#------------------------------------------------------------------------------ #$Date: 2021-11-05 03:51:41 +0200 (Fri, 05 Nov 2021) $ #$Revision: 270320 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/83/7158392.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_7158392 loop_ _publ_author_name 'Goryaeva, Marina V.' 'Kushch, Svetlana O.' 'Burgart, Yanina V.' 'Ezhikova, Marina A.' 'Kodess, Mikhail I.' 'Slepukhin, Pavel A.' 'Triandafilova, Galina A.' 'Krasnykh, Olga P.' 'Yakovleva, Ekaterina I.' 'Zarubaev, Vladimir V.' 'Sinegubova, Ekaterina O.' 'Esaulkova, Iana L.' 'Shtro, Anna A.' 'Galochkina, Anastasia V.' 'Nikolaeva, Yulia V.' 'Saloutin, Victor I.' _publ_section_title ; New heteroanalogs of tricyclic ascidian alkaloids: synthesis and biological activity ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D1OB01843D _journal_year 2021 _chemical_formula_moiety 'C12 H16 F3 N O3' _chemical_formula_sum 'C12 H16 F3 N O3' _chemical_formula_weight 279.26 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2020-08-04 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139) ; _audit_update_record ; 2021-09-04 deposited with the CCDC. 2021-10-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.644(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.7173(16) _cell_length_b 5.9455(8) _cell_length_c 24.594(3) _cell_measurement_reflns_used 1476 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 26.0000 _cell_measurement_theta_min 4.1260 _cell_volume 2537.4(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)' _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 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 295(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.5253 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -8.00 92.00 1.00 60.00 -- 22.21 77.00 150.00 100 2 \w -8.00 92.00 1.00 60.00 -- 22.21 77.00 -90.00 100 3 \w 17.00 46.00 1.00 60.00 -- -23.92 77.00 30.00 29 4 \w -39.00 16.00 1.00 60.00 -- -23.92 77.00 30.00 55 5 \w 9.00 45.00 1.00 60.00 -- -23.92 77.00 0.00 36 6 \w -47.00 8.00 1.00 60.00 -- -23.92 77.00 0.00 55 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0032960000 _diffrn_orient_matrix_UB_12 0.0236950000 _diffrn_orient_matrix_UB_13 -0.0286523000 _diffrn_orient_matrix_UB_21 -0.0382206000 _diffrn_orient_matrix_UB_22 -0.0421175000 _diffrn_orient_matrix_UB_23 -0.0054059000 _diffrn_orient_matrix_UB_31 -0.0140476000 _diffrn_orient_matrix_UB_32 0.1090749000 _diffrn_orient_matrix_UB_33 0.0041968000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_unetI/netI 0.0655 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 7899 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.354 _diffrn_reflns_theta_min 3.622 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.132 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.50678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.462 _exptl_crystal_description plank _exptl_crystal_F_000 1168 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.221 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.054 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 176 _refine_ls_number_reflns 2593 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0642 _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^)+(0.0840P)^2^+0.1538P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1575 _refine_ls_wR_factor_ref 0.1922 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1586 _reflns_number_total 2593 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ob01843d2.cif _cod_data_source_block exp_815 _cod_original_cell_volume 2537.3(5) _cod_database_code 7158392 _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_max 0.991 _shelx_estimated_absorpt_t_min 0.939 _reflns_odcompleteness_completeness 82.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 28.22 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Ternary CH refined with riding coordinates: C10(H10) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B) ; _shelx_res_file ; TITL exp_815 in C2/c #15 exp_815.res created by SHELXL-2018/3 at 10:50:04 on 04-Aug-2020 REM reset to C2/c #15 CELL 0.71073 17.717325 5.945452 24.593975 90 101.6444 90 ZERR 8 0.001642 0.000767 0.002691 0 0.0102 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H F N O UNIT 96 128 24 8 24 L.S. 10 PLAN 5 SIZE 0.48 0.21 0.07 TEMP 22(2) CONF fmap 2 53 MORE -1 ACTA BOND $H OMIT 3 1 12 OMIT -20 0 16 OMIT 1 1 13 OMIT 20 2 1 OMIT -4 2 14 OMIT -8 0 6 OMIT 1 1 5 OMIT -22 0 8 OMIT -21 1 7 REM REM REM WGHT 0.084000 0.153800 FVAR 4.24477 F1 3 0.662946 0.064156 0.413941 11.00000 0.06485 0.11493 = 0.09707 0.00521 0.04069 -0.02107 F2 3 0.695633 0.389125 0.390335 11.00000 0.06116 0.07252 = 0.13229 -0.02810 0.04208 -0.00086 F3 3 0.626237 0.173179 0.330792 11.00000 0.03960 0.11179 = 0.09766 -0.00491 0.00852 0.00336 O1 5 0.746596 -0.152507 0.348638 11.00000 0.06036 0.04302 = 0.06040 -0.00530 -0.00679 -0.00897 O2 5 0.856692 0.237537 0.243619 11.00000 0.05654 0.11394 = 0.04866 0.02600 0.01262 0.01327 O4 5 0.965857 0.158055 0.415269 11.00000 0.04020 0.07265 = 0.05088 -0.00130 0.00390 -0.00900 N1 4 0.904604 0.097376 0.327425 11.00000 0.03900 0.08351 = 0.03951 0.00880 0.00914 0.01177 C2 1 0.985084 0.129195 0.323267 11.00000 0.03846 0.14373 = 0.06527 0.02005 0.01912 0.01546 AFIX 23 H2A 2 0.991021 0.259250 0.300689 11.00000 -1.20000 H2B 2 1.005170 -0.002652 0.307781 11.00000 -1.20000 AFIX 0 C3 1 1.024446 0.165140 0.383192 11.00000 0.03919 0.14107 = 0.07354 0.00665 0.01507 -0.00129 AFIX 23 H3A 2 1.062285 0.048022 0.395112 11.00000 -1.20000 H3B 2 1.050429 0.309576 0.387538 11.00000 -1.20000 AFIX 0 C5 1 0.902419 0.035622 0.384770 11.00000 0.04084 0.05309 = 0.03555 -0.00279 0.00109 -0.00258 C6 1 0.915871 -0.215292 0.393793 11.00000 0.06252 0.05199 = 0.05644 -0.00405 -0.00610 0.01021 AFIX 23 H6A 2 0.964890 -0.256030 0.384722 11.00000 -1.20000 H6B 2 0.875644 -0.298001 0.369230 11.00000 -1.20000 AFIX 0 C7 1 0.916045 -0.280347 0.454196 11.00000 0.08683 0.05556 = 0.05891 0.01263 -0.01887 -0.00646 AFIX 23 H7A 2 0.921835 -0.442007 0.458442 11.00000 -1.20000 H7B 2 0.959482 -0.209568 0.478498 11.00000 -1.20000 AFIX 0 C8 1 0.842545 -0.208006 0.470586 11.00000 0.08394 0.07872 = 0.05105 0.01643 -0.00135 -0.02368 AFIX 23 H8A 2 0.844628 -0.245198 0.509263 11.00000 -1.20000 H8B 2 0.799445 -0.288198 0.448351 11.00000 -1.20000 AFIX 0 C9 1 0.830613 0.041930 0.462233 11.00000 0.05903 0.08238 = 0.04415 -0.00564 0.01354 -0.01582 AFIX 23 H9A 2 0.871203 0.120258 0.487546 11.00000 -1.20000 H9B 2 0.781985 0.082772 0.471921 11.00000 -1.20000 AFIX 0 C10 1 0.830144 0.123324 0.402781 11.00000 0.04233 0.04551 = 0.04366 -0.00662 0.01132 -0.00711 AFIX 13 H10 2 0.835786 0.287205 0.405158 11.00000 -1.20000 AFIX 0 C11 1 0.758389 0.078573 0.357449 11.00000 0.03954 0.04595 = 0.04800 -0.00101 0.01005 -0.00500 C12 1 0.768772 0.198396 0.304289 11.00000 0.03942 0.05548 = 0.05165 0.00856 0.00431 0.00333 AFIX 23 H12A 2 0.730521 0.140528 0.273598 11.00000 -1.20000 H12B 2 0.758120 0.357094 0.307961 11.00000 -1.20000 AFIX 0 C13 1 0.846875 0.176080 0.289593 11.00000 0.04491 0.06178 = 0.04018 0.00502 0.00424 0.00699 C16 1 0.686325 0.175732 0.373434 11.00000 0.04564 0.06587 = 0.07254 -0.00069 0.01992 -0.00905 H1 2 0.710431 -0.202725 0.314599 11.00000 0.10795 HKLF 4 REM exp_815 in C2/c #15 REM wR2 = 0.1922, GooF = S = 1.034, Restrained GooF = 1.034 for all data REM R1 = 0.0642 for 1586 Fo > 4sig(Fo) and 0.1039 for all 2593 data REM 176 parameters refined using 0 restraints END WGHT 0.0784 0.0325 REM Highest difference peak 0.221, deepest hole -0.217, 1-sigma level 0.054 Q1 1 0.7957 0.0781 0.3798 11.00000 0.05 0.22 Q2 1 0.7799 -0.2371 0.3901 11.00000 0.05 0.21 Q3 1 0.6981 0.4983 0.3241 11.00000 0.05 0.19 Q4 1 0.8806 0.0367 0.3026 11.00000 0.05 0.19 Q5 1 0.8193 0.1682 0.2171 11.00000 0.05 0.16 ; _shelx_res_checksum 77774 _shelx_hkl_file ; 0 0 -5 11809.0 1373.80 3 0 0 5 419.590 435.057 1 0 0 -6 12213.1 828.028 3 0 0 6 15755.4 1137.80 1 0 0 -6 14719.4 1267.30 1 0 0 -7-98.3191 322.009 1 0 0 -8 12610.7 1049.71 3 0 0 -8 12514.0 1354.33 1 0 0 -9 1227.28 786.684 1 0 0 -9 1637.74 591.906 3 0 0 -10 42134.6 2453.99 1 0 0 -10 36735.8 2003.48 3 0 0 -11 2330.58 1009.48 1 0 0 -11 2266.31 664.878 3 0 0 -12 9992.80 1402.66 1 0 0 -12 9662.26 1138.84 3 0 0 -13 6575.50 1288.90 3 0 0 -13 12330.1 2393.22 1 0 0 -14 225206. 6617.08 1 0 0 -14 193074. 5472.55 3 0 0 -15 12184.1 1965.27 1 0 0 -15 7900.66 1476.03 3 0 0 -16 22627.7 1957.00 3 0 0 -16 22308.4 2368.75 1 0 0 -17 683.049 370.884 3 0 0 -17 719.292 429.308 1 0 0 -18 2243.59 918.727 1 0 0 -18 2265.74 677.962 3 0 0 -19-152.372 512.384 5 0 0 -19 102.267 229.689 3 0 0 -19-146.996 135.646 1 0 0 -20 958.237 490.897 1 0 0 -20 642.107 402.097 5 0 0 -21 325.479 422.938 5 0 0 -21 182.169 260.727 1 0 0 -22-284.575 432.386 5 0 0 -22 481.836 599.565 1 0 0 -23-80.2724 259.547 4 0 0 -23-233.020 242.340 5 0 0 -23 413.686 574.917 1 0 0 -24 6778.83 1687.11 1 0 0 -24 6957.67 1385.50 4 0 0 -24 7303.53 1801.20 5 0 0 -25 163.142 276.496 1 0 0 -25-99.1142 270.635 5 0 0 -25-51.3624 500.271 4 0 0 -26-22.3027 79.9465 5 0 0 -26-224.817 439.201 4 0 0 -26-149.008 248.110 1 0 0 -27 44.9666 139.183 1 0 0 -27 20.8049 144.827 4 0 0 -27 586.331 668.043 5 0 0 -28 3306.25 1396.24 5 0 0 -28 2358.79 1082.24 1 0 0 -29 600.456 731.435 5 0 0 -29 296.276 536.987 1 0 0 -30-649.432 624.546 5 0 0 -30 54.3056 609.391 1 0 2 0 384424. 7258.15 6 0 -2 0 369688. 5940.61 2 0 -2 1 484855. 6833.90 2 0 -2 -1 467494. 6807.65 2 0 2 -1 483352. 8271.31 6 0 2 1 490178. 8299.86 6 0 2 -2 46047.3 2002.08 2 0 2 -2 50495.6 2653.81 6 0 -2 2 42571.9 1950.91 2 0 -2 -2 51967.1 2393.04 2 0 2 -2 46776.0 2478.95 4 0 2 -3 59883.6 2915.60 4 0 -2 3 51412.0 2175.49 2 0 2 -3 50843.0 1938.95 2 0 -2 -3 64720.1 2703.42 2 0 -2 -3 51436.7 2053.58 1 0 2 -3 65070.5 3022.97 6 0 2 -4 32107.8 1630.14 2 0 -2 -4 27455.5 1598.91 1 0 2 -4 34769.6 2356.73 6 0 -2 -4 41158.9 2577.20 2 0 -2 4 25908.9 1488.52 2 0 2 -4 32850.1 2251.46 4 0 2 -5 119.974 159.384 2 0 -2 5 167.194 117.583 2 0 2 -6-649.055 452.240 4 0 -2 -6-510.828 279.965 1 0 -2 6-289.229 225.251 2 0 2 -6-373.818 366.870 6 0 2 -6 71.4632 86.7810 2 0 2 6 88.0036 120.923 1 0 -2 7 13143.7 1163.12 2 0 2 -7 13354.4 941.061 2 0 2 -7 14287.8 1455.92 4 0 -2 -7 12020.9 1083.18 1 0 2 -7 14889.2 1633.37 6 0 -2 8 961.440 364.241 2 0 2 -8 552.298 173.106 2 0 2 -8 2281.52 858.807 4 0 -2 -8 2457.09 688.631 1 0 2 -8 1684.66 975.990 6 0 -2 9 73641.0 2806.20 2 0 -2 -9 72865.4 3072.88 1 0 2 -9 67797.8 2226.67 2 0 2 -9 77287.0 3712.15 4 0 2 -10 7648.22 1748.46 4 0 2 -10 9683.76 1712.06 5 0 -2 -10 2795.68 642.655 1 0 2 -10 2418.95 441.124 2 0 -2 10 3004.62 580.897 2 0 2 -11 2016.61 689.297 5 0 2 -11 3119.60 809.623 4 0 2 -11 1812.05 362.681 2 0 -2 -11 2595.63 751.965 1 0 2 -12 341.146 494.579 5 0 -2 -12-806.027 492.501 1 0 2 -12 1282.13 711.158 4 0 2 -13 10194.3 1658.20 5 0 -2 -13 7587.71 1140.16 1 0 2 -13 10283.4 1493.26 4 0 2 -14 5531.99 1134.59 4 0 2 -14 5729.74 1394.26 5 0 -2 -14 5628.83 1008.19 1 0 -2 -15-326.919 262.077 1 0 2 -15 452.387 563.149 5 0 2 -15 74.4635 264.413 4 0 -2 -16-308.435 311.326 1 0 2 -16 117.046 229.267 4 0 2 -16 663.015 363.439 5 0 2 -17 46.3236 423.915 5 0 2 -17-179.443 185.412 4 0 -2 -17-133.051 283.589 1 0 -2 -18 1271.99 553.773 1 0 2 -18 1044.09 630.394 5 0 2 -18 1007.21 489.772 4 0 2 -19 323.164 481.094 5 0 -2 -19-525.320 469.632 1 0 2 -19 524.216 426.862 4 0 2 -20 7799.94 1856.56 5 0 2 -20 5755.02 1319.80 4 0 -2 -20 5574.62 1325.50 1 0 -2 -21 17536.1 2063.36 3 0 2 -21 16526.4 2679.43 5 0 -2 -21 14130.1 2046.29 1 0 2 -21 16812.7 2261.62 4 0 -2 -22 2036.50 856.514 1 0 2 -22 2762.65 1182.51 5 0 2 -22 2023.72 720.845 4 0 -2 -22 2128.59 812.939 3 0 2 -23 1164.26 905.242 5 0 -2 -23-147.984 120.258 3 0 2 -23 1380.17 563.570 4 0 2 -24 1231.60 558.795 4 0 2 -24 905.381 866.310 5 0 -2 -24-4.02034 236.114 1 0 -2 -24 111.754 60.4939 3 0 -2 -25 6498.74 1605.16 1 0 -2 -25 12618.0 2036.32 3 0 2 -25 9709.31 1821.77 4 0 2 -25 10867.8 2308.02 5 0 2 -26 662.933 660.651 5 0 2 -26 832.383 579.104 4 0 -2 -26 672.195 619.519 1 0 -2 -27 32.5186 118.329 1 0 2 -27 306.599 182.969 5 0 2 -27 174.380 409.734 4 0 2 -28 71.0499 120.156 4 0 -2 -28 453.896 459.511 1 0 -2 -28-112.441 244.590 2 0 2 -28 526.628 702.385 5 0 -4 0 31789.7 2682.41 2 0 4 0 36605.7 3299.66 6 0 4 1 2273.15 996.444 6 0 -4 -1 1209.03 561.403 2 0 -4 1 2150.42 692.501 2 0 -4 -2 3299.67 881.573 2 0 4 -2 3020.82 948.365 6 0 -4 2 2009.85 560.413 2 0 -4 -3 18467.1 2100.90 2 0 4 -3 18064.5 2253.58 6 0 -4 3 13956.4 1707.38 2 0 -4 -3 14962.7 1635.74 1 0 -4 -4 57138.7 2966.18 1 0 -4 4 53025.5 3289.54 2 0 -4 -4 60174.2 3747.32 2 0 -4 5 535.031 359.855 2 0 -4 -5 1144.46 496.836 1 0 -4 -5 2086.37 1038.66 2 0 -4 -6 3682.59 981.449 2 0 -4 -6 4001.28 874.170 1 0 -4 6 2633.52 695.932 2 0 4 -6 2707.66 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2 -1 3 -24-352.875 565.997 5 -1 3 -25-183.230 367.680 5 -1 -3 -25 68.9774 114.027 2 -1 3 -25 94.2771 375.885 4 -1 -3 -25-654.431 527.760 1 -1 3 -26 22.3343 421.537 4 -1 -3 -26 108.805 209.389 1 -1 -3 -26-387.453 340.369 2 -1 3 -26 936.068 741.550 5 -1 -3 -27 68.7973 467.320 1 -1 -3 -27 18.8758 187.302 2 -1 3 -27 616.620 522.957 4 -1 3 -27 262.643 535.232 5 1 5 -22 306.569 430.887 4 1 5 -22 2184.09 1056.84 6 1 -5 -22 1091.01 846.329 2 1 5 -21 3.35258 68.9505 4 1 5 -21 479.596 541.440 6 1 5 -20 407.085 390.074 4 1 -5 -20 989.756 654.488 2 1 5 -20 429.002 507.093 6 1 5 -19 464.858 464.839 4 1 -5 -19 1573.14 766.887 2 1 5 -19 2089.32 929.693 6 1 -5 -18-246.960 552.748 2 1 5 -18 380.581 525.829 6 1 5 -18 90.7334 427.076 4 1 5 -17 1593.38 819.664 4 1 -5 -17 1890.71 804.474 2 1 5 -17 1913.97 959.490 6 1 5 -16 1264.21 898.211 6 1 5 -16 328.228 228.683 4 1 -5 -16 255.133 390.613 2 1 5 -15 5030.81 1410.34 6 1 5 -15 4352.01 1308.08 4 1 -5 -15 3254.94 1081.37 2 1 -5 -14 1939.99 831.790 2 1 5 -14 1866.55 829.338 4 1 5 -14 2076.81 1056.70 6 1 -5 -13 2546.66 801.440 1 1 5 -13 2309.98 1072.94 6 1 -5 -13 1127.26 703.613 2 1 -5 -12 2934.55 1045.06 2 -1 -5 12 2847.72 923.620 2 1 -5 -12 2943.17 969.478 1 1 5 -12 2570.38 1032.86 6 1 5 -11 3181.54 1149.01 6 1 -5 -11 3661.24 1221.89 2 -1 -5 11 2336.17 871.671 2 1 -5 -11 1485.22 647.635 1 1 5 -10 8969.68 2026.94 6 -1 -5 10 9366.12 1593.18 2 1 -5 -10 11674.7 2060.38 2 1 -5 -10 9065.65 1547.40 1 1 5 -9 12891.5 2226.85 6 -1 -5 9 13075.7 1887.05 2 1 -5 -9 16708.1 2105.31 1 1 -5 -9 16542.9 2382.00 2 1 -5 -8 2708.05 992.919 1 -1 -5 8 76.1277 285.512 2 1 -5 -8 3878.88 1299.54 2 1 5 -8 1413.17 909.585 6 1 -5 -7 6019.12 1271.69 1 -1 -5 7 4129.24 1033.17 2 1 -5 -7 3268.63 926.791 2 1 5 -7 5772.97 1510.93 6 -1 -5 6 821.074 503.927 2 1 5 -6 1225.03 784.301 6 1 -5 -6 1329.80 503.338 2 1 -5 -6 1601.75 695.033 1 -1 -5 5 1355.83 720.354 2 1 -5 -5 770.765 388.708 1 1 -5 -5 588.455 286.143 2 1 5 -5 1638.92 806.021 6 1 -5 -4-284.070 413.136 1 1 5 -4-111.993 233.673 6 -1 -5 4 323.624 383.593 2 1 -5 -4-415.135 645.093 2 1 -5 -3 383.282 249.868 1 -1 -5 3 975.872 703.461 2 1 5 -3 1942.57 953.936 6 1 -5 -3 532.210 526.854 2 -1 -5 2 2623.14 960.511 2 1 5 -2 2940.29 1059.13 6 1 -5 -2 2542.56 770.729 2 -1 -5 1 351.105 196.271 2 1 5 -1 457.854 332.736 6 1 -5 -1 459.056 488.742 2 -1 5 1 1013.19 668.861 6 1 5 0 933.442 655.867 6 -1 -5 0 49.4043 154.772 2 1 -5 0 709.819 483.440 2 -1 5 0 158.460 27.6020 6 -1 5 -1-385.791 588.047 6 -1 -5 -1 413.409 372.496 2 1 -5 1 139.788 274.179 2 -1 5 -2 1583.19 705.211 6 1 -5 2 1370.09 602.371 2 -1 -5 -2 1178.79 665.222 1 -1 -5 -2 1413.96 830.558 2 -1 -5 -3 5871.73 1006.70 1 -1 5 -3 7493.73 1632.03 6 -1 -5 -3 6908.97 1540.63 2 1 -5 3 6187.68 1283.94 2 -1 5 -4 4447.43 1316.36 6 -1 -5 -4 2069.95 657.786 1 1 -5 4 3054.26 909.645 2 -1 -5 -4 3693.44 1132.89 2 1 -5 5 1325.08 609.479 2 -1 -5 -5 2582.10 947.718 2 -1 5 -5 2315.02 911.792 6 -1 -5 -5 2171.35 689.241 1 -1 -5 -6 3978.73 993.523 1 -1 5 -6 2308.56 893.089 6 -1 -5 -6 2830.74 1002.10 2 1 -5 6 1734.82 568.375 2 -1 -5 -7 7040.27 1169.78 1 1 -5 7 6666.83 1241.56 2 -1 5 -7 8358.50 1784.34 6 -1 -5 -7 6196.80 1511.77 2 -1 -5 -8 3201.66 1139.55 2 1 -5 8 3867.21 991.912 2 -1 5 -8 4091.22 1301.05 6 1 -5 9-561.485 552.022 2 -1 5 -9 664.762 647.811 4 -1 5 -9 978.967 679.716 6 -1 -5 -9-94.6946 383.924 2 -1 -5 -10 698.117 654.366 2 -1 5 -10 404.573 547.264 4 1 -5 10-267.195 277.504 2 -1 5 -10-22.1192 378.645 6 -1 5 -11 1538.33 936.232 6 -1 5 -11 2832.33 1146.04 4 -1 -5 -11 3175.52 1131.23 2 -1 -5 -12 7055.21 1527.83 2 -1 5 -12 7196.87 1655.05 6 -1 5 -12 7375.10 1638.75 4 -1 -5 -13 1540.34 824.418 2 -1 5 -13 1403.05 931.701 4 -1 5 -13 1201.77 948.590 6 -1 5 -14 4567.54 1332.24 4 -1 5 -14 3962.74 1237.35 6 -1 -5 -14 3702.38 1107.98 2 -1 5 -15 777.457 721.512 6 -1 5 -15 662.721 582.873 4 -1 -5 -15 173.046 157.157 2 -1 5 -16 1023.14 716.445 4 -1 5 -16 1705.53 801.510 6 -1 -5 -16 758.522 548.652 2 -1 5 -17-310.754 364.803 4 -1 -5 -17-319.078 385.428 2 -1 5 -17 726.368 688.465 6 -1 5 -18-0.53886 183.767 4 -1 -5 -18-45.6701 391.891 2 -1 5 -19 577.282 305.295 6 -1 5 -19 572.677 604.192 4 -1 -5 -19-215.895 347.702 2 -1 -5 -20 1028.79 653.645 2 -1 5 -20 756.714 680.022 4 -1 5 -20 630.238 447.816 6 -1 5 -21-850.837 646.551 6 -1 -5 -21-422.870 435.879 2 -1 5 -21-214.800 320.533 4 1 7 -10 788.427 903.711 6 1 -7 -10 484.031 594.837 2 1 -7 -9 10.1678 130.031 2 1 7 -9 349.742 223.821 6 1 7 -8 689.459 385.576 6 1 -7 -8 633.490 740.026 2 1 -7 -7-820.113 626.517 2 1 7 -7 1589.56 988.626 6 1 7 -6 629.082 859.178 6 1 -7 -6-1012.49 673.676 2 1 7 -5-289.796 231.269 6 1 -7 -5-401.904 423.409 2 -1 -7 5 356.481 473.050 2 1 -7 -4-0.17860 340.526 2 -1 -7 4-333.521 392.973 2 -1 -7 3 515.371 815.543 2 1 -7 -3 8.36085 426.719 2 1 -7 -2 1.49874 252.835 2 -1 -7 2 635.523 772.566 2 -1 -7 1 0.53446 198.485 2 1 -7 -1 1.25244 68.2028 2 1 -7 0 1091.89 697.060 2 -1 -7 0-218.208 316.048 2 1 -7 1-509.099 299.661 2 -1 -7 -1-263.858 351.473 2 1 -7 2 1120.32 841.857 2 -1 -7 -2-9.38332 413.190 2 -1 7 -3 592.598 686.027 6 -1 -7 -3-969.723 679.087 2 1 -7 3 509.799 596.595 2 -1 7 -4-155.975 124.729 6 -1 -7 -4 145.560 270.695 2 -1 7 -5 1943.83 892.169 6 -1 -7 -5 497.477 516.615 2 -1 -7 -6 436.926 671.257 2 -1 7 -6 611.119 697.673 6 -1 -7 -7 1319.55 968.131 2 -1 7 -7 316.198 283.251 6 -1 -7 -8 465.499 715.818 2 -1 7 -8 1358.17 746.118 6 -1 7 -9 399.477 648.086 6 -1 -7 -9-131.601 256.164 2 2 0 -30 41.3256 558.442 5 2 0 -30 141.166 528.465 1 2 0 -29 253.477 814.340 5 2 0 -29-184.731 369.436 1 2 0 -28 713.540 992.169 5 2 0 -28 583.938 435.826 1 2 0 -27 1185.79 1142.58 5 2 0 -27 384.536 524.135 1 2 0 -26 4620.34 1540.80 1 2 0 -26 3911.05 1289.96 5 2 0 -25 56.7116 149.959 4 2 0 -25 483.204 638.994 5 2 0 -25 270.897 466.472 1 2 0 -24 5579.47 1525.14 5 2 0 -24 4014.49 1136.51 1 2 0 -24 5913.46 1136.92 4 2 0 -23-235.109 322.574 4 2 0 -23 25.0323 186.279 1 2 0 -23 453.934 584.036 5 2 0 -22 932.129 573.140 5 2 0 -22 1584.96 665.059 4 2 0 -22 1196.89 590.727 1 2 0 -21 267.997 557.997 5 2 0 -21 463.895 450.091 4 2 0 -21 73.3861 275.265 1 2 0 -20 13842.4 1709.06 4 2 0 -20 13082.0 2030.21 5 2 0 -20 11427.5 1979.28 1 2 0 -19-254.406 387.420 1 2 0 -19 143.106 361.223 5 2 0 -19 149.762 169.039 4 2 0 -18-138.532 356.212 1 2 0 -18 354.584 217.608 4 2 0 -18 317.564 357.517 5 2 0 -17-138.327 317.204 1 2 0 -17 461.188 410.260 5 2 0 -17 498.565 285.391 4 2 0 -16 3890.70 1025.24 5 2 0 -16 4962.03 1103.17 1 2 0 -15 861.542 1205.30 1 2 0 -14 83146.8 4241.04 1 2 0 -13 2499.17 1421.48 1 2 0 -12 164415. 5457.87 1 2 0 -11 2542.06 1260.71 1 2 0 -10 168442. 5064.61 1 2 0 -9-181.721 489.146 1 -2 0 8 3766.09 425.380 3 2 0 -8 3057.27 588.228 1 -2 0 7-35.9014 87.0635 3 2 0 -7 194.054 226.306 4 -2 0 6 129603. 3313.40 1 2 0 -6 114695. 2025.27 4 2 0 -6 132330. 3549.07 1 -2 0 6 114708. 1972.20 3 -2 0 5 115.709 130.607 1 2 0 -5-765.196 347.728 1 2 0 -4 147981. 3177.66 1 -2 0 4 157300. 3013.68 1 2 0 3 2988.62 394.339 2 -2 0 -3 2278.03 350.723 2 -2 0 -4 73896.1 1475.24 2 2 0 4 65354.3 2138.06 1 2 0 5 13766.9 1585.28 1 -2 0 -5 17150.3 1045.92 2 2 0 6 399278. 5746.63 1 -2 0 -6 382415. 5627.01 1 -2 0 -7 15032.7 2041.98 3 -2 0 -7 2155.85 910.488 1 -2 0 -8 120161. 3886.88 3 -2 0 -8 122194. 3816.31 1 -2 0 -9 1119.83 889.205 3 -2 0 -9 3157.27 1223.88 1 -2 0 -10 208.172 305.109 3 -2 0 -10 177.962 95.9990 1 -2 0 -11 144.220 407.738 1 -2 0 -11 21.2729 57.4228 3 -2 0 -12 10390.4 1377.49 1 -2 0 -12 9231.48 1252.12 3 -2 0 -13 74.4487 225.778 3 -2 0 -13 695.051 577.229 1 -2 0 -14 3182.09 815.445 3 -2 0 -14 2773.48 902.706 1 -2 0 -15 1314.54 739.868 1 -2 0 -15 886.461 605.383 3 -2 0 -16 19598.5 2166.43 1 -2 0 -16 18645.5 1996.86 3 -2 0 -17 2893.36 1353.31 3 -2 0 -17 4285.79 1538.72 1 -2 0 -18 91181.3 4743.45 3 -2 0 -18 90789.0 4864.56 1 -2 0 -19 3964.74 1252.27 1 -2 0 -19 3916.48 1135.15 3 -2 0 -20 22136.3 2607.65 1 -2 0 -20 23905.4 2472.61 3 -2 0 -21 1115.31 827.959 5 -2 0 -21 736.871 550.422 3 -2 0 -21 758.510 605.518 1 -2 0 -22 6565.83 1379.90 3 -2 0 -22 5079.32 1312.20 1 -2 0 -22 5654.08 1553.39 5 -2 0 -23-118.210 340.528 1 -2 0 -23-232.046 166.369 5 -2 0 -24 1390.70 857.330 5 -2 0 -25 541.859 683.103 5 -2 0 -26 1680.51 711.260 4 -2 0 -26 2554.45 1197.65 5 -2 0 -27-455.723 462.333 4 -2 0 -27-155.568 315.430 5 -2 0 -28 609.499 608.662 5 -2 0 -28 853.898 689.971 4 -2 0 -29-180.219 286.674 5 2 -2 -29-334.163 401.735 1 2 2 -29-591.755 570.258 5 2 -2 -28 14.0174 80.3255 1 2 2 -28 104.120 338.891 5 2 -2 -27 427.055 432.195 1 2 2 -27 496.116 322.075 4 2 2 -27 408.066 581.783 5 2 -2 -26-220.426 409.104 1 2 2 -26-462.205 389.841 4 2 2 -26-844.528 637.216 5 2 2 -25 503.645 448.844 4 2 2 -25 636.630 520.541 5 2 -2 -25-123.678 233.476 1 2 2 -24 2272.63 903.566 1 2 -2 -24 1974.65 919.096 1 2 2 -24 2937.20 1185.79 5 2 2 -24 2146.26 806.234 4 2 2 -23 4553.22 1432.30 5 2 2 -23 4562.25 1293.47 1 2 -2 -23 3936.01 1296.09 1 2 -2 -23 6051.54 1244.84 3 2 2 -23 5073.76 1191.90 4 2 2 -22 1329.96 814.030 5 2 2 -22 1629.04 702.319 4 2 -2 -22 2925.93 858.346 3 2 -2 -22 2001.14 881.300 1 2 2 -22 1615.01 717.613 1 2 -2 -21 604.076 407.993 1 2 2 -21 709.873 655.116 5 2 -2 -21 466.585 143.264 3 2 2 -21 625.160 558.257 1 2 2 -21 640.192 438.943 4 2 -2 -20-223.774 336.146 3 2 2 -20 602.425 570.495 5 2 2 -20-53.4042 144.083 4 2 -2 -20 194.400 282.385 1 2 2 -20 354.492 425.078 1 2 2 -19 307.781 447.889 1 2 2 -19 560.284 464.630 4 2 2 -19 963.565 686.914 5 2 -2 -19 527.571 531.389 1 2 2 -18 12076.5 1688.22 4 2 -2 -18 10903.7 1811.98 1 2 2 -18 11347.9 1882.09 5 2 2 -18 10528.1 1786.39 1 2 2 -17 2452.43 972.394 1 2 -2 -17 1238.62 630.025 1 2 2 -17 1939.00 767.670 4 2 2 -17 2844.01 1068.24 5 2 2 -16 3073.30 965.634 1 2 2 -16 2515.16 716.279 4 2 2 -16 2913.77 940.109 5 2 -2 -16 2349.45 796.497 1 2 2 -15-12.9739 187.001 1 2 2 -15 242.830 298.725 4 2 2 -15 543.580 447.271 5 2 -2 -15 170.107 437.235 1 2 2 -14 3079.70 1278.85 4 2 2 -14 4643.64 1355.73 1 2 2 -14 3918.36 1215.44 5 2 -2 -14 939.217 565.824 1 2 2 -13 60083.7 3739.07 5 2 -2 -13 61475.1 3564.34 1 2 2 -13 62228.7 3603.95 1 2 2 -13 58514.3 3241.90 4 2 -2 -12 6818.86 1412.47 1 2 2 -12 6472.85 1234.46 4 2 2 -12 10477.0 1711.11 1 2 -2 -11 15011.0 1679.04 1 -2 -2 11 13484.4 1520.43 2 2 2 -11 14613.5 1627.44 1 2 2 -11 13479.4 1518.70 4 2 2 -10 1369.10 726.694 1 2 2 -10 787.964 529.559 4 -2 -2 10 751.684 418.667 2 2 -2 -10-711.108 474.976 1 2 2 -10 1600.82 713.855 6 -2 -2 9 10205.5 1129.81 2 2 2 -9 12088.8 1638.13 6 2 2 -9 13223.1 1571.10 4 2 2 -9 12454.1 1466.25 1 2 -2 -9 10970.5 1267.01 1 2 2 -8 16261.6 1743.85 6 -2 -2 8 15912.3 1445.38 2 2 2 -8 15496.5 1549.33 1 2 -2 -8 20103.9 1753.23 1 2 2 -8 16705.1 1657.43 4 -2 -2 7 11577.9 1291.33 2 2 2 -7 10978.9 1257.27 4 2 -2 -7 12483.6 1447.82 1 2 2 -7 10676.3 1367.79 6 2 2 -6 3779.52 766.440 6 2 2 -6 4111.74 719.980 4 2 -2 -6 4921.67 850.211 1 -2 -2 6 2580.78 567.900 2 2 -2 -5 24100.9 1781.61 1 -2 -2 5 20836.9 1533.47 2 2 2 -5 25958.5 1911.23 6 2 2 -4 19012.6 1698.10 6 -2 -2 4 16413.9 1338.19 2 2 -2 -4 18671.8 1565.59 1 -2 -2 3 73333.2 2951.54 2 2 2 -3 76130.9 3438.38 6 -2 -2 2 98202.6 3384.37 2 -2 -2 2 83612.2 2377.29 1 2 2 -2 104332. 4005.93 6 -2 2 2 119676. 4021.02 6 -2 -2 1 851.749 245.604 1 -2 -2 1-329.761 376.060 2 -2 2 1 1801.21 692.944 4 -2 2 1 1495.45 541.663 6 2 2 -1 1602.85 643.775 6 -2 2 0 3018.76 600.958 6 -2 -2 0 2549.73 500.234 2 -2 2 0 3168.05 610.539 4 2 2 0 4452.86 904.415 6 -2 2 -1 128992. 4152.45 4 2 -2 1 119572. 3093.57 2 -2 2 -1 128296. 4058.72 6 -2 -2 -1 135336. 4033.92 2 -2 -2 -2 39106.5 1170.45 1 -2 2 -2 41855.3 2348.70 4 -2 -2 -2 48835.4 2569.53 2 2 -2 2 39068.8 1670.79 2 -2 2 -2 43840.8 2355.27 6 -2 -2 -3 22998.3 925.922 1 2 -2 3 20160.5 1204.95 2 -2 2 -3 24048.7 1887.68 6 -2 2 -3 22213.7 1755.43 4 -2 -2 -3 26005.8 1924.85 2 -2 2 -4 175265. 5068.41 6 -2 2 -4 165912. 4977.36 4 -2 -2 -4 178634. 4773.08 2 -2 -2 -4 147619. 2633.88 1 2 -2 4 136340. 2826.64 2 -2 2 -5 39134.9 2522.14 6 -2 -2 -5 37682.2 2305.77 2 2 -2 5 31271.8 1314.23 2 2 2 5 30144.3 1244.91 1 -2 -2 -5 32447.8 1361.36 1 -2 -2 -6 74585.2 3262.49 2 -2 2 -6 78455.1 3691.94 4 2 2 6 62214.4 2106.73 1 -2 -2 -6 56797.4 2031.88 1 -2 2 -6 66968.6 3509.00 6 2 -2 6 55236.6 1709.47 2 -2 -2 -7 6664.81 741.062 1 -2 2 -7 5299.85 479.391 2 2 -2 7 5844.28 504.653 2 2 2 7 6164.63 671.795 1 -2 -2 -7 7397.36 1353.10 2 -2 -2 -8 33511.7 2425.28 2 -2 2 -8 34505.8 2552.24 5 -2 2 -8 34380.6 2500.81 4 2 -2 8 19158.5 1018.87 2 -2 -2 -8 27595.8 1579.24 1 -2 2 -8 25629.1 969.658 2 -2 2 -9 311.954 107.454 2 -2 -2 -9-43.4953 141.560 1 -2 2 -9 1588.95 945.083 5 -2 -2 -9 468.045 566.953 2 -2 2 -9 2407.97 1222.96 4 -2 2 -10 89.0697 393.373 4 -2 -2 -10 455.244 404.415 2 -2 -2 -10 397.651 264.620 1 -2 2 -10 41.6801 19.1330 2 -2 2 -10-48.3621 411.014 5 -2 2 -11 4369.96 955.890 4 -2 -2 -11 3726.09 703.819 1 -2 2 -11 3328.66 359.398 2 -2 -2 -11 5298.67 1053.02 2 -2 2 -11 4823.25 1109.82 5 -2 -2 -12 572.455 283.589 1 -2 2 -12 753.419 182.480 2 -2 2 -12 507.520 366.598 5 -2 2 -12 1679.45 733.960 4 -2 -2 -12 1838.63 738.044 2 -2 2 -13 1987.44 342.362 2 -2 -2 -13 2867.55 864.339 2 -2 -2 -13 1787.82 535.181 1 -2 2 -13 2411.66 793.860 4 -2 2 -13 1602.50 543.650 5 -2 -2 -14 856.524 566.528 2 -2 -2 -14 15.1990 95.1177 1 -2 2 -14 686.044 543.433 4 -2 2 -14 5.02048 86.5256 5 -2 2 -14-379.674 202.651 2 -2 -2 -15 1360.26 733.911 1 -2 2 -15 1549.54 1153.76 5 -2 2 -15 271.902 90.4478 2 -2 2 -15 3744.03 1232.80 4 -2 -2 -15 2678.13 1253.28 2 -2 2 -16 27912.2 2766.79 4 -2 -2 -16 23618.0 2344.02 1 -2 -2 -16 34601.7 3286.64 2 -2 2 -16 30297.1 3218.68 5 -2 -2 -17 5922.49 1542.09 2 -2 2 -17 7093.12 1543.03 4 -2 -2 -17 3902.99 943.710 1 -2 2 -17 7080.45 1959.77 5 -2 2 -18 17008.3 2639.39 5 -2 -2 -18 19873.4 2614.26 2 -2 2 -18 16774.3 2219.90 4 -2 -2 -18 14952.9 1830.28 1 -2 2 -19 15255.8 2151.98 4 -2 -2 -19 17967.6 2383.68 2 -2 2 -19 16514.8 2590.34 5 -2 -2 -19 11580.6 1764.14 1 -2 -2 -20-83.6762 271.711 1 -2 2 -20 325.342 358.796 4 -2 -2 -20 246.986 398.050 2 -2 2 -20 660.911 713.001 5 -2 2 -21-213.688 321.087 4 -2 -2 -21 482.894 547.921 2 -2 2 -21 267.293 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4245.96 1 -3 -1 8 145347. 4495.70 2 3 1 -8 158385. 4299.96 1 3 1 -8 149515. 3780.67 4 -3 -1 7 2541.86 477.341 2 3 1 -7 3173.04 520.616 4 3 1 -7 2929.22 577.038 1 -3 -1 7 4332.26 650.124 4 3 -1 -7 1362.73 406.761 1 3 1 -6 7659.86 859.735 6 -3 -1 6 9680.48 1018.44 5 -3 -1 6 6649.32 802.692 2 3 1 -6 7191.85 1191.53 1 3 -1 -6 6008.20 990.228 1 -3 -1 6 8080.55 807.649 4 3 1 -5 312412. 4851.28 1 -3 -1 5 322811. 5629.14 5 3 -1 -5 302422. 3550.52 4 -3 -1 5 316827. 5261.87 4 3 -1 -5 321141. 6442.22 1 -3 -1 5 313109. 5818.57 2 3 1 -5 300103. 5232.69 6 -3 -1 4 54753.7 2238.46 6 -3 -1 4 44465.1 1881.52 4 3 -1 -4 56400.3 1630.68 4 3 -1 -4 47245.3 2321.29 1 3 1 -4 48794.5 2066.34 2 -3 1 4 49627.1 2134.82 1 -3 -1 4 52034.2 1903.30 1 3 -1 -4 45007.1 1683.17 6 3 1 -4 48758.9 2006.08 6 3 1 -4 53487.5 1870.12 1 3 1 -3 851138. 8442.50 6 3 -1 -3 991367. 7095.72 4 -3 -1 3 810861. 6636.78 1 -3 -1 3 940997. 9193.29 2 -3 -1 3 933693. 8805.07 6 3 -1 -3 850505. 9237.32 1 3 1 -3 890368. 6578.70 1 3 -1 -3 852683. 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2486.22 1087.69 1 8 2 -19 631.720 463.541 6 8 2 -19 1670.97 790.923 1 8 2 -18 743.731 532.303 6 8 -2 -18 758.895 524.519 1 8 2 -18 910.031 431.836 1 8 2 -17 3804.39 1012.43 6 8 -2 -17 4487.96 1315.52 1 8 2 -17 3897.46 1026.98 1 8 2 -16 5187.93 1159.40 6 8 2 -16 6442.53 1301.79 1 8 -2 -16 6078.68 1502.33 1 8 -2 -15 10050.0 1925.33 1 8 2 -15 10074.5 1547.57 1 8 2 -15 8226.79 1408.09 6 8 2 -14 1085.93 487.789 6 8 2 -14 933.796 604.053 1 8 -2 -14 665.826 579.958 1 -8 -2 14 1599.23 774.105 2 8 2 -13 477.525 425.991 6 8 2 -13 883.062 559.244 1 8 -2 -13 487.473 112.391 3 8 -2 -13 651.892 616.402 1 -8 -2 13 770.672 291.771 2 8 -2 -12 9170.84 673.874 3 8 -2 -12 15680.6 2237.24 1 -8 -2 12 12129.4 1994.26 2 8 2 -12 12464.3 1494.64 1 8 2 -12 10458.8 1415.92 6 -8 -2 11 1872.36 719.545 2 8 2 -11 1204.10 468.335 6 8 2 -11 1345.95 494.953 1 8 -2 -11 1459.53 302.973 3 8 -2 -11 943.891 697.912 1 -8 -2 10 8394.45 1590.02 2 8 2 -10 9595.32 1267.88 1 8 2 -10 7685.44 1214.49 6 -8 -2 9 6272.03 1354.44 2 8 2 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1021.66 425.433 4 -8 2 1 52542.2 2930.93 4 -8 2 1 53378.8 2536.33 6 8 2 -1 46489.3 1647.84 1 -8 2 0 20434.7 1939.50 4 8 2 0 14876.4 816.150 1 -8 -2 0 20863.8 2060.17 2 -8 2 0 19784.4 1601.45 6 -8 -2 -1 907.135 319.563 2 -8 2 -1 1684.56 625.172 4 8 2 1 1252.28 275.978 1 -8 2 -1 1286.81 409.019 6 8 2 2 29992.2 1203.34 1 -8 2 -2 28971.0 2262.66 4 -8 -2 -2 35707.4 2748.07 2 -8 2 -2 29919.7 2099.34 6 8 -2 3 1151.87 347.223 2 8 2 3 1268.04 241.343 1 -8 -2 -3 1650.54 575.911 2 8 2 3 1735.07 272.324 1 8 -2 4 2194.25 492.636 2 8 2 4 1836.52 289.342 1 -8 2 -4 2011.35 541.270 5 -8 -2 -4 3501.69 954.559 2 -8 2 -4 2973.74 867.647 4 -8 2 -5 13300.6 1599.48 5 -8 2 -5 14789.6 1931.25 4 8 2 5 10248.7 778.841 1 -8 -2 -5 16270.7 1847.58 2 -8 2 -6 6947.49 1211.80 5 -8 -2 -6 8012.31 1257.76 2 -8 2 -6 7822.59 1445.19 4 8 2 6 4835.43 569.853 1 -8 2 -7 10578.4 1563.55 5 -8 2 -7 10891.3 1691.42 4 -8 -2 -7 11395.9 1559.23 2 -8 2 -8-217.608 266.966 5 -8 2 -8 561.186 626.113 4 -8 -2 -8 141.150 443.431 2 -8 2 -9 139.837 118.367 5 -8 2 -9-225.141 488.692 4 -8 -2 -9 189.900 312.538 2 -8 2 -10-153.505 106.199 5 -8 -2 -10 157.350 80.7306 2 -8 2 -11 9587.01 1733.15 5 -8 2 -11 10067.9 1778.66 4 -8 -2 -11 8957.54 1368.36 2 -8 2 -12 2614.84 1066.82 5 -8 2 -12 3265.72 1158.93 4 -8 -2 -12 2814.52 873.539 2 -8 2 -13 10602.0 1915.04 5 -8 2 -13 11139.1 1925.22 4 -8 -2 -13 9730.38 1514.25 2 -8 2 -14 7305.37 1675.08 5 -8 2 -14 8506.86 1826.99 4 -8 -2 -14 5898.89 1195.57 2 -8 2 -15 3152.14 1120.17 5 -8 2 -15 3409.43 1189.11 4 -8 -2 -15 1737.76 650.099 2 -8 2 -16 6757.26 1639.19 5 -8 2 -16 6477.30 1544.21 4 -8 -2 -16 4540.81 1015.12 2 -8 2 -17 4091.39 1352.80 5 -8 2 -17 3762.44 1207.02 4 -8 -2 -17 3635.91 925.597 2 -8 2 -18 1976.47 948.809 5 -8 -2 -18 1587.45 586.488 2 -8 2 -18 2128.68 975.326 4 -8 2 -19 5219.35 1451.02 5 -8 2 -19 4804.27 1359.46 4 -8 -2 -19 4385.48 1114.64 2 -8 -2 -19 4774.70 1391.60 3 -8 2 -20 1182.46 865.863 5 -8 2 -20 678.939 623.788 4 -8 -2 -20 721.824 513.060 2 -8 -2 -20-292.682 431.732 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1231.99 2 -8 4 1 4995.85 1230.88 4 -8 4 0 350.886 490.726 6 -8 -4 0-699.250 417.777 2 -8 4 0 354.871 474.281 4 -8 4 -1 1050.63 476.253 6 -8 -4 -1 1817.23 1094.40 2 -8 4 -1 1172.36 700.431 4 -8 4 -2 11868.6 1877.71 4 -8 -4 -2 14044.4 2256.78 2 -8 4 -2 13185.9 1815.39 6 8 -4 2 11382.3 1409.87 2 -8 4 -3 18366.2 2321.90 4 -8 -4 -3 17997.3 2504.26 2 -8 4 -3 18717.0 2192.71 6 8 -4 3 11484.3 1284.25 2 -8 4 -4 6094.73 1401.95 6 -8 -4 -4 3919.91 1210.36 2 -8 4 -4 4792.24 1420.84 4 8 -4 4 2951.79 656.792 2 -8 4 -5 864.215 564.834 6 -8 -4 -5 2755.95 1522.23 2 -8 4 -5 2273.52 953.054 4 8 -4 5 484.420 275.456 2 -8 4 -6 16759.8 2266.77 4 -8 -4 -6 18032.9 2472.40 2 -8 4 -6 17310.1 2209.43 6 -8 4 -7 2294.25 975.695 6 -8 -4 -7 1925.70 1006.94 2 -8 4 -7 2291.13 1048.30 4 -8 4 -8 3749.11 1038.70 6 -8 -4 -8 3683.34 1182.49 2 -8 4 -8 4051.01 1178.17 4 -8 4 -9 1110.96 677.084 6 -8 -4 -9 1487.39 879.243 2 -8 4 -9 907.070 764.660 4 -8 4 -10 4640.27 1223.48 6 -8 -4 -10 5644.65 1568.00 2 -8 4 -10 5189.88 1419.94 4 -8 4 -11 7413.98 1577.24 6 -8 -4 -11 5637.94 1482.11 2 -8 4 -11 6794.69 1595.10 4 -8 4 -12 453.741 608.357 6 -8 -4 -12 917.442 917.108 2 -8 4 -12 962.709 809.563 4 -8 -4 -13 8623.65 1847.42 2 -8 4 -13 10130.7 1978.21 4 -8 4 -13 8799.96 1816.61 6 -8 -4 -14 699.800 563.696 2 -8 4 -14 1043.14 715.269 4 -8 4 -14 1289.07 796.160 6 -8 4 -15-11.5012 300.590 6 -8 4 -15 245.596 633.486 4 -8 -4 -15 98.4411 288.754 2 -8 4 -16 837.378 667.684 4 -8 -4 -16 457.018 445.448 2 -8 4 -16-145.076 482.528 6 -8 4 -17 615.502 492.953 4 -8 -4 -17 475.335 347.052 2 -8 4 -17 68.8080 193.068 6 -8 4 -18 1249.91 840.212 4 -8 -4 -18 254.253 364.149 2 -8 4 -18 353.347 189.273 6 -8 4 -19 1589.68 1019.36 4 -8 -4 -19 499.442 468.336 2 -8 4 -19 1480.22 767.746 6 -8 4 -20-201.129 453.456 4 -8 -4 -20 182.790 270.759 2 -8 4 -20 13.2819 68.8493 6 -8 -6 16 310.582 677.266 2 8 6 -16 41.8472 260.362 6 8 -6 -16-189.934 439.554 1 8 -6 -16 6.22863 333.775 2 -8 -6 15 489.856 825.632 2 8 6 -15 195.845 421.509 6 8 -6 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-9-328.790 257.918 3 -18 0 -10 2123.00 883.017 5 -18 0 -10 1545.73 921.835 3 -18 0 -11-313.903 444.233 5 -18 0 -11-1047.68 878.321 3 -18 0 -12-313.686 428.609 5 -18 0 -12-1046.83 760.930 3 18 -2 -20-46.5212 436.147 1 18 2 -20-5.98881 376.994 1 18 -2 -19 354.515 353.561 1 18 2 -19 141.613 327.015 1 18 -2 -18 877.753 875.430 1 18 2 -18 1311.55 768.889 1 18 -2 -17 272.176 520.605 1 18 2 -17 227.109 192.996 1 18 -2 -16 324.057 244.807 1 18 2 -16 424.449 647.609 1 18 -2 -15-712.866 599.217 1 18 2 -15 322.413 518.637 1 18 -2 -14 50.7881 53.2265 1 18 2 -14 625.222 601.683 1 18 2 -13 992.400 479.395 1 18 -2 -13 1074.39 817.616 1 18 2 -12 46.9498 191.872 1 18 -2 -12 173.554 162.283 1 18 -2 -11 1238.59 934.922 1 -18 -2 11 1270.99 749.208 2 18 -2 -10-411.748 531.903 1 -18 -2 10-343.657 415.984 2 -18 -2 9 30.0907 183.847 2 18 -2 -9 606.148 531.485 1 -18 -2 8 978.054 689.672 2 18 -2 -8 1191.78 795.753 1 -18 -2 7-119.571 521.093 2 18 -2 -7 469.828 394.808 1 -18 -2 6 2884.14 1092.83 2 18 -2 -6 2760.30 1062.85 1 -18 -2 5-195.025 210.782 2 18 -2 -5 180.634 267.045 1 -18 -2 4 338.113 408.822 2 18 -2 -4 479.864 198.901 1 -18 2 4 85.6963 255.105 4 -18 -2 3 252.517 366.402 2 -18 2 3 213.338 118.891 4 18 -2 -3 160.182 424.454 1 -18 -2 2 1649.22 823.333 2 -18 2 2 1647.01 755.217 4 18 -2 -2 893.913 814.449 1 -18 -2 1 1602.88 989.245 2 -18 2 1 638.118 476.253 4 18 -2 -1 544.928 662.876 1 -18 -2 0 4128.61 1340.28 2 -18 2 0 3807.70 1091.53 4 -18 -2 -1 684.244 598.542 2 -18 2 -1 216.467 33.3029 4 -18 -2 -2-126.258 93.4911 2 -18 2 -2 155.679 219.833 4 -18 -2 -3 800.549 450.790 2 -18 2 -3 1050.63 682.015 4 -18 -2 -4-214.610 217.907 2 -18 2 -4-546.114 607.654 4 -18 -2 -5-169.106 367.730 2 -18 2 -5-74.9287 235.424 4 -18 -2 -6 1411.35 857.087 2 -18 2 -6 1237.70 794.389 4 -18 -2 -7 483.247 493.546 2 -18 2 -7 179.512 193.593 4 -18 -2 -8 1421.75 890.659 2 -18 2 -8-82.2105 189.994 4 -18 -2 -9 1640.88 954.174 2 -18 2 -9 640.308 259.617 4 -18 2 -10 118.493 261.460 4 -18 -2 -10-1026.76 746.356 3 -18 -4 11 1712.35 1263.81 2 18 -4 -11 982.372 662.316 1 -18 -4 10 669.024 783.620 2 18 -4 -10 626.483 616.570 1 -18 -4 9-401.945 492.112 2 18 -4 -9-689.927 637.450 1 -18 -4 8 93.7232 403.942 2 18 -4 -8-6.83945 328.106 1 -18 -4 7 619.411 728.169 2 18 -4 -7 41.9681 186.792 1 -18 -4 6 1063.03 903.427 2 18 -4 -6 1489.40 895.878 1 -18 -4 5 1981.10 1334.51 2 18 -4 -5 898.181 801.089 1 -18 -4 4 4010.92 1577.71 2 18 -4 -4 2116.07 1234.72 1 -18 -4 3 1050.33 885.121 2 18 -4 -3 2462.02 1097.98 1 -18 -4 2-27.6021 321.230 2 18 -4 -2-1072.10 762.562 1 -18 -4 1 32.1832 580.276 2 -18 4 1 309.700 524.904 4 -18 -4 0-6.25656 501.578 2 -18 4 0 442.218 424.011 4 -18 -4 -1-456.107 537.562 2 -18 4 -1 155.316 297.365 4 19 -1 -20 1379.59 1172.36 1 19 1 -20 1279.40 826.143 1 19 1 -19 1696.82 1045.11 1 19 -1 -19 2785.32 1212.52 1 19 1 -18 356.761 487.148 1 19 -1 -18-9.69580 322.381 1 19 1 -17-271.653 634.342 1 19 -1 -17 1058.48 761.892 1 19 1 -16-1033.47 712.586 1 19 -1 -16-63.0766 610.929 1 19 1 -15-51.5887 377.720 1 19 -1 -15 200.291 412.601 1 19 1 -14-492.200 678.380 1 19 -1 -14-121.401 330.044 1 19 1 -13 61.3135 304.523 1 19 -1 -13 312.226 365.021 1 19 1 -12 400.138 243.813 1 19 -1 -12 772.688 700.326 1 19 -1 -11 27.2650 111.970 1 19 1 -11 12.9856 454.211 1 19 -1 -10 1089.10 922.655 1 19 1 -10 1001.59 470.958 1 19 -1 -9 2705.38 1322.43 1 19 1 -9 2379.16 896.623 1 19 -1 -8 770.207 620.417 1 19 1 -8 932.821 575.323 1 19 -1 -7-209.058 179.871 1 19 1 -7 302.744 268.781 1 -19 -1 6 2945.43 852.094 3 19 -1 -6 3504.40 1283.76 1 19 1 -6 4071.46 1258.82 1 -19 -1 6 3528.26 1366.77 2 19 1 -5 5336.33 1551.77 1 19 -1 -5 4004.79 1313.36 1 -19 -1 5 5506.37 1297.66 3 -19 -1 5 4890.33 1563.02 2 19 1 -4 2787.49 975.635 1 19 -1 -4 1952.43 844.135 1 -19 -1 4 2406.96 946.192 3 -19 -1 4 2342.55 1022.80 2 -19 -1 3-240.480 360.205 2 19 1 -3 516.894 571.641 1 -19 -1 3-400.596 446.218 3 19 -1 -3-102.277 201.402 1 -19 1 3-333.940 307.960 3 -19 -1 2-243.478 238.625 2 19 -1 -2 24.6237 296.391 1 -19 -1 2 551.837 468.549 3 -19 1 2 68.6656 257.174 3 -19 -1 1 167.646 396.767 2 -19 -1 1 496.003 416.221 3 19 -1 -1-289.752 551.866 1 -19 1 1-56.3132 159.079 3 -19 -1 0-130.263 58.8283 2 19 -1 0 175.484 157.632 1 -19 -1 0-131.084 271.293 3 -19 1 0 144.146 229.322 3 -19 -1 -1-53.7663 270.423 2 19 -1 1 226.411 315.257 1 -19 -1 -1-267.328 543.105 3 -19 1 -1-299.400 446.224 3 -19 -1 -2 326.947 442.863 3 -19 1 -2 74.5958 51.3270 3 -19 -1 -3 456.796 320.167 2 -19 -1 -3 693.910 599.042 3 -19 1 -3 633.944 499.980 3 -19 -1 -4-271.708 391.846 3 -19 1 -4-1215.98 661.338 3 -19 -1 -5 929.963 743.348 2 -19 -1 -5 104.305 479.941 3 -19 1 -5 442.600 437.245 3 -19 -1 -6-76.4928 227.486 3 -19 1 -6-85.3031 250.222 3 -19 -1 -7-91.1543 280.237 3 -19 1 -7 520.167 397.018 3 -19 -1 -8 200.984 474.297 3 -19 1 -8 280.777 317.952 3 -19 -1 -9 167.302 493.690 3 -19 1 -9 608.397 574.564 3 19 -3 -14 0.28207 476.765 1 -19 -3 14-85.3542 686.832 2 19 -3 -13 370.631 599.066 1 -19 -3 13 104.862 227.526 2 -19 -3 12 578.539 380.272 2 19 -3 -12 495.158 835.489 1 -19 -3 11 1010.52 903.104 2 19 -3 -11 84.6682 254.505 1 -19 -3 10 181.113 382.395 2 19 -3 -10 634.278 826.589 1 -19 -3 9 553.150 642.862 2 19 -3 -9 603.589 736.271 1 -19 -3 8-136.039 500.575 2 19 -3 -8 592.526 485.034 1 -19 -3 7 809.722 77.5323 2 19 -3 -7 1297.21 760.274 1 -19 -3 6 896.938 821.717 2 19 -3 -6 402.367 382.358 1 -19 -3 5 932.311 934.766 2 19 -3 -5 277.281 85.3440 1 -19 -3 4-628.634 571.199 2 19 -3 -4 232.519 511.407 1 -19 -3 3 2894.52 1458.12 2 19 -3 -3 3427.61 1353.01 1 -19 -3 2 447.776 622.215 2 19 -3 -2 393.601 332.670 1 -19 -3 1 54.5583 212.712 2 19 -3 -1 159.854 606.111 1 -19 3 1 335.688 407.653 4 -19 -3 0 1081.13 939.092 2 -19 3 0-56.7306 296.950 4 -19 -3 -1-1326.38 825.251 2 -19 3 -1 748.486 323.570 4 -19 -3 -2 6.95646 552.796 2 -19 3 -2-137.156 368.090 4 -19 -3 -3-30.3032 124.460 2 -19 3 -3-339.666 424.659 4 -19 -3 -4-0.21209 477.836 2 -19 3 -4 248.044 312.619 4 20 0 -18 1227.50 1319.56 1 20 0 -17 984.268 1037.55 1 20 0 -16 405.491 157.792 1 20 0 -15-519.534 566.368 1 20 0 -14-357.732 108.908 1 20 0 -13 201.421 148.291 1 20 0 -12 184.227 272.577 1 20 0 -11-250.885 509.654 1 20 0 -10 1455.11 819.406 1 20 0 -9 519.158 492.987 1 20 0 -8 7248.69 1862.51 1 20 0 -7-14.3358 320.575 1 20 0 -6-443.293 659.510 1 20 0 -5-286.892 384.863 1 20 0 -4-142.560 307.990 1 -20 0 4-128.479 165.595 3 -20 0 3-174.853 331.407 3 20 0 -3-196.241 97.2014 1 20 0 -2 1822.70 789.821 1 -20 0 2 2665.70 923.385 3 20 0 -1-16.4081 44.2240 1 -20 0 1-385.484 296.426 3 20 0 0-378.924 417.690 1 -20 0 0 905.790 592.681 3 20 0 1 146.835 431.431 1 -20 0 -1 19.3685 180.475 3 20 0 2 21.9586 228.267 1 -20 0 -2 345.704 401.983 3 20 0 3-16.6876 250.130 1 -20 0 -3 78.3098 340.427 3 20 0 4 834.292 632.828 1 -20 0 -4 955.879 664.547 3 -20 0 -5 356.421 474.996 3 -20 0 -6-31.2579 257.417 3 -20 0 -7-55.7903 215.980 3 20 -2 -15 604.439 860.796 1 20 -2 -14 1918.85 1137.81 1 20 -2 -13 3.44148 592.361 1 20 -2 -12-256.162 406.501 1 20 -2 -11-1620.82 1043.22 1 20 -2 -10 269.686 514.661 1 -20 -2 10 567.604 438.189 2 20 -2 -9 37.5121 153.338 1 -20 -2 9-228.954 566.304 2 20 -2 -8-93.0302 211.371 1 -20 -2 8 139.858 29.5232 2 -20 -2 7-171.200 220.402 2 20 -2 -7 115.441 294.284 1 -20 -2 6 1393.59 990.068 2 20 -2 -6 1799.98 977.787 1 -20 -2 5 130.319 452.890 2 20 -2 -5 46.7346 290.339 1 -20 -2 4 2592.47 1237.56 2 20 -2 -4 1486.97 890.394 1 20 -2 -3 1840.83 922.820 1 -20 -2 3 3105.56 1406.63 2 -20 -2 2 441.845 783.740 2 20 -2 -2 573.111 549.599 1 20 -2 -1 169.502 500.697 1 -20 -2 1-1033.45 703.547 2 -20 2 1 29.9181 281.360 4 20 -2 0 267.219 538.056 1 -20 2 0 1194.39 634.992 4 -20 -2 -1-440.811 674.990 2 20 -2 1 52.4954 286.576 1 -20 -2 -2-924.872 720.876 2 -20 2 -2 467.990 455.722 4 -20 -2 -3 259.569 396.332 2 -20 2 -3 944.348 650.970 4 -20 -2 -4 1508.95 783.756 2 -20 2 -4 3574.59 1272.32 4 21 1 -14-560.242 622.657 1 21 -1 -14-806.901 665.606 1 21 1 -13-726.317 809.659 1 21 -1 -13 57.8499 180.492 1 21 1 -12 661.561 579.869 1 21 -1 -12 1168.84 962.806 1 21 -1 -11-1980.71 1307.08 1 21 1 -11 2548.04 1104.49 1 21 -1 -10-445.299 521.945 1 21 -1 -9 519.345 668.599 1 21 -1 -8-1037.67 935.233 1 21 -1 -7-291.524 714.279 1 21 -1 -6-318.780 569.155 1 21 -1 -5-433.325 686.670 1 21 -1 -4 822.961 665.241 1 -21 -1 4 1713.67 728.712 3 21 -1 -3 2594.89 1228.29 1 -21 -1 3 868.819 432.548 2 21 -1 -2 1018.32 826.676 1 -21 -1 2 792.023 678.314 3 -21 -1 2 1143.63 916.972 2 -21 -1 1 1632.64 798.544 3 21 -1 -1 523.701 382.456 1 -21 -1 1 1434.26 953.971 2 21 -1 0 725.541 559.059 1 -21 -1 0 798.041 710.341 3 -21 1 0 939.099 602.676 3 -21 -1 0-56.9177 296.941 2 -21 -1 -1 667.575 633.637 2 -21 -1 -1 109.898 397.890 3 -21 1 -1 407.222 426.838 3 21 -1 1 230.605 166.897 1 -21 -1 -2-109.971 338.168 2 21 -1 2 496.303 559.955 1 -21 -1 -2-0.18739 228.926 3 -21 1 -2 166.845 195.005 3 22 0 -9-272.219 695.076 1 22 0 -8 208.437 338.285 1 22 0 -7-230.835 482.432 1 22 0 -6 141.669 416.766 1 22 0 -5-1048.00 862.322 1 22 0 -4 5440.68 1624.61 1 22 0 -3 153.084 524.987 1 0 0 0 0.00 0.00 0 TITL exp_815 in C2/c REM C2/c (#15 in standard setting) CELL 0.71073 17.717325 5.945452 24.593975 90.0000 101.6444 90.0000 ZERR 11.00 0.001642 0.000767 0.002691 0.0000 0.0102 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O UNIT 121.00 110.00 11.00 11.00 TREF HKLF 4 END ; _shelx_hkl_checksum 74116 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.401 _oxdiff_exptl_absorpt_empirical_full_min 0.733 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 F1 F 0.66295(12) 0.0642(4) 0.41394(10) 0.0889(7) Uani 1 1 d . . . . . F2 F 0.69563(11) 0.3891(4) 0.39033(10) 0.0855(7) Uani 1 1 d . . . . . F3 F 0.62624(10) 0.1732(4) 0.33079(9) 0.0838(7) Uani 1 1 d . . . . . O1 O 0.74660(12) -0.1525(4) 0.34864(9) 0.0573(6) Uani 1 1 d . . . . . O2 O 0.85669(12) 0.2375(4) 0.24362(9) 0.0728(8) Uani 1 1 d . . . . . O4 O 0.96586(11) 0.1581(4) 0.41527(8) 0.0553(6) Uani 1 1 d . . . . . N1 N 0.90460(12) 0.0974(5) 0.32742(9) 0.0538(7) Uani 1 1 d . . . . . C2 C 0.98508(17) 0.1292(8) 0.32327(14) 0.0813(12) Uani 1 1 d . . . . . H2A H 0.991021 0.259250 0.300689 0.098 Uiso 1 1 calc R U . . . H2B H 1.005170 -0.002652 0.307781 0.098 Uiso 1 1 calc R U . . . C3 C 1.02445(18) 0.1651(8) 0.38319(15) 0.0841(12) Uani 1 1 d . . . . . H3A H 1.062285 0.048022 0.395112 0.101 Uiso 1 1 calc R U . . . H3B H 1.050429 0.309576 0.387538 0.101 Uiso 1 1 calc R U . . . C5 C 0.90242(14) 0.0356(5) 0.38477(10) 0.0441(7) Uani 1 1 d . . . . . C6 C 0.91587(19) -0.2153(5) 0.39379(13) 0.0595(8) Uani 1 1 d . . . . . H6A H 0.964890 -0.256030 0.384722 0.071 Uiso 1 1 calc R U . . . H6B H 0.875644 -0.298001 0.369230 0.071 Uiso 1 1 calc R U . . . C7 C 0.9160(2) -0.2803(6) 0.45420(13) 0.0718(11) Uani 1 1 d . . . . . H7A H 0.921835 -0.442007 0.458442 0.086 Uiso 1 1 calc R U . . . H7B H 0.959482 -0.209568 0.478498 0.086 Uiso 1 1 calc R U . . . C8 C 0.8425(2) -0.2080(6) 0.47059(14) 0.0733(11) Uani 1 1 d . . . . . H8A H 0.844628 -0.245198 0.509263 0.088 Uiso 1 1 calc R U . . . H8B H 0.799445 -0.288198 0.448351 0.088 Uiso 1 1 calc R U . . . C9 C 0.83061(18) 0.0419(6) 0.46223(12) 0.0614(9) Uani 1 1 d . . . . . H9A H 0.871203 0.120258 0.487546 0.074 Uiso 1 1 calc R U . . . H9B H 0.781985 0.082772 0.471921 0.074 Uiso 1 1 calc R U . . . C10 C 0.83014(15) 0.1233(5) 0.40278(10) 0.0435(6) Uani 1 1 d . . . . . H10 H 0.835786 0.287205 0.405158 0.052 Uiso 1 1 calc R U . . . C11 C 0.75839(15) 0.0786(5) 0.35745(11) 0.0443(7) Uani 1 1 d . . . . . C12 C 0.76877(15) 0.1984(5) 0.30429(12) 0.0495(7) Uani 1 1 d . . . . . H12A H 0.730521 0.140528 0.273598 0.059 Uiso 1 1 calc R U . . . H12B H 0.758120 0.357094 0.307961 0.059 Uiso 1 1 calc R U . . . C13 C 0.84688(16) 0.1761(5) 0.28959(11) 0.0496(7) Uani 1 1 d . . . . . C16 C 0.68632(18) 0.1757(6) 0.37343(14) 0.0602(8) Uani 1 1 d . . . . . H1 H 0.710(3) -0.203(7) 0.3146(19) 0.108(14) 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 F1 0.0649(12) 0.1149(19) 0.0971(15) 0.0052(14) 0.0407(11) -0.0211(12) F2 0.0612(12) 0.0725(14) 0.1323(19) -0.0281(13) 0.0421(12) -0.0009(10) F3 0.0396(10) 0.1118(18) 0.0977(15) -0.0049(13) 0.0085(10) 0.0034(10) O1 0.0604(13) 0.0430(12) 0.0604(13) -0.0053(10) -0.0068(11) -0.0090(10) O2 0.0565(13) 0.114(2) 0.0487(12) 0.0260(13) 0.0126(11) 0.0133(12) O4 0.0402(10) 0.0726(15) 0.0509(11) -0.0013(10) 0.0039(9) -0.0090(10) N1 0.0390(12) 0.084(2) 0.0395(12) 0.0088(12) 0.0091(10) 0.0118(12) C2 0.0385(16) 0.144(4) 0.065(2) 0.020(2) 0.0191(15) 0.0155(19) C3 0.0392(17) 0.141(4) 0.074(2) 0.007(2) 0.0151(16) -0.001(2) C5 0.0408(14) 0.0531(17) 0.0356(13) -0.0028(12) 0.0011(11) -0.0026(12) C6 0.0625(19) 0.0520(19) 0.0564(17) -0.0041(15) -0.0061(15) 0.0102(15) C7 0.087(3) 0.056(2) 0.0589(19) 0.0126(16) -0.0189(18) -0.0065(18) C8 0.084(3) 0.079(3) 0.0510(18) 0.0164(17) -0.0013(17) -0.024(2) C9 0.0590(18) 0.082(2) 0.0441(16) -0.0056(16) 0.0135(14) -0.0158(17) C10 0.0423(14) 0.0455(15) 0.0437(14) -0.0066(12) 0.0113(12) -0.0071(12) C11 0.0395(14) 0.0460(17) 0.0480(15) -0.0010(13) 0.0101(12) -0.0050(12) C12 0.0394(14) 0.0555(18) 0.0517(16) 0.0086(13) 0.0043(12) 0.0033(12) C13 0.0449(15) 0.0618(19) 0.0402(15) 0.0050(13) 0.0042(12) 0.0070(14) C16 0.0456(17) 0.066(2) 0.073(2) -0.0007(17) 0.0199(16) -0.0091(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' F F 0.0171 0.0103 '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 C11 O1 H1 118(2) . . ? C5 O4 C3 108.1(2) . . ? C2 N1 C5 108.4(2) . . ? C13 N1 C2 122.1(3) . . ? C13 N1 C5 126.8(2) . . ? N1 C2 H2A 111.3 . . ? N1 C2 H2B 111.3 . . ? N1 C2 C3 102.4(2) . . ? H2A C2 H2B 109.2 . . ? C3 C2 H2A 111.3 . . ? C3 C2 H2B 111.3 . . ? O4 C3 C2 106.9(3) . . ? O4 C3 H3A 110.3 . . ? O4 C3 H3B 110.3 . . ? C2 C3 H3A 110.3 . . ? C2 C3 H3B 110.3 . . ? H3A C3 H3B 108.6 . . ? O4 C5 N1 102.0(2) . . ? O4 C5 C6 110.0(2) . . ? O4 C5 C10 107.0(2) . . ? N1 C5 C6 110.6(2) . . ? N1 C5 C10 112.3(2) . . ? C6 C5 C10 114.1(2) . . ? C5 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C5 C6 C7 111.0(3) . . ? H6A C6 H6B 108.0 . . ? C7 C6 H6A 109.4 . . ? C7 C6 H6B 109.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C8 C7 C6 110.8(3) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 C9 110.5(3) . . ? H8A C8 H8B 108.1 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C8 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? C8 C9 C10 114.4(3) . . ? H9A C9 H9B 107.6 . . ? C10 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C5 C10 C9 108.9(2) . . ? C5 C10 H10 106.0 . . ? C5 C10 C11 110.5(2) . . ? C9 C10 H10 106.0 . . ? C11 C10 C9 118.7(2) . . ? C11 C10 H10 106.0 . . ? O1 C11 C10 111.0(2) . . ? O1 C11 C12 111.4(2) . . ? O1 C11 C16 107.8(2) . . ? C12 C11 C10 108.3(2) . . ? C16 C11 C10 111.2(2) . . ? C16 C11 C12 107.2(2) . . ? C11 C12 H12A 108.3 . . ? C11 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C13 C12 C11 116.0(2) . . ? C13 C12 H12A 108.3 . . ? C13 C12 H12B 108.3 . . ? O2 C13 N1 121.2(3) . . ? O2 C13 C12 120.0(2) . . ? N1 C13 C12 118.7(2) . . ? F1 C16 F2 106.2(3) . . ? F1 C16 F3 105.3(2) . . ? F1 C16 C11 114.1(3) . . ? F2 C16 F3 106.5(3) . . ? F2 C16 C11 112.5(2) . . ? F3 C16 C11 111.7(3) . . ? 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 F1 C16 1.331(4) . ? F2 C16 1.335(4) . ? F3 C16 1.335(4) . ? O1 C11 1.400(3) . ? O1 H1 0.99(5) . ? O2 C13 1.234(3) . ? O4 C3 1.426(4) . ? O4 C5 1.420(3) . ? N1 C2 1.462(4) . ? N1 C5 1.465(3) . ? N1 C13 1.322(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C3 1.513(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.520(4) . ? C5 C10 1.529(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C7 1.534(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.502(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C9 1.509(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C10 1.539(4) . ? C10 H10 0.9800 . ? C10 C11 1.536(4) . ? C11 C12 1.532(4) . ? C11 C16 1.523(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C13 1.505(4) . ? 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 O1 C11 C12 C13 -78.4(3) . . . . ? O1 C11 C16 F1 50.1(3) . . . . ? O1 C11 C16 F2 171.2(3) . . . . ? O1 C11 C16 F3 -69.1(3) . . . . ? O4 C5 C6 C7 66.4(3) . . . . ? O4 C5 C10 C9 -71.5(3) . . . . ? O4 C5 C10 C11 156.5(2) . . . . ? N1 C2 C3 O4 -1.6(5) . . . . ? N1 C5 C6 C7 178.3(2) . . . . ? N1 C5 C10 C9 177.4(2) . . . . ? N1 C5 C10 C11 45.3(3) . . . . ? C2 N1 C5 O4 33.5(3) . . . . ? C2 N1 C5 C6 -83.5(3) . . . . ? C2 N1 C5 C10 147.7(3) . . . . ? C2 N1 C13 O2 15.5(5) . . . . ? C2 N1 C13 C12 -162.1(3) . . . . ? C3 O4 C5 N1 -34.3(3) . . . . ? C3 O4 C5 C6 83.2(3) . . . . ? C3 O4 C5 C10 -152.4(3) . . . . ? C5 O4 C3 C2 23.0(4) . . . . ? C5 N1 C2 C3 -19.6(4) . . . . ? C5 N1 C13 O2 174.8(3) . . . . ? C5 N1 C13 C12 -2.8(5) . . . . ? C5 C6 C7 C8 56.0(4) . . . . ? C5 C10 C11 O1 63.0(3) . . . . ? C5 C10 C11 C12 -59.6(3) . . . . ? C5 C10 C11 C16 -177.1(2) . . . . ? C6 C5 C10 C9 50.4(3) . . . . ? C6 C5 C10 C11 -81.6(3) . . . . ? C6 C7 C8 C9 -56.9(4) . . . . ? C7 C8 C9 C10 56.5(4) . . . . ? C8 C9 C10 C5 -51.8(3) . . . . ? C8 C9 C10 C11 75.7(4) . . . . ? C9 C10 C11 O1 -63.8(3) . . . . ? C9 C10 C11 C12 173.7(3) . . . . ? C9 C10 C11 C16 56.2(4) . . . . ? C10 C5 C6 C7 -53.8(3) . . . . ? C10 C11 C12 C13 43.9(3) . . . . ? C10 C11 C16 F1 -71.7(3) . . . . ? C10 C11 C16 F2 49.3(4) . . . . ? C10 C11 C16 F3 169.1(2) . . . . ? C11 C12 C13 O2 169.0(3) . . . . ? C11 C12 C13 N1 -13.3(4) . . . . ? C12 C11 C16 F1 170.1(3) . . . . ? C12 C11 C16 F2 -68.9(3) . . . . ? C12 C11 C16 F3 50.9(3) . . . . ? C13 N1 C2 C3 143.0(3) . . . . ? C13 N1 C5 O4 -128.1(3) . . . . ? C13 N1 C5 C6 114.9(3) . . . . ? C13 N1 C5 C10 -13.9(4) . . . . ? C16 C11 C12 C13 163.9(3) . . . . ?