#------------------------------------------------------------------------------ #$Date: 2020-09-18 06:25:59 +0300 (Fri, 18 Sep 2020) $ #$Revision: 256520 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/77/7157707.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_7157707 loop_ _publ_author_name 'Chen, Junrong' 'Li, Zhenmin' 'Suleman, Muhammad' 'Wang, Zaibin' 'Lu, Ping' 'Wang, Yanguang' _publ_section_title ; TfOH-Promoted Synthesis of 4,5-Dihydrooxazolo[5,4-c]isoquinolines via Formal [3+2] Cycloaddition of 4-Diazoisoquinolin-3-one and Benzonitriles ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D0OB01748E _journal_year 2020 _chemical_formula_moiety 'C16 H9 Cl N2 O' _chemical_formula_sum 'C16 H9 Cl N2 O' _chemical_formula_weight 280.70 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-12-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-05-11 deposited with the CCDC. 2020-09-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.854(16) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 22.757(10) _cell_length_b 4.748(2) _cell_length_c 23.677(10) _cell_measurement_reflns_used 6809 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 27.08 _cell_measurement_theta_min 2.79 _cell_volume 2472.8(18) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 170.0 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_unetI/netI 0.0425 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 18641 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.058 _diffrn_reflns_theta_min 2.778 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.7008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1587 before and 0.0479 after correction. The Ratio of minimum to maximum transmission is 0.9400. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.508 _exptl_crystal_description plate _exptl_crystal_F_000 1152 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.226 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 361 _refine_ls_number_reflns 5370 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0439 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+2.6219P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.1108 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4372 _reflns_number_total 5370 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob01748e2.cif _cod_data_source_block 191224_cjr490177_1_c_0m _cod_original_cell_volume 2472.8(19) _cod_database_code 7157707 _shelx_shelxl_version_number 2016/6 _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 0.985 _shelx_estimated_absorpt_t_min 0.868 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C23(H23), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32) ; _shelx_res_file ; TITL 191224_cjr490177_1_c_0m_a.res in P2(1)/c 191224_cjr490177_1_c_0m.res created by SHELXL-2016/6 at 15:22:48 on 24-Dec-2019 REM Old TITL 191224_CJR490177_1_C_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.100, Rweak 0.002, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C32 Cl2 N4 O2 CELL 0.71073 22.7569 4.748 23.6766 90 104.854 90 ZERR 8 0.0104 0.0021 0.0096 0 0.016 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O UNIT 128 72 8 16 8 L.S. 4 0 0 PLAN 20 SIZE 0.05 0.2 0.48 TEMP -103.15 BOND $H htab list 4 fmap 2 53 ACTA OMIT -2 0 2 OMIT -12 0 8 OMIT -6 0 6 OMIT 7 0 2 OMIT -4 0 2 OMIT -5 0 2 REM REM REM WGHT 0.035500 2.621900 FVAR 0.28016 CL1 3 0.793836 0.002976 0.386448 11.00000 0.02772 0.02824 = 0.03006 -0.00471 0.00487 0.00414 O1 5 0.557666 1.117510 0.450162 11.00000 0.02823 0.03149 = 0.01990 -0.00052 0.00419 0.00494 N1 4 0.637648 0.828283 0.506064 11.00000 0.03572 0.03824 = 0.01980 -0.00124 0.00388 0.00733 N2 4 0.561381 0.995402 0.358440 11.00000 0.02387 0.02389 = 0.02168 0.00041 0.00375 -0.00113 C1 1 0.731956 0.335927 0.443525 11.00000 0.02671 0.02399 = 0.02092 0.00061 0.00173 -0.00046 AFIX 43 H1 2 0.757734 0.262863 0.478542 11.00000 -1.20000 AFIX 0 C2 1 0.738051 0.248797 0.390190 11.00000 0.02209 0.02038 = 0.02570 -0.00208 0.00557 -0.00204 C3 1 0.700115 0.351115 0.337305 11.00000 0.02890 0.02626 = 0.01935 -0.00301 0.00556 -0.00347 AFIX 43 H3 2 0.705139 0.284261 0.301014 11.00000 -1.20000 AFIX 0 C4 1 0.656304 0.545618 0.338233 11.00000 0.02781 0.02585 = 0.02078 -0.00139 0.00236 -0.00236 AFIX 43 H4 2 0.631138 0.615847 0.302621 11.00000 -1.20000 AFIX 0 C5 1 0.648356 0.642717 0.392238 11.00000 0.02196 0.02141 = 0.02052 -0.00056 0.00405 -0.00470 C6 1 0.686404 0.537532 0.445591 11.00000 0.02408 0.02439 = 0.02022 -0.00051 0.00285 -0.00244 C7 1 0.678381 0.638506 0.499987 11.00000 0.03281 0.03523 = 0.02005 0.00074 0.00181 0.00528 AFIX 43 H7 2 0.704379 0.563497 0.534682 11.00000 -1.20000 AFIX 0 C8 1 0.602862 0.919335 0.454614 11.00000 0.02395 0.02622 = 0.02289 -0.00005 0.00612 0.00174 C9 1 0.604960 0.843681 0.399086 11.00000 0.02123 0.02233 = 0.02153 0.00028 0.00397 -0.00249 C10 1 0.535141 1.150410 0.390241 11.00000 0.02418 0.02569 = 0.02072 -0.00003 0.00453 -0.00307 C11 1 0.486452 1.354004 0.369376 11.00000 0.02460 0.02352 = 0.02440 -0.00020 0.00450 -0.00287 C12 1 0.467706 1.404523 0.309128 11.00000 0.02885 0.02762 = 0.02565 -0.00120 0.00635 0.00040 AFIX 43 H12 2 0.486247 1.306410 0.283265 11.00000 -1.20000 AFIX 0 C13 1 0.421901 1.598677 0.287434 11.00000 0.03030 0.03112 = 0.02646 0.00222 0.00308 0.00195 AFIX 43 H13 2 0.409091 1.633197 0.246589 11.00000 -1.20000 AFIX 0 C14 1 0.394674 1.742795 0.325030 11.00000 0.02711 0.02835 = 0.03580 0.00085 0.00577 0.00415 AFIX 43 H14 2 0.363391 1.875636 0.309866 11.00000 -1.20000 AFIX 0 C15 1 0.413214 1.692744 0.385122 11.00000 0.03174 0.03350 = 0.03380 -0.00445 0.01134 0.00463 AFIX 43 H15 2 0.394681 1.791858 0.410861 11.00000 -1.20000 AFIX 0 C16 1 0.458784 1.497833 0.407133 11.00000 0.02884 0.03171 = 0.02653 -0.00122 0.00758 0.00008 AFIX 43 H16 2 0.471177 1.462194 0.447953 11.00000 -1.20000 AFIX 0 CL2 3 1.090358 1.515742 0.608095 11.00000 0.02900 0.02758 = 0.03436 0.00066 0.00853 -0.00566 O2 5 0.822557 0.416243 0.588876 11.00000 0.02569 0.02917 = 0.02041 0.00253 0.00375 -0.00388 N3 4 0.856323 0.726727 0.525670 11.00000 0.03119 0.04184 = 0.01921 0.00417 0.00154 -0.00798 N4 4 0.891711 0.505983 0.674588 11.00000 0.02424 0.02232 = 0.01913 0.00104 0.00602 0.00082 C17 1 0.990588 1.196857 0.568227 11.00000 0.02813 0.02558 = 0.02386 0.00329 0.00737 0.00192 AFIX 43 H17 2 0.988531 1.280582 0.531328 11.00000 -1.20000 AFIX 0 C18 1 1.035913 1.270012 0.615963 11.00000 0.02609 0.02022 = 0.02994 -0.00086 0.01131 0.00077 C19 1 1.040131 1.150627 0.671707 11.00000 0.02581 0.02556 = 0.02632 -0.00280 0.00451 -0.00098 AFIX 43 H19 2 1.072034 1.205449 0.704279 11.00000 -1.20000 AFIX 0 C20 1 0.998030 0.955795 0.678473 11.00000 0.02660 0.02588 = 0.02249 0.00002 0.00527 0.00154 AFIX 43 H20 2 1.000790 0.876166 0.715873 11.00000 -1.20000 AFIX 0 C21 1 0.950418 0.872287 0.630087 11.00000 0.02398 0.02113 = 0.02082 -0.00135 0.00601 0.00287 C22 1 0.946675 0.995348 0.574101 11.00000 0.02449 0.02452 = 0.02290 -0.00003 0.00548 0.00021 C23 1 0.898979 0.915222 0.524867 11.00000 0.03299 0.03697 = 0.02153 0.00672 0.00368 -0.00540 AFIX 43 H23 2 0.897704 1.004103 0.488625 11.00000 -1.20000 AFIX 0 C24 1 0.862125 0.617194 0.578571 11.00000 0.02356 0.02552 = 0.02309 0.00058 0.00602 -0.00255 C25 1 0.904537 0.671522 0.630598 11.00000 0.02354 0.02229 = 0.01916 0.00067 0.00491 0.00335 C26 1 0.843677 0.361645 0.647892 11.00000 0.02486 0.02298 = 0.01989 0.00047 0.00649 0.00414 C27 1 0.809566 0.152845 0.671761 11.00000 0.02292 0.02073 = 0.02500 0.00019 0.00749 0.00367 C28 1 0.759797 0.013172 0.635541 11.00000 0.02758 0.02462 = 0.02436 -0.00110 0.00726 0.00036 AFIX 43 H28 2 0.747837 0.054081 0.594922 11.00000 -1.20000 AFIX 0 C29 1 0.727825 -0.185750 0.659067 11.00000 0.02859 0.02736 = 0.03414 -0.00363 0.01163 -0.00245 AFIX 43 H29 2 0.694065 -0.280869 0.634549 11.00000 -1.20000 AFIX 0 C30 1 0.745423 -0.244526 0.718385 11.00000 0.03189 0.02514 = 0.03803 0.00525 0.01457 0.00164 AFIX 43 H30 2 0.723670 -0.380489 0.734429 11.00000 -1.20000 AFIX 0 C31 1 0.794775 -0.105504 0.754573 11.00000 0.03356 0.03413 = 0.02743 0.00666 0.01117 0.00314 AFIX 43 H31 2 0.806403 -0.146461 0.795197 11.00000 -1.20000 AFIX 0 C32 1 0.827097 0.092763 0.731587 11.00000 0.02657 0.02823 = 0.02639 0.00196 0.00493 0.00068 AFIX 43 H32 2 0.860870 0.186914 0.756310 11.00000 -1.20000 AFIX 0 HKLF 4 REM 191224_cjr490177_1_c_0m_a.res in P2(1)/c REM R1 = 0.0439 for 4372 Fo > 4sig(Fo) and 0.0573 for all 5370 data REM 361 parameters refined using 0 restraints END WGHT 0.0380 2.6228 REM Instructions for potential hydrogen bonds EQIV $1 x, y+1, z HTAB C23 Cl1_$1 REM Highest difference peak 0.226, deepest hole -0.283, 1-sigma level 0.059 Q1 1 0.6995 0.4039 0.4413 11.00000 0.05 0.23 Q2 1 0.8780 0.6795 0.6058 11.00000 0.05 0.22 Q3 1 0.6415 0.5400 0.3625 11.00000 0.05 0.22 Q4 1 0.6775 0.6268 0.4206 11.00000 0.05 0.22 Q5 1 0.6178 0.6965 0.3951 11.00000 0.05 0.21 Q6 1 0.4619 1.3444 0.3784 11.00000 0.05 0.21 Q7 1 0.8219 0.2840 0.6653 11.00000 0.05 0.20 Q8 1 0.6004 0.8647 0.4233 11.00000 0.05 0.20 Q9 1 0.7949 0.5297 0.3870 11.00000 0.05 0.20 Q10 1 1.0583 1.3778 0.7184 11.00000 0.05 0.20 Q11 1 0.6201 0.8758 0.4807 11.00000 0.05 0.20 Q12 1 0.5023 1.2360 0.3773 11.00000 0.05 0.19 Q13 1 0.8172 0.1303 0.7005 11.00000 0.05 0.19 Q14 1 0.7384 -0.1416 0.6998 11.00000 0.05 0.19 Q15 1 1.0996 0.9758 0.6156 11.00000 0.05 0.18 Q16 1 0.7588 0.2485 0.2788 11.00000 0.05 0.18 Q17 1 0.4774 1.4038 0.3416 11.00000 0.05 0.18 Q18 1 0.6823 0.5519 0.4760 11.00000 0.05 0.18 Q19 1 1.1207 1.4420 0.6440 11.00000 0.05 0.18 Q20 1 0.7267 0.3280 0.3620 11.00000 0.05 0.18 ; _shelx_res_checksum 94042 _shelx_hkl_file ; -3 0 0 173.98 5.00 3 0 0 173.28 4.90 -4 0 0 14.60 0.70 4 0 0 15.60 0.70 -5 0 0 124.29 4.00 5 0 0 134.79 3.90 -6 0 0 182.28 5.80 6 0 0 196.88 5.60 -7 0 0 5.70 0.60 7 0 0 5.60 0.60 -8 0 0 140.69 4.80 8 0 0 155.38 4.70 -9 0 0 57.69 2.50 9 0 0 64.99 2.40 -10 0 0 118.19 4.30 10 0 0 128.09 4.20 -11 0 0 451.15 13.80 11 0 0 481.65 13.60 -12 0 0 2.80 0.60 12 0 0 2.80 0.60 -13 0 0 35.60 2.10 13 0 0 39.80 2.10 -14 0 0 81.69 3.60 14 0 0 83.19 3.40 -15 0 0 30.90 2.10 15 0 0 35.00 2.10 -16 0 0 94.69 4.30 16 0 0 101.49 4.20 -17 0 0 150.28 6.00 17 0 0 152.28 5.90 18 0 0 25.50 2.10 -19 0 0 110.89 5.30 19 0 0 128.49 5.40 -20 0 0 360.96 12.60 20 0 0 385.56 12.70 -21 0 0 15.70 2.00 21 0 0 16.10 1.90 22 0 0 57.69 3.80 -23 0 0 134.69 6.50 23 0 0 147.29 6.70 -24 0 0 0.30 0.90 24 0 0 0.80 0.80 -25 0 0 3.90 1.40 25 0 0 5.20 1.50 -26 0 0 9.50 3.00 26 0 0 10.40 2.20 -27 0 0 54.89 4.20 27 0 0 54.29 4.30 -28 0 0 1.20 1.40 28 0 0 2.70 1.00 27 -1 0 23.20 2.60 -27 1 0 24.10 3.30 26 -1 0 2.80 2.00 -26 1 0 1.30 1.40 25 -1 0 -0.40 0.70 -25 1 0 0.70 1.10 24 -1 0 3.90 1.20 -24 1 0 3.40 1.40 23 -1 0 13.10 1.70 -23 1 0 13.40 2.40 22 -1 0 0.50 0.70 21 -1 0 0.20 0.50 -21 1 0 -0.30 0.70 20 -1 0 31.70 2.20 -20 1 0 34.20 3.00 19 -1 0 42.90 3.30 -19 1 0 41.80 3.30 18 -1 0 91.49 3.90 -18 1 0 87.09 4.90 17 -1 0 11.50 1.30 -17 1 0 8.20 1.60 16 -1 0 2.80 0.80 -16 1 0 2.20 0.90 15 -1 0 3.30 0.80 -15 1 0 4.20 1.00 14 -1 0 39.50 2.20 -14 1 0 40.00 2.70 13 -1 0 33.90 2.00 -13 1 0 32.10 2.40 12 -1 0 58.29 2.70 -12 1 0 56.29 3.20 11 -1 0 41.40 2.20 -11 1 0 42.60 2.60 10 -1 0 24.90 1.60 -10 1 0 27.10 2.00 9 -1 0 446.66 13.20 -9 1 0 440.96 13.70 8 -1 0 194.88 6.60 -8 1 0 199.88 7.00 7 -1 0 0.50 0.40 -7 1 0 0.50 0.50 6 -1 0 106.59 4.00 -6 1 0 104.49 4.20 5 -1 0 71.49 3.00 4 -1 0 1274.27 35.50 -4 1 0 1264.97 35.60 3 -1 0 189.28 6.30 -3 1 0 188.28 6.30 2 -1 0 57.59 2.60 -2 1 0 58.59 2.60 1 -1 0 66.09 2.80 -1 1 0 61.69 2.70 0 -1 0 0.10 0.40 0 -1 0 -0.20 0.30 -1 -1 0 66.29 2.90 1 1 0 67.99 2.90 -2 -1 0 58.39 2.70 2 1 0 59.59 2.70 -3 -1 0 192.18 6.30 3 1 0 184.18 6.40 4 1 0 1231.08 34.60 -5 -1 0 69.69 3.00 5 1 0 75.59 3.30 -6 -1 0 115.89 4.20 6 1 0 105.79 4.40 -7 -1 0 0.10 0.30 7 1 0 -0.70 0.50 -8 -1 0 202.88 6.60 8 1 0 201.88 7.20 -9 -1 0 477.85 14.00 9 1 0 468.65 14.70 -10 -1 0 26.80 1.60 10 1 0 27.90 2.10 -11 -1 0 46.00 2.20 11 1 0 44.00 2.80 -12 -1 0 64.59 2.80 12 1 0 67.59 3.60 -13 -1 0 32.30 1.80 13 1 0 34.50 2.50 -14 -1 0 40.70 2.10 14 1 0 41.40 2.90 -15 -1 0 3.70 0.80 15 1 0 3.70 1.10 -16 -1 0 2.50 0.70 16 1 0 2.10 0.90 17 1 0 10.50 1.80 -18 -1 0 92.59 4.10 18 1 0 92.59 5.10 -19 -1 0 43.20 3.00 19 1 0 46.70 3.60 20 1 0 29.50 2.90 21 1 0 -0.20 0.70 -22 -1 0 2.20 0.90 22 1 0 1.20 1.00 -23 -1 0 11.30 1.80 23 1 0 9.60 2.20 -24 -1 0 4.50 1.30 24 1 0 5.00 1.70 25 1 0 -0.60 0.90 -26 -1 0 0.80 1.20 26 1 0 4.00 1.70 -27 -1 0 23.40 2.70 27 1 0 19.30 3.20 26 -2 0 23.80 2.30 -26 2 0 22.10 4.10 -25 2 0 2.90 1.70 24 -2 0 26.00 2.20 -24 2 0 27.90 3.50 23 -2 0 0.20 0.80 -23 2 0 -0.90 1.00 22 -2 0 2.90 0.90 21 -2 0 15.10 1.70 -21 2 0 16.10 2.70 20 -2 0 34.80 2.50 -20 2 0 35.90 3.40 19 -2 0 8.00 1.40 -19 2 0 6.20 1.60 18 -2 0 6.10 1.50 -18 2 0 6.40 2.10 17 -2 0 4.70 1.20 -17 2 0 3.70 1.30 16 -2 0 4.40 1.20 -16 2 0 6.00 1.60 15 -2 0 14.60 1.60 -15 2 0 12.70 2.10 14 -2 0 2.80 0.90 -14 2 0 1.80 0.90 13 -2 0 13.00 1.50 -13 2 0 13.70 2.20 12 -2 0 6.20 1.20 -12 2 0 6.30 1.40 11 -2 0 96.49 4.40 -11 2 0 94.79 5.00 10 -2 0 233.68 8.40 -10 2 0 227.68 9.00 9 -2 0 827.62 24.50 -9 2 0 818.12 25.20 8 -2 0 524.95 16.30 -8 2 0 505.65 16.60 7 -2 0 468.25 15.00 -7 2 0 469.25 15.30 6 -2 0 32.50 2.40 -6 2 0 30.40 2.50 5 -2 0 11.60 1.50 -5 2 0 11.40 1.50 4 -2 0 47.40 3.40 -4 2 0 42.20 2.80 3 -2 0 405.06 14.00 -3 2 0 400.26 13.00 2 -2 0 14.90 1.60 -2 2 0 13.90 1.50 1 -2 0 120.89 5.30 1 -2 0 123.19 5.40 0 -2 0 434.46 13.90 0 -2 0 419.96 13.90 -1 -2 0 115.59 5.20 -1 -2 0 114.89 5.10 -2 -2 0 16.20 1.70 2 2 0 15.60 1.70 -3 -2 0 402.36 13.30 3 2 0 409.26 13.30 -4 -2 0 40.20 2.70 4 2 0 45.60 3.00 -5 -2 0 10.50 1.40 5 2 0 11.40 1.70 -6 -2 0 32.30 2.40 6 2 0 31.50 2.60 -7 -2 0 452.05 14.90 7 2 0 481.65 15.50 -8 -2 0 531.55 16.40 8 2 0 507.65 16.90 -9 -2 0 866.51 25.00 9 2 0 808.52 25.70 -10 -2 0 244.68 8.60 10 2 0 229.38 9.30 -11 -2 0 100.99 4.50 11 2 0 96.09 5.20 -12 -2 0 5.00 1.00 12 2 0 7.10 1.70 -13 -2 0 12.00 1.40 13 2 0 11.30 2.00 -14 -2 0 1.80 0.70 14 2 0 2.20 1.20 15 2 0 11.90 2.10 -16 -2 0 4.70 1.00 16 2 0 5.80 1.60 17 2 0 8.20 1.90 18 2 0 6.50 1.80 19 2 0 7.30 1.90 20 2 0 39.50 3.80 21 2 0 11.70 2.40 -22 -2 0 4.00 1.00 22 2 0 3.80 1.50 -23 -2 0 0.60 0.80 23 2 0 1.10 1.20 -24 -2 0 26.00 2.40 24 2 0 32.40 3.90 -25 -2 0 4.60 1.30 25 2 0 4.10 1.90 26 2 0 22.30 3.90 24 -3 0 2.10 1.10 -24 3 0 2.70 1.80 -23 3 0 14.40 2.90 22 -3 0 1.40 1.00 -22 3 0 -1.00 1.30 21 -3 0 23.20 2.40 20 -3 0 10.90 1.80 -20 3 0 10.80 2.40 19 -3 0 -0.20 0.60 -19 3 0 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8.30 1.60 9 3 0 9.50 2.00 -10 -3 0 21.30 2.30 10 3 0 23.20 2.70 -11 -3 0 95.59 5.20 11 3 0 93.69 5.80 -12 -3 0 49.60 3.60 12 3 0 50.59 4.20 -13 -3 0 2.70 1.00 13 3 0 1.60 1.10 -14 -3 0 78.99 4.50 14 3 0 75.79 5.30 -15 -3 0 0.80 0.70 15 3 0 -0.50 0.70 -16 -3 0 17.80 1.90 16 3 0 12.70 2.70 -17 -3 0 16.30 1.90 17 3 0 18.10 3.20 -18 -3 0 1.10 0.90 18 3 0 0.30 0.90 -19 -3 0 0.20 0.60 19 3 0 2.10 1.30 -20 -3 0 14.70 1.80 20 3 0 15.00 3.00 -21 -3 0 29.00 3.70 21 3 0 28.80 3.70 -22 -3 0 -0.80 0.60 22 3 0 1.90 1.40 -23 -3 0 13.40 1.70 23 3 0 16.80 3.40 24 3 0 -0.80 1.60 21 -4 0 -2.20 0.80 20 -4 0 12.90 3.10 19 -4 0 5.70 1.70 -19 4 0 10.10 2.40 18 -4 0 -2.10 0.90 -18 4 0 2.20 1.40 17 -4 0 65.79 4.40 -17 4 0 68.09 5.20 16 -4 0 1.40 1.00 -16 4 0 1.70 1.30 -15 4 0 4.00 2.00 14 -4 0 0.20 0.90 -14 4 0 0.60 0.90 13 -4 0 1.30 0.90 -13 4 0 0.80 1.00 12 -4 0 0.60 0.80 -12 4 0 0.70 1.10 11 -4 0 12.10 2.10 -11 4 0 10.10 2.20 10 -4 0 42.40 3.80 -10 4 0 38.40 3.50 9 -4 0 78.39 5.20 -9 4 0 89.99 5.40 8 -4 0 8.00 2.00 7 -4 0 35.70 3.40 6 -4 0 163.98 8.80 6 -4 0 168.68 8.30 5 -4 0 1.30 1.00 5 -4 0 1.10 1.00 4 -4 0 14.30 2.60 4 -4 0 16.10 2.90 3 -4 0 0.40 0.90 3 -4 0 0.00 0.60 2 -4 0 10.60 2.30 2 -4 0 9.90 2.20 1 -4 0 111.79 6.70 1 -4 0 110.19 6.60 0 -4 0 16.30 2.90 0 -4 0 10.10 2.20 -1 -4 0 112.19 6.60 -1 -4 0 104.19 6.50 -2 -4 0 13.60 2.70 -2 -4 0 13.50 2.50 -3 -4 0 0.60 0.70 -3 -4 0 0.60 0.80 -4 -4 0 14.20 2.80 -4 -4 0 15.30 2.70 -5 -4 0 0.70 1.00 -6 -4 0 172.28 9.10 -6 -4 0 160.08 8.20 -7 -4 0 42.50 4.20 -7 -4 0 35.90 3.50 -8 -4 0 7.60 2.10 -8 -4 0 10.40 2.20 8 4 0 6.40 2.00 -9 -4 0 88.59 5.60 9 4 0 88.79 5.80 -10 -4 0 43.80 3.70 10 4 0 40.10 3.90 -11 -4 0 10.10 2.00 11 4 0 7.30 2.00 -12 -4 0 2.40 1.20 12 4 0 1.90 1.10 -13 -4 0 1.30 1.00 13 4 0 -1.20 0.80 -14 -4 0 0.00 0.80 -15 -4 0 0.50 0.80 15 4 0 1.20 1.20 -16 -4 0 2.60 1.20 16 4 0 3.10 1.60 -17 -4 0 79.69 5.00 17 4 0 76.39 6.10 -18 -4 0 1.30 1.10 18 4 0 2.50 1.60 -19 -4 0 7.60 1.70 19 4 0 8.60 2.50 -20 -4 0 16.50 2.20 20 4 0 18.50 3.60 21 4 0 0.40 1.30 15 -5 0 2.60 1.50 14 -5 0 1.30 1.40 13 -5 0 1.80 1.40 12 -5 0 1.50 1.10 11 -5 0 0.80 1.10 10 -5 0 8.30 2.60 10 -5 0 8.00 2.10 9 -5 0 0.80 1.40 9 -5 0 1.00 1.20 8 -5 0 7.30 2.30 8 -5 0 6.70 1.90 7 -5 0 29.70 3.80 7 -5 0 22.80 3.10 6 -5 0 28.00 3.50 6 -5 0 25.20 4.00 5 -5 0 -1.20 1.00 5 -5 0 0.50 1.00 4 -5 0 8.70 2.40 4 -5 0 12.00 2.80 3 -5 0 14.60 2.80 3 -5 0 9.10 2.30 2 -5 0 0.80 1.20 2 -5 0 2.20 1.10 1 -5 0 0.10 0.90 1 -5 0 -1.60 0.90 0 -5 0 0.80 1.00 0 -5 0 -1.10 0.90 -1 -5 0 0.60 1.00 -1 -5 0 0.90 1.00 -2 -5 0 2.30 1.30 -2 -5 0 -1.90 0.90 -3 -5 0 12.80 2.80 -3 -5 0 17.70 3.50 -4 -5 0 7.70 2.10 -4 -5 0 10.20 2.60 -5 -5 0 1.50 1.00 -6 -5 0 28.00 3.50 -6 -5 0 29.30 4.60 -7 -5 0 22.50 4.10 -7 -5 0 23.50 3.80 -8 -5 0 3.80 1.90 -8 -5 0 8.60 2.20 -9 -5 0 1.00 1.00 -9 -5 0 3.10 1.60 -10 -5 0 8.10 2.20 -10 -5 0 12.50 3.20 -11 -5 0 1.30 1.40 -11 -5 0 1.50 0.90 -13 -5 0 4.60 1.70 -13 -5 0 4.00 1.80 13 5 0 7.40 1.90 -14 -5 0 2.60 1.40 14 5 0 1.90 1.70 -15 -5 0 7.70 2.50 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347.97 12.00 13 3 -3 297.17 11.90 12 3 -3 52.09 4.00 -12 -3 3 55.39 3.60 11 3 -3 30.60 3.00 -11 -3 3 33.90 2.80 10 3 -3 1.90 1.00 -10 -3 3 4.00 1.10 9 3 -3 1.30 0.90 -9 -3 3 1.30 0.70 8 3 -3 2.50 1.00 -8 -3 3 3.70 1.20 7 3 -3 63.19 3.90 -7 -3 3 60.89 3.90 -6 -3 3 25.40 2.50 -5 -3 3 85.99 4.70 -4 -3 3 136.49 6.40 -3 -3 3 155.58 7.00 -2 -3 3 32.80 2.80 -2 -3 3 31.60 2.80 -1 -3 3 68.29 4.20 -1 -3 3 72.59 4.30 0 -3 3 17.60 2.00 0 -3 3 14.70 1.90 1 -3 3 179.38 7.70 1 -3 3 178.88 7.60 2 -3 3 71.89 4.30 3 -3 3 327.17 11.80 4 -3 3 6.00 1.40 5 -3 3 133.89 6.20 6 -3 3 185.78 7.80 -7 3 -3 97.49 4.60 7 -3 3 99.39 5.10 -8 3 -3 2.00 0.90 8 -3 3 1.50 0.80 -9 3 -3 84.39 4.50 9 -3 3 87.79 4.70 -10 3 -3 35.60 2.90 10 -3 3 35.90 2.80 -11 3 -3 6.80 1.50 11 -3 3 5.10 1.30 -12 3 -3 37.00 3.10 12 -3 3 38.00 2.90 -13 3 -3 33.50 3.00 13 -3 3 31.80 2.60 -14 3 -3 5.00 1.40 14 -3 3 6.20 1.30 -15 3 -3 13.00 2.20 15 -3 3 11.90 1.90 -16 3 -3 50.39 3.90 16 -3 3 52.89 3.30 -17 3 -3 2.20 1.20 17 -3 3 1.20 0.80 -18 3 -3 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2.90 4 -1 26 2.30 1.20 5 -1 26 0.40 1.10 6 -1 26 -1.60 0.80 7 -1 26 -0.40 0.80 -20 0 26 3.70 1.30 -19 0 26 24.30 3.20 -18 0 26 5.00 1.90 -17 0 26 2.10 1.30 -16 0 26 28.60 3.40 -15 0 26 11.00 2.30 -14 0 26 28.90 3.20 -13 0 26 0.20 1.00 -12 0 26 64.39 4.80 -11 0 26 0.40 0.90 -10 0 26 41.50 3.90 -8 0 26 22.60 3.00 -7 0 26 7.10 2.10 -6 0 26 3.50 1.60 -5 0 26 -1.00 0.80 -4 0 26 -1.90 0.80 -4 0 26 1.40 1.00 -3 0 26 10.50 2.30 -3 0 26 13.60 2.70 -2 0 26 31.00 3.50 -2 0 26 34.90 3.70 -1 0 26 -0.80 1.00 -1 0 26 -0.70 0.80 0 0 26 -0.10 0.90 1 0 26 1.60 1.20 2 0 26 2.00 1.20 4 0 26 1.50 1.10 5 0 26 9.40 2.40 6 0 26 33.00 3.60 7 0 26 16.40 3.10 8 0 26 56.29 4.90 20 -1 -26 -1.40 1.00 20 -1 -26 -0.20 0.60 19 -1 -26 2.70 1.20 19 -1 -26 1.50 0.70 -19 1 26 6.30 1.90 18 -1 -26 19.30 2.30 18 -1 -26 19.10 1.50 17 -1 -26 2.90 0.70 17 -1 -26 5.20 1.30 -17 1 26 3.70 1.50 16 -1 -26 2.70 1.20 16 -1 -26 5.50 0.80 -16 1 26 5.00 1.90 15 -1 -26 17.80 1.80 15 -1 -26 18.30 1.30 -15 1 26 21.60 3.80 14 -1 -26 8.80 1.30 -14 1 26 11.40 2.80 13 -1 -26 2.80 0.70 13 -1 -26 4.30 0.60 -13 1 26 3.70 1.70 12 -1 -26 0.90 0.30 -12 1 26 -1.40 1.00 -11 1 26 -1.30 1.00 -10 1 26 0.50 1.50 -9 1 26 -1.90 1.30 -7 1 26 3.00 1.70 -6 1 26 2.60 1.50 -5 1 26 1.50 1.40 -4 1 26 0.20 1.00 -4 1 26 -0.10 1.20 -3 1 26 4.20 1.70 -3 1 26 2.40 1.60 -2 1 26 1.10 1.20 -2 1 26 0.40 1.20 -1 1 26 -1.50 1.40 -1 1 26 6.70 2.00 0 1 26 4.80 1.90 1 1 26 9.10 2.20 2 1 26 25.80 4.10 3 1 26 31.00 3.90 4 1 26 3.40 1.50 5 1 26 7.20 2.00 6 1 26 -2.80 1.00 7 1 26 -1.30 1.20 17 -2 -26 31.00 2.50 -17 2 26 36.50 4.90 16 -2 -26 26.20 2.70 16 -2 -26 29.30 3.40 -16 2 26 29.20 5.00 15 -2 -26 5.20 1.60 15 -2 -26 5.30 1.10 -15 2 26 9.40 2.40 14 -2 -26 1.60 0.90 14 -2 -26 3.20 1.40 -14 2 26 5.10 2.10 13 -2 -26 1.00 1.20 13 -2 -26 0.30 0.70 12 -2 -26 13.10 3.30 12 -2 -26 14.20 1.60 -12 2 26 14.00 3.40 11 -2 -26 1.50 0.80 -11 2 26 -1.50 1.10 10 -2 -26 11.90 1.50 10 -2 -26 12.00 2.00 -10 2 26 12.80 3.20 9 -2 -26 -1.20 0.60 9 -2 -26 1.00 0.90 -9 2 26 -1.70 1.20 8 -2 -26 1.00 0.90 8 -2 -26 0.90 0.80 -8 2 26 0.60 1.10 7 -2 -26 43.80 2.60 7 -2 -26 42.10 3.00 -7 2 26 47.50 5.10 6 -2 -26 1.80 0.90 6 -2 -26 1.80 0.80 -6 2 26 2.20 1.50 5 -2 -26 2.60 0.80 5 -2 -26 1.80 0.80 -5 2 26 2.60 1.50 4 -2 -26 0.30 0.70 4 -2 -26 1.80 0.80 -4 2 26 3.00 1.40 3 -2 -26 30.00 2.10 3 -2 -26 29.20 2.20 -3 2 26 31.10 4.20 -3 2 26 36.00 4.40 2 -2 -26 47.30 2.60 2 -2 -26 48.90 2.90 -2 2 26 51.99 5.40 -2 2 26 52.79 5.40 1 -2 -26 3.50 0.80 1 -2 -26 0.90 0.90 -1 2 26 1.50 1.70 0 -2 -26 0.80 0.50 0 -2 -26 1.40 0.90 0 2 26 -0.80 1.50 -1 -2 -26 11.70 1.10 -1 -2 -26 11.90 1.70 1 2 26 4.00 2.20 -2 -2 -26 8.30 1.00 -2 -2 -26 6.90 1.30 2 2 26 4.50 2.20 -3 -2 -26 3.30 1.10 3 2 26 1.50 1.70 -4 -2 -26 13.90 1.20 -4 -2 -26 9.00 1.60 4 2 26 8.40 2.50 10 -3 -26 18.20 2.30 10 -3 -26 21.70 3.40 9 -3 -26 -0.90 0.90 9 -3 -26 0.50 1.20 -9 3 26 4.70 2.50 8 -3 -26 0.60 1.10 8 -3 -26 -0.50 0.80 -8 3 26 3.30 2.10 7 -3 -26 0.90 1.20 7 -3 -26 -1.60 0.80 -7 3 26 -3.00 1.50 6 -3 -26 19.00 2.90 6 -3 -26 16.80 2.40 -6 3 26 12.00 3.40 5 -3 -26 0.60 1.10 5 -3 -26 0.90 1.10 -5 3 26 -1.20 1.90 4 -3 -26 -0.30 1.10 4 -3 -26 0.30 0.90 -4 3 26 -2.50 1.40 3 -3 -26 2.10 1.20 3 -3 -26 3.40 1.30 -15 -2 27 3.70 1.30 -14 -2 27 3.40 1.10 -13 -2 27 3.80 0.90 -11 -2 27 0.80 0.70 -10 -2 27 1.00 0.80 -9 -2 27 13.20 1.90 -8 -2 27 3.60 1.20 -7 -2 27 9.60 1.70 -4 -2 27 7.00 1.50 -3 -2 27 4.60 1.20 -3 -2 27 4.80 1.20 -2 -2 27 1.80 0.70 -1 -2 27 0.60 0.70 0 -2 27 1.50 0.90 1 -2 27 2.00 1.10 2 -2 27 4.60 1.20 -18 -1 27 3.00 1.80 -17 -1 27 2.50 1.40 -16 -1 27 47.60 4.00 -15 -1 27 43.70 3.80 -14 -1 27 4.30 1.60 -13 -1 27 -1.70 0.90 -12 -1 27 39.70 3.50 -11 -1 27 4.70 1.40 -10 -1 27 3.00 1.30 -8 -1 27 49.10 3.70 -7 -1 27 5.00 1.60 -6 -1 27 38.50 3.40 -5 -1 27 38.80 3.30 -4 -1 27 9.00 1.90 -4 -1 27 9.30 1.90 -3 -1 27 1.50 1.10 -3 -1 27 3.40 1.30 -2 -1 27 -0.20 0.80 -2 -1 27 -1.20 0.80 -1 -1 27 0.80 0.80 0 -1 27 15.80 2.50 1 -1 27 24.50 2.80 2 -1 27 43.40 3.80 3 -1 27 -0.60 0.80 4 -1 27 43.50 3.70 5 -1 27 8.00 1.90 -19 0 27 2.30 1.20 -18 0 27 -0.80 1.10 -17 0 27 2.90 1.20 -16 0 27 3.00 1.20 -15 0 27 1.30 0.90 -14 0 27 0.60 1.10 -13 0 27 0.60 0.80 -12 0 27 -0.10 1.00 -11 0 27 1.00 0.90 -10 0 27 1.80 1.00 -9 0 27 1.40 1.30 -8 0 27 -1.30 1.00 -7 0 27 -1.50 0.90 -4 0 27 2.40 1.00 -3 0 27 2.10 0.90 -2 0 27 -2.40 1.00 -2 0 27 1.00 1.00 -1 0 27 0.10 1.00 -1 0 27 0.00 0.80 0 0 27 0.10 0.90 3 0 27 0.20 0.90 5 0 27 -0.20 1.00 6 0 27 1.30 1.30 18 -1 -27 2.40 0.70 18 -1 -27 4.90 1.20 -18 1 27 3.70 1.70 17 -1 -27 3.60 0.90 17 -1 -27 2.90 0.90 16 -1 -27 48.00 2.60 -16 1 27 51.79 5.30 15 -1 -27 38.00 1.70 15 -1 -27 41.50 2.40 -15 1 27 37.60 4.60 -14 1 27 8.70 2.30 -13 1 27 0.20 1.10 -12 1 27 46.00 4.90 -11 1 27 4.20 1.90 -10 1 27 7.90 2.10 -8 1 27 43.70 4.70 -7 1 27 6.20 2.10 -6 1 27 36.70 4.20 -5 1 27 29.60 3.90 -4 1 27 10.70 2.70 -4 1 27 11.40 2.70 -3 1 27 5.20 2.00 -3 1 27 7.30 2.20 -2 1 27 0.20 1.30 -2 1 27 -0.40 0.80 -1 1 27 -0.70 1.10 0 1 27 12.60 3.10 1 1 27 22.70 3.80 2 1 27 40.10 4.50 3 1 27 0.80 1.50 4 1 27 47.20 4.90 5 1 27 4.80 2.20 15 -2 -27 7.60 2.00 15 -2 -27 7.10 1.20 -15 2 27 12.30 3.00 14 -2 -27 4.50 1.50 14 -2 -27 2.40 0.90 -14 2 27 5.40 2.10 13 -2 -27 2.20 1.70 13 -2 -27 2.10 0.90 -13 2 27 1.60 1.50 12 -2 -27 -0.80 0.70 -12 2 27 1.00 1.40 11 -2 -27 -0.70 0.70 11 -2 -27 0.50 0.90 -11 2 27 -0.10 1.90 10 -2 -27 1.30 0.90 10 -2 -27 -0.70 0.70 9 -2 -27 15.40 1.70 9 -2 -27 17.00 2.00 -9 2 27 18.50 4.10 8 -2 -27 5.70 1.10 8 -2 -27 7.20 1.40 -8 2 27 10.90 2.80 7 -2 -27 12.10 1.60 7 -2 -27 13.70 1.50 -7 2 27 17.30 3.50 6 -2 -27 -0.50 0.70 6 -2 -27 -0.10 0.60 -6 2 27 2.70 1.60 5 -2 -27 -0.30 0.70 5 -2 -27 0.60 0.60 -5 2 27 1.90 1.70 4 -2 -27 8.90 1.20 4 -2 -27 9.00 1.30 -4 2 27 13.80 2.80 3 -2 -27 7.10 1.10 3 -2 -27 4.80 0.90 -3 2 27 10.60 2.70 2 -2 -27 0.40 0.50 2 -2 -27 0.10 0.60 -2 2 27 -0.10 1.20 1 -2 -27 -0.20 0.40 1 -2 -27 0.10 0.60 -1 2 27 0.90 1.60 0 -2 -27 1.30 0.70 0 -2 -27 0.00 0.40 0 2 27 1.70 1.80 -1 -2 -27 0.70 0.40 -1 -2 -27 0.20 0.70 1 2 27 4.10 1.70 -2 -2 -27 1.10 0.80 -2 -2 -27 1.40 0.50 2 2 27 0.40 1.60 -12 -2 28 -0.90 0.80 -11 -2 28 13.80 2.10 -10 -2 28 30.70 2.60 -8 -2 28 23.50 2.30 -7 -2 28 26.10 2.40 -6 -2 28 10.40 1.70 -5 -2 28 0.70 0.70 -4 -2 28 8.70 1.60 -3 -2 28 11.50 1.90 -2 -2 28 2.90 1.20 -16 -1 28 0.40 1.40 -15 -1 28 -1.20 1.00 -14 -1 28 0.10 1.00 -13 -1 28 6.00 1.50 -12 -1 28 -0.80 1.30 -11 -1 28 3.40 1.30 -10 -1 28 -1.40 0.80 -9 -1 28 1.80 1.00 -8 -1 28 -0.30 0.80 -7 -1 28 -2.20 0.80 -6 -1 28 0.80 1.00 -5 -1 28 0.70 0.70 -4 -1 28 6.20 1.30 -4 -1 28 4.00 1.30 -3 -1 28 2.90 1.20 -3 -1 28 3.40 1.20 -2 -1 28 10.00 2.00 -2 -1 28 8.00 1.90 -1 -1 28 -0.60 0.70 0 -1 28 1.00 1.00 1 -1 28 14.50 2.40 2 -1 28 -1.30 1.00 -17 0 28 28.90 4.20 -16 0 28 -0.40 1.20 -15 0 28 2.20 1.50 -14 0 28 17.40 3.00 -13 0 28 6.20 1.60 -12 0 28 23.80 3.60 -11 0 28 34.10 3.60 -10 0 28 27.10 3.50 -9 0 28 4.20 1.70 -8 0 28 3.20 1.60 -7 0 28 14.40 2.80 -6 0 28 13.90 2.60 -5 0 28 74.69 5.40 -4 0 28 22.50 3.00 -4 0 28 27.40 3.70 -3 0 28 12.00 3.60 -3 0 28 13.40 2.50 -2 0 28 75.69 5.70 -1 0 28 48.90 5.00 0 0 28 36.40 3.90 1 0 28 2.50 1.30 2 0 28 6.70 1.90 3 0 28 1.70 1.00 -16 1 28 0.90 3.30 -15 1 28 1.60 1.70 -14 1 28 3.10 1.50 -13 1 28 7.10 2.30 -12 1 28 1.20 1.30 -11 1 28 5.30 2.10 -10 1 28 2.20 1.50 -9 1 28 1.20 1.30 -8 1 28 1.40 1.40 -7 1 28 -2.20 1.20 -6 1 28 1.10 1.60 -5 1 28 -2.30 1.20 -4 1 28 1.50 1.80 -3 1 28 2.30 1.70 -3 1 28 1.20 1.20 -2 1 28 7.50 2.40 -2 1 28 11.10 2.70 -1 1 28 3.40 1.80 0 1 28 3.30 1.50 1 1 28 18.80 3.50 2 1 28 0.40 1.70 12 -2 -28 1.10 1.00 12 -2 -28 0.50 0.70 -12 2 28 3.70 1.80 11 -2 -28 11.80 1.40 11 -2 -28 12.10 1.80 -11 2 28 14.40 3.60 10 -2 -28 25.00 2.20 10 -2 -28 23.50 1.80 -10 2 28 32.50 4.20 9 -2 -28 -0.20 0.70 9 -2 -28 0.10 0.70 -9 2 28 0.90 1.40 8 -2 -28 21.80 1.70 8 -2 -28 20.00 1.90 -8 2 28 19.20 4.10 7 -2 -28 27.50 1.80 7 -2 -28 22.70 1.80 -7 2 28 23.50 4.30 6 -2 -28 11.50 1.30 6 -2 -28 10.00 1.20 -6 2 28 10.20 2.90 5 -2 -28 0.00 0.60 5 -2 -28 0.20 0.60 -5 2 28 -1.90 1.10 4 -2 -28 10.70 1.10 4 -2 -28 11.00 1.20 -4 2 28 9.80 2.90 3 -2 -28 12.80 1.10 3 -2 -28 11.00 1.20 -3 2 28 12.40 3.30 2 -2 -28 2.70 0.60 2 -2 -28 3.80 1.50 -2 2 28 5.70 1.90 -13 -1 29 -0.70 1.00 -12 -1 29 2.60 1.10 -11 -1 29 -1.30 0.80 -10 -1 29 -0.20 0.90 -9 -1 29 23.10 3.30 -8 -1 29 2.20 1.30 -7 -1 29 11.30 2.20 -6 -1 29 17.50 2.30 -5 -1 29 8.60 1.60 -4 -1 29 2.30 1.00 -3 -1 29 0.40 1.00 -3 -1 29 3.30 1.30 -2 -1 29 -2.20 0.80 -1 -1 29 14.30 2.60 -15 0 29 0.00 1.10 -14 0 29 0.30 1.20 -13 0 29 2.70 1.30 -12 0 29 3.00 1.30 -11 0 29 2.50 1.40 -10 0 29 0.60 1.20 -9 0 29 0.40 1.30 -8 0 29 1.20 1.20 -7 0 29 1.30 1.30 -6 0 29 1.80 1.30 -5 0 29 0.80 1.00 -4 0 29 1.40 1.10 -4 0 29 0.80 1.10 -3 0 29 2.00 1.10 -3 0 29 2.00 1.30 -2 0 29 -0.50 1.10 -2 0 29 1.30 1.20 -1 0 29 1.20 1.10 0 0 29 0.60 1.20 1 0 29 1.70 1.20 -13 1 29 3.00 1.60 -12 1 29 5.80 1.90 -11 1 29 2.30 1.50 -10 1 29 0.40 1.30 -9 1 29 35.10 4.00 -8 1 29 7.60 2.00 -7 1 29 16.80 3.20 -6 1 29 11.00 2.80 -5 1 29 2.60 2.20 -3 1 29 3.40 1.80 -3 1 29 0.00 1.70 -2 1 29 -0.20 1.20 -2 1 29 -2.60 1.00 -1 1 29 19.30 3.80 -11 0 30 3.60 1.70 -10 0 30 22.90 3.70 -9 0 30 3.60 1.80 -8 0 30 19.00 3.40 -7 0 30 3.30 1.80 -6 0 30 2.50 1.30 -5 0 30 3.20 1.40 -4 0 30 28.50 3.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 443 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.79384(2) 0.00298(12) 0.38645(2) 0.02914(13) Uani 1 1 d . . . . . O1 O 0.55767(6) 1.1175(3) 0.45016(6) 0.0269(3) Uani 1 1 d . . . . . N1 N 0.63765(9) 0.8283(4) 0.50606(8) 0.0318(4) Uani 1 1 d . . . . . N2 N 0.56138(8) 0.9954(4) 0.35844(7) 0.0235(4) Uani 1 1 d . . . . . C1 C 0.73196(9) 0.3359(5) 0.44352(9) 0.0247(4) Uani 1 1 d . . . . . H1 H 0.757734 0.262863 0.478542 0.030 Uiso 1 1 calc R . . . . C2 C 0.73805(9) 0.2488(4) 0.39019(9) 0.0228(4) Uani 1 1 d . . . . . C3 C 0.70012(9) 0.3511(5) 0.33731(9) 0.0250(4) Uani 1 1 d . . . . . H3 H 0.705139 0.284261 0.301014 0.030 Uiso 1 1 calc R . . . . C4 C 0.65630(10) 0.5456(5) 0.33823(9) 0.0255(4) Uani 1 1 d . . . . . H4 H 0.631138 0.615847 0.302621 0.031 Uiso 1 1 calc R . . . . C5 C 0.64836(9) 0.6427(4) 0.39224(8) 0.0216(4) Uani 1 1 d . . . . . C6 C 0.68640(9) 0.5375(5) 0.44559(9) 0.0234(4) Uani 1 1 d . . . . . C7 C 0.67838(10) 0.6385(5) 0.49999(9) 0.0303(5) Uani 1 1 d . . . . . H7 H 0.704379 0.563497 0.534682 0.036 Uiso 1 1 calc R . . . . C8 C 0.60286(9) 0.9193(5) 0.45461(9) 0.0243(4) Uani 1 1 d . . . . . C9 C 0.60496(9) 0.8437(4) 0.39909(8) 0.0220(4) Uani 1 1 d . . . . . C10 C 0.53514(9) 1.1504(5) 0.39024(9) 0.0238(4) Uani 1 1 d . . . . . C11 C 0.48645(9) 1.3540(5) 0.36938(9) 0.0245(4) Uani 1 1 d . . . . . C12 C 0.46771(10) 1.4045(5) 0.30913(9) 0.0275(5) Uani 1 1 d . . . . . H12 H 0.486247 1.306410 0.283265 0.033 Uiso 1 1 calc R . . . . C13 C 0.42190(10) 1.5987(5) 0.28743(10) 0.0301(5) Uani 1 1 d . . . . . H13 H 0.409091 1.633197 0.246589 0.036 Uiso 1 1 calc R . . . . C14 C 0.39467(10) 1.7428(5) 0.32503(10) 0.0308(5) Uani 1 1 d . . . . . H14 H 0.363391 1.875636 0.309866 0.037 Uiso 1 1 calc R . . . . C15 C 0.41321(10) 1.6927(5) 0.38512(10) 0.0325(5) Uani 1 1 d . . . . . H15 H 0.394681 1.791858 0.410861 0.039 Uiso 1 1 calc R . . . . C16 C 0.45878(10) 1.4978(5) 0.40713(10) 0.0289(5) Uani 1 1 d . . . . . H16 H 0.471177 1.462194 0.447953 0.035 Uiso 1 1 calc R . . . . Cl2 Cl 1.09036(2) 1.51574(12) 0.60810(2) 0.03024(14) Uani 1 1 d . . . . . O2 O 0.82256(6) 0.4162(3) 0.58888(6) 0.0255(3) Uani 1 1 d . . . . . N3 N 0.85632(9) 0.7267(4) 0.52567(8) 0.0316(4) Uani 1 1 d . . . . . N4 N 0.89171(7) 0.5060(4) 0.67459(7) 0.0218(3) Uani 1 1 d . . . . . C17 C 0.99059(10) 1.1969(5) 0.56823(9) 0.0257(4) Uani 1 1 d . . . . . H17 H 0.988531 1.280582 0.531328 0.031 Uiso 1 1 calc R . . . . C18 C 1.03591(9) 1.2700(4) 0.61596(9) 0.0247(4) Uani 1 1 d . . . . . C19 C 1.04013(9) 1.1506(5) 0.67171(9) 0.0263(4) Uani 1 1 d . . . . . H19 H 1.072034 1.205449 0.704279 0.032 Uiso 1 1 calc R . . . . C20 C 0.99803(9) 0.9558(5) 0.67847(9) 0.0252(4) Uani 1 1 d . . . . . H20 H 1.000790 0.876166 0.715873 0.030 Uiso 1 1 calc R . . . . C21 C 0.95042(9) 0.8723(4) 0.63009(8) 0.0219(4) Uani 1 1 d . . . . . C22 C 0.94667(9) 0.9953(5) 0.57410(9) 0.0241(4) Uani 1 1 d . . . . . C23 C 0.89898(10) 0.9152(5) 0.52487(9) 0.0311(5) Uani 1 1 d . . . . . H23 H 0.897704 1.004103 0.488625 0.037 Uiso 1 1 calc R . . . . C24 C 0.86213(9) 0.6172(5) 0.57857(9) 0.0240(4) Uani 1 1 d . . . . . C25 C 0.90454(9) 0.6715(4) 0.63060(8) 0.0218(4) Uani 1 1 d . . . . . C26 C 0.84368(9) 0.3616(5) 0.64789(8) 0.0224(4) Uani 1 1 d . . . . . C27 C 0.80957(9) 0.1528(4) 0.67176(9) 0.0226(4) Uani 1 1 d . . . . . C28 C 0.75980(9) 0.0132(5) 0.63554(9) 0.0254(4) Uani 1 1 d . . . . . H28 H 0.747837 0.054081 0.594922 0.030 Uiso 1 1 calc R . . . . C29 C 0.72782(10) -0.1858(5) 0.65907(10) 0.0294(5) Uani 1 1 d . . . . . H29 H 0.694065 -0.280869 0.634549 0.035 Uiso 1 1 calc R . . . . C30 C 0.74542(10) -0.2445(5) 0.71839(10) 0.0307(5) Uani 1 1 d . . . . . H30 H 0.723670 -0.380489 0.734429 0.037 Uiso 1 1 calc R . . . . C31 C 0.79477(10) -0.1055(5) 0.75457(10) 0.0311(5) Uani 1 1 d . . . . . H31 H 0.806403 -0.146461 0.795197 0.037 Uiso 1 1 calc R . . . . C32 C 0.82710(10) 0.0928(5) 0.73159(9) 0.0274(5) Uani 1 1 d . . . . . H32 H 0.860870 0.186914 0.756310 0.033 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0277(3) 0.0282(3) 0.0301(3) -0.0047(2) 0.0049(2) 0.0041(2) O1 0.0282(7) 0.0315(8) 0.0199(7) -0.0005(6) 0.0042(6) 0.0049(7) N1 0.0357(10) 0.0382(11) 0.0198(9) -0.0012(8) 0.0039(7) 0.0073(9) N2 0.0239(8) 0.0239(9) 0.0217(8) 0.0004(7) 0.0038(7) -0.0011(7) C1 0.0267(10) 0.0240(11) 0.0209(10) 0.0006(8) 0.0017(8) -0.0005(8) C2 0.0221(9) 0.0204(10) 0.0257(10) -0.0021(8) 0.0056(8) -0.0020(8) C3 0.0289(10) 0.0263(11) 0.0194(9) -0.0030(8) 0.0056(8) -0.0035(9) C4 0.0278(10) 0.0258(11) 0.0208(10) -0.0014(8) 0.0024(8) -0.0024(9) C5 0.0220(9) 0.0214(10) 0.0205(9) -0.0006(8) 0.0041(7) -0.0047(8) C6 0.0241(10) 0.0244(11) 0.0202(9) -0.0005(8) 0.0029(7) -0.0024(8) C7 0.0328(11) 0.0352(13) 0.0201(10) 0.0007(9) 0.0018(8) 0.0053(10) C8 0.0240(10) 0.0262(11) 0.0229(10) -0.0001(8) 0.0061(8) 0.0017(8) C9 0.0212(9) 0.0223(10) 0.0215(10) 0.0003(8) 0.0040(7) -0.0025(8) C10 0.0242(10) 0.0257(11) 0.0207(10) 0.0000(8) 0.0045(8) -0.0031(8) C11 0.0246(10) 0.0235(11) 0.0244(10) -0.0002(8) 0.0045(8) -0.0029(8) C12 0.0288(11) 0.0276(12) 0.0256(10) -0.0012(9) 0.0063(8) 0.0004(9) C13 0.0303(11) 0.0311(12) 0.0265(11) 0.0022(9) 0.0031(8) 0.0020(9) C14 0.0271(11) 0.0283(12) 0.0358(12) 0.0009(9) 0.0058(9) 0.0041(9) C15 0.0317(12) 0.0335(13) 0.0338(12) -0.0044(10) 0.0113(9) 0.0046(10) C16 0.0288(11) 0.0317(12) 0.0265(10) -0.0012(9) 0.0076(8) 0.0001(9) Cl2 0.0290(3) 0.0276(3) 0.0344(3) 0.0007(2) 0.0085(2) -0.0057(2) O2 0.0257(7) 0.0292(8) 0.0204(7) 0.0025(6) 0.0037(6) -0.0039(6) N3 0.0312(10) 0.0418(12) 0.0192(9) 0.0042(8) 0.0015(7) -0.0080(8) N4 0.0242(8) 0.0223(9) 0.0191(8) 0.0010(7) 0.0060(6) 0.0008(7) C17 0.0281(10) 0.0256(11) 0.0239(10) 0.0033(8) 0.0074(8) 0.0019(9) C18 0.0261(10) 0.0202(10) 0.0299(11) -0.0009(8) 0.0113(8) 0.0008(8) C19 0.0258(10) 0.0256(11) 0.0263(10) -0.0028(9) 0.0045(8) -0.0010(9) C20 0.0266(10) 0.0259(11) 0.0225(10) 0.0000(8) 0.0053(8) 0.0015(8) C21 0.0240(10) 0.0211(10) 0.0208(9) -0.0014(8) 0.0060(7) 0.0029(8) C22 0.0245(10) 0.0245(11) 0.0229(10) 0.0000(8) 0.0055(8) 0.0002(8) C23 0.0330(11) 0.0370(13) 0.0215(10) 0.0067(9) 0.0037(8) -0.0054(10) C24 0.0236(10) 0.0255(11) 0.0231(10) 0.0006(8) 0.0060(8) -0.0026(8) C25 0.0235(9) 0.0223(10) 0.0192(9) 0.0007(8) 0.0049(7) 0.0034(8) C26 0.0249(10) 0.0230(11) 0.0199(9) 0.0005(8) 0.0065(8) 0.0041(8) C27 0.0229(9) 0.0207(10) 0.0250(10) 0.0002(8) 0.0075(8) 0.0037(8) C28 0.0276(10) 0.0246(11) 0.0244(10) -0.0011(8) 0.0073(8) 0.0004(9) C29 0.0286(11) 0.0274(12) 0.0341(12) -0.0036(9) 0.0116(9) -0.0024(9) C30 0.0319(12) 0.0251(12) 0.0380(12) 0.0052(9) 0.0146(10) 0.0016(9) C31 0.0336(11) 0.0341(13) 0.0274(11) 0.0067(9) 0.0112(9) 0.0031(10) C32 0.0266(10) 0.0282(12) 0.0264(11) 0.0020(9) 0.0049(8) 0.0007(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 O1 C10 103.17(15) . . ? C7 N1 C8 112.71(18) . . ? C10 N2 C9 104.10(17) . . ? C2 C1 H1 120.6 . . ? C2 C1 C6 118.85(18) . . ? C6 C1 H1 120.6 . . ? C1 C2 Cl1 119.76(16) . . ? C1 C2 C3 122.0(2) . . ? C3 C2 Cl1 118.21(16) . . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.14(19) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 120.0 . . ? C3 C4 C5 119.94(19) . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 119.83(19) . . ? C9 C5 C4 125.42(19) . . ? C9 C5 C6 114.74(18) . . ? C1 C6 C5 119.21(18) . . ? C1 C6 C7 121.32(18) . . ? C5 C6 C7 119.47(19) . . ? N1 C7 C6 125.44(19) . . ? N1 C7 H7 117.3 . . ? C6 C7 H7 117.3 . . ? N1 C8 O1 122.97(18) . . ? N1 C8 C9 128.8(2) . . ? C9 C8 O1 108.26(17) . . ? N2 C9 C5 131.71(18) . . ? C8 C9 N2 109.41(18) . . ? C8 C9 C5 118.87(18) . . ? O1 C10 C11 118.06(18) . . ? N2 C10 O1 115.05(18) . . ? N2 C10 C11 126.88(18) . . ? C12 C11 C10 117.72(19) . . ? C16 C11 C10 122.38(19) . . ? C16 C11 C12 119.9(2) . . ? C11 C12 H12 120.2 . . ? C13 C12 C11 119.6(2) . . ? C13 C12 H12 120.2 . . ? C12 C13 H13 119.8 . . ? C12 C13 C14 120.4(2) . . ? C14 C13 H13 119.8 . . ? C13 C14 H14 120.0 . . ? C13 C14 C15 120.1(2) . . ? C15 C14 H14 120.0 . . ? C14 C15 H15 120.1 . . ? C16 C15 C14 119.8(2) . . ? C16 C15 H15 120.1 . . ? C11 C16 H16 119.9 . . ? C15 C16 C11 120.1(2) . . ? C15 C16 H16 119.9 . . ? C24 O2 C26 103.64(15) . . ? C23 N3 C24 112.42(18) . . ? C26 N4 C25 104.10(16) . . ? C18 C17 H17 120.2 . . ? C18 C17 C22 119.54(19) . . ? C22 C17 H17 120.2 . . ? C17 C18 Cl2 119.19(17) . . ? C17 C18 C19 121.7(2) . . ? C19 C18 Cl2 119.09(16) . . ? C18 C19 H19 120.1 . . ? C20 C19 C18 119.8(2) . . ? C20 C19 H19 120.1 . . ? C19 C20 H20 119.8 . . ? C19 C20 C21 120.5(2) . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 119.10(19) . . ? C25 C21 C20 126.45(19) . . ? C25 C21 C22 114.44(18) . . ? C17 C22 C21 119.41(19) . . ? C17 C22 C23 120.57(19) . . ? C23 C22 C21 120.03(19) . . ? N3 C23 C22 125.2(2) . . ? N3 C23 H23 117.4 . . ? C22 C23 H23 117.4 . . ? O2 C24 C25 108.12(17) . . ? N3 C24 O2 121.75(18) . . ? N3 C24 C25 130.1(2) . . ? N4 C25 C21 132.99(18) . . ? C24 C25 N4 109.20(18) . . ? C24 C25 C21 117.81(18) . . ? O2 C26 C27 115.96(17) . . ? N4 C26 O2 114.95(18) . . ? N4 C26 C27 129.09(18) . . ? C28 C27 C26 120.78(19) . . ? C32 C27 C26 119.25(19) . . ? C32 C27 C28 120.0(2) . . ? C27 C28 H28 120.0 . . ? C29 C28 C27 120.0(2) . . ? C29 C28 H28 120.0 . . ? C28 C29 H29 120.1 . . ? C30 C29 C28 119.8(2) . . ? C30 C29 H29 120.1 . . ? C29 C30 H30 119.8 . . ? C29 C30 C31 120.4(2) . . ? C31 C30 H30 119.8 . . ? C30 C31 H31 119.8 . . ? C32 C31 C30 120.3(2) . . ? C32 C31 H31 119.8 . . ? C27 C32 H32 120.2 . . ? C31 C32 C27 119.5(2) . . ? C31 C32 H32 120.2 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C2 1.743(2) . ? O1 C8 1.378(3) . ? O1 C10 1.388(2) . ? N1 C7 1.327(3) . ? N1 C8 1.343(3) . ? N2 C9 1.393(3) . ? N2 C10 1.302(3) . ? C1 H1 0.9500 . ? C1 C2 1.369(3) . ? C1 C6 1.421(3) . ? C2 C3 1.412(3) . ? C3 H3 0.9500 . ? C3 C4 1.363(3) . ? C4 H4 0.9500 . ? C4 C5 1.414(3) . ? C5 C6 1.426(3) . ? C5 C9 1.412(3) . ? C6 C7 1.429(3) . ? C7 H7 0.9500 . ? C8 C9 1.375(3) . ? C10 C11 1.458(3) . ? C11 C12 1.401(3) . ? C11 C16 1.397(3) . ? C12 H12 0.9500 . ? C12 C13 1.388(3) . ? C13 H13 0.9500 . ? C13 C14 1.388(3) . ? C14 H14 0.9500 . ? C14 C15 1.397(3) . ? C15 H15 0.9500 . ? C15 C16 1.388(3) . ? C16 H16 0.9500 . ? Cl2 C18 1.746(2) . ? O2 C24 1.376(3) . ? O2 C26 1.381(2) . ? N3 C23 1.324(3) . ? N3 C24 1.331(3) . ? N4 C25 1.394(3) . ? N4 C26 1.308(3) . ? C17 H17 0.9500 . ? C17 C18 1.365(3) . ? C17 C22 1.416(3) . ? C18 C19 1.417(3) . ? C19 H19 0.9500 . ? C19 C20 1.370(3) . ? C20 H20 0.9500 . ? C20 C21 1.417(3) . ? C21 C22 1.431(3) . ? C21 C25 1.416(3) . ? C22 C23 1.426(3) . ? C23 H23 0.9500 . ? C24 C25 1.381(3) . ? C26 C27 1.459(3) . ? C27 C28 1.400(3) . ? C27 C32 1.399(3) . ? C28 H28 0.9500 . ? C28 C29 1.393(3) . ? C29 H29 0.9500 . ? C29 C30 1.387(3) . ? C30 H30 0.9500 . ? C30 C31 1.392(3) . ? C31 H31 0.9500 . ? C31 C32 1.389(3) . ? C32 H32 0.9500 . ?