#------------------------------------------------------------------------------ #$Date: 2019-11-17 14:45:58 +0200 (Sun, 17 Nov 2019) $ #$Revision: 230598 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/62/7156263.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_7156263 loop_ _publ_author_name 'Maiden, T. M. M.' 'Mbelesi, N.' 'Procopiou, P. A.' 'Swanson, S.' 'Harrity, J. P. A.' _publ_section_title ; A convergent strategy towards febrifugine and related compounds. ; _journal_issue 22 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 4159 _journal_page_last 4169 _journal_paper_doi 10.1039/c8ob00935j _journal_volume 16 _journal_year 2018 _chemical_formula_moiety 'C16 H19 N3 O3' _chemical_formula_sum 'C16 H19 N3 O3' _chemical_formula_weight 301.34 _chemical_name_common Febrifugine _chemical_name_systematic Febrifugine _chemical_properties_physical Heat-sensitive _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2016-01-28 deposited with the CCDC. 2018-05-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.2591(6) _cell_length_b 9.6617(5) _cell_length_c 30.5377(16) _cell_measurement_reflns_used 2758 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 66.49 _cell_measurement_theta_min 5.19 _cell_volume 3026.9(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.1251 _diffrn_reflns_av_unetI/netI 0.0895 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 12393 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 66.664 _diffrn_reflns_theta_max 66.664 _diffrn_reflns_theta_min 2.894 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.323 _exptl_crystal_description Plate _exptl_crystal_F_000 1280 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: ethyl acetate' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.276 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.517 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 200 _refine_ls_number_reflns 2658 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.517 _refine_ls_R_factor_all 0.1345 _refine_ls_R_factor_gt 0.0784 _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^)] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.0889 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1725 _reflns_number_total 2658 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8ob00935j2.cif _cod_data_source_block ohj328_a _cod_depositor_comments 'Adding full bibliography for 7156263.cif.' _cod_database_code 7156263 _shelx_shelxl_version_number 2014/7 _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 0.863 _shelx_estimated_absorpt_t_max 0.970 _shelx_res_file ; ohj328_a.res created by SHELXL-2014/7 TITL ohj328_a.res in Pbca CELL 1.54178 10.2591 9.6617 30.5377 90.000 90.000 90.000 ZERR 8.000 0.0006 0.0005 0.0016 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O UNIT 128 152 24 24 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 EQIV $1 -x+3/2, y+1/2, z HTAB O3 N3_$1 HTAB N3 O2 EQIV $2 -x+1, -y+1, -z+1 HTAB N3 O2_$2 EQIV $3 -x+1, -y+2, -z+1 HTAB C8 O3_$3 HTAB C9 O1_$1 EQIV $4 x-1/2, -y+3/2, -z+1 HTAB C14 O1_$4 SIZE 0.04 0.08 0.20 HTAB 2.0 TEMP -173.190 WGHT 0.000000 FVAR 0.30464 O1 4 0.789926 0.611824 0.394222 11.00000 0.02944 0.03109 = 0.03834 0.01030 -0.01008 -0.00041 O2 4 0.528283 0.648162 0.468455 11.00000 0.04391 0.02670 = 0.02261 0.00111 -0.00102 -0.01871 O3 4 0.648235 1.001791 0.576095 11.00000 0.02630 0.01517 = 0.03642 -0.00270 0.00468 -0.00113 AFIX 147 H3 2 0.720106 1.038800 0.570048 11.00000 -1.50000 AFIX 0 N1 3 0.612726 0.749212 0.386913 11.00000 0.02648 0.01830 = 0.01811 -0.00081 0.00044 -0.00211 N2 3 0.466785 0.737225 0.326935 11.00000 0.02908 0.02264 = 0.02357 0.00389 -0.00125 0.00423 N3 3 0.612242 0.622893 0.564582 11.00000 0.02668 0.01349 = 0.01763 -0.00381 0.00119 -0.00825 AFIX 3 H3N 2 0.579858 0.557443 0.542025 11.00000 -1.20000 AFIX 0 C1 1 0.695365 0.646690 0.372028 11.00000 0.02296 0.01742 = 0.02498 0.00919 -0.00134 -0.00294 C2 1 0.660998 0.591641 0.329263 11.00000 0.02137 0.01728 = 0.01905 0.00265 0.00478 -0.00027 C3 1 0.737912 0.490153 0.309330 11.00000 0.03366 0.02994 = 0.03448 0.00295 0.01289 0.00297 AFIX 43 H3A 2 0.813897 0.457110 0.323712 11.00000 -1.20000 AFIX 0 C4 1 0.704336 0.438259 0.269267 11.00000 0.05234 0.02756 = 0.03711 -0.00492 0.02739 -0.00051 AFIX 43 H4 2 0.756658 0.368895 0.255956 11.00000 -1.20000 AFIX 0 C5 1 0.593910 0.486771 0.248012 11.00000 0.06157 0.03395 = 0.02166 -0.00490 0.00953 -0.01728 AFIX 43 H5 2 0.571367 0.451155 0.220022 11.00000 -1.20000 AFIX 0 C6 1 0.517282 0.585665 0.267156 11.00000 0.03968 0.03034 = 0.02257 0.00576 -0.00394 -0.00590 AFIX 43 H6 2 0.441606 0.617858 0.252402 11.00000 -1.20000 AFIX 0 C7 1 0.549417 0.639855 0.308308 11.00000 0.02695 0.01671 = 0.02070 0.00458 0.00676 -0.00457 C8 1 0.503549 0.786283 0.364169 11.00000 0.02457 0.01814 = 0.02872 0.00359 0.00711 0.00197 AFIX 43 H8 2 0.449458 0.854912 0.377057 11.00000 -1.20000 AFIX 0 C9 1 0.644270 0.819547 0.427763 11.00000 0.03977 0.02266 = 0.01980 -0.00019 -0.00161 -0.00944 AFIX 23 H9A 2 0.599035 0.910047 0.428204 11.00000 -1.20000 H9B 2 0.739179 0.837955 0.428416 11.00000 -1.20000 AFIX 0 C10 1 0.607773 0.740745 0.468370 11.00000 0.02442 0.01673 = 0.02154 0.00155 0.00382 -0.00297 C11 1 0.674893 0.792668 0.508706 11.00000 0.02590 0.01909 = 0.02333 -0.00097 0.00048 -0.00288 AFIX 23 H11A 2 0.690081 0.893204 0.505073 11.00000 -1.20000 H11B 2 0.761407 0.747606 0.510438 11.00000 -1.20000 AFIX 0 C12 1 0.606119 0.770653 0.552094 11.00000 0.02118 0.01813 = 0.01955 0.00131 0.00030 -0.00421 AFIX 13 H12 2 0.512679 0.798376 0.548931 11.00000 -1.20000 AFIX 0 C13 1 0.668730 0.858751 0.587481 11.00000 0.02186 0.01567 = 0.02371 0.00032 -0.00204 -0.00047 AFIX 13 H13 2 0.764523 0.839685 0.588014 11.00000 -1.20000 AFIX 0 C14 1 0.612818 0.830231 0.632456 11.00000 0.03187 0.02309 = 0.02228 -0.00442 0.00276 -0.00089 AFIX 23 H14A 2 0.522482 0.866001 0.633835 11.00000 -1.20000 H14B 2 0.665030 0.879959 0.654722 11.00000 -1.20000 AFIX 0 C15 1 0.612451 0.676443 0.643026 11.00000 0.03240 0.02457 = 0.02179 0.00314 0.00325 -0.00903 AFIX 23 H15A 2 0.703212 0.643308 0.646399 11.00000 -1.20000 H15B 2 0.566151 0.660585 0.671024 11.00000 -1.20000 AFIX 0 C16 1 0.546028 0.596679 0.606904 11.00000 0.02592 0.02057 = 0.02961 0.00459 0.00467 -0.00269 AFIX 23 H16A 2 0.548539 0.496478 0.613630 11.00000 -1.20000 H16B 2 0.453582 0.625341 0.604852 11.00000 -1.20000 AFIX 0 HKLF 4 REM ohj328_a.res in Pbca REM R1 = 0.0784 for 1725 Fo > 4sig(Fo) and 0.1345 for all 2658 data REM 200 parameters refined using 0 restraints END WGHT 0.0281 5.2783 REM Instructions for potential hydrogen bonds HTAB O3 N3_$1 HTAB N3 O2 HTAB N3 O2_$2 HTAB C8 O3_$3 HTAB C9 O1_$1 HTAB C14 O1_$4 REM Highest difference peak 0.276, deepest hole -0.313, 1-sigma level 0.069 Q1 1 0.8392 0.5991 0.5219 11.00000 0.05 0.28 Q2 1 0.6013 1.0145 0.5395 11.00000 0.05 0.25 Q3 1 0.3945 0.7154 0.3898 11.00000 0.05 0.23 Q4 1 0.4840 0.9048 0.5498 11.00000 0.05 0.23 Q5 1 0.4491 0.5309 0.6080 11.00000 0.05 0.22 Q6 1 0.6041 0.6759 0.3814 11.00000 0.05 0.22 Q7 1 0.3923 0.8411 0.5225 11.00000 0.05 0.22 Q8 1 0.4005 0.7834 0.2255 11.00000 0.05 0.21 Q9 1 0.4561 0.6770 0.6196 11.00000 0.05 0.21 Q10 1 0.8352 0.6997 0.4113 11.00000 0.05 0.21 Q11 1 0.5351 0.7994 0.2979 11.00000 0.05 0.21 Q12 1 0.5755 0.9405 0.4988 11.00000 0.05 0.21 Q13 1 0.4726 0.8770 0.4926 11.00000 0.05 0.20 Q14 1 0.3502 0.8035 0.3998 11.00000 0.05 0.20 Q15 1 0.3752 0.5815 0.2322 11.00000 0.05 0.20 Q16 1 0.3969 0.6686 0.5576 11.00000 0.05 0.20 Q17 1 0.7076 0.9066 0.4272 11.00000 0.05 0.20 Q18 1 0.5657 0.3772 0.6413 11.00000 0.05 0.20 Q19 1 0.8750 0.8762 0.4874 11.00000 0.05 0.19 Q20 1 0.7423 0.9279 0.6896 11.00000 0.05 0.19 ; _shelx_res_checksum 50064 _shelx_hkl_file ; 0 1 0 -2.30 0.80 0 -1 0 -1.60 0.60 0 -1 0 -1.50 0.70 0 1 0 -1.90 0.50 0 2 0 1359.56 42.40 0 2 0 1363.76 42.10 0 -2 0 1375.86 42.10 0 3 0 -1.50 1.50 0 3 0 -0.80 2.00 0 -3 0 3.90 2.20 0 4 0 184.18 8.40 0 5 0 1.50 6.50 0 5 0 10.10 5.20 0 6 0 21.10 7.10 0 7 0 -5.60 5.50 0 7 0 -1.50 19.10 0 8 0 705.03 25.50 0 8 0 682.93 27.90 0 9 0 7.80 9.30 0 9 0 -1.00 6.00 0 -9 0 1.20 6.20 0 10 0 -13.40 11.00 0 -10 0 -0.20 6.60 0 11 0 1.80 12.70 1 1 0 -1.50 1.00 -1 -1 0 -2.50 1.40 1 -1 0 -1.60 0.80 -1 2 0 0.30 1.60 1 2 0 0.00 1.60 1 -2 0 -1.60 1.30 1 3 0 -0.60 1.50 -1 3 0 2.10 2.10 1 3 0 -0.40 2.20 1 -3 0 -1.70 2.20 1 4 0 -2.90 3.30 1 4 0 0.80 2.30 -1 4 0 -0.70 2.90 -1 5 0 6.80 4.80 1 5 0 5.80 5.70 1 5 0 0.70 4.60 -1 5 0 6.40 7.60 -1 6 0 6.20 5.00 1 6 0 -3.50 6.40 -1 7 0 -1.90 5.60 1 7 0 3.40 10.70 -1 7 0 -1.60 4.80 1 7 0 -1.70 5.30 -1 -8 0 7.80 5.50 1 8 0 -0.40 5.80 -1 8 0 4.00 4.90 -1 8 0 -2.10 7.60 1 9 0 1.40 10.40 -1 -9 0 4.20 6.10 1 9 0 -0.30 5.90 -1 10 0 10.20 9.90 1 -10 0 2.30 6.20 1 10 0 6.40 11.70 1 11 0 5.80 12.70 -1 11 0 -11.90 11.80 2 0 0 326.67 11.70 2 1 0 9999.00 307.17 2 2 0 1268.17 40.10 2 3 0 74.29 5.00 -2 4 0 3.20 4.20 -2 4 0 3.00 5.00 2 4 0 2.40 2.40 -2 -4 0 2.80 4.80 2 -5 0 296.37 14.70 -2 5 0 311.57 13.20 2 5 0 321.57 15.20 -2 5 0 300.37 14.20 -2 -5 0 308.47 13.30 2 5 0 310.07 12.20 2 5 0 299.17 13.60 -2 6 0 82.19 8.80 -2 6 0 81.59 8.10 2 6 0 83.99 10.20 2 6 0 80.19 9.60 2 -6 0 75.29 12.70 2 7 0 90.79 13.00 2 7 0 75.99 10.10 -2 7 0 82.49 8.10 -2 7 0 64.39 10.20 -2 -7 0 77.79 8.90 -2 8 0 19.50 9.90 2 8 0 15.50 6.50 -2 -8 0 12.40 6.30 -2 8 0 10.20 5.00 2 9 0 17.90 5.90 -2 9 0 10.30 9.20 -2 -9 0 30.60 6.00 2 9 0 32.10 11.00 2 -10 0 13.50 5.90 -2 10 0 24.30 9.90 2 10 0 -0.30 13.50 2 11 0 72.79 16.40 -2 11 0 42.20 12.30 3 0 0 -5.50 3.30 3 1 0 -0.80 2.70 3 2 0 2.20 2.90 3 3 0 1.10 4.70 -3 3 0 2.20 4.90 3 4 0 -4.00 7.00 -3 4 0 8.80 4.00 -3 4 0 -0.20 4.50 3 4 0 0.70 4.10 -3 -4 0 7.50 4.30 3 -4 0 -2.00 5.60 3 4 0 -0.10 3.00 3 5 0 -3.90 6.30 -3 5 0 0.50 5.60 -3 5 0 -1.80 4.50 3 5 0 3.30 5.80 3 -5 0 6.30 5.70 -3 -5 0 2.40 4.60 3 5 0 -2.50 4.30 3 -6 0 -10.40 9.00 3 6 0 1.10 6.40 -3 6 0 0.40 4.40 3 6 0 10.10 8.60 -3 -6 0 -4.10 4.60 -3 6 0 2.00 6.00 -3 7 0 14.80 7.00 -3 -7 0 4.00 5.20 3 7 0 3.70 14.70 -3 7 0 3.30 4.70 3 7 0 1.60 6.30 -3 -8 0 0.90 5.70 3 8 0 5.30 7.20 -3 8 0 -0.70 11.80 -3 9 0 -3.30 8.00 3 9 0 1.70 5.90 -3 10 0 -15.70 10.30 -3 11 0 4.30 12.30 4 0 0 445.66 17.20 -4 2 0 192.98 9.90 -4 2 0 175.48 9.20 4 2 0 177.18 9.30 -4 -2 0 178.18 9.10 -4 3 0 317.37 12.90 4 -3 0 283.27 13.20 4 3 0 268.37 12.10 -4 -3 0 267.07 11.70 -4 -3 0 266.37 11.50 -4 3 0 268.37 11.70 4 -4 0 248.68 12.60 4 4 0 245.58 12.00 -4 -4 0 258.57 11.20 -4 4 0 253.67 12.30 -4 4 0 238.58 10.50 4 4 0 232.98 14.50 4 5 0 0.60 6.70 4 5 0 -6.10 6.90 -4 5 0 7.20 4.50 4 5 0 7.30 7.10 -4 -5 0 11.40 4.60 4 -5 0 -3.70 6.30 -4 5 0 5.30 5.10 4 6 0 43.60 12.50 4 -6 0 31.70 7.90 -4 6 0 42.00 6.70 -4 -6 0 26.00 5.40 4 6 0 30.90 12.90 -4 6 0 35.50 8.30 4 7 0 41.60 8.10 -4 -7 0 49.40 6.10 -4 7 0 64.39 11.20 4 7 0 52.29 18.80 4 -7 0 42.30 10.20 -4 8 0 24.80 9.60 4 8 0 20.00 8.90 -4 9 0 2.90 9.60 4 9 0 13.90 5.50 4 10 0 29.70 17.90 -4 10 0 18.80 12.40 -5 0 0 -4.20 4.70 5 0 0 3.10 4.90 -5 0 0 7.60 3.70 5 -1 0 -6.40 6.80 -5 1 0 1.90 3.70 5 1 0 1.90 4.70 -5 1 0 -4.30 4.90 -5 -1 0 1.60 5.80 5 2 0 -4.20 4.50 -5 -2 0 -0.40 3.70 -5 -2 0 1.60 4.50 -5 2 0 -1.20 3.90 -5 2 0 2.90 5.30 5 -2 0 12.20 10.00 5 -3 0 -7.10 5.10 5 3 0 2.90 5.00 -5 3 0 0.50 5.20 -5 -3 0 4.20 4.40 -5 3 0 2.30 3.80 5 3 0 2.50 8.00 -5 -3 0 -1.30 3.90 -5 -4 0 1.30 4.20 5 4 0 4.70 6.50 5 -4 0 2.00 5.70 5 4 0 15.80 7.40 -5 -4 0 7.10 8.50 -5 4 0 -2.70 5.30 -5 4 0 -1.70 4.50 5 5 0 -4.20 9.30 -5 5 0 -0.90 6.40 5 5 0 3.90 7.10 5 -5 0 16.50 9.00 -5 -5 0 -4.00 4.30 5 6 0 5.50 7.10 5 6 0 -6.60 15.00 -5 6 0 16.70 8.20 -5 -6 0 8.70 4.70 5 7 0 58.79 22.60 5 -7 0 -0.30 9.70 5 7 0 -0.50 8.00 5 8 0 -5.40 6.60 -5 8 0 13.40 10.30 5 9 0 5.00 6.10 -5 9 0 1.40 10.10 -5 10 0 39.30 10.80 6 1 0 509.95 20.90 -6 -1 0 520.05 19.50 -6 1 0 544.95 20.00 -6 -1 0 547.75 18.00 6 1 0 439.66 26.50 -6 -2 0 -3.40 4.00 6 2 0 16.00 6.30 6 2 0 4.20 9.30 6 -2 0 8.10 10.80 -6 -2 0 1.80 5.20 -6 2 0 4.10 6.00 -6 -3 0 268.47 11.50 -6 3 0 270.07 13.30 -6 -3 0 268.27 12.50 6 -3 0 255.57 14.00 6 3 0 259.27 16.40 6 3 0 263.57 14.30 -6 4 0 75.79 9.10 6 -4 0 75.59 9.50 6 4 0 81.39 11.50 6 4 0 66.29 8.80 -6 -4 0 77.79 9.00 -6 5 0 193.58 13.70 6 5 0 215.08 15.70 6 -5 0 179.88 28.60 6 5 0 228.58 18.20 6 -5 0 205.08 14.00 6 -6 0 2.10 8.20 6 6 0 44.30 20.70 6 6 0 10.10 8.10 -6 6 0 -9.60 8.90 6 -7 0 38.50 10.20 6 7 0 34.40 8.20 -6 7 0 57.59 11.60 6 8 0 51.39 8.00 -6 8 0 48.50 11.50 -6 9 0 23.40 12.50 6 9 0 -4.10 7.40 -6 10 0 34.60 18.30 7 0 0 2.20 9.80 7 0 0 -0.50 9.60 -7 0 0 2.80 6.10 7 1 0 -9.70 8.80 7 -1 0 3.10 12.50 7 1 0 11.70 16.00 -7 -1 0 -3.40 5.90 -7 1 0 -5.30 6.10 -7 -2 0 3.30 6.40 7 -2 0 -6.60 7.20 7 -2 0 12.70 13.40 -7 2 0 1.30 6.50 7 2 0 4.10 9.70 7 2 0 6.40 9.00 -7 -3 0 2.10 6.30 7 3 0 -6.30 11.40 -7 3 0 -7.30 7.10 7 -3 0 3.80 6.60 7 -3 0 4.30 18.00 7 4 0 6.50 8.10 7 -4 0 7.30 6.50 -7 4 0 4.00 8.00 7 -4 0 14.60 20.00 -7 5 0 2.50 10.00 7 -5 0 12.00 8.40 7 5 0 -2.70 8.30 7 5 0 -13.90 17.60 7 6 0 -2.60 8.90 7 -6 0 7.80 9.30 -7 6 0 -10.80 10.10 7 -7 0 14.10 10.30 7 7 0 -3.20 7.50 -7 7 0 -0.20 10.80 7 8 0 0.40 7.00 -7 8 0 -11.60 11.30 -7 9 0 9.90 12.90 8 0 0 96.29 12.30 8 0 0 93.49 18.00 -8 0 0 101.89 11.40 8 1 0 -9.70 12.60 -8 -1 0 1.20 8.10 8 1 0 -3.60 9.40 8 -1 0 -6.00 16.00 -8 -2 0 74.39 12.60 -8 2 0 109.49 12.10 8 2 0 103.79 16.30 8 -2 0 92.99 11.40 8 2 0 83.89 10.90 8 3 0 583.34 25.30 -8 3 0 562.34 24.50 -8 -3 0 563.34 23.10 8 -3 0 529.15 23.40 8 3 0 480.25 30.40 -8 4 0 211.68 20.60 8 -4 0 214.78 16.20 8 4 0 166.88 28.90 8 4 0 240.38 19.50 8 5 0 86.79 11.20 -8 5 0 108.79 14.70 8 -5 0 82.39 13.60 8 -6 0 6.60 9.40 8 6 0 9.50 7.90 -8 6 0 17.60 11.40 -8 7 0 20.80 11.20 8 7 0 16.00 7.40 8 -7 0 5.20 13.80 -8 8 0 13.10 12.20 8 8 0 -10.80 10.30 9 0 0 4.80 21.80 -9 0 0 25.70 12.90 9 1 0 38.10 23.20 9 1 0 20.40 10.70 9 -1 0 31.40 23.40 -9 2 0 12.10 10.00 9 -2 0 16.70 18.50 -9 3 0 20.30 10.60 9 -3 0 -1.70 6.80 9 3 0 -0.40 11.20 9 -4 0 -3.60 7.70 9 4 0 7.70 9.40 -9 4 0 -3.60 10.40 9 -5 0 0.40 8.40 9 5 0 -2.60 8.50 -9 5 0 1.90 12.20 9 -6 0 9.40 12.20 9 6 0 -1.80 8.00 -9 6 0 -26.90 19.90 9 7 0 24.30 9.60 -9 7 0 -11.00 13.50 9 -7 0 -42.10 19.90 10 0 0 47.40 8.70 10 1 0 13.50 9.10 10 -1 0 10.30 7.50 10 2 0 167.48 16.10 10 -2 0 114.89 11.80 -10 3 0 -8.20 13.40 10 3 0 -4.60 13.80 -10 4 0 19.20 20.00 10 4 0 17.10 9.00 10 -4 0 4.90 8.10 10 -5 0 14.70 22.90 -10 5 0 16.30 20.80 10 -6 0 15.00 8.40 11 0 0 13.90 8.60 11 -1 0 2.90 7.90 11 1 0 -3.80 10.30 11 -2 0 -4.00 8.20 11 2 0 14.00 15.90 11 -3 0 6.30 15.00 11 -4 0 -2.80 9.90 12 0 0 27.20 12.20 12 -1 0 93.19 14.40 12 1 0 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7.20 9.60 -2 10 4 1.40 11.00 -2 -10 -4 14.70 6.80 2 10 -4 25.80 7.30 2 10 -4 8.70 11.30 -2 11 -4 34.90 12.00 -2 11 4 42.60 13.80 2 11 -4 41.00 13.70 3 0 4 32.30 3.30 3 1 4 55.39 4.20 3 -1 4 67.79 4.80 3 1 -4 67.69 5.50 3 2 4 59.19 4.90 3 2 -4 53.59 4.60 3 -2 4 44.10 5.30 -3 -3 4 364.26 13.50 3 3 4 359.56 14.90 -3 3 -4 342.77 14.50 -3 3 4 341.57 14.40 3 -3 4 349.67 14.40 3 3 -4 350.36 13.80 3 4 4 348.97 15.10 -3 4 -4 375.56 15.70 3 4 4 380.76 15.60 -3 -4 4 365.66 13.50 3 4 4 388.56 13.20 -3 -4 4 375.46 14.50 -3 4 -4 371.86 15.60 3 4 -4 372.06 14.20 3 -4 4 379.46 15.20 3 4 -4 374.16 15.10 -3 4 4 391.36 15.80 -3 -4 -4 352.86 16.20 -3 5 -4 171.48 10.90 3 5 4 164.98 11.00 -3 5 -4 174.58 10.80 3 5 4 162.08 10.30 -3 -5 4 168.88 8.50 -3 5 4 158.08 10.40 3 -5 4 185.48 10.70 3 5 -4 173.68 10.20 -3 -5 -4 155.28 11.30 3 5 -4 153.78 10.70 3 5 -4 176.28 17.90 3 6 4 17.90 9.70 -3 6 -4 15.50 5.40 -3 -6 4 16.20 4.20 -3 6 -4 10.20 5.80 3 6 4 10.60 5.10 -3 6 4 9.20 5.80 3 6 -4 14.50 9.10 3 -6 4 9.80 6.40 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33.90 7.50 8 1 4 14.00 13.80 8 -1 -4 2.20 17.80 -8 1 4 39.00 8.20 8 1 -4 11.00 15.80 8 -1 4 32.70 7.20 8 -1 4 54.29 15.50 -8 2 -4 57.29 13.60 8 2 4 64.29 11.70 -8 -2 4 65.49 10.40 8 -2 4 60.99 10.30 8 2 -4 94.69 18.80 8 -2 4 49.50 17.10 -8 2 4 60.39 9.50 8 3 4 35.20 17.90 8 -3 -4 19.30 21.80 -8 3 -4 31.20 12.40 -8 -3 4 19.60 7.60 8 3 4 20.70 7.60 8 -3 -4 13.20 8.40 8 -3 4 19.00 7.50 8 3 -4 11.60 13.00 -8 3 4 17.50 8.50 8 3 -4 35.80 16.60 8 -4 -4 31.90 28.70 8 4 4 88.79 13.70 -8 4 -4 118.89 15.50 8 -4 -4 89.29 15.60 8 4 4 182.18 36.30 -8 -4 4 104.29 14.50 8 -4 4 65.39 13.60 -8 4 4 92.99 14.10 8 4 -4 71.29 24.60 8 4 -4 101.49 14.00 8 -5 -4 3.20 9.70 -8 5 -4 11.50 12.00 8 5 4 -5.50 6.40 -8 5 4 -1.10 9.00 8 5 -4 24.40 11.10 8 -5 4 2.70 7.50 8 6 4 6.50 6.50 8 -6 -4 -6.40 11.60 -8 6 -4 27.60 18.60 8 -6 4 11.50 8.50 -8 6 4 11.60 9.40 8 6 -4 19.30 10.20 -8 7 4 81.19 15.00 8 7 -4 76.49 10.80 8 -7 4 69.89 11.70 -8 8 -4 51.69 17.00 8 8 -4 47.80 11.40 -8 8 4 34.50 12.10 -9 0 4 -5.60 9.80 9 0 4 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54.39 7.70 1 5 -5 47.00 9.80 1 5 -5 43.20 9.60 1 -5 5 39.80 7.00 -1 5 5 43.90 5.30 1 6 5 -9.80 11.60 1 6 5 9.30 6.60 -1 6 5 10.00 7.60 1 6 -5 9.00 6.30 1 6 -5 9.10 7.60 -1 6 5 12.40 6.30 1 6 -5 9.40 9.60 1 7 5 36.40 5.00 1 7 5 51.69 8.10 1 7 5 36.40 12.90 -1 7 -5 42.50 7.10 -1 -7 5 48.20 7.00 -1 7 5 52.09 8.20 1 7 -5 45.30 8.40 -1 7 5 21.60 10.60 1 8 5 6.60 22.00 1 8 5 18.00 10.10 -1 8 -5 22.00 9.60 -1 8 -5 28.60 7.70 -1 8 5 40.60 10.00 1 8 -5 27.50 7.50 1 9 5 1.90 11.20 -1 9 -5 2.60 9.10 -1 9 -5 5.80 6.30 1 9 -5 7.60 6.60 -1 -9 -5 -7.10 6.90 -1 9 5 16.70 12.00 1 -10 -5 21.40 6.50 1 10 5 50.09 15.70 -1 10 -5 22.00 9.70 1 10 -5 29.10 7.20 -1 -10 -5 29.20 6.80 -1 10 5 34.40 12.70 1 10 -5 1.10 11.00 -1 11 -5 10.70 11.40 1 -11 -5 15.60 8.90 -1 11 5 48.20 15.10 1 11 -5 9.60 11.50 2 0 5 0.70 1.60 2 1 5 160.18 6.60 2 -1 5 161.48 6.60 2 1 -5 172.48 7.30 2 -1 5 129.99 6.00 2 2 5 1183.78 38.80 2 -2 5 1184.48 38.00 2 -2 5 1293.27 37.90 2 2 -5 1169.58 38.30 2 3 5 541.25 19.30 -2 -3 5 526.95 18.60 2 3 -5 527.15 18.20 -2 3 5 527.95 19.80 2 3 -5 530.45 18.10 2 4 5 3.20 3.90 -2 4 -5 0.80 7.00 2 4 5 1.20 4.30 2 -4 5 7.70 4.50 2 4 -5 9.40 3.20 2 4 -5 3.10 4.00 -2 4 5 3.20 5.00 -2 -5 5 494.65 17.20 2 5 5 497.95 19.80 2 5 5 478.65 18.00 -2 5 -5 485.15 19.60 2 5 -5 497.75 19.20 -2 5 5 496.65 19.60 2 5 -5 471.95 23.30 2 5 -5 477.35 18.40 2 -5 5 514.35 18.70 -2 6 -5 3.00 5.20 2 6 5 0.70 7.70 2 6 5 9.70 4.30 -2 6 -5 10.50 5.70 -2 -6 5 -4.60 4.00 2 -6 5 -1.80 5.60 -2 6 5 -4.50 6.20 2 6 -5 11.10 8.30 2 6 -5 7.10 9.80 -2 7 -5 8.70 7.10 2 7 5 14.70 12.20 -2 7 -5 10.00 6.20 2 7 5 0.90 4.30 -2 -7 -5 20.50 6.70 2 7 -5 26.20 8.60 -2 7 5 2.60 6.40 -2 8 -5 16.00 6.70 -2 8 -5 14.00 13.10 2 8 5 16.00 12.20 2 8 5 27.90 22.20 -2 8 5 3.50 10.80 2 8 -5 8.40 7.90 -2 -8 -5 10.20 7.40 -2 9 -5 40.60 9.80 -2 9 -5 61.39 10.00 2 9 5 65.29 14.50 -2 -9 -5 44.10 8.00 2 -9 5 53.89 9.00 -2 9 5 50.59 10.40 2 9 -5 51.09 8.70 2 10 5 44.50 19.70 -2 10 -5 0.30 10.10 -2 -10 -5 23.00 6.70 2 10 -5 10.10 12.20 2 10 -5 24.10 7.40 -2 10 5 -1.40 12.80 2 -11 -5 5.00 9.40 -2 11 -5 5.20 11.20 2 11 -5 15.30 13.00 -2 11 5 32.10 14.00 3 0 5 0.30 2.00 3 1 5 341.87 12.80 3 -1 5 324.87 12.70 3 1 -5 382.96 13.90 -3 -2 5 474.95 17.60 3 2 5 493.45 17.90 3 -2 5 503.45 17.30 -3 2 5 503.65 18.60 -3 -3 5 284.27 11.60 3 3 5 295.87 12.60 3 3 5 279.47 12.20 -3 3 -5 293.67 13.10 -3 3 5 286.47 12.50 3 -3 5 289.47 12.50 3 3 -5 288.37 12.00 -3 4 -5 -1.60 5.50 -3 4 -5 3.00 5.60 -3 -4 5 0.50 3.30 3 4 5 3.90 4.80 3 4 5 1.00 4.30 3 -4 5 6.30 4.60 3 4 -5 0.40 4.80 3 4 -5 3.10 3.00 -3 -4 -5 -3.40 6.20 -3 4 5 5.10 4.40 3 5 5 16.00 8.80 -3 5 -5 31.40 6.60 3 5 5 38.60 7.00 -3 5 -5 39.60 6.50 3 5 -5 27.10 12.20 3 -5 5 40.30 6.20 -3 5 5 30.00 6.30 -3 -5 -5 28.90 6.90 3 5 -5 35.50 6.40 3 5 -5 47.10 8.00 -3 6 -5 6.80 5.30 3 6 5 2.90 4.70 3 6 5 4.00 9.30 -3 6 -5 8.50 6.70 3 6 -5 25.90 10.40 3 6 -5 24.00 11.30 3 -6 5 2.40 6.20 -3 -6 -5 12.40 6.60 -3 6 5 4.50 5.80 3 6 -5 3.40 7.90 -3 7 -5 26.50 8.50 3 7 5 28.40 5.40 3 7 5 24.00 14.50 -3 7 -5 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13.50 14.50 10 -4 -5 27.90 9.90 -10 4 5 27.50 11.80 10 4 -5 21.80 13.80 10 -4 5 32.50 8.20 10 -5 -5 9.50 8.70 10 5 -5 26.50 13.30 -10 5 5 12.60 13.70 10 -6 5 31.10 7.20 -10 6 5 43.00 13.30 11 0 5 -2.30 11.10 11 0 -5 -6.00 8.80 11 -1 -5 15.90 8.80 -11 1 5 20.40 15.50 11 1 -5 12.30 9.60 11 -1 5 -1.60 9.60 11 2 5 67.09 20.00 11 -2 -5 29.40 8.70 11 2 -5 43.70 11.70 11 -2 5 31.00 9.80 -11 2 5 22.40 13.20 11 -3 -5 -9.90 10.00 -11 3 5 37.90 14.70 11 3 -5 -6.00 13.10 11 -3 5 3.10 9.40 11 -4 -5 16.50 8.20 11 4 -5 5.30 25.90 11 -4 5 25.50 10.00 12 0 -5 -0.20 11.30 12 -1 -5 -15.30 11.00 12 1 -5 14.60 12.50 12 -1 5 -12.30 11.90 0 0 -6 1145.39 35.00 0 0 -6 1128.79 34.60 0 0 6 1097.19 34.80 0 1 6 -1.80 1.50 0 1 -6 -1.70 1.30 0 2 6 2277.27 71.59 0 2 -6 2328.37 71.09 0 3 -6 1.40 2.10 0 3 6 0.50 2.50 0 4 6 114.19 6.80 0 4 6 119.49 9.40 0 4 -6 114.39 6.30 0 4 6 108.79 7.30 0 5 6 2.80 5.10 0 5 -6 -4.30 8.50 0 5 -6 3.20 3.40 0 5 6 7.90 6.10 0 5 6 2.70 3.50 0 6 6 29.70 7.00 0 6 6 34.80 8.50 0 6 6 21.00 8.30 0 6 -6 40.50 8.20 0 7 6 24.40 10.10 0 7 6 -0.90 8.10 0 7 6 8.00 14.00 0 7 -6 -5.80 6.90 0 -7 6 0.90 4.10 0 8 6 123.09 22.10 0 8 -6 72.49 12.50 0 8 6 83.19 13.80 0 9 -6 3.90 6.60 0 9 -6 5.90 8.90 0 9 6 17.10 11.80 0 -10 -6 17.10 6.80 0 10 -6 29.70 10.00 0 10 6 35.00 14.60 0 10 -6 28.80 7.20 0 11 -6 -2.30 12.10 1 0 6 0.40 1.30 1 0 6 0.00 1.10 -1 1 -6 382.16 12.90 1 1 6 385.06 13.40 1 -1 6 406.66 13.20 -1 1 6 371.16 13.20 1 2 6 116.39 5.90 -1 2 -6 118.19 5.60 1 2 -6 121.59 5.30 -1 2 6 121.09 5.80 1 2 -6 114.49 4.80 1 -3 -6 787.02 24.40 1 3 6 771.12 26.20 1 3 -6 794.82 24.70 -1 3 6 760.72 26.00 1 3 -6 731.83 25.10 1 4 6 3.40 3.60 1 -4 -6 -0.80 3.40 -1 -4 6 10.20 3.40 1 4 6 1.30 3.40 1 4 -6 -0.60 2.60 1 4 -6 3.10 3.30 -1 4 6 7.40 5.10 -1 4 6 -0.40 3.80 1 -4 6 3.30 4.30 -1 5 -6 384.06 18.20 1 5 6 380.26 16.60 -1 -5 6 407.96 14.50 1 5 6 398.36 14.70 -1 5 6 404.36 16.70 -1 5 6 402.66 16.70 1 -5 6 400.16 15.60 1 5 -6 388.86 21.80 1 5 -6 392.76 14.80 1 5 -6 420.76 15.80 1 6 6 87.79 7.70 1 6 6 78.99 12.80 -1 6 -6 104.09 13.20 -1 -6 6 84.49 7.00 1 6 6 80.29 10.70 1 6 6 80.19 10.20 1 6 -6 84.79 13.00 1 6 -6 69.69 12.30 -1 6 6 87.49 11.20 -1 6 6 58.39 9.00 -1 -7 6 11.60 4.50 -1 7 -6 7.70 6.60 1 7 6 7.50 7.80 1 7 -6 25.10 8.20 -1 7 6 10.90 9.70 -1 7 6 13.10 8.00 -1 8 -6 111.99 17.10 -1 8 -6 106.09 13.30 1 8 6 93.49 13.00 1 8 6 157.48 27.80 1 8 -6 111.89 13.80 -1 8 6 90.79 13.70 1 -8 6 77.39 8.80 -1 9 -6 1.40 9.20 1 9 6 -11.60 13.50 -1 9 -6 11.10 6.30 -1 -9 -6 -8.50 7.10 -1 9 6 -18.90 10.20 1 9 -6 2.50 6.90 -1 10 -6 20.30 8.20 1 -10 -6 -0.90 6.70 -1 10 -6 17.90 10.10 1 10 6 -20.10 18.50 1 10 -6 7.50 6.90 -1 -10 -6 6.60 6.60 -1 10 6 -6.10 12.30 1 10 -6 -8.00 10.10 -1 11 -6 3.60 12.10 -1 11 6 9.70 19.50 2 0 6 220.28 8.30 2 0 6 233.68 8.30 2 1 6 0.50 1.70 2 -1 6 -1.30 2.00 2 -1 6 -0.10 1.40 2 2 6 461.35 16.40 -2 -3 6 152.78 7.60 -2 3 6 153.28 9.40 2 3 -6 161.08 7.20 2 3 -6 158.58 7.10 2 4 6 3.90 3.90 2 4 6 14.80 4.60 -2 4 -6 31.80 12.80 2 4 -6 18.80 4.10 2 4 -6 11.20 3.00 -2 4 6 11.70 4.80 2 -4 6 13.80 4.40 2 5 6 3.30 4.10 2 5 6 10.30 5.80 -2 5 -6 12.90 6.50 -2 5 6 24.60 10.80 2 5 -6 8.70 4.50 2 -5 6 0.40 4.60 -2 6 -6 21.50 6.40 2 6 6 25.20 8.70 2 6 6 23.70 4.60 -2 6 -6 21.60 6.70 2 6 -6 16.40 7.50 2 6 -6 14.00 9.60 -2 6 6 24.90 6.00 2 -6 6 22.80 5.90 2 7 6 62.29 14.20 -2 7 -6 44.10 7.50 2 7 6 53.39 9.90 2 7 6 56.49 6.80 -2 7 -6 50.39 8.60 -2 7 6 51.39 9.30 -2 7 6 59.79 9.80 -2 -7 -6 52.59 8.20 2 7 -6 38.40 9.20 2 8 6 12.70 14.50 -2 8 -6 14.80 6.90 2 8 6 -2.70 25.50 -2 8 6 -5.90 12.30 -2 -8 -6 16.70 7.80 2 8 -6 16.00 8.80 -2 9 -6 7.20 9.30 2 9 6 31.60 14.80 -2 9 -6 27.70 6.30 -2 9 6 28.60 10.00 2 9 -6 19.60 8.10 -2 -9 -6 24.00 7.40 -2 10 -6 73.49 12.40 2 10 -6 84.99 15.00 2 10 -6 102.99 12.70 -2 -10 -6 59.19 10.30 -2 10 6 97.29 15.60 2 -11 -6 -8.90 9.50 -2 11 -6 9.60 11.30 2 11 -6 4.50 13.00 3 0 6 218.08 8.70 3 1 6 130.09 6.50 3 -1 6 126.69 5.90 -3 -2 6 75.89 5.60 3 2 6 74.19 5.80 3 -2 6 55.29 4.90 -3 2 6 77.29 6.90 -3 -3 6 126.59 7.10 3 3 6 142.09 8.10 -3 3 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28.40 6.10 -3 4 27 19.10 5.10 3 5 27 -0.20 5.30 3 -5 27 3.00 6.60 3 6 27 -4.90 6.00 3 -6 27 5.70 12.80 -3 6 27 1.80 3.70 3 7 27 20.90 8.80 4 0 27 5.60 5.40 4 1 27 16.30 6.40 4 -1 27 17.20 6.80 4 3 27 -0.10 5.50 4 -3 27 6.30 5.80 4 4 27 6.00 5.90 4 -4 27 25.10 7.30 -4 4 27 17.50 4.40 4 5 27 29.70 7.00 4 -5 27 40.50 9.80 -4 5 27 18.10 4.30 4 6 27 -7.00 10.50 -4 6 -27 -26.50 14.70 -4 6 27 2.40 3.80 5 0 27 5.60 6.60 -5 0 27 -0.50 11.70 5 1 27 14.70 6.00 -5 -1 27 35.30 10.60 5 -1 27 13.50 6.70 5 2 27 20.60 6.70 5 -2 27 26.20 7.40 5 3 27 8.50 7.10 5 -3 27 22.10 9.40 5 4 27 -13.30 7.50 5 -4 27 -11.30 10.80 -5 5 -27 9.00 14.10 5 -5 27 -22.10 12.50 -5 6 -27 14.50 12.50 6 0 27 13.00 14.00 6 1 27 31.90 9.40 -6 -1 27 2.20 19.40 -6 1 27 13.50 11.50 6 -1 27 46.30 9.30 6 2 27 -2.50 8.90 6 -2 27 0.10 10.20 -6 -2 -27 11.50 16.80 -6 3 -27 -17.80 14.00 -6 4 -27 7.00 12.80 6 4 27 -23.80 12.60 -6 -4 -27 -7.70 15.20 -6 5 -27 42.50 12.30 -6 -5 -27 0.20 19.50 -7 0 -27 -6.90 12.00 -7 0 27 16.10 9.10 -7 1 -27 7.20 11.60 -7 -1 27 17.50 8.60 -7 1 27 7.10 10.70 -7 -1 -27 -18.20 12.30 -7 2 -27 -3.30 11.90 -7 -2 -27 -5.60 12.30 -7 3 -27 28.20 11.70 -7 -3 -27 38.30 12.10 -7 4 -27 44.40 12.30 -7 -4 -27 16.80 12.70 -8 0 -27 -13.60 10.70 -8 1 -27 9.10 11.30 -8 -1 -27 -4.70 11.10 0 0 28 178.68 10.10 0 -1 28 -7.70 4.10 0 1 28 -1.30 4.20 0 -2 28 7.90 4.30 0 2 28 3.00 4.60 0 3 28 5.30 4.80 0 -3 28 7.20 4.30 0 -4 28 21.40 5.20 0 4 28 16.20 5.40 0 5 28 -7.00 4.30 0 -5 28 1.90 3.80 0 6 28 2.30 4.40 0 7 28 -9.30 4.90 -1 0 28 9.80 4.50 1 0 28 9.40 4.20 1 1 28 20.90 4.60 -1 -1 28 18.50 4.70 1 -1 28 24.00 5.00 -1 1 28 21.30 4.70 -1 -2 28 12.50 4.40 1 2 28 1.90 4.60 1 -2 28 4.00 4.30 -1 2 28 8.80 5.60 -1 -3 28 24.50 4.80 1 3 28 10.70 5.50 1 -3 28 25.40 5.20 -1 3 28 21.50 5.40 -1 -4 28 0.40 3.90 -1 4 28 0.60 4.60 1 -4 28 -2.80 4.20 -1 -5 28 35.50 5.20 1 -5 28 28.60 5.40 -1 5 28 45.70 6.80 1 6 28 -2.80 4.80 -1 6 28 -0.40 4.40 -1 7 28 5.20 4.50 2 0 28 47.70 7.40 2 1 28 6.70 4.60 2 -1 28 17.30 7.70 -2 -2 28 4.60 4.60 2 2 28 2.10 4.70 2 -2 28 0.50 4.70 2 3 28 -0.40 7.10 -2 3 28 0.80 6.40 2 4 28 3.10 5.50 -2 -4 28 5.00 3.90 2 -4 28 -0.60 4.60 -2 4 28 4.80 4.50 2 5 28 -6.20 4.90 2 -5 28 -6.70 4.70 -2 5 28 -3.50 3.90 2 6 28 7.20 5.40 -2 6 28 5.00 4.10 2 7 28 3.40 6.60 -2 7 28 13.20 5.40 3 0 28 47.00 8.00 3 1 28 8.20 5.30 3 -1 28 9.30 5.50 3 2 28 40.20 7.10 -3 -2 28 29.90 10.30 3 -2 28 46.90 8.80 -3 -3 28 28.30 5.00 3 -3 28 31.90 5.80 -3 3 28 27.30 6.30 3 4 28 27.50 5.50 -3 4 28 21.50 4.40 3 -4 28 24.30 6.00 3 5 28 11.40 5.40 -3 5 28 10.70 4.00 3 6 28 19.10 6.50 4 0 28 71.29 10.80 4 1 28 8.10 5.80 4 -1 28 10.50 6.30 4 2 28 10.20 5.20 4 -2 28 14.10 5.80 4 3 28 11.90 5.20 4 -3 28 21.00 6.70 4 4 28 8.30 5.60 4 -4 28 -4.00 7.20 -4 4 28 9.60 4.30 4 5 28 55.09 7.40 -4 5 28 47.80 6.50 4 -5 28 69.79 11.00 4 6 28 1.10 9.30 -4 6 28 -3.30 6.00 5 0 28 81.19 10.80 5 1 28 134.99 11.90 5 -1 28 145.69 12.90 5 2 28 9.60 6.30 5 -2 28 10.90 7.70 5 3 28 8.40 6.50 5 -3 28 -4.30 8.30 -5 4 -28 50.19 18.50 5 4 28 35.30 8.10 5 -4 28 9.00 12.10 -5 4 28 24.00 4.20 5 5 28 2.20 10.00 -5 5 28 5.90 4.10 6 0 28 -2.10 9.00 6 1 28 61.69 8.60 -6 1 -28 58.89 17.90 6 -1 28 65.49 10.00 -6 2 -28 -12.80 15.90 6 2 28 16.60 9.00 6 -2 28 -11.00 10.80 -6 -2 -28 13.00 27.70 -6 3 -28 29.50 14.90 -6 -3 -28 -7.40 17.10 -6 4 -28 9.20 13.10 6 4 28 -5.20 14.20 -6 -4 -28 -27.10 16.40 -7 0 -28 139.19 14.10 -7 1 -28 5.10 12.50 -7 -1 -28 36.20 12.50 -7 2 -28 -24.80 12.30 -7 -2 -28 9.50 12.50 -7 3 -28 10.70 12.40 0 0 29 3.80 4.50 0 1 29 3.10 4.40 0 -1 29 3.00 4.50 0 -2 29 84.49 8.60 0 2 29 98.69 8.70 0 3 29 -4.70 5.20 0 -3 29 -5.20 4.50 0 -4 29 9.50 3.90 0 4 29 8.30 4.60 0 5 29 -5.20 4.40 0 -5 29 1.80 3.80 0 6 29 16.30 4.50 -1 0 29 -5.30 4.50 1 0 29 7.40 4.30 1 1 29 9.80 4.80 -1 -1 29 7.20 5.20 -1 1 29 6.90 4.80 1 -1 29 11.50 4.60 1 2 29 73.49 8.90 -1 -2 29 63.39 8.00 1 -2 29 54.59 8.40 -1 2 29 59.89 8.50 1 3 29 9.10 5.50 -1 -3 29 16.60 4.90 -1 3 29 14.30 4.90 1 -3 29 12.60 5.20 1 4 29 17.90 4.70 -1 -4 29 20.30 4.10 -1 4 29 16.60 4.40 1 -4 29 9.20 4.50 1 5 29 26.20 5.10 1 -5 29 39.90 7.10 -1 5 29 20.00 4.40 1 6 29 12.10 4.60 -1 6 29 13.70 4.00 2 0 29 -2.10 4.90 2 1 29 2.90 5.00 2 -1 29 -1.10 5.10 -2 -2 29 32.40 5.40 -2 -3 29 104.79 7.60 2 3 29 97.49 8.80 -2 3 29 107.09 7.70 2 -3 29 103.19 8.90 2 4 29 15.20 5.00 -2 -4 29 22.60 4.30 -2 4 29 18.20 4.30 2 -4 29 18.70 4.90 2 5 29 12.10 5.20 -2 5 29 10.60 4.00 2 -5 29 12.70 5.30 2 6 29 -1.60 5.60 -2 6 29 5.00 4.00 3 1 29 5.10 5.80 3 -1 29 3.60 6.10 -3 -2 29 -2.80 3.90 3 2 29 -4.70 4.60 3 -2 29 -2.10 4.90 3 3 29 2.60 4.40 -3 3 29 -2.60 4.10 3 -3 29 -1.50 4.90 3 4 29 3.50 4.60 3 -4 29 -6.00 5.20 -3 4 29 -3.60 3.80 3 5 29 6.00 5.00 -3 5 29 6.70 3.90 3 -5 29 11.80 7.50 3 6 29 1.80 7.10 -3 6 29 -2.10 4.10 4 0 29 -5.60 5.10 4 1 29 0.50 4.70 4 -1 29 -5.80 5.00 4 2 29 -3.60 5.10 4 -2 29 0.60 5.30 4 3 29 4.60 4.90 4 -3 29 -1.30 5.60 4 4 29 16.60 5.80 -4 4 29 17.90 4.20 4 -4 29 21.80 8.20 4 5 29 6.60 7.20 -4 5 29 2.70 3.90 4 -5 29 11.40 7.80 5 0 29 6.10 5.90 5 1 29 2.70 6.20 5 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38.30 6.90 2 0 30 33.00 5.90 2 1 30 12.40 4.90 -2 -1 30 15.80 4.80 2 -1 30 11.90 5.40 2 2 30 11.80 4.40 -2 -2 30 7.60 4.20 2 -2 30 13.10 4.80 2 3 30 36.30 5.30 -2 -3 30 34.80 6.10 2 -3 30 44.90 7.30 -2 3 30 39.20 6.30 2 4 30 6.70 4.40 -2 4 30 6.90 3.90 2 -4 30 0.90 4.30 2 5 30 26.70 4.90 -2 5 30 26.70 4.20 2 -5 30 33.30 4.60 2 6 30 7.10 6.30 3 0 30 7.60 6.60 3 1 30 1.50 4.50 3 -1 30 3.10 4.90 3 2 30 1.70 4.50 -3 -2 30 7.80 4.00 3 -2 30 -3.10 4.40 3 3 30 50.59 7.60 3 -3 30 44.80 8.10 3 4 30 -0.10 4.50 -3 4 30 10.20 4.10 3 -4 30 14.60 5.60 3 5 30 6.20 5.40 -3 5 30 11.60 4.00 3 -5 30 4.10 5.10 4 0 30 54.29 8.70 4 1 30 10.90 4.70 4 -1 30 16.90 5.20 4 2 30 -1.60 4.60 4 -2 30 5.90 5.30 4 3 30 27.10 5.50 4 4 30 27.90 6.20 4 -4 30 24.20 8.90 4 5 30 7.80 7.70 4 -5 30 -13.30 8.10 -4 5 30 10.00 4.00 5 0 30 83.39 10.90 5 1 30 13.00 6.50 5 -1 30 5.30 6.70 5 2 30 -2.30 6.30 5 -2 30 8.80 7.90 5 3 30 -0.50 7.10 5 -3 30 -0.40 10.50 5 4 30 34.40 9.60 5 -4 30 -3.70 12.60 6 0 30 18.20 15.30 6 1 30 -18.80 10.90 6 -1 30 -23.50 11.40 6 2 30 -2.30 9.70 6 3 30 10.00 11.60 0 0 31 0.00 5.10 0 -1 31 8.70 4.30 0 1 31 9.10 5.50 0 2 31 7.90 4.10 0 -2 31 5.20 3.70 0 3 31 -6.10 3.90 0 -3 31 1.80 3.40 0 4 31 28.60 4.40 0 -4 31 41.10 5.70 0 5 31 -6.00 3.80 0 6 31 5.20 4.10 -1 0 31 0.50 3.90 1 0 31 1.40 3.90 -1 -1 31 38.40 5.60 1 1 31 28.70 4.80 -1 1 31 46.40 6.80 1 -1 31 35.70 5.30 1 2 31 5.00 3.90 -1 -2 31 2.00 3.70 1 -2 31 5.60 3.90 -1 2 31 2.90 4.10 1 3 31 0.80 3.80 -1 -3 31 0.90 3.70 1 -3 31 -2.40 3.30 -1 3 31 11.50 4.10 1 4 31 8.20 4.00 -1 -4 31 11.90 3.80 1 -4 31 6.00 3.90 -1 4 31 5.70 3.90 1 5 31 3.30 4.10 1 -5 31 -2.80 3.90 -1 5 31 7.10 4.00 2 0 31 7.00 3.90 2 1 31 -0.90 3.90 -2 -1 31 1.50 3.80 2 -1 31 8.10 4.20 2 2 31 -2.80 3.80 -2 -2 31 9.70 3.80 2 -2 31 -0.60 4.00 2 3 31 38.40 6.50 -2 -3 31 23.20 4.30 -2 3 31 22.00 4.30 2 -3 31 25.80 4.30 2 4 31 3.30 4.10 2 -4 31 5.10 4.40 -2 4 31 3.00 4.20 2 5 31 7.10 4.40 -2 5 31 5.60 4.00 2 -5 31 -6.20 4.60 3 0 31 4.20 4.80 3 1 31 6.50 4.20 3 -1 31 0.10 4.50 3 2 31 3.10 4.10 3 -2 31 8.70 4.40 3 3 31 9.10 4.30 3 -3 31 19.60 4.60 3 4 31 4.30 4.20 -3 4 31 14.10 4.40 3 -4 31 6.70 6.10 3 5 31 1.20 6.60 3 -5 31 -4.50 5.70 -3 5 31 4.70 3.90 4 0 31 -1.10 4.60 4 1 31 15.60 5.00 4 -1 31 19.10 5.20 4 2 31 -3.40 4.50 4 -2 31 0.80 5.40 4 3 31 27.50 5.40 4 -3 31 18.30 6.90 4 4 31 -4.80 6.80 4 -4 31 -11.80 9.20 5 0 31 8.30 6.90 5 1 31 25.70 6.30 5 -1 31 27.10 7.30 5 2 31 16.40 6.90 5 -2 31 20.40 8.60 5 3 31 24.30 8.10 5 -3 31 28.70 10.40 6 0 31 -10.50 11.20 6 1 31 11.10 11.50 6 2 31 -5.70 12.80 0 0 32 60.69 6.60 0 1 32 5.80 4.10 0 -1 32 -1.40 3.80 0 2 32 2.00 4.00 0 -2 32 4.90 3.60 0 -3 32 5.00 3.50 0 3 32 -1.50 3.70 0 4 32 34.80 4.40 0 -4 32 42.40 5.50 0 5 32 -2.70 3.90 1 0 32 36.10 6.30 -1 0 32 37.70 4.50 -1 -1 32 15.40 3.90 1 1 32 13.70 4.20 1 -1 32 8.00 3.90 -1 1 32 12.80 4.10 -1 -2 32 0.70 3.50 1 2 32 4.20 3.70 -1 2 32 -0.90 3.90 1 -2 32 8.70 3.80 -1 -3 32 1.70 3.50 1 3 32 -2.00 3.80 -1 3 32 -5.90 3.80 1 -3 32 2.10 3.40 1 4 32 19.20 4.20 -1 4 32 24.30 4.00 1 -4 32 27.50 4.30 1 5 32 -2.50 4.10 -1 5 32 2.50 4.80 2 0 32 -3.80 4.10 2 1 32 -4.80 3.70 2 -1 32 3.00 3.90 -2 -2 32 12.00 3.80 2 2 32 9.50 4.00 2 -2 32 7.10 3.90 2 3 32 3.30 3.70 -2 3 32 2.30 3.80 2 -3 32 1.80 3.80 2 4 32 15.90 4.30 -2 4 32 17.80 4.20 2 -4 32 18.40 4.70 2 5 32 22.50 5.20 2 -5 32 21.50 4.80 -2 5 32 12.80 4.10 3 0 32 -6.70 4.10 3 1 32 4.10 4.00 3 -1 32 6.40 4.10 3 2 32 15.00 4.50 3 -2 32 9.70 4.40 3 3 32 1.80 4.30 3 -3 32 6.30 4.90 3 4 32 1.10 4.90 3 -4 32 20.90 7.00 4 0 32 8.80 5.10 4 1 32 1.40 5.00 4 -1 32 -3.10 5.00 4 2 32 3.60 4.70 4 -2 32 -12.10 5.90 4 3 32 12.90 7.10 4 -3 32 20.30 9.40 5 0 32 20.30 8.20 5 1 32 5.30 12.20 5 2 32 11.50 6.90 5 -2 32 7.60 9.20 0 0 33 -1.40 3.70 0 -1 33 0.10 3.60 0 1 33 1.10 3.70 0 2 33 -2.00 3.60 0 -2 33 7.70 3.60 0 -3 33 1.20 3.50 0 3 33 3.70 3.80 0 -4 33 43.80 6.50 0 4 33 43.00 6.70 -1 0 33 -0.90 3.80 1 0 33 2.80 3.80 1 1 33 1.00 3.50 -1 -1 33 -0.10 3.60 1 -1 33 3.60 3.60 -1 1 33 -4.50 3.90 -1 -2 33 5.00 3.70 1 2 33 -3.70 3.60 -1 2 33 -1.30 4.00 1 -2 33 2.70 3.60 -1 -3 33 35.60 5.80 1 3 33 26.80 4.00 -1 3 33 30.20 4.20 1 -3 33 36.20 5.80 1 4 33 16.30 3.80 1 -4 33 20.90 4.30 2 0 33 1.90 3.80 2 1 33 4.60 3.60 2 -1 33 4.50 3.80 -2 -2 33 10.60 4.30 2 -2 33 8.70 3.80 2 3 33 3.20 3.80 2 -3 33 6.80 4.10 2 4 33 6.80 4.30 2 -4 33 0.90 5.60 -2 4 33 1.20 4.10 3 0 33 6.20 4.00 3 1 33 9.00 4.20 3 -1 33 6.10 4.10 3 2 33 15.10 4.10 3 -2 33 9.80 4.50 3 3 33 2.20 4.30 3 -3 33 7.00 5.40 4 0 33 5.60 5.40 4 1 33 13.30 5.10 4 -1 33 9.40 5.90 4 2 33 0.60 5.50 4 -2 33 10.80 8.00 4 3 33 -3.30 5.90 4 -3 33 -12.20 8.40 5 0 33 11.10 8.20 5 1 33 9.60 8.60 5 -1 33 5.60 8.80 0 0 34 11.50 3.80 0 1 34 4.10 3.80 0 -1 34 0.40 3.50 0 -2 34 56.19 6.00 0 2 34 43.10 4.80 0 -3 34 -4.40 3.70 0 3 34 3.10 3.90 0 4 34 2.20 3.90 1 0 34 8.30 3.60 -1 0 34 2.10 3.80 1 1 34 -3.50 3.50 -1 -1 34 -7.70 4.00 1 -1 34 -4.30 3.40 1 2 34 2.60 3.50 -1 -2 34 4.60 3.90 1 -2 34 0.70 3.30 -1 2 34 15.20 9.40 -1 -3 34 8.10 4.40 1 3 34 2.40 3.70 1 -3 34 0.00 3.70 2 0 34 17.90 3.80 2 1 34 3.10 3.80 2 -1 34 1.10 3.40 2 2 34 9.50 3.40 2 -2 34 3.40 3.60 2 3 34 7.10 3.80 2 -3 34 -1.10 4.50 3 0 34 13.00 4.20 3 1 34 -3.80 4.00 3 -1 34 -0.90 4.20 3 2 34 15.30 4.60 3 -2 34 15.40 5.10 4 0 34 -3.30 6.00 4 1 34 17.10 6.20 4 -1 34 8.80 6.30 0 0 35 3.50 4.40 0 1 35 -1.90 3.90 0 -2 35 -3.70 4.20 0 3 35 -7.10 3.80 0 -3 35 1.80 4.20 1 0 35 -2.50 3.60 1 1 35 34.30 6.00 1 -1 35 43.20 6.00 -1 -2 35 8.10 4.80 1 2 35 -0.40 3.80 1 -2 35 5.20 4.20 2 0 35 -1.30 3.60 2 1 35 8.20 3.90 2 -1 35 14.00 3.90 3 1 35 26.50 5.40 3 -1 35 5.90 4.80 0 0 36 116.39 7.90 0 -1 36 -1.70 4.60 0 1 36 -2.10 3.90 1 0 36 11.20 3.80 1 1 36 17.30 3.90 1 -1 36 10.20 4.10 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 66120 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 O1 O 0.7899(2) 0.61182(18) 0.39422(7) 0.0330(6) Uani 1 1 d . . O2 O 0.5283(2) 0.64816(19) 0.46846(6) 0.0311(5) Uani 1 1 d . . O3 O 0.64824(17) 1.00179(17) 0.57609(7) 0.0260(5) Uani 1 1 d . . H3 H 0.7201 1.0388 0.5700 0.039 Uiso 1 1 calc R U N1 N 0.6127(2) 0.7492(2) 0.38691(7) 0.0210(6) Uani 1 1 d . . N2 N 0.4668(2) 0.7372(2) 0.32693(8) 0.0251(6) Uani 1 1 d . . N3 N 0.6122(2) 0.6229(2) 0.56458(7) 0.0193(6) Uani 1 1 d . . H3N H 0.5799 0.5574 0.5420 0.023 Uiso 1 1 d R U C1 C 0.6954(3) 0.6467(3) 0.37203(9) 0.0218(7) Uani 1 1 d . . C2 C 0.6610(3) 0.5916(3) 0.32926(9) 0.0192(7) Uani 1 1 d . . C3 C 0.7379(3) 0.4902(3) 0.30933(10) 0.0327(9) Uani 1 1 d . . H3A H 0.8139 0.4571 0.3237 0.039 Uiso 1 1 calc R U C4 C 0.7043(4) 0.4383(3) 0.26927(11) 0.0390(10) Uani 1 1 d . . H4 H 0.7567 0.3689 0.2560 0.047 Uiso 1 1 calc R U C5 C 0.5939(4) 0.4868(3) 0.24801(10) 0.0391(9) Uani 1 1 d . . H5 H 0.5714 0.4512 0.2200 0.047 Uiso 1 1 calc R U C6 C 0.5173(3) 0.5857(3) 0.26716(10) 0.0309(8) Uani 1 1 d . . H6 H 0.4416 0.6179 0.2524 0.037 Uiso 1 1 calc R U C7 C 0.5494(3) 0.6399(3) 0.30831(9) 0.0214(7) Uani 1 1 d . . C8 C 0.5035(3) 0.7863(3) 0.36417(9) 0.0238(7) Uani 1 1 d . . H8 H 0.4495 0.8549 0.3771 0.029 Uiso 1 1 calc R U C9 C 0.6443(3) 0.8195(3) 0.42776(8) 0.0274(8) Uani 1 1 d . . H9A H 0.5990 0.9100 0.4282 0.033 Uiso 1 1 calc R U H9B H 0.7392 0.8380 0.4284 0.033 Uiso 1 1 calc R U C10 C 0.6078(3) 0.7407(3) 0.46837(9) 0.0209(7) Uani 1 1 d . . C11 C 0.6749(3) 0.7927(3) 0.50871(9) 0.0228(8) Uani 1 1 d . . H11A H 0.6901 0.8932 0.5051 0.027 Uiso 1 1 calc R U H11B H 0.7614 0.7476 0.5104 0.027 Uiso 1 1 calc R U C12 C 0.6061(3) 0.7707(3) 0.55209(9) 0.0196(7) Uani 1 1 d . . H12 H 0.5127 0.7984 0.5489 0.024 Uiso 1 1 calc R U C13 C 0.6687(3) 0.8588(3) 0.58748(9) 0.0204(7) Uani 1 1 d . . H13 H 0.7645 0.8397 0.5880 0.024 Uiso 1 1 calc R U C14 C 0.6128(3) 0.8302(3) 0.63246(9) 0.0257(8) Uani 1 1 d . . H14A H 0.5225 0.8660 0.6338 0.031 Uiso 1 1 calc R U H14B H 0.6650 0.8800 0.6547 0.031 Uiso 1 1 calc R U C15 C 0.6125(3) 0.6764(3) 0.64303(9) 0.0263(8) Uani 1 1 d . . H15A H 0.7032 0.6433 0.6464 0.032 Uiso 1 1 calc R U H15B H 0.5662 0.6606 0.6710 0.032 Uiso 1 1 calc R U C16 C 0.5460(3) 0.5967(3) 0.60690(9) 0.0254(7) Uani 1 1 d . . H16A H 0.5485 0.4965 0.6136 0.030 Uiso 1 1 calc R U H16B H 0.4536 0.6253 0.6049 0.030 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 0.0294(13) 0.0311(13) 0.0383(13) 0.0103(11) -0.0101(12) -0.0004(10) O2 0.0439(14) 0.0267(12) 0.0226(11) 0.0011(10) -0.0010(12) -0.0187(11) O3 0.0263(12) 0.0152(10) 0.0364(13) -0.0027(10) 0.0047(11) -0.0011(9) N1 0.0265(15) 0.0183(13) 0.0181(13) -0.0008(12) 0.0004(13) -0.0021(13) N2 0.0291(16) 0.0226(14) 0.0236(14) 0.0039(13) -0.0013(14) 0.0042(13) N3 0.0267(14) 0.0135(12) 0.0176(13) -0.0038(11) 0.0012(12) -0.0083(11) C1 0.0230(19) 0.0174(17) 0.0250(18) 0.0092(15) -0.0013(17) -0.0029(15) C2 0.0214(19) 0.0173(16) 0.0190(16) 0.0026(14) 0.0048(16) -0.0003(14) C3 0.034(2) 0.030(2) 0.034(2) 0.0029(18) 0.0129(18) 0.0030(17) C4 0.052(3) 0.028(2) 0.037(2) -0.0049(19) 0.027(2) -0.0005(17) C5 0.062(3) 0.034(2) 0.0217(18) -0.0049(18) 0.010(2) -0.017(2) C6 0.040(2) 0.0303(19) 0.0226(17) 0.0058(16) -0.0039(18) -0.0059(17) C7 0.0269(19) 0.0167(16) 0.0207(16) 0.0046(15) 0.0068(16) -0.0046(16) C8 0.025(2) 0.0181(17) 0.0287(18) 0.0036(15) 0.0071(17) 0.0020(14) C9 0.040(2) 0.0227(17) 0.0198(17) -0.0002(15) -0.0016(17) -0.0094(14) C10 0.0244(18) 0.0167(16) 0.0215(16) 0.0016(15) 0.0038(17) -0.0030(15) C11 0.026(2) 0.0191(17) 0.0233(17) -0.0010(15) 0.0005(16) -0.0029(14) C12 0.0212(18) 0.0181(17) 0.0195(16) 0.0013(14) 0.0003(15) -0.0042(14) C13 0.0219(18) 0.0157(16) 0.0237(16) 0.0003(15) -0.0020(15) -0.0005(14) C14 0.032(2) 0.0231(18) 0.0223(16) -0.0044(16) 0.0028(17) -0.0009(16) C15 0.032(2) 0.0246(18) 0.0218(17) 0.0031(15) 0.0033(16) -0.0090(16) C16 0.0259(18) 0.0206(17) 0.0296(18) 0.0046(15) 0.0047(17) -0.0027(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 C13 O3 H3 109.5 C8 N1 C1 121.6(2) C8 N1 C9 119.7(2) C1 N1 C9 118.7(3) C8 N2 C7 115.6(3) C12 N3 C16 111.7(2) C12 N3 H3N 115.0 C16 N3 H3N 110.1 O1 C1 N1 119.9(3) O1 C1 C2 125.9(3) N1 C1 C2 114.2(3) C7 C2 C3 119.9(3) C7 C2 C1 119.4(3) C3 C2 C1 120.7(3) C4 C3 C2 120.3(3) C4 C3 H3A 119.8 C2 C3 H3A 119.8 C3 C4 C5 120.1(3) C3 C4 H4 120.0 C5 C4 H4 120.0 C6 C5 C4 120.3(3) C6 C5 H5 119.8 C4 C5 H5 119.8 C5 C6 C7 120.6(3) C5 C6 H6 119.7 C7 C6 H6 119.7 N2 C7 C2 122.7(3) N2 C7 C6 118.5(3) C2 C7 C6 118.8(3) N2 C8 N1 126.3(3) N2 C8 H8 116.8 N1 C8 H8 116.8 N1 C9 C10 114.5(2) N1 C9 H9A 108.6 C10 C9 H9A 108.6 N1 C9 H9B 108.6 C10 C9 H9B 108.6 H9A C9 H9B 107.6 O2 C10 C11 123.7(3) O2 C10 C9 123.0(3) C11 C10 C9 113.2(2) C10 C11 C12 117.2(2) C10 C11 H11A 108.0 C12 C11 H11A 108.0 C10 C11 H11B 108.0 C12 C11 H11B 108.0 H11A C11 H11B 107.2 N3 C12 C11 109.9(2) N3 C12 C13 109.9(2) C11 C12 C13 110.3(2) N3 C12 H12 108.9 C11 C12 H12 108.9 C13 C12 H12 108.9 O3 C13 C14 109.8(2) O3 C13 C12 107.7(2) C14 C13 C12 112.5(2) O3 C13 H13 108.9 C14 C13 H13 108.9 C12 C13 H13 108.9 C13 C14 C15 111.8(2) C13 C14 H14A 109.3 C15 C14 H14A 109.3 C13 C14 H14B 109.3 C15 C14 H14B 109.3 H14A C14 H14B 107.9 C16 C15 C14 110.2(2) C16 C15 H15A 109.6 C14 C15 H15A 109.6 C16 C15 H15B 109.6 C14 C15 H15B 109.6 H15A C15 H15B 108.1 N3 C16 C15 110.1(2) N3 C16 H16A 109.6 C15 C16 H16A 109.6 N3 C16 H16B 109.6 C15 C16 H16B 109.6 H16A C16 H16B 108.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.230(3) O2 C10 1.210(3) O3 C13 1.441(3) O3 H3 0.8400 N1 C8 1.366(3) N1 C1 1.381(3) N1 C9 1.457(3) N2 C8 1.288(3) N2 C7 1.388(3) N3 C12 1.479(3) N3 C16 1.482(3) N3 H3N 0.9923 C1 C2 1.453(4) C2 C7 1.392(4) C2 C3 1.398(4) C3 C4 1.366(4) C3 H3A 0.9500 C4 C5 1.387(4) C4 H4 0.9500 C5 C6 1.368(4) C5 H5 0.9500 C6 C7 1.401(4) C6 H6 0.9500 C8 H8 0.9500 C9 C10 1.503(3) C9 H9A 0.9900 C9 H9B 0.9900 C10 C11 1.498(4) C11 C12 1.516(3) C11 H11A 0.9900 C11 H11B 0.9900 C12 C13 1.518(3) C12 H12 1.0000 C13 C14 1.514(3) C13 H13 1.0000 C14 C15 1.521(3) C14 H14A 0.9900 C14 H14B 0.9900 C15 C16 1.508(3) C15 H15A 0.9900 C15 H15B 0.9900 C16 H16A 0.9900 C16 H16B 0.9900 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 N3 0.84 1.91 2.744(3) 172.3 8_765 N3 H3N O2 0.99 2.47 3.069(3) 118.5 . N3 H3N O2 0.99 2.30 3.155(3) 144.0 5_666 C8 H8 O3 0.95 2.23 3.154(3) 164.2 5_676 C9 H9A O1 0.99 2.48 3.079(3) 118.2 8_765 C14 H14A O1 0.99 2.54 3.457(4) 153.2 4_466