#------------------------------------------------------------------------------ #$Date: 2021-06-04 04:06:30 +0300 (Fri, 04 Jun 2021) $ #$Revision: 265769 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/23/1562362.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_1562362 loop_ _publ_author_name 'Corbin, Daniel A.' 'Puffer, Katherine O.' 'Chism, Katherine A.' 'Cole, Justin P.' 'Theriot, Jordan C.' 'McCarthy, Blaine G.' 'Buss, Bonnie L.' 'Lim, Chern-Hooi' 'Lincoln, Sarah R.' 'Newell, Brian S.' 'Miyake, Garret M.' _publ_section_title ; Radical Addition to N,N-Diaryl Dihydrophenazine Photoredox Catalysts and Implications in Photoinduced Organocatalyzed Atom Transfer Radical Polymerization ; _journal_issue 10 _journal_name_full Macromolecules _journal_page_first 4507 _journal_page_last 4516 _journal_paper_doi 10.1021/acs.macromol.1c00501 _journal_volume 54 _journal_year 2021 _chemical_formula_moiety 'C66 H56 F6 N2 O8' _chemical_formula_sum 'C66 H56 F6 N2 O8' _chemical_formula_weight 1119.12 _chemical_name_common JC-1-93 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2021-03-03 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _cell_angle_alpha 114.080(4) _cell_angle_beta 93.910(4) _cell_angle_gamma 102.462(4) _cell_formula_units_Z 1 _cell_length_a 6.5181(6) _cell_length_b 14.7409(12) _cell_length_c 16.2314(13) _cell_measurement_reflns_used 5490 _cell_measurement_temperature 104.(2) _cell_measurement_theta_max 25.1532 _cell_measurement_theta_min 2.5138 _cell_volume 1368.8(2) _computing_cell_refinement 'SAINT V8.40A (Bruker Nano, Inc., 2019)' _computing_data_collection 'Bruker Instrument Service V6.2.6 (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.40A (Bruker Nano, Inc., 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 104.(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 QUEST' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'curved graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1100 _diffrn_reflns_av_unetI/netI 0.0563 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 51869 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.51 _diffrn_source 'sealed tube' _diffrn_source_type 'Siemans KFF Mo2K-90' _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.108 _exptl_crystal_size_mid 0.049 _exptl_crystal_size_min 0.026 _refine_diff_density_max 0.406 _refine_diff_density_min -0.231 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 372 _refine_ls_number_reflns 4844 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.014 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0568 _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^)+(0.0649P)^2^+1.4421P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1310 _refine_ls_wR_factor_ref 0.1563 _reflns_number_gt 3099 _reflns_number_total 4844 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ma1c00501_si_002.cif _cod_data_source_block gm15 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 1562361--1562362.cif. ; _cod_database_code 1562362 _olex2_refinement_description ; 1.a Ternary CH refined with riding coordinates: C7(H7), C17(H17) 1.b Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C25(H25A,H25B) 1.c Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C28(H28), C29(H29), C31(H31), C32(H32) 1.d Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C26(H26A,H26B,H26C) ; _shelx_res_file ; TITL gm15_a.res in P-1 gm15_a.res created by SHELXL-2018/3 at 21:05:58 on 17-Sep-2020 REM Old TITL gm15 in P-1 REM SHELXT solution in P-1 REM R1 0.187, Rweak 0.016, Alpha 0.043, Orientation as input REM Formula found by SHELXT: C33 F3 N O4 CELL 0.71073 6.5181 14.7409 16.2314 114.080 93.910 102.462 ZERR 1.000 0.0006 0.0012 0.0013 0.004 0.004 0.004 LATT 1 SFAC C H F N O UNIT 66 56 6 2 8 TEMP -169.010 SIZE 0.026 0.049 0.108 L.S. 10 BOND $H EQIV $2 x+1, y, z HTAB C7 O3_$2 EQIV $3 x-1, y-1, z-1 HTAB C26 F3_$3 CONF LIST 4 ACTA FMAP 2 PLAN 5 WGHT 0.064900 1.442100 FVAR 0.62157 F1 3 0.986478 0.961092 0.627348 11.00000 0.03530 0.05108 = 0.11358 0.03641 0.00616 -0.01345 F2 3 0.772019 0.985561 0.540557 11.00000 0.08259 0.03860 = 0.04520 0.02220 0.01117 -0.01956 F3 3 0.764396 1.045589 0.682960 11.00000 0.08708 0.02449 = 0.05294 -0.00349 0.03108 -0.01290 O1 5 0.089734 0.510044 0.147896 11.00000 0.03686 0.05098 = 0.02764 0.01966 0.00928 0.01962 O2 5 0.315031 0.432483 0.064905 11.00000 0.03537 0.03691 = 0.01885 0.01340 0.00799 0.00949 O3 5 -0.341061 0.296266 0.143848 11.00000 0.03621 0.04000 = 0.02868 0.01157 0.00635 0.01163 O4 5 -0.179171 0.252957 0.021402 11.00000 0.03852 0.03616 = 0.02234 0.01013 0.00425 0.00912 N1 4 0.169977 0.588571 0.530812 11.00000 0.03726 0.02481 = 0.01520 0.00307 0.00955 -0.01256 C1 1 0.137103 0.512853 0.439829 11.00000 0.02795 0.02287 = 0.01694 0.00793 0.00504 0.00082 C2 1 -0.029903 0.423185 0.409976 11.00000 0.02681 0.02479 = 0.01665 0.01150 0.00501 0.00024 C3 1 0.265952 0.525523 0.379226 11.00000 0.02357 0.02000 = 0.01927 0.00935 0.00351 -0.00084 AFIX 43 H3 2 0.380527 0.586201 0.400092 11.00000 -1.20000 AFIX 0 C4 1 -0.057814 0.348826 0.320908 11.00000 0.02356 0.01961 = 0.01864 0.00771 0.00228 -0.00174 AFIX 43 H4 2 -0.168313 0.286781 0.301016 11.00000 -1.20000 AFIX 0 C5 1 0.233691 0.452103 0.288123 11.00000 0.02147 0.02380 = 0.01974 0.01291 0.00510 0.00496 C6 1 0.070811 0.361900 0.259356 11.00000 0.02437 0.02011 = 0.01829 0.00839 0.00381 0.00353 C7 1 0.374291 0.473619 0.222836 11.00000 0.02508 0.02211 = 0.01746 0.00815 0.00733 0.00321 AFIX 13 H7 2 0.445395 0.416685 0.197652 11.00000 -1.20000 AFIX 0 C8 1 0.547204 0.575180 0.268959 11.00000 0.02548 0.02907 = 0.01631 0.01217 0.00823 0.00344 C9 1 0.500922 0.668955 0.289997 11.00000 0.02965 0.02904 = 0.02515 0.01473 0.00901 0.00366 AFIX 43 H9 2 0.359556 0.670172 0.272927 11.00000 -1.20000 AFIX 0 C10 1 0.659177 0.760820 0.335690 11.00000 0.04358 0.02688 = 0.02955 0.01454 0.01223 0.00723 AFIX 43 H10 2 0.625461 0.824572 0.350204 11.00000 -1.20000 AFIX 0 C11 1 0.863415 0.760063 0.359939 11.00000 0.03872 0.02857 = 0.02705 0.01037 0.00366 -0.00627 AFIX 43 H11 2 0.971649 0.823035 0.391729 11.00000 -1.20000 AFIX 0 C12 1 0.911241 0.666891 0.337824 11.00000 0.02590 0.04006 = 0.02855 0.01607 0.00101 0.00065 AFIX 43 H12 2 1.053753 0.665969 0.353290 11.00000 -1.20000 AFIX 0 C13 1 0.753769 0.575116 0.293449 11.00000 0.03201 0.02717 = 0.02458 0.01342 0.00587 0.00609 AFIX 43 H13 2 0.788031 0.511620 0.279739 11.00000 -1.20000 AFIX 0 C14 1 0.241203 0.475140 0.142629 11.00000 0.02626 0.02385 = 0.02146 0.01004 0.00805 0.00110 C15 1 0.201314 0.432026 -0.015852 11.00000 0.03887 0.03521 = 0.02101 0.01462 0.00436 0.01088 AFIX 23 H15A 2 0.249073 0.500465 -0.015919 11.00000 -1.20000 H15B 2 0.046021 0.416938 -0.015251 11.00000 -1.20000 AFIX 0 C16 1 0.246378 0.351666 -0.099006 11.00000 0.04422 0.04325 = 0.02415 0.01391 0.00499 0.01124 AFIX 137 H16A 2 0.171378 0.350730 -0.153888 11.00000 -1.50000 H16B 2 0.197176 0.284088 -0.098784 11.00000 -1.50000 H16C 2 0.400281 0.367215 -0.099152 11.00000 -1.50000 AFIX 0 C17 1 0.019753 0.278755 0.160288 11.00000 0.02770 0.02135 = 0.01970 0.00680 0.00851 0.00244 AFIX 13 H17 2 0.138128 0.295704 0.128512 11.00000 -1.20000 AFIX 0 C18 1 0.001349 0.170184 0.151578 11.00000 0.03602 0.02041 = 0.02298 0.00481 -0.00093 0.00096 C19 1 0.171577 0.128272 0.130037 11.00000 0.03159 0.02989 = 0.05339 0.01630 0.00161 0.00591 AFIX 43 H19 2 0.298855 0.168456 0.123432 11.00000 -1.20000 AFIX 0 C20 1 0.159506 0.028486 0.117915 11.00000 0.04270 0.04133 = 0.08344 0.02338 0.00231 0.01599 AFIX 43 H20 2 0.277145 0.000318 0.102332 11.00000 -1.20000 AFIX 0 C21 1 -0.022835 -0.029481 0.128487 11.00000 0.05345 0.03436 = 0.08655 0.02859 0.00026 0.01025 AFIX 43 H21 2 -0.031719 -0.097917 0.120240 11.00000 -1.20000 AFIX 0 C22 1 -0.191947 0.011378 0.150927 11.00000 0.05200 0.03355 = 0.05729 0.02074 0.00272 -0.00227 AFIX 43 H22 2 -0.316374 -0.028361 0.159878 11.00000 -1.20000 AFIX 0 C23 1 -0.183720 0.110760 0.160815 11.00000 0.04019 0.02767 = 0.03386 0.01201 0.00701 0.00187 AFIX 43 H23 2 -0.304044 0.137466 0.173775 11.00000 -1.20000 AFIX 0 C24 1 -0.186899 0.279392 0.110244 11.00000 0.03650 0.02168 = 0.01721 0.00453 0.00478 -0.00081 C25 1 -0.375380 0.244955 -0.032988 11.00000 0.03606 0.03895 = 0.03125 0.01336 -0.00500 0.00857 AFIX 23 H25A 2 -0.411539 0.311888 -0.008632 11.00000 -1.20000 H25B 2 -0.494861 0.192231 -0.030557 11.00000 -1.20000 AFIX 0 C26 1 -0.339859 0.215239 -0.129160 11.00000 0.05238 0.04737 = 0.03062 0.01554 0.00121 0.01182 AFIX 137 H26A 2 -0.295137 0.151243 -0.151230 11.00000 -1.50000 H26B 2 -0.228385 0.270241 -0.131427 11.00000 -1.50000 H26C 2 -0.472679 0.204677 -0.168117 11.00000 -1.50000 AFIX 0 C27 1 0.325584 0.685104 0.557444 11.00000 0.03206 0.02069 = 0.01075 0.00310 0.00676 -0.00564 C28 1 0.263819 0.764472 0.547006 11.00000 0.02410 0.03655 = 0.02221 0.01127 0.00308 -0.00067 AFIX 43 H28 2 0.118019 0.756248 0.526547 11.00000 -1.20000 AFIX 0 C29 1 0.413901 0.855646 0.566298 11.00000 0.03841 0.02695 = 0.03166 0.01677 0.00882 0.00598 AFIX 43 H29 2 0.372359 0.910122 0.558772 11.00000 -1.20000 AFIX 0 C30 1 0.626238 0.866786 0.596826 11.00000 0.02942 0.02355 = 0.02205 0.00711 0.00702 -0.00380 C31 1 0.685463 0.789158 0.610651 11.00000 0.02666 0.02913 = 0.03107 0.01122 0.00159 -0.00074 AFIX 43 H31 2 0.829919 0.798190 0.633825 11.00000 -1.20000 AFIX 0 C32 1 0.534034 0.698014 0.590701 11.00000 0.03477 0.02200 = 0.02648 0.01168 0.00439 0.00108 AFIX 43 H32 2 0.574566 0.644311 0.600062 11.00000 -1.20000 AFIX 0 C33 1 0.786304 0.964073 0.612762 11.00000 0.04042 0.02694 = 0.03385 0.01097 0.00811 -0.00468 HKLF 4 REM gm15_a.res in P-1 REM wR2 = 0.156316, GooF = S = 1.01415, Restrained GooF = 1.01415 for all data REM R1 = 0.056754 for 3099 Fo > 4sig(Fo) and 0.104118 for all 4844 data REM 372 parameters refined using 0 restraints END WGHT 0.0649 1.4422 REM Highest difference peak 0.406, deepest hole -0.231, 1-sigma level 0.058 Q1 1 -0.0552 0.2001 0.0002 11.00000 0.05 0.41 Q2 1 0.9062 0.9635 0.5604 11.00000 0.05 0.36 Q3 1 0.1251 0.1536 0.1884 11.00000 0.05 0.35 Q4 1 -0.0302 0.1375 0.2197 11.00000 0.05 0.35 Q5 1 0.9210 1.0057 0.6885 11.00000 0.05 0.34 ; _shelx_res_checksum 28715 _shelx_hkl_file ; -1 0 0 1291.87 82.69 -1 0 0 1237.48 82.79 -1 0 0 1343.67 82.89 -1 0 0 1271.87 82.59 -1 0 0 1332.27 82.99 -1 0 0 1301.57 82.59 -1 0 0 1192.68 82.59 -1 0 0 1145.89 82.99 -1 0 0 1007.80 82.79 1 0 0 1285.17 82.89 1 0 0 1292.27 82.59 1 0 0 1169.58 82.49 1 0 0 1319.47 82.89 1 0 0 1171.48 82.69 1 0 0 1266.27 82.59 1 0 0 1271.07 82.79 1 0 0 1287.67 82.69 1 0 0 1210.88 82.89 -2 0 0 1456.45 103.19 -2 0 0 1551.84 102.99 -2 0 0 1576.04 103.59 -2 0 0 1585.54 103.19 -2 0 0 1719.73 103.99 -2 0 0 1526.15 103.09 -2 0 0 1455.25 103.89 2 0 0 1595.04 103.49 2 0 0 1544.45 103.89 2 0 0 1591.44 103.19 2 0 0 1585.24 103.79 2 0 0 1491.05 102.99 2 0 0 1559.04 103.29 2 0 0 1559.54 103.79 2 0 0 1519.95 103.69 2 0 0 1476.95 103.89 -3 0 0 16.50 6.30 -3 0 0 17.80 6.40 -3 0 0 21.60 8.40 -3 0 0 12.10 6.90 -3 0 0 12.10 9.20 -3 0 0 21.80 6.50 -3 0 0 27.80 9.00 3 0 0 19.40 9.20 3 0 0 8.00 7.20 3 0 0 26.50 10.90 3 0 0 15.60 8.10 3 0 0 26.80 9.60 3 0 0 9.30 9.40 3 0 0 27.60 7.80 3 0 0 20.50 7.10 3 0 0 27.50 7.10 -4 0 0 96.29 15.00 -4 0 0 110.49 11.80 -4 0 0 110.39 11.50 -4 0 0 112.69 10.70 -4 0 0 97.39 12.80 4 0 0 96.89 11.40 4 0 0 87.29 13.80 4 0 0 119.19 12.60 4 0 0 96.49 12.60 4 0 0 99.69 14.10 4 0 0 99.49 14.30 4 0 0 138.99 12.60 -5 0 0 126.29 11.70 -5 0 0 78.69 12.50 -5 0 0 114.49 15.40 -5 0 0 92.79 12.20 -5 0 0 66.79 17.20 -5 0 0 125.49 12.10 5 0 0 123.09 13.80 5 0 0 117.59 16.60 5 0 0 82.69 16.20 5 0 0 91.49 16.20 5 0 0 103.99 13.70 5 0 0 92.39 16.00 5 0 0 115.89 13.70 -6 0 0 46.70 17.60 -6 0 0 51.19 10.50 -6 0 0 54.19 11.10 -6 0 0 43.90 11.70 -6 0 0 62.89 14.90 6 0 0 62.39 16.90 6 0 0 32.70 15.50 6 0 0 33.90 13.70 6 0 0 30.70 16.10 6 0 0 47.80 16.40 6 0 0 26.10 16.40 -7 0 0 19.00 16.80 -7 0 0 34.60 10.60 7 0 0 46.00 14.50 7 0 0 29.70 18.70 7 0 0 26.60 15.40 7 0 0 35.60 18.80 7 0 0 31.60 18.30 7 -1 0 -28.40 16.00 7 -1 0 11.10 13.20 7 -1 0 -2.60 13.40 7 -1 0 25.70 18.10 7 -1 0 -18.20 17.40 -7 1 0 6.10 12.10 -7 1 0 9.60 9.00 -7 1 0 -9.80 16.20 6 -1 0 23.10 14.80 6 -1 0 27.10 15.00 6 -1 0 -3.90 14.70 6 -1 0 -7.60 14.90 -6 1 0 10.60 10.00 -6 1 0 17.40 13.60 -6 1 0 14.40 15.00 -6 1 0 7.70 10.80 -6 1 0 -0.40 8.50 -6 1 0 8.50 10.20 5 -1 0 434.56 32.80 5 -1 0 453.35 33.60 5 -1 0 414.96 31.90 5 -1 0 393.26 34.50 5 -1 0 391.36 34.60 5 -1 0 422.36 34.40 5 -1 0 395.46 34.50 -5 1 0 416.26 32.40 -5 1 0 442.96 31.20 -5 1 0 408.66 34.20 -5 1 0 416.46 32.20 -5 1 0 387.66 35.80 4 -1 0 34.90 11.10 4 -1 0 29.40 11.00 4 -1 0 55.29 11.30 4 -1 0 33.80 9.20 4 -1 0 53.29 9.80 4 -1 0 34.30 9.40 4 -1 0 32.00 7.60 4 -1 0 41.40 11.40 -4 1 0 32.30 8.70 -4 1 0 47.00 7.80 -4 1 0 38.60 8.10 -4 1 0 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10.10 3 -5 0 36.60 8.90 3 -5 0 13.50 6.80 3 -5 0 9.60 11.30 3 -5 0 21.10 7.20 3 -5 0 12.10 8.80 3 -5 0 26.80 9.40 3 -5 0 5.60 10.00 3 -5 0 36.60 10.60 -3 5 0 23.20 9.40 -3 5 0 24.30 7.20 -3 5 0 19.70 8.10 -3 5 0 23.90 10.00 -3 5 0 18.30 9.70 -3 5 0 21.70 10.50 -3 5 0 31.40 11.50 -3 5 0 28.20 8.80 2 -5 0 317.17 26.10 2 -5 0 306.07 24.10 2 -5 0 294.37 24.90 2 -5 0 294.47 25.60 2 -5 0 358.06 26.50 2 -5 0 305.47 23.90 2 -5 0 324.57 24.80 -2 5 0 305.17 25.20 -2 5 0 323.27 24.70 -2 5 0 291.87 24.50 -2 5 0 318.47 25.20 -2 5 0 288.77 22.10 -2 5 0 313.87 25.70 -2 5 0 351.86 24.20 1 -5 0 65.89 10.50 1 -5 0 49.99 9.30 1 -5 0 47.30 10.40 1 -5 0 31.80 10.80 1 -5 0 49.00 10.30 -1 5 0 45.40 9.90 -1 5 0 58.09 5.20 -1 5 0 56.79 9.60 -1 5 0 40.60 9.90 -1 5 0 60.19 8.30 -1 5 0 50.49 10.40 -1 5 0 78.09 10.50 -1 5 0 58.29 8.20 0 -5 0 9.00 7.50 0 -5 0 -2.70 7.90 0 -5 0 4.70 9.60 0 -5 0 4.50 7.50 0 -5 0 11.10 5.50 0 -5 0 12.40 9.00 0 5 0 17.70 4.80 0 5 0 8.40 7.30 0 5 0 16.10 7.30 0 5 0 6.70 7.20 0 5 0 13.90 7.60 0 5 0 10.10 7.60 0 5 0 7.70 6.20 0 5 0 7.30 7.40 0 5 0 13.90 7.80 0 5 0 13.00 8.40 0 5 0 10.10 8.30 -1 -5 0 36.30 10.10 -1 -5 0 55.89 7.90 -1 -5 0 39.50 8.90 -1 -5 0 53.09 10.00 -1 -5 0 30.90 9.80 1 5 0 47.50 9.30 1 5 0 57.49 10.80 1 5 0 43.50 8.10 1 5 0 40.50 8.40 1 5 0 39.00 7.80 1 5 0 39.50 8.60 1 5 0 46.50 10.30 1 5 0 46.20 7.50 1 5 0 35.20 9.50 1 5 0 47.90 9.50 -2 -5 0 6.50 7.90 -2 -5 0 -0.20 9.40 -2 -5 0 15.00 6.40 -2 -5 0 4.60 5.80 -2 -5 0 8.20 9.90 -2 -5 0 -10.50 9.90 2 5 0 15.40 6.60 2 5 0 18.50 8.80 2 5 0 7.60 9.60 2 5 0 11.40 9.40 2 5 0 12.30 9.60 2 5 0 -3.10 7.60 2 5 0 0.30 10.80 2 5 0 12.10 6.70 2 5 0 1.30 6.40 -3 -5 0 15.10 7.30 -3 -5 0 22.60 9.50 -3 -5 0 10.30 9.50 -3 -5 0 4.90 11.80 3 5 0 6.70 9.60 3 5 0 -13.30 9.90 3 5 0 13.80 6.80 3 5 0 11.30 10.60 3 5 0 -8.40 10.70 3 5 0 14.20 9.80 3 5 0 8.80 6.70 3 5 0 2.00 6.90 -4 -5 0 31.50 12.10 -4 -5 0 1.20 12.00 -4 -5 0 18.70 9.80 -4 -5 0 34.50 10.50 -4 -5 0 32.00 15.20 4 5 0 57.49 8.80 4 5 0 27.40 12.50 4 5 0 44.50 8.80 4 5 0 17.90 14.40 4 5 0 20.50 13.30 4 5 0 9.60 13.50 4 5 0 16.80 8.70 4 5 0 41.70 8.70 -5 -5 0 -16.80 13.20 -5 -5 0 10.70 12.40 -5 -5 0 -1.80 11.00 5 5 0 7.80 15.30 5 5 0 -1.10 9.10 5 5 0 6.10 8.90 5 5 0 0.60 13.30 5 5 0 -11.20 16.20 5 5 0 5.80 9.30 5 5 0 -13.90 13.40 5 5 0 -9.60 9.40 5 5 0 11.20 15.00 -6 -5 0 -26.80 11.90 -6 -5 0 -8.80 12.80 -6 -5 0 20.90 14.90 6 5 0 -1.90 15.80 6 5 0 2.30 16.50 6 5 0 12.30 10.60 6 5 0 1.50 14.80 6 5 0 5.80 10.00 6 5 0 -1.70 17.40 6 5 0 -12.80 10.10 6 5 0 -15.00 16.50 7 -6 0 28.20 17.50 7 -6 0 5.20 13.20 7 -6 0 4.40 14.80 7 -6 0 -5.90 15.60 7 -6 0 3.80 12.80 7 -6 0 16.50 13.80 -7 6 0 22.10 17.20 -7 6 0 -18.50 14.30 -7 6 0 9.00 16.80 -7 6 0 -26.40 14.10 -7 6 0 8.90 13.90 6 -6 0 46.00 15.60 6 -6 0 80.79 16.70 6 -6 0 78.39 13.40 6 -6 0 77.49 14.50 6 -6 0 45.10 9.60 6 -6 0 73.59 16.10 6 -6 0 81.59 14.70 -6 6 0 50.79 14.80 -6 6 0 68.49 16.20 -6 6 0 51.19 14.70 -6 6 0 56.39 15.40 -6 6 0 66.99 16.10 5 -6 0 83.99 16.00 5 -6 0 89.59 15.10 5 -6 0 97.29 11.30 5 -6 0 95.89 13.60 5 -6 0 116.49 14.80 5 -6 0 108.59 16.60 -5 6 0 128.39 15.60 -5 6 0 117.49 14.60 -5 6 0 129.09 15.90 -5 6 0 116.09 15.40 -5 6 0 105.49 14.30 4 -6 0 39.60 10.60 4 -6 0 49.60 12.20 4 -6 0 47.20 11.80 4 -6 0 26.20 7.90 4 -6 0 48.90 10.80 4 -6 0 54.19 9.90 4 -6 0 53.69 9.20 4 -6 0 25.40 11.90 -4 6 0 54.79 12.60 -4 6 0 36.80 9.10 -4 6 0 23.20 11.20 -4 6 0 22.10 11.00 -4 6 0 43.50 12.30 -4 6 0 51.89 10.80 -4 6 0 47.20 13.20 3 -6 0 47.00 11.60 3 -6 0 61.79 14.90 3 -6 0 60.39 9.30 3 -6 0 52.29 7.00 3 -6 0 41.10 10.80 3 -6 0 30.70 11.20 3 -6 0 47.80 12.40 3 -6 0 51.99 9.60 -3 6 0 43.60 11.10 -3 6 0 56.79 10.30 -3 6 0 49.80 11.00 -3 6 0 45.10 9.60 -3 6 0 78.99 11.70 -3 6 0 39.40 10.90 2 -6 0 496.25 36.30 2 -6 0 458.15 37.50 2 -6 0 472.05 37.90 2 -6 0 500.65 36.30 2 -6 0 493.55 35.70 2 -6 0 543.95 37.40 2 -6 0 521.55 36.60 -2 6 0 493.85 33.60 -2 6 0 486.85 36.20 -2 6 0 552.54 37.10 -2 6 0 485.25 36.90 -2 6 0 441.76 36.70 -2 6 0 491.65 36.70 -2 6 0 511.15 36.50 1 -6 0 118.59 14.50 1 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11.90 2 6 0 2.80 7.10 2 6 0 14.80 7.40 2 6 0 10.50 9.00 -3 -6 0 -13.40 11.90 -3 -6 0 -1.70 11.50 -3 -6 0 1.80 9.00 -3 -6 0 -2.10 7.20 3 6 0 9.70 10.40 3 6 0 4.80 11.30 3 6 0 -5.30 9.40 3 6 0 -4.30 7.20 3 6 0 -7.40 11.00 3 6 0 -3.50 7.50 3 6 0 4.20 7.40 -4 -6 0 13.60 15.70 -4 -6 0 3.90 10.70 -4 -6 0 7.90 9.20 -4 -6 0 -4.60 11.90 4 6 0 11.90 8.70 4 6 0 -1.90 8.50 4 6 0 15.70 12.50 4 6 0 -10.30 8.20 4 6 0 -3.10 13.50 4 6 0 16.00 14.60 4 6 0 -4.70 8.20 4 6 0 -4.40 12.80 4 6 0 -0.40 12.30 -5 -6 0 -11.80 12.60 -5 -6 0 -4.20 12.00 -5 -6 0 1.60 14.10 -5 -6 0 -18.50 17.70 5 6 0 -3.10 14.40 5 6 0 5.50 14.50 5 6 0 24.90 10.30 5 6 0 -0.50 9.20 5 6 0 -0.70 9.50 5 6 0 20.10 9.80 5 6 0 24.20 16.30 5 6 0 -15.90 14.30 5 6 0 -3.30 15.80 -6 -6 0 -21.00 12.50 -6 -6 0 29.60 16.40 -6 -6 0 6.90 14.00 6 6 0 28.00 10.80 6 6 0 2.60 10.70 6 6 0 36.00 20.10 6 6 0 14.30 18.10 6 6 0 35.30 18.20 6 6 0 8.40 17.40 6 6 0 19.30 10.80 7 -7 0 24.60 14.20 7 -7 0 16.00 17.70 7 -7 0 8.00 9.40 7 -7 0 -4.00 15.10 7 -7 0 -11.00 14.60 7 -7 0 12.50 15.20 7 -7 0 -6.30 16.40 -7 7 0 17.80 15.70 -7 7 0 31.90 17.80 -7 7 0 19.90 16.90 -7 7 0 26.40 18.30 -7 7 0 30.10 15.70 6 -7 0 187.68 22.80 6 -7 0 232.68 19.30 6 -7 0 209.88 22.10 6 -7 0 190.08 21.70 6 -7 0 205.18 20.30 6 -7 0 204.38 21.60 6 -7 0 200.18 22.40 -6 7 0 185.88 21.40 -6 7 0 164.48 22.50 -6 7 0 212.18 22.30 -6 7 0 176.28 21.80 -6 7 0 201.78 20.50 5 -7 0 277.17 27.30 5 -7 0 251.47 26.70 5 -7 0 301.77 25.80 5 -7 0 223.78 23.50 5 -7 0 250.57 21.60 5 -7 0 271.07 26.60 5 -7 0 291.67 23.80 5 -7 0 265.37 25.90 -5 7 0 291.37 24.90 -5 7 0 269.87 24.20 -5 7 0 274.27 26.60 -5 7 0 230.18 23.70 -5 7 0 240.28 24.30 -5 7 0 217.88 23.90 4 -7 0 34.20 11.40 4 -7 0 14.60 8.20 4 -7 0 12.50 9.50 4 -7 0 27.40 10.10 4 -7 0 15.80 7.50 4 -7 0 17.30 9.70 4 -7 0 18.00 11.10 -4 7 0 27.60 13.70 -4 7 0 24.80 8.20 -4 7 0 12.90 10.90 -4 7 0 24.80 11.60 -4 7 0 17.10 10.60 3 -7 0 76.79 10.70 3 -7 0 60.19 13.50 3 -7 0 78.19 12.60 3 -7 0 49.50 12.70 3 -7 0 46.30 10.60 3 -7 0 62.19 9.90 -3 7 0 67.69 11.20 -3 7 0 68.49 11.70 -3 7 0 51.39 11.80 -3 7 0 70.09 11.30 -3 7 0 47.50 12.30 -3 7 0 81.09 12.80 -3 7 0 57.29 7.20 2 -7 0 6.10 10.70 2 -7 0 3.90 9.30 2 -7 0 -6.00 11.10 2 -7 0 8.90 9.20 2 -7 0 11.80 12.10 2 -7 0 21.50 9.40 2 -7 0 16.90 11.50 -2 7 0 1.40 8.10 -2 7 0 4.20 8.10 -2 7 0 -6.90 9.70 -2 7 0 -2.50 9.60 -2 7 0 2.00 3.50 -2 7 0 8.10 10.30 -2 7 0 13.80 10.40 -2 7 0 35.90 9.60 -2 7 0 6.80 3.10 1 -7 0 21.50 10.20 1 -7 0 32.80 9.40 1 -7 0 25.90 10.30 1 -7 0 21.30 9.30 1 -7 0 18.50 11.30 -1 7 0 22.10 9.70 -1 7 0 23.30 9.90 -1 7 0 42.20 10.10 -1 7 0 13.50 9.70 -1 7 0 15.80 10.10 -1 7 0 17.40 6.90 -1 7 0 18.50 4.90 -1 7 0 29.30 9.60 0 -7 0 328.97 27.30 0 -7 0 319.37 25.00 0 -7 0 343.37 26.70 0 -7 0 347.27 28.00 0 -7 0 375.26 26.90 0 -7 0 321.27 29.10 0 7 0 315.47 27.70 0 7 0 320.77 26.40 0 7 0 327.27 27.00 0 7 0 348.77 27.60 0 7 0 351.46 28.00 0 7 0 343.67 24.40 0 7 0 312.07 26.40 0 7 0 409.26 28.10 0 7 0 386.36 25.60 -1 -7 0 247.78 23.10 -1 -7 0 258.67 21.90 -1 -7 0 254.17 21.30 -1 -7 0 221.08 23.00 -1 -7 0 246.28 23.90 -1 -7 0 253.67 21.10 1 7 0 280.77 18.60 1 7 0 288.47 23.00 1 7 0 254.87 23.00 1 7 0 244.68 20.60 1 7 0 306.47 22.00 1 7 0 236.48 22.60 1 7 0 237.58 21.30 1 7 0 232.18 23.40 1 7 0 240.48 21.30 1 7 0 232.98 20.70 1 7 0 234.28 23.10 -2 -7 0 93.99 14.70 -2 -7 0 122.39 14.50 -2 -7 0 106.89 14.10 -2 -7 0 121.39 12.10 2 7 0 103.89 11.80 2 7 0 127.09 16.20 2 7 0 106.49 14.90 2 7 0 127.89 12.40 2 7 0 97.89 15.50 2 7 0 116.39 13.60 2 7 0 125.69 14.30 2 7 0 112.59 11.90 -3 -7 0 1.30 12.90 -3 -7 0 19.80 10.60 -3 -7 0 -1.80 13.00 -3 -7 0 5.10 7.10 3 7 0 -5.40 11.10 3 7 0 21.00 13.00 3 7 0 4.70 13.70 3 7 0 -0.50 8.10 3 7 0 10.80 14.70 3 7 0 -2.70 12.50 3 7 0 -5.30 8.40 3 7 0 -1.40 7.90 -4 -7 0 110.39 13.00 -4 -7 0 98.59 16.80 -4 -7 0 94.39 19.10 -4 -7 0 89.89 15.40 4 7 0 104.19 13.00 4 7 0 126.59 12.90 4 7 0 97.79 16.40 4 7 0 132.19 18.80 4 7 0 114.09 13.00 4 7 0 96.69 16.90 4 7 0 87.09 17.50 4 7 0 118.79 16.60 -5 -7 0 72.29 16.00 -5 -7 0 59.99 12.90 -5 -7 0 57.69 15.20 -5 -7 0 97.49 23.60 5 7 0 56.89 11.90 5 7 0 42.10 19.40 5 7 0 74.39 18.70 5 7 0 76.89 12.10 5 7 0 88.19 12.40 5 7 0 86.49 17.90 5 7 0 64.79 11.90 5 7 0 25.40 17.70 7 -8 0 50.49 16.70 7 -8 0 11.00 15.10 7 -8 0 22.20 15.40 7 -8 0 -18.40 17.00 7 -8 0 5.20 9.70 7 -8 0 14.80 17.10 7 -8 0 -11.80 17.70 -7 8 0 15.10 16.60 -7 8 0 -23.70 14.60 -7 8 0 -3.90 16.30 -7 8 0 1.20 17.80 -7 8 0 22.90 17.70 6 -8 0 39.90 16.40 6 -8 0 44.60 16.00 6 -8 0 17.60 12.80 6 -8 0 30.00 12.60 6 -8 0 44.50 15.70 6 -8 0 22.20 9.70 6 -8 0 1.90 14.50 -6 8 0 22.60 12.70 -6 8 0 1.00 15.10 -6 8 0 29.10 15.10 -6 8 0 36.30 15.70 -6 8 0 33.80 15.60 5 -8 0 34.30 13.20 5 -8 0 61.99 14.50 5 -8 0 47.20 14.80 5 -8 0 47.50 14.40 5 -8 0 56.39 10.50 5 -8 0 52.99 15.50 5 -8 0 59.19 10.80 5 -8 0 66.59 14.40 -5 8 0 52.99 15.00 -5 8 0 74.19 14.60 -5 8 0 20.80 17.90 -5 8 0 57.49 14.90 -5 8 0 49.30 14.60 -5 8 0 35.90 10.70 4 -8 0 105.89 15.50 4 -8 0 101.49 14.10 4 -8 0 129.09 10.90 4 -8 0 107.59 14.30 4 -8 0 92.29 14.70 4 -8 0 133.29 13.30 4 -8 0 114.49 14.00 -4 8 0 131.69 16.40 -4 8 0 116.09 14.90 -4 8 0 92.19 13.80 -4 8 0 69.99 17.30 -4 8 0 105.59 11.00 -4 8 0 87.29 15.60 3 -8 0 39.20 12.80 3 -8 0 53.59 10.30 3 -8 0 33.70 9.70 3 -8 0 38.70 13.70 3 -8 0 23.40 13.50 3 -8 0 70.89 11.20 -3 8 0 50.29 12.50 -3 8 0 31.20 11.00 -3 8 0 54.09 11.60 -3 8 0 29.90 11.40 -3 8 0 37.20 5.80 -3 8 0 45.20 11.10 2 -8 0 -1.90 9.10 2 -8 0 2.90 11.30 2 -8 0 5.50 9.20 2 -8 0 -8.40 12.80 2 -8 0 2.70 9.00 2 -8 0 -7.60 8.90 -2 8 0 4.20 8.10 -2 8 0 -5.40 9.50 -2 8 0 7.50 10.40 -2 8 0 9.70 3.20 -2 8 0 -7.90 8.50 -2 8 0 11.90 10.30 -2 8 0 9.20 8.90 -2 8 0 9.10 2.90 1 -8 0 63.69 12.90 1 -8 0 22.50 12.40 1 -8 0 27.90 11.90 1 -8 0 55.89 10.70 1 -8 0 39.90 11.50 -1 8 0 36.20 10.80 -1 8 0 20.90 9.70 -1 8 0 26.60 10.10 -1 8 0 49.00 7.60 -1 8 0 47.30 6.10 -1 8 0 44.20 9.60 -1 8 0 36.10 10.90 0 -8 0 3.40 9.30 0 -8 0 11.70 6.30 0 -8 0 19.00 10.00 0 -8 0 -1.50 11.80 0 -8 0 -7.30 10.60 0 -8 0 19.50 9.30 0 8 0 15.40 5.30 0 8 0 19.60 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16.70 13.70 3 9 -9 29.10 14.80 3 9 -9 13.00 15.10 3 9 -9 9.20 10.40 -3 -9 9 7.00 14.70 -3 -9 9 22.70 7.90 -3 -9 9 7.60 14.00 2 9 -9 60.29 15.70 2 9 -9 94.29 12.70 2 9 -9 75.59 14.40 2 9 -9 63.29 13.10 2 9 -9 72.09 15.50 2 9 -9 55.49 14.20 -2 -9 9 74.09 8.00 -2 -9 9 75.89 15.20 -2 -9 9 86.89 8.30 -2 -9 9 76.29 8.70 -2 -9 9 94.79 13.20 -2 -9 9 82.89 8.20 1 9 -9 11.10 11.90 1 9 -9 28.60 7.70 1 9 -9 29.80 10.80 1 9 -9 42.30 13.10 1 9 -9 37.60 12.10 1 9 -9 36.50 11.90 -1 -9 9 33.30 7.40 -1 -9 9 40.40 7.00 -1 -9 9 26.10 9.40 -1 -9 9 35.40 11.80 0 9 -9 29.00 12.30 0 9 -9 46.10 10.10 0 9 -9 27.00 9.50 0 9 -9 38.60 12.50 0 9 -9 25.80 12.30 0 -9 9 30.00 11.00 0 -9 9 30.60 8.30 0 -9 9 39.60 8.20 -1 9 -9 360.16 29.60 -1 9 -9 401.96 31.00 -1 9 -9 358.56 31.00 -1 9 -9 393.66 28.70 -1 9 -9 357.86 29.50 1 -9 9 354.16 27.60 1 -9 9 346.67 28.80 1 -9 9 386.56 29.00 1 -9 9 363.86 27.70 -2 9 -9 -8.30 11.10 -2 9 -9 -3.90 11.30 -2 9 -9 -1.40 9.30 -2 9 -9 14.50 13.00 2 -9 9 6.60 8.50 2 -9 9 3.90 7.60 2 -9 9 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24.30 9.40 3 -5 9 27.20 11.50 3 -5 9 26.60 4.30 -4 5 -9 -16.80 13.30 -4 5 -9 34.70 12.60 4 -5 9 39.90 13.80 4 -5 9 13.20 13.50 4 -5 9 8.90 13.40 4 -5 9 9.80 5.70 4 -5 9 34.90 11.70 4 -5 9 10.40 10.90 -5 5 -9 17.80 15.90 -5 5 -9 10.30 14.20 5 -5 9 -0.90 14.50 5 -5 9 -13.60 11.70 5 -5 9 -1.40 5.20 5 -5 9 11.80 13.50 5 -5 9 11.90 12.40 5 -5 9 3.60 13.60 -6 5 -9 -3.20 15.90 -6 5 -9 14.50 18.20 6 -5 9 -14.90 13.00 6 -5 9 4.30 16.10 6 -5 9 -1.80 14.90 6 -5 9 6.50 16.90 6 -5 9 1.60 4.10 6 4 -9 108.49 22.00 6 4 -9 147.79 20.30 6 4 -9 109.49 18.10 6 4 -9 132.79 20.60 6 4 -9 103.69 21.50 -6 -4 9 133.39 18.80 5 4 -9 9.30 15.20 5 4 -9 21.70 16.00 5 4 -9 2.90 12.40 5 4 -9 7.90 12.60 5 4 -9 17.90 15.00 -5 -4 9 10.70 15.50 -5 -4 9 -21.60 13.70 4 4 -9 9.40 10.40 4 4 -9 6.30 12.60 4 4 -9 4.10 12.90 4 4 -9 19.20 11.00 4 4 -9 9.50 9.30 -4 -4 9 4.20 4.40 -4 -4 9 -5.20 12.30 -4 -4 9 13.50 4.80 -4 -4 9 4.20 4.40 -4 -4 9 12.80 11.00 3 4 -9 1.10 10.60 3 4 -9 11.50 10.90 3 4 -9 5.90 9.10 3 4 -9 5.80 8.40 3 4 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9 4.20 13.00 -5 -3 9 -0.10 14.50 4 3 -9 15.40 9.70 4 3 -9 33.00 12.80 4 3 -9 17.10 13.20 4 3 -9 8.50 13.30 4 3 -9 35.60 7.40 4 3 -9 42.00 13.30 4 3 -9 31.10 10.60 4 3 -9 36.40 13.90 -4 -3 9 22.60 6.70 -4 -3 9 12.20 12.40 -4 -3 9 33.60 7.10 -4 -3 9 18.70 6.80 3 3 -9 0.00 7.30 3 3 -9 9.90 10.50 3 3 -9 12.10 12.20 3 3 -9 -5.10 6.80 3 3 -9 15.20 11.50 3 3 -9 1.10 8.10 -3 -3 9 2.60 6.40 -3 -3 9 -8.60 6.00 -3 -3 9 29.30 8.20 -3 -3 9 17.20 11.20 -3 -3 9 11.80 9.20 -3 -3 9 4.80 6.50 2 3 -9 509.15 36.60 2 3 -9 490.55 39.20 2 3 -9 494.35 39.00 2 3 -9 542.65 38.60 2 3 -9 510.95 36.80 2 3 -9 569.04 37.60 2 3 -9 573.14 38.10 2 3 -9 555.64 39.10 -2 -3 9 532.85 35.50 -2 -3 9 526.85 36.80 -2 -3 9 515.15 36.90 -2 -3 9 502.35 38.70 -2 -3 9 495.55 36.90 -2 -3 9 505.75 38.20 -2 -3 9 519.95 36.90 1 3 -9 17.20 8.90 1 3 -9 26.90 9.60 1 3 -9 13.10 9.90 1 3 -9 22.10 7.30 1 3 -9 1.60 7.80 -1 -3 9 17.40 7.20 -1 -3 9 20.00 7.80 -1 -3 9 16.90 6.50 -1 -3 9 20.10 9.60 -1 -3 9 25.10 9.20 -1 -3 9 16.80 5.80 -1 -3 9 29.80 8.20 0 3 -9 187.78 17.50 0 3 -9 172.68 17.10 0 3 -9 177.18 17.70 0 -3 9 204.68 16.20 0 -3 9 185.48 17.70 0 -3 9 161.58 17.00 0 -3 9 210.08 19.20 0 -3 9 179.08 15.50 0 -3 9 158.18 16.60 -1 3 -9 160.08 15.60 -1 3 -9 165.98 15.80 -1 3 -9 156.48 16.90 -1 3 -9 202.78 15.00 -1 3 -9 166.78 16.70 1 -3 9 185.58 15.30 1 -3 9 173.48 15.20 1 -3 9 180.78 14.90 1 -3 9 144.39 16.70 1 -3 9 177.38 17.30 1 -3 9 184.08 18.10 1 -3 9 173.58 15.20 1 -3 9 143.89 15.80 -2 3 -9 58.69 8.50 -2 3 -9 53.79 12.50 -2 3 -9 51.99 11.30 -2 3 -9 64.39 10.90 2 -3 9 60.39 8.50 2 -3 9 67.69 10.90 2 -3 9 54.39 12.20 2 -3 9 61.59 10.30 2 -3 9 61.99 8.40 2 -3 9 63.79 6.90 2 -3 9 66.79 12.30 2 -3 9 70.99 6.20 -3 3 -9 8.10 12.30 -3 3 -9 10.20 12.10 -3 3 -9 3.10 5.50 3 -3 9 7.00 10.10 3 -3 9 8.20 8.40 3 -3 9 -0.10 12.00 3 -3 9 7.30 8.90 3 -3 9 12.50 11.90 -4 3 -9 16.60 13.30 -4 3 -9 -9.40 13.60 4 -3 9 -13.30 10.70 4 -3 9 17.20 13.00 4 -3 9 -7.00 12.90 4 -3 9 -3.40 13.70 4 -3 9 -2.50 10.30 4 -3 9 15.00 13.90 -5 3 -9 26.60 15.60 -5 3 -9 45.60 17.50 5 -3 9 24.10 16.40 5 -3 9 24.20 13.00 5 -3 9 4.90 13.30 5 -3 9 23.00 16.20 5 -3 9 8.50 15.60 5 -3 9 17.10 15.30 -6 3 -9 8.40 18.40 6 -3 9 -12.20 15.40 6 -3 9 17.40 18.00 6 -3 9 -3.80 18.70 6 -3 9 1.50 13.90 6 2 -9 49.40 14.10 6 2 -9 28.50 17.00 6 2 -9 21.60 13.20 6 2 -9 11.50 9.30 6 2 -9 11.40 16.30 6 2 -9 23.80 13.80 6 2 -9 28.80 14.80 -6 -2 9 19.80 8.10 -6 -2 9 15.50 15.70 -6 -2 9 5.30 8.30 -6 -2 9 28.30 18.10 -6 -2 9 18.50 8.20 5 2 -9 40.10 11.10 5 2 -9 35.50 9.20 5 2 -9 -4.50 13.60 5 2 -9 28.50 15.70 5 2 -9 48.60 13.00 5 2 -9 29.00 14.80 5 2 -9 23.90 14.20 5 2 -9 22.40 15.20 -5 -2 9 42.60 8.30 -5 -2 9 27.00 8.30 -5 -2 9 49.70 14.80 -5 -2 9 14.20 14.30 -5 -2 9 36.40 8.30 4 2 -9 15.00 13.30 4 2 -9 24.90 8.90 4 2 -9 18.30 8.40 4 2 -9 26.60 12.40 4 2 -9 39.20 10.80 4 2 -9 48.80 12.50 4 2 -9 38.30 10.30 4 2 -9 42.50 12.30 -4 -2 9 24.90 8.30 -4 -2 9 27.00 12.00 -4 -2 9 31.00 8.20 -4 -2 9 11.50 10.20 -4 -2 9 -0.20 12.10 -4 -2 9 28.60 8.20 3 2 -9 2.80 9.80 3 2 -9 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18 87.89 15.80 -1 -11 18 105.99 15.80 -1 -11 18 79.39 14.70 -1 -11 18 73.69 14.80 0 -11 18 14.80 14.30 0 -11 18 -9.00 13.90 0 -11 18 1.80 14.60 0 -11 18 -1.30 13.70 1 -11 18 8.00 15.10 1 -11 18 4.90 14.50 1 -11 18 -11.50 14.70 1 -11 18 -12.10 14.20 2 10 -18 -34.40 17.50 2 10 -18 -6.10 18.20 2 10 -18 0.20 16.70 -2 -10 18 1.90 14.50 -2 -10 18 -11.00 10.60 -2 -10 18 0.20 11.20 -2 -10 18 15.50 11.90 -2 -10 18 -0.30 10.70 -1 -10 18 -5.70 13.10 -1 -10 18 1.20 13.30 -1 -10 18 -21.80 11.20 -1 -10 18 -4.60 11.90 0 -10 18 1.20 12.60 0 -10 18 -10.00 12.90 0 -10 18 15.10 15.10 0 -10 18 -20.20 13.70 1 -10 18 30.60 14.60 1 -10 18 2.00 14.90 1 -10 18 14.30 13.70 1 -10 18 5.70 13.10 1 -10 18 21.60 14.20 2 -10 18 28.90 16.50 2 -10 18 30.20 13.50 2 -10 18 5.50 14.20 2 -10 18 15.10 13.80 2 -10 18 48.80 18.10 2 -10 18 38.50 12.90 2 -10 18 36.60 13.70 2 9 -18 40.80 16.60 2 9 -18 42.30 18.60 2 9 -18 31.00 16.80 -2 -9 18 27.50 12.80 -2 -9 18 20.70 11.10 -2 -9 18 52.49 11.60 -2 -9 18 27.30 11.50 -2 -9 18 58.39 16.60 1 9 -18 37.30 16.50 -1 -9 18 13.20 12.10 -1 -9 18 22.20 13.40 -1 -9 18 5.20 15.60 -1 -9 18 -1.80 11.80 -1 -9 18 14.70 13.40 -1 -9 18 -4.70 12.40 0 -9 18 42.50 14.20 0 -9 18 43.10 14.00 0 -9 18 61.79 14.20 0 -9 18 49.99 15.10 0 -9 18 43.70 17.10 0 -9 18 33.20 14.50 1 -9 18 28.90 18.30 1 -9 18 48.40 13.00 1 -9 18 22.60 13.80 1 -9 18 43.60 12.20 1 -9 18 69.39 13.80 1 -9 18 17.40 15.80 2 -9 18 156.48 19.90 2 -9 18 198.98 19.70 2 -9 18 173.78 21.70 2 -9 18 160.38 20.90 2 -9 18 190.48 19.10 2 -9 18 172.38 18.80 2 -9 18 181.78 22.60 2 8 -18 -32.80 17.30 2 8 -18 -22.70 15.80 2 8 -18 -6.30 15.30 -2 -8 18 -19.00 12.50 -2 -8 18 26.40 14.80 -2 -8 18 -11.10 11.20 -2 -8 18 3.50 11.50 -2 -8 18 2.40 10.20 1 8 -18 -9.00 16.70 1 8 -18 0.00 15.00 -1 -8 18 40.10 14.10 -1 -8 18 5.70 12.00 -1 -8 18 16.70 12.20 -1 -8 18 17.10 15.10 -1 -8 18 33.90 14.50 -1 -8 18 26.80 12.30 0 8 -18 -20.70 14.80 0 -8 18 25.00 15.30 0 -8 18 -0.60 11.50 0 -8 18 8.50 14.00 0 -8 18 3.20 12.50 0 -8 18 6.10 13.80 0 -8 18 -5.10 11.90 1 -8 18 -22.60 10.70 1 -8 18 -22.80 10.10 1 -8 18 17.10 12.80 1 -8 18 -22.90 14.70 1 -8 18 10.90 12.40 1 -8 18 -7.40 15.50 2 -8 18 28.50 11.90 2 -8 18 20.90 13.50 2 -8 18 32.50 12.90 2 -8 18 10.70 11.40 2 -8 18 41.20 15.20 2 -8 18 25.60 17.10 2 -8 18 33.70 12.00 3 7 -18 24.30 17.50 3 7 -18 -15.20 18.00 3 7 -18 -5.30 16.90 3 7 -18 -15.30 17.30 -3 -7 18 10.00 13.10 -3 -7 18 -11.80 11.40 -3 -7 18 17.90 15.70 -3 -7 18 5.60 11.80 -3 -7 18 -3.80 4.70 2 7 -18 65.09 18.00 2 7 -18 107.69 20.40 2 7 -18 91.39 17.20 2 7 -18 53.09 15.90 -2 -7 18 67.09 14.90 -2 -7 18 48.10 17.90 -2 -7 18 55.39 14.40 -2 -7 18 68.29 12.70 -2 -7 18 64.69 11.50 -2 -7 18 85.69 16.00 1 7 -18 16.40 16.90 1 7 -18 -15.10 16.20 -1 -7 18 15.60 11.50 -1 -7 18 46.10 16.80 -1 -7 18 19.40 13.90 -1 -7 18 54.89 14.90 -1 -7 18 16.50 11.30 -1 -7 18 44.90 13.70 -1 -7 18 43.90 10.90 0 7 -18 -4.40 14.80 0 -7 18 30.00 14.40 0 -7 18 18.10 14.30 0 -7 18 -20.90 10.70 0 -7 18 -9.40 12.40 0 -7 18 12.30 16.30 -1 7 -18 5.40 14.70 1 -7 18 24.60 12.20 1 -7 18 28.90 16.40 1 -7 18 2.90 10.50 1 -7 18 30.50 15.80 1 -7 18 31.40 16.90 1 -7 18 45.00 12.40 -2 7 -18 10.60 13.80 2 -7 18 -4.10 17.00 2 -7 18 -24.80 10.10 2 -7 18 4.60 13.50 2 -7 18 18.90 13.90 2 -7 18 -0.20 15.90 2 -7 18 16.30 10.40 3 6 -18 13.70 19.50 3 6 -18 53.09 18.60 3 6 -18 -0.60 15.00 3 6 -18 8.90 15.90 -3 -6 18 12.10 14.20 -3 -6 18 28.40 13.10 -3 -6 18 10.70 4.80 -3 -6 18 -4.70 12.50 -3 -6 18 13.60 17.10 2 6 -18 24.30 14.80 2 6 -18 -2.70 17.50 2 6 -18 -10.10 15.70 2 6 -18 23.40 14.50 -2 -6 18 -21.00 15.40 -2 -6 18 7.30 12.50 -2 -6 18 20.50 8.10 -2 -6 18 16.00 10.00 -2 -6 18 9.60 9.40 -2 -6 18 27.30 14.60 -2 -6 18 16.70 9.80 -2 -6 18 10.70 14.60 1 6 -18 10.50 15.60 1 6 -18 2.50 15.90 -1 -6 18 3.90 16.10 -1 -6 18 -10.50 8.70 -1 -6 18 2.20 8.80 -1 -6 18 6.00 15.20 -1 -6 18 -5.90 13.50 -1 -6 18 -2.50 14.70 -1 -6 18 0.80 10.80 -1 -6 18 -3.90 9.60 0 6 -18 7.40 13.60 0 6 -18 -10.90 16.10 0 -6 18 -4.00 15.10 0 -6 18 -4.30 15.80 0 -6 18 -7.20 9.60 0 -6 18 -20.90 14.50 0 -6 18 1.60 9.40 0 -6 18 -6.50 13.30 -1 6 -18 1.70 13.90 1 -6 18 -1.10 10.90 1 -6 18 18.70 16.20 1 -6 18 -2.30 16.70 1 -6 18 -15.30 15.90 1 -6 18 1.20 9.20 1 -6 18 -4.40 9.10 1 -6 18 17.00 11.40 -2 6 -18 19.40 14.30 2 -6 18 8.40 17.50 2 -6 18 9.60 18.40 2 -6 18 4.00 13.50 2 -6 18 -1.10 9.00 2 -6 18 -16.60 8.60 2 -6 18 2.50 18.00 2 -6 18 3.40 12.60 2 -6 18 17.30 8.80 3 5 -18 2.50 14.60 3 5 -18 -2.40 15.30 3 5 -18 28.60 18.50 3 5 -18 9.00 17.30 -3 -5 18 -1.20 7.90 -3 -5 18 8.60 8.70 -3 -5 18 35.10 15.20 -3 -5 18 -22.10 13.60 -3 -5 18 13.30 13.60 -3 -5 18 -5.50 5.70 -3 -5 18 2.90 16.30 2 5 -18 59.59 14.20 2 5 -18 29.30 16.30 2 5 -18 39.50 15.30 2 5 -18 51.49 18.80 -2 -5 18 50.99 8.60 -2 -5 18 51.79 15.60 -2 -5 18 55.39 15.20 -2 -5 18 41.30 6.70 -2 -5 18 49.20 8.20 -2 -5 18 63.49 11.20 -2 -5 18 68.69 16.30 -2 -5 18 51.09 18.10 1 5 -18 36.20 16.90 1 5 -18 53.99 14.80 -1 -5 18 24.70 15.20 -1 -5 18 52.19 16.50 -1 -5 18 71.99 18.50 -1 -5 18 43.60 8.30 -1 -5 18 28.20 8.40 -1 -5 18 38.30 13.20 -1 -5 18 46.40 9.00 -1 -5 18 36.50 17.00 0 5 -18 -3.00 12.90 0 5 -18 7.00 16.30 0 -5 18 14.50 10.40 0 -5 18 8.20 9.00 0 -5 18 47.40 17.10 0 -5 18 37.60 16.10 0 -5 18 14.60 8.30 0 -5 18 18.00 9.10 0 -5 18 1.20 19.80 0 -5 18 32.90 13.40 0 -5 18 3.30 8.60 -1 5 -18 7.30 15.00 1 -5 18 3.40 7.20 1 -5 18 -15.60 15.80 1 -5 18 -4.80 10.00 1 -5 18 13.70 17.20 1 -5 18 6.20 10.90 1 -5 18 0.40 6.90 1 -5 18 -9.50 16.40 3 4 -18 18.70 17.40 3 4 -18 28.10 19.60 3 4 -18 -12.40 13.90 3 4 -18 6.30 14.00 -3 -4 18 3.50 15.90 -3 -4 18 5.80 13.70 -3 -4 18 -24.40 14.50 -3 -4 18 7.20 6.70 -3 -4 18 29.70 17.30 2 4 -18 38.10 17.40 2 4 -18 33.30 12.40 2 4 -18 18.50 18.50 -2 -4 18 20.60 16.70 -2 -4 18 55.39 11.40 -2 -4 18 60.79 15.90 -2 -4 18 32.30 16.10 -2 -4 18 40.40 18.10 1 4 -18 -12.10 15.90 1 4 -18 -23.30 15.20 1 4 -18 -13.00 12.70 -1 -4 18 -2.10 15.80 -1 -4 18 -1.00 5.40 -1 -4 18 -9.70 14.90 -1 -4 18 0.90 16.80 -1 -4 18 8.00 13.10 -1 -4 18 -9.10 6.80 -1 -4 18 7.70 15.20 -1 -4 18 5.10 6.10 0 4 -18 -12.10 12.10 0 4 -18 34.40 16.10 0 -4 18 6.10 6.10 0 -4 18 23.10 9.10 0 -4 18 14.40 9.00 0 -4 18 18.50 15.50 0 -4 18 14.20 6.40 0 -4 18 19.40 7.60 0 -4 18 36.00 16.70 0 -4 18 18.70 16.60 -1 4 -18 -7.10 15.50 1 -4 18 2.00 17.60 1 -4 18 25.80 18.20 1 -4 18 26.30 13.00 1 -4 18 8.20 10.10 1 -4 18 39.80 18.20 3 3 -18 30.10 19.40 3 3 -18 -6.70 16.60 3 3 -18 -9.30 13.20 3 3 -18 20.00 14.00 -3 -3 18 -24.40 13.70 -3 -3 18 -11.30 17.20 -3 -3 18 0.10 16.10 -3 -3 18 -6.00 7.90 -3 -3 18 14.80 17.40 2 3 -18 9.30 17.20 2 3 -18 7.50 16.70 -2 -3 18 -7.70 16.30 -2 -3 18 39.30 18.60 -2 -3 18 15.30 15.60 -2 -3 18 32.80 16.90 -2 -3 18 10.50 11.60 1 3 -18 -17.40 16.80 1 3 -18 13.90 13.80 1 3 -18 5.40 17.10 -1 -3 18 16.00 13.50 -1 -3 18 5.50 17.70 -1 -3 18 12.90 3.80 -1 -3 18 10.10 16.20 -1 -3 18 38.90 18.30 0 3 -18 11.10 16.00 0 3 -18 3.70 12.10 0 3 -18 8.30 16.10 0 -3 18 0.50 17.00 0 -3 18 7.50 8.40 0 -3 18 22.80 16.80 0 -3 18 -4.60 17.30 0 -3 18 1.10 6.50 -1 3 -18 4.90 15.70 1 -3 18 -7.30 18.00 1 -3 18 3.80 15.30 1 -3 18 -9.00 17.70 1 -3 18 -2.00 17.60 1 -3 18 -1.80 9.50 2 2 -18 12.30 17.90 2 2 -18 11.40 16.30 -2 -2 18 15.00 16.80 -2 -2 18 -4.50 17.20 -2 -2 18 8.40 18.00 1 2 -18 -8.90 16.30 1 2 -18 -2.80 14.10 1 2 -18 28.10 16.70 -1 -2 18 -16.10 14.00 -1 -2 18 38.20 18.20 -1 -2 18 6.00 16.40 -1 -2 18 -10.60 17.10 0 2 -18 -28.00 16.80 0 2 -18 0.20 16.20 0 -2 18 -20.50 17.10 0 -2 18 -8.30 8.10 0 -2 18 -5.10 16.80 0 -2 18 -11.30 17.60 0 -2 18 -18.00 16.80 1 1 -18 8.90 18.80 1 1 -18 28.00 18.30 1 1 -18 14.70 14.80 -1 -1 18 43.00 18.40 -1 -1 18 0.50 16.90 -1 -1 18 -29.00 16.90 -1 -1 18 -10.90 14.80 1 9 -19 22.50 16.40 -1 -9 19 12.50 14.10 -1 -9 19 12.20 12.30 -1 -9 19 -12.90 13.40 -1 -9 19 15.90 14.60 -1 -9 19 -7.00 12.30 -1 -9 19 -10.40 14.80 0 -9 19 -7.20 13.60 0 -9 19 12.90 13.90 0 -9 19 -1.70 14.50 0 -9 19 -6.80 13.30 0 -9 19 8.90 12.50 0 -9 19 8.20 13.70 1 8 -19 16.60 18.20 1 8 -19 28.90 15.90 -1 -8 19 -16.10 13.90 -1 -8 19 9.20 13.00 -1 -8 19 -1.00 12.50 -1 -8 19 6.80 16.20 -1 -8 19 -14.60 11.40 -1 -8 19 25.20 15.10 0 8 -19 0.90 17.30 0 -8 19 -30.30 13.00 0 -8 19 0.50 19.50 0 -8 19 19.00 15.80 0 -8 19 -15.70 14.20 0 -8 19 -12.10 11.20 0 -8 19 7.20 12.20 1 7 -19 32.70 18.40 1 7 -19 28.80 15.50 -1 -7 19 10.90 15.50 -1 -7 19 -2.50 11.80 -1 -7 19 -13.30 15.30 -1 -7 19 9.10 16.90 -1 -7 19 2.80 13.90 -1 -7 19 11.00 10.50 -1 -7 19 10.30 9.90 0 7 -19 4.80 15.80 0 -7 19 0.90 12.40 0 -7 19 -14.70 15.30 0 -7 19 -7.00 13.20 0 -7 19 -7.80 16.70 0 -7 19 1.60 10.70 1 6 -19 39.30 18.10 1 6 -19 7.00 15.90 -1 -6 19 -5.20 8.90 -1 -6 19 -13.70 17.00 -1 -6 19 19.90 9.00 -1 -6 19 32.40 13.20 -1 -6 19 -1.20 15.20 -1 -6 19 -2.10 14.70 -1 -6 19 20.20 10.00 -1 -6 19 31.80 16.40 0 6 -19 -30.80 15.10 0 6 -19 1.70 14.00 0 -6 19 12.70 9.70 0 -6 19 16.20 13.30 0 -6 19 7.30 10.00 0 -6 19 -7.00 16.30 0 -6 19 6.60 9.60 0 -6 19 24.00 16.60 0 -6 19 6.70 10.00 1 5 -19 -6.00 15.30 1 5 -19 11.70 18.80 -1 -5 19 43.40 13.60 -1 -5 19 9.80 9.30 -1 -5 19 44.50 16.60 -1 -5 19 3.50 17.00 -1 -5 19 7.50 18.50 -1 -5 19 12.60 7.30 -1 -5 19 12.20 7.80 0 5 -19 -19.80 15.90 0 5 -19 17.00 13.80 0 -5 19 19.60 10.00 0 -5 19 12.20 9.20 0 -5 19 -12.30 18.10 0 -5 19 2.50 14.90 0 -5 19 -8.90 16.70 0 -5 19 1.80 7.90 0 -5 19 -5.80 8.10 0 -5 19 12.70 8.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 30195 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group F F1 0.9865(3) 0.96109(17) 0.62735(19) 0.0710(8) Uani d . . . 1 . . F F2 0.7720(4) 0.98556(16) 0.54056(14) 0.0602(7) Uani d . . . 1 . . F F3 0.7644(4) 1.04559(15) 0.68296(15) 0.0656(7) Uani d . . . 1 . . O O1 0.0897(4) 0.51004(18) 0.14790(14) 0.0361(6) Uani d . . . 1 . . O O2 0.3150(3) 0.43248(16) 0.06490(13) 0.0298(5) Uani d . . . 1 . . O O3 -0.3411(3) 0.29627(17) 0.14385(14) 0.0358(6) Uani d . . . 1 . . O O4 -0.1792(3) 0.25296(16) 0.02140(14) 0.0334(5) Uani d . . . 1 . . N N1 0.1700(4) 0.58857(19) 0.53081(15) 0.0310(7) Uani d . . . 1 . . C C1 0.1371(5) 0.5129(2) 0.43983(18) 0.0238(7) Uani d . . . 1 . . C C2 -0.0299(5) 0.4232(2) 0.40998(18) 0.0230(6) Uani d . . . 1 . . C C3 0.2660(4) 0.5255(2) 0.37923(18) 0.0218(6) Uani d . . . 1 . . H H3 0.380527 0.586201 0.400092 0.026 Uiso calc U . R 1 . . C C4 -0.0578(4) 0.3488(2) 0.32091(18) 0.0222(6) Uani d . . . 1 . . H H4 -0.168313 0.286781 0.301016 0.027 Uiso calc U . R 1 . . C C5 0.2337(4) 0.4521(2) 0.28812(18) 0.0206(6) Uani d . . . 1 . . C C6 0.0708(4) 0.3619(2) 0.25936(18) 0.0213(6) Uani d . . . 1 . . C C7 0.3743(4) 0.4736(2) 0.22284(18) 0.0220(6) Uani d . . . 1 . . H H7 0.445395 0.416685 0.197652 0.026 Uiso calc U . R 1 . . C C8 0.5472(4) 0.5752(2) 0.26896(18) 0.0232(7) Uani d . . . 1 . . C C9 0.5009(5) 0.6690(2) 0.2900(2) 0.0274(7) Uani d . . . 1 . . H H9 0.359556 0.670172 0.272927 0.033 Uiso calc U . R 1 . . C C10 0.6592(5) 0.7608(2) 0.3357(2) 0.0326(8) Uani d . . . 1 . . H H10 0.625461 0.824572 0.350204 0.039 Uiso calc U . R 1 . . C C11 0.8634(5) 0.7601(2) 0.3599(2) 0.0347(8) Uani d . . . 1 . . H H11 0.971649 0.823035 0.391729 0.042 Uiso calc U . R 1 . . C C12 0.9112(5) 0.6669(3) 0.3378(2) 0.0327(8) Uani d . . . 1 . . H H12 1.053753 0.665969 0.35329 0.039 Uiso calc U . R 1 . . C C13 0.7538(5) 0.5751(2) 0.29345(19) 0.0274(7) Uani d . . . 1 . . H H13 0.788031 0.51162 0.279739 0.033 Uiso calc U . R 1 . . C C14 0.2412(5) 0.4751(2) 0.14263(19) 0.0245(7) Uani d . . . 1 . . C C15 0.2013(5) 0.4320(2) -0.01585(19) 0.0307(7) Uani d . . . 1 . . H H15A 0.249073 0.500465 -0.015919 0.037 Uiso calc U . R 1 . . H H15B 0.046021 0.416938 -0.015251 0.037 Uiso calc U . R 1 . . C C16 0.2464(6) 0.3517(3) -0.0990(2) 0.0376(8) Uani d . . . 1 . . H H16A 0.171378 0.35073 -0.153888 0.056 Uiso calc U . R 1 . . H H16B 0.197176 0.284088 -0.098784 0.056 Uiso calc U . R 1 . . H H16C 0.400281 0.367215 -0.099152 0.056 Uiso calc U . R 1 . . C C17 0.0198(5) 0.2788(2) 0.16029(19) 0.0241(7) Uani d . . . 1 . . H H17 0.138128 0.295704 0.128512 0.029 Uiso calc U . R 1 . . C C18 0.0013(5) 0.1702(2) 0.1516(2) 0.0295(7) Uani d . . . 1 . . C C19 0.1716(5) 0.1283(3) 0.1300(2) 0.0396(8) Uani d . . . 1 . . H H19 0.298855 0.168456 0.123432 0.048 Uiso calc U . R 1 . . C C20 0.1595(6) 0.0285(3) 0.1179(3) 0.0567(11) Uani d . . . 1 . . H H20 0.277145 0.000318 0.102332 0.068 Uiso calc U . R 1 . . C C21 -0.0228(7) -0.0295(3) 0.1285(3) 0.0582(11) Uani d . . . 1 . . H H21 -0.031719 -0.097917 0.12024 0.07 Uiso calc U . R 1 . . C C22 -0.1919(6) 0.0114(3) 0.1509(3) 0.0500(10) Uani d . . . 1 . . H H22 -0.316374 -0.028361 0.159878 0.06 Uiso calc U . R 1 . . C C23 -0.1837(5) 0.1108(2) 0.1608(2) 0.0356(8) Uani d . . . 1 . . H H23 -0.304044 0.137466 0.173775 0.043 Uiso calc U . R 1 . . C C24 -0.1869(5) 0.2794(2) 0.11024(19) 0.0279(7) Uani d . . . 1 . . C C25 -0.3754(5) 0.2450(3) -0.0330(2) 0.0369(8) Uani d . . . 1 . . H H25A -0.411539 0.311888 -0.008632 0.044 Uiso calc U . R 1 . . H H25B -0.494861 0.192231 -0.030557 0.044 Uiso calc U . R 1 . . C C26 -0.3399(6) 0.2152(3) -0.1292(2) 0.0445(9) Uani d . . . 1 . . H H26A -0.295137 0.151243 -0.15123 0.067 Uiso calc U . R 1 . . H H26B -0.228385 0.270241 -0.131427 0.067 Uiso calc U . R 1 . . H H26C -0.472679 0.204677 -0.168117 0.067 Uiso calc U . R 1 . . C C27 0.3256(5) 0.6851(2) 0.55744(18) 0.0244(7) Uani d . . . 1 . . C C28 0.2638(5) 0.7645(2) 0.5470(2) 0.0297(7) Uani d . . . 1 . . H H28 0.118019 0.756248 0.526547 0.036 Uiso calc U . R 1 . . C C29 0.4139(5) 0.8556(2) 0.5663(2) 0.0313(7) Uani d . . . 1 . . H H29 0.372359 0.910122 0.558772 0.038 Uiso calc U . R 1 . . C C30 0.6262(5) 0.8668(2) 0.5968(2) 0.0277(7) Uani d . . . 1 . . C C31 0.6855(5) 0.7892(2) 0.6107(2) 0.0312(7) Uani d . . . 1 . . H H31 0.829919 0.79819 0.633825 0.037 Uiso calc U . R 1 . . C C32 0.5340(5) 0.6980(2) 0.5907(2) 0.0285(7) Uani d . . . 1 . . H H32 0.574566 0.644311 0.600062 0.034 Uiso calc U . R 1 . . C C33 0.7863(5) 0.9641(2) 0.6128(2) 0.0367(8) Uani d . . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 F1 0.0353(13) 0.0511(14) 0.114(2) -0.0135(10) 0.0062(13) 0.0364(14) F2 0.0826(17) 0.0386(12) 0.0452(13) -0.0196(11) 0.0112(11) 0.0222(10) F3 0.0871(17) 0.0245(11) 0.0529(14) -0.0129(11) 0.0311(12) -0.0035(10) O1 0.0369(13) 0.0510(15) 0.0276(12) 0.0196(11) 0.0093(10) 0.0197(11) O2 0.0354(12) 0.0369(12) 0.0188(11) 0.0095(10) 0.0080(9) 0.0134(9) O3 0.0362(13) 0.0400(14) 0.0287(12) 0.0116(11) 0.0063(10) 0.0116(10) O4 0.0385(13) 0.0362(13) 0.0223(11) 0.0091(10) 0.0043(9) 0.0101(10) N1 0.0373(15) 0.0248(14) 0.0152(12) -0.0126(11) 0.0095(11) 0.0031(11) C1 0.0280(16) 0.0229(16) 0.0169(14) 0.0008(13) 0.0050(12) 0.0079(12) C2 0.0268(16) 0.0248(16) 0.0166(14) 0.0002(13) 0.0050(12) 0.0115(12) C3 0.0236(15) 0.0200(15) 0.0193(15) -0.0008(12) 0.0035(12) 0.0093(12) C4 0.0236(15) 0.0196(15) 0.0186(14) -0.0017(12) 0.0023(11) 0.0077(12) C5 0.0215(15) 0.0238(15) 0.0197(14) 0.0050(12) 0.0051(11) 0.0129(12) C6 0.0244(15) 0.0201(15) 0.0183(14) 0.0035(12) 0.0038(12) 0.0084(12) C7 0.0251(15) 0.0221(15) 0.0175(14) 0.0032(12) 0.0073(11) 0.0081(12) C8 0.0255(16) 0.0291(16) 0.0163(14) 0.0034(13) 0.0082(12) 0.0122(12) C9 0.0296(17) 0.0290(17) 0.0251(16) 0.0037(13) 0.0090(13) 0.0147(14) C10 0.044(2) 0.0269(17) 0.0296(17) 0.0072(15) 0.0122(15) 0.0145(14) C11 0.039(2) 0.0286(18) 0.0271(17) -0.0063(15) 0.0037(14) 0.0104(14) C12 0.0259(17) 0.0401(19) 0.0286(17) 0.0006(14) 0.0010(13) 0.0161(15) C13 0.0320(18) 0.0272(16) 0.0246(16) 0.0061(13) 0.0059(13) 0.0134(13) C14 0.0263(17) 0.0239(16) 0.0215(16) 0.0011(13) 0.0081(12) 0.0100(13) C15 0.0389(19) 0.0352(18) 0.0210(16) 0.0109(15) 0.0044(13) 0.0146(14) C16 0.044(2) 0.043(2) 0.0242(17) 0.0112(16) 0.0050(14) 0.0139(15) C17 0.0277(16) 0.0213(15) 0.0197(15) 0.0024(12) 0.0085(12) 0.0068(12) C18 0.0360(18) 0.0204(16) 0.0230(16) 0.0010(14) -0.0009(13) 0.0048(13) C19 0.0316(19) 0.0299(18) 0.053(2) 0.0059(15) 0.0016(16) 0.0163(17) C20 0.043(2) 0.041(2) 0.083(3) 0.0160(19) 0.002(2) 0.023(2) C21 0.053(3) 0.034(2) 0.087(3) 0.0103(19) 0.000(2) 0.029(2) C22 0.052(2) 0.034(2) 0.057(2) -0.0023(18) 0.0027(19) 0.0207(18) C23 0.0402(19) 0.0277(18) 0.0339(18) 0.0019(15) 0.0070(15) 0.0120(15) C24 0.0365(18) 0.0217(16) 0.0172(15) -0.0008(13) 0.0048(13) 0.0045(12) C25 0.0361(19) 0.039(2) 0.0313(18) 0.0086(15) -0.0050(14) 0.0134(15) C26 0.052(2) 0.047(2) 0.0306(19) 0.0118(18) 0.0012(16) 0.0155(17) C27 0.0321(17) 0.0207(15) 0.0107(13) -0.0056(13) 0.0068(12) 0.0031(12) C28 0.0241(16) 0.0366(18) 0.0222(16) -0.0007(14) 0.0031(12) 0.0113(14) C29 0.0384(19) 0.0270(17) 0.0317(17) 0.0060(14) 0.0088(14) 0.0168(14) C30 0.0294(17) 0.0236(16) 0.0220(15) -0.0038(13) 0.0070(13) 0.0071(13) C31 0.0267(17) 0.0291(17) 0.0311(17) -0.0007(14) 0.0016(13) 0.0112(14) C32 0.0348(18) 0.0220(16) 0.0265(16) 0.0011(13) 0.0044(13) 0.0117(13) C33 0.040(2) 0.0269(18) 0.0339(19) -0.0047(15) 0.0081(15) 0.0110(15) 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' F F 0.0171 0.0103 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C14 O2 C15 . . 115.6(2) ? C24 O4 C25 . . 114.7(2) ? C1 N1 C27 . . 118.8(2) ? C2 N1 C1 2_566 . 120.5(2) ? C2 N1 C27 2_566 . 120.0(2) ? C2 C1 N1 . . 119.5(2) ? C3 C1 N1 . . 121.3(2) ? C3 C1 C2 . . 119.2(2) ? C1 C2 N1 . 2_566 120.0(2) ? C4 C2 N1 . 2_566 121.2(2) ? C4 C2 C1 . . 118.7(3) ? C1 C3 H3 . . 118.9 ? C1 C3 C5 . . 122.3(3) ? C5 C3 H3 . . 118.9 ? C2 C4 H4 . . 118.9 ? C2 C4 C6 . . 122.1(3) ? C6 C4 H4 . . 118.9 ? C3 C5 C7 . . 119.7(2) ? C6 C5 C3 . . 118.3(2) ? C6 C5 C7 . . 122.0(2) ? C4 C6 C17 . . 118.7(2) ? C5 C6 C4 . . 119.3(2) ? C5 C6 C17 . . 121.9(2) ? C5 C7 H7 . . 108.1 ? C8 C7 C5 . . 113.4(2) ? C8 C7 H7 . . 108.1 ? C8 C7 C14 . . 107.9(2) ? C14 C7 C5 . . 111.2(2) ? C14 C7 H7 . . 108.1 ? C9 C8 C7 . . 121.5(3) ? C13 C8 C7 . . 119.7(3) ? C13 C8 C9 . . 118.8(3) ? C8 C9 H9 . . 119.7 ? C10 C9 C8 . . 120.6(3) ? C10 C9 H9 . . 119.7 ? C9 C10 H10 . . 119.9 ? C11 C10 C9 . . 120.3(3) ? C11 C10 H10 . . 119.9 ? C10 C11 H11 . . 120.3 ? C10 C11 C12 . . 119.4(3) ? C12 C11 H11 . . 120.3 ? C11 C12 H12 . . 119.7 ? C13 C12 C11 . . 120.6(3) ? C13 C12 H12 . . 119.7 ? C8 C13 C12 . . 120.3(3) ? C8 C13 H13 . . 119.8 ? C12 C13 H13 . . 119.8 ? O1 C14 O2 . . 123.9(3) ? O1 C14 C7 . . 124.9(3) ? O2 C14 C7 . . 111.2(2) ? O2 C15 H15A . . 110.0 ? O2 C15 H15B . . 110.0 ? O2 C15 C16 . . 108.6(3) ? H15A C15 H15B . . 108.4 ? C16 C15 H15A . . 110.0 ? C16 C15 H15B . . 110.0 ? C15 C16 H16A . . 109.5 ? C15 C16 H16B . . 109.5 ? C15 C16 H16C . . 109.5 ? H16A C16 H16B . . 109.5 ? H16A C16 H16C . . 109.5 ? H16B C16 H16C . . 109.5 ? C6 C17 H17 . . 107.8 ? C18 C17 C6 . . 113.9(2) ? C18 C17 H17 . . 107.8 ? C18 C17 C24 . . 108.8(2) ? C24 C17 C6 . . 110.6(2) ? C24 C17 H17 . . 107.8 ? C19 C18 C17 . . 118.8(3) ? C19 C18 C23 . . 119.0(3) ? C23 C18 C17 . . 122.1(3) ? C18 C19 H19 . . 119.5 ? C18 C19 C20 . . 121.0(3) ? C20 C19 H19 . . 119.5 ? C19 C20 H20 . . 120.1 ? C21 C20 C19 . . 119.8(4) ? C21 C20 H20 . . 120.1 ? C20 C21 H21 . . 120.0 ? C22 C21 C20 . . 119.9(4) ? C22 C21 H21 . . 120.0 ? C21 C22 H22 . . 119.6 ? C21 C22 C23 . . 120.8(4) ? C23 C22 H22 . . 119.6 ? C18 C23 C22 . . 119.5(3) ? C18 C23 H23 . . 120.3 ? C22 C23 H23 . . 120.3 ? O3 C24 O4 . . 123.6(3) ? O3 C24 C17 . . 125.4(3) ? O4 C24 C17 . . 111.0(3) ? O4 C25 H25A . . 110.1 ? O4 C25 H25B . . 110.1 ? O4 C25 C26 . . 107.8(3) ? H25A C25 H25B . . 108.5 ? C26 C25 H25A . . 110.1 ? C26 C25 H25B . . 110.1 ? C25 C26 H26A . . 109.5 ? C25 C26 H26B . . 109.5 ? C25 C26 H26C . . 109.5 ? H26A C26 H26B . . 109.5 ? H26A C26 H26C . . 109.5 ? H26B C26 H26C . . 109.5 ? C28 C27 N1 . . 119.1(3) ? C32 C27 N1 . . 120.6(3) ? C32 C27 C28 . . 120.3(3) ? C27 C28 H28 . . 120.0 ? C29 C28 C27 . . 120.1(3) ? C29 C28 H28 . . 120.0 ? C28 C29 H29 . . 120.4 ? C28 C29 C30 . . 119.3(3) ? C30 C29 H29 . . 120.4 ? C29 C30 C33 . . 118.1(3) ? C31 C30 C29 . . 120.4(3) ? C31 C30 C33 . . 121.5(3) ? C30 C31 H31 . . 120.1 ? C30 C31 C32 . . 119.8(3) ? C32 C31 H31 . . 120.1 ? C27 C32 C31 . . 120.1(3) ? C27 C32 H32 . . 120.0 ? C31 C32 H32 . . 120.0 ? F1 C33 F2 . . 104.7(3) ? F1 C33 C30 . . 113.6(3) ? F2 C33 C30 . . 112.1(3) ? F3 C33 F1 . . 106.8(3) ? F3 C33 F2 . . 106.0(3) ? F3 C33 C30 . . 113.0(3) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag F1 C33 . 1.323(4) ? F2 C33 . 1.335(4) ? F3 C33 . 1.320(4) ? O1 C14 . 1.201(4) ? O2 C14 . 1.336(3) ? O2 C15 . 1.458(3) ? O3 C24 . 1.200(4) ? O4 C24 . 1.339(3) ? O4 C25 . 1.458(4) ? N1 C1 . 1.408(3) ? N1 C2 2_566 1.405(4) ? N1 C27 . 1.434(4) ? C1 C2 . 1.397(4) ? C1 C3 . 1.379(4) ? C2 C4 . 1.382(4) ? C3 H3 . 0.95 ? C3 C5 . 1.398(4) ? C4 H4 . 0.95 ? C4 C6 . 1.393(4) ? C5 C6 . 1.389(4) ? C5 C7 . 1.531(4) ? C6 C17 . 1.530(4) ? C7 H7 . 1.0 ? C7 C8 . 1.521(4) ? C7 C14 . 1.525(4) ? C8 C9 . 1.388(4) ? C8 C13 . 1.378(4) ? C9 H9 . 0.95 ? C9 C10 . 1.386(4) ? C10 H10 . 0.95 ? C10 C11 . 1.366(5) ? C11 H11 . 0.95 ? C11 C12 . 1.382(5) ? C12 H12 . 0.95 ? C12 C13 . 1.381(4) ? C13 H13 . 0.95 ? C15 H15A . 0.99 ? C15 H15B . 0.99 ? C15 C16 . 1.487(4) ? C16 H16A . 0.98 ? C16 H16B . 0.98 ? C16 H16C . 0.98 ? C17 H17 . 1.0 ? C17 C18 . 1.525(4) ? C17 C24 . 1.529(4) ? C18 C19 . 1.381(5) ? C18 C23 . 1.386(4) ? C19 H19 . 0.95 ? C19 C20 . 1.386(5) ? C20 H20 . 0.95 ? C20 C21 . 1.372(6) ? C21 H21 . 0.95 ? C21 C22 . 1.368(6) ? C22 H22 . 0.95 ? C22 C23 . 1.396(5) ? C23 H23 . 0.95 ? C25 H25A . 0.99 ? C25 H25B . 0.99 ? C25 C26 . 1.489(5) ? C26 H26A . 0.98 ? C26 H26B . 0.98 ? C26 H26C . 0.98 ? C27 C28 . 1.384(4) ? C27 C32 . 1.370(4) ? C28 H28 . 0.95 ? C28 C29 . 1.382(4) ? C29 H29 . 0.95 ? C29 C30 . 1.389(4) ? C30 C31 . 1.377(4) ? C30 C33 . 1.492(4) ? C31 H31 . 0.95 ? C31 C32 . 1.383(4) ? C32 H32 . 0.95 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C7 H7 O3 1_655 1.00 2.41 3.406(4) 172.7 ? C26 H26A F3 1_444 0.98 2.61 3.288(4) 126.6 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 C1 C2 N1 . . . 2_566 3.2(5) ? N1 C1 C2 C4 . . . . -178.9(3) ? N1 C1 C3 C5 . . . . -178.8(3) ? N1 C2 C4 C6 2_566 . . . 175.8(3) ? N1 C27 C28 C29 . . . . -175.6(3) ? N1 C27 C32 C31 . . . . 175.9(3) ? C1 N1 C27 C28 . . . . 88.9(3) ? C1 N1 C27 C32 . . . . -89.5(3) ? C1 C2 C4 C6 . . . . -2.0(5) ? C1 C3 C5 C6 . . . . -2.4(4) ? C1 C3 C5 C7 . . . . 176.5(3) ? C2 N1 C1 C2 2_566 . . . -3.2(5) ? C2 N1 C1 C3 2_566 . . . 176.5(3) ? C2 N1 C27 C28 2_566 . . . -80.8(3) ? C2 N1 C27 C32 2_566 . . . 100.8(3) ? C2 C1 C3 C5 . . . . 0.9(4) ? C2 C4 C6 C5 . . . . 0.5(4) ? C2 C4 C6 C17 . . . . -176.1(3) ? C3 C1 C2 N1 . . . 2_566 -176.5(3) ? C3 C1 C2 C4 . . . . 1.4(4) ? C3 C5 C6 C4 . . . . 1.8(4) ? C3 C5 C6 C17 . . . . 178.2(3) ? C3 C5 C7 C8 . . . . 2.9(4) ? C3 C5 C7 C14 . . . . -118.8(3) ? C4 C6 C17 C18 . . . . -52.9(4) ? C4 C6 C17 C24 . . . . 70.0(3) ? C5 C6 C17 C18 . . . . 130.6(3) ? C5 C6 C17 C24 . . . . -106.4(3) ? C5 C7 C8 C9 . . . . -76.6(3) ? C5 C7 C8 C13 . . . . 101.2(3) ? C5 C7 C14 O1 . . . . 37.8(4) ? C5 C7 C14 O2 . . . . -142.3(2) ? C6 C5 C7 C8 . . . . -178.2(3) ? C6 C5 C7 C14 . . . . 60.1(3) ? C6 C17 C18 C19 . . . . -100.9(3) ? C6 C17 C18 C23 . . . . 81.8(4) ? C6 C17 C24 O3 . . . . -36.3(4) ? C6 C17 C24 O4 . . . . 147.0(2) ? C7 C5 C6 C4 . . . . -177.1(3) ? C7 C5 C6 C17 . . . . -0.7(4) ? C7 C8 C9 C10 . . . . 177.1(3) ? C7 C8 C13 C12 . . . . -178.1(3) ? C8 C7 C14 O1 . . . . -87.2(3) ? C8 C7 C14 O2 . . . . 92.7(3) ? C8 C9 C10 C11 . . . . 0.5(4) ? C9 C8 C13 C12 . . . . -0.2(4) ? C9 C10 C11 C12 . . . . 0.5(5) ? C10 C11 C12 C13 . . . . -1.5(5) ? C11 C12 C13 C8 . . . . 1.3(5) ? C13 C8 C9 C10 . . . . -0.7(4) ? C14 O2 C15 C16 . . . . -159.6(3) ? C14 C7 C8 C9 . . . . 47.0(3) ? C14 C7 C8 C13 . . . . -135.2(3) ? C15 O2 C14 O1 . . . . 1.1(4) ? C15 O2 C14 C7 . . . . -178.8(2) ? C17 C18 C19 C20 . . . . -177.5(3) ? C17 C18 C23 C22 . . . . 179.2(3) ? C18 C17 C24 O3 . . . . 89.5(3) ? C18 C17 C24 O4 . . . . -87.2(3) ? C18 C19 C20 C21 . . . . -0.8(6) ? C19 C18 C23 C22 . . . . 1.9(5) ? C19 C20 C21 C22 . . . . 0.0(7) ? C20 C21 C22 C23 . . . . 1.8(6) ? C21 C22 C23 C18 . . . . -2.7(6) ? C23 C18 C19 C20 . . . . -0.2(5) ? C24 O4 C25 C26 . . . . 180.0(3) ? C24 C17 C18 C19 . . . . 135.3(3) ? C24 C17 C18 C23 . . . . -42.0(4) ? C25 O4 C24 O3 . . . . -0.6(4) ? C25 O4 C24 C17 . . . . 176.2(2) ? C27 N1 C1 C2 . . . . -172.8(3) ? C27 N1 C1 C3 . . . . 6.9(4) ? C27 C28 C29 C30 . . . . -0.5(4) ? C28 C27 C32 C31 . . . . -2.5(4) ? C28 C29 C30 C31 . . . . -2.2(4) ? C28 C29 C30 C33 . . . . 177.1(3) ? C29 C30 C31 C32 . . . . 2.5(5) ? C29 C30 C33 F1 . . . . -169.8(3) ? C29 C30 C33 F2 . . . . -51.3(4) ? C29 C30 C33 F3 . . . . 68.4(4) ? C30 C31 C32 C27 . . . . -0.1(4) ? C31 C30 C33 F1 . . . . 9.5(4) ? C31 C30 C33 F2 . . . . 127.9(3) ? C31 C30 C33 F3 . . . . -112.4(4) ? C32 C27 C28 C29 . . . . 2.8(4) ? C33 C30 C31 C32 . . . . -176.7(3) ?