#------------------------------------------------------------------------------ #$Date: 2021-06-26 00:25:43 +0300 (Sat, 26 Jun 2021) $ #$Revision: 266685 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/88/4518829.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_4518829 loop_ _publ_author_name 'Xie, Ming-Sheng' 'Li, Ning' 'Tian, Yin' 'Wu, Xiao-Xia' 'Deng, Yun' 'Qu, Gui-Rong' 'Guo, Hai-Ming' _publ_section_title ; Dynamic Kinetic Resolution of Carboxylic Esters Catalyzed by Chiral PPY N-Oxides: Synthesis of Nonsteroidal Anti-Inflammatory Drugs and Mechanistic Insights ; _journal_name_full 'ACS Catalysis' _journal_page_first 8183 _journal_page_last 8196 _journal_paper_doi 10.1021/acscatal.1c01438 _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'Cl, C22 H29 N4 O2' _chemical_formula_sum 'C22 H29 Cl N4 O2' _chemical_formula_weight 416.94 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-09-23 _audit_creation_method ; Olex2 1.3 (compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.90840(10) _cell_length_b 11.7353(2) _cell_length_c 16.7685(2) _cell_measurement_reflns_used 21359 _cell_measurement_temperature 297 _cell_measurement_theta_max 71.3850 _cell_measurement_theta_min 3.7720 _cell_volume 2146.59(5) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 297 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0521 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -82.00 9.00 1.00 1.00 -- -35.62 112.00 -88.00 91 2 \w 14.00 106.00 1.00 1.00 -- 35.62 30.00 64.00 92 3 \w 37.00 129.00 1.00 1.00 -- 107.12 -30.00 -96.00 92 4 \w 37.00 111.00 1.00 1.00 -- 107.12 -98.00 77.00 74 5 \w 101.00 177.00 1.00 1.00 -- 107.12 112.00 -88.00 76 6 \w -103.00 -19.00 1.00 1.00 -- -35.62 -57.00 120.00 84 7 \w 55.00 108.00 1.00 1.00 -- 35.62-178.00-150.00 53 8 \w 0.00 74.00 1.00 1.00 -- 35.62 -98.00 77.00 74 9 \w 40.00 125.00 1.00 1.00 -- 107.12 -61.00 -30.00 85 10 \w 38.00 110.00 1.00 1.00 -- 107.12 -95.00 -30.00 72 11 \w 100.00 177.00 1.00 1.00 -- 107.12 111.00 0.00 77 12 \w 38.00 110.00 1.00 1.00 -- 107.12 -95.00-180.00 72 13 \w 40.00 125.00 1.00 1.00 -- 107.12 -61.00-150.00 85 14 \w 37.00 129.00 1.00 1.00 -- 107.12 -30.00 30.00 92 15 \w -103.00 -19.00 1.00 1.00 -- -35.62 -57.00 -60.00 84 16 \w -103.00 -9.00 1.00 1.00 -- -35.62 -77.00-120.00 94 17 \w 9.00 103.00 1.00 1.00 -- 35.62 77.00 60.00 94 18 \w 57.00 108.00 1.00 1.00 -- 35.62 178.00 -60.00 51 19 \w 80.00 175.00 1.00 1.00 -- 107.12 77.00 -30.00 95 20 \w 86.00 177.00 1.00 1.00 -- 107.12 30.00 0.00 91 21 \w 69.00 178.00 1.00 1.00 -- 107.12 15.00 -90.00 109 22 \w 80.00 175.00 1.00 1.00 -- 107.12 77.00 60.00 95 23 \w 69.00 178.00 1.00 1.00 -- 107.12 15.00 90.00 109 24 \w 80.00 175.00 1.00 1.00 -- 107.12 77.00-180.00 95 25 \w 90.00 176.00 1.00 1.00 -- 107.12 45.00 -60.00 86 26 \w 69.00 178.00 1.00 1.00 -- 107.12 15.00-180.00 109 27 \w 9.00 103.00 1.00 1.00 -- 35.62 77.00-180.00 94 28 \w -34.00 55.00 1.00 1.00 -- 35.62 -38.00-150.00 89 29 \w -34.00 55.00 1.00 1.00 -- 35.62 -38.00 -30.00 89 30 \w -36.00 65.00 1.00 1.00 -- 35.62 -19.00 60.00 101 31 \w 80.00 175.00 1.00 1.00 -- 107.12 77.00 90.00 95 32 \w 80.00 175.00 1.00 1.00 -- 107.12 77.00 0.00 95 33 \w 80.00 175.00 1.00 1.00 -- 107.12 77.00-120.00 95 34 \w 80.00 175.00 1.00 1.00 -- 107.12 77.00 30.00 95 35 \w 80.00 144.00 1.00 1.00 -- 107.12 77.00 -60.00 64 36 \w 80.00 175.00 1.00 1.00 -- 107.12 77.00 150.00 95 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, EosS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0952877000 _diffrn_orient_matrix_UB_12 0.0471789000 _diffrn_orient_matrix_UB_13 -0.0592384000 _diffrn_orient_matrix_UB_21 0.1008393000 _diffrn_orient_matrix_UB_22 -0.0125870000 _diffrn_orient_matrix_UB_23 0.0637321000 _diffrn_orient_matrix_UB_31 0.0264131000 _diffrn_orient_matrix_UB_32 -0.1218570000 _diffrn_orient_matrix_UB_33 -0.0294803000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_unetI/netI 0.0336 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 30789 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.299 _diffrn_reflns_theta_min 4.599 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.777 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.46817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.290 _exptl_crystal_description block _exptl_crystal_F_000 888 _refine_diff_density_max 0.307 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.037 _refine_ls_abs_structure_details ; Flack x determined using 1667 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.011(8) _refine_ls_extinction_coef 0.0152(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 275 _refine_ls_number_reflns 4170 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0376 _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^)+(0.0683P)^2^+0.1663P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1045 _refine_ls_wR_factor_ref 0.1055 _reflns_Friedel_coverage 0.754 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 4033 _reflns_number_total 4170 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c01438_si_003.cif _cod_data_source_block ln-20200909 _cod_database_code 4518829 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C1 H1 O1 N1' _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. ; _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Others Sof(H18C)=Sof(H18D)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=1-FVAR(1) Sof(H18A)=Sof(H18B)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=FVAR(1) 3.a Ternary CH refined with riding coordinates: C4(H4), C10(H10) 3.b Secondary CH2 refined with riding coordinates: C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C18(H18A, H18B), C18(H18C,H18D), C21(H21A,H21B), C21(H21C,H21D), C22(H22A,H22B), C22A(H22C,H22D) 3.c Aromatic/amide H refined with riding coordinates: N2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C14(H14), C16(H16), C19(H19), C20(H20) 3.d Idealised Me refined as rotating group: C17(H17A,H17B,H17C) 3.e Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; TITL ln-20200909_a.res in P2(1)2(1)2(1) ln-20200909.res created by SHELXL-2018/3 at 21:26:47 on 23-Sep-2020 REM Old TITL ln-20200909 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.200, Rweak 0.065, Alpha 0.001 REM 1.372 for 23 systematic absences, Orientation as input REM Flack x = -2.694 ( 0.242 ) from 1684 Parsons' quotients REM Formula found by SHELXT: C15 N3 O3 CELL 1.54184 10.9084 11.7353 16.7685 90 90 90 ZERR 4 0.0001 0.0002 0.0002 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cl N O UNIT 88 116 4 16 8 L.S. 4 PLAN 4 TEMP 23.85 CONF MORE -1 BOND $H fmap 2 acta OMIT 7 8 13 OMIT 5 2 0 REM REM REM WGHT 0.068300 0.166300 EXTI 0.015163 FVAR 0.91320 0.69570 CL1 3 0.709990 0.280227 0.305869 11.00000 0.08433 0.04668 = 0.05389 -0.01014 -0.00198 -0.01368 O1 5 0.337920 0.554830 0.129813 11.00000 0.07415 0.04813 = 0.03166 0.00634 0.00192 -0.00364 AFIX 147 H1 2 0.321176 0.620483 0.142526 11.00000 -1.50000 AFIX 0 O2 5 0.396810 0.587906 0.483207 11.00000 0.05650 0.06392 = 0.03241 0.00526 -0.00182 0.00567 N1 4 0.450207 0.548467 0.275750 11.00000 0.03318 0.03625 = 0.03379 0.00036 0.00354 -0.00233 N2 4 0.322589 0.694001 0.381544 11.00000 0.03541 0.04391 = 0.03594 -0.00106 0.00096 0.00515 AFIX 43 H2 2 0.336349 0.719061 0.334188 11.00000 -1.20000 AFIX 0 N3 4 0.297742 0.480733 0.188749 11.00000 0.04906 0.03759 = 0.02911 0.00053 -0.00068 -0.00149 N4 4 0.145852 0.280376 0.362546 11.00000 0.03982 0.04303 = 0.03868 -0.00154 -0.00289 -0.00998 C1 1 0.353512 0.479535 0.262116 11.00000 0.03550 0.02973 = 0.03219 -0.00365 0.00052 0.00383 C2 1 0.398860 0.616836 0.413334 11.00000 0.03177 0.03769 = 0.03457 -0.00439 -0.00452 -0.00361 C3 1 0.301527 0.410109 0.320230 11.00000 0.03520 0.03404 = 0.03226 -0.00029 -0.00580 -0.00133 AFIX 43 H3 2 0.337515 0.407013 0.370461 11.00000 -1.20000 AFIX 0 C4 1 0.494486 0.564848 0.357686 11.00000 0.03054 0.03038 = 0.03970 0.00089 -0.00199 -0.00094 AFIX 13 H4 2 0.519516 0.490772 0.379200 11.00000 -1.20000 AFIX 0 C5 1 0.196464 0.344660 0.305305 11.00000 0.03334 0.03221 = 0.03831 -0.00271 -0.00181 0.00079 C6 1 0.110694 0.651590 0.421890 11.00000 0.03511 0.04188 = 0.03897 -0.00342 0.00100 0.01194 C7 1 0.069038 0.610594 0.349006 11.00000 0.03880 0.05364 = 0.03784 0.00243 -0.00143 0.00604 AFIX 43 H7 2 0.107590 0.633570 0.302226 11.00000 -1.20000 AFIX 0 C8 1 0.148090 0.345717 0.226218 11.00000 0.04032 0.03972 = 0.04394 -0.00451 -0.00913 -0.00447 AFIX 43 H8 2 0.081890 0.299610 0.212795 11.00000 -1.20000 AFIX 0 C9 1 0.200028 0.414932 0.170876 11.00000 0.04997 0.04623 = 0.03444 -0.00675 -0.01225 0.00113 AFIX 43 H9 2 0.167640 0.417072 0.119594 11.00000 -1.20000 AFIX 0 C10 1 0.216164 0.736549 0.425883 11.00000 0.04097 0.04849 = 0.04295 -0.01115 0.00164 0.00683 AFIX 13 H10 2 0.240015 0.745384 0.481888 11.00000 -1.20000 AFIX 0 C11 1 0.608796 0.637879 0.345451 11.00000 0.03427 0.03850 = 0.06082 -0.00436 -0.00140 -0.00453 AFIX 23 H11A 2 0.587848 0.717632 0.338723 11.00000 -1.20000 H11B 2 0.665458 0.630107 0.389700 11.00000 -1.20000 AFIX 0 C12 1 0.549743 0.570736 0.216944 11.00000 0.04498 0.05614 = 0.04689 0.00339 0.01430 -0.00404 AFIX 23 H12A 2 0.532545 0.638400 0.185660 11.00000 -1.20000 H12B 2 0.560600 0.506443 0.181281 11.00000 -1.20000 AFIX 0 C13 1 0.661680 0.587757 0.269230 11.00000 0.03691 0.04154 = 0.07011 0.00096 0.01289 -0.00461 AFIX 23 H13A 2 0.719393 0.639893 0.244625 11.00000 -1.20000 H13B 2 0.702580 0.515883 0.279628 11.00000 -1.20000 AFIX 0 C14 1 -0.028476 0.536476 0.345167 11.00000 0.03999 0.05298 = 0.05218 -0.00445 -0.00879 0.00455 AFIX 43 H14 2 -0.055702 0.510296 0.295907 11.00000 -1.20000 AFIX 0 C15 1 0.035391 0.210985 0.352611 11.00000 0.04186 0.05278 = 0.05421 -0.00340 -0.00068 -0.01396 AFIX 23 H15A 2 0.051416 0.145385 0.318997 11.00000 -1.20000 H15B 2 -0.030687 0.255267 0.329415 11.00000 -1.20000 AFIX 0 C16 1 0.053064 0.614920 0.490335 11.00000 0.05939 0.07221 = 0.03823 -0.00546 0.00218 -0.00036 AFIX 43 H16 2 0.080027 0.640744 0.539748 11.00000 -1.20000 AFIX 0 C17 1 0.177587 0.852624 0.394369 11.00000 0.05142 0.04168 = 0.08970 -0.01110 0.00394 0.00725 AFIX 137 H17A 2 0.244257 0.905388 0.400110 11.00000 -1.50000 H17B 2 0.108142 0.879572 0.424051 11.00000 -1.50000 H17C 2 0.156005 0.846199 0.339050 11.00000 -1.50000 AFIX 0 C18 1 0.191833 0.276995 0.444315 11.00000 0.07672 0.06995 = 0.03963 0.00851 -0.00946 -0.03310 PART 1 AFIX 23 H18A 2 0.173152 0.347175 0.472356 21.00000 -1.20000 H18B 2 0.279738 0.264611 0.445320 21.00000 -1.20000 AFIX 23 PART 2 H18C 2 0.219590 0.351278 0.462137 -21.00000 -1.20000 H18D 2 0.257508 0.221973 0.450495 -21.00000 -1.20000 AFIX 0 PART 0 C19 1 -0.086055 0.500800 0.413963 11.00000 0.04275 0.05582 = 0.07269 0.00701 0.00032 -0.00194 AFIX 43 H19 2 -0.152108 0.450834 0.411346 11.00000 -1.20000 AFIX 0 C20 1 -0.045072 0.539620 0.486108 11.00000 0.06705 0.09074 = 0.05260 0.01282 0.01452 -0.00960 AFIX 43 H20 2 -0.083199 0.515422 0.532734 11.00000 -1.20000 AFIX 0 C21 1 0.004516 0.174776 0.436691 11.00000 0.07711 0.08701 = 0.07047 0.01332 0.00680 -0.03763 PART 1 AFIX 23 H21A 2 -0.053336 0.227408 0.460631 21.00000 -1.20000 H21B 2 -0.031010 0.099004 0.437017 21.00000 -1.20000 AFIX 23 PART 2 H21C 2 -0.082726 0.184203 0.445735 -21.00000 -1.20000 H21D 2 0.024224 0.094762 0.443490 -21.00000 -1.20000 AFIX 0 PART 1 C22 1 0.123272 0.175963 0.481046 21.00000 0.08506 0.06277 = 0.04893 0.00700 0.00032 -0.02589 AFIX 23 H22A 2 0.167998 0.105428 0.473112 21.00000 -1.20000 H22B 2 0.110054 0.187340 0.537693 21.00000 -1.20000 AFIX 0 PART 2 C22A 1 0.067380 0.236966 0.490527 -21.00000 0.06815 0.06430 = 0.04378 0.00389 0.00565 -0.02411 AFIX 23 H22C 2 0.087307 0.191411 0.537021 -21.00000 -1.20000 H22D 2 0.019941 0.302585 0.507410 -21.00000 -1.20000 AFIX 0 HKLF 4 REM ln-20200909_a.res in P2(1)2(1)2(1) REM wR2 = 0.1055, GooF = S = 1.051, Restrained GooF = 1.051 for all data REM R1 = 0.0376 for 4033 Fo > 4sig(Fo) and 0.0388 for all 4170 data REM 275 parameters refined using 0 restraints END WGHT 0.0681 0.1689 REM Highest difference peak 0.307, deepest hole -0.247, 1-sigma level 0.037 Q1 1 0.6352 0.2902 0.3039 11.00000 0.05 0.31 Q2 1 0.7256 0.2068 0.3106 11.00000 0.05 0.24 Q3 1 0.7146 0.2793 0.3564 11.00000 0.05 0.22 Q4 1 0.7328 0.3590 0.3083 11.00000 0.05 0.17 ; _shelx_res_checksum 28265 _shelx_hkl_file ; 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661.86 19.36 0 -6 0 613.24 19.66 0 -6 0 594.56 20.90 0 6 0 598.13 15.41 0 -6 -1 53.18 6.81 0 -6 -1 74.42 6.79 0 -6 1 81.86 6.96 0 6 -1 77.60 7.21 0 -6 1 74.91 7.14 0 -6 -1 78.38 6.77 0 -6 1 68.42 7.18 0 -6 -1 74.96 7.43 0 6 1 66.05 5.49 0 6 -1 75.23 9.27 0 6 1 91.45 9.94 0 -6 2 2.86 1.82 0 -6 -2 6.46 2.43 0 6 2 4.63 1.55 0 -6 -2 8.92 2.75 0 6 -2 3.49 1.70 0 -6 2 4.80 1.74 0 -6 -2 2.06 2.03 0 -6 2 5.80 1.91 0 6 2 8.58 3.32 0 6 -2 7.34 3.28 0 -6 3 121.65 9.76 0 6 3 121.97 8.63 0 -6 -3 154.38 10.46 0 -6 -3 124.75 10.33 0 -6 3 140.05 10.26 0 6 -3 151.58 10.57 0 -6 3 154.68 10.10 0 6 -3 92.13 11.19 0 6 3 116.77 11.02 0 6 4 0.03 1.23 0 -6 4 1.29 1.42 0 -6 -4 -0.31 1.25 0 6 -4 1.67 1.53 0 -6 4 1.52 1.74 0 -6 4 0.08 1.76 0 6 -4 0.19 1.76 0 6 5 63.92 7.12 0 -6 5 60.06 7.04 0 -6 5 77.01 8.06 0 6 -5 82.77 8.37 0 -6 -5 68.02 7.96 0 -6 5 68.39 7.89 0 -6 6 1083.83 30.18 0 6 6 1076.52 31.51 0 -6 6 1210.76 34.04 0 -6 -6 957.45 31.19 0 6 -6 1235.28 33.66 0 -6 6 1126.00 33.75 0 6 7 494.11 22.68 0 -6 7 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18.31 4.50 -10 6 -6 12.71 4.75 10 6 6 16.60 3.99 10 -6 -6 21.62 4.54 -10 -6 7 12.98 4.01 -10 -6 7 18.71 4.72 10 -6 -7 12.29 3.75 10 6 7 15.60 4.19 -10 -6 7 15.10 3.83 10 6 7 11.60 3.17 -10 6 -7 27.53 7.64 -10 -6 8 1.17 1.84 -10 -6 8 2.48 1.99 10 -6 -8 0.74 2.04 10 6 8 1.36 1.78 -10 -6 8 1.62 1.71 10 6 8 0.79 1.35 -10 -6 9 62.02 7.42 -10 -6 9 59.16 7.17 10 -6 -9 48.64 6.39 -10 -6 9 59.58 5.97 10 6 9 57.65 6.91 -10 -6 10 18.53 3.77 -10 -6 10 18.54 3.83 10 -6 -10 13.59 3.09 10 6 10 18.82 3.75 -10 6 -10 6.84 5.79 -10 -7 -9 12.15 2.38 10 7 -9 11.03 2.42 10 7 -9 7.53 2.08 -10 -7 -8 17.01 3.39 10 -7 8 19.61 4.04 -10 -7 -8 14.71 2.94 -10 -7 -8 13.04 2.91 -10 -7 -8 13.22 2.72 10 7 -8 11.50 2.85 10 7 -8 9.87 2.66 10 7 -8 7.98 2.48 -10 -7 -7 26.39 4.52 10 -7 7 28.89 4.87 -10 -7 -7 22.90 3.99 -10 -7 -7 20.45 3.89 -10 -7 -7 20.23 3.47 10 7 -7 16.90 3.54 10 7 -7 20.46 3.85 10 7 -7 14.40 3.39 -10 -7 -6 8.63 2.96 10 -7 6 7.64 2.81 -10 -7 -6 7.22 2.68 -10 -7 -6 6.96 2.62 -10 -7 -6 5.92 2.00 10 7 -6 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3.81 -12 2 7 10.21 2.69 12 2 -7 12.46 3.00 -12 -2 -6 6.79 2.17 12 2 -6 4.52 2.34 -12 2 6 7.61 2.66 -12 -2 -6 8.41 2.66 -12 2 6 9.66 3.01 12 2 -6 8.94 3.18 -12 -2 -6 5.93 2.42 -12 2 6 4.76 2.33 12 2 -6 7.19 2.73 -12 -2 -5 34.43 4.86 12 2 -5 20.87 4.49 -12 -2 -5 29.15 4.81 -12 2 5 22.47 4.52 -12 -2 -5 27.50 4.67 12 2 -5 22.49 5.06 12 2 -5 18.97 3.82 -12 2 5 11.73 3.24 12 2 -5 24.51 4.78 -12 -2 -4 26.87 4.60 12 2 -4 21.56 4.66 -12 -2 -4 24.94 4.62 -12 2 4 24.06 4.97 12 2 -4 15.65 3.70 -12 -2 -4 27.60 4.92 12 2 -4 18.14 4.62 -12 2 4 8.31 2.93 12 2 -4 14.42 3.93 -12 -2 -3 2.45 1.96 12 2 -3 0.73 1.73 -12 -2 -3 2.49 2.28 -12 2 3 1.65 2.15 12 2 -3 1.36 2.00 -12 -2 -3 3.06 2.22 -12 2 3 1.84 1.62 12 -2 3 1.28 1.62 12 2 -3 0.66 1.47 12 2 -3 1.06 1.75 -12 -2 -2 12.73 4.09 12 2 -2 10.53 3.68 -12 -2 -2 15.65 4.12 -12 2 2 14.27 3.93 -12 -2 -2 13.14 3.71 -12 2 2 7.13 2.87 12 2 -2 8.51 2.97 12 -2 2 13.46 3.98 12 2 -2 13.73 4.12 -12 -2 -1 38.90 6.26 12 2 -1 34.85 6.45 -12 -2 -1 36.69 5.64 -12 -2 -1 33.92 5.46 -12 2 1 32.72 5.85 12 2 -1 27.60 5.31 -12 -2 -1 32.76 5.62 -12 2 1 12.97 3.62 12 -2 1 30.16 5.85 12 2 -1 27.91 5.48 -12 -2 0 15.32 4.34 -12 -2 0 20.32 5.24 -12 -2 0 8.21 2.97 -12 -2 0 10.05 3.28 -12 2 0 10.34 3.61 -12 2 0 5.11 2.57 -12 -2 0 7.14 2.71 12 2 0 5.37 2.67 12 -2 0 6.02 2.89 12 2 0 10.23 3.52 -12 -2 1 46.48 7.24 12 -2 -1 32.83 6.52 -12 -2 1 36.68 5.97 -12 -2 1 35.33 5.61 -12 2 -1 35.21 5.86 -12 -2 1 37.37 6.61 12 2 1 25.93 5.32 -12 -2 1 37.71 6.31 -12 2 -1 30.82 7.60 -12 2 -1 25.11 5.15 12 2 1 29.17 5.26 12 -2 -1 23.99 5.39 -12 -2 2 16.81 4.41 -12 -2 2 32.36 6.48 12 -2 -2 18.35 4.88 -12 -2 2 16.35 4.12 -12 -2 2 16.21 3.86 -12 2 -2 16.45 3.95 -12 2 -2 14.19 4.02 -12 -2 2 11.32 3.58 12 2 2 12.02 3.71 12 -2 -2 13.30 4.20 12 2 2 16.97 4.01 -12 -2 3 1.20 2.18 12 -2 -3 2.59 2.43 -12 -2 3 1.01 1.75 -12 2 -3 0.49 1.74 -12 -2 3 1.45 1.94 -12 2 -3 1.85 1.66 12 2 3 2.61 2.27 -12 -2 3 1.92 1.86 12 -2 -3 2.73 1.67 -12 -2 4 23.63 5.14 -12 -2 4 40.95 6.24 12 -2 -4 19.27 4.61 12 -2 -4 17.18 4.06 -12 -2 4 25.58 5.11 -12 2 -4 24.07 4.45 -12 -2 4 23.36 4.13 -12 2 -4 24.75 4.92 12 2 4 18.14 4.41 -12 -2 4 16.97 4.16 12 -2 -4 21.38 4.59 -12 -2 5 44.23 6.03 12 -2 -5 26.36 5.35 12 -2 -5 22.40 4.64 -12 -2 5 30.40 5.38 -12 2 -5 32.24 4.86 12 2 5 26.53 5.07 -12 2 -5 35.98 5.80 -12 -2 5 28.84 5.08 -12 -2 5 32.34 5.68 12 -2 -5 24.05 4.67 -12 -2 6 5.76 2.63 -12 -2 6 16.26 3.87 12 -2 -6 7.14 2.87 12 -2 -6 7.01 2.56 -12 -2 6 9.32 3.06 -12 2 -6 14.58 3.28 -12 2 -6 10.51 8.12 12 2 6 7.41 3.00 -12 2 -6 9.80 3.06 -12 -2 6 6.11 2.56 12 -2 -6 8.15 2.85 -12 -2 7 17.20 3.90 12 -2 -7 11.06 3.31 12 -2 -7 14.47 3.46 -12 -2 7 17.53 3.88 -12 2 -7 23.09 4.25 12 2 7 18.54 4.00 -12 2 -7 16.50 7.77 -12 -2 7 16.64 3.74 12 -2 -7 14.23 3.07 12 -2 -8 6.46 2.16 12 -2 -8 7.00 2.38 -12 -2 8 10.10 2.84 12 2 8 11.44 3.19 -12 2 -8 10.99 6.59 -12 2 -8 11.68 2.90 -12 -2 8 5.11 2.04 -12 -3 -8 41.23 4.35 12 3 -8 27.89 4.18 12 -3 7 84.84 7.23 12 3 -7 71.33 6.31 -12 -3 -7 85.71 6.79 -12 3 7 82.76 7.32 12 3 -7 63.17 6.87 12 3 -7 65.71 6.16 -12 -3 -6 41.35 4.78 12 3 -6 34.39 4.80 -12 -3 -6 41.38 5.15 -12 3 6 33.59 5.01 12 3 -6 27.68 4.87 -12 -3 -6 36.50 4.66 12 3 -6 26.68 3.99 12 3 -6 30.04 4.61 -12 -3 -5 23.24 4.01 12 -3 5 27.01 4.36 12 3 -5 20.04 4.04 -12 -3 -5 24.21 4.23 -12 3 5 20.80 4.19 12 3 -5 13.74 3.25 -12 -3 -5 27.22 4.35 12 3 -5 20.98 4.61 12 3 -5 14.99 3.57 -12 -3 -4 3.09 2.03 12 3 -4 2.59 1.99 12 -3 4 0.63 1.95 -12 -3 -4 1.78 1.90 -12 3 4 1.34 2.01 12 3 -4 1.22 1.51 12 3 -4 1.14 1.82 -12 -3 -4 2.42 1.83 -12 3 4 0.52 1.38 12 -3 4 2.83 2.25 12 3 -4 2.64 1.96 -12 -3 -3 1.67 1.71 12 3 -3 1.29 1.90 -12 -3 -3 3.21 1.97 -12 -3 -3 2.83 2.03 -12 3 3 4.66 2.57 12 3 -3 0.83 1.31 12 3 -3 2.82 2.20 -12 -3 -3 3.54 2.17 -12 3 3 -0.67 1.52 12 -3 3 2.64 1.83 12 3 -3 2.13 1.60 -12 -3 -2 20.99 4.44 -12 -3 -2 19.04 4.02 -12 -3 -2 19.18 4.04 -12 3 2 14.80 3.96 -12 -3 -2 17.09 3.91 12 -3 2 15.47 4.21 12 3 -2 13.35 3.75 12 3 -2 10.43 3.19 -12 -3 -1 14.30 3.86 -12 -3 -1 12.38 3.54 -12 -3 -1 14.77 3.65 -12 3 1 14.98 4.03 -12 3 1 -0.16 1.96 -12 -3 -1 11.16 3.24 12 3 -1 7.96 2.96 12 -3 1 10.99 3.76 12 3 -1 10.02 3.28 -12 -3 0 40.42 6.32 -12 -3 0 44.16 6.32 -12 -3 0 39.58 5.50 -12 3 0 38.76 6.09 -12 -3 0 45.56 6.99 12 3 0 33.54 5.84 -12 -3 0 36.53 5.65 -12 3 0 1.14 9.80 -12 3 0 9.11 2.87 12 -3 0 33.88 6.03 12 3 0 33.66 5.57 -12 -3 1 18.65 4.67 -12 -3 1 15.82 4.21 -12 -3 1 12.68 3.67 -12 -3 1 14.10 3.43 -12 3 -1 16.24 3.86 -12 3 -1 5.92 2.51 -12 -3 1 12.48 3.50 12 3 1 9.80 3.41 12 -3 -1 12.67 4.00 12 3 1 13.50 3.59 -12 -3 2 17.74 4.55 -12 -3 2 17.34 4.26 12 -3 -2 14.36 4.04 -12 -3 2 16.76 4.07 -12 -3 2 17.72 3.58 -12 3 -2 15.35 3.63 -12 3 -2 9.90 3.07 -12 -3 2 18.34 4.19 12 3 2 17.49 4.28 12 -3 -2 13.63 4.08 -12 -3 3 3.42 2.46 -12 -3 3 7.52 3.29 12 -3 -3 5.44 2.75 -12 -3 3 5.33 2.56 -12 -3 3 5.13 2.14 -12 3 -3 3.17 1.99 -12 3 -3 3.29 2.12 12 3 3 3.57 2.07 -12 -3 3 4.10 2.25 12 -3 -3 2.36 2.02 -12 -3 4 2.19 2.29 -12 -3 4 5.12 3.01 12 -3 -4 2.34 1.87 -12 -3 4 2.89 2.46 -12 3 -4 0.06 1.51 12 3 4 -0.25 1.49 -12 3 -4 6.21 2.96 -12 -3 4 0.91 1.38 12 -3 -4 0.17 1.85 -12 -3 5 22.95 4.68 -12 -3 5 32.14 4.87 12 -3 -5 16.89 4.01 12 -3 -5 25.52 4.17 -12 -3 5 24.60 4.65 -12 3 -5 30.02 4.44 12 3 5 23.12 4.67 -12 -3 5 21.17 4.18 -12 3 -5 24.36 4.42 12 -3 -5 25.96 4.72 -12 -3 6 41.35 4.66 12 -3 -6 39.43 4.48 12 -3 -6 29.61 4.96 12 -3 -6 29.85 4.94 -12 -3 6 36.33 5.46 12 3 6 36.77 5.48 -12 3 -6 39.76 5.33 -12 -3 6 31.93 4.92 -12 -3 6 41.08 6.04 12 -3 -6 36.29 5.03 12 -3 -7 65.98 6.61 12 -3 -7 74.62 7.35 -12 -3 7 86.44 7.75 12 3 7 78.68 7.40 -12 3 -7 99.23 7.84 -12 -3 7 69.37 6.54 12 -3 -7 87.17 6.77 -12 -3 7 93.51 8.34 -12 -3 8 37.45 4.72 12 3 8 35.09 4.62 12 -4 7 1.78 1.33 -12 -4 -7 3.25 1.60 -12 4 7 3.50 1.70 12 4 -7 2.32 1.69 12 4 -7 1.98 1.33 12 -4 6 31.67 4.50 -12 -4 -6 34.58 4.17 -12 -4 -6 30.86 4.09 -12 4 6 25.44 4.31 12 4 -6 22.65 4.13 12 4 -6 20.91 3.47 12 4 -6 23.62 3.91 -12 -4 -5 32.32 4.40 -12 -4 -5 27.93 4.10 -12 4 5 26.57 4.58 12 4 -5 22.84 4.47 12 4 -5 19.44 3.64 12 4 -5 24.07 4.15 -12 -4 -4 5.13 2.05 12 -4 4 5.11 2.37 -12 -4 -4 3.81 1.90 -12 -4 -4 4.32 2.02 -12 4 4 6.42 2.63 12 4 -4 3.48 1.89 12 4 -4 2.66 2.18 -12 -4 -4 5.55 2.08 12 -4 4 8.47 3.08 12 4 -4 1.45 1.45 -12 -4 -3 38.56 5.27 12 -4 3 42.99 6.06 -12 -4 -3 41.27 5.37 -12 -4 -3 35.32 4.80 -12 4 3 32.46 5.33 -12 -4 -3 35.76 4.63 12 4 -3 26.32 4.66 12 -4 3 44.04 6.45 12 4 -3 29.77 4.76 -12 -4 -2 11.68 3.13 12 -4 2 13.00 3.58 -12 -4 -2 14.82 3.36 -12 -4 -2 12.63 3.04 -12 4 2 10.29 3.15 -12 -4 -2 13.20 3.08 12 -4 2 14.02 3.92 12 4 -2 10.17 3.02 12 4 -2 8.73 2.89 -12 -4 -1 3.50 2.26 12 -4 1 1.41 1.78 -12 -4 -1 2.43 2.04 -12 -4 -1 0.77 1.33 -12 4 1 4.06 2.57 -12 -4 -1 3.09 1.95 12 -4 1 0.47 1.63 12 4 -1 1.89 1.86 12 4 -1 1.85 1.80 -12 -4 0 20.98 4.75 -12 -4 0 24.39 4.49 12 -4 0 24.43 4.34 12 -4 0 15.98 3.92 -12 -4 0 24.78 4.65 -12 -4 0 20.59 3.69 -12 4 0 21.24 4.40 -12 -4 0 20.28 3.82 -12 4 0 19.71 4.84 12 4 0 19.11 4.09 12 -4 0 23.03 5.13 12 4 0 18.43 3.91 -12 -4 1 5.60 2.87 -12 -4 1 5.56 2.49 12 -4 -1 1.14 2.16 12 -4 -1 0.68 1.97 -12 -4 1 3.09 2.28 -12 -4 1 3.09 1.75 -12 4 -1 1.25 1.83 -12 -4 1 2.01 1.41 12 4 1 2.26 1.99 12 -4 -1 3.08 2.27 -12 -4 2 15.22 4.09 -12 -4 2 12.93 3.26 12 -4 -2 6.51 1.91 12 -4 -2 11.34 3.28 -12 -4 2 14.10 3.70 -12 4 -2 6.38 2.08 -12 -4 2 10.31 2.78 12 4 2 10.84 3.30 12 -4 -2 12.10 3.55 -12 -4 3 36.94 5.07 12 -4 -3 27.19 4.21 12 -4 -3 36.73 5.35 -12 -4 3 38.80 5.81 -12 4 -3 33.41 4.70 12 4 3 29.66 5.15 -12 -4 3 32.80 4.82 -12 -4 3 35.92 5.95 12 -4 -3 33.11 5.49 -12 -4 4 2.80 1.68 -12 -4 4 5.54 2.16 12 -4 -4 -2.68 2.71 12 -4 -4 5.71 2.03 -12 -4 4 4.19 2.34 12 4 4 3.61 1.76 -12 4 -4 -1.60 2.36 -12 -4 4 5.16 2.17 12 -4 -4 4.10 2.26 -12 -4 5 28.71 3.85 12 -4 -5 16.43 3.00 12 -4 -5 28.02 4.04 -12 -4 5 26.78 4.62 12 4 5 22.95 4.29 -12 -4 5 22.09 3.72 12 -4 -5 25.50 4.37 -12 -4 5 28.65 5.05 -12 -4 6 28.40 4.49 12 4 6 29.46 4.54 -12 -4 6 28.98 4.74 -12 -4 6 19.60 3.33 12 -4 -6 26.16 3.97 -12 -4 7 1.74 1.58 -12 -4 7 2.96 1.65 12 4 7 1.73 1.39 12 -5 5 40.57 4.79 -12 -5 -5 43.73 4.68 -12 5 5 31.71 4.52 12 5 -5 26.18 3.83 12 5 -5 32.12 4.21 12 -5 4 3.69 1.52 -12 -5 -4 5.99 2.23 -12 -5 -4 4.87 1.84 -12 -5 -4 6.68 2.04 -12 5 4 4.13 2.09 12 5 -4 3.25 1.74 12 5 -4 3.48 1.49 12 -5 3 2.84 1.33 -12 -5 -3 4.67 2.11 12 -5 3 11.04 3.62 12 -5 3 8.70 2.91 -12 -5 -3 3.54 1.80 -12 -5 -3 4.26 1.83 -12 5 3 2.78 1.87 12 5 -3 4.58 1.99 12 5 -3 5.37 2.32 -12 -5 -2 -0.65 1.52 12 -5 2 -0.43 1.54 -12 -5 -2 1.21 1.60 -12 -5 -2 0.08 1.15 -12 5 2 0.72 1.52 12 -5 2 1.25 1.82 12 5 -2 1.33 1.50 12 5 -2 -0.05 1.38 -12 -5 -1 4.67 1.93 12 -5 1 16.23 4.23 12 -5 1 2.98 2.01 -12 -5 -1 4.67 2.21 -12 5 1 5.44 2.41 -12 5 1 -8.76 5.39 12 5 -1 2.76 1.87 12 -5 1 4.72 2.57 12 5 -1 5.28 2.21 -12 -5 0 19.25 3.69 12 -5 0 25.99 4.42 12 -5 0 18.82 4.00 -12 -5 0 21.53 4.14 -12 5 0 13.57 3.09 -12 5 0 20.47 5.37 12 5 0 16.09 3.61 12 -5 0 16.59 4.14 12 5 0 18.52 3.34 -12 -5 1 6.41 2.80 -12 -5 1 4.53 1.87 12 -5 -1 2.42 1.70 12 -5 -1 4.33 2.35 -12 -5 1 6.30 2.54 -12 5 -1 -0.25 1.90 12 5 1 4.01 2.13 12 -5 -1 5.53 2.62 -12 -5 2 1.91 2.04 -12 -5 2 0.12 1.54 12 -5 -2 -0.42 2.37 12 -5 -2 0.48 1.61 -12 -5 2 0.44 1.65 12 5 2 1.92 1.79 12 -5 -2 1.06 1.48 -12 -5 3 6.97 2.93 -12 -5 3 2.37 1.26 12 -5 -3 -1.23 2.34 12 -5 -3 4.88 2.26 -12 -5 3 3.99 1.93 12 5 3 2.83 2.09 12 -5 -3 5.14 2.44 -12 -5 4 4.89 2.33 12 -5 -4 -1.72 2.49 12 -5 -4 6.13 2.21 -12 -5 4 4.10 1.95 12 5 4 4.40 2.04 12 -5 -4 4.58 2.19 -12 -5 5 38.72 4.85 12 5 5 36.64 4.66 -12 -5 5 42.65 5.52 -12 -6 -3 37.94 4.32 12 6 -3 28.04 3.95 -12 -6 -2 3.97 1.76 12 -6 2 7.06 2.47 -12 -6 -2 3.89 1.79 12 6 -2 4.22 1.89 -12 -6 -1 58.22 5.50 12 -6 1 67.83 6.71 -12 -6 -1 65.48 6.15 12 6 -1 43.33 5.08 -12 6 1 41.28 6.83 -12 -6 0 4.48 1.98 12 -6 0 4.06 2.00 -12 -6 0 3.71 1.88 -12 6 0 9.27 4.32 12 6 0 2.52 1.79 -12 -6 1 66.49 5.63 12 -6 -1 70.75 6.47 12 -6 -1 75.19 7.05 -12 -6 1 65.50 6.24 -12 6 -1 85.52 9.63 12 6 1 55.44 5.69 12 -6 -2 4.64 2.08 -12 -6 2 3.87 1.82 12 6 2 2.92 1.71 -12 -6 3 42.34 4.84 -12 -6 3 44.63 5.35 -13 0 0 1.83 2.36 -13 0 0 0.25 1.55 -13 0 0 -0.01 1.59 13 0 0 -0.82 1.33 -13 0 -1 2.26 2.02 -13 0 1 7.24 3.21 -13 0 -1 1.04 1.53 -13 0 1 1.51 1.79 -13 0 -1 0.48 1.35 -13 0 1 0.08 1.62 13 0 1 0.59 1.42 13 0 -1 -0.21 1.37 -13 0 -2 1.18 1.52 -13 0 -2 -0.35 1.46 -13 0 2 2.03 1.68 -13 0 -2 0.33 1.38 -13 0 2 0.39 1.46 13 0 -2 -0.80 1.57 -13 0 -3 0.79 1.57 -13 0 3 2.10 1.68 -13 0 -3 2.22 2.15 -13 0 3 0.06 1.33 13 0 -3 2.15 1.76 -13 0 -4 15.63 3.02 -13 0 4 12.66 2.70 -13 0 -4 15.98 3.30 -13 0 4 10.30 2.82 13 0 -4 9.40 2.66 13 0 -5 0.47 1.12 -13 0 -5 -1.84 1.60 13 0 -5 -0.03 1.03 -13 -1 -4 11.57 2.71 -13 1 4 8.18 2.45 -13 -1 -4 12.21 2.86 -13 1 4 8.84 2.49 13 1 -4 6.44 2.19 -13 -1 -3 18.48 3.24 -13 -1 -3 16.72 3.22 -13 1 3 13.55 2.98 -13 -1 -3 18.76 3.61 -13 1 3 10.44 2.78 13 1 -3 10.73 2.82 -13 -1 -2 60.59 6.07 -13 -1 -2 54.44 5.73 -13 1 2 49.05 5.64 -13 -1 -2 54.41 5.95 -13 1 2 41.45 5.39 13 1 -2 45.49 5.57 -13 -1 -1 2.13 1.71 -13 -1 -1 2.33 1.74 -13 1 1 0.83 1.52 -13 -1 -1 1.59 1.62 -13 1 1 1.93 1.43 13 -1 1 -0.05 1.35 13 1 -1 0.79 1.52 -13 1 0 41.63 5.50 -13 -1 0 35.39 5.15 -13 -1 0 35.75 4.76 -13 1 0 36.85 4.97 -13 1 0 29.97 4.79 -13 -1 0 35.31 5.01 13 -1 0 30.23 4.76 13 1 0 32.42 4.67 -13 -1 1 6.00 2.83 -13 1 -1 4.65 2.51 -13 -1 1 4.21 1.97 -13 1 -1 2.45 1.57 13 1 1 1.62 1.32 -13 1 -1 0.63 1.47 -13 -1 1 0.80 1.57 13 -1 -1 1.74 1.63 13 1 1 1.45 1.33 -13 -1 2 63.84 6.54 -13 1 -2 49.76 5.64 -13 1 -2 58.03 6.06 -13 -1 2 53.21 5.40 13 1 2 41.85 5.06 -13 1 -2 56.88 6.27 -13 -1 2 46.26 5.69 13 -1 -2 42.49 5.63 -13 -1 3 23.90 4.10 -13 -1 3 17.04 3.11 -13 1 -3 15.29 3.07 -13 1 -3 20.80 3.88 13 1 3 11.93 2.78 -13 -1 3 12.90 3.16 13 -1 -3 11.76 2.99 -13 -1 4 15.54 3.20 -13 1 -4 12.20 2.69 -13 1 -4 13.00 3.10 -13 -1 4 9.60 2.68 13 -1 -4 7.56 2.44 -13 -2 -4 22.98 3.34 -13 2 4 19.80 3.30 13 2 -4 16.78 3.09 -13 -2 -3 15.38 2.85 -13 -2 -3 14.72 2.86 -13 2 3 11.52 2.69 -13 -2 -3 13.79 2.82 13 2 -3 10.38 2.66 -13 -2 -2 13.55 2.89 -13 -2 -2 9.48 2.43 -13 2 2 11.16 2.77 -13 -2 -2 12.20 2.90 -13 2 2 4.56 1.73 13 2 -2 11.61 2.81 -13 -2 -1 0.68 1.45 -13 -2 -1 0.77 1.21 -13 2 1 0.39 1.76 -13 -2 -1 2.17 1.72 -13 2 1 0.59 0.97 13 2 -1 1.04 1.05 13 -2 1 1.88 1.54 13 2 -1 1.24 1.23 -13 -2 0 -0.34 1.48 -13 -2 0 -1.71 1.60 -13 2 0 -0.92 1.45 13 2 0 -0.53 1.04 -13 2 0 -0.26 1.29 -13 -2 0 -1.43 1.80 13 -2 0 0.27 1.26 13 2 0 -0.85 1.25 -13 -2 1 1.96 1.84 -13 2 -1 4.11 2.13 -13 -2 1 2.94 1.66 -13 2 -1 1.83 1.67 13 2 1 1.58 1.37 -13 2 -1 1.54 1.27 -13 -2 1 1.62 1.66 13 -2 -1 1.65 1.65 -13 -2 2 9.36 2.73 -13 2 -2 11.40 2.72 13 2 2 9.63 2.54 -13 2 -2 11.02 2.76 -13 -2 2 10.82 2.73 13 -2 -2 7.19 2.40 -13 -2 3 11.84 2.83 -13 2 -3 15.74 3.03 13 2 3 9.95 2.59 -13 2 -3 12.12 2.83 -13 -2 3 12.31 2.84 13 -2 -3 10.19 2.74 13 -2 -4 19.60 3.47 -13 -3 -2 8.78 2.18 -13 3 2 10.10 2.56 -13 -3 -1 14.06 2.88 13 -3 1 15.51 3.17 -13 3 1 14.14 3.00 -13 -3 0 10.25 2.45 13 -3 0 10.39 2.63 -13 3 0 14.01 2.93 13 3 0 7.86 2.21 13 -3 0 10.86 2.82 -13 -3 1 15.73 2.90 13 -3 -1 12.34 2.77 13 3 1 11.07 2.64 13 -3 -1 12.54 3.02 -13 -3 2 12.07 2.53 13 -3 -2 9.45 2.36 13 3 2 9.44 2.53 13 -3 -2 8.79 2.59 0 0 0 0.00 0.00 TITL ln-20200909 in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 10.908364 11.735326 16.768499 90.0000 90.0000 90.0000 ZERR 40.00 0.000109 0.000153 0.000163 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 40.00 40.00 40.00 40.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 54833 _olex2_date_sample_data_collection 2020-09-09 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.762 _oxdiff_exptl_absorpt_empirical_full_min 0.632 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.70999(8) 0.28023(6) 0.30587(4) 0.0616(2) Uani 1 1 d . . . . . O1 O 0.3379(2) 0.55483(16) 0.12981(10) 0.0513(5) Uani 1 1 d . . . . . H1 H 0.321176 0.620483 0.142526 0.077 Uiso 1 1 calc R U . . . O2 O 0.39681(19) 0.58791(19) 0.48321(10) 0.0509(5) Uani 1 1 d . . . . . N1 N 0.45021(17) 0.54847(17) 0.27575(11) 0.0344(4) Uani 1 1 d . . . . . N2 N 0.32259(17) 0.69400(18) 0.38154(12) 0.0384(4) Uani 1 1 d . . . . . H2 H 0.336349 0.719061 0.334188 0.046 Uiso 1 1 calc R U . . . N3 N 0.29774(19) 0.48073(18) 0.18875(10) 0.0386(4) Uani 1 1 d . . . . . N4 N 0.14585(18) 0.28038(19) 0.36255(12) 0.0405(5) Uani 1 1 d . . . . . C1 C 0.3535(2) 0.47953(19) 0.26212(12) 0.0325(5) Uani 1 1 d . . . . . C2 C 0.39886(19) 0.6168(2) 0.41333(13) 0.0347(5) Uani 1 1 d . . . . . C3 C 0.3015(2) 0.4101(2) 0.32023(12) 0.0338(4) Uani 1 1 d . . . . . H3 H 0.337515 0.407013 0.370461 0.041 Uiso 1 1 calc R U . . . C4 C 0.49449(19) 0.56485(19) 0.35769(13) 0.0335(5) Uani 1 1 d . . . . . H4 H 0.519516 0.490772 0.379200 0.040 Uiso 1 1 calc R U . . . C5 C 0.19646(19) 0.3447(2) 0.30531(13) 0.0346(5) Uani 1 1 d . . . . . C6 C 0.1107(2) 0.6516(2) 0.42189(14) 0.0387(5) Uani 1 1 d . . . . . C7 C 0.0690(2) 0.6106(3) 0.34901(14) 0.0434(6) Uani 1 1 d . . . . . H7 H 0.107590 0.633570 0.302226 0.052 Uiso 1 1 calc R U . . . C8 C 0.1481(2) 0.3457(2) 0.22622(15) 0.0413(5) Uani 1 1 d . . . . . H8 H 0.081890 0.299610 0.212795 0.050 Uiso 1 1 calc R U . . . C9 C 0.2000(2) 0.4149(2) 0.17088(14) 0.0435(6) Uani 1 1 d . . . . . H9 H 0.167640 0.417072 0.119594 0.052 Uiso 1 1 calc R U . . . C10 C 0.2162(2) 0.7365(2) 0.42588(15) 0.0441(6) Uani 1 1 d . . . . . H10 H 0.240015 0.745384 0.481888 0.053 Uiso 1 1 calc R U . . . C11 C 0.6088(2) 0.6379(2) 0.34545(17) 0.0445(6) Uani 1 1 d . . . . . H11A H 0.587848 0.717632 0.338723 0.053 Uiso 1 1 calc R U . . . H11B H 0.665458 0.630107 0.389700 0.053 Uiso 1 1 calc R U . . . C12 C 0.5497(2) 0.5707(3) 0.21694(16) 0.0493(6) Uani 1 1 d . . . . . H12A H 0.532545 0.638400 0.185660 0.059 Uiso 1 1 calc R U . . . H12B H 0.560600 0.506443 0.181281 0.059 Uiso 1 1 calc R U . . . C13 C 0.6617(2) 0.5878(2) 0.26923(18) 0.0495(6) Uani 1 1 d . . . . . H13A H 0.719393 0.639893 0.244625 0.059 Uiso 1 1 calc R U . . . H13B H 0.702580 0.515883 0.279628 0.059 Uiso 1 1 calc R U . . . C14 C -0.0285(2) 0.5365(3) 0.34517(17) 0.0484(6) Uani 1 1 d . . . . . H14 H -0.055702 0.510296 0.295907 0.058 Uiso 1 1 calc R U . . . C15 C 0.0354(2) 0.2110(3) 0.35261(17) 0.0496(6) Uani 1 1 d . . . . . H15A H 0.051416 0.145385 0.318997 0.060 Uiso 1 1 calc R U . . . H15B H -0.030687 0.255267 0.329415 0.060 Uiso 1 1 calc R U . . . C16 C 0.0531(3) 0.6149(3) 0.49033(16) 0.0566(7) Uani 1 1 d . . . . . H16 H 0.080027 0.640744 0.539748 0.068 Uiso 1 1 calc R U . . . C17 C 0.1776(3) 0.8526(3) 0.3944(2) 0.0609(8) Uani 1 1 d . . . . . H17A H 0.244257 0.905388 0.400110 0.091 Uiso 1 1 calc R U . . . H17B H 0.108142 0.879572 0.424051 0.091 Uiso 1 1 calc R U . . . H17C H 0.156005 0.846199 0.339050 0.091 Uiso 1 1 calc R U . . . C18 C 0.1918(3) 0.2770(3) 0.44432(17) 0.0621(8) Uani 1 1 d . . . . . H18A H 0.173152 0.347175 0.472356 0.075 Uiso 0.696(17) 1 calc R U P A 1 H18B H 0.279738 0.264611 0.445320 0.075 Uiso 0.696(17) 1 calc R U P A 1 H18C H 0.219590 0.351278 0.462137 0.075 Uiso 0.304(17) 1 calc R U P A 2 H18D H 0.257508 0.221973 0.450495 0.075 Uiso 0.304(17) 1 calc R U P A 2 C19 C -0.0861(3) 0.5008(3) 0.4140(2) 0.0571(7) Uani 1 1 d . . . . . H19 H -0.152108 0.450834 0.411346 0.069 Uiso 1 1 calc R U . . . C20 C -0.0451(3) 0.5396(4) 0.4861(2) 0.0701(9) Uani 1 1 d . . . . . H20 H -0.083199 0.515422 0.532734 0.084 Uiso 1 1 calc R U . . . C21 C 0.0045(4) 0.1748(4) 0.4367(2) 0.0782(11) Uani 1 1 d . . . . . H21A H -0.053336 0.227408 0.460631 0.094 Uiso 0.696(17) 1 calc R U P A 1 H21B H -0.031010 0.099004 0.437017 0.094 Uiso 0.696(17) 1 calc R U P A 1 H21C H -0.082726 0.184203 0.445735 0.094 Uiso 0.304(17) 1 calc R U P A 2 H21D H 0.024224 0.094762 0.443490 0.094 Uiso 0.304(17) 1 calc R U P A 2 C22 C 0.1233(8) 0.1760(7) 0.4810(3) 0.066(2) Uani 0.696(17) 1 d . . P A 1 H22A H 0.167998 0.105428 0.473112 0.079 Uiso 0.696(17) 1 calc R U P A 1 H22B H 0.110054 0.187340 0.537693 0.079 Uiso 0.696(17) 1 calc R U P A 1 C22A C 0.0674(15) 0.2370(16) 0.4905(6) 0.059(4) Uani 0.304(17) 1 d . . P A 2 H22C H 0.087307 0.191411 0.537021 0.070 Uiso 0.304(17) 1 calc R U P A 2 H22D H 0.019941 0.302585 0.507410 0.070 Uiso 0.304(17) 1 calc R U P A 2 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 0.0843(5) 0.0467(4) 0.0539(4) -0.0101(3) -0.0020(3) -0.0137(3) O1 0.0741(12) 0.0481(11) 0.0317(8) 0.0063(7) 0.0019(8) -0.0036(10) O2 0.0565(10) 0.0639(12) 0.0324(8) 0.0053(8) -0.0018(7) 0.0057(9) N1 0.0332(8) 0.0362(10) 0.0338(9) 0.0004(7) 0.0035(7) -0.0023(8) N2 0.0354(9) 0.0439(12) 0.0359(9) -0.0011(8) 0.0010(7) 0.0052(8) N3 0.0491(10) 0.0376(11) 0.0291(8) 0.0005(7) -0.0007(8) -0.0015(8) N4 0.0398(9) 0.0430(11) 0.0387(10) -0.0015(8) -0.0029(8) -0.0100(9) C1 0.0355(10) 0.0297(11) 0.0322(10) -0.0036(8) 0.0005(8) 0.0038(9) C2 0.0318(9) 0.0377(12) 0.0346(10) -0.0044(9) -0.0045(8) -0.0036(9) C3 0.0352(10) 0.0340(11) 0.0323(9) -0.0003(8) -0.0058(8) -0.0013(9) C4 0.0305(9) 0.0304(11) 0.0397(11) 0.0009(8) -0.0020(8) -0.0009(9) C5 0.0333(10) 0.0322(11) 0.0383(10) -0.0027(9) -0.0018(9) 0.0008(8) C6 0.0351(10) 0.0419(13) 0.0390(11) -0.0034(10) 0.0010(9) 0.0119(10) C7 0.0388(11) 0.0536(16) 0.0378(11) 0.0024(11) -0.0014(9) 0.0060(11) C8 0.0403(11) 0.0397(13) 0.0439(12) -0.0045(10) -0.0091(10) -0.0045(10) C9 0.0500(12) 0.0462(14) 0.0344(10) -0.0067(9) -0.0122(10) 0.0011(11) C10 0.0410(11) 0.0485(15) 0.0430(12) -0.0111(10) 0.0016(10) 0.0068(11) C11 0.0343(10) 0.0385(13) 0.0608(15) -0.0044(11) -0.0014(10) -0.0045(10) C12 0.0450(12) 0.0561(16) 0.0469(13) 0.0034(11) 0.0143(11) -0.0040(12) C13 0.0369(11) 0.0415(14) 0.0701(17) 0.0010(12) 0.0129(11) -0.0046(10) C14 0.0400(12) 0.0530(16) 0.0522(14) -0.0045(12) -0.0088(10) 0.0046(11) C15 0.0419(12) 0.0528(16) 0.0542(15) -0.0034(12) -0.0007(11) -0.0140(12) C16 0.0594(15) 0.072(2) 0.0382(12) -0.0055(13) 0.0022(11) -0.0004(15) C17 0.0514(14) 0.0417(15) 0.090(2) -0.0111(15) 0.0039(15) 0.0072(13) C18 0.0767(19) 0.070(2) 0.0396(13) 0.0085(13) -0.0095(13) -0.0331(17) C19 0.0428(13) 0.0558(17) 0.0727(18) 0.0070(15) 0.0003(12) -0.0019(12) C20 0.0670(19) 0.091(3) 0.0526(16) 0.0128(17) 0.0145(15) -0.0096(18) C21 0.077(2) 0.087(3) 0.070(2) 0.0133(19) 0.0068(17) -0.038(2) C22 0.085(4) 0.063(4) 0.049(2) 0.007(2) 0.000(2) -0.026(4) C22A 0.068(7) 0.064(9) 0.044(5) 0.004(5) 0.006(5) -0.024(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' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 O1 H1 109.5 . . ? C1 N1 C4 119.61(17) . . ? C1 N1 C12 124.26(19) . . ? C4 N1 C12 110.88(19) . . ? C2 N2 H2 119.3 . . ? C2 N2 C10 121.3(2) . . ? C10 N2 H2 119.3 . . ? C1 N3 O1 120.32(19) . . ? C9 N3 O1 116.73(19) . . ? C9 N3 C1 122.9(2) . . ? C5 N4 C15 124.8(2) . . ? C5 N4 C18 123.1(2) . . ? C18 N4 C15 112.0(2) . . ? N1 C1 N3 119.5(2) . . ? N1 C1 C3 123.46(19) . . ? N3 C1 C3 116.95(19) . . ? O2 C2 N2 124.0(2) . . ? O2 C2 C4 119.2(2) . . ? N2 C2 C4 116.8(2) . . ? C1 C3 H3 119.0 . . ? C1 C3 C5 121.94(19) . . ? C5 C3 H3 119.0 . . ? N1 C4 C2 113.53(17) . . ? N1 C4 H4 108.7 . . ? N1 C4 C11 102.49(18) . . ? C2 C4 H4 108.7 . . ? C11 C4 C2 114.57(19) . . ? C11 C4 H4 108.7 . . ? N4 C5 C3 121.2(2) . . ? N4 C5 C8 121.2(2) . . ? C3 C5 C8 117.6(2) . . ? C7 C6 C10 120.8(2) . . ? C16 C6 C7 118.4(2) . . ? C16 C6 C10 120.8(2) . . ? C6 C7 H7 119.6 . . ? C14 C7 C6 120.9(2) . . ? C14 C7 H7 119.6 . . ? C5 C8 H8 120.5 . . ? C9 C8 C5 119.1(2) . . ? C9 C8 H8 120.5 . . ? N3 C9 C8 121.3(2) . . ? N3 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? N2 C10 C6 110.65(19) . . ? N2 C10 H10 108.2 . . ? N2 C10 C17 110.4(2) . . ? C6 C10 H10 108.2 . . ? C17 C10 C6 111.2(2) . . ? C17 C10 H10 108.2 . . ? C4 C11 H11A 111.4 . . ? C4 C11 H11B 111.4 . . ? H11A C11 H11B 109.3 . . ? C13 C11 C4 101.9(2) . . ? C13 C11 H11A 111.4 . . ? C13 C11 H11B 111.4 . . ? N1 C12 H12A 111.1 . . ? N1 C12 H12B 111.1 . . ? N1 C12 C13 103.1(2) . . ? H12A C12 H12B 109.1 . . ? C13 C12 H12A 111.1 . . ? C13 C12 H12B 111.1 . . ? C11 C13 H13A 111.1 . . ? C11 C13 H13B 111.1 . . ? C12 C13 C11 103.4(2) . . ? C12 C13 H13A 111.1 . . ? C12 C13 H13B 111.1 . . ? H13A C13 H13B 109.1 . . ? C7 C14 H14 119.8 . . ? C7 C14 C19 120.3(3) . . ? C19 C14 H14 119.8 . . ? N4 C15 H15A 111.1 . . ? N4 C15 H15B 111.1 . . ? N4 C15 C21 103.5(2) . . ? H15A C15 H15B 109.0 . . ? C21 C15 H15A 111.1 . . ? C21 C15 H15B 111.1 . . ? C6 C16 H16 119.7 . . ? C6 C16 C20 120.5(3) . . ? C20 C16 H16 119.7 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 H18A 111.1 . . ? N4 C18 H18B 111.1 . . ? N4 C18 H18C 111.8 . . ? N4 C18 H18D 111.8 . . ? N4 C18 C22 103.4(3) . . ? N4 C18 C22A 99.7(4) . . ? H18A C18 H18B 109.1 . . ? H18C C18 H18D 109.6 . . ? C22 C18 H18A 111.1 . . ? C22 C18 H18B 111.1 . . ? C22A C18 H18C 111.8 . . ? C22A C18 H18D 111.8 . . ? C14 C19 H19 120.3 . . ? C20 C19 C14 119.3(3) . . ? C20 C19 H19 120.3 . . ? C16 C20 H20 119.7 . . ? C19 C20 C16 120.6(3) . . ? C19 C20 H20 119.7 . . ? C15 C21 H21A 110.6 . . ? C15 C21 H21B 110.6 . . ? C15 C21 H21C 109.4 . . ? C15 C21 H21D 109.4 . . ? H21A C21 H21B 108.8 . . ? H21C C21 H21D 108.0 . . ? C22 C21 C15 105.6(3) . . ? C22 C21 H21A 110.6 . . ? C22 C21 H21B 110.6 . . ? C22A C21 C15 111.1(5) . . ? C22A C21 H21C 109.4 . . ? C22A C21 H21D 109.4 . . ? C18 C22 H22A 111.1 . . ? C18 C22 H22B 111.1 . . ? C21 C22 C18 103.3(5) . . ? C21 C22 H22A 111.1 . . ? C21 C22 H22B 111.1 . . ? H22A C22 H22B 109.1 . . ? C18 C22A H22C 110.7 . . ? C18 C22A H22D 110.7 . . ? C21 C22A C18 105.1(8) . . ? C21 C22A H22C 110.7 . . ? C21 C22A H22D 110.7 . . ? H22C C22A H22D 108.8 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 H1 0.8200 . ? O1 N3 1.387(3) . ? O2 C2 1.220(3) . ? N1 C1 1.349(3) . ? N1 C4 1.469(3) . ? N1 C12 1.490(3) . ? N2 H2 0.8600 . ? N2 C2 1.340(3) . ? N2 C10 1.466(3) . ? N3 C1 1.373(3) . ? N3 C9 1.350(3) . ? N4 C5 1.340(3) . ? N4 C15 1.464(3) . ? N4 C18 1.461(3) . ? C1 C3 1.391(3) . ? C2 C4 1.527(3) . ? C3 H3 0.9300 . ? C3 C5 1.402(3) . ? C4 H4 0.9800 . ? C4 C11 1.527(3) . ? C5 C8 1.427(3) . ? C6 C7 1.390(3) . ? C6 C10 1.524(4) . ? C6 C16 1.378(4) . ? C7 H7 0.9300 . ? C7 C14 1.376(4) . ? C8 H8 0.9300 . ? C8 C9 1.357(4) . ? C9 H9 0.9300 . ? C10 H10 0.9800 . ? C10 C17 1.520(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C13 1.521(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C13 1.516(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14 0.9300 . ? C14 C19 1.379(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C21 1.511(4) . ? C16 H16 0.9300 . ? C16 C20 1.390(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C18 H18D 0.9700 . ? C18 C22 1.531(6) . ? C18 C22A 1.632(12) . ? C19 H19 0.9300 . ? C19 C20 1.368(5) . ? C20 H20 0.9300 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21 H21D 0.9700 . ? C21 C22 1.494(8) . ? C21 C22A 1.348(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22A H22C 0.9700 . ? C22A H22D 0.9700 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 N3 C1 N1 -2.0(3) . . . . ? O1 N3 C1 C3 174.6(2) . . . . ? O1 N3 C9 C8 -175.2(2) . . . . ? O2 C2 C4 N1 145.7(2) . . . . ? O2 C2 C4 C11 -97.0(3) . . . . ? N1 C1 C3 C5 176.1(2) . . . . ? N1 C4 C11 C13 -37.7(2) . . . . ? N1 C12 C13 C11 -30.4(3) . . . . ? N2 C2 C4 N1 -35.3(3) . . . . ? N2 C2 C4 C11 82.0(3) . . . . ? N3 C1 C3 C5 -0.4(3) . . . . ? N4 C5 C8 C9 177.9(2) . . . . ? N4 C15 C21 C22 -26.4(5) . . . . ? N4 C15 C21 C22A 14.1(11) . . . . ? N4 C18 C22 C21 -30.2(7) . . . . ? N4 C18 C22A C21 29.0(13) . . . . ? C1 N1 C4 C2 -60.8(3) . . . . ? C1 N1 C4 C11 175.03(19) . . . . ? C1 N1 C12 C13 -147.5(2) . . . . ? C1 N3 C9 C8 2.3(4) . . . . ? C1 C3 C5 N4 -178.4(2) . . . . ? C1 C3 C5 C8 3.9(3) . . . . ? C2 N2 C10 C6 -80.0(3) . . . . ? C2 N2 C10 C17 156.5(2) . . . . ? C2 C4 C11 C13 -161.1(2) . . . . ? C3 C5 C8 C9 -4.3(4) . . . . ? C4 N1 C1 N3 167.7(2) . . . . ? C4 N1 C1 C3 -8.7(3) . . . . ? C4 N1 C12 C13 6.6(3) . . . . ? C4 C11 C13 C12 42.5(3) . . . . ? C5 N4 C15 C21 -169.7(3) . . . . ? C5 N4 C18 C22 -168.7(5) . . . . ? C5 N4 C18 C22A 155.8(8) . . . . ? C5 C8 C9 N3 1.4(4) . . . . ? C6 C7 C14 C19 -0.5(4) . . . . ? C6 C16 C20 C19 -0.1(6) . . . . ? C7 C6 C10 N2 -52.8(3) . . . . ? C7 C6 C10 C17 70.2(3) . . . . ? C7 C6 C16 C20 -0.6(4) . . . . ? C7 C14 C19 C20 -0.2(5) . . . . ? C9 N3 C1 N1 -179.4(2) . . . . ? C9 N3 C1 C3 -2.8(3) . . . . ? C10 N2 C2 O2 -10.3(4) . . . . ? C10 N2 C2 C4 170.7(2) . . . . ? C10 C6 C7 C14 -178.1(2) . . . . ? C10 C6 C16 C20 178.4(3) . . . . ? C12 N1 C1 N3 -40.2(3) . . . . ? C12 N1 C1 C3 143.3(2) . . . . ? C12 N1 C4 C2 143.7(2) . . . . ? C12 N1 C4 C11 19.5(3) . . . . ? C14 C19 C20 C16 0.4(5) . . . . ? C15 N4 C5 C3 179.0(2) . . . . ? C15 N4 C5 C8 -3.4(4) . . . . ? C15 N4 C18 C22 14.5(5) . . . . ? C15 N4 C18 C22A -21.0(8) . . . . ? C15 C21 C22 C18 35.4(7) . . . . ? C15 C21 C22A C18 -26.9(15) . . . . ? C16 C6 C7 C14 0.9(4) . . . . ? C16 C6 C10 N2 128.2(3) . . . . ? C16 C6 C10 C17 -108.8(3) . . . . ? C18 N4 C5 C3 2.6(4) . . . . ? C18 N4 C5 C8 -179.7(3) . . . . ? C18 N4 C15 C21 7.0(4) . . . . ?