#------------------------------------------------------------------------------ #$Date: 2019-07-20 06:59:05 +0300 (Sat, 20 Jul 2019) $ #$Revision: 217185 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/84/2108446.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2108446 loop_ _publ_author_name 'Bodart, Laurie' 'Tumanov, Nikolay' 'Wouters, Johan' _publ_section_title ; Structural variety of clofaziminium salts: effect of the counter-ion on clofaziminium conformation and crystal packing ; _journal_coeditor_code AW5025 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first ; ; _journal_paper_doi 10.1107/S2052520619007649 _journal_volume 75 _journal_year 2019 _chemical_formula_moiety ; C27 H23 Cl2 N4 + , 0.5C8 H4 O4 2- , 0.5C8 H6 O4 ; _chemical_formula_sum 'C35 H28 Cl2 N4 O4' _chemical_formula_weight 639.51 _chemical_name_common ; bis-clofaziminium terephthalate terephthalic acid ; _chemical_name_systematic ; N-[(2E)-10-(4-chlorophenyl)-3-[(4-chlorophenyl)amino] -2,10-dihydrophenazin-2-ylidene]propan-2-aminium benzene-1,4-dicarboxylic acid benzene-1,4-dicarboxylate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary dual _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 72.472(3) _cell_angle_beta 80.688(3) _cell_angle_gamma 72.030(3) _cell_formula_units_Z 2 _cell_length_a 11.7990(4) _cell_length_b 12.0736(4) _cell_length_c 14.6803(5) _cell_measurement_reflns_used 9616 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 32.2400 _cell_measurement_theta_min 2.2350 _cell_volume 1891.44(12) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.3712 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur Ruby Gemini ultra' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_unetI/netI 0.0430 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 20823 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.508 _diffrn_reflns_theta_min 2.202 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.210 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_correction_T_min 0.917 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'Metallic dark red' _exptl_crystal_density_diffrn 1.123 _exptl_crystal_description Polygon _exptl_crystal_F_000 664 _exptl_crystal_size_max 0.571 _exptl_crystal_size_mid 0.391 _exptl_crystal_size_min 0.260 _refine_diff_density_max 0.408 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 420 _refine_ls_number_reflns 11543 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0440 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.3325P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1087 _refine_ls_wR_factor_ref 0.1178 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9100 _reflns_number_total 11543 _reflns_threshold_expression I>2\s(I) _cod_data_source_file aw5025sup1.cif _cod_data_source_block lb0221_clz-trpta_100k_remo_sq _cod_database_code 2108446 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL lb0221_clz-trpta_100k_remo_a.res in P-1 lb0221_clz-trpta_100k_remo_sq.res created by SHELXL-2016/6 at 18:09:22 on 13-Jul-2018 REM Old TITL lb0221_CLZ-TRPTA_100K_reMo in P-1 REM SHELXT solution in P-1 REM R1 0.191, Rweak 0.010, Alpha 0.043, Orientation as input REM Formula found by SHELXT: C40 N4 O5 Cl2 CELL 0.71073 11.799 12.0736 14.6803 72.472 80.688 72.03 ZERR 2 0.0004 0.0004 0.0005 0.003 0.003 0.003 LATT 1 SFAC C H N O Cl UNIT 70 56 8 8 4 EQIV $1 1-X,1-Y,1-Z L.S. 5 0 79 PLAN 30 CONF HTAB C15 O2_$1 HTAB N4 O1 HTAB N3 O1 HTAB O1A O1 BOND $H list 4 TEMP -173 ABIN fmap 2 53 acta SHEL 99 0.7 WGHT 0.051900 0.332500 FVAR 0.59782 CL1 5 -0.022007 0.699837 0.317605 11.00000 0.02217 0.05639 = 0.04420 -0.02555 0.01047 -0.02169 N1 3 0.426631 0.839160 0.177394 11.00000 0.01330 0.01432 = 0.02082 -0.00217 -0.00032 -0.00278 O2 4 0.933493 0.329364 0.427440 11.00000 0.06250 0.01591 = 0.02473 -0.00466 -0.00742 -0.00891 C12 1 0.416134 0.961695 0.146352 11.00000 0.01716 0.01409 = 0.01979 -0.00276 -0.00129 -0.00316 N2 3 0.631759 0.917843 0.111977 11.00000 0.01640 0.01460 = 0.02221 -0.00313 -0.00018 -0.00340 O1 4 0.915878 0.273221 0.300782 11.00000 0.02246 0.01461 = 0.01885 -0.00095 -0.00255 -0.00202 CL2 5 1.351230 0.558503 0.007490 11.00000 0.01732 0.02804 = 0.04906 -0.00075 0.01013 -0.00443 C1 1 0.305145 1.049314 0.148590 11.00000 0.01594 0.01779 = 0.02554 -0.00448 -0.00186 -0.00141 AFIX 43 H1 2 0.233955 1.025325 0.171479 11.00000 -1.20000 AFIX 0 C2 1 0.300931 1.169335 0.117457 11.00000 0.01975 0.01746 = 0.02859 -0.00549 -0.00234 0.00072 AFIX 43 H2 2 0.225922 1.228185 0.118495 11.00000 -1.20000 AFIX 0 O1A 4 1.003833 0.152716 0.178207 11.00000 0.02005 0.02265 = 0.02197 -0.00846 -0.00072 -0.00591 N3 3 0.878290 0.511481 0.191331 11.00000 0.01364 0.01441 = 0.02365 0.00140 -0.00032 -0.00209 C3 1 0.404672 1.207567 0.084051 11.00000 0.02642 0.01472 = 0.02901 -0.00342 -0.00237 -0.00263 AFIX 43 H3A 2 0.399521 1.291346 0.062445 11.00000 -1.20000 AFIX 0 O2A 4 0.821170 0.127056 0.192681 11.00000 0.02028 0.03711 = 0.03199 -0.01680 0.00482 -0.00890 N4 3 0.678115 0.433466 0.265316 11.00000 0.01396 0.01436 = 0.02818 0.00068 -0.00025 -0.00239 C4 1 0.513625 1.123311 0.082748 11.00000 0.02258 0.01591 = 0.02632 -0.00373 0.00122 -0.00664 AFIX 43 H4A 2 0.584011 1.149090 0.060939 11.00000 -1.20000 AFIX 0 C5 1 0.521898 0.998410 0.113624 11.00000 0.01699 0.01486 = 0.02011 -0.00301 -0.00144 -0.00286 C6 1 0.639109 0.801600 0.144285 11.00000 0.01586 0.01498 = 0.01860 -0.00228 -0.00132 -0.00387 C7 1 0.753379 0.716514 0.147069 11.00000 0.01395 0.01604 = 0.02254 -0.00294 0.00070 -0.00477 AFIX 43 H7 2 0.821628 0.744957 0.121491 11.00000 -1.20000 AFIX 0 C8 1 0.768864 0.595402 0.185107 11.00000 0.01365 0.01520 = 0.01962 -0.00140 -0.00121 -0.00332 C10 1 0.548869 0.633001 0.216159 11.00000 0.01415 0.01564 = 0.02638 -0.00261 0.00046 -0.00420 AFIX 43 H10 2 0.480083 0.604120 0.236262 11.00000 -1.20000 AFIX 0 C14 1 0.286564 0.773777 0.309970 11.00000 0.01675 0.02357 = 0.02333 -0.00569 -0.00116 -0.00544 AFIX 43 H14 2 0.335456 0.778084 0.353537 11.00000 -1.20000 AFIX 0 C9 1 0.662792 0.550569 0.223506 11.00000 0.01614 0.01500 = 0.02054 -0.00198 -0.00117 -0.00394 C13 1 0.319327 0.799882 0.212676 11.00000 0.01269 0.01355 = 0.02348 -0.00263 -0.00049 -0.00235 C11 1 0.535338 0.755596 0.180094 11.00000 0.01353 0.01668 = 0.01981 -0.00313 -0.00137 -0.00268 C15 1 0.181174 0.741189 0.343006 11.00000 0.02042 0.02789 = 0.02440 -0.00739 0.00311 -0.00819 AFIX 43 H15 2 0.157191 0.722034 0.409542 11.00000 -1.20000 AFIX 0 C17 1 0.145033 0.762038 0.180018 11.00000 0.01670 0.02149 = 0.02865 -0.00864 -0.00415 -0.00292 AFIX 43 H17 2 0.096326 0.757713 0.136321 11.00000 -1.20000 AFIX 0 C16 1 0.111413 0.737099 0.276994 11.00000 0.01362 0.02444 = 0.03221 -0.01069 0.00313 -0.00598 C19 1 0.987595 0.530848 0.146384 11.00000 0.01440 0.01365 = 0.02480 -0.00516 0.00059 -0.00306 C18 1 0.250800 0.793456 0.147349 11.00000 0.01857 0.01806 = 0.02205 -0.00427 -0.00095 -0.00248 AFIX 43 H18 2 0.275915 0.810354 0.080994 11.00000 -1.20000 AFIX 0 C20 1 1.089054 0.470154 0.197637 11.00000 0.01800 0.01677 = 0.02431 -0.00043 -0.00093 -0.00271 AFIX 43 H20 2 1.081257 0.423520 0.262039 11.00000 -1.20000 AFIX 0 C21 1 1.200928 0.477841 0.154752 11.00000 0.01484 0.01864 = 0.03377 -0.00048 -0.00209 -0.00054 AFIX 43 H21 2 1.269973 0.436789 0.189493 11.00000 -1.20000 AFIX 0 C22 1 1.211190 0.545744 0.061006 11.00000 0.01474 0.01664 = 0.03354 -0.00472 0.00561 -0.00276 C23 1 1.112330 0.605873 0.008734 11.00000 0.02296 0.01441 = 0.02259 -0.00356 0.00321 -0.00356 AFIX 43 H23 2 1.120964 0.651686 -0.055833 11.00000 -1.20000 AFIX 0 C24 1 1.000379 0.598461 0.051760 11.00000 0.01858 0.01563 = 0.02295 -0.00375 -0.00140 -0.00286 AFIX 43 H24 2 0.931801 0.639781 0.016497 11.00000 -1.20000 AFIX 0 C25 1 0.582349 0.376056 0.311392 11.00000 0.01654 0.01712 = 0.03584 0.00395 0.00146 -0.00489 AFIX 13 H25 2 0.517188 0.434256 0.339923 11.00000 -1.20000 AFIX 0 C26 1 0.531543 0.342645 0.237848 11.00000 0.03038 0.03510 = 0.04993 -0.00061 -0.00630 -0.01786 AFIX 137 H26A 2 0.498922 0.415734 0.187652 11.00000 -1.50000 H26B 2 0.467882 0.304633 0.269222 11.00000 -1.50000 H26C 2 0.595057 0.286019 0.209238 11.00000 -1.50000 AFIX 0 C27 1 0.633425 0.265355 0.390685 11.00000 0.02729 0.02701 = 0.04415 0.01230 -0.00210 -0.00887 AFIX 137 H27A 2 0.696242 0.207131 0.363096 11.00000 -1.50000 H27B 2 0.569822 0.228217 0.424034 11.00000 -1.50000 H27C 2 0.667233 0.289142 0.436192 11.00000 -1.50000 AFIX 0 C28 1 0.938593 0.250537 0.388222 11.00000 0.02140 0.01588 = 0.01926 -0.00231 -0.00067 -0.00378 C29 1 0.971303 0.120173 0.445093 11.00000 0.01795 0.01467 = 0.01799 -0.00213 0.00037 -0.00338 C30 1 1.030998 0.086285 0.527988 11.00000 0.02147 0.01758 = 0.01990 -0.00446 -0.00143 -0.00648 AFIX 43 H30 2 1.052091 0.145265 0.547257 11.00000 -1.20000 AFIX 0 C31 1 0.940235 0.033192 0.417491 11.00000 0.01905 0.01775 = 0.01837 -0.00242 -0.00268 -0.00370 AFIX 43 H31 2 0.899274 0.055737 0.361227 11.00000 -1.20000 AFIX 0 C32 1 0.921619 0.114842 0.154021 11.00000 0.01847 0.01698 = 0.02112 -0.00341 -0.00218 -0.00292 C33 1 0.963720 0.055869 0.074043 11.00000 0.01679 0.01537 = 0.01825 -0.00158 -0.00250 -0.00261 C34 1 0.895029 -0.009612 0.056555 11.00000 0.01497 0.01905 = 0.02049 -0.00255 0.00006 -0.00542 AFIX 43 H34 2 0.823201 -0.015822 0.095099 11.00000 -1.20000 AFIX 0 C35 1 1.069013 0.065786 0.016851 11.00000 0.01858 0.01613 = 0.02091 -0.00196 -0.00269 -0.00644 AFIX 43 H35 2 1.115769 0.110999 0.028368 11.00000 -1.20000 AFIX 0 H4 2 0.747038 0.385173 0.267425 11.00000 0.02843 H3 2 0.884876 0.445104 0.236851 11.00000 0.03547 H3B 2 0.969587 0.189329 0.225903 11.00000 0.05273 HKLF 4 REM lb0221_clz-trpta_100k_remo_a.res in P-1 REM R1 = 0.0440 for 9100 Fo > 4sig(Fo) and 0.0580 for all 11543 data REM 420 parameters refined using 0 restraints END WGHT 0.0514 0.3547 REM Highest difference peak 0.408, deepest hole -0.298, 1-sigma level 0.051 Q1 1 0.5169 1.0573 0.0963 11.00000 0.05 0.41 Q2 1 0.4665 0.9827 0.1249 11.00000 0.05 0.40 Q3 1 0.3577 1.0075 0.1465 11.00000 0.05 0.38 Q4 1 0.9511 0.0749 0.1145 11.00000 0.05 0.37 Q5 1 0.9654 0.1824 0.4177 11.00000 0.05 0.37 Q6 1 0.5860 0.7829 0.1671 11.00000 0.05 0.37 Q7 1 0.9817 0.1021 0.4978 11.00000 0.05 0.34 Q8 1 0.6993 0.7619 0.1514 11.00000 0.05 0.34 Q9 1 1.1604 0.5832 0.0381 11.00000 0.05 0.33 Q10 1 0.9963 0.5723 0.0995 11.00000 0.05 0.32 Q11 1 0.7580 0.6584 0.1672 11.00000 0.05 0.31 Q12 1 0.6348 0.8589 0.1262 11.00000 0.05 0.31 Q13 1 0.4214 0.8995 0.1550 11.00000 0.05 0.30 Q14 1 0.1599 0.7262 0.3071 11.00000 0.05 0.30 Q15 1 0.2827 0.7988 0.1807 11.00000 0.05 0.29 Q16 1 0.6035 0.5979 0.2192 11.00000 0.05 0.29 Q17 1 0.3487 1.1843 0.0869 11.00000 0.05 0.29 Q18 1 0.5398 0.6981 0.2107 11.00000 0.05 0.28 Q19 1 1.0226 0.0351 0.0526 11.00000 0.05 0.28 Q20 1 0.4807 0.7989 0.1812 11.00000 0.05 0.28 Q21 1 0.2015 0.7880 0.1679 11.00000 0.05 0.28 Q22 1 -0.0440 0.7620 0.3127 11.00000 0.05 0.28 Q23 1 0.7096 0.5806 0.2013 11.00000 0.05 0.28 Q24 1 0.9422 -0.0204 0.4536 11.00000 0.05 0.27 Q25 1 1.0355 0.5102 0.1740 11.00000 0.05 0.27 Q26 1 1.0020 0.0834 0.0363 11.00000 0.05 0.27 Q27 1 0.9437 0.0007 0.0777 11.00000 0.05 0.26 Q28 1 0.3159 1.1029 0.1391 11.00000 0.05 0.26 Q29 1 0.3647 0.8223 0.2021 11.00000 0.05 0.26 Q30 1 0.6123 0.3231 0.3414 11.00000 0.05 0.26 ; _shelx_res_checksum 45766 _shelx_hkl_file ; 0 0 -2 821.92 7.63 0 0 3 414.71 4.43 0 0 -3 414.68 6.69 0 0 4 2073.19 11.37 0 0 -4 2034.35 17.13 0 0 -5 1429.46 16.13 0 0 -6 1618.60 18.81 0 0 -7 340.00 9.36 0 0 -8 436.69 11.43 0 0 -9 1.61 1.15 0 0 -10 51.51 4.42 0 0 -11 28.29 3.60 0 0 -12 26.03 3.70 0 0 -13 119.03 8.04 0 0 14 16.79 3.26 0 0 -14 10.78 2.64 0 0 -15 35.45 4.99 0 0 15 33.01 4.81 0 0 -16 52.03 6.15 0 0 16 42.45 5.56 0 0 -17 3.64 2.01 0 0 17 1.25 1.67 0 0 18 0.89 2.03 0 0 -18 2.83 1.44 0 0 19 22.15 4.70 0 0 -19 16.03 4.12 0 0 20 5.89 2.82 0 0 -20 5.27 3.19 0 1 -20 18.33 4.19 0 -1 19 1.74 2.44 0 1 -19 2.26 2.19 0 1 -18 -0.80 1.35 0 -1 18 -0.45 1.59 0 1 -17 3.87 1.81 0 -1 17 2.28 2.17 0 -1 16 13.46 3.54 0 1 -16 9.04 2.50 0 -1 15 44.84 5.78 0 1 -15 39.71 5.25 0 1 -14 6.69 2.08 0 1 -13 5.61 2.08 0 1 -12 -0.81 1.02 0 1 -11 15.82 2.74 0 1 -10 222.14 9.52 0 1 -9 374.19 11.59 0 -1 9 332.41 7.28 0 1 -8 109.70 5.86 0 -1 8 106.14 3.92 0 -1 7 1481.14 13.88 0 1 -7 1498.35 20.18 0 -1 7 1543.04 20.33 0 -1 6 50.53 3.42 0 -1 6 47.30 2.42 0 1 -6 47.42 3.33 0 -1 5 127.90 5.04 0 -1 5 118.01 2.11 0 1 -5 121.17 4.87 0 -1 4 6298.63 31.49 0 -1 4 6290.39 16.15 0 1 -4 6383.83 31.46 0 1 -3 196.20 4.87 0 -1 3 208.33 3.00 0 1 -2 33.68 1.74 0 1 -2 31.71 1.19 0 -1 2 30.59 1.18 0 1 -1 940.90 6.53 0 1 -1 956.78 7.32 0 -1 -2 962.87 6.56 0 -1 -2 937.03 7.28 0 -1 -2 950.49 8.54 0 1 2 927.99 6.42 0 -1 -3 1463.62 7.99 0 1 3 1433.96 7.90 0 -1 -4 5052.72 26.72 0 -1 -4 4918.06 14.20 0 -1 -5 2911.35 10.48 0 -1 -5 3055.62 23.31 0 -1 -6 84.89 2.76 0 -1 -6 78.72 4.17 0 -1 -7 298.39 5.57 0 -1 -7 275.98 8.41 0 -1 -8 7.24 1.71 0 -1 -9 9.46 2.04 0 -1 -10 -0.53 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2 -3 48.38 2.10 0 -2 3 49.43 2.13 0 -2 2 6704.10 24.65 0 -2 2 6769.46 27.84 0 2 -2 6778.96 27.71 0 2 -1 3176.48 16.86 0 -2 1 3235.38 17.29 0 -2 1 3178.33 16.96 0 2 -1 3201.74 17.00 0 -2 0 36.57 1.84 0 2 0 34.85 1.79 0 -2 -1 1079.93 9.91 0 2 1 1074.32 9.96 0 2 2 467.13 6.52 0 2 2 446.00 5.07 0 -2 -2 469.00 5.18 0 -2 -2 468.22 6.99 0 -2 -3 1774.51 12.68 0 -2 -3 1831.90 15.17 0 -2 -3 1810.78 12.14 0 2 3 1799.91 12.76 0 2 3 1798.58 12.21 0 2 4 746.13 9.27 0 -2 -4 765.49 8.31 0 -2 -4 774.78 11.04 0 2 4 769.71 8.28 0 -2 -5 116.28 4.78 0 -2 -5 110.11 3.08 0 2 5 113.94 4.13 0 2 6 716.81 11.39 0 -2 -6 714.46 12.80 0 -2 -6 723.14 7.70 0 -2 -7 536.04 11.75 0 -2 -7 501.31 6.26 0 2 7 515.38 10.72 0 -2 -8 230.00 5.44 0 -2 -8 237.80 8.43 0 -2 -8 215.73 3.93 0 -2 -9 188.25 3.29 0 -2 -9 205.35 8.33 0 -2 -9 202.74 5.27 0 2 10 95.95 5.79 0 -2 -10 105.64 3.95 0 -2 -10 99.21 6.20 0 2 11 23.84 3.11 0 -2 -11 21.61 3.11 0 -2 -12 0.04 1.08 0 2 12 -1.40 1.25 0 -2 -13 63.88 5.87 0 2 13 64.50 5.70 0 -2 -14 13.93 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5 -12 3 5.91 1.82 5 -12 4 0.88 1.42 5 -12 4 9.55 3.22 5 -12 5 27.28 4.58 5 -12 6 19.21 4.24 5 -11 -16 0.70 1.80 5 -11 -15 10.71 3.25 5 -11 -14 -0.89 1.98 5 -11 -13 19.59 4.10 5 -11 -13 20.16 4.16 5 -11 -12 10.48 2.93 5 -11 -12 9.52 2.77 5 -11 -12 4.17 2.36 5 -11 -11 123.20 9.75 5 -11 -11 123.98 9.23 5 -11 -10 7.63 2.57 5 -11 -10 9.05 2.93 5 -11 -9 16.55 4.00 5 -11 -9 12.90 3.33 5 -11 -8 -0.46 1.65 5 -11 -8 2.89 1.38 5 -11 -7 21.55 3.65 5 -11 -7 23.34 4.31 5 -11 -6 6.25 2.46 5 -11 -6 6.55 2.37 5 -11 -5 21.72 4.09 5 -11 -5 20.48 3.55 5 -11 -4 40.57 5.11 5 -11 -4 34.34 5.22 5 -11 -3 3.54 2.03 5 -11 -3 0.47 0.98 5 -11 -2 3.72 2.13 5 -11 -2 2.72 1.16 5 -11 -1 40.88 5.64 5 -11 -1 40.71 4.80 5 -11 0 33.66 5.16 5 -11 0 42.52 5.07 5 -11 1 11.76 3.18 5 -11 1 15.88 3.15 5 -11 2 1.62 1.52 5 -11 2 -1.34 2.40 5 -11 3 21.93 4.28 5 -11 3 31.34 4.66 5 -11 4 -1.12 1.36 5 -11 4 1.98 2.38 5 -11 5 0.70 1.55 5 -11 5 1.71 1.59 5 -11 6 30.01 4.67 5 -11 6 28.29 4.73 5 -11 7 12.82 3.31 5 -11 8 5.39 1.79 5 -10 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15.61 3.19 5 -10 7 12.36 3.18 5 -10 8 41.14 5.28 5 -10 8 48.78 6.12 5 -10 8 42.66 5.62 5 -10 9 1.08 1.25 5 -10 9 -0.45 1.35 5 -10 10 30.22 4.96 5 -10 10 35.60 5.44 5 -10 11 60.67 7.30 5 -9 -17 8.24 2.64 5 -9 -16 1.70 1.53 5 -9 -15 88.60 8.52 5 -9 -14 29.13 5.09 5 -9 -14 31.68 4.56 5 -9 -13 154.99 9.89 5 -9 -13 171.88 11.09 5 -9 -12 208.16 11.75 5 -9 -12 208.39 12.22 5 -9 -12 195.73 11.19 5 -9 -11 -0.52 1.38 5 -9 -11 1.84 1.94 5 -9 -11 1.53 1.59 5 -9 -10 0.37 1.55 5 -9 -10 0.77 1.13 5 -9 -10 0.71 1.08 5 -9 -9 6.16 2.19 5 -9 -9 7.87 2.26 5 -9 -8 8.90 2.68 5 -9 -8 9.88 2.58 5 -9 -7 41.28 4.77 5 -9 -7 35.82 4.79 5 -9 -6 0.88 1.34 5 -9 -6 7.15 1.82 5 -9 -5 0.27 1.26 5 -9 -5 1.05 1.22 5 -9 -4 -0.30 1.18 5 -9 -4 1.85 1.46 5 -9 -3 28.53 3.62 5 -9 -3 30.92 4.48 5 -9 -2 3.22 1.95 5 -9 -2 8.79 2.25 5 -9 -1 2.84 1.83 5 -9 -1 3.35 1.60 5 -9 0 46.25 2.78 5 -9 0 41.56 5.14 5 -9 0 44.69 4.55 5 -9 1 19.02 3.09 5 -9 1 13.43 3.08 5 -9 1 15.60 1.97 5 -9 2 -0.94 0.84 5 -9 2 0.37 1.70 5 -9 2 -1.52 1.19 5 -9 3 0.96 1.08 5 -9 3 0.86 1.20 5 -9 3 1.42 1.08 5 -9 4 64.30 5.85 5 -9 4 73.10 6.78 5 -9 4 68.68 5.39 5 -9 5 1.11 1.37 5 -9 5 -1.07 1.75 5 -9 5 4.28 1.61 5 -9 6 2.88 1.61 5 -9 6 3.86 1.68 5 -9 6 0.31 1.00 5 -9 7 63.47 6.42 5 -9 7 69.87 6.72 5 -9 7 62.12 5.87 5 -9 8 74.81 7.08 5 -9 8 70.59 6.72 5 -9 8 64.42 6.48 5 -9 9 20.16 3.95 5 -9 9 10.59 2.90 5 -9 9 15.32 3.34 5 -9 10 -1.77 1.70 5 -9 10 1.30 1.11 5 -9 11 13.44 3.73 5 -9 11 23.94 4.42 5 -9 12 22.38 4.60 5 -9 12 21.36 4.31 5 -9 13 9.34 3.09 5 -8 -18 3.70 1.61 5 -8 -17 -0.46 2.42 5 -8 -16 3.25 1.85 5 -8 -15 9.45 3.12 5 -8 -14 5.36 2.60 5 -8 -14 2.54 1.68 5 -8 -13 3.07 1.61 5 -8 -13 6.12 2.51 5 -8 -12 56.94 5.73 5 -8 -12 49.42 5.63 5 -8 -11 -0.05 1.11 5 -8 -11 1.72 1.20 5 -8 -11 1.17 1.17 5 -8 -10 1.68 1.41 5 -8 -10 1.91 1.14 5 -8 -10 1.80 1.15 5 -8 -9 7.34 2.43 5 -8 -9 5.47 1.48 5 -8 -9 9.80 2.54 5 -8 -8 20.44 3.50 5 -8 -8 22.98 3.49 5 -8 -7 58.62 5.30 5 -8 -7 53.49 5.61 5 -8 -6 0.24 1.35 5 -8 -6 1.68 1.06 5 -8 -5 2.01 1.17 5 -8 -5 0.97 1.14 5 -8 -4 27.54 4.03 5 -8 -4 24.21 3.20 5 -8 -3 8.37 2.36 5 -8 -3 3.75 1.04 5 -8 -2 181.17 9.97 5 -8 -2 180.43 8.49 5 -8 -1 43.46 1.61 5 -8 -1 51.88 5.34 5 -8 -1 47.41 4.39 5 -8 0 0.35 1.01 5 -8 0 -0.77 1.31 5 -8 0 0.78 0.37 5 -8 1 19.80 3.49 5 -8 1 18.61 2.04 5 -8 1 22.83 3.11 5 -8 2 1.72 1.63 5 -8 2 0.15 0.58 5 -8 2 1.56 1.17 5 -8 3 5.51 1.99 5 -8 3 10.59 2.47 5 -8 3 6.84 1.73 5 -8 4 63.41 5.50 5 -8 4 56.37 4.63 5 -8 4 60.19 5.92 5 -8 5 16.18 3.14 5 -8 5 16.19 2.75 5 -8 5 14.83 2.82 5 -8 6 0.06 1.09 5 -8 6 0.33 1.06 5 -8 6 -1.46 1.30 5 -8 7 2.43 1.45 5 -8 7 2.05 1.65 5 -8 7 0.77 1.18 5 -8 8 30.26 4.18 5 -8 8 35.02 4.57 5 -8 8 33.63 4.42 5 -8 9 75.75 6.59 5 -8 9 86.77 7.55 5 -8 9 76.46 7.07 5 -8 10 44.22 5.59 5 -8 10 46.50 5.08 5 -8 10 41.53 5.69 5 -8 11 9.53 3.16 5 -8 11 6.16 2.50 5 -8 12 -1.52 2.27 5 -8 12 0.18 1.76 5 -8 13 3.03 2.01 5 -8 13 -0.64 1.28 5 -8 14 1.19 2.01 5 -7 -18 0.80 1.72 5 -7 -17 14.96 4.17 5 -7 -16 35.80 5.60 5 -7 -15 9.05 2.83 5 -7 -14 65.00 5.78 5 -7 -14 65.76 7.12 5 -7 -13 -0.22 1.00 5 -7 -13 -1.04 1.28 5 -7 -12 0.31 1.17 5 -7 -12 -1.16 1.69 5 -7 -11 7.79 2.19 5 -7 -11 3.20 1.39 5 -7 -10 1.00 1.26 5 -7 -10 4.99 2.00 5 -7 -10 5.49 2.03 5 -7 -9 15.18 2.92 5 -7 -9 13.45 2.65 5 -7 -9 13.99 2.70 5 -7 -8 12.55 2.48 5 -7 -8 16.38 2.94 5 -7 -8 16.35 2.65 5 -7 -7 6.36 2.11 5 -7 -7 7.36 2.08 5 -7 -6 327.77 11.55 5 -7 -6 326.99 12.74 5 -7 -5 157.02 7.73 5 -7 -5 136.08 8.16 5 -7 -4 33.53 3.49 5 -7 -4 29.90 3.89 5 -7 -3 20.03 2.77 -5 7 3 21.86 3.40 5 -7 -3 28.51 3.85 5 -7 -2 32.60 3.32 5 -7 -2 33.97 4.24 -5 7 2 32.43 4.10 5 -7 -1 11.38 1.63 -5 7 1 13.61 2.61 5 -7 -1 15.38 2.37 5 -7 -1 13.64 2.52 5 -7 -1 11.71 0.78 5 -7 0 10.66 1.21 5 -7 0 12.65 2.16 5 -7 0 9.15 2.15 5 -7 0 10.66 1.55 5 -7 1 52.98 4.36 5 -7 1 51.81 3.20 5 -7 1 47.01 3.21 5 -7 1 53.07 5.15 5 -7 2 35.64 3.02 5 -7 2 31.85 4.12 5 -7 2 30.97 2.60 5 -7 2 33.40 3.45 5 -7 3 266.32 8.90 5 -7 3 268.92 10.03 5 -7 3 257.16 11.37 5 -7 3 243.88 7.36 5 -7 4 180.02 8.45 5 -7 4 196.15 9.93 5 -7 4 193.27 8.19 5 -7 5 10.32 2.32 5 -7 5 8.20 1.98 5 -7 5 13.07 2.48 5 -7 6 48.04 5.02 5 -7 6 57.12 5.16 5 -7 6 50.11 4.83 5 -7 7 17.37 2.95 5 -7 7 18.54 3.20 5 -7 7 19.52 3.29 5 -7 8 -0.92 1.44 5 -7 8 0.82 1.00 5 -7 8 0.31 1.71 5 -7 9 63.26 6.05 5 -7 9 54.07 5.79 5 -7 9 62.44 5.73 5 -7 10 19.46 3.29 5 -7 10 17.09 3.56 5 -7 10 25.04 4.00 5 -7 11 3.98 2.31 5 -7 11 4.15 2.30 5 -7 12 1.90 1.89 5 -7 12 4.29 2.51 5 -7 13 3.56 1.88 5 -7 14 2.56 2.50 5 -6 -18 68.44 8.20 5 -6 -17 0.04 1.80 5 -6 -16 29.43 4.79 5 -6 -15 70.41 7.29 5 -6 -14 10.71 2.43 5 -6 -14 15.97 3.68 5 -6 -13 5.09 1.68 5 -6 -13 2.67 1.73 5 -6 -12 52.60 5.70 5 -6 -12 55.50 5.05 5 -6 -11 90.40 6.52 -5 6 11 87.32 4.02 5 -6 -11 86.05 6.98 -5 6 10 295.92 6.14 5 -6 -10 289.15 11.39 5 -6 -10 298.55 12.19 5 -6 -9 21.98 3.18 5 -6 -9 22.63 3.42 5 -6 -9 24.92 3.42 5 -6 -8 14.33 2.68 5 -6 -8 17.12 2.74 5 -6 -8 19.42 2.97 -5 6 7 20.26 3.01 5 -6 -7 20.04 3.08 5 -6 -7 21.36 2.94 5 -6 -7 17.99 2.68 5 -6 -6 187.17 8.28 -5 6 6 190.75 9.10 -5 6 5 43.43 4.31 5 -6 -5 43.47 3.91 -5 6 4 247.02 10.38 5 -6 -4 230.80 8.53 -5 6 3 26.27 3.50 5 -6 -3 25.32 2.86 5 -6 -2 26.65 2.81 -5 6 2 22.26 3.20 -5 6 1 49.33 4.76 5 -6 -1 47.59 3.67 -5 6 0 170.59 8.58 5 -6 0 156.24 4.39 5 -6 0 160.04 6.81 5 -6 0 147.45 5.13 5 -6 1 3.60 0.93 -5 6 -1 1.79 1.14 5 -6 1 3.31 1.15 5 -6 1 2.55 0.69 -5 6 -2 419.60 13.60 5 -6 2 410.55 11.07 5 -6 2 397.75 9.52 5 -6 2 394.65 8.14 -5 6 -3 41.56 4.37 5 -6 3 42.51 2.77 5 -6 3 42.98 3.72 5 -6 3 41.74 3.44 -5 6 -4 847.48 19.33 5 -6 4 874.87 17.30 5 -6 4 819.27 12.65 5 -6 4 877.92 16.73 5 -6 4 864.31 19.50 5 -6 5 155.98 7.57 5 -6 5 163.41 7.74 5 -6 5 139.01 5.53 5 -6 5 156.62 8.44 5 -6 6 33.01 3.64 5 -6 6 29.38 3.81 5 -6 6 30.73 3.51 5 -6 7 94.55 6.49 5 -6 7 98.68 6.76 5 -6 7 96.09 6.79 5 -6 8 186.23 9.44 5 -6 8 196.64 9.46 5 -6 8 190.79 10.05 -5 6 -9 112.84 6.25 5 -6 9 107.96 7.96 5 -6 9 109.50 7.04 -5 6 -10 148.72 7.57 5 -6 10 153.27 8.33 5 -6 10 155.38 9.96 -5 6 -11 40.38 4.19 5 -6 11 39.06 4.21 5 -6 11 49.67 5.98 5 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1.31 5 -5 0 15.44 1.45 -5 5 -1 1.51 0.96 5 -5 1 4.24 0.85 5 -5 1 3.55 0.74 5 -5 1 6.34 1.35 -5 5 -2 112.79 6.65 5 -5 2 111.76 3.73 5 -5 2 108.36 5.20 5 -5 2 115.43 4.90 5 -5 3 11.08 1.76 -5 5 -3 12.05 2.24 5 -5 3 10.49 1.74 5 -5 3 12.47 1.36 5 -5 4 57.32 4.09 -5 5 -4 50.55 4.55 5 -5 4 51.01 2.83 5 -5 4 57.40 4.16 -5 5 -5 343.95 11.65 5 -5 5 358.03 10.64 5 -5 5 327.78 7.80 5 -5 5 351.04 11.03 -5 5 -6 456.54 13.44 5 -5 6 459.44 12.74 5 -5 6 410.70 9.40 5 -5 6 446.74 13.20 5 -5 7 0.93 1.34 5 -5 7 3.49 1.51 5 -5 7 0.21 0.60 -5 5 -8 97.71 5.23 5 -5 8 96.38 6.88 5 -5 8 96.15 6.20 5 -5 9 209.01 9.19 5 -5 9 199.18 10.44 -5 5 -9 214.78 8.36 -5 5 -10 1.33 0.82 5 -5 10 0.78 1.28 5 -5 10 3.64 1.60 -5 5 -11 437.82 13.39 5 -5 11 419.39 12.81 5 -5 11 416.07 16.50 5 -5 12 269.44 13.94 -5 5 -12 296.61 11.60 -5 5 -13 16.06 2.84 5 -5 13 14.75 3.45 5 -5 14 13.61 3.56 5 -5 15 29.04 5.20 5 -5 16 -1.35 1.62 5 -4 -18 81.85 8.92 5 -4 -17 35.62 5.57 5 -4 -16 40.92 5.94 -5 4 16 43.27 4.92 -5 4 15 21.41 3.39 5 -4 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1.51 6 -9 8 -1.74 1.83 6 -9 9 5.77 2.36 6 -9 9 2.17 1.82 6 -9 9 6.94 2.46 6 -9 10 20.80 3.94 6 -9 11 12.41 3.47 6 -9 12 2.04 1.54 6 -8 -17 -2.26 2.83 6 -8 -16 1.85 2.16 6 -8 -15 30.60 5.34 6 -8 -14 21.32 3.72 6 -8 -14 19.78 3.97 6 -8 -13 130.16 9.70 6 -8 -13 114.70 8.45 6 -8 -12 39.84 5.26 6 -8 -12 35.89 4.77 6 -8 -11 54.74 5.87 6 -8 -11 46.21 5.42 6 -8 -10 57.93 5.95 6 -8 -10 62.54 5.94 6 -8 -10 60.65 6.27 6 -8 -9 88.01 7.05 6 -8 -9 86.16 7.33 6 -8 -9 94.46 6.93 6 -8 -8 281.31 12.21 6 -8 -8 299.24 11.79 6 -8 -8 275.54 12.93 6 -8 -7 42.69 5.27 6 -8 -7 38.12 4.43 6 -8 -7 48.06 4.56 6 -8 -6 43.44 4.56 6 -8 -6 36.75 4.75 6 -8 -5 13.76 3.01 6 -8 -5 11.53 2.31 6 -8 -4 126.52 7.22 6 -8 -4 135.51 8.95 6 -8 -3 21.52 3.09 6 -8 -3 25.74 4.01 6 -8 -2 4.75 2.29 6 -8 -2 4.68 1.58 6 -8 -1 2.96 1.29 6 -8 -1 3.15 1.49 6 -8 0 156.59 4.03 6 -8 0 170.67 10.10 6 -8 0 167.11 8.11 6 -8 1 3.07 0.83 6 -8 1 2.18 1.35 6 -8 2 28.22 4.31 6 -8 2 27.94 2.72 6 -8 2 25.93 3.39 6 -8 3 24.93 2.91 6 -8 3 23.54 4.02 6 -8 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6 -7 -4 11.22 2.42 6 -7 -4 16.92 2.54 -6 7 4 15.92 3.07 -6 7 3 71.97 6.16 6 -7 -3 69.77 4.93 -6 7 2 1.77 1.70 6 -7 -2 -0.64 1.28 6 -7 -1 39.20 3.62 -6 7 1 39.62 4.61 6 -7 -1 34.62 2.69 -6 7 0 28.47 3.89 6 -7 0 29.63 1.79 6 -7 0 27.23 2.28 6 -7 0 28.88 3.18 6 -7 1 5.15 1.36 -6 7 -1 6.47 2.22 6 -7 1 5.10 2.01 6 -7 1 4.20 0.91 -6 7 -2 32.04 4.20 6 -7 2 32.41 3.40 6 -7 2 32.86 2.84 6 -7 2 31.92 4.26 6 -7 3 1.20 0.96 6 -7 3 1.51 0.99 6 -7 3 0.22 1.00 6 -7 4 -0.19 1.00 6 -7 4 0.20 0.89 6 -7 4 -0.64 0.91 6 -7 5 13.44 2.43 6 -7 5 14.80 3.04 6 -7 5 16.20 2.83 6 -7 6 15.11 3.13 6 -7 6 17.50 2.88 6 -7 6 15.21 2.67 6 -7 7 11.12 2.62 6 -7 7 10.69 2.55 6 -7 7 11.20 2.34 6 -7 8 52.55 5.28 6 -7 8 50.93 5.34 6 -7 8 56.20 5.68 6 -7 9 20.56 3.71 6 -7 9 22.43 3.82 6 -7 9 24.19 3.83 6 -7 10 24.24 3.81 6 -7 10 20.74 3.96 6 -7 10 22.53 3.95 6 -7 11 -0.17 1.58 6 -7 11 -0.40 1.43 6 -7 12 2.01 1.56 6 -7 12 -0.47 1.58 6 -7 13 8.10 2.35 6 -7 13 9.73 2.96 6 -7 14 -3.99 3.31 6 -6 -18 6.41 2.66 6 -6 -17 2.53 2.25 6 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14.55 2.73 6 -6 4 9.34 1.84 6 -6 4 11.10 1.30 6 -6 4 13.06 2.18 -6 6 -5 25.48 3.70 6 -6 5 20.21 3.27 6 -6 5 24.41 3.13 6 -6 5 20.79 2.85 6 -6 6 16.97 2.98 6 -6 6 12.47 2.34 6 -6 6 15.39 2.48 6 -6 7 52.94 5.33 6 -6 7 60.95 5.15 6 -6 7 54.77 5.17 6 -6 8 60.51 5.34 6 -6 8 48.06 5.11 6 -6 8 59.96 5.64 6 -6 9 102.02 7.17 6 -6 9 82.25 7.05 6 -6 9 90.54 6.81 6 -6 10 208.34 10.79 6 -6 10 195.32 9.96 6 -6 10 180.95 10.87 6 -6 11 1.22 1.18 6 -6 11 -0.55 1.38 6 -6 11 1.47 1.96 6 -6 12 23.51 4.52 6 -6 13 3.18 1.97 6 -6 14 0.56 1.72 6 -6 15 5.96 2.85 6 -5 -18 49.74 7.00 6 -5 -17 4.73 2.65 6 -5 -16 41.03 6.01 6 -5 -15 107.09 9.18 6 -5 -14 6.94 2.01 6 -5 -13 -0.72 1.02 6 -5 -13 -1.71 2.12 6 -5 -12 39.94 4.96 6 -5 -12 44.35 4.55 6 -5 -11 28.14 3.68 6 -5 -11 34.06 4.37 -6 5 11 26.87 2.42 -6 5 10 9.30 2.27 6 -5 -10 13.30 2.64 -6 5 10 9.17 1.29 6 -5 -10 10.71 2.51 -6 5 9 36.26 4.14 -6 5 9 33.40 1.95 6 -5 -9 36.86 4.24 -6 5 8 3.41 1.66 6 -5 -8 2.79 1.09 -6 5 7 347.16 12.34 6 -5 -7 345.70 11.21 6 -5 -7 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326.77 11.07 -10 -7 -9 309.33 13.89 -10 -7 -10 3.74 1.44 -10 -7 -10 5.35 2.39 -10 -7 -11 11.24 2.67 -10 -7 -11 7.45 2.47 -10 -7 -11 9.54 2.08 10 7 12 130.10 9.65 -10 -7 -12 109.51 8.02 -10 -7 -12 110.44 8.72 10 7 13 9.28 3.21 -10 -7 -13 4.34 1.76 -10 -7 -13 8.27 3.06 10 7 14 2.91 2.18 -10 -7 -14 -1.42 1.86 -10 -7 -14 2.14 1.72 10 7 15 -3.07 2.36 -10 -7 -15 1.35 1.38 -10 -7 -15 -1.89 2.08 10 7 16 1.13 1.93 -10 -7 -16 6.82 2.43 -10 -7 -16 4.19 1.81 -10 -7 -17 1.23 1.47 -10 -7 -17 4.95 2.44 10 7 18 17.91 4.50 -10 -7 -18 14.55 3.29 10 8 -11 44.84 6.63 10 8 -10 13.38 3.93 10 8 -9 2.08 1.91 -10 -8 9 -0.38 1.24 10 8 -8 125.04 10.09 -10 -8 8 121.17 8.75 10 8 -7 46.24 5.98 -10 -8 7 40.60 5.16 10 8 -6 4.00 2.11 -10 -8 6 1.85 1.24 10 8 -5 4.09 2.66 -10 -8 5 0.77 1.35 -10 -8 4 108.45 8.03 -10 -8 3 -1.19 1.31 -10 -8 2 73.95 6.18 -10 -8 1 238.81 10.71 -10 -8 0 105.55 7.01 -10 -8 -1 0.76 0.92 -10 -8 -2 122.65 7.24 -10 -8 -3 94.54 6.16 -10 -8 -4 2.76 1.35 -10 -8 -5 54.46 4.61 -10 -8 -6 68.23 5.17 -10 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36.73 5.70 -11 7 5 7.95 3.06 -11 7 4 18.97 4.44 -11 7 3 6.82 2.59 -11 7 2 84.53 8.52 -11 7 1 11.38 3.45 -11 7 0 131.83 10.61 -11 7 -1 38.47 5.83 -11 7 -2 0.19 1.89 -11 7 -3 17.72 4.21 -11 7 -4 19.12 4.40 -11 7 -5 8.07 3.09 -11 7 -6 69.02 7.86 11 -7 6 64.98 7.69 11 -7 7 46.09 6.52 11 -7 8 33.02 5.60 11 -7 9 14.92 4.24 11 -6 -12 9.01 2.99 -11 6 11 -1.86 2.78 11 -6 -11 -2.57 2.51 -11 6 10 73.62 7.92 -11 6 9 119.38 9.90 -11 6 8 12.89 3.63 -11 6 7 15.89 3.71 -11 6 6 85.35 8.35 -11 6 5 2.33 1.94 -11 6 4 33.99 5.50 -11 6 3 62.04 7.04 -11 6 2 -1.18 1.61 -11 6 1 10.90 3.09 -11 6 0 9.50 3.05 -11 6 -1 18.46 4.04 -11 6 -2 39.86 5.69 -11 6 -3 252.44 14.15 -11 6 -4 1.89 1.57 -11 6 -5 0.75 1.33 -11 6 -6 64.64 7.39 -11 6 -7 39.91 6.03 -11 6 -8 8.87 3.00 -11 6 -9 -1.43 2.03 11 -6 9 -0.86 1.54 11 -6 10 39.54 5.80 -11 5 12 37.49 5.58 11 -5 -12 44.52 5.95 -11 5 11 -2.37 2.17 -11 5 10 5.73 2.53 -11 5 9 5.58 1.69 -11 5 8 4.40 2.19 -11 5 7 80.40 7.89 -11 5 6 9.74 2.95 -11 5 5 38.27 5.52 -11 5 4 48.63 6.10 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2 0.10 1.10 -11 -4 2 0.35 0.71 -11 -4 1 10.90 2.79 -11 -4 1 16.81 2.11 -11 -4 1 10.65 2.25 -11 -4 0 2.01 1.47 -11 -4 0 0.30 0.87 -11 -4 0 2.82 0.69 -11 -4 -1 90.24 7.23 -11 -4 -1 92.88 3.86 -11 -4 -2 278.78 5.73 -11 -4 -2 266.90 12.46 -11 -4 -2 277.08 11.65 -11 -4 -3 9.34 0.92 -11 -4 -3 8.96 2.56 -11 -4 -3 10.31 2.37 -11 -4 -4 48.69 5.41 -11 -4 -4 61.95 5.90 -11 -4 -5 3.55 1.64 -11 -4 -5 5.06 1.69 -11 -4 -6 205.19 10.92 -11 -4 -6 218.41 11.25 -11 -4 -7 153.37 9.47 -11 -4 -7 165.55 10.16 -11 -4 -8 17.76 3.46 -11 -4 -8 13.65 3.22 11 4 9 158.10 9.88 -11 -4 -9 149.91 9.31 11 4 10 -0.90 1.64 -11 -4 -10 -0.42 1.37 11 4 11 139.04 9.85 -11 -4 -11 128.44 8.67 -11 -4 -11 144.04 6.92 -11 -4 -12 71.03 6.55 11 4 12 65.27 6.99 11 4 13 1.66 1.95 -11 -4 -13 2.22 1.63 11 4 14 20.38 4.29 -11 -4 -14 21.72 3.57 11 4 15 7.75 3.25 11 4 16 10.64 3.08 11 4 17 2.36 2.34 11 5 -13 -1.34 1.64 11 5 -12 73.07 8.35 11 5 -11 7.17 2.84 11 5 -10 -9.30 3.02 -11 -5 9 138.93 9.02 11 5 -9 143.62 10.43 -11 -5 8 135.43 8.99 11 5 -8 156.14 10.50 11 5 -7 2.65 2.01 -11 -5 7 3.43 1.69 -11 -5 6 50.71 5.68 11 5 -6 48.85 5.52 11 5 -5 14.03 3.08 -11 -5 5 16.69 3.41 11 5 -4 45.50 4.84 -11 -5 4 40.91 5.05 -11 -5 4 51.07 4.68 -11 -5 4 42.00 4.03 -11 -5 3 1.02 1.35 -11 -5 3 0.16 1.01 -11 -5 3 0.27 0.94 -11 -5 2 99.67 7.78 -11 -5 2 96.26 6.48 -11 -5 2 104.65 5.98 -11 -5 1 -1.53 1.48 -11 -5 1 -0.68 0.85 -11 -5 1 2.34 1.03 -11 -5 0 69.58 6.44 -11 -5 0 63.50 5.44 -11 -5 0 71.87 4.43 -11 -5 -1 7.04 2.42 -11 -5 -1 9.52 2.40 -11 -5 -1 5.98 1.26 -11 -5 -2 323.70 13.77 -11 -5 -2 306.22 12.49 -11 -5 -2 317.98 8.20 -11 -5 -3 72.68 3.68 -11 -5 -3 74.25 6.68 -11 -5 -3 69.73 6.22 -11 -5 -4 21.75 1.97 -11 -5 -4 18.15 3.42 -11 -5 -4 21.98 3.68 -11 -5 -5 101.70 4.14 -11 -5 -5 100.33 7.68 -11 -5 -5 95.99 7.41 -11 -5 -6 -0.24 1.25 -11 -5 -6 -0.18 0.57 -11 -5 -6 1.02 1.32 -11 -5 -7 134.80 8.89 -11 -5 -7 131.92 9.03 -11 -5 -8 42.93 5.18 -11 -5 -8 57.53 6.13 -11 -5 -9 52.58 5.76 -11 -5 -9 53.56 6.02 11 5 10 176.26 10.76 -11 -5 -10 160.51 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4.12 -16 -9 -3 15.21 4.11 -16 -9 -4 2.68 1.94 -16 -9 -4 3.84 2.23 -16 -9 -5 27.80 5.55 -16 -9 -5 28.35 5.21 -16 -9 -6 9.97 3.91 -16 -9 -6 15.25 4.45 -16 -9 -7 -1.46 2.49 -16 -9 -7 0.21 1.74 -16 -9 -8 25.31 5.17 -16 -9 -8 14.83 4.17 -16 -9 -9 5.72 2.68 -16 -9 -9 4.93 2.76 -16 -9 -10 -1.02 2.02 -16 -10 -1 10.49 3.30 -16 -10 -2 90.41 9.01 -16 -10 -3 7.15 3.29 -16 -10 -3 3.16 2.60 -16 -10 -4 79.14 9.12 -16 -10 -4 79.67 8.69 -16 -10 -5 109.42 10.72 -16 -10 -5 80.57 8.90 -16 -10 -6 1.82 2.51 -16 -10 -6 -1.89 2.34 -16 -10 -7 4.50 3.06 -16 -10 -7 -0.13 2.09 -16 -10 -8 3.12 2.61 -16 -11 -1 8.40 3.64 -16 -11 -2 17.49 4.14 -16 -11 -3 7.56 2.67 -16 -11 -4 114.87 10.50 -16 -11 -5 24.10 4.84 -16 -11 -6 39.71 6.60 -16 -11 -7 4.30 2.46 -16 -12 -2 1.56 1.94 -16 -12 -3 8.22 3.21 -16 -12 -4 6.74 2.52 -17 -9 -4 8.98 2.37 -17 -9 -5 42.47 6.69 -17 -10 -2 22.84 4.70 -17 -10 -3 30.18 5.59 -17 -10 -4 1.20 2.07 0 0 0 0.00 0.00 TITL lb0221_CLZ-TRPTA_100K_reMo in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 11.799003 12.073640 14.680253 72.4717 80.6885 72.0304 ZERR 2.00 0.000440 0.000421 0.000498 0.0031 0.0030 0.0032 LATT 1 SFAC C H N O Cl UNIT 70.00 56.00 8.00 8.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 43677 _shelx_fab_file ; 2 0 0 -23.31 0.00 3 0 0 6.05 0.00 4 0 0 17.62 0.00 5 0 0 -20.46 0.00 6 0 0 15.90 0.00 7 0 0 -4.97 0.00 8 0 0 -1.73 0.00 9 0 0 1.26 0.00 10 0 0 -0.78 0.00 11 0 0 1.29 0.00 12 0 0 -1.36 0.00 13 0 0 0.53 0.00 14 0 0 -0.76 0.00 15 0 0 1.24 0.00 16 0 0 -1.10 0.00 -15 1 0 1.51 0.00 -14 1 0 -0.97 0.00 -13 1 0 0.19 0.00 -12 1 0 -0.72 0.00 -11 1 0 3.09 0.00 -10 1 0 -4.32 0.00 -9 1 0 2.68 0.00 -8 1 0 -1.15 0.00 -7 1 0 2.28 0.00 -6 1 0 2.73 0.00 -5 1 0 -10.69 0.00 -4 1 0 4.30 0.00 -3 1 0 2.58 0.00 -2 1 0 -3.29 0.00 -1 1 0 13.55 0.00 1 1 0 -92.41 0.00 2 1 0 44.90 0.00 3 1 0 18.67 0.00 4 1 0 -3.25 0.00 5 1 0 -24.37 0.00 6 1 0 24.39 0.00 7 1 0 -12.84 0.00 8 1 0 3.75 0.00 9 1 0 -0.96 0.00 10 1 0 1.96 0.00 11 1 0 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0.00 -4 7 20 0.14 0.00 -3 7 20 -0.33 0.00 -2 7 20 0.27 0.00 10 7 20 -0.35 0.00 -3 8 20 0.04 0.00 -2 8 20 -0.35 0.00 -1 8 20 -0.17 0.00 10 8 20 -0.37 0.00 -3 9 20 -0.11 0.00 -2 9 20 -0.03 0.00 -1 9 20 0.33 0.00 0 9 20 0.16 0.00 -2 10 20 0.12 0.00 -1 10 20 -0.06 0.00 0 10 20 0.01 0.00 1 10 20 0.12 0.00 2 10 20 -1.07 0.00 -1 11 20 -0.21 0.00 0 11 20 0.26 0.00 1 11 20 0.37 0.00 2 11 20 -0.92 0.00 3 11 20 1.00 0.00 1 12 20 -0.52 0.00 2 12 20 -0.26 0.00 3 12 20 0.73 0.00 4 12 20 -0.75 0.00 5 12 20 -0.65 0.00 6 12 20 0.94 0.00 7 12 20 0.84 0.00 8 12 20 -0.88 0.00 4 13 20 -0.10 0.00 5 13 20 0.31 0.00 6 13 20 0.43 0.00 0 -1 21 -0.24 0.00 1 -1 21 0.22 0.00 2 -1 21 0.20 0.00 -2 0 21 0.01 0.00 -1 0 21 -0.26 0.00 0 0 21 -0.53 0.00 1 0 21 0.33 0.00 2 0 21 -0.15 0.00 3 0 21 0.23 0.00 5 0 21 0.47 0.00 -3 1 21 0.65 0.00 -2 1 21 -1.13 0.00 -1 1 21 -0.51 0.00 0 1 21 0.04 0.00 1 1 21 1.57 0.00 2 1 21 -0.73 0.00 6 1 21 -0.48 0.00 -3 2 21 -1.06 0.00 7 2 21 0.35 0.00 -3 3 21 -0.72 0.00 7 3 21 0.35 0.00 8 3 21 -0.47 0.00 -3 4 21 -0.99 0.00 8 4 21 -0.27 0.00 -3 5 21 -0.44 0.00 -2 5 21 0.47 0.00 8 5 21 0.07 0.00 -3 6 21 -0.49 0.00 -2 6 21 0.72 0.00 -1 6 21 -0.48 0.00 9 6 21 0.17 0.00 -2 7 21 0.13 0.00 -1 7 21 0.07 0.00 0 7 21 0.18 0.00 9 7 21 -0.58 0.00 -2 8 21 0.68 0.00 -1 8 21 -0.10 0.00 0 8 21 -0.41 0.00 1 8 21 -0.19 0.00 9 8 21 -0.32 0.00 -1 9 21 -0.39 0.00 0 9 21 -0.14 0.00 1 9 21 -0.27 0.00 2 9 21 0.63 0.00 6 9 21 -0.67 0.00 7 9 21 -0.01 0.00 8 9 21 0.02 0.00 0 10 21 -0.05 0.00 1 10 21 0.02 0.00 2 10 21 0.68 0.00 3 10 21 -0.41 0.00 6 10 21 0.65 0.00 7 10 21 0.90 0.00 8 10 21 -0.09 0.00 2 11 21 0.32 0.00 3 11 21 -0.49 0.00 4 11 21 0.12 0.00 5 11 21 -0.55 0.00 6 11 21 1.56 0.00 7 11 21 -0.41 0.00 0 2 22 -1.28 0.00 1 2 22 0.55 0.00 2 2 22 0.82 0.00 3 2 22 -0.85 0.00 0 3 22 0.52 0.00 1 3 22 0.59 0.00 2 3 22 -0.01 0.00 3 3 22 -0.44 0.00 4 3 22 0.27 0.00 5 3 22 0.00 0.00 -1 4 22 0.29 0.00 0 4 22 0.15 0.00 1 4 22 0.06 0.00 2 4 22 -0.15 0.00 3 4 22 -0.49 0.00 4 4 22 0.48 0.00 5 4 22 -0.11 0.00 6 4 22 -0.33 0.00 -1 5 22 0.06 0.00 0 5 22 -0.13 0.00 1 5 22 0.66 0.00 2 5 22 -0.43 0.00 3 5 22 -0.04 0.00 4 5 22 0.24 0.00 5 5 22 -0.52 0.00 6 5 22 0.39 0.00 0 6 22 0.20 0.00 2 6 22 -0.79 0.00 3 6 22 0.37 0.00 4 6 22 0.00 0.00 5 6 22 -0.30 0.00 6 6 22 0.57 0.00 0 7 22 -0.01 0.00 1 7 22 0.27 0.00 3 7 22 0.41 0.00 4 7 22 -0.44 0.00 5 7 22 0.28 0.00 6 7 22 0.74 0.00 1 8 22 -0.06 0.00 2 8 22 -0.62 0.00 3 8 22 0.96 0.00 4 8 22 -0.27 0.00 5 8 22 0.44 0.00 6 8 22 -0.56 0.00 3 9 22 0.56 0.00 4 9 22 -1.38 0.00 5 9 22 0.36 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 91117) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.022 0.517 0.500 489 141 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 1 0 0 1.820 0 1 0 1.840 0 0 1 1.459 0 1 1 2.019 1 1 4 5.624 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL lb0221_CLZP -1ta_100k_rR = 0.18 CELL 11.7990 12.0736 14.6803 72.47 80.69 72.03 SPGR P-1 # Solvent Accessible Volume = 489 # Electrons Found in S.A.V. = 141 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.518 0.849 0.359 ! 11.04 eA-3 C102 0.478 0.025 0.376 ! 9.66 eA-3 C103 0.672 0.929 0.341 ! 8.15 eA-3 C104 0.348 0.049 0.392 ! 7.73 eA-3 C105 0.548 0.925 0.364 ! 7.64 eA-3 C106 0.287 0.175 0.381 ! 6.59 eA-3 C107 0.782 0.560 0.417 ! 6.08 eA-3 C108 0.621 0.839 0.372 ! 3.25 eA-3 C109 0.672 0.548 0.472 ! 2.97 eA-3 C110 0.712 0.748 0.420 ! 2.93 eA-3 C111 0.173 0.430 0.480 ! 2.58 eA-3 C112 0.731 0.593 0.471 ! 2.43 eA-3 C113 0.558 0.558 0.473 ! 2.41 eA-3 C114 0.161 0.369 0.438 ! 2.23 eA-3 C115 0.298 0.235 0.455 ! 2.00 eA-3 C116 0.222 0.241 0.330 ! 1.72 eA-3 C117 0.234 0.358 0.457 ! 1.56 eA-3 C118 0.643 0.642 0.452 ! 1.33 eA-3 C119 0.278 0.456 0.461 ! 1.28 eA-3 C120 0.333 0.009 0.456 ! 1.21 eA-3 C121 0.283 0.243 0.310 ! 1.05 eA-3 C122 0.423 0.996 0.428 ! 1.00 eA-3 C123 0.310 0.386 0.360 ! 0.84 eA-3 C124 0.341 0.475 0.470 ! 0.72 eA-3 Q125 0.364 0.994 0.160 ! 0.70 eA-3 C126 0.526 0.672 0.434 ! 0.67 eA-3 Q127 0.516 0.064 0.100 ! 0.66 eA-3 Q128 0.171 0.581 0.030 ! 0.64 eA-3 Q129 0.957 0.753 0.321 ! 0.64 eA-3 Q130 0.909 0.976 0.016 ! 0.63 eA-3 Q131 0.762 0.673 0.150 ! 0.60 eA-3 Q132 0.742 0.967 0.324 ! 0.59 eA-3 Q133 0.952 0.206 0.404 ! 0.58 eA-3 Q134 0.470 0.811 0.186 ! 0.58 eA-3 Q135 0.600 0.594 0.224 ! 0.57 eA-3 Q136 0.707 0.754 0.147 ! 0.57 eA-3 Q137 0.638 0.863 0.124 ! 0.57 eA-3 Q138 0.283 0.800 0.172 ! 0.56 eA-3 Q139 0.575 0.777 0.164 ! 0.56 eA-3 Q140 0.606 0.939 0.096 ! 0.55 eA-3 Q141 0.950 0.069 0.434 ! 0.55 eA-3 C142 0.642 0.797 0.438 ! 0.55 eA-3 Q143 0.013 0.687 0.308 ! 0.55 eA-3 Q144 0.905 0.303 0.282 ! 0.54 eA-3 Q145 0.337 0.187 0.087 ! 0.53 eA-3 Q146 0.953 0.979 0.433 ! 0.53 eA-3 Q147 0.423 0.894 0.160 ! 0.53 eA-3 Q148 0.061 0.612 0.030 ! 0.53 eA-3 Q149 0.207 0.499 0.114 ! 0.52 eA-3 Q150 0.516 0.993 0.299 ! 0.52 eA-3 Q151 0.939 0.103 0.107 ! 0.52 eA-3 Q152 0.156 0.488 0.173 ! 0.52 eA-3 Q153 0.468 0.158 0.084 ! 0.52 eA-3 Q154 0.192 0.507 0.417 ! 0.52 eA-3 Q155 0.480 0.989 0.114 ! 0.51 eA-3 Q156 0.344 0.560 0.048 ! 0.51 eA-3 Q157 0.996 0.552 0.111 ! 0.50 eA-3 Q158 0.314 0.565 0.017 ! 0.50 eA-3 Q159 0.154 0.717 0.319 ! 0.50 eA-3 ) ; _shelx_fab_checksum 88917 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 Cl1 Cl -0.02201(3) 0.69984(4) 0.31761(3) 0.03712(10) Uani 1 1 d . . N1 N 0.42663(8) 0.83916(9) 0.17739(7) 0.0171(2) Uani 1 1 d . . O2 O 0.93349(10) 0.32936(9) 0.42744(7) 0.0345(2) Uani 1 1 d . . C12 C 0.41613(10) 0.96169(11) 0.14635(8) 0.0177(2) Uani 1 1 d . . N2 N 0.63176(9) 0.91784(9) 0.11198(7) 0.0185(2) Uani 1 1 d . . O1 O 0.91588(7) 0.27322(8) 0.30078(6) 0.02007(18) Uani 1 1 d . . Cl2 Cl 1.35123(3) 0.55850(3) 0.00749(3) 0.03562(10) Uani 1 1 d . . C1 C 0.30515(10) 1.04931(11) 0.14859(9) 0.0208(2) Uani 1 1 d . . H1 H 0.233955 1.025325 0.171479 0.025 Uiso 1 1 calc R U C2 C 0.30093(11) 1.16933(12) 0.11746(9) 0.0234(3) Uani 1 1 d . . H2 H 0.225922 1.228185 0.118495 0.028 Uiso 1 1 calc R U O1A O 1.00383(8) 0.15272(8) 0.17821(6) 0.02108(18) Uani 1 1 d . . N3 N 0.87829(9) 0.51148(10) 0.19133(8) 0.0193(2) Uani 1 1 d . . C3 C 0.40467(12) 1.20757(12) 0.08405(9) 0.0246(3) Uani 1 1 d . . H3A H 0.399521 1.291346 0.062445 0.030 Uiso 1 1 calc R U O2A O 0.82117(8) 0.12706(10) 0.19268(7) 0.0286(2) Uani 1 1 d . . N4 N 0.67811(9) 0.43347(10) 0.26532(8) 0.0208(2) Uani 1 1 d . . C4 C 0.51363(11) 1.12331(11) 0.08275(9) 0.0221(2) Uani 1 1 d . . H4A H 0.584011 1.149090 0.060939 0.027 Uiso 1 1 calc R U C5 C 0.52190(10) 0.99841(11) 0.11362(8) 0.0181(2) Uani 1 1 d . . C6 C 0.63911(10) 0.80160(11) 0.14428(8) 0.0171(2) Uani 1 1 d . . C7 C 0.75338(10) 0.71651(11) 0.14707(9) 0.0181(2) Uani 1 1 d . . H7 H 0.821628 0.744957 0.121491 0.022 Uiso 1 1 calc R U C8 C 0.76886(10) 0.59540(11) 0.18511(8) 0.0171(2) Uani 1 1 d . . C10 C 0.54887(10) 0.63300(11) 0.21616(9) 0.0196(2) Uani 1 1 d . . H10 H 0.480083 0.604120 0.236262 0.024 Uiso 1 1 calc R U C14 C 0.28656(11) 0.77378(12) 0.30997(9) 0.0214(2) Uani 1 1 d . . H14 H 0.335456 0.778084 0.353537 0.026 Uiso 1 1 calc R U C9 C 0.66279(10) 0.55057(11) 0.22351(8) 0.0180(2) Uani 1 1 d . . C13 C 0.31933(10) 0.79988(11) 0.21268(9) 0.0175(2) Uani 1 1 d . . C11 C 0.53534(10) 0.75560(11) 0.18009(8) 0.0174(2) Uani 1 1 d . . C15 C 0.18117(11) 0.74119(13) 0.34301(9) 0.0244(3) Uani 1 1 d . . H15 H 0.157191 0.722034 0.409542 0.029 Uiso 1 1 calc R U C17 C 0.14503(11) 0.76204(12) 0.18002(9) 0.0221(3) Uani 1 1 d . . H17 H 0.096326 0.757713 0.136321 0.027 Uiso 1 1 calc R U C16 C 0.11141(10) 0.73710(12) 0.27699(10) 0.0231(3) Uani 1 1 d . . C19 C 0.98759(10) 0.53085(11) 0.14638(9) 0.0181(2) Uani 1 1 d . . C18 C 0.25080(11) 0.79346(11) 0.14735(9) 0.0205(2) Uani 1 1 d . . H18 H 0.275915 0.810354 0.080994 0.025 Uiso 1 1 calc R U C20 C 1.08905(11) 0.47015(12) 0.19764(9) 0.0214(2) Uani 1 1 d . . H20 H 1.081257 0.423520 0.262039 0.026 Uiso 1 1 calc R U C21 C 1.20093(11) 0.47784(12) 0.15475(10) 0.0249(3) Uani 1 1 d . . H21 H 1.269973 0.436789 0.189493 0.030 Uiso 1 1 calc R U C22 C 1.21119(10) 0.54574(12) 0.06101(10) 0.0234(3) Uani 1 1 d . . C23 C 1.11233(11) 0.60587(11) 0.00873(9) 0.0213(2) Uani 1 1 d . . H23 H 1.120964 0.651686 -0.055833 0.026 Uiso 1 1 calc R U C24 C 1.00038(11) 0.59846(11) 0.05176(9) 0.0198(2) Uani 1 1 d . . H24 H 0.931801 0.639781 0.016497 0.024 Uiso 1 1 calc R U C25 C 0.58235(11) 0.37606(12) 0.31139(10) 0.0261(3) Uani 1 1 d . . H25 H 0.517188 0.434256 0.339923 0.031 Uiso 1 1 calc R U C26 C 0.53154(14) 0.34265(15) 0.23785(12) 0.0385(4) Uani 1 1 d . . H26A H 0.498922 0.415734 0.187652 0.058 Uiso 1 1 calc R U H26B H 0.467882 0.304633 0.269222 0.058 Uiso 1 1 calc R U H26C H 0.595057 0.286019 0.209238 0.058 Uiso 1 1 calc R U C27 C 0.63342(13) 0.26535(14) 0.39069(12) 0.0376(4) Uani 1 1 d . . H27A H 0.696242 0.207131 0.363096 0.056 Uiso 1 1 calc R U H27B H 0.569822 0.228217 0.424034 0.056 Uiso 1 1 calc R U H27C H 0.667233 0.289142 0.436192 0.056 Uiso 1 1 calc R U C28 C 0.93859(11) 0.25054(11) 0.38822(9) 0.0198(2) Uani 1 1 d . . C29 C 0.97130(10) 0.12017(11) 0.44509(8) 0.0179(2) Uani 1 1 d . . C30 C 1.03100(11) 0.08628(11) 0.52799(9) 0.0195(2) Uani 1 1 d . . H30 H 1.052091 0.145265 0.547257 0.023 Uiso 1 1 calc R U C31 C 0.94024(10) 0.03319(11) 0.41749(8) 0.0191(2) Uani 1 1 d . . H31 H 0.899274 0.055737 0.361227 0.023 Uiso 1 1 calc R U C32 C 0.92162(11) 0.11484(11) 0.15402(9) 0.0196(2) Uani 1 1 d . . C33 C 0.96372(10) 0.05587(11) 0.07404(8) 0.0178(2) Uani 1 1 d . . C34 C 0.89503(10) -0.00961(11) 0.05655(8) 0.0188(2) Uani 1 1 d . . H34 H 0.823201 -0.015822 0.095099 0.023 Uiso 1 1 calc R U C35 C 1.06901(10) 0.06579(11) 0.01685(8) 0.0187(2) Uani 1 1 d . . H35 H 1.115769 0.110999 0.028368 0.022 Uiso 1 1 calc R U H4 H 0.7470(15) 0.3852(15) 0.2674(11) 0.028(4) Uiso 1 1 d . . H3 H 0.8849(14) 0.4451(16) 0.2369(12) 0.035(5) Uiso 1 1 d . . H3B H 0.9696(17) 0.1893(19) 0.2259(14) 0.053(6) Uiso 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.02217(17) 0.0564(3) 0.0442(2) -0.02555(19) 0.01047(13) -0.02169(16) N1 0.0133(4) 0.0143(5) 0.0208(5) -0.0022(4) -0.0003(3) -0.0028(4) O2 0.0625(7) 0.0159(5) 0.0247(5) -0.0047(4) -0.0074(5) -0.0089(5) C12 0.0172(5) 0.0141(6) 0.0198(5) -0.0028(4) -0.0013(4) -0.0032(4) N2 0.0164(5) 0.0146(5) 0.0222(5) -0.0031(4) -0.0002(4) -0.0034(4) O1 0.0225(4) 0.0146(4) 0.0188(4) -0.0010(3) -0.0026(3) -0.0020(3) Cl2 0.01732(15) 0.02804(19) 0.0491(2) -0.00075(15) 0.01013(13) -0.00443(12) C1 0.0159(5) 0.0178(6) 0.0255(6) -0.0045(5) -0.0019(4) -0.0014(4) C2 0.0198(6) 0.0175(6) 0.0286(7) -0.0055(5) -0.0023(5) 0.0007(5) O1A 0.0200(4) 0.0226(5) 0.0220(4) -0.0085(4) -0.0007(3) -0.0059(3) N3 0.0136(5) 0.0144(5) 0.0237(5) 0.0014(4) -0.0003(4) -0.0021(4) C3 0.0264(6) 0.0147(6) 0.0290(7) -0.0034(5) -0.0024(5) -0.0026(5) O2A 0.0203(5) 0.0371(6) 0.0320(5) -0.0168(4) 0.0048(4) -0.0089(4) N4 0.0140(5) 0.0144(5) 0.0282(6) 0.0007(4) -0.0002(4) -0.0024(4) C4 0.0226(6) 0.0159(6) 0.0263(6) -0.0037(5) 0.0012(5) -0.0066(5) C5 0.0170(5) 0.0149(6) 0.0201(6) -0.0030(4) -0.0014(4) -0.0029(4) C6 0.0159(5) 0.0150(5) 0.0186(5) -0.0023(4) -0.0013(4) -0.0039(4) C7 0.0139(5) 0.0160(6) 0.0225(6) -0.0029(5) 0.0007(4) -0.0048(4) C8 0.0137(5) 0.0152(6) 0.0196(5) -0.0014(4) -0.0012(4) -0.0033(4) C10 0.0141(5) 0.0156(6) 0.0264(6) -0.0026(5) 0.0005(4) -0.0042(4) C14 0.0168(6) 0.0236(6) 0.0233(6) -0.0057(5) -0.0012(4) -0.0054(5) C9 0.0161(5) 0.0150(6) 0.0205(6) -0.0020(4) -0.0012(4) -0.0039(4) C13 0.0127(5) 0.0136(5) 0.0235(6) -0.0026(4) -0.0005(4) -0.0023(4) C11 0.0135(5) 0.0167(6) 0.0198(5) -0.0031(4) -0.0014(4) -0.0027(4) C15 0.0204(6) 0.0279(7) 0.0244(6) -0.0074(5) 0.0031(5) -0.0082(5) C17 0.0167(6) 0.0215(6) 0.0287(6) -0.0086(5) -0.0041(4) -0.0029(5) C16 0.0136(5) 0.0244(7) 0.0322(7) -0.0107(5) 0.0031(4) -0.0060(5) C19 0.0144(5) 0.0137(5) 0.0248(6) -0.0052(5) 0.0006(4) -0.0031(4) C18 0.0186(6) 0.0181(6) 0.0220(6) -0.0043(5) -0.0010(4) -0.0025(4) C20 0.0180(6) 0.0168(6) 0.0243(6) -0.0004(5) -0.0009(4) -0.0027(4) C21 0.0148(6) 0.0186(6) 0.0338(7) -0.0005(5) -0.0021(5) -0.0005(4) C22 0.0147(5) 0.0166(6) 0.0335(7) -0.0047(5) 0.0056(5) -0.0028(4) C23 0.0230(6) 0.0144(6) 0.0226(6) -0.0036(5) 0.0032(4) -0.0036(4) C24 0.0186(6) 0.0156(6) 0.0230(6) -0.0038(5) -0.0014(4) -0.0029(4) C25 0.0165(6) 0.0171(6) 0.0358(7) 0.0040(5) 0.0015(5) -0.0049(5) C26 0.0304(8) 0.0351(9) 0.0499(10) -0.0006(7) -0.0063(6) -0.0179(6) C27 0.0273(7) 0.0270(8) 0.0441(9) 0.0123(6) -0.0021(6) -0.0089(6) C28 0.0214(6) 0.0159(6) 0.0193(6) -0.0023(5) -0.0007(4) -0.0038(4) C29 0.0179(5) 0.0147(6) 0.0180(5) -0.0021(4) 0.0004(4) -0.0034(4) C30 0.0215(6) 0.0176(6) 0.0199(6) -0.0045(5) -0.0014(4) -0.0065(4) C31 0.0190(6) 0.0177(6) 0.0184(5) -0.0024(5) -0.0027(4) -0.0037(4) C32 0.0185(6) 0.0170(6) 0.0211(6) -0.0034(5) -0.0022(4) -0.0029(4) C33 0.0168(5) 0.0154(6) 0.0182(5) -0.0016(4) -0.0025(4) -0.0026(4) C34 0.0150(5) 0.0191(6) 0.0205(6) -0.0026(5) 0.0001(4) -0.0054(4) C35 0.0186(6) 0.0161(6) 0.0209(6) -0.0020(4) -0.0027(4) -0.0064(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 C11 N1 C12 121.51(10) . C11 N1 C13 119.76(10) . C12 N1 C13 118.64(9) . N1 C12 C1 122.24(11) . N1 C12 C5 117.90(10) . C1 C12 C5 119.85(11) . C6 N2 C5 118.23(10) . C2 C1 C12 119.37(12) . C2 C1 H1 120.3 . C12 C1 H1 120.3 . C1 C2 C3 121.64(11) . C1 C2 H2 119.2 . C3 C2 H2 119.2 . C32 O1A H3B 107.5(13) . C8 N3 C19 126.60(10) . C8 N3 H3 117.3(11) . C19 N3 H3 114.5(11) . C4 C3 C2 119.68(12) . C4 C3 H3A 120.2 . C2 C3 H3A 120.2 . C9 N4 C25 125.53(10) . C9 N4 H4 120.3(12) . C25 N4 H4 114.1(12) . C3 C4 C5 120.51(12) . C3 C4 H4A 119.7 . C5 C4 H4A 119.7 . N2 C5 C4 118.64(11) . N2 C5 C12 122.41(11) . C4 C5 C12 118.95(11) . N2 C6 C7 118.99(11) . N2 C6 C11 123.15(10) . C7 C6 C11 117.84(11) . C8 C7 C6 122.43(11) . C8 C7 H7 118.8 . C6 C7 H7 118.8 . C7 C8 N3 123.74(11) . C7 C8 C9 118.97(10) . N3 C8 C9 117.28(11) . C11 C10 C9 120.87(11) . C11 C10 H10 119.6 . C9 C10 H10 119.6 . C13 C14 C15 119.03(11) . C13 C14 H14 120.5 . C15 C14 H14 120.5 . N4 C9 C10 121.80(11) . N4 C9 C8 119.05(10) . C10 C9 C8 119.14(11) . C18 C13 C14 121.99(11) . C18 C13 N1 118.75(11) . C14 C13 N1 119.22(11) . N1 C11 C10 122.67(11) . N1 C11 C6 116.74(11) . C10 C11 C6 120.58(10) . C14 C15 C16 118.81(12) . C14 C15 H15 120.6 . C16 C15 H15 120.6 . C16 C17 C18 119.07(12) . C16 C17 H17 120.5 . C18 C17 H17 120.5 . C17 C16 C15 121.98(12) . C17 C16 Cl1 119.02(10) . C15 C16 Cl1 119.00(10) . C24 C19 C20 119.32(11) . C24 C19 N3 123.19(10) . C20 C19 N3 117.25(11) . C13 C18 C17 119.10(11) . C13 C18 H18 120.5 . C17 C18 H18 120.5 . C21 C20 C19 120.17(12) . C21 C20 H20 119.9 . C19 C20 H20 119.9 . C22 C21 C20 119.40(11) . C22 C21 H21 120.3 . C20 C21 H21 120.3 . C23 C22 C21 121.48(11) . C23 C22 Cl2 118.88(10) . C21 C22 Cl2 119.63(10) . C22 C23 C24 119.10(11) . C22 C23 H23 120.4 . C24 C23 H23 120.4 . C23 C24 C19 120.53(11) . C23 C24 H24 119.7 . C19 C24 H24 119.7 . N4 C25 C27 108.49(11) . N4 C25 C26 110.14(11) . C27 C25 C26 111.17(13) . N4 C25 H25 109.0 . C27 C25 H25 109.0 . C26 C25 H25 109.0 . C25 C26 H26A 109.5 . C25 C26 H26B 109.5 . H26A C26 H26B 109.5 . C25 C26 H26C 109.5 . H26A C26 H26C 109.5 . H26B C26 H26C 109.5 . C25 C27 H27A 109.5 . C25 C27 H27B 109.5 . H27A C27 H27B 109.5 . C25 C27 H27C 109.5 . H27A C27 H27C 109.5 . H27B C27 H27C 109.5 . O2 C28 O1 123.67(12) . O2 C28 C29 119.13(11) . O1 C28 C29 117.19(11) . C31 C29 C30 119.49(11) . C31 C29 C28 120.99(11) . C30 C29 C28 119.50(11) . C31 C30 C29 120.34(12) 2_756 C31 C30 H30 119.8 2_756 C29 C30 H30 119.8 . C30 C31 C29 120.17(11) 2_756 C30 C31 H31 119.9 2_756 C29 C31 H31 119.9 . O2A C32 O1A 123.51(12) . O2A C32 C33 122.74(12) . O1A C32 C33 113.74(10) . C34 C33 C35 119.92(11) . C34 C33 C32 118.38(11) . C35 C33 C32 121.70(11) . C35 C34 C33 120.20(11) 2_755 C35 C34 H34 119.9 2_755 C33 C34 H34 119.9 . C34 C35 C33 119.89(11) 2_755 C34 C35 H35 120.1 2_755 C33 C35 H35 120.1 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cl1 C16 1.7343(13) . N1 C11 1.3633(14) . N1 C12 1.3823(15) . N1 C13 1.4514(15) . O2 C28 1.2346(16) . C12 C1 1.4097(16) . C12 C5 1.4155(17) . N2 C6 1.3189(16) . N2 C5 1.3613(14) . O1 C28 1.2841(14) . Cl2 C22 1.7422(13) . C1 C2 1.3694(18) . C1 H1 0.9500 . C2 C3 1.4035(19) . C2 H2 0.9500 . O1A C32 1.3263(15) . O1A H3B 0.91(2) . N3 C8 1.3701(14) . N3 C19 1.4040(15) . N3 H3 0.866(18) . C3 C4 1.3728(17) . C3 H3A 0.9500 . O2A C32 1.2138(15) . N4 C9 1.3281(16) . N4 C25 1.4725(16) . N4 H4 0.841(16) . C4 C5 1.4145(17) . C4 H4A 0.9500 . C6 C7 1.4187(16) . C6 C11 1.4558(16) . C7 C8 1.3637(17) . C7 H7 0.9500 . C8 C9 1.4775(16) . C10 C11 1.3806(17) . C10 C9 1.4021(16) . C10 H10 0.9500 . C14 C13 1.3835(17) . C14 C15 1.3886(17) . C14 H14 0.9500 . C13 C18 1.3835(17) . C15 C16 1.3896(18) . C15 H15 0.9500 . C17 C16 1.3811(18) . C17 C18 1.3857(17) . C17 H17 0.9500 . C19 C24 1.3942(17) . C19 C20 1.3980(16) . C18 H18 0.9500 . C20 C21 1.3852(17) . C20 H20 0.9500 . C21 C22 1.3815(19) . C21 H21 0.9500 . C22 C23 1.3813(18) . C23 C24 1.3859(17) . C23 H23 0.9500 . C24 H24 0.9500 . C25 C27 1.5157(18) . C25 C26 1.519(2) . C25 H25 1.0000 . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C28 C29 1.5037(17) . C29 C31 1.3940(17) . C29 C30 1.3943(16) . C30 C31 1.3882(17) 2_756 C30 H30 0.9500 . C31 H31 0.9500 . C32 C33 1.4929(17) . C33 C34 1.3903(17) . C33 C35 1.3987(16) . C34 C35 1.3842(17) 2_755 C34 H34 0.9500 . C35 H35 0.9500 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C15 H15 O2 0.95 2.44 3.3792(17) 170.8 2_666 N4 H4 O1 0.841(16) 2.071(16) 2.8985(13) 167.7(15) . N3 H3 O1 0.866(18) 1.947(18) 2.7772(14) 160.1(16) . O1A H3B O1 0.91(2) 1.64(2) 2.5442(13) 171(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_4 C11 N1 C12 C1 -176.05(11) . C13 N1 C12 C1 0.52(17) . C11 N1 C12 C5 2.43(17) . C13 N1 C12 C5 179.00(10) . N1 C12 C1 C2 179.51(11) . C5 C12 C1 C2 1.06(18) . C12 C1 C2 C3 -0.58(19) . C1 C2 C3 C4 -0.4(2) . C2 C3 C4 C5 0.82(19) . C6 N2 C5 C4 177.48(11) . C6 N2 C5 C12 -1.59(17) . C3 C4 C5 N2 -179.43(11) . C3 C4 C5 C12 -0.33(18) . N1 C12 C5 N2 -0.07(17) . C1 C12 C5 N2 178.45(11) . N1 C12 C5 C4 -179.13(11) . C1 C12 C5 C4 -0.62(17) . C5 N2 C6 C7 -177.23(10) . C5 N2 C6 C11 1.00(17) . N2 C6 C7 C8 175.72(12) . C11 C6 C7 C8 -2.60(18) . C6 C7 C8 N3 -178.02(11) . C6 C7 C8 C9 1.01(18) . C19 N3 C8 C7 -12.0(2) . C19 N3 C8 C9 168.99(11) . C25 N4 C9 C10 -2.4(2) . C25 N4 C9 C8 176.60(12) . C11 C10 C9 N4 174.24(12) . C11 C10 C9 C8 -4.75(18) . C7 C8 C9 N4 -176.34(12) . N3 C8 C9 N4 2.75(17) . C7 C8 C9 C10 2.68(17) . N3 C8 C9 C10 -178.23(11) . C15 C14 C13 C18 -0.59(19) . C15 C14 C13 N1 177.29(11) . C11 N1 C13 C18 -99.59(13) . C12 N1 C13 C18 83.78(14) . C11 N1 C13 C14 82.46(14) . C12 N1 C13 C14 -94.17(14) . C12 N1 C11 C10 175.98(11) . C13 N1 C11 C10 -0.55(17) . C12 N1 C11 C6 -2.95(16) . C13 N1 C11 C6 -179.48(10) . C9 C10 C11 N1 -175.73(11) . C9 C10 C11 C6 3.16(18) . N2 C6 C11 N1 1.23(17) . C7 C6 C11 N1 179.48(10) . N2 C6 C11 C10 -177.72(12) . C7 C6 C11 C10 0.52(17) . C13 C14 C15 C16 -0.66(19) . C18 C17 C16 C15 -0.8(2) . C18 C17 C16 Cl1 179.11(10) . C14 C15 C16 C17 1.3(2) . C14 C15 C16 Cl1 -178.53(10) . C8 N3 C19 C24 -42.48(19) . C8 N3 C19 C20 143.09(13) . C14 C13 C18 C17 1.18(18) . N1 C13 C18 C17 -176.72(11) . C16 C17 C18 C13 -0.49(18) . C24 C19 C20 C21 0.3(2) . N3 C19 C20 C21 174.99(12) . C19 C20 C21 C22 -0.1(2) . C20 C21 C22 C23 -0.3(2) . C20 C21 C22 Cl2 178.59(11) . C21 C22 C23 C24 0.5(2) . Cl2 C22 C23 C24 -178.41(10) . C22 C23 C24 C19 -0.27(19) . C20 C19 C24 C23 -0.13(19) . N3 C19 C24 C23 -174.46(12) . C9 N4 C25 C27 -150.77(14) . C9 N4 C25 C26 87.34(16) . O2 C28 C29 C31 158.11(12) . O1 C28 C29 C31 -21.02(17) . O2 C28 C29 C30 -20.29(18) . O1 C28 C29 C30 160.58(11) . C31 C29 C30 C31 0.25(19) 2_756 C28 C29 C30 C31 178.67(11) 2_756 C30 C29 C31 C30 -0.25(19) 2_756 C28 C29 C31 C30 -178.65(11) 2_756 O2A C32 C33 C34 -13.81(18) . O1A C32 C33 C34 166.46(11) . O2A C32 C33 C35 165.77(12) . O1A C32 C33 C35 -13.96(16) . C35 C33 C34 C35 0.48(19) 2_755 C32 C33 C34 C35 -179.93(11) 2_755 C34 C33 C35 C34 -0.48(19) 2_755 C32 C33 C35 C34 179.94(11) 2_755 _cod_database_fobs_code 2108446