#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:38:48 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242524 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132569.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_4132569 loop_ _publ_author_name 'Yuan, Shuai' 'Zhang, Peng' 'Zhang, Liangliang' 'Garcia-Esparza, Angel T' 'Sokaras, Dimosthenis' 'Qin, Jun-Sheng' 'Feng, Liang' 'Day, Gregory S.' 'Chen, Wenmiao' 'Drake, Hannah F.' 'Elumalai, Palani' 'Madrahimov, Sherzod T.' 'Sun, Daofeng' 'Zhou, Hong-Cai' _publ_section_title ; Exposed Equatorial Positions of Metal Centers via Sequential Ligand Elimination and Installation in MOFs. ; _journal_issue 34 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 10814 _journal_page_last 10819 _journal_paper_doi 10.1021/jacs.8b04886 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety 'C16 H22 Cl2 Cu N2 O6 S2, 2(C2 H6 O S)' _chemical_formula_sum 'C20 H34 Cl2 Cu N2 O8 S4' _chemical_formula_weight 693.17 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-05-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492) ; _cell_angle_alpha 71.8866(9) _cell_angle_beta 83.9415(10) _cell_angle_gamma 76.9365(10) _cell_formula_units_Z 1 _cell_length_a 7.0833(3) _cell_length_b 10.3708(5) _cell_length_c 10.9549(5) _cell_measurement_reflns_used 9898 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 78.747 _cell_measurement_theta_min 4.249 _cell_volume 744.53(6) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 99.99 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.907 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_unetI/netI 0.0252 _diffrn_reflns_Laue_measured_fraction_full 0.907 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 11845 _diffrn_reflns_point_group_measured_fraction_full 0.907 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 74.744 _diffrn_reflns_theta_min 4.249 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 5.699 _exptl_absorpt_correction_T_max 0.7538 _exptl_absorpt_correction_T_min 0.4581 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour blue _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.546 _exptl_crystal_description needle _exptl_crystal_F_000 359 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.454 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 174 _refine_ls_number_reflns 2989 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.081 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0267 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.5316P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.0780 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2901 _reflns_number_total 2989 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04886_si_002.cif _cod_data_source_block CuINA2 _cod_database_code 4132569 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C11(H11), C20(H20) 2.b Idealised Me refined as rotating group: C1AA(H1Aa,H1Ab,H1Ac), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C5(H5a,H5b,H5c) 2.c Idealised tetrahedral OH refined as rotating group: O10(H10) ; _shelx_res_file ; CuINA2.res created by SHELXL-2014/7 TITL CuINA2 in P-1 #2 REM reset to P-1 #2 CELL 1.54184 7.0833 10.3708 10.9549 71.8866 83.9415 76.9365 ZERR 1 0.0003 0.0005 0.0005 0.0009 0.001 0.001 LATT 1 SFAC C H Cl Cu N O S UNIT 20 34 2 1 2 8 4 L.S. 90 PLAN 20 TEMP -173.16 BOND MORE -1 BOND $H CONF fmap 2 acta 52 REM REM REM WGHT 0.041800 0.531600 FVAR 1.16279 CU1 4 1.000000 0.000000 0.000000 10.50000 0.01558 0.01047 = 0.00886 0.00018 -0.00369 -0.00189 CL2 3 0.893470 -0.187823 -0.027381 11.00000 0.01916 0.01301 = 0.01282 -0.00240 -0.00162 -0.00380 S3 7 1.323435 -0.139195 -0.215571 11.00000 0.02085 0.01385 = 0.01345 -0.00351 -0.00112 -0.00172 S4 7 0.964005 0.508688 -0.271970 11.00000 0.02050 0.01856 = 0.01289 -0.00542 -0.00033 -0.00550 O2 6 1.258452 -0.020668 -0.158746 11.00000 0.02070 0.01605 = 0.01174 -0.00454 0.00037 -0.00250 O0AA 6 0.523368 0.377328 -0.567927 11.00000 0.02113 0.02140 = 0.00931 -0.00086 0.00016 -0.00435 C7 1 0.505224 0.212152 -0.222596 11.00000 0.01697 0.01446 = 0.01093 -0.00278 0.00057 -0.00328 AFIX 43 H7 2 0.368975 0.221140 -0.207585 11.00000 -1.20000 AFIX 0 C8 1 0.781521 0.260327 -0.361143 11.00000 0.01607 0.01380 = 0.00994 -0.00203 -0.00094 -0.00361 AFIX 43 H8 2 0.837503 0.301802 -0.442613 11.00000 -1.20000 AFIX 0 O10 6 0.275721 0.321746 -0.431544 11.00000 0.01567 0.04635 = 0.00955 0.00104 -0.00341 -0.00586 AFIX 147 H10 2 0.214806 0.346955 -0.499569 11.00000 -1.50000 AFIX 0 C11 1 0.630880 0.141977 -0.123777 11.00000 0.01767 0.01388 = 0.00904 -0.00101 -0.00005 -0.00452 AFIX 43 H11 2 0.578110 0.101807 -0.040816 11.00000 -1.20000 AFIX 0 C13 1 0.583146 0.269450 -0.344846 11.00000 0.01686 0.01083 = 0.00966 -0.00148 -0.00231 -0.00160 C16 1 0.458135 0.330683 -0.459999 11.00000 0.01719 0.01281 = 0.01131 -0.00247 -0.00134 0.00062 C20 1 0.897673 0.189662 -0.256688 11.00000 0.01233 0.01386 = 0.01243 -0.00192 -0.00174 -0.00266 AFIX 43 H20 2 1.033735 0.184480 -0.267865 11.00000 -1.20000 AFIX 0 N28 5 0.824003 0.128212 -0.140059 11.00000 0.01575 0.01124 = 0.01005 -0.00209 -0.00282 -0.00272 O1 6 0.917162 0.647451 -0.376356 11.00000 0.02100 0.02967 = 0.01176 0.00174 -0.00462 -0.00738 C1AA 1 1.148769 0.527692 -0.184782 11.00000 0.02128 0.01943 = 0.01656 0.00039 -0.00556 -0.00573 AFIX 137 H1AA 2 1.263759 0.541544 -0.241472 11.00000 -1.50000 H1AB 2 1.182538 0.444004 -0.112159 11.00000 -1.50000 H1AC 2 1.101845 0.608001 -0.152659 11.00000 -1.50000 AFIX 0 C3 1 1.171718 -0.102783 -0.347740 11.00000 0.02551 0.02809 = 0.01949 -0.01203 -0.00339 -0.00412 AFIX 137 H3A 2 1.038942 -0.109815 -0.315316 11.00000 -1.50000 H3B 2 1.220656 -0.169737 -0.395860 11.00000 -1.50000 H3C 2 1.172425 -0.008844 -0.404466 11.00000 -1.50000 AFIX 0 C4 1 0.768631 0.511145 -0.154966 11.00000 0.02351 0.03017 = 0.01375 -0.00020 0.00247 -0.00556 AFIX 137 H4A 2 0.754538 0.593255 -0.125865 11.00000 -1.50000 H4B 2 0.795901 0.427465 -0.081542 11.00000 -1.50000 H4C 2 0.648230 0.514062 -0.193279 11.00000 -1.50000 AFIX 0 C5 1 1.543049 -0.107033 -0.305688 11.00000 0.02416 0.02535 = 0.02266 -0.01106 0.00427 -0.00273 AFIX 137 H5A 2 1.518570 -0.013992 -0.367254 11.00000 -1.50000 H5B 2 1.588308 -0.175922 -0.352151 11.00000 -1.50000 H5C 2 1.642366 -0.113597 -0.246941 11.00000 -1.50000 AFIX 0 HKLF 4 REM CuINA2 in P-1 #2 REM R1 = 0.0267 for 2901 Fo > 4sig(Fo) and 0.0277 for all 2989 data REM 174 parameters refined using 0 restraints END WGHT 0.0418 0.5316 REM Highest difference peak 0.454, deepest hole -0.528, 1-sigma level 0.072 Q1 1 1.2607 -0.0743 -0.1838 11.00000 0.05 0.45 Q2 1 1.0607 -0.0753 -0.0406 11.00000 0.05 0.45 Q3 1 1.0029 0.4394 -0.3039 11.00000 0.05 0.43 Q4 1 0.9425 -0.2652 -0.0658 11.00000 0.05 0.33 Q5 1 1.0587 0.5223 -0.2216 11.00000 0.05 0.31 Q6 1 0.6655 0.2762 -0.3603 11.00000 0.05 0.30 Q7 1 0.8598 0.5149 -0.2192 11.00000 0.05 0.29 Q8 1 0.5168 0.2953 -0.3926 11.00000 0.05 0.29 Q9 1 1.4439 -0.1268 -0.2597 11.00000 0.05 0.27 Q10 1 0.8373 -0.1211 0.0171 11.00000 0.05 0.26 Q11 1 0.8786 0.0956 -0.1051 11.00000 0.05 0.25 Q12 1 0.9265 -0.1401 0.0173 11.00000 0.05 0.25 Q13 1 0.8546 0.1608 -0.1928 11.00000 0.05 0.24 Q14 1 1.0329 -0.2162 -0.0354 11.00000 0.05 0.24 Q15 1 0.8364 0.2379 -0.3062 11.00000 0.05 0.23 Q16 1 0.7247 0.1131 -0.1527 11.00000 0.05 0.23 Q17 1 0.5597 0.2393 -0.2966 11.00000 0.05 0.22 Q18 1 1.1570 0.0196 0.0197 11.00000 0.05 0.22 Q19 1 0.5359 0.3180 -0.5933 11.00000 0.05 0.22 Q20 1 1.0678 0.5831 -0.1404 11.00000 0.05 0.22 ; _shelx_res_checksum 23736 _shelx_hkl_file ; -2 0 0 853.051 35.7522 4 -3 0 0 13.4554 1.18992 4 -3 0 0 17.4206 2.14156 7 -3 0 0 13.1201 1.28519 4 -4 0 0 556.628 24.6018 7 4 0 0 548.821 24.4339 11 4 0 0 538.543 24.1018 2 5 0 0 190.197 10.4187 11 5 0 0 183.941 9.53980 1 5 0 0 181.916 9.28237 2 6 0 0 193.586 9.98283 11 6 0 0 174.120 9.41679 1 6 0 0 185.352 9.41408 2 7 0 0 27.7321 4.43204 2 7 0 0 34.9035 4.07658 11 8 0 0 54.5205 4.29510 11 8 0 0 53.3027 3.73408 2 8 -1 0 19.9102 2.41549 2 7 -1 0 75.7172 4.96046 2 7 -1 0 77.9128 5.76041 11 6 -1 0 9.37017 2.46218 11 6 -1 0 7.39805 1.75300 2 5 -1 0 354.495 17.3648 1 5 -1 0 383.470 17.5722 11 5 -1 0 392.985 17.3424 2 4 -1 0 93.1337 5.77895 11 4 -1 0 85.6984 5.13815 2 -4 1 0 77.4462 7.27480 7 -4 1 0 76.6785 4.93349 4 -4 1 0 83.1395 4.42177 4 -3 1 0 1414.51 59.3897 4 2 -1 0 350.914 14.6698 4 2 -1 0 327.168 14.6335 4 -2 1 0 372.425 14.6647 4 -2 1 0 329.212 14.6931 4 1 -1 0 1117.85 48.2625 4 -1 1 0 1222.53 48.2702 4 -1 1 0 1118.38 48.3013 4 0 -1 0 964.226 40.1946 4 0 -1 0 976.442 40.2336 4 0 1 0 941.127 40.2254 7 -1 -1 0 315.253 13.3862 4 -1 -1 0 326.110 13.4335 4 -1 -1 0 326.349 13.5262 7 1 1 0 319.440 13.5329 7 1 1 0 303.740 13.3995 4 1 1 0 316.265 13.3743 4 -2 -1 0 2400.05 101.669 4 -2 -1 0 2443.46 101.954 7 -2 -1 0 2454.08 101.645 4 -3 -1 0 2.09265 1.07362 7 -3 -1 0 2.56594 0.64468 4 -4 -1 0 742.044 31.4779 7 4 1 0 692.755 31.4697 11 5 1 0 213.070 12.1984 9 5 1 0 230.811 11.1341 1 5 1 0 228.160 11.4777 11 5 1 0 233.874 11.0030 2 6 1 0 997.028 43.1308 2 6 1 0 976.470 42.9988 1 6 1 0 1020.11 43.7164 11 7 1 0 956.419 40.9193 11 7 1 0 962.481 40.4116 2 7 1 0 881.575 41.5789 1 8 1 0 100.208 5.58134 2 8 1 0 99.6993 5.99555 11 8 -2 0 1.44267 1.17909 2 7 -2 0 7.41370 2.47423 11 7 -2 0 6.21684 1.63683 2 6 -2 0 160.318 8.50153 2 6 -2 0 165.896 9.11747 11 5 -2 0 2298.44 94.8762 2 5 -2 0 2172.68 94.8563 11 4 -2 0 568.384 26.2297 5 4 -2 0 538.384 23.9911 2 4 -2 0 565.241 24.3273 11 4 -2 0 499.541 23.4537 3 -4 2 0 547.893 23.5592 4 -3 2 0 3147.53 132.806 4 -3 2 0 3187.42 132.729 4 2 -2 0 941.086 41.2994 4 2 -2 0 1014.18 41.3547 4 -2 2 0 1000.50 41.2592 4 -2 2 0 961.373 41.3460 4 1 -2 0 13.7316 1.32850 4 -1 2 0 16.2265 1.31749 4 -1 2 0 16.6910 1.14341 4 0 -2 0 178.888 7.73771 4 0 2 0 176.393 7.83616 7 0 2 0 182.320 7.73692 4 0 2 0 176.341 7.80273 4 -2 -2 0 11.5974 1.19474 4 -2 -2 0 13.4460 1.06745 4 -2 -2 0 10.8857 1.41133 7 2 2 0 12.3676 1.21005 4 2 2 0 13.5217 1.62703 7 2 2 0 13.0703 1.05455 4 -3 -2 0 438.659 19.4444 7 -3 -2 0 440.478 18.7547 4 -4 -2 0 5399.81 214.392 7 4 2 0 4945.18 214.017 1 4 2 0 4967.38 214.419 11 5 2 0 940.577 43.5219 2 5 2 0 1009.92 42.9043 11 5 2 0 994.945 42.3922 1 6 2 0 1015.34 44.2204 11 6 2 0 994.420 43.6160 9 6 2 0 1016.94 43.5828 1 6 2 0 1008.14 43.4855 2 7 2 0 967.638 41.2412 11 7 2 0 914.224 41.1161 2 7 2 0 929.418 40.4309 1 7 -3 0 111.429 5.97481 2 7 -3 0 113.429 6.81514 11 6 -3 0 14.1037 2.95655 11 6 -3 0 10.3594 2.05476 2 5 -3 0 1300.34 56.5186 11 5 -3 0 1321.12 56.3125 2 4 -3 0 1292.56 56.2543 2 4 -3 0 1338.05 56.4761 11 3 -3 0 70.7685 4.51727 2 3 -3 0 54.1760 4.68569 3 3 -3 0 71.6266 5.60775 11 -3 3 0 67.6683 4.09050 4 2 -3 0 44.8607 3.93635 4 -2 3 0 48.1197 3.43968 4 -2 3 0 47.6495 2.84760 4 1 -3 0 2456.31 105.606 4 -1 3 0 2568.24 105.744 4 -1 3 0 2534.42 105.599 4 0 -3 0 2731.79 116.018 4 0 -3 0 2826.63 115.919 4 0 3 0 2728.80 115.903 4 0 3 0 2849.76 116.029 4 0 3 0 2703.50 116.034 7 -1 -3 0 3.91782 0.76186 4 -1 -3 0 5.10849 0.99374 4 -1 -3 0 4.16910 0.80251 7 1 3 0 4.20386 0.94636 4 1 3 0 4.55477 1.06613 7 -2 -3 0 397.514 17.1595 4 -2 -3 0 414.287 17.4310 7 -2 -3 0 401.021 17.3046 4 2 3 0 372.642 17.2148 4 2 3 0 393.328 17.5595 7 2 3 0 423.565 17.2619 4 -3 -3 0 -0.3216 1.43606 7 -3 -3 0 1.72821 1.09444 4 -3 -3 0 2.24072 1.07068 4 3 3 0 2.46129 1.75605 7 -4 -3 0 3803.00 156.165 7 -4 -3 0 3692.79 155.251 4 -4 -3 0 3671.99 155.209 4 4 3 0 3596.50 155.807 1 4 3 0 3768.63 155.918 9 5 3 0 6.77529 2.63975 9 6 3 0 295.362 14.1371 9 6 3 0 292.440 14.0159 1 6 3 0 301.789 14.7989 11 8 3 0 70.0494 5.00343 11 8 3 0 70.9451 4.57379 1 7 -4 0 495.776 22.8340 11 7 -4 0 548.007 22.7300 2 6 -4 0 128.768 6.79092 2 6 -4 0 132.075 7.89067 11 -6 4 0 113.443 7.22077 6 5 -4 0 1001.13 41.3177 2 5 -4 0 889.870 43.9636 5 5 -4 0 980.507 41.7230 11 -5 4 0 933.566 41.0230 6 4 -4 0 1404.69 56.3366 11 4 -4 0 1320.52 55.2137 3 4 -4 0 1370.97 55.9161 2 -4 4 0 1291.37 56.5482 8 -4 4 0 1130.96 56.3769 6 3 -4 0 125.686 6.59566 3 3 -4 0 130.457 6.80960 2 3 -4 0 147.990 8.77780 11 -3 4 0 118.088 8.32109 8 -3 4 0 107.503 8.09690 6 -3 4 0 127.157 7.37248 4 2 -4 0 -0.2879 2.40357 4 2 -4 0 -0.7749 2.54113 3 2 -4 0 -4.2771 3.33182 11 -2 4 0 1.92518 1.54726 4 -2 4 0 2.05840 2.57162 4 -2 4 0 1.47628 2.31756 7 1 -4 0 3241.37 136.291 4 1 -4 0 3208.91 136.403 4 -1 4 0 3353.56 136.265 4 -1 4 0 3190.95 136.394 7 0 -4 0 67.2188 3.88105 4 0 4 0 69.4590 3.61864 4 0 4 0 64.4386 4.05357 4 0 4 0 67.6938 4.27928 7 -1 -4 0 3821.17 148.920 7 -1 -4 0 3467.38 149.003 4 -1 -4 0 3642.32 148.879 4 1 4 0 3320.48 148.807 4 1 4 0 3391.40 148.973 4 1 4 0 3678.87 149.297 7 -2 -4 0 2936.23 126.772 4 -2 -4 0 3120.81 126.402 7 -2 -4 0 3072.95 126.465 4 2 4 0 2817.47 126.341 4 2 4 0 3066.36 126.841 7 2 4 0 3052.38 126.236 4 -3 -4 0 1364.57 59.2960 4 -3 -4 0 1420.00 59.7169 7 -3 -4 0 1462.73 59.4795 4 3 4 0 1366.77 60.1865 7 -4 -4 0 1952.37 79.1684 4 4 4 0 1897.39 80.1520 11 4 4 0 1880.37 79.4985 9 4 4 0 1764.44 78.9148 3 5 4 0 1517.00 66.0621 11 5 4 0 1520.89 65.3443 9 5 4 0 1551.95 65.3870 1 6 4 0 6.99370 2.29324 9 6 4 0 8.16089 2.24195 1 7 4 0 0.30867 2.31561 11 7 4 0 4.64974 2.19099 1 7 4 0 4.43601 2.58594 9 8 4 0 365.005 17.4684 11 8 4 0 392.890 16.9707 1 7 -5 0 293.918 13.4423 11 7 -5 0 314.144 13.2988 2 6 -5 0 12.1819 2.16042 2 -6 5 0 11.2246 2.07763 6 5 -5 0 1028.45 42.2353 2 5 -5 0 988.621 42.5434 11 -5 5 0 936.758 42.6980 8 -5 5 0 954.378 41.9140 6 4 -5 0 125.893 6.82797 3 4 -5 0 136.479 7.10165 2 4 -5 0 145.518 8.17095 11 -4 5 0 133.942 8.34882 8 -4 5 0 117.256 7.10618 6 3 -5 0 125.441 7.32352 11 3 -5 0 112.579 7.07248 3 3 -5 0 104.735 6.35537 2 -3 5 0 118.485 6.54259 6 -3 5 0 118.550 7.43797 8 2 -5 0 6.42528 2.47510 2 2 -5 0 6.46390 2.40412 11 2 -5 0 11.2374 1.88215 3 -2 5 0 8.12119 2.47555 8 -2 5 0 5.66964 1.95157 6 -2 5 0 4.43715 2.24230 4 1 -5 0 291.757 13.3180 3 1 -5 0 296.457 13.6960 11 -1 5 0 277.069 13.1871 6 -1 5 0 291.195 13.9536 4 -1 5 0 302.861 13.9960 8 -1 5 0 311.068 14.8108 4 -1 5 0 274.604 14.2948 7 0 -5 0 6.63415 2.14531 4 0 -5 0 9.50737 2.92842 4 0 5 0 4.28087 1.46546 4 0 5 0 5.83231 2.62605 7 -1 -5 0 554.922 23.0829 4 -1 -5 0 520.544 23.0955 4 1 5 0 515.087 23.7393 7 1 5 0 508.902 22.7931 4 -2 -5 0 3361.39 134.475 7 -2 -5 0 3042.69 134.632 4 2 5 0 3189.63 135.293 7 -3 -5 0 1.76313 2.22952 4 -3 -5 0 2.98131 3.45578 7 3 5 0 2.62867 2.39052 9 3 5 0 8.25921 2.84200 1 3 5 0 3.51377 2.17458 3 -4 -5 0 220.732 11.1792 4 4 5 0 190.494 10.0100 1 4 5 0 201.656 10.2090 9 5 5 0 0.18212 2.36893 11 5 5 0 -0.5558 2.46887 3 5 5 0 5.29494 2.01595 9 6 5 0 223.917 10.7977 1 6 5 0 207.566 10.7451 9 6 5 0 209.179 11.6913 11 7 5 0 438.110 19.4812 9 7 5 0 403.741 20.2804 11 7 5 0 444.703 19.5203 1 8 5 0 691.178 27.1984 1 8 5 0 564.960 27.5804 11 8 5 0 617.875 26.9904 9 6 -6 0 7.26110 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73.3802 5.56070 6 3 -4 2 82.0728 5.86334 11 3 -4 2 69.6259 4.42344 2 3 -4 2 58.9629 4.40899 3 -4 4 -2 337.146 15.7186 6 -4 4 -2 335.077 16.5606 8 4 -4 2 340.148 15.0748 3 4 -4 2 349.739 17.8622 5 4 -4 2 338.635 16.2076 11 4 -4 2 335.554 15.5366 2 -5 4 -2 613.832 27.1664 6 5 -4 2 618.251 27.1367 2 5 -4 2 614.140 27.6023 11 5 -4 2 623.030 29.7822 5 -6 4 -2 897.109 42.4744 6 6 -4 2 1111.70 42.8021 2 6 -4 2 851.371 44.6681 5 6 -4 2 1113.38 43.0301 11 7 -4 2 464.414 20.1611 2 8 3 -2 2.92734 1.89533 1 8 3 -2 1.64842 1.70918 11 7 3 -2 504.075 22.4695 11 7 3 -2 482.293 21.7445 1 -7 -3 2 478.875 21.9968 6 6 3 -2 595.849 26.6690 9 6 3 -2 606.322 26.6865 1 6 3 -2 604.222 27.3931 11 5 3 -2 473.724 21.7129 3 5 3 -2 499.960 22.2168 9 5 3 -2 510.009 22.2037 1 4 3 -2 2050.01 85.3179 9 4 3 -2 2008.92 84.6320 3 -4 -3 2 2083.50 85.0044 4 -4 -3 2 1890.95 85.1708 8 3 3 -2 6191.84 256.654 7 3 3 -2 5697.40 256.314 9 -3 -3 2 6271.89 256.001 4 -3 -3 2 6199.98 256.335 7 -3 -3 2 6202.88 255.977 4 2 3 -2 171.781 8.57069 7 2 3 -2 158.276 8.79716 4 2 3 -2 164.346 8.01809 4 -2 -3 2 176.160 8.20010 4 -2 -3 2 178.386 8.37959 7 -2 -3 2 174.663 8.17381 4 1 3 -2 125.001 5.99500 4 1 3 -2 124.815 6.40479 7 1 3 -2 120.921 6.51539 4 -1 -3 2 125.796 6.15617 7 -1 -3 2 127.412 6.12648 4 -1 -3 2 125.208 6.17861 4 0 3 -2 2545.45 108.096 4 0 3 -2 2568.70 107.909 4 0 3 -2 2525.23 108.051 7 0 -3 2 2605.48 107.936 4 0 -3 2 2610.98 108.056 4 -1 3 -2 1136.87 47.1411 4 -1 3 -2 1097.78 47.2463 7 1 -3 2 1107.46 47.2001 4 -2 3 -2 1480.96 61.2728 4 -2 3 -2 1409.70 61.4738 7 -2 3 -2 1462.65 61.6330 4 -3 3 -2 1674.56 71.1455 4 3 -3 2 1747.57 71.8359 11 3 -3 2 1703.10 71.4213 2 3 -3 2 1611.61 70.8820 3 4 -3 2 1686.61 73.2749 2 4 -3 2 1714.31 73.7710 11 4 -3 2 1618.79 72.6084 3 4 -3 2 1888.91 75.6448 5 5 -3 2 40.0501 3.43694 2 5 -3 2 35.2988 5.60383 5 5 -3 2 47.9379 5.17587 11 6 -3 2 1989.15 77.3838 2 6 -3 2 1702.01 79.7258 5 6 -3 2 1766.08 78.4868 11 7 -3 2 2.54287 1.26460 2 7 -3 2 5.92022 2.44447 11 8 2 -2 70.3492 4.60738 1 8 2 -2 73.1727 4.65326 11 7 2 -2 14.4878 2.63962 2 7 2 -2 20.7146 4.28487 11 7 2 -2 20.0206 3.16147 1 6 2 -2 906.773 40.1814 1 6 2 -2 955.750 40.8641 11 6 2 -2 932.976 40.3404 2 6 2 -2 916.880 40.1516 9 5 2 -2 33.6181 3.61681 1 5 2 -2 29.1850 4.07884 11 5 2 -2 34.2070 4.24051 3 5 2 -2 29.1959 4.17746 2 4 2 -2 734.738 31.4961 1 4 2 -2 701.536 31.5383 9 4 2 -2 728.377 31.0703 3 4 2 -2 700.422 31.9108 11 -4 -2 2 754.930 31.2912 4 -3 -2 2 113.357 6.56950 7 -3 -2 2 121.209 5.96131 4 -3 -2 2 121.100 6.16046 4 2 2 -2 152.222 7.49238 4 2 2 -2 154.583 7.03296 4 2 2 -2 154.521 7.51099 7 -2 -2 2 156.982 7.17248 4 -2 -2 2 150.673 7.11409 4 -2 -2 2 152.992 7.35764 7 1 2 -2 1948.92 80.1446 4 1 2 -2 1888.65 80.1261 7 1 2 -2 1872.48 79.9472 4 -1 -2 2 1878.85 80.0573 7 -1 -2 2 1895.67 80.0673 4 -1 -2 2 1948.07 79.9985 4 0 2 -2 1729.73 71.5110 4 0 2 -2 1676.37 71.6211 4 0 2 -2 1636.47 71.5524 7 0 -2 2 1733.46 71.5090 7 0 -2 2 1708.30 71.5958 4 0 -2 2 1734.21 71.5187 4 -1 2 -2 597.812 25.6188 4 -1 2 -2 602.740 25.5136 7 -1 2 -2 607.906 25.4655 4 1 -2 2 600.134 25.4586 4 1 -2 2 586.317 25.5317 4 -2 2 -2 2875.47 115.083 4 -2 2 -2 2415.40 115.169 7 -2 2 -2 2650.56 115.632 4 2 -2 2 2836.08 115.095 4 2 -2 2 2953.11 115.135 4 -3 2 -2 1478.62 60.3768 4 3 -2 2 1386.80 60.7433 2 -4 2 -2 2145.64 90.9781 4 4 -2 2 2106.50 91.4109 2 4 -2 2 2173.96 91.7852 11 4 -2 2 2228.32 93.2128 5 5 -2 2 288.993 13.7499 2 5 -2 2 284.223 14.3571 11 5 -2 2 309.386 15.9275 5 6 -2 2 3.83263 3.95069 5 7 -2 2 20.2717 4.24773 11 8 -2 2 1.98633 1.93593 11 8 -2 2 0.25379 1.22189 2 8 1 -2 754.614 32.9126 2 8 1 -2 776.558 33.1174 11 7 1 -2 676.371 30.7218 1 7 1 -2 713.137 31.0296 2 7 1 -2 724.301 31.7274 11 6 1 -2 665.362 29.2830 11 6 1 -2 644.096 28.6569 1 6 1 -2 647.580 28.9716 2 5 1 -2 261.359 12.0705 3 5 1 -2 258.806 12.8504 11 5 1 -2 260.919 12.4099 1 5 1 -2 257.427 12.7653 9 4 1 -2 17.2428 3.76957 9 4 1 -2 19.3884 3.55221 1 4 1 -2 21.2242 2.84891 3 4 1 -2 24.1272 3.81582 11 -4 -1 2 18.6027 2.98435 4 -3 -1 2 3645.24 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367.651 17.8643 2 -4 6 -3 2.13723 1.58169 6 -4 6 -3 0.95017 2.28692 8 4 -6 3 1.66344 1.62991 3 4 -6 3 4.16097 1.85808 2 -5 6 -3 156.265 7.00001 6 5 -6 3 126.888 8.36200 5 5 -6 3 134.658 7.03482 2 -6 6 -3 99.3616 5.13210 6 8 5 -3 49.4903 3.70125 11 7 5 -3 155.890 8.31798 11 7 5 -3 154.193 7.66996 1 -7 -5 3 149.335 7.54216 6 6 5 -3 685.188 30.4945 11 6 5 -3 691.635 29.7679 9 -6 -5 3 614.986 29.1400 8 -6 -5 3 654.555 28.6213 6 5 5 -3 3.19158 1.96771 1 5 5 -3 4.58157 1.87966 3 5 5 -3 1.28197 2.10753 11 5 5 -3 1.97187 1.86918 9 -5 -5 3 4.20893 2.14595 6 -5 -5 3 3.43437 2.81489 10 -5 -5 3 1.70824 2.71284 8 4 5 -3 90.5332 5.80971 1 4 5 -3 100.599 5.69311 3 4 5 -3 94.7239 6.97893 11 4 5 -3 95.1050 5.82046 9 -4 -5 3 94.6526 6.22738 8 -4 -5 3 94.1145 5.78768 10 -4 -5 3 91.9378 5.54722 6 3 5 -3 2159.42 92.1821 3 3 5 -3 2137.20 92.0831 1 3 5 -3 2241.24 92.4879 9 2 5 -3 16.7886 2.60033 3 2 5 -3 22.8570 3.50248 8 2 5 -3 8.50862 2.36228 9 -2 -5 3 13.5901 1.81925 6 -2 -5 3 19.3692 4.58467 4 -2 -5 3 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5 88.3041 6.88607 1 5 5 5 84.4620 6.39207 9 6 5 5 2227.09 96.6708 9 6 5 5 2397.89 96.8394 1 6 5 5 2173.03 97.9485 5 7 5 5 214.160 10.8346 1 7 5 5 204.031 11.1797 9 8 5 5 1136.83 51.9834 9 8 5 5 1304.06 51.8165 1 6 -6 -5 30.6649 2.42141 2 -6 6 5 34.0720 2.35813 6 -6 6 5 30.3195 3.39660 8 5 -6 -5 10.8041 2.30740 2 5 -6 -5 11.8703 1.88355 3 5 -6 -5 8.15366 2.28341 11 -5 6 5 11.4917 1.74397 6 -5 6 5 6.86077 2.18683 8 4 -6 -5 623.142 27.3787 2 4 -6 -5 621.750 26.9810 3 4 -6 -5 593.736 27.9363 11 -4 6 5 653.513 27.0540 6 -4 6 5 612.311 27.7995 8 3 -6 -5 1784.68 80.9523 11 3 -6 -5 1914.13 81.1261 2 3 -6 -5 1928.91 80.8082 3 -3 6 5 1958.74 80.7273 6 -3 6 5 1961.33 81.5518 8 2 -6 -5 348.044 15.7548 8 2 -6 -5 328.413 15.4440 3 -2 6 5 353.040 16.1350 8 -2 6 5 331.428 15.2215 6 -2 6 5 342.346 17.2243 3 1 -6 -5 801.876 34.5797 6 1 -6 -5 813.293 35.0346 3 1 -6 -5 835.164 35.1796 8 -1 6 5 805.963 35.6193 3 -1 6 5 866.806 35.5710 8 -1 6 5 788.990 34.6668 6 -1 6 5 768.936 36.0462 4 0 -6 -5 2366.49 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5 1907.16 79.8685 5 4 7 5 1844.68 77.6869 9 5 7 5 83.7485 8.14833 5 5 7 5 79.1727 5.82863 9 5 7 5 82.5137 6.40045 1 6 7 5 1527.98 63.9240 9 6 7 5 1458.44 64.2543 1 6 7 5 1469.53 65.3671 5 7 7 5 833.249 39.9057 1 7 7 5 1001.62 39.9805 9 8 7 5 149.475 7.44218 9 8 7 5 135.277 7.18926 1 -5 8 5 441.674 19.5756 8 -5 8 5 454.411 19.1027 6 4 -8 -5 96.0747 5.15906 3 -4 8 5 97.2339 4.96432 6 -4 8 5 97.4899 5.72993 8 3 -8 -5 454.343 19.9961 3 -3 8 5 454.027 20.6402 8 -3 8 5 440.192 20.2578 6 2 -8 -5 19.0418 3.01822 3 -2 8 5 18.8926 3.16069 8 -2 8 5 11.4383 3.56670 3 -2 8 5 17.0932 2.33920 6 1 -8 -5 282.517 13.2129 8 1 -8 -5 269.615 13.0890 3 -1 8 5 287.752 12.5247 6 -1 8 5 279.810 13.5597 8 -1 8 5 272.952 13.8229 3 0 -8 -5 136.657 6.88933 6 0 -8 -5 147.203 7.69526 8 0 -8 -5 140.424 8.03224 3 0 8 5 140.992 7.91018 8 0 8 5 142.973 8.03322 3 -1 -8 -5 1122.96 46.2882 6 -1 -8 -5 1040.49 47.0211 3 -1 -8 -5 1119.62 46.9168 8 1 8 5 1060.40 47.0673 3 1 8 5 1097.93 47.0438 8 -2 -8 -5 22.5392 3.52822 8 -2 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313.191 13.5867 3 -1 6 -9 1.22835 1.28323 8 1 -6 9 2.25396 0.98786 3 4 5 -9 154.351 7.08104 3 -4 -5 9 152.367 7.12390 8 3 5 -9 868.792 36.8644 3 -3 -5 9 868.961 37.0150 3 -3 -5 9 843.958 36.7687 8 -3 -5 9 879.139 36.9419 10 2 5 -9 1795.67 78.3734 8 2 5 -9 1854.68 78.6003 3 -2 -5 9 1797.24 78.6178 10 -2 -5 9 1956.41 78.5907 3 -2 -5 9 1907.91 78.3858 8 1 5 -9 6.95166 1.69891 8 1 5 -9 5.10343 2.52166 3 -1 -5 9 4.05687 1.67052 10 -1 -5 9 4.55989 1.36660 3 0 5 -9 238.205 11.1803 8 0 -5 9 243.783 10.9694 3 0 -5 9 240.992 11.3967 10 -1 5 -9 368.542 16.3743 6 -1 5 -9 365.246 16.6348 8 1 -5 9 376.907 16.9597 10 1 -5 9 385.743 16.3492 3 -2 5 -9 91.0195 5.10506 6 -2 5 -9 85.9219 4.82481 8 -3 5 -9 23.2289 2.93510 8 -3 5 -9 30.3492 2.83158 6 4 4 -9 38.0640 2.87009 3 -4 -4 9 33.4865 2.78441 8 -4 -4 9 42.2777 5.52444 10 3 4 -9 59.4590 3.97314 3 -3 -4 9 53.5486 4.18990 10 -3 -4 9 55.9777 3.65441 8 -3 -4 9 49.5529 4.67341 3 2 4 -9 333.355 15.3697 8 2 4 -9 329.431 15.5656 3 -2 -4 9 334.742 15.5334 10 -2 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3 -9 279.559 13.5277 8 -1 -3 9 300.295 13.3802 3 -1 -3 9 307.856 13.4951 8 -1 -3 9 278.975 13.5541 10 0 3 -9 73.2158 5.12838 6 0 3 -9 62.1415 4.60343 8 0 3 -9 56.2327 7.53825 3 0 -3 9 65.7396 4.15712 3 0 -3 9 64.2814 4.88442 10 -1 3 -9 1480.28 63.1964 8 -1 3 -9 1388.73 62.4805 6 1 -3 9 1526.20 62.2077 3 -2 3 -9 1502.64 63.5576 6 -2 3 -9 1511.33 63.6734 8 2 -3 9 1546.03 63.1490 3 2 -3 9 1467.60 63.5312 2 2 -3 9 1514.79 63.9730 10 2 -3 9 1421.09 64.6073 5 -3 3 -9 380.134 16.6749 8 -3 3 -9 372.580 16.6574 6 3 -3 9 361.674 16.5046 2 3 -3 9 361.682 17.6067 5 -4 3 -9 592.128 24.4992 6 4 -3 9 551.102 24.3859 2 4 -3 9 550.268 25.3988 5 5 2 -9 67.1257 3.76510 3 5 2 -9 67.7246 4.66648 2 -5 -2 9 59.0768 3.59005 6 -5 -2 9 65.6477 4.00097 8 4 2 -9 10.0425 1.88490 3 -4 -2 9 6.13225 1.74157 8 -4 -2 9 7.63402 1.52373 6 3 2 -9 458.512 20.6662 3 3 2 -9 443.992 20.4522 8 -3 -2 9 471.807 20.8072 10 -3 -2 9 466.899 20.6526 8 -3 -2 9 469.832 20.8742 3 2 2 -9 48.2738 3.94124 8 2 2 -9 42.7169 4.67928 3 -2 -2 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275.016 12.3242 6 -5 -1 9 284.501 12.9043 8 4 1 -9 69.3518 4.37835 3 -4 -1 9 66.6458 4.53812 8 -4 -1 9 65.5154 3.97311 6 3 1 -9 1293.99 56.1753 8 -3 -1 9 1352.35 56.9165 3 -3 -1 9 1281.24 56.3298 8 -3 -1 9 1341.61 56.6861 10 2 1 -9 103.758 6.00378 8 2 1 -9 100.435 6.39842 3 -2 -1 9 99.6593 6.42039 10 -2 -1 9 106.038 5.95191 8 -2 -1 9 104.466 6.18018 3 1 1 -9 3314.14 139.527 8 1 1 -9 3269.01 139.494 3 1 1 -9 3137.11 138.797 6 -1 -1 9 3326.37 139.276 3 -1 -1 9 3524.51 139.323 8 -1 -1 9 3276.70 139.471 10 0 1 -9 1054.08 45.5066 8 0 1 -9 1043.16 45.1139 6 0 1 -9 1003.32 45.7457 3 0 -1 9 1096.75 45.1225 3 0 -1 9 1059.39 45.5019 10 -1 1 -9 1605.94 69.5639 6 -1 1 -9 1666.06 69.8047 8 1 -1 9 1629.34 69.6895 2 1 -1 9 1596.27 69.8529 10 1 -1 9 1672.71 69.2984 3 -2 1 -9 982.320 41.4297 8 -2 1 -9 953.347 41.2527 6 2 -1 9 935.489 41.1733 2 2 -1 9 940.549 40.7649 3 2 -1 9 955.593 41.7148 10 2 -1 9 957.733 44.2500 5 -3 1 -9 280.317 13.3129 6 3 -1 9 275.130 13.1231 2 3 -1 9 283.048 14.7534 5 3 -1 9 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13.8414 2.31979 9 3 5 12 15.0751 3.85913 5 -4 -5 -12 684.925 28.0602 6 4 5 12 658.378 28.5689 9 4 5 12 635.845 29.4176 5 5 5 12 186.662 8.65340 9 5 5 12 186.730 9.32170 5 2 -6 -12 45.6886 3.71023 3 -2 6 12 52.5923 3.79130 3 1 -6 -12 124.030 7.13368 3 1 -6 -12 122.005 6.14885 8 -1 6 12 123.593 6.42306 3 0 -6 -12 160.299 7.69314 8 0 -6 -12 146.348 7.07516 6 0 6 12 161.084 7.78288 3 -1 -6 -12 1092.19 45.9842 6 -1 -6 -12 1117.84 46.5435 8 1 6 12 1096.76 46.4530 3 1 6 12 1050.22 46.4841 9 -2 -6 -12 154.468 7.71504 8 -2 -6 -12 156.968 7.19893 6 2 6 12 160.710 9.98667 5 2 6 12 157.972 7.88885 9 2 6 12 143.029 7.46261 3 2 6 12 151.315 7.86352 1 -3 -6 -12 55.6122 4.18012 8 -3 -6 -12 67.7081 3.50138 6 3 6 12 53.5789 5.04555 5 3 6 12 59.9521 4.09491 9 3 6 12 58.7104 4.22155 1 -4 -6 -12 341.822 14.5954 6 4 6 12 298.689 16.0510 1 4 6 12 325.778 14.4976 9 -2 7 12 137.175 6.89916 3 1 -7 -12 4.84763 2.22556 8 1 -7 -12 5.53242 2.96256 3 -1 7 12 2.52581 1.40252 3 0 -7 -12 61.2510 3.77136 8 0 7 12 58.4584 3.91559 3 -1 -7 -12 99.2879 4.77328 6 -1 -7 -12 92.0760 5.28386 8 1 7 12 101.063 5.34161 3 -2 -7 -12 1044.51 44.0435 8 -2 -7 -12 1050.99 43.6319 6 2 7 12 1040.39 43.7226 3 2 7 12 1034.86 44.2095 1 2 7 12 994.588 44.0274 9 -3 -7 -12 216.878 9.18391 6 -3 -7 -12 202.080 10.5386 8 3 7 12 202.613 9.66446 9 3 7 12 213.739 9.72522 1 3 7 12 187.571 12.0705 5 -4 -7 -12 1072.19 43.6497 6 4 7 12 989.818 43.8792 1 4 7 12 1010.99 44.8184 5 4 7 12 1072.15 44.9290 9 1 -8 -12 219.082 10.7246 8 -1 8 12 266.079 10.9762 3 0 -8 -12 329.045 15.1790 8 0 8 12 347.519 15.3090 3 0 8 12 362.445 15.4209 1 -1 -8 -12 46.6000 3.30591 8 1 8 12 51.8465 3.37877 3 1 8 12 47.8338 3.35502 1 -2 -8 -12 958.583 40.0600 8 -2 -8 -12 948.523 39.6545 6 2 8 12 937.923 40.1806 1 2 8 12 915.201 39.6191 3 -3 -8 -12 4.79852 1.13244 6 -3 -8 -12 2.87131 1.93053 8 3 8 12 1.20002 1.92990 9 3 8 12 2.42791 2.16901 1 -4 -8 -12 26.0284 2.10241 6 4 8 12 24.0374 2.75221 9 4 8 12 23.4877 2.64298 1 0 -9 -12 150.506 7.01146 8 0 9 12 153.706 7.11945 3 -1 -9 -12 84.2081 4.48296 8 1 9 12 84.5226 4.55734 1 1 9 12 90.1835 4.56836 3 -2 -9 -12 17.8541 2.30488 8 -2 -9 -12 13.2221 1.82685 6 2 9 12 18.5338 2.17183 1 -3 -9 -12 327.370 13.7808 6 3 9 12 315.085 14.1305 1 0 0 -13 28.6004 2.35077 8 0 0 13 31.3663 2.75956 9 0 0 13 30.5427 2.49345 3 0 0 13 35.3041 3.11521 10 1 -1 -13 53.5661 3.44906 8 -1 1 13 60.6013 3.54915 3 -1 1 13 63.6545 3.69006 9 0 -1 -13 215.282 9.82675 8 0 1 13 219.090 10.1072 10 0 1 13 212.393 10.0601 9 0 1 13 223.074 9.79005 3 -1 -1 -13 6.30839 1.35820 8 1 1 13 4.56903 1.82680 10 1 1 13 4.97123 1.63600 9 -2 -1 -13 316.998 13.8536 8 -2 -1 -13 316.840 13.5665 6 2 1 13 318.782 14.0486 9 1 -2 -13 260.750 11.6088 8 -1 2 13 262.904 11.7834 9 -1 2 13 264.631 11.7681 3 0 -2 -13 42.6771 2.90496 8 0 2 13 34.8453 3.60358 10 0 2 13 39.0044 3.11460 9 0 2 13 45.8582 3.03619 3 -1 -2 -13 37.6121 2.70634 8 -1 -2 -13 36.2755 2.84331 6 1 2 13 35.1146 2.99216 9 1 2 13 33.1896 3.35478 10 1 2 13 32.1733 3.07182 3 -2 -2 -13 51.1516 3.37028 8 -3 -2 -13 914.450 38.4459 6 1 -3 -13 248.143 10.9520 8 -1 3 13 243.046 11.1866 9 0 -3 -13 1288.18 53.5620 8 0 3 13 1257.49 53.5488 3 0 3 13 1251.48 53.6606 9 -1 -3 -13 1333.18 55.3623 8 -1 -3 -13 1302.00 54.9181 6 1 3 13 1293.35 55.1722 3 1 3 13 1304.67 55.5287 9 -2 -3 -13 440.540 19.3606 8 -2 -3 -13 448.639 18.9845 6 2 3 13 445.191 19.5169 9 -3 -3 -13 250.792 10.8891 6 3 3 13 251.329 11.3682 9 1 -4 -13 11.9882 1.69969 8 -1 4 13 11.7905 3.13161 3 0 -4 -13 1.79027 1.31660 8 0 4 13 0.23685 1.82878 9 0 4 13 -1.1567 1.23112 3 -1 -4 -13 98.0847 4.66897 6 -1 -4 -13 95.9841 5.09890 8 1 4 13 96.6237 5.09304 3 1 4 13 98.2793 5.40161 9 -2 -4 -13 103.649 5.85955 8 -2 -4 -13 103.571 4.88567 6 2 4 13 98.4482 5.43495 9 -3 -4 -13 790.966 33.2179 6 3 4 13 783.073 33.6715 9 1 -5 -13 676.866 29.1554 8 -1 5 13 695.529 29.3445 3 0 -5 -13 22.9351 2.29544 8 0 5 13 18.3185 2.98328 9 0 5 13 23.2020 2.46750 3 -1 -5 -13 165.584 7.66275 8 -1 -5 -13 150.081 7.27089 6 1 5 13 160.130 7.84184 1 1 5 13 168.181 7.59434 3 -2 -5 -13 2.48595 1.01643 6 -2 -5 -13 -1.2732 2.81243 8 2 5 13 1.21783 1.53806 9 -3 -5 -13 23.7506 1.95701 6 -3 -5 -13 22.1408 4.17889 8 3 5 13 17.4370 2.35976 9 1 -6 -13 2.99039 2.41741 8 -1 6 13 -0.1408 1.34336 3 0 -6 -13 29.3020 2.98313 8 0 6 13 31.7932 3.28741 3 -1 -6 -13 93.5465 4.78037 8 -1 -6 -13 89.5969 4.32346 6 1 6 13 88.6825 4.90753 1 1 6 13 97.0767 5.47727 9 1 6 13 79.8232 4.72693 3 -2 -6 -13 6.12884 1.64909 8 2 6 13 7.50590 2.13575 1 2 6 13 8.09855 1.83375 9 -3 -6 -13 52.5445 2.92525 6 3 6 13 54.1849 3.48173 9 0 -7 -13 78.5808 4.30309 8 0 7 13 85.3536 4.43567 3 0 7 13 87.6316 4.45394 1 -1 -7 -13 774.142 32.4564 8 1 7 13 756.426 32.5002 1 1 7 13 756.851 32.2317 3 -2 -7 -13 515.663 21.9015 8 -2 -7 -13 508.223 21.5548 6 2 7 13 503.586 21.9296 1 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7538 _exptl_absorpt_correction_T_min 0.4581 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54172 7.092 10.372 10.957 71.918 83.951 76.994 ) ; _shelx_hkl_checksum 5565 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Cu1 Cu 1.0000 0.0000 0.0000 0.01223(11) Uani 1 2 d S T P Cl2 Cl 0.89347(6) -0.18782(4) -0.02738(3) 0.01517(11) Uani 1 1 d . . . S3 S 1.32343(6) -0.13920(4) -0.21557(4) 0.01644(11) Uani 1 1 d . . . S4 S 0.96400(6) 0.50869(4) -0.27197(4) 0.01691(11) Uani 1 1 d . . . O2 O 1.25845(18) -0.02067(12) -0.15875(11) 0.0163(2) Uani 1 1 d . . . O0AA O 0.52337(18) 0.37733(13) -0.56793(11) 0.0182(3) Uani 1 1 d . . . C7 C 0.5052(2) 0.21215(17) -0.22260(15) 0.0144(3) Uani 1 1 d . . . H7 H 0.3690 0.2211 -0.2076 0.017 Uiso 1 1 calc R . . C8 C 0.7815(2) 0.26033(16) -0.36114(15) 0.0135(3) Uani 1 1 d . . . H8 H 0.8375 0.3018 -0.4426 0.016 Uiso 1 1 calc R . . O10 O 0.27572(19) 0.32175(16) -0.43154(11) 0.0259(3) Uani 1 1 d . . . H10 H 0.2148 0.3470 -0.4996 0.039 Uiso 1 1 calc GR . . C11 C 0.6309(2) 0.14198(16) -0.12378(15) 0.0139(3) Uani 1 1 d . . . H11 H 0.5781 0.1018 -0.0408 0.017 Uiso 1 1 calc R . . C13 C 0.5831(2) 0.26945(16) -0.34485(14) 0.0129(3) Uani 1 1 d . . . C16 C 0.4581(2) 0.33068(17) -0.46000(15) 0.0146(3) Uani 1 1 d . . . C20 C 0.8977(2) 0.18966(16) -0.25669(15) 0.0132(3) Uani 1 1 d . . . H20 H 1.0337 0.1845 -0.2679 0.016 Uiso 1 1 calc R . . N28 N 0.8240(2) 0.12821(14) -0.14006(12) 0.0124(3) Uani 1 1 d . . . O1 O 0.91716(19) 0.64745(14) -0.37636(11) 0.0220(3) Uani 1 1 d . . . C1AA C 1.1488(3) 0.52769(18) -0.18478(17) 0.0198(4) Uani 1 1 d . . . H1AA H 1.2638 0.5415 -0.2415 0.030 Uiso 1 1 calc GR . . H1AB H 1.1825 0.4440 -0.1122 0.030 Uiso 1 1 calc GR . . H1AC H 1.1018 0.6080 -0.1527 0.030 Uiso 1 1 calc GR . . C3 C 1.1717(3) -0.1028(2) -0.34774(17) 0.0232(4) Uani 1 1 d . . . H3A H 1.0389 -0.1098 -0.3153 0.035 Uiso 1 1 calc GR . . H3B H 1.2207 -0.1697 -0.3959 0.035 Uiso 1 1 calc GR . . H3C H 1.1724 -0.0088 -0.4045 0.035 Uiso 1 1 calc GR . . C4 C 0.7686(3) 0.5111(2) -0.15497(17) 0.0242(4) Uani 1 1 d . . . H4A H 0.7545 0.5933 -0.1259 0.036 Uiso 1 1 calc GR . . H4B H 0.7959 0.4275 -0.0815 0.036 Uiso 1 1 calc GR . . H4C H 0.6482 0.5141 -0.1933 0.036 Uiso 1 1 calc GR . . C5 C 1.5430(3) -0.1070(2) -0.30569(18) 0.0239(4) Uani 1 1 d . . . H5A H 1.5186 -0.0140 -0.3673 0.036 Uiso 1 1 calc GR . . H5B H 1.5883 -0.1759 -0.3522 0.036 Uiso 1 1 calc GR . . H5C H 1.6424 -0.1136 -0.2469 0.036 Uiso 1 1 calc GR . . 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 Cu1 0.01558(19) 0.01047(17) 0.00886(17) 0.00018(12) -0.00369(13) -0.00189(13) Cl2 0.0192(2) 0.01301(19) 0.01282(18) -0.00240(14) -0.00162(14) -0.00380(14) S3 0.0208(2) 0.0138(2) 0.01345(19) -0.00351(15) -0.00112(15) -0.00172(15) S4 0.0205(2) 0.0186(2) 0.01289(19) -0.00542(15) -0.00033(15) -0.00550(16) O2 0.0207(6) 0.0160(6) 0.0117(5) -0.0045(4) 0.0004(4) -0.0025(5) O0AA 0.0211(6) 0.0214(6) 0.0093(5) -0.0009(4) 0.0002(5) -0.0044(5) C7 0.0170(8) 0.0145(7) 0.0109(7) -0.0028(6) 0.0006(6) -0.0033(6) C8 0.0161(8) 0.0138(7) 0.0099(7) -0.0020(6) -0.0009(6) -0.0036(6) O10 0.0157(6) 0.0463(8) 0.0095(5) 0.0010(5) -0.0034(5) -0.0059(6) C11 0.0177(8) 0.0139(7) 0.0090(7) -0.0010(6) 0.0000(6) -0.0045(6) C13 0.0169(8) 0.0108(7) 0.0097(7) -0.0015(6) -0.0023(6) -0.0016(6) C16 0.0172(8) 0.0128(7) 0.0113(7) -0.0025(6) -0.0013(6) 0.0006(6) C20 0.0123(8) 0.0139(7) 0.0124(7) -0.0019(6) -0.0017(6) -0.0027(6) N28 0.0158(7) 0.0112(6) 0.0100(6) -0.0021(5) -0.0028(5) -0.0027(5) O1 0.0210(6) 0.0297(7) 0.0118(6) 0.0017(5) -0.0046(5) -0.0074(5) C1AA 0.0213(9) 0.0194(8) 0.0166(8) 0.0004(6) -0.0056(7) -0.0057(7) C3 0.0255(10) 0.0281(10) 0.0195(8) -0.0120(7) -0.0034(7) -0.0041(8) C4 0.0235(10) 0.0302(10) 0.0137(8) -0.0002(7) 0.0025(7) -0.0056(8) C5 0.0242(10) 0.0253(9) 0.0227(9) -0.0111(7) 0.0043(7) -0.0027(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 Cl2 Cu1 Cl2 180.0 . 2_755 Cl2 Cu1 O2 89.41(3) . 2_755 Cl2 Cu1 O2 90.59(3) 2_755 2_755 Cl2 Cu1 O2 89.41(3) 2_755 . Cl2 Cu1 O2 90.59(3) . . O2 Cu1 O2 180.0 . 2_755 N28 Cu1 Cl2 91.21(4) 2_755 . N28 Cu1 Cl2 88.79(4) . . N28 Cu1 Cl2 88.79(4) 2_755 2_755 N28 Cu1 Cl2 91.21(4) . 2_755 N28 Cu1 O2 89.68(5) . . N28 Cu1 O2 89.68(5) 2_755 2_755 N28 Cu1 O2 90.32(5) . 2_755 N28 Cu1 O2 90.32(5) 2_755 . N28 Cu1 N28 180.0 . 2_755 O2 S3 C3 106.40(8) . . O2 S3 C5 104.71(8) . . C3 S3 C5 98.19(9) . . O1 S4 C1AA 104.21(8) . . O1 S4 C4 105.65(8) . . C1AA S4 C4 99.29(9) . . S3 O2 Cu1 126.50(7) . . C11 C7 H7 120.7 . . C11 C7 C13 118.51(15) . . C13 C7 H7 120.7 . . C13 C8 H8 120.5 . . C13 C8 C20 119.03(14) . . C20 C8 H8 120.5 . . C16 O10 H10 109.5 . . C7 C11 H11 118.6 . . N28 C11 C7 122.84(14) . . N28 C11 H11 118.6 . . C7 C13 C16 121.36(15) . . C8 C13 C7 118.89(15) . . C8 C13 C16 119.59(14) . . O0AA C16 O10 124.50(16) . . O0AA C16 C13 122.62(16) . . O10 C16 C13 112.80(14) . . C8 C20 H20 118.9 . . N28 C20 C8 122.24(15) . . N28 C20 H20 118.9 . . C11 N28 Cu1 120.54(10) . . C11 N28 C20 118.35(14) . . C20 N28 Cu1 120.70(11) . . S4 C1AA H1AA 109.5 . . S4 C1AA H1AB 109.5 . . S4 C1AA H1AC 109.5 . . H1AA C1AA H1AB 109.5 . . H1AA C1AA H1AC 109.5 . . H1AB C1AA H1AC 109.5 . . S3 C3 H3A 109.5 . . S3 C3 H3B 109.5 . . S3 C3 H3C 109.5 . . H3A C3 H3B 109.5 . . H3A C3 H3C 109.5 . . H3B C3 H3C 109.5 . . S4 C4 H4A 109.5 . . S4 C4 H4B 109.5 . . S4 C4 H4C 109.5 . . H4A C4 H4B 109.5 . . H4A C4 H4C 109.5 . . H4B C4 H4C 109.5 . . S3 C5 H5A 109.5 . . S3 C5 H5B 109.5 . . S3 C5 H5C 109.5 . . H5A C5 H5B 109.5 . . H5A C5 H5C 109.5 . . H5B C5 H5C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 Cl2 2.3514(4) . Cu1 Cl2 2.3514(4) 2_755 Cu1 O2 2.4092(11) 2_755 Cu1 O2 2.4092(11) . Cu1 N28 2.0155(13) 2_755 Cu1 N28 2.0155(13) . S3 O2 1.5066(12) . S3 C3 1.7886(19) . S3 C5 1.7920(19) . S4 O1 1.5263(13) . S4 C1AA 1.7780(18) . S4 C4 1.7857(18) . O0AA C16 1.215(2) . C7 H7 0.9500 . C7 C11 1.384(2) . C7 C13 1.396(2) . C8 H8 0.9500 . C8 C13 1.383(2) . C8 C20 1.389(2) . O10 H10 0.8400 . O10 C16 1.314(2) . C11 H11 0.9500 . C11 N28 1.341(2) . C13 C16 1.504(2) . C20 H20 0.9500 . C20 N28 1.347(2) . C1AA H1AA 0.9800 . C1AA H1AB 0.9800 . C1AA H1AC 0.9800 . C3 H3A 0.9800 . C3 H3B 0.9800 . C3 H3C 0.9800 . C4 H4A 0.9800 . C4 H4B 0.9800 . C4 H4C 0.9800 . C5 H5A 0.9800 . C5 H5B 0.9800 . C5 H5C 0.9800 . 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 C7 C11 N28 Cu1 -170.30(12) C7 C11 N28 C20 2.4(2) C7 C13 C16 O0AA -177.70(16) C7 C13 C16 O10 -0.8(2) C8 C13 C16 O0AA -2.5(2) C8 C13 C16 O10 174.49(15) C8 C20 N28 Cu1 169.46(12) C8 C20 N28 C11 -3.2(2) C11 C7 C13 C8 -3.4(2) C11 C7 C13 C16 171.93(15) C13 C7 C11 N28 0.9(2) C13 C8 C20 N28 0.7(2) C20 C8 C13 C7 2.6(2) C20 C8 C13 C16 -172.78(14) C3 S3 O2 Cu1 85.93(10) C5 S3 O2 Cu1 -170.73(9)