#------------------------------------------------------------------------------ #$Date: 2020-03-27 00:27:32 +0200 (Fri, 27 Mar 2020) $ #$Revision: 249737 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/75/4517521.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_4517521 loop_ _publ_author_name 'Zhu, Cuiju' 'Kuniyil, Rositha' 'Jei, Becky B.' 'Ackermann, Lutz' _publ_section_title ; Domino C--H Activation/Directing Group Migration/Alkyne Annulation: Unique Selectivity by d6-Cobalt(III) Catalysts ; _journal_name_full 'ACS Catalysis' _journal_page_first 4444 _journal_paper_doi 10.1021/acscatal.9b05413 _journal_year 2020 _chemical_formula_moiety 'C25 H20 N2 O' _chemical_formula_sum 'C25 H20 N2 O' _chemical_formula_weight 364.43 _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 _atom_sites_solution_primary dual _audit_creation_date 2019-05-20 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 110.430(3) _cell_angle_beta 100.373(3) _cell_angle_gamma 101.270(4) _cell_formula_units_Z 2 _cell_length_a 8.7963(9) _cell_length_b 10.3540(12) _cell_length_c 11.5419(14) _cell_measurement_reflns_used 9996 _cell_measurement_temperature 100.01 _cell_measurement_theta_max 29.616 _cell_measurement_theta_min 2.281 _cell_volume 930.16(19) _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 0.973 _diffrn_measurement_device_type 'Bruker D8 Venture' _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 0.0231 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 17309 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.612 _diffrn_reflns_theta_min 2.452 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_T_max 0.8879 _exptl_absorpt_correction_T_min 0.8426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1013 before and 0.0404 after correction. The Ratio of minimum to maximum transmission is 0.9490. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.301 _exptl_crystal_description block _exptl_crystal_F_000 384 _exptl_crystal_size_max 0.348 _exptl_crystal_size_mid 0.281 _exptl_crystal_size_min 0.191 _refine_diff_density_max 0.384 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.043 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 255 _refine_ls_number_reflns 5094 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0410 _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^)+(0.0458P)^2^+0.3945P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1026 _refine_ls_wR_factor_ref 0.1081 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4496 _reflns_number_total 5094 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs9b05413_si_003.cif _cod_data_source_block 0677_cg_0m _cod_original_cell_volume 930.16(18) _cod_database_code 4517521 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.985 _shelx_estimated_absorpt_t_min 0.973 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C13(H13), C14(H14), C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25) 2.b Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C19(H19A,H19B,H19C) ; _shelx_res_file ; TITL 0677_cg_0m_a.res in P-1 0677_cg_0m.res created by SHELXL-2018/3 at 17:02:22 on 20-May-2019 REM Old TITL 0677_CG_0m in P-1 REM SHELXT solution in P-1 REM R1 0.155, Rweak 0.006, Alpha 0.042, Orientation as input REM Formula found by SHELXT: C25 N2 O CELL 0.71073 8.7963 10.354 11.5419 110.43 100.373 101.27 ZERR 2 0.0009 0.0012 0.0014 0.003 0.003 0.004 LATT 1 SFAC C H N O UNIT 50 40 4 2 L.S. 4 PLAN 20 SIZE 0.191 0.281 0.348 TEMP -173.14 BOND $H list 4 fmap 2 acta OMIT 0 -1 1 OMIT -7 1 13 OMIT 1 2 0 OMIT -1 -4 1 OMIT 7 0 0 REM REM REM WGHT 0.045800 0.394500 FVAR 1.13359 O1 4 0.730779 0.524257 0.847014 11.00000 0.03224 0.02181 = 0.01936 0.01125 0.01156 0.01136 N1 3 0.743904 0.474041 0.640474 11.00000 0.02044 0.01415 = 0.01588 0.00696 0.00640 0.00678 N2 3 0.827159 0.059771 0.429472 11.00000 0.02650 0.01780 = 0.02183 0.00819 0.00806 0.01026 C1 1 0.743485 0.565747 0.760328 11.00000 0.01947 0.01754 = 0.01686 0.00721 0.00660 0.00728 C2 1 0.759259 0.715478 0.775282 11.00000 0.02009 0.01619 = 0.01738 0.00654 0.00636 0.00707 C3 1 0.764383 0.816346 0.895791 11.00000 0.02556 0.02032 = 0.01801 0.00679 0.00808 0.00798 AFIX 43 H3 2 0.753627 0.786422 0.963625 11.00000 -1.20000 AFIX 0 C4 1 0.784976 0.958618 0.915869 11.00000 0.02986 0.01883 = 0.01951 0.00385 0.00795 0.00775 AFIX 43 H4 2 0.788908 1.026822 0.997543 11.00000 -1.20000 AFIX 0 C5 1 0.800127 1.002527 0.815409 11.00000 0.02840 0.01538 = 0.02355 0.00593 0.00737 0.00591 AFIX 43 H5 2 0.814840 1.100780 0.829719 11.00000 -1.20000 AFIX 0 C6 1 0.793893 0.904512 0.695921 11.00000 0.02429 0.01641 = 0.02117 0.00846 0.00689 0.00686 AFIX 43 H6 2 0.803575 0.935713 0.628657 11.00000 -1.20000 AFIX 0 C7 1 0.773199 0.758136 0.673193 11.00000 0.01723 0.01566 = 0.01730 0.00620 0.00442 0.00589 C8 1 0.769441 0.652763 0.551672 11.00000 0.02051 0.01603 = 0.01609 0.00748 0.00524 0.00655 AFIX 43 H8 2 0.777267 0.678821 0.481329 11.00000 -1.20000 AFIX 0 C9 1 0.754504 0.515215 0.539055 11.00000 0.01603 0.01609 = 0.01470 0.00652 0.00425 0.00577 C10 1 0.750954 0.387916 0.429734 11.00000 0.01639 0.01549 = 0.01498 0.00585 0.00383 0.00575 C11 1 0.745874 0.276878 0.466626 11.00000 0.01638 0.01547 = 0.01557 0.00616 0.00457 0.00537 C12 1 0.732046 0.127333 0.382611 11.00000 0.01968 0.01429 = 0.01760 0.00681 0.00747 0.00475 C13 1 0.623051 0.061077 0.260388 11.00000 0.02213 0.01776 = 0.02004 0.00682 0.00473 0.00307 AFIX 43 H13 2 0.554921 0.110506 0.231158 11.00000 -1.20000 AFIX 0 C14 1 0.616148 -0.077734 0.182751 11.00000 0.02927 0.01805 = 0.02134 0.00365 0.00645 -0.00027 AFIX 43 H14 2 0.543301 -0.125044 0.099393 11.00000 -1.20000 AFIX 0 C15 1 0.717523 -0.146499 0.228877 11.00000 0.03627 0.01551 = 0.02654 0.00585 0.01583 0.00663 AFIX 43 H15 2 0.717529 -0.240742 0.177057 11.00000 -1.20000 AFIX 0 C16 1 0.818640 -0.074429 0.352233 11.00000 0.03277 0.01822 = 0.02837 0.01085 0.01458 0.01239 AFIX 43 H16 2 0.885934 -0.122823 0.384057 11.00000 -1.20000 AFIX 0 C17 1 0.743521 0.320781 0.606375 11.00000 0.01976 0.01329 = 0.01669 0.00659 0.00638 0.00600 C18 1 0.588500 0.233388 0.616784 11.00000 0.02249 0.01939 = 0.02308 0.00972 0.00899 0.00427 AFIX 137 H18A 2 0.584779 0.268219 0.706543 11.00000 -1.50000 H18B 2 0.586303 0.131877 0.586512 11.00000 -1.50000 H18C 2 0.495217 0.244144 0.563959 11.00000 -1.50000 AFIX 0 C19 1 0.893153 0.312524 0.692099 11.00000 0.02284 0.01722 = 0.01741 0.00779 0.00443 0.00761 AFIX 137 H19A 2 0.990213 0.364708 0.679576 11.00000 -1.50000 H19B 2 0.892177 0.211825 0.669234 11.00000 -1.50000 H19C 2 0.892670 0.355765 0.782258 11.00000 -1.50000 AFIX 0 C20 1 0.752422 0.389166 0.302322 11.00000 0.01820 0.01289 = 0.01415 0.00509 0.00242 0.00266 C21 1 0.855682 0.328959 0.234968 11.00000 0.01960 0.01472 = 0.01611 0.00521 0.00378 0.00364 AFIX 43 H21 2 0.926810 0.286638 0.271509 11.00000 -1.20000 AFIX 0 C22 1 0.855059 0.330554 0.114885 11.00000 0.02685 0.01723 = 0.01623 0.00367 0.00624 0.00147 AFIX 43 H22 2 0.926809 0.290648 0.070462 11.00000 -1.20000 AFIX 0 C23 1 0.749802 0.390347 0.059556 11.00000 0.03800 0.01949 = 0.01378 0.00672 0.00176 0.00134 AFIX 43 H23 2 0.749187 0.391239 -0.022552 11.00000 -1.20000 AFIX 0 C24 1 0.645676 0.448697 0.125357 11.00000 0.03375 0.01916 = 0.01962 0.00905 -0.00248 0.00622 AFIX 43 H24 2 0.572379 0.488224 0.087326 11.00000 -1.20000 AFIX 0 C25 1 0.647723 0.449791 0.246245 11.00000 0.02340 0.01729 = 0.01887 0.00675 0.00194 0.00691 AFIX 43 H25 2 0.577585 0.491974 0.291153 11.00000 -1.20000 AFIX 0 HKLF 4 REM 0677_cg_0m_a.res in P-1 REM wR2 = 0.108107, GooF = S = 1.04825, Restrained GooF = 1.04825 for all data REM R1 = 0.040979 for 4496 Fo > 4sig(Fo) and 0.046878 for all 5094 data REM 255 parameters refined using 0 restraints END WGHT 0.0458 0.3945 REM Highest difference peak 0.384, deepest hole -0.206, 1-sigma level 0.043 Q1 1 0.7557 0.6425 0.7664 11.00000 0.05 0.38 Q2 1 0.7608 0.4579 0.4816 11.00000 0.05 0.37 Q3 1 0.7782 0.7027 0.6156 11.00000 0.05 0.35 Q4 1 0.7428 0.2014 0.4203 11.00000 0.05 0.34 Q5 1 0.7554 0.7657 0.8339 11.00000 0.05 0.34 Q6 1 0.7390 0.2897 0.5350 11.00000 0.05 0.33 Q7 1 0.6886 0.0921 0.3223 11.00000 0.05 0.32 Q8 1 0.7673 0.8243 0.6805 11.00000 0.05 0.31 Q9 1 0.6266 -0.0067 0.2193 11.00000 0.05 0.30 Q10 1 0.7689 0.7393 0.7257 11.00000 0.05 0.30 Q11 1 0.8175 0.3230 0.6538 11.00000 0.05 0.29 Q12 1 0.7582 0.3974 0.3680 11.00000 0.05 0.28 Q13 1 0.7774 0.5875 0.5454 11.00000 0.05 0.28 Q14 1 0.6704 0.2785 0.6167 11.00000 0.05 0.28 Q15 1 0.7626 0.8834 0.8945 11.00000 0.05 0.26 Q16 1 0.7446 0.3989 0.6298 11.00000 0.05 0.26 Q17 1 0.8001 0.3633 0.2639 11.00000 0.05 0.26 Q18 1 0.7001 0.4161 0.2739 11.00000 0.05 0.26 Q19 1 0.7768 0.3426 0.0839 11.00000 0.05 0.26 Q20 1 0.7726 0.3411 0.4465 11.00000 0.05 0.26 ; _shelx_res_checksum 2568 _shelx_hkl_file ; -1 0 0 1.13531 0.16704 5 -1 0 0 0.76312 0.23137 4 1 0 0 0.72429 0.24649 4 -3 0 0 921.076 15.6966 4 -3 0 0 917.892 14.0746 5 3 0 0 898.156 15.8537 4 -4 0 0 3362.43 51.6492 4 -4 0 0 3352.04 49.3390 5 4 0 0 3312.81 52.0383 4 -5 0 0 721.998 11.9107 5 -5 0 0 749.187 14.4737 4 5 0 0 735.118 14.9507 4 -6 0 0 2196.96 36.3132 4 6 0 0 2161.95 37.1752 4 -7 0 0 173.257 6.12067 4 7 0 0 152.931 6.34605 4 -8 0 0 1141.80 22.0155 3 -8 0 0 1197.54 22.9865 4 8 0 0 1219.60 24.4838 4 -9 0 0 10.8386 2.07245 4 -9 0 0 5.68188 1.77959 2 -9 0 0 7.51038 1.68370 3 9 0 0 7.57906 1.97261 4 -10 0 0 310.859 11.2434 2 -10 0 0 308.016 8.99613 3 -10 0 0 309.123 9.72392 4 -11 0 0 3.82363 1.48643 4 -11 0 0 5.71506 1.95303 2 -11 0 0 4.14379 2.15628 3 -11 0 0 5.66987 1.61856 3 -11 1 0 67.2457 3.55179 3 -11 1 0 69.7268 4.48370 3 -11 1 0 67.8273 4.68235 4 -11 1 0 64.4750 6.11964 2 -10 1 0 666.922 16.4209 4 -10 1 0 663.073 13.9275 3 9 -1 0 159.128 7.52636 4 -9 1 0 160.808 5.43332 3 -9 1 0 161.011 6.81759 4 8 -1 0 1486.26 29.2608 4 -8 1 0 1435.48 25.0649 3 -8 1 0 1472.39 27.7034 4 7 -1 0 1.94489 1.21966 4 -7 1 0 0.26134 0.80283 4 -7 1 0 1.16445 0.67128 3 6 -1 0 1999.11 34.9561 4 -6 1 0 1977.68 30.1421 5 -6 1 0 1950.51 31.6865 3 -6 1 0 2004.29 34.0633 4 5 -1 0 1761.91 30.5633 4 -5 1 0 1749.74 27.8267 3 -5 1 0 1772.34 26.9503 5 -5 1 0 1725.15 29.8414 4 4 -1 0 1861.78 30.3352 4 4 -1 0 1846.03 27.1412 5 -4 1 0 1635.67 30.1613 4 -4 1 0 1833.63 27.4630 5 3 -1 0 5437.33 118.951 1 -3 1 0 5285.09 125.161 1 2 -1 0 1020.79 16.2204 5 2 -1 0 1052.07 17.4299 4 -2 1 0 1057.60 17.3361 4 -2 1 0 1051.72 16.2651 5 1 -1 0 245.375 4.55031 5 1 -1 0 244.697 4.85092 4 -1 1 0 250.235 4.47059 2 -1 1 0 248.609 4.54890 5 -1 1 0 249.240 4.06408 3 -1 -1 0 623.565 10.4937 2 -1 -1 0 647.462 9.53694 4 -2 -1 0 1410.46 21.2771 4 2 1 0 1369.72 21.3646 4 -3 -1 0 10.1609 0.97392 4 -3 -1 0 6.11775 0.91964 2 3 1 0 8.04959 0.94272 4 -4 -1 0 495.121 9.59354 4 -4 -1 0 485.544 8.35147 5 4 1 0 483.349 9.90089 4 -5 -1 0 322.790 7.53471 4 -5 -1 0 317.606 6.03745 5 -5 -1 0 311.973 8.35763 2 5 1 0 332.260 8.05861 4 -6 -1 0 57.7113 2.99511 4 -6 -1 0 57.6061 1.94313 5 -6 -1 0 59.6907 3.57528 2 6 1 0 57.6756 3.26813 4 -7 -1 0 235.077 6.88187 4 -7 -1 0 220.990 7.82394 2 7 1 0 230.246 7.46829 4 -8 -1 0 112.902 5.78534 2 -8 -1 0 114.745 4.83116 4 8 1 0 124.813 5.62348 4 -9 -1 0 11.0264 2.36141 2 -9 -1 0 8.53014 1.77071 4 -10 -1 0 229.363 9.45165 2 -10 -1 0 228.559 7.53811 4 -10 -1 0 221.056 8.09304 3 -11 -1 0 17.4380 3.19566 3 -11 -1 0 16.9421 3.02961 2 -11 -1 0 19.1009 2.82781 3 -11 -1 0 19.8737 2.43700 4 11 -2 0 58.4859 5.36010 4 -11 2 0 70.6744 3.78341 3 -11 2 0 69.8628 4.95760 4 -11 2 0 72.7328 3.23530 3 10 -2 0 4.12678 1.87609 4 -10 2 0 5.64152 1.67869 4 -10 2 0 3.60434 1.11855 3 9 -2 0 0.75479 1.02615 4 -9 2 0 0.56245 0.68187 3 -9 2 0 -0.7816 0.92867 4 8 -2 0 52.2233 4.23328 4 -8 2 0 47.6045 2.39340 3 -8 2 0 50.1772 3.90975 4 7 -2 0 290.786 9.63905 4 -7 2 0 277.261 6.21772 3 -7 2 0 270.090 8.71062 4 6 -2 0 158.488 3.82859 5 6 -2 0 160.879 6.48465 4 -6 2 0 162.066 6.10225 4 -6 2 0 159.317 4.09684 5 -6 2 0 153.724 3.92603 3 5 -2 0 233.810 7.49070 4 5 -2 0 236.889 5.24635 5 -5 2 0 240.960 4.88444 3 -5 2 0 230.835 7.09919 4 -5 2 0 245.339 5.44773 5 4 -2 0 1.03807 0.72527 4 4 -2 0 0.82048 0.46421 5 -4 2 0 0.68751 0.68002 4 -4 2 0 0.79657 0.43908 5 -4 2 0 0.04977 0.23708 3 3 -2 0 4.42414 0.92193 4 3 -2 0 6.07134 0.85755 5 3 -2 0 5.85302 0.49892 3 -3 2 0 6.69955 0.53998 3 -3 2 0 6.30246 0.85713 5 2 -2 0 255.768 4.44353 3 2 -2 0 249.078 5.99262 4 2 -2 0 250.205 5.45638 5 -2 2 0 249.495 5.28831 2 -2 2 0 257.565 4.62791 3 -2 2 0 249.613 5.40074 5 1 -2 0 3209.45 92.7637 1 -1 2 0 2824.82 89.5140 1 0 -2 0 1223.35 18.7026 4 1 2 0 2745.00 83.1086 1 -2 -2 0 2109.47 72.4764 1 2 2 0 2069.73 71.0569 1 -3 -2 0 458.313 9.82552 2 -3 -2 0 478.712 8.05200 4 -4 -2 0 8.27172 1.42605 2 -4 -2 0 10.7855 0.97897 4 4 2 0 8.74177 0.98615 4 -5 -2 0 127.519 3.75886 4 -5 -2 0 112.635 4.77183 2 5 2 0 121.984 4.05275 4 -6 -2 0 81.7866 2.64132 5 -6 -2 0 78.7087 4.26342 2 -7 -2 0 1.63076 1.05887 2 -7 -2 0 2.34109 0.80164 4 -7 -2 0 2.65844 0.62305 5 -7 -2 0 3.10388 0.64062 5 -8 -2 0 -0.5651 0.64552 2 -8 -2 0 2.15794 0.90523 4 -9 -2 0 173.584 5.63603 4 -9 -2 0 163.963 7.72064 2 -10 -2 0 8.76731 1.62381 4 -10 -2 0 7.75228 2.41190 2 -10 -2 0 10.8292 2.42394 3 -12 3 0 4.60561 1.59564 4 -11 3 0 5.38770 1.90160 4 10 -3 0 2.35892 1.60558 4 -10 3 0 1.32190 0.62435 3 -10 3 0 -0.4088 0.91216 4 -9 3 0 88.7231 5.35806 4 -9 3 0 81.9724 2.84296 3 8 -3 0 70.0784 5.05886 4 8 -3 0 66.4592 2.41880 5 -8 3 0 67.4434 2.44355 3 -8 3 0 67.2859 4.57381 4 7 -3 0 5.36658 1.65251 4 7 -3 0 8.00234 1.14214 5 -7 3 0 8.37429 0.89175 3 -7 3 0 5.38500 1.59165 4 6 -3 0 18.1084 1.51905 5 6 -3 0 17.5605 2.74521 4 -6 3 0 21.3983 1.64995 5 -6 3 0 19.0866 2.32626 4 5 -3 0 233.551 5.86752 5 5 -3 0 221.601 7.53883 4 -5 3 0 233.686 4.50121 3 -5 3 0 221.179 7.17343 4 -5 3 0 226.286 5.79482 5 4 -3 0 629.331 10.0364 3 4 -3 0 634.663 12.0593 5 4 -3 0 618.062 13.6550 4 -4 3 0 632.219 10.2544 3 -4 3 0 621.104 11.8811 5 -4 3 0 620.778 12.1114 2 -4 3 0 605.612 13.2113 4 3 -3 0 610.690 9.83448 3 3 -3 0 598.120 12.5674 4 3 -3 0 602.197 11.6451 5 -3 3 0 607.390 11.5752 5 -3 3 0 592.108 11.3663 2 -3 3 0 608.587 10.2082 3 2 -3 0 106.952 3.60863 5 2 -3 0 103.493 3.28212 2 2 -3 0 106.418 2.96686 3 2 -3 0 107.520 3.78544 4 -2 3 0 109.855 3.60584 5 -2 3 0 110.197 3.71634 4 -2 3 0 113.394 3.48931 2 1 -3 0 710.223 12.8288 4 1 -3 0 725.236 12.9237 2 1 -3 0 737.189 13.0258 3 1 -3 0 717.946 13.2950 5 -1 3 0 727.591 12.6992 4 -1 3 0 733.944 12.9258 2 0 -3 0 392.128 8.11343 2 0 -3 0 402.290 7.25588 4 0 -3 0 400.387 8.42330 5 0 3 0 403.840 7.03465 4 0 3 0 386.565 8.03974 2 -2 -3 0 129.334 4.26184 2 2 3 0 125.696 4.19225 2 -3 -3 0 2227.61 36.4100 2 -4 -3 0 35.1640 1.24195 4 -4 -3 0 34.8764 2.54984 2 -5 -3 0 93.2120 3.51535 5 -5 -3 0 96.9363 2.68020 4 -5 -3 0 99.9538 4.63927 2 -6 -3 0 89.6080 2.84960 4 -6 -3 0 89.3638 4.71898 2 -6 -3 0 83.6828 3.32352 5 -7 -3 0 30.9982 1.78159 5 -7 -3 0 29.2198 3.00685 2 -7 -3 0 32.2616 1.98284 4 -7 -3 0 31.2113 1.91920 5 -8 -3 0 14.7236 1.46596 4 -8 -3 0 10.7985 2.24267 2 -9 -3 0 215.187 9.16475 2 -9 -3 0 201.816 5.50421 4 -10 -3 0 0.84896 0.76813 4 -10 -3 0 0.09520 1.22237 2 -12 4 0 1.10056 1.44806 4 -11 4 0 0.50292 1.53578 4 10 -4 0 37.9092 4.23406 4 -10 4 0 30.5876 3.56817 4 9 -4 0 11.0906 1.24579 5 9 -4 0 7.86246 2.65581 4 -9 4 0 9.91920 2.37956 4 8 -4 0 228.122 5.98484 5 8 -4 0 219.663 9.37463 4 -8 4 0 221.863 12.9555 4 7 -4 0 3.96042 1.46268 4 7 -4 0 3.87422 1.00484 5 -7 4 0 2.23370 1.25306 4 6 -4 0 307.731 7.83510 5 6 -4 0 319.449 10.2126 4 -6 4 0 305.737 8.37511 2 -6 4 0 312.606 7.82484 5 -6 4 0 313.169 9.57572 4 5 -4 0 30.7964 2.81436 4 5 -4 0 32.2477 2.25573 5 -5 4 0 33.6618 2.27030 5 -5 4 0 35.4940 2.87081 4 -5 4 0 33.4695 2.33469 2 -5 4 0 34.1712 1.44812 3 4 -4 0 16.2508 1.66212 5 4 -4 0 17.1593 2.02595 4 4 -4 0 18.5784 1.01221 3 -4 4 0 21.9124 2.13969 4 -4 4 0 15.5307 1.58245 2 -4 4 0 19.5330 1.75631 5 3 -4 0 16.5050 1.68919 5 3 -4 0 16.8611 1.80919 4 3 -4 0 16.6124 1.21193 3 3 -4 0 18.0222 1.56217 2 -3 4 0 17.9815 1.82045 4 -3 4 0 19.8198 2.15042 5 -3 4 0 15.8905 1.53899 2 2 -4 0 838.388 15.7517 4 2 -4 0 827.646 15.7741 5 2 -4 0 833.926 14.8127 3 2 -4 0 810.237 16.5883 2 -2 4 0 828.924 15.2970 2 -2 4 0 843.606 15.4554 4 1 -4 0 485.658 9.77778 4 1 -4 0 477.914 10.4852 5 -1 4 0 476.758 9.45636 4 -1 4 0 502.410 10.1335 2 0 -4 0 17.5173 1.49651 4 0 -4 0 19.5848 1.68743 2 0 4 0 20.7280 1.66559 2 0 4 0 21.7706 1.19964 4 -1 -4 0 2.30997 0.80334 5 -1 -4 0 1.68305 0.68813 2 1 4 0 1.04166 0.54480 2 -2 -4 0 520.846 11.3719 2 -2 -4 0 509.052 11.0837 5 2 4 0 527.713 11.3307 2 -3 -4 0 5.47928 1.29229 2 -3 -4 0 2.89052 0.93154 5 3 4 0 1.98255 0.82573 2 -4 -4 0 24.6590 2.36338 2 -4 -4 0 27.8498 2.16860 5 -5 -4 0 51.7169 3.62713 2 -5 -4 0 55.9084 3.03533 5 -6 -4 0 385.756 12.6569 2 -6 -4 0 360.366 8.95546 5 -7 -4 0 100.499 3.63897 5 -7 -4 0 107.628 5.84117 2 -7 -4 0 92.1788 3.83230 5 -8 -4 0 47.4862 4.22688 2 -8 -4 0 50.1321 2.52638 5 -9 -4 0 70.6938 5.82870 2 -10 -4 0 1.23933 1.94441 3 -11 5 0 34.2177 4.10614 4 10 -5 0 19.6974 3.72508 4 10 -5 0 24.5664 1.81589 5 -10 5 0 23.0293 3.66355 4 -10 5 0 25.2904 3.41748 2 9 -5 0 114.227 4.31536 5 -9 5 0 125.243 6.00125 2 -9 5 0 121.804 6.72950 4 8 -5 0 15.3018 2.04152 5 -8 5 0 15.6318 2.26871 2 -8 5 0 11.8421 2.33905 4 7 -5 0 246.204 9.67319 4 7 -5 0 259.511 7.52616 5 -7 5 0 257.294 9.17214 4 -7 5 0 230.159 7.73393 2 6 -5 0 33.0022 3.30425 4 6 -5 0 36.9807 2.69010 5 -6 5 0 37.0787 3.27471 4 -6 5 0 39.2989 2.85096 2 5 -5 0 464.349 8.04677 3 5 -5 0 456.841 10.9892 5 5 -5 0 461.669 12.5089 4 -5 5 0 443.198 10.7666 2 -5 5 0 451.134 11.8209 4 4 -5 0 0.29018 0.66650 4 4 -5 0 1.54459 0.84777 5 4 -5 0 0.23125 0.39395 3 -4 5 0 0.13783 0.61060 4 -4 5 0 0.20774 0.61864 2 3 -5 0 286.647 8.00305 5 3 -5 0 277.572 6.64154 3 3 -5 0 285.608 7.33122 2 3 -5 0 285.301 8.19148 4 -3 5 0 271.213 7.69231 4 -3 5 0 276.131 7.49298 2 2 -5 0 1669.46 28.2900 2 2 -5 0 1669.84 28.1457 3 2 -5 0 1648.06 29.0675 5 2 -5 0 1696.42 28.7270 4 -2 5 0 1662.80 28.3737 2 -2 5 0 1689.37 28.1702 4 1 -5 0 62.1798 2.89903 4 1 -5 0 62.4846 3.16739 2 1 -5 0 66.5343 3.42406 3 1 -5 0 61.5286 3.38876 5 -1 5 0 66.6981 2.76803 4 0 -5 0 1228.17 22.9167 5 0 -5 0 1254.84 22.5436 2 0 -5 0 1260.01 20.7629 4 0 5 0 1297.85 20.1936 4 0 5 0 1235.31 22.3428 2 -1 -5 0 224.477 6.95564 5 -1 -5 0 232.874 6.89554 2 -1 -5 0 233.366 4.58285 4 1 5 0 223.190 6.71092 2 -2 -5 0 196.215 6.43537 2 -2 -5 0 186.000 6.29354 5 -3 -5 0 371.062 9.60380 5 -3 -5 0 360.881 9.83560 2 3 5 0 359.503 9.77335 2 -4 -5 0 108.551 4.70696 5 -4 -5 0 110.086 5.20931 2 -5 -5 0 24.9897 2.35345 5 -5 -5 0 27.9364 3.22942 2 -6 -5 0 42.9009 3.70252 2 -6 -5 0 48.6994 3.12421 5 -7 -5 0 0.87085 0.83906 5 -7 -5 0 -0.4259 0.99293 2 -8 -5 0 44.4463 2.80594 5 -8 -5 0 39.2720 4.07341 2 -8 -5 0 49.0396 2.60941 5 -9 -5 0 -0.0259 1.33686 2 11 -6 0 0.48955 0.81959 5 -11 6 0 0.23109 1.23084 4 10 -6 0 0.23176 0.80881 5 -10 6 0 1.44662 1.20478 2 -10 6 0 2.05785 1.64750 4 9 -6 0 20.6942 3.82667 4 9 -6 0 18.2242 2.11558 5 -9 6 0 23.7901 2.93618 2 -9 6 0 18.9851 3.23290 4 8 -6 0 21.7021 2.33890 5 -8 6 0 24.2104 2.68471 2 -8 6 0 18.8887 2.98671 4 7 -6 0 196.108 6.96580 5 -7 6 0 188.372 10.2289 4 -7 6 0 177.511 6.89493 2 6 -6 0 1.90260 0.99719 5 6 -6 0 2.86169 0.55727 3 6 -6 0 1.09315 1.00484 4 -6 6 0 3.16010 1.41865 4 -6 6 0 1.51115 0.97484 2 5 -6 0 742.919 17.5742 4 5 -6 0 724.097 16.1650 5 5 -6 0 742.169 12.8165 3 -5 6 0 703.557 16.8477 2 -5 6 0 748.999 16.8046 4 4 -6 0 153.352 6.41747 4 4 -6 0 156.875 4.64729 3 4 -6 0 156.711 5.56701 2 4 -6 0 153.026 6.12658 5 -4 6 0 154.189 6.04981 4 -4 6 0 155.371 5.80054 2 3 -6 0 24.0409 2.09762 3 3 -6 0 26.2428 2.22527 2 3 -6 0 22.9344 2.33171 4 -3 6 0 23.1713 2.21756 4 -3 6 0 22.6369 2.16026 2 2 -6 0 46.3543 2.92915 2 2 -6 0 42.1059 3.08625 5 2 -6 0 46.8861 2.97477 3 2 -6 0 48.0444 2.98589 4 -2 6 0 48.2807 3.00664 2 -2 6 0 45.5704 2.69439 4 1 -6 0 191.421 6.77606 5 1 -6 0 185.951 6.61924 3 1 -6 0 190.967 6.34683 2 1 -6 0 193.588 5.78291 4 -1 6 0 187.221 5.26166 4 0 -6 0 9.81343 1.68454 2 0 -6 0 10.8946 2.00848 5 0 -6 0 11.4173 1.23926 4 0 6 0 11.6220 1.06799 4 0 6 0 12.2909 1.92521 2 -1 -6 0 245.357 7.86143 5 -1 -6 0 244.180 7.66718 2 1 6 0 235.687 7.74771 2 -2 -6 0 10.4820 1.74681 2 -2 -6 0 14.8092 2.31170 5 2 6 0 11.4694 1.91605 2 -3 -6 0 199.908 7.25036 2 -3 -6 0 179.721 6.75428 5 3 6 0 179.717 6.87255 2 -4 -6 0 4.70958 2.56744 2 -4 -6 0 0.33768 1.04068 5 4 6 0 1.12595 0.86214 2 -5 -6 0 38.1843 3.56797 2 -6 -6 0 5.83208 1.68380 2 -6 -6 0 5.07062 1.66071 5 -7 -6 0 30.0082 3.58751 2 -7 -6 0 26.2773 4.31580 5 -8 -6 0 48.4946 3.36380 5 -8 -6 0 51.4413 3.02491 5 -8 -6 0 53.1102 4.91311 2 11 -7 0 -0.3913 1.17543 5 -11 7 0 0.84986 1.61278 4 10 -7 0 1.36348 1.09443 5 -10 7 0 3.14747 2.85355 4 9 -7 0 12.7849 2.82657 4 9 -7 0 13.7744 2.33618 5 -9 7 0 7.31939 1.72200 2 -9 7 0 14.1590 3.09732 4 8 -7 0 28.7717 2.82415 5 -8 7 0 17.8873 2.94107 4 -8 7 0 19.7103 2.86221 2 7 -7 0 101.107 5.27757 5 -7 7 0 96.6367 5.72655 4 -7 7 0 89.7933 5.04604 2 6 -7 0 16.8923 1.27694 3 6 -7 0 12.7223 2.33781 4 6 -7 0 16.8792 2.54499 5 -6 7 0 15.8441 2.48996 2 -6 7 0 17.2012 2.86258 4 5 -7 0 156.951 7.17821 4 5 -7 0 151.374 4.59360 3 5 -7 0 155.894 6.67420 5 -5 7 0 159.884 6.71279 4 -5 7 0 153.451 6.29697 2 4 -7 0 81.5416 5.70005 4 4 -7 0 78.7938 4.12171 2 4 -7 0 83.7254 4.76995 5 4 -7 0 81.9205 3.66659 3 -4 7 0 80.8432 4.39662 2 -4 7 0 82.4391 4.46674 4 3 -7 0 116.233 4.87350 3 3 -7 0 121.153 5.68372 5 3 -7 0 116.438 5.38729 4 3 -7 0 115.890 5.05139 2 -3 7 0 105.346 4.95044 2 -3 7 0 116.831 4.96661 4 2 -7 0 68.0526 3.95985 3 2 -7 0 68.8427 3.79718 4 2 -7 0 75.7245 4.05966 2 2 -7 0 67.3906 4.19214 5 -2 7 0 65.8031 3.38172 4 -2 7 0 77.9650 4.10908 2 1 -7 0 0.01665 0.75297 3 1 -7 0 0.26422 0.63418 2 1 -7 0 -0.0357 0.50770 4 1 -7 0 0.54517 0.73058 5 -1 7 0 0.24132 0.51010 4 -1 7 0 0.40986 0.63444 2 0 -7 0 117.421 5.65198 5 0 -7 0 118.193 4.06133 4 0 -7 0 124.527 5.49759 2 0 7 0 121.475 5.30676 2 0 7 0 122.851 3.51563 4 -1 -7 0 7.50051 1.88907 5 -1 -7 0 5.84749 1.46027 2 1 7 0 3.07003 0.99401 2 -2 -7 0 51.0878 3.71093 2 -2 -7 0 46.2258 3.61178 5 2 7 0 47.4777 3.49275 2 -3 -7 0 764.443 17.8168 5 -3 -7 0 796.897 18.3119 2 -4 -7 0 30.3813 3.30848 2 -4 -7 0 33.8157 3.18107 5 -5 -7 0 1064.06 22.8050 5 -5 -7 0 1124.61 24.5140 2 -6 -7 0 0.22737 0.97781 5 -6 -7 0 -0.6984 1.15737 2 -7 -7 0 67.7508 5.46940 2 -7 -7 0 71.8626 4.40273 5 -8 -7 0 5.05889 1.61043 5 11 -8 0 26.4828 2.85835 5 10 -8 0 14.5903 2.40384 5 -10 8 0 8.63623 2.61348 4 9 -8 0 9.51077 2.00101 5 -9 8 0 5.02064 1.66600 2 -9 8 0 5.01792 1.89480 4 8 -8 0 5.55987 1.67515 4 8 -8 0 3.44623 1.42929 5 -8 8 0 3.26360 1.54266 4 7 -8 0 68.9850 4.77362 5 7 -8 0 73.0681 5.59919 4 -7 8 0 81.0550 5.46867 4 -7 8 0 80.3279 5.01056 2 6 -8 0 510.907 13.2727 3 6 -8 0 523.750 14.4277 5 6 -8 0 538.540 15.7519 4 -6 8 0 515.953 13.8838 2 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5.09288 2 -3 -8 0 77.9364 4.94790 5 -4 -8 0 289.154 10.2586 5 -4 -8 0 317.311 11.0642 2 4 8 0 296.805 10.7206 2 -5 -8 0 58.0014 4.34403 5 -5 -8 0 50.1948 4.60990 2 -6 -8 0 23.6442 3.37157 5 -6 -8 0 19.7137 3.35546 2 -6 -8 0 17.6068 3.58838 3 -7 -8 0 5.83078 1.69014 5 10 -9 0 43.9536 4.10501 5 -10 9 0 50.0685 7.68777 4 9 -9 0 35.9285 3.84992 5 -9 9 0 33.8427 5.15076 4 -8 9 0 53.8837 4.29260 2 -8 9 0 59.8725 5.04262 4 7 -9 0 3.99867 0.84646 3 7 -9 0 4.22854 1.86812 4 -7 9 0 3.27085 1.56356 2 -7 9 0 2.78822 1.52107 4 6 -9 0 12.8597 1.56865 3 6 -9 0 14.3460 3.03274 4 -6 9 0 10.7203 2.23668 4 -6 9 0 14.6250 2.61563 2 5 -9 0 1.53849 1.01060 3 5 -9 0 1.11750 1.05496 2 5 -9 0 1.40481 1.30536 4 5 -9 0 -1.1594 0.64363 5 -5 9 0 0.31377 1.24152 4 -5 9 0 -0.3322 0.88167 2 4 -9 0 131.108 6.10982 2 4 -9 0 117.417 6.30446 4 4 -9 0 122.104 5.46729 3 -4 9 0 126.030 5.87000 4 -4 9 0 117.305 5.94046 2 3 -9 0 27.9412 3.09787 2 3 -9 0 30.4289 3.03995 3 3 -9 0 28.7585 2.96718 4 -3 9 0 29.7959 3.02215 2 -3 9 0 27.5749 2.71409 4 2 -9 0 232.764 8.89661 3 2 -9 0 238.656 8.11785 4 2 -9 0 256.129 8.98853 2 -2 9 0 246.224 7.30786 4 1 -9 0 8.22847 1.64881 4 1 -9 0 15.5048 2.84229 2 1 -9 0 8.75012 2.37170 3 -1 9 0 10.4792 1.50751 4 0 -9 0 2.06809 1.05904 5 0 -9 0 2.65498 1.09931 2 0 -9 0 2.03214 1.45326 3 0 9 0 0.90238 0.52940 4 -1 -9 0 0.03414 1.04507 5 -1 -9 0 2.97552 1.28418 2 -1 -9 0 0.46340 1.32631 3 -2 -9 0 3.08908 1.37337 5 -2 -9 0 5.44238 2.06087 3 -2 -9 0 3.85296 1.55063 2 -3 -9 0 4.30967 1.92814 3 -3 -9 0 8.75717 2.23418 2 -3 -9 0 4.98821 1.82977 5 3 9 0 3.04536 1.31280 2 -4 -9 0 247.373 11.6263 3 -4 -9 0 216.586 9.55875 2 -4 -9 0 216.611 9.59985 5 -5 -9 0 8.18878 2.25540 5 -5 -9 0 8.07279 2.26727 2 -5 -9 0 9.48233 3.08931 3 -6 -9 0 114.930 6.72161 5 10 -10 0 1.34386 1.76486 5 9 -10 0 20.1508 3.24795 5 -9 10 0 18.7929 3.08168 4 8 -10 0 10.2344 2.41321 5 -8 10 0 10.4862 2.58973 4 7 -10 0 -1.4674 0.97529 5 7 -10 0 -0.4325 1.12369 4 7 -10 0 1.64780 0.68647 3 -7 10 0 0.01919 0.89437 4 -7 10 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3.61611 4 -1 3 -13 110.700 4.96882 2 1 -3 13 91.8203 5.97309 5 -2 3 -13 31.7901 2.97949 2 2 -3 13 33.3866 3.51037 5 -3 3 -13 -0.9675 0.89624 2 3 -3 13 0.30496 1.32966 5 -4 3 -13 46.8258 4.05062 2 -8 -2 13 29.1496 4.97665 5 -8 -2 13 47.6499 3.67359 3 -7 -2 13 8.69301 2.52170 4 -7 -2 13 1.63247 1.74135 5 -7 -2 13 4.85331 1.63136 3 6 2 -13 58.1464 5.45870 3 -6 -2 13 52.0722 6.61714 5 -6 -2 13 47.2712 3.80110 3 5 2 -13 1.61486 1.75022 3 -5 -2 13 2.78709 1.24269 3 -4 -2 13 157.057 8.64710 5 -4 -2 13 156.857 7.33054 3 3 2 -13 1.97903 1.36017 3 -3 -2 13 5.72268 2.13933 5 -3 -2 13 5.37092 1.84628 3 2 2 -13 58.0637 4.62372 3 -2 -2 13 57.5699 5.05754 5 -2 -2 13 60.3603 4.80310 3 1 2 -13 -0.3362 1.04948 3 1 2 -13 2.33061 0.86040 2 -1 -2 13 1.38320 1.49826 5 0 2 -13 -1.1044 0.60257 2 0 -2 13 1.50176 1.27973 5 0 -2 13 0.33453 1.05962 4 -1 2 -13 1.29848 0.90171 2 1 -2 13 -0.4068 0.98303 5 -2 2 -13 54.7679 3.91042 2 2 -2 13 50.6623 4.36874 5 -3 2 -13 7.99983 1.87171 2 3 -2 13 2.45097 1.62347 5 4 -2 13 160.856 8.01987 5 8 1 -13 1.57071 1.33058 3 -7 -1 13 3.17135 1.53759 5 -7 -1 13 -1.3673 1.25239 4 -6 -1 13 11.9197 2.41048 3 -6 -1 13 15.0484 3.31645 5 5 1 -13 2.04843 1.43036 3 -5 -1 13 4.35408 1.86342 5 4 1 -13 27.8248 5.08839 3 -4 -1 13 37.7967 4.46074 5 3 1 -13 2.71548 1.50146 3 -3 -1 13 4.75583 1.77629 5 2 1 -13 125.340 6.87161 5 2 1 -13 126.516 6.71085 3 -2 -1 13 127.211 7.60148 5 1 1 -13 15.6992 2.65919 5 1 1 -13 10.9206 1.61154 2 -1 -1 13 13.1090 2.87173 5 0 1 -13 96.2492 5.61517 5 0 1 -13 95.2709 4.41681 2 0 -1 13 97.9100 6.37983 5 0 -1 13 84.6218 7.76741 4 1 -1 13 9.51488 2.28146 5 -2 1 -13 3.67878 1.39799 2 2 -1 13 3.26164 1.75031 5 -3 1 -13 -1.9862 1.02467 2 3 -1 13 0.48969 1.12718 5 8 0 -13 62.2819 4.53053 3 -7 0 13 24.2969 4.28515 5 -7 0 13 34.1922 5.53976 4 -6 0 13 337.762 14.1774 4 -6 0 13 329.395 13.7507 5 5 0 -13 0.15497 1.40704 3 -5 0 13 -1.5683 1.52259 5 4 0 -13 216.945 8.75165 3 -4 0 13 206.643 10.3736 5 3 0 -13 61.1535 4.67773 3 -3 0 13 59.1316 5.41458 5 2 0 -13 79.8887 6.35092 3 -2 0 13 78.4576 6.03583 5 1 0 -13 44.8825 2.82321 2 -1 0 13 46.9784 4.68084 5 0 0 -13 185.885 8.08851 5 0 0 -13 193.261 6.89796 2 0 0 13 189.836 9.16741 5 -1 0 -13 14.8758 2.42867 2 -1 0 -13 17.5047 2.99759 5 1 0 13 20.0136 3.32569 5 -2 0 -13 256.712 9.37738 2 2 0 13 232.482 9.85048 5 8 -1 -13 52.7904 4.14307 3 7 -1 -13 3.41941 1.46428 3 -6 1 13 19.8820 3.84698 5 -6 1 13 21.2202 3.79221 4 -5 1 13 28.5876 4.80763 4 -5 1 13 33.7684 5.01457 5 4 -1 -13 10.8225 2.32710 3 -4 1 13 9.16536 2.76412 5 3 -1 -13 8.40850 2.17961 3 -3 1 13 13.9395 3.83472 5 2 -1 -13 97.6841 3.89554 2 -2 1 13 96.6257 6.85454 5 1 -1 -13 1.73820 1.07426 2 -1 1 13 -2.0997 1.12611 5 0 -1 -13 58.7267 5.38004 2 0 1 13 63.5987 5.37282 5 -1 -1 -13 2.54510 1.24180 2 1 1 13 4.49973 1.72984 5 -2 -1 -13 3.18629 1.35398 2 2 1 13 -0.6758 1.85952 5 7 -2 -13 36.9863 3.80264 3 6 -2 -13 19.6697 3.03922 3 -6 2 13 14.4889 4.07352 4 5 -2 -13 88.2706 5.40988 3 -5 2 13 99.0969 7.39418 4 -5 2 13 95.4551 7.35583 5 4 -2 -13 28.0801 3.37169 3 -4 2 13 17.6189 3.78200 5 -4 2 13 26.8891 4.61063 4 3 -2 -13 11.8743 1.43308 2 -3 2 13 16.7405 3.18860 5 2 -2 -13 153.149 5.59680 2 -2 2 13 155.115 8.99039 5 1 -2 -13 2.62673 1.09690 2 -1 2 13 2.08252 1.78586 5 0 -2 -13 131.221 6.17614 2 -1 -2 -13 7.42439 1.88064 2 1 2 13 0.25753 2.04815 5 6 -3 -13 17.4023 3.19380 3 5 -3 -13 38.9818 3.99505 3 -5 3 13 48.2998 5.53750 4 -4 3 13 -0.7804 1.26832 4 3 -3 -13 63.5249 3.26161 2 -3 3 13 68.4905 6.06946 4 -3 3 13 60.5479 6.92545 5 2 -3 -13 5.97623 1.41142 2 -2 3 13 3.89231 1.98788 5 1 -3 -13 125.829 5.93733 2 -1 3 13 121.126 7.64298 4 -1 3 13 127.930 8.06943 5 3 10 -14 30.2546 3.10263 2 2 10 -14 5.67052 1.46959 2 1 10 -14 48.7619 3.38761 2 0 -10 14 0.74402 1.73012 5 -1 10 -14 17.2111 2.84264 2 1 -10 14 16.3283 3.70746 5 2 -10 14 10.7323 2.50420 5 3 9 -14 12.3543 1.51744 2 -3 -9 14 9.52992 2.69878 3 2 9 -14 133.835 4.94002 2 -2 -9 14 147.794 8.18646 5 -2 -9 14 123.364 7.46436 3 1 9 -14 -2.1019 0.84059 2 -1 -9 14 -0.2044 1.27953 3 -1 -9 14 -0.2318 1.62283 5 0 9 -14 150.436 6.18409 2 0 -9 14 163.910 8.56309 5 0 -9 14 168.790 8.75579 3 1 -9 14 1.30484 1.72742 5 -2 9 -14 20.2725 3.08161 2 3 -9 14 27.1115 3.98283 5 -5 -8 14 96.2639 6.23160 3 -4 -8 14 16.6766 3.21483 3 -3 -8 14 196.656 9.67693 5 -3 -8 14 190.161 8.96667 3 2 8 -14 9.32033 1.39073 2 -2 -8 14 9.38819 2.50074 5 -2 -8 14 13.4901 3.13336 3 1 8 -14 173.587 7.11814 2 -1 -8 14 199.146 9.05458 3 -1 -8 14 183.656 9.34687 5 0 8 -14 0.15850 1.23149 2 0 -8 14 0.33936 1.58231 5 0 -8 14 -0.2239 1.36621 3 1 -8 14 32.1116 3.90263 3 1 -8 14 30.6590 3.87882 5 -2 8 -14 1.71034 1.88967 2 2 -8 14 2.30746 1.50025 5 2 -8 14 1.94676 2.15581 3 3 -8 14 3.23219 1.89468 5 -6 -7 14 32.9542 3.78927 3 -5 -7 14 21.5846 3.58896 3 -4 -7 14 2.96001 1.67274 5 -4 -7 14 1.29922 1.26832 3 -3 -7 14 12.5629 2.90057 5 -3 -7 14 7.92061 3.00416 3 -2 -7 14 16.9257 4.32101 3 -2 -7 14 14.2935 4.28275 5 1 7 -14 175.131 5.61880 2 -1 -7 14 183.963 9.04456 5 -1 -7 14 200.886 9.25275 3 0 7 -14 11.7027 1.84831 2 0 -7 14 10.0189 2.67472 5 0 -7 14 14.8457 3.04850 3 -1 7 -14 49.1198 3.41797 2 1 -7 14 39.6361 4.18655 3 1 -7 14 44.7805 4.44484 5 -2 7 -14 4.23774 1.55291 2 2 -7 14 3.28369 1.74897 3 2 -7 14 2.85889 1.54725 5 -3 7 -14 6.62375 1.68932 2 3 -7 14 2.63815 1.58116 5 -5 -6 14 23.4053 4.20839 5 -5 -6 14 32.6830 3.67724 3 -4 -6 14 -1.4247 0.97929 3 -4 -6 14 1.74594 1.65293 5 -3 -6 14 1.59384 2.50528 5 -3 -6 14 1.17793 1.49924 3 -2 -6 14 89.8946 5.94738 3 -2 -6 14 95.9343 6.54894 5 1 6 -14 5.50395 1.12474 2 -1 -6 14 5.09996 1.96717 5 -1 -6 14 6.66290 2.81874 3 0 6 -14 25.4521 2.97426 2 0 -6 14 20.6657 3.31296 3 0 -6 14 20.2156 3.26134 5 -1 6 -14 116.081 5.29057 2 1 -6 14 116.492 6.84608 5 1 -6 14 118.043 7.13583 3 2 -6 14 8.04011 2.21523 3 2 -6 14 5.44008 2.10736 5 -3 6 -14 203.008 8.14617 2 3 -6 14 207.219 8.88707 5 -7 -5 14 30.9416 3.40477 3 -6 -5 14 105.795 6.08361 3 -6 -5 14 96.9260 8.75502 5 -5 -5 14 68.2264 5.94514 5 -5 -5 14 63.9616 4.80571 3 -4 -5 14 12.1052 2.78541 5 -4 -5 14 18.2348 3.05233 3 -3 -5 14 1.36818 1.40747 5 -3 -5 14 1.89883 1.20962 3 -2 -5 14 2.75225 1.58722 5 -2 -5 14 -1.0431 1.01182 3 1 5 -14 4.33943 0.91980 2 1 5 -14 3.69683 0.91908 2 -1 -5 14 3.36147 2.24347 5 -1 -5 14 2.31909 1.39267 3 0 5 -14 1.15107 0.90861 2 0 5 -14 2.24822 1.06161 2 0 -5 14 2.23425 1.56234 3 0 -5 14 4.66798 1.80965 5 -1 5 -14 39.8738 3.05878 2 -1 5 -14 38.0811 2.98857 2 1 -5 14 31.4955 3.93672 5 1 -5 14 47.7203 4.69040 3 2 -5 14 19.1178 3.63763 3 2 -5 14 18.5703 3.12556 5 -3 5 -14 2.42026 1.42440 2 3 -5 14 -0.8196 1.35231 5 -7 -4 14 12.5795 2.47315 3 -6 -4 14 3.14567 1.48728 3 -6 -4 14 0.93273 1.73743 5 -5 -4 14 18.3887 3.05099 3 -5 -4 14 11.6405 2.94286 5 -4 -4 14 16.5298 2.72045 3 -4 -4 14 20.6053 3.77126 5 -3 -4 14 61.4815 4.77995 3 -3 -4 14 59.7073 5.34717 5 -2 -4 14 102.774 6.82288 5 -2 -4 14 95.9122 6.07511 3 1 4 -14 46.8236 2.37361 2 1 4 -14 53.0551 2.61003 2 -1 -4 14 50.1790 4.62686 3 -1 -4 14 54.0175 4.89525 5 0 4 -14 0.96180 0.96812 2 0 4 -14 0.08613 0.83857 2 0 -4 14 0.45145 1.22866 5 0 -4 14 1.54899 1.82642 3 -1 4 -14 42.5658 3.20198 2 -1 4 -14 39.9788 3.12559 2 1 -4 14 41.0700 4.31939 5 -2 4 -14 81.4333 4.65894 2 2 -4 14 70.3903 5.12298 5 -3 4 -14 75.1871 4.97205 2 3 -4 14 72.4235 5.13948 5 7 3 -14 200.833 9.59923 3 -7 -3 14 221.644 8.59999 3 6 3 -14 76.6233 5.60988 3 -6 -3 14 63.5661 6.09154 5 -6 -3 14 76.2783 5.02271 3 5 3 -14 203.214 9.34907 3 -5 -3 14 216.159 10.6338 5 -5 -3 14 222.838 8.98824 3 4 3 -14 56.4471 6.00402 3 -4 -3 14 49.0045 4.33873 3 -4 -3 14 62.9793 5.74512 5 -3 -3 14 51.2011 5.09016 5 -3 -3 14 44.3299 4.03815 3 -2 -3 14 19.4359 3.13311 3 -2 -3 14 20.9270 3.63238 5 1 3 -14 47.5550 2.41213 2 1 3 -14 48.8966 2.46530 2 -1 -3 14 53.3603 4.73787 3 -1 -3 14 47.1769 4.79262 5 0 3 -14 35.4036 3.94889 2 0 3 -14 36.3405 2.64754 2 0 -3 14 32.2211 4.74342 5 -1 3 -14 41.8373 3.21951 2 1 -3 14 43.0290 4.33846 5 -2 3 -14 52.9342 3.86292 2 2 -3 14 54.4837 4.76807 5 -3 3 -14 1.23647 1.28270 2 3 -3 14 -1.2918 1.29764 5 7 2 -14 11.4549 2.79855 3 -7 -2 14 13.6029 2.64892 3 6 2 -14 0.50147 1.58103 3 -6 -2 14 0.98144 1.34622 3 -6 -2 14 0.39327 1.49981 5 5 2 -14 23.7791 3.84306 3 -5 -2 14 21.2587 3.56231 5 -5 -2 14 31.4380 3.48108 3 4 2 -14 5.09210 2.42403 3 -4 -2 14 6.50821 2.53794 5 -4 -2 14 7.77433 2.41227 3 -3 -2 14 45.2668 9.45453 5 -2 -2 14 33.0050 4.86560 5 1 2 -14 84.5684 3.30969 2 1 2 -14 92.4927 3.55690 2 -1 -2 14 84.5291 6.31064 5 0 2 -14 53.9540 3.27988 2 0 -2 14 46.9253 4.69899 5 -1 2 -14 -0.0965 0.92821 2 1 -2 14 -1.0893 1.26411 5 -2 2 -14 11.1257 2.21459 2 2 -2 14 8.11332 2.20024 5 7 1 -14 6.94119 2.20533 3 6 1 -14 278.943 10.6859 3 5 1 -14 2.96730 1.72672 3 -5 -1 14 -2.4343 1.44775 5 -4 -1 14 13.7271 3.32913 5 -3 -1 14 12.2169 3.13979 5 -2 -1 14 23.2215 5.37187 5 1 1 -14 8.68395 1.38122 2 -1 -1 14 8.60296 2.60867 5 0 1 -14 3.38756 1.13206 2 0 -1 14 3.42907 1.75258 5 -1 1 -14 112.653 5.44706 2 1 -1 14 101.603 6.62947 5 -2 1 -14 34.9194 3.46668 2 2 -1 14 20.4524 3.63160 5 7 0 -14 14.8118 4.56948 3 6 0 -14 117.633 6.63088 3 5 0 -14 4.31675 1.80963 3 -5 0 14 0.24165 1.72968 5 -4 0 14 1.99492 1.86363 5 -3 0 14 24.5493 4.22271 5 -2 0 14 -0.4067 1.21095 5 1 0 -14 184.596 6.13680 2 -1 0 14 196.781 10.2879 5 0 0 -14 86.4124 5.42621 2 -1 0 -14 55.3611 4.04619 2 1 0 14 59.9146 5.47073 5 6 -1 -14 71.9511 5.28371 3 -3 1 14 45.7494 5.45004 5 2 -1 -14 60.2177 3.03825 2 -2 1 14 75.0442 6.23561 5 1 -1 -14 0.29029 0.94295 2 -1 1 14 1.65477 1.58175 5 -3 2 14 108.973 7.84047 4 2 9 -15 0.07642 0.89958 2 1 9 -15 116.427 4.76757 2 0 9 -15 -0.2613 1.20966 2 1 8 -15 149.965 5.20435 2 -1 -8 15 157.674 8.85399 5 0 8 -15 101.600 4.76041 2 0 -8 15 95.2086 6.76963 5 1 -8 15 19.9813 3.53805 5 -5 -7 15 54.7571 6.73724 3 -4 -7 15 20.8670 3.32584 3 -3 -7 15 167.129 8.59456 3 -2 -7 15 111.255 6.93670 3 -2 -7 15 88.5117 6.75140 5 1 7 -15 67.3116 3.08955 2 -1 -7 15 68.5705 6.53083 3 -1 -7 15 61.0482 5.72482 5 0 7 -15 -0.8026 1.13397 2 0 -7 15 0.22211 1.62395 5 -1 7 -15 -1.3421 1.19935 2 1 -7 15 3.63122 1.64197 5 -2 7 -15 1.91572 1.58139 2 -5 -6 15 2.49782 1.93215 3 -4 -6 15 1.26289 1.27021 3 -3 -6 15 101.675 6.39224 3 -3 -6 15 93.8591 7.06480 5 -2 -6 15 1.80668 1.73997 5 -2 -6 15 -0.3803 1.36315 3 1 6 -15 93.2182 3.42290 2 1 6 -15 96.2553 3.43078 2 -1 -6 15 89.9802 6.40981 3 -1 -6 15 90.3718 6.58849 5 0 6 -15 1.94950 1.06896 2 0 6 -15 1.19422 1.01987 2 0 -6 15 1.51736 1.46394 5 1 -6 15 7.72146 3.43389 5 -2 6 -15 25.9242 3.38163 2 2 -6 15 22.0894 3.53747 5 -6 -5 15 5.25969 1.78279 3 -5 -5 15 19.5308 3.48306 3 -4 -5 15 7.44758 1.98834 3 -4 -5 15 5.82832 3.74099 5 -3 -5 15 0.13961 1.62709 5 -3 -5 15 0.97465 1.51983 3 -2 -5 15 11.2767 3.02293 5 -2 -5 15 9.74832 2.42111 3 -1 -5 15 -1.7044 0.97332 3 -1 -5 15 -1.7620 1.72278 5 0 5 -15 5.93450 1.25442 2 0 -5 15 5.99618 2.80374 3 0 -5 15 8.64117 3.57257 5 -1 5 -15 56.5329 4.26468 2 1 -5 15 66.4502 5.91683 5 -2 5 -15 -0.4879 1.00001 2 2 -5 15 1.85679 1.51028 5 -5 -4 15 72.4581 8.09288 3 -4 -4 15 107.090 7.25309 3 -4 -4 15 115.516 9.33251 5 -3 -4 15 41.5960 4.31411 3 -3 -4 15 46.0116 5.15025 5 -2 -4 15 288.430 11.4813 3 -2 -4 15 282.337 12.0654 5 1 4 -15 0.86691 0.74330 2 -1 -4 15 4.70171 1.61258 5 -1 -4 15 1.58969 1.64315 3 0 4 -15 212.542 6.50318 2 0 4 -15 203.892 7.60399 2 -1 4 -15 -2.9901 1.03967 2 1 -4 15 2.36096 1.65815 5 -6 -3 15 3.10878 1.67823 3 -5 -3 15 63.0736 5.65962 3 -4 -3 15 -0.7352 2.27602 5 -4 -3 15 6.65228 3.58801 3 -3 -3 15 118.132 7.14414 3 -3 -3 15 114.709 7.80953 5 -2 -3 15 1.45215 1.86082 5 1 3 -15 37.7589 3.23189 2 1 3 -15 35.2107 2.05832 2 -1 -3 15 37.8456 4.36601 5 0 3 -15 68.3397 3.54991 2 0 3 -15 65.3308 3.38490 2 0 -3 15 58.4449 6.16952 5 -1 3 -15 9.83856 1.87705 2 1 -3 15 7.29495 3.44083 5 -3 -2 15 2.26365 1.66209 5 -2 -2 15 -1.0844 1.82444 5 1 2 -15 77.5899 3.13008 2 1 2 -15 79.2116 3.21558 2 -1 -2 15 76.5527 6.24549 5 0 2 -15 -0.2781 1.05445 2 0 -2 15 2.08344 1.71030 5 -2 -1 15 0.43415 1.75173 5 1 1 -15 2.92977 1.16304 2 -1 -1 15 2.47708 1.93711 5 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 multi-scan _exptl_absorpt_correction_T_max 0.8879 _exptl_absorpt_correction_T_min 0.8426 _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 0.71119 8.804 10.369 11.549 110.423 100.358 101.290 ) ; _shelx_hkl_checksum 9207 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder in NVH oil' _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.73078(10) 0.52426(9) 0.84701(8) 0.02237(17) Uani 1 1 d . . . . . N1 N 0.74390(11) 0.47404(9) 0.64047(8) 0.01603(17) Uani 1 1 d . . . . . N2 N 0.82716(12) 0.05977(10) 0.42947(9) 0.02112(19) Uani 1 1 d . . . . . C1 C 0.74349(13) 0.56575(11) 0.76033(10) 0.0173(2) Uani 1 1 d . . . . . C2 C 0.75926(13) 0.71548(11) 0.77528(10) 0.0174(2) Uani 1 1 d . . . . . C3 C 0.76438(14) 0.81635(12) 0.89579(11) 0.0210(2) Uani 1 1 d . . . . . H3 H 0.753627 0.786422 0.963625 0.025 Uiso 1 1 calc R . . . . C4 C 0.78498(15) 0.95862(12) 0.91587(11) 0.0235(2) Uani 1 1 d . . . . . H4 H 0.788908 1.026822 0.997543 0.028 Uiso 1 1 calc R . . . . C5 C 0.80013(14) 1.00253(12) 0.81541(11) 0.0230(2) Uani 1 1 d . . . . . H5 H 0.814840 1.100780 0.829719 0.028 Uiso 1 1 calc R . . . . C6 C 0.79389(14) 0.90451(11) 0.69592(11) 0.0201(2) Uani 1 1 d . . . . . H6 H 0.803575 0.935713 0.628657 0.024 Uiso 1 1 calc R . . . . C7 C 0.77320(12) 0.75814(11) 0.67319(10) 0.01668(19) Uani 1 1 d . . . . . C8 C 0.76944(13) 0.65276(11) 0.55167(10) 0.01697(19) Uani 1 1 d . . . . . H8 H 0.777267 0.678821 0.481329 0.020 Uiso 1 1 calc R . . . . C9 C 0.75450(12) 0.51522(11) 0.53905(9) 0.01529(19) Uani 1 1 d . . . . . C10 C 0.75095(12) 0.38792(11) 0.42973(10) 0.01554(19) Uani 1 1 d . . . . . C11 C 0.74587(12) 0.27688(11) 0.46663(10) 0.01564(19) Uani 1 1 d . . . . . C12 C 0.73205(12) 0.12733(11) 0.38261(10) 0.01672(19) Uani 1 1 d . . . . . C13 C 0.62305(13) 0.06108(11) 0.26039(10) 0.0207(2) Uani 1 1 d . . . . . H13 H 0.554921 0.110506 0.231158 0.025 Uiso 1 1 calc R . . . . C14 C 0.61615(15) -0.07773(12) 0.18275(11) 0.0252(2) Uani 1 1 d . . . . . H14 H 0.543301 -0.125044 0.099393 0.030 Uiso 1 1 calc R . . . . C15 C 0.71752(16) -0.14650(12) 0.22888(12) 0.0259(2) Uani 1 1 d . . . . . H15 H 0.717529 -0.240742 0.177057 0.031 Uiso 1 1 calc R . . . . C16 C 0.81864(15) -0.07443(12) 0.35223(12) 0.0243(2) Uani 1 1 d . . . . . H16 H 0.885934 -0.122823 0.384057 0.029 Uiso 1 1 calc R . . . . C17 C 0.74352(12) 0.32078(10) 0.60637(10) 0.01599(19) Uani 1 1 d . . . . . C18 C 0.58850(13) 0.23339(12) 0.61678(11) 0.0211(2) Uani 1 1 d . . . . . H18A H 0.584779 0.268219 0.706543 0.032 Uiso 1 1 calc GR . . . . H18B H 0.586303 0.131877 0.586512 0.032 Uiso 1 1 calc GR . . . . H18C H 0.495217 0.244144 0.563959 0.032 Uiso 1 1 calc GR . . . . C19 C 0.89315(13) 0.31252(11) 0.69210(10) 0.0187(2) Uani 1 1 d . . . . . H19A H 0.990213 0.364708 0.679576 0.028 Uiso 1 1 calc GR . . . . H19B H 0.892177 0.211825 0.669234 0.028 Uiso 1 1 calc GR . . . . H19C H 0.892670 0.355765 0.782258 0.028 Uiso 1 1 calc GR . . . . C20 C 0.75242(12) 0.38917(10) 0.30232(9) 0.01570(19) Uani 1 1 d . . . . . C21 C 0.85568(13) 0.32896(11) 0.23497(10) 0.0174(2) Uani 1 1 d . . . . . H21 H 0.926810 0.286638 0.271509 0.021 Uiso 1 1 calc R . . . . C22 C 0.85506(14) 0.33055(11) 0.11488(10) 0.0216(2) Uani 1 1 d . . . . . H22 H 0.926809 0.290648 0.070462 0.026 Uiso 1 1 calc R . . . . C23 C 0.74980(16) 0.39035(12) 0.05956(11) 0.0255(2) Uani 1 1 d . . . . . H23 H 0.749187 0.391239 -0.022552 0.031 Uiso 1 1 calc R . . . . C24 C 0.64568(15) 0.44870(12) 0.12536(11) 0.0253(2) Uani 1 1 d . . . . . H24 H 0.572379 0.488224 0.087326 0.030 Uiso 1 1 calc R . . . . C25 C 0.64772(14) 0.44979(11) 0.24624(10) 0.0203(2) Uani 1 1 d . . . . . H25 H 0.577585 0.491974 0.291153 0.024 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 O1 0.0322(4) 0.0218(4) 0.0194(4) 0.0112(3) 0.0116(3) 0.0114(3) N1 0.0204(4) 0.0142(4) 0.0159(4) 0.0070(3) 0.0064(3) 0.0068(3) N2 0.0265(5) 0.0178(4) 0.0218(4) 0.0082(4) 0.0081(4) 0.0103(4) C1 0.0195(5) 0.0175(5) 0.0169(5) 0.0072(4) 0.0066(4) 0.0073(4) C2 0.0201(5) 0.0162(5) 0.0174(5) 0.0065(4) 0.0064(4) 0.0071(4) C3 0.0256(5) 0.0203(5) 0.0180(5) 0.0068(4) 0.0081(4) 0.0080(4) C4 0.0299(6) 0.0188(5) 0.0195(5) 0.0038(4) 0.0080(4) 0.0077(4) C5 0.0284(6) 0.0154(5) 0.0235(5) 0.0059(4) 0.0074(4) 0.0059(4) C6 0.0243(5) 0.0164(5) 0.0212(5) 0.0085(4) 0.0069(4) 0.0069(4) C7 0.0172(4) 0.0157(4) 0.0173(5) 0.0062(4) 0.0044(4) 0.0059(4) C8 0.0205(5) 0.0160(5) 0.0161(4) 0.0075(4) 0.0052(4) 0.0065(4) C9 0.0160(4) 0.0161(4) 0.0147(4) 0.0065(4) 0.0043(3) 0.0058(3) C10 0.0164(4) 0.0155(4) 0.0150(4) 0.0059(4) 0.0038(4) 0.0057(4) C11 0.0164(4) 0.0155(4) 0.0156(4) 0.0062(4) 0.0046(4) 0.0054(3) C12 0.0197(5) 0.0143(4) 0.0176(5) 0.0068(4) 0.0075(4) 0.0048(4) C13 0.0221(5) 0.0178(5) 0.0200(5) 0.0068(4) 0.0047(4) 0.0031(4) C14 0.0293(6) 0.0180(5) 0.0213(5) 0.0037(4) 0.0064(4) -0.0003(4) C15 0.0363(6) 0.0155(5) 0.0265(6) 0.0059(4) 0.0158(5) 0.0066(4) C16 0.0328(6) 0.0182(5) 0.0284(6) 0.0109(4) 0.0146(5) 0.0124(4) C17 0.0198(5) 0.0133(4) 0.0167(4) 0.0066(4) 0.0064(4) 0.0060(4) C18 0.0225(5) 0.0194(5) 0.0231(5) 0.0097(4) 0.0090(4) 0.0043(4) C19 0.0228(5) 0.0172(5) 0.0174(5) 0.0078(4) 0.0044(4) 0.0076(4) C20 0.0182(4) 0.0129(4) 0.0141(4) 0.0051(3) 0.0024(4) 0.0027(3) C21 0.0196(5) 0.0147(4) 0.0161(5) 0.0052(4) 0.0038(4) 0.0036(4) C22 0.0269(5) 0.0172(5) 0.0162(5) 0.0037(4) 0.0062(4) 0.0015(4) C23 0.0380(6) 0.0195(5) 0.0138(5) 0.0067(4) 0.0018(4) 0.0013(5) C24 0.0337(6) 0.0192(5) 0.0196(5) 0.0091(4) -0.0025(4) 0.0062(4) C25 0.0234(5) 0.0173(5) 0.0189(5) 0.0067(4) 0.0019(4) 0.0069(4) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C9 124.06(9) . . ? C1 N1 C17 124.06(8) . . ? C9 N1 C17 111.77(8) . . ? C16 N2 C12 117.36(10) . . ? O1 C1 N1 122.02(9) . . ? O1 C1 C2 123.40(9) . . ? N1 C1 C2 114.58(9) . . ? C3 C2 C1 117.99(9) . . ? C3 C2 C7 120.53(9) . . ? C7 C2 C1 121.46(9) . . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.15(10) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 120.1 . . ? C3 C4 C5 119.85(10) . . ? C5 C4 H4 120.1 . . ? C4 C5 H5 119.6 . . ? C6 C5 C4 120.76(10) . . ? C6 C5 H5 119.6 . . ? C5 C6 H6 119.8 . . ? C5 C6 C7 120.38(10) . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 118.32(9) . . ? C2 C7 C8 119.16(9) . . ? C6 C7 C8 122.50(9) . . ? C7 C8 H8 120.6 . . ? C9 C8 C7 118.80(9) . . ? C9 C8 H8 120.6 . . ? N1 C9 C10 107.24(8) . . ? C8 C9 N1 121.92(9) . . ? C8 C9 C10 130.82(9) . . ? C9 C10 C20 122.63(9) . . ? C11 C10 C9 108.94(9) . . ? C11 C10 C20 128.43(9) . . ? C10 C11 C12 125.89(9) . . ? C10 C11 C17 111.62(9) . . ? C12 C11 C17 122.34(9) . . ? N2 C12 C11 117.10(9) . . ? N2 C12 C13 122.52(9) . . ? C13 C12 C11 120.38(9) . . ? C12 C13 H13 120.5 . . ? C14 C13 C12 118.93(10) . . ? C14 C13 H13 120.5 . . ? C13 C14 H14 120.6 . . ? C13 C14 C15 118.85(11) . . ? C15 C14 H14 120.6 . . ? C14 C15 H15 120.8 . . ? C16 C15 C14 118.41(10) . . ? C16 C15 H15 120.8 . . ? N2 C16 C15 123.86(11) . . ? N2 C16 H16 118.1 . . ? C15 C16 H16 118.1 . . ? N1 C17 C11 100.31(8) . . ? N1 C17 C18 110.87(8) . . ? N1 C17 C19 109.89(8) . . ? C11 C17 C18 110.49(9) . . ? C11 C17 C19 113.37(8) . . ? C18 C17 C19 111.42(9) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C10 121.26(9) . . ? C21 C20 C25 118.79(9) . . ? C25 C20 C10 119.95(9) . . ? C20 C21 H21 119.7 . . ? C22 C21 C20 120.51(10) . . ? C22 C21 H21 119.7 . . ? C21 C22 H22 119.9 . . ? C21 C22 C23 120.28(10) . . ? C23 C22 H22 119.9 . . ? C22 C23 H23 120.3 . . ? C24 C23 C22 119.43(10) . . ? C24 C23 H23 120.3 . . ? C23 C24 H24 119.7 . . ? C25 C24 C23 120.58(10) . . ? C25 C24 H24 119.7 . . ? C20 C25 H25 119.8 . . ? C24 C25 C20 120.40(10) . . ? C24 C25 H25 119.8 . . ? 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 O1 C1 1.2327(13) . ? N1 C1 1.3789(13) . ? N1 C9 1.3903(13) . ? N1 C17 1.4948(12) . ? N2 C12 1.3460(13) . ? N2 C16 1.3422(14) . ? C1 C2 1.4741(14) . ? C2 C3 1.4044(14) . ? C2 C7 1.4116(14) . ? C3 H3 0.9500 . ? C3 C4 1.3780(15) . ? C4 H4 0.9500 . ? C4 C5 1.4032(16) . ? C5 H5 0.9500 . ? C5 C6 1.3816(15) . ? C6 H6 0.9500 . ? C6 C7 1.4129(14) . ? C7 C8 1.4351(14) . ? C8 H8 0.9500 . ? C8 C9 1.3572(14) . ? C9 C10 1.4625(14) . ? C10 C11 1.3541(14) . ? C10 C20 1.4775(14) . ? C11 C12 1.4793(14) . ? C11 C17 1.5207(14) . ? C12 C13 1.4000(15) . ? C13 H13 0.9500 . ? C13 C14 1.3855(15) . ? C14 H14 0.9500 . ? C14 C15 1.3883(18) . ? C15 H15 0.9500 . ? C15 C16 1.3849(18) . ? C16 H16 0.9500 . ? C17 C18 1.5314(15) . ? C17 C19 1.5339(14) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.3983(14) . ? C20 C25 1.3986(14) . ? C21 H21 0.9500 . ? C21 C22 1.3909(15) . ? C22 H22 0.9500 . ? C22 C23 1.3912(17) . ? C23 H23 0.9500 . ? C23 C24 1.3882(18) . ? C24 H24 0.9500 . ? C24 C25 1.3882(16) . ? C25 H25 0.9500 . ?