# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 B3 Cl12 F6 N9' _chemical_formula_weight 1444.90 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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.068(5) _cell_length_b 14.208(5) _cell_length_c 30.518(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.173(4) _cell_angle_gamma 90.00 _cell_volume 6450(4) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 14836 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 30.77 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8930 _exptl_absorpt_correction_T_max 0.8930 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.111 _diffrn_reflns_number 26983 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11168 _reflns_number_gt 8711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1873P)^2^+8.0535P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11168 _refine_ls_number_parameters 913 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.2931 _refine_ls_wR_factor_gt 0.2718 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9129(2) -0.0198(3) 0.83820(13) 0.0327(8) Uani 1 1 d . . . C2 C 0.9535(3) -0.0756(3) 0.80718(14) 0.0374(9) Uani 1 1 d . . . H1 H 1.0076 -0.1109 0.8135 0.045 Uiso 1 1 calc R . . C3 C 0.8999(3) -0.0677(3) 0.76762(14) 0.0386(9) Uani 1 1 d . . . H2 H 0.9095 -0.0968 0.7407 0.046 Uiso 1 1 calc R . . C4 C 0.8248(3) -0.0073(3) 0.77305(13) 0.0326(8) Uani 1 1 d . . . C5 C 0.7544(3) 0.0222(3) 0.74282(13) 0.0319(8) Uani 1 1 d . . . C6 C 0.6879(2) 0.0830(3) 0.75692(12) 0.0298(8) Uani 1 1 d . . . C7 C 0.6112(3) 0.1192(3) 0.73123(12) 0.0312(8) Uani 1 1 d . . . H3 H 0.5909 0.1074 0.7006 0.037 Uiso 1 1 calc R . . C8 C 0.5692(2) 0.1770(3) 0.75961(12) 0.0296(8) Uani 1 1 d . . . C9 C 0.6249(2) 0.1718(2) 0.80323(12) 0.0281(7) Uani 1 1 d . . . C10 C 0.4783(2) 0.2744(2) 0.78712(12) 0.0285(8) Uani 1 1 d . . . C11 C 0.5335(2) 0.2694(3) 0.83051(12) 0.0298(8) Uani 1 1 d . . . C12 C 0.4948(3) 0.3307(3) 0.85828(13) 0.0332(8) Uani 1 1 d . . . H4 H 0.5156 0.3426 0.8888 0.040 Uiso 1 1 calc R . . C13 C 0.4195(2) 0.3708(3) 0.83215(14) 0.0330(8) Uani 1 1 d . . . C14 C 0.3603(3) 0.4403(3) 0.84485(14) 0.0356(9) Uani 1 1 d . . . C15 C 0.2906(3) 0.4731(3) 0.81390(15) 0.0382(9) Uani 1 1 d . . . C16 C 0.2257(3) 0.5457(3) 0.81714(18) 0.0496(11) Uani 1 1 d . . . H5 H 0.2183 0.5791 0.8433 0.059 Uiso 1 1 calc R . . C17 C 0.1770(3) 0.5581(3) 0.77616(19) 0.0541(13) Uani 1 1 d . . . H6 H 0.1293 0.6016 0.7682 0.065 Uiso 1 1 calc R . . C18 C 0.2114(3) 0.4928(3) 0.74729(17) 0.0478(11) Uani 1 1 d . . . H7 H 0.1901 0.4868 0.7164 0.057 Uiso 1 1 calc R . . C19 C 1.0355(3) -0.0644(3) 0.94892(14) 0.0365(9) Uani 1 1 d . . . H53 H 0.9877 -0.0697 0.9657 0.044 Uiso 1 1 calc R . . C20 C 1.0268(3) -0.0363(3) 0.90481(13) 0.0351(9) Uani 1 1 d . . . C21 C 1.1112(3) -0.0381(3) 0.89197(14) 0.0357(9) Uani 1 1 d . . . H8 H 1.1253 -0.0226 0.8636 0.043 Uiso 1 1 calc R . . C22 C 1.1714(2) -0.0675(3) 0.92951(13) 0.0323(8) Uani 1 1 d . . . C23 C 1.2658(3) -0.0778(3) 0.93727(14) 0.0362(9) Uani 1 1 d . . . C24 C 1.3104(3) -0.1009(3) 0.97938(15) 0.0400(9) Uani 1 1 d . . . C25 C 1.4034(3) -0.1110(4) 0.99540(17) 0.0530(12) Uani 1 1 d . . . H9 H 1.4512 -0.1034 0.9788 0.064 Uiso 1 1 calc R . . C26 C 1.4113(3) -0.1342(4) 1.03991(17) 0.0583(13) Uani 1 1 d . . . H10 H 1.4657 -0.1460 1.0595 0.070 Uiso 1 1 calc R . . C27 C 1.3248(3) -0.1372(4) 1.05094(16) 0.0515(12) Uani 1 1 d . . . H11 H 1.3112 -0.1511 1.0796 0.062 Uiso 1 1 calc R . . C28 C 0.7459(3) -0.0051(3) 0.69497(13) 0.0343(8) Uani 1 1 d . . . C29 C 0.7700(3) 0.0606(3) 0.66471(14) 0.0390(9) Uani 1 1 d . . . C30 C 0.7590(3) 0.0356(3) 0.62000(14) 0.0451(10) Uani 1 1 d . . . H12 H 0.7743 0.0798 0.5990 0.054 Uiso 1 1 calc R . . C31 C 0.7261(3) -0.0526(3) 0.60525(15) 0.0471(11) Uani 1 1 d . . . C32 C 0.7057(4) -0.1169(3) 0.63658(15) 0.0495(11) Uani 1 1 d . . . H13 H 0.6855 -0.1780 0.6270 0.059 Uiso 1 1 calc R . . C33 C 0.7137(3) -0.0946(3) 0.68139(14) 0.0420(10) Uani 1 1 d . . . C34 C 0.8055(4) 0.1563(3) 0.67977(16) 0.0519(12) Uani 1 1 d . . . H14 H 0.8292 0.1876 0.6555 0.078 Uiso 1 1 calc R . . H15 H 0.8535 0.1494 0.7053 0.078 Uiso 1 1 calc R . . H16 H 0.7567 0.1942 0.6884 0.078 Uiso 1 1 calc R . . C35 C 0.7088(5) -0.0766(4) 0.55633(17) 0.0681(16) Uani 1 1 d . . . H17 H 0.7530 -0.1232 0.5499 0.102 Uiso 1 1 calc R . . H18 H 0.7141 -0.0196 0.5389 0.102 Uiso 1 1 calc R . . H19 H 0.6482 -0.1027 0.5485 0.102 Uiso 1 1 calc R . . C36 C 0.6884(4) -0.1655(3) 0.71367(16) 0.0515(12) Uani 1 1 d . . . H20 H 0.6524 -0.2155 0.6974 0.077 Uiso 1 1 calc R . . H21 H 0.6534 -0.1346 0.7340 0.077 Uiso 1 1 calc R . . H22 H 0.7431 -0.1927 0.7307 0.077 Uiso 1 1 calc R . . C37 C 0.3789(3) 0.4822(3) 0.89014(15) 0.0393(9) Uani 1 1 d . . . C38 C 0.3347(3) 0.4487(3) 0.92369(16) 0.0481(11) Uani 1 1 d . . . C39 C 0.3530(4) 0.4927(4) 0.96548(18) 0.0609(14) Uani 1 1 d . . . H23 H 0.3242 0.4702 0.9889 0.073 Uiso 1 1 calc R . . C40 C 0.4123(4) 0.5685(4) 0.97339(18) 0.0607(15) Uani 1 1 d . . . C41 C 0.4550(4) 0.5986(4) 0.9396(2) 0.0599(14) Uani 1 1 d . . . H24 H 0.4960 0.6497 0.9451 0.072 Uiso 1 1 calc R . . C42 C 0.4410(3) 0.5574(3) 0.89744(17) 0.0479(11) Uani 1 1 d . . . C43 C 0.2690(4) 0.3693(4) 0.9157(2) 0.0697(16) Uani 1 1 d . . . H25 H 0.2164 0.3893 0.8947 0.105 Uiso 1 1 calc R . . H26 H 0.2503 0.3510 0.9438 0.105 Uiso 1 1 calc R . . H27 H 0.2974 0.3154 0.9034 0.105 Uiso 1 1 calc R . . C44 C 0.4292(5) 0.6163(5) 1.0182(2) 0.084(2) Uani 1 1 d . . . H28 H 0.3846 0.6661 1.0191 0.126 Uiso 1 1 calc R . . H29 H 0.4896 0.6437 1.0230 0.126 Uiso 1 1 calc R . . H30 H 0.4244 0.5699 1.0415 0.126 Uiso 1 1 calc R . . C45 C 0.4889(4) 0.5933(4) 0.8617(2) 0.0602(13) Uani 1 1 d . . . H31 H 0.5230 0.6499 0.8721 0.090 Uiso 1 1 calc R . . H32 H 0.4451 0.6085 0.8354 0.090 Uiso 1 1 calc R . . H33 H 0.5303 0.5449 0.8541 0.090 Uiso 1 1 calc R . . C46 C 1.3222(3) -0.0658(3) 0.90123(15) 0.0399(9) Uani 1 1 d . . . C47 C 1.3648(3) 0.0202(3) 0.89568(17) 0.0477(11) Uani 1 1 d . . . C48 C 1.4275(3) 0.0240(4) 0.86623(17) 0.0518(12) Uani 1 1 d . . . H34 H 1.4563 0.0821 0.8621 0.062 Uiso 1 1 calc R . . C49 C 1.4486(3) -0.0547(4) 0.84294(16) 0.0492(11) Uani 1 1 d . . . C50 C 1.4026(3) -0.1378(3) 0.84760(15) 0.0463(10) Uani 1 1 d . . . H35 H 1.4145 -0.1913 0.8308 0.056 Uiso 1 1 calc R . . C51 C 1.3392(3) -0.1453(3) 0.87620(14) 0.0384(9) Uani 1 1 d . . . C52 C 1.3457(4) 0.1057(4) 0.9220(2) 0.0649(15) Uani 1 1 d . . . H36 H 1.2806 0.1139 0.9198 0.097 Uiso 1 1 calc R . . H37 H 1.3718 0.1615 0.9101 0.097 Uiso 1 1 calc R . . H38 H 1.3724 0.0971 0.9532 0.097 Uiso 1 1 calc R . . C53 C 1.5193(4) -0.0517(5) 0.81259(19) 0.0650(15) Uani 1 1 d . . . H39 H 1.4995 -0.0091 0.7877 0.098 Uiso 1 1 calc R . . H40 H 1.5276 -0.1151 0.8012 0.098 Uiso 1 1 calc R . . H41 H 1.5763 -0.0292 0.8293 0.098 Uiso 1 1 calc R . . C54 C 1.2911(3) -0.2361(3) 0.87938(17) 0.0487(11) Uani 1 1 d . . . H42 H 1.3115 -0.2822 0.8592 0.073 Uiso 1 1 calc R . . H43 H 1.2263 -0.2261 0.8711 0.073 Uiso 1 1 calc R . . H44 H 1.3040 -0.2597 0.9099 0.073 Uiso 1 1 calc R . . N1 N 0.8360(2) 0.0192(2) 0.81784(10) 0.0317(7) Uani 1 1 d . . . N2 N 0.6965(2) 0.1132(2) 0.80059(10) 0.0292(7) Uani 1 1 d . . . N3 N 0.4087(2) 0.3368(2) 0.78880(11) 0.0313(7) Uani 1 1 d . . . N4 N 0.2772(2) 0.4419(2) 0.76982(12) 0.0365(8) Uani 1 1 d . . . N5 N 0.6087(2) 0.2155(2) 0.83922(10) 0.0298(7) Uani 1 1 d . . . N6 N 0.4935(2) 0.2283(2) 0.75107(10) 0.0276(6) Uani 1 1 d . . . N7 N 1.1227(2) -0.0830(2) 0.96404(11) 0.0341(7) Uani 1 1 d . . . N8 N 1.2637(2) -0.1174(3) 1.01484(12) 0.0416(8) Uani 1 1 d . . . N9 N 0.9428(2) -0.0058(2) 0.88118(11) 0.0365(8) Uani 1 1 d . . . H45 H 0.9072 0.0251 0.8963 0.044 Uiso 1 1 calc R . . B1 B 0.7672(3) 0.0782(3) 0.83925(14) 0.0316(9) Uani 1 1 d . . . B2 B 0.3310(3) 0.3617(3) 0.75070(16) 0.0363(10) Uani 1 1 d . . . B3 B 1.1606(3) -0.1177(4) 1.01156(16) 0.0403(11) Uani 1 1 d . . . F1 F 0.72830(15) 0.02165(17) 0.86826(8) 0.0390(6) Uani 1 1 d . . . F2 F 0.81260(15) 0.15195(16) 0.86336(8) 0.0386(6) Uani 1 1 d . . . F3 F 0.36119(17) 0.3938(2) 0.71324(9) 0.0539(7) Uani 1 1 d . . . F4 F 0.27546(15) 0.28471(17) 0.73979(9) 0.0448(6) Uani 1 1 d . . . F5 F 1.12908(19) -0.2073(2) 1.01733(11) 0.0618(8) Uani 1 1 d . . . F6 F 1.13401(17) -0.0557(2) 1.04211(8) 0.0548(7) Uani 1 1 d . . . C55 C 1.1336(4) 0.2013(5) 0.7796(2) 0.0764(17) Uani 1 1 d . . . H46 H 1.1630 0.2047 0.7525 0.092 Uiso 1 1 calc R . . Cl1 Cl 1.08940(16) 0.31231(15) 0.78878(12) 0.1276(10) Uani 1 1 d . . . Cl2 Cl 1.04910(15) 0.11490(17) 0.77119(7) 0.1063(7) Uani 1 1 d . . . Cl3 Cl 1.21439(14) 0.16901(15) 0.82464(6) 0.0926(6) Uani 1 1 d . . . C56 C 1.059(3) 0.662(3) 0.9249(15) 0.157(17) Uani 0.491(12) 1 d P A 2 H47 H 1.0718 0.7197 0.9432 0.188 Uiso 0.491(12) 1 calc PR A 2 Cl4 Cl 1.0333(10) 0.7058(8) 0.8719(5) 0.187(6) Uani 0.491(12) 1 d P A 2 Cl5 Cl 0.9680(5) 0.6138(7) 0.9452(6) 0.199(6) Uani 0.491(12) 1 d P A 2 Cl6 Cl 1.1526(2) 0.6027(3) 0.93612(15) 0.0392(11) Uani 0.491(12) 1 d P A 2 C57 C 0.993(2) 0.770(2) 1.0688(7) 0.251(8) Uani 0.484(5) 1 d PDU B 3 H48 H 1.0566 0.7893 1.0670 0.301 Uiso 0.484(5) 1 calc PR B 3 Cl7 Cl 0.9116(5) 0.8298(5) 1.0332(3) 0.157(3) Uani 0.484(5) 1 d PDU B 3 Cl8 Cl 0.9658(8) 0.7721(14) 1.1221(5) 0.286(7) Uani 0.484(5) 1 d PDU B 3 Cl9 Cl 0.9713(12) 0.6503(18) 1.0614(8) 0.309(8) Uani 0.484(5) 1 d PDU B 3 C58 C 0.7111(19) 0.838(2) 0.9517(12) 0.188(8) Uani 0.329(6) 1 d PDU C 4 H49 H 0.7330 0.8886 0.9735 0.226 Uiso 0.329(6) 1 calc PR C 4 Cl10 Cl 0.6095(14) 0.8655(15) 0.9210(9) 0.180(7) Uani 0.329(6) 1 d PDU C 4 Cl11 Cl 0.6901(7) 0.7366(7) 0.9773(3) 0.144(4) Uani 0.329(6) 1 d PDU C 4 Cl12 Cl 0.7904(18) 0.8097(18) 0.9183(9) 0.246(9) Uani 0.329(6) 1 d PDU C 4 C59 C 1.0472(13) 0.6669(11) 0.9198(7) 0.054(4) Uani 0.509(12) 1 d P A 1 H50 H 1.0375 0.7170 0.9416 0.064 Uiso 0.509(12) 1 calc PR A 1 Cl13 Cl 1.0453(2) 0.7127(4) 0.8664(2) 0.0655(15) Uani 0.509(12) 1 d P A 1 Cl14 Cl 0.9549(3) 0.5809(3) 0.91202(16) 0.0862(18) Uani 0.509(12) 1 d P A 1 Cl15 Cl 1.1483(8) 0.6060(8) 0.9363(4) 0.130(4) Uani 0.509(12) 1 d P A 1 C60 C 0.9898(11) 0.6938(12) 1.0753(5) 0.19(2) Uani 0.516(5) 1 d PD B 1 H51 H 1.0547 0.7080 1.0749 0.227 Uiso 0.516(5) 1 calc PR B 1 Cl16 Cl 0.9844(3) 0.6088(4) 1.11627(16) 0.1137(17) Uani 0.516(5) 1 d PD B 1 Cl17 Cl 0.9454(2) 0.6466(2) 1.02354(12) 0.0762(11) Uani 0.516(5) 1 d PD B 1 Cl18 Cl 0.9384(3) 0.7970(3) 1.08665(15) 0.0901(13) Uani 0.516(5) 1 d PD B 1 C61 C 0.7411(7) 0.8652(6) 0.9391(3) 0.071(3) Uani 0.671(6) 1 d P C 1 H52 H 0.7457 0.9331 0.9312 0.085 Uiso 0.671(6) 1 calc PR C 1 Cl19 Cl 0.7891(3) 0.8537(2) 0.99437(9) 0.1067(14) Uani 0.671(6) 1 d P C 1 Cl20 Cl 0.6306(4) 0.8334(4) 0.9243(3) 0.1144(19) Uani 0.671(6) 1 d P C 1 Cl21 Cl 0.8085(2) 0.80233(19) 0.90772(11) 0.0737(8) Uani 0.671(6) 1 d P C 1 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 C1 0.0237(18) 0.0333(19) 0.039(2) -0.0010(16) -0.0028(15) 0.0076(15) C2 0.029(2) 0.039(2) 0.043(2) -0.0029(17) 0.0004(17) 0.0112(16) C3 0.031(2) 0.040(2) 0.044(2) -0.0049(17) 0.0037(17) 0.0104(17) C4 0.0288(19) 0.0329(19) 0.0348(19) -0.0031(15) 0.0013(15) 0.0044(15) C5 0.0286(19) 0.0324(19) 0.034(2) -0.0003(15) 0.0028(15) 0.0062(15) C6 0.0265(18) 0.0319(18) 0.0300(18) 0.0012(14) 0.0014(14) 0.0031(15) C7 0.0271(19) 0.0350(19) 0.0298(18) -0.0014(15) -0.0006(15) 0.0037(15) C8 0.0246(18) 0.0291(18) 0.0330(19) 0.0007(14) -0.0015(14) 0.0005(14) C9 0.0220(17) 0.0286(17) 0.0313(18) 0.0025(14) -0.0028(14) 0.0017(14) C10 0.0206(17) 0.0259(17) 0.0371(19) 0.0008(14) -0.0018(14) -0.0005(13) C11 0.0250(18) 0.0300(18) 0.0318(19) 0.0024(15) -0.0037(14) 0.0049(14) C12 0.0249(19) 0.0349(19) 0.038(2) -0.0040(16) -0.0020(15) 0.0070(15) C13 0.0225(18) 0.0300(18) 0.045(2) -0.0065(16) -0.0002(16) 0.0005(14) C14 0.0249(19) 0.033(2) 0.048(2) -0.0067(17) 0.0009(16) 0.0039(15) C15 0.028(2) 0.032(2) 0.052(2) -0.0081(17) -0.0022(17) 0.0043(16) C16 0.031(2) 0.041(2) 0.072(3) -0.012(2) -0.006(2) 0.0112(18) C17 0.036(2) 0.039(2) 0.080(3) -0.009(2) -0.014(2) 0.0143(19) C18 0.034(2) 0.039(2) 0.064(3) 0.000(2) -0.012(2) 0.0084(18) C19 0.0232(19) 0.039(2) 0.044(2) -0.0082(17) -0.0061(16) 0.0085(15) C20 0.0229(19) 0.038(2) 0.040(2) -0.0056(16) -0.0077(16) 0.0063(15) C21 0.0238(19) 0.034(2) 0.045(2) -0.0023(16) -0.0059(16) 0.0033(15) C22 0.0225(18) 0.0309(19) 0.040(2) -0.0049(15) -0.0048(15) 0.0013(14) C23 0.0220(19) 0.0327(19) 0.050(2) -0.0066(17) -0.0069(16) 0.0022(15) C24 0.025(2) 0.043(2) 0.047(2) -0.0065(18) -0.0079(17) 0.0064(16) C25 0.029(2) 0.065(3) 0.059(3) -0.009(2) -0.012(2) 0.009(2) C26 0.029(2) 0.086(4) 0.052(3) -0.013(3) -0.018(2) 0.016(2) C27 0.041(2) 0.067(3) 0.042(2) -0.014(2) -0.0088(19) 0.019(2) C28 0.030(2) 0.038(2) 0.034(2) -0.0010(16) 0.0018(16) 0.0088(16) C29 0.034(2) 0.042(2) 0.040(2) -0.0014(17) 0.0004(17) 0.0025(17) C30 0.045(3) 0.053(3) 0.037(2) 0.0041(19) 0.0066(19) 0.000(2) C31 0.054(3) 0.052(3) 0.037(2) -0.0078(19) 0.008(2) 0.005(2) C32 0.064(3) 0.040(2) 0.044(2) -0.0108(19) 0.008(2) -0.001(2) C33 0.047(2) 0.038(2) 0.041(2) -0.0036(17) 0.0074(19) 0.0068(18) C34 0.058(3) 0.051(3) 0.047(3) -0.003(2) 0.009(2) -0.012(2) C35 0.095(5) 0.071(4) 0.040(3) -0.011(2) 0.015(3) -0.013(3) C36 0.072(3) 0.037(2) 0.046(3) -0.0008(19) 0.010(2) 0.002(2) C37 0.032(2) 0.034(2) 0.049(2) -0.0089(17) -0.0031(17) 0.0118(16) C38 0.040(2) 0.049(3) 0.055(3) -0.011(2) 0.005(2) 0.0125(19) C39 0.057(3) 0.073(3) 0.052(3) -0.011(3) 0.006(2) 0.028(3) C40 0.052(3) 0.069(3) 0.055(3) -0.024(3) -0.011(2) 0.029(3) C41 0.045(3) 0.052(3) 0.074(4) -0.024(3) -0.016(3) 0.014(2) C42 0.035(2) 0.044(2) 0.059(3) -0.013(2) -0.009(2) 0.0063(18) C43 0.071(4) 0.061(3) 0.085(4) -0.015(3) 0.037(3) -0.005(3) C44 0.080(4) 0.094(5) 0.069(4) -0.040(3) -0.014(3) 0.037(4) C45 0.048(3) 0.054(3) 0.076(4) -0.011(3) 0.002(3) -0.012(2) C46 0.0215(19) 0.043(2) 0.052(2) 0.0036(18) -0.0061(17) 0.0001(16) C47 0.029(2) 0.041(2) 0.066(3) 0.005(2) -0.013(2) -0.0055(17) C48 0.031(2) 0.055(3) 0.064(3) 0.015(2) -0.008(2) -0.014(2) C49 0.032(2) 0.062(3) 0.050(3) 0.009(2) -0.0005(19) -0.010(2) C50 0.035(2) 0.055(3) 0.048(2) 0.005(2) 0.0026(19) -0.0009(19) C51 0.028(2) 0.041(2) 0.043(2) 0.0048(17) -0.0013(17) -0.0015(16) C52 0.047(3) 0.043(3) 0.101(4) -0.005(3) 0.002(3) -0.007(2) C53 0.043(3) 0.091(4) 0.060(3) 0.008(3) 0.005(2) -0.020(3) C54 0.049(3) 0.042(2) 0.056(3) -0.002(2) 0.014(2) -0.004(2) N1 0.0235(15) 0.0356(17) 0.0335(16) -0.0025(13) -0.0026(13) 0.0059(13) N2 0.0255(16) 0.0298(15) 0.0306(16) -0.0009(12) -0.0007(13) 0.0062(12) N3 0.0195(15) 0.0308(16) 0.0402(17) -0.0003(13) -0.0056(13) 0.0052(12) N4 0.0240(16) 0.0316(16) 0.050(2) 0.0010(14) -0.0057(14) 0.0059(13) N5 0.0231(15) 0.0309(16) 0.0333(16) -0.0032(13) -0.0015(12) 0.0048(12) N6 0.0227(15) 0.0250(14) 0.0331(16) -0.0002(12) -0.0017(12) 0.0002(11) N7 0.0230(16) 0.0377(17) 0.0378(18) -0.0057(14) -0.0067(13) 0.0076(13) N8 0.0303(18) 0.049(2) 0.0410(19) -0.0048(15) -0.0087(15) 0.0161(15) N9 0.0205(16) 0.0487(19) 0.0373(17) -0.0034(15) -0.0051(13) 0.0140(14) B1 0.021(2) 0.036(2) 0.035(2) 0.0005(17) -0.0045(17) 0.0087(17) B2 0.024(2) 0.039(2) 0.044(2) 0.0028(19) -0.0016(18) 0.0061(17) B3 0.029(2) 0.048(3) 0.041(3) 0.001(2) -0.0032(19) 0.012(2) F1 0.0300(12) 0.0471(13) 0.0391(12) 0.0090(10) 0.0029(9) 0.0106(10) F2 0.0306(12) 0.0390(12) 0.0411(12) -0.0086(10) -0.0100(10) 0.0071(9) F3 0.0364(14) 0.0761(18) 0.0487(15) 0.0233(13) 0.0050(11) 0.0191(13) F4 0.0267(12) 0.0421(13) 0.0603(15) -0.0137(11) -0.0097(11) 0.0033(10) F5 0.0437(16) 0.0623(18) 0.0743(19) 0.0212(15) -0.0065(14) 0.0056(13) F6 0.0369(14) 0.086(2) 0.0378(13) -0.0079(13) -0.0064(11) 0.0284(13) C55 0.065(4) 0.084(4) 0.077(4) 0.022(3) 0.002(3) -0.009(3) Cl1 0.0873(14) 0.0763(12) 0.225(3) 0.0468(15) 0.0411(16) 0.0161(10) Cl2 0.0954(14) 0.1232(16) 0.0972(14) -0.0008(12) 0.0062(11) -0.0512(12) Cl3 0.0902(13) 0.1037(13) 0.0758(11) 0.0063(9) -0.0118(9) 0.0052(10) C56 0.10(2) 0.18(3) 0.19(3) 0.10(2) 0.04(2) 0.06(2) Cl4 0.254(12) 0.109(6) 0.152(8) -0.002(5) -0.112(8) 0.013(6) Cl5 0.078(4) 0.204(8) 0.324(17) -0.048(9) 0.062(7) -0.002(4) Cl6 0.0336(19) 0.042(2) 0.041(2) 0.0104(16) 0.0023(15) 0.0072(14) C57 0.180(13) 0.317(15) 0.253(14) 0.069(14) 0.027(12) 0.034(13) Cl7 0.116(5) 0.143(5) 0.210(8) -0.006(5) 0.016(4) 0.011(4) Cl8 0.179(9) 0.432(17) 0.237(12) 0.127(12) 0.001(8) 0.022(11) Cl9 0.228(14) 0.380(17) 0.314(17) 0.087(16) 0.022(12) 0.039(14) C58 0.158(13) 0.201(14) 0.206(14) 0.021(13) 0.033(12) -0.006(12) Cl10 0.123(10) 0.203(15) 0.225(13) 0.059(12) 0.066(9) 0.016(9) Cl11 0.133(7) 0.158(7) 0.137(7) 0.005(6) 0.010(5) -0.030(6) Cl12 0.228(11) 0.243(11) 0.265(12) 0.000(8) 0.034(8) -0.013(8) C59 0.043(7) 0.043(7) 0.073(9) -0.016(7) 0.005(6) -0.003(6) Cl13 0.0346(18) 0.055(2) 0.096(3) 0.028(2) -0.0224(17) -0.0036(13) Cl14 0.072(2) 0.095(3) 0.092(3) -0.0054(19) 0.0134(18) -0.0411(19) Cl15 0.149(8) 0.141(8) 0.093(7) 0.022(5) 0.000(6) 0.008(6) C60 0.051(9) 0.44(6) 0.082(12) -0.05(2) 0.040(9) -0.039(19) Cl16 0.077(2) 0.152(4) 0.110(3) 0.043(3) 0.009(2) -0.001(2) Cl17 0.082(2) 0.0723(19) 0.078(2) -0.0082(15) 0.0252(17) -0.0025(15) Cl18 0.073(2) 0.094(2) 0.099(3) -0.017(2) 0.0015(19) -0.0053(17) C61 0.092(7) 0.057(5) 0.061(5) -0.009(4) 0.007(5) 0.026(5) Cl19 0.177(4) 0.0740(17) 0.0614(15) 0.0109(12) -0.0032(17) 0.0069(18) Cl20 0.078(3) 0.113(3) 0.159(4) -0.027(3) 0.039(3) -0.025(3) Cl21 0.0705(16) 0.0582(13) 0.0864(17) -0.0158(11) -0.0059(12) -0.0075(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N9 1.332(5) . ? C1 N1 1.345(5) . ? C1 C2 1.443(5) . ? C2 C3 1.346(6) . ? C2 H1 0.9500 . ? C3 C4 1.451(5) . ? C3 H2 0.9500 . ? C4 C5 1.356(6) . ? C4 N1 1.402(5) . ? C5 C6 1.440(5) . ? C5 C28 1.497(5) . ? C6 N2 1.386(5) . ? C6 C7 1.388(5) . ? C7 C8 1.415(5) . ? C7 H3 0.9500 . ? C8 N6 1.344(5) . ? C8 C9 1.459(5) . ? C9 N5 1.318(5) . ? C9 N2 1.374(5) . ? C10 N6 1.331(5) . ? C10 N3 1.380(5) . ? C10 C11 1.449(5) . ? C11 N5 1.358(5) . ? C11 C12 1.405(5) . ? C12 C13 1.400(5) . ? C12 H4 0.9500 . ? C13 N3 1.393(5) . ? C13 C14 1.426(5) . ? C14 C15 1.377(6) . ? C14 C37 1.489(6) . ? C15 N4 1.400(6) . ? C15 C16 1.436(6) . ? C16 C17 1.357(7) . ? C16 H5 0.9500 . ? C17 C18 1.432(7) . ? C17 H6 0.9500 . ? C18 N4 1.328(5) . ? C18 H7 0.9500 . ? C19 N7 1.348(5) . ? C19 C20 1.390(6) . ? C19 H53 0.9500 . ? C20 C21 1.389(6) . ? C20 N9 1.421(5) . ? C21 C22 1.407(6) . ? C21 H8 0.9500 . ? C22 N7 1.394(5) . ? C22 C23 1.412(5) . ? C23 C24 1.391(6) . ? C23 C46 1.503(6) . ? C24 N8 1.401(6) . ? C24 C25 1.417(6) . ? C25 C26 1.384(8) . ? C25 H9 0.9500 . ? C26 C27 1.397(7) . ? C26 H10 0.9500 . ? C27 N8 1.349(6) . ? C27 H11 0.9500 . ? C28 C29 1.400(6) . ? C28 C33 1.401(6) . ? C29 C30 1.394(6) . ? C29 C34 1.506(6) . ? C30 C31 1.396(7) . ? C30 H12 0.9500 . ? C31 C32 1.392(7) . ? C31 C35 1.513(6) . ? C32 C33 1.390(6) . ? C32 H13 0.9500 . ? C33 C36 1.500(6) . ? C34 H14 0.9800 . ? C34 H15 0.9800 . ? C34 H16 0.9800 . ? C35 H17 0.9800 . ? C35 H18 0.9800 . ? C35 H19 0.9800 . ? C36 H20 0.9800 . ? C36 H21 0.9800 . ? C36 H22 0.9800 . ? C37 C38 1.391(7) . ? C37 C42 1.415(6) . ? C38 C39 1.408(7) . ? C38 C43 1.495(8) . ? C39 C40 1.395(9) . ? C39 H23 0.9500 . ? C40 C41 1.368(9) . ? C40 C44 1.510(7) . ? C41 C42 1.399(7) . ? C41 H24 0.9500 . ? C42 C45 1.491(8) . ? C43 H25 0.9800 . ? C43 H26 0.9800 . ? C43 H27 0.9800 . ? C44 H28 0.9800 . ? C44 H29 0.9800 . ? C44 H30 0.9800 . ? C45 H31 0.9800 . ? C45 H32 0.9800 . ? C45 H33 0.9800 . ? C46 C47 1.403(6) . ? C46 C51 1.410(6) . ? C47 C48 1.405(7) . ? C47 C52 1.509(8) . ? C48 C49 1.388(8) . ? C48 H34 0.9500 . ? C49 C50 1.388(7) . ? C49 C53 1.520(7) . ? C50 C51 1.396(6) . ? C50 H35 0.9500 . ? C51 C54 1.490(6) . ? C52 H36 0.9800 . ? C52 H37 0.9800 . ? C52 H38 0.9800 . ? C53 H39 0.9800 . ? C53 H40 0.9800 . ? C53 H41 0.9800 . ? C54 H42 0.9800 . ? C54 H43 0.9800 . ? C54 H44 0.9800 . ? N1 B1 1.555(5) . ? N2 B1 1.541(5) . ? N3 B2 1.554(5) . ? N4 B2 1.564(6) . ? N7 B3 1.552(6) . ? N8 B3 1.540(6) . ? N9 H45 0.8800 . ? B1 F1 1.392(5) . ? B1 F2 1.395(5) . ? B2 F3 1.374(6) . ? B2 F4 1.385(5) . ? B3 F5 1.380(6) . ? B3 F6 1.388(6) . ? C55 Cl3 1.747(7) . ? C55 Cl1 1.752(8) . ? C55 Cl2 1.757(7) . ? C55 H46 1.0000 . ? C56 Cl6 1.63(4) . ? C56 Cl4 1.72(4) . ? C56 Cl5 1.73(4) . ? C56 H47 1.0000 . ? C57 Cl7 1.730(19) . ? C57 Cl8 1.74(2) . ? C57 Cl9 1.74(2) . ? C57 H48 1.0000 . ? C58 Cl11 1.69(2) . ? C58 Cl10 1.71(2) . ? C58 Cl12 1.74(2) . ? C58 H49 1.0000 . ? C59 Cl13 1.75(2) . ? C59 Cl15 1.75(2) . ? C59 Cl14 1.837(16) . ? C59 H50 1.0000 . ? C60 Cl18 1.719(16) . ? C60 Cl17 1.747(15) . ? C60 Cl16 1.751(16) . ? C60 H51 1.0000 . ? C61 Cl20 1.716(12) . ? C61 Cl19 1.734(10) . ? C61 Cl21 1.747(9) . ? C61 H52 1.0000 . ? 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 N9 C1 N1 121.7(3) . . ? N9 C1 C2 128.0(3) . . ? N1 C1 C2 110.3(3) . . ? C3 C2 C1 106.6(3) . . ? C3 C2 H1 126.7 . . ? C1 C2 H1 126.7 . . ? C2 C3 C4 108.3(4) . . ? C2 C3 H2 125.8 . . ? C4 C3 H2 125.8 . . ? C5 C4 N1 122.7(3) . . ? C5 C4 C3 130.2(4) . . ? N1 C4 C3 107.2(3) . . ? C4 C5 C6 119.2(3) . . ? C4 C5 C28 121.3(3) . . ? C6 C5 C28 119.5(3) . . ? N2 C6 C7 111.7(3) . . ? N2 C6 C5 120.7(3) . . ? C7 C6 C5 127.6(3) . . ? C6 C7 C8 106.4(3) . . ? C6 C7 H3 126.8 . . ? C8 C7 H3 126.8 . . ? N6 C8 C7 130.2(3) . . ? N6 C8 C9 123.6(3) . . ? C7 C8 C9 106.3(3) . . ? N5 C9 N2 125.9(3) . . ? N5 C9 C8 125.4(3) . . ? N2 C9 C8 108.7(3) . . ? N6 C10 N3 125.3(3) . . ? N6 C10 C11 125.6(3) . . ? N3 C10 C11 109.1(3) . . ? N5 C11 C12 130.2(3) . . ? N5 C11 C10 123.1(3) . . ? C12 C11 C10 106.7(3) . . ? C13 C12 C11 106.6(3) . . ? C13 C12 H4 126.7 . . ? C11 C12 H4 126.7 . . ? N3 C13 C12 111.2(3) . . ? N3 C13 C14 121.0(3) . . ? C12 C13 C14 127.8(4) . . ? C15 C14 C13 119.3(4) . . ? C15 C14 C37 120.8(3) . . ? C13 C14 C37 119.7(4) . . ? C14 C15 N4 122.0(4) . . ? C14 C15 C16 130.5(4) . . ? N4 C15 C16 107.4(4) . . ? C17 C16 C15 107.7(4) . . ? C17 C16 H5 126.2 . . ? C15 C16 H5 126.2 . . ? C16 C17 C18 106.7(4) . . ? C16 C17 H6 126.6 . . ? C18 C17 H6 126.6 . . ? N4 C18 C17 110.3(4) . . ? N4 C18 H7 124.8 . . ? C17 C18 H7 124.8 . . ? N7 C19 C20 108.9(4) . . ? N7 C19 H53 125.5 . . ? C20 C19 H53 125.5 . . ? C21 C20 C19 108.6(3) . . ? C21 C20 N9 130.1(4) . . ? C19 C20 N9 121.2(4) . . ? C20 C21 C22 106.1(4) . . ? C20 C21 H8 127.0 . . ? C22 C21 H8 127.0 . . ? N7 C22 C21 108.3(3) . . ? N7 C22 C23 119.6(4) . . ? C21 C22 C23 132.0(4) . . ? C24 C23 C22 120.3(4) . . ? C24 C23 C46 117.2(4) . . ? C22 C23 C46 122.5(4) . . ? C23 C24 N8 121.7(4) . . ? C23 C24 C25 130.4(4) . . ? N8 C24 C25 107.9(4) . . ? C26 C25 C24 106.7(5) . . ? C26 C25 H9 126.6 . . ? C24 C25 H9 126.6 . . ? C25 C26 C27 107.9(4) . . ? C25 C26 H10 126.1 . . ? C27 C26 H10 126.1 . . ? N8 C27 C26 109.8(4) . . ? N8 C27 H11 125.1 . . ? C26 C27 H11 125.1 . . ? C29 C28 C33 121.6(4) . . ? C29 C28 C5 118.7(4) . . ? C33 C28 C5 119.7(4) . . ? C30 C29 C28 118.3(4) . . ? C30 C29 C34 120.6(4) . . ? C28 C29 C34 121.1(4) . . ? C29 C30 C31 121.6(4) . . ? C29 C30 H12 119.2 . . ? C31 C30 H12 119.2 . . ? C32 C31 C30 118.3(4) . . ? C32 C31 C35 120.5(4) . . ? C30 C31 C35 121.1(4) . . ? C33 C32 C31 122.2(4) . . ? C33 C32 H13 118.9 . . ? C31 C32 H13 118.9 . . ? C32 C33 C28 118.0(4) . . ? C32 C33 C36 120.1(4) . . ? C28 C33 C36 121.9(4) . . ? C29 C34 H14 109.5 . . ? C29 C34 H15 109.5 . . ? H14 C34 H15 109.5 . . ? C29 C34 H16 109.5 . . ? H14 C34 H16 109.5 . . ? H15 C34 H16 109.5 . . ? C31 C35 H17 109.5 . . ? C31 C35 H18 109.5 . . ? H17 C35 H18 109.5 . . ? C31 C35 H19 109.5 . . ? H17 C35 H19 109.5 . . ? H18 C35 H19 109.5 . . ? C33 C36 H20 109.5 . . ? C33 C36 H21 109.5 . . ? H20 C36 H21 109.5 . . ? C33 C36 H22 109.5 . . ? H20 C36 H22 109.5 . . ? H21 C36 H22 109.5 . . ? C38 C37 C42 121.6(4) . . ? C38 C37 C14 120.4(4) . . ? C42 C37 C14 118.0(4) . . ? C37 C38 C39 117.9(5) . . ? C37 C38 C43 121.3(4) . . ? C39 C38 C43 120.8(5) . . ? C40 C39 C38 121.8(5) . . ? C40 C39 H23 119.1 . . ? C38 C39 H23 119.1 . . ? C41 C40 C39 118.4(5) . . ? C41 C40 C44 120.6(6) . . ? C39 C40 C44 120.9(6) . . ? C40 C41 C42 122.8(5) . . ? C40 C41 H24 118.6 . . ? C42 C41 H24 118.6 . . ? C41 C42 C37 117.4(5) . . ? C41 C42 C45 120.7(5) . . ? C37 C42 C45 121.9(4) . . ? C38 C43 H25 109.5 . . ? C38 C43 H26 109.5 . . ? H25 C43 H26 109.5 . . ? C38 C43 H27 109.5 . . ? H25 C43 H27 109.5 . . ? H26 C43 H27 109.5 . . ? C40 C44 H28 109.5 . . ? C40 C44 H29 109.5 . . ? H28 C44 H29 109.5 . . ? C40 C44 H30 109.5 . . ? H28 C44 H30 109.5 . . ? H29 C44 H30 109.5 . . ? C42 C45 H31 109.5 . . ? C42 C45 H32 109.5 . . ? H31 C45 H32 109.5 . . ? C42 C45 H33 109.5 . . ? H31 C45 H33 109.5 . . ? H32 C45 H33 109.5 . . ? C47 C46 C51 120.4(4) . . ? C47 C46 C23 120.6(4) . . ? C51 C46 C23 118.6(4) . . ? C46 C47 C48 118.5(4) . . ? C46 C47 C52 120.5(5) . . ? C48 C47 C52 121.0(4) . . ? C49 C48 C47 121.9(4) . . ? C49 C48 H34 119.0 . . ? C47 C48 H34 119.0 . . ? C50 C49 C48 118.3(4) . . ? C50 C49 C53 119.7(5) . . ? C48 C49 C53 122.0(5) . . ? C49 C50 C51 122.1(5) . . ? C49 C50 H35 119.0 . . ? C51 C50 H35 119.0 . . ? C50 C51 C46 118.6(4) . . ? C50 C51 C54 119.7(4) . . ? C46 C51 C54 121.7(4) . . ? C47 C52 H36 109.5 . . ? C47 C52 H37 109.5 . . ? H36 C52 H37 109.5 . . ? C47 C52 H38 109.5 . . ? H36 C52 H38 109.5 . . ? H37 C52 H38 109.5 . . ? C49 C53 H39 109.5 . . ? C49 C53 H40 109.5 . . ? H39 C53 H40 109.5 . . ? C49 C53 H41 109.5 . . ? H39 C53 H41 109.5 . . ? H40 C53 H41 109.5 . . ? C51 C54 H42 109.5 . . ? C51 C54 H43 109.5 . . ? H42 C54 H43 109.5 . . ? C51 C54 H44 109.5 . . ? H42 C54 H44 109.5 . . ? H43 C54 H44 109.5 . . ? C1 N1 C4 107.5(3) . . ? C1 N1 B1 127.7(3) . . ? C4 N1 B1 124.7(3) . . ? C9 N2 C6 106.8(3) . . ? C9 N2 B1 127.1(3) . . ? C6 N2 B1 125.7(3) . . ? C10 N3 C13 106.5(3) . . ? C10 N3 B2 127.2(3) . . ? C13 N3 B2 126.3(3) . . ? C18 N4 C15 107.8(4) . . ? C18 N4 B2 126.3(4) . . ? C15 N4 B2 125.8(3) . . ? C9 N5 C11 111.3(3) . . ? C10 N6 C8 111.0(3) . . ? C19 N7 C22 108.2(3) . . ? C19 N7 B3 125.1(4) . . ? C22 N7 B3 126.6(3) . . ? C27 N8 C24 107.7(4) . . ? C27 N8 B3 127.1(4) . . ? C24 N8 B3 125.1(3) . . ? C1 N9 C20 126.1(3) . . ? C1 N9 H45 117.0 . . ? C20 N9 H45 117.0 . . ? F1 B1 F2 108.6(3) . . ? F1 B1 N2 111.3(3) . . ? F2 B1 N2 112.5(3) . . ? F1 B1 N1 109.4(3) . . ? F2 B1 N1 108.8(3) . . ? N2 B1 N1 106.1(3) . . ? F3 B2 F4 109.2(4) . . ? F3 B2 N3 112.9(3) . . ? F4 B2 N3 110.8(3) . . ? F3 B2 N4 109.2(3) . . ? F4 B2 N4 109.6(3) . . ? N3 B2 N4 105.1(3) . . ? F5 B3 F6 111.0(4) . . ? F5 B3 N8 111.0(3) . . ? F6 B3 N8 110.5(4) . . ? F5 B3 N7 109.2(4) . . ? F6 B3 N7 108.9(3) . . ? N8 B3 N7 106.1(4) . . ? Cl3 C55 Cl1 110.2(4) . . ? Cl3 C55 Cl2 109.2(3) . . ? Cl1 C55 Cl2 111.6(4) . . ? Cl3 C55 H46 108.6 . . ? Cl1 C55 H46 108.6 . . ? Cl2 C55 H46 108.6 . . ? Cl6 C56 Cl4 116(3) . . ? Cl6 C56 Cl5 116(2) . . ? Cl4 C56 Cl5 114(2) . . ? Cl6 C56 H47 102.7 . . ? Cl4 C56 H47 102.7 . . ? Cl5 C56 H47 102.7 . . ? Cl7 C57 Cl8 109.1(15) . . ? Cl7 C57 Cl9 107.1(17) . . ? Cl8 C57 Cl9 93.8(18) . . ? Cl7 C57 H48 114.9 . . ? Cl8 C57 H48 114.9 . . ? Cl9 C57 H48 114.9 . . ? Cl11 C58 Cl10 103.4(18) . . ? Cl11 C58 Cl12 105.8(19) . . ? Cl10 C58 Cl12 112(2) . . ? Cl11 C58 H49 111.8 . . ? Cl10 C58 H49 111.8 . . ? Cl12 C58 H49 111.8 . . ? Cl13 C59 Cl15 109.4(11) . . ? Cl13 C59 Cl14 103.1(9) . . ? Cl15 C59 Cl14 108.3(10) . . ? Cl13 C59 H50 111.9 . . ? Cl15 C59 H50 111.9 . . ? Cl14 C59 H50 111.9 . . ? Cl18 C60 Cl17 113.0(9) . . ? Cl18 C60 Cl16 111.8(8) . . ? Cl17 C60 Cl16 109.0(10) . . ? Cl18 C60 H51 107.6 . . ? Cl17 C60 H51 107.6 . . ? Cl16 C60 H51 107.6 . . ? Cl20 C61 Cl19 117.9(7) . . ? Cl20 C61 Cl21 110.2(6) . . ? Cl19 C61 Cl21 107.2(5) . . ? Cl20 C61 H52 107.0 . . ? Cl19 C61 H52 107.0 . . ? Cl21 C61 H52 107.0 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.805 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 971649' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_I _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C80.12 H67.72 B3 Cl1.09 F6 N15.52 O6.25' _chemical_formula_iupac ? _chemical_formula_weight 1533.00 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.6707(6) _cell_length_b 17.1450(7) _cell_length_c 18.0545(10) _cell_angle_alpha 118.3350(17) _cell_angle_beta 96.657(3) _cell_angle_gamma 90.695(2) _cell_volume 3958.5(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9986 _cell_measurement_theta_min 2.2742 _cell_measurement_theta_max 25.0313 _cell_measurement_temperature 90.(2) _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.160 _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1589 _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.98 _exptl_special_details ; ; _diffrn_ambient_temperature 90.(2) _diffrn_source ? _diffrn_source_type ? _diffrn_radiation_type Mo _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 10.4167 _diffrn_reflns_number 24961 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.946 _diffrn_measured_fraction_theta_full 0.946 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _refine_special_details ; ; _reflns_number_total 13197 _reflns_number_gt 9709 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0871 _refine_ls_wR_factor_gt 0.2442 _refine_ls_wR_factor_ref 0.2809 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_number_reflns 13197 _refine_ls_number_parameters 1082 _refine_ls_number_restraints 36 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1529P)^2^+8.6441P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.082 _refine_ls_shift/su_mean 0.004 _refine_diff_density_max 1.217 _refine_diff_density_min -0.734 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'APEX 2' _computing_cell_refinement 'SAINT V8.32B (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group B B1 0.1833(3) 0.7442(3) 0.8052(3) 0.0356(10) Uani d . . . 1.0 . . B B2 -0.2781(4) 0.6490(4) 0.5081(4) 0.0568(14) Uani d . . . 1.0 . . B B3 0.6777(3) 0.9600(3) 1.0617(3) 0.0427(12) Uani d . . . 1.0 . . C C1 0.3239(2) 0.7202(2) 0.8929(2) 0.0291(8) Uani d . . . 1.0 . . C C2 0.3514(3) 0.6569(2) 0.9224(2) 0.0309(8) Uani d . . . 1.0 . . C C3 0.2793(3) 0.5938(2) 0.8923(2) 0.0315(8) Uani d . . . 1.0 . . H H3 0.2768 0.5432 0.9006 0.038 Uiso calc U . R 1.0 . . C C4 0.2086(3) 0.6162(2) 0.8463(2) 0.0301(8) Uani d . . . 1.0 . . C C5 0.1227(3) 0.5739(2) 0.8059(2) 0.0311(8) Uani d . . . 1.0 . . C C6 0.0630(3) 0.6112(3) 0.7636(2) 0.0323(8) Uani d . . . 1.0 . . C C7 -0.0213(3) 0.5758(3) 0.7144(3) 0.0362(9) Uani d . . . 1.0 . . H H7 -0.0525 0.521 0.7014 0.043 Uiso calc U . R 1.0 . . C C8 -0.0522(3) 0.6364(3) 0.6871(3) 0.0350(9) Uani d . . . 1.0 . . C C9 0.0171(3) 0.7108(2) 0.7245(2) 0.0326(8) Uani d . . . 1.0 . . C C10 -0.1313(3) 0.7037(3) 0.6248(3) 0.0357(9) Uani d . . . 1.0 . . C C11 -0.0647(3) 0.7803(3) 0.6657(2) 0.0338(9) Uani d . . . 1.0 . . C C012 0.4677(3) 0.8112(2) 0.9291(2) 0.0307(8) Uani d . . . 1.0 . . C C12 -0.0951(3) 0.8413(3) 0.6390(3) 0.0366(9) Uani d . . . 1.0 . . H H12 -0.0662 0.8981 0.6555 0.044 Uiso calc U . R 1.0 . . C C013 0.9256(3) 0.9084(3) 1.0412(3) 0.0364(9) Uani d . . . 1.0 . . C C13 -0.1769(3) 0.8018(3) 0.5830(2) 0.0354(9) Uani d . . . 1.0 . . C C14 -0.2319(3) 0.8361(3) 0.5358(2) 0.0356(9) Uani d . . . 1.0 . . C C15 -0.3053(3) 0.7843(3) 0.4767(3) 0.0380(9) Uani d . . . 1.0 . . C C016 0.6196(3) 0.7992(2) 0.9403(2) 0.0315(8) Uani d . . . 1.0 . . C C16 -0.3681(3) 0.8026(3) 0.4214(3) 0.0409(10) Uani d . . . 1.0 . . H H16 -0.3694 0.8568 0.4191 0.049 Uiso calc U . R 1.0 . . C C17 -0.4268(3) 0.7270(3) 0.3716(3) 0.0416(10) Uani d . . . 1.0 . . C C18 -0.3986(3) 0.6635(3) 0.3989(3) 0.0438(10) Uani d . . . 1.0 . . H H18 -0.4268 0.605 0.3757 0.053 Uiso calc U . R 1.0 . . C C19 0.0892(2) 0.4940(2) 0.8105(2) 0.0302(8) Uani d . . . 1.0 . . C C20 0.0321(3) 0.5062(3) 0.8715(2) 0.0327(8) Uani d . . . 1.0 . . C C21 -0.0022(3) 0.4324(3) 0.8759(3) 0.0339(9) Uani d . . . 1.0 . . H H21 -0.0419 0.4407 0.9166 0.041 Uiso calc U . R 1.0 . . C C22 0.0207(3) 0.3469(3) 0.8219(3) 0.0350(9) Uani d . . . 1.0 . . C C23 0.0798(3) 0.3371(3) 0.7635(3) 0.0387(9) Uani d . . . 1.0 . . H H23 0.0979 0.2795 0.728 0.046 Uiso calc U . R 1.0 . . C C24 0.1136(3) 0.4085(3) 0.7550(3) 0.0353(9) Uani d . . . 1.0 . . C C25 0.0100(3) 0.5984(3) 0.9338(3) 0.0396(9) Uani d . . . 1.0 . . H H25A -0.0323 0.5943 0.9703 0.059 Uiso calc U . R 1.0 . . H H25B -0.0189 0.6275 0.9027 0.059 Uiso calc U . R 1.0 . . H H25C 0.0669 0.6332 0.9689 0.059 Uiso calc U . R 1.0 . . C C26 -0.0153(3) 0.2676(3) 0.8280(3) 0.0433(10) Uani d . . . 1.0 . . H H26A 0.0243 0.2617 0.8725 0.065 Uiso calc U . R 1.0 . . H H26B -0.0152 0.2137 0.7734 0.065 Uiso calc U . R 1.0 . . H H26C -0.0782 0.2758 0.8422 0.065 Uiso calc U . R 1.0 . . C C27 0.1749(3) 0.3930(3) 0.6885(3) 0.0462(11) Uani d . . . 1.0 . . H H27A 0.2095 0.341 0.6778 0.069 Uiso calc U . R 1.0 . . H H27B 0.218 0.4454 0.7086 0.069 Uiso calc U . R 1.0 . . H H27C 0.1371 0.3827 0.6357 0.069 Uiso calc U . R 1.0 . . C C28 0.7274(3) 0.6804(3) 0.8702(3) 0.0371(9) Uani d . . . 1.0 . . C C29 0.7626(3) 0.6253(3) 0.9026(3) 0.0374(9) Uani d . . . 1.0 . . C C30 0.7803(3) 0.5388(3) 0.8444(3) 0.0425(10) Uani d . . . 1.0 . . H H30 0.8047 0.501 0.8656 0.051 Uiso calc U . R 1.0 . . C C31 0.7637(3) 0.5062(3) 0.7576(3) 0.0449(11) Uani d . . . 1.0 . . C C32 0.7288(3) 0.5621(3) 0.7279(3) 0.0466(11) Uani d . . . 1.0 . . H H32 0.7172 0.5404 0.6683 0.056 Uiso calc U . R 1.0 . . C C33 0.7098(3) 0.6492(3) 0.7818(3) 0.0395(10) Uani d . . . 1.0 . . C C34 0.7808(3) 0.6567(3) 0.9969(3) 0.0415(10) Uani d . . . 1.0 . . H H34A 0.8402 0.6917 1.0205 0.062 Uiso calc U . R 1.0 . . H H34B 0.782 0.6051 1.0067 0.062 Uiso calc U . R 1.0 . . H H34C 0.7318 0.6935 1.0247 0.062 Uiso calc U . R 1.0 . . C C35 0.7841(4) 0.4123(3) 0.6980(4) 0.0624(14) Uani d . . . 1.0 . . H H35A 0.8417 0.3984 0.721 0.094 Uiso calc U . R 1.0 . . H H35B 0.7903 0.4068 0.6423 0.094 Uiso calc U . R 1.0 . . H H35C 0.7337 0.3708 0.692 0.094 Uiso calc U . R 1.0 . . C C36 0.6756(4) 0.7077(3) 0.7456(3) 0.0530(12) Uani d . . . 1.0 . . H H36A 0.6841 0.6803 0.6855 0.079 Uiso calc U . R 1.0 . . H H36B 0.7103 0.7659 0.7768 0.079 Uiso calc U . R 1.0 . . H H36C 0.6101 0.715 0.7506 0.079 Uiso calc U . R 1.0 . . C C37 -0.2064(3) 0.9281(3) 0.5517(3) 0.0364(9) Uani d . . . 1.0 . . C C38 -0.2332(3) 1.0024(3) 0.6233(3) 0.0492(11) Uani d . . . 1.0 . . C C39 -0.2061(4) 1.0863(3) 0.6369(3) 0.0548(13) Uani d . . . 1.0 . . H H39 -0.2236 1.1363 0.6849 0.066 Uiso calc U . R 1.0 . . C C40 -0.1552(3) 1.1018(3) 0.5847(3) 0.0502(12) Uani d . . . 1.0 . . C C41 -0.1289(3) 1.0271(3) 0.5150(3) 0.0452(10) Uani d . . . 1.0 . . H H41 -0.093 1.0355 0.4784 0.054 Uiso calc U . R 1.0 . . C C42 -0.1540(3) 0.9409(3) 0.4980(3) 0.0389(9) Uani d . . . 1.0 . . C C43 -0.2907(5) 0.9899(4) 0.6806(4) 0.0714(16) Uani d . . . 1.0 . . H H43A -0.2857 1.0448 0.735 0.107 Uiso calc U . R 1.0 . . H H43B -0.2688 0.9413 0.6904 0.107 Uiso calc U . R 1.0 . . H H43C -0.3551 0.9754 0.6541 0.107 Uiso calc U . R 1.0 . . C C44 -0.1293(4) 1.1942(3) 0.5999(4) 0.0679(16) Uani d . . . 1.0 . . H H44A -0.1834 1.2182 0.5831 0.102 Uiso calc U . R 1.0 . . H H44B -0.0807 1.1918 0.5661 0.102 Uiso calc U . R 1.0 . . H H44C -0.107 1.2326 0.6603 0.102 Uiso calc U . R 1.0 . . C C45 -0.1249(3) 0.8625(3) 0.4210(3) 0.0477(11) Uani d . . . 1.0 . . H H45A -0.095 0.8218 0.4384 0.072 Uiso calc U . R 1.0 . . H H45B -0.0817 0.8838 0.3959 0.072 Uiso calc U . R 1.0 . . H H45C -0.1792 0.8312 0.3791 0.072 Uiso calc U . R 1.0 . . C C46 0.4335(2) 0.6659(3) 0.9823(2) 0.0315(8) Uani d . . . 1.0 . . C C47 0.4601(3) 0.7470(3) 1.0571(3) 0.0361(9) Uani d . . . 1.0 . . H H47 0.4267 0.7976 1.0678 0.043 Uiso calc U . R 1.0 . . C C48 0.5339(3) 0.7534(3) 1.1149(3) 0.0370(9) Uani d . . . 1.0 . . H H48 0.5521 0.8082 1.165 0.044 Uiso calc U . R 1.0 . . C C49 0.5810(3) 0.6790(3) 1.0988(3) 0.0359(9) Uani d . . . 1.0 . . C C50 0.5581(3) 0.5990(3) 1.0258(3) 0.0374(9) Uani d . . . 1.0 . . H H50 0.5921 0.5489 1.0159 0.045 Uiso calc U . R 1.0 . . C C51 0.4844(3) 0.5928(3) 0.9670(3) 0.0338(9) Uani d . . . 1.0 . . H H51 0.4685 0.5383 0.916 0.041 Uiso calc U . R 1.0 . . C C52 1.0254(3) 0.9325(3) 1.0657(3) 0.0341(9) Uani d . . . 1.0 . . C C53 1.0601(3) 1.0205(3) 1.1101(3) 0.0408(10) Uani d . . . 1.0 . . H H53 1.0189 1.0662 1.1272 0.049 Uiso calc U . R 1.0 . . C C54 1.1537(3) 1.0428(3) 1.1300(3) 0.0432(10) Uani d . . . 1.0 . . H H54 1.1769 1.1034 1.1598 0.052 Uiso calc U . R 1.0 . . C C55 1.2134(3) 0.9756(3) 1.1058(3) 0.0361(9) Uani d . . . 1.0 . . C C56 1.1811(3) 0.8872(3) 1.0634(3) 0.0461(11) Uani d . . . 1.0 . . H H56 1.2227 0.8417 1.0485 0.055 Uiso calc U . R 1.0 . . C C57 1.0873(3) 0.8660(3) 1.0429(3) 0.0470(11) Uani d . . . 1.0 . . H H57 1.0644 0.8053 1.013 0.056 Uiso calc U . R 1.0 . . C C58 -0.5026(3) 0.7101(3) 0.3038(3) 0.0430(10) Uani d . . . 1.0 . . C C59 -0.5443(3) 0.7802(3) 0.2983(3) 0.0485(11) Uani d . . . 1.0 . . H H59 -0.5233 0.8397 0.3389 0.058 Uiso calc U . R 1.0 . . C C60 -0.6166(3) 0.7642(3) 0.2339(3) 0.0507(12) Uani d . . . 1.0 . . H H60 -0.6444 0.812 0.2299 0.061 Uiso calc U . R 1.0 . . C C61 -0.6466(3) 0.6774(3) 0.1763(3) 0.0439(10) Uani d . . . 1.0 . . C C62 -0.6071(3) 0.6064(3) 0.1797(3) 0.0454(10) Uani d . . . 1.0 . . H H62 -0.6288 0.5472 0.1387 0.054 Uiso calc U . R 1.0 . . C C63 -0.5354(3) 0.6223(3) 0.2434(3) 0.0448(10) Uani d . . . 1.0 . . H H63 -0.5082 0.5737 0.2465 0.054 Uiso calc U . R 1.0 . . C C01A 0.5119(3) 0.8925(3) 0.9928(3) 0.0332(8) Uani d . . . 1.0 . . H H01A 0.482 0.9441 1.026 0.04 Uiso calc U . R 1.0 . . C C01B 0.7849(3) 0.8356(2) 0.9794(3) 0.0350(9) Uani d . . . 1.0 . . C C01D 0.7107(3) 0.7740(2) 0.9310(3) 0.0342(9) Uani d . . . 1.0 . . C C01G 0.5347(3) 0.7525(2) 0.8961(3) 0.0316(8) Uani d . . . 1.0 . . H H01G 0.5249 0.6925 0.8523 0.038 Uiso calc U . R 1.0 . . C C01I 0.8551(3) 0.9660(3) 1.0755(3) 0.0367(9) Uani d . . . 1.0 . . H H01I 0.8655 1.0265 1.1182 0.044 Uiso calc U . R 1.0 . . C C01Q 0.8806(3) 0.8270(3) 0.9808(3) 0.0387(9) Uani d . . . 1.0 . . H H01Q 0.9093 0.7748 0.9465 0.046 Uiso calc U . R 1.0 . . C C3S 0.5456(10) 0.1342(10) 0.2550(8) 0.063(3) Uani d U P . 0.515(10) A 1 H H3S1 0.5896 0.1778 0.2553 0.094 Uiso calc U P . 0.5152 A 1 H H3S2 0.497 0.1153 0.2065 0.094 Uiso calc U P . 0.5152 A 1 H H3S3 0.5776 0.0825 0.2503 0.094 Uiso calc U P . 0.5152 A 1 C C4S 0.5053(8) 0.1739(8) 0.3330(8) 0.064(3) Uani d U P . 0.515(10) A 1 N N1S 0.4735(8) 0.1982(7) 0.3920(7) 0.085(4) Uani d U P . 0.515(10) A 1 C C6S 0.5922(10) 0.0841(11) 0.4825(8) 0.085(4) Uani d . P . 0.515(10) A 1 H H6S1 0.6504 0.0787 0.5118 0.127 Uiso calc U P . 0.5152 A 1 H H6S2 0.5412 0.0797 0.5112 0.127 Uiso calc U P . 0.5152 A 1 H H6S3 0.5941 0.1418 0.4835 0.127 Uiso calc U P . 0.5152 A 1 C C7S 0.5793(17) 0.0158(13) 0.3980(16) 0.143(9) Uani d . P . 0.515(10) A 1 N N2S 0.5957(17) -0.0268(9) 0.3328(10) 0.123(7) Uani d . P . 0.515(10) A 1 C C1S 0.1723(8) 0.8663(7) 0.6406(9) 0.064(3) Uani d . P . 0.544(5) B 1 H H1S1 0.1161 0.8537 0.5994 0.077 Uiso calc U P R 0.544(5) B 1 H H1S2 0.157 0.8484 0.6827 0.077 Uiso calc U P R 0.544(5) B 1 C C2S 0.1932(10) 0.9459(18) 0.6772(9) 0.147(9) Uani d . P . 0.544(5) B 1 H H2S1 0.22 0.9604 0.637 0.177 Uiso calc U P R 0.544(5) B 1 H H2S2 0.2429 0.9583 0.7243 0.177 Uiso calc U P R 0.544(5) B 1 Cl Cl1S 0.2545(2) 0.8037(2) 0.5886(2) 0.0836(11) Uani d . P . 0.544(5) B 1 Cl Cl2S 0.0966(3) 1.0314(2) 0.7262(2) 0.0861(12) Uani d . P . 0.544(5) B 1 F F1 0.22921(17) 0.7403(2) 0.73998(18) 0.0546(7) Uani d . . . 1.0 . . F F2 0.17862(18) 0.83120(15) 0.86423(18) 0.0548(7) Uani d . . . 1.0 . . F F3 -0.3427(2) 0.6273(3) 0.5472(2) 0.0796(10) Uani d . . . 1.0 . . F F4 -0.2451(3) 0.5710(2) 0.4511(2) 0.0744(9) Uani d . . . 1.0 . . F F5 0.66876(18) 0.9825(2) 1.14444(18) 0.0699(9) Uani d . . . 1.0 . . F F6 0.66731(17) 1.03352(16) 1.0485(2) 0.0659(9) Uani d . . . 1.0 . . N N1 0.2389(2) 0.6954(2) 0.8484(2) 0.0315(7) Uani d . . . 1.0 . . N N2 0.0882(2) 0.6925(2) 0.7699(2) 0.0328(7) Uani d . . . 1.0 . . N N3 0.0129(2) 0.7838(2) 0.7166(2) 0.0347(7) Uani d . . . 1.0 . . N N4 -0.1285(2) 0.6319(2) 0.6344(2) 0.0376(8) Uani d . . . 1.0 . . N N5 -0.1994(2) 0.7181(2) 0.5741(2) 0.0377(8) Uani d . . . 1.0 . . N N6 -0.3279(2) 0.6976(2) 0.4609(2) 0.0405(8) Uani d . . . 1.0 . . N N7 0.6037(2) 0.8854(2) 0.9992(2) 0.0339(7) Uani d . . . 1.0 . . N N8 0.7722(2) 0.9231(2) 1.0392(2) 0.0365(8) Uani d . . . 1.0 . . N N9 0.6562(2) 0.6836(3) 1.1632(2) 0.0446(9) Uani d . . . 1.0 . . N N10 -0.7224(3) 0.6605(3) 0.1087(3) 0.0489(10) Uani d . . . 1.0 . . N N11 1.3127(2) 0.9982(2) 1.1265(2) 0.0427(9) Uani d . . . 1.0 . . N N12 0.3708(2) 0.7944(2) 0.9066(2) 0.0324(7) Uani d . . . 1.0 . . H H12A 0.3395 0.8354 0.9014 0.039 Uiso calc U . R 1.0 . . O O1 0.6849(2) 0.7573(2) 1.2223(2) 0.0617(10) Uani d . . . 1.0 . . O O2 0.6852(2) 0.6143(2) 1.1551(2) 0.0583(9) Uani d . . . 1.0 . . O O3 -0.7475(2) 0.5825(3) 0.0561(2) 0.0611(9) Uani d . . . 1.0 . . O O4 -0.7575(2) 0.7243(3) 0.1068(2) 0.0609(9) Uani d . . . 1.0 . . O O5 1.3412(2) 1.0748(2) 1.1506(3) 0.0669(11) Uani d . . . 1.0 . . O O6 1.3640(2) 0.9394(2) 1.1195(2) 0.0504(8) Uani d . . . 1.0 . . C C10S 0.1217(6) 0.5766(5) 0.5408(5) 0.101(2) Uani d . . . 1.0 C 1 H H10A 0.1541 0.5322 0.4967 0.151 Uiso calc U . . 1.0 D 1 H H10B 0.0835 0.5469 0.5626 0.151 Uiso calc U . . 1.0 E 1 H H10C 0.1667 0.6199 0.5874 0.151 Uiso calc U . . 1.0 F 1 C C11S 0.0590(6) 0.6257(5) 0.5022(5) 0.073(2) Uani d . . . 1.0 C 1 N N5S 0.0246(6) 0.6553(7) 0.4806(5) 0.110(3) Uani d . . . 1.0 C 1 N N6S 0.4374(6) 0.5662(4) 0.7211(5) 0.107(2) Uani d . . . 1.0 G 1 C C8S 0.4191(9) 0.5826(6) 0.6704(8) 0.130(4) Uani d . . . 1.0 G 1 C C9S 0.3981(15) 0.6048(9) 0.5983(11) 0.247(11) Uani d . . . 1.0 G 1 H H9S1 0.3782 0.6653 0.6208 0.371 Uiso calc U . . 1.0 H 1 H H9S2 0.3489 0.5626 0.556 0.371 Uiso calc U . . 1.0 I 1 H H9S3 0.4535 0.6007 0.5715 0.371 Uiso calc U . . 1.0 J 1 C C12S 0.5339(18) 0.061(2) 0.281(2) 0.166(9) Uani d U P . 0.485(10) A 4 N N7S 0.5422(18) -0.007(2) 0.301(2) 0.180(9) Uani d U P . 0.485(10) A 4 C C13S 0.554(3) 0.165(3) 0.272(3) 0.197(13) Uani d U P . 0.485(10) A 4 H H13A 0.6135 0.1652 0.2535 0.295 Uiso calc U P . 0.4848 A 4 H H13B 0.5524 0.2169 0.3279 0.295 Uiso calc U P . 0.4848 A 4 H H13C 0.505 0.1663 0.231 0.295 Uiso calc U P . 0.4848 A 4 O O1W 0.5 0 0.5 0.124(10) Uani d . . S 0.50(2) K 6 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 B1 0.033(2) 0.036(2) 0.037(2) -0.0028(19) -0.007(2) 0.019(2) B2 0.053(3) 0.068(4) 0.054(3) 0.006(3) 0.008(3) 0.032(3) B3 0.026(2) 0.029(2) 0.054(3) 0.0036(18) -0.005(2) 0.006(2) C1 0.0252(19) 0.0283(18) 0.0296(19) -0.0025(15) -0.0008(15) 0.0117(16) C2 0.0244(19) 0.035(2) 0.033(2) 0.0033(15) 0.0005(16) 0.0164(17) C3 0.0264(19) 0.033(2) 0.035(2) 0.0002(15) -0.0018(16) 0.0173(17) C4 0.0276(19) 0.0276(19) 0.032(2) -0.0006(15) 0.0001(16) 0.0130(16) C5 0.0256(19) 0.0298(19) 0.033(2) 0.0008(15) 0.0005(16) 0.0122(16) C6 0.028(2) 0.034(2) 0.033(2) -0.0003(15) 0.0004(16) 0.0153(17) C7 0.030(2) 0.038(2) 0.040(2) -0.0055(16) -0.0043(17) 0.0201(18) C8 0.027(2) 0.042(2) 0.036(2) -0.0011(16) -0.0024(17) 0.0196(18) C9 0.029(2) 0.031(2) 0.032(2) 0.0040(15) -0.0015(16) 0.0124(17) C10 0.029(2) 0.042(2) 0.034(2) 0.0020(17) -0.0013(17) 0.0183(18) C11 0.033(2) 0.033(2) 0.030(2) 0.0055(16) -0.0008(17) 0.0116(17) C012 0.0253(19) 0.0302(19) 0.034(2) 0.0000(15) -0.0020(16) 0.0151(17) C12 0.034(2) 0.035(2) 0.035(2) 0.0051(17) -0.0022(18) 0.0138(18) C013 0.026(2) 0.033(2) 0.046(2) 0.0011(16) 0.0003(18) 0.0172(18) C13 0.034(2) 0.039(2) 0.032(2) 0.0104(17) 0.0032(17) 0.0162(18) C14 0.030(2) 0.041(2) 0.029(2) 0.0054(17) 0.0006(17) 0.0112(17) C15 0.034(2) 0.042(2) 0.035(2) 0.0070(17) 0.0028(18) 0.0165(18) C016 0.0271(19) 0.0263(18) 0.037(2) 0.0013(15) 0.0029(16) 0.0123(16) C16 0.038(2) 0.046(2) 0.037(2) 0.0105(19) 0.0022(19) 0.019(2) C17 0.034(2) 0.054(3) 0.034(2) 0.0060(19) -0.0007(18) 0.019(2) C18 0.035(2) 0.052(3) 0.041(2) -0.0017(19) -0.005(2) 0.021(2) C19 0.0229(18) 0.033(2) 0.033(2) -0.0005(15) -0.0054(16) 0.0165(17) C20 0.0261(19) 0.035(2) 0.033(2) 0.0027(15) -0.0045(16) 0.0148(17) C21 0.0254(19) 0.037(2) 0.038(2) 0.0002(16) 0.0001(17) 0.0180(18) C22 0.028(2) 0.038(2) 0.033(2) -0.0045(16) -0.0062(16) 0.0138(18) C23 0.039(2) 0.031(2) 0.035(2) -0.0010(17) 0.0013(18) 0.0082(17) C24 0.031(2) 0.037(2) 0.034(2) -0.0013(16) -0.0006(17) 0.0144(18) C25 0.040(2) 0.037(2) 0.041(2) 0.0071(18) 0.0067(19) 0.0185(19) C26 0.045(2) 0.037(2) 0.043(2) -0.0046(18) 0.003(2) 0.017(2) C27 0.053(3) 0.038(2) 0.042(2) 0.000(2) 0.012(2) 0.013(2) C28 0.0221(19) 0.030(2) 0.051(3) -0.0007(15) 0.0061(18) 0.0127(18) C29 0.0254(19) 0.030(2) 0.049(2) -0.0011(15) 0.0040(18) 0.0126(18) C30 0.031(2) 0.031(2) 0.062(3) 0.0041(17) 0.010(2) 0.019(2) C31 0.038(2) 0.029(2) 0.052(3) -0.0012(17) 0.014(2) 0.006(2) C32 0.041(2) 0.045(2) 0.044(2) 0.0004(19) 0.012(2) 0.013(2) C33 0.030(2) 0.035(2) 0.044(2) 0.0005(16) 0.0057(18) 0.0118(19) C34 0.033(2) 0.036(2) 0.053(3) 0.0037(17) 0.0029(19) 0.020(2) C35 0.057(3) 0.036(2) 0.073(4) 0.000(2) 0.020(3) 0.007(2) C36 0.055(3) 0.054(3) 0.050(3) 0.009(2) 0.014(2) 0.023(2) C37 0.033(2) 0.036(2) 0.036(2) 0.0085(17) -0.0022(18) 0.0151(18) C38 0.052(3) 0.046(3) 0.046(3) 0.016(2) 0.007(2) 0.019(2) C39 0.054(3) 0.043(3) 0.052(3) 0.017(2) 0.005(2) 0.010(2) C40 0.045(3) 0.038(2) 0.057(3) 0.011(2) -0.007(2) 0.016(2) C41 0.042(2) 0.040(2) 0.048(3) 0.0031(19) -0.003(2) 0.018(2) C42 0.041(2) 0.033(2) 0.036(2) 0.0075(17) -0.0025(18) 0.0123(18) C43 0.088(4) 0.065(3) 0.059(3) 0.026(3) 0.033(3) 0.023(3) C44 0.068(4) 0.036(3) 0.084(4) 0.011(2) -0.004(3) 0.020(3) C45 0.053(3) 0.038(2) 0.042(2) 0.000(2) 0.011(2) 0.010(2) C46 0.0225(18) 0.037(2) 0.035(2) -0.0006(15) -0.0021(16) 0.0191(17) C47 0.030(2) 0.039(2) 0.039(2) 0.0019(17) 0.0010(18) 0.0192(19) C48 0.030(2) 0.038(2) 0.036(2) -0.0036(17) -0.0028(18) 0.0144(18) C49 0.0251(19) 0.049(2) 0.036(2) 0.0001(17) -0.0036(17) 0.0238(19) C50 0.031(2) 0.037(2) 0.045(2) 0.0034(17) 0.0010(18) 0.0217(19) C51 0.028(2) 0.034(2) 0.037(2) 0.0012(16) -0.0027(17) 0.0165(17) C52 0.026(2) 0.032(2) 0.042(2) 0.0028(15) 0.0023(17) 0.0164(18) C53 0.029(2) 0.033(2) 0.051(3) 0.0046(16) 0.0012(19) 0.0140(19) C54 0.036(2) 0.029(2) 0.055(3) -0.0005(17) 0.002(2) 0.0127(19) C55 0.026(2) 0.037(2) 0.043(2) 0.0011(16) 0.0019(17) 0.0173(18) C56 0.034(2) 0.032(2) 0.061(3) 0.0089(17) 0.009(2) 0.012(2) C57 0.029(2) 0.029(2) 0.069(3) 0.0008(17) 0.002(2) 0.014(2) C58 0.031(2) 0.058(3) 0.039(2) 0.0054(19) 0.0018(18) 0.023(2) C59 0.045(3) 0.055(3) 0.041(2) 0.009(2) 0.000(2) 0.020(2) C60 0.046(3) 0.066(3) 0.047(3) 0.019(2) 0.009(2) 0.032(2) C61 0.029(2) 0.068(3) 0.038(2) 0.001(2) -0.0008(18) 0.029(2) C62 0.033(2) 0.058(3) 0.045(3) -0.0032(19) -0.001(2) 0.026(2) C63 0.034(2) 0.060(3) 0.042(2) 0.005(2) -0.0011(19) 0.027(2) C01A 0.0267(19) 0.031(2) 0.038(2) 0.0018(15) -0.0019(17) 0.0149(17) C01B 0.027(2) 0.0241(19) 0.046(2) 0.0031(15) 0.0002(17) 0.0114(17) C01D 0.031(2) 0.0270(19) 0.041(2) 0.0024(15) 0.0022(17) 0.0141(17) C01G 0.029(2) 0.0258(18) 0.036(2) -0.0015(15) -0.0011(16) 0.0130(16) C01I 0.027(2) 0.0257(19) 0.049(2) 0.0013(15) -0.0036(18) 0.0134(18) C01Q 0.031(2) 0.029(2) 0.051(3) 0.0047(16) 0.0048(19) 0.0150(19) C3S 0.048(6) 0.085(8) 0.047(6) 0.017(5) 0.002(5) 0.026(5) C4S 0.058(6) 0.071(6) 0.064(6) 0.010(5) 0.014(5) 0.032(5) N1S 0.088(7) 0.087(7) 0.084(7) 0.024(6) 0.035(6) 0.039(6) C6S 0.085(9) 0.128(12) 0.062(7) 0.043(8) 0.018(6) 0.060(8) C7S 0.20(2) 0.090(12) 0.132(18) 0.067(14) -0.008(16) 0.054(13) N2S 0.25(2) 0.056(7) 0.074(8) 0.056(10) 0.050(11) 0.035(6) C1S 0.060(7) 0.058(6) 0.092(8) -0.004(5) 0.026(6) 0.047(6) C2S 0.054(8) 0.31(3) 0.052(8) 0.003(13) -0.017(6) 0.076(13) Cl1S 0.0679(19) 0.113(3) 0.0755(19) -0.0003(16) -0.0135(14) 0.0545(18) Cl2S 0.107(3) 0.090(2) 0.0711(19) -0.0063(17) 0.0070(17) 0.0483(17) F1 0.0351(14) 0.0817(19) 0.0638(17) -0.0056(13) -0.0054(12) 0.0512(16) F2 0.0525(16) 0.0290(13) 0.0662(17) 0.0002(11) -0.0256(14) 0.0168(12) F3 0.062(2) 0.115(3) 0.070(2) -0.0148(19) -0.0046(16) 0.054(2) F4 0.088(2) 0.0637(19) 0.0628(19) 0.0036(17) -0.0062(17) 0.0270(16) F5 0.0313(14) 0.089(2) 0.0446(16) 0.0072(14) -0.0010(12) -0.0025(15) F6 0.0294(13) 0.0281(13) 0.116(3) 0.0012(10) -0.0139(14) 0.0204(14) N1 0.0257(16) 0.0297(16) 0.0333(17) 0.0001(13) -0.0036(14) 0.0120(14) N2 0.0288(17) 0.0288(16) 0.0375(18) 0.0016(13) -0.0046(14) 0.0152(14) N3 0.0318(17) 0.0318(17) 0.0348(18) 0.0022(13) -0.0049(15) 0.0133(14) N4 0.0271(17) 0.046(2) 0.0413(19) 0.0001(14) -0.0041(15) 0.0246(17) N5 0.0331(18) 0.0424(19) 0.0407(19) 0.0043(15) -0.0001(15) 0.0235(16) N6 0.0337(19) 0.046(2) 0.042(2) 0.0010(15) -0.0026(16) 0.0227(17) N7 0.0247(16) 0.0306(17) 0.0401(19) 0.0037(13) 0.0004(14) 0.0126(15) N8 0.0247(17) 0.0298(17) 0.047(2) 0.0035(13) -0.0014(15) 0.0133(15) N9 0.0314(19) 0.059(2) 0.046(2) 0.0051(17) -0.0004(17) 0.028(2) N10 0.033(2) 0.075(3) 0.051(2) 0.000(2) 0.0015(18) 0.041(2) N11 0.0315(18) 0.036(2) 0.054(2) -0.0008(15) 0.0061(16) 0.0157(17) N12 0.0263(16) 0.0279(16) 0.0385(18) 0.0009(13) -0.0011(14) 0.0135(14) O1 0.048(2) 0.068(2) 0.0467(19) 0.0040(17) -0.0164(16) 0.0142(18) O2 0.050(2) 0.063(2) 0.064(2) 0.0107(17) -0.0130(17) 0.0364(18) O3 0.052(2) 0.079(3) 0.057(2) -0.0185(18) -0.0145(17) 0.042(2) O4 0.0402(19) 0.085(3) 0.066(2) 0.0127(17) -0.0012(17) 0.045(2) O5 0.0368(18) 0.0415(19) 0.110(3) -0.0038(14) 0.0033(19) 0.028(2) O6 0.0307(16) 0.0435(17) 0.068(2) 0.0060(13) 0.0099(15) 0.0192(16) C10S 0.109(6) 0.091(5) 0.071(4) -0.007(4) 0.016(4) 0.014(4) C11S 0.062(5) 0.063(4) 0.063(5) 0.000(3) 0.016(4) 0.004(3) N5S 0.081(6) 0.139(8) 0.062(4) -0.020(5) 0.005(4) 0.012(4) N6S 0.146(7) 0.063(4) 0.075(4) -0.019(4) -0.010(4) 0.009(3) C8S 0.165(10) 0.068(5) 0.112(8) -0.025(5) -0.030(7) 0.018(5) C9S 0.37(3) 0.140(10) 0.220(15) -0.100(13) -0.152(17) 0.120(11) C12S 0.116(13) 0.202(19) 0.204(17) 0.024(13) 0.047(13) 0.111(15) N7S 0.142(15) 0.19(2) 0.22(2) 0.017(14) 0.061(14) 0.106(17) C13S 0.162(16) 0.218(19) 0.206(18) 0.030(14) 0.041(14) 0.095(14) O1W 0.128(14) 0.080(10) 0.076(10) 0.060(9) -0.030(9) -0.026(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag B1 F2 . 1.370(5) ? B1 F1 . 1.398(6) ? B1 N2 . 1.538(6) ? B1 N1 . 1.570(6) ? B2 F4 . 1.381(7) ? B2 F3 . 1.390(7) ? B2 N5 . 1.570(7) ? B2 N6 . 1.581(7) ? B3 F5 . 1.377(7) ? B3 F6 . 1.396(6) ? B3 N8 . 1.548(6) ? B3 N7 . 1.550(6) ? C1 N12 . 1.339(5) ? C1 N1 . 1.346(5) ? C1 C2 . 1.460(5) ? C2 C3 . 1.365(5) ? C2 C46 . 1.477(5) ? C3 C4 . 1.423(5) ? C3 H3 . 0.95 ? C4 C5 . 1.381(5) ? C4 N1 . 1.404(5) ? C5 C6 . 1.444(6) ? C5 C19 . 1.491(5) ? C6 C7 . 1.380(6) ? C6 N2 . 1.386(5) ? C7 C8 . 1.403(6) ? C7 H7 . 0.95 ? C8 N4 . 1.358(5) ? C8 C9 . 1.452(6) ? C9 N3 . 1.326(5) ? C9 N2 . 1.382(5) ? C10 N4 . 1.323(5) ? C10 N5 . 1.380(5) ? C10 C11 . 1.451(6) ? C11 N3 . 1.359(5) ? C11 C12 . 1.403(6) ? C012 C01G . 1.386(5) ? C012 C01A . 1.403(5) ? C012 N12 . 1.419(5) ? C12 C13 . 1.403(6) ? C12 H12 . 0.95 ? C013 C01Q . 1.393(6) ? C013 C01I . 1.421(5) ? C013 C52 . 1.473(5) ? C13 N5 . 1.397(5) ? C13 C14 . 1.433(6) ? C14 C15 . 1.378(6) ? C14 C37 . 1.497(6) ? C15 N6 . 1.402(5) ? C15 C16 . 1.428(6) ? C016 N7 . 1.394(5) ? C016 C01G . 1.404(5) ? C016 C01D . 1.413(5) ? C16 C17 . 1.385(6) ? C16 H16 . 0.95 ? C17 C18 . 1.440(6) ? C17 C58 . 1.469(6) ? C18 N6 . 1.329(6) ? C18 H18 . 0.95 ? C19 C20 . 1.400(6) ? C19 C24 . 1.408(5) ? C20 C21 . 1.395(6) ? C20 C25 . 1.509(5) ? C21 C22 . 1.394(6) ? C21 H21 . 0.95 ? C22 C23 . 1.392(6) ? C22 C26 . 1.510(6) ? C23 C24 . 1.395(6) ? C23 H23 . 0.95 ? C24 C27 . 1.509(6) ? C25 H25A . 0.98 ? C25 H25B . 0.98 ? C25 H25C . 0.98 ? C26 H26A . 0.98 ? C26 H26B . 0.98 ? C26 H26C . 0.98 ? C27 H27A . 0.98 ? C27 H27B . 0.98 ? C27 H27C . 0.98 ? C28 C29 . 1.403(6) ? C28 C33 . 1.411(6) ? C28 C01D . 1.496(5) ? C29 C30 . 1.401(6) ? C29 C34 . 1.511(6) ? C30 C31 . 1.380(7) ? C30 H30 . 0.95 ? C31 C32 . 1.380(7) ? C31 C35 . 1.511(6) ? C32 C33 . 1.396(6) ? C32 H32 . 0.95 ? C33 C36 . 1.498(7) ? C34 H34A . 0.98 ? C34 H34B . 0.98 ? C34 H34C . 0.98 ? C35 H35A . 0.98 ? C35 H35B . 0.98 ? C35 H35C . 0.98 ? C36 H36A . 0.98 ? C36 H36B . 0.98 ? C36 H36C . 0.98 ? C37 C42 . 1.396(6) ? C37 C38 . 1.420(6) ? C38 C39 . 1.384(7) ? C38 C43 . 1.496(8) ? C39 C40 . 1.383(8) ? C39 H39 . 0.95 ? C40 C41 . 1.403(6) ? C40 C44 . 1.509(7) ? C41 C42 . 1.396(6) ? C41 H41 . 0.95 ? C42 C45 . 1.515(6) ? C43 H43A . 0.98 ? C43 H43B . 0.98 ? C43 H43C . 0.98 ? C44 H44A . 0.98 ? C44 H44B . 0.98 ? C44 H44C . 0.98 ? C45 H45A . 0.98 ? C45 H45B . 0.98 ? C45 H45C . 0.98 ? C46 C51 . 1.396(5) ? C46 C47 . 1.411(6) ? C47 C48 . 1.378(6) ? C47 H47 . 0.95 ? C48 C49 . 1.380(6) ? C48 H48 . 0.95 ? C49 C50 . 1.379(6) ? C49 N9 . 1.479(5) ? C50 C51 . 1.390(6) ? C50 H50 . 0.95 ? C51 H51 . 0.95 ? C52 C53 . 1.384(6) ? C52 C57 . 1.401(6) ? C53 C54 . 1.379(6) ? C53 H53 . 0.95 ? C54 C55 . 1.386(6) ? C54 H54 . 0.95 ? C55 C56 . 1.381(6) ? C55 N11 . 1.460(5) ? C56 C57 . 1.380(6) ? C56 H56 . 0.95 ? C57 H57 . 0.95 ? C58 C59 . 1.395(6) ? C58 C63 . 1.410(7) ? C59 C60 . 1.398(7) ? C59 H59 . 0.95 ? C60 C61 . 1.378(7) ? C60 H60 . 0.95 ? C61 C62 . 1.378(7) ? C61 N10 . 1.468(6) ? C62 C63 . 1.386(6) ? C62 H62 . 0.95 ? C63 H63 . 0.95 ? C01A N7 . 1.351(5) ? C01A H01A . 0.95 ? C01B C01D . 1.393(6) ? C01B N8 . 1.402(5) ? C01B C01Q . 1.412(6) ? C01G H01G . 0.95 ? C01I N8 . 1.336(5) ? C01I H01I . 0.95 ? C01Q H01Q . 0.95 ? C3S C4S . 1.45(2) ? C3S H3S1 . 0.9797 ? C3S H3S2 . 0.9801 ? C3S H3S3 . 0.9802 ? C4S N1S . 1.106(15) ? C6S C7S . 1.40(3) ? C6S H6S1 . 0.98 ? C6S H6S2 . 0.9799 ? C6S H6S3 . 0.9802 ? C7S N2S . 1.11(3) ? C1S C2S . 1.22(2) ? C1S Cl1S . 1.681(11) ? C1S H1S1 . 0.99 ? C1S H1S2 . 0.99 ? C2S Cl2S . 2.01(2) ? C2S H2S1 . 0.99 ? C2S H2S2 . 0.99 ? N9 O2 . 1.214(5) ? N9 O1 . 1.231(5) ? N10 O4 . 1.227(5) ? N10 O3 . 1.236(5) ? N11 O5 . 1.222(5) ? N11 O6 . 1.232(5) ? N12 H12A . 0.88 ? C10S C11S . 1.571(13) ? C10S H10A . 0.98 ? C10S H10B . 0.98 ? C10S H10C . 0.98 ? C11S N5S . 0.902(10) ? N6S C8S . 1.085(12) ? C8S C9S . 1.521(18) ? C9S H9S1 . 0.9802 ? C9S H9S2 . 0.9801 ? C9S H9S3 . 0.9798 ? C12S N7S . 1.39(4) ? C12S C13S . 1.87(5) ? C13S H13A . 0.9804 ? C13S H13B . 0.9801 ? C13S H13C . 0.9796 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag F2 B1 F1 . . 109.5(4) ? F2 B1 N2 . . 112.7(4) ? F1 B1 N2 . . 111.3(3) ? F2 B1 N1 . . 109.3(3) ? F1 B1 N1 . . 108.5(3) ? N2 B1 N1 . . 105.3(3) ? F4 B2 F3 . . 107.9(5) ? F4 B2 N5 . . 112.7(4) ? F3 B2 N5 . . 112.2(4) ? F4 B2 N6 . . 110.9(4) ? F3 B2 N6 . . 107.9(4) ? N5 B2 N6 . . 105.2(4) ? F5 B3 F6 . . 110.6(4) ? F5 B3 N8 . . 111.0(4) ? F6 B3 N8 . . 109.8(4) ? F5 B3 N7 . . 110.6(4) ? F6 B3 N7 . . 108.4(4) ? N8 B3 N7 . . 106.4(3) ? N12 C1 N1 . . 121.5(3) ? N12 C1 C2 . . 128.5(3) ? N1 C1 C2 . . 110.0(3) ? C3 C2 C1 . . 105.5(3) ? C3 C2 C46 . . 126.8(4) ? C1 C2 C46 . . 127.1(3) ? C2 C3 C4 . . 109.0(3) ? C2 C3 H3 . . 125.5 ? C4 C3 H3 . . 125.5 ? C5 C4 N1 . . 121.9(3) ? C5 C4 C3 . . 130.2(3) ? N1 C4 C3 . . 108.0(3) ? C4 C5 C6 . . 119.1(3) ? C4 C5 C19 . . 120.8(3) ? C6 C5 C19 . . 120.0(3) ? C7 C6 N2 . . 111.7(3) ? C7 C6 C5 . . 128.0(4) ? N2 C6 C5 . . 120.3(3) ? C6 C7 C8 . . 106.8(3) ? C6 C7 H7 . . 126.6 ? C8 C7 H7 . . 126.6 ? N4 C8 C7 . . 130.8(4) ? N4 C8 C9 . . 122.5(4) ? C7 C8 C9 . . 106.7(3) ? N3 C9 N2 . . 125.8(3) ? N3 C9 C8 . . 125.9(4) ? N2 C9 C8 . . 108.2(3) ? N4 C10 N5 . . 125.1(4) ? N4 C10 C11 . . 126.2(4) ? N5 C10 C11 . . 108.7(3) ? N3 C11 C12 . . 130.4(4) ? N3 C11 C10 . . 122.4(4) ? C12 C11 C10 . . 107.2(3) ? C01G C012 C01A . . 108.1(3) ? C01G C012 N12 . . 127.8(3) ? C01A C012 N12 . . 124.1(3) ? C11 C12 C13 . . 106.3(4) ? C11 C12 H12 . . 126.8 ? C13 C12 H12 . . 126.8 ? C01Q C013 C01I . . 105.9(4) ? C01Q C013 C52 . . 128.3(4) ? C01I C013 C52 . . 125.8(4) ? N5 C13 C12 . . 111.1(3) ? N5 C13 C14 . . 121.2(4) ? C12 C13 C14 . . 127.6(4) ? C15 C14 C13 . . 120.0(4) ? C15 C14 C37 . . 121.7(4) ? C13 C14 C37 . . 118.3(4) ? C14 C15 N6 . . 121.5(4) ? C14 C15 C16 . . 130.3(4) ? N6 C15 C16 . . 108.2(4) ? N7 C016 C01G . . 108.6(3) ? N7 C016 C01D . . 120.1(3) ? C01G C016 C01D . . 131.2(3) ? C17 C16 C15 . . 107.5(4) ? C17 C16 H16 . . 126.2 ? C15 C16 H16 . . 126.2 ? C16 C17 C18 . . 105.7(4) ? C16 C17 C58 . . 129.6(4) ? C18 C17 C58 . . 124.7(4) ? N6 C18 C17 . . 110.9(4) ? N6 C18 H18 . . 124.5 ? C17 C18 H18 . . 124.5 ? C20 C19 C24 . . 120.5(3) ? C20 C19 C5 . . 118.1(3) ? C24 C19 C5 . . 121.4(3) ? C21 C20 C19 . . 119.4(3) ? C21 C20 C25 . . 120.1(4) ? C19 C20 C25 . . 120.5(3) ? C22 C21 C20 . . 121.4(4) ? C22 C21 H21 . . 119.3 ? C20 C21 H21 . . 119.3 ? C23 C22 C21 . . 117.9(4) ? C23 C22 C26 . . 120.9(4) ? C21 C22 C26 . . 121.2(4) ? C22 C23 C24 . . 122.7(4) ? C22 C23 H23 . . 118.7 ? C24 C23 H23 . . 118.7 ? C23 C24 C19 . . 118.0(4) ? C23 C24 C27 . . 120.1(4) ? C19 C24 C27 . . 121.9(4) ? C20 C25 H25A . . 109.5 ? C20 C25 H25B . . 109.5 ? H25A C25 H25B . . 109.5 ? C20 C25 H25C . . 109.5 ? H25A C25 H25C . . 109.5 ? H25B C25 H25C . . 109.5 ? C22 C26 H26A . . 109.5 ? C22 C26 H26B . . 109.5 ? H26A C26 H26B . . 109.5 ? C22 C26 H26C . . 109.5 ? H26A C26 H26C . . 109.5 ? H26B C26 H26C . . 109.5 ? C24 C27 H27A . . 109.5 ? C24 C27 H27B . . 109.5 ? H27A C27 H27B . . 109.5 ? C24 C27 H27C . . 109.5 ? H27A C27 H27C . . 109.5 ? H27B C27 H27C . . 109.5 ? C29 C28 C33 . . 120.8(4) ? C29 C28 C01D . . 119.0(4) ? C33 C28 C01D . . 120.2(4) ? C30 C29 C28 . . 117.9(4) ? C30 C29 C34 . . 120.3(4) ? C28 C29 C34 . . 121.9(4) ? C31 C30 C29 . . 122.7(4) ? C31 C30 H30 . . 118.7 ? C29 C30 H30 . . 118.7 ? C32 C31 C30 . . 118.0(4) ? C32 C31 C35 . . 121.8(5) ? C30 C31 C35 . . 120.3(5) ? C31 C32 C33 . . 122.7(4) ? C31 C32 H32 . . 118.6 ? C33 C32 H32 . . 118.6 ? C32 C33 C28 . . 117.9(4) ? C32 C33 C36 . . 120.1(4) ? C28 C33 C36 . . 122.0(4) ? C29 C34 H34A . . 109.5 ? C29 C34 H34B . . 109.5 ? H34A C34 H34B . . 109.5 ? C29 C34 H34C . . 109.5 ? H34A C34 H34C . . 109.5 ? H34B C34 H34C . . 109.5 ? C31 C35 H35A . . 109.5 ? C31 C35 H35B . . 109.5 ? H35A C35 H35B . . 109.5 ? C31 C35 H35C . . 109.5 ? H35A C35 H35C . . 109.5 ? H35B C35 H35C . . 109.5 ? C33 C36 H36A . . 109.5 ? C33 C36 H36B . . 109.5 ? H36A C36 H36B . . 109.5 ? C33 C36 H36C . . 109.5 ? H36A C36 H36C . . 109.5 ? H36B C36 H36C . . 109.5 ? C42 C37 C38 . . 120.1(4) ? C42 C37 C14 . . 120.2(3) ? C38 C37 C14 . . 119.6(4) ? C39 C38 C37 . . 117.8(4) ? C39 C38 C43 . . 121.4(4) ? C37 C38 C43 . . 120.8(4) ? C40 C39 C38 . . 123.9(4) ? C40 C39 H39 . . 118.1 ? C38 C39 H39 . . 118.1 ? C39 C40 C41 . . 117.1(4) ? C39 C40 C44 . . 122.5(5) ? C41 C40 C44 . . 120.4(5) ? C42 C41 C40 . . 121.7(5) ? C42 C41 H41 . . 119.2 ? C40 C41 H41 . . 119.2 ? C37 C42 C41 . . 119.4(4) ? C37 C42 C45 . . 121.0(4) ? C41 C42 C45 . . 119.6(4) ? C38 C43 H43A . . 109.5 ? C38 C43 H43B . . 109.5 ? H43A C43 H43B . . 109.5 ? C38 C43 H43C . . 109.5 ? H43A C43 H43C . . 109.5 ? H43B C43 H43C . . 109.5 ? C40 C44 H44A . . 109.5 ? C40 C44 H44B . . 109.5 ? H44A C44 H44B . . 109.5 ? C40 C44 H44C . . 109.5 ? H44A C44 H44C . . 109.5 ? H44B C44 H44C . . 109.5 ? C42 C45 H45A . . 109.5 ? C42 C45 H45B . . 109.5 ? H45A C45 H45B . . 109.5 ? C42 C45 H45C . . 109.5 ? H45A C45 H45C . . 109.5 ? H45B C45 H45C . . 109.5 ? C51 C46 C47 . . 118.8(4) ? C51 C46 C2 . . 120.1(3) ? C47 C46 C2 . . 121.1(3) ? C48 C47 C46 . . 120.6(4) ? C48 C47 H47 . . 119.7 ? C46 C47 H47 . . 119.7 ? C47 C48 C49 . . 118.9(4) ? C47 C48 H48 . . 120.6 ? C49 C48 H48 . . 120.5 ? C50 C49 C48 . . 122.2(4) ? C50 C49 N9 . . 118.4(4) ? C48 C49 N9 . . 119.3(4) ? C49 C50 C51 . . 118.9(4) ? C49 C50 H50 . . 120.6 ? C51 C50 H50 . . 120.6 ? C50 C51 C46 . . 120.5(4) ? C50 C51 H51 . . 119.8 ? C46 C51 H51 . . 119.8 ? C53 C52 C57 . . 118.6(4) ? C53 C52 C013 . . 121.3(3) ? C57 C52 C013 . . 120.1(4) ? C54 C53 C52 . . 121.1(4) ? C54 C53 H53 . . 119.4 ? C52 C53 H53 . . 119.4 ? C53 C54 C55 . . 119.1(4) ? C53 C54 H54 . . 120.5 ? C55 C54 H54 . . 120.5 ? C56 C55 C54 . . 121.4(4) ? C56 C55 N11 . . 118.9(4) ? C54 C55 N11 . . 119.7(4) ? C57 C56 C55 . . 118.8(4) ? C57 C56 H56 . . 120.6 ? C55 C56 H56 . . 120.6 ? C56 C57 C52 . . 121.1(4) ? C56 C57 H57 . . 119.5 ? C52 C57 H57 . . 119.5 ? C59 C58 C63 . . 118.7(4) ? C59 C58 C17 . . 120.9(4) ? C63 C58 C17 . . 120.4(4) ? C58 C59 C60 . . 120.9(5) ? C58 C59 H59 . . 119.6 ? C60 C59 H59 . . 119.5 ? C61 C60 C59 . . 118.5(4) ? C61 C60 H60 . . 120.7 ? C59 C60 H60 . . 120.7 ? C60 C61 C62 . . 122.2(4) ? C60 C61 N10 . . 118.5(4) ? C62 C61 N10 . . 119.3(4) ? C61 C62 C63 . . 119.3(4) ? C61 C62 H62 . . 120.4 ? C63 C62 H62 . . 120.4 ? C62 C63 C58 . . 120.4(4) ? C62 C63 H63 . . 119.8 ? C58 C63 H63 . . 119.8 ? N7 C01A C012 . . 109.0(3) ? N7 C01A H01A . . 125.5 ? C012 C01A H01A . . 125.5 ? C01D C01B N8 . . 121.7(3) ? C01D C01B C01Q . . 130.7(4) ? N8 C01B C01Q . . 107.6(3) ? C01B C01D C016 . . 120.2(3) ? C01B C01D C28 . . 119.9(3) ? C016 C01D C28 . . 119.9(3) ? C012 C01G C016 . . 106.5(3) ? C012 C01G H01G . . 126.8 ? C016 C01G H01G . . 126.8 ? N8 C01I C013 . . 110.4(3) ? N8 C01I H01I . . 124.8 ? C013 C01I H01I . . 124.8 ? C013 C01Q C01B . . 107.9(3) ? C013 C01Q H01Q . . 126.0 ? C01B C01Q H01Q . . 126.0 ? C4S C3S H3S1 . . 109.5 ? C4S C3S H3S2 . . 109.5 ? H3S1 C3S H3S2 . . 109.5 ? C4S C3S H3S3 . . 109.5 ? H3S1 C3S H3S3 . . 109.5 ? H3S2 C3S H3S3 . . 109.4 ? N1S C4S C3S . . 174.9(14) ? C7S C6S H6S1 . . 109.5 ? C7S C6S H6S2 . . 109.5 ? H6S1 C6S H6S2 . . 109.5 ? C7S C6S H6S3 . . 109.5 ? H6S1 C6S H6S3 . . 109.5 ? H6S2 C6S H6S3 . . 109.5 ? N2S C7S C6S . . 158.(3) ? C2S C1S Cl1S . . 114.4(10) ? C2S C1S H1S1 . . 108.7 ? Cl1S C1S H1S1 . . 108.7 ? C2S C1S H1S2 . . 108.6 ? Cl1S C1S H1S2 . . 108.7 ? H1S1 C1S H1S2 . . 107.6 ? C1S C2S Cl2S . . 119.7(12) ? C1S C2S H2S1 . . 107.4 ? Cl2S C2S H2S1 . . 107.4 ? C1S C2S H2S2 . . 107.5 ? Cl2S C2S H2S2 . . 107.4 ? H2S1 C2S H2S2 . . 106.9 ? C1 N1 C4 . . 107.5(3) ? C1 N1 B1 . . 126.9(3) ? C4 N1 B1 . . 125.6(3) ? C9 N2 C6 . . 106.6(3) ? C9 N2 B1 . . 125.5(3) ? C6 N2 B1 . . 126.9(3) ? C9 N3 C11 . . 111.5(3) ? C10 N4 C8 . . 111.4(3) ? C10 N5 C13 . . 106.6(3) ? C10 N5 B2 . . 127.0(4) ? C13 N5 B2 . . 125.7(4) ? C18 N6 C15 . . 107.6(4) ? C18 N6 B2 . . 126.1(4) ? C15 N6 B2 . . 126.2(4) ? C01A N7 C016 . . 107.9(3) ? C01A N7 B3 . . 125.8(3) ? C016 N7 B3 . . 126.4(3) ? C01I N8 C01B . . 108.1(3) ? C01I N8 B3 . . 126.9(3) ? C01B N8 B3 . . 124.9(3) ? O2 N9 O1 . . 123.9(4) ? O2 N9 C49 . . 118.0(4) ? O1 N9 C49 . . 118.1(4) ? O4 N10 O3 . . 123.3(4) ? O4 N10 C61 . . 118.6(4) ? O3 N10 C61 . . 118.1(4) ? O5 N11 O6 . . 122.9(4) ? O5 N11 C55 . . 118.5(3) ? O6 N11 C55 . . 118.7(3) ? C1 N12 C012 . . 124.2(3) ? C1 N12 H12A . . 117.9 ? C012 N12 H12A . . 117.9 ? C11S C10S H10A . . 109.5 ? C11S C10S H10B . . 109.5 ? H10A C10S H10B . . 109.5 ? C11S C10S H10C . . 109.5 ? H10A C10S H10C . . 109.5 ? H10B C10S H10C . . 109.5 ? N5S C11S C10S . . 178.0(13) ? N6S C8S C9S . . 177.3(17) ? C8S C9S H9S1 . . 109.5 ? C8S C9S H9S2 . . 109.5 ? H9S1 C9S H9S2 . . 109.4 ? C8S C9S H9S3 . . 109.5 ? H9S1 C9S H9S3 . . 109.5 ? H9S2 C9S H9S3 . . 109.5 ? N7S C12S C13S . . 164.(3) ? C12S C13S H13A . . 109.5 ? C12S C13S H13B . . 109.5 ? H13A C13S H13B . . 109.4 ? C12S C13S H13C . . 109.5 ? H13A C13S H13C . . 109.5 ? H13B C13S H13C . . 109.5 ? _shelx_res_file ; TITL shino131003hy_ref in P-1 CELL 0.71073 14.6707 17.1450 18.0545 118.335 96.657 90.695 ZERR 2.00 0.00060 0.00070 0.00099 0.0017 0.0028 0.0020 LATT 1 SFAC C H B N O F Cl UNIT 160.24 135.44 6 31.04 12.5 12 2.18 OMIT -10 50 L.S. 2 SHEL 999 0.839 ACTA BOND $h FMAP 2 PLAN 5 SIZE 0.19 0.17 0.16 SIMU 0.01 C3S C4S N1S SIMU 0.01 C13S C12S N7S ISOR 0.01 C13S ISOR 0.01 C3S TEMP -183 WGHT 0.152900 8.644100 FVAR 0.29799 0.51518 0.80401 0.54400 B1 3 0.183291 0.744183 0.805168 11.00000 0.03308 0.03558 = 0.03675 0.01895 -0.00688 -0.00283 B2 3 -0.278074 0.648978 0.508101 11.00000 0.05296 0.06776 = 0.05371 0.03228 0.00797 0.00627 B3 3 0.677726 0.960029 1.061736 11.00000 0.02596 0.02892 = 0.05377 0.00625 -0.00491 0.00359 C1 1 0.323912 0.720206 0.892926 11.00000 0.02519 0.02830 = 0.02965 0.01174 -0.00080 -0.00250 C2 1 0.351357 0.656922 0.922409 11.00000 0.02442 0.03464 = 0.03296 0.01639 0.00055 0.00334 C3 1 0.279318 0.593839 0.892253 11.00000 0.02635 0.03299 = 0.03471 0.01725 -0.00179 0.00022 AFIX 43 H3 2 0.276810 0.543197 0.900593 11.00000 -1.20000 AFIX 0 C4 1 0.208568 0.616226 0.846287 11.00000 0.02761 0.02764 = 0.03227 0.01303 0.00009 -0.00058 C5 1 0.122709 0.573852 0.805922 11.00000 0.02561 0.02979 = 0.03340 0.01221 0.00047 0.00080 C6 1 0.063004 0.611228 0.763623 11.00000 0.02820 0.03399 = 0.03284 0.01530 0.00040 -0.00031 C7 1 -0.021309 0.575791 0.714357 11.00000 0.02953 0.03800 = 0.04020 0.02009 -0.00425 -0.00548 AFIX 43 H7 2 -0.052450 0.520979 0.701379 11.00000 -1.20000 AFIX 0 C8 1 -0.052173 0.636363 0.687126 11.00000 0.02658 0.04176 = 0.03597 0.01960 -0.00236 -0.00106 C9 1 0.017104 0.710771 0.724494 11.00000 0.02905 0.03135 = 0.03232 0.01236 -0.00154 0.00402 C10 1 -0.131267 0.703694 0.624831 11.00000 0.02883 0.04212 = 0.03448 0.01829 -0.00128 0.00199 C11 1 -0.064691 0.780286 0.665748 11.00000 0.03261 0.03262 = 0.03040 0.01161 -0.00077 0.00554 C012 1 0.467726 0.811207 0.929074 11.00000 0.02526 0.03023 = 0.03449 0.01514 -0.00202 0.00004 C12 1 -0.095136 0.841315 0.639017 11.00000 0.03420 0.03510 = 0.03500 0.01381 -0.00218 0.00514 AFIX 43 H12 2 -0.066170 0.898106 0.655537 11.00000 -1.20000 AFIX 0 C013 1 0.925621 0.908375 1.041244 11.00000 0.02646 0.03338 = 0.04593 0.01723 0.00033 0.00114 C13 1 -0.176877 0.801776 0.583027 11.00000 0.03400 0.03892 = 0.03204 0.01620 0.00317 0.01037 C14 1 -0.231892 0.836143 0.535831 11.00000 0.02984 0.04064 = 0.02878 0.01121 0.00058 0.00541 C15 1 -0.305326 0.784337 0.476742 11.00000 0.03441 0.04224 = 0.03457 0.01653 0.00283 0.00702 C016 1 0.619633 0.799207 0.940261 11.00000 0.02706 0.02627 = 0.03718 0.01231 0.00290 0.00126 C16 1 -0.368130 0.802645 0.421354 11.00000 0.03795 0.04622 = 0.03709 0.01929 0.00215 0.01053 AFIX 43 H16 2 -0.369442 0.856850 0.419064 11.00000 -1.20000 AFIX 0 C17 1 -0.426790 0.726969 0.371574 11.00000 0.03359 0.05391 = 0.03351 0.01893 -0.00067 0.00596 C18 1 -0.398597 0.663470 0.398877 11.00000 0.03465 0.05200 = 0.04080 0.02130 -0.00507 -0.00173 AFIX 43 H18 2 -0.426769 0.604995 0.375657 11.00000 -1.20000 AFIX 0 C19 1 0.089245 0.494014 0.810498 11.00000 0.02286 0.03308 = 0.03299 0.01647 -0.00536 -0.00048 C20 1 0.032090 0.506184 0.871499 11.00000 0.02611 0.03510 = 0.03277 0.01484 -0.00449 0.00273 C21 1 -0.002154 0.432440 0.875885 11.00000 0.02542 0.03721 = 0.03782 0.01802 0.00006 0.00017 AFIX 43 H21 2 -0.041905 0.440678 0.916573 11.00000 -1.20000 AFIX 0 C22 1 0.020682 0.346925 0.821868 11.00000 0.02766 0.03779 = 0.03266 0.01382 -0.00617 -0.00451 C23 1 0.079798 0.337105 0.763478 11.00000 0.03886 0.03090 = 0.03546 0.00816 0.00127 -0.00096 AFIX 43 H23 2 0.097877 0.279459 0.727969 11.00000 -1.20000 AFIX 0 C24 1 0.113569 0.408467 0.754988 11.00000 0.03094 0.03684 = 0.03364 0.01441 -0.00064 -0.00128 C25 1 0.010001 0.598357 0.933820 11.00000 0.04043 0.03696 = 0.04146 0.01851 0.00674 0.00706 AFIX 137 H25A 2 -0.032295 0.594320 0.970292 11.00000 -1.50000 H25B 2 -0.018924 0.627451 0.902702 11.00000 -1.50000 H25C 2 0.066879 0.633156 0.968937 11.00000 -1.50000 AFIX 0 C26 1 -0.015264 0.267569 0.828022 11.00000 0.04521 0.03749 = 0.04337 0.01723 0.00290 -0.00459 AFIX 137 H26A 2 0.024302 0.261714 0.872454 11.00000 -1.50000 H26B 2 -0.015249 0.213690 0.773439 11.00000 -1.50000 H26C 2 -0.078169 0.275812 0.842167 11.00000 -1.50000 AFIX 0 C27 1 0.174894 0.393021 0.688457 11.00000 0.05286 0.03779 = 0.04205 0.01324 0.01164 0.00049 AFIX 137 H27A 2 0.209458 0.340998 0.677798 11.00000 -1.50000 H27B 2 0.217971 0.445383 0.708643 11.00000 -1.50000 H27C 2 0.137081 0.382652 0.635719 11.00000 -1.50000 AFIX 0 C28 1 0.727432 0.680413 0.870244 11.00000 0.02205 0.03018 = 0.05086 0.01269 0.00609 -0.00074 C29 1 0.762621 0.625273 0.902612 11.00000 0.02536 0.03014 = 0.04857 0.01256 0.00397 -0.00113 C30 1 0.780276 0.538777 0.844425 11.00000 0.03101 0.03125 = 0.06172 0.01867 0.01027 0.00414 AFIX 43 H30 2 0.804674 0.500996 0.865585 11.00000 -1.20000 AFIX 0 C31 1 0.763667 0.506244 0.757641 11.00000 0.03836 0.02911 = 0.05240 0.00609 0.01368 -0.00121 C32 1 0.728808 0.562134 0.727918 11.00000 0.04099 0.04514 = 0.04434 0.01269 0.01204 0.00037 AFIX 43 H32 2 0.717239 0.540422 0.668276 11.00000 -1.20000 AFIX 0 C33 1 0.709841 0.649222 0.781821 11.00000 0.03011 0.03502 = 0.04449 0.01182 0.00574 0.00050 C34 1 0.780753 0.656653 0.996937 11.00000 0.03347 0.03559 = 0.05322 0.02017 0.00289 0.00369 AFIX 137 H34A 2 0.840174 0.691679 1.020535 11.00000 -1.50000 H34B 2 0.782040 0.605117 1.006736 11.00000 -1.50000 H34C 2 0.731808 0.693520 1.024729 11.00000 -1.50000 AFIX 0 C35 1 0.784125 0.412313 0.697993 11.00000 0.05681 0.03642 = 0.07301 0.00702 0.02049 0.00044 AFIX 137 H35A 2 0.841673 0.398409 0.721043 11.00000 -1.50000 H35B 2 0.790252 0.406803 0.642262 11.00000 -1.50000 H35C 2 0.733715 0.370814 0.691994 11.00000 -1.50000 AFIX 0 C36 1 0.675601 0.707690 0.745563 11.00000 0.05496 0.05401 = 0.04993 0.02345 0.01359 0.00936 AFIX 137 H36A 2 0.684052 0.680346 0.685522 11.00000 -1.50000 H36B 2 0.710266 0.765931 0.776809 11.00000 -1.50000 H36C 2 0.610089 0.715037 0.750641 11.00000 -1.50000 AFIX 0 C37 1 -0.206404 0.928101 0.551653 11.00000 0.03326 0.03579 = 0.03594 0.01511 -0.00219 0.00849 C38 1 -0.233227 1.002422 0.623258 11.00000 0.05206 0.04643 = 0.04554 0.01880 0.00705 0.01649 C39 1 -0.206129 1.086344 0.636892 11.00000 0.05376 0.04260 = 0.05175 0.00962 0.00501 0.01743 AFIX 43 H39 2 -0.223558 1.136265 0.684945 11.00000 -1.20000 AFIX 0 C40 1 -0.155182 1.101820 0.584698 11.00000 0.04485 0.03757 = 0.05671 0.01631 -0.00692 0.01106 C41 1 -0.128863 1.027148 0.514976 11.00000 0.04174 0.03995 = 0.04798 0.01829 -0.00332 0.00310 AFIX 43 H41 2 -0.092991 1.035517 0.478393 11.00000 -1.20000 AFIX 0 C42 1 -0.154027 0.940852 0.497964 11.00000 0.04063 0.03327 = 0.03559 0.01235 -0.00245 0.00748 C43 1 -0.290673 0.989921 0.680645 11.00000 0.08817 0.06475 = 0.05902 0.02261 0.03275 0.02581 AFIX 137 H43A 2 -0.285737 1.044837 0.735044 11.00000 -1.50000 H43B 2 -0.268824 0.941303 0.690352 11.00000 -1.50000 H43C 2 -0.355085 0.975436 0.654128 11.00000 -1.50000 AFIX 0 C44 1 -0.129287 1.194220 0.599885 11.00000 0.06825 0.03639 = 0.08428 0.01984 -0.00368 0.01073 AFIX 137 H44A 2 -0.183356 1.218199 0.583107 11.00000 -1.50000 H44B 2 -0.080652 1.191814 0.566107 11.00000 -1.50000 H44C 2 -0.107040 1.232642 0.660299 11.00000 -1.50000 AFIX 0 C45 1 -0.124930 0.862473 0.421045 11.00000 0.05305 0.03831 = 0.04183 0.01039 0.01078 -0.00019 AFIX 137 H45A 2 -0.095036 0.821793 0.438420 11.00000 -1.50000 H45B 2 -0.081696 0.883760 0.395884 11.00000 -1.50000 H45C 2 -0.179240 0.831180 0.379089 11.00000 -1.50000 AFIX 0 C46 1 0.433511 0.665939 0.982304 11.00000 0.02251 0.03707 = 0.03535 0.01910 -0.00207 -0.00058 C47 1 0.460072 0.746958 1.057137 11.00000 0.03050 0.03896 = 0.03861 0.01923 0.00099 0.00193 AFIX 43 H47 2 0.426740 0.797562 1.067802 11.00000 -1.20000 AFIX 0 C48 1 0.533895 0.753415 1.114920 11.00000 0.03047 0.03816 = 0.03597 0.01436 -0.00282 -0.00361 AFIX 43 H48 2 0.552054 0.808165 1.165030 11.00000 -1.20000 AFIX 0 C49 1 0.581016 0.679017 1.098783 11.00000 0.02513 0.04909 = 0.03557 0.02382 -0.00363 0.00013 C50 1 0.558091 0.598983 1.025813 11.00000 0.03089 0.03734 = 0.04530 0.02174 0.00096 0.00339 AFIX 43 H50 2 0.592100 0.548942 1.015920 11.00000 -1.20000 AFIX 0 C51 1 0.484377 0.592755 0.966972 11.00000 0.02768 0.03388 = 0.03731 0.01653 -0.00271 0.00124 AFIX 43 H51 2 0.468507 0.538313 0.915970 11.00000 -1.20000 AFIX 0 C52 1 1.025385 0.932532 1.065662 11.00000 0.02633 0.03175 = 0.04190 0.01641 0.00230 0.00281 C53 1 1.060147 1.020460 1.110079 11.00000 0.02897 0.03326 = 0.05135 0.01400 0.00124 0.00456 AFIX 43 H53 2 1.018870 1.066221 1.127171 11.00000 -1.20000 AFIX 0 C54 1 1.153705 1.042776 1.129951 11.00000 0.03582 0.02855 = 0.05497 0.01266 0.00236 -0.00052 AFIX 43 H54 2 1.176893 1.103356 1.159759 11.00000 -1.20000 AFIX 0 C55 1 1.213426 0.975601 1.105833 11.00000 0.02614 0.03651 = 0.04268 0.01730 0.00193 0.00111 C56 1 1.181144 0.887151 1.063377 11.00000 0.03397 0.03203 = 0.06059 0.01223 0.00876 0.00895 AFIX 43 H56 2 1.222730 0.841699 1.048505 11.00000 -1.20000 AFIX 0 C57 1 1.087317 0.866000 1.042942 11.00000 0.02946 0.02929 = 0.06915 0.01401 0.00210 0.00085 AFIX 43 H57 2 1.064377 0.805350 1.012991 11.00000 -1.20000 AFIX 0 C58 1 -0.502597 0.710075 0.303771 11.00000 0.03117 0.05798 = 0.03859 0.02280 0.00177 0.00543 C59 1 -0.544274 0.780212 0.298294 11.00000 0.04480 0.05473 = 0.04109 0.02009 0.00025 0.00900 AFIX 43 H59 2 -0.523255 0.839691 0.338864 11.00000 -1.20000 AFIX 0 C60 1 -0.616570 0.764154 0.233897 11.00000 0.04580 0.06585 = 0.04727 0.03177 0.00887 0.01913 AFIX 43 H60 2 -0.644354 0.812035 0.229918 11.00000 -1.20000 AFIX 0 C61 1 -0.646617 0.677364 0.176348 11.00000 0.02884 0.06829 = 0.03782 0.02922 -0.00075 0.00097 C62 1 -0.607090 0.606372 0.179689 11.00000 0.03255 0.05765 = 0.04521 0.02556 -0.00090 -0.00323 AFIX 43 H62 2 -0.628761 0.547206 0.138732 11.00000 -1.20000 AFIX 0 C63 1 -0.535403 0.622254 0.243442 11.00000 0.03417 0.05970 = 0.04236 0.02728 -0.00108 0.00477 AFIX 43 H63 2 -0.508188 0.573700 0.246534 11.00000 -1.20000 AFIX 0 C01A 1 0.511868 0.892460 0.992755 11.00000 0.02670 0.03115 = 0.03800 0.01490 -0.00187 0.00178 AFIX 43 H01A 2 0.481991 0.944104 1.026023 11.00000 -1.20000 AFIX 0 C01B 1 0.784899 0.835599 0.979421 11.00000 0.02652 0.02409 = 0.04646 0.01144 0.00018 0.00314 C01D 1 0.710674 0.773973 0.931023 11.00000 0.03104 0.02695 = 0.04114 0.01413 0.00215 0.00238 C01G 1 0.534651 0.752507 0.896133 11.00000 0.02903 0.02584 = 0.03592 0.01295 -0.00108 -0.00148 AFIX 43 H01G 2 0.524914 0.692491 0.852320 11.00000 -1.20000 AFIX 0 C01I 1 0.855149 0.965990 1.075518 11.00000 0.02740 0.02570 = 0.04904 0.01345 -0.00358 0.00128 AFIX 43 H01I 2 0.865526 1.026462 1.118200 11.00000 -1.20000 AFIX 0 C01Q 1 0.880625 0.826977 0.980791 11.00000 0.03135 0.02867 = 0.05093 0.01498 0.00476 0.00474 AFIX 43 H01Q 2 0.909259 0.774850 0.946520 11.00000 -1.20000 PART 1 AFIX 0 C3S 1 0.545648 0.134161 0.255001 21.00000 0.04841 0.08498 = 0.04747 0.02600 0.00248 0.01655 AFIX 31 H3S1 2 0.589634 0.177810 0.255283 21.00000 -1.50000 H3S2 2 0.497034 0.115296 0.206517 21.00000 -1.50000 H3S3 2 0.577607 0.082474 0.250316 21.00000 -1.50000 AFIX 0 C4S 1 0.505319 0.173855 0.333035 21.00000 0.05779 0.07054 = 0.06371 0.03202 0.01430 0.00993 N1S 4 0.473460 0.198192 0.391962 21.00000 0.08838 0.08653 = 0.08421 0.03936 0.03513 0.02398 C6S 1 0.592226 0.084120 0.482467 21.00000 0.08535 0.12775 = 0.06154 0.05971 0.01833 0.04294 AFIX 31 H6S1 2 0.650360 0.078652 0.511765 21.00000 -1.50000 H6S2 2 0.541220 0.079682 0.511178 21.00000 -1.50000 H6S3 2 0.594131 0.141789 0.483500 21.00000 -1.50000 AFIX 0 C7S 1 0.579304 0.015819 0.398035 21.00000 0.20311 0.08958 = 0.13158 0.05366 -0.00788 0.06723 N2S 4 0.595678 -0.026822 0.332781 21.00000 0.25142 0.05593 = 0.07372 0.03466 0.04983 0.05588 C1S 1 0.172275 0.866282 0.640605 41.00000 0.06050 0.05761 = 0.09220 0.04704 0.02557 -0.00447 AFIX 23 H1S1 2 0.116121 0.853736 0.599400 41.00000 -1.20000 H1S2 2 0.157050 0.848399 0.682692 41.00000 -1.20000 AFIX 0 C2S 1 0.193238 0.945885 0.677248 41.00000 0.05394 0.31470 = 0.05161 0.07562 -0.01672 0.00328 AFIX 23 H2S1 2 0.220028 0.960378 0.636981 41.00000 -1.20000 H2S2 2 0.242947 0.958285 0.724311 41.00000 -1.20000 AFIX 0 CL1S 7 0.254529 0.803694 0.588597 41.00000 0.06787 0.11254 = 0.07550 0.05448 -0.01355 -0.00029 CL2S 7 0.096646 1.031377 0.726181 41.00000 0.10726 0.09015 = 0.07109 0.04832 0.00699 -0.00632 PART 0 F1 6 0.229211 0.740295 0.739978 11.00000 0.03505 0.08175 = 0.06377 0.05122 -0.00543 -0.00564 F2 6 0.178624 0.831200 0.864235 11.00000 0.05249 0.02896 = 0.06624 0.01681 -0.02559 0.00021 F3 6 -0.342668 0.627324 0.547237 11.00000 0.06208 0.11475 = 0.07005 0.05415 -0.00462 -0.01483 F4 6 -0.245120 0.570978 0.451053 11.00000 0.08798 0.06372 = 0.06279 0.02699 -0.00620 0.00365 F5 6 0.668765 0.982469 1.144441 11.00000 0.03131 0.08910 = 0.04463 -0.00253 -0.00105 0.00721 F6 6 0.667315 1.033523 1.048536 11.00000 0.02937 0.02811 = 0.11618 0.02035 -0.01386 0.00121 N1 4 0.238937 0.695357 0.848411 11.00000 0.02569 0.02966 = 0.03330 0.01202 -0.00360 0.00009 N2 4 0.088204 0.692534 0.769877 11.00000 0.02882 0.02878 = 0.03750 0.01521 -0.00462 0.00163 N3 4 0.012874 0.783773 0.716617 11.00000 0.03179 0.03178 = 0.03477 0.01326 -0.00488 0.00217 N4 4 -0.128460 0.631864 0.634438 11.00000 0.02710 0.04637 = 0.04126 0.02458 -0.00407 0.00006 N5 4 -0.199378 0.718102 0.574140 11.00000 0.03315 0.04236 = 0.04068 0.02348 -0.00011 0.00429 N6 4 -0.327883 0.697584 0.460915 11.00000 0.03369 0.04575 = 0.04202 0.02266 -0.00259 0.00098 N7 4 0.603725 0.885436 0.999152 11.00000 0.02475 0.03057 = 0.04014 0.01265 0.00045 0.00367 N8 4 0.772250 0.923099 1.039234 11.00000 0.02475 0.02982 = 0.04691 0.01326 -0.00142 0.00347 N9 4 0.656232 0.683580 1.163155 11.00000 0.03140 0.05925 = 0.04563 0.02826 -0.00040 0.00507 N10 4 -0.722431 0.660517 0.108672 11.00000 0.03304 0.07485 = 0.05126 0.04140 0.00146 0.00033 N11 4 1.312687 0.998173 1.126459 11.00000 0.03145 0.03551 = 0.05399 0.01572 0.00609 -0.00081 N12 4 0.370821 0.794391 0.906629 11.00000 0.02634 0.02793 = 0.03850 0.01354 -0.00114 0.00089 AFIX 43 H12A 2 0.339530 0.835373 0.901377 11.00000 -1.20000 AFIX 0 O1 5 0.684856 0.757250 1.222302 11.00000 0.04797 0.06776 = 0.04673 0.01420 -0.01644 0.00403 O2 5 0.685182 0.614326 1.155111 11.00000 0.04989 0.06333 = 0.06370 0.03639 -0.01297 0.01074 O3 5 -0.747492 0.582489 0.056051 11.00000 0.05228 0.07934 = 0.05711 0.04232 -0.01448 -0.01850 O4 5 -0.757471 0.724321 0.106810 11.00000 0.04021 0.08488 = 0.06634 0.04487 -0.00119 0.01266 O5 5 1.341158 1.074830 1.150606 11.00000 0.03685 0.04152 = 0.11003 0.02792 0.00333 -0.00375 O6 5 1.363973 0.939399 1.119450 11.00000 0.03069 0.04354 = 0.06838 0.01923 0.00993 0.00603 PART 1 C10S 1 0.121702 0.576569 0.540849 11.00000 0.10927 0.09070 = 0.07149 0.01408 0.01554 -0.00659 AFIX 31 H10A 2 0.154064 0.532249 0.496660 11.00000 -1.50000 H10B 2 0.083451 0.546942 0.562589 11.00000 -1.50000 H10C 2 0.166710 0.619880 0.587374 11.00000 -1.50000 AFIX 0 C11S 1 0.058979 0.625688 0.502245 11.00000 0.06203 0.06314 = 0.06275 0.00422 0.01564 0.00050 N5S 4 0.024635 0.655275 0.480572 11.00000 0.08115 0.13852 = 0.06207 0.01187 0.00549 -0.01951 N6S 4 0.437374 0.566202 0.721054 11.00000 0.14606 0.06268 = 0.07503 0.00906 -0.00997 -0.01932 C8S 1 0.419084 0.582595 0.670403 11.00000 0.16533 0.06769 = 0.11170 0.01792 -0.02952 -0.02549 C9S 1 0.398067 0.604769 0.598279 11.00000 0.36885 0.14025 = 0.21975 0.11978 -0.15214 -0.10004 AFIX 31 H9S1 2 0.378243 0.665278 0.620848 11.00000 -1.50000 H9S2 2 0.348912 0.562648 0.556025 11.00000 -1.50000 H9S3 2 0.453510 0.600663 0.571509 11.00000 -1.50000 PART 4 AFIX 0 C12S 1 0.533929 0.061415 0.280666 -21.00000 0.11601 0.20212 = 0.20426 0.11091 0.04692 0.02440 N7S 4 0.542230 -0.006924 0.301270 -21.00000 0.14239 0.19143 = 0.22442 0.10624 0.06062 0.01654 C13S 1 0.553545 0.164774 0.272268 -21.00000 0.16220 0.21756 = 0.20634 0.09513 0.04059 0.02960 AFIX 31 H13A 2 0.613531 0.165216 0.253522 -21.00000 -1.50000 H13B 2 0.552429 0.216941 0.327896 -21.00000 -1.50000 H13C 2 0.504952 0.166315 0.230985 -21.00000 -1.50000 PART 6 AFIX 0 O1W 5 0.500000 0.000000 0.500000 0.24917 0.12773 0.07986 = 0.07645 -0.02571 -0.02953 0.06037 PART HKLF 4 REM shino131003hy_ref in P-1 REM R1 = 0.0871 for 9709 Fo > 4sig(Fo) and 0.1129 for all 13197 data REM 1082 parameters refined using 36 restraints END WGHT 0.1504 8.4854 REM Highest difference peak 1.217, deepest hole -0.734, 1-sigma level 0.085 Q1 1 0.2875 0.7321 0.5501 11.00000 0.05 1.22 Q2 1 -0.2532 0.4699 0.4109 11.00000 0.05 1.08 Q3 1 0.0301 1.0336 0.7064 11.00000 0.05 0.97 Q4 1 0.1833 1.1310 0.7890 11.00000 0.05 0.79 Q5 1 0.6263 0.1592 0.5078 11.00000 0.05 0.77 ; _shelx_res_checksum 42097 _shelx_hkl_file ; -3 0 0 17.40 0.80 3 0 0 14.60 0.80 -4 0 0 245.58 7.10 4 0 0 239.28 7.10 -6 0 0 46.10 1.80 6 0 0 43.40 1.90 -7 0 0 274.67 8.00 7 0 0 255.97 8.00 -8 0 0 26.30 1.50 8 0 0 24.80 1.60 -9 0 0 476.65 13.90 9 0 0 471.65 14.00 -10 0 0 8.90 1.20 10 0 0 12.40 1.40 -11 0 0 14.40 1.40 11 0 0 14.30 1.60 -12 0 0 3.10 0.80 12 0 0 4.20 1.00 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6.80 2 7 -6 1.20 0.50 -2 -7 6 0.70 0.50 -2 -7 6 1.50 0.30 1 7 -6 164.18 4.80 1 7 -6 155.18 4.50 -1 -7 6 150.08 4.50 -1 -7 6 157.68 4.80 0 7 -6 170.48 5.10 0 7 -6 161.68 4.80 0 -7 6 170.08 4.80 -1 7 -6 952.50 27.50 -1 7 -6 947.51 27.00 1 -7 6 1011.80 27.00 -2 7 -6 0.00 0.30 -3 7 -6 2.30 0.40 -4 7 -6 61.79 2.00 -4 7 -6 58.59 2.40 -5 7 -6 1.90 0.60 -5 7 -6 2.00 0.40 -6 7 -6 20.90 1.50 -6 7 -6 21.30 1.10 -7 7 -6 7.30 1.20 -8 7 -6 81.39 3.20 -9 7 -6 50.39 2.50 9 -7 6 50.39 2.70 -10 7 -6 30.70 2.20 10 -7 6 27.60 2.30 -11 7 -6 231.18 7.70 11 -7 6 236.18 7.80 12 -7 6 3.60 1.20 13 -7 6 6.80 1.40 14 -7 6 3.90 1.20 15 -7 6 2.60 1.40 15 8 -7 -0.70 1.00 14 8 -7 29.50 2.40 13 8 -7 -0.40 0.80 12 8 -7 19.70 2.00 11 8 -7 35.90 2.30 -11 -8 7 31.30 2.10 10 8 -7 39.90 2.30 -10 -8 7 37.90 2.10 9 8 -7 138.99 4.70 -9 -8 7 142.59 4.70 8 8 -7 16.50 1.40 -8 -8 7 13.30 1.30 7 8 -7 3.30 0.70 -7 -8 7 2.40 0.60 6 8 -7 91.89 3.30 -6 -8 7 97.49 3.30 -6 -8 7 100.59 3.30 5 8 -7 94.49 3.20 -5 -8 7 96.69 3.10 -5 -8 7 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201.68 6.20 -4 -9 11 20.90 1.40 4 9 -11 21.20 1.50 -5 -9 11 131.29 4.40 5 9 -11 132.29 4.40 -6 -9 11 13.90 1.40 -6 -9 11 17.50 1.30 6 9 -11 12.70 1.40 -7 -9 11 12.40 1.40 7 9 -11 9.60 1.30 -8 -9 11 -0.60 0.70 8 9 -11 0.10 0.70 -9 -9 11 19.40 1.70 9 9 -11 18.70 1.70 10 9 -11 9.30 1.10 11 9 -11 9.70 1.70 12 9 -11 2.00 0.90 13 9 -11 25.00 2.20 14 9 -11 -0.50 0.90 -9 8 -10 -0.60 0.70 -8 8 -10 -0.20 0.60 -7 8 -10 1.10 0.70 -6 8 -10 5.70 0.90 -5 8 -10 4.40 0.80 -4 8 -10 15.30 1.40 -4 8 -10 14.60 0.90 -2 8 -10 8.80 1.30 -1 8 -10 3.40 0.70 0 8 -10 73.59 2.80 1 8 -10 0.00 0.50 -2 -8 10 73.19 2.80 2 8 -10 76.09 2.70 -3 -8 10 14.30 1.20 3 8 -10 13.60 1.30 -4 -8 10 0.80 0.60 4 8 -10 1.20 0.50 -5 -8 10 10.50 1.20 5 8 -10 10.00 1.20 -6 -8 10 3.60 0.70 6 8 -10 3.50 0.70 -7 -8 10 142.29 4.80 7 8 -10 144.69 4.70 -8 -8 10 0.70 0.70 8 8 -10 0.70 0.60 -9 -8 10 121.79 4.30 9 8 -10 121.59 4.30 -10 -8 10 14.20 1.70 10 8 -10 17.70 1.80 11 8 -10 4.30 1.00 12 8 -10 -1.30 0.80 13 8 -10 20.10 2.00 14 8 -10 0.00 0.90 15 8 -10 5.20 1.10 -10 7 -9 18.80 1.80 -9 7 -9 39.80 2.30 -8 7 -9 25.60 1.80 -7 7 -9 18.90 1.70 -6 7 -9 1.50 0.60 -5 7 -9 7.10 1.20 -4 7 -9 1.20 0.50 -3 7 -9 57.09 1.80 -1 7 -9 1.00 0.60 0 7 -9 64.89 2.50 1 7 -9 15.40 1.20 -2 -7 9 39.60 1.80 2 7 -9 39.10 1.80 -3 -7 9 26.90 1.50 -4 -7 9 7.30 1.10 4 7 -9 7.30 1.00 -5 -7 9 4.20 0.70 5 7 -9 6.40 1.10 -6 -7 9 38.20 1.90 6 7 -9 39.70 1.80 -7 -7 9 108.49 3.80 7 7 -9 110.39 3.70 -8 -7 9 3.60 0.70 8 7 -9 4.50 0.70 -9 -7 9 1.00 0.70 9 7 -9 0.90 0.70 -10 -7 9 12.40 1.70 10 7 -9 14.60 1.70 -11 -7 9 13.30 1.90 11 7 -9 16.90 1.80 12 7 -9 18.50 1.90 13 7 -9 6.10 1.10 14 7 -9 1.90 0.90 15 7 -9 -0.50 0.90 15 -6 8 -1.00 1.30 14 -6 8 -1.50 1.20 13 -6 8 11.50 1.60 12 -6 8 22.20 2.40 11 -6 8 -0.20 1.00 -10 6 -8 134.19 4.80 -9 6 -8 -0.70 0.60 -8 6 -8 0.30 0.60 -7 6 -8 70.89 2.90 -6 6 -8 30.50 1.70 -5 6 -8 9.20 1.10 -4 6 -8 63.29 2.50 -1 6 -8 521.25 15.10 0 6 -8 23.30 1.40 1 6 -8 142.79 4.50 -2 -6 8 44.50 1.90 -3 -6 8 1.70 0.60 3 6 -8 2.10 0.50 -4 -6 8 9.60 1.10 4 6 -8 7.80 1.00 -5 -6 8 3.90 0.70 5 6 -8 3.50 0.60 -6 -6 8 92.59 3.30 6 6 -8 95.89 3.20 -7 -6 8 36.60 1.80 7 6 -8 35.00 1.80 -8 -6 8 37.20 1.90 8 6 -8 37.80 1.90 -9 -6 8 26.40 1.70 9 6 -8 27.50 1.70 -10 -6 8 5.00 0.80 10 6 -8 8.10 1.40 -11 -6 8 0.10 0.80 11 6 -8 0.70 0.70 12 6 -8 3.90 0.90 13 6 -8 47.60 2.60 14 6 -8 6.30 1.10 15 6 -8 3.30 1.00 16 6 -8 3.40 1.10 15 -5 7 2.30 1.20 14 -5 7 7.20 1.30 13 -5 7 0.30 1.00 12 -5 7 66.39 3.30 11 -5 7 188.38 6.40 -11 5 -7 173.08 6.10 10 -5 7 41.90 2.50 -10 5 -7 40.60 2.30 9 -5 7 1.40 0.80 -9 5 -7 1.30 0.60 8 -5 7 114.79 4.20 -8 5 -7 110.09 4.10 -7 5 -7 82.99 3.20 -6 5 -7 28.00 1.70 -5 5 -7 46.00 2.10 -4 5 -7 671.73 19.40 -3 5 -7 8.20 1.20 0 5 -7 30.80 1.50 -1 -5 7 392.46 11.70 1 5 -7 414.56 11.70 -2 -5 7 162.28 4.90 2 5 -7 155.08 4.80 -3 -5 7 0.80 0.50 3 5 -7 0.90 0.50 -4 -5 7 3.70 0.60 4 5 -7 3.70 0.50 -5 -5 7 0.70 0.50 5 5 -7 1.20 0.50 -6 -5 7 169.28 5.20 6 5 -7 160.58 5.10 -7 -5 7 85.49 3.00 7 5 -7 83.89 3.00 -8 -5 7 56.89 2.30 8 5 -7 54.99 2.30 -9 -5 7 101.89 3.60 9 5 -7 100.69 3.60 -10 -5 7 1.30 0.70 10 5 -7 1.40 0.70 -11 -5 7 19.50 1.80 11 5 -7 21.00 1.80 -12 -5 7 0.40 0.80 12 5 -7 1.20 0.80 13 5 -7 50.19 2.70 14 5 -7 0.20 0.90 15 5 -7 2.90 1.10 16 5 -7 1.40 1.10 15 -4 6 4.50 1.30 14 -4 6 1.70 1.00 13 -4 6 18.50 2.20 12 -4 6 43.00 2.80 11 -4 6 38.10 2.50 -11 4 -6 33.30 2.10 10 -4 6 103.99 4.10 -10 4 -6 99.19 3.90 9 -4 6 78.79 3.30 -9 4 -6 77.39 3.20 8 -4 6 2.50 0.70 -8 4 -6 2.20 0.60 7 -4 6 190.08 6.10 -7 4 -6 187.48 6.00 6 -4 6 8.60 1.30 -6 4 -6 12.10 1.30 -5 4 -6 1123.39 32.00 -4 4 -6 303.67 9.10 -3 4 -6 6.90 1.10 0 4 -6 649.43 18.50 1 4 -6 16.10 1.00 -2 -4 6 40.40 1.60 2 4 -6 37.50 1.50 -3 -4 6 288.87 8.40 3 4 -6 286.77 8.40 -4 -4 6 159.18 4.80 4 4 -6 153.48 4.70 -5 -4 6 40.80 1.70 5 4 -6 36.30 1.60 -6 -4 6 50.19 2.00 6 4 -6 49.80 2.00 -7 -4 6 60.59 2.30 7 4 -6 59.89 2.30 -8 -4 6 2.40 0.60 8 4 -6 3.10 0.60 -9 -4 6 18.90 1.40 9 4 -6 19.80 1.50 -10 -4 6 0.20 0.60 10 4 -6 1.20 0.70 -11 -4 6 28.40 1.80 11 4 -6 26.20 1.90 -12 -4 6 4.80 0.90 12 4 -6 5.00 0.90 13 4 -6 67.59 3.10 14 4 -6 11.00 1.80 15 4 -6 3.00 1.00 16 4 -6 2.00 1.00 16 -3 5 1.50 1.20 15 -3 5 15.70 2.20 14 -3 5 0.50 0.90 13 -3 5 1.00 0.90 12 -3 5 0.90 0.90 -12 3 -5 1.90 0.80 11 -3 5 16.10 1.90 -11 3 -5 17.50 1.70 -10 3 -5 8.40 1.30 9 -3 5 21.60 1.80 -9 3 -5 21.10 1.60 8 -3 5 55.29 2.50 -8 3 -5 52.89 2.40 7 -3 5 46.10 2.20 -7 3 -5 44.70 2.10 -6 3 -5 135.59 4.50 5 -3 5 160.38 5.20 -5 3 -5 164.08 5.20 -4 3 -5 3.20 0.60 -3 3 -5 853.11 24.30 -1 -3 5 2197.08 61.99 -2 -3 5 128.39 3.90 -3 -3 5 88.79 2.90 3 3 -5 94.49 2.90 -4 -3 5 48.70 1.80 4 3 -5 49.10 1.80 -5 -3 5 36.60 1.60 5 3 -5 37.00 1.50 -6 -3 5 158.98 4.90 6 3 -5 155.98 4.90 -7 -3 5 53.69 2.10 -8 -3 5 82.69 2.90 8 3 -5 79.09 2.90 -9 -3 5 13.00 1.20 9 3 -5 14.20 1.30 -10 -3 5 88.59 3.20 10 3 -5 86.39 3.30 -11 -3 5 1.10 0.60 11 3 -5 0.50 0.70 -12 -3 5 20.10 1.70 12 3 -5 18.30 1.90 -13 -3 5 29.10 2.00 13 3 -5 25.30 2.10 14 3 -5 -0.40 0.80 15 3 -5 -1.10 0.90 16 3 -5 7.10 1.40 17 3 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58.99 3.00 12 4 -2 58.29 2.90 -12 -4 2 55.79 2.50 11 4 -2 5.90 1.00 -11 -4 2 4.30 0.80 10 4 -2 10.80 1.20 -10 -4 2 8.10 1.00 9 4 -2 58.59 2.50 -9 -4 2 56.89 2.30 8 4 -2 102.59 3.50 -8 -4 2 98.39 3.40 7 4 -2 309.17 9.30 -7 -4 2 320.17 9.30 6 4 -2 2.10 0.50 -6 -4 2 2.90 0.50 5 4 -2 105.19 3.50 -5 -4 2 111.59 3.40 4 4 -2 0.50 0.30 -4 -4 2 1.10 0.30 3 4 -2 204.48 5.90 -3 -4 2 194.08 5.80 -3 -4 2 204.88 5.90 2 4 -2 14.50 0.70 -2 -4 2 11.60 0.70 -2 -4 2 12.30 0.70 1 4 -2 25.90 1.00 1 4 -2 24.60 0.90 -1 -4 2 22.80 0.90 -1 -4 2 25.20 0.90 0 4 -2 1885.61 52.89 0 4 -2 1867.91 52.39 0 -4 2 1830.42 52.29 0 -4 2 1924.71 52.89 -1 4 -2 194.18 5.70 1 -4 2 206.08 5.70 -2 4 -2 583.74 16.50 -2 4 -2 584.14 16.60 2 -4 2 595.04 16.40 -3 4 -2 265.27 7.40 -3 4 -2 260.07 7.60 3 -4 2 255.37 7.60 -4 4 -2 1.30 0.40 -4 4 -2 1.70 0.30 4 -4 2 1.50 0.40 -5 4 -2 569.94 16.00 5 -4 2 545.95 16.00 -6 4 -2 8.20 1.00 6 -4 2 6.00 1.10 -7 4 -2 36.70 1.70 7 -4 2 40.40 1.90 -8 4 -2 134.69 4.40 8 -4 2 134.59 4.50 -9 4 -2 12.30 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86.09 2.90 -4 5 -3 86.49 2.70 4 -5 3 83.29 2.90 -5 5 -3 70.39 2.30 -5 5 -3 69.69 2.50 5 -5 3 65.89 2.50 -6 5 -3 65.79 2.50 6 -5 3 65.69 2.60 -7 5 -3 0.10 0.50 7 -5 3 0.10 0.60 -8 5 -3 0.00 0.50 8 -5 3 0.20 0.60 -9 5 -3 1.80 0.60 9 -5 3 1.50 0.70 -10 5 -3 92.99 3.50 10 -5 3 94.39 3.70 -11 5 -3 60.89 2.70 11 -5 3 50.39 2.80 -12 5 -3 80.09 3.40 12 -5 3 75.19 3.60 13 -5 3 22.60 2.40 14 -5 3 12.40 2.30 15 -5 3 21.40 2.60 16 -5 3 -0.20 1.30 16 6 -4 39.50 3.00 15 6 -4 1.90 1.00 14 6 -4 6.10 1.10 13 6 -4 125.59 4.80 12 6 -4 162.28 5.60 -12 -6 4 159.18 5.40 11 6 -4 2.10 0.80 -11 -6 4 2.30 0.70 10 6 -4 14.20 1.60 -10 -6 4 17.70 1.40 9 6 -4 0.80 0.60 -9 -6 4 -0.20 0.50 8 6 -4 10.50 1.30 -8 -6 4 11.00 1.20 7 6 -4 0.60 0.50 -7 -6 4 0.80 0.50 6 6 -4 16.40 1.20 -6 -6 4 17.00 1.20 5 6 -4 0.90 0.50 -5 -6 4 0.20 0.40 4 6 -4 112.69 3.50 -4 -6 4 107.59 3.50 -4 -6 4 114.69 3.50 3 6 -4 210.08 6.10 -3 -6 4 204.28 6.10 -3 -6 4 202.48 6.00 2 6 -4 129.19 3.80 2 6 -4 119.79 3.70 -2 -6 4 120.09 3.70 -2 -6 4 125.89 3.80 1 6 -4 2.50 0.40 1 6 -4 3.50 0.50 -1 -6 4 2.30 0.30 -1 -6 4 2.40 0.40 0 6 -4 60.89 1.90 0 6 -4 61.69 2.00 0 -6 4 60.59 1.90 -1 6 -4 6.20 0.60 -1 6 -4 6.70 0.80 1 -6 4 7.00 0.60 -2 6 -4 103.39 3.20 2 -6 4 112.99 3.20 -3 6 -4 1.00 0.50 -3 6 -4 1.10 0.30 -4 6 -4 31.90 1.30 -4 6 -4 33.80 1.60 -5 6 -4 0.90 0.40 -5 6 -4 0.00 0.50 -6 6 -4 166.78 4.90 -6 6 -4 154.78 5.10 6 -6 4 163.58 5.20 -7 6 -4 227.18 7.00 7 -6 4 227.38 7.10 -8 6 -4 0.50 0.60 8 -6 4 0.30 0.70 -9 6 -4 3.00 0.80 9 -6 4 4.30 0.90 -10 6 -4 28.50 2.00 10 -6 4 30.80 2.20 -11 6 -4 43.70 2.50 11 -6 4 49.70 2.80 -12 6 -4 20.20 2.00 12 -6 4 22.80 2.30 13 -6 4 16.00 2.20 14 -6 4 25.40 2.60 15 -6 4 4.80 1.30 16 -6 4 3.20 1.50 16 7 -5 1.50 1.30 15 7 -5 1.60 1.10 14 7 -5 24.90 2.30 13 7 -5 21.30 2.10 12 7 -5 70.49 3.30 -12 -7 5 76.59 3.20 11 7 -5 60.99 2.90 -11 -7 5 60.69 2.70 10 7 -5 37.20 2.20 -10 -7 5 38.70 2.00 9 7 -5 27.50 1.80 -9 -7 5 25.30 1.60 8 7 -5 -0.40 0.50 -8 -7 5 0.40 0.50 7 7 -5 51.79 2.20 -7 -7 5 52.49 2.10 6 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358.46 10.10 4 5 -2 9.60 0.90 -4 -5 2 11.60 0.80 -4 -5 2 9.90 0.90 3 5 -2 26.60 1.10 -3 -5 2 27.20 1.10 -3 -5 2 25.60 1.20 2 5 -2 121.99 3.60 2 5 -2 116.69 3.60 -2 -5 2 116.49 3.60 -2 -5 2 121.79 3.50 1 5 -2 1.70 0.30 1 5 -2 1.40 0.30 -1 -5 2 1.00 0.30 -1 -5 2 1.90 0.30 0 5 -2 33.90 1.20 0 5 -2 36.20 1.20 0 -5 2 32.90 1.20 0 -5 2 32.80 1.20 -1 5 -2 12.20 0.70 -1 5 -2 12.60 0.70 -2 5 -2 2.30 0.40 -2 5 -2 1.40 0.20 -3 5 -2 15.50 0.90 -3 5 -2 14.50 0.80 3 -5 2 15.20 0.80 -4 5 -2 26.70 1.10 -4 5 -2 25.60 1.30 4 -5 2 25.90 1.30 -5 5 -2 604.24 17.30 -5 5 -2 616.24 17.00 5 -5 2 591.34 17.30 -6 5 -2 9.10 1.00 -6 5 -2 9.00 0.90 6 -5 2 10.10 1.20 -7 5 -2 108.39 3.60 -7 5 -2 108.69 3.50 7 -5 2 106.59 3.70 -8 5 -2 49.00 2.10 8 -5 2 46.00 2.20 -9 5 -2 13.10 1.30 9 -5 2 11.70 1.50 -10 5 -2 117.49 4.10 10 -5 2 112.49 4.20 -11 5 -2 1.00 0.70 11 -5 2 0.20 0.90 -12 5 -2 59.59 2.90 12 -5 2 54.69 3.00 -13 5 -2 14.50 2.10 13 -5 2 17.30 2.20 14 -5 2 5.00 1.30 15 -5 2 8.30 1.40 16 -5 2 0.80 1.40 16 6 -3 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11 -8 29.10 2.00 -10 11 -8 10.60 1.50 -10 11 -8 12.00 1.70 -11 11 -8 46.00 2.50 -12 11 -8 2.00 0.80 -13 11 -8 1.20 0.90 13 12 -9 28.10 2.60 12 12 -9 2.00 1.10 11 12 -9 -0.30 0.90 -11 -12 9 -0.30 1.20 10 12 -9 46.90 2.70 -10 -12 9 46.70 3.10 9 12 -9 13.70 1.90 -9 -12 9 13.70 1.90 -9 -12 9 15.60 2.40 8 12 -9 -1.50 0.80 -8 -12 9 1.30 0.90 7 12 -9 40.40 2.20 -7 -12 9 37.10 2.40 -7 -12 9 41.30 2.20 6 12 -9 31.00 1.90 -6 -12 9 32.60 1.90 -6 -12 9 32.20 2.10 5 12 -9 2.90 0.70 -5 -12 9 3.20 0.70 -5 -12 9 2.80 0.70 4 12 -9 0.90 0.60 -4 -12 9 0.10 0.70 -4 -12 9 0.70 0.60 3 12 -9 35.70 1.80 -3 -12 9 35.20 1.90 -3 -12 9 35.70 1.80 2 12 -9 4.30 0.70 -2 -12 9 3.10 0.60 -2 -12 9 5.10 0.80 1 12 -9 0.80 0.60 1 12 -9 1.00 0.50 -1 -12 9 1.00 0.50 0 12 -9 3.20 0.70 0 -12 9 2.80 0.50 -1 12 -9 -0.50 0.50 -1 12 -9 -0.60 0.60 1 -12 9 0.00 0.40 -2 12 -9 11.20 1.40 -2 12 -9 8.90 1.20 -3 12 -9 32.00 1.70 -3 12 -9 32.40 1.90 -4 12 -9 1.50 0.80 -4 12 -9 0.70 0.60 -4 12 -9 0.90 0.80 -5 12 -9 86.09 3.60 -5 12 -9 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2.40 -8 5 -9 1.90 0.80 -7 5 -9 12.30 1.50 -6 5 -9 50.29 2.40 -5 5 -9 11.50 1.30 -4 5 -9 2.00 0.60 -3 5 -9 50.89 2.20 -1 5 -9 6.40 1.20 0 5 -9 382.66 11.20 1 5 -9 176.48 5.40 -2 -5 9 56.99 2.30 2 5 -9 60.19 2.30 -3 -5 9 42.00 1.90 3 5 -9 43.00 1.80 -4 -5 9 6.60 1.10 4 5 -9 5.90 1.00 -5 -5 9 71.99 2.70 5 5 -9 72.09 2.60 -6 -5 9 160.88 5.10 6 5 -9 163.28 5.10 -7 -5 9 319.77 9.40 7 5 -9 311.57 9.40 -8 -5 9 21.20 1.40 8 5 -9 24.50 1.50 -9 -5 9 4.90 0.80 9 5 -9 8.40 1.30 -10 -5 9 74.99 3.00 10 5 -9 75.59 3.00 -11 -5 9 15.30 1.60 11 5 -9 18.80 1.70 12 5 -9 5.30 1.00 13 5 -9 -0.90 0.80 14 5 -9 35.30 2.40 15 5 -9 -1.50 1.00 16 5 -9 22.80 2.60 15 -4 8 -0.30 1.20 14 -4 8 -1.80 1.00 13 -4 8 8.50 1.40 12 -4 8 0.60 1.00 11 -4 8 194.48 6.80 10 -4 8 253.97 8.20 -10 4 -8 238.78 8.00 9 -4 8 118.39 4.50 -9 4 -8 117.79 4.30 -8 4 -8 137.39 4.80 -7 4 -8 14.50 1.50 -6 4 -8 63.49 2.70 -5 4 -8 0.80 0.50 -4 4 -8 2.80 0.70 -3 4 -8 154.38 5.00 0 4 -8 1.10 0.50 1 4 -8 5.90 1.00 -2 -4 8 195.58 5.90 2 4 -8 193.38 5.90 -3 -4 8 0.10 0.50 3 4 -8 0.50 0.50 -4 -4 8 75.79 2.20 -4 -4 8 67.09 2.50 4 4 -8 67.79 2.50 -5 -4 8 285.17 8.30 5 4 -8 274.67 8.30 -6 -4 8 48.80 2.10 6 4 -8 51.59 2.10 -8 -4 8 21.30 1.40 8 4 -8 24.00 1.50 -9 -4 8 21.60 1.50 9 4 -8 24.70 1.60 -10 -4 8 4.60 0.80 10 4 -8 4.80 0.80 -11 -4 8 2.00 0.80 11 4 -8 1.70 0.80 -12 -4 8 0.80 0.70 12 4 -8 -0.10 0.70 13 4 -8 1.30 0.90 14 4 -8 -0.30 0.90 15 4 -8 19.20 2.30 16 4 -8 7.50 1.40 14 -3 7 -0.70 1.00 13 -3 7 1.10 0.90 12 -3 7 0.70 0.80 -11 3 -7 -0.30 0.70 10 -3 7 281.67 9.00 -10 3 -7 276.27 8.80 9 -3 7 279.47 9.20 -9 3 -7 308.07 9.20 8 -3 7 15.90 1.60 -8 3 -7 15.10 1.40 7 -3 7 23.60 1.80 -7 3 -7 26.00 1.60 -6 3 -7 425.56 12.60 -5 3 -7 19.30 1.40 -4 3 -7 49.10 2.20 -3 3 -7 109.99 3.70 0 3 -7 14.50 1.10 1 3 -7 2508.75 70.89 -2 -3 7 55.49 2.10 2 3 -7 55.09 2.00 -3 -3 7 547.05 15.30 -3 -3 7 556.14 15.70 3 3 -7 542.15 15.60 -4 -3 7 109.49 3.20 -4 -3 7 107.19 3.50 4 3 -7 107.69 3.50 -5 -3 7 582.94 16.70 5 3 -7 585.94 16.70 -6 -3 7 181.98 5.60 6 3 -7 186.28 5.60 -7 -3 7 414.36 12.00 7 3 -7 411.76 12.00 -8 -3 7 4.50 0.70 -9 -3 7 34.40 1.80 9 3 -7 34.20 1.80 -10 -3 7 18.90 1.50 10 3 -7 19.70 1.60 -11 -3 7 0.90 0.70 11 3 -7 0.90 0.80 -12 -3 7 -0.40 0.60 12 3 -7 1.60 0.70 13 3 -7 11.10 1.80 14 3 -7 2.00 0.90 15 3 -7 0.80 1.10 16 3 -7 14.50 2.40 17 3 -7 3.60 1.40 15 -2 6 19.50 2.50 14 -2 6 14.30 2.20 13 -2 6 0.70 0.90 12 -2 6 90.79 3.90 11 -2 6 54.29 2.90 -11 2 -6 48.90 2.60 10 -2 6 10.90 1.80 -10 2 -6 8.00 1.40 9 -2 6 3.50 0.90 -9 2 -6 2.90 0.80 8 -2 6 1.40 0.70 -8 2 -6 0.40 0.50 7 -2 6 17.50 1.60 -7 2 -6 18.50 1.30 6 -2 6 8.20 1.30 5 -2 6 195.28 6.20 -5 2 -6 196.58 6.10 -4 2 -6 83.49 3.00 -3 2 -6 597.74 17.20 -2 2 -6 104.99 3.20 -2 2 -6 108.69 3.50 -1 2 -6 201.58 5.70 0 2 -6 177.08 5.30 -1 -2 6 2289.67 65.49 1 2 -6 2355.26 65.69 -2 -2 6 0.00 0.40 2 2 -6 0.00 0.30 -3 -2 6 18.50 1.00 -3 -2 6 19.30 0.80 3 2 -6 19.90 1.00 -4 -2 6 207.78 6.10 -4 -2 6 211.68 5.90 4 2 -6 201.28 6.10 -5 -2 6 85.89 2.80 5 2 -6 77.09 2.70 -6 -2 6 106.89 3.40 6 2 -6 103.89 3.40 -7 -2 6 2.40 0.60 7 2 -6 2.40 0.60 -8 -2 6 27.20 1.50 8 2 -6 25.50 1.50 -9 -2 6 1.80 0.60 9 2 -6 2.20 0.60 -10 -2 6 42.00 2.00 10 2 -6 39.70 2.10 -11 -2 6 1.30 0.60 11 2 -6 0.90 0.70 -12 -2 6 2.90 0.80 12 2 -6 1.90 0.80 -13 -2 6 1.80 0.70 13 2 -6 1.40 0.80 14 2 -6 33.60 2.40 15 2 -6 -0.20 1.00 16 2 -6 23.10 2.70 17 2 -6 16.20 2.90 16 -1 5 3.60 1.30 15 -1 5 3.20 1.10 14 -1 5 37.30 2.70 13 -1 5 5.60 1.20 12 -1 5 3.10 1.00 -12 1 -5 4.10 0.90 11 -1 5 17.00 2.00 -11 1 -5 20.60 1.60 10 -1 5 74.79 3.30 -10 1 -5 80.39 3.10 9 -1 5 22.30 1.80 -9 1 -5 24.20 1.50 8 -1 5 0.40 0.60 -8 1 -5 -0.30 0.40 7 -1 5 49.20 2.30 -7 1 -5 45.10 2.10 6 -1 5 60.69 2.50 -6 1 -5 57.29 2.30 5 -1 5 227.68 7.00 -5 1 -5 229.18 7.00 4 -1 5 1393.96 40.40 -4 1 -5 1465.45 40.50 -3 1 -5 283.77 8.40 -2 1 -5 329.47 9.40 -2 1 -5 336.27 9.70 -1 1 -5 418.96 11.80 0 -1 5 3.50 0.50 0 1 -5 3.00 0.50 0 1 -5 2.30 0.40 -1 -1 5 1396.96 38.60 -1 -1 5 1356.66 39.30 1 1 -5 1409.16 39.20 1 1 -5 1382.46 38.70 -2 -1 5 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155.98 4.60 0 3 -8 0.30 0.50 1 3 -8 598.74 17.10 -2 -3 8 17.60 1.30 2 3 -8 18.80 1.20 -3 -3 8 15.30 1.20 -3 -3 8 16.30 0.80 -4 -3 8 20.70 1.40 -4 -3 8 24.90 1.00 4 3 -8 24.70 1.30 -5 -3 8 20.90 1.00 -5 -3 8 20.00 1.30 5 3 -8 22.90 1.30 -6 -3 8 66.89 2.50 -6 -3 8 64.59 2.20 6 3 -8 66.89 2.50 -7 -3 8 56.89 2.30 7 3 -8 61.39 2.30 -8 -3 8 0.30 0.50 8 3 -8 1.00 0.50 -9 -3 8 14.90 1.30 9 3 -8 17.70 1.40 -10 -3 8 96.69 3.50 10 3 -8 98.29 3.60 -11 -3 8 6.20 0.90 11 3 -8 6.20 0.90 -12 -3 8 6.50 1.00 12 3 -8 5.00 1.00 13 3 -8 1.40 0.80 14 3 -8 1.00 1.10 15 3 -8 3.80 1.10 16 3 -8 -0.40 1.10 15 -2 7 2.60 1.30 14 -2 7 0.80 1.10 13 -2 7 1.50 1.00 12 -2 7 47.50 2.90 11 -2 7 1.10 0.90 -11 2 -7 0.60 0.60 10 -2 7 26.60 2.20 -10 2 -7 25.90 1.80 9 -2 7 0.10 0.70 -9 2 -7 1.20 0.60 8 -2 7 151.58 5.20 -8 2 -7 151.58 5.10 -7 2 -7 68.49 2.70 -6 2 -7 115.49 4.00 -5 2 -7 7.70 1.00 -4 2 -7 362.36 10.80 -3 2 -7 1010.40 27.90 -3 2 -7 946.21 27.30 -2 2 -7 148.49 4.40 -1 2 -7 3.70 0.60 0 -2 7 195.28 5.60 0 2 -7 192.68 5.60 0 2 -7 196.38 5.90 -1 -2 7 368.26 10.80 1 2 -7 402.36 11.10 -2 -2 7 104.29 3.30 -2 -2 7 94.89 3.10 2 2 -7 102.79 3.00 2 2 -7 111.19 3.30 -3 -2 7 76.49 2.40 -3 -2 7 75.59 2.60 3 2 -7 80.19 2.60 -4 -2 7 40.00 1.70 -4 -2 7 41.40 1.50 4 2 -7 43.70 1.70 -5 -2 7 67.99 2.40 -5 -2 7 70.19 2.20 5 2 -7 65.99 2.40 -6 -2 7 8.50 1.00 6 2 -7 9.60 1.00 -7 -2 7 14.70 1.20 7 2 -7 17.10 1.30 -8 -2 7 50.99 2.10 8 2 -7 50.69 2.10 -9 -2 7 1.60 0.60 9 2 -7 1.40 0.60 -10 -2 7 14.20 1.40 10 2 -7 12.90 1.50 -11 -2 7 8.30 1.40 11 2 -7 10.50 1.60 -12 -2 7 0.30 0.70 12 2 -7 0.20 0.80 -13 -2 7 2.10 0.90 13 2 -7 0.80 0.90 14 2 -7 0.10 0.80 15 2 -7 8.30 1.30 16 2 -7 -0.30 1.10 17 2 -7 8.70 1.70 15 -1 6 3.00 1.20 14 -1 6 -0.40 1.00 13 -1 6 12.60 2.10 12 -1 6 26.80 2.30 11 -1 6 38.40 2.50 -11 1 -6 40.10 2.20 10 -1 6 28.90 2.30 -10 1 -6 34.00 1.90 9 -1 6 42.10 2.40 -9 1 -6 44.40 2.10 8 -1 6 32.50 2.00 -8 1 -6 29.10 1.70 7 -1 6 1.40 0.60 -7 1 -6 0.30 0.50 6 -1 6 14.00 1.40 -6 1 -6 12.90 1.20 5 -1 6 339.47 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1.00 0.80 13 0 -5 2.20 0.90 14 0 -5 1.10 1.00 15 0 -5 4.60 1.20 16 0 -5 4.00 1.30 17 0 -5 15.20 2.70 16 1 4 0.00 1.20 15 1 4 -1.00 1.00 14 1 4 1.50 1.10 13 1 4 1.90 0.90 12 1 4 2.20 0.90 -12 -1 -4 1.90 0.80 11 1 4 10.90 1.80 -11 -1 -4 14.10 1.40 10 1 4 112.09 4.30 -10 -1 -4 121.99 4.20 9 1 4 11.50 1.60 -9 -1 -4 14.30 1.30 8 1 4 13.20 1.50 -8 -1 -4 15.30 1.20 7 1 4 3.30 0.70 -7 -1 -4 4.30 0.70 6 1 4 420.76 12.40 -6 -1 -4 417.56 12.30 5 1 4 324.97 9.70 -5 -1 -4 331.47 9.70 4 1 4 187.08 5.90 -4 -1 -4 196.98 5.80 -4 -1 -4 195.48 5.90 3 1 4 169.88 5.30 -3 -1 -4 178.58 5.20 -3 -1 -4 180.48 5.30 2 1 4 13.60 0.90 -2 -1 -4 15.40 0.90 -2 -1 -4 15.60 0.80 1 1 4 15.80 0.90 0 1 4 946.61 26.70 0 -1 -4 945.71 26.40 -1 1 4 13.80 0.80 1 -1 -4 12.50 0.70 -2 1 4 1268.87 35.90 -2 1 4 1209.58 35.50 2 -1 -4 1307.97 35.80 2 -1 -4 1301.47 35.90 -3 1 4 4899.91 138.29 -3 1 4 5044.90 139.29 3 -1 -4 4984.20 139.29 3 -1 -4 4921.01 138.09 -4 1 4 294.97 8.30 -4 1 4 286.47 8.20 4 -1 -4 280.57 8.30 -5 1 4 63.39 2.10 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1.00 -10 -7 13 3.60 0.80 10 7 -13 5.00 1.00 -11 -7 13 -1.30 0.70 11 7 -13 0.20 0.90 -12 -7 13 24.80 2.20 12 7 -13 25.80 2.10 -13 -7 13 4.90 1.10 13 7 -13 4.70 1.10 -14 -7 13 -1.80 1.10 14 7 -13 -1.20 1.10 -7 6 -12 5.60 0.90 -6 6 -12 5.80 0.90 -5 6 -12 -0.60 0.60 -4 6 -12 7.50 1.10 -4 6 -12 9.20 1.20 -2 6 -12 0.30 0.60 -1 6 -12 108.59 3.90 0 6 -12 32.90 1.80 1 6 -12 12.40 1.30 2 6 -12 3.90 0.70 -3 -6 12 1.60 0.60 3 6 -12 3.20 0.70 -4 -6 12 0.10 0.50 4 6 -12 0.70 0.50 -5 -6 12 1.30 0.60 5 6 -12 1.00 0.60 -6 -6 12 0.30 0.60 6 6 -12 0.20 0.60 -7 -6 12 0.60 0.50 -7 -6 12 1.20 0.60 7 6 -12 0.80 0.60 -8 -6 12 2.90 0.60 -8 -6 12 1.80 0.70 8 6 -12 2.30 0.80 -9 -6 12 79.29 2.90 -9 -6 12 81.09 3.20 9 6 -12 78.29 3.20 -10 -6 12 49.10 2.30 -10 -6 12 47.70 2.50 10 6 -12 47.80 2.50 -11 -6 12 -0.10 0.80 11 6 -12 1.40 0.90 12 6 -12 -0.30 0.80 13 6 -12 -0.10 1.00 14 6 -12 2.70 1.20 15 6 -12 -1.00 1.10 -8 5 -11 111.09 4.20 -7 5 -11 22.60 1.80 -6 5 -11 90.89 3.50 -5 5 -11 10.10 1.20 -4 5 -11 0.10 0.40 -4 5 -11 0.20 0.50 -3 5 -11 -0.20 0.40 -3 5 -11 0.10 0.50 -1 5 -11 2.20 0.80 0 5 -11 204.68 6.40 1 5 -11 388.86 11.40 2 5 -11 399.86 11.70 -3 -5 11 0.20 0.50 3 5 -11 1.00 0.60 -4 -5 11 29.10 1.60 4 5 -11 31.70 1.60 -5 -5 11 5.50 0.80 5 5 -11 4.60 0.70 -6 -5 11 25.40 1.30 -6 -5 11 26.90 1.60 6 5 -11 27.30 1.60 -7 -5 11 127.39 4.40 -7 -5 11 136.19 4.10 7 5 -11 134.19 4.40 -8 -5 11 0.10 0.50 -8 -5 11 1.70 0.60 8 5 -11 1.10 0.60 -9 -5 11 38.80 2.20 -9 -5 11 41.50 1.90 9 5 -11 44.20 2.20 -10 -5 11 149.19 5.30 -10 -5 11 167.88 5.10 10 5 -11 165.08 5.40 -11 -5 11 9.20 1.60 11 5 -11 13.50 1.70 12 5 -11 16.10 1.90 13 5 -11 5.20 1.10 14 5 -11 -0.60 0.90 15 5 -11 4.10 1.20 -9 4 -10 220.38 7.30 -8 4 -10 11.80 1.40 -7 4 -10 22.50 1.60 -6 4 -10 16.40 1.50 -5 4 -10 2.60 0.60 -4 4 -10 1.20 0.50 -4 4 -10 0.60 0.40 -3 4 -10 19.80 1.40 -3 4 -10 16.80 1.00 -2 4 -10 43.40 1.60 -1 4 -10 -0.60 0.60 0 4 -10 301.47 9.00 1 4 -10 198.88 6.10 2 4 -10 296.87 8.80 -3 -4 10 8.20 1.10 3 4 -10 9.50 1.10 -4 -4 10 2.80 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26.60 1.80 -5 -13 7 27.40 2.10 -5 -13 7 28.10 2.00 4 13 -7 5.50 0.80 -4 -13 7 4.60 0.90 -4 -13 7 6.00 0.90 3 13 -7 2.90 0.70 3 13 -7 2.20 0.60 -3 -13 7 2.00 0.80 -3 -13 7 3.80 0.90 2 13 -7 8.90 1.30 2 13 -7 9.50 1.40 -2 -13 7 10.20 1.50 -2 -13 7 6.60 0.90 1 13 -7 89.29 3.10 1 13 -7 92.89 3.30 -1 -13 7 91.19 3.20 0 13 -7 9.80 1.50 0 13 -7 9.40 1.30 0 -13 7 9.90 1.30 -1 13 -7 49.70 2.20 -1 13 -7 46.20 2.10 1 -13 7 52.39 2.20 -2 13 -7 188.28 5.90 -2 13 -7 183.08 5.90 2 -13 7 194.08 5.80 -3 13 -7 1.70 0.70 -3 13 -7 2.20 0.70 3 -13 7 2.50 0.60 -4 13 -7 0.20 0.60 -4 13 -7 0.50 0.70 -4 13 -7 1.50 0.80 4 -13 7 0.30 0.60 -5 13 -7 11.80 1.60 -5 13 -7 13.40 1.90 -6 13 -7 35.30 2.50 -6 13 -7 35.10 2.20 -7 13 -7 0.80 0.80 -7 13 -7 1.60 1.10 -8 13 -7 6.10 1.30 -8 13 -7 5.00 1.00 -9 13 -7 121.19 4.80 -9 13 -7 122.79 4.50 -10 13 -7 17.60 2.10 -10 13 -7 15.70 2.70 -11 13 -7 -1.40 0.80 -12 13 -7 -1.00 0.90 -13 13 -7 1.40 1.10 12 14 -8 0.40 1.40 11 14 -8 1.80 1.20 10 14 -8 -0.20 1.00 9 14 -8 2.30 1.10 -9 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2.20 -1 7 -14 55.39 2.60 0 7 -14 2.10 0.80 1 7 -14 -0.50 0.70 2 7 -14 2.20 0.70 3 7 -14 3.00 0.80 -4 -7 14 22.30 1.70 4 7 -14 23.20 1.70 -5 -7 14 14.00 1.50 5 7 -14 12.40 1.50 -6 -7 14 11.10 1.50 6 7 -14 9.50 1.50 -7 -7 14 4.90 0.90 7 7 -14 4.20 0.80 -8 -7 14 17.20 1.70 -8 -7 14 17.40 1.50 8 7 -14 12.70 1.60 -9 -7 14 14.30 1.60 9 7 -14 13.50 1.70 -10 -7 14 22.70 1.80 10 7 -14 16.80 1.90 -11 -7 14 16.90 1.90 11 7 -14 18.20 2.00 -12 -7 14 7.80 1.10 12 7 -14 8.10 1.30 -13 -7 14 -0.70 1.00 13 7 -14 -0.30 1.10 -14 -7 14 -0.30 1.20 14 7 -14 0.30 1.20 -7 6 -13 74.19 3.40 -6 6 -13 64.59 2.70 -6 6 -13 71.89 3.10 -5 6 -13 0.50 0.60 -5 6 -13 0.10 0.70 -4 6 -13 97.69 3.70 -4 6 -13 96.79 3.30 -3 6 -13 4.70 0.80 -2 6 -13 77.39 3.10 -1 6 -13 9.30 1.50 0 6 -13 11.40 1.40 1 6 -13 41.90 2.10 2 6 -13 13.00 1.40 3 6 -13 5.20 0.80 -4 -6 13 1.70 0.60 4 6 -13 0.80 0.60 -5 -6 13 7.50 1.20 5 6 -13 4.70 0.70 -6 -6 13 0.60 0.60 6 6 -13 0.10 0.60 -7 -6 13 4.90 0.90 -7 -6 13 4.20 0.60 7 6 -13 4.70 0.80 -8 -6 13 2.50 0.90 8 6 -13 3.70 0.90 -9 -6 13 26.90 1.70 -9 -6 13 25.70 1.90 9 6 -13 20.80 1.80 -10 -6 13 23.20 1.80 10 6 -13 22.90 1.90 -11 -6 13 5.20 0.90 11 6 -13 5.30 1.10 -12 -6 13 1.10 0.90 12 6 -13 1.90 1.00 -13 -6 13 -1.60 0.90 13 6 -13 0.30 1.00 -14 -6 13 0.70 1.10 14 6 -13 1.30 1.10 15 6 -13 -1.10 1.20 -8 5 -12 32.90 2.20 -7 5 -12 12.10 1.60 -6 5 -12 4.60 0.80 -5 5 -12 22.20 1.50 -5 5 -12 22.90 1.70 -4 5 -12 4.20 0.80 -4 5 -12 3.40 0.60 -3 5 -12 21.10 1.50 -3 5 -12 19.30 1.30 -2 5 -12 12.50 1.50 -1 5 -12 1.50 0.60 0 5 -12 29.70 1.70 1 5 -12 0.30 0.60 2 5 -12 32.70 1.80 -3 -5 12 3.20 0.70 3 5 -12 3.80 0.70 -4 -5 12 4.20 0.70 4 5 -12 3.90 0.70 -5 -5 12 3.90 0.70 5 5 -12 5.00 0.70 -6 -5 12 19.90 1.50 -6 -5 12 21.80 1.30 6 5 -12 21.00 1.50 -7 -5 12 44.50 2.20 -7 -5 12 47.00 1.90 7 5 -12 44.40 2.10 -8 -5 12 0.70 0.60 -8 -5 12 0.30 0.60 -9 -5 12 211.18 6.20 -9 -5 12 201.28 6.60 9 5 -12 202.78 6.60 -10 -5 12 19.00 1.80 -10 -5 12 17.30 1.70 10 5 -12 18.40 1.80 -11 -5 12 1.90 0.80 11 5 -12 3.60 0.90 -12 -5 12 35.00 2.30 12 5 -12 39.60 2.40 -13 -5 12 10.00 1.20 13 5 -12 15.10 2.10 -14 -5 12 -1.30 1.00 14 5 -12 1.10 1.10 -15 -5 12 6.30 1.30 15 5 -12 8.30 1.40 -8 4 -11 86.19 3.60 -7 4 -11 75.79 3.20 -6 4 -11 0.90 0.60 -6 4 -11 1.70 0.70 -5 4 -11 54.99 2.20 -5 4 -11 58.89 2.60 -4 4 -11 54.29 2.10 -4 4 -11 59.19 2.50 -3 4 -11 84.09 2.80 -3 4 -11 84.39 3.20 -2 4 -11 90.89 2.90 -1 4 -11 67.79 2.70 0 4 -11 11.70 1.50 1 4 -11 176.48 5.60 2 4 -11 123.49 4.10 -3 -4 11 241.98 7.40 3 4 -11 242.48 7.30 -4 -4 11 6.70 0.80 4 4 -11 8.40 1.20 -5 -4 11 31.20 1.70 -5 -4 11 31.20 1.40 5 4 -11 31.30 1.70 -6 -4 11 10.50 1.20 -6 -4 11 11.60 1.00 6 4 -11 12.60 1.20 -7 -4 11 0.20 0.50 -7 -4 11 -0.10 0.50 7 4 -11 0.60 0.60 -8 -4 11 85.39 3.30 -8 -4 11 94.29 3.10 8 4 -11 86.09 3.30 -9 -4 11 0.90 0.60 -9 -4 11 0.80 0.70 9 4 -11 1.10 0.70 -10 -4 11 13.00 1.70 -10 -4 11 14.50 1.60 10 4 -11 18.30 1.80 -11 -4 11 2.30 0.90 -11 -4 11 1.70 0.80 11 4 -11 4.60 1.00 -12 -4 11 -1.20 0.80 12 4 -11 -0.30 0.80 -13 -4 11 22.00 2.20 13 4 -11 27.30 2.20 -14 -4 11 0.30 1.00 14 4 -11 1.10 1.00 -15 -4 11 0.50 1.10 15 4 -11 4.60 1.30 -9 3 -10 128.69 4.70 -8 3 -10 3.10 0.80 -7 3 -10 1.30 0.60 -6 3 -10 23.80 1.70 -5 3 -10 38.70 2.00 -5 3 -10 30.30 1.60 -4 3 -10 11.60 1.30 -4 3 -10 14.10 1.10 -3 3 -10 9.20 1.20 -3 3 -10 9.90 1.00 -2 3 -10 13.30 1.00 -1 3 -10 50.89 1.80 -1 3 -10 50.19 2.20 0 3 -10 0.50 0.60 1 3 -10 148.99 4.70 2 3 -10 23.90 1.50 -3 -3 10 218.68 6.80 3 3 -10 228.28 6.70 -4 -3 10 239.28 7.10 -4 -3 10 240.48 7.40 4 3 -10 258.07 7.40 -5 -3 10 18.40 1.10 -5 -3 10 14.20 1.30 5 3 -10 16.30 1.30 -6 -3 10 82.69 2.70 -6 -3 10 79.79 3.00 6 3 -10 83.99 3.00 -7 -3 10 6.20 1.00 -7 -3 10 4.40 0.70 7 3 -10 4.30 0.70 -8 -3 10 -0.40 0.60 -8 -3 10 0.40 0.50 8 3 -10 0.20 0.60 -9 -3 10 103.89 3.80 -9 -3 10 114.19 3.70 9 3 -10 110.79 3.90 -10 -3 10 21.60 1.70 -10 -3 10 20.30 1.70 10 3 -10 23.90 1.80 -11 -3 10 4.70 0.90 -11 -3 10 3.50 0.80 -12 -3 10 9.50 1.70 -12 -3 10 12.30 1.90 12 3 -10 13.50 1.90 -13 -3 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