#------------------------------------------------------------------------------ #$Date: 2021-08-05 03:36:00 +0300 (Thu, 05 Aug 2021) $ #$Revision: 267948 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564324.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_1564324 loop_ _publ_author_name 'Mandal, Swadhin K.' 'Maji, Subir' 'Das, Arpan' _publ_section_title ; Mesoionic N-heterocyclic Olefin Catalysed Reductive Functionalization of CO2 for Consecutive N-Methylation of Amines ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC02819G _journal_year 2021 _chemical_formula_moiety '2(C48 H61 B N2)' _chemical_formula_sum 'C96 H122 B2 N4' _chemical_formula_weight 1353.59 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-02-28 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-02-27 deposited with the CCDC. 2021-08-03 downloaded from the CCDC. ; _cell_angle_alpha 90.009(3) _cell_angle_beta 93.393(2) _cell_angle_gamma 90.024(3) _cell_formula_units_Z 2 _cell_length_a 13.9680(11) _cell_length_b 15.6349(13) _cell_length_c 22.5739(17) _cell_measurement_reflns_used 9978 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.39 _cell_volume 4921.2(7) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.61 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1058 _diffrn_reflns_av_unetI/netI 0.1239 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 50073 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.444 _diffrn_reflns_theta_min 2.191 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.052 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.3437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1577 before and 0.1063 after correction. The Ratio of minimum to maximum transmission is 0.4612. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 0.913 _exptl_crystal_description block _exptl_crystal_F_000 1472 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.349 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 935 _refine_ls_number_reflns 18007 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0761 _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^)+(0.1210P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2034 _refine_ls_wR_factor_ref 0.2410 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10714 _reflns_number_total 18007 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc02819g2.cif _cod_data_source_block mo_tkp180121_0ma_a _cod_database_code 1564324 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.995 _shelx_estimated_absorpt_t_min 0.990 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All B(H) groups, All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C12(H12), C19(H19), C30(H30), C38(H38), C41(H41), C44(H44), B1(H1), C54(H54), C62(H62), C72(H72), C80(H80), C89(H89), C93(H93), B2(H2) 2.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C42(H42A,H42B), C43(H43A,H43B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C90(H90A,H90B), C91(H91B,H91A), C92(H92A,H92B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B) 2.c Aromatic/amide H refined with riding coordinates: C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16), C17(H17), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C33(H33), C34(H34), C35(H35), C57(H57), C58(H58), C59(H59), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70), C75(H75), C76(H76), C77(H77), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88) 2.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B, H21C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C), C40(H40A, H40B,H40C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C81(H81A,H81B, H81C), C82(H82A,H82B,H82C) ; _shelx_res_file ; mo_tkp180121_0ma_a.res created by SHELXL-2014/7 TITL mo_tkp180121_0ma_a_a.res in P-1 REM Old TITL mo_TKP180121_0ma_a.res in P-1 REM SHELXT solution in P-1 REM R1 0.228, Rweak 0.004, Alpha 0.041, Orientation as input REM Formula found by SHELXT: C229 B4 N14 CELL 0.71073 13.968 15.6349 22.5739 90.009 93.393 90.024 ZERR 2 0.0011 0.0013 0.0017 0.003 0.002 0.003 LATT 1 SFAC C H B N UNIT 192 244 4 8 L.S. 10 PLAN 20 SIZE 0.2 0.15 0.1 TEMP -172.54 BOND $H list 4 ABIN fmap 2 acta OMIT -9 -3 6 OMIT 1 0 2 OMIT 0 1 3 OMIT -1 1 3 OMIT -4 3 1 OMIT -4 -3 1 OMIT -5 3 6 OMIT -2 -1 3 OMIT -2 1 3 OMIT 1 1 3 OMIT 0 -1 3 OMIT -1 -1 3 OMIT 1 -1 3 OMIT -5 -4 3 OMIT -3 -3 1 OMIT -3 3 1 OMIT -4 3 3 OMIT 2 1 1 OMIT -1 0 6 OMIT -6 -2 3 OMIT -1 -1 5 OMIT 3 0 6 REM REM REM WGHT 0.121000 FVAR 0.48629 N1 4 0.592692 0.714443 0.410307 11.00000 0.01485 0.02119 = 0.01995 0.00102 -0.00069 -0.00805 N2 4 0.622316 0.646645 0.329413 11.00000 0.02051 0.02016 = 0.02026 0.00285 0.00139 -0.00765 C1 1 0.422544 0.768120 0.388642 11.00000 0.02106 0.02122 = 0.02083 0.00236 0.00079 -0.00624 AFIX 23 H1A 2 0.389453 0.788322 0.351245 11.00000 -1.20000 H1B 2 0.443365 0.819495 0.411595 11.00000 -1.20000 AFIX 0 C2 1 0.509753 0.721020 0.373166 11.00000 0.01595 0.02254 = 0.02249 0.00497 -0.00216 -0.00985 C3 1 0.528227 0.678357 0.322107 11.00000 0.01560 0.01983 = 0.02509 0.00640 0.00014 -0.00656 C4 1 0.659448 0.668254 0.383350 11.00000 0.02274 0.01757 = 0.02298 0.00252 -0.00015 -0.01177 C5 1 0.754823 0.642750 0.408488 11.00000 0.02017 0.02651 = 0.02029 0.00399 0.00276 -0.00841 C6 1 0.815851 0.699978 0.439471 11.00000 0.01794 0.02362 = 0.02929 0.00382 0.00029 -0.00868 AFIX 43 H6 2 0.796241 0.757396 0.445269 11.00000 -1.20000 AFIX 0 C7 1 0.905175 0.672692 0.461742 11.00000 0.02215 0.03190 = 0.03383 0.00293 -0.00228 -0.01393 AFIX 43 H7 2 0.946614 0.711619 0.483002 11.00000 -1.20000 AFIX 0 C8 1 0.934760 0.589154 0.453337 11.00000 0.01980 0.03716 = 0.03973 0.01272 0.00182 -0.00805 AFIX 43 H8 2 0.996624 0.571298 0.468152 11.00000 -1.20000 AFIX 0 C9 1 0.874037 0.531960 0.423364 11.00000 0.02996 0.02604 = 0.03558 0.00671 0.00543 -0.00016 AFIX 43 H9 2 0.893654 0.474437 0.418032 11.00000 -1.20000 AFIX 0 C10 1 0.784004 0.558838 0.400986 11.00000 0.02186 0.02612 = 0.02991 0.00246 -0.00104 -0.00820 AFIX 43 H10 2 0.742255 0.519432 0.380432 11.00000 -1.20000 AFIX 0 C11 1 0.718162 0.932037 0.398181 11.00000 0.02839 0.03089 = 0.04334 0.00379 0.00751 -0.01107 AFIX 137 H11A 2 0.741801 0.968510 0.431201 11.00000 -1.50000 H11B 2 0.715904 0.965059 0.361229 11.00000 -1.50000 H11C 2 0.761296 0.883096 0.394751 11.00000 -1.50000 AFIX 0 C12 1 0.616990 0.899805 0.409725 11.00000 0.02684 0.02294 = 0.02742 0.00343 0.00147 -0.01069 AFIX 13 H12 2 0.595023 0.862086 0.375808 11.00000 -1.20000 AFIX 0 C13 1 0.547319 0.974917 0.411542 11.00000 0.03070 0.02506 = 0.03650 0.00446 0.00083 -0.01087 AFIX 137 H13A 2 0.483853 0.953848 0.420855 11.00000 -1.50000 H13B 2 0.542837 1.003443 0.372824 11.00000 -1.50000 H13C 2 0.570570 1.015646 0.442113 11.00000 -1.50000 AFIX 0 C14 1 0.618024 0.846482 0.466386 11.00000 0.01752 0.02179 = 0.03271 0.00244 0.00022 -0.00776 C15 1 0.632454 0.886842 0.520871 11.00000 0.02677 0.02448 = 0.03208 -0.00389 -0.00099 -0.00583 AFIX 43 H15 2 0.640188 0.947194 0.522236 11.00000 -1.20000 AFIX 0 C16 1 0.635795 0.840811 0.573304 11.00000 0.03296 0.03362 = 0.02706 -0.00573 -0.00707 -0.00520 AFIX 43 H16 2 0.644545 0.869847 0.610200 11.00000 -1.20000 AFIX 0 C17 1 0.626496 0.753076 0.572271 11.00000 0.02931 0.03136 = 0.02504 0.00537 -0.00216 -0.00712 AFIX 43 H17 2 0.629483 0.722460 0.608681 11.00000 -1.20000 AFIX 0 C18 1 0.612886 0.708392 0.519390 11.00000 0.01878 0.02611 = 0.02277 0.00172 -0.00038 -0.00554 C19 1 0.605503 0.611436 0.521006 11.00000 0.02504 0.02573 = 0.02353 0.00517 -0.00149 -0.00873 AFIX 13 H19 2 0.597890 0.590177 0.479209 11.00000 -1.20000 AFIX 0 C20 1 0.517599 0.582753 0.553632 11.00000 0.03093 0.03301 = 0.03520 0.00723 0.00624 -0.01227 AFIX 137 H20A 2 0.520006 0.608461 0.593289 11.00000 -1.50000 H20B 2 0.517683 0.520287 0.557218 11.00000 -1.50000 H20C 2 0.459006 0.601204 0.531212 11.00000 -1.50000 AFIX 0 C21 1 0.695522 0.571069 0.550412 11.00000 0.03086 0.03203 = 0.03544 0.00991 -0.00043 -0.00467 AFIX 137 H21A 2 0.751689 0.589588 0.529735 11.00000 -1.50000 H21B 2 0.690121 0.508628 0.548379 11.00000 -1.50000 H21C 2 0.702651 0.589031 0.592035 11.00000 -1.50000 AFIX 0 C22 1 0.608039 0.756930 0.466982 11.00000 0.01801 0.02402 = 0.02072 -0.00142 0.00016 -0.00938 C23 1 0.462548 0.665913 0.269423 11.00000 0.02322 0.01875 = 0.02252 0.00106 -0.00164 -0.00914 C24 1 0.488131 0.679255 0.211076 11.00000 0.02470 0.02025 = 0.02479 0.00062 0.00022 -0.00546 AFIX 43 H24 2 0.552290 0.694063 0.203646 11.00000 -1.20000 AFIX 0 C25 1 0.420457 0.670970 0.164316 11.00000 0.03296 0.02123 = 0.02273 -0.00028 -0.00041 -0.00323 AFIX 43 H25 2 0.438252 0.679945 0.124823 11.00000 -1.20000 AFIX 0 C26 1 0.325928 0.649437 0.174882 11.00000 0.03264 0.02592 = 0.02892 -0.00219 -0.01136 -0.00358 AFIX 43 H26 2 0.279406 0.644342 0.142634 11.00000 -1.20000 AFIX 0 C27 1 0.300192 0.635611 0.231945 11.00000 0.02247 0.02939 = 0.03634 -0.00123 -0.00237 -0.01014 AFIX 43 H27 2 0.235808 0.621020 0.238952 11.00000 -1.20000 AFIX 0 C28 1 0.367781 0.642836 0.279537 11.00000 0.02892 0.02392 = 0.02510 0.00228 0.00156 -0.00892 AFIX 43 H28 2 0.349792 0.632165 0.318790 11.00000 -1.20000 AFIX 0 C29 1 0.499198 0.442908 0.253687 11.00000 0.03184 0.03381 = 0.04365 -0.00026 -0.00078 -0.01378 AFIX 137 H29A 2 0.466035 0.494971 0.239666 11.00000 -1.50000 H29B 2 0.455472 0.407771 0.275821 11.00000 -1.50000 H29C 2 0.520056 0.410466 0.219612 11.00000 -1.50000 AFIX 0 C30 1 0.586246 0.467013 0.294024 11.00000 0.03042 0.02327 = 0.02669 -0.00056 0.00298 -0.01089 AFIX 13 H30 2 0.563327 0.497427 0.329492 11.00000 -1.20000 AFIX 0 C31 1 0.638954 0.385275 0.315381 11.00000 0.04447 0.02478 = 0.03359 0.00473 0.00539 -0.00875 AFIX 137 H31A 2 0.653057 0.350094 0.281038 11.00000 -1.50000 H31B 2 0.598339 0.352885 0.341322 11.00000 -1.50000 H31C 2 0.699042 0.400777 0.337387 11.00000 -1.50000 AFIX 0 C32 1 0.654759 0.526113 0.263398 11.00000 0.02781 0.02210 = 0.01876 0.00285 -0.00433 -0.00388 C33 1 0.701683 0.495855 0.215193 11.00000 0.03183 0.02652 = 0.02375 -0.00066 0.00042 -0.00508 AFIX 43 H33 2 0.687010 0.440185 0.200418 11.00000 -1.20000 AFIX 0 C34 1 0.768815 0.544135 0.188192 11.00000 0.03132 0.03636 = 0.02005 0.00203 0.00276 0.00258 AFIX 43 H34 2 0.800134 0.521551 0.155397 11.00000 -1.20000 AFIX 0 C35 1 0.791005 0.626141 0.208843 11.00000 0.02300 0.03573 = 0.02760 0.00677 0.00177 -0.00487 AFIX 43 H35 2 0.838210 0.658710 0.190263 11.00000 -1.20000 AFIX 0 C36 1 0.675597 0.609252 0.281932 11.00000 0.01954 0.02675 = 0.01621 0.00097 -0.00129 -0.00316 C37 1 0.744876 0.661343 0.256531 11.00000 0.02022 0.03210 = 0.01935 0.00604 -0.00216 -0.00639 C38 1 0.770306 0.751463 0.276367 11.00000 0.02674 0.03194 = 0.02921 0.00439 0.00123 -0.01351 AFIX 13 H38 2 0.733276 0.764643 0.311832 11.00000 -1.20000 AFIX 0 C39 1 0.877232 0.758914 0.295113 11.00000 0.02950 0.04591 = 0.04056 0.00583 0.00249 -0.02005 AFIX 137 H39A 2 0.894523 0.715137 0.324914 11.00000 -1.50000 H39B 2 0.890397 0.815752 0.312007 11.00000 -1.50000 H39C 2 0.915157 0.750619 0.260407 11.00000 -1.50000 AFIX 0 C40 1 0.741980 0.817220 0.228271 11.00000 0.03653 0.02896 = 0.04137 0.00475 0.00278 -0.01271 AFIX 137 H40A 2 0.780413 0.808101 0.193885 11.00000 -1.50000 H40B 2 0.753569 0.875006 0.243928 11.00000 -1.50000 H40C 2 0.673818 0.810661 0.216202 11.00000 -1.50000 AFIX 0 C41 1 0.336542 0.750914 0.495512 11.00000 0.01800 0.02835 = 0.02550 0.00570 -0.00152 -0.00804 AFIX 13 H41 2 0.401437 0.743609 0.516051 11.00000 -1.20000 AFIX 0 C42 1 0.265057 0.695422 0.528097 11.00000 0.02471 0.03350 = 0.02190 0.00664 0.00032 -0.00738 AFIX 23 H42A 2 0.290738 0.636511 0.531549 11.00000 -1.20000 H42B 2 0.260656 0.718077 0.568800 11.00000 -1.20000 AFIX 0 C43 1 0.209098 0.827237 0.398013 11.00000 0.02200 0.03781 = 0.02922 0.01074 0.00373 -0.00402 AFIX 23 H43A 2 0.141941 0.834315 0.382198 11.00000 -1.20000 H43B 2 0.250711 0.856417 0.370305 11.00000 -1.20000 AFIX 0 C44 1 0.233132 0.732193 0.398346 11.00000 0.01953 0.03109 = 0.02235 0.00170 0.00191 -0.01343 AFIX 13 H44 2 0.231625 0.712480 0.356156 11.00000 -1.20000 AFIX 0 C45 1 0.161131 0.676945 0.430918 11.00000 0.01811 0.03622 = 0.03288 0.00675 -0.00346 -0.01292 AFIX 23 H45A 2 0.095610 0.689136 0.413895 11.00000 -1.20000 H45B 2 0.174771 0.615890 0.423418 11.00000 -1.20000 AFIX 0 C46 1 0.163458 0.691559 0.497868 11.00000 0.02102 0.03934 = 0.03022 0.01282 0.00029 -0.01212 AFIX 23 H46A 2 0.127520 0.644844 0.516151 11.00000 -1.20000 H46B 2 0.130005 0.745872 0.505628 11.00000 -1.20000 AFIX 0 C47 1 0.220553 0.872543 0.458565 11.00000 0.03040 0.02604 = 0.03969 0.00620 0.00644 -0.00568 AFIX 23 H47A 2 0.163749 0.859750 0.481262 11.00000 -1.20000 H47B 2 0.222165 0.935105 0.451937 11.00000 -1.20000 AFIX 0 C48 1 0.311551 0.846170 0.496013 11.00000 0.02982 0.02970 = 0.02596 -0.00145 0.00587 -0.01166 AFIX 23 H48A 2 0.366508 0.878573 0.481658 11.00000 -1.20000 H48B 2 0.303844 0.863682 0.537608 11.00000 -1.20000 AFIX 0 B1 3 0.341404 0.715605 0.427692 11.00000 0.01695 0.01894 = 0.02858 0.00327 -0.00115 -0.00670 AFIX 13 H1 2 0.355809 0.652955 0.428162 11.00000 -1.20000 AFIX 0 N3 4 0.407668 0.214297 0.089834 11.00000 0.01635 0.02130 = 0.01947 0.00353 0.00023 -0.00648 N4 4 0.377690 0.146860 0.170758 11.00000 0.01821 0.02216 = 0.02135 0.00446 0.00101 -0.01060 C49 1 0.577576 0.267977 0.111282 11.00000 0.02078 0.02591 = 0.02333 0.00461 0.00099 -0.01193 AFIX 23 H49A 2 0.610422 0.288340 0.148723 11.00000 -1.20000 H49B 2 0.556959 0.319266 0.088196 11.00000 -1.20000 AFIX 0 C50 1 0.490211 0.221075 0.126623 11.00000 0.01896 0.02371 = 0.01864 0.00025 -0.00054 -0.00478 C51 1 0.472004 0.178271 0.177994 11.00000 0.01509 0.02094 = 0.02440 -0.00009 0.00237 -0.00835 C52 1 0.340199 0.168486 0.116716 11.00000 0.01916 0.02397 = 0.02078 0.00139 0.00007 -0.00814 C53 1 0.453012 0.474728 0.088466 11.00000 0.03052 0.02335 = 0.03767 0.00009 -0.00259 -0.00820 AFIX 137 H53A 2 0.516402 0.453728 0.078970 11.00000 -1.50000 H53B 2 0.457737 0.503150 0.127226 11.00000 -1.50000 H53C 2 0.429589 0.515525 0.058006 11.00000 -1.50000 AFIX 0 C54 1 0.383079 0.399271 0.090337 11.00000 0.02364 0.02360 = 0.02759 0.00483 -0.00062 -0.00437 AFIX 13 H54 2 0.404979 0.361422 0.124180 11.00000 -1.20000 AFIX 0 C55 1 0.281641 0.432454 0.102079 11.00000 0.03152 0.02650 = 0.04030 0.00166 0.00967 -0.00686 AFIX 137 H55A 2 0.258618 0.469677 0.069343 11.00000 -1.50000 H55B 2 0.284189 0.464849 0.139309 11.00000 -1.50000 H55C 2 0.237840 0.383861 0.105027 11.00000 -1.50000 AFIX 0 C56 1 0.381454 0.346384 0.033586 11.00000 0.01748 0.02288 = 0.02983 0.00398 -0.00002 -0.00637 C57 1 0.367516 0.386956 -0.021121 11.00000 0.02877 0.02483 = 0.02926 0.01043 -0.00158 -0.00762 AFIX 43 H57 2 0.360012 0.447326 -0.022432 11.00000 -1.20000 AFIX 0 C58 1 0.364402 0.341565 -0.073113 11.00000 0.03352 0.03814 = 0.02848 0.01335 -0.00127 -0.00634 AFIX 43 H58 2 0.355821 0.370738 -0.109956 11.00000 -1.20000 AFIX 0 C59 1 0.373686 0.253470 -0.072258 11.00000 0.03271 0.03040 = 0.02311 0.00094 -0.00223 -0.00733 AFIX 43 H59 2 0.370784 0.223049 -0.108753 11.00000 -1.20000 AFIX 0 C60 1 0.387194 0.208171 -0.019209 11.00000 0.01870 0.02944 = 0.02336 0.00240 -0.00053 -0.00989 C61 1 0.392228 0.256921 0.032802 11.00000 0.01495 0.02400 = 0.02012 0.00593 -0.00043 -0.00889 C62 1 0.394996 0.111191 -0.020994 11.00000 0.02567 0.02527 = 0.02077 0.00003 -0.00082 -0.00540 AFIX 13 H62 2 0.402516 0.089793 0.020765 11.00000 -1.20000 AFIX 0 C63 1 0.303760 0.071317 -0.050580 11.00000 0.03118 0.02962 = 0.03582 -0.00210 -0.00058 -0.01261 AFIX 137 H63A 2 0.248009 0.089377 -0.029339 11.00000 -1.50000 H63B 2 0.308986 0.008831 -0.049325 11.00000 -1.50000 H63C 2 0.296050 0.090291 -0.091961 11.00000 -1.50000 AFIX 0 C64 1 0.482381 0.082224 -0.053652 11.00000 0.03096 0.03032 = 0.03440 0.00011 0.00344 -0.00393 AFIX 137 H64A 2 0.479896 0.107785 -0.093350 11.00000 -1.50000 H64B 2 0.482023 0.019746 -0.057145 11.00000 -1.50000 H64C 2 0.541144 0.100606 -0.031361 11.00000 -1.50000 AFIX 0 C65 1 0.183790 0.199771 0.060547 11.00000 0.01962 0.02428 = 0.02770 0.00320 0.00016 -0.00849 AFIX 43 H65 2 0.203249 0.257233 0.054701 11.00000 -1.20000 AFIX 0 C66 1 0.245194 0.142755 0.091550 11.00000 0.01900 0.02603 = 0.01924 0.00174 0.00216 -0.01000 C67 1 0.216148 0.058777 0.098919 11.00000 0.02454 0.02529 = 0.02797 0.00243 0.00256 -0.00875 AFIX 43 H67 2 0.258122 0.019136 0.119011 11.00000 -1.20000 AFIX 0 C68 1 0.125747 0.032420 0.076981 11.00000 0.02833 0.03018 = 0.03404 -0.00135 0.00096 -0.01536 AFIX 43 H68 2 0.105638 -0.024840 0.082898 11.00000 -1.20000 AFIX 0 C69 1 0.065408 0.088973 0.046762 11.00000 0.02094 0.03559 = 0.04106 -0.01008 -0.00065 -0.00996 AFIX 43 H69 2 0.003781 0.070864 0.031652 11.00000 -1.20000 AFIX 0 C70 1 0.094917 0.172479 0.038459 11.00000 0.02145 0.02837 = 0.03680 0.00045 -0.00348 -0.00475 AFIX 43 H70 2 0.053390 0.211386 0.017286 11.00000 -1.20000 AFIX 0 C71 1 0.361464 -0.114282 0.184480 11.00000 0.04524 0.02377 = 0.03362 0.00460 0.00259 -0.00791 AFIX 137 H71A 2 0.348814 -0.150312 0.218670 11.00000 -1.50000 H71B 2 0.401757 -0.145642 0.157791 11.00000 -1.50000 H71C 2 0.300628 -0.099110 0.163231 11.00000 -1.50000 AFIX 0 C72 1 0.413301 -0.032738 0.205951 11.00000 0.03173 0.02656 = 0.02785 0.00543 0.00487 -0.00485 AFIX 13 H72 2 0.436398 -0.002235 0.170568 11.00000 -1.20000 AFIX 0 C73 1 0.500522 -0.057467 0.246255 11.00000 0.03152 0.03228 = 0.04573 0.00743 -0.00188 -0.00273 AFIX 137 H73A 2 0.534106 -0.005613 0.260341 11.00000 -1.50000 H73B 2 0.543918 -0.092753 0.224000 11.00000 -1.50000 H73C 2 0.479530 -0.089910 0.280295 11.00000 -1.50000 AFIX 0 C74 1 0.345812 0.026151 0.236526 11.00000 0.02439 0.02162 = 0.02268 0.00270 -0.00096 -0.00911 C75 1 0.297759 -0.004517 0.284780 11.00000 0.03242 0.03062 = 0.02623 0.00606 -0.00016 -0.01671 AFIX 43 H75 2 0.311552 -0.060464 0.299302 11.00000 -1.20000 AFIX 0 C76 1 0.230985 0.044337 0.311753 11.00000 0.03039 0.03678 = 0.02343 0.00390 0.00309 -0.01888 AFIX 43 H76 2 0.200055 0.022233 0.344851 11.00000 -1.20000 AFIX 0 C77 1 0.208555 0.125992 0.290759 11.00000 0.02450 0.03613 = 0.02957 0.00133 0.00450 -0.01058 AFIX 43 H77 2 0.160689 0.158367 0.308848 11.00000 -1.20000 AFIX 0 C78 1 0.255395 0.161044 0.243478 11.00000 0.01947 0.02604 = 0.02288 -0.00057 -0.00143 -0.01072 C79 1 0.324373 0.109254 0.217771 11.00000 0.02040 0.02770 = 0.01758 0.00296 -0.00021 -0.01220 C80 1 0.229507 0.251428 0.222966 11.00000 0.02868 0.02990 = 0.02842 0.00610 0.00328 -0.00303 AFIX 13 H80 2 0.266453 0.264486 0.187442 11.00000 -1.20000 AFIX 0 C81 1 0.257683 0.317593 0.271212 11.00000 0.03773 0.02890 = 0.04281 0.00393 0.00528 -0.00516 AFIX 137 H81A 2 0.224881 0.304278 0.307282 11.00000 -1.50000 H81B 2 0.238923 0.374833 0.257179 11.00000 -1.50000 H81C 2 0.327220 0.315880 0.279953 11.00000 -1.50000 AFIX 0 C82 1 0.122314 0.258918 0.204535 11.00000 0.03002 0.04333 = 0.03744 0.00549 -0.00048 -0.00055 AFIX 137 H82A 2 0.104258 0.213941 0.175759 11.00000 -1.50000 H82B 2 0.109459 0.315060 0.186481 11.00000 -1.50000 H82C 2 0.084774 0.252537 0.239595 11.00000 -1.50000 AFIX 0 C83 1 0.537333 0.165509 0.230433 11.00000 0.02013 0.02245 = 0.02266 0.00580 -0.00204 -0.00945 C84 1 0.631630 0.142878 0.220536 11.00000 0.02606 0.02578 = 0.02416 0.00437 0.00110 -0.00896 AFIX 43 H84 2 0.649712 0.132617 0.181250 11.00000 -1.20000 AFIX 0 C85 1 0.699190 0.135290 0.267907 11.00000 0.01982 0.03340 = 0.03212 0.00732 -0.00340 -0.00725 AFIX 43 H85 2 0.763391 0.120258 0.260786 11.00000 -1.20000 AFIX 0 C86 1 0.673847 0.149377 0.325076 11.00000 0.03079 0.02812 = 0.02632 0.00765 -0.00873 -0.01256 AFIX 43 H86 2 0.720532 0.144311 0.357233 11.00000 -1.20000 AFIX 0 C87 1 0.579567 0.171102 0.335794 11.00000 0.03167 0.02143 = 0.02191 0.00789 -0.00148 -0.01380 AFIX 43 H87 2 0.561660 0.180260 0.375244 11.00000 -1.20000 AFIX 0 C88 1 0.512616 0.179192 0.288854 11.00000 0.02098 0.02288 = 0.02630 0.00383 0.00193 -0.01045 AFIX 43 H88 2 0.448553 0.194322 0.296259 11.00000 -1.20000 AFIX 0 C89 1 0.663634 0.251014 0.004633 11.00000 0.01969 0.02607 = 0.02687 0.00143 0.00104 -0.00934 AFIX 13 H89 2 0.598650 0.243813 -0.015817 11.00000 -1.20000 AFIX 0 C90 1 0.734802 0.195616 -0.028401 11.00000 0.02854 0.03377 = 0.02609 0.00034 0.00184 -0.00793 AFIX 23 H90A 2 0.739237 0.218625 -0.069002 11.00000 -1.20000 H90B 2 0.708996 0.136748 -0.032078 11.00000 -1.20000 AFIX 0 C91 1 0.836696 0.191620 0.002071 11.00000 0.02306 0.04073 = 0.03164 -0.00305 0.00305 -0.00629 AFIX 23 H91B 2 0.872589 0.144856 -0.016169 11.00000 -1.20000 H91A 2 0.870317 0.245892 -0.005625 11.00000 -1.20000 AFIX 0 C92 1 0.838712 0.176930 0.069379 11.00000 0.02132 0.03467 = 0.03366 0.00080 -0.00231 -0.00576 AFIX 23 H92A 2 0.904275 0.188943 0.086424 11.00000 -1.20000 H92B 2 0.824939 0.115862 0.076762 11.00000 -1.20000 AFIX 0 C93 1 0.767316 0.231754 0.102176 11.00000 0.02178 0.02863 = 0.02268 0.00330 0.00046 -0.00835 AFIX 13 H93 2 0.768994 0.212037 0.144364 11.00000 -1.20000 AFIX 0 C94 1 0.790939 0.327711 0.102259 11.00000 0.01955 0.03754 = 0.03020 -0.00276 0.00142 -0.01130 AFIX 23 H94A 2 0.858109 0.335234 0.117947 11.00000 -1.20000 H94B 2 0.749275 0.356780 0.129981 11.00000 -1.20000 AFIX 0 C95 1 0.778943 0.372670 0.041655 11.00000 0.02932 0.02807 = 0.04464 0.00044 0.00731 -0.01251 AFIX 23 H95A 2 0.777540 0.435243 0.048270 11.00000 -1.20000 H95B 2 0.835700 0.359845 0.018931 11.00000 -1.20000 AFIX 0 C96 1 0.688719 0.346972 0.004225 11.00000 0.02780 0.02966 = 0.03007 0.00665 0.00846 -0.00646 AFIX 23 H96A 2 0.696692 0.364599 -0.037315 11.00000 -1.20000 H96B 2 0.633747 0.379353 0.018547 11.00000 -1.20000 AFIX 0 B2 3 0.658564 0.215749 0.072792 11.00000 0.02256 0.01798 = 0.02628 0.00329 -0.00138 -0.00849 AFIX 13 H2 2 0.643864 0.153142 0.072266 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_tkp180121_0ma_a_a.res in P-1 REM R1 = 0.0761 for 10714 Fo > 4sig(Fo) and 0.1184 for all 18007 data REM 935 parameters refined using 0 restraints END WGHT 0.1214 0.0000 REM Highest difference peak 0.349, deepest hole -0.348, 1-sigma level 0.068 Q1 1 0.3807 0.6287 0.4228 11.00000 0.05 0.35 Q2 1 1.0000 0.5000 0.5000 10.50000 0.05 0.34 Q3 1 0.3629 0.3852 0.0410 11.00000 0.05 0.32 Q4 1 0.4995 0.7234 0.3295 11.00000 0.05 0.31 Q5 1 0.6448 0.6224 0.3172 11.00000 0.05 0.29 Q6 1 0.0944 0.3208 0.2123 11.00000 0.05 0.29 Q7 1 0.4951 0.6825 0.2947 11.00000 0.05 0.29 Q8 1 0.2345 0.8378 0.3424 11.00000 0.05 0.28 Q9 1 0.3143 0.7596 0.4515 11.00000 0.05 0.27 Q10 1 0.3985 0.3357 -0.0178 11.00000 0.05 0.27 Q11 1 0.6120 0.2499 -0.0430 11.00000 0.05 0.26 Q12 1 0.4013 0.3506 0.0760 11.00000 0.05 0.26 Q13 1 0.5105 0.1691 0.2137 11.00000 0.05 0.25 Q14 1 0.1608 0.8385 0.3566 11.00000 0.05 0.25 Q15 1 0.1112 0.3433 0.1889 11.00000 0.05 0.25 Q16 1 0.0958 0.0834 0.0823 11.00000 0.05 0.25 Q17 1 0.7222 0.6187 0.3276 11.00000 0.05 0.25 Q18 1 0.3594 0.7394 0.4897 11.00000 0.05 0.25 Q19 1 0.3379 0.4721 -0.0090 11.00000 0.05 0.25 Q20 1 0.7583 0.3866 0.1071 11.00000 0.05 0.24 ; _shelx_res_checksum 26158 _shelx_hkl_file ; 2 0 0 92.29 9.60 2 0 0 65.69 9.30 -2 0 0 81.59 9.40 -2 0 0 62.99 9.30 4 0 0 11.50 2.90 4 0 0 10.80 2.90 -4 0 0 6.10 2.80 -4 0 0 6.50 2.90 -4 0 0 8.40 2.80 5 0 0 967.10 97.19 5 0 0 726.73 96.89 -5 0 0 735.03 96.99 -5 0 0 914.21 97.19 6 0 0 59.89 9.50 6 0 0 69.79 10.30 -6 0 0 51.89 9.80 -6 0 0 47.20 9.70 7 0 0 3761.32 373.86 7 0 0 2928.11 373.56 -7 0 0 2992.90 373.66 -7 0 0 3359.66 373.76 8 0 0 1621.44 171.78 8 0 0 1492.65 171.98 -8 0 0 1273.47 171.48 -8 0 0 1526.65 171.78 9 0 0 86.79 15.20 9 0 0 117.29 15.70 -9 0 0 77.79 16.60 -9 0 0 85.39 15.00 -9 0 0 88.39 15.00 10 0 0 86.29 17.70 10 0 0 104.19 16.00 -10 0 0 92.59 16.00 -10 0 0 94.29 16.50 -10 0 0 92.29 20.10 11 0 0 188.28 27.10 11 0 0 196.28 27.10 -11 0 0 177.98 31.30 -11 0 0 173.78 26.80 12 0 0 4.10 7.00 -12 0 0 -2.30 5.60 13 0 0 151.68 24.80 -13 0 0 160.88 25.90 14 0 0 -4.50 6.50 -14 0 0 10.40 7.10 15 0 0 3.50 8.80 -15 0 0 -9.70 7.00 16 0 0 0.40 13.80 -16 0 0 -11.40 5.60 -16 -1 0 49.40 16.60 16 1 0 65.79 24.20 -15 -1 0 264.07 38.50 15 1 0 245.98 37.00 -14 -1 0 7.30 7.40 14 1 0 7.00 7.80 -13 -1 0 18.20 8.40 13 1 0 27.30 10.60 -12 -1 0 60.29 13.30 12 1 0 49.20 12.70 -11 -1 0 887.51 106.69 -11 -1 0 887.61 109.59 11 1 0 993.90 106.19 11 1 0 777.22 105.69 -10 -1 0 478.35 54.19 -10 -1 0 353.26 52.89 -10 -1 0 420.66 59.29 10 1 0 482.95 55.49 10 1 0 427.86 53.79 -9 -1 0 440.66 61.79 -9 -1 0 567.14 65.39 -9 -1 0 492.75 62.19 9 1 0 552.34 62.59 -8 -1 0 29.60 8.20 -8 -1 0 32.70 8.90 -8 -1 0 19.80 6.30 8 1 0 28.20 7.50 8 1 0 27.40 7.10 -7 -1 0 2406.46 268.07 7 1 0 2254.27 267.87 -6 -1 0 2771.52 299.07 -6 -1 0 2547.65 298.87 6 1 0 2504.75 298.87 -5 -1 0 107.79 14.60 -5 -1 0 89.69 12.70 -5 -1 0 77.59 12.40 5 1 0 100.69 12.80 -4 -1 0 12.60 4.40 -4 -1 0 15.50 3.60 -4 -1 0 12.30 3.50 4 1 0 27.00 5.50 4 1 0 20.30 4.10 4 1 0 15.70 3.80 -3 -1 0 1113.69 130.59 3 1 0 1176.18 130.19 3 1 0 1111.59 130.09 -2 -1 0 1132.79 128.59 -2 -1 0 1223.88 129.79 2 1 0 1021.00 128.49 2 -1 0 1036.20 120.39 2 -1 0 1025.10 120.29 -2 1 0 949.40 120.79 -2 1 0 1176.98 120.49 3 -1 0 1322.97 137.99 3 -1 0 1202.88 137.89 -3 1 0 1070.99 137.79 4 -1 0 13.90 3.90 -4 1 0 10.30 3.40 -4 1 0 20.70 5.20 5 -1 0 79.89 12.20 5 -1 0 89.99 12.60 -5 1 0 85.49 12.60 6 -1 0 2698.53 294.97 6 -1 0 2725.33 294.57 -6 1 0 2276.37 294.47 7 -1 0 2353.46 270.87 7 -1 0 2582.04 271.67 -7 1 0 2136.09 271.07 8 -1 0 24.90 7.70 8 -1 0 31.10 7.60 -8 1 0 29.70 7.30 -8 1 0 20.50 7.10 -8 1 0 19.80 7.50 9 -1 0 471.85 60.79 9 -1 0 533.95 61.89 -9 1 0 557.64 61.69 -9 1 0 435.26 60.89 10 -1 0 435.66 58.49 10 -1 0 399.06 57.89 -10 1 0 475.25 58.39 -10 1 0 466.55 61.09 -10 1 0 576.94 61.89 11 -1 0 746.73 99.69 11 -1 0 885.41 102.49 -11 1 0 772.62 100.59 -11 1 0 950.10 104.49 12 -1 0 34.70 11.10 -12 1 0 42.50 11.90 -12 1 0 44.20 15.80 13 -1 0 22.90 10.60 -13 1 0 22.70 10.10 14 -1 0 0.20 7.50 -14 1 0 1.00 8.30 15 -1 0 202.08 33.70 -15 1 0 229.58 34.70 16 -1 0 61.79 17.50 -16 1 0 27.80 11.90 -16 -2 0 1.60 8.80 16 2 0 -2.10 9.90 -15 -2 0 -0.30 8.20 15 2 0 -3.70 7.90 -14 -2 0 194.88 29.20 14 2 0 179.28 28.70 -13 -2 0 -10.50 4.80 13 2 0 -4.90 6.40 -12 -2 0 286.37 42.60 12 2 0 386.76 43.50 12 2 0 305.47 42.90 -11 -2 0 10.80 5.90 -11 -2 0 -5.80 7.60 11 2 0 2.20 5.50 11 2 0 6.90 7.00 -10 -2 0 4.10 4.40 -10 -2 0 -1.90 6.40 10 2 0 2.60 5.00 10 2 0 2.40 5.50 -9 -2 0 63.69 12.30 -9 -2 0 50.19 13.30 9 2 0 98.99 13.80 9 2 0 73.69 12.50 -8 -2 0 491.45 63.79 -8 -2 0 528.15 61.09 8 2 0 576.74 61.29 8 2 0 432.66 60.69 -7 -2 0 478.75 60.19 -7 -2 0 498.95 57.59 7 2 0 411.06 57.29 7 2 0 532.15 57.59 -6 -2 0 419.16 52.59 -6 -2 0 501.65 55.79 6 2 0 465.75 52.99 6 2 0 393.86 52.69 -5 -2 0 665.03 74.89 -5 -2 0 670.33 77.19 5 2 0 600.04 74.89 5 2 0 631.74 74.89 -4 -2 0 4408.56 476.15 -4 -2 0 4228.58 478.25 4 2 0 3890.31 476.15 -3 -2 0 1172.08 130.29 -3 -2 0 1222.98 132.69 3 2 0 1020.50 130.29 -2 -2 0 3216.68 351.66 -2 -2 0 2920.01 349.17 -1 -2 0 4066.69 463.25 -1 -2 0 4224.98 461.95 1 2 0 3877.21 461.95 1 2 0 4029.10 463.25 0 -2 0 7048.09 780.52 0 2 0 6949.10 780.52 0 2 0 6565.44 781.32 1 -2 0 3139.19 368.56 1 -2 0 2997.80 369.06 1 -2 0 3058.29 368.76 -1 2 0 3628.04 370.06 -1 2 0 3042.50 369.06 -1 2 0 3531.35 368.96 2 -2 0 2283.07 295.27 2 -2 0 2620.54 295.17 2 -2 0 2619.64 295.17 -2 2 0 2270.37 294.97 -2 2 0 2994.40 295.27 -2 2 0 2710.23 295.57 3 -2 0 966.40 116.49 3 -2 0 1125.39 116.59 3 -2 0 1012.60 116.19 -3 2 0 920.61 116.19 4 -2 0 3513.55 414.36 4 -2 0 3651.43 414.26 4 -2 0 4013.60 414.76 -4 2 0 3323.47 414.26 5 -2 0 534.45 64.89 5 -2 0 619.04 65.39 -5 2 0 487.25 64.69 6 -2 0 453.05 47.70 6 -2 0 350.16 47.00 -6 2 0 353.06 46.80 7 -2 0 374.26 49.10 7 -2 0 470.15 50.19 -7 2 0 364.56 49.20 8 -2 0 530.55 56.49 8 -2 0 391.96 54.99 -8 2 0 440.26 55.69 9 -2 0 62.89 12.70 9 -2 0 48.10 11.70 -9 2 0 69.39 13.20 10 -2 0 9.30 6.20 10 -2 0 0.10 6.50 -10 2 0 -1.10 5.70 -10 2 0 -4.50 5.80 -10 2 0 0.40 3.90 11 -2 0 -3.60 5.50 -11 2 0 3.40 8.30 -11 2 0 11.80 7.10 -12 2 0 348.97 49.80 -12 2 0 332.87 46.10 13 -2 0 13.00 7.20 -13 2 0 0.20 5.10 14 -2 0 99.19 21.60 -14 2 0 135.89 25.00 15 -2 0 0.40 8.20 -15 2 0 -1.20 7.10 16 -2 0 13.50 11.90 16 -2 0 -0.50 8.60 -16 2 0 6.90 9.90 -16 -3 0 13.40 10.00 16 3 0 20.50 13.80 -15 -3 0 38.30 13.50 15 3 0 49.99 14.70 -14 -3 0 -4.80 6.10 14 3 0 -5.00 8.40 -13 -3 0 -3.10 5.40 13 3 0 3.20 7.30 -12 -3 0 -0.10 4.70 12 3 0 19.60 7.40 12 3 0 3.40 7.50 -11 -3 0 89.09 16.40 11 3 0 107.69 17.30 11 3 0 69.99 16.80 -10 -3 0 52.69 15.20 -10 -3 0 65.59 12.30 10 3 0 54.89 11.70 10 3 0 58.79 12.50 -9 -3 0 85.99 15.10 9 3 0 119.19 16.40 9 3 0 100.29 15.70 -8 -3 0 25.10 6.00 -8 -3 0 22.80 8.50 8 3 0 23.40 6.80 8 3 0 33.00 9.80 8 3 0 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279.97 36.80 -2 6 0 241.18 35.50 3 -6 0 202.18 24.50 3 -6 0 135.99 25.90 3 -6 0 163.58 25.60 -3 6 0 193.38 29.60 -3 6 0 191.38 26.70 -3 6 0 201.18 26.00 -3 6 0 155.68 24.20 4 -6 0 10.50 6.70 4 -6 0 12.80 8.50 4 -6 0 1.00 4.10 -4 6 0 0.00 5.00 -4 6 0 8.20 7.40 -4 6 0 10.10 5.50 -4 6 0 10.10 7.00 5 -6 0 77.79 17.50 5 -6 0 82.29 16.00 -5 6 0 92.19 16.50 -5 6 0 84.99 16.90 -5 6 0 94.59 15.50 6 -6 0 100.19 21.10 6 -6 0 112.59 20.70 -6 6 0 118.59 19.00 -6 6 0 142.79 20.70 7 -6 0 180.48 29.40 7 -6 0 215.58 28.40 8 -6 0 -0.80 5.80 8 -6 0 -3.10 5.70 8 -6 0 2.40 4.40 -8 6 0 1.50 5.00 -8 6 0 2.90 5.40 9 -6 0 55.49 13.20 9 -6 0 56.89 15.10 -9 6 0 62.39 14.20 10 -6 0 33.00 13.10 10 -6 0 56.69 13.70 -10 6 0 68.69 15.20 11 -6 0 381.26 53.49 11 -6 0 415.86 52.89 -11 6 0 402.56 54.09 12 -6 0 34.60 11.80 12 -6 0 23.10 9.70 -12 6 0 25.00 11.80 13 -6 0 -6.40 5.90 13 -6 0 4.40 7.90 -13 6 0 -1.80 7.50 14 -6 0 57.89 15.10 14 -6 0 54.69 17.00 -14 6 0 110.29 26.50 15 -6 0 2.40 10.80 15 -6 0 -8.20 7.90 -15 6 0 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3.70 10.70 -15 -6 3 189.48 29.90 15 6 -3 212.58 32.80 -14 -6 3 53.49 12.10 14 6 -3 23.90 18.00 14 6 -3 34.60 12.80 -13 -6 3 9.90 6.40 13 6 -3 -14.40 6.40 13 6 -3 1.90 10.80 13 6 -3 0.40 8.50 -12 -6 3 30.20 8.50 12 6 -3 19.00 11.30 12 6 -3 26.30 12.20 12 6 -3 25.50 8.60 -11 -6 3 308.27 37.60 11 6 -3 358.96 41.30 11 6 -3 236.88 37.70 -10 -6 3 336.87 38.90 10 6 -3 348.77 42.70 10 6 -3 260.67 38.50 -9 -6 3 35.90 7.50 -9 -6 3 30.80 13.30 9 6 -3 44.30 12.10 9 6 -3 51.69 15.30 9 6 -3 32.90 7.70 -8 -6 3 21.80 4.80 -8 -6 3 14.00 9.90 8 6 -3 20.90 8.60 -7 -6 3 13.70 11.90 7 6 -3 22.40 10.70 -6 -6 3 51.19 15.80 -6 -6 3 52.49 6.80 6 6 -3 33.40 12.50 -5 -6 3 161.88 33.30 5 6 -3 220.68 33.50 -4 -6 3 718.63 89.19 4 6 -3 651.53 86.39 -3 -6 3 565.64 70.79 -3 -6 3 650.93 81.39 3 6 -3 640.04 79.99 3 6 -3 686.73 75.99 -2 -6 3 301.07 34.30 -2 -6 3 273.57 42.40 2 6 -3 321.97 43.00 2 6 -3 267.17 37.60 -1 -6 3 12.40 8.20 1 6 -3 20.40 6.30 1 6 -3 21.60 9.50 0 -6 3 1963.20 214.88 0 -6 3 1939.01 213.18 0 -6 3 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31.80 11 -6 3 103.49 19.20 11 -6 3 81.99 20.00 -11 6 -3 126.99 22.70 12 -6 3 -2.60 5.00 12 -6 3 -2.50 7.70 -12 6 -3 -8.10 6.00 13 -6 3 5.70 5.60 13 -6 3 22.00 10.60 -13 6 -3 18.60 10.60 14 -6 3 18.30 9.20 14 -6 3 29.70 11.20 -14 6 -3 16.70 11.60 15 -6 3 83.79 18.40 -15 6 -3 88.59 22.80 -15 -7 3 8.70 8.30 15 7 -3 -13.00 11.30 15 7 -3 7.60 14.20 -14 -7 3 82.39 15.80 14 7 -3 52.39 16.10 14 7 -3 114.79 29.90 14 7 -3 144.09 28.60 -13 -7 3 120.79 17.90 13 7 -3 84.49 18.30 -12 -7 3 17.50 6.00 12 7 -3 3.10 10.40 12 7 -3 10.40 10.80 -11 -7 3 73.09 13.00 11 7 -3 98.29 22.90 11 7 -3 79.99 18.00 -10 -7 3 1.90 3.50 10 7 -3 8.40 10.40 10 7 -3 -0.20 7.20 -9 -7 3 493.75 55.89 9 7 -3 434.46 59.79 -8 -7 3 681.13 94.89 -8 -7 3 743.03 83.89 -7 -7 3 4.60 10.80 7 7 -3 1.00 8.00 6 7 -3 13.30 9.80 6 7 -3 22.30 9.10 -5 -7 3 553.14 72.49 5 7 -3 476.45 65.09 5 7 -3 536.15 69.89 -4 -7 3 2104.49 243.28 4 7 -3 1915.81 240.18 4 7 -3 2073.79 236.88 -3 -7 3 743.73 84.29 -3 -7 3 767.82 95.99 3 7 -3 804.72 94.69 3 7 -3 633.64 88.59 -2 -7 3 6.20 10.10 -2 -7 3 4.30 2.20 2 7 -3 -7.40 3.30 2 7 -3 13.80 10.00 -1 -7 3 987.90 120.49 -1 -7 3 999.80 111.89 1 7 -3 867.11 114.79 1 7 -3 1013.80 120.49 0 -7 3 746.93 88.39 0 -7 3 756.12 80.69 0 -7 3 682.73 82.19 0 7 -3 584.54 80.49 0 7 -3 743.63 88.99 0 7 -3 633.64 82.69 1 -7 3 104.49 13.40 1 -7 3 81.69 19.50 1 -7 3 92.79 15.20 -1 7 -3 69.49 13.40 -1 7 -3 98.59 19.50 -1 7 -3 96.49 16.90 -1 7 -3 81.29 20.10 2 -7 3 264.27 36.80 2 -7 3 358.46 36.60 -2 7 -3 223.18 37.90 -2 7 -3 282.57 36.40 -2 7 -3 277.37 42.90 -2 7 -3 298.77 37.50 3 -7 3 -0.20 3.90 3 -7 3 5.30 4.30 -3 7 -3 1.70 4.20 -3 7 -3 1.80 3.70 -3 7 -3 1.60 7.00 -3 7 -3 1.20 5.10 4 -7 3 7.30 5.50 4 -7 3 5.60 4.20 4 -7 3 -1.00 6.60 -4 7 -3 5.20 4.50 -4 7 -3 7.80 9.20 -4 7 -3 1.20 5.60 -4 7 -3 3.30 4.50 5 -7 3 -5.50 4.00 5 -7 3 -2.60 5.60 5 -7 3 1.40 3.80 -5 7 -3 -0.50 3.60 -5 7 -3 -3.70 3.60 -5 7 -3 -0.70 4.70 6 -7 3 63.29 13.30 6 -7 3 46.10 14.60 6 -7 3 100.89 14.70 -6 7 -3 71.79 15.60 -6 7 -3 61.99 15.30 7 -7 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1023.60 130.59 7 9 -3 -0.50 9.10 6 9 -3 255.87 42.70 -5 -9 3 206.38 39.30 5 9 -3 201.18 37.40 5 9 -3 228.28 33.00 -4 -9 3 114.29 27.00 -4 -9 3 105.69 13.20 4 9 -3 99.89 23.40 4 9 -3 102.59 21.10 -3 -9 3 49.20 7.20 -3 -9 3 43.10 16.90 3 9 -3 49.50 13.20 3 9 -3 35.50 15.60 -2 -9 3 115.89 15.30 -2 -9 3 132.89 30.60 2 9 -3 106.39 21.50 2 9 -3 112.29 24.80 -1 -9 3 541.15 64.49 1 9 -3 553.64 69.49 1 9 -3 544.85 74.29 0 -9 3 23.90 5.60 0 -9 3 13.90 6.90 0 -9 3 12.10 11.10 0 9 -3 10.60 6.60 0 9 -3 18.90 11.30 1 -9 3 79.49 14.70 1 -9 3 77.39 19.90 1 -9 3 77.59 11.20 -1 9 -3 42.00 10.60 -1 9 -3 44.40 16.00 -1 9 -3 70.89 15.00 -1 9 -3 51.89 17.80 2 -9 3 37.90 10.30 2 -9 3 52.29 9.50 -2 9 -3 32.10 9.70 -2 9 -3 28.30 8.60 -2 9 -3 38.70 15.10 3 -9 3 11.80 5.60 3 -9 3 15.80 7.70 -3 9 -3 10.30 7.90 -3 9 -3 -2.50 6.70 -3 9 -3 4.70 5.60 -3 9 -3 6.00 5.60 4 -9 3 5.40 6.20 4 -9 3 2.50 5.90 -4 9 -3 24.40 11.00 -4 9 -3 11.80 6.00 -4 9 -3 10.70 5.50 -4 9 -3 10.90 7.50 5 -9 3 -6.70 4.50 5 -9 3 1.60 4.70 -5 9 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5 10 -3 213.68 37.00 -4 -10 3 968.30 109.09 4 10 -3 915.71 121.19 4 10 -3 939.41 116.69 -3 -10 3 120.89 32.10 -3 -10 3 159.18 18.90 3 10 -3 135.39 29.90 3 10 -3 131.29 26.30 -2 -10 3 29.90 15.20 -2 -10 3 8.60 3.50 2 10 -3 -1.10 8.40 2 10 -3 -7.20 5.90 -1 -10 3 678.43 77.59 -1 -10 3 579.04 87.49 1 10 -3 654.03 82.69 1 10 -3 700.53 89.19 0 -10 3 20.00 5.50 0 -10 3 13.50 11.80 0 -10 3 22.90 9.00 0 10 -3 12.30 10.80 0 10 -3 8.90 7.20 1 -10 3 5.20 4.60 1 -10 3 1.90 9.90 1 -10 3 3.90 5.60 -1 10 -3 -8.40 6.90 -1 10 -3 4.60 6.20 -1 10 -3 17.10 8.20 2 -10 3 -4.90 3.60 2 -10 3 5.70 7.30 -2 10 -3 0.50 10.00 -2 10 -3 1.90 5.50 -2 10 -3 1.60 7.10 -2 10 -3 2.90 5.30 3 -10 3 97.99 18.90 3 -10 3 132.09 18.10 -3 10 -3 91.29 25.70 -3 10 -3 112.89 21.20 -3 10 -3 88.59 20.40 -3 10 -3 91.49 18.30 4 -10 3 33.30 8.80 4 -10 3 35.30 10.40 -4 10 -3 20.00 11.20 -4 10 -3 29.00 11.40 -4 10 -3 18.80 12.80 -4 10 -3 28.10 10.10 5 -10 3 4.50 6.90 5 -10 3 14.00 7.20 -5 10 -3 -2.80 8.90 -5 10 -3 3.80 6.00 -5 10 -3 -7.50 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142.19 16.40 1 -7 4 113.69 17.30 -1 7 -4 97.99 17.80 -1 7 -4 105.59 16.30 -1 7 -4 95.79 22.70 2 -7 4 -3.00 3.20 2 -7 4 0.50 2.90 -2 7 -4 -7.20 3.20 -2 7 -4 11.10 9.70 -2 7 -4 -3.70 3.20 -2 7 -4 0.70 5.80 3 -7 4 886.91 91.59 -3 7 -4 798.32 91.19 -3 7 -4 684.83 97.59 -3 7 -4 799.72 92.89 -3 7 -4 639.14 92.29 4 -7 4 49.50 10.10 4 -7 4 50.79 10.60 -4 7 -4 47.80 11.50 -4 7 -4 34.80 10.60 -4 7 -4 29.80 13.50 -4 7 -4 46.40 10.50 5 -7 4 11.50 5.60 5 -7 4 17.40 9.00 5 -7 4 15.30 6.20 -5 7 -4 11.10 5.90 -5 7 -4 9.20 4.60 -5 7 -4 17.30 7.80 6 -7 4 62.49 12.20 6 -7 4 37.10 9.10 6 -7 4 35.40 12.90 -6 7 -4 33.20 10.70 7 -7 4 41.90 9.50 7 -7 4 60.89 12.60 7 -7 4 22.40 11.10 -7 7 -4 60.39 12.90 -7 7 -4 41.40 12.30 8 -7 4 32.00 10.80 8 -7 4 24.40 7.60 -8 7 -4 19.20 8.40 -8 7 -4 12.50 8.60 9 -7 4 28.40 9.80 9 -7 4 37.40 13.30 -9 7 -4 70.09 15.00 10 -7 4 21.90 9.00 10 -7 4 34.30 11.80 -10 7 -4 37.70 11.50 11 -7 4 53.59 14.80 11 -7 4 44.40 12.20 -11 7 -4 84.79 18.40 12 -7 4 119.69 26.50 12 -7 4 157.48 24.50 -12 7 -4 210.68 30.10 13 -7 4 24.20 10.30 13 -7 4 27.70 12.70 -13 7 -4 19.00 12.00 14 -7 4 27.20 13.10 14 -7 4 13.70 7.90 -14 7 -4 2.00 9.60 15 -7 4 75.89 20.20 15 -7 4 9.30 10.70 -15 7 -4 20.70 13.30 15 8 -4 138.09 30.80 15 8 -4 81.79 23.20 14 8 -4 40.50 20.30 14 8 -4 52.79 17.50 13 8 -4 94.59 25.30 12 8 -4 436.96 58.59 11 8 -4 11.00 11.00 11 8 -4 1.20 11.80 10 8 -4 18.20 12.70 10 8 -4 9.10 10.00 9 8 -4 255.87 41.30 9 8 -4 200.78 34.20 8 8 -4 29.50 13.90 -7 -8 4 68.09 22.90 7 8 -4 91.59 21.80 -6 -8 4 69.29 22.20 6 8 -4 42.10 14.70 6 8 -4 54.89 13.90 -5 -8 4 171.98 35.80 5 8 -4 192.38 29.90 5 8 -4 261.87 42.20 4 8 -4 620.84 75.89 4 8 -4 592.24 80.39 -3 -8 4 1109.19 128.59 -3 -8 4 912.01 114.99 3 8 -4 1081.99 126.29 3 8 -4 1006.50 120.69 -2 -8 4 433.36 50.29 -2 -8 4 464.35 62.69 2 8 -4 391.86 54.49 2 8 -4 433.26 60.79 -1 -8 4 480.35 57.59 -1 -8 4 523.15 67.89 1 8 -4 468.65 61.29 1 8 -4 497.95 67.69 0 -8 4 245.98 28.50 0 -8 4 232.58 37.10 0 8 -4 212.38 31.50 0 8 -4 193.48 28.80 0 8 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9.40 13 -8 4 0.50 8.50 13 -8 4 -1.70 6.70 -13 8 -4 2.60 9.10 14 -8 4 39.00 16.00 14 -8 4 45.90 12.60 -14 8 -4 65.19 19.20 14 9 -4 -19.10 10.80 14 9 -4 18.80 16.20 13 9 -4 5.80 11.60 13 9 -4 -6.50 13.00 12 9 -4 4.90 12.60 12 9 -4 3.20 13.40 11 9 -4 128.09 29.70 11 9 -4 138.89 26.60 10 9 -4 33.60 16.70 10 9 -4 50.69 14.00 9 9 -4 74.69 21.60 8 9 -4 9.90 11.40 7 9 -4 304.17 48.30 6 9 -4 63.59 18.80 -5 -9 4 33.00 15.40 5 9 -4 42.90 12.90 5 9 -4 37.70 14.30 -4 -9 4 1070.09 129.59 -4 -9 4 957.00 113.19 4 9 -4 992.30 125.19 4 9 -4 993.80 120.49 -3 -9 4 14.90 3.40 -3 -9 4 7.40 11.40 3 9 -4 15.90 8.00 -2 -9 4 264.17 45.90 -2 -9 4 287.97 33.50 2 9 -4 291.47 44.40 2 9 -4 253.17 38.10 -1 -9 4 94.29 11.90 -1 -9 4 57.39 20.80 1 9 -4 64.39 18.90 1 9 -4 72.29 16.30 0 -9 4 2.10 2.80 0 9 -4 -1.70 5.90 0 9 -4 -1.50 8.20 1 -9 4 336.47 39.10 1 -9 4 344.17 41.00 -1 9 -4 327.67 41.70 -1 9 -4 271.07 39.20 -1 9 -4 275.77 48.00 2 -9 4 6.70 5.10 2 -9 4 1.70 4.30 -2 9 -4 -1.70 4.80 -2 9 -4 21.70 13.40 -2 9 -4 1.00 9.60 -2 9 -4 -1.00 3.30 3 -9 4 158.88 20.10 3 -9 4 154.88 21.20 -3 9 -4 114.49 19.50 -3 9 -4 145.59 20.70 -3 9 -4 79.79 24.10 -3 9 -4 104.49 23.30 4 -9 4 62.89 13.30 -4 9 -4 60.99 13.00 -4 9 -4 52.69 11.90 -4 9 -4 58.69 14.50 5 -9 4 32.10 9.20 5 -9 4 53.59 11.30 -5 9 -4 36.70 12.00 -5 9 -4 9.60 13.10 -5 9 -4 26.10 8.50 -5 9 -4 23.70 7.90 6 -9 4 1.00 5.40 -6 9 -4 5.30 5.70 -6 9 -4 4.20 4.90 -6 9 -4 3.70 6.50 -6 9 -4 8.30 11.60 7 -9 4 26.20 13.00 7 -9 4 -1.70 6.10 -7 9 -4 13.50 13.50 9 -9 4 77.79 15.10 9 -9 4 53.69 18.20 -9 9 -4 72.59 17.10 10 -9 4 -2.50 6.40 10 -9 4 5.60 6.40 -10 9 -4 30.80 11.80 11 -9 4 127.59 27.40 11 -9 4 156.48 23.50 -11 9 -4 127.39 26.20 12 -9 4 -0.30 9.60 -12 9 -4 0.80 8.10 13 -9 4 31.40 13.60 13 -9 4 24.60 10.90 -13 9 -4 31.40 13.20 14 -9 4 63.09 18.80 14 -9 4 58.59 13.70 -14 9 -4 68.29 18.60 14 10 -4 -13.30 13.80 14 10 -4 12.00 17.80 13 10 -4 -11.40 12.00 13 10 -4 4.20 11.30 12 10 -4 53.39 25.50 12 10 -4 21.70 16.20 11 10 -4 17.30 13.20 11 10 -4 2.10 13.60 10 10 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10 -4 33.10 9.90 -5 10 -4 35.00 15.70 6 -10 4 41.90 11.50 -6 10 -4 40.00 18.10 -6 10 -4 53.59 14.00 -6 10 -4 42.20 11.30 7 -10 4 -3.10 6.00 -7 10 -4 13.80 7.60 -7 10 -4 -1.60 9.80 8 -10 4 91.19 21.50 8 -10 4 73.69 16.10 -8 10 -4 82.89 17.70 -8 10 -4 50.49 23.40 9 -10 4 12.50 7.90 9 -10 4 -3.60 8.30 -9 10 -4 -0.80 14.20 -9 10 -4 -4.80 6.60 10 -10 4 4.90 7.70 10 -10 4 28.40 11.10 -10 10 -4 3.30 8.10 11 -10 4 93.39 20.70 -11 10 -4 38.30 20.20 12 -10 4 23.00 7.70 12 -10 4 5.90 10.90 -12 10 -4 -3.80 10.30 13 -10 4 8.70 9.50 13 -10 4 13.30 13.30 -13 10 -4 11.10 11.00 13 11 -4 -7.80 13.60 13 11 -4 -9.70 11.40 12 11 -4 320.87 55.29 12 11 -4 436.46 64.49 11 11 -4 4.70 22.40 11 11 -4 -0.70 12.10 10 11 -4 19.50 17.60 9 11 -4 0.30 12.10 8 11 -4 382.56 60.59 7 11 -4 341.47 55.19 6 11 -4 15.20 12.70 5 11 -4 653.23 89.39 -4 -11 4 522.55 59.99 4 11 -4 496.75 74.09 -3 -11 4 90.99 11.90 3 11 -4 65.29 20.30 3 11 -4 75.09 17.60 -2 -11 4 460.95 53.59 2 11 -4 463.55 66.79 2 11 -4 407.66 58.99 -1 -11 4 119.09 15.70 1 11 -4 77.59 22.50 0 -11 4 124.59 16.60 0 11 -4 76.69 24.10 0 11 -4 109.99 22.40 1 -11 4 12.60 7.10 1 -11 4 9.70 4.80 -1 11 -4 16.70 8.20 -1 11 -4 -3.70 8.40 2 -11 4 266.77 35.50 2 -11 4 273.77 33.10 -2 11 -4 190.78 32.50 -2 11 -4 257.87 36.50 3 -11 4 43.50 12.40 3 -11 4 53.59 12.00 -3 11 -4 42.10 12.80 -3 11 -4 37.20 11.20 -3 11 -4 28.30 16.50 4 -11 4 63.79 15.40 4 -11 4 71.09 14.10 -4 11 -4 86.39 17.00 -4 11 -4 62.69 21.50 -4 11 -4 47.30 13.30 5 -11 4 118.29 23.40 -5 11 -4 133.49 22.80 -5 11 -4 154.98 24.20 6 -11 4 65.09 15.00 -6 11 -4 42.70 19.00 -6 11 -4 49.99 12.90 -6 11 -4 49.60 13.20 7 -11 4 27.70 11.60 -7 11 -4 46.60 13.20 -7 11 -4 46.80 12.00 -7 11 -4 57.19 21.90 -8 11 -4 37.00 18.00 9 -11 4 38.40 11.60 9 -11 4 35.90 15.20 -9 11 -4 46.60 20.50 -9 11 -4 41.10 12.30 10 -11 4 36.40 15.80 10 -11 4 44.60 11.90 -10 11 -4 34.50 12.30 -10 11 -4 50.39 24.10 11 -11 4 23.20 9.80 11 -11 4 24.40 14.60 -11 11 -4 16.80 18.40 -11 11 -4 14.60 11.80 12 -11 4 32.90 23.40 12 -11 4 25.70 11.80 -12 11 -4 21.80 20.80 -12 11 -4 34.50 12.80 13 -11 4 -14.50 7.80 13 -11 4 11.60 13.30 -13 11 -4 3.70 10.90 12 12 -4 -12.40 14.30 12 12 -4 21.90 17.30 11 12 -4 45.30 21.20 11 12 -4 31.20 18.40 10 12 -4 31.40 19.80 9 12 -4 14.90 15.50 8 12 -4 17.20 13.00 7 12 -4 -0.20 10.80 6 12 -4 -2.80 12.80 5 12 -4 317.27 53.89 -4 -12 4 808.52 87.89 4 12 -4 648.44 100.99 -3 -12 4 -0.80 3.70 3 12 -4 3.40 10.00 -2 -12 4 2.90 3.30 2 12 -4 4.10 10.50 2 12 -4 -2.10 9.70 -1 -12 4 46.00 9.30 1 12 -4 33.10 18.30 1 12 -4 34.10 13.20 0 -12 4 31.80 8.10 0 12 -4 20.50 14.20 0 12 -4 23.20 11.10 1 -12 4 188.28 25.80 1 -12 4 137.89 20.20 -1 12 -4 81.09 28.40 -1 12 -4 108.99 27.80 2 -12 4 258.17 34.20 2 -12 4 278.17 35.60 -2 12 -4 174.48 41.00 -2 12 -4 204.18 35.10 -3 12 -4 77.59 18.40 -3 12 -4 62.89 21.00 -3 12 -4 60.49 14.60 4 -12 4 64.09 15.10 -4 12 -4 41.90 18.10 -4 12 -4 50.99 13.90 -4 12 -4 50.99 12.50 5 -12 4 25.30 11.20 -5 12 -4 28.40 10.40 -5 12 -4 28.60 11.20 -5 12 -4 15.60 17.40 6 -12 4 22.70 10.70 -6 12 -4 28.90 9.90 -6 12 -4 29.30 9.90 -6 12 -4 16.80 12.40 7 -12 4 23.10 10.30 -7 12 -4 20.20 14.70 -7 12 -4 -2.30 6.30 -7 12 -4 8.60 8.30 8 -12 4 -7.70 6.80 -8 12 -4 -1.20 6.90 9 -12 4 48.30 12.80 -9 12 -4 38.90 14.30 -9 12 -4 72.29 25.30 10 -12 4 4.30 8.40 -10 12 -4 11.00 14.10 -10 12 -4 -1.40 8.50 11 -12 4 14.80 10.10 11 -12 4 13.30 11.00 -11 12 -4 13.90 20.60 -11 12 -4 8.10 9.90 12 -12 4 9.30 9.80 12 -12 4 -0.40 12.90 -12 12 -4 -17.20 20.10 -12 12 -4 -4.50 8.10 12 13 -4 20.60 19.80 12 13 -4 1.30 15.10 11 13 -4 1.40 14.50 10 13 -4 -0.90 12.00 8 13 -4 11.30 15.90 7 13 -4 594.34 86.69 6 13 -4 75.89 24.60 5 13 -4 28.70 15.90 -4 -13 4 105.79 13.80 4 13 -4 79.79 24.80 -3 -13 4 109.39 14.70 3 13 -4 60.99 22.50 -2 -13 4 77.19 12.30 2 13 -4 54.79 20.40 -1 -13 4 165.28 21.00 1 13 -4 92.69 31.00 0 -13 4 23.70 7.40 0 13 -4 18.90 15.80 0 13 -4 31.00 12.10 1 -13 4 137.49 27.00 1 -13 4 189.88 26.30 -1 13 -4 132.79 33.60 -1 13 -4 153.18 29.80 2 -13 4 147.09 21.50 2 -13 4 160.48 28.50 -2 13 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221.28 26.40 3 12 -7 172.18 39.90 -2 -12 7 34.80 7.20 2 12 -7 17.50 16.40 2 12 -7 17.60 11.10 -1 -12 7 295.67 35.40 1 12 -7 282.77 51.39 1 12 -7 237.58 40.00 0 -12 7 173.98 25.60 0 12 -7 292.67 47.10 0 12 -7 165.58 31.80 1 -12 7 35.70 8.70 -1 12 -7 32.00 18.70 -1 12 -7 22.10 8.80 -1 12 -7 45.00 12.20 2 -12 7 16.30 7.10 -2 12 -7 22.20 14.90 -2 12 -7 6.00 9.30 -2 12 -7 12.50 7.30 3 -12 7 2.70 7.40 -3 12 -7 2.70 14.10 -3 12 -7 10.50 6.40 -3 12 -7 3.10 6.50 -4 12 -7 16.30 8.10 -4 12 -7 21.70 7.50 -4 12 -7 5.50 13.70 5 -12 7 381.26 42.40 -5 12 -7 290.27 43.20 -5 12 -7 237.48 55.29 -5 12 -7 315.67 41.60 6 -12 7 14.60 7.70 -6 12 -7 31.10 16.80 -6 12 -7 16.90 8.50 -6 12 -7 12.60 7.00 7 -12 7 180.58 26.70 8 -12 7 68.49 13.20 -8 12 -7 53.59 15.80 -8 12 -7 48.70 23.60 9 -12 7 72.19 15.00 -9 12 -7 60.09 19.20 -9 12 -7 59.79 28.10 10 -12 7 8.80 7.30 -10 12 -7 -0.70 6.10 -10 12 -7 -7.30 26.20 11 -12 7 5.40 7.30 -11 12 -7 5.70 9.90 -11 12 -7 34.50 24.30 11 13 -7 -2.80 18.30 11 13 -7 -22.50 12.70 10 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5.7174 0.0011 2 -17 10 -0.6382 -0.0014 2 -17 11 -0.6584 0.0005 2 -16 0 0.1641 0.0032 2 -16 1 -1.6761 -0.0006 2 -16 2 3.5102 -0.0009 2 -16 3 -3.2202 0.0001 2 -16 4 -1.4825 0.0006 2 -16 5 2.1295 0.0002 2 -16 6 0.8693 0.0006 2 -16 7 -1.2049 -0.0014 2 -16 8 -1.0528 0.0004 2 -16 9 -2.6760 -0.0003 2 -16 10 -2.6711 0.0006 2 -16 11 -2.1525 -0.0003 2 -16 12 0.4266 -0.0007 2 -16 13 2.3282 -0.0009 2 -15 0 -1.1494 -0.0006 2 -15 1 0.7991 0.0018 2 -15 2 0.5497 -0.0005 2 -15 3 -3.6439 0.0009 2 -15 4 1.4986 0.0012 2 -15 5 -0.4393 0.0004 2 -15 6 -0.5154 -0.0003 2 -15 7 3.2968 0.0004 2 -15 8 -0.2244 -0.0002 2 -15 9 1.2693 0.0002 2 -15 10 -2.1557 0.0004 2 -15 11 -0.9118 0.0001 2 -15 12 1.1441 0.0006 2 -15 13 -0.6765 -0.0008 2 -15 14 -1.2747 -0.0009 2 -15 15 -1.1201 0.0002 2 -15 16 0.9716 -0.0013 2 -14 0 2.7507 -0.0029 2 -14 1 1.8654 -0.0024 2 -14 2 0.5239 0.0013 2 -14 3 0.1885 -0.0001 2 -14 4 -3.0189 -0.0003 2 -14 5 -1.9930 0.0010 2 -14 6 5.2457 0.0005 2 -14 7 4.0020 0.0000 2 -14 8 -3.5475 0.0013 2 -14 9 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12 8 8 -0.5842 -0.0004 12 8 9 1.7146 0.0003 12 8 10 3.4614 0.0002 12 8 11 -1.0884 -0.0023 12 8 12 0.4388 0.0004 12 8 13 1.1180 -0.0006 12 8 14 -0.6377 0.0011 12 9 0 -4.1632 0.0007 12 9 1 0.7223 0.0027 12 9 2 -2.2066 0.0000 12 9 3 -1.3029 0.0004 12 9 4 2.2487 0.0043 12 9 5 1.1821 0.0001 12 9 6 1.5690 0.0012 12 9 7 -2.4518 -0.0009 12 9 8 -3.7311 0.0016 12 9 9 -0.3923 -0.0036 12 9 10 1.8700 0.0006 12 9 11 0.5795 0.0047 12 9 12 -0.5070 -0.0002 12 10 0 1.3929 -0.0061 12 10 1 -0.9675 -0.0022 12 10 2 0.9127 -0.0037 12 10 3 0.4912 -0.0008 12 10 4 0.0881 -0.0009 12 10 5 -0.1758 -0.0027 12 10 6 1.2618 0.0035 12 10 7 2.0602 -0.0008 12 10 8 -3.4949 0.0016 12 10 9 -0.0220 -0.0011 12 10 10 3.1243 0.0026 12 10 11 0.3592 -0.0007 12 11 0 1.0386 0.0044 12 11 1 -3.5468 -0.0044 12 11 2 0.1550 -0.0014 12 11 3 0.8049 0.0007 12 11 4 -1.9030 -0.0012 12 11 5 1.5471 -0.0030 12 11 6 2.2391 0.0039 12 11 7 -1.5164 -0.0029 12 11 8 -3.7958 0.0046 12 11 9 -1.0067 -0.0006 12 12 0 3.6264 -0.0049 12 12 1 -1.1679 0.0051 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0.0010 14 4 1 5.1634 0.0061 14 4 2 3.2809 -0.0007 14 4 3 -1.9990 -0.0003 14 4 4 -3.5900 0.0016 14 4 5 -7.8495 -0.0018 14 4 6 -0.0012 0.0008 14 4 7 2.1108 -0.0016 14 4 8 2.0864 0.0012 14 4 9 -1.7945 -0.0021 14 4 10 0.3621 -0.0011 14 4 11 0.6972 -0.0003 14 4 12 -0.4475 -0.0022 14 5 0 -6.5103 -0.0032 14 5 1 -2.8086 0.0024 14 5 2 7.2391 -0.0043 14 5 3 5.9441 -0.0000 14 5 4 -1.9949 -0.0009 14 5 5 -6.1461 0.0020 14 5 6 2.1305 0.0005 14 5 7 0.6140 -0.0019 14 5 8 1.1020 0.0002 14 5 9 0.2747 -0.0022 14 5 10 -0.8374 0.0022 14 5 11 -0.6357 0.0011 14 6 0 -2.4509 0.0058 14 6 1 3.1069 -0.0033 14 6 2 0.5114 0.0035 14 6 3 3.5620 -0.0002 14 6 4 4.2728 -0.0002 14 6 5 -4.7130 0.0011 14 6 6 -3.7895 0.0009 14 6 7 -1.5640 -0.0004 14 6 8 4.5114 0.0003 14 6 9 1.0102 -0.0018 14 6 10 -2.7369 -0.0032 14 6 11 -2.3277 -0.0023 14 7 0 -3.1272 -0.0005 14 7 1 -4.0532 0.0009 14 7 2 -4.1640 0.0021 14 7 3 4.6361 -0.0001 14 7 4 5.6036 -0.0003 14 7 5 0.1212 -0.0015 14 7 6 -2.4368 0.0028 14 7 7 -3.9284 -0.0011 14 7 8 3.1489 0.0007 14 7 9 2.1799 0.0002 14 8 0 4.8725 0.0028 14 8 1 -2.5015 -0.0023 14 8 2 -2.8617 -0.0037 14 8 3 1.7880 0.0016 14 8 4 2.2964 -0.0030 14 8 5 0.1549 -0.0020 14 8 6 -1.4208 0.0057 14 8 7 -1.4623 -0.0005 14 8 8 0.1732 0.0011 14 9 0 0.8900 0.0045 14 9 1 -1.2386 -0.0028 14 9 2 -1.5880 0.0030 14 9 3 -3.1026 0.0023 14 9 4 1.4009 -0.0056 14 9 5 3.8206 0.0023 14 9 6 -0.4817 0.0005 14 10 0 3.3662 0.0046 14 10 1 0.8830 0.0012 14 10 2 0.3339 -0.0003 14 10 3 -1.6520 -0.0050 15 -8 0 0.2727 0.0022 15 -8 1 0.6628 0.0011 15 -8 2 -0.6318 -0.0037 15 -8 3 0.3479 -0.0007 15 -7 0 1.5626 0.0001 15 -7 1 -1.3032 0.0009 15 -7 2 0.5815 -0.0022 15 -7 3 3.2043 -0.0006 15 -7 4 -2.9129 0.0011 15 -7 5 1.4299 -0.0005 15 -6 0 -2.0586 0.0051 15 -6 1 -3.7677 0.0023 15 -6 2 0.2420 0.0020 15 -6 3 -0.5352 0.0013 15 -6 4 0.1357 0.0008 15 -6 5 3.7423 -0.0005 15 -6 6 -4.4581 0.0017 15 -6 7 -0.2384 0.0011 15 -5 0 3.3283 -0.0023 15 -5 1 -2.5503 0.0021 15 -5 2 -5.7909 -0.0010 15 -5 3 2.9956 -0.0007 15 -5 4 2.6433 -0.0012 15 -5 5 0.0384 0.0008 15 -5 6 0.8066 0.0000 15 -5 7 1.6457 -0.0002 15 -5 8 -4.3506 -0.0001 15 -4 0 -0.0135 0.0038 15 -4 1 -3.8290 -0.0015 15 -4 2 0.1450 -0.0008 15 -4 3 -0.2572 0.0007 15 -4 4 -0.3661 0.0003 15 -4 5 4.7112 -0.0002 15 -4 6 0.7291 0.0006 15 -4 7 -0.8878 0.0027 15 -4 8 2.1078 0.0000 15 -4 9 -0.0174 0.0028 15 -3 0 2.7677 -0.0013 15 -3 1 2.6738 -0.0064 15 -3 2 -5.4093 0.0019 15 -3 3 -2.3873 0.0018 15 -3 4 -1.0770 0.0005 15 -3 5 -0.0598 -0.0002 15 -3 6 0.9474 0.0005 15 -3 7 0.2290 -0.0019 15 -3 8 -0.7661 0.0005 15 -3 9 -1.1974 -0.0010 15 -3 10 0.3663 -0.0031 15 -2 0 2.2449 -0.0077 15 -2 1 -1.6356 0.0016 15 -2 2 0.1878 -0.0012 15 -2 3 1.6861 -0.0021 15 -2 4 -1.8495 -0.0007 15 -2 5 2.7612 0.0000 15 -2 6 -1.2754 0.0016 15 -2 7 -3.4286 0.0012 15 -2 8 1.6372 0.0007 15 -2 9 0.7775 -0.0003 15 -2 10 -1.1791 -0.0003 15 -1 0 -0.8363 0.0047 15 -1 1 5.2595 0.0004 15 -1 2 -1.3350 -0.0005 15 -1 3 -3.4030 -0.0006 15 -1 4 3.0413 -0.0005 15 -1 5 1.7679 0.0007 15 -1 6 -3.2739 -0.0013 15 -1 7 3.9670 0.0015 15 -1 8 0.5466 0.0018 15 -1 9 -3.4757 -0.0020 15 -1 10 0.4222 0.0013 15 0 0 2.1904 0.0020 15 0 1 3.1478 -0.0002 15 0 2 -3.3238 -0.0051 15 0 3 -0.8013 -0.0002 15 0 4 -3.9121 0.0025 15 0 5 -0.2674 0.0001 15 0 6 4.6768 -0.0013 15 0 7 -0.1416 0.0000 15 0 8 -2.1563 -0.0019 15 0 9 0.3603 -0.0001 15 0 10 -2.6103 0.0041 15 1 0 1.9460 -0.0048 15 1 1 4.7171 0.0003 15 1 2 2.1075 0.0005 15 1 3 -0.9036 -0.0006 15 1 4 -2.4622 0.0006 15 1 5 2.1252 0.0009 15 1 6 1.2190 0.0016 15 1 7 1.8859 0.0012 15 1 8 3.3684 -0.0022 15 1 9 -2.4700 -0.0019 15 1 10 -0.3902 -0.0011 15 2 0 1.4721 -0.0083 15 2 1 1.8446 -0.0021 15 2 2 -2.3916 -0.0019 15 2 3 -2.7987 0.0022 15 2 4 -1.9038 -0.0007 15 2 5 -3.9433 -0.0003 15 2 6 1.3081 0.0018 15 2 7 2.7079 -0.0015 15 2 8 -0.2069 0.0010 15 2 9 -0.2188 0.0008 15 2 10 1.3045 -0.0000 15 3 0 -3.5597 0.0018 15 3 1 4.8640 -0.0079 15 3 2 3.5783 -0.0023 15 3 3 -0.7794 0.0024 15 3 4 -1.1096 -0.0003 15 3 5 -1.2616 -0.0003 15 3 6 4.0736 0.0000 15 3 7 0.3840 -0.0012 15 3 8 0.2903 -0.0001 15 3 9 -0.8037 -0.0016 15 3 10 0.1645 0.0030 15 4 0 -0.5804 0.0046 15 4 1 4.9962 0.0025 15 4 2 1.8541 -0.0009 15 4 3 -1.5407 -0.0006 15 4 4 -3.5610 0.0001 15 4 5 -5.7463 -0.0038 15 4 6 0.6813 0.0010 15 4 7 0.6472 -0.0024 15 4 9 -1.5700 -0.0029 15 5 0 -5.1816 0.0025 15 5 1 1.0498 0.0034 15 5 2 5.2404 0.0016 15 5 3 5.4712 -0.0010 15 5 4 -2.0118 0.0009 15 5 5 -2.6002 0.0009 15 5 6 2.3093 0.0010 15 5 7 -0.5057 -0.0011 15 5 8 0.2560 0.0005 15 6 0 -2.3572 0.0065 15 6 1 1.1037 -0.0032 15 6 2 0.3835 0.0026 15 6 3 2.2141 -0.0020 15 6 4 0.9807 0.0014 15 6 5 -1.9094 0.0011 15 6 6 -1.7007 0.0022 15 6 7 0.2180 -0.0016 15 7 0 -2.5131 0.0005 15 7 1 -1.3717 0.0011 15 7 2 -1.9900 0.0029 15 7 3 1.2959 -0.0006 15 7 4 3.7975 -0.0018 15 7 5 1.0124 -0.0004 15 8 0 2.7490 0.0034 15 8 1 -2.5860 -0.0012 15 8 2 -1.8309 -0.0060 15 8 3 1.1550 0.0009 16 -5 0 1.9300 -0.0017 16 -5 1 -1.5266 0.0019 16 -5 2 -4.7558 -0.0037 16 -5 3 3.0272 -0.0008 16 -4 0 -1.8253 0.0049 16 -4 1 -2.7135 0.0018 16 -4 2 -0.4084 0.0005 16 -4 3 0.5796 0.0008 16 -4 4 1.4106 0.0004 16 -3 0 1.3725 -0.0006 16 -3 1 0.7861 -0.0075 16 -3 2 -4.4643 0.0003 16 -3 3 -1.3628 0.0015 16 -3 4 -1.7368 -0.0001 16 -3 5 -0.3241 -0.0003 16 -2 0 1.3573 -0.0023 16 -2 1 -0.9672 -0.0009 16 -2 2 1.0087 -0.0000 16 -2 3 1.6330 -0.0009 16 -2 4 -2.0722 -0.0009 16 -2 5 1.8924 0.0003 16 -2 6 -1.3364 0.0015 16 -1 0 0.1911 -0.0017 16 -1 2 -1.4610 0.0042 16 -1 3 -0.6594 -0.0017 16 -1 4 3.0990 -0.0021 16 -1 5 0.9219 -0.0008 16 -1 6 -3.5655 -0.0030 16 0 0 0.2787 0.0012 16 0 1 2.8638 0.0001 16 0 2 -1.9250 -0.0032 16 0 3 -0.6064 -0.0001 16 0 4 -1.2679 0.0026 16 0 5 0.8236 0.0000 16 0 6 1.2507 -0.0004 16 0 7 -0.2565 0.0001 16 1 0 0.4566 0.0020 16 1 1 3.2645 -0.0011 16 1 2 0.8302 -0.0044 16 1 3 0.4189 -0.0012 16 1 4 -1.6827 0.0024 16 1 5 0.2270 -0.0008 16 1 6 0.3198 0.0030 16 2 0 -0.1132 -0.0034 16 2 1 1.2102 0.0007 16 2 2 -1.6990 -0.0006 16 2 3 -1.5137 0.0010 16 2 4 -0.8858 -0.0011 16 2 5 -1.9606 -0.0007 16 2 6 0.5590 0.0023 16 3 0 -1.1616 0.0007 16 3 1 3.8140 -0.0090 16 3 2 1.0230 -0.0001 16 3 3 0.7374 0.0015 16 3 4 0.2296 0.0008 16 3 5 -1.1604 -0.0000 16 4 0 -1.8237 0.0060 16 4 1 2.9507 -0.0019 16 4 2 0.6219 0.0001 16 4 3 -0.3269 -0.0001 16 4 4 -1.8790 0.0002 16 5 0 -3.5774 0.0017 16 5 1 1.9605 0.0030 16 5 2 3.5112 0.0054 0 0 0 0.0 0.0 ; _shelx_fab_checksum 63023 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.59269(15) 0.71444(14) 0.41031(9) 0.0187(5) Uani 1 1 d . . . . . N2 N 0.62232(15) 0.64665(14) 0.32941(9) 0.0203(5) Uani 1 1 d . . . . . C1 C 0.42254(18) 0.76812(18) 0.38864(12) 0.0211(6) Uani 1 1 d . . . . . H1A H 0.3895 0.7883 0.3512 0.025 Uiso 1 1 calc R . . . . H1B H 0.4434 0.8195 0.4116 0.025 Uiso 1 1 calc R . . . . C2 C 0.50975(18) 0.72102(18) 0.37317(11) 0.0205(6) Uani 1 1 d . . . . . C3 C 0.52823(18) 0.67836(17) 0.32211(12) 0.0202(6) Uani 1 1 d . . . . . C4 C 0.65945(19) 0.66825(18) 0.38335(11) 0.0212(6) Uani 1 1 d . . . . . C5 C 0.75482(19) 0.64275(18) 0.40849(11) 0.0223(6) Uani 1 1 d . . . . . C6 C 0.81585(18) 0.69998(19) 0.43947(12) 0.0237(6) Uani 1 1 d . . . . . H6 H 0.7962 0.7574 0.4453 0.028 Uiso 1 1 calc R . . . . C7 C 0.9052(2) 0.6727(2) 0.46174(13) 0.0295(7) Uani 1 1 d . . . . . H7 H 0.9466 0.7116 0.4830 0.035 Uiso 1 1 calc R . . . . C8 C 0.9348(2) 0.5892(2) 0.45334(13) 0.0322(7) Uani 1 1 d . . . . . H8 H 0.9966 0.5713 0.4682 0.039 Uiso 1 1 calc R . . . . C9 C 0.8740(2) 0.5320(2) 0.42336(13) 0.0304(7) Uani 1 1 d . . . . . H9 H 0.8937 0.4744 0.4180 0.036 Uiso 1 1 calc R . . . . C10 C 0.7840(2) 0.55884(19) 0.40099(12) 0.0261(7) Uani 1 1 d . . . . . H10 H 0.7423 0.5194 0.3804 0.031 Uiso 1 1 calc R . . . . C11 C 0.7182(2) 0.9320(2) 0.39818(14) 0.0340(7) Uani 1 1 d . . . . . H11A H 0.7418 0.9685 0.4312 0.051 Uiso 1 1 calc GR . . . . H11B H 0.7159 0.9651 0.3612 0.051 Uiso 1 1 calc GR . . . . H11C H 0.7613 0.8831 0.3948 0.051 Uiso 1 1 calc GR . . . . C12 C 0.6170(2) 0.89981(18) 0.40972(12) 0.0257(7) Uani 1 1 d . . . . . H12 H 0.5950 0.8621 0.3758 0.031 Uiso 1 1 calc R . . . . C13 C 0.5473(2) 0.97492(19) 0.41154(13) 0.0308(7) Uani 1 1 d . . . . . H13A H 0.4839 0.9538 0.4209 0.046 Uiso 1 1 calc GR . . . . H13B H 0.5428 1.0034 0.3728 0.046 Uiso 1 1 calc GR . . . . H13C H 0.5706 1.0156 0.4421 0.046 Uiso 1 1 calc GR . . . . C14 C 0.61802(19) 0.84648(18) 0.46639(12) 0.0241(6) Uani 1 1 d . . . . . C15 C 0.6325(2) 0.8868(2) 0.52087(12) 0.0279(7) Uani 1 1 d . . . . . H15 H 0.6402 0.9472 0.5222 0.033 Uiso 1 1 calc R . . . . C16 C 0.6358(2) 0.8408(2) 0.57330(13) 0.0316(7) Uani 1 1 d . . . . . H16 H 0.6445 0.8698 0.6102 0.038 Uiso 1 1 calc R . . . . C17 C 0.6265(2) 0.7531(2) 0.57227(13) 0.0287(7) Uani 1 1 d . . . . . H17 H 0.6295 0.7225 0.6087 0.034 Uiso 1 1 calc R . . . . C18 C 0.61289(19) 0.70839(18) 0.51939(12) 0.0226(6) Uani 1 1 d . . . . . C19 C 0.60550(19) 0.61144(18) 0.52101(12) 0.0249(6) Uani 1 1 d . . . . . H19 H 0.5979 0.5902 0.4792 0.030 Uiso 1 1 calc R . . . . C20 C 0.5176(2) 0.5828(2) 0.55363(13) 0.0329(7) Uani 1 1 d . . . . . H20A H 0.5200 0.6085 0.5933 0.049 Uiso 1 1 calc GR . . . . H20B H 0.5177 0.5203 0.5572 0.049 Uiso 1 1 calc GR . . . . H20C H 0.4590 0.6012 0.5312 0.049 Uiso 1 1 calc GR . . . . C21 C 0.6955(2) 0.5711(2) 0.55041(13) 0.0329(7) Uani 1 1 d . . . . . H21A H 0.7517 0.5896 0.5297 0.049 Uiso 1 1 calc GR . . . . H21B H 0.6901 0.5086 0.5484 0.049 Uiso 1 1 calc GR . . . . H21C H 0.7027 0.5890 0.5920 0.049 Uiso 1 1 calc GR . . . . C22 C 0.60804(18) 0.75693(18) 0.46698(11) 0.0210(6) Uani 1 1 d . . . . . C23 C 0.46255(19) 0.66591(17) 0.26942(12) 0.0216(6) Uani 1 1 d . . . . . C24 C 0.4881(2) 0.67926(18) 0.21108(11) 0.0233(6) Uani 1 1 d . . . . . H24 H 0.5523 0.6941 0.2036 0.028 Uiso 1 1 calc R . . . . C25 C 0.4205(2) 0.67097(18) 0.16432(12) 0.0257(7) Uani 1 1 d . . . . . H25 H 0.4383 0.6799 0.1248 0.031 Uiso 1 1 calc R . . . . C26 C 0.3259(2) 0.64944(19) 0.17488(13) 0.0297(7) Uani 1 1 d . . . . . H26 H 0.2794 0.6443 0.1426 0.036 Uiso 1 1 calc R . . . . C27 C 0.3002(2) 0.63561(19) 0.23195(13) 0.0296(7) Uani 1 1 d . . . . . H27 H 0.2358 0.6210 0.2390 0.035 Uiso 1 1 calc R . . . . C28 C 0.3678(2) 0.64284(18) 0.27954(12) 0.0260(7) Uani 1 1 d . . . . . H28 H 0.3498 0.6322 0.3188 0.031 Uiso 1 1 calc R . . . . C29 C 0.4992(2) 0.4429(2) 0.25369(14) 0.0366(8) Uani 1 1 d . . . . . H29A H 0.4660 0.4950 0.2397 0.055 Uiso 1 1 calc GR . . . . H29B H 0.4555 0.4078 0.2758 0.055 Uiso 1 1 calc GR . . . . H29C H 0.5201 0.4105 0.2196 0.055 Uiso 1 1 calc GR . . . . C30 C 0.5862(2) 0.46701(19) 0.29402(12) 0.0267(7) Uani 1 1 d . . . . . H30 H 0.5633 0.4974 0.3295 0.032 Uiso 1 1 calc R . . . . C31 C 0.6390(2) 0.38528(19) 0.31538(13) 0.0342(8) Uani 1 1 d . . . . . H31A H 0.6531 0.3501 0.2810 0.051 Uiso 1 1 calc GR . . . . H31B H 0.5983 0.3529 0.3413 0.051 Uiso 1 1 calc GR . . . . H31C H 0.6990 0.4008 0.3374 0.051 Uiso 1 1 calc GR . . . . C32 C 0.6548(2) 0.52611(18) 0.26340(11) 0.0231(6) Uani 1 1 d . . . . . C33 C 0.7017(2) 0.4959(2) 0.21519(12) 0.0274(7) Uani 1 1 d . . . . . H33 H 0.6870 0.4402 0.2004 0.033 Uiso 1 1 calc R . . . . C34 C 0.7688(2) 0.5441(2) 0.18819(12) 0.0292(7) Uani 1 1 d . . . . . H34 H 0.8001 0.5216 0.1554 0.035 Uiso 1 1 calc R . . . . C35 C 0.7910(2) 0.6261(2) 0.20884(12) 0.0288(7) Uani 1 1 d . . . . . H35 H 0.8382 0.6587 0.1903 0.035 Uiso 1 1 calc R . . . . C36 C 0.67560(18) 0.60925(18) 0.28193(11) 0.0209(6) Uani 1 1 d . . . . . C37 C 0.74488(19) 0.66134(19) 0.25653(11) 0.0240(6) Uani 1 1 d . . . . . C38 C 0.7703(2) 0.7515(2) 0.27637(13) 0.0293(7) Uani 1 1 d . . . . . H38 H 0.7333 0.7646 0.3118 0.035 Uiso 1 1 calc R . . . . C39 C 0.8772(2) 0.7589(2) 0.29511(14) 0.0386(8) Uani 1 1 d . . . . . H39A H 0.8945 0.7151 0.3249 0.058 Uiso 1 1 calc GR . . . . H39B H 0.8904 0.8158 0.3120 0.058 Uiso 1 1 calc GR . . . . H39C H 0.9152 0.7506 0.2604 0.058 Uiso 1 1 calc GR . . . . C40 C 0.7420(2) 0.8172(2) 0.22827(14) 0.0356(8) Uani 1 1 d . . . . . H40A H 0.7804 0.8081 0.1939 0.053 Uiso 1 1 calc GR . . . . H40B H 0.7536 0.8750 0.2439 0.053 Uiso 1 1 calc GR . . . . H40C H 0.6738 0.8107 0.2162 0.053 Uiso 1 1 calc GR . . . . C41 C 0.33654(19) 0.75091(18) 0.49551(12) 0.0241(6) Uani 1 1 d . . . . . H41 H 0.4014 0.7436 0.5161 0.029 Uiso 1 1 calc R . . . . C42 C 0.26506(19) 0.6954(2) 0.52810(12) 0.0267(7) Uani 1 1 d . . . . . H42A H 0.2907 0.6365 0.5315 0.032 Uiso 1 1 calc R . . . . H42B H 0.2607 0.7181 0.5688 0.032 Uiso 1 1 calc R . . . . C43 C 0.2091(2) 0.8272(2) 0.39801(12) 0.0296(7) Uani 1 1 d . . . . . H43A H 0.1419 0.8343 0.3822 0.036 Uiso 1 1 calc R . . . . H43B H 0.2507 0.8564 0.3703 0.036 Uiso 1 1 calc R . . . . C44 C 0.23313(19) 0.73219(18) 0.39835(12) 0.0243(6) Uani 1 1 d . . . . . H44 H 0.2316 0.7125 0.3562 0.029 Uiso 1 1 calc R . . . . C45 C 0.1611(2) 0.6769(2) 0.43092(12) 0.0293(7) Uani 1 1 d . . . . . H45A H 0.0956 0.6891 0.4139 0.035 Uiso 1 1 calc R . . . . H45B H 0.1748 0.6159 0.4234 0.035 Uiso 1 1 calc R . . . . C46 C 0.1635(2) 0.6916(2) 0.49787(12) 0.0302(7) Uani 1 1 d . . . . . H46A H 0.1275 0.6448 0.5162 0.036 Uiso 1 1 calc R . . . . H46B H 0.1300 0.7459 0.5056 0.036 Uiso 1 1 calc R . . . . C47 C 0.2206(2) 0.8725(2) 0.45856(13) 0.0319(7) Uani 1 1 d . . . . . H47A H 0.1637 0.8597 0.4813 0.038 Uiso 1 1 calc R . . . . H47B H 0.2222 0.9351 0.4519 0.038 Uiso 1 1 calc R . . . . C48 C 0.3116(2) 0.84617(19) 0.49601(12) 0.0283(7) Uani 1 1 d . . . . . H48A H 0.3665 0.8786 0.4817 0.034 Uiso 1 1 calc R . . . . H48B H 0.3038 0.8637 0.5376 0.034 Uiso 1 1 calc R . . . . B1 B 0.3414(2) 0.7156(2) 0.42769(14) 0.0216(7) Uani 1 1 d . . . . . H1 H 0.3558 0.6530 0.4282 0.026 Uiso 1 1 calc R . . . . N3 N 0.40767(15) 0.21430(14) 0.08983(9) 0.0191(5) Uani 1 1 d . . . . . N4 N 0.37769(15) 0.14686(14) 0.17076(9) 0.0206(5) Uani 1 1 d . . . . . C49 C 0.57758(19) 0.26798(18) 0.11128(12) 0.0234(6) Uani 1 1 d . . . . . H49A H 0.6104 0.2883 0.1487 0.028 Uiso 1 1 calc R . . . . H49B H 0.5570 0.3193 0.0882 0.028 Uiso 1 1 calc R . . . . C50 C 0.49021(19) 0.22108(18) 0.12662(11) 0.0205(6) Uani 1 1 d . . . . . C51 C 0.47200(18) 0.17827(17) 0.17799(11) 0.0201(6) Uani 1 1 d . . . . . C52 C 0.34020(19) 0.16849(18) 0.11672(11) 0.0214(6) Uani 1 1 d . . . . . C53 C 0.4530(2) 0.47473(19) 0.08847(13) 0.0307(7) Uani 1 1 d . . . . . H53A H 0.5164 0.4537 0.0790 0.046 Uiso 1 1 calc GR . . . . H53B H 0.4577 0.5031 0.1272 0.046 Uiso 1 1 calc GR . . . . H53C H 0.4296 0.5155 0.0580 0.046 Uiso 1 1 calc GR . . . . C54 C 0.38308(19) 0.39927(18) 0.09034(12) 0.0250(6) Uani 1 1 d . . . . . H54 H 0.4050 0.3614 0.1242 0.030 Uiso 1 1 calc R . . . . C55 C 0.2816(2) 0.4325(2) 0.10208(14) 0.0325(7) Uani 1 1 d . . . . . H55A H 0.2586 0.4697 0.0693 0.049 Uiso 1 1 calc GR . . . . H55B H 0.2842 0.4648 0.1393 0.049 Uiso 1 1 calc GR . . . . H55C H 0.2378 0.3839 0.1050 0.049 Uiso 1 1 calc GR . . . . C56 C 0.38145(19) 0.34638(18) 0.03359(12) 0.0235(6) Uani 1 1 d . . . . . C57 C 0.3675(2) 0.38696(19) -0.02112(12) 0.0278(7) Uani 1 1 d . . . . . H57 H 0.3600 0.4473 -0.0224 0.033 Uiso 1 1 calc R . . . . C58 C 0.3644(2) 0.3416(2) -0.07311(13) 0.0335(7) Uani 1 1 d . . . . . H58 H 0.3558 0.3707 -0.1100 0.040 Uiso 1 1 calc R . . . . C59 C 0.3737(2) 0.25347(19) -0.07226(13) 0.0289(7) Uani 1 1 d . . . . . H59 H 0.3708 0.2230 -0.1088 0.035 Uiso 1 1 calc R . . . . C60 C 0.38719(19) 0.20817(19) -0.01921(12) 0.0239(6) Uani 1 1 d . . . . . C61 C 0.39223(18) 0.25692(18) 0.03280(11) 0.0197(6) Uani 1 1 d . . . . . C62 C 0.39500(19) 0.11119(18) -0.02099(12) 0.0240(6) Uani 1 1 d . . . . . H62 H 0.4025 0.0898 0.0208 0.029 Uiso 1 1 calc R . . . . C63 C 0.3038(2) 0.0713(2) -0.05058(13) 0.0323(7) Uani 1 1 d . . . . . H63A H 0.2480 0.0894 -0.0293 0.048 Uiso 1 1 calc GR . . . . H63B H 0.3090 0.0088 -0.0493 0.048 Uiso 1 1 calc GR . . . . H63C H 0.2960 0.0903 -0.0920 0.048 Uiso 1 1 calc GR . . . . C64 C 0.4824(2) 0.0822(2) -0.05365(13) 0.0318(7) Uani 1 1 d . . . . . H64A H 0.4799 0.1078 -0.0933 0.048 Uiso 1 1 calc GR . . . . H64B H 0.4820 0.0197 -0.0571 0.048 Uiso 1 1 calc GR . . . . H64C H 0.5411 0.1006 -0.0314 0.048 Uiso 1 1 calc GR . . . . C65 C 0.18379(19) 0.19977(19) 0.06055(12) 0.0239(6) Uani 1 1 d . . . . . H65 H 0.2032 0.2572 0.0547 0.029 Uiso 1 1 calc R . . . . C66 C 0.24519(19) 0.14276(18) 0.09155(11) 0.0214(6) Uani 1 1 d . . . . . C67 C 0.2161(2) 0.05878(19) 0.09892(12) 0.0259(7) Uani 1 1 d . . . . . H67 H 0.2581 0.0191 0.1190 0.031 Uiso 1 1 calc R . . . . C68 C 0.1257(2) 0.0324(2) 0.07698(13) 0.0309(7) Uani 1 1 d . . . . . H68 H 0.1056 -0.0248 0.0829 0.037 Uiso 1 1 calc R . . . . C69 C 0.0654(2) 0.0890(2) 0.04676(13) 0.0326(7) Uani 1 1 d . . . . . H69 H 0.0038 0.0709 0.0317 0.039 Uiso 1 1 calc R . . . . C70 C 0.0949(2) 0.1725(2) 0.03846(13) 0.0291(7) Uani 1 1 d . . . . . H70 H 0.0534 0.2114 0.0173 0.035 Uiso 1 1 calc R . . . . C71 C 0.3615(2) -0.11428(19) 0.18448(13) 0.0342(8) Uani 1 1 d . . . . . H71A H 0.3488 -0.1503 0.2187 0.051 Uiso 1 1 calc GR . . . . H71B H 0.4018 -0.1456 0.1578 0.051 Uiso 1 1 calc GR . . . . H71C H 0.3006 -0.0991 0.1632 0.051 Uiso 1 1 calc GR . . . . C72 C 0.4133(2) -0.03274(19) 0.20595(13) 0.0286(7) Uani 1 1 d . . . . . H72 H 0.4364 -0.0022 0.1706 0.034 Uiso 1 1 calc R . . . . C73 C 0.5005(2) -0.0575(2) 0.24625(14) 0.0367(8) Uani 1 1 d . . . . . H73A H 0.5341 -0.0056 0.2603 0.055 Uiso 1 1 calc GR . . . . H73B H 0.5439 -0.0928 0.2240 0.055 Uiso 1 1 calc GR . . . . H73C H 0.4795 -0.0899 0.2803 0.055 Uiso 1 1 calc GR . . . . C74 C 0.34581(19) 0.02615(18) 0.23653(12) 0.0230(6) Uani 1 1 d . . . . . C75 C 0.2978(2) -0.0045(2) 0.28478(12) 0.0298(7) Uani 1 1 d . . . . . H75 H 0.3116 -0.0605 0.2993 0.036 Uiso 1 1 calc R . . . . C76 C 0.2310(2) 0.0443(2) 0.31175(12) 0.0301(7) Uani 1 1 d . . . . . H76 H 0.2001 0.0222 0.3449 0.036 Uiso 1 1 calc R . . . . C77 C 0.2086(2) 0.1260(2) 0.29076(12) 0.0300(7) Uani 1 1 d . . . . . H77 H 0.1607 0.1584 0.3088 0.036 Uiso 1 1 calc R . . . . C78 C 0.25540(19) 0.16104(18) 0.24348(12) 0.0229(6) Uani 1 1 d . . . . . C79 C 0.32437(19) 0.10925(18) 0.21777(11) 0.0219(6) Uani 1 1 d . . . . . C80 C 0.2295(2) 0.25143(19) 0.22297(13) 0.0289(7) Uani 1 1 d . . . . . H80 H 0.2665 0.2645 0.1874 0.035 Uiso 1 1 calc R . . . . C81 C 0.2577(2) 0.3176(2) 0.27121(14) 0.0364(8) Uani 1 1 d . . . . . H81A H 0.2249 0.3043 0.3073 0.055 Uiso 1 1 calc GR . . . . H81B H 0.2389 0.3748 0.2572 0.055 Uiso 1 1 calc GR . . . . H81C H 0.3272 0.3159 0.2800 0.055 Uiso 1 1 calc GR . . . . C82 C 0.1223(2) 0.2589(2) 0.20453(14) 0.0370(8) Uani 1 1 d . . . . . H82A H 0.1043 0.2139 0.1758 0.056 Uiso 1 1 calc GR . . . . H82B H 0.1095 0.3151 0.1865 0.056 Uiso 1 1 calc GR . . . . H82C H 0.0848 0.2525 0.2396 0.056 Uiso 1 1 calc GR . . . . C83 C 0.53733(19) 0.16551(18) 0.23043(12) 0.0219(6) Uani 1 1 d . . . . . C84 C 0.63163(19) 0.14288(18) 0.22054(12) 0.0253(7) Uani 1 1 d . . . . . H84 H 0.6497 0.1326 0.1812 0.030 Uiso 1 1 calc R . . . . C85 C 0.6992(2) 0.13529(19) 0.26791(12) 0.0286(7) Uani 1 1 d . . . . . H85 H 0.7634 0.1203 0.2608 0.034 Uiso 1 1 calc R . . . . C86 C 0.6738(2) 0.14938(19) 0.32508(13) 0.0288(7) Uani 1 1 d . . . . . H86 H 0.7205 0.1443 0.3572 0.035 Uiso 1 1 calc R . . . . C87 C 0.5796(2) 0.17110(18) 0.33579(12) 0.0251(7) Uani 1 1 d . . . . . H87 H 0.5617 0.1803 0.3752 0.030 Uiso 1 1 calc R . . . . C88 C 0.5126(2) 0.17919(18) 0.28885(12) 0.0234(6) Uani 1 1 d . . . . . H88 H 0.4486 0.1943 0.2963 0.028 Uiso 1 1 calc R . . . . C89 C 0.66363(19) 0.25101(18) 0.00463(12) 0.0242(6) Uani 1 1 d . . . . . H89 H 0.5986 0.2438 -0.0158 0.029 Uiso 1 1 calc R . . . . C90 C 0.7348(2) 0.1956(2) -0.02840(12) 0.0295(7) Uani 1 1 d . . . . . H90A H 0.7392 0.2186 -0.0690 0.035 Uiso 1 1 calc R . . . . H90B H 0.7090 0.1367 -0.0321 0.035 Uiso 1 1 calc R . . . . C91 C 0.8367(2) 0.1916(2) 0.00207(13) 0.0318(7) Uani 1 1 d . . . . . H91B H 0.8726 0.1449 -0.0162 0.038 Uiso 1 1 calc R . . . . H91A H 0.8703 0.2459 -0.0056 0.038 Uiso 1 1 calc R . . . . C92 C 0.8387(2) 0.1769(2) 0.06938(12) 0.0300(7) Uani 1 1 d . . . . . H92A H 0.9043 0.1889 0.0864 0.036 Uiso 1 1 calc R . . . . H92B H 0.8249 0.1159 0.0768 0.036 Uiso 1 1 calc R . . . . C93 C 0.76732(19) 0.23175(19) 0.10218(12) 0.0244(6) Uani 1 1 d . . . . . H93 H 0.7690 0.2120 0.1444 0.029 Uiso 1 1 calc R . . . . C94 C 0.7909(2) 0.3277(2) 0.10226(12) 0.0291(7) Uani 1 1 d . . . . . H94A H 0.8581 0.3352 0.1179 0.035 Uiso 1 1 calc R . . . . H94B H 0.7493 0.3568 0.1300 0.035 Uiso 1 1 calc R . . . . C95 C 0.7789(2) 0.3727(2) 0.04165(14) 0.0338(7) Uani 1 1 d . . . . . H95A H 0.7775 0.4352 0.0483 0.041 Uiso 1 1 calc R . . . . H95B H 0.8357 0.3598 0.0189 0.041 Uiso 1 1 calc R . . . . C96 C 0.6887(2) 0.34697(19) 0.00422(13) 0.0289(7) Uani 1 1 d . . . . . H96A H 0.6967 0.3646 -0.0373 0.035 Uiso 1 1 calc R . . . . H96B H 0.6337 0.3794 0.0185 0.035 Uiso 1 1 calc R . . . . B2 B 0.6586(2) 0.2157(2) 0.07279(14) 0.0224(7) Uani 1 1 d . . . . . H2 H 0.6439 0.1531 0.0723 0.027 Uiso 1 1 calc R . . . . 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 N1 0.0149(11) 0.0212(13) 0.0199(11) 0.0010(10) -0.0007(9) -0.0081(9) N2 0.0205(12) 0.0202(13) 0.0203(11) 0.0029(10) 0.0014(10) -0.0077(10) C1 0.0211(14) 0.0212(16) 0.0208(13) 0.0024(12) 0.0008(11) -0.0062(12) C2 0.0160(13) 0.0225(16) 0.0225(14) 0.0050(12) -0.0022(11) -0.0098(11) C3 0.0156(13) 0.0198(15) 0.0251(14) 0.0064(12) 0.0001(11) -0.0066(11) C4 0.0227(14) 0.0176(15) 0.0230(14) 0.0025(12) -0.0002(12) -0.0118(12) C5 0.0202(14) 0.0265(17) 0.0203(14) 0.0040(12) 0.0028(12) -0.0084(12) C6 0.0179(14) 0.0236(16) 0.0293(15) 0.0038(12) 0.0003(12) -0.0087(12) C7 0.0221(15) 0.0319(19) 0.0338(16) 0.0029(14) -0.0023(13) -0.0139(13) C8 0.0198(15) 0.037(2) 0.0397(18) 0.0127(15) 0.0018(13) -0.0080(14) C9 0.0300(16) 0.0260(18) 0.0356(17) 0.0067(14) 0.0054(14) -0.0002(14) C10 0.0219(15) 0.0261(18) 0.0299(15) 0.0025(13) -0.0010(13) -0.0082(13) C11 0.0284(16) 0.0309(19) 0.0433(18) 0.0038(15) 0.0075(14) -0.0111(14) C12 0.0268(15) 0.0229(16) 0.0274(15) 0.0034(12) 0.0015(12) -0.0107(13) C13 0.0307(16) 0.0251(17) 0.0365(17) 0.0045(14) 0.0008(14) -0.0109(13) C14 0.0175(14) 0.0218(16) 0.0327(16) 0.0024(13) 0.0002(12) -0.0078(12) C15 0.0268(16) 0.0245(17) 0.0321(16) -0.0039(13) -0.0010(13) -0.0058(13) C16 0.0330(17) 0.0336(19) 0.0271(16) -0.0057(14) -0.0071(14) -0.0052(14) C17 0.0293(16) 0.0314(19) 0.0250(15) 0.0054(13) -0.0022(13) -0.0071(14) C18 0.0188(14) 0.0261(17) 0.0228(14) 0.0017(12) -0.0004(12) -0.0055(12) C19 0.0250(15) 0.0257(17) 0.0235(14) 0.0052(12) -0.0015(12) -0.0087(13) C20 0.0309(17) 0.0330(19) 0.0352(17) 0.0072(14) 0.0062(14) -0.0123(14) C21 0.0309(17) 0.0320(19) 0.0354(17) 0.0099(14) -0.0004(14) -0.0047(14) C22 0.0180(14) 0.0240(16) 0.0207(14) -0.0014(12) 0.0002(11) -0.0094(12) C23 0.0232(14) 0.0188(15) 0.0225(14) 0.0011(12) -0.0016(12) -0.0091(12) C24 0.0247(15) 0.0203(16) 0.0248(14) 0.0006(12) 0.0002(12) -0.0055(12) C25 0.0330(16) 0.0212(16) 0.0227(14) -0.0003(12) -0.0004(13) -0.0032(13) C26 0.0326(17) 0.0259(17) 0.0289(16) -0.0022(13) -0.0114(14) -0.0036(14) C27 0.0225(15) 0.0294(18) 0.0363(17) -0.0012(14) -0.0024(13) -0.0101(13) C28 0.0289(16) 0.0239(17) 0.0251(15) 0.0023(12) 0.0016(13) -0.0089(13) C29 0.0318(17) 0.034(2) 0.0437(19) -0.0003(15) -0.0008(15) -0.0138(15) C30 0.0304(16) 0.0233(17) 0.0267(15) -0.0006(13) 0.0030(13) -0.0109(13) C31 0.0445(19) 0.0248(18) 0.0336(17) 0.0047(14) 0.0054(15) -0.0087(15) C32 0.0278(15) 0.0221(16) 0.0188(13) 0.0028(12) -0.0043(12) -0.0039(12) C33 0.0318(16) 0.0265(17) 0.0237(14) -0.0007(13) 0.0004(13) -0.0051(13) C34 0.0313(16) 0.0364(19) 0.0200(14) 0.0020(13) 0.0028(13) 0.0026(14) C35 0.0230(15) 0.0357(19) 0.0276(15) 0.0068(14) 0.0018(13) -0.0049(14) C36 0.0195(14) 0.0268(17) 0.0162(13) 0.0010(12) -0.0013(11) -0.0032(12) C37 0.0202(14) 0.0321(18) 0.0193(14) 0.0060(12) -0.0022(12) -0.0064(13) C38 0.0267(16) 0.0319(18) 0.0292(16) 0.0044(13) 0.0012(13) -0.0135(13) C39 0.0295(17) 0.046(2) 0.0406(18) 0.0058(16) 0.0025(15) -0.0201(15) C40 0.0365(18) 0.0290(18) 0.0414(18) 0.0047(15) 0.0028(15) -0.0127(15) C41 0.0180(14) 0.0284(17) 0.0255(15) 0.0057(13) -0.0015(12) -0.0080(12) C42 0.0247(15) 0.0335(18) 0.0219(14) 0.0066(13) 0.0003(12) -0.0074(13) C43 0.0220(15) 0.0378(19) 0.0292(16) 0.0107(14) 0.0037(13) -0.0040(14) C44 0.0195(14) 0.0311(18) 0.0223(14) 0.0017(12) 0.0019(12) -0.0134(13) C45 0.0181(14) 0.0362(19) 0.0329(16) 0.0068(14) -0.0035(13) -0.0129(13) C46 0.0210(15) 0.0393(19) 0.0302(16) 0.0128(14) 0.0003(13) -0.0121(13) C47 0.0304(16) 0.0260(18) 0.0397(17) 0.0062(14) 0.0064(14) -0.0057(14) C48 0.0298(16) 0.0297(18) 0.0260(15) -0.0014(13) 0.0059(13) -0.0117(13) B1 0.0169(15) 0.0189(18) 0.0286(17) 0.0033(14) -0.0011(13) -0.0067(13) N3 0.0163(11) 0.0213(13) 0.0195(11) 0.0035(10) 0.0002(9) -0.0065(10) N4 0.0182(11) 0.0222(13) 0.0213(12) 0.0045(10) 0.0010(10) -0.0106(10) C49 0.0208(14) 0.0259(17) 0.0233(14) 0.0046(12) 0.0010(12) -0.0119(12) C50 0.0190(14) 0.0237(16) 0.0186(13) 0.0003(11) -0.0005(11) -0.0048(12) C51 0.0151(13) 0.0209(16) 0.0244(14) -0.0001(12) 0.0024(11) -0.0084(11) C52 0.0192(14) 0.0240(16) 0.0208(14) 0.0014(12) 0.0001(11) -0.0081(12) C53 0.0305(16) 0.0234(17) 0.0377(17) 0.0001(14) -0.0026(14) -0.0082(13) C54 0.0236(15) 0.0236(17) 0.0276(15) 0.0048(12) -0.0006(12) -0.0044(12) C55 0.0315(17) 0.0265(18) 0.0403(18) 0.0017(14) 0.0097(14) -0.0069(14) C56 0.0175(14) 0.0229(16) 0.0298(15) 0.0040(12) 0.0000(12) -0.0064(12) C57 0.0288(16) 0.0248(17) 0.0293(16) 0.0104(13) -0.0016(13) -0.0076(13) C58 0.0335(17) 0.038(2) 0.0285(16) 0.0133(14) -0.0013(14) -0.0063(15) C59 0.0327(17) 0.0304(19) 0.0231(15) 0.0009(13) -0.0022(13) -0.0073(14) C60 0.0187(14) 0.0294(17) 0.0234(14) 0.0024(13) -0.0005(12) -0.0099(12) C61 0.0149(13) 0.0240(16) 0.0201(13) 0.0059(12) -0.0004(11) -0.0089(12) C62 0.0257(15) 0.0253(17) 0.0208(14) 0.0000(12) -0.0008(12) -0.0054(13) C63 0.0312(17) 0.0296(18) 0.0358(17) -0.0021(14) -0.0006(14) -0.0126(14) C64 0.0310(17) 0.0303(18) 0.0344(17) 0.0001(14) 0.0034(14) -0.0039(14) C65 0.0196(14) 0.0243(17) 0.0277(15) 0.0032(13) 0.0002(12) -0.0085(12) C66 0.0190(14) 0.0260(17) 0.0192(13) 0.0017(12) 0.0022(11) -0.0100(12) C67 0.0245(15) 0.0253(17) 0.0280(15) 0.0024(13) 0.0026(12) -0.0088(13) C68 0.0283(16) 0.0302(18) 0.0340(16) -0.0014(14) 0.0010(14) -0.0154(14) C69 0.0209(15) 0.0356(19) 0.0411(18) -0.0101(15) -0.0006(14) -0.0100(14) C70 0.0214(15) 0.0284(18) 0.0368(17) 0.0004(14) -0.0035(13) -0.0047(13) C71 0.0452(19) 0.0238(18) 0.0336(17) 0.0046(14) 0.0026(15) -0.0079(15) C72 0.0317(16) 0.0266(18) 0.0278(15) 0.0054(13) 0.0049(13) -0.0049(13) C73 0.0315(17) 0.0323(19) 0.0457(19) 0.0074(15) -0.0019(15) -0.0027(15) C74 0.0244(15) 0.0216(16) 0.0227(14) 0.0027(12) -0.0010(12) -0.0091(12) C75 0.0324(17) 0.0306(18) 0.0262(15) 0.0061(13) -0.0002(13) -0.0167(14) C76 0.0304(16) 0.0368(19) 0.0234(15) 0.0039(14) 0.0031(13) -0.0189(14) C77 0.0245(15) 0.0361(19) 0.0296(16) 0.0013(14) 0.0045(13) -0.0106(14) C78 0.0195(14) 0.0260(17) 0.0229(14) -0.0006(12) -0.0014(12) -0.0107(12) C79 0.0204(14) 0.0277(17) 0.0176(13) 0.0030(12) -0.0002(11) -0.0122(12) C80 0.0287(16) 0.0299(18) 0.0284(16) 0.0061(13) 0.0033(13) -0.0030(13) C81 0.0377(18) 0.0289(19) 0.0428(19) 0.0039(15) 0.0053(15) -0.0052(15) C82 0.0300(17) 0.043(2) 0.0374(18) 0.0055(15) -0.0005(14) -0.0006(15) C83 0.0201(14) 0.0225(16) 0.0227(14) 0.0058(12) -0.0020(12) -0.0095(12) C84 0.0261(15) 0.0258(17) 0.0242(14) 0.0044(12) 0.0011(12) -0.0090(13) C85 0.0198(14) 0.0334(18) 0.0321(16) 0.0073(14) -0.0034(13) -0.0073(13) C86 0.0308(16) 0.0281(18) 0.0263(15) 0.0077(13) -0.0087(13) -0.0126(14) C87 0.0317(16) 0.0214(16) 0.0219(14) 0.0079(12) -0.0015(13) -0.0138(13) C88 0.0210(14) 0.0229(16) 0.0263(15) 0.0038(12) 0.0019(12) -0.0105(12) C89 0.0197(14) 0.0261(17) 0.0269(15) 0.0014(13) 0.0010(12) -0.0093(12) C90 0.0285(16) 0.0338(19) 0.0261(15) 0.0003(13) 0.0018(13) -0.0079(14) C91 0.0231(15) 0.041(2) 0.0316(16) -0.0030(14) 0.0031(13) -0.0063(14) C92 0.0213(15) 0.0347(19) 0.0337(16) 0.0008(14) -0.0023(13) -0.0058(13) C93 0.0218(14) 0.0286(17) 0.0227(14) 0.0033(12) 0.0005(12) -0.0083(12) C94 0.0196(15) 0.0375(19) 0.0302(16) -0.0028(14) 0.0014(13) -0.0113(13) C95 0.0293(17) 0.0281(18) 0.0446(19) 0.0004(15) 0.0073(14) -0.0125(14) C96 0.0278(16) 0.0297(18) 0.0301(16) 0.0066(13) 0.0085(13) -0.0065(13) B2 0.0226(16) 0.0180(18) 0.0263(17) 0.0033(14) -0.0014(14) -0.0085(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 N1 C22 124.9(2) . . ? C4 N1 C2 109.9(2) . . ? C4 N1 C22 125.0(2) . . ? C3 N2 C36 124.6(2) . . ? C4 N2 C3 109.1(2) . . ? C4 N2 C36 125.5(2) . . ? H1A C1 H1B 107.2 . . ? C2 C1 H1A 107.8 . . ? C2 C1 H1B 107.8 . . ? C2 C1 B1 117.9(2) . . ? B1 C1 H1A 107.8 . . ? B1 C1 H1B 107.8 . . ? N1 C2 C1 124.1(2) . . ? C3 C2 N1 106.2(2) . . ? C3 C2 C1 129.7(2) . . ? N2 C3 C23 125.6(2) . . ? C2 C3 N2 107.1(2) . . ? C2 C3 C23 127.2(2) . . ? N1 C4 C5 127.1(2) . . ? N2 C4 N1 107.7(2) . . ? N2 C4 C5 125.1(3) . . ? C6 C5 C4 122.1(3) . . ? C10 C5 C4 118.4(2) . . ? C10 C5 C6 119.5(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 C5 119.7(3) . . ? C7 C6 H6 120.2 . . ? C6 C7 H7 119.7 . . ? C6 C7 C8 120.7(3) . . ? C8 C7 H7 119.7 . . ? C7 C8 H8 120.1 . . ? C9 C8 C7 119.8(3) . . ? C9 C8 H8 120.1 . . ? C8 C9 H9 120.1 . . ? C8 C9 C10 119.8(3) . . ? C10 C9 H9 120.1 . . ? C5 C10 C9 120.5(3) . . ? C5 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? C11 C12 H12 107.9 . . ? C13 C12 C11 110.3(2) . . ? C13 C12 H12 107.9 . . ? C14 C12 C11 111.0(2) . . ? C14 C12 H12 107.9 . . ? C14 C12 C13 111.8(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C12 119.2(3) . . ? C15 C14 C22 117.0(3) . . ? C22 C14 C12 123.8(2) . . ? C14 C15 H15 119.4 . . ? C16 C15 C14 121.2(3) . . ? C16 C15 H15 119.4 . . ? C15 C16 H16 119.8 . . ? C17 C16 C15 120.3(3) . . ? C17 C16 H16 119.8 . . ? C16 C17 H17 119.2 . . ? C16 C17 C18 121.6(3) . . ? C18 C17 H17 119.2 . . ? C17 C18 C19 119.2(2) . . ? C17 C18 C22 116.8(3) . . ? C22 C18 C19 124.0(2) . . ? C18 C19 H19 108.2 . . ? C18 C19 C20 111.1(2) . . ? C18 C19 C21 111.6(2) . . ? C20 C19 H19 108.2 . . ? C21 C19 H19 108.2 . . ? C21 C19 C20 109.4(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 N1 117.3(2) . . ? C18 C22 N1 119.6(2) . . ? C18 C22 C14 123.1(2) . . ? C24 C23 C3 124.0(2) . . ? C24 C23 C28 119.1(2) . . ? C28 C23 C3 116.8(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 C23 120.3(3) . . ? C25 C24 H24 119.9 . . ? C24 C25 H25 119.9 . . ? C24 C25 C26 120.2(3) . . ? C26 C25 H25 119.9 . . ? C25 C26 H26 120.0 . . ? C27 C26 C25 120.0(3) . . ? C27 C26 H26 120.0 . . ? C26 C27 H27 119.8 . . ? C26 C27 C28 120.5(3) . . ? C28 C27 H27 119.8 . . ? C23 C28 H28 120.1 . . ? C27 C28 C23 119.9(3) . . ? C27 C28 H28 120.1 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? C29 C30 H30 108.3 . . ? C29 C30 C31 109.4(3) . . ? C29 C30 C32 112.3(2) . . ? C31 C30 H30 108.3 . . ? C32 C30 H30 108.3 . . ? C32 C30 C31 110.1(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C30 119.2(3) . . ? C33 C32 C36 117.1(3) . . ? C36 C32 C30 123.7(2) . . ? C32 C33 H33 119.1 . . ? C34 C33 C32 121.8(3) . . ? C34 C33 H33 119.1 . . ? C33 C34 H34 120.0 . . ? C33 C34 C35 120.1(3) . . ? C35 C34 H34 120.0 . . ? C34 C35 H35 119.5 . . ? C34 C35 C37 121.1(3) . . ? C37 C35 H35 119.5 . . ? C32 C36 N2 119.2(2) . . ? C32 C36 C37 123.6(3) . . ? C37 C36 N2 117.2(2) . . ? C35 C37 C36 116.3(3) . . ? C35 C37 C38 118.9(3) . . ? C36 C37 C38 124.8(2) . . ? C37 C38 H38 107.8 . . ? C37 C38 C39 111.1(3) . . ? C37 C38 C40 111.7(2) . . ? C39 C38 H38 107.8 . . ? C40 C38 H38 107.8 . . ? C40 C38 C39 110.6(2) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41 108.0 . . ? C42 C41 B1 108.7(2) . . ? C48 C41 H41 108.0 . . ? C48 C41 C42 112.9(2) . . ? C48 C41 B1 111.0(2) . . ? B1 C41 H41 108.0 . . ? C41 C42 H42A 108.6 . . ? C41 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C46 C42 C41 114.6(2) . . ? C46 C42 H42A 108.6 . . ? C46 C42 H42B 108.6 . . ? H43A C43 H43B 107.4 . . ? C44 C43 H43A 108.4 . . ? C44 C43 H43B 108.4 . . ? C44 C43 C47 115.7(2) . . ? C47 C43 H43A 108.4 . . ? C47 C43 H43B 108.4 . . ? C43 C44 H44 107.7 . . ? C43 C44 C45 113.5(2) . . ? C43 C44 B1 110.8(2) . . ? C45 C44 H44 107.7 . . ? C45 C44 B1 109.3(2) . . ? B1 C44 H44 107.7 . . ? C44 C45 H45A 108.7 . . ? C44 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? C46 C45 C44 114.3(2) . . ? C46 C45 H45A 108.7 . . ? C46 C45 H45B 108.7 . . ? C42 C46 H46A 108.7 . . ? C42 C46 H46B 108.7 . . ? C45 C46 C42 114.2(2) . . ? C45 C46 H46A 108.7 . . ? C45 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? C43 C47 H47A 108.8 . . ? C43 C47 H47B 108.8 . . ? C43 C47 C48 113.8(2) . . ? H47A C47 H47B 107.7 . . ? C48 C47 H47A 108.8 . . ? C48 C47 H47B 108.8 . . ? C41 C48 C47 116.0(2) . . ? C41 C48 H48A 108.3 . . ? C41 C48 H48B 108.3 . . ? C47 C48 H48A 108.3 . . ? C47 C48 H48B 108.3 . . ? H48A C48 H48B 107.4 . . ? C1 B1 H1 109.9 . . ? C41 B1 C1 113.1(2) . . ? C41 B1 C44 103.7(2) . . ? C41 B1 H1 109.9 . . ? C44 B1 C1 110.1(2) . . ? C44 B1 H1 109.9 . . ? C50 N3 C61 124.8(2) . . ? C52 N3 C50 110.4(2) . . ? C52 N3 C61 124.6(2) . . ? C51 N4 C79 124.9(2) . . ? C52 N4 C51 109.3(2) . . ? C52 N4 C79 125.1(2) . . ? H49A C49 H49B 107.1 . . ? C50 C49 H49A 107.8 . . ? C50 C49 H49B 107.8 . . ? C50 C49 B2 118.0(2) . . ? B2 C49 H49A 107.8 . . ? B2 C49 H49B 107.8 . . ? N3 C50 C49 124.4(2) . . ? C51 C50 N3 106.2(2) . . ? C51 C50 C49 129.3(2) . . ? N4 C51 C83 125.5(2) . . ? C50 C51 N4 106.9(2) . . ? C50 C51 C83 127.6(2) . . ? N3 C52 C66 127.4(2) . . ? N4 C52 N3 107.2(2) . . ? N4 C52 C66 125.3(2) . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C54 C53 H53A 109.5 . . ? C54 C53 H53B 109.5 . . ? C54 C53 H53C 109.5 . . ? C53 C54 H54 108.0 . . ? C53 C54 C55 109.8(2) . . ? C55 C54 H54 108.0 . . ? C56 C54 C53 111.8(2) . . ? C56 C54 H54 108.0 . . ? C56 C54 C55 111.0(2) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 C54 119.5(3) . . ? C57 C56 C61 116.8(3) . . ? C61 C56 C54 123.6(2) . . ? C56 C57 H57 119.3 . . ? C58 C57 C56 121.3(3) . . ? C58 C57 H57 119.3 . . ? C57 C58 H58 119.8 . . ? C57 C58 C59 120.4(3) . . ? C59 C58 H58 119.8 . . ? C58 C59 H59 119.1 . . ? C58 C59 C60 121.7(3) . . ? C60 C59 H59 119.1 . . ? C59 C60 C61 116.2(3) . . ? C59 C60 C62 119.3(2) . . ? C61 C60 C62 124.4(2) . . ? C56 C61 N3 117.1(2) . . ? C60 C61 N3 119.4(2) . . ? C60 C61 C56 123.5(2) . . ? C60 C62 H62 108.2 . . ? C60 C62 C63 110.9(2) . . ? C60 C62 C64 111.6(2) . . ? C63 C62 H62 108.2 . . ? C64 C62 H62 108.2 . . ? C64 C62 C63 109.6(2) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63B 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64B 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 H65 120.1 . . ? C70 C65 H65 120.1 . . ? C70 C65 C66 119.8(3) . . ? C65 C66 C52 122.2(3) . . ? C67 C66 C52 118.5(2) . . ? C67 C66 C65 119.3(2) . . ? C66 C67 H67 119.9 . . ? C66 C67 C68 120.2(3) . . ? C68 C67 H67 119.9 . . ? C67 C68 H68 119.9 . . ? C69 C68 C67 120.2(3) . . ? C69 C68 H68 119.9 . . ? C68 C69 H69 120.2 . . ? C68 C69 C70 119.7(3) . . ? C70 C69 H69 120.2 . . ? C65 C70 C69 120.8(3) . . ? C65 C70 H70 119.6 . . ? C69 C70 H70 119.6 . . ? H71A C71 H71B 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? C71 C72 H72 108.3 . . ? C73 C72 C71 108.9(2) . . ? C73 C72 H72 108.3 . . ? C74 C72 C71 110.8(2) . . ? C74 C72 H72 108.3 . . ? C74 C72 C73 112.3(2) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73B 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C75 C74 C72 119.2(3) . . ? C79 C74 C72 123.9(2) . . ? C79 C74 C75 116.9(3) . . ? C74 C75 H75 119.2 . . ? C76 C75 C74 121.6(3) . . ? C76 C75 H75 119.2 . . ? C75 C76 H76 119.9 . . ? C75 C76 C77 120.3(3) . . ? C77 C76 H76 119.9 . . ? C76 C77 H77 119.5 . . ? C76 C77 C78 120.9(3) . . ? C78 C77 H77 119.5 . . ? C77 C78 C79 116.9(3) . . ? C77 C78 C80 118.9(3) . . ? C79 C78 C80 124.3(2) . . ? C74 C79 N4 119.2(2) . . ? C74 C79 C78 123.4(2) . . ? C78 C79 N4 117.4(2) . . ? C78 C80 H80 108.0 . . ? C78 C80 C81 111.3(2) . . ? C78 C80 C82 111.3(2) . . ? C81 C80 H80 108.0 . . ? C82 C80 H80 108.0 . . ? C82 C80 C81 110.2(3) . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81B 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80 C82 H82A 109.5 . . ? C80 C82 H82B 109.5 . . ? C80 C82 H82C 109.5 . . ? H82A C82 H82B 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 C83 C51 117.0(2) . . ? C84 C83 C88 118.5(2) . . ? C88 C83 C51 124.3(2) . . ? C83 C84 H84 119.9 . . ? C85 C84 C83 120.2(3) . . ? C85 C84 H84 119.9 . . ? C84 C85 H85 119.7 . . ? C86 C85 C84 120.5(3) . . ? C86 C85 H85 119.7 . . ? C85 C86 H86 120.0 . . ? C85 C86 C87 120.0(3) . . ? C87 C86 H86 120.0 . . ? C86 C87 H87 120.2 . . ? C88 C87 C86 119.6(3) . . ? C88 C87 H87 120.2 . . ? C83 C88 H88 119.4 . . ? C87 C88 C83 121.1(3) . . ? C87 C88 H88 119.4 . . ? C90 C89 H89 107.9 . . ? C90 C89 B2 109.2(2) . . ? C96 C89 H89 107.9 . . ? C96 C89 C90 113.0(2) . . ? C96 C89 B2 110.8(2) . . ? B2 C89 H89 107.9 . . ? C89 C90 H90A 108.7 . . ? C89 C90 H90B 108.7 . . ? C89 C90 C91 114.2(2) . . ? H90A C90 H90B 107.6 . . ? C91 C90 H90A 108.7 . . ? C91 C90 H90B 108.7 . . ? C90 C91 H91B 108.7 . . ? C90 C91 H91A 108.7 . . ? H91B C91 H91A 107.6 . . ? C92 C91 C90 114.2(2) . . ? C92 C91 H91B 108.7 . . ? C92 C91 H91A 108.7 . . ? C91 C92 H92A 108.6 . . ? C91 C92 H92B 108.6 . . ? C91 C92 C93 114.7(2) . . ? H92A C92 H92B 107.6 . . ? C93 C92 H92A 108.6 . . ? C93 C92 H92B 108.6 . . ? C92 C93 H93 107.9 . . ? C92 C93 B2 109.4(2) . . ? C94 C93 C92 113.6(2) . . ? C94 C93 H93 107.9 . . ? C94 C93 B2 110.0(2) . . ? B2 C93 H93 107.9 . . ? C93 C94 H94A 108.4 . . ? C93 C94 H94B 108.4 . . ? C93 C94 C95 115.7(2) . . ? H94A C94 H94B 107.4 . . ? C95 C94 H94A 108.4 . . ? C95 C94 H94B 108.4 . . ? C94 C95 H95A 108.6 . . ? C94 C95 H95B 108.6 . . ? H95A C95 H95B 107.6 . . ? C96 C95 C94 114.5(2) . . ? C96 C95 H95A 108.6 . . ? C96 C95 H95B 108.6 . . ? C89 C96 H96A 108.4 . . ? C89 C96 H96B 108.4 . . ? C95 C96 C89 115.6(2) . . ? C95 C96 H96A 108.4 . . ? C95 C96 H96B 108.4 . . ? H96A C96 H96B 107.4 . . ? C49 B2 H2 109.8 . . ? C89 B2 C49 112.9(2) . . ? C89 B2 C93 103.8(2) . . ? C89 B2 H2 109.8 . . ? C93 B2 C49 110.7(2) . . ? C93 B2 H2 109.8 . . ? 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 N1 C2 1.393(3) . ? N1 C4 1.352(3) . ? N1 C22 1.446(3) . ? N2 C3 1.405(3) . ? N2 C4 1.338(3) . ? N2 C36 1.463(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.483(4) . ? C1 B1 1.689(4) . ? C2 C3 1.369(4) . ? C3 C23 1.471(4) . ? C4 C5 1.472(4) . ? C5 C6 1.395(4) . ? C5 C10 1.387(4) . ? C6 H6 0.9500 . ? C6 C7 1.385(4) . ? C7 H7 0.9500 . ? C7 C8 1.386(4) . ? C8 H8 0.9500 . ? C8 C9 1.381(4) . ? C9 H9 0.9500 . ? C9 C10 1.392(4) . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 C12 1.537(4) . ? C12 H12 1.0000 . ? C12 C13 1.528(4) . ? C12 C14 1.526(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.386(4) . ? C14 C22 1.407(4) . ? C15 H15 0.9500 . ? C15 C16 1.384(4) . ? C16 H16 0.9500 . ? C16 C17 1.378(4) . ? C17 H17 0.9500 . ? C17 C18 1.386(4) . ? C18 C19 1.520(4) . ? C18 C22 1.404(4) . ? C19 H19 1.0000 . ? C19 C20 1.536(4) . ? C19 C21 1.524(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 C24 1.401(4) . ? C23 C28 1.404(4) . ? C24 H24 0.9500 . ? C24 C25 1.381(4) . ? C25 H25 0.9500 . ? C25 C26 1.397(4) . ? C26 H26 0.9500 . ? C26 C27 1.375(4) . ? C27 H27 0.9500 . ? C27 C28 1.392(4) . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C29 C30 1.522(4) . ? C30 H30 1.0000 . ? C30 C31 1.538(4) . ? C30 C32 1.525(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.386(4) . ? C32 C36 1.391(4) . ? C33 H33 0.9500 . ? C33 C34 1.374(4) . ? C34 H34 0.9500 . ? C34 C35 1.393(4) . ? C35 H35 0.9500 . ? C35 C37 1.400(4) . ? C36 C37 1.412(4) . ? C37 C38 1.514(4) . ? C38 H38 1.0000 . ? C38 C39 1.532(4) . ? C38 C40 1.530(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41 1.0000 . ? C41 C42 1.542(4) . ? C41 C48 1.530(4) . ? C41 B1 1.633(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42 C46 1.539(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.524(4) . ? C43 C47 1.539(4) . ? C44 H44 1.0000 . ? C44 C45 1.544(4) . ? C44 B1 1.636(4) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.527(4) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 C48 1.541(4) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? B1 H1 1.0000 . ? N3 C50 1.384(3) . ? N3 C52 1.355(3) . ? N3 C61 1.455(3) . ? N4 C51 1.406(3) . ? N4 C52 1.342(3) . ? N4 C79 1.456(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C49 C50 1.482(4) . ? C49 B2 1.679(4) . ? C50 C51 1.376(4) . ? C51 C83 1.465(4) . ? C52 C66 1.468(4) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C53 C54 1.534(4) . ? C54 H54 1.0000 . ? C54 C55 1.547(4) . ? C54 C56 1.524(4) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.392(4) . ? C56 C61 1.407(4) . ? C57 H57 0.9500 . ? C57 C58 1.370(4) . ? C58 H58 0.9500 . ? C58 C59 1.384(4) . ? C59 H59 0.9500 . ? C59 C60 1.395(4) . ? C60 C61 1.398(4) . ? C60 C62 1.521(4) . ? C62 H62 1.0000 . ? C62 C63 1.535(4) . ? C62 C64 1.531(4) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65 0.9500 . ? C65 C66 1.396(4) . ? C65 C70 1.378(4) . ? C66 C67 1.387(4) . ? C67 H67 0.9500 . ? C67 C68 1.391(4) . ? C68 H68 0.9500 . ? C68 C69 1.375(4) . ? C69 H69 0.9500 . ? C69 C70 1.385(4) . ? C70 H70 0.9500 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C71 C72 1.530(4) . ? C72 H72 1.0000 . ? C72 C73 1.527(4) . ? C72 C74 1.513(4) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C75 1.398(4) . ? C74 C79 1.394(4) . ? C75 H75 0.9500 . ? C75 C76 1.375(4) . ? C76 H76 0.9500 . ? C76 C77 1.391(4) . ? C77 H77 0.9500 . ? C77 C78 1.396(4) . ? C78 C79 1.410(4) . ? C78 C80 1.524(4) . ? C80 H80 1.0000 . ? C80 C81 1.536(4) . ? C80 C82 1.535(4) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 C84 1.395(4) . ? C83 C88 1.399(4) . ? C84 H84 0.9500 . ? C84 C85 1.389(4) . ? C85 H85 0.9500 . ? C85 C86 1.376(4) . ? C86 H86 0.9500 . ? C86 C87 1.395(4) . ? C87 H87 0.9500 . ? C87 C88 1.377(4) . ? C88 H88 0.9500 . ? C89 H89 1.0000 . ? C89 C90 1.544(4) . ? C89 C96 1.541(4) . ? C89 B2 1.640(4) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C90 C91 1.545(4) . ? C91 H91B 0.9900 . ? C91 H91A 0.9900 . ? C91 C92 1.535(4) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C92 C93 1.538(4) . ? C93 H93 1.0000 . ? C93 C94 1.536(4) . ? C93 B2 1.640(4) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C94 C95 1.539(4) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C95 C96 1.529(4) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? B2 H2 1.0000 . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.974 -0.322 1419.3 267.3 ?