#------------------------------------------------------------------------------ #$Date: 2019-10-29 02:26:27 +0200 (Tue, 29 Oct 2019) $ #$Revision: 220329 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/24/1552499.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_1552499 loop_ _publ_author_name 'Gu, Han' 'Ghosh, Saptarshi' 'Staples, Richard J.' 'Bane, Susan L.' _publ_section_title ; \b-Hydroxy-Stabilized Boron-Nitrogen Heterocycles Enable Rapid and Efficient C-Terminal Protein Modification. ; _journal_issue 10 _journal_name_full 'Bioconjugate chemistry' _journal_page_first 2604 _journal_page_last 2613 _journal_paper_doi 10.1021/acs.bioconjchem.9b00534 _journal_volume 30 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_moiety 'C18 H16 B N3 O4' _chemical_formula_sum 'C18 H16 B N3 O4' _chemical_formula_weight 349.15 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2018-12-17 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 92.8770(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.20330(10) _cell_length_b 8.90940(10) _cell_length_c 16.9484(2) _cell_measurement_reflns_used 9967 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 70.04 _cell_measurement_theta_min 2.61 _cell_volume 1689.57(3) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'COSMO (BRUKER, V1.61, 2009)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)' _computing_structure_solution 'SHELXT (Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 8.36 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w and \f' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_unetI/netI 0.0281 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 18758 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 70.068 _diffrn_reflns_theta_min 2.610 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_T_max 0.7533 _exptl_absorpt_correction_T_min 0.6686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0642 before and 0.0499 after correction. The Ratio of minimum to maximum transmission is 0.8876. The \l/2 correction factor is 0.0015.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.373 _exptl_crystal_description needle _exptl_crystal_F_000 728 _exptl_crystal_recrystallization_method 'Used as received' _exptl_crystal_size_max 0.502 _exptl_crystal_size_mid 0.224 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.852 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.059 _refine_ls_abs_structure_details ; Flack x determined using 2375 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.05(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 477 _refine_ls_number_reflns 6315 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0559 _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^)+(0.1011P)^2^+0.7355P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1581 _refine_ls_wR_factor_ref 0.1656 _reflns_Friedel_coverage 0.842 _reflns_Friedel_fraction_full 0.972 _reflns_Friedel_fraction_max 0.963 _reflns_number_gt 5751 _reflns_number_total 6315 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bc9b00534_si_002.cif _cod_data_source_block jh1218a _cod_database_code 1552499 _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 0.968 _shelx_estimated_absorpt_t_min 0.688 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Ternary CH refined with riding coordinates: C2A(H2A), C2B(H2B) 2.b Secondary CH2 refined with riding coordinates: C3A(H3AA,H3AB), C12A(H12A,H12B), C3B(H3BA,H3BB), C12B(H12C,H12D) 2.c Aromatic/amide H refined with riding coordinates: C4A(H4A), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A), C4B(H4B), C7B(H7B), C8B(H8B), C9B(H9B), C10B(H10B), C14B(H14B), C15B(H15B), C16B(H16B), C17B(H17B), C18B(H18B) ; _shelx_res_file ; TITL jh1218a_a.res in P2(1) jh1218a.res created by SHELXL-2018/3 at 09:29:15 on 17-Dec-2018 REM Old TITL JH1218a in P2(1) REM SHELXT solution in P2(1): R1 0.137, Rweak 0.016, Alpha 0.002 REM 0.308 for 5 systematic absences, Orientation as input REM Flack x = -0.051 ( 0.085 ) from 2481 Parsons' quotients REM Formula found by SHELXT: C38 N6 O8 CELL 1.54178 11.2033 8.9094 16.9484 90 92.877 90 ZERR 4 0.0001 0.0001 0.0002 0 0.001 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H B N O UNIT 72 64 4 12 16 EQIV $1 -X,0.5+Y,-Z EQIV $2 1-X,-0.5+Y,1-Z L.S. 16 PLAN 20 SIZE 0.04 0.224 0.502 TEMP -100(2) HTAB N3B N2B_$1 HTAB C3B O4B HTAB N3A N2A_$2 BOND $H CONF fmap 2 53 acta REM REM REM WGHT 0.101100 0.735500 FVAR 0.51916 O1A 5 0.494468 0.352750 0.499428 11.00000 0.03524 0.05836 = 0.04582 -0.01399 -0.00611 -0.00094 O2A 5 0.351898 0.141052 0.302470 11.00000 0.03236 0.03586 = 0.04660 -0.00717 -0.00816 0.00213 O3A 5 0.837793 0.120059 0.418282 11.00000 0.02616 0.05202 = 0.04520 0.01795 0.00565 0.00559 O4A 5 0.745017 0.247304 0.317509 11.00000 0.03639 0.08620 = 0.05870 0.03527 0.01151 0.01260 N1A 4 0.346965 0.342464 0.400789 11.00000 0.02604 0.03319 = 0.03735 -0.00236 0.00403 -0.00234 N2A 4 0.289872 0.460911 0.436770 11.00000 0.03117 0.03645 = 0.03943 -0.00555 0.00459 -0.00121 N3A 4 0.641006 0.153998 0.417293 11.00000 0.02589 0.03888 = 0.03826 0.00735 -0.00096 -0.00168 H3A 2 0.646193 0.097859 0.456059 11.00000 0.04938 C1A 1 0.458627 0.305853 0.436418 11.00000 0.02852 0.03196 = 0.03937 -0.00119 0.00000 -0.00668 C2A 1 0.530013 0.207403 0.382241 11.00000 0.02637 0.03312 = 0.03733 0.00283 0.00056 -0.00122 AFIX 13 H2A 2 0.551249 0.272976 0.337158 11.00000 -1.20000 AFIX 0 C3A 1 0.453581 0.080256 0.346049 11.00000 0.03506 0.03456 = 0.04516 -0.00354 -0.00470 0.00085 AFIX 23 H3AA 2 0.501819 0.019621 0.310476 11.00000 -1.20000 H3AB 2 0.426611 0.013833 0.388465 11.00000 -1.20000 AFIX 0 C4A 1 0.191558 0.507704 0.403030 11.00000 0.03259 0.03841 = 0.04240 -0.00097 0.00708 0.00112 AFIX 43 H4A 2 0.152674 0.587590 0.428562 11.00000 -1.20000 AFIX 0 C5A 1 0.132695 0.452078 0.329853 11.00000 0.03066 0.03768 = 0.03817 0.00920 0.00467 -0.00064 C6A 1 0.182798 0.330876 0.291414 11.00000 0.02844 0.03737 = 0.03602 0.00475 0.00357 -0.00443 C7A 1 0.126059 0.277341 0.221249 11.00000 0.03266 0.04627 = 0.03946 0.00500 -0.00274 -0.00346 AFIX 43 H7A 2 0.158741 0.194359 0.194522 11.00000 -1.20000 AFIX 0 C8A 1 0.022488 0.345352 0.190936 11.00000 0.04336 0.05711 = 0.03760 0.00735 -0.00720 -0.00776 AFIX 43 H8A 2 -0.014449 0.309927 0.142801 11.00000 -1.20000 AFIX 0 C9A 1 -0.027550 0.463577 0.229681 11.00000 0.03691 0.05916 = 0.05084 0.02110 -0.00620 0.00706 AFIX 43 H9A 2 -0.099545 0.507795 0.208787 11.00000 -1.20000 AFIX 0 C10A 1 0.026814 0.518498 0.299222 11.00000 0.03685 0.04445 = 0.04927 0.01155 0.00418 0.00681 AFIX 43 H10A 2 -0.007492 0.600491 0.325854 11.00000 -1.20000 AFIX 0 C11A 1 0.740569 0.178572 0.379043 11.00000 0.03259 0.04245 = 0.03825 0.00661 0.00390 0.00209 C12A 1 0.946905 0.142590 0.378724 11.00000 0.03212 0.15215 = 0.07521 0.06529 0.01986 0.02872 AFIX 23 H12A 2 0.952152 0.248117 0.360934 11.00000 -1.20000 H12B 2 0.948158 0.076801 0.331699 11.00000 -1.20000 AFIX 0 C13A 1 1.051610 0.106326 0.434928 11.00000 0.02982 0.07049 = 0.05777 0.03056 0.01707 0.00666 C14A 1 1.081741 0.200730 0.497971 11.00000 0.05512 0.05472 = 0.08667 0.01639 0.03845 0.01751 AFIX 43 H14A 2 1.035151 0.287567 0.507010 11.00000 -1.20000 AFIX 0 C15A 1 1.180606 0.167360 0.547832 11.00000 0.05904 0.06574 = 0.06560 -0.01248 0.02079 -0.01270 AFIX 43 H15A 2 1.201823 0.231634 0.591011 11.00000 -1.20000 AFIX 0 C16A 1 1.248159 0.040349 0.534523 11.00000 0.03062 0.06345 = 0.05106 0.00695 -0.00156 -0.00264 AFIX 43 H16A 2 1.314696 0.016153 0.569142 11.00000 -1.20000 AFIX 0 C17A 1 1.218723 -0.049321 0.471731 11.00000 0.03720 0.04802 = 0.05222 0.01091 0.00292 0.00231 AFIX 43 H17A 2 1.265972 -0.135270 0.462008 11.00000 -1.20000 AFIX 0 C18A 1 1.120880 -0.016920 0.421878 11.00000 0.03311 0.05889 = 0.04483 0.00982 0.00032 -0.00784 AFIX 43 H18A 2 1.101463 -0.080660 0.378166 11.00000 -1.20000 AFIX 0 B1A 3 0.297410 0.264626 0.330928 11.00000 0.02881 0.03502 = 0.03688 0.00257 0.00219 -0.00610 O1B 5 -0.004843 0.670818 0.013598 11.00000 0.04400 0.05584 = 0.04031 -0.00853 -0.00512 -0.00244 O2B 5 0.139507 0.856061 0.219338 11.00000 0.04187 0.04002 = 0.03816 -0.01026 -0.00606 -0.00145 O3B 5 -0.321725 0.886504 0.076872 11.00000 0.03737 0.05606 = 0.05341 0.02417 0.00338 -0.00169 O4B 5 -0.208319 0.733198 0.156426 11.00000 0.04536 0.05004 = 0.05827 0.02415 -0.00655 -0.00459 N1B 4 0.147305 0.679310 0.109415 11.00000 0.03701 0.03141 = 0.03293 -0.00214 0.00128 -0.00423 N2B 4 0.201637 0.560849 0.070261 11.00000 0.04110 0.03837 = 0.03477 -0.00802 0.00148 -0.00124 N3B 4 -0.124418 0.912148 0.081122 11.00000 0.04253 0.04115 = 0.03903 0.01490 0.00243 0.00212 H3B 2 -0.135430 0.962418 0.047019 11.00000 0.03123 C1B 1 0.042153 0.730707 0.071112 11.00000 0.03483 0.03729 = 0.03121 0.00133 0.00258 -0.00673 C2B 1 -0.001257 0.879088 0.104321 11.00000 0.03572 0.03579 = 0.03935 0.00318 0.00020 -0.00476 AFIX 13 H2B 2 0.047958 0.959701 0.080857 11.00000 -1.20000 AFIX 0 C3B 1 0.019407 0.891788 0.194170 11.00000 0.04169 0.03817 = 0.04373 -0.00440 -0.00195 0.00307 AFIX 23 H3BA 2 0.001011 0.995381 0.210852 11.00000 -1.20000 H3BB 2 -0.035775 0.822881 0.220137 11.00000 -1.20000 AFIX 0 C4B 1 0.300816 0.509779 0.101320 11.00000 0.04586 0.03822 = 0.03284 -0.00373 0.00571 0.00279 AFIX 43 H4B 2 0.336342 0.429523 0.074006 11.00000 -1.20000 AFIX 0 C5B 1 0.364378 0.560005 0.172690 11.00000 0.03742 0.03502 = 0.03358 0.00248 0.00364 -0.00489 C6B 1 0.315778 0.677718 0.215753 11.00000 0.03585 0.03347 = 0.03425 0.00342 0.00367 -0.00709 C7B 1 0.375611 0.725402 0.285187 11.00000 0.04485 0.03872 = 0.03456 -0.00214 -0.00091 -0.00715 AFIX 43 H7B 2 0.341596 0.801898 0.316005 11.00000 -1.20000 AFIX 0 C8B 1 0.483982 0.662700 0.309809 11.00000 0.04597 0.04527 = 0.04082 0.00514 -0.00463 -0.00859 AFIX 43 H8B 2 0.524678 0.697419 0.356842 11.00000 -1.20000 AFIX 0 C9B 1 0.533831 0.548266 0.265625 11.00000 0.04459 0.04315 = 0.04199 0.01265 -0.00362 -0.00447 AFIX 43 H9B 2 0.609089 0.506785 0.282185 11.00000 -1.20000 AFIX 0 C10B 1 0.474050 0.495211 0.197922 11.00000 0.04570 0.03793 = 0.03938 0.00693 0.00393 0.00052 AFIX 43 H10B 2 0.506886 0.415564 0.168697 11.00000 -1.20000 AFIX 0 C11B 1 -0.216636 0.833853 0.108863 11.00000 0.03945 0.03657 = 0.04566 0.00638 0.00135 0.00307 C12B 1 -0.425798 0.811535 0.106639 11.00000 0.03957 0.07691 = 0.08009 0.04370 0.00151 -0.00344 AFIX 23 H12C 2 -0.427419 0.825297 0.164538 11.00000 -1.20000 H12D 2 -0.422146 0.702629 0.095415 11.00000 -1.20000 AFIX 0 C13B 1 -0.535154 0.877438 0.067146 11.00000 0.03812 0.06275 = 0.06750 0.03598 0.02293 0.01353 C14B 1 -0.582517 0.806054 -0.000130 11.00000 0.04594 0.12337 = 0.07843 0.02965 0.01352 0.00213 AFIX 43 H14B 2 -0.538770 0.722156 -0.017722 11.00000 -1.20000 AFIX 0 C15B 1 -0.683325 0.840843 -0.043959 11.00000 0.06694 0.10727 = 0.08434 0.00716 0.01588 -0.00447 AFIX 43 H15B 2 -0.710803 0.782638 -0.088190 11.00000 -1.20000 AFIX 0 C16B 1 -0.740969 0.962169 -0.020639 11.00000 0.08379 0.07251 = 0.08706 0.02451 0.03004 0.00848 AFIX 43 H16B 2 -0.810733 0.991277 -0.050997 11.00000 -1.20000 AFIX 0 C17B 1 -0.707640 1.049233 0.044106 11.00000 0.03950 0.06337 = 0.08482 0.01870 0.01920 0.00822 AFIX 43 H17B 2 -0.750781 1.136601 0.057553 11.00000 -1.20000 AFIX 0 C18B 1 -0.599918 0.997831 0.091588 11.00000 0.08547 0.06778 = 0.10504 0.01699 0.04482 -0.00173 AFIX 43 H18B 2 -0.575959 1.048698 0.139038 11.00000 -1.20000 AFIX 0 B1B 3 0.197062 0.743973 0.182604 11.00000 0.04001 0.03241 = 0.03172 -0.00188 0.00305 -0.00797 HKLF 4 REM jh1218a_a.res in P2(1) REM wR2 = 0.1656, GooF = S = 1.037, Restrained GooF = 1.037 for all data REM R1 = 0.0559 for 5751 Fo > 4sig(Fo) and 0.0611 for all 6315 data REM 477 parameters refined using 1 restraints END WGHT 0.1011 0.7355 REM Highest difference peak 0.852, deepest hole -0.296, 1-sigma level 0.059 Q1 1 -0.6425 1.1022 0.1149 11.00000 0.05 0.85 Q2 1 -0.6549 0.6996 -0.1656 11.00000 0.05 0.82 Q3 1 -0.5414 1.0183 0.1337 11.00000 0.05 0.67 Q4 1 1.1396 -0.0911 0.3832 11.00000 0.05 0.32 Q5 1 1.1478 0.3236 0.6728 11.00000 0.05 0.31 Q6 1 -0.5970 0.8998 0.0095 11.00000 0.05 0.27 Q7 1 -0.6650 0.9600 -0.0107 11.00000 0.05 0.26 Q8 1 0.2559 0.7048 0.2024 11.00000 0.05 0.25 Q9 1 1.0420 0.0076 0.3670 11.00000 0.05 0.18 Q10 1 0.2467 0.3133 0.2983 11.00000 0.05 0.18 Q11 1 -0.4291 0.8862 0.1775 11.00000 0.05 0.16 Q12 1 -0.6963 0.9721 -0.1404 11.00000 0.05 0.16 Q13 1 0.1779 0.2563 0.1748 11.00000 0.05 0.16 Q14 1 -0.1369 0.2179 0.1397 11.00000 0.05 0.16 Q15 1 0.3156 0.5972 0.2034 11.00000 0.05 0.16 Q16 1 0.9404 0.2434 0.4076 11.00000 0.05 0.16 Q17 1 0.3505 0.7240 0.2344 11.00000 0.05 0.15 Q18 1 0.1457 0.2838 0.2641 11.00000 0.05 0.15 Q19 1 0.4395 0.5490 0.1729 11.00000 0.05 0.15 Q20 1 0.6627 0.5358 0.1781 11.00000 0.05 0.14 ; _shelx_res_checksum 72252 _shelx_hkl_file ; -1 0 0 8.20 0.40 1 0 0 8.40 0.40 2 0 0 4.50 0.50 -2 0 0 4.80 0.50 3 0 0 -1.10 0.40 -3 0 0 -0.60 0.50 4 0 0 525.15 11.60 -4 0 0 529.15 11.90 5 0 0 6.50 0.90 -5 0 0 8.70 1.00 -6 0 0 1239.58 27.40 6 0 0 1261.07 26.90 -7 0 0 18.50 1.60 7 0 0 18.10 1.50 -8 0 0 22.00 1.40 -8 0 0 22.70 1.90 8 0 0 20.50 1.70 9 0 0 16.60 2.00 9 0 0 18.20 2.10 -9 0 0 16.00 1.30 9 0 0 16.10 1.90 9 0 0 18.80 1.90 10 0 0 15.60 1.70 10 0 0 13.90 1.70 10 0 0 15.20 2.00 10 0 0 14.80 2.20 -10 0 0 15.40 1.30 -11 0 0 2.00 1.00 11 0 0 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110.09 4.50 7 4 -3 89.29 4.50 -7 4 3 120.39 4.30 -7 4 3 118.59 4.20 6 -4 -3 4.00 1.00 -6 4 3 3.40 0.90 -5 -4 3 88.69 3.50 5 -4 -3 82.09 3.40 -5 4 3 89.09 3.40 4 -4 -3 73.59 2.60 4 -4 -3 70.39 2.90 4 4 -3 65.49 2.50 -4 4 3 73.89 2.90 4 4 -3 74.49 3.00 3 -4 -3 7.50 1.10 3 -4 -3 4.90 0.70 -3 -4 3 6.00 0.80 -3 4 3 7.20 1.00 3 4 -3 5.40 0.90 3 4 -3 7.60 1.10 -2 -4 3 622.44 14.10 2 -4 -3 635.24 14.50 2 -4 -3 655.23 14.10 2 4 -3 644.04 14.70 2 4 -3 661.43 14.10 1 -4 -3 754.22 16.00 -1 -4 3 740.73 16.10 1 -4 -3 733.13 16.40 1 4 -3 740.63 16.00 1 4 -3 745.43 16.70 0 -4 -3 6.10 0.90 0 -4 3 5.00 0.80 0 -4 -3 4.60 0.80 0 4 -3 6.30 0.90 0 4 -3 6.20 0.90 -1 -4 -3 275.07 7.10 -1 -4 -3 282.47 6.90 1 -4 3 287.77 7.00 -1 4 -3 289.47 7.30 -1 4 -3 284.87 6.90 -2 -4 -3 13.70 1.10 2 -4 3 11.40 1.10 -2 4 -3 13.60 1.10 -2 4 -3 12.20 1.20 2 4 3 10.20 1.10 -3 -4 -3 35.70 1.80 3 -4 3 36.50 1.90 -3 4 -3 34.00 1.90 -3 4 -3 35.00 1.70 3 4 3 35.60 1.80 4 -4 3 7.00 1.10 -4 -4 -3 5.80 0.90 -4 4 -3 4.80 0.90 -4 4 -3 7.40 0.90 4 4 3 6.30 1.00 5 -4 3 38.00 2.30 -5 4 -3 38.50 2.20 5 4 3 42.80 2.30 6 -4 3 1.10 0.80 6 4 3 -0.40 0.60 -6 4 -3 1.30 0.60 7 -4 3 20.70 2.10 7 4 3 20.30 1.90 7 4 3 23.70 2.00 7 4 3 21.40 2.00 -7 4 -3 20.90 2.00 -7 4 -3 20.30 1.90 8 -4 3 10.90 1.80 -8 4 -3 11.00 1.40 -8 4 -3 13.30 1.60 8 4 3 13.70 1.90 8 4 3 10.50 1.70 8 4 3 13.70 1.70 8 4 3 14.70 1.80 9 -4 3 5.30 1.40 9 4 3 10.60 1.80 9 4 3 12.90 1.80 -9 4 -3 6.80 1.20 9 4 3 9.30 1.50 -9 4 -3 8.40 1.40 -10 -4 -3 50.29 2.10 10 -4 3 51.29 3.00 10 4 3 50.29 2.80 -10 4 -3 44.10 2.60 10 4 3 49.80 2.80 10 4 3 55.79 3.00 11 -4 3 10.50 1.60 -11 -4 -3 12.60 1.00 11 4 3 12.70 1.60 11 4 3 10.80 1.20 -11 4 -3 9.60 1.10 11 4 3 8.30 1.10 -12 -4 -3 5.80 0.70 12 -4 3 3.40 0.70 12 4 3 3.00 0.70 -12 4 -3 4.90 0.80 12 4 3 3.20 0.70 12 4 3 4.40 0.80 12 -5 -3 2.40 0.50 -12 5 3 3.30 0.60 11 -5 -3 0.80 0.60 11 5 -3 2.00 0.70 -11 5 3 0.70 0.50 -11 5 3 0.20 0.60 10 -5 -3 19.10 1.90 10 -5 -3 14.00 1.60 -10 5 3 17.70 1.40 10 5 -3 19.30 1.80 -10 5 3 17.00 1.60 9 -5 -3 4.00 1.20 9 -5 -3 5.90 1.30 -9 5 3 5.90 1.10 -9 5 3 3.60 1.00 9 5 -3 4.50 1.10 8 -5 -3 10.20 1.60 8 -5 -3 8.90 1.60 -8 5 3 12.80 1.80 8 5 -3 7.50 1.40 -8 5 3 8.00 1.40 7 -5 -3 6.40 1.40 7 -5 -3 5.70 1.30 -7 5 3 7.50 1.30 -7 5 3 7.40 1.30 6 -5 -3 19.30 2.10 -6 5 3 20.30 1.90 -6 5 3 19.60 1.90 5 -5 -3 18.10 1.40 5 -5 -3 19.70 1.80 4 -5 -3 58.39 2.80 4 -5 -3 54.29 2.20 -4 -5 3 57.09 2.50 4 5 -3 54.59 2.50 -4 5 3 55.69 2.60 3 -5 -3 7.20 1.00 3 -5 -3 7.20 1.20 3 5 -3 8.20 1.20 3 5 -3 7.00 1.10 2 -5 -3 47.80 2.20 2 -5 -3 48.10 2.30 2 5 -3 48.90 2.30 2 5 -3 49.30 2.30 1 -5 -3 22.20 1.50 -1 -5 3 21.80 1.40 1 -5 -3 22.90 1.60 1 5 -3 23.30 1.60 1 5 -3 24.50 1.60 0 -5 3 95.09 3.40 0 -5 -3 98.49 3.50 0 -5 -3 100.99 3.40 0 5 -3 106.49 3.60 0 5 -3 100.89 3.40 -1 -5 -3 206.78 5.70 -1 -5 -3 203.08 5.80 1 -5 3 208.58 5.80 -1 5 -3 212.58 6.00 -1 5 -3 210.88 5.70 -2 -5 -3 16.20 1.30 2 -5 3 18.40 1.50 -2 -5 -3 16.80 1.40 -2 5 -3 19.60 1.60 -2 5 -3 20.50 1.50 -3 -5 -3 31.60 2.00 -3 -5 -3 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7.50 1.00 3 0 -4 22.40 0.90 -3 0 4 23.80 1.30 3 0 -4 22.50 0.90 -2 0 4 140.19 3.70 2 0 -4 138.59 3.20 2 0 -4 143.59 3.40 1 0 -4 31.40 1.20 1 0 -4 30.70 1.30 0 0 -4 153.28 3.60 0 0 -4 150.88 3.70 0 0 4 153.08 3.40 1 0 4 36.10 1.20 -1 0 -4 38.90 1.20 -1 0 -4 34.20 1.40 2 0 4 408.76 8.90 -2 0 -4 408.16 8.90 -2 0 -4 401.36 8.70 -3 0 -4 14.40 0.80 -3 0 -4 13.90 0.90 3 0 4 14.90 1.00 -4 0 -4 506.25 11.20 4 0 4 503.85 11.30 -4 0 -4 490.75 10.50 5 0 4 7.10 1.00 6 0 4 160.38 4.90 7 0 4 15.90 1.60 -8 0 -4 35.50 1.90 9 0 4 4.60 1.10 -9 0 -4 3.20 1.00 9 0 4 2.50 1.00 -9 0 -4 3.10 0.80 9 0 4 4.00 1.30 10 0 4 127.79 4.60 10 0 4 128.69 4.60 -10 0 -4 130.49 4.10 10 0 4 132.29 5.00 -11 0 -4 1.20 0.60 11 0 4 0.00 0.60 11 0 4 1.80 0.70 -11 0 -4 1.50 0.70 11 0 4 0.20 1.10 -12 0 -4 3.80 0.90 -12 0 -4 2.90 0.60 12 0 4 4.10 1.00 -13 0 -4 0.40 0.50 13 0 4 0.50 0.50 13 0 4 1.60 0.70 -13 0 -4 0.60 0.60 13 -1 -4 11.90 1.20 -13 -1 4 12.90 1.10 13 1 -4 14.20 1.30 -13 1 4 11.70 1.20 12 -1 -4 3.30 1.00 -12 -1 4 4.00 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202.78 5.00 4 3 4 196.98 5.40 -4 3 -4 196.08 5.60 5 -3 4 4.90 0.90 5 3 4 4.60 0.90 -5 3 -4 5.50 0.90 6 -3 4 3.40 0.90 6 3 4 5.80 1.00 -6 3 -4 3.70 1.00 -7 3 -4 5.10 1.20 8 -3 4 30.30 2.50 8 3 4 29.80 2.50 8 3 4 34.50 2.30 -8 3 -4 36.00 2.30 8 3 4 31.30 2.20 8 3 4 36.40 2.50 -8 3 -4 35.80 2.40 -9 -3 -4 196.58 5.40 9 -3 4 197.38 6.50 -9 3 -4 197.78 5.90 9 3 4 190.88 6.30 -9 3 -4 191.28 6.00 9 3 4 206.08 6.80 9 3 4 206.28 6.00 9 3 4 194.18 6.20 10 -3 4 71.69 3.50 -10 -3 -4 64.49 2.60 -10 3 -4 68.79 3.00 10 3 4 74.79 3.60 -10 3 -4 72.09 3.30 10 3 4 65.99 3.20 10 3 4 69.59 3.20 -11 -3 -4 28.60 1.50 11 -3 4 22.90 1.80 11 3 4 30.30 1.90 11 3 4 28.50 2.00 -11 3 -4 23.30 1.90 11 3 4 27.50 1.90 -12 -3 -4 3.30 0.60 12 3 4 2.80 0.60 -12 3 -4 2.50 0.60 12 3 4 2.60 0.70 12 3 4 2.10 0.70 12 -4 -4 2.90 0.60 12 4 -4 2.20 0.60 -12 4 4 1.40 0.50 11 -4 -4 18.10 1.50 11 4 -4 18.00 1.60 -11 4 4 17.40 1.50 10 -4 -4 16.40 1.80 10 -4 -4 15.00 1.90 10 4 -4 17.40 1.90 -10 4 4 15.70 1.60 -10 4 4 15.00 1.70 9 -4 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4 16.40 1.30 -2 4 -4 17.50 1.40 3 -4 4 31.50 1.80 -3 -4 -4 34.60 1.80 -3 4 -4 33.90 1.70 -3 4 -4 30.60 1.90 3 4 4 32.10 1.80 4 -4 4 395.16 10.10 -4 -4 -4 410.76 9.60 -4 4 -4 406.16 10.30 -4 4 -4 400.16 9.50 4 4 4 409.86 10.00 5 -4 4 195.68 5.90 -5 4 -4 184.28 5.90 5 4 4 190.68 5.70 6 -4 4 65.59 3.20 6 4 4 71.49 3.20 -6 4 -4 67.59 3.30 7 -4 4 19.60 2.10 -7 4 -4 22.30 1.90 7 4 4 18.20 1.90 7 4 4 16.30 1.80 -7 4 -4 16.80 1.90 7 4 4 19.00 1.90 8 -4 4 15.00 2.00 8 4 4 17.80 1.90 -8 4 -4 21.00 1.80 8 4 4 18.00 1.90 8 4 4 18.40 2.10 -8 4 -4 19.10 2.00 8 4 4 19.10 1.90 9 -4 4 25.20 2.30 -9 4 -4 27.70 2.20 -9 4 -4 23.10 1.90 9 4 4 24.50 2.20 9 4 4 24.60 2.30 9 4 4 23.60 2.10 9 4 4 25.00 2.00 -10 -4 -4 169.08 4.70 10 -4 4 164.28 5.50 10 4 4 166.18 5.30 -10 4 -4 171.68 5.40 10 4 4 174.58 5.50 10 4 4 171.38 5.70 -10 4 -4 161.38 4.90 11 -4 4 13.20 1.60 -11 -4 -4 16.60 1.20 11 4 4 13.80 1.40 11 4 4 15.90 1.50 -11 4 -4 13.20 1.20 11 4 4 14.10 1.40 12 -4 4 9.00 1.00 12 4 4 10.00 1.00 -12 4 -4 8.60 0.90 12 4 4 10.00 1.10 12 4 4 12.40 1.20 11 -5 -4 2.90 0.70 11 -5 -4 2.40 0.70 -11 5 4 3.00 0.70 -11 5 4 2.30 0.70 11 5 -4 3.00 0.80 10 -5 -4 13.90 1.70 10 -5 -4 11.30 1.50 -10 5 4 13.40 1.30 10 5 -4 14.50 1.60 -10 5 4 13.40 1.40 9 -5 -4 13.60 1.90 9 -5 -4 14.80 1.80 9 5 -4 16.10 1.80 -9 5 4 16.30 1.60 -9 5 4 16.40 1.80 8 -5 -4 47.40 2.90 -8 5 4 48.00 2.60 8 5 -4 48.70 2.80 -8 5 4 48.10 2.70 7 -5 -4 2.80 1.20 7 -5 -4 3.70 1.40 7 5 -4 6.10 1.30 -7 5 4 2.80 0.90 -7 5 4 5.30 1.10 6 -5 -4 7.40 1.30 -6 5 4 8.30 1.40 -6 5 4 9.40 1.60 -6 5 4 10.00 1.40 5 -5 -4 8.50 1.10 5 -5 -4 6.20 1.20 4 -5 -4 34.80 2.20 4 -5 -4 35.50 1.80 4 5 -4 39.20 2.50 4 5 -4 37.90 2.10 3 -5 -4 33.90 2.00 3 -5 -4 35.80 2.10 3 5 -4 41.20 2.30 3 5 -4 38.20 2.10 2 -5 -4 0.50 0.60 2 -5 -4 -0.40 0.50 2 5 -4 0.30 0.60 2 5 -4 0.90 0.60 1 -5 -4 17.00 1.40 1 -5 -4 16.40 1.40 1 5 -4 18.90 1.50 1 5 -4 17.60 1.40 0 -5 -4 97.99 3.40 0 -5 -4 87.99 3.30 0 5 -4 96.39 3.40 0 5 -4 92.89 3.50 1 -5 4 42.90 2.10 -1 -5 -4 40.40 2.10 -1 -5 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0.50 11 -6 -4 6.90 1.00 -11 6 4 5.80 0.90 10 -6 -4 2.50 0.80 10 -6 -4 2.20 0.90 -10 6 4 0.70 0.60 -10 6 4 2.30 0.80 9 -6 -4 22.20 1.80 9 -6 -4 29.20 2.10 -9 6 4 24.40 1.80 -9 6 4 22.20 1.60 8 -6 -4 0.20 0.70 8 -6 -4 2.80 0.90 -8 6 4 1.50 0.90 -8 6 4 1.40 0.70 7 -6 -4 4.70 1.30 7 -6 -4 3.50 1.30 -7 6 4 3.20 1.10 -7 6 4 3.20 1.00 6 -6 -4 58.89 3.20 -6 6 4 54.89 3.00 -6 6 4 51.29 2.90 -6 6 4 53.29 2.80 5 -6 -4 52.29 3.10 5 -6 -4 54.39 2.30 -5 6 4 54.19 2.90 -5 6 4 57.09 2.90 -5 6 4 49.50 2.90 4 -6 -4 51.59 2.30 4 -6 -4 56.29 3.00 -4 6 4 55.09 2.90 -4 6 4 49.90 2.80 -4 6 4 52.69 2.90 3 -6 -4 12.70 1.50 3 -6 -4 13.40 1.20 3 6 -4 13.90 1.50 2 -6 -4 53.89 2.80 2 -6 -4 56.09 2.30 2 -6 -4 57.19 2.70 2 6 -4 57.39 2.90 2 6 -4 52.29 2.70 1 -6 -4 15.20 1.20 1 -6 -4 14.20 1.60 1 -6 -4 16.20 1.50 1 6 -4 17.10 1.70 1 6 -4 15.40 1.40 0 -6 -4 16.60 1.60 0 -6 -4 16.70 1.60 0 6 -4 20.70 1.70 0 6 -4 16.20 1.70 -1 -6 -4 3.20 0.80 -1 -6 -4 4.10 0.80 -1 6 -4 3.60 0.90 -1 6 -4 3.00 1.00 -2 -6 -4 38.30 2.30 2 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7.70 1 -3 -5 322.47 7.60 1 3 -5 330.57 7.70 1 3 -5 319.17 8.00 0 -3 -5 56.69 2.10 0 -3 5 54.89 1.80 0 -3 -5 58.29 2.10 0 3 -5 59.39 2.20 0 3 -5 53.39 2.20 1 -3 5 160.08 4.30 -1 -3 -5 170.78 4.50 1 3 5 166.88 4.40 -1 3 -5 165.68 4.40 -1 3 -5 169.18 4.70 2 -3 5 60.49 2.20 -2 -3 -5 59.89 2.30 2 3 5 60.29 2.30 -2 3 -5 67.09 2.30 -2 3 -5 62.79 2.50 3 -3 5 300.07 7.60 -3 -3 -5 307.17 7.50 -3 3 -5 318.07 8.00 -3 3 -5 311.97 7.30 3 3 5 305.77 7.60 4 -3 5 371.16 9.20 -4 -3 -5 371.86 8.90 4 3 5 374.36 9.20 -4 3 -5 370.16 8.70 -4 3 -5 378.36 9.50 5 -3 5 64.19 2.80 5 3 5 58.49 2.60 -5 3 -5 61.39 2.80 6 -3 5 2.20 0.90 -6 3 -5 1.60 0.80 6 3 5 2.80 0.70 -7 3 -5 25.70 2.10 7 3 5 27.90 2.40 -7 3 -5 28.20 2.10 7 3 5 27.00 2.00 7 3 5 22.20 2.00 7 3 5 24.40 2.10 8 -3 5 8.80 1.50 -8 -3 -5 10.30 1.30 -8 3 -5 6.90 1.30 8 3 5 9.30 1.50 8 3 5 8.00 1.40 8 3 5 8.60 1.40 8 3 5 9.60 1.70 -8 3 -5 10.10 1.50 9 -3 5 326.87 9.20 -9 -3 -5 317.27 8.10 -9 3 -5 324.87 8.50 -9 3 -5 323.57 8.80 9 3 5 318.37 9.00 9 3 5 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204.98 6.20 4 -4 -5 527.55 12.50 4 4 -5 512.75 11.90 4 4 -5 527.45 12.90 3 -4 -5 312.37 7.60 3 -4 -5 310.07 7.90 3 4 -5 302.97 7.60 3 4 -5 302.37 8.10 2 -4 -5 193.18 5.30 2 -4 -5 195.68 5.40 2 4 -5 194.08 5.30 2 4 -5 197.88 5.70 1 -4 -5 14.60 1.20 1 -4 -5 14.60 1.20 1 4 -5 15.40 1.30 1 4 -5 16.20 1.40 0 -4 -5 3.20 0.70 0 -4 -5 3.90 0.80 0 4 -5 2.90 0.70 0 4 -5 4.20 0.80 -1 -4 -5 379.86 8.90 -1 -4 -5 374.16 9.10 1 -4 5 355.06 8.70 -1 4 -5 365.86 9.30 -1 4 -5 386.86 8.90 2 -4 5 140.89 4.30 -2 -4 -5 143.49 4.40 -2 -4 -5 149.59 4.40 -2 4 -5 149.49 4.30 2 4 5 147.49 4.40 -2 4 -5 145.19 4.60 3 -4 5 224.68 6.30 -3 -4 -5 241.68 6.30 -3 4 -5 238.38 6.10 3 4 5 225.08 6.30 -3 4 -5 235.18 6.70 -4 -4 -5 207.88 5.90 4 -4 5 211.78 6.20 -4 4 -5 213.28 6.40 4 4 5 218.78 6.10 5 -4 5 5.20 1.10 5 -4 5 4.50 0.80 5 4 5 9.40 1.30 -5 4 -5 4.70 1.00 7 -4 5 29.00 2.40 -7 4 -5 31.80 2.30 -7 4 -5 36.90 2.30 7 4 5 33.20 2.40 7 4 5 30.90 2.30 7 4 5 31.30 2.30 8 -4 5 1.00 1.00 -8 4 -5 0.40 0.90 8 4 5 0.30 0.70 8 4 5 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6 -5 19.80 1.90 -5 6 -5 22.00 2.00 -5 6 -5 23.40 2.10 -5 6 -5 18.00 1.80 6 -6 5 36.20 2.40 6 6 5 32.20 2.40 6 6 5 35.70 2.50 -6 6 -5 39.70 2.50 6 6 5 36.60 2.50 6 6 5 38.00 2.60 -6 6 -5 36.70 2.40 -6 6 -5 36.90 2.40 7 -6 5 15.30 2.00 7 6 5 18.00 1.70 7 6 5 14.90 1.60 7 6 5 15.40 1.80 -7 6 -5 18.40 1.80 -7 6 -5 13.60 1.80 8 -6 5 12.60 1.50 8 6 5 12.40 1.60 -8 6 -5 10.90 1.50 8 6 5 12.70 1.40 8 6 5 13.80 1.70 -8 6 -5 11.00 1.30 -9 -6 -5 17.00 1.10 9 -6 5 15.00 1.50 9 6 5 16.60 1.30 -9 6 -5 16.10 1.40 9 6 5 16.30 1.40 9 6 5 16.60 1.60 -9 6 -5 14.60 1.30 10 -6 5 6.00 0.90 -10 -6 -5 4.30 0.70 -10 6 -5 3.70 0.70 10 6 5 4.00 0.70 10 6 5 6.00 0.90 -10 6 -5 3.90 0.70 10 -7 -5 9.20 1.00 -10 7 5 7.30 0.90 9 -7 -5 0.50 0.70 -9 7 5 0.40 0.60 -9 7 5 1.40 0.50 8 -7 -5 10.40 1.40 -8 7 5 10.70 1.40 -8 7 5 9.20 1.10 7 -7 -5 6.90 1.30 7 -7 -5 6.70 1.40 -7 7 5 7.00 1.20 -7 7 5 8.30 1.30 6 -7 -5 31.00 2.50 6 -7 -5 31.90 2.50 -6 7 5 30.80 2.20 -6 7 5 27.90 2.00 5 -7 -5 21.40 2.00 -5 7 5 20.40 2.00 -5 7 5 22.70 1.80 -5 7 5 23.60 2.20 4 -7 -5 3.80 0.80 4 -7 -5 4.90 1.30 4 7 -5 3.60 1.10 4 7 -5 3.40 1.10 -4 7 5 5.40 1.30 4 7 -5 5.30 1.30 -4 7 5 4.80 1.20 -4 7 5 4.70 1.20 3 -7 -5 21.30 1.50 3 -7 -5 20.30 2.00 3 7 -5 20.00 2.00 -3 7 5 21.80 2.00 -3 7 5 20.80 1.90 -3 7 5 18.50 1.90 -3 7 5 19.10 1.90 3 7 -5 21.30 1.90 3 7 -5 16.50 1.80 -3 7 5 18.20 2.00 2 -7 -5 0.60 0.60 2 -7 -5 1.40 1.00 -2 7 5 0.20 0.80 2 7 -5 -0.40 0.80 -2 7 5 1.20 0.90 -2 7 5 1.00 0.80 -2 7 5 1.40 0.90 -2 7 5 1.00 0.90 2 7 -5 1.10 0.90 2 7 -5 -0.20 0.70 -2 7 5 0.60 0.90 1 -7 -5 14.40 1.30 -1 7 5 16.80 1.90 -1 7 5 11.50 1.70 -1 7 5 13.40 1.70 1 7 -5 12.10 1.60 1 7 -5 12.70 1.60 -1 7 5 10.90 1.60 1 7 -5 11.50 1.70 -1 7 5 14.60 1.80 -1 7 5 13.30 1.70 1 7 -5 13.10 1.70 1 7 -5 11.70 1.60 0 -7 -5 14.60 1.20 0 7 -5 13.50 1.70 0 7 -5 16.80 1.70 0 7 5 15.70 1.80 0 7 5 13.60 1.80 0 7 5 18.10 1.90 0 7 5 13.00 1.50 0 7 -5 14.60 1.70 0 7 5 12.30 1.70 0 7 -5 12.50 1.70 0 7 -5 17.10 1.90 0 7 5 15.10 1.80 -1 -7 -5 47.20 2.10 1 -7 5 46.50 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2 -17 0.20 0.80 3 -2 17 0.60 1.00 -3 -2 -17 1.10 0.80 -3 2 -17 2.20 0.70 4 -2 17 13.40 1.70 -4 -2 -17 14.40 1.50 -4 2 -17 10.40 1.20 4 2 17 10.10 1.50 -5 -2 -17 5.10 0.90 5 -2 17 6.70 1.10 5 2 17 6.70 1.10 -5 2 -17 5.00 0.80 -6 -2 -17 6.60 0.90 6 -2 17 7.60 1.00 6 2 17 6.80 1.10 -6 2 -17 7.90 0.90 7 -3 -17 3.90 0.70 7 3 -17 3.50 0.70 7 3 -17 3.60 0.80 7 3 -17 4.20 0.70 7 3 -17 3.90 0.60 -6 -3 17 5.30 0.80 6 -3 -17 7.10 1.00 6 3 -17 6.30 1.00 6 3 -17 8.80 1.00 6 3 -17 7.40 1.00 6 3 -17 7.10 1.10 -5 -3 17 25.90 1.50 5 -3 -17 26.10 1.90 5 3 -17 25.50 1.60 5 3 -17 23.90 1.60 5 3 -17 25.70 1.70 5 3 -17 29.20 1.80 4 -3 -17 9.90 1.50 -4 -3 17 8.10 1.00 4 3 -17 7.80 1.30 4 3 -17 10.20 1.20 4 3 -17 8.50 1.30 4 3 -17 8.90 1.40 -3 -3 17 1.70 0.70 3 -3 -17 1.00 0.90 3 3 -17 2.70 1.00 3 3 -17 2.10 0.80 3 3 -17 3.10 1.00 2 -3 -17 2.50 0.80 -2 -3 17 4.20 1.00 -2 -3 17 1.60 0.60 2 3 -17 3.70 0.90 2 3 -17 3.90 0.90 -1 -3 17 13.50 1.20 -1 -3 17 13.60 1.60 1 -3 -17 13.30 1.40 1 3 -17 15.70 1.70 0 -3 17 2.00 0.90 0 3 -17 0.30 0.80 1 -3 17 31.10 2.40 -1 3 -17 25.20 1.70 -2 -3 -17 57.39 2.70 2 -3 17 64.19 3.20 -2 3 -17 57.09 2.70 -3 -3 -17 4.80 1.00 3 -3 17 10.10 1.60 -3 3 -17 6.40 1.00 -4 -3 -17 8.40 1.30 4 -3 17 8.00 1.30 -4 3 -17 8.60 1.10 -5 -3 -17 0.70 0.60 5 -3 17 -0.40 0.70 -5 3 -17 -0.30 0.40 6 -3 17 1.90 0.70 -6 -3 -17 3.20 0.70 -6 3 -17 3.10 0.60 6 -4 -17 0.00 0.40 6 4 -17 0.00 0.50 6 4 -17 -0.10 0.50 6 4 -17 -0.10 0.40 6 4 -17 0.70 0.50 -5 -4 17 -0.20 0.40 5 -4 -17 0.60 0.50 5 4 -17 1.20 0.50 5 4 -17 0.00 0.60 5 4 -17 -0.50 0.60 5 4 -17 -0.40 0.60 4 -4 -17 0.40 0.50 -4 -4 17 0.10 0.50 -4 -4 17 0.90 0.70 4 4 -17 1.60 0.60 4 4 -17 1.40 0.60 4 4 -17 1.70 0.80 4 4 -17 1.10 0.70 -3 -4 17 6.80 1.20 3 -4 -17 6.00 1.00 -3 -4 17 4.90 0.70 3 4 -17 6.50 1.00 3 4 -17 6.10 0.90 3 4 -17 8.10 1.40 3 4 -17 6.90 1.00 -2 -4 17 22.40 1.40 -2 -4 17 18.80 1.70 2 -4 -17 23.10 1.80 2 4 -17 22.30 1.70 2 4 -17 22.90 1.80 2 4 -17 18.80 1.50 -1 -4 17 28.70 2.10 1 -4 -17 25.20 1.80 -1 -4 17 22.30 1.40 1 4 -17 26.40 1.90 0 -4 17 18.40 1.90 0 -4 17 14.90 1.20 0 4 -17 14.50 1.30 -1 -4 -17 7.30 1.10 1 -4 17 9.00 1.30 -1 4 -17 10.30 1.30 2 -4 17 10.40 1.60 -2 -4 -17 12.40 1.40 -2 4 -17 10.20 1.30 3 -4 17 -0.30 0.80 -3 -4 -17 0.10 0.70 -3 4 -17 1.10 0.50 -4 -4 -17 2.90 0.60 4 -4 17 3.30 0.90 -4 4 -17 2.00 0.60 -5 -4 -17 2.00 0.60 -5 4 -17 3.70 0.70 5 -5 -17 10.20 1.10 -5 -5 17 6.60 1.00 5 5 -17 6.40 0.70 5 5 -17 7.00 0.80 5 5 -17 8.90 1.00 -4 -5 17 7.80 0.80 -4 -5 17 9.10 1.20 4 -5 -17 8.70 1.00 4 5 -17 6.50 0.90 4 5 -17 9.40 1.10 4 5 -17 9.30 1.10 3 -5 -17 3.80 0.70 -3 -5 17 3.70 0.60 -3 -5 17 4.70 0.80 3 5 -17 5.30 0.90 3 5 -17 6.10 0.90 3 5 -17 4.50 0.90 2 -5 -17 11.00 1.30 -2 -5 17 9.20 1.20 -2 -5 17 7.50 0.90 2 5 -17 10.20 1.10 2 5 -17 10.70 1.30 2 5 -17 10.40 1.20 -1 -5 17 0.80 0.80 -1 -5 17 0.60 0.50 1 5 -17 0.10 0.40 1 5 -17 0.60 0.50 0 -5 17 10.40 1.20 0 -5 17 9.60 0.90 0 5 -17 12.60 1.30 0 5 -17 11.40 1.30 1 -5 17 63.89 2.70 -1 5 -17 64.79 2.50 -2 -5 -17 22.00 1.50 -2 5 -17 26.10 1.60 -3 -5 -17 2.40 0.60 -3 5 -17 1.60 0.50 2 6 -17 11.10 1.00 2 6 -17 9.90 0.90 1 6 -17 1.00 0.50 1 6 -17 1.40 0.60 7 0 -18 16.70 1.30 7 0 -18 19.30 1.30 6 0 -18 28.50 1.70 -6 0 18 33.30 1.90 6 0 -18 37.20 1.80 5 0 -18 0.70 0.60 -5 0 18 0.80 0.80 -4 0 18 33.20 2.20 4 0 -18 39.20 2.30 3 0 -18 0.90 0.60 -3 0 18 1.70 0.90 2 0 -18 0.80 0.90 -2 0 18 0.30 0.90 1 0 -18 4.30 0.90 -1 0 18 2.00 1.00 0 0 18 7.60 1.30 1 0 18 16.00 1.90 2 0 18 0.50 0.80 -2 0 -18 -0.40 0.50 3 0 18 4.10 0.90 -3 0 -18 3.00 0.80 4 0 18 12.40 1.50 -4 0 -18 15.00 1.50 -5 0 -18 12.80 1.20 5 0 18 12.60 1.40 -6 0 -18 32.80 1.70 6 0 18 33.10 1.80 7 -1 -18 0.50 0.50 -7 -1 18 0.00 0.50 7 1 -18 0.20 0.50 7 1 -18 0.60 0.40 7 1 -18 0.20 0.60 6 -1 -18 0.50 0.50 -6 -1 18 0.30 0.50 6 1 -18 1.20 0.60 6 1 -18 1.10 0.60 6 1 -18 0.10 0.60 5 -1 -18 24.30 1.70 -5 -1 18 24.60 1.70 5 1 -18 23.60 1.60 5 1 -18 27.70 1.70 5 1 -18 31.70 1.80 -4 -1 18 2.70 1.00 4 -1 -18 3.40 0.80 4 1 -18 4.50 1.10 4 1 -18 2.30 1.00 3 -1 -18 9.10 1.50 -3 -1 18 7.90 1.30 3 1 -18 7.30 1.20 2 -1 -18 3.90 1.00 -2 -1 18 2.40 1.00 2 1 -18 2.80 0.90 -1 -1 18 14.00 1.80 1 -1 -18 13.10 1.60 1 1 -18 13.40 1.50 -1 1 18 10.80 1.60 0 -1 18 19.00 2.00 0 1 18 15.50 1.70 1 -1 18 47.60 2.70 1 1 18 47.90 2.70 -2 -1 -18 3.20 0.80 2 -1 18 4.80 1.10 -2 1 -18 5.40 1.00 2 1 18 3.70 0.90 -3 -1 -18 4.20 0.80 3 -1 18 3.90 0.90 -3 1 -18 2.50 0.80 3 1 18 2.50 0.80 4 -1 18 7.90 1.20 -4 -1 -18 7.60 1.20 4 1 18 7.30 1.10 -4 1 -18 8.70 1.20 -5 -1 -18 20.10 1.40 5 -1 18 19.90 1.50 5 1 18 23.90 1.60 -5 1 -18 22.50 1.40 6 -2 -18 3.00 0.80 6 2 -18 5.00 0.90 6 2 -18 3.60 0.80 6 2 -18 2.00 0.60 5 -2 -18 0.80 0.60 5 2 -18 0.10 0.70 5 2 -18 0.50 0.50 5 2 -18 1.20 0.70 4 -2 -18 6.70 1.00 -4 -2 18 7.30 1.20 4 2 -18 6.80 1.10 4 2 -18 8.60 1.30 4 2 -18 9.80 1.30 3 -2 -18 30.10 2.00 -3 -2 18 26.30 2.10 3 2 -18 30.70 2.10 -2 -2 18 0.40 0.90 2 -2 -18 0.00 0.70 2 2 -18 -0.70 0.50 1 -2 -18 20.10 1.70 -1 -2 18 21.90 2.00 1 2 -18 21.30 1.80 0 -2 18 41.10 2.60 1 -2 18 16.50 1.90 -2 -2 -18 0.30 0.60 2 -2 18 -1.10 0.80 -2 2 -18 0.20 0.50 3 -2 18 2.60 1.00 -3 -2 -18 2.70 0.80 -3 2 -18 1.60 0.70 4 -2 18 5.20 1.10 -4 -2 -18 5.20 0.90 -4 2 -18 5.90 0.90 5 -2 18 2.80 0.80 -5 -2 -18 3.40 0.70 -5 2 -18 1.80 0.50 6 -3 -18 -0.20 0.60 -6 -3 18 0.70 0.50 6 3 -18 0.40 0.40 6 3 -18 0.50 0.50 6 3 -18 0.20 0.50 5 -3 -18 0.90 0.70 -5 -3 18 1.10 0.50 5 3 -18 1.30 0.60 5 3 -18 1.50 0.70 5 3 -18 1.00 0.50 4 -3 -18 10.30 1.30 -4 -3 18 8.10 1.20 -4 -3 18 8.20 0.80 4 3 -18 6.80 1.00 4 3 -18 7.80 1.20 4 3 -18 7.90 1.30 3 -3 -18 1.10 0.60 -3 -3 18 0.70 0.50 -3 -3 18 2.10 0.70 3 3 -18 1.60 0.60 2 -3 -18 8.10 1.30 -2 -3 18 7.20 1.20 2 3 -18 8.60 1.10 -1 -3 18 5.20 1.00 1 -3 -18 5.60 1.00 1 3 -18 5.20 0.90 0 -3 18 2.90 0.80 0 3 -18 4.60 0.80 1 -3 18 1.20 0.70 -1 3 -18 1.00 0.70 -2 -3 -18 3.40 0.80 2 -3 18 7.40 1.20 -2 3 -18 5.00 0.80 3 -3 18 0.00 0.80 -3 -3 -18 0.20 0.40 -3 3 -18 0.30 0.60 -4 -3 -18 0.40 0.40 4 -3 18 0.50 0.70 -4 3 -18 0.80 0.40 5 -4 -18 3.20 0.60 -5 -4 18 4.70 0.80 5 4 -18 3.40 0.70 5 4 -18 2.30 0.50 -4 -4 18 18.20 1.50 4 -4 -18 18.30 1.40 4 4 -18 17.10 1.30 4 4 -18 18.80 1.40 4 4 -18 18.20 1.30 -3 -4 18 5.20 1.00 3 -4 -18 8.00 1.20 -3 -4 18 5.90 0.70 3 4 -18 6.80 0.90 3 4 -18 6.00 1.00 -2 -4 18 0.50 0.40 2 -4 -18 -1.30 0.60 -2 -4 18 -0.10 0.70 2 4 -18 -0.10 0.60 -1 -4 18 2.00 0.60 1 4 -18 0.80 0.50 0 -4 18 5.50 1.00 0 4 -18 7.10 1.10 1 -4 18 23.60 1.60 -2 -4 -18 6.70 1.00 2 -4 18 8.50 1.30 -2 4 -18 6.40 1.00 -3 -4 -18 8.30 0.80 3 -4 18 8.40 1.00 -3 4 -18 8.60 0.90 2 5 -18 -0.20 0.50 1 5 -18 16.70 1.10 5 0 -19 24.40 1.60 4 0 -19 0.40 0.50 -4 0 19 0.70 0.60 3 0 -19 -1.50 0.60 -3 0 19 -0.20 0.50 2 0 -19 -0.40 0.70 -2 0 19 0.10 0.70 1 0 -19 8.40 1.00 -1 0 19 7.10 1.20 0 0 19 0.70 0.80 1 0 19 4.20 1.10 -2 0 -19 19.60 1.50 2 0 19 21.80 1.80 3 0 19 1.60 0.60 -3 0 -19 2.30 0.70 -4 0 -19 -0.50 0.50 4 0 19 0.40 0.70 5 -1 -19 18.30 1.30 -5 -1 19 18.70 1.40 5 1 -19 22.20 1.50 4 -1 -19 19.30 1.40 -4 -1 19 15.60 1.30 4 1 -19 14.30 1.20 -3 -1 19 4.70 0.90 3 -1 -19 5.70 1.00 3 1 -19 6.00 1.00 -2 -1 19 0.40 0.50 2 -1 -19 0.50 0.70 2 1 -19 -0.20 0.70 -1 -1 19 6.30 1.10 -1 1 19 5.80 1.10 1 1 -19 6.20 1.00 0 -1 19 2.30 0.80 0 1 19 3.10 0.90 1 -1 19 11.70 1.30 1 1 19 10.10 1.20 2 -1 19 4.50 1.00 -2 -1 -19 2.80 0.70 2 1 19 3.80 0.90 -2 1 -19 3.40 0.70 3 -1 19 12.20 1.50 -3 -1 -19 12.00 1.20 -3 1 -19 12.10 1.20 3 1 19 9.80 1.20 4 -1 19 2.90 0.80 -4 -1 -19 3.30 0.60 -4 1 -19 3.00 0.70 4 1 19 2.60 0.70 5 -2 -19 17.50 1.30 -5 -2 19 16.40 1.40 5 2 -19 12.60 1.00 -4 -2 19 -0.10 0.60 4 -2 -19 -0.50 0.60 4 2 -19 -0.20 0.40 3 -2 -19 2.20 0.60 -3 -2 19 1.30 0.80 3 2 -19 1.30 0.70 2 -2 -19 0.50 0.50 -2 -2 19 0.70 0.80 2 2 -19 0.20 0.60 -1 -2 19 0.10 0.50 1 2 -19 -0.30 0.60 0 -2 19 16.90 1.70 1 -2 19 3.70 1.00 2 -2 19 3.00 0.90 -2 -2 -19 0.50 0.60 -2 2 -19 0.90 0.50 3 -2 19 3.40 0.90 -3 -2 -19 2.70 0.60 -3 2 -19 3.60 0.70 -4 -2 -19 0.60 0.50 4 -2 19 0.80 0.50 -4 2 -19 0.40 0.40 -4 -3 19 4.90 0.80 4 -3 -19 4.20 0.80 4 3 -19 3.10 0.60 -3 -3 19 11.60 1.10 3 -3 -19 10.70 1.00 3 3 -19 15.80 1.30 2 -3 -19 5.60 0.80 -2 -3 19 6.20 1.00 2 3 -19 7.20 1.00 -1 -3 19 27.40 1.80 1 3 -19 35.90 1.80 0 -3 19 2.90 0.90 1 -3 19 5.90 1.10 2 -3 19 8.20 1.30 3 -3 19 1.40 0.70 -2 -4 19 1.10 0.70 2 4 -19 1.80 0.60 -1 -4 19 1.30 0.70 0 -4 19 1.10 0.50 1 -4 19 7.30 1.00 4 0 -20 9.20 1.00 3 0 -20 3.50 0.70 2 0 -20 14.60 1.20 -2 0 20 9.10 1.20 -1 0 20 12.90 1.10 0 0 20 4.40 0.80 1 0 20 0.20 0.60 2 0 20 0.50 0.40 -3 -1 20 1.50 0.70 3 -1 -20 2.40 0.70 3 1 -20 0.30 0.40 2 -1 -20 2.10 0.60 -2 -1 20 1.20 0.70 2 1 -20 1.70 0.60 -1 -1 20 12.50 1.20 0 -1 20 24.10 1.50 1 -1 20 4.80 0.80 2 -1 20 9.30 1.20 -3 -2 20 8.50 1.10 3 2 -20 7.90 0.80 -2 -2 20 2.40 0.60 2 2 -20 1.40 0.50 -1 -2 20 0.40 0.70 0 -2 20 2.00 0.80 1 -2 20 0.50 0.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 62047 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a nylon loop with paratone oil' _olex2_submission_original_sample_id 'Vial 2 CBZ' _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 O1A O 0.4945(3) 0.3527(4) 0.4994(2) 0.0467(8) Uani 1 1 d . O2A O 0.3519(2) 0.1411(3) 0.30247(17) 0.0386(7) Uani 1 1 d . O3A O 0.8378(2) 0.1201(4) 0.41828(18) 0.0410(7) Uani 1 1 d . O4A O 0.7450(3) 0.2473(5) 0.3175(2) 0.0601(10) Uani 1 1 d . N1A N 0.3470(3) 0.3425(4) 0.4008(2) 0.0321(7) Uani 1 1 d . N2A N 0.2899(3) 0.4609(4) 0.4368(2) 0.0356(7) Uani 1 1 d . N3A N 0.6410(3) 0.1540(4) 0.4173(2) 0.0344(7) Uani 1 1 d . H3A H 0.646(4) 0.098(7) 0.456(3) 0.049(15) Uiso 1 1 d . C1A C 0.4586(3) 0.3059(5) 0.4364(2) 0.0333(8) Uani 1 1 d . C2A C 0.5300(3) 0.2074(4) 0.3822(2) 0.0323(8) Uani 1 1 d . H2A H 0.551249 0.272976 0.337158 0.039 Uiso 1 1 calc R C3A C 0.4536(4) 0.0803(5) 0.3460(3) 0.0385(9) Uani 1 1 d . H3AA H 0.501819 0.019621 0.310476 0.046 Uiso 1 1 calc R H3AB H 0.426611 0.013833 0.388465 0.046 Uiso 1 1 calc R C4A C 0.1916(4) 0.5077(5) 0.4030(3) 0.0376(9) Uani 1 1 d . H4A H 0.152674 0.587590 0.428562 0.045 Uiso 1 1 calc R C5A C 0.1327(4) 0.4521(5) 0.3299(2) 0.0354(9) Uani 1 1 d . C6A C 0.1828(3) 0.3309(5) 0.2914(2) 0.0339(8) Uani 1 1 d . C7A C 0.1261(4) 0.2773(5) 0.2212(3) 0.0396(9) Uani 1 1 d . H7A H 0.158741 0.194359 0.194522 0.048 Uiso 1 1 calc R C8A C 0.0225(4) 0.3454(6) 0.1909(3) 0.0463(11) Uani 1 1 d . H8A H -0.014449 0.309927 0.142801 0.056 Uiso 1 1 calc R C9A C -0.0276(4) 0.4636(6) 0.2297(3) 0.0493(12) Uani 1 1 d . H9A H -0.099545 0.507795 0.208787 0.059 Uiso 1 1 calc R C10A C 0.0268(4) 0.5185(5) 0.2992(3) 0.0435(10) Uani 1 1 d . H10A H -0.007492 0.600491 0.325854 0.052 Uiso 1 1 calc R C11A C 0.7406(4) 0.1786(5) 0.3790(2) 0.0377(9) Uani 1 1 d . C12A C 0.9469(4) 0.1426(10) 0.3787(4) 0.086(3) Uani 1 1 d . H12A H 0.952152 0.248117 0.360934 0.103 Uiso 1 1 calc R H12B H 0.948158 0.076801 0.331699 0.103 Uiso 1 1 calc R C13A C 1.0516(4) 0.1063(7) 0.4349(3) 0.0522(13) Uani 1 1 d . C14A C 1.0817(5) 0.2007(7) 0.4980(4) 0.0643(16) Uani 1 1 d . H14A H 1.035151 0.287567 0.507010 0.077 Uiso 1 1 calc R C15A C 1.1806(5) 0.1674(7) 0.5478(3) 0.0629(14) Uani 1 1 d . H15A H 1.201823 0.231634 0.591011 0.075 Uiso 1 1 calc R C16A C 1.2482(4) 0.0403(6) 0.5345(3) 0.0485(11) Uani 1 1 d . H16A H 1.314696 0.016153 0.569142 0.058 Uiso 1 1 calc R C17A C 1.2187(4) -0.0493(6) 0.4717(3) 0.0458(11) Uani 1 1 d . H17A H 1.265972 -0.135270 0.462008 0.055 Uiso 1 1 calc R C18A C 1.1209(4) -0.0169(6) 0.4219(3) 0.0457(11) Uani 1 1 d . H18A H 1.101463 -0.080660 0.378166 0.055 Uiso 1 1 calc R B1A B 0.2974(4) 0.2646(5) 0.3309(3) 0.0336(9) Uani 1 1 d . O1B O -0.0048(3) 0.6708(4) 0.01360(18) 0.0470(7) Uani 1 1 d . O2B O 0.1395(3) 0.8561(3) 0.21934(18) 0.0403(7) Uani 1 1 d . O3B O -0.3217(3) 0.8865(4) 0.0769(2) 0.0489(8) Uani 1 1 d . O4B O -0.2083(3) 0.7332(4) 0.1564(2) 0.0515(8) Uani 1 1 d . N1B N 0.1473(3) 0.6793(4) 0.10941(19) 0.0338(7) Uani 1 1 d . N2B N 0.2016(3) 0.5608(4) 0.0703(2) 0.0381(8) Uani 1 1 d . N3B N -0.1244(3) 0.9121(4) 0.0811(2) 0.0409(8) Uani 1 1 d . H3B H -0.135(4) 0.962(6) 0.047(3) 0.031(12) Uiso 1 1 d . C1B C 0.0422(4) 0.7307(5) 0.0711(2) 0.0344(8) Uani 1 1 d . C2B C -0.0013(4) 0.8791(5) 0.1043(2) 0.0370(9) Uani 1 1 d . H2B H 0.047958 0.959701 0.080857 0.044 Uiso 1 1 calc R C3B C 0.0194(4) 0.8918(5) 0.1942(3) 0.0413(10) Uani 1 1 d . H3BA H 0.001011 0.995381 0.210852 0.050 Uiso 1 1 calc R H3BB H -0.035775 0.822881 0.220137 0.050 Uiso 1 1 calc R C4B C 0.3008(4) 0.5098(5) 0.1013(2) 0.0388(9) Uani 1 1 d . H4B H 0.336342 0.429523 0.074006 0.047 Uiso 1 1 calc R C5B C 0.3644(4) 0.5600(5) 0.1727(2) 0.0353(8) Uani 1 1 d . C6B C 0.3158(3) 0.6777(5) 0.2158(2) 0.0345(8) Uani 1 1 d . C7B C 0.3756(4) 0.7254(5) 0.2852(2) 0.0395(9) Uani 1 1 d . H7B H 0.341596 0.801898 0.316005 0.047 Uiso 1 1 calc R C8B C 0.4840(4) 0.6627(5) 0.3098(3) 0.0443(10) Uani 1 1 d . H8B H 0.524678 0.697419 0.356842 0.053 Uiso 1 1 calc R C9B C 0.5338(4) 0.5483(5) 0.2656(3) 0.0434(10) Uani 1 1 d . H9B H 0.609089 0.506785 0.282185 0.052 Uiso 1 1 calc R C10B C 0.4740(4) 0.4952(5) 0.1979(3) 0.0409(9) Uani 1 1 d . H10B H 0.506886 0.415564 0.168697 0.049 Uiso 1 1 calc R C11B C -0.2166(4) 0.8339(5) 0.1089(3) 0.0406(9) Uani 1 1 d . C12B C -0.4258(4) 0.8115(8) 0.1066(4) 0.0656(17) Uani 1 1 d . H12C H -0.427419 0.825297 0.164538 0.079 Uiso 1 1 calc R H12D H -0.422146 0.702629 0.095415 0.079 Uiso 1 1 calc R C13B C -0.5352(4) 0.8774(6) 0.0671(3) 0.0554(14) Uani 1 1 d . C14B C -0.5825(5) 0.8061(11) -0.0001(4) 0.082(2) Uani 1 1 d . H14B H -0.538770 0.722156 -0.017722 0.099 Uiso 1 1 calc R C15B C -0.6833(6) 0.8408(11) -0.0440(5) 0.086(2) Uani 1 1 d . H15B H -0.710803 0.782638 -0.088190 0.103 Uiso 1 1 calc R C16B C -0.7410(7) 0.9622(8) -0.0206(5) 0.080(2) Uani 1 1 d . H16B H -0.810733 0.991277 -0.050997 0.096 Uiso 1 1 calc R C17B C -0.7076(4) 1.0492(7) 0.0441(4) 0.0620(15) Uani 1 1 d . H17B H -0.750781 1.136601 0.057553 0.074 Uiso 1 1 calc R C18B C -0.5999(6) 0.9978(8) 0.0916(5) 0.085(2) Uani 1 1 d . H18B H -0.575959 1.048698 0.139038 0.102 Uiso 1 1 calc R B1B B 0.1971(4) 0.7440(5) 0.1826(3) 0.0347(9) Uani 1 1 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 O1A 0.0352(14) 0.058(2) 0.0458(16) -0.0140(16) -0.0061(12) -0.0009(14) O2A 0.0324(13) 0.0359(15) 0.0466(16) -0.0072(12) -0.0082(11) 0.0021(11) O3A 0.0262(13) 0.0520(18) 0.0452(16) 0.0180(13) 0.0057(11) 0.0056(12) O4A 0.0364(16) 0.086(3) 0.059(2) 0.035(2) 0.0115(14) 0.0126(17) N1A 0.0260(14) 0.0332(16) 0.0373(17) -0.0024(14) 0.0040(12) -0.0023(13) N2A 0.0312(16) 0.0364(17) 0.0394(19) -0.0056(15) 0.0046(13) -0.0012(14) N3A 0.0259(15) 0.0389(18) 0.0383(18) 0.0074(15) -0.0010(12) -0.0017(14) C1A 0.0285(18) 0.0320(19) 0.039(2) -0.0012(16) 0.0000(15) -0.0067(15) C2A 0.0264(16) 0.0331(19) 0.0373(19) 0.0028(15) 0.0006(14) -0.0012(15) C3A 0.035(2) 0.035(2) 0.045(2) -0.0035(18) -0.0047(17) 0.0009(17) C4A 0.033(2) 0.038(2) 0.042(2) -0.0010(18) 0.0071(16) 0.0011(17) C5A 0.0307(19) 0.038(2) 0.038(2) 0.0092(17) 0.0047(16) -0.0006(16) C6A 0.0284(18) 0.037(2) 0.036(2) 0.0047(17) 0.0036(15) -0.0044(16) C7A 0.033(2) 0.046(2) 0.039(2) 0.0050(18) -0.0027(16) -0.0035(18) C8A 0.043(2) 0.057(3) 0.038(2) 0.007(2) -0.0072(18) -0.008(2) C9A 0.037(2) 0.059(3) 0.051(3) 0.021(2) -0.0062(19) 0.007(2) C10A 0.037(2) 0.044(2) 0.049(2) 0.0116(19) 0.0042(18) 0.0068(19) C11A 0.0326(19) 0.042(2) 0.038(2) 0.0066(18) 0.0039(15) 0.0021(17) C12A 0.032(2) 0.152(7) 0.075(4) 0.065(4) 0.020(2) 0.029(3) C13A 0.030(2) 0.070(3) 0.058(3) 0.031(3) 0.0171(19) 0.007(2) C14A 0.055(3) 0.055(3) 0.087(4) 0.016(3) 0.038(3) 0.018(3) C15A 0.059(3) 0.066(3) 0.066(3) -0.012(3) 0.021(3) -0.013(3) C16A 0.031(2) 0.063(3) 0.051(3) 0.007(2) -0.0016(18) -0.003(2) C17A 0.037(2) 0.048(3) 0.052(3) 0.011(2) 0.0029(18) 0.0023(19) C18A 0.033(2) 0.059(3) 0.045(2) 0.010(2) 0.0003(18) -0.008(2) B1A 0.029(2) 0.035(2) 0.037(2) 0.0026(18) 0.0022(17) -0.0061(18) O1B 0.0440(15) 0.0558(18) 0.0403(16) -0.0085(15) -0.0051(13) -0.0024(15) O2B 0.0419(15) 0.0400(16) 0.0382(15) -0.0103(12) -0.0061(12) -0.0015(13) O3B 0.0374(15) 0.056(2) 0.0534(19) 0.0242(15) 0.0034(13) -0.0017(14) O4B 0.0454(17) 0.0500(19) 0.058(2) 0.0241(16) -0.0065(14) -0.0046(15) N1B 0.0370(16) 0.0314(16) 0.0329(16) -0.0021(14) 0.0013(13) -0.0042(14) N2B 0.0411(18) 0.0384(18) 0.0348(17) -0.0080(15) 0.0015(14) -0.0012(15) N3B 0.043(2) 0.0411(19) 0.039(2) 0.0149(17) 0.0024(15) 0.0021(16) C1B 0.0348(19) 0.037(2) 0.0312(19) 0.0013(16) 0.0026(15) -0.0067(17) C2B 0.036(2) 0.036(2) 0.039(2) 0.0032(16) 0.0002(16) -0.0048(16) C3B 0.042(2) 0.038(2) 0.044(2) -0.0044(18) -0.0019(18) 0.0031(18) C4B 0.046(2) 0.038(2) 0.033(2) -0.0037(17) 0.0057(17) 0.0028(18) C5B 0.037(2) 0.035(2) 0.0336(19) 0.0025(16) 0.0036(16) -0.0049(17) C6B 0.0358(19) 0.0335(19) 0.0342(19) 0.0034(16) 0.0037(15) -0.0071(17) C7B 0.045(2) 0.039(2) 0.035(2) -0.0021(17) -0.0009(17) -0.0071(19) C8B 0.046(2) 0.045(2) 0.041(2) 0.005(2) -0.0046(18) -0.009(2) C9B 0.045(2) 0.043(2) 0.042(2) 0.0127(19) -0.0036(18) -0.0045(19) C10B 0.046(2) 0.038(2) 0.039(2) 0.0069(18) 0.0039(18) 0.0005(19) C11B 0.039(2) 0.037(2) 0.046(2) 0.0064(19) 0.0013(17) 0.0031(18) C12B 0.040(2) 0.077(4) 0.080(4) 0.044(3) 0.002(2) -0.003(2) C13B 0.038(2) 0.063(3) 0.068(3) 0.036(3) 0.023(2) 0.014(2) C14B 0.046(3) 0.123(6) 0.078(4) 0.030(4) 0.014(3) 0.002(4) C15B 0.067(4) 0.107(6) 0.084(5) 0.007(5) 0.016(3) -0.004(4) C16B 0.084(4) 0.073(4) 0.087(5) 0.025(4) 0.030(4) 0.008(4) C17B 0.039(3) 0.063(3) 0.085(4) 0.019(3) 0.019(2) 0.008(2) C18B 0.085(5) 0.068(4) 0.105(5) 0.017(4) 0.045(4) -0.002(4) B1B 0.040(2) 0.032(2) 0.032(2) -0.0019(18) 0.0030(17) -0.0080(19) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle B1A O2A C3A 118.9(3) C11A O3A C12A 113.6(3) N2A N1A C1A 114.1(3) N2A N1A B1A 123.5(3) C1A N1A B1A 122.4(3) C4A N2A N1A 117.0(3) C2A N3A H3A 124(4) C11A N3A H3A 117(4) C11A N3A C2A 118.2(3) O1A C1A N1A 123.8(4) O1A C1A C2A 125.1(4) N1A C1A C2A 111.0(3) N3A C2A C1A 114.3(3) N3A C2A H2A 106.0 N3A C2A C3A 112.2(3) C1A C2A H2A 106.0 C1A C2A C3A 111.6(3) C3A C2A H2A 106.0 O2A C3A C2A 110.0(3) O2A C3A H3AA 109.7 O2A C3A H3AB 109.7 C2A C3A H3AA 109.7 C2A C3A H3AB 109.7 H3AA C3A H3AB 108.2 N2A C4A H4A 116.3 N2A C4A C5A 127.4(4) C5A C4A H4A 116.3 C6A C5A C4A 119.0(4) C6A C5A C10A 120.5(4) C10A C5A C4A 120.6(4) C5A C6A C7A 118.9(4) C5A C6A B1A 116.2(4) C7A C6A B1A 124.9(4) C6A C7A H7A 120.0 C8A C7A C6A 120.1(4) C8A C7A H7A 120.0 C7A C8A H8A 119.6 C9A C8A C7A 120.8(4) C9A C8A H8A 119.6 C8A C9A H9A 119.9 C8A C9A C10A 120.2(4) C10A C9A H9A 119.9 C5A C10A H10A 120.2 C9A C10A C5A 119.5(5) C9A C10A H10A 120.2 O4A C11A O3A 123.4(4) O4A C11A N3A 124.9(4) N3A C11A O3A 111.7(3) O3A C12A H12A 109.8 O3A C12A H12B 109.8 O3A C12A C13A 109.2(4) H12A C12A H12B 108.3 C13A C12A H12A 109.8 C13A C12A H12B 109.8 C14A C13A C12A 120.5(6) C18A C13A C12A 119.9(6) C18A C13A C14A 119.5(5) C13A C14A H14A 120.2 C13A C14A C15A 119.6(5) C15A C14A H14A 120.2 C14A C15A H15A 120.0 C16A C15A C14A 120.0(5) C16A C15A H15A 120.0 C15A C16A H16A 120.2 C17A C16A C15A 119.6(5) C17A C16A H16A 120.2 C16A C17A H17A 119.6 C16A C17A C18A 120.7(5) C18A C17A H17A 119.6 C13A C18A C17A 120.5(5) C13A C18A H18A 119.7 C17A C18A H18A 119.7 O2A B1A N1A 120.9(4) O2A B1A C6A 122.5(4) N1A B1A C6A 116.6(4) B1B O2B C3B 119.3(3) C11B O3B C12B 113.4(3) N2B N1B B1B 123.1(3) C1B N1B N2B 113.8(3) C1B N1B B1B 123.1(4) C4B N2B N1B 117.3(3) C2B N3B H3B 117(4) C11B N3B H3B 119(4) C11B N3B C2B 122.4(4) O1B C1B N1B 123.7(4) O1B C1B C2B 123.1(4) N1B C1B C2B 113.0(3) N3B C2B C1B 113.2(3) N3B C2B H2B 106.5 N3B C2B C3B 110.5(3) C1B C2B H2B 106.5 C1B C2B C3B 113.3(3) C3B C2B H2B 106.5 O2B C3B C2B 111.9(4) O2B C3B H3BA 109.2 O2B C3B H3BB 109.2 C2B C3B H3BA 109.2 C2B C3B H3BB 109.2 H3BA C3B H3BB 107.9 N2B C4B H4B 116.1 N2B C4B C5B 127.7(4) C5B C4B H4B 116.1 C6B C5B C4B 118.7(4) C6B C5B C10B 120.3(4) C10B C5B C4B 121.0(4) C5B C6B B1B 116.7(4) C7B C6B C5B 119.0(4) C7B C6B B1B 124.3(4) C6B C7B H7B 119.6 C8B C7B C6B 120.7(4) C8B C7B H7B 119.6 C7B C8B H8B 119.9 C7B C8B C9B 120.1(4) C9B C8B H8B 119.9 C8B C9B H9B 119.9 C10B C9B C8B 120.3(4) C10B C9B H9B 119.9 C5B C10B H10B 120.3 C9B C10B C5B 119.5(4) C9B C10B H10B 120.3 O4B C11B O3B 124.1(4) O4B C11B N3B 125.6(4) N3B C11B O3B 110.3(4) O3B C12B H12C 110.0 O3B C12B H12D 110.0 O3B C12B C13B 108.6(4) H12C C12B H12D 108.4 C13B C12B H12C 110.0 C13B C12B H12D 110.0 C14B C13B C12B 117.5(6) C18B C13B C12B 127.6(7) C18B C13B C14B 114.9(6) C13B C14B H14B 115.9 C15B C14B C13B 128.2(8) C15B C14B H14B 115.9 C14B C15B H15B 122.4 C16B C15B C14B 115.3(9) C16B C15B H15B 122.4 C15B C16B H16B 117.4 C15B C16B C17B 125.3(8) C17B C16B H16B 117.4 C16B C17B H17B 122.1 C16B C17B C18B 115.9(6) C18B C17B H17B 122.1 C13B C18B C17B 120.3(7) C13B C18B H18B 119.9 C17B C18B H18B 119.9 O2B B1B N1B 120.8(4) O2B B1B C6B 122.5(4) N1B B1B C6B 116.6(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1A C1A 1.197(5) O2A C3A 1.433(5) O2A B1A 1.359(6) O3A C11A 1.352(5) O3A C12A 1.437(5) O4A C11A 1.213(5) N1A N2A 1.391(5) N1A C1A 1.400(5) N1A B1A 1.458(6) N2A C4A 1.285(5) N3A H3A 0.83(6) N3A C2A 1.432(5) N3A C11A 1.336(5) C1A C2A 1.525(6) C2A H2A 1.0000 C2A C3A 1.530(5) C3A H3AA 0.9900 C3A H3AB 0.9900 C4A H4A 0.9500 C4A C5A 1.462(6) C5A C6A 1.394(6) C5A C10A 1.402(6) C6A C7A 1.404(6) C6A B1A 1.536(6) C7A H7A 0.9500 C7A C8A 1.385(6) C8A H8A 0.9500 C8A C9A 1.375(8) C9A H9A 0.9500 C9A C10A 1.388(7) C10A H10A 0.9500 C12A H12A 0.9900 C12A H12B 0.9900 C12A C13A 1.509(7) C13A C14A 1.388(9) C13A C18A 1.369(7) C14A H14A 0.9500 C14A C15A 1.391(8) C15A H15A 0.9500 C15A C16A 1.386(8) C16A H16A 0.9500 C16A C17A 1.358(7) C17A H17A 0.9500 C17A C18A 1.381(6) C18A H18A 0.9500 O1B C1B 1.209(5) O2B C3B 1.427(5) O2B B1B 1.357(6) O3B C11B 1.355(5) O3B C12B 1.456(6) O4B C11B 1.206(5) N1B N2B 1.402(5) N1B C1B 1.394(5) N1B B1B 1.453(5) N2B C4B 1.288(6) N3B H3B 0.74(5) N3B C2B 1.446(5) N3B C11B 1.350(6) C1B C2B 1.526(6) C2B H2B 1.0000 C2B C3B 1.533(6) C3B H3BA 0.9900 C3B H3BB 0.9900 C4B H4B 0.9500 C4B C5B 1.444(6) C5B C6B 1.403(6) C5B C10B 1.405(6) C6B C7B 1.391(6) C6B B1B 1.536(6) C7B H7B 0.9500 C7B C8B 1.382(6) C8B H8B 0.9500 C8B C9B 1.398(7) C9B H9B 0.9500 C9B C10B 1.383(6) C10B H10B 0.9500 C12B H12C 0.9900 C12B H12D 0.9900 C12B C13B 1.487(7) C13B C14B 1.388(10) C13B C18B 1.371(9) C14B H14B 0.9500 C14B C15B 1.356(9) C15B H15B 0.9500 C15B C16B 1.329(11) C16B H16B 0.9500 C16B C17B 1.380(10) C17B H17B 0.9500 C17B C18B 1.489(9) C18B H18B 0.9500 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 N3A H3A N2A 0.83(6) 2.27(6) 3.080(5) 165(5) 2_646 yes N3B H3B N2B 0.74(5) 2.26(5) 2.977(5) 164(5) 2 yes C3B H3BB O4B 0.99 2.31 2.958(5) 122.2 . 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 O1A C1A C2A N3A 8.9(6) O1A C1A C2A C3A 137.5(4) O3A C12A C13A C14A -71.3(8) O3A C12A C13A C18A 111.6(6) N1A N2A C4A C5A -1.0(6) N1A C1A C2A N3A -174.7(3) N1A C1A C2A C3A -46.1(4) N2A N1A C1A O1A 12.1(6) N2A N1A C1A C2A -164.4(3) N2A N1A B1A O2A -174.0(3) N2A N1A B1A C6A 6.8(5) N2A C4A C5A C6A 2.6(7) N2A C4A C5A C10A -178.0(4) N3A C2A C3A O2A -172.0(3) C1A N1A N2A C4A 174.5(4) C1A N1A B1A O2A 7.6(6) C1A N1A B1A C6A -171.6(3) C1A C2A C3A O2A 58.3(4) C2A N3A C11A O3A -179.0(4) C2A N3A C11A O4A 2.4(7) C3A O2A B1A N1A 5.3(6) C3A O2A B1A C6A -175.6(4) C4A C5A C6A C7A 179.9(4) C4A C5A C6A B1A 0.5(5) C4A C5A C10A C9A -179.9(4) C5A C6A C7A C8A 0.4(6) C5A C6A B1A O2A 176.1(4) C5A C6A B1A N1A -4.7(5) C6A C5A C10A C9A -0.6(6) C6A C7A C8A C9A -1.4(7) C7A C6A B1A O2A -3.2(6) C7A C6A B1A N1A 176.0(4) C7A C8A C9A C10A 1.3(7) C8A C9A C10A C5A -0.3(7) C10A C5A C6A C7A 0.5(6) C10A C5A C6A B1A -178.8(4) C11A O3A C12A C13A 167.0(5) C11A N3A C2A C1A -126.6(4) C11A N3A C2A C3A 105.1(4) C12A O3A C11A O4A -2.0(8) C12A O3A C11A N3A 179.4(5) C12A C13A C14A C15A -178.2(5) C12A C13A C18A C17A 178.4(4) C13A C14A C15A C16A -0.1(8) C14A C13A C18A C17A 1.3(7) C14A C15A C16A C17A 1.3(8) C15A C16A C17A C18A -1.2(7) C16A C17A C18A C13A -0.1(7) C18A C13A C14A C15A -1.1(7) B1A O2A C3A C2A -37.3(5) B1A N1A N2A C4A -4.0(6) B1A N1A C1A O1A -169.3(4) B1A N1A C1A C2A 14.2(5) B1A C6A C7A C8A 179.7(4) O1B C1B C2B N3B 21.7(6) O1B C1B C2B C3B 148.5(4) O3B C12B C13B C14B 94.0(7) O3B C12B C13B C18B -89.7(7) N1B N2B C4B C5B 0.0(7) N1B C1B C2B N3B -163.8(3) N1B C1B C2B C3B -37.1(5) N2B N1B C1B O1B 6.7(6) N2B N1B C1B C2B -167.8(3) N2B N1B B1B O2B -178.3(4) N2B N1B B1B C6B 1.0(6) N2B C4B C5B C6B 0.3(7) N2B C4B C5B C10B -178.2(4) N3B C2B C3B O2B 178.5(3) C1B N1B N2B C4B 178.4(4) C1B N1B B1B O2B 2.6(6) C1B N1B B1B C6B -178.1(3) C1B C2B C3B O2B 50.3(5) C2B N3B C11B O3B -179.1(4) C2B N3B C11B O4B 2.2(8) C3B O2B B1B N1B 11.6(6) C3B O2B B1B C6B -167.7(4) C4B C5B C6B C7B 179.1(4) C4B C5B C6B B1B 0.0(6) C4B C5B C10B C9B 178.6(4) C5B C6B C7B C8B 2.8(6) C5B C6B B1B O2B 178.7(4) C5B C6B B1B N1B -0.6(6) C6B C5B C10B C9B 0.0(6) C6B C7B C8B C9B -1.1(7) C7B C6B B1B O2B -0.4(7) C7B C6B B1B N1B -179.7(4) C7B C8B C9B C10B -1.2(7) C8B C9B C10B C5B 1.7(7) C10B C5B C6B C7B -2.3(6) C10B C5B C6B B1B 178.6(4) C11B O3B C12B C13B -179.6(5) C11B N3B C2B C1B 69.9(5) C11B N3B C2B C3B -58.3(5) C12B O3B C11B O4B 1.2(7) C12B O3B C11B N3B -177.5(5) C12B C13B C14B C15B 177.0(6) C12B C13B C18B C17B 179.7(5) C13B C14B C15B C16B 2.7(11) C14B C13B C18B C17B -3.9(8) C14B C15B C16B C17B -1.7(11) C15B C16B C17B C18B -1.7(9) C16B C17B C18B C13B 4.7(8) C18B C13B C14B C15B 0.2(10) B1B O2B C3B C2B -37.5(5) B1B N1B N2B C4B -0.7(6) B1B N1B C1B O1B -174.2(4) B1B N1B C1B C2B 11.4(5) B1B C6B C7B C8B -178.1(4)