4(7) . . ? C17 C16 H16 119.3 . . ? C16 C17 H17 119.1 . . ? C16 C17 C18 121.7(7) . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 116.6(6) . . ? C17 C18 C21 122.1(6) . . ? C19 C18 C21 121.3(6) . . ? C18 C19 H19 119.2 . . ? C20 C19 C18 121.6(7) . . ? C20 C19 H19 119.2 . . ? C15 C20 H20 119.4 . . ? C19 C20 C15 121.1(7) . . ? C19 C20 H20 119.4 . . ? N1 C21 C18 113.7(6) 3_666 . ? N1 C21 H21A 108.8 3_666 . ? N1 C21 H21B 108.8 3_666 . ? C18 C21 H21A 108.8 . . ? C18 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? 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 1.228(8) . ? N1 C1 1.359(9) . ? N1 C21 1.453(9) 3_666 ? N1 H1 0.90(6) . ? N2 C1 1.354(9) . ? N2 C2 1.455(9) . ? N2 H2 0.91(6) . ? N3 C6 1.430(9) . ? N3 C9 1.411(8) . ? N3 C15 1.437(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.517(10) . ? C3 C4 1.374(10) . ? C3 C8 1.391(10) . ? C4 H4 0.9500 . ? C4 C5 1.375(10) . ? C5 H5 0.9500 . ? C5 C6 1.381(10) . ? C6 C7 1.382(10) . ? C7 H7 0.9500 . ? C7 C8 1.397(11) . ? C8 H8 0.9500 . ? C9 C10 1.377(10) . ? C9 C14 1.378(11) . ? C10 H10 0.9500 . ? C10 C11 1.381(11) . ? C11 H11 0.9500 . ? C11 C12 1.363(13) . ? C12 H12 0.9500 . ? C12 C13 1.365(13) . ? C13 H13 0.9500 . ? C13 C14 1.379(11) . ? C14 H14 0.9500 . ? C15 C16 1.385(10) . ? C15 C20 1.387(10) . ? C16 H16 0.9500 . ? C16 C17 1.370(10) . ? C17 H17 0.9500 . ? C17 C18 1.390(9) . ? C18 C19 1.398(10) . ? C18 C21 1.507(9) . ? C19 H19 0.9500 . ? C19 C20 1.374(10) . ? C20 H20 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N2 H2 O1 0.91(6) 2.09(6) 2.935(8) 154(6) 1_565 yes N1 H1 O1 0.90(6) 2.08(6) 2.895(8) 149(6) 1_565 yes 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 101.9(8) . . . . ? N2 C2 C3 C8 -76.5(9) . . . . ? N3 C6 C7 C8 179.2(7) . . . . ? N3 C9 C10 C11 -178.5(8) . . . . ? N3 C9 C14 C13 179.4(8) . . . . ? N3 C15 C16 C17 179.9(7) . . . . ? N3 C15 C20 C19 -179.3(7) . . . . ? C1 N2 C2 C3 123.9(8) . . . . ? C2 N2 C1 O1 -5.8(11) . . . . ? C2 N2 C1 N1 173.6(6) . . . . ? C2 C3 C4 C5 -179.8(7) . . . . ? C2 C3 C8 C7 -178.8(7) . . . . ? C3 C4 C5 C6 -0.7(12) . . . . ? C4 C3 C8 C7 2.7(12) . . . . ? C4 C5 C6 N3 -177.8(7) . . . . ? C4 C5 C6 C7 1.4(11) . . . . ? C5 C6 C7 C8 0.0(12) . . . . ? C6 N3 C9 C10 34.1(11) . . . . ? C6 N3 C9 C14 -146.1(8) . . . . ? C6 N3 C15 C16 -138.4(7) . . . . ? C6 N3 C15 C20 41.7(11) . . . . ? C6 C7 C8 C3 -2.0(13) . . . . ? C8 C3 C4 C5 -1.3(11) . . . . ? C9 N3 C6 C5 38.8(10) . . . . ? C9 N3 C6 C7 -140.4(7) . . . . ? C9 N3 C15 C16 37.3(11) . . . . ? C9 N3 C15 C20 -142.6(8) . . . . ? C9 C10 C11 C12 -1.3(14) . . . . ? C10 C9 C14 C13 -0.7(13) . . . . ? C10 C11 C12 C13 -0.1(14) . . . . ? C11 C12 C13 C14 1.1(15) . . . . ? C12 C13 C14 C9 -0.7(15) . . . . ? C14 C9 C10 C11 1.7(12) . . . . ? C15 N3 C6 C5 -145.4(7) . . . . ? C15 N3 C6 C7 35.4(10) . . . . ? C15 N3 C9 C10 -141.6(8) . . . . ? C15 N3 C9 C14 38.2(11) . . . . ? C15 C16 C17 C18 -0.8(13) . . . . ? C16 C15 C20 C19 0.8(12) . . . . ? C16 C17 C18 C19 1.2(11) . . . . ? C16 C17 C18 C21 -178.8(7) . . . . ? C17 C18 C19 C20 -0.6(11) . . . . ? C17 C18 C21 N1 126.5(7) . . . 3_666 ? C18 C19 C20 C15 -0.3(12) . . . . ? C19 C18 C21 N1 -53.6(10) . . . 3_666 ? C20 C15 C16 C17 -0.2(12) . . . . ? C21 N1 C1 O1 -4.9(11) 3_666 . . . ? C21 N1 C1 N2 175.6(6) 3_666 . . . ? C21 C18 C19 C20 179.4(7) . . . . ?