#------------------------------------------------------------------------------ #$Date: 2021-09-16 01:09:30 +0300 (Thu, 16 Sep 2021) $ #$Revision: 269157 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/46/1564660.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_1564660 loop_ _publ_author_name 'Wong, Jeff Yuk Fung' 'Thomson, Christopher' 'Vilela, Filipe' 'Barker, Graeme' _publ_section_title ; Flash Chemistry Enables High Productivity Metalation-Substitution of 5-Alkyltetrazoles  ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC04176B _journal_year 2021 _chemical_formula_moiety 'C31 H29 Cl N4 O' _chemical_formula_sum 'C31 H29 Cl N4 O' _chemical_formula_weight 509.03 _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-07-15 _audit_creation_method ; Olex2 1.3 (compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132) ; _audit_update_record ; 2021-06-04 deposited with the CCDC. 2021-09-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.7597(7) _cell_length_b 14.3832(5) _cell_length_c 10.4096(4) _cell_measurement_reflns_used 9939 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 74.578 _cell_measurement_theta_min 3.072 _cell_volume 2659.04(17) _computing_cell_refinement 'SAINT V8.40A (Bruker, 2016)' _computing_data_reduction 'SAINT V8.40A (Bruker, 2016)' _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 (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0802 _diffrn_reflns_av_unetI/netI 0.0492 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 37580 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.603 _diffrn_reflns_theta_min 3.072 _diffrn_source_current 1.1 _diffrn_source_power 0.055 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.511 _exptl_absorpt_correction_T_max 0.7534 _exptl_absorpt_correction_T_min 0.5897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1375 before and 0.1019 after correction. The Ratio of minimum to maximum transmission is 0.7827. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.272 _exptl_crystal_description plate _exptl_crystal_F_000 1072 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.350 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.079 _refine_ls_abs_structure_details ; Flack x determined using 2214 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.039(16) _refine_ls_extinction_coef 0.0011(3) _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 1.195 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 338 _refine_ls_number_reflns 5421 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.195 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0735 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+8.6951P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1876 _refine_ls_wR_factor_ref 0.1885 _reflns_Friedel_coverage 0.882 _reflns_Friedel_fraction_full 0.996 _reflns_Friedel_fraction_max 0.990 _reflns_number_gt 5262 _reflns_number_total 5421 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc04176b2.cif _cod_data_source_block pca21_a _cod_database_code 1564660 _shelx_shelxl_version_number 2018/3 _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_estimated_absorpt_t_max 0.915 _shelx_estimated_absorpt_t_min 0.612 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Ternary CH refined with riding coordinates: C15(H15) 2.b Secondary CH2 refined with riding coordinates: C16(H16A,H16B) 2.c Aromatic/amide H refined with riding coordinates: C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35) 2.d Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C8(H8A,H8B,H8C) 2.e Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; TITL PCA21_a.res in Pca2(1) pca21_a.res created by SHELXL-2018/3 at 10:55:34 on 15-Jul-2020 REM Old TITL PCA21 in Pca2(1) REM SHELXT solution in Pca2(1) REM R1 0.143, Rweak 0.063, Alpha 0.027, Orientation as input REM Flack x = 0.220 ( 0.009 ) from Parsons' quotients REM Formula found by SHELXT: C32 Cl N3 O CELL 1.54178 17.7597 14.3832 10.4096 90 90 90 ZERR 4 0.0007 0.0005 0.0004 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H Cl N O UNIT 124 116 4 16 4 L.S. 10 PLAN 2 SIZE 0.06 0.18 0.36 TEMP -173.15 CONF HTAB O1 N3 BOND $H LIST 6 fmap 2 MORE -1 ACTA REM REM REM WGHT 0.000000 8.695101 EXTI 0.001106 FVAR 0.18121 CL1 3 0.308147 0.853242 0.907529 11.00000 0.07158 0.03483 = 0.04568 -0.00403 0.02584 0.00496 O1 5 0.376966 0.710721 0.240403 11.00000 0.02945 0.02495 = 0.02348 0.00234 -0.00241 0.00446 AFIX 147 H1 2 0.374002 0.761798 0.279202 11.00000 -1.50000 AFIX 0 N1 4 0.487884 0.879339 0.580956 11.00000 0.03022 0.01988 = 0.02632 0.00019 0.00153 0.00256 N2 4 0.442071 0.912834 0.492602 11.00000 0.03543 0.02575 = 0.02176 0.00042 -0.00050 0.00038 N3 4 0.412821 0.839269 0.433454 11.00000 0.03256 0.02284 = 0.03291 -0.00614 -0.00323 0.00103 C4 1 0.443716 0.763175 0.487798 11.00000 0.02348 0.02059 = 0.02703 -0.00015 0.00039 -0.00077 N5 4 0.491062 0.785676 0.581088 11.00000 0.03109 0.02020 = 0.02423 0.00051 0.00519 0.00113 C6 1 0.535948 0.938000 0.665732 11.00000 0.03716 0.02120 = 0.01391 0.00005 -0.00290 -0.00225 C7 1 0.528597 0.894898 0.799619 11.00000 0.05374 0.03082 = 0.01791 -0.00217 0.00349 -0.00343 AFIX 137 H7A 2 0.475362 0.892669 0.824212 11.00000 -1.50000 H7B 2 0.556493 0.932725 0.861798 11.00000 -1.50000 H7C 2 0.549229 0.831710 0.798552 11.00000 -1.50000 AFIX 0 C8 1 0.502622 1.036514 0.664363 11.00000 0.04716 0.02669 = 0.02169 -0.00430 0.00133 -0.00030 AFIX 137 H8A 2 0.504266 1.061339 0.576735 11.00000 -1.50000 H8B 2 0.532047 1.076720 0.721430 11.00000 -1.50000 H8C 2 0.450285 1.034351 0.694050 11.00000 -1.50000 AFIX 0 C9 1 0.615806 0.937401 0.615010 11.00000 0.03825 0.02188 = 0.01659 0.00361 -0.00264 -0.00371 C10 1 0.670889 0.983665 0.686630 11.00000 0.04675 0.03135 = 0.01780 0.00210 -0.00738 -0.00499 AFIX 43 H10 2 0.657577 1.014207 0.764297 11.00000 -1.20000 AFIX 0 C11 1 0.744769 0.984989 0.644455 11.00000 0.04843 0.04115 = 0.01862 0.00180 -0.01212 -0.01180 AFIX 43 H11 2 0.781901 1.016087 0.694148 11.00000 -1.20000 AFIX 0 C12 1 0.765436 0.941755 0.531085 11.00000 0.03509 0.03718 = 0.03542 0.01136 -0.00567 -0.00722 AFIX 43 H12 2 0.816230 0.943919 0.502627 11.00000 -1.20000 AFIX 0 C13 1 0.711925 0.895581 0.459778 11.00000 0.04211 0.03421 = 0.01263 -0.00542 0.00301 -0.00022 AFIX 43 H13 2 0.725718 0.865253 0.382196 11.00000 -1.20000 AFIX 0 C14 1 0.637335 0.893491 0.501893 11.00000 0.04120 0.02667 = 0.02103 -0.00019 0.00099 -0.00641 AFIX 43 H14 2 0.600633 0.861490 0.452367 11.00000 -1.20000 AFIX 0 C15 1 0.423223 0.665663 0.451853 11.00000 0.02474 0.02006 = 0.02747 0.00036 -0.00330 0.00058 AFIX 13 H15 2 0.459049 0.622122 0.495132 11.00000 -1.20000 AFIX 0 C16 1 0.342835 0.645016 0.500673 11.00000 0.02831 0.02988 = 0.03142 0.00759 -0.00670 0.00039 AFIX 23 H16A 2 0.307065 0.689575 0.461558 11.00000 -1.20000 H16B 2 0.327883 0.581553 0.474121 11.00000 -1.20000 AFIX 0 C17 1 0.338995 0.652671 0.644854 11.00000 0.02348 0.02904 = 0.03384 0.00373 0.00349 0.00001 C18 1 0.323510 0.738312 0.702493 11.00000 0.02990 0.02806 = 0.03852 0.00719 0.00979 0.00228 AFIX 43 H18 2 0.311002 0.790756 0.651282 11.00000 -1.20000 AFIX 0 C19 1 0.326604 0.746034 0.836079 11.00000 0.03239 0.02885 = 0.03617 -0.00060 0.01163 0.00102 C20 1 0.342102 0.671434 0.913735 11.00000 0.02527 0.04104 = 0.03045 -0.00055 0.00865 0.00202 AFIX 43 H20 2 0.344060 0.678105 1.004469 11.00000 -1.20000 AFIX 0 C21 1 0.354952 0.585184 0.855470 11.00000 0.02737 0.03395 = 0.03860 0.00781 0.00345 0.00487 AFIX 43 H21 2 0.364369 0.532058 0.907260 11.00000 -1.20000 AFIX 0 C22 1 0.354051 0.576578 0.722274 11.00000 0.02450 0.02856 = 0.04026 0.00121 0.00160 0.00147 AFIX 43 H22 2 0.363874 0.517846 0.684036 11.00000 -1.20000 AFIX 0 C23 1 0.430206 0.652566 0.303597 11.00000 0.02423 0.02573 = 0.02360 0.00240 -0.00214 0.00059 C24 1 0.510712 0.676291 0.257873 11.00000 0.02711 0.02008 = 0.03053 -0.00392 0.00256 -0.00020 C25 1 0.574312 0.664665 0.335085 11.00000 0.03211 0.02374 = 0.03139 -0.00546 0.00124 0.00273 AFIX 43 H25 2 0.568557 0.642546 0.420515 11.00000 -1.20000 AFIX 0 C26 1 0.645225 0.684738 0.289411 11.00000 0.02936 0.02579 = 0.03751 -0.00675 -0.00736 -0.00045 AFIX 43 H26 2 0.687720 0.676575 0.343682 11.00000 -1.20000 AFIX 0 C27 1 0.655166 0.716682 0.165223 11.00000 0.02911 0.03030 = 0.04406 0.00124 0.00861 -0.00111 AFIX 43 H27 2 0.704082 0.731169 0.134184 11.00000 -1.20000 AFIX 0 C28 1 0.592786 0.727227 0.086849 11.00000 0.04328 0.04156 = 0.03661 0.01574 0.00227 -0.00254 AFIX 43 H28 2 0.599222 0.748475 0.001139 11.00000 -1.20000 AFIX 0 C29 1 0.521013 0.707234 0.131578 11.00000 0.03322 0.04064 = 0.03215 0.00458 0.00231 0.00231 AFIX 43 H29 2 0.478799 0.714549 0.076444 11.00000 -1.20000 AFIX 0 C30 1 0.410327 0.552248 0.267290 11.00000 0.02794 0.02472 = 0.02601 0.00124 0.00352 -0.00076 C31 1 0.459127 0.480620 0.296626 11.00000 0.02835 0.02546 = 0.04202 -0.00815 -0.00003 -0.00092 AFIX 43 H31 2 0.504489 0.493651 0.341517 11.00000 -1.20000 AFIX 0 C32 1 0.442616 0.389216 0.261103 11.00000 0.03782 0.02648 = 0.03762 -0.01098 -0.00171 0.00445 AFIX 43 H32 2 0.477082 0.340726 0.280645 11.00000 -1.20000 AFIX 0 C33 1 0.376688 0.369321 0.198018 11.00000 0.03769 0.02846 = 0.03977 -0.00753 0.00354 -0.00589 AFIX 43 H33 2 0.365659 0.307154 0.173598 11.00000 -1.20000 AFIX 0 C34 1 0.326282 0.439853 0.169990 11.00000 0.03120 0.03299 = 0.04171 0.00123 -0.00707 -0.00710 AFIX 43 H34 2 0.280440 0.426328 0.126831 11.00000 -1.20000 AFIX 0 C35 1 0.343376 0.531273 0.205733 11.00000 0.02756 0.02994 = 0.03661 -0.00197 0.00027 -0.00024 AFIX 43 H35 2 0.308523 0.579605 0.187475 11.00000 -1.20000 AFIX 0 HKLF 4 REM PCA21_a.res in Pca2(1) REM wR2 = 0.1885, GooF = S = 1.195, Restrained GooF = 1.195 for all data REM R1 = 0.0735 for 5262 Fo > 4sig(Fo) and 0.0749 for all 5421 data REM 338 parameters refined using 1 restraints END WGHT 0.0000 8.6953 REM Highest difference peak 0.350, deepest hole -0.393, 1-sigma level 0.079 Q1 1 0.6993 0.8010 0.4029 11.00000 0.05 0.35 Q2 1 0.2401 0.7041 0.7003 11.00000 0.05 0.32 ; _shelx_res_checksum 20132 _shelx_hkl_file ; 0 0 -1 0.02 0.10 0 0 1 0.02 0.09 0 0 1 -0.03 0.09 0 0 2 316.58 24.68 0 0 -2 334.24 26.64 0 0 2 306.24 24.68 0 0 2 304.84 24.55 0 0 3 0.34 0.32 0 0 3 -0.05 0.22 0 0 3 0.19 0.35 0 0 -3 -0.04 0.27 0 0 4 215.59 17.82 0 0 4 227.21 17.59 0 0 4 210.10 17.85 0 0 5 -0.01 0.31 0 0 -5 0.04 0.42 0 0 5 -0.35 0.54 0 0 6 49.95 5.16 0 0 -6 49.66 5.00 0 0 6 52.31 4.73 0 0 7 0.03 0.24 0 0 -7 0.09 0.36 0 0 -7 0.00 0.29 0 0 7 -1.77 1.27 0 0 7 -0.07 0.43 0 0 -7 -0.17 0.79 0 0 -8 12.36 1.45 0 0 -8 14.19 1.74 0 0 -8 12.54 3.00 0 0 8 13.56 1.54 0 0 8 14.86 1.51 0 0 8 15.70 2.10 0 0 9 0.10 0.31 0 0 9 -0.21 0.75 0 0 9 -0.38 0.29 0 0 -9 0.14 0.35 0 0 -9 0.18 0.35 0 0 10 13.00 1.43 0 0 -11 0.01 0.32 0 0 11 0.14 0.35 0 0 11 0.03 0.27 0 0 11 0.19 0.37 0 0 -12 16.82 1.59 0 0 12 18.96 1.72 0 0 13 -0.08 0.15 0 1 0 4.29 0.42 0 1 0 4.34 0.39 0 -1 0 4.40 0.41 0 -1 0 4.64 0.43 0 -1 0 4.08 0.39 0 -1 1 0.09 0.10 0 1 -1 0.29 0.18 0 1 1 0.22 0.16 0 -1 -1 0.03 0.14 0 1 1 0.01 0.10 0 -1 1 0.22 0.20 0 -1 1 0.02 0.12 0 1 1 0.26 0.18 0 1 -1 0.16 0.10 0 -1 1 0.04 0.13 0 1 2 989.17 78.67 0 -1 2 1000.00 78.68 0 -1 3 7.05 0.98 0 -1 3 5.40 0.87 0 -1 3 4.02 0.68 0 1 3 7.08 0.99 0 -1 -3 6.67 0.98 0 1 -3 6.57 0.99 0 1 3 5.52 0.89 0 1 4 106.92 9.13 0 -1 4 99.40 9.05 0 -1 4 112.49 8.84 0 -1 4 106.43 9.04 0 1 -4 117.96 10.01 0 1 4 106.32 9.08 0 1 4 110.26 8.86 0 -1 4 102.35 8.83 0 -1 -5 34.60 3.51 0 1 -5 33.50 3.56 0 -1 5 15.33 1.77 0 1 5 15.51 1.75 0 1 -6 4.46 1.25 0 1 6 5.74 1.92 0 -1 -6 4.54 1.20 0 1 6 5.04 1.01 0 -1 6 4.85 1.39 0 -1 6 5.86 1.09 0 1 -7 1.80 0.54 0 -1 7 0.90 0.64 0 1 -7 1.64 0.60 0 -1 7 1.73 0.51 0 1 7 1.34 0.61 0 -1 -7 2.40 0.57 0 1 -7 1.68 0.50 0 1 -7 2.33 1.27 0 -1 -7 2.69 0.84 0 -1 7 1.96 1.35 0 1 7 0.83 0.36 0 -1 7 1.47 0.41 0 1 8 10.28 1.66 0 -1 -8 9.00 1.16 0 1 -8 9.22 1.16 0 -1 8 12.07 1.74 0 1 8 9.26 1.17 0 1 8 9.06 1.10 0 1 -8 9.44 2.79 0 -1 -8 9.49 1.42 0 -1 8 9.08 1.09 0 -1 8 8.70 1.13 0 -1 9 19.24 1.83 0 -1 -9 17.83 1.86 0 1 9 18.58 1.83 0 -1 -9 18.60 2.16 0 1 -9 17.22 1.86 0 1 9 16.27 1.77 0 -1 9 16.00 1.74 0 1 -10 5.72 1.46 0 -1 10 3.42 0.71 0 -1 10 3.41 0.73 0 -1 -10 4.03 0.64 0 1 10 3.93 1.57 0 -1 -10 2.79 0.80 0 1 10 3.05 0.97 0 1 10 2.59 0.57 0 -1 10 6.79 2.09 0 1 11 0.26 0.31 0 -1 11 0.70 0.36 0 1 11 0.11 0.36 0 -1 -11 0.74 0.38 0 -1 11 0.25 0.29 0 -1 11 0.12 0.38 0 1 -11 0.45 0.38 0 1 12 4.87 0.68 0 -1 -12 4.49 0.65 0 -1 12 5.00 0.65 0 1 -12 4.57 0.67 0 2 0 57.87 4.38 0 2 0 52.25 4.33 0 -2 0 55.41 4.39 0 -2 0 50.45 4.33 0 2 1 0.15 0.18 0 -2 1 0.15 0.15 0 2 1 0.09 0.13 0 -2 -1 0.46 0.22 0 -2 1 0.35 0.26 0 -2 1 0.07 0.19 0 2 -1 0.22 0.26 0 2 -1 0.18 0.15 0 -2 2 200.36 15.91 0 -2 2 206.12 16.13 0 2 2 200.87 16.12 0 -2 2 196.31 15.95 0 2 2 190.92 15.87 0 -2 -2 183.06 15.56 0 -2 2 201.50 16.15 0 2 -2 203.50 15.68 0 2 3 5.27 0.92 0 2 -3 5.16 0.90 0 2 3 4.33 0.82 0 -2 3 5.00 0.84 0 -2 3 3.79 0.58 0 -2 3 2.67 0.65 0 -2 4 25.56 2.41 0 2 4 23.06 2.66 0 -2 4 22.39 2.32 0 -2 4 24.00 2.85 0 2 4 26.47 2.40 0 -2 4 25.04 2.59 0 2 -4 27.33 2.89 0 2 -5 9.75 1.59 0 2 5 4.91 0.91 0 -2 5 5.08 0.95 0 -2 6 81.51 6.92 0 2 -6 81.72 7.72 0 -2 6 72.34 7.79 0 2 6 79.38 6.82 0 2 -7 7.91 1.94 0 2 -7 5.62 0.90 0 -2 -7 5.75 1.13 0 -2 7 4.77 0.70 0 2 7 4.77 0.73 0 -2 7 5.49 0.96 0 -2 -7 6.11 0.87 0 -2 -8 16.81 2.07 0 -2 8 16.20 2.25 0 -2 8 15.18 3.53 0 -2 8 18.39 1.84 0 2 8 15.19 1.64 0 -2 -8 15.73 1.82 0 -2 8 15.88 1.64 0 2 -8 16.48 1.78 0 2 -8 20.81 2.02 0 2 8 16.49 2.18 0 2 9 5.73 0.91 0 -2 -9 7.47 1.05 0 -2 -9 7.32 1.35 0 -2 9 6.30 0.91 0 2 9 4.38 1.31 0 -2 9 8.20 1.01 0 2 -9 7.45 1.07 0 -2 10 2.09 0.54 0 2 -10 2.95 0.71 0 -2 -10 2.59 0.65 0 -2 10 3.14 0.64 0 2 10 2.75 0.67 0 -2 -10 3.59 0.62 0 -2 10 3.50 0.73 0 -2 10 5.38 1.81 0 2 10 2.46 1.38 0 2 11 0.46 0.36 0 -2 -11 1.16 0.41 0 -2 11 0.75 0.35 0 -2 11 0.77 0.35 0 -2 11 0.43 0.51 0 2 -11 0.66 0.36 0 -2 -11 0.56 0.33 0 -2 12 5.62 0.83 0 2 12 6.01 0.90 0 -2 -12 6.04 0.75 0 2 -12 6.41 0.83 0 2 12 6.50 0.78 0 -3 0 521.25 42.19 0 -3 0 535.81 42.30 0 3 0 545.71 42.27 0 3 -1 1.98 0.45 0 3 1 1.27 0.30 0 3 1 1.55 0.40 0 -3 1 0.99 0.32 0 3 -1 1.32 0.34 0 -3 2 563.01 45.21 0 3 -2 621.06 46.85 0 3 2 550.89 45.12 0 -3 -2 561.56 46.84 0 -3 2 598.06 45.35 0 3 2 530.96 45.43 0 -3 2 609.80 45.21 0 3 -2 590.61 47.10 0 3 3 0.56 0.45 0 -3 3 0.69 0.47 0 3 -3 1.05 0.64 0 -3 3 0.63 0.25 0 3 3 0.33 0.26 0 -3 -3 1.30 0.52 0 -3 3 0.41 0.30 0 -3 3 0.64 0.46 0 3 -4 11.78 1.66 0 -3 4 6.08 0.91 0 3 4 6.86 0.91 0 -3 4 6.70 1.01 0 -3 -4 10.81 1.90 0 -3 4 6.07 1.14 0 -3 5 0.56 0.50 0 -3 5 1.50 0.79 0 3 5 0.11 0.32 0 3 -5 0.76 0.59 0 -3 6 130.71 10.87 0 3 6 129.76 10.75 0 -3 6 123.29 11.19 0 3 -6 131.26 11.90 0 -3 -6 135.51 12.18 0 -3 -7 5.33 1.18 0 3 7 3.92 0.73 0 -3 7 6.01 0.79 0 -3 -7 5.28 0.83 0 -3 7 4.53 0.71 0 3 -7 5.62 0.88 0 3 -7 7.01 2.10 0 -3 7 4.08 1.54 0 3 8 10.97 1.69 0 3 8 8.24 1.38 0 -3 -8 7.38 1.05 0 -3 -8 6.80 1.31 0 -3 8 7.31 2.24 0 3 -8 5.18 1.03 0 3 -8 6.36 1.07 0 -3 8 9.14 1.12 0 -3 8 8.88 1.73 0 -3 8 9.81 1.21 0 -3 8 8.25 1.11 0 -3 9 0.40 0.87 0 -3 -9 0.42 0.59 0 3 -9 0.00 0.43 0 -3 9 1.12 0.44 0 3 9 1.15 0.78 0 -3 9 0.68 0.36 0 -3 9 0.67 0.40 0 3 9 0.74 0.40 0 3 -9 1.14 0.52 0 -3 -9 0.99 0.45 0 3 10 20.49 1.90 0 -3 10 18.52 1.93 0 3 10 19.45 3.01 0 -3 -10 19.19 2.26 0 -3 -10 19.71 1.94 0 -3 10 19.02 1.81 0 -3 10 16.82 1.84 0 -3 -10 20.48 1.84 0 3 -10 18.25 1.93 0 -3 -11 0.29 0.31 0 3 11 0.08 0.30 0 3 -11 0.04 0.28 0 -3 -11 0.56 0.30 0 -3 11 0.10 0.28 0 -3 11 0.17 0.28 0 -3 -12 0.72 0.27 0 3 12 0.48 0.34 0 3 -12 0.58 0.29 0 3 12 0.28 0.44 0 -3 12 0.46 0.24 0 4 0 161.48 12.26 0 -4 0 149.61 12.39 0 -4 0 143.51 12.22 0 4 0 159.41 12.34 0 4 -1 3.06 0.73 0 -4 1 0.97 0.33 0 4 1 1.39 0.32 0 -4 1 1.78 0.43 0 4 -1 2.15 0.48 0 4 -1 1.53 0.40 0 4 1 2.02 0.45 0 -4 2 801.56 63.40 0 4 2 789.22 63.28 0 -4 -2 827.64 68.57 0 -4 2 884.13 63.58 0 -4 2 846.59 63.44 0 4 2 683.38 63.56 0 4 -2 905.61 68.62 0 4 -3 0.11 0.36 0 -4 3 0.57 0.43 0 -4 3 0.22 0.29 0 4 3 0.14 0.26 0 -4 -3 0.40 0.40 0 -4 3 0.49 0.34 0 4 3 0.80 0.56 0 4 3 0.18 0.29 0 -4 4 10.78 1.39 0 -4 -4 7.59 1.40 0 4 4 10.27 1.25 0 -4 4 12.54 1.60 0 4 -4 8.94 1.50 0 -4 -5 1.27 1.21 0 4 -5 1.59 0.91 0 -4 5 0.77 0.46 0 4 5 1.10 0.51 0 -4 6 39.95 3.41 0 -4 6 39.23 3.44 0 -4 6 40.11 4.28 0 4 6 42.83 3.84 0 4 -6 38.86 4.58 0 -4 -6 41.08 3.89 0 -4 6 36.72 3.42 0 -4 6 41.43 3.96 0 4 6 40.81 4.08 0 -4 6 39.94 3.40 0 -4 7 0.37 0.28 0 -4 -7 0.78 0.36 0 4 -7 0.66 0.34 0 -4 -7 0.12 0.41 0 4 7 0.23 0.30 0 4 7 0.42 0.47 0 -4 7 0.76 1.01 0 4 7 0.22 1.10 0 -4 7 0.29 0.29 0 -4 7 0.60 0.31 0 -4 -7 0.21 0.59 0 -4 7 0.53 0.61 0 -4 -8 5.85 1.31 0 4 -8 7.09 1.02 0 4 -8 7.66 1.15 0 -4 -8 6.93 1.03 0 -4 8 7.36 1.70 0 4 8 7.17 1.45 0 -4 8 4.81 0.88 0 -4 8 7.57 0.94 0 4 8 6.16 0.88 0 -4 8 5.58 0.85 0 4 -9 0.33 0.45 0 -4 9 -0.37 1.28 0 -4 -9 0.66 0.66 0 -4 9 -1.05 3.72 0 -4 9 0.07 0.37 0 -4 -9 0.58 0.41 0 -4 9 0.31 0.45 0 4 -9 0.46 0.40 0 4 9 0.14 0.75 0 4 9 0.42 0.35 0 -4 9 0.21 0.30 0 4 -10 7.85 1.03 0 4 10 7.85 1.02 0 -4 10 8.11 0.94 0 -4 -10 6.22 1.29 0 -4 10 7.23 1.00 0 -4 -10 8.12 0.99 0 -4 -10 8.39 1.01 0 4 11 1.45 0.46 0 -4 -11 0.67 0.34 0 -4 -11 1.48 0.41 0 -4 11 2.84 0.67 0 4 -11 1.45 0.44 0 -4 11 1.73 0.39 0 -4 -12 0.93 0.24 0 4 -12 0.87 0.32 0 -4 12 0.83 0.24 0 4 12 0.69 0.43 0 4 12 0.93 0.31 0 5 0 488.26 38.81 0 -5 0 485.04 38.97 0 5 0 495.04 38.88 0 5 -1 -0.08 0.20 0 -5 -1 0.38 0.36 0 5 -1 0.31 0.38 0 5 1 0.30 0.32 0 5 1 0.11 0.22 0 5 -1 0.07 0.23 0 -5 1 0.22 0.24 0 -5 1 0.22 0.26 0 5 2 25.65 2.37 0 5 2 23.80 2.13 0 -5 2 23.78 2.27 0 5 -2 25.96 2.41 0 -5 -2 25.15 2.41 0 5 -2 25.05 2.75 0 -5 2 25.26 2.34 0 5 3 1.42 0.40 0 5 -3 3.43 1.10 0 -5 3 1.18 0.47 0 -5 -3 3.37 0.79 0 5 3 2.34 0.71 0 5 -3 2.11 0.64 0 -5 -4 43.02 4.09 0 5 4 41.98 4.05 0 5 4 42.96 3.79 0 5 -4 44.40 4.59 0 -5 4 45.44 4.21 0 -5 4 42.20 4.11 0 -5 5 5.05 0.74 0 5 5 7.19 1.22 0 -5 5 4.72 1.05 0 5 -5 9.75 1.89 0 5 5 4.57 0.90 0 -5 6 36.53 3.88 0 -5 6 31.80 2.90 0 -5 6 32.87 3.43 0 -5 6 32.38 2.90 0 5 6 34.62 3.28 0 -5 -6 37.71 3.58 0 -5 6 31.98 2.88 0 5 -6 35.17 4.46 0 -5 -6 31.46 3.52 0 5 6 33.60 3.62 0 5 7 11.13 1.19 0 5 -7 18.94 3.97 0 -5 7 8.29 1.15 0 5 7 8.38 1.47 0 5 -7 16.80 1.74 0 -5 -7 16.07 2.18 0 -5 7 11.93 1.11 0 -5 -7 15.32 1.64 0 -5 7 8.25 1.09 0 -5 8 0.74 0.41 0 5 -8 0.71 0.38 0 5 8 0.86 0.40 0 -5 -8 0.99 0.53 0 -5 -8 1.00 0.45 0 -5 -8 0.22 0.73 0 -5 8 1.40 1.54 0 -5 8 0.32 0.32 0 5 -8 1.23 0.59 0 -5 8 0.60 1.05 0 -5 8 0.36 0.34 0 -5 9 7.94 0.95 0 -5 9 3.99 1.98 0 5 -9 8.41 1.27 0 5 9 7.38 1.04 0 5 -9 10.03 1.21 0 -5 -9 10.40 1.19 0 -5 9 9.78 1.09 0 5 9 4.89 1.47 0 -5 -9 8.05 1.51 0 5 10 5.12 0.80 0 -5 -10 4.95 0.80 0 5 -10 5.80 0.99 0 -5 10 5.02 0.69 0 5 -10 4.71 0.80 0 -5 -10 3.79 1.06 0 -5 10 4.13 0.79 0 -5 -10 4.74 0.75 0 5 -11 5.46 0.77 0 -5 -11 6.12 0.77 0 5 11 4.05 0.99 0 -5 11 5.12 0.63 0 5 -12 2.06 0.43 0 -5 -12 2.10 0.45 0 -5 -12 2.35 0.46 0 5 12 1.94 0.42 0 6 0 6.86 0.81 0 6 0 6.57 0.92 0 -6 0 5.05 1.00 0 6 1 0.61 0.34 0 6 -1 0.42 0.35 0 6 -1 0.70 0.51 0 -6 1 0.90 0.34 0 -6 1 0.29 0.42 0 6 -1 0.86 0.39 0 6 1 1.00 0.35 0 -6 2 152.65 13.05 0 6 2 154.14 13.12 0 6 2 173.65 13.04 0 -6 2 161.87 13.19 0 6 -2 179.97 14.51 0 -6 -2 169.49 14.42 0 6 -2 184.36 15.06 0 6 3 3.43 0.81 0 6 -3 3.67 0.86 0 -6 3 3.55 0.79 0 6 3 3.04 0.60 0 6 -3 5.25 1.25 0 -6 -3 5.42 1.09 0 6 4 76.66 6.65 0 -6 4 77.20 6.73 0 -6 -4 74.14 6.49 0 6 4 76.08 6.29 0 -6 4 69.18 6.63 0 -6 5 2.02 0.43 0 6 -5 1.66 1.10 0 -6 -5 0.90 0.52 0 -6 5 1.31 0.36 0 6 5 0.96 0.73 0 -6 -5 0.82 0.92 0 -6 5 0.42 0.62 0 -6 5 1.07 0.36 0 -6 5 1.27 0.84 0 6 5 0.80 0.49 0 -6 6 47.53 4.15 0 -6 6 48.88 4.23 0 6 6 54.46 4.63 0 -6 6 50.39 4.40 0 -6 6 54.01 4.25 0 -6 6 54.26 4.87 0 6 -6 42.57 3.89 0 6 6 46.45 4.26 0 -6 6 45.54 4.22 0 -6 -6 45.04 3.95 0 -6 -6 46.11 4.39 0 6 6 50.96 5.09 0 -6 -7 0.80 0.40 0 -6 7 0.08 1.35 0 -6 -7 0.41 0.99 0 6 7 0.41 0.56 0 -6 7 -1.00 0.93 0 -6 -7 0.50 0.64 0 -6 7 0.55 0.34 0 6 7 1.46 0.44 0 6 -7 1.67 0.53 0 -6 7 0.89 0.50 0 -6 8 81.02 7.57 0 6 8 83.93 7.09 0 -6 8 74.03 6.52 0 6 -8 80.12 6.45 0 -6 -8 78.02 6.34 0 6 8 77.97 6.55 0 6 -8 73.66 6.32 0 -6 8 75.96 6.41 0 -6 -8 69.12 6.80 0 -6 -8 74.31 6.27 0 -6 -9 9.07 1.40 0 6 9 8.37 1.17 0 6 -9 8.23 1.09 0 6 -9 7.53 1.20 0 6 9 6.16 1.70 0 -6 9 8.69 1.16 0 -6 -10 5.45 0.76 0 -6 10 6.26 0.80 0 -6 -10 6.63 0.88 0 6 -10 6.80 1.19 0 -6 -10 4.28 1.11 0 6 10 8.05 0.98 0 6 -10 4.54 0.80 0 -6 -11 6.51 0.74 0 -6 11 4.90 0.76 0 6 11 5.83 0.75 0 6 -11 6.84 0.84 0 -6 -12 0.09 0.19 0 6 12 0.02 0.19 0 -6 -12 0.02 0.21 0 6 -12 -0.03 0.20 0 7 0 31.91 2.75 0 7 0 29.01 2.88 0 7 1 4.76 0.86 0 7 -1 6.20 1.65 0 7 1 4.73 0.73 0 7 -1 3.98 0.85 0 7 2 60.50 5.32 0 -7 2 58.27 5.12 0 7 2 62.28 5.07 0 7 -2 73.76 7.16 0 7 -2 78.56 6.61 0 7 -3 5.91 1.17 0 7 -3 7.53 1.61 0 -7 -3 8.14 1.32 0 -7 3 4.15 0.94 0 7 3 3.94 0.70 0 -7 -4 120.43 10.43 0 -7 4 117.64 10.30 0 7 4 136.32 10.64 0 -7 4 115.06 10.06 0 7 4 126.72 10.10 0 -7 4 114.74 9.90 0 7 -4 126.81 11.46 0 -7 4 128.31 9.96 0 -7 -4 124.47 10.56 0 -7 -4 124.79 10.13 0 -7 -5 0.06 0.50 0 7 5 0.29 0.46 0 -7 5 0.44 0.29 0 -7 5 0.26 0.35 0 -7 5 0.50 0.27 0 -7 5 -0.19 0.62 0 -7 -5 0.47 0.69 0 7 -5 0.39 1.01 0 7 5 0.55 0.77 0 -7 -6 88.71 8.11 0 -7 6 80.24 7.13 0 7 6 96.51 7.53 0 -7 6 80.01 7.03 0 7 6 85.70 7.19 0 -7 -6 94.03 7.66 0 -7 6 90.28 7.15 0 -7 6 94.78 7.16 0 -7 6 81.85 7.13 0 -7 7 0.85 0.54 0 7 7 1.11 0.62 0 -7 7 1.32 0.43 0 7 7 1.30 0.64 0 -7 7 1.37 0.39 0 -7 7 0.07 1.42 0 -7 -7 1.87 0.49 0 -7 -7 0.59 0.81 0 -7 -7 1.81 1.06 0 7 -7 2.95 0.90 0 -7 8 6.39 0.89 0 -7 8 6.50 0.91 0 7 -8 5.55 0.96 0 7 8 5.91 0.90 0 -7 8 5.48 0.93 0 -7 8 5.75 0.77 0 7 -8 5.33 1.11 0 -7 -8 6.76 0.89 0 -7 -8 6.28 1.63 0 7 8 5.14 1.26 0 -7 -8 5.66 1.08 0 7 -9 2.76 0.77 0 -7 -9 2.32 0.63 0 -7 -9 3.35 0.61 0 7 -9 2.98 0.73 0 -7 9 2.21 0.49 0 7 9 2.69 0.64 0 -7 -9 1.88 0.86 0 7 -10 2.47 0.65 0 7 -10 2.28 0.64 0 -7 -10 2.59 0.60 0 -7 -10 2.26 0.51 0 -7 -10 1.58 0.80 0 -7 -11 4.72 0.65 0 -7 -11 3.97 0.61 0 7 11 5.71 0.74 0 8 0 0.48 0.50 0 8 0 0.36 0.34 0 8 -1 1.21 0.52 0 -8 1 0.99 0.58 0 8 -1 1.32 0.78 0 8 1 1.68 0.65 0 8 -2 23.09 3.14 0 8 2 27.79 2.53 0 8 2 26.54 2.79 0 8 -2 25.12 2.59 0 8 -3 -0.23 0.56 0 -8 3 0.56 0.35 0 -8 -3 0.46 0.42 0 8 3 0.47 0.36 0 -8 -3 0.26 0.58 0 8 3 0.24 0.52 0 -8 3 0.12 0.26 0 8 -3 -0.68 0.63 0 8 4 0.32 0.57 0 -8 4 0.27 0.29 0 -8 -4 0.08 0.67 0 -8 4 0.48 0.35 0 -8 -4 0.32 0.48 0 -8 4 0.20 0.27 0 8 -4 0.09 0.83 0 -8 4 0.18 0.36 0 -8 -4 0.03 0.47 0 -8 4 0.01 0.34 0 8 4 0.15 0.34 0 8 5 1.12 1.13 0 -8 5 0.78 0.45 0 -8 5 1.84 0.43 0 -8 5 1.05 0.41 0 8 5 1.12 0.57 0 8 -5 0.72 1.34 0 -8 -5 1.27 0.85 0 -8 -5 1.25 0.92 0 -8 -5 0.65 0.62 0 -8 5 1.29 0.49 0 -8 5 1.22 0.42 0 -8 5 1.87 0.55 0 8 6 2.76 0.62 0 -8 6 3.75 0.68 0 -8 6 5.04 0.72 0 -8 -6 5.04 1.19 0 -8 6 5.04 0.85 0 -8 6 2.86 0.62 0 -8 -6 5.05 1.45 0 -8 6 2.98 0.63 0 8 6 3.71 0.92 0 -8 6 3.78 0.81 0 -8 -7 0.44 0.97 0 -8 -7 3.57 0.64 0 8 7 1.21 0.47 0 -8 7 0.65 0.37 0 -8 7 3.01 0.70 0 8 -7 2.66 0.85 0 -8 7 2.43 0.55 0 -8 -7 2.52 1.15 0 8 -7 2.57 0.66 0 -8 7 1.93 0.62 0 -8 7 1.74 0.39 0 8 7 1.10 0.73 0 -8 8 6.47 1.00 0 8 -8 7.74 1.21 0 -8 -8 7.77 2.02 0 -8 -8 7.07 1.08 0 -8 -8 7.59 1.36 0 8 -8 6.86 1.14 0 -8 8 7.47 1.42 0 8 8 11.04 1.96 0 -8 -9 0.17 0.36 0 8 -9 0.97 0.42 0 8 -9 0.22 0.46 0 -8 -9 0.30 0.40 0 -8 -9 0.03 0.94 0 8 9 0.04 0.28 0 -8 -9 0.59 0.29 0 8 -10 15.58 1.66 0 -8 -10 13.60 1.98 0 8 -10 17.97 1.79 0 -8 -10 20.03 1.75 0 8 10 17.02 1.63 0 -8 -10 20.64 1.73 0 8 -11 4.48 0.59 0 8 11 3.45 0.51 0 -8 -11 3.49 0.56 0 -8 -11 3.10 0.57 0 9 0 19.95 2.92 0 -9 0 21.81 2.44 0 -9 0 19.76 2.01 0 9 0 21.60 2.15 0 -9 0 20.53 1.97 0 9 0 19.80 2.34 0 -9 0 23.60 2.03 0 9 1 0.63 0.56 0 -9 -1 0.28 0.60 0 9 1 0.54 0.40 0 -9 1 1.23 0.72 0 -9 1 0.37 0.32 0 -9 1 0.26 0.36 0 9 -1 0.47 0.52 0 -9 -1 0.87 0.45 0 9 -1 0.89 0.98 0 -9 1 0.77 0.43 0 -9 -1 0.26 0.40 0 -9 1 0.62 0.35 0 9 -2 14.09 2.64 0 -9 -2 15.86 1.57 0 9 2 15.04 1.60 0 -9 -2 14.97 2.03 0 9 -2 12.27 1.94 0 -9 2 13.72 1.49 0 -9 2 14.88 1.50 0 9 2 14.79 1.92 0 -9 2 14.44 1.47 0 9 -3 0.30 1.05 0 9 -3 0.42 0.80 0 -9 3 0.41 0.33 0 -9 3 0.90 0.42 0 -9 -3 0.26 0.44 0 -9 3 0.61 0.40 0 -9 3 0.37 0.38 0 -9 -3 -0.28 0.41 0 9 3 0.67 0.47 0 9 3 0.80 0.92 0 -9 -3 0.69 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1 0.14 0.25 -20 1 -1 0.63 0.21 -20 -1 1 0.43 0.33 -20 -1 1 0.26 0.28 -20 1 -1 0.34 0.28 -20 -1 -1 0.28 0.19 -20 1 1 0.90 0.33 -20 -1 -1 0.56 0.46 -20 -1 -1 -0.02 0.32 -20 -1 -1 0.32 0.30 -20 -1 -1 0.32 0.38 -20 1 -2 2.01 0.44 -20 1 -2 1.75 0.48 -20 -1 2 1.16 0.41 -20 -1 2 0.51 0.38 -20 -1 2 0.64 0.34 -20 1 -2 1.08 0.25 -20 1 2 1.84 0.48 -20 -1 -2 0.67 0.24 20 -1 2 1.41 0.57 -20 -1 -2 0.57 0.34 -20 1 2 2.01 0.41 -20 -1 -2 0.96 0.42 -20 -1 -2 1.10 0.36 -20 1 -3 0.13 0.18 -20 1 -3 0.00 0.24 -20 1 -3 0.06 0.22 -20 -1 3 0.46 0.28 -20 -1 3 -0.15 0.26 -20 1 3 0.02 0.17 -20 -1 -3 -0.10 0.16 -20 -1 -3 -0.24 0.26 -20 -1 -3 0.43 0.39 20 -1 3 0.17 0.20 -20 1 3 0.10 0.20 -20 1 -4 2.09 0.44 -20 -1 4 2.40 0.45 -20 1 -4 2.10 0.33 20 -1 4 2.51 0.51 -20 -1 -4 2.97 0.48 -20 -1 -4 2.53 0.44 -20 1 4 2.40 0.43 -20 -1 -4 2.53 0.39 -20 -1 5 0.77 0.28 -20 1 -5 0.53 0.20 -20 1 -5 0.18 0.20 -20 1 5 0.67 0.22 -20 -1 -5 1.15 0.27 -20 1 5 0.15 0.20 20 -1 5 0.55 0.17 -20 2 0 2.38 0.50 -20 -2 0 1.55 0.47 -20 -2 0 1.65 0.40 -20 2 0 2.12 0.42 -20 -2 0 2.12 0.47 -20 -2 0 2.59 0.53 -20 -2 0 1.72 0.34 -20 -2 1 2.26 0.41 -20 2 -1 1.13 0.42 -20 -2 1 2.20 0.57 -20 2 -1 1.00 0.36 -20 -2 1 1.95 0.47 -20 2 -1 0.53 0.45 -20 -2 1 2.91 0.54 -20 -2 -1 1.58 0.44 -20 -2 -1 2.39 0.52 -20 -2 -1 2.20 0.35 -20 2 1 1.44 0.41 -20 2 1 1.64 0.37 -20 -2 -1 1.40 0.44 -20 2 -2 5.15 0.61 -20 -2 2 6.35 0.74 -20 2 -2 5.71 0.76 -20 -2 2 5.80 0.76 -20 -2 2 5.71 0.72 -20 2 2 6.17 0.73 -20 -2 -2 5.77 0.63 20 -2 2 4.00 0.76 -20 -2 -2 5.78 0.84 -20 -2 -2 6.73 0.77 -20 -2 -2 6.11 0.84 -20 2 2 4.80 0.61 -20 -2 3 1.72 0.46 -20 -2 3 2.14 0.45 -20 -2 3 1.99 0.44 -20 2 -3 3.11 0.73 -20 -2 -3 2.24 0.48 -20 -2 -3 2.07 0.36 -20 -2 -3 2.19 0.50 -20 -2 -3 2.17 0.42 -20 -2 4 0.25 0.23 -20 2 -4 0.40 0.25 -20 -2 -4 0.02 0.16 -20 2 4 0.53 0.21 -20 -2 -4 0.27 0.35 20 -2 4 0.54 0.24 -20 -2 -4 0.26 0.23 20 -2 5 2.95 0.38 -20 -2 -5 1.66 0.28 -20 -2 -5 1.42 0.37 -20 2 5 1.93 0.39 -20 2 5 2.51 0.33 -20 -3 0 5.08 0.73 -20 -3 0 4.78 0.65 -20 -3 0 4.23 0.78 -20 -3 0 4.06 0.61 -20 3 0 4.55 0.62 -20 3 0 4.35 0.65 -20 -3 0 4.24 0.54 -20 -3 1 0.19 0.40 -20 -3 1 0.29 0.25 -20 3 -1 0.46 0.30 -20 -3 1 0.29 0.30 -20 -3 1 0.13 0.23 -20 -3 1 0.28 0.37 -20 3 -1 0.20 0.29 -20 3 1 0.30 0.25 -20 -3 -1 0.10 0.20 -20 -3 -1 0.11 0.23 -20 -3 -1 0.23 0.39 -20 -3 -1 0.16 0.39 -20 3 1 0.28 0.27 -20 3 -2 1.54 0.36 -20 -3 2 1.96 0.46 -20 -3 2 1.82 0.45 -20 -3 2 2.52 0.50 -20 3 -2 1.51 0.38 -20 -3 2 2.25 0.43 20 -3 2 1.26 0.53 -20 -3 -2 2.48 0.50 -20 -3 -2 3.22 0.77 -20 -3 -2 2.14 0.47 -20 -3 -2 1.87 0.34 -20 3 2 1.86 0.51 -20 3 2 1.43 0.48 -20 -3 3 3.75 0.62 -20 -3 3 3.45 0.56 -20 -3 3 3.13 0.55 -20 3 -3 3.48 0.58 -20 -3 -3 3.03 0.44 20 -3 3 4.01 0.55 -20 -3 -3 3.82 0.66 -20 3 3 4.14 0.56 -20 -3 -3 3.21 0.53 -20 -3 -3 3.47 0.52 -20 -3 4 0.26 0.22 -20 3 -4 0.16 0.23 -20 -3 4 0.09 0.21 -20 -3 -4 0.12 0.18 20 -3 4 0.10 0.19 -20 -3 -4 0.35 0.49 -20 -3 -4 0.24 0.32 -20 -3 -4 0.40 0.21 -20 3 4 0.00 0.18 -20 -3 5 6.81 0.73 -20 3 -5 8.30 0.77 -20 -3 -5 7.49 0.80 20 -3 5 7.60 0.72 -20 -3 -5 8.01 0.73 -20 3 5 7.20 0.69 -20 -4 0 0.34 0.25 -20 -4 0 0.43 0.34 -20 -4 0 0.07 0.44 -20 -4 0 0.31 0.22 -20 4 0 0.29 0.29 -20 -4 0 -0.02 0.26 -20 4 0 0.48 0.27 -20 -4 1 1.41 0.37 -20 -4 1 1.39 0.34 -20 4 -1 1.55 0.55 -20 -4 1 2.03 0.55 -20 -4 1 1.61 0.53 -20 -4 -1 1.36 0.30 -20 -4 -1 1.50 0.38 -20 -4 -1 1.41 0.48 -20 -4 -1 1.53 0.53 -20 -4 2 1.07 0.32 -20 -4 2 0.73 0.25 -20 -4 2 1.01 0.40 -20 4 -2 0.88 0.29 -20 -4 2 0.68 0.25 -20 -4 2 1.11 0.35 -20 -4 -2 1.00 0.28 -20 -4 -2 1.04 0.40 -20 -4 -2 1.02 0.32 -20 4 2 0.66 0.29 -20 -4 -2 1.05 0.49 20 -4 2 0.51 0.28 -20 4 -3 1.15 0.33 -20 -4 3 2.28 0.35 -20 4 -3 1.65 0.37 -20 -4 3 1.81 0.40 -20 -4 3 1.90 0.49 -20 -4 -3 2.08 0.41 -20 -4 -3 2.28 0.57 -20 -4 -3 2.02 0.33 20 -4 3 1.67 0.38 -20 4 3 1.56 0.39 -20 -4 -3 1.81 0.47 -20 -4 4 0.57 0.24 -20 4 -4 -0.06 0.25 20 -4 4 0.19 0.30 -20 -4 -4 0.14 0.16 -20 -4 -4 0.33 0.24 -20 -4 -4 -0.11 0.35 -20 4 4 0.02 0.25 -20 -4 -4 0.05 0.17 -20 5 0 2.99 0.54 -20 -5 0 4.02 0.63 -20 -5 0 4.35 0.79 -20 5 0 2.45 0.49 -20 -5 0 4.57 0.49 -20 -5 1 3.14 0.47 -20 -5 1 2.86 0.49 -20 -5 1 2.51 0.51 -20 5 -1 2.05 0.45 -20 -5 1 3.07 0.62 -20 -5 1 3.11 0.53 -20 -5 -1 3.79 0.52 -20 -5 -1 3.16 0.42 -20 -5 -1 2.43 0.56 -20 5 1 2.29 0.49 -20 -5 -1 3.45 0.71 -20 -5 2 0.27 0.21 -20 5 -2 0.06 0.21 -20 -5 2 0.06 0.20 -20 -5 2 0.10 0.36 -20 -5 2 0.26 0.21 -20 -5 -2 0.20 0.23 -20 5 2 0.22 0.24 -20 -5 -2 0.54 0.37 -20 -5 -2 0.14 0.20 -20 -5 -2 0.21 0.44 -20 -5 3 0.37 0.29 -20 5 -3 0.51 0.26 -20 -5 3 0.23 0.25 -20 -5 3 0.45 0.20 -20 -5 -3 0.60 0.23 -20 -5 -3 0.66 0.23 -20 -5 -3 0.45 0.31 20 -5 3 0.86 0.26 -20 -5 -3 0.63 0.43 -20 5 -4 0.15 0.20 -20 -5 4 0.22 0.18 -20 -5 4 0.11 0.21 -20 -5 -4 0.10 0.14 20 -5 4 0.54 0.21 -20 5 4 0.26 0.19 -20 -5 -4 -0.10 0.44 -20 -5 -4 0.11 0.26 -20 -6 0 0.06 0.19 -20 6 0 0.24 0.23 -20 -6 0 0.12 0.44 -20 6 0 0.05 0.22 -20 -6 0 -0.07 0.28 -20 -6 0 -0.05 0.25 -20 -6 0 0.12 0.26 -20 -6 1 1.08 0.28 -20 -6 1 1.29 0.46 -20 -6 1 1.12 0.28 -20 -6 1 1.47 0.51 -20 -6 1 1.15 0.27 -20 6 -1 1.84 0.46 -20 -6 -1 1.15 0.30 -20 -6 -1 1.03 0.29 -20 -6 -1 1.50 0.50 -20 6 1 0.94 0.34 -20 -6 -1 1.37 0.40 -20 -6 2 0.77 0.46 -20 -6 2 0.62 0.24 -20 -6 2 0.66 0.24 -20 -6 2 0.71 0.23 -20 6 -2 0.90 0.32 -20 6 2 0.71 0.28 -20 -6 -2 1.15 0.34 -20 -6 -2 1.64 0.51 -20 -6 -2 1.09 0.36 -20 -6 -2 0.68 0.47 -20 -6 3 1.11 0.26 -20 -6 3 0.81 0.28 -20 -6 3 0.69 0.23 -20 -6 -3 0.72 0.34 -20 -6 -3 0.77 0.21 -20 -6 -3 0.68 0.37 -20 -6 -3 0.90 0.22 -20 -7 0 0.56 0.44 -20 7 0 0.43 0.25 -20 7 0 0.44 0.28 -20 -7 0 0.66 0.24 -20 -7 0 0.72 0.25 -20 -7 0 0.57 0.25 -20 -7 1 0.13 0.20 -20 -7 1 0.24 0.21 -20 7 -1 0.48 0.23 -20 -7 1 0.37 0.37 -20 -7 1 0.28 0.20 -20 7 -1 1.02 0.28 -20 -7 -1 0.36 0.40 -20 -7 -1 0.48 0.22 -20 -7 -1 0.48 0.22 -20 7 1 0.65 0.28 -20 -7 -1 0.56 0.35 -20 7 -2 2.10 0.38 -20 -7 2 1.08 0.25 -20 -7 2 0.67 0.33 -20 -7 2 1.52 0.31 -20 -7 2 1.25 0.34 -20 -7 -2 0.92 0.41 -20 7 2 1.77 0.37 -20 -7 -2 1.50 0.35 -20 -7 -2 1.71 0.32 -20 -7 -2 1.72 0.32 -21 0 0 0.43 0.27 -21 0 0 0.10 0.22 -21 0 -1 0.08 0.22 -21 0 -1 0.15 0.23 -21 0 1 0.23 0.21 -21 0 1 -0.01 0.24 -21 0 2 -0.01 0.21 -21 0 -2 0.68 0.40 -21 0 2 0.29 0.19 -21 0 -2 0.30 0.25 -21 0 3 0.13 0.24 -21 0 -3 0.31 0.27 -21 0 4 -0.15 0.14 -21 0 -4 0.04 0.16 -21 -1 0 0.72 0.29 -21 1 0 0.62 0.28 -21 -1 0 1.36 0.34 -21 1 0 0.45 0.26 -21 -1 0 0.85 0.29 -21 -1 1 1.40 0.32 -21 1 -1 1.32 0.38 -21 -1 1 2.08 0.38 -21 1 1 0.62 0.27 -21 1 1 1.21 0.32 -21 -1 -1 2.37 0.44 -21 -1 -1 2.13 0.46 -21 1 -2 9.19 0.86 -21 -1 2 6.48 0.81 -21 -1 2 7.76 0.74 -21 -1 -2 8.56 0.86 -21 1 2 6.63 0.86 -21 -1 -2 8.28 0.84 -21 1 2 7.56 0.71 -21 -1 -2 6.27 0.77 -21 -1 3 0.28 0.22 -21 1 -3 0.29 0.28 -21 -1 -3 0.44 0.21 -21 1 3 0.33 0.21 -21 -1 -3 0.59 0.22 -21 -1 -3 0.48 0.33 -21 1 -4 1.49 0.30 -21 -1 4 0.73 0.22 -21 1 4 0.94 0.24 -21 -1 -4 1.27 0.25 -21 2 0 0.73 0.41 -21 -2 0 1.36 0.43 -21 -2 0 2.02 0.40 -21 2 0 1.25 0.32 -21 -2 0 2.05 0.39 -21 -2 0 1.19 0.33 -21 2 -1 1.34 0.32 -21 -2 1 1.56 0.33 -21 -2 1 1.22 0.29 -21 2 1 0.62 0.26 -21 -2 -1 1.20 0.33 -21 2 1 1.05 0.19 -21 -2 -1 1.13 0.26 -21 -2 -1 1.47 0.38 -21 2 1 1.25 0.37 -21 2 -2 0.70 0.29 -21 -2 2 0.32 0.19 -21 -2 2 0.38 0.22 -21 -2 -2 0.39 0.26 -21 -2 -2 0.31 0.22 -21 2 2 0.23 0.23 -21 2 2 0.07 0.29 -21 2 2 0.56 0.16 -21 -2 -2 0.44 0.17 -21 2 -3 0.77 0.32 -21 -2 3 0.78 0.24 -21 -2 -3 0.26 0.19 -21 -2 -3 0.56 0.24 -21 2 3 0.69 0.23 -21 -2 -3 0.72 0.17 -21 -3 0 9.23 0.98 -21 -3 0 11.41 1.04 -21 3 0 9.98 0.95 -21 -3 0 9.59 0.98 -21 3 0 10.55 1.06 -21 -3 0 11.45 1.01 -21 -3 1 2.64 0.41 -21 -3 1 2.59 0.43 -21 -3 1 3.75 0.48 -21 -3 1 3.47 0.51 -21 -3 -1 4.24 0.56 -21 -3 -1 3.92 0.52 -21 3 1 2.65 0.43 -21 -3 -1 3.25 0.62 -21 -3 -1 2.93 0.40 -21 -3 2 3.05 0.39 -21 3 -2 3.66 0.53 -21 -3 2 2.51 0.40 -21 -3 2 2.40 0.47 -21 -3 -2 2.93 0.39 -21 -3 -2 3.64 0.51 -21 -3 -2 4.13 0.68 -21 3 2 2.82 0.36 -21 3 -3 2.22 0.38 -21 -3 -3 1.25 0.26 -21 3 3 1.77 0.29 -21 -3 -3 1.49 0.30 -21 -3 -3 1.83 0.39 -21 4 0 0.76 0.22 -21 -4 0 1.02 0.26 -21 -4 0 0.89 0.33 -21 4 0 0.80 0.25 -21 -4 0 1.39 0.30 -21 -4 0 1.39 0.34 -21 -4 1 1.16 0.30 -21 -4 1 1.49 0.33 -21 4 -1 2.37 0.33 -21 -4 1 1.86 0.34 -21 4 -1 2.22 0.40 -21 -4 -1 1.63 0.37 -21 4 1 2.41 0.35 -21 -4 -1 2.48 0.42 -21 4 1 2.00 0.39 -21 -4 -1 1.54 0.40 -21 -4 -1 1.73 0.30 -21 -4 2 3.38 0.43 -21 -4 2 3.17 0.52 -21 -4 2 3.96 0.43 -21 4 -2 3.27 0.50 -21 -4 -2 3.88 0.43 -21 -4 -2 4.54 0.51 -21 -4 -2 2.96 0.60 -21 -4 -2 4.82 0.57 -21 4 2 3.37 0.43 -21 -4 3 0.78 0.20 -21 -4 -3 0.73 0.21 -21 -4 -3 0.94 0.23 -21 5 0 0.21 0.17 -21 -5 0 0.19 0.19 -21 -5 0 0.09 0.19 -21 5 0 0.14 0.18 -21 -5 0 0.05 0.25 -21 -5 0 0.05 0.18 -21 -5 1 0.75 0.29 -21 5 -1 1.12 0.25 -21 5 -1 1.09 0.26 -21 -5 1 0.79 0.23 -21 -5 -1 0.83 0.36 -21 -5 -1 0.95 0.24 -21 -5 -1 1.06 0.21 -21 5 1 1.26 0.27 -21 -5 -1 1.39 0.30 -21 -5 2 0.06 0.25 -21 -5 2 0.12 0.18 -21 5 -2 0.01 0.17 -21 -5 2 0.12 0.16 -21 -5 -2 0.04 0.36 -21 -5 -2 0.25 0.22 -21 -5 -2 0.08 0.16 -21 -5 -2 0.03 0.15 -21 5 2 0.03 0.14 -22 0 0 1.37 0.30 -22 0 1 16.66 1.46 -22 0 -1 20.95 1.78 -22 1 0 0.61 0.20 -22 -1 0 0.55 0.21 -22 1 -1 1.94 0.34 -22 1 1 1.36 0.33 -22 -1 -1 2.40 0.36 -22 2 0 1.55 0.30 -22 -2 0 0.99 0.22 -22 2 -1 0.96 0.26 -22 -2 -1 0.92 0.25 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 56113 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.30815(14) 0.85324(14) 0.9075(2) 0.0507(6) Uani 1 1 d . . . . . O1 O 0.3770(3) 0.7107(3) 0.2404(4) 0.0260(10) Uani 1 1 d . . . . . H1 H 0.374002 0.761798 0.279202 0.039 Uiso 1 1 calc R U . . . N1 N 0.4879(3) 0.8793(4) 0.5810(6) 0.0255(12) Uani 1 1 d . . . . . N2 N 0.4421(3) 0.9128(4) 0.4926(6) 0.0276(12) Uani 1 1 d . . . . . N3 N 0.4128(3) 0.8393(4) 0.4335(6) 0.0294(13) Uani 1 1 d . . . . . C4 C 0.4437(4) 0.7632(4) 0.4878(7) 0.0237(13) Uani 1 1 d . . . . . N5 N 0.4911(3) 0.7857(4) 0.5811(6) 0.0252(12) Uani 1 1 d . . . . . C6 C 0.5359(4) 0.9380(4) 0.6657(6) 0.0241(13) Uani 1 1 d . . . . . C7 C 0.5286(5) 0.8949(5) 0.7996(6) 0.0342(17) Uani 1 1 d . . . . . H7A H 0.475362 0.892669 0.824212 0.051 Uiso 1 1 calc R U . . . H7B H 0.556493 0.932725 0.861798 0.051 Uiso 1 1 calc R U . . . H7C H 0.549229 0.831710 0.798552 0.051 Uiso 1 1 calc R U . . . C8 C 0.5026(4) 1.0365(5) 0.6644(7) 0.0318(16) Uani 1 1 d . . . . . H8A H 0.504266 1.061339 0.576735 0.048 Uiso 1 1 calc R U . . . H8B H 0.532047 1.076720 0.721430 0.048 Uiso 1 1 calc R U . . . H8C H 0.450285 1.034351 0.694050 0.048 Uiso 1 1 calc R U . . . C9 C 0.6158(4) 0.9374(4) 0.6150(6) 0.0256(14) Uani 1 1 d . . . . . C10 C 0.6709(4) 0.9837(5) 0.6866(7) 0.0320(16) Uani 1 1 d . . . . . H10 H 0.657577 1.014207 0.764297 0.038 Uiso 1 1 calc R U . . . C11 C 0.7448(5) 0.9850(5) 0.6445(7) 0.0361(17) Uani 1 1 d . . . . . H11 H 0.781901 1.016087 0.694148 0.043 Uiso 1 1 calc R U . . . C12 C 0.7654(4) 0.9418(6) 0.5311(8) 0.0359(17) Uani 1 1 d . . . . . H12 H 0.816230 0.943919 0.502627 0.043 Uiso 1 1 calc R U . . . C13 C 0.7119(4) 0.8956(5) 0.4598(6) 0.0297(15) Uani 1 1 d . . . . . H13 H 0.725718 0.865253 0.382196 0.036 Uiso 1 1 calc R U . . . C14 C 0.6373(4) 0.8935(5) 0.5019(7) 0.0296(15) Uani 1 1 d . . . . . H14 H 0.600633 0.861490 0.452367 0.036 Uiso 1 1 calc R U . . . C15 C 0.4232(4) 0.6657(4) 0.4519(7) 0.0241(14) Uani 1 1 d . . . . . H15 H 0.459049 0.622122 0.495132 0.029 Uiso 1 1 calc R U . . . C16 C 0.3428(4) 0.6450(5) 0.5007(7) 0.0299(15) Uani 1 1 d . . . . . H16A H 0.307065 0.689575 0.461558 0.036 Uiso 1 1 calc R U . . . H16B H 0.327883 0.581553 0.474121 0.036 Uiso 1 1 calc R U . . . C17 C 0.3390(4) 0.6527(5) 0.6449(7) 0.0288(14) Uani 1 1 d . . . . . C18 C 0.3235(4) 0.7383(5) 0.7025(8) 0.0322(16) Uani 1 1 d . . . . . H18 H 0.311002 0.790756 0.651282 0.039 Uiso 1 1 calc R U . . . C19 C 0.3266(4) 0.7460(5) 0.8361(8) 0.0325(16) Uani 1 1 d . . . . . C20 C 0.3421(4) 0.6714(5) 0.9137(8) 0.0323(16) Uani 1 1 d . . . . . H20 H 0.344060 0.678105 1.004469 0.039 Uiso 1 1 calc R U . . . C21 C 0.3550(4) 0.5852(5) 0.8555(8) 0.0333(17) Uani 1 1 d . . . . . H21 H 0.364369 0.532058 0.907260 0.040 Uiso 1 1 calc R U . . . C22 C 0.3541(4) 0.5766(5) 0.7223(8) 0.0311(16) Uani 1 1 d . . . . . H22 H 0.363874 0.517846 0.684036 0.037 Uiso 1 1 calc R U . . . C23 C 0.4302(4) 0.6526(5) 0.3036(6) 0.0245(13) Uani 1 1 d . . . . . C24 C 0.5107(4) 0.6763(4) 0.2579(7) 0.0259(14) Uani 1 1 d . . . . . C25 C 0.5743(4) 0.6647(5) 0.3351(7) 0.0291(15) Uani 1 1 d . . . . . H25 H 0.568557 0.642546 0.420515 0.035 Uiso 1 1 calc R U . . . C26 C 0.6452(4) 0.6847(5) 0.2894(8) 0.0309(16) Uani 1 1 d . . . . . H26 H 0.687720 0.676575 0.343682 0.037 Uiso 1 1 calc R U . . . C27 C 0.6552(4) 0.7167(5) 0.1652(8) 0.0345(17) Uani 1 1 d . . . . . H27 H 0.704082 0.731169 0.134184 0.041 Uiso 1 1 calc R U . . . C28 C 0.5928(5) 0.7272(6) 0.0868(8) 0.0405(18) Uani 1 1 d . . . . . H28 H 0.599222 0.748475 0.001139 0.049 Uiso 1 1 calc R U . . . C29 C 0.5210(4) 0.7072(5) 0.1316(8) 0.0353(17) Uani 1 1 d . . . . . H29 H 0.478799 0.714549 0.076444 0.042 Uiso 1 1 calc R U . . . C30 C 0.4103(4) 0.5522(5) 0.2673(7) 0.0262(14) Uani 1 1 d . . . . . C31 C 0.4591(4) 0.4806(5) 0.2966(8) 0.0319(16) Uani 1 1 d . . . . . H31 H 0.504489 0.493651 0.341517 0.038 Uiso 1 1 calc R U . . . C32 C 0.4426(4) 0.3892(5) 0.2611(8) 0.0340(16) Uani 1 1 d . . . . . H32 H 0.477082 0.340726 0.280645 0.041 Uiso 1 1 calc R U . . . C33 C 0.3767(4) 0.3693(5) 0.1980(8) 0.0353(17) Uani 1 1 d . . . . . H33 H 0.365659 0.307154 0.173598 0.042 Uiso 1 1 calc R U . . . C34 C 0.3263(4) 0.4399(5) 0.1700(8) 0.0353(17) Uani 1 1 d . . . . . H34 H 0.280440 0.426328 0.126831 0.042 Uiso 1 1 calc R U . . . C35 C 0.3434(4) 0.5313(5) 0.2057(7) 0.0314(15) Uani 1 1 d . . . . . H35 H 0.308523 0.579605 0.187475 0.038 Uiso 1 1 calc R U . . . 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 0.0716(14) 0.0348(9) 0.0457(11) -0.0040(10) 0.0258(11) 0.0050(10) O1 0.029(2) 0.025(2) 0.023(2) 0.0023(19) -0.0024(19) 0.0045(19) N1 0.030(3) 0.020(3) 0.026(3) 0.000(2) 0.002(2) 0.003(2) N2 0.035(3) 0.026(3) 0.022(3) 0.000(2) 0.000(2) 0.000(2) N3 0.033(3) 0.023(3) 0.033(3) -0.006(2) -0.003(2) 0.001(2) C4 0.023(3) 0.021(3) 0.027(3) 0.000(3) 0.000(3) -0.001(2) N5 0.031(3) 0.020(3) 0.024(3) 0.001(2) 0.005(2) 0.001(2) C6 0.037(3) 0.021(3) 0.014(3) 0.000(2) -0.003(3) -0.002(3) C7 0.054(5) 0.031(4) 0.018(3) -0.002(3) 0.003(3) -0.003(3) C8 0.047(4) 0.027(3) 0.022(3) -0.004(3) 0.001(3) 0.000(3) C9 0.038(4) 0.022(3) 0.017(3) 0.004(2) -0.003(3) -0.004(3) C10 0.047(4) 0.031(4) 0.018(3) 0.002(3) -0.007(3) -0.005(3) C11 0.048(4) 0.041(4) 0.019(3) 0.002(3) -0.012(3) -0.012(4) C12 0.035(4) 0.037(4) 0.035(4) 0.011(3) -0.006(3) -0.007(3) C13 0.042(4) 0.034(4) 0.013(3) -0.005(3) 0.003(3) 0.000(3) C14 0.041(4) 0.027(3) 0.021(3) 0.000(3) 0.001(3) -0.006(3) C15 0.025(3) 0.020(3) 0.027(3) 0.000(3) -0.003(3) 0.001(2) C16 0.028(3) 0.030(4) 0.031(4) 0.008(3) -0.007(3) 0.000(3) C17 0.023(3) 0.029(3) 0.034(4) 0.004(3) 0.003(3) 0.000(3) C18 0.030(4) 0.028(3) 0.039(4) 0.007(3) 0.010(3) 0.002(3) C19 0.032(4) 0.029(4) 0.036(4) -0.001(3) 0.012(3) 0.001(3) C20 0.025(3) 0.041(4) 0.030(4) -0.001(3) 0.009(3) 0.002(3) C21 0.027(4) 0.034(4) 0.039(4) 0.008(3) 0.003(3) 0.005(3) C22 0.024(3) 0.029(3) 0.040(4) 0.001(3) 0.002(3) 0.001(3) C23 0.024(3) 0.026(3) 0.024(3) 0.002(3) -0.002(3) 0.001(3) C24 0.027(3) 0.020(3) 0.031(4) -0.004(3) 0.003(3) 0.000(2) C25 0.032(4) 0.024(3) 0.031(4) -0.005(3) 0.001(3) 0.003(3) C26 0.029(3) 0.026(3) 0.038(4) -0.007(3) -0.007(3) 0.000(3) C27 0.029(4) 0.030(4) 0.044(4) 0.001(3) 0.009(3) -0.001(3) C28 0.043(4) 0.042(4) 0.037(4) 0.016(4) 0.002(4) -0.003(3) C29 0.033(4) 0.041(4) 0.032(4) 0.005(3) 0.002(3) 0.002(3) C30 0.028(3) 0.025(3) 0.026(3) 0.001(3) 0.004(3) -0.001(3) C31 0.028(3) 0.025(3) 0.042(4) -0.008(3) 0.000(3) -0.001(3) C32 0.038(4) 0.026(3) 0.038(4) -0.011(3) -0.002(3) 0.004(3) C33 0.038(4) 0.028(4) 0.040(4) -0.008(3) 0.004(3) -0.006(3) C34 0.031(4) 0.033(4) 0.042(4) 0.001(3) -0.007(3) -0.007(3) C35 0.028(3) 0.030(4) 0.037(4) -0.002(3) 0.000(3) 0.000(3) 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 C23 O1 H1 109.5 . . ? N2 N1 N5 113.0(6) . . ? N2 N1 C6 124.0(5) . . ? N5 N1 C6 122.8(6) . . ? N1 N2 N3 105.9(5) . . ? N2 N3 C4 107.0(5) . . ? N3 C4 C15 123.8(6) . . ? N5 C4 N3 111.6(6) . . ? N5 C4 C15 124.5(6) . . ? C4 N5 N1 102.5(5) . . ? N1 C6 C7 105.1(5) . . ? N1 C6 C8 107.2(5) . . ? N1 C6 C9 109.1(5) . . ? C7 C6 C8 110.4(6) . . ? C9 C6 C7 113.3(6) . . ? C9 C6 C8 111.3(6) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C6 117.8(6) . . ? C14 C9 C6 123.8(6) . . ? C14 C9 C10 118.4(7) . . ? C9 C10 H10 120.0 . . ? C11 C10 C9 120.0(7) . . ? C11 C10 H10 120.0 . . ? C10 C11 H11 119.5 . . ? C12 C11 C10 121.1(7) . . ? C12 C11 H11 119.5 . . ? C11 C12 H12 120.2 . . ? C13 C12 C11 119.6(7) . . ? C13 C12 H12 120.2 . . ? C12 C13 H13 120.1 . . ? C12 C13 C14 119.8(7) . . ? C14 C13 H13 120.1 . . ? C9 C14 C13 121.2(7) . . ? C9 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C4 C15 H15 108.6 . . ? C4 C15 C16 108.8(5) . . ? C4 C15 C23 110.0(5) . . ? C16 C15 H15 108.6 . . ? C16 C15 C23 112.1(5) . . ? C23 C15 H15 108.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C17 C16 C15 110.8(6) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C18 C17 C16 120.1(7) . . ? C22 C17 C16 120.9(7) . . ? C22 C17 C18 119.0(7) . . ? C17 C18 H18 120.3 . . ? C19 C18 C17 119.3(7) . . ? C19 C18 H18 120.3 . . ? C18 C19 Cl1 119.2(6) . . ? C20 C19 Cl1 118.6(6) . . ? C20 C19 C18 122.2(7) . . ? C19 C20 H20 121.0 . . ? C19 C20 C21 118.1(7) . . ? C21 C20 H20 121.0 . . ? C20 C21 H21 119.7 . . ? C22 C21 C20 120.6(7) . . ? C22 C21 H21 119.7 . . ? C17 C22 C21 120.8(7) . . ? C17 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? O1 C23 C15 109.5(5) . . ? O1 C23 C24 110.0(5) . . ? O1 C23 C30 106.6(5) . . ? C24 C23 C15 110.6(5) . . ? C30 C23 C15 109.8(5) . . ? C30 C23 C24 110.2(5) . . ? C25 C24 C23 123.0(6) . . ? C25 C24 C29 118.2(6) . . ? C29 C24 C23 118.7(6) . . ? C24 C25 H25 119.5 . . ? C26 C25 C24 121.1(7) . . ? C26 C25 H25 119.5 . . ? C25 C26 H26 119.7 . . ? C25 C26 C27 120.6(7) . . ? C27 C26 H26 119.7 . . ? C26 C27 H27 120.5 . . ? C26 C27 C28 119.0(7) . . ? C28 C27 H27 120.5 . . ? C27 C28 H28 119.5 . . ? C27 C28 C29 121.0(8) . . ? C29 C28 H28 119.5 . . ? C24 C29 H29 120.0 . . ? C28 C29 C24 120.1(7) . . ? C28 C29 H29 120.0 . . ? C31 C30 C23 120.2(6) . . ? C31 C30 C35 118.6(6) . . ? C35 C30 C23 121.1(6) . . ? C30 C31 H31 119.6 . . ? C30 C31 C32 120.8(7) . . ? C32 C31 H31 119.6 . . ? C31 C32 H32 119.9 . . ? C33 C32 C31 120.1(7) . . ? C33 C32 H32 119.9 . . ? C32 C33 H33 120.0 . . ? C32 C33 C34 120.0(7) . . ? C34 C33 H33 120.0 . . ? C33 C34 H34 120.3 . . ? C33 C34 C35 119.5(7) . . ? C35 C34 H34 120.3 . . ? C30 C35 C34 120.9(7) . . ? C30 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? 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 Cl1 C19 1.743(8) . ? O1 H1 0.8400 . ? O1 C23 1.424(8) . ? N1 N2 1.319(8) . ? N1 N5 1.348(7) . ? N1 C6 1.490(8) . ? N2 N3 1.330(8) . ? N3 C4 1.349(8) . ? C4 N5 1.325(9) . ? C4 C15 1.497(9) . ? C6 C7 1.531(9) . ? C6 C8 1.536(9) . ? C6 C9 1.513(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.398(10) . ? C9 C14 1.390(10) . ? C10 H10 0.9500 . ? C10 C11 1.384(11) . ? C11 H11 0.9500 . ? C11 C12 1.384(11) . ? C12 H12 0.9500 . ? C12 C13 1.377(10) . ? C13 H13 0.9500 . ? C13 C14 1.396(10) . ? C14 H14 0.9500 . ? C15 H15 1.0000 . ? C15 C16 1.544(9) . ? C15 C23 1.560(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.506(10) . ? C17 C18 1.397(10) . ? C17 C22 1.385(10) . ? C18 H18 0.9500 . ? C18 C19 1.396(11) . ? C19 C20 1.371(10) . ? C20 H20 0.9500 . ? C20 C21 1.400(11) . ? C21 H21 0.9500 . ? C21 C22 1.392(11) . ? C22 H22 0.9500 . ? C23 C24 1.545(9) . ? C23 C30 1.533(9) . ? C24 C25 1.396(10) . ? C24 C29 1.400(10) . ? C25 H25 0.9500 . ? C25 C26 1.377(10) . ? C26 H26 0.9500 . ? C26 C27 1.383(11) . ? C27 H27 0.9500 . ? C27 C28 1.384(11) . ? C28 H28 0.9500 . ? C28 C29 1.387(11) . ? C29 H29 0.9500 . ? C30 C31 1.381(10) . ? C30 C35 1.384(10) . ? C31 H31 0.9500 . ? C31 C32 1.397(9) . ? C32 H32 0.9500 . ? C32 C33 1.373(11) . ? C33 H33 0.9500 . ? C33 C34 1.384(11) . ? C34 H34 0.9500 . ? C34 C35 1.400(10) . ? 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 _geom_hbond_publ_flag O1 H1 N3 0.84 2.07 2.804(7) 145.3 . yes 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 Cl1 C19 C20 C21 178.4(6) . . . . ? O1 C23 C24 C25 150.7(6) . . . . ? O1 C23 C24 C29 -32.0(8) . . . . ? O1 C23 C30 C31 169.3(6) . . . . ? O1 C23 C30 C35 -11.1(8) . . . . ? N1 N2 N3 C4 -1.1(7) . . . . ? N1 C6 C9 C10 -175.8(6) . . . . ? N1 C6 C9 C14 4.1(9) . . . . ? N2 N1 N5 C4 -0.5(7) . . . . ? N2 N1 C6 C7 136.9(6) . . . . ? N2 N1 C6 C8 19.3(9) . . . . ? N2 N1 C6 C9 -101.3(7) . . . . ? N2 N3 C4 N5 0.9(8) . . . . ? N2 N3 C4 C15 177.5(6) . . . . ? N3 C4 N5 N1 -0.2(7) . . . . ? N3 C4 C15 C16 -70.6(8) . . . . ? N3 C4 C15 C23 52.6(8) . . . . ? C4 C15 C16 C17 -61.6(7) . . . . ? C4 C15 C23 O1 -64.1(7) . . . . ? C4 C15 C23 C24 57.3(7) . . . . ? C4 C15 C23 C30 179.2(5) . . . . ? N5 N1 N2 N3 1.1(8) . . . . ? N5 N1 C6 C7 -48.0(8) . . . . ? N5 N1 C6 C8 -165.5(6) . . . . ? N5 N1 C6 C9 73.8(7) . . . . ? N5 C4 C15 C16 105.6(7) . . . . ? N5 C4 C15 C23 -131.3(7) . . . . ? C6 N1 N2 N3 176.6(6) . . . . ? C6 N1 N5 C4 -176.2(6) . . . . ? C6 C9 C10 C11 179.9(7) . . . . ? C6 C9 C14 C13 179.8(6) . . . . ? C7 C6 C9 C10 -59.1(8) . . . . ? C7 C6 C9 C14 120.8(7) . . . . ? C8 C6 C9 C10 66.1(8) . . . . ? C8 C6 C9 C14 -114.0(7) . . . . ? C9 C10 C11 C12 0.6(11) . . . . ? C10 C9 C14 C13 -0.3(10) . . . . ? C10 C11 C12 C13 -0.9(11) . . . . ? C11 C12 C13 C14 0.5(11) . . . . ? C12 C13 C14 C9 0.0(11) . . . . ? C14 C9 C10 C11 0.0(10) . . . . ? C15 C4 N5 N1 -176.8(6) . . . . ? C15 C16 C17 C18 88.3(8) . . . . ? C15 C16 C17 C22 -88.7(8) . . . . ? C15 C23 C24 C25 29.6(8) . . . . ? C15 C23 C24 C29 -153.1(6) . . . . ? C15 C23 C30 C31 -72.1(8) . . . . ? C15 C23 C30 C35 107.4(7) . . . . ? C16 C15 C23 O1 57.1(7) . . . . ? C16 C15 C23 C24 178.5(5) . . . . ? C16 C15 C23 C30 -59.7(7) . . . . ? C16 C17 C18 C19 -174.5(7) . . . . ? C16 C17 C22 C21 176.1(7) . . . . ? C17 C18 C19 Cl1 179.4(5) . . . . ? C17 C18 C19 C20 -2.1(12) . . . . ? C18 C17 C22 C21 -1.0(11) . . . . ? C18 C19 C20 C21 -0.1(11) . . . . ? C19 C20 C21 C22 1.8(11) . . . . ? C20 C21 C22 C17 -1.3(11) . . . . ? C22 C17 C18 C19 2.6(10) . . . . ? C23 C15 C16 C17 176.6(6) . . . . ? C23 C24 C25 C26 178.5(6) . . . . ? C23 C24 C29 C28 -178.7(7) . . . . ? C23 C30 C31 C32 -178.3(7) . . . . ? C23 C30 C35 C34 178.4(7) . . . . ? C24 C23 C30 C31 50.0(8) . . . . ? C24 C23 C30 C35 -130.5(7) . . . . ? C24 C25 C26 C27 -0.3(10) . . . . ? C25 C24 C29 C28 -1.3(11) . . . . ? C25 C26 C27 C28 -0.7(11) . . . . ? C26 C27 C28 C29 0.7(12) . . . . ? C27 C28 C29 C24 0.3(12) . . . . ? C29 C24 C25 C26 1.2(10) . . . . ? C30 C23 C24 C25 -92.0(7) . . . . ? C30 C23 C24 C29 85.3(7) . . . . ? C30 C31 C32 C33 -1.0(12) . . . . ? C31 C30 C35 C34 -2.0(11) . . . . ? C31 C32 C33 C34 -0.3(12) . . . . ? C32 C33 C34 C35 0.4(12) . . . . ? C33 C34 C35 C30 0.8(12) . . . . ? C35 C30 C31 C32 2.2(11) . . . . ?