#------------------------------------------------------------------------------ #$Date: 2024-01-06 11:53:54 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288906 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247689.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_7247689 loop_ _publ_author_name 'Atceken, Nurunnisa' 'Hemingway, Jack' 'Bull, Craig L.' 'Liu, Xiaojiao' 'Michalchuk, Adam A. L.' 'Konar, Sumit' 'Morrison, Carole A.' 'Pulham, Colin R.' _publ_section_title ; High-pressure structural studies and pressure-induced sensitisation of 3,4,5-trinitro-1H-pyrazole. ; _journal_issue 46 _journal_name_full 'Physical chemistry chemical physics : PCCP' _journal_page_first 31646 _journal_page_last 31654 _journal_paper_doi 10.1039/d3cp04526a _journal_volume 25 _journal_year 2023 _chemical_formula_moiety '6(C3 H N5 O6)' _chemical_formula_sum 'C18 H6 N30 O36' _chemical_formula_weight 1218.53 _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 _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc29gp1j _audit_creation_date 2021-12-16 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2021-12-16 deposited with the CCDC. 2023-11-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.113(8) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.815(2) _cell_length_b 8.0553(13) _cell_length_c 16.9050(19) _cell_measurement_reflns_used 1840 _cell_measurement_temperature 298.0 _cell_measurement_theta_max 25.19 _cell_measurement_theta_min 2.75 _cell_volume 2016.1(5) _computing_cell_refinement 'SAINT V8.40A (?, 2016)' _computing_data_reduction 'SAINT V8.40A (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 298.0 _diffrn_measured_fraction_theta_full 0.596 _diffrn_measured_fraction_theta_max 0.596 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_unetI/netI 0.0610 _diffrn_reflns_Laue_measured_fraction_full 0.596 _diffrn_reflns_Laue_measured_fraction_max 0.596 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 10884 _diffrn_reflns_point_group_measured_fraction_full 0.596 _diffrn_reflns_point_group_measured_fraction_max 0.596 _diffrn_reflns_theta_full 23.504 _diffrn_reflns_theta_max 23.504 _diffrn_reflns_theta_min 2.411 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.195 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0780 before and 0.0591 after correction. The Ratio of minimum to maximum transmission is 0.8876. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.007 _exptl_crystal_description block _exptl_crystal_F_000 1224 _refine_diff_density_max 0.197 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 391 _refine_ls_number_reflns 1775 _refine_ls_number_restraints 306 _refine_ls_restrained_S_all 0.973 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0488 _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^)+(0.0598P)^2^+2.9315P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1193 _refine_ls_wR_factor_ref 0.1407 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1214 _reflns_number_total 1775 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3cp04526a2.cif _cod_data_source_block 2tnp_p03_p _cod_depositor_comments 'Adding full bibliography for 7247689--7247697.cif.' _cod_original_cell_volume 2016.0(5) _cod_database_code 7247689 _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. ; _olex2_refinement_description ; 1. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 ; _shelx_res_file ; TITL 2tnp_p03_p_a.res in P2(1)/c 2tnp_p03_p.res created by SHELXL-2018/3 at 13:43:34 on 16-Dec-2021 REM Old TITL 2TNP_P03_P in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.209, Rweak 0.005, Alpha 0.118 REM 0.392 for 92 systematic absences, Orientation as input REM Formula found by SHELXT: C32 N O9 CELL 0.71073 14.8148 8.0553 16.905 90 92.113 90 ZERR 2 0.002 0.0013 0.0019 0 0.008 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 36 12 60 72 RIGU L.S. 10 PLAN 5 TEMP 24.85 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT -1 1 8 OMIT -7 1 2 OMIT -4 3 3 OMIT -5 3 1 OMIT -6 2 3 OMIT 6 1 4 OMIT 7 1 1 OMIT 1 1 8 OMIT -2 2 7 OMIT 1 2 7 OMIT -1 2 7 REM REM REM WGHT 0.059800 2.931500 FVAR 0.60896 O001 4 0.683020 0.596442 0.650563 11.00000 0.05724 0.03644 = 0.04916 0.01375 0.00841 -0.00991 O002 4 0.831181 0.598960 0.354198 11.00000 0.06268 0.03808 = 0.05162 -0.01284 0.01411 0.01296 O003 4 0.522936 0.495347 0.812450 11.00000 0.04055 0.05636 = 0.03250 -0.00914 0.00691 0.01920 O004 4 0.662160 0.420766 0.833844 11.00000 0.03468 0.05614 = 0.03545 -0.01124 -0.01146 -0.00131 O005 4 0.925722 0.108414 0.510236 11.00000 0.04387 0.07692 = 0.04641 0.03765 0.00137 -0.00675 O006 4 0.563467 0.126409 0.481259 11.00000 0.05242 0.05596 = 0.04243 -0.02351 -0.00104 0.00545 O007 4 0.979537 0.460475 0.176720 11.00000 0.03590 0.07536 = 0.03486 0.01246 0.00556 -0.01293 O008 4 0.836400 0.410299 0.158381 11.00000 0.03879 0.07993 = 0.03638 0.01917 -0.01187 -0.00588 O009 4 0.828397 0.434091 0.526774 11.00000 0.06416 0.04244 = 0.06907 0.00069 -0.01813 0.02078 O00A 4 1.032861 0.285823 0.494297 11.00000 0.03587 0.07709 = 0.04141 0.01253 -0.01296 -0.01555 O00B 4 0.690347 0.419558 0.484000 11.00000 0.05566 0.03754 = 0.06499 -0.00566 -0.00303 -0.01892 N00C 3 0.687030 0.743693 0.634528 11.00000 0.03210 0.03675 = 0.02906 0.00177 0.00328 -0.00534 O00D 4 0.457057 0.305965 0.499309 11.00000 0.03686 0.07879 = 0.03854 -0.01261 -0.01034 0.01486 O00E 4 0.443951 0.595845 0.655724 11.00000 0.07838 0.04909 = 0.05729 -0.00961 -0.01110 0.03310 N00F 3 0.760828 0.935146 0.464811 11.00000 0.02804 0.02233 = 0.02463 0.00559 0.00274 0.00060 N00G 3 0.844153 0.207945 0.375059 11.00000 0.02676 0.02891 = 0.02747 0.00262 -0.00114 -0.00297 O00H 4 1.121769 0.297283 0.340553 11.00000 0.02560 0.09603 = 0.05543 0.00964 0.00256 0.00839 N00I 3 0.727468 0.941715 0.536262 11.00000 0.02875 0.02949 = 0.02263 0.00118 0.00188 -0.00121 N00J 3 0.832121 0.260586 0.300588 11.00000 0.02591 0.02774 = 0.02568 -0.00321 -0.00467 -0.00146 N00K 3 0.640093 0.202701 0.625905 11.00000 0.02723 0.02843 = 0.02719 -0.00475 0.00451 0.00560 N00L 3 0.814369 0.743418 0.367189 11.00000 0.03535 0.03203 = 0.03025 -0.00316 0.00550 0.00129 N00M 3 0.592141 0.425233 0.793972 11.00000 0.03212 0.02390 = 0.02832 0.00080 0.00208 0.00282 O00N 4 0.372226 0.360861 0.656464 11.00000 0.02736 0.10222 = 0.05335 0.00426 -0.00039 -0.00357 O00O 4 1.070330 0.546059 0.326470 11.00000 0.06586 0.05827 = 0.06337 0.02606 -0.02339 -0.03635 N00P 3 1.061402 0.399673 0.333781 11.00000 0.02720 0.05699 = 0.02717 0.01051 0.00196 -0.00998 N00Q 3 0.660461 0.252152 0.699004 11.00000 0.02740 0.03158 = 0.02318 -0.00295 0.00218 0.00501 O00R 4 0.827170 0.859352 0.322987 11.00000 0.09817 0.04477 = 0.04003 0.00889 0.03519 0.00226 N00S 3 0.439795 0.445839 0.657056 11.00000 0.03351 0.05617 = 0.02056 -0.00308 0.00193 0.01351 O00T 4 0.665021 0.855881 0.676932 11.00000 0.09681 0.04684 = 0.04054 -0.00075 0.03420 0.00911 N00U 3 0.907387 0.406692 0.197227 11.00000 0.02966 0.04301 = 0.02577 0.00391 0.00019 -0.00086 N00V 3 0.757368 0.496378 0.504151 11.00000 0.04350 0.02950 = 0.02785 0.00097 0.00247 0.00036 C00W 1 0.721872 0.785872 0.558480 11.00000 0.01798 0.02601 = 0.02325 0.00353 0.00137 -0.00280 C00X 1 0.777683 0.778291 0.442269 11.00000 0.02492 0.02235 = 0.02398 -0.00158 0.00138 0.00150 C00Y 1 0.905736 0.337544 0.274650 11.00000 0.02649 0.02705 = 0.02406 0.00207 0.00084 0.00124 N00Z 3 0.524863 0.229341 0.519901 11.00000 0.03015 0.04580 = 0.03157 -0.00637 -0.00421 -0.00246 C010 1 0.560515 0.263632 0.598809 11.00000 0.02446 0.02864 = 0.02457 -0.00106 -0.00002 -0.00182 C011 1 0.591106 0.343822 0.718264 11.00000 0.02352 0.02553 = 0.02125 -0.00036 0.00562 -0.00573 N012 3 0.964988 0.211567 0.472798 11.00000 0.02525 0.04806 = 0.02669 0.01092 0.00420 0.00189 C013 1 0.928144 0.251875 0.394083 11.00000 0.02352 0.01644 = 0.03120 0.00396 0.00225 0.00598 C014 1 0.525285 0.356919 0.657738 11.00000 0.01622 0.02588 = 0.02960 0.00094 0.00089 0.00002 C015 1 0.970157 0.332858 0.334224 11.00000 0.01795 0.03285 = 0.02551 0.00254 0.00416 -0.00100 C016 1 0.752489 0.675196 0.501900 11.00000 0.01920 0.02332 = 0.02508 0.00188 0.00183 0.00173 H00J 2 0.776805 0.258878 0.272142 11.00000 0.05293 H00K 2 0.671951 0.130097 0.597545 11.00000 0.01977 H00F 2 0.774551 1.029252 0.437594 11.00000 0.04588 HKLF 4 REM 2tnp_p03_p_a.res in P2(1)/c REM wR2 = 0.1407, GooF = S = 1.053, Restrained GooF = 0.973 for all data REM R1 = 0.0488 for 1214 Fo > 4sig(Fo) and 0.0833 for all 1775 data REM 391 parameters refined using 306 restraints END WGHT 0.0598 2.9317 REM Highest difference peak 0.197, deepest hole -0.218, 1-sigma level 0.046 Q1 1 0.6179 0.5202 0.6005 11.00000 0.05 0.20 Q2 1 0.5578 0.5137 0.8645 11.00000 0.05 0.19 Q3 1 0.9405 0.5588 0.1403 11.00000 0.05 0.17 Q4 1 0.3693 0.3628 0.4585 11.00000 0.05 0.17 Q5 1 0.7840 0.7431 0.2843 11.00000 0.05 0.16 ; _shelx_res_checksum 61388 _shelx_hkl_file ; 2 0 0 326.97 25.80 -2 0 0 351.16 25.70 -3 0 0 145.59 11.60 3 0 0 138.59 11.80 3 0 0 150.08 11.70 -3 0 0 141.09 11.90 -4 0 0 37.00 5.10 4 0 0 42.70 5.00 4 0 0 32.30 4.20 -4 0 0 40.60 5.20 -1 -1 0 173.58 13.60 -1 -1 0 174.38 13.40 1 1 0 166.18 13.40 1 1 0 165.38 13.30 1 1 0 173.78 13.40 1 1 0 174.88 13.50 -2 -1 0 1.30 1.80 -2 -1 0 1.90 1.50 -2 -1 0 2.60 1.60 -2 -1 0 0.90 1.50 -2 -1 0 2.20 1.60 -2 -1 0 1.00 1.40 -2 -1 0 -1.50 1.60 2 1 0 3.00 1.40 2 1 0 -0.20 1.40 2 1 0 1.70 1.30 2 1 0 0.90 1.30 2 1 0 0.00 1.50 2 1 0 2.40 1.40 2 1 0 0.70 1.70 -4 -1 0 68.69 8.50 -4 -1 0 72.69 7.50 -4 -1 0 58.89 7.60 -4 -1 0 76.39 7.70 -4 -1 0 56.19 7.40 4 1 0 66.89 7.50 4 1 0 57.79 6.70 4 1 0 62.29 7.20 4 1 0 83.19 9.00 4 1 0 84.29 9.10 -5 -1 0 79.29 8.70 -5 -1 0 88.79 17.70 -5 -1 0 55.99 7.70 -5 -1 0 53.29 7.40 5 1 0 85.29 8.20 5 1 0 77.59 13.10 5 1 0 77.69 8.90 5 1 0 72.89 8.90 5 1 0 73.29 8.10 5 1 0 63.69 7.40 -6 -1 0 -2.40 4.20 -6 -1 0 0.50 3.90 -6 -1 0 3.10 4.60 -6 -1 0 10.40 7.60 -6 -1 0 2.20 5.20 6 1 0 -2.00 3.50 6 1 0 -1.30 4.90 6 1 0 -2.60 3.50 6 1 0 3.70 5.00 6 1 0 4.20 4.60 -7 -1 0 671.83 51.99 -7 -1 0 688.43 51.19 -7 -1 0 703.23 51.39 7 1 0 649.54 52.39 7 1 0 610.84 51.09 7 1 0 636.94 52.49 7 1 0 625.94 50.79 -8 -1 0 19.30 7.40 -8 -1 0 14.50 7.10 -8 -1 0 26.40 7.10 -8 -1 0 18.70 11.70 -8 -1 0 22.50 8.20 8 1 0 6.60 7.90 8 1 0 20.90 8.30 8 1 0 10.70 5.60 8 1 0 17.50 8.60 8 1 0 19.20 6.60 -9 -1 0 6.50 12.70 -9 -1 0 1.40 8.50 -9 -1 0 12.30 7.60 -9 -1 0 16.80 7.20 -9 -1 0 23.00 9.10 9 1 0 30.70 11.10 9 1 0 -3.30 7.80 9 1 0 38.80 10.40 9 1 0 13.10 6.30 9 1 0 20.40 7.70 -10 -1 0 119.59 16.20 10 1 0 119.89 14.60 -2 -2 0 15.20 3.80 -2 -2 0 25.90 4.10 -2 -2 0 17.10 3.80 -2 -2 0 16.40 3.50 2 2 0 27.20 3.80 2 2 0 6.20 2.60 2 2 0 12.40 3.00 2 2 0 16.50 3.30 2 2 0 16.90 3.40 -3 -2 0 8.50 6.60 -3 -2 0 14.20 4.30 -3 -2 0 17.40 3.90 -3 -2 0 10.80 4.30 -3 -2 0 8.20 3.80 -3 -2 0 16.30 4.60 3 2 0 14.60 3.80 3 2 0 19.00 4.60 3 2 0 9.90 4.30 3 2 0 18.60 3.50 3 2 0 11.50 3.60 3 2 0 16.40 3.60 3 2 0 11.30 4.10 -4 -2 0 580.54 44.80 -4 -2 0 570.14 45.30 -4 -2 0 579.44 45.60 -4 -2 0 547.05 45.40 4 2 0 564.04 45.10 4 2 0 606.54 46.60 4 2 0 608.84 45.00 4 2 0 555.74 45.00 4 2 0 567.54 44.50 4 2 0 588.04 44.60 4 2 0 592.74 45.30 4 2 0 596.74 45.70 -5 -2 0 25.00 6.70 -5 -2 0 33.90 6.30 -5 -2 0 28.00 7.00 -5 -2 0 28.60 6.30 -5 -2 0 23.00 6.10 -5 -2 0 37.00 7.30 -5 -2 0 38.40 6.00 5 2 0 28.40 5.50 5 2 0 37.00 6.20 5 2 0 32.70 7.80 5 2 0 32.50 8.40 5 2 0 32.60 6.00 5 2 0 27.00 6.80 5 2 0 27.80 5.70 5 2 0 31.30 5.60 5 2 0 25.90 5.10 5 2 0 25.00 6.10 5 2 0 23.80 6.30 -6 -2 0 767.92 72.79 -6 -2 0 953.70 72.19 -6 -2 0 945.31 72.39 -6 -2 0 1003.90 71.49 -6 -2 0 1049.70 71.59 6 2 0 800.62 70.29 6 2 0 910.91 71.19 6 2 0 680.33 73.19 6 2 0 989.40 70.49 6 2 0 860.01 70.49 6 2 0 1045.20 73.09 6 2 0 918.81 71.19 6 2 0 919.91 70.39 6 2 0 952.30 70.89 -7 -2 0 13.00 7.70 -7 -2 0 5.90 8.20 -7 -2 0 2.10 6.90 7 2 0 8.30 9.50 7 2 0 8.70 7.10 7 2 0 15.40 6.30 7 2 0 5.80 6.90 7 2 0 13.50 6.80 7 2 0 9.80 6.40 7 2 0 10.10 5.60 7 2 0 9.90 7.00 -8 -2 0 13.70 9.30 -8 -2 0 25.20 9.10 8 2 0 24.20 7.30 8 2 0 10.20 6.50 8 2 0 18.60 7.30 8 2 0 25.40 8.90 8 2 0 11.60 8.10 8 2 0 20.70 7.80 -9 -2 0 -3.50 9.80 -9 -2 0 12.90 10.00 9 2 0 1.40 7.20 9 2 0 16.50 8.50 9 2 0 3.40 6.90 9 2 0 6.90 7.90 9 2 0 3.30 9.20 9 2 0 4.80 9.30 -10 -2 0 76.09 15.00 -10 -2 0 61.99 14.80 10 2 0 100.39 14.30 10 2 0 94.99 13.00 10 2 0 114.79 14.20 10 2 0 77.39 15.10 -11 -2 0 5.50 12.80 -11 -2 0 12.10 11.70 11 2 0 10.40 9.80 11 2 0 12.20 8.30 11 2 0 6.20 11.60 11 2 0 10.20 10.00 -12 -2 0 339.47 34.00 -12 -2 0 428.16 37.10 12 2 0 349.77 34.80 12 2 0 260.67 30.50 12 2 0 328.07 30.90 12 2 0 328.57 32.70 -13 -2 0 63.49 17.50 -13 -2 0 74.19 17.50 13 2 0 99.89 14.40 13 2 0 25.80 13.40 13 2 0 74.29 17.80 13 2 0 34.60 12.90 -3 -3 0 522.35 39.60 -3 -3 0 475.95 40.10 -3 -3 0 487.35 39.70 -3 -3 0 479.75 39.30 3 3 0 545.05 39.00 3 3 0 475.15 39.40 3 3 0 492.65 40.20 3 3 0 476.55 39.30 -4 -3 0 -2.30 5.60 -4 -3 0 -2.50 6.00 -4 -3 0 -0.40 6.80 -4 -3 0 -1.90 6.10 -4 -3 0 6.10 5.60 -4 -3 0 3.60 5.70 4 3 0 7.60 5.20 4 3 0 5.50 6.80 4 3 0 -4.40 6.40 4 3 0 6.50 5.20 4 3 0 4.60 4.50 4 3 0 0.80 4.50 4 3 0 7.20 4.50 4 3 0 5.90 5.00 -5 -3 0 521.95 38.30 -5 -3 0 423.46 37.10 -5 -3 0 516.15 40.30 -5 -3 0 462.25 36.50 5 3 0 493.85 35.90 5 3 0 342.47 35.90 5 3 0 430.16 37.10 5 3 0 428.36 36.80 -6 -3 0 115.09 14.00 -6 -3 0 100.49 12.40 -6 -3 0 97.49 13.80 6 3 0 92.39 14.00 6 3 0 102.59 13.20 6 3 0 94.89 12.00 6 3 0 112.49 12.10 6 3 0 101.29 11.50 6 3 0 108.79 13.60 6 3 0 110.19 12.90 6 3 0 81.89 14.50 -7 -3 0 3.40 7.40 -7 -3 0 4.00 9.20 -7 -3 0 1.60 6.60 -7 -3 0 -14.10 8.30 7 3 0 -8.80 7.20 7 3 0 3.20 5.90 7 3 0 -4.50 6.00 7 3 0 1.40 6.70 7 3 0 -1.30 6.70 7 3 0 10.10 6.80 7 3 0 -4.30 7.40 7 3 0 3.40 10.50 7 3 0 -3.40 6.70 -8 -3 0 -19.30 7.60 -8 -3 0 -3.30 9.00 -8 -3 0 -7.80 9.60 -8 -3 0 6.10 8.70 8 3 0 2.50 10.90 8 3 0 1.20 7.10 8 3 0 -3.90 7.00 8 3 0 -0.20 6.40 8 3 0 7.60 9.00 8 3 0 -8.20 7.60 8 3 0 2.30 8.00 8 3 0 2.60 7.60 8 3 0 1.60 8.50 -9 -3 0 696.73 55.69 -9 -3 0 668.73 55.69 -9 -3 0 667.53 55.89 -9 -3 0 689.83 56.19 9 3 0 689.63 56.59 9 3 0 663.73 55.29 9 3 0 689.03 53.99 9 3 0 716.73 55.59 9 3 0 631.24 55.29 9 3 0 671.03 58.29 9 3 0 648.04 53.99 -10 -3 0 199.68 22.50 -10 -3 0 165.88 21.30 -10 -3 0 229.48 23.70 10 3 0 157.58 21.10 10 3 0 201.78 21.60 10 3 0 218.78 20.60 10 3 0 185.68 23.60 10 3 0 188.88 21.00 10 3 0 176.38 22.00 -11 -3 0 279.27 29.50 11 3 0 276.87 33.80 11 3 0 289.87 29.00 11 3 0 289.77 27.60 11 3 0 281.87 27.80 11 3 0 295.67 32.70 -12 -3 0 -9.50 13.80 -12 -3 0 1.20 13.00 -12 -3 0 5.30 13.10 12 3 0 -23.50 9.00 12 3 0 3.40 13.90 12 3 0 24.90 15.60 12 3 0 1.80 11.00 12 3 0 -3.50 10.50 -13 -3 0 57.19 17.80 -13 -3 0 58.29 18.60 -13 -3 0 51.09 16.80 13 3 0 67.69 19.70 13 3 0 70.89 13.80 13 3 0 84.49 17.60 13 3 0 72.89 14.60 13 3 0 88.49 18.90 -14 -3 0 -6.50 13.90 -14 -3 0 6.00 15.90 -14 -3 0 8.30 16.70 14 3 0 2.50 15.70 14 3 0 -1.30 10.90 14 3 0 -14.20 16.00 14 3 0 2.10 12.20 14 3 0 10.00 11.20 -15 -3 0 3.70 17.70 -15 -3 0 -7.40 14.80 15 3 0 -7.90 17.50 15 3 0 6.70 12.60 15 3 0 -3.90 16.10 -4 -4 0 1244.78 94.79 -4 -4 0 1235.58 95.19 -4 -4 0 1251.37 94.89 -4 -4 0 1277.07 94.39 -4 -4 0 1234.08 95.59 4 4 0 1231.38 94.29 4 4 0 1163.28 93.99 4 4 0 1227.88 96.19 -5 -4 0 -2.10 7.60 -5 -4 0 2.10 9.40 -5 -4 0 -3.70 7.10 -5 -4 0 1.10 8.80 5 4 0 1.00 6.60 5 4 0 -0.40 6.60 5 4 0 -10.50 8.00 5 4 0 8.80 6.90 -6 -4 0 79.99 11.90 -6 -4 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712.63 57.39 -7 -1 -14 657.03 63.09 7 -1 14 731.13 58.69 7 -1 14 780.82 58.79 7 -1 14 648.64 56.39 -7 -1 -14 768.92 61.89 7 1 14 673.43 58.29 7 1 14 705.13 58.59 8 -1 14 -1.60 9.30 -8 -1 -14 8.10 14.80 8 -1 14 -1.10 10.90 8 1 14 -3.70 8.70 8 1 14 -11.40 10.20 9 -1 14 134.09 20.00 -9 -1 -14 109.29 21.50 9 -1 14 156.68 18.10 9 1 14 165.18 19.70 9 1 14 123.19 20.80 10 -1 14 23.10 13.90 10 1 14 8.90 14.70 10 1 14 30.10 13.80 -3 -2 14 -28.90 19.80 2 2 -14 240.08 44.60 -1 -2 14 6.20 19.70 1 2 -14 1.80 16.00 1 2 -14 -3.20 14.80 0 -2 14 248.18 31.60 0 -2 14 236.38 30.30 0 2 -14 207.98 28.90 0 2 -14 204.38 29.00 0 2 -14 137.79 25.80 1 -2 14 -12.30 16.50 1 -2 14 8.70 17.80 -1 2 -14 8.40 12.60 -1 2 -14 15.90 17.30 -1 2 -14 0.00 13.30 2 -2 14 13.70 16.80 -2 2 -14 11.10 12.40 -2 2 -14 -9.50 15.70 3 -2 14 17.50 15.00 -3 2 -14 -2.40 11.90 -3 2 -14 -8.70 15.70 -3 2 -14 6.00 11.20 -3 2 -14 3.60 12.80 -4 2 -14 123.19 16.80 -4 2 -14 93.59 17.40 -4 2 -14 134.49 19.50 -4 2 -14 96.09 21.30 -5 2 -14 -3.90 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394.76 43.90 -1 -3 14 336.97 43.10 1 3 -14 406.56 40.70 1 3 -14 453.05 42.20 1 3 -14 455.45 49.90 0 -3 14 -18.30 18.10 0 3 -14 30.10 25.70 0 3 -14 -0.80 20.20 1 -3 14 38.00 18.40 -1 3 -14 36.20 14.20 -1 3 -14 9.60 17.10 -2 3 -14 7.80 12.70 -2 3 -14 -1.20 16.00 -3 3 -14 22.80 13.00 -3 3 -14 11.60 16.50 -4 3 -14 18.60 13.80 -4 3 -14 15.30 17.10 5 -3 14 18.50 16.80 -5 3 -14 25.60 17.30 6 -3 14 -13.40 14.60 -6 3 -14 -8.40 15.30 7 -3 14 1.20 14.40 -7 3 -14 23.00 15.90 -7 3 -14 9.30 17.60 8 -3 14 39.80 15.70 -8 3 -14 15.70 15.90 -8 3 -14 52.59 16.50 -7 -4 14 20.00 26.70 -7 -4 14 -27.40 23.80 7 4 -14 11.70 19.50 7 4 -14 -9.30 20.40 7 4 -14 -28.90 18.60 -6 -4 14 67.79 27.40 -6 -4 14 67.19 27.30 6 4 -14 108.39 30.80 6 4 -14 126.99 23.70 6 4 -14 120.39 25.60 -5 -4 14 -11.70 22.00 -5 -4 14 -15.70 22.80 5 4 -14 -26.20 16.60 5 4 -14 -17.50 17.50 5 4 -14 -31.40 24.60 -4 -4 14 428.06 51.29 -4 -4 14 440.86 50.59 4 4 -14 463.05 56.39 4 4 -14 521.05 49.50 4 4 -14 462.55 46.60 -3 -4 14 37.40 23.30 3 4 -14 37.50 17.70 3 4 -14 60.59 25.60 -2 -4 14 612.64 52.29 2 4 -14 392.36 48.30 2 4 -14 373.66 43.10 -1 -4 14 -13.40 20.40 1 4 -14 -9.10 15.00 1 4 -14 -6.40 20.30 0 -4 14 8.40 19.90 0 4 -14 -34.30 18.20 0 4 -14 11.10 15.10 1 -4 14 80.09 21.30 -1 4 -14 0.60 14.00 -1 4 -14 26.90 21.30 2 -4 14 66.79 22.10 -2 4 -14 106.19 19.50 -2 4 -14 38.60 22.40 3 -4 14 34.40 20.60 -3 4 -14 48.70 21.80 -3 4 -14 12.70 14.80 4 -4 14 152.18 26.10 -4 4 -14 120.99 26.50 5 -4 14 16.90 17.80 -5 4 -14 65.79 22.00 6 -4 14 18.80 20.30 6 -4 14 -13.50 19.70 -6 4 -14 -36.40 51.19 -6 -5 14 13.50 28.60 6 5 -14 26.20 22.50 6 5 -14 61.69 43.00 -5 -5 14 18.60 23.90 5 5 -14 38.10 29.20 5 5 -14 21.00 19.50 -4 -5 14 -8.30 21.90 4 5 -14 3.30 23.90 4 5 -14 -30.70 14.90 3 5 -14 319.57 35.50 3 5 -14 279.07 41.10 -2 -5 14 15.90 22.30 2 5 -14 -35.80 12.90 2 5 -14 -15.70 22.50 -1 -5 14 -6.70 19.40 1 5 -14 38.30 24.30 1 5 -14 37.80 15.90 0 -5 14 5.40 21.10 0 5 -14 24.20 14.90 0 5 -14 21.60 23.40 1 -5 14 6.90 20.90 -1 5 -14 -4.10 21.10 -1 5 -14 30.80 17.70 2 -5 14 50.99 22.50 2 -5 14 62.39 24.00 -2 5 -14 47.20 24.20 -2 5 -14 69.69 30.30 -2 5 -14 67.49 18.40 3 -5 14 15.10 22.10 3 -5 14 11.20 20.20 -3 5 -14 28.00 23.00 -3 5 -14 10.50 21.30 4 -5 14 35.80 24.20 4 -5 14 -4.30 19.00 -4 5 -14 -32.70 19.60 -4 5 -14 -2.90 24.90 -2 -6 14 59.09 27.80 2 6 -14 36.40 25.30 2 6 -14 82.19 30.40 1 6 -14 39.30 21.30 0 -6 14 18.00 24.40 0 -6 14 -9.90 22.90 0 6 -14 -26.10 28.40 0 6 -14 -41.50 22.60 0 6 -14 -32.40 17.00 1 -6 14 5.10 23.30 1 -6 14 -23.40 22.10 -1 6 -14 23.10 25.00 -1 6 -14 12.20 25.20 2 0 15 17.50 16.40 3 0 15 24.10 9.80 3 0 15 25.20 9.70 4 0 15 7.40 14.40 4 0 15 8.80 8.40 -4 0 -15 3.20 14.10 -4 0 -15 5.40 11.50 4 0 15 -10.80 8.30 -4 0 -15 6.70 13.70 4 0 15 -1.70 9.00 4 0 15 19.30 14.60 -4 0 -15 -5.90 10.80 -4 0 -15 2.20 11.50 -5 0 -15 15.40 12.40 -5 0 -15 3.70 11.90 -5 0 -15 1.60 9.60 -5 0 -15 -8.20 14.70 5 0 15 -2.00 9.00 5 0 15 8.90 9.10 5 0 15 8.00 12.90 5 0 15 0.20 8.80 6 0 15 17.00 9.80 -6 0 -15 -1.70 11.70 -7 0 -15 -1.90 13.70 8 0 15 -12.00 11.30 9 0 15 6.00 11.20 9 0 15 -12.30 11.90 0 -1 15 1.50 6.30 0 -1 15 6.00 17.10 0 1 -15 0.10 8.30 1 -1 15 -1.30 5.80 1 -1 15 2.80 6.80 1 -1 15 -2.40 5.80 1 -1 15 -7.40 16.50 -1 1 -15 39.40 19.90 -1 1 -15 -3.20 9.70 -1 1 -15 -8.50 7.60 2 -1 15 943.01 74.89 2 -1 15 853.91 66.19 2 -1 15 849.22 74.49 2 -1 15 835.22 66.59 -2 1 -15 863.91 67.39 -2 1 -15 871.11 71.89 -2 1 -15 882.81 71.49 3 -1 15 10.20 15.70 3 -1 15 -3.30 6.90 3 -1 15 -7.80 6.20 3 -1 15 8.60 15.90 -3 1 -15 2.90 14.70 -3 1 -15 13.10 13.30 -3 1 -15 -3.40 11.90 -3 1 -15 -15.20 7.90 4 -1 15 311.57 27.60 4 -1 15 295.87 26.50 4 -1 15 299.77 32.20 -4 1 -15 318.37 30.20 -4 1 -15 269.67 31.80 -5 -1 -15 45.50 14.40 5 -1 15 34.80 9.00 -5 -1 -15 25.00 15.20 -5 -1 -15 23.50 18.20 5 -1 15 41.60 9.70 -5 1 -15 23.10 11.00 -5 1 -15 5.90 14.00 5 1 15 8.30 11.40 6 -1 15 135.19 16.20 -6 -1 -15 97.99 20.40 6 -1 15 141.29 15.60 -6 -1 -15 108.29 22.60 6 1 15 107.79 17.10 6 1 15 150.78 18.70 -6 1 -15 120.59 17.00 -6 1 -15 142.89 17.40 -7 -1 -15 18.20 20.10 7 -1 15 -7.40 8.50 7 -1 15 -2.10 7.00 -7 -1 -15 7.70 14.40 7 -1 15 7.30 8.70 7 -1 15 -5.40 7.00 7 1 15 -23.40 11.60 7 1 15 -4.10 10.40 -8 -1 -15 205.18 27.20 8 -1 15 205.08 23.30 8 -1 15 138.49 26.30 8 1 15 237.88 24.00 -9 -1 -15 25.10 16.70 9 -1 15 25.70 13.10 9 1 15 12.00 12.90 -3 -2 15 67.69 25.90 3 2 -15 71.99 23.50 -2 -2 15 24.80 21.60 2 2 -15 -18.90 21.20 -1 -2 15 347.67 41.30 1 2 -15 313.67 38.10 1 2 -15 398.26 38.50 0 -2 15 35.50 22.70 0 -2 15 -14.70 19.40 0 2 -15 -0.50 15.50 0 2 -15 4.50 15.20 0 2 -15 2.70 15.20 1 -2 15 11.50 17.30 1 -2 15 -17.30 16.60 -1 2 -15 4.00 14.30 -1 2 -15 14.80 13.70 -1 2 -15 4.10 12.90 2 -2 15 107.89 24.70 -2 2 -15 103.89 21.00 3 -2 15 36.80 16.90 -3 2 -15 10.90 14.60 -3 2 -15 10.20 12.30 -4 2 -15 12.10 14.70 -4 2 -15 14.80 11.80 -5 2 -15 609.34 58.79 -5 2 -15 750.72 57.39 -5 2 -15 623.84 54.59 -5 2 -15 621.64 55.29 -6 2 -15 33.10 13.30 -6 2 -15 29.00 14.50 -8 -2 -15 30.00 18.20 -8 -2 -15 -3.10 20.10 8 -2 15 7.10 10.70 8 2 15 2.90 13.20 8 2 15 0.10 13.20 -9 -2 -15 -3.90 18.60 -9 -2 -15 4.40 22.20 9 -2 15 -15.30 11.00 9 2 15 5.30 14.00 9 2 15 -3.70 13.10 -5 -3 15 -1.60 38.00 5 3 -15 8.70 17.50 5 3 -15 23.10 19.60 -4 -3 15 -31.40 22.00 4 3 -15 24.70 18.80 4 3 -15 -14.30 16.70 -3 -3 15 51.29 25.60 -3 -3 15 93.19 27.10 3 3 -15 115.29 24.50 3 3 -15 120.29 22.60 3 3 -15 56.19 24.30 -2 -3 15 427.66 47.80 -2 -3 15 367.16 45.60 2 3 -15 382.26 47.50 2 3 -15 440.56 43.10 2 3 -15 410.46 41.90 -1 -3 15 -5.00 20.40 -1 -3 15 20.90 21.90 1 3 -15 7.40 21.60 1 3 -15 9.40 16.30 1 3 -15 -0.40 15.00 0 -3 15 15.00 20.60 0 3 -15 14.00 15.20 0 3 -15 -12.60 22.60 1 -3 15 23.90 19.70 -1 3 -15 36.10 22.70 -1 3 -15 25.40 15.10 -2 3 -15 48.90 23.80 -2 3 -15 93.99 20.00 -3 3 -15 6.60 19.30 -3 3 -15 9.50 12.90 -4 3 -15 -21.40 12.30 -4 3 -15 23.60 17.40 -5 3 -15 33.60 16.90 -5 3 -15 41.10 17.90 -6 3 -15 -4.90 15.20 -7 3 -15 17.30 16.60 -7 -4 15 332.37 44.90 -7 -4 15 332.37 45.50 7 4 -15 288.97 41.80 7 4 -15 245.48 36.20 7 4 -15 292.27 40.30 -6 -4 15 -5.40 25.60 -6 -4 15 -5.00 25.40 6 4 -15 -1.60 18.70 6 4 -15 -44.60 17.80 6 4 -15 22.10 24.40 -5 -4 15 0.10 24.10 -5 -4 15 21.90 26.30 5 4 -15 -4.80 17.80 5 4 -15 19.40 25.80 5 4 -15 6.40 19.60 -4 -4 15 0.50 22.70 -4 -4 15 1.00 23.30 4 4 -15 -5.80 17.40 4 4 -15 -25.90 16.50 4 4 -15 -3.80 25.40 -3 -4 15 -25.70 21.10 3 4 -15 14.00 26.50 3 4 -15 -9.80 16.50 -2 -4 15 1.10 20.40 2 4 -15 23.40 17.30 2 4 -15 -34.50 26.00 -1 -4 15 3.50 20.30 1 4 -15 7.90 15.30 1 4 -15 12.50 20.40 0 4 -15 -4.10 18.50 0 4 -15 5.50 15.20 -1 4 -15 73.29 23.40 -1 4 -15 68.99 17.70 -2 4 -15 23.80 14.10 -2 4 -15 36.00 20.90 3 -4 15 133.09 26.20 -3 4 -15 122.39 21.40 -3 4 -15 83.99 24.60 4 -4 15 -5.20 17.30 -4 4 -15 26.90 19.90 -4 4 -15 4.00 15.00 5 -4 15 8.80 18.70 -5 4 -15 17.50 19.80 6 -4 15 0.80 18.30 -6 4 -15 8.80 19.20 -4 -5 15 18.00 40.50 4 5 -15 6.00 34.10 4 5 -15 -22.40 29.50 3 5 -15 -2.30 17.70 3 5 -15 40.80 25.10 2 5 -15 54.29 19.30 2 5 -15 38.60 24.80 -1 -5 15 3.70 21.40 1 5 -15 -13.50 20.40 1 5 -15 0.60 15.90 0 -5 15 23.70 22.00 0 5 -15 26.80 15.80 0 5 -15 9.90 23.30 1 -5 15 33.50 22.80 -1 5 -15 62.59 25.50 -1 5 -15 50.79 19.00 2 -5 15 114.39 28.20 -2 5 -15 123.49 29.80 -2 5 -15 140.09 23.60 3 -5 15 10.50 20.70 -3 5 -15 -13.60 20.90 4 0 16 374.96 38.10 -4 0 -16 525.05 41.90 -4 0 -16 486.05 42.00 4 0 16 461.05 39.70 -4 0 -16 464.85 44.00 -4 0 -16 485.95 44.80 -4 0 -16 455.45 41.10 4 0 16 412.56 38.40 4 0 16 459.45 45.40 4 0 16 435.16 43.60 -5 0 -16 -11.00 11.70 -5 0 -16 22.60 13.90 5 0 16 16.20 10.50 5 0 16 -2.30 13.30 5 0 16 9.40 9.50 -5 0 -16 8.50 11.00 6 0 16 57.99 12.60 -6 0 -16 69.49 15.00 7 0 16 112.09 16.30 8 0 16 175.88 21.00 1 -1 16 112.19 13.40 1 -1 16 98.69 12.50 1 -1 16 125.49 13.00 1 -1 16 200.58 28.60 -1 1 -16 146.79 15.30 -1 1 -16 172.08 23.00 2 -1 16 0.60 7.00 2 -1 16 7.80 6.60 -2 1 -16 4.60 14.70 -2 1 -16 -6.20 8.30 -2 1 -16 -14.60 15.10 3 -1 16 24.90 17.90 3 -1 16 11.00 7.90 3 -1 16 64.19 19.70 3 -1 16 26.80 8.00 -3 1 -16 25.60 10.90 -3 1 -16 35.30 15.20 -3 1 -16 28.20 14.80 4 -1 16 96.59 20.80 4 -1 16 120.69 13.60 4 -1 16 119.79 14.30 -4 1 -16 100.69 20.40 -4 1 -16 97.59 17.50 5 -1 16 111.49 15.00 5 -1 16 131.59 14.50 -5 1 -16 134.09 19.30 -5 1 -16 98.09 16.60 6 -1 16 13.20 8.90 6 -1 16 5.70 8.40 6 1 16 19.50 13.60 6 1 16 15.00 17.70 -7 -1 -16 -5.60 19.00 -7 -1 -16 4.10 15.60 7 -1 16 -4.40 8.70 7 1 16 -13.80 11.40 7 1 16 -4.80 11.10 8 -1 16 24.80 10.70 -8 -1 -16 -13.80 14.70 8 1 16 26.80 13.00 -2 -2 16 290.87 40.70 2 2 -16 344.87 41.40 -1 -2 16 25.40 22.90 1 2 -16 40.00 17.80 0 -2 16 153.88 28.00 0 -2 16 149.69 27.40 0 2 -16 99.59 22.30 0 2 -16 127.59 23.00 1 -2 16 22.30 19.80 1 -2 16 50.79 21.30 -1 2 -16 6.70 17.20 -1 2 -16 -1.30 15.20 2 -2 16 515.45 50.89 -2 2 -16 487.85 47.00 -2 2 -16 509.15 54.69 3 -2 16 57.39 18.60 -3 2 -16 52.19 17.40 -3 2 -16 62.19 15.70 -4 2 -16 71.59 17.60 -4 2 -16 71.79 17.60 -5 2 -16 117.69 20.70 -5 2 -16 125.49 18.90 -6 2 -16 99.19 15.60 -4 -3 16 -1.90 25.40 4 3 -16 40.30 20.10 4 3 -16 -3.60 16.70 -3 -3 16 22.80 22.80 -3 -3 16 5.40 23.70 3 3 -16 6.40 17.80 3 3 -16 15.10 18.70 3 3 -16 19.10 19.40 -2 -3 16 -15.90 21.90 -2 -3 16 21.80 22.60 2 3 -16 -9.90 16.50 2 3 -16 4.50 18.60 2 3 -16 5.20 17.10 -1 -3 16 271.77 37.30 -1 -3 16 280.47 36.00 1 3 -16 220.78 30.70 1 3 -16 260.77 32.20 1 3 -16 239.68 35.60 0 -3 16 -16.30 19.80 0 3 -16 -16.50 18.10 0 3 -16 -1.50 15.40 1 -3 16 -1.70 17.80 -1 3 -16 10.20 15.10 -1 3 -16 -1.00 18.70 -2 3 -16 -1.30 18.80 -2 3 -16 29.80 15.10 -3 3 -16 7.30 13.50 -3 3 -16 13.70 18.40 -4 3 -16 95.79 24.00 -4 3 -16 92.39 23.90 -5 3 -16 523.25 44.60 -5 3 -16 421.26 53.19 -6 3 -16 15.40 17.40 -5 -4 16 -14.10 28.40 -5 -4 16 21.30 30.20 5 4 -16 -31.60 34.50 5 4 -16 -14.00 23.50 5 4 -16 -22.70 33.90 -4 -4 16 48.60 27.90 -4 -4 16 2.50 25.80 4 4 -16 4.20 25.30 4 4 -16 32.00 20.30 4 4 -16 46.80 21.70 -3 -4 16 -9.50 23.70 3 4 -16 1.80 24.80 3 4 -16 -10.20 17.30 -2 -4 16 109.69 28.50 2 4 -16 53.59 19.70 2 4 -16 62.59 30.10 -1 -4 16 -13.30 21.40 1 4 -16 22.30 17.10 1 4 -16 28.30 26.20 0 4 -16 293.37 37.50 0 4 -16 444.06 50.49 -1 4 -16 7.70 16.00 -1 4 -16 17.20 20.60 -2 4 -16 159.28 28.50 -2 4 -16 136.29 23.40 -3 4 -16 16.60 20.20 -3 4 -16 17.30 18.20 -4 4 -16 49.40 17.40 -4 4 -16 46.70 21.70 -5 0 -17 1.20 12.40 -6 0 -17 2.00 13.80 2 -1 17 28.70 18.40 2 -1 17 15.10 19.00 -2 1 -17 3.10 14.80 -2 1 -17 -10.70 13.50 3 -1 17 -4.00 16.40 -3 1 -17 7.50 20.90 -3 1 -17 19.40 15.60 4 -1 17 44.20 17.90 -4 1 -17 44.70 14.40 -5 1 -17 23.10 13.30 -5 1 -17 2.70 11.50 -1 -2 17 251.87 35.70 1 2 -17 222.38 31.70 0 -2 17 33.70 21.90 0 -2 17 26.30 22.00 0 2 -17 -7.40 15.70 0 2 -17 40.70 17.40 1 -2 17 27.30 21.70 1 -2 17 40.50 21.40 -1 2 -17 5.90 15.60 -1 2 -17 40.80 17.60 2 -2 17 11.20 18.40 -2 2 -17 5.70 14.30 -4 2 -17 -17.60 11.90 -5 2 -17 122.49 28.30 -3 -3 17 36.10 24.40 -3 -3 17 13.80 26.20 3 3 -17 20.60 20.10 3 3 -17 29.30 19.70 -2 -3 17 117.99 29.30 -2 -3 17 52.79 25.80 2 3 -17 81.69 23.10 2 3 -17 88.29 23.10 2 3 -17 48.50 21.40 -1 -3 17 64.09 25.30 -1 -3 17 42.40 24.50 1 3 -17 46.60 19.80 1 3 -17 43.10 18.90 1 3 -17 24.70 20.20 0 -3 17 -26.50 19.90 0 3 -17 -4.70 15.40 0 3 -17 -9.80 17.20 1 -3 17 -21.10 19.20 -1 3 -17 10.60 15.90 -1 3 -17 32.50 19.00 -2 3 -17 314.57 41.30 -2 3 -17 405.56 39.00 -3 3 -17 6.90 17.70 -3 3 -17 5.10 14.60 -4 3 -17 75.49 21.30 -4 3 -17 86.29 18.10 -1 -4 17 102.89 27.40 1 4 -17 62.59 20.10 1 4 -17 54.69 27.90 0 4 -17 -0.60 23.30 0 4 -17 7.30 17.10 -3 1 -18 -12.20 13.20 4 -1 18 36.90 18.60 -4 1 -18 9.00 14.00 0 -2 18 6.80 22.00 0 -2 18 44.40 23.60 0 2 -18 35.60 18.20 0 2 -18 39.90 18.80 1 -2 18 4.80 21.40 1 -2 18 5.70 22.50 -1 2 -18 13.90 17.20 -1 2 -18 -19.70 17.00 2 -2 18 11.40 20.60 -2 2 -18 33.20 17.10 -3 2 -18 61.79 17.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 9472 _olex2_submission_special_instructions 'No special instructions were received' 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 O001 O 0.6830(3) 0.5964(6) 0.6506(2) 0.0475(12) Uani 1 1 d . . . . . O002 O 0.8312(3) 0.5990(6) 0.3542(2) 0.0505(13) Uani 1 1 d . . . . . O003 O 0.5229(2) 0.4953(6) 0.8124(2) 0.0430(12) Uani 1 1 d . . . . . O004 O 0.6622(2) 0.4208(5) 0.8338(2) 0.0424(11) Uani 1 1 d . . . . . O005 O 0.9257(3) 0.1084(7) 0.5102(2) 0.0557(14) Uani 1 1 d . . . . . O006 O 0.5635(3) 0.1264(6) 0.4813(2) 0.0503(13) Uani 1 1 d . . . . . O007 O 0.9795(3) 0.4605(6) 0.1767(2) 0.0486(13) Uani 1 1 d . . . . . O008 O 0.8364(2) 0.4103(5) 0.1584(2) 0.0520(13) Uani 1 1 d . . . . . O009 O 0.8284(3) 0.4341(6) 0.5268(2) 0.0591(14) Uani 1 1 d . . . . . O00A O 1.0329(3) 0.2858(6) 0.4943(2) 0.0518(13) Uani 1 1 d . . . . . O00B O 0.6903(3) 0.4196(6) 0.4840(2) 0.0529(13) Uani 1 1 d . . . . . N00C N 0.6870(3) 0.7437(8) 0.6345(3) 0.0326(12) Uani 1 1 d . . . . . O00D O 0.4571(3) 0.3060(6) 0.4993(2) 0.0517(13) Uani 1 1 d . . . . . O00E O 0.4440(3) 0.5958(7) 0.6557(3) 0.0619(15) Uani 1 1 d . . . . . N00F N 0.7608(3) 0.9351(7) 0.4648(3) 0.0250(11) Uani 1 1 d . . . . . N00G N 0.8442(3) 0.2079(6) 0.3751(2) 0.0278(11) Uani 1 1 d . . . . . O00H O 1.1218(3) 0.2973(6) 0.3406(2) 0.0590(14) Uani 1 1 d . . . . . N00I N 0.7275(3) 0.9417(6) 0.5363(3) 0.0269(11) Uani 1 1 d . . . . . N00J N 0.8321(3) 0.2606(6) 0.3006(2) 0.0266(11) Uani 1 1 d . . . . . N00K N 0.6401(3) 0.2027(7) 0.6259(3) 0.0275(12) Uani 1 1 d . . . . . N00L N 0.8144(3) 0.7434(7) 0.3672(3) 0.0324(13) Uani 1 1 d . . . . . N00M N 0.5921(3) 0.4252(6) 0.7940(2) 0.0281(12) Uani 1 1 d . . . . . O00N O 0.3722(3) 0.3609(6) 0.6565(2) 0.0610(14) Uani 1 1 d . . . . . O00O O 1.0703(3) 0.5461(7) 0.3265(3) 0.0631(17) Uani 1 1 d . . . . . N00P N 1.0614(3) 0.3997(8) 0.3338(3) 0.0371(14) Uani 1 1 d . . . . . N00Q N 0.6605(3) 0.2522(6) 0.6990(2) 0.0274(12) Uani 1 1 d . . . . . O00R O 0.8272(3) 0.8594(6) 0.3230(2) 0.0602(14) Uani 1 1 d . . . . . N00S N 0.4398(3) 0.4458(8) 0.6571(3) 0.0367(13) Uani 1 1 d . . . . . O00T O 0.6650(3) 0.8559(7) 0.6769(3) 0.0606(14) Uani 1 1 d . . . . . N00U N 0.9074(3) 0.4067(6) 0.1972(2) 0.0328(13) Uani 1 1 d . . . . . N00V N 0.7574(3) 0.4964(7) 0.5042(2) 0.0336(12) Uani 1 1 d . . . . . C00W C 0.7219(3) 0.7859(8) 0.5585(3) 0.0224(13) Uani 1 1 d . . . . . C00X C 0.7777(3) 0.7783(7) 0.4423(3) 0.0237(13) Uani 1 1 d . . . . . C00Y C 0.9057(3) 0.3375(7) 0.2746(3) 0.0259(13) Uani 1 1 d . . . . . N00Z N 0.5249(3) 0.2293(7) 0.5199(3) 0.0360(13) Uani 1 1 d . . . . . C010 C 0.5605(3) 0.2636(7) 0.5988(3) 0.0259(13) Uani 1 1 d . . . . . C011 C 0.5911(3) 0.3438(7) 0.7183(3) 0.0233(13) Uani 1 1 d . . . . . N012 N 0.9650(3) 0.2116(7) 0.4728(3) 0.0333(13) Uani 1 1 d . . . . . C013 C 0.9281(3) 0.2519(7) 0.3941(3) 0.0237(13) Uani 1 1 d . . . . . C014 C 0.5253(3) 0.3569(7) 0.6577(3) 0.0239(13) Uani 1 1 d . . . . . C015 C 0.9702(3) 0.3329(7) 0.3342(3) 0.0254(14) Uani 1 1 d . . . . . C016 C 0.7525(3) 0.6752(8) 0.5019(3) 0.0225(12) Uani 1 1 d . . . . . H00J H 0.777(4) 0.259(7) 0.272(3) 0.053(17) Uiso 1 1 d . . . . . H00K H 0.672(3) 0.130(7) 0.598(3) 0.020(14) Uiso 1 1 d . . . . . H00F H 0.775(4) 1.029(8) 0.438(3) 0.046(19) Uiso 1 1 d . . . . . 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 O001 0.057(3) 0.036(4) 0.049(3) 0.014(2) 0.008(2) -0.010(2) O002 0.063(3) 0.038(4) 0.052(3) -0.013(2) 0.014(2) 0.013(2) O003 0.041(3) 0.056(4) 0.032(2) -0.009(2) 0.007(2) 0.019(2) O004 0.035(2) 0.056(4) 0.035(2) -0.0112(19) -0.011(2) -0.0013(17) O005 0.044(3) 0.077(5) 0.046(3) 0.038(2) 0.001(2) -0.007(2) O006 0.052(3) 0.056(5) 0.042(3) -0.024(2) -0.001(2) 0.005(2) O007 0.036(3) 0.075(4) 0.035(3) 0.012(2) 0.006(2) -0.013(2) O008 0.039(3) 0.080(5) 0.036(3) 0.019(2) -0.012(2) -0.0059(19) O009 0.064(3) 0.042(4) 0.069(3) 0.001(2) -0.018(3) 0.021(2) O00A 0.036(3) 0.077(4) 0.041(3) 0.013(2) -0.013(2) -0.016(2) O00B 0.056(3) 0.038(4) 0.065(3) -0.006(2) -0.003(2) -0.0189(19) N00C 0.032(3) 0.037(4) 0.029(3) 0.002(3) 0.003(2) -0.005(2) O00D 0.037(3) 0.079(4) 0.039(3) -0.013(2) -0.010(2) 0.015(2) O00E 0.078(4) 0.049(4) 0.057(3) -0.010(3) -0.011(3) 0.033(2) N00F 0.028(3) 0.022(4) 0.025(3) 0.006(2) 0.003(2) 0.0006(19) N00G 0.027(3) 0.029(4) 0.027(3) 0.003(2) -0.001(2) -0.0030(17) O00H 0.026(3) 0.096(5) 0.055(3) 0.010(3) 0.003(2) 0.008(2) N00I 0.029(3) 0.029(4) 0.023(2) 0.001(2) 0.002(2) -0.0012(18) N00J 0.026(3) 0.028(4) 0.026(3) -0.003(2) -0.005(2) -0.0015(18) N00K 0.027(3) 0.028(4) 0.027(3) -0.005(2) 0.005(2) 0.0056(19) N00L 0.035(3) 0.032(4) 0.030(3) -0.003(2) 0.006(2) 0.001(2) N00M 0.032(3) 0.024(4) 0.028(3) 0.001(2) 0.002(2) 0.0028(19) O00N 0.027(3) 0.102(5) 0.053(3) 0.004(3) 0.000(2) -0.004(2) O00O 0.066(3) 0.058(4) 0.063(3) 0.026(3) -0.023(3) -0.036(3) N00P 0.027(3) 0.057(5) 0.027(3) 0.011(3) 0.002(2) -0.010(2) N00Q 0.027(3) 0.032(4) 0.023(3) -0.003(2) 0.002(2) 0.0050(18) O00R 0.098(4) 0.045(4) 0.040(3) 0.009(2) 0.035(3) 0.002(2) N00S 0.034(3) 0.056(5) 0.021(3) -0.003(3) 0.002(2) 0.014(2) O00T 0.097(4) 0.047(4) 0.041(3) -0.001(2) 0.034(3) 0.009(2) N00U 0.030(3) 0.043(4) 0.026(3) 0.004(2) 0.000(2) -0.001(2) N00V 0.043(3) 0.030(4) 0.028(3) 0.001(2) 0.002(2) 0.000(2) C00W 0.018(3) 0.026(4) 0.023(3) 0.004(2) 0.001(2) -0.003(2) C00X 0.025(3) 0.022(4) 0.024(3) -0.002(2) 0.001(2) 0.001(2) C00Y 0.026(3) 0.027(5) 0.024(3) 0.002(2) 0.001(2) 0.001(2) N00Z 0.030(3) 0.046(5) 0.032(3) -0.006(2) -0.004(2) -0.002(2) C010 0.024(3) 0.029(5) 0.025(3) -0.001(2) 0.000(3) -0.002(2) C011 0.024(3) 0.026(5) 0.021(3) 0.000(2) 0.006(3) -0.006(2) N012 0.025(3) 0.048(5) 0.027(3) 0.011(2) 0.004(2) 0.002(2) C013 0.024(3) 0.016(5) 0.031(3) 0.004(2) 0.002(3) 0.006(2) C014 0.016(3) 0.026(5) 0.030(3) 0.001(2) 0.001(2) 0.0000(19) C015 0.018(3) 0.033(5) 0.026(3) 0.003(2) 0.004(2) -0.001(2) C016 0.019(3) 0.023(4) 0.025(3) 0.002(2) 0.002(2) 0.002(2) 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 O001 N00C C00W 116.7(5) . . ? O00T N00C O001 125.5(7) . . ? O00T N00C C00W 117.8(7) . . ? N00I N00F C00X 112.1(5) . . ? N00I N00F H00F 122(5) . . ? C00X N00F H00F 126(5) . . ? C013 N00G N00J 103.7(4) . . ? C00W N00I N00F 104.6(5) . . ? N00G N00J C00Y 111.9(4) . . ? N00G N00J H00J 124(3) . . ? C00Y N00J H00J 123(3) . . ? N00Q N00K C010 112.1(4) . . ? N00Q N00K H00K 126(3) . . ? C010 N00K H00K 122(3) . . ? O002 N00L O00R 126.1(6) . . ? O002 N00L C00X 116.0(5) . . ? O00R N00L C00X 118.0(6) . . ? O003 N00M C011 117.2(4) . . ? O004 N00M O003 125.4(4) . . ? O004 N00M C011 117.4(4) . . ? O00H N00P C015 115.3(6) . . ? O00O N00P O00H 126.5(6) . . ? O00O N00P C015 118.2(5) . . ? C011 N00Q N00K 104.3(4) . . ? O00E N00S O00N 127.3(6) . . ? O00E N00S C014 116.5(5) . . ? O00N N00S C014 116.1(6) . . ? O007 N00U O008 126.0(4) . . ? O007 N00U C00Y 116.5(4) . . ? O008 N00U C00Y 117.4(4) . . ? O009 N00V C016 117.6(5) . . ? O00B N00V O009 124.8(6) . . ? O00B N00V C016 117.6(5) . . ? N00I C00W N00C 120.5(5) . . ? N00I C00W C016 112.9(6) . . ? C016 C00W N00C 126.6(6) . . ? N00F C00X N00L 121.2(5) . . ? N00F C00X C016 107.6(6) . . ? C016 C00X N00L 131.2(6) . . ? N00J C00Y N00U 121.5(4) . . ? N00J C00Y C015 107.5(5) . . ? C015 C00Y N00U 130.9(5) . . ? O006 N00Z O00D 126.4(4) . . ? O006 N00Z C010 117.7(4) . . ? O00D N00Z C010 115.9(4) . . ? N00K C010 N00Z 122.2(5) . . ? N00K C010 C014 107.9(4) . . ? C014 C010 N00Z 130.0(4) . . ? N00Q C011 N00M 119.6(4) . . ? N00Q C011 C014 113.1(5) . . ? C014 C011 N00M 127.2(5) . . ? O005 N012 O00A 126.3(4) . . ? O005 N012 C013 117.5(4) . . ? O00A N012 C013 116.2(4) . . ? N00G C013 N012 118.7(5) . . ? N00G C013 C015 113.3(4) . . ? C015 C013 N012 127.9(4) . . ? C010 C014 N00S 128.4(4) . . ? C010 C014 C011 102.6(4) . . ? C011 C014 N00S 129.0(5) . . ? C00Y C015 N00P 127.7(5) . . ? C00Y C015 C013 103.5(4) . . ? C013 C015 N00P 128.8(4) . . ? C00W C016 N00V 129.6(6) . . ? C00X C016 N00V 127.6(5) . . ? C00X C016 C00W 102.8(6) . . ? 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 O001 N00C 1.219(6) . ? O002 N00L 1.212(6) . ? O003 N00M 1.221(5) . ? O004 N00M 1.217(4) . ? O005 N012 1.207(6) . ? O006 N00Z 1.212(6) . ? O007 N00U 1.216(5) . ? O008 N00U 1.219(5) . ? O009 N00V 1.215(5) . ? O00A N012 1.214(5) . ? O00B N00V 1.208(5) . ? N00C O00T 1.206(7) . ? N00C C00W 1.443(8) . ? O00D N00Z 1.219(5) . ? O00E N00S 1.210(6) . ? N00F N00I 1.323(7) . ? N00F C00X 1.346(8) . ? N00F H00F 0.91(6) . ? N00G N00J 1.334(6) . ? N00G C013 1.322(6) . ? O00H N00P 1.219(6) . ? N00I C00W 1.314(7) . ? N00J C00Y 1.342(7) . ? N00J H00J 0.93(5) . ? N00K N00Q 1.323(6) . ? N00K C010 1.342(6) . ? N00K H00K 0.90(5) . ? N00L O00R 1.215(7) . ? N00L C00X 1.427(8) . ? N00M C011 1.438(6) . ? O00N N00S 1.212(6) . ? O00O N00P 1.194(6) . ? N00P C015 1.455(6) . ? N00Q C011 1.316(6) . ? N00S C014 1.455(7) . ? N00U C00Y 1.423(6) . ? N00V C016 1.443(7) . ? C00W C016 1.396(8) . ? C00X C016 1.369(8) . ? C00Y C015 1.362(6) . ? N00Z C010 1.443(6) . ? C010 C014 1.367(7) . ? C011 C014 1.391(6) . ? N012 C013 1.456(6) . ? C013 C015 1.372(7) . ? 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 O001 N00C C00W N00I 179.2(4) . . . . ? O001 N00C C00W C016 -0.9(7) . . . . ? O002 N00L C00X N00F 176.5(4) . . . . ? O002 N00L C00X C016 -4.5(8) . . . . ? O003 N00M C011 N00Q -173.0(6) . . . . ? O003 N00M C011 C014 11.0(9) . . . . ? O004 N00M C011 N00Q 8.1(9) . . . . ? O004 N00M C011 C014 -167.9(5) . . . . ? O005 N012 C013 N00G 16.6(9) . . . . ? O005 N012 C013 C015 -163.5(7) . . . . ? O006 N00Z C010 N00K 9.0(11) . . . . ? O006 N00Z C010 C014 -171.3(7) . . . . ? O007 N00U C00Y N00J -173.6(5) . . . . ? O007 N00U C00Y C015 6.5(9) . . . . ? O008 N00U C00Y N00J 8.1(8) . . . . ? O008 N00U C00Y C015 -171.8(6) . . . . ? O009 N00V C016 C00W -94.5(6) . . . . ? O009 N00V C016 C00X 85.4(6) . . . . ? O00A N012 C013 N00G -163.5(5) . . . . ? O00A N012 C013 C015 16.4(10) . . . . ? O00B N00V C016 C00W 85.0(6) . . . . ? O00B N00V C016 C00X -95.2(6) . . . . ? N00C C00W C016 N00V 0.0(8) . . . . ? N00C C00W C016 C00X -179.9(4) . . . . ? O00D N00Z C010 N00K -172.3(6) . . . . ? O00D N00Z C010 C014 7.4(11) . . . . ? O00E N00S C014 C010 -109.7(7) . . . . ? O00E N00S C014 C011 71.0(8) . . . . ? N00F N00I C00W N00C -179.5(4) . . . . ? N00F N00I C00W C016 0.6(5) . . . . ? N00F C00X C016 N00V 179.5(4) . . . . ? N00F C00X C016 C00W -0.6(5) . . . . ? N00G N00J C00Y N00U -178.8(5) . . . . ? N00G N00J C00Y C015 1.2(7) . . . . ? N00G C013 C015 N00P 179.6(6) . . . . ? N00G C013 C015 C00Y 0.0(7) . . . . ? O00H N00P C015 C00Y -116.4(6) . . . . ? O00H N00P C015 C013 64.1(8) . . . . ? N00I N00F C00X N00L -179.7(4) . . . . ? N00I N00F C00X C016 1.1(5) . . . . ? N00I C00W C016 N00V 179.9(4) . . . . ? N00I C00W C016 C00X 0.0(5) . . . . ? N00J N00G C013 N012 -179.4(5) . . . . ? N00J N00G C013 C015 0.7(6) . . . . ? N00J C00Y C015 N00P 179.7(6) . . . . ? N00J C00Y C015 C013 -0.7(7) . . . . ? N00K N00Q C011 N00M -177.3(5) . . . . ? N00K N00Q C011 C014 -0.7(8) . . . . ? N00K C010 C014 N00S -179.0(6) . . . . ? N00K C010 C014 C011 0.5(7) . . . . ? N00L C00X C016 N00V 0.4(9) . . . . ? N00L C00X C016 C00W -179.8(5) . . . . ? N00M C011 C014 N00S -4.2(10) . . . . ? N00M C011 C014 C010 176.4(6) . . . . ? O00N N00S C014 C010 69.0(8) . . . . ? O00N N00S C014 C011 -110.3(7) . . . . ? O00O N00P C015 C00Y 63.1(8) . . . . ? O00O N00P C015 C013 -116.4(7) . . . . ? N00Q N00K C010 N00Z 178.8(6) . . . . ? N00Q N00K C010 C014 -1.0(8) . . . . ? N00Q C011 C014 N00S 179.6(6) . . . . ? N00Q C011 C014 C010 0.2(7) . . . . ? O00R N00L C00X N00F -2.4(7) . . . . ? O00R N00L C00X C016 176.6(5) . . . . ? O00T N00C C00W N00I -1.3(7) . . . . ? O00T N00C C00W C016 178.6(5) . . . . ? N00U C00Y C015 N00P -0.3(11) . . . . ? N00U C00Y C015 C013 179.2(6) . . . . ? C00X N00F N00I C00W -1.0(5) . . . . ? N00Z C010 C014 N00S 1.3(12) . . . . ? N00Z C010 C014 C011 -179.3(6) . . . . ? C010 N00K N00Q C011 1.0(8) . . . . ? N012 C013 C015 N00P -0.3(11) . . . . ? N012 C013 C015 C00Y -179.9(6) . . . . ? C013 N00G N00J C00Y -1.1(6) . . . . ?