#------------------------------------------------------------------------------ #$Date: 2020-05-13 02:14:59 +0300 (Wed, 13 May 2020) $ #$Revision: 251986 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/83/4038341.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_4038341 loop_ _publ_author_name 'Tsyrenova, Biligma' 'Khrustalev, Victor N.' 'Nenajdenko, Valentine Georgievich' _publ_section_title ; 2H-bis-1,2,3-triazolo-isoquinoline. Design, synthesis and photophysical study. ; _journal_name_full 'The Journal of organic chemistry' _journal_paper_doi 10.1021/acs.joc.0c00263 _journal_year 2020 _chemical_formula_moiety 'C23 H16 N6 O' _chemical_formula_sum 'C23 H16 N6 O' _chemical_formula_weight 392.42 _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 difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 112.346(3) _cell_angle_beta 101.577(3) _cell_angle_gamma 106.514(3) _cell_formula_units_Z 2 _cell_length_a 9.4118(12) _cell_length_b 10.1482(14) _cell_length_c 11.4542(15) _cell_measurement_reflns_used 3403 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 32.54 _cell_measurement_theta_min 3.16 _cell_volume 909.4(2) _computing_cell_refinement 'SAINT (Bruker, 2013)' _computing_data_collection 'APEX3 (Bruker, 2018)' _computing_data_reduction 'SAINT (Bruker, 2013)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2015)' _computing_publication_material 'SHELXTL (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON-III CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_unetI/netI 0.0896 _diffrn_reflns_Laue_measured_fraction_full 0.956 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 15676 _diffrn_reflns_point_group_measured_fraction_full 0.956 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.717 _diffrn_reflns_theta_min 2.619 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_correction_T_min 0.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2016)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.433 _exptl_crystal_description prism _exptl_crystal_F_000 408 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.491 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.089 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 272 _refine_ls_number_reflns 6510 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0792 _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^)+(0.085P)^2^+0.9346P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1899 _refine_ls_wR_factor_ref 0.2167 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4381 _reflns_number_total 6510 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo0c00263_si_002.cif _cod_data_source_block Bil405 _cod_database_code 4038341 _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_min 0.982 _shelx_estimated_absorpt_t_max 0.986 _shelx_res_file ; TITL Bil405 in P-1 Bil405.res created by SHELXL-2018/3 at 12:43:35 on 13-Nov-2019 CELL 0.71073 9.4118 10.1482 11.4542 112.346 101.577 106.514 ZERR 2.000 0.0012 0.0014 0.0015 0.003 0.003 0.003 LATT 1 SFAC C H N O UNIT 46 32 12 2 TEMP -173.0 SIZE 0.15 0.20 0.20 OMIT -2 1 2 OMIT -3 -3 3 OMIT -4 4 0 OMIT -4 2 0 OMIT -7 -4 7 OMIT -2 -7 2 OMIT -5 1 9 OMIT 1 0 3 OMIT -1 2 1 OMIT -2 -6 2 OMIT -1 1 5 OMIT -4 -2 4 OMIT -4 -5 8 OMIT -1 -1 5 OMIT -6 -3 2 OMIT -2 -3 6 OMIT -6 -4 6 OMIT -2 2 2 OMIT -9 -1 1 OMIT -3 -6 7 OMIT -8 -9 4 OMIT 7 1 1 OMIT -1 -4 1 OMIT -12 0 8 OMIT -2 -7 6 OMIT -3 4 3 OMIT -5 -4 1 OMIT -1 5 1 OMIT 0 3 4 OMIT 2 4 2 OMIT 2 -6 2 OMIT -5 -6 9 OMIT -3 1 7 OMIT -2 0 6 OMIT -4 5 8 OMIT -3 -7 3 OMIT -4 -6 8 OMIT -5 -5 9 OMIT -5 -10 1 OMIT -8 -7 4 OMIT 0 5 4 OMIT -6 -10 2 OMIT -4 -3 4 OMIT 1 2 3 OMIT -5 -2 5 OMIT 0 4 4 OMIT -3 -1 3 OMIT 1 3 3 OMIT -2 4 2 OMIT -6 -2 10 OMIT -6 3 2 OMIT 0 -2 4 OMIT 7 -1 1 OMIT 6 -2 2 OMIT 4 2 0 OMIT -8 1 0 OMIT -6 5 2 OMIT -7 -1 7 OMIT -7 2 11 OMIT -6 9 6 OMIT 2 8 6 OMIT 1 1 7 OMIT -7 -9 3 OMIT -2 1 6 OMIT 2 -4 2 OMIT -6 -2 6 OMIT -9 0 1 OMIT -6 3 6 OMIT 6 0 2 OMIT 1 -7 3 OMIT -2 -2 10 OMIT -5 4 5 OMIT -3 -2 11 OMIT -9 -7 5 OMIT -7 7 7 OMIT 3 -1 1 OMIT -2 -5 10 OMIT 1 1 3 OMIT 0 7 4 OMIT -5 -5 1 OMIT -5 -7 9 OMIT -4 6 4 OMIT 4 4 4 OMIT -9 2 9 OMIT 0 2 4 OMIT -4 -3 8 OMIT -3 8 3 OMIT -4 4 4 OMIT -2 -3 2 OMIT -1 1 1 OMIT -9 -3 9 OMIT 1 2 7 OMIT -6 4 2 OMIT -2 2 6 OMIT 4 -2 4 OMIT -5 -1 9 OMIT -4 1 8 OMIT -6 -1 10 OMIT -8 -2 12 OMIT -3 10 3 OMIT -6 -6 6 OMIT -7 3 7 OMIT 4 3 4 OMIT -6 -9 10 OMIT 8 0 0 OMIT -7 2 7 OMIT -9 1 1 OMIT -4 3 8 OMIT -4 -4 8 OMIT -4 6 8 OMIT -9 1 9 L.S. 12 BOND $H ACTA CONF WGHT 0.085000 0.934600 FVAR 1.04850 O1 4 0.978457 0.959720 1.332163 11.00000 0.02480 0.02129 = 0.01236 0.00585 0.00406 0.01102 N1 3 0.923849 0.593635 0.834080 11.00000 0.01728 0.01609 = 0.01657 0.00263 0.00220 0.00740 N2 3 0.874019 0.462213 0.723546 11.00000 0.01340 0.01660 = 0.01679 0.00239 0.00077 0.00633 N3 3 0.720758 0.428350 0.661295 11.00000 0.01359 0.01495 = 0.01268 0.00302 0.00242 0.00646 N4 3 0.645977 0.175592 0.470763 11.00000 0.01468 0.01407 = 0.01319 0.00304 0.00317 0.00558 N5 3 0.501796 0.082206 0.375159 11.00000 0.01441 0.01223 = 0.01304 0.00227 0.00216 0.00572 N6 3 0.387739 0.135347 0.384444 11.00000 0.01499 0.01472 = 0.01431 0.00480 0.00483 0.00775 C1 1 0.804930 0.644246 0.843348 11.00000 0.01631 0.01604 = 0.01235 0.00525 0.00393 0.00737 C2 1 0.670116 0.538343 0.731601 11.00000 0.01630 0.01264 = 0.01233 0.00462 0.00407 0.00663 C3 1 0.505339 0.515595 0.683181 11.00000 0.01659 0.01370 = 0.01231 0.00424 0.00483 0.00638 C4 1 0.443873 0.616504 0.756826 11.00000 0.01838 0.01838 = 0.01795 0.00653 0.00721 0.00944 AFIX 43 H4 2 0.511850 0.704859 0.840171 11.00000 -1.20000 AFIX 0 C5 1 0.286347 0.589132 0.709872 11.00000 0.02179 0.02283 = 0.02160 0.00758 0.01144 0.01406 AFIX 43 H5 2 0.247008 0.658744 0.761252 11.00000 -1.20000 AFIX 0 C6 1 0.183718 0.460212 0.587583 11.00000 0.01689 0.02115 = 0.02191 0.00897 0.00641 0.01012 AFIX 43 H6 2 0.075534 0.443065 0.555518 11.00000 -1.20000 AFIX 0 C7 1 0.240006 0.358156 0.513762 11.00000 0.01583 0.01667 = 0.01672 0.00494 0.00410 0.00773 AFIX 43 H7 2 0.170573 0.270333 0.430575 11.00000 -1.20000 AFIX 0 C8 1 0.399113 0.383571 0.561024 11.00000 0.01500 0.01382 = 0.01300 0.00566 0.00503 0.00759 C9 1 0.461540 0.274156 0.493907 11.00000 0.01444 0.01504 = 0.01303 0.00621 0.00485 0.00704 C10 1 0.618458 0.295478 0.544495 11.00000 0.01376 0.01335 = 0.01149 0.00341 0.00284 0.00491 C11 1 0.470847 -0.068734 0.275009 11.00000 0.01759 0.01078 = 0.01094 0.00212 0.00455 0.00557 C12 1 0.587811 -0.125847 0.282521 11.00000 0.01503 0.01585 = 0.01597 0.00443 0.00458 0.00595 AFIX 43 H12 2 0.688019 -0.065153 0.352523 11.00000 -1.20000 AFIX 0 C13 1 0.554438 -0.274850 0.184529 11.00000 0.01971 0.01488 = 0.02010 0.00604 0.00832 0.00845 AFIX 43 H13 2 0.633042 -0.316248 0.187577 11.00000 -1.20000 AFIX 0 C14 1 0.407826 -0.363480 0.082570 11.00000 0.02176 0.01366 = 0.01649 0.00233 0.00666 0.00613 AFIX 43 H14 2 0.386113 -0.465064 0.016454 11.00000 -1.20000 AFIX 0 C15 1 0.293136 -0.302936 0.077714 11.00000 0.01909 0.01526 = 0.01462 0.00305 0.00190 0.00492 AFIX 43 H15 2 0.192834 -0.363395 0.007812 11.00000 -1.20000 AFIX 0 C16 1 0.323621 -0.155028 0.173951 11.00000 0.01612 0.01540 = 0.01389 0.00468 0.00452 0.00674 AFIX 43 H16 2 0.245106 -0.113535 0.170740 11.00000 -1.20000 AFIX 0 C17 1 0.831966 0.787100 0.962093 11.00000 0.01645 0.01343 = 0.01256 0.00379 0.00259 0.00491 C18 1 0.899236 0.803776 1.089717 11.00000 0.01619 0.01252 = 0.01565 0.00506 0.00474 0.00625 AFIX 43 H18 2 0.929693 0.725660 1.098943 11.00000 -1.20000 AFIX 0 C19 1 0.921373 0.935213 1.203103 11.00000 0.01471 0.01755 = 0.01141 0.00407 0.00328 0.00506 C20 1 0.879069 1.051147 1.189962 11.00000 0.02093 0.01651 = 0.01620 0.00367 0.00417 0.00788 AFIX 43 H20 2 0.893162 1.140476 1.267684 11.00000 -1.20000 AFIX 0 C21 1 0.816282 1.035173 1.062672 11.00000 0.02378 0.01425 = 0.01728 0.00531 0.00413 0.00904 AFIX 43 H21 2 0.789381 1.115037 1.053530 11.00000 -1.20000 AFIX 0 C22 1 0.792300 0.903598 0.948356 11.00000 0.02148 0.01495 = 0.01484 0.00475 0.00331 0.00729 AFIX 43 H22 2 0.749092 0.893325 0.861408 11.00000 -1.20000 AFIX 0 C23 1 1.025658 0.845933 1.352324 11.00000 0.02545 0.02499 = 0.01733 0.01085 0.00506 0.01239 AFIX 137 H23A 2 1.056483 0.873433 1.448167 11.00000 -1.50000 H23B 2 1.115597 0.842271 1.322370 11.00000 -1.50000 H23C 2 0.937302 0.743970 1.300277 11.00000 -1.50000 AFIX 0 HKLF 4 REM Bil405 in P-1 REM wR2 = 0.216731, GooF = S = 1.05332, Restrained GooF = 1.05332 for all data REM R1 = 0.079218 for 4381 Fo > 4sig(Fo) and 0.120174 for all 6510 data REM 272 parameters refined using 0 restraints END WGHT 0.0850 0.9346 REM Highest difference peak 0.491, deepest hole -0.379, 1-sigma level 0.089 Q1 1 0.5950 0.5284 0.7405 11.00000 0.05 0.49 Q2 1 0.8625 0.8140 1.0369 11.00000 0.05 0.45 Q3 1 0.3209 0.3776 0.5468 11.00000 0.05 0.43 Q4 1 0.3754 0.6443 0.7400 11.00000 0.05 0.43 Q5 1 0.7452 0.9623 1.0879 11.00000 0.05 0.42 Q6 1 0.5433 -0.0837 0.2966 11.00000 0.05 0.42 Q7 1 0.3580 -0.3228 0.0959 11.00000 0.05 0.42 Q8 1 0.2296 0.5236 0.6456 11.00000 0.05 0.41 Q9 1 0.8582 0.6223 0.8098 11.00000 0.05 0.41 Q10 1 0.2145 0.4195 0.5409 11.00000 0.05 0.40 Q11 1 0.4291 0.4396 0.6235 11.00000 0.05 0.40 Q12 1 0.6495 0.2396 0.5141 11.00000 0.05 0.39 Q13 1 0.1228 -0.5409 -0.0216 11.00000 0.05 0.39 Q14 1 0.6681 0.9155 0.9381 11.00000 0.05 0.38 Q15 1 0.6229 0.8333 0.8123 11.00000 0.05 0.38 Q16 1 1.0220 0.5621 1.0996 11.00000 0.05 0.37 Q17 1 0.9452 0.8712 1.1628 11.00000 0.05 0.37 Q18 1 0.4494 0.3504 0.5308 11.00000 0.05 0.37 Q19 1 0.7180 0.1542 0.3935 11.00000 0.05 0.36 Q20 1 0.3766 0.5264 0.5316 11.00000 0.05 0.36 ; _shelx_res_checksum 1639 _shelx_hkl_file ; -2 0 0 291.17 14.80 2 0 0 307.67 18.30 -3 0 0 249.68 15.60 3 0 0 274.67 17.00 -4 0 0 60.69 8.20 4 0 0 55.09 9.60 -5 0 0 -2.00 1.80 5 0 0 4.80 3.60 -6 0 0 5.80 3.90 6 0 0 6.50 5.20 -7 0 0 8.80 5.10 7 0 0 14.00 5.80 -8 0 0 46.50 12.40 8 0 0 63.49 12.90 -9 0 0 28.50 10.10 9 0 0 23.20 9.80 -10 0 0 180.28 24.10 10 0 0 194.48 25.10 -11 0 0 12.80 8.10 11 0 0 12.80 11.10 -12 0 0 24.10 11.20 12 0 0 13.00 12.40 13 -1 0 41.70 15.70 -13 1 0 38.00 15.60 12 -1 0 -3.30 8.60 -12 1 0 12.90 7.60 11 -1 0 23.90 11.60 -11 1 0 15.40 9.30 10 -1 0 2.10 7.20 -10 1 0 4.40 3.80 9 -1 0 6.00 6.20 -9 1 0 9.00 6.70 -8 1 0 116.29 16.00 7 -1 0 109.99 15.60 -7 1 0 108.99 14.90 6 -1 0 461.75 30.70 -6 1 0 458.45 29.40 5 -1 0 680.43 36.20 -5 1 0 636.84 33.50 4 -1 0 913.31 41.50 -4 1 0 873.01 39.00 3 -1 0 554.84 27.20 3 -1 0 554.44 19.00 -3 1 0 522.75 24.50 -3 1 0 541.65 19.50 2 -1 0 6298.27 192.28 -2 1 0 5970.20 195.78 -2 1 0 6208.38 192.38 -1 1 0 1448.36 47.60 -1 -1 0 505.05 20.70 -1 -1 0 512.35 20.90 -1 -1 0 549.15 18.60 1 1 0 487.05 20.70 1 1 0 510.45 18.50 1 1 0 530.75 21.00 -2 -1 0 1.40 0.90 -2 -1 0 -1.00 1.40 2 1 0 -0.40 0.80 2 1 0 1.00 1.30 -3 -1 0 307.47 19.00 -3 -1 0 320.37 12.20 3 1 0 324.97 12.40 3 1 0 320.77 19.20 -4 -1 0 879.61 40.80 4 1 0 818.02 39.90 -5 -1 0 -0.40 2.70 5 1 0 -0.60 2.70 -6 -1 0 6.90 4.30 6 1 0 9.10 5.30 -7 -1 0 27.70 9.40 7 1 0 31.90 10.50 -8 -1 0 99.99 17.70 8 1 0 101.09 18.90 -9 -1 0 91.09 19.90 9 1 0 136.49 25.70 -10 -1 0 13.30 8.10 10 1 0 13.40 10.20 -11 -1 0 27.10 17.10 11 1 0 8.70 11.80 -12 -1 0 65.99 19.20 12 1 0 45.50 15.90 13 -2 0 239.38 32.00 -13 2 0 130.99 27.40 12 -2 0 28.60 14.30 -12 2 0 20.80 12.40 11 -2 0 -12.50 6.30 -11 2 0 2.30 6.20 10 -2 0 25.70 11.00 -10 2 0 35.70 10.80 9 -2 0 172.78 21.10 -9 2 0 155.38 20.10 8 -2 0 614.94 40.60 -8 2 0 576.54 38.30 7 -2 0 428.16 31.90 -7 2 0 448.66 30.40 6 -2 0 -3.20 3.00 -6 2 0 1.40 2.50 5 -2 0 54.49 11.10 5 -2 0 56.49 4.50 -5 2 0 74.89 5.20 -5 2 0 61.89 10.70 -4 2 0 1195.98 48.20 3 -2 0 123.29 7.40 -3 2 0 117.19 9.10 -3 2 0 117.59 9.40 2 -2 0 353.26 15.20 -2 2 0 341.27 15.90 -2 2 0 339.17 16.20 1 -2 0 1370.36 45.40 1 -2 0 1271.27 44.50 1 -2 0 1268.17 44.40 -1 2 0 1315.27 44.60 -1 2 0 1275.27 44.50 0 -2 0 1393.86 46.90 0 -2 0 1425.66 47.60 0 -2 0 1246.58 46.90 0 2 0 1369.56 47.50 0 2 0 1377.66 47.00 -1 -2 0 430.56 21.30 -1 -2 0 484.05 21.60 1 2 0 475.15 20.70 -2 -2 0 481.55 24.00 2 2 0 465.25 23.30 -3 -2 0 300.07 19.60 -3 -2 0 282.27 16.80 3 2 0 307.67 19.60 -4 -2 0 760.42 37.60 -4 -2 0 600.34 25.40 4 2 0 763.22 37.40 -5 -2 0 286.27 22.90 5 2 0 282.67 22.70 -6 -2 0 234.08 21.80 6 2 0 205.08 20.90 -7 -2 0 83.89 15.90 7 2 0 93.99 18.00 -8 -2 0 103.39 19.50 8 2 0 90.49 18.60 -9 -2 0 10.00 6.50 9 2 0 23.70 9.80 -10 -2 0 86.39 21.20 10 2 0 73.19 19.50 -11 -2 0 102.39 24.10 11 2 0 79.79 20.90 13 -3 0 185.98 34.10 -13 3 0 165.78 32.10 12 -3 0 236.78 29.80 -12 3 0 228.28 29.20 11 -3 0 3.70 7.80 -11 3 0 -1.90 5.80 10 -3 0 2.00 7.10 9 -3 0 191.48 22.90 -9 3 0 195.58 21.60 8 -3 0 46.10 12.70 -8 3 0 47.90 11.60 7 -3 0 5.60 5.30 7 -3 0 8.40 2.40 -7 3 0 0.40 3.80 6 -3 0 779.02 43.20 6 -3 0 773.22 29.70 -6 3 0 723.63 40.90 5 -3 0 78.39 6.60 -5 3 0 71.39 9.50 -5 3 0 68.39 9.00 4 -3 0 1935.11 66.69 -4 3 0 1913.41 71.19 -4 3 0 1909.81 70.69 3 -3 0 128.79 9.10 -3 3 0 120.79 9.50 -3 3 0 120.99 9.90 -2 3 0 17.00 3.60 -2 3 0 13.80 3.20 1 -3 0 28.50 4.80 -1 3 0 28.30 3.70 -1 3 0 24.60 4.40 0 -3 0 35.40 4.80 0 -3 0 33.00 5.20 0 3 0 38.30 4.70 -1 -3 0 1.50 1.40 1 3 0 0.70 1.60 -2 -3 0 60.69 8.50 -2 -3 0 70.69 6.50 2 3 0 63.59 7.80 -3 -3 0 75.39 6.70 -3 -3 0 69.39 10.00 3 3 0 67.49 10.90 -4 -3 0 27.30 4.70 -4 -3 0 34.80 9.00 4 3 0 23.30 7.10 -5 -3 0 185.48 10.90 -5 -3 0 179.58 18.90 5 3 0 189.18 18.60 -6 -3 0 1672.43 78.19 6 3 0 1701.33 77.39 7 3 0 132.99 21.70 -8 -3 0 3.50 9.10 8 3 0 4.70 7.20 -9 -3 0 59.29 17.40 9 3 0 77.79 19.90 10 3 0 -1.00 8.70 -11 -3 0 46.30 15.60 11 3 0 37.90 16.80 13 -4 0 119.69 25.30 -13 4 0 116.39 24.10 12 -4 0 9.30 8.80 -12 4 0 14.60 7.50 11 -4 0 28.30 12.20 -11 4 0 9.00 8.40 10 -4 0 -2.60 5.10 -10 4 0 -0.10 5.40 9 -4 0 164.68 20.40 -9 4 0 153.78 19.00 8 -4 0 -0.20 2.00 8 -4 0 11.20 5.50 -8 4 0 -1.00 3.50 7 -4 0 80.19 7.50 7 -4 0 49.40 12.00 -7 4 0 82.29 14.30 6 -4 0 683.93 29.80 -6 4 0 711.13 37.50 5 -4 0 5.60 3.00 -5 4 0 13.30 5.30 -5 4 0 11.40 4.40 -4 4 0 2369.46 85.19 3 -4 0 1219.98 46.70 -3 4 0 1197.18 46.60 -3 4 0 1164.98 46.80 2 -4 0 0.10 1.50 -2 4 0 5.60 2.70 -2 4 0 3.30 1.80 1 -4 0 472.25 23.50 -1 4 0 489.75 23.30 -1 4 0 498.55 22.90 0 -4 0 1358.46 54.99 0 -4 0 1520.65 56.39 0 4 0 1566.74 55.89 -1 -4 0 192.28 12.80 -1 -4 0 185.98 14.30 1 4 0 163.88 12.90 -2 -4 0 230.78 14.60 -2 -4 0 224.08 17.80 2 4 0 226.28 16.80 -3 -4 0 19.10 6.90 -3 -4 0 31.30 5.80 3 4 0 23.60 6.80 -4 -4 0 77.39 13.90 -4 -4 0 79.89 8.10 4 4 0 81.79 14.10 -5 -4 0 499.95 34.50 -5 -4 0 495.55 23.50 5 4 0 466.35 32.70 -6 -4 0 213.58 12.60 -6 -4 0 207.78 23.40 6 4 0 198.28 21.60 -7 -4 0 4.10 5.30 7 4 0 -3.60 4.10 -8 -4 0 32.40 10.80 8 4 0 5.00 7.20 -9 -4 0 13.90 9.00 9 4 0 7.80 9.50 -10 -4 0 108.49 25.20 10 4 0 113.09 24.50 13 -5 0 7.00 12.00 -13 5 0 26.20 10.90 12 -5 0 183.28 24.80 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42.80 13.20 -3 14 -1 -1.20 9.20 -3 14 -1 10.40 9.60 3 -14 1 -13.10 7.10 -4 14 -1 13.80 10.50 -4 14 -1 3.80 8.10 4 -14 1 29.30 11.00 -5 14 -1 -11.20 8.00 -5 14 -1 26.90 11.30 5 -14 1 4.70 8.40 -6 14 -1 4.30 8.70 -6 14 -1 2.70 8.50 6 -14 1 12.30 8.50 -7 14 -1 9.40 7.80 -7 14 -1 3.70 9.60 7 -14 1 6.60 7.50 -8 14 -1 191.58 27.70 8 -14 1 187.38 28.60 1 13 -1 65.89 15.70 0 13 -1 30.70 10.70 0 13 -1 12.60 11.50 0 -13 1 10.20 9.00 -1 13 -1 44.30 11.90 -1 13 -1 10.50 10.40 1 -13 1 37.60 12.90 -2 13 -1 22.20 9.90 -2 13 -1 -16.60 7.10 2 -13 1 -6.50 6.40 -3 13 -1 20.10 8.70 -3 13 -1 3.40 8.10 -4 13 -1 46.00 12.10 -4 13 -1 64.49 16.70 4 -13 1 82.89 23.80 -5 13 -1 26.10 10.90 5 -13 1 32.40 14.30 -6 13 -1 13.50 8.40 -6 13 -1 22.80 9.30 6 -13 1 18.40 14.90 -7 13 -1 49.30 12.30 -7 13 -1 30.10 10.10 -8 13 -1 39.10 10.80 -8 13 -1 20.20 8.50 8 -13 1 22.00 11.30 -9 13 -1 25.20 10.90 -9 13 -1 53.29 14.80 9 -13 1 20.60 9.20 -10 13 -1 81.89 18.30 -10 13 -1 75.49 18.80 10 -13 1 63.59 17.70 2 12 -1 5.80 7.90 2 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22.60 7.80 -2 -11 4 11.80 7.20 1 11 -4 13.30 6.30 1 11 -4 12.80 6.90 -1 -11 4 0.70 4.90 0 11 -4 186.68 16.60 0 11 -4 235.78 25.10 0 -11 4 179.88 21.40 -1 11 -4 273.57 31.80 -1 11 -4 290.67 20.10 1 -11 4 313.07 27.80 -2 11 -4 7.60 4.90 -2 11 -4 17.20 9.00 2 -11 4 12.20 6.00 -3 11 -4 34.80 7.10 -3 11 -4 31.60 10.60 3 -11 4 38.70 11.00 -4 11 -4 3.00 3.90 -5 11 -4 -2.10 3.60 -6 11 -4 -6.70 3.70 -6 11 -4 -7.50 5.90 6 -11 4 -6.30 3.00 -7 11 -4 16.20 8.70 -7 11 -4 20.70 8.00 7 -11 4 8.00 5.80 -8 11 -4 40.20 14.60 -8 11 -4 17.60 7.50 8 -11 4 9.00 7.30 -9 11 -4 1.60 8.50 -9 11 -4 14.30 5.90 9 -11 4 -4.30 4.90 -10 11 -4 106.59 21.60 -10 11 -4 83.99 18.90 10 -11 4 107.69 14.60 -11 11 -4 -8.60 8.70 -11 11 -4 27.80 10.40 11 -11 4 -10.80 8.00 -12 11 -4 110.39 24.40 -12 11 -4 103.89 21.30 12 -11 4 99.99 27.80 7 10 -4 54.19 21.10 -7 -10 4 77.29 21.70 6 10 -4 149.49 31.10 -6 -10 4 131.59 22.70 5 10 -4 153.88 28.20 -5 -10 4 109.59 18.60 -5 -10 4 144.59 16.10 4 10 -4 58.09 15.40 -4 -10 4 30.50 10.70 -4 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48.30 12.90 5 9 -4 225.38 28.40 -5 -9 4 263.47 21.10 -5 -9 4 262.17 25.50 4 9 -4 6.40 6.90 -4 -9 4 2.90 6.40 -4 -9 4 2.00 3.80 3 9 -4 119.49 21.00 -3 -9 4 107.69 14.50 -3 -9 4 106.89 13.80 2 9 -4 21.50 8.20 -2 -9 4 20.40 7.20 -2 -9 4 33.80 8.80 1 9 -4 72.39 15.00 -1 -9 4 91.99 15.70 -1 9 -4 12.40 4.70 -1 9 -4 21.00 8.20 1 -9 4 13.90 6.30 -2 9 -4 322.87 27.00 2 -9 4 387.66 27.90 -3 9 -4 268.87 25.10 3 -9 4 316.97 24.60 4 -9 4 21.90 7.30 -5 9 -4 14.40 7.70 -5 9 -4 27.10 6.40 5 -9 4 31.50 8.00 -6 9 -4 -2.30 4.00 -6 9 -4 15.10 7.30 6 -9 4 2.90 4.00 -7 9 -4 156.98 15.60 -7 9 -4 125.09 24.70 7 -9 4 148.69 16.40 -8 9 -4 114.89 20.70 -8 9 -4 100.69 14.30 8 -9 4 148.59 15.70 -9 9 -4 6.20 8.60 -9 9 -4 6.10 5.70 9 -9 4 19.20 7.00 -10 9 -4 86.79 17.20 -10 9 -4 62.19 17.20 10 -9 4 51.99 11.00 -11 9 -4 112.59 22.70 -11 9 -4 91.69 17.20 11 -9 4 96.99 14.10 -12 9 -4 40.40 13.80 12 -9 4 73.89 25.70 8 8 -4 60.79 19.50 -8 -8 4 51.49 16.60 7 8 -4 -5.20 7.40 -7 -8 4 -13.70 6.00 -7 -8 4 -1.60 5.40 6 8 -4 3.50 7.40 -6 -8 4 3.10 4.80 -6 -8 4 2.10 6.60 5 8 -4 -3.90 4.60 -5 -8 4 8.00 4.40 -5 -8 4 11.40 5.10 -4 -8 4 10.00 7.20 -4 -8 4 1.90 3.70 3 8 -4 0.20 4.80 -3 -8 4 5.50 4.90 -3 -8 4 -1.20 3.00 2 8 -4 185.88 19.80 -2 -8 4 207.58 18.60 -2 -8 4 152.18 15.00 1 8 -4 189.78 20.20 -1 -8 4 223.28 15.90 -1 -8 4 228.58 19.80 0 8 -4 32.40 8.70 0 -8 4 21.00 6.90 -1 8 -4 51.19 11.60 1 -8 4 36.30 8.40 -2 8 -4 72.89 14.10 2 -8 4 103.89 13.20 -3 8 -4 136.79 16.70 3 -8 4 120.79 14.10 -4 8 -4 16.90 6.80 -4 8 -4 8.70 3.00 4 -8 4 5.70 4.60 -5 8 -4 33.60 6.60 -5 8 -4 32.70 10.70 5 -8 4 24.20 6.80 -6 8 -4 481.85 27.40 -6 8 -4 455.75 35.10 6 -8 4 518.85 31.20 -7 8 -4 404.16 27.20 -7 8 -4 420.16 34.40 7 -8 4 465.15 29.10 -8 8 -4 41.00 13.40 -8 8 -4 54.69 11.60 8 -8 4 53.19 10.70 -9 8 -4 16.60 9.90 -9 8 -4 17.00 7.00 9 -8 4 19.20 7.20 -10 8 -4 0.20 5.20 -10 8 -4 -6.50 6.50 -11 8 -4 42.80 13.10 11 -8 4 2.50 11.40 -12 8 -4 -8.60 8.10 12 -8 4 11.80 13.00 9 7 -4 -7.80 8.10 -9 -7 4 -11.50 8.30 8 7 -4 219.58 28.30 -8 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14.20 4 -15 5 8.50 8.80 -5 15 -5 119.89 27.60 5 -15 5 121.09 24.30 -6 15 -5 -1.50 10.70 6 -15 5 1.10 7.50 7 -15 5 6.20 9.20 1 14 -5 2.80 10.40 -1 -14 5 6.70 7.70 0 -14 5 22.60 11.40 -1 14 -5 69.49 18.00 1 -14 5 71.89 18.10 -2 14 -5 33.90 15.10 2 -14 5 32.50 11.20 -3 14 -5 16.60 10.70 3 -14 5 -2.20 7.20 -4 14 -5 3.10 8.60 4 -14 5 1.00 6.60 -5 14 -5 -12.90 8.80 5 -14 5 -6.90 5.70 -6 14 -5 -8.70 10.30 6 -14 5 -3.20 7.70 -7 14 -5 78.89 22.30 7 -14 5 89.89 19.40 -8 14 -5 40.20 16.00 8 -14 5 15.80 11.40 -9 14 -5 28.10 17.60 9 -14 5 71.09 16.30 3 13 -5 -0.40 11.60 -3 -13 5 -13.40 7.20 -2 -13 5 17.00 14.30 1 13 -5 -10.60 6.70 -1 -13 5 -3.50 5.30 0 13 -5 188.18 25.80 0 -13 5 174.58 26.90 -1 13 -5 81.09 17.60 1 -13 5 105.99 21.30 -2 13 -5 2.50 6.70 2 -13 5 -5.10 6.40 -3 13 -5 11.60 9.00 3 -13 5 29.20 11.10 -4 13 -5 11.90 7.70 4 -13 5 1.70 6.10 -5 13 -5 187.78 25.00 5 -13 5 172.88 26.50 -6 13 -5 -13.40 7.10 6 -13 5 -3.60 5.80 -7 13 -5 31.60 12.00 7 -13 5 38.30 13.20 -8 13 -5 -1.20 8.00 8 -13 5 3.00 9.50 -9 13 -5 17.10 12.10 9 -13 5 5.40 7.00 -10 13 -5 323.67 36.90 10 -13 5 309.57 36.30 4 12 -5 32.50 16.40 -4 -12 5 32.70 13.10 3 12 -5 1.80 9.00 3 12 -5 13.80 8.30 -3 -12 5 3.90 6.80 2 12 -5 29.80 13.20 -2 -12 5 63.39 13.60 1 12 -5 22.80 10.80 -1 -12 5 24.80 9.70 0 12 -5 64.89 17.30 0 -12 5 75.79 16.20 -1 12 -5 9.20 7.80 1 -12 5 1.30 4.50 -2 12 -5 2.20 5.90 2 -12 5 0.80 6.00 -3 12 -5 4.10 6.90 3 -12 5 1.00 4.30 -4 12 -5 137.39 23.60 4 -12 5 107.09 18.20 -5 12 -5 232.08 26.30 5 -12 5 218.18 24.80 -6 12 -5 2.90 8.70 6 -12 5 20.70 9.50 -7 12 -5 -1.30 8.20 -7 12 -5 2.60 8.90 7 -12 5 7.20 7.30 -8 12 -5 95.59 20.20 8 -12 5 101.49 17.90 -9 12 -5 18.50 11.20 9 -12 5 5.70 8.80 -10 12 -5 146.89 29.70 10 -12 5 153.58 20.50 -11 12 -5 33.00 16.80 11 -12 5 27.60 11.40 6 11 -5 25.30 12.10 -6 -11 5 37.70 13.90 -6 -11 5 11.20 8.80 5 11 -5 55.59 20.00 -5 -11 5 67.99 13.70 -5 -11 5 51.49 12.90 4 11 -5 160.48 28.40 -4 -11 5 177.88 19.70 3 11 -5 37.70 13.60 -3 -11 5 16.70 6.80 -3 -11 5 20.90 7.60 2 11 -5 -3.90 6.20 -2 -11 5 -3.10 4.20 1 11 -5 3.50 4.90 -1 -11 5 -0.60 5.10 0 11 -5 72.89 16.30 0 -11 5 73.59 15.60 -1 11 -5 8.20 6.50 1 -11 5 -5.10 3.60 2 -11 5 11.80 6.50 3 -11 5 641.54 42.20 -4 11 -5 242.58 26.40 4 -11 5 216.48 22.80 -5 11 -5 23.20 10.20 5 -11 5 14.40 7.60 -6 11 -5 225.28 26.10 6 -11 5 212.98 22.80 -7 11 -5 3.90 6.90 -7 11 -5 1.40 6.30 7 -11 5 4.80 4.50 -8 11 -5 64.49 17.30 8 -11 5 65.09 13.50 -9 11 -5 7.20 6.60 -9 11 -5 16.60 10.90 9 -11 5 1.80 5.30 -10 11 -5 -0.40 9.20 -10 11 -5 7.10 9.10 10 -11 5 12.40 6.10 -11 11 -5 4.10 8.40 -11 11 -5 20.10 14.30 11 -11 5 13.00 8.60 7 10 -5 15.70 11.40 -7 -10 5 19.40 11.40 6 10 -5 59.29 31.20 -6 -10 5 75.39 17.20 -6 -10 5 125.99 15.00 5 10 -5 13.40 8.80 -5 -10 5 0.20 8.20 -5 -10 5 1.00 5.00 4 10 -5 4.70 6.60 -4 -10 5 7.10 5.80 -4 -10 5 12.40 6.40 3 10 -5 76.69 18.30 -3 -10 5 131.79 15.10 -3 -10 5 123.19 16.20 2 10 -5 1.80 5.90 -2 -10 5 2.40 5.60 -2 -10 5 0.30 5.70 1 10 -5 53.99 9.10 -1 -10 5 62.59 18.70 0 10 -5 18.40 8.40 0 -10 5 13.50 6.00 -1 10 -5 18.30 8.00 1 -10 5 7.90 6.40 -2 10 -5 0.00 5.10 2 -10 5 11.80 5.40 -3 10 -5 94.29 17.90 3 -10 5 59.99 12.90 -4 10 -5 448.66 35.20 4 -10 5 421.16 31.60 -5 10 -5 104.69 19.10 5 -10 5 90.59 16.20 -6 10 -5 92.59 10.40 -6 10 -5 84.69 16.90 -7 10 -5 8.50 7.40 7 -10 5 -0.30 4.10 -8 10 -5 20.60 8.00 -8 10 -5 1.20 7.40 8 -10 5 19.20 7.20 -9 10 -5 10.30 6.60 -9 10 -5 19.50 11.90 9 -10 5 22.30 8.00 -10 10 -5 -1.90 8.30 10 -10 5 6.20 5.70 -11 10 -5 41.30 12.20 -11 10 -5 53.39 16.70 11 -10 5 46.70 9.60 -12 10 -5 20.10 10.90 12 -10 5 18.70 14.40 8 9 -5 -2.70 10.50 7 9 -5 3.50 16.60 -7 -9 5 7.70 8.40 -7 -9 5 16.70 8.30 6 9 -5 110.59 24.00 -6 -9 5 85.39 15.90 -6 -9 5 119.09 13.90 5 9 -5 13.70 7.80 -5 -9 5 18.80 6.50 -5 -9 5 8.20 7.20 4 9 -5 263.47 28.60 -4 -9 5 289.47 23.50 -4 -9 5 249.08 23.20 3 9 -5 -3.20 3.70 -3 -9 5 7.70 4.80 -3 -9 5 -5.80 4.50 2 9 -5 32.00 10.00 -2 -9 5 53.79 10.40 -2 -9 5 37.50 10.10 1 9 -5 49.90 12.10 1 9 -5 59.39 9.20 -1 -9 5 68.39 13.10 0 -9 5 5.30 3.60 -1 9 -5 184.38 20.30 1 -9 5 174.98 18.10 -2 9 -5 412.16 31.60 2 -9 5 437.86 30.00 -3 9 -5 48.50 11.60 3 -9 5 53.59 10.70 -4 9 -5 6.70 5.80 4 -9 5 -1.10 3.10 -5 9 -5 45.80 7.20 -5 9 -5 41.50 11.30 5 -9 5 44.20 11.00 -6 9 -5 334.27 20.60 -6 9 -5 334.17 30.50 6 -9 5 300.67 24.70 -7 9 -5 284.87 28.70 -7 9 -5 278.47 20.90 7 -9 5 254.97 22.40 -8 9 -5 2.20 5.70 -8 9 -5 11.80 8.50 8 -9 5 8.90 5.70 -9 9 -5 0.60 7.30 -9 9 -5 -6.40 6.00 9 -9 5 10.10 5.80 -10 9 -5 5.20 9.00 -10 9 -5 28.50 9.20 10 -9 5 17.80 7.60 -11 9 -5 162.18 25.10 -11 9 -5 246.48 31.60 11 -9 5 169.58 17.30 -12 9 -5 10.30 11.90 12 -9 5 -3.30 14.30 9 8 -5 14.80 12.80 -9 -8 5 28.60 13.60 8 8 -5 -5.60 7.70 -8 -8 5 3.00 8.00 7 8 -5 45.10 16.20 -7 -8 5 98.69 17.70 6 8 -5 18.90 10.30 -6 -8 5 22.00 7.30 5 8 -5 32.50 10.80 -5 -8 5 61.39 12.70 -5 -8 5 45.50 10.10 4 8 -5 74.19 22.10 -4 -8 5 79.49 13.40 -4 -8 5 84.69 14.90 3 8 -5 -7.10 4.00 -3 -8 5 -1.20 5.00 -3 -8 5 3.70 3.10 2 8 -5 142.19 18.60 -2 -8 5 173.28 14.00 -2 -8 5 166.48 16.90 1 8 -5 113.09 15.80 -1 -8 5 117.29 9.90 -1 -8 5 125.49 14.60 0 8 -5 209.68 20.90 0 -8 5 207.38 19.00 -1 8 -5 84.89 15.50 1 -8 5 88.39 12.30 -2 8 -5 172.88 18.50 2 -8 5 141.99 15.90 -3 8 -5 145.89 17.10 3 -8 5 98.89 13.10 -4 8 -5 52.69 13.00 4 -8 5 64.99 12.50 -5 8 -5 31.50 5.60 -5 8 -5 42.00 12.50 5 -8 5 21.50 7.40 -6 8 -5 169.98 15.10 -6 8 -5 186.68 21.90 6 -8 5 202.18 18.40 -7 8 -5 3.00 4.40 7 -8 5 11.70 4.80 -8 8 -5 17.30 7.00 -8 8 -5 27.10 10.10 8 -8 5 14.80 5.40 -9 8 -5 8.80 6.70 -9 8 -5 18.70 12.90 9 -8 5 3.10 4.80 -10 8 -5 11.50 8.50 -10 8 -5 -0.80 5.60 10 -8 5 -0.60 4.50 -11 8 -5 101.89 19.50 -12 8 -5 156.28 25.80 12 -8 5 213.58 38.20 10 7 -5 15.20 13.20 -10 -7 5 6.50 11.10 9 7 -5 100.19 24.20 -9 -7 5 73.89 18.30 8 7 -5 4.10 6.80 -8 -7 5 -12.00 6.00 7 7 -5 158.58 27.30 -7 -7 5 135.39 13.30 -7 -7 5 151.28 23.90 6 7 -5 0.60 6.60 -6 -7 5 -0.70 5.00 -6 -7 5 14.50 5.50 -5 -7 5 119.09 15.60 -5 -7 5 107.59 13.50 4 7 -5 4.00 3.30 -4 -7 5 4.00 3.80 -4 -7 5 -5.80 3.40 3 7 -5 271.77 25.10 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106.49 14.80 2 10 -7 31.60 12.20 -2 -10 7 42.10 11.40 1 10 -7 48.10 13.70 -1 -10 7 34.90 10.60 0 10 -7 8.00 6.50 0 -10 7 -1.70 4.40 1 -10 7 11.80 10.70 -2 10 -7 48.80 15.70 2 -10 7 51.19 17.40 -3 10 -7 23.30 13.90 3 -10 7 28.00 11.30 -4 10 -7 2.90 5.10 4 -10 7 10.30 5.60 -5 10 -7 79.59 18.60 5 -10 7 82.29 15.80 -6 10 -7 351.66 34.90 6 -10 7 433.26 31.40 -7 10 -7 132.39 26.80 7 -10 7 105.79 17.00 -8 10 -7 68.49 19.30 8 -10 7 50.69 11.30 -9 10 -7 -4.90 6.70 -9 10 -7 18.70 11.50 9 -10 7 15.10 7.90 -10 10 -7 103.79 22.90 10 -10 7 132.19 16.30 -11 10 -7 -20.70 9.20 -11 10 -7 14.20 11.30 8 9 -7 -1.60 10.80 -8 -9 7 -7.10 10.30 -7 -9 7 34.50 10.60 -7 -9 7 10.30 6.50 -6 -9 7 8.90 6.30 -6 -9 7 -10.50 4.40 5 9 -7 6.00 6.00 -5 -9 7 3.00 4.50 4 9 -7 8.40 7.50 -4 -9 7 15.70 7.40 -4 -9 7 18.90 6.80 3 9 -7 268.57 28.20 -3 -9 7 261.97 18.50 -3 -9 7 259.97 22.80 -2 -9 7 85.89 14.80 1 9 -7 0.30 4.70 -1 -9 7 -5.40 2.50 0 9 -7 4.00 4.40 0 -9 7 0.20 3.40 -1 9 -7 10.40 5.50 1 -9 7 -2.80 3.10 -2 9 -7 2.40 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1.20 5.90 -4 -6 9 17.00 6.30 -4 -6 9 14.90 6.10 3 6 -9 450.85 34.60 -3 -6 9 534.95 33.40 -3 -6 9 488.05 24.60 2 6 -9 2073.59 89.89 -2 -6 9 2009.60 85.49 1 6 -9 576.94 36.80 -1 -6 9 464.65 31.90 0 6 -9 68.59 14.10 0 -6 9 64.09 12.00 -1 6 -9 227.38 22.20 1 -6 9 220.98 20.30 -2 6 -9 9.30 5.70 2 -6 9 3.00 3.20 3 -6 9 15.00 6.30 -4 6 -9 -2.30 5.90 -4 6 -9 6.40 4.60 4 -6 9 3.40 4.80 -5 6 -9 6.50 9.40 -5 6 -9 5.70 6.50 5 -6 9 15.50 6.50 -6 6 -9 6.80 6.80 -6 6 -9 9.60 6.80 6 -6 9 9.30 4.80 -7 6 -9 83.69 18.50 -7 6 -9 75.29 15.20 7 -6 9 99.29 16.40 -8 6 -9 36.40 12.00 -8 6 -9 20.80 11.60 8 -6 9 35.50 8.90 -9 6 -9 15.10 9.70 9 -6 9 6.80 8.00 -10 6 -9 4.40 11.00 10 -6 9 25.60 16.70 11 5 -9 5.60 11.00 10 5 -9 11.00 9.70 -10 -5 9 7.10 9.60 9 5 -9 5.90 8.60 -9 -5 9 11.60 7.90 -9 -5 9 -3.80 5.20 8 5 -9 8.20 7.00 -8 -5 9 -7.30 3.90 -7 -5 9 32.10 8.40 -7 -5 9 37.70 9.00 6 5 -9 142.19 19.30 -6 -5 9 118.99 14.90 -6 -5 9 160.08 16.60 5 5 -9 195.48 21.90 4 5 -9 638.94 40.70 -4 -5 9 663.03 34.00 -4 -5 9 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22.10 14.90 9 -3 9 -0.80 11.60 12 2 -9 9.60 11.30 -12 -2 9 -6.30 8.00 11 2 -9 53.19 15.40 -11 -2 9 19.10 11.60 10 2 -9 8.20 5.30 -10 -2 9 -7.40 5.60 -10 -2 9 7.80 5.60 9 2 -9 98.99 18.70 -9 -2 9 97.89 18.60 8 2 -9 356.16 24.50 8 2 -9 370.06 30.00 -8 -2 9 319.77 28.50 7 2 -9 235.08 19.20 7 2 -9 247.38 23.00 -7 -2 9 224.48 21.50 6 2 -9 31.40 9.90 6 2 -9 43.30 8.70 -6 -2 9 31.70 8.20 5 2 -9 372.16 26.20 5 2 -9 395.06 26.20 -5 -2 9 394.26 26.90 4 2 -9 156.98 15.90 4 2 -9 135.49 14.80 -4 -2 9 147.39 15.00 3 2 -9 19.80 6.60 3 2 -9 25.70 6.50 -3 -2 9 28.50 7.40 2 2 -9 33.90 9.10 2 2 -9 29.60 7.40 -2 -2 9 49.90 11.50 1 2 -9 2.00 2.80 1 2 -9 3.30 3.40 -1 -2 9 9.50 4.60 0 2 -9 6.20 4.80 0 2 -9 -0.50 2.80 0 -2 9 0.20 3.60 -1 2 -9 25.50 7.20 1 -2 9 26.50 8.20 -2 2 -9 38.10 9.40 -2 2 -9 32.40 9.70 -2 2 -9 51.69 11.30 -3 2 -9 60.19 11.30 -3 2 -9 43.50 10.60 -3 2 -9 56.39 11.80 -4 2 -9 68.99 12.40 -4 2 -9 64.09 13.70 -4 2 -9 78.79 14.70 -5 2 -9 4.60 4.60 -5 2 -9 12.90 6.40 5 -2 9 2.40 5.10 -6 2 -9 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-15 50.49 13.10 -5 -5 15 46.40 13.40 4 5 -15 15.10 7.90 4 5 -15 5.50 7.60 -4 -5 15 12.50 7.30 3 5 -15 87.89 18.80 3 5 -15 122.79 17.20 -3 -5 15 127.19 15.70 2 5 -15 0.00 7.30 2 5 -15 -0.70 7.80 -2 -5 15 11.10 6.10 1 5 -15 18.60 9.80 1 5 -15 21.90 10.20 -1 -5 15 7.50 7.00 0 5 -15 48.80 14.00 0 5 -15 60.29 15.70 0 -5 15 55.79 12.40 -1 5 -15 69.79 15.80 -1 5 -15 82.09 22.80 1 -5 15 36.30 11.20 -2 5 -15 25.70 11.70 -2 5 -15 32.80 13.40 2 -5 15 56.99 13.40 -3 5 -15 30.90 12.80 -3 5 -15 41.20 14.80 3 -5 15 31.70 10.60 4 -5 15 246.68 29.40 4 -5 15 196.28 28.00 9 4 -15 4.30 11.20 -9 -4 15 -1.00 7.20 8 4 -15 20.90 14.70 8 4 -15 27.50 12.90 -8 -4 15 9.10 8.70 7 4 -15 9.80 9.60 7 4 -15 8.10 8.30 -7 -4 15 9.20 7.90 6 4 -15 18.00 9.10 6 4 -15 30.90 10.10 -6 -4 15 42.40 11.40 5 4 -15 26.80 11.90 5 4 -15 14.30 9.20 -5 -4 15 22.00 8.40 4 4 -15 62.09 15.50 4 4 -15 31.20 11.70 -4 -4 15 33.70 9.60 3 4 -15 28.80 9.50 3 4 -15 6.80 8.20 -3 -4 15 10.80 7.50 2 4 -15 19.40 9.10 2 4 -15 12.60 9.40 -2 -4 15 30.90 9.00 1 4 -15 33.50 11.70 1 4 -15 38.20 11.30 -1 -4 15 33.60 10.60 0 4 -15 44.90 13.80 0 -4 15 52.69 13.30 -1 4 -15 5.10 7.80 1 -4 15 4.40 6.20 -2 4 -15 60.49 15.00 -2 4 -15 87.69 17.20 -3 4 -15 44.00 14.50 -3 4 -15 49.70 14.20 3 -4 15 39.40 14.00 9 3 -15 52.69 16.40 9 3 -15 73.29 16.70 8 3 -15 -10.30 8.30 -8 -3 15 -7.30 7.30 7 3 -15 -3.10 6.20 7 3 -15 0.30 7.80 -7 -3 15 9.50 7.90 6 3 -15 -2.50 7.60 5 3 -15 1.50 8.50 5 3 -15 24.40 9.90 -5 -3 15 21.30 8.50 4 3 -15 57.89 14.10 -4 -3 15 76.59 15.80 3 3 -15 137.59 23.20 -3 -3 15 161.98 20.00 2 3 -15 36.60 13.10 -2 -3 15 20.80 8.80 1 3 -15 302.57 33.20 -1 -3 15 331.87 29.80 0 3 -15 117.89 34.50 0 -3 15 128.69 23.10 -1 3 -15 36.00 12.00 -1 3 -15 2.30 8.00 1 -3 15 25.80 11.20 -2 3 -15 1.10 7.40 2 -3 15 1.40 10.00 3 -3 15 10.70 10.50 9 2 -15 158.98 21.60 -9 -2 15 151.78 25.50 8 2 -15 66.99 16.40 -8 -2 15 65.59 17.50 -7 -2 15 27.70 10.50 6 2 -15 1.00 6.00 -6 -2 15 -1.50 6.60 5 2 -15 216.28 27.40 -5 -2 15 190.78 23.60 4 2 -15 -7.00 4.20 -4 -2 15 -5.70 6.70 3 2 -15 25.30 12.20 -3 -2 15 -2.10 5.70 -2 -2 15 7.50 7.30 1 2 -15 27.00 11.80 -1 -2 15 12.20 10.10 0 2 -15 16.60 9.90 0 -2 15 -0.40 8.30 -1 2 -15 21.60 11.30 1 -2 15 30.30 13.20 -2 2 -15 23.10 10.90 2 -2 15 7.30 9.40 9 1 -15 78.99 16.30 -9 -1 15 80.29 19.20 8 1 -15 40.40 13.00 -8 -1 15 45.00 21.40 7 1 -15 6.30 7.30 -7 -1 15 18.90 11.00 6 1 -15 7.90 7.00 -6 -1 15 -13.30 8.20 5 1 -15 30.10 12.10 -5 -1 15 34.00 11.10 4 1 -15 23.60 10.40 -4 -1 15 14.30 8.50 3 1 -15 -10.30 5.70 -3 -1 15 -0.80 5.70 2 1 -15 125.19 24.10 -2 -1 15 98.09 20.30 1 1 -15 7.20 7.10 -1 -1 15 19.70 11.70 0 1 -15 5.70 8.00 -1 1 -15 -16.20 6.20 1 -1 15 12.90 11.30 9 0 -15 -2.60 7.30 -9 0 15 5.60 9.90 8 0 -15 -1.70 10.30 -8 0 15 24.80 12.10 7 0 -15 43.90 15.00 -7 0 15 82.89 19.80 6 0 -15 25.30 11.70 -6 0 15 29.70 13.70 5 0 -15 53.69 14.80 -5 0 15 40.90 14.50 4 0 -15 17.20 10.30 -4 0 15 22.80 11.50 3 0 -15 109.59 21.70 -3 0 15 64.09 17.00 2 0 -15 0.60 7.90 1 0 -15 13.40 9.30 -1 0 15 -3.80 7.40 0 0 -15 2.40 7.50 0 0 15 13.70 10.20 8 -1 -15 -6.50 7.10 -8 1 15 -5.40 8.00 7 -1 -15 10.70 9.50 -7 1 15 4.30 11.20 6 -1 -15 71.59 17.80 -6 1 15 43.00 15.30 5 -1 -15 58.59 16.80 -5 1 15 56.99 15.80 4 -1 -15 41.10 12.40 -4 1 15 24.20 11.50 3 -1 -15 111.49 21.90 -3 1 15 98.79 22.60 2 -1 -15 106.19 21.10 -2 1 15 71.09 18.50 6 -2 -15 36.20 13.50 -6 2 15 56.09 18.00 5 -2 -15 -9.70 7.10 -5 2 15 8.40 11.60 -4 2 15 12.30 11.60 3 10 -16 24.10 11.40 -3 -10 16 15.40 11.00 2 10 -16 2.00 12.00 -2 -10 16 1.30 8.40 1 10 -16 6.80 11.80 -1 -10 16 -6.10 9.70 0 10 -16 -7.90 12.30 0 -10 16 3.80 8.30 -1 10 -16 32.60 16.10 1 -10 16 50.49 14.40 2 -10 16 91.29 22.00 -5 -9 16 9.90 10.20 4 9 -16 2.70 12.80 -4 -9 16 10.40 12.60 3 9 -16 -2.70 10.30 -3 -9 16 47.10 14.60 2 9 -16 37.90 19.00 -2 -9 16 42.20 16.90 -1 -9 16 25.80 12.50 0 9 -16 23.40 16.70 0 -9 16 7.30 8.90 -1 9 -16 25.70 13.20 1 -9 16 1.80 9.20 -2 9 -16 31.10 14.20 2 -9 16 10.50 11.60 -6 -8 16 0.80 8.50 5 8 -16 -19.70 7.90 -5 -8 16 18.60 9.70 4 8 -16 11.20 11.00 -4 -8 16 -10.10 6.40 3 8 -16 -19.10 9.20 -3 -8 16 -4.90 6.30 2 8 -16 83.29 18.60 -2 -8 16 45.80 16.90 1 8 -16 17.00 10.70 -1 -8 16 47.50 14.60 0 8 -16 32.80 14.60 0 -8 16 21.10 11.40 -1 8 -16 18.10 14.70 1 -8 16 10.70 10.60 -2 8 -16 11.20 17.00 2 -8 16 24.70 11.90 -6 -7 16 31.30 13.50 5 7 -16 3.80 9.80 -5 -7 16 7.70 8.70 4 7 -16 31.10 11.40 -4 -7 16 10.40 8.10 3 7 -16 21.90 12.30 -3 -7 16 43.80 13.10 2 7 -16 -7.40 8.90 -2 -7 16 10.30 9.00 1 7 -16 22.10 13.90 -1 -7 16 0.80 9.00 0 7 -16 -0.70 10.00 0 -7 16 -0.90 8.20 -1 7 -16 98.39 22.60 1 -7 16 84.79 20.60 -2 7 -16 23.10 15.30 2 -7 16 15.40 11.80 7 6 -16 -9.00 9.90 -7 -6 16 -4.60 7.20 6 6 -16 -5.10 9.90 -6 -6 16 15.20 8.70 5 6 -16 7.60 10.20 -5 -6 16 36.90 12.70 4 6 -16 11.80 10.60 -4 -6 16 5.40 6.70 3 6 -16 29.40 11.80 3 6 -16 15.50 10.00 2 6 -16 6.90 8.60 2 6 -16 -14.40 8.80 1 6 -16 24.30 11.70 1 6 -16 27.60 11.90 0 6 -16 130.69 23.10 0 6 -16 97.09 21.30 -1 6 -16 63.89 16.30 1 -6 16 46.00 15.50 -2 6 -16 317.67 34.20 2 -6 16 279.47 33.40 7 5 -16 1.60 11.50 -7 -5 16 7.40 10.20 -7 -5 16 -0.20 8.00 6 5 -16 9.30 7.50 6 5 -16 29.90 11.10 -6 -5 16 -8.50 9.20 5 5 -16 16.60 10.80 5 5 -16 14.00 8.50 -5 -5 16 27.50 8.20 4 5 -16 55.09 14.50 4 5 -16 21.80 11.10 -4 -5 16 63.29 13.90 3 5 -16 18.10 8.10 3 5 -16 -2.70 9.10 -3 -5 16 9.90 8.20 2 5 -16 -3.30 5.80 2 5 -16 19.60 9.70 -2 -5 16 -4.60 5.70 1 5 -16 20.20 12.00 1 5 -16 39.60 13.50 -1 -5 16 11.50 8.00 0 5 -16 224.38 27.60 0 5 -16 213.68 24.70 0 -5 16 225.88 22.40 -1 5 -16 35.10 11.60 -1 5 -16 -11.30 8.40 1 -5 16 7.50 9.90 -2 5 -16 22.90 14.70 -2 5 -16 20.50 11.00 2 -5 16 43.50 13.10 -8 -4 16 14.90 10.30 7 4 -16 -0.70 8.50 -7 -4 16 -10.30 8.00 6 4 -16 -11.40 9.30 6 4 -16 0.10 7.50 -6 -4 16 -3.00 8.00 5 4 -16 104.39 20.90 -5 -4 16 77.99 17.10 4 4 -16 138.29 25.10 -4 -4 16 128.29 18.10 3 4 -16 112.09 21.30 -3 -4 16 151.18 18.20 2 4 -16 -1.80 7.50 2 4 -16 23.50 17.50 -2 -4 16 13.50 6.60 1 4 -16 12.60 11.30 1 4 -16 16.10 9.60 -1 -4 16 5.80 8.10 0 4 -16 16.50 10.40 0 4 -16 17.70 10.80 0 -4 16 48.10 12.80 -1 4 -16 -3.30 7.10 1 -4 16 12.90 12.20 8 3 -16 -2.50 7.80 7 3 -16 46.70 14.30 -7 -3 16 17.30 11.50 6 3 -16 -2.00 8.10 -6 -3 16 2.00 8.70 5 3 -16 28.70 11.00 -5 -3 16 -0.70 8.40 4 3 -16 244.18 27.70 -4 -3 16 257.47 27.20 3 3 -16 -2.60 6.70 -3 -3 16 19.90 10.60 2 3 -16 18.70 10.10 -2 -3 16 20.50 12.10 1 3 -16 14.50 9.50 -1 -3 16 4.30 8.80 0 3 -16 5.30 9.70 0 -3 16 23.20 11.70 7 2 -16 3.40 8.50 6 2 -16 57.69 15.60 -6 -2 16 78.29 18.80 5 2 -16 -0.70 6.90 -5 -2 16 -11.10 6.90 4 2 -16 62.99 16.90 -4 -2 16 79.09 17.30 3 2 -16 -14.60 6.70 -3 -2 16 13.40 9.90 2 2 -16 -12.40 5.40 -2 -2 16 -0.90 6.80 1 2 -16 -8.40 7.10 -1 -2 16 -23.40 10.20 0 -2 16 41.90 14.10 7 1 -16 15.20 9.80 -7 -1 16 23.80 12.20 6 1 -16 16.70 11.00 -6 -1 16 28.90 12.00 5 1 -16 24.10 9.50 -5 -1 16 13.20 19.30 4 1 -16 26.40 9.60 3 1 -16 4.70 8.60 -3 -1 16 -18.00 7.00 2 1 -16 0.60 7.60 -2 -1 16 -4.30 8.60 -6 0 16 15.50 13.20 5 0 -16 16.70 11.00 -5 0 16 0.20 9.60 4 0 -16 1.70 5.80 -4 0 16 -0.70 10.50 3 8 -17 24.60 12.70 -3 -8 17 6.30 10.80 2 8 -17 30.20 15.70 -2 -8 17 28.30 11.50 1 8 -17 112.89 29.30 -1 -8 17 105.69 24.50 4 7 -17 5.70 12.20 -4 -7 17 5.90 8.60 3 7 -17 1.90 12.10 -3 -7 17 -2.60 8.00 2 7 -17 40.20 16.20 -2 -7 17 98.59 23.00 1 7 -17 180.38 30.60 -1 -7 17 157.08 29.20 0 -7 17 173.08 29.10 5 6 -17 23.70 13.20 -5 -6 17 9.20 9.20 4 6 -17 11.60 10.60 -4 -6 17 -11.30 6.70 3 6 -17 33.50 14.50 3 6 -17 57.39 15.70 2 6 -17 116.49 23.30 2 6 -17 131.79 23.50 1 6 -17 50.39 15.20 1 6 -17 69.59 19.20 0 -6 17 -8.10 5.50 5 5 -17 52.59 15.20 5 5 -17 -2.30 11.00 4 5 -17 -3.90 11.40 4 5 -17 59.49 15.90 3 5 -17 -0.30 11.50 3 5 -17 13.10 8.30 2 5 -17 -25.00 11.60 2 5 -17 9.20 9.60 1 5 -17 -2.30 15.90 1 5 -17 36.10 13.60 5 4 -17 181.88 24.70 -5 -4 17 181.18 23.80 4 4 -17 53.59 15.70 -4 -4 17 58.39 14.70 3 4 -17 38.80 13.80 -3 -4 17 46.10 13.40 2 4 -17 132.79 23.70 -2 -4 17 136.99 22.90 4 3 -17 64.99 15.90 -4 -3 17 92.89 20.30 -3 -3 17 79.89 17.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 68069 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 0.9785(2) 0.95972(19) 1.33216(15) 0.0201(3) Uani 1 1 d . . . . . N1 N 0.9238(2) 0.5936(2) 0.83408(19) 0.0188(4) Uani 1 1 d . . . . . N2 N 0.8740(2) 0.4622(2) 0.72355(19) 0.0181(4) Uani 1 1 d . . . . . N3 N 0.7208(2) 0.4283(2) 0.66129(17) 0.0151(3) Uani 1 1 d . . . . . N4 N 0.6460(2) 0.1756(2) 0.47076(18) 0.0154(3) Uani 1 1 d . . . . . N5 N 0.5018(2) 0.0822(2) 0.37516(17) 0.0148(3) Uani 1 1 d . . . . . N6 N 0.3877(2) 0.1353(2) 0.38444(18) 0.0149(3) Uani 1 1 d . . . . . C1 C 0.8049(2) 0.6442(2) 0.8433(2) 0.0153(4) Uani 1 1 d . . . . . C2 C 0.6701(2) 0.5383(2) 0.7316(2) 0.0141(4) Uani 1 1 d . . . . . C3 C 0.5053(2) 0.5156(2) 0.6832(2) 0.0148(4) Uani 1 1 d . . . . . C4 C 0.4439(3) 0.6165(3) 0.7568(2) 0.0182(4) Uani 1 1 d . . . . . H4 H 0.511850 0.704859 0.840171 0.022 Uiso 1 1 calc R U . . . C5 C 0.2863(3) 0.5891(3) 0.7099(2) 0.0211(4) Uani 1 1 d . . . . . H5 H 0.247008 0.658744 0.761252 0.025 Uiso 1 1 calc R U . . . C6 C 0.1837(3) 0.4602(3) 0.5876(2) 0.0198(4) Uani 1 1 d . . . . . H6 H 0.075534 0.443065 0.555518 0.024 Uiso 1 1 calc R U . . . C7 C 0.2400(3) 0.3582(3) 0.5138(2) 0.0173(4) Uani 1 1 d . . . . . H7 H 0.170573 0.270333 0.430575 0.021 Uiso 1 1 calc R U . . . C8 C 0.3991(2) 0.3836(2) 0.5610(2) 0.0137(4) Uani 1 1 d . . . . . C9 C 0.4615(2) 0.2742(2) 0.4939(2) 0.0140(4) Uani 1 1 d . . . . . C10 C 0.6185(2) 0.2955(2) 0.5445(2) 0.0141(4) Uani 1 1 d . . . . . C11 C 0.4708(2) -0.0687(2) 0.2750(2) 0.0142(4) Uani 1 1 d . . . . . C12 C 0.5878(3) -0.1258(2) 0.2825(2) 0.0168(4) Uani 1 1 d . . . . . H12 H 0.688019 -0.065153 0.352523 0.020 Uiso 1 1 calc R U . . . C13 C 0.5544(3) -0.2748(2) 0.1845(2) 0.0183(4) Uani 1 1 d . . . . . H13 H 0.633042 -0.316248 0.187577 0.022 Uiso 1 1 calc R U . . . C14 C 0.4078(3) -0.3635(3) 0.0826(2) 0.0191(4) Uani 1 1 d . . . . . H14 H 0.386113 -0.465064 0.016454 0.023 Uiso 1 1 calc R U . . . C15 C 0.2931(3) -0.3029(3) 0.0777(2) 0.0188(4) Uani 1 1 d . . . . . H15 H 0.192834 -0.363395 0.007812 0.023 Uiso 1 1 calc R U . . . C16 C 0.3236(3) -0.1550(2) 0.1740(2) 0.0159(4) Uani 1 1 d . . . . . H16 H 0.245106 -0.113535 0.170740 0.019 Uiso 1 1 calc R U . . . C17 C 0.8320(3) 0.7871(2) 0.9621(2) 0.0156(4) Uani 1 1 d . . . . . C18 C 0.8992(2) 0.8038(2) 1.0897(2) 0.0153(4) Uani 1 1 d . . . . . H18 H 0.929693 0.725660 1.098943 0.018 Uiso 1 1 calc R U . . . C19 C 0.9214(2) 0.9352(2) 1.2031(2) 0.0160(4) Uani 1 1 d . . . . . C20 C 0.8791(3) 1.0511(3) 1.1900(2) 0.0195(4) Uani 1 1 d . . . . . H20 H 0.893162 1.140476 1.267684 0.023 Uiso 1 1 calc R U . . . C21 C 0.8163(3) 1.0352(3) 1.0627(2) 0.0193(4) Uani 1 1 d . . . . . H21 H 0.789381 1.115037 1.053530 0.023 Uiso 1 1 calc R U . . . C22 C 0.7923(3) 0.9036(2) 0.9484(2) 0.0183(4) Uani 1 1 d . . . . . H22 H 0.749092 0.893325 0.861408 0.022 Uiso 1 1 calc R U . . . C23 C 1.0257(3) 0.8459(3) 1.3523(2) 0.0221(4) Uani 1 1 d . . . . . H23A H 1.056483 0.873433 1.448167 0.033 Uiso 1 1 calc R U . . . H23B H 1.115597 0.842271 1.322370 0.033 Uiso 1 1 calc R U . . . H23C H 0.937302 0.743970 1.300277 0.033 Uiso 1 1 calc R U . . . 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 0.0248(8) 0.0213(8) 0.0124(7) 0.0058(6) 0.0041(6) 0.0110(6) N1 0.0173(9) 0.0161(8) 0.0166(8) 0.0026(7) 0.0022(7) 0.0074(7) N2 0.0134(8) 0.0166(8) 0.0168(8) 0.0024(7) 0.0008(6) 0.0063(7) N3 0.0136(8) 0.0149(8) 0.0127(7) 0.0030(6) 0.0024(6) 0.0065(6) N4 0.0147(8) 0.0141(8) 0.0132(7) 0.0030(6) 0.0032(6) 0.0056(6) N5 0.0144(8) 0.0122(7) 0.0130(7) 0.0023(6) 0.0022(6) 0.0057(6) N6 0.0150(8) 0.0147(8) 0.0143(8) 0.0048(6) 0.0048(6) 0.0077(6) C1 0.0163(9) 0.0160(9) 0.0124(8) 0.0052(7) 0.0039(7) 0.0074(7) C2 0.0163(9) 0.0126(8) 0.0123(8) 0.0046(7) 0.0041(7) 0.0066(7) C3 0.0166(9) 0.0137(8) 0.0123(8) 0.0042(7) 0.0048(7) 0.0064(7) C4 0.0184(10) 0.0184(9) 0.0179(9) 0.0065(8) 0.0072(8) 0.0094(8) C5 0.0218(11) 0.0228(10) 0.0216(10) 0.0076(9) 0.0114(8) 0.0141(9) C6 0.0169(10) 0.0211(10) 0.0219(10) 0.0090(9) 0.0064(8) 0.0101(8) C7 0.0158(10) 0.0167(9) 0.0167(9) 0.0049(8) 0.0041(7) 0.0077(8) C8 0.0150(9) 0.0138(8) 0.0130(8) 0.0057(7) 0.0050(7) 0.0076(7) C9 0.0144(9) 0.0150(8) 0.0130(8) 0.0062(7) 0.0049(7) 0.0070(7) C10 0.0138(9) 0.0133(8) 0.0115(8) 0.0034(7) 0.0028(7) 0.0049(7) C11 0.0176(10) 0.0108(8) 0.0109(8) 0.0021(7) 0.0046(7) 0.0056(7) C12 0.0150(9) 0.0159(9) 0.0160(9) 0.0044(7) 0.0046(7) 0.0059(7) C13 0.0197(10) 0.0149(9) 0.0201(10) 0.0060(8) 0.0083(8) 0.0085(8) C14 0.0218(11) 0.0137(9) 0.0165(9) 0.0023(8) 0.0067(8) 0.0061(8) C15 0.0191(10) 0.0153(9) 0.0146(9) 0.0031(8) 0.0019(7) 0.0049(8) C16 0.0161(9) 0.0154(9) 0.0139(9) 0.0047(7) 0.0045(7) 0.0067(7) C17 0.0164(9) 0.0134(8) 0.0126(8) 0.0038(7) 0.0026(7) 0.0049(7) C18 0.0162(9) 0.0125(8) 0.0156(9) 0.0051(7) 0.0047(7) 0.0063(7) C19 0.0147(9) 0.0175(9) 0.0114(8) 0.0041(7) 0.0033(7) 0.0051(7) C20 0.0209(11) 0.0165(9) 0.0162(9) 0.0037(8) 0.0042(8) 0.0079(8) C21 0.0238(11) 0.0143(9) 0.0173(9) 0.0053(8) 0.0041(8) 0.0090(8) C22 0.0215(11) 0.0149(9) 0.0148(9) 0.0048(8) 0.0033(7) 0.0073(8) C23 0.0254(12) 0.0250(11) 0.0173(10) 0.0109(9) 0.0051(8) 0.0124(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C19 O1 C23 117.80(17) . . ? N2 N1 C1 110.38(18) . . ? N1 N2 N3 105.84(17) . . ? N2 N3 C2 112.56(17) . . ? N2 N3 C10 125.87(18) . . ? C2 N3 C10 121.47(18) . . ? C10 N4 N5 101.08(17) . . ? N6 N5 N4 116.47(17) . . ? N6 N5 C11 121.81(17) . . ? N4 N5 C11 121.61(17) . . ? N5 N6 C9 103.32(17) . . ? N1 C1 C2 108.73(18) . . ? N1 C1 C17 120.00(19) . . ? C2 C1 C17 131.23(19) . . ? N3 C2 C1 102.50(17) . . ? N3 C2 C3 119.91(18) . . ? C1 C2 C3 137.45(19) . . ? C4 C3 C8 117.64(19) . . ? C4 C3 C2 122.38(19) . . ? C8 C3 C2 119.90(18) . . ? C5 C4 C3 120.9(2) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.8(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 119.7(2) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 120.1(2) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C3 120.87(19) . . ? C7 C8 C9 122.42(19) . . ? C3 C8 C9 116.60(18) . . ? N6 C9 C10 107.38(18) . . ? N6 C9 C8 129.91(19) . . ? C10 C9 C8 122.54(19) . . ? N4 C10 N3 128.72(19) . . ? N4 C10 C9 111.74(18) . . ? N3 C10 C9 119.49(18) . . ? C12 C11 C16 122.03(19) . . ? C12 C11 N5 119.02(18) . . ? C16 C11 N5 118.94(18) . . ? C11 C12 C13 118.2(2) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? C14 C13 C12 120.8(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.6(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 C14 120.6(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C11 118.8(2) . . ? C15 C16 H16 120.6 . . ? C11 C16 H16 120.6 . . ? C22 C17 C18 120.32(19) . . ? C22 C17 C1 121.15(19) . . ? C18 C17 C1 118.52(19) . . ? C19 C18 C17 119.57(19) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? O1 C19 C18 124.4(2) . . ? O1 C19 C20 115.15(19) . . ? C18 C19 C20 120.37(19) . . ? C21 C20 C19 119.5(2) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.7(2) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C17 119.5(2) . . ? C21 C22 H22 120.2 . . ? C17 C22 H22 120.2 . . ? O1 C23 H23A 109.5 . . ? O1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 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 C19 1.364(3) . ? O1 C23 1.427(3) . ? N1 N2 1.313(2) . ? N1 C1 1.364(3) . ? N2 N3 1.351(2) . ? N3 C2 1.376(3) . ? N3 C10 1.381(3) . ? N4 C10 1.321(3) . ? N4 N5 1.350(2) . ? N5 N6 1.336(2) . ? N5 C11 1.422(2) . ? N6 C9 1.338(3) . ? C1 C2 1.389(3) . ? C1 C17 1.473(3) . ? C2 C3 1.456(3) . ? C3 C4 1.404(3) . ? C3 C8 1.416(3) . ? C4 C5 1.377(3) . ? C4 H4 0.9500 . ? C5 C6 1.397(3) . ? C5 H5 0.9500 . ? C6 C7 1.376(3) . ? C6 H6 0.9500 . ? C7 C8 1.397(3) . ? C7 H7 0.9500 . ? C8 C9 1.440(3) . ? C9 C10 1.394(3) . ? C11 C12 1.385(3) . ? C11 C16 1.387(3) . ? C12 C13 1.394(3) . ? C12 H12 0.9500 . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 C15 1.387(3) . ? C14 H14 0.9500 . ? C15 C16 1.386(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.389(3) . ? C17 C18 1.395(3) . ? C18 C19 1.388(3) . ? C18 H18 0.9500 . ? C19 C20 1.394(3) . ? C20 C21 1.386(3) . ? C20 H20 0.9500 . ? C21 C22 1.389(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 N2 N3 0.0(2) . . . . ? N1 N2 N3 C2 0.0(2) . . . . ? N1 N2 N3 C10 -176.3(2) . . . . ? C10 N4 N5 N6 0.0(2) . . . . ? C10 N4 N5 C11 -176.19(19) . . . . ? N4 N5 N6 C9 0.1(2) . . . . ? C11 N5 N6 C9 176.29(18) . . . . ? N2 N1 C1 C2 0.1(3) . . . . ? N2 N1 C1 C17 177.73(19) . . . . ? N2 N3 C2 C1 0.0(2) . . . . ? C10 N3 C2 C1 176.48(19) . . . . ? N2 N3 C2 C3 -176.31(18) . . . . ? C10 N3 C2 C3 0.1(3) . . . . ? N1 C1 C2 N3 -0.1(2) . . . . ? C17 C1 C2 N3 -177.4(2) . . . . ? N1 C1 C2 C3 175.3(2) . . . . ? C17 C1 C2 C3 -2.1(4) . . . . ? N3 C2 C3 C4 174.1(2) . . . . ? C1 C2 C3 C4 -0.6(4) . . . . ? N3 C2 C3 C8 -2.6(3) . . . . ? C1 C2 C3 C8 -177.3(2) . . . . ? C8 C3 C4 C5 -1.4(3) . . . . ? C2 C3 C4 C5 -178.1(2) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C4 C5 C6 C7 0.8(4) . . . . ? C5 C6 C7 C8 0.0(3) . . . . ? C6 C7 C8 C3 -1.5(3) . . . . ? C6 C7 C8 C9 174.7(2) . . . . ? C4 C3 C8 C7 2.1(3) . . . . ? C2 C3 C8 C7 179.0(2) . . . . ? C4 C3 C8 C9 -174.22(19) . . . . ? C2 C3 C8 C9 2.6(3) . . . . ? N5 N6 C9 C10 -0.2(2) . . . . ? N5 N6 C9 C8 -175.5(2) . . . . ? C7 C8 C9 N6 -2.0(4) . . . . ? C3 C8 C9 N6 174.2(2) . . . . ? C7 C8 C9 C10 -176.7(2) . . . . ? C3 C8 C9 C10 -0.4(3) . . . . ? N5 N4 C10 N3 177.5(2) . . . . ? N5 N4 C10 C9 -0.1(2) . . . . ? N2 N3 C10 N4 0.6(4) . . . . ? C2 N3 C10 N4 -175.3(2) . . . . ? N2 N3 C10 C9 178.1(2) . . . . ? C2 N3 C10 C9 2.1(3) . . . . ? N6 C9 C10 N4 0.2(2) . . . . ? C8 C9 C10 N4 175.88(19) . . . . ? N6 C9 C10 N3 -177.70(18) . . . . ? C8 C9 C10 N3 -2.0(3) . . . . ? N6 N5 C11 C12 -170.58(19) . . . . ? N4 N5 C11 C12 5.4(3) . . . . ? N6 N5 C11 C16 8.5(3) . . . . ? N4 N5 C11 C16 -175.56(19) . . . . ? C16 C11 C12 C13 0.1(3) . . . . ? N5 C11 C12 C13 179.11(19) . . . . ? C11 C12 C13 C14 -0.2(3) . . . . ? C12 C13 C14 C15 0.2(3) . . . . ? C13 C14 C15 C16 -0.2(3) . . . . ? C14 C15 C16 C11 0.1(3) . . . . ? C12 C11 C16 C15 0.0(3) . . . . ? N5 C11 C16 C15 -179.05(19) . . . . ? N1 C1 C17 C22 130.1(2) . . . . ? C2 C1 C17 C22 -52.9(3) . . . . ? N1 C1 C17 C18 -49.7(3) . . . . ? C2 C1 C17 C18 127.4(3) . . . . ? C22 C17 C18 C19 2.2(3) . . . . ? C1 C17 C18 C19 -178.0(2) . . . . ? C23 O1 C19 C18 3.1(3) . . . . ? C23 O1 C19 C20 -179.3(2) . . . . ? C17 C18 C19 O1 176.5(2) . . . . ? C17 C18 C19 C20 -1.0(3) . . . . ? O1 C19 C20 C21 -178.5(2) . . . . ? C18 C19 C20 C21 -0.7(3) . . . . ? C19 C20 C21 C22 1.3(4) . . . . ? C20 C21 C22 C17 -0.1(4) . . . . ? C18 C17 C22 C21 -1.7(3) . . . . ? C1 C17 C22 C21 178.6(2) . . . . ?