#------------------------------------------------------------------------------ #$Date: 2019-10-29 03:12:03 +0200 (Tue, 29 Oct 2019) $ #$Revision: 220332 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/25/1552501.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_1552501 loop_ _publ_author_name 'Shi, Taoda' 'Wijeratne, E. M. Kithsiri' 'Solano, Cristian' 'Ambrose, Andrew J.' 'Ross, Alison B.' 'Norwood, Charles' 'Orido, Charles K.' 'Grigoryan, Tigran' 'Tillotson, Joseph' 'Kang, Minjin' 'Luo, Gang' 'Keegan, Bradley M.' 'Hu, Wenhao' 'Blagg, Brian S. J.' 'Zhang, Donna D.' 'Gunatilaka, A. A. Leslie' 'Chapman, Eli' _publ_section_title ; An Isoform-Selective PTP1B Inhibitor Derived from Nitrogen-Atom Augmentation of Radicicol. ; _journal_issue 30 _journal_name_full Biochemistry _journal_page_first 3225 _journal_page_last 3231 _journal_paper_doi 10.1021/acs.biochem.9b00499 _journal_volume 58 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_moiety 'C18 H21 Cl N2 O5' _chemical_formula_sum 'C18 H21 Cl N2 O5' _chemical_formula_weight 380.82 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-11-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 103.59(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 32.35(2) _cell_length_b 6.672(4) _cell_length_c 8.016(5) _cell_measurement_reflns_used 2061 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.221 _cell_measurement_theta_min 2.59 _cell_volume 1681.7(18) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_unetI/netI 0.0668 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 10146 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.751 _diffrn_reflns_theta_min 1.295 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6527 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0551 before and 0.0484 after correction. The Ratio of minimum to maximum transmission is 0.8758. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour 'metallic light colourless' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.504 _exptl_crystal_description plate _exptl_crystal_F_000 800 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.277 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.057 _refine_ls_abs_structure_details ; Flack x determined using 913 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.14(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.802 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 240 _refine_ls_number_reflns 3212 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.802 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0430 _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1062 _refine_ls_wR_factor_ref 0.1227 _reflns_Friedel_coverage 0.829 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.993 _reflns_number_gt 2540 _reflns_number_total 3212 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bi9b00499_si_002.cif _cod_data_source_block mo_ts100k_0ma _cod_original_cell_volume 1681.6(18) _cod_database_code 1552501 _shelx_shelxl_version_number 2014/7 _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 0.987 _shelx_estimated_absorpt_t_min 0.914 _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, All O(H) groups 2.a Ternary CH refined with riding coordinates: C17(H17), C11(H11), C14(H14), C15(H15) 2.b Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C16(H16A,H16B), C10(H10A,H10B), C12(H12A,H12B) 2.c Aromatic/amide H refined with riding coordinates: C4(H4A), C8(H8) 2.d Idealised Me refined as rotating group: C18(H18A,H18B,H18C) 2.e Idealised tetrahedral OH refined as rotating group: O3(H3), O5(H5), O4(H4), O2(H2) ; _shelx_res_file ; mo_ts100k_0ma.res created by SHELXL-2014/7 TITL mo_ts100k_0ma_a.res in C2 REM Old TITL mo_TS100K_0ma in P1 REM SHELXT solution in C2 REM R1 0.091, Rweak 0.021, Alpha 0.008, Orientation as input REM Flack x = 0.121 ( 0.051 ) from Parsons' quotients REM Formula found by SHELXT: C18 N2 O5 Cl CELL 0.71073 32.3475 6.6719 8.0161 90.001 103.589 89.999 ZERR 4 0.0228 0.0038 0.0049 0 0.02 0 LATT -7 SYMM -X,+Y,-Z SFAC C H Cl N O UNIT 72 84 4 8 20 L.S. 15 PLAN 60 SIZE 0.05 0.2 0.35 TEMP -173.15 BOND $H list 4 fmap 2 53 ACTA REM REM REM WGHT 0.100000 FVAR 0.22929 CL1 3 0.196120 0.753072 0.535122 11.00000 0.01724 0.01761 = 0.01181 -0.00014 0.00651 0.00035 O1 5 0.358098 0.807000 0.212327 11.00000 0.01898 0.01900 = 0.01222 0.00090 0.00947 -0.00103 O3 5 0.158808 0.753711 0.170147 11.00000 0.01696 0.02740 = 0.01266 -0.00129 0.00173 0.00084 AFIX 147 H3 2 0.149152 0.723492 0.066579 11.00000 -1.50000 AFIX 0 O5 5 0.377537 0.208945 0.161996 11.00000 0.02053 0.02227 = 0.01425 0.00003 0.00000 -0.00357 AFIX 147 H5 2 0.375743 0.090570 0.195281 11.00000 -1.50000 AFIX 0 O4 5 0.407820 0.365505 0.673752 11.00000 0.02232 0.02229 = 0.01334 0.00006 0.00764 -0.00459 AFIX 147 H4 2 0.383326 0.325896 0.676288 11.00000 -1.50000 AFIX 0 O2 5 0.287478 0.769215 -0.016816 11.00000 0.01889 0.03024 = 0.00941 -0.00050 0.00615 -0.00335 AFIX 147 H2 2 0.313798 0.757508 0.023228 11.00000 -1.50000 AFIX 0 N1 4 0.356546 0.778027 0.493392 11.00000 0.01386 0.01607 = 0.01053 -0.00006 0.00457 -0.00040 N2 4 0.401150 0.806418 0.547172 11.00000 0.01249 0.01186 = 0.01171 -0.00188 0.00254 -0.00346 C5 1 0.202191 0.757240 0.205238 11.00000 0.01406 0.01233 = 0.01591 -0.00177 0.00244 0.00087 C7 1 0.269045 0.760817 0.420684 11.00000 0.01735 0.00815 = 0.01136 -0.00140 0.00320 0.00093 C3 1 0.267276 0.765768 0.113217 11.00000 0.02220 0.01440 = 0.00938 0.00056 0.00672 -0.00140 C2 1 0.290784 0.767478 0.286177 11.00000 0.01592 0.01212 = 0.01114 -0.00168 0.00556 -0.00224 C4 1 0.223788 0.762335 0.073475 11.00000 0.02014 0.01651 = 0.00899 0.00416 0.00227 0.00360 AFIX 43 H4A 2 0.208358 0.763408 -0.043042 11.00000 -1.20000 AFIX 0 C1 1 0.336401 0.784719 0.324866 11.00000 0.02243 0.01091 = 0.00904 0.00090 0.00280 -0.00280 C8 1 0.293672 0.758794 0.595211 11.00000 0.01775 0.01182 = 0.00981 -0.00112 0.00560 -0.00072 AFIX 43 H8 2 0.279730 0.751694 0.686966 11.00000 -1.20000 AFIX 0 C6 1 0.224332 0.755659 0.374734 11.00000 0.01989 0.01044 = 0.01278 0.00297 0.00879 0.00127 C13 1 0.467941 0.665750 0.656662 11.00000 0.01458 0.02145 = 0.02003 -0.00256 0.00299 -0.00248 AFIX 23 H13A 2 0.483637 0.537833 0.682813 11.00000 -1.20000 H13B 2 0.487080 0.766781 0.624353 11.00000 -1.20000 AFIX 0 C17 1 0.420492 0.279835 0.223355 11.00000 0.01748 0.01590 = 0.01489 -0.00369 0.00141 -0.00377 AFIX 13 H17 2 0.421917 0.421656 0.184736 11.00000 -1.20000 AFIX 0 C11 1 0.409572 0.844398 0.735887 11.00000 0.01733 0.01748 = 0.01432 -0.00432 0.00352 -0.00635 AFIX 13 H11 2 0.413172 0.991648 0.757807 11.00000 -1.20000 AFIX 0 C16 1 0.432631 0.275746 0.419385 11.00000 0.01729 0.01599 = 0.02174 -0.00401 0.00564 -0.00108 AFIX 23 H16A 2 0.463458 0.303244 0.459005 11.00000 -1.20000 H16B 2 0.427357 0.139541 0.458799 11.00000 -1.20000 AFIX 0 C10 1 0.369920 0.771261 0.792713 11.00000 0.01802 0.01543 = 0.01079 -0.00266 0.00492 -0.00071 AFIX 23 H10A 2 0.374548 0.636183 0.844881 11.00000 -1.20000 H10B 2 0.362206 0.865006 0.876227 11.00000 -1.20000 AFIX 0 C9 1 0.336378 0.766922 0.628933 11.00000 0.02163 0.01089 = 0.00844 0.00258 0.00819 0.00058 C12 1 0.451885 0.737439 0.811861 11.00000 0.01939 0.02149 = 0.01290 -0.00428 0.00294 0.00171 AFIX 23 H12A 2 0.472514 0.830781 0.883087 11.00000 -1.20000 H12B 2 0.447454 0.622416 0.883719 11.00000 -1.20000 AFIX 0 C14 1 0.427919 0.637100 0.510760 11.00000 0.01519 0.01409 = 0.01332 -0.00315 0.00544 -0.00076 AFIX 13 H14 2 0.435626 0.664354 0.399181 11.00000 -1.20000 AFIX 0 C15 1 0.408202 0.427225 0.502330 11.00000 0.02087 0.01453 = 0.01102 -0.00245 0.00598 -0.00119 AFIX 13 H15 2 0.378211 0.434173 0.432775 11.00000 -1.20000 AFIX 0 C18 1 0.450720 0.154225 0.146987 11.00000 0.02675 0.03766 = 0.02406 -0.00971 0.01064 0.00353 AFIX 137 H18A 2 0.449833 0.014694 0.184183 11.00000 -1.50000 H18B 2 0.479716 0.206256 0.186125 11.00000 -1.50000 H18C 2 0.442083 0.160809 0.021460 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_ts100k_0ma_a.res in C2 REM R1 = 0.0430 for 2540 Fo > 4sig(Fo) and 0.0663 for all 3212 data REM 240 parameters refined using 1 restraints END WGHT 0.0404 0.0000 REM Highest difference peak 0.277, deepest hole -0.242, 1-sigma level 0.057 Q1 1 0.5000 0.1269 0.0000 10.50000 0.05 0.28 Q2 1 0.3418 0.7709 0.5629 11.00000 0.05 0.23 Q3 1 0.1760 0.7573 0.3766 11.00000 0.05 0.22 Q4 1 0.2797 0.7650 0.1924 11.00000 0.05 0.22 Q5 1 0.2399 0.7548 0.1010 11.00000 0.05 0.22 Q6 1 0.2783 0.7500 0.3456 11.00000 0.05 0.20 Q7 1 0.5181 0.8374 0.9238 11.00000 0.05 0.20 Q8 1 0.4396 0.1788 -0.0202 11.00000 0.05 0.20 Q9 1 0.2202 0.7795 0.1494 11.00000 0.05 0.20 Q10 1 0.3978 0.8269 0.1999 11.00000 0.05 0.19 Q11 1 0.2219 0.7297 0.1404 11.00000 0.05 0.19 Q12 1 0.5000 0.3270 0.0000 10.50000 0.05 0.19 Q13 1 0.2223 0.7562 0.0274 11.00000 0.05 0.19 Q14 1 0.4954 0.7575 0.9474 11.00000 0.05 0.19 Q15 1 0.1984 0.7604 -0.0876 11.00000 0.05 0.18 Q16 1 0.3013 0.7485 0.2838 11.00000 0.05 0.18 Q17 1 0.4763 0.8489 0.5975 11.00000 0.05 0.18 Q18 1 0.4407 -0.1778 0.2607 11.00000 0.05 0.17 Q19 1 0.3613 0.6408 0.4180 11.00000 0.05 0.17 Q20 1 0.2575 0.9792 0.4366 11.00000 0.05 0.17 Q21 1 0.3566 0.3202 0.1184 11.00000 0.05 0.17 Q22 1 0.3804 0.3791 0.0496 11.00000 0.05 0.16 Q23 1 0.2393 0.6734 0.7274 11.00000 0.05 0.16 Q24 1 0.5247 0.7612 0.8161 11.00000 0.05 0.16 Q25 1 0.4146 0.7037 0.7951 11.00000 0.05 0.16 Q26 1 0.4174 0.5288 0.4774 11.00000 0.05 0.16 Q27 1 0.5007 0.0717 0.3615 11.00000 0.05 0.16 Q28 1 0.2856 0.7533 0.5004 11.00000 0.05 0.16 Q29 1 0.2241 0.7560 0.6279 11.00000 0.05 0.16 Q30 1 0.4213 0.8172 0.7981 11.00000 0.05 0.16 Q31 1 0.1823 0.7607 0.0536 11.00000 0.05 0.16 Q32 1 0.3444 0.8811 0.1720 11.00000 0.05 0.15 Q33 1 0.4402 0.2863 0.3287 11.00000 0.05 0.15 Q34 1 0.4409 0.1810 0.2051 11.00000 0.05 0.15 Q35 1 0.3835 0.5446 0.9982 11.00000 0.05 0.15 Q36 1 0.3413 0.2440 0.0837 11.00000 0.05 0.15 Q37 1 0.5024 0.8781 0.9396 11.00000 0.05 0.15 Q38 1 0.4020 0.8190 0.9393 11.00000 0.05 0.15 Q39 1 0.4388 0.3341 0.7186 11.00000 0.05 0.14 Q40 1 0.4233 0.7080 0.9431 11.00000 0.05 0.14 Q41 1 0.2358 0.8133 0.7322 11.00000 0.05 0.14 Q42 1 0.4784 0.6220 0.9234 11.00000 0.05 0.14 Q43 1 0.2836 0.9066 0.7160 11.00000 0.05 0.14 Q44 1 0.1569 0.8613 0.0541 11.00000 0.05 0.14 Q45 1 0.2558 0.6769 0.0952 11.00000 0.05 0.14 Q46 1 0.2600 0.8453 -0.0671 11.00000 0.05 0.14 Q47 1 0.4921 0.7445 0.7014 11.00000 0.05 0.14 Q48 1 0.2668 0.7336 -0.1702 11.00000 0.05 0.14 Q49 1 0.4554 0.4931 0.9020 11.00000 0.05 0.14 Q50 1 0.4761 0.9185 0.9154 11.00000 0.05 0.14 Q51 1 0.3200 0.6637 0.5611 11.00000 0.05 0.14 Q52 1 0.4336 0.3093 -0.0314 11.00000 0.05 0.14 Q53 1 0.2202 0.6842 -0.2202 11.00000 0.05 0.14 Q54 1 0.4798 0.0857 0.2148 11.00000 0.05 0.14 Q55 1 0.5000 0.5745 1.0000 10.50000 0.05 0.14 Q56 1 0.2397 0.7991 0.3967 11.00000 0.05 0.14 Q57 1 0.4804 0.2922 0.6637 11.00000 0.05 0.14 Q58 1 0.4433 0.8327 0.3979 11.00000 0.05 0.13 Q59 1 0.1401 0.7439 -0.0110 11.00000 0.05 0.13 Q60 1 0.3176 0.8344 0.6141 11.00000 0.05 0.13 ; _shelx_res_checksum 16411 _shelx_hkl_file ; 2 0 0 572.24 9.80 -2 0 0 459.85 9.70 -2 0 0 465.95 9.80 4 0 0 261.77 5.90 4 0 0 265.37 5.90 -4 0 0 263.17 6.00 -4 0 0 281.47 6.30 -4 0 0 251.37 5.90 6 0 0 277.27 6.70 6 0 0 272.77 6.80 -6 0 0 265.17 6.80 -6 0 0 280.37 7.20 -6 0 0 274.67 6.70 -6 0 0 280.67 7.20 8 0 0 313.77 7.70 8 0 0 321.17 10.70 8 0 0 291.47 7.80 -8 0 0 305.07 7.80 -8 0 0 307.37 8.40 -8 0 0 311.17 7.70 -8 0 0 301.77 8.20 10 0 0 70.09 4.20 10 0 0 76.79 4.20 -10 0 0 76.59 4.90 -10 0 0 74.59 4.30 -10 0 0 75.79 5.00 -10 0 0 75.49 4.60 12 0 0 209.48 7.00 12 0 0 217.98 6.80 -12 0 0 204.68 7.50 -12 0 0 209.08 6.80 -12 0 0 206.48 7.50 14 0 0 481.45 12.10 14 0 0 452.05 11.90 14 0 0 459.55 11.40 -14 0 0 462.75 11.60 -14 0 0 446.96 12.10 -14 0 0 448.56 11.60 -14 0 0 454.85 12.30 16 0 0 288.47 9.00 16 0 0 302.47 8.80 -16 0 0 282.97 9.00 -16 0 0 294.87 9.50 -16 0 0 280.47 9.50 -16 0 0 300.77 9.20 18 0 0 44.20 4.30 18 0 0 53.69 4.40 -18 0 0 41.30 4.30 -18 0 0 34.70 4.20 -18 0 0 43.90 4.80 20 0 0 39.80 4.50 20 0 0 37.30 4.40 -20 0 0 49.40 4.60 -20 0 0 43.50 4.90 -20 0 0 45.90 5.00 22 0 0 2.10 3.10 -22 0 0 1.50 3.70 -22 0 0 1.50 3.40 -22 0 0 -3.80 3.70 24 0 0 16.90 4.20 -24 0 0 22.30 4.50 -24 0 0 12.40 4.50 -24 0 0 15.40 5.00 26 0 0 3.20 4.00 -26 0 0 7.10 5.00 -26 0 0 13.20 4.50 -26 0 0 -0.60 4.40 28 0 0 132.69 8.60 -28 0 0 124.09 8.30 -28 0 0 114.49 9.20 -28 0 0 121.39 9.70 30 0 0 61.39 6.80 -30 0 0 61.89 7.40 -30 0 0 64.89 7.50 -30 0 0 69.09 7.00 32 0 0 4.80 5.00 -32 0 0 -2.00 5.50 -32 0 0 -3.70 5.30 -32 0 0 -5.10 5.40 34 0 0 -0.60 5.00 -34 0 0 -4.50 5.60 -34 0 0 -0.80 5.90 -34 0 0 -0.50 6.00 36 0 0 -3.20 5.30 -36 0 0 12.70 6.70 -36 0 0 6.20 6.40 -36 0 0 -0.60 6.10 38 0 0 24.20 6.80 -38 0 0 17.80 7.20 -38 0 0 22.60 8.40 -38 0 0 24.20 7.60 -37 1 0 12.10 7.10 -37 1 0 4.30 6.30 37 -1 0 7.90 6.00 -35 1 0 12.60 6.30 -35 1 0 6.40 6.40 35 -1 0 8.60 5.50 -33 1 0 14.60 5.70 -33 1 0 18.30 6.50 -33 1 0 17.80 6.30 33 -1 0 20.60 6.00 -31 1 0 72.99 6.90 -31 1 0 71.79 7.90 -31 1 0 57.59 7.60 31 -1 0 60.99 7.20 -29 1 0 159.88 10.50 -29 1 0 163.88 10.70 -29 1 0 164.98 8.90 29 -1 0 136.39 9.00 -27 1 0 -0.20 4.80 -27 1 0 -4.10 4.90 -27 1 0 2.90 4.00 27 -1 0 0.10 4.10 -25 1 0 109.09 8.50 -25 1 0 110.59 8.30 -25 1 0 103.29 6.90 25 -1 0 100.19 7.20 -23 1 0 61.99 5.00 -23 1 0 61.89 6.00 -23 1 0 51.39 5.90 23 -1 0 58.09 5.50 23 -1 0 59.19 4.90 -21 1 0 4.60 3.10 -21 1 0 6.60 4.10 -21 1 0 4.40 3.70 21 -1 0 10.90 3.40 21 -1 0 1.60 2.50 -19 1 0 18.60 3.10 -19 1 0 22.00 4.20 -19 1 0 23.50 4.20 19 -1 0 20.10 2.90 19 -1 0 13.10 3.40 -17 1 0 33.30 4.50 -17 1 0 34.70 4.30 -17 1 0 30.10 3.20 17 -1 0 36.40 3.30 17 -1 0 33.10 3.80 -15 1 0 105.49 4.90 -15 1 0 98.89 6.30 -15 1 0 94.59 6.10 15 -1 0 99.19 4.60 15 -1 0 100.79 5.80 15 -1 0 108.89 5.80 -13 1 0 134.09 5.10 -13 1 0 125.49 6.20 -13 1 0 126.59 6.50 13 -1 0 142.69 5.00 13 -1 0 136.89 6.00 13 -1 0 142.29 6.10 -11 1 0 420.66 9.70 -11 1 0 413.96 11.10 -11 1 0 406.56 10.90 11 -1 0 447.66 11.00 11 -1 0 425.06 9.70 11 -1 0 402.36 10.80 -9 1 0 9.30 2.90 -9 1 0 3.00 2.60 -9 1 0 6.50 1.80 9 -1 0 9.40 2.60 9 -1 0 5.80 2.30 9 -1 0 4.70 1.70 -7 1 0 327.57 8.60 -7 1 0 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164.08 8.50 -5 -3 7 162.48 8.90 -5 -3 7 158.28 8.40 -7 -3 7 223.18 9.80 -7 -3 7 230.88 10.70 -7 -3 7 225.88 9.60 -9 -3 7 18.10 4.90 -9 -3 7 12.00 3.80 -9 -3 7 15.30 4.20 -11 -3 7 63.69 5.90 -11 -3 7 65.99 6.40 -11 -3 7 49.60 6.70 -13 -3 7 12.80 4.00 -13 -3 7 13.10 5.20 -15 -3 7 36.50 6.40 -15 -3 7 29.70 4.60 -17 -3 7 7.40 5.20 -17 -3 7 7.10 3.70 -19 -3 7 19.00 4.50 -19 -3 7 17.10 5.90 -21 -3 7 33.60 5.20 -21 -3 7 24.70 6.50 -23 -3 7 55.59 6.30 -23 -3 7 46.40 7.60 -25 -3 7 4.90 4.60 -25 -3 7 -9.20 5.10 -27 -3 7 53.39 8.60 -27 -3 7 48.00 6.50 -29 -3 7 14.20 6.10 -29 -3 7 15.20 6.50 -12 4 -7 26.90 8.70 12 -4 7 34.80 6.70 -10 4 -7 19.60 7.70 10 -4 7 0.90 5.20 -8 4 -7 19.80 7.80 8 -4 7 9.20 5.10 -6 4 -7 7.80 7.10 6 -4 7 7.60 5.00 -4 4 -7 9.80 7.10 4 -4 7 15.00 5.30 -2 4 -7 8.90 6.40 2 -4 7 15.50 5.00 0 4 -7 3.70 6.50 0 -4 7 -7.60 4.00 0 -4 7 3.30 3.70 2 4 -7 14.40 6.60 -2 -4 7 12.40 4.00 -2 -4 7 17.50 5.00 -2 -4 7 21.20 4.80 -4 -4 7 77.59 6.50 -4 -4 7 87.79 7.70 -4 -4 7 69.09 6.80 -6 -4 7 50.79 5.50 -6 -4 7 52.59 6.20 -6 -4 7 60.79 6.90 -8 -4 7 34.90 6.00 -8 -4 7 32.90 4.80 -8 -4 7 41.10 5.90 -10 -4 7 46.20 6.40 -10 -4 7 58.89 6.80 -10 -4 7 55.99 5.60 -12 -4 7 47.20 6.60 -12 -4 7 34.20 6.00 -12 -4 7 40.90 4.90 -14 -4 7 21.10 5.40 -14 -4 7 25.50 4.30 -14 -4 7 29.70 6.20 -16 -4 7 39.40 6.90 -16 -4 7 22.10 5.80 -18 -4 7 0.90 5.50 -20 -4 7 3.40 5.70 -22 -4 7 58.69 8.30 -24 -4 7 28.40 7.10 -5 5 -7 14.70 7.30 5 -5 7 7.90 5.50 -3 5 -7 17.10 7.10 3 -5 7 12.70 5.60 -1 5 -7 13.20 6.70 1 -5 7 8.00 5.30 -1 -5 7 31.10 6.50 -3 -5 7 9.40 5.50 -5 -5 7 97.79 8.80 -7 -5 7 141.49 8.90 -7 -5 7 125.09 9.90 -9 -5 7 9.10 5.20 -9 -5 7 1.70 4.40 -11 -5 7 8.40 5.10 -11 -5 7 23.50 5.60 -13 -5 7 5.80 5.20 -13 -5 7 -1.40 4.70 -15 -5 7 11.40 5.40 -15 -5 7 7.70 5.60 -17 -5 7 8.20 5.30 -17 -5 7 -1.80 5.10 -19 -5 7 23.80 6.80 4 4 8 15.30 6.50 2 4 8 30.80 6.70 2 4 8 43.00 7.80 0 4 8 14.40 6.30 0 4 8 10.00 5.70 -2 4 8 4.80 5.90 -2 4 8 15.90 5.80 -4 4 8 10.90 6.20 -4 4 8 12.30 5.80 -6 4 8 35.30 7.40 -6 4 8 42.00 7.10 -8 4 8 16.20 5.90 -8 4 8 15.50 6.50 -10 4 8 8.40 5.90 -10 4 8 9.10 5.80 -12 4 8 25.90 6.20 -12 4 8 16.90 6.40 -14 4 8 1.60 5.60 -14 4 8 8.10 5.40 -16 4 8 12.80 6.20 -16 4 8 13.00 5.90 -18 4 8 15.70 6.40 -18 4 8 6.90 6.00 -9 -3 -8 14.80 7.60 -7 -3 -8 19.30 7.60 7 3 8 4.50 5.30 7 3 8 11.90 6.10 -5 -3 -8 1.40 6.60 5 3 8 6.40 5.60 5 3 8 10.10 5.20 3 3 8 -1.30 5.50 3 3 8 12.50 5.50 1 3 8 10.20 5.00 1 3 8 9.40 6.00 -1 3 8 19.80 5.50 -1 3 8 9.80 5.70 -3 3 8 10.80 5.60 -3 3 8 19.80 5.60 -5 3 8 13.50 6.10 -5 3 8 8.80 5.00 -7 3 8 7.10 5.60 -7 3 8 6.90 4.90 -9 3 8 32.50 5.90 -9 3 8 29.10 6.70 -11 3 8 2.00 5.20 -11 3 8 -3.60 4.50 -13 3 8 1.20 4.80 -13 3 8 10.00 5.60 -15 3 8 12.00 5.30 -15 3 8 29.60 6.20 -17 3 8 24.70 6.00 -17 3 8 24.50 6.50 -19 3 8 47.60 6.80 -19 3 8 69.29 8.40 -21 3 8 3.00 5.60 -21 3 8 7.10 5.40 -23 3 8 19.00 6.60 -23 3 8 21.00 6.90 -23 3 8 16.70 5.90 -12 -2 -8 9.30 7.80 -10 -2 -8 -3.20 7.20 -8 -2 -8 -1.30 6.90 -6 -2 -8 13.60 7.40 -4 -2 -8 72.89 9.70 4 2 8 52.19 6.20 4 2 8 75.59 8.50 -2 -2 -8 18.90 7.50 2 2 8 16.60 5.70 2 2 8 25.80 5.20 0 2 8 10.60 4.70 0 2 8 13.80 5.80 -2 2 8 10.10 4.50 -2 2 8 8.80 5.50 -4 2 8 32.90 5.30 -4 2 8 31.10 6.50 -6 2 8 29.40 5.10 -6 2 8 25.90 6.20 -8 2 8 30.60 5.20 -8 2 8 19.10 5.80 -10 2 8 38.20 5.60 -10 2 8 37.90 6.70 -12 2 8 14.80 4.70 -12 2 8 15.90 5.60 -14 2 8 9.10 5.30 -14 2 8 1.40 4.20 -16 2 8 21.30 5.80 -16 2 8 26.30 5.10 -18 2 8 10.20 5.40 -18 2 8 9.70 4.60 -20 2 8 19.50 5.40 -20 2 8 30.30 6.40 -22 2 8 31.60 6.00 -22 2 8 22.90 6.30 -22 2 8 38.60 7.30 -24 2 8 35.20 7.40 -24 2 8 25.40 6.50 -24 2 8 35.90 6.10 -26 2 8 2.10 5.50 -26 2 8 4.40 5.10 -26 2 8 11.50 6.30 -13 -1 -8 6.10 7.70 -11 -1 -8 8.00 7.80 -9 -1 -8 31.10 8.50 -7 -1 -8 15.20 7.50 -5 -1 -8 3.70 6.90 -3 -1 -8 33.20 8.10 3 1 8 26.50 6.10 -1 -1 -8 11.20 6.70 1 1 8 14.80 5.40 1 -1 -8 1.50 6.30 -1 1 8 1.20 4.60 -1 1 8 -5.80 3.50 -3 1 8 10.20 5.30 -3 1 8 10.50 4.00 -5 1 8 11.50 3.80 -5 1 8 5.80 5.00 -7 1 8 39.80 4.80 -7 1 8 33.30 6.40 -9 1 8 23.00 4.20 -9 1 8 12.30 5.50 -11 1 8 2.40 3.50 -11 1 8 -6.30 4.20 -13 1 8 2.50 3.60 -13 1 8 7.40 5.00 -15 1 8 34.50 4.90 -15 1 8 27.80 6.10 -17 1 8 50.39 5.30 -17 1 8 55.19 7.40 -19 1 8 6.80 5.70 -19 1 8 21.90 4.70 -19 1 8 14.60 5.60 -21 1 8 15.90 4.70 -21 1 8 29.30 6.50 -21 1 8 19.10 5.90 -23 1 8 2.60 5.10 -23 1 8 3.90 5.60 -23 1 8 -1.50 4.10 -25 1 8 52.39 7.70 -25 1 8 69.09 8.50 -25 1 8 55.89 6.60 -27 1 8 30.40 6.80 -27 1 8 33.60 7.40 -27 1 8 41.10 6.30 -29 1 8 29.00 7.40 -29 1 8 37.30 6.50 -29 1 8 33.70 7.40 -14 0 -8 5.90 7.90 -12 0 -8 -2.50 7.40 -10 0 -8 25.10 8.30 -8 0 -8 14.60 7.50 -6 0 -8 20.20 7.60 -4 0 -8 95.89 10.40 -2 0 -8 4.00 6.70 2 0 8 -2.50 4.80 0 0 -8 8.80 6.80 0 0 8 5.70 4.90 2 0 -8 9.10 6.80 -2 0 8 3.20 4.80 -4 0 8 76.49 7.80 -6 0 8 -3.20 4.50 -8 0 8 -2.50 4.30 -10 0 8 27.20 4.10 -10 0 8 20.60 5.50 -12 0 8 9.10 5.00 -14 0 8 -5.10 4.70 -14 0 8 3.90 4.60 -16 0 8 15.60 5.80 -16 0 8 36.00 6.20 -18 0 8 15.90 5.90 -18 0 8 17.80 5.40 -20 0 8 20.90 6.10 -20 0 8 16.20 5.50 -22 0 8 47.70 7.50 -22 0 8 55.69 7.50 -24 0 8 17.20 6.30 -24 0 8 27.70 6.50 -26 0 8 6.40 5.90 -26 0 8 6.50 5.60 -28 0 8 31.70 7.30 -28 0 8 23.20 6.60 -13 1 -8 8.50 8.30 -11 1 -8 14.00 8.10 -9 1 -8 20.00 8.20 -7 1 -8 0.60 7.40 -5 1 -8 11.60 7.50 -3 1 -8 17.50 7.20 -1 1 -8 13.50 7.30 1 -1 8 6.50 5.10 1 -1 8 11.80 4.50 1 1 -8 2.30 6.80 -1 -1 8 0.00 3.30 -1 -1 8 2.70 4.50 3 1 -8 12.30 7.00 -3 -1 8 5.90 4.80 -3 -1 8 13.20 3.80 -5 -1 8 -3.40 4.30 -5 -1 8 2.20 3.60 -7 -1 8 53.39 5.20 -7 -1 8 41.30 6.20 -9 -1 8 34.30 5.80 -9 -1 8 25.40 4.40 -9 -1 8 19.80 5.80 -11 -1 8 -2.90 4.80 -11 -1 8 1.60 4.20 -11 -1 8 -0.60 3.40 -13 -1 8 3.40 5.10 -13 -1 8 4.50 4.40 -15 -1 8 35.70 6.00 -15 -1 8 28.70 6.20 -17 -1 8 65.49 7.20 -17 -1 8 62.99 7.80 -19 -1 8 16.90 5.90 -19 -1 8 16.40 5.30 -21 -1 8 19.90 5.60 -21 -1 8 22.10 6.20 -23 -1 8 1.50 5.20 -23 -1 8 4.10 4.90 -25 -1 8 45.90 7.40 -25 -1 8 52.59 7.40 -27 -1 8 37.40 6.90 -27 -1 8 31.50 7.40 -29 -1 8 34.30 7.50 -29 -1 8 37.40 7.00 -12 2 -8 -6.50 7.70 -10 2 -8 13.50 8.10 -8 2 -8 12.70 7.90 8 -2 8 1.40 3.90 -6 2 -8 10.60 7.70 6 -2 8 10.10 4.20 -4 2 -8 62.49 9.20 4 -2 8 61.39 5.90 -2 2 -8 16.70 7.50 2 -2 8 17.10 4.30 0 2 -8 24.90 7.90 0 -2 8 13.00 4.80 0 -2 8 14.20 4.60 0 -2 8 21.00 4.30 2 2 -8 -0.40 6.50 -2 -2 8 0.90 4.10 -2 -2 8 2.50 4.20 -2 -2 8 -1.10 3.40 -4 -2 8 30.80 5.50 -4 -2 8 28.00 4.70 -4 -2 8 33.40 5.50 -6 -2 8 20.50 4.40 -6 -2 8 29.00 5.20 -6 -2 8 21.40 5.30 -8 -2 8 19.00 5.40 -8 -2 8 20.50 4.80 -8 -2 8 19.70 4.30 -10 -2 8 33.60 5.30 -10 -2 8 45.30 6.70 -10 -2 8 35.90 5.00 -12 -2 8 21.90 4.80 -12 -2 8 15.10 4.10 -12 -2 8 20.90 6.10 -14 -2 8 3.40 3.80 -14 -2 8 4.00 4.90 -16 -2 8 18.50 5.90 -16 -2 8 23.90 5.00 -18 -2 8 9.50 4.60 -18 -2 8 30.10 6.50 -20 -2 8 27.50 5.80 -20 -2 8 14.60 6.10 -22 -2 8 30.20 7.20 -22 -2 8 33.50 6.20 -24 -2 8 24.60 6.00 -24 -2 8 24.50 6.90 -26 -2 8 -0.50 5.10 -26 -2 8 -0.70 5.80 -9 3 -8 11.70 8.00 9 -3 8 21.70 5.40 -7 3 -8 2.70 8.00 7 -3 8 14.30 4.80 -5 3 -8 -3.90 7.20 5 -3 8 9.80 4.30 -3 3 -8 -0.40 6.90 3 -3 8 16.40 4.40 -1 3 -8 8.00 7.30 1 -3 8 12.30 4.10 1 -3 8 5.30 4.50 1 -3 8 9.00 4.10 1 3 -8 13.80 7.20 -1 -3 8 7.10 4.10 -1 -3 8 8.10 4.00 -1 -3 8 5.30 4.30 -3 -3 8 13.10 4.30 -3 -3 8 11.90 4.40 -3 -3 8 10.70 4.50 -5 -3 8 22.20 4.60 -5 -3 8 14.30 4.70 -5 -3 8 16.20 4.40 -7 -3 8 3.50 3.80 -7 -3 8 8.40 4.70 -7 -3 8 4.70 3.70 -9 -3 8 29.80 4.90 -9 -3 8 26.70 5.50 -9 -3 8 25.30 5.00 -11 -3 8 1.80 3.60 -11 -3 8 8.50 5.10 -11 -3 8 1.60 3.60 -13 -3 8 -0.20 3.50 -13 -3 8 6.70 3.90 -13 -3 8 5.40 5.20 -15 -3 8 16.60 4.40 -15 -3 8 12.50 5.90 -17 -3 8 30.90 7.00 -17 -3 8 39.20 5.60 -19 -3 8 55.29 8.20 -19 -3 8 59.79 6.50 -21 -3 8 4.60 4.20 -21 -3 8 4.40 5.90 -23 -3 8 12.10 6.40 -23 -3 8 17.80 5.30 -4 4 -8 4.30 7.50 -2 4 -8 50.09 9.10 2 -4 8 39.70 5.60 2 -4 8 37.20 6.40 0 4 -8 0.50 7.10 0 -4 8 14.00 4.90 0 -4 8 6.20 4.20 -2 -4 8 7.30 4.30 -2 -4 8 16.00 4.90 -4 -4 8 18.70 5.10 -4 -4 8 5.40 4.20 -6 -4 8 38.50 5.90 -6 -4 8 42.60 6.20 -6 -4 8 32.10 5.80 -8 -4 8 3.00 6.10 -8 -4 8 24.60 5.60 -8 -4 8 16.20 5.10 -10 -4 8 15.50 5.10 -10 -4 8 10.80 4.90 -12 -4 8 25.80 6.10 -12 -4 8 28.30 5.90 -14 -4 8 5.60 4.90 -14 -4 8 10.90 5.60 -16 -4 8 12.50 5.30 -16 -4 8 10.60 5.90 -18 -4 8 11.90 6.40 -5 3 9 24.60 7.10 -7 3 9 45.30 6.90 -7 3 9 37.50 7.70 -9 3 9 7.40 6.00 -9 3 9 3.10 5.40 -11 3 9 -4.20 5.20 -11 3 9 -2.50 5.60 -13 3 9 30.50 7.50 -13 3 9 42.60 6.80 2 2 9 12.20 6.20 0 2 9 5.10 5.80 -2 2 9 -0.60 5.50 -4 2 9 8.20 5.90 -6 2 9 32.90 6.90 -8 2 9 -7.90 5.00 -10 2 9 10.00 6.00 -12 2 9 7.90 5.80 -14 2 9 71.39 8.70 -16 2 9 12.90 6.10 -18 2 9 8.10 6.00 -20 2 9 23.80 6.60 -5 -1 -9 -6.40 7.60 5 1 9 -1.20 5.30 -3 -1 -9 23.60 8.30 3 1 9 -0.50 5.20 -1 -1 -9 73.59 10.30 1 1 9 66.39 8.50 -1 1 9 82.19 9.00 -3 1 9 23.80 6.70 -5 1 9 8.10 5.70 -7 1 9 66.29 8.20 -9 1 9 16.40 5.90 -11 1 9 5.30 5.50 -13 1 9 18.30 6.10 -15 1 9 32.00 6.80 -17 1 9 25.00 6.60 -17 1 9 24.90 6.50 -19 1 9 19.80 6.70 -19 1 9 26.40 6.70 -21 1 9 0.00 5.80 -21 1 9 3.70 5.50 -23 1 9 -0.40 5.70 -23 1 9 1.70 5.90 -6 0 -9 16.50 8.20 -4 0 -9 5.50 7.80 4 0 9 -1.80 5.10 -2 0 -9 -5.00 7.30 2 0 9 3.50 5.30 0 0 -9 1.00 7.80 0 0 9 -3.90 5.00 -2 0 9 -2.20 5.20 -4 0 9 26.70 6.60 -6 0 9 20.00 6.10 -8 0 9 -3.50 4.80 -10 0 9 7.30 5.40 -12 0 9 26.10 6.60 -14 0 9 69.19 8.70 -14 0 9 68.69 8.20 -16 0 9 0.00 5.50 -16 0 9 1.30 5.20 -18 0 9 12.30 6.00 -18 0 9 9.60 5.50 -20 0 9 36.80 7.10 -20 0 9 19.80 6.70 -22 0 9 17.50 6.40 -22 0 9 21.00 6.70 -5 1 -9 3.30 7.80 -3 1 -9 -4.50 7.40 3 -1 9 4.00 5.20 -1 1 -9 76.69 10.40 1 -1 9 72.09 8.20 1 1 -9 82.29 10.50 -1 -1 9 77.79 8.60 -3 -1 9 19.40 5.90 -5 -1 9 7.30 5.10 -7 -1 9 69.69 8.10 -7 -1 9 61.49 8.00 -9 -1 9 8.20 5.50 -9 -1 9 14.30 6.10 -11 -1 9 5.40 5.70 -11 -1 9 3.70 5.40 -13 -1 9 19.50 6.30 -13 -1 9 24.30 6.20 -15 -1 9 48.30 7.20 -15 -1 9 39.80 7.30 -17 -1 9 29.20 7.10 -17 -1 9 31.70 6.60 -19 -1 9 36.70 7.20 -19 -1 9 31.00 6.50 -21 -1 9 -3.30 5.50 -21 -1 9 10.90 5.40 -23 -1 9 3.00 5.80 -23 -1 9 2.10 5.20 -2 2 -9 -7.80 7.60 2 -2 9 1.20 4.70 2 -2 9 1.50 4.30 0 2 -9 -5.70 7.60 0 -2 9 6.10 5.00 0 -2 9 12.00 4.90 -2 -2 9 4.00 4.80 -2 -2 9 5.40 4.60 -4 -2 9 17.90 5.40 -4 -2 9 20.70 5.60 -6 -2 9 31.40 6.20 -6 -2 9 23.30 5.40 -8 -2 9 4.20 4.20 -8 -2 9 0.20 4.90 -10 -2 9 5.20 5.40 -10 -2 9 2.20 4.20 -10 -2 9 12.60 4.90 -12 -2 9 13.30 6.00 -12 -2 9 12.60 5.00 -12 -2 9 13.30 4.80 -14 -2 9 69.59 6.80 -14 -2 9 66.29 8.30 -14 -2 9 71.29 7.60 -16 -2 9 14.50 5.20 -16 -2 9 5.50 5.70 -16 -2 9 17.20 4.70 -18 -2 9 19.80 5.50 -18 -2 9 13.40 6.40 -20 -2 9 30.00 6.30 -20 -2 9 32.50 7.30 -3 -3 9 51.39 7.10 -5 -3 9 17.70 4.80 -5 -3 9 18.30 5.40 -5 -3 9 12.30 4.60 -7 -3 9 26.20 5.80 -7 -3 9 30.10 5.50 -7 -3 9 31.30 5.60 -9 -3 9 8.60 4.50 -9 -3 9 10.40 4.40 -9 -3 9 9.10 5.20 -11 -3 9 2.60 4.10 -11 -3 9 0.40 5.10 -11 -3 9 -0.70 3.90 -13 -3 9 34.80 7.10 -13 -3 9 45.00 6.30 -13 -3 9 53.69 6.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 1504 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn Cl1 Cl 0.19612(3) 0.75307(17) 0.53512(13) 0.0150(3) Uani 1 1 d . O1 O 0.35810(10) 0.8070(5) 0.2123(4) 0.0158(8) Uani 1 1 d . O3 O 0.15881(9) 0.7537(7) 0.1701(4) 0.0193(7) Uani 1 1 d . H3 H 0.1492 0.7235 0.0666 0.029 Uiso 1 1 calc GR O5 O 0.37754(10) 0.2089(5) 0.1620(4) 0.0197(9) Uani 1 1 d . H5 H 0.3757 0.0906 0.1953 0.030 Uiso 1 1 calc GR O4 O 0.40782(11) 0.3655(5) 0.6738(4) 0.0187(8) Uani 1 1 d . H4 H 0.3833 0.3259 0.6763 0.028 Uiso 1 1 calc GR O2 O 0.28748(10) 0.7692(7) -0.0168(4) 0.0190(7) Uani 1 1 d . H2 H 0.3138 0.7575 0.0232 0.029 Uiso 1 1 calc GR N1 N 0.35655(11) 0.7780(7) 0.4934(5) 0.0132(8) Uani 1 1 d . N2 N 0.40115(12) 0.8064(5) 0.5472(5) 0.0121(9) Uani 1 1 d . C5 C 0.20219(13) 0.7572(9) 0.2052(5) 0.0143(9) Uani 1 1 d . C7 C 0.26905(13) 0.7608(9) 0.4207(5) 0.0123(8) Uani 1 1 d . C3 C 0.26728(14) 0.7658(9) 0.1132(5) 0.0148(9) Uani 1 1 d . C2 C 0.29078(13) 0.7675(9) 0.2862(5) 0.0127(9) Uani 1 1 d . C4 C 0.22379(14) 0.7623(9) 0.0735(5) 0.0154(9) Uani 1 1 d . H4A H 0.2084 0.7634 -0.0430 0.018 Uiso 1 1 calc R C1 C 0.33640(15) 0.7847(7) 0.3249(5) 0.0143(10) Uani 1 1 d . C8 C 0.29367(13) 0.7588(9) 0.5952(5) 0.0127(9) Uani 1 1 d . H8 H 0.2797 0.7517 0.6870 0.015 Uiso 1 1 calc R C6 C 0.22433(13) 0.7557(9) 0.3747(5) 0.0135(9) Uani 1 1 d . C13 C 0.46794(15) 0.6657(8) 0.6567(6) 0.0189(11) Uani 1 1 d . H13A H 0.4836 0.5378 0.6828 0.023 Uiso 1 1 calc R H13B H 0.4871 0.7668 0.6244 0.023 Uiso 1 1 calc R C17 C 0.42049(14) 0.2798(9) 0.2234(6) 0.0165(10) Uani 1 1 d . H17 H 0.4219 0.4217 0.1847 0.020 Uiso 1 1 calc R C11 C 0.40957(16) 0.8444(7) 0.7359(6) 0.0164(11) Uani 1 1 d . H11 H 0.4132 0.9916 0.7578 0.020 Uiso 1 1 calc R C16 C 0.43263(14) 0.2757(9) 0.4194(6) 0.0182(10) Uani 1 1 d . H16A H 0.4635 0.3032 0.4590 0.022 Uiso 1 1 calc R H16B H 0.4274 0.1395 0.4588 0.022 Uiso 1 1 calc R C10 C 0.36992(13) 0.7713(9) 0.7927(5) 0.0145(9) Uani 1 1 d . H10A H 0.3745 0.6362 0.8449 0.017 Uiso 1 1 calc R H10B H 0.3622 0.8650 0.8762 0.017 Uiso 1 1 calc R C9 C 0.33638(14) 0.7669(9) 0.6289(5) 0.0129(9) Uani 1 1 d . C12 C 0.45188(14) 0.7374(9) 0.8119(6) 0.0181(10) Uani 1 1 d . H12A H 0.4725 0.8308 0.8831 0.022 Uiso 1 1 calc R H12B H 0.4475 0.6224 0.8837 0.022 Uiso 1 1 calc R C14 C 0.42792(14) 0.6371(7) 0.5108(6) 0.0139(11) Uani 1 1 d . H14 H 0.4356 0.6644 0.3992 0.017 Uiso 1 1 calc R C15 C 0.40820(17) 0.4272(7) 0.5023(6) 0.0151(11) Uani 1 1 d . H15 H 0.3782 0.4342 0.4328 0.018 Uiso 1 1 calc R C18 C 0.45072(18) 0.1542(9) 0.1470(7) 0.0287(13) Uani 1 1 d . H18A H 0.4498 0.0147 0.1842 0.043 Uiso 1 1 calc GR H18B H 0.4797 0.2063 0.1861 0.043 Uiso 1 1 calc GR H18C H 0.4421 0.1608 0.0215 0.043 Uiso 1 1 calc GR 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 Cl1 0.0172(5) 0.0176(6) 0.0118(5) -0.0001(6) 0.0065(4) 0.0003(6) O1 0.0190(17) 0.019(2) 0.0122(17) 0.0009(14) 0.0095(14) -0.0010(13) O3 0.0170(16) 0.0274(18) 0.0127(15) -0.001(2) 0.0017(12) 0.001(2) O5 0.0205(18) 0.022(2) 0.0142(18) 0.0000(15) 0.0000(14) -0.0036(14) O4 0.022(2) 0.0223(19) 0.0133(19) 0.0001(15) 0.0076(15) -0.0046(16) O2 0.0189(16) 0.0302(19) 0.0094(14) -0.001(2) 0.0062(12) -0.003(2) N1 0.0139(18) 0.016(2) 0.0105(18) -0.0001(19) 0.0046(15) 0.000(2) N2 0.012(2) 0.012(2) 0.012(2) -0.0019(15) 0.0025(16) -0.0035(15) C5 0.014(2) 0.012(2) 0.016(2) -0.002(3) 0.0024(17) 0.001(3) C7 0.017(2) 0.0081(19) 0.011(2) -0.001(2) 0.0032(17) 0.001(3) C3 0.022(2) 0.014(2) 0.009(2) 0.001(3) 0.0067(18) -0.001(3) C2 0.016(2) 0.012(2) 0.011(2) -0.002(2) 0.0056(17) -0.002(3) C4 0.020(2) 0.017(2) 0.009(2) 0.004(3) 0.0023(17) 0.004(3) C1 0.022(2) 0.011(3) 0.009(2) 0.001(2) 0.0028(19) -0.003(2) C8 0.018(2) 0.012(2) 0.010(2) -0.001(2) 0.0056(17) -0.001(3) C6 0.020(2) 0.010(2) 0.013(2) 0.003(3) 0.0088(18) 0.001(3) C13 0.015(3) 0.021(3) 0.020(3) -0.003(2) 0.003(2) -0.002(2) C17 0.017(2) 0.016(3) 0.015(2) -0.004(2) 0.0014(18) -0.004(2) C11 0.017(3) 0.017(2) 0.014(3) -0.004(2) 0.004(2) -0.006(2) C16 0.017(2) 0.016(2) 0.022(2) -0.004(2) 0.0056(19) -0.001(2) C10 0.018(2) 0.015(2) 0.011(2) -0.003(2) 0.0049(18) -0.001(3) C9 0.022(2) 0.011(2) 0.008(2) 0.003(2) 0.0082(18) 0.001(3) C12 0.019(2) 0.021(3) 0.013(2) -0.004(2) 0.0029(18) 0.002(3) C14 0.015(3) 0.014(2) 0.013(3) -0.003(2) 0.005(2) -0.001(2) C15 0.021(3) 0.015(2) 0.011(3) -0.002(2) 0.006(2) -0.001(2) C18 0.027(3) 0.038(3) 0.024(3) -0.010(3) 0.011(3) 0.004(3) 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' Cl Cl 0.1484 0.1585 '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 C5 O3 H3 109.5 C17 O5 H5 109.5 C15 O4 H4 109.5 C3 O2 H2 109.5 C1 N1 N2 121.0(3) C1 N1 C9 125.1(4) C9 N1 N2 113.5(3) N1 N2 C11 105.1(3) N1 N2 C14 115.8(4) C14 N2 C11 110.5(4) O3 C5 C4 121.1(4) O3 C5 C6 118.3(4) C6 C5 C4 120.6(4) C2 C7 C8 118.6(4) C6 C7 C2 117.7(4) C6 C7 C8 123.7(4) O2 C3 C2 120.5(4) O2 C3 C4 118.5(4) C4 C3 C2 121.0(4) C7 C2 C1 120.3(4) C3 C2 C7 119.7(4) C3 C2 C1 119.9(4) C5 C4 H4A 120.2 C3 C4 C5 119.6(4) C3 C4 H4A 120.2 O1 C1 N1 119.6(4) O1 C1 C2 124.3(4) N1 C1 C2 116.1(4) C7 C8 H8 119.9 C9 C8 C7 120.2(4) C9 C8 H8 119.9 C5 C6 Cl1 119.1(3) C5 C6 C7 121.5(4) C7 C6 Cl1 119.4(3) H13A C13 H13B 108.7 C12 C13 H13A 110.6 C12 C13 H13B 110.6 C12 C13 C14 105.7(4) C14 C13 H13A 110.6 C14 C13 H13B 110.6 O5 C17 H17 108.4 O5 C17 C16 109.8(4) O5 C17 C18 110.0(4) C16 C17 H17 108.4 C18 C17 H17 108.4 C18 C17 C16 111.7(4) N2 C11 H11 109.3 N2 C11 C10 106.2(4) N2 C11 C12 104.8(4) C10 C11 H11 109.3 C12 C11 H11 109.3 C12 C11 C10 117.5(4) C17 C16 H16A 108.8 C17 C16 H16B 108.8 C17 C16 C15 113.7(4) H16A C16 H16B 107.7 C15 C16 H16A 108.8 C15 C16 H16B 108.8 C11 C10 H10A 111.1 C11 C10 H10B 111.1 H10A C10 H10B 109.1 C9 C10 C11 103.3(4) C9 C10 H10A 111.1 C9 C10 H10B 111.1 N1 C9 C10 107.9(4) C8 C9 N1 119.5(4) C8 C9 C10 132.6(4) C13 C12 C11 105.3(4) C13 C12 H12A 110.7 C13 C12 H12B 110.7 C11 C12 H12A 110.7 C11 C12 H12B 110.7 H12A C12 H12B 108.8 N2 C14 C13 100.4(4) N2 C14 H14 108.4 N2 C14 C15 116.4(4) C13 C14 H14 108.4 C15 C14 C13 114.4(4) C15 C14 H14 108.4 O4 C15 C16 110.4(4) O4 C15 C14 108.4(4) O4 C15 H15 108.7 C16 C15 C14 111.8(4) C16 C15 H15 108.7 C14 C15 H15 108.7 C17 C18 H18A 109.5 C17 C18 H18B 109.5 C17 C18 H18C 109.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl1 C6 1.743(4) O1 C1 1.275(5) O3 H3 0.8400 O3 C5 1.365(5) O5 H5 0.8400 O5 C17 1.441(6) O4 H4 0.8400 O4 C15 1.437(6) O2 H2 0.8400 O2 C3 1.354(5) N1 N2 1.418(5) N1 C1 1.356(6) N1 C9 1.395(5) N2 C11 1.494(6) N2 C14 1.493(6) C5 C4 1.397(6) C5 C6 1.379(6) C7 C2 1.420(5) C7 C8 1.438(6) C7 C6 1.407(6) C3 C2 1.416(6) C3 C4 1.368(6) C2 C1 1.439(6) C4 H4A 0.9500 C8 H8 0.9500 C8 C9 1.345(6) C13 H13A 0.9900 C13 H13B 0.9900 C13 C12 1.533(6) C13 C14 1.539(6) C17 H17 1.0000 C17 C16 1.528(6) C17 C18 1.521(7) C11 H11 1.0000 C11 C10 1.538(6) C11 C12 1.537(7) C16 H16A 0.9900 C16 H16B 0.9900 C16 C15 1.528(7) C10 H10A 0.9900 C10 H10B 0.9900 C10 C9 1.494(6) C12 H12A 0.9900 C12 H12B 0.9900 C14 H14 1.0000 C14 C15 1.534(7) C15 H15 1.0000 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800