#------------------------------------------------------------------------------ #$Date: 2024-09-26 01:33:43 +0300 (Thu, 26 Sep 2024) $ #$Revision: 294892 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/93/7249379.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_7249379 loop_ _publ_author_name 'Jeon, Ie-Rang' 'Jeannin, olivier' 'Robert, Antoine' 'Barriere, Frederic' 'Fourmigu\'e, Marc' _publ_section_title ; N-iodophtalimide as halogen bond donor, a comparison with N-iodosuccinimide and N-iodosaccharin† ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00654B _journal_year 2024 _chemical_formula_moiety 'C15 H14 I N3 O2' _chemical_formula_sum 'C15 H14 I N3 O2' _chemical_formula_weight 395.19 _chemical_name_common (NIPht)(DMAP) _chemical_name_systematic (N-iodophtalimide)(4-dimethylaminopyridine) _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 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 2024-03-29T15:54:07-00:00 _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 100.135(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.2802(9) _cell_length_b 11.8980(11) _cell_length_c 13.5467(11) _cell_measurement_reflns_used 9853 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.44 _cell_measurement_theta_min 2.81 _cell_measurement_wavelength 0.71073 _cell_volume 1472.4(2) _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)' _diffrn_ambient_temperature 150(2) _diffrn_detector CMOS-PHOTON70 _diffrn_detector_area_resol_mean 7.39 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'D8 VENTURE Bruker AXS' _diffrn_measurement_method 'rotation images' _diffrn_orient_matrix_UB_11 -0.044896 _diffrn_orient_matrix_UB_12 -0.066363 _diffrn_orient_matrix_UB_13 0.028282 _diffrn_orient_matrix_UB_21 -0.099773 _diffrn_orient_matrix_UB_22 0.031293 _diffrn_orient_matrix_UB_23 -0.024941 _diffrn_orient_matrix_UB_31 -0.003483 _diffrn_orient_matrix_UB_32 -0.040997 _diffrn_orient_matrix_UB_33 -0.064818 _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 0.0249 _diffrn_reflns_av_unetI/netI 0.0176 _diffrn_reflns_Laue_measured_fraction_full 0.979 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 20445 _diffrn_reflns_point_group_measured_fraction_full 0.979 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.452 _diffrn_reflns_theta_min 2.811 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.183 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 776 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CH2Cl2/pentane' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.339 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 192 _refine_ls_number_reflns 3308 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.115 _refine_ls_R_factor_all 0.0182 _refine_ls_R_factor_gt 0.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0117P)^2^+0.8853P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0399 _reflns_Friedel_coverage 0 _reflns_number_gt 3086 _reflns_number_total 3308 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00654b1.cif _cod_data_source_block shelx_CCDC2 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7249379 _shelx_res_file ; TITL shelxt_a.res in P2(1)/n shelx.res created by SHELXL-2019/3 at 15:53:50 on 29-Mar-2024 CELL 0.71073 9.2802 11.8980 13.5467 90.000 100.135 90.000 ZERR 4.00 0.0009 0.0011 0.0011 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H I N O UNIT 60 56 4 12 8 MERG 2 OMIT 0 4 0 OMIT 1 0 3 OMIT 0 1 1 OMIT -1 4 1 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP -123.00 WGHT 0.011700 0.885300 FVAR 0.56313 C1 1 0.087373 0.303898 0.453134 11.00000 0.03336 0.02181 = 0.02042 -0.00269 -0.00083 -0.00167 AFIX 43 H1 2 0.078429 0.257400 0.395366 11.00000 -1.20000 AFIX 0 C2 1 -0.021085 0.299920 0.509670 11.00000 0.02749 0.02084 = 0.02174 0.00014 -0.00309 -0.00469 AFIX 43 H2 2 -0.103498 0.252496 0.490028 11.00000 -1.20000 AFIX 0 C3 1 -0.010710 0.366475 0.597560 11.00000 0.02222 0.01864 = 0.02098 0.00253 -0.00083 0.00050 C4 1 0.116089 0.434792 0.619844 11.00000 0.02549 0.02113 = 0.02361 -0.00547 0.00042 -0.00259 AFIX 43 H4 2 0.130794 0.480802 0.678067 11.00000 -1.20000 AFIX 0 C5 1 0.217015 0.434492 0.557706 11.00000 0.02546 0.02347 = 0.02633 -0.00304 0.00160 -0.00368 AFIX 43 H5 2 0.299704 0.482413 0.573758 11.00000 -1.20000 AFIX 0 C6 1 -0.092512 0.428568 0.750060 11.00000 0.02927 0.03391 = 0.02563 -0.00273 0.00486 0.00365 AFIX 137 H6A 2 -0.004911 0.400730 0.794470 11.00000 -1.50000 H6B 2 -0.178035 0.418582 0.782532 11.00000 -1.50000 H6C 2 -0.080253 0.508536 0.736306 11.00000 -1.50000 AFIX 0 C7 1 -0.246030 0.298392 0.628455 11.00000 0.02646 0.03962 = 0.03259 0.00334 0.00270 -0.00814 AFIX 137 H7A 2 -0.292135 0.315897 0.559412 11.00000 -1.50000 H7B 2 -0.314349 0.315568 0.673914 11.00000 -1.50000 H7C 2 -0.220474 0.218430 0.633565 11.00000 -1.50000 AFIX 0 C8 1 0.540860 0.469075 0.201826 11.00000 0.02537 0.02597 = 0.02490 -0.00052 0.00336 -0.00082 C9 1 0.664927 0.316551 0.278605 11.00000 0.02247 0.02213 = 0.02545 -0.00466 -0.00206 -0.00312 C10 1 0.738952 0.351085 0.193729 11.00000 0.02329 0.02197 = 0.02464 -0.00640 -0.00090 -0.00383 C11 1 0.662676 0.442612 0.146379 11.00000 0.02317 0.02202 = 0.02485 -0.00484 0.00168 -0.00195 C12 1 0.702209 0.492314 0.063205 11.00000 0.03228 0.02610 = 0.02743 -0.00090 0.00568 -0.00347 AFIX 43 H12 2 0.649699 0.554626 0.031015 11.00000 -1.20000 AFIX 0 C13 1 0.822546 0.447250 0.028317 11.00000 0.03515 0.03481 = 0.02976 -0.00701 0.01139 -0.00857 AFIX 43 H13 2 0.851764 0.478760 -0.029510 11.00000 -1.20000 AFIX 0 C14 1 0.900826 0.356977 0.076496 11.00000 0.02701 0.03451 = 0.04035 -0.01350 0.01031 -0.00321 AFIX 43 H14 2 0.983643 0.329092 0.051853 11.00000 -1.20000 AFIX 0 C15 1 0.859490 0.306823 0.160445 11.00000 0.02356 0.02600 = 0.03515 -0.00872 0.00066 -0.00016 AFIX 43 H15 2 0.912027 0.244880 0.193290 11.00000 -1.20000 AFIX 0 I1 3 0.385715 0.378105 0.375521 11.00000 0.02559 0.02395 = 0.02040 0.00013 0.00229 0.00040 N1 4 0.206080 0.370348 0.475223 11.00000 0.02692 0.02339 = 0.02211 -0.00051 0.00337 0.00007 N2 4 -0.113892 0.365719 0.655921 11.00000 0.02423 0.02790 = 0.02545 -0.00140 0.00258 -0.00341 N3 4 0.548169 0.389802 0.277988 11.00000 0.02464 0.02578 = 0.02361 0.00165 0.00341 0.00081 O1 5 0.452051 0.545065 0.185146 11.00000 0.03510 0.03431 = 0.03844 0.01066 0.01122 0.01315 O2 5 0.698451 0.240303 0.337688 11.00000 0.03023 0.02882 = 0.03138 0.00560 -0.00351 0.00078 HKLF 4 REM shelxt_a.res in P2(1)/n REM wR2 = 0.0399, GooF = S = 1.115, Restrained GooF = 1.115 for all data REM R1 = 0.0160 for 3086 Fo > 4sig(Fo) and 0.0182 for all 3308 data REM 192 parameters refined using 0 restraints END WGHT 0.0110 0.9092 REM Highest difference peak 0.339, deepest hole -0.518, 1-sigma level 0.055 Q1 1 0.0538 0.3926 0.6121 11.00000 0.05 0.34 Q2 1 0.6120 0.4642 0.1731 11.00000 0.05 0.32 Q3 1 0.6981 0.3918 0.1682 11.00000 0.05 0.31 Q4 1 0.7059 0.3243 0.2369 11.00000 0.05 0.30 Q5 1 -0.0037 0.3291 0.5635 11.00000 0.05 0.29 Q6 1 0.6048 0.3483 0.2779 11.00000 0.05 0.27 Q7 1 0.5425 0.4262 0.2439 11.00000 0.05 0.27 Q8 1 0.2093 0.4010 0.5156 11.00000 0.05 0.26 Q9 1 -0.1072 0.3999 0.6957 11.00000 0.05 0.25 Q10 1 0.1564 0.3337 0.4702 11.00000 0.05 0.24 Q11 1 0.0200 0.3150 0.4789 11.00000 0.05 0.23 Q12 1 -0.1660 0.3378 0.6433 11.00000 0.05 0.22 Q13 1 0.0402 0.2901 0.4956 11.00000 0.05 0.22 Q14 1 0.3109 0.3636 0.3715 11.00000 0.05 0.21 Q15 1 0.8403 0.3838 0.0392 11.00000 0.05 0.21 Q16 1 0.8825 0.3372 0.1260 11.00000 0.05 0.21 Q17 1 -0.0662 0.3691 0.6227 11.00000 0.05 0.21 Q18 1 0.8027 0.3344 0.1849 11.00000 0.05 0.21 Q19 1 0.8612 0.3146 0.1072 11.00000 0.05 0.20 Q20 1 0.1864 0.4181 0.6023 11.00000 0.05 0.20 ; _shelx_res_checksum 44055 _shelx_hkl_file ; 1 0 0 0.18965 0.18326 2 1 0 0 1.10691 0.27369 3 1 0 0 0.63837 0.21618 4 -1 0 0 0.80839 0.28707 2 2 0 0 2.20884 0.58735 4 2 0 0 2.85312 0.69428 3 2 0 0 2.78446 0.76822 2 -2 0 0 1.49891 0.55685 4 -2 0 0 1.40915 0.63157 3 -2 0 0 2.16953 0.66318 2 3 0 0 0.40914 0.4849 4 3 0 0 0.32898 0.63121 3 -3 0 0 2.43134 0.91399 2 -3 0 0 1.43223 0.63995 4 -3 0 0 0.74352 0.63472 3 -4 0 0 5870.81 169.719 1 4 0 0 5768.79 168.392 1 5 0 0 -0.0287 1.10363 2 5 0 0 1.70468 1.06309 4 -5 0 0 -2.3883 0.83828 3 -5 0 0 -0.6171 0.8744 4 -5 0 0 -1.32 1.00845 2 5 0 0 0.01972 1.20409 3 6 0 0 664.363 19.4618 2 6 0 0 655.892 18.3577 4 -6 0 0 670.282 19.1973 3 -6 0 0 636.60 19.2755 2 6 0 0 666.065 18.9816 3 -6 0 0 638.109 18.3748 4 -7 0 0 -3.0423 1.19832 4 -7 0 0 0.7365 1.85366 2 -7 0 0 -3.8418 1.51539 3 7 0 0 1.25587 1.89008 3 7 0 0 -1.0248 1.70815 2 7 0 0 -0.7134 1.51299 4 -8 0 0 1384.19 36.6529 4 8 0 0 1399.47 36.5146 4 -8 0 0 1350.41 37.9021 2 -8 0 0 1386.99 37.6235 3 8 0 0 1465.59 38.3907 2 8 0 0 1362.91 37.0929 3 -9 0 0 -0.4342 2.11957 3 9 0 0 -3.5736 2.00872 2 -9 0 0 -1.3759 1.84539 4 9 0 0 -2.7141 1.83017 3 -10 0 0 529.097 18.2778 4 10 0 0 557.703 19.0786 3 -10 0 0 578.419 20.2255 2 10 0 0 530.105 19.6992 2 -10 0 0 530.594 19.332 3 11 0 0 -0.2601 2.77829 3 -11 0 0 -1.209 1.98348 4 -11 0 0 -5.0265 2.87447 2 11 0 0 -0.2067 2.71858 2 -11 0 0 -6.5278 1.95246 3 -1 -1 0 2104.87 59.9364 1 1 -1 0 2235.89 62.2309 1 -1 1 0 2214.69 61.757 1 1 1 0 2130.48 60.2337 1 -2 -1 0 3679.32 104.108 1 2 -1 0 3760.18 104.277 1 2 1 0 3780.87 104.058 1 -3 -1 0 203.389 6.4845 4 -3 -1 0 203.752 6.9276 3 -3 -1 0 214.85 6.97761 2 3 -1 0 228.45 6.70017 3 3 -1 0 216.81 7.11558 2 3 -1 0 209.324 6.5275 4 -3 1 0 206.094 6.56069 3 3 1 0 206.212 6.77259 3 3 1 0 213.23 6.51566 4 -3 1 0 231.544 7.09625 2 -3 1 0 215.601 6.53522 4 3 1 0 198.075 6.9495 2 -4 -1 0 1287.23 57.7587 1 4 -1 0 1176.75 55.6227 1 -4 1 0 1228.00 57.4315 1 4 1 0 1279.42 56.583 1 5 -1 0 1147.98 28.9306 3 5 -1 0 1108.53 28.6629 4 -5 -1 0 1107.14 28.6817 4 -5 -1 0 1165.00 29.6685 2 -5 -1 0 1125.78 29.4326 3 5 -1 0 1082.42 29.4095 2 5 1 0 1157.76 29.2976 3 5 1 0 1143.65 29.5947 2 -5 1 0 1113.30 28.9935 3 6 -1 0 3827.53 138.037 1 -6 1 0 3955.52 142.091 1 -7 -1 0 65.3227 5.29019 2 7 -1 0 72.9505 5.02931 3 -7 -1 0 67.6095 5.28361 3 7 -1 0 79.4963 5.66459 2 -7 -1 0 80.0625 5.17901 4 -7 1 0 78.3429 5.52805 2 -7 1 0 84.4174 5.39878 3 -7 1 0 68.0363 4.86104 4 7 1 0 73.4515 5.56294 2 7 1 0 76.827 5.11637 3 7 1 0 79.6462 4.79518 4 -8 -1 0 148.609 8.09025 3 -8 -1 0 156.265 8.42452 2 8 -1 0 164.678 8.62918 2 8 -1 0 149.568 7.63974 3 -8 -1 0 140.512 7.36891 4 -8 1 0 146.53 7.85134 3 -8 1 0 150.418 8.18211 2 -8 1 0 148.054 7.48422 4 8 1 0 165.447 8.79026 2 8 1 0 160.092 8.04943 3 8 1 0 151.359 7.29264 4 9 -1 0 99.351 6.7505 3 -9 -1 0 94.3931 7.17505 3 -9 -1 0 110.509 7.658 2 9 -1 0 98.357 7.36722 2 -9 -1 0 101.828 6.48441 4 9 1 0 99.0591 7.0289 3 9 1 0 93.4971 6.14887 4 9 1 0 108.792 7.42112 2 -9 1 0 104.35 7.39213 2 -9 1 0 100.275 6.92998 3 -9 1 0 107.133 6.47928 4 -10 -1 0 462.346 17.8173 3 -10 -1 0 482.62 16.6851 4 10 -1 0 458.034 17.8609 2 -10 -1 0 480.393 18.1715 2 10 -1 0 466.96 16.9312 3 10 1 0 480.023 18.0443 2 -10 1 0 433.295 17.051 3 10 1 0 471.20 17.3249 3 -10 1 0 462.765 16.4653 4 -10 1 0 473.887 18.194 2 10 1 0 474.311 16.2218 4 -11 -1 0 41.7983 5.80531 3 11 -1 0 50.9147 6.40993 2 -11 -1 0 48.7286 5.60576 4 -11 -1 0 49.9749 6.69652 2 11 -1 0 46.9343 5.69006 3 -11 1 0 59.553 6.4768 3 -11 1 0 38.7021 5.10688 4 -11 1 0 50.8579 6.50888 2 11 1 0 51.1483 6.41766 2 11 1 0 64.3964 6.43435 3 0 2 0 168.671 4.82939 2 2 -2 0 206.259 5.83722 3 -2 -2 0 211.922 6.35793 4 -2 -2 0 216.099 6.51006 2 2 -2 0 204.983 6.4882 2 -2 -2 0 211.116 6.4206 3 -2 2 0 200.337 5.83462 3 2 2 0 206.795 6.46461 2 2 2 0 210.005 6.2996 4 -2 2 0 228.257 6.65175 2 2 2 0 213.689 6.39255 3 3 -2 0 1743.12 67.6738 1 -3 -2 0 1675.97 63.3906 1 3 -2 0 1646.53 63.4057 1 3 2 0 1669.25 63.4891 1 4 -2 0 66.1691 3.42978 3 -4 -2 0 70.4348 4.1257 4 -4 -2 0 63.5398 3.73331 3 -4 -2 0 84.1459 4.21667 2 4 -2 0 73.6063 4.00708 2 -4 2 0 73.5073 4.05101 2 -4 2 0 70.3376 3.60503 4 4 2 0 69.6207 3.50529 4 4 2 0 71.3261 3.92438 2 -4 2 0 74.6758 3.67222 3 -5 -2 0 1475.53 37.1058 3 5 -2 0 1448.83 36.1714 3 5 2 0 1455.93 37.0942 2 5 2 0 1448.95 36.804 3 -5 2 0 1443.02 36.35 3 -6 -2 0 -3.1575 1.19459 4 -6 -2 0 -0.044 1.59269 2 -6 -2 0 2.32151 1.67333 3 6 -2 0 -2.6862 1.35236 2 6 -2 0 2.38829 1.52771 3 -6 2 0 0.81219 1.62916 4 -6 2 0 3.68363 2.00963 2 6 2 0 -0.1672 1.66524 2 6 2 0 4.43974 1.81209 3 6 2 0 0.09491 1.50448 4 -6 2 0 0.8359 1.42213 3 7 -2 0 2992.96 72.152 3 7 2 0 2937.93 72.7644 3 7 2 0 2975.40 73.3327 2 8 -2 0 42.2347 4.2739 3 -8 -2 0 43.428 5.05634 2 -8 -2 0 39.5467 4.78449 3 -8 -2 0 44.6108 4.51084 4 8 -2 0 48.8196 5.00251 2 -8 2 0 46.8498 5.1534 2 8 2 0 32.9555 4.18068 3 8 2 0 40.744 4.13872 4 8 2 0 41.7644 5.53744 2 -8 2 0 42.5829 4.45777 3 -8 2 0 42.3345 4.45325 4 -9 -2 0 20.9165 4.09363 2 9 -2 0 9.10752 3.4513 2 -9 -2 0 17.1444 3.3012 4 -9 -2 0 13.6139 3.66966 3 -9 2 0 11.5827 2.9235 4 9 2 0 12.2537 2.87871 4 9 2 0 16.724 3.38258 3 -9 2 0 12.5384 3.8404 3 -9 2 0 24.1946 4.29124 2 9 2 0 10.1328 3.15419 2 -10 -2 0 -1.161 2.13795 4 10 -2 0 -2.1447 2.61184 2 10 -2 0 -1.4994 1.98164 3 -10 -2 0 1.89025 2.82358 2 -10 -2 0 -2.1897 2.2054 3 -10 2 0 -4.9573 2.37206 2 10 2 0 -1.7926 2.12858 2 10 2 0 1.45661 2.58234 3 -10 2 0 -1.8946 1.98141 4 10 2 0 2.61474 2.11079 4 -10 2 0 -1.1138 2.17222 3 -11 -2 0 867.748 28.612 2 11 -2 0 854.932 28.4309 2 -11 -2 0 907.253 28.8115 3 -11 -2 0 873.769 26.8237 4 11 -2 0 840.941 26.6651 3 11 2 0 865.785 26.0456 4 -11 2 0 887.101 28.6774 2 -11 2 0 785.263 29.3514 3 -11 2 0 849.919 26.4542 4 11 2 0 858.621 28.4415 2 11 2 0 852.268 27.5399 3 0 3 0 0.51044 0.48294 2 1 -3 0 5.19483 0.95802 2 -1 -3 0 4.64781 0.89712 3 1 -3 0 5.10151 0.56942 3 1 3 0 5.01537 0.97289 2 -1 3 0 5.52469 0.94984 2 -2 -3 0 4183.42 120.15 1 2 -3 0 4225.59 123.804 1 -2 3 0 4167.90 122.845 1 2 3 0 3906.80 118.977 1 -3 -3 0 1603.32 62.4524 1 3 -3 0 1480.34 64.2603 1 3 3 0 1508.50 62.2816 1 -4 -3 0 39.7246 3.00309 2 4 -3 0 33.1068 2.94968 2 -4 -3 0 30.4176 2.64079 4 -4 -3 0 31.5124 2.81641 3 -4 3 0 40.771 3.20288 2 -4 3 0 37.2939 2.8677 3 -4 3 0 29.8786 2.55751 4 4 3 0 41.593 3.04434 2 4 3 0 34.6707 2.6021 4 4 3 0 32.9436 2.78821 3 5 -3 0 1839.33 85.5217 1 5 -3 0 1764.01 78.7022 1 -5 -3 0 1786.50 79.7421 1 5 3 0 1666.45 77.6374 1 -7 -3 0 109.008 6.79444 2 -7 -3 0 127.519 7.16139 3 -7 -3 0 131.094 6.75125 4 7 -3 0 120.707 6.34925 3 7 -3 0 129.452 7.25774 2 -7 3 0 124.036 6.43064 3 7 3 0 131.405 6.91413 3 7 3 0 124.367 7.08057 2 7 3 0 120.295 6.1322 4 -7 3 0 114.313 6.41357 4 -7 3 0 126.51 7.07946 2 -8 -3 0 569.211 19.313 2 -8 -3 0 600.213 19.9063 3 8 -3 0 568.11 17.8827 3 8 -3 0 578.844 19.765 2 -8 -3 0 576.258 18.3173 4 8 3 0 611.885 18.0181 4 -8 3 0 551.774 18.0974 3 8 3 0 570.501 21.2427 2 -8 3 0 590.349 18.2103 4 -9 -3 0 372.503 14.6797 2 9 -3 0 332.82 14.3289 2 -9 -3 0 317.579 13.9047 3 -9 -3 0 341.306 13.1939 4 9 -3 0 330.777 12.8265 3 9 3 0 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2.65959 3 -9 -2 10 663.671 24.0596 4 -9 -2 10 671.692 23.4241 2 -9 -2 10 708.412 23.5159 3 -9 2 10 691.574 22.2581 3 9 2 -10 677.243 21.1035 2 -9 2 10 684.288 23.9133 4 9 2 -10 709.94 23.66 4 -9 2 10 724.448 22.9928 2 8 -2 -10 -2.091 2.31935 4 -8 -2 10 1.9108 2.63188 4 -8 -2 10 2.51108 2.50237 3 -8 -2 10 1.96268 2.39871 2 8 -2 -10 3.04957 1.47733 2 -8 2 10 4.16288 3.41774 2 8 2 -10 0.53411 2.13249 2 8 2 -10 0.58761 2.03198 2 8 2 -10 0.65536 2.42931 4 -8 2 10 3.82207 2.88882 4 -8 2 10 2.41572 2.40176 3 7 -2 -10 388.412 15.5843 4 -7 -2 10 394.016 15.9912 4 -7 2 10 416.736 14.3503 3 7 2 -10 406.22 15.5257 4 7 2 -10 406.02 13.2418 2 -7 2 10 389.124 15.6226 4 7 2 -10 387.577 13.2147 2 -7 2 10 406.286 14.1958 2 -6 -2 10 26.1908 4.03656 2 -6 2 10 25.4346 3.37785 2 6 2 -10 28.7564 3.46016 2 -6 2 10 28.967 4.90378 4 6 2 -10 31.8122 3.67929 2 5 -2 -10 875.872 25.7655 4 -5 -2 10 838.508 24.9637 2 -5 -2 10 838.188 25.8614 4 5 2 -10 868.052 25.492 4 -5 2 10 873.603 25.6962 4 -5 2 10 922.964 23.7466 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10 1.21401 1.18129 4 0 2 10 1.78075 0.78429 2 0 2 -10 1.61806 0.87826 2 0 2 -10 1.80271 0.77797 2 1 -2 10 1908.57 48.6214 2 1 -2 10 1934.12 50.0766 3 -1 2 -10 1990.95 46.2079 2 1 2 10 1958.13 49.7508 3 -1 2 -10 2000.24 46.2727 2 -1 2 -10 1893.52 47.4497 4 2 -2 10 4.4633 2.32884 3 2 -2 10 3.80379 1.8823 2 2 2 10 6.53441 2.44106 3 2 2 10 5.54956 1.41761 2 -2 2 -10 6.74483 1.11051 4 3 -2 10 377.128 13.7124 2 3 -2 10 414.634 14.9975 3 -3 2 -10 417.552 12.173 2 3 2 10 408.063 12.774 2 -3 2 -10 415.026 12.19 2 3 2 10 375.014 14.4136 3 4 -2 10 72.0656 5.80471 2 4 -2 10 75.4391 6.30391 3 4 2 10 66.648 4.98523 2 4 2 10 77.8946 6.33922 3 -4 2 -10 68.2261 4.59002 2 -4 2 -10 76.6064 4.75176 2 5 -2 10 2099.51 55.7166 2 -5 -2 -10 2101.14 56.0143 3 5 -2 10 2137.93 56.4644 3 5 2 10 2231.17 56.8479 3 -5 2 -10 2163.86 53.4832 2 5 2 10 2119.07 54.4766 2 -5 2 -10 2173.47 53.263 2 6 -2 10 1.63138 2.3524 3 6 -2 10 6.51458 2.75591 2 -6 -2 -10 8.77185 3.15449 3 6 2 10 -0.1851 2.0439 2 -6 2 -10 2.72404 2.09632 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10 719.216 23.4946 4 7 3 -10 725.522 23.1901 4 7 3 -10 699.354 21.012 2 -6 -3 10 198.374 9.89509 2 -6 -3 10 186.886 10.1526 4 6 3 -10 194.758 8.40852 2 -6 3 10 191.904 9.9972 4 6 3 -10 207.919 10.0487 4 -6 3 10 194.283 8.26676 2 6 3 -10 200.063 8.35198 2 -5 -3 10 284.661 12.3863 4 -5 -3 10 288.132 11.8552 2 5 3 -10 305.428 10.4296 2 5 3 -10 318.726 10.6507 2 5 3 -10 305.656 12.146 4 -5 3 10 316.418 10.2675 2 -5 3 10 297.565 12.0874 4 -4 -3 10 342.235 13.2534 4 -4 -3 10 335.125 12.5859 2 4 3 -10 350.947 12.7445 4 4 3 -10 343.67 10.9329 2 -4 3 10 345.556 12.6572 4 -4 3 10 334.738 10.3726 2 4 3 -10 364.507 11.3043 2 -3 -3 10 36.337 3.83913 2 -3 -3 10 28.3751 3.62712 4 3 3 -10 28.3054 2.86273 2 3 3 -10 33.082 3.73704 4 3 3 -10 34.0878 2.88993 2 -3 3 10 32.722 2.16576 2 -3 3 10 28.6335 3.50532 4 -2 -3 10 46.9651 3.93009 2 -2 -3 10 52.4096 4.24673 4 -2 -3 10 54.0825 4.37691 2 2 3 -10 54.0398 3.37756 2 -2 3 10 54.1488 2.25609 2 -2 3 10 53.3174 2.20383 2 2 3 -10 46.8864 3.33291 2 -2 3 10 58.1586 4.19806 4 2 3 -10 53.5747 4.21784 4 -1 -3 10 409.075 13.6192 2 -1 -3 10 397.441 13.0782 4 -1 -3 10 406.762 13.3145 2 1 3 -10 408.956 11.8047 2 -1 3 10 403.068 9.84142 2 -1 3 10 403.752 13.259 3 -1 3 10 393.25 12.4217 4 1 3 -10 383.787 12.7018 4 1 3 -10 394.157 11.5442 2 -1 3 10 398.693 9.84447 2 0 3 10 2198.91 56.2903 3 0 3 -10 2220.91 54.0857 2 0 3 -10 2334.06 54.3248 2 0 3 -10 2294.05 54.9985 4 1 -3 10 433.453 15.1302 3 1 -3 10 418.504 14.1579 2 1 3 10 424.589 14.5267 3 -1 3 -10 444.132 12.726 2 1 3 10 413.977 11.8763 4 -1 3 -10 446.376 12.7761 2 1 3 10 435.162 11.6659 2 -1 3 -10 426.132 12.5956 4 2 -3 10 24.8843 3.56763 3 2 -3 10 23.662 3.33379 2 -2 3 -10 26.8722 2.94632 2 2 3 10 24.9877 2.41929 2 2 3 10 20.7758 1.52564 4 -2 3 -10 22.6276 2.77194 2 2 3 10 22.1676 3.42734 3 3 -3 10 1021.95 29.4626 2 3 -3 10 1123.45 33.4551 3 3 3 10 1046.01 27.443 2 -3 3 -10 1032.85 25.5352 4 -3 3 -10 1050.18 27.7115 2 3 3 10 1057.13 30.0085 3 -3 3 -10 1021.55 27.7315 2 4 -3 10 932.098 27.2101 2 4 -3 10 934.431 27.683 3 4 3 10 907.384 25.1512 2 4 3 10 872.634 27.1094 3 -4 3 -10 910.618 25.0726 2 -4 3 -10 905.381 25.1806 2 -5 -3 -10 18.4733 3.78826 3 5 -3 10 2.75831 2.64803 3 5 -3 10 6.37009 2.65187 2 -5 3 -10 7.44209 2.60579 2 5 3 10 4.08983 2.63663 3 5 3 10 6.79438 2.52567 2 -5 3 -10 6.4241 2.3634 2 -6 -3 -10 240.699 11.5446 3 6 -3 10 214.24 11.4268 2 6 -3 10 207.372 11.0928 3 6 3 10 222.639 11.4565 3 -6 3 -10 234.689 10.3635 2 6 3 10 225.392 10.3265 2 -6 3 -10 218.509 9.96457 2 7 -3 10 404.15 16.7691 2 -7 -3 -10 409.116 16.7794 3 7 -3 10 393.678 16.4662 3 7 3 10 406.584 16.918 3 7 3 10 393.439 15.564 2 -8 -3 -10 301.897 14.6205 3 8 -3 10 304.544 15.1484 2 8 -3 10 330.447 14.6752 3 8 3 10 306.688 14.8398 3 8 3 10 290.963 13.5963 2 -10 -4 10 402.501 18.2761 4 -10 -4 10 414.266 23.5942 2 -10 -4 10 439.258 18.0724 3 10 4 -10 408.911 17.4386 4 -10 4 10 398.693 17.5508 4 -10 4 10 438.535 17.0246 2 10 4 -10 430.397 16.171 2 -9 -4 10 62.1268 6.60194 3 -9 -4 10 64.9514 6.78773 2 -9 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412.424 14.8283 2 4 4 -10 399.927 13.2315 2 4 4 -10 412.671 13.0619 2 4 4 -10 420.581 14.5861 4 -4 4 10 412.803 14.3804 4 -4 4 10 417.856 11.8265 2 -3 -4 10 97.1498 6.23439 2 -3 -4 10 95.0968 6.1606 4 -3 4 10 89.8765 5.61469 4 3 4 -10 98.5696 5.33827 2 3 4 -10 101.258 5.20613 2 3 4 -10 88.4299 5.79835 4 -3 4 10 96.9014 3.65461 2 -2 -4 10 1880.95 48.2334 2 -2 -4 10 1861.45 48.3684 4 -2 -4 10 1820.27 48.5254 2 -2 4 10 1943.90 47.6031 4 2 4 -10 1929.34 47.9256 4 2 4 -10 1888.08 46.8235 2 -2 4 10 1953.82 47.403 3 2 4 -10 1863.00 46.5068 2 -1 -4 10 -1.4332 1.37519 2 -1 -4 10 -0.6817 1.4516 2 -1 4 10 -1.3561 1.29027 4 1 4 -10 1.94077 1.45067 2 1 4 -10 2.09097 1.39295 2 1 4 -10 -0.8493 1.4268 4 -1 4 10 0.29874 1.49697 3 0 -4 10 40.6409 4.03261 2 0 4 10 35.3949 1.47815 2 0 4 10 33.662 3.10497 4 0 4 -10 39.1741 3.43126 2 0 4 -10 42.4213 3.47526 2 0 4 -10 35.5768 3.4909 4 0 4 10 44.2669 4.11696 3 1 -4 10 62.9488 5.13307 3 1 -4 10 58.2996 4.88511 2 -1 4 -10 58.2761 4.13287 2 -1 4 -10 62.0291 4.18192 2 1 4 10 57.3372 2.74397 2 1 4 10 57.081 3.30985 4 -1 4 -10 53.1774 3.82044 4 1 4 10 48.6393 4.44449 3 2 -4 10 2661.29 67.6819 3 2 -4 10 2632.79 67.1623 2 2 4 10 2718.90 67.1594 3 -2 4 -10 2673.18 65.5667 2 -2 4 -10 2754.30 64.372 4 -2 4 -10 2726.42 65.5443 2 3 -4 10 2.2889 2.21236 2 3 -4 10 1.06558 1.79256 3 3 4 10 2.37024 1.22285 2 3 4 10 -1.1432 1.85757 3 -3 4 -10 2.14063 1.20032 4 -3 4 -10 2.25443 1.91123 2 -3 4 -10 -0.9901 1.72164 2 4 -4 10 50.5496 5.28484 2 4 -4 10 57.8579 5.85939 3 -4 -4 -10 54.4468 5.36167 3 4 4 10 59.8287 4.3766 2 -4 4 -10 56.7545 2.9803 4 4 4 10 55.9414 5.65508 3 -4 4 -10 43.5402 4.68721 2 -4 4 -10 51.9163 4.907 2 -5 -4 -10 119.809 7.91091 3 5 -4 10 112.707 7.84246 3 5 -4 10 116.115 7.84505 2 -5 4 -10 108.579 3.68448 4 -5 4 -10 114.675 3.8001 4 5 4 10 112.146 7.68227 3 -5 4 -10 117.265 7.01349 2 5 4 10 113.354 6.5712 2 -5 4 -10 109.152 7.01349 2 6 -4 10 1510.69 43.1619 2 -6 -4 -10 1509.65 42.7139 3 6 -4 10 1536.57 43.0674 3 -6 4 -10 1606.95 42.4031 2 6 4 10 1467.28 40.898 2 6 4 10 1496.48 42.8592 3 -6 4 -10 1542.09 41.2995 2 7 -4 10 -0.9375 2.36693 2 -7 -4 -10 -1.5657 2.31181 3 7 -4 10 1.84627 2.52479 3 7 4 10 -2.5562 2.41762 3 7 4 10 -0.1775 2.08298 2 -7 4 -10 1.33367 2.71966 2 -8 -4 -10 206.583 11.9621 3 8 -4 10 221.329 11.8584 3 8 -4 10 206.097 12.1099 2 8 4 10 201.944 10.8901 2 8 4 10 187.094 11.5809 3 -10 -5 10 121.419 9.81644 4 -10 -5 10 146.349 10.5624 2 -10 -5 10 111.95 9.11304 3 10 5 -10 107.954 8.82543 4 10 5 -10 133.558 8.85608 2 -10 5 10 115.755 8.38392 2 10 5 -10 110.01 8.37229 2 -9 -5 10 10.3525 3.55412 4 -9 -5 10 8.38059 3.28562 3 -9 -5 10 6.22476 3.13829 2 -9 5 10 6.34628 2.84766 2 9 5 -10 4.85022 3.05477 2 9 5 -10 3.70996 2.91567 4 9 5 -10 4.00327 2.71819 2 -9 5 10 3.54032 2.97661 4 -8 -5 10 121.612 9.08442 4 -8 -5 10 138.405 10.6374 3 -8 -5 10 130.712 9.02342 2 8 5 -10 129.068 8.03439 2 -8 5 10 124.865 7.49038 2 8 5 -10 128.087 7.84397 2 8 5 -10 130.359 9.97739 4 -8 5 10 117.409 8.44266 4 -8 5 10 128.536 6.87716 3 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5 -10 517.677 16.6668 2 3 5 10 505.979 17.1914 3 -3 5 -10 518.161 16.5402 2 -3 5 -10 512.238 14.7469 4 3 5 10 538.286 15.0354 2 4 -5 10 274.697 12.1418 2 4 -5 10 271.938 11.9969 3 -4 -5 -10 249.835 11.0567 3 -4 5 -10 251.277 8.54224 4 -4 5 -10 246.832 10.5173 2 4 5 10 248.803 9.59167 2 -4 5 -10 269.696 11.1046 2 4 5 10 231.379 11.0723 3 -5 -5 -10 414.02 15.6849 3 5 -5 10 412.078 15.9477 3 5 -5 10 396.083 16.2147 2 -5 5 -10 423.738 11.846 4 -5 5 -10 413.855 14.957 2 5 5 10 386.504 13.9553 2 -5 5 -10 399.824 15.1534 2 5 5 10 388.314 15.5724 3 6 -5 10 43.739 5.64984 3 6 -5 10 55.852 6.3329 2 6 5 10 45.7316 5.03348 2 -6 5 -10 49.6188 5.98078 2 6 5 10 43.4264 5.625 3 7 -5 10 286.969 13.4512 3 7 -5 10 267.41 15.5839 2 -7 -5 -10 275.61 13.441 3 -7 5 -10 285.024 12.6313 2 7 5 10 257.099 13.2014 3 7 5 10 290.536 12.5029 2 -9 -6 10 429.185 24.8489 3 -9 -6 10 485.934 28.1145 2 9 6 -10 430.718 20.2925 4 9 6 -10 430.285 16.7203 2 -9 6 10 399.655 15.9591 2 9 6 -10 403.748 16.014 2 -8 -6 10 3.99063 2.82638 4 -8 -6 10 1.8933 2.61716 2 -8 -6 10 3.00405 2.93938 3 8 6 -10 0.95347 2.38149 2 -8 6 10 -0.5136 1.62596 2 -8 6 10 1.03315 2.53314 4 8 6 -10 5.19672 2.75244 2 8 6 -10 2.94242 2.63716 4 -7 -6 10 82.5574 7.63314 4 -7 -6 10 90.9883 7.86462 2 -7 -6 10 97.0362 7.48277 3 7 6 -10 85.3646 6.58797 2 -7 6 10 89.1272 5.84991 2 7 6 -10 85.3907 6.82562 2 7 6 -10 88.6589 7.20398 4 -7 6 10 72.7272 6.89418 4 -6 -6 10 10.2184 3.34497 2 -6 -6 10 13.9174 3.88843 4 6 6 -10 10.2312 2.97015 2 -6 6 10 7.5152 2.99967 4 -6 6 10 7.4379 2.17444 2 6 6 -10 8.32609 3.05468 4 -6 6 10 12.4018 2.26275 3 6 6 -10 10.3564 2.99751 2 -5 -6 10 1845.31 50.2214 2 -5 -6 10 1876.97 50.5075 4 5 6 -10 1884.05 48.2944 2 -5 6 10 1859.56 45.8007 2 -5 6 10 1821.31 48.9024 4 5 6 -10 1850.09 49.2172 4 5 6 -10 1845.03 47.7935 2 -4 6 10 65.3938 3.72507 2 4 6 -10 67.0671 5.34432 2 4 6 -10 65.6303 5.59662 2 -4 6 10 70.9387 5.69659 4 -4 6 10 72.2927 4.23123 3 -3 -6 10 512.228 18.4542 2 -3 6 10 520.434 13.8982 2 3 6 -10 550.40 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3 1 4 15 1029.85 30.9097 3 2 -4 15 11.7018 3.14867 2 2 4 15 18.8733 4.0824 3 3 -4 15 45.8019 6.00646 3 3 -4 15 51.2269 5.99699 2 3 4 15 46.1943 5.97745 3 -6 -5 15 47.1511 6.30801 4 -6 -5 15 62.7531 6.96201 2 -6 5 15 50.2241 6.12233 4 6 5 -15 38.1902 5.30668 4 -5 -5 15 206.655 11.7653 2 -5 -5 15 230.762 12.0205 4 5 5 -15 229.566 11.4019 4 -5 5 15 193.123 10.8475 4 -4 -5 15 441.393 17.2748 4 -4 -5 15 412.092 16.9955 2 -4 5 15 411.277 15.9593 4 -4 5 15 395.154 15.0766 3 4 5 -15 407.336 15.8617 4 -3 -5 15 26.1194 4.80039 2 3 5 -15 22.8324 3.95035 4 -3 5 15 26.3135 4.23444 3 -3 5 15 26.8667 4.04117 4 -2 -5 15 416.207 16.0972 2 -2 5 15 384.944 15.0543 3 -2 5 15 398.864 14.374 4 2 5 -15 403.833 14.8442 4 -1 -5 15 284.70 13.0685 2 -1 5 15 306.806 13.1599 3 1 5 -15 309.818 11.9606 4 0 -5 15 166.595 10.2712 3 0 -5 15 153.837 9.2645 2 0 5 15 178.821 9.95193 3 1 -5 15 6.66167 3.63875 3 1 5 15 3.19107 2.71713 3 2 -5 15 366.497 16.4402 3 2 -5 15 368.286 15.4689 2 2 5 15 376.384 15.8714 3 3 -5 15 293.166 14.4666 3 3 -5 15 271.314 13.3061 2 3 5 15 300.649 14.1386 3 -5 -6 15 3.18153 2.92467 2 -5 -6 15 3.95885 2.79065 4 -5 6 15 5.73596 3.24799 4 5 6 -15 6.04656 3.30313 4 -4 -6 15 360.461 16.3346 2 -4 6 15 389.943 15.2756 4 3 6 -15 4.47703 2.72166 4 -3 6 15 3.32195 2.41334 4 2 6 -15 230.85 10.5545 4 -2 6 15 196.873 10.1031 4 -2 6 15 213.419 10.3596 3 -1 6 15 0.61102 2.49238 3 1 6 -15 2.59138 2.33161 4 0 -6 15 639.276 22.1838 2 0 6 15 620.302 21.2857 3 1 -6 15 -0.5169 2.86374 3 1 -6 15 6.41308 2.7666 2 1 6 15 4.87962 3.03368 3 2 -6 15 183.465 11.1392 2 2 -6 15 218.173 12.0603 3 2 6 15 199.649 11.1231 3 -4 -7 15 344.404 16.3009 2 4 7 -15 319.716 14.3637 4 -4 7 15 324.504 14.017 4 -3 7 15 12.0519 3.38699 4 3 7 -15 19.6891 6.57676 4 2 7 -15 55.3874 5.86794 4 -1 -7 15 560.281 20.3585 2 1 7 -15 493.027 19.2522 4 0 -7 15 -2.634 2.10159 2 0 -7 15 3.89398 2.57659 3 1 -7 15 5.84047 3.33748 3 1 7 15 2.31835 2.99712 3 -6 0 16 302.288 13.9319 4 6 0 -16 260.785 13.0136 4 5 0 -16 -4.4731 2.02064 4 -5 0 16 -1.783 2.42482 4 4 0 -16 527.425 18.6638 4 -4 0 16 531.799 18.9265 4 3 0 -16 2.10359 2.59773 4 -2 0 16 16.2125 3.8234 3 -2 0 16 16.7436 3.08168 4 -1 0 16 3.31438 3.01746 3 0 0 16 841.359 27.7226 3 1 0 16 -1.4389 2.81722 3 2 0 16 0.27289 3.65797 3 -6 -1 16 219.822 12.1443 4 -6 -1 16 209.71 11.5275 2 -6 1 16 232.85 12.0676 4 6 1 -16 221.538 11.6465 4 -5 -1 16 121.511 7.68419 2 -5 -1 16 127.183 8.8525 4 5 1 -16 102.098 7.77011 4 -5 1 16 115.612 8.40174 4 -4 -1 16 5.97417 2.94148 4 4 1 -16 11.3778 3.15195 4 -4 1 16 9.92967 3.18622 4 -3 -1 16 145.157 8.61114 4 -3 -1 16 140.92 8.05224 2 -3 1 16 154.883 9.51646 3 -3 1 16 146.269 8.62879 4 3 1 -16 150.943 8.35505 4 -2 -1 16 524.999 17.8133 4 -2 -1 16 532.852 19.8464 3 -2 -1 16 528.539 17.4371 2 -2 1 16 545.843 19.7218 3 -2 1 16 526.008 18.8703 4 -1 -1 16 433.665 15.2358 2 -1 -1 16 443.218 17.7583 3 -1 1 16 453.914 17.633 3 0 -1 16 45.6076 6.08701 3 0 -1 16 37.1811 4.95933 2 0 1 16 45.3376 5.94872 3 1 -1 16 152.357 9.9194 3 1 -1 16 133.23 9.13267 2 1 1 16 138.167 9.58344 3 2 -1 16 363.874 16.4919 3 -6 -2 16 2.37067 2.37041 2 -6 -2 16 1.7873 2.66881 4 -6 2 16 0.2386 2.71133 4 6 2 -16 2.98258 2.73722 4 -5 -2 16 205.992 11.2906 4 -5 -2 16 194.434 10.3567 2 5 2 -16 192.146 11.6785 4 -5 2 16 191.601 10.5397 4 -4 -2 16 -0.1374 2.38458 4 -4 -2 16 -0.338 2.04899 2 -4 2 16 -0.229 2.16285 4 4 2 -16 -3.5777 2.11836 4 -3 -2 16 716.034 23.2117 2 -3 -2 16 725.47 23.3083 4 3 2 -16 720.004 22.6849 4 -3 2 16 715.43 23.9822 3 -3 2 16 749.555 23.0321 4 -2 -2 16 1.82947 2.24554 4 -2 -2 16 1.46178 2.00135 2 -2 -2 16 6.27652 3.07759 3 -2 2 16 0.61572 2.63815 3 2 2 -16 3.90121 2.31875 4 -1 -2 16 573.902 18.9985 2 -1 -2 16 567.352 21.1385 3 -1 2 16 582.404 20.8257 3 0 -2 16 43.1601 4.95921 2 0 -2 16 37.3471 5.47896 3 0 2 16 38.1083 5.28643 3 1 -2 16 338.062 13.6525 2 1 2 16 362.256 15.9348 3 2 -2 16 -0.2228 1.93949 2 2 -2 16 -2.0696 2.5726 3 2 2 16 0.23951 4.4718 3 -6 -3 16 309.184 14.2915 2 -6 -3 16 310.48 14.8715 4 6 3 -16 315.913 14.2769 4 -6 3 16 319.428 14.5248 4 -5 -3 16 274.041 13.4192 4 -5 -3 16 271.27 12.9793 2 5 3 -16 279.421 14.4746 4 -5 3 16 269.456 12.7331 4 -4 -3 16 24.9073 4.18161 2 -4 -3 16 28.636 4.76065 4 -4 3 16 33.6351 4.67048 3 4 3 -16 31.0508 4.53786 4 -4 3 16 24.213 4.09285 4 -3 -3 16 279.586 12.4085 2 -3 3 16 235.053 11.7928 3 -3 3 16 240.097 11.0427 4 3 3 -16 239.747 11.1428 4 -2 -3 16 415.415 15.8797 2 -2 3 16 456.721 17.2188 3 -1 -3 16 211.651 10.3122 2 -1 -3 16 210.061 11.699 3 -1 3 16 215.76 11.1897 3 0 -3 16 -2.0946 3.34195 3 0 -3 16 -0.8484 1.92332 2 0 3 16 -3.0776 2.20751 3 1 -3 16 219.649 12.3136 3 1 -3 16 213.317 10.6407 2 1 3 16 214.315 11.8283 3 2 -3 16 302.792 14.9399 3 2 3 16 295.797 20.7481 3 -5 -4 16 -1.5088 2.54918 4 -5 -4 16 -0.6359 2.65793 2 -5 4 16 -3.3164 2.23819 4 -5 4 16 3.76028 2.73478 3 5 4 -16 -1.9057 2.45163 4 -4 -4 16 835.092 26.5511 4 -4 -4 16 804.582 26.4029 2 -4 4 16 781.533 25.1457 3 4 4 -16 763.835 25.0229 4 -4 4 16 787.342 25.1862 4 -3 -4 16 5.77106 3.11037 2 -3 4 16 8.44785 2.87275 3 -3 4 16 3.87207 2.54281 4 3 4 -16 7.82708 2.91927 4 -2 -4 16 9.58987 3.00085 2 2 4 -16 9.67348 2.91214 4 -2 4 16 5.41783 2.76007 3 -1 -4 16 76.6725 6.64067 2 -1 4 16 93.5025 7.58151 3 0 -4 16 528.244 18.689 2 0 -4 16 504.449 20.3497 3 0 4 16 485.356 19.0248 3 1 4 16 2.75072 2.6643 3 -4 -5 16 0.62698 2.61463 2 -4 5 16 6.06507 2.91204 4 -3 5 16 86.9068 7.05429 3 3 5 -16 115.356 7.69269 4 2 5 -16 322.636 18.0617 4 -2 5 16 313.331 13.5441 3 -1 -5 16 295.503 18.176 2 -1 -5 16 238.902 12.8632 3 -1 5 16 237.932 11.819 3 0 -5 16 0.76522 2.23072 2 0 -5 16 -2.3087 1.8911 3 0 5 16 0.70793 2.40092 3 1 -5 16 169.924 10.0235 2 1 -5 16 171.867 10.8067 3 1 5 16 171.243 10.295 3 3 6 -16 705.646 24.5754 4 -1 -6 16 258.575 13.2962 3 -1 -6 16 248.719 12.4093 2 5 0 -17 511.994 19.4864 4 -5 0 17 525.73 19.6911 4 -4 0 17 -0.3451 2.14192 4 -3 0 17 19.7794 4.1416 3 -2 0 17 2.37108 2.83063 3 -1 0 17 742.423 28.327 3 0 0 17 2.17263 3.02565 3 -4 -1 17 83.1611 7.08795 4 -4 1 17 90.238 7.23135 4 4 1 -17 87.7317 6.98747 4 -3 1 17 337.195 14.9443 3 -2 1 17 281.02 13.4875 3 -1 -1 17 0.36054 3.19544 3 -1 1 17 1.00551 2.48092 3 0 -1 17 343.082 15.7657 3 -4 2 17 309.945 14.061 3 4 2 -17 314.317 13.5182 4 -3 2 17 43.7206 5.61881 3 -2 -2 17 328.612 15.5615 3 -2 2 17 333.466 14.8445 3 -1 -2 17 5.25128 3.09048 3 -1 2 17 1.81219 2.66559 3 0 -2 17 274.912 13.9548 3 0 2 17 278.237 15.8068 3 -3 3 17 526.241 19.5468 3 -2 -3 17 302.326 14.5439 3 -2 -3 17 284.517 13.7653 2 -2 3 17 280.472 13.4923 3 -1 -3 17 9.78185 3.45625 3 -1 -3 17 9.79134 4.64161 2 -1 3 17 10.8569 3.59419 3 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 70142 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.08737(18) 0.30390(13) 0.45313(12) 0.0259(3) Uani 1 1 d . . . . . H1 H 0.078429 0.2574 0.395366 0.031 Uiso 1 1 calc R U . . . C2 C -0.02108(17) 0.29992(13) 0.50967(11) 0.0243(3) Uani 1 1 d . . . . . H2 H -0.103498 0.252496 0.490028 0.029 Uiso 1 1 calc R U . . . C3 C -0.01071(16) 0.36647(12) 0.59756(11) 0.0212(3) Uani 1 1 d . . . . . C4 C 0.11609(16) 0.43479(14) 0.61984(11) 0.0239(3) Uani 1 1 d . . . . . H4 H 0.130794 0.480802 0.678067 0.029 Uiso 1 1 calc R U . . . C5 C 0.21702(17) 0.43449(14) 0.55771(12) 0.0254(3) Uani 1 1 d . . . . . H5 H 0.299704 0.482413 0.573758 0.031 Uiso 1 1 calc R U . . . C6 C -0.09251(18) 0.42857(16) 0.75006(12) 0.0296(3) Uani 1 1 d . . . . . H6A H -0.004911 0.40073 0.79447 0.044 Uiso 1 1 calc R U . . . H6B H -0.178035 0.418582 0.782532 0.044 Uiso 1 1 calc R U . . . H6C H -0.080253 0.508536 0.736306 0.044 Uiso 1 1 calc R U . . . C7 C -0.24603(18) 0.29839(16) 0.62845(14) 0.0332(4) Uani 1 1 d . . . . . H7A H -0.292135 0.315897 0.559412 0.05 Uiso 1 1 calc R U . . . H7B H -0.314349 0.315568 0.673914 0.05 Uiso 1 1 calc R U . . . H7C H -0.220474 0.21843 0.633565 0.05 Uiso 1 1 calc R U . . . C8 C 0.54086(17) 0.46908(14) 0.20183(12) 0.0255(3) Uani 1 1 d . . . . . C9 C 0.66493(16) 0.31655(13) 0.27861(12) 0.0241(3) Uani 1 1 d . . . . . C10 C 0.73895(17) 0.35109(13) 0.19373(12) 0.0239(3) Uani 1 1 d . . . . . C11 C 0.66268(17) 0.44261(13) 0.14638(12) 0.0237(3) Uani 1 1 d . . . . . C12 C 0.70221(18) 0.49231(15) 0.06321(13) 0.0286(3) Uani 1 1 d . . . . . H12 H 0.649699 0.554626 0.031015 0.034 Uiso 1 1 calc R U . . . C13 C 0.82255(19) 0.44725(16) 0.02832(13) 0.0326(4) Uani 1 1 d . . . . . H13 H 0.851764 0.47876 -0.02951 0.039 Uiso 1 1 calc R U . . . C14 C 0.90083(19) 0.35698(16) 0.07650(15) 0.0334(4) Uani 1 1 d . . . . . H14 H 0.983643 0.329092 0.051853 0.04 Uiso 1 1 calc R U . . . C15 C 0.85949(17) 0.30682(14) 0.16044(13) 0.0288(3) Uani 1 1 d . . . . . H15 H 0.912027 0.24488 0.19329 0.035 Uiso 1 1 calc R U . . . I1 I 0.38572(2) 0.37811(2) 0.37552(2) 0.02353(4) Uani 1 1 d . . . . . N1 N 0.20608(15) 0.37035(11) 0.47522(10) 0.0243(3) Uani 1 1 d . . . . . N2 N -0.11389(15) 0.36572(12) 0.65592(11) 0.0261(3) Uani 1 1 d . . . . . N3 N 0.54817(15) 0.38980(11) 0.27799(10) 0.0248(3) Uani 1 1 d . . . . . O1 O 0.45205(14) 0.54506(11) 0.18515(10) 0.0354(3) Uani 1 1 d . . . . . O2 O 0.69845(13) 0.24030(10) 0.33769(9) 0.0312(3) 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 0.0334(8) 0.0218(7) 0.0204(7) -0.0027(6) -0.0008(6) -0.0017(6) C2 0.0275(7) 0.0208(7) 0.0217(7) 0.0001(6) -0.0031(6) -0.0047(6) C3 0.0222(7) 0.0186(7) 0.0210(7) 0.0025(5) -0.0008(5) 0.0005(5) C4 0.0255(7) 0.0211(7) 0.0236(8) -0.0055(6) 0.0004(6) -0.0026(6) C5 0.0255(7) 0.0235(8) 0.0263(8) -0.0030(6) 0.0016(6) -0.0037(6) C6 0.0293(8) 0.0339(9) 0.0256(8) -0.0027(7) 0.0049(6) 0.0036(7) C7 0.0265(8) 0.0396(10) 0.0326(9) 0.0033(7) 0.0027(7) -0.0081(7) C8 0.0254(7) 0.0260(8) 0.0249(8) -0.0005(6) 0.0034(6) -0.0008(6) C9 0.0225(7) 0.0221(7) 0.0255(8) -0.0047(6) -0.0021(6) -0.0031(6) C10 0.0233(7) 0.0220(7) 0.0246(8) -0.0064(6) -0.0009(6) -0.0038(6) C11 0.0232(7) 0.0220(7) 0.0248(8) -0.0048(6) 0.0017(6) -0.0020(6) C12 0.0323(8) 0.0261(8) 0.0274(8) -0.0009(6) 0.0057(6) -0.0035(6) C13 0.0351(9) 0.0348(9) 0.0298(9) -0.0070(7) 0.0114(7) -0.0086(7) C14 0.0270(8) 0.0345(9) 0.0403(10) -0.0135(8) 0.0103(7) -0.0032(7) C15 0.0236(7) 0.0260(8) 0.0352(9) -0.0087(7) 0.0007(6) -0.0002(6) I1 0.02559(6) 0.02395(6) 0.02040(6) 0.00013(4) 0.00229(4) 0.00040(4) N1 0.0269(6) 0.0234(7) 0.0221(6) -0.0005(5) 0.0034(5) 0.0001(5) N2 0.0242(6) 0.0279(7) 0.0255(7) -0.0014(5) 0.0026(5) -0.0034(5) N3 0.0246(6) 0.0258(7) 0.0236(7) 0.0017(5) 0.0034(5) 0.0008(5) O1 0.0351(6) 0.0343(7) 0.0384(7) 0.0107(5) 0.0112(5) 0.0132(5) O2 0.0302(6) 0.0288(6) 0.0314(6) 0.0056(5) -0.0035(5) 0.0008(5) 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 123.34(15) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 120.15(14) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? N2 C3 C4 121.91(14) . . ? N2 C3 C2 122.64(14) . . ? C4 C3 C2 115.45(14) . . ? C5 C4 C3 120.06(14) . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? N1 C5 C4 123.73(14) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 N3 125.76(15) . . ? O1 C8 C11 127.55(15) . . ? N3 C8 C11 106.68(13) . . ? O2 C9 N3 125.59(15) . . ? O2 C9 C10 127.79(15) . . ? N3 C9 C10 106.62(13) . . ? C15 C10 C11 121.53(16) . . ? C15 C10 C9 130.79(16) . . ? C11 C10 C9 107.68(14) . . ? C12 C11 C10 121.69(15) . . ? C12 C11 C8 130.79(15) . . ? C10 C11 C8 107.52(14) . . ? C11 C12 C13 117.16(16) . . ? C11 C12 H12 121.4 . . ? C13 C12 H12 121.4 . . ? C14 C13 C12 121.37(17) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 121.04(16) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C10 C15 C14 117.20(16) . . ? C10 C15 H15 121.4 . . ? C14 C15 H15 121.4 . . ? N3 I1 N1 177.68(5) . . ? C5 N1 C1 117.26(14) . . ? C5 N1 I1 120.28(10) . . ? C1 N1 I1 122.45(11) . . ? C3 N2 C7 120.52(14) . . ? C3 N2 C6 120.54(13) . . ? C7 N2 C6 118.88(14) . . ? C9 N3 C8 111.47(13) . . ? C9 N3 I1 125.37(11) . . ? C8 N3 I1 123.03(10) . . ? 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 1.346(2) . ? C1 C2 1.369(2) . ? C1 H1 0.95 . ? C2 C3 1.419(2) . ? C2 H2 0.95 . ? C3 N2 1.345(2) . ? C3 C4 1.418(2) . ? C4 C5 1.365(2) . ? C4 H4 0.95 . ? C5 N1 1.342(2) . ? C5 H5 0.95 . ? C6 N2 1.461(2) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 N2 1.457(2) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 O1 1.217(2) . ? C8 N3 1.391(2) . ? C8 C11 1.497(2) . ? C9 O2 1.214(2) . ? C9 N3 1.389(2) . ? C9 C10 1.497(2) . ? C10 C15 1.382(2) . ? C10 C11 1.392(2) . ? C11 C12 1.378(2) . ? C12 C13 1.394(2) . ? C12 H12 0.95 . ? C13 C14 1.393(3) . ? C13 H13 0.95 . ? C14 C15 1.396(3) . ? C14 H14 0.95 . ? C15 H15 0.95 . ? I1 N3 2.1769(14) . ? I1 N1 2.3247(14) . ? 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 -1.1(2) . . . . ? C1 C2 C3 N2 -179.90(15) . . . . ? C1 C2 C3 C4 0.4(2) . . . . ? N2 C3 C4 C5 -178.89(15) . . . . ? C2 C3 C4 C5 0.8(2) . . . . ? C3 C4 C5 N1 -1.4(3) . . . . ? O2 C9 C10 C15 0.7(3) . . . . ? N3 C9 C10 C15 -179.66(16) . . . . ? O2 C9 C10 C11 -179.97(15) . . . . ? N3 C9 C10 C11 -0.29(17) . . . . ? C15 C10 C11 C12 1.0(2) . . . . ? C9 C10 C11 C12 -178.40(14) . . . . ? C15 C10 C11 C8 -179.41(14) . . . . ? C9 C10 C11 C8 1.15(16) . . . . ? O1 C8 C11 C12 -2.5(3) . . . . ? N3 C8 C11 C12 177.87(16) . . . . ? O1 C8 C11 C10 178.00(17) . . . . ? N3 C8 C11 C10 -1.62(17) . . . . ? C10 C11 C12 C13 -0.2(2) . . . . ? C8 C11 C12 C13 -179.61(16) . . . . ? C11 C12 C13 C14 -1.0(2) . . . . ? C12 C13 C14 C15 1.4(3) . . . . ? C11 C10 C15 C14 -0.7(2) . . . . ? C9 C10 C15 C14 178.61(15) . . . . ? C13 C14 C15 C10 -0.5(2) . . . . ? C4 C5 N1 C1 0.7(2) . . . . ? C4 C5 N1 I1 179.89(12) . . . . ? C2 C1 N1 C5 0.6(2) . . . . ? C2 C1 N1 I1 -178.56(12) . . . . ? C4 C3 N2 C7 177.22(15) . . . . ? C2 C3 N2 C7 -2.5(2) . . . . ? C4 C3 N2 C6 -5.4(2) . . . . ? C2 C3 N2 C6 174.90(15) . . . . ? O2 C9 N3 C8 178.91(15) . . . . ? C10 C9 N3 C8 -0.78(17) . . . . ? O2 C9 N3 I1 -5.1(2) . . . . ? C10 C9 N3 I1 175.20(10) . . . . ? O1 C8 N3 C9 -178.16(16) . . . . ? C11 C8 N3 C9 1.48(17) . . . . ? O1 C8 N3 I1 5.7(2) . . . . ? C11 C8 N3 I1 -174.62(10) . . . . ?