#------------------------------------------------------------------------------ #$Date: 2018-01-04 00:27:18 +0200 (Thu, 04 Jan 2018) $ #$Revision: 204694 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/43/4514340.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_4514340 loop_ _publ_author_name 'Korvorapun, Korkit' 'Kaplaneris, Nikolaos' 'Rogge, Torben' 'Warratz, Svenja' 'St\"uckl, A. Claudia' 'Ackermann, Lutz' _publ_section_title ; Sequential meta-/ortho-C--H Functionalizations by One-Pot Ruthenium(II/III) Catalysis ; _journal_name_full 'ACS Catalysis' _journal_page_first 886 _journal_paper_doi 10.1021/acscatal.7b03648 _journal_year 2018 _chemical_formula_moiety 'C17 H19 N3 O2' _chemical_formula_sum 'C17 H19 N3 O2' _chemical_formula_weight 297.35 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-08-02 _audit_creation_method ; Olex2 1.2 (compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370) ; _cell_angle_alpha 90 _cell_angle_beta 99.887(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.0431(10) _cell_length_b 9.7828(11) _cell_length_c 15.4733(11) _cell_measurement_reflns_used 1825 _cell_measurement_temperature 100 _cell_measurement_theta_max 26.84 _cell_measurement_theta_min 2.64 _cell_volume 1497.7(2) _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 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.01 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _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 0.0229 _diffrn_reflns_av_unetI/netI 0.0212 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 20654 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.598 _diffrn_reflns_theta_min 2.253 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9206 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0897 before and 0.0455 after correction. The Ratio of minimum to maximum transmission is 0.9169. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.319 _exptl_crystal_description block _exptl_crystal_F_000 632 _exptl_crystal_size_max 0.283 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.138 _refine_diff_density_max 0.458 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 255 _refine_ls_number_reflns 5448 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0406 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.4105P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1135 _refine_ls_wR_factor_ref 0.1176 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4815 _reflns_number_total 5448 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs7b03648_si_005.cif _cod_data_source_block mo_0090_cg_0m _cod_database_code 4514340 _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 0.988 _shelx_estimated_absorpt_t_min 0.975 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Sof(O2B)=Sof(N3B)=Sof(C14B)=Sof(H14C)=Sof(H14D)=Sof(C15B)=Sof(H15C)=Sof(H15D)= Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=1-FVAR(1) Sof(O2A)=Sof(N3A)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)= Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=FVAR(1) 3.a Ternary CH refined with riding coordinates: C11(H11) 3.b Secondary CH2 refined with riding coordinates: C14A(H14A,H14B), C14B(H14C,H14D), C15A(H15A,H15B), C15B(H15C,H15D), C16A(H16A, H16B), C16B(H16C,H16D), C17A(H17A,H17B), C17B(H17C,H17D) 3.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C6(H6), C8(H8), C9(H9), C10(H10) 3.d Idealised Me refined as rotating group: C12(H12A,H12B,H12C) ; _shelx_res_file ; TITL mo_0090_cg_0m_a.res in P2(1)/n mo_0090_cg_0m.res created by SHELXL-2016/6 at 13:07:34 on 02-Aug-2017 REM Old TITL mo_0090_CG_0m in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.251, Rweak 0.068, Alpha 0.066, Orientation as input REM Formula found by SHELXT: C19 N2 O CELL 0.71073 10.0431 9.7828 15.4733 90 99.887 90 ZERR 4 0.001 0.0011 0.0011 0 0.004 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 68 76 12 8 L.S. 4 PLAN 5 SIZE 0.138 0.2 0.283 TEMP -173.14 BOND $H list 4 fmap 2 ACTA OMIT -6 0 6 OMIT 0 6 6 OMIT 0 7 7 REM REM REM WGHT 0.060500 0.410500 FVAR 0.78066 0.73345 O1 4 0.081391 0.772917 0.417029 11.00000 0.02308 0.02133 = 0.01992 -0.00484 0.00315 0.00258 PART 1 O2A 4 0.348560 0.397827 0.569767 21.00000 0.04989 0.02481 = 0.01974 0.00472 -0.00091 0.00461 PART 0 PART 2 O2B 4 0.365410 0.423590 0.559258 -21.00000 0.03792 0.03865 = 0.02509 0.00183 -0.00818 0.00624 PART 0 N1 3 0.545343 0.925533 0.398694 11.00000 0.01477 0.02052 = 0.01582 -0.00542 0.00291 -0.00042 N2 3 0.702057 0.854612 0.308058 11.00000 0.01563 0.02382 = 0.02068 -0.00594 0.00633 -0.00204 PART 1 N3A 3 0.198952 0.575570 0.445759 21.00000 0.02537 0.01505 = 0.01298 -0.00023 0.00199 0.00108 PART 0 PART 2 N3B 3 0.158033 0.558313 0.441581 -21.00000 0.02939 0.02387 = 0.01351 -0.00450 0.00082 0.00126 PART 0 C1 1 0.580046 0.853949 0.332170 11.00000 0.01344 0.01611 = 0.01341 -0.00162 0.00189 0.00104 C2 1 0.642402 1.002505 0.445342 11.00000 0.01659 0.02111 = 0.01533 -0.00441 0.00245 -0.00130 AFIX 43 H2 2 0.621063 1.055200 0.492697 11.00000 -1.20000 AFIX 0 C3 1 0.772605 1.008183 0.427172 11.00000 0.01508 0.02028 = 0.01664 -0.00175 0.00105 -0.00182 AFIX 43 H3 2 0.841101 1.062042 0.461107 11.00000 -1.20000 AFIX 0 C4 1 0.797090 0.930718 0.356612 11.00000 0.01510 0.02405 = 0.02282 -0.00480 0.00574 -0.00211 AFIX 43 H4 2 0.885264 0.931778 0.342142 11.00000 -1.20000 AFIX 0 C5 1 0.474379 0.766812 0.280562 11.00000 0.01421 0.01561 = 0.01387 -0.00253 0.00131 0.00125 C6 1 0.350609 0.747218 0.308539 11.00000 0.01506 0.01410 = 0.01293 -0.00198 0.00138 0.00083 AFIX 43 H6 2 0.333889 0.792048 0.360078 11.00000 -1.20000 AFIX 0 C7 1 0.251357 0.663078 0.262139 11.00000 0.01505 0.01300 = 0.01341 -0.00090 0.00063 0.00116 C8 1 0.276660 0.598868 0.185974 11.00000 0.01908 0.01679 = 0.01594 -0.00480 0.00030 0.00054 AFIX 43 H8 2 0.209625 0.541844 0.153357 11.00000 -1.20000 AFIX 0 C9 1 0.399465 0.617967 0.157633 11.00000 0.02045 0.02394 = 0.01688 -0.00849 0.00333 0.00135 AFIX 43 H9 2 0.415756 0.573889 0.105742 11.00000 -1.20000 AFIX 0 C10 1 0.498648 0.701155 0.204713 11.00000 0.01733 0.02392 = 0.01736 -0.00663 0.00369 0.00128 AFIX 43 H10 2 0.582617 0.713219 0.185287 11.00000 -1.20000 AFIX 0 C11 1 0.115435 0.642689 0.290892 11.00000 0.01680 0.01512 = 0.01417 -0.00240 0.00155 -0.00223 AFIX 13 H11 2 0.086762 0.545724 0.278627 11.00000 -1.20000 AFIX 0 C12 1 0.009067 0.735893 0.238345 11.00000 0.01631 0.02719 = 0.01848 -0.00163 -0.00006 0.00267 AFIX 137 H12A 2 0.034537 0.831607 0.250355 11.00000 -1.50000 H12B 2 -0.078954 0.718461 0.255408 11.00000 -1.50000 H12C 2 0.003406 0.717380 0.175576 11.00000 -1.50000 AFIX 0 C13 1 0.126610 0.668105 0.389414 11.00000 0.02003 0.01629 = 0.01563 -0.00110 0.00301 -0.00161 PART 1 C14A 1 0.284727 0.467852 0.418412 21.00000 0.03210 0.01553 = 0.01734 0.00201 0.00366 0.00450 AFIX 23 H14A 2 0.375136 0.505561 0.414952 21.00000 -1.20000 H14B 2 0.244114 0.433856 0.359505 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C14B 1 0.215517 0.428642 0.418089 -21.00000 0.03913 0.01851 = 0.02097 -0.00364 0.00067 -0.00046 AFIX 23 H14C 2 0.213851 0.425525 0.353961 -21.00000 -1.20000 H14D 2 0.160394 0.351701 0.433966 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C15A 1 0.298546 0.351155 0.483717 21.00000 0.04810 0.01707 = 0.02058 0.00385 0.00119 0.00297 AFIX 23 H15A 2 0.209268 0.307547 0.482406 21.00000 -1.20000 H15B 2 0.360838 0.281510 0.466820 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C15B 1 0.358485 0.414153 0.465399 -21.00000 0.04364 0.02529 = 0.02154 0.00369 0.00328 0.00449 AFIX 23 H15C 2 0.395033 0.324771 0.450658 -21.00000 -1.20000 H15D 2 0.414947 0.486889 0.445703 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C16A 1 0.252799 0.488917 0.596354 21.00000 0.04802 0.02825 = 0.01563 0.00485 0.00517 0.00088 AFIX 23 H16A 2 0.284272 0.517108 0.657921 21.00000 -1.20000 H16B 2 0.165107 0.441392 0.593413 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C16B 1 0.313006 0.550991 0.581123 -21.00000 0.04788 0.03255 = 0.01603 -0.00090 0.00348 -0.00783 AFIX 23 H16C 2 0.368530 0.625659 0.562724 -21.00000 -1.20000 H16D 2 0.318980 0.556746 0.645552 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C17A 1 0.233763 0.614386 0.538210 21.00000 0.03934 0.02119 = 0.01357 -0.00118 0.00185 0.00004 AFIX 23 H17A 2 0.160879 0.671983 0.554494 21.00000 -1.20000 H17B 2 0.318136 0.668786 0.547310 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C17B 1 0.168308 0.569828 0.537691 -21.00000 0.04352 0.03210 = 0.01600 -0.00198 0.00999 -0.00257 AFIX 23 H17C 2 0.111039 0.499336 0.558993 -21.00000 -1.20000 H17D 2 0.135702 0.660781 0.552825 -21.00000 -1.20000 AFIX 0 HKLF 4 REM mo_0090_cg_0m_a.res in P2(1)/n REM R1 = 0.0406 for 4815 Fo > 4sig(Fo) and 0.0452 for all 5448 data REM 255 parameters refined using 0 restraints END WGHT 0.0605 0.4105 REM Highest difference peak 0.458, deepest hole -0.224, 1-sigma level 0.046 Q1 1 0.7095 1.0075 0.4334 11.00000 0.05 0.46 Q2 1 0.4170 0.7558 0.2978 11.00000 0.05 0.45 Q3 1 0.3040 0.7043 0.2861 11.00000 0.05 0.43 Q4 1 0.4823 0.7394 0.2413 11.00000 0.05 0.43 Q5 1 0.7783 0.9737 0.3896 11.00000 0.05 0.42 ; _shelx_res_checksum 43744 _shelx_hkl_file ; 2 0 0 4270.18 121.600 1 -2 0 0 4227.08 121.155 1 3 0 0 -0.0192 0.13451 2 -3 0 0 0.54259 0.20320 5 3 0 0 0.02794 0.12227 5 -3 0 0 0.19141 0.15171 2 4 0 0 128.817 3.48718 2 -4 0 0 129.195 3.50543 2 -4 0 0 147.988 3.76523 5 4 0 0 145.562 3.75770 5 -5 0 0 3.99042 0.45730 2 5 0 0 2.52867 0.45445 5 -5 0 0 2.48716 0.43951 5 5 0 0 2.31246 0.35132 2 -6 0 0 49.1080 1.73649 2 -7 0 0 12.0827 1.01187 5 -8 0 0 216.901 5.81612 2 -8 0 0 214.157 6.19541 5 8 0 0 217.823 5.75701 3 -9 0 0 0.35120 0.42026 5 9 0 0 0.80610 0.45317 3 -9 0 0 0.77977 0.40386 2 10 0 0 60.2843 2.39877 3 -10 0 0 59.2772 2.42554 2 -10 0 0 58.6185 2.78157 5 -11 0 0 -0.0092 0.40900 2 -11 0 0 0.46024 0.54369 5 -12 0 0 9.13721 1.14779 2 -12 0 0 7.83694 1.28042 5 12 0 0 9.50176 1.17369 3 -13 0 0 0.17484 0.52869 2 13 0 0 -0.4772 0.52538 3 -14 0 0 93.1762 4.37882 5 14 0 0 92.5373 3.72151 3 -14 0 0 96.4404 3.74091 2 -1 -1 0 328.781 7.41563 5 1 -1 0 315.370 7.42490 3 -1 -1 0 316.606 7.31304 4 1 1 0 326.467 7.31334 4 -1 1 0 341.033 7.43540 3 -2 -1 0 3000.25 94.4522 1 2 -1 0 2868.00 92.8340 1 2 1 0 2870.36 94.9773 1 -2 1 0 2871.41 93.7594 1 3 -1 0 130.272 3.44325 3 3 -1 0 133.552 3.49838 2 3 -1 0 145.183 3.63615 5 -3 -1 0 144.438 3.60772 5 3 1 0 144.255 3.61461 5 -3 1 0 130.631 3.49892 2 -3 1 0 145.392 3.64758 5 4 -1 0 94.8382 2.82560 5 4 -1 0 106.065 2.73943 2 -4 -1 0 105.192 2.65586 2 4 -1 0 97.3926 2.66372 3 -4 -1 0 93.6111 2.80132 5 4 1 0 91.1817 2.79283 5 -4 1 0 94.0106 2.83237 5 -4 1 0 101.025 2.75565 2 5 -1 0 150.218 3.98998 2 5 -1 0 155.040 3.96818 3 -5 -1 0 144.741 4.09463 2 5 -1 0 155.134 4.22856 5 -5 -1 0 156.062 4.20844 5 -5 1 0 147.260 4.01703 2 5 1 0 147.652 4.17654 5 6 -1 0 1.58861 0.36415 3 -6 -1 0 1.35632 0.34603 2 6 -1 0 3.40410 0.49372 2 -6 -1 0 1.38593 0.34480 5 -6 1 0 2.58766 0.56685 5 -6 1 0 1.12810 0.31898 2 7 -1 0 75.9305 2.50381 3 -7 -1 0 77.1440 2.76903 5 -7 -1 0 76.0675 2.46165 2 -7 1 0 74.1317 2.54254 2 -7 1 0 78.4307 2.82526 5 -8 -1 0 125.743 4.04410 5 -8 -1 0 119.608 3.61617 2 8 -1 0 116.589 3.63171 3 -8 1 0 124.174 4.07450 5 -8 1 0 121.759 3.73972 2 -9 -1 0 148.472 4.92031 5 -9 -1 0 152.711 4.45281 2 9 -1 0 156.820 4.53885 3 -9 1 0 153.166 4.58932 2 -10 -1 0 14.9047 1.13578 2 10 -1 0 15.8590 1.23346 3 -10 -1 0 14.0502 1.37993 5 -10 1 0 15.5536 1.44777 5 -10 1 0 16.4742 1.26039 2 -11 -1 0 0.28763 0.53906 5 -11 -1 0 1.49350 0.52731 2 -11 1 0 0.73385 0.62285 5 11 1 0 1.62050 0.70512 3 -11 1 0 0.87335 0.54100 2 -12 -1 0 1.85736 0.58945 2 -12 -1 0 -0.2791 0.47175 5 12 -1 0 0.64213 0.54217 3 12 1 0 0.02357 0.43765 3 -12 1 0 0.49232 0.56032 2 -12 1 0 0.16730 0.63576 5 13 -1 0 42.9229 2.35212 3 -13 -1 0 44.9155 2.27264 2 -13 -1 0 43.4795 3.02016 5 -13 1 0 40.5565 2.30386 2 13 1 0 40.6881 2.21173 3 -13 1 0 37.5611 3.42602 5 -14 -1 0 31.5874 1.98864 2 -14 -1 0 33.1756 2.52832 5 14 -1 0 34.8806 2.17437 3 14 1 0 29.5970 1.99041 3 -14 1 0 30.1919 2.04963 2 0 -2 0 12.7167 0.55803 2 0 -2 0 13.2444 0.63313 3 0 2 0 12.8061 0.61352 3 -1 -2 0 6332.32 171.378 1 1 -2 0 5813.00 167.651 1 -1 2 0 5867.01 169.660 1 1 2 0 5776.30 169.036 1 2 -2 0 7229.35 207.056 1 -2 -2 0 7496.79 208.710 1 2 2 0 7533.05 212.183 1 -2 2 0 7632.75 211.055 1 3 -2 0 0.64154 0.21430 2 3 -2 0 1.95099 0.30535 5 -3 -2 0 0.62100 0.22239 5 3 -2 0 0.53377 0.23124 3 -3 -2 0 0.87696 0.19171 4 3 2 0 0.69992 0.21752 5 -3 2 0 1.25767 0.28986 2 -3 2 0 0.72434 0.21707 3 4 -2 0 1.90347 0.36887 3 -4 -2 0 2.60135 0.32180 4 4 -2 0 1.06291 0.26811 2 -4 -2 0 1.76017 0.32022 5 4 -2 0 2.90152 0.50808 5 -4 2 0 1.60196 0.31312 5 4 2 0 2.94040 0.46310 5 -4 2 0 1.52776 0.33136 2 -4 2 0 1.24887 0.27588 3 -5 -2 0 547.143 12.8628 2 -5 -2 0 565.228 12.8313 4 5 -2 0 556.026 13.0345 2 5 -2 0 553.128 12.9965 3 -5 -2 0 550.807 13.1504 5 -5 2 0 546.627 13.2138 5 -5 2 0 550.242 13.0801 2 5 2 0 561.226 13.1966 5 6 -2 0 76.5461 2.48795 3 -6 -2 0 82.8183 2.71099 5 -6 -2 0 76.7642 2.36931 2 6 -2 0 75.8446 2.49439 2 -6 2 0 74.4603 2.53446 2 -7 -2 0 129.212 3.90228 5 7 -2 0 117.979 3.59995 3 -7 -2 0 115.591 3.45810 2 -7 2 0 128.307 3.95400 5 -7 2 0 116.425 3.66824 2 -8 -2 0 55.4969 2.10661 2 8 -2 0 59.4671 2.25220 3 -8 -2 0 58.4580 2.46854 5 -8 2 0 55.8902 2.27743 2 -8 2 0 56.1248 2.50471 5 9 -2 0 33.9403 1.72779 3 -9 -2 0 32.3956 1.57767 2 -9 -2 0 32.6941 1.92811 5 -9 2 0 33.2957 1.76591 2 -9 2 0 31.2790 1.95927 5 -10 -2 0 58.4281 2.28054 2 10 -2 0 56.0658 2.41551 3 -10 -2 0 54.9888 2.63269 5 -10 2 0 54.5245 2.45686 2 -10 2 0 47.8120 2.58873 5 -11 -2 0 66.5063 2.63091 2 -11 -2 0 64.2919 3.07345 5 11 -2 0 71.4413 2.88454 3 -11 2 0 70.4830 3.28947 5 -11 2 0 63.4921 2.81282 2 -12 -2 0 162.420 5.14524 2 -12 -2 0 177.096 5.97986 5 12 -2 0 177.449 5.52660 3 12 2 0 170.329 5.24929 3 -12 2 0 164.525 5.46583 2 13 -2 0 1.44218 0.71141 3 -13 -2 0 1.16288 0.75578 5 -13 -2 0 0.95680 0.55407 2 13 2 0 0.82980 0.60279 3 -13 2 0 1.17236 0.67658 2 14 -2 0 -0.7291 0.56385 3 -14 -2 0 1.63173 0.83639 5 -14 -2 0 1.00099 0.56430 2 14 2 0 0.22959 0.57587 3 -14 2 0 -0.3817 0.60747 2 0 -3 0 0.04058 0.12032 2 0 -3 0 -0.2147 0.15472 3 0 3 0 -0.1678 0.13625 3 0 3 0 0.09176 0.16252 2 1 -3 0 6.84353 0.49885 2 1 -3 0 7.24086 0.58851 3 -1 -3 0 6.91477 0.57425 3 1 3 0 7.00796 0.41328 4 -1 3 0 6.67109 0.53870 3 -1 3 0 6.47605 0.51330 2 1 3 0 6.39918 0.54736 3 -2 -3 0 873.304 19.9707 4 2 -3 0 913.807 20.3962 3 -2 -3 0 892.192 20.2197 5 2 3 0 890.989 19.9958 4 2 3 0 886.824 20.3779 3 -2 3 0 886.431 20.3068 3 3 -3 0 216.031 5.40250 5 3 -3 0 202.017 5.42112 3 -3 -3 0 212.413 5.35092 5 3 -3 0 210.460 5.39145 2 -3 -3 0 213.429 5.07676 4 -3 3 0 213.778 5.45802 2 3 3 0 216.076 5.06216 4 -3 3 0 219.719 5.36620 3 3 3 0 212.884 5.38447 5 3 3 0 214.086 5.45612 3 4 -3 0 282.484 7.41614 3 -4 -3 0 300.749 7.08832 4 4 -3 0 303.827 7.47943 5 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3 0 19.0579 1.54634 2 -12 -3 0 19.0900 1.78286 5 12 -3 0 19.4485 1.64176 3 -12 -3 0 19.5113 1.41865 2 -12 3 0 16.8073 1.58440 2 13 -3 0 14.3023 1.54946 3 -13 -3 0 17.6324 1.37317 2 -13 3 0 16.4284 1.60776 2 -14 -3 0 4.78654 1.23962 5 -14 -3 0 5.80789 0.98220 2 14 -3 0 6.96344 1.26133 3 14 3 0 5.73014 1.04298 3 -14 3 0 6.54905 1.26055 2 0 -4 0 86.0326 2.73775 3 0 -4 0 86.8927 2.58002 2 0 4 0 93.1846 2.49513 4 0 4 0 87.8865 2.71938 3 -1 -4 0 -0.1430 0.20935 3 1 -4 0 -0.0704 0.20343 3 1 -4 0 0.04523 0.14412 2 -1 -4 0 -0.0564 0.12457 2 -1 4 0 0.13317 0.17379 3 1 4 0 0.28806 0.20842 3 1 4 0 0.11573 0.17003 4 -1 4 0 0.16753 0.18341 2 -2 -4 0 973.876 21.8713 5 2 -4 0 955.390 22.1214 3 -2 -4 0 957.218 21.5613 4 2 4 0 960.878 22.1065 3 -2 4 0 936.011 22.0037 3 2 4 0 968.225 21.6232 4 -3 -4 0 30.2680 1.26213 5 -3 -4 0 31.0250 1.02124 4 3 -4 0 29.7219 1.29535 2 3 -4 0 29.8252 1.39659 3 3 4 0 30.1531 1.37139 3 -3 4 0 25.6108 1.35057 3 3 4 0 29.5905 1.02636 4 4 -4 0 211.547 5.60510 5 -4 -4 0 221.279 5.59307 5 4 -4 0 204.066 5.59258 2 4 -4 0 207.858 5.69656 3 -4 -4 0 219.778 5.18882 4 4 4 0 216.199 5.88120 5 -4 4 0 216.356 5.73432 2 -4 4 0 208.911 5.52240 3 4 4 0 208.820 5.67374 3 5 -4 0 208.705 5.72721 3 -5 -4 0 210.058 5.19263 4 -5 -4 0 217.909 5.65976 5 -5 4 0 201.628 5.49749 3 -5 4 0 217.915 5.78576 2 5 4 0 203.287 5.66285 5 -6 -4 0 197.748 5.03907 4 -6 -4 0 203.391 5.53225 5 6 -4 0 193.300 5.54101 3 -6 4 0 197.730 5.58950 2 -7 -4 0 303.050 7.65050 4 7 -4 0 315.706 8.23683 3 -7 -4 0 310.774 8.20597 5 -7 4 0 315.910 8.27941 2 -8 -4 0 56.9874 2.15807 2 8 -4 0 62.8244 2.55826 3 -8 -4 0 56.9927 2.48829 5 -8 -4 0 57.0149 2.05535 4 -8 4 0 55.8665 2.47503 2 -9 -4 0 137.846 4.55408 5 9 -4 0 133.495 4.43554 3 -9 -4 0 131.829 4.01751 2 -9 4 0 134.880 4.50450 2 10 -4 0 63.8391 2.81575 3 -10 -4 0 64.9009 2.92393 5 -10 -4 0 62.6290 2.43621 2 -10 4 0 61.4076 2.83598 2 -11 -4 0 15.2099 1.19675 2 -11 -4 0 15.7040 1.54679 5 11 -4 0 12.4682 1.36847 3 -11 4 0 15.3141 1.49839 2 -12 -4 0 48.1350 2.72270 5 12 -4 0 47.7091 2.59212 3 -12 -4 0 47.7142 2.20185 2 -12 4 0 46.2882 2.59996 2 -13 -4 0 3.14534 1.08774 5 13 -4 0 1.74561 0.74976 3 -13 -4 0 1.89285 0.63618 2 -13 4 0 2.84689 0.88723 2 -14 -4 0 48.3181 2.35824 2 14 -4 0 55.1223 2.97005 3 -14 -4 0 50.4858 3.06136 5 -14 4 0 52.9279 2.97483 2 0 -5 0 -0.2978 0.25727 3 0 -5 0 0.06356 0.16455 2 0 5 0 -0.0906 0.22554 3 0 5 0 0.00250 0.19857 4 -1 -5 0 3.07641 0.43105 2 1 -5 0 5.32511 0.65742 2 1 -5 0 3.25546 0.57492 3 -1 -5 0 3.44462 0.57688 3 1 5 0 3.89901 0.47451 4 1 5 0 3.07497 0.50763 3 -1 5 0 2.97098 0.47964 2 -1 5 0 3.87933 0.57750 3 2 -5 0 376.214 9.35807 2 -2 -5 0 374.402 9.29290 2 2 -5 0 388.654 9.60585 3 -2 -5 0 385.402 9.25512 5 2 5 0 384.558 9.01248 4 -2 5 0 382.083 9.47726 3 -2 5 0 387.685 9.48871 2 2 5 0 373.359 9.53823 3 3 -5 0 329.834 8.41100 5 -3 -5 0 342.532 8.01920 4 3 -5 0 336.902 8.73024 3 -3 -5 0 342.361 8.42560 5 -3 5 0 341.013 8.57000 3 3 5 0 343.047 8.08334 4 -3 5 0 352.787 8.71515 2 3 5 0 343.615 9.07105 3 -4 -5 0 264.752 6.39510 4 4 -5 0 265.232 7.12691 3 -4 -5 0 269.105 6.87267 5 4 5 0 264.072 6.41706 4 -4 5 0 273.626 7.12251 2 5 -5 0 86.6725 3.08196 3 -5 -5 0 90.0104 2.92589 5 -5 -5 0 84.7338 2.43754 4 -5 5 0 87.6223 3.06859 2 6 -5 0 10.8853 1.11438 3 -6 -5 0 10.7358 0.98102 5 -6 -5 0 11.0465 0.69118 4 -6 5 0 10.3857 1.03655 2 7 -5 0 275.547 7.77286 3 -7 -5 0 276.397 7.00444 4 -7 -5 0 295.266 7.71784 5 -7 5 0 289.395 7.86925 2 8 -5 0 2.81534 0.79427 3 -8 -5 0 1.42785 0.53715 5 -8 5 0 3.23156 0.78910 2 -9 -5 0 0.50047 0.50132 5 -9 -5 0 0.30932 0.33056 4 -9 -5 0 0.21946 0.37805 2 -9 5 0 -0.1043 0.49677 2 -10 -5 0 23.9516 1.43592 2 10 -5 0 26.7366 1.85501 3 -10 -5 0 26.4688 1.84143 5 -10 5 0 27.3010 1.92958 2 -11 -5 0 8.63300 0.99744 2 -11 -5 0 8.82569 1.29710 5 11 -5 0 7.69219 1.26476 3 -11 5 0 7.44010 1.24475 2 -12 -5 0 3.92058 0.81687 2 -12 -5 0 3.04956 0.86227 5 12 -5 0 3.37745 0.94240 3 -12 5 0 5.26198 1.05742 2 -13 -5 0 5.07087 1.04008 5 -13 -5 0 5.71137 0.90768 2 13 -5 0 6.84765 1.29697 3 -13 5 0 4.32350 1.16885 2 -14 -5 0 20.2998 1.97628 5 -14 -5 0 14.8171 1.37269 2 14 -5 0 17.1057 2.19334 3 -14 5 0 14.0011 1.77920 2 0 -6 0 237.196 6.63601 3 0 6 0 246.784 6.21224 4 -1 -6 0 562.461 13.6638 3 1 -6 0 560.958 13.7029 3 -1 6 0 553.832 13.5263 2 1 6 0 549.740 13.0754 4 -2 -6 0 363.511 9.58170 2 -2 -6 0 398.422 9.56147 5 2 -6 0 396.565 9.99658 3 -2 6 0 387.421 9.83979 2 2 6 0 394.396 9.56527 4 3 -6 0 79.6383 2.89457 3 -3 -6 0 65.4984 2.67645 2 -3 -6 0 76.8605 2.54862 5 3 6 0 74.6196 2.24427 4 -4 -6 0 0.27689 0.20593 4 -4 -6 0 0.29620 0.34054 5 4 -6 0 0.34042 0.44518 3 -4 6 0 0.65760 0.42228 2 4 6 0 0.46521 0.23360 4 -5 -6 0 226.637 6.08600 5 5 -6 0 221.778 6.40486 3 -5 -6 0 216.933 5.43974 4 -5 6 0 221.903 6.36662 2 6 -6 0 260.839 7.27727 3 -6 -6 0 245.072 6.22759 4 -6 -6 0 258.704 6.95515 5 -6 6 0 258.897 7.25613 2 -7 -6 0 303.546 8.08565 5 7 -6 0 304.562 8.37664 3 -7 -6 0 287.928 7.26731 4 -7 6 0 303.181 8.37129 2 -8 -6 0 126.583 4.32593 5 8 -6 0 130.547 5.18043 3 -8 -6 0 126.772 3.56058 4 -8 6 0 134.448 4.59407 2 -9 -6 0 14.3215 1.12913 2 -9 -6 0 15.0346 1.37916 5 9 -6 0 15.3004 1.50557 3 -9 6 0 15.5692 1.48736 2 -10 -6 0 0.76909 0.58516 5 -10 -6 0 0.13282 0.55352 4 -10 -6 0 0.54894 0.41472 2 10 -6 0 0.74014 0.65053 3 -10 6 0 0.82698 0.61714 2 -11 -6 0 7.15368 0.98096 2 11 -6 0 9.25806 1.36839 3 -11 -6 0 8.73648 1.25253 5 -11 6 0 9.76414 1.44428 2 12 -6 0 3.25858 1.02247 3 -12 -6 0 4.50549 0.83963 2 -12 -6 0 3.83102 0.99511 5 -12 6 0 4.50882 1.06873 2 -13 -6 0 5.00864 0.88288 2 13 -6 0 5.54317 1.25497 3 -13 -6 0 5.36580 1.21634 5 -13 6 0 5.85268 1.30266 2 0 -7 0 -0.1103 0.36450 3 0 7 0 -0.1195 0.30662 4 1 -7 0 128.473 4.23025 3 -1 -7 0 124.869 4.15902 3 1 7 0 120.789 3.62667 4 -1 7 0 127.245 3.80771 4 -2 -7 0 83.2108 2.82379 5 2 -7 0 82.8936 3.18864 3 -2 7 0 81.2836 3.06612 2 2 7 0 82.9907 2.61424 4 -3 -7 0 268.429 7.18444 5 3 -7 0 280.590 7.73591 3 3 7 0 273.332 6.84994 4 -3 7 0 277.907 7.61291 2 4 -7 0 11.0788 1.38840 3 -4 -7 0 9.33576 0.96037 5 -4 7 0 10.1136 1.22723 2 4 7 0 9.06421 0.69112 4 -5 -7 0 255.880 6.74498 5 5 -7 0 251.984 7.20424 3 -5 7 0 223.529 8.41696 2 -6 -7 0 -0.0332 0.23102 4 -6 -7 0 0.39459 0.43663 5 6 -7 0 0.30774 0.59235 3 -6 7 0 0.06163 0.49434 2 -7 -7 0 24.3491 1.53171 5 -7 -7 0 15.6548 0.82440 4 -7 7 0 23.1440 1.73743 2 8 -7 0 14.5659 1.52583 3 -8 -7 0 16.0535 0.82194 4 -8 -7 0 16.4290 1.38367 5 -8 7 0 17.0501 1.57099 2 9 -7 0 21.6874 1.84676 3 -9 -7 0 25.1229 1.74691 5 -9 -7 0 21.6826 1.02693 4 -9 7 0 25.0071 1.93594 2 -10 -7 0 57.9692 2.47840 2 10 -7 0 60.0937 3.08112 3 -10 -7 0 58.5790 2.84282 5 -10 7 0 56.2354 3.03980 2 -11 -7 0 17.6127 1.71077 5 11 -7 0 20.3275 1.87957 3 -11 -7 0 17.3029 1.34923 2 -11 7 0 18.6971 1.87636 2 -12 -7 0 2.63280 0.86375 5 -12 -7 0 1.50273 0.57522 2 12 -7 0 2.70934 1.03566 3 -12 7 0 3.02143 0.93545 2 13 -7 0 10.9314 1.73340 3 -13 -7 0 6.54510 1.03840 2 -13 -7 0 9.36658 1.43484 5 -13 7 0 8.57608 1.51954 2 0 -8 0 273.978 7.80413 3 0 8 0 271.794 7.19856 4 1 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18.1796 1.80368 5 -12 -8 0 15.9914 1.40037 2 -12 8 0 17.5680 1.96382 2 0 -9 0 -0.2432 0.49589 3 0 9 0 1.86573 0.59407 4 1 -9 0 120.723 4.46282 3 -1 -9 0 118.095 4.41880 3 -1 9 0 118.115 3.95458 4 1 9 0 119.840 3.79865 4 -2 -9 0 5.26400 0.87680 5 2 -9 0 4.40485 1.00853 3 2 9 0 3.96715 0.68358 4 -2 9 0 3.73618 0.82605 4 3 -9 0 93.2358 3.85220 3 -3 -9 0 92.6300 3.28817 5 3 9 0 92.5885 2.99762 4 -3 9 0 88.4762 3.86494 4 4 -9 0 29.2634 2.10541 3 -4 -9 0 31.1585 1.76273 5 4 9 0 30.0187 1.41777 4 -4 9 0 31.1597 2.08876 2 -5 -9 0 107.138 3.71557 5 5 -9 0 112.780 4.40034 3 5 9 0 106.413 3.11650 4 -5 9 0 104.471 4.20787 2 6 -9 0 84.6556 3.78233 3 -6 -9 0 85.6227 3.24625 5 -6 9 0 76.6969 3.59236 2 7 -9 0 62.2449 3.23348 3 -7 -9 0 58.7934 2.68321 5 -7 9 0 59.6150 3.14071 2 -8 -9 0 344.318 9.54598 5 8 -9 0 355.906 10.3232 3 -8 9 0 347.883 10.2890 2 -9 -9 0 8.13810 1.23409 5 9 -9 0 7.78139 1.43496 3 -9 9 0 8.08983 1.39546 2 -10 -9 0 2.07867 0.76727 5 10 -9 0 3.54253 1.11912 3 -10 9 0 3.87176 1.03234 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21 3.51525 1.19590 4 5 -5 -21 65.4257 3.83239 5 5 -5 -21 70.7274 3.66389 3 -5 5 21 71.4752 3.98197 4 4 -5 -21 5.65841 1.37504 5 4 -5 -21 7.01830 1.35984 3 -4 5 21 7.93099 1.62416 4 3 -5 -21 10.5969 1.52650 3 3 -5 -21 4.89886 1.33635 5 -3 5 21 5.85116 1.39636 4 3 5 -21 5.41024 0.84245 2 2 -5 -21 20.7390 1.72117 3 2 -5 -21 18.3961 2.12052 5 2 5 -21 18.5543 1.44148 2 -2 5 21 17.8437 2.24961 4 1 -5 -21 22.5297 2.25991 5 1 -5 -21 21.3448 1.56953 3 -1 5 21 17.9424 2.19718 4 1 5 -21 21.1884 1.66639 2 0 -5 -21 41.2312 3.03711 5 0 5 -21 46.0844 2.61437 2 0 5 21 47.2713 3.19340 4 -1 -5 -21 4.24166 1.14435 2 -1 -5 -21 3.65551 1.11330 5 1 5 21 3.64938 1.29667 4 -1 5 -21 6.25448 1.20202 2 -2 -5 -21 18.7214 2.05320 2 -2 5 -21 19.7497 1.94700 2 5 -6 -21 87.8654 4.62031 5 5 -6 -21 95.6359 4.42641 3 -5 6 21 95.0902 4.72667 4 4 -6 -21 0.74787 1.02236 5 4 -6 -21 -0.2194 0.72836 3 -4 6 21 -0.5258 0.84622 4 3 -6 -21 2.59145 1.21485 5 3 -6 -21 3.25142 0.99372 3 3 6 -21 1.46972 0.57535 2 -3 6 21 1.49124 1.10308 4 2 -6 -21 2.17502 0.93121 3 2 -6 -21 2.37529 1.15196 5 2 6 -21 1.99972 0.75076 2 -2 6 21 2.38368 1.22959 4 1 -6 -21 1.30710 0.87611 5 1 -6 -21 0.12253 0.61384 3 1 6 -21 0.60952 0.59596 2 -1 6 21 0.58344 0.99765 4 0 -6 -21 10.9062 1.89542 5 0 6 21 11.6738 1.90670 4 7 0 -22 1.04486 0.75020 3 7 0 -22 -1.6736 0.67738 5 6 0 -22 58.2462 3.59293 3 6 0 -22 66.4300 3.04011 5 5 0 -22 -0.0434 0.58507 5 5 0 -22 0.96664 0.52859 2 5 0 -22 -0.1231 0.56118 3 -5 0 22 2.77468 1.63227 4 4 0 -22 165.378 5.54603 5 4 0 -22 166.517 5.52246 3 4 0 -22 165.469 5.16590 2 -4 0 22 175.324 6.70162 4 3 0 -22 -0.2947 0.50653 3 3 0 -22 0.18556 0.51553 2 3 0 -22 -0.9053 0.47923 5 2 0 -22 57.3449 2.75325 2 2 0 -22 50.5867 2.32218 3 2 0 -22 48.8245 2.70068 5 1 0 -22 -1.0047 0.51709 5 1 0 -22 -0.8410 0.55325 2 1 0 -22 -0.5239 0.34760 3 0 0 -22 9.63252 1.37729 5 -1 0 -22 -0.0057 0.60854 5 -1 0 -22 -0.3529 0.64923 2 -2 0 -22 15.5882 1.90836 2 -7 -1 22 37.9205 2.32608 4 7 -1 -22 35.1237 2.46414 5 7 -1 -22 34.7908 2.48140 3 7 1 -22 35.6436 2.42625 3 -7 1 22 37.7453 2.60944 4 7 1 -22 34.3295 2.11522 5 6 -1 -22 12.1277 1.71885 3 6 -1 -22 11.3812 1.59508 5 -6 1 22 11.0351 1.60034 4 6 1 -22 8.73505 1.10842 5 6 1 -22 12.5318 1.76390 3 5 -1 -22 18.3346 1.68752 3 5 -1 -22 18.9006 1.36854 2 5 -1 -22 16.2126 1.71485 5 5 1 -22 14.0544 1.38203 5 5 1 -22 15.8617 1.57425 3 5 1 -22 12.0072 1.07929 2 -5 1 22 21.4929 1.97220 4 4 -1 -22 6.36444 1.19749 5 4 -1 -22 8.54496 1.23775 3 4 -1 -22 7.28670 1.04439 2 4 1 -22 7.63732 1.11950 3 -4 1 22 8.26881 1.48249 4 4 1 -22 7.28177 0.94702 2 4 1 -22 6.38272 1.00779 5 3 -1 -22 -0.3518 0.55139 3 3 -1 -22 -0.1696 0.63290 5 3 -1 -22 -0.3042 0.51099 2 3 1 -22 -0.8357 0.47659 5 3 1 -22 -0.2643 0.51972 3 -3 1 22 0.84029 0.79756 4 3 1 -22 -0.3839 0.45843 2 2 -1 -22 231.171 6.83804 3 2 -1 -22 250.915 7.41170 2 2 -1 -22 239.785 7.56584 5 2 1 -22 246.470 7.23958 2 2 1 -22 249.209 7.13364 5 2 1 -22 232.363 6.74123 3 1 -1 -22 8.94834 1.01990 3 1 -1 -22 7.67423 1.24978 2 1 -1 -22 7.83046 1.39490 5 1 1 -22 7.40053 1.23873 2 1 1 -22 8.41370 1.26423 5 1 1 -22 9.52997 1.13441 3 0 -1 -22 0.58032 0.66622 2 0 -1 -22 0.90420 0.80446 5 0 1 -22 1.52827 0.87218 2 0 1 -22 0.10813 0.62649 5 -1 -1 -22 29.7416 2.28145 2 -1 1 -22 30.3622 2.08860 5 -1 1 -22 30.4505 2.25008 2 -2 -1 -22 50.7572 3.07003 2 -2 -1 -22 53.7986 3.11113 5 -2 1 -22 50.9064 3.03177 2 -2 1 -22 51.7142 2.80435 5 7 -2 -22 6.07262 1.31392 3 -7 2 22 4.92715 1.29197 4 7 2 -22 4.18321 1.14992 3 6 -2 -22 5.12628 1.20341 5 6 -2 -22 6.94851 0.93036 2 6 -2 -22 6.55729 1.29967 3 -6 2 22 5.07111 1.19399 4 6 2 -22 6.81544 1.31223 3 5 -2 -22 57.8482 2.60525 2 5 -2 -22 60.7921 3.25743 5 5 -2 -22 63.5643 3.15248 3 5 2 -22 55.9626 2.84409 3 -5 2 22 53.4180 3.25222 4 4 -2 -22 7.81651 1.16505 2 4 -2 -22 5.54189 1.11724 3 4 -2 -22 5.66027 1.22748 5 4 2 -22 4.80540 0.78573 2 -4 2 22 8.00543 1.40941 4 4 2 -22 6.08716 1.01049 3 4 2 -22 5.17609 0.84381 5 3 -2 -22 165.568 5.42966 2 3 -2 -22 154.249 5.22029 3 3 -2 -22 157.424 5.76928 5 -3 2 22 155.586 6.01173 4 3 2 -22 156.012 4.87764 5 3 2 -22 159.334 5.01451 2 3 2 -22 152.821 5.00099 3 2 -2 -22 90.9072 4.12573 5 2 -2 -22 87.7091 3.42365 3 2 -2 -22 87.1347 3.80064 2 -2 2 22 96.1536 4.42073 4 2 2 -22 90.8712 3.24997 3 2 2 -22 87.7096 3.26533 5 2 2 -22 94.9008 3.64229 2 1 -2 -22 8.06067 1.43029 5 1 -2 -22 7.51443 0.84984 3 -1 2 22 4.23039 1.21318 4 1 2 -22 10.3339 1.41408 3 1 2 -22 7.61591 1.17014 2 1 2 -22 8.09273 1.04778 5 0 -2 -22 5.44480 1.14488 2 0 -2 -22 5.47754 1.44597 5 0 2 -22 5.63504 1.00646 5 0 2 -22 6.29982 1.16868 2 -1 -2 -22 2.25120 0.97992 5 -1 -2 -22 2.94555 1.09350 2 -1 2 -22 4.53044 1.07391 2 -1 2 -22 2.82627 0.80589 5 -2 -2 -22 47.6006 3.05300 5 -2 -2 -22 51.4048 3.10793 2 -2 2 -22 52.0568 3.01234 2 -2 2 -22 48.6663 2.58159 5 6 -3 -22 1.68434 0.93681 5 6 -3 -22 0.99185 0.92164 3 -6 3 22 1.61727 0.96914 4 6 3 -22 -0.1377 0.65896 3 5 -3 -22 1.41585 0.70483 2 5 -3 -22 2.24999 0.99962 3 5 -3 -22 4.72470 1.21656 5 5 3 -22 2.51219 0.86238 3 -5 3 22 2.74159 0.98056 4 4 -3 -22 117.848 5.23891 5 4 -3 -22 114.627 4.33132 2 4 -3 -22 115.938 4.55012 3 -4 3 22 115.131 5.08329 4 4 3 -22 117.398 4.25864 3 3 -3 -22 224.900 7.03409 2 3 -3 -22 226.809 7.76247 5 3 -3 -22 224.044 6.97454 3 -3 3 22 230.319 7.87340 4 3 3 -22 224.513 6.60034 3 3 3 -22 218.754 6.44918 2 2 -3 -22 0.92634 0.60527 3 2 -3 -22 0.20502 1.09937 2 2 -3 -22 -0.5308 0.81205 5 -2 3 22 0.51047 0.89199 4 2 3 -22 -0.0469 0.44714 3 2 3 -22 0.54323 0.56954 2 1 -3 -22 36.1790 2.69049 5 1 -3 -22 42.5373 2.57915 2 1 3 -22 37.7302 2.32164 2 -1 3 22 40.9040 2.89240 4 0 -3 -22 141.188 5.32181 2 0 -3 -22 133.606 5.46239 5 0 3 -22 125.269 4.27094 5 0 3 -22 145.471 5.61302 2 -1 -3 -22 17.8722 1.96494 2 -1 -3 -22 14.9595 1.97451 5 -1 3 -22 17.5351 1.43172 5 -1 3 -22 16.6932 1.82080 2 5 -4 -22 -1.1543 0.71245 5 5 -4 -22 0.87768 0.65767 2 5 -4 -22 0.63272 0.75034 3 5 4 -22 0.00098 0.69233 3 -5 4 22 3.29821 1.11774 4 4 -4 -22 116.603 5.15080 5 4 -4 -22 123.927 4.62022 2 4 -4 -22 119.430 4.76320 3 -4 4 22 122.201 5.29777 4 4 4 -22 119.684 4.36389 3 3 -4 -22 41.3125 2.45639 3 3 -4 -22 42.1247 3.30498 2 3 -4 -22 34.2757 2.74974 5 3 4 -22 39.4074 2.00757 2 -3 4 22 44.8945 3.10598 4 3 4 -22 37.4405 2.11328 3 2 -4 -22 17.2113 2.06333 5 2 -4 -22 14.8583 1.44792 3 2 -4 -22 15.3773 1.73572 2 -2 4 22 19.3075 2.16561 4 2 4 -22 17.0233 1.50323 2 2 4 -22 16.6881 1.31186 3 1 -4 -22 53.0897 3.32306 5 1 -4 -22 53.9475 3.02881 2 1 -4 -22 57.4897 2.88393 3 -1 4 22 52.9303 3.40790 4 1 4 -22 53.8512 2.73849 2 0 -4 -22 30.4459 2.40741 2 0 -4 -22 29.5528 2.57801 5 0 4 22 30.9959 2.60799 4 3 -5 -22 7.68446 1.57384 5 3 -5 -22 7.32356 1.30817 3 -3 5 22 6.03076 1.51550 4 3 5 -22 6.25796 1.13063 2 2 -5 -22 -0.5519 0.52312 3 2 -5 -22 0.69319 0.85247 5 2 5 -22 0.10922 0.54421 3 2 5 -22 -0.5065 0.47497 2 -2 5 22 -1.2368 0.87411 4 5 0 -23 1.86268 0.91968 3 -5 0 23 0.38716 0.78982 4 5 0 -23 -0.0632 0.62809 5 4 0 -23 0.09681 0.62529 3 4 0 -23 -0.0588 0.56580 5 3 0 -23 24.5672 1.72491 3 3 0 -23 24.4583 1.92733 5 3 0 -23 24.7044 1.75399 2 2 0 -23 0.29901 0.63649 2 2 0 -23 0.67093 0.49118 3 2 0 -23 0.00548 0.66765 5 1 0 -23 0.30488 0.72072 2 1 0 -23 -0.0349 0.69255 5 0 0 -23 5.87821 1.18396 2 0 0 -23 3.96465 1.05628 5 5 -1 -23 44.5692 2.68309 5 5 -1 -23 41.3269 2.10030 2 5 1 -23 43.1564 3.04560 3 -5 1 23 49.3800 2.98946 4 4 -1 -23 20.6718 1.87307 5 4 -1 -23 17.3230 1.63544 3 4 -1 -23 16.5198 1.49050 2 -4 1 23 16.8252 2.07359 4 4 1 -23 16.1048 1.54423 3 4 1 -23 13.5593 1.25764 2 4 1 -23 13.7066 1.37942 5 3 -1 -23 18.6451 1.85589 5 3 -1 -23 19.2588 1.54929 3 3 -1 -23 18.7907 1.66916 2 3 1 -23 15.4087 1.48117 5 -3 1 23 18.2837 1.99643 4 3 1 -23 18.5105 1.52187 2 3 1 -23 17.5525 1.44956 3 2 -1 -23 1.93422 0.79020 5 2 -1 -23 2.67552 0.63939 3 2 -1 -23 1.09100 0.76228 2 2 1 -23 1.49703 0.61543 3 2 1 -23 1.94404 0.77012 2 2 1 -23 0.97239 0.70390 5 1 -1 -23 -1.0184 0.63157 5 1 -1 -23 -0.4296 0.66299 2 1 1 -23 -1.0045 0.56032 5 0 -1 -23 11.6039 1.63178 5 0 -1 -23 11.1192 1.59193 2 0 1 -23 7.94855 1.28492 2 0 1 -23 8.75220 1.24631 5 4 -2 -23 1.60042 0.73366 3 4 -2 -23 1.35625 0.67769 2 4 -2 -23 0.47870 0.94071 5 4 2 -23 0.71982 0.65659 3 -4 2 23 3.86907 1.11331 4 3 -2 -23 33.4931 2.09756 3 3 -2 -23 34.0265 2.19236 2 3 -2 -23 31.1216 2.70655 5 3 2 -23 28.0609 1.82577 3 3 2 -23 34.7447 1.97628 2 -3 2 23 34.7142 2.65955 4 2 -2 -23 97.5982 4.30734 5 2 -2 -23 108.714 4.25542 2 2 -2 -23 92.1050 3.76765 3 -2 2 23 101.560 4.63693 4 2 2 -23 95.0896 3.81779 2 1 -2 -23 1.74233 0.83477 2 1 -2 -23 1.08144 0.94490 5 1 2 -23 -0.0009 0.50796 5 1 2 -23 0.02787 0.61377 2 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9206 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71076 10.039 9.786 15.474 90.020 99.869 90.006 ) ; _shelx_hkl_checksum 87131 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.08139(6) 0.77292(6) 0.41703(4) 0.02151(13) Uani 1 1 d . . . . O2A O 0.3486(5) 0.3978(4) 0.5698(3) 0.0323(5) Uani 0.733(2) 1 d . P A 1 O2B O 0.3654(12) 0.4236(11) 0.5593(8) 0.0355(16) Uani 0.267(2) 1 d . P A 2 N1 N 0.54534(6) 0.92553(7) 0.39869(4) 0.01700(13) Uani 1 1 d . . . . N2 N 0.70206(7) 0.85461(8) 0.30806(5) 0.01966(14) Uani 1 1 d . . . . N3A N 0.19895(17) 0.5756(2) 0.44576(14) 0.0180(3) Uani 0.733(2) 1 d . P A 1 N3B N 0.1580(5) 0.5583(7) 0.4416(4) 0.0226(9) Uani 0.267(2) 1 d . P A 2 C1 C 0.58005(7) 0.85395(7) 0.33217(5) 0.01437(13) Uani 1 1 d . . . . C2 C 0.64240(7) 1.00250(8) 0.44534(5) 0.01771(14) Uani 1 1 d . . . . H2 H 0.621063 1.055200 0.492697 0.021 Uiso 1 1 calc R . . . C3 C 0.77261(7) 1.00818(8) 0.42717(5) 0.01753(14) Uani 1 1 d . . . . H3 H 0.841101 1.062042 0.461107 0.021 Uiso 1 1 calc R . . . C4 C 0.79709(8) 0.93072(9) 0.35661(5) 0.02036(15) Uani 1 1 d . . . . H4 H 0.885264 0.931778 0.342142 0.024 Uiso 1 1 calc R . . . C5 C 0.47438(7) 0.76681(7) 0.28056(5) 0.01469(13) Uani 1 1 d . . . . C6 C 0.35061(7) 0.74722(7) 0.30854(4) 0.01415(13) Uani 1 1 d . . . . H6 H 0.333889 0.792048 0.360078 0.017 Uiso 1 1 calc R . . . C7 C 0.25136(7) 0.66308(7) 0.26214(4) 0.01403(13) Uani 1 1 d . . . . C8 C 0.27666(8) 0.59887(8) 0.18597(5) 0.01759(14) Uani 1 1 d . . . . H8 H 0.209625 0.541844 0.153357 0.021 Uiso 1 1 calc R . . . C9 C 0.39947(8) 0.61797(9) 0.15763(5) 0.02041(15) Uani 1 1 d . . . . H9 H 0.415756 0.573889 0.105742 0.024 Uiso 1 1 calc R . . . C10 C 0.49865(8) 0.70115(9) 0.20471(5) 0.01945(15) Uani 1 1 d . . . . H10 H 0.582617 0.713219 0.185287 0.023 Uiso 1 1 calc R . . . C11 C 0.11543(7) 0.64269(8) 0.29089(5) 0.01550(13) Uani 1 1 d . . . . H11 H 0.086762 0.545724 0.278627 0.019 Uiso 1 1 calc R . . . C12 C 0.00907(8) 0.73589(9) 0.23835(5) 0.02102(15) Uani 1 1 d . . . . H12A H 0.034537 0.831607 0.250355 0.032 Uiso 1 1 calc GR . . . H12B H -0.078954 0.718461 0.255408 0.032 Uiso 1 1 calc GR . . . H12C H 0.003406 0.717380 0.175576 0.032 Uiso 1 1 calc GR . . . C13 C 0.12661(8) 0.66810(8) 0.38941(5) 0.01732(14) Uani 1 1 d . . . . C14A C 0.28473(15) 0.46785(12) 0.41841(7) 0.0217(2) Uani 0.733(2) 1 d . P A 1 H14A H 0.375136 0.505561 0.414952 0.026 Uiso 0.733(2) 1 calc R P A 1 H14B H 0.244114 0.433856 0.359505 0.026 Uiso 0.733(2) 1 calc R P A 1 C14B C 0.2155(5) 0.4286(4) 0.4181(2) 0.0267(8) Uani 0.267(2) 1 d . P A 2 H14C H 0.213851 0.425525 0.353961 0.032 Uiso 0.267(2) 1 calc R P A 2 H14D H 0.160394 0.351701 0.433966 0.032 Uiso 0.267(2) 1 calc R P A 2 C15A C 0.29855(16) 0.35115(13) 0.48372(8) 0.0291(3) Uani 0.733(2) 1 d . P A 1 H15A H 0.209268 0.307547 0.482406 0.035 Uiso 0.733(2) 1 calc R P A 1 H15B H 0.360838 0.281510 0.466820 0.035 Uiso 0.733(2) 1 calc R P A 1 C15B C 0.3585(4) 0.4142(4) 0.4654(2) 0.0304(8) Uani 0.267(2) 1 d . P A 2 H15C H 0.395033 0.324771 0.450658 0.037 Uiso 0.267(2) 1 calc R P A 2 H15D H 0.414947 0.486889 0.445703 0.037 Uiso 0.267(2) 1 calc R P A 2 C16A C 0.25280(17) 0.48892(15) 0.59635(8) 0.0307(3) Uani 0.733(2) 1 d . P A 1 H16A H 0.284272 0.517108 0.657921 0.037 Uiso 0.733(2) 1 calc R P A 1 H16B H 0.165107 0.441392 0.593413 0.037 Uiso 0.733(2) 1 calc R P A 1 C16B C 0.3130(5) 0.5510(4) 0.5811(2) 0.0324(9) Uani 0.267(2) 1 d . P A 2 H16C H 0.368530 0.625659 0.562724 0.039 Uiso 0.267(2) 1 calc R P A 2 H16D H 0.318980 0.556746 0.645552 0.039 Uiso 0.267(2) 1 calc R P A 2 C17A C 0.23376(17) 0.61439(14) 0.53821(7) 0.0250(3) Uani 0.733(2) 1 d . P A 1 H17A H 0.160879 0.671983 0.554494 0.030 Uiso 0.733(2) 1 calc R P A 1 H17B H 0.318136 0.668786 0.547310 0.030 Uiso 0.733(2) 1 calc R P A 1 C17B C 0.1683(5) 0.5698(5) 0.5377(2) 0.0300(8) Uani 0.267(2) 1 d . P A 2 H17C H 0.111039 0.499336 0.558993 0.036 Uiso 0.267(2) 1 calc R P A 2 H17D H 0.135702 0.660781 0.552825 0.036 Uiso 0.267(2) 1 calc R P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0231(3) 0.0213(3) 0.0199(3) -0.0048(2) 0.0031(2) 0.0026(2) O2A 0.0499(14) 0.0248(10) 0.0197(8) 0.0047(6) -0.0009(7) 0.0046(8) O2B 0.038(3) 0.039(5) 0.025(3) 0.002(2) -0.008(2) 0.006(3) N1 0.0148(3) 0.0205(3) 0.0158(3) -0.0054(2) 0.0029(2) -0.0004(2) N2 0.0156(3) 0.0238(3) 0.0207(3) -0.0059(2) 0.0063(2) -0.0020(2) N3A 0.0254(8) 0.0151(6) 0.0130(5) -0.0002(4) 0.0020(6) 0.0011(6) N3B 0.029(2) 0.024(2) 0.0135(13) -0.0045(12) 0.0008(19) 0.0013(19) C1 0.0134(3) 0.0161(3) 0.0134(3) -0.0016(2) 0.0019(2) 0.0010(2) C2 0.0166(3) 0.0211(3) 0.0153(3) -0.0044(2) 0.0025(2) -0.0013(3) C3 0.0151(3) 0.0203(3) 0.0166(3) -0.0017(2) 0.0011(2) -0.0018(2) C4 0.0151(3) 0.0240(4) 0.0228(3) -0.0048(3) 0.0057(3) -0.0021(3) C5 0.0142(3) 0.0156(3) 0.0139(3) -0.0025(2) 0.0013(2) 0.0012(2) C6 0.0151(3) 0.0141(3) 0.0129(3) -0.0020(2) 0.0014(2) 0.0008(2) C7 0.0151(3) 0.0130(3) 0.0134(3) -0.0009(2) 0.0006(2) 0.0012(2) C8 0.0191(3) 0.0168(3) 0.0159(3) -0.0048(2) 0.0003(2) 0.0005(2) C9 0.0205(3) 0.0239(4) 0.0169(3) -0.0085(3) 0.0033(3) 0.0013(3) C10 0.0173(3) 0.0239(4) 0.0174(3) -0.0066(3) 0.0037(2) 0.0013(3) C11 0.0168(3) 0.0151(3) 0.0142(3) -0.0024(2) 0.0016(2) -0.0022(2) C12 0.0163(3) 0.0272(4) 0.0185(3) -0.0016(3) -0.0001(2) 0.0027(3) C13 0.0200(3) 0.0163(3) 0.0156(3) -0.0011(2) 0.0030(2) -0.0016(2) C14A 0.0321(6) 0.0155(5) 0.0173(4) 0.0020(4) 0.0037(4) 0.0045(5) C14B 0.039(2) 0.0185(14) 0.0210(14) -0.0036(11) 0.0007(13) -0.0005(14) C15A 0.0481(8) 0.0171(5) 0.0206(5) 0.0038(4) 0.0012(5) 0.0030(5) C15B 0.044(2) 0.0253(16) 0.0215(14) 0.0037(12) 0.0033(14) 0.0045(15) C16A 0.0480(8) 0.0283(6) 0.0156(5) 0.0049(4) 0.0052(5) 0.0009(6) C16B 0.048(2) 0.0325(19) 0.0160(13) -0.0009(12) 0.0035(13) -0.0078(17) C17A 0.0393(7) 0.0212(5) 0.0136(4) -0.0012(4) 0.0018(4) 0.0000(5) C17B 0.044(2) 0.0321(18) 0.0160(13) -0.0020(12) 0.0100(14) -0.0026(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C15A O2A C16A 109.0(3) C16B O2B C15B 109.9(6) C1 N1 C2 116.51(6) C4 N2 C1 116.43(7) C13 N3A C14A 124.20(17) C13 N3A C17A 117.43(16) C17A N3A C14A 114.48(15) C13 N3B C14B 127.1(5) C13 N3B C17B 120.7(5) C14B N3B C17B 110.7(5) N1 C1 N2 125.59(7) N1 C1 C5 117.24(6) N2 C1 C5 117.17(6) N1 C2 H2 118.7 N1 C2 C3 122.54(7) C3 C2 H2 118.7 C2 C3 H3 122.0 C2 C3 C4 116.08(7) C4 C3 H3 122.0 N2 C4 C3 122.82(7) N2 C4 H4 118.6 C3 C4 H4 118.6 C6 C5 C1 120.28(6) C10 C5 C1 120.35(7) C10 C5 C6 119.36(7) C5 C6 H6 119.4 C7 C6 C5 121.13(6) C7 C6 H6 119.4 C6 C7 C8 118.87(7) C6 C7 C11 121.72(6) C8 C7 C11 119.39(6) C7 C8 H8 119.8 C9 C8 C7 120.35(7) C9 C8 H8 119.8 C8 C9 H9 119.8 C8 C9 C10 120.49(7) C10 C9 H9 119.8 C5 C10 H10 120.1 C9 C10 C5 119.79(7) C9 C10 H10 120.1 C7 C11 H11 108.2 C7 C11 C12 110.30(6) C7 C11 C13 110.77(6) C12 C11 H11 108.2 C12 C11 C13 110.99(6) C13 C11 H11 108.2 C11 C12 H12A 109.5 C11 C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12B 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 O1 C13 N3A 121.07(11) O1 C13 N3B 121.3(3) O1 C13 C11 120.96(7) N3A C13 C11 117.73(11) N3B C13 C11 115.9(3) N3A C14A H14A 109.7 N3A C14A H14B 109.7 N3A C14A C15A 109.85(13) H14A C14A H14B 108.2 C15A C14A H14A 109.7 C15A C14A H14B 109.7 N3B C14B H14C 109.6 N3B C14B H14D 109.6 N3B C14B C15B 110.2(3) H14C C14B H14D 108.1 C15B C14B H14C 109.6 C15B C14B H14D 109.6 O2A C15A C14A 111.18(16) O2A C15A H15A 109.4 O2A C15A H15B 109.4 C14A C15A H15A 109.4 C14A C15A H15B 109.4 H15A C15A H15B 108.0 O2B C15B C14B 111.1(6) O2B C15B H15C 109.4 O2B C15B H15D 109.4 C14B C15B H15C 109.4 C14B C15B H15D 109.4 H15C C15B H15D 108.0 O2A C16A H16A 109.4 O2A C16A H16B 109.4 O2A C16A C17A 111.01(15) H16A C16A H16B 108.0 C17A C16A H16A 109.4 C17A C16A H16B 109.4 O2B C16B H16C 109.3 O2B C16B H16D 109.3 O2B C16B C17B 111.8(6) H16C C16B H16D 107.9 C17B C16B H16C 109.3 C17B C16B H16D 109.3 N3A C17A C16A 110.80(13) N3A C17A H17A 109.5 N3A C17A H17B 109.5 C16A C17A H17A 109.5 C16A C17A H17B 109.5 H17A C17A H17B 108.1 N3B C17B C16B 109.6(4) N3B C17B H17C 109.7 N3B C17B H17D 109.7 C16B C17B H17C 109.7 C16B C17B H17D 109.7 H17C C17B H17D 108.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C13 1.2275(10) O2A C15A 1.416(5) O2A C16A 1.423(5) O2B C15B 1.445(12) O2B C16B 1.416(14) N1 C1 1.3396(9) N1 C2 1.3404(9) N2 C1 1.3408(9) N2 C4 1.3355(10) N3A C13 1.375(2) N3A C14A 1.469(2) N3A C17A 1.463(2) N3B C13 1.348(7) N3B C14B 1.465(7) N3B C17B 1.477(7) C1 C5 1.4831(10) C2 H2 0.9500 C2 C3 1.3850(10) C3 H3 0.9500 C3 C4 1.3853(11) C4 H4 0.9500 C5 C6 1.3979(10) C5 C10 1.3956(10) C6 H6 0.9500 C6 C7 1.3931(10) C7 C8 1.3968(10) C7 C11 1.5198(10) C8 H8 0.9500 C8 C9 1.3907(11) C9 H9 0.9500 C9 C10 1.3914(11) C10 H10 0.9500 C11 H11 1.0000 C11 C12 1.5282(11) C11 C13 1.5296(10) C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C14A H14A 0.9900 C14A H14B 0.9900 C14A C15A 1.5151(17) C14B H14C 0.9900 C14B H14D 0.9900 C14B C15B 1.502(6) C15A H15A 0.9900 C15A H15B 0.9900 C15B H15C 0.9900 C15B H15D 0.9900 C16A H16A 0.9900 C16A H16B 0.9900 C16A C17A 1.5144(18) C16B H16C 0.9900 C16B H16D 0.9900 C16B C17B 1.504(6) C17A H17A 0.9900 C17A H17B 0.9900 C17B H17C 0.9900 C17B H17D 0.9900