#------------------------------------------------------------------------------ #$Date: 2024-12-06 19:29:44 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296459 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/93/7249384.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_7249384 loop_ _publ_author_name 'Jeon, Ie-Rang' 'Jeannin, Olivier' 'Robert, Antoine' 'Barri\`ere, Fr\'ed\'eric' 'Fourmigu\'e, Marc' _publ_section_title ; N-Iodophthalimide as a halogen bond donor, a comparison with N-iodosuccinimide and N-iodosaccharin ; _journal_issue 42 _journal_name_full CrystEngComm _journal_page_first 6075 _journal_page_last 6081 _journal_paper_doi 10.1039/D4CE00654B _journal_volume 26 _journal_year 2024 _chemical_formula_moiety 'C18 H16 I2 N4 O4' _chemical_formula_sum 'C18 H16 I2 N4 O4' _chemical_formula_weight 606.15 _chemical_name_common (NISucc)2(o-bipy) _chemical_name_systematic Bis(N-iodosuccinimide)(2,2'-bipyridine) _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2024-04-12T11:27:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2024-06-27 deposited with the CCDC. 2024-09-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.324(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.488(2) _cell_length_b 10.0888(8) _cell_length_c 9.4428(9) _cell_measurement_reflns_used 9975 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.49 _cell_measurement_theta_min 2.84 _cell_measurement_wavelength 0.71073 _cell_volume 2047.1(3) _computing_cell_refinement 'APEX3 (Bruker, 2015)' _computing_data_collection 'Bruker APEX3 (Bruker, 2015)' _computing_data_reduction 'SAINT (Bruker, 2014)' _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_detector CMOS-PHOTON70 _diffrn_detector_area_resol_mean 7.39 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'D8 VENTURE Bruker AXS' _diffrn_measurement_method 'rotation images' _diffrn_orient_matrix_UB_11 0.060001 _diffrn_orient_matrix_UB_12 -0.005338 _diffrn_orient_matrix_UB_13 -0.038116 _diffrn_orient_matrix_UB_21 0.06871 _diffrn_orient_matrix_UB_22 0.063865 _diffrn_orient_matrix_UB_23 0.019012 _diffrn_orient_matrix_UB_31 0.053797 _diffrn_orient_matrix_UB_32 -0.075615 _diffrn_orient_matrix_UB_33 0.018748 _diffrn_radiation_monochromator 'multilayer monochromator' _diffrn_radiation_probe x-ray _diffrn_radiation_source 'Incoatec microfocus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_unetI/netI 0.0183 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 26687 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.488 _diffrn_reflns_theta_min 2.23 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.104 _exptl_absorpt_correction_T_max 0.883 _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.967 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1160 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CH2Cl2/pentane' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.412 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 253 _refine_ls_number_reflns 4638 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.197 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0206 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+2.8728P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0447 _reflns_Friedel_coverage 0 _reflns_number_gt 4525 _reflns_number_total 4638 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00654b1.cif _cod_data_source_block shelx_CCDC7 _cod_depositor_comments 'Adding full bibliography for 7249377--7249386.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7249384 _shelx_res_file ; TITL shelxt_a.res in P2(1)/c shelx.res created by SHELXL-2019/3 at 11:27:38 on 12-Apr-2024 CELL 0.71073 21.4880 10.0888 9.4428 90.000 90.324 90.000 ZERR 4.00 0.0020 0.0008 0.0009 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H I N O UNIT 72 64 8 16 16 MERG 2 OMIT -3 1 2 OMIT 1 3 3 FMAP 2 PLAN 20 ACTA BOND $H CONF TEMP -123 LIST 4 L.S. 10 WGHT 0.000000 2.872800 FVAR 0.35836 C1 1 0.764170 0.400624 0.792851 11.00000 0.01812 0.02071 = 0.02221 0.00533 0.00302 0.00098 C2 1 0.821608 0.378252 0.856129 11.00000 0.02185 0.02806 = 0.03431 0.00122 -0.00403 -0.00126 AFIX 43 H2 2 0.841510 0.445985 0.909617 11.00000 -1.20000 AFIX 0 C3 1 0.849488 0.255214 0.839936 11.00000 0.01939 0.03711 = 0.04177 0.00595 -0.00330 0.00546 AFIX 43 H3 2 0.888691 0.237358 0.882857 11.00000 -1.20000 AFIX 0 C4 1 0.819799 0.159364 0.761125 11.00000 0.02672 0.02728 = 0.04214 0.00424 0.00064 0.01010 AFIX 43 H4 2 0.837914 0.074191 0.749470 11.00000 -1.20000 AFIX 0 C5 1 0.763233 0.189260 0.699345 11.00000 0.02697 0.02284 = 0.03931 -0.00305 -0.00291 0.00593 AFIX 43 H5 2 0.742954 0.123371 0.643981 11.00000 -1.20000 AFIX 0 C6 1 0.729831 0.526427 0.820253 11.00000 0.02036 0.01984 = 0.01855 0.00285 -0.00261 -0.00097 C7 1 0.676657 0.524672 0.902975 11.00000 0.02531 0.02255 = 0.02847 0.00628 0.00507 0.00226 AFIX 43 H7 2 0.660094 0.442843 0.935283 11.00000 -1.20000 AFIX 0 C8 1 0.647954 0.642620 0.938057 11.00000 0.02781 0.03078 = 0.02636 0.00381 0.00331 0.00762 AFIX 43 H8 2 0.611962 0.643130 0.996018 11.00000 -1.20000 AFIX 0 C9 1 0.672425 0.759390 0.887549 11.00000 0.03882 0.02171 = 0.03121 -0.00038 -0.00225 0.00755 AFIX 43 H9 2 0.653766 0.842018 0.910225 11.00000 -1.20000 AFIX 0 C10 1 0.724546 0.753949 0.803416 11.00000 0.03878 0.01971 = 0.04038 0.00521 0.00307 -0.00147 AFIX 43 H10 2 0.740659 0.834492 0.766584 11.00000 -1.20000 AFIX 0 C11 1 0.584066 0.443633 0.272401 11.00000 0.04557 0.01588 = 0.02013 -0.00425 -0.00193 0.00131 C12 1 0.521541 0.458652 0.200378 11.00000 0.05473 0.02661 = 0.02596 0.00057 -0.01552 0.00298 AFIX 23 H12A 2 0.521729 0.416212 0.105853 11.00000 -1.20000 H12B 2 0.510651 0.553430 0.189105 11.00000 -1.20000 AFIX 0 C13 1 0.475859 0.389701 0.297874 11.00000 0.03375 0.03522 = 0.03119 -0.00820 -0.01175 0.01073 AFIX 23 H13A 2 0.440608 0.448909 0.320995 11.00000 -1.20000 H13B 2 0.459365 0.307983 0.253386 11.00000 -1.20000 AFIX 0 C14 1 0.513297 0.357243 0.428902 11.00000 0.02757 0.02145 = 0.02772 -0.00472 -0.00291 0.00311 C15 1 0.944307 0.826762 0.448479 11.00000 0.02631 0.04506 = 0.03234 0.01899 -0.01146 -0.01123 C16 1 0.999376 0.811717 0.351048 11.00000 0.03129 0.07561 = 0.03244 0.02017 -0.00284 -0.02299 AFIX 23 H16A 2 0.992585 0.861889 0.262193 11.00000 -1.20000 H16B 2 1.037848 0.844562 0.397327 11.00000 -1.20000 AFIX 0 C17 1 1.004192 0.665045 0.321161 11.00000 0.03941 0.07977 = 0.02343 -0.01015 0.00879 -0.03102 AFIX 23 H17A 2 1.044896 0.630025 0.353505 11.00000 -1.20000 H17B 2 0.999504 0.647301 0.218541 11.00000 -1.20000 AFIX 0 C18 1 0.951690 0.602280 0.403107 11.00000 0.03007 0.06354 = 0.02050 -0.01347 0.00338 -0.02151 I1 3 0.647944 0.352079 0.551505 11.00000 0.02380 0.01683 = 0.02070 -0.00065 -0.00064 0.00345 I2 3 0.844716 0.666925 0.608547 11.00000 0.02391 0.03018 = 0.02399 0.00627 -0.00064 -0.00645 N1 4 0.735702 0.307743 0.714338 11.00000 0.02093 0.02061 = 0.02690 0.00075 -0.00075 0.00385 N2 4 0.753676 0.640147 0.770975 11.00000 0.02681 0.02195 = 0.02934 0.00394 0.00219 -0.00206 N3 4 0.574875 0.385473 0.403786 11.00000 0.02701 0.02120 = 0.02018 0.00086 -0.00307 0.00263 N4 4 0.920614 0.701816 0.474666 11.00000 0.02434 0.04237 = 0.02164 0.00686 -0.00017 -0.01221 O1 5 0.634140 0.477756 0.226788 11.00000 0.05080 0.03265 = 0.02612 0.00072 0.00799 -0.00751 O2 5 0.493397 0.312750 0.539252 11.00000 0.03099 0.04155 = 0.03425 0.00670 0.00143 -0.00240 O3 5 0.923952 0.927721 0.498340 11.00000 0.03153 0.03857 = 0.06598 0.02277 -0.00955 -0.00587 O4 5 0.937858 0.487020 0.407961 11.00000 0.04037 0.05944 = 0.04986 -0.02985 0.01553 -0.02746 HKLF 4 REM shelxt_a.res in P2(1)/c REM wR2 = 0.0447, GooF = S = 1.197, Restrained GooF = 1.197 for all data REM R1 = 0.0206 for 4525 Fo > 4sig(Fo) and 0.0213 for all 4638 data REM 253 parameters refined using 0 restraints END WGHT 0.0000 2.8855 REM Highest difference peak 0.412, deepest hole -0.776, 1-sigma level 0.072 Q1 1 0.8270 0.6171 0.5467 11.00000 0.05 0.41 Q2 1 0.7481 0.4646 0.7996 11.00000 0.05 0.39 Q3 1 0.8561 0.7766 0.7793 11.00000 0.05 0.37 Q4 1 0.8583 0.5164 0.7918 11.00000 0.05 0.37 Q5 1 0.8620 0.6074 0.6581 11.00000 0.05 0.37 Q6 1 0.8499 0.7235 0.6946 11.00000 0.05 0.36 Q7 1 0.6318 0.3447 0.8684 11.00000 0.05 0.35 Q8 1 0.6623 0.5613 0.7285 11.00000 0.05 0.32 Q9 1 0.5498 0.4561 0.2475 11.00000 0.05 0.31 Q10 1 0.7048 0.5258 0.8543 11.00000 0.05 0.31 Q11 1 0.8461 -0.0135 0.6141 11.00000 0.05 0.30 Q12 1 0.6582 0.5791 0.8955 11.00000 0.05 0.30 Q13 1 0.4982 0.3699 0.3599 11.00000 0.05 0.29 Q14 1 0.7482 0.6503 0.5632 11.00000 0.05 0.29 Q15 1 0.6610 0.6855 0.8938 11.00000 0.05 0.28 Q16 1 0.7441 0.5888 0.8179 11.00000 0.05 0.28 Q17 1 0.9726 0.8263 0.4047 11.00000 0.05 0.27 Q18 1 1.0574 0.9836 0.3488 11.00000 0.05 0.27 Q19 1 0.6659 0.7081 0.9484 11.00000 0.05 0.27 Q20 1 0.9386 0.6569 0.4467 11.00000 0.05 0.27 ; _shelx_res_checksum 52704 _shelx_hkl_file ; 0 0 -1 1.13 0.27 0 0 -2 1297.17 45.60 0 0 3 -0.36 0.40 0 0 -3 0.63 0.56 0 0 -3 0.23 0.42 0 0 3 -0.05 0.37 0 0 4 499.07 14.60 0 0 -4 501.54 14.12 0 0 -4 489.18 14.48 0 0 4 486.31 13.87 0 0 5 0.02 0.76 0 0 -5 1.25 0.84 0 0 5 0.44 0.64 0 0 -5 0.34 0.75 0 0 6 2432.38 63.76 0 0 6 2527.30 65.14 0 0 7 0.96 1.41 0 0 -7 0.28 1.26 0 0 -7 4.42 1.53 0 0 7 2.21 1.15 0 0 8 172.94 8.31 0 0 8 166.81 6.95 0 0 -8 166.58 7.99 0 0 -8 162.69 7.62 0 0 -9 -1.84 1.40 0 0 -9 -1.13 1.24 0 0 9 1.26 1.57 0 0 9 1.76 1.88 0 0 -10 1.83 2.09 0 0 -10 0.75 1.90 0 0 10 1.64 2.15 0 0 11 1.73 1.70 0 0 -11 -1.00 1.71 0 0 -11 0.61 1.47 0 0 -12 402.91 16.53 0 1 0 0.05 0.08 0 1 0 0.00 0.08 0 -1 0 0.19 0.12 0 1 -2 8.39 1.00 0 1 2 7.96 0.59 0 1 -2 7.88 1.08 0 1 2 10.28 0.83 0 -1 -2 8.67 0.69 0 -1 2 6.93 1.06 0 -1 -2 8.35 0.78 0 1 -3 223.55 7.45 0 1 3 225.10 6.50 0 1 3 240.11 7.11 0 1 -3 227.10 7.16 0 -1 -3 220.46 6.98 0 -1 3 226.37 7.10 0 -1 -3 236.13 6.77 0 -1 3 213.10 7.44 0 1 4 652.44 18.48 0 1 4 656.94 17.73 0 1 -4 673.29 18.56 0 1 -4 644.20 18.92 0 -1 -4 668.26 18.11 0 -1 4 683.40 18.47 0 -1 4 650.57 19.03 0 -1 -4 679.52 18.52 0 1 5 1809.50 45.86 0 1 5 1818.83 46.82 0 1 -5 1811.54 47.32 0 -1 -5 1712.07 46.60 0 -1 5 1864.78 46.57 0 -1 5 1657.15 47.16 0 1 -6 5453.15 184.19 0 1 6 5400.14 175.03 0 -1 6 5382.88 181.82 0 -1 -6 5840.14 181.58 0 1 -7 234.65 9.44 0 1 7 251.54 8.45 0 1 -7 263.37 10.16 0 1 7 268.52 10.04 0 -1 -7 264.80 9.72 0 -1 7 244.61 10.20 0 -1 7 251.32 9.18 0 -1 -7 239.85 9.19 0 1 -8 1228.92 36.13 0 1 8 1275.49 33.87 0 1 8 1289.54 36.00 0 1 -8 1236.74 35.58 0 -1 -8 1311.85 35.81 0 -1 8 1276.72 34.89 0 -1 -8 1206.15 35.05 0 -1 8 1239.70 36.57 0 1 9 8.33 2.61 0 1 -9 17.98 3.36 0 1 -9 11.29 2.91 0 -1 9 9.53 2.29 0 -1 -9 10.35 2.72 0 -1 9 9.46 2.99 0 -1 -9 10.23 2.59 0 1 -10 67.72 5.45 0 1 -10 64.54 5.76 0 1 10 72.38 5.97 0 -1 -10 67.17 5.48 0 -1 -10 69.11 5.38 0 -1 10 69.99 6.05 0 1 -11 42.31 5.55 0 1 -11 32.03 4.84 0 -1 -11 32.52 4.69 0 -1 11 36.82 5.62 0 1 -12 347.88 20.30 0 -1 -12 361.23 14.82 0 2 0 3772.99 103.78 0 2 1 1738.06 51.21 0 2 -1 1767.52 58.86 0 -2 -1 1806.63 51.14 0 -2 1 1729.42 58.73 0 2 -2 654.92 17.77 0 2 -2 638.66 18.09 0 -2 -2 686.30 17.21 0 -2 2 676.43 17.83 0 -2 -2 665.42 16.88 0 -2 2 642.78 18.14 0 2 -3 43.67 2.41 0 2 -3 37.21 2.89 0 2 3 37.58 1.94 0 -2 -3 40.78 2.00 0 -2 3 36.43 2.28 0 -2 -3 41.11 1.82 0 -2 3 39.37 2.58 0 2 4 399.41 10.61 0 2 -4 391.77 12.55 0 2 4 383.71 11.56 0 2 -4 426.29 12.25 0 -2 -4 407.14 11.65 0 -2 -4 393.48 11.29 0 -2 4 365.59 12.50 0 -2 4 406.43 12.10 0 2 -5 1686.08 44.92 0 2 -5 1635.58 44.25 0 2 5 1661.86 43.81 0 2 5 1662.75 42.46 0 -2 5 1699.09 45.14 0 -2 5 1693.38 44.17 0 -2 -5 1663.84 43.38 0 2 6 38.18 2.07 0 2 -6 38.95 3.16 0 2 6 40.85 2.99 0 2 -6 38.02 3.38 0 -2 6 33.18 2.86 0 -2 -6 39.74 2.90 0 -2 6 34.53 3.26 0 -2 -6 37.50 2.67 0 2 -8 4.39 2.14 0 2 -8 0.97 1.57 0 -2 8 1.05 1.49 0 -2 -8 3.41 1.53 0 -2 8 1.17 1.77 0 -2 -8 1.04 1.47 0 2 9 166.43 8.32 0 2 -9 183.55 9.26 0 2 -9 169.17 8.50 0 -2 -9 169.69 7.95 0 -2 -9 176.33 8.27 0 -2 9 165.96 9.17 0 -2 9 176.39 8.16 0 2 -10 5.65 2.61 0 2 -10 8.75 2.74 0 2 10 8.26 2.58 0 -2 10 7.24 2.38 0 -2 10 11.75 3.21 0 -2 -10 4.66 2.29 0 -2 -10 13.58 2.88 0 2 -11 363.29 14.92 0 2 -11 354.26 15.30 0 -2 11 409.52 23.71 0 -2 -11 353.93 14.16 0 2 -12 78.53 6.47 0 -2 -12 81.44 6.25 0 3 0 0.73 0.34 0 -3 0 1.39 0.48 0 -3 0 2.45 0.60 0 3 -2 11.12 1.31 0 -3 2 7.14 1.33 0 -3 -2 6.50 0.72 0 -3 -2 7.78 0.59 0 3 -3 17.58 2.29 0 3 -3 18.29 1.72 0 -3 3 16.33 2.18 0 -3 -3 17.69 1.09 0 -3 -3 16.16 1.22 0 -3 3 11.64 1.68 0 3 4 291.07 9.07 0 3 -4 302.84 10.00 0 3 -4 309.14 10.54 0 -3 4 304.68 10.64 0 -3 4 300.99 9.99 0 -3 -4 312.68 9.22 0 -3 -4 311.83 8.90 0 3 5 1106.37 29.72 0 3 -5 1097.70 31.34 0 3 -5 1159.44 30.84 0 -3 -5 1060.12 29.62 0 -3 -5 1122.06 29.77 0 -3 5 1153.67 30.75 0 -3 5 1090.71 31.51 0 3 -6 28.83 3.15 0 3 -6 22.07 2.57 0 3 6 27.49 2.30 0 -3 6 26.50 2.99 0 -3 -6 23.46 2.06 0 -3 -6 25.68 2.31 0 3 -7 595.00 19.11 0 3 -7 557.28 18.19 0 3 7 568.98 17.44 0 -3 7 544.51 19.00 0 -3 -7 592.71 17.53 0 -3 -7 572.17 17.17 0 -3 7 568.00 18.03 0 3 -8 99.05 6.41 0 3 -8 98.64 6.10 0 3 8 101.70 5.50 0 -3 -8 96.44 5.21 0 -3 -8 95.72 5.35 0 -3 8 100.04 6.53 0 -3 8 95.48 5.74 0 3 -9 9.61 2.88 0 3 9 7.92 2.37 0 3 -9 3.08 2.63 0 -3 9 12.94 3.17 0 -3 -9 9.69 2.42 0 -3 -9 11.40 3.91 0 -3 9 16.79 4.11 0 3 10 9.73 3.07 0 3 -10 3.09 3.15 0 3 -10 8.77 2.76 0 -3 -10 8.94 3.90 0 -3 10 8.74 2.47 0 -3 -10 6.88 2.31 0 3 -11 40.39 5.85 0 3 -11 44.42 5.06 0 -3 -11 36.36 4.19 0 -3 11 43.76 6.19 0 4 0 6913.92 189.32 0 4 0 6679.84 188.37 0 4 -1 48.13 2.33 0 4 -1 46.81 2.68 0 4 -1 51.34 2.42 0 -4 1 49.92 2.77 0 -4 -1 51.80 2.04 0 -4 -1 52.16 2.27 0 -4 1 48.02 2.51 0 -4 -1 47.62 2.03 0 -4 -1 59.16 2.39 0 4 -2 2258.58 83.10 0 4 2 2059.21 67.66 0 -4 -2 2138.02 67.32 0 -4 2 2277.44 84.28 0 4 -3 325.63 11.07 0 4 -3 329.57 10.54 0 -4 3 356.72 11.37 0 -4 -3 336.14 9.54 0 -4 -3 348.81 9.25 0 -4 3 307.71 10.53 0 4 -4 28.76 2.72 0 4 -4 30.50 2.57 0 -4 4 20.89 2.31 0 -4 -4 25.40 1.75 0 -4 4 30.60 2.93 0 -4 -4 30.38 1.71 0 4 -5 1380.68 38.25 0 4 5 1387.02 36.82 0 4 -5 1440.01 39.17 0 -4 5 1438.65 39.41 0 -4 -5 1423.39 36.92 0 -4 5 1380.16 38.28 0 4 -6 882.72 25.92 0 4 -6 837.11 24.93 0 4 6 854.38 23.58 0 -4 6 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890.90 28.40 10 -5 8 833.40 28.14 -10 -5 -8 839.06 24.13 -10 5 -9 88.86 6.49 -10 5 -9 99.01 6.77 10 -5 9 107.96 7.55 10 -5 9 98.65 7.37 -10 5 -10 -1.29 2.04 -10 5 -10 3.96 2.50 10 -5 10 2.06 3.06 10 -5 10 3.39 2.76 10 6 -9 33.42 5.34 10 6 -9 29.02 4.71 -10 -6 9 29.56 5.45 10 -6 -9 28.57 4.26 -10 -6 9 28.49 4.49 10 6 -8 2.75 2.20 -10 6 8 1.90 2.99 -10 -6 8 -0.25 2.35 -10 -6 8 4.63 2.55 10 -6 -8 2.14 1.63 10 6 -7 144.48 7.53 -10 6 7 140.28 7.62 -10 6 7 131.20 5.74 10 6 -7 147.37 8.47 -10 -6 7 135.54 7.79 -10 -6 7 130.79 8.49 10 -6 -7 140.92 7.30 10 -6 -7 145.65 7.80 -10 6 6 386.85 14.12 10 6 -6 377.52 13.67 -10 6 6 396.75 12.32 10 6 -6 371.31 14.61 10 -6 -6 396.53 13.79 10 -6 -6 385.67 14.38 -10 -6 6 365.21 15.10 -10 -6 6 377.11 14.11 10 6 -5 350.01 13.48 -10 6 5 357.06 12.99 10 6 -5 336.63 12.28 -10 6 5 340.79 11.43 10 -6 -5 346.09 12.44 -10 -6 5 358.33 14.22 -10 -6 5 352.40 13.17 10 -6 -5 365.28 13.44 -10 6 4 399.40 12.77 10 6 -4 401.04 14.30 -10 6 4 402.08 13.99 10 6 -4 388.06 12.98 -10 -6 4 421.76 14.87 10 -6 -4 399.52 13.52 -10 -6 4 385.66 13.69 10 -6 -4 395.51 14.29 -10 6 3 750.63 21.07 10 6 -3 703.82 20.50 10 6 -3 724.33 22.03 -10 6 3 723.65 22.08 10 -6 -3 737.45 21.62 -10 -6 3 698.22 22.24 10 -6 -3 716.57 22.48 -10 -6 3 735.89 21.59 -10 6 2 376.76 13.29 -10 6 2 389.01 12.55 10 6 -2 370.97 12.80 10 6 -2 390.36 11.60 -10 -6 2 373.68 13.07 10 -6 -2 390.72 13.77 -10 -6 2 399.02 12.64 10 -6 -2 380.63 12.80 10 6 -1 108.09 5.09 -10 6 1 101.90 5.16 -10 6 1 103.77 5.63 10 -6 -1 112.07 6.08 10 -6 -1 105.85 5.29 -10 -6 1 97.33 4.98 -10 -6 1 104.14 4.76 10 6 0 3661.17 91.36 -10 6 0 3536.09 93.19 10 6 1 21.83 1.71 -10 6 -1 19.45 2.80 -10 6 -1 22.78 3.08 -10 6 -1 19.81 3.05 10 -6 1 20.58 2.78 10 -6 1 29.69 3.87 -10 -6 -1 17.31 1.65 -10 6 -2 1107.35 31.62 -10 6 -2 1118.52 31.46 -10 -6 -2 1142.63 28.93 -10 -6 -2 1114.15 28.45 10 -6 2 1141.14 32.85 10 -6 2 1093.53 32.33 -10 6 -3 228.93 9.21 -10 6 -3 233.42 9.38 10 -6 3 245.73 10.34 -10 -6 -3 231.86 6.52 10 -6 3 219.04 9.77 -10 6 -4 100.03 5.87 -10 6 -4 99.86 5.75 10 -6 4 103.01 6.40 10 -6 4 98.33 6.44 -10 6 -5 429.44 15.10 -10 6 -5 445.74 16.33 10 -6 5 422.22 16.02 10 -6 5 416.52 15.82 -10 6 -6 877.61 26.08 -10 6 -6 811.33 25.71 10 -6 6 829.44 27.06 -10 6 -7 276.85 11.55 -10 6 -7 274.55 11.52 10 -6 7 282.47 12.68 -10 -6 -7 251.16 8.37 10 -6 7 254.68 12.15 -10 6 -8 14.11 3.29 -10 6 -8 17.85 3.61 10 -6 8 23.57 4.18 -10 6 -9 7.03 3.08 -10 6 -9 6.29 3.47 10 -6 9 5.81 3.18 10 -6 9 4.88 3.00 10 7 -9 84.33 7.12 10 7 -9 76.86 6.42 -10 -7 9 75.35 7.11 -10 -7 9 79.53 6.55 10 -7 -9 76.76 5.90 10 7 -8 17.75 3.76 10 7 -8 14.83 3.79 10 -7 -8 11.87 2.65 -10 -7 8 13.92 3.70 -10 -7 8 18.33 3.68 -10 7 7 303.30 12.72 10 7 -7 297.93 16.36 10 7 -7 302.81 12.24 10 -7 -7 343.80 12.56 -10 -7 7 320.02 13.43 10 -7 -7 307.14 13.96 -10 -7 7 284.54 13.71 -10 7 6 470.95 16.96 10 7 -6 503.96 16.82 -10 7 6 502.40 14.72 10 7 -6 502.06 18.26 10 -7 -6 526.12 17.87 -10 -7 6 490.18 18.73 10 -7 -6 496.59 17.01 -10 -7 6 516.76 17.72 -10 7 5 199.86 7.32 -10 7 5 198.55 8.89 10 7 -5 202.18 9.51 10 7 -5 194.43 8.28 -10 -7 5 196.94 9.86 10 -7 -5 191.91 8.55 -10 -7 5 195.02 8.97 10 -7 -5 198.70 9.26 10 7 -4 16.74 3.08 -10 7 4 18.39 3.08 10 7 -4 22.83 2.95 -10 7 4 22.16 2.69 10 -7 -4 23.51 3.47 -10 -7 4 14.95 3.08 10 -7 -4 20.11 3.08 -10 -7 4 19.70 3.24 10 7 -3 29.64 2.66 -10 7 3 38.34 3.01 10 7 -3 28.86 3.40 -10 7 3 35.69 3.65 -10 -7 3 35.84 3.68 -10 -7 3 31.34 3.34 10 -7 -3 39.58 3.43 10 -7 -3 30.63 3.57 10 7 -2 670.39 20.14 10 7 -2 668.33 17.82 -10 7 2 666.04 19.62 10 7 -2 678.96 17.77 -10 7 2 630.76 20.46 -10 -7 2 648.24 19.75 10 -7 -2 655.66 20.11 10 -7 -2 659.68 21.18 -10 -7 2 675.06 20.48 -10 7 1 1903.40 50.74 10 7 -1 1880.30 50.38 -10 7 1 1938.52 50.54 -10 7 1 1930.31 51.77 -10 -7 1 1863.45 50.67 -10 -7 1 1919.98 50.29 10 -7 -1 1922.25 52.42 10 -7 -1 1917.05 51.10 -10 7 0 2.75 1.63 -10 7 0 5.19 1.64 10 7 0 2.11 1.07 -10 7 0 2.75 1.67 -10 -7 0 1.59 1.03 10 -7 0 3.31 1.94 10 -7 0 2.11 1.43 -10 -7 0 4.00 1.23 10 7 1 1441.68 38.08 -10 7 -1 1390.40 41.02 -10 7 -1 1459.27 40.47 -10 7 -1 1507.88 40.33 -10 -7 -1 1526.78 38.40 10 -7 1 1438.02 40.43 10 -7 1 1447.62 41.48 10 -7 1 1522.28 42.05 -10 -7 -1 1555.27 38.58 -10 7 -2 196.62 8.46 -10 7 -2 193.28 8.21 10 -7 2 202.98 9.44 10 -7 2 215.21 9.38 -10 -7 -2 186.92 6.18 -10 7 -3 400.77 13.88 -10 7 -3 389.52 13.96 10 -7 3 390.88 14.76 -10 -7 -3 398.31 10.75 10 -7 3 411.97 15.31 10 -7 4 297.72 12.64 -10 7 -5 202.61 9.26 -10 7 -5 219.00 9.66 10 -7 5 206.95 12.16 10 -7 5 199.20 10.11 -10 7 -6 625.20 21.00 -10 7 -6 658.84 21.11 10 -7 6 612.23 22.13 10 -7 6 646.05 22.45 -10 7 -7 54.42 5.75 -10 7 -7 49.48 5.00 10 -7 7 50.04 5.64 10 -7 7 58.49 5.82 -10 7 -8 316.89 13.60 -10 7 -8 350.53 13.96 10 -7 8 321.35 14.77 10 -7 8 317.32 14.86 -10 7 -9 90.22 6.65 -10 7 -9 75.92 6.37 10 -7 9 76.09 7.21 10 -7 9 77.50 7.25 10 8 -8 160.48 9.88 10 8 -8 163.95 8.72 -10 -8 8 158.83 11.59 10 -8 -8 172.58 8.76 -10 -8 8 180.41 9.86 10 8 -7 730.50 23.23 10 8 -7 714.14 24.83 -10 -8 7 715.67 24.20 10 -8 -7 763.13 23.40 -10 -8 7 705.63 25.57 10 8 -6 13.92 5.30 -10 -8 6 6.18 2.43 -10 -8 6 11.70 3.27 10 -8 -6 11.29 2.72 -10 8 5 813.28 22.42 10 8 -5 860.08 24.43 -10 8 5 812.27 22.31 10 8 -5 807.37 26.03 -10 8 5 864.96 25.41 10 -8 -5 818.19 25.17 -10 -8 5 847.18 26.97 -10 -8 5 782.81 25.41 10 -8 -5 801.09 25.75 -10 8 4 133.11 5.52 10 8 -4 132.43 7.32 -10 8 4 132.99 7.06 -10 8 4 126.74 5.36 10 8 -4 132.90 5.92 10 -8 -4 141.73 7.51 -10 -8 4 129.16 6.93 -10 -8 4 134.12 7.76 10 -8 -4 127.17 6.69 -10 8 3 109.22 6.17 10 8 -3 110.03 6.32 10 8 -3 108.14 4.65 -10 8 3 112.68 5.21 10 8 -3 111.82 4.59 -10 8 3 110.90 5.05 10 -8 -3 111.36 6.64 10 -8 -3 109.87 5.95 -10 -8 3 110.69 6.55 -10 -8 3 110.44 6.01 -10 8 2 199.44 7.64 -10 8 2 204.88 7.90 10 8 -2 204.52 8.48 -10 8 2 201.78 8.86 -10 -8 2 189.97 8.53 10 -8 -2 198.99 9.32 10 -8 -2 202.46 8.46 -10 -8 2 199.45 8.26 -10 8 1 104.25 5.20 -10 8 1 102.63 5.38 -10 8 1 100.08 5.97 10 8 -1 102.13 5.21 10 -8 -1 107.91 5.77 -10 -8 1 103.85 5.24 10 -8 -1 103.40 6.38 -10 -8 1 102.49 5.41 -10 8 0 43.45 3.91 10 8 0 35.21 2.71 -10 8 0 44.36 3.43 -10 8 0 43.65 3.58 10 -8 0 40.10 3.99 -10 -8 0 40.07 2.92 10 -8 0 43.85 3.67 -10 -8 0 43.79 3.02 -10 8 -1 76.21 4.99 -10 8 -1 81.44 4.91 -10 -8 -1 80.94 3.61 10 -8 1 85.63 5.99 10 -8 1 92.30 5.78 10 -8 1 86.36 5.65 -10 -8 -1 83.25 3.93 -10 8 -2 3.55 1.83 -10 8 -2 6.62 2.08 -10 -8 -2 6.21 1.32 10 -8 2 2.07 2.01 10 -8 2 5.45 2.51 -10 8 -3 17.73 3.42 -10 -8 -3 16.92 1.33 -10 8 -4 210.55 9.34 -10 8 -4 224.21 9.72 10 -8 4 204.86 10.19 10 -8 4 205.93 10.48 -10 8 -5 459.47 16.19 -10 8 -5 433.31 15.75 10 -8 5 429.20 17.00 10 -8 5 448.80 17.50 -10 8 -6 25.62 4.18 -10 8 -6 18.95 3.57 10 -8 6 19.75 4.30 -10 8 -7 814.84 26.50 -10 8 -7 858.39 26.76 10 -8 7 798.55 28.01 -10 8 -8 61.58 7.17 -10 8 -8 91.56 9.82 10 -8 8 86.04 7.32 10 -8 8 91.21 7.66 10 9 -7 3.74 1.92 10 9 -7 -0.51 2.03 -10 -9 7 3.51 2.66 10 -9 -7 0.76 1.56 10 9 -6 178.84 9.86 -10 -9 6 212.95 11.05 10 -9 -6 206.99 9.32 -10 -9 6 200.47 10.01 10 9 -5 363.28 12.34 10 -9 -5 342.18 13.12 -10 -9 5 370.97 15.06 -10 -9 5 333.34 13.61 -10 9 4 382.53 13.96 10 9 -4 379.85 12.17 -10 9 4 382.32 11.35 -10 9 4 390.00 11.42 10 9 -4 376.07 11.95 10 9 -4 405.38 14.74 -10 -9 4 362.58 14.76 -10 -9 4 371.69 14.10 10 -9 -4 378.96 13.73 10 -9 -4 375.41 14.63 -10 9 3 78.34 5.31 -10 9 3 73.33 3.95 -10 9 3 71.28 3.87 10 9 -3 85.19 5.68 -10 -9 3 83.58 8.20 10 -9 -3 74.98 5.69 -10 -9 3 65.67 5.21 10 -9 -3 77.17 5.14 -10 9 2 344.01 13.13 -10 9 2 351.68 11.69 -10 9 2 369.94 11.64 10 9 -2 360.56 12.73 10 -9 -2 355.32 13.93 -10 -9 2 335.28 12.85 -10 -9 2 364.01 12.67 10 -9 -2 344.59 12.79 10 9 -1 526.26 16.25 -10 9 1 511.91 15.95 -10 9 1 531.59 17.61 -10 9 1 509.90 16.20 10 -9 -1 509.62 18.23 10 -9 -1 499.39 16.93 -10 -9 1 521.16 16.58 -10 -9 1 524.77 16.36 -10 9 0 136.52 6.60 -10 9 0 131.76 6.25 10 9 0 132.81 5.60 10 -9 0 124.57 7.61 10 -9 0 147.97 7.68 10 -9 0 136.40 6.99 -10 -9 0 133.97 5.93 -10 -9 0 123.39 5.71 -10 9 -1 883.82 26.35 -10 9 -1 919.08 26.84 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432.72 13.59 -10 10 2 441.10 13.52 10 10 -2 460.89 15.31 -10 10 2 413.07 15.57 -10 -10 2 442.01 15.62 10 -10 -2 439.92 16.60 10 -10 -2 470.91 15.70 -10 10 1 94.37 5.06 -10 10 1 88.67 4.81 10 10 -1 89.38 5.17 -10 -10 1 91.68 5.32 -10 -10 1 90.94 5.32 10 -10 -1 100.71 6.70 10 -10 -1 113.02 6.80 10 -10 -1 97.68 5.95 -10 10 0 1082.90 30.75 -10 10 0 1063.62 30.39 -10 -10 0 1078.29 30.31 10 -10 0 1114.27 33.58 10 -10 0 1075.52 31.91 10 -10 0 1106.78 32.92 -10 -10 0 1058.44 29.89 -10 10 -1 80.38 4.89 -10 10 -1 66.22 4.75 10 -10 1 69.30 5.91 -10 -10 -1 59.17 3.78 -10 -10 -1 69.88 3.30 10 -10 1 84.60 6.13 -10 10 -2 667.23 23.03 10 -10 2 682.32 23.00 -10 -10 -2 677.98 20.74 10 -10 2 654.66 23.34 -10 10 -3 451.08 15.51 10 -10 3 413.62 16.77 -10 10 -4 22.05 3.91 10 -10 4 23.11 4.62 10 -10 4 14.79 3.86 -10 10 -5 18.21 3.80 10 -10 5 20.57 4.63 10 -10 5 26.70 5.00 -10 10 -6 90.46 6.94 -10 10 -6 89.78 6.71 10 -10 6 103.66 8.19 10 -10 6 100.76 8.01 10 11 -5 22.56 4.16 -10 -11 5 18.87 4.46 -10 -11 5 17.59 4.03 10 -11 -5 18.92 3.48 10 11 -4 139.81 8.23 -10 -11 4 142.61 8.75 10 -11 -4 154.49 7.98 -10 -11 4 159.65 8.40 10 11 -3 194.85 9.26 10 -11 -3 193.39 9.07 10 -11 -3 196.15 9.67 -10 -11 3 185.39 9.42 -10 -11 3 188.97 9.18 10 11 -2 7.29 2.57 -10 -11 2 7.81 2.38 -10 -11 1 126.85 6.64 10 -11 -1 147.21 8.31 10 -11 -1 153.12 8.00 -10 -11 0 2.66 1.33 -10 -11 0 0.84 1.70 -10 11 -1 30.42 3.41 -10 11 -1 38.34 3.56 10 -11 1 44.12 4.86 -10 11 -2 29.66 4.00 10 -11 2 30.39 5.18 -10 11 -3 108.50 6.87 -10 11 -3 127.45 6.99 10 -11 3 159.58 12.80 10 -11 3 113.86 8.44 -10 11 -4 69.67 5.91 -10 11 -4 94.19 6.19 10 -11 4 76.05 6.64 10 -11 4 81.74 7.43 10 -12 -2 -0.25 1.93 10 -12 -2 2.44 2.13 -10 -12 2 2.68 2.04 10 -12 -1 147.27 8.74 10 -12 -1 154.55 8.48 -10 -12 1 143.09 7.09 10 -12 0 309.07 13.48 10 -12 1 1.90 2.21 10 -12 2 144.86 9.00 11 0 -11 9.52 3.27 11 0 -11 0.81 2.43 -11 0 11 1.34 2.76 -11 0 11 -0.86 2.77 -11 0 10 228.90 10.34 -11 0 10 229.84 12.17 11 0 -10 223.45 10.90 11 0 -10 221.68 11.59 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168.37 9.21 13 -6 5 162.76 9.27 -13 6 -6 454.41 16.14 -13 6 -6 411.98 15.62 13 -6 6 429.89 16.88 -13 -6 -6 414.00 12.26 13 -6 6 437.13 17.11 -13 6 -7 191.69 9.58 -13 6 -7 189.68 10.96 13 -6 7 205.83 12.06 13 -6 7 193.71 10.36 -13 6 -8 381.31 15.59 -13 6 -8 393.95 15.71 13 -6 8 415.03 17.14 13 -6 8 408.09 17.08 -13 6 -9 54.90 5.70 -13 6 -9 65.11 5.96 13 -6 9 68.76 6.97 13 -6 9 75.55 7.08 13 7 -8 48.35 5.44 13 7 -8 54.82 5.04 -13 -7 8 48.28 5.17 13 -7 -8 52.81 5.03 -13 -7 8 45.96 7.71 13 7 -7 292.12 11.94 13 7 -7 283.99 13.10 -13 -7 7 308.32 12.97 13 -7 -7 287.87 12.17 -13 -7 7 276.68 13.69 -13 7 6 251.99 11.24 -13 7 6 238.54 9.32 13 -7 -6 254.43 10.85 -13 -7 6 237.37 10.93 13 -7 -6 261.76 11.73 -13 -7 6 240.66 11.98 13 7 -5 27.64 4.36 -13 7 5 32.16 3.24 -13 7 5 33.25 4.49 13 7 -5 34.54 3.35 -13 -7 5 29.11 4.46 -13 -7 5 32.15 4.51 13 -7 -5 31.00 4.42 13 -7 -5 32.87 3.75 -13 7 4 150.66 8.01 -13 7 4 152.67 7.14 13 7 -4 157.54 8.10 13 7 -4 162.45 6.78 -13 -7 4 153.98 7.74 13 -7 -4 159.26 8.60 -13 -7 4 163.26 8.57 13 -7 -4 153.80 7.74 13 7 -3 91.53 5.69 -13 7 3 83.65 5.12 13 7 -3 92.90 4.28 -13 7 3 90.58 5.96 -13 -7 3 85.94 5.77 -13 -7 3 80.16 5.21 13 -7 -3 80.35 5.95 13 -7 -3 95.20 5.64 13 7 -2 859.42 22.96 -13 7 2 911.87 27.11 13 7 -2 870.32 25.95 -13 7 2 912.01 26.06 13 -7 -2 881.70 27.68 -13 -7 2 865.04 26.30 -13 -7 2 880.14 25.72 -13 7 1 120.95 6.25 13 7 -1 112.91 5.70 -13 7 1 118.98 6.79 -13 -7 1 117.31 5.65 13 -7 -1 119.09 7.20 -13 -7 1 112.06 5.85 13 -7 -1 106.61 8.23 -13 7 0 67.06 5.17 13 7 0 72.18 4.05 -13 7 0 78.48 5.09 13 -7 0 74.39 5.72 -13 -7 0 74.87 4.23 -13 -7 0 76.90 4.11 -13 7 -1 116.20 6.62 -13 7 -1 110.88 6.04 -13 7 -1 98.90 6.09 13 7 1 103.53 4.51 13 -7 1 118.92 6.41 13 -7 1 126.73 7.31 -13 -7 -1 105.17 4.65 -13 -7 -1 107.06 4.76 -13 7 -2 221.80 9.62 -13 7 -2 239.01 11.28 13 -7 2 236.60 10.58 -13 -7 -2 223.23 7.49 -13 -7 -2 217.59 6.74 13 -7 2 230.60 10.84 -13 7 -3 1048.63 31.06 -13 7 -3 1098.51 31.52 13 -7 3 1060.20 32.77 13 -7 3 1058.31 32.31 -13 -7 -3 1040.75 28.45 -13 7 -4 481.88 16.72 -13 7 -4 455.83 16.28 13 -7 4 482.45 18.03 -13 -7 -4 460.15 12.87 13 -7 4 449.53 17.32 -13 7 -5 355.09 13.64 -13 7 -5 348.31 13.40 13 -7 5 339.50 14.53 13 -7 5 334.01 14.56 -13 -7 -5 326.69 9.62 -13 7 -6 91.80 6.39 -13 7 -6 92.99 7.63 13 -7 6 92.91 7.19 -13 7 -7 8.60 2.71 -13 7 -7 3.02 2.17 13 -7 7 -0.39 2.34 13 -7 7 4.72 2.76 -13 7 -8 86.76 6.72 -13 7 -8 67.60 6.15 13 8 -7 66.76 6.96 13 8 -7 61.16 5.00 -13 -8 7 63.46 11.47 -13 -8 7 72.73 11.23 13 -8 -7 74.43 5.77 13 8 -6 19.30 3.22 13 8 -6 13.09 3.12 -13 -8 6 20.39 4.19 13 -8 -6 20.93 3.78 -13 -8 6 10.39 3.03 13 8 -5 158.43 7.05 -13 8 5 152.54 8.15 -13 8 5 136.73 6.44 13 8 -5 155.32 11.74 -13 -8 5 144.42 8.04 13 -8 -5 136.30 8.29 13 -8 -5 142.57 7.75 -13 -8 5 145.76 8.77 -13 8 4 159.18 7.19 13 8 -4 161.01 6.67 13 8 -4 169.94 8.53 -13 8 4 170.86 8.66 13 -8 -4 152.04 8.63 -13 -8 4 167.03 8.22 13 -8 -4 157.70 8.09 -13 -8 4 170.50 8.91 13 8 -3 1811.99 47.86 -13 8 3 1715.24 46.57 -13 8 3 1715.99 48.18 13 8 -3 1769.93 44.46 13 -8 -3 1671.26 48.96 -13 -8 3 1681.35 48.15 13 -8 -3 1663.32 47.49 13 8 -2 29.48 3.36 -13 8 2 30.44 3.34 -13 8 2 30.31 3.57 -13 -8 2 26.56 3.06 -13 -8 2 31.17 3.45 13 -8 -2 23.58 4.03 13 -8 -2 38.88 3.77 -13 8 1 734.07 23.89 -13 8 1 748.07 22.64 -13 8 1 756.44 23.03 13 8 -1 774.87 22.31 13 -8 -1 745.68 23.28 -13 -8 1 750.34 22.61 13 -8 -1 762.67 24.87 -13 -8 1 758.00 22.35 -13 8 0 576.61 18.47 -13 8 0 559.69 18.07 -13 8 0 560.66 19.19 13 8 0 553.57 16.72 13 -8 0 551.33 18.51 -13 -8 0 557.69 17.04 13 -8 0 595.60 20.29 -13 -8 0 569.49 17.10 -13 8 -1 43.08 4.47 -13 8 -1 45.81 5.00 -13 8 -1 53.33 4.36 13 8 1 36.64 2.46 -13 -8 -1 43.48 2.75 13 -8 1 43.48 4.13 13 -8 1 46.51 4.77 13 -8 1 42.69 4.96 -13 -8 -1 41.06 2.99 -13 8 -2 405.51 14.72 -13 8 -2 397.45 14.40 -13 -8 -2 409.53 12.14 13 -8 2 406.50 16.10 13 -8 2 399.22 15.53 -13 8 -3 669.97 21.15 -13 8 -3 641.38 21.27 13 -8 3 648.36 22.28 -13 -8 -3 624.88 17.74 13 -8 3 670.93 23.34 -13 8 -4 26.58 4.11 -13 8 -4 26.33 3.98 13 -8 4 31.60 5.15 13 -8 4 27.38 4.44 -13 -8 -4 26.29 2.24 -13 8 -5 261.41 11.51 -13 8 -5 267.14 11.87 13 -8 5 283.05 13.02 13 -8 5 277.58 13.29 -13 8 -6 25.63 4.43 -13 8 -6 20.73 4.02 13 -8 6 17.99 4.36 13 -8 7 2.09 2.50 13 -8 7 6.68 3.34 13 9 -6 117.10 8.77 -13 -9 6 112.37 7.61 13 -9 -6 124.13 7.34 -13 -9 6 106.72 9.12 13 9 -5 67.32 5.82 13 -9 -5 75.95 5.64 -13 -9 5 60.73 5.92 -13 -9 5 69.36 6.90 -13 9 4 371.70 16.02 -13 9 4 373.64 13.51 13 -9 -4 380.76 14.37 -13 -9 4 383.36 14.41 -13 -9 4 374.05 15.12 -13 9 3 148.10 6.68 -13 9 3 152.86 6.98 13 9 -3 151.12 7.83 -13 9 3 143.48 7.96 -13 -9 3 151.26 7.69 13 -9 -3 158.21 8.88 13 -9 -3 152.96 7.78 -13 -9 3 150.87 8.08 -13 9 2 278.51 10.34 13 9 -2 278.43 10.83 -13 9 2 287.20 10.74 -13 9 2 265.15 11.60 -13 -9 2 279.64 11.43 13 -9 -2 269.70 11.28 -13 -9 2 276.66 11.20 13 -9 -2 281.05 12.53 -13 9 1 130.21 6.69 -13 9 1 138.34 7.63 13 9 -1 121.73 6.10 -13 9 1 133.15 6.51 13 -9 -1 127.09 7.97 -13 -9 1 123.94 6.24 -13 -9 1 120.80 6.29 13 -9 -1 133.34 7.09 -13 9 0 80.55 5.19 -13 9 0 81.74 5.93 -13 9 0 92.55 5.80 13 9 0 81.81 4.30 -13 -9 0 81.01 4.66 13 -9 0 90.75 5.95 13 -9 0 79.78 6.27 -13 -9 0 85.82 4.59 -13 9 -1 4.28 1.93 -13 9 -1 5.61 2.25 -13 -9 -1 3.56 1.40 13 -9 1 5.69 2.45 -13 -9 -1 4.55 1.11 -13 9 -2 61.29 4.86 -13 9 -2 65.47 5.27 13 -9 2 62.91 5.78 -13 -9 -2 64.46 3.48 -13 9 -3 308.70 12.83 -13 9 -3 305.33 12.44 13 -9 3 355.69 14.53 13 -9 3 319.51 14.53 -13 9 -4 107.60 6.92 -13 9 -4 110.89 7.22 13 -9 4 108.66 7.86 13 -9 4 122.82 8.49 -13 9 -5 701.14 22.80 -13 9 -5 638.68 22.57 13 -9 5 641.47 24.34 13 -9 5 718.00 24.62 -13 9 -6 406.22 15.88 -13 9 -6 418.22 16.54 13 -9 6 386.34 17.54 13 -9 6 378.37 17.24 13 10 -5 89.77 6.72 -13 -10 5 94.05 6.56 13 -10 -5 78.07 6.04 -13 -10 5 78.83 6.75 13 10 -4 9.43 2.87 -13 -10 4 18.40 3.60 13 -10 -4 10.32 2.75 13 10 -3 131.34 8.25 13 -10 -3 133.41 7.51 -13 -10 3 126.12 7.16 -13 -10 3 127.35 7.46 13 10 -2 3.99 1.96 -13 10 2 2.47 1.84 -13 10 2 4.67 1.84 13 -10 -2 2.90 1.71 -13 -10 2 2.44 1.87 -13 -10 2 1.27 1.84 -13 10 1 154.16 7.42 -13 10 1 161.68 7.36 13 10 -1 155.94 7.00 -13 10 1 150.26 8.44 -13 -10 1 152.27 7.36 13 -10 -1 160.66 8.30 13 -10 -1 150.28 9.08 -13 -10 1 159.50 7.38 -13 10 0 222.64 10.30 13 -10 0 219.28 10.07 -13 -10 0 190.42 8.22 13 -10 0 207.29 10.92 13 -10 0 200.24 10.28 -13 -10 0 201.14 7.88 -13 10 -1 43.22 4.32 -13 10 -1 53.28 4.44 13 -10 1 53.90 6.53 -13 -10 -1 50.65 2.64 13 -10 1 62.59 5.71 -13 10 -2 361.05 14.01 -13 10 -2 356.03 13.60 13 -10 2 368.16 15.43 13 -10 2 376.16 16.05 -13 10 -3 140.46 7.78 -13 10 -3 125.28 7.72 13 -10 3 142.36 9.32 13 -10 3 124.34 8.60 -13 10 -4 509.33 18.82 -13 10 -4 534.74 18.59 13 -10 4 519.57 20.75 -13 10 -5 24.03 4.28 -13 10 -5 14.35 3.70 13 -10 5 25.12 4.94 13 -10 5 19.76 4.82 13 11 -3 16.91 3.43 13 -11 -3 18.25 3.70 -13 -11 3 15.22 3.24 13 11 -2 649.78 21.32 13 -11 -2 696.34 22.76 -13 -11 2 699.49 22.03 13 -11 -2 677.27 23.78 -13 -11 2 654.68 21.74 13 -11 -1 109.62 10.94 13 -11 -1 150.09 8.19 -13 -11 1 137.65 6.79 13 -11 0 42.50 8.25 -13 11 -1 383.68 14.03 -13 11 -1 357.57 14.73 13 -11 1 385.91 16.40 -13 11 -2 244.99 10.43 -13 11 -2 192.39 9.92 13 -11 2 249.13 12.17 -13 11 -3 127.85 7.82 13 -11 3 141.26 9.11 -14 0 10 269.74 11.83 -14 0 10 247.19 13.41 14 0 -10 260.65 13.04 -14 0 9 -1.21 1.90 14 0 -9 0.48 1.70 -14 0 9 1.76 2.50 14 0 -9 1.77 2.20 14 0 -8 49.47 5.39 -14 0 8 56.55 4.89 14 0 -8 46.89 4.71 -14 0 8 52.76 5.43 14 0 -7 2.38 2.29 -14 0 7 3.88 2.13 14 0 -7 4.48 2.22 -14 0 7 7.05 2.83 14 0 -6 372.55 14.65 -14 0 6 384.14 14.09 -14 0 6 384.44 14.98 14 0 -5 1.54 1.58 -14 0 5 1.44 1.97 14 0 -4 120.16 6.07 14 0 -4 121.79 6.85 -14 0 4 121.31 6.77 -14 0 4 136.25 6.49 14 0 -3 3.32 1.63 -14 0 3 2.27 1.69 14 0 -3 1.10 1.20 -14 0 3 1.71 1.40 14 0 -2 106.96 5.24 -14 0 2 114.04 6.04 -14 0 2 113.33 5.55 14 0 -2 109.84 5.92 14 0 -1 2.58 1.24 -14 0 1 -0.21 1.05 14 0 -1 1.75 1.26 -14 0 1 -0.88 1.11 -14 0 0 4383.12 157.22 14 0 0 4504.64 157.69 -14 0 -1 5.13 1.61 -14 0 -1 3.40 1.32 14 0 1 3.00 1.41 14 0 1 1.74 1.02 -14 0 -3 0.98 1.13 14 0 3 -0.66 1.04 -14 0 -3 1.45 1.31 -14 0 -4 22.09 2.91 -14 0 -4 16.08 2.47 14 0 4 14.95 2.48 14 0 4 16.99 2.66 14 0 5 -0.92 1.13 -14 0 -5 -0.98 1.04 14 0 5 -1.43 1.17 14 0 6 2015.92 54.39 -14 0 -6 2017.30 53.73 14 0 6 2009.84 54.28 -14 0 -7 2.20 1.72 14 0 7 -1.82 1.49 -14 0 -7 2.19 1.65 14 0 7 0.29 1.58 -14 0 -8 1198.72 34.89 14 0 8 1230.07 35.55 14 0 8 1207.39 35.15 -14 0 -8 1212.56 34.73 -14 0 -9 0.12 1.71 14 0 9 1.70 2.21 -14 0 -10 47.40 4.63 14 0 10 42.64 4.65 14 1 -10 87.07 8.32 -14 1 10 76.15 7.17 14 1 -10 69.04 7.34 14 -1 -10 64.83 6.38 14 -1 -10 73.01 11.60 -14 -1 10 63.74 6.80 -14 -1 10 63.69 5.79 -14 1 9 2.09 1.95 -14 1 9 2.00 2.15 14 1 -9 2.20 2.38 14 1 -9 -0.33 1.57 -14 -1 9 6.34 2.77 14 -1 -9 4.78 2.47 14 -1 -9 1.05 1.97 -14 -1 9 2.10 2.32 14 1 -8 169.67 9.49 -14 1 8 151.65 8.17 14 1 -8 168.60 8.76 14 -1 -8 171.94 8.81 -14 -1 8 173.28 9.76 -14 -1 8 180.24 8.91 14 -1 -8 176.02 9.63 -14 1 7 99.16 6.23 -14 1 7 103.58 7.13 14 1 -7 98.00 6.31 14 1 -7 99.73 6.95 14 -1 -7 92.48 6.15 14 -1 -7 94.74 6.87 -14 -1 7 96.97 7.96 -14 -1 7 100.79 6.30 14 1 -6 2540.95 70.49 -14 1 6 2618.19 70.78 -14 1 6 2624.17 69.29 -14 -1 6 2654.04 71.08 14 -1 -6 2380.95 72.98 -14 -1 6 2559.89 71.52 14 -1 -6 2836.10 71.10 -14 1 5 9.20 2.45 14 1 -5 9.75 2.27 14 1 -5 10.90 2.70 -14 1 5 9.43 2.61 14 -1 -5 9.74 2.57 14 -1 -5 6.44 2.12 -14 -1 5 10.50 2.40 -14 -1 5 6.31 2.29 -14 1 4 1384.04 37.83 -14 1 4 1348.20 38.75 14 1 -4 1331.84 37.47 14 1 -4 1299.70 38.44 14 -1 -4 1388.60 38.94 14 -1 -4 1360.37 37.71 -14 -1 4 1390.18 39.00 -14 -1 4 1372.18 37.84 14 1 -3 67.73 4.12 -14 1 3 66.75 4.37 14 1 -3 72.27 4.90 -14 1 3 59.15 4.64 14 -1 -3 65.92 4.89 -14 -1 3 73.51 5.00 -14 -1 3 69.04 4.35 14 -1 -3 68.28 4.26 -14 1 2 220.39 8.55 -14 1 2 214.28 9.06 14 1 -2 206.43 8.04 14 1 -2 222.64 9.03 -14 -1 2 223.94 8.51 -14 -1 2 235.36 9.22 14 -1 -2 221.74 9.17 14 -1 -2 208.54 8.26 -14 1 1 513.53 16.74 14 1 -1 534.20 15.54 14 1 -1 508.63 16.47 -14 1 1 533.29 16.21 -14 -1 1 513.12 16.52 -14 -1 1 520.77 15.95 14 -1 -1 507.17 15.82 14 -1 -1 515.37 16.84 -14 1 0 1489.30 39.69 -14 1 0 1405.89 40.16 14 1 0 1436.96 38.68 14 1 0 1417.86 39.85 -14 -1 0 1465.52 39.98 14 -1 0 1540.79 40.64 14 -1 0 1508.75 39.33 -14 -1 0 1479.19 39.33 -14 1 -1 1777.04 47.29 14 1 1 1714.93 47.39 -14 1 -1 1841.09 48.06 14 1 1 1748.49 46.11 -14 -1 -1 1846.70 47.62 14 -1 1 1715.66 46.71 14 -1 1 1766.31 48.07 -14 -1 -1 1826.25 46.96 -14 1 -2 517.09 15.76 14 1 2 525.32 15.85 -14 1 -2 507.81 16.18 -14 -1 -2 502.16 15.25 14 -1 2 494.43 16.25 -14 -1 -2 495.12 15.65 -14 1 -3 179.34 7.27 14 1 3 170.52 7.17 -14 1 -3 172.62 7.56 14 -1 3 187.09 7.90 -14 -1 -3 169.36 7.09 -14 -1 -3 184.49 6.93 -14 1 -4 1.53 1.47 14 1 4 2.73 1.37 -14 1 -4 2.21 1.46 14 1 4 2.09 1.36 14 -1 4 0.49 1.33 14 -1 4 1.53 1.46 -14 -1 -4 5.58 1.62 -14 -1 -4 2.51 1.27 14 1 5 549.96 17.47 -14 1 -5 576.17 17.70 14 1 5 567.07 17.50 14 -1 5 547.27 18.21 -14 -1 -5 586.30 17.16 14 -1 5 560.95 18.26 14 1 6 226.80 9.07 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244.36 16.74 -26 3 1 230.39 11.64 26 -3 -1 239.36 10.95 26 -3 -1 215.97 17.18 -26 -3 1 258.25 11.55 26 3 0 26.08 4.98 -26 3 0 30.72 4.96 -26 -3 0 30.92 4.69 -26 -3 0 32.33 5.49 26 -3 0 29.46 4.46 26 -3 0 23.24 7.46 -26 3 -1 859.37 31.10 -26 3 -1 841.37 27.55 26 3 1 823.37 26.83 26 -3 1 824.19 28.65 26 -3 1 805.83 25.96 -26 -3 -1 815.99 26.40 -26 -3 -1 813.30 27.01 -26 3 -2 0.48 1.98 -26 3 -2 2.61 2.60 26 3 2 -2.05 1.92 -26 -3 -2 0.38 1.68 26 -3 2 5.27 2.73 -26 -3 -2 1.75 1.87 -26 3 -3 141.62 9.26 26 3 3 136.83 8.86 -26 3 -3 151.48 9.14 -26 -3 -3 163.02 11.98 -26 -3 -3 140.39 7.96 26 -3 3 150.72 9.78 26 4 -2 22.27 4.53 -26 4 2 19.79 4.06 -26 4 2 21.55 4.79 -26 -4 2 15.86 3.62 26 -4 -2 21.40 3.76 26 -4 -2 13.52 4.54 -26 4 1 3.24 2.63 -26 4 1 0.96 1.99 26 4 -1 0.68 2.22 26 -4 -1 2.69 2.85 -26 -4 1 3.34 2.02 -26 -4 1 4.33 2.31 -26 4 0 195.56 11.18 -26 4 0 218.88 11.10 -26 -4 0 210.97 10.23 26 -4 0 211.53 10.43 26 -4 0 199.20 11.62 -26 4 -1 132.85 8.67 26 4 1 127.29 9.09 -26 4 -1 131.18 9.08 -26 -4 -1 128.91 7.59 26 -4 1 138.73 9.61 26 -4 1 110.00 7.44 -26 4 -2 274.02 13.46 26 4 2 275.53 12.17 -26 4 -2 276.04 13.08 26 -4 2 278.99 14.18 -26 -4 -2 277.18 11.94 -26 -4 -2 269.79 12.78 -27 0 3 3.08 2.63 -27 0 3 -1.56 1.95 27 0 -3 4.99 2.28 27 0 -3 2.49 2.71 27 0 -2 626.81 23.96 -27 0 2 681.32 23.55 -27 0 2 683.08 24.47 27 0 -2 661.62 21.82 27 0 -1 -1.29 2.06 27 0 -1 -2.13 1.65 -27 0 1 1.74 2.40 -27 0 1 2.65 2.51 -27 0 0 93.14 7.22 27 0 0 100.39 7.63 27 0 0 90.18 5.79 -27 0 0 88.47 10.25 -27 0 -1 2.11 2.02 27 0 1 0.85 2.12 -27 0 -2 7.13 2.48 27 0 2 3.24 2.25 -27 0 -3 1.90 2.39 27 0 3 -3.64 2.20 27 1 -3 92.55 7.76 27 1 -3 106.21 6.73 27 -1 -3 90.93 7.79 27 -1 -3 99.65 6.92 -27 1 2 358.87 15.14 27 1 -2 359.30 13.52 27 1 -2 324.40 15.27 -27 1 2 356.49 15.85 -27 -1 2 352.98 14.94 27 -1 -2 336.95 13.74 27 -1 -2 353.67 16.04 -27 -1 2 367.08 15.81 27 1 -1 114.58 7.34 -27 1 1 137.64 8.59 -27 1 1 133.13 8.82 27 1 -1 138.17 8.88 -27 -1 1 137.70 8.68 27 -1 -1 133.01 8.99 27 -1 -1 137.77 7.64 -27 -1 1 112.02 8.78 -27 1 0 154.40 9.40 27 1 0 173.78 9.78 -27 1 0 153.07 9.12 -27 -1 0 157.87 9.30 -27 -1 0 187.08 14.68 27 -1 0 153.68 9.79 27 -1 0 148.84 7.96 27 1 1 9.64 3.35 -27 1 -1 4.01 2.42 -27 1 -1 5.79 2.58 -27 -1 -1 11.48 3.30 27 -1 1 9.68 3.09 -27 -1 -1 10.75 3.47 27 1 2 53.15 5.70 -27 1 -2 50.72 5.31 -27 1 -2 55.22 5.51 -27 -1 -2 60.79 5.50 27 -1 2 55.70 5.75 -27 -1 -2 48.42 5.69 -27 2 2 115.38 8.56 -27 2 2 115.43 8.10 27 2 -2 132.61 8.66 27 -2 -2 125.25 9.16 -27 -2 2 115.16 7.85 27 -2 -2 114.20 7.45 -27 -2 2 119.80 8.27 -27 2 1 266.38 13.40 -27 2 1 287.37 13.26 27 2 -1 297.20 13.50 27 -2 -1 317.91 14.78 -27 -2 1 283.57 13.36 -27 -2 1 281.30 15.80 27 -2 -1 283.19 12.18 -27 2 0 3.50 2.57 27 2 0 2.59 2.70 -27 2 0 2.85 2.62 -27 -2 0 5.04 2.93 -27 -2 0 4.86 2.49 27 -2 0 5.28 2.55 27 -2 0 6.62 2.64 27 2 1 8.75 3.17 -27 2 -1 8.67 3.32 -27 2 -1 8.13 2.93 -27 -2 -1 12.82 3.14 27 -2 1 14.26 3.66 -27 -2 -1 10.50 2.96 27 2 2 7.49 3.21 -27 2 -2 9.55 3.27 -27 2 -2 8.57 3.04 27 -2 2 9.41 3.39 -27 -2 -2 10.50 3.20 -27 -2 -2 11.93 3.01 -27 3 1 222.71 12.03 27 3 -1 210.00 11.12 -27 3 1 213.56 11.21 -27 -3 1 214.78 11.90 27 -3 -1 219.36 12.14 27 -3 -1 193.78 12.43 -27 -3 1 208.65 11.05 -27 3 0 2.47 2.64 -27 3 0 3.49 2.79 27 3 0 2.45 2.32 27 -3 0 3.89 2.96 -27 -3 0 -0.30 2.31 -27 -3 0 4.62 2.25 27 -3 0 1.68 2.41 -27 3 -1 1.73 2.33 27 3 1 4.65 2.55 -27 3 -1 5.88 2.97 27 -3 1 5.33 2.84 -27 -3 -1 3.76 1.97 -27 -3 -1 3.05 2.26 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 29710 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.76417(10) 0.4006(2) 0.7929(2) 0.0203(4) Uani 1 1 d . . . . . C2 C 0.82161(11) 0.3783(3) 0.8561(3) 0.0281(5) Uani 1 1 d . . . . . H2 H 0.84151 0.445985 0.909617 0.034 Uiso 1 1 calc R U . . . C3 C 0.84949(11) 0.2552(3) 0.8399(3) 0.0328(6) Uani 1 1 d . . . . . H3 H 0.888691 0.237358 0.882857 0.039 Uiso 1 1 calc R U . . . C4 C 0.81980(12) 0.1594(3) 0.7611(3) 0.0320(6) Uani 1 1 d . . . . . H4 H 0.837914 0.074191 0.74947 0.038 Uiso 1 1 calc R U . . . C5 C 0.76323(11) 0.1893(2) 0.6993(3) 0.0297(5) Uani 1 1 d . . . . . H5 H 0.742954 0.123371 0.643981 0.036 Uiso 1 1 calc R U . . . C6 C 0.72983(10) 0.5264(2) 0.8203(2) 0.0196(4) Uani 1 1 d . . . . . C7 C 0.67666(11) 0.5247(2) 0.9030(3) 0.0254(5) Uani 1 1 d . . . . . H7 H 0.660094 0.442843 0.935283 0.031 Uiso 1 1 calc R U . . . C8 C 0.64795(12) 0.6426(3) 0.9381(3) 0.0283(5) Uani 1 1 d . . . . . H8 H 0.611962 0.64313 0.996018 0.034 Uiso 1 1 calc R U . . . C9 C 0.67242(12) 0.7594(2) 0.8875(3) 0.0306(5) Uani 1 1 d . . . . . H9 H 0.653766 0.842018 0.910225 0.037 Uiso 1 1 calc R U . . . C10 C 0.72455(13) 0.7539(2) 0.8034(3) 0.0329(6) Uani 1 1 d . . . . . H10 H 0.740659 0.834492 0.766584 0.04 Uiso 1 1 calc R U . . . C11 C 0.58407(12) 0.4436(2) 0.2724(2) 0.0272(5) Uani 1 1 d . . . . . C12 C 0.52154(14) 0.4587(3) 0.2004(3) 0.0358(6) Uani 1 1 d . . . . . H12A H 0.521729 0.416212 0.105853 0.043 Uiso 1 1 calc R U . . . H12B H 0.510651 0.55343 0.189105 0.043 Uiso 1 1 calc R U . . . C13 C 0.47586(12) 0.3897(3) 0.2979(3) 0.0334(6) Uani 1 1 d . . . . . H13A H 0.440608 0.448909 0.320995 0.04 Uiso 1 1 calc R U . . . H13B H 0.459365 0.307983 0.253386 0.04 Uiso 1 1 calc R U . . . C14 C 0.51330(11) 0.3572(2) 0.4289(3) 0.0256(5) Uani 1 1 d . . . . . C15 C 0.94431(12) 0.8268(3) 0.4485(3) 0.0346(6) Uani 1 1 d . . . . . C16 C 0.99938(13) 0.8117(4) 0.3510(3) 0.0465(8) Uani 1 1 d . . . . . H16A H 0.992585 0.861889 0.262193 0.056 Uiso 1 1 calc R U . . . H16B H 1.037848 0.844562 0.397327 0.056 Uiso 1 1 calc R U . . . C17 C 1.00419(14) 0.6650(4) 0.3212(3) 0.0475(8) Uani 1 1 d . . . . . H17A H 1.044896 0.630025 0.353505 0.057 Uiso 1 1 calc R U . . . H17B H 0.999504 0.647301 0.218541 0.057 Uiso 1 1 calc R U . . . C18 C 0.95169(12) 0.6023(3) 0.4031(3) 0.0380(7) Uani 1 1 d . . . . . I1 I 0.64794(2) 0.35208(2) 0.55151(2) 0.02045(5) Uani 1 1 d . . . . . I2 I 0.84472(2) 0.66693(2) 0.60855(2) 0.02603(5) Uani 1 1 d . . . . . N1 N 0.73570(9) 0.30774(19) 0.7143(2) 0.0228(4) Uani 1 1 d . . . . . N2 N 0.75368(9) 0.6401(2) 0.7710(2) 0.0260(4) Uani 1 1 d . . . . . N3 N 0.57488(9) 0.38547(19) 0.4038(2) 0.0228(4) Uani 1 1 d . . . . . N4 N 0.92061(9) 0.7018(2) 0.4747(2) 0.0295(4) Uani 1 1 d . . . . . O1 O 0.63414(9) 0.47776(19) 0.22679(19) 0.0365(4) Uani 1 1 d . . . . . O2 O 0.49340(9) 0.3127(2) 0.5393(2) 0.0356(4) Uani 1 1 d . . . . . O3 O 0.92395(9) 0.9277(2) 0.4983(2) 0.0454(5) Uani 1 1 d . . . . . O4 O 0.93786(10) 0.4870(2) 0.4080(2) 0.0498(6) Uani 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 C1 0.0181(10) 0.0207(10) 0.0222(10) 0.0053(8) 0.0030(8) 0.0010(8) C2 0.0218(11) 0.0281(12) 0.0343(13) 0.0012(10) -0.0040(9) -0.0013(9) C3 0.0194(11) 0.0371(14) 0.0418(15) 0.0059(12) -0.0033(10) 0.0055(10) C4 0.0267(12) 0.0273(13) 0.0421(15) 0.0042(11) 0.0006(10) 0.0101(10) C5 0.0270(12) 0.0228(12) 0.0393(14) -0.0031(10) -0.0029(10) 0.0059(9) C6 0.0204(10) 0.0198(10) 0.0186(10) 0.0028(8) -0.0026(8) -0.0010(8) C7 0.0253(11) 0.0225(11) 0.0285(12) 0.0063(9) 0.0051(9) 0.0023(9) C8 0.0278(12) 0.0308(13) 0.0264(12) 0.0038(10) 0.0033(9) 0.0076(10) C9 0.0388(14) 0.0217(12) 0.0312(13) -0.0004(10) -0.0022(10) 0.0076(10) C10 0.0388(14) 0.0197(12) 0.0404(14) 0.0052(10) 0.0031(11) -0.0015(10) C11 0.0456(14) 0.0159(10) 0.0201(11) -0.0042(8) -0.0019(10) 0.0013(10) C12 0.0547(17) 0.0266(13) 0.0260(12) 0.0006(10) -0.0155(11) 0.0030(12) C13 0.0338(13) 0.0352(14) 0.0312(13) -0.0082(11) -0.0118(10) 0.0107(11) C14 0.0276(11) 0.0214(11) 0.0277(12) -0.0047(9) -0.0029(9) 0.0031(9) C15 0.0263(12) 0.0451(17) 0.0323(13) 0.0190(12) -0.0115(10) -0.0112(11) C16 0.0313(14) 0.076(2) 0.0324(14) 0.0202(15) -0.0028(11) -0.0230(14) C17 0.0394(15) 0.080(2) 0.0234(13) -0.0101(14) 0.0088(11) -0.0310(15) C18 0.0301(13) 0.0635(19) 0.0205(12) -0.0135(12) 0.0034(10) -0.0215(13) I1 0.02380(7) 0.01683(7) 0.02070(7) -0.00065(5) -0.00064(5) 0.00345(5) I2 0.02391(8) 0.03018(9) 0.02399(8) 0.00627(6) -0.00064(5) -0.00645(6) N1 0.0209(9) 0.0206(9) 0.0269(10) 0.0007(8) -0.0008(7) 0.0038(7) N2 0.0268(10) 0.0220(10) 0.0293(10) 0.0039(8) 0.0022(8) -0.0021(8) N3 0.0270(10) 0.0212(9) 0.0202(9) 0.0009(7) -0.0031(7) 0.0026(7) N4 0.0243(10) 0.0424(12) 0.0216(9) 0.0069(9) -0.0002(8) -0.0122(9) O1 0.0508(12) 0.0326(10) 0.0261(9) 0.0007(8) 0.0080(8) -0.0075(9) O2 0.0310(9) 0.0415(11) 0.0343(10) 0.0067(8) 0.0014(8) -0.0024(8) O3 0.0315(10) 0.0386(12) 0.0660(14) 0.0228(11) -0.0096(9) -0.0059(9) O4 0.0404(11) 0.0594(14) 0.0499(12) -0.0299(11) 0.0155(9) -0.0275(10) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.8(2) . . ? N1 C1 C6 117.79(19) . . ? C2 C1 C6 120.2(2) . . ? C1 C2 C3 118.8(2) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 119.3(2) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 118.7(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.6(2) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? N2 C6 C7 121.6(2) . . ? N2 C6 C1 118.52(19) . . ? C7 C6 C1 119.77(19) . . ? C8 C7 C6 119.6(2) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C9 C8 C7 118.8(2) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 118.6(2) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 123.1(2) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? O1 C11 N3 124.7(2) . . ? O1 C11 C12 127.0(2) . . ? N3 C11 C12 108.3(2) . . ? C11 C12 C13 104.9(2) . . ? C11 C12 H12A 110.8 . . ? C13 C12 H12A 110.8 . . ? C11 C12 H12B 110.8 . . ? C13 C12 H12B 110.8 . . ? H12A C12 H12B 108.8 . . ? C14 C13 C12 104.7(2) . . ? C14 C13 H13A 110.8 . . ? C12 C13 H13A 110.8 . . ? C14 C13 H13B 110.8 . . ? C12 C13 H13B 110.8 . . ? H13A C13 H13B 108.9 . . ? O2 C14 N3 124.6(2) . . ? O2 C14 C13 126.5(2) . . ? N3 C14 C13 108.8(2) . . ? O3 C15 N4 124.5(3) . . ? O3 C15 C16 127.6(3) . . ? N4 C15 C16 107.9(3) . . ? C17 C16 C15 105.5(2) . . ? C17 C16 H16A 110.6 . . ? C15 C16 H16A 110.6 . . ? C17 C16 H16B 110.6 . . ? C15 C16 H16B 110.6 . . ? H16A C16 H16B 108.8 . . ? C16 C17 C18 105.2(3) . . ? C16 C17 H17A 110.7 . . ? C18 C17 H17A 110.7 . . ? C16 C17 H17B 110.7 . . ? C18 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? O4 C18 N4 124.3(2) . . ? O4 C18 C17 127.7(3) . . ? N4 C18 C17 108.0(3) . . ? N3 I1 N1 177.27(7) . . ? N4 I2 N2 176.52(8) . . ? C1 N1 C5 118.8(2) . . ? C1 N1 I1 124.25(14) . . ? C5 N1 I1 115.58(16) . . ? C6 N2 C10 118.2(2) . . ? C6 N2 I2 127.26(15) . . ? C10 N2 I2 114.42(16) . . ? C14 N3 C11 112.6(2) . . ? C14 N3 I1 124.26(16) . . ? C11 N3 I1 123.13(16) . . ? C15 N4 C18 113.3(2) . . ? C15 N4 I2 123.29(19) . . ? C18 N4 I2 123.44(18) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.340(3) . ? C1 C2 1.387(3) . ? C1 C6 1.491(3) . ? C2 C3 1.387(4) . ? C2 H2 0.95 . ? C3 C4 1.375(4) . ? C3 H3 0.95 . ? C4 C5 1.379(4) . ? C4 H4 0.95 . ? C5 N1 1.342(3) . ? C5 H5 0.95 . ? C6 N2 1.341(3) . ? C6 C7 1.388(3) . ? C7 C8 1.381(3) . ? C7 H7 0.95 . ? C8 C9 1.376(4) . ? C8 H8 0.95 . ? C9 C10 1.378(4) . ? C9 H9 0.95 . ? C10 N2 1.344(3) . ? C10 H10 0.95 . ? C11 O1 1.211(3) . ? C11 N3 1.388(3) . ? C11 C12 1.510(4) . ? C12 C13 1.518(4) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.508(3) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 O2 1.215(3) . ? C14 N3 1.375(3) . ? C15 O3 1.205(4) . ? C15 N4 1.382(3) . ? C15 C16 1.511(4) . ? C16 C17 1.510(5) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.511(4) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 O4 1.201(4) . ? C18 N4 1.384(4) . ? I1 N3 2.1212(19) . ? I1 N1 2.4673(19) . ? I2 N4 2.099(2) . ? I2 N2 2.507(2) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.4(4) . . . . ? C6 C1 C2 C3 173.6(2) . . . . ? C1 C2 C3 C4 0.4(4) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? C3 C4 C5 N1 -0.7(4) . . . . ? N1 C1 C6 N2 -117.4(2) . . . . ? C2 C1 C6 N2 67.3(3) . . . . ? N1 C1 C6 C7 66.7(3) . . . . ? C2 C1 C6 C7 -108.6(3) . . . . ? N2 C6 C7 C8 -1.2(4) . . . . ? C1 C6 C7 C8 174.6(2) . . . . ? C6 C7 C8 C9 1.1(4) . . . . ? C7 C8 C9 C10 0.2(4) . . . . ? C8 C9 C10 N2 -1.7(4) . . . . ? O1 C11 C12 C13 175.5(2) . . . . ? N3 C11 C12 C13 -5.8(3) . . . . ? C11 C12 C13 C14 8.0(3) . . . . ? C12 C13 C14 O2 172.6(2) . . . . ? C12 C13 C14 N3 -7.8(3) . . . . ? O3 C15 C16 C17 -179.9(3) . . . . ? N4 C15 C16 C17 1.2(3) . . . . ? C15 C16 C17 C18 -0.1(3) . . . . ? C16 C17 C18 O4 179.0(3) . . . . ? C16 C17 C18 N4 -1.0(3) . . . . ? C2 C1 N1 C5 1.3(3) . . . . ? C6 C1 N1 C5 -173.9(2) . . . . ? C2 C1 N1 I1 -164.43(17) . . . . ? C6 C1 N1 I1 20.4(3) . . . . ? C4 C5 N1 C1 -0.2(4) . . . . ? C4 C5 N1 I1 166.7(2) . . . . ? C7 C6 N2 C10 -0.2(3) . . . . ? C1 C6 N2 C10 -176.0(2) . . . . ? C7 C6 N2 I2 -175.94(17) . . . . ? C1 C6 N2 I2 8.2(3) . . . . ? C9 C10 N2 C6 1.7(4) . . . . ? C9 C10 N2 I2 178.0(2) . . . . ? O2 C14 N3 C11 -175.9(2) . . . . ? C13 C14 N3 C11 4.5(3) . . . . ? O2 C14 N3 I1 1.7(3) . . . . ? C13 C14 N3 I1 -177.95(15) . . . . ? O1 C11 N3 C14 179.7(2) . . . . ? C12 C11 N3 C14 0.9(3) . . . . ? O1 C11 N3 I1 2.1(3) . . . . ? C12 C11 N3 I1 -176.70(15) . . . . ? O3 C15 N4 C18 179.1(3) . . . . ? C16 C15 N4 C18 -1.9(3) . . . . ? O3 C15 N4 I2 -0.5(4) . . . . ? C16 C15 N4 I2 178.48(16) . . . . ? O4 C18 N4 C15 -178.1(3) . . . . ? C17 C18 N4 C15 1.8(3) . . . . ? O4 C18 N4 I2 1.5(4) . . . . ? C17 C18 N4 I2 -178.55(17) . . . . ?