#------------------------------------------------------------------------------ #$Date: 2021-08-07 03:30:23 +0300 (Sat, 07 Aug 2021) $ #$Revision: 267977 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564332.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_1564332 loop_ _publ_author_name 'Ravi, Arthi' 'Shijad, Amina' 'Sureshan, Kana M.' _publ_section_title ; Single-crystal-to-single-crystal synthesis of a pseudostarch via topochemical azide-alkyne cycloaddition polymerization ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC03727G _journal_year 2021 _chemical_formula_moiety 'C9 H13 N3 O5' _chemical_formula_sum 'C9 H13 N3 O5' _chemical_formula_weight 243.22 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-10-16 deposited with the CCDC. 2021-08-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.159(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.792(2) _cell_length_b 17.062(5) _cell_length_c 9.698(3) _cell_measurement_reflns_used 1701 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.62 _cell_measurement_theta_min 2.41 _cell_volume 1061.6(6) _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)' _computing_publication_material 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2013/5 (Sheldrick, 2013)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker KAPPA APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_unetI/netI 0.0539 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 14418 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.993 _diffrn_reflns_theta_max 24.993 _diffrn_reflns_theta_min 2.523 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_meas 1.521 _exptl_crystal_density_method NONE _exptl_crystal_description plate _exptl_crystal_F_000 512 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.486 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 158 _refine_ls_number_reflns 1868 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0496 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.4424P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1169 _refine_ls_wR_factor_ref 0.1365 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1238 _reflns_number_total 1868 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc03727g2.cif _cod_data_source_block POLYMER2 _cod_original_cell_volume 1061.5(6) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1564332 _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 0.969 _shelx_estimated_absorpt_t_max 0.994 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL KMSIV95_a.res in P2(1)/c CELL 0.71073 6.7915 17.0618 9.6982 90.000 109.159 90.000 ZERR 4.00 0.0024 0.0054 0.0032 0.000 0.008 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 36 52 12 20 MERG 2 OMIT -3.00 50.00 OMIT 0 0 2 EQIV $1 x, -y+3/2, z-1/2 HTAB C3 N2_$1 EQIV $2 -x+1, -y+1, -z HTAB C1 N3_$2 EQIV $3 x-1, -y+3/2, z-1/2 HTAB C9 O3_$3 HTAB C7 O3 EQIV $4 x+1, -y+3/2, z+1/2 HTAB O4 O6_$4 EQIV $5 x+1, y, z HTAB O3 O1_$5 HTAB O1 N3 EQIV $6 x-1, y, z HTAB O6 O4_$6 FMAP 2 PLAN 20 SIZE 0.050 0.120 0.250 ACTA HTAB 2.00000 BOND $H CONF L.S. 10 TEMP 20.00 WGHT 0.063600 0.442400 FVAR 0.75790 C4 1 0.764395 0.731377 0.166667 11.00000 0.02106 0.02736 = 0.02785 -0.00275 0.01010 -0.00602 AFIX 13 H4 2 0.775024 0.734326 0.269781 11.00000 -1.20000 AFIX 0 C3 1 0.797707 0.645831 0.128596 11.00000 0.01975 0.02924 = 0.02797 -0.00093 0.00801 0.00353 AFIX 13 H3 2 0.792669 0.643118 0.026557 11.00000 -1.20000 AFIX 0 C2 1 0.626632 0.592676 0.149508 11.00000 0.02639 0.01825 = 0.02835 -0.00319 0.01046 0.00306 AFIX 13 H2 2 0.651203 0.538411 0.126299 11.00000 -1.20000 AFIX 0 C1 1 0.409856 0.619667 0.048261 11.00000 0.02408 0.02383 = 0.02801 -0.00270 0.00991 -0.00260 AFIX 13 H1 2 0.410609 0.617282 -0.052527 11.00000 -1.20000 AFIX 0 C6 1 0.365709 0.705138 0.080249 11.00000 0.02126 0.02585 = 0.02541 0.00133 0.00408 0.00408 AFIX 13 H6 2 0.354660 0.708322 0.178339 11.00000 -1.20000 AFIX 0 C5 1 0.544921 0.759815 0.071481 11.00000 0.02956 0.01833 = 0.02691 -0.00074 0.01053 0.00192 AFIX 13 H5 2 0.541470 0.761008 -0.030315 11.00000 -1.20000 AFIX 0 C9 1 0.354661 0.893006 0.039959 11.00000 0.03140 0.02761 = 0.03005 0.00003 0.00352 0.00285 AFIX 43 H9 2 0.251190 0.884989 -0.049486 11.00000 -1.20000 AFIX 0 C7 1 0.737558 0.535585 0.394883 11.00000 0.03273 0.02675 = 0.03386 0.00458 0.00544 -0.00104 AFIX 23 H7B 2 0.771507 0.552908 0.495263 11.00000 -1.20000 H7A 2 0.867315 0.526072 0.376165 11.00000 -1.20000 AFIX 0 C8 1 0.613340 0.459151 0.374419 11.00000 0.02915 0.02531 = 0.03198 -0.00161 0.01044 0.00015 N1 3 0.506422 0.841694 0.113736 11.00000 0.03084 0.01809 = 0.02454 -0.00238 0.00713 -0.00092 N2 3 0.631115 0.873221 0.240652 11.00000 0.03753 0.02881 = 0.03255 -0.00569 0.00467 0.00354 N3 3 0.441951 0.445524 0.252315 11.00000 0.03586 0.02640 = 0.03707 0.00308 0.00787 -0.00598 O4 4 0.924052 0.780985 0.142454 11.00000 0.02874 0.03655 = 0.05347 -0.00326 0.01714 -0.00742 AFIX 147 H4A 2 1.003948 0.796112 0.221212 11.00000 -1.50000 AFIX 0 O3 4 1.000548 0.620212 0.221812 11.00000 0.02164 0.04231 = 0.03932 -0.00111 0.00854 0.00702 AFIX 147 H3A 2 1.073115 0.609191 0.171641 11.00000 -1.50000 AFIX 0 O2 4 0.622810 0.596805 0.298389 11.00000 0.03409 0.02297 = 0.03032 0.00338 0.01239 0.00280 O1 4 0.243592 0.569578 0.058716 11.00000 0.02406 0.02698 = 0.04450 0.00171 0.00897 -0.00251 AFIX 147 H1A 2 0.292610 0.534461 0.117740 11.00000 -1.50000 AFIX 0 O6 4 0.170585 0.729206 -0.025666 11.00000 0.02390 0.03260 = 0.04106 0.00021 0.00519 0.00680 AFIX 147 H6A 2 0.093789 0.746796 0.016773 11.00000 -1.50000 AFIX 0 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM KMSIV95_a.res in P2(1)/c REM R1 = 0.0496 for 1238 Fo > 4sig(Fo) and 0.0885 for all 1868 data REM 158 parameters refined using 0 restraints END WGHT 0.0636 0.4386 REM Instructions for potential hydrogen bonds HTAB C3 N2_$1 HTAB C1 N3_$2 HTAB C9 O3_$3 HTAB C7 O3 HTAB O4 O6_$4 HTAB O3 O1_$5 HTAB O1 N3 HTAB O6 O4_$6 REM Highest difference peak 0.486, deepest hole -0.305, 1-sigma level 0.082 Q1 1 1.0228 0.9228 0.2641 11.00000 0.05 0.49 Q2 1 0.1987 0.7337 -0.1249 11.00000 0.05 0.26 Q3 1 0.9540 0.7579 0.0539 11.00000 0.05 0.24 Q4 1 0.9308 0.8572 0.3035 11.00000 0.05 0.23 Q5 1 0.9302 0.5318 0.6568 11.00000 0.05 0.23 Q6 1 0.8894 0.5126 0.3029 11.00000 0.05 0.23 Q7 1 1.0777 0.4896 0.2521 11.00000 0.05 0.22 Q8 1 0.9119 0.8232 0.0518 11.00000 0.05 0.22 Q9 1 0.1997 0.8415 -0.0601 11.00000 0.05 0.22 Q10 1 0.1339 0.5648 -0.0619 11.00000 0.05 0.22 Q11 1 0.0746 0.7886 -0.0362 11.00000 0.05 0.22 Q12 1 0.9257 0.9152 0.3411 11.00000 0.05 0.21 Q13 1 0.9566 0.4444 0.4534 11.00000 0.05 0.21 Q14 1 0.9381 0.5445 0.4341 11.00000 0.05 0.21 Q15 1 0.9356 0.6160 0.5012 11.00000 0.05 0.21 Q16 1 0.0677 0.6940 -0.0841 11.00000 0.05 0.21 Q17 1 0.8970 0.8222 0.1990 11.00000 0.05 0.20 Q18 1 1.0592 0.7264 0.1556 11.00000 0.05 0.20 Q19 1 0.0707 0.5732 -0.1271 11.00000 0.05 0.20 Q20 1 0.9483 0.6133 0.0508 11.00000 0.05 0.20 ; _shelx_res_checksum 53208 _shelx_hkl_file ; 1 0 0 4176.18 100.99 -1 0 0 3751.42 102.79 -1 0 0 3793.92 103.19 2 0 0 -6.20 5.50 -2 0 0 -0.80 4.20 2 0 0 9.10 8.40 2 0 0 4.50 3.00 2 0 0 1.50 4.80 -2 0 0 11.60 5.70 2 0 0 3.70 5.90 -2 0 0 5.50 7.90 -2 0 0 2.80 6.00 -2 0 0 2.10 4.00 3 0 0 262.17 14.00 -3 0 0 265.97 16.30 3 0 0 279.17 18.20 -3 0 0 343.47 20.20 3 0 0 327.57 22.80 -3 0 0 364.96 29.60 3 0 0 243.68 19.60 -3 0 0 282.27 22.20 -3 0 0 297.57 17.10 4 0 0 21.20 13.60 4 0 0 25.30 7.10 -4 0 0 27.40 11.40 4 0 0 49.60 13.20 -4 0 0 35.10 13.70 -4 0 0 16.20 13.30 5 0 0 890.31 48.60 5 0 0 915.51 46.70 5 0 0 906.01 31.90 -5 0 0 950.80 50.39 -5 0 0 948.61 60.39 6 0 0 25.70 23.10 -6 0 0 31.70 21.90 6 0 0 33.30 21.60 -6 0 0 29.60 20.90 -7 0 0 246.58 49.20 -7 0 0 223.58 37.00 7 0 0 257.67 38.60 7 0 0 157.98 34.10 8 0 0 185.88 40.40 -8 0 0 159.38 42.10 -8 0 0 170.08 40.20 0 -1 0 0.30 1.10 0 -1 0 0.20 0.60 0 -1 0 0.30 1.10 0 -1 0 0.80 1.30 0 1 0 -0.30 1.10 0 1 0 0.00 1.60 0 1 0 1.30 1.00 0 1 0 0.40 0.60 1 -1 0 284.47 14.90 1 -1 0 282.67 11.20 1 -1 0 284.77 11.60 -1 -1 0 212.98 10.20 -1 -1 0 301.67 14.90 1 -1 0 201.68 11.00 -1 -1 0 287.77 10.70 1 -1 0 299.77 9.80 -1 -1 0 290.57 11.10 -1 1 0 217.68 10.20 -1 1 0 238.58 10.90 1 1 0 215.48 9.80 -1 1 0 287.57 12.30 -1 1 0 228.38 13.60 1 1 0 243.58 13.60 1 1 0 278.27 10.20 1 1 0 282.57 11.30 -2 -1 0 8.60 7.30 -2 -1 0 6.30 5.60 -2 -1 0 12.20 4.70 2 -1 0 12.60 6.40 -2 -1 0 5.50 6.20 2 -1 0 -2.30 8.00 2 -1 0 0.10 3.80 2 -1 0 8.30 5.10 2 -1 0 7.40 6.00 -2 -1 0 11.10 4.60 -2 1 0 10.20 5.00 -2 1 0 5.60 2.90 -2 1 0 16.70 6.60 -2 1 0 10.80 8.90 2 1 0 15.10 6.30 2 1 0 8.70 4.90 -2 1 0 12.60 4.70 2 1 0 9.20 4.70 2 1 0 8.00 7.70 -2 1 0 13.50 6.70 2 1 0 9.40 6.20 -3 -1 0 127.69 22.10 3 -1 0 128.89 15.80 3 -1 0 126.19 13.50 3 -1 0 117.89 10.40 -3 -1 0 106.59 11.70 -3 -1 0 122.19 12.30 3 -1 0 154.38 16.50 -3 -1 0 123.19 14.20 -3 -1 0 126.99 15.50 3 1 0 129.99 12.70 3 1 0 85.99 13.70 -3 1 0 134.39 13.00 3 1 0 115.39 12.00 -3 1 0 151.28 14.10 3 1 0 115.39 8.90 -3 1 0 141.19 15.40 -3 1 0 163.48 24.20 -3 1 0 96.39 14.60 3 1 0 135.09 15.30 4 -1 0 7.80 12.10 -4 -1 0 -21.70 10.70 4 -1 0 11.50 13.60 4 -1 0 6.40 7.40 -4 -1 0 -15.60 9.90 -4 -1 0 4.40 10.30 -4 1 0 4.60 10.30 4 1 0 -3.80 13.00 4 1 0 -11.80 10.80 -4 1 0 30.80 16.10 4 1 0 2.60 5.80 -4 1 0 6.10 12.00 5 -1 0 312.47 30.00 -5 -1 0 347.37 42.20 5 -1 0 341.27 21.00 5 -1 0 371.76 32.90 -5 -1 0 354.96 32.20 -5 1 0 398.66 40.90 5 1 0 298.17 30.40 5 1 0 373.66 32.00 -5 1 0 315.47 31.60 5 1 0 326.37 17.40 6 -1 0 -12.10 19.60 -6 -1 0 13.50 22.40 -6 -1 0 20.40 21.40 6 -1 0 -3.50 21.90 -6 1 0 8.30 21.10 6 1 0 -1.90 21.60 -6 1 0 -10.00 20.60 6 1 0 9.10 22.40 7 -1 0 -1.20 27.50 -7 -1 0 22.60 26.10 7 -1 0 -6.20 28.60 -7 -1 0 15.70 25.90 7 1 0 10.10 28.00 -7 1 0 2.00 23.80 7 1 0 0.00 28.40 -7 1 0 -3.20 25.30 8 -1 0 49.99 35.90 -8 -1 0 113.59 37.50 -8 -1 0 76.09 36.40 -8 1 0 96.19 34.80 8 1 0 41.20 36.50 -8 1 0 93.49 35.30 -1 -2 0 1075.69 37.40 1 -2 0 1107.99 33.10 -1 -2 0 1061.29 33.30 1 -2 0 1213.78 35.80 1 -2 0 1189.18 34.00 1 -2 0 1120.09 38.20 1 -2 0 1133.99 34.40 -1 -2 0 1158.98 33.80 -1 -2 0 1067.79 31.30 1 2 0 1130.89 33.50 -1 2 0 1147.09 35.60 -1 2 0 1085.19 32.80 1 2 0 1149.19 33.70 1 2 0 1131.39 37.70 1 2 0 1159.68 31.60 -1 2 0 1137.89 33.50 -1 2 0 1161.68 38.40 -1 2 0 1185.68 34.40 1 2 0 1144.19 32.10 2 -2 0 225.48 19.30 -2 -2 0 234.78 13.50 2 -2 0 240.38 15.00 -2 -2 0 239.98 19.40 2 -2 0 256.57 15.30 2 -2 0 245.58 12.60 -2 -2 0 231.38 11.80 -2 -2 0 238.68 15.20 -2 -2 0 267.57 13.90 2 -2 0 242.08 14.30 -2 2 0 248.28 16.30 2 2 0 233.78 12.80 -2 2 0 276.47 14.70 2 2 0 231.18 13.40 2 2 0 251.57 15.00 -2 2 0 245.78 11.20 -2 2 0 228.68 19.20 -2 2 0 255.17 13.60 2 2 0 259.37 18.60 -3 -2 0 948.51 35.30 -3 -2 0 922.01 35.30 3 -2 0 916.11 37.00 -3 -2 0 914.01 38.10 3 -2 0 935.11 37.50 -3 -2 0 975.30 48.70 -3 -2 0 959.80 33.10 3 -2 0 896.21 32.20 3 -2 0 938.41 38.10 -3 2 0 1006.80 35.70 -3 2 0 1030.70 42.30 -3 2 0 923.41 30.20 -3 2 0 998.20 50.59 -3 2 0 980.60 37.40 3 2 0 937.01 36.10 -3 2 0 910.81 39.30 3 2 0 887.11 37.80 3 2 0 952.90 33.80 4 -2 0 11.20 12.30 -4 -2 0 1.90 12.30 -4 -2 0 4.40 12.30 -4 -2 0 10.20 10.30 4 -2 0 3.50 8.20 4 -2 0 -10.10 12.20 -4 2 0 0.70 13.40 -4 2 0 2.40 11.90 4 2 0 8.60 6.10 4 2 0 12.20 12.20 4 2 0 0.00 12.20 4 2 0 -0.80 6.20 5 -2 0 35.00 11.90 5 -2 0 -28.60 17.90 5 -2 0 16.10 21.10 -5 -2 0 31.20 21.40 -5 -2 0 15.70 18.60 5 2 0 25.00 21.60 -5 2 0 17.30 19.10 -5 2 0 22.70 19.60 5 2 0 26.80 8.10 5 2 0 -10.30 16.40 6 -2 0 50.79 23.70 -6 -2 0 85.89 23.70 -6 -2 0 80.89 32.20 6 -2 0 52.09 24.00 -6 2 0 64.39 26.10 -6 2 0 39.70 23.30 6 2 0 38.60 22.60 6 2 0 37.90 23.30 7 -2 0 28.50 30.40 -7 -2 0 110.79 37.90 -7 -2 0 60.89 28.80 7 -2 0 59.59 30.30 -7 2 0 31.60 28.60 -7 2 0 45.10 26.40 7 2 0 50.29 31.10 7 2 0 63.29 30.00 -8 -2 0 55.19 33.20 8 -2 0 62.09 35.70 -8 -2 0 50.49 35.90 8 2 0 91.59 35.70 -8 2 0 -3.60 30.90 -8 2 0 54.49 30.20 0 -3 0 10.80 3.10 0 -3 0 7.90 2.90 0 -3 0 9.50 3.60 0 -3 0 6.90 4.30 0 3 0 10.90 3.00 0 3 0 -0.30 3.50 0 3 0 6.70 3.30 0 3 0 3.80 2.90 1 -3 0 72.29 7.20 -1 -3 0 81.99 7.70 1 -3 0 71.49 11.20 -1 -3 0 75.69 10.20 1 -3 0 56.99 7.60 1 -3 0 72.59 8.80 -1 -3 0 84.29 6.80 1 -3 0 58.69 6.90 1 3 0 78.29 7.90 -1 3 0 83.99 7.30 1 3 0 77.69 7.10 1 3 0 87.59 10.70 -1 3 0 70.09 7.90 -1 3 0 86.59 11.00 1 3 0 77.39 5.60 -1 3 0 85.89 7.10 1 3 0 84.59 8.30 -1 3 0 90.79 9.50 2 -3 0 425.76 26.00 2 -3 0 419.56 20.30 2 -3 0 424.06 21.10 -2 -3 0 435.86 25.60 -2 -3 0 419.26 18.30 2 -3 0 397.16 19.80 -2 -3 0 400.06 18.90 -2 -3 0 394.86 15.60 2 -3 0 359.96 17.70 -2 3 0 414.76 21.40 2 3 0 419.26 20.10 2 3 0 416.16 24.10 2 3 0 428.96 17.40 2 3 0 401.06 17.90 -2 3 0 416.76 19.70 2 3 0 415.56 16.00 -2 3 0 449.76 18.70 -2 3 0 392.76 16.50 -2 3 0 417.46 25.30 3 -3 0 119.89 15.50 -3 -3 0 152.48 11.10 3 -3 0 136.59 13.20 -3 -3 0 181.78 16.80 -3 -3 0 148.69 16.00 -3 -3 0 159.08 14.80 3 -3 0 160.98 17.00 -3 -3 0 178.98 24.20 -3 3 0 150.08 14.60 -3 3 0 142.79 26.00 -3 3 0 140.09 10.20 3 3 0 164.58 17.50 3 3 0 143.29 13.00 3 3 0 176.28 15.90 3 3 0 138.29 11.60 -3 3 0 161.08 17.70 4 -3 0 84.59 12.20 -4 -3 0 83.89 16.50 -4 -3 0 72.29 20.20 -4 -3 0 76.49 12.50 4 -3 0 69.79 15.20 -4 -3 0 64.79 13.50 4 -3 0 72.19 16.90 -4 3 0 67.09 8.60 4 3 0 89.49 12.20 4 3 0 66.39 14.90 4 3 0 84.89 9.10 4 3 0 71.09 16.60 -4 3 0 56.99 19.30 4 3 0 105.39 9.50 -4 3 0 60.49 16.20 5 -3 0 656.83 41.30 -5 -3 0 629.14 43.10 5 -3 0 678.83 45.00 -5 -3 0 643.84 49.60 5 -3 0 689.53 32.30 -5 3 0 691.53 45.60 5 3 0 659.63 24.20 5 3 0 657.13 44.10 5 3 0 679.23 24.50 5 3 0 688.63 39.70 -5 3 0 717.93 51.89 6 -3 0 0.00 21.70 6 -3 0 39.20 22.70 -6 -3 0 16.90 25.30 -6 -3 0 13.20 20.80 -6 3 0 7.30 20.80 6 3 0 64.19 24.10 -6 3 0 36.70 23.20 6 3 0 16.20 21.50 7 -3 0 46.80 30.10 -7 -3 0 7.20 26.80 -7 -3 0 35.40 28.40 7 -3 0 -5.70 28.20 -7 3 0 22.40 26.70 7 3 0 38.50 30.90 7 3 0 65.39 30.30 -7 3 0 14.40 20.20 -8 -3 0 25.70 35.10 8 -3 0 20.00 35.10 -8 -3 0 50.89 33.30 -8 3 0 32.40 26.00 -8 3 0 24.50 32.00 0 -4 0 846.82 29.10 0 -4 0 830.12 27.70 0 -4 0 816.72 27.10 0 -4 0 804.92 26.80 0 4 0 838.52 27.70 0 4 0 825.62 28.50 0 4 0 805.72 27.10 0 4 0 827.72 26.80 1 -4 0 893.61 34.70 1 -4 0 902.81 32.40 -1 -4 0 898.01 29.30 1 -4 0 861.51 30.40 1 -4 0 878.01 30.40 1 -4 0 924.21 30.20 -1 -4 0 922.41 34.10 -1 -4 0 926.11 30.00 1 4 0 922.11 29.60 -1 4 0 915.91 30.50 -1 4 0 945.71 29.90 1 4 0 915.01 30.40 -1 4 0 934.91 33.10 -1 4 0 935.31 30.30 1 4 0 939.61 30.90 -1 4 0 918.51 30.70 1 4 0 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37.10 22.40 -7 -4 4 72.09 40.30 7 -4 -4 97.19 25.70 7 -4 -4 29.30 18.90 7 4 -4 67.59 21.90 -7 4 4 63.99 29.00 -7 4 4 46.90 28.20 7 4 -4 26.50 23.70 7 4 -4 1.70 21.80 -6 -4 4 111.39 40.90 6 -4 -4 140.99 23.40 -6 -4 4 139.59 19.10 6 -4 -4 97.29 22.40 6 -4 -4 105.39 21.80 6 4 -4 107.29 23.90 6 4 -4 136.89 21.80 6 4 -4 127.69 24.10 -6 4 4 135.69 26.70 -6 4 4 125.49 31.40 5 -4 -4 -3.90 11.40 -5 -4 4 -3.70 10.90 -5 -4 4 11.40 29.60 5 -4 -4 -6.00 15.80 5 -4 -4 -4.40 12.10 5 4 -4 -6.50 12.70 5 4 -4 -12.10 15.90 -5 4 4 22.10 20.60 -4 -4 4 319.17 39.20 4 -4 -4 301.67 22.10 4 -4 -4 267.37 23.20 4 -4 -4 326.67 26.50 4 4 -4 330.27 25.20 4 4 -4 305.97 22.50 -4 4 4 272.97 26.80 3 -4 -4 1959.20 64.19 3 -4 -4 1912.31 64.59 3 -4 -4 1980.80 62.69 3 -4 -4 1924.71 65.29 -3 -4 4 2014.10 75.29 3 4 -4 2007.00 70.99 3 4 -4 1993.00 63.09 -3 4 4 1920.21 60.59 3 4 -4 1913.01 63.99 -3 4 4 1916.71 65.99 2 -4 -4 4.40 5.80 2 -4 -4 9.20 6.50 2 -4 -4 2.60 4.60 2 -4 -4 -7.60 5.40 -2 4 4 8.40 10.20 2 4 -4 1.20 6.00 2 4 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16.20 2 9 -10 8.40 9.30 1 -9 -10 0.00 19.90 1 -9 -10 -9.40 10.40 -1 9 10 -2.30 24.40 1 9 -10 5.60 7.10 0 -9 -10 -9.90 19.50 0 -9 -10 11.90 12.30 0 9 -10 22.50 17.70 0 9 10 7.10 25.10 -1 -9 -10 -6.40 20.70 1 9 10 -7.70 24.60 -1 9 -10 -19.70 14.80 6 -10 -10 4.50 21.00 6 -10 -10 16.70 31.60 6 10 -10 15.20 24.70 5 -10 -10 14.70 12.90 5 -10 -10 5.20 18.70 5 -10 -10 2.50 19.00 5 10 -10 12.80 13.70 5 10 -10 15.70 22.10 4 -10 -10 39.30 18.10 4 -10 -10 -2.90 9.30 4 -10 -10 10.80 15.70 4 10 -10 0.40 18.60 4 10 -10 -6.10 11.70 3 -10 -10 22.40 11.50 3 -10 -10 33.50 16.20 3 -10 -10 9.40 16.40 3 10 -10 34.90 18.90 -3 10 10 -2.00 28.10 3 10 -10 29.90 12.50 2 -10 -10 -2.50 12.10 2 10 -10 22.90 10.40 -2 10 10 6.80 28.30 2 10 -10 -2.70 13.80 1 -10 -10 14.80 22.50 1 -10 -10 6.10 13.00 1 10 -10 8.70 8.50 -1 10 10 42.10 26.70 0 -10 -10 6.40 22.90 0 -10 -10 -3.70 13.10 0 10 10 0.40 26.70 -1 -10 -10 24.90 26.90 1 10 10 15.30 24.70 -1 10 -10 3.60 18.00 5 -11 -10 17.60 19.60 5 -11 -10 -23.90 17.30 5 -11 -10 21.10 14.40 5 11 -10 24.20 15.30 5 11 -10 13.80 19.90 4 -11 -10 -12.90 15.70 4 -11 -10 -3.20 11.00 4 -11 -10 14.60 18.10 4 11 -10 22.60 20.30 4 11 -10 9.30 13.20 3 -11 -10 49.99 19.60 3 -11 -10 49.99 14.40 3 11 -10 44.10 13.30 -3 11 10 71.89 33.50 3 11 -10 20.90 18.00 2 -11 -10 17.40 15.50 2 11 -10 -3.10 9.70 -2 11 10 -18.00 27.00 2 11 -10 22.40 17.80 1 -11 -10 17.30 25.50 1 -11 -10 13.40 14.30 -1 11 10 14.80 29.00 1 11 -10 0.80 9.40 0 -11 -10 13.20 26.80 0 -11 -10 4.50 13.30 0 11 -10 -4.50 15.70 0 11 10 5.90 28.50 5 -12 -10 -30.10 21.10 5 -12 -10 -1.80 18.90 5 12 -10 -28.10 22.90 5 12 -10 8.00 14.80 4 -12 -10 5.10 12.60 4 -12 -10 16.70 17.40 4 12 -10 15.80 14.20 4 12 -10 7.30 20.40 3 -12 -10 -14.40 13.00 3 -12 -10 4.70 11.60 -3 12 10 -0.70 30.30 3 12 -10 26.10 21.10 3 12 -10 8.30 12.20 2 -12 -10 -2.40 14.00 -2 12 10 15.90 30.20 2 12 -10 -9.70 14.70 2 12 -10 6.10 11.30 1 -12 -10 11.60 14.30 1 -12 -10 19.10 26.10 -1 12 10 26.10 31.00 1 12 -10 16.30 11.50 0 -12 -10 10.30 26.50 0 12 10 11.90 26.80 0 12 -10 9.00 12.00 4 -13 -10 -10.60 12.50 4 -13 -10 -5.40 18.10 4 13 -10 -4.80 20.10 4 13 -10 6.20 14.80 3 -13 -10 24.00 17.30 3 -13 -10 16.20 13.10 3 13 -10 39.40 14.80 -3 13 10 42.30 32.80 3 13 -10 19.00 19.30 2 -13 -10 -3.50 15.90 2 13 -10 23.20 20.60 -2 13 10 63.39 33.40 2 13 -10 -4.80 11.60 1 -13 -10 37.90 30.20 1 -13 -10 13.70 16.60 1 13 -10 -12.00 11.20 -1 13 10 5.90 30.20 3 14 -10 24.00 31.30 -2 14 10 57.19 34.30 2 14 -10 48.00 30.90 6 0 -11 -8.00 18.00 6 0 -11 16.40 21.80 6 0 -11 28.90 14.00 5 0 -11 13.50 9.90 5 0 -11 27.30 17.30 5 0 -11 -1.00 13.60 4 0 -11 6.70 7.70 4 0 -11 12.90 13.80 4 0 -11 -6.40 13.50 3 0 -11 5.30 13.00 3 0 -11 10.90 13.20 2 0 -11 0.50 11.80 2 0 -11 0.80 10.80 2 0 -11 5.90 12.70 1 0 -11 23.10 19.10 1 0 -11 -6.50 10.30 1 0 -11 -0.70 11.50 1 0 -11 -10.70 11.90 0 0 -11 0.00 11.60 0 0 -11 -11.00 12.80 0 0 -11 11.40 17.70 0 0 -11 6.00 12.40 -1 0 -11 12.20 15.70 -1 0 -11 6.20 17.70 -1 0 -11 -15.30 12.00 6 -1 -11 25.80 13.90 6 -1 -11 6.50 19.00 6 -1 -11 9.50 18.90 6 1 -11 9.50 19.90 6 1 -11 2.80 11.70 6 1 -11 -7.00 17.70 5 -1 -11 65.19 21.80 5 -1 -11 26.90 11.40 5 -1 -11 17.70 17.40 5 1 -11 13.90 10.50 5 1 -11 11.60 15.30 5 1 -11 23.20 18.00 4 -1 -11 23.20 15.80 4 -1 -11 9.80 7.50 4 -1 -11 0.80 14.40 4 1 -11 21.10 8.80 4 1 -11 28.70 16.50 4 1 -11 12.10 15.30 3 -1 -11 20.00 15.10 3 -1 -11 0.90 11.40 3 1 -11 9.60 12.80 3 1 -11 -10.70 12.20 2 -1 -11 35.60 15.50 2 -1 -11 26.60 14.30 2 -1 -11 21.30 13.40 2 1 -11 47.70 16.70 2 1 -11 40.50 16.00 2 1 -11 9.40 16.00 2 1 -11 23.00 14.20 1 -1 -11 118.39 20.30 1 -1 -11 91.79 19.40 1 -1 -11 91.19 20.40 1 1 -11 80.59 18.70 1 1 -11 102.09 20.40 1 1 -11 119.29 21.40 0 -1 -11 11.20 13.50 0 -1 -11 1.10 13.10 0 -1 -11 0.90 15.50 0 -1 -11 5.70 11.40 0 1 -11 0.60 14.10 0 1 -11 7.10 14.10 0 1 -11 12.20 12.20 0 1 -11 29.50 13.90 -1 -1 -11 5.10 15.80 -1 -1 -11 21.40 21.00 -1 1 -11 33.40 17.10 -1 1 -11 14.20 17.50 -1 1 -11 27.60 20.30 6 -2 -11 21.00 13.80 6 -2 -11 4.30 17.20 6 -2 -11 -1.40 18.40 6 2 -11 33.50 14.10 6 2 -11 31.80 20.00 6 2 -11 37.30 24.00 5 -2 -11 71.39 14.30 5 -2 -11 31.80 19.60 5 -2 -11 42.30 18.40 5 2 -11 57.59 14.00 5 2 -11 70.29 21.20 5 2 -11 44.10 18.80 4 -2 -11 6.30 13.50 4 -2 -11 3.00 14.00 4 -2 -11 22.20 8.90 4 2 -11 10.30 14.40 4 2 -11 21.20 16.10 4 2 -11 11.90 8.40 3 -2 -11 20.10 14.00 3 -2 -11 12.30 14.10 3 2 -11 15.30 14.90 3 2 -11 26.40 15.80 2 -2 -11 -4.90 11.20 2 -2 -11 2.10 12.10 2 -2 -11 16.90 13.20 2 2 -11 7.60 14.20 2 2 -11 -13.30 11.20 2 2 -11 9.70 16.20 1 -2 -11 3.00 11.80 1 -2 -11 3.50 11.30 1 -2 -11 -6.90 11.40 1 -2 -11 -10.30 15.20 1 2 -11 -4.20 11.80 1 2 -11 3.30 11.70 1 2 -11 -0.80 15.40 1 2 -11 11.70 13.10 0 -2 -11 -1.70 12.60 0 -2 -11 -2.70 16.40 0 -2 -11 6.70 11.50 0 -2 -11 -1.60 11.20 0 2 -11 11.70 14.00 0 2 -11 15.20 20.70 0 2 -11 -8.60 12.70 0 2 -11 -0.60 11.30 -1 -2 -11 15.80 17.50 -1 -2 -11 3.10 19.40 -1 2 -11 15.60 17.60 6 -3 -11 16.40 13.00 6 -3 -11 34.00 22.90 6 -3 -11 12.50 18.30 6 3 -11 -4.80 19.20 6 3 -11 32.30 14.60 6 3 -11 15.50 17.20 5 -3 -11 3.00 14.60 5 -3 -11 14.90 18.50 5 -3 -11 7.00 9.50 5 3 -11 -2.80 9.30 5 3 -11 -1.50 16.60 5 3 -11 13.90 17.80 4 -3 -11 0.20 7.60 4 -3 -11 -33.50 13.20 4 -3 -11 3.60 13.90 4 3 -11 -1.40 14.20 4 3 -11 5.20 8.60 4 3 -11 -4.40 13.90 3 -3 -11 -8.80 12.30 3 -3 -11 6.70 12.30 3 3 -11 10.00 15.10 2 -3 -11 12.90 14.30 2 -3 -11 -0.80 10.90 2 3 -11 7.50 13.00 2 3 -11 5.80 16.30 1 -3 -11 -5.60 12.30 1 -3 -11 -3.50 17.10 1 -3 -11 11.90 13.10 1 -3 -11 6.70 13.60 1 3 -11 -9.00 11.20 1 3 -11 -6.30 11.20 0 -3 -11 0.40 11.20 0 -3 -11 -4.80 13.00 0 -3 -11 -19.70 13.10 0 -3 -11 2.80 16.90 0 3 -11 21.70 14.40 0 3 -11 25.00 14.30 0 3 -11 16.30 14.60 -1 -3 -11 11.70 17.80 -1 -3 -11 16.90 16.40 -1 3 -11 10.20 15.90 6 -4 -11 -7.10 21.70 6 -4 -11 -9.60 15.70 6 -4 -11 18.70 12.70 6 4 -11 -18.60 18.70 6 4 -11 7.40 13.60 6 4 -11 2.80 19.30 5 -4 -11 19.80 16.00 5 -4 -11 -18.60 15.30 5 -4 -11 7.70 9.80 5 4 -11 0.60 10.60 5 4 -11 4.40 16.10 5 4 -11 -17.30 16.20 4 -4 -11 -7.90 13.60 4 -4 -11 -5.20 14.70 4 -4 -11 9.10 8.60 4 4 -11 -15.10 14.70 4 4 -11 4.60 8.30 3 -4 -11 33.90 17.60 3 -4 -11 10.60 13.80 3 4 -11 13.30 15.20 -3 4 11 -15.20 26.80 2 -4 -11 34.60 14.20 2 -4 -11 -7.10 11.30 -2 4 11 32.00 29.20 2 4 -11 8.70 14.20 1 -4 -11 18.50 13.60 1 -4 -11 21.00 19.80 1 -4 -11 3.00 14.00 1 -4 -11 11.60 12.80 1 4 -11 -0.70 18.70 1 4 -11 34.40 15.40 -1 4 11 51.59 31.30 0 -4 -11 10.10 13.20 0 -4 -11 -4.30 17.80 0 -4 -11 19.60 16.70 0 4 -11 38.10 17.30 0 4 11 5.50 27.00 -1 -4 -11 -10.60 15.50 -1 -4 -11 -10.80 16.20 -1 4 -11 1.60 15.90 6 -5 -11 -7.30 21.60 6 -5 -11 -4.70 18.40 6 -5 -11 -9.50 11.40 6 5 -11 -1.10 16.20 6 5 -11 -3.90 19.20 6 5 -11 -6.60 13.00 5 -5 -11 49.90 20.70 5 -5 -11 35.00 12.40 5 -5 -11 29.00 20.70 5 5 -11 38.50 20.20 5 5 -11 50.09 14.60 4 -5 -11 7.60 14.70 4 -5 -11 11.30 9.10 4 -5 -11 3.70 15.10 4 5 -11 6.10 9.70 4 5 -11 8.60 16.20 3 -5 -11 -13.00 13.20 3 -5 -11 13.60 13.30 -3 5 11 -8.80 26.20 3 5 -11 6.40 8.20 3 5 -11 20.00 17.30 2 -5 -11 0.00 12.60 2 -5 -11 0.40 11.60 2 5 -11 19.20 16.10 -2 5 11 22.50 28.30 1 -5 -11 8.60 12.80 1 -5 -11 -3.60 18.40 1 -5 -11 9.30 13.80 -1 5 11 3.20 27.80 1 5 -11 -7.90 12.40 0 -5 -11 14.30 13.80 0 -5 -11 30.10 18.50 0 -5 -11 -3.10 19.40 0 5 11 33.10 32.10 0 5 -11 61.89 19.40 -1 -5 -11 -21.80 15.70 -1 -5 -11 6.50 17.50 -1 5 -11 11.50 17.20 1 5 11 45.20 29.80 6 -6 -11 25.00 20.10 6 -6 -11 0.40 22.10 6 -6 -11 -3.80 12.20 6 6 -11 21.30 14.70 6 6 -11 -18.20 19.00 5 -6 -11 38.40 23.20 5 -6 -11 39.50 20.30 5 -6 -11 11.10 11.50 5 6 -11 3.70 12.20 5 6 -11 10.10 15.50 4 -6 -11 17.10 9.80 4 -6 -11 28.00 15.60 4 -6 -11 30.50 19.60 4 6 -11 16.80 10.90 4 6 -11 16.80 18.70 3 -6 -11 9.70 14.00 3 -6 -11 37.20 17.00 3 6 -11 73.39 11.90 -3 6 11 75.49 31.10 3 6 -11 34.60 16.80 2 -6 -11 117.69 20.30 2 -6 -11 103.39 21.50 -2 6 11 155.08 37.20 2 6 -11 140.19 24.40 1 -6 -11 11.80 20.00 1 -6 -11 0.80 12.40 -1 6 11 -5.40 26.60 1 6 -11 9.10 14.10 0 -6 -11 -4.00 18.10 0 -6 -11 -13.50 15.30 0 -6 -11 8.80 22.70 0 6 11 18.30 28.30 0 6 -11 14.90 16.90 -1 -6 -11 -14.20 17.30 -1 -6 -11 9.50 17.50 -1 6 -11 -15.30 16.30 1 6 11 8.20 27.40 6 -7 -11 -13.00 17.20 5 -7 -11 1.10 19.20 5 -7 -11 18.30 17.30 5 -7 -11 6.50 11.70 5 7 -11 -12.10 11.20 5 7 -11 -8.70 15.50 4 -7 -11 14.10 16.60 4 -7 -11 -7.60 14.60 4 -7 -11 9.00 9.30 4 7 -11 -11.60 9.80 4 7 -11 5.10 14.80 3 -7 -11 10.10 10.90 3 -7 -11 6.50 13.50 3 -7 -11 -6.50 13.20 3 7 -11 45.80 19.60 -3 7 11 16.30 29.40 3 7 -11 20.90 9.50 2 -7 -11 4.50 15.90 2 -7 -11 -13.80 12.40 2 7 -11 24.70 16.90 -2 7 11 -18.60 27.70 1 -7 -11 -4.40 12.30 1 -7 -11 -7.00 17.80 -1 7 11 13.00 31.20 1 7 -11 15.90 15.50 0 -7 -11 -6.90 21.10 0 7 11 4.70 27.10 5 -8 -11 -28.20 17.80 5 -8 -11 8.30 12.50 5 -8 -11 -2.70 16.70 5 8 -11 -3.80 18.00 5 8 -11 -17.50 11.80 4 -8 -11 9.90 16.60 4 -8 -11 -2.80 9.60 4 -8 -11 -3.30 16.10 4 8 -11 -10.30 14.30 4 8 -11 2.30 11.30 3 -8 -11 -3.20 14.20 3 -8 -11 9.50 9.80 3 -8 -11 12.30 17.00 3 8 -11 3.10 17.50 3 8 -11 23.80 11.00 -3 8 11 17.90 29.60 2 -8 -11 178.88 27.60 -2 8 11 184.88 38.70 2 8 -11 215.08 29.60 1 -8 -11 9.20 13.30 1 -8 -11 -11.50 17.80 -1 8 11 2.90 28.30 1 8 -11 -24.40 13.90 0 -8 -11 -2.50 23.00 0 8 11 34.80 30.60 5 -9 -11 -17.00 17.60 5 -9 -11 9.10 21.90 5 -9 -11 14.30 12.60 5 9 -11 3.90 20.30 5 9 -11 -13.50 12.30 4 -9 -11 5.10 11.00 4 -9 -11 -1.00 17.00 4 -9 -11 2.50 16.40 4 9 -11 5.80 12.50 4 9 -11 -7.20 15.30 3 -9 -11 37.10 19.20 3 -9 -11 24.20 11.10 3 9 -11 11.20 17.30 -3 9 11 54.29 32.90 3 9 -11 46.20 13.20 2 -9 -11 9.50 14.50 2 9 -11 -4.40 13.80 -2 9 11 66.29 32.10 1 -9 -11 13.10 22.40 1 -9 -11 -8.90 12.50 -1 9 11 -31.50 26.00 0 -9 -11 -1.50 24.30 0 9 11 5.00 27.60 4 -10 -11 21.00 13.80 4 -10 -11 4.10 19.10 4 -10 -11 -6.20 16.10 4 10 -11 -12.70 19.00 4 10 -11 18.60 13.60 3 -10 -11 23.70 11.60 3 -10 -11 19.20 17.80 3 10 -11 23.40 13.10 3 10 -11 6.20 15.70 -3 10 11 17.00 31.60 2 -10 -11 24.30 16.80 -2 10 11 -3.40 29.40 2 10 -11 6.80 15.30 1 -10 -11 7.10 26.70 1 -10 -11 0.50 14.90 -1 10 11 31.50 31.50 3 -11 -11 1.90 11.20 3 -11 -11 25.30 18.30 3 11 -11 -12.40 11.80 -3 11 11 18.60 32.80 3 11 -11 -0.90 19.10 2 -11 -11 -8.50 15.60 -2 11 11 -8.80 30.00 2 11 -11 -21.50 16.50 5 0 -12 31.20 18.60 5 0 -12 8.30 11.40 5 0 -12 5.50 18.40 4 0 -12 6.40 17.00 4 0 -12 17.30 17.30 3 0 -12 -5.70 14.30 3 0 -12 14.30 14.50 2 0 -12 36.60 16.80 2 0 -12 -2.00 12.90 2 0 -12 9.50 18.90 1 0 -12 3.30 13.90 1 0 -12 -0.40 14.90 1 0 -12 -13.20 12.20 1 0 -12 -8.60 18.50 0 0 -12 3.80 17.90 0 0 -12 4.90 15.80 5 -1 -12 6.20 16.00 5 -1 -12 11.50 11.20 5 -1 -12 7.80 18.70 5 1 -12 -13.80 15.90 5 1 -12 13.00 11.30 5 1 -12 3.60 17.20 4 -1 -12 -3.00 14.80 4 -1 -12 4.20 16.30 4 1 -12 6.00 16.70 4 1 -12 -4.70 16.10 3 -1 -12 -7.90 13.40 3 -1 -12 3.80 15.10 3 1 -12 3.00 15.50 3 1 -12 10.40 15.60 2 -1 -12 7.20 14.60 2 -1 -12 26.00 22.50 2 -1 -12 1.20 14.60 2 1 -12 3.90 21.60 2 1 -12 14.60 14.30 2 1 -12 -8.90 13.70 1 -1 -12 -11.30 11.80 1 -1 -12 5.80 14.10 1 -1 -12 -24.10 16.10 1 -1 -12 12.70 15.10 1 1 -12 0.10 14.40 1 1 -12 27.80 16.20 0 -1 -12 110.39 26.90 0 -1 -12 48.80 24.40 0 -1 -12 20.60 26.60 0 1 -12 52.69 19.50 0 1 -12 24.60 17.50 5 -2 -12 40.50 21.60 5 -2 -12 37.60 12.60 5 -2 -12 48.30 22.20 5 2 -12 39.20 13.00 5 2 -12 65.59 23.20 5 2 -12 56.49 23.20 4 -2 -12 -14.50 14.20 4 -2 -12 10.70 16.20 4 2 -12 0.20 15.30 4 2 -12 -8.10 14.30 3 -2 -12 6.90 14.50 3 -2 -12 30.50 18.80 3 2 -12 -2.00 14.00 3 2 -12 34.40 17.30 2 -2 -12 26.10 15.60 2 -2 -12 -16.40 12.90 2 -2 -12 8.00 20.50 2 2 -12 -3.30 13.20 2 2 -12 1.60 14.10 1 -2 -12 23.70 16.60 1 -2 -12 0.60 21.60 1 -2 -12 -5.20 13.60 1 -2 -12 18.90 16.00 1 2 -12 -8.30 14.10 1 2 -12 6.00 15.70 0 -2 -12 26.30 19.70 0 2 -12 21.30 17.40 0 2 -12 28.80 19.10 5 -3 -12 42.40 20.80 5 -3 -12 65.39 23.30 5 -3 -12 50.99 13.50 5 3 -12 77.59 23.90 5 3 -12 78.29 15.90 5 3 -12 45.20 21.40 4 -3 -12 -24.60 14.70 4 -3 -12 9.80 15.70 4 3 -12 0.60 16.50 4 3 -12 6.80 15.40 3 -3 -12 -1.90 16.00 3 -3 -12 -4.40 14.10 3 3 -12 3.60 15.00 3 3 -12 -5.30 14.00 2 -3 -12 17.70 15.10 2 -3 -12 1.30 14.90 2 -3 -12 -1.20 15.50 2 -3 -12 -10.00 18.20 2 3 -12 34.10 18.10 2 3 -12 -4.10 13.00 1 -3 -12 -11.70 13.80 1 -3 -12 -17.90 17.30 1 -3 -12 3.50 14.60 1 -3 -12 -0.50 14.90 1 3 -12 14.30 15.40 1 3 -12 -11.90 15.10 0 -3 -12 16.10 17.40 0 3 -12 25.70 16.60 5 -4 -12 96.09 16.60 5 -4 -12 142.19 30.40 5 -4 -12 60.49 21.70 5 4 -12 154.88 19.60 5 4 -12 113.39 26.70 5 4 -12 128.19 27.00 4 -4 -12 -7.60 17.20 4 -4 -12 -7.80 15.00 4 4 -12 -16.80 14.30 4 4 -12 17.50 17.40 3 -4 -12 -18.20 13.10 3 -4 -12 -20.70 13.40 3 4 -12 10.60 17.10 2 -4 -12 8.90 14.20 2 -4 -12 7.00 20.30 2 -4 -12 2.50 15.00 2 -4 -12 17.90 15.20 2 4 -12 21.70 16.20 1 -4 -12 -3.40 19.50 1 -4 -12 2.20 16.40 1 -4 -12 37.30 17.00 1 4 -12 26.30 17.00 5 -5 -12 20.80 28.80 5 -5 -12 18.10 18.90 5 5 -12 67.59 32.80 5 5 -12 25.60 23.90 4 -5 -12 59.89 20.50 4 -5 -12 75.39 24.30 4 5 -12 91.49 25.30 3 -5 -12 32.70 17.70 3 -5 -12 12.10 16.40 3 5 -12 5.60 15.60 2 -5 -12 -5.80 13.80 2 -5 -12 7.70 22.70 2 -5 -12 2.60 17.50 2 5 -12 -11.90 15.40 -2 5 12 28.90 33.30 1 -5 -12 59.29 19.60 1 -5 -12 42.20 19.60 1 -5 -12 17.90 25.60 1 5 -12 40.90 18.80 -1 5 12 68.59 34.30 4 -6 -12 11.20 17.90 4 -6 -12 30.30 21.70 4 6 -12 22.50 18.90 3 -6 -12 -15.30 15.00 3 -6 -12 9.20 16.10 3 6 -12 34.60 19.20 2 -6 -12 -2.50 21.50 2 -6 -12 1.60 15.60 2 6 -12 9.30 15.70 -2 6 12 -3.50 31.40 1 -6 -12 -17.60 13.50 1 -6 -12 -22.10 16.60 1 6 -12 23.70 17.10 4 -7 -12 -7.80 16.10 4 -7 -12 -15.50 16.10 4 7 -12 4.50 23.20 3 -7 -12 9.20 16.70 3 7 -12 -2.90 17.60 2 -7 -12 3.30 24.30 2 -7 -12 9.10 17.90 2 7 -12 38.80 18.70 -2 7 12 36.20 33.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 2962 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C4 C 0.7644(4) 0.73138(16) 0.1667(3) 0.0249(7) Uani 1 1 d . . . . . H4 H 0.7750 0.7343 0.2698 0.030 Uiso 1 1 calc R U . . . C3 C 0.7977(4) 0.64583(16) 0.1286(3) 0.0256(7) Uani 1 1 d . . . . . H3 H 0.7927 0.6431 0.0266 0.031 Uiso 1 1 calc R U . . . C2 C 0.6266(4) 0.59268(16) 0.1495(3) 0.0240(7) Uani 1 1 d . . . . . H2 H 0.6512 0.5384 0.1263 0.029 Uiso 1 1 calc R U . . . C1 C 0.4099(4) 0.61967(16) 0.0483(3) 0.0250(7) Uani 1 1 d . . . . . H1 H 0.4106 0.6173 -0.0525 0.030 Uiso 1 1 calc R U . . . C6 C 0.3657(4) 0.70514(16) 0.0802(3) 0.0251(7) Uani 1 1 d . . . . . H6 H 0.3547 0.7083 0.1783 0.030 Uiso 1 1 calc R U . . . C5 C 0.5449(4) 0.75981(15) 0.0715(3) 0.0246(7) Uani 1 1 d . . . . . H5 H 0.5415 0.7610 -0.0303 0.030 Uiso 1 1 calc R U . . . C9 C 0.3547(5) 0.89301(17) 0.0400(3) 0.0313(7) Uani 1 1 d . . . . . H9 H 0.2512 0.8850 -0.0495 0.038 Uiso 1 1 calc R U . . . C7 C 0.7376(5) 0.53558(17) 0.3949(3) 0.0325(8) Uani 1 1 d . . . . . H7B H 0.7715 0.5529 0.4953 0.039 Uiso 1 1 calc R U . . . H7A H 0.8673 0.5261 0.3762 0.039 Uiso 1 1 calc R U . . . C8 C 0.6133(4) 0.45915(17) 0.3744(3) 0.0287(7) Uani 1 1 d . . . . . N1 N 0.5064(4) 0.84169(13) 0.1137(2) 0.0250(6) Uani 1 1 d . . . . . N2 N 0.6311(4) 0.87322(15) 0.2407(3) 0.0346(7) Uani 1 1 d . . . . . N3 N 0.4420(4) 0.44552(15) 0.2523(3) 0.0341(7) Uani 1 1 d . . . . . O4 O 0.9241(3) 0.78099(13) 0.1425(2) 0.0387(6) Uani 1 1 d . . . . . H4A H 1.0039 0.7961 0.2212 0.058 Uiso 1 1 calc R U . . . O3 O 1.0005(3) 0.62021(13) 0.2218(2) 0.0348(6) Uani 1 1 d . . . . . H3A H 1.0731 0.6092 0.1716 0.052 Uiso 1 1 calc R U . . . O2 O 0.6228(3) 0.59680(11) 0.2984(2) 0.0287(5) Uani 1 1 d . . . . . O1 O 0.2436(3) 0.56958(12) 0.0587(2) 0.0324(5) Uani 1 1 d . . . . . H1A H 0.2926 0.5345 0.1177 0.049 Uiso 1 1 calc R U . . . O6 O 0.1706(3) 0.72921(12) -0.0257(2) 0.0339(6) Uani 1 1 d . . . . . H6A H 0.0938 0.7468 0.0168 0.051 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 C4 0.0211(15) 0.0274(17) 0.0279(15) -0.0028(12) 0.0101(13) -0.0060(13) C3 0.0197(16) 0.0292(18) 0.0280(15) -0.0009(12) 0.0080(12) 0.0035(13) C2 0.0264(16) 0.0182(16) 0.0283(15) -0.0032(12) 0.0105(13) 0.0031(12) C1 0.0241(16) 0.0238(17) 0.0280(15) -0.0027(12) 0.0099(12) -0.0026(13) C6 0.0213(16) 0.0259(17) 0.0254(15) 0.0013(12) 0.0041(12) 0.0041(13) C5 0.0296(17) 0.0183(16) 0.0269(15) -0.0007(12) 0.0105(13) 0.0019(13) C9 0.0314(18) 0.0276(18) 0.0301(16) 0.0000(13) 0.0035(14) 0.0029(14) C7 0.0327(18) 0.0267(18) 0.0339(17) 0.0046(13) 0.0054(14) -0.0010(14) C8 0.0292(18) 0.0253(18) 0.0320(16) -0.0016(13) 0.0104(13) 0.0002(14) N1 0.0308(14) 0.0181(13) 0.0245(13) -0.0024(10) 0.0071(11) -0.0009(11) N2 0.0375(15) 0.0288(16) 0.0325(14) -0.0057(11) 0.0047(12) 0.0035(12) N3 0.0359(16) 0.0264(16) 0.0371(15) 0.0031(11) 0.0079(12) -0.0060(12) O4 0.0287(13) 0.0365(14) 0.0535(14) -0.0033(11) 0.0171(11) -0.0074(10) O3 0.0216(11) 0.0423(14) 0.0393(12) -0.0011(10) 0.0085(9) 0.0070(10) O2 0.0341(12) 0.0230(12) 0.0303(11) 0.0034(8) 0.0124(9) 0.0028(9) O1 0.0241(11) 0.0270(13) 0.0445(13) 0.0017(9) 0.0090(10) -0.0025(9) O6 0.0239(12) 0.0326(13) 0.0411(12) 0.0002(9) 0.0052(10) 0.0068(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 O4 C4 C3 109.7(2) . . ? O4 C4 C5 110.1(2) . . ? C3 C4 C5 110.0(2) . . ? O4 C4 H4 109.0 . . ? C3 C4 H4 109.0 . . ? C5 C4 H4 109.0 . . ? O3 C3 C2 110.2(2) . . ? O3 C3 C4 108.8(2) . . ? C2 C3 C4 110.5(2) . . ? O3 C3 H3 109.1 . . ? C2 C3 H3 109.1 . . ? C4 C3 H3 109.1 . . ? O2 C2 C3 111.3(2) . . ? O2 C2 C1 107.0(2) . . ? C3 C2 C1 110.1(2) . . ? O2 C2 H2 109.5 . . ? C3 C2 H2 109.5 . . ? C1 C2 H2 109.5 . . ? O1 C1 C6 109.7(2) . . ? O1 C1 C2 112.4(2) . . ? C6 C1 C2 111.2(2) . . ? O1 C1 H1 107.8 . . ? C6 C1 H1 107.8 . . ? C2 C1 H1 107.8 . . ? O6 C6 C1 108.6(2) . . ? O6 C6 C5 110.0(2) . . ? C1 C6 C5 110.4(2) . . ? O6 C6 H6 109.3 . . ? C1 C6 H6 109.3 . . ? C5 C6 H6 109.3 . . ? N1 C5 C4 110.3(2) . . ? N1 C5 C6 109.4(2) . . ? C4 C5 C6 113.3(2) . . ? N1 C5 H5 107.9 . . ? C4 C5 H5 107.9 . . ? C6 C5 H5 107.9 . . ? N1 C9 C8 105.5(2) . 2_655 ? N1 C9 H9 127.2 . . ? C8 C9 H9 127.2 2_655 . ? O2 C7 C8 112.0(2) . . ? O2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? O2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? H7B C7 H7A 107.9 . . ? C9 C8 N3 107.5(2) 2_645 . ? C9 C8 C7 130.5(3) 2_645 . ? N3 C8 C7 121.9(2) . . ? N2 N1 C9 111.2(2) . . ? N2 N1 C5 120.3(2) . . ? C9 N1 C5 128.6(2) . . ? N3 N2 N1 106.3(2) 2_655 . ? N2 N3 C8 109.5(2) 2_645 . ? C4 O4 H4A 109.5 . . ? C3 O3 H3A 109.5 . . ? C7 O2 C2 115.2(2) . . ? C1 O1 H1A 109.5 . . ? C6 O6 H6A 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 C4 O4 1.454(3) . ? C4 C3 1.540(4) . ? C4 C5 1.551(4) . ? C4 H4 0.9800 . ? C3 O3 1.445(3) . ? C3 C2 1.539(4) . ? C3 H3 0.9800 . ? C2 O2 1.454(3) . ? C2 C1 1.548(4) . ? C2 H2 0.9800 . ? C1 O1 1.446(3) . ? C1 C6 1.541(4) . ? C1 H1 0.9800 . ? C6 O6 1.444(3) . ? C6 C5 1.558(4) . ? C6 H6 0.9800 . ? C5 N1 1.503(3) . ? C5 H5 0.9800 . ? C9 N1 1.363(4) . ? C9 C8 1.376(4) 2_655 ? C9 H9 0.9300 . ? C7 O2 1.448(3) . ? C7 C8 1.530(4) . ? C7 H7B 0.9700 . ? C7 H7A 0.9700 . ? C8 C9 1.375(4) 2_645 ? C8 N3 1.381(4) . ? N1 N2 1.355(3) . ? N2 N3 1.340(3) 2_655 ? N3 N2 1.340(3) 2_645 ? O4 H4A 0.8200 . ? O3 H3A 0.8200 . ? O1 H1A 0.8200 . ? O6 H6A 0.8200 . ? 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 C3 H3 N2 0.98 2.64 3.570(4) 158.4 4_575 C1 H1 N3 0.98 2.68 3.560(4) 149.7 3_665 C9 H9 O3 0.93 2.31 3.238(4) 173.4 4_475 C7 H7A O3 0.97 2.56 3.172(4) 121.5 . O4 H4A O6 0.82 2.38 3.107(3) 148.0 4_676 O3 H3A O1 0.82 1.96 2.772(3) 173.0 1_655 O1 H1A N3 0.82 2.04 2.857(3) 172.9 . O6 H6A O4 0.82 2.02 2.834(3) 172.7 1_455 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 O4 C4 C3 O3 60.5(3) . . . . ? C5 C4 C3 O3 -178.3(2) . . . . ? O4 C4 C3 C2 -178.5(2) . . . . ? C5 C4 C3 C2 -57.2(3) . . . . ? O3 C3 C2 O2 62.2(3) . . . . ? C4 C3 C2 O2 -58.0(3) . . . . ? O3 C3 C2 C1 -179.3(2) . . . . ? C4 C3 C2 C1 60.4(3) . . . . ? O2 C2 C1 O1 -61.5(3) . . . . ? C3 C2 C1 O1 177.5(2) . . . . ? O2 C2 C1 C6 61.9(3) . . . . ? C3 C2 C1 C6 -59.1(3) . . . . ? O1 C1 C6 O6 -60.1(3) . . . . ? C2 C1 C6 O6 174.9(2) . . . . ? O1 C1 C6 C5 179.3(2) . . . . ? C2 C1 C6 C5 54.2(3) . . . . ? O4 C4 C5 N1 -62.2(3) . . . . ? C3 C4 C5 N1 176.8(2) . . . . ? O4 C4 C5 C6 174.7(2) . . . . ? C3 C4 C5 C6 53.7(3) . . . . ? O6 C6 C5 N1 64.2(3) . . . . ? C1 C6 C5 N1 -175.9(2) . . . . ? O6 C6 C5 C4 -172.2(2) . . . . ? C1 C6 C5 C4 -52.3(3) . . . . ? O2 C7 C8 C9 -166.0(3) . . . 2_645 ? O2 C7 C8 N3 16.7(4) . . . . ? C8 C9 N1 N2 -0.2(3) 2_655 . . . ? C8 C9 N1 C5 179.4(2) 2_655 . . . ? C4 C5 N1 N2 -14.7(3) . . . . ? C6 C5 N1 N2 110.6(3) . . . . ? C4 C5 N1 C9 165.6(3) . . . . ? C6 C5 N1 C9 -69.0(3) . . . . ? C9 N1 N2 N3 -0.1(3) . . . 2_655 ? C5 N1 N2 N3 -179.8(2) . . . 2_655 ? C9 C8 N3 N2 -0.5(3) 2_645 . . 2_645 ? C7 C8 N3 N2 177.3(3) . . . 2_645 ? C8 C7 O2 C2 -80.4(3) . . . . ? C3 C2 O2 C7 -95.9(3) . . . . ? C1 C2 O2 C7 143.8(2) . . . . ?