#------------------------------------------------------------------------------ #$Date: 2020-10-04 05:50:44 +0300 (Sun, 04 Oct 2020) $ #$Revision: 257006 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/75/4517520.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_4517520 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_issue 7 _journal_name_full 'ACS Catalysis' _journal_page_first 4444 _journal_page_last 4450 _journal_paper_doi 10.1021/acscatal.9b05413 _journal_volume 10 _journal_year 2020 _chemical_formula_moiety 'C22 H20 N2 O' _chemical_formula_sum 'C22 H20 N2 O' _chemical_formula_weight 328.40 _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 2019-02-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 105.947(4) _cell_angle_beta 96.819(4) _cell_angle_gamma 97.151(4) _cell_formula_units_Z 2 _cell_length_a 9.0581(12) _cell_length_b 9.9273(12) _cell_length_c 10.2645(12) _cell_measurement_reflns_used 1492 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 25.84 _cell_measurement_theta_min 2.85 _cell_volume 869.20(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 100.0 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_unetI/netI 0.0172 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 24237 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.756 _diffrn_reflns_theta_min 2.296 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_T_max 0.8879 _exptl_absorpt_correction_T_min 0.8417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0919 before and 0.0406 after correction. The Ratio of minimum to maximum transmission is 0.9480. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.255 _exptl_crystal_description block _exptl_crystal_F_000 348 _exptl_crystal_recrystallization_method 'The material was recrystallised from --- by as supplied' _exptl_crystal_size_max 0.346 _exptl_crystal_size_mid 0.235 _exptl_crystal_size_min 0.178 _refine_diff_density_max 0.429 _refine_diff_density_min -0.187 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 229 _refine_ls_number_reflns 4505 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0409 _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^)+(0.0508P)^2^+0.3749P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1051 _refine_ls_wR_factor_ref 0.1077 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4180 _reflns_number_total 4505 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs9b05413_si_004.cif _cod_data_source_block 0577_cg_0m _cod_depositor_comments ;Adding full bibliography for 4517519--4517521.cif. Adding full bibliography for 4517519--4517521.cif. ; _cod_database_code 4517520 _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 0.986 _shelx_estimated_absorpt_t_min 0.974 _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: C2(H2), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21) 2.b Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C) ; _shelx_res_file ; TITL 0577_cg_0m_a.res in P-1 0577_cg_0m.res created by SHELXL-2018/3 at 10:29:10 on 21-Feb-2019 REM Old TITL 0577_CG_0m in P-1 REM SHELXT solution in P-1 REM R1 0.153, Rweak 0.008, Alpha 0.042, Orientation as input REM Formula found by SHELXT: C22 N2 O CELL 0.71073 9.0581 9.9273 10.2645 105.947 96.819 97.151 ZERR 2 0.0012 0.0012 0.0012 0.004 0.004 0.004 LATT 1 SFAC C H N O UNIT 44 40 4 2 L.S. 4 0 0 PLAN 20 SIZE 0.178 0.235 0.346 TEMP -173.15 BOND $H list 4 fmap 2 53 acta OMIT -6 3 0 REM REM REM WGHT 0.050800 0.374900 FVAR 1.36325 O1 4 0.098861 0.073330 0.280629 11.00000 0.02527 0.01789 = 0.02250 0.00325 0.00366 -0.00016 N1 3 0.188041 0.311753 0.372861 11.00000 0.01823 0.01628 = 0.01548 0.00507 0.00355 0.00116 N2 3 0.352296 0.547932 0.098876 11.00000 0.02361 0.02132 = 0.01983 0.00845 0.00725 0.00500 C1 1 0.140215 0.176880 0.383700 11.00000 0.01677 0.01703 = 0.02150 0.00614 0.00421 0.00167 C2 1 0.142933 0.171997 0.523232 11.00000 0.02006 0.01811 = 0.02218 0.00887 0.00475 0.00131 AFIX 43 H2 2 0.114633 0.082701 0.538170 11.00000 -1.20000 AFIX 0 C3 1 0.184171 0.289384 0.634881 11.00000 0.01867 0.02099 = 0.01946 0.00902 0.00506 0.00349 C4 1 0.228625 0.423981 0.615011 11.00000 0.02083 0.01741 = 0.01746 0.00548 0.00402 0.00261 AFIX 43 H4 2 0.257196 0.507129 0.691064 11.00000 -1.20000 AFIX 0 C5 1 0.229232 0.430744 0.484326 11.00000 0.01610 0.01613 = 0.01778 0.00503 0.00348 0.00222 C6 1 0.270694 0.551652 0.433427 11.00000 0.01667 0.01684 = 0.01801 0.00650 0.00411 0.00239 C7 1 0.257890 0.505224 0.295686 11.00000 0.01631 0.01687 = 0.01858 0.00615 0.00395 0.00295 C8 1 0.277727 0.594930 0.203580 11.00000 0.01731 0.01807 = 0.01580 0.00577 0.00223 0.00158 C9 1 0.218065 0.721159 0.224244 11.00000 0.02079 0.01989 = 0.01783 0.00485 0.00302 0.00413 AFIX 43 H9 2 0.165405 0.751545 0.298975 11.00000 -1.20000 AFIX 0 C10 1 0.236700 0.801182 0.134511 11.00000 0.02462 0.01833 = 0.02143 0.00619 -0.00012 0.00343 AFIX 43 H10 2 0.196230 0.886742 0.145988 11.00000 -1.20000 AFIX 0 C11 1 0.315682 0.754076 0.027344 11.00000 0.02409 0.02142 = 0.02025 0.00965 0.00156 0.00057 AFIX 43 H11 2 0.331533 0.807219 -0.035338 11.00000 -1.20000 AFIX 0 C12 1 0.370757 0.627863 0.014028 11.00000 0.02356 0.02406 = 0.01941 0.00879 0.00679 0.00323 AFIX 43 H12 2 0.424731 0.596042 -0.059433 11.00000 -1.20000 AFIX 0 C13 1 0.204733 0.345434 0.241661 11.00000 0.01943 0.01759 = 0.01499 0.00560 0.00385 0.00164 C14 1 0.320233 0.263489 0.171042 11.00000 0.02591 0.01917 = 0.02092 0.00593 0.00904 0.00496 AFIX 137 H14A 2 0.417993 0.290965 0.231542 11.00000 -1.50000 H14B 2 0.330353 0.285833 0.084950 11.00000 -1.50000 H14C 2 0.286194 0.161279 0.151485 11.00000 -1.50000 AFIX 0 C15 1 0.052255 0.312522 0.147201 11.00000 0.02204 0.02634 = 0.01970 0.00840 0.00014 -0.00039 AFIX 137 H15A 2 0.014388 0.210338 0.120841 11.00000 -1.50000 H15B 2 0.064632 0.341490 0.064717 11.00000 -1.50000 H15C 2 -0.019732 0.364697 0.195657 11.00000 -1.50000 AFIX 0 C16 1 0.318218 0.697612 0.526434 11.00000 0.01977 0.01575 = 0.01593 0.00660 0.00213 0.00272 C17 1 0.456214 0.777125 0.525285 11.00000 0.01854 0.01993 = 0.02014 0.00760 0.00339 0.00348 AFIX 43 H17 2 0.520711 0.737596 0.463772 11.00000 -1.20000 AFIX 0 C18 1 0.499406 0.913933 0.613912 11.00000 0.02011 0.01930 = 0.02653 0.00852 -0.00001 0.00004 AFIX 43 H18 2 0.593926 0.967271 0.613527 11.00000 -1.20000 AFIX 0 C19 1 0.405137 0.973034 0.702991 11.00000 0.02722 0.01693 = 0.02373 0.00379 -0.00055 0.00360 AFIX 43 H19 2 0.434947 1.066796 0.763134 11.00000 -1.20000 AFIX 0 C20 1 0.266937 0.894955 0.704220 11.00000 0.02718 0.02057 = 0.02150 0.00527 0.00618 0.00701 AFIX 43 H20 2 0.201900 0.935500 0.764655 11.00000 -1.20000 AFIX 0 C21 1 0.224343 0.757478 0.616765 11.00000 0.02104 0.01904 = 0.02097 0.00717 0.00539 0.00292 AFIX 43 H21 2 0.130521 0.703809 0.618501 11.00000 -1.20000 AFIX 0 C22 1 0.185492 0.279284 0.778413 11.00000 0.03261 0.02524 = 0.02078 0.01042 0.00610 0.00366 AFIX 137 H22A 2 0.135584 0.184652 0.774968 11.00000 -1.50000 H22B 2 0.131852 0.351333 0.829097 11.00000 -1.50000 H22C 2 0.289904 0.295281 0.824781 11.00000 -1.50000 AFIX 0 HKLF 4 REM 0577_cg_0m_a.res in P-1 REM wR2 = 0.107685, GooF = S = 1.03572, Restrained GooF = 1.03572 for all data REM R1 = 0.040860 for 4180 Fo > 4sig(Fo) and 0.043713 for all 4505 data REM 229 parameters refined using 0 restraints END WGHT 0.0508 0.3749 REM Highest difference peak 0.429, deepest hole -0.187, 1-sigma level 0.048 Q1 1 0.1430 0.1783 0.4586 11.00000 0.05 0.43 Q2 1 0.2351 0.4232 0.2637 11.00000 0.05 0.39 Q3 1 0.2568 0.3040 0.2040 11.00000 0.05 0.37 Q4 1 0.1811 0.2809 0.6996 11.00000 0.05 0.35 Q5 1 0.2347 0.5375 0.3619 11.00000 0.05 0.32 Q6 1 0.1342 0.3225 0.1850 11.00000 0.05 0.32 Q7 1 0.2595 0.6644 0.2183 11.00000 0.05 0.32 Q8 1 0.2772 0.7774 0.0823 11.00000 0.05 0.31 Q9 1 0.2023 0.3573 0.6238 11.00000 0.05 0.31 Q10 1 0.2107 0.4208 0.5470 11.00000 0.05 0.30 Q11 1 0.1500 0.2379 0.5749 11.00000 0.05 0.30 Q12 1 0.2932 0.6268 0.4804 11.00000 0.05 0.29 Q13 1 0.4831 0.8431 0.5751 11.00000 0.05 0.29 Q14 1 0.2436 0.4991 0.4641 11.00000 0.05 0.28 Q15 1 0.4334 0.9409 0.6429 11.00000 0.05 0.28 Q16 1 0.2610 0.7272 0.5614 11.00000 0.05 0.28 Q17 1 0.2751 0.5565 0.2570 11.00000 0.05 0.27 Q18 1 0.2237 0.3647 0.4334 11.00000 0.05 0.27 Q19 1 0.3241 0.5792 0.1558 11.00000 0.05 0.25 Q20 1 0.2274 0.6411 0.2013 11.00000 0.05 0.25 ; _shelx_res_checksum 76598 _shelx_hkl_file ; -1 0 0 5.55756 0.41288 2 -1 0 0 5.74533 0.43427 4 1 0 0 5.56549 0.38969 7 -3 0 0 957.470 20.9833 7 -3 0 0 944.431 21.0776 2 -3 0 0 936.930 21.0282 4 3 0 0 1008.05 20.9994 7 3 0 0 934.178 21.0685 4 3 0 0 939.703 21.0645 2 3 0 0 934.218 21.1028 2 -4 0 0 725.142 16.7694 2 -4 0 0 735.399 16.6428 7 -4 0 0 731.296 16.6930 4 -4 0 0 749.982 16.7749 2 4 0 0 725.805 17.3739 7 4 0 0 742.496 16.7659 2 4 0 0 717.473 16.8017 2 4 0 0 748.995 16.7919 4 -5 0 0 43.6796 1.93555 7 -5 0 0 42.1437 1.98500 2 -5 0 0 42.5637 2.05963 2 -5 0 0 40.7196 1.97352 4 5 0 0 46.7697 1.96047 7 5 0 0 37.9632 1.94877 4 5 0 0 39.5425 1.99385 2 5 0 0 46.3327 2.12019 2 -7 0 0 267.867 7.78682 2 -7 0 0 270.849 7.58193 7 -7 0 0 275.492 7.68190 2 7 0 0 293.886 7.51744 7 7 0 0 248.673 7.64274 4 7 0 0 288.669 7.79283 2 -8 0 0 26.4566 1.96706 7 -8 0 0 23.5687 2.09960 2 -8 0 0 29.8947 2.16367 2 8 0 0 31.0016 2.07861 7 8 0 0 28.8445 2.30332 2 8 0 0 24.7090 2.07857 2 -9 0 0 28.4792 2.45536 2 -9 0 0 23.3051 2.14354 7 -9 0 0 23.7351 2.82314 2 9 0 0 30.7636 2.43745 2 9 0 0 25.8053 2.07504 7 9 0 0 23.0731 2.30027 4 9 0 0 26.1215 2.47560 2 -10 0 0 0.02747 0.94325 7 -10 0 0 1.17183 1.20093 2 -10 0 0 4.09030 1.29458 2 10 0 0 0.62237 1.01212 4 10 0 0 0.81581 1.08370 2 -11 0 0 29.5128 2.66005 2 -11 0 0 25.5738 2.84809 2 11 0 0 32.7595 2.88097 2 -12 0 0 4.55157 1.48796 2 12 0 0 4.24805 1.62919 2 12 -1 0 52.5637 3.73482 2 -12 1 0 56.3494 3.81714 2 -12 1 0 57.1153 4.73529 2 11 -1 0 43.5538 2.84337 7 11 -1 0 44.9183 3.37545 2 11 -1 0 47.9836 3.49135 2 -11 1 0 46.4112 3.41437 2 10 -1 0 24.5128 2.48561 2 10 -1 0 26.4450 2.67299 2 10 -1 0 25.4649 2.22726 7 10 -1 0 27.1060 2.50456 4 -10 1 0 23.3429 2.54024 2 -10 1 0 27.0958 2.47237 2 9 -1 0 99.9221 4.36477 2 9 -1 0 96.8285 4.28702 2 9 -1 0 95.2615 3.94985 7 9 -1 0 99.3722 4.37812 4 -9 1 0 95.2723 4.31667 2 -9 1 0 96.9865 4.19877 2 -9 1 0 98.9325 4.03201 7 8 -1 0 120.917 4.65376 4 8 -1 0 123.301 4.69866 2 8 -1 0 121.318 4.66654 2 8 -1 0 126.358 4.36405 7 -8 1 0 121.111 4.56351 2 -8 1 0 115.576 4.29893 7 -8 1 0 123.533 4.67699 2 7 -1 0 653.947 16.0733 2 7 -1 0 660.320 16.1575 4 7 -1 0 673.825 15.7739 7 7 -1 0 649.190 16.1475 2 -7 1 0 665.608 15.9734 7 -7 1 0 672.896 16.0536 4 -7 1 0 650.869 16.1434 2 -7 1 0 655.967 16.0745 2 6 -1 0 93.0697 3.51199 2 6 -1 0 96.3161 3.31782 7 6 -1 0 95.2393 3.52855 4 -6 1 0 100.595 3.54209 4 -6 1 0 94.4261 3.32161 7 -6 1 0 89.2406 3.47852 2 -6 1 0 92.2722 3.48652 2 5 -1 0 1872.35 41.9312 4 5 -1 0 1903.87 41.9474 2 5 -1 0 1940.03 41.7001 7 5 -1 0 1871.21 41.9640 2 -5 1 0 1907.53 41.9514 2 -5 1 0 1875.40 41.9545 2 -5 1 0 1924.78 41.7375 7 -5 1 0 1916.48 41.8772 4 4 -1 0 2782.39 60.3042 2 4 -1 0 2722.26 60.2833 4 4 -1 0 2723.33 60.5326 7 4 -1 0 2747.08 60.3158 2 -4 1 0 2767.40 60.3086 2 -4 1 0 2859.81 60.2870 4 -4 1 0 2801.39 60.3252 2 -4 1 0 2822.02 60.1273 7 3 -1 0 7.02682 0.78092 2 3 -1 0 6.56401 0.80534 2 -3 1 0 7.61746 0.76527 2 -3 1 0 6.81991 0.75475 4 -3 1 0 5.76654 0.74078 2 1 -1 0 41.6651 1.22479 2 1 -1 0 42.3299 1.18455 7 1 -1 0 40.6341 1.20807 2 1 -1 0 40.9355 1.19599 4 -1 1 0 41.7426 1.19944 4 -1 1 0 42.8014 1.22567 2 -1 1 0 41.2749 1.21389 2 -1 1 0 44.7476 1.18404 7 1 1 0 7.10808 0.44289 6 1 1 0 6.45289 0.42662 2 -2 -1 0 190.980 4.69277 2 -2 -1 0 197.716 4.65884 7 -2 -1 0 191.839 4.63767 2 -2 -1 0 196.268 4.60637 4 2 1 0 193.051 4.66432 2 2 1 0 194.259 4.68982 2 2 1 0 186.912 4.65074 4 -3 -1 0 3697.78 116.432 1 -4 -1 0 46.5978 1.98835 2 -4 -1 0 42.7761 1.82223 2 -4 -1 0 44.9367 2.20055 4 -4 -1 0 42.9229 1.81997 7 4 1 0 42.9590 1.84522 4 4 1 0 42.9223 1.89451 2 4 1 0 46.4652 1.78774 7 4 1 0 43.1684 1.89085 2 -5 -1 0 33.6380 1.73872 2 -5 -1 0 35.0205 1.76752 4 -5 -1 0 33.3198 1.74596 7 -5 -1 0 34.5293 1.87403 2 5 1 0 31.9259 1.74373 4 5 1 0 32.8854 1.81451 2 5 1 0 34.1567 1.67717 7 5 1 0 33.5671 1.83986 2 -6 -1 0 50.3217 2.32726 7 -6 -1 0 49.8972 2.49974 2 -6 -1 0 53.4332 2.37978 2 6 1 0 48.9553 2.38453 2 6 1 0 51.1387 2.28549 7 6 1 0 46.5928 2.39132 2 6 1 0 50.4413 2.38243 4 -7 -1 0 5.19358 1.17269 2 -7 -1 0 3.88325 0.98190 7 -7 -1 0 5.55116 1.11025 2 7 1 0 4.53682 1.10635 4 7 1 0 5.68793 1.17325 2 7 1 0 3.27048 1.17684 2 -8 -1 0 38.6917 2.64987 2 -8 -1 0 39.9034 2.42899 7 -8 -1 0 41.7596 2.48422 2 8 1 0 40.0581 2.63530 2 8 1 0 43.1183 2.60966 4 8 1 0 40.8575 2.59170 2 -9 -1 0 45.7897 3.09855 2 -9 -1 0 49.7880 2.93620 7 -9 -1 0 49.9639 2.90518 2 9 1 0 50.0192 3.05303 2 9 1 0 55.5736 3.21794 2 9 1 0 54.5400 3.13631 4 -10 -1 0 105.863 4.58567 7 -10 -1 0 104.481 4.43614 2 10 1 0 103.251 4.68871 2 10 1 0 113.162 4.95039 2 10 1 0 105.458 4.69467 4 -11 -1 0 43.0389 3.05087 2 -11 -1 0 52.0702 3.60734 2 11 1 0 40.2031 2.93797 6 11 1 0 46.1648 3.28300 2 12 -2 0 95.9583 4.52944 7 12 -2 0 93.8030 5.04109 2 -12 2 0 100.735 6.62892 2 -12 2 0 92.0606 4.78627 2 11 -2 0 73.8717 4.23663 2 11 -2 0 73.3288 5.21579 2 11 -2 0 73.4562 3.70602 7 -11 2 0 65.7869 4.76732 7 -11 2 0 73.4729 4.04386 2 -11 2 0 72.9336 4.18322 2 10 -2 0 34.7632 2.84809 2 10 -2 0 33.3931 2.98071 2 10 -2 0 29.1495 2.41219 7 10 -2 0 31.0147 2.70711 4 -10 2 0 24.1081 2.62161 7 -10 2 0 32.2852 2.73627 2 -10 2 0 26.1807 2.68098 2 9 -2 0 4.22308 1.22366 7 9 -2 0 3.30189 1.29007 4 9 -2 0 3.18938 1.31830 2 9 -2 0 4.99677 1.24231 2 -9 2 0 4.82742 1.19478 7 -9 2 0 3.83016 1.27940 2 8 -2 0 1358.51 31.6401 2 8 -2 0 1396.87 31.2378 7 8 -2 0 1366.63 31.7140 2 8 -2 0 1369.41 31.7150 4 -8 2 0 1362.00 31.6568 2 -8 2 0 1346.34 31.2216 7 -8 2 0 1401.96 31.7517 4 -8 2 0 1363.34 31.6864 2 7 -2 0 40.3406 2.51338 4 7 -2 0 48.3065 2.73443 2 7 -2 0 45.5826 2.57394 2 7 -2 0 47.5625 2.43084 7 -7 2 0 44.9118 2.55929 4 -7 2 0 46.9607 2.56413 2 -7 2 0 46.6567 2.59983 2 -7 2 0 42.8245 2.53760 7 6 -2 0 3976.07 84.3578 7 6 -2 0 3834.32 84.6350 2 6 -2 0 3895.48 84.6524 2 6 -2 0 3819.70 84.6755 4 -6 2 0 3908.00 84.3245 7 -6 2 0 3978.85 84.6090 4 -6 2 0 3886.38 84.6852 2 -6 2 0 3832.41 84.6102 2 5 -2 0 1969.20 41.8660 7 5 -2 0 1877.36 42.0577 2 5 -2 0 1891.69 42.0881 4 -5 2 0 1942.64 41.8389 7 -5 2 0 1917.32 42.0796 2 -5 2 0 1901.59 42.0247 4 -5 2 0 1840.26 42.2246 2 4 -2 0 1399.89 33.0084 7 4 -2 0 1500.36 32.7548 2 4 -2 0 1462.61 32.6774 2 4 -2 0 1448.28 32.6635 4 -4 2 0 1511.43 32.7140 4 -4 2 0 1521.97 32.5093 7 -4 2 0 1503.34 32.7069 2 -4 2 0 1484.52 32.7492 2 3 -2 0 6050.21 186.219 1 -3 2 0 7527.44 207.292 1 2 -2 0 125.315 3.28151 4 2 -2 0 131.368 3.25231 7 2 -2 0 119.932 3.28040 2 2 -2 0 122.991 3.31547 2 -2 2 0 121.063 3.25331 4 -2 2 0 123.420 3.18671 7 -2 2 0 125.815 3.29506 2 -2 2 0 123.183 3.31348 2 1 -2 0 1493.21 34.6759 3 -1 2 0 1654.92 34.5011 3 -1 2 0 1579.26 34.3892 2 -1 2 0 1648.19 34.2983 4 0 -2 0 5057.45 125.005 1 -1 -2 0 350.200 7.83124 2 -1 -2 0 338.281 7.74124 2 -1 -2 0 330.020 8.06519 6 1 2 0 366.665 8.11113 3 1 2 0 355.344 7.82683 6 1 2 0 340.213 7.76596 2 -2 -2 0 2075.10 44.5198 2 2 2 0 2046.48 44.4587 2 -3 -2 0 137.710 3.82546 2 -3 -2 0 144.356 3.82218 7 3 2 0 133.037 3.65371 4 3 2 0 133.781 3.77230 2 3 2 0 140.285 3.77615 2 3 2 0 136.992 3.71708 6 -4 -2 0 1012.99 23.0367 2 -4 -2 0 1027.60 22.8824 7 -4 -2 0 1007.32 22.7148 2 4 2 0 1004.82 22.7246 4 4 2 0 1034.40 22.8295 2 4 2 0 1028.41 22.9444 2 -5 -2 0 239.074 6.33931 2 -5 -2 0 238.493 6.46335 7 5 2 0 237.909 6.41761 2 5 2 0 241.285 6.35420 6 5 2 0 239.082 6.55980 2 5 2 0 242.122 6.40425 4 -6 -2 0 21.9389 2.07491 7 -6 -2 0 26.2056 1.92960 2 -6 -2 0 28.6277 1.75180 2 6 2 0 26.0551 1.83882 2 6 2 0 28.5840 1.76738 4 6 2 0 26.2778 1.71865 6 -7 -2 0 193.633 5.80776 2 -7 -2 0 196.622 5.97846 7 -7 -2 0 189.125 6.11507 2 7 2 0 187.249 5.90504 4 7 2 0 198.381 5.84156 6 7 2 0 191.557 6.04231 2 7 2 0 193.433 6.11932 2 -8 -2 0 354.181 11.4358 2 -8 -2 0 324.597 9.51720 2 -8 -2 0 323.531 9.33943 7 8 2 0 338.716 9.37011 4 8 2 0 335.351 9.32405 2 8 2 0 342.478 9.65827 2 8 2 0 336.256 9.22731 6 -9 -2 0 310.929 9.20785 7 -9 -2 0 318.327 9.46892 2 -9 -2 0 312.805 8.93086 2 9 2 0 315.168 9.20066 4 9 2 0 316.622 9.14408 2 9 2 0 323.396 9.55054 2 9 2 0 295.680 11.2762 6 -10 -2 0 2.89918 1.12037 2 -10 -2 0 3.84798 1.21363 7 -10 -2 0 1.10640 1.19437 2 10 2 0 2.25743 1.11818 6 10 2 0 1.76486 1.19317 2 10 2 0 2.86995 1.32611 2 10 2 0 2.84614 1.26816 4 -11 -2 0 72.0861 4.06723 2 -11 -2 0 68.3220 4.77553 2 11 2 0 67.6081 3.67188 6 11 2 0 68.3614 3.90832 2 12 -3 0 392.705 11.3211 7 12 -3 0 399.377 12.0729 2 -12 3 0 380.153 11.9921 2 -12 3 0 391.799 11.9008 2 11 -3 0 22.9980 2.74205 2 11 -3 0 20.9618 2.46080 7 11 -3 0 24.5068 3.03187 2 -11 3 0 28.0325 2.85397 2 -11 3 0 22.6967 3.62401 7 -11 3 0 21.6813 2.67627 2 10 -3 0 1799.66 43.3366 4 10 -3 0 1913.05 42.7068 7 10 -3 0 1900.05 43.3745 2 10 -3 0 1872.16 43.3277 2 -10 3 0 1883.56 43.3200 2 -10 3 0 1883.51 43.3345 2 -10 3 0 1905.65 44.7028 7 9 -3 0 22.1159 2.22928 7 9 -3 0 24.5907 2.37742 2 9 -3 0 23.0050 2.34361 4 -9 3 0 24.1029 2.38451 2 -9 3 0 20.5561 2.05844 7 -9 3 0 18.5093 2.23225 2 8 -3 0 3177.62 70.1020 2 8 -3 0 3192.48 70.0072 4 8 -3 0 3262.02 69.5378 7 8 -3 0 3226.51 70.0285 2 -8 3 0 3189.81 71.0085 2 -8 3 0 3163.11 69.4314 7 -8 3 0 3171.33 70.0231 2 -8 3 0 2931.26 72.6982 4 7 -3 0 711.325 17.5212 2 7 -3 0 719.886 17.6366 2 7 -3 0 719.319 17.5847 4 7 -3 0 731.459 17.2436 7 -7 3 0 730.967 17.1965 7 -7 3 0 736.219 17.5137 4 -7 3 0 718.470 17.5274 2 -7 3 0 721.936 17.6273 2 6 -3 0 339.597 8.47504 7 6 -3 0 347.238 8.81954 2 6 -3 0 325.698 8.66630 2 6 -3 0 285.099 9.61806 4 -6 3 0 328.564 8.77084 2 -6 3 0 314.842 8.58766 4 -6 3 0 322.207 8.31962 7 -6 3 0 318.586 8.60533 2 5 -3 0 2204.90 47.7401 7 5 -3 0 2210.18 47.9744 2 5 -3 0 2205.26 48.0736 2 5 -3 0 2176.79 47.9496 4 -5 3 0 2085.51 48.7069 2 -5 3 0 2161.58 47.9227 2 -5 3 0 2173.69 47.6448 7 -5 3 0 2212.46 47.9258 4 4 -3 0 667.933 15.7206 4 4 -3 0 697.550 15.6483 7 4 -3 0 677.182 15.7517 2 4 -3 0 685.257 15.6688 3 4 -3 0 676.741 16.4252 2 -4 3 0 678.611 15.8416 2 -4 3 0 676.182 15.7285 4 -4 3 0 677.770 15.7399 2 -4 3 0 690.941 15.5510 7 3 -3 0 1.92986 0.52071 3 3 -3 0 1.71194 0.50146 7 3 -3 0 2.50210 0.54555 2 3 -3 0 1.82003 0.54338 2 -3 3 0 1.29374 0.54821 4 -3 3 0 1.76920 0.48286 7 -3 3 0 1.61007 0.51200 2 -3 3 0 1.76717 0.51425 2 2 -3 0 1879.55 41.1815 2 2 -3 0 1930.48 41.1737 7 2 -3 0 1862.09 41.2539 2 2 -3 0 1947.30 41.1229 4 2 -3 0 1879.27 41.2580 3 -2 3 0 1860.62 41.2471 2 -2 3 0 1894.45 41.1663 2 -2 3 0 1943.57 41.1391 4 -2 3 0 1896.10 41.1250 7 1 -3 0 0.30384 0.29262 2 1 -3 0 0.30318 0.30358 7 1 -3 0 -0.0908 0.31281 3 1 -3 0 0.51128 0.29540 2 -1 3 0 1.09547 0.45173 3 -1 3 0 0.35604 0.26401 2 0 -3 0 369.332 8.35510 2 0 -3 0 362.831 8.65322 3 0 -3 0 370.693 8.35327 2 0 3 0 378.309 8.37787 2 0 3 0 361.465 8.29209 2 0 3 0 369.813 8.73125 3 -1 -3 0 96.0201 2.88490 3 -1 -3 0 95.8222 2.69076 6 -1 -3 0 98.5794 2.58007 2 -1 -3 0 95.8234 2.64548 2 1 3 0 97.9897 2.58415 2 1 3 0 98.5491 2.98945 3 1 3 0 99.7165 2.62042 2 -2 -3 0 280.457 6.77008 2 -2 -3 0 287.740 6.80785 6 2 3 0 283.246 6.72865 6 2 3 0 277.181 7.08898 3 2 3 0 282.744 6.72325 2 2 3 0 279.139 6.70629 2 -3 -3 0 19.2329 1.24473 2 -3 -3 0 18.4212 1.05695 2 3 3 0 18.0796 1.32078 3 3 3 0 19.1255 1.15937 2 3 3 0 19.5947 1.17458 2 3 3 0 17.3014 1.12777 6 -4 -3 0 3.69073 0.72354 7 -4 -3 0 4.00659 0.70513 2 4 3 0 4.41191 0.73311 6 4 3 0 4.88935 0.80565 2 4 3 0 3.66148 0.67516 4 4 3 0 5.86765 0.87188 2 -5 -3 0 9.11989 1.16453 7 -5 -3 0 10.3501 1.11665 2 -5 -3 0 10.1988 1.27909 2 5 3 0 11.3826 1.12759 4 5 3 0 10.1226 1.12189 6 5 3 0 9.63005 1.22592 2 5 3 0 9.27985 1.19685 2 -6 -3 0 42.5109 2.29109 7 -6 -3 0 44.3022 2.18784 2 6 3 0 45.1638 2.38920 2 6 3 0 42.2031 2.19122 6 6 3 0 43.6395 2.31415 2 6 3 0 45.0455 2.20562 4 -7 -3 0 51.1800 2.80613 2 -7 -3 0 48.0180 2.44731 2 -7 -3 0 47.8888 2.63969 7 7 3 0 45.8187 2.67494 2 7 3 0 51.4528 2.67091 2 7 3 0 50.9911 2.56119 6 7 3 0 48.0593 2.47677 4 -8 -3 0 5.86696 1.18658 2 -8 -3 0 5.13771 1.30309 7 -8 -3 0 6.83566 1.43798 2 8 3 0 4.57052 1.22931 2 8 3 0 6.99602 1.44530 2 8 3 0 5.09273 1.15757 4 8 3 0 4.60275 1.15194 6 -9 -3 0 8.72842 1.66845 7 -9 -3 0 8.85743 1.54006 2 9 3 0 9.56782 1.61531 2 9 3 0 8.76254 1.56112 4 9 3 0 11.5428 1.97755 2 -10 -3 0 3.39112 1.29728 2 -10 -3 0 6.77113 1.44567 2 10 3 0 4.33791 1.32063 6 10 3 0 6.39603 1.81753 3 10 3 0 3.47479 1.27637 4 10 3 0 3.10724 1.42762 2 -11 -3 0 -0.4393 1.26601 2 -11 -3 0 5.03582 1.41351 2 11 3 0 1.07803 0.99806 6 11 3 0 0.60074 1.39392 3 11 3 0 -0.7792 1.06151 2 12 -4 0 542.147 14.5513 7 12 -4 0 530.424 15.2563 2 -12 4 0 529.647 15.1061 2 -12 4 0 517.852 15.2034 2 11 -4 0 11.0847 2.10794 2 11 -4 0 12.7066 2.00096 7 -11 4 0 11.2526 1.98716 2 -11 4 0 8.36881 2.06821 2 10 -4 0 347.413 10.3707 2 10 -4 0 354.511 9.98198 7 10 -4 0 318.257 11.9652 4 -10 4 0 337.851 10.2790 2 -10 4 0 346.821 10.8806 7 -10 4 0 338.806 10.6098 2 9 -4 0 3.90739 1.49959 2 9 -4 0 2.26055 1.53095 4 9 -4 0 2.71274 1.15172 7 9 -4 0 5.05309 1.36312 2 -9 4 0 3.27575 1.28632 2 -9 4 0 6.22277 1.51455 2 -9 4 0 4.79533 1.28180 7 8 -4 0 392.737 10.3474 7 8 -4 0 367.350 10.6045 4 8 -4 0 391.958 10.7998 2 -8 4 0 382.331 10.5919 4 -8 4 0 388.069 10.1801 7 -8 4 0 382.662 10.5868 2 -8 4 0 384.530 10.7328 2 7 -4 0 98.5520 3.93787 2 7 -4 0 87.2121 3.81518 3 7 -4 0 101.755 4.10723 2 7 -4 0 101.335 3.78546 7 7 -4 0 102.309 4.03590 4 -7 4 0 103.312 4.02000 4 -7 4 0 96.5718 3.90712 2 -7 4 0 97.7723 3.59848 7 -7 4 0 95.1660 3.98616 2 6 -4 0 86.8484 3.43763 2 6 -4 0 84.7591 3.36557 3 6 -4 0 89.9145 3.61426 2 6 -4 0 89.2664 3.50202 4 6 -4 0 88.5184 3.31541 7 -6 4 0 86.8453 3.40601 2 -6 4 0 87.8713 3.17759 7 -6 4 0 84.5827 3.48731 2 -6 4 0 85.9258 3.44251 4 5 -4 0 298.591 7.93880 4 5 -4 0 302.750 7.98393 2 5 -4 0 278.867 7.78441 3 5 -4 0 316.857 7.89999 7 5 -4 0 306.786 8.13318 2 -5 4 0 294.793 8.06590 2 -5 4 0 303.078 7.97227 2 -5 4 0 308.127 7.70193 7 -5 4 0 300.470 7.92604 4 4 -4 0 191.207 5.39454 2 4 -4 0 197.415 5.25590 7 4 -4 0 187.546 5.23634 4 4 -4 0 183.767 5.23707 2 4 -4 0 176.913 5.19350 3 -4 4 0 193.291 5.12213 7 -4 4 0 186.230 5.22090 4 -4 4 0 191.313 5.39485 2 -4 4 0 188.257 5.24485 2 3 -4 0 178.172 4.95654 2 3 -4 0 174.324 4.82048 2 3 -4 0 186.104 4.86346 7 3 -4 0 172.630 4.74136 4 3 -4 0 175.499 4.90915 3 -3 4 0 180.066 4.97665 3 -3 4 0 186.403 4.78278 7 -3 4 0 176.593 4.79996 2 -3 4 0 181.278 4.88346 4 -3 4 0 174.499 4.92465 2 2 -4 0 352.593 8.46681 4 2 -4 0 364.737 8.80209 2 2 -4 0 353.096 8.82324 3 2 -4 0 356.996 8.61937 2 2 -4 0 371.267 8.78173 7 -2 4 0 369.884 8.92931 3 -2 4 0 370.100 8.74611 2 -2 4 0 362.931 8.61092 2 -2 4 0 377.597 8.51987 4 1 -4 0 167.734 4.56844 3 1 -4 0 166.559 4.23769 2 -1 4 0 165.720 4.64174 3 -1 4 0 163.278 4.19021 2 -1 4 0 165.811 4.31236 2 0 -4 0 993.616 21.9177 3 0 -4 0 965.584 21.4611 2 0 -4 0 998.607 21.7622 2 0 4 0 985.631 22.0218 3 0 4 0 959.591 21.3852 2 0 4 0 956.800 21.4753 2 -1 -4 0 1832.55 39.4270 2 -1 -4 0 1812.42 39.8416 3 -1 -4 0 1817.44 39.3274 2 -1 -4 0 1778.18 39.4708 6 1 4 0 1824.15 39.3221 2 1 4 0 1845.49 39.3984 2 1 4 0 1803.08 39.9930 3 -2 -4 0 524.704 12.4141 2 -2 -4 0 573.878 12.6478 2 -2 -4 0 550.907 12.6401 6 2 4 0 550.047 13.1605 3 2 4 0 533.215 12.4911 2 2 4 0 561.149 12.5423 2 -3 -4 0 0.97498 0.52694 6 -3 -4 0 1.61782 0.60515 2 -3 -4 0 0.64933 0.43535 2 3 4 0 0.59624 0.47280 2 3 4 0 1.19239 0.50151 2 3 4 0 0.72821 0.59403 3 3 4 0 1.00301 0.47067 6 -4 -4 0 0.15294 0.50871 7 -4 -4 0 1.66549 0.58172 2 4 4 0 0.57458 0.53074 2 4 4 0 0.85900 0.53281 6 4 4 0 1.30363 0.59472 2 4 4 0 -0.1129 0.64755 3 -5 -4 0 8.01140 1.05102 2 -5 -4 0 6.97319 1.18354 2 -5 -4 0 6.84394 1.09069 7 5 4 0 7.92852 1.20809 2 5 4 0 8.13729 1.15119 2 5 4 0 7.76634 1.07765 6 5 4 0 7.07159 1.26206 3 -6 -4 0 15.0858 1.57440 7 -6 -4 0 16.1787 1.47936 2 -6 -4 0 15.7260 1.79923 2 6 4 0 14.2517 1.51806 6 6 4 0 16.3375 1.88854 3 6 4 0 17.6091 1.71075 2 6 4 0 15.7544 1.65760 2 -7 -4 0 87.6345 3.79789 7 -7 -4 0 87.4210 3.44877 2 -7 -4 0 89.3646 3.94083 2 7 4 0 89.4421 3.56534 6 7 4 0 88.7088 3.49356 4 7 4 0 95.2397 3.73110 2 7 4 0 92.5848 3.95817 2 7 4 0 90.2781 4.22071 3 -8 -4 0 69.8806 3.67042 7 -8 -4 0 57.8032 3.38529 2 -8 -4 0 62.2112 3.00743 2 8 4 0 61.5969 3.00407 4 8 4 0 66.6755 3.72594 3 8 4 0 59.7253 3.05502 6 8 4 0 60.8848 3.31331 2 8 4 0 67.8209 3.91554 2 -9 -4 0 256.539 8.35035 7 -9 -4 0 270.934 8.60174 2 -9 -4 0 263.027 7.79377 2 9 4 0 263.549 8.69626 2 9 4 0 261.276 8.07066 2 9 4 0 266.045 7.96917 6 9 4 0 259.937 7.94620 4 9 4 0 272.410 8.79942 3 -10 -4 0 227.418 8.71520 2 -10 -4 0 230.063 8.00974 2 10 4 0 219.516 7.33885 6 10 4 0 229.636 7.50635 2 10 4 0 236.942 8.25078 3 10 4 0 224.678 7.39468 4 11 -5 0 33.7035 3.98683 2 11 -5 0 35.5153 2.91503 7 -11 5 0 37.8159 3.13897 2 -11 5 0 39.4412 3.31813 2 10 -5 0 129.348 5.51979 2 10 -5 0 132.487 5.22339 7 10 -5 0 122.628 5.63856 2 -10 5 0 135.195 5.52814 2 -10 5 0 127.826 4.97578 7 -10 5 0 146.636 8.56708 2 9 -5 0 9.70898 1.60683 7 9 -5 0 6.12959 1.47011 4 9 -5 0 8.47246 1.60187 2 9 -5 0 11.8303 2.03526 2 -9 5 0 8.38145 1.56349 2 -9 5 0 8.83348 1.46177 7 -9 5 0 10.2971 1.70216 2 -9 5 0 9.72180 1.69933 4 8 -5 0 97.2109 4.27253 4 8 -5 0 104.524 4.52431 2 8 -5 0 100.458 4.10808 7 -8 5 0 105.048 4.44313 2 -8 5 0 106.437 4.41160 4 -8 5 0 103.649 3.94235 7 -8 5 0 102.323 4.29235 2 7 -5 0 47.0262 2.56288 7 7 -5 0 44.7119 2.61287 2 7 -5 0 42.6696 2.60104 4 7 -5 0 43.1007 2.77308 2 -7 5 0 43.4117 2.55395 2 -7 5 0 49.4635 2.79366 2 -7 5 0 45.7870 2.40248 7 -7 5 0 54.6306 2.88262 4 6 -5 0 102.891 3.85156 4 6 -5 0 102.284 3.85717 2 6 -5 0 94.4582 3.71698 3 6 -5 0 102.995 4.02987 2 6 -5 0 104.504 3.78780 7 -6 5 0 104.881 3.63812 7 -6 5 0 97.8994 3.81624 2 -6 5 0 104.690 3.99647 2 -6 5 0 105.769 3.88039 4 5 -5 0 62.7579 2.67944 4 5 -5 0 63.9090 2.69752 7 5 -5 0 65.3372 2.87535 2 5 -5 0 62.0020 2.69627 2 -5 5 0 61.1722 2.63368 2 -5 5 0 61.5799 2.80731 2 -5 5 0 64.7705 2.56595 7 -5 5 0 64.0983 2.72534 4 4 -5 0 1.50999 0.64468 2 4 -5 0 1.90463 0.74017 2 4 -5 0 2.49700 0.68770 7 4 -5 0 1.99784 0.66868 3 -4 5 0 3.51248 0.71898 7 -4 5 0 0.90595 0.63414 4 -4 5 0 1.73529 0.69279 2 -4 5 0 1.93981 0.70638 2 3 -5 0 151.874 4.38710 2 3 -5 0 143.833 4.47841 3 3 -5 0 153.497 4.53840 2 3 -5 0 159.631 4.45990 7 3 -5 0 147.041 4.22001 4 -3 5 0 159.973 4.69901 3 -3 5 0 151.567 4.33581 2 -3 5 0 158.883 4.39880 4 -3 5 0 154.550 4.53499 2 2 -5 0 127.486 3.92267 3 2 -5 0 128.093 3.78688 2 2 -5 0 122.345 3.99368 2 2 -5 0 129.080 3.78053 7 -2 5 0 127.255 3.79760 2 -2 5 0 128.524 4.04986 3 -2 5 0 127.085 3.61285 2 1 -5 0 1661.27 35.7696 2 1 -5 0 1636.98 35.8724 2 1 -5 0 1641.54 36.2463 3 -1 5 0 1646.38 36.3865 3 -1 5 0 1629.62 35.8684 2 -1 5 0 1615.72 35.6730 2 0 -5 0 615.811 14.6034 3 0 -5 0 615.670 14.1072 2 0 -5 0 625.367 14.1388 2 0 5 0 635.297 14.1707 2 0 5 0 624.843 14.8069 3 0 5 0 617.725 14.0192 2 -1 -5 0 139.321 3.85898 2 -1 -5 0 134.465 4.38354 3 -1 -5 0 141.209 3.95611 6 -1 -5 0 136.827 3.76690 2 1 5 0 142.114 3.83544 2 1 5 0 138.607 3.74126 2 1 5 0 137.902 4.45921 3 -2 -5 0 14.9358 1.02786 2 -2 -5 0 16.7334 1.24015 2 -2 -5 0 15.4602 1.20039 6 2 5 0 15.0252 1.08777 2 2 5 0 15.5822 1.05856 2 2 5 0 14.6449 1.45841 3 -3 -5 0 1.16500 0.68989 2 -3 -5 0 0.87886 0.52545 6 -3 -5 0 1.10130 0.51298 2 3 5 0 1.13103 0.75949 3 3 5 0 1.05205 0.52921 2 3 5 0 1.80945 0.58083 2 -4 -5 0 138.765 4.16555 2 -4 -5 0 145.196 6.29213 2 4 5 0 149.955 4.36193 6 4 5 0 147.967 4.38403 2 4 5 0 147.370 5.05234 3 4 5 0 144.573 4.47073 2 -5 -5 0 43.7838 2.10148 2 -5 -5 0 43.5153 2.45762 2 -5 -5 0 43.4315 2.36575 7 5 5 0 42.9493 2.22092 2 5 5 0 45.5401 2.78712 3 5 5 0 43.5718 2.21136 6 5 5 0 41.3054 2.28484 2 -6 -5 0 153.714 5.31356 2 -6 -5 0 153.654 5.25733 7 6 5 0 162.375 4.99260 6 6 5 0 158.810 5.04609 2 6 5 0 160.346 5.34636 2 -7 -5 0 230.665 6.61804 2 -7 -5 0 226.098 7.14021 7 7 5 0 226.698 7.59286 3 7 5 0 219.641 7.12870 2 7 5 0 225.693 6.70376 6 7 5 0 238.360 6.92853 2 -8 -5 0 324.832 8.90203 2 -8 -5 0 323.095 9.61279 7 -8 -5 0 320.782 9.60865 2 8 5 0 319.364 9.19590 6 8 5 0 313.807 9.56458 2 8 5 0 333.215 10.1207 3 -9 -5 0 85.7801 4.31535 2 -9 -5 0 94.3417 3.94728 2 9 5 0 81.2518 3.71358 4 9 5 0 84.5461 3.89360 6 9 5 0 90.1950 4.11792 2 9 5 0 86.5272 4.75315 3 -10 -5 0 67.3123 3.86556 2 -10 -5 0 59.1459 3.34183 2 10 5 0 71.5797 4.51075 3 10 5 0 71.8135 3.77243 2 10 5 0 64.1513 3.47333 6 10 5 0 58.7490 3.25573 4 11 -6 0 5.35559 2.11130 2 11 -6 0 4.67268 1.81456 2 11 -6 0 4.89569 1.46642 7 -11 6 0 3.84000 1.54883 2 -11 6 0 4.93004 1.99187 2 10 -6 0 12.4778 1.92317 2 10 -6 0 10.0464 1.75324 7 10 -6 0 12.2849 2.02742 2 -10 6 0 14.5651 1.93543 7 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6 0 529.325 12.1453 2 -2 -6 0 79.5895 2.70596 2 -2 -6 0 83.9014 2.92274 2 -2 -6 0 79.0698 2.93550 6 2 6 0 81.6830 2.79512 2 2 6 0 79.2294 3.48191 3 -3 -6 0 3.87329 0.91702 6 -3 -6 0 3.45920 0.75747 2 -3 -6 0 3.34438 0.92897 2 3 6 0 4.61583 0.87988 2 3 6 0 5.00740 0.90394 2 3 6 0 2.90284 1.05381 3 -4 -6 0 1124.62 25.7612 6 -4 -6 0 1132.74 25.3928 2 -4 -6 0 1122.93 26.6372 2 4 6 0 1154.45 25.5697 2 4 6 0 1141.43 26.7426 3 4 6 0 1110.06 25.7063 2 -5 -6 0 330.993 8.86997 2 -5 -6 0 303.312 8.77002 7 5 6 0 331.546 8.50751 2 5 6 0 319.141 8.70564 2 -6 -6 0 264.514 7.92084 2 -6 -6 0 269.287 7.99193 7 -6 -6 0 268.243 7.37138 2 6 6 0 268.569 7.94282 2 6 6 0 267.664 7.48593 6 6 6 0 280.464 7.67814 2 6 6 0 281.184 8.75356 3 -7 -6 0 255.512 7.97642 2 -7 -6 0 245.344 7.86520 7 -7 -6 0 260.815 7.31189 2 7 6 0 268.652 8.75307 3 7 6 0 260.501 8.02309 2 7 6 0 254.118 7.37966 6 7 6 0 257.580 7.52381 2 -8 -6 0 2.51734 1.04954 2 -8 -6 0 1.56116 1.27356 2 8 6 0 1.98912 1.51462 3 8 6 0 2.86638 1.36956 2 8 6 0 3.83488 1.21202 6 -9 -6 0 120.608 5.31602 2 -9 -6 0 130.753 4.87004 2 9 6 0 131.414 5.03012 2 9 6 0 121.548 4.81909 6 9 6 0 130.865 6.17459 3 11 -7 0 2.62868 1.49288 2 11 -7 0 1.80059 1.21286 7 11 -7 0 0.97122 1.46828 2 -11 7 0 4.00821 1.60335 2 10 -7 0 2.13677 1.11214 7 10 -7 0 4.00442 1.40820 2 10 -7 0 2.99281 1.38971 2 -10 7 0 0.73450 1.13830 2 -10 7 0 7.84530 2.64060 2 9 -7 0 7.02914 1.54486 2 9 -7 0 5.87641 1.58408 2 9 -7 0 6.84879 1.61352 4 9 -7 0 6.20762 1.51783 7 -9 7 0 7.02615 1.63413 2 -9 7 0 4.70414 1.36992 7 8 -7 0 41.8497 2.80126 7 8 -7 0 46.8497 2.97973 4 8 -7 0 40.7272 3.06411 2 -8 7 0 46.4553 2.68215 7 -8 7 0 40.8392 2.95203 2 -8 7 0 45.0709 2.86380 2 -8 7 0 43.5048 2.93357 4 7 -7 0 23.2778 2.12508 2 7 -7 0 25.3061 3.00860 2 7 -7 0 24.1255 2.28380 7 7 -7 0 24.0278 2.13291 4 -7 7 0 22.9827 2.19529 2 -7 7 0 24.3513 2.08854 2 -7 7 0 23.3134 1.96720 7 -7 7 0 22.6212 2.97718 4 6 -7 0 63.8262 3.06656 2 6 -7 0 62.5412 3.09891 7 6 -7 0 63.8347 3.29902 2 6 -7 0 63.1656 2.98453 4 -6 7 0 65.9675 3.28039 2 -6 7 0 63.9208 3.05883 4 -6 7 0 66.7213 3.02620 2 5 -7 0 207.757 6.33818 7 5 -7 0 212.727 6.59967 2 5 -7 0 216.125 6.16985 4 5 -7 0 211.631 6.29968 2 -5 7 0 217.396 6.17033 4 -5 7 0 212.282 6.18536 2 -5 7 0 208.725 7.29759 2 4 -7 0 102.776 3.77526 7 4 -7 0 101.863 3.66409 2 4 -7 0 103.924 3.47578 4 4 -7 0 105.086 3.93371 2 -4 7 0 108.776 3.56184 4 -4 7 0 99.4840 3.54503 2 -4 7 0 102.007 3.89218 2 -4 7 0 100.690 4.08260 3 3 -7 0 0.31621 0.63983 2 3 -7 0 0.22697 0.70578 3 3 -7 0 0.29258 0.60848 7 3 -7 0 -0.5817 0.58235 2 -3 7 0 0.13594 0.61251 2 -3 7 0 -0.1408 0.87891 3 -3 7 0 -0.1519 0.45831 2 2 -7 0 5.66754 1.02919 7 2 -7 0 4.28090 0.92124 2 2 -7 0 5.05258 0.88939 2 -2 7 0 5.33907 1.25440 3 -2 7 0 4.68601 0.79068 2 -2 7 0 3.45614 0.80646 2 1 -7 0 383.329 9.63433 2 -1 7 0 389.741 9.66130 2 -1 7 0 377.943 9.32146 2 -1 7 0 397.943 10.4040 3 0 -7 0 96.3737 3.27812 2 0 -7 0 103.227 3.36284 2 0 7 0 98.2960 4.09224 3 0 7 0 103.510 3.39874 2 0 7 0 98.2448 3.15564 2 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4 -5 8 0 0.09788 0.75240 2 4 -8 0 1.82724 0.72695 4 4 -8 0 2.75022 1.03856 2 4 -8 0 2.40735 0.96194 7 4 -8 0 2.31927 0.90101 2 -4 8 0 2.80470 1.01218 2 -4 8 0 1.25401 0.72048 2 -4 8 0 1.02711 1.20523 3 3 -8 0 36.8103 2.33217 2 3 -8 0 36.8621 2.10643 2 3 -8 0 38.0224 2.30113 7 -3 8 0 38.6898 2.31794 2 -3 8 0 37.8470 2.82934 3 -3 8 0 38.3852 2.00449 2 2 -8 0 14.9782 1.54981 2 2 -8 0 12.0705 1.55189 7 2 -8 0 15.0173 1.52394 2 -2 8 0 13.4676 1.57359 2 -2 8 0 13.9572 1.31270 2 -2 8 0 15.4520 2.18717 3 1 -8 0 1.39637 0.77015 2 1 -8 0 1.83500 0.85186 2 -1 8 0 1.53092 0.63157 2 -1 8 0 0.13308 1.08322 3 -1 8 0 0.95469 0.74495 2 0 -8 0 482.188 11.7156 2 0 8 0 475.358 11.6966 2 0 8 0 472.614 12.7616 3 0 8 0 469.147 11.3941 2 -1 -8 0 812.964 19.2147 6 -1 -8 0 815.360 18.9631 2 -1 -8 0 838.769 19.7296 2 1 8 0 789.158 18.7517 2 1 8 0 823.316 20.2692 3 1 8 0 827.961 18.9915 2 -2 -8 0 0.45830 0.87794 2 -2 -8 0 2.54983 0.99111 6 -2 -8 0 3.87621 1.26783 2 2 8 0 2.24546 0.87118 2 2 8 0 3.10314 1.44722 3 2 8 0 3.01175 0.87308 2 -3 -8 0 395.819 11.9796 2 -3 -8 0 376.913 9.71289 2 -3 -8 0 375.095 10.1080 6 3 8 0 394.643 11.3225 3 3 8 0 377.148 9.86881 2 3 8 0 389.968 9.84506 2 -4 -8 0 51.9989 2.79705 6 -4 -8 0 52.0059 2.52193 2 -4 -8 0 53.2655 2.91994 2 4 8 0 47.1025 3.53639 3 4 8 0 50.6572 2.70074 2 4 8 0 56.8615 2.74990 2 -5 -8 0 3.51434 0.99343 2 -5 -8 0 5.64049 1.35741 2 5 8 0 4.85457 1.13700 2 5 8 0 7.59653 1.40596 2 5 8 0 4.32534 1.60348 3 -6 -8 0 4.70809 1.06812 2 -6 -8 0 2.33903 1.35318 2 6 8 0 4.24774 1.13009 2 6 8 0 3.81353 1.59800 3 -7 -8 0 2.38912 1.28345 2 -7 -8 0 1.80513 0.95245 2 7 8 0 2.25998 1.09280 2 7 8 0 4.25879 1.77011 3 8 8 0 1.50286 0.97304 2 8 8 0 0.23192 1.55561 3 10 -9 0 9.73939 1.89897 2 10 -9 0 8.59523 1.81083 7 -10 9 0 9.07787 1.91476 2 9 -9 0 4.76369 1.57495 2 9 -9 0 5.07626 1.42523 7 9 -9 0 5.09126 1.46953 2 -9 9 0 4.54904 1.69067 2 8 -9 0 4.02346 1.27883 2 8 -9 0 5.04922 1.55863 2 8 -9 0 3.08529 1.26734 7 -8 9 0 6.46367 1.50784 2 -8 9 0 3.87529 1.42990 2 7 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9 0 580.073 14.1815 2 0 -9 0 12.4968 1.54546 2 0 -9 0 10.6769 1.48397 6 0 9 0 10.6872 1.40726 2 -1 -9 0 46.0556 2.46211 2 -1 -9 0 46.7584 2.59984 6 -1 -9 0 42.4193 3.10131 2 1 9 0 46.0377 2.27011 2 1 9 0 46.2375 2.50776 2 1 9 0 42.9315 3.46300 3 -2 -9 0 114.180 4.03263 2 -2 -9 0 117.038 4.31005 6 -2 -9 0 102.131 4.79270 2 2 9 0 112.379 4.03972 2 2 9 0 119.101 5.34187 3 2 9 0 108.583 3.91049 2 -3 -9 0 164.460 5.60610 6 -3 -9 0 169.342 5.30065 2 -3 -9 0 175.454 5.72561 2 3 9 0 163.656 5.37393 2 3 9 0 172.538 5.36054 2 3 9 0 170.310 6.74737 3 -4 -9 0 21.8438 1.89428 2 -4 -9 0 19.9230 2.21050 2 -4 -9 0 24.5854 2.15459 6 4 9 0 21.9976 2.96206 3 4 9 0 24.9102 2.02386 2 4 9 0 19.9759 1.96830 2 -5 -9 0 2.74623 0.98362 2 -5 -9 0 3.69122 1.29546 2 5 9 0 1.54830 1.60151 3 5 9 0 3.88417 1.18763 2 -6 -9 0 10.3591 1.55600 2 -6 -9 0 9.16998 1.75636 2 6 9 0 9.26985 2.27217 3 6 9 0 7.12413 1.38251 2 -7 -9 0 76.2265 4.21755 2 7 9 0 83.4907 5.33721 3 9 -10 0 35.4351 3.32289 2 9 -10 0 30.4521 2.90247 7 9 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2938.19 64.2096 5 0 -3 4 3063.33 64.1304 5 0 -3 4 2987.02 64.2400 3 0 -3 4 2925.22 63.9306 6 -1 3 -4 6.04414 0.54965 2 -1 3 -4 7.39873 1.14283 5 -1 3 -4 4.64290 0.60493 2 -1 3 -4 4.71317 0.67549 7 1 -3 4 6.82923 0.81164 7 1 -3 4 6.49752 0.61928 2 1 -3 4 4.87234 0.56864 2 1 -3 4 7.87726 0.96088 5 1 -3 4 7.67152 1.04882 3 -2 3 -4 632.815 14.8793 7 -2 3 -4 632.598 14.6822 2 -2 3 -4 635.553 14.5694 2 -2 3 -4 684.398 15.1507 5 2 -3 4 648.350 14.6484 2 2 -3 4 650.903 14.7366 2 2 -3 4 658.174 15.3908 3 2 -3 4 660.345 14.9904 7 -3 3 -4 2010.53 44.5047 2 -3 3 -4 2036.82 44.6420 7 -3 3 -4 2030.96 44.7719 5 3 -3 4 2063.73 44.7316 7 3 -3 4 2050.92 44.5683 2 3 -3 4 2027.87 44.4146 2 -4 3 -4 2.50004 0.74757 7 -4 3 -4 1.51487 0.68677 2 -4 3 -4 1.78506 0.64938 2 4 -3 4 1.24942 0.63935 7 4 -3 4 2.94769 0.80018 2 4 -3 4 2.29837 0.73756 2 -5 3 -4 475.828 11.9404 7 -5 3 -4 486.960 11.7700 2 5 -3 4 473.381 11.9479 4 5 -3 4 479.994 11.8298 2 5 -3 4 489.813 12.0379 7 5 -3 4 464.626 11.9276 2 -6 3 -4 166.307 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7.30398 2.27784 5 -5 4 -9 9.12507 1.56640 2 5 -4 9 7.93742 1.47986 7 5 -4 9 6.96197 1.40094 2 5 -4 9 9.82783 1.62303 2 -6 4 -9 75.5479 3.28900 2 -6 4 -9 70.0055 3.70206 7 -6 4 -9 76.3064 4.97507 5 6 -4 9 73.6701 3.55843 2 6 -4 9 71.7771 3.76459 7 6 -4 9 74.4874 3.87096 2 -7 4 -9 81.8736 5.35037 5 -7 4 -9 80.7838 3.63162 2 7 -4 9 76.9005 4.36993 2 7 -4 9 78.4007 4.21876 7 7 -4 9 79.2954 4.20654 2 -8 4 -9 21.6291 3.29872 5 -8 4 -9 21.2419 2.31071 2 8 -4 9 18.0262 2.26338 2 8 -4 9 20.0636 2.53065 2 8 -4 9 15.0285 2.27751 7 9 3 -9 72.4554 3.15811 2 9 3 -9 74.6993 4.32454 6 -9 -3 9 70.9614 4.00750 4 -9 -3 9 79.8860 3.18618 2 -9 -3 9 75.5969 3.27633 2 8 3 -9 1.45200 1.01421 4 8 3 -9 2.95272 0.83696 2 8 3 -9 2.48523 1.37414 6 -8 -3 9 2.02896 1.14891 4 -8 -3 9 3.14315 0.79109 2 -8 -3 9 3.60950 0.96715 2 7 3 -9 80.0673 4.13690 6 7 3 -9 81.4185 3.78354 4 -7 -3 9 77.2089 3.11677 2 -7 -3 9 83.9406 3.07973 2 -7 -3 9 87.7813 4.02176 4 6 3 -9 138.577 4.93338 4 6 3 -9 140.237 5.39862 6 -6 -3 9 150.981 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53.8197 3.18350 6 3 -7 10 55.8022 3.11779 7 -4 7 -10 22.0421 3.04359 5 -4 7 -10 20.1986 2.18235 7 -4 7 -10 21.7763 1.48901 2 4 -7 10 20.7092 2.20993 7 4 -7 10 21.5533 1.79398 2 4 -7 10 21.1559 1.95319 2 4 -7 10 22.4169 2.28993 6 -5 7 -10 29.2306 1.90880 2 -5 7 -10 27.0912 3.52662 5 5 -7 10 28.4585 2.53641 6 5 -7 10 27.2231 2.56704 7 5 -7 10 28.1264 2.22458 2 -6 7 -10 12.2734 2.66179 5 -6 7 -10 6.47811 1.24379 2 6 -7 10 3.01591 1.34114 7 6 -7 10 4.95462 1.40264 2 6 -7 10 6.36194 1.43710 6 6 -7 10 6.81214 1.51070 2 -8 -6 10 9.52988 1.67613 4 7 6 -10 17.9497 2.40890 6 -7 -6 10 20.9183 2.20561 4 6 6 -10 33.3759 2.81312 6 -6 -6 10 30.0946 2.45544 4 5 6 -10 36.5370 2.90039 6 5 6 -10 36.6019 2.94028 3 -5 -6 10 41.1252 2.65979 4 4 6 -10 11.8892 2.53359 5 4 6 -10 9.62712 1.71533 6 -4 -6 10 13.0756 1.80821 4 3 6 -10 107.179 5.62729 5 -3 -6 10 102.949 4.10963 4 2 6 -10 52.3853 4.11169 5 -2 -6 10 49.7184 3.15908 4 -2 -6 10 48.5845 3.01228 6 1 6 -10 16.0215 2.65109 5 -1 -6 10 17.4851 1.91598 4 -1 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1.26843 6 4 0 -13 4.23372 1.17179 2 4 0 -13 4.59133 2.54659 5 -4 0 13 4.19530 1.07505 2 3 0 -13 87.5112 6.29349 5 3 0 -13 91.4162 5.22315 2 -3 0 13 100.173 3.83780 2 2 0 -13 164.816 8.16086 5 2 0 -13 165.159 5.53422 2 -2 0 13 168.678 5.48455 2 -2 0 13 163.109 7.68725 4 -2 0 13 147.036 7.79720 2 1 0 -13 4.69530 1.20371 2 1 0 -13 2.60592 2.42879 5 -1 0 13 4.47210 1.36395 2 0 0 -13 305.385 11.3830 5 0 0 13 304.941 8.90649 2 2 -1 -13 117.870 6.93990 5 -2 1 13 109.485 4.42894 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 multi-scan _exptl_absorpt_correction_T_max 0.8879 _exptl_absorpt_correction_T_min 0.8417 _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 0.71122 9.066 9.937 10.274 105.956 96.819 97.171 ) ; _shelx_hkl_checksum 1472 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder 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 0.09886(9) 0.07333(8) 0.28063(8) 0.02278(17) Uani 1 1 d . . . . . N1 N 0.18804(9) 0.31175(9) 0.37286(8) 0.01666(17) Uani 1 1 d . . . . . N2 N 0.35230(10) 0.54793(10) 0.09888(9) 0.02066(18) Uani 1 1 d . . . . . C1 C 0.14021(11) 0.17688(11) 0.38370(10) 0.01834(19) Uani 1 1 d . . . . . C2 C 0.14293(11) 0.17200(11) 0.52323(11) 0.0196(2) Uani 1 1 d . . . . . H2 H 0.114633 0.082701 0.538170 0.023 Uiso 1 1 calc R . . . . C3 C 0.18417(11) 0.28938(11) 0.63488(10) 0.0189(2) Uani 1 1 d . . . . . C4 C 0.22863(11) 0.42398(11) 0.61501(10) 0.01846(19) Uani 1 1 d . . . . . H4 H 0.257196 0.507129 0.691064 0.022 Uiso 1 1 calc R . . . . C5 C 0.22923(11) 0.43074(10) 0.48433(10) 0.01663(19) Uani 1 1 d . . . . . C6 C 0.27069(11) 0.55165(10) 0.43343(10) 0.01681(19) Uani 1 1 d . . . . . C7 C 0.25789(11) 0.50522(10) 0.29569(10) 0.01694(19) Uani 1 1 d . . . . . C8 C 0.27773(11) 0.59493(10) 0.20358(10) 0.01705(19) Uani 1 1 d . . . . . C9 C 0.21806(11) 0.72116(11) 0.22424(10) 0.0196(2) Uani 1 1 d . . . . . H9 H 0.165405 0.751545 0.298975 0.023 Uiso 1 1 calc R . . . . C10 C 0.23670(12) 0.80118(11) 0.13451(11) 0.0217(2) Uani 1 1 d . . . . . H10 H 0.196230 0.886742 0.145988 0.026 Uiso 1 1 calc R . . . . C11 C 0.31568(12) 0.75408(11) 0.02734(11) 0.0217(2) Uani 1 1 d . . . . . H11 H 0.331533 0.807219 -0.035338 0.026 Uiso 1 1 calc R . . . . C12 C 0.37076(12) 0.62786(12) 0.01403(11) 0.0216(2) Uani 1 1 d . . . . . H12 H 0.424731 0.596042 -0.059433 0.026 Uiso 1 1 calc R . . . . C13 C 0.20473(11) 0.34543(10) 0.24166(10) 0.01721(19) Uani 1 1 d . . . . . C14 C 0.32023(12) 0.26349(11) 0.17104(11) 0.0214(2) Uani 1 1 d . . . . . H14A H 0.417993 0.290965 0.231542 0.032 Uiso 1 1 calc GR . . . . H14B H 0.330353 0.285833 0.084950 0.032 Uiso 1 1 calc GR . . . . H14C H 0.286194 0.161279 0.151485 0.032 Uiso 1 1 calc GR . . . . C15 C 0.05225(12) 0.31252(12) 0.14720(11) 0.0230(2) Uani 1 1 d . . . . . H15A H 0.014388 0.210338 0.120841 0.035 Uiso 1 1 calc GR . . . . H15B H 0.064632 0.341490 0.064717 0.035 Uiso 1 1 calc GR . . . . H15C H -0.019732 0.364697 0.195657 0.035 Uiso 1 1 calc GR . . . . C16 C 0.31822(11) 0.69761(10) 0.52643(10) 0.01684(19) Uani 1 1 d . . . . . C17 C 0.45621(11) 0.77712(11) 0.52529(10) 0.0191(2) Uani 1 1 d . . . . . H17 H 0.520711 0.737596 0.463772 0.023 Uiso 1 1 calc R . . . . C18 C 0.49941(12) 0.91393(11) 0.61391(11) 0.0222(2) Uani 1 1 d . . . . . H18 H 0.593926 0.967271 0.613527 0.027 Uiso 1 1 calc R . . . . C19 C 0.40514(13) 0.97303(11) 0.70299(11) 0.0235(2) Uani 1 1 d . . . . . H19 H 0.434947 1.066796 0.763134 0.028 Uiso 1 1 calc R . . . . C20 C 0.26694(13) 0.89495(11) 0.70422(11) 0.0228(2) Uani 1 1 d . . . . . H20 H 0.201900 0.935500 0.764655 0.027 Uiso 1 1 calc R . . . . C21 C 0.22434(12) 0.75748(11) 0.61677(11) 0.0200(2) Uani 1 1 d . . . . . H21 H 0.130521 0.703809 0.618501 0.024 Uiso 1 1 calc R . . . . C22 C 0.18549(14) 0.27928(12) 0.77841(11) 0.0254(2) Uani 1 1 d . . . . . H22A H 0.135584 0.184652 0.774968 0.038 Uiso 1 1 calc GR . . . . H22B H 0.131852 0.351333 0.829097 0.038 Uiso 1 1 calc GR . . . . H22C H 0.289904 0.295281 0.824781 0.038 Uiso 1 1 calc GR . . . . 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 0.0253(4) 0.0179(3) 0.0225(4) 0.0032(3) 0.0037(3) -0.0002(3) N1 0.0182(4) 0.0163(4) 0.0155(4) 0.0051(3) 0.0036(3) 0.0012(3) N2 0.0236(4) 0.0213(4) 0.0198(4) 0.0085(3) 0.0073(3) 0.0050(3) C1 0.0168(4) 0.0170(4) 0.0215(5) 0.0061(4) 0.0042(3) 0.0017(3) C2 0.0201(5) 0.0181(4) 0.0222(5) 0.0089(4) 0.0048(4) 0.0013(4) C3 0.0187(4) 0.0210(5) 0.0195(5) 0.0090(4) 0.0051(3) 0.0035(4) C4 0.0208(4) 0.0174(4) 0.0175(4) 0.0055(3) 0.0040(3) 0.0026(3) C5 0.0161(4) 0.0161(4) 0.0178(4) 0.0050(3) 0.0035(3) 0.0022(3) C6 0.0167(4) 0.0168(4) 0.0180(4) 0.0065(3) 0.0041(3) 0.0024(3) C7 0.0163(4) 0.0169(4) 0.0186(4) 0.0061(3) 0.0040(3) 0.0030(3) C8 0.0173(4) 0.0181(4) 0.0158(4) 0.0058(3) 0.0022(3) 0.0016(3) C9 0.0208(5) 0.0199(5) 0.0178(4) 0.0048(4) 0.0030(4) 0.0041(4) C10 0.0246(5) 0.0183(5) 0.0214(5) 0.0062(4) -0.0001(4) 0.0034(4) C11 0.0241(5) 0.0214(5) 0.0202(5) 0.0096(4) 0.0016(4) 0.0006(4) C12 0.0236(5) 0.0241(5) 0.0194(5) 0.0088(4) 0.0068(4) 0.0032(4) C13 0.0194(4) 0.0176(4) 0.0150(4) 0.0056(3) 0.0038(3) 0.0016(3) C14 0.0259(5) 0.0192(5) 0.0209(5) 0.0059(4) 0.0090(4) 0.0050(4) C15 0.0220(5) 0.0263(5) 0.0197(5) 0.0084(4) 0.0001(4) -0.0004(4) C16 0.0198(4) 0.0158(4) 0.0159(4) 0.0066(3) 0.0021(3) 0.0027(3) C17 0.0185(4) 0.0199(5) 0.0201(5) 0.0076(4) 0.0034(4) 0.0035(4) C18 0.0201(5) 0.0193(5) 0.0265(5) 0.0085(4) 0.0000(4) 0.0000(4) C19 0.0272(5) 0.0169(5) 0.0237(5) 0.0038(4) -0.0005(4) 0.0036(4) C20 0.0272(5) 0.0206(5) 0.0215(5) 0.0053(4) 0.0062(4) 0.0070(4) C21 0.0210(5) 0.0190(5) 0.0210(5) 0.0072(4) 0.0054(4) 0.0029(4) C22 0.0326(6) 0.0252(5) 0.0208(5) 0.0104(4) 0.0061(4) 0.0037(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 C13 125.09(8) . . ? C5 N1 C1 123.29(9) . . ? C5 N1 C13 111.60(8) . . ? C12 N2 C8 117.65(9) . . ? O1 C1 N1 121.33(9) . . ? O1 C1 C2 124.71(9) . . ? N1 C1 C2 113.95(9) . . ? C1 C2 H2 118.4 . . ? C3 C2 C1 123.28(9) . . ? C3 C2 H2 118.4 . . ? C2 C3 C4 119.32(9) . . ? C2 C3 C22 121.47(9) . . ? C4 C3 C22 119.20(9) . . ? C3 C4 H4 120.8 . . ? C5 C4 C3 118.40(9) . . ? C5 C4 H4 120.8 . . ? N1 C5 C6 107.79(8) . . ? C4 C5 N1 121.72(9) . . ? C4 C5 C6 130.49(9) . . ? C5 C6 C16 122.11(9) . . ? C7 C6 C5 108.88(9) . . ? C7 C6 C16 129.01(9) . . ? C6 C7 C8 126.08(9) . . ? C6 C7 C13 111.32(9) . . ? C8 C7 C13 122.38(8) . . ? N2 C8 C7 116.91(9) . . ? N2 C8 C9 122.27(9) . . ? C9 C8 C7 120.81(9) . . ? C8 C9 H9 120.4 . . ? C10 C9 C8 119.18(9) . . ? C10 C9 H9 120.4 . . ? C9 C10 H10 120.6 . . ? C9 C10 C11 118.74(10) . . ? C11 C10 H10 120.6 . . ? C10 C11 H11 120.8 . . ? C12 C11 C10 118.41(10) . . ? C12 C11 H11 120.8 . . ? N2 C12 C11 123.75(10) . . ? N2 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? N1 C13 C7 100.37(7) . . ? N1 C13 C14 109.92(8) . . ? N1 C13 C15 110.88(8) . . ? C7 C13 C14 113.59(8) . . ? C7 C13 C15 110.30(8) . . ? C14 C13 C15 111.31(8) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C6 120.90(9) . . ? C21 C16 C6 119.84(9) . . ? C21 C16 C17 119.25(9) . . ? C16 C17 H17 119.9 . . ? C18 C17 C16 120.13(9) . . ? C18 C17 H17 119.9 . . ? C17 C18 H18 119.8 . . ? C19 C18 C17 120.30(10) . . ? C19 C18 H18 119.8 . . ? C18 C19 H19 120.0 . . ? C18 C19 C20 119.98(10) . . ? C20 C19 H19 120.0 . . ? C19 C20 H20 120.1 . . ? C21 C20 C19 119.79(10) . . ? C21 C20 H20 120.1 . . ? C16 C21 H21 119.7 . . ? C20 C21 C16 120.55(10) . . ? C20 C21 H21 119.7 . . ? C3 C22 H22A 109.5 . . ? C3 C22 H22B 109.5 . . ? C3 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 1.2364(12) . ? N1 C1 1.3934(13) . ? N1 C5 1.3747(12) . ? N1 C13 1.4938(12) . ? N2 C8 1.3432(13) . ? N2 C12 1.3407(13) . ? C1 C2 1.4437(14) . ? C2 H2 0.9500 . ? C2 C3 1.3664(14) . ? C3 C4 1.4228(14) . ? C3 C22 1.5027(14) . ? C4 H4 0.9500 . ? C4 C5 1.3620(14) . ? C5 C6 1.4607(13) . ? C6 C7 1.3470(14) . ? C6 C16 1.4776(13) . ? C7 C8 1.4773(13) . ? C7 C13 1.5227(14) . ? C8 C9 1.3990(14) . ? C9 H9 0.9500 . ? C9 C10 1.3833(15) . ? C10 H10 0.9500 . ? C10 C11 1.3886(15) . ? C11 H11 0.9500 . ? C11 C12 1.3839(15) . ? C12 H12 0.9500 . ? C13 C14 1.5329(14) . ? C13 C15 1.5330(14) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.3959(14) . ? C16 C21 1.3951(14) . ? C17 H17 0.9500 . ? C17 C18 1.3890(14) . ? C18 H18 0.9500 . ? C18 C19 1.3874(15) . ? C19 H19 0.9500 . ? C19 C20 1.3913(16) . ? C20 H20 0.9500 . ? C20 C21 1.3895(14) . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ?