#------------------------------------------------------------------------------ #$Date: 2021-05-18 06:08:41 +0300 (Tue, 18 May 2021) $ #$Revision: 265286 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/26/1562622.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_1562622 loop_ _publ_author_name 'Chen, Xiao-Xian' 'Zhang, X. Y.' 'Liu, De-Xuan' 'Huang, Rui-Kang' 'Wang, Sha-Sha' 'Xiong, Li-Qun' 'Zhang, Wei-Xiong' 'Chen, Xiao-Ming' _publ_section_title ; Room-temperature ferroelectric and ferroelastic orders coexisting in a new tetrafluoroborate-based perovskite ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC01345A _journal_year 2021 _chemical_formula_moiety '0.25(B12 F48 K4), C5 H14 N2' _chemical_formula_sum 'C5 H14 B3 F12 K N2' _chemical_formula_weight 401.71 _space_group_crystal_system orthorhombic _space_group_IT_number 57 _space_group_name_Hall '-P 2c 2b' _space_group_name_H-M_alt 'P b c m' _atom_sites_solution_hydrogens geom _audit_creation_date 2020-02-22 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-03-04 deposited with the CCDC. 2021-05-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.5005(4) _cell_length_b 9.7685(4) _cell_length_c 14.0216(5) _cell_measurement_reflns_used 4371 _cell_measurement_temperature 338(2) _cell_measurement_theta_max 28.39 _cell_measurement_theta_min 3.49 _cell_volume 1438.25(10) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 338 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.77487 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 12852 _diffrn_reflns_point_group_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 27.705 _diffrn_reflns_theta_max 28.999 _diffrn_reflns_theta_min 2.115 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_correction_T_min 0.3586 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.855 _exptl_crystal_description block _exptl_crystal_F_000 800 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.334 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 1515 _refine_ls_number_restraints 165 _refine_ls_restrained_S_all 1.162 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0678 _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^)+(0.1700P)^2^+0.2800P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2200 _refine_ls_wR_factor_ref 0.2297 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1204 _reflns_number_total 1515 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc01345a3.cif _cod_data_source_block 338K _cod_database_code 1562622 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H,H) groups 2. Restrained distances F33A-B3 = F34-B3 = F34A-B3 = F31A-B3 = F32A-B3 = F31-B3 = F32-B3 = F33-B3 1.36 with sigma of 0.04 N1-C1 = N1-C5 = N2-C3 = N2-C2 1.49 with sigma of 0.02 C2-C1 = C4-C3 = C5-C4 1.53 with sigma of 0.02 F33A-F31A \\sim F33A-F34A \\sim F31A-F34A \\sim F33A-F32A \\sim F31A-F32A \\sim F34A-F32A \\sim F32- F31 \\sim F32-F34 \\sim F31-F34 \\sim F32-F33 \\sim F31-F33 \\sim F34-F33 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints F31 \\sim F31A \\sim F32 \\sim F32A \\sim F33 \\sim F33A \\sim F34 \\sim F34A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 4. Others Sof(F31A)=Sof(F32A)=Sof(F33A)=Sof(F34A)=0.5*(1-FVAR(2)) Sof(F31)=Sof(F32)=Sof(F33)=Sof(F34)=0.5*FVAR(2) Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) N2(0.5) H2A(0.5) H2B(0.5) C1(0.5) H1C(0.5) H1D(0.5) C2(0.5) H2C(0.5) H2D(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) 5.a Secondary CH2 refined with riding coordinates: N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B) ; _shelx_res_file ; 338k.res created by SHELXL-2014/7 TITL c_a.res in Pbcm REM Old TITL c in Pbcm REM SHELXT solution in Pbcm REM R1 0.233, Rweak 0.007, Alpha 0.046, Orientation as input REM Formula found by SHELXT: C7 B3 F31 K CELL 0.77487 10.5005 9.7685 14.0216 90 90 90 ZERR 4 0.0004 0.0004 0.0005 0 0 0 LATT 1 SYMM -X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM +X,0.5-Y,-Z SFAC C H B F K N DISP B 0.002 0.001 7.68 DISP C 0.004 0.002 13.872 DISP F 0.022 0.013 65.454 DISP H -0 0 0.627 DISP K 0.237 0.314 1346.215 DISP N 0.008 0.004 24.297 UNIT 20 56 12 48 4 8 DFIX 1.36 0.04 F33A B3 F34 B3 F34A B3 F31A B3 F32A B3 F31 B3 F32 B3 F33 B3 DFIX 1.49 N1 C1 N1 C5 N2 C3 N2 C2 DFIX 1.53 C2 C1 C4 C3 C5 C4 SADI 0.04 F33A F31A F33A F34A F31A F34A F33A F32A F31A F32A F34A F32A F32 = F31 F32 F34 F31 F34 F32 F33 F31 F33 F34 F33 SIMU 0.01 0.02 2 F31 > F34A SIMU N1 > C5 L.S. 50 PLAN 4 TEMP 0 CONN 24 B3 BOND $H list 4 fmap 2 acta OMIT -3 58 REM REM REM WGHT 0.170000 0.280000 FVAR 1.29084 0.59129 K1 5 0.245932 0.712626 0.250000 10.50000 0.04473 0.05273 = 0.05059 0.00000 0.00000 -0.00131 F11 4 0.111028 0.972056 0.250000 10.50000 0.06216 0.10123 = 0.08932 0.00000 0.00000 0.01582 F12 4 -0.033965 0.808856 0.250000 10.50000 0.12820 0.05515 = 0.17065 0.00000 0.00000 0.00197 F13 4 -0.072707 1.005716 0.328804 11.00000 0.08984 0.11113 = 0.10919 -0.01151 0.02738 0.02608 F21 4 0.171423 0.816790 0.435427 11.00000 0.08924 0.21394 = 0.07585 0.03177 -0.01542 0.02034 F22 4 0.322167 0.837348 0.551691 11.00000 0.09114 0.14863 = 0.09108 -0.02709 -0.01101 -0.00399 PART -1 F31 4 0.362135 0.434658 0.247904 20.50000 0.07631 0.13308 = 0.19842 -0.03667 -0.05869 0.03778 PART 0 PART -2 F31A 4 0.377126 0.380503 0.224967 -20.50000 0.08590 0.14775 = 0.19098 -0.03411 -0.05129 -0.00191 PART 0 PART -1 F32 4 0.510106 0.587822 0.248509 20.50000 0.11557 0.07252 = 0.20784 -0.04353 -0.05661 0.02225 PART 0 PART -2 F32A 4 0.465039 0.582663 0.248397 -20.50000 0.09777 0.09577 = 0.19974 -0.03962 -0.05546 0.05922 PART 0 PART -1 F33 4 0.552383 0.392218 0.174976 20.50000 0.08435 0.14964 = 0.16664 0.00201 -0.01299 0.01529 PART 0 PART -2 F33A 4 0.591234 0.409090 0.212969 -20.50000 0.08177 0.13080 = 0.15100 0.01135 0.00710 0.05733 PART 0 PART -1 F34 4 0.542383 0.388409 0.329881 20.50000 0.08925 0.08371 = 0.10414 0.01205 -0.03456 0.04604 PART 0 PART -2 F34A 4 0.492332 0.413268 0.352265 -20.50000 0.10564 0.11545 = 0.12796 0.04703 0.00854 0.03352 PART 0 B1 3 -0.017901 0.947183 0.250000 10.50000 0.05773 0.05428 = 0.07352 0.00000 0.00000 0.01458 B2 3 0.246288 0.750000 0.500000 10.50000 0.04546 0.14454 = 0.03867 -0.00198 0.00000 0.00000 B3 3 0.486041 0.448372 0.250000 10.50000 0.06007 0.06378 = 0.10938 0.00000 0.00000 0.01442 PART -1 N1 6 0.865324 0.842191 0.533909 10.50000 0.16124 0.16011 = 0.11937 -0.06258 0.01704 -0.09957 AFIX 23 H1A 2 0.931350 0.867150 0.569709 10.50000 -1.20000 H1B 2 0.855279 0.904779 0.488400 10.50000 -1.20000 AFIX 0 N2 6 0.682563 0.661733 0.419245 10.50000 0.19343 0.18802 = 0.19234 -0.07195 -0.02743 -0.03431 AFIX 23 H2A 2 0.652529 0.691960 0.363751 10.50000 -1.20000 H2B 2 0.665269 0.572555 0.420382 10.50000 -1.20000 AFIX 0 C1 1 0.892426 0.707066 0.489337 10.50000 0.04564 0.13136 = 0.14738 -0.01733 0.02758 0.02352 AFIX 23 H1C 2 0.981256 0.706201 0.470361 10.50000 -1.20000 H1D 2 0.881972 0.637276 0.537921 10.50000 -1.20000 AFIX 0 C2 1 0.817882 0.667942 0.408528 10.50000 0.18343 0.14583 = 0.12462 -0.03473 0.02150 -0.01774 AFIX 23 H2C 2 0.846896 0.578426 0.387928 10.50000 -1.20000 H2D 2 0.836488 0.731628 0.357312 10.50000 -1.20000 AFIX 0 C3 1 0.602219 0.716619 0.485549 10.50000 0.06449 0.08236 = 0.19108 -0.00994 -0.03691 -0.02893 AFIX 23 H3A 2 0.593324 0.650640 0.536818 10.50000 -1.20000 H3B 2 0.519139 0.726194 0.456048 10.50000 -1.20000 AFIX 0 C4 1 0.635829 0.850962 0.529231 10.50000 0.10280 0.09959 = 0.15733 -0.05277 -0.01767 0.05382 AFIX 23 H4A 2 0.564382 0.884336 0.566411 10.50000 -1.20000 H4B 2 0.653210 0.917041 0.479260 10.50000 -1.20000 AFIX 0 C5 1 0.751201 0.837333 0.592697 10.50000 0.09514 0.11345 = 0.08843 -0.05648 -0.01133 0.00116 AFIX 23 H5A 2 0.752672 0.911298 0.638841 10.50000 -1.20000 H5B 2 0.747805 0.751282 0.627124 10.50000 -1.20000 AFIX 0 HKLF 4 REM c_a.res in Pbcm REM R1 = 0.0678 for 1204 Fo > 4sig(Fo) and 0.0769 for all 1515 data REM 199 parameters refined using 165 restraints END WGHT 0.1542 0.2417 REM Highest difference peak 0.334, deepest hole -0.305, 1-sigma level 0.062 Q1 1 0.6369 0.6686 0.5372 11.00000 0.05 0.33 Q2 1 0.4827 0.2982 0.2500 10.50000 0.05 0.33 Q3 1 0.2396 0.7938 0.5620 11.00000 0.05 0.32 Q4 1 0.0586 0.8867 0.2500 10.50000 0.05 0.29 ; _shelx_res_checksum 97814 _shelx_hkl_file ; 0 1 0 0.20 0.20 0 -1 0 0.30 0.20 0 3 0 -0.70 0.60 0 -3 0 0.80 0.60 0 -4 0 1.70 0.90 0 4 0 2.40 1.00 0 -5 0 0.40 1.10 0 5 0 0.90 1.10 0 6 0 1211.98 68.79 0 -6 0 1247.88 68.89 0 -7 0 -0.90 1.60 0 -8 0 259.67 15.80 0 9 0 7.30 3.70 0 -9 0 -1.80 2.60 0 -10 0 182.68 12.90 0 10 0 179.18 13.70 0 -11 0 -4.90 5.20 0 11 0 -3.70 6.60 0 -12 0 88.19 11.70 0 12 0 68.99 12.20 0 -13 0 0.60 12.40 0 13 0 -1.20 15.00 1 0 0 22.00 1.60 -1 0 0 27.80 1.70 1 0 0 28.50 1.70 -1 -2 0 50.49 3.10 -1 2 0 48.50 3.10 1 2 0 47.10 3.10 1 -2 0 49.40 3.10 1 -5 0 715.93 42.50 1 5 0 743.93 42.60 -1 5 0 843.52 42.90 -1 -5 0 731.83 42.70 1 -6 0 3596.54 195.28 -1 -6 0 3561.14 195.38 1 6 0 3585.34 195.28 -1 6 0 3321.17 195.48 1 7 0 17.20 2.60 -1 7 0 18.60 3.10 1 -7 0 17.60 2.60 -1 -7 0 19.60 3.00 1 -8 0 11.90 2.70 -1 8 0 10.00 3.40 -1 -8 0 10.10 2.80 1 8 0 10.80 2.60 -1 -9 0 41.40 5.30 1 -9 0 43.30 5.10 -1 9 0 47.40 6.10 1 9 0 47.00 5.10 1 -10 0 0.10 3.70 -1 -10 0 5.40 4.30 -1 10 0 2.50 4.90 -1 11 0 115.39 13.10 1 -11 0 123.69 11.30 1 11 0 123.79 13.10 -1 -11 0 124.79 11.50 -1 -12 0 -0.60 8.00 1 -12 0 6.50 7.80 1 12 0 -0.20 9.10 -1 12 0 -7.40 9.40 -1 -13 0 24.70 13.40 1 13 0 24.50 23.60 -1 13 0 4.00 15.90 1 -13 0 11.80 12.30 1 13 0 22.00 15.80 -2 0 0 689.23 45.50 2 0 0 863.11 45.70 2 0 0 840.92 45.60 -2 0 0 875.71 45.70 2 1 0 1.70 0.80 2 1 0 4.00 1.20 -2 -1 0 1.80 0.90 -2 -1 0 5.30 1.30 -2 1 0 5.00 1.00 2 -1 0 5.30 0.90 2 -3 0 7.40 1.20 -2 -3 0 2.10 1.10 -2 3 0 7.20 1.20 2 3 0 5.30 1.10 2 4 0 8.90 1.50 -2 -4 0 11.80 1.70 -2 5 0 774.62 47.90 2 5 0 890.81 47.80 -2 -5 0 880.11 48.00 2 -5 0 856.41 47.70 2 6 0 246.18 14.30 2 -6 0 239.98 14.20 -2 -6 0 233.48 14.40 -2 7 0 10.10 2.90 2 -7 0 10.70 2.30 2 7 0 17.50 2.70 -2 -7 0 13.40 2.90 -2 -8 0 6.20 2.80 -2 8 0 8.80 3.20 2 -8 0 4.80 2.20 2 8 0 2.30 2.20 2 -9 0 50.99 5.40 -2 -9 0 53.69 6.00 -2 9 0 39.30 6.00 2 9 0 49.99 5.10 2 10 0 26.10 4.70 2 -10 0 16.90 4.60 -2 10 0 33.90 6.60 -2 -10 0 21.00 5.50 2 11 0 2.30 10.70 2 -11 0 -2.40 5.10 -2 -11 0 2.90 6.00 -2 11 0 3.70 7.70 2 12 0 24.20 10.10 -2 -12 0 20.80 9.10 2 -12 0 29.70 8.40 2 12 0 29.70 16.40 -2 12 0 9.80 10.40 -2 13 0 -6.90 17.40 2 -13 0 2.20 12.10 2 13 0 5.60 23.90 -2 -13 0 1.40 13.50 3 0 0 667.23 37.80 -3 0 0 629.24 37.80 3 0 0 723.43 37.70 -3 0 0 660.53 37.60 -3 2 0 51.79 3.90 3 2 0 59.49 4.40 3 2 0 63.49 3.90 -3 -2 0 54.99 3.90 -3 -2 0 54.49 4.30 3 -2 0 51.69 3.80 3 4 0 14.40 1.90 3 -4 0 8.00 1.70 -3 4 0 9.00 1.90 -3 -4 0 14.10 2.20 3 4 0 9.90 2.60 3 5 0 19.80 2.50 -3 -5 0 29.60 3.30 3 -5 0 19.70 2.20 -3 5 0 19.80 2.70 3 5 0 23.00 3.70 3 6 0 486.25 28.50 3 -6 0 485.65 27.10 3 6 0 491.55 27.30 -3 6 0 441.56 27.50 -3 -6 0 467.55 27.50 3 7 0 45.00 4.20 3 -7 0 44.90 4.00 3 7 0 56.29 7.10 -3 -7 0 53.09 5.30 -3 7 0 44.50 4.70 3 8 0 62.79 8.10 -3 8 0 54.59 6.20 -3 -8 0 50.29 5.70 3 -8 0 63.59 5.20 3 8 0 55.39 5.00 3 9 0 232.78 14.90 3 9 0 268.97 18.30 -3 -9 0 220.38 15.70 -3 9 0 245.28 16.00 3 -9 0 226.18 14.80 -3 -10 0 5.20 4.90 3 10 0 11.60 8.50 -3 10 0 8.20 5.90 3 -10 0 5.40 3.90 3 10 0 13.90 4.20 -3 -11 0 49.20 8.80 3 11 0 41.40 13.50 3 11 0 46.80 7.00 3 -11 0 36.90 7.20 -3 11 0 29.40 9.10 -3 -12 0 0.80 9.70 3 -12 0 -2.90 7.90 -3 12 0 2.90 11.90 3 12 0 -3.00 16.90 -4 0 0 4.00 1.30 -4 0 0 4.00 1.70 4 0 0 4.90 1.50 4 0 0 1.40 1.40 -4 -1 0 1785.92 104.29 4 -1 0 1962.40 104.09 4 -1 0 1862.91 103.89 4 1 0 1893.51 103.99 4 1 0 1947.31 104.39 -4 -1 0 1787.72 103.89 -4 1 0 1814.42 104.09 -4 2 0 3174.38 169.28 4 -2 0 3069.79 169.08 4 2 0 3073.69 169.68 4 2 0 2884.61 169.08 -4 -2 0 3062.29 169.58 -4 -2 0 2806.82 169.08 4 -2 0 3225.98 169.18 -4 -3 0 -0.40 1.40 -4 3 0 0.30 1.40 4 3 0 -0.30 2.00 4 3 0 -0.30 1.30 4 -3 0 0.70 1.30 4 4 0 64.09 4.60 -4 4 0 68.69 5.00 4 4 0 65.89 5.90 4 -4 0 68.59 4.80 -4 -4 0 57.89 4.90 4 -5 0 5.70 2.00 4 5 0 5.10 3.00 -4 5 0 5.00 2.20 4 5 0 4.20 1.80 -4 -5 0 0.30 1.90 -4 6 0 977.80 56.89 4 -6 0 1036.40 56.39 4 6 0 1004.50 57.99 -4 -6 0 980.30 56.89 4 6 0 1008.00 56.49 4 -7 0 57.69 4.80 -4 7 0 55.59 5.70 4 7 0 55.29 4.80 -4 -7 0 57.69 5.50 4 7 0 53.09 7.20 -4 8 0 156.28 10.80 -4 -8 0 130.19 10.40 4 8 0 145.39 12.40 4 8 0 129.59 9.40 4 -8 0 140.89 9.40 4 -9 0 66.39 6.50 4 9 0 65.39 10.30 4 9 0 75.49 6.40 -4 -9 0 63.99 7.60 -4 9 0 71.79 8.40 4 -10 0 64.29 7.20 -4 10 0 49.30 8.90 4 10 0 62.99 12.20 4 10 0 63.19 7.00 -4 -10 0 76.59 9.00 -4 -11 0 5.20 7.60 4 -11 0 5.40 6.10 -4 11 0 -3.30 8.80 4 11 0 -5.00 12.50 4 11 0 2.70 5.30 4 12 0 59.79 9.50 -4 -12 0 80.69 13.80 4 12 0 90.09 22.20 -4 12 0 59.89 16.20 4 -12 0 71.19 11.40 5 0 0 1787.22 94.69 5 0 0 1618.04 94.89 -5 0 0 1591.34 95.09 -5 0 0 1777.62 94.69 5 -1 0 1248.08 68.89 5 -1 0 1178.38 68.69 -5 1 0 1249.97 69.09 -5 -1 0 1178.98 68.69 5 1 0 1274.37 69.29 -5 -1 0 1200.28 69.29 5 1 0 1241.58 68.79 -5 -2 0 2258.47 128.09 5 2 0 2294.17 128.69 5 -2 0 2374.16 128.09 -5 -2 0 2212.48 128.69 5 2 0 2312.27 128.09 -5 2 0 2188.18 128.29 5 -2 0 2436.66 128.19 -5 -3 0 30.80 2.90 5 3 0 29.80 3.00 5 -3 0 32.30 3.00 -5 3 0 18.40 3.10 5 -3 0 17.10 2.80 5 3 0 30.50 4.40 -5 4 0 36.10 4.00 5 4 0 40.00 3.60 5 -4 0 33.40 3.60 5 4 0 49.20 5.70 -5 -4 0 36.60 3.90 5 -5 0 520.15 29.10 5 5 0 515.55 30.40 5 5 0 510.15 28.90 -5 5 0 483.55 29.30 -5 -5 0 474.55 29.20 5 6 0 117.09 8.20 5 -6 0 119.49 8.70 5 6 0 135.09 10.60 -5 -6 0 111.79 8.80 -5 6 0 129.79 9.00 -5 -7 0 159.38 10.80 5 7 0 164.38 10.10 5 -7 0 152.68 9.90 -5 7 0 129.99 10.90 5 7 0 134.49 12.30 5 -8 0 54.29 5.30 5 8 0 41.40 8.30 -5 8 0 49.10 6.70 -5 -8 0 47.60 6.50 5 8 0 53.79 5.20 5 9 0 6.90 3.50 -5 9 0 9.90 6.00 5 9 0 -1.10 7.80 -5 -9 0 4.10 5.20 5 -9 0 7.60 3.70 -5 10 0 -0.10 7.80 5 -10 0 0.30 4.40 5 10 0 -8.60 10.10 5 10 0 2.50 4.40 -5 -10 0 0.60 6.20 -5 11 0 84.29 14.10 -5 -11 0 80.79 11.90 5 11 0 66.99 8.60 5 11 0 69.49 17.50 5 -11 0 58.39 9.40 -5 -12 0 17.60 13.10 5 -12 0 0.90 9.40 -5 12 0 1.80 16.90 5 12 0 12.60 20.70 6 0 0 405.26 26.50 -6 0 0 493.15 27.40 -6 0 0 432.16 26.50 6 0 0 512.15 27.20 6 1 0 629.44 37.10 6 -1 0 622.04 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9.30 3 4 -7 128.49 8.70 3 5 7 1259.57 71.29 3 -5 -7 1209.48 71.39 -3 -5 7 1287.57 71.59 -3 5 7 1255.77 71.99 3 5 -7 1299.87 72.19 -3 -5 -7 1295.57 71.59 3 5 -7 1276.87 71.39 -3 -6 7 4.00 3.10 3 6 7 2.40 2.40 3 -6 -7 5.70 2.50 3 6 -7 0.30 3.60 -3 -6 -7 2.00 2.50 -3 6 7 3.00 3.30 3 6 -7 7.40 2.50 3 -7 -7 58.29 5.70 -3 -7 7 72.79 6.90 3 7 7 69.79 5.80 3 7 -7 66.29 5.60 -3 7 7 70.89 7.30 -3 -7 -7 63.19 6.20 3 -7 7 64.59 4.10 3 7 -7 60.39 7.80 -3 -8 7 7.60 4.90 3 -8 -7 3.60 3.10 -3 8 -7 3.30 2.90 3 8 7 4.00 3.10 -3 8 -7 3.40 3.20 -3 8 7 -0.30 4.20 3 -8 7 3.00 2.30 -3 -8 -7 2.30 3.70 3 8 -7 5.80 6.20 3 8 -7 0.60 2.80 -3 9 -7 172.08 13.20 -3 -9 7 212.78 15.60 3 -9 -7 223.28 13.40 -3 9 -7 153.38 13.50 -3 9 7 238.18 15.50 3 9 -7 200.98 17.80 -3 -9 -7 236.08 14.30 3 9 -7 187.88 13.00 3 -9 7 157.28 12.40 -3 -10 7 -2.00 8.60 -3 10 -7 1.60 6.10 3 -10 -7 -3.50 4.80 -3 10 -7 -1.90 6.90 3 10 -7 -3.20 10.70 3 -10 7 1.10 5.10 -3 -10 -7 1.30 5.60 3 10 -7 1.50 4.80 -3 10 7 -4.80 7.20 -3 11 -7 2.40 10.60 -3 -11 7 12.60 12.30 -3 11 -7 5.70 9.10 3 -11 -7 11.20 7.00 3 11 -7 -5.30 15.20 -3 -11 -7 15.40 8.20 3 11 -7 13.10 6.90 -4 0 -7 -0.50 1.40 4 0 7 0.00 2.00 4 0 7 -0.10 1.00 4 0 -7 -2.00 1.60 4 0 -7 2.70 2.10 -4 0 7 0.50 2.20 -4 1 -7 2018.80 109.59 4 -1 -7 1949.70 110.19 -4 -1 7 1910.61 110.59 4 1 7 1889.81 110.39 4 1 7 2048.40 109.59 4 1 -7 1982.50 110.29 4 -1 7 2030.80 109.39 -4 -1 -7 2005.80 109.89 4 1 -7 2021.90 110.19 -4 1 7 1888.91 110.39 4 -1 7 1899.51 109.89 4 2 7 1396.36 76.19 4 -2 -7 1333.97 76.69 -4 -2 7 1345.17 77.29 4 2 -7 1362.96 76.79 4 2 -7 1403.66 76.69 -4 2 7 1304.77 76.89 4 -2 7 1249.28 75.89 -4 -2 -7 1433.56 76.49 4 -2 7 1423.66 75.59 4 -3 -7 1.00 2.20 -4 -3 7 -0.10 2.90 4 3 7 0.30 1.50 4 3 -7 2.60 2.20 4 3 -7 -1.80 2.30 -4 3 7 -0.20 2.30 4 -3 7 0.50 0.50 4 -3 7 0.70 0.40 -4 -3 -7 0.30 1.90 -4 -4 7 1005.50 55.09 -4 -4 7 946.51 53.99 4 4 7 943.21 53.59 4 -4 -7 920.71 54.19 -4 -4 -7 925.31 53.89 4 4 -7 945.61 53.99 4 4 -7 996.10 54.59 -4 4 7 922.31 54.39 4 5 7 30.90 3.60 -4 -5 7 33.50 4.30 4 5 -7 28.70 4.90 -4 -5 -7 29.60 4.20 -4 5 7 28.10 4.70 4 5 -7 33.30 4.00 4 6 7 221.58 14.40 4 -6 -7 224.98 14.50 -4 -6 7 233.28 15.20 -4 -6 -7 222.08 14.80 4 6 -7 261.17 16.50 -4 6 7 245.18 15.60 4 6 -7 229.18 14.50 4 7 7 56.89 5.60 -4 -7 7 41.40 5.90 4 -7 -7 48.40 5.10 4 7 -7 39.00 4.90 -4 -7 -7 38.80 5.60 -4 7 7 33.30 6.10 4 7 -7 39.80 7.60 -4 -8 7 192.68 13.50 -4 8 -7 148.39 10.40 -4 8 -7 140.99 10.40 4 -8 -7 166.58 11.20 4 8 7 167.38 11.20 -4 -8 -7 180.48 12.10 4 -8 7 141.79 9.70 -4 8 7 188.68 13.30 4 -8 7 156.38 10.00 4 8 -7 176.38 15.40 4 8 -7 168.18 11.20 4 9 7 18.10 4.60 4 -9 -7 8.00 4.60 -4 9 -7 6.40 4.80 -4 -9 7 14.90 7.20 -4 9 -7 4.90 4.70 4 9 -7 9.50 9.40 4 -9 7 6.20 3.40 -4 9 7 9.30 6.60 4 9 -7 10.10 4.60 -4 -9 -7 11.80 5.50 4 -9 7 6.60 3.60 -4 -10 7 54.59 11.60 4 -10 -7 49.99 7.20 4 10 7 54.89 6.90 -4 10 -7 24.60 7.20 -4 10 -7 21.20 7.30 -4 -10 -7 64.69 9.00 4 10 -7 54.59 14.60 4 -10 7 27.60 5.50 -4 10 7 55.79 10.80 4 -11 -7 -3.60 6.80 -4 -11 7 6.70 14.30 4 11 -7 2.40 7.80 4 11 -7 3.40 17.70 5 0 7 0.00 1.30 5 0 -7 -0.50 2.00 -5 0 7 0.60 2.60 5 0 -7 -1.20 2.20 -5 0 -7 0.10 1.70 5 0 7 -0.90 2.50 5 -1 -7 15.70 3.20 -5 -1 7 18.80 4.10 -5 1 -7 18.50 2.60 5 1 7 15.60 2.30 5 1 7 17.40 3.80 5 -1 -7 18.90 3.30 5 1 -7 17.40 3.20 -5 1 7 12.80 3.60 5 -1 7 18.30 2.10 5 1 -7 18.40 3.40 5 -1 7 13.70 3.00 -5 -1 -7 15.90 2.90 5 2 7 80.09 5.20 5 -2 -7 79.59 6.30 5 2 7 68.79 7.00 -5 -2 7 62.39 7.10 5 -2 7 63.99 5.30 -5 2 7 68.19 6.50 5 -2 7 72.59 4.70 5 2 -7 75.29 6.00 -5 -2 -7 69.19 5.60 5 2 -7 68.69 6.30 5 3 7 480.75 27.60 -5 -3 7 489.75 29.30 5 3 7 484.35 29.20 5 -3 -7 476.25 28.30 5 3 -7 475.35 28.20 5 -3 7 448.46 27.20 5 -3 7 476.25 27.00 -5 -3 -7 505.45 28.20 5 3 -7 498.05 28.70 -5 3 7 466.55 28.60 5 4 7 14.70 4.90 5 -4 -7 8.10 3.40 5 4 7 10.70 2.50 -5 -4 7 13.30 3.20 -5 -4 7 8.80 4.60 -5 -4 -7 13.10 3.20 5 4 -7 13.90 3.30 -5 4 7 11.50 3.70 5 4 -7 13.50 4.10 5 -4 7 8.50 1.40 5 5 7 201.78 13.90 -5 -5 7 165.68 11.90 5 5 7 154.38 11.00 -5 -5 7 188.98 13.80 5 -5 -7 182.58 12.20 5 5 -7 175.78 11.70 5 -5 7 161.28 9.90 -5 5 7 154.78 12.30 -5 -5 -7 187.08 11.80 5 5 -7 184.08 13.10 -5 -6 7 20.10 4.80 5 6 7 18.30 3.60 -5 6 7 21.20 4.90 5 -6 7 16.90 1.80 5 -6 7 13.10 1.50 5 6 -7 17.50 6.00 -5 -6 -7 17.40 4.10 5 6 -7 19.80 4.00 5 7 7 503.75 27.70 -5 -7 7 473.65 28.90 -5 7 -7 397.16 26.50 5 -7 -7 497.95 27.80 5 7 -7 472.55 27.90 5 7 -7 480.45 30.40 5 -7 7 437.36 26.40 -5 7 7 487.55 29.20 -5 -7 -7 491.65 28.40 5 -8 -7 6.70 4.00 5 8 7 4.80 3.80 -5 -8 7 6.90 6.20 -5 8 -7 4.20 3.70 5 8 -7 9.60 4.60 5 -8 7 4.90 2.90 -5 8 7 -0.60 5.80 -5 -8 -7 12.40 5.30 5 8 -7 1.10 8.30 5 -8 7 3.30 2.20 5 9 7 56.39 6.70 -5 9 -7 32.70 6.10 -5 9 -7 34.00 5.60 5 9 7 48.00 12.80 -5 -9 7 71.09 10.50 5 9 -7 42.10 11.90 5 -9 7 31.20 4.90 -5 -9 -7 52.69 8.10 -5 9 7 75.39 10.30 5 -9 7 25.80 4.00 -5 10 -7 3.90 6.20 -5 -10 7 -0.20 10.80 5 -10 -7 1.50 5.80 5 10 7 -1.00 5.70 -5 10 -7 1.10 6.70 5 10 7 -7.20 14.80 -5 10 7 -4.00 9.40 5 -10 7 0.40 3.90 -5 -10 -7 0.60 7.50 5 10 -7 1.00 6.40 5 -10 7 0.40 4.80 5 10 -7 -0.50 14.60 -5 -11 7 25.10 16.20 5 11 -7 8.00 9.50 5 11 -7 10.50 20.80 6 0 -7 2.60 3.00 6 0 7 0.40 1.70 6 0 -7 -0.50 2.70 -6 0 7 2.50 3.60 6 0 7 -1.50 3.00 -6 0 -7 -0.70 2.20 -6 1 -7 27.00 3.60 -6 -1 7 39.70 5.90 6 1 7 29.90 5.20 6 -1 -7 34.80 4.70 6 1 7 35.50 3.60 6 -1 -7 27.60 4.20 6 -1 7 27.80 3.10 -6 1 7 20.80 4.70 -6 -1 -7 32.20 4.30 6 1 -7 28.90 4.60 6 -1 7 33.50 4.70 6 1 -7 33.20 4.50 6 -2 -7 538.85 33.00 6 2 7 583.74 34.10 6 -2 -7 543.25 32.90 6 2 7 560.34 32.20 -6 -2 7 609.14 34.30 6 2 -7 566.74 33.00 6 2 -7 576.74 33.30 6 -2 7 553.24 32.60 6 -2 7 568.04 32.00 -6 -2 -7 541.95 32.70 -6 2 7 541.05 33.50 -6 -3 7 -1.90 4.30 6 3 7 -1.60 1.80 6 3 7 1.10 4.30 6 -3 -7 -1.10 3.10 6 3 -7 -0.50 2.80 6 -3 7 -2.00 1.60 6 -3 7 0.90 2.10 6 3 -7 3.00 3.70 -6 -3 -7 -0.50 2.70 -6 3 7 4.50 3.70 6 4 7 346.47 22.60 -6 -4 7 364.96 23.00 -6 -4 7 381.66 21.20 6 4 7 334.07 20.20 6 -4 -7 317.17 21.00 -6 4 7 306.87 21.50 6 -4 7 309.97 19.80 6 4 -7 362.06 22.10 6 -4 7 326.17 19.70 6 4 -7 365.76 21.10 -6 -4 -7 347.27 21.00 -6 -5 7 58.09 6.60 -6 5 -7 47.20 5.30 -6 -5 7 61.49 8.90 6 -5 -7 51.79 6.50 6 5 7 68.69 9.20 6 5 7 49.90 5.10 6 5 -7 44.70 5.80 -6 5 7 54.29 7.10 6 5 -7 50.69 7.60 -6 -5 -7 55.49 6.30 6 -5 7 49.40 4.40 6 6 7 274.97 16.70 6 6 7 296.37 20.70 -6 -6 7 268.97 18.00 6 -6 -7 284.97 18.00 -6 6 -7 261.97 16.50 6 -6 7 243.88 15.80 -6 -6 -7 284.67 17.80 6 6 -7 306.57 19.70 6 -6 7 222.98 15.40 -6 6 7 296.37 18.70 6 6 -7 278.37 17.30 -6 -7 7 12.50 5.70 6 7 7 1.50 3.40 -6 7 -7 6.20 4.10 6 7 7 10.30 8.20 6 -7 -7 5.20 3.50 -6 7 7 2.40 5.60 -6 -7 -7 7.30 4.90 6 7 -7 -1.00 4.20 6 -7 7 4.30 2.00 6 -7 7 7.30 3.10 6 7 -7 7.70 7.10 -6 -8 7 57.19 9.60 6 8 7 98.39 14.40 6 8 7 64.59 7.10 6 -8 -7 68.89 7.20 -6 8 -7 44.10 6.80 6 8 -7 57.99 7.20 6 8 -7 46.40 11.10 -6 8 7 88.39 10.80 6 -8 7 57.29 6.20 6 -8 7 52.59 5.10 -6 -8 -7 82.59 9.30 6 -9 -7 -0.90 4.80 -6 9 -7 3.40 5.90 -6 -9 7 -5.60 9.20 6 9 7 0.10 5.10 6 9 7 1.60 12.80 6 -9 7 0.90 4.30 -6 9 7 -0.50 8.80 6 -9 7 1.30 3.20 6 9 -7 -0.50 5.30 -6 -9 -7 -1.40 7.00 6 9 -7 1.60 12.20 6 -10 -7 12.00 7.10 -6 -10 7 31.30 13.60 6 10 7 27.50 18.10 -6 -10 -7 6.80 9.50 6 10 -7 24.70 17.50 6 10 -7 20.60 8.20 7 0 -7 0.20 3.30 7 0 7 0.80 2.20 7 0 7 0.00 4.10 -7 0 -7 -0.40 2.80 7 0 -7 1.80 3.50 -7 0 7 -0.10 4.40 7 1 7 67.79 5.40 7 -1 -7 61.89 6.50 7 1 7 59.09 7.60 7 -1 -7 58.29 6.70 -7 -1 7 67.39 8.50 -7 1 -7 65.49 6.00 7 -1 7 47.70 6.50 7 1 -7 67.19 7.20 7 1 -7 65.99 6.60 -7 1 7 60.19 7.80 7 -1 7 74.29 5.50 -7 -1 -7 63.39 6.20 -7 -2 7 27.80 6.40 7 2 7 38.20 4.20 7 -2 -7 32.30 5.20 7 2 7 39.10 7.10 7 -2 -7 30.50 5.00 -7 -2 -7 33.80 5.10 7 2 -7 35.90 5.40 7 2 -7 36.60 5.90 -7 2 7 36.10 6.20 7 -2 7 28.90 4.70 7 -2 7 29.40 3.70 7 -3 -7 521.55 33.70 7 3 7 594.34 35.40 7 -3 -7 547.55 33.70 -7 -3 7 591.54 35.50 7 3 7 568.84 32.90 7 3 -7 585.04 33.80 7 -3 7 542.45 32.70 7 -3 7 568.94 33.20 -7 3 7 545.05 34.50 -7 -3 -7 618.64 33.80 7 3 -7 575.74 34.40 7 4 7 28.70 7.60 -7 -4 7 38.10 7.80 7 -4 -7 27.40 5.30 7 4 7 24.20 3.90 7 -4 7 19.70 3.90 -7 4 7 33.50 6.60 7 -4 7 19.50 3.50 7 4 -7 33.90 6.60 7 4 -7 24.70 5.10 -7 -4 -7 32.90 5.60 -7 5 -7 298.27 20.80 7 -5 -7 327.37 21.30 7 5 7 347.77 23.70 -7 -5 7 345.27 23.70 7 5 7 364.36 20.30 -7 -5 7 351.26 21.40 7 -5 7 320.17 19.80 7 5 -7 352.16 21.20 -7 5 7 306.77 22.00 7 5 -7 341.87 22.60 7 -5 7 292.17 19.80 -7 -5 -7 337.27 21.20 -7 6 -7 5.20 5.00 7 6 7 6.00 7.80 -7 -6 7 -0.60 5.00 7 -6 -7 3.60 5.10 7 6 7 -3.80 3.40 -7 6 7 0.80 6.10 -7 -6 -7 -0.80 4.50 7 6 -7 2.30 4.40 7 6 -7 4.10 6.90 7 -6 7 3.10 3.40 7 -6 7 2.10 2.30 -7 -7 7 140.19 13.00 7 7 7 157.78 17.40 -7 7 -7 107.59 11.50 7 7 7 138.89 10.20 -7 -7 -7 146.89 12.10 7 -7 7 106.39 9.80 7 7 -7 143.99 11.30 -7 7 7 126.79 13.40 7 7 -7 154.08 16.10 7 8 7 -5.00 11.80 7 8 7 5.30 5.00 7 -8 -7 0.80 4.80 -7 -8 7 0.70 8.20 -7 8 -7 1.60 6.50 7 -8 7 3.70 3.10 -7 -8 -7 4.80 7.10 -7 8 7 4.00 8.70 7 8 -7 10.30 11.30 7 8 -7 2.20 5.90 7 -8 7 1.90 4.60 -7 -9 7 27.70 11.60 7 -9 -7 29.50 6.80 -7 9 -7 12.00 8.00 7 9 7 31.90 16.50 7 9 -7 39.50 15.60 7 -9 7 13.50 5.60 -7 9 7 22.20 11.50 7 9 -7 39.40 8.50 7 -9 7 15.40 4.00 -7 -9 -7 52.39 10.40 -7 -10 7 11.30 16.50 7 10 -7 -1.20 9.30 7 10 -7 -5.10 19.60 -8 0 -7 2.20 3.80 -8 0 7 7.20 5.60 8 0 -7 0.80 3.30 8 0 7 0.40 5.30 8 0 -7 2.00 4.20 8 0 7 1.90 2.80 8 1 7 61.49 5.60 8 1 7 58.49 8.50 -8 -1 7 57.49 9.30 8 -1 -7 63.49 7.40 -8 1 -7 62.69 6.70 8 -1 -7 42.70 6.70 8 -1 7 58.79 5.80 -8 -1 -7 64.49 6.70 8 1 -7 77.19 7.70 8 -1 7 55.59 7.60 8 1 -7 62.39 7.70 -8 1 7 45.60 8.10 8 2 7 23.70 6.70 -8 -2 7 20.40 7.60 8 2 7 25.80 4.00 8 -2 -7 13.50 4.80 8 -2 -7 23.30 5.20 8 2 -7 15.70 4.80 -8 -2 -7 21.10 5.00 8 -2 7 19.60 3.90 8 2 -7 17.60 5.40 -8 2 7 20.10 6.50 8 -2 7 11.60 4.90 8 -3 -7 16.90 4.80 8 3 7 14.80 7.00 8 3 7 13.70 3.60 -8 -3 7 12.00 7.50 8 -3 -7 15.80 5.10 8 3 -7 18.80 6.20 8 -3 7 14.80 3.90 -8 3 7 18.90 6.40 -8 -3 -7 18.50 5.20 8 3 -7 23.10 5.30 8 -3 7 8.70 4.50 8 4 7 242.48 20.30 8 -4 -7 236.78 17.50 8 -4 -7 275.47 17.70 -8 -4 7 267.77 20.70 8 4 7 252.97 16.10 8 4 -7 276.17 19.20 8 -4 7 255.57 16.30 -8 4 7 246.48 18.70 8 -4 7 227.58 16.70 -8 -4 -7 275.17 17.80 8 4 -7 261.37 17.50 -8 -5 7 24.30 9.50 8 5 7 42.20 10.30 -8 5 -7 25.40 7.20 -8 -5 7 38.10 7.10 8 -5 -7 38.50 7.10 8 5 7 31.20 5.00 8 -5 -7 24.90 6.50 8 5 -7 26.70 8.20 -8 -5 -7 31.40 6.70 8 5 -7 37.40 6.50 8 -5 7 24.20 5.30 -8 5 7 22.80 7.60 8 -5 7 27.30 5.10 8 6 7 93.09 14.20 8 -6 -7 95.59 10.30 8 6 7 71.49 7.50 -8 6 -7 41.60 9.20 -8 -6 7 65.69 9.30 -8 -6 -7 80.09 9.60 -8 6 7 91.19 11.60 8 6 -7 61.79 8.40 8 6 -7 60.19 11.00 8 -6 7 67.39 7.50 8 7 7 12.50 5.20 -8 7 -7 3.10 8.30 -8 -7 7 19.90 8.00 8 -7 -7 17.80 7.60 8 7 7 11.20 11.80 8 7 -7 17.70 6.80 8 -7 7 5.00 3.60 -8 -7 -7 17.40 7.80 -8 7 7 6.50 9.00 8 7 -7 11.10 10.20 8 -7 7 13.10 5.60 8 -8 -7 56.09 7.90 -8 8 -7 35.10 10.10 -8 -8 7 67.19 11.70 8 8 7 81.59 8.40 8 8 7 37.10 15.80 -8 -8 -7 69.49 11.20 8 -8 7 45.90 7.40 8 8 -7 64.89 9.20 8 8 -7 54.19 14.60 -8 8 7 46.70 12.50 8 -8 7 41.60 5.40 8 -9 -7 1.60 7.20 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12.30 5 4 -15 3.00 8.90 5 4 -15 -7.30 9.80 -5 -4 -15 -2.30 8.60 5 5 15 33.00 18.40 5 5 15 38.80 13.10 5 -5 -15 42.80 8.30 5 5 -15 27.30 9.30 -5 -5 -15 45.20 11.40 5 5 -15 8.30 11.40 -5 5 15 31.60 14.70 5 6 15 3.00 22.30 5 6 15 0.90 14.00 -5 -6 -15 1.00 12.10 6 0 15 -4.60 6.80 6 0 15 0.60 8.80 6 0 -15 2.40 9.30 -6 0 -15 2.20 6.40 -6 0 15 -5.10 14.70 6 0 -15 2.80 9.50 6 -1 -15 1.30 9.40 6 1 15 -4.50 11.50 -6 -1 15 4.00 16.80 6 -1 -15 -3.80 9.10 6 1 15 0.90 9.00 -6 -1 -15 4.60 8.20 -6 1 15 1.40 14.50 6 1 -15 1.60 9.60 6 1 -15 6.40 9.60 6 2 15 -0.90 13.80 -6 -2 15 31.10 19.20 6 -2 -15 2.30 9.20 6 2 15 17.00 10.80 6 -2 -15 10.50 9.90 6 2 -15 6.40 10.20 -6 -2 -15 10.50 9.80 6 2 -15 8.50 9.90 -6 2 15 6.80 13.90 6 -3 -15 -2.90 10.10 6 3 15 -0.50 15.90 6 3 15 -0.20 11.30 -6 -3 15 -0.60 20.40 6 3 -15 2.10 10.00 6 3 -15 6.90 11.40 -6 -3 -15 -0.30 10.20 -6 3 15 7.20 14.60 6 4 15 6.10 18.60 -6 -4 15 20.70 22.20 6 -4 -15 20.40 7.50 6 4 15 8.40 12.30 -6 -4 -15 34.00 12.50 6 4 -15 11.10 12.80 -6 4 15 15.10 15.40 6 4 -15 22.80 11.60 -6 -5 15 -13.10 24.00 6 5 15 5.00 21.30 6 5 15 11.60 14.60 -6 -5 -15 4.30 13.50 6 5 -15 -9.60 14.40 6 5 -15 -4.00 10.40 7 0 15 -3.50 8.00 7 0 -15 3.40 11.00 -7 0 15 5.50 17.70 -7 0 -15 -3.50 7.80 7 0 15 -9.30 11.60 7 0 -15 -5.10 10.70 7 1 15 -2.90 13.50 7 -1 -15 17.80 11.10 7 1 15 5.60 10.50 -7 -1 15 5.30 18.80 7 -1 -15 2.30 11.10 7 1 -15 12.60 11.50 -7 -1 -15 -0.60 9.90 7 1 -15 2.30 11.40 -7 1 15 -3.70 17.40 7 -2 -15 8.80 11.90 7 2 15 -5.30 11.80 7 -2 -15 -5.30 11.10 -7 -2 15 6.20 22.70 7 2 15 -3.90 16.50 -7 -2 -15 9.90 11.60 -7 2 15 -0.80 16.90 7 2 -15 -9.50 11.90 7 2 -15 2.00 11.90 7 3 15 1.10 13.20 7 3 15 2.00 19.40 -7 -3 15 23.50 26.90 7 3 -15 2.30 12.30 -7 -3 -15 11.70 13.60 7 3 -15 8.10 14.20 -7 -4 15 -2.10 27.50 7 4 15 5.70 14.90 7 4 15 -4.50 21.50 -7 -4 -15 -11.20 14.30 7 4 -15 14.00 14.80 7 4 -15 1.60 15.70 -8 0 15 -6.70 21.60 8 0 -15 6.30 13.30 8 0 -15 1.10 13.10 -8 -1 15 -2.00 24.70 8 -1 -15 10.80 13.50 8 1 -15 -0.10 13.60 -8 -1 -15 -7.70 15.90 8 1 -15 -1.10 14.00 -8 -2 15 3.60 29.00 8 -2 -15 -4.60 13.30 8 2 -15 9.30 15.30 -8 -2 -15 2.90 15.80 8 2 -15 -8.00 15.50 -8 -3 15 -0.30 30.50 8 3 15 -7.10 18.60 -8 -3 -15 2.00 17.80 8 3 -15 3.70 16.70 8 3 -15 2.30 17.70 0 0 16 410.66 28.90 0 -1 -16 -2.20 4.50 0 1 16 -1.70 9.20 0 -1 16 -0.80 8.40 0 1 -16 -2.50 5.00 0 1 -16 1.90 3.80 0 2 -16 97.99 7.70 0 -2 16 114.09 11.30 0 2 -16 95.79 7.20 0 3 16 -0.20 9.90 0 -3 -16 -6.70 5.10 0 4 16 86.19 14.40 0 -4 -16 87.19 10.00 0 5 16 -4.70 11.50 0 -5 -16 -1.20 6.90 0 6 16 -1.50 13.90 0 -6 -16 8.30 8.60 1 0 16 2.80 8.50 1 0 -16 5.60 6.30 -1 0 -16 3.10 4.50 1 0 -16 2.60 4.40 -1 0 16 -2.60 9.70 1 1 16 351.46 23.40 -1 -1 16 353.46 24.80 -1 1 -16 268.07 18.10 -1 1 -16 259.27 18.50 -1 1 16 389.86 25.40 1 -1 16 289.27 21.20 1 1 -16 280.47 20.00 1 -2 -16 1.00 5.30 -1 -2 16 -5.70 8.70 1 2 16 -4.70 9.70 -1 -2 -16 -3.40 5.40 1 2 -16 -1.80 5.10 1 2 -16 0.80 3.50 -1 2 16 -3.60 10.20 1 -3 -16 103.89 9.60 -1 3 16 111.99 14.30 1 3 -16 56.19 4.80 1 3 -16 60.59 4.60 1 4 16 2.00 10.90 1 -4 -16 -8.90 5.70 -1 -4 -16 3.20 6.60 -1 4 16 0.20 10.90 1 5 16 5.50 11.80 1 -5 -16 6.10 7.30 -1 -5 -16 9.30 8.10 -1 5 16 4.40 12.80 1 6 16 -7.30 13.20 1 -6 -16 -0.40 8.10 -1 6 16 1.30 14.10 -1 -6 -16 -1.30 8.90 -2 0 -16 146.09 12.70 -2 0 16 251.07 21.30 2 0 -16 192.88 13.10 2 0 -16 176.58 15.20 2 0 16 162.98 16.20 -2 -1 16 2.40 11.50 2 1 16 8.20 9.00 -2 1 -16 1.60 3.40 -2 1 -16 4.80 3.50 2 -1 -16 3.40 5.30 -2 1 16 0.90 11.00 -2 -1 -16 6.80 5.50 2 -1 16 -1.40 5.60 2 -1 16 9.30 5.60 2 1 -16 4.30 4.60 2 1 -16 7.10 7.00 2 -2 -16 168.28 13.40 2 2 16 188.88 18.50 -2 -2 16 139.89 17.90 -2 -2 -16 181.98 14.20 -2 2 16 219.48 20.60 2 -3 -16 -4.70 5.30 2 3 16 -3.90 9.90 -2 -3 16 -7.90 9.60 2 3 -16 -3.10 5.00 -2 3 16 -0.20 10.70 -2 -3 -16 -2.20 6.30 2 3 -16 -0.10 3.40 2 4 16 24.80 11.30 2 -4 -16 51.59 7.80 -2 -4 -16 30.60 8.20 2 4 -16 15.80 2.50 2 4 -16 16.20 2.70 -2 4 16 35.50 12.90 2 5 16 -2.50 11.80 2 -5 -16 3.00 7.20 -2 5 16 -3.90 12.70 -2 -5 -16 2.20 8.20 2 6 16 -3.40 13.70 2 -6 -16 4.00 8.20 -2 -6 -16 2.40 9.50 3 0 -16 2.10 5.20 3 0 -16 4.50 7.50 3 0 16 3.00 8.10 -3 0 -16 3.20 5.10 3 0 16 0.50 7.20 -3 0 16 6.90 12.70 3 -1 -16 193.18 14.20 3 -1 -16 202.68 16.70 3 1 16 171.18 17.50 3 1 -16 184.08 16.30 -3 1 16 214.78 22.40 -3 -1 -16 158.78 14.30 3 2 16 -5.90 9.60 -3 -2 16 2.40 13.20 3 -2 -16 0.20 5.90 -3 2 16 -6.00 11.50 -3 -2 -16 4.50 6.70 3 2 -16 -0.10 4.90 3 2 -16 0.00 7.30 3 3 16 77.99 13.60 -3 -3 16 31.20 14.40 3 -3 -16 89.39 9.30 -3 3 16 47.10 14.00 -3 -3 -16 69.09 10.20 3 3 -16 51.89 9.00 3 4 16 0.50 11.80 3 -4 -16 3.70 6.60 -3 -4 -16 7.70 8.30 3 4 -16 3.40 5.50 3 4 -16 1.40 4.30 -3 4 16 3.60 13.00 3 5 16 -4.50 12.80 3 -5 -16 2.20 7.50 -3 -5 -16 8.30 9.80 -3 5 16 -0.40 13.70 3 -6 -16 -9.30 8.30 3 6 16 -2.30 15.30 -3 -6 -16 4.30 11.30 4 0 -16 61.89 7.90 -4 0 -16 50.39 7.40 -4 0 16 110.39 18.10 4 0 -16 73.09 11.00 4 0 16 30.10 9.70 4 0 16 48.40 8.70 -4 -1 16 16.20 16.20 4 1 16 5.80 10.80 4 -1 -16 1.50 5.70 4 -1 -16 -1.10 8.70 4 1 16 -6.50 8.90 -4 1 16 4.30 13.40 4 1 -16 3.60 8.60 -4 -1 -16 3.00 7.20 -4 -2 16 67.79 18.80 4 -2 -16 77.09 11.90 4 2 16 56.49 12.40 4 2 16 44.10 14.10 4 -2 -16 97.49 9.90 -4 -2 -16 69.29 10.50 -4 2 16 84.09 16.60 4 2 -16 59.79 11.00 4 -3 -16 3.50 6.60 4 3 16 10.30 12.20 -4 -3 16 -5.10 16.70 -4 3 16 8.90 14.00 4 3 -16 6.80 8.70 -4 -3 -16 0.30 8.50 4 4 16 12.30 13.10 -4 -4 16 27.90 16.80 4 -4 -16 22.90 7.50 -4 -4 -16 33.80 10.80 4 4 -16 11.10 8.00 -4 4 16 19.70 15.00 4 -5 -16 -2.50 8.00 4 5 16 -4.50 14.80 -4 -5 -16 12.60 12.00 -4 -6 -16 10.60 12.90 5 0 16 2.20 7.10 5 0 16 3.80 8.80 -5 0 -16 0.90 5.80 -5 0 16 -0.80 16.90 5 0 -16 -3.40 9.60 5 -1 -16 56.19 11.60 5 1 16 19.10 12.80 5 1 16 32.30 10.50 -5 -1 16 62.69 20.30 -5 1 16 68.29 18.20 5 1 -16 45.30 11.60 5 1 -16 37.80 11.40 -5 -1 -16 41.60 9.60 -5 -2 16 -5.80 19.30 5 2 16 3.40 11.70 5 -2 -16 2.40 7.00 5 2 16 7.50 14.10 5 -2 -16 4.10 10.10 -5 -2 -16 4.20 9.80 5 2 -16 6.90 10.30 5 2 -16 6.80 11.20 -5 2 16 3.60 15.90 5 3 16 17.30 13.40 -5 -3 16 37.90 23.00 5 3 16 5.80 16.50 5 -3 -16 50.29 8.70 5 -3 -16 42.10 12.70 5 3 -16 25.00 12.30 -5 -3 -16 36.00 11.70 5 3 -16 16.70 10.60 -5 3 16 23.80 16.50 -5 -4 16 -1.80 22.40 5 -4 -16 2.90 7.90 5 4 16 11.30 19.10 5 4 16 2.20 14.00 5 4 -16 -9.00 10.00 5 4 -16 1.00 12.60 -5 4 16 -6.40 17.50 -5 -4 -16 -2.70 11.90 5 5 16 0.10 15.90 5 5 16 -8.80 23.00 -5 -5 -16 24.90 13.90 6 0 -16 40.40 13.70 -6 0 -16 9.90 7.40 6 0 -16 35.50 12.40 -6 0 16 35.70 21.80 6 1 16 1.50 12.40 6 -1 -16 2.90 11.90 -6 -1 16 -14.80 20.80 6 1 -16 -7.00 11.90 -6 1 16 -1.80 18.40 6 1 -16 9.30 12.00 -6 -1 -16 -0.60 9.90 -6 -2 16 21.40 23.20 6 -2 -16 21.70 12.70 6 2 16 12.40 13.50 6 2 16 10.10 17.20 -6 -2 -16 41.90 13.10 -6 2 16 15.70 18.50 6 2 -16 39.30 14.00 6 2 -16 26.00 13.90 -6 -3 16 5.30 26.30 6 3 16 -10.60 14.80 6 3 16 -11.30 19.10 6 -3 -16 1.50 8.00 6 -3 -16 5.70 12.70 6 3 -16 17.10 13.80 -6 -3 -16 6.00 13.60 6 3 -16 8.20 14.60 6 4 16 9.70 16.70 6 4 16 39.10 24.50 -6 -4 -16 19.80 15.30 6 4 -16 10.00 16.50 6 4 -16 29.40 13.60 -7 0 16 13.30 25.60 7 0 -16 -4.80 14.30 7 0 -16 -8.90 13.50 7 -1 -16 37.20 15.60 7 -1 -16 55.69 17.20 -7 -1 16 30.60 27.30 7 1 -16 49.30 16.80 7 1 -16 12.00 14.80 -7 1 16 50.99 25.30 -7 -2 16 2.10 28.70 7 2 -16 -2.20 15.90 7 2 -16 9.00 15.70 0 0 -17 0.30 5.40 0 0 -17 -2.40 6.60 0 0 17 4.20 11.70 0 -1 -17 -0.20 6.20 0 1 -17 -2.20 4.40 0 1 17 5.00 12.70 0 -1 17 -1.60 10.40 0 1 -17 2.10 5.90 0 -2 17 0.70 5.30 0 -2 -17 8.90 7.20 0 2 17 -2.80 13.10 0 -3 -17 -4.80 7.40 0 3 17 -3.50 13.60 0 4 17 6.10 14.60 0 -4 -17 15.10 8.50 0 5 17 -15.20 16.20 0 -5 -17 -5.10 9.00 -1 0 -17 -2.00 6.20 1 0 -17 -0.20 5.60 1 0 -17 0.10 7.50 1 0 17 -1.60 10.40 -1 0 -17 -2.30 5.50 -1 0 17 -4.40 12.50 1 -1 -17 -2.00 6.10 -1 1 -17 1.40 4.60 1 1 17 -3.50 11.50 -1 -1 17 -1.00 12.50 -1 1 -17 3.20 3.90 1 -1 17 -4.40 8.10 -1 -1 -17 -0.30 6.20 1 1 -17 -1.20 6.90 -1 1 17 -0.40 13.50 1 1 -17 -2.60 4.70 1 2 17 -7.00 12.80 -1 -2 17 -0.90 10.20 1 -2 -17 1.60 6.80 1 2 -17 -3.10 3.70 -1 -2 -17 -3.30 6.80 1 2 -17 2.60 5.40 -1 2 17 -1.10 13.80 1 3 17 12.80 14.50 1 -3 -17 9.40 7.70 -1 3 17 10.70 13.90 -1 -3 -17 12.80 8.10 1 4 17 -2.10 14.40 1 -4 -17 -3.40 8.30 -1 -4 -17 -5.80 8.40 -1 4 17 -11.10 14.60 1 5 17 34.20 18.00 1 -5 -17 35.70 10.00 -1 5 17 11.40 17.00 -1 -5 -17 40.20 11.30 -2 0 17 1.40 15.00 -2 0 -17 1.50 5.50 2 0 -17 0.80 5.90 2 0 -17 -3.60 8.30 2 -1 -17 -2.50 6.50 2 -1 -17 3.50 9.00 2 1 17 3.20 10.90 -2 -1 17 -5.60 14.30 -2 1 17 -5.30 14.80 2 -1 17 -1.00 4.60 2 1 -17 1.80 8.10 -2 -1 -17 3.00 6.70 2 1 -17 4.90 5.60 2 -1 17 -2.60 4.30 2 2 17 0.30 12.70 -2 -2 17 -2.10 13.30 2 -2 -17 3.90 7.10 2 2 -17 6.30 7.30 2 2 -17 0.20 4.70 -2 2 17 8.10 15.40 -2 -2 -17 5.40 7.80 2 3 17 -10.20 13.80 2 -3 -17 3.80 7.40 -2 -3 -17 -3.80 8.70 -2 3 17 -1.80 15.00 2 3 -17 -4.40 3.90 2 3 -17 4.00 5.60 2 4 17 7.50 15.20 2 -4 -17 7.10 8.20 -2 4 17 2.00 16.00 -2 -4 -17 16.20 10.10 2 -5 -17 0.30 9.10 2 5 17 2.50 16.50 -2 -5 -17 6.00 11.00 3 0 -17 5.80 10.00 3 0 17 4.50 9.20 -3 0 17 -0.40 17.10 3 0 17 -5.00 8.40 -3 0 -17 3.30 6.20 3 0 -17 -3.40 6.80 -3 -1 17 -2.80 16.50 3 -1 -17 4.10 7.00 3 1 17 6.60 11.30 3 -1 -17 14.60 10.40 3 1 17 -4.20 11.80 3 1 -17 1.60 9.40 -3 1 17 10.20 16.40 3 1 -17 6.50 6.60 -3 -1 -17 6.70 7.40 -3 -2 17 3.70 16.80 3 -2 -17 4.40 7.30 3 2 17 -7.70 12.50 3 2 -17 2.60 6.10 3 2 -17 4.00 9.00 -3 -2 -17 8.80 8.80 -3 2 17 -16.50 16.50 3 -3 -17 9.80 8.10 3 3 17 15.30 15.00 3 3 -17 12.60 6.10 -3 -3 -17 12.30 10.50 -3 3 17 7.00 17.00 3 3 -17 9.70 8.40 3 -4 -17 2.20 8.50 3 4 17 -7.50 14.90 -3 4 17 -2.60 17.70 -3 -4 -17 -6.50 10.50 3 -5 -17 32.40 10.30 3 5 17 29.10 17.90 -3 -5 -17 41.80 13.60 4 0 -17 3.60 11.40 -4 0 17 6.00 19.20 -4 0 -17 1.80 6.50 4 0 -17 6.10 7.60 4 1 17 -0.90 11.20 4 -1 -17 1.60 7.50 4 1 17 1.00 13.80 4 -1 -17 -5.20 11.10 -4 -1 17 6.00 20.70 4 1 -17 3.70 10.80 4 1 -17 0.00 7.40 -4 -1 -17 6.10 9.20 -4 1 17 8.00 19.50 -4 -2 17 -0.70 20.90 4 2 17 -1.30 13.50 4 -2 -17 11.50 11.80 4 -2 -17 21.00 8.20 4 2 17 -2.90 15.50 -4 2 17 14.60 18.30 4 2 -17 16.60 11.20 4 2 -17 9.90 7.50 -4 -2 -17 8.90 10.10 4 -3 -17 -3.00 8.30 4 3 17 -14.10 15.00 4 3 17 3.50 19.60 -4 3 17 1.40 19.10 -4 -3 -17 5.90 10.90 4 3 -17 10.50 10.80 4 3 -17 4.20 7.70 4 -4 -17 38.10 10.40 4 4 17 21.30 18.20 -4 -4 -17 45.50 14.60 -5 0 17 -5.70 22.90 5 0 -17 7.10 8.70 5 0 -17 12.10 13.30 5 -1 -17 -0.10 13.40 -5 -1 17 20.30 25.00 5 -1 -17 5.70 8.60 -5 1 17 2.80 21.30 5 1 -17 4.60 13.10 5 -2 -17 1.30 13.90 -5 -2 17 3.60 25.80 5 -2 -17 -0.20 8.60 5 2 -17 9.50 13.00 -5 2 17 4.20 21.60 -5 -2 -17 14.60 13.20 5 -3 -17 28.90 10.60 5 -3 -17 57.89 17.40 -5 -3 -17 43.00 15.90 -6 0 17 6.30 27.90 6 0 -17 3.80 16.40 -6 -1 17 -7.20 28.20 6 -1 -17 7.70 16.90 -6 1 17 -2.00 26.40 6 1 -17 -11.30 15.70 6 1 -17 0.60 16.20 0 0 -18 22.20 7.70 0 0 -18 12.90 9.20 0 1 18 -6.70 16.30 0 -1 -18 -6.30 7.80 0 2 18 -17.00 17.80 0 -2 -18 2.60 8.70 0 3 18 3.80 18.80 0 -3 -18 -8.60 9.90 0 -4 -18 -8.20 11.30 0 4 18 -1.00 21.70 1 0 -18 4.80 7.20 -1 0 -18 2.60 8.30 -1 0 -18 -2.30 7.10 1 0 -18 10.80 9.90 -1 0 18 5.90 16.90 1 1 18 5.10 15.00 1 -1 -18 5.40 10.50 1 -1 -18 11.60 8.20 1 1 -18 4.90 6.60 -1 -1 -18 4.30 8.60 -1 1 18 14.30 18.50 1 1 -18 6.80 9.20 1 -2 -18 4.60 8.70 1 2 18 1.10 16.90 -1 2 18 -3.40 18.30 -1 -2 -18 2.00 9.30 1 -3 -18 15.20 10.10 1 3 18 12.20 19.80 -1 -3 -18 12.50 10.40 -1 3 18 15.10 20.00 1 -4 -18 0.00 10.50 1 4 18 -6.20 20.90 -1 4 18 -12.70 20.20 -1 -4 -18 -1.00 12.20 2 0 -18 8.10 10.90 2 0 -18 12.40 8.00 -2 0 18 3.00 19.20 2 -1 -18 0.10 8.10 2 -1 -18 3.20 11.50 2 1 -18 1.40 7.30 -2 1 18 -17.80 18.80 2 1 -18 1.70 10.40 -2 -1 -18 0.00 9.40 2 2 18 0.10 23.00 2 -2 -18 15.20 9.30 -2 2 18 1.70 20.90 -2 -2 -18 11.40 10.80 2 -3 -18 -3.50 9.40 2 3 18 0.70 18.80 -2 -3 -18 5.00 11.70 -2 3 18 7.60 21.30 3 0 -18 -9.20 8.60 -3 0 18 4.20 22.50 3 0 -18 -5.40 12.80 3 -1 -18 6.90 13.60 3 -1 -18 15.10 9.30 3 1 -18 19.50 9.00 -3 1 18 15.60 22.50 3 1 -18 7.50 12.40 3 -2 -18 -0.70 9.60 3 -2 -18 5.30 15.50 -3 -2 -18 5.30 15.10 -3 2 18 -2.20 22.30 3 -3 -18 22.80 10.80 -3 -3 -18 3.40 13.70 -3 3 18 13.80 25.00 -4 0 18 31.90 28.30 4 0 -18 30.70 11.00 4 0 -18 14.80 15.30 4 -1 -18 8.00 10.00 4 -1 -18 2.30 15.80 4 1 -18 5.40 17.30 -4 1 18 8.70 25.80 4 1 -18 -4.80 9.90 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 69295 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.24593(6) 0.71263(8) 0.2500 0.0493(4) Uani 1 2 d S T P A . F11 F 0.1110(3) 0.9721(3) 0.2500 0.0842(9) Uani 1 2 d S T P A . F12 F -0.0340(4) 0.8089(3) 0.2500 0.1180(14) Uani 1 2 d S T P A . F13 F -0.0727(2) 1.0057(2) 0.32880(17) 0.1034(9) Uani 1 1 d . . . . . F21 F 0.1714(2) 0.8168(3) 0.43543(18) 0.1263(13) Uani 1 1 d . . . . . F22 F 0.3222(2) 0.8373(3) 0.55169(18) 0.1103(9) Uani 1 1 d . . . . . F31 F 0.3621(10) 0.4347(16) 0.248(2) 0.136(4) Uani 0.296(13) 1 d D U . A -1 F31A F 0.3771(19) 0.381(3) 0.2250(18) 0.142(7) Uani 0.204(13) 1 d D U . A -2 F32 F 0.5101(16) 0.5878(11) 0.249(2) 0.132(4) Uani 0.296(13) 1 d D U . A -1 F32A F 0.4650(19) 0.5827(18) 0.248(3) 0.131(4) Uani 0.204(13) 1 d D U . A -2 F33 F 0.552(3) 0.392(3) 0.175(2) 0.134(7) Uani 0.296(13) 1 d D U . A -1 F33A F 0.5912(18) 0.409(3) 0.2130(18) 0.121(6) Uani 0.204(13) 1 d D U . A -2 F34 F 0.542(3) 0.3884(17) 0.3299(18) 0.092(5) Uani 0.296(13) 1 d D U . A -1 F34A F 0.492(2) 0.413(3) 0.3523(13) 0.116(6) Uani 0.204(13) 1 d D U . A -2 B1 B -0.0179(5) 0.9472(5) 0.2500 0.0618(12) Uani 1 2 d S T P . . B2 B 0.2463(4) 0.7500 0.5000 0.0762(16) Uani 1 2 d S T P A . B3 B 0.4860(6) 0.4484(6) 0.2500 0.0777(16) Uani 1 2 d DS T P . . N1 N 0.8653(13) 0.8422(17) 0.5339(12) 0.147(6) Uani 0.5 1 d D U . B -1 H1A H 0.9313 0.8671 0.5697 0.176 Uiso 0.5 1 calc R . . B -1 H1B H 0.8553 0.9048 0.4884 0.176 Uiso 0.5 1 calc R . . B -1 N2 N 0.6826(12) 0.662(2) 0.4192(14) 0.191(9) Uani 0.5 1 d D U . B -1 H2A H 0.6525 0.6920 0.3638 0.230 Uiso 0.5 1 calc R . . B -1 H2B H 0.6653 0.5726 0.4204 0.230 Uiso 0.5 1 calc R . . B -1 C1 C 0.8924(9) 0.7071(15) 0.4893(12) 0.108(6) Uani 0.5 1 d D U . B -1 H1C H 0.9813 0.7062 0.4704 0.130 Uiso 0.5 1 calc R . . B -1 H1D H 0.8820 0.6373 0.5379 0.130 Uiso 0.5 1 calc R . . B -1 C2 C 0.8179(12) 0.668(2) 0.4085(14) 0.151(7) Uani 0.5 1 d D U . B -1 H2C H 0.8469 0.5784 0.3879 0.182 Uiso 0.5 1 calc R . . B -1 H2D H 0.8365 0.7316 0.3573 0.182 Uiso 0.5 1 calc R . . B -1 C3 C 0.6022(9) 0.7166(8) 0.4855(11) 0.113(6) Uani 0.5 1 d D U . B -1 H3A H 0.5933 0.6506 0.5368 0.135 Uiso 0.5 1 calc R . . B -1 H3B H 0.5191 0.7262 0.4560 0.135 Uiso 0.5 1 calc R . . B -1 C4 C 0.6358(14) 0.8510(14) 0.5292(13) 0.120(5) Uani 0.5 1 d D U . B -1 H4A H 0.5644 0.8843 0.5664 0.144 Uiso 0.5 1 calc R . . B -1 H4B H 0.6532 0.9170 0.4793 0.144 Uiso 0.5 1 calc R . . B -1 C5 C 0.7512(8) 0.8373(19) 0.5927(11) 0.099(4) Uani 0.5 1 d D U . B -1 H5A H 0.7527 0.9113 0.6388 0.119 Uiso 0.5 1 calc R . . B -1 H5B H 0.7478 0.7513 0.6271 0.119 Uiso 0.5 1 calc R . . B -1 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 K1 0.0447(6) 0.0527(6) 0.0506(6) 0.000 0.000 -0.0013(3) F11 0.0622(16) 0.101(2) 0.0893(19) 0.000 0.000 0.0158(14) F12 0.128(3) 0.0552(16) 0.171(4) 0.000 0.000 0.0020(15) F13 0.0898(16) 0.1111(17) 0.1092(18) -0.0115(13) 0.0274(12) 0.0261(12) F21 0.0892(16) 0.214(4) 0.0758(12) 0.0318(17) -0.0154(11) 0.0203(17) F22 0.0911(17) 0.149(2) 0.0911(14) -0.0271(16) -0.0110(11) -0.0040(15) F31 0.076(5) 0.133(7) 0.198(9) -0.037(11) -0.059(9) 0.038(4) F31A 0.086(8) 0.148(12) 0.191(15) -0.034(12) -0.051(10) -0.002(8) F32 0.116(9) 0.073(4) 0.208(7) -0.044(9) -0.057(12) 0.022(5) F32A 0.098(8) 0.096(6) 0.200(7) -0.040(9) -0.055(11) 0.059(5) F33 0.084(11) 0.150(12) 0.167(14) 0.002(12) -0.013(10) 0.015(10) F33A 0.082(9) 0.131(9) 0.151(15) 0.011(9) 0.007(8) 0.057(8) F34 0.089(11) 0.084(6) 0.104(9) 0.012(6) -0.035(9) 0.046(7) F34A 0.106(13) 0.115(12) 0.128(11) 0.047(9) 0.009(9) 0.034(9) B1 0.058(3) 0.054(2) 0.074(3) 0.000 0.000 0.0146(19) B2 0.045(3) 0.145(5) 0.039(2) -0.002(3) 0.000 0.000 B3 0.060(3) 0.064(3) 0.109(5) 0.000 0.000 0.014(2) N1 0.161(11) 0.160(13) 0.119(8) -0.063(8) 0.017(8) -0.100(10) N2 0.19(2) 0.188(14) 0.192(19) -0.072(14) -0.027(15) -0.034(16) C1 0.046(3) 0.131(15) 0.147(14) -0.017(13) 0.028(7) 0.024(4) C2 0.183(19) 0.146(11) 0.125(12) -0.035(10) 0.022(14) -0.018(15) C3 0.064(4) 0.082(13) 0.191(18) -0.010(12) -0.037(9) -0.029(5) C4 0.103(9) 0.100(10) 0.157(11) -0.053(10) -0.018(8) 0.054(7) C5 0.095(9) 0.113(9) 0.088(7) -0.056(7) -0.011(7) 0.001(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 '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' B B 0.0020 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0220 0.0130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2370 0.3140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0080 0.0040 '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 F11 K1 F12 43.06(8) . . ? F11 K1 F13 107.38(7) . 8 ? F11 K1 F13 107.38(7) . 3_545 ? F11 K1 F22 106.16(5) . 7_575 ? F11 K1 F22 106.16(5) . 4_566 ? F11 K1 F31 175.0(3) . . ? F11 K1 F32 142.9(2) . . ? F11 K1 B2 84.84(3) . . ? F12 K1 B2 88.25(6) . . ? F13 K1 F12 67.64(7) 8 . ? F13 K1 F12 67.64(7) 3_545 . ? F13 K1 F13 44.23(9) 3_545 8 ? F13 K1 F31 67.8(3) 3_545 . ? F13 K1 F31 68.3(4) 8 . ? F13 K1 F32 107.0(3) 8 . ? F13 K1 F32 106.7(3) 3_545 . ? F13 K1 B2 72.40(6) 8 . ? F13 K1 B2 116.51(6) 3_545 . ? F21 K1 F11 64.03(5) . . ? F21 K1 F11 64.03(5) 6_556 . ? F21 K1 F12 68.66(5) . . ? F21 K1 F12 68.66(5) 6_556 . ? F21 K1 F13 74.74(8) . 8 ? F21 K1 F13 114.33(8) 6_556 8 ? F21 K1 F13 114.33(8) . 3_545 ? F21 K1 F13 74.74(8) 6_556 3_545 ? F21 K1 F21 127.45(10) . 6_556 ? F21 K1 F22 44.14(7) . 4_566 ? F21 K1 F22 169.01(7) 6_556 4_566 ? F21 K1 F22 44.14(7) 6_556 7_575 ? F21 K1 F22 169.01(7) . 7_575 ? F21 K1 F31 114.9(6) 6_556 . ? F21 K1 F31 116.1(6) . . ? F21 K1 F32 113.2(6) . . ? F21 K1 F32 112.5(6) 6_556 . ? F21 K1 B2 148.85(6) 6_556 . ? F21 K1 B2 21.89(7) . . ? F22 K1 F12 108.09(5) 4_566 . ? F22 K1 F12 108.09(5) 7_575 . ? F22 K1 F13 72.41(7) 4_566 8 ? F22 K1 F13 72.41(7) 7_575 3_545 ? F22 K1 F13 114.28(7) 4_566 3_545 ? F22 K1 F13 114.28(7) 7_575 8 ? F22 K1 F22 142.73(9) 4_566 7_575 ? F22 K1 F31 75.3(6) 4_566 . ? F22 K1 F31 74.2(6) 7_575 . ? F22 K1 F32 71.1(6) 7_575 . ? F22 K1 F32 71.9(6) 4_566 . ? F22 K1 B2 22.25(7) 4_566 . ? F22 K1 B2 163.62(8) 7_575 . ? F31 K1 F12 131.9(3) . . ? F31 K1 F32 42.1(3) . . ? F31 K1 B2 96.0(6) . . ? F32 K1 F12 174.0(2) . . ? F32 K1 B2 92.7(6) . . ? F32A K1 F11 148.1(5) . . ? F32A K1 F12 168.8(5) . . ? F32A K1 F13 101.9(6) . 3_545 ? F32A K1 F13 102.3(6) . 8 ? F32A K1 F21 114.4(10) . . ? F32A K1 F21 113.5(10) . 6_556 ? F32A K1 F22 71.9(10) . 4_566 ? F32A K1 F22 70.9(10) . 7_575 ? F32A K1 B2 93.3(10) . . ? B1 F11 K1 109.0(3) . . ? B1 F12 K1 100.6(3) . . ? B1 F13 K1 104.12(19) . 3 ? B2 F21 K1 105.76(17) . . ? B2 F22 K1 103.79(16) . 7_576 ? B3 F31 K1 108.3(9) . . ? B3 F32 K1 103.2(9) . . ? B3 F32A K1 128.4(13) . . ? F11 B1 K1 122.5(3) . 3 ? F12 B1 K1 130.2(3) . 3 ? F12 B1 F11 107.3(4) . . ? F12 B1 F13 111.2(3) . 6_556 ? F12 B1 F13 111.2(3) . . ? F13 B1 K1 53.75(17) . 3 ? F13 B1 K1 53.75(17) 6_556 3 ? F13 B1 F11 109.8(3) . . ? F13 B1 F11 109.8(3) 6_556 . ? F13 B1 F13 107.4(3) 6_556 . ? K1 B2 K1 179.88(13) 7_576 . ? F21 B2 K1 52.35(13) . . ? F21 B2 K1 127.56(18) 4_566 . ? F21 B2 K1 127.56(18) . 7_576 ? F21 B2 K1 52.35(13) 4_566 7_576 ? F21 B2 F21 109.7(4) 4_566 . ? F21 B2 F22 112.8(2) . . ? F21 B2 F22 106.3(2) . 4_566 ? F21 B2 F22 106.3(2) 4_566 . ? F21 B2 F22 112.8(2) 4_566 4_566 ? F22 B2 K1 53.96(12) 4_566 . ? F22 B2 K1 126.12(17) 4_566 7_576 ? F22 B2 K1 53.96(12) . 7_576 ? F22 B2 K1 126.13(17) . . ? F22 B2 F22 109.1(4) . 4_566 ? F31 B3 F32 106.4(7) . . ? F31 B3 F33 116.5(15) . . ? F31 B3 F34 113.4(16) . . ? F31A B3 F34A 100.0(13) . . ? F32 B3 F34 110.3(12) . . ? F32A B3 F31A 109.6(11) . . ? F32A B3 F34A 104.7(18) . . ? F33 B3 F32 106.7(15) . . ? F33 B3 F34 103.4(7) . . ? F33A B3 F31A 118.2(12) . . ? F33A B3 F32A 115.6(16) . . ? F33A B3 F34A 106.6(10) . . ? H1A N1 H1B 108.0 . . ? C1 N1 H1A 109.3 . . ? C1 N1 H1B 109.3 . . ? C5 N1 H1A 109.3 . . ? C5 N1 H1B 109.3 . . ? C5 N1 C1 111.5(11) . . ? H2A N2 H2B 105.6 . . ? C2 N2 H2A 104.2 . . ? C2 N2 H2B 104.2 . . ? C3 N2 H2A 104.2 . . ? C3 N2 H2B 104.2 . . ? C3 N2 C2 132.0(15) . . ? N1 C1 H1C 107.9 . . ? N1 C1 H1D 107.9 . . ? H1C C1 H1D 107.2 . . ? C2 C1 N1 117.7(15) . . ? C2 C1 H1C 107.9 . . ? C2 C1 H1D 107.9 . . ? N2 C2 H2C 107.8 . . ? N2 C2 H2D 107.8 . . ? C1 C2 N2 118.2(16) . . ? C1 C2 H2C 107.8 . . ? C1 C2 H2D 107.8 . . ? H2C C2 H2D 107.1 . . ? N2 C3 H3A 107.7 . . ? N2 C3 H3B 107.7 . . ? N2 C3 C4 118.6(15) . . ? H3A C3 H3B 107.1 . . ? C4 C3 H3A 107.7 . . ? C4 C3 H3B 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 C5 110.8(12) . . ? H4A C4 H4B 108.1 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? N1 C5 C4 108.9(14) . . ? N1 C5 H5A 109.9 . . ? N1 C5 H5B 109.9 . . ? C4 C5 H5A 109.9 . . ? C4 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? 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 K1 F11 2.903(3) . ? K1 F12 3.086(4) . ? K1 F13 2.935(2) 3_545 ? K1 F13 2.935(2) 8 ? K1 F21 2.900(3) . ? K1 F21 2.900(3) 6_556 ? K1 F22 2.934(3) 4_566 ? K1 F22 2.934(3) 7_575 ? K1 F31 2.977(13) . ? K1 F32 3.030(16) . ? K1 F32A 2.628(16) . ? K1 B2 3.52436(15) . ? F11 B1 1.375(6) . ? F12 B1 1.362(6) . ? F13 K1 2.935(2) 3 ? F13 B1 1.371(3) . ? F21 B2 1.365(3) . ? F22 K1 2.934(3) 7_576 ? F22 B2 1.374(3) . ? F31 B3 1.308(13) . ? F31A B3 1.368(16) . ? F32 B3 1.386(12) . ? F32A B3 1.330(17) . ? F33 B3 1.376(17) . ? F33A B3 1.279(17) . ? F34 B3 1.396(14) . ? F34A B3 1.476(18) . ? B1 K1 3.529(4) 3 ? B1 F13 1.371(3) 6_556 ? B2 K1 3.52436(14) 7_576 ? B2 F21 1.365(3) 4_566 ? B2 F22 1.374(3) 4_566 ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 C1 1.488(13) . ? N1 C5 1.455(14) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 C2 1.430(16) . ? N2 C3 1.365(15) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C1 C2 1.429(16) . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.491(15) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 C5 1.509(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ?