#------------------------------------------------------------------------------ #$Date: 2021-09-01 02:03:20 +0300 (Wed, 01 Sep 2021) $ #$Revision: 268338 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/81/7708161.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_7708161 loop_ _publ_author_name 'Yang, Feng' 'Xu, Yuangang' 'Wang, Pengcheng' 'Lin, Qiuhan' 'Lu, Ming' _publ_section_title ; Novel metal--organic frameworks assembled from the combination of polynitro-pyrazole and 5-nitroamine-1,2,4-oxadiazole: synthesis, structure and thermal properties ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02093E _journal_year 2021 _chemical_formula_moiety 'C6 H4 K2 N10 O10' _chemical_formula_sum 'C6 H4 K2 N10 O10' _chemical_formula_weight 454.39 _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 difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-05-25 deposited with the CCDC. 2021-08-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.452(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3408(7) _cell_length_b 18.3261(13) _cell_length_c 8.4021(5) _cell_measurement_reflns_used 7761 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.39 _cell_measurement_theta_min 2.22 _cell_volume 1560.55(18) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON 100' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 15559 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.580 _diffrn_reflns_theta_min 2.223 _diffrn_source.source 'Ius 2.0' _diffrn_source.type microfocus _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.934 _exptl_crystal_description plate _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.229 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 253 _refine_ls_number_reflns 3583 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0350 _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^)+(0.0405P)^2^+0.4865P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.0845 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2884 _reflns_number_total 3583 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02093e2.cif _cod_data_source_block Y019_a _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7708161 _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 0.846 _shelx_estimated_absorpt_t_max 0.986 _shelx_res_file ; TITL Y019_a.res in P2(1)/c Y019_a.res created by SHELXL-2018/3 at 17:12:04 on 16-May-2020 CELL 0.71073 10.3408 18.3261 8.4021 90.000 101.452 90.000 ZERR 4.00 0.0007 0.0013 0.0005 0.000 0.002 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N O K UNIT 24 16 40 40 8 L.S. 10 omit -2 5 1 ACTA BOND $H FMAP 2 PLAN -5 CONF EQIV $10 x, y, z+1 HTAB C4 O3_$10 EQIV $11 -x+1, -y+1, -z+1 HTAB C4 O5_$11 HTAB O10 O1_$10 HTAB O10 O2_$10 size 0.25 0.23 0.02 FREE K1 N10 FREE K1 K2 TEMP 23.000 WGHT 0.040500 0.486500 FVAR 0.60746 C1 1 0.367031 0.438107 0.251406 11.00000 0.02851 0.02383 = 0.02291 -0.00001 0.00558 -0.00220 C2 1 0.493288 0.407008 0.280672 11.00000 0.02680 0.02427 = 0.02599 -0.00110 0.00928 -0.00201 C3 1 0.523585 0.395736 0.447912 11.00000 0.02403 0.02315 = 0.02697 0.00048 0.00673 -0.00339 C4 1 0.393017 0.414065 0.668392 11.00000 0.03174 0.02660 = 0.02091 -0.00143 0.00781 -0.00376 AFIX 3 H4B 2 0.475948 0.425565 0.746016 11.00000 -1.50000 H4A 2 0.326148 0.452765 0.672116 11.00000 -1.50000 AFIX 0 C5 1 0.346665 0.339242 0.699044 11.00000 0.02345 0.02700 = 0.02155 -0.00093 0.00797 0.00070 C6 1 0.225220 0.248034 0.686878 11.00000 0.02251 0.02791 = 0.02953 0.00326 0.00625 0.00262 K1 5 -0.282838 0.200872 0.383140 11.00000 0.03523 0.05253 = 0.03273 0.00248 0.00398 -0.00057 K2 5 0.036933 0.396685 0.408407 11.00000 0.02932 0.03801 = 0.04404 -0.00150 0.00515 0.00812 N1 3 0.318732 0.445119 0.383421 11.00000 0.02588 0.02666 = 0.02516 -0.00041 0.00449 -0.00081 N2 3 0.416633 0.419919 0.502686 11.00000 0.02358 0.02573 = 0.02111 0.00007 0.00546 -0.00206 N3 3 0.225233 0.314039 0.627081 11.00000 0.02517 0.02579 = 0.02771 0.00237 0.00411 -0.00086 N4 3 0.420613 0.294698 0.796545 11.00000 0.02531 0.03109 = 0.04319 0.00736 0.00193 -0.00397 N5 3 0.281084 0.456866 0.098397 11.00000 0.03153 0.05032 = 0.02720 0.00566 0.00652 0.00274 N6 3 0.569844 0.384602 0.165983 11.00000 0.03064 0.03231 = 0.02767 -0.00047 0.00944 -0.00170 N7 3 0.624580 0.366058 0.559127 11.00000 0.02282 0.04084 = 0.03183 0.00668 0.00571 -0.00148 N8 3 0.744388 0.379604 0.532944 11.00000 0.02476 0.03900 = 0.03611 0.00048 0.00674 0.00172 N9 3 0.139215 0.191940 0.676606 11.00000 0.02871 0.03144 = 0.04366 0.00751 0.00052 -0.00435 N10 3 0.026555 0.198532 0.569296 11.00000 0.03477 0.03465 = 0.04369 0.00525 0.00042 -0.00720 O1 4 0.203385 0.505900 0.097726 11.00000 0.06855 0.09843 = 0.04859 0.01623 0.00882 0.05230 O2 4 0.291930 0.421536 -0.019569 11.00000 0.05889 0.08007 = 0.02551 -0.00852 0.00406 0.00398 O3 4 0.570747 0.422706 0.047329 11.00000 0.05074 0.05293 = 0.03417 0.01253 0.02096 0.00126 O4 4 0.630425 0.327057 0.190552 11.00000 0.05756 0.03992 = 0.04446 0.00194 0.02182 0.01786 O5 4 0.766998 0.419870 0.423124 11.00000 0.03010 0.05190 = 0.04543 0.01189 0.01485 -0.00266 O6 4 0.836728 0.349562 0.630134 11.00000 0.02808 0.08081 = 0.06003 0.02527 0.00457 0.01345 O7 4 0.339480 0.232262 0.791287 11.00000 0.02614 0.02981 = 0.05276 0.01369 -0.00153 -0.00192 O8 4 -0.056431 0.149970 0.578220 11.00000 0.04662 0.06324 = 0.08182 0.02946 -0.01719 -0.03128 O9 4 0.002349 0.246652 0.465649 11.00000 0.04871 0.04639 = 0.05138 0.01746 -0.01179 -0.01296 O10 4 0.038948 0.466112 0.718604 11.00000 0.04868 0.05852 = 0.04683 0.00649 -0.00008 -0.00262 AFIX 3 H10A 2 0.094546 0.468180 0.804370 11.00000 -1.50000 H10B 2 -0.020654 0.432880 0.733970 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM Y019_a.res in P2(1)/c REM wR2 = 0.0845, GooF = S = 1.022, Restrained GooF = 1.022 for all data REM R1 = 0.0350 for 2884 Fo > 4sig(Fo) and 0.0498 for all 3583 data REM 253 parameters refined using 0 restraints END WGHT 0.0400 0.4857 REM Highest difference peak 0.229, deepest hole -0.310, 1-sigma level 0.061 Q1 1 -0.3768 0.1612 0.1444 11.00000 0.05 0.23 Q2 1 0.3790 0.3738 0.6781 11.00000 0.05 0.23 Q3 1 0.4223 0.4120 0.2393 11.00000 0.05 0.22 Q4 1 0.5358 0.4086 0.3629 11.00000 0.05 0.22 Q5 1 0.0819 0.2411 0.4393 11.00000 0.05 0.20 ; _shelx_res_checksum 97136 _shelx_hkl_file ; 0 0 -1 0.00 0.10 0 0 1 0.60 0.30 0 0 1 0.30 0.20 0 0 -1 -0.20 0.30 0 0 2 740.03 27.50 0 0 -2 729.93 27.50 0 0 -2 724.03 27.00 0 0 2 751.92 27.10 0 0 3 -0.70 0.80 0 0 -3 1.00 0.40 0 0 -3 0.10 1.00 0 0 3 0.50 0.60 0 0 -4 1136.39 43.10 0 0 4 1234.38 42.70 0 0 -4 1121.09 42.30 0 0 -4 1107.89 44.20 0 0 -5 1.20 2.00 0 0 5 -0.50 1.30 0 0 -5 0.40 0.80 0 0 -5 1.30 1.60 0 0 6 401.26 15.30 0 0 -6 366.36 14.90 0 0 -6 377.96 16.00 0 0 -6 382.36 16.70 0 0 -7 4.30 2.50 0 0 -7 2.10 1.20 0 0 -7 0.80 2.90 0 0 -8 1.10 1.70 0 0 -8 8.00 3.80 0 0 -8 -0.30 3.30 0 0 -9 -4.20 4.30 0 0 -9 -0.20 2.10 0 0 -10 128.39 12.20 0 0 -10 133.79 7.90 0 1 0 -0.10 0.10 0 1 0 0.00 0.10 0 -1 0 0.00 0.20 0 -1 0 -0.10 0.10 0 1 1 840.32 31.00 0 1 -1 792.12 30.50 0 1 1 865.51 30.90 0 1 -1 818.52 30.60 0 -1 -1 841.22 31.00 0 -1 1 836.82 30.60 0 -1 1 833.02 30.50 0 -1 -1 868.71 30.80 0 1 -2 199.98 7.60 0 1 -2 195.08 7.50 0 1 2 201.98 7.80 0 1 -2 189.58 7.70 0 1 2 193.88 8.10 0 -1 2 197.38 7.40 0 -1 -2 195.48 7.70 0 -1 -2 189.68 8.10 0 1 -3 56.19 3.10 0 1 3 60.39 3.70 0 1 -3 61.79 2.80 0 1 -3 61.39 3.40 0 -1 -3 62.89 2.90 0 -1 -3 62.59 3.80 0 -1 3 62.49 2.80 0 1 4 722.43 26.60 0 1 -4 712.73 26.90 0 1 -4 709.13 26.50 0 1 -4 683.93 26.00 0 -1 4 710.03 26.10 0 -1 -4 685.53 26.00 0 -1 -4 663.73 27.20 0 1 -5 -0.30 1.40 0 1 5 2.50 1.50 0 1 5 -1.20 1.70 0 1 -5 0.50 1.80 0 1 -5 -0.10 0.80 0 -1 -5 4.70 2.10 0 -1 -5 1.40 0.70 0 -1 5 1.20 1.20 0 1 6 202.88 9.40 0 1 -6 216.18 10.60 0 1 -6 246.78 9.90 0 1 -6 235.68 9.10 0 -1 6 214.58 9.10 0 -1 -6 208.48 10.90 0 -1 -6 199.38 8.90 0 -1 -6 208.18 10.30 0 1 -7 79.39 5.40 0 1 -7 74.49 6.20 0 1 -7 82.09 4.40 0 -1 -7 70.19 6.10 0 -1 -7 71.39 4.10 0 -1 -7 72.49 6.80 0 1 -8 198.28 11.30 0 1 -8 207.78 9.40 0 1 -8 218.58 10.50 0 -1 -8 211.38 9.10 0 -1 -8 206.58 11.10 0 -1 -8 196.28 11.80 0 1 -9 6.60 4.40 0 1 -9 17.40 3.00 0 -1 -9 9.00 4.80 0 -1 -9 17.80 2.80 0 1 -10 122.69 7.90 0 -1 -10 115.69 11.10 0 -1 -10 125.89 7.50 0 -2 0 336.97 13.10 0 -2 0 346.67 12.90 0 2 1 1011.20 36.50 0 2 -1 957.90 35.80 0 2 -1 993.10 36.30 0 2 1 1007.10 36.50 0 -2 -1 1004.70 36.50 0 -2 1 923.11 35.80 0 -2 1 993.70 36.20 0 -2 -1 969.40 36.50 0 2 -2 971.20 34.70 0 2 2 1033.10 35.40 0 2 2 979.60 35.50 0 2 -2 795.12 34.90 0 -2 -2 985.40 35.50 0 -2 2 968.10 34.60 0 -2 -2 853.21 35.40 0 -2 2 956.90 34.60 0 2 3 784.42 30.00 0 2 -3 746.43 29.00 0 2 3 807.02 29.80 0 2 -3 800.12 29.00 0 2 -3 783.32 29.20 0 -2 -3 766.22 29.30 0 2 4 291.17 12.80 0 2 -4 292.67 12.20 0 2 4 305.97 12.40 0 2 -4 292.27 11.60 0 2 -4 308.77 11.80 0 -2 -4 282.97 12.90 0 -2 4 313.57 11.40 0 -2 -4 284.57 11.70 0 2 -5 502.85 19.30 0 2 -5 523.05 19.50 0 2 -5 504.15 20.10 0 2 5 486.25 20.50 0 2 5 506.15 20.00 0 -2 -5 492.85 20.90 0 -2 5 503.65 19.10 0 -2 -5 495.65 19.20 0 2 -6 260.77 10.40 0 2 6 226.78 11.30 0 2 -6 231.48 11.00 0 2 6 227.98 10.60 0 2 -6 243.58 10.00 0 -2 -6 222.58 11.80 0 -2 -6 240.18 9.70 0 -2 6 229.78 9.60 0 2 -7 45.60 4.30 0 2 -7 46.70 3.70 0 2 -7 42.60 5.30 0 -2 -7 44.40 5.60 0 -2 -7 42.70 3.20 0 -2 -7 48.60 6.40 0 2 -8 21.30 3.10 0 2 -8 21.40 4.20 0 2 -8 20.80 3.60 0 -2 -8 18.30 2.40 0 -2 -8 18.40 4.80 0 -2 -8 16.00 4.60 0 2 -9 162.38 10.40 0 2 -9 162.68 8.60 0 -2 -9 159.88 7.80 0 -2 -9 149.39 11.40 0 2 -10 10.90 3.80 0 -2 -10 6.30 6.20 0 -2 -10 8.50 2.90 0 3 0 -0.20 0.60 0 3 0 -0.60 0.50 0 -3 0 -0.10 0.50 0 -3 0 0.20 0.50 0 -3 0 0.50 0.60 0 3 -1 86.19 3.50 0 3 1 83.69 4.30 0 3 -1 81.19 4.10 0 3 1 90.49 4.30 0 -3 -1 83.79 4.20 0 -3 1 86.99 4.10 0 -3 -1 83.09 4.30 0 -3 1 88.89 3.40 0 3 -2 17.90 1.80 0 3 -2 18.10 1.10 0 3 2 20.50 2.20 0 3 2 20.60 2.10 0 -3 2 17.20 1.20 0 -3 2 18.20 1.40 0 -3 -2 18.60 2.00 0 -3 -2 18.10 2.30 0 3 3 901.21 32.80 0 3 -3 856.21 32.10 0 3 -3 778.02 31.80 0 -3 -3 820.32 32.90 0 -3 3 909.71 31.60 0 -3 -3 873.01 32.40 0 -3 3 851.81 31.80 0 3 -4 424.26 16.80 0 3 -4 441.16 16.60 0 3 -4 420.06 16.80 0 3 4 450.95 17.60 0 3 4 434.56 18.00 0 -3 -4 431.36 18.10 0 -3 4 422.16 16.20 0 -3 -4 422.86 16.90 0 3 -5 159.78 7.40 0 3 5 174.78 8.90 0 3 5 162.58 8.20 0 3 -5 171.98 7.40 0 -3 5 172.18 6.80 0 -3 -5 168.08 9.10 0 -3 -5 157.88 7.30 0 3 -6 67.99 4.30 0 3 6 60.89 5.10 0 3 -6 65.29 4.10 0 3 -6 58.59 4.90 0 3 6 57.19 5.70 0 -3 -6 61.09 3.60 0 -3 6 55.99 3.40 0 -3 -6 55.99 5.90 0 3 7 13.20 3.80 0 3 -7 9.30 2.60 0 3 -7 6.60 2.80 0 3 -7 9.10 2.30 0 -3 -7 9.90 1.70 0 -3 -7 11.70 3.80 0 -3 -7 9.70 3.90 0 3 -8 123.09 8.20 0 3 -8 107.89 7.50 0 3 -8 125.39 7.20 0 -3 -8 129.49 6.30 0 -3 -8 129.39 9.60 0 -3 -8 130.39 9.80 0 3 -9 0.30 3.00 0 3 -9 10.10 4.10 0 -3 -9 1.90 2.10 0 -3 -9 3.90 5.10 0 3 -10 9.40 4.10 0 -3 -10 10.00 2.80 0 -3 -10 9.70 7.40 0 4 0 3398.86 122.29 0 4 0 3385.06 121.69 0 -4 0 3303.97 122.19 0 -4 0 3234.28 121.59 0 4 -1 2318.17 87.99 0 4 1 2450.85 88.79 0 4 -1 2409.86 88.79 0 -4 1 2522.95 88.69 0 -4 -1 2430.06 88.69 0 -4 1 2325.57 87.79 0 4 -2 2124.99 79.69 0 4 -2 2071.99 78.59 0 4 2 2238.28 80.09 0 4 2 2259.07 80.19 0 -4 2 2118.19 79.29 0 -4 -2 2197.28 80.09 0 -4 -2 2105.69 79.89 0 4 3 4218.38 154.38 0 4 3 4385.26 154.28 0 4 -3 4122.99 153.58 0 -4 3 4221.58 152.98 0 -4 -3 4091.79 153.88 0 -4 -3 4229.78 154.48 0 -4 3 4128.59 152.78 0 4 4 25.00 3.50 0 4 -4 19.50 2.10 0 4 4 25.20 3.10 0 4 -4 19.40 2.10 0 4 -4 23.20 2.50 0 -4 4 25.00 1.70 0 -4 -4 20.70 2.50 0 -4 -4 22.80 3.40 0 4 -5 1.10 1.50 0 4 5 0.30 2.00 0 4 5 0.50 2.60 0 4 -5 -0.60 1.50 0 4 -5 1.00 1.50 0 -4 5 0.50 0.80 0 -4 -5 0.70 2.40 0 -4 -5 -0.90 1.20 0 4 -6 1.60 1.80 0 4 -6 3.60 2.20 0 4 6 2.60 2.70 0 4 6 -0.70 3.00 0 -4 6 2.20 1.20 0 -4 -6 0.20 1.30 0 -4 -6 1.10 3.00 0 4 -7 829.32 35.60 0 4 7 950.50 37.60 0 4 -7 937.81 36.10 0 4 -7 953.00 36.10 0 -4 -7 950.80 38.00 0 -4 -7 969.10 35.30 0 4 -8 52.89 5.30 0 4 -8 48.20 5.60 0 4 -8 51.49 6.00 0 -4 -8 46.80 3.70 0 -4 -8 64.09 7.80 0 4 -9 7.00 4.00 0 4 -9 5.80 3.40 0 -4 -9 1.60 5.20 0 -4 -9 2.60 2.10 0 4 -10 25.50 5.00 0 -4 -10 14.80 2.90 0 -4 -10 23.10 7.30 0 5 0 0.50 1.00 0 5 0 1.40 1.00 0 -5 0 1.70 1.20 0 -5 0 -1.10 1.00 0 -5 0 0.30 0.70 0 5 -1 8591.74 339.87 0 5 1 9561.34 339.07 0 5 1 9999.00 339.57 0 -5 1 9191.18 339.07 0 -5 1 8810.32 339.17 0 -5 -1 9701.93 339.37 0 5 -2 3145.19 111.79 0 5 -2 2899.41 110.49 0 5 2 3193.98 112.19 0 5 2 3207.38 112.09 0 -5 2 2902.21 110.39 0 -5 2 2648.24 111.79 0 -5 -2 3132.19 111.99 0 -5 -2 3128.59 111.99 0 5 3 801.32 31.60 0 5 -3 809.72 29.70 0 5 3 779.72 31.60 0 5 -3 800.42 31.00 0 -5 -3 774.02 31.20 0 -5 3 832.52 29.90 0 -5 3 827.32 30.30 0 -5 -3 807.82 31.70 0 5 4 48.70 4.40 0 5 -4 42.90 3.70 0 5 -4 45.70 2.30 0 5 4 51.29 4.80 0 -5 4 40.10 2.80 0 -5 -4 45.70 4.70 0 -5 4 44.70 2.60 0 -5 -4 48.40 3.80 0 5 5 1103.59 42.60 0 5 -5 1085.39 41.90 0 5 5 1078.59 43.00 0 5 -5 1109.59 40.70 0 5 -5 1123.39 41.20 0 -5 -5 1108.99 43.30 0 -5 5 1067.49 40.70 0 -5 -5 1106.09 41.80 0 5 -6 46.20 4.40 0 5 -6 44.10 3.50 0 5 -6 46.30 4.20 0 5 6 47.10 5.90 0 5 6 42.90 5.40 0 -5 6 46.20 4.30 0 -5 6 47.90 2.90 0 -5 -6 45.30 6.20 0 -5 -6 43.30 3.80 0 5 7 176.78 11.70 0 5 -7 179.58 9.30 0 5 -7 190.88 8.70 0 5 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206.78 8.80 1 1 3 221.08 9.20 -1 1 -3 198.08 8.50 1 -1 3 218.78 8.50 -1 -1 -3 210.38 9.10 1 -1 3 206.48 8.50 -1 -1 -3 209.98 8.40 1 1 4 176.58 7.90 -1 1 -4 172.88 7.50 1 1 4 177.78 8.30 -1 1 -4 173.68 7.40 -1 1 -4 176.48 7.80 1 -1 4 186.58 7.60 -1 -1 -4 173.28 8.30 1 -1 4 187.98 7.50 -1 -1 -4 167.78 7.30 -1 1 -5 218.28 9.10 1 1 5 219.68 9.60 -1 1 -5 196.18 10.00 1 1 5 219.78 9.90 -1 1 -5 204.68 8.90 -1 -1 -5 210.38 8.80 1 -1 5 201.38 9.00 -1 -1 -5 208.88 9.90 -1 1 -6 90.49 5.20 1 1 6 85.29 6.00 -1 1 -6 81.39 5.60 -1 1 -6 85.39 4.70 1 1 6 99.19 6.10 1 -1 6 83.49 5.20 -1 -1 -6 82.89 6.10 -1 -1 -6 87.39 4.70 -1 1 -7 569.44 23.50 -1 1 -7 588.84 23.00 -1 1 -7 604.44 23.00 -1 -1 -7 581.44 23.70 -1 -1 -7 568.24 24.10 -1 -1 -7 566.74 22.70 -1 1 -8 146.99 8.60 -1 1 -8 145.39 8.20 -1 1 -8 149.59 7.70 -1 -1 -8 121.09 7.10 -1 -1 -8 148.69 9.10 -1 -1 -8 143.39 9.30 -1 1 -9 8.30 3.10 -1 1 -9 7.40 4.10 -1 -1 -9 7.80 4.50 -1 -1 -9 4.10 2.60 -1 1 -10 56.09 6.70 -1 -1 -10 58.09 6.30 1 2 -10 8.20 5.80 1 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5.30 1.70 -5 -7 0 6.60 1.90 -5 7 -1 63.59 6.30 5 7 1 74.39 6.00 5 7 1 54.79 6.20 5 -7 1 63.99 4.70 -5 -7 -1 63.59 4.70 5 -7 1 62.49 4.20 -5 -7 -1 61.89 4.00 5 -7 1 63.59 4.60 5 7 2 19.90 4.10 5 7 2 20.90 4.30 -5 7 -2 20.90 4.30 5 -7 2 17.50 2.40 5 -7 2 25.00 3.10 -5 -7 -2 23.50 2.90 -5 -7 -2 16.60 2.70 5 -7 2 15.20 2.00 5 7 3 269.27 14.80 5 7 3 274.47 15.10 -5 7 -3 307.47 15.10 -5 -7 -3 306.67 12.90 5 -7 3 294.07 12.80 -5 -7 -3 281.27 12.90 -5 7 -4 574.34 25.40 5 7 4 566.04 26.50 5 7 4 550.94 25.70 -5 -7 -4 573.44 23.30 -5 -7 -4 593.04 23.30 -5 7 -5 135.99 10.30 -5 -7 -5 134.59 7.80 -5 -7 -5 124.99 7.80 -5 7 -6 14.00 7.60 -5 -7 -6 14.10 3.60 -5 7 -7 5.60 6.00 -5 -7 -7 4.40 3.80 -5 -7 -7 15.40 3.30 -5 7 -8 14.40 6.60 -5 -7 -8 19.70 4.50 -5 -7 -8 18.40 5.00 5 8 -10 3.00 7.00 5 -8 -10 3.10 2.90 5 -8 -10 16.90 10.60 5 -8 -10 4.50 3.10 5 8 -9 45.80 7.10 5 -8 -9 19.50 9.10 5 -8 -9 38.50 5.00 5 -8 -9 39.90 4.80 5 -8 -8 82.39 7.10 5 -8 -8 93.29 11.20 5 -8 -8 92.39 8.10 -5 -8 8 93.99 9.90 5 -8 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181.58 9.60 -5 -9 5 169.38 7.40 5 -9 -5 193.48 11.50 5 -9 -5 165.78 11.80 5 -9 -5 162.08 9.90 -5 -9 5 129.19 9.60 5 9 -4 24.90 3.50 5 9 -4 22.50 4.40 -5 -9 4 19.70 4.30 -5 -9 4 23.60 2.80 5 -9 -4 20.30 3.70 5 -9 -4 15.50 4.70 5 9 -3 777.22 31.20 5 9 -3 812.22 32.80 5 -9 -3 816.42 32.10 -5 -9 3 795.72 32.40 -5 -9 3 782.92 30.70 5 -9 -3 768.22 32.00 5 -9 -3 781.82 33.00 5 9 -2 140.19 8.10 5 9 -2 134.49 9.20 -5 9 2 150.18 9.90 5 -9 -2 139.19 8.50 5 -9 -2 148.89 8.60 5 -9 -2 147.99 9.20 -5 -9 2 142.39 7.90 5 9 -1 48.40 6.10 5 9 -1 57.39 5.70 -5 9 1 60.09 7.00 5 -9 -1 57.69 5.10 -5 -9 1 55.99 4.00 -5 -9 1 52.89 4.60 5 -9 -1 54.09 5.10 5 -9 -1 60.79 5.70 5 9 0 20.30 4.10 -5 9 0 4.70 3.70 5 9 0 7.40 4.00 5 -9 0 9.20 2.70 -5 -9 0 8.00 2.40 5 -9 0 13.90 3.00 5 -9 0 10.10 2.40 -5 -9 0 11.30 2.10 5 9 1 -1.80 3.50 5 9 1 -0.80 3.90 -5 9 -1 -4.90 3.10 5 -9 1 3.50 2.40 -5 -9 -1 1.00 1.50 5 -9 1 1.00 2.30 5 -9 1 1.80 1.60 -5 -9 -1 3.70 2.30 5 9 2 501.15 23.70 -5 9 -2 535.05 24.40 5 9 2 565.14 25.10 -5 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52.49 4.20 7 -10 -5 59.19 6.60 7 10 -4 5.30 4.60 -7 10 4 9.60 5.50 7 -10 -4 9.60 5.00 -7 -10 4 9.70 4.80 -7 -10 4 7.60 2.20 7 -10 -4 11.60 3.90 -7 10 3 4.40 4.90 7 10 -3 2.60 4.10 -7 -10 3 2.40 4.20 -7 -10 3 5.30 2.00 7 -10 -3 9.90 3.30 7 -10 -3 5.10 4.60 7 10 -2 184.58 12.70 -7 10 2 165.78 12.70 7 -10 -2 188.48 12.00 -7 -10 2 175.88 11.20 7 -10 -2 183.68 10.20 -7 -10 2 174.38 9.00 7 10 -1 144.79 11.80 -7 10 1 169.48 12.90 -7 -10 1 138.19 9.80 7 -10 -1 152.88 10.30 7 -10 -1 132.69 9.40 -7 -10 1 146.89 8.20 7 -10 -1 145.19 8.90 7 10 0 298.17 17.70 -7 10 0 316.27 17.90 -7 -10 0 297.17 13.60 7 -10 0 290.17 14.80 -7 -10 0 300.47 13.90 7 -10 0 294.67 13.50 7 10 1 54.39 8.20 -7 10 -1 73.79 9.90 -7 -10 -1 49.60 5.40 7 -10 1 44.50 4.90 7 -10 1 55.19 6.20 -7 -10 -1 56.19 4.80 7 -10 1 52.59 5.50 -7 10 -2 43.10 7.80 7 10 2 49.50 9.20 7 -10 2 31.70 4.40 -7 -10 -2 43.40 4.50 -7 -10 -2 42.80 5.30 7 -10 2 40.10 5.40 -7 10 -3 21.60 7.40 -7 -10 -3 26.40 4.50 7 -10 3 16.20 2.30 7 -10 3 21.50 2.40 -7 -10 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27.80 5.60 8 8 -1 610.34 27.50 -8 8 1 563.84 30.80 -8 -8 1 575.14 24.20 -8 -8 1 597.14 26.40 8 -8 -1 578.74 24.80 8 -8 -1 676.63 26.50 8 -8 -1 620.84 26.60 -8 8 0 4.10 5.10 8 8 0 5.50 5.20 -8 -8 0 5.70 2.70 8 -8 0 6.20 3.70 8 -8 0 5.60 2.50 8 -8 0 7.00 3.40 -8 -8 0 3.90 3.40 8 8 1 447.76 22.30 -8 8 -1 431.76 22.30 -8 -8 -1 431.76 18.50 8 -8 1 422.86 18.80 8 -8 1 430.26 19.40 -8 -8 -1 465.65 19.30 8 -8 1 409.56 18.20 8 8 2 925.21 41.70 -8 8 -2 957.60 41.50 8 -8 2 923.91 38.20 -8 -8 -2 962.40 38.00 8 -8 2 1010.40 36.30 -8 -8 -2 1020.50 38.00 8 -8 2 947.21 37.90 -8 8 -3 42.30 7.70 -8 -8 -3 55.79 6.20 -8 -8 -3 51.19 5.90 -8 8 -4 91.29 12.40 -8 -8 -4 92.39 7.70 -8 -8 -4 99.49 7.00 -8 8 -5 306.07 20.70 -8 -8 -5 320.07 14.60 -8 -8 -5 320.57 15.90 -8 8 -6 9.50 8.20 -8 -8 -6 16.30 4.00 -8 -8 -6 8.40 3.80 8 -9 -8 119.99 12.20 -8 -9 8 114.29 14.20 8 -9 -8 140.79 17.20 8 9 -7 59.69 7.50 8 -9 -7 62.19 8.50 8 -9 -7 71.19 10.50 -8 -9 7 48.30 8.70 8 9 -6 176.48 12.10 -8 -9 6 169.88 12.70 8 -9 -6 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241.18 15.10 10 -7 2 238.18 13.30 -10 -7 -2 225.88 12.60 -10 7 -3 -4.40 11.80 -10 -7 -3 2.80 3.70 -10 -7 -3 8.00 6.20 -10 7 -4 4.50 7.60 -10 -7 -4 7.20 6.50 10 -8 -7 -3.50 8.60 -10 -8 7 13.00 8.10 10 -8 -6 9.00 8.40 -10 -8 6 29.80 7.70 -10 -8 5 34.30 7.00 10 -8 -5 40.70 8.80 10 -8 -4 22.80 7.50 -10 -8 4 25.40 6.10 -10 -8 3 -2.60 4.30 -10 -8 2 15.70 5.30 -10 8 1 131.89 14.80 -10 -8 1 131.79 11.60 10 -8 -1 138.99 11.90 -10 8 0 36.00 8.20 10 -8 0 49.99 7.30 -10 -8 0 52.99 8.10 -10 -8 0 50.59 6.00 -10 8 -1 86.59 11.20 10 -8 1 81.19 8.70 -10 -8 -1 87.79 7.40 -10 -8 -1 87.09 10.40 -10 8 -2 13.60 7.50 -10 -8 -2 14.50 4.10 10 -8 2 3.20 5.20 -10 -8 -2 13.70 6.10 -10 8 -3 142.99 17.10 -10 -8 -3 158.68 12.80 -10 -8 -3 139.69 10.30 -10 8 -4 6.30 10.20 -10 -8 -4 18.20 5.40 -10 -8 -4 16.70 6.80 -10 -9 7 18.80 8.80 10 -9 -7 10.60 9.70 10 -9 -6 11.70 9.20 -10 -9 6 12.10 7.00 10 -9 -5 -4.50 7.50 -10 -9 5 -1.70 5.60 -10 -9 4 208.38 13.60 10 -9 -4 152.58 15.60 10 -9 -3 31.60 8.30 -10 -9 3 48.60 7.40 10 -9 -2 -3.60 6.80 -10 -9 2 -2.50 5.30 10 -9 -1 108.29 11.40 -10 -9 1 97.59 11.10 -10 9 0 56.49 9.80 -10 -9 0 44.90 7.40 10 -9 0 58.99 8.10 -10 9 -1 22.30 8.70 -10 -9 -1 23.00 4.60 10 -9 1 25.00 6.20 -10 -9 -1 39.00 7.60 -10 9 -2 24.40 7.80 -10 -9 -2 34.00 6.90 -10 -9 -2 27.60 4.70 -10 9 -3 14.40 12.70 -10 -9 -3 14.00 6.20 -10 9 -4 17.30 11.10 -10 -9 -4 15.10 6.50 -10 -9 -4 8.60 4.20 10 -10 -7 8.20 10.40 -10 -10 7 19.90 8.70 10 -10 -6 8.10 9.10 -10 -10 6 7.30 7.00 10 -10 -5 -9.90 8.40 -10 -10 5 -2.90 6.30 10 -10 -4 1.90 7.30 -10 -10 4 3.90 6.00 10 -10 -3 8.10 7.40 -10 -10 3 9.60 6.00 -10 -10 2 385.06 20.60 -10 -10 1 21.20 6.80 10 -10 -1 21.50 7.00 -10 10 0 21.70 9.40 10 -10 0 10.30 6.50 -10 -10 0 20.30 6.30 -10 10 -1 13.20 9.20 10 -10 1 6.30 5.80 -10 -10 -1 18.40 6.80 -10 10 -2 12.30 9.30 -10 -10 -2 5.80 6.40 -10 -10 -3 27.50 6.30 -10 -10 -3 26.20 6.70 -10 -11 6 208.28 15.60 10 -11 -6 183.38 19.40 10 -11 -5 30.20 10.60 -10 -11 5 44.20 8.00 10 -11 -4 29.50 9.30 -10 -11 4 29.50 7.50 10 -11 -3 26.40 8.70 -10 -11 3 20.60 6.70 -10 -11 2 23.70 6.60 10 -11 -1 25.70 7.50 -10 -11 1 5.10 5.90 -10 -11 0 127.69 12.80 10 -11 0 127.89 12.70 -10 11 -1 5.70 10.10 10 -11 1 -8.50 6.00 -10 -11 -1 -0.10 6.30 -10 11 -2 9.00 10.80 -10 -11 -2 20.00 6.50 -10 11 -3 13.70 12.90 -10 -11 -3 0.60 5.90 -10 -12 6 -5.60 6.90 10 -12 -6 2.00 10.20 10 -12 -5 10.50 9.80 -10 -12 5 -3.00 6.60 10 -12 -4 14.00 9.20 -10 -12 4 7.40 6.80 -10 -12 3 23.10 7.90 10 -12 -3 25.50 8.70 10 -12 -2 153.48 15.60 -10 -12 2 163.38 14.30 -10 -12 1 3.10 6.80 10 -12 0 0.00 6.70 -10 -12 0 0.00 6.50 -10 -12 -1 23.10 7.20 -10 -12 -2 60.69 8.20 -10 -12 -3 71.99 9.00 10 -13 -5 33.50 11.80 -10 -13 5 44.80 8.60 -10 -13 4 3.70 7.30 10 -13 -4 9.40 9.40 -10 -13 3 64.09 9.70 10 -13 -3 58.89 10.60 10 -13 -2 80.99 11.30 -10 -13 2 48.50 9.60 -10 -13 1 9.60 7.20 -10 -13 0 6.80 7.40 10 -13 0 3.60 7.10 -10 -13 -1 31.50 7.90 -10 -13 -2 28.70 7.30 -10 -14 5 8.80 7.30 10 -14 -5 0.50 11.00 10 -14 -4 58.39 11.90 -10 -14 4 48.90 9.20 -10 -14 3 37.70 8.90 10 -14 -3 27.80 10.10 10 -14 -2 11.40 9.10 -10 -14 2 3.00 7.30 -10 -14 1 13.80 7.50 -10 -14 0 31.40 8.10 10 -14 0 15.20 8.30 -10 -14 -1 7.40 6.70 10 -15 -4 16.10 12.00 -10 -15 4 7.50 8.20 -10 -15 3 45.60 9.30 10 -15 -3 56.89 11.50 -10 -15 2 -1.50 7.90 10 -15 -2 11.40 9.50 10 -15 -1 63.09 11.60 -10 -15 1 105.49 12.50 -10 -15 0 32.50 8.80 11 0 -7 5.20 8.10 -11 0 7 13.70 8.50 -11 0 6 5.50 8.00 -11 0 5 1.40 6.60 -11 0 4 -2.70 5.20 -11 0 3 -3.50 4.90 -11 0 2 199.98 13.10 -11 0 1 11.10 4.50 -11 0 0 144.09 11.10 -11 0 0 148.19 10.50 -11 0 -1 -1.20 4.40 -11 0 -1 -0.90 4.00 -11 0 -2 81.49 8.20 -11 0 -2 97.79 9.60 -11 0 -3 -2.70 4.20 -11 0 -3 -1.70 4.60 -11 0 -4 14.20 6.70 11 -1 -7 27.40 8.40 -11 -1 7 44.00 10.30 -11 1 6 37.30 9.50 11 -1 -6 45.20 9.00 -11 -1 6 41.30 8.90 -11 1 5 25.40 7.80 -11 -1 5 50.59 8.70 -11 1 4 38.90 8.00 -11 -1 4 53.19 8.20 -11 1 3 20.80 6.20 -11 -1 3 9.70 5.10 -11 1 2 106.59 9.80 -11 -1 2 94.89 9.30 -11 1 1 370.66 17.80 -11 -1 1 330.47 17.60 -11 1 0 -6.90 3.60 -11 -1 0 4.10 4.30 -11 -1 0 0.70 4.00 -11 1 -1 30.80 5.90 -11 1 -1 47.50 6.20 -11 -1 -1 42.80 6.10 -11 -1 -1 34.60 6.60 -11 1 -2 7.70 4.70 -11 1 -2 11.30 4.50 -11 -1 -2 7.30 5.50 -11 -1 -2 5.30 4.90 -11 1 -3 75.99 8.00 -11 1 -3 77.29 9.80 -11 -1 -3 50.99 7.00 -11 -1 -3 81.69 8.60 -11 1 -4 -7.60 5.80 -11 -1 -4 -13.80 5.80 11 -2 -7 30.40 9.20 -11 -2 7 43.90 10.60 11 -2 -6 25.10 8.60 -11 -2 6 29.20 8.70 -11 2 5 112.09 13.70 -11 -2 5 132.89 12.50 -11 2 4 14.40 6.30 -11 -2 4 9.30 5.80 -11 2 3 540.05 25.70 -11 -2 3 530.15 24.80 -11 2 2 202.78 13.10 -11 -2 2 164.48 12.10 -11 2 1 45.60 6.80 -11 -2 1 73.99 8.20 -11 2 0 50.19 6.90 -11 2 0 47.40 7.20 -11 -2 0 45.50 6.30 -11 -2 0 34.10 5.80 -11 2 -1 72.69 8.30 -11 2 -1 73.19 9.50 -11 -2 -1 87.09 8.20 -11 -2 -1 77.89 8.50 -11 2 -2 -3.40 4.20 -11 2 -2 0.40 5.60 -11 -2 -2 0.00 4.40 -11 -2 -2 6.40 4.70 -11 2 -3 50.89 6.60 -11 2 -3 54.09 9.90 -11 -2 -3 40.70 6.10 -11 -2 -3 41.30 6.40 -11 2 -4 -3.50 6.90 -11 -2 -4 4.60 5.10 11 -3 -7 11.20 8.70 -11 -3 7 -9.20 8.40 -11 -3 6 11.10 7.70 11 -3 -6 21.40 8.30 -11 3 5 48.00 9.30 -11 -3 5 50.79 8.90 11 -3 -5 44.80 9.20 -11 3 4 177.48 14.70 -11 -3 4 218.28 14.10 -11 3 3 0.30 5.30 -11 -3 3 3.90 5.00 -11 3 2 514.25 24.80 -11 -3 2 537.05 24.10 -11 3 1 25.10 5.70 -11 -3 1 33.60 6.10 -11 3 0 321.37 18.20 -11 3 0 323.27 16.90 -11 -3 0 335.97 16.70 -11 3 -1 29.30 5.50 -11 3 -1 20.70 6.20 -11 -3 -1 28.60 5.50 -11 -3 -1 28.90 4.70 -11 3 -2 178.48 13.70 -11 3 -2 177.18 11.40 -11 -3 -2 174.38 11.40 -11 -3 -2 159.98 11.50 -11 -3 -3 17.50 5.50 -11 -3 -3 13.90 5.10 -11 3 -4 15.00 8.10 -11 -3 -4 4.30 4.60 -11 -3 -4 1.70 5.40 11 -4 -7 30.50 9.80 -11 -4 7 36.70 10.00 11 -4 -6 39.60 9.70 -11 -4 6 61.19 9.60 -11 -4 5 -2.70 5.50 11 -4 -5 1.70 6.30 -11 4 4 28.10 7.20 -11 -4 4 15.50 6.20 11 -4 -4 3.20 6.30 -11 4 3 14.70 6.50 -11 -4 3 11.00 5.30 11 -4 -3 12.40 6.20 -11 4 2 147.29 12.10 -11 -4 2 141.09 11.20 -11 4 1 -3.40 5.40 -11 -4 1 3.50 4.80 -11 4 0 47.70 7.90 -11 4 0 45.30 6.90 -11 -4 0 52.99 6.70 -11 4 -1 22.30 5.40 -11 4 -1 28.70 7.50 -11 -4 -1 22.10 4.20 -11 -4 -1 31.30 5.90 -11 4 -2 5.90 7.00 -11 4 -2 3.50 4.70 -11 -4 -2 6.50 5.00 -11 -4 -2 6.20 3.80 -11 4 -3 2.30 8.50 -11 -4 -3 5.10 3.90 -11 -4 -3 10.40 5.70 -11 -4 -4 13.00 5.10 -11 -4 -4 15.50 6.30 -11 -5 7 42.10 9.90 11 -5 -7 48.30 11.20 11 -5 -6 35.60 9.40 -11 -5 6 34.50 9.00 11 -5 -5 20.90 12.00 -11 -5 5 19.40 6.40 11 -5 -4 7.50 6.50 -11 -5 4 10.30 5.70 11 -5 -3 9.00 6.20 -11 -5 3 3.20 4.90 -11 5 2 7.20 6.00 -11 -5 2 -0.60 4.60 -11 5 1 18.50 6.60 -11 -5 1 15.80 5.40 -11 5 0 -1.00 4.90 -11 -5 0 4.00 4.80 -11 5 -1 21.40 5.90 -11 5 -1 14.80 7.00 -11 -5 -1 29.60 6.20 -11 5 -2 0.00 4.80 -11 5 -2 2.50 7.30 -11 -5 -2 -0.20 4.60 11 -5 2 -2.70 5.00 -11 -5 -2 -1.60 5.60 -11 5 -3 19.20 8.20 -11 -5 -3 17.20 6.50 -11 -5 -3 16.70 6.30 11 -6 -7 3.40 9.80 -11 -6 7 18.70 9.40 -11 -6 6 119.09 13.70 11 -6 -6 114.69 15.60 11 -6 -5 69.79 11.30 -11 -6 5 88.79 11.00 11 -6 -4 15.10 7.40 -11 -6 4 2.00 5.50 11 -6 -3 31.70 8.20 -11 -6 3 49.00 7.40 -11 -6 2 11.40 5.50 -11 -6 1 17.10 5.50 11 -6 -1 4.30 7.00 11 -6 0 172.58 13.00 -11 -6 0 180.38 12.60 -11 6 -1 11.40 6.80 -11 -6 -1 21.40 6.30 11 -6 1 31.30 6.50 -11 6 -2 -4.80 6.40 -11 -6 -2 -3.50 6.10 -11 -6 -3 11.90 7.00 11 -7 -7 -5.40 10.30 -11 -7 7 7.50 8.50 11 -7 -6 56.69 11.40 -11 -7 6 30.80 8.50 -11 -7 5 43.40 8.50 11 -7 -5 35.90 8.90 -11 -7 4 106.29 11.20 11 -7 -4 100.39 12.00 -11 -7 3 22.50 6.30 11 -7 -3 14.20 7.70 -11 -7 2 83.29 9.80 11 -7 -2 69.29 10.10 11 -7 -1 232.78 17.50 -11 -7 1 217.38 14.40 11 -7 0 68.39 8.80 -11 -7 0 71.79 9.10 11 -7 1 121.39 11.80 -11 -7 -1 116.19 12.20 -11 7 -2 17.10 9.60 -11 -7 -2 22.40 7.60 -11 -7 -3 17.90 7.20 11 -8 -6 67.89 12.40 -11 -8 6 78.39 10.20 -11 -8 5 47.00 8.30 11 -8 -5 46.10 10.90 11 -8 -4 0.20 8.30 -11 -8 4 12.40 6.00 11 -8 -3 191.98 16.60 -11 -8 3 191.88 13.70 -11 -8 2 -1.70 5.20 11 -8 -2 2.40 7.00 -11 -8 1 27.20 7.00 11 -8 0 -1.10 6.50 -11 -8 0 -0.20 6.10 11 -8 1 82.59 9.20 -11 -8 -1 98.89 12.20 -11 -8 -2 68.89 9.80 -11 -8 -3 -13.80 7.30 11 -9 -6 60.29 12.30 -11 -9 6 102.19 12.90 11 -9 -5 80.99 13.20 -11 -9 5 112.19 12.50 11 -9 -4 18.00 9.20 -11 -9 4 23.30 7.00 -11 -9 3 27.70 6.50 11 -9 -3 19.50 8.90 11 -9 -2 14.10 7.90 -11 -9 2 10.10 6.30 -11 -9 1 26.40 7.40 -11 -9 0 0.60 6.50 11 -9 0 -5.80 6.60 11 -9 1 -3.00 7.20 -11 -9 -1 3.40 6.90 -11 -9 -2 -3.50 7.30 -11 -10 6 40.20 8.70 -11 -10 5 5.90 6.70 11 -10 -5 -3.60 10.00 11 -10 -4 10.00 9.30 -11 -10 4 15.00 6.50 11 -10 -3 37.80 9.80 -11 -10 3 28.40 7.30 11 -10 -2 -2.30 7.70 -11 -10 2 5.40 6.00 -11 -10 1 8.80 7.30 11 -10 0 84.89 10.30 -11 -10 0 62.19 9.30 -11 -10 -1 4.10 7.80 -11 -10 -2 12.50 8.30 11 -11 -5 11.60 10.20 -11 -11 5 3.10 7.30 11 -11 -4 -4.90 9.50 -11 -11 4 2.30 6.80 11 -11 -3 4.90 9.00 -11 -11 3 -6.60 6.40 11 -11 -2 12.40 8.60 -11 -11 2 -7.90 7.00 -11 -11 1 112.79 13.20 11 -11 0 11.00 7.70 -11 -11 0 -1.90 7.60 -11 -11 -1 19.10 8.30 -11 -12 4 13.10 7.40 11 -12 -4 23.50 10.50 -11 -12 3 11.80 7.30 11 -12 -3 14.10 10.10 11 -12 -2 59.09 11.30 -11 -12 2 48.20 8.80 -11 -12 1 11.10 7.90 11 -12 -1 10.70 8.80 -11 -12 0 35.40 9.00 -11 -12 -1 48.20 10.50 11 -13 -3 -1.50 10.00 -11 -13 3 4.70 7.30 -11 -13 2 0.40 7.30 11 -13 -2 17.80 9.80 -11 -13 1 23.90 8.70 11 -13 -1 36.90 10.00 -11 -13 0 2.90 8.50 -12 0 6 23.80 8.90 -12 0 5 11.00 7.90 -12 0 4 214.58 15.90 -12 0 3 -0.40 5.70 -12 0 2 60.59 8.00 -12 0 1 -1.40 4.90 -12 0 0 65.49 7.90 -12 0 -1 10.70 5.00 -12 0 -2 -3.20 5.20 -12 1 6 15.00 9.60 12 -1 -6 -0.30 8.00 -12 -1 6 5.40 8.60 -12 1 5 7.90 7.90 -12 -1 5 -7.80 7.00 -12 1 4 4.60 7.30 -12 -1 4 6.50 7.00 -12 1 3 53.29 8.70 -12 -1 3 45.20 8.30 -12 1 2 14.60 6.00 -12 -1 2 5.20 5.90 -12 1 1 5.80 5.10 -12 -1 1 -0.90 4.90 -12 1 0 0.30 5.20 -12 -1 0 6.60 5.30 -12 1 -1 11.60 5.40 -12 -1 -1 16.20 5.60 -12 1 -2 53.29 7.10 -12 -1 -2 69.49 9.10 -12 -2 6 12.40 8.70 12 -2 -6 9.00 8.90 -12 2 5 13.60 8.60 12 -2 -5 10.00 7.80 -12 -2 5 9.00 7.50 -12 2 4 95.69 13.00 -12 -2 4 113.89 12.70 -12 2 3 27.10 7.20 -12 -2 3 32.50 7.60 -12 2 2 8.90 5.70 -12 -2 2 9.60 5.60 -12 2 1 10.30 5.80 -12 -2 1 0.20 5.20 -12 2 0 6.80 5.50 -12 -2 0 -3.20 4.70 -12 2 -1 52.29 7.30 -12 -2 -1 49.40 7.10 -12 -2 -2 12.80 5.40 -12 -3 6 147.89 16.10 12 -3 -6 118.59 15.80 12 -3 -5 15.30 8.30 -12 -3 5 14.00 7.30 -12 3 4 53.89 9.90 -12 -3 4 46.30 8.10 12 -3 -4 32.60 8.90 -12 3 3 217.68 15.70 -12 -3 3 189.48 14.30 -12 3 2 7.10 6.10 -12 -3 2 7.80 5.70 -12 3 1 1.20 5.50 -12 -3 1 10.40 5.10 -12 3 0 39.00 7.00 -12 -3 0 22.80 5.70 -12 3 -1 5.70 5.40 -12 -3 -1 4.60 5.40 -12 -3 -2 38.10 7.10 12 -4 -6 51.19 10.70 -12 -4 6 61.59 10.90 12 -4 -5 -0.90 8.00 -12 -4 5 3.10 7.00 12 -4 -4 36.30 8.60 -12 -4 4 32.20 7.10 -12 4 3 -2.20 7.00 -12 -4 3 -2.50 5.90 12 -4 -3 2.40 6.80 -12 4 2 90.69 11.50 -12 -4 2 98.19 10.30 -12 4 1 -1.20 5.80 -12 -4 1 10.10 5.50 -12 4 0 6.90 5.90 -12 -4 0 -3.60 4.90 -12 4 -1 -4.10 5.70 -12 -4 -1 6.40 5.60 -12 -4 -2 2.60 5.50 -12 -5 6 1.30 8.30 12 -5 -6 6.20 9.30 -12 -5 5 68.79 9.60 12 -5 -5 83.89 11.70 -12 -5 4 10.50 6.20 12 -5 -4 4.60 7.90 12 -5 -3 82.99 10.50 -12 -5 3 77.69 9.40 -12 -5 2 33.70 6.90 12 -5 -2 21.10 7.60 -12 5 1 70.39 9.40 -12 -5 1 59.29 7.90 12 -5 -1 63.09 9.20 -12 5 0 3.40 6.20 -12 -5 0 3.90 5.50 -12 -5 -1 77.79 10.10 -12 -5 -2 27.10 6.80 -12 -6 6 3.80 8.00 12 -6 -5 3.90 9.70 -12 -6 5 0.30 7.30 -12 -6 4 3.60 6.50 12 -6 -4 7.50 8.40 12 -6 -3 124.19 14.80 -12 -6 3 116.59 11.80 12 -6 -2 52.09 9.30 -12 -6 2 60.19 8.30 -12 -6 1 4.60 5.80 12 -6 -1 1.00 7.20 -12 -6 0 15.30 6.00 -12 -6 -1 65.09 8.50 12 -6 1 66.59 10.50 -12 -6 -2 65.09 9.20 -12 -7 5 4.60 6.60 12 -7 -5 1.10 8.90 -12 -7 4 115.19 12.40 12 -7 -4 111.49 13.80 12 -7 -3 -8.80 8.30 -12 -7 3 3.20 5.90 12 -7 -2 1.90 7.90 -12 -7 2 3.90 6.30 -12 -7 1 11.70 6.10 12 -7 -1 0.20 7.80 -12 -7 0 21.10 6.80 -12 -7 -1 75.99 9.60 12 -8 -5 129.19 15.90 -12 -8 5 149.59 14.50 -12 -8 4 -1.10 6.80 12 -8 -4 12.50 9.80 -12 -8 3 8.50 6.70 12 -8 -3 -0.10 8.70 -12 -8 2 101.49 11.60 12 -8 -2 117.79 15.10 -12 -8 1 83.49 10.00 12 -8 -1 73.79 10.60 -12 -8 0 8.10 8.70 -12 -8 -1 20.10 8.10 -12 -9 4 13.10 7.20 12 -9 -4 11.70 10.70 12 -9 -3 5.10 9.40 -12 -9 3 8.90 6.90 -12 -9 2 -3.50 6.00 12 -9 -2 6.90 9.00 12 -9 -1 72.19 11.40 -12 -9 1 71.09 9.90 -12 -9 0 31.20 8.60 -12 -10 3 60.49 9.50 12 -10 -3 48.60 11.60 -12 -10 2 80.49 10.20 12 -10 -2 109.79 13.30 -12 -10 1 5.30 7.70 12 -10 -1 -2.80 9.20 -13 0 4 2.40 7.80 -13 0 3 8.30 7.30 -13 0 2 45.50 8.20 -13 0 1 -6.00 6.20 -13 0 0 103.69 11.70 -13 1 4 7.00 7.80 -13 -1 4 2.50 8.00 -13 1 3 18.50 11.00 -13 -1 3 11.20 7.10 -13 1 2 67.99 9.70 -13 -1 2 64.99 8.90 -13 1 1 4.00 6.80 -13 -1 1 9.10 6.40 -13 1 0 43.50 7.60 -13 -1 0 32.10 7.20 -13 2 4 16.80 8.50 -13 -2 4 9.60 7.50 -13 2 3 28.10 8.20 -13 -2 3 48.10 8.80 -13 2 2 11.20 7.20 -13 -2 2 5.50 6.20 -13 2 1 72.19 9.70 -13 -2 1 57.59 8.30 -13 2 0 7.90 6.50 -13 -2 0 13.30 6.30 -13 3 4 18.30 9.40 13 -3 -4 31.00 9.60 -13 -3 4 22.80 8.20 -13 3 3 8.40 8.50 -13 -3 3 -1.10 6.80 -13 3 2 -7.40 7.00 -13 -3 2 2.80 6.30 -13 3 1 -4.30 6.60 -13 -3 1 -8.00 5.80 -13 3 0 0.60 6.60 -13 -3 0 0.70 6.10 13 -4 -4 4.20 8.70 -13 -4 4 17.30 7.50 -13 4 3 16.40 8.30 -13 -4 3 8.10 6.70 13 -4 -3 35.30 9.20 -13 4 2 18.40 8.30 13 -4 -2 3.70 8.10 -13 -4 2 5.90 6.50 -13 4 1 4.10 7.70 -13 -4 1 22.80 6.90 -13 4 0 31.60 8.30 -13 -4 0 30.00 7.10 -13 -5 3 -1.10 6.30 13 -5 -3 17.80 8.80 13 -5 -2 29.40 9.30 -13 -5 2 11.70 6.50 -13 -5 1 91.49 11.80 13 -5 -1 101.59 11.90 -13 -6 2 -8.50 6.30 13 -6 -2 -16.00 8.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 78097 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 C1 C 0.36703(16) 0.43811(9) 0.25141(19) 0.0250(4) Uani 1 1 d . . . . . C2 C 0.49329(16) 0.40701(9) 0.28067(19) 0.0251(4) Uani 1 1 d . . . . . C3 C 0.52359(16) 0.39574(9) 0.4479(2) 0.0245(3) Uani 1 1 d . . . . . C4 C 0.39302(17) 0.41407(9) 0.66839(19) 0.0261(4) Uani 1 1 d . . . . . H4B H 0.475948 0.425565 0.746016 0.039 Uiso 1 1 d R U . . . H4A H 0.326148 0.452765 0.672116 0.039 Uiso 1 1 d R U . . . C5 C 0.34666(16) 0.33924(9) 0.69904(19) 0.0235(3) Uani 1 1 d . . . . . C6 C 0.22522(16) 0.24803(9) 0.6869(2) 0.0265(4) Uani 1 1 d . . . . . K1 K -0.28284(4) 0.20087(3) 0.38314(5) 0.04055(13) Uani 1 1 d . . . . . K2 K 0.03693(4) 0.39669(2) 0.40841(5) 0.03742(13) Uani 1 1 d . . . . . N1 N 0.31873(13) 0.44512(8) 0.38342(16) 0.0260(3) Uani 1 1 d . . . . . N2 N 0.41663(13) 0.41992(8) 0.50269(15) 0.0233(3) Uani 1 1 d . . . . . N3 N 0.22523(13) 0.31404(8) 0.62708(17) 0.0264(3) Uani 1 1 d . . . . . N4 N 0.42061(14) 0.29470(8) 0.79655(19) 0.0339(4) Uani 1 1 d . . . . . N5 N 0.28108(15) 0.45687(10) 0.09840(18) 0.0363(4) Uani 1 1 d . . . . . N6 N 0.56984(14) 0.38460(8) 0.16598(17) 0.0297(3) Uani 1 1 d . . . . . N7 N 0.62458(14) 0.36606(9) 0.55913(17) 0.0318(3) Uani 1 1 d . . . . . N8 N 0.74439(14) 0.37960(9) 0.53294(19) 0.0332(4) Uani 1 1 d . . . . . N9 N 0.13921(15) 0.19194(8) 0.6766(2) 0.0355(4) Uani 1 1 d . . . . . N10 N 0.02656(16) 0.19853(9) 0.5693(2) 0.0387(4) Uani 1 1 d . . . . . O1 O 0.20339(18) 0.50590(11) 0.0977(2) 0.0722(6) Uani 1 1 d . . . . . O2 O 0.29193(16) 0.42154(10) -0.01957(16) 0.0554(4) Uani 1 1 d . . . . . O3 O 0.57075(14) 0.42271(8) 0.04733(16) 0.0442(3) Uani 1 1 d . . . . . O4 O 0.63043(15) 0.32706(8) 0.19055(17) 0.0457(4) Uani 1 1 d . . . . . O5 O 0.76700(12) 0.41987(8) 0.42312(16) 0.0415(3) Uani 1 1 d . . . . . O6 O 0.83673(14) 0.34956(10) 0.63013(19) 0.0569(4) Uani 1 1 d . . . . . O7 O 0.33948(12) 0.23226(7) 0.79129(17) 0.0375(3) Uani 1 1 d . . . . . O8 O -0.05643(16) 0.14997(10) 0.5782(2) 0.0680(5) Uani 1 1 d . . . . . O9 O 0.00235(14) 0.24665(8) 0.46565(18) 0.0518(4) Uani 1 1 d . . . . . O10 O 0.03895(15) 0.46611(9) 0.71860(18) 0.0527(4) Uani 1 1 d . . . . . H10A H 0.094546 0.468180 0.804370 0.079 Uiso 1 1 d R U . . . H10B H -0.020654 0.432880 0.733970 0.079 Uiso 1 1 d 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 C1 0.0285(9) 0.0238(9) 0.0229(8) 0.0000(7) 0.0056(6) -0.0022(7) C2 0.0268(8) 0.0243(9) 0.0260(8) -0.0011(7) 0.0093(7) -0.0020(7) C3 0.0240(8) 0.0232(8) 0.0270(8) 0.0005(7) 0.0067(6) -0.0034(7) C4 0.0317(9) 0.0266(9) 0.0209(8) -0.0014(7) 0.0078(7) -0.0038(7) C5 0.0234(8) 0.0270(9) 0.0216(8) -0.0009(7) 0.0080(6) 0.0007(7) C6 0.0225(8) 0.0279(9) 0.0295(8) 0.0033(7) 0.0063(7) 0.0026(7) K1 0.0352(2) 0.0525(3) 0.0327(2) 0.00248(19) 0.00398(17) -0.00057(19) K2 0.0293(2) 0.0380(2) 0.0440(2) -0.00150(18) 0.00515(17) 0.00812(17) N1 0.0259(7) 0.0267(8) 0.0252(7) -0.0004(6) 0.0045(6) -0.0008(6) N2 0.0236(7) 0.0257(7) 0.0211(7) 0.0001(5) 0.0055(5) -0.0021(6) N3 0.0252(7) 0.0258(8) 0.0277(7) 0.0024(6) 0.0041(6) -0.0009(6) N4 0.0253(7) 0.0311(8) 0.0432(9) 0.0074(7) 0.0019(6) -0.0040(6) N5 0.0315(8) 0.0503(10) 0.0272(8) 0.0057(7) 0.0065(6) 0.0027(7) N6 0.0306(8) 0.0323(9) 0.0277(7) -0.0005(6) 0.0094(6) -0.0017(7) N7 0.0228(7) 0.0408(9) 0.0318(8) 0.0067(7) 0.0057(6) -0.0015(6) N8 0.0248(8) 0.0390(9) 0.0361(8) 0.0005(7) 0.0067(6) 0.0017(7) N9 0.0287(8) 0.0314(9) 0.0437(9) 0.0075(7) 0.0005(7) -0.0044(6) N10 0.0348(9) 0.0347(9) 0.0437(9) 0.0052(7) 0.0004(7) -0.0072(7) O1 0.0686(11) 0.0984(14) 0.0486(9) 0.0162(9) 0.0088(8) 0.0523(11) O2 0.0589(10) 0.0801(12) 0.0255(7) -0.0085(7) 0.0041(6) 0.0040(8) O3 0.0507(8) 0.0529(9) 0.0342(7) 0.0125(6) 0.0210(6) 0.0013(7) O4 0.0576(9) 0.0399(8) 0.0445(8) 0.0019(6) 0.0218(7) 0.0179(7) O5 0.0301(7) 0.0519(9) 0.0454(8) 0.0119(7) 0.0148(6) -0.0027(6) O6 0.0281(7) 0.0808(12) 0.0600(10) 0.0253(9) 0.0046(7) 0.0135(7) O7 0.0261(6) 0.0298(7) 0.0528(8) 0.0137(6) -0.0015(6) -0.0019(5) O8 0.0466(9) 0.0632(11) 0.0818(12) 0.0295(9) -0.0172(8) -0.0313(8) O9 0.0487(8) 0.0464(9) 0.0514(9) 0.0175(7) -0.0118(7) -0.0130(7) O10 0.0487(9) 0.0585(10) 0.0468(8) 0.0065(7) -0.0001(7) -0.0026(7) 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' K K 0.2009 0.2494 '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 N1 C1 C2 112.95(14) . . ? N1 C1 N5 117.21(15) . . ? C2 C1 N5 129.58(15) . . ? C3 C2 C1 104.63(14) . . ? C3 C2 N6 126.59(15) . . ? C1 C2 N6 128.51(15) . . ? N2 C3 N7 117.53(15) . . ? N2 C3 C2 105.01(14) . . ? N7 C3 C2 137.40(16) . . ? N2 C4 C5 110.57(13) . . ? N2 C4 H4B 108.9 . . ? C5 C4 H4B 110.3 . . ? N2 C4 H4A 103.0 . . ? C5 C4 H4A 113.6 . . ? H4B C4 H4A 110.1 . . ? N4 C5 N3 116.37(15) . . ? N4 C5 C4 121.30(15) . . ? N3 C5 C4 122.32(15) . . ? N3 C6 N9 136.76(16) . . ? N3 C6 O7 112.25(14) . . ? N9 C6 O7 110.93(14) . . ? O8 K1 O6 83.62(6) . 4_465 ? O8 K1 O4 138.37(5) . 1_455 ? O6 K1 O4 88.49(5) 4_465 1_455 ? O8 K1 O4 77.81(5) . 4_466 ? O6 K1 O4 149.40(5) 4_465 4_466 ? O4 K1 O4 121.39(4) 1_455 4_466 ? O8 K1 N7 119.33(5) . 4_465 ? O6 K1 N7 44.13(4) 4_465 4_465 ? O4 K1 N7 78.90(4) 1_455 4_465 ? O4 K1 N7 129.40(4) 4_466 4_465 ? O8 K1 N4 149.56(5) . 4_465 ? O6 K1 N4 113.89(4) 4_465 4_465 ? O4 K1 N4 69.61(4) 1_455 4_465 ? O4 K1 N4 75.13(4) 4_466 4_465 ? N7 K1 N4 70.21(4) 4_465 4_465 ? O8 K1 O9 43.62(4) . . ? O6 K1 O9 73.07(4) 4_465 . ? O4 K1 O9 95.03(4) 1_455 . ? O4 K1 O9 107.55(4) 4_466 . ? N7 K1 O9 116.70(4) 4_465 . ? N4 K1 O9 162.28(4) 4_465 . ? O8 K1 O3 85.53(4) . 4_466 ? O6 K1 O3 114.25(4) 4_465 4_466 ? O4 K1 O3 134.14(4) 1_455 4_466 ? O4 K1 O3 40.75(4) 4_466 4_466 ? N7 K1 O3 90.51(4) 4_465 4_466 ? N4 K1 O3 64.84(4) 4_465 4_466 ? O9 K1 O3 128.76(4) . 4_466 ? O8 K1 N8 99.47(5) . 4_465 ? O6 K1 N8 21.26(4) 4_465 4_465 ? O4 K1 N8 86.03(4) 1_455 4_465 ? O4 K1 N8 141.93(4) 4_466 4_465 ? N7 K1 N8 23.17(4) 4_465 4_465 ? N4 K1 N8 93.37(4) 4_465 4_465 ? O9 K1 N8 94.33(4) . 4_465 ? O3 K1 N8 101.37(4) 4_466 4_465 ? O8 K1 N6 82.81(4) . 4_466 ? O6 K1 N6 133.76(5) 4_465 4_466 ? O4 K1 N6 128.73(4) 1_455 4_466 ? O4 K1 N6 20.18(4) 4_466 4_466 ? N7 K1 N6 109.81(4) 4_465 4_466 ? N4 K1 N6 67.04(4) 4_465 4_466 ? O9 K1 N6 121.00(4) . 4_466 ? O3 K1 N6 20.72(3) 4_466 4_466 ? N8 K1 N6 122.09(4) 4_465 4_466 ? O8 K1 K1 74.95(5) . 4_566 ? O6 K1 K1 154.47(3) 4_465 4_566 ? O4 K1 K1 98.29(3) 1_455 4_566 ? O4 K1 K1 37.45(3) 4_466 4_566 ? N7 K1 K1 161.38(3) 4_465 4_566 ? N4 K1 K1 91.47(3) 4_465 4_566 ? O9 K1 K1 81.80(3) . 4_566 ? O3 K1 K1 78.19(2) 4_466 4_566 ? N8 K1 K1 174.41(3) 4_465 4_566 ? N6 K1 K1 57.60(3) 4_466 4_566 ? O8 K1 K1 121.86(4) . 4_565 ? O6 K1 K1 49.91(4) 4_465 4_565 ? O4 K1 K1 38.68(3) 1_455 4_565 ? O4 K1 K1 158.59(3) 4_466 4_565 ? N7 K1 K1 51.55(3) 4_465 4_565 ? N4 K1 K1 87.31(3) 4_465 4_565 ? O9 K1 K1 85.59(3) . 4_565 ? O3 K1 K1 139.87(3) 4_466 4_565 ? N8 K1 K1 49.56(3) 4_465 4_565 ? N6 K1 K1 153.40(3) 4_466 4_565 ? K1 K1 K1 133.60(2) 4_566 4_565 ? O10 K2 O9 155.33(4) 3_566 . ? O10 K2 N3 146.74(4) 3_566 . ? O9 K2 N3 57.58(4) . . ? O10 K2 O5 71.21(4) 3_566 1_455 ? O9 K2 O5 88.83(4) . 1_455 ? N3 K2 O5 127.15(4) . 1_455 ? O10 K2 O8 83.33(5) 3_566 4_565 ? O9 K2 O8 81.12(5) . 4_565 ? N3 K2 O8 121.42(4) . 4_565 ? O5 K2 O8 86.69(4) 1_455 4_565 ? O10 K2 N9 111.23(5) 3_566 4_565 ? O9 K2 N9 69.14(5) . 4_565 ? N3 K2 N9 80.82(4) . 4_565 ? O5 K2 N9 127.23(4) 1_455 4_565 ? O8 K2 N9 44.13(4) 4_565 4_565 ? O10 K2 O10 84.22(5) 3_566 . ? O9 K2 O10 104.64(5) . . ? N3 K2 O10 76.72(4) . . ? O5 K2 O10 74.20(4) 1_455 . ? O8 K2 O10 159.75(4) 4_565 . ? N9 K2 O10 156.09(4) 4_565 . ? O10 K2 N1 84.97(4) 3_566 . ? O9 K2 N1 116.33(4) . . ? N3 K2 N1 70.26(4) . . ? O5 K2 N1 154.71(4) 1_455 . ? O8 K2 N1 99.20(5) 4_565 . ? N9 K2 N1 68.91(4) 4_565 . ? O10 K2 N1 95.54(4) . . ? O10 K2 O6 107.72(4) 3_566 1_455 ? O9 K2 O6 61.00(5) . 1_455 ? N3 K2 O6 85.31(4) . 1_455 ? O5 K2 O6 41.85(4) 1_455 1_455 ? O8 K2 O6 110.63(5) 4_565 1_455 ? N9 K2 O6 127.73(5) 4_565 1_455 ? O10 K2 O6 58.62(5) . 1_455 ? N1 K2 O6 148.51(4) . 1_455 ? O10 K2 N10 100.77(4) 3_566 4_565 ? O9 K2 N10 69.61(5) . 4_565 ? N3 K2 N10 100.14(4) . 4_565 ? O5 K2 N10 104.49(4) 1_455 4_565 ? O8 K2 N10 21.74(4) 4_565 4_565 ? N9 K2 N10 23.39(4) 4_565 4_565 ? O10 K2 N10 174.21(5) . 4_565 ? N1 K2 N10 87.88(4) . 4_565 ? O6 K2 N10 116.57(5) 1_455 4_565 ? O10 K2 N8 90.05(4) 3_566 1_455 ? O9 K2 N8 73.03(4) . 1_455 ? N3 K2 N8 106.82(4) . 1_455 ? O5 K2 N8 20.48(4) 1_455 1_455 ? O8 K2 N8 96.91(5) 4_565 1_455 ? N9 K2 N8 128.39(4) 4_565 1_455 ? O10 K2 N8 67.18(4) . 1_455 ? N1 K2 N8 162.45(4) . 1_455 ? O6 K2 N8 21.60(3) 1_455 1_455 ? N10 K2 N8 109.61(4) 4_565 1_455 ? O10 K2 K2 43.15(3) 3_566 3_566 ? O9 K2 K2 140.70(4) . 3_566 ? N3 K2 K2 113.22(3) . 3_566 ? O5 K2 K2 66.43(3) 1_455 3_566 ? O8 K2 K2 124.62(4) 4_565 3_566 ? N9 K2 K2 150.17(4) 4_565 3_566 ? O10 K2 K2 41.07(3) . 3_566 ? N1 K2 K2 90.48(3) . 3_566 ? O6 K2 K2 80.98(4) 1_455 3_566 ? N10 K2 K2 143.83(3) 4_565 3_566 ? N8 K2 K2 74.57(3) 1_455 3_566 ? O10 K2 H10B 93.3 3_566 . ? O9 K2 H10B 90.3 . . ? N3 K2 H10B 76.2 . . ? O5 K2 H10B 63.4 1_455 . ? O8 K2 H10B 149.1 4_565 . ? N9 K2 H10B 155.1 4_565 . ? O10 K2 H10B 17.4 . . ? N1 K2 H10B 111.1 . . ? O6 K2 H10B 41.4 1_455 . ? N10 K2 H10B 157.4 4_565 . ? N8 K2 H10B 52.3 1_455 . ? K2 K2 H10B 51.9 3_566 . ? C1 N1 N2 103.77(13) . . ? C1 N1 K2 123.51(10) . . ? N2 N1 K2 115.29(9) . . ? C3 N2 N1 113.61(13) . . ? C3 N2 C4 126.93(14) . . ? N1 N2 C4 119.11(13) . . ? C6 N3 C5 102.31(14) . . ? C6 N3 K2 133.59(11) . . ? C5 N3 K2 124.10(11) . . ? C5 N4 O7 102.61(13) . . ? C5 N4 K1 125.59(11) . 4_666 ? O7 N4 K1 126.81(9) . 4_666 ? O1 N5 O2 124.52(17) . . ? O1 N5 C1 118.12(16) . . ? O2 N5 C1 117.36(16) . . ? O3 N6 O4 123.04(15) . . ? O3 N6 C2 118.95(15) . . ? O4 N6 C2 118.00(14) . . ? O3 N6 K1 67.66(9) . 4_665 ? O4 N6 K1 56.11(9) . 4_665 ? C2 N6 K1 168.49(11) . 4_665 ? N8 N7 C3 115.12(14) . . ? N8 N7 K1 95.04(10) . 4_666 ? C3 N7 K1 148.73(11) . 4_666 ? O5 N8 O6 120.96(15) . . ? O5 N8 N7 123.80(15) . . ? O6 N8 N7 115.22(15) . . ? O5 N8 K1 167.51(12) . 4_666 ? O6 N8 K1 54.62(9) . 4_666 ? N7 N8 K1 61.79(9) . 4_666 ? O5 N8 K2 53.58(8) . 1_655 ? O6 N8 K2 68.43(10) . 1_655 ? N7 N8 K2 170.29(12) . 1_655 ? K1 N8 K2 122.99(5) 4_666 1_655 ? N10 N9 C6 116.83(15) . . ? N10 N9 K2 96.85(10) . 4_566 ? C6 N9 K2 135.10(12) . 4_566 ? O9 N10 O8 120.52(15) . . ? O9 N10 N9 124.97(15) . . ? O8 N10 N9 114.49(15) . . ? O9 N10 K2 161.94(14) . 4_566 ? O8 N10 K2 58.68(10) . 4_566 ? N9 N10 K2 59.75(9) . 4_566 ? N6 O3 K1 91.63(10) . 4_665 ? N6 O4 K1 152.19(11) . 1_655 ? N6 O4 K1 103.71(10) . 4_665 ? K1 O4 K1 103.87(4) 1_655 4_665 ? N8 O5 K2 105.94(10) . 1_655 ? N8 O6 K1 104.11(11) . 4_666 ? N8 O6 K2 89.97(10) . 1_655 ? K1 O6 K2 165.62(5) 4_666 1_655 ? C6 O7 N4 106.45(12) . . ? N10 O8 K1 103.71(11) . . ? N10 O8 K2 99.58(11) . 4_566 ? K1 O8 K2 139.47(8) . 4_566 ? N10 O9 K2 143.45(12) . . ? N10 O9 K1 90.89(10) . . ? K2 O9 K1 112.52(5) . . ? K2 O10 K2 95.78(5) 3_566 . ? K2 O10 H10A 112.7 3_566 . ? K2 O10 H10A 133.0 . . ? K2 O10 H10B 121.4 3_566 . ? K2 O10 H10B 87.1 . . ? H10A O10 H10B 106.5 . . ? 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 C1 N1 1.310(2) . ? C1 C2 1.401(2) . ? C1 N5 1.452(2) . ? C2 C3 1.393(2) . ? C2 N6 1.424(2) . ? C3 N2 1.354(2) . ? C3 N7 1.368(2) . ? C4 N2 1.464(2) . ? C4 C5 1.492(2) . ? C4 H4B 0.9915 . ? C4 H4A 0.9953 . ? C5 N4 1.294(2) . ? C5 N3 1.362(2) . ? C6 N3 1.310(2) . ? C6 N9 1.351(2) . ? C6 O7 1.356(2) . ? K1 O8 2.7412(16) . ? K1 O6 2.8188(16) 4_465 ? K1 O4 2.8625(15) 1_455 ? K1 O4 2.9424(14) 4_466 ? K1 N7 2.9660(15) 4_465 ? K1 N4 3.0090(15) 4_465 ? K1 O9 3.0116(15) . ? K1 O3 3.1864(15) 4_466 ? K1 N8 3.3528(16) 4_465 ? K1 N6 3.4438(15) 4_466 ? K1 K1 4.5707(4) 4_566 ? K1 K1 4.5707(4) 4_565 ? K2 O10 2.7829(16) 3_566 ? K2 O9 2.8262(15) . ? K2 N3 2.8356(14) . ? K2 O5 2.8504(13) 1_455 ? K2 O8 2.8803(17) 4_565 ? K2 N9 2.8927(16) 4_565 ? K2 O10 2.8966(16) . ? K2 N1 3.0930(14) . ? K2 O6 3.1677(15) 1_455 ? K2 N10 3.3247(17) 4_565 ? K2 N8 3.4061(16) 1_455 ? K2 K2 4.2141(9) 3_566 ? K2 H10B 2.9873 . ? N1 N2 1.3563(19) . ? N4 O7 1.4143(19) . ? N5 O1 1.205(2) . ? N5 O2 1.208(2) . ? N6 O3 1.2187(19) . ? N6 O4 1.223(2) . ? N7 N8 1.324(2) . ? N8 O5 1.239(2) . ? N8 O6 1.254(2) . ? N9 N10 1.330(2) . ? N10 O9 1.230(2) . ? N10 O8 1.249(2) . ? O10 H10A 0.8287 . ? O10 H10B 0.8939 . ? 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 _geom_hbond_publ_flag C4 H4B O3 0.99 2.53 3.349(2) 140.1 1_556 yes C4 H4A O5 1.00 2.59 3.476(2) 148.3 3_666 yes O10 H10A O1 0.83 2.59 3.379(2) 159.1 1_556 yes O10 H10A O2 0.83 2.43 3.173(2) 150.3 1_556 yes 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 N1 C1 C2 C3 -1.18(19) . . . . ? N5 C1 C2 C3 -175.22(17) . . . . ? N1 C1 C2 N6 173.06(16) . . . . ? N5 C1 C2 N6 -1.0(3) . . . . ? C1 C2 C3 N2 0.20(17) . . . . ? N6 C2 C3 N2 -174.18(15) . . . . ? C1 C2 C3 N7 177.19(19) . . . . ? N6 C2 C3 N7 2.8(3) . . . . ? N2 C4 C5 N4 110.22(18) . . . . ? N2 C4 C5 N3 -69.89(19) . . . . ? C2 C1 N1 N2 1.60(19) . . . . ? N5 C1 N1 N2 176.45(14) . . . . ? C2 C1 N1 K2 -132.01(12) . . . . ? N5 C1 N1 K2 42.8(2) . . . . ? N7 C3 N2 N1 -176.91(14) . . . . ? C2 C3 N2 N1 0.80(18) . . . . ? N7 C3 N2 C4 -3.8(2) . . . . ? C2 C3 N2 C4 173.86(15) . . . . ? C1 N1 N2 C3 -1.49(18) . . . . ? K2 N1 N2 C3 136.62(11) . . . . ? C1 N1 N2 C4 -175.14(14) . . . . ? K2 N1 N2 C4 -37.04(16) . . . . ? C5 C4 N2 C3 -79.1(2) . . . . ? C5 C4 N2 N1 93.60(17) . . . . ? N9 C6 N3 C5 177.3(2) . . . . ? O7 C6 N3 C5 0.30(18) . . . . ? N9 C6 N3 K2 -2.0(3) . . . . ? O7 C6 N3 K2 -179.06(11) . . . . ? N4 C5 N3 C6 0.21(19) . . . . ? C4 C5 N3 C6 -179.69(15) . . . . ? N4 C5 N3 K2 179.65(12) . . . . ? C4 C5 N3 K2 -0.2(2) . . . . ? N3 C5 N4 O7 -0.58(19) . . . . ? C4 C5 N4 O7 179.31(14) . . . . ? N3 C5 N4 K1 155.64(11) . . . 4_666 ? C4 C5 N4 K1 -24.5(2) . . . 4_666 ? N1 C1 N5 O1 33.9(2) . . . . ? C2 C1 N5 O1 -152.2(2) . . . . ? N1 C1 N5 O2 -145.44(17) . . . . ? C2 C1 N5 O2 28.4(3) . . . . ? C3 C2 N6 O3 -146.35(17) . . . . ? C1 C2 N6 O3 40.6(3) . . . . ? C3 C2 N6 O4 34.7(2) . . . . ? C1 C2 N6 O4 -138.37(18) . . . . ? C3 C2 N6 K1 91.0(6) . . . 4_665 ? C1 C2 N6 K1 -82.0(6) . . . 4_665 ? N2 C3 N7 N8 -144.45(16) . . . . ? C2 C3 N7 N8 38.8(3) . . . . ? N2 C3 N7 K1 19.1(3) . . . 4_666 ? C2 C3 N7 K1 -157.65(17) . . . 4_666 ? C3 N7 N8 O5 4.5(3) . . . . ? K1 N7 N8 O5 -166.96(15) 4_666 . . . ? C3 N7 N8 O6 -176.70(16) . . . . ? K1 N7 N8 O6 11.80(17) 4_666 . . . ? C3 N7 N8 K1 171.50(17) . . . 4_666 ? N3 C6 N9 N10 7.5(3) . . . . ? O7 C6 N9 N10 -175.42(16) . . . . ? N3 C6 N9 K2 -126.65(19) . . . 4_566 ? O7 C6 N9 K2 50.4(2) . . . 4_566 ? C6 N9 N10 O9 9.9(3) . . . . ? K2 N9 N10 O9 159.26(18) 4_566 . . . ? C6 N9 N10 O8 -171.40(18) . . . . ? K2 N9 N10 O8 -22.04(19) 4_566 . . . ? C6 N9 N10 K2 -149.35(18) . . . 4_566 ? O4 N6 O3 K1 9.39(17) . . . 4_665 ? C2 N6 O3 K1 -169.53(13) . . . 4_665 ? O3 N6 O4 K1 177.01(18) . . . 1_655 ? C2 N6 O4 K1 -4.1(3) . . . 1_655 ? K1 N6 O4 K1 -172.5(3) 4_665 . . 1_655 ? O3 N6 O4 K1 -10.47(19) . . . 4_665 ? C2 N6 O4 K1 168.46(12) . . . 4_665 ? O6 N8 O5 K2 12.8(2) . . . 1_655 ? N7 N8 O5 K2 -168.57(14) . . . 1_655 ? K1 N8 O5 K2 78.3(5) 4_666 . . 1_655 ? O5 N8 O6 K1 166.03(14) . . . 4_666 ? N7 N8 O6 K1 -12.76(18) . . . 4_666 ? K2 N8 O6 K1 177.04(10) 1_655 . . 4_666 ? O5 N8 O6 K2 -11.01(17) . . . 1_655 ? N7 N8 O6 K2 170.20(14) . . . 1_655 ? K1 N8 O6 K2 -177.04(10) 4_666 . . 1_655 ? N3 C6 O7 N4 -0.65(19) . . . . ? N9 C6 O7 N4 -178.46(14) . . . . ? C5 N4 O7 C6 0.71(18) . . . . ? K1 N4 O7 C6 -155.12(11) 4_666 . . . ? O9 N10 O8 K1 -12.4(2) . . . . ? N9 N10 O8 K1 168.89(13) . . . . ? K2 N10 O8 K1 146.58(13) 4_566 . . . ? O9 N10 O8 K2 -158.93(16) . . . 4_566 ? N9 N10 O8 K2 22.30(19) . . . 4_566 ? O8 N10 O9 K2 142.54(19) . . . . ? N9 N10 O9 K2 -38.8(3) . . . . ? K2 N10 O9 K2 60.5(5) 4_566 . . . ? O8 N10 O9 K1 10.9(2) . . . . ? N9 N10 O9 K1 -170.47(18) . . . . ? K2 N10 O9 K1 -71.1(4) 4_566 . . . ?