# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_201000819_2 _database_code_depnum_ccdc_archive 'CCDC 864644' #TrackingRef '9283_web_deposit_cif_file_0_HidemitsuUno_1327631718.cisEtBCODbisBODIPY.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C34 H40 B2 F4 N4' _chemical_formula_moiety 'C34 H40 B2 F4 N4' _chemical_formula_weight 602.33 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,+Z 3 +X,1/2-Y,1/2+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,-Z 7 -X,1/2+Y,1/2-Z 8 1/2+X,+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 16.8468(3) _cell_length_b 14.7846(2) _cell_length_c 24.5438(4) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 6113.20(17) _cell_formula_units_Z 8 _cell_measurement_reflns_used 44920 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 68.25 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544.00 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.941 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_source 'VariMax Rotating Anode, 40 kV x 30 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 66009 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_theta_max 68.25 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 #============================================================================== # REFINEMENT DATA _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. ; _reflns_number_total 5591 _reflns_number_gt 4660 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5589 _refine_ls_number_parameters 398 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0564P)^2^+1.6944P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_diff_density_max 0.610 _refine_diff_density_min -0.200 _refine_ls_extinction_method none _iucr_refine_instructions_details ; TITL 201000819_2 CELL 1.54187 16.84675 14.78463 24.54381 90.000 90.000 90.000 ZERR 8 0.00030 0.00020 0.00040 0.000 0.000 0.000 LATT 1 SYMM .50-X, .50+Y, +Z SYMM +X, .50-Y, .50+Z SYMM .50-X, -Y, .50+Z SFAC C H B F N UNIT 272 320 16 32 32 SHEL 99999.000000 0.000000 L.S. 5 FMAP 2 PLAN -20 WPDB -2 HTAB BOND $H CONF OMIT 4 1 28 OMIT 1 1 4 TEMP -173.0 ACTA SIZE 0.200 0.180 0.080 WGHT 0.056400 1.694400 FVAR 0.90169 0.00000 F1 4 0.218190 0.681806 0.538332 11.00000 0.03980 0.02639 = 0.03120 -0.00808 -0.00155 0.00735 F2 4 0.299188 0.669762 0.465105 11.00000 0.03814 0.03083 = 0.02601 0.00571 -0.00185 -0.01166 F3 4 0.113439 0.308081 0.195560 11.00000 0.06113 0.03116 = 0.02329 -0.00045 0.00810 0.00121 F4 4 0.005410 0.223619 0.216264 11.00000 0.03499 0.04603 = 0.03795 -0.01296 -0.01243 0.00379 N1 5 0.197863 0.556588 0.476138 11.00000 0.02337 0.02036 = 0.02159 0.00035 0.00238 0.00036 N2 5 0.315459 0.561498 0.537674 11.00000 0.02450 0.02195 = 0.02050 -0.00107 0.00162 -0.00163 N3 5 0.073313 0.301699 0.289904 11.00000 0.02564 0.02812 = 0.01957 -0.00157 -0.00104 0.00203 N4 5 0.134012 0.167794 0.243883 11.00000 0.02798 0.02817 = 0.01923 -0.00422 0.00039 -0.00057 C1 1 0.138538 0.581114 0.441010 11.00000 0.02485 0.02386 = 0.01990 -0.00003 0.00308 0.00276 C2 1 0.097743 0.502973 0.425317 11.00000 0.02434 0.02298 = 0.01983 -0.00096 0.00302 0.00275 C3 1 0.133313 0.429167 0.450770 11.00000 0.02216 0.02340 = 0.01885 -0.00165 0.00402 0.00153 C4 1 0.196078 0.462665 0.483132 11.00000 0.02226 0.01878 = 0.02065 -0.00158 0.00357 0.00043 C5 1 0.251538 0.419922 0.516739 11.00000 0.02308 0.01988 = 0.02227 -0.00092 0.00447 -0.00001 AFIX 43 H5 2 0.248789 0.356173 0.521213 11.00000 -1.20000 AFIX 0 C6 1 0.310431 0.467611 0.543750 11.00000 0.02357 0.01937 = 0.02292 -0.00128 0.00255 0.00096 C7 1 0.377481 0.438034 0.574861 11.00000 0.02497 0.02503 = 0.02204 -0.00405 0.00129 0.00112 C8 1 0.422591 0.514287 0.585789 11.00000 0.02509 0.02582 = 0.01967 -0.00346 0.00231 -0.00073 C9 1 0.382675 0.589352 0.562540 11.00000 0.02679 0.02579 = 0.01809 -0.00252 0.00302 -0.00397 C10 1 0.041369 0.385002 0.299249 11.00000 0.02349 0.02907 = 0.02288 -0.00037 0.00024 0.00256 C11 1 0.047519 0.404071 0.354925 11.00000 0.02341 0.02552 = 0.02138 -0.00134 0.00028 0.00145 C12 1 0.082834 0.330821 0.380379 11.00000 0.02126 0.02412 = 0.02153 -0.00159 0.00100 -0.00045 C13 1 0.099509 0.265970 0.339765 11.00000 0.02337 0.02743 = 0.01960 -0.00172 -0.00033 -0.00071 C14 1 0.140239 0.184042 0.341526 11.00000 0.02363 0.02640 = 0.02086 -0.00166 -0.00095 -0.00186 AFIX 43 H14 2 0.156119 0.160570 0.375869 11.00000 -1.20000 AFIX 0 C15 1 0.158328 0.135709 0.294833 11.00000 0.02598 0.02930 = 0.02155 -0.00270 -0.00129 -0.00006 C16 1 0.206242 0.056954 0.286825 11.00000 0.02540 0.02836 = 0.02599 -0.00523 -0.00080 0.00072 C17 1 0.210712 0.043227 0.230951 11.00000 0.02589 0.02917 = 0.02588 -0.00709 0.00034 -0.00073 C18 1 0.165364 0.112098 0.205827 11.00000 0.02859 0.02961 = 0.02267 -0.00646 0.00332 -0.00338 C19 1 0.024635 0.480896 0.392286 11.00000 0.02562 0.02413 = 0.02124 -0.00096 -0.00092 0.00433 AFIX 13 H19 2 0.001937 0.534270 0.372701 11.00000 -1.20000 AFIX 0 C20 1 -0.034084 0.437354 0.434384 11.00000 0.02312 0.02938 = 0.02304 -0.00467 -0.00066 0.00149 AFIX 23 H20A 2 -0.050425 0.483350 0.461467 11.00000 -1.20000 H20B 2 -0.082243 0.415869 0.415231 11.00000 -1.20000 AFIX 0 C21 1 0.006455 0.356707 0.463949 11.00000 0.02376 0.02418 = 0.02360 -0.00328 0.00313 -0.00218 AFIX 23 H21A 2 -0.025902 0.301461 0.458828 11.00000 -1.20000 H21B 2 0.009275 0.369542 0.503490 11.00000 -1.20000 AFIX 0 C22 1 0.092662 0.339760 0.441333 11.00000 0.02347 0.02161 = 0.01885 -0.00164 0.00008 -0.00005 AFIX 13 H22 2 0.120335 0.287267 0.458636 11.00000 -1.20000 AFIX 0 C23 1 0.126218 0.676321 0.422470 11.00000 0.03165 0.02496 = 0.03080 0.00293 0.00096 0.00197 AFIX 133 H23A 2 0.122383 0.716187 0.454261 11.00000 -1.50000 H23B 2 0.077069 0.680115 0.401234 11.00000 -1.50000 H23C 2 0.171120 0.695121 0.399751 11.00000 -1.50000 AFIX 0 C24 1 0.397532 0.343439 0.591579 11.00000 0.02948 0.02374 = 0.04528 -0.00491 -0.01030 0.00236 AFIX 23 H24A 2 0.453208 0.330698 0.581204 11.00000 -1.20000 H24B 2 0.363174 0.301016 0.571140 11.00000 -1.20000 AFIX 0 C25 1 0.387668 0.325299 0.652566 11.00000 0.03895 0.03196 = 0.05672 0.01540 -0.00661 -0.00101 AFIX 133 H25A 2 0.419969 0.368387 0.673280 11.00000 -1.50000 H25B 2 0.404983 0.263520 0.660820 11.00000 -1.50000 H25C 2 0.331732 0.332369 0.662669 11.00000 -1.50000 AFIX 0 C26 1 0.504074 0.518645 0.610590 11.00000 0.02611 0.03094 = 0.02365 -0.00391 -0.00072 -0.00281 AFIX 23 H26A 2 0.510925 0.467868 0.636461 11.00000 -1.20000 H26B 2 0.509923 0.575892 0.631125 11.00000 -1.20000 AFIX 0 C27 1 0.567861 0.513420 0.566564 11.00000 0.02528 0.08231 = 0.03001 -0.00795 0.00056 -0.00136 AFIX 133 H27A 2 0.562937 0.456023 0.546880 11.00000 -1.50000 H27B 2 0.620441 0.517071 0.583503 11.00000 -1.50000 H27C 2 0.561172 0.563811 0.541033 11.00000 -1.50000 AFIX 0 C28 1 0.410173 0.684816 0.562542 11.00000 0.03859 0.02651 = 0.02643 0.00041 -0.00432 -0.00830 AFIX 133 H28A 2 0.448532 0.693726 0.533009 11.00000 -1.50000 H28B 2 0.435469 0.698607 0.597525 11.00000 -1.50000 H28C 2 0.364659 0.725093 0.557095 11.00000 -1.50000 AFIX 0 C29 1 0.007062 0.442513 0.255243 11.00000 0.03432 0.03624 = 0.02200 0.00073 -0.00178 0.00621 AFIX 133 H29A 2 0.048931 0.459234 0.229418 11.00000 -1.50000 H29B 2 -0.015773 0.497367 0.271267 11.00000 -1.50000 H29C 2 -0.034520 0.408732 0.236122 11.00000 -1.50000 AFIX 0 C30 1 0.245821 0.003244 0.330904 11.00000 0.03169 0.03603 = 0.02666 -0.00814 -0.00494 0.00648 AFIX 23 H30A 2 0.235144 0.032720 0.366373 11.00000 -1.20000 H30B 2 0.303907 0.004593 0.324847 11.00000 -1.20000 AFIX 0 C31 1 0.218859 -0.095291 0.334086 11.00000 0.04715 0.03441 = 0.03257 -0.00373 -0.00667 0.00885 AFIX 133 H31A 2 0.160814 -0.097645 0.336310 11.00000 -1.50000 H31B 2 0.241818 -0.123735 0.366527 11.00000 -1.50000 H31C 2 0.236650 -0.127691 0.301464 11.00000 -1.50000 AFIX 0 C32 1 0.256206 -0.029201 0.200935 11.00000 0.03503 0.03363 = 0.02982 -0.00770 0.00481 0.00380 AFIX 23 H32A 2 0.298712 -0.052498 0.224994 11.00000 -1.20000 H32B 2 0.281884 -0.001832 0.168616 11.00000 -1.20000 AFIX 0 C33 1 0.204694 -0.108178 0.182425 11.00000 0.04510 0.03738 = 0.03592 -0.01308 -0.00534 0.00407 AFIX 133 H33A 2 0.183009 -0.139296 0.214384 11.00000 -1.50000 H33B 2 0.236917 -0.150551 0.161127 11.00000 -1.50000 H33C 2 0.161033 -0.085470 0.159862 11.00000 -1.50000 AFIX 0 C34 1 0.154027 0.127657 0.146326 11.00000 0.03971 0.03381 = 0.02296 -0.00544 0.00256 -0.00069 AFIX 133 H34A 2 0.099174 0.146554 0.139458 11.00000 -1.50000 H34B 2 0.164993 0.071559 0.126433 11.00000 -1.50000 H34C 2 0.190459 0.175087 0.133970 11.00000 -1.50000 AFIX 0 B1 3 0.256997 0.620602 0.504250 11.00000 0.02775 0.02022 = 0.02242 0.00041 0.00191 -0.00134 B2 3 0.079842 0.251474 0.234467 11.00000 0.03213 0.02979 = 0.01969 -0.00138 -0.00078 0.00022 HKLF 4 REM 201000819_2 REM R1 = 0.0421 for 4660 Fo > 4sig(Fo) and 0.0489 for all 5589 data REM 398 parameters refined using 0 restraints END WGHT 0.0566 1.6816 REM Highest difference peak 0.613, deepest hole -0.197, 1-sigma level 0.045 Q1 1 0.1131 -0.3753 0.2814 11.00000 0.05 0.61 Q2 1 0.1561 -0.2917 0.2769 11.00000 0.05 0.43 Q3 1 0.0989 0.3329 0.4084 11.00000 0.05 0.21 Q4 1 0.0371 0.4418 0.3694 11.00000 0.05 0.20 Q5 1 0.1042 0.4762 0.4371 11.00000 0.05 0.20 Q6 1 0.5578 0.5070 0.5214 11.00000 0.05 0.19 Q7 1 0.1608 0.1157 0.1814 11.00000 0.05 0.19 Q8 1 0.1118 0.6776 0.3802 11.00000 0.05 0.18 Q9 1 0.2873 0.4400 0.5261 11.00000 0.05 0.18 Q10 1 0.1504 0.4386 0.4679 11.00000 0.05 0.18 Q11 1 0.0144 0.4051 0.2812 11.00000 0.05 0.17 Q12 1 0.0365 0.3972 0.3292 11.00000 0.05 0.17 Q13 1 0.1922 -0.1830 0.2551 11.00000 0.05 0.17 Q14 1 0.3582 0.4430 0.5580 11.00000 0.05 0.16 Q15 1 0.0640 0.4955 0.4111 11.00000 0.05 0.16 Q16 1 0.1209 0.5445 0.4226 11.00000 0.05 0.16 Q17 1 0.2287 0.4366 0.4950 11.00000 0.05 0.16 Q18 1 0.4580 0.5191 0.5942 11.00000 0.05 0.16 Q19 1 0.0818 0.3838 0.3698 11.00000 0.05 0.15 Q20 1 0.2167 0.0453 0.2599 11.00000 0.05 0.15 ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.0090 0.0039 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0727 0.0534 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0311 0.0180 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 F(1) F 0.21819(6) 0.68181(6) 0.53833(4) 0.0325(3) Uani 1.0 8 d . . . F(2) F 0.29919(6) 0.66976(6) 0.46510(3) 0.0317(3) Uani 1.0 8 d . . . F(3) F 0.11344(7) 0.30808(6) 0.19556(4) 0.0385(3) Uani 1.0 8 d . . . F(4) F 0.00541(6) 0.22362(7) 0.21626(4) 0.0397(3) Uani 1.0 8 d . . . N(1) N 0.19786(7) 0.55659(8) 0.47614(5) 0.0218(3) Uani 1.0 8 d . . . N(2) N 0.31546(7) 0.56150(8) 0.53767(5) 0.0223(3) Uani 1.0 8 d . . . N(3) N 0.07331(8) 0.30170(9) 0.28990(5) 0.0244(3) Uani 1.0 8 d . . . N(4) N 0.13401(8) 0.16779(9) 0.24388(5) 0.0251(3) Uani 1.0 8 d . . . C(1) C 0.13854(9) 0.58111(10) 0.44101(6) 0.0229(4) Uani 1.0 8 d . . . C(2) C 0.09774(9) 0.50297(10) 0.42532(6) 0.0224(4) Uani 1.0 8 d . . . C(3) C 0.13331(9) 0.42917(10) 0.45077(6) 0.0215(4) Uani 1.0 8 d . . . C(4) C 0.19608(9) 0.46266(10) 0.48313(6) 0.0206(3) Uani 1.0 8 d . . . C(5) C 0.25154(9) 0.41992(10) 0.51674(6) 0.0217(4) Uani 1.0 8 d . . . C(6) C 0.31043(9) 0.46761(10) 0.54375(6) 0.0220(4) Uani 1.0 8 d . . . C(7) C 0.37748(9) 0.43803(10) 0.57486(6) 0.0240(4) Uani 1.0 8 d . . . C(8) C 0.42259(9) 0.51429(10) 0.58579(6) 0.0235(4) Uani 1.0 8 d . . . C(9) C 0.38268(9) 0.58935(10) 0.56254(6) 0.0236(4) Uani 1.0 8 d . . . C(10) C 0.04137(9) 0.38500(11) 0.29925(6) 0.0251(4) Uani 1.0 8 d . . . C(11) C 0.04752(9) 0.40407(11) 0.35492(6) 0.0234(4) Uani 1.0 8 d . . . C(12) C 0.08283(9) 0.33082(10) 0.38038(6) 0.0223(4) Uani 1.0 8 d . . . C(13) C 0.09951(9) 0.26597(11) 0.33977(6) 0.0235(4) Uani 1.0 8 d . . . C(14) C 0.14024(9) 0.18404(10) 0.34153(6) 0.0236(4) Uani 1.0 8 d . . . C(15) C 0.15833(9) 0.13571(11) 0.29483(6) 0.0256(4) Uani 1.0 8 d . . . C(16) C 0.20624(9) 0.05695(11) 0.28683(6) 0.0266(4) Uani 1.0 8 d . . . C(17) C 0.21071(9) 0.04323(11) 0.23095(6) 0.0270(4) Uani 1.0 8 d . . . C(18) C 0.16536(9) 0.11210(11) 0.20583(6) 0.0270(4) Uani 1.0 8 d . . . C(19) C 0.02463(9) 0.48090(10) 0.39229(6) 0.0237(4) Uani 1.0 8 d . . . C(20) C -0.03408(9) 0.43735(11) 0.43438(6) 0.0252(4) Uani 1.0 8 d . . . C(21) C 0.00646(9) 0.35671(10) 0.46395(6) 0.0238(4) Uani 1.0 8 d . . . C(22) C 0.09266(9) 0.33976(10) 0.44133(6) 0.0213(4) Uani 1.0 8 d . . . C(23) C 0.12622(10) 0.67632(11) 0.42247(7) 0.0291(4) Uani 1.0 8 d . . . C(24) C 0.39753(10) 0.34344(11) 0.59158(7) 0.0328(4) Uani 1.0 8 d . . . C(25) C 0.38767(12) 0.32530(13) 0.65257(8) 0.0425(5) Uani 1.0 8 d . . . C(26) C 0.50407(9) 0.51864(11) 0.61059(6) 0.0269(4) Uani 1.0 8 d . . . C(27) C 0.56786(11) 0.51342(16) 0.56656(7) 0.0459(5) Uani 1.0 8 d . . . C(28) C 0.41017(10) 0.68482(11) 0.56254(7) 0.0305(4) Uani 1.0 8 d . . . C(29) C 0.00706(10) 0.44251(12) 0.25524(6) 0.0309(4) Uani 1.0 8 d . . . C(30) C 0.24582(10) 0.00324(12) 0.33090(6) 0.0315(4) Uani 1.0 8 d . . . C(31) C 0.21886(12) -0.09529(12) 0.33409(7) 0.0380(5) Uani 1.0 8 d . . . C(32) C 0.25621(10) -0.02920(12) 0.20094(7) 0.0328(4) Uani 1.0 8 d . . . C(33) C 0.20469(12) -0.10818(13) 0.18243(7) 0.0395(5) Uani 1.0 8 d . . . C(34) C 0.15403(11) 0.12766(12) 0.14633(6) 0.0322(4) Uani 1.0 8 d . . . B(1) B 0.25700(11) 0.62060(12) 0.50425(7) 0.0235(4) Uani 1.0 8 d . . . B(2) B 0.07984(11) 0.25147(13) 0.23447(7) 0.0272(4) Uani 1.0 8 d . . . H(5) H 0.2488 0.3562 0.5212 0.0261 Uiso 1.0 8 calc R . . H(14) H 0.1561 0.1606 0.3759 0.0283 Uiso 1.0 8 calc R . . H(19) H 0.0019 0.5343 0.3727 0.0284 Uiso 1.0 8 calc R . . H(20A) H -0.0504 0.4834 0.4615 0.0302 Uiso 1.0 8 calc R . . H(20B) H -0.0822 0.4159 0.4152 0.0302 Uiso 1.0 8 calc R . . H(21A) H -0.0259 0.3015 0.4588 0.0286 Uiso 1.0 8 calc R . . H(21B) H 0.0093 0.3695 0.5035 0.0286 Uiso 1.0 8 calc R . . H(22) H 0.1203 0.2873 0.4586 0.0256 Uiso 1.0 8 calc R . . H(23A) H 0.1224 0.7162 0.4543 0.0437 Uiso 1.0 8 calc R . . H(23B) H 0.0771 0.6801 0.4012 0.0437 Uiso 1.0 8 calc R . . H(23C) H 0.1711 0.6951 0.3997 0.0437 Uiso 1.0 8 calc R . . H(24A) H 0.4532 0.3307 0.5812 0.0394 Uiso 1.0 8 calc R . . H(24B) H 0.3632 0.3010 0.5711 0.0394 Uiso 1.0 8 calc R . . H(25A) H 0.4200 0.3684 0.6733 0.0638 Uiso 1.0 8 calc R . . H(25B) H 0.4050 0.2635 0.6608 0.0638 Uiso 1.0 8 calc R . . H(25C) H 0.3317 0.3324 0.6627 0.0638 Uiso 1.0 8 calc R . . H(26A) H 0.5109 0.4679 0.6365 0.0323 Uiso 1.0 8 calc R . . H(26B) H 0.5099 0.5759 0.6311 0.0323 Uiso 1.0 8 calc R . . H(27A) H 0.5629 0.4560 0.5469 0.0688 Uiso 1.0 8 calc R . . H(27B) H 0.6204 0.5171 0.5835 0.0688 Uiso 1.0 8 calc R . . H(27C) H 0.5612 0.5638 0.5410 0.0688 Uiso 1.0 8 calc R . . H(28A) H 0.4485 0.6937 0.5330 0.0458 Uiso 1.0 8 calc R . . H(28B) H 0.4355 0.6986 0.5975 0.0458 Uiso 1.0 8 calc R . . H(28C) H 0.3647 0.7251 0.5571 0.0458 Uiso 1.0 8 calc R . . H(29A) H 0.0489 0.4592 0.2294 0.0463 Uiso 1.0 8 calc R . . H(29B) H -0.0158 0.4974 0.2713 0.0463 Uiso 1.0 8 calc R . . H(29C) H -0.0345 0.4087 0.2361 0.0463 Uiso 1.0 8 calc R . . H(30A) H 0.2351 0.0327 0.3664 0.0377 Uiso 1.0 8 calc R . . H(30B) H 0.3039 0.0046 0.3249 0.0377 Uiso 1.0 8 calc R . . H(31A) H 0.1608 -0.0977 0.3363 0.0571 Uiso 1.0 8 calc R . . H(31B) H 0.2418 -0.1237 0.3665 0.0571 Uiso 1.0 8 calc R . . H(31C) H 0.2367 -0.1277 0.3015 0.0571 Uiso 1.0 8 calc R . . H(32A) H 0.2987 -0.0525 0.2250 0.0394 Uiso 1.0 8 calc R . . H(32B) H 0.2819 -0.0018 0.1686 0.0394 Uiso 1.0 8 calc R . . H(33A) H 0.1830 -0.1393 0.2144 0.0592 Uiso 1.0 8 calc R . . H(33B) H 0.2369 -0.1505 0.1611 0.0592 Uiso 1.0 8 calc R . . H(33C) H 0.1610 -0.0855 0.1599 0.0592 Uiso 1.0 8 calc R . . H(34A) H 0.0992 0.1466 0.1395 0.0482 Uiso 1.0 8 calc R . . H(34B) H 0.1650 0.0716 0.1264 0.0482 Uiso 1.0 8 calc R . . H(34C) H 0.1905 0.1751 0.1340 0.0482 Uiso 1.0 8 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 F(1) 0.0398(6) 0.0264(6) 0.0312(5) 0.0073(4) -0.0015(5) -0.0081(4) F(2) 0.0381(6) 0.0308(6) 0.0260(5) -0.0117(4) -0.0019(4) 0.0057(4) F(3) 0.0611(7) 0.0312(6) 0.0233(5) 0.0012(5) 0.0081(5) -0.0004(4) F(4) 0.0350(6) 0.0460(7) 0.0379(6) 0.0038(5) -0.0124(5) -0.0130(5) N(1) 0.0234(7) 0.0204(7) 0.0216(6) 0.0004(5) 0.0024(6) 0.0004(5) N(2) 0.0245(7) 0.0220(7) 0.0205(6) -0.0016(6) 0.0016(5) -0.0011(5) N(3) 0.0256(7) 0.0281(8) 0.0196(7) 0.0020(6) -0.0010(6) -0.0016(6) N(4) 0.0280(7) 0.0282(8) 0.0192(7) -0.0006(6) 0.0004(6) -0.0042(5) C(1) 0.0249(8) 0.0239(8) 0.0199(7) 0.0028(7) 0.0031(6) -0.0000(6) C(2) 0.0243(8) 0.0230(8) 0.0198(7) 0.0027(6) 0.0030(6) -0.0010(6) C(3) 0.0222(8) 0.0234(8) 0.0188(7) 0.0015(6) 0.0040(6) -0.0017(6) C(4) 0.0223(8) 0.0188(8) 0.0207(7) 0.0004(6) 0.0036(6) -0.0016(6) C(5) 0.0231(8) 0.0199(8) 0.0223(8) -0.0000(6) 0.0045(6) -0.0009(6) C(6) 0.0236(8) 0.0194(8) 0.0229(8) 0.0010(6) 0.0026(6) -0.0013(6) C(7) 0.0250(8) 0.0250(9) 0.0220(8) 0.0011(7) 0.0013(6) -0.0040(6) C(8) 0.0251(8) 0.0258(9) 0.0197(7) -0.0007(7) 0.0023(6) -0.0035(6) C(9) 0.0268(8) 0.0258(9) 0.0181(7) -0.0040(7) 0.0030(6) -0.0025(6) C(10) 0.0235(8) 0.0291(9) 0.0229(8) 0.0026(7) 0.0002(7) -0.0004(7) C(11) 0.0234(8) 0.0255(9) 0.0214(8) 0.0014(7) 0.0003(6) -0.0013(6) C(12) 0.0213(8) 0.0241(9) 0.0215(8) -0.0004(6) 0.0010(6) -0.0016(6) C(13) 0.0234(8) 0.0274(9) 0.0196(8) -0.0007(7) -0.0003(6) -0.0017(6) C(14) 0.0236(8) 0.0264(9) 0.0209(8) -0.0019(7) -0.0010(6) -0.0017(6) C(15) 0.0260(8) 0.0293(9) 0.0216(8) -0.0001(7) -0.0013(7) -0.0027(7) C(16) 0.0254(8) 0.0284(9) 0.0260(8) 0.0007(7) -0.0008(7) -0.0052(7) C(17) 0.0259(9) 0.0292(9) 0.0259(8) -0.0007(7) 0.0003(7) -0.0071(7) C(18) 0.0286(9) 0.0296(9) 0.0227(8) -0.0034(7) 0.0033(7) -0.0065(7) C(19) 0.0256(8) 0.0241(9) 0.0212(7) 0.0043(7) -0.0009(7) -0.0010(6) C(20) 0.0231(8) 0.0294(9) 0.0230(8) 0.0015(7) -0.0007(7) -0.0047(7) C(21) 0.0238(8) 0.0242(9) 0.0236(8) -0.0022(7) 0.0031(7) -0.0033(6) C(22) 0.0235(8) 0.0216(8) 0.0188(7) -0.0001(6) 0.0001(6) -0.0016(6) C(23) 0.0316(9) 0.0250(9) 0.0308(9) 0.0020(7) 0.0010(7) 0.0029(7) C(24) 0.0295(9) 0.0237(9) 0.0453(10) 0.0024(7) -0.0103(8) -0.0049(7) C(25) 0.0389(11) 0.0320(11) 0.0567(12) -0.0010(8) -0.0066(9) 0.0154(9) C(26) 0.0261(8) 0.0309(9) 0.0237(8) -0.0028(7) -0.0007(7) -0.0039(7) C(27) 0.0253(9) 0.0823(16) 0.0300(9) -0.0014(10) 0.0006(8) -0.0080(10) C(28) 0.0386(10) 0.0265(9) 0.0264(9) -0.0083(7) -0.0043(7) 0.0004(7) C(29) 0.0343(10) 0.0362(10) 0.0220(8) 0.0062(8) -0.0018(7) 0.0007(7) C(30) 0.0317(9) 0.0360(10) 0.0267(9) 0.0065(8) -0.0049(7) -0.0081(7) C(31) 0.0471(11) 0.0344(11) 0.0326(9) 0.0089(9) -0.0067(8) -0.0037(8) C(32) 0.0350(10) 0.0336(10) 0.0298(9) 0.0038(8) 0.0048(8) -0.0077(7) C(33) 0.0451(11) 0.0374(11) 0.0359(10) 0.0041(9) -0.0053(9) -0.0131(8) C(34) 0.0397(10) 0.0338(10) 0.0230(8) -0.0007(8) 0.0026(7) -0.0054(7) B(1) 0.0278(10) 0.0202(9) 0.0224(9) -0.0013(7) 0.0019(7) 0.0004(7) B(2) 0.0321(10) 0.0298(11) 0.0197(9) 0.0002(8) -0.0008(8) -0.0014(7) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 F(1) B(1) 1.395(2) yes . . F(2) B(1) 1.399(2) yes . . F(3) B(2) 1.390(2) yes . . F(4) B(2) 1.393(2) yes . . N(1) C(1) 1.369(2) yes . . N(1) C(4) 1.3996(19) yes . . N(1) B(1) 1.538(3) yes . . N(2) C(6) 1.3987(19) yes . . N(2) C(9) 1.351(2) yes . . N(2) B(1) 1.551(3) yes . . N(3) C(10) 1.363(2) yes . . N(3) C(13) 1.404(2) yes . . N(3) B(2) 1.554(3) yes . . N(4) C(15) 1.399(2) yes . . N(4) C(18) 1.352(2) yes . . N(4) B(2) 1.555(3) yes . . C(1) C(2) 1.398(2) yes . . C(1) C(23) 1.494(3) yes . . C(2) C(3) 1.393(2) yes . . C(2) C(19) 1.510(3) yes . . C(3) C(4) 1.412(3) yes . . C(3) C(22) 1.507(2) yes . . C(4) C(5) 1.397(3) yes . . C(5) C(6) 1.386(3) yes . . C(6) C(7) 1.432(3) yes . . C(7) C(8) 1.386(2) yes . . C(7) C(24) 1.496(3) yes . . C(8) C(9) 1.417(2) yes . . C(8) C(26) 1.503(3) yes . . C(9) C(28) 1.486(3) yes . . C(10) C(11) 1.399(2) yes . . C(10) C(29) 1.491(3) yes . . C(11) C(12) 1.385(3) yes . . C(11) C(19) 1.510(3) yes . . C(12) C(13) 1.411(3) yes . . C(12) C(22) 1.511(2) yes . . C(13) C(14) 1.393(3) yes . . C(14) C(15) 1.385(3) yes . . C(15) C(16) 1.430(3) yes . . C(16) C(17) 1.388(2) yes . . C(16) C(30) 1.498(3) yes . . C(17) C(18) 1.414(3) yes . . C(17) C(32) 1.509(3) yes . . C(18) C(34) 1.491(2) yes . . C(19) C(20) 1.568(3) yes . . C(20) C(21) 1.554(3) yes . . C(21) C(22) 1.575(3) yes . . C(24) C(25) 1.530(3) yes . . C(26) C(27) 1.526(3) yes . . C(30) C(31) 1.528(3) yes . . C(32) C(33) 1.524(3) yes . . C(5) H(5) 0.950 no . . C(14) H(14) 0.950 no . . C(19) H(19) 1.000 no . . C(20) H(20A) 0.990 no . . C(20) H(20B) 0.990 no . . C(21) H(21A) 0.990 no . . C(21) H(21B) 0.990 no . . C(22) H(22) 1.000 no . . C(23) H(23A) 0.980 no . . C(23) H(23B) 0.980 no . . C(23) H(23C) 0.980 no . . C(24) H(24A) 0.990 no . . C(24) H(24B) 0.990 no . . C(25) H(25A) 0.980 no . . C(25) H(25B) 0.980 no . . C(25) H(25C) 0.980 no . . C(26) H(26A) 0.990 no . . C(26) H(26B) 0.990 no . . C(27) H(27A) 0.980 no . . C(27) H(27B) 0.980 no . . C(27) H(27C) 0.980 no . . C(28) H(28A) 0.980 no . . C(28) H(28B) 0.980 no . . C(28) H(28C) 0.980 no . . C(29) H(29A) 0.980 no . . C(29) H(29B) 0.980 no . . C(29) H(29C) 0.980 no . . C(30) H(30A) 0.990 no . . C(30) H(30B) 0.990 no . . C(31) H(31A) 0.980 no . . C(31) H(31B) 0.980 no . . C(31) H(31C) 0.980 no . . C(32) H(32A) 0.990 no . . C(32) H(32B) 0.990 no . . C(33) H(33A) 0.980 no . . C(33) H(33B) 0.980 no . . C(33) H(33C) 0.980 no . . C(34) H(34A) 0.980 no . . C(34) H(34B) 0.980 no . . C(34) H(34C) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(1) N(1) C(4) 108.93(12) yes . . . C(1) N(1) B(1) 126.35(13) yes . . . C(4) N(1) B(1) 124.72(13) yes . . . C(6) N(2) C(9) 107.76(12) yes . . . C(6) N(2) B(1) 125.24(13) yes . . . C(9) N(2) B(1) 126.84(13) yes . . . C(10) N(3) C(13) 108.49(13) yes . . . C(10) N(3) B(2) 127.37(13) yes . . . C(13) N(3) B(2) 124.13(14) yes . . . C(15) N(4) C(18) 107.25(13) yes . . . C(15) N(4) B(2) 125.07(13) yes . . . C(18) N(4) B(2) 127.67(13) yes . . . N(1) C(1) C(2) 108.27(13) yes . . . N(1) C(1) C(23) 122.88(14) yes . . . C(2) C(1) C(23) 128.78(14) yes . . . C(1) C(2) C(3) 108.19(14) yes . . . C(1) C(2) C(19) 136.65(14) yes . . . C(3) C(2) C(19) 114.99(13) yes . . . C(2) C(3) C(4) 107.44(13) yes . . . C(2) C(3) C(22) 115.01(13) yes . . . C(4) C(3) C(22) 137.26(14) yes . . . N(1) C(4) C(3) 107.16(13) yes . . . N(1) C(4) C(5) 120.45(14) yes . . . C(3) C(4) C(5) 132.39(14) yes . . . C(4) C(5) C(6) 122.07(14) yes . . . N(2) C(6) C(5) 119.82(14) yes . . . N(2) C(6) C(7) 108.19(13) yes . . . C(5) C(6) C(7) 131.64(14) yes . . . C(6) C(7) C(8) 106.70(13) yes . . . C(6) C(7) C(24) 127.58(14) yes . . . C(8) C(7) C(24) 125.70(14) yes . . . C(7) C(8) C(9) 107.39(14) yes . . . C(7) C(8) C(26) 127.88(14) yes . . . C(9) C(8) C(26) 124.25(14) yes . . . N(2) C(9) C(8) 109.93(13) yes . . . N(2) C(9) C(28) 123.44(14) yes . . . C(8) C(9) C(28) 126.58(14) yes . . . N(3) C(10) C(11) 108.49(14) yes . . . N(3) C(10) C(29) 123.10(14) yes . . . C(11) C(10) C(29) 128.41(15) yes . . . C(10) C(11) C(12) 108.36(14) yes . . . C(10) C(11) C(19) 136.55(15) yes . . . C(12) C(11) C(19) 115.08(13) yes . . . C(11) C(12) C(13) 107.35(14) yes . . . C(11) C(12) C(22) 115.18(13) yes . . . C(13) C(12) C(22) 137.47(14) yes . . . N(3) C(13) C(12) 107.30(14) yes . . . N(3) C(13) C(14) 120.60(14) yes . . . C(12) C(13) C(14) 131.84(14) yes . . . C(13) C(14) C(15) 122.11(14) yes . . . N(4) C(15) C(14) 120.04(14) yes . . . N(4) C(15) C(16) 108.58(13) yes . . . C(14) C(15) C(16) 131.14(14) yes . . . C(15) C(16) C(17) 106.57(14) yes . . . C(15) C(16) C(30) 125.69(14) yes . . . C(17) C(16) C(30) 127.70(15) yes . . . C(16) C(17) C(18) 107.22(14) yes . . . C(16) C(17) C(32) 127.84(15) yes . . . C(18) C(17) C(32) 124.93(14) yes . . . N(4) C(18) C(17) 110.38(13) yes . . . N(4) C(18) C(34) 122.18(15) yes . . . C(17) C(18) C(34) 127.39(15) yes . . . C(2) C(19) C(11) 106.28(13) yes . . . C(2) C(19) C(20) 104.44(12) yes . . . C(11) C(19) C(20) 104.61(12) yes . . . C(19) C(20) C(21) 110.21(12) yes . . . C(20) C(21) C(22) 111.27(12) yes . . . C(3) C(22) C(12) 106.19(12) yes . . . C(3) C(22) C(21) 103.02(12) yes . . . C(12) C(22) C(21) 105.18(12) yes . . . C(7) C(24) C(25) 114.06(14) yes . . . C(8) C(26) C(27) 110.75(13) yes . . . C(16) C(30) C(31) 114.20(14) yes . . . C(17) C(32) C(33) 113.57(15) yes . . . F(1) B(1) F(2) 108.24(13) yes . . . F(1) B(1) N(1) 111.38(14) yes . . . F(1) B(1) N(2) 110.24(13) yes . . . F(2) B(1) N(1) 109.93(13) yes . . . F(2) B(1) N(2) 109.47(14) yes . . . N(1) B(1) N(2) 107.58(13) yes . . . F(3) B(2) F(4) 108.90(14) yes . . . F(3) B(2) N(3) 110.03(14) yes . . . F(3) B(2) N(4) 110.01(14) yes . . . F(4) B(2) N(3) 111.00(14) yes . . . F(4) B(2) N(4) 109.92(14) yes . . . N(3) B(2) N(4) 106.97(13) yes . . . C(4) C(5) H(5) 118.960 no . . . C(6) C(5) H(5) 118.972 no . . . C(13) C(14) H(14) 118.943 no . . . C(15) C(14) H(14) 118.946 no . . . C(2) C(19) H(19) 113.540 no . . . C(11) C(19) H(19) 113.524 no . . . C(20) C(19) H(19) 113.551 no . . . C(19) C(20) H(20A) 109.611 no . . . C(19) C(20) H(20B) 109.621 no . . . C(21) C(20) H(20A) 109.606 no . . . C(21) C(20) H(20B) 109.623 no . . . H(20A) C(20) H(20B) 108.138 no . . . C(20) C(21) H(21A) 109.374 no . . . C(20) C(21) H(21B) 109.382 no . . . C(22) C(21) H(21A) 109.374 no . . . C(22) C(21) H(21B) 109.390 no . . . H(21A) C(21) H(21B) 107.990 no . . . C(3) C(22) H(22) 113.807 no . . . C(12) C(22) H(22) 113.819 no . . . C(21) C(22) H(22) 113.802 no . . . C(1) C(23) H(23A) 109.477 no . . . C(1) C(23) H(23B) 109.468 no . . . C(1) C(23) H(23C) 109.472 no . . . H(23A) C(23) H(23B) 109.471 no . . . H(23A) C(23) H(23C) 109.474 no . . . H(23B) C(23) H(23C) 109.465 no . . . C(7) C(24) H(24A) 108.733 no . . . C(7) C(24) H(24B) 108.733 no . . . C(25) C(24) H(24A) 108.742 no . . . C(25) C(24) H(24B) 108.742 no . . . H(24A) C(24) H(24B) 107.641 no . . . C(24) C(25) H(25A) 109.468 no . . . C(24) C(25) H(25B) 109.468 no . . . C(24) C(25) H(25C) 109.464 no . . . H(25A) C(25) H(25B) 109.483 no . . . H(25A) C(25) H(25C) 109.476 no . . . H(25B) C(25) H(25C) 109.469 no . . . C(8) C(26) H(26A) 109.500 no . . . C(8) C(26) H(26B) 109.494 no . . . C(27) C(26) H(26A) 109.499 no . . . C(27) C(26) H(26B) 109.495 no . . . H(26A) C(26) H(26B) 108.062 no . . . C(26) C(27) H(27A) 109.468 no . . . C(26) C(27) H(27B) 109.469 no . . . C(26) C(27) H(27C) 109.473 no . . . H(27A) C(27) H(27B) 109.466 no . . . H(27A) C(27) H(27C) 109.478 no . . . H(27B) C(27) H(27C) 109.473 no . . . C(9) C(28) H(28A) 109.470 no . . . C(9) C(28) H(28B) 109.463 no . . . C(9) C(28) H(28C) 109.475 no . . . H(28A) C(28) H(28B) 109.469 no . . . H(28A) C(28) H(28C) 109.472 no . . . H(28B) C(28) H(28C) 109.479 no . . . C(10) C(29) H(29A) 109.467 no . . . C(10) C(29) H(29B) 109.462 no . . . C(10) C(29) H(29C) 109.472 no . . . H(29A) C(29) H(29B) 109.470 no . . . H(29A) C(29) H(29C) 109.476 no . . . H(29B) C(29) H(29C) 109.480 no . . . C(16) C(30) H(30A) 108.698 no . . . C(16) C(30) H(30B) 108.719 no . . . C(31) C(30) H(30A) 108.702 no . . . C(31) C(30) H(30B) 108.708 no . . . H(30A) C(30) H(30B) 107.616 no . . . C(30) C(31) H(31A) 109.476 no . . . C(30) C(31) H(31B) 109.482 no . . . C(30) C(31) H(31C) 109.463 no . . . H(31A) C(31) H(31B) 109.474 no . . . H(31A) C(31) H(31C) 109.459 no . . . H(31B) C(31) H(31C) 109.474 no . . . C(17) C(32) H(32A) 108.866 no . . . C(17) C(32) H(32B) 108.843 no . . . C(33) C(32) H(32A) 108.846 no . . . C(33) C(32) H(32B) 108.849 no . . . H(32A) C(32) H(32B) 107.706 no . . . C(32) C(33) H(33A) 109.479 no . . . C(32) C(33) H(33B) 109.462 no . . . C(32) C(33) H(33C) 109.473 no . . . H(33A) C(33) H(33B) 109.469 no . . . H(33A) C(33) H(33C) 109.480 no . . . H(33B) C(33) H(33C) 109.466 no . . . C(18) C(34) H(34A) 109.467 no . . . C(18) C(34) H(34B) 109.481 no . . . C(18) C(34) H(34C) 109.481 no . . . H(34A) C(34) H(34B) 109.455 no . . . H(34A) C(34) H(34C) 109.474 no . . . H(34B) C(34) H(34C) 109.469 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(1) N(1) C(4) C(3) 0.19(15) no . . . . C(1) N(1) C(4) C(5) 179.17(12) no . . . . C(4) N(1) C(1) C(2) 0.33(16) no . . . . C(4) N(1) C(1) C(23) -176.90(12) no . . . . C(1) N(1) B(1) F(1) 61.97(19) no . . . . C(1) N(1) B(1) F(2) -57.99(19) no . . . . C(1) N(1) B(1) N(2) -177.12(12) no . . . . B(1) N(1) C(1) C(2) -179.15(12) no . . . . B(1) N(1) C(1) C(23) 3.6(3) no . . . . C(4) N(1) B(1) F(1) -117.42(15) no . . . . C(4) N(1) B(1) F(2) 122.62(15) no . . . . C(4) N(1) B(1) N(2) 3.49(19) no . . . . B(1) N(1) C(4) C(3) 179.67(12) no . . . . B(1) N(1) C(4) C(5) -1.3(2) no . . . . C(6) N(2) C(9) C(8) -0.51(16) no . . . . C(6) N(2) C(9) C(28) 177.19(12) no . . . . C(9) N(2) C(6) C(5) -172.75(12) no . . . . C(9) N(2) C(6) C(7) 1.18(15) no . . . . C(6) N(2) B(1) F(1) 117.33(15) no . . . . C(6) N(2) B(1) F(2) -123.71(14) no . . . . C(6) N(2) B(1) N(1) -4.30(19) no . . . . B(1) N(2) C(6) C(5) 2.9(2) no . . . . B(1) N(2) C(6) C(7) 176.83(12) no . . . . C(9) N(2) B(1) F(1) -67.85(19) no . . . . C(9) N(2) B(1) F(2) 51.11(19) no . . . . C(9) N(2) B(1) N(1) 170.52(13) no . . . . B(1) N(2) C(9) C(8) -176.07(12) no . . . . B(1) N(2) C(9) C(28) 1.6(3) no . . . . C(10) N(3) C(13) C(12) -0.29(16) no . . . . C(10) N(3) C(13) C(14) -175.10(13) no . . . . C(13) N(3) C(10) C(11) 0.68(16) no . . . . C(13) N(3) C(10) C(29) -179.62(12) no . . . . C(10) N(3) B(2) F(3) 50.5(2) no . . . . C(10) N(3) B(2) F(4) -70.2(2) no . . . . C(10) N(3) B(2) N(4) 169.92(14) no . . . . B(2) N(3) C(10) C(11) 179.85(13) no . . . . B(2) N(3) C(10) C(29) -0.4(3) no . . . . C(13) N(3) B(2) F(3) -130.49(15) no . . . . C(13) N(3) B(2) F(4) 108.89(16) no . . . . C(13) N(3) B(2) N(4) -11.0(2) no . . . . B(2) N(3) C(13) C(12) -179.50(13) no . . . . B(2) N(3) C(13) C(14) 5.7(3) no . . . . C(15) N(4) C(18) C(17) -0.22(17) no . . . . C(15) N(4) C(18) C(34) -177.84(12) no . . . . C(18) N(4) C(15) C(14) 174.78(13) no . . . . C(18) N(4) C(15) C(16) -0.21(16) no . . . . C(15) N(4) B(2) F(3) 130.79(15) no . . . . C(15) N(4) B(2) F(4) -109.30(16) no . . . . C(15) N(4) B(2) N(3) 11.3(2) no . . . . B(2) N(4) C(15) C(14) -6.0(3) no . . . . B(2) N(4) C(15) C(16) 178.96(13) no . . . . C(18) N(4) B(2) F(3) -50.2(2) no . . . . C(18) N(4) B(2) F(4) 69.7(2) no . . . . C(18) N(4) B(2) N(3) -169.70(14) no . . . . B(2) N(4) C(18) C(17) -179.37(13) no . . . . B(2) N(4) C(18) C(34) 3.0(3) no . . . . N(1) C(1) C(2) C(3) -0.73(16) no . . . . N(1) C(1) C(2) C(19) 174.12(14) no . . . . C(23) C(1) C(2) C(3) 176.28(14) no . . . . C(23) C(1) C(2) C(19) -8.9(3) no . . . . C(1) C(2) C(3) C(4) 0.84(16) no . . . . C(1) C(2) C(3) C(22) 175.79(11) no . . . . C(1) C(2) C(19) C(11) 134.20(18) no . . . . C(1) C(2) C(19) C(20) -115.52(19) no . . . . C(3) C(2) C(19) C(11) -51.20(16) no . . . . C(3) C(2) C(19) C(20) 59.08(15) no . . . . C(19) C(2) C(3) C(4) -175.26(11) no . . . . C(19) C(2) C(3) C(22) -0.30(18) no . . . . C(2) C(3) C(4) N(1) -0.63(16) no . . . . C(2) C(3) C(4) C(5) -179.45(14) no . . . . C(2) C(3) C(22) C(12) 51.60(16) no . . . . C(2) C(3) C(22) C(21) -58.71(15) no . . . . C(4) C(3) C(22) C(12) -135.50(18) no . . . . C(4) C(3) C(22) C(21) 114.19(19) no . . . . C(22) C(3) C(4) N(1) -173.89(16) no . . . . C(22) C(3) C(4) C(5) 7.3(3) no . . . . N(1) C(4) C(5) C(6) -0.7(3) no . . . . C(3) C(4) C(5) C(6) 177.94(14) no . . . . C(4) C(5) C(6) N(2) -0.0(3) no . . . . C(4) C(5) C(6) C(7) -172.29(14) no . . . . N(2) C(6) C(7) C(8) -1.41(16) no . . . . N(2) C(6) C(7) C(24) -179.91(12) no . . . . C(5) C(6) C(7) C(8) 171.54(15) no . . . . C(5) C(6) C(7) C(24) -7.0(3) no . . . . C(6) C(7) C(8) C(9) 1.09(16) no . . . . C(6) C(7) C(8) C(26) -171.14(13) no . . . . C(6) C(7) C(24) C(25) -109.45(17) no . . . . C(8) C(7) C(24) C(25) 72.32(19) no . . . . C(24) C(7) C(8) C(9) 179.62(13) no . . . . C(24) C(7) C(8) C(26) 7.4(3) no . . . . C(7) C(8) C(9) N(2) -0.39(17) no . . . . C(7) C(8) C(9) C(28) -177.99(13) no . . . . C(7) C(8) C(26) C(27) 89.26(18) no . . . . C(9) C(8) C(26) C(27) -81.76(17) no . . . . C(26) C(8) C(9) N(2) 172.19(13) no . . . . C(26) C(8) C(9) C(28) -5.4(3) no . . . . N(3) C(10) C(11) C(12) -0.82(17) no . . . . N(3) C(10) C(11) C(19) -179.45(15) no . . . . C(29) C(10) C(11) C(12) 179.50(14) no . . . . C(29) C(10) C(11) C(19) 0.9(3) no . . . . C(10) C(11) C(12) C(13) 0.63(17) no . . . . C(10) C(11) C(12) C(22) -178.96(12) no . . . . C(10) C(11) C(19) C(2) -130.04(18) no . . . . C(10) C(11) C(19) C(20) 119.80(19) no . . . . C(12) C(11) C(19) C(2) 51.39(16) no . . . . C(12) C(11) C(19) C(20) -58.77(16) no . . . . C(19) C(11) C(12) C(13) 179.59(12) no . . . . C(19) C(11) C(12) C(22) 0.00(19) no . . . . C(11) C(12) C(13) N(3) -0.21(17) no . . . . C(11) C(12) C(13) C(14) 173.79(15) no . . . . C(11) C(12) C(22) C(3) -51.57(16) no . . . . C(11) C(12) C(22) C(21) 57.21(16) no . . . . C(13) C(12) C(22) C(3) 129.02(18) no . . . . C(13) C(12) C(22) C(21) -122.21(19) no . . . . C(22) C(12) C(13) N(3) 179.23(16) no . . . . C(22) C(12) C(13) C(14) -6.8(3) no . . . . N(3) C(13) C(14) C(15) 1.6(3) no . . . . C(12) C(13) C(14) C(15) -171.73(15) no . . . . C(13) C(14) C(15) N(4) -1.5(3) no . . . . C(13) C(14) C(15) C(16) 172.22(14) no . . . . N(4) C(15) C(16) C(17) 0.57(17) no . . . . N(4) C(15) C(16) C(30) 178.37(12) no . . . . C(14) C(15) C(16) C(17) -173.67(15) no . . . . C(14) C(15) C(16) C(30) 4.1(3) no . . . . C(15) C(16) C(17) C(18) -0.68(17) no . . . . C(15) C(16) C(17) C(32) 177.98(13) no . . . . C(15) C(16) C(30) C(31) 119.27(16) no . . . . C(17) C(16) C(30) C(31) -63.4(2) no . . . . C(30) C(16) C(17) C(18) -178.43(14) no . . . . C(30) C(16) C(17) C(32) 0.2(3) no . . . . C(16) C(17) C(18) N(4) 0.58(18) no . . . . C(16) C(17) C(18) C(34) 178.05(13) no . . . . C(16) C(17) C(32) C(33) 100.36(18) no . . . . C(18) C(17) C(32) C(33) -81.20(19) no . . . . C(32) C(17) C(18) N(4) -178.13(14) no . . . . C(32) C(17) C(18) C(34) -0.7(3) no . . . . C(2) C(19) C(20) C(21) -54.36(14) no . . . . C(11) C(19) C(20) C(21) 57.13(14) no . . . . C(19) C(20) C(21) C(22) -2.49(16) no . . . . C(20) C(21) C(22) C(3) 57.84(14) no . . . . C(20) C(21) C(22) C(12) -53.22(14) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 F(1) C(1) 3.1181(18) no . . F(1) C(4) 3.5316(18) no . . F(1) C(6) 3.5301(18) no . . F(1) C(9) 3.1466(18) no . . F(1) C(23) 3.239(2) no . . F(1) C(28) 3.289(2) no . . F(2) C(1) 3.0647(18) no . . F(2) C(4) 3.5480(18) no . . F(2) C(6) 3.5629(17) no . . F(2) C(9) 3.0185(17) no . . F(2) C(23) 3.098(2) no . . F(2) C(28) 3.0438(19) no . . F(3) C(10) 3.0404(18) no . . F(3) C(18) 3.0371(19) no . . F(3) C(29) 3.051(2) no . . F(3) C(34) 3.007(2) no . . F(4) C(10) 3.1951(19) no . . F(4) C(13) 3.4777(18) no . . F(4) C(15) 3.4706(19) no . . F(4) C(18) 3.1694(19) no . . F(4) C(29) 3.375(2) no . . F(4) C(34) 3.351(2) no . . N(1) C(6) 2.843(2) no . . N(2) C(4) 2.823(2) no . . N(3) C(15) 2.844(2) no . . N(4) C(13) 2.826(2) no . . C(1) C(5) 3.572(2) no . . C(2) C(12) 2.785(2) no . . C(2) C(21) 2.818(2) no . . C(3) C(11) 2.786(2) no . . C(3) C(20) 2.851(3) no . . C(4) C(21) 3.589(3) no . . C(5) C(9) 3.524(3) no . . C(5) C(22) 3.463(3) no . . C(5) C(24) 3.271(3) no . . C(5) B(1) 2.984(3) no . . C(7) C(27) 3.402(3) no . . C(8) C(25) 3.292(3) no . . C(9) C(27) 3.317(3) no . . C(10) C(14) 3.561(3) no . . C(11) C(21) 2.851(2) no . . C(12) C(20) 2.849(3) no . . C(14) C(18) 3.522(2) no . . C(14) C(22) 3.456(2) no . . C(14) C(30) 3.221(3) no . . C(14) B(2) 2.989(3) no . . C(16) C(33) 3.539(3) no . . C(17) C(31) 3.259(3) no . . C(18) C(33) 3.373(3) no . . C(19) C(22) 2.668(2) no . . C(19) C(23) 3.439(3) no . . C(19) C(29) 3.424(2) no . . C(23) B(1) 3.092(3) no . . C(24) C(26) 3.186(3) no . . C(26) C(28) 3.151(3) no . . C(28) B(1) 3.099(3) no . . C(29) B(2) 3.121(3) no . . C(30) C(32) 3.230(3) no . . C(31) C(32) 3.469(3) no . . C(32) C(34) 3.184(3) no . . C(34) B(2) 3.097(3) no . . F(1) C(5) 3.5964(18) no . 2_555 F(1) C(24) 3.349(2) no . 2_555 F(2) C(14) 3.2069(17) no . 2_555 F(2) C(22) 3.1587(18) no . 2_555 F(2) C(27) 3.599(3) no . 5_666 F(3) C(28) 3.291(2) no . 4_564 F(3) C(32) 3.260(2) no . 2_555 F(3) C(33) 3.320(3) no . 2_555 N(1) C(20) 3.528(2) no . 5_566 N(2) C(27) 3.411(3) no . 5_666 C(1) C(20) 3.539(2) no . 5_566 C(1) C(21) 3.501(3) no . 5_566 C(1) C(30) 3.525(3) no . 2_555 C(2) C(30) 3.509(3) no . 2_555 C(5) F(1) 3.5964(18) no . 2_545 C(6) C(27) 3.408(3) no . 5_666 C(14) F(2) 3.2069(17) no . 2_545 C(20) N(1) 3.528(2) no . 5_566 C(20) C(1) 3.539(2) no . 5_566 C(21) C(1) 3.501(3) no . 5_566 C(22) F(2) 3.1587(18) no . 2_545 C(24) F(1) 3.349(2) no . 2_545 C(27) F(2) 3.599(3) no . 5_666 C(27) N(2) 3.411(3) no . 5_666 C(27) C(6) 3.408(3) no . 5_666 C(28) F(3) 3.291(2) no . 4_565 C(30) C(1) 3.525(3) no . 2_545 C(30) C(2) 3.509(3) no . 2_545 C(32) F(3) 3.260(2) no . 2_545 C(33) F(3) 3.320(3) no . 2_545 F(1) H(23A) 2.6686 no . . F(1) H(23C) 3.4980 no . . F(1) H(28C) 2.5904 no . . F(2) H(23A) 3.0683 no . . F(2) H(23C) 2.7145 no . . F(2) H(28A) 3.0387 no . . F(2) H(28C) 2.6426 no . . F(3) H(29A) 2.6202 no . . F(3) H(29C) 3.0690 no . . F(3) H(34A) 2.7671 no . . F(3) H(34C) 2.7990 no . . F(4) H(29A) 3.5744 no . . F(4) H(29C) 2.8601 no . . F(4) H(34A) 2.7104 no . . N(1) H(5) 3.2772 no . . N(1) H(23A) 2.7337 no . . N(1) H(23B) 3.2949 no . . N(1) H(23C) 2.8130 no . . N(2) H(5) 3.2620 no . . N(2) H(28A) 2.9767 no . . N(2) H(28B) 3.2180 no . . N(2) H(28C) 2.6008 no . . N(3) H(14) 3.2791 no . . N(3) H(29A) 2.7922 no . . N(3) H(29B) 3.2909 no . . N(3) H(29C) 2.7470 no . . N(4) H(14) 3.2626 no . . N(4) H(34A) 2.6479 no . . N(4) H(34B) 3.2567 no . . N(4) H(34C) 2.8624 no . . C(1) H(19) 2.9302 no . . C(1) H(20A) 3.5320 no . . C(2) H(20A) 2.6649 no . . C(2) H(20B) 3.3035 no . . C(2) H(21B) 3.1295 no . . C(2) H(22) 3.3142 no . . C(2) H(23A) 3.2580 no . . C(2) H(23B) 2.7073 no . . C(2) H(23C) 3.1611 no . . C(3) H(5) 2.8176 no . . C(3) H(19) 3.3142 no . . C(3) H(20A) 3.2080 no . . C(3) H(21A) 3.2861 no . . C(3) H(21B) 2.6112 no . . C(4) H(21B) 3.4713 no . . C(4) H(22) 2.9519 no . . C(5) H(22) 3.2811 no . . C(5) H(24B) 2.8999 no . . C(6) H(24A) 3.2754 no . . C(6) H(24B) 2.7033 no . . C(6) H(25C) 3.5561 no . . C(7) H(5) 2.8105 no . . C(7) H(25A) 2.7217 no . . C(7) H(25B) 3.3649 no . . C(7) H(25C) 2.7711 no . . C(7) H(26A) 2.7448 no . . C(7) H(26B) 3.3226 no . . C(7) H(27A) 3.2100 no . . C(8) H(24A) 2.7652 no . . C(8) H(24B) 3.3277 no . . C(8) H(25A) 3.0440 no . . C(8) H(27A) 2.6916 no . . C(8) H(27B) 3.3339 no . . C(8) H(27C) 2.6820 no . . C(8) H(28A) 2.9845 no . . C(8) H(28B) 2.7489 no . . C(8) H(28C) 3.3409 no . . C(9) H(26A) 3.3444 no . . C(9) H(26B) 2.7329 no . . C(9) H(27C) 3.0762 no . . C(10) H(19) 2.9260 no . . C(10) H(20B) 3.5564 no . . C(11) H(20A) 3.3068 no . . C(11) H(20B) 2.6458 no . . C(11) H(21A) 3.2149 no . . C(11) H(22) 3.3117 no . . C(11) H(29A) 3.1865 no . . C(11) H(29B) 2.6935 no . . C(11) H(29C) 3.2275 no . . C(12) H(14) 2.8058 no . . C(12) H(19) 3.3076 no . . C(12) H(20B) 3.1696 no . . C(12) H(21A) 2.6928 no . . C(12) H(21B) 3.3156 no . . C(13) H(22) 2.9554 no . . C(14) H(22) 3.2716 no . . C(14) H(30A) 2.8165 no . . C(15) H(30A) 2.6601 no . . C(15) H(30B) 3.2118 no . . C(15) H(31A) 3.5975 no . . C(16) H(14) 2.7993 no . . C(16) H(31A) 2.6991 no . . C(16) H(31B) 3.3649 no . . C(16) H(31C) 2.8006 no . . C(16) H(32A) 2.7109 no . . C(16) H(32B) 3.2858 no . . C(16) H(33A) 3.4255 no . . C(17) H(30A) 3.3527 no . . C(17) H(30B) 2.8466 no . . C(17) H(31A) 3.4252 no . . C(17) H(31C) 3.0938 no . . C(17) H(33A) 2.7687 no . . C(17) H(33B) 3.3674 no . . C(17) H(33C) 2.7139 no . . C(17) H(34A) 3.3025 no . . C(17) H(34B) 2.7110 no . . C(17) H(34C) 3.0956 no . . C(18) H(32A) 3.3452 no . . C(18) H(32B) 2.7431 no . . C(18) H(33C) 3.1322 no . . C(19) H(21A) 3.2295 no . . C(19) H(21B) 3.1979 no . . C(19) H(23B) 3.0827 no . . C(19) H(29B) 3.0570 no . . C(20) H(22) 3.4706 no . . C(21) H(19) 3.4515 no . . C(22) H(5) 3.2895 no . . C(22) H(14) 3.2776 no . . C(22) H(20A) 3.2498 no . . C(22) H(20B) 3.2184 no . . C(23) H(19) 3.2073 no . . C(24) H(5) 3.0492 no . . C(24) H(26A) 2.8717 no . . C(24) H(27A) 3.4263 no . . C(25) H(26A) 2.9851 no . . C(26) H(24A) 2.9959 no . . C(26) H(25A) 3.0511 no . . C(26) H(28A) 3.3470 no . . C(26) H(28B) 2.9186 no . . C(27) H(24A) 3.3403 no . . C(27) H(28A) 3.4389 no . . C(28) H(26B) 2.8726 no . . C(28) H(27C) 3.1545 no . . C(29) H(19) 3.1873 no . . C(30) H(14) 2.9854 no . . C(30) H(32A) 2.8688 no . . C(31) H(32A) 3.0627 no . . C(31) H(33A) 3.0693 no . . C(32) H(30B) 3.1850 no . . C(32) H(31C) 2.8837 no . . C(32) H(34B) 2.8152 no . . C(33) H(31C) 2.9846 no . . C(33) H(34B) 3.0656 no . . C(34) H(32B) 2.9332 no . . C(34) H(33C) 3.1707 no . . B(1) H(23A) 2.9404 no . . B(1) H(23C) 3.1441 no . . B(1) H(28A) 3.4754 no . . B(1) H(28C) 2.7126 no . . B(2) H(29A) 3.1179 no . . B(2) H(29C) 3.0198 no . . B(2) H(34A) 2.8196 no . . B(2) H(34C) 3.2913 no . . H(5) H(22) 2.8425 no . . H(5) H(24B) 2.4248 no . . H(14) H(22) 2.8283 no . . H(14) H(30A) 2.3237 no . . H(19) H(20A) 2.4682 no . . H(19) H(20B) 2.4830 no . . H(19) H(23B) 2.5964 no . . H(19) H(29B) 2.5660 no . . H(20A) H(21A) 2.7215 no . . H(20A) H(21B) 2.2150 no . . H(20B) H(21A) 2.2152 no . . H(20B) H(21B) 2.7456 no . . H(21A) H(22) 2.4724 no . . H(21B) H(22) 2.4883 no . . H(24A) H(25A) 2.3941 no . . H(24A) H(25B) 2.3378 no . . H(24A) H(25C) 2.8613 no . . H(24A) H(26A) 2.6263 no . . H(24A) H(27A) 2.7495 no . . H(24B) H(25A) 2.8622 no . . H(24B) H(25B) 2.3766 no . . H(24B) H(25C) 2.3542 no . . H(25A) H(26A) 2.3081 no . . H(25A) H(26B) 3.5746 no . . H(25B) H(26A) 3.5596 no . . H(26A) H(27A) 2.3733 no . . H(26A) H(27B) 2.3713 no . . H(26A) H(27C) 2.8661 no . . H(26B) H(27A) 2.8661 no . . H(26B) H(27B) 2.3642 no . . H(26B) H(27C) 2.3807 no . . H(26B) H(28A) 3.1472 no . . H(26B) H(28B) 2.3548 no . . H(27C) H(28A) 2.7073 no . . H(27C) H(28B) 3.2217 no . . H(30A) H(31A) 2.4140 no . . H(30A) H(31B) 2.3159 no . . H(30A) H(31C) 2.8571 no . . H(30B) H(31A) 2.8593 no . . H(30B) H(31B) 2.3959 no . . H(30B) H(31C) 2.3320 no . . H(30B) H(32A) 2.5937 no . . H(31A) H(33A) 3.0781 no . . H(31C) H(32A) 2.4190 no . . H(31C) H(33A) 2.3268 no . . H(31C) H(33B) 3.4608 no . . H(32A) H(33A) 2.3482 no . . H(32A) H(33B) 2.3752 no . . H(32A) H(33C) 2.8588 no . . H(32B) H(33A) 2.8577 no . . H(32B) H(33B) 2.3328 no . . H(32B) H(33C) 2.3917 no . . H(32B) H(34B) 2.4754 no . . H(32B) H(34C) 3.1523 no . . H(33C) H(34B) 2.4633 no . . F(1) H(5) 2.6705 no . 2_555 F(1) H(20B) 2.9377 no . 5_566 F(1) H(21A) 3.2496 no . 5_566 F(1) H(24B) 2.3735 no . 2_555 F(1) H(33B) 3.0655 no . 3_555 F(1) H(33C) 3.4429 no . 3_555 F(1) H(34C) 3.5149 no . 4_565 F(2) H(5) 3.1852 no . 2_555 F(2) H(14) 2.3198 no . 2_555 F(2) H(22) 2.2095 no . 2_555 F(2) H(27A) 2.9899 no . 5_666 F(2) H(27B) 3.2994 no . 5_666 F(2) H(30A) 3.2111 no . 2_555 F(3) H(26B) 3.1245 no . 4_564 F(3) H(28B) 2.5451 no . 4_564 F(3) H(28C) 3.4535 no . 4_564 F(3) H(32A) 2.6384 no . 2_555 F(3) H(32B) 3.3831 no . 2_555 F(3) H(33A) 3.5465 no . 2_555 F(3) H(33B) 2.7283 no . 2_555 F(4) H(19) 3.5524 no . 7_545 F(4) H(23B) 3.2650 no . 7_545 F(4) H(25A) 3.3574 no . 6_456 F(4) H(25B) 3.4642 no . 6_456 F(4) H(28B) 3.2872 no . 4_564 F(4) H(29B) 3.3635 no . 7_545 N(1) H(20A) 2.9771 no . 5_566 N(1) H(20B) 3.3269 no . 5_566 N(1) H(27B) 3.5635 no . 5_666 N(1) H(30A) 2.9423 no . 2_555 N(2) H(27A) 2.9275 no . 5_666 N(2) H(27B) 3.3705 no . 5_666 N(2) H(27C) 3.3887 no . 5_666 N(2) H(32B) 3.3806 no . 3_555 N(2) H(33B) 3.5589 no . 3_555 N(3) H(25B) 3.2303 no . 6_456 N(3) H(31C) 3.3794 no . 2_555 N(3) H(32A) 3.4399 no . 2_555 N(4) H(29B) 3.2333 no . 7_545 C(1) H(20A) 2.9734 no . 5_566 C(1) H(21A) 3.5579 no . 5_566 C(1) H(21B) 2.9306 no . 5_566 C(1) H(30A) 2.8977 no . 2_555 C(1) H(30B) 3.2169 no . 2_555 C(2) H(20A) 2.8978 no . 5_566 C(2) H(21B) 3.1394 no . 5_566 C(2) H(30A) 3.1959 no . 2_555 C(2) H(30B) 2.9710 no . 2_555 C(2) H(31B) 3.5913 no . 2_555 C(3) H(20A) 2.8744 no . 5_566 C(3) H(30A) 3.3980 no . 2_555 C(3) H(30B) 3.4516 no . 2_555 C(3) H(31B) 3.0516 no . 2_555 C(4) H(20A) 2.9168 no . 5_566 C(4) H(27B) 3.5098 no . 5_666 C(4) H(30A) 3.2601 no . 2_555 C(4) H(31B) 3.3040 no . 2_555 C(4) H(34B) 3.5917 no . 3_555 C(5) H(27B) 3.4018 no . 5_666 C(5) H(27C) 3.4675 no . 5_666 C(5) H(34B) 3.0643 no . 3_555 C(5) H(34C) 3.3631 no . 3_555 C(6) H(27A) 3.2824 no . 5_666 C(6) H(27B) 3.3410 no . 5_666 C(6) H(27C) 3.0372 no . 5_666 C(6) H(32B) 3.1433 no . 3_555 C(6) H(34B) 3.2337 no . 3_555 C(7) H(27A) 3.5198 no . 5_666 C(7) H(27C) 3.0265 no . 5_666 C(7) H(32B) 2.9630 no . 3_555 C(8) H(27A) 3.2947 no . 5_666 C(8) H(27C) 3.3312 no . 5_666 C(8) H(29A) 3.5792 no . 4_565 C(8) H(32B) 3.1283 no . 3_555 C(9) H(27A) 2.9157 no . 5_666 C(9) H(27C) 3.5333 no . 5_666 C(9) H(32B) 3.3670 no . 3_555 C(9) H(33B) 3.5643 no . 3_555 C(10) H(25B) 3.3259 no . 6_456 C(10) H(30B) 3.2117 no . 2_555 C(10) H(32A) 3.3814 no . 2_555 C(10) H(33C) 3.5811 no . 7_555 C(11) H(25B) 3.4720 no . 6_456 C(11) H(30B) 3.0030 no . 2_555 C(11) H(31B) 3.5840 no . 2_555 C(11) H(33C) 3.5355 no . 7_555 C(12) H(24A) 3.3705 no . 6_456 C(12) H(25B) 3.4562 no . 6_456 C(12) H(30B) 3.4783 no . 2_555 C(12) H(31B) 3.0485 no . 2_555 C(13) H(24A) 3.4467 no . 6_456 C(13) H(25B) 3.3061 no . 6_456 C(13) H(31B) 3.1993 no . 2_555 C(13) H(31C) 3.3128 no . 2_555 C(14) H(23C) 3.4883 no . 2_545 C(14) H(26A) 3.1753 no . 6_456 C(14) H(27B) 3.5125 no . 6_456 C(14) H(31B) 3.5215 no . 2_555 C(15) H(26A) 3.3699 no . 6_456 C(15) H(29B) 3.5473 no . 7_545 C(17) H(25C) 3.2168 no . 3_554 C(17) H(29B) 3.3538 no . 7_545 C(18) H(25C) 3.1067 no . 3_554 C(18) H(29B) 3.0893 no . 7_545 C(19) H(21B) 3.4291 no . 5_566 C(19) H(30B) 3.3476 no . 2_555 C(19) H(33C) 3.5191 no . 7_555 C(19) H(34A) 3.3098 no . 7_555 C(19) H(34B) 3.4946 no . 7_555 C(20) H(20A) 3.1521 no . 5_566 C(20) H(21B) 3.2636 no . 5_566 C(20) H(33C) 3.1683 no . 7_555 C(20) H(34B) 3.3209 no . 7_555 C(21) H(20A) 3.0807 no . 5_566 C(21) H(23A) 3.1469 no . 5_566 C(21) H(24A) 3.1161 no . 6_456 C(21) H(24B) 3.4651 no . 6_456 C(21) H(28A) 3.0421 no . 2_545 C(22) H(24A) 3.4894 no . 6_456 C(22) H(28A) 3.1947 no . 2_545 C(22) H(28C) 3.3858 no . 2_545 C(22) H(31B) 3.3819 no . 2_555 C(23) H(21A) 3.3841 no . 5_566 C(23) H(21B) 2.9954 no . 5_566 C(23) H(30A) 3.4436 no . 2_555 C(24) H(21A) 2.7900 no . 6_556 C(24) H(27C) 3.5997 no . 5_666 C(24) H(32B) 3.5854 no . 3_555 C(25) H(32B) 3.1848 no . 3_555 C(25) H(33A) 3.3588 no . 4_555 C(25) H(33B) 3.3354 no . 4_555 C(25) H(34C) 3.3536 no . 3_555 C(26) H(29A) 3.0677 no . 4_565 C(26) H(29C) 3.3028 no . 4_565 C(26) H(31A) 3.1679 no . 6_556 C(27) H(14) 3.2901 no . 6_556 C(27) H(27A) 3.5794 no . 5_666 C(27) H(30A) 3.3342 no . 6_556 C(27) H(31A) 3.1122 no . 6_556 C(28) H(21B) 3.3765 no . 2_555 C(28) H(22) 3.0102 no . 2_555 C(28) H(23B) 3.5615 no . 6_566 C(28) H(27A) 3.4283 no . 5_666 C(28) H(34A) 3.1312 no . 4_565 C(28) H(34C) 3.1996 no . 4_565 C(29) H(26A) 3.2166 no . 4_564 C(29) H(26B) 3.0716 no . 4_564 C(29) H(32A) 3.3561 no . 2_555 C(29) H(33A) 3.5032 no . 7_555 C(29) H(33C) 3.5401 no . 7_555 C(30) H(23C) 3.5863 no . 2_545 C(30) H(27B) 2.9943 no . 6_456 C(31) H(23C) 3.5841 no . 1_545 C(31) H(27B) 2.8597 no . 6_456 C(31) H(29C) 3.5521 no . 7_545 C(32) H(25C) 3.3120 no . 3_554 C(32) H(29A) 3.3607 no . 2_545 C(33) H(20B) 3.1823 no . 7_545 C(33) H(25B) 2.9949 no . 4_554 C(33) H(25C) 3.4056 no . 4_554 C(33) H(29C) 3.5039 no . 7_545 C(34) H(5) 3.4693 no . 3_554 C(34) H(19) 3.0048 no . 7_545 C(34) H(25C) 3.0777 no . 3_554 C(34) H(28B) 3.2102 no . 4_564 C(34) H(28C) 3.1042 no . 4_564 B(1) H(5) 3.5090 no . 2_555 B(1) H(14) 3.5242 no . 2_555 B(1) H(20B) 3.5867 no . 5_566 B(1) H(22) 3.4053 no . 2_555 B(1) H(27A) 3.4727 no . 5_666 B(2) H(28B) 3.4508 no . 4_564 B(2) H(32A) 3.5553 no . 2_555 H(5) F(1) 2.6705 no . 2_545 H(5) F(2) 3.1852 no . 2_545 H(5) C(34) 3.4693 no . 3_555 H(5) B(1) 3.5090 no . 2_545 H(5) H(23A) 3.4196 no . 2_545 H(5) H(28C) 2.8608 no . 2_545 H(5) H(34B) 3.1311 no . 3_555 H(5) H(34C) 2.9730 no . 3_555 H(14) F(2) 2.3198 no . 2_545 H(14) C(27) 3.2901 no . 6_456 H(14) B(1) 3.5242 no . 2_545 H(14) H(23C) 3.0125 no . 2_545 H(14) H(24A) 3.5794 no . 6_456 H(14) H(26A) 3.1115 no . 6_456 H(14) H(27A) 3.0051 no . 6_456 H(14) H(27B) 2.8729 no . 6_456 H(19) F(4) 3.5524 no . 7_555 H(19) C(34) 3.0048 no . 7_555 H(19) H(21B) 3.3604 no . 5_566 H(19) H(30B) 3.5028 no . 2_555 H(19) H(33C) 3.3631 no . 7_555 H(19) H(34A) 2.3971 no . 7_555 H(19) H(34B) 2.8658 no . 7_555 H(20A) N(1) 2.9771 no . 5_566 H(20A) C(1) 2.9734 no . 5_566 H(20A) C(2) 2.8978 no . 5_566 H(20A) C(3) 2.8744 no . 5_566 H(20A) C(4) 2.9168 no . 5_566 H(20A) C(20) 3.1521 no . 5_566 H(20A) C(21) 3.0807 no . 5_566 H(20A) H(20A) 2.5895 no . 5_566 H(20A) H(21B) 2.4394 no . 5_566 H(20A) H(34A) 3.5543 no . 7_555 H(20A) H(34B) 3.1750 no . 7_555 H(20B) F(1) 2.9377 no . 5_566 H(20B) N(1) 3.3269 no . 5_566 H(20B) C(33) 3.1823 no . 7_555 H(20B) B(1) 3.5867 no . 5_566 H(20B) H(24B) 3.3526 no . 6_456 H(20B) H(25B) 3.2503 no . 6_456 H(20B) H(33B) 3.3567 no . 7_555 H(20B) H(33C) 2.2713 no . 7_555 H(20B) H(34B) 2.8788 no . 7_555 H(21A) F(1) 3.2496 no . 5_566 H(21A) C(1) 3.5579 no . 5_566 H(21A) C(23) 3.3841 no . 5_566 H(21A) C(24) 2.7900 no . 6_456 H(21A) H(23A) 2.6944 no . 5_566 H(21A) H(23B) 3.5517 no . 5_566 H(21A) H(24A) 2.2152 no . 6_456 H(21A) H(24B) 2.5158 no . 6_456 H(21A) H(25B) 3.3020 no . 6_456 H(21A) H(28A) 2.7478 no . 2_545 H(21B) C(1) 2.9306 no . 5_566 H(21B) C(2) 3.1394 no . 5_566 H(21B) C(19) 3.4291 no . 5_566 H(21B) C(20) 3.2636 no . 5_566 H(21B) C(23) 2.9954 no . 5_566 H(21B) C(28) 3.3765 no . 2_545 H(21B) H(19) 3.3604 no . 5_566 H(21B) H(20A) 2.4394 no . 5_566 H(21B) H(23A) 2.7570 no . 5_566 H(21B) H(23B) 2.8501 no . 5_566 H(21B) H(28A) 2.7905 no . 2_545 H(21B) H(28B) 3.5469 no . 2_545 H(21B) H(28C) 3.2867 no . 2_545 H(22) F(2) 2.2095 no . 2_545 H(22) C(28) 3.0102 no . 2_545 H(22) B(1) 3.4053 no . 2_545 H(22) H(24A) 3.4532 no . 6_456 H(22) H(28A) 2.5671 no . 2_545 H(22) H(28C) 2.5976 no . 2_545 H(22) H(31B) 3.4979 no . 2_555 H(23A) C(21) 3.1469 no . 5_566 H(23A) H(5) 3.4196 no . 2_555 H(23A) H(21A) 2.6944 no . 5_566 H(23A) H(21B) 2.7570 no . 5_566 H(23A) H(24B) 3.1403 no . 2_555 H(23A) H(27C) 3.4141 no . 6_466 H(23A) H(28A) 3.2325 no . 6_466 H(23B) F(4) 3.2650 no . 7_555 H(23B) C(28) 3.5615 no . 6_466 H(23B) H(21A) 3.5517 no . 5_566 H(23B) H(21B) 2.8501 no . 5_566 H(23B) H(28A) 3.2823 no . 6_466 H(23B) H(28B) 2.9844 no . 6_466 H(23B) H(34A) 3.1716 no . 7_555 H(23C) C(14) 3.4883 no . 2_555 H(23C) C(30) 3.5863 no . 2_555 H(23C) C(31) 3.5841 no . 1_565 H(23C) H(14) 3.0125 no . 2_555 H(23C) H(30A) 2.9883 no . 2_555 H(23C) H(30B) 3.3899 no . 2_555 H(23C) H(31A) 3.4412 no . 1_565 H(23C) H(31B) 3.0423 no . 1_565 H(24A) C(12) 3.3705 no . 6_556 H(24A) C(13) 3.4467 no . 6_556 H(24A) C(21) 3.1161 no . 6_556 H(24A) C(22) 3.4894 no . 6_556 H(24A) H(14) 3.5794 no . 6_556 H(24A) H(21A) 2.2152 no . 6_556 H(24A) H(22) 3.4532 no . 6_556 H(24A) H(27C) 3.3898 no . 5_666 H(24A) H(28A) 3.2754 no . 5_666 H(24B) F(1) 2.3735 no . 2_545 H(24B) C(21) 3.4651 no . 6_556 H(24B) H(20B) 3.3526 no . 6_556 H(24B) H(21A) 2.5158 no . 6_556 H(24B) H(23A) 3.1403 no . 2_545 H(24B) H(33B) 3.5596 no . 4_555 H(24B) H(34C) 3.3119 no . 3_555 H(25A) F(4) 3.3574 no . 6_556 H(25A) H(29A) 2.9442 no . 4_565 H(25A) H(29B) 3.5111 no . 4_565 H(25A) H(32B) 3.0524 no . 3_555 H(25B) F(4) 3.4642 no . 6_556 H(25B) N(3) 3.2303 no . 6_556 H(25B) C(10) 3.3259 no . 6_556 H(25B) C(11) 3.4720 no . 6_556 H(25B) C(12) 3.4562 no . 6_556 H(25B) C(13) 3.3061 no . 6_556 H(25B) C(33) 2.9949 no . 4_555 H(25B) H(20B) 3.2503 no . 6_556 H(25B) H(21A) 3.3020 no . 6_556 H(25B) H(33A) 2.7015 no . 4_555 H(25B) H(33B) 2.9162 no . 4_555 H(25B) H(33C) 2.8578 no . 4_555 H(25C) C(17) 3.2168 no . 3_555 H(25C) C(18) 3.1067 no . 3_555 H(25C) C(32) 3.3120 no . 3_555 H(25C) C(33) 3.4056 no . 4_555 H(25C) C(34) 3.0777 no . 3_555 H(25C) H(32B) 2.6464 no . 3_555 H(25C) H(33A) 3.1338 no . 4_555 H(25C) H(33B) 2.9266 no . 4_555 H(25C) H(34B) 3.2710 no . 3_555 H(25C) H(34C) 2.4844 no . 3_555 H(26A) C(14) 3.1753 no . 6_556 H(26A) C(15) 3.3699 no . 6_556 H(26A) C(29) 3.2166 no . 4_565 H(26A) H(14) 3.1115 no . 6_556 H(26A) H(29A) 2.7173 no . 4_565 H(26A) H(29B) 3.3494 no . 4_565 H(26A) H(29C) 3.0773 no . 4_565 H(26A) H(31A) 3.2411 no . 6_556 H(26B) F(3) 3.1245 no . 4_565 H(26B) C(29) 3.0716 no . 4_565 H(26B) H(29A) 2.6594 no . 4_565 H(26B) H(29C) 2.6199 no . 4_565 H(26B) H(31A) 2.6840 no . 6_556 H(27A) F(2) 2.9899 no . 5_666 H(27A) N(2) 2.9275 no . 5_666 H(27A) C(6) 3.2824 no . 5_666 H(27A) C(7) 3.5198 no . 5_666 H(27A) C(8) 3.2947 no . 5_666 H(27A) C(9) 2.9157 no . 5_666 H(27A) C(27) 3.5794 no . 5_666 H(27A) C(28) 3.4283 no . 5_666 H(27A) B(1) 3.4727 no . 5_666 H(27A) H(14) 3.0051 no . 6_556 H(27A) H(27A) 3.3888 no . 5_666 H(27A) H(27C) 3.0188 no . 5_666 H(27A) H(28A) 2.9638 no . 5_666 H(27B) F(2) 3.2994 no . 5_666 H(27B) N(1) 3.5635 no . 5_666 H(27B) N(2) 3.3705 no . 5_666 H(27B) C(4) 3.5098 no . 5_666 H(27B) C(5) 3.4018 no . 5_666 H(27B) C(6) 3.3410 no . 5_666 H(27B) C(14) 3.5125 no . 6_556 H(27B) C(30) 2.9943 no . 6_556 H(27B) C(31) 2.8597 no . 6_556 H(27B) H(14) 2.8729 no . 6_556 H(27B) H(30A) 2.4062 no . 6_556 H(27B) H(31A) 2.3991 no . 6_556 H(27B) H(31B) 2.8588 no . 6_556 H(27C) N(2) 3.3887 no . 5_666 H(27C) C(5) 3.4675 no . 5_666 H(27C) C(6) 3.0372 no . 5_666 H(27C) C(7) 3.0265 no . 5_666 H(27C) C(8) 3.3312 no . 5_666 H(27C) C(9) 3.5333 no . 5_666 H(27C) C(24) 3.5997 no . 5_666 H(27C) H(23A) 3.4141 no . 6_566 H(27C) H(24A) 3.3898 no . 5_666 H(27C) H(27A) 3.0188 no . 5_666 H(27C) H(27C) 3.4445 no . 5_666 H(27C) H(31A) 3.4830 no . 6_556 H(28A) C(21) 3.0421 no . 2_555 H(28A) C(22) 3.1947 no . 2_555 H(28A) H(21A) 2.7478 no . 2_555 H(28A) H(21B) 2.7905 no . 2_555 H(28A) H(22) 2.5671 no . 2_555 H(28A) H(23A) 3.2325 no . 6_566 H(28A) H(23B) 3.2823 no . 6_566 H(28A) H(24A) 3.2754 no . 5_666 H(28A) H(27A) 2.9638 no . 5_666 H(28B) F(3) 2.5451 no . 4_565 H(28B) F(4) 3.2872 no . 4_565 H(28B) C(34) 3.2102 no . 4_565 H(28B) B(2) 3.4508 no . 4_565 H(28B) H(21B) 3.5469 no . 2_555 H(28B) H(23B) 2.9844 no . 6_566 H(28B) H(34A) 2.5769 no . 4_565 H(28B) H(34C) 2.9644 no . 4_565 H(28C) F(3) 3.4535 no . 4_565 H(28C) C(22) 3.3858 no . 2_555 H(28C) C(34) 3.1042 no . 4_565 H(28C) H(5) 2.8608 no . 2_555 H(28C) H(21B) 3.2867 no . 2_555 H(28C) H(22) 2.5976 no . 2_555 H(28C) H(33B) 3.5166 no . 3_555 H(28C) H(34A) 2.8390 no . 4_565 H(28C) H(34B) 3.4906 no . 4_565 H(28C) H(34C) 2.5692 no . 4_565 H(29A) C(8) 3.5792 no . 4_564 H(29A) C(26) 3.0677 no . 4_564 H(29A) C(32) 3.3607 no . 2_555 H(29A) H(25A) 2.9442 no . 4_564 H(29A) H(26A) 2.7173 no . 4_564 H(29A) H(26B) 2.6594 no . 4_564 H(29A) H(30B) 3.4759 no . 2_555 H(29A) H(32A) 2.5749 no . 2_555 H(29A) H(32B) 3.2684 no . 2_555 H(29B) F(4) 3.3635 no . 7_555 H(29B) N(4) 3.2333 no . 7_555 H(29B) C(15) 3.5473 no . 7_555 H(29B) C(17) 3.3538 no . 7_555 H(29B) C(18) 3.0893 no . 7_555 H(29B) H(25A) 3.5111 no . 4_564 H(29B) H(26A) 3.3494 no . 4_564 H(29B) H(33A) 3.4850 no . 7_555 H(29B) H(33C) 3.2165 no . 7_555 H(29B) H(34A) 3.4116 no . 7_555 H(29C) C(26) 3.3028 no . 4_564 H(29C) C(31) 3.5521 no . 7_555 H(29C) C(33) 3.5039 no . 7_555 H(29C) H(26A) 3.0773 no . 4_564 H(29C) H(26B) 2.6199 no . 4_564 H(29C) H(31A) 2.7741 no . 7_555 H(29C) H(31C) 3.5688 no . 7_555 H(29C) H(33A) 2.8702 no . 7_555 H(29C) H(33C) 3.3268 no . 7_555 H(30A) F(2) 3.2111 no . 2_545 H(30A) N(1) 2.9423 no . 2_545 H(30A) C(1) 2.8977 no . 2_545 H(30A) C(2) 3.1959 no . 2_545 H(30A) C(3) 3.3980 no . 2_545 H(30A) C(4) 3.2601 no . 2_545 H(30A) C(23) 3.4436 no . 2_545 H(30A) C(27) 3.3342 no . 6_456 H(30A) H(23C) 2.9883 no . 2_545 H(30A) H(27B) 2.4062 no . 6_456 H(30B) C(1) 3.2169 no . 2_545 H(30B) C(2) 2.9710 no . 2_545 H(30B) C(3) 3.4516 no . 2_545 H(30B) C(10) 3.2117 no . 2_545 H(30B) C(11) 3.0030 no . 2_545 H(30B) C(12) 3.4783 no . 2_545 H(30B) C(19) 3.3476 no . 2_545 H(30B) H(19) 3.5028 no . 2_545 H(30B) H(23C) 3.3899 no . 2_545 H(30B) H(29A) 3.4759 no . 2_545 H(31A) C(26) 3.1679 no . 6_456 H(31A) C(27) 3.1122 no . 6_456 H(31A) H(23C) 3.4412 no . 1_545 H(31A) H(26A) 3.2411 no . 6_456 H(31A) H(26B) 2.6840 no . 6_456 H(31A) H(27B) 2.3991 no . 6_456 H(31A) H(27C) 3.4830 no . 6_456 H(31A) H(29C) 2.7741 no . 7_545 H(31B) C(2) 3.5913 no . 2_545 H(31B) C(3) 3.0516 no . 2_545 H(31B) C(4) 3.3040 no . 2_545 H(31B) C(11) 3.5840 no . 2_545 H(31B) C(12) 3.0485 no . 2_545 H(31B) C(13) 3.1993 no . 2_545 H(31B) C(14) 3.5215 no . 2_545 H(31B) C(22) 3.3819 no . 2_545 H(31B) H(22) 3.4979 no . 2_545 H(31B) H(23C) 3.0423 no . 1_545 H(31B) H(27B) 2.8588 no . 6_456 H(31C) N(3) 3.3794 no . 2_545 H(31C) C(13) 3.3128 no . 2_545 H(31C) H(29C) 3.5688 no . 7_545 H(32A) F(3) 2.6384 no . 2_545 H(32A) N(3) 3.4399 no . 2_545 H(32A) C(10) 3.3814 no . 2_545 H(32A) C(29) 3.3561 no . 2_545 H(32A) B(2) 3.5553 no . 2_545 H(32A) H(29A) 2.5749 no . 2_545 H(32B) F(3) 3.3831 no . 2_545 H(32B) N(2) 3.3806 no . 3_554 H(32B) C(6) 3.1433 no . 3_554 H(32B) C(7) 2.9630 no . 3_554 H(32B) C(8) 3.1283 no . 3_554 H(32B) C(9) 3.3670 no . 3_554 H(32B) C(24) 3.5854 no . 3_554 H(32B) C(25) 3.1848 no . 3_554 H(32B) H(25A) 3.0524 no . 3_554 H(32B) H(25C) 2.6464 no . 3_554 H(32B) H(29A) 3.2684 no . 2_545 H(33A) F(3) 3.5465 no . 2_545 H(33A) C(25) 3.3588 no . 4_554 H(33A) C(29) 3.5032 no . 7_545 H(33A) H(25B) 2.7015 no . 4_554 H(33A) H(25C) 3.1338 no . 4_554 H(33A) H(29B) 3.4850 no . 7_545 H(33A) H(29C) 2.8702 no . 7_545 H(33B) F(1) 3.0655 no . 3_554 H(33B) F(3) 2.7283 no . 2_545 H(33B) N(2) 3.5589 no . 3_554 H(33B) C(9) 3.5643 no . 3_554 H(33B) C(25) 3.3354 no . 4_554 H(33B) H(20B) 3.3567 no . 7_545 H(33B) H(24B) 3.5596 no . 4_554 H(33B) H(25B) 2.9162 no . 4_554 H(33B) H(25C) 2.9266 no . 4_554 H(33B) H(28C) 3.5166 no . 3_554 H(33B) H(34C) 2.9303 no . 2_545 H(33C) F(1) 3.4429 no . 3_554 H(33C) C(10) 3.5811 no . 7_545 H(33C) C(11) 3.5355 no . 7_545 H(33C) C(19) 3.5191 no . 7_545 H(33C) C(20) 3.1683 no . 7_545 H(33C) C(29) 3.5401 no . 7_545 H(33C) H(19) 3.3631 no . 7_545 H(33C) H(20B) 2.2713 no . 7_545 H(33C) H(25B) 2.8578 no . 4_554 H(33C) H(29B) 3.2165 no . 7_545 H(33C) H(29C) 3.3268 no . 7_545 H(34A) C(19) 3.3098 no . 7_545 H(34A) C(28) 3.1312 no . 4_564 H(34A) H(19) 2.3971 no . 7_545 H(34A) H(20A) 3.5543 no . 7_545 H(34A) H(23B) 3.1716 no . 7_545 H(34A) H(28B) 2.5769 no . 4_564 H(34A) H(28C) 2.8390 no . 4_564 H(34A) H(29B) 3.4116 no . 7_545 H(34B) C(4) 3.5917 no . 3_554 H(34B) C(5) 3.0643 no . 3_554 H(34B) C(6) 3.2337 no . 3_554 H(34B) C(19) 3.4946 no . 7_545 H(34B) C(20) 3.3209 no . 7_545 H(34B) H(5) 3.1311 no . 3_554 H(34B) H(19) 2.8658 no . 7_545 H(34B) H(20A) 3.1750 no . 7_545 H(34B) H(20B) 2.8788 no . 7_545 H(34B) H(25C) 3.2710 no . 3_554 H(34B) H(28C) 3.4906 no . 4_564 H(34C) F(1) 3.5149 no . 4_564 H(34C) C(5) 3.3631 no . 3_554 H(34C) C(25) 3.3536 no . 3_554 H(34C) C(28) 3.1996 no . 4_564 H(34C) H(5) 2.9730 no . 3_554 H(34C) H(24B) 3.3119 no . 3_554 H(34C) H(25C) 2.4844 no . 3_554 H(34C) H(28B) 2.9644 no . 4_564 H(34C) H(28C) 2.5692 no . 4_564 H(34C) H(33B) 2.9303 no . 2_555 data__20100730 _database_code_depnum_ccdc_archive 'CCDC 864645' #TrackingRef '9284_web_deposit_cif_file_0_HidemitsuUno_1327633261.transEtBCODbisBODIPY.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C160 H180 B8 Cl4 F16 N16 ' _chemical_formula_moiety '4(C34 H40 B2 F4 N4), 4(C6 H5 Cl) ' _chemical_formula_weight 2859.56 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.4208(4) _cell_length_b 11.8609(2) _cell_length_c 29.0741(5) _cell_angle_alpha 90.00 _cell_angle_beta 118.0000(10) _cell_angle_gamma 90.00 _cell_volume 7435.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 28016 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 68.2 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 1.359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 0.873 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'VariMax 2.4 kW Ultra fine focus' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 83677 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 68.25 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_full 0.999 #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement SHELXL97 _computing_publication_material 'CrystalStructure 3.8.2' _computing_molecular_graphics ? #============================================================================== _reflns_number_total 13608 _reflns_number_gt 10614 _reflns_threshold_expression >2sigma(I) _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. All solvent chlorobenzene molecules disordered. The atomic coordinates of the disordered molecules were restrained. ; _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^)+(0.0658P)^2^+0.5113P] 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_number_reflns 13608 _refine_ls_number_parameters 1193 _refine_ls_number_restraints 711 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.203 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.358 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.041 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 Cl1 Cl 0.20696(10) 0.45900(15) 0.77960(5) 0.0837(6) Uani 0.663(4) 1 d PDU A 1 C69 C 0.2317(3) 0.4460(5) 0.7325(2) 0.0480(15) Uani 0.663(4) 1 d PDU A 1 C70 C 0.2847(3) 0.5015(6) 0.7417(3) 0.0636(19) Uani 0.663(4) 1 d PDU A 1 H70 H 0.3081 0.5427 0.7729 0.076 Uiso 0.663(4) 1 calc PR A 1 C71 C 0.3025(3) 0.4947(6) 0.7031(4) 0.071(2) Uani 0.663(4) 1 d PDU A 1 H71 H 0.3388 0.5337 0.7079 0.085 Uiso 0.663(4) 1 calc PR A 1 C72 C 0.2705(3) 0.4350(7) 0.6589(3) 0.064(2) Uani 0.663(4) 1 d PDU A 1 H72 H 0.2848 0.4323 0.6336 0.077 Uiso 0.663(4) 1 calc PR A 1 C73 C 0.2168(3) 0.3775(6) 0.6500(3) 0.0463(14) Uani 0.663(4) 1 d PDU A 1 H73 H 0.1945 0.3347 0.6192 0.056 Uiso 0.663(4) 1 calc PR A 1 C74 C 0.1965(3) 0.3840(5) 0.6871(2) 0.0373(11) Uani 0.663(4) 1 d PDU A 1 H74 H 0.1595 0.3471 0.6818 0.045 Uiso 0.663(4) 1 calc PR A 1 Cl1A Cl 0.2392(4) 0.5013(5) 0.7925(3) 0.131(3) Uani 0.261(4) 1 d PDU B 2 C69A C 0.2490(8) 0.4676(16) 0.7398(6) 0.055(4) Uani 0.261(4) 1 d PDU B 2 C70A C 0.2951(8) 0.5021(14) 0.7288(5) 0.037(3) Uani 0.261(4) 1 d PDU B 2 H70A H 0.3266 0.5494 0.7534 0.044 Uiso 0.261(4) 1 calc PR B 2 C71A C 0.2993(8) 0.4731(11) 0.6845(5) 0.039(3) Uani 0.261(4) 1 d PDU B 2 H71A H 0.3322 0.4999 0.6787 0.047 Uiso 0.261(4) 1 calc PR B 2 C72A C 0.2535(8) 0.4035(13) 0.6487(6) 0.052(4) Uani 0.261(4) 1 d PDU B 2 H72A H 0.2545 0.3794 0.6179 0.062 Uiso 0.261(4) 1 calc PR B 2 C73A C 0.2053(9) 0.3695(18) 0.6596(8) 0.070(6) Uani 0.261(4) 1 d PDU B 2 H73A H 0.1723 0.3260 0.6342 0.084 Uiso 0.261(4) 1 calc PR B 2 C74A C 0.2034(9) 0.3959(17) 0.7050(8) 0.072(5) Uani 0.261(4) 1 d PDU B 2 H74A H 0.1721 0.3661 0.7123 0.087 Uiso 0.261(4) 1 calc PR B 2 Cl1B Cl 0.3122(5) 0.4661(8) 0.6388(4) 0.087(4) Uani 0.0764(19) 1 d PDU C 3 C69B C 0.2781(17) 0.447(3) 0.6779(14) 0.080(8) Uani 0.0764(19) 1 d PDU C 3 C70B C 0.225(2) 0.381(4) 0.6576(17) 0.078(8) Uani 0.0764(19) 1 d PDU C 3 H70B H 0.2093 0.3504 0.6234 0.094 Uiso 0.0764(19) 1 calc PR C 3 C71B C 0.195(2) 0.358(4) 0.6865(18) 0.078(9) Uani 0.0764(19) 1 d PDU C 3 H71B H 0.1593 0.3098 0.6727 0.093 Uiso 0.0764(19) 1 calc PR C 3 C72B C 0.216(2) 0.405(4) 0.7356(17) 0.077(8) Uani 0.0764(19) 1 d PDU C 3 H72B H 0.1923 0.3984 0.7539 0.092 Uiso 0.0764(19) 1 calc PR C 3 C73B C 0.272(2) 0.464(4) 0.7575(14) 0.078(8) Uani 0.0764(19) 1 d PDU C 3 H73B H 0.2909 0.4842 0.7932 0.093 Uiso 0.0764(19) 1 calc PR C 3 C74B C 0.300(2) 0.492(5) 0.7271(17) 0.079(8) Uani 0.0764(19) 1 d PDU C 3 H74B H 0.3341 0.5419 0.7403 0.095 Uiso 0.0764(19) 1 calc PR C 3 Cl2 Cl 0.08324(8) 0.19426(12) 0.54756(6) 0.0834(4) Uani 0.50 1 d PDU D -1 C75 C 0.0392(4) 0.0764(5) 0.5224(3) 0.0475(17) Uani 0.50 1 d PDU D -1 C76 C 0.0639(4) -0.0332(6) 0.5305(4) 0.0372(14) Uani 0.50 1 d PDU D -1 H76 H 0.1075 -0.0423 0.5511 0.045 Uiso 0.50 1 calc PR D -1 C77 C 0.0281(4) -0.1278(7) 0.5099(5) 0.057(2) Uani 0.50 1 d PDU D -1 H77 H 0.0477 -0.1995 0.5159 0.069 Uiso 0.50 1 calc PR D -1 C78 C -0.0338(4) -0.1211(8) 0.4816(3) 0.070(2) Uani 0.50 1 d PDU D -1 H78 H -0.0588 -0.1867 0.4686 0.084 Uiso 0.50 1 calc PR D -1 C79 C -0.0603(5) -0.0116(9) 0.4719(4) 0.072(3) Uani 0.50 1 d PDU D -1 H79 H -0.1040 -0.0053 0.4515 0.086 Uiso 0.50 1 calc PR D -1 C80 C -0.0262(6) 0.0868(8) 0.4904(6) 0.072(3) Uani 0.50 1 d PDU D -1 H80 H -0.0458 0.1586 0.4821 0.086 Uiso 0.50 1 calc PR D -1 Cl3A Cl 0.5167(7) 0.6302(10) 0.5087(5) 0.139(4) Uani 0.126(3) 1 d PDU E -2 C81A C 0.5085(10) 0.4879(11) 0.5015(6) 0.101(4) Uani 0.126(3) 1 d PDU E -2 C82A C 0.4512(10) 0.4341(16) 0.4833(14) 0.099(4) Uani 0.126(3) 1 d PDU E -2 H82A H 0.4149 0.4765 0.4756 0.118 Uiso 0.126(3) 1 calc PR E -2 C83A C 0.4479(9) 0.3170(16) 0.4767(9) 0.097(4) Uani 0.126(3) 1 d PDU E -2 H83A H 0.4086 0.2816 0.4637 0.116 Uiso 0.126(3) 1 calc PR E -2 C84A C 0.4985(10) 0.2510(15) 0.4879(11) 0.093(4) Uani 0.126(3) 1 d PDU E -2 H84A H 0.4947 0.1721 0.4813 0.112 Uiso 0.126(3) 1 calc PR E -2 C85A C 0.5566(9) 0.3051(15) 0.5098(11) 0.099(4) Uani 0.126(3) 1 d PDU E -2 H85A H 0.5933 0.2615 0.5212 0.119 Uiso 0.126(3) 1 calc PR E -2 C86A C 0.5606(10) 0.4209(14) 0.5147(18) 0.101(4) Uani 0.126(3) 1 d PDU E -2 H86A H 0.6000 0.4560 0.5276 0.121 Uiso 0.126(3) 1 calc PR E -2 Cl3 Cl 0.47366(19) 0.7137(4) 0.49124(14) 0.1179(14) Uani 0.374(3) 1 d PDU F -3 C81 C 0.4896(4) 0.5721(6) 0.4959(3) 0.0761(17) Uani 0.374(3) 1 d PDU F -3 C82 C 0.4438(5) 0.4946(8) 0.4838(5) 0.074(2) Uani 0.374(3) 1 d PDU F -3 H82 H 0.4032 0.5198 0.4751 0.089 Uiso 0.374(3) 1 calc PR F -3 C83 C 0.4548(4) 0.3799(9) 0.4837(4) 0.079(2) Uani 0.374(3) 1 d PDU F -3 H83 H 0.4213 0.3278 0.4704 0.095 Uiso 0.374(3) 1 calc PR F -3 C84 C 0.5180(4) 0.3414(8) 0.5041(5) 0.072(2) Uani 0.374(3) 1 d PDU F -3 H84 H 0.5284 0.2637 0.5102 0.087 Uiso 0.374(3) 1 calc PR F -3 C85 C 0.5616(4) 0.4215(7) 0.5141(4) 0.0683(17) Uani 0.374(3) 1 d PDU F -3 H85 H 0.6023 0.3973 0.5227 0.082 Uiso 0.374(3) 1 calc PR F -3 C86 C 0.5509(5) 0.5374(8) 0.5128(5) 0.0714(19) Uani 0.374(3) 1 d PDU F -3 H86 H 0.5838 0.5903 0.5230 0.086 Uiso 0.374(3) 1 calc PR F -3 F1 F 0.38373(5) 0.68644(8) 0.80800(4) 0.0429(3) Uani 1 1 d . . . F2 F 0.47287(5) 0.78562(8) 0.83422(4) 0.0399(3) Uani 1 1 d . . . F3 F 0.22911(5) 0.43445(8) 0.46111(4) 0.0364(2) Uani 1 1 d . . . F4 F 0.29722(5) 0.47393(8) 0.43105(4) 0.0365(2) Uani 1 1 d . . . F5 F 0.21125(5) -0.01245(8) 0.57515(4) 0.0359(2) Uani 1 1 d . . . F6 F 0.26943(4) -0.05216(8) 0.53532(4) 0.0380(3) Uani 1 1 d . . . F7 F 0.11761(6) 0.27798(9) 0.21398(4) 0.0521(3) Uani 1 1 d . . . F8 F 0.03109(5) 0.38316(8) 0.18796(4) 0.0441(3) Uani 1 1 d . . . N1 N 0.41972(7) 0.72278(12) 0.74472(5) 0.0302(3) Uani 1 1 d . . . N2 N 0.37639(7) 0.87793(12) 0.77669(5) 0.0329(3) Uani 1 1 d . . . N3 N 0.33284(7) 0.49357(11) 0.52348(5) 0.0289(3) Uani 1 1 d . . . N4 N 0.31409(7) 0.30302(11) 0.48199(5) 0.0295(3) Uani 1 1 d . . . N5 N 0.16890(6) 0.03764(11) 0.48411(5) 0.0270(3) Uani 1 1 d . . . N6 N 0.17693(6) -0.16365(11) 0.51180(5) 0.0279(3) Uani 1 1 d . . . N7 N 0.08218(6) 0.31686(11) 0.27670(5) 0.0302(3) Uani 1 1 d . . . N8 N 0.12925(7) 0.46744(12) 0.24688(5) 0.0306(3) Uani 1 1 d . . . C1 C 0.44482(8) 0.62374(14) 0.73941(6) 0.0312(4) Uani 1 1 d . . . C2 C 0.44119(8) 0.62074(14) 0.68994(6) 0.0307(4) Uani 1 1 d . . . C3 C 0.41394(8) 0.72079(14) 0.66484(6) 0.0301(4) Uani 1 1 d . . . C4 C 0.40054(8) 0.78493(14) 0.69874(6) 0.0293(4) Uani 1 1 d . . . C5 C 0.37243(8) 0.89004(14) 0.69262(6) 0.0315(4) Uani 1 1 d . . . H5 H 0.3609 0.9307 0.6612 0.038 Uiso 1 1 calc R . . C6 C 0.36086(8) 0.93675(14) 0.73017(7) 0.0322(4) Uani 1 1 d . . . C7 C 0.32957(8) 1.03855(15) 0.73045(7) 0.0363(4) Uani 1 1 d . . . C8 C 0.32528(9) 1.03909(15) 0.77599(7) 0.0376(4) Uani 1 1 d . . . C9 C 0.35509(9) 0.93954(16) 0.80396(7) 0.0367(4) Uani 1 1 d . . . C10 C 0.33407(8) 0.60767(14) 0.53065(6) 0.0299(4) Uani 1 1 d . . . C11 C 0.37988(8) 0.63245(14) 0.58144(6) 0.0306(4) Uani 1 1 d . . . C12 C 0.40662(8) 0.53138(14) 0.60617(6) 0.0304(4) Uani 1 1 d . . . C13 C 0.37799(8) 0.44456(14) 0.56984(6) 0.0304(4) Uani 1 1 d . . . C14 C 0.39006(8) 0.32923(14) 0.57211(7) 0.0309(4) Uani 1 1 d . . . H14 H 0.4203 0.2975 0.6040 0.037 Uiso 1 1 calc R . . C15 C 0.35948(8) 0.26003(14) 0.52954(6) 0.0307(4) Uani 1 1 d . . . C16 C 0.36627(8) 0.14205(14) 0.52322(7) 0.0326(4) Uani 1 1 d . . . C17 C 0.32490(9) 0.11618(14) 0.47193(7) 0.0337(4) Uani 1 1 d . . . C18 C 0.29325(8) 0.21734(14) 0.44768(7) 0.0312(4) Uani 1 1 d . . . C19 C 0.46150(8) 0.54322(15) 0.65943(7) 0.0334(4) Uani 1 1 d . . . H19 H 0.4788 0.4696 0.6771 0.040 Uiso 1 1 calc R . . C20 C 0.50834(9) 0.61534(17) 0.64926(8) 0.0428(5) Uani 1 1 d . . . H20A H 0.5460 0.6294 0.6827 0.051 Uiso 1 1 calc R . . H20B H 0.5208 0.5728 0.6264 0.051 Uiso 1 1 calc R . . C21 C 0.47940(9) 0.72953(16) 0.62331(8) 0.0419(5) Uani 1 1 d . . . H21A H 0.4815 0.7373 0.5903 0.050 Uiso 1 1 calc R . . H21B H 0.5034 0.7921 0.6466 0.050 Uiso 1 1 calc R . . C22 C 0.40996(8) 0.73712(14) 0.61206(6) 0.0329(4) Uani 1 1 d . . . H22 H 0.3887 0.8085 0.5944 0.039 Uiso 1 1 calc R . . C23 C 0.47099(9) 0.53690(15) 0.78156(7) 0.0391(4) Uani 1 1 d . . . H23A H 0.5008 0.5726 0.8142 0.059 Uiso 0.663(4) 1 calc PR . . H23B H 0.4920 0.4783 0.7719 0.059 Uiso 0.663(4) 1 calc PR . . H23C H 0.4374 0.5030 0.7862 0.059 Uiso 0.663(4) 1 calc PR . . H23D H 0.4526 0.4633 0.7674 0.059 Uiso 0.337(4) 1 calc PR . . H23E H 0.4615 0.5576 0.8097 0.059 Uiso 0.337(4) 1 calc PR . . H23F H 0.5161 0.5329 0.7953 0.059 Uiso 0.337(4) 1 calc PR . . C24 C 0.30972(10) 1.12626(15) 0.68864(8) 0.0442(5) Uani 1 1 d . . . H24A H 0.2806 1.1790 0.6923 0.053 Uiso 1 1 calc R . . H24B H 0.2874 1.0892 0.6542 0.053 Uiso 1 1 calc R . . C25 C 0.36456(11) 1.19329(18) 0.69074(9) 0.0552(6) Uani 1 1 d . . . H25A H 0.3853 1.2340 0.7239 0.083 Uiso 1 1 calc R . . H25B H 0.3494 1.2473 0.6619 0.083 Uiso 1 1 calc R . . H25C H 0.3940 1.1414 0.6878 0.083 Uiso 1 1 calc R . . C26 C 0.29653(9) 1.12839(17) 0.79469(8) 0.0459(5) Uani 1 1 d . . . H26A H 0.2803 1.0926 0.8166 0.055 Uiso 1 1 calc R . . H26B H 0.2611 1.1626 0.7642 0.055 Uiso 1 1 calc R . . C27 C 0.34205(10) 1.22094(18) 0.82599(9) 0.0591(6) Uani 1 1 d . . . H27A H 0.3750 1.1889 0.8582 0.089 Uiso 1 1 calc R . . H27B H 0.3202 1.2797 0.8346 0.089 Uiso 1 1 calc R . . H27C H 0.3602 1.2537 0.8053 0.089 Uiso 1 1 calc R . . C28 C 0.36414(10) 0.90398(18) 0.85611(7) 0.0475(5) Uani 1 1 d . . . H28A H 0.3507 0.8256 0.8545 0.071 Uiso 0.730(11) 1 calc PR . . H28B H 0.3396 0.9526 0.8667 0.071 Uiso 0.730(11) 1 calc PR . . H28C H 0.4081 0.9103 0.8815 0.071 Uiso 0.730(11) 1 calc PR . . H28D H 0.3816 0.9668 0.8807 0.071 Uiso 0.270(11) 1 calc PR . . H28E H 0.3927 0.8397 0.8684 0.071 Uiso 0.270(11) 1 calc PR . . H28F H 0.3241 0.8820 0.8536 0.071 Uiso 0.270(11) 1 calc PR . . C29 C 0.29233(9) 0.68679(14) 0.48903(7) 0.0352(4) Uani 1 1 d . . . H29A H 0.3063 0.6940 0.4626 0.053 Uiso 1 1 calc R . . H29B H 0.2934 0.7609 0.5043 0.053 Uiso 1 1 calc R . . H29C H 0.2498 0.6575 0.4728 0.053 Uiso 1 1 calc R . . C30 C 0.41018(9) 0.06479(15) 0.56470(7) 0.0418(5) Uani 1 1 d . . . H30A H 0.3925 -0.0123 0.5578 0.050 Uiso 1 1 calc R . . H30B H 0.4143 0.0894 0.5987 0.050 Uiso 1 1 calc R . . C31 C 0.47429(10) 0.0611(2) 0.56819(8) 0.0603(6) Uani 1 1 d . . . H31A H 0.4705 0.0398 0.5343 0.091 Uiso 1 1 calc R . . H31B H 0.4999 0.0055 0.5944 0.091 Uiso 1 1 calc R . . H31C H 0.4937 0.1356 0.5781 0.091 Uiso 1 1 calc R . . C32 C 0.31376(10) 0.00304(15) 0.44549(8) 0.0430(5) Uani 1 1 d . . . H32A H 0.2695 -0.0025 0.4192 0.052 Uiso 1 1 calc R . . H32B H 0.3222 -0.0568 0.4717 0.052 Uiso 1 1 calc R . . C33 C 0.35350(12) -0.01793(19) 0.41888(9) 0.0615(6) Uani 1 1 d . . . H33A H 0.3454 0.0408 0.3928 0.092 Uiso 1 1 calc R . . H33B H 0.3433 -0.0918 0.4018 0.092 Uiso 1 1 calc R . . H33C H 0.3974 -0.0163 0.4449 0.092 Uiso 1 1 calc R . . C34 C 0.24311(8) 0.22998(15) 0.39308(6) 0.0353(4) Uani 1 1 d . . . H34A H 0.2033 0.2089 0.3911 0.053 Uiso 1 1 calc R . . H34B H 0.2517 0.1808 0.3702 0.053 Uiso 1 1 calc R . . H34C H 0.2413 0.3085 0.3820 0.053 Uiso 1 1 calc R . . C35 C 0.17241(8) 0.15287(13) 0.48458(6) 0.0274(4) Uani 1 1 d . . . C36 C 0.12593(8) 0.19431(13) 0.43667(6) 0.0276(4) Uani 1 1 d . . . C37 C 0.09364(8) 0.10259(14) 0.40691(6) 0.0285(4) Uani 1 1 d . . . C38 C 0.12008(8) 0.00456(14) 0.43596(6) 0.0276(4) Uani 1 1 d . . . C39 C 0.10240(8) -0.10705(14) 0.42507(6) 0.0290(4) Uani 1 1 d . . . H39 H 0.0705 -0.1268 0.3914 0.035 Uiso 1 1 calc R . . C40 C 0.13008(8) -0.19044(14) 0.46201(6) 0.0285(4) Uani 1 1 d . . . C41 C 0.11416(8) -0.30592(14) 0.46080(7) 0.0306(4) Uani 1 1 d . . . C42 C 0.15109(8) -0.34782(14) 0.51067(7) 0.0323(4) Uani 1 1 d . . . C43 C 0.18965(8) -0.25823(14) 0.54111(6) 0.0302(4) Uani 1 1 d . . . C44 C 0.05420(8) 0.21900(14) 0.27936(6) 0.0330(4) Uani 1 1 d . . . C45 C 0.05890(8) 0.21103(14) 0.32886(6) 0.0310(4) Uani 1 1 d . . . C46 C 0.09050(8) 0.30485(13) 0.35757(6) 0.0287(4) Uani 1 1 d . . . C47 C 0.10453(8) 0.37279(14) 0.32477(6) 0.0289(4) Uani 1 1 d . . . C48 C 0.13642(8) 0.47442(14) 0.33245(6) 0.0299(4) Uani 1 1 d . . . H48 H 0.1507 0.5120 0.3649 0.036 Uiso 1 1 calc R . . C49 C 0.14796(8) 0.52244(14) 0.29450(6) 0.0310(4) Uani 1 1 d . . . C50 C 0.18167(9) 0.62105(15) 0.29513(7) 0.0360(4) Uani 1 1 d . . . C51 C 0.18416(8) 0.62288(15) 0.24847(7) 0.0358(4) Uani 1 1 d . . . C52 C 0.15178(8) 0.52725(15) 0.21981(7) 0.0335(4) Uani 1 1 d . . . C53 C 0.09902(8) 0.30793(14) 0.41263(6) 0.0300(4) Uani 1 1 d . . . H53 H 0.1240 0.3736 0.4335 0.036 Uiso 1 1 calc R . . C54 C 0.03083(9) 0.30575(15) 0.40499(8) 0.0387(4) Uani 1 1 d . . . H54A H 0.0319 0.3043 0.4394 0.046 Uiso 1 1 calc R . . H54B H 0.0087 0.3750 0.3866 0.046 Uiso 1 1 calc R . . C55 C -0.00441(9) 0.20063(15) 0.37307(8) 0.0402(5) Uani 1 1 d . . . H55A H -0.0422 0.2251 0.3416 0.048 Uiso 1 1 calc R . . H55B H -0.0174 0.1534 0.3943 0.048 Uiso 1 1 calc R . . C56 C 0.03711(8) 0.12924(14) 0.35640(7) 0.0328(4) Uani 1 1 d . . . H56 H 0.0159 0.0611 0.3352 0.039 Uiso 1 1 calc R . . C57 C 0.21823(8) 0.21610(14) 0.53082(6) 0.0324(4) Uani 1 1 d . . . H57A H 0.2077 0.2085 0.5593 0.049 Uiso 1 1 calc R . . H57B H 0.2174 0.2959 0.5218 0.049 Uiso 1 1 calc R . . H57C H 0.2598 0.1856 0.5418 0.049 Uiso 1 1 calc R . . C58 C 0.06639(9) -0.36638(15) 0.41436(7) 0.0385(4) Uani 1 1 d . . . H58A H 0.0767 -0.4477 0.4180 0.046 Uiso 1 1 calc R . . H58B H 0.0682 -0.3387 0.3830 0.046 Uiso 1 1 calc R . . C59 C 0.00078(10) -0.35225(19) 0.40622(8) 0.0526(6) Uani 1 1 d . . . H59A H -0.0015 -0.3790 0.4371 0.079 Uiso 1 1 calc R . . H59B H -0.0277 -0.3962 0.3758 0.079 Uiso 1 1 calc R . . H59C H -0.0108 -0.2724 0.4005 0.079 Uiso 1 1 calc R . . C60 C 0.14876(11) -0.46389(15) 0.53035(8) 0.0459(5) Uani 1 1 d . . . H60A H 0.1902 -0.4836 0.5589 0.055 Uiso 1 1 calc R . . H60B H 0.1382 -0.5191 0.5019 0.055 Uiso 1 1 calc R . . C61 C 0.10121(11) -0.4722(2) 0.55025(10) 0.0713(8) Uani 1 1 d . . . H61A H 0.1134 -0.4221 0.5803 0.107 Uiso 1 1 calc R . . H61B H 0.0993 -0.5500 0.5607 0.107 Uiso 1 1 calc R . . H61C H 0.0604 -0.4497 0.5225 0.107 Uiso 1 1 calc R . . C62 C 0.23963(9) -0.26310(15) 0.59615(6) 0.0365(4) Uani 1 1 d . . . H62A H 0.2802 -0.2615 0.5969 0.055 Uiso 0.730(11) 1 calc PR . . H62B H 0.2356 -0.3329 0.6124 0.055 Uiso 0.730(11) 1 calc PR . . H62C H 0.2360 -0.1981 0.6153 0.055 Uiso 0.730(11) 1 calc PR . . H62D H 0.2210 -0.2668 0.6195 0.055 Uiso 0.270(11) 1 calc PR . . H62E H 0.2655 -0.1955 0.6041 0.055 Uiso 0.270(11) 1 calc PR . . H62F H 0.2652 -0.3302 0.6011 0.055 Uiso 0.270(11) 1 calc PR . . C63 C 0.02560(10) 0.13753(16) 0.23548(7) 0.0447(5) Uani 1 1 d . . . H63A H -0.0015 0.1781 0.2034 0.067 Uiso 0.730(11) 1 calc PR . . H63B H 0.0012 0.0821 0.2431 0.067 Uiso 0.730(11) 1 calc PR . . H63C H 0.0583 0.0987 0.2311 0.067 Uiso 0.730(11) 1 calc PR . . H63D H 0.0401 0.0612 0.2483 0.067 Uiso 0.270(11) 1 calc PR . . H63E H 0.0375 0.1572 0.2086 0.067 Uiso 0.270(11) 1 calc PR . . H63F H -0.0196 0.1405 0.2206 0.067 Uiso 0.270(11) 1 calc PR . . C64 C 0.20683(11) 0.70606(17) 0.33821(8) 0.0518(6) Uani 1 1 d . . . H64A H 0.2419 0.7463 0.3375 0.062 Uiso 1 1 calc R . . H64B H 0.2230 0.6663 0.3720 0.062 Uiso 1 1 calc R . . C65 C 0.15856(13) 0.7915(2) 0.33426(11) 0.0809(9) Uani 1 1 d . . . H65A H 0.1442 0.8343 0.3018 0.121 Uiso 1 1 calc R . . H65B H 0.1769 0.8432 0.3640 0.121 Uiso 1 1 calc R . . H65C H 0.1234 0.7521 0.3344 0.121 Uiso 1 1 calc R . . C66 C 0.21483(9) 0.70908(17) 0.22982(7) 0.0431(5) Uani 1 1 d . . . H66A H 0.2392 0.6692 0.2156 0.052 Uiso 1 1 calc R . . H66B H 0.2441 0.7544 0.2600 0.052 Uiso 1 1 calc R . . C67 C 0.16904(9) 0.78829(16) 0.18819(7) 0.0420(5) Uani 1 1 d . . . H67A H 0.1410 0.7444 0.1576 0.063 Uiso 1 1 calc R . . H67B H 0.1918 0.8427 0.1782 0.063 Uiso 1 1 calc R . . H67C H 0.1449 0.8287 0.2020 0.063 Uiso 1 1 calc R . . C68 C 0.14301(10) 0.48956(17) 0.16779(7) 0.0433(5) Uani 1 1 d . . . H68A H 0.1608 0.4141 0.1709 0.065 Uiso 0.730(11) 1 calc PR . . H68B H 0.1639 0.5424 0.1552 0.065 Uiso 0.730(11) 1 calc PR . . H68C H 0.0986 0.4874 0.1431 0.065 Uiso 0.730(11) 1 calc PR . . H68D H 0.1214 0.5485 0.1419 0.065 Uiso 0.270(11) 1 calc PR . . H68E H 0.1183 0.4202 0.1576 0.065 Uiso 0.270(11) 1 calc PR . . H68F H 0.1836 0.4752 0.1697 0.065 Uiso 0.270(11) 1 calc PR . . B1 B 0.41375(10) 0.76553(17) 0.79268(8) 0.0323(4) Uani 1 1 d . . . B2 B 0.29133(10) 0.42835(16) 0.47277(7) 0.0299(4) Uani 1 1 d . . . B3 B 0.20892(9) -0.04601(16) 0.52813(7) 0.0291(4) Uani 1 1 d . . . B4 B 0.08916(10) 0.35906(16) 0.22961(8) 0.0319(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.1174(14) 0.0717(10) 0.0407(6) 0.0103(5) 0.0194(7) 0.0169(8) C69 0.036(3) 0.033(3) 0.046(2) 0.011(2) -0.005(2) -0.004(2) C70 0.040(3) 0.045(3) 0.070(4) 0.015(3) -0.004(3) -0.006(2) C71 0.033(2) 0.059(4) 0.101(6) 0.037(4) 0.014(4) 0.002(2) C72 0.039(4) 0.061(5) 0.090(5) 0.048(4) 0.028(4) 0.018(3) C73 0.046(3) 0.043(2) 0.052(2) 0.0185(19) 0.025(2) 0.012(2) C74 0.032(2) 0.034(2) 0.034(2) 0.011(2) 0.0064(19) -0.0046(17) Cl1A 0.212(7) 0.101(4) 0.139(5) 0.059(3) 0.132(5) 0.064(4) C69A 0.045(8) 0.045(8) 0.072(8) 0.010(5) 0.026(6) -0.004(6) C70A 0.037(6) 0.042(6) 0.034(6) -0.005(5) 0.019(4) -0.002(4) C71A 0.055(7) 0.029(5) 0.021(5) -0.010(4) 0.007(5) 0.005(4) C72A 0.037(7) 0.037(6) 0.053(6) -0.007(4) -0.002(5) -0.005(5) C73A 0.053(7) 0.069(8) 0.068(9) 0.003(7) 0.011(6) -0.007(6) C74A 0.068(8) 0.057(8) 0.085(9) 0.024(7) 0.029(7) -0.011(6) Cl1B 0.078(6) 0.067(5) 0.130(8) 0.020(5) 0.061(6) 0.002(4) C69B 0.079(9) 0.076(10) 0.083(9) 0.000(6) 0.037(6) 0.004(6) C70B 0.078(10) 0.078(10) 0.080(10) 0.002(7) 0.038(7) 0.002(7) C71B 0.078(10) 0.078(10) 0.077(10) -0.001(7) 0.037(7) 0.002(7) C72B 0.078(10) 0.075(10) 0.076(10) -0.002(7) 0.035(7) 0.003(7) C73B 0.078(10) 0.077(10) 0.079(10) 0.001(7) 0.036(7) -0.001(7) C74B 0.078(10) 0.078(10) 0.082(9) 0.000(7) 0.037(7) 0.004(7) Cl2 0.1181(13) 0.0738(9) 0.0946(10) 0.0055(7) 0.0800(11) 0.0104(8) C75 0.067(4) 0.046(3) 0.042(3) 0.012(3) 0.036(3) 0.030(3) C76 0.030(3) 0.052(3) 0.034(3) -0.004(3) 0.018(2) 0.006(3) C77 0.050(4) 0.087(5) 0.048(4) -0.019(4) 0.034(3) 0.000(4) C78 0.042(4) 0.130(7) 0.047(3) -0.004(5) 0.028(3) 0.004(5) C79 0.061(4) 0.120(8) 0.042(3) 0.002(6) 0.029(3) 0.024(5) C80 0.078(5) 0.094(6) 0.055(4) 0.010(5) 0.040(4) 0.036(5) Cl3A 0.133(7) 0.154(6) 0.126(6) 0.014(5) 0.058(6) -0.005(5) C81A 0.107(6) 0.117(6) 0.091(5) 0.006(4) 0.056(4) -0.018(4) C82A 0.104(6) 0.112(6) 0.090(6) 0.005(5) 0.054(5) -0.017(4) C83A 0.104(6) 0.110(6) 0.086(6) 0.006(5) 0.053(5) -0.023(4) C84A 0.104(6) 0.109(6) 0.082(6) 0.010(4) 0.056(5) -0.026(4) C85A 0.104(6) 0.116(6) 0.087(6) 0.007(5) 0.054(5) -0.022(5) C86A 0.104(6) 0.118(6) 0.090(6) 0.006(5) 0.054(5) -0.020(4) Cl3 0.131(3) 0.179(3) 0.0652(15) 0.0267(19) 0.0646(18) 0.022(2) C81 0.058(3) 0.138(4) 0.043(2) 0.009(3) 0.033(2) 0.003(3) C82 0.050(3) 0.133(4) 0.047(3) 0.012(3) 0.028(2) -0.001(3) C83 0.053(3) 0.132(4) 0.050(3) 0.011(3) 0.023(3) -0.009(3) C84 0.057(3) 0.128(4) 0.040(3) -0.003(3) 0.029(2) -0.004(3) C85 0.044(3) 0.134(4) 0.042(2) -0.004(3) 0.032(2) -0.004(3) C86 0.047(3) 0.134(4) 0.046(3) -0.001(3) 0.032(2) 0.002(3) F1 0.0532(7) 0.0401(6) 0.0401(6) -0.0042(5) 0.0258(6) -0.0085(5) F2 0.0371(6) 0.0409(6) 0.0281(5) -0.0052(4) 0.0039(5) -0.0012(5) F3 0.0307(6) 0.0340(5) 0.0385(6) 0.0016(4) 0.0112(5) 0.0036(4) F4 0.0469(7) 0.0342(5) 0.0267(5) 0.0011(4) 0.0158(5) -0.0004(5) F5 0.0430(6) 0.0343(5) 0.0246(5) -0.0001(4) 0.0111(5) -0.0014(5) F6 0.0268(6) 0.0371(6) 0.0437(6) 0.0049(5) 0.0111(5) -0.0001(4) F7 0.0776(9) 0.0332(6) 0.0601(7) 0.0008(5) 0.0444(7) 0.0093(6) F8 0.0460(7) 0.0375(6) 0.0282(5) 0.0063(4) 0.0004(5) -0.0041(5) N1 0.0278(8) 0.0322(8) 0.0256(7) -0.0021(6) 0.0084(6) 0.0007(6) N2 0.0307(8) 0.0361(8) 0.0285(8) -0.0058(6) 0.0109(7) -0.0016(7) N3 0.0317(8) 0.0282(7) 0.0245(7) 0.0022(6) 0.0113(7) 0.0051(6) N4 0.0303(8) 0.0295(7) 0.0263(7) 0.0000(6) 0.0114(7) 0.0025(6) N5 0.0281(8) 0.0267(7) 0.0231(7) -0.0007(6) 0.0096(6) -0.0022(6) N6 0.0285(8) 0.0271(7) 0.0245(7) 0.0015(6) 0.0096(6) -0.0008(6) N7 0.0298(8) 0.0278(7) 0.0244(7) 0.0014(6) 0.0057(6) -0.0013(6) N8 0.0296(8) 0.0327(8) 0.0260(7) 0.0036(6) 0.0102(7) 0.0029(6) C1 0.0244(9) 0.0330(9) 0.0287(9) -0.0020(7) 0.0063(8) 0.0007(7) C2 0.0276(9) 0.0327(9) 0.0265(9) -0.0031(7) 0.0082(8) 0.0001(7) C3 0.0284(9) 0.0310(9) 0.0286(9) -0.0030(7) 0.0115(8) -0.0025(7) C4 0.0269(9) 0.0318(9) 0.0252(8) -0.0019(7) 0.0089(7) -0.0020(7) C5 0.0318(10) 0.0300(9) 0.0280(9) -0.0028(7) 0.0101(8) -0.0028(8) C6 0.0280(10) 0.0325(9) 0.0299(9) -0.0046(7) 0.0085(8) -0.0016(8) C7 0.0302(10) 0.0356(10) 0.0367(10) -0.0078(8) 0.0105(9) -0.0018(8) C8 0.0306(10) 0.0389(10) 0.0409(11) -0.0120(8) 0.0147(9) -0.0023(8) C9 0.0326(10) 0.0422(10) 0.0343(10) -0.0106(8) 0.0147(9) -0.0053(8) C10 0.0348(10) 0.0288(8) 0.0281(9) 0.0007(7) 0.0164(8) 0.0033(8) C11 0.0339(10) 0.0301(9) 0.0300(9) -0.0018(7) 0.0170(8) 0.0016(8) C12 0.0301(10) 0.0330(9) 0.0271(9) -0.0014(7) 0.0126(8) 0.0037(8) C13 0.0307(10) 0.0323(9) 0.0253(9) 0.0014(7) 0.0107(8) 0.0043(8) C14 0.0311(10) 0.0311(9) 0.0274(9) 0.0034(7) 0.0111(8) 0.0050(8) C15 0.0312(10) 0.0301(9) 0.0293(9) 0.0031(7) 0.0130(8) 0.0042(8) C16 0.0340(10) 0.0292(9) 0.0352(10) 0.0024(7) 0.0169(8) 0.0032(8) C17 0.0354(10) 0.0298(9) 0.0372(10) -0.0009(8) 0.0182(9) 0.0003(8) C18 0.0315(10) 0.0314(9) 0.0321(9) -0.0021(7) 0.0162(8) -0.0008(8) C19 0.0296(10) 0.0348(9) 0.0301(9) -0.0033(7) 0.0092(8) 0.0035(8) C20 0.0342(11) 0.0499(12) 0.0428(11) -0.0087(9) 0.0168(9) -0.0001(9) C21 0.0410(12) 0.0466(11) 0.0417(11) -0.0076(9) 0.0223(10) -0.0076(9) C22 0.0366(11) 0.0304(9) 0.0322(9) -0.0018(7) 0.0165(9) -0.0005(8) C23 0.0383(11) 0.0401(10) 0.0303(10) 0.0015(8) 0.0089(9) 0.0061(9) C24 0.0468(12) 0.0351(10) 0.0451(11) -0.0037(9) 0.0170(10) 0.0079(9) C25 0.0621(15) 0.0454(12) 0.0657(15) 0.0079(11) 0.0364(13) 0.0069(11) C26 0.0391(11) 0.0483(12) 0.0527(12) -0.0130(10) 0.0236(10) 0.0025(10) C27 0.0519(14) 0.0548(13) 0.0803(17) -0.0297(12) 0.0392(13) -0.0055(11) C28 0.0522(13) 0.0551(12) 0.0396(11) -0.0084(9) 0.0252(10) -0.0024(10) C29 0.0436(11) 0.0303(9) 0.0294(9) 0.0029(7) 0.0151(9) 0.0058(8) C30 0.0456(12) 0.0302(9) 0.0416(11) 0.0039(8) 0.0139(10) 0.0065(9) C31 0.0446(14) 0.0802(17) 0.0440(12) 0.0002(11) 0.0107(11) 0.0215(12) C32 0.0523(13) 0.0301(9) 0.0432(11) -0.0041(8) 0.0195(10) 0.0001(9) C33 0.0756(18) 0.0521(13) 0.0606(15) -0.0189(11) 0.0351(14) 0.0017(12) C34 0.0367(11) 0.0373(10) 0.0309(9) -0.0021(8) 0.0150(9) 0.0019(8) C35 0.0295(9) 0.0268(8) 0.0271(9) -0.0004(7) 0.0142(8) -0.0018(7) C36 0.0286(9) 0.0266(8) 0.0271(9) 0.0004(7) 0.0127(8) -0.0028(7) C37 0.0265(9) 0.0291(8) 0.0267(9) 0.0028(7) 0.0098(8) -0.0016(7) C38 0.0264(9) 0.0284(8) 0.0246(8) 0.0005(7) 0.0091(8) -0.0013(7) C39 0.0289(9) 0.0309(9) 0.0246(8) -0.0002(7) 0.0104(8) -0.0012(7) C40 0.0293(9) 0.0287(9) 0.0248(8) -0.0015(7) 0.0104(8) -0.0017(7) C41 0.0339(10) 0.0272(9) 0.0299(9) 0.0001(7) 0.0143(8) -0.0002(7) C42 0.0378(10) 0.0276(9) 0.0310(9) 0.0019(7) 0.0157(8) 0.0009(8) C43 0.0340(10) 0.0294(9) 0.0261(9) 0.0030(7) 0.0132(8) 0.0039(8) C44 0.0308(10) 0.0290(9) 0.0273(9) 0.0037(7) 0.0037(8) -0.0008(8) C45 0.0255(9) 0.0296(9) 0.0276(9) 0.0047(7) 0.0038(8) -0.0005(7) C46 0.0251(9) 0.0267(8) 0.0280(9) 0.0030(7) 0.0073(8) 0.0007(7) C47 0.0265(9) 0.0294(9) 0.0242(8) 0.0016(7) 0.0064(7) 0.0012(7) C48 0.0288(9) 0.0282(9) 0.0270(9) 0.0016(7) 0.0084(8) 0.0007(7) C49 0.0292(10) 0.0318(9) 0.0264(9) 0.0027(7) 0.0084(8) 0.0000(8) C50 0.0329(10) 0.0386(10) 0.0307(9) 0.0045(8) 0.0100(8) -0.0046(8) C51 0.0301(10) 0.0420(10) 0.0317(9) 0.0078(8) 0.0114(8) -0.0002(8) C52 0.0309(10) 0.0380(10) 0.0291(9) 0.0074(8) 0.0121(8) 0.0048(8) C53 0.0309(10) 0.0262(8) 0.0303(9) 0.0029(7) 0.0123(8) 0.0007(7) C54 0.0373(11) 0.0345(10) 0.0456(11) 0.0063(8) 0.0205(10) 0.0048(8) C55 0.0303(10) 0.0402(10) 0.0466(11) 0.0092(9) 0.0151(9) 0.0000(8) C56 0.0286(9) 0.0286(9) 0.0312(9) 0.0047(7) 0.0058(8) -0.0020(7) C57 0.0377(10) 0.0304(9) 0.0262(9) -0.0016(7) 0.0126(8) -0.0048(8) C58 0.0462(12) 0.0279(9) 0.0322(10) -0.0006(7) 0.0108(9) -0.0059(8) C59 0.0453(13) 0.0588(14) 0.0397(12) 0.0004(10) 0.0084(10) -0.0110(11) C60 0.0671(15) 0.0289(10) 0.0348(10) 0.0025(8) 0.0181(10) -0.0048(10) C61 0.0540(15) 0.0731(17) 0.0696(16) 0.0355(13) 0.0149(13) -0.0168(13) C62 0.0396(11) 0.0354(10) 0.0284(9) 0.0054(8) 0.0108(9) 0.0016(8) C63 0.0488(13) 0.0400(11) 0.0287(10) -0.0014(8) 0.0044(9) -0.0100(9) C64 0.0657(15) 0.0492(12) 0.0348(11) -0.0028(9) 0.0190(11) -0.0262(11) C65 0.098(2) 0.0779(18) 0.104(2) -0.0515(16) 0.0782(19) -0.0426(16) C66 0.0361(11) 0.0532(12) 0.0369(11) 0.0077(9) 0.0145(9) -0.0092(9) C67 0.0398(11) 0.0443(11) 0.0419(11) 0.0056(9) 0.0192(10) -0.0066(9) C68 0.0499(13) 0.0466(11) 0.0368(11) 0.0056(9) 0.0233(10) 0.0040(10) B1 0.0316(11) 0.0352(11) 0.0271(10) -0.0050(8) 0.0112(9) -0.0050(9) B2 0.0321(11) 0.0288(10) 0.0263(10) 0.0010(8) 0.0118(9) 0.0019(9) B3 0.0280(11) 0.0284(10) 0.0275(10) 0.0009(8) 0.0101(9) -0.0008(8) B4 0.0356(12) 0.0280(10) 0.0270(10) 0.0027(8) 0.0105(9) 0.0040(9) _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 Cl1 C69 1.743(7) . ? C69 C70 1.361(7) . ? C69 C74 1.400(7) . ? C70 C71 1.384(8) . ? C70 H70 0.9500 . ? C71 C72 1.350(8) . ? C71 H71 0.9500 . ? C72 C73 1.391(7) . ? C72 H72 0.9500 . ? C73 C74 1.383(6) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? Cl1A C69A 1.706(14) . ? C69A C70A 1.369(14) . ? C69A C74A 1.389(15) . ? C70A C71A 1.383(12) . ? C70A H70A 0.9500 . ? C71A C72A 1.386(13) . ? C71A H71A 0.9500 . ? C72A C73A 1.416(15) . ? C72A H72A 0.9500 . ? C73A C74A 1.377(15) . ? C73A H73A 0.9500 . ? C74A H74A 0.9500 . ? Cl1B C69B 1.711(18) . ? C69B C74B 1.378(19) . ? C69B C70B 1.390(19) . ? C70B C71B 1.383(19) . ? C70B H70B 0.9500 . ? C71B C72B 1.391(19) . ? C71B H71B 0.9500 . ? C72B C73B 1.393(19) . ? C72B H72B 0.9500 . ? C73B C74B 1.387(19) . ? C73B H73B 0.9500 . ? C74B H74B 0.9500 . ? Cl2 C75 1.705(8) . ? C75 C76 1.406(7) . ? C75 C80 1.427(12) . ? C76 C77 1.374(10) . ? C76 H76 0.9500 . ? C77 C78 1.343(11) . ? C77 H77 0.9500 . ? C78 C79 1.419(9) . ? C78 H78 0.9500 . ? C79 C80 1.387(11) . ? C79 H79 0.9500 . ? C80 H80 0.9500 . ? Cl3A C81A 1.702(9) . ? C81A C86A 1.391(10) . ? C81A C82A 1.397(10) . ? C82A C83A 1.400(10) . ? C82A H82A 0.9500 . ? C83A C84A 1.366(10) . ? C83A H83A 0.9500 . ? C84A C85A 1.407(10) . ? C84A H84A 0.9500 . ? C85A C86A 1.381(10) . ? C85A H85A 0.9500 . ? C86A H86A 0.9500 . ? Cl3 C81 1.715(7) . ? C81 C82 1.360(8) . ? C81 C86 1.401(8) . ? C82 C83 1.387(8) . ? C82 H82 0.9500 . ? C83 C84 1.444(9) . ? C83 H83 0.9500 . ? C84 C85 1.353(8) . ? C84 H84 0.9500 . ? C85 C86 1.396(8) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? F1 B1 1.387(2) . ? F2 B1 1.401(2) . ? F3 B2 1.395(2) . ? F4 B2 1.396(2) . ? F5 B3 1.399(2) . ? F6 B3 1.394(2) . ? F7 B4 1.382(2) . ? F8 B4 1.395(2) . ? N1 C1 1.367(2) . ? N1 C4 1.401(2) . ? N1 B1 1.554(2) . ? N2 C9 1.349(2) . ? N2 C6 1.406(2) . ? N2 B1 1.558(2) . ? N3 C10 1.367(2) . ? N3 C13 1.405(2) . ? N3 B2 1.548(2) . ? N4 C18 1.345(2) . ? N4 C15 1.401(2) . ? N4 B2 1.565(2) . ? N5 C35 1.3691(19) . ? N5 C38 1.403(2) . ? N5 B3 1.550(2) . ? N6 C43 1.354(2) . ? N6 C40 1.397(2) . ? N6 B3 1.560(2) . ? N7 C44 1.367(2) . ? N7 C47 1.405(2) . ? N7 B4 1.540(2) . ? N8 C52 1.353(2) . ? N8 C49 1.399(2) . ? N8 B4 1.550(2) . ? C1 C2 1.399(2) . ? C1 C23 1.495(2) . ? C2 C3 1.388(2) . ? C2 C19 1.514(2) . ? C3 C4 1.400(2) . ? C3 C22 1.504(2) . ? C4 C5 1.394(2) . ? C5 C6 1.367(2) . ? C5 H5 0.9500 . ? C6 C7 1.431(2) . ? C7 C8 1.376(2) . ? C7 C24 1.497(3) . ? C8 C9 1.425(3) . ? C8 C26 1.506(2) . ? C9 C28 1.487(2) . ? C10 C11 1.403(2) . ? C10 C29 1.492(2) . ? C11 C12 1.393(2) . ? C11 C22 1.503(2) . ? C12 C13 1.404(2) . ? C12 C19 1.505(2) . ? C13 C14 1.394(2) . ? C14 C15 1.377(2) . ? C14 H14 0.9500 . ? C15 C16 1.431(2) . ? C16 C17 1.387(2) . ? C16 C30 1.493(2) . ? C17 C18 1.422(2) . ? C17 C32 1.507(2) . ? C18 C34 1.489(2) . ? C19 C20 1.564(3) . ? C19 H19 1.0000 . ? C20 C21 1.550(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.572(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 H23D 0.9800 . ? C23 H23E 0.9800 . ? C23 H23F 0.9800 . ? C24 C25 1.534(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.523(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C28 H28D 0.9800 . ? C28 H28E 0.9800 . ? C28 H28F 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.521(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.519(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.409(2) . ? C35 C57 1.486(2) . ? C36 C37 1.383(2) . ? C36 C53 1.518(2) . ? C37 C38 1.404(2) . ? C37 C56 1.503(2) . ? C38 C39 1.382(2) . ? C39 C40 1.381(2) . ? C39 H39 0.9500 . ? C40 C41 1.420(2) . ? C41 C42 1.391(2) . ? C41 C58 1.490(2) . ? C42 C43 1.420(2) . ? C42 C60 1.502(2) . ? C43 C62 1.490(2) . ? C44 C45 1.392(2) . ? C44 C63 1.488(2) . ? C45 C46 1.388(2) . ? C45 C56 1.505(2) . ? C46 C47 1.408(2) . ? C46 C53 1.515(2) . ? C47 C48 1.395(2) . ? C48 C49 1.383(2) . ? C48 H48 0.9500 . ? C49 C50 1.426(2) . ? C50 C51 1.386(2) . ? C50 C64 1.497(3) . ? C51 C52 1.410(2) . ? C51 C66 1.511(2) . ? C52 C68 1.493(2) . ? C53 C54 1.574(2) . ? C53 H53 1.0000 . ? C54 C55 1.551(3) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.562(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.515(3) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.524(3) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C62 H62D 0.9800 . ? C62 H62E 0.9800 . ? C62 H62F 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C63 H63D 0.9800 . ? C63 H63E 0.9800 . ? C63 H63F 0.9800 . ? C64 C65 1.517(3) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.526(3) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C68 H68D 0.9800 . ? C68 H68E 0.9800 . ? C68 H68F 0.9800 . ? 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 C70 C69 C74 123.0(6) . . ? C70 C69 Cl1 116.8(6) . . ? C74 C69 Cl1 120.1(5) . . ? C69 C70 C71 116.4(7) . . ? C69 C70 H70 121.8 . . ? C71 C70 H70 121.8 . . ? C72 C71 C70 122.8(6) . . ? C72 C71 H71 118.6 . . ? C70 C71 H71 118.6 . . ? C71 C72 C73 120.5(6) . . ? C71 C72 H72 119.8 . . ? C73 C72 H72 119.8 . . ? C74 C73 C72 118.7(6) . . ? C74 C73 H73 120.6 . . ? C72 C73 H73 120.6 . . ? C73 C74 C69 118.6(5) . . ? C73 C74 H74 120.7 . . ? C69 C74 H74 120.7 . . ? C70A C69A C74A 118.7(14) . . ? C70A C69A Cl1A 128.1(13) . . ? C74A C69A Cl1A 113.2(14) . . ? C69A C70A C71A 124.8(15) . . ? C69A C70A H70A 117.6 . . ? C71A C70A H70A 117.6 . . ? C70A C71A C72A 117.4(16) . . ? C70A C71A H71A 121.3 . . ? C72A C71A H71A 121.3 . . ? C71A C72A C73A 117.7(15) . . ? C71A C72A H72A 121.2 . . ? C73A C72A H72A 121.2 . . ? C74A C73A C72A 123.8(16) . . ? C74A C73A H73A 118.1 . . ? C72A C73A H73A 118.1 . . ? C73A C74A C69A 117.4(16) . . ? C73A C74A H74A 121.3 . . ? C69A C74A H74A 121.3 . . ? C74B C69B C70B 119(2) . . ? C74B C69B Cl1B 125(2) . . ? C70B C69B Cl1B 116(2) . . ? C71B C70B C69B 121(2) . . ? C71B C70B H70B 119.6 . . ? C69B C70B H70B 119.6 . . ? C70B C71B C72B 120(2) . . ? C70B C71B H71B 120.1 . . ? C72B C71B H71B 120.1 . . ? C71B C72B C73B 119(2) . . ? C71B C72B H72B 120.6 . . ? C73B C72B H72B 120.6 . . ? C74B C73B C72B 120(2) . . ? C74B C73B H73B 120.0 . . ? C72B C73B H73B 120.0 . . ? C69B C74B C73B 120(2) . . ? C69B C74B H74B 119.8 . . ? C73B C74B H74B 119.8 . . ? C76 C75 C80 116.8(7) . . ? C76 C75 Cl2 123.4(7) . . ? C80 C75 Cl2 119.8(6) . . ? C77 C76 C75 123.1(8) . . ? C77 C76 H76 118.5 . . ? C75 C76 H76 118.5 . . ? C78 C77 C76 121.5(8) . . ? C78 C77 H77 119.3 . . ? C76 C77 H77 119.3 . . ? C77 C78 C79 116.9(9) . . ? C77 C78 H78 121.5 . . ? C79 C78 H78 121.5 . . ? C80 C79 C78 124.0(9) . . ? C80 C79 H79 118.0 . . ? C78 C79 H79 118.0 . . ? C79 C80 C75 117.6(7) . . ? C79 C80 H80 121.2 . . ? C75 C80 H80 121.2 . . ? C86A C81A C82A 117.9(11) . . ? C86A C81A Cl3A 119.6(12) . . ? C82A C81A Cl3A 122.5(12) . . ? C81A C82A C83A 119.2(12) . . ? C81A C82A H82A 120.4 . . ? C83A C82A H82A 120.4 . . ? C84A C83A C82A 123.3(12) . . ? C84A C83A H83A 118.4 . . ? C82A C83A H83A 118.4 . . ? C83A C84A C85A 116.9(12) . . ? C83A C84A H84A 121.5 . . ? C85A C84A H84A 121.5 . . ? C86A C85A C84A 120.5(13) . . ? C86A C85A H85A 119.7 . . ? C84A C85A H85A 119.7 . . ? C85A C86A C81A 121.9(12) . . ? C85A C86A H86A 119.0 . . ? C81A C86A H86A 119.0 . . ? C82 C81 C86 120.4(7) . . ? C82 C81 Cl3 120.9(6) . . ? C86 C81 Cl3 118.8(6) . . ? C81 C82 C83 121.9(8) . . ? C81 C82 H82 119.1 . . ? C83 C82 H82 119.1 . . ? C82 C83 C84 118.7(9) . . ? C82 C83 H83 120.7 . . ? C84 C83 H83 120.7 . . ? C85 C84 C83 116.6(8) . . ? C85 C84 H84 121.7 . . ? C83 C84 H84 121.7 . . ? C84 C85 C86 124.7(8) . . ? C84 C85 H85 117.7 . . ? C86 C85 H85 117.7 . . ? C85 C86 C81 117.0(8) . . ? C85 C86 H86 121.5 . . ? C81 C86 H86 121.5 . . ? C1 N1 C4 108.13(13) . . ? C1 N1 B1 128.16(14) . . ? C4 N1 B1 123.69(14) . . ? C9 N2 C6 106.98(15) . . ? C9 N2 B1 128.41(15) . . ? C6 N2 B1 124.56(14) . . ? C10 N3 C13 108.18(13) . . ? C10 N3 B2 126.68(14) . . ? C13 N3 B2 125.09(13) . . ? C18 N4 C15 107.79(14) . . ? C18 N4 B2 127.60(14) . . ? C15 N4 B2 124.58(14) . . ? C35 N5 C38 108.01(13) . . ? C35 N5 B3 128.20(14) . . ? C38 N5 B3 123.77(13) . . ? C43 N6 C40 107.35(14) . . ? C43 N6 B3 127.98(14) . . ? C40 N6 B3 124.64(13) . . ? C44 N7 C47 108.39(14) . . ? C44 N7 B4 126.37(14) . . ? C47 N7 B4 125.24(14) . . ? C52 N8 C49 107.34(14) . . ? C52 N8 B4 127.87(14) . . ? C49 N8 B4 124.78(14) . . ? N1 C1 C2 108.82(15) . . ? N1 C1 C23 122.76(15) . . ? C2 C1 C23 128.42(16) . . ? C3 C2 C1 107.57(15) . . ? C3 C2 C19 114.79(15) . . ? C1 C2 C19 137.53(16) . . ? C2 C3 C4 107.90(15) . . ? C2 C3 C22 115.58(15) . . ? C4 C3 C22 136.37(16) . . ? C5 C4 C3 131.31(16) . . ? C5 C4 N1 121.10(15) . . ? C3 C4 N1 107.58(14) . . ? C6 C5 C4 122.33(16) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 N2 120.22(16) . . ? C5 C6 C7 131.12(17) . . ? N2 C6 C7 108.48(15) . . ? C8 C7 C6 106.94(16) . . ? C8 C7 C24 129.49(17) . . ? C6 C7 C24 123.50(16) . . ? C7 C8 C9 107.21(16) . . ? C7 C8 C26 127.55(18) . . ? C9 C8 C26 125.22(17) . . ? N2 C9 C8 110.38(16) . . ? N2 C9 C28 122.14(17) . . ? C8 C9 C28 127.48(17) . . ? N3 C10 C11 108.50(14) . . ? N3 C10 C29 122.77(15) . . ? C11 C10 C29 128.73(15) . . ? C12 C11 C10 108.19(15) . . ? C12 C11 C22 115.14(15) . . ? C10 C11 C22 136.31(16) . . ? C11 C12 C13 107.20(15) . . ? C11 C12 C19 115.22(15) . . ? C13 C12 C19 136.95(15) . . ? C14 C13 C12 131.63(16) . . ? C14 C13 N3 120.29(15) . . ? C12 C13 N3 107.91(14) . . ? C15 C14 C13 121.94(16) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 N4 120.95(15) . . ? C14 C15 C16 130.68(16) . . ? N4 C15 C16 108.36(14) . . ? C17 C16 C15 106.54(15) . . ? C17 C16 C30 128.10(16) . . ? C15 C16 C30 125.37(16) . . ? C16 C17 C18 107.37(15) . . ? C16 C17 C32 127.70(16) . . ? C18 C17 C32 124.93(16) . . ? N4 C18 C17 109.95(15) . . ? N4 C18 C34 123.36(15) . . ? C17 C18 C34 126.67(16) . . ? C12 C19 C2 106.33(14) . . ? C12 C19 C20 103.51(14) . . ? C2 C19 C20 104.39(14) . . ? C12 C19 H19 113.9 . . ? C2 C19 H19 113.9 . . ? C20 C19 H19 113.9 . . ? C21 C20 C19 111.29(15) . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C20 C21 C22 110.63(15) . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C11 C22 C3 106.11(14) . . ? C11 C22 C21 104.80(14) . . ? C3 C22 C21 103.52(14) . . ? C11 C22 H22 113.8 . . ? C3 C22 H22 113.8 . . ? C21 C22 H22 113.8 . . ? C1 C23 H23A 109.5 . . ? C1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C1 C23 H23D 109.5 . . ? H23A C23 H23D 141.1 . . ? H23B C23 H23D 56.3 . . ? H23C C23 H23D 56.3 . . ? C1 C23 H23E 109.5 . . ? H23A C23 H23E 56.3 . . ? H23B C23 H23E 141.1 . . ? H23C C23 H23E 56.3 . . ? H23D C23 H23E 109.5 . . ? C1 C23 H23F 109.5 . . ? H23A C23 H23F 56.3 . . ? H23B C23 H23F 56.3 . . ? H23C C23 H23F 141.1 . . ? H23D C23 H23F 109.5 . . ? H23E C23 H23F 109.5 . . ? C7 C24 C25 112.58(17) . . ? C7 C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? C7 C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C8 C26 C27 112.92(16) . . ? C8 C26 H26A 109.0 . . ? C27 C26 H26A 109.0 . . ? C8 C26 H26B 109.0 . . ? C27 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C9 C28 H28A 109.5 . . ? C9 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C9 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C9 C28 H28D 109.5 . . ? H28A C28 H28D 141.1 . . ? H28B C28 H28D 56.3 . . ? H28C C28 H28D 56.3 . . ? C9 C28 H28E 109.5 . . ? H28A C28 H28E 56.3 . . ? H28B C28 H28E 141.1 . . ? H28C C28 H28E 56.3 . . ? H28D C28 H28E 109.5 . . ? C9 C28 H28F 109.5 . . ? H28A C28 H28F 56.3 . . ? H28B C28 H28F 56.3 . . ? H28C C28 H28F 141.1 . . ? H28D C28 H28F 109.5 . . ? H28E C28 H28F 109.5 . . ? C10 C29 H29A 109.5 . . ? C10 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C10 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C16 C30 C31 113.46(17) . . ? C16 C30 H30A 108.9 . . ? C31 C30 H30A 108.9 . . ? C16 C30 H30B 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C17 C32 C33 113.60(17) . . ? C17 C32 H32A 108.8 . . ? C33 C32 H32A 108.8 . . ? C17 C32 H32B 108.8 . . ? C33 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C18 C34 H34A 109.5 . . ? C18 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C18 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N5 C35 C36 108.70(14) . . ? N5 C35 C57 121.99(14) . . ? C36 C35 C57 129.28(15) . . ? C37 C36 C35 107.58(14) . . ? C37 C36 C53 114.43(15) . . ? C35 C36 C53 137.59(15) . . ? C36 C37 C38 108.00(14) . . ? C36 C37 C56 115.99(15) . . ? C38 C37 C56 135.58(15) . . ? C39 C38 N5 121.62(14) . . ? C39 C38 C37 130.50(16) . . ? N5 C38 C37 107.71(14) . . ? C40 C39 C38 121.43(16) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C39 C40 N6 120.46(15) . . ? C39 C40 C41 130.04(16) . . ? N6 C40 C41 109.07(14) . . ? C42 C41 C40 106.44(15) . . ? C42 C41 C58 128.42(15) . . ? C40 C41 C58 125.14(15) . . ? C41 C42 C43 107.34(14) . . ? C41 C42 C60 127.05(16) . . ? C43 C42 C60 125.52(16) . . ? N6 C43 C42 109.80(14) . . ? N6 C43 C62 122.57(15) . . ? C42 C43 C62 127.56(15) . . ? N7 C44 C45 108.38(15) . . ? N7 C44 C63 123.28(16) . . ? C45 C44 C63 128.33(16) . . ? C46 C45 C44 108.66(15) . . ? C46 C45 C56 115.63(15) . . ? C44 C45 C56 135.69(16) . . ? C45 C46 C47 107.16(15) . . ? C45 C46 C53 114.62(14) . . ? C47 C46 C53 138.20(15) . . ? C48 C47 N7 119.61(15) . . ? C48 C47 C46 132.93(15) . . ? N7 C47 C46 107.39(14) . . ? C49 C48 C47 122.38(15) . . ? C49 C48 H48 118.8 . . ? C47 C48 H48 118.8 . . ? C48 C49 N8 120.22(15) . . ? C48 C49 C50 131.33(16) . . ? N8 C49 C50 108.27(15) . . ? C51 C50 C49 106.90(16) . . ? C51 C50 C64 128.24(17) . . ? C49 C50 C64 124.83(16) . . ? C50 C51 C52 107.19(16) . . ? C50 C51 C66 128.22(17) . . ? C52 C51 C66 124.59(16) . . ? N8 C52 C51 110.27(15) . . ? N8 C52 C68 121.87(16) . . ? C51 C52 C68 127.84(16) . . ? C46 C53 C36 106.27(13) . . ? C46 C53 C54 103.84(14) . . ? C36 C53 C54 104.54(13) . . ? C46 C53 H53 113.7 . . ? C36 C53 H53 113.7 . . ? C54 C53 H53 113.7 . . ? C55 C54 C53 110.53(14) . . ? C55 C54 H54A 109.5 . . ? C53 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? C54 C55 C56 111.26(14) . . ? C54 C55 H55A 109.4 . . ? C56 C55 H55A 109.4 . . ? C54 C55 H55B 109.4 . . ? C56 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? C37 C56 C45 105.28(14) . . ? C37 C56 C55 104.06(14) . . ? C45 C56 C55 104.99(14) . . ? C37 C56 H56 113.8 . . ? C45 C56 H56 113.8 . . ? C55 C56 H56 113.8 . . ? C35 C57 H57A 109.5 . . ? C35 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C35 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C41 C58 C59 114.13(16) . . ? C41 C58 H58A 108.7 . . ? C59 C58 H58A 108.7 . . ? C41 C58 H58B 108.7 . . ? C59 C58 H58B 108.7 . . ? H58A C58 H58B 107.6 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C42 C60 C61 112.06(18) . . ? C42 C60 H60A 109.2 . . ? C61 C60 H60A 109.2 . . ? C42 C60 H60B 109.2 . . ? C61 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C43 C62 H62A 109.5 . . ? C43 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C43 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C43 C62 H62D 109.5 . . ? H62A C62 H62D 141.1 . . ? H62B C62 H62D 56.3 . . ? H62C C62 H62D 56.3 . . ? C43 C62 H62E 109.5 . . ? H62A C62 H62E 56.3 . . ? H62B C62 H62E 141.1 . . ? H62C C62 H62E 56.3 . . ? H62D C62 H62E 109.5 . . ? C43 C62 H62F 109.5 . . ? H62A C62 H62F 56.3 . . ? H62B C62 H62F 56.3 . . ? H62C C62 H62F 141.1 . . ? H62D C62 H62F 109.5 . . ? H62E C62 H62F 109.5 . . ? C44 C63 H63A 109.5 . . ? C44 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C44 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C44 C63 H63D 109.5 . . ? H63A C63 H63D 141.1 . . ? H63B C63 H63D 56.3 . . ? H63C C63 H63D 56.3 . . ? C44 C63 H63E 109.5 . . ? H63A C63 H63E 56.3 . . ? H63B C63 H63E 141.1 . . ? H63C C63 H63E 56.3 . . ? H63D C63 H63E 109.5 . . ? C44 C63 H63F 109.5 . . ? H63A C63 H63F 56.3 . . ? H63B C63 H63F 56.3 . . ? H63C C63 H63F 141.1 . . ? H63D C63 H63F 109.5 . . ? H63E C63 H63F 109.5 . . ? C50 C64 C65 112.79(18) . . ? C50 C64 H64A 109.0 . . ? C65 C64 H64A 109.0 . . ? C50 C64 H64B 109.0 . . ? C65 C64 H64B 109.0 . . ? H64A C64 H64B 107.8 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C51 C66 C67 113.53(16) . . ? C51 C66 H66A 108.9 . . ? C67 C66 H66A 108.9 . . ? C51 C66 H66B 108.9 . . ? C67 C66 H66B 108.9 . . ? H66A C66 H66B 107.7 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C52 C68 H68A 109.5 . . ? C52 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C52 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C52 C68 H68D 109.5 . . ? H68A C68 H68D 141.1 . . ? H68B C68 H68D 56.3 . . ? H68C C68 H68D 56.3 . . ? C52 C68 H68E 109.5 . . ? H68A C68 H68E 56.3 . . ? H68B C68 H68E 141.1 . . ? H68C C68 H68E 56.3 . . ? H68D C68 H68E 109.5 . . ? C52 C68 H68F 109.5 . . ? H68A C68 H68F 56.3 . . ? H68B C68 H68F 56.3 . . ? H68C C68 H68F 141.1 . . ? H68D C68 H68F 109.5 . . ? H68E C68 H68F 109.5 . . ? F1 B1 F2 108.93(15) . . ? F1 B1 N1 110.75(14) . . ? F2 B1 N1 109.66(15) . . ? F1 B1 N2 110.54(15) . . ? F2 B1 N2 109.50(14) . . ? N1 B1 N2 107.45(14) . . ? F3 B2 F4 108.28(14) . . ? F3 B2 N3 110.91(14) . . ? F4 B2 N3 110.22(14) . . ? F3 B2 N4 110.46(14) . . ? F4 B2 N4 110.09(14) . . ? N3 B2 N4 106.88(14) . . ? F6 B3 F5 108.33(15) . . ? F6 B3 N5 111.74(14) . . ? F5 B3 N5 110.20(14) . . ? F6 B3 N6 110.06(14) . . ? F5 B3 N6 109.67(14) . . ? N5 B3 N6 106.83(14) . . ? F7 B4 F8 108.67(15) . . ? F7 B4 N7 110.39(14) . . ? F8 B4 N7 110.27(16) . . ? F7 B4 N8 110.18(16) . . ? F8 B4 N8 109.96(14) . . ? N7 B4 N8 107.36(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C74 C69 C70 C71 0.5(8) . . . . ? Cl1 C69 C70 C71 -177.3(5) . . . . ? C69 C70 C71 C72 -1.2(8) . . . . ? C70 C71 C72 C73 0.6(9) . . . . ? C71 C72 C73 C74 0.8(9) . . . . ? C72 C73 C74 C69 -1.5(9) . . . . ? C70 C69 C74 C73 0.8(9) . . . . ? Cl1 C69 C74 C73 178.6(5) . . . . ? C74A C69A C70A C71A 1.7(18) . . . . ? Cl1A C69A C70A C71A -178.5(14) . . . . ? C69A C70A C71A C72A -0.4(16) . . . . ? C70A C71A C72A C73A 1(2) . . . . ? C71A C72A C73A C74A -4(3) . . . . ? C72A C73A C74A C69A 6(3) . . . . ? C70A C69A C74A C73A -4(3) . . . . ? Cl1A C69A C74A C73A 176.1(16) . . . . ? C74B C69B C70B C71B -1(3) . . . . ? Cl1B C69B C70B C71B 179(2) . . . . ? C69B C70B C71B C72B 3(2) . . . . ? C70B C71B C72B C73B -8(5) . . . . ? C71B C72B C73B C74B 12(6) . . . . ? C70B C69B C74B C73B 5(6) . . . . ? Cl1B C69B C74B C73B -175(4) . . . . ? C72B C73B C74B C69B -11(7) . . . . ? C80 C75 C76 C77 -1.2(11) . . . . ? Cl2 C75 C76 C77 -179.8(9) . . . . ? C75 C76 C77 C78 -1.8(18) . . . . ? C76 C77 C78 C79 2.7(15) . . . . ? C77 C78 C79 C80 -0.9(13) . . . . ? C78 C79 C80 C75 -1.9(19) . . . . ? C76 C75 C80 C79 2.8(14) . . . . ? Cl2 C75 C80 C79 -178.4(9) . . . . ? C86A C81A C82A C83A -3(3) . . . . ? Cl3A C81A C82A C83A 177.8(19) . . . . ? C81A C82A C83A C84A 1(4) . . . . ? C82A C83A C84A C85A 3(4) . . . . ? C83A C84A C85A C86A -6(4) . . . . ? C84A C85A C86A C81A 4(5) . . . . ? C82A C81A C86A C85A 1(4) . . . . ? Cl3A C81A C86A C85A 180(3) . . . . ? C86 C81 C82 C83 -5.1(18) . . . . ? Cl3 C81 C82 C83 175.3(8) . . . . ? C81 C82 C83 C84 9.0(15) . . . . ? C82 C83 C84 C85 -10.6(16) . . . . ? C83 C84 C85 C86 9.1(18) . . . . ? C84 C85 C86 C81 -5.3(18) . . . . ? C82 C81 C86 C85 2.9(18) . . . . ? Cl3 C81 C86 C85 -177.6(8) . . . . ? C4 N1 C1 C2 -0.84(19) . . . . ? B1 N1 C1 C2 -179.25(16) . . . . ? C4 N1 C1 C23 179.18(16) . . . . ? B1 N1 C1 C23 0.8(3) . . . . ? N1 C1 C2 C3 0.7(2) . . . . ? C23 C1 C2 C3 -179.30(17) . . . . ? N1 C1 C2 C19 176.62(19) . . . . ? C23 C1 C2 C19 -3.4(3) . . . . ? C1 C2 C3 C4 -0.3(2) . . . . ? C19 C2 C3 C4 -177.26(15) . . . . ? C1 C2 C3 C22 175.92(15) . . . . ? C19 C2 C3 C22 -1.0(2) . . . . ? C2 C3 C4 C5 -178.76(18) . . . . ? C22 C3 C4 C5 6.2(3) . . . . ? C2 C3 C4 N1 -0.19(19) . . . . ? C22 C3 C4 N1 -175.26(19) . . . . ? C1 N1 C4 C5 179.38(16) . . . . ? B1 N1 C4 C5 -2.1(2) . . . . ? C1 N1 C4 C3 0.64(19) . . . . ? B1 N1 C4 C3 179.14(15) . . . . ? C3 C4 C5 C6 176.91(18) . . . . ? N1 C4 C5 C6 -1.5(3) . . . . ? C4 C5 C6 N2 -1.1(3) . . . . ? C4 C5 C6 C7 -175.63(18) . . . . ? C9 N2 C6 C5 -174.94(16) . . . . ? B1 N2 C6 C5 7.4(3) . . . . ? C9 N2 C6 C7 0.73(19) . . . . ? B1 N2 C6 C7 -176.94(15) . . . . ? C5 C6 C7 C8 173.70(19) . . . . ? N2 C6 C7 C8 -1.3(2) . . . . ? C5 C6 C7 C24 -9.1(3) . . . . ? N2 C6 C7 C24 175.91(16) . . . . ? C6 C7 C8 C9 1.4(2) . . . . ? C24 C7 C8 C9 -175.64(18) . . . . ? C6 C7 C8 C26 179.68(18) . . . . ? C24 C7 C8 C26 2.7(3) . . . . ? C6 N2 C9 C8 0.1(2) . . . . ? B1 N2 C9 C8 177.68(16) . . . . ? C6 N2 C9 C28 -178.96(17) . . . . ? B1 N2 C9 C28 -1.4(3) . . . . ? C7 C8 C9 N2 -1.0(2) . . . . ? C26 C8 C9 N2 -179.33(17) . . . . ? C7 C8 C9 C28 178.06(19) . . . . ? C26 C8 C9 C28 -0.3(3) . . . . ? C13 N3 C10 C11 0.04(19) . . . . ? B2 N3 C10 C11 -177.53(15) . . . . ? C13 N3 C10 C29 179.52(15) . . . . ? B2 N3 C10 C29 1.9(3) . . . . ? N3 C10 C11 C12 -0.92(19) . . . . ? C29 C10 C11 C12 179.64(17) . . . . ? N3 C10 C11 C22 171.48(18) . . . . ? C29 C10 C11 C22 -8.0(3) . . . . ? C10 C11 C12 C13 1.42(19) . . . . ? C22 C11 C12 C13 -172.78(14) . . . . ? C10 C11 C12 C19 173.91(15) . . . . ? C22 C11 C12 C19 -0.3(2) . . . . ? C11 C12 C13 C14 173.86(18) . . . . ? C19 C12 C13 C14 3.8(4) . . . . ? C11 C12 C13 N3 -1.39(19) . . . . ? C19 C12 C13 N3 -171.41(19) . . . . ? C10 N3 C13 C14 -175.05(16) . . . . ? B2 N3 C13 C14 2.6(2) . . . . ? C10 N3 C13 C12 0.84(18) . . . . ? B2 N3 C13 C12 178.46(15) . . . . ? C12 C13 C14 C15 -173.74(18) . . . . ? N3 C13 C14 C15 1.0(3) . . . . ? C13 C14 C15 N4 -0.7(3) . . . . ? C13 C14 C15 C16 177.69(18) . . . . ? C18 N4 C15 C14 178.94(16) . . . . ? B2 N4 C15 C14 -3.1(3) . . . . ? C18 N4 C15 C16 0.20(19) . . . . ? B2 N4 C15 C16 178.14(15) . . . . ? C14 C15 C16 C17 -178.49(18) . . . . ? N4 C15 C16 C17 0.08(19) . . . . ? C14 C15 C16 C30 1.2(3) . . . . ? N4 C15 C16 C30 179.79(16) . . . . ? C15 C16 C17 C18 -0.32(19) . . . . ? C30 C16 C17 C18 179.99(17) . . . . ? C15 C16 C17 C32 -179.84(18) . . . . ? C30 C16 C17 C32 0.5(3) . . . . ? C15 N4 C18 C17 -0.41(19) . . . . ? B2 N4 C18 C17 -178.26(16) . . . . ? C15 N4 C18 C34 178.12(16) . . . . ? B2 N4 C18 C34 0.3(3) . . . . ? C16 C17 C18 N4 0.5(2) . . . . ? C32 C17 C18 N4 180.00(17) . . . . ? C16 C17 C18 C34 -178.00(17) . . . . ? C32 C17 C18 C34 1.5(3) . . . . ? C11 C12 C19 C2 51.3(2) . . . . ? C13 C12 C19 C2 -139.3(2) . . . . ? C11 C12 C19 C20 -58.41(19) . . . . ? C13 C12 C19 C20 111.0(2) . . . . ? C3 C2 C19 C12 -50.5(2) . . . . ? C1 C2 C19 C12 133.8(2) . . . . ? C3 C2 C19 C20 58.58(19) . . . . ? C1 C2 C19 C20 -117.1(2) . . . . ? C12 C19 C20 C21 57.53(18) . . . . ? C2 C19 C20 C21 -53.58(19) . . . . ? C19 C20 C21 C22 -2.9(2) . . . . ? C12 C11 C22 C3 -51.15(19) . . . . ? C10 C11 C22 C3 136.8(2) . . . . ? C12 C11 C22 C21 58.00(18) . . . . ? C10 C11 C22 C21 -114.0(2) . . . . ? C2 C3 C22 C11 52.0(2) . . . . ? C4 C3 C22 C11 -133.3(2) . . . . ? C2 C3 C22 C21 -58.10(19) . . . . ? C4 C3 C22 C21 116.7(2) . . . . ? C20 C21 C22 C11 -53.44(18) . . . . ? C20 C21 C22 C3 57.58(18) . . . . ? C8 C7 C24 C25 104.2(2) . . . . ? C6 C7 C24 C25 -72.4(2) . . . . ? C7 C8 C26 C27 -88.2(3) . . . . ? C9 C8 C26 C27 89.8(2) . . . . ? C17 C16 C30 C31 92.2(2) . . . . ? C15 C16 C30 C31 -87.5(2) . . . . ? C16 C17 C32 C33 -91.7(2) . . . . ? C18 C17 C32 C33 88.8(2) . . . . ? C38 N5 C35 C36 -0.14(18) . . . . ? B3 N5 C35 C36 -178.44(15) . . . . ? C38 N5 C35 C57 178.07(15) . . . . ? B3 N5 C35 C57 -0.2(3) . . . . ? N5 C35 C36 C37 0.32(19) . . . . ? C57 C35 C36 C37 -177.73(17) . . . . ? N5 C35 C36 C53 172.36(18) . . . . ? C57 C35 C36 C53 -5.7(3) . . . . ? C35 C36 C37 C38 -0.37(19) . . . . ? C53 C36 C37 C38 -174.48(14) . . . . ? C35 C36 C37 C56 173.26(14) . . . . ? C53 C36 C37 C56 -0.8(2) . . . . ? C35 N5 C38 C39 -175.73(15) . . . . ? B3 N5 C38 C39 2.7(2) . . . . ? C35 N5 C38 C37 -0.09(18) . . . . ? B3 N5 C38 C37 178.30(15) . . . . ? C36 C37 C38 C39 175.41(17) . . . . ? C56 C37 C38 C39 3.6(3) . . . . ? C36 C37 C38 N5 0.29(19) . . . . ? C56 C37 C38 N5 -171.53(18) . . . . ? N5 C38 C39 C40 3.1(3) . . . . ? C37 C38 C39 C40 -171.42(17) . . . . ? C38 C39 C40 N6 0.2(3) . . . . ? C38 C39 C40 C41 171.78(17) . . . . ? C43 N6 C40 C39 172.54(16) . . . . ? B3 N6 C40 C39 -9.5(2) . . . . ? C43 N6 C40 C41 -0.64(18) . . . . ? B3 N6 C40 C41 177.36(15) . . . . ? C39 C40 C41 C42 -171.21(18) . . . . ? N6 C40 C41 C42 1.10(19) . . . . ? C39 C40 C41 C58 8.2(3) . . . . ? N6 C40 C41 C58 -179.46(16) . . . . ? C40 C41 C42 C43 -1.12(19) . . . . ? C58 C41 C42 C43 179.47(17) . . . . ? C40 C41 C42 C60 175.57(18) . . . . ? C58 C41 C42 C60 -3.8(3) . . . . ? C40 N6 C43 C42 -0.07(19) . . . . ? B3 N6 C43 C42 -177.98(16) . . . . ? C40 N6 C43 C62 177.07(16) . . . . ? B3 N6 C43 C62 -0.8(3) . . . . ? C41 C42 C43 N6 0.8(2) . . . . ? C60 C42 C43 N6 -175.99(17) . . . . ? C41 C42 C43 C62 -176.20(17) . . . . ? C60 C42 C43 C62 7.0(3) . . . . ? C47 N7 C44 C45 -0.56(19) . . . . ? B4 N7 C44 C45 178.70(16) . . . . ? C47 N7 C44 C63 -179.44(17) . . . . ? B4 N7 C44 C63 -0.2(3) . . . . ? N7 C44 C45 C46 -0.3(2) . . . . ? C63 C44 C45 C46 178.50(18) . . . . ? N7 C44 C45 C56 177.85(18) . . . . ? C63 C44 C45 C56 -3.3(3) . . . . ? C44 C45 C46 C47 1.0(2) . . . . ? C56 C45 C46 C47 -177.53(14) . . . . ? C44 C45 C46 C53 179.83(15) . . . . ? C56 C45 C46 C53 1.3(2) . . . . ? C44 N7 C47 C48 178.60(15) . . . . ? B4 N7 C47 C48 -0.7(2) . . . . ? C44 N7 C47 C46 1.20(19) . . . . ? B4 N7 C47 C46 -178.07(15) . . . . ? C45 C46 C47 C48 -178.28(18) . . . . ? C53 C46 C47 C48 3.4(4) . . . . ? C45 C46 C47 N7 -1.37(19) . . . . ? C53 C46 C47 N7 -179.71(19) . . . . ? N7 C47 C48 C49 -1.0(3) . . . . ? C46 C47 C48 C49 175.65(18) . . . . ? C47 C48 C49 N8 -2.1(3) . . . . ? C47 C48 C49 C50 -176.54(18) . . . . ? C52 N8 C49 C48 -174.00(16) . . . . ? B4 N8 C49 C48 6.9(3) . . . . ? C52 N8 C49 C50 1.65(19) . . . . ? B4 N8 C49 C50 -177.47(15) . . . . ? C48 C49 C50 C51 173.59(19) . . . . ? N8 C49 C50 C51 -1.4(2) . . . . ? C48 C49 C50 C64 -8.3(3) . . . . ? N8 C49 C50 C64 176.74(18) . . . . ? C49 C50 C51 C52 0.6(2) . . . . ? C64 C50 C51 C52 -177.44(19) . . . . ? C49 C50 C51 C66 -179.62(18) . . . . ? C64 C50 C51 C66 2.3(3) . . . . ? C49 N8 C52 C51 -1.28(19) . . . . ? B4 N8 C52 C51 177.80(16) . . . . ? C49 N8 C52 C68 177.17(16) . . . . ? B4 N8 C52 C68 -3.8(3) . . . . ? C50 C51 C52 N8 0.4(2) . . . . ? C66 C51 C52 N8 -179.37(17) . . . . ? C50 C51 C52 C68 -177.92(18) . . . . ? C66 C51 C52 C68 2.3(3) . . . . ? C45 C46 C53 C36 50.65(19) . . . . ? C47 C46 C53 C36 -131.1(2) . . . . ? C45 C46 C53 C54 -59.30(18) . . . . ? C47 C46 C53 C54 119.0(2) . . . . ? C37 C36 C53 C46 -50.92(19) . . . . ? C35 C36 C53 C46 137.4(2) . . . . ? C37 C36 C53 C54 58.55(18) . . . . ? C35 C36 C53 C54 -113.1(2) . . . . ? C46 C53 C54 C55 56.80(17) . . . . ? C36 C53 C54 C55 -54.43(18) . . . . ? C53 C54 C55 C56 -1.6(2) . . . . ? C36 C37 C56 C45 52.34(19) . . . . ? C38 C37 C56 C45 -136.3(2) . . . . ? C36 C37 C56 C55 -57.83(18) . . . . ? C38 C37 C56 C55 113.5(2) . . . . ? C46 C45 C56 C37 -52.51(19) . . . . ? C44 C45 C56 C37 129.4(2) . . . . ? C46 C45 C56 C55 57.00(19) . . . . ? C44 C45 C56 C55 -121.1(2) . . . . ? C54 C55 C56 C37 56.36(18) . . . . ? C54 C55 C56 C45 -54.02(18) . . . . ? C42 C41 C58 C59 95.5(2) . . . . ? C40 C41 C58 C59 -83.8(2) . . . . ? C41 C42 C60 C61 -86.6(2) . . . . ? C43 C42 C60 C61 89.5(2) . . . . ? C51 C50 C64 C65 95.2(3) . . . . ? C49 C50 C64 C65 -82.6(2) . . . . ? C50 C51 C66 C67 -105.0(2) . . . . ? C52 C51 C66 C67 74.7(2) . . . . ? C1 N1 B1 F1 -54.1(2) . . . . ? C4 N1 B1 F1 127.71(17) . . . . ? C1 N1 B1 F2 66.1(2) . . . . ? C4 N1 B1 F2 -112.05(18) . . . . ? C1 N1 B1 N2 -174.93(15) . . . . ? C4 N1 B1 N2 6.9(2) . . . . ? C9 N2 B1 F1 52.3(2) . . . . ? C6 N2 B1 F1 -130.51(16) . . . . ? C9 N2 B1 F2 -67.7(2) . . . . ? C6 N2 B1 F2 109.48(18) . . . . ? C9 N2 B1 N1 173.29(16) . . . . ? C6 N2 B1 N1 -9.6(2) . . . . ? C10 N3 B2 F3 -67.7(2) . . . . ? C13 N3 B2 F3 115.10(17) . . . . ? C10 N3 B2 F4 52.2(2) . . . . ? C13 N3 B2 F4 -125.00(17) . . . . ? C10 N3 B2 N4 171.82(15) . . . . ? C13 N3 B2 N4 -5.4(2) . . . . ? C18 N4 B2 F3 62.4(2) . . . . ? C15 N4 B2 F3 -115.12(17) . . . . ? C18 N4 B2 F4 -57.1(2) . . . . ? C15 N4 B2 F4 125.35(16) . . . . ? C18 N4 B2 N3 -176.84(15) . . . . ? C15 N4 B2 N3 5.6(2) . . . . ? C35 N5 B3 F6 -71.2(2) . . . . ? C38 N5 B3 F6 110.75(17) . . . . ? C35 N5 B3 F5 49.3(2) . . . . ? C38 N5 B3 F5 -128.75(16) . . . . ? C35 N5 B3 N6 168.38(15) . . . . ? C38 N5 B3 N6 -9.7(2) . . . . ? C43 N6 B3 F6 69.2(2) . . . . ? C40 N6 B3 F6 -108.36(17) . . . . ? C43 N6 B3 F5 -49.9(2) . . . . ? C40 N6 B3 F5 132.56(16) . . . . ? C43 N6 B3 N5 -169.28(15) . . . . ? C40 N6 B3 N5 13.1(2) . . . . ? C44 N7 B4 F7 -54.6(2) . . . . ? C47 N7 B4 F7 124.51(17) . . . . ? C44 N7 B4 F8 65.5(2) . . . . ? C47 N7 B4 F8 -115.39(17) . . . . ? C44 N7 B4 N8 -174.75(15) . . . . ? C47 N7 B4 N8 4.4(2) . . . . ? C52 N8 B4 F7 53.3(2) . . . . ? C49 N8 B4 F7 -127.75(17) . . . . ? C52 N8 B4 F8 -66.4(2) . . . . ? C49 N8 B4 F8 112.49(18) . . . . ? C52 N8 B4 N7 173.58(15) . . . . ? C49 N8 B4 N7 -7.5(2) . . . . ? data_BCODBisBODIPI _database_code_depnum_ccdc_archive 'CCDC 864646' #TrackingRef '9381_web_deposit_cif_file_0_HidemitsuUno_1328148953.CisBCODBisBODIPY.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C39 H37 B2 Cl3 F4 N4' _chemical_formula_moiety 'C38 H36 B2 F4 N4, C H Cl3' _chemical_formula_weight 765.72 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' #------------------------------------------------------------------------------ _cell_length_a 16.5658(16) _cell_length_b 15.3933(15) _cell_length_c 14.3780(12) _cell_angle_alpha 90.0000 _cell_angle_beta 95.115(4) _cell_angle_gamma 90.0000 _cell_volume 3651.8(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11538 _cell_measurement_theta_min 3.92 _cell_measurement_theta_max 68.03 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.010 _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584.00 _exptl_absorpt_coefficient_mu 2.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.707 _exptl_absorpt_correction_T_max 0.973 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'VariMax 50 kV 24 mA Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 41492 _diffrn_reflns_av_R_equivalents 0.0885 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_theta_max 68.25 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 #============================================================================== # REFINEMENT DATA _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. BCOD moieties and solvent chloroform disorder. The atomic coordinates of the disordered atoms are restrained. ; _reflns_number_total 6632 _reflns_number_gt 2313 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1747 _refine_ls_R_factor_gt 0.0951 _refine_ls_wR_factor_ref 0.2128 _refine_ls_wR_factor_gt 0.1861 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_number_restraints 388 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6632 _refine_ls_number_parameters 512 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0100P)^2^+4.5500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_diff_density_max 0.410 _refine_diff_density_min -0.320 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.0090 0.0039 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0727 0.0534 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0311 0.0180 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.3639 0.7018 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== 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 Cl1 Cl 0.1607(6) 0.8124(8) 0.1655(10) 0.341(7) Uani 0.444(6) 1 d PDU A 1 Cl2 Cl 0.2564(5) 0.7189(5) 0.3008(4) 0.203(3) Uani 0.444(6) 1 d PDU A 1 Cl3 Cl 0.0734(6) 0.7556(7) 0.3074(7) 0.325(6) Uani 0.444(6) 1 d PDU A 1 C39 C 0.1551(9) 0.7240(14) 0.2449(11) 0.205(7) Uani 0.444(6) 1 d PDU A 1 H39 H 0.1417 0.6690 0.2099 0.246 Uiso 0.444(6) 1 calc PR A 1 Cl1A Cl 0.1792(5) 0.9354(9) 0.2163(6) 0.430(6) Uani 0.556(6) 1 d PDU A 2 Cl2A Cl 0.2097(12) 0.7517(12) 0.3088(15) 0.582(11) Uani 0.556(6) 1 d PDU A 2 Cl3A Cl 0.1806(16) 0.7916(14) 0.0971(15) 0.712(15) Uani 0.556(6) 1 d PDU A 2 C39A C 0.155(3) 0.8199(15) 0.2148(19) 0.485(13) Uani 0.556(6) 1 d PDU A 2 H39A H 0.0952 0.8127 0.2177 0.582 Uiso 0.556(6) 1 calc PR A 2 F1 F 0.4077(2) 0.2005(2) 0.70446(19) 0.1172(11) Uani 1 1 d . . . F2 F 0.5048(2) 0.3008(2) 0.73641(18) 0.1251(11) Uani 1 1 d . . . F3 F 0.0638(3) 0.5636(4) 0.1985(3) 0.205(2) Uani 1 1 d . . . F4 F 0.0111(3) 0.4522(5) 0.2739(3) 0.231(3) Uani 1 1 d . . . N1 N 0.4179(3) 0.3172(4) 0.5947(3) 0.1064(15) Uani 1 1 d . . . N2 N 0.5206(3) 0.2000(3) 0.6114(3) 0.1041(14) Uani 1 1 d . . . N3 N 0.1556(4) 0.4764(4) 0.2978(4) 0.137(2) Uani 1 1 d . . . N4 N 0.0917(4) 0.4198(5) 0.1460(4) 0.142(2) Uani 1 1 d . . . C1 C 0.3670(4) 0.3836(5) 0.6147(4) 0.113(2) Uani 1 1 d . . . C2 C 0.3463(4) 0.4328(5) 0.5339(4) 0.1104(19) Uani 1 1 d . . . C3 C 0.3845(4) 0.3934(4) 0.4629(4) 0.1057(18) Uani 1 1 d . . . C4 C 0.4297(4) 0.3221(5) 0.4990(3) 0.1021(18) Uani 1 1 d . . . C5 C 0.4798(4) 0.2630(4) 0.4603(3) 0.1018(18) Uani 1 1 d . . . H5 H 0.4826 0.2631 0.3946 0.122 Uiso 1 1 calc R . . C6 C 0.5255(4) 0.2045(4) 0.5134(3) 0.1014(17) Uani 1 1 d . . . C7 C 0.5814(4) 0.1409(4) 0.4915(4) 0.1078(18) Uani 1 1 d . C . C8 C 0.6116(4) 0.0990(5) 0.5720(4) 0.1118(19) Uani 1 1 d . C . C9 C 0.5732(4) 0.1380(5) 0.6463(4) 0.118(2) Uani 1 1 d . . . C10 C 0.1665(5) 0.5109(5) 0.3865(5) 0.148(3) Uani 1 1 d . . . C11 C 0.2498(4) 0.4974(5) 0.4193(5) 0.125(2) Uani 1 1 d . . . C12 C 0.2865(4) 0.4567(4) 0.3503(4) 0.113(2) Uani 1 1 d . . . C13 C 0.2290(5) 0.4414(5) 0.2753(5) 0.125(2) Uani 1 1 d . . . C14 C 0.2324(4) 0.3947(4) 0.1936(4) 0.120(2) Uani 1 1 d . . . H14 H 0.2829 0.3705 0.1801 0.145 Uiso 1 1 calc R . . C15 C 0.1662(5) 0.3818(5) 0.1314(5) 0.131(2) Uani 1 1 d . . . C16 C 0.1540(5) 0.3335(5) 0.0487(6) 0.132(2) Uani 1 1 d . E . C17 C 0.0749(6) 0.3430(6) 0.0127(6) 0.158(3) Uani 1 1 d . E . C18 C 0.0375(5) 0.3947(7) 0.0743(6) 0.160(3) Uani 1 1 d . . . C19 C 0.3023(4) 0.5166(5) 0.5076(4) 0.120(2) Uani 1 1 d . . . H19 H 0.2721 0.5417 0.5585 0.144 Uiso 1 1 calc R . . C20 C 0.3704(4) 0.5777(4) 0.4750(4) 0.130(2) Uani 1 1 d . . . H20A H 0.3464 0.6341 0.4541 0.156 Uiso 1 1 calc R . . H20B H 0.4114 0.5888 0.5280 0.156 Uiso 1 1 calc R . . C21 C 0.4115(4) 0.5350(4) 0.3939(4) 0.120(2) Uani 1 1 d . . . H21A H 0.4705 0.5301 0.4114 0.144 Uiso 1 1 calc R . . H21B H 0.4035 0.5723 0.3378 0.144 Uiso 1 1 calc R . . C22 C 0.3759(4) 0.4427(4) 0.3706(3) 0.1088(19) Uani 1 1 d . . . H22 H 0.4016 0.4127 0.3191 0.131 Uiso 1 1 calc R . . C23 C 0.6157(4) 0.1029(5) 0.4056(4) 0.116(2) Uani 1 1 d . . . H23 H 0.5944 0.1325 0.3465 0.140 Uiso 1 1 calc R B 1 C24 C 0.5970(4) 0.0071(6) 0.4053(4) 0.133(2) Uani 0.61(4) 1 d PU C 1 H24 H 0.5685 -0.0216 0.3539 0.159 Uiso 0.61(4) 1 calc PR C 1 C25 C 0.6264(4) -0.0372(5) 0.4902(5) 0.134(2) Uani 0.61(4) 1 d PU C 1 H25 H 0.6197 -0.0975 0.5011 0.160 Uiso 0.61(4) 1 calc PR C 1 C31 C 0.7080(4) 0.1082(5) 0.4230(4) 0.142(2) Uani 0.61(4) 1 d PU C 1 H31A H 0.7329 0.0811 0.3700 0.170 Uiso 0.61(4) 1 calc PR C 1 H31B H 0.7247 0.1700 0.4264 0.170 Uiso 0.61(4) 1 calc PR C 1 C32 C 0.7371(4) 0.0646(5) 0.5091(5) 0.146(2) Uani 0.61(4) 1 d PU C 1 H32A H 0.7675 0.1068 0.5507 0.175 Uiso 0.61(4) 1 calc PR C 1 H32B H 0.7752 0.0180 0.4945 0.175 Uiso 0.61(4) 1 calc PR C 1 C24A C 0.5970(4) 0.0071(6) 0.4053(4) 0.133(2) Uani 0.39(4) 1 d PU C 2 H24A H 0.5376 -0.0008 0.3952 0.159 Uiso 0.39(4) 1 calc PR C 2 H24B H 0.6213 -0.0203 0.3521 0.159 Uiso 0.39(4) 1 calc PR C 2 C25A C 0.6264(4) -0.0372(5) 0.4902(5) 0.134(2) Uani 0.39(4) 1 d PU C 2 H25A H 0.6643 -0.0839 0.4753 0.160 Uiso 0.39(4) 1 calc PR C 2 H25B H 0.5803 -0.0644 0.5184 0.160 Uiso 0.39(4) 1 calc PR C 2 C31A C 0.7080(4) 0.1082(5) 0.4230(4) 0.142(2) Uani 0.39(4) 1 d PU C 2 H31C H 0.7420 0.1365 0.3825 0.170 Uiso 0.39(4) 1 calc PR C 2 C32A C 0.7371(4) 0.0646(5) 0.5091(5) 0.146(2) Uani 0.39(4) 1 d PU C 2 H32C H 0.7928 0.0610 0.5311 0.175 Uiso 0.39(4) 1 calc PR C 2 C26 C 0.6697(4) 0.0254(5) 0.5603(4) 0.129(2) Uani 1 1 d . . . H26 H 0.6896 -0.0030 0.6206 0.154 Uiso 1 1 calc R C 1 C27 C 0.2030(5) 0.2735(6) -0.0049(6) 0.151(3) Uani 1 1 d . . . H27 H 0.2602 0.2661 0.0225 0.181 Uiso 1 1 calc R D 1 C28 C 0.1554(7) 0.1904(8) -0.0133(8) 0.238(4) Uani 0.55(6) 1 d PU E 1 H28 H 0.1784 0.1355 0.0038 0.285 Uiso 0.55(6) 1 calc PR E 1 C29 C 0.0706(7) 0.2011(8) -0.0499(9) 0.235(5) Uani 0.55(6) 1 d PU E 1 H29 H 0.0333 0.1543 -0.0584 0.282 Uiso 0.55(6) 1 calc PR E 1 C33 C 0.1956(6) 0.3003(7) -0.1033(6) 0.196(4) Uani 0.55(6) 1 d PU E 1 H33A H 0.2209 0.2555 -0.1407 0.235 Uiso 0.55(6) 1 calc PR E 1 H33B H 0.2259 0.3552 -0.1092 0.235 Uiso 0.55(6) 1 calc PR E 1 C34 C 0.1098(7) 0.3134(8) -0.1422(7) 0.216(4) Uani 0.55(6) 1 d PU E 1 H34A H 0.0987 0.2761 -0.1980 0.259 Uiso 0.55(6) 1 calc PR E 1 H34B H 0.1024 0.3746 -0.1624 0.259 Uiso 0.55(6) 1 calc PR E 1 C28A C 0.1554(7) 0.1904(8) -0.0133(8) 0.238(4) Uani 0.45(6) 1 d PU E 2 H28A H 0.1822 0.1502 -0.0547 0.285 Uiso 0.45(6) 1 calc PR E 2 H28B H 0.1569 0.1630 0.0492 0.285 Uiso 0.45(6) 1 calc PR E 2 C29A C 0.0706(7) 0.2011(8) -0.0499(9) 0.235(5) Uani 0.45(6) 1 d PU E 2 H29A H 0.0352 0.1792 -0.0032 0.282 Uiso 0.45(6) 1 calc PR E 2 H29B H 0.0603 0.1655 -0.1071 0.282 Uiso 0.45(6) 1 calc PR E 2 C33A C 0.1956(6) 0.3003(7) -0.1033(6) 0.196(4) Uani 0.45(6) 1 d PU E 2 H33C H 0.2408 0.3085 -0.1386 0.235 Uiso 0.45(6) 1 calc PR E 2 C34A C 0.1098(7) 0.3134(8) -0.1422(7) 0.216(4) Uani 0.45(6) 1 d PU E 2 H34C H 0.0947 0.3328 -0.2041 0.259 Uiso 0.45(6) 1 calc PR E 2 C30 C 0.0493(6) 0.2922(8) -0.0722(8) 0.192(4) Uani 1 1 d . . . H30 H -0.0087 0.3011 -0.0964 0.231 Uiso 1 1 calc R E 1 C35 C 0.3404(4) 0.3955(4) 0.7115(4) 0.142(2) Uani 1 1 d . . . H35A H 0.3160 0.3415 0.7318 0.213 Uiso 1 1 calc R . . H35B H 0.3004 0.4425 0.7107 0.213 Uiso 1 1 calc R . . H35C H 0.3874 0.4104 0.7548 0.213 Uiso 1 1 calc R . . C36 C 0.5847(4) 0.1186(5) 0.7494(3) 0.143(3) Uani 1 1 d . . . H36A H 0.5807 0.1727 0.7847 0.214 Uiso 1 1 calc R . . H36B H 0.6383 0.0927 0.7646 0.214 Uiso 1 1 calc R . . H36C H 0.5428 0.0780 0.7659 0.214 Uiso 1 1 calc R . . C37 C 0.1003(5) 0.5528(6) 0.4351(5) 0.187(4) Uani 1 1 d . . . H37A H 0.1001 0.6154 0.4232 0.281 Uiso 1 1 calc R . . H37B H 0.1096 0.5422 0.5024 0.281 Uiso 1 1 calc R . . H37C H 0.0480 0.5280 0.4114 0.281 Uiso 1 1 calc R . . C38 C -0.0498(5) 0.4247(7) 0.0685(6) 0.218(4) Uani 1 1 d . . . H38A H -0.0857 0.3751 0.0533 0.326 Uiso 1 1 calc R . . H38B H -0.0587 0.4691 0.0198 0.326 Uiso 1 1 calc R . . H38C H -0.0615 0.4492 0.1288 0.326 Uiso 1 1 calc R . . B1 B 0.4626(5) 0.2558(5) 0.6636(4) 0.106(2) Uani 1 1 d . . . B2 B 0.0757(8) 0.4778(10) 0.2302(8) 0.170(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.211(7) 0.291(12) 0.495(15) 0.170(11) -0.118(8) 0.014(7) Cl2 0.265(7) 0.189(6) 0.139(4) 0.016(4) -0.069(4) -0.013(5) Cl3 0.308(10) 0.349(12) 0.314(10) -0.102(8) 0.001(7) 0.036(8) C39 0.202(14) 0.29(2) 0.123(13) -0.031(12) 0.010(11) -0.037(17) Cl1A 0.369(10) 0.629(15) 0.299(9) -0.061(9) 0.070(7) -0.243(11) Cl2A 0.52(2) 0.479(18) 0.72(2) -0.113(15) -0.104(19) 0.071(17) Cl3A 0.87(3) 0.61(2) 0.66(2) -0.123(18) 0.09(2) -0.15(2) C39A 0.41(3) 0.55(2) 0.48(2) -0.05(2) -0.05(2) -0.11(3) F1 0.133(3) 0.141(3) 0.0772(18) 0.0097(18) 0.0077(17) -0.001(2) F2 0.153(3) 0.156(3) 0.0629(16) -0.0042(18) -0.0122(17) -0.008(2) F3 0.214(5) 0.256(6) 0.135(3) -0.010(4) -0.036(3) 0.097(4) F4 0.124(3) 0.422(9) 0.144(4) -0.004(5) -0.004(3) 0.011(5) N1 0.122(4) 0.136(4) 0.060(3) 0.003(3) 0.000(2) -0.003(3) N2 0.120(4) 0.135(4) 0.056(2) 0.007(3) -0.003(2) 0.004(3) N3 0.137(5) 0.177(6) 0.095(4) 0.017(4) -0.006(4) 0.027(4) N4 0.114(5) 0.197(6) 0.111(4) 0.016(4) -0.019(4) 0.011(4) C1 0.131(5) 0.135(6) 0.071(4) -0.001(4) -0.001(3) -0.006(4) C2 0.126(5) 0.134(6) 0.070(4) -0.003(4) 0.002(3) 0.001(4) C3 0.108(4) 0.136(5) 0.070(3) 0.002(4) -0.008(3) -0.013(4) C4 0.111(5) 0.136(5) 0.057(3) 0.006(3) -0.004(3) -0.011(4) C5 0.111(4) 0.135(5) 0.058(3) -0.002(3) -0.003(3) -0.001(4) C6 0.107(4) 0.132(5) 0.063(3) -0.003(3) -0.002(3) -0.002(4) C7 0.116(5) 0.140(5) 0.064(3) 0.006(3) -0.008(3) -0.004(4) C8 0.125(5) 0.142(6) 0.067(3) 0.005(4) -0.003(3) 0.002(4) C9 0.120(5) 0.163(6) 0.067(3) 0.013(4) -0.011(3) -0.003(4) C10 0.158(7) 0.185(8) 0.099(5) 0.020(5) 0.004(5) 0.021(6) C11 0.123(5) 0.153(6) 0.095(5) 0.021(4) -0.007(4) 0.017(5) C12 0.123(5) 0.144(6) 0.071(4) 0.009(4) 0.001(4) 0.010(4) C13 0.121(5) 0.166(7) 0.087(4) 0.019(4) 0.000(4) 0.023(5) C14 0.120(5) 0.152(6) 0.086(4) 0.022(4) -0.011(4) 0.003(4) C15 0.114(6) 0.165(7) 0.109(5) 0.020(5) -0.013(5) 0.008(5) C16 0.132(6) 0.143(7) 0.114(5) 0.008(5) -0.026(5) 0.001(5) C17 0.145(7) 0.195(9) 0.124(6) -0.019(6) -0.043(6) 0.020(6) C18 0.117(6) 0.217(10) 0.140(7) 0.001(6) -0.031(6) 0.004(6) C19 0.137(5) 0.139(6) 0.084(4) -0.001(4) 0.006(4) 0.016(5) C20 0.156(6) 0.133(6) 0.099(4) -0.002(4) -0.001(4) 0.003(5) C21 0.132(5) 0.135(6) 0.090(4) 0.014(4) -0.005(4) -0.011(5) C22 0.114(5) 0.143(6) 0.068(3) 0.011(3) -0.001(3) 0.011(4) C23 0.120(5) 0.163(7) 0.064(3) 0.005(4) -0.004(3) 0.004(5) C24 0.142(6) 0.158(7) 0.096(4) -0.015(4) 0.002(4) -0.010(5) C25 0.144(6) 0.145(6) 0.110(5) -0.003(4) -0.002(4) 0.001(5) C31 0.129(6) 0.200(7) 0.097(4) 0.014(4) 0.013(4) -0.001(5) C32 0.121(5) 0.199(7) 0.114(5) 0.009(5) -0.005(4) -0.004(5) C24A 0.142(6) 0.158(7) 0.096(4) -0.015(4) 0.002(4) -0.010(5) C25A 0.144(6) 0.145(6) 0.110(5) -0.003(4) -0.002(4) 0.001(5) C31A 0.129(6) 0.200(7) 0.097(4) 0.014(4) 0.013(4) -0.001(5) C32A 0.121(5) 0.199(7) 0.114(5) 0.009(5) -0.005(4) -0.004(5) C26 0.137(6) 0.161(7) 0.087(4) 0.026(4) 0.002(4) 0.032(5) C27 0.143(7) 0.163(8) 0.138(7) -0.019(6) -0.037(5) 0.000(6) C28 0.172(8) 0.210(9) 0.313(12) -0.047(9) -0.080(8) 0.023(8) C29 0.169(8) 0.214(10) 0.306(12) -0.051(9) -0.065(8) -0.005(8) C33 0.170(7) 0.295(11) 0.116(6) -0.032(7) -0.025(5) -0.001(8) C34 0.202(9) 0.298(12) 0.139(7) -0.048(8) -0.039(7) 0.028(9) C28A 0.172(8) 0.210(9) 0.313(12) -0.047(9) -0.080(8) 0.023(8) C29A 0.169(8) 0.214(10) 0.306(12) -0.051(9) -0.065(8) -0.005(8) C33A 0.170(7) 0.295(11) 0.116(6) -0.032(7) -0.025(5) -0.001(8) C34A 0.202(9) 0.298(12) 0.139(7) -0.048(8) -0.039(7) 0.028(9) C30 0.158(9) 0.210(11) 0.197(10) -0.032(9) -0.047(7) 0.038(8) C35 0.186(7) 0.167(6) 0.076(4) -0.009(4) 0.032(4) 0.015(5) C36 0.157(6) 0.206(7) 0.063(3) 0.023(4) -0.001(3) 0.043(5) C37 0.173(7) 0.260(10) 0.130(6) -0.017(6) 0.021(5) 0.069(7) C38 0.122(6) 0.347(13) 0.173(7) 0.001(8) -0.046(5) 0.045(7) B1 0.135(6) 0.120(6) 0.059(3) 0.001(4) -0.010(4) -0.007(5) B2 0.169(11) 0.218(13) 0.117(8) 0.026(9) -0.017(8) 0.034(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 Cl1 C39 1.784(17) . ? Cl2 C39 1.796(16) . ? Cl3 C39 1.758(15) . ? C39 H39 1.0000 . ? Cl1A C39A 1.82(2) . ? Cl2A C39A 1.88(2) . ? Cl3A C39A 1.83(2) . ? C39A H39A 1.0000 . ? F1 B1 1.411(8) . ? F2 B1 1.390(7) . ? F3 B2 1.406(12) . ? F4 B2 1.347(13) . ? N1 C1 1.371(7) . ? N1 C4 1.408(6) . ? N1 B1 1.514(8) . ? N2 C9 1.358(7) . ? N2 C6 1.419(6) . ? N2 B1 1.535(8) . ? N3 C10 1.379(8) . ? N3 C13 1.394(7) . ? N3 B2 1.571(11) . ? N4 C18 1.362(8) . ? N4 C15 1.398(8) . ? N4 B2 1.545(13) . ? C1 C2 1.404(7) . ? C1 C35 1.508(7) . ? C2 C3 1.388(7) . ? C2 C19 1.514(8) . ? C3 C4 1.402(8) . ? C3 C22 1.525(7) . ? C4 C5 1.382(7) . ? C5 C6 1.365(7) . ? C5 H5 0.9500 . ? C6 C7 1.402(7) . ? C7 C8 1.379(7) . ? C7 C23 1.522(8) . ? C8 C9 1.423(8) . ? C8 C26 1.507(8) . ? C9 C36 1.507(7) . ? C10 C11 1.433(8) . ? C10 C37 1.497(9) . ? C11 C12 1.361(8) . ? C11 C19 1.502(8) . ? C12 C13 1.394(8) . ? C12 C22 1.500(7) . ? C13 C14 1.383(8) . ? C14 C15 1.367(8) . ? C14 H14 0.9500 . ? C15 C16 1.401(9) . ? C16 C17 1.374(9) . ? C16 C27 1.489(9) . ? C17 C18 1.378(10) . ? C17 C30 1.480(11) . ? C18 C38 1.513(10) . ? C19 C20 1.572(8) . ? C19 H19 1.0000 . ? C20 C21 1.548(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.563(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22 1.0000 . ? C23 C24 1.507(8) . ? C23 C31 1.529(8) . ? C23 H23 1.0000 . ? C24 C25 1.444(8) . ? C24 H24 0.9500 . ? C25 C26 1.526(8) . ? C25 H25 0.9500 . ? C31 C32 1.453(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C26 1.516(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C26 H26 1.0000 . ? C27 C33 1.468(10) . ? C27 C28 1.501(12) . ? C27 H27 1.0000 . ? C28 C29 1.465(12) . ? C28 H28 0.9500 . ? C29 C30 1.474(13) . ? C29 H29 0.9500 . ? C33 C34 1.495(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C30 1.518(12) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C30 H30 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? 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 Cl3 C39 Cl1 101.7(12) . . ? Cl3 C39 Cl2 121.0(10) . . ? Cl1 C39 Cl2 102.7(9) . . ? Cl3 C39 H39 110.2 . . ? Cl1 C39 H39 110.2 . . ? Cl2 C39 H39 110.2 . . ? Cl1A C39A Cl3A 100.0(16) . . ? Cl1A C39A Cl2A 116.3(19) . . ? Cl3A C39A Cl2A 113(2) . . ? Cl1A C39A H39A 109.0 . . ? Cl3A C39A H39A 109.0 . . ? Cl2A C39A H39A 109.0 . . ? C1 N1 C4 107.9(5) . . ? C1 N1 B1 127.0(5) . . ? C4 N1 B1 124.8(6) . . ? C9 N2 C6 108.1(5) . . ? C9 N2 B1 128.5(5) . . ? C6 N2 B1 123.4(5) . . ? C10 N3 C13 108.5(6) . . ? C10 N3 B2 127.0(8) . . ? C13 N3 B2 124.5(7) . . ? C18 N4 C15 107.4(7) . . ? C18 N4 B2 127.5(8) . . ? C15 N4 B2 125.1(7) . . ? N1 C1 C2 109.8(5) . . ? N1 C1 C35 121.4(6) . . ? C2 C1 C35 128.8(7) . . ? C3 C2 C1 106.2(6) . . ? C3 C2 C19 115.4(5) . . ? C1 C2 C19 138.1(6) . . ? C2 C3 C4 109.4(5) . . ? C2 C3 C22 114.2(6) . . ? C4 C3 C22 135.9(6) . . ? C5 C4 C3 133.3(5) . . ? C5 C4 N1 120.0(6) . . ? C3 C4 N1 106.7(6) . . ? C6 C5 C4 122.1(5) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 132.7(5) . . ? C5 C6 N2 120.7(6) . . ? C7 C6 N2 106.6(5) . . ? C8 C7 C6 109.6(6) . . ? C8 C7 C23 111.6(6) . . ? C6 C7 C23 138.8(5) . . ? C7 C8 C9 106.3(6) . . ? C7 C8 C26 116.4(6) . . ? C9 C8 C26 137.2(6) . . ? N2 C9 C8 109.5(5) . . ? N2 C9 C36 121.6(6) . . ? C8 C9 C36 129.0(6) . . ? N3 C10 C11 107.0(7) . . ? N3 C10 C37 123.8(8) . . ? C11 C10 C37 129.3(7) . . ? C12 C11 C10 107.8(6) . . ? C12 C11 C19 116.4(6) . . ? C10 C11 C19 135.8(7) . . ? C11 C12 C13 108.9(6) . . ? C11 C12 C22 114.9(6) . . ? C13 C12 C22 136.1(7) . . ? C14 C13 C12 131.9(7) . . ? C14 C13 N3 120.1(7) . . ? C12 C13 N3 107.7(6) . . ? C15 C14 C13 122.6(7) . . ? C15 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? C14 C15 N4 120.6(7) . . ? C14 C15 C16 132.7(8) . . ? N4 C15 C16 106.7(7) . . ? C17 C16 C15 108.9(8) . . ? C17 C16 C27 114.6(8) . . ? C15 C16 C27 136.4(8) . . ? C16 C17 C18 106.7(8) . . ? C16 C17 C30 116.7(9) . . ? C18 C17 C30 136.3(9) . . ? N4 C18 C17 110.2(8) . . ? N4 C18 C38 121.2(9) . . ? C17 C18 C38 128.6(8) . . ? C11 C19 C2 105.8(6) . . ? C11 C19 C20 104.1(5) . . ? C2 C19 C20 104.0(5) . . ? C11 C19 H19 114.0 . . ? C2 C19 H19 114.0 . . ? C20 C19 H19 114.0 . . ? C21 C20 C19 110.2(5) . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C20 C21 C22 111.4(5) . . ? C20 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? C20 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C12 C22 C3 104.7(5) . . ? C12 C22 C21 105.0(5) . . ? C3 C22 C21 105.1(5) . . ? C12 C22 H22 113.7 . . ? C3 C22 H22 113.7 . . ? C21 C22 H22 113.7 . . ? C24 C23 C7 106.7(5) . . ? C24 C23 C31 104.8(6) . . ? C7 C23 C31 106.7(5) . . ? C24 C23 H23 112.7 . . ? C7 C23 H23 112.7 . . ? C31 C23 H23 112.7 . . ? C25 C24 C23 113.9(6) . . ? C25 C24 H24 123.0 . . ? C23 C24 H24 123.0 . . ? C24 C25 C26 111.3(6) . . ? C24 C25 H25 124.3 . . ? C26 C25 H25 124.3 . . ? C32 C31 C23 111.4(6) . . ? C32 C31 H31A 109.3 . . ? C23 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? C23 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C31 C32 C26 113.3(6) . . ? C31 C32 H32A 108.9 . . ? C26 C32 H32A 108.9 . . ? C31 C32 H32B 108.9 . . ? C26 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C8 C26 C32 105.1(6) . . ? C8 C26 C25 106.3(5) . . ? C32 C26 C25 104.7(5) . . ? C8 C26 H26 113.3 . . ? C32 C26 H26 113.3 . . ? C25 C26 H26 113.3 . . ? C33 C27 C16 108.8(7) . . ? C33 C27 C28 99.5(7) . . ? C16 C27 C28 105.2(8) . . ? C33 C27 H27 114.0 . . ? C16 C27 H27 114.0 . . ? C28 C27 H27 114.0 . . ? C29 C28 C27 114.4(9) . . ? C29 C28 H28 122.8 . . ? C27 C28 H28 122.8 . . ? C28 C29 C30 112.9(10) . . ? C28 C29 H29 123.6 . . ? C30 C29 H29 123.6 . . ? C27 C33 C34 113.2(8) . . ? C27 C33 H33A 108.9 . . ? C34 C33 H33A 108.9 . . ? C27 C33 H33B 108.9 . . ? C34 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C33 C34 C30 112.6(8) . . ? C33 C34 H34A 109.1 . . ? C30 C34 H34A 109.1 . . ? C33 C34 H34B 109.1 . . ? C30 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? C29 C30 C17 106.1(9) . . ? C29 C30 C34 100.9(10) . . ? C17 C30 C34 106.0(9) . . ? C29 C30 H30 114.2 . . ? C17 C30 H30 114.2 . . ? C34 C30 H30 114.2 . . ? C1 C35 H35A 109.5 . . ? C1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C9 C36 H36A 109.5 . . ? C9 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C9 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C10 C37 H37A 109.5 . . ? C10 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C10 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C18 C38 H38A 109.5 . . ? C18 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C18 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? F2 B1 F1 106.6(5) . . ? F2 B1 N1 111.5(6) . . ? F1 B1 N1 110.7(6) . . ? F2 B1 N2 110.7(6) . . ? F1 B1 N2 108.7(6) . . ? N1 B1 N2 108.7(5) . . ? F4 B2 F3 109.3(11) . . ? F4 B2 N4 113.3(11) . . ? F3 B2 N4 108.5(8) . . ? F4 B2 N3 111.6(8) . . ? F3 B2 N3 107.4(10) . . ? N4 B2 N3 106.4(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C2 -1.0(7) . . . . ? B1 N1 C1 C2 172.0(6) . . . . ? C4 N1 C1 C35 178.5(5) . . . . ? B1 N1 C1 C35 -8.5(10) . . . . ? N1 C1 C2 C3 1.3(7) . . . . ? C35 C1 C2 C3 -178.1(6) . . . . ? N1 C1 C2 C19 -171.9(7) . . . . ? C35 C1 C2 C19 8.7(13) . . . . ? C1 C2 C3 C4 -1.2(7) . . . . ? C19 C2 C3 C4 173.8(5) . . . . ? C1 C2 C3 C22 -174.4(5) . . . . ? C19 C2 C3 C22 0.6(8) . . . . ? C2 C3 C4 C5 -178.0(6) . . . . ? C22 C3 C4 C5 -6.9(12) . . . . ? C2 C3 C4 N1 0.6(6) . . . . ? C22 C3 C4 N1 171.7(6) . . . . ? C1 N1 C4 C5 179.1(5) . . . . ? B1 N1 C4 C5 5.9(9) . . . . ? C1 N1 C4 C3 0.2(6) . . . . ? B1 N1 C4 C3 -173.0(5) . . . . ? C3 C4 C5 C6 171.8(6) . . . . ? N1 C4 C5 C6 -6.7(9) . . . . ? C4 C5 C6 C7 -178.2(6) . . . . ? C4 C5 C6 N2 2.5(9) . . . . ? C9 N2 C6 C5 -178.8(5) . . . . ? B1 N2 C6 C5 2.8(8) . . . . ? C9 N2 C6 C7 1.7(6) . . . . ? B1 N2 C6 C7 -176.7(5) . . . . ? C5 C6 C7 C8 179.6(6) . . . . ? N2 C6 C7 C8 -1.0(7) . . . . ? C5 C6 C7 C23 -3.2(13) . . . . ? N2 C6 C7 C23 176.2(7) . . . . ? C6 C7 C8 C9 0.0(7) . . . . ? C23 C7 C8 C9 -178.0(5) . . . . ? C6 C7 C8 C26 177.1(6) . . . . ? C23 C7 C8 C26 -0.9(8) . . . . ? C6 N2 C9 C8 -1.8(7) . . . . ? B1 N2 C9 C8 176.6(6) . . . . ? C6 N2 C9 C36 178.1(6) . . . . ? B1 N2 C9 C36 -3.5(10) . . . . ? C7 C8 C9 N2 1.1(7) . . . . ? C26 C8 C9 N2 -175.1(7) . . . . ? C7 C8 C9 C36 -178.7(6) . . . . ? C26 C8 C9 C36 5.0(13) . . . . ? C13 N3 C10 C11 0.6(8) . . . . ? B2 N3 C10 C11 -177.6(8) . . . . ? C13 N3 C10 C37 -178.8(7) . . . . ? B2 N3 C10 C37 3.0(13) . . . . ? N3 C10 C11 C12 0.7(8) . . . . ? C37 C10 C11 C12 180.0(8) . . . . ? N3 C10 C11 C19 -179.1(8) . . . . ? C37 C10 C11 C19 0.2(15) . . . . ? C10 C11 C12 C13 -1.7(8) . . . . ? C19 C11 C12 C13 178.1(6) . . . . ? C10 C11 C12 C22 176.1(6) . . . . ? C19 C11 C12 C22 -4.1(9) . . . . ? C11 C12 C13 C14 -172.0(7) . . . . ? C22 C12 C13 C14 10.9(14) . . . . ? C11 C12 C13 N3 2.1(8) . . . . ? C22 C12 C13 N3 -175.0(7) . . . . ? C10 N3 C13 C14 173.3(6) . . . . ? B2 N3 C13 C14 -8.4(12) . . . . ? C10 N3 C13 C12 -1.6(8) . . . . ? B2 N3 C13 C12 176.7(8) . . . . ? C12 C13 C14 C15 174.5(7) . . . . ? N3 C13 C14 C15 1.0(10) . . . . ? C13 C14 C15 N4 3.3(11) . . . . ? C13 C14 C15 C16 -175.5(7) . . . . ? C18 N4 C15 C14 -179.1(7) . . . . ? B2 N4 C15 C14 -0.3(12) . . . . ? C18 N4 C15 C16 0.0(8) . . . . ? B2 N4 C15 C16 178.8(8) . . . . ? C14 C15 C16 C17 -179.9(8) . . . . ? N4 C15 C16 C17 1.2(9) . . . . ? C14 C15 C16 C27 3.6(15) . . . . ? N4 C15 C16 C27 -175.4(9) . . . . ? C15 C16 C17 C18 -1.9(10) . . . . ? C27 C16 C17 C18 175.5(8) . . . . ? C15 C16 C17 C30 -176.5(9) . . . . ? C27 C16 C17 C30 0.9(12) . . . . ? C15 N4 C18 C17 -1.2(10) . . . . ? B2 N4 C18 C17 -179.9(9) . . . . ? C15 N4 C18 C38 180.0(8) . . . . ? B2 N4 C18 C38 1.3(14) . . . . ? C16 C17 C18 N4 1.9(11) . . . . ? C30 C17 C18 N4 174.9(11) . . . . ? C16 C17 C18 C38 -179.4(9) . . . . ? C30 C17 C18 C38 -6(2) . . . . ? C12 C11 C19 C2 -48.8(8) . . . . ? C10 C11 C19 C2 130.9(9) . . . . ? C12 C11 C19 C20 60.4(8) . . . . ? C10 C11 C19 C20 -119.8(9) . . . . ? C3 C2 C19 C11 50.1(7) . . . . ? C1 C2 C19 C11 -137.1(8) . . . . ? C3 C2 C19 C20 -59.2(7) . . . . ? C1 C2 C19 C20 113.6(8) . . . . ? C11 C19 C20 C21 -53.3(7) . . . . ? C2 C19 C20 C21 57.3(6) . . . . ? C19 C20 C21 C22 -2.1(7) . . . . ? C11 C12 C22 C3 55.3(8) . . . . ? C13 C12 C22 C3 -127.8(8) . . . . ? C11 C12 C22 C21 -55.2(7) . . . . ? C13 C12 C22 C21 121.7(8) . . . . ? C2 C3 C22 C12 -52.9(7) . . . . ? C4 C3 C22 C12 136.3(7) . . . . ? C2 C3 C22 C21 57.5(7) . . . . ? C4 C3 C22 C21 -113.3(7) . . . . ? C20 C21 C22 C12 56.0(6) . . . . ? C20 C21 C22 C3 -54.2(6) . . . . ? C8 C7 C23 C24 55.8(7) . . . . ? C6 C7 C23 C24 -121.4(8) . . . . ? C8 C7 C23 C31 -55.8(7) . . . . ? C6 C7 C23 C31 127.0(8) . . . . ? C7 C23 C24 C25 -55.3(7) . . . . ? C31 C23 C24 C25 57.7(7) . . . . ? C23 C24 C25 C26 0.1(8) . . . . ? C24 C23 C31 C32 -57.0(7) . . . . ? C7 C23 C31 C32 55.9(8) . . . . ? C23 C31 C32 C26 -0.3(9) . . . . ? C7 C8 C26 C32 56.1(7) . . . . ? C9 C8 C26 C32 -127.9(8) . . . . ? C7 C8 C26 C25 -54.6(8) . . . . ? C9 C8 C26 C25 121.4(8) . . . . ? C31 C32 C26 C8 -54.0(8) . . . . ? C31 C32 C26 C25 57.9(8) . . . . ? C24 C25 C26 C8 53.4(7) . . . . ? C24 C25 C26 C32 -57.6(7) . . . . ? C17 C16 C27 C33 52.6(10) . . . . ? C15 C16 C27 C33 -131.0(9) . . . . ? C17 C16 C27 C28 -53.2(10) . . . . ? C15 C16 C27 C28 123.2(10) . . . . ? C33 C27 C28 C29 -60.6(12) . . . . ? C16 C27 C28 C29 52.0(12) . . . . ? C27 C28 C29 C30 0.5(16) . . . . ? C16 C27 C33 C34 -49.9(11) . . . . ? C28 C27 C33 C34 59.8(11) . . . . ? C27 C33 C34 C30 -2.4(14) . . . . ? C28 C29 C30 C17 -52.3(14) . . . . ? C28 C29 C30 C34 58.0(12) . . . . ? C16 C17 C30 C29 53.5(13) . . . . ? C18 C17 C30 C29 -119.0(13) . . . . ? C16 C17 C30 C34 -53.2(12) . . . . ? C18 C17 C30 C34 134.3(12) . . . . ? C33 C34 C30 C29 -57.7(12) . . . . ? C33 C34 C30 C17 52.7(12) . . . . ? C1 N1 B1 F2 -50.6(9) . . . . ? C4 N1 B1 F2 121.3(6) . . . . ? C1 N1 B1 F1 67.9(8) . . . . ? C4 N1 B1 F1 -120.3(6) . . . . ? C1 N1 B1 N2 -172.8(5) . . . . ? C4 N1 B1 N2 -1.0(8) . . . . ? C9 N2 B1 F2 55.9(9) . . . . ? C6 N2 B1 F2 -126.0(5) . . . . ? C9 N2 B1 F1 -60.8(8) . . . . ? C6 N2 B1 F1 117.3(6) . . . . ? C9 N2 B1 N1 178.6(5) . . . . ? C6 N2 B1 N1 -3.3(8) . . . . ? C18 N4 B2 F4 50.0(13) . . . . ? C15 N4 B2 F4 -128.6(9) . . . . ? C18 N4 B2 F3 -71.7(13) . . . . ? C15 N4 B2 F3 109.8(9) . . . . ? C18 N4 B2 N3 173.0(7) . . . . ? C15 N4 B2 N3 -5.5(13) . . . . ? C10 N3 B2 F4 -48.1(15) . . . . ? C13 N3 B2 F4 134.0(10) . . . . ? C10 N3 B2 F3 71.8(12) . . . . ? C13 N3 B2 F3 -106.2(10) . . . . ? C10 N3 B2 N4 -172.2(7) . . . . ? C13 N3 B2 N4 9.8(13) . . . . ? #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_transBCODbisBCODBODIPY _database_code_depnum_ccdc_archive 'CCDC 864647' #TrackingRef '9286_web_deposit_cif_file_2_HidemitsuUno_1327633261.transBCODbisBCODBODIPY.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C40 H38 B2 Cl6 F4 N4' _chemical_formula_moiety 'C38 H36 B2 F4 N4, 2(C H Cl3)' _chemical_formula_weight 885.10 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' #------------------------------------------------------------------------------ _cell_length_a 13.753(3) _cell_length_b 13.110(3) _cell_length_c 25.759(5) _cell_angle_alpha 90.0000 _cell_angle_beta 119.635(3) _cell_angle_gamma 90.0000 _cell_volume 4036.9(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4087 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.46 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816.00 _exptl_absorpt_coefficient_mu 0.480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.734 _exptl_absorpt_correction_T_max 0.908 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.222 _diffrn_reflns_number 35544 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 #============================================================================== # REFINEMENT DATA _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. ; _reflns_number_total 9252 _reflns_number_gt 7147 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1569 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 9252 _refine_ls_number_parameters 584 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+3.4759P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_diff_density_max 0.510 _refine_diff_density_min -0.710 _refine_ls_extinction_method none _iucr_refine_instructions_details ; TITL transBCODbisBCODBODIPY CELL 0.71070 13.75270 13.10970 25.75884 90.000 119.635 90.000 ZERR 4 0.00260 0.00230 0.00475 0.000 0.003 0.000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H B F N CL UNIT 160 152 8 16 16 24 SHEL 99999.000000 0.769575 L.S. 5 FMAP 2 PLAN -20 WPDB -2 HTAB TEMP -172.9 ACTA BOND $H CONF EXYZ C24 C24A EADP C24 C24A EXYZ C27 C27A EADP C27 C27A EXYZ C32 C32A EADP C32 C32A EXYZ C35 C35A EADP C35 C35A DFIX 1.35 0.02 C25 C26 C28A C29A C33 C34 C36A C37A DFIX 1.54 0.02 C25A C26A C28 C29 C33A C34A C36 C37 C24 C29 C28 C27 C24A C25A = C26A C27A C24 C29 C28 C27 C32A C33A C34A C35A C32 C37 C36 C35 DFIX 1.45 0.02 C24 C25 C26 C27 C24A C29A C28A C27A C32 C33 C34 C35 C32A C37A = C36A C35A ISOR 0.05 0.1 C24 > C29A C32 > C37A DELU 0.01 C24 > C29A C32 > C37A SIMU 0.02 0.04 C24 > C29A C32 > C37A SIZE 0.400 0.300 0.200 WGHT 0.079700 3.475900 FVAR 0.69180 0.55438 0.58118 0.56745 CL1 6 0.389421 -0.014044 0.283913 11.00000 0.05899 0.05371 = 0.05021 0.00092 0.03262 -0.00066 CL2 6 0.208215 0.004047 0.309099 11.00000 0.04137 0.13022 = 0.03918 -0.00189 0.01870 -0.02580 CL3 6 0.420186 0.095488 0.388481 11.00000 0.04965 0.06237 = 0.05358 -0.01500 0.02302 -0.01672 CL4 6 0.674821 0.049550 0.530620 11.00000 0.08004 0.04345 = 0.05167 0.01267 0.04720 0.01414 CL5 6 0.730731 0.057377 0.436414 11.00000 0.07130 0.04721 = 0.04308 0.00657 0.03807 0.02055 CL6 6 0.840086 0.193220 0.538285 11.00000 0.04244 0.08096 = 0.05352 -0.01179 0.02145 0.00104 F1 4 0.673466 0.385462 0.343499 11.00000 0.02586 0.05070 = 0.04720 -0.01271 0.02176 -0.01158 F2 4 0.622946 0.290707 0.399362 11.00000 0.04532 0.02878 = 0.03193 0.00609 0.00717 0.00270 F3 4 -0.181537 0.069414 0.119884 11.00000 0.01895 0.03400 = 0.06032 -0.00569 0.00711 0.00319 F4 4 -0.082863 0.030977 0.218145 11.00000 0.05219 0.04658 = 0.04831 -0.01752 0.03817 -0.01538 N1 5 0.479307 0.340806 0.300926 11.00000 0.02024 0.02414 = 0.02609 0.00004 0.01156 -0.00057 N2 5 0.569009 0.467181 0.384219 11.00000 0.02157 0.02877 = 0.02479 -0.00042 0.00996 -0.00286 N3 5 0.014988 0.109876 0.171635 11.00000 0.01969 0.02399 = 0.02851 -0.00272 0.01230 0.00243 N4 5 -0.052119 -0.070702 0.150104 11.00000 0.02153 0.02681 = 0.02619 -0.00011 0.01244 0.00003 C1 1 0.461411 0.259776 0.263673 11.00000 0.02254 0.02481 = 0.03050 0.00012 0.01644 -0.00101 C2 1 0.346499 0.256387 0.221173 11.00000 0.02316 0.02203 = 0.02736 -0.00007 0.01416 -0.00052 C3 1 0.295020 0.337853 0.232705 11.00000 0.02261 0.02283 = 0.02397 0.00435 0.01250 0.00172 C4 1 0.377408 0.391218 0.281906 11.00000 0.02113 0.02316 = 0.02389 0.00157 0.01086 -0.00031 C5 1 0.371848 0.478079 0.311345 11.00000 0.02401 0.02209 = 0.02606 0.00247 0.01281 -0.00085 AFIX 43 H5 2 0.302241 0.512290 0.296654 11.00000 -1.20000 AFIX 0 C6 1 0.464303 0.515909 0.361157 11.00000 0.02447 0.02366 = 0.02762 0.00028 0.01353 -0.00116 C7 1 0.477670 0.598562 0.398920 11.00000 0.02959 0.02633 = 0.03270 -0.00239 0.01466 -0.00427 C8 1 0.587564 0.599290 0.444305 11.00000 0.03104 0.03457 = 0.03241 -0.00741 0.01094 -0.00722 C9 1 0.642859 0.517405 0.434562 11.00000 0.02496 0.03669 = 0.02765 -0.00109 0.01046 -0.00592 C10 1 0.024337 0.211535 0.184624 11.00000 0.02060 0.02600 = 0.02503 -0.00192 0.00889 0.00189 C11 1 0.119627 0.248895 0.184047 11.00000 0.02173 0.02463 = 0.02422 -0.00160 0.00997 0.00134 C12 1 0.169870 0.168201 0.171246 11.00000 0.01943 0.02598 = 0.02285 -0.00054 0.00892 -0.00003 C13 1 0.103858 0.081468 0.162595 11.00000 0.01943 0.02549 = 0.02523 0.00036 0.01101 0.00130 C14 1 0.113479 -0.017948 0.147273 11.00000 0.02074 0.02676 = 0.02536 -0.00285 0.01117 0.00090 AFIX 43 H14 2 0.174703 -0.035088 0.141599 11.00000 -1.20000 AFIX 0 C15 1 0.037492 -0.092564 0.140008 11.00000 0.02009 0.02579 = 0.02511 -0.00162 0.01029 0.00108 C16 1 0.028227 -0.196192 0.123432 11.00000 0.02557 0.02674 = 0.02853 -0.00273 0.01356 -0.00036 C17 1 -0.065611 -0.235201 0.122851 11.00000 0.02864 0.02641 = 0.03211 -0.00139 0.01646 -0.00149 C18 1 -0.113640 -0.156784 0.140270 11.00000 0.02601 0.02741 = 0.02480 -0.00077 0.01270 -0.00193 C19 1 0.271269 0.195610 0.166099 11.00000 0.02358 0.02747 = 0.02566 -0.00420 0.01325 -0.00133 AFIX 13 H19 2 0.308832 0.135485 0.159678 11.00000 -1.20000 AFIX 0 C20 1 0.225187 0.274830 0.113757 11.00000 0.03456 0.03619 = 0.02683 0.00012 0.01732 -0.00089 AFIX 23 H20A 2 0.287426 0.300322 0.108402 11.00000 -1.20000 H20B 2 0.170136 0.241148 0.076188 11.00000 -1.20000 AFIX 0 C21 1 0.168441 0.366034 0.127121 11.00000 0.03312 0.02992 = 0.02842 0.00423 0.01369 0.00238 AFIX 23 H21A 2 0.089527 0.371540 0.094966 11.00000 -1.20000 H21B 2 0.207078 0.430167 0.127818 11.00000 -1.20000 AFIX 0 C22 1 0.172857 0.351422 0.188837 11.00000 0.02295 0.02343 = 0.02544 0.00058 0.00987 0.00206 AFIX 13 H22 2 0.137041 0.408232 0.199254 11.00000 -1.20000 AFIX 0 C23 1 0.552742 0.191900 0.269656 11.00000 0.02359 0.03305 = 0.03983 -0.00350 0.01777 0.00200 AFIX 137 H23A 2 0.607275 0.231825 0.264200 11.00000 -1.50000 H23B 2 0.521485 0.138219 0.239254 11.00000 -1.50000 H23C 2 0.589786 0.160827 0.309466 11.00000 -1.50000 AFIX 0 PART 1 C24 1 0.405935 0.678485 0.404407 21.00000 0.03451 0.02747 = 0.03834 -0.00677 0.01810 -0.00449 AFIX 13 H24 2 0.327232 0.680405 0.370506 21.00000 -1.20000 AFIX 0 C25 1 0.468629 0.777197 0.415424 21.00000 0.05140 0.02957 = 0.04943 -0.00503 0.03483 -0.00414 AFIX 43 H25 2 0.434328 0.836078 0.391920 21.00000 -1.20000 AFIX 0 C26 1 0.574320 0.778561 0.459549 21.00000 0.04725 0.03545 = 0.05469 -0.01694 0.03252 -0.01837 AFIX 43 H26 2 0.620526 0.837409 0.469912 21.00000 -1.20000 AFIX 0 C27 1 0.613010 0.679895 0.490898 21.00000 0.03672 0.04497 = 0.03884 -0.01461 0.01426 -0.01097 AFIX 13 H27 2 0.694178 0.681431 0.521691 21.00000 -1.20000 AFIX 0 C28 1 0.537187 0.652552 0.518742 21.00000 0.04459 0.04601 = 0.02954 -0.00697 0.01848 -0.02062 AFIX 23 H28A 2 0.557489 0.584750 0.538159 21.00000 -1.20000 H28B 2 0.546135 0.703994 0.548933 21.00000 -1.20000 AFIX 0 C29 1 0.417402 0.652000 0.467088 21.00000 0.03452 0.04278 = 0.03736 -0.00439 0.02399 -0.01152 AFIX 23 H29A 2 0.373164 0.701915 0.475665 21.00000 -1.20000 H29B 2 0.384750 0.583670 0.464647 21.00000 -1.20000 AFIX 0 PART 2 C24A 1 0.405935 0.678485 0.404407 -21.00000 0.03451 0.02747 = 0.03834 -0.00677 0.01810 -0.00449 AFIX 13 H24A 2 0.326801 0.674450 0.371093 -21.00000 -1.20000 AFIX 0 C25A 1 0.461404 0.783405 0.404866 -21.00000 0.05003 0.02127 = 0.04358 -0.00285 0.03312 -0.00651 AFIX 23 H25A 2 0.462716 0.792348 0.367054 -21.00000 -1.20000 H25B 2 0.417672 0.840051 0.408622 -21.00000 -1.20000 AFIX 0 C26A 1 0.580218 0.784604 0.457515 -21.00000 0.04243 0.02919 = 0.05165 -0.01066 0.03489 -0.01490 AFIX 23 H26A 2 0.586749 0.838872 0.485793 -21.00000 -1.20000 H26B 2 0.632973 0.800748 0.442977 -21.00000 -1.20000 AFIX 0 C27A 1 0.613010 0.679895 0.490898 -21.00000 0.03672 0.04497 = 0.03884 -0.01461 0.01426 -0.01097 AFIX 13 H27A 2 0.691193 0.677384 0.525290 -21.00000 -1.20000 AFIX 0 C28A 1 0.521488 0.668710 0.509006 -21.00000 0.05582 0.03945 = 0.02343 -0.00090 0.02151 -0.01178 AFIX 43 H28 2 0.540461 0.662881 0.549706 -21.00000 -1.20000 AFIX 0 C29A 1 0.413742 0.667565 0.464730 -21.00000 0.03333 0.03247 = 0.04344 -0.00747 0.02131 -0.00840 AFIX 43 H29 2 0.351228 0.660794 0.470737 -21.00000 -1.20000 AFIX 0 PART 0 C30 1 0.762091 0.487119 0.471709 11.00000 0.02582 0.04627 = 0.03569 -0.00429 0.01035 -0.00586 AFIX 127 H30A 2 0.768930 0.413103 0.469231 41.00000 -1.50000 H30B 2 0.788929 0.506630 0.513344 41.00000 -1.50000 H30C 2 0.807008 0.521662 0.457036 41.00000 -1.50000 H30D 2 0.807648 0.547827 0.490510 -41.00000 -1.50000 H30E 2 0.787649 0.454300 0.446397 -41.00000 -1.50000 H30F 2 0.769570 0.439267 0.502705 -41.00000 -1.50000 AFIX 0 C31 1 -0.055102 0.267084 0.197916 11.00000 0.02586 0.02870 = 0.03558 -0.00437 0.01470 0.00437 AFIX 137 H31A 2 -0.130578 0.263293 0.163262 11.00000 -1.50000 H31B 2 -0.032218 0.338666 0.206689 11.00000 -1.50000 H31C 2 -0.054865 0.235904 0.232556 11.00000 -1.50000 AFIX 0 PART 1 C32 1 0.091345 -0.272382 0.108130 31.00000 0.02984 0.02647 = 0.03912 -0.00498 0.01901 -0.00200 AFIX 13 H32 2 0.158382 -0.243425 0.107880 31.00000 -1.20000 AFIX 0 C33 1 0.003922 -0.315426 0.048322 31.00000 0.03997 0.03921 = 0.03121 -0.00757 0.02239 0.00440 AFIX 43 H33 2 0.014475 -0.316508 0.014558 31.00000 -1.20000 AFIX 0 C34 1 -0.088992 -0.351765 0.046181 31.00000 0.03595 0.04005 = 0.03710 -0.01386 0.01265 -0.00500 AFIX 43 H34 2 -0.149525 -0.379550 0.010936 31.00000 -1.20000 AFIX 0 C35 1 -0.089243 -0.344733 0.104887 31.00000 0.04202 0.02823 = 0.04968 -0.00435 0.03090 -0.00677 AFIX 13 H35 2 -0.160928 -0.369057 0.101685 31.00000 -1.20000 AFIX 0 C36 1 0.014118 -0.408846 0.150033 31.00000 0.05404 0.01751 = 0.04246 0.01119 0.02786 0.00480 AFIX 23 H36A 2 0.020986 -0.406412 0.190127 31.00000 -1.20000 H36B 2 0.004605 -0.480921 0.136935 31.00000 -1.20000 AFIX 0 C37 1 0.118912 -0.364578 0.152651 31.00000 0.03240 0.02505 = 0.03441 0.00081 0.01310 0.00832 AFIX 23 H37A 2 0.157240 -0.418698 0.142718 31.00000 -1.20000 H37B 2 0.170656 -0.341144 0.193849 31.00000 -1.20000 AFIX 0 PART 2 C32A 1 0.091345 -0.272382 0.108130 -31.00000 0.02984 0.02647 = 0.03912 -0.00498 0.01901 -0.00200 AFIX 13 H32A 2 0.160996 -0.243510 0.110819 -31.00000 -1.20000 AFIX 0 C33A 1 0.007352 -0.314920 0.044219 -31.00000 0.03260 0.03459 = 0.03379 -0.00578 0.01986 -0.01089 AFIX 23 H33A 2 -0.013833 -0.259613 0.014373 -31.00000 -1.20000 H33B 2 0.044043 -0.369637 0.033614 -31.00000 -1.20000 AFIX 0 C34A 1 -0.097060 -0.356946 0.042823 -31.00000 0.02874 0.03451 = 0.03773 -0.01161 0.01731 -0.01285 AFIX 23 H34A 2 -0.105679 -0.430021 0.031716 -31.00000 -1.20000 H34B 2 -0.163727 -0.320131 0.012226 -31.00000 -1.20000 AFIX 0 C35A 1 -0.089243 -0.344733 0.104887 -31.00000 0.04202 0.02823 = 0.04968 -0.00435 0.03090 -0.00677 AFIX 13 H35A 2 -0.155121 -0.372928 0.106641 -31.00000 -1.20000 AFIX 0 C36A 1 0.019443 -0.394583 0.147435 -31.00000 0.06484 0.02190 = 0.04516 0.00785 0.03128 -0.00111 AFIX 43 H36 2 0.021710 -0.451815 0.170631 -31.00000 -1.20000 AFIX 0 C37A 1 0.114182 -0.355650 0.151814 -31.00000 0.03504 0.03677 = 0.04031 -0.00098 0.01306 0.00937 AFIX 43 H37 2 0.187140 -0.378892 0.179674 -31.00000 -1.20000 AFIX 0 PART 0 C38 1 -0.209951 -0.163045 0.150476 11.00000 0.03010 0.03707 = 0.03532 -0.00362 0.01974 -0.00673 AFIX 137 H38A 2 -0.183252 -0.161936 0.193491 11.00000 -1.50000 H38B 2 -0.250911 -0.226583 0.133303 11.00000 -1.50000 H38C 2 -0.259694 -0.104777 0.131415 11.00000 -1.50000 AFIX 0 C39 1 0.326425 0.063650 0.314142 11.00000 0.04234 0.05124 = 0.03900 0.01209 0.02224 0.00289 AFIX 13 H39 2 0.301822 0.128160 0.290360 11.00000 -1.20000 AFIX 0 C40 1 0.714999 0.128331 0.489613 11.00000 0.04563 0.03524 = 0.03512 0.00649 0.02545 0.01212 AFIX 13 H40 2 0.654858 0.180175 0.468077 11.00000 -1.20000 AFIX 0 B1 3 0.589714 0.369281 0.357789 11.00000 0.02126 0.03028 = 0.02677 0.00246 0.01095 -0.00099 B2 3 -0.078554 0.036165 0.165334 11.00000 0.02149 0.02955 = 0.03341 -0.00705 0.01292 -0.00116 HKLF 4 REM transBCODbisBCODBODIPY REM R1 = 0.0600 for 7147 Fo > 4sig(Fo) and 0.0784 for all 9252 data REM 584 parameters refined using 578 restraints END WGHT 0.0797 3.4763 REM Highest difference peak 0.506, deepest hole -0.706, 1-sigma level 0.074 Q1 1 0.4650 -0.0517 0.3147 11.00000 0.05 0.51 Q2 1 0.4117 0.1370 0.3562 11.00000 0.05 0.42 Q3 1 0.8027 0.1302 0.5422 11.00000 0.05 0.39 Q4 1 -0.1661 0.0708 0.1558 11.00000 0.05 0.37 Q5 1 0.2407 -0.0438 0.2979 11.00000 0.05 0.37 Q6 1 0.4193 0.3686 0.2935 11.00000 0.05 0.35 Q7 1 0.3749 0.4171 0.2993 11.00000 0.05 0.34 Q8 1 0.2233 0.0586 0.3054 11.00000 0.05 0.33 Q9 1 0.1890 0.3184 0.1223 11.00000 0.05 0.33 Q10 1 -0.0240 0.2350 0.1912 11.00000 0.05 0.32 Q11 1 0.0833 0.2306 0.1884 11.00000 0.05 0.32 Q12 1 0.5936 0.0391 0.4855 11.00000 0.05 0.31 Q13 1 0.0207 0.1656 0.1817 11.00000 0.05 0.31 Q14 1 0.1380 0.1223 0.1644 11.00000 0.05 0.31 Q15 1 0.2761 -0.1012 0.2981 11.00000 0.05 0.30 Q16 1 0.0303 -0.1462 0.1237 11.00000 0.05 0.30 Q17 1 0.1364 0.3021 0.1821 11.00000 0.05 0.30 Q18 1 -0.0904 -0.1051 0.1411 11.00000 0.05 0.29 Q19 1 0.4286 0.4932 0.3448 11.00000 0.05 0.28 Q20 1 0.2804 -0.1412 0.2840 11.00000 0.05 0.27 ; 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.0013 0.0007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl1 Cl 0.38942(8) -0.01404(7) 0.28391(4) 0.0519(2) Uani 1 1 d . . . Cl2 Cl 0.20822(8) 0.00405(10) 0.30910(4) 0.0708(3) Uani 1 1 d . . . Cl3 Cl 0.42019(8) 0.09549(7) 0.38848(4) 0.0563(2) Uani 1 1 d . . . Cl4 Cl 0.67482(8) 0.04955(6) 0.53062(4) 0.0520(2) Uani 1 1 d . . . Cl5 Cl 0.73073(8) 0.05738(6) 0.43641(4) 0.0496(2) Uani 1 1 d . . . Cl6 Cl 0.84009(8) 0.19322(8) 0.53828(4) 0.0600(3) Uani 1 1 d . . . F1 F 0.67347(13) 0.38546(13) 0.34350(8) 0.0396(4) Uani 1 1 d . A . F2 F 0.62295(15) 0.29071(12) 0.39936(7) 0.0405(4) Uani 1 1 d . A . F3 F -0.18154(13) 0.06941(12) 0.11988(8) 0.0432(4) Uani 1 1 d . B . F4 F -0.08286(15) 0.03098(13) 0.21814(8) 0.0432(4) Uani 1 1 d . B . N1 N 0.47931(16) 0.34081(15) 0.30093(9) 0.0234(4) Uani 1 1 d . A . N2 N 0.56901(17) 0.46718(16) 0.38422(9) 0.0257(4) Uani 1 1 d . A . N3 N 0.01499(16) 0.10988(15) 0.17164(9) 0.0239(4) Uani 1 1 d . B . N4 N -0.05212(17) -0.07070(15) 0.15010(9) 0.0246(4) Uani 1 1 d . B . C1 C 0.4614(2) 0.25978(18) 0.26367(11) 0.0245(5) Uani 1 1 d . . . C2 C 0.3465(2) 0.25639(18) 0.22117(11) 0.0235(5) Uani 1 1 d . . . C3 C 0.2950(2) 0.33785(18) 0.23270(10) 0.0227(5) Uani 1 1 d . . . C4 C 0.3774(2) 0.39122(18) 0.28191(10) 0.0228(5) Uani 1 1 d . . . C5 C 0.3718(2) 0.47808(18) 0.31134(11) 0.0239(5) Uani 1 1 d . . . H5 H 0.3022 0.5123 0.2967 0.029 Uiso 1 1 calc R . . C6 C 0.4643(2) 0.51591(18) 0.36116(11) 0.0250(5) Uani 1 1 d . A . C7 C 0.4777(2) 0.59856(19) 0.39892(12) 0.0299(5) Uani 1 1 d . . . C8 C 0.5876(2) 0.5993(2) 0.44431(13) 0.0347(6) Uani 1 1 d . A . C9 C 0.6429(2) 0.5174(2) 0.43456(12) 0.0309(5) Uani 1 1 d . . . C10 C 0.0243(2) 0.21154(18) 0.18462(11) 0.0249(5) Uani 1 1 d . . . C11 C 0.1196(2) 0.24889(18) 0.18405(11) 0.0241(5) Uani 1 1 d . . . C12 C 0.16987(19) 0.16820(18) 0.17125(10) 0.0234(5) Uani 1 1 d . . . C13 C 0.10386(19) 0.08147(18) 0.16260(11) 0.0234(5) Uani 1 1 d . . . C14 C 0.1135(2) -0.01795(18) 0.14727(11) 0.0244(5) Uani 1 1 d . . . H14 H 0.1747 -0.0351 0.1416 0.029 Uiso 1 1 calc R . . C15 C 0.0375(2) -0.09256(18) 0.14001(11) 0.0241(5) Uani 1 1 d . B . C16 C 0.0282(2) -0.19619(19) 0.12343(11) 0.0269(5) Uani 1 1 d . . . C17 C -0.0656(2) -0.23520(19) 0.12285(12) 0.0284(5) Uani 1 1 d . B . C18 C -0.1136(2) -0.15678(19) 0.14027(11) 0.0260(5) Uani 1 1 d . . . C19 C 0.2713(2) 0.19561(19) 0.16610(11) 0.0251(5) Uani 1 1 d . . . H19 H 0.3088 0.1355 0.1597 0.030 Uiso 1 1 calc R . . C20 C 0.2252(2) 0.2748(2) 0.11376(12) 0.0316(6) Uani 1 1 d . . . H20A H 0.2874 0.3003 0.1084 0.038 Uiso 1 1 calc R . . H20B H 0.1701 0.2411 0.0762 0.038 Uiso 1 1 calc R . . C21 C 0.1684(2) 0.3660(2) 0.12712(12) 0.0312(5) Uani 1 1 d . . . H21A H 0.0895 0.3715 0.0950 0.037 Uiso 1 1 calc R . . H21B H 0.2071 0.4302 0.1278 0.037 Uiso 1 1 calc R . . C22 C 0.1729(2) 0.35142(18) 0.18884(11) 0.0249(5) Uani 1 1 d . . . H22 H 0.1370 0.4082 0.1993 0.030 Uiso 1 1 calc R . . C23 C 0.5527(2) 0.1919(2) 0.26966(13) 0.0312(6) Uani 1 1 d . . . H23A H 0.6073 0.2318 0.2642 0.047 Uiso 1 1 calc R . . H23B H 0.5215 0.1382 0.2393 0.047 Uiso 1 1 calc R . . H23C H 0.5898 0.1608 0.3095 0.047 Uiso 1 1 calc R . . C24 C 0.4059(2) 0.6785(2) 0.40441(13) 0.0334(6) Uani 0.554(19) 1 d PDU A 1 H24 H 0.3272 0.6804 0.3705 0.040 Uiso 0.554(19) 1 calc PR A 1 C25 C 0.4686(14) 0.7772(12) 0.4154(7) 0.039(2) Uani 0.554(19) 1 d PDU A 1 H25 H 0.4343 0.8361 0.3919 0.047 Uiso 0.554(19) 1 calc PR A 1 C26 C 0.5743(15) 0.7786(13) 0.4595(9) 0.043(3) Uani 0.554(19) 1 d PDU A 1 H26 H 0.6205 0.8374 0.4699 0.051 Uiso 0.554(19) 1 calc PR A 1 C27 C 0.6130(3) 0.6799(2) 0.49090(14) 0.0421(7) Uani 0.554(19) 1 d PDU A 1 H27 H 0.6942 0.6814 0.5217 0.051 Uiso 0.554(19) 1 calc PR A 1 C28 C 0.5372(9) 0.6526(13) 0.5187(6) 0.040(2) Uani 0.554(19) 1 d PDU A 1 H28A H 0.5575 0.5847 0.5382 0.048 Uiso 0.554(19) 1 calc PR A 1 H28B H 0.5461 0.7040 0.5489 0.048 Uiso 0.554(19) 1 calc PR A 1 C29 C 0.4174(14) 0.6520(16) 0.4671(5) 0.036(3) Uani 0.554(19) 1 d PDU A 1 H29A H 0.3732 0.7019 0.4757 0.043 Uiso 0.554(19) 1 calc PR A 1 H29B H 0.3847 0.5837 0.4646 0.043 Uiso 0.554(19) 1 calc PR A 1 C24A C 0.4059(2) 0.6785(2) 0.40441(13) 0.0334(6) Uani 0.446(19) 1 d PDU A 2 H24A H 0.3268 0.6745 0.3711 0.040 Uiso 0.446(19) 1 calc PR A 2 C25A C 0.4614(16) 0.7834(13) 0.4049(9) 0.034(3) Uani 0.446(19) 1 d PDU A 2 H25A H 0.4627 0.7923 0.3671 0.041 Uiso 0.446(19) 1 calc PR A 2 H25B H 0.4177 0.8401 0.4086 0.041 Uiso 0.446(19) 1 calc PR A 2 C26A C 0.5802(18) 0.7846(15) 0.4575(11) 0.036(3) Uani 0.446(19) 1 d PDU A 2 H26A H 0.5867 0.8389 0.4858 0.043 Uiso 0.446(19) 1 calc PR A 2 H26B H 0.6330 0.8007 0.4430 0.043 Uiso 0.446(19) 1 calc PR A 2 C27A C 0.6130(3) 0.6799(2) 0.49090(14) 0.0421(7) Uani 0.446(19) 1 d PDU A 2 H27A H 0.6912 0.6774 0.5253 0.051 Uiso 0.446(19) 1 calc PR A 2 C28A C 0.5215(12) 0.6687(16) 0.5090(7) 0.039(3) Uani 0.446(19) 1 d PDU A 2 H28 H 0.5405 0.6629 0.5497 0.046 Uiso 0.446(19) 1 calc PR A 2 C29A C 0.4137(18) 0.6676(19) 0.4647(6) 0.035(3) Uani 0.446(19) 1 d PDU A 2 H29 H 0.3512 0.6608 0.4707 0.042 Uiso 0.446(19) 1 calc PR A 2 C30 C 0.7621(2) 0.4871(2) 0.47171(13) 0.0380(6) Uani 1 1 d . A . H30A H 0.7689 0.4131 0.4692 0.057 Uiso 0.57(4) 1 calc PR . . H30B H 0.7889 0.5066 0.5133 0.057 Uiso 0.57(4) 1 calc PR . . H30C H 0.8070 0.5217 0.4570 0.057 Uiso 0.57(4) 1 calc PR . . H30D H 0.8076 0.5478 0.4905 0.057 Uiso 0.43(4) 1 calc PR . . H30E H 0.7876 0.4543 0.4464 0.057 Uiso 0.43(4) 1 calc PR . . H30F H 0.7696 0.4393 0.5027 0.057 Uiso 0.43(4) 1 calc PR . . C31 C -0.0551(2) 0.2671(2) 0.19792(12) 0.0303(5) Uani 1 1 d . . . H31A H -0.1306 0.2633 0.1633 0.045 Uiso 1 1 calc R . . H31B H -0.0322 0.3387 0.2067 0.045 Uiso 1 1 calc R . . H31C H -0.0549 0.2359 0.2326 0.045 Uiso 1 1 calc R . . C32 C 0.0913(2) -0.2724(2) 0.10813(12) 0.0310(5) Uani 0.58(2) 1 d PDU B 1 H32 H 0.1584 -0.2434 0.1079 0.037 Uiso 0.58(2) 1 calc PR B 1 C33 C 0.0039(13) -0.3154(14) 0.0483(6) 0.035(2) Uani 0.58(2) 1 d PDU B 1 H33 H 0.0145 -0.3165 0.0146 0.042 Uiso 0.58(2) 1 calc PR B 1 C34 C -0.0890(16) -0.3518(17) 0.0462(6) 0.040(3) Uani 0.58(2) 1 d PDU B 1 H34 H -0.1495 -0.3795 0.0109 0.048 Uiso 0.58(2) 1 calc PR B 1 C35 C -0.0892(3) -0.3447(2) 0.10489(14) 0.0364(6) Uani 0.58(2) 1 d PDU B 1 H35 H -0.1609 -0.3691 0.1017 0.044 Uiso 0.58(2) 1 calc PR B 1 C36 C 0.0141(10) -0.4088(12) 0.1500(8) 0.036(2) Uani 0.58(2) 1 d PDU B 1 H36A H 0.0210 -0.4064 0.1901 0.044 Uiso 0.58(2) 1 calc PR B 1 H36B H 0.0046 -0.4809 0.1369 0.044 Uiso 0.58(2) 1 calc PR B 1 C37 C 0.1189(14) -0.3646(13) 0.1527(8) 0.032(2) Uani 0.58(2) 1 d PDU B 1 H37A H 0.1572 -0.4187 0.1427 0.039 Uiso 0.58(2) 1 calc PR B 1 H37B H 0.1707 -0.3411 0.1938 0.039 Uiso 0.58(2) 1 calc PR B 1 C32A C 0.0913(2) -0.2724(2) 0.10813(12) 0.0310(5) Uani 0.42(2) 1 d PDU B 2 H32A H 0.1610 -0.2435 0.1108 0.037 Uiso 0.42(2) 1 calc PR B 2 C33A C 0.0074(17) -0.315(2) 0.0442(8) 0.032(3) Uani 0.42(2) 1 d PDU B 2 H33A H -0.0138 -0.2596 0.0144 0.039 Uiso 0.42(2) 1 calc PR B 2 H33B H 0.0440 -0.3696 0.0336 0.039 Uiso 0.42(2) 1 calc PR B 2 C34A C -0.097(2) -0.357(2) 0.0428(8) 0.033(3) Uani 0.42(2) 1 d PDU B 2 H34A H -0.1057 -0.4300 0.0317 0.040 Uiso 0.42(2) 1 calc PR B 2 H34B H -0.1637 -0.3201 0.0122 0.040 Uiso 0.42(2) 1 calc PR B 2 C35A C -0.0892(3) -0.3447(2) 0.10489(14) 0.0364(6) Uani 0.42(2) 1 d PDU B 2 H35A H -0.1551 -0.3729 0.1066 0.044 Uiso 0.42(2) 1 calc PR B 2 C36A C 0.0194(15) -0.3946(17) 0.1474(11) 0.042(3) Uani 0.42(2) 1 d PDU B 2 H36 H 0.0217 -0.4518 0.1706 0.051 Uiso 0.42(2) 1 calc PR B 2 C37A C 0.114(2) -0.3556(19) 0.1518(12) 0.040(4) Uani 0.42(2) 1 d PDU B 2 H37 H 0.1871 -0.3789 0.1797 0.048 Uiso 0.42(2) 1 calc PR B 2 C38 C -0.2100(2) -0.1630(2) 0.15048(13) 0.0326(6) Uani 1 1 d . B . H38A H -0.1833 -0.1619 0.1935 0.049 Uiso 1 1 calc R . . H38B H -0.2509 -0.2266 0.1333 0.049 Uiso 1 1 calc R . . H38C H -0.2597 -0.1048 0.1314 0.049 Uiso 1 1 calc R . . C39 C 0.3264(3) 0.0636(3) 0.31414(14) 0.0433(7) Uani 1 1 d . . . H39 H 0.3018 0.1282 0.2904 0.052 Uiso 1 1 calc R . . C40 C 0.7150(3) 0.1283(2) 0.48961(13) 0.0363(6) Uani 1 1 d . . . H40 H 0.6549 0.1802 0.4681 0.044 Uiso 1 1 calc R . . B1 B 0.5897(2) 0.3693(2) 0.35779(13) 0.0265(6) Uani 1 1 d . . . B2 B -0.0786(2) 0.0362(2) 0.16533(14) 0.0284(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0590(5) 0.0537(5) 0.0502(5) 0.0009(4) 0.0326(4) -0.0007(4) Cl2 0.0414(5) 0.1302(10) 0.0392(4) -0.0019(5) 0.0187(4) -0.0258(5) Cl3 0.0497(5) 0.0624(5) 0.0536(5) -0.0150(4) 0.0230(4) -0.0167(4) Cl4 0.0800(6) 0.0435(4) 0.0517(5) 0.0127(3) 0.0472(5) 0.0141(4) Cl5 0.0713(6) 0.0472(4) 0.0431(4) 0.0066(3) 0.0381(4) 0.0205(4) Cl6 0.0424(5) 0.0810(6) 0.0535(5) -0.0118(4) 0.0214(4) 0.0010(4) F1 0.0259(8) 0.0507(10) 0.0472(10) -0.0127(8) 0.0218(7) -0.0116(7) F2 0.0453(10) 0.0288(8) 0.0319(8) 0.0061(6) 0.0072(7) 0.0027(7) F3 0.0190(7) 0.0340(9) 0.0603(11) -0.0057(8) 0.0071(7) 0.0032(6) F4 0.0522(11) 0.0466(10) 0.0483(10) -0.0175(8) 0.0382(9) -0.0154(8) N1 0.0202(10) 0.0241(10) 0.0261(10) 0.0000(8) 0.0116(8) -0.0006(8) N2 0.0216(10) 0.0288(11) 0.0248(10) -0.0004(8) 0.0100(8) -0.0029(8) N3 0.0197(10) 0.0240(10) 0.0285(10) -0.0027(8) 0.0123(8) 0.0024(8) N4 0.0215(10) 0.0268(10) 0.0262(10) -0.0001(8) 0.0124(8) 0.0000(8) C1 0.0225(11) 0.0248(12) 0.0305(12) 0.0001(9) 0.0164(10) -0.0010(9) C2 0.0232(11) 0.0220(11) 0.0274(12) -0.0001(9) 0.0142(10) -0.0005(9) C3 0.0226(11) 0.0228(11) 0.0240(11) 0.0043(9) 0.0125(10) 0.0017(9) C4 0.0211(11) 0.0232(11) 0.0239(11) 0.0016(9) 0.0109(9) -0.0003(9) C5 0.0240(11) 0.0221(11) 0.0261(12) 0.0025(9) 0.0128(10) -0.0008(9) C6 0.0245(12) 0.0237(11) 0.0276(12) 0.0003(9) 0.0135(10) -0.0012(9) C7 0.0296(13) 0.0263(12) 0.0327(13) -0.0024(10) 0.0147(11) -0.0043(10) C8 0.0310(14) 0.0346(14) 0.0324(14) -0.0074(11) 0.0109(12) -0.0072(11) C9 0.0250(12) 0.0367(14) 0.0277(12) -0.0011(10) 0.0105(10) -0.0059(11) C10 0.0206(11) 0.0260(12) 0.0250(12) -0.0019(9) 0.0089(9) 0.0019(9) C11 0.0217(11) 0.0246(12) 0.0242(11) -0.0016(9) 0.0100(9) 0.0013(9) C12 0.0194(11) 0.0260(12) 0.0228(11) -0.0005(9) 0.0089(9) 0.0000(9) C13 0.0194(11) 0.0255(12) 0.0252(11) 0.0004(9) 0.0110(9) 0.0013(9) C14 0.0207(11) 0.0268(12) 0.0254(11) -0.0029(9) 0.0112(9) 0.0009(9) C15 0.0201(11) 0.0258(12) 0.0251(11) -0.0016(9) 0.0103(9) 0.0011(9) C16 0.0256(12) 0.0267(12) 0.0285(12) -0.0027(10) 0.0136(10) -0.0004(10) C17 0.0286(13) 0.0264(12) 0.0321(13) -0.0014(10) 0.0165(11) -0.0015(10) C18 0.0260(12) 0.0274(12) 0.0248(12) -0.0008(9) 0.0127(10) -0.0019(10) C19 0.0236(12) 0.0275(12) 0.0257(12) -0.0042(9) 0.0132(10) -0.0013(9) C20 0.0346(14) 0.0362(14) 0.0268(13) 0.0001(10) 0.0173(11) -0.0009(11) C21 0.0331(14) 0.0299(13) 0.0284(13) 0.0042(10) 0.0137(11) 0.0024(11) C22 0.0230(12) 0.0234(11) 0.0254(12) 0.0006(9) 0.0099(10) 0.0021(9) C23 0.0236(12) 0.0330(13) 0.0398(14) -0.0035(11) 0.0178(11) 0.0020(10) C24 0.0345(14) 0.0275(13) 0.0383(14) -0.0068(11) 0.0181(12) -0.0045(10) C25 0.051(4) 0.030(4) 0.049(5) -0.005(3) 0.035(3) -0.004(3) C26 0.047(4) 0.035(4) 0.055(5) -0.017(4) 0.033(4) -0.018(4) C27 0.0367(15) 0.0450(16) 0.0388(15) -0.0146(12) 0.0143(13) -0.0110(13) C28 0.045(4) 0.046(5) 0.030(4) -0.007(3) 0.018(3) -0.021(4) C29 0.035(4) 0.043(6) 0.037(4) -0.004(3) 0.024(3) -0.012(4) C24A 0.0345(14) 0.0275(13) 0.0383(14) -0.0068(11) 0.0181(12) -0.0045(10) C25A 0.050(5) 0.021(4) 0.044(5) -0.003(3) 0.033(4) -0.007(3) C26A 0.042(4) 0.029(5) 0.052(5) -0.011(4) 0.035(4) -0.015(4) C27A 0.0367(15) 0.0450(16) 0.0388(15) -0.0146(12) 0.0143(13) -0.0110(13) C28A 0.056(5) 0.039(5) 0.023(4) -0.001(4) 0.022(4) -0.012(4) C29A 0.033(4) 0.032(6) 0.043(5) -0.007(4) 0.021(4) -0.008(4) C30 0.0258(13) 0.0463(16) 0.0357(15) -0.0043(12) 0.0104(12) -0.0059(12) C31 0.0259(12) 0.0287(13) 0.0356(14) -0.0044(10) 0.0147(11) 0.0044(10) C32 0.0298(13) 0.0265(12) 0.0391(14) -0.0050(10) 0.0190(11) -0.0020(10) C33 0.040(4) 0.039(5) 0.031(3) -0.008(3) 0.022(3) 0.004(3) C34 0.036(4) 0.040(5) 0.037(4) -0.014(4) 0.013(3) -0.005(4) C35 0.0420(15) 0.0282(13) 0.0497(16) -0.0044(11) 0.0309(13) -0.0068(11) C36 0.054(4) 0.018(4) 0.042(3) 0.011(3) 0.028(3) 0.005(3) C37 0.032(3) 0.025(4) 0.034(4) 0.001(3) 0.013(3) 0.008(3) C32A 0.0298(13) 0.0265(12) 0.0391(14) -0.0050(10) 0.0190(11) -0.0020(10) C33A 0.033(5) 0.035(6) 0.034(5) -0.006(4) 0.020(4) -0.011(4) C34A 0.029(5) 0.035(6) 0.038(5) -0.012(5) 0.017(4) -0.013(4) C35A 0.0420(15) 0.0282(13) 0.0497(16) -0.0044(11) 0.0309(13) -0.0068(11) C36A 0.065(5) 0.022(6) 0.045(5) 0.008(4) 0.031(4) -0.001(4) C37A 0.035(5) 0.037(6) 0.040(5) -0.001(5) 0.013(5) 0.009(5) C38 0.0301(13) 0.0371(14) 0.0353(14) -0.0036(11) 0.0197(12) -0.0067(11) C39 0.0423(17) 0.0512(18) 0.0390(16) 0.0121(14) 0.0222(14) 0.0029(14) C40 0.0456(16) 0.0352(14) 0.0351(14) 0.0065(11) 0.0254(13) 0.0121(12) B1 0.0213(13) 0.0303(14) 0.0268(13) 0.0025(11) 0.0109(11) -0.0010(11) B2 0.0215(13) 0.0295(14) 0.0334(15) -0.0071(11) 0.0129(12) -0.0012(11) _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 Cl1 C39 1.750(3) . ? Cl2 C39 1.750(3) . ? Cl3 C39 1.750(3) . ? Cl4 C40 1.751(3) . ? Cl5 C40 1.756(3) . ? Cl6 C40 1.767(3) . ? F1 B1 1.388(3) . ? F2 B1 1.390(3) . ? F3 B2 1.388(3) . ? F4 B2 1.392(3) . ? N1 C1 1.370(3) . ? N1 C4 1.401(3) . ? N1 B1 1.546(3) . ? N2 C9 1.358(3) . ? N2 C6 1.410(3) . ? N2 B1 1.544(4) . ? N3 C10 1.365(3) . ? N3 C13 1.403(3) . ? N3 B2 1.552(3) . ? N4 C18 1.357(3) . ? N4 C15 1.409(3) . ? N4 B2 1.546(3) . ? C1 C2 1.410(3) . ? C1 C23 1.484(3) . ? C2 C3 1.392(3) . ? C2 C19 1.505(3) . ? C3 C4 1.400(3) . ? C3 C22 1.501(3) . ? C4 C5 1.391(3) . ? C5 C6 1.377(3) . ? C5 H5 0.9500 . ? C6 C7 1.406(3) . ? C7 C8 1.380(4) . ? C7 C24 1.493(4) . ? C8 C9 1.408(4) . ? C8 C27 1.505(4) . ? C9 C30 1.487(4) . ? C10 C11 1.406(3) . ? C10 C31 1.487(3) . ? C11 C12 1.389(3) . ? C11 C22 1.506(3) . ? C12 C13 1.402(3) . ? C12 C19 1.508(3) . ? C13 C14 1.387(3) . ? C14 C15 1.375(3) . ? C14 H14 0.9500 . ? C15 C16 1.411(3) . ? C16 C17 1.381(3) . ? C16 C32 1.498(3) . ? C17 C18 1.410(3) . ? C17 C35 1.494(4) . ? C18 C38 1.475(3) . ? C19 C20 1.566(4) . ? C19 H19 1.0000 . ? C20 C21 1.557(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.572(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.502(12) . ? C24 C29 1.581(10) . ? C24 H24 1.0000 . ? C25 C26 1.331(14) . ? C25 H25 0.9500 . ? C26 C27 1.478(13) . ? C26 H26 0.9500 . ? C27 C28 1.572(10) . ? C27 H27 1.0000 . ? C28 C29 1.522(13) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C25A C26A 1.522(16) . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C28A C29A 1.351(16) . ? C28A H28 0.9500 . ? C29A H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C30 H30D 0.9800 . ? C30 H30E 0.9800 . ? C30 H30F 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.518(11) . ? C32 C37 1.578(11) . ? C32 H32 1.0000 . ? C33 C34 1.339(13) . ? C33 H33 0.9500 . ? C34 C35 1.517(12) . ? C34 H34 0.9500 . ? C35 C36 1.564(11) . ? C35 H35 1.0000 . ? C36 C37 1.524(12) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C33A C34A 1.522(15) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C34A H34A 0.9900 . ? C34A H34B 0.9900 . ? C36A C37A 1.351(17) . ? C36A H36 0.9500 . ? C37A H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39 1.0000 . ? C40 H40 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 C1 N1 C4 108.6(2) . . ? C1 N1 B1 127.1(2) . . ? C4 N1 B1 124.2(2) . . ? C9 N2 C6 108.0(2) . . ? C9 N2 B1 127.6(2) . . ? C6 N2 B1 124.3(2) . . ? C10 N3 C13 108.4(2) . . ? C10 N3 B2 127.3(2) . . ? C13 N3 B2 124.2(2) . . ? C18 N4 C15 108.5(2) . . ? C18 N4 B2 126.7(2) . . ? C15 N4 B2 124.6(2) . . ? N1 C1 C2 108.2(2) . . ? N1 C1 C23 122.9(2) . . ? C2 C1 C23 128.9(2) . . ? C3 C2 C1 107.7(2) . . ? C3 C2 C19 115.0(2) . . ? C1 C2 C19 137.1(2) . . ? C2 C3 C4 107.9(2) . . ? C2 C3 C22 115.4(2) . . ? C4 C3 C22 136.5(2) . . ? C5 C4 C3 131.7(2) . . ? C5 C4 N1 120.7(2) . . ? C3 C4 N1 107.6(2) . . ? C6 C5 C4 121.9(2) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 131.8(2) . . ? C5 C6 N2 120.6(2) . . ? C7 C6 N2 107.5(2) . . ? C8 C7 C6 107.8(2) . . ? C8 C7 C24 114.4(2) . . ? C6 C7 C24 137.7(2) . . ? C7 C8 C9 107.8(2) . . ? C7 C8 C27 114.0(3) . . ? C9 C8 C27 138.1(3) . . ? N2 C9 C8 109.0(2) . . ? N2 C9 C30 123.4(2) . . ? C8 C9 C30 127.6(2) . . ? N3 C10 C11 108.2(2) . . ? N3 C10 C31 122.9(2) . . ? C11 C10 C31 128.8(2) . . ? C12 C11 C10 108.2(2) . . ? C12 C11 C22 114.9(2) . . ? C10 C11 C22 136.7(2) . . ? C11 C12 C13 107.2(2) . . ? C11 C12 C19 115.4(2) . . ? C13 C12 C19 137.2(2) . . ? C14 C13 C12 131.4(2) . . ? C14 C13 N3 120.7(2) . . ? C12 C13 N3 107.9(2) . . ? C15 C14 C13 122.3(2) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 N4 120.4(2) . . ? C14 C15 C16 132.5(2) . . ? N4 C15 C16 107.2(2) . . ? C17 C16 C15 107.7(2) . . ? C17 C16 C32 114.2(2) . . ? C15 C16 C32 138.1(2) . . ? C16 C17 C18 108.0(2) . . ? C16 C17 C35 114.7(2) . . ? C18 C17 C35 137.3(2) . . ? N4 C18 C17 108.6(2) . . ? N4 C18 C38 123.0(2) . . ? C17 C18 C38 128.3(2) . . ? C2 C19 C12 106.13(19) . . ? C2 C19 C20 104.9(2) . . ? C12 C19 C20 103.6(2) . . ? C2 C19 H19 113.7 . . ? C12 C19 H19 113.7 . . ? C20 C19 H19 113.7 . . ? C21 C20 C19 110.7(2) . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C20 C21 C22 110.9(2) . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.0 . . ? C3 C22 C11 105.88(19) . . ? C3 C22 C21 104.2(2) . . ? C11 C22 C21 104.6(2) . . ? C3 C22 H22 113.7 . . ? C11 C22 H22 113.7 . . ? C21 C22 H22 113.7 . . ? C1 C23 H23A 109.5 . . ? C1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C7 C24 C25 106.1(8) . . ? C7 C24 C29 101.9(8) . . ? C25 C24 C29 103.8(9) . . ? C7 C24 H24 114.6 . . ? C25 C24 H24 114.6 . . ? C29 C24 H24 114.6 . . ? C26 C25 C24 117.1(13) . . ? C26 C25 H25 121.5 . . ? C24 C25 H25 121.5 . . ? C25 C26 C27 113.6(14) . . ? C25 C26 H26 123.2 . . ? C27 C26 H26 123.2 . . ? C26 C27 C8 107.5(10) . . ? C26 C27 C28 107.9(11) . . ? C8 C27 C28 105.0(7) . . ? C26 C27 H27 112.0 . . ? C8 C27 H27 112.0 . . ? C28 C27 H27 112.0 . . ? C29 C28 C27 106.1(9) . . ? C29 C28 H28A 110.5 . . ? C27 C28 H28A 110.5 . . ? C29 C28 H28B 110.5 . . ? C27 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? C28 C29 C24 114.2(10) . . ? C28 C29 H29A 108.7 . . ? C24 C29 H29A 108.7 . . ? C28 C29 H29B 108.7 . . ? C24 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C26A C25A H25A 110.0 . . ? C26A C25A H25B 110.0 . . ? H25A C25A H25B 108.3 . . ? C25A C26A H26A 109.3 . . ? C25A C26A H26B 109.3 . . ? H26A C26A H26B 107.9 . . ? C29A C28A H28 121.2 . . ? C28A C29A H29 124.5 . . ? C9 C30 H30A 109.5 . . ? C9 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C9 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C9 C30 H30D 109.5 . . ? H30A C30 H30D 141.1 . . ? H30B C30 H30D 56.3 . . ? H30C C30 H30D 56.3 . . ? C9 C30 H30E 109.5 . . ? H30A C30 H30E 56.3 . . ? H30B C30 H30E 141.1 . . ? H30C C30 H30E 56.3 . . ? H30D C30 H30E 109.5 . . ? C9 C30 H30F 109.5 . . ? H30A C30 H30F 56.3 . . ? H30B C30 H30F 56.3 . . ? H30C C30 H30F 141.1 . . ? H30D C30 H30F 109.5 . . ? H30E C30 H30F 109.5 . . ? C10 C31 H31A 109.5 . . ? C10 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C10 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C16 C32 C33 104.1(7) . . ? C16 C32 C37 106.4(8) . . ? C33 C32 C37 103.8(11) . . ? C16 C32 H32 113.9 . . ? C33 C32 H32 113.9 . . ? C37 C32 H32 113.9 . . ? C34 C33 C32 115.8(13) . . ? C34 C33 H33 122.1 . . ? C32 C33 H33 122.1 . . ? C33 C34 C35 114.2(13) . . ? C33 C34 H34 122.9 . . ? C35 C34 H34 122.9 . . ? C17 C35 C34 105.1(8) . . ? C17 C35 C36 107.9(7) . . ? C34 C35 C36 105.0(11) . . ? C17 C35 H35 112.7 . . ? C34 C35 H35 112.7 . . ? C36 C35 H35 112.7 . . ? C37 C36 C35 108.7(10) . . ? C37 C36 H36A 110.0 . . ? C35 C36 H36A 110.0 . . ? C37 C36 H36B 110.0 . . ? C35 C36 H36B 110.0 . . ? H36A C36 H36B 108.3 . . ? C36 C37 C32 112.2(11) . . ? C36 C37 H37A 109.2 . . ? C32 C37 H37A 109.2 . . ? C36 C37 H37B 109.2 . . ? C32 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C34A C33A H33A 109.6 . . ? C34A C33A H33B 109.6 . . ? H33A C33A H33B 108.1 . . ? C33A C34A H34A 109.5 . . ? C33A C34A H34B 109.5 . . ? H34A C34A H34B 108.1 . . ? C37A C36A H36 121.0 . . ? C36A C37A H37 123.8 . . ? C18 C38 H38A 109.5 . . ? C18 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C18 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Cl1 C39 Cl2 110.69(19) . . ? Cl1 C39 Cl3 111.52(18) . . ? Cl2 C39 Cl3 110.04(17) . . ? Cl1 C39 H39 108.2 . . ? Cl2 C39 H39 108.2 . . ? Cl3 C39 H39 108.2 . . ? Cl4 C40 Cl5 110.84(16) . . ? Cl4 C40 Cl6 110.05(16) . . ? Cl5 C40 Cl6 110.88(16) . . ? Cl4 C40 H40 108.3 . . ? Cl5 C40 H40 108.3 . . ? Cl6 C40 H40 108.3 . . ? F1 B1 F2 108.5(2) . . ? F1 B1 N2 110.4(2) . . ? F2 B1 N2 109.8(2) . . ? F1 B1 N1 109.9(2) . . ? F2 B1 N1 110.2(2) . . ? N2 B1 N1 108.0(2) . . ? F3 B2 F4 108.7(2) . . ? F3 B2 N4 109.9(2) . . ? F4 B2 N4 109.4(2) . . ? F3 B2 N3 109.9(2) . . ? F4 B2 N3 111.2(2) . . ? N4 B2 N3 107.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C2 -1.5(3) . . . . ? B1 N1 C1 C2 173.9(2) . . . . ? C4 N1 C1 C23 177.7(2) . . . . ? B1 N1 C1 C23 -7.0(4) . . . . ? N1 C1 C2 C3 0.9(3) . . . . ? C23 C1 C2 C3 -178.2(2) . . . . ? N1 C1 C2 C19 174.3(3) . . . . ? C23 C1 C2 C19 -4.7(5) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C19 C2 C3 C4 -175.1(2) . . . . ? C1 C2 C3 C22 175.6(2) . . . . ? C19 C2 C3 C22 0.6(3) . . . . ? C2 C3 C4 C5 179.4(2) . . . . ? C22 C3 C4 C5 5.1(5) . . . . ? C2 C3 C4 N1 -0.9(3) . . . . ? C22 C3 C4 N1 -175.1(3) . . . . ? C1 N1 C4 C5 -178.8(2) . . . . ? B1 N1 C4 C5 5.7(3) . . . . ? C1 N1 C4 C3 1.5(3) . . . . ? B1 N1 C4 C3 -174.1(2) . . . . ? C3 C4 C5 C6 177.4(2) . . . . ? N1 C4 C5 C6 -2.3(4) . . . . ? C4 C5 C6 C7 -177.2(3) . . . . ? C4 C5 C6 N2 0.0(4) . . . . ? C9 N2 C6 C5 -177.0(2) . . . . ? B1 N2 C6 C5 -1.1(4) . . . . ? C9 N2 C6 C7 0.8(3) . . . . ? B1 N2 C6 C7 176.8(2) . . . . ? C5 C6 C7 C8 176.8(3) . . . . ? N2 C6 C7 C8 -0.7(3) . . . . ? C5 C6 C7 C24 1.0(5) . . . . ? N2 C6 C7 C24 -176.5(3) . . . . ? C6 C7 C8 C9 0.4(3) . . . . ? C24 C7 C8 C9 177.3(2) . . . . ? C6 C7 C8 C27 -176.1(2) . . . . ? C24 C7 C8 C27 0.8(4) . . . . ? C6 N2 C9 C8 -0.6(3) . . . . ? B1 N2 C9 C8 -176.4(2) . . . . ? C6 N2 C9 C30 179.3(2) . . . . ? B1 N2 C9 C30 3.5(4) . . . . ? C7 C8 C9 N2 0.1(3) . . . . ? C27 C8 C9 N2 175.4(3) . . . . ? C7 C8 C9 C30 -179.8(3) . . . . ? C27 C8 C9 C30 -4.6(6) . . . . ? C13 N3 C10 C11 -0.1(3) . . . . ? B2 N3 C10 C11 -178.1(2) . . . . ? C13 N3 C10 C31 -178.9(2) . . . . ? B2 N3 C10 C31 3.1(4) . . . . ? N3 C10 C11 C12 -0.8(3) . . . . ? C31 C10 C11 C12 177.9(2) . . . . ? N3 C10 C11 C22 173.4(3) . . . . ? C31 C10 C11 C22 -7.9(5) . . . . ? C10 C11 C12 C13 1.3(3) . . . . ? C22 C11 C12 C13 -174.3(2) . . . . ? C10 C11 C12 C19 177.4(2) . . . . ? C22 C11 C12 C19 1.8(3) . . . . ? C11 C12 C13 C14 177.9(3) . . . . ? C19 C12 C13 C14 3.2(5) . . . . ? C11 C12 C13 N3 -1.4(3) . . . . ? C19 C12 C13 N3 -176.1(3) . . . . ? C10 N3 C13 C14 -178.5(2) . . . . ? B2 N3 C13 C14 -0.4(4) . . . . ? C10 N3 C13 C12 0.9(3) . . . . ? B2 N3 C13 C12 179.0(2) . . . . ? C12 C13 C14 C15 -179.0(3) . . . . ? N3 C13 C14 C15 0.3(4) . . . . ? C13 C14 C15 N4 -2.2(4) . . . . ? C13 C14 C15 C16 178.2(3) . . . . ? C18 N4 C15 C14 -179.6(2) . . . . ? B2 N4 C15 C14 4.4(4) . . . . ? C18 N4 C15 C16 0.1(3) . . . . ? B2 N4 C15 C16 -175.9(2) . . . . ? C14 C15 C16 C17 -179.6(3) . . . . ? N4 C15 C16 C17 0.7(3) . . . . ? C14 C15 C16 C32 1.9(5) . . . . ? N4 C15 C16 C32 -177.8(3) . . . . ? C15 C16 C17 C18 -1.2(3) . . . . ? C32 C16 C17 C18 177.7(2) . . . . ? C15 C16 C17 C35 178.9(2) . . . . ? C32 C16 C17 C35 -2.2(3) . . . . ? C15 N4 C18 C17 -0.8(3) . . . . ? B2 N4 C18 C17 175.1(2) . . . . ? C15 N4 C18 C38 176.0(2) . . . . ? B2 N4 C18 C38 -8.1(4) . . . . ? C16 C17 C18 N4 1.3(3) . . . . ? C35 C17 C18 N4 -178.9(3) . . . . ? C16 C17 C18 C38 -175.3(3) . . . . ? C35 C17 C18 C38 4.6(5) . . . . ? C3 C2 C19 C12 -51.4(3) . . . . ? C1 C2 C19 C12 135.5(3) . . . . ? C3 C2 C19 C20 57.9(3) . . . . ? C1 C2 C19 C20 -115.2(3) . . . . ? C11 C12 C19 C2 50.2(3) . . . . ? C13 C12 C19 C2 -135.3(3) . . . . ? C11 C12 C19 C20 -60.0(3) . . . . ? C13 C12 C19 C20 114.5(3) . . . . ? C2 C19 C20 C21 -54.9(3) . . . . ? C12 C19 C20 C21 56.2(3) . . . . ? C19 C20 C21 C22 -0.6(3) . . . . ? C2 C3 C22 C11 51.5(3) . . . . ? C4 C3 C22 C11 -134.6(3) . . . . ? C2 C3 C22 C21 -58.5(3) . . . . ? C4 C3 C22 C21 115.4(3) . . . . ? C12 C11 C22 C3 -52.7(3) . . . . ? C10 C11 C22 C3 133.5(3) . . . . ? C12 C11 C22 C21 57.0(3) . . . . ? C10 C11 C22 C21 -116.8(3) . . . . ? C20 C21 C22 C3 55.8(3) . . . . ? C20 C21 C22 C11 -55.1(3) . . . . ? C8 C7 C24 C25 49.6(7) . . . . ? C6 C7 C24 C25 -134.8(7) . . . . ? C8 C7 C24 C29 -58.7(7) . . . . ? C6 C7 C24 C29 116.9(7) . . . . ? C7 C24 C25 C26 -52(2) . . . . ? C29 C24 C25 C26 55(2) . . . . ? C24 C25 C26 C27 0(3) . . . . ? C25 C26 C27 C8 52(2) . . . . ? C25 C26 C27 C28 -61(2) . . . . ? C7 C8 C27 C26 -52.9(9) . . . . ? C9 C8 C27 C26 132.1(9) . . . . ? C7 C8 C27 C28 61.9(6) . . . . ? C9 C8 C27 C28 -113.2(6) . . . . ? C26 C27 C28 C29 56.8(15) . . . . ? C8 C27 C28 C29 -57.6(12) . . . . ? C27 C28 C29 C24 -0.4(17) . . . . ? C7 C24 C29 C28 57.6(14) . . . . ? C25 C24 C29 C28 -52.5(16) . . . . ? C17 C16 C32 C33 54.4(8) . . . . ? C15 C16 C32 C33 -127.2(8) . . . . ? C17 C16 C32 C37 -54.9(8) . . . . ? C15 C16 C32 C37 123.6(8) . . . . ? C16 C32 C33 C34 -53.2(18) . . . . ? C37 C32 C33 C34 57.9(19) . . . . ? C32 C33 C34 C35 -1(3) . . . . ? C16 C17 C35 C34 -52.2(8) . . . . ? C18 C17 C35 C34 128.0(9) . . . . ? C16 C17 C35 C36 59.5(7) . . . . ? C18 C17 C35 C36 -120.3(8) . . . . ? C33 C34 C35 C17 54.0(19) . . . . ? C33 C34 C35 C36 -60(2) . . . . ? C17 C35 C36 C37 -53.6(15) . . . . ? C34 C35 C36 C37 58.0(16) . . . . ? C35 C36 C37 C32 -2(2) . . . . ? C16 C32 C37 C36 55.8(16) . . . . ? C33 C32 C37 C36 -53.6(17) . . . . ? C9 N2 B1 F1 -61.0(3) . . . . ? C6 N2 B1 F1 123.8(2) . . . . ? C9 N2 B1 F2 58.6(3) . . . . ? C6 N2 B1 F2 -116.6(2) . . . . ? C9 N2 B1 N1 178.8(2) . . . . ? C6 N2 B1 N1 3.6(3) . . . . ? C1 N1 B1 F1 58.9(3) . . . . ? C4 N1 B1 F1 -126.4(2) . . . . ? C1 N1 B1 F2 -60.7(3) . . . . ? C4 N1 B1 F2 114.0(3) . . . . ? C1 N1 B1 N2 179.4(2) . . . . ? C4 N1 B1 N2 -5.9(3) . . . . ? C18 N4 B2 F3 -59.6(3) . . . . ? C15 N4 B2 F3 115.7(3) . . . . ? C18 N4 B2 F4 59.7(3) . . . . ? C15 N4 B2 F4 -125.0(2) . . . . ? C18 N4 B2 N3 -179.2(2) . . . . ? C15 N4 B2 N3 -4.0(3) . . . . ? C10 N3 B2 F3 60.1(3) . . . . ? C13 N3 B2 F3 -117.7(2) . . . . ? C10 N3 B2 F4 -60.3(3) . . . . ? C13 N3 B2 F4 121.9(2) . . . . ? C10 N3 B2 N4 179.8(2) . . . . ? C13 N3 B2 N4 2.0(3) . . . . ? data_201000906 _database_code_depnum_ccdc_archive 'CCDC 864648' #TrackingRef '9287_web_deposit_cif_file_3_HidemitsuUno_1327633261.cisbisBODIPY.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C39 H44 B2 F4 N4' _chemical_formula_moiety 'C39 H44 B2 F4 N4' _chemical_formula_weight 666.42 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' #------------------------------------------------------------------------------ _cell_length_a 11.0884(3) _cell_length_b 23.5088(9) _cell_length_c 13.9282(5) _cell_angle_alpha 90.0000 _cell_angle_beta 102.6061(14) _cell_angle_gamma 90.0000 _cell_volume 3543.2(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8277 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 68.22 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.090 _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408.00 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.938 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_source 'VariMax Rotating Anode, 40 kV x 30 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 40679 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_theta_max 68.22 _diffrn_reflns_theta_full 68.22 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _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. Four ethyl groups and the solvent toluene molecule disorder. Atomic coordinates of the disordered groups and molecules are restrained. The disordered toluene atoms with the least population is refined isotropically and other non-hydrogen atoms are refined anisotropically. ; _reflns_number_total 6472 _reflns_number_gt 4116 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.2203 _refine_ls_wR_factor_gt 0.1978 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_number_restraints 527 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6470 _refine_ls_number_parameters 613 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0907P)^2^+1.9357P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_diff_density_max 0.285 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _iucr_refine_instructions_details ; TITL 201000906 CELL 1.54187 11.08836 23.50885 13.92816 90.000 102.606 90.000 ZERR 4 0.00030 0.00082 0.00044 0.000 0.001 0.000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H B F N UNIT 156 176 8 16 16 MERG 2 SHEL 99999.000000 0.000000 DFIX 1.50 0.02 C33 C39 DFIX 1.39 0.02 C33 C34 DFIX 1.39 0.02 C34 C35 DFIX 1.39 0.02 C35 C36 DFIX 1.39 0.02 C36 C37 DFIX 1.39 0.02 C37 C38 DFIX 1.39 0.02 C38 C33 DANG 2.50 0.04 C39 C34 DANG 2.50 0.04 C39 C38 DANG 2.41 0.04 C33 C35 DANG 2.41 0.04 C34 C36 DANG 2.41 0.04 C35 C37 DANG 2.41 0.04 C36 C38 DANG 2.41 0.04 C37 C33 DANG 2.41 0.04 C38 C34 FLAT 0.10 C33 C34 C35 C36 C37 C38 C39 SIMU 0.04 0.08 C33 C34 C35 C36 C37 C38 C39 ISOR 0.1 0.2 C33 C34 C35 C36 C37 C38 C39 DELU 0.01 C33 C34 C35 C36 C37 C38 C39 DFIX 1.50 0.02 C33a C39a DFIX 1.39 0.02 C33a C34a DFIX 1.39 0.02 C34a C35a DFIX 1.39 0.02 C35a C36a DFIX 1.39 0.02 C36a C37a DFIX 1.39 0.02 C37a C38a DFIX 1.39 0.02 C38a C33a DANG 2.50 0.04 C39a C34a DANG 2.50 0.04 C39a C38a DANG 2.41 0.04 C33a C35a DANG 2.41 0.04 C34a C36a DANG 2.41 0.04 C35a C37a DANG 2.41 0.04 C36a C38a DANG 2.41 0.04 C37a C33a DANG 2.41 0.04 C38a C34a FLAT 0.10 C33a C34a C35a C36a C37a C38a C39a SIMU 0.04 0.08 C33a C34a C35a C36a C37a C38a C39a ISOR 0.1 0.2 C33a C34a C35a C36a C37a C38a C39a DELU 0.01 C33a C34a C35a C36a C37a C38a C39a DFIX 1.50 0.02 C33b C39b DFIX 1.39 0.02 C33b C34b DFIX 1.39 0.02 C34b C35b DFIX 1.39 0.02 C35b C36b DFIX 1.39 0.02 C36b C37b DFIX 1.39 0.02 C37b C38b DFIX 1.39 0.02 C38b C33b DANG 2.50 0.04 C39b C34b DANG 2.50 0.04 C39b C38b DANG 2.41 0.04 C33b C35b DANG 2.41 0.04 C34b C36b DANG 2.41 0.04 C35b C37b DANG 2.41 0.04 C36b C38b DANG 2.41 0.04 C37b C33b DANG 2.41 0.04 C38b C34b FLAT 0.10 C33b C34b C35b C36b C37b C38b C39b SIMU 0.04 0.08 C33b C34b C35b C36b C37b C38b C39b ISOR 0.1 0.2 C33b C34b C35b C36b C37b C38b C39b DELU 0.01 C33b C34b C35b C36b C37b C38b C39b DFIX 1.50 0.02 C10 C29 DFIX 1.54 0.02 C29 C30 DANG 2.50 0.04 C9 C29 DANG 2.50 0.04 C11 C29 DANG 2.47 0.04 C10 C30 DFIX 1.50 0.02 C10 C29a DFIX 1.54 0.02 C29a C30a DANG 2.50 0.04 C9 C29a DANG 2.50 0.04 C11 C29a DANG 2.47 0.04 C10 C30a SIMU 0.04 0.08 C29 C30 C29a C30a ISOR 0.1 0.2 C29 C30 C29a C30a DELU 0.01 C29 C30 C29a C30a DFIX 1.50 0.02 C2 C23 DFIX 1.54 0.02 C23 C24 DANG 2.50 0.04 C1 C23 DANG 2.50 0.04 C3 C23 DANG 2.47 0.04 C2 C24 DFIX 1.50 0.02 C2 C23a DFIX 1.54 0.02 C23a C24a DANG 2.50 0.04 C1 C23a DANG 2.50 0.04 C3 C23a DANG 2.47 0.04 C2 C24a SIMU 0.04 0.08 C23 C24 C23a C24a ISOR 0.1 0.2 C23 C24 C23a C24a DELU 0.01 C23 C24 C23a C24a DFIX 1.50 0.02 C11 C31 DFIX 1.54 0.02 C31 C32 DANG 2.50 0.04 C10 C31 DANG 2.50 0.04 C12 C31 DANG 2.47 0.04 C11 C32 DFIX 1.50 0.02 C11 C31a DFIX 1.54 0.02 C31a C32a DANG 2.50 0.04 C10 C31a DANG 2.50 0.04 C12 C31a DANG 2.47 0.04 C11 C32a SIMU 0.04 0.08 C31 C32 C31a C32a ISOR 0.1 0.2 C31 C32 C31a C32a DELU 0.01 C31 C32 C31a C32a DFIX 1.50 0.02 C1 C21 DFIX 1.54 0.02 C21 C22 DANG 2.50 0.04 C2 C21 DANG 2.50 0.04 C20 C21 DANG 2.47 0.04 C1 C22 DFIX 1.50 0.02 C1 C21a DFIX 1.54 0.02 C21a C22a DANG 2.50 0.04 C2 C21a DANG 2.50 0.04 C20 C21a DANG 2.47 0.04 C1 C22a SIMU 0.04 0.08 C21 C22 C21a C22a ISOR 0.1 0.2 C21 C22 C21a C22a DELU 0.01 C21 C22 C21a C22a OMIT 4 2 9 OMIT 0 17 2 SUMP 1.0 0.00001 1.0 2 1.0 3 1.0 4 FMAP 2 PLAN -20 SIZE 0.09 0.18 0.21 ACTA HTAB 2.00000 BOND $H CONF WPDB -2 L.S. 5 TEMP -173.00 WGHT 0.090700 1.935700 FVAR 2.06701 0.53723 0.24673 0.21603 0.51940 0.38557 0.60983 FVAR 0.52438 0.69289 F1 4 0.761496 0.554237 0.509946 11.00000 0.06821 0.09746 = 0.10436 0.01343 0.04430 0.00709 F2 4 0.888361 0.501600 0.624352 11.00000 0.03934 0.08837 = 0.16837 -0.00091 -0.00145 0.00371 F3 4 0.384332 0.140938 0.228587 11.00000 0.08483 0.11518 = 0.13005 -0.02361 0.06703 -0.01516 F5 4 0.269713 0.209268 0.137479 11.00000 0.18603 0.12542 = 0.05093 0.00104 0.03464 -0.05283 N1 5 0.693735 0.532320 0.658726 11.00000 0.04527 0.09388 = 0.06296 0.01569 -0.00040 -0.00216 N2 5 0.702241 0.457245 0.532376 11.00000 0.03952 0.09475 = 0.07756 0.00891 0.01522 -0.00078 N3 5 0.393548 0.236169 0.295108 11.00000 0.06775 0.11256 = 0.06305 -0.00242 0.03513 -0.01126 N4 5 0.205246 0.175996 0.281860 11.00000 0.04917 0.09025 = 0.05046 0.00743 0.01174 0.00517 C1 1 0.540122 0.539224 0.743514 11.00000 0.09233 0.13008 = 0.04606 -0.00606 0.02287 -0.03319 C2 1 0.627634 0.581683 0.776395 11.00000 0.09768 0.12477 = 0.04717 -0.00425 0.01325 -0.02853 C3 1 0.719920 0.576817 0.722759 11.00000 0.06270 0.10174 = 0.06022 0.01112 -0.01095 -0.01206 C4 1 0.738306 0.425644 0.463553 11.00000 0.05063 0.10541 = 0.10615 -0.00493 0.03618 -0.00027 C5 1 0.650409 0.380849 0.433148 11.00000 0.04801 0.10665 = 0.08778 -0.00571 0.03155 -0.00760 C6 1 0.642020 0.339042 0.361091 11.00000 0.07767 0.12782 = 0.12085 -0.02702 0.06538 -0.02490 AFIX 43 H6 2 0.702500 0.335398 0.322543 11.00000 -1.20000 AFIX 0 C7 1 0.540196 0.302838 0.348538 11.00000 0.06698 0.11603 = 0.08493 -0.01454 0.04341 -0.01817 C8 1 0.499931 0.257323 0.280459 11.00000 0.09830 0.12511 = 0.10025 -0.02221 0.06970 -0.03012 C9 1 0.117013 0.134874 0.256174 11.00000 0.04567 0.08867 = 0.07863 0.00506 0.01210 0.00700 C10 1 0.031528 0.138667 0.315765 11.00000 0.05257 0.10758 = 0.13621 -0.02923 0.04028 -0.00716 C11 1 0.068619 0.184152 0.380609 11.00000 0.05042 0.13288 = 0.12108 -0.02292 0.04158 -0.00576 C12 1 0.176330 0.207151 0.358056 11.00000 0.04020 0.09874 = 0.06228 0.00833 0.01130 0.00533 C13 1 0.253121 0.251245 0.402569 11.00000 0.04139 0.10538 = 0.05115 0.00745 0.01201 0.00594 AFIX 43 H13 2 0.231492 0.271712 0.455171 11.00000 -1.20000 AFIX 0 C14 1 0.358223 0.265721 0.372627 11.00000 0.04747 0.10090 = 0.04394 0.00811 0.01429 0.00169 C15 1 0.449186 0.308563 0.406415 11.00000 0.04423 0.10182 = 0.04787 0.00655 0.01678 -0.00123 C16 1 0.456547 0.350820 0.477202 11.00000 0.03905 0.09966 = 0.04458 0.00797 0.01061 0.00220 AFIX 43 H16 2 0.395693 0.354600 0.515376 11.00000 -1.20000 AFIX 0 C17 1 0.557236 0.387220 0.489337 11.00000 0.04155 0.09280 = 0.05024 0.01094 0.00974 0.00167 C18 1 0.591050 0.435536 0.551012 11.00000 0.03970 0.09400 = 0.05359 0.01499 0.00828 0.00081 C19 1 0.534055 0.460913 0.617443 11.00000 0.04979 0.10060 = 0.04561 0.01272 0.00879 -0.00375 AFIX 43 H19 2 0.458521 0.445410 0.627205 11.00000 -1.20000 AFIX 0 C20 1 0.582432 0.508427 0.671070 11.00000 0.05290 0.10635 = 0.04903 0.01355 0.00594 -0.01003 PART 1 C21 1 0.406721 0.538457 0.765601 81.00000 0.13612 0.05291 = 0.06564 0.00043 0.04894 -0.00210 AFIX 23 H21A 2 0.385916 0.576683 0.787049 81.00000 -1.20000 H21B 2 0.345194 0.528266 0.705198 81.00000 -1.20000 AFIX 0 C22 1 0.402889 0.495495 0.845444 81.00000 0.15480 0.08859 = 0.05840 -0.00371 0.03422 -0.00016 AFIX 133 H22A 2 0.419442 0.457461 0.822551 81.00000 -1.50000 H22B 2 0.321000 0.496031 0.861254 81.00000 -1.50000 H22C 2 0.465737 0.505107 0.904357 81.00000 -1.50000 AFIX 0 PART 2 C21A 1 0.437795 0.514633 0.785189 -81.00000 0.08400 0.08215 = 0.05185 0.00786 0.04062 -0.00323 AFIX 23 H21C 2 0.374587 0.499678 0.729446 -81.00000 -1.20000 H21D 2 0.399065 0.546384 0.814163 -81.00000 -1.20000 AFIX 0 C22A 1 0.466005 0.468444 0.861292 -81.00000 0.06971 0.11396 = 0.07394 0.03126 0.03057 0.01460 AFIX 133 H22D 2 0.451945 0.431253 0.828999 -81.00000 -1.50000 H22E 2 0.411981 0.472558 0.907948 -81.00000 -1.50000 H22F 2 0.552496 0.471382 0.896585 -81.00000 -1.50000 AFIX 0 PART 1 C23 1 0.599026 0.629880 0.845245 61.00000 0.09662 0.13355 = 0.03533 -0.01256 -0.00723 -0.06668 AFIX 23 H23A 2 0.634173 0.666133 0.827636 61.00000 -1.20000 H23B 2 0.508397 0.634689 0.834846 61.00000 -1.20000 AFIX 0 C24 1 0.652161 0.616915 0.953316 61.00000 0.10145 0.07864 = 0.06786 0.00547 -0.00724 -0.00222 AFIX 133 H24A 2 0.620884 0.580099 0.970215 61.00000 -1.50000 H24B 2 0.627260 0.646750 0.994162 61.00000 -1.50000 H24C 2 0.742538 0.615551 0.965125 61.00000 -1.50000 AFIX 0 PART 2 C23A 1 0.647089 0.620384 0.864531 -61.00000 0.07887 0.18790 = 0.04048 -0.01353 -0.00098 -0.02103 AFIX 23 H23C 2 0.565681 0.630588 0.877871 -61.00000 -1.20000 H23D 2 0.687039 0.655900 0.849216 -61.00000 -1.20000 AFIX 0 C24A 1 0.727052 0.593493 0.957201 -61.00000 0.11304 0.15706 = 0.05769 -0.01150 -0.00747 0.01484 AFIX 133 H24D 2 0.686828 0.558907 0.974007 -61.00000 -1.50000 H24E 2 0.737092 0.620554 1.011895 -61.00000 -1.50000 H24F 2 0.808332 0.583835 0.944915 -61.00000 -1.50000 AFIX 0 PART 0 C25 1 0.832648 0.612558 0.729084 11.00000 0.05951 0.10312 = 0.10220 0.00999 -0.01480 -0.00702 AFIX 133 H25A 2 0.905927 0.590708 0.760507 11.00000 -1.50000 H25B 2 0.826374 0.646667 0.768149 11.00000 -1.50000 H25C 2 0.839655 0.623763 0.662749 11.00000 -1.50000 AFIX 0 C26 1 0.853557 0.436848 0.426559 11.00000 0.06611 0.12767 = 0.16524 -0.03019 0.06836 -0.02220 AFIX 133 H26A 2 0.866755 0.477973 0.423623 11.00000 -1.50000 H26B 2 0.844668 0.420495 0.360663 11.00000 -1.50000 H26C 2 0.924455 0.419387 0.471251 11.00000 -1.50000 AFIX 0 C27 1 0.559686 0.235443 0.201022 11.00000 0.17606 0.16246 = 0.19101 -0.07811 0.15489 -0.08018 AFIX 123 H27A 2 0.575329 0.194567 0.210282 91.00000 -1.50000 H27B 2 0.638069 0.255382 0.204174 91.00000 -1.50000 H27C 2 0.504718 0.242079 0.136686 91.00000 -1.50000 H27D 2 0.570082 0.266785 0.157146 -91.00000 -1.50000 H27E 2 0.507342 0.205970 0.163255 -91.00000 -1.50000 H27F 2 0.640693 0.219273 0.230742 -91.00000 -1.50000 AFIX 0 C28 1 0.119329 0.093625 0.175305 11.00000 0.07291 0.08848 = 0.09516 -0.00251 0.02401 0.00353 AFIX 133 H28A 2 0.126365 0.114379 0.115752 11.00000 -1.50000 H28B 2 0.042854 0.071295 0.162102 11.00000 -1.50000 H28C 2 0.190290 0.068084 0.194898 11.00000 -1.50000 AFIX 0 PART 1 C29 1 -0.083519 0.100056 0.295162 51.00000 0.06693 0.17187 = 0.12911 -0.09283 0.05835 -0.04052 AFIX 23 H29A 2 -0.107312 0.092021 0.223748 51.00000 -1.20000 H29B 2 -0.153062 0.120355 0.314050 51.00000 -1.20000 AFIX 0 C30 1 -0.060536 0.041697 0.353561 51.00000 0.13953 0.21386 = 0.09198 -0.04791 0.05068 -0.11616 AFIX 133 H30A 2 0.005341 0.020508 0.332572 51.00000 -1.50000 H30B 2 -0.136672 0.019125 0.339884 51.00000 -1.50000 H30C 2 -0.036083 0.049420 0.424291 51.00000 -1.50000 AFIX 0 PART 2 C29A 1 -0.069981 0.101059 0.334973 -51.00000 0.07738 0.15175 = 0.21281 -0.08158 0.08489 -0.03116 AFIX 23 H29C 2 -0.075756 0.103296 0.404807 -51.00000 -1.20000 H29D 2 -0.055660 0.060983 0.318678 -51.00000 -1.20000 AFIX 0 C30A 1 -0.187378 0.124243 0.267503 -51.00000 0.06396 0.30132 = 0.21657 -0.16960 0.03695 -0.03347 AFIX 133 H30D 2 -0.220170 0.155628 0.300476 -51.00000 -1.50000 H30E 2 -0.249241 0.093899 0.252575 -51.00000 -1.50000 H30F 2 -0.167919 0.138053 0.206240 -51.00000 -1.50000 AFIX 0 PART 1 C31 1 0.022520 0.198420 0.477081 71.00000 0.06316 0.09706 = 0.11669 0.03857 0.04586 0.02110 AFIX 23 H31A 2 -0.023693 0.165954 0.496625 71.00000 -1.20000 H31B 2 0.093138 0.207442 0.531898 71.00000 -1.20000 AFIX 0 C32 1 -0.061679 0.250162 0.450574 71.00000 0.07092 0.08735 = 0.16060 0.00959 0.00497 0.00644 AFIX 133 H32A 2 -0.013168 0.282442 0.435304 71.00000 -1.50000 H32B 2 -0.098477 0.259945 0.506314 71.00000 -1.50000 H32C 2 -0.127368 0.241266 0.393109 71.00000 -1.50000 AFIX 0 PART 2 C31A 1 -0.011150 0.220474 0.429570 -71.00000 0.04486 0.06815 = 0.06928 -0.00333 0.02558 0.00277 AFIX 23 H31C 2 0.040035 0.231002 0.494633 -71.00000 -1.20000 H31D 2 -0.077682 0.195468 0.442485 -71.00000 -1.20000 AFIX 0 C32A 1 -0.074309 0.275439 0.384627 -71.00000 0.07116 0.07251 = 0.10747 0.00422 0.05072 0.01513 AFIX 133 H32D 2 -0.011688 0.302031 0.371650 -71.00000 -1.50000 H32E 2 -0.118802 0.292804 0.430717 -71.00000 -1.50000 H32F 2 -0.132721 0.266541 0.322848 -71.00000 -1.50000 AFIX 0 PART 1 C33 1 0.810527 0.222516 0.605265 21.00000 0.05248 0.19924 = 0.08971 -0.06144 0.03572 -0.01473 C34 1 0.710943 0.215416 0.528073 21.00000 0.05175 0.18139 = 0.07040 -0.03745 0.03073 -0.02151 AFIX 43 H34 2 0.669567 0.248474 0.498399 21.00000 -1.20000 AFIX 0 C35 1 0.666829 0.162341 0.490553 21.00000 0.05397 0.18005 = 0.06484 -0.01509 0.01060 -0.03937 AFIX 43 H35 2 0.595949 0.159509 0.438277 21.00000 -1.20000 AFIX 0 C36 1 0.728482 0.114426 0.531128 21.00000 0.08207 0.18450 = 0.07578 -0.01187 0.02000 -0.03230 AFIX 43 H36 2 0.703779 0.078018 0.504308 21.00000 -1.20000 AFIX 0 C37 1 0.826123 0.119387 0.610743 21.00000 0.06739 0.19932 = 0.07990 -0.00942 0.02189 -0.01243 AFIX 43 H37 2 0.866231 0.086190 0.640985 21.00000 -1.20000 AFIX 0 C38 1 0.866819 0.173340 0.647550 21.00000 0.05559 0.22763 = 0.07706 -0.03736 0.02089 -0.01429 AFIX 43 H38 2 0.934373 0.176093 0.702600 21.00000 -1.20000 AFIX 0 C39 1 0.861343 0.279107 0.641861 21.00000 0.09908 0.24053 = 0.14284 -0.12412 0.05366 -0.04800 AFIX 133 H39A 2 0.937532 0.286381 0.619096 21.00000 -1.50000 H39B 2 0.879322 0.279378 0.713944 21.00000 -1.50000 H39C 2 0.800584 0.308767 0.616603 21.00000 -1.50000 AFIX 0 PART 2 C33A 1 0.687602 0.110752 0.507895 31.00000 0.04844 0.09270 = 0.06432 0.01751 0.02890 0.01222 C34A 1 0.758111 0.138783 0.588903 31.00000 0.04351 0.07647 = 0.05859 0.01655 0.02749 0.00436 AFIX 43 H34A 2 0.742637 0.177845 0.598891 31.00000 -1.20000 AFIX 0 C35A 1 0.849587 0.111214 0.654737 31.00000 0.04137 0.08880 = 0.05533 0.01590 0.03015 0.00623 AFIX 43 H35A 2 0.895910 0.131664 0.709322 31.00000 -1.20000 AFIX 0 C36A 1 0.876245 0.053958 0.643527 31.00000 0.03914 0.07519 = 0.07297 0.01237 0.00721 0.00094 AFIX 43 H36A 2 0.939488 0.034849 0.689124 31.00000 -1.20000 AFIX 0 C37A 1 0.805719 0.026291 0.562389 31.00000 0.04818 0.07873 = 0.06976 0.00949 0.00649 -0.00194 AFIX 43 H37A 2 0.822707 -0.012502 0.551525 31.00000 -1.20000 AFIX 0 C38A 1 0.712218 0.053132 0.497313 31.00000 0.03931 0.08662 = 0.05871 0.00260 0.01206 0.00003 AFIX 43 H38A 2 0.663616 0.032216 0.444371 31.00000 -1.20000 AFIX 0 C39A 1 0.585470 0.140161 0.438945 31.00000 0.05707 0.10307 = 0.07399 0.00662 0.01247 0.01877 AFIX 133 H39D 2 0.571461 0.121727 0.374348 31.00000 -1.50000 H39E 2 0.607682 0.180117 0.432574 31.00000 -1.50000 H39F 2 0.509910 0.138035 0.464438 31.00000 -1.50000 AFIX 0 PART 3 C33B 1 0.816181 0.071609 0.590875 41.00000 0.06304 C34B 1 0.724338 0.070703 0.505198 41.00000 0.08537 AFIX 43 H34B 2 0.706371 0.036026 0.469957 41.00000 -1.20000 AFIX 0 C35B 1 0.657654 0.119747 0.469616 41.00000 0.08206 AFIX 43 H35B 2 0.594358 0.118519 0.411399 41.00000 -1.20000 AFIX 0 C36B 1 0.687003 0.171604 0.522843 41.00000 0.06078 AFIX 43 H36B 2 0.644489 0.205629 0.499236 41.00000 -1.20000 AFIX 0 C37B 1 0.777755 0.172349 0.609201 41.00000 0.07589 AFIX 43 H37B 2 0.795470 0.206587 0.645793 41.00000 -1.20000 AFIX 0 C38B 1 0.842252 0.123145 0.641787 41.00000 0.07278 AFIX 43 H38B 2 0.905620 0.124309 0.699963 41.00000 -1.20000 AFIX 0 C39B 1 0.882059 0.016356 0.623684 41.00000 0.09619 AFIX 133 H39G 2 0.957002 0.013792 0.597439 41.00000 -1.50000 H39H 2 0.827377 -0.015662 0.599171 41.00000 -1.50000 H39I 2 0.904517 0.015109 0.695716 41.00000 -1.50000 AFIX 0 PART 0 B1 3 0.765935 0.512762 0.582577 11.00000 0.03796 0.09282 = 0.09307 0.01952 0.01408 0.00629 B2 3 0.312841 0.188014 0.231960 11.00000 0.08046 0.10484 = 0.05664 0.00279 0.02609 -0.01541 HKLF 4 REM 201000906 REM R1 = 0.0785 for 4116 Fo > 4sig(Fo) and 0.1076 for all 6470 data REM 613 parameters refined using 527 restraints END WGHT 0.0976 1.3838 REM Highest difference peak 0.285, deepest hole -0.367, 1-sigma level 0.046 Q1 1 0.8651 0.4980 0.6803 11.00000 0.05 0.29 Q2 1 0.5206 0.2505 0.1824 11.00000 0.05 0.27 Q3 1 0.2193 0.2281 0.1543 11.00000 0.05 0.27 Q4 1 0.6054 0.2291 0.2450 11.00000 0.05 0.25 Q5 1 0.8904 0.4979 0.6009 11.00000 0.05 0.24 Q6 1 -0.1903 0.0993 0.2850 11.00000 0.05 0.21 Q7 1 0.3262 0.2056 0.1597 11.00000 0.05 0.19 Q8 1 0.8678 0.4349 0.4789 11.00000 0.05 0.18 Q9 1 0.8509 0.2416 0.6618 11.00000 0.05 0.18 Q10 1 0.0424 0.2046 0.3429 11.00000 0.05 0.18 Q11 1 -0.1477 0.0855 0.2184 11.00000 0.05 0.17 Q12 1 0.0649 0.1591 0.3753 11.00000 0.05 0.17 Q13 1 0.5425 0.2170 0.1665 11.00000 0.05 0.16 Q14 1 -0.1072 0.1203 0.2794 11.00000 0.05 0.16 Q15 1 0.8721 0.6161 0.8060 11.00000 0.05 0.16 Q16 1 0.2365 0.1942 0.1053 11.00000 0.05 0.15 Q17 1 0.0925 0.1965 0.4324 11.00000 0.05 0.15 Q18 1 0.8267 0.4415 0.4028 11.00000 0.05 0.15 Q19 1 -0.2010 0.1492 0.2238 11.00000 0.05 0.15 Q20 1 0.8451 0.4571 0.4012 11.00000 0.05 0.14 ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 F1 F 0.76150(16) 0.55424(8) 0.50995(15) 0.0861(6) Uani 1 1 d . A . F2 F 0.88836(15) 0.50160(8) 0.62435(18) 0.1024(7) Uani 1 1 d . A . F3 F 0.38433(19) 0.14094(10) 0.22859(17) 0.1034(7) Uani 1 1 d . B . F5 F 0.2697(3) 0.20927(10) 0.13748(14) 0.1195(9) Uani 1 1 d . B . N1 N 0.6937(2) 0.53232(12) 0.65873(18) 0.0692(7) Uani 1 1 d . A . N2 N 0.7022(2) 0.45724(12) 0.53238(19) 0.0702(7) Uani 1 1 d . A . N3 N 0.3935(2) 0.23617(13) 0.29511(19) 0.0779(8) Uani 1 1 d . B . N4 N 0.2052(2) 0.17600(11) 0.28186(17) 0.0632(6) Uani 1 1 d . B . C1 C 0.5401(3) 0.53922(18) 0.7435(2) 0.0883(11) Uani 1 1 d D . . C2 C 0.6276(4) 0.58168(18) 0.7764(2) 0.0903(11) Uani 1 1 d D A . C3 C 0.7199(3) 0.57682(16) 0.7228(2) 0.0786(10) Uani 1 1 d D . . C4 C 0.7383(3) 0.42564(17) 0.4636(3) 0.0845(10) Uani 1 1 d . . . C5 C 0.6504(3) 0.38085(16) 0.4331(3) 0.0783(9) Uani 1 1 d . . . C6 C 0.6420(3) 0.33904(19) 0.3611(3) 0.1021(13) Uani 1 1 d . . . H6 H 0.7025 0.3354 0.3225 0.123 Uiso 1 1 calc R . . C7 C 0.5402(3) 0.30284(17) 0.3485(3) 0.0852(10) Uani 1 1 d . . . C8 C 0.4999(4) 0.25732(19) 0.2805(3) 0.1006(13) Uani 1 1 d . . . C9 C 0.1170(3) 0.13487(15) 0.2562(2) 0.0712(8) Uani 1 1 d D B . C10 C 0.0315(3) 0.13867(18) 0.3158(3) 0.0958(12) Uani 1 1 d D . . C11 C 0.0686(3) 0.18415(19) 0.3806(3) 0.0980(12) Uani 1 1 d D B . C12 C 0.1763(2) 0.20715(15) 0.3581(2) 0.0671(8) Uani 1 1 d D . . C13 C 0.2531(2) 0.25125(15) 0.4026(2) 0.0657(8) Uani 1 1 d . B . H13 H 0.2315 0.2717 0.4552 0.079 Uiso 1 1 calc R . . C14 C 0.3582(2) 0.26572(14) 0.37263(19) 0.0634(8) Uani 1 1 d . . . C15 C 0.4492(2) 0.30856(14) 0.4064(2) 0.0636(8) Uani 1 1 d . B . C16 C 0.4565(2) 0.35082(14) 0.47720(19) 0.0609(8) Uani 1 1 d . . . H16 H 0.3957 0.3546 0.5154 0.073 Uiso 1 1 calc R B . C17 C 0.5572(2) 0.38722(14) 0.4893(2) 0.0616(7) Uani 1 1 d . B . C18 C 0.5911(2) 0.43554(14) 0.5510(2) 0.0627(8) Uani 1 1 d . . . C19 C 0.5341(3) 0.46091(14) 0.6174(2) 0.0656(8) Uani 1 1 d . A . H19 H 0.4585 0.4454 0.6272 0.079 Uiso 1 1 calc R . . C20 C 0.5824(3) 0.50843(15) 0.6711(2) 0.0702(9) Uani 1 1 d D A . C21 C 0.4067(11) 0.5385(5) 0.7656(9) 0.081(3) Uani 0.524(18) 1 d PDU A 1 H21A H 0.3859 0.5767 0.7870 0.097 Uiso 0.524(18) 1 calc PR A 1 H21B H 0.3452 0.5283 0.7052 0.097 Uiso 0.524(18) 1 calc PR A 1 C22 C 0.4029(16) 0.4955(5) 0.8454(7) 0.099(4) Uani 0.524(18) 1 d PDU A 1 H22A H 0.4194 0.4575 0.8226 0.148 Uiso 0.524(18) 1 calc PR A 1 H22B H 0.3210 0.4960 0.8613 0.148 Uiso 0.524(18) 1 calc PR A 1 H22C H 0.4657 0.5051 0.9044 0.148 Uiso 0.524(18) 1 calc PR A 1 C21A C 0.4378(10) 0.5146(6) 0.7852(7) 0.069(3) Uani 0.476(18) 1 d PDU A 2 H21C H 0.3746 0.4997 0.7294 0.082 Uiso 0.476(18) 1 calc PR A 2 H21D H 0.3991 0.5464 0.8142 0.082 Uiso 0.476(18) 1 calc PR A 2 C22A C 0.4660(9) 0.4684(6) 0.8613(6) 0.084(3) Uani 0.476(18) 1 d PDU A 2 H22D H 0.4519 0.4313 0.8290 0.125 Uiso 0.476(18) 1 calc PR A 2 H22E H 0.4120 0.4726 0.9079 0.125 Uiso 0.476(18) 1 calc PR A 2 H22F H 0.5525 0.4714 0.8966 0.125 Uiso 0.476(18) 1 calc PR A 2 C23 C 0.5990(16) 0.6299(6) 0.8452(10) 0.092(5) Uani 0.386(19) 1 d PDU A 1 H23A H 0.6342 0.6661 0.8276 0.110 Uiso 0.386(19) 1 calc PR A 1 H23B H 0.5084 0.6347 0.8348 0.110 Uiso 0.386(19) 1 calc PR A 1 C24 C 0.6522(18) 0.6169(5) 0.9533(7) 0.087(5) Uani 0.386(19) 1 d PDU A 1 H24A H 0.6209 0.5801 0.9702 0.130 Uiso 0.386(19) 1 calc PR A 1 H24B H 0.6273 0.6467 0.9942 0.130 Uiso 0.386(19) 1 calc PR A 1 H24C H 0.7425 0.6156 0.9651 0.130 Uiso 0.386(19) 1 calc PR A 1 C23A C 0.6471(11) 0.6204(5) 0.8645(7) 0.105(3) Uani 0.614(19) 1 d PDU A 2 H23C H 0.5657 0.6306 0.8779 0.125 Uiso 0.614(19) 1 calc PR A 2 H23D H 0.6870 0.6559 0.8492 0.125 Uiso 0.614(19) 1 calc PR A 2 C24A C 0.7271(11) 0.5935(6) 0.9572(5) 0.113(3) Uani 0.614(19) 1 d PDU A 2 H24D H 0.6868 0.5589 0.9740 0.170 Uiso 0.614(19) 1 calc PR A 2 H24E H 0.7371 0.6206 1.0119 0.170 Uiso 0.614(19) 1 calc PR A 2 H24F H 0.8083 0.5838 0.9449 0.170 Uiso 0.614(19) 1 calc PR A 2 C25 C 0.8326(3) 0.61256(17) 0.7291(3) 0.0932(12) Uani 1 1 d . A . H25A H 0.9059 0.5907 0.7605 0.140 Uiso 1 1 calc R . . H25B H 0.8264 0.6467 0.7681 0.140 Uiso 1 1 calc R . . H25C H 0.8397 0.6238 0.6627 0.140 Uiso 1 1 calc R . . C26 C 0.8536(3) 0.43685(19) 0.4266(4) 0.1131(15) Uani 1 1 d . . . H26A H 0.8668 0.4780 0.4236 0.170 Uiso 1 1 calc R . . H26B H 0.8447 0.4205 0.3607 0.170 Uiso 1 1 calc R . . H26C H 0.9245 0.4194 0.4713 0.170 Uiso 1 1 calc R . . C27 C 0.5597(5) 0.2354(2) 0.2010(4) 0.159(3) Uani 1 1 d . . . H27A H 0.5753 0.1946 0.2103 0.238 Uiso 0.69(8) 1 calc PR . . H27B H 0.6381 0.2554 0.2042 0.238 Uiso 0.69(8) 1 calc PR . . H27C H 0.5047 0.2421 0.1367 0.238 Uiso 0.69(8) 1 calc PR . . H27D H 0.5701 0.2668 0.1571 0.238 Uiso 0.31(8) 1 calc PR . . H27E H 0.5073 0.2060 0.1633 0.238 Uiso 0.31(8) 1 calc PR . . H27F H 0.6407 0.2193 0.2307 0.238 Uiso 0.31(8) 1 calc PR . . C28 C 0.1193(3) 0.09362(15) 0.1753(3) 0.0847(10) Uani 1 1 d . . . H28A H 0.1264 0.1144 0.1158 0.127 Uiso 1 1 calc R B . H28B H 0.0429 0.0713 0.1621 0.127 Uiso 1 1 calc R . . H28C H 0.1903 0.0681 0.1949 0.127 Uiso 1 1 calc R . . C29 C -0.0835(12) 0.1001(6) 0.2952(10) 0.117(4) Uani 0.519(9) 1 d PDU B 1 H29A H -0.1073 0.0920 0.2237 0.140 Uiso 0.519(9) 1 calc PR B 1 H29B H -0.1531 0.1204 0.3140 0.140 Uiso 0.519(9) 1 calc PR B 1 C30 C -0.0605(9) 0.0417(5) 0.3536(6) 0.145(5) Uani 0.519(9) 1 d PDU B 1 H30A H 0.0053 0.0205 0.3326 0.217 Uiso 0.519(9) 1 calc PR B 1 H30B H -0.1367 0.0191 0.3399 0.217 Uiso 0.519(9) 1 calc PR B 1 H30C H -0.0361 0.0494 0.4243 0.217 Uiso 0.519(9) 1 calc PR B 1 C29A C -0.0700(13) 0.1011(7) 0.3350(13) 0.139(7) Uani 0.481(9) 1 d PDU B 2 H29C H -0.0758 0.1033 0.4048 0.167 Uiso 0.481(9) 1 calc PR B 2 H29D H -0.0557 0.0610 0.3187 0.167 Uiso 0.481(9) 1 calc PR B 2 C30A C -0.1874(9) 0.1242(6) 0.2675(9) 0.193(7) Uani 0.481(9) 1 d PDU B 2 H30D H -0.2202 0.1556 0.3005 0.289 Uiso 0.481(9) 1 calc PR B 2 H30E H -0.2492 0.0939 0.2526 0.289 Uiso 0.481(9) 1 calc PR B 2 H30F H -0.1679 0.1381 0.2062 0.289 Uiso 0.481(9) 1 calc PR B 2 C31 C 0.0225(7) 0.1984(4) 0.4771(7) 0.088(2) Uani 0.610(14) 1 d PDU B 1 H31A H -0.0237 0.1660 0.4966 0.106 Uiso 0.610(14) 1 calc PR B 1 H31B H 0.0931 0.2074 0.5319 0.106 Uiso 0.610(14) 1 calc PR B 1 C32 C -0.0617(7) 0.2502(4) 0.4506(10) 0.109(4) Uani 0.610(14) 1 d PDU B 1 H32A H -0.0132 0.2824 0.4353 0.164 Uiso 0.610(14) 1 calc PR B 1 H32B H -0.0985 0.2599 0.5063 0.164 Uiso 0.610(14) 1 calc PR B 1 H32C H -0.1274 0.2413 0.3931 0.164 Uiso 0.610(14) 1 calc PR B 1 C31A C -0.0112(8) 0.2205(5) 0.4296(8) 0.059(3) Uani 0.390(14) 1 d PDU B 2 H31C H 0.0400 0.2310 0.4946 0.071 Uiso 0.390(14) 1 calc PR B 2 H31D H -0.0777 0.1955 0.4425 0.071 Uiso 0.390(14) 1 calc PR B 2 C32A C -0.0743(9) 0.2754(5) 0.3846(11) 0.079(4) Uani 0.390(14) 1 d PDU B 2 H32D H -0.0117 0.3020 0.3717 0.118 Uiso 0.390(14) 1 calc PR B 2 H32E H -0.1188 0.2928 0.4307 0.118 Uiso 0.390(14) 1 calc PR B 2 H32F H -0.1327 0.2665 0.3228 0.118 Uiso 0.390(14) 1 calc PR B 2 C33 C 0.8105(6) 0.2225(4) 0.6053(6) 0.111(3) Uani 0.537(3) 1 d PDU C 1 C34 C 0.7109(5) 0.2154(4) 0.5281(5) 0.099(2) Uani 0.537(3) 1 d PDU C 1 H34 H 0.6696 0.2485 0.4984 0.118 Uiso 0.537(3) 1 calc PR C 1 C35 C 0.6668(7) 0.1623(5) 0.4906(7) 0.100(3) Uani 0.537(3) 1 d PDU C 1 H35 H 0.5959 0.1595 0.4383 0.120 Uiso 0.537(3) 1 calc PR C 1 C36 C 0.7285(10) 0.1144(6) 0.5311(9) 0.114(4) Uani 0.537(3) 1 d PDU C 1 H36 H 0.7038 0.0780 0.5043 0.136 Uiso 0.537(3) 1 calc PR C 1 C37 C 0.8261(12) 0.1194(6) 0.6107(9) 0.115(4) Uani 0.537(3) 1 d PDU C 1 H37 H 0.8662 0.0862 0.6410 0.138 Uiso 0.537(3) 1 calc PR C 1 C38 C 0.8668(7) 0.1733(5) 0.6475(6) 0.119(3) Uani 0.537(3) 1 d PDU C 1 H38 H 0.9344 0.1761 0.7026 0.143 Uiso 0.537(3) 1 calc PR C 1 C39 C 0.8613(8) 0.2791(5) 0.6419(7) 0.157(4) Uani 0.537(3) 1 d PDU C 1 H39A H 0.9375 0.2864 0.6191 0.235 Uiso 0.537(3) 1 calc PR C 1 H39B H 0.8793 0.2794 0.7139 0.235 Uiso 0.537(3) 1 calc PR C 1 H39C H 0.8006 0.3088 0.6166 0.235 Uiso 0.537(3) 1 calc PR C 1 C33A C 0.6876(14) 0.1108(7) 0.5079(13) 0.066(4) Uani 0.247(5) 1 d PDU D 2 C34A C 0.7581(11) 0.1388(6) 0.5889(10) 0.057(3) Uani 0.247(5) 1 d PDU D 2 H34A H 0.7426 0.1778 0.5989 0.068 Uiso 0.247(5) 1 calc PR D 2 C35A C 0.8496(14) 0.1112(7) 0.6547(12) 0.059(4) Uani 0.247(5) 1 d PDU D 2 H35A H 0.8959 0.1317 0.7093 0.071 Uiso 0.247(5) 1 calc PR D 2 C36A C 0.8762(10) 0.0540(5) 0.6435(9) 0.063(3) Uani 0.247(5) 1 d PDU D 2 H36A H 0.9395 0.0348 0.6891 0.076 Uiso 0.247(5) 1 calc PR D 2 C37A C 0.8057(10) 0.0263(5) 0.5624(8) 0.067(3) Uani 0.247(5) 1 d PDU D 2 H37A H 0.8227 -0.0125 0.5515 0.080 Uiso 0.247(5) 1 calc PR D 2 C38A C 0.7122(12) 0.0531(7) 0.4973(10) 0.061(3) Uani 0.247(5) 1 d PDU D 2 H38A H 0.6636 0.0322 0.4444 0.074 Uiso 0.247(5) 1 calc PR D 2 C39A C 0.5855(12) 0.1402(7) 0.4389(10) 0.078(4) Uani 0.247(5) 1 d PDU D 2 H39D H 0.5715 0.1217 0.3743 0.117 Uiso 0.247(5) 1 calc PR D 2 H39E H 0.6077 0.1801 0.4326 0.117 Uiso 0.247(5) 1 calc PR D 2 H39F H 0.5099 0.1380 0.4644 0.117 Uiso 0.247(5) 1 calc PR D 2 C33B C 0.8162(13) 0.0716(6) 0.5909(10) 0.063(4) Uiso 0.216(6) 1 d PDU E 3 C34B C 0.7243(18) 0.0707(9) 0.5052(14) 0.085(9) Uiso 0.216(6) 1 d PDU E 3 H34B H 0.7064 0.0360 0.4700 0.102 Uiso 0.216(6) 1 calc PR E 3 C35B C 0.658(2) 0.1197(8) 0.4696(14) 0.082(7) Uiso 0.216(6) 1 d PDU E 3 H35B H 0.5944 0.1185 0.4114 0.098 Uiso 0.216(6) 1 calc PR E 3 C36B C 0.6870(18) 0.1716(7) 0.5228(12) 0.061(5) Uiso 0.216(6) 1 d PDU E 3 H36B H 0.6445 0.2056 0.4992 0.073 Uiso 0.216(6) 1 calc PR E 3 C37B C 0.7778(16) 0.1723(8) 0.6092(12) 0.076(5) Uiso 0.216(6) 1 d PDU E 3 H37B H 0.7955 0.2066 0.6458 0.091 Uiso 0.216(6) 1 calc PR E 3 C38B C 0.842(3) 0.1231(8) 0.642(2) 0.073(9) Uiso 0.216(6) 1 d PDU E 3 H38B H 0.9056 0.1243 0.7000 0.087 Uiso 0.216(6) 1 calc PR E 3 C39B C 0.8821(18) 0.0164(7) 0.6237(14) 0.096(6) Uiso 0.216(6) 1 d PDU E 3 H39G H 0.9570 0.0138 0.5974 0.144 Uiso 0.216(6) 1 calc PR E 3 H39H H 0.8274 -0.0157 0.5992 0.144 Uiso 0.216(6) 1 calc PR E 3 H39I H 0.9045 0.0151 0.6957 0.144 Uiso 0.216(6) 1 calc PR E 3 B1 B 0.7659(3) 0.51276(18) 0.5826(3) 0.0747(11) Uani 1 1 d . . . B2 B 0.3128(4) 0.1880(2) 0.2320(3) 0.0789(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0682(11) 0.0975(14) 0.1044(15) 0.0134(11) 0.0443(10) 0.0071(9) F2 0.0393(9) 0.0884(13) 0.168(2) -0.0009(13) -0.0014(11) 0.0037(8) F3 0.0848(13) 0.1152(17) 0.1301(18) -0.0236(14) 0.0670(13) -0.0152(12) F5 0.186(3) 0.1254(18) 0.0509(11) 0.0010(11) 0.0346(13) -0.0528(17) N1 0.0453(13) 0.0939(19) 0.0630(15) 0.0157(14) -0.0004(11) -0.0022(12) N2 0.0395(12) 0.0948(19) 0.0776(17) 0.0089(14) 0.0152(11) -0.0008(12) N3 0.0677(16) 0.113(2) 0.0630(16) -0.0024(15) 0.0351(13) -0.0113(15) N4 0.0492(13) 0.0903(18) 0.0505(13) 0.0074(12) 0.0117(10) 0.0052(12) C1 0.092(2) 0.130(3) 0.0461(17) -0.0061(19) 0.0229(17) -0.033(2) C2 0.098(3) 0.125(3) 0.0472(18) -0.0042(19) 0.0132(17) -0.029(2) C3 0.0627(19) 0.102(3) 0.0602(19) 0.0111(18) -0.0110(15) -0.0121(17) C4 0.0506(17) 0.105(3) 0.106(3) -0.005(2) 0.0362(18) -0.0003(17) C5 0.0480(16) 0.107(3) 0.088(2) -0.006(2) 0.0315(16) -0.0076(16) C6 0.078(2) 0.128(3) 0.121(3) -0.027(3) 0.065(2) -0.025(2) C7 0.067(2) 0.116(3) 0.085(2) -0.015(2) 0.0434(18) -0.0182(19) C8 0.098(3) 0.125(3) 0.100(3) -0.022(2) 0.070(2) -0.030(2) C9 0.0457(15) 0.089(2) 0.079(2) 0.0051(17) 0.0121(14) 0.0070(15) C10 0.0526(18) 0.108(3) 0.136(3) -0.029(3) 0.040(2) -0.0072(18) C11 0.0504(18) 0.133(3) 0.121(3) -0.023(3) 0.0416(19) -0.0058(19) C12 0.0402(14) 0.099(2) 0.0623(18) 0.0083(16) 0.0113(12) 0.0053(14) C13 0.0414(14) 0.105(2) 0.0511(16) 0.0075(15) 0.0120(12) 0.0059(14) C14 0.0475(15) 0.101(2) 0.0439(15) 0.0081(14) 0.0143(12) 0.0017(14) C15 0.0442(14) 0.102(2) 0.0479(15) 0.0066(15) 0.0168(12) -0.0012(14) C16 0.0391(13) 0.100(2) 0.0446(15) 0.0080(15) 0.0106(11) 0.0022(13) C17 0.0415(14) 0.093(2) 0.0502(15) 0.0109(15) 0.0097(11) 0.0017(13) C18 0.0397(13) 0.094(2) 0.0536(16) 0.0150(15) 0.0083(12) 0.0008(13) C19 0.0498(15) 0.101(2) 0.0456(15) 0.0127(15) 0.0088(12) -0.0037(15) C20 0.0529(16) 0.106(3) 0.0490(16) 0.0135(16) 0.0059(13) -0.0100(16) C21 0.136(8) 0.053(5) 0.066(5) 0.000(4) 0.049(5) -0.002(5) C22 0.155(11) 0.089(6) 0.058(5) -0.004(4) 0.034(6) 0.000(7) C21A 0.084(5) 0.082(8) 0.052(5) 0.008(5) 0.041(4) -0.003(5) C22A 0.070(5) 0.114(8) 0.074(5) 0.031(5) 0.031(4) 0.015(5) C23 0.097(11) 0.134(10) 0.035(5) -0.013(6) -0.007(6) -0.067(8) C24 0.101(11) 0.079(7) 0.068(6) 0.005(5) -0.007(6) -0.002(6) C23A 0.079(6) 0.188(8) 0.040(5) -0.014(4) -0.001(4) -0.021(6) C24A 0.113(7) 0.157(8) 0.058(4) -0.012(4) -0.007(4) 0.015(6) C25 0.0595(19) 0.103(3) 0.102(3) 0.010(2) -0.0148(18) -0.0070(18) C26 0.066(2) 0.128(3) 0.165(4) -0.030(3) 0.068(3) -0.022(2) C27 0.176(5) 0.162(5) 0.191(5) -0.078(4) 0.155(5) -0.080(4) C28 0.073(2) 0.088(2) 0.095(3) -0.003(2) 0.0240(19) 0.0035(18) C29 0.067(6) 0.172(9) 0.129(8) -0.093(6) 0.058(6) -0.041(6) C30 0.140(8) 0.214(11) 0.092(6) -0.048(6) 0.051(5) -0.116(8) C29A 0.077(7) 0.152(11) 0.213(17) -0.082(11) 0.085(8) -0.031(6) C30A 0.064(6) 0.301(17) 0.217(13) -0.170(12) 0.037(6) -0.033(7) C31 0.063(4) 0.097(5) 0.117(6) 0.039(4) 0.046(4) 0.021(3) C32 0.071(4) 0.087(6) 0.161(10) 0.010(6) 0.005(5) 0.006(4) C31A 0.045(5) 0.068(7) 0.069(6) -0.003(5) 0.026(4) 0.003(4) C32A 0.071(6) 0.073(7) 0.107(9) 0.004(6) 0.051(5) 0.015(4) C33 0.052(4) 0.199(8) 0.090(5) -0.061(5) 0.036(3) -0.015(4) C34 0.052(3) 0.181(7) 0.070(4) -0.037(4) 0.031(3) -0.022(4) C35 0.054(4) 0.180(9) 0.065(5) -0.015(5) 0.011(4) -0.039(5) C36 0.082(8) 0.185(9) 0.076(6) -0.012(7) 0.020(5) -0.032(6) C37 0.067(6) 0.199(9) 0.080(8) -0.009(7) 0.022(5) -0.012(6) C38 0.056(4) 0.228(9) 0.077(5) -0.037(5) 0.021(3) -0.014(5) C39 0.099(6) 0.241(9) 0.143(8) -0.124(8) 0.054(6) -0.048(6) C33A 0.048(10) 0.093(9) 0.064(10) 0.018(7) 0.029(6) 0.012(7) C34A 0.044(7) 0.076(8) 0.059(8) 0.017(6) 0.027(6) 0.004(5) C35A 0.041(7) 0.089(8) 0.055(8) 0.016(7) 0.030(6) 0.006(6) C36A 0.039(5) 0.075(7) 0.073(7) 0.012(6) 0.007(5) 0.001(5) C37A 0.048(6) 0.079(8) 0.070(7) 0.009(5) 0.006(5) -0.002(5) C38A 0.039(6) 0.087(8) 0.059(7) 0.003(6) 0.012(4) 0.000(6) C39A 0.057(7) 0.103(10) 0.074(8) 0.007(7) 0.012(6) 0.019(7) B1 0.0380(16) 0.093(3) 0.093(3) 0.020(2) 0.0141(17) 0.0063(16) B2 0.080(3) 0.105(3) 0.057(2) 0.003(2) 0.0261(19) -0.015(2) _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 F1 B1 1.398(4) . ? F2 B1 1.380(4) . ? F3 B2 1.368(5) . ? F5 B2 1.391(4) . ? N1 C3 1.364(4) . ? N1 C20 1.400(4) . ? N1 B1 1.532(5) . ? N2 C4 1.341(4) . ? N2 C18 1.410(3) . ? N2 B1 1.573(5) . ? N3 C8 1.336(4) . ? N3 C14 1.409(4) . ? N3 B2 1.585(5) . ? N4 C9 1.366(4) . ? N4 C12 1.383(4) . ? N4 B2 1.532(4) . ? C1 C2 1.398(5) . ? C1 C20 1.403(5) . ? C1 C21A 1.499(9) . ? C1 C21 1.575(11) . ? C2 C3 1.397(5) . ? C2 C23A 1.505(10) . ? C2 C23 1.561(13) . ? C3 C25 1.493(5) . ? C4 C5 1.435(5) . ? C4 C26 1.502(4) . ? C5 C6 1.393(5) . ? C5 C17 1.434(4) . ? C6 C7 1.394(5) . ? C6 H6 0.9500 . ? C7 C15 1.429(4) . ? C7 C8 1.435(5) . ? C8 C27 1.499(5) . ? C9 C10 1.392(4) . ? C9 C28 1.491(5) . ? C10 C11 1.402(5) . ? C10 C29A 1.501(13) . ? C10 C29 1.541(12) . ? C11 C12 1.408(4) . ? C11 C31A 1.497(9) . ? C11 C31 1.575(8) . ? C12 C13 1.398(4) . ? C13 C14 1.364(4) . ? C13 H13 0.9500 . ? C14 C15 1.430(4) . ? C15 C16 1.389(4) . ? C16 C17 1.387(4) . ? C16 H16 0.9500 . ? C17 C18 1.424(4) . ? C18 C19 1.366(4) . ? C19 C20 1.385(4) . ? C19 H19 0.9500 . ? C21 C22 1.510(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C21A C22A 1.502(10) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23 C24 1.523(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C23A C24A 1.534(10) . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C27 H27F 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.587(15) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C29A C30A 1.530(16) . ? C29A H29C 0.9900 . ? C29A H29D 0.9900 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31 C32 1.529(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C31A C32A 1.536(11) . ? C31A H31C 0.9900 . ? C31A H31D 0.9900 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33 C34 1.373(9) . ? C33 C38 1.383(11) . ? C33 C39 1.491(10) . ? C34 C35 1.399(11) . ? C34 H34 0.9500 . ? C35 C36 1.374(12) . ? C35 H35 0.9500 . ? C36 C37 1.375(12) . ? C36 H36 0.9500 . ? C37 C38 1.405(13) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C33A C34A 1.390(15) . ? C33A C38A 1.396(15) . ? C33A C39A 1.486(15) . ? C34A C35A 1.372(15) . ? C34A H34A 0.9500 . ? C35A C36A 1.394(16) . ? C35A H35A 0.9500 . ? C36A C37A 1.388(13) . ? C36A H36A 0.9500 . ? C37A C38A 1.373(13) . ? C37A H37A 0.9500 . ? C38A H38A 0.9500 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C33B C34B 1.390(16) . ? C33B C38B 1.402(16) . ? C33B C39B 1.511(15) . ? C34B C35B 1.401(17) . ? C34B H34B 0.9500 . ? C35B C36B 1.427(16) . ? C35B H35B 0.9500 . ? C36B C37B 1.390(16) . ? C36B H36B 0.9500 . ? C37B C38B 1.383(17) . ? C37B H37B 0.9500 . ? C38B H38B 0.9500 . ? C39B H39G 0.9800 . ? C39B H39H 0.9800 . ? C39B H39I 0.9800 . ? 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 C3 N1 C20 107.1(3) . . ? C3 N1 B1 127.9(3) . . ? C20 N1 B1 124.9(3) . . ? C4 N2 C18 109.9(3) . . ? C4 N2 B1 127.0(3) . . ? C18 N2 B1 123.0(3) . . ? C8 N3 C14 109.6(3) . . ? C8 N3 B2 126.3(3) . . ? C14 N3 B2 124.0(3) . . ? C9 N4 C12 107.6(2) . . ? C9 N4 B2 126.6(3) . . ? C12 N4 B2 125.7(3) . . ? C2 C1 C20 106.7(3) . . ? C2 C1 C21A 132.7(5) . . ? C20 C1 C21A 118.7(6) . . ? C2 C1 C21 124.0(5) . . ? C20 C1 C21 127.6(5) . . ? C3 C2 C1 107.7(3) . . ? C3 C2 C23A 119.6(6) . . ? C1 C2 C23A 131.6(6) . . ? C3 C2 C23 131.2(7) . . ? C1 C2 C23 120.0(7) . . ? N1 C3 C2 109.6(3) . . ? N1 C3 C25 121.8(3) . . ? C2 C3 C25 128.6(4) . . ? N2 C4 C5 109.2(3) . . ? N2 C4 C26 123.8(3) . . ? C5 C4 C26 127.0(3) . . ? C6 C5 C17 121.6(3) . . ? C6 C5 C4 131.7(3) . . ? C17 C5 C4 106.6(3) . . ? C5 C6 C7 116.5(3) . . ? C5 C6 H6 121.8 . . ? C7 C6 H6 121.8 . . ? C6 C7 C15 121.6(3) . . ? C6 C7 C8 131.7(3) . . ? C15 C7 C8 106.7(3) . . ? N3 C8 C7 109.5(3) . . ? N3 C8 C27 122.1(4) . . ? C7 C8 C27 128.3(3) . . ? N4 C9 C10 109.9(3) . . ? N4 C9 C28 121.9(3) . . ? C10 C9 C28 128.2(3) . . ? C9 C10 C11 106.9(3) . . ? C9 C10 C29A 134.7(8) . . ? C11 C10 C29A 117.4(8) . . ? C9 C10 C29 119.7(6) . . ? C11 C10 C29 133.1(6) . . ? C10 C11 C12 107.0(3) . . ? C10 C11 C31A 127.5(4) . . ? C12 C11 C31A 119.8(5) . . ? C10 C11 C31 127.4(4) . . ? C12 C11 C31 123.9(4) . . ? N4 C12 C13 120.8(3) . . ? N4 C12 C11 108.5(3) . . ? C13 C12 C11 130.6(3) . . ? C14 C13 C12 121.9(3) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 N3 120.7(3) . . ? C13 C14 C15 131.6(3) . . ? N3 C14 C15 107.8(2) . . ? C16 C15 C7 121.9(3) . . ? C16 C15 C14 131.7(2) . . ? C7 C15 C14 106.4(3) . . ? C17 C16 C15 116.6(3) . . ? C17 C16 H16 121.7 . . ? C15 C16 H16 121.7 . . ? C16 C17 C18 131.6(3) . . ? C16 C17 C5 121.7(3) . . ? C18 C17 C5 106.6(3) . . ? C19 C18 N2 121.3(3) . . ? C19 C18 C17 131.1(3) . . ? N2 C18 C17 107.7(3) . . ? C18 C19 C20 122.4(3) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 N1 120.3(3) . . ? C19 C20 C1 130.8(3) . . ? N1 C20 C1 108.9(3) . . ? C22 C21 C1 109.3(7) . . ? C22 C21 H21A 109.8 . . ? C1 C21 H21A 109.8 . . ? C22 C21 H21B 109.8 . . ? C1 C21 H21B 109.8 . . ? H21A C21 H21B 108.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1 C21A C22A 119.6(8) . . ? C1 C21A H21C 107.4 . . ? C22A C21A H21C 107.4 . . ? C1 C21A H21D 107.4 . . ? C22A C21A H21D 107.4 . . ? H21C C21A H21D 107.0 . . ? C21A C22A H22D 109.5 . . ? C21A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C21A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C24 C23 C2 112.0(10) . . ? C24 C23 H23A 109.2 . . ? C2 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C2 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C2 C23A C24A 113.0(8) . . ? C2 C23A H23C 109.0 . . ? C24A C23A H23C 109.0 . . ? C2 C23A H23D 109.0 . . ? C24A C23A H23D 109.0 . . ? H23C C23A H23D 107.8 . . ? C23A C24A H24D 109.5 . . ? C23A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C23A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C3 C25 H25A 109.5 . . ? C3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C4 C26 H26A 109.5 . . ? C4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 H27A 109.5 . . ? C8 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C8 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C8 C27 H27D 109.5 . . ? H27A C27 H27D 141.1 . . ? H27B C27 H27D 56.3 . . ? H27C C27 H27D 56.3 . . ? C8 C27 H27E 109.5 . . ? H27A C27 H27E 56.3 . . ? H27B C27 H27E 141.1 . . ? H27C C27 H27E 56.3 . . ? H27D C27 H27E 109.5 . . ? C8 C27 H27F 109.5 . . ? H27A C27 H27F 56.3 . . ? H27B C27 H27F 56.3 . . ? H27C C27 H27F 141.1 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? C9 C28 H28A 109.5 . . ? C9 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C9 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C10 C29 C30 112.3(9) . . ? C10 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? C10 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C10 C29A C30A 104.6(11) . . ? C10 C29A H29C 110.8 . . ? C30A C29A H29C 110.8 . . ? C10 C29A H29D 110.8 . . ? C30A C29A H29D 110.8 . . ? H29C C29A H29D 108.9 . . ? C29A C30A H30D 109.5 . . ? C29A C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C29A C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C32 C31 C11 105.0(6) . . ? C32 C31 H31A 110.8 . . ? C11 C31 H31A 110.8 . . ? C32 C31 H31B 110.8 . . ? C11 C31 H31B 110.8 . . ? H31A C31 H31B 108.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C11 C31A C32A 123.8(7) . . ? C11 C31A H31C 106.4 . . ? C32A C31A H31C 106.4 . . ? C11 C31A H31D 106.4 . . ? C32A C31A H31D 106.4 . . ? H31C C31A H31D 106.5 . . ? C31A C32A H32D 109.5 . . ? C31A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C31A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C34 C33 C38 116.3(8) . . ? C34 C33 C39 123.8(9) . . ? C38 C33 C39 119.9(8) . . ? C33 C34 C35 123.8(9) . . ? C33 C34 H34 118.1 . . ? C35 C34 H34 118.1 . . ? C36 C35 C34 118.4(9) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C35 C36 C37 119.7(12) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 120.3(13) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C33 C38 C37 121.3(9) . . ? C33 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C33 C39 H39A 109.5 . . ? C33 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C33 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34A C33A C38A 117.2(13) . . ? C34A C33A C39A 121.2(13) . . ? C38A C33A C39A 121.5(13) . . ? C35A C34A C33A 121.4(14) . . ? C35A C34A H34A 119.3 . . ? C33A C34A H34A 119.3 . . ? C34A C35A C36A 121.7(14) . . ? C34A C35A H35A 119.2 . . ? C36A C35A H35A 119.2 . . ? C37A C36A C35A 116.6(11) . . ? C37A C36A H36A 121.7 . . ? C35A C36A H36A 121.7 . . ? C38A C37A C36A 122.2(12) . . ? C38A C37A H37A 118.9 . . ? C36A C37A H37A 118.9 . . ? C37A C38A C33A 120.9(13) . . ? C37A C38A H38A 119.6 . . ? C33A C38A H38A 119.6 . . ? C33A C39A H39D 109.5 . . ? C33A C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C33A C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C34B C33B C38B 118.6(14) . . ? C34B C33B C39B 117.5(14) . . ? C38B C33B C39B 123.9(14) . . ? C33B C34B C35B 121.5(17) . . ? C33B C34B H34B 119.2 . . ? C35B C34B H34B 119.2 . . ? C34B C35B C36B 118.5(17) . . ? C34B C35B H35B 120.8 . . ? C36B C35B H35B 120.8 . . ? C37B C36B C35B 120.0(15) . . ? C37B C36B H36B 120.0 . . ? C35B C36B H36B 120.0 . . ? C38B C37B C36B 119.9(17) . . ? C38B C37B H37B 120.1 . . ? C36B C37B H37B 120.1 . . ? C37B C38B C33B 121.5(18) . . ? C37B C38B H38B 119.3 . . ? C33B C38B H38B 119.3 . . ? C33B C39B H39G 109.5 . . ? C33B C39B H39H 109.5 . . ? H39G C39B H39H 109.5 . . ? C33B C39B H39I 109.5 . . ? H39G C39B H39I 109.5 . . ? H39H C39B H39I 109.5 . . ? F2 B1 F1 108.3(3) . . ? F2 B1 N1 112.3(3) . . ? F1 B1 N1 110.5(3) . . ? F2 B1 N2 109.5(3) . . ? F1 B1 N2 108.4(3) . . ? N1 B1 N2 107.7(3) . . ? F3 B2 F5 109.9(3) . . ? F3 B2 N4 112.4(3) . . ? F5 B2 N4 110.8(3) . . ? F3 B2 N3 109.6(3) . . ? F5 B2 N3 107.7(3) . . ? N4 B2 N3 106.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 C1 C2 C3 1.0(4) . . . . ? C21A C1 C2 C3 164.5(8) . . . . ? C21 C1 C2 C3 -164.7(7) . . . . ? C20 C1 C2 C23A -166.7(7) . . . . ? C21A C1 C2 C23A -3.3(12) . . . . ? C21 C1 C2 C23A 27.5(11) . . . . ? C20 C1 C2 C23 170.2(7) . . . . ? C21A C1 C2 C23 -26.4(12) . . . . ? C21 C1 C2 C23 4.4(10) . . . . ? C20 N1 C3 C2 0.3(4) . . . . ? B1 N1 C3 C2 177.2(3) . . . . ? C20 N1 C3 C25 -179.6(3) . . . . ? B1 N1 C3 C25 -2.7(5) . . . . ? C1 C2 C3 N1 -0.9(4) . . . . ? C23A C2 C3 N1 168.6(6) . . . . ? C23 C2 C3 N1 -168.3(8) . . . . ? C1 C2 C3 C25 179.1(3) . . . . ? C23A C2 C3 C25 -11.4(8) . . . . ? C23 C2 C3 C25 11.6(10) . . . . ? C18 N2 C4 C5 0.1(4) . . . . ? B1 N2 C4 C5 -176.3(3) . . . . ? C18 N2 C4 C26 -179.7(4) . . . . ? B1 N2 C4 C26 3.8(6) . . . . ? N2 C4 C5 C6 176.2(4) . . . . ? C26 C4 C5 C6 -4.0(7) . . . . ? N2 C4 C5 C17 -0.3(4) . . . . ? C26 C4 C5 C17 179.5(4) . . . . ? C17 C5 C6 C7 -1.7(6) . . . . ? C4 C5 C6 C7 -177.8(4) . . . . ? C5 C6 C7 C15 0.2(6) . . . . ? C5 C6 C7 C8 177.4(4) . . . . ? C14 N3 C8 C7 -0.3(5) . . . . ? B2 N3 C8 C7 176.1(3) . . . . ? C14 N3 C8 C27 -178.5(5) . . . . ? B2 N3 C8 C27 -2.2(7) . . . . ? C6 C7 C8 N3 -178.0(4) . . . . ? C15 C7 C8 N3 -0.5(5) . . . . ? C6 C7 C8 C27 0.2(9) . . . . ? C15 C7 C8 C27 177.7(5) . . . . ? C12 N4 C9 C10 -0.6(4) . . . . ? B2 N4 C9 C10 -177.4(3) . . . . ? C12 N4 C9 C28 179.5(3) . . . . ? B2 N4 C9 C28 2.8(5) . . . . ? N4 C9 C10 C11 0.2(4) . . . . ? C28 C9 C10 C11 -180.0(3) . . . . ? N4 C9 C10 C29A -167.6(10) . . . . ? C28 C9 C10 C29A 12.2(11) . . . . ? N4 C9 C10 C29 174.7(7) . . . . ? C28 C9 C10 C29 -5.4(9) . . . . ? C9 C10 C11 C12 0.3(5) . . . . ? C29A C10 C11 C12 170.6(8) . . . . ? C29 C10 C11 C12 -173.2(9) . . . . ? C9 C10 C11 C31A 153.3(8) . . . . ? C29A C10 C11 C31A -36.4(12) . . . . ? C29 C10 C11 C31A -20.2(13) . . . . ? C9 C10 C11 C31 -165.6(6) . . . . ? C29A C10 C11 C31 4.7(10) . . . . ? C29 C10 C11 C31 21.0(12) . . . . ? C9 N4 C12 C13 177.6(3) . . . . ? B2 N4 C12 C13 -5.6(5) . . . . ? C9 N4 C12 C11 0.8(4) . . . . ? B2 N4 C12 C11 177.6(3) . . . . ? C10 C11 C12 N4 -0.7(4) . . . . ? C31A C11 C12 N4 -156.2(6) . . . . ? C31 C11 C12 N4 165.8(5) . . . . ? C10 C11 C12 C13 -177.1(3) . . . . ? C31A C11 C12 C13 27.4(8) . . . . ? C31 C11 C12 C13 -10.6(8) . . . . ? N4 C12 C13 C14 0.6(4) . . . . ? C11 C12 C13 C14 176.7(4) . . . . ? C12 C13 C14 N3 -0.3(5) . . . . ? C12 C13 C14 C15 179.9(3) . . . . ? C8 N3 C14 C13 -179.0(3) . . . . ? B2 N3 C14 C13 4.6(5) . . . . ? C8 N3 C14 C15 0.9(4) . . . . ? B2 N3 C14 C15 -175.5(3) . . . . ? C6 C7 C15 C16 0.8(6) . . . . ? C8 C7 C15 C16 -177.0(3) . . . . ? C6 C7 C15 C14 178.8(4) . . . . ? C8 C7 C15 C14 1.0(4) . . . . ? C13 C14 C15 C16 -3.6(6) . . . . ? N3 C14 C15 C16 176.5(3) . . . . ? C13 C14 C15 C7 178.7(3) . . . . ? N3 C14 C15 C7 -1.2(3) . . . . ? C7 C15 C16 C17 -0.3(4) . . . . ? C14 C15 C16 C17 -177.7(3) . . . . ? C15 C16 C17 C18 177.3(3) . . . . ? C15 C16 C17 C5 -1.3(4) . . . . ? C6 C5 C17 C16 2.4(5) . . . . ? C4 C5 C17 C16 179.3(3) . . . . ? C6 C5 C17 C18 -176.5(3) . . . . ? C4 C5 C17 C18 0.4(4) . . . . ? C4 N2 C18 C19 -179.0(3) . . . . ? B1 N2 C18 C19 -2.4(4) . . . . ? C4 N2 C18 C17 0.2(3) . . . . ? B1 N2 C18 C17 176.8(3) . . . . ? C16 C17 C18 C19 0.0(5) . . . . ? C5 C17 C18 C19 178.7(3) . . . . ? C16 C17 C18 N2 -179.1(3) . . . . ? C5 C17 C18 N2 -0.3(3) . . . . ? N2 C18 C19 C20 -1.0(4) . . . . ? C17 C18 C19 C20 -179.9(3) . . . . ? C18 C19 C20 N1 -0.2(4) . . . . ? C18 C19 C20 C1 -178.1(3) . . . . ? C3 N1 C20 C19 -178.0(3) . . . . ? B1 N1 C20 C19 5.0(4) . . . . ? C3 N1 C20 C1 0.3(3) . . . . ? B1 N1 C20 C1 -176.7(3) . . . . ? C2 C1 C20 C19 177.3(3) . . . . ? C21A C1 C20 C19 11.0(8) . . . . ? C21 C1 C20 C19 -17.6(8) . . . . ? C2 C1 C20 N1 -0.9(4) . . . . ? C21A C1 C20 N1 -167.1(6) . . . . ? C21 C1 C20 N1 164.2(7) . . . . ? C2 C1 C21 C22 -103.4(7) . . . . ? C20 C1 C21 C22 93.9(9) . . . . ? C21A C1 C21 C22 15.9(14) . . . . ? C2 C1 C21A C22A -83.5(11) . . . . ? C20 C1 C21A C22A 78.4(10) . . . . ? C21 C1 C21A C22A -164(2) . . . . ? C3 C2 C23 C24 -97.8(11) . . . . ? C1 C2 C23 C24 96.0(10) . . . . ? C23A C2 C23 C24 -32(2) . . . . ? C3 C2 C23A C24A -80.4(9) . . . . ? C1 C2 C23A C24A 86.2(9) . . . . ? C23 C2 C23A C24A 152(3) . . . . ? C9 C10 C29 C30 90.6(10) . . . . ? C11 C10 C29 C30 -96.6(11) . . . . ? C29A C10 C29 C30 -51(3) . . . . ? C9 C10 C29A C30A -96.6(12) . . . . ? C11 C10 C29A C30A 96.6(11) . . . . ? C29 C10 C29A C30A -48(3) . . . . ? C10 C11 C31 C32 -106.4(6) . . . . ? C12 C11 C31 C32 90.0(7) . . . . ? C31A C11 C31 C32 -3.4(7) . . . . ? C10 C11 C31A C32A -89.7(10) . . . . ? C12 C11 C31A C32A 60.3(10) . . . . ? C31 C11 C31A C32A 167.6(14) . . . . ? C38 C33 C34 C35 -1.1(9) . . . . ? C39 C33 C34 C35 176.8(7) . . . . ? C33 C34 C35 C36 -2.0(12) . . . . ? C34 C35 C36 C37 4.1(17) . . . . ? C35 C36 C37 C38 -3(2) . . . . ? C34 C33 C38 C37 2.1(12) . . . . ? C39 C33 C38 C37 -175.9(9) . . . . ? C36 C37 C38 C33 0.0(18) . . . . ? C38A C33A C34A C35A 1.1(15) . . . . ? C39A C33A C34A C35A 177.6(14) . . . . ? C33A C34A C35A C36A 0.1(15) . . . . ? C34A C35A C36A C37A 0.1(18) . . . . ? C35A C36A C37A C38A -1.5(19) . . . . ? C36A C37A C38A C33A 3(2) . . . . ? C34A C33A C38A C37A -3(2) . . . . ? C39A C33A C38A C37A -179.0(13) . . . . ? C38B C33B C34B C35B 0(2) . . . . ? C39B C33B C34B C35B 179.5(14) . . . . ? C33B C34B C35B C36B 0.8(17) . . . . ? C34B C35B C36B C37B -2(3) . . . . ? C35B C36B C37B C38B 2(4) . . . . ? C36B C37B C38B C33B -2(4) . . . . ? C34B C33B C38B C37B 1(4) . . . . ? C39B C33B C38B C37B -179(2) . . . . ? C3 N1 B1 F2 55.6(4) . . . . ? C20 N1 B1 F2 -128.0(3) . . . . ? C3 N1 B1 F1 -65.4(4) . . . . ? C20 N1 B1 F1 111.0(3) . . . . ? C3 N1 B1 N2 176.4(3) . . . . ? C20 N1 B1 N2 -7.2(4) . . . . ? C4 N2 B1 F2 -55.6(5) . . . . ? C18 N2 B1 F2 128.4(3) . . . . ? C4 N2 B1 F1 62.3(4) . . . . ? C18 N2 B1 F1 -113.7(3) . . . . ? C4 N2 B1 N1 -178.1(3) . . . . ? C18 N2 B1 N1 5.9(4) . . . . ? C9 N4 B2 F3 -55.5(4) . . . . ? C12 N4 B2 F3 128.3(3) . . . . ? C9 N4 B2 F5 67.8(5) . . . . ? C12 N4 B2 F5 -108.4(3) . . . . ? C9 N4 B2 N3 -175.4(3) . . . . ? C12 N4 B2 N3 8.4(4) . . . . ? C8 N3 B2 F3 54.6(5) . . . . ? C14 N3 B2 F3 -129.6(3) . . . . ? C8 N3 B2 F5 -64.9(5) . . . . ? C14 N3 B2 F5 110.9(3) . . . . ? C8 N3 B2 N4 176.3(4) . . . . ? C14 N3 B2 N4 -7.9(4) . . . . ? data_tahara _database_code_depnum_ccdc_archive 'CCDC 864649' #TrackingRef '9288_web_deposit_cif_file_4_HidemitsuUno_1327633261.transBenzobisEtBODIPY.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C52 H50 B2 Cl2 F4 N4' _chemical_formula_moiety 'C32 H36 B2 F4 N4, 2(C10 H7 Cl)' _chemical_formula_weight 899.51 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.944(3) _cell_length_b 10.964(4) _cell_length_c 13.432(4) _cell_angle_alpha 98.902(13) _cell_angle_beta 93.514(13) _cell_angle_gamma 104.888(14) _cell_volume 1110.7(7) _cell_formula_units_Z 1 _cell_measurement_reflns_used 1924 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 30.44 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470.00 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.996 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.111 _diffrn_reflns_number 12159 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measured_fraction_theta_full 0.983 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #============================================================================== # REFINEMENT DATA _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. ; _reflns_number_total 5031 _reflns_number_gt 3071 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1916 _refine_ls_R_factor_gt 0.1653 _refine_ls_wR_factor_ref 0.3974 _refine_ls_wR_factor_gt 0.3905 _refine_ls_goodness_of_fit_ref 1.233 _refine_ls_restrained_S_all 1.233 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5020 _refine_ls_number_parameters 293 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0000P)^2^+17.4958P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_diff_density_max 0.880 _refine_diff_density_min -0.750 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.042(10) _iucr_refine_instructions_details ; TITL tahara CELL 0.71075 7.94390 10.96420 13.43150 98.902 93.514 104.888 ZERR 1 0.00280 0.00370 0.00370 0.013 0.013 0.013 LATT 1 SFAC C H B F N CL UNIT 52 50 2 4 4 2 SHEL 99999.000000 0.769625 L.S. 5 FMAP 2 PLAN -25 WPDB -2 HTAB TEMP -172.8 ACTA SIZE 0.400 0.150 0.020 OMIT 1 -3 1 OMIT 2 3 5 OMIT 2 -2 2 OMIT 2 1 7 OMIT 1 -1 2 OMIT -2 4 2 OMIT 3 -5 1 OMIT -2 6 3 OMIT 3 -5 3 OMIT 1 -3 4 OMIT -2 4 7 CONF BOND $H WGHT 0.000000 17.495800 FVAR 1.21564 CL1 6 0.691243 0.319085 0.639172 11.00000 0.04585 0.10654 = 0.06212 -0.02461 -0.00684 -0.00766 F1 4 0.456645 0.198755 -0.069790 11.00000 0.02380 0.02163 = 0.01846 -0.00095 0.00260 0.01174 F2 4 0.316856 0.119424 0.060872 11.00000 0.02183 0.01461 = 0.03015 0.00646 0.00160 0.00345 N1 5 0.562119 0.310262 0.101946 11.00000 0.02025 0.01382 = 0.02039 0.00424 0.00115 0.00882 N2 5 0.274626 0.316310 0.017733 11.00000 0.01809 0.00898 = 0.02130 0.00114 0.00539 0.00381 C1 1 0.704967 0.273580 0.133702 11.00000 0.02046 0.01671 = 0.02047 0.00816 0.00653 0.00962 C2 1 0.821258 0.375107 0.200873 11.00000 0.02311 0.02421 = 0.01893 0.00606 0.00521 0.01279 C3 1 0.749497 0.479391 0.209817 11.00000 0.01734 0.01760 = 0.01583 0.00089 0.00262 0.00507 C4 1 0.586723 0.438536 0.148312 11.00000 0.01921 0.01546 = 0.01739 0.00075 0.00258 0.00550 C5 1 0.460482 0.502755 0.130619 11.00000 0.01583 0.01674 = 0.01897 0.00136 0.00353 0.00595 AFIX 43 H5 2 0.480258 0.589483 0.162673 11.00000 -1.20000 AFIX 0 C6 1 0.308909 0.444474 0.068415 11.00000 0.02208 0.01158 = 0.01893 0.00298 0.00325 0.00578 C7 1 0.159335 0.490494 0.039990 11.00000 0.01514 0.01905 = 0.01502 0.00256 0.00144 0.00368 C8 1 0.037087 0.384428 -0.026293 11.00000 0.01677 0.01372 = 0.01719 0.00278 0.00355 0.00247 C9 1 0.119209 0.280275 -0.037007 11.00000 0.02178 0.01495 = 0.01939 0.00164 0.00475 0.00701 C10 1 0.123241 0.607187 0.066997 11.00000 0.01551 0.01563 = 0.01595 -0.00067 -0.00130 0.00433 AFIX 43 H10 2 0.203267 0.677240 0.110703 11.00000 -1.20000 AFIX 0 C11 1 0.720803 0.140654 0.098926 11.00000 0.02364 0.01828 = 0.02877 -0.00042 -0.00503 0.01236 AFIX 137 H11A 2 0.629067 0.078785 0.124681 11.00000 -1.20000 H11B 2 0.836029 0.134734 0.124681 11.00000 -1.20000 H11C 2 0.707662 0.121575 0.024687 11.00000 -1.20000 AFIX 0 C12 1 0.998015 0.371624 0.249440 11.00000 0.02419 0.02587 = 0.02283 0.00492 -0.00174 0.01019 AFIX 23 H12A 2 1.046273 0.313551 0.202540 11.00000 -1.20000 H12B 2 1.079590 0.458561 0.258643 11.00000 -1.20000 AFIX 0 C13 1 0.990643 0.327641 0.350454 11.00000 0.04325 0.08231 = 0.02426 0.01939 0.00749 0.04278 AFIX 137 H13A 2 0.936806 0.381452 0.396348 11.00000 -1.50000 H13B 2 1.109634 0.334747 0.379626 11.00000 -1.50000 H13C 2 0.920699 0.238143 0.341026 11.00000 -1.50000 AFIX 0 C14 1 0.822102 0.611247 0.274069 11.00000 0.02472 0.02140 = 0.02801 -0.00078 0.00130 0.00686 AFIX 23 H14A 2 0.948796 0.641008 0.267155 11.00000 -1.20000 H14B 2 0.764638 0.671237 0.247089 11.00000 -1.20000 AFIX 0 C15 1 0.798635 0.617883 0.383591 11.00000 0.07506 0.04326 = 0.01613 -0.00341 0.00061 0.02938 AFIX 137 H15A 2 0.674415 0.583565 0.391392 11.00000 -1.50000 H15B 2 0.839075 0.707327 0.418284 11.00000 -1.50000 H15C 2 0.866951 0.567131 0.413271 11.00000 -1.50000 AFIX 0 C16 1 0.044046 0.148706 -0.098737 11.00000 0.01711 0.01980 = 0.02855 0.00204 -0.00113 0.00486 AFIX 137 H16A 2 0.129132 0.127881 -0.143701 11.00000 -1.20000 H16B 2 -0.063792 0.146448 -0.139406 11.00000 -1.20000 H16C 2 0.017706 0.085857 -0.053422 11.00000 -1.20000 AFIX 0 C17 1 0.501841 0.187269 0.601543 11.00000 0.02622 0.04751 = 0.04200 -0.00749 0.00624 0.00885 C18 1 0.432701 0.115254 0.674339 11.00000 0.05229 0.07555 = 0.02814 -0.01256 -0.01021 0.04577 AFIX 43 H18 2 0.482131 0.136336 0.743060 11.00000 -1.20000 AFIX 0 C19 1 0.293543 0.015379 0.641839 11.00000 0.06427 0.06180 = 0.03934 0.02031 0.02231 0.03619 AFIX 43 H19 2 0.243068 -0.035390 0.689252 11.00000 -1.20000 AFIX 0 C20 1 0.220912 -0.016836 0.543803 11.00000 0.04786 0.03914 = 0.03888 0.01259 0.01069 0.01383 AFIX 43 H20 2 0.124147 -0.090551 0.524627 11.00000 -1.20000 AFIX 0 C21 1 0.285825 0.056748 0.469338 11.00000 0.03330 0.03094 = 0.03204 0.00447 0.01035 0.01483 C22 1 0.204369 0.027746 0.367711 11.00000 0.03689 0.04795 = 0.02331 0.00301 0.00333 0.01359 AFIX 43 H22 2 0.103438 -0.042839 0.348440 11.00000 -1.20000 AFIX 0 C23 1 0.269595 0.099981 0.298221 11.00000 0.05712 0.05071 = 0.02490 0.00336 0.00675 0.02745 AFIX 43 H23 2 0.217015 0.077138 0.230115 11.00000 -1.20000 AFIX 0 C24 1 0.413829 0.207991 0.325980 11.00000 0.04922 0.04668 = 0.04311 0.01327 0.01701 0.01993 AFIX 43 H24 2 0.456500 0.259140 0.277172 11.00000 -1.20000 AFIX 0 C25 1 0.493868 0.240028 0.424269 11.00000 0.03818 0.04764 = 0.04763 0.01449 0.01423 0.01153 AFIX 43 H25 2 0.591334 0.313342 0.442937 11.00000 -1.20000 AFIX 0 C26 1 0.430101 0.162740 0.498406 11.00000 0.03381 0.04128 = 0.02839 -0.00353 0.00381 0.01865 B1 3 0.405911 0.231769 0.027102 11.00000 0.02401 0.01057 = 0.01532 0.00304 0.00703 0.00833 HKLF 4 REM tahara REM R1 = 0.1653 for 3071 Fo > 4sig(Fo) and 0.1916 for all 5020 data REM 293 parameters refined using 0 restraints END WGHT 0.0971 22.6393 REM Highest difference peak 0.882, deepest hole -0.751, 1-sigma level 0.145 Q1 1 0.6660 0.3915 0.5355 11.00000 0.05 0.88 Q2 1 0.1694 0.3607 0.0773 11.00000 0.05 0.75 Q3 1 0.8971 0.2369 0.0692 11.00000 0.05 0.70 Q4 1 0.3196 -0.1192 0.6399 11.00000 0.05 0.69 Q5 1 0.0569 0.3232 -0.0588 11.00000 0.05 0.69 Q6 1 0.9413 0.2245 0.3596 11.00000 0.05 0.63 Q7 1 0.1846 -0.1214 0.1154 11.00000 0.05 0.58 Q8 1 0.1304 -0.0656 0.2053 11.00000 0.05 0.58 Q9 1 0.3239 -0.1613 0.1446 11.00000 0.05 0.57 Q10 1 0.3173 0.4376 -0.0572 11.00000 0.05 0.56 Q11 1 0.5742 0.3154 0.4662 11.00000 0.05 0.55 Q12 1 0.1412 0.1174 0.3738 11.00000 0.05 0.54 Q13 1 0.4912 0.0335 0.4860 11.00000 0.05 0.54 Q14 1 0.5644 0.4783 0.3579 11.00000 0.05 0.53 Q15 1 0.2215 0.3207 -0.0342 11.00000 0.05 0.50 Q16 1 0.9026 0.2638 0.7000 11.00000 0.05 0.49 Q17 1 0.5845 0.2480 0.6443 11.00000 0.05 0.49 Q18 1 0.1362 -0.0630 0.3501 11.00000 0.05 0.49 Q19 1 0.6382 0.1733 0.7249 11.00000 0.05 0.47 Q20 1 0.1101 0.1292 -0.0245 11.00000 0.05 0.47 Q21 1 1.0835 0.4258 0.3609 11.00000 0.05 0.47 Q22 1 0.6696 0.5171 0.4549 11.00000 0.05 0.46 Q23 1 0.5042 0.2728 0.0349 11.00000 0.05 0.46 Q24 1 0.6421 0.0257 0.0592 11.00000 0.05 0.46 Q25 1 0.6479 0.3114 -0.1037 11.00000 0.05 0.45 ; 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.0013 0.0007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl1 Cl 0.6912(5) 0.3191(5) 0.6392(3) 0.0838(14) Uani 1.0 2 d . . . F1 F 0.4567(6) 0.1987(4) -0.0698(4) 0.0224(11) Uani 1.0 2 d . . . F2 F 0.3168(6) 0.1194(4) 0.0609(4) 0.0239(11) Uani 1.0 2 d . . . N1 N 0.5620(9) 0.3103(6) 0.1020(5) 0.0187(14) Uani 1.0 2 d . . . N2 N 0.2746(8) 0.3163(6) 0.0179(5) 0.0176(13) Uani 1.0 2 d . . . C1 C 0.7049(10) 0.2736(7) 0.1338(6) 0.0189(15) Uani 1.0 2 d . . . C2 C 0.8211(11) 0.3752(8) 0.2008(6) 0.0218(16) Uani 1.0 2 d . . . C3 C 0.7496(10) 0.4794(7) 0.2097(6) 0.0184(15) Uani 1.0 2 d . . . C4 C 0.5868(10) 0.4385(7) 0.1483(6) 0.0187(15) Uani 1.0 2 d . . . C5 C 0.4605(10) 0.5026(7) 0.1306(6) 0.0182(15) Uani 1.0 2 d . . . C6 C 0.3089(10) 0.4444(7) 0.0685(6) 0.0186(15) Uani 1.0 2 d . . . C7 C 0.1594(10) 0.4904(7) 0.0400(6) 0.0180(15) Uani 1.0 2 d . . . C8 C 0.0371(10) 0.3844(7) -0.0262(6) 0.0175(15) Uani 1.0 2 d . . . C9 C 0.1191(10) 0.2803(7) -0.0370(6) 0.0197(16) Uani 1.0 2 d . . . C10 C 0.1231(10) 0.6072(7) 0.0670(6) 0.0174(15) Uani 1.0 2 d . . . C11 C 0.7207(11) 0.1408(7) 0.0990(7) 0.0246(18) Uani 1.0 2 d . . . C12 C 0.9981(11) 0.3718(8) 0.2495(6) 0.0250(17) Uani 1.0 2 d . . . C13 C 0.9908(15) 0.3276(12) 0.3504(7) 0.046(3) Uani 1.0 2 d . . . C14 C 0.8221(12) 0.6112(8) 0.2740(7) 0.0268(18) Uani 1.0 2 d . . . C15 C 0.7986(17) 0.6181(10) 0.3836(7) 0.045(3) Uani 1.0 2 d . . . C16 C 0.0441(11) 0.1488(7) -0.0988(7) 0.0238(17) Uani 1.0 2 d . . . C17 C 0.5019(13) 0.1873(10) 0.6015(8) 0.042(3) Uani 1.0 2 d . . . C18 C 0.4331(16) 0.1155(12) 0.6741(8) 0.051(4) Uani 1.0 2 d . . . C19 C 0.2940(17) 0.0155(12) 0.6416(9) 0.051(3) Uani 1.0 2 d . . . C20 C 0.2211(15) -0.0169(10) 0.5438(8) 0.042(3) Uani 1.0 2 d . . . C21 C 0.2858(13) 0.0568(9) 0.4694(7) 0.033(2) Uani 1.0 2 d . . . C22 C 0.2046(14) 0.0277(10) 0.3678(7) 0.037(3) Uani 1.0 2 d . . . C23 C 0.2695(15) 0.0999(11) 0.2983(8) 0.044(3) Uani 1.0 2 d . . . C24 C 0.4137(15) 0.2079(11) 0.3262(9) 0.046(3) Uani 1.0 2 d . . . C25 C 0.4938(15) 0.2399(11) 0.4242(9) 0.045(3) Uani 1.0 2 d . . . C26 C 0.4301(13) 0.1627(10) 0.4986(7) 0.036(3) Uani 1.0 2 d . . . B1 B 0.4060(12) 0.2317(8) 0.0272(6) 0.0171(17) Uani 1.0 2 d . . . H5 H 0.4803 0.5894 0.1626 0.0218 Uiso 1.0 2 calc R . . H10 H 0.2031 0.6773 0.1107 0.0209 Uiso 1.0 2 calc R . . H11A H 0.6282 0.0788 0.1242 0.0295 Uiso 1.0 2 calc R . . H11B H 0.8355 0.1346 0.1253 0.0295 Uiso 1.0 2 calc R . . H11C H 0.7087 0.1220 0.0248 0.0295 Uiso 1.0 2 calc R . . H12A H 1.0465 0.3139 0.2026 0.0300 Uiso 1.0 2 calc R . . H12B H 1.0796 0.4588 0.2588 0.0300 Uiso 1.0 2 calc R . . H13A H 0.9352 0.3804 0.3961 0.0685 Uiso 1.0 2 calc R . . H13B H 1.1099 0.3361 0.3801 0.0685 Uiso 1.0 2 calc R . . H13C H 0.9225 0.2377 0.3408 0.0685 Uiso 1.0 2 calc R . . H14A H 0.9488 0.6410 0.2671 0.0322 Uiso 1.0 2 calc R . . H14B H 0.7646 0.6712 0.2470 0.0322 Uiso 1.0 2 calc R . . H15A H 0.6745 0.5830 0.3914 0.0676 Uiso 1.0 2 calc R . . H15B H 0.8379 0.7077 0.4181 0.0676 Uiso 1.0 2 calc R . . H15C H 0.8678 0.5681 0.4135 0.0676 Uiso 1.0 2 calc R . . H16A H 0.1296 0.1278 -0.1434 0.0286 Uiso 1.0 2 calc R . . H16B H -0.0633 0.1467 -0.1398 0.0286 Uiso 1.0 2 calc R . . H16C H 0.0170 0.0860 -0.0535 0.0286 Uiso 1.0 2 calc R . . H18 H 0.4825 0.1366 0.7428 0.0614 Uiso 1.0 2 calc R . . H19 H 0.2438 -0.0353 0.6890 0.0618 Uiso 1.0 2 calc R . . H20 H 0.1244 -0.0906 0.5248 0.0505 Uiso 1.0 2 calc R . . H22 H 0.1038 -0.0431 0.3485 0.0450 Uiso 1.0 2 calc R . . H23 H 0.2168 0.0771 0.2303 0.0524 Uiso 1.0 2 calc R . . H24 H 0.4562 0.2591 0.2774 0.0547 Uiso 1.0 2 calc R . . H25 H 0.5914 0.3131 0.4427 0.0539 Uiso 1.0 2 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl1 0.0478(19) 0.109(3) 0.064(3) -0.0071(19) -0.0069(16) -0.025(2) F1 0.025(3) 0.023(3) 0.020(3) 0.0121(19) 0.0027(18) -0.0008(17) F2 0.023(3) 0.016(2) 0.032(3) 0.0040(18) 0.0015(19) 0.0065(18) N1 0.022(4) 0.015(3) 0.022(3) 0.009(3) 0.002(3) 0.005(3) N2 0.020(4) 0.011(3) 0.022(4) 0.004(3) 0.006(3) 0.002(3) C1 0.022(4) 0.018(4) 0.022(4) 0.010(3) 0.007(3) 0.009(3) C2 0.025(4) 0.026(4) 0.020(4) 0.013(4) 0.006(3) 0.006(3) C3 0.019(4) 0.019(4) 0.017(4) 0.005(3) 0.003(3) 0.001(3) C4 0.021(4) 0.017(4) 0.018(4) 0.006(3) 0.003(3) 0.001(3) C5 0.017(4) 0.018(4) 0.020(4) 0.007(3) 0.004(3) 0.002(3) C6 0.024(4) 0.013(4) 0.020(4) 0.006(3) 0.004(3) 0.003(3) C7 0.016(4) 0.021(4) 0.016(4) 0.004(3) 0.002(3) 0.003(3) C8 0.019(4) 0.015(4) 0.018(4) 0.003(3) 0.004(3) 0.003(3) C9 0.023(4) 0.017(4) 0.021(4) 0.007(3) 0.005(3) 0.002(3) C10 0.017(4) 0.017(4) 0.017(4) 0.005(3) -0.001(3) -0.000(3) C11 0.025(5) 0.020(4) 0.030(5) 0.013(4) -0.005(4) -0.000(3) C12 0.026(5) 0.027(4) 0.024(4) 0.011(4) -0.001(4) 0.005(3) C13 0.045(6) 0.085(8) 0.025(5) 0.044(6) 0.007(5) 0.019(5) C14 0.026(5) 0.023(4) 0.030(5) 0.007(4) 0.002(4) -0.000(4) C15 0.077(8) 0.045(6) 0.018(5) 0.030(6) 0.001(5) -0.003(4) C16 0.018(4) 0.021(4) 0.031(5) 0.005(3) -0.001(4) 0.002(3) C17 0.028(5) 0.049(6) 0.043(6) 0.010(5) 0.007(5) -0.007(5) C18 0.054(7) 0.077(8) 0.030(5) 0.046(7) -0.010(5) -0.013(5) C19 0.066(8) 0.064(8) 0.042(6) 0.037(7) 0.023(6) 0.021(6) C20 0.050(7) 0.041(6) 0.040(6) 0.015(5) 0.011(5) 0.013(5) C21 0.035(5) 0.032(5) 0.034(5) 0.015(4) 0.011(4) 0.005(4) C22 0.039(6) 0.049(6) 0.025(5) 0.014(5) 0.004(4) 0.003(4) C23 0.059(7) 0.052(6) 0.026(5) 0.028(6) 0.007(5) 0.004(5) C24 0.051(7) 0.049(6) 0.044(6) 0.021(5) 0.018(5) 0.014(5) C25 0.039(6) 0.050(6) 0.049(7) 0.012(5) 0.014(5) 0.015(5) C26 0.035(5) 0.043(6) 0.030(5) 0.019(5) 0.004(4) -0.004(4) B1 0.025(5) 0.012(4) 0.017(4) 0.009(3) 0.007(4) 0.003(3) #============================================================================== _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' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl1 C17 1.780(10) yes . . F1 B1 1.408(10) yes . . F2 B1 1.409(9) yes . . N1 C1 1.364(11) yes . . N1 C4 1.406(10) yes . . N1 B1 1.522(10) yes . . N2 C6 1.412(9) yes . . N2 C9 1.331(10) yes . . N2 B1 1.576(12) yes . . C1 C2 1.401(9) yes . . C1 C11 1.499(12) yes . . C2 C3 1.393(13) yes . . C2 C12 1.525(13) yes . . C3 C4 1.418(10) yes . . C3 C14 1.514(10) yes . . C4 C5 1.393(12) yes . . C5 C6 1.368(10) yes . . C6 C7 1.457(12) yes . . C7 C8 1.442(9) yes . . C7 C10 1.383(12) yes . . C8 C9 1.446(12) yes . . C8 C10 1.385(11) yes . 2_565 C9 C16 1.500(10) yes . . C12 C13 1.508(14) yes . . C14 C15 1.488(13) yes . . C17 C18 1.397(17) yes . . C17 C26 1.421(14) yes . . C18 C19 1.336(15) yes . . C19 C20 1.357(15) yes . . C20 C21 1.419(15) yes . . C21 C22 1.426(13) yes . . C21 C26 1.392(12) yes . . C22 C23 1.356(15) yes . . C23 C24 1.403(14) yes . . C24 C25 1.378(16) yes . . C25 C26 1.440(16) yes . . C5 H5 0.950 no . . C10 H10 0.950 no . . C11 H11A 0.980 no . . C11 H11B 0.980 no . . C11 H11C 0.980 no . . C12 H12A 0.990 no . . C12 H12B 0.990 no . . C13 H13A 0.980 no . . C13 H13B 0.980 no . . C13 H13C 0.980 no . . C14 H14A 0.990 no . . C14 H14B 0.990 no . . C15 H15A 0.980 no . . C15 H15B 0.980 no . . C15 H15C 0.980 no . . C16 H16A 0.980 no . . C16 H16B 0.980 no . . C16 H16C 0.980 no . . C18 H18 0.950 no . . C19 H19 0.950 no . . C20 H20 0.950 no . . C22 H22 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . C25 H25 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C1 N1 C4 107.2(6) yes . . . C1 N1 B1 127.7(7) yes . . . C4 N1 B1 125.0(7) yes . . . C6 N2 C9 110.3(7) yes . . . C6 N2 B1 123.3(6) yes . . . C9 N2 B1 126.4(6) yes . . . N1 C1 C2 109.9(7) yes . . . N1 C1 C11 121.3(6) yes . . . C2 C1 C11 128.8(8) yes . . . C1 C2 C3 107.7(7) yes . . . C1 C2 C12 125.1(8) yes . . . C3 C2 C12 127.2(7) yes . . . C2 C3 C4 106.9(6) yes . . . C2 C3 C14 128.6(7) yes . . . C4 C3 C14 124.5(8) yes . . . N1 C4 C3 108.3(7) yes . . . N1 C4 C5 120.5(6) yes . . . C3 C4 C5 131.2(7) yes . . . C4 C5 C6 122.0(7) yes . . . N2 C6 C5 121.2(8) yes . . . N2 C6 C7 107.1(6) yes . . . C5 C6 C7 131.8(7) yes . . . C6 C7 C8 106.4(7) yes . . . C6 C7 C10 131.9(6) yes . . . C8 C7 C10 121.7(8) yes . . . C7 C8 C9 106.0(7) yes . . . C7 C8 C10 122.5(7) yes . . 2_565 C9 C8 C10 131.5(6) yes . . 2_565 N2 C9 C8 110.2(6) yes . . . N2 C9 C16 123.2(8) yes . . . C8 C9 C16 126.6(7) yes . . . C7 C10 C8 115.8(6) yes . . 2_565 C2 C12 C13 114.1(8) yes . . . C3 C14 C15 114.9(8) yes . . . Cl1 C17 C18 118.6(8) yes . . . Cl1 C17 C26 117.2(8) yes . . . C18 C17 C26 124.3(9) yes . . . C17 C18 C19 116.3(10) yes . . . C18 C19 C20 123.0(12) yes . . . C19 C20 C21 121.6(9) yes . . . C20 C21 C22 122.1(8) yes . . . C20 C21 C26 118.2(9) yes . . . C22 C21 C26 119.7(9) yes . . . C21 C22 C23 120.7(9) yes . . . C22 C23 C24 120.6(9) yes . . . C23 C24 C25 120.2(11) yes . . . C24 C25 C26 120.2(9) yes . . . C17 C26 C21 116.5(9) yes . . . C17 C26 C25 124.9(9) yes . . . C21 C26 C25 118.5(9) yes . . . F1 B1 F2 109.4(6) yes . . . F1 B1 N1 111.6(7) yes . . . F1 B1 N2 108.0(7) yes . . . F2 B1 N1 111.8(7) yes . . . F2 B1 N2 108.0(7) yes . . . N1 B1 N2 107.9(6) yes . . . C4 C5 H5 119.013 no . . . C6 C5 H5 119.008 no . . . C7 C10 H10 122.094 no . . . C8 C10 H10 122.098 no 2_565 . . C1 C11 H11A 109.476 no . . . C1 C11 H11B 109.471 no . . . C1 C11 H11C 109.472 no . . . H11A C11 H11B 109.467 no . . . H11A C11 H11C 109.467 no . . . H11B C11 H11C 109.474 no . . . C2 C12 H12A 108.728 no . . . C2 C12 H12B 108.730 no . . . C13 C12 H12A 108.720 no . . . C13 C12 H12B 108.722 no . . . H12A C12 H12B 107.637 no . . . C12 C13 H13A 109.473 no . . . C12 C13 H13B 109.473 no . . . C12 C13 H13C 109.477 no . . . H13A C13 H13B 109.471 no . . . H13A C13 H13C 109.468 no . . . H13B C13 H13C 109.466 no . . . C3 C14 H14A 108.539 no . . . C3 C14 H14B 108.540 no . . . C15 C14 H14A 108.545 no . . . C15 C14 H14B 108.540 no . . . H14A C14 H14B 107.532 no . . . C14 C15 H15A 109.468 no . . . C14 C15 H15B 109.473 no . . . C14 C15 H15C 109.471 no . . . H15A C15 H15B 109.474 no . . . H15A C15 H15C 109.471 no . . . H15B C15 H15C 109.470 no . . . C9 C16 H16A 109.467 no . . . C9 C16 H16B 109.472 no . . . C9 C16 H16C 109.473 no . . . H16A C16 H16B 109.476 no . . . H16A C16 H16C 109.471 no . . . H16B C16 H16C 109.468 no . . . C17 C18 H18 121.830 no . . . C19 C18 H18 121.834 no . . . C18 C19 H19 118.497 no . . . C20 C19 H19 118.498 no . . . C19 C20 H20 119.187 no . . . C21 C20 H20 119.190 no . . . C21 C22 H22 119.625 no . . . C23 C22 H22 119.632 no . . . C22 C23 H23 119.713 no . . . C24 C23 H23 119.709 no . . . C23 C24 H24 119.920 no . . . C25 C24 H24 119.919 no . . . C24 C25 H25 119.878 no . . . C26 C25 H25 119.873 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C1 N1 C4 C3 -0.1(8) no . . . . C1 N1 C4 C5 -179.6(6) no . . . . C4 N1 C1 C2 0.7(8) no . . . . C4 N1 C1 C11 179.6(6) no . . . . C1 N1 B1 F1 -62.7(10) no . . . . C1 N1 B1 F2 60.2(10) no . . . . C1 N1 B1 N2 178.8(7) no . . . . B1 N1 C1 C2 178.4(7) no . . . . B1 N1 C1 C11 -2.6(12) no . . . . C4 N1 B1 F1 114.7(8) no . . . . C4 N1 B1 F2 -122.4(8) no . . . . C4 N1 B1 N2 -3.8(10) no . . . . B1 N1 C4 C3 -177.9(6) no . . . . B1 N1 C4 C5 2.6(11) no . . . . C6 N2 C9 C8 -0.1(9) no . . . . C6 N2 C9 C16 -179.3(6) no . . . . C9 N2 C6 C5 179.3(7) no . . . . C9 N2 C6 C7 -0.8(8) no . . . . C6 N2 B1 F1 -117.9(7) no . . . . C6 N2 B1 F2 123.9(7) no . . . . C6 N2 B1 N1 2.9(10) no . . . . B1 N2 C6 C5 -0.7(11) no . . . . B1 N2 C6 C7 179.2(6) no . . . . C9 N2 B1 F1 62.0(9) no . . . . C9 N2 B1 F2 -56.2(9) no . . . . C9 N2 B1 N1 -177.2(7) no . . . . B1 N2 C9 C8 180.0(6) no . . . . B1 N2 C9 C16 0.8(12) no . . . . N1 C1 C2 C3 -1.0(9) no . . . . N1 C1 C2 C12 -177.9(6) no . . . . C11 C1 C2 C3 -179.9(7) no . . . . C11 C1 C2 C12 3.2(13) no . . . . C1 C2 C3 C4 0.9(9) no . . . . C1 C2 C3 C14 179.0(7) no . . . . C1 C2 C12 C13 -90.8(9) no . . . . C3 C2 C12 C13 92.8(10) no . . . . C12 C2 C3 C4 177.8(7) no . . . . C12 C2 C3 C14 -4.2(13) no . . . . C2 C3 C4 N1 -0.6(9) no . . . . C2 C3 C4 C5 178.9(7) no . . . . C2 C3 C14 C15 -77.4(11) no . . . . C4 C3 C14 C15 100.3(9) no . . . . C14 C3 C4 N1 -178.7(7) no . . . . C14 C3 C4 C5 0.7(13) no . . . . N1 C4 C5 C6 0.2(11) no . . . . C3 C4 C5 C6 -179.2(7) no . . . . C4 C5 C6 N2 -1.0(12) no . . . . C4 C5 C6 C7 179.1(7) no . . . . N2 C6 C7 C8 1.3(8) no . . . . N2 C6 C7 C10 179.9(7) no . . . . C5 C6 C7 C8 -178.8(8) no . . . . C5 C6 C7 C10 -0.2(15) no . . . . C6 C7 C8 C9 -1.3(8) no . . . . C6 C7 C8 C10 178.8(6) no . . . 2_565 C6 C7 C10 C8 -178.4(7) no . . . 2_565 C8 C7 C10 C8 -0.1(11) no . . . 2_565 C10 C7 C8 C9 179.9(7) no . . . . C10 C7 C8 C10 0.1(12) no . . . 2_565 C7 C8 C9 N2 0.9(9) no . . . . C7 C8 C9 C16 -179.9(7) no . . . . C7 C8 C10 C7 -0.1(11) no . . 2_565 2_565 C9 C8 C10 C7 -179.9(7) no . . 2_565 2_565 C10 C8 C9 N2 -179.3(8) no 2_565 . . . C10 C8 C9 C16 -0.1(14) no 2_565 . . . Cl1 C17 C18 C19 -178.2(8) no . . . . Cl1 C17 C26 C21 177.8(7) no . . . . Cl1 C17 C26 C25 -3.2(15) no . . . . C18 C17 C26 C21 -2.5(17) no . . . . C18 C17 C26 C25 176.5(11) no . . . . C26 C17 C18 C19 2.1(19) no . . . . C17 C18 C19 C20 0(2) no . . . . C18 C19 C20 C21 -2(2) no . . . . C19 C20 C21 C22 -176.6(11) no . . . . C19 C20 C21 C26 1.4(17) no . . . . C20 C21 C22 C23 180.0(10) no . . . . C20 C21 C26 C17 0.6(15) no . . . . C20 C21 C26 C25 -178.4(9) no . . . . C22 C21 C26 C17 178.7(9) no . . . . C22 C21 C26 C25 -0.3(15) no . . . . C26 C21 C22 C23 2.0(16) no . . . . C21 C22 C23 C24 -2.6(18) no . . . . C22 C23 C24 C25 1.7(19) no . . . . C23 C24 C25 C26 -0.0(18) no . . . . C24 C25 C26 C17 -179.6(11) no . . . . C24 C25 C26 C21 -0.6(17) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl1 C25 3.085(12) no . . F1 C1 3.139(9) no . . F1 C4 3.523(8) no . . F1 C6 3.525(9) no . . F1 C9 3.072(10) no . . F1 C11 3.239(10) no . . F1 C16 3.170(10) no . . F2 C1 3.124(9) no . . F2 C4 3.575(8) no . . F2 C6 3.565(9) no . . F2 C9 3.032(10) no . . F2 C11 3.160(10) no . . F2 C16 3.066(10) no . . N1 C6 2.832(12) no . . N2 C4 2.837(9) no . . C1 C5 3.550(13) no . . C1 C13 3.455(13) no . . C2 C15 3.380(13) no . . C3 C13 3.490(16) no . . C4 C15 3.523(11) no . . C5 C9 3.539(9) no . . C5 C10 3.291(12) no . . C5 C14 3.198(11) no . . C5 B1 2.988(11) no . . C7 C7 2.761(12) no . 2_565 C8 C8 2.745(11) no . 2_565 C10 C10 2.913(9) no . 2_565 C10 C16 3.263(12) no . 2_565 C11 C12 3.219(10) no . . C11 B1 3.075(14) no . . C12 C14 3.260(14) no . . C16 B1 3.088(12) no . . C17 C20 2.697(13) no . . C18 C21 2.830(14) no . . C19 C26 2.789(16) no . . C21 C24 2.800(16) no . . C22 C25 2.786(14) no . . C23 C26 2.809(14) no . . F1 C5 3.407(9) no . 2_665 F1 C10 3.462(8) no . 2_665 F1 C11 3.575(9) no . 2_655 F1 C18 3.401(11) no . 1_554 F2 C11 3.229(9) no . 2_655 F2 C23 3.268(12) no . . F2 C24 3.528(12) no . . N1 C7 3.555(10) no . 2_665 N1 C10 3.520(10) no . 2_665 N1 C24 3.539(14) no . . N2 C5 3.455(10) no . 2_665 C1 C8 3.594(11) no . 1_655 C1 C10 3.387(11) no . 2_665 C2 C8 3.592(11) no . 1_655 C3 C7 3.522(11) no . 2_665 C3 C8 3.395(11) no . 2_665 C4 C6 3.424(11) no . 2_665 C4 C7 3.391(11) no . 2_665 C5 F1 3.407(9) no . 2_665 C5 N2 3.455(10) no . 2_665 C5 C5 3.596(11) no . 2_665 C5 C6 3.373(11) no . 2_665 C6 C4 3.424(11) no . 2_665 C6 C5 3.373(11) no . 2_665 C7 N1 3.555(10) no . 2_665 C7 C3 3.522(11) no . 2_665 C7 C4 3.391(11) no . 2_665 C7 C12 3.459(12) no . 1_455 C8 C1 3.594(11) no . 1_455 C8 C2 3.592(11) no . 1_455 C8 C3 3.395(11) no . 2_665 C8 C14 3.578(12) no . 2_665 C9 C14 3.583(12) no . 2_665 C10 F1 3.462(8) no . 2_665 C10 N1 3.520(10) no . 2_665 C10 C1 3.387(11) no . 2_665 C11 F1 3.575(9) no . 2_655 C11 F2 3.229(9) no . 2_655 C12 C7 3.459(12) no . 1_655 C14 C8 3.578(12) no . 2_665 C14 C9 3.583(12) no . 2_665 C15 C17 3.582(18) no . 2_666 C17 C15 3.582(18) no . 2_666 C17 C21 3.556(16) no . 2_656 C18 F1 3.401(11) no . 1_556 C20 C26 3.571(17) no . 2_656 C21 C17 3.556(16) no . 2_656 C23 F2 3.268(12) no . . C24 F2 3.528(12) no . . C24 N1 3.539(14) no . . C26 C20 3.571(17) no . 2_656 Cl1 H18 2.8510 no . . Cl1 H25 2.6941 no . . F1 H11A 3.4523 no . . F1 H11C 2.6857 no . . F1 H16A 2.5965 no . . F1 H16C 3.4252 no . . F2 H11A 2.7324 no . . F2 H11C 3.1737 no . . F2 H16A 3.0653 no . . F2 H16C 2.6634 no . . N1 H5 3.2808 no . . N1 H11A 2.7758 no . . N1 H11B 3.2835 no . . N1 H11C 2.7229 no . . N2 H5 3.2726 no . . N2 H16A 2.7153 no . . N2 H16B 3.2659 no . . N2 H16C 2.7994 no . . C1 H12A 2.7130 no . . C1 H12B 3.3204 no . . C1 H13C 3.3124 no . . C2 H11A 3.1910 no . . C2 H11B 2.7102 no . . C2 H11C 3.2454 no . . C2 H13A 2.7084 no . . C2 H13B 3.3756 no . . C2 H13C 2.7880 no . . C2 H14A 2.8073 no . . C2 H14B 3.3579 no . . C2 H15C 3.2200 no . . C3 H5 2.7975 no . . C3 H12A 3.3221 no . . C3 H12B 2.7376 no . . C3 H13A 3.2898 no . . C3 H15A 2.6962 no . . C3 H15B 3.3584 no . . C3 H15C 2.7772 no . . C4 H14A 3.2868 no . . C4 H14B 2.6701 no . . C4 H15A 3.3478 no . . C5 H10 3.1662 no . . C5 H14B 2.8356 no . . C6 H10 2.8740 no . . C7 H5 2.8108 no . . C7 H10 3.3439 no . 2_565 C8 H10 3.3359 no . . C8 H16A 3.2806 no . . C8 H16B 2.7033 no . . C8 H16C 3.1968 no . . C9 H10 2.8621 no . 2_565 C10 H5 3.1076 no . . C10 H16B 2.8918 no . 2_565 C11 H12A 2.9072 no . . C11 H13C 3.4153 no . . C12 H11B 2.8077 no . . C12 H14A 3.0517 no . . C12 H15C 3.2424 no . . C13 H11B 3.3714 no . . C13 H15C 3.0591 no . . C14 H5 2.9531 no . . C14 H12B 2.9534 no . . C14 H13A 3.4887 no . . C15 H12B 3.5211 no . . C15 H13A 3.0922 no . . C16 H10 3.0819 no . 2_565 C17 H19 3.1867 no . . C17 H25 2.7476 no . . C18 H20 3.2079 no . . C20 H18 3.2278 no . . C20 H22 2.6768 no . . C21 H19 3.2711 no . . C21 H23 3.2768 no . . C21 H25 3.2916 no . . C22 H20 2.6685 no . . C22 H24 3.2487 no . . C23 H25 3.2687 no . . C24 H22 3.2536 no . . C25 H23 3.2640 no . . C26 H18 3.3466 no . . C26 H20 3.2677 no . . C26 H22 3.2893 no . . C26 H24 3.3045 no . . B1 H11A 3.0879 no . . B1 H11C 2.9516 no . . B1 H16A 2.9425 no . . B1 H16C 3.1289 no . . H5 H10 2.7160 no . . H5 H14B 2.3488 no . . H5 H15A 3.3713 no . . H10 H16B 2.4561 no . 2_565 H11A H13C 3.5312 no . . H11B H12A 2.2832 no . . H11B H13C 2.9108 no . . H11C H12A 3.4765 no . . H12A H13A 2.8451 no . . H12A H13B 2.3684 no . . H12A H13C 2.3228 no . . H12B H13A 2.3863 no . . H12B H13B 2.3065 no . . H12B H13C 2.8435 no . . H12B H14A 2.4692 no . . H12B H15C 3.0459 no . . H13A H14A 3.5457 no . . H13A H15A 3.4083 no . . H13A H15C 2.2378 no . . H13B H15C 3.5555 no . . H14A H15A 2.8283 no . . H14A H15B 2.3476 no . . H14A H15C 2.3017 no . . H14B H15A 2.3674 no . . H14B H15B 2.2834 no . . H14B H15C 2.8265 no . . H18 H19 2.2902 no . . H19 H20 2.2736 no . . H20 H22 2.5066 no . . H22 H23 2.2973 no . . H23 H24 2.3479 no . . H24 H25 2.3253 no . . Cl1 H5 3.2046 no . 2_666 Cl1 H10 3.4045 no . 2_666 Cl1 H12B 2.7401 no . 2_766 Cl1 H14A 2.9501 no . 2_766 Cl1 H15A 3.3693 no . 2_666 Cl1 H15C 3.5571 no . 2_766 F1 H5 2.7530 no . 2_665 F1 H10 2.8249 no . 2_665 F1 H11A 2.9062 no . 2_655 F1 H11C 3.5838 no . 2_655 F1 H14B 3.5513 no . 2_665 F1 H18 2.5390 no . 1_554 F2 H11A 3.1687 no . 2_655 F2 H11B 3.3490 no . 2_655 F2 H11C 2.6696 no . 2_655 F2 H16B 3.4489 no . 2_555 F2 H16C 2.9911 no . 2_555 F2 H23 2.5260 no . . F2 H24 3.0638 no . . N1 H10 3.5073 no . 2_665 N1 H24 2.6428 no . . N2 H5 3.3251 no . 2_665 N2 H12A 3.1602 no . 1_455 N2 H14B 3.5784 no . 2_665 C1 H10 3.4993 no . 2_665 C1 H24 2.8376 no . . C2 H24 3.1555 no . . C3 H24 3.1835 no . . C4 H24 2.8600 no . . C5 H12B 3.5360 no . 1_455 C5 H24 3.5505 no . . C6 H12A 3.0594 no . 1_455 C6 H12B 3.2360 no . 1_455 C7 H12A 3.1576 no . 1_455 C7 H12B 3.0963 no . 1_455 C8 H11C 3.5390 no . 1_455 C8 H12A 3.2843 no . 1_455 C8 H14A 3.2152 no . 2_665 C8 H14B 3.4853 no . 2_665 C9 H11B 3.4947 no . 1_455 C9 H11C 3.4925 no . 1_455 C9 H12A 3.2851 no . 1_455 C9 H14A 3.3833 no . 2_665 C9 H14B 3.1017 no . 2_665 C10 H11C 3.3783 no . 2_665 C10 H12B 3.2440 no . 1_455 C10 H14A 3.1134 no . 1_455 C11 H16A 3.5637 no . 2_655 C11 H16C 3.3214 no . 1_655 C11 H19 3.2577 no . 2_656 C11 H24 3.5916 no . . C13 H15B 3.4339 no . 2_766 C13 H15C 3.2250 no . 2_766 C13 H19 3.2109 no . 2_656 C13 H20 3.2731 no . 2_656 C13 H25 3.4510 no . . C14 H16A 3.5329 no . 2_665 C15 H13A 3.5259 no . 2_766 C15 H13B 3.1448 no . 2_766 C15 H25 3.5602 no . . C16 H11B 3.5288 no . 1_455 C16 H11B 3.4530 no . 2_655 C16 H11C 3.1980 no . 1_455 C16 H14A 3.4621 no . 2_665 C16 H14B 3.1956 no . 2_665 C16 H16C 3.4864 no . 2_555 C16 H22 3.4041 no . 2_555 C16 H23 3.0184 no . 2_555 C17 H14B 3.5025 no . 2_666 C17 H15A 3.1729 no . 2_666 C17 H15B 3.2071 no . 2_666 C18 H5 3.4970 no . 2_666 C18 H14B 3.2226 no . 2_666 C18 H15B 3.5339 no . 2_666 C18 H16A 3.5543 no . 1_556 C19 H11A 3.5284 no . 2_656 C19 H13C 2.9189 no . 2_656 C19 H16A 3.4287 no . 1_556 C19 H22 3.2599 no . 2_556 C20 H13C 3.0860 no . 2_656 C20 H15B 3.5050 no . 2_666 C20 H20 3.3851 no . 2_556 C20 H22 3.1974 no . 2_556 C21 H15B 3.1936 no . 2_666 C21 H20 3.3772 no . 2_556 C22 H16B 3.3100 no . 2_555 C22 H20 3.2357 no . 2_556 C23 H13B 3.2393 no . 1_455 C23 H13C 3.5028 no . 1_455 C23 H16B 3.1691 no . 2_555 C24 H11A 3.5904 no . . C24 H13B 3.1561 no . 1_455 C25 H13A 3.5181 no . . C25 H13B 3.5192 no . 1_455 C25 H15A 3.4561 no . 2_666 C25 H15B 3.5848 no . 2_666 C26 H15A 3.2727 no . 2_666 C26 H15B 3.0265 no . 2_666 B1 H5 3.4768 no . 2_665 B1 H24 3.3175 no . . H5 Cl1 3.2046 no . 2_666 H5 F1 2.7530 no . 2_665 H5 N2 3.3251 no . 2_665 H5 C18 3.4970 no . 2_666 H5 B1 3.4768 no . 2_665 H5 H12B 3.5482 no . 1_455 H5 H18 3.0075 no . 2_666 H10 Cl1 3.4045 no . 2_666 H10 F1 2.8249 no . 2_665 H10 N1 3.5073 no . 2_665 H10 C1 3.4993 no . 2_665 H10 H11C 3.0405 no . 2_665 H10 H12B 3.3416 no . 1_455 H10 H14A 3.0034 no . 1_455 H10 H18 3.1322 no . 2_666 H11A F1 2.9062 no . 2_655 H11A F2 3.1687 no . 2_655 H11A C19 3.5284 no . 2_656 H11A C24 3.5904 no . . H11A H11C 3.3116 no . 2_655 H11A H16A 3.3560 no . 2_655 H11A H18 3.1587 no . 2_656 H11A H19 2.8044 no . 2_656 H11A H24 3.2385 no . . H11B F2 3.3490 no . 2_655 H11B C9 3.4947 no . 1_655 H11B C16 3.5288 no . 1_655 H11B C16 3.4530 no . 2_655 H11B H16A 3.0054 no . 2_655 H11B H16C 2.9245 no . 1_655 H11B H16C 3.0041 no . 2_655 H11B H19 2.9123 no . 2_656 H11B H23 3.5060 no . 1_655 H11C F1 3.5838 no . 2_655 H11C F2 2.6696 no . 2_655 H11C C8 3.5390 no . 1_655 H11C C9 3.4925 no . 1_655 H11C C10 3.3783 no . 2_665 H11C C16 3.1980 no . 1_655 H11C H10 3.0405 no . 2_665 H11C H11A 3.3116 no . 2_655 H11C H16B 2.9431 no . 1_655 H11C H16C 2.8182 no . 1_655 H11C H16C 3.5806 no . 2_655 H12A N2 3.1602 no . 1_655 H12A C6 3.0594 no . 1_655 H12A C7 3.1576 no . 1_655 H12A C8 3.2843 no . 1_655 H12A C9 3.2851 no . 1_655 H12A H23 3.2786 no . 1_655 H12A H24 3.5714 no . 1_655 H12B Cl1 2.7401 no . 2_766 H12B C5 3.5360 no . 1_655 H12B C6 3.2360 no . 1_655 H12B C7 3.0963 no . 1_655 H12B C10 3.2440 no . 1_655 H12B H5 3.5482 no . 1_655 H12B H10 3.3416 no . 1_655 H13A C15 3.5259 no . 2_766 H13A C25 3.5181 no . . H13A H13A 3.4246 no . 2_766 H13A H15B 3.3915 no . 2_766 H13A H15C 2.8138 no . 2_766 H13A H20 3.4330 no . 2_656 H13A H25 2.7770 no . . H13B C15 3.1448 no . 2_766 H13B C23 3.2393 no . 1_655 H13B C24 3.1561 no . 1_655 H13B C25 3.5192 no . 1_655 H13B H15A 3.2971 no . 2_766 H13B H15B 2.8490 no . 2_766 H13B H15C 2.7861 no . 2_766 H13B H20 3.3348 no . 2_656 H13B H23 3.5371 no . 1_655 H13B H24 3.3877 no . 1_655 H13C C19 2.9189 no . 2_656 H13C C20 3.0860 no . 2_656 H13C C23 3.5028 no . 1_655 H13C H15B 3.5395 no . 2_766 H13C H19 2.2323 no . 2_656 H13C H20 2.5836 no . 2_656 H13C H23 3.5355 no . 1_655 H13C H25 3.2687 no . . H14A Cl1 2.9501 no . 2_766 H14A C8 3.2152 no . 2_665 H14A C9 3.3833 no . 2_665 H14A C10 3.1134 no . 1_655 H14A C16 3.4621 no . 2_665 H14A H10 3.0034 no . 1_655 H14A H16A 3.3997 no . 2_665 H14A H16B 3.0826 no . 2_665 H14A H22 3.3434 no . 1_665 H14B F1 3.5513 no . 2_665 H14B N2 3.5784 no . 2_665 H14B C8 3.4853 no . 2_665 H14B C9 3.1017 no . 2_665 H14B C16 3.1956 no . 2_665 H14B C17 3.5025 no . 2_666 H14B C18 3.2226 no . 2_666 H14B H16A 2.7638 no . 2_665 H14B H16B 3.2500 no . 2_665 H14B H18 3.2223 no . 2_666 H14B H22 3.5814 no . 1_665 H15A Cl1 3.3693 no . 2_666 H15A C17 3.1729 no . 2_666 H15A C25 3.4561 no . 2_666 H15A C26 3.2727 no . 2_666 H15A H13B 3.2971 no . 2_766 H15A H24 3.5761 no . . H15A H25 3.0582 no . . H15A H25 3.4283 no . 2_666 H15B C13 3.4339 no . 2_766 H15B C17 3.2071 no . 2_666 H15B C18 3.5339 no . 2_666 H15B C20 3.5050 no . 2_666 H15B C21 3.1936 no . 2_666 H15B C25 3.5848 no . 2_666 H15B C26 3.0265 no . 2_666 H15B H13A 3.3915 no . 2_766 H15B H13B 2.8490 no . 2_766 H15B H13C 3.5395 no . 2_766 H15B H20 2.8556 no . 1_665 H15B H22 3.2971 no . 1_665 H15C Cl1 3.5571 no . 2_766 H15C C13 3.2250 no . 2_766 H15C H13A 2.8138 no . 2_766 H15C H13B 2.7861 no . 2_766 H15C H25 3.1752 no . . H16A C11 3.5637 no . 2_655 H16A C14 3.5329 no . 2_665 H16A C18 3.5543 no . 1_554 H16A C19 3.4287 no . 1_554 H16A H11A 3.3560 no . 2_655 H16A H11B 3.0054 no . 2_655 H16A H14A 3.3997 no . 2_665 H16A H14B 2.7638 no . 2_665 H16A H18 3.2620 no . 1_554 H16A H19 2.9881 no . 1_554 H16A H22 3.0962 no . 2_555 H16A H23 3.0984 no . 2_555 H16B F2 3.4489 no . 2_555 H16B C22 3.3100 no . 2_555 H16B C23 3.1691 no . 2_555 H16B H11C 2.9431 no . 1_455 H16B H14A 3.0826 no . 2_665 H16B H14B 3.2500 no . 2_665 H16B H22 2.8225 no . 2_555 H16B H23 2.5187 no . 2_555 H16C F2 2.9911 no . 2_555 H16C C11 3.3214 no . 1_455 H16C C16 3.4864 no . 2_555 H16C H11B 2.9245 no . 1_455 H16C H11B 3.0041 no . 2_655 H16C H11C 2.8182 no . 1_455 H16C H11C 3.5806 no . 2_655 H16C H16C 2.5135 no . 2_555 H16C H23 2.9538 no . 2_555 H18 F1 2.5390 no . 1_556 H18 H5 3.0075 no . 2_666 H18 H10 3.1322 no . 2_666 H18 H11A 3.1587 no . 2_656 H18 H14B 3.2223 no . 2_666 H18 H16A 3.2620 no . 1_556 H19 C11 3.2577 no . 2_656 H19 C13 3.2109 no . 2_656 H19 H11A 2.8044 no . 2_656 H19 H11B 2.9123 no . 2_656 H19 H13C 2.2323 no . 2_656 H19 H16A 2.9881 no . 1_556 H19 H22 3.1306 no . 2_556 H20 C13 3.2731 no . 2_656 H20 C20 3.3851 no . 2_556 H20 C21 3.3772 no . 2_556 H20 C22 3.2357 no . 2_556 H20 H13A 3.4330 no . 2_656 H20 H13B 3.3348 no . 2_656 H20 H13C 2.5836 no . 2_656 H20 H15B 2.8556 no . 1_445 H20 H20 3.2502 no . 2_556 H20 H22 3.0508 no . 2_556 H22 C16 3.4041 no . 2_555 H22 C19 3.2599 no . 2_556 H22 C20 3.1974 no . 2_556 H22 H14A 3.3434 no . 1_445 H22 H14B 3.5814 no . 1_445 H22 H15B 3.2971 no . 1_445 H22 H16A 3.0962 no . 2_555 H22 H16B 2.8225 no . 2_555 H22 H19 3.1306 no . 2_556 H22 H20 3.0508 no . 2_556 H23 F2 2.5260 no . . H23 C16 3.0184 no . 2_555 H23 H11B 3.5060 no . 1_455 H23 H12A 3.2786 no . 1_455 H23 H13B 3.5371 no . 1_455 H23 H13C 3.5355 no . 1_455 H23 H16A 3.0984 no . 2_555 H23 H16B 2.5187 no . 2_555 H23 H16C 2.9538 no . 2_555 H24 F2 3.0638 no . . H24 N1 2.6428 no . . H24 C1 2.8376 no . . H24 C2 3.1555 no . . H24 C3 3.1835 no . . H24 C4 2.8600 no . . H24 C5 3.5505 no . . H24 C11 3.5916 no . . H24 B1 3.3175 no . . H24 H11A 3.2385 no . . H24 H12A 3.5714 no . 1_455 H24 H13B 3.3877 no . 1_455 H24 H15A 3.5761 no . . H25 C13 3.4510 no . . H25 C15 3.5602 no . . H25 H13A 2.7770 no . . H25 H13C 3.2687 no . . H25 H15A 3.0582 no . . H25 H15A 3.4283 no . 2_666 H25 H15C 3.1752 no . . data_20111001_2 _database_code_depnum_ccdc_archive 'CCDC 864650' #TrackingRef '9289_web_deposit_cif_file_5_HidemitsuUno_1327633261.20111001Takahashi.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C60 H62 B2 Cl6 F4 N4' _chemical_formula_moiety 'C58 H60 B2 F4 N4, 2(C H Cl3)' _chemical_formula_weight 1149.51 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' #------------------------------------------------------------------------------ _cell_length_a 11.3126(2) _cell_length_b 29.2235(6) _cell_length_c 17.1103(3) _cell_angle_alpha 90.0000 _cell_angle_beta 92.3136(11) _cell_angle_gamma 90.0000 _cell_volume 5651.93(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 41186 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 68.26 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392.00 _exptl_absorpt_coefficient_mu 3.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 0.724 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_source 'VariMax Rotating Anode, 40 kV x 30 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 65588 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_theta_max 68.25 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 #============================================================================== # REFINEMENT DATA _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. Bicyclo[2.2.2]octadiene moieties and one of the solvent chloroform molecules disorder. Atomic coordinates of the disordered groups and molecules are restrained. ; _reflns_number_total 10206 _reflns_number_gt 7145 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1916 _refine_ls_wR_factor_gt 0.1806 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_number_restraints 867 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 10189 _refine_ls_number_parameters 870 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0786P)^2^+3.5600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_diff_density_max 0.420 _refine_diff_density_min -0.730 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.0090 0.0039 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0311 0.0180 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0727 0.0534 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.3639 0.7018 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl4 Cl 0.6390(7) 0.2027(4) 0.5484(6) 0.0450(15) Uani 0.246(4) 1 d PDU A 1 Cl5 Cl 0.4609(11) 0.2303(5) 0.4421(8) 0.129(4) Uani 0.246(4) 1 d PDU A 1 Cl6 Cl 0.5445(8) 0.1453(4) 0.4042(6) 0.112(3) Uani 0.246(4) 1 d PDU A 1 C60 C 0.524(3) 0.1816(8) 0.4863(14) 0.099(4) Uani 0.246(4) 1 d PDU A 1 H60 H 0.4630 0.1672 0.5195 0.119 Uiso 0.246(4) 1 calc PR A 1 Cl4A Cl 0.6136(5) 0.2011(2) 0.5515(4) 0.110(2) Uani 0.624(5) 1 d PDU B 2 Cl5A Cl 0.4485(3) 0.20982(12) 0.41528(18) 0.0826(9) Uani 0.624(5) 1 d PDU B 2 Cl6A Cl 0.5842(3) 0.12988(10) 0.43432(14) 0.0796(9) Uani 0.624(5) 1 d PDU B 2 C60A C 0.5145(10) 0.1734(3) 0.4866(6) 0.077(2) Uani 0.624(5) 1 d PDU B 2 H60A H 0.4506 0.1592 0.5172 0.093 Uiso 0.624(5) 1 calc PR B 2 Cl4B Cl 0.4987(14) 0.2081(5) 0.5423(10) 0.118(4) Uani 0.130(3) 1 d PDU C 3 Cl5B Cl 0.525(3) 0.2313(9) 0.3798(14) 0.214(8) Uani 0.130(3) 1 d PDU C 3 Cl6B Cl 0.6453(15) 0.1541(7) 0.4538(10) 0.130(5) Uani 0.130(3) 1 d PDU C 3 C60B C 0.512(3) 0.1866(11) 0.4455(14) 0.113(5) Uani 0.130(3) 1 d PDU C 3 H60B H 0.4429 0.1666 0.4301 0.135 Uiso 0.130(3) 1 calc PR C 3 F1 F 0.33077(17) 0.45700(6) 0.30731(10) 0.0405(4) Uani 1 1 d . D . F2 F 0.16042(17) 0.49692(6) 0.28798(10) 0.0426(5) Uani 1 1 d . D . F3 F 0.42875(16) 0.27323(6) 0.68132(12) 0.0417(4) Uani 1 1 d . E . F4 F 0.29750(17) 0.26391(6) 0.77605(10) 0.0382(4) Uani 1 1 d . E . N1 N 0.1882(2) 0.45554(8) 0.40914(14) 0.0316(6) Uani 1 1 d . D . N2 N 0.3055(2) 0.52606(9) 0.38340(15) 0.0338(6) Uani 1 1 d . D . N3 N 0.2305(2) 0.30233(8) 0.65777(14) 0.0297(5) Uani 1 1 d . E . N4 N 0.2708(2) 0.21871(8) 0.65863(14) 0.0316(6) Uani 1 1 d . E . C1 C 0.1297(3) 0.41502(10) 0.40017(18) 0.0324(7) Uani 1 1 d . . . C2 C 0.0974(3) 0.39942(10) 0.47350(17) 0.0314(6) Uani 1 1 d . . . C3 C 0.1378(3) 0.43077(10) 0.52910(17) 0.0315(6) Uani 1 1 d . . . C4 C 0.1950(3) 0.46614(10) 0.48914(17) 0.0303(6) Uani 1 1 d . . . C5 C 0.2569(3) 0.50486(10) 0.51600(18) 0.0315(6) Uani 1 1 d . . . C6 C 0.3100(3) 0.53431(10) 0.46433(18) 0.0326(7) Uani 1 1 d . D . C7 C 0.3703(3) 0.57681(11) 0.47673(19) 0.0374(7) Uani 1 1 d D . . C8 C 0.4009(3) 0.59249(11) 0.4047(2) 0.0389(7) Uani 1 1 d D D . C9 C 0.3606(3) 0.56131(11) 0.3473(2) 0.0392(7) Uani 1 1 d . . . C10 C 0.1071(3) 0.39264(11) 0.32268(18) 0.0394(7) Uani 1 1 d . . . H10A H 0.0469 0.4100 0.2924 0.059 Uiso 1 1 calc R . . H10B H 0.0791 0.3613 0.3305 0.059 Uiso 1 1 calc R . . H10C H 0.1806 0.3919 0.2942 0.059 Uiso 1 1 calc R . . C11 C 0.2678(3) 0.51482(10) 0.60082(18) 0.0330(7) Uani 1 1 d . . . C12 C 0.1737(3) 0.53176(11) 0.64185(19) 0.0382(7) Uani 1 1 d . . . H12 H 0.0980 0.5351 0.6163 0.046 Uiso 1 1 calc R . . C13 C 0.1900(3) 0.54381(12) 0.71993(19) 0.0411(8) Uani 1 1 d . . . H13 H 0.1250 0.5558 0.7469 0.049 Uiso 1 1 calc R . . C14 C 0.2993(3) 0.53884(11) 0.7601(2) 0.0401(7) Uani 1 1 d . . . C15 C 0.3906(3) 0.52074(13) 0.7184(2) 0.0453(8) Uani 1 1 d . . . H15 H 0.4655 0.5161 0.7443 0.054 Uiso 1 1 calc R . . C16 C 0.3765(3) 0.50908(12) 0.6398(2) 0.0438(8) Uani 1 1 d . . . H16 H 0.4415 0.4972 0.6128 0.053 Uiso 1 1 calc R . . C17 C 0.3242(4) 0.55503(14) 0.8443(2) 0.0505(9) Uani 1 1 d . . . C18 C 0.4183(4) 0.59353(16) 0.8433(3) 0.0672(12) Uani 1 1 d . . . H18A H 0.4894 0.5821 0.8187 0.101 Uiso 1 1 calc R . . H18B H 0.4388 0.6031 0.8970 0.101 Uiso 1 1 calc R . . H18C H 0.3864 0.6197 0.8134 0.101 Uiso 1 1 calc R . . C19 C 0.3712(4) 0.51608(16) 0.8947(2) 0.0664(12) Uani 1 1 d . . . H19A H 0.3128 0.4913 0.8946 0.100 Uiso 1 1 calc R . . H19B H 0.3862 0.5270 0.9484 0.100 Uiso 1 1 calc R . . H19C H 0.4451 0.5047 0.8739 0.100 Uiso 1 1 calc R . . C20 C 0.2157(4) 0.57595(16) 0.8803(2) 0.0643(11) Uani 1 1 d . . . H20A H 0.1890 0.6024 0.8492 0.096 Uiso 1 1 calc R . . H20B H 0.2361 0.5857 0.9339 0.096 Uiso 1 1 calc R . . H20C H 0.1523 0.5531 0.8809 0.096 Uiso 1 1 calc R . . C21A C 0.4193(19) 0.6052(5) 0.5441(8) 0.041(3) Uani 0.422(17) 1 d PDU D 1 H21A H 0.4039 0.5909 0.5958 0.049 Uiso 0.422(17) 1 calc PR D 1 C22A C 0.551(2) 0.6157(9) 0.5354(15) 0.045(3) Uani 0.422(17) 1 d PDU D 1 H22 H 0.6088 0.6116 0.5764 0.054 Uiso 0.422(17) 1 calc PR D 1 C23A C 0.578(2) 0.6327(8) 0.4575(14) 0.047(3) Uani 0.422(17) 1 d PDU D 1 H23 H 0.6551 0.6410 0.4419 0.056 Uiso 0.422(17) 1 calc PR D 1 C24A C 0.476(2) 0.6350(6) 0.4099(11) 0.041(3) Uani 0.422(17) 1 d PDU D 1 H24A H 0.4924 0.6473 0.3568 0.049 Uiso 0.422(17) 1 calc PR D 1 C25A C 0.3837(18) 0.6701(8) 0.4588(11) 0.036(3) Uani 0.422(17) 1 d PDU D 1 H25A H 0.4198 0.7009 0.4629 0.044 Uiso 0.422(17) 1 calc PR D 1 H25B H 0.3082 0.6730 0.4279 0.044 Uiso 0.422(17) 1 calc PR D 1 C26A C 0.359(2) 0.6546(9) 0.5350(11) 0.047(3) Uani 0.422(17) 1 d PDU D 1 H26A H 0.2725 0.6524 0.5411 0.057 Uiso 0.422(17) 1 calc PR D 1 H26B H 0.3924 0.6759 0.5750 0.057 Uiso 0.422(17) 1 calc PR D 1 C21 C 0.4009(14) 0.6089(4) 0.5424(6) 0.040(2) Uani 0.578(17) 1 d PDU D 2 H21 H 0.3701 0.5993 0.5938 0.048 Uiso 0.578(17) 1 calc PR D 2 C22 C 0.5417(15) 0.6094(6) 0.5401(10) 0.039(2) Uani 0.578(17) 1 d PDU D 2 H22A H 0.5748 0.6299 0.5816 0.047 Uiso 0.578(17) 1 calc PR D 2 H22B H 0.5729 0.5782 0.5500 0.047 Uiso 0.578(17) 1 calc PR D 2 C23 C 0.5765(15) 0.6250(6) 0.4655(10) 0.048(3) Uani 0.578(17) 1 d PDU D 2 H23A H 0.6245 0.6009 0.4413 0.058 Uiso 0.578(17) 1 calc PR D 2 H23B H 0.6273 0.6524 0.4730 0.058 Uiso 0.578(17) 1 calc PR D 2 C24 C 0.4615(18) 0.6385(5) 0.4030(8) 0.044(3) Uani 0.578(17) 1 d PDU D 2 H24 H 0.4857 0.6480 0.3498 0.053 Uiso 0.578(17) 1 calc PR D 2 C25 C 0.3991(14) 0.6720(6) 0.4424(8) 0.039(2) Uani 0.578(17) 1 d PDU D 2 H25 H 0.3835 0.7017 0.4223 0.046 Uiso 0.578(17) 1 calc PR D 2 C26 C 0.3617(16) 0.6563(6) 0.5164(8) 0.042(2) Uani 0.578(17) 1 d PDU D 2 H26 H 0.3141 0.6749 0.5481 0.051 Uiso 0.578(17) 1 calc PR D 2 C27 C 0.3745(3) 0.56430(13) 0.2614(2) 0.0491(9) Uani 1 1 d . D . H27A H 0.3508 0.5352 0.2369 0.074 Uiso 1 1 calc R . . H27B H 0.4574 0.5707 0.2509 0.074 Uiso 1 1 calc R . . H27C H 0.3245 0.5890 0.2398 0.074 Uiso 1 1 calc R . . C28 C 0.2227(3) 0.34700(10) 0.67968(17) 0.0316(6) Uani 1 1 d . . . C29 C 0.1500(3) 0.36998(10) 0.62453(17) 0.0311(6) Uani 1 1 d . . . C30 C 0.1116(3) 0.33903(10) 0.56797(17) 0.0301(6) Uani 1 1 d . . . C31 C 0.1617(3) 0.29624(10) 0.58864(16) 0.0291(6) Uani 1 1 d . . . C32 C 0.1496(3) 0.25329(10) 0.55319(17) 0.0312(6) Uani 1 1 d . . . C33 C 0.2036(3) 0.21477(11) 0.58829(17) 0.0340(7) Uani 1 1 d . E . C34 C 0.1983(3) 0.16806(11) 0.56889(19) 0.0391(7) Uani 1 1 d D . . C35 C 0.2574(3) 0.14439(10) 0.62819(18) 0.0382(7) Uani 1 1 d D E . C36 C 0.3029(3) 0.17611(11) 0.68282(18) 0.0349(7) Uani 1 1 d . . . C37 C 0.2846(3) 0.36572(11) 0.75142(18) 0.0380(7) Uani 1 1 d . . . H37A H 0.2407 0.3572 0.7975 0.057 Uiso 1 1 calc R . . H37B H 0.2887 0.3991 0.7476 0.057 Uiso 1 1 calc R . . H37C H 0.3648 0.3531 0.7563 0.057 Uiso 1 1 calc R . . C38 C 0.0732(3) 0.24905(10) 0.48038(17) 0.0321(6) Uani 1 1 d . . . C39 C 0.1192(3) 0.25638(13) 0.40742(19) 0.0434(8) Uani 1 1 d . . . H39 H 0.2019 0.2611 0.4034 0.052 Uiso 1 1 calc R . . C40 C 0.0465(3) 0.25695(13) 0.34081(19) 0.0444(8) Uani 1 1 d . . . H40 H 0.0805 0.2620 0.2917 0.053 Uiso 1 1 calc R . . C41 C -0.0746(3) 0.25043(11) 0.34328(18) 0.0387(7) Uani 1 1 d . . . C42 C -0.1188(3) 0.24138(12) 0.4158(2) 0.0436(8) Uani 1 1 d . . . H42 H -0.2009 0.2355 0.4196 0.052 Uiso 1 1 calc R . . C43 C -0.0458(3) 0.24067(12) 0.48361(19) 0.0410(8) Uani 1 1 d . . . H43 H -0.0789 0.2343 0.5326 0.049 Uiso 1 1 calc R . . C44 C -0.1534(3) 0.25409(13) 0.2680(2) 0.0480(9) Uani 1 1 d . . . C45 C -0.1471(6) 0.30354(16) 0.2382(3) 0.096(2) Uani 1 1 d . . . H45A H -0.2004 0.3071 0.1919 0.145 Uiso 1 1 calc R . . H45B H -0.0659 0.3105 0.2242 0.145 Uiso 1 1 calc R . . H45C H -0.1712 0.3246 0.2792 0.145 Uiso 1 1 calc R . . C46 C -0.1084(4) 0.22274(16) 0.2049(2) 0.0596(11) Uani 1 1 d . . . H46A H -0.1133 0.1909 0.2222 0.089 Uiso 1 1 calc R . . H46B H -0.0260 0.2303 0.1950 0.089 Uiso 1 1 calc R . . H46C H -0.1570 0.2268 0.1566 0.089 Uiso 1 1 calc R . . C47 C -0.2819(4) 0.2413(2) 0.2811(3) 0.0805(16) Uani 1 1 d . . . H47A H -0.3263 0.2406 0.2308 0.121 Uiso 1 1 calc R . . H47B H -0.3170 0.2640 0.3153 0.121 Uiso 1 1 calc R . . H47C H -0.2849 0.2111 0.3057 0.121 Uiso 1 1 calc R . . C48 C 0.1524(17) 0.1387(5) 0.5024(9) 0.037(3) Uani 0.524(19) 1 d PDU E 1 H48 H 0.1188 0.1568 0.4572 0.044 Uiso 0.524(19) 1 calc PR E 1 C49 C 0.2478(17) 0.1037(6) 0.4784(12) 0.041(3) Uani 0.524(19) 1 d PDU E 1 H49 H 0.2722 0.0996 0.4264 0.049 Uiso 0.524(19) 1 calc PR E 1 C50 C 0.291(2) 0.0801(7) 0.5398(15) 0.045(3) Uani 0.524(19) 1 d PDU E 1 H50 H 0.3494 0.0569 0.5346 0.054 Uiso 0.524(19) 1 calc PR E 1 C51 C 0.241(2) 0.0931(4) 0.6215(12) 0.037(3) Uani 0.524(19) 1 d PDU E 1 H51 H 0.2805 0.0761 0.6659 0.044 Uiso 0.524(19) 1 calc PR E 1 C52 C 0.112(2) 0.0834(9) 0.6135(13) 0.038(3) Uani 0.524(19) 1 d PDU E 1 H52A H 0.0732 0.0929 0.6616 0.046 Uiso 0.524(19) 1 calc PR E 1 H52B H 0.0994 0.0502 0.6060 0.046 Uiso 0.524(19) 1 calc PR E 1 C53 C 0.0590(15) 0.1099(7) 0.5428(10) 0.038(3) Uani 0.524(19) 1 d PDU E 1 H53A H 0.0232 0.0879 0.5047 0.046 Uiso 0.524(19) 1 calc PR E 1 H53B H -0.0046 0.1302 0.5604 0.046 Uiso 0.524(19) 1 calc PR E 1 C48A C 0.1325(19) 0.1380(5) 0.5110(10) 0.038(3) Uani 0.476(19) 1 d PDU E 2 H48A H 0.0848 0.1554 0.4705 0.046 Uiso 0.476(19) 1 calc PR E 2 C49A C 0.2354(19) 0.1110(7) 0.4775(12) 0.041(3) Uani 0.476(19) 1 d PDU E 2 H49A H 0.2887 0.1326 0.4517 0.049 Uiso 0.476(19) 1 calc PR E 2 H49B H 0.2032 0.0897 0.4369 0.049 Uiso 0.476(19) 1 calc PR E 2 C50A C 0.308(2) 0.0834(7) 0.5391(16) 0.042(3) Uani 0.476(19) 1 d PDU E 2 H50A H 0.3025 0.0503 0.5272 0.050 Uiso 0.476(19) 1 calc PR E 2 H50B H 0.3922 0.0926 0.5390 0.050 Uiso 0.476(19) 1 calc PR E 2 C51A C 0.259(2) 0.0930(4) 0.6170(14) 0.040(3) Uani 0.476(19) 1 d PDU E 2 H51A H 0.3019 0.0765 0.6607 0.048 Uiso 0.476(19) 1 calc PR E 2 C52A C 0.124(3) 0.0798(11) 0.6088(16) 0.061(8) Uani 0.476(19) 1 d PD E 2 H52C H 0.0908 0.0574 0.6414 0.074 Uiso 0.476(19) 1 calc PR E 2 C53A C 0.060(2) 0.1016(8) 0.5540(13) 0.057(6) Uani 0.476(19) 1 d PD E 2 H53C H -0.0214 0.0955 0.5425 0.068 Uiso 0.476(19) 1 calc PR E 2 C54 C 0.3777(3) 0.16808(11) 0.75548(19) 0.0413(8) Uani 1 1 d . E . H54A H 0.4544 0.1832 0.7507 0.062 Uiso 1 1 calc R . . H54B H 0.3899 0.1351 0.7628 0.062 Uiso 1 1 calc R . . H54C H 0.3379 0.1806 0.8006 0.062 Uiso 1 1 calc R . . C55 C 0.1079(3) 0.41873(10) 0.61244(17) 0.0319(6) Uani 1 1 d . . . H55 H 0.1410 0.4407 0.6525 0.038 Uiso 1 1 calc R . . C56 C -0.0301(3) 0.41563(11) 0.6099(2) 0.0397(8) Uani 1 1 d . . . H56A H -0.0570 0.4066 0.6621 0.048 Uiso 1 1 calc R . . H56B H -0.0641 0.4461 0.5971 0.048 Uiso 1 1 calc R . . C57 C -0.0753(3) 0.38024(11) 0.54806(19) 0.0380(7) Uani 1 1 d . . . H57A H -0.1303 0.3954 0.5098 0.046 Uiso 1 1 calc R . . H57B H -0.1191 0.3556 0.5742 0.046 Uiso 1 1 calc R . . C58 C 0.0306(3) 0.35884(10) 0.50407(17) 0.0315(6) Uani 1 1 d . . . H58 H 0.0057 0.3362 0.4627 0.038 Uiso 1 1 calc R . . B1 B 0.2468(3) 0.48329(12) 0.3441(2) 0.0351(8) Uani 1 1 d . . . B2 B 0.3106(3) 0.26484(12) 0.6963(2) 0.0307(7) Uani 1 1 d . . . Cl1 Cl 0.17232(12) 0.54193(4) 0.08815(6) 0.0712(3) Uani 1 1 d . . . Cl2 Cl 0.08120(13) 0.62411(4) 0.15598(7) 0.0800(4) Uani 1 1 d . . . Cl3 Cl -0.05263(11) 0.54042(4) 0.16296(8) 0.0805(4) Uani 1 1 d . . . C59 C 0.0885(4) 0.56454(13) 0.1630(2) 0.0554(10) Uani 1 1 d . . . H59 H 0.1299 0.5568 0.2140 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl4 0.039(2) 0.044(3) 0.051(3) 0.006(2) -0.0011(19) 0.014(2) Cl5 0.106(6) 0.149(8) 0.131(8) 0.039(6) -0.023(6) 0.003(6) Cl6 0.104(5) 0.131(7) 0.102(6) -0.022(5) -0.001(4) 0.018(5) C60 0.097(7) 0.115(8) 0.083(7) 0.017(7) -0.012(7) -0.001(7) Cl4A 0.164(5) 0.064(2) 0.099(3) 0.0097(19) -0.047(3) -0.019(3) Cl5A 0.0811(17) 0.098(2) 0.0688(17) 0.0284(13) 0.0040(13) 0.0255(16) Cl6A 0.110(2) 0.0782(16) 0.0515(13) 0.0048(10) 0.0118(12) 0.0236(14) C60A 0.077(4) 0.092(5) 0.062(4) 0.031(4) -0.009(4) -0.003(4) Cl4B 0.091(8) 0.098(8) 0.165(9) 0.001(7) 0.034(7) 0.000(6) Cl5B 0.225(15) 0.226(14) 0.193(14) 0.036(12) 0.019(14) 0.008(14) Cl6B 0.114(9) 0.142(10) 0.134(10) 0.031(9) 0.002(8) -0.007(8) C60B 0.108(8) 0.123(8) 0.107(8) 0.015(8) -0.004(8) 0.009(8) F1 0.0448(11) 0.0386(10) 0.0389(10) 0.0008(8) 0.0125(8) 0.0048(8) F2 0.0486(11) 0.0421(11) 0.0368(10) 0.0119(8) -0.0026(8) 0.0022(9) F3 0.0336(10) 0.0337(10) 0.0575(12) 0.0095(8) -0.0003(8) -0.0002(8) F4 0.0534(11) 0.0352(10) 0.0256(9) 0.0014(7) -0.0059(8) -0.0003(8) N1 0.0342(14) 0.0306(13) 0.0302(13) 0.0038(10) 0.0027(10) 0.0052(10) N2 0.0357(14) 0.0300(13) 0.0358(14) 0.0079(11) 0.0040(11) 0.0033(11) N3 0.0336(13) 0.0292(13) 0.0263(12) 0.0007(10) -0.0004(10) 0.0010(10) N4 0.0404(14) 0.0282(13) 0.0259(12) 0.0025(10) -0.0030(10) 0.0007(11) C1 0.0311(15) 0.0304(16) 0.0356(16) 0.0045(12) -0.0001(12) 0.0050(12) C2 0.0313(16) 0.0291(15) 0.0339(16) 0.0042(12) 0.0006(12) 0.0036(12) C3 0.0338(16) 0.0320(16) 0.0288(15) 0.0051(12) 0.0026(12) 0.0083(12) C4 0.0309(15) 0.0280(15) 0.0322(15) 0.0028(12) 0.0051(12) 0.0073(12) C5 0.0305(15) 0.0284(15) 0.0359(16) 0.0031(12) 0.0048(12) 0.0100(12) C6 0.0341(16) 0.0277(15) 0.0363(16) 0.0022(12) 0.0047(13) 0.0071(12) C7 0.0370(17) 0.0302(16) 0.0457(19) 0.0026(14) 0.0103(14) 0.0061(13) C8 0.0369(17) 0.0301(16) 0.050(2) 0.0051(14) 0.0082(14) 0.0030(13) C9 0.0365(17) 0.0350(17) 0.0467(19) 0.0132(14) 0.0076(14) 0.0053(14) C10 0.0466(19) 0.0394(18) 0.0320(16) 0.0047(13) -0.0018(14) 0.0025(15) C11 0.0340(16) 0.0269(15) 0.0382(17) 0.0025(12) 0.0038(13) 0.0032(12) C12 0.0396(18) 0.0371(17) 0.0381(18) 0.0035(14) 0.0041(14) 0.0085(14) C13 0.0452(19) 0.0420(19) 0.0368(18) 0.0017(14) 0.0086(14) 0.0082(15) C14 0.0458(19) 0.0368(18) 0.0380(18) 0.0008(14) 0.0027(14) -0.0011(14) C15 0.0394(18) 0.056(2) 0.0401(19) -0.0028(16) -0.0034(15) 0.0037(16) C16 0.0354(18) 0.050(2) 0.047(2) -0.0036(16) 0.0041(14) 0.0043(15) C17 0.054(2) 0.055(2) 0.042(2) -0.0019(17) 0.0028(16) -0.0014(18) C18 0.080(3) 0.064(3) 0.057(3) -0.009(2) -0.003(2) -0.018(2) C19 0.082(3) 0.073(3) 0.044(2) 0.009(2) -0.009(2) -0.011(2) C20 0.075(3) 0.074(3) 0.045(2) -0.010(2) 0.010(2) 0.001(2) C21A 0.038(6) 0.030(5) 0.056(5) 0.001(4) 0.015(4) 0.005(4) C22A 0.039(5) 0.040(6) 0.057(5) 0.006(5) 0.000(5) 0.004(5) C23A 0.039(5) 0.035(6) 0.066(5) 0.019(5) 0.011(4) -0.004(5) C24A 0.037(6) 0.029(5) 0.058(5) 0.011(4) 0.011(5) 0.004(4) C25A 0.036(5) 0.024(4) 0.050(7) 0.007(5) 0.011(5) -0.001(4) C26A 0.040(5) 0.038(5) 0.065(7) -0.003(5) 0.006(5) 0.002(4) C21 0.031(5) 0.033(4) 0.057(4) -0.005(3) 0.012(3) 0.001(3) C22 0.035(4) 0.034(5) 0.049(4) 0.010(3) 0.005(3) -0.003(3) C23 0.033(4) 0.036(5) 0.075(5) 0.017(4) 0.004(4) -0.003(4) C24 0.039(5) 0.037(4) 0.057(4) 0.017(3) 0.004(3) 0.001(4) C25 0.040(4) 0.028(3) 0.049(5) 0.010(3) 0.011(4) -0.004(3) C26 0.038(4) 0.030(3) 0.059(6) -0.008(4) 0.009(4) 0.001(3) C27 0.051(2) 0.053(2) 0.044(2) 0.0160(17) 0.0025(16) -0.0046(17) C28 0.0345(16) 0.0308(15) 0.0297(15) 0.0007(12) 0.0045(12) -0.0001(12) C29 0.0328(16) 0.0296(15) 0.0312(15) 0.0035(12) 0.0057(12) 0.0009(12) C30 0.0300(15) 0.0311(15) 0.0294(15) 0.0027(12) 0.0027(12) 0.0000(12) C31 0.0320(15) 0.0310(15) 0.0240(14) 0.0021(11) -0.0010(11) 0.0008(12) C32 0.0325(16) 0.0328(16) 0.0282(15) 0.0015(12) -0.0012(12) 0.0002(12) C33 0.0403(17) 0.0328(16) 0.0284(15) 0.0015(12) -0.0044(12) -0.0010(13) C34 0.052(2) 0.0309(16) 0.0341(17) 0.0002(13) -0.0062(14) -0.0011(14) C35 0.055(2) 0.0285(16) 0.0313(16) 0.0016(13) -0.0023(14) -0.0005(14) C36 0.0440(18) 0.0310(16) 0.0293(15) 0.0012(12) -0.0036(13) 0.0002(13) C37 0.050(2) 0.0354(17) 0.0278(16) -0.0023(13) -0.0033(14) 0.0018(14) C38 0.0381(16) 0.0295(15) 0.0283(15) 0.0009(12) -0.0040(12) 0.0037(13) C39 0.0397(18) 0.061(2) 0.0296(16) 0.0011(15) 0.0001(13) 0.0053(16) C40 0.0448(19) 0.062(2) 0.0261(16) -0.0008(15) 0.0004(14) 0.0058(17) C41 0.0441(18) 0.0427(18) 0.0288(16) -0.0050(13) -0.0073(13) 0.0090(15) C42 0.0367(18) 0.055(2) 0.0385(18) -0.0056(15) -0.0034(14) -0.0010(15) C43 0.0440(19) 0.049(2) 0.0301(17) 0.0018(14) -0.0032(14) -0.0063(15) C44 0.050(2) 0.057(2) 0.0360(19) -0.0057(16) -0.0123(16) 0.0079(17) C45 0.139(5) 0.059(3) 0.086(4) 0.009(3) -0.073(4) 0.007(3) C46 0.063(3) 0.082(3) 0.0331(19) -0.0091(19) -0.0101(17) 0.004(2) C47 0.047(2) 0.144(5) 0.049(2) -0.014(3) -0.0143(19) 0.011(3) C48 0.051(6) 0.034(4) 0.025(4) 0.001(3) -0.001(4) -0.003(4) C49 0.054(5) 0.031(5) 0.038(4) -0.013(4) 0.001(4) 0.006(4) C50 0.058(6) 0.035(5) 0.042(4) -0.002(4) -0.002(4) -0.001(4) C51 0.054(7) 0.032(4) 0.026(4) 0.003(4) -0.002(4) 0.001(4) C52 0.050(6) 0.032(6) 0.032(6) 0.003(5) -0.006(5) -0.004(5) C53 0.049(6) 0.038(6) 0.026(4) -0.003(5) -0.009(4) -0.008(4) C48A 0.053(7) 0.031(4) 0.031(5) -0.002(4) -0.008(5) 0.001(4) C49A 0.060(6) 0.029(5) 0.032(4) 0.005(4) -0.007(4) 0.000(4) C50A 0.060(6) 0.029(5) 0.036(4) -0.002(4) -0.005(5) 0.000(4) C51A 0.053(7) 0.030(5) 0.037(5) 0.004(4) -0.006(5) -0.002(4) C52A 0.096(17) 0.048(12) 0.040(9) 0.003(7) -0.001(9) -0.020(10) C53A 0.076(11) 0.044(9) 0.052(10) 0.002(6) 0.020(8) -0.027(7) C54 0.060(2) 0.0317(16) 0.0317(16) 0.0038(13) -0.0106(15) 0.0030(15) C55 0.0354(16) 0.0303(16) 0.0302(15) 0.0034(12) 0.0050(12) 0.0034(13) C56 0.0361(18) 0.0412(18) 0.0424(18) 0.0057(14) 0.0086(14) 0.0100(14) C57 0.0305(16) 0.0411(18) 0.0426(18) 0.0073(14) 0.0029(13) 0.0027(13) C58 0.0308(16) 0.0325(16) 0.0312(15) 0.0033(12) 0.0003(12) 0.0023(12) B1 0.040(2) 0.0332(18) 0.0325(18) 0.0066(14) 0.0032(15) 0.0040(15) B2 0.0337(18) 0.0286(17) 0.0295(17) 0.0031(13) -0.0016(13) -0.0006(14) Cl1 0.0931(9) 0.0675(7) 0.0533(6) 0.0032(5) 0.0063(6) 0.0045(6) Cl2 0.1138(10) 0.0457(6) 0.0776(8) 0.0019(5) -0.0330(7) 0.0058(6) Cl3 0.0624(7) 0.0776(8) 0.1007(10) 0.0175(7) -0.0055(6) -0.0031(6) C59 0.067(3) 0.046(2) 0.052(2) 0.0097(17) -0.0078(19) 0.0051(19) _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 Cl4 C60 1.761(19) . ? Cl5 C60 1.749(19) . ? Cl6 C60 1.783(19) . ? C60 H60 1.0000 . ? Cl4A C60A 1.746(9) . ? Cl5A C60A 1.763(8) . ? Cl6A C60A 1.758(10) . ? C60A H60A 1.0000 . ? Cl4B C60B 1.78(2) . ? Cl5B C60B 1.73(2) . ? Cl6B C60B 1.79(2) . ? C60B H60B 1.0000 . ? F1 B1 1.392(4) . ? F2 B1 1.399(4) . ? F3 B2 1.393(4) . ? F4 B2 1.379(4) . ? N1 C1 1.362(4) . ? N1 C4 1.403(4) . ? N1 B1 1.548(4) . ? N2 C9 1.364(4) . ? N2 C6 1.405(4) . ? N2 B1 1.556(5) . ? N3 C28 1.362(4) . ? N3 C31 1.401(4) . ? N3 B2 1.552(4) . ? N4 C36 1.357(4) . ? N4 C33 1.402(4) . ? N4 B2 1.553(4) . ? C1 C2 1.397(4) . ? C1 C10 1.491(4) . ? C2 C3 1.385(4) . ? C2 C58 1.511(4) . ? C3 C4 1.411(4) . ? C3 C55 1.520(4) . ? C4 C5 1.399(4) . ? C5 C6 1.388(4) . ? C5 C11 1.480(4) . ? C6 C7 1.429(4) . ? C7 C8 1.372(4) . ? C7 C21 1.493(10) . ? C7 C21A 1.508(12) . ? C8 C9 1.402(5) . ? C8 C24A 1.505(12) . ? C8 C24 1.509(10) . ? C9 C27 1.488(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.385(5) . ? C11 C12 1.390(4) . ? C12 C13 1.387(5) . ? C12 H12 0.9500 . ? C13 C14 1.398(5) . ? C13 H13 0.9500 . ? C14 C15 1.385(5) . ? C14 C17 1.530(5) . ? C15 C16 1.389(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C19 1.512(6) . ? C17 C20 1.523(6) . ? C17 C18 1.550(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.53(2) . ? C21A C26A 1.60(3) . ? C21A H21A 1.0000 . ? C22A C23A 1.467(15) . ? C22A H22 0.9500 . ? C23A C24A 1.39(3) . ? C23A H23 0.9500 . ? C24A C25A 1.71(3) . ? C24A H24A 1.0000 . ? C25A C26A 1.418(10) . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C21 C26 1.517(19) . ? C21 C22 1.595(19) . ? C21 H21 1.0000 . ? C22 C23 1.427(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.70(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.40(3) . ? C24 H24 1.0000 . ? C25 C26 1.425(10) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.398(4) . ? C28 C37 1.492(4) . ? C29 C30 1.382(4) . ? C29 C55 1.514(4) . ? C30 C31 1.412(4) . ? C30 C58 1.513(4) . ? C31 C32 1.398(4) . ? C32 C33 1.404(4) . ? C32 C38 1.493(4) . ? C33 C34 1.405(4) . ? C34 C35 1.379(4) . ? C34 C48A 1.500(11) . ? C34 C48 1.502(10) . ? C35 C36 1.399(4) . ? C35 C51 1.514(11) . ? C35 C51A 1.515(11) . ? C36 C54 1.494(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C43 1.371(5) . ? C38 C39 1.389(4) . ? C39 C40 1.379(4) . ? C39 H39 0.9500 . ? C40 C41 1.385(5) . ? C40 H40 0.9500 . ? C41 C42 1.382(5) . ? C41 C44 1.540(4) . ? C42 C43 1.397(4) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C46 1.520(5) . ? C44 C47 1.527(6) . ? C44 C45 1.535(6) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C53 1.54(2) . ? C48 C49 1.553(19) . ? C48 H48 1.0000 . ? C49 C50 1.334(15) . ? C49 H49 0.9500 . ? C50 C51 1.58(3) . ? C50 H50 0.9500 . ? C51 C52 1.48(3) . ? C51 H51 1.0000 . ? C52 C53 1.538(14) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C48A C49A 1.54(2) . ? C48A C53A 1.55(2) . ? C48A H48A 1.0000 . ? C49A C50A 1.538(18) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C50A C51A 1.49(3) . ? C50A H50A 0.9900 . ? C50A H50B 0.9900 . ? C51A C52A 1.57(3) . ? C51A H51A 1.0000 . ? C52A C53A 1.33(2) . ? C52A H52C 0.9500 . ? C53A H53C 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.563(4) . ? C55 H55 1.0000 . ? C56 C57 1.552(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.570(4) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58 1.0000 . ? Cl1 C59 1.753(4) . ? Cl2 C59 1.747(4) . ? Cl3 C59 1.745(4) . ? C59 H59 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 Cl5 C60 Cl4 104.7(13) . . ? Cl5 C60 Cl6 102.0(13) . . ? Cl4 C60 Cl6 124.4(18) . . ? Cl5 C60 H60 108.2 . . ? Cl4 C60 H60 108.2 . . ? Cl6 C60 H60 108.2 . . ? Cl4A C60A Cl6A 111.7(6) . . ? Cl4A C60A Cl5A 113.7(6) . . ? Cl6A C60A Cl5A 105.7(5) . . ? Cl4A C60A H60A 108.5 . . ? Cl6A C60A H60A 108.5 . . ? Cl5A C60A H60A 108.5 . . ? Cl5B C60B Cl4B 110.6(19) . . ? Cl5B C60B Cl6B 111.0(18) . . ? Cl4B C60B Cl6B 102.3(15) . . ? Cl5B C60B H60B 110.9 . . ? Cl4B C60B H60B 110.9 . . ? Cl6B C60B H60B 110.9 . . ? C1 N1 C4 108.0(2) . . ? C1 N1 B1 126.5(3) . . ? C4 N1 B1 125.3(3) . . ? C9 N2 C6 108.5(3) . . ? C9 N2 B1 127.3(3) . . ? C6 N2 B1 124.2(2) . . ? C28 N3 C31 108.3(2) . . ? C28 N3 B2 127.1(2) . . ? C31 N3 B2 124.4(2) . . ? C36 N4 C33 108.4(2) . . ? C36 N4 B2 126.9(2) . . ? C33 N4 B2 124.5(2) . . ? N1 C1 C2 109.0(3) . . ? N1 C1 C10 123.1(3) . . ? C2 C1 C10 127.9(3) . . ? C3 C2 C1 108.1(3) . . ? C3 C2 C58 115.9(3) . . ? C1 C2 C58 136.0(3) . . ? C2 C3 C4 107.3(3) . . ? C2 C3 C55 114.3(3) . . ? C4 C3 C55 138.4(3) . . ? C5 C4 N1 120.4(3) . . ? C5 C4 C3 131.8(3) . . ? N1 C4 C3 107.6(3) . . ? C6 C5 C4 121.1(3) . . ? C6 C5 C11 118.8(3) . . ? C4 C5 C11 120.1(3) . . ? C5 C6 N2 121.5(3) . . ? C5 C6 C7 131.4(3) . . ? N2 C6 C7 107.0(3) . . ? C8 C7 C6 107.1(3) . . ? C8 C7 C21 114.0(5) . . ? C6 C7 C21 138.8(5) . . ? C8 C7 C21A 113.9(6) . . ? C6 C7 C21A 138.6(6) . . ? C7 C8 C9 108.9(3) . . ? C7 C8 C24A 112.7(8) . . ? C9 C8 C24A 138.1(8) . . ? C7 C8 C24 116.5(6) . . ? C9 C8 C24 134.4(6) . . ? N2 C9 C8 108.4(3) . . ? N2 C9 C27 124.0(3) . . ? C8 C9 C27 127.5(3) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 118.9(3) . . ? C16 C11 C5 119.0(3) . . ? C12 C11 C5 122.0(3) . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 121.9(3) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C15 C14 C13 116.7(3) . . ? C15 C14 C17 119.4(3) . . ? C13 C14 C17 123.8(3) . . ? C14 C15 C16 122.3(3) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C11 C16 C15 120.1(3) . . ? C11 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C19 C17 C20 110.0(4) . . ? C19 C17 C14 110.6(3) . . ? C20 C17 C14 112.6(3) . . ? C19 C17 C18 109.1(4) . . ? C20 C17 C18 106.2(4) . . ? C14 C17 C18 108.3(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C7 C21A C22A 111.3(16) . . ? C7 C21A C26A 106.2(14) . . ? C22A C21A C26A 102.7(12) . . ? C7 C21A H21A 112.0 . . ? C22A C21A H21A 112.0 . . ? C26A C21A H21A 112.0 . . ? C23A C22A C21A 113.6(18) . . ? C23A C22A H22 123.2 . . ? C21A C22A H22 123.2 . . ? C24A C23A C22A 110.2(19) . . ? C24A C23A H23 124.9 . . ? C22A C23A H23 124.9 . . ? C23A C24A C8 116.7(18) . . ? C23A C24A C25A 104.6(12) . . ? C8 C24A C25A 99.8(15) . . ? C23A C24A H24A 111.6 . . ? C8 C24A H24A 111.6 . . ? C25A C24A H24A 111.6 . . ? C26A C25A C24A 114.0(16) . . ? C26A C25A H25A 108.7 . . ? C24A C25A H25A 108.7 . . ? C26A C25A H25B 108.7 . . ? C24A C25A H25B 108.7 . . ? H25A C25A H25B 107.6 . . ? C25A C26A C21A 106.2(15) . . ? C25A C26A H26A 110.5 . . ? C21A C26A H26A 110.5 . . ? C25A C26A H26B 110.5 . . ? C21A C26A H26B 110.5 . . ? H26A C26A H26B 108.7 . . ? C7 C21 C26 107.3(9) . . ? C7 C21 C22 100.9(11) . . ? C26 C21 C22 105.4(9) . . ? C7 C21 H21 114.0 . . ? C26 C21 H21 114.0 . . ? C22 C21 H21 114.0 . . ? C23 C22 C21 109.7(12) . . ? C23 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? C23 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C22 C23 C24 114.0(13) . . ? C22 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? C22 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C25 C24 C8 112.1(14) . . ? C25 C24 C23 104.3(9) . . ? C8 C24 C23 96.8(11) . . ? C25 C24 H24 114.0 . . ? C8 C24 H24 114.0 . . ? C23 C24 H24 114.0 . . ? C24 C25 C26 112.3(13) . . ? C24 C25 H25 123.9 . . ? C26 C25 H25 123.9 . . ? C25 C26 C21 117.3(12) . . ? C25 C26 H26 121.3 . . ? C21 C26 H26 121.3 . . ? C9 C27 H27A 109.5 . . ? C9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 108.5(3) . . ? N3 C28 C37 123.0(3) . . ? C29 C28 C37 128.5(3) . . ? C30 C29 C28 108.5(3) . . ? C30 C29 C55 115.6(3) . . ? C28 C29 C55 135.9(3) . . ? C29 C30 C31 107.0(3) . . ? C29 C30 C58 114.8(3) . . ? C31 C30 C58 138.2(3) . . ? C32 C31 N3 121.4(3) . . ? C32 C31 C30 130.9(3) . . ? N3 C31 C30 107.6(2) . . ? C31 C32 C33 120.1(3) . . ? C31 C32 C38 118.7(3) . . ? C33 C32 C38 121.2(3) . . ? N4 C33 C32 120.8(3) . . ? N4 C33 C34 107.4(3) . . ? C32 C33 C34 131.6(3) . . ? C35 C34 C33 107.4(3) . . ? C35 C34 C48A 113.9(7) . . ? C33 C34 C48A 137.8(7) . . ? C35 C34 C48 114.4(7) . . ? C33 C34 C48 138.1(7) . . ? C34 C35 C36 108.3(3) . . ? C34 C35 C51 112.7(7) . . ? C36 C35 C51 138.3(7) . . ? C34 C35 C51A 114.3(8) . . ? C36 C35 C51A 137.4(8) . . ? N4 C36 C35 108.5(3) . . ? N4 C36 C54 122.2(3) . . ? C35 C36 C54 129.2(3) . . ? C28 C37 H37A 109.5 . . ? C28 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C28 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C43 C38 C39 117.9(3) . . ? C43 C38 C32 121.2(3) . . ? C39 C38 C32 120.8(3) . . ? C40 C39 C38 120.8(3) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C41 122.1(3) . . ? C39 C40 H40 119.0 . . ? C41 C40 H40 119.0 . . ? C42 C41 C40 116.6(3) . . ? C42 C41 C44 123.1(3) . . ? C40 C41 C44 120.3(3) . . ? C41 C42 C43 121.7(3) . . ? C41 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C38 C43 C42 120.8(3) . . ? C38 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C46 C44 C47 107.7(3) . . ? C46 C44 C45 108.0(4) . . ? C47 C44 C45 109.6(4) . . ? C46 C44 C41 110.7(3) . . ? C47 C44 C41 112.5(3) . . ? C45 C44 C41 108.1(3) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C34 C48 C53 101.3(12) . . ? C34 C48 C49 110.7(12) . . ? C53 C48 C49 104.9(10) . . ? C34 C48 H48 113.0 . . ? C53 C48 H48 113.0 . . ? C49 C48 H48 113.0 . . ? C50 C49 C48 111.7(18) . . ? C50 C49 H49 124.1 . . ? C48 C49 H49 124.1 . . ? C49 C50 C51 116.0(19) . . ? C49 C50 H50 122.0 . . ? C51 C50 H50 122.0 . . ? C52 C51 C35 108.3(16) . . ? C52 C51 C50 105.1(11) . . ? C35 C51 C50 104.8(14) . . ? C52 C51 H51 112.7 . . ? C35 C51 H51 112.7 . . ? C50 C51 H51 112.7 . . ? C51 C52 C53 109.3(17) . . ? C51 C52 H52A 109.8 . . ? C53 C52 H52A 109.8 . . ? C51 C52 H52B 109.8 . . ? C53 C52 H52B 109.8 . . ? H52A C52 H52B 108.3 . . ? C48 C53 C52 111.9(14) . . ? C48 C53 H53A 109.2 . . ? C52 C53 H53A 109.2 . . ? C48 C53 H53B 109.2 . . ? C52 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? C34 C48A C49A 100.6(14) . . ? C34 C48A C53A 110.4(14) . . ? C49A C48A C53A 104.4(11) . . ? C34 C48A H48A 113.5 . . ? C49A C48A H48A 113.5 . . ? C53A C48A H48A 113.5 . . ? C48A C49A C50A 113.9(17) . . ? C48A C49A H49A 108.8 . . ? C50A C49A H49A 108.8 . . ? C48A C49A H49B 108.8 . . ? C50A C49A H49B 108.8 . . ? H49A C49A H49B 107.7 . . ? C51A C50A C49A 107.9(18) . . ? C51A C50A H50A 110.1 . . ? C49A C50A H50A 110.1 . . ? C51A C50A H50B 110.1 . . ? C49A C50A H50B 110.1 . . ? H50A C50A H50B 108.4 . . ? C50A C51A C35 107.7(16) . . ? C50A C51A C52A 105.6(12) . . ? C35 C51A C52A 103.9(18) . . ? C50A C51A H51A 113.0 . . ? C35 C51A H51A 113.0 . . ? C52A C51A H51A 113.0 . . ? C53A C52A C51A 117(2) . . ? C53A C52A H52C 121.7 . . ? C51A C52A H52C 121.7 . . ? C52A C53A C48A 112(2) . . ? C52A C53A H53C 123.9 . . ? C48A C53A H53C 123.9 . . ? C36 C54 H54A 109.5 . . ? C36 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C36 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C29 C55 C3 105.4(2) . . ? C29 C55 C56 104.9(2) . . ? C3 C55 C56 104.3(2) . . ? C29 C55 H55 113.7 . . ? C3 C55 H55 113.7 . . ? C56 C55 H55 113.7 . . ? C57 C56 C55 111.0(3) . . ? C57 C56 H56A 109.4 . . ? C55 C56 H56A 109.4 . . ? C57 C56 H56B 109.4 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C56 C57 C58 110.9(3) . . ? C56 C57 H57A 109.5 . . ? C58 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 108.1 . . ? C2 C58 C30 104.7(2) . . ? C2 C58 C57 104.8(2) . . ? C30 C58 C57 104.9(2) . . ? C2 C58 H58 113.8 . . ? C30 C58 H58 113.8 . . ? C57 C58 H58 113.8 . . ? F1 B1 F2 108.5(3) . . ? F1 B1 N1 110.8(3) . . ? F2 B1 N1 109.6(3) . . ? F1 B1 N2 110.6(3) . . ? F2 B1 N2 110.0(3) . . ? N1 B1 N2 107.3(3) . . ? F4 B2 F3 109.2(3) . . ? F4 B2 N3 110.5(3) . . ? F3 B2 N3 110.2(2) . . ? F4 B2 N4 110.7(2) . . ? F3 B2 N4 109.9(3) . . ? N3 B2 N4 106.4(2) . . ? Cl3 C59 Cl2 111.2(2) . . ? Cl3 C59 Cl1 111.7(2) . . ? Cl2 C59 Cl1 110.5(2) . . ? Cl3 C59 H59 107.7 . . ? Cl2 C59 H59 107.7 . . ? Cl1 C59 H59 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C2 0.6(3) . . . . ? B1 N1 C1 C2 175.8(3) . . . . ? C4 N1 C1 C10 -179.2(3) . . . . ? B1 N1 C1 C10 -4.0(5) . . . . ? N1 C1 C2 C3 -0.6(3) . . . . ? C10 C1 C2 C3 179.2(3) . . . . ? N1 C1 C2 C58 178.3(3) . . . . ? C10 C1 C2 C58 -1.9(6) . . . . ? C1 C2 C3 C4 0.4(3) . . . . ? C58 C2 C3 C4 -178.8(2) . . . . ? C1 C2 C3 C55 179.3(2) . . . . ? C58 C2 C3 C55 0.1(4) . . . . ? C1 N1 C4 C5 176.3(3) . . . . ? B1 N1 C4 C5 1.0(4) . . . . ? C1 N1 C4 C3 -0.3(3) . . . . ? B1 N1 C4 C3 -175.6(3) . . . . ? C2 C3 C4 C5 -176.1(3) . . . . ? C55 C3 C4 C5 5.4(6) . . . . ? C2 C3 C4 N1 0.0(3) . . . . ? C55 C3 C4 N1 -178.5(3) . . . . ? N1 C4 C5 C6 1.9(4) . . . . ? C3 C4 C5 C6 177.5(3) . . . . ? N1 C4 C5 C11 -177.5(3) . . . . ? C3 C4 C5 C11 -1.8(5) . . . . ? C4 C5 C6 N2 -1.1(4) . . . . ? C11 C5 C6 N2 178.3(3) . . . . ? C4 C5 C6 C7 175.4(3) . . . . ? C11 C5 C6 C7 -5.2(5) . . . . ? C9 N2 C6 C5 177.6(3) . . . . ? B1 N2 C6 C5 -2.5(4) . . . . ? C9 N2 C6 C7 0.3(3) . . . . ? B1 N2 C6 C7 -179.8(3) . . . . ? C5 C6 C7 C8 -177.5(3) . . . . ? N2 C6 C7 C8 -0.6(3) . . . . ? C5 C6 C7 C21 -2.5(12) . . . . ? N2 C6 C7 C21 174.4(10) . . . . ? C5 C6 C7 C21A 11.1(15) . . . . ? N2 C6 C7 C21A -171.9(14) . . . . ? C6 C7 C8 C9 0.6(4) . . . . ? C21 C7 C8 C9 -175.8(7) . . . . ? C21A C7 C8 C9 174.4(10) . . . . ? C6 C7 C8 C24A -174.4(12) . . . . ? C21 C7 C8 C24A 9.3(14) . . . . ? C21A C7 C8 C24A -0.6(15) . . . . ? C6 C7 C8 C24 177.4(10) . . . . ? C21 C7 C8 C24 1.0(12) . . . . ? C21A C7 C8 C24 -8.9(14) . . . . ? C6 N2 C9 C8 0.0(3) . . . . ? B1 N2 C9 C8 -179.9(3) . . . . ? C6 N2 C9 C27 179.3(3) . . . . ? B1 N2 C9 C27 -0.6(5) . . . . ? C7 C8 C9 N2 -0.4(4) . . . . ? C24A C8 C9 N2 172.6(16) . . . . ? C24 C8 C9 N2 -176.4(13) . . . . ? C7 C8 C9 C27 -179.7(3) . . . . ? C24A C8 C9 C27 -6.6(17) . . . . ? C24 C8 C9 C27 4.4(14) . . . . ? C6 C5 C11 C16 -70.9(4) . . . . ? C4 C5 C11 C16 108.5(4) . . . . ? C6 C5 C11 C12 106.0(4) . . . . ? C4 C5 C11 C12 -74.6(4) . . . . ? C16 C11 C12 C13 1.7(5) . . . . ? C5 C11 C12 C13 -175.2(3) . . . . ? C11 C12 C13 C14 -1.0(5) . . . . ? C12 C13 C14 C15 -0.7(5) . . . . ? C12 C13 C14 C17 175.1(3) . . . . ? C13 C14 C15 C16 1.7(5) . . . . ? C17 C14 C15 C16 -174.3(3) . . . . ? C12 C11 C16 C15 -0.8(5) . . . . ? C5 C11 C16 C15 176.2(3) . . . . ? C14 C15 C16 C11 -1.0(6) . . . . ? C15 C14 C17 C19 -59.2(5) . . . . ? C13 C14 C17 C19 125.1(4) . . . . ? C15 C14 C17 C20 177.4(4) . . . . ? C13 C14 C17 C20 1.6(5) . . . . ? C15 C14 C17 C18 60.3(5) . . . . ? C13 C14 C17 C18 -115.4(4) . . . . ? C8 C7 C21A C22A -46.7(16) . . . . ? C6 C7 C21A C22A 124.3(12) . . . . ? C21 C7 C21A C22A -139(7) . . . . ? C8 C7 C21A C26A 64.4(14) . . . . ? C6 C7 C21A C26A -124.6(11) . . . . ? C21 C7 C21A C26A -28(6) . . . . ? C7 C21A C22A C23A 48(2) . . . . ? C26A C21A C22A C23A -65(2) . . . . ? C21A C22A C23A C24A 0(3) . . . . ? C22A C23A C24A C8 -51(2) . . . . ? C22A C23A C24A C25A 58(2) . . . . ? C7 C8 C24A C23A 54(2) . . . . ? C9 C8 C24A C23A -118.5(14) . . . . ? C24 C8 C24A C23A 173(11) . . . . ? C7 C8 C24A C25A -57.6(14) . . . . ? C9 C8 C24A C25A 129.6(10) . . . . ? C24 C8 C24A C25A 61(10) . . . . ? C23A C24A C25A C26A -58(2) . . . . ? C8 C24A C25A C26A 63(2) . . . . ? C24A C25A C26A C21A -6(2) . . . . ? C7 C21A C26A C25A -55(2) . . . . ? C22A C21A C26A C25A 62(2) . . . . ? C8 C7 C21 C26 45.8(12) . . . . ? C6 C7 C21 C26 -128.9(9) . . . . ? C21A C7 C21 C26 137(7) . . . . ? C8 C7 C21 C22 -64.2(10) . . . . ? C6 C7 C21 C22 121.0(9) . . . . ? C21A C7 C21 C22 27(6) . . . . ? C7 C21 C22 C23 59.3(14) . . . . ? C26 C21 C22 C23 -52.2(14) . . . . ? C21 C22 C23 C24 0.4(17) . . . . ? C7 C8 C24 C25 -51.3(15) . . . . ? C9 C8 C24 C25 124.5(9) . . . . ? C24A C8 C24 C25 -116(10) . . . . ? C7 C8 C24 C23 57.2(12) . . . . ? C9 C8 C24 C23 -127.1(8) . . . . ? C24A C8 C24 C23 -7(9) . . . . ? C22 C23 C24 C25 57.8(15) . . . . ? C22 C23 C24 C8 -57.1(16) . . . . ? C8 C24 C25 C26 45.9(17) . . . . ? C23 C24 C25 C26 -57.7(15) . . . . ? C24 C25 C26 C21 4(2) . . . . ? C7 C21 C26 C25 -50.9(17) . . . . ? C22 C21 C26 C25 56.0(16) . . . . ? C31 N3 C28 C29 -0.6(3) . . . . ? B2 N3 C28 C29 173.7(3) . . . . ? C31 N3 C28 C37 179.6(3) . . . . ? B2 N3 C28 C37 -6.2(5) . . . . ? N3 C28 C29 C30 0.4(3) . . . . ? C37 C28 C29 C30 -179.8(3) . . . . ? N3 C28 C29 C55 -178.2(3) . . . . ? C37 C28 C29 C55 1.7(6) . . . . ? C28 C29 C30 C31 -0.1(3) . . . . ? C55 C29 C30 C31 178.8(3) . . . . ? C28 C29 C30 C58 179.5(2) . . . . ? C55 C29 C30 C58 -1.6(4) . . . . ? C28 N3 C31 C32 -178.1(3) . . . . ? B2 N3 C31 C32 7.5(4) . . . . ? C28 N3 C31 C30 0.5(3) . . . . ? B2 N3 C31 C30 -173.9(3) . . . . ? C29 C30 C31 C32 178.1(3) . . . . ? C58 C30 C31 C32 -1.3(6) . . . . ? C29 C30 C31 N3 -0.3(3) . . . . ? C58 C30 C31 N3 -179.7(3) . . . . ? N3 C31 C32 C33 2.3(4) . . . . ? C30 C31 C32 C33 -175.9(3) . . . . ? N3 C31 C32 C38 178.9(3) . . . . ? C30 C31 C32 C38 0.7(5) . . . . ? C36 N4 C33 C32 174.4(3) . . . . ? B2 N4 C33 C32 -11.1(5) . . . . ? C36 N4 C33 C34 -1.7(4) . . . . ? B2 N4 C33 C34 172.8(3) . . . . ? C31 C32 C33 N4 -0.6(5) . . . . ? C38 C32 C33 N4 -177.1(3) . . . . ? C31 C32 C33 C34 174.4(3) . . . . ? C38 C32 C33 C34 -2.1(5) . . . . ? N4 C33 C34 C35 2.3(4) . . . . ? C32 C33 C34 C35 -173.2(3) . . . . ? N4 C33 C34 C48A 169.9(14) . . . . ? C32 C33 C34 C48A -5.6(15) . . . . ? N4 C33 C34 C48 -174.4(13) . . . . ? C32 C33 C34 C48 10.1(14) . . . . ? C33 C34 C35 C36 -2.1(4) . . . . ? C48A C34 C35 C36 -173.0(11) . . . . ? C48 C34 C35 C36 175.5(9) . . . . ? C33 C34 C35 C51 170.2(11) . . . . ? C48A C34 C35 C51 -0.7(16) . . . . ? C48 C34 C35 C51 -12.2(15) . . . . ? C33 C34 C35 C51A 179.2(13) . . . . ? C48A C34 C35 C51A 8.3(17) . . . . ? C48 C34 C35 C51A -3.2(16) . . . . ? C33 N4 C36 C35 0.4(4) . . . . ? B2 N4 C36 C35 -173.9(3) . . . . ? C33 N4 C36 C54 178.8(3) . . . . ? B2 N4 C36 C54 4.4(5) . . . . ? C34 C35 C36 N4 1.1(4) . . . . ? C51 C35 C36 N4 -168.2(16) . . . . ? C51A C35 C36 N4 179.4(17) . . . . ? C34 C35 C36 C54 -177.1(3) . . . . ? C51 C35 C36 C54 13.6(17) . . . . ? C51A C35 C36 C54 1.2(18) . . . . ? C31 C32 C38 C43 -88.0(4) . . . . ? C33 C32 C38 C43 88.6(4) . . . . ? C31 C32 C38 C39 87.9(4) . . . . ? C33 C32 C38 C39 -95.6(4) . . . . ? C43 C38 C39 C40 2.5(5) . . . . ? C32 C38 C39 C40 -173.5(3) . . . . ? C38 C39 C40 C41 0.1(6) . . . . ? C39 C40 C41 C42 -2.6(5) . . . . ? C39 C40 C41 C44 176.5(3) . . . . ? C40 C41 C42 C43 2.5(5) . . . . ? C44 C41 C42 C43 -176.5(3) . . . . ? C39 C38 C43 C42 -2.6(5) . . . . ? C32 C38 C43 C42 173.4(3) . . . . ? C41 C42 C43 C38 0.1(6) . . . . ? C42 C41 C44 C46 -127.2(4) . . . . ? C40 C41 C44 C46 53.8(5) . . . . ? C42 C41 C44 C47 -6.5(5) . . . . ? C40 C41 C44 C47 174.5(4) . . . . ? C42 C41 C44 C45 114.7(5) . . . . ? C40 C41 C44 C45 -64.4(5) . . . . ? C35 C34 C48 C53 65.9(11) . . . . ? C33 C34 C48 C53 -117.6(10) . . . . ? C48A C34 C48 C53 -24(7) . . . . ? C35 C34 C48 C49 -44.9(14) . . . . ? C33 C34 C48 C49 131.6(11) . . . . ? C48A C34 C48 C49 -135(7) . . . . ? C34 C48 C49 C50 51.8(19) . . . . ? C53 C48 C49 C50 -56.7(17) . . . . ? C48 C49 C50 C51 -1(2) . . . . ? C34 C35 C51 C52 -52.0(16) . . . . ? C36 C35 C51 C52 117.0(12) . . . . ? C51A C35 C51 C52 -155(10) . . . . ? C34 C35 C51 C50 59.9(13) . . . . ? C36 C35 C51 C50 -131.2(11) . . . . ? C51A C35 C51 C50 -43(9) . . . . ? C49 C50 C51 C52 61.1(19) . . . . ? C49 C50 C51 C35 -53.0(19) . . . . ? C35 C51 C52 C53 56(2) . . . . ? C50 C51 C52 C53 -55(2) . . . . ? C34 C48 C53 C52 -57.1(18) . . . . ? C49 C48 C53 C52 58.1(18) . . . . ? C51 C52 C53 C48 -1(2) . . . . ? C35 C34 C48A C49A -62.9(13) . . . . ? C33 C34 C48A C49A 130.1(11) . . . . ? C48 C34 C48A C49A 32(6) . . . . ? C35 C34 C48A C53A 46.9(16) . . . . ? C33 C34 C48A C53A -120.1(12) . . . . ? C48 C34 C48A C53A 142(8) . . . . ? C34 C48A C49A C50A 59.4(18) . . . . ? C53A C48A C49A C50A -55.0(19) . . . . ? C48A C49A C50A C51A -3(2) . . . . ? C49A C50A C51A C35 -53.9(18) . . . . ? C49A C50A C51A C52A 56.6(18) . . . . ? C34 C35 C51A C50A 54.7(16) . . . . ? C36 C35 C51A C50A -123.6(12) . . . . ? C51 C35 C51A C50A 135(10) . . . . ? C34 C35 C51A C52A -57.0(17) . . . . ? C36 C35 C51A C52A 124.7(13) . . . . ? C51 C35 C51A C52A 24(9) . . . . ? C50A C51A C52A C53A -59(3) . . . . ? C35 C51A C52A C53A 55(3) . . . . ? C51A C52A C53A C48A -3(3) . . . . ? C34 C48A C53A C52A -50(2) . . . . ? C49A C48A C53A C52A 58(2) . . . . ? C30 C29 C55 C3 -51.3(3) . . . . ? C28 C29 C55 C3 127.3(4) . . . . ? C30 C29 C55 C56 58.6(3) . . . . ? C28 C29 C55 C56 -122.9(4) . . . . ? C2 C3 C55 C29 51.7(3) . . . . ? C4 C3 C55 C29 -129.8(4) . . . . ? C2 C3 C55 C56 -58.5(3) . . . . ? C4 C3 C55 C56 119.9(4) . . . . ? C29 C55 C56 C57 -53.7(3) . . . . ? C3 C55 C56 C57 56.8(3) . . . . ? C55 C56 C57 C58 -1.7(4) . . . . ? C3 C2 C58 C30 -52.6(3) . . . . ? C1 C2 C58 C30 128.5(4) . . . . ? C3 C2 C58 C57 57.5(3) . . . . ? C1 C2 C58 C57 -121.3(4) . . . . ? C29 C30 C58 C2 53.2(3) . . . . ? C31 C30 C58 C2 -127.4(4) . . . . ? C29 C30 C58 C57 -56.8(3) . . . . ? C31 C30 C58 C57 122.6(4) . . . . ? C56 C57 C58 C2 -53.8(3) . . . . ? C56 C57 C58 C30 56.2(3) . . . . ? C1 N1 B1 F1 -57.4(4) . . . . ? C4 N1 B1 F1 117.0(3) . . . . ? C1 N1 B1 F2 62.3(4) . . . . ? C4 N1 B1 F2 -123.3(3) . . . . ? C1 N1 B1 N2 -178.2(3) . . . . ? C4 N1 B1 N2 -3.8(4) . . . . ? C9 N2 B1 F1 63.5(4) . . . . ? C6 N2 B1 F1 -116.5(3) . . . . ? C9 N2 B1 F2 -56.4(4) . . . . ? C6 N2 B1 F2 123.7(3) . . . . ? C9 N2 B1 N1 -175.6(3) . . . . ? C6 N2 B1 N1 4.5(4) . . . . ? C28 N3 B2 F4 50.5(4) . . . . ? C31 N3 B2 F4 -136.1(3) . . . . ? C28 N3 B2 F3 -70.2(4) . . . . ? C31 N3 B2 F3 103.2(3) . . . . ? C28 N3 B2 N4 170.7(3) . . . . ? C31 N3 B2 N4 -15.9(4) . . . . ? C36 N4 B2 F4 -48.7(4) . . . . ? C33 N4 B2 F4 137.8(3) . . . . ? C36 N4 B2 F3 71.9(4) . . . . ? C33 N4 B2 F3 -101.5(3) . . . . ? C36 N4 B2 N3 -168.8(3) . . . . ? C33 N4 B2 N3 17.8(4) . . . . ? data_transBCODBisbenzoBODIPY _database_code_depnum_ccdc_archive 'CCDC 864651' #TrackingRef '9290_web_deposit_cif_file_6_HidemitsuUno_1327633261.transBCODBisBenzoBODIPY.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C64 H65 B2 Cl F4 N4' _chemical_formula_moiety 'C58 H60 B2 F4 N4, C6 H5 Cl' _chemical_formula_weight 1023.31 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' #------------------------------------------------------------------------------ _cell_length_a 11.247(4) _cell_length_b 27.084(9) _cell_length_c 17.815(6) _cell_angle_alpha 90.0000 _cell_angle_beta 94.678(6) _cell_angle_gamma 90.0000 _cell_volume 5409(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12793 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160.00 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_T_max 0.974 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 41427 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_theta_max 27.57 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 #============================================================================== # REFINEMENT DATA _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. BCOD moieties disorder and their atomic coordinates are restrained. A small void is found by Platon. However, no electron peak is found ; _reflns_number_total 12384 _reflns_number_gt 9355 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_number_restraints 243 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 12378 _refine_ls_number_parameters 733 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0575P)^2^+2.8022P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_diff_density_max 0.300 _refine_diff_density_min -0.760 _refine_ls_extinction_method none _iucr_refine_instructions_details ; TITL transBCODBisbenzoBODIPY CELL 0.71070 11.24710 27.08430 17.81460 90.000 94.678 90.000 ZERR 4 0.00330 0.00830 0.00550 0.000 0.006 0.000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H CL B F N UNIT 256 260 4 8 16 16 SHEL 99999.000000 0.000000 L.S. 10 FMAP 2 PLAN -25 WPDB -2 HTAB TEMP -172.9 ACTA BOND $H CONF BUMP 0.005 OMIT 0 1 1 OMIT 1 0 0 OMIT 2 2 3 OMIT 4 4 1 OMIT 4 0 6 OMIT 0 3 1 EXYZ C53 C53A EADP C53 C53A EXYZ C54 C54A EADP C54 C54A EXYZ C56 C56A EADP C56 C56A EXYZ C57 C57A EADP C57 C57A SIZE 0.500 0.350 0.200 WGHT 0.057500 2.802200 FVAR 0.55851 0.71388 0.50798 0.56779 CL1 3 -0.198879 0.407674 0.566666 11.00000 0.10214 0.06142 = 0.03647 0.00535 0.01296 0.03400 F1 5 0.169313 0.053295 0.691990 11.00000 0.03813 0.02861 = 0.03327 -0.00129 0.01487 0.00479 F2 5 0.342198 0.010935 0.712041 11.00000 0.03373 0.03465 = 0.02589 0.00810 -0.00388 -0.00183 F3 5 0.066583 0.236277 0.301870 11.00000 0.02153 0.02477 = 0.03662 0.00285 -0.00262 -0.00094 F4 5 0.212017 0.255472 0.226524 11.00000 0.03408 0.02601 = 0.02013 0.00169 0.00182 0.00471 N1 6 0.306872 0.055351 0.594877 11.00000 0.02260 0.02022 = 0.02068 0.00150 0.00157 0.00308 N2 6 0.192536 -0.020626 0.620187 11.00000 0.02291 0.02180 = 0.02343 0.00445 0.00501 0.00217 N3 6 0.267627 0.212251 0.343002 11.00000 0.02308 0.01753 = 0.02042 0.00059 -0.00015 0.00114 N4 6 0.205745 0.300321 0.342960 11.00000 0.02350 0.01777 = 0.02109 0.00182 -0.00024 0.00209 C1 1 0.362407 0.099850 0.602387 11.00000 0.01995 0.01995 = 0.02375 0.00168 -0.00104 0.00429 C2 1 0.397724 0.114027 0.531787 11.00000 0.01884 0.01986 = 0.02417 0.00295 -0.00149 0.00272 C3 1 0.361009 0.078050 0.479594 11.00000 0.01818 0.01995 = 0.02315 0.00375 0.00083 0.00427 C4 1 0.304876 0.040642 0.519172 11.00000 0.02116 0.01954 = 0.02197 0.00177 0.00097 0.00480 C5 1 0.248456 -0.002933 0.494515 11.00000 0.01796 0.01920 = 0.02402 0.00185 0.00197 0.00475 C6 1 0.192009 -0.033072 0.543651 11.00000 0.02004 0.02056 = 0.02499 0.00126 0.00300 0.00321 C7 1 0.134199 -0.079395 0.533588 11.00000 0.02298 0.02161 = 0.03353 0.00198 0.00665 0.00248 C8 1 0.100812 -0.093455 0.603300 11.00000 0.02391 0.02227 = 0.03699 0.00518 0.00684 0.00228 C9 1 0.137853 -0.057334 0.656047 11.00000 0.02241 0.02530 = 0.02995 0.00815 0.00469 0.00498 C10 1 0.277441 0.163455 0.325669 11.00000 0.02153 0.01859 = 0.02101 0.00000 0.00352 0.00013 C11 1 0.349690 0.140507 0.382932 11.00000 0.02023 0.01962 = 0.02291 0.00310 0.00321 0.00079 C12 1 0.386621 0.175854 0.436101 11.00000 0.01959 0.01949 = 0.02191 0.00250 0.00033 -0.00032 C13 1 0.335654 0.221000 0.411277 11.00000 0.01957 0.02127 = 0.02047 0.00201 -0.00099 -0.00089 C14 1 0.343442 0.268122 0.443117 11.00000 0.02064 0.02175 = 0.02169 0.00222 0.00110 -0.00063 C15 1 0.280782 0.307261 0.409202 11.00000 0.02423 0.02305 = 0.02134 -0.00006 -0.00146 -0.00034 C16 1 0.272341 0.357613 0.429423 11.00000 0.03059 0.02139 = 0.02694 -0.00122 -0.00107 0.00062 C17 1 0.194855 0.379921 0.375877 11.00000 0.03105 0.02095 = 0.02824 -0.00129 -0.00099 0.00119 C18 1 0.153167 0.343986 0.323343 11.00000 0.02463 0.02028 = 0.02524 0.00275 0.00084 0.00182 C19 1 0.465795 0.156188 0.501651 11.00000 0.02068 0.02208 = 0.02537 0.00415 -0.00198 0.00040 AFIX 13 H19 2 0.489901 0.181800 0.540371 11.00000 -1.20000 AFIX 0 C20 1 0.573219 0.132311 0.465269 11.00000 0.02030 0.02951 = 0.03380 0.00710 0.00277 0.00138 AFIX 23 H20A 2 0.617461 0.158199 0.439903 11.00000 -1.20000 H20B 2 0.628251 0.117376 0.505165 11.00000 -1.20000 AFIX 0 C21 1 0.530846 0.092035 0.407151 11.00000 0.02429 0.02690 = 0.03245 0.00496 0.00740 0.00608 AFIX 23 H21A 2 0.564769 0.059675 0.423467 11.00000 -1.20000 H21B 2 0.559496 0.100093 0.357507 11.00000 -1.20000 AFIX 0 C22 1 0.391993 0.088981 0.400072 11.00000 0.02240 0.01955 = 0.02377 0.00265 0.00279 0.00220 AFIX 13 H22 2 0.359557 0.064099 0.362299 11.00000 -1.20000 AFIX 0 C23 1 0.376629 0.127892 0.674856 11.00000 0.02982 0.02590 = 0.02526 0.00039 0.00006 0.00066 AFIX 133 H23A 2 0.312960 0.152535 0.675763 11.00000 -1.50000 H23B 2 0.454273 0.144521 0.679188 11.00000 -1.50000 H23C 2 0.371976 0.105000 0.717118 11.00000 -1.50000 AFIX 0 C24 1 0.253345 -0.016870 0.414517 11.00000 0.02151 0.01703 = 0.02379 0.00204 0.00268 0.00135 C25 1 0.152956 -0.014752 0.363972 11.00000 0.02058 0.02979 = 0.02995 0.00009 0.00301 0.00258 AFIX 43 H25 2 0.077684 -0.006599 0.381233 11.00000 -1.20000 AFIX 0 C26 1 0.162305 -0.024531 0.288176 11.00000 0.02434 0.03587 = 0.02825 -0.00014 -0.00397 0.00166 AFIX 43 H26 2 0.092732 -0.023089 0.254222 11.00000 -1.20000 AFIX 0 C27 1 0.270716 -0.036354 0.260797 11.00000 0.02949 0.02278 = 0.02362 0.00116 0.00046 0.00155 C28 1 0.370148 -0.039776 0.312838 11.00000 0.02189 0.02336 = 0.02561 0.00018 0.00470 0.00468 AFIX 43 H28 2 0.445051 -0.048802 0.295863 11.00000 -1.20000 AFIX 0 C29 1 0.362076 -0.030358 0.388236 11.00000 0.02049 0.01949 = 0.02774 0.00228 0.00069 0.00322 AFIX 43 H29 2 0.431031 -0.033074 0.422513 11.00000 -1.20000 AFIX 0 C30 1 0.286250 -0.044189 0.177294 11.00000 0.03484 0.03602 = 0.02226 -0.00118 0.00023 0.00652 C31 1 0.376344 -0.006427 0.152142 11.00000 0.04273 0.05455 = 0.03012 0.00858 0.00655 0.00559 AFIX 133 H31A 2 0.348292 0.027008 0.162130 11.00000 -1.50000 H31B 2 0.384446 -0.010258 0.098095 11.00000 -1.50000 H31C 2 0.453917 -0.011878 0.180113 11.00000 -1.50000 AFIX 0 C32 1 0.169075 -0.037949 0.128920 11.00000 0.04079 0.04548 = 0.02395 -0.00212 -0.00458 0.00822 AFIX 133 H32A 2 0.111970 -0.062960 0.142983 11.00000 -1.50000 H32B 2 0.183261 -0.041915 0.075705 11.00000 -1.50000 H32C 2 0.136649 -0.004960 0.136968 11.00000 -1.50000 AFIX 0 C33 1 0.333623 -0.096608 0.165752 11.00000 0.05090 0.04821 = 0.02700 -0.00931 -0.00287 0.01576 AFIX 133 H33A 2 0.410361 -0.100732 0.195301 11.00000 -1.50000 H33B 2 0.344325 -0.101766 0.112272 11.00000 -1.50000 H33C 2 0.276403 -0.120767 0.182319 11.00000 -1.50000 AFIX 0 PART 1 ISOR 0.1 0.2 C34 > C37A DELU 0.005 C34 > C37A SIMU 0.005 0.01 C34 > C37A SADI 0.02 C7 C34 C7 C34A C8 C37 C8 C37A SAME 0.02 C34A C39A < C35A SAME 0.02 C37 C36 C35 C34 C39 C38 C37 C34 1 0.100091 -0.116002 0.473275 21.00000 0.02473 0.02164 = 0.03224 -0.00026 0.00541 -0.00115 AFIX 13 H34 2 0.129667 -0.107315 0.423513 21.00000 -1.20000 AFIX 0 C35 1 0.140101 -0.166698 0.501799 21.00000 0.02407 0.02240 = 0.03638 -0.00183 0.00031 -0.00361 AFIX 43 H35 2 0.186744 -0.187848 0.473405 21.00000 -1.20000 AFIX 0 C36 1 0.106326 -0.179724 0.568398 21.00000 0.02607 0.02383 = 0.03710 0.00509 -0.00190 -0.00294 AFIX 43 H36 2 0.125306 -0.210946 0.590541 21.00000 -1.20000 AFIX 0 C37 1 0.035664 -0.141350 0.606303 21.00000 0.02691 0.02652 = 0.03120 0.00543 0.00162 -0.00353 AFIX 13 H37 2 0.016290 -0.150834 0.658169 21.00000 -1.20000 AFIX 0 C38 1 -0.077402 -0.131656 0.550574 21.00000 0.02496 0.02857 = 0.03453 0.00552 0.00343 -0.00453 AFIX 23 H38A 2 -0.127332 -0.161785 0.546270 21.00000 -1.20000 H38B 2 -0.125526 -0.104731 0.570358 21.00000 -1.20000 AFIX 0 C39 1 -0.039180 -0.117231 0.472119 21.00000 0.02752 0.02899 = 0.03209 0.00347 0.00065 -0.00136 AFIX 23 H39A 2 -0.071982 -0.084330 0.457771 21.00000 -1.20000 H39B 2 -0.071616 -0.141452 0.434176 21.00000 -1.20000 AFIX 0 PART 2 SAME 0.02 C37A C36A C35A C34A C39A C38A C34A 1 0.085316 -0.110964 0.465905 -21.00000 0.02858 0.02053 = 0.03442 0.00144 0.00576 -0.00057 AFIX 13 H34A 2 0.105237 -0.096799 0.416631 -21.00000 -1.20000 AFIX 0 C35A 1 0.138484 -0.164408 0.480004 -21.00000 0.02508 0.02333 = 0.03457 0.00164 0.00123 -0.00404 AFIX 23 H35A 2 0.098651 -0.188144 0.443925 -21.00000 -1.20000 H35B 2 0.225021 -0.164501 0.473358 -21.00000 -1.20000 AFIX 0 C36A 1 0.116655 -0.178771 0.560757 -21.00000 0.02635 0.02400 = 0.03567 0.00333 -0.00097 -0.00254 AFIX 23 H36A 2 0.193333 -0.178969 0.592278 -21.00000 -1.20000 H36B 2 0.082394 -0.212427 0.561289 -21.00000 -1.20000 AFIX 0 C37A 1 0.027511 -0.140682 0.594548 -21.00000 0.02776 0.02562 = 0.03203 0.00675 0.00440 -0.00483 AFIX 13 H37A 2 0.000912 -0.152253 0.643789 -21.00000 -1.20000 AFIX 0 C38A 1 -0.075913 -0.137714 0.534056 -21.00000 0.01326 0.03706 = 0.04476 -0.01082 0.00154 0.00376 AFIX 43 H38C 2 -0.154750 -0.147489 0.542727 -21.00000 -1.20000 AFIX 0 C39A 1 -0.047317 -0.120447 0.468472 -21.00000 0.01110 0.05965 = 0.03750 0.00340 -0.00959 0.00091 AFIX 43 H39C 2 -0.104185 -0.114556 0.427033 -21.00000 -1.20000 AFIX 0 PART 0 C40 1 0.124438 -0.056474 0.738429 11.00000 0.03626 0.03417 = 0.02740 0.00910 0.00741 0.00064 AFIX 133 H40A 2 0.200810 -0.064891 0.765880 11.00000 -1.50000 H40B 2 0.063808 -0.080566 0.750441 11.00000 -1.50000 H40C 2 0.099861 -0.023398 0.753234 11.00000 -1.50000 AFIX 0 C41 1 0.217871 0.141069 0.255717 11.00000 0.03274 0.02015 = 0.02512 -0.00108 -0.00244 0.00126 AFIX 133 H41A 2 0.135292 0.152788 0.248520 11.00000 -1.50000 H41B 2 0.218431 0.105018 0.260440 11.00000 -1.50000 H41C 2 0.260826 0.150719 0.212317 11.00000 -1.50000 AFIX 0 C42 1 0.419890 0.274550 0.514873 11.00000 0.02460 0.01953 = 0.02188 -0.00048 -0.00166 -0.00010 C43 1 0.373580 0.267728 0.583597 11.00000 0.02333 0.03724 = 0.02557 0.00068 0.00050 -0.00064 AFIX 43 H43 2 0.290283 0.262526 0.585142 11.00000 -1.20000 AFIX 0 C44 1 0.445977 0.268312 0.650238 11.00000 0.02637 0.03681 = 0.02196 0.00035 0.00255 -0.00079 AFIX 43 H44 2 0.411237 0.263765 0.696596 11.00000 -1.20000 AFIX 0 C45 1 0.568096 0.275391 0.650790 11.00000 0.02534 0.02680 = 0.02408 -0.00149 -0.00107 -0.00116 C46 1 0.613916 0.283375 0.581116 11.00000 0.02436 0.04132 = 0.02756 0.00012 0.00114 -0.00779 AFIX 43 H46 2 0.696841 0.289497 0.579515 11.00000 -1.20000 AFIX 0 C47 1 0.541310 0.282581 0.514257 11.00000 0.02659 0.03492 = 0.02172 0.00181 0.00260 -0.00710 AFIX 43 H47 2 0.575239 0.287589 0.467734 11.00000 -1.20000 AFIX 0 C48 1 0.650358 0.275833 0.723654 11.00000 0.02820 0.04237 = 0.02354 -0.00010 -0.00251 -0.00383 C49 1 0.756074 0.241173 0.716473 11.00000 0.03573 0.06366 = 0.03799 0.00379 -0.00588 0.00769 AFIX 133 H49A 2 0.726832 0.207424 0.707566 11.00000 -1.50000 H49B 2 0.808722 0.242126 0.763078 11.00000 -1.50000 H49C 2 0.800452 0.251748 0.674171 11.00000 -1.50000 AFIX 0 C50 1 0.586244 0.259488 0.792102 11.00000 0.04178 0.06915 = 0.02354 0.00862 -0.00504 -0.00639 AFIX 133 H50A 2 0.553536 0.226258 0.783323 11.00000 -1.50000 H50B 2 0.521245 0.282553 0.799879 11.00000 -1.50000 H50C 2 0.642932 0.259194 0.836898 11.00000 -1.50000 AFIX 0 C51 1 0.694994 0.328732 0.737453 11.00000 0.04802 0.05231 = 0.03322 -0.00670 -0.00913 -0.01388 AFIX 133 H51A 2 0.749910 0.329662 0.783061 11.00000 -1.50000 H51B 2 0.626992 0.350522 0.743840 11.00000 -1.50000 H51C 2 0.736645 0.339865 0.694290 11.00000 -1.50000 AFIX 0 C52 1 0.320220 0.391256 0.491554 11.00000 0.03554 0.02307 = 0.03001 -0.00406 -0.00665 0.00128 AFIX 13 H52 2 0.375554 0.374239 0.530031 11.00000 -1.20000 AFIX 0 PART 1 C53 1 0.210093 0.413134 0.524616 31.00000 0.03727 0.03140 = 0.02785 -0.00450 0.00434 -0.00273 AFIX 43 H53 2 0.195323 0.410661 0.576232 31.00000 -1.20000 AFIX 0 C54 1 0.131910 0.437720 0.469092 31.00000 0.03546 0.02853 = 0.04367 -0.00702 0.00875 0.00003 AFIX 43 H54 2 0.061233 0.454492 0.480138 31.00000 -1.20000 AFIX 0 C56 1 0.298894 0.457799 0.396241 31.00000 0.04312 0.02433 = 0.03607 0.00207 0.00552 -0.00347 AFIX 23 H56A 2 0.333271 0.456085 0.346888 31.00000 -1.20000 H56B 2 0.290861 0.493076 0.409476 31.00000 -1.20000 AFIX 0 C57 1 0.379287 0.434123 0.452475 31.00000 0.03322 0.03261 = 0.03755 -0.00626 0.00266 -0.00735 AFIX 23 H57A 2 0.407861 0.458826 0.490749 31.00000 -1.20000 H57B 2 0.449476 0.421547 0.428302 31.00000 -1.20000 AFIX 0 PART 2 C53A 1 0.210093 0.413134 0.524616 -31.00000 0.03727 0.03140 = 0.02785 -0.00450 0.00434 -0.00273 AFIX 23 H53A 2 0.165739 0.386321 0.547779 -31.00000 -1.20000 H53B 2 0.236317 0.436912 0.564815 -31.00000 -1.20000 AFIX 0 C54A 1 0.131910 0.437720 0.469092 -31.00000 0.03546 0.02853 = 0.04367 -0.00702 0.00875 0.00003 AFIX 23 H54A 2 0.125822 0.472978 0.482928 -31.00000 -1.20000 H54B 2 0.051256 0.423047 0.468813 -31.00000 -1.20000 AFIX 0 C56A 1 0.298894 0.457799 0.396241 -31.00000 0.04312 0.02433 = 0.03607 0.00207 0.00552 -0.00347 AFIX 43 H56C 2 0.320360 0.485148 0.366810 -31.00000 -1.20000 AFIX 0 C57A 1 0.379287 0.434123 0.452475 -31.00000 0.03322 0.03261 = 0.03755 -0.00626 0.00266 -0.00735 AFIX 43 H57C 2 0.459761 0.444004 0.463965 -31.00000 -1.20000 AFIX 0 PART 0 C55 1 0.175343 0.433904 0.389391 11.00000 0.04021 0.02135 = 0.03501 -0.00181 -0.00526 0.00399 AFIX 13 H55 2 0.119415 0.449569 0.349833 11.00000 -1.20000 AFIX 0 C58 1 0.062229 0.349123 0.258231 11.00000 0.03008 0.02226 = 0.02787 0.00323 -0.00207 0.00283 AFIX 123 H58A 2 0.052332 0.317395 0.232019 10.50000 -1.50000 H58B 2 0.088553 0.374136 0.223452 10.50000 -1.50000 H58C 2 -0.014048 0.359219 0.276372 10.50000 -1.50000 H58D 2 0.032226 0.383105 0.255876 10.50000 -1.50000 H58E 2 -0.003995 0.326364 0.264443 10.50000 -1.50000 H58F 2 0.098606 0.341281 0.211524 10.50000 -1.50000 AFIX 0 C59 1 -0.106778 0.358296 0.548890 11.00000 0.04570 0.04237 = 0.03366 0.00608 0.00820 0.00147 C60 1 -0.100292 0.342709 0.475111 11.00000 0.05978 0.04051 = 0.03123 0.00577 0.00751 0.00137 AFIX 43 H60 2 -0.145975 0.358698 0.434990 11.00000 -1.20000 AFIX 0 C61 1 -0.027177 0.303985 0.460950 11.00000 0.05191 0.03616 = 0.03607 -0.00296 0.00987 -0.01172 AFIX 43 H61 2 -0.020503 0.293434 0.410610 11.00000 -1.20000 AFIX 0 C62 1 0.036944 0.280218 0.519792 11.00000 0.03373 0.04008 = 0.05516 -0.00611 0.00177 -0.00594 AFIX 43 H62 2 0.087788 0.253409 0.509802 11.00000 -1.20000 AFIX 0 C63 1 0.027358 0.295236 0.592558 11.00000 0.03257 0.04853 = 0.04229 -0.00077 -0.00458 0.00049 AFIX 43 H63 2 0.070047 0.278168 0.632821 11.00000 -1.20000 AFIX 0 C64 1 -0.043294 0.334669 0.607727 11.00000 0.04294 0.05266 = 0.03244 -0.00366 -0.00126 -0.00440 AFIX 43 H64 2 -0.048367 0.345525 0.658074 11.00000 -1.20000 AFIX 0 B1 4 0.253299 0.025403 0.657838 11.00000 0.02481 0.02404 = 0.02228 0.00327 0.00387 0.00146 B2 4 0.185337 0.250693 0.301043 11.00000 0.02125 0.02108 = 0.02041 0.00054 0.00095 0.00010 HKLF 4 REM transBCODBisbenzoBODIPY REM R1 = 0.0619 for 9355 Fo > 4sig(Fo) and 0.0860 for all 12378 data REM 733 parameters refined using 243 restraints END WGHT 0.0579 2.8053 REM Highest difference peak 0.300, deepest hole -0.763, 1-sigma level 0.053 Q1 1 -0.0908 0.3889 0.5778 11.00000 0.05 0.30 Q2 1 0.3950 0.0938 0.5036 11.00000 0.05 0.25 Q3 1 -0.1240 0.3106 0.4423 11.00000 0.05 0.25 Q4 1 0.2486 -0.0103 0.4555 11.00000 0.05 0.24 Q5 1 0.3769 0.0829 0.4362 11.00000 0.05 0.24 Q6 1 0.1080 -0.0853 0.5671 11.00000 0.05 0.23 Q7 1 0.3164 0.2894 0.4216 11.00000 0.05 0.22 Q8 1 0.2795 -0.0384 0.2247 11.00000 0.05 0.21 Q9 1 0.3104 -0.0342 0.2849 11.00000 0.05 0.21 Q10 1 0.1053 -0.0876 0.5009 11.00000 0.05 0.21 Q11 1 0.1534 0.3631 0.3556 11.00000 0.05 0.21 Q12 1 0.3776 0.1118 0.5646 11.00000 0.05 0.20 Q13 1 0.5601 0.2582 0.3985 11.00000 0.05 0.20 Q14 1 0.2303 0.2288 0.3224 11.00000 0.05 0.20 Q15 1 0.4193 0.2632 0.5197 11.00000 0.05 0.20 Q16 1 0.2220 -0.0146 0.5199 11.00000 0.05 0.20 Q17 1 0.2149 0.3705 0.4028 11.00000 0.05 0.20 Q18 1 0.3679 0.1556 0.4194 11.00000 0.05 0.20 Q19 1 -0.0917 0.4244 0.5696 11.00000 0.05 0.20 Q20 1 0.0837 -0.0731 0.6272 11.00000 0.05 0.19 Q21 1 0.3384 0.0544 0.4945 11.00000 0.05 0.19 Q22 1 0.2915 0.0491 0.6179 11.00000 0.05 0.19 Q23 1 0.4373 0.1674 0.4789 11.00000 0.05 0.19 Q24 1 0.2328 -0.0022 0.6360 11.00000 0.05 0.19 Q25 1 0.1925 0.2793 0.3264 11.00000 0.05 0.19 ; 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.0013 0.0007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl1 Cl -0.19888(9) 0.40767(3) 0.56667(4) 0.0663(3) Uani 1 1 d . . . F1 F 0.16931(11) 0.05329(5) 0.69199(7) 0.0327(3) Uani 1 1 d . A . F2 F 0.34220(11) 0.01094(5) 0.71204(7) 0.0318(3) Uani 1 1 d . A . F3 F 0.06658(10) 0.23628(4) 0.30187(7) 0.0279(3) Uani 1 1 d . . . F4 F 0.21202(11) 0.25547(4) 0.22652(6) 0.0268(3) Uani 1 1 d . . . N1 N 0.30687(15) 0.05535(6) 0.59488(9) 0.0212(3) Uani 1 1 d . A . N2 N 0.19254(15) -0.02063(6) 0.62019(9) 0.0225(4) Uani 1 1 d . A . N3 N 0.26763(14) 0.21225(6) 0.34300(9) 0.0204(3) Uani 1 1 d . . . N4 N 0.20574(15) 0.30032(6) 0.34296(9) 0.0209(3) Uani 1 1 d . . . C1 C 0.36241(17) 0.09985(7) 0.60239(11) 0.0214(4) Uani 1 1 d . . . C2 C 0.39772(17) 0.11403(7) 0.53179(11) 0.0211(4) Uani 1 1 d . . . C3 C 0.36101(17) 0.07805(7) 0.47959(11) 0.0205(4) Uani 1 1 d . . . C4 C 0.30488(17) 0.04064(7) 0.51917(11) 0.0209(4) Uani 1 1 d . . . C5 C 0.24846(17) -0.00293(7) 0.49452(11) 0.0204(4) Uani 1 1 d . . . C6 C 0.19201(17) -0.03307(7) 0.54365(11) 0.0218(4) Uani 1 1 d . A . C7 C 0.13420(18) -0.07939(8) 0.53359(12) 0.0258(4) Uani 1 1 d D . . C8 C 0.10081(19) -0.09346(8) 0.60330(13) 0.0275(5) Uani 1 1 d D A . C9 C 0.13785(18) -0.05733(8) 0.65605(12) 0.0257(4) Uani 1 1 d . . . C10 C 0.27744(17) 0.16346(7) 0.32567(11) 0.0203(4) Uani 1 1 d . . . C11 C 0.34969(17) 0.14051(7) 0.38293(11) 0.0208(4) Uani 1 1 d . . . C12 C 0.38662(17) 0.17585(7) 0.43610(11) 0.0204(4) Uani 1 1 d . . . C13 C 0.33565(17) 0.22100(7) 0.41128(11) 0.0206(4) Uani 1 1 d . . . C14 C 0.34344(17) 0.26812(7) 0.44312(11) 0.0214(4) Uani 1 1 d . . . C15 C 0.28078(18) 0.30726(7) 0.40920(11) 0.0231(4) Uani 1 1 d . . . C16 C 0.27234(19) 0.35761(8) 0.42942(12) 0.0265(4) Uani 1 1 d . C . C17 C 0.19485(19) 0.37992(8) 0.37588(12) 0.0269(5) Uani 1 1 d . C . C18 C 0.15317(18) 0.34399(7) 0.32334(11) 0.0234(4) Uani 1 1 d . . . C19 C 0.46580(17) 0.15619(7) 0.50165(11) 0.0229(4) Uani 1 1 d . . . H19 H 0.4899 0.1818 0.5404 0.028 Uiso 1 1 calc R . . C20 C 0.57322(18) 0.13231(8) 0.46527(12) 0.0278(5) Uani 1 1 d . . . H20A H 0.6175 0.1582 0.4399 0.033 Uiso 1 1 calc R . . H20B H 0.6283 0.1174 0.5052 0.033 Uiso 1 1 calc R . . C21 C 0.53085(18) 0.09203(8) 0.40715(12) 0.0276(5) Uani 1 1 d . . . H21A H 0.5648 0.0597 0.4235 0.033 Uiso 1 1 calc R . . H21B H 0.5595 0.1001 0.3575 0.033 Uiso 1 1 calc R . . C22 C 0.39199(17) 0.08898(7) 0.40007(11) 0.0219(4) Uani 1 1 d . . . H22 H 0.3596 0.0641 0.3623 0.026 Uiso 1 1 calc R . . C23 C 0.37663(19) 0.12789(8) 0.67486(11) 0.0271(5) Uani 1 1 d . . . H23A H 0.3130 0.1525 0.6758 0.041 Uiso 1 1 calc R . . H23B H 0.4543 0.1445 0.6792 0.041 Uiso 1 1 calc R . . H23C H 0.3720 0.1050 0.7171 0.041 Uiso 1 1 calc R . . C24 C 0.25335(17) -0.01687(7) 0.41452(11) 0.0207(4) Uani 1 1 d . . . C25 C 0.15296(19) -0.01475(8) 0.36397(12) 0.0267(4) Uani 1 1 d . . . H25 H 0.0777 -0.0066 0.3812 0.032 Uiso 1 1 calc R . . C26 C 0.16231(19) -0.02453(8) 0.28818(12) 0.0298(5) Uani 1 1 d . . . H26 H 0.0927 -0.0231 0.2542 0.036 Uiso 1 1 calc R . . C27 C 0.27072(19) -0.03635(8) 0.26080(11) 0.0254(4) Uani 1 1 d . . . C28 C 0.37015(18) -0.03978(7) 0.31284(11) 0.0235(4) Uani 1 1 d . . . H28 H 0.4451 -0.0488 0.2959 0.028 Uiso 1 1 calc R . . C29 C 0.36208(18) -0.03036(7) 0.38824(11) 0.0226(4) Uani 1 1 d . . . H29 H 0.4310 -0.0331 0.4225 0.027 Uiso 1 1 calc R . . C30 C 0.2863(2) -0.04419(9) 0.17729(12) 0.0312(5) Uani 1 1 d . . . C31 C 0.3763(2) -0.00643(10) 0.15214(14) 0.0423(6) Uani 1 1 d . . . H31A H 0.3483 0.0270 0.1621 0.063 Uiso 1 1 calc R . . H31B H 0.3844 -0.0103 0.0981 0.063 Uiso 1 1 calc R . . H31C H 0.4539 -0.0119 0.1801 0.063 Uiso 1 1 calc R . . C32 C 0.1691(2) -0.03795(10) 0.12892(13) 0.0371(6) Uani 1 1 d . . . H32A H 0.1120 -0.0630 0.1430 0.056 Uiso 1 1 calc R . . H32B H 0.1833 -0.0419 0.0757 0.056 Uiso 1 1 calc R . . H32C H 0.1366 -0.0050 0.1370 0.056 Uiso 1 1 calc R . . C33 C 0.3336(2) -0.09661(10) 0.16575(13) 0.0424(6) Uani 1 1 d . . . H33A H 0.4104 -0.1007 0.1953 0.064 Uiso 1 1 calc R . . H33B H 0.3443 -0.1018 0.1123 0.064 Uiso 1 1 calc R . . H33C H 0.2764 -0.1208 0.1823 0.064 Uiso 1 1 calc R . . C34 C 0.1001(6) -0.1160(2) 0.4733(4) 0.0260(9) Uani 0.714(13) 1 d PDU A 1 H34 H 0.1297 -0.1073 0.4235 0.031 Uiso 0.714(13) 1 calc PR A 1 C35 C 0.1401(4) -0.16670(17) 0.5018(3) 0.0277(9) Uani 0.714(13) 1 d PDU A 1 H35 H 0.1867 -0.1878 0.4734 0.033 Uiso 0.714(13) 1 calc PR A 1 C36 C 0.1063(7) -0.1797(3) 0.5684(5) 0.0292(9) Uani 0.714(13) 1 d PDU A 1 H36 H 0.1253 -0.2109 0.5905 0.035 Uiso 0.714(13) 1 calc PR A 1 C37 C 0.0357(6) -0.1413(2) 0.6063(4) 0.0282(9) Uani 0.714(13) 1 d PDU A 1 H37 H 0.0163 -0.1508 0.6582 0.034 Uiso 0.714(13) 1 calc PR A 1 C38 C -0.0774(7) -0.1317(3) 0.5506(4) 0.0293(12) Uani 0.714(13) 1 d PDU A 1 H38A H -0.1273 -0.1618 0.5463 0.035 Uiso 0.714(13) 1 calc PR A 1 H38B H -0.1255 -0.1047 0.5704 0.035 Uiso 0.714(13) 1 calc PR A 1 C39 C -0.0392(7) -0.1172(4) 0.4721(6) 0.0296(14) Uani 0.714(13) 1 d PDU A 1 H39A H -0.0720 -0.0843 0.4578 0.036 Uiso 0.714(13) 1 calc PR A 1 H39B H -0.0716 -0.1415 0.4342 0.036 Uiso 0.714(13) 1 calc PR A 1 C34A C 0.0853(16) -0.1110(5) 0.4659(9) 0.0277(15) Uani 0.286(13) 1 d PDU A 2 H34A H 0.1052 -0.0968 0.4166 0.033 Uiso 0.286(13) 1 calc PR A 2 C35A C 0.1385(8) -0.1644(4) 0.4800(8) 0.0277(13) Uani 0.286(13) 1 d PDU A 2 H35A H 0.0987 -0.1881 0.4439 0.033 Uiso 0.286(13) 1 calc PR A 2 H35B H 0.2250 -0.1645 0.4734 0.033 Uiso 0.286(13) 1 calc PR A 2 C36A C 0.1167(19) -0.1788(9) 0.5608(13) 0.0289(13) Uani 0.286(13) 1 d PDU A 2 H36A H 0.1933 -0.1790 0.5923 0.035 Uiso 0.286(13) 1 calc PR A 2 H36B H 0.0824 -0.2124 0.5613 0.035 Uiso 0.286(13) 1 calc PR A 2 C37A C 0.0275(16) -0.1407(6) 0.5945(10) 0.0284(14) Uani 0.286(13) 1 d PDU A 2 H37A H 0.0009 -0.1523 0.6438 0.034 Uiso 0.286(13) 1 calc PR A 2 C38A C -0.0759(15) -0.1377(8) 0.5341(10) 0.032(4) Uani 0.286(13) 1 d PD A 2 H38C H -0.1547 -0.1475 0.5427 0.038 Uiso 0.286(13) 1 calc PR A 2 C39A C -0.0473(17) -0.1204(11) 0.4685(15) 0.037(5) Uani 0.286(13) 1 d PD A 2 H39C H -0.1042 -0.1146 0.4270 0.044 Uiso 0.286(13) 1 calc PR A 2 C40 C 0.1244(2) -0.05647(9) 0.73843(12) 0.0323(5) Uani 1 1 d . A . H40A H 0.2008 -0.0649 0.7659 0.049 Uiso 1 1 calc R . . H40B H 0.0638 -0.0806 0.7504 0.049 Uiso 1 1 calc R . . H40C H 0.0999 -0.0234 0.7532 0.049 Uiso 1 1 calc R . . C41 C 0.21787(19) 0.14107(7) 0.25572(11) 0.0263(4) Uani 1 1 d . . . H41A H 0.1353 0.1528 0.2485 0.039 Uiso 1 1 calc R . . H41B H 0.2184 0.1050 0.2604 0.039 Uiso 1 1 calc R . . H41C H 0.2608 0.1507 0.2123 0.039 Uiso 1 1 calc R . . C42 C 0.41989(18) 0.27455(7) 0.51487(11) 0.0222(4) Uani 1 1 d . . . C43 C 0.37358(19) 0.26773(8) 0.58360(12) 0.0288(5) Uani 1 1 d . . . H43 H 0.2903 0.2625 0.5851 0.035 Uiso 1 1 calc R . . C44 C 0.44598(19) 0.26831(8) 0.65024(12) 0.0283(5) Uani 1 1 d . . . H44 H 0.4112 0.2638 0.6966 0.034 Uiso 1 1 calc R . . C45 C 0.56810(18) 0.27539(8) 0.65079(11) 0.0256(4) Uani 1 1 d . . . C46 C 0.6139(2) 0.28338(9) 0.58112(12) 0.0311(5) Uani 1 1 d . . . H46 H 0.6968 0.2895 0.5795 0.037 Uiso 1 1 calc R . . C47 C 0.54131(19) 0.28258(8) 0.51426(12) 0.0277(5) Uani 1 1 d . . . H47 H 0.5752 0.2876 0.4677 0.033 Uiso 1 1 calc R . . C48 C 0.6504(2) 0.27583(9) 0.72365(12) 0.0316(5) Uani 1 1 d . . . C49 C 0.7561(2) 0.24117(11) 0.71647(15) 0.0463(7) Uani 1 1 d . . . H49A H 0.7268 0.2074 0.7076 0.069 Uiso 1 1 calc R . . H49B H 0.8087 0.2421 0.7631 0.069 Uiso 1 1 calc R . . H49C H 0.8005 0.2517 0.6742 0.069 Uiso 1 1 calc R . . C50 C 0.5862(2) 0.25949(11) 0.79210(13) 0.0452(7) Uani 1 1 d . . . H50A H 0.5535 0.2263 0.7833 0.068 Uiso 1 1 calc R . . H50B H 0.5212 0.2826 0.7999 0.068 Uiso 1 1 calc R . . H50C H 0.6429 0.2592 0.8369 0.068 Uiso 1 1 calc R . . C51 C 0.6950(2) 0.32873(10) 0.73745(14) 0.0452(6) Uani 1 1 d . . . H51A H 0.7499 0.3297 0.7831 0.068 Uiso 1 1 calc R . . H51B H 0.6270 0.3505 0.7438 0.068 Uiso 1 1 calc R . . H51C H 0.7366 0.3399 0.6943 0.068 Uiso 1 1 calc R . . C52 C 0.3202(2) 0.39126(8) 0.49155(12) 0.0300(5) Uani 1 1 d . . . H52 H 0.3756 0.3742 0.5300 0.036 Uiso 1 1 calc R B 1 C53 C 0.2101(2) 0.41313(8) 0.52462(13) 0.0321(5) Uani 0.508(16) 1 d P C 1 H53 H 0.1953 0.4107 0.5762 0.038 Uiso 0.508(16) 1 calc PR C 1 C54 C 0.1319(2) 0.43772(9) 0.46909(14) 0.0356(5) Uani 0.508(16) 1 d P C 1 H54 H 0.0612 0.4545 0.4801 0.043 Uiso 0.508(16) 1 calc PR C 1 C56 C 0.2989(2) 0.45780(8) 0.39624(13) 0.0344(5) Uani 0.508(16) 1 d P C 1 H56A H 0.3333 0.4561 0.3469 0.041 Uiso 0.508(16) 1 calc PR C 1 H56B H 0.2909 0.4931 0.4095 0.041 Uiso 0.508(16) 1 calc PR C 1 C57 C 0.3793(2) 0.43412(8) 0.45247(13) 0.0345(5) Uani 0.508(16) 1 d P C 1 H57A H 0.4079 0.4588 0.4907 0.041 Uiso 0.508(16) 1 calc PR C 1 H57B H 0.4495 0.4215 0.4283 0.041 Uiso 0.508(16) 1 calc PR C 1 C53A C 0.2101(2) 0.41313(8) 0.52462(13) 0.0321(5) Uani 0.492(16) 1 d P C 2 H53A H 0.1657 0.3863 0.5478 0.038 Uiso 0.492(16) 1 calc PR C 2 H53B H 0.2363 0.4369 0.5648 0.038 Uiso 0.492(16) 1 calc PR C 2 C54A C 0.1319(2) 0.43772(9) 0.46909(14) 0.0356(5) Uani 0.492(16) 1 d P C 2 H54A H 0.1258 0.4730 0.4829 0.043 Uiso 0.492(16) 1 calc PR C 2 H54B H 0.0513 0.4230 0.4688 0.043 Uiso 0.492(16) 1 calc PR C 2 C56A C 0.2989(2) 0.45780(8) 0.39624(13) 0.0344(5) Uani 0.492(16) 1 d P C 2 H56C H 0.3204 0.4851 0.3668 0.041 Uiso 0.492(16) 1 calc PR C 2 C57A C 0.3793(2) 0.43412(8) 0.45247(13) 0.0345(5) Uani 0.492(16) 1 d P C 2 H57C H 0.4598 0.4440 0.4640 0.041 Uiso 0.492(16) 1 calc PR C 2 C55 C 0.1753(2) 0.43390(8) 0.38939(13) 0.0326(5) Uani 1 1 d . . . H55 H 0.1194 0.4496 0.3498 0.039 Uiso 1 1 calc R C 1 C58 C 0.06223(19) 0.34912(8) 0.25823(12) 0.0270(5) Uani 1 1 d . . . H58A H 0.0523 0.3174 0.2320 0.040 Uiso 0.50 1 calc PR . . H58B H 0.0886 0.3741 0.2235 0.040 Uiso 0.50 1 calc PR . . H58C H -0.0140 0.3592 0.2764 0.040 Uiso 0.50 1 calc PR . . H58D H 0.0322 0.3831 0.2559 0.040 Uiso 0.50 1 calc PR . . H58E H -0.0040 0.3264 0.2644 0.040 Uiso 0.50 1 calc PR . . H58F H 0.0986 0.3413 0.2115 0.040 Uiso 0.50 1 calc PR . . C59 C -0.1068(2) 0.35830(10) 0.54889(14) 0.0403(6) Uani 1 1 d . . . C60 C -0.1003(3) 0.34271(10) 0.47511(14) 0.0436(6) Uani 1 1 d . . . H60 H -0.1460 0.3587 0.4350 0.052 Uiso 1 1 calc R . . C61 C -0.0272(2) 0.30398(9) 0.46095(14) 0.0410(6) Uani 1 1 d . . . H61 H -0.0205 0.2934 0.4106 0.049 Uiso 1 1 calc R . . C62 C 0.0369(2) 0.28022(10) 0.51979(16) 0.0431(6) Uani 1 1 d . . . H62 H 0.0878 0.2534 0.5098 0.052 Uiso 1 1 calc R . . C63 C 0.0274(2) 0.29524(10) 0.59256(15) 0.0415(6) Uani 1 1 d . . . H63 H 0.0700 0.2782 0.6328 0.050 Uiso 1 1 calc R . . C64 C -0.0433(2) 0.33467(10) 0.60773(14) 0.0429(6) Uani 1 1 d . . . H64 H -0.0484 0.3455 0.6581 0.052 Uiso 1 1 calc R . . B2 B 0.1853(2) 0.25069(8) 0.30104(12) 0.0210(4) Uani 1 1 d . . . B1 B 0.2533(2) 0.02540(9) 0.65784(13) 0.0236(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.1021(7) 0.0614(5) 0.0365(4) 0.0054(3) 0.0130(4) 0.0340(5) F1 0.0381(7) 0.0286(7) 0.0333(7) -0.0013(5) 0.0149(6) 0.0048(6) F2 0.0337(7) 0.0346(7) 0.0259(6) 0.0081(5) -0.0039(5) -0.0018(6) F3 0.0215(6) 0.0248(6) 0.0366(7) 0.0029(5) -0.0026(5) -0.0009(5) F4 0.0341(7) 0.0260(6) 0.0201(6) 0.0017(5) 0.0018(5) 0.0047(5) N1 0.0226(8) 0.0202(8) 0.0207(8) 0.0015(6) 0.0016(7) 0.0031(7) N2 0.0229(9) 0.0218(8) 0.0234(8) 0.0045(7) 0.0050(7) 0.0022(7) N3 0.0231(8) 0.0175(8) 0.0204(8) 0.0006(6) -0.0001(7) 0.0011(7) N4 0.0235(9) 0.0178(8) 0.0211(8) 0.0018(6) -0.0002(7) 0.0021(7) C1 0.0199(9) 0.0199(9) 0.0237(10) 0.0017(8) -0.0010(8) 0.0043(8) C2 0.0188(9) 0.0199(9) 0.0242(10) 0.0029(8) -0.0015(8) 0.0027(8) C3 0.0182(9) 0.0199(9) 0.0232(10) 0.0038(8) 0.0008(7) 0.0043(8) C4 0.0212(10) 0.0195(9) 0.0220(9) 0.0018(7) 0.0010(8) 0.0048(8) C5 0.0180(9) 0.0192(9) 0.0240(10) 0.0018(8) 0.0020(8) 0.0048(8) C6 0.0200(10) 0.0206(10) 0.0250(10) 0.0013(8) 0.0030(8) 0.0032(8) C7 0.0230(10) 0.0216(10) 0.0335(11) 0.0020(8) 0.0067(9) 0.0025(8) C8 0.0239(10) 0.0223(10) 0.0370(12) 0.0052(9) 0.0068(9) 0.0023(9) C9 0.0224(10) 0.0253(10) 0.0299(11) 0.0081(9) 0.0047(8) 0.0050(9) C10 0.0215(10) 0.0186(9) 0.0210(9) 0.0000(7) 0.0035(8) 0.0001(8) C11 0.0202(9) 0.0196(9) 0.0229(9) 0.0031(8) 0.0032(8) 0.0008(8) C12 0.0196(9) 0.0195(9) 0.0219(9) 0.0025(7) 0.0003(8) -0.0003(8) C13 0.0196(9) 0.0213(9) 0.0205(9) 0.0020(8) -0.0010(7) -0.0009(8) C14 0.0206(10) 0.0218(10) 0.0217(9) 0.0022(8) 0.0011(8) -0.0006(8) C15 0.0242(10) 0.0231(10) 0.0213(9) -0.0001(8) -0.0015(8) -0.0003(8) C16 0.0306(11) 0.0214(10) 0.0269(10) -0.0012(8) -0.0011(9) 0.0006(9) C17 0.0311(11) 0.0209(10) 0.0282(11) -0.0013(8) -0.0010(9) 0.0012(9) C18 0.0246(10) 0.0203(10) 0.0252(10) 0.0027(8) 0.0008(8) 0.0018(8) C19 0.0207(10) 0.0221(10) 0.0254(10) 0.0041(8) -0.0020(8) 0.0004(8) C20 0.0203(10) 0.0295(11) 0.0338(11) 0.0071(9) 0.0028(9) 0.0014(9) C21 0.0243(11) 0.0269(11) 0.0324(11) 0.0050(9) 0.0074(9) 0.0061(9) C22 0.0224(10) 0.0195(9) 0.0238(10) 0.0026(8) 0.0028(8) 0.0022(8) C23 0.0298(11) 0.0259(11) 0.0253(10) 0.0004(8) 0.0001(9) 0.0007(9) C24 0.0215(10) 0.0170(9) 0.0238(10) 0.0020(7) 0.0027(8) 0.0014(8) C25 0.0206(10) 0.0298(11) 0.0300(11) 0.0001(9) 0.0030(8) 0.0026(9) C26 0.0243(11) 0.0359(12) 0.0282(11) -0.0001(9) -0.0040(9) 0.0017(9) C27 0.0295(11) 0.0228(10) 0.0236(10) 0.0012(8) 0.0005(8) 0.0016(9) C28 0.0219(10) 0.0234(10) 0.0256(10) 0.0002(8) 0.0047(8) 0.0047(8) C29 0.0205(10) 0.0195(9) 0.0277(10) 0.0023(8) 0.0007(8) 0.0032(8) C30 0.0348(12) 0.0360(12) 0.0223(10) -0.0012(9) 0.0002(9) 0.0065(10) C31 0.0427(14) 0.0545(16) 0.0301(12) 0.0086(11) 0.0065(11) 0.0056(13) C32 0.0408(13) 0.0455(14) 0.0240(11) -0.0021(10) -0.0046(10) 0.0082(12) C33 0.0509(15) 0.0482(15) 0.0270(12) -0.0093(11) -0.0029(11) 0.0158(13) C34 0.0247(19) 0.0216(16) 0.0322(17) -0.0003(14) 0.0054(14) -0.0011(14) C35 0.0241(13) 0.0224(13) 0.036(2) -0.0018(15) 0.0003(14) -0.0036(11) C36 0.0261(17) 0.0238(13) 0.037(2) 0.0051(13) -0.0019(14) -0.0029(14) C37 0.0269(16) 0.0265(14) 0.031(2) 0.0054(14) 0.0016(15) -0.0035(13) C38 0.0250(19) 0.029(2) 0.035(2) 0.006(2) 0.0034(16) -0.0045(16) C39 0.028(3) 0.029(2) 0.032(3) 0.003(2) 0.001(2) -0.001(2) C34A 0.029(3) 0.021(3) 0.034(3) 0.001(2) 0.006(3) -0.001(3) C35A 0.025(2) 0.023(2) 0.035(3) 0.002(2) 0.001(2) -0.0040(19) C36A 0.026(2) 0.024(2) 0.036(3) 0.003(2) -0.001(2) -0.003(2) C37A 0.028(2) 0.026(2) 0.032(3) 0.007(2) 0.004(2) -0.005(2) C38A 0.013(5) 0.037(7) 0.045(9) -0.011(6) 0.002(5) 0.004(4) C39A 0.011(6) 0.060(13) 0.037(8) 0.003(8) -0.010(6) 0.001(7) C40 0.0363(12) 0.0342(12) 0.0274(11) 0.0091(9) 0.0074(9) 0.0006(10) C41 0.0327(11) 0.0202(10) 0.0251(10) -0.0011(8) -0.0024(9) 0.0013(9) C42 0.0246(10) 0.0195(9) 0.0219(10) -0.0005(8) -0.0017(8) -0.0001(8) C43 0.0233(10) 0.0372(12) 0.0256(10) 0.0007(9) 0.0005(8) -0.0006(9) C44 0.0264(11) 0.0368(12) 0.0220(10) 0.0003(9) 0.0026(8) -0.0008(10) C45 0.0253(11) 0.0268(11) 0.0241(10) -0.0015(8) -0.0011(8) -0.0012(9) C46 0.0244(11) 0.0413(13) 0.0276(11) 0.0001(10) 0.0011(9) -0.0078(10) C47 0.0266(11) 0.0349(12) 0.0217(10) 0.0018(9) 0.0026(8) -0.0071(9) C48 0.0282(11) 0.0424(13) 0.0235(10) -0.0001(9) -0.0025(9) -0.0038(10) C49 0.0357(14) 0.0637(18) 0.0380(14) 0.0038(13) -0.0059(11) 0.0077(13) C50 0.0418(14) 0.0692(19) 0.0235(11) 0.0086(12) -0.0050(10) -0.0064(13) C51 0.0480(15) 0.0523(16) 0.0332(13) -0.0067(11) -0.0091(11) -0.0139(13) C52 0.0355(12) 0.0231(10) 0.0300(11) -0.0041(9) -0.0066(9) 0.0013(9) C53 0.0373(13) 0.0314(12) 0.0278(11) -0.0045(9) 0.0043(9) -0.0027(10) C54 0.0355(13) 0.0285(12) 0.0437(14) -0.0070(10) 0.0088(10) 0.0000(10) C56 0.0431(14) 0.0243(11) 0.0361(13) 0.0021(9) 0.0055(10) -0.0035(10) C57 0.0332(12) 0.0326(12) 0.0375(13) -0.0063(10) 0.0027(10) -0.0073(10) C53A 0.0373(13) 0.0314(12) 0.0278(11) -0.0045(9) 0.0043(9) -0.0027(10) C54A 0.0355(13) 0.0285(12) 0.0437(14) -0.0070(10) 0.0088(10) 0.0000(10) C56A 0.0431(14) 0.0243(11) 0.0361(13) 0.0021(9) 0.0055(10) -0.0035(10) C57A 0.0332(12) 0.0326(12) 0.0375(13) -0.0063(10) 0.0027(10) -0.0073(10) C55 0.0402(13) 0.0214(10) 0.0350(12) -0.0018(9) -0.0053(10) 0.0040(10) C58 0.0301(11) 0.0223(10) 0.0279(11) 0.0032(8) -0.0021(9) 0.0028(9) C59 0.0457(15) 0.0424(14) 0.0337(13) 0.0061(11) 0.0082(11) 0.0015(12) C60 0.0598(17) 0.0405(14) 0.0312(12) 0.0058(11) 0.0075(12) 0.0014(13) C61 0.0519(16) 0.0362(13) 0.0361(13) -0.0030(11) 0.0099(11) -0.0117(12) C62 0.0337(13) 0.0401(14) 0.0552(16) -0.0061(12) 0.0018(12) -0.0059(11) C63 0.0326(13) 0.0485(15) 0.0423(14) -0.0008(12) -0.0046(11) 0.0005(12) C64 0.0429(14) 0.0527(16) 0.0324(13) -0.0037(11) -0.0013(11) -0.0044(13) B2 0.0212(11) 0.0211(11) 0.0204(10) 0.0005(8) 0.0010(8) 0.0001(9) B1 0.0248(12) 0.0240(11) 0.0223(11) 0.0033(9) 0.0039(9) 0.0015(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 Cl1 C59 1.736(3) . ? F1 B1 1.388(3) . ? F2 B1 1.389(3) . ? F3 B2 1.393(3) . ? F4 B2 1.391(2) . ? N1 C1 1.359(3) . ? N1 C4 1.405(2) . ? N1 B1 1.546(3) . ? N2 C9 1.356(3) . ? N2 C6 1.404(3) . ? N2 B1 1.548(3) . ? N3 C10 1.364(2) . ? N3 C13 1.403(2) . ? N3 B2 1.545(3) . ? N4 C18 1.355(2) . ? N4 C15 1.406(2) . ? N4 B2 1.546(3) . ? C1 C2 1.403(3) . ? C1 C23 1.495(3) . ? C2 C3 1.386(3) . ? C2 C19 1.498(3) . ? C3 C4 1.412(3) . ? C3 C22 1.515(3) . ? C4 C5 1.394(3) . ? C5 C6 1.388(3) . ? C5 C24 1.480(3) . ? C6 C7 1.418(3) . ? C7 C8 1.380(3) . ? C7 C34 1.489(6) . ? C7 C34A 1.542(13) . ? C8 C9 1.396(3) . ? C8 C37 1.493(6) . ? C8 C37A 1.523(13) . ? C9 C40 1.488(3) . ? C10 C11 1.397(3) . ? C10 C41 1.494(3) . ? C11 C12 1.386(3) . ? C11 C22 1.498(3) . ? C12 C13 1.406(3) . ? C12 C19 1.507(3) . ? C13 C14 1.396(3) . ? C14 C15 1.384(3) . ? C14 C42 1.491(3) . ? C15 C16 1.416(3) . ? C16 C17 1.378(3) . ? C16 C52 1.499(3) . ? C17 C18 1.404(3) . ? C17 C55 1.501(3) . ? C18 C58 1.489(3) . ? C19 C20 1.557(3) . ? C19 H19 1.0000 . ? C20 C21 1.552(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.559(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.387(3) . ? C24 C29 1.393(3) . ? C25 C26 1.388(3) . ? C25 H25 0.9500 . ? C26 C27 1.387(3) . ? C26 H26 0.9500 . ? C27 C28 1.396(3) . ? C27 C30 1.527(3) . ? C28 C29 1.377(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C32 1.524(3) . ? C30 C31 1.532(4) . ? C30 C33 1.536(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.519(6) . ? C34 C39 1.565(8) . ? C34 H34 1.0000 . ? C35 C36 1.323(8) . ? C35 H35 0.9500 . ? C36 C37 1.502(8) . ? C36 H36 0.9500 . ? C37 C38 1.570(8) . ? C37 H37 1.0000 . ? C38 C39 1.546(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C34A C39A 1.518(16) . ? C34A C35A 1.578(14) . ? C34A H34A 1.0000 . ? C35A C36A 1.529(17) . ? C35A H35A 0.9900 . ? C35A H35B 0.9900 . ? C36A C37A 1.591(16) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C37A C38A 1.522(15) . ? C37A H37A 1.0000 . ? C38A C39A 1.32(2) . ? C38A H38C 0.9500 . ? C39A H39C 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.381(3) . ? C42 C47 1.384(3) . ? C43 C44 1.384(3) . ? C43 H43 0.9500 . ? C44 C45 1.386(3) . ? C44 H44 0.9500 . ? C45 C46 1.399(3) . ? C45 C48 1.531(3) . ? C46 C47 1.388(3) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.528(3) . ? C48 C51 1.531(3) . ? C48 C50 1.532(3) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C57 1.533(3) . ? C52 C53 1.533(3) . ? C52 H52 1.0000 . ? C53 C54 1.433(3) . ? C53 H53 0.9500 . ? C54 C55 1.542(3) . ? C54 H54 0.9500 . ? C56 C57 1.444(2) . ? C56 C55 1.529(3) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C55 H55 1.0000 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C58 H58D 0.9800 . ? C58 H58E 0.9800 . ? C58 H58F 0.9800 . ? C59 C64 1.377(3) . ? C59 C60 1.388(3) . ? C60 C61 1.369(4) . ? C60 H60 0.9500 . ? C61 C62 1.382(4) . ? C61 H61 0.9500 . ? C62 C63 1.371(4) . ? C62 H62 0.9500 . ? C63 C64 1.371(4) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? 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 C1 N1 C4 108.50(16) . . ? C1 N1 B1 126.67(17) . . ? C4 N1 B1 124.83(17) . . ? C9 N2 C6 108.38(17) . . ? C9 N2 B1 125.98(17) . . ? C6 N2 B1 125.51(16) . . ? C10 N3 C13 108.14(16) . . ? C10 N3 B2 126.87(16) . . ? C13 N3 B2 124.64(16) . . ? C18 N4 C15 108.61(16) . . ? C18 N4 B2 126.14(16) . . ? C15 N4 B2 125.24(16) . . ? N1 C1 C2 108.41(17) . . ? N1 C1 C23 123.47(18) . . ? C2 C1 C23 128.09(18) . . ? C3 C2 C1 108.56(17) . . ? C3 C2 C19 115.36(18) . . ? C1 C2 C19 136.05(18) . . ? C2 C3 C4 106.87(17) . . ? C2 C3 C22 114.27(17) . . ? C4 C3 C22 138.85(18) . . ? C5 C4 N1 120.92(18) . . ? C5 C4 C3 131.34(18) . . ? N1 C4 C3 107.64(17) . . ? C6 C5 C4 121.27(18) . . ? C6 C5 C24 120.81(17) . . ? C4 C5 C24 117.89(17) . . ? C5 C6 N2 120.35(18) . . ? C5 C6 C7 132.02(19) . . ? N2 C6 C7 107.51(17) . . ? C8 C7 C6 106.62(19) . . ? C8 C7 C34 113.1(3) . . ? C6 C7 C34 140.3(3) . . ? C8 C7 C34A 116.4(7) . . ? C6 C7 C34A 136.1(7) . . ? C7 C8 C9 108.91(18) . . ? C7 C8 C37 116.3(3) . . ? C9 C8 C37 134.8(3) . . ? C7 C8 C37A 108.9(7) . . ? C9 C8 C37A 141.9(7) . . ? N2 C9 C8 108.57(18) . . ? N2 C9 C40 122.7(2) . . ? C8 C9 C40 128.77(19) . . ? N3 C10 C11 108.59(17) . . ? N3 C10 C41 122.88(17) . . ? C11 C10 C41 128.53(18) . . ? C12 C11 C10 108.40(17) . . ? C12 C11 C22 115.57(17) . . ? C10 C11 C22 136.01(18) . . ? C11 C12 C13 107.09(17) . . ? C11 C12 C19 114.24(17) . . ? C13 C12 C19 138.67(18) . . ? C14 C13 N3 121.20(17) . . ? C14 C13 C12 131.03(18) . . ? N3 C13 C12 107.77(16) . . ? C15 C14 C13 120.65(18) . . ? C15 C14 C42 121.48(18) . . ? C13 C14 C42 117.87(17) . . ? C14 C15 N4 120.88(18) . . ? C14 C15 C16 131.99(19) . . ? N4 C15 C16 107.11(17) . . ? C17 C16 C15 107.34(18) . . ? C17 C16 C52 114.41(18) . . ? C15 C16 C52 138.23(19) . . ? C16 C17 C18 108.39(18) . . ? C16 C17 C55 114.12(19) . . ? C18 C17 C55 137.47(19) . . ? N4 C18 C17 108.55(17) . . ? N4 C18 C58 122.68(18) . . ? C17 C18 C58 128.70(18) . . ? C2 C19 C12 105.08(16) . . ? C2 C19 C20 105.61(16) . . ? C12 C19 C20 104.70(16) . . ? C2 C19 H19 113.5 . . ? C12 C19 H19 113.5 . . ? C20 C19 H19 113.5 . . ? C21 C20 C19 111.29(16) . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C20 C21 C22 110.02(16) . . ? C20 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? C20 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C11 C22 C3 106.21(16) . . ? C11 C22 C21 105.46(15) . . ? C3 C22 C21 103.89(16) . . ? C11 C22 H22 113.5 . . ? C3 C22 H22 113.5 . . ? C21 C22 H22 113.5 . . ? C1 C23 H23A 109.5 . . ? C1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 118.89(19) . . ? C25 C24 C5 121.51(18) . . ? C29 C24 C5 119.54(17) . . ? C24 C25 C26 120.1(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 121.63(19) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C26 C27 C28 117.47(19) . . ? C26 C27 C30 123.26(19) . . ? C28 C27 C30 119.25(19) . . ? C29 C28 C27 121.48(19) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C24 120.37(19) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? C32 C30 C27 111.91(19) . . ? C32 C30 C31 108.82(19) . . ? C27 C30 C31 108.85(19) . . ? C32 C30 C33 108.67(19) . . ? C27 C30 C33 109.11(18) . . ? C31 C30 C33 109.4(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C7 C34 C35 108.0(4) . . ? C7 C34 C39 102.8(6) . . ? C35 C34 C39 104.7(5) . . ? C7 C34 H34 113.5 . . ? C35 C34 H34 113.5 . . ? C39 C34 H34 113.5 . . ? C36 C35 C34 116.2(5) . . ? C36 C35 H35 121.9 . . ? C34 C35 H35 121.9 . . ? C35 C36 C37 114.8(6) . . ? C35 C36 H36 122.6 . . ? C37 C36 H36 122.6 . . ? C8 C37 C36 107.8(6) . . ? C8 C37 C38 101.9(5) . . ? C36 C37 C38 105.2(5) . . ? C8 C37 H37 113.6 . . ? C36 C37 H37 113.6 . . ? C38 C37 H37 113.6 . . ? C39 C38 C37 110.1(5) . . ? C39 C38 H38A 109.6 . . ? C37 C38 H38A 109.6 . . ? C39 C38 H38B 109.6 . . ? C37 C38 H38B 109.6 . . ? H38A C38 H38B 108.2 . . ? C38 C39 C34 110.2(5) . . ? C38 C39 H39A 109.6 . . ? C34 C39 H39A 109.6 . . ? C38 C39 H39B 109.6 . . ? C34 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C39A C34A C7 111.0(15) . . ? C39A C34A C35A 101.6(12) . . ? C7 C34A C35A 106.1(9) . . ? C39A C34A H34A 112.5 . . ? C7 C34A H34A 112.5 . . ? C35A C34A H34A 112.5 . . ? C36A C35A C34A 107.2(10) . . ? C36A C35A H35A 110.3 . . ? C34A C35A H35A 110.3 . . ? C36A C35A H35B 110.3 . . ? C34A C35A H35B 110.3 . . ? H35A C35A H35B 108.5 . . ? C35A C36A C37A 110.2(11) . . ? C35A C36A H36A 109.6 . . ? C37A C36A H36A 109.6 . . ? C35A C36A H36B 109.6 . . ? C37A C36A H36B 109.6 . . ? H36A C36A H36B 108.1 . . ? C38A C37A C8 113.8(12) . . ? C38A C37A C36A 103.6(11) . . ? C8 C37A C36A 103.3(15) . . ? C38A C37A H37A 111.8 . . ? C8 C37A H37A 111.8 . . ? C36A C37A H37A 111.8 . . ? C39A C38A C37A 114.7(13) . . ? C39A C38A H38C 122.7 . . ? C37A C38A H38C 122.7 . . ? C38A C39A C34A 113.4(14) . . ? C38A C39A H39C 123.3 . . ? C34A C39A H39C 123.3 . . ? C9 C40 H40A 109.5 . . ? C9 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C9 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C10 C41 H41A 109.5 . . ? C10 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C10 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C47 118.15(19) . . ? C43 C42 C14 120.75(18) . . ? C47 C42 C14 120.79(18) . . ? C42 C43 C44 121.4(2) . . ? C42 C43 H43 119.3 . . ? C44 C43 H43 119.3 . . ? C43 C44 C45 121.4(2) . . ? C43 C44 H44 119.3 . . ? C45 C44 H44 119.3 . . ? C44 C45 C46 116.85(19) . . ? C44 C45 C48 122.47(19) . . ? C46 C45 C48 120.66(19) . . ? C47 C46 C45 121.7(2) . . ? C47 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C42 C47 C46 120.50(19) . . ? C42 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C49 C48 C45 110.16(19) . . ? C49 C48 C51 109.9(2) . . ? C45 C48 C51 108.11(19) . . ? C49 C48 C50 108.0(2) . . ? C45 C48 C50 112.42(19) . . ? C51 C48 C50 108.2(2) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C16 C52 C57 105.54(18) . . ? C16 C52 C53 105.41(18) . . ? C57 C52 C53 105.98(18) . . ? C16 C52 H52 113.1 . . ? C57 C52 H52 113.1 . . ? C53 C52 H52 113.1 . . ? C54 C53 C52 112.57(19) . . ? C54 C53 H53 123.7 . . ? C52 C53 H53 123.7 . . ? C53 C54 C55 112.4(2) . . ? C53 C54 H54 123.8 . . ? C55 C54 H54 123.8 . . ? C57 C56 C55 112.40(19) . . ? C57 C56 H56A 109.1 . . ? C55 C56 H56A 109.1 . . ? C57 C56 H56B 109.1 . . ? C55 C56 H56B 109.1 . . ? H56A C56 H56B 107.9 . . ? C56 C57 C52 112.42(19) . . ? C56 C57 H57A 109.1 . . ? C52 C57 H57A 109.1 . . ? C56 C57 H57B 109.1 . . ? C52 C57 H57B 109.1 . . ? H57A C57 H57B 107.9 . . ? C17 C55 C56 106.34(19) . . ? C17 C55 C54 105.93(18) . . ? C56 C55 C54 104.61(18) . . ? C17 C55 H55 113.1 . . ? C56 C55 H55 113.1 . . ? C54 C55 H55 113.1 . . ? C18 C58 H58A 109.5 . . ? C18 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C18 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C18 C58 H58D 109.5 . . ? H58A C58 H58D 141.1 . . ? H58B C58 H58D 56.3 . . ? H58C C58 H58D 56.3 . . ? C18 C58 H58E 109.5 . . ? H58A C58 H58E 56.3 . . ? H58B C58 H58E 141.1 . . ? H58C C58 H58E 56.3 . . ? H58D C58 H58E 109.5 . . ? C18 C58 H58F 109.5 . . ? H58A C58 H58F 56.3 . . ? H58B C58 H58F 56.3 . . ? H58C C58 H58F 141.1 . . ? H58D C58 H58F 109.5 . . ? H58E C58 H58F 109.5 . . ? C64 C59 C60 121.0(2) . . ? C64 C59 Cl1 119.9(2) . . ? C60 C59 Cl1 119.0(2) . . ? C61 C60 C59 119.1(2) . . ? C61 C60 H60 120.5 . . ? C59 C60 H60 120.5 . . ? C60 C61 C62 120.1(2) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C63 C62 C61 120.2(3) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C64 C63 C62 120.6(2) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C63 C64 C59 119.0(2) . . ? C63 C64 H64 120.5 . . ? C59 C64 H64 120.5 . . ? F4 B2 F3 108.54(16) . . ? F4 B2 N3 110.93(17) . . ? F3 B2 N3 110.07(16) . . ? F4 B2 N4 110.19(17) . . ? F3 B2 N4 110.09(17) . . ? N3 B2 N4 107.03(16) . . ? F1 B1 F2 109.02(17) . . ? F1 B1 N1 110.61(17) . . ? F2 B1 N1 110.58(17) . . ? F1 B1 N2 109.63(17) . . ? F2 B1 N2 109.97(17) . . ? N1 B1 N2 107.02(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C2 -0.6(2) . . . . ? B1 N1 C1 C2 179.90(18) . . . . ? C4 N1 C1 C23 177.48(18) . . . . ? B1 N1 C1 C23 -2.1(3) . . . . ? N1 C1 C2 C3 1.2(2) . . . . ? C23 C1 C2 C3 -176.66(19) . . . . ? N1 C1 C2 C19 -176.5(2) . . . . ? C23 C1 C2 C19 5.5(4) . . . . ? C1 C2 C3 C4 -1.4(2) . . . . ? C19 C2 C3 C4 176.87(16) . . . . ? C1 C2 C3 C22 179.21(16) . . . . ? C19 C2 C3 C22 -2.5(2) . . . . ? C1 N1 C4 C5 -177.24(17) . . . . ? B1 N1 C4 C5 2.3(3) . . . . ? C1 N1 C4 C3 -0.3(2) . . . . ? B1 N1 C4 C3 179.23(17) . . . . ? C2 C3 C4 C5 177.6(2) . . . . ? C22 C3 C4 C5 -3.3(4) . . . . ? C2 C3 C4 N1 1.1(2) . . . . ? C22 C3 C4 N1 -179.8(2) . . . . ? N1 C4 C5 C6 0.3(3) . . . . ? C3 C4 C5 C6 -175.77(19) . . . . ? N1 C4 C5 C24 -178.06(16) . . . . ? C3 C4 C5 C24 5.9(3) . . . . ? C4 C5 C6 N2 -1.2(3) . . . . ? C24 C5 C6 N2 177.11(17) . . . . ? C4 C5 C6 C7 -176.7(2) . . . . ? C24 C5 C6 C7 1.6(3) . . . . ? C9 N2 C6 C5 -176.48(18) . . . . ? B1 N2 C6 C5 -0.5(3) . . . . ? C9 N2 C6 C7 0.0(2) . . . . ? B1 N2 C6 C7 176.04(18) . . . . ? C5 C6 C7 C8 176.4(2) . . . . ? N2 C6 C7 C8 0.4(2) . . . . ? C5 C6 C7 C34 -3.5(6) . . . . ? N2 C6 C7 C34 -179.5(5) . . . . ? C5 C6 C7 C34A -15.5(10) . . . . ? N2 C6 C7 C34A 168.5(10) . . . . ? C6 C7 C8 C9 -0.7(2) . . . . ? C34 C7 C8 C9 179.2(3) . . . . ? C34A C7 C8 C9 -171.5(7) . . . . ? C6 C7 C8 C37 179.0(4) . . . . ? C34 C7 C8 C37 -1.1(4) . . . . ? C34A C7 C8 C37 8.2(9) . . . . ? C6 C7 C8 C37A 174.6(8) . . . . ? C34 C7 C8 C37A -5.5(9) . . . . ? C34A C7 C8 C37A 3.8(9) . . . . ? C6 N2 C9 C8 -0.5(2) . . . . ? B1 N2 C9 C8 -176.47(18) . . . . ? C6 N2 C9 C40 179.02(19) . . . . ? B1 N2 C9 C40 3.0(3) . . . . ? C7 C8 C9 N2 0.8(2) . . . . ? C37 C8 C9 N2 -178.9(5) . . . . ? C37A C8 C9 N2 -172.0(12) . . . . ? C7 C8 C9 C40 -178.7(2) . . . . ? C37 C8 C9 C40 1.7(6) . . . . ? C37A C8 C9 C40 8.5(13) . . . . ? C13 N3 C10 C11 1.0(2) . . . . ? B2 N3 C10 C11 -172.42(18) . . . . ? C13 N3 C10 C41 -179.00(18) . . . . ? B2 N3 C10 C41 7.6(3) . . . . ? N3 C10 C11 C12 -0.9(2) . . . . ? C41 C10 C11 C12 179.13(19) . . . . ? N3 C10 C11 C22 177.5(2) . . . . ? C41 C10 C11 C22 -2.5(4) . . . . ? C10 C11 C12 C13 0.4(2) . . . . ? C22 C11 C12 C13 -178.38(17) . . . . ? C10 C11 C12 C19 179.99(16) . . . . ? C22 C11 C12 C19 1.2(2) . . . . ? C10 N3 C13 C14 179.50(18) . . . . ? B2 N3 C13 C14 -6.9(3) . . . . ? C10 N3 C13 C12 -0.8(2) . . . . ? B2 N3 C13 C12 172.83(17) . . . . ? C11 C12 C13 C14 179.9(2) . . . . ? C19 C12 C13 C14 0.5(4) . . . . ? C11 C12 C13 N3 0.2(2) . . . . ? C19 C12 C13 N3 -179.3(2) . . . . ? N3 C13 C14 C15 2.1(3) . . . . ? C12 C13 C14 C15 -177.5(2) . . . . ? N3 C13 C14 C42 -178.59(17) . . . . ? C12 C13 C14 C42 1.7(3) . . . . ? C13 C14 C15 N4 1.5(3) . . . . ? C42 C14 C15 N4 -177.75(18) . . . . ? C13 C14 C15 C16 179.5(2) . . . . ? C42 C14 C15 C16 0.3(4) . . . . ? C18 N4 C15 C14 178.20(19) . . . . ? B2 N4 C15 C14 -0.6(3) . . . . ? C18 N4 C15 C16 -0.3(2) . . . . ? B2 N4 C15 C16 -179.04(18) . . . . ? C14 C15 C16 C17 -178.7(2) . . . . ? N4 C15 C16 C17 -0.5(2) . . . . ? C14 C15 C16 C52 -0.8(5) . . . . ? N4 C15 C16 C52 177.5(3) . . . . ? C15 C16 C17 C18 1.1(3) . . . . ? C52 C16 C17 C18 -177.44(19) . . . . ? C15 C16 C17 C55 179.68(19) . . . . ? C52 C16 C17 C55 1.2(3) . . . . ? C15 N4 C18 C17 0.9(2) . . . . ? B2 N4 C18 C17 179.70(19) . . . . ? C15 N4 C18 C58 -176.17(19) . . . . ? B2 N4 C18 C58 2.6(3) . . . . ? C16 C17 C18 N4 -1.3(3) . . . . ? C55 C17 C18 N4 -179.4(2) . . . . ? C16 C17 C18 C58 175.6(2) . . . . ? C55 C17 C18 C58 -2.5(4) . . . . ? C3 C2 C19 C12 54.4(2) . . . . ? C1 C2 C19 C12 -127.9(2) . . . . ? C3 C2 C19 C20 -55.9(2) . . . . ? C1 C2 C19 C20 121.7(2) . . . . ? C11 C12 C19 C2 -53.7(2) . . . . ? C13 C12 C19 C2 125.8(3) . . . . ? C11 C12 C19 C20 57.3(2) . . . . ? C13 C12 C19 C20 -123.2(3) . . . . ? C2 C19 C20 C21 53.6(2) . . . . ? C12 C19 C20 C21 -57.0(2) . . . . ? C19 C20 C21 C22 2.3(2) . . . . ? C12 C11 C22 C3 51.0(2) . . . . ? C10 C11 C22 C3 -127.3(2) . . . . ? C12 C11 C22 C21 -58.9(2) . . . . ? C10 C11 C22 C21 122.8(2) . . . . ? C2 C3 C22 C11 -50.2(2) . . . . ? C4 C3 C22 C11 130.8(2) . . . . ? C2 C3 C22 C21 60.8(2) . . . . ? C4 C3 C22 C21 -118.3(2) . . . . ? C20 C21 C22 C11 53.8(2) . . . . ? C20 C21 C22 C3 -57.7(2) . . . . ? C6 C5 C24 C25 72.2(3) . . . . ? C4 C5 C24 C25 -109.4(2) . . . . ? C6 C5 C24 C29 -110.7(2) . . . . ? C4 C5 C24 C29 67.7(2) . . . . ? C29 C24 C25 C26 -1.9(3) . . . . ? C5 C24 C25 C26 175.20(19) . . . . ? C24 C25 C26 C27 -0.3(3) . . . . ? C25 C26 C27 C28 2.2(3) . . . . ? C25 C26 C27 C30 -176.0(2) . . . . ? C26 C27 C28 C29 -1.9(3) . . . . ? C30 C27 C28 C29 176.38(19) . . . . ? C27 C28 C29 C24 -0.2(3) . . . . ? C25 C24 C29 C28 2.2(3) . . . . ? C5 C24 C29 C28 -175.00(18) . . . . ? C26 C27 C30 C32 -0.6(3) . . . . ? C28 C27 C30 C32 -178.7(2) . . . . ? C26 C27 C30 C31 119.8(2) . . . . ? C28 C27 C30 C31 -58.4(3) . . . . ? C26 C27 C30 C33 -120.9(2) . . . . ? C28 C27 C30 C33 61.0(3) . . . . ? C8 C7 C34 C35 -48.8(6) . . . . ? C6 C7 C34 C35 131.1(4) . . . . ? C34A C7 C34 C35 -162(7) . . . . ? C8 C7 C34 C39 61.6(5) . . . . ? C6 C7 C34 C39 -118.5(5) . . . . ? C34A C7 C34 C39 -52(7) . . . . ? C7 C34 C35 C36 51.6(7) . . . . ? C39 C34 C35 C36 -57.5(7) . . . . ? C34 C35 C36 C37 -1.5(9) . . . . ? C7 C8 C37 C36 50.6(5) . . . . ? C9 C8 C37 C36 -129.8(4) . . . . ? C37A C8 C37 C36 81(7) . . . . ? C7 C8 C37 C38 -59.8(6) . . . . ? C9 C8 C37 C38 119.8(4) . . . . ? C37A C8 C37 C38 -30(7) . . . . ? C35 C36 C37 C8 -48.7(8) . . . . ? C35 C36 C37 C38 59.5(9) . . . . ? C8 C37 C38 C39 57.3(8) . . . . ? C36 C37 C38 C39 -55.1(8) . . . . ? C37 C38 C39 C34 -0.9(10) . . . . ? C7 C34 C39 C38 -57.9(8) . . . . ? C35 C34 C39 C38 54.9(9) . . . . ? C8 C7 C34A C39A 46.7(13) . . . . ? C6 C7 C34A C39A -120.6(11) . . . . ? C34 C7 C34A C39A 117(7) . . . . ? C8 C7 C34A C35A -62.9(12) . . . . ? C6 C7 C34A C35A 129.9(8) . . . . ? C34 C7 C34A C35A 8(6) . . . . ? C39A C34A C35A C36A -67.1(15) . . . . ? C7 C34A C35A C36A 49.0(16) . . . . ? C34A C35A C36A C37A 11.4(19) . . . . ? C7 C8 C37A C38A -51.8(14) . . . . ? C9 C8 C37A C38A 120.9(11) . . . . ? C37 C8 C37A C38A 156(8) . . . . ? C7 C8 C37A C36A 59.8(11) . . . . ? C9 C8 C37A C36A -127.4(10) . . . . ? C37 C8 C37A C36A -92(8) . . . . ? C35A C36A C37A C38A 49.8(19) . . . . ? C35A C36A C37A C8 -69.2(17) . . . . ? C8 C37A C38A C39A 49(2) . . . . ? C36A C37A C38A C39A -62(2) . . . . ? C37A C38A C39A C34A 4(3) . . . . ? C7 C34A C39A C38A -51(2) . . . . ? C35A C34A C39A C38A 62(2) . . . . ? C15 C14 C42 C43 90.5(3) . . . . ? C13 C14 C42 C43 -88.7(2) . . . . ? C15 C14 C42 C47 -96.0(2) . . . . ? C13 C14 C42 C47 84.7(2) . . . . ? C47 C42 C43 C44 -0.7(3) . . . . ? C14 C42 C43 C44 172.9(2) . . . . ? C42 C43 C44 C45 -0.5(3) . . . . ? C43 C44 C45 C46 1.9(3) . . . . ? C43 C44 C45 C48 -179.6(2) . . . . ? C44 C45 C46 C47 -2.1(3) . . . . ? C48 C45 C46 C47 179.2(2) . . . . ? C43 C42 C47 C46 0.4(3) . . . . ? C14 C42 C47 C46 -173.2(2) . . . . ? C45 C46 C47 C42 1.0(3) . . . . ? C44 C45 C48 C49 129.8(2) . . . . ? C46 C45 C48 C49 -51.7(3) . . . . ? C44 C45 C48 C51 -110.1(2) . . . . ? C46 C45 C48 C51 68.4(3) . . . . ? C44 C45 C48 C50 9.3(3) . . . . ? C46 C45 C48 C50 -172.2(2) . . . . ? C17 C16 C52 C57 -56.5(2) . . . . ? C15 C16 C52 C57 125.6(3) . . . . ? C17 C16 C52 C53 55.4(2) . . . . ? C15 C16 C52 C53 -122.5(3) . . . . ? C16 C52 C53 C54 -56.4(2) . . . . ? C57 C52 C53 C54 55.2(2) . . . . ? C52 C53 C54 C55 2.6(3) . . . . ? C55 C56 C57 C52 -0.4(3) . . . . ? C16 C52 C57 C56 55.0(2) . . . . ? C53 C52 C57 C56 -56.5(2) . . . . ? C16 C17 C55 C56 54.9(2) . . . . ? C18 C17 C55 C56 -127.1(3) . . . . ? C16 C17 C55 C54 -56.1(3) . . . . ? C18 C17 C55 C54 122.0(3) . . . . ? C57 C56 C55 C17 -54.1(3) . . . . ? C57 C56 C55 C54 57.7(2) . . . . ? C53 C54 C55 C17 52.9(2) . . . . ? C53 C54 C55 C56 -59.2(2) . . . . ? C64 C59 C60 C61 -1.6(4) . . . . ? Cl1 C59 C60 C61 179.6(2) . . . . ? C59 C60 C61 C62 1.4(4) . . . . ? C60 C61 C62 C63 0.2(4) . . . . ? C61 C62 C63 C64 -1.7(4) . . . . ? C62 C63 C64 C59 1.5(4) . . . . ? C60 C59 C64 C63 0.1(4) . . . . ? Cl1 C59 C64 C63 178.9(2) . . . . ? C10 N3 B2 F4 -60.5(3) . . . . ? C13 N3 B2 F4 127.12(19) . . . . ? C10 N3 B2 F3 59.6(3) . . . . ? C13 N3 B2 F3 -112.7(2) . . . . ? C10 N3 B2 N4 179.27(17) . . . . ? C13 N3 B2 N4 6.9(3) . . . . ? C18 N4 B2 F4 57.5(3) . . . . ? C15 N4 B2 F4 -123.94(19) . . . . ? C18 N4 B2 F3 -62.2(3) . . . . ? C15 N4 B2 F3 116.4(2) . . . . ? C18 N4 B2 N3 178.20(18) . . . . ? C15 N4 B2 N3 -3.2(3) . . . . ? C1 N1 B1 F1 56.7(3) . . . . ? C4 N1 B1 F1 -122.8(2) . . . . ? C1 N1 B1 F2 -64.2(3) . . . . ? C4 N1 B1 F2 116.3(2) . . . . ? C1 N1 B1 N2 176.07(17) . . . . ? C4 N1 B1 N2 -3.4(3) . . . . ? C9 N2 B1 F1 -62.2(2) . . . . ? C6 N2 B1 F1 122.50(19) . . . . ? C9 N2 B1 F2 57.7(3) . . . . ? C6 N2 B1 F2 -117.6(2) . . . . ? C9 N2 B1 N1 177.84(17) . . . . ? C6 N2 B1 N1 2.5(3) . . . . ? data_20111022_2 _database_code_depnum_ccdc_archive 'CCDC 864652' #TrackingRef '9291_web_deposit_cif_file_7_HidemitsuUno_1327633261.20111024Takahashi.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C123 H122 B4 Cl2 F8 N8 O' _chemical_formula_moiety '2(C54 H52 B2 F4 N4), 2(C6 H5 Cl), C3 H8 O ' _chemical_formula_weight 1994.50 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 12.9946(3) _cell_length_b 13.0045(3) _cell_length_c 17.9199(4) _cell_angle_alpha 74.7391(8) _cell_angle_beta 88.1657(9) _cell_angle_gamma 62.0910(10) _cell_volume 2566.87(11) _cell_formula_units_Z 1 _cell_measurement_reflns_used 17035 _cell_measurement_theta_min 3.87 _cell_measurement_theta_max 68.22 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1050.00 _exptl_absorpt_coefficient_mu 1.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.912 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_source 'VariMax Rotating Anode, 40 kV x 30 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 47893 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_theta_max 68.25 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measured_fraction_theta_full 0.984 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 #============================================================================== # REFINEMENT DATA _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. The solvent molecules are found around a special position with a disordered fashion. Therefore, the atomic coordinates of the disordered solvent atoms are restrained. ; _reflns_number_total 9258 _reflns_number_gt 8081 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1572 _refine_ls_wR_factor_gt 0.1527 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_number_restraints 269 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 9257 _refine_ls_number_parameters 739 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0941P)^2^+0.5144P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_diff_density_max 0.320 _refine_diff_density_min -0.380 _refine_ls_extinction_method none _iucr_refine_instructions_details ; TITL 20111022_2 CELL 1.54187 12.99456 13.00451 17.91987 74.739 88.166 62.091 ZERR 1 0.00024 0.00024 0.00033 0.001 0.001 0.001 LATT 1 SFAC C H B F N CL O UNIT 123 122 4 8 8 2 1 SHEL 99999.000000 0.000000 L.S. 5 FMAP 2 PLAN -25 WPDB -2 HTAB TEMP -173.0 BOND $H CONF ACTA OMIT 0 1 1 DFIX 1.70 0.02 Cl1 C55 Cl2 C61 DFIX 1.39 0.02 C55 C56 C56 C57 C57 C58 C58 C59 C59 C60 C60 C55 = C61 C62 C62 C63 C63 C64 C64 C65 C65 C66 C66 C61 DFIX 1.54 0.02 C67 C68 C67 C69 DFIX 1.43 0.02 O1 C67 DANG 2.68 0.04 Cl1 C56 Cl1 C60 Cl2 C62 Cl2 C66 DANG 2.41 0.04 C55 C57 C56 C58 C57 C59 C58 C60 C59 C55 C60 C56 = C61 C63 C62 C64 C63 C65 C64 C66 C65 C61 C66 C62 DANG 2.40 0.04 O1 C68 O1 C69 DANG 2.49 0.04 C68 C69 FLAT 0.1 Cl1 > C60 FLAT 0.1 Cl2 > C66 SIZE 0.170 0.130 0.080 WGHT 0.094100 0.514400 FVAR 1.42092 PART -1 ISOR 0.1 0.2 Cl1 > C68 DELU 0.02 Cl1 > C68 SIMU 0.04 0.08 Cl1 > C68 CL1 6 -0.189597 1.220039 0.291962 10.50000 0.06867 0.07500 = 0.03669 -0.02653 0.01098 -0.02198 C55 1 -0.269709 1.357790 0.321571 10.50000 0.05542 0.07416 = 0.04431 -0.01816 0.00902 -0.03256 C56 1 -0.324046 1.349890 0.388864 10.50000 0.05608 0.05372 = 0.04593 -0.00941 0.00727 -0.03109 AFIX 43 H56 2 -0.315279 1.274575 0.420630 10.50000 -1.20000 AFIX 0 C57 1 -0.390895 1.455753 0.407328 10.50000 0.04178 0.06006 = 0.09767 -0.03001 0.02577 -0.02993 AFIX 43 H57 2 -0.437314 1.458161 0.449536 10.50000 -1.20000 AFIX 0 C58 1 -0.389226 1.563061 0.361424 10.50000 0.04673 0.04936 = 0.13788 -0.02801 -0.02173 -0.02123 AFIX 43 H58 2 -0.428925 1.635282 0.377063 10.50000 -1.20000 AFIX 0 C59 1 -0.335851 1.565311 0.299659 10.50000 0.06578 0.08655 = 0.06674 0.02466 -0.02312 -0.04662 AFIX 43 H59 2 -0.339020 1.639148 0.269942 10.50000 -1.20000 AFIX 0 C60 1 -0.273106 1.459816 0.275855 10.50000 0.05891 0.09220 = 0.04942 0.00767 -0.00273 -0.05248 AFIX 43 H60 2 -0.234930 1.460406 0.229759 10.50000 -1.20000 AFIX 0 CL2 6 0.185978 0.783385 0.699491 10.50000 0.23707 0.23102 = 0.21432 -0.06898 0.06637 -0.09203 C61 1 0.102544 0.874663 0.614970 10.50000 0.06717 0.09308 = 0.05932 -0.02251 0.01338 -0.05137 C62 1 -0.020608 0.933910 0.608117 10.50000 0.07427 0.06608 = 0.08763 -0.02619 0.02735 -0.04203 AFIX 43 H62 2 -0.059859 0.921809 0.652566 10.50000 -1.20000 AFIX 0 C63 1 -0.086894 1.011354 0.535867 10.50000 0.06235 0.06311 = 0.09816 -0.03796 0.01709 -0.04063 AFIX 43 H63 2 -0.169217 1.041304 0.530176 10.50000 -1.20000 AFIX 0 C64 1 -0.032839 1.042917 0.474598 10.50000 0.07909 0.09155 = 0.07029 -0.02768 0.01137 -0.04408 AFIX 43 H64 2 -0.077245 1.106661 0.429506 10.50000 -1.20000 AFIX 0 C65 1 0.088326 0.980217 0.479270 10.50000 0.08973 0.13768 = 0.09646 -0.03091 0.03865 -0.05991 AFIX 43 H65 2 0.126073 0.990890 0.433797 10.50000 -1.20000 AFIX 0 C66 1 0.155691 0.902178 0.548949 10.50000 0.06536 0.06960 = 0.08462 -0.02605 0.01659 -0.03572 AFIX 43 H66 2 0.238598 0.867118 0.551877 10.50000 -1.20000 AFIX 0 O1 7 0.397165 0.548062 0.622214 10.50000 0.18969 0.19020 = 0.29610 -0.01755 0.09442 -0.10952 AFIX 83 H1 2 0.348347 0.604900 0.639027 10.50000 -1.50000 AFIX 0 C67 1 0.380231 0.440699 0.652054 10.50000 0.13460 0.10560 = 0.18397 0.04590 -0.05584 -0.04106 AFIX 13 H67 2 0.400529 0.390480 0.614757 10.50000 -1.20000 AFIX 0 C68 1 0.457588 0.374247 0.725951 10.50000 0.06685 0.07365 = 0.08243 0.00790 -0.00347 -0.04114 AFIX 133 H68A 2 0.489914 0.423436 0.737867 10.50000 -1.50000 H68B 2 0.521694 0.297505 0.721088 10.50000 -1.50000 H68C 2 0.412498 0.357699 0.767941 10.50000 -1.50000 AFIX 0 C69 1 0.259779 0.474404 0.675674 10.50000 0.08253 0.11050 = 0.13543 0.03704 0.00856 -0.05238 AFIX 133 H69A 2 0.251863 0.400971 0.695674 10.50000 -1.50000 H69B 2 0.201895 0.528652 0.630499 10.50000 -1.50000 H69C 2 0.246608 0.515686 0.716337 10.50000 -1.50000 AFIX 0 PART 0 F1 4 0.142303 0.355846 0.989696 11.00000 0.08434 0.06125 = 0.07156 -0.02570 0.04278 -0.02987 F2 4 0.150557 0.501829 0.890826 11.00000 0.07521 0.04203 = 0.06619 -0.01054 0.01484 -0.01116 F3 4 0.615337 0.049756 0.506052 11.00000 0.04831 0.05035 = 0.04140 -0.01207 0.00867 -0.01993 F4 4 0.541683 0.246683 0.503804 11.00000 0.06099 0.05113 = 0.04270 -0.00514 0.00279 -0.03560 N1 5 0.269887 0.292524 0.891701 11.00000 0.05560 0.04090 = 0.04543 -0.00896 0.01630 -0.01600 N2 5 0.317576 0.376865 0.987035 11.00000 0.07798 0.03599 = 0.04139 -0.00977 0.02124 -0.01857 N3 5 0.480838 0.122047 0.599259 11.00000 0.04344 0.04150 = 0.03526 -0.00836 0.00554 -0.02113 N4 5 0.411429 0.186369 0.458183 11.00000 0.04957 0.03883 = 0.03554 -0.00828 0.00563 -0.02309 C1 1 0.209804 0.269748 0.842453 11.00000 0.05237 0.04468 = 0.04339 -0.00533 0.01336 -0.01811 C2 1 0.290925 0.180229 0.811249 11.00000 0.04794 0.04389 = 0.03912 -0.00556 0.01153 -0.01812 C3 1 0.403040 0.146832 0.841809 11.00000 0.05174 0.04067 = 0.03624 -0.00701 0.01120 -0.01888 C4 1 0.389796 0.218178 0.892147 11.00000 0.05365 0.03778 = 0.03820 -0.00775 0.01304 -0.01568 C5 1 0.472843 0.227787 0.935058 11.00000 0.06327 0.03707 = 0.03427 -0.00667 0.01251 -0.02049 C6 1 0.437363 0.307329 0.980677 11.00000 0.07183 0.03743 = 0.03706 -0.00798 0.01464 -0.02129 C7 1 0.501997 0.330704 1.031944 11.00000 0.08971 0.03866 = 0.03388 -0.00807 0.01257 -0.02691 C8 1 0.416789 0.412954 1.068550 11.00000 0.10822 0.03687 = 0.03564 -0.00841 0.01668 -0.02593 C9 1 0.304629 0.438462 1.038969 11.00000 0.09515 0.03654 = 0.04085 -0.00824 0.02045 -0.01937 C10 1 0.549761 0.081943 0.667719 11.00000 0.04674 0.03805 = 0.03616 -0.00913 0.00579 -0.02105 C11 1 0.479599 0.081958 0.728344 11.00000 0.04545 0.03894 = 0.03599 -0.00831 0.00601 -0.01802 C12 1 0.366720 0.120267 0.696921 11.00000 0.04499 0.04187 = 0.04014 -0.00864 0.00844 -0.02039 C13 1 0.366785 0.148026 0.615506 11.00000 0.04371 0.04179 = 0.03936 -0.00773 0.00631 -0.02116 C14 1 0.275984 0.196590 0.555174 11.00000 0.04663 0.03900 = 0.04248 -0.00789 0.00479 -0.02241 C15 1 0.297849 0.212594 0.478404 11.00000 0.04705 0.03848 = 0.04134 -0.00826 0.00284 -0.02227 C16 1 0.224058 0.251913 0.407486 11.00000 0.05427 0.03800 = 0.04474 -0.00862 -0.00041 -0.02431 C17 1 0.296784 0.248681 0.346537 11.00000 0.05812 0.03861 = 0.04119 -0.00997 0.00014 -0.02404 C18 1 0.411982 0.207720 0.380929 11.00000 0.05823 0.03881 = 0.03672 -0.00991 0.00472 -0.02431 C19 1 0.283824 0.112904 0.756903 11.00000 0.04779 0.05110 = 0.04084 -0.00817 0.01031 -0.02330 AFIX 13 H19 2 0.202318 0.143154 0.733816 11.00000 -1.20000 AFIX 0 C20 1 0.343395 -0.022591 0.807687 11.00000 0.05985 0.05028 = 0.04216 -0.01064 0.01490 -0.02910 AFIX 23 H20A 2 0.296149 -0.031872 0.850871 11.00000 -1.20000 H20B 2 0.346481 -0.075001 0.775449 11.00000 -1.20000 AFIX 0 C21 1 0.469198 -0.063157 0.841337 11.00000 0.05815 0.04122 = 0.03769 -0.00888 0.00960 -0.02031 AFIX 23 H21A 2 0.525906 -0.132241 0.822907 11.00000 -1.20000 H21B 2 0.475791 -0.090796 0.898837 11.00000 -1.20000 AFIX 0 C22 1 0.499990 0.043622 0.815716 11.00000 0.04764 0.04173 = 0.03486 -0.00949 0.00726 -0.01767 AFIX 13 H22 2 0.580570 0.021330 0.836233 11.00000 -1.20000 AFIX 0 C23 1 0.079702 0.334698 0.827023 11.00000 0.05159 0.05766 = 0.05908 -0.00884 0.01573 -0.01432 AFIX 133 H23A 2 0.045543 0.323265 0.876095 11.00000 -1.50000 H23B 2 0.055541 0.302187 0.791532 11.00000 -1.50000 H23C 2 0.052415 0.421380 0.803288 11.00000 -1.50000 AFIX 0 C24 1 0.599191 0.150745 0.928957 11.00000 0.05880 0.04158 = 0.03311 -0.01263 0.00731 -0.02248 C25 1 0.659546 0.196881 0.877244 11.00000 0.06114 0.03959 = 0.04299 -0.00708 0.00561 -0.02292 AFIX 43 H25 2 0.621097 0.279821 0.847982 11.00000 -1.20000 AFIX 0 C26 1 0.774958 0.123418 0.867895 11.00000 0.06011 0.04778 = 0.04339 -0.00989 0.00773 -0.02863 AFIX 43 H26 2 0.814069 0.157489 0.832314 11.00000 -1.20000 AFIX 0 C27 1 0.835362 0.001459 0.908906 11.00000 0.05512 0.04672 = 0.03547 -0.01284 0.00023 -0.02509 C28 1 0.773919 -0.043853 0.961113 11.00000 0.06103 0.04053 = 0.03626 -0.00770 0.00265 -0.02098 AFIX 43 H28 2 0.812303 -0.126828 0.990305 11.00000 -1.20000 AFIX 0 C29 1 0.659125 0.028790 0.971286 11.00000 0.06421 0.04446 = 0.03537 -0.00926 0.00935 -0.02555 AFIX 43 H29 2 0.620392 -0.004740 1.007625 11.00000 -1.20000 AFIX 0 C30 1 0.960182 -0.084103 0.895870 11.00000 0.05120 0.04870 = 0.04624 -0.01159 -0.00012 -0.02306 C31 1 0.955546 -0.176292 0.859257 11.00000 0.05494 0.06144 = 0.05844 -0.02670 0.00931 -0.02541 AFIX 133 H31A 2 1.035045 -0.232991 0.851640 11.00000 -1.50000 H31B 2 0.907432 -0.133524 0.808918 11.00000 -1.50000 H31C 2 0.921200 -0.221224 0.893834 11.00000 -1.50000 AFIX 0 C32 1 1.017341 -0.016754 0.842250 11.00000 0.05233 0.05940 = 0.07590 -0.01070 0.00619 -0.02563 AFIX 133 H32A 2 1.018986 0.043612 0.864668 11.00000 -1.50000 H32B 2 0.971943 0.023971 0.790919 11.00000 -1.50000 H32C 2 1.097537 -0.074902 0.836973 11.00000 -1.50000 AFIX 0 C33 1 1.037704 -0.153659 0.974273 11.00000 0.06443 0.05450 = 0.05862 -0.01474 -0.00865 -0.01847 AFIX 133 H33A 2 1.002954 -0.197755 1.009233 11.00000 -1.50000 H33B 2 1.043290 -0.096159 0.997779 11.00000 -1.50000 H33C 2 1.116158 -0.211288 0.965660 11.00000 -1.50000 AFIX 0 C34 1 0.620718 0.291683 1.049912 11.00000 0.09481 0.04667 = 0.03784 -0.01046 0.00834 -0.03321 AFIX 43 H34 2 0.678885 0.236351 1.026124 11.00000 -1.20000 AFIX 0 C35 1 0.651955 0.335531 1.103342 11.00000 0.10939 0.05427 = 0.03939 -0.00951 0.00042 -0.03624 AFIX 43 H35 2 0.732327 0.310443 1.115445 11.00000 -1.20000 AFIX 0 C36 1 0.566863 0.416338 1.139842 11.00000 0.13902 0.05137 = 0.04036 -0.01291 0.00140 -0.03811 AFIX 43 H36 2 0.590648 0.444215 1.176528 11.00000 -1.20000 AFIX 0 C37 1 0.450261 0.455196 1.123080 11.00000 0.12756 0.04401 = 0.03990 -0.01300 0.01334 -0.02770 AFIX 43 H37 2 0.393009 0.509672 1.147808 11.00000 -1.20000 AFIX 0 C38 1 0.188810 0.518966 1.060851 11.00000 0.10810 0.04595 = 0.05516 -0.01599 0.03276 -0.01411 AFIX 133 H38A 2 0.131887 0.563960 1.014394 11.00000 -1.50000 H38B 2 0.196335 0.576178 1.083636 11.00000 -1.50000 H38C 2 0.162001 0.469731 1.098922 11.00000 -1.50000 AFIX 0 C39 1 0.676346 0.045730 0.671498 11.00000 0.04654 0.04557 = 0.03957 -0.01117 0.00579 -0.02424 AFIX 133 H39A 2 0.719555 -0.031369 0.658614 11.00000 -1.50000 H39B 2 0.704751 0.036270 0.724154 11.00000 -1.50000 H39C 2 0.688420 0.108346 0.634225 11.00000 -1.50000 AFIX 0 C40 1 0.154245 0.238086 0.576546 11.00000 0.04505 0.04474 = 0.03935 -0.00536 0.00202 -0.02273 C41 1 0.102138 0.164437 0.590632 11.00000 0.05233 0.04366 = 0.08337 -0.01802 0.01231 -0.02540 AFIX 43 H41 2 0.144446 0.083995 0.586445 11.00000 -1.20000 AFIX 0 C42 1 -0.011756 0.207160 0.610888 11.00000 0.05208 0.04686 = 0.08293 -0.01588 0.01253 -0.03048 AFIX 43 H42 2 -0.046030 0.155123 0.619809 11.00000 -1.20000 AFIX 0 C43 1 -0.076732 0.323173 0.618457 11.00000 0.04677 0.04395 = 0.04651 -0.00603 0.00245 -0.02442 C44 1 -0.022124 0.395410 0.604835 11.00000 0.05291 0.04259 = 0.06853 -0.01472 0.01353 -0.02583 AFIX 43 H44 2 -0.063684 0.475416 0.609863 11.00000 -1.20000 AFIX 0 C45 1 0.090510 0.354229 0.584262 11.00000 0.05286 0.04612 = 0.06391 -0.01144 0.01281 -0.02995 AFIX 43 H45 2 0.124856 0.406206 0.575260 11.00000 -1.20000 AFIX 0 C46 1 -0.202776 0.374018 0.639910 11.00000 0.04643 0.04669 = 0.06122 -0.01130 0.00741 -0.02570 C47 1 -0.206996 0.400902 0.718457 11.00000 0.05885 0.06975 = 0.07352 -0.02954 0.02096 -0.03805 AFIX 133 H47A 2 -0.155670 0.326111 0.758426 11.00000 -1.50000 H47B 2 -0.287500 0.432669 0.732393 11.00000 -1.50000 H47C 2 -0.180521 0.461141 0.714845 11.00000 -1.50000 AFIX 0 C48 1 -0.251361 0.285558 0.644766 11.00000 0.04989 0.05260 = 0.06593 -0.01220 0.00762 -0.03008 AFIX 133 H48A 2 -0.251771 0.270404 0.594050 11.00000 -1.50000 H48B 2 -0.331447 0.320777 0.659342 11.00000 -1.50000 H48C 2 -0.201903 0.208980 0.684008 11.00000 -1.50000 AFIX 0 C49 1 -0.281613 0.492417 0.577212 11.00000 0.04958 0.04892 = 0.09052 -0.00390 -0.00014 -0.02313 AFIX 133 H49A 2 -0.254786 0.552023 0.575085 11.00000 -1.50000 H49B 2 -0.362656 0.524464 0.590109 11.00000 -1.50000 H49C 2 -0.277596 0.476150 0.526521 11.00000 -1.50000 AFIX 0 C50 1 0.105475 0.288639 0.389886 11.00000 0.05522 0.04758 = 0.05633 -0.01233 -0.00135 -0.02742 AFIX 43 H50 2 0.055340 0.290800 0.429882 11.00000 -1.20000 AFIX 0 C51 1 0.063361 0.321748 0.312423 11.00000 0.05977 0.04992 = 0.06141 -0.01111 -0.01142 -0.02720 AFIX 43 H51 2 -0.016866 0.346969 0.299645 11.00000 -1.20000 AFIX 0 C52 1 0.135780 0.319059 0.252468 11.00000 0.07150 0.04670 = 0.04893 -0.01112 -0.01115 -0.02714 AFIX 43 H52 2 0.103753 0.342697 0.200075 11.00000 -1.20000 AFIX 0 C53 1 0.252090 0.282828 0.268345 11.00000 0.07001 0.04348 = 0.04296 -0.01131 -0.00180 -0.02655 AFIX 43 H53 2 0.301185 0.280813 0.227713 11.00000 -1.20000 AFIX 0 C54 1 0.517049 0.191098 0.340117 11.00000 0.06332 0.05545 = 0.03587 -0.01249 0.00812 -0.02910 AFIX 123 H54A 2 0.570022 0.202826 0.370541 10.50000 -1.50000 H54B 2 0.493463 0.250477 0.288728 10.50000 -1.50000 H54C 2 0.557262 0.108981 0.334048 10.50000 -1.50000 H54D 2 0.510476 0.172030 0.291670 10.50000 -1.50000 H54E 2 0.587035 0.124379 0.373483 10.50000 -1.50000 H54F 2 0.523236 0.265875 0.328164 10.50000 -1.50000 AFIX 0 B1 3 0.214609 0.384433 0.939288 11.00000 0.06525 0.04050 = 0.05156 -0.01125 0.02271 -0.01630 B2 3 0.517930 0.149562 0.517139 11.00000 0.04554 0.04074 = 0.03647 -0.00743 0.00640 -0.02198 HKLF 4 REM 20111022_2 REM R1 = 0.0554 for 8081 Fo > 4sig(Fo) and 0.0595 for all 9257 data REM 739 parameters refined using 269 restraints END WGHT 0.1010 0.4231 REM Highest difference peak 0.320, deepest hole -0.379, 1-sigma level 0.088 Q1 1 -0.1333 1.2011 0.3819 11.00000 0.05 0.32 Q2 1 0.6137 0.4309 1.1647 11.00000 0.05 0.28 Q3 1 0.7399 0.4026 1.0812 11.00000 0.05 0.25 Q4 1 -0.1477 0.0932 0.6540 11.00000 0.05 0.25 Q5 1 1.0092 0.0686 0.8189 11.00000 0.05 0.24 Q6 1 -0.1605 1.6086 0.3938 11.00000 0.05 0.24 Q7 1 0.7780 -0.2373 0.9070 11.00000 0.05 0.24 Q8 1 -0.2001 0.1145 0.6933 11.00000 0.05 0.24 Q9 1 -0.2175 0.1276 0.6772 11.00000 0.05 0.24 Q10 1 0.5417 0.4508 1.1286 11.00000 0.05 0.24 Q11 1 0.6806 0.4556 1.1297 11.00000 0.05 0.23 Q12 1 -0.3174 1.5126 0.2323 11.00000 0.05 0.23 Q13 1 0.1959 0.5732 0.5999 11.00000 0.05 0.23 Q14 1 -0.2873 0.1587 0.7174 11.00000 0.05 0.23 Q15 1 0.6647 0.4498 1.0808 11.00000 0.05 0.22 Q16 1 0.6137 0.4999 1.1241 11.00000 0.05 0.22 Q17 1 0.1854 0.6230 1.0273 11.00000 0.05 0.22 Q18 1 -0.0495 0.0610 0.6834 11.00000 0.05 0.21 Q19 1 0.9337 -0.2554 0.9117 11.00000 0.05 0.21 Q20 1 0.2102 0.6260 1.0428 11.00000 0.05 0.21 Q21 1 1.1615 -0.3460 1.0102 11.00000 0.05 0.21 Q22 1 -0.4503 1.7039 0.2585 11.00000 0.05 0.21 Q23 1 1.0380 -0.0011 0.7385 11.00000 0.05 0.20 Q24 1 1.0595 0.0316 0.9353 11.00000 0.05 0.19 Q25 1 -0.2252 1.6124 0.3125 11.00000 0.05 0.19 ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.0090 0.0039 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0727 0.0534 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0311 0.0180 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.3639 0.7018 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0492 0.0322 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl1 Cl -0.18960(13) 1.22004(14) 0.29196(7) 0.0631(3) Uani 0.50 1 d PDU A -1 C55 C -0.2697(3) 1.3578(4) 0.3216(2) 0.0570(9) Uani 0.50 1 d PDU A -1 C56 C -0.3240(3) 1.3499(4) 0.3889(2) 0.0509(8) Uani 0.50 1 d PDU A -1 H56 H -0.3153 1.2746 0.4206 0.061 Uiso 0.50 1 calc PR A -1 C57 C -0.3909(5) 1.4558(6) 0.4073(4) 0.0629(13) Uani 0.50 1 d PDU A -1 H57 H -0.4373 1.4582 0.4495 0.075 Uiso 0.50 1 calc PR A -1 C58 C -0.3892(6) 1.5631(7) 0.3614(6) 0.078(2) Uani 0.50 1 d PDU A -1 H58 H -0.4289 1.6353 0.3771 0.093 Uiso 0.50 1 calc PR A -1 C59 C -0.3359(6) 1.5653(6) 0.2997(3) 0.0779(16) Uani 0.50 1 d PDU A -1 H59 H -0.3390 1.6391 0.2699 0.093 Uiso 0.50 1 calc PR A -1 C60 C -0.2731(4) 1.4598(5) 0.2759(2) 0.0657(12) Uani 0.50 1 d PDU A -1 H60 H -0.2349 1.4604 0.2298 0.079 Uiso 0.50 1 calc PR A -1 Cl2 Cl 0.1860(5) 0.7834(5) 0.6995(3) 0.235(2) Uani 0.50 1 d PDU B -1 C61 C 0.1025(4) 0.8747(4) 0.6150(3) 0.0676(11) Uani 0.50 1 d PDU B -1 C62 C -0.0206(4) 0.9339(4) 0.6081(3) 0.0719(12) Uani 0.50 1 d PDU B -1 H62 H -0.0599 0.9218 0.6526 0.086 Uiso 0.50 1 calc PR B -1 C63 C -0.0869(8) 1.0114(7) 0.5359(6) 0.067(2) Uani 0.50 1 d PDU B -1 H63 H -0.1692 1.0413 0.5302 0.080 Uiso 0.50 1 calc PR B -1 C64 C -0.0328(5) 1.0429(5) 0.4746(3) 0.0779(13) Uani 0.50 1 d PDU B -1 H64 H -0.0772 1.1067 0.4295 0.093 Uiso 0.50 1 calc PR B -1 C65 C 0.0883(11) 0.9802(12) 0.4793(8) 0.107(4) Uani 0.50 1 d PDU B -1 H65 H 0.1261 0.9909 0.4338 0.128 Uiso 0.50 1 calc PR B -1 C66 C 0.1557(4) 0.9022(4) 0.5489(3) 0.0710(11) Uani 0.50 1 d PDU B -1 H66 H 0.2386 0.8671 0.5519 0.085 Uiso 0.50 1 calc PR B -1 O1 O 0.3972(10) 0.5481(11) 0.6222(7) 0.230(6) Uani 0.50 1 d PDU C -1 H1 H 0.3483 0.6049 0.6390 0.345 Uiso 0.50 1 calc PR C -1 C67 C 0.3802(12) 0.4407(12) 0.6521(9) 0.165(7) Uani 0.50 1 d PDU C -1 H67 H 0.4005 0.3905 0.6148 0.198 Uiso 0.50 1 calc PR C -1 C68 C 0.4576(4) 0.3742(5) 0.7260(3) 0.0773(13) Uani 0.50 1 d PDU C -1 H68A H 0.4899 0.4234 0.7379 0.116 Uiso 0.50 1 calc PR C -1 H68B H 0.5217 0.2975 0.7211 0.116 Uiso 0.50 1 calc PR C -1 H68C H 0.4125 0.3577 0.7679 0.116 Uiso 0.50 1 calc PR C -1 C69 C 0.2598(6) 0.4744(7) 0.6757(5) 0.122(3) Uani 0.50 1 d PD C -1 H69A H 0.2519 0.4010 0.6957 0.183 Uiso 0.50 1 calc PR C -1 H69B H 0.2019 0.5287 0.6305 0.183 Uiso 0.50 1 calc PR C -1 H69C H 0.2466 0.5157 0.7163 0.183 Uiso 0.50 1 calc PR C -1 F1 F 0.14230(12) 0.35585(11) 0.98970(7) 0.0738(4) Uani 1 1 d . . . F2 F 0.15056(11) 0.50183(10) 0.89083(7) 0.0694(3) Uani 1 1 d . . . F3 F 0.61534(8) 0.04976(9) 0.50605(5) 0.0485(2) Uani 1 1 d . . . F4 F 0.54168(9) 0.24668(9) 0.50380(5) 0.0496(3) Uani 1 1 d . . . N1 N 0.26989(14) 0.29252(13) 0.89170(9) 0.0512(4) Uani 1 1 d . . . N2 N 0.31758(16) 0.37686(13) 0.98704(9) 0.0560(4) Uani 1 1 d . . . N3 N 0.48084(12) 0.12205(12) 0.59926(7) 0.0403(3) Uani 1 1 d . . . N4 N 0.41143(12) 0.18637(12) 0.45818(7) 0.0410(3) Uani 1 1 d . . . C1 C 0.20980(16) 0.26975(16) 0.84245(10) 0.0506(4) Uani 1 1 d . . . C2 C 0.29092(15) 0.18023(16) 0.81125(10) 0.0467(4) Uani 1 1 d . . . C3 C 0.40304(15) 0.14683(15) 0.84181(9) 0.0452(4) Uani 1 1 d . . . C4 C 0.38980(16) 0.21818(15) 0.89215(9) 0.0466(4) Uani 1 1 d . . . C5 C 0.47284(16) 0.22779(15) 0.93506(9) 0.0472(4) Uani 1 1 d . . . C6 C 0.43736(18) 0.30733(15) 0.98068(10) 0.0515(4) Uani 1 1 d . . . C7 C 0.5020(2) 0.33070(16) 1.03194(10) 0.0562(5) Uani 1 1 d . . . C8 C 0.4168(2) 0.41295(17) 1.06855(10) 0.0645(6) Uani 1 1 d . . . C9 C 0.3046(2) 0.43846(17) 1.03897(11) 0.0634(6) Uani 1 1 d . . . C10 C 0.54976(14) 0.08194(14) 0.66772(9) 0.0403(3) Uani 1 1 d . . . C11 C 0.47960(14) 0.08196(15) 0.72834(9) 0.0415(4) Uani 1 1 d . . . C12 C 0.36672(15) 0.12027(15) 0.69692(9) 0.0432(4) Uani 1 1 d . . . C13 C 0.36678(14) 0.14803(15) 0.61551(9) 0.0421(4) Uani 1 1 d . . . C14 C 0.27598(15) 0.19659(15) 0.55517(10) 0.0426(4) Uani 1 1 d . . . C15 C 0.29785(15) 0.21259(14) 0.47840(9) 0.0421(4) Uani 1 1 d . . . C16 C 0.22406(16) 0.25191(15) 0.40749(10) 0.0452(4) Uani 1 1 d . . . C17 C 0.29678(16) 0.24868(15) 0.34654(10) 0.0457(4) Uani 1 1 d . . . C18 C 0.41198(16) 0.20772(15) 0.38093(9) 0.0442(4) Uani 1 1 d . . . C19 C 0.28382(16) 0.11290(16) 0.75690(10) 0.0479(4) Uani 1 1 d . . . H19 H 0.2023 0.1432 0.7338 0.057 Uiso 1 1 calc R . . C20 C 0.34339(17) -0.02259(17) 0.80769(10) 0.0503(4) Uani 1 1 d . . . H20A H 0.2961 -0.0319 0.8509 0.060 Uiso 1 1 calc R . . H20B H 0.3465 -0.0750 0.7754 0.060 Uiso 1 1 calc R . . C21 C 0.46920(16) -0.06316(15) 0.84134(10) 0.0477(4) Uani 1 1 d . . . H21A H 0.5259 -0.1322 0.8229 0.057 Uiso 1 1 calc R . . H21B H 0.4758 -0.0908 0.8988 0.057 Uiso 1 1 calc R . . C22 C 0.49999(15) 0.04362(15) 0.81572(9) 0.0433(4) Uani 1 1 d . . . H22 H 0.5806 0.0213 0.8362 0.052 Uiso 1 1 calc R . . C23 C 0.07970(17) 0.33470(19) 0.82702(12) 0.0629(5) Uani 1 1 d . . . H23A H 0.0455 0.3233 0.8761 0.094 Uiso 1 1 calc R . . H23B H 0.0555 0.3022 0.7915 0.094 Uiso 1 1 calc R . . H23C H 0.0524 0.4214 0.8033 0.094 Uiso 1 1 calc R . . C24 C 0.59919(16) 0.15074(15) 0.92896(9) 0.0447(4) Uani 1 1 d . . . C25 C 0.65955(17) 0.19688(16) 0.87724(10) 0.0493(4) Uani 1 1 d . . . H25 H 0.6211 0.2798 0.8480 0.059 Uiso 1 1 calc R . . C26 C 0.77496(17) 0.12342(16) 0.86790(10) 0.0499(4) Uani 1 1 d . . . H26 H 0.8141 0.1575 0.8323 0.060 Uiso 1 1 calc R . . C27 C 0.83536(16) 0.00146(16) 0.90891(9) 0.0450(4) Uani 1 1 d . . . C28 C 0.77392(16) -0.04385(16) 0.96111(10) 0.0479(4) Uani 1 1 d . . . H28 H 0.8123 -0.1268 0.9903 0.057 Uiso 1 1 calc R . . C29 C 0.65913(17) 0.02879(16) 0.97129(9) 0.0487(4) Uani 1 1 d . . . H29 H 0.6204 -0.0047 1.0076 0.058 Uiso 1 1 calc R . . C30 C 0.96018(16) -0.08410(17) 0.89587(10) 0.0493(4) Uani 1 1 d . . . C31 C 0.95555(18) -0.17629(19) 0.85926(12) 0.0572(5) Uani 1 1 d . . . H31A H 1.0350 -0.2330 0.8516 0.086 Uiso 1 1 calc R . . H31B H 0.9074 -0.1335 0.8089 0.086 Uiso 1 1 calc R . . H31C H 0.9212 -0.2212 0.8938 0.086 Uiso 1 1 calc R . . C32 C 1.01734(18) -0.0168(2) 0.84225(14) 0.0647(5) Uani 1 1 d . . . H32A H 1.0190 0.0436 0.8647 0.097 Uiso 1 1 calc R . . H32B H 0.9719 0.0240 0.7909 0.097 Uiso 1 1 calc R . . H32C H 1.0975 -0.0749 0.8370 0.097 Uiso 1 1 calc R . . C33 C 1.03770(19) -0.15366(19) 0.97427(12) 0.0632(5) Uani 1 1 d . . . H33A H 1.0030 -0.1978 1.0092 0.095 Uiso 1 1 calc R . . H33B H 1.0433 -0.0962 0.9978 0.095 Uiso 1 1 calc R . . H33C H 1.1162 -0.2113 0.9657 0.095 Uiso 1 1 calc R . . C34 C 0.6207(2) 0.29168(18) 1.04991(10) 0.0603(5) Uani 1 1 d . . . H34 H 0.6789 0.2364 1.0261 0.072 Uiso 1 1 calc R . . C35 C 0.6520(2) 0.33553(19) 1.10334(11) 0.0694(6) Uani 1 1 d . . . H35 H 0.7323 0.3104 1.1154 0.083 Uiso 1 1 calc R . . C36 C 0.5669(3) 0.4163(2) 1.13984(12) 0.0797(8) Uani 1 1 d . . . H36 H 0.5906 0.4442 1.1765 0.096 Uiso 1 1 calc R . . C37 C 0.4503(3) 0.45520(19) 1.12308(12) 0.0759(7) Uani 1 1 d . . . H37 H 0.3930 0.5097 1.1478 0.091 Uiso 1 1 calc R . . C38 C 0.1888(2) 0.51897(19) 1.06085(13) 0.0794(8) Uani 1 1 d . . . H38A H 0.1319 0.5640 1.0144 0.119 Uiso 1 1 calc R . . H38B H 0.1963 0.5762 1.0836 0.119 Uiso 1 1 calc R . . H38C H 0.1620 0.4697 1.0989 0.119 Uiso 1 1 calc R . . C39 C 0.67635(14) 0.04573(16) 0.67150(9) 0.0431(4) Uani 1 1 d . . . H39A H 0.7196 -0.0314 0.6586 0.065 Uiso 1 1 calc R . . H39B H 0.7048 0.0363 0.7242 0.065 Uiso 1 1 calc R . . H39C H 0.6884 0.1083 0.6342 0.065 Uiso 1 1 calc R . . C40 C 0.15424(15) 0.23809(15) 0.57655(9) 0.0438(4) Uani 1 1 d . . . C41 C 0.10214(17) 0.16444(18) 0.59063(13) 0.0588(5) Uani 1 1 d . . . H41 H 0.1444 0.0840 0.5864 0.071 Uiso 1 1 calc R . . C42 C -0.01176(17) 0.20716(18) 0.61089(13) 0.0584(5) Uani 1 1 d . . . H42 H -0.0460 0.1551 0.6198 0.070 Uiso 1 1 calc R . . C43 C -0.07673(15) 0.32317(16) 0.61846(10) 0.0460(4) Uani 1 1 d . . . C44 C -0.02212(17) 0.39541(17) 0.60484(12) 0.0538(4) Uani 1 1 d . . . H44 H -0.0637 0.4754 0.6099 0.065 Uiso 1 1 calc R . . C45 C 0.09051(16) 0.35423(17) 0.58426(11) 0.0527(4) Uani 1 1 d . . . H45 H 0.1249 0.4062 0.5753 0.063 Uiso 1 1 calc R . . C46 C -0.20278(16) 0.37402(17) 0.63991(11) 0.0509(4) Uani 1 1 d . . . C47 C -0.20700(19) 0.4009(2) 0.71846(13) 0.0626(5) Uani 1 1 d . . . H47A H -0.1557 0.3261 0.7584 0.094 Uiso 1 1 calc R . . H47B H -0.2875 0.4327 0.7324 0.094 Uiso 1 1 calc R . . H47C H -0.1805 0.4611 0.7148 0.094 Uiso 1 1 calc R . . C48 C -0.25136(16) 0.28556(18) 0.64477(12) 0.0548(4) Uani 1 1 d . . . H48A H -0.2518 0.2704 0.5940 0.082 Uiso 1 1 calc R . . H48B H -0.3314 0.3208 0.6593 0.082 Uiso 1 1 calc R . . H48C H -0.2019 0.2090 0.6840 0.082 Uiso 1 1 calc R . . C49 C -0.28161(18) 0.49242(18) 0.57721(15) 0.0663(6) Uani 1 1 d . . . H49A H -0.2548 0.5520 0.5751 0.100 Uiso 1 1 calc R . . H49B H -0.3627 0.5245 0.5901 0.100 Uiso 1 1 calc R . . H49C H -0.2776 0.4762 0.5265 0.100 Uiso 1 1 calc R . . C50 C 0.10548(17) 0.28864(17) 0.38989(11) 0.0521(4) Uani 1 1 d . . . H50 H 0.0553 0.2908 0.4299 0.063 Uiso 1 1 calc R . . C51 C 0.06336(18) 0.32175(18) 0.31242(12) 0.0571(5) Uani 1 1 d . . . H51 H -0.0169 0.3470 0.2996 0.069 Uiso 1 1 calc R . . C52 C 0.13578(18) 0.31906(17) 0.25247(11) 0.0562(5) Uani 1 1 d . . . H52 H 0.1038 0.3427 0.2001 0.067 Uiso 1 1 calc R . . C53 C 0.25209(18) 0.28283(16) 0.26834(11) 0.0523(4) Uani 1 1 d . . . H53 H 0.3012 0.2808 0.2277 0.063 Uiso 1 1 calc R . . C54 C 0.51705(17) 0.19110(18) 0.34012(10) 0.0514(4) Uani 1 1 d . . . H54A H 0.5700 0.2028 0.3705 0.077 Uiso 0.50 1 calc PR . . H54B H 0.4935 0.2505 0.2887 0.077 Uiso 0.50 1 calc PR . . H54C H 0.5573 0.1090 0.3340 0.077 Uiso 0.50 1 calc PR . . H54D H 0.5105 0.1720 0.2917 0.077 Uiso 0.50 1 calc PR . . H54E H 0.5870 0.1244 0.3735 0.077 Uiso 0.50 1 calc PR . . H54F H 0.5232 0.2659 0.3282 0.077 Uiso 0.50 1 calc PR . . B1 B 0.2146(2) 0.38443(19) 0.93929(13) 0.0569(5) Uani 1 1 d . . . B2 B 0.51793(17) 0.14956(17) 0.51714(10) 0.0411(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0687(7) 0.0750(8) 0.0367(5) -0.0265(5) 0.0110(5) -0.0220(6) C55 0.055(2) 0.074(3) 0.0443(18) -0.0182(18) 0.0090(16) -0.033(2) C56 0.056(2) 0.054(2) 0.0459(18) -0.0094(16) 0.0073(16) -0.0311(18) C57 0.042(2) 0.060(3) 0.098(4) -0.030(3) 0.026(2) -0.030(2) C58 0.047(3) 0.049(4) 0.138(6) -0.028(4) -0.022(4) -0.021(3) C59 0.066(3) 0.087(4) 0.067(3) 0.025(3) -0.023(3) -0.047(3) C60 0.059(2) 0.092(3) 0.049(2) 0.008(2) -0.0027(17) -0.052(3) Cl2 0.237(5) 0.231(5) 0.214(4) -0.069(4) 0.066(4) -0.092(4) C61 0.067(3) 0.093(3) 0.059(2) -0.023(2) 0.013(2) -0.051(2) C62 0.074(3) 0.066(3) 0.088(3) -0.026(2) 0.027(2) -0.042(2) C63 0.062(4) 0.063(4) 0.098(5) -0.038(3) 0.017(3) -0.041(3) C64 0.079(3) 0.092(4) 0.070(3) -0.028(2) 0.011(2) -0.044(3) C65 0.090(7) 0.138(9) 0.096(6) -0.031(5) 0.039(5) -0.060(6) C66 0.065(3) 0.070(3) 0.085(3) -0.026(2) 0.017(2) -0.036(2) O1 0.190(9) 0.190(9) 0.296(14) -0.018(9) 0.094(9) -0.110(8) C67 0.135(13) 0.106(10) 0.184(14) 0.046(9) -0.056(10) -0.041(9) C68 0.067(3) 0.074(3) 0.082(3) 0.008(2) -0.003(2) -0.041(2) C69 0.083(4) 0.111(5) 0.135(6) 0.037(5) 0.009(4) -0.052(4) F1 0.0843(8) 0.0613(7) 0.0716(8) -0.0257(6) 0.0428(7) -0.0299(6) F2 0.0752(8) 0.0420(6) 0.0662(7) -0.0105(5) 0.0148(6) -0.0112(5) F3 0.0483(5) 0.0504(6) 0.0414(5) -0.0121(4) 0.0087(4) -0.0199(5) F4 0.0610(6) 0.0511(6) 0.0427(5) -0.0051(4) 0.0028(4) -0.0356(5) N1 0.0556(9) 0.0409(8) 0.0454(8) -0.0090(6) 0.0163(7) -0.0160(7) N2 0.0780(11) 0.0360(7) 0.0414(8) -0.0098(6) 0.0212(7) -0.0186(7) N3 0.0434(7) 0.0415(7) 0.0353(7) -0.0084(5) 0.0055(5) -0.0211(6) N4 0.0496(8) 0.0388(7) 0.0355(7) -0.0083(5) 0.0056(6) -0.0231(6) C1 0.0524(10) 0.0447(9) 0.0434(9) -0.0053(7) 0.0134(8) -0.0181(8) C2 0.0479(9) 0.0439(9) 0.0391(8) -0.0056(7) 0.0115(7) -0.0181(8) C3 0.0517(9) 0.0407(9) 0.0362(8) -0.0070(7) 0.0112(7) -0.0189(8) C4 0.0537(10) 0.0378(8) 0.0382(8) -0.0078(7) 0.0130(7) -0.0157(8) C5 0.0633(11) 0.0371(8) 0.0343(8) -0.0067(7) 0.0125(7) -0.0205(8) C6 0.0718(12) 0.0374(9) 0.0371(8) -0.0080(7) 0.0146(8) -0.0213(9) C7 0.0897(15) 0.0387(9) 0.0339(8) -0.0081(7) 0.0126(9) -0.0269(10) C8 0.1082(18) 0.0369(9) 0.0356(9) -0.0084(7) 0.0167(10) -0.0259(11) C9 0.0951(16) 0.0365(9) 0.0408(9) -0.0082(7) 0.0205(10) -0.0194(10) C10 0.0467(9) 0.0381(8) 0.0362(8) -0.0091(6) 0.0058(6) -0.0211(7) C11 0.0454(9) 0.0389(8) 0.0360(8) -0.0083(6) 0.0060(7) -0.0180(7) C12 0.0450(9) 0.0419(9) 0.0401(8) -0.0086(7) 0.0084(7) -0.0204(7) C13 0.0437(9) 0.0418(9) 0.0394(8) -0.0077(7) 0.0063(7) -0.0212(7) C14 0.0466(9) 0.0390(8) 0.0425(8) -0.0079(7) 0.0048(7) -0.0224(7) C15 0.0470(9) 0.0385(8) 0.0413(8) -0.0083(7) 0.0028(7) -0.0223(7) C16 0.0543(10) 0.0380(8) 0.0447(9) -0.0086(7) -0.0004(7) -0.0243(8) C17 0.0581(10) 0.0386(9) 0.0412(8) -0.0100(7) 0.0001(7) -0.0240(8) C18 0.0582(10) 0.0388(8) 0.0367(8) -0.0099(6) 0.0047(7) -0.0243(8) C19 0.0478(9) 0.0511(10) 0.0408(9) -0.0082(7) 0.0103(7) -0.0233(8) C20 0.0599(11) 0.0503(10) 0.0422(9) -0.0106(7) 0.0149(8) -0.0291(9) C21 0.0582(10) 0.0412(9) 0.0377(8) -0.0089(7) 0.0096(7) -0.0203(8) C22 0.0476(9) 0.0417(9) 0.0349(8) -0.0095(7) 0.0073(7) -0.0177(7) C23 0.0516(11) 0.0577(12) 0.0591(11) -0.0088(9) 0.0157(9) -0.0143(9) C24 0.0588(10) 0.0416(9) 0.0331(8) -0.0126(7) 0.0073(7) -0.0225(8) C25 0.0611(11) 0.0396(9) 0.0430(9) -0.0071(7) 0.0056(8) -0.0229(8) C26 0.0601(11) 0.0478(10) 0.0434(9) -0.0099(7) 0.0077(8) -0.0286(9) C27 0.0551(10) 0.0467(9) 0.0355(8) -0.0128(7) 0.0002(7) -0.0251(8) C28 0.0610(11) 0.0405(9) 0.0363(8) -0.0077(7) 0.0027(7) -0.0210(8) C29 0.0642(11) 0.0445(9) 0.0354(8) -0.0093(7) 0.0093(7) -0.0256(8) C30 0.0512(10) 0.0487(10) 0.0462(9) -0.0116(8) -0.0001(7) -0.0231(8) C31 0.0549(11) 0.0614(12) 0.0584(11) -0.0267(9) 0.0093(9) -0.0254(9) C32 0.0523(11) 0.0594(12) 0.0759(14) -0.0107(10) 0.0062(10) -0.0256(10) C33 0.0644(12) 0.0545(11) 0.0586(12) -0.0147(9) -0.0086(9) -0.0185(10) C34 0.0948(16) 0.0467(10) 0.0378(9) -0.0105(8) 0.0083(9) -0.0332(11) C35 0.1094(18) 0.0543(12) 0.0394(10) -0.0095(8) 0.0004(10) -0.0362(12) C36 0.139(3) 0.0514(12) 0.0404(10) -0.0129(9) 0.0014(13) -0.0381(15) C37 0.128(2) 0.0440(11) 0.0399(10) -0.0130(8) 0.0133(12) -0.0277(13) C38 0.1081(19) 0.0459(11) 0.0552(12) -0.0160(9) 0.0328(12) -0.0141(12) C39 0.0465(9) 0.0456(9) 0.0396(8) -0.0112(7) 0.0058(7) -0.0242(8) C40 0.0451(9) 0.0447(9) 0.0394(8) -0.0054(7) 0.0020(7) -0.0227(8) C41 0.0523(10) 0.0437(10) 0.0834(14) -0.0180(9) 0.0123(10) -0.0254(9) C42 0.0521(10) 0.0469(10) 0.0829(14) -0.0159(9) 0.0125(10) -0.0305(9) C43 0.0468(9) 0.0439(9) 0.0465(9) -0.0060(7) 0.0025(7) -0.0244(8) C44 0.0529(10) 0.0426(9) 0.0685(12) -0.0147(8) 0.0135(9) -0.0258(8) C45 0.0529(10) 0.0461(10) 0.0639(11) -0.0114(8) 0.0128(8) -0.0300(8) C46 0.0464(9) 0.0467(10) 0.0612(11) -0.0113(8) 0.0074(8) -0.0257(8) C47 0.0588(11) 0.0697(13) 0.0735(13) -0.0295(11) 0.0210(10) -0.0381(10) C48 0.0499(10) 0.0526(11) 0.0659(12) -0.0122(9) 0.0076(9) -0.0301(9) C49 0.0496(11) 0.0489(11) 0.0905(15) -0.0039(10) -0.0001(10) -0.0231(9) C50 0.0552(10) 0.0476(10) 0.0563(10) -0.0123(8) -0.0013(8) -0.0274(9) C51 0.0598(11) 0.0499(10) 0.0614(11) -0.0111(9) -0.0114(9) -0.0272(9) C52 0.0715(13) 0.0467(10) 0.0489(10) -0.0111(8) -0.0111(9) -0.0271(9) C53 0.0700(12) 0.0435(9) 0.0430(9) -0.0113(7) -0.0018(8) -0.0266(9) C54 0.0633(11) 0.0554(11) 0.0359(8) -0.0125(7) 0.0081(8) -0.0291(9) B1 0.0652(13) 0.0405(11) 0.0516(12) -0.0113(9) 0.0227(10) -0.0163(10) B2 0.0455(10) 0.0407(10) 0.0365(9) -0.0074(7) 0.0064(7) -0.0220(8) _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 Cl1 C55 1.815(4) . ? C55 C60 1.345(6) . ? C55 C56 1.383(5) . ? C56 C57 1.364(7) . ? C56 H56 0.9500 . ? C57 C58 1.431(9) . ? C57 H57 0.9500 . ? C58 C59 1.288(11) . ? C58 H58 0.9500 . ? C59 C60 1.403(8) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? Cl2 C61 1.683(7) . ? C61 C66 1.400(6) . ? C61 C62 1.406(6) . ? C62 C63 1.416(10) . ? C62 H62 0.9500 . ? C63 C64 1.360(10) . ? C63 H63 0.9500 . ? C64 C65 1.386(12) . ? C64 H64 0.9500 . ? C65 C66 1.388(12) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? O1 C67 1.473(13) . ? O1 H1 0.8400 . ? C67 C68 1.477(13) . ? C67 C69 1.495(14) . ? C67 H67 1.0000 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? F1 B1 1.390(2) . ? F2 B1 1.392(2) . ? F3 B2 1.381(2) . ? F4 B2 1.396(2) . ? N1 C1 1.369(3) . ? N1 C4 1.396(2) . ? N1 B1 1.538(3) . ? N2 C9 1.339(3) . ? N2 C6 1.407(2) . ? N2 B1 1.561(3) . ? N3 C10 1.369(2) . ? N3 C13 1.397(2) . ? N3 B2 1.538(2) . ? N4 C18 1.339(2) . ? N4 C15 1.409(2) . ? N4 B2 1.571(2) . ? C1 C2 1.391(2) . ? C1 C23 1.489(3) . ? C2 C3 1.394(3) . ? C2 C19 1.501(3) . ? C3 C4 1.409(2) . ? C3 C22 1.522(2) . ? C4 C5 1.415(3) . ? C5 C6 1.388(2) . ? C5 C24 1.489(2) . ? C6 C7 1.441(3) . ? C7 C34 1.398(3) . ? C7 C8 1.419(3) . ? C8 C37 1.407(3) . ? C8 C9 1.421(4) . ? C9 C38 1.489(3) . ? C10 C11 1.396(2) . ? C10 C39 1.482(2) . ? C11 C12 1.392(2) . ? C11 C22 1.504(2) . ? C12 C13 1.408(2) . ? C12 C19 1.514(2) . ? C13 C14 1.409(2) . ? C14 C15 1.377(2) . ? C14 C40 1.487(2) . ? C15 C16 1.440(2) . ? C16 C50 1.402(3) . ? C16 C17 1.417(2) . ? C17 C53 1.407(2) . ? C17 C18 1.430(2) . ? C18 C54 1.479(2) . ? C19 C20 1.567(2) . ? C19 H19 1.0000 . ? C20 C21 1.550(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.572(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.391(2) . ? C24 C29 1.395(2) . ? C25 C26 1.385(3) . ? C25 H25 0.9500 . ? C26 C27 1.389(2) . ? C26 H26 0.9500 . ? C27 C28 1.401(2) . ? C27 C30 1.532(3) . ? C28 C29 1.380(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.535(3) . ? C30 C32 1.537(3) . ? C30 C33 1.541(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.391(3) . ? C34 H34 0.9500 . ? C35 C36 1.408(3) . ? C35 H35 0.9500 . ? C36 C37 1.369(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.381(2) . ? C40 C45 1.385(3) . ? C41 C42 1.390(3) . ? C41 H41 0.9500 . ? C42 C43 1.384(3) . ? C42 H42 0.9500 . ? C43 C44 1.392(2) . ? C43 C46 1.532(2) . ? C44 C45 1.379(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.531(3) . ? C46 C48 1.534(2) . ? C46 C49 1.539(3) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.387(3) . ? C50 H50 0.9500 . ? C51 C52 1.402(3) . ? C51 H51 0.9500 . ? C52 C53 1.370(3) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C54 H54D 0.9800 . ? C54 H54E 0.9800 . ? C54 H54F 0.9800 . ? 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 C60 C55 C56 125.1(4) . . ? C60 C55 Cl1 117.6(3) . . ? C56 C55 Cl1 117.3(3) . . ? C57 C56 C55 116.6(4) . . ? C57 C56 H56 121.7 . . ? C55 C56 H56 121.7 . . ? C56 C57 C58 118.2(6) . . ? C56 C57 H57 120.9 . . ? C58 C57 H57 120.9 . . ? C59 C58 C57 122.4(7) . . ? C59 C58 H58 118.8 . . ? C57 C58 H58 118.8 . . ? C58 C59 C60 120.7(5) . . ? C58 C59 H59 119.7 . . ? C60 C59 H59 119.7 . . ? C55 C60 C59 116.6(4) . . ? C55 C60 H60 121.7 . . ? C59 C60 H60 121.7 . . ? C66 C61 C62 117.1(4) . . ? C66 C61 Cl2 119.6(4) . . ? C62 C61 Cl2 123.1(4) . . ? C61 C62 C63 120.9(6) . . ? C61 C62 H62 119.5 . . ? C63 C62 H62 119.5 . . ? C64 C63 C62 120.1(7) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C65 118.7(8) . . ? C63 C64 H64 120.7 . . ? C65 C64 H64 120.7 . . ? C64 C65 C66 121.4(10) . . ? C64 C65 H65 119.3 . . ? C66 C65 H65 119.3 . . ? C65 C66 C61 120.6(7) . . ? C65 C66 H66 119.7 . . ? C61 C66 H66 119.7 . . ? C67 O1 H1 109.5 . . ? O1 C67 C68 104.0(10) . . ? O1 C67 C69 111.7(10) . . ? C68 C67 C69 104.4(11) . . ? O1 C67 H67 112.1 . . ? C68 C67 H67 112.1 . . ? C69 C67 H67 112.1 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C1 N1 C4 108.93(15) . . ? C1 N1 B1 125.68(17) . . ? C4 N1 B1 125.39(17) . . ? C9 N2 C6 109.74(19) . . ? C9 N2 B1 124.81(18) . . ? C6 N2 B1 125.43(15) . . ? C10 N3 C13 109.03(13) . . ? C10 N3 B2 125.86(13) . . ? C13 N3 B2 124.71(13) . . ? C18 N4 C15 109.85(14) . . ? C18 N4 B2 125.34(14) . . ? C15 N4 B2 124.57(13) . . ? N1 C1 C2 108.13(16) . . ? N1 C1 C23 123.30(17) . . ? C2 C1 C23 128.56(19) . . ? C1 C2 C3 108.50(17) . . ? C1 C2 C19 135.16(17) . . ? C3 C2 C19 116.30(15) . . ? C2 C3 C4 107.10(15) . . ? C2 C3 C22 113.64(15) . . ? C4 C3 C22 139.16(17) . . ? N1 C4 C3 107.33(16) . . ? N1 C4 C5 120.85(15) . . ? C3 C4 C5 131.73(16) . . ? C6 C5 C4 120.93(17) . . ? C6 C5 C24 121.26(17) . . ? C4 C5 C24 117.81(14) . . ? C5 C6 N2 120.16(18) . . ? C5 C6 C7 132.20(19) . . ? N2 C6 C7 107.47(15) . . ? C34 C7 C8 119.6(2) . . ? C34 C7 C6 134.59(17) . . ? C8 C7 C6 105.8(2) . . ? C37 C8 C7 120.9(2) . . ? C37 C8 C9 131.4(2) . . ? C7 C8 C9 107.77(19) . . ? N2 C9 C8 109.21(18) . . ? N2 C9 C38 123.6(2) . . ? C8 C9 C38 127.2(2) . . ? N3 C10 C11 107.82(14) . . ? N3 C10 C39 123.08(14) . . ? C11 C10 C39 129.09(15) . . ? C12 C11 C10 108.63(14) . . ? C12 C11 C22 115.87(14) . . ? C10 C11 C22 135.34(15) . . ? C11 C12 C13 107.10(14) . . ? C11 C12 C19 114.25(14) . . ? C13 C12 C19 138.49(16) . . ? N3 C13 C12 107.38(14) . . ? N3 C13 C14 121.06(14) . . ? C12 C13 C14 131.54(15) . . ? C15 C14 C13 121.26(15) . . ? C15 C14 C40 120.77(15) . . ? C13 C14 C40 117.83(14) . . ? C14 C15 N4 120.36(15) . . ? C14 C15 C16 132.24(16) . . ? N4 C15 C16 107.39(14) . . ? C50 C16 C17 119.55(16) . . ? C50 C16 C15 134.30(17) . . ? C17 C16 C15 106.15(15) . . ? C53 C17 C16 121.31(17) . . ? C53 C17 C18 131.13(17) . . ? C16 C17 C18 107.56(14) . . ? N4 C18 C17 109.04(15) . . ? N4 C18 C54 123.86(16) . . ? C17 C18 C54 127.09(15) . . ? C2 C19 C12 105.58(14) . . ? C2 C19 C20 103.74(14) . . ? C12 C19 C20 105.66(14) . . ? C2 C19 H19 113.6 . . ? C12 C19 H19 113.6 . . ? C20 C19 H19 113.6 . . ? C21 C20 C19 110.75(14) . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C20 C21 C22 111.07(14) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C11 C22 C3 105.77(13) . . ? C11 C22 C21 104.14(13) . . ? C3 C22 C21 104.79(13) . . ? C11 C22 H22 113.7 . . ? C3 C22 H22 113.7 . . ? C21 C22 H22 113.7 . . ? C1 C23 H23A 109.5 . . ? C1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 117.79(16) . . ? C25 C24 C5 120.67(15) . . ? C29 C24 C5 121.44(15) . . ? C26 C25 C24 120.82(16) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 122.07(16) . . ? C25 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C26 C27 C28 116.62(16) . . ? C26 C27 C30 123.29(16) . . ? C28 C27 C30 119.99(16) . . ? C29 C28 C27 121.78(16) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C28 C29 C24 120.92(16) . . ? C28 C29 H29 119.5 . . ? C24 C29 H29 119.5 . . ? C27 C30 C31 108.42(14) . . ? C27 C30 C32 112.60(16) . . ? C31 C30 C32 108.99(16) . . ? C27 C30 C33 110.07(15) . . ? C31 C30 C33 108.46(16) . . ? C32 C30 C33 108.21(16) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C7 118.6(2) . . ? C35 C34 H34 120.7 . . ? C7 C34 H34 120.7 . . ? C34 C35 C36 121.3(3) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C37 C36 C35 120.8(2) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C8 118.8(2) . . ? C36 C37 H37 120.6 . . ? C8 C37 H37 120.6 . . ? C9 C38 H38A 109.5 . . ? C9 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C9 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C10 C39 H39A 109.5 . . ? C10 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C10 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 118.15(16) . . ? C41 C40 C14 122.62(16) . . ? C45 C40 C14 119.22(15) . . ? C40 C41 C42 120.49(17) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C43 C42 C41 122.02(17) . . ? C43 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? C42 C43 C44 116.55(16) . . ? C42 C43 C46 123.60(15) . . ? C44 C43 C46 119.85(16) . . ? C45 C44 C43 121.92(17) . . ? C45 C44 H44 119.0 . . ? C43 C44 H44 119.0 . . ? C44 C45 C40 120.87(16) . . ? C44 C45 H45 119.6 . . ? C40 C45 H45 119.6 . . ? C47 C46 C43 109.51(15) . . ? C47 C46 C48 109.03(16) . . ? C43 C46 C48 111.98(15) . . ? C47 C46 C49 109.11(17) . . ? C43 C46 C49 109.14(15) . . ? C48 C46 C49 108.02(15) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C16 118.15(18) . . ? C51 C50 H50 120.9 . . ? C16 C50 H50 120.9 . . ? C50 C51 C52 121.90(18) . . ? C50 C51 H51 119.0 . . ? C52 C51 H51 119.0 . . ? C53 C52 C51 120.95(17) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C52 C53 C17 118.14(18) . . ? C52 C53 H53 120.9 . . ? C17 C53 H53 120.9 . . ? C18 C54 H54A 109.5 . . ? C18 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C18 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C18 C54 H54D 109.5 . . ? H54A C54 H54D 141.1 . . ? H54B C54 H54D 56.3 . . ? H54C C54 H54D 56.3 . . ? C18 C54 H54E 109.5 . . ? H54A C54 H54E 56.3 . . ? H54B C54 H54E 141.1 . . ? H54C C54 H54E 56.3 . . ? H54D C54 H54E 109.5 . . ? C18 C54 H54F 109.5 . . ? H54A C54 H54F 56.3 . . ? H54B C54 H54F 56.3 . . ? H54C C54 H54F 141.1 . . ? H54D C54 H54F 109.5 . . ? H54E C54 H54F 109.5 . . ? F1 B1 F2 109.52(17) . . ? F1 B1 N1 110.66(17) . . ? F2 B1 N1 111.08(16) . . ? F1 B1 N2 109.69(17) . . ? F2 B1 N2 108.97(17) . . ? N1 B1 N2 106.86(16) . . ? F3 B2 F4 109.27(14) . . ? F3 B2 N3 111.50(14) . . ? F4 B2 N3 110.70(14) . . ? F3 B2 N4 109.85(14) . . ? F4 B2 N4 108.62(13) . . ? N3 B2 N4 106.82(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C60 C55 C56 C57 3.6(6) . . . . ? Cl1 C55 C56 C57 -175.4(3) . . . . ? C55 C56 C57 C58 -6.9(7) . . . . ? C56 C57 C58 C59 6.5(9) . . . . ? C57 C58 C59 C60 -2.0(10) . . . . ? C56 C55 C60 C59 0.8(6) . . . . ? Cl1 C55 C60 C59 179.8(3) . . . . ? C58 C59 C60 C55 -1.6(8) . . . . ? C66 C61 C62 C63 4.2(7) . . . . ? Cl2 C61 C62 C63 179.0(5) . . . . ? C61 C62 C63 C64 -9.2(9) . . . . ? C62 C63 C64 C65 12.5(14) . . . . ? C63 C64 C65 C66 -11.5(18) . . . . ? C64 C65 C66 C61 6.8(15) . . . . ? C62 C61 C66 C65 -3.0(10) . . . . ? Cl2 C61 C66 C65 -178.0(8) . . . . ? C4 N1 C1 C2 0.23(19) . . . . ? B1 N1 C1 C2 -179.43(15) . . . . ? C4 N1 C1 C23 -179.01(16) . . . . ? B1 N1 C1 C23 1.3(3) . . . . ? N1 C1 C2 C3 0.14(19) . . . . ? C23 C1 C2 C3 179.33(17) . . . . ? N1 C1 C2 C19 177.79(17) . . . . ? C23 C1 C2 C19 -3.0(3) . . . . ? C1 C2 C3 C4 -0.45(19) . . . . ? C19 C2 C3 C4 -178.61(14) . . . . ? C1 C2 C3 C22 176.59(14) . . . . ? C19 C2 C3 C22 -1.6(2) . . . . ? C1 N1 C4 C3 -0.51(18) . . . . ? B1 N1 C4 C3 179.15(15) . . . . ? C1 N1 C4 C5 176.48(15) . . . . ? B1 N1 C4 C5 -3.9(2) . . . . ? C2 C3 C4 N1 0.59(18) . . . . ? C22 C3 C4 N1 -175.26(18) . . . . ? C2 C3 C4 C5 -175.95(17) . . . . ? C22 C3 C4 C5 8.2(3) . . . . ? N1 C4 C5 C6 3.0(2) . . . . ? C3 C4 C5 C6 179.16(17) . . . . ? N1 C4 C5 C24 -176.39(14) . . . . ? C3 C4 C5 C24 -0.2(3) . . . . ? C4 C5 C6 N2 2.2(2) . . . . ? C24 C5 C6 N2 -178.38(14) . . . . ? C4 C5 C6 C7 176.75(17) . . . . ? C24 C5 C6 C7 -3.9(3) . . . . ? C9 N2 C6 C5 174.56(15) . . . . ? B1 N2 C6 C5 -7.0(2) . . . . ? C9 N2 C6 C7 -1.18(19) . . . . ? B1 N2 C6 C7 177.24(15) . . . . ? C5 C6 C7 C34 6.4(3) . . . . ? N2 C6 C7 C34 -178.56(19) . . . . ? C5 C6 C7 C8 -173.95(18) . . . . ? N2 C6 C7 C8 1.07(19) . . . . ? C34 C7 C8 C37 -0.4(3) . . . . ? C6 C7 C8 C37 179.90(17) . . . . ? C34 C7 C8 C9 179.09(16) . . . . ? C6 C7 C8 C9 -0.61(19) . . . . ? C6 N2 C9 C8 0.8(2) . . . . ? B1 N2 C9 C8 -177.63(16) . . . . ? C6 N2 C9 C38 -178.63(17) . . . . ? B1 N2 C9 C38 2.9(3) . . . . ? C37 C8 C9 N2 179.32(19) . . . . ? C7 C8 C9 N2 -0.1(2) . . . . ? C37 C8 C9 C38 -1.3(3) . . . . ? C7 C8 C9 C38 179.30(18) . . . . ? C13 N3 C10 C11 0.10(18) . . . . ? B2 N3 C10 C11 173.09(14) . . . . ? C13 N3 C10 C39 179.66(14) . . . . ? B2 N3 C10 C39 -7.4(2) . . . . ? N3 C10 C11 C12 1.16(19) . . . . ? C39 C10 C11 C12 -178.37(16) . . . . ? N3 C10 C11 C22 176.25(17) . . . . ? C39 C10 C11 C22 -3.3(3) . . . . ? C10 C11 C12 C13 -1.94(19) . . . . ? C22 C11 C12 C13 -178.11(14) . . . . ? C10 C11 C12 C19 174.32(14) . . . . ? C22 C11 C12 C19 -1.9(2) . . . . ? C10 N3 C13 C12 -1.29(18) . . . . ? B2 N3 C13 C12 -174.38(14) . . . . ? C10 N3 C13 C14 176.97(15) . . . . ? B2 N3 C13 C14 3.9(2) . . . . ? C11 C12 C13 N3 1.97(18) . . . . ? C19 C12 C13 N3 -172.87(19) . . . . ? C11 C12 C13 C14 -176.04(17) . . . . ? C19 C12 C13 C14 9.1(4) . . . . ? N3 C13 C14 C15 4.4(2) . . . . ? C12 C13 C14 C15 -177.85(17) . . . . ? N3 C13 C14 C40 -171.49(14) . . . . ? C12 C13 C14 C40 6.3(3) . . . . ? C13 C14 C15 N4 -3.3(2) . . . . ? C40 C14 C15 N4 172.41(14) . . . . ? C13 C14 C15 C16 175.31(17) . . . . ? C40 C14 C15 C16 -9.0(3) . . . . ? C18 N4 C15 C14 179.53(15) . . . . ? B2 N4 C15 C14 -5.8(2) . . . . ? C18 N4 C15 C16 0.59(17) . . . . ? B2 N4 C15 C16 175.26(14) . . . . ? C14 C15 C16 C50 0.6(3) . . . . ? N4 C15 C16 C50 179.34(18) . . . . ? C14 C15 C16 C17 -179.21(17) . . . . ? N4 C15 C16 C17 -0.45(17) . . . . ? C50 C16 C17 C53 0.6(2) . . . . ? C15 C16 C17 C53 -179.54(15) . . . . ? C50 C16 C17 C18 -179.66(15) . . . . ? C15 C16 C17 C18 0.16(18) . . . . ? C15 N4 C18 C17 -0.50(18) . . . . ? B2 N4 C18 C17 -175.12(14) . . . . ? C15 N4 C18 C54 179.12(15) . . . . ? B2 N4 C18 C54 4.5(3) . . . . ? C53 C17 C18 N4 179.86(17) . . . . ? C16 C17 C18 N4 0.20(19) . . . . ? C53 C17 C18 C54 0.3(3) . . . . ? C16 C17 C18 C54 -179.40(16) . . . . ? C1 C2 C19 C12 131.3(2) . . . . ? C3 C2 C19 C12 -51.21(19) . . . . ? C1 C2 C19 C20 -117.8(2) . . . . ? C3 C2 C19 C20 59.69(18) . . . . ? C11 C12 C19 C2 52.90(19) . . . . ? C13 C12 C19 C2 -132.5(2) . . . . ? C11 C12 C19 C20 -56.63(19) . . . . ? C13 C12 C19 C20 118.0(2) . . . . ? C2 C19 C20 C21 -56.20(17) . . . . ? C12 C19 C20 C21 54.64(18) . . . . ? C19 C20 C21 C22 0.72(19) . . . . ? C12 C11 C22 C3 -51.09(19) . . . . ? C10 C11 C22 C3 134.1(2) . . . . ? C12 C11 C22 C21 59.07(18) . . . . ? C10 C11 C22 C21 -115.8(2) . . . . ? C2 C3 C22 C11 52.66(18) . . . . ? C4 C3 C22 C11 -131.7(2) . . . . ? C2 C3 C22 C21 -57.04(17) . . . . ? C4 C3 C22 C21 118.6(2) . . . . ? C20 C21 C22 C11 -55.70(17) . . . . ? C20 C21 C22 C3 55.17(17) . . . . ? C6 C5 C24 C25 -83.0(2) . . . . ? C4 C5 C24 C25 96.4(2) . . . . ? C6 C5 C24 C29 100.7(2) . . . . ? C4 C5 C24 C29 -79.9(2) . . . . ? C29 C24 C25 C26 0.5(3) . . . . ? C5 C24 C25 C26 -175.93(16) . . . . ? C24 C25 C26 C27 0.3(3) . . . . ? C25 C26 C27 C28 -0.6(3) . . . . ? C25 C26 C27 C30 175.73(16) . . . . ? C26 C27 C28 C29 0.1(2) . . . . ? C30 C27 C28 C29 -176.33(16) . . . . ? C27 C28 C29 C24 0.7(3) . . . . ? C25 C24 C29 C28 -1.0(3) . . . . ? C5 C24 C29 C28 175.43(16) . . . . ? C26 C27 C30 C31 -111.90(19) . . . . ? C28 C27 C30 C31 64.3(2) . . . . ? C26 C27 C30 C32 8.8(2) . . . . ? C28 C27 C30 C32 -175.04(16) . . . . ? C26 C27 C30 C33 129.62(18) . . . . ? C28 C27 C30 C33 -54.2(2) . . . . ? C8 C7 C34 C35 -0.3(3) . . . . ? C6 C7 C34 C35 179.28(19) . . . . ? C7 C34 C35 C36 0.8(3) . . . . ? C34 C35 C36 C37 -0.7(3) . . . . ? C35 C36 C37 C8 0.0(3) . . . . ? C7 C8 C37 C36 0.6(3) . . . . ? C9 C8 C37 C36 -178.8(2) . . . . ? C15 C14 C40 C41 90.6(2) . . . . ? C13 C14 C40 C41 -93.5(2) . . . . ? C15 C14 C40 C45 -90.7(2) . . . . ? C13 C14 C40 C45 85.2(2) . . . . ? C45 C40 C41 C42 0.9(3) . . . . ? C14 C40 C41 C42 179.63(18) . . . . ? C40 C41 C42 C43 -0.6(3) . . . . ? C41 C42 C43 C44 -0.1(3) . . . . ? C41 C42 C43 C46 179.40(19) . . . . ? C42 C43 C44 C45 0.5(3) . . . . ? C46 C43 C44 C45 -179.03(18) . . . . ? C43 C44 C45 C40 -0.2(3) . . . . ? C41 C40 C45 C44 -0.5(3) . . . . ? C14 C40 C45 C44 -179.28(17) . . . . ? C42 C43 C46 C47 116.0(2) . . . . ? C44 C43 C46 C47 -64.5(2) . . . . ? C42 C43 C46 C48 -5.1(3) . . . . ? C44 C43 C46 C48 174.43(17) . . . . ? C42 C43 C46 C49 -124.6(2) . . . . ? C44 C43 C46 C49 54.9(2) . . . . ? C17 C16 C50 C51 -0.5(2) . . . . ? C15 C16 C50 C51 179.70(18) . . . . ? C16 C50 C51 C52 0.1(3) . . . . ? C50 C51 C52 C53 0.3(3) . . . . ? C51 C52 C53 C17 -0.2(3) . . . . ? C16 C17 C53 C52 -0.3(3) . . . . ? C18 C17 C53 C52 -179.89(17) . . . . ? C1 N1 B1 F1 60.0(2) . . . . ? C4 N1 B1 F1 -119.7(2) . . . . ? C1 N1 B1 F2 -61.9(2) . . . . ? C4 N1 B1 F2 118.5(2) . . . . ? C1 N1 B1 N2 179.33(15) . . . . ? C4 N1 B1 N2 -0.3(2) . . . . ? C9 N2 B1 F1 -56.1(2) . . . . ? C6 N2 B1 F1 125.72(17) . . . . ? C9 N2 B1 F2 63.8(2) . . . . ? C6 N2 B1 F2 -114.40(18) . . . . ? C9 N2 B1 N1 -176.11(16) . . . . ? C6 N2 B1 N1 5.7(2) . . . . ? C10 N3 B2 F3 57.2(2) . . . . ? C13 N3 B2 F3 -130.84(16) . . . . ? C10 N3 B2 F4 -64.6(2) . . . . ? C13 N3 B2 F4 107.28(17) . . . . ? C10 N3 B2 N4 177.26(14) . . . . ? C13 N3 B2 N4 -10.8(2) . . . . ? C18 N4 B2 F3 -53.2(2) . . . . ? C15 N4 B2 F3 132.92(15) . . . . ? C18 N4 B2 F4 66.2(2) . . . . ? C15 N4 B2 F4 -107.61(16) . . . . ? C18 N4 B2 N3 -174.30(14) . . . . ? C15 N4 B2 N3 11.8(2) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 F1 C1 3.078(3) no . . F1 C4 3.536(3) no . . F1 C6 3.588(3) no . . F1 C9 3.020(4) no . . F1 C23 3.165(3) no . . F1 C38 3.027(4) no . . F2 C1 3.100(3) no . . F2 C4 3.5349(19) no . . F2 C6 3.506(3) no . . F2 C9 3.062(3) no . . F2 C23 3.183(4) no . . F2 C38 3.184(3) no . . F3 C10 3.073(2) no . . F3 C18 3.0171(18) no . . F3 C39 3.074(2) no . . F3 C54 3.0032(18) no . . F4 C10 3.1186(18) no . . F4 C13 3.450(3) no . . F4 C15 3.458(3) no . . F4 C18 3.093(3) no . . F4 C39 3.2930(16) no . . F4 C54 3.259(3) no . . N1 C6 2.845(4) no . . N2 C4 2.822(3) no . . N3 C15 2.846(3) no . . N4 C13 2.821(2) no . . C1 C5 3.588(3) no . . C1 C20 3.585(3) no . . C2 C11 2.772(3) no . . C2 C21 2.827(3) no . . C3 C12 2.790(3) no . . C3 C20 2.858(4) no . . C3 C24 3.059(4) no . . C3 C29 3.557(3) no . . C4 C25 3.392(4) no . . C4 C29 3.277(3) no . . C5 C9 3.545(3) no . . C5 C22 3.506(3) no . . C5 C34 3.357(4) no . . C5 B1 3.014(3) no . . C6 C25 3.318(3) no . . C6 C29 3.460(3) no . . C7 C24 3.136(3) no . . C7 C36 2.794(4) no . . C8 C35 2.766(5) no . . C10 C14 3.586(3) no . . C10 C21 3.590(3) no . . C11 C20 2.842(4) no . . C12 C21 2.856(2) no . . C12 C40 3.050(3) no . . C13 C41 3.381(4) no . . C13 C45 3.274(3) no . . C14 C18 3.541(3) no . . C14 C19 3.480(3) no . . C14 C50 3.344(3) no . . C14 B2 3.001(3) no . . C15 C41 3.377(3) no . . C15 C45 3.334(3) no . . C16 C40 3.118(3) no . . C16 C52 2.790(3) no . . C17 C51 2.755(3) no . . C19 C22 2.671(3) no . . C19 C23 3.386(3) no . . C19 C40 3.308(3) no . . C19 C41 3.580(4) no . . C22 C24 3.325(4) no . . C22 C29 3.435(3) no . . C22 C39 3.402(3) no . . C23 B1 3.084(4) no . . C24 C27 2.835(3) no . . C24 C34 3.278(4) no . . C25 C28 2.753(3) no . . C25 C34 3.560(3) no . . C26 C29 2.751(3) no . . C26 C31 3.529(3) no . . C26 C32 2.903(3) no . . C28 C31 3.073(3) no . . C28 C33 3.023(3) no . . C34 C37 2.832(4) no . . C37 C38 3.255(5) no . . C38 B1 3.054(4) no . . C39 B2 3.084(3) no . . C40 C43 2.825(3) no . . C40 C50 3.257(3) no . . C41 C44 2.744(3) no . . C41 C50 3.542(3) no . . C42 C45 2.740(4) no . . C42 C47 3.572(4) no . . C42 C48 2.887(3) no . . C44 C47 3.086(4) no . . C44 C49 3.000(3) no . . C50 C53 2.840(3) no . . C53 C54 3.250(4) no . . C54 B2 3.074(3) no . . C55 C58 2.664(10) no . . C56 C59 2.772(9) no . . C57 C60 2.770(9) no . . C61 C64 2.827(6) no . . C62 C65 2.749(15) no . . C63 C66 2.773(11) no . . Cl1 C64 3.498(5) no . . Cl2 O1 3.597(14) no . . F1 C28 3.531(3) no . 2_657 F3 N4 3.148(3) no . 2_656 F3 C14 3.313(3) no . 2_656 F3 C15 2.984(2) no . 2_656 F3 C16 3.3896(18) no . 2_656 F3 C18 3.597(3) no . 2_656 F4 C49 3.4680(19) no . 2_566 O1 Cl2 3.597(14) no . . N4 F3 3.148(3) no . 2_656 N4 C49 3.574(3) no . 2_566 C3 C68 3.492(7) no . . C4 C68 3.477(6) no . . C7 C21 3.475(3) no . 2_657 C14 F3 3.313(3) no . 2_656 C15 F3 2.984(2) no . 2_656 C16 F3 3.3896(18) no . 2_656 C18 F3 3.597(3) no . 2_656 C20 C34 3.581(3) no . 2_657 C21 C7 3.475(3) no . 2_657 C25 C68 3.325(5) no . . C28 F1 3.531(3) no . 2_657 C34 C20 3.581(3) no . 2_657 C39 C48 3.573(4) no . 1_655 C48 C39 3.573(4) no . 1_455 C49 F4 3.4680(19) no . 2_566 C49 N4 3.574(3) no . 2_566 C64 Cl1 3.498(5) no . . C68 C3 3.492(7) no . . C68 C4 3.477(6) no . . C68 C25 3.325(5) no . . Cl1 H56 2.8323 no . . Cl1 H60 2.8008 no . . Cl2 H62 2.8539 no . . Cl2 H66 2.7776 no . . F1 H23A 2.6498 no . . F1 H23C 3.3269 no . . F1 H38A 2.7968 no . . F1 H38C 2.8288 no . . F2 H23A 3.2615 no . . F2 H23C 2.7245 no . . F2 H38A 2.5176 no . . F3 H39A 2.7932 no . . F3 H39C 2.9149 no . . F3 H54A 2.5798 no . . F3 H54C 3.0030 no . . F3 H54E 2.2867 no . . F3 H54F 3.4456 no . . F4 H39C 2.6825 no . . F4 H54A 2.5744 no . . F4 H54E 3.0529 no . . F4 H54F 3.0992 no . . O1 H68A 2.2221 no . . O1 H68B 2.9298 no . . O1 H68C 3.0259 no . . O1 H69A 3.2945 no . . O1 H69B 2.6609 no . . O1 H69C 2.6526 no . . N1 H23A 2.7640 no . . N1 H23B 3.2969 no . . N1 H23C 2.7857 no . . N2 H38A 2.6531 no . . N2 H38B 3.2499 no . . N2 H38C 2.8801 no . . N3 H39A 2.8346 no . . N3 H39B 3.2838 no . . N3 H39C 2.7019 no . . N4 H54A 2.6054 no . . N4 H54B 3.2162 no . . N4 H54C 2.9454 no . . N4 H54D 3.2276 no . . N4 H54E 2.6193 no . . N4 H54F 2.9206 no . . C1 H19 2.8911 no . . C1 H20A 3.4995 no . . C2 H20A 2.6293 no . . C2 H20B 3.2860 no . . C2 H21B 3.1718 no . . C2 H22 3.3132 no . . C2 H23A 3.2134 no . . C2 H23B 2.6886 no . . C2 H23C 3.1866 no . . C3 H19 3.3225 no . . C3 H20A 3.1882 no . . C3 H21A 3.3201 no . . C3 H21B 2.6744 no . . C3 H29 3.5963 no . . C4 H22 2.9922 no . . C4 H25 3.4745 no . . C4 H29 3.2820 no . . C5 H22 3.3363 no . . C5 H25 2.6602 no . . C5 H29 2.6783 no . . C5 H34 3.2402 no . . C6 H25 3.2815 no . . C6 H29 3.5165 no . . C6 H34 2.9020 no . . C7 H35 3.2570 no . . C7 H37 3.3172 no . . C8 H34 3.2990 no . . C8 H36 3.2508 no . . C8 H38A 3.3053 no . . C8 H38B 2.7103 no . . C8 H38C 3.1002 no . . C9 H37 2.8408 no . . C10 H21A 3.5019 no . . C10 H22 2.9033 no . . C11 H19 3.3106 no . . C11 H20B 3.1900 no . . C11 H21A 2.6466 no . . C11 H21B 3.2963 no . . C11 H39A 3.1424 no . . C11 H39B 2.7020 no . . C11 H39C 3.2556 no . . C12 H20A 3.3210 no . . C12 H20B 2.6867 no . . C12 H21A 3.1932 no . . C12 H22 3.3190 no . . C13 H19 2.9719 no . . C13 H41 3.4479 no . . C13 H45 3.2658 no . . C14 H19 3.3020 no . . C14 H41 2.6886 no . . C14 H45 2.6224 no . . C14 H50 3.2308 no . . C15 H41 3.4188 no . . C15 H45 3.3404 no . . C15 H50 2.9036 no . . C16 H51 3.2513 no . . C16 H53 3.3216 no . . C17 H50 3.3009 no . . C17 H52 3.2461 no . . C17 H54A 3.3359 no . . C17 H54B 2.7349 no . . C17 H54C 3.0359 no . . C17 H54D 2.7243 no . . C17 H54E 3.3271 no . . C17 H54F 3.0550 no . . C18 H53 2.8484 no . . C19 H21A 3.2130 no . . C19 H21B 3.2222 no . . C19 H23B 3.0157 no . . C20 H22 3.4626 no . . C21 H19 3.4545 no . . C22 H20A 3.2216 no . . C22 H20B 3.2308 no . . C22 H29 3.5991 no . . C22 H39B 3.0572 no . . C23 H19 3.1365 no . . C23 H47A 3.3927 no . . C23 H47C 3.4160 no . . C24 H22 2.7443 no . . C24 H26 3.2625 no . . C24 H28 3.2642 no . . C24 H34 2.7493 no . . C25 H22 3.1512 no . . C25 H29 3.2466 no . . C25 H34 2.8860 no . . C26 H22 3.4775 no . . C26 H28 3.2357 no . . C26 H31B 3.4063 no . . C26 H32A 2.8417 no . . C26 H32B 2.7824 no . . C26 H34 3.4646 no . . C26 H39B 3.3775 no . . C27 H22 3.4674 no . . C27 H25 3.2752 no . . C27 H29 3.2800 no . . C27 H31A 3.3396 no . . C27 H31B 2.6792 no . . C27 H31C 2.6593 no . . C27 H32A 2.7381 no . . C27 H32B 2.7616 no . . C27 H32C 3.3883 no . . C27 H33A 2.6839 no . . C27 H33B 2.7292 no . . C27 H33C 3.3629 no . . C27 H39B 3.5915 no . . C28 H22 3.0670 no . . C28 H26 3.2366 no . . C28 H31B 3.3593 no . . C28 H31C 2.7605 no . . C28 H33A 2.6993 no . . C28 H33B 3.2909 no . . C29 H22 2.6988 no . . C29 H25 3.2475 no . . C29 H34 3.2215 no . . C30 H26 2.7282 no . . C30 H28 2.6762 no . . C31 H28 2.9645 no . . C31 H32A 3.3503 no . . C31 H32B 2.6741 no . . C31 H32C 2.6936 no . . C31 H33A 2.6888 no . . C31 H33B 3.3470 no . . C31 H33C 2.6659 no . . C31 H39B 3.5599 no . . C32 H26 2.5215 no . . C32 H31A 2.6715 no . . C32 H31B 2.6954 no . . C32 H31C 3.3508 no . . C32 H33A 3.3463 no . . C32 H33B 2.6771 no . . C32 H33C 2.6712 no . . C33 H28 2.7974 no . . C33 H31A 2.6695 no . . C33 H31B 3.3483 no . . C33 H31C 2.6820 no . . C33 H32A 2.7004 no . . C33 H32B 3.3463 no . . C33 H32C 2.6465 no . . C34 H36 3.2899 no . . C35 H37 3.2758 no . . C36 H34 3.2988 no . . C37 H35 3.2621 no . . C37 H38B 2.9269 no . . C38 H37 3.0576 no . . C39 H22 3.1631 no . . C39 H31B 3.3784 no . . C40 H19 2.7233 no . . C40 H42 3.2553 no . . C40 H44 3.2528 no . . C40 H50 2.7336 no . . C41 H19 2.8032 no . . C41 H45 3.2336 no . . C41 H50 2.8377 no . . C42 H19 3.2471 no . . C42 H44 3.2232 no . . C42 H47A 3.4653 no . . C42 H48A 2.8325 no . . C42 H48C 2.7526 no . . C42 H49C 3.5628 no . . C42 H50 3.3637 no . . C43 H19 3.5900 no . . C43 H23B 3.4791 no . . C43 H41 3.2755 no . . C43 H45 3.2720 no . . C43 H47A 2.6822 no . . C43 H47B 3.3494 no . . C43 H47C 2.6904 no . . C43 H48A 2.7421 no . . C43 H48B 3.3797 no . . C43 H48C 2.7297 no . . C43 H49A 2.6956 no . . C43 H49B 3.3513 no . . C43 H49C 2.6785 no . . C44 H19 3.4775 no . . C44 H23B 3.2582 no . . C44 H42 3.2242 no . . C44 H47A 3.3544 no . . C44 H47C 2.7988 no . . C44 H49A 2.7093 no . . C44 H49C 3.2176 no . . C45 H19 3.0776 no . . C45 H41 3.2351 no . . C45 H50 3.1903 no . . C46 H42 2.7289 no . . C46 H44 2.6629 no . . C47 H23B 3.2098 no . . C47 H44 2.9427 no . . C47 H48A 3.3448 no . . C47 H48B 2.6630 no . . C47 H48C 2.6960 no . . C47 H49A 2.6741 no . . C47 H49B 2.6969 no . . C47 H49C 3.3495 no . . C48 H42 2.5065 no . . C48 H47A 2.7045 no . . C48 H47B 2.6531 no . . C48 H47C 3.3449 no . . C48 H49A 3.3392 no . . C48 H49B 2.6430 no . . C48 H49C 2.6907 no . . C49 H44 2.8041 no . . C49 H47A 3.3513 no . . C49 H47B 2.6920 no . . C49 H47C 2.6745 no . . C49 H48A 2.6605 no . . C49 H48B 2.6703 no . . C49 H48C 3.3409 no . . C50 H52 3.2858 no . . C51 H53 3.2746 no . . C52 H50 3.2964 no . . C53 H51 3.2584 no . . C53 H54B 2.9842 no . . C53 H54C 3.5676 no . . C53 H54D 2.9612 no . . C54 H53 3.0575 no . . C55 H57 3.2094 no . . C55 H59 3.2002 no . . C56 H58 3.2475 no . . C56 H60 3.2749 no . . C57 H59 3.2422 no . . C58 H56 3.2740 no . . C58 H60 3.1966 no . . C59 H57 3.2275 no . . C60 H56 3.2694 no . . C60 H58 3.1958 no . . C61 H63 3.3048 no . . C61 H65 3.2717 no . . C62 H64 3.2635 no . . C62 H66 3.2589 no . . C63 H65 3.2121 no . . C64 H62 3.2522 no . . C64 H66 3.2685 no . . C65 H63 3.2189 no . . C66 H62 3.2567 no . . C66 H64 3.2708 no . . C68 H69A 2.5857 no . . C68 H69B 3.2105 no . . C68 H69C 2.4641 no . . C68 H1 2.6710 no . . C69 H68A 2.9315 no . . C69 H68B 3.0660 no . . C69 H68C 2.2461 no . . C69 H1 2.4144 no . . B1 H23A 3.0019 no . . B1 H23C 3.0621 no . . B1 H38A 2.7622 no . . B1 H38C 3.2735 no . . B2 H39A 3.2159 no . . B2 H39C 2.8622 no . . B2 H54A 2.6845 no . . B2 H54C 3.4432 no . . B2 H54E 2.7498 no . . B2 H54F 3.3387 no . . H56 H57 2.3532 no . . H57 H58 2.3781 no . . H58 H59 2.2165 no . . H59 H60 2.3720 no . . H62 H63 2.3627 no . . H63 H64 2.3261 no . . H64 H65 2.3412 no . . H65 H66 2.3255 no . . H67 H68A 2.7436 no . . H67 H68B 2.1837 no . . H67 H68C 2.6627 no . . H67 H69A 2.3518 no . . H67 H69B 2.4184 no . . H67 H69C 2.8712 no . . H67 H1 2.6970 no . . H68A H69A 3.3672 no . . H68A H69C 2.8049 no . . H68A H1 2.4565 no . . H68B H69A 3.1105 no . . H68B H69C 3.3516 no . . H68B H1 3.4503 no . . H68C H69A 2.2452 no . . H68C H69B 3.2173 no . . H68C H69C 2.1690 no . . H68C H1 3.1735 no . . H69A H1 3.3541 no . . H69B H1 2.5482 no . . H69C H1 2.3421 no . . H19 H20A 2.4737 no . . H19 H20B 2.4727 no . . H19 H23B 2.5084 no . . H19 H41 3.1415 no . . H19 H45 3.5542 no . . H20A H21A 2.7330 no . . H20A H21B 2.2096 no . . H20B H21A 2.2097 no . . H20B H21B 2.7259 no . . H21A H22 2.4778 no . . H21B H22 2.4776 no . . H21B H29 3.4547 no . . H22 H28 3.5642 no . . H22 H29 3.0340 no . . H22 H39B 2.5605 no . . H23A H47A 3.3919 no . . H23B H44 3.3568 no . . H23B H47A 2.6813 no . . H23B H47C 2.8999 no . . H23C H44 3.5839 no . . H23C H47C 3.2175 no . . H25 H26 2.3137 no . . H25 H34 3.1432 no . . H26 H31B 3.5319 no . . H26 H32A 2.3612 no . . H26 H32B 2.2404 no . . H26 H32C 3.4892 no . . H26 H39B 3.4844 no . . H28 H29 2.3107 no . . H28 H31B 3.4485 no . . H28 H31C 2.4151 no . . H28 H33A 2.2030 no . . H28 H33B 3.2189 no . . H31A H32A 3.5739 no . . H31A H32B 2.9327 no . . H31A H32C 2.4940 no . . H31A H33A 2.9641 no . . H31A H33B 3.5617 no . . H31A H33C 2.4668 no . . H31B H32A 3.5827 no . . H31B H32B 2.4987 no . . H31B H32C 2.9968 no . . H31B H33A 3.5860 no . . H31B H33C 3.5627 no . . H31B H39A 3.2375 no . . H31B H39B 2.6769 no . . H31C H32B 3.5773 no . . H31C H32C 3.5807 no . . H31C H33A 2.5048 no . . H31C H33B 3.5821 no . . H31C H33C 2.9486 no . . H32A H33A 3.5922 no . . H32A H33B 2.5143 no . . H32A H33C 2.9879 no . . H32B H33B 3.5856 no . . H32B H33C 3.5556 no . . H32C H33A 3.5485 no . . H32C H33B 2.9173 no . . H32C H33C 2.4502 no . . H34 H35 2.3415 no . . H35 H36 2.3429 no . . H36 H37 2.3223 no . . H37 H38B 2.4895 no . . H37 H38C 3.4520 no . . H41 H42 2.3222 no . . H41 H50 3.1251 no . . H42 H47A 3.5861 no . . H42 H48A 2.3603 no . . H42 H48B 3.4719 no . . H42 H48C 2.2054 no . . H44 H45 2.3085 no . . H44 H47A 3.3963 no . . H44 H47C 2.4033 no . . H44 H49A 2.2371 no . . H44 H49C 3.1924 no . . H47A H48B 2.9746 no . . H47A H48C 2.5371 no . . H47A H49A 3.5682 no . . H47A H49B 3.5937 no . . H47B H48A 3.5465 no . . H47B H48B 2.4465 no . . H47B H48C 2.9475 no . . H47B H49A 2.9621 no . . H47B H49B 2.5190 no . . H47B H49C 3.5897 no . . H47C H48B 3.5496 no . . H47C H48C 3.5989 no . . H47C H49A 2.4758 no . . H47C H49B 2.9700 no . . H47C H49C 3.5656 no . . H48A H49A 3.5694 no . . H48A H49B 2.9024 no . . H48A H49C 2.4934 no . . H48B H49A 3.5543 no . . H48B H49B 2.4528 no . . H48B H49C 2.9870 no . . H48C H49B 3.5489 no . . H48C H49C 3.5806 no . . H50 H51 2.3370 no . . H51 H52 2.3315 no . . H52 H53 2.3267 no . . H53 H54B 2.5728 no . . H53 H54C 3.3017 no . . H53 H54D 2.5409 no . . H53 H54F 3.3508 no . . Cl1 H64 2.5852 no . . Cl2 H69C 3.1186 no . . Cl2 H1 2.7579 no . . F1 H28 2.6746 no . 2_657 F1 H31C 2.7241 no . 2_657 F1 H33A 3.3762 no . 2_657 F1 H38A 3.2072 no . 2_567 F2 H69C 3.3214 no . . F2 H31A 2.9301 no . 1_465 F2 H31C 3.4497 no . 1_465 F2 H35 3.4075 no . 2_667 F2 H51 3.4906 no . 2_566 F2 H52 3.1651 no . 2_566 F3 H41 3.4089 no . 2_656 F4 H67 3.0542 no . . F4 H48A 3.3512 no . 1_655 F4 H49A 3.4645 no . 2_566 F4 H49B 2.8695 no . 2_566 F4 H49C 3.5458 no . 2_566 O1 H66 3.5299 no . . N1 H68C 3.0478 no . . N1 H69A 3.3940 no . . N1 H69C 3.5815 no . . N1 H28 3.1409 no . 2_657 N1 H29 3.3029 no . 2_657 N2 H21B 3.4966 no . 2_657 N3 H67 3.2301 no . . N3 H54C 3.1882 no . 2_656 N4 H49A 2.9326 no . 2_566 N4 H49B 3.3739 no . 2_566 C1 H68C 3.4380 no . . C1 H69A 2.9236 no . . C1 H28 3.1671 no . 2_657 C1 H29 3.5144 no . 2_657 C2 H68C 3.2889 no . . C2 H69A 2.8916 no . . C2 H29 3.3090 no . 2_657 C3 H68B 3.3585 no . . C3 H68C 2.7716 no . . C3 H69A 3.3668 no . . C3 H29 2.9388 no . 2_657 C4 H68C 2.5819 no . . C4 H29 2.9415 no . 2_657 C5 H68C 2.9469 no . . C5 H21B 2.9498 no . 2_657 C5 H29 3.5466 no . 2_657 C6 H21A 3.5597 no . 2_657 C6 H21B 2.8008 no . 2_657 C6 H36 3.5611 no . 2_667 C7 H20A 3.5925 no . 2_657 C7 H21A 3.2924 no . 2_657 C7 H21B 2.9151 no . 2_657 C8 H21A 3.3873 no . 2_657 C8 H53 3.5926 no . 1_556 C9 H35 3.5229 no . 2_667 C9 H53 3.4743 no . 1_556 C10 H67 3.4044 no . . C10 H68B 3.0558 no . . C10 H54C 3.3728 no . 2_656 C11 H68B 3.0678 no . . C11 H68C 3.5349 no . . C11 H54C 3.2022 no . 2_656 C11 H54D 3.3581 no . 2_656 C12 H69A 3.2268 no . . C12 H54C 2.8724 no . 2_656 C12 H54D 3.3122 no . 2_656 C12 H54E 3.5142 no . 2_656 C13 H67 3.3772 no . . C13 H69A 3.5868 no . . C13 H54C 2.8880 no . 2_656 C13 H54D 3.5980 no . 2_656 C13 H54E 3.2555 no . 2_656 C14 H49A 3.3753 no . 2_566 C14 H54C 3.5340 no . 2_656 C14 H54E 3.5506 no . 2_656 C15 H49A 2.7365 no . 2_566 C16 H39A 3.1514 no . 2_656 C16 H44 3.0914 no . 2_566 C16 H47C 3.5843 no . 2_566 C16 H49A 2.8529 no . 2_566 C17 H39A 2.9564 no . 2_656 C17 H47C 3.2120 no . 2_566 C17 H49A 3.0873 no . 2_566 C18 H49A 3.1265 no . 2_566 C18 H49B 3.4134 no . 2_566 C19 H69A 3.4379 no . . C19 H54C 3.4538 no . 2_656 C20 H29 3.4896 no . 2_657 C20 H32C 3.5614 no . 1_455 C20 H54B 3.5836 no . 2_656 C20 H54C 3.0520 no . 2_656 C20 H54D 2.9501 no . 2_656 C21 H29 3.0911 no . 2_657 C21 H53 3.4852 no . 2_656 C21 H54C 3.4056 no . 2_656 C21 H54D 3.0235 no . 2_656 C22 H68B 3.4277 no . . C22 H68C 3.5472 no . . C22 H29 3.5079 no . 2_657 C23 H69A 3.4187 no . . C23 H28 3.4752 no . 2_657 C23 H33A 3.4312 no . 2_657 C23 H38C 3.4823 no . 2_567 C24 H68C 3.4209 no . . C24 H21B 3.2142 no . 2_657 C25 H68A 3.1900 no . . C25 H68B 2.9917 no . . C25 H68C 3.2368 no . . C25 H37 3.4509 no . 2_667 C26 H33B 3.2601 no . 2_757 C26 H47A 3.3163 no . 1_655 C26 H48C 3.2414 no . 1_655 C27 H33B 3.1417 no . 2_757 C29 H20A 3.2715 no . 2_657 C29 H21B 2.9229 no . 2_657 C30 H33B 3.3729 no . 2_757 C31 H35 3.5744 no . 2_757 C31 H38A 3.5507 no . 1_645 C31 H52 3.0384 no . 2_656 C32 H20A 3.5414 no . 1_655 C32 H33B 3.4616 no . 2_757 C32 H35 3.5702 no . 2_757 C33 H23A 3.4869 no . 2_657 C33 H32A 3.4601 no . 2_757 C33 H33B 3.0879 no . 2_757 C33 H34 3.3188 no . 2_757 C33 H35 3.3744 no . 2_757 C33 H38A 3.1558 no . 1_645 C33 H38B 3.2075 no . 1_645 C34 H20A 3.0476 no . 2_657 C34 H20B 3.4978 no . 2_657 C34 H21B 3.3122 no . 2_657 C34 H33C 3.0996 no . 2_757 C35 H20A 3.5439 no . 2_657 C35 H20B 3.5017 no . 2_657 C35 H32C 3.3487 no . 2_757 C35 H33C 3.0780 no . 2_757 C36 H54B 3.3785 no . 1_556 C37 H25 3.3048 no . 2_667 C37 H47B 3.4724 no . 2_567 C37 H54B 3.2805 no . 1_556 C38 H23A 3.1481 no . 2_567 C38 H33A 3.2061 no . 1_465 C38 H33C 3.1558 no . 1_465 C38 H52 3.4475 no . 1_556 C38 H53 3.4403 no . 1_556 C39 H68B 3.2873 no . . C39 H48A 3.4165 no . 1_655 C39 H48B 3.4790 no . 1_655 C39 H48C 3.2369 no . 1_655 C42 H32B 3.5371 no . 1_455 C44 H45 3.3945 no . 2_566 C45 H69A 3.2941 no . . C45 H69B 3.4737 no . . C45 H44 3.5253 no . 2_566 C47 H26 3.1752 no . 1_455 C47 H37 3.3768 no . 2_567 C48 H26 3.2714 no . 1_455 C48 H39B 3.4799 no . 1_455 C48 H39C 2.8081 no . 1_455 C50 H39A 3.3766 no . 2_656 C50 H44 2.8559 no . 2_566 C51 H23C 3.0936 no . 2_566 C51 H31B 3.5698 no . 2_656 C51 H39A 3.4024 no . 2_656 C51 H44 3.2927 no . 2_566 C52 H23C 3.0043 no . 2_566 C52 H31B 3.1706 no . 2_656 C52 H31C 3.4355 no . 2_656 C52 H38C 3.0419 no . 1_554 C52 H39A 3.2465 no . 2_656 C52 H47C 3.3631 no . 2_566 C53 H21A 3.3055 no . 2_656 C53 H38C 3.1898 no . 1_554 C53 H39A 3.0319 no . 2_656 C53 H47C 3.1070 no . 2_566 C54 H20B 2.9356 no . 2_656 C54 H21A 3.3338 no . 2_656 C55 H64 3.1623 no . . C56 H64 3.2033 no . . C61 H1 3.3908 no . . C63 H56 3.4570 no . . C64 H56 3.4386 no . . C66 H1 3.4252 no . . C68 H25 2.6918 no . . C69 H45 3.0976 no . . B1 H28 3.4321 no . 2_657 H56 C63 3.4570 no . . H56 C64 3.4386 no . . H56 H63 2.8935 no . . H56 H64 2.8083 no . . H63 H56 2.8935 no . . H64 Cl1 2.5852 no . . H64 C55 3.1623 no . . H64 C56 3.2033 no . . H64 H56 2.8083 no . . H66 O1 3.5299 no . . H66 H1 2.9812 no . . H67 F4 3.0542 no . . H67 N3 3.2301 no . . H67 C10 3.4044 no . . H67 C13 3.3772 no . . H67 H45 3.5742 no . . H68A C25 3.1900 no . . H68A H25 2.3627 no . . H68B C3 3.3585 no . . H68B C10 3.0558 no . . H68B C11 3.0678 no . . H68B C22 3.4277 no . . H68B C25 2.9917 no . . H68B C39 3.2873 no . . H68B H22 3.3718 no . . H68B H25 2.5548 no . . H68B H39B 3.0899 no . . H68B H39C 3.1588 no . . H68C N1 3.0478 no . . H68C C1 3.4380 no . . H68C C2 3.2889 no . . H68C C3 2.7716 no . . H68C C4 2.5819 no . . H68C C5 2.9469 no . . H68C C11 3.5349 no . . H68C C22 3.5472 no . . H68C C24 3.4209 no . . H68C C25 3.2368 no . . H68C H25 2.7101 no . . H69A N1 3.3940 no . . H69A C1 2.9236 no . . H69A C2 2.8916 no . . H69A C3 3.3668 no . . H69A C12 3.2268 no . . H69A C13 3.5868 no . . H69A C19 3.4379 no . . H69A C23 3.4187 no . . H69A C45 3.2941 no . . H69A H19 3.5929 no . . H69A H23B 3.5686 no . . H69A H23C 3.1324 no . . H69A H45 2.7257 no . . H69B C45 3.4737 no . . H69B H45 2.6273 no . . H69C Cl2 3.1186 no . . H69C F2 3.3214 no . . H69C N1 3.5815 no . . H69C H23C 3.4553 no . . H19 H69A 3.5929 no . . H20A C7 3.5925 no . 2_657 H20A C29 3.2715 no . 2_657 H20A C32 3.5414 no . 1_455 H20A C34 3.0476 no . 2_657 H20A C35 3.5439 no . 2_657 H20A H29 3.0213 no . 2_657 H20A H32A 3.2798 no . 1_455 H20A H32C 2.9159 no . 1_455 H20A H34 2.8615 no . 2_657 H20B C34 3.4978 no . 2_657 H20B C35 3.5017 no . 2_657 H20B C54 2.9356 no . 2_656 H20B H32C 3.3835 no . 1_455 H20B H54A 3.3472 no . 2_656 H20B H54B 2.7643 no . 2_656 H20B H54C 2.3221 no . 2_656 H20B H54D 2.2258 no . 2_656 H20B H54E 2.9183 no . 2_656 H20B H54F 3.2811 no . 2_656 H21A C6 3.5597 no . 2_657 H21A C7 3.2924 no . 2_657 H21A C8 3.3873 no . 2_657 H21A C53 3.3055 no . 2_656 H21A C54 3.3338 no . 2_656 H21A H53 2.5164 no . 2_656 H21A H54B 2.9059 no . 2_656 H21A H54C 2.9345 no . 2_656 H21A H54D 2.3575 no . 2_656 H21B N2 3.4966 no . 2_657 H21B C5 2.9498 no . 2_657 H21B C6 2.8008 no . 2_657 H21B C7 2.9151 no . 2_657 H21B C24 3.2142 no . 2_657 H21B C29 2.9229 no . 2_657 H21B C34 3.3122 no . 2_657 H21B H29 2.3290 no . 2_657 H21B H34 3.3882 no . 2_657 H22 H68B 3.3718 no . . H23A C33 3.4869 no . 2_657 H23A C38 3.1481 no . 2_567 H23A H28 2.8836 no . 2_657 H23A H33A 2.5293 no . 2_657 H23A H38A 3.0623 no . 2_567 H23A H38B 2.9348 no . 2_567 H23A H38C 2.9123 no . 2_567 H23B H69A 3.5686 no . . H23B H32A 3.5194 no . 1_455 H23C C51 3.0936 no . 2_566 H23C C52 3.0043 no . 2_566 H23C H69A 3.1324 no . . H23C H69C 3.4553 no . . H23C H38C 3.1843 no . 2_567 H23C H51 2.9185 no . 2_566 H23C H52 2.7598 no . 2_566 H25 C37 3.3048 no . 2_667 H25 C68 2.6918 no . . H25 H68A 2.3627 no . . H25 H68B 2.5548 no . . H25 H68C 2.7101 no . . H25 H36 3.2629 no . 2_667 H25 H37 2.6780 no . 2_667 H25 H47A 3.4900 no . 1_655 H25 H47B 3.0883 no . 1_655 H25 H48B 3.3641 no . 1_655 H26 C47 3.1752 no . 1_655 H26 C48 3.2714 no . 1_655 H26 H33B 3.3228 no . 2_757 H26 H47A 2.4416 no . 1_655 H26 H47B 3.1798 no . 1_655 H26 H48B 3.2930 no . 1_655 H26 H48C 2.5539 no . 1_655 H28 F1 2.6746 no . 2_657 H28 N1 3.1409 no . 2_657 H28 C1 3.1671 no . 2_657 H28 C23 3.4752 no . 2_657 H28 B1 3.4321 no . 2_657 H28 H23A 2.8836 no . 2_657 H29 N1 3.3029 no . 2_657 H29 C1 3.5144 no . 2_657 H29 C2 3.3090 no . 2_657 H29 C3 2.9388 no . 2_657 H29 C4 2.9415 no . 2_657 H29 C5 3.5466 no . 2_657 H29 C20 3.4896 no . 2_657 H29 C21 3.0911 no . 2_657 H29 C22 3.5079 no . 2_657 H29 H20A 3.0213 no . 2_657 H29 H21B 2.3290 no . 2_657 H29 H29 3.0912 no . 2_657 H31A F2 2.9301 no . 1_645 H31A H35 2.7296 no . 2_757 H31A H38A 3.1831 no . 1_645 H31A H51 3.4767 no . 2_656 H31A H52 3.0593 no . 2_656 H31B C51 3.5698 no . 2_656 H31B C52 3.1706 no . 2_656 H31B H51 3.5332 no . 2_656 H31B H52 2.8371 no . 2_656 H31C F1 2.7241 no . 2_657 H31C F2 3.4497 no . 1_645 H31C C52 3.4355 no . 2_656 H31C H38A 3.1637 no . 1_645 H31C H52 2.7104 no . 2_656 H32A C33 3.4601 no . 2_757 H32A H20A 3.2798 no . 1_655 H32A H23B 3.5194 no . 1_655 H32A H33A 3.3188 no . 2_757 H32A H33B 2.7274 no . 2_757 H32A H47A 3.3259 no . 1_655 H32B C42 3.5371 no . 1_655 H32B H42 3.0472 no . 1_655 H32B H47A 3.3594 no . 1_655 H32B H48C 2.7064 no . 1_655 H32C C20 3.5614 no . 1_655 H32C C35 3.3487 no . 2_757 H32C H20A 2.9159 no . 1_655 H32C H20B 3.3835 no . 1_655 H32C H34 3.3018 no . 2_757 H32C H35 2.7209 no . 2_757 H33A F1 3.3762 no . 2_657 H33A C23 3.4312 no . 2_657 H33A C38 3.2061 no . 1_645 H33A H23A 2.5293 no . 2_657 H33A H32A 3.3188 no . 2_757 H33A H33B 3.5481 no . 2_757 H33A H38A 2.7234 no . 1_645 H33A H38B 2.8232 no . 1_645 H33B C26 3.2601 no . 2_757 H33B C27 3.1417 no . 2_757 H33B C30 3.3729 no . 2_757 H33B C32 3.4616 no . 2_757 H33B C33 3.0879 no . 2_757 H33B H26 3.3228 no . 2_757 H33B H32A 2.7274 no . 2_757 H33B H33A 3.5481 no . 2_757 H33B H33B 2.2343 no . 2_757 H33B H34 3.2697 no . 2_757 H33C C34 3.0996 no . 2_757 H33C C35 3.0780 no . 2_757 H33C C38 3.1558 no . 1_645 H33C H34 2.5314 no . 2_757 H33C H35 2.4654 no . 2_757 H33C H38A 2.7305 no . 1_645 H33C H38B 2.7502 no . 1_645 H34 C33 3.3188 no . 2_757 H34 H20A 2.8615 no . 2_657 H34 H21B 3.3882 no . 2_657 H34 H32C 3.3018 no . 2_757 H34 H33B 3.2697 no . 2_757 H34 H33C 2.5314 no . 2_757 H35 F2 3.4075 no . 2_667 H35 C9 3.5229 no . 2_667 H35 C31 3.5744 no . 2_757 H35 C32 3.5702 no . 2_757 H35 C33 3.3744 no . 2_757 H35 H31A 2.7296 no . 2_757 H35 H32C 2.7209 no . 2_757 H35 H33C 2.4654 no . 2_757 H35 H38A 3.4101 no . 2_667 H36 C6 3.5611 no . 2_667 H36 H25 3.2629 no . 2_667 H36 H54B 3.4835 no . 1_556 H36 H54F 3.4586 no . 1_556 H37 C25 3.4509 no . 2_667 H37 C47 3.3768 no . 2_567 H37 H25 2.6780 no . 2_667 H37 H47A 3.5053 no . 2_567 H37 H47B 2.5976 no . 2_567 H37 H47C 3.5919 no . 2_567 H37 H54B 3.3247 no . 1_556 H38A F1 3.2072 no . 2_567 H38A C31 3.5507 no . 1_465 H38A C33 3.1558 no . 1_465 H38A H23A 3.0623 no . 2_567 H38A H31A 3.1831 no . 1_465 H38A H31C 3.1637 no . 1_465 H38A H33A 2.7234 no . 1_465 H38A H33C 2.7305 no . 1_465 H38A H35 3.4101 no . 2_667 H38B C33 3.2075 no . 1_465 H38B H23A 2.9348 no . 2_567 H38B H33A 2.8232 no . 1_465 H38B H33C 2.7502 no . 1_465 H38B H47A 3.3275 no . 2_567 H38B H47B 3.4940 no . 2_567 H38B H47C 3.5273 no . 2_567 H38C C23 3.4823 no . 2_567 H38C C52 3.0419 no . 1_556 H38C C53 3.1898 no . 1_556 H38C H23A 2.9123 no . 2_567 H38C H23C 3.1843 no . 2_567 H38C H52 2.4686 no . 1_556 H38C H53 2.7850 no . 1_556 H39A C16 3.1514 no . 2_656 H39A C17 2.9564 no . 2_656 H39A C50 3.3766 no . 2_656 H39A C51 3.4024 no . 2_656 H39A C52 3.2465 no . 2_656 H39A C53 3.0319 no . 2_656 H39A H53 3.4713 no . 2_656 H39B C48 3.4799 no . 1_655 H39B H68B 3.0899 no . . H39B H48A 3.5797 no . 1_655 H39B H48B 3.3768 no . 1_655 H39B H48C 2.9458 no . 1_655 H39C C48 2.8081 no . 1_655 H39C H68B 3.1588 no . . H39C H48A 2.5024 no . 1_655 H39C H48B 2.8071 no . 1_655 H39C H48C 2.6423 no . 1_655 H41 F3 3.4089 no . 2_656 H41 H54C 3.5661 no . 2_656 H41 H54E 3.2123 no . 2_656 H42 H32B 3.0472 no . 1_455 H44 C16 3.0914 no . 2_566 H44 C45 3.5253 no . 2_566 H44 C50 2.8559 no . 2_566 H44 C51 3.2927 no . 2_566 H44 H45 3.2158 no . 2_566 H44 H50 2.9875 no . 2_566 H45 C44 3.3945 no . 2_566 H45 C69 3.0976 no . . H45 H67 3.5742 no . . H45 H69A 2.7257 no . . H45 H69B 2.6273 no . . H45 H44 3.2158 no . 2_566 H45 H49A 3.1939 no . 2_566 H45 H49C 3.2785 no . 2_566 H45 H50 3.4932 no . 2_566 H47A C26 3.3163 no . 1_455 H47A H25 3.4900 no . 1_455 H47A H26 2.4416 no . 1_455 H47A H32A 3.3259 no . 1_455 H47A H32B 3.3594 no . 1_455 H47A H37 3.5053 no . 2_567 H47A H38B 3.3275 no . 2_567 H47B C37 3.4724 no . 2_567 H47B H25 3.0883 no . 1_455 H47B H26 3.1798 no . 1_455 H47B H37 2.5976 no . 2_567 H47B H38B 3.4940 no . 2_567 H47B H54F 3.5583 no . 2_566 H47C C16 3.5843 no . 2_566 H47C C17 3.2120 no . 2_566 H47C C52 3.3631 no . 2_566 H47C C53 3.1070 no . 2_566 H47C H37 3.5919 no . 2_567 H47C H38B 3.5273 no . 2_567 H47C H53 3.4014 no . 2_566 H48A F4 3.3512 no . 1_455 H48A C39 3.4165 no . 1_455 H48A H39B 3.5797 no . 1_455 H48A H39C 2.5024 no . 1_455 H48B C39 3.4790 no . 1_455 H48B H25 3.3641 no . 1_455 H48B H26 3.2930 no . 1_455 H48B H39B 3.3768 no . 1_455 H48B H39C 2.8071 no . 1_455 H48C C26 3.2414 no . 1_455 H48C C39 3.2369 no . 1_455 H48C H26 2.5539 no . 1_455 H48C H32B 2.7064 no . 1_455 H48C H39B 2.9458 no . 1_455 H48C H39C 2.6423 no . 1_455 H49A F4 3.4645 no . 2_566 H49A N4 2.9326 no . 2_566 H49A C14 3.3753 no . 2_566 H49A C15 2.7365 no . 2_566 H49A C16 2.8529 no . 2_566 H49A C17 3.0873 no . 2_566 H49A C18 3.1265 no . 2_566 H49A H45 3.1939 no . 2_566 H49B F4 2.8695 no . 2_566 H49B N4 3.3739 no . 2_566 H49B C18 3.4134 no . 2_566 H49B H54A 3.5474 no . 2_566 H49B H54F 3.2426 no . 2_566 H49C F4 3.5458 no . 2_566 H49C H45 3.2785 no . 2_566 H50 H44 2.9875 no . 2_566 H50 H45 3.4932 no . 2_566 H51 F2 3.4906 no . 2_566 H51 H23C 2.9185 no . 2_566 H51 H31A 3.4767 no . 2_656 H51 H31B 3.5332 no . 2_656 H52 F2 3.1651 no . 2_566 H52 C31 3.0384 no . 2_656 H52 C38 3.4475 no . 1_554 H52 H23C 2.7598 no . 2_566 H52 H31A 3.0593 no . 2_656 H52 H31B 2.8371 no . 2_656 H52 H31C 2.7104 no . 2_656 H52 H38C 2.4686 no . 1_554 H53 C8 3.5926 no . 1_554 H53 C9 3.4743 no . 1_554 H53 C21 3.4852 no . 2_656 H53 C38 3.4403 no . 1_554 H53 H21A 2.5164 no . 2_656 H53 H38C 2.7850 no . 1_554 H53 H39A 3.4713 no . 2_656 H53 H47C 3.4014 no . 2_566 H54A H20B 3.3472 no . 2_656 H54A H49B 3.5474 no . 2_566 H54B C20 3.5836 no . 2_656 H54B C36 3.3785 no . 1_554 H54B C37 3.2805 no . 1_554 H54B H20B 2.7643 no . 2_656 H54B H21A 2.9059 no . 2_656 H54B H36 3.4835 no . 1_554 H54B H37 3.3247 no . 1_554 H54C N3 3.1882 no . 2_656 H54C C10 3.3728 no . 2_656 H54C C11 3.2022 no . 2_656 H54C C12 2.8724 no . 2_656 H54C C13 2.8880 no . 2_656 H54C C14 3.5340 no . 2_656 H54C C19 3.4538 no . 2_656 H54C C20 3.0520 no . 2_656 H54C C21 3.4056 no . 2_656 H54C H20B 2.3221 no . 2_656 H54C H21A 2.9345 no . 2_656 H54C H41 3.5661 no . 2_656 H1 Cl2 2.7579 no . . H1 C61 3.3908 no . . H1 C66 3.4252 no . . H1 H66 2.9812 no . . H54D C11 3.3581 no . 2_656 H54D C12 3.3122 no . 2_656 H54D C13 3.5980 no . 2_656 H54D C20 2.9501 no . 2_656 H54D C21 3.0235 no . 2_656 H54D H20B 2.2258 no . 2_656 H54D H21A 2.3575 no . 2_656 H54E C12 3.5142 no . 2_656 H54E C13 3.2555 no . 2_656 H54E C14 3.5506 no . 2_656 H54E H20B 2.9183 no . 2_656 H54E H41 3.2123 no . 2_656 H54F H20B 3.2811 no . 2_656 H54F H36 3.4586 no . 1_554 H54F H47B 3.5583 no . 2_566 H54F H49B 3.2426 no . 2_566 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_20100730 _database_code_depnum_ccdc_archive 'CCDC 865408' #TrackingRef '9380_web_deposit_cif_file_0_HidemitsuUno_1328145883.trans-BCODBODIPYsq.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C34 H40 B2 F4 N4' _chemical_formula_moiety 'C34 H40 B2 F4 N4' _chemical_formula_weight 602.33 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 24.4208(5) _cell_length_b 11.8609(3) _cell_length_c 27.8392(5) _cell_angle_alpha 90.0000 _cell_angle_beta 112.7627(8) _cell_angle_gamma 90.0000 _cell_volume 7435.6(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 28016 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 68.20 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544.00 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.772 _exptl_absorpt_correction_T_max 0.939 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'VariMax 2.4 kW Ultra fine focus' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 82237 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 68.24 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.964 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 #============================================================================== # REFINEMENT DATA _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. In an asymmetric unit cell, two bis-BODIPY molecules and two solvent accessible spaces near special positions are found. In the spaces, large electron peaks due to solvent chlorobenzene are found. However, we fail to model them. Therefore, the bis-BODIPY molecules are refined without the solvent molecules by the Platon Squeeze technique. ; _reflns_number_total 13133 _reflns_number_gt 10180 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_number_restraints 1 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 13133 _refine_ls_number_parameters 810 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0679P)^2^+0.0840P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_diff_density_max 0.240 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.039 _refine_ls_extinction_method none loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 202 61 'C6 H5 Cl ' 2 0.000 0.500 0.000 511 177 '3(C6 H5 Cl) ' 3 1.000 0.000 0.500 511 177 '3(C6 H5 Cl) ' 4 0.958 0.133 0.778 7 0 ' ' 5 0.500 0.500 0.500 202 61 'C6 H5 Cl ' 6 0.958 0.367 0.278 7 0 ' ' 7 0.042 0.633 0.722 7 0 ' ' 8 0.042 0.867 0.222 7 0 ' ' _platon_squeeze_details ; ; _iucr_refine_instructions_details ; TITL 20100730 CELL 1.54187 24.42078 11.86089 27.83915 90.000 112.763 90.000 ZERR 8 0.00044 0.00022 0.00051 0.000 0.001 0.000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H B N F UNIT 272 320 16 32 32 SHEL 99999.000000 0.830022 L.S. 5 FMAP 2 PLAN -25 WPDB -2 BOND $H CONF HTAB TEMP -173.0 ACTA DELU 0.002 C64 C65 SIZE 0.240 0.220 0.100 OMIT -18 3 14 OMIT -17 0 12 OMIT -7 1 5 OMIT -15 0 20 WGHT 0.067900 0.084000 FVAR 10.47836 0.74840 0.71147 F1 5 0.383630 0.686406 0.807886 11.00000 0.06122 0.04086 = 0.04137 -0.00402 0.02999 -0.00874 F2 5 0.472835 0.785863 0.834243 11.00000 0.04400 0.04205 = 0.02904 -0.00523 0.00794 -0.00151 F3 5 0.229156 0.434484 0.461068 11.00000 0.03749 0.03477 = 0.03875 0.00184 0.01524 0.00353 F4 5 0.297261 0.473788 0.431042 11.00000 0.05606 0.03455 = 0.02695 0.00100 0.02055 -0.00058 F5 5 0.211259 -0.012400 0.575126 11.00000 0.05169 0.03497 = 0.02569 -0.00073 0.01522 -0.00232 F6 5 0.269441 -0.052061 0.535418 11.00000 0.03302 0.03779 = 0.04474 0.00598 0.01597 -0.00029 F7 5 0.117497 0.277898 0.213906 11.00000 0.08796 0.03376 = 0.06133 0.00146 0.04960 0.01013 F8 5 0.031132 0.383101 0.187953 11.00000 0.05409 0.03843 = 0.02985 0.00689 0.00420 -0.00409 N1 4 0.419660 0.722756 0.744809 11.00000 0.03486 0.03314 = 0.02617 -0.00103 0.01165 0.00110 N2 4 0.376328 0.877831 0.776631 11.00000 0.03614 0.03695 = 0.03030 -0.00773 0.01487 -0.00291 N3 4 0.332848 0.493411 0.523539 11.00000 0.03764 0.02958 = 0.02536 0.00238 0.01492 0.00497 N4 4 0.314059 0.303121 0.482080 11.00000 0.03724 0.02947 = 0.02730 -0.00081 0.01523 0.00206 N5 4 0.168918 0.037721 0.484014 11.00000 0.03420 0.02721 = 0.02439 -0.00127 0.01313 -0.00263 N6 4 0.176899 -0.163481 0.511757 11.00000 0.03406 0.02761 = 0.02587 0.00141 0.01324 0.00022 N7 4 0.082227 0.316596 0.276734 11.00000 0.03689 0.02925 = 0.02461 0.00233 0.00921 -0.00091 N8 4 0.129222 0.467492 0.246829 11.00000 0.03525 0.03372 = 0.02672 0.00359 0.01309 0.00361 C1 1 0.444886 0.623753 0.739438 11.00000 0.03003 0.03429 = 0.02826 -0.00164 0.00849 0.00066 C2 1 0.441186 0.620613 0.689878 11.00000 0.03071 0.03400 = 0.02797 -0.00341 0.01012 -0.00093 C3 1 0.414062 0.720643 0.664844 11.00000 0.03377 0.03129 = 0.02952 -0.00323 0.01451 -0.00259 C4 1 0.400449 0.784882 0.698606 11.00000 0.03195 0.03346 = 0.02586 -0.00259 0.01062 -0.00252 C5 1 0.372251 0.889912 0.692504 11.00000 0.03699 0.03074 = 0.02937 -0.00285 0.01361 -0.00173 AFIX 43 H5 2 0.361258 0.928291 0.660171 11.00000 -1.20000 AFIX 0 C6 1 0.360635 0.936620 0.730156 11.00000 0.03511 0.03250 = 0.02972 -0.00451 0.01193 -0.00075 C7 1 0.329735 1.038121 0.730416 11.00000 0.03431 0.03723 = 0.03525 -0.00757 0.01349 -0.00157 C8 1 0.325068 1.038949 0.775897 11.00000 0.03455 0.04050 = 0.04315 -0.01160 0.01741 -0.00264 C9 1 0.354925 0.939706 0.803955 11.00000 0.03817 0.04293 = 0.03526 -0.01055 0.01769 -0.00524 C10 1 0.334031 0.607620 0.530656 11.00000 0.04074 0.02926 = 0.02958 -0.00051 0.02004 0.00290 C11 1 0.379697 0.632321 0.581369 11.00000 0.03853 0.03117 = 0.03089 -0.00190 0.01956 0.00158 C12 1 0.406611 0.531403 0.606127 11.00000 0.03501 0.03437 = 0.02904 -0.00104 0.01580 0.00401 C13 1 0.377884 0.444314 0.569721 11.00000 0.03618 0.03362 = 0.02641 0.00161 0.01364 0.00460 C14 1 0.390035 0.329191 0.572022 11.00000 0.03489 0.03157 = 0.02969 0.00412 0.01484 0.00422 AFIX 43 H14 2 0.419183 0.297736 0.602627 11.00000 -1.20000 AFIX 0 C15 1 0.359554 0.260027 0.529557 11.00000 0.03487 0.03111 = 0.02977 0.00304 0.01414 0.00374 C16 1 0.366164 0.142333 0.523196 11.00000 0.03831 0.03166 = 0.03570 0.00291 0.01908 0.00345 C17 1 0.324933 0.116215 0.471846 11.00000 0.04292 0.02925 = 0.03971 -0.00173 0.02337 -0.00056 C18 1 0.293177 0.217146 0.447518 11.00000 0.03593 0.03361 = 0.03324 -0.00191 0.01918 -0.00149 C19 1 0.461550 0.543000 0.659424 11.00000 0.03479 0.03662 = 0.03091 -0.00294 0.01235 0.00290 AFIX 13 H19 2 0.476980 0.469575 0.677147 11.00000 -1.20000 AFIX 0 C20 1 0.508395 0.615114 0.649170 11.00000 0.03750 0.05185 = 0.04216 -0.00755 0.01858 -0.00113 AFIX 23 H20A 2 0.523437 0.574023 0.625814 11.00000 -1.20000 H20B 2 0.542300 0.630112 0.682396 11.00000 -1.20000 AFIX 0 C21 1 0.479403 0.729644 0.623223 11.00000 0.04748 0.04759 = 0.04342 -0.00778 0.02683 -0.00826 AFIX 23 H21A 2 0.484717 0.738704 0.589938 11.00000 -1.20000 H21B 2 0.500389 0.792606 0.646373 11.00000 -1.20000 AFIX 0 C22 1 0.409925 0.737341 0.612106 11.00000 0.04362 0.03135 = 0.03311 -0.00135 0.02020 -0.00086 AFIX 13 H22 2 0.390814 0.810016 0.595997 11.00000 -1.20000 AFIX 0 C23 1 0.471111 0.536743 0.781517 11.00000 0.04407 0.04138 = 0.03244 0.00147 0.01268 0.00533 AFIX 127 H23A 2 0.499844 0.572910 0.812754 21.00000 -1.50000 H23B 2 0.491166 0.478489 0.769349 21.00000 -1.50000 H23C 2 0.439392 0.502196 0.789838 21.00000 -1.50000 H23D 2 0.453757 0.462820 0.768540 -21.00000 -1.50000 H23E 2 0.462435 0.557241 0.811945 -21.00000 -1.50000 H23F 2 0.514209 0.533534 0.791456 -21.00000 -1.50000 AFIX 0 C24 1 0.309595 1.126699 0.688572 11.00000 0.05530 0.03750 = 0.04693 -0.00396 0.02156 0.00799 AFIX 23 H24A 2 0.280732 1.177971 0.694345 11.00000 -1.20000 H24B 2 0.290047 1.090848 0.653986 11.00000 -1.20000 AFIX 0 C25 1 0.364696 1.193447 0.690736 11.00000 0.07560 0.04612 = 0.06856 0.00771 0.04537 0.00624 AFIX 137 H25A 2 0.381658 1.234048 0.723911 11.00000 -1.50000 H25B 2 0.353124 1.247520 0.661892 11.00000 -1.50000 H25C 2 0.394320 1.141188 0.687781 11.00000 -1.50000 AFIX 0 C26 1 0.296620 1.128315 0.794696 11.00000 0.04646 0.04943 = 0.05532 -0.01424 0.02836 0.00251 AFIX 23 H26A 2 0.278253 1.094602 0.817403 11.00000 -1.20000 H26B 2 0.264663 1.163560 0.764590 11.00000 -1.20000 AFIX 0 C27 1 0.341858 1.220806 0.825724 11.00000 0.06151 0.05401 = 0.08301 -0.02782 0.04634 -0.00422 AFIX 137 H27A 2 0.372571 1.186844 0.856462 11.00000 -1.50000 H27B 2 0.321082 1.279695 0.836763 11.00000 -1.50000 H27C 2 0.360352 1.254007 0.803448 11.00000 -1.50000 AFIX 0 C28 1 0.363882 0.903613 0.855986 11.00000 0.05809 0.05720 = 0.04182 -0.00917 0.03003 -0.00281 AFIX 127 H28A 2 0.350906 0.825172 0.855064 31.00000 -1.50000 H28B 2 0.340711 0.951729 0.869748 31.00000 -1.50000 H28C 2 0.406108 0.909439 0.878466 31.00000 -1.50000 H28D 2 0.380911 0.965721 0.880455 -31.00000 -1.50000 H28E 2 0.391105 0.839164 0.865771 -31.00000 -1.50000 H28F 2 0.325709 0.881454 0.857053 -31.00000 -1.50000 AFIX 0 C29 1 0.292317 0.686681 0.488915 11.00000 0.05043 0.03003 = 0.02976 0.00155 0.01864 0.00426 AFIX 137 H29A 2 0.305297 0.691967 0.459796 11.00000 -1.50000 H29B 2 0.293240 0.761732 0.503932 11.00000 -1.50000 H29C 2 0.251756 0.656870 0.476341 11.00000 -1.50000 AFIX 0 C30 1 0.410331 0.064821 0.564700 11.00000 0.05243 0.03142 = 0.04445 0.00414 0.01928 0.00563 AFIX 23 H30A 2 0.411276 0.088126 0.599160 11.00000 -1.20000 H30B 2 0.394347 -0.012898 0.558256 11.00000 -1.20000 AFIX 0 C31 1 0.474209 0.061181 0.568155 11.00000 0.05480 0.08140 = 0.04498 0.00168 0.01576 0.02539 AFIX 137 H31A 2 0.474389 0.041095 0.534071 11.00000 -1.50000 H31B 2 0.496643 0.004726 0.593973 11.00000 -1.50000 H31C 2 0.492618 0.135385 0.578641 11.00000 -1.50000 AFIX 0 C32 1 0.313968 0.003061 0.445597 11.00000 0.05992 0.03197 = 0.04382 -0.00525 0.02405 -0.00022 AFIX 23 H32A 2 0.319679 -0.056488 0.472022 11.00000 -1.20000 H32B 2 0.272293 -0.000789 0.420247 11.00000 -1.20000 AFIX 0 C33 1 0.353317 -0.018067 0.418787 11.00000 0.08821 0.05249 = 0.05890 -0.01639 0.04002 0.00312 AFIX 137 H33A 2 0.346243 0.038254 0.391273 11.00000 -1.50000 H33B 2 0.345682 -0.093579 0.403310 11.00000 -1.50000 H33C 2 0.394648 -0.013170 0.443639 11.00000 -1.50000 AFIX 0 C34 1 0.243002 0.230153 0.393135 11.00000 0.04434 0.03791 = 0.03075 -0.00325 0.01784 0.00092 AFIX 137 H34A 2 0.204932 0.210177 0.394996 11.00000 -1.50000 H34B 2 0.250664 0.180096 0.368423 11.00000 -1.50000 H34C 2 0.241549 0.308444 0.381453 11.00000 -1.50000 AFIX 0 C35 1 0.172366 0.153032 0.484590 11.00000 0.03589 0.02726 = 0.02744 0.00049 0.01656 -0.00143 C36 1 0.126009 0.194215 0.436747 11.00000 0.03337 0.02779 = 0.02877 0.00049 0.01569 -0.00228 C37 1 0.093543 0.102773 0.406815 11.00000 0.03230 0.02908 = 0.02809 0.00227 0.01305 -0.00212 C38 1 0.120013 0.004692 0.435925 11.00000 0.03227 0.02892 = 0.02632 0.00110 0.01272 -0.00108 C39 1 0.102578 -0.107459 0.425081 11.00000 0.03532 0.03188 = 0.02515 -0.00053 0.01256 -0.00062 AFIX 43 H39 2 0.072114 -0.127236 0.392690 11.00000 -1.20000 AFIX 0 C40 1 0.130053 -0.190375 0.461982 11.00000 0.03355 0.02877 = 0.02679 -0.00102 0.01457 -0.00009 C41 1 0.114173 -0.305789 0.460821 11.00000 0.04033 0.02817 = 0.03087 -0.00050 0.01760 0.00053 C42 1 0.151050 -0.347551 0.510774 11.00000 0.04339 0.02781 = 0.03298 0.00210 0.02008 0.00184 C43 1 0.189835 -0.258410 0.541161 11.00000 0.03990 0.03061 = 0.02810 0.00444 0.01664 0.00486 C44 1 0.054278 0.219152 0.279400 11.00000 0.03612 0.02910 = 0.02824 0.00475 0.00620 0.00013 C45 1 0.058859 0.211099 0.328819 11.00000 0.02984 0.03038 = 0.03053 0.00645 0.00706 0.00026 C46 1 0.090510 0.304788 0.357617 11.00000 0.02867 0.02729 = 0.02891 0.00296 0.00893 -0.00007 C47 1 0.104607 0.372736 0.324773 11.00000 0.03059 0.03027 = 0.02555 0.00228 0.00742 0.00237 C48 1 0.136360 0.474357 0.332397 11.00000 0.03427 0.03026 = 0.02632 0.00159 0.00966 0.00031 AFIX 43 H48 2 0.149789 0.509534 0.365624 11.00000 -1.20000 AFIX 0 C49 1 0.148078 0.522420 0.294562 11.00000 0.03672 0.03158 = 0.02762 0.00219 0.01258 -0.00044 C50 1 0.181695 0.620782 0.295213 11.00000 0.03934 0.03973 = 0.03114 0.00402 0.01296 -0.00563 C51 1 0.183991 0.622984 0.248354 11.00000 0.03557 0.04289 = 0.03308 0.00780 0.01502 -0.00162 C52 1 0.151648 0.527234 0.219680 11.00000 0.03636 0.03948 = 0.02971 0.00639 0.01514 0.00383 C53 1 0.099152 0.307748 0.412523 11.00000 0.03715 0.02735 = 0.03188 0.00297 0.01555 0.00024 AFIX 13 H53 2 0.121668 0.374995 0.431901 11.00000 -1.20000 AFIX 0 C54 1 0.030764 0.305644 0.405076 11.00000 0.04339 0.03588 = 0.04611 0.00577 0.02323 0.00422 AFIX 23 H54A 2 0.028482 0.305370 0.439815 11.00000 -1.20000 H54B 2 0.011301 0.375396 0.386911 11.00000 -1.20000 AFIX 0 C55 1 -0.004351 0.200587 0.373175 11.00000 0.03405 0.04023 = 0.04950 0.01131 0.01815 0.00214 AFIX 23 H55A 2 -0.019760 0.154949 0.394986 11.00000 -1.20000 H55B 2 -0.038509 0.226324 0.342064 11.00000 -1.20000 AFIX 0 C56 1 0.037199 0.129384 0.356516 11.00000 0.03515 0.02943 = 0.03410 0.00481 0.01000 -0.00384 AFIX 13 H56 2 0.018062 0.061362 0.335502 11.00000 -1.20000 AFIX 0 C57 1 0.218047 0.216170 0.530805 11.00000 0.04573 0.03083 = 0.02736 -0.00092 0.01615 -0.00549 AFIX 137 H57A 2 0.208262 0.206779 0.561550 11.00000 -1.50000 H57B 2 0.217334 0.296487 0.522323 11.00000 -1.50000 H57C 2 0.257748 0.185607 0.538086 11.00000 -1.50000 AFIX 0 C58 1 0.066374 -0.366374 0.414254 11.00000 0.05117 0.02870 = 0.03395 0.00038 0.01350 -0.00563 AFIX 23 H58A 2 0.070508 -0.340077 0.382073 11.00000 -1.20000 H58B 2 0.075645 -0.447962 0.417621 11.00000 -1.20000 AFIX 0 C59 1 0.000862 -0.352640 0.406488 11.00000 0.05231 0.05902 = 0.04165 0.00048 0.01230 -0.01124 AFIX 137 H59A 2 -0.004886 -0.381234 0.437235 11.00000 -1.50000 H59B 2 -0.024262 -0.395248 0.375675 11.00000 -1.50000 H59C 2 -0.010012 -0.272685 0.401606 11.00000 -1.50000 AFIX 0 C60 1 0.148640 -0.464013 0.530332 11.00000 0.07634 0.03006 = 0.03555 0.00306 0.02276 -0.00446 AFIX 23 H60A 2 0.141361 -0.518919 0.501732 11.00000 -1.20000 H60B 2 0.187218 -0.482593 0.558532 11.00000 -1.20000 AFIX 0 C61 1 0.100994 -0.472433 0.550175 11.00000 0.06284 0.07519 = 0.07032 0.03542 0.02197 -0.01709 AFIX 137 H61A 2 0.110299 -0.423525 0.580690 11.00000 -1.50000 H61B 2 0.097663 -0.550646 0.560068 11.00000 -1.50000 H61C 2 0.063296 -0.448732 0.522979 11.00000 -1.50000 AFIX 0 C62 1 0.239545 -0.263104 0.596190 11.00000 0.04792 0.03573 = 0.02968 0.00536 0.01443 0.00288 AFIX 127 H62A 2 0.278248 -0.255404 0.593566 31.00000 -1.50000 H62B 2 0.237776 -0.335440 0.612541 31.00000 -1.50000 H62C 2 0.234161 -0.201446 0.617387 31.00000 -1.50000 H62D 2 0.221875 -0.272789 0.622097 -31.00000 -1.50000 H62E 2 0.262347 -0.192753 0.603122 -31.00000 -1.50000 H62F 2 0.265962 -0.326748 0.598275 -31.00000 -1.50000 AFIX 0 C63 1 0.025646 0.137152 0.235291 11.00000 0.05569 0.04131 = 0.02829 0.00015 0.00756 -0.00829 AFIX 127 H63A 2 -0.000652 0.178185 0.204432 31.00000 -1.50000 H63B 2 0.002498 0.081631 0.245573 31.00000 -1.50000 H63C 2 0.056504 0.098400 0.227228 31.00000 -1.50000 H63D 2 0.039552 0.060626 0.247057 -31.00000 -1.50000 H63E 2 0.036402 0.157180 0.205916 -31.00000 -1.50000 H63F 2 -0.017604 0.140411 0.224261 -31.00000 -1.50000 AFIX 0 C64 1 0.206854 0.706183 0.338347 11.00000 0.07596 0.05188 = 0.03560 -0.00295 0.02384 -0.02977 AFIX 23 H64A 2 0.241166 0.745165 0.335212 11.00000 -1.20000 H64B 2 0.220644 0.667961 0.372608 11.00000 -1.20000 AFIX 0 C65 1 0.158294 0.791645 0.334165 11.00000 0.10540 0.07620 = 0.10667 -0.04988 0.08393 -0.03889 AFIX 133 H65A 2 0.146587 0.832338 0.301055 11.00000 -1.50000 H65B 2 0.173418 0.845312 0.363105 11.00000 -1.50000 H65C 2 0.123771 0.752030 0.335658 11.00000 -1.50000 AFIX 0 C66 1 0.214582 0.708891 0.229593 11.00000 0.04062 0.05489 = 0.03704 0.00871 0.01825 -0.00942 AFIX 23 H66A 2 0.239759 0.671127 0.213828 11.00000 -1.20000 H66B 2 0.240769 0.754440 0.259442 11.00000 -1.20000 AFIX 0 C67 1 0.169187 0.788450 0.188271 11.00000 0.04851 0.04377 = 0.04367 0.00439 0.02344 -0.00832 AFIX 137 H67A 2 0.143500 0.743611 0.158517 11.00000 -1.50000 H67B 2 0.190814 0.844196 0.176400 11.00000 -1.50000 H67C 2 0.144859 0.827297 0.204057 11.00000 -1.50000 AFIX 0 C68 1 0.143188 0.489575 0.167783 11.00000 0.05671 0.04847 = 0.03737 0.00567 0.02584 0.00550 AFIX 127 H68A 2 0.159211 0.413225 0.169603 31.00000 -1.50000 H68B 2 0.163933 0.540800 0.152885 31.00000 -1.50000 H68C 2 0.100698 0.489224 0.145753 31.00000 -1.50000 H68D 2 0.123350 0.548941 0.142557 -31.00000 -1.50000 H68E 2 0.118628 0.421367 0.159276 -31.00000 -1.50000 H68F 2 0.181863 0.472942 0.166408 -31.00000 -1.50000 AFIX 0 B1 3 0.413837 0.765637 0.792619 11.00000 0.03655 0.03416 = 0.02872 -0.00351 0.01419 -0.00319 B2 3 0.291339 0.428236 0.472834 11.00000 0.03548 0.02984 = 0.02716 0.00224 0.01333 0.00244 B3 3 0.209069 -0.045885 0.528240 11.00000 0.03047 0.03131 = 0.02827 0.00165 0.01172 0.00053 B4 3 0.089304 0.359252 0.229593 11.00000 0.04267 0.02819 = 0.02879 0.00372 0.01571 0.00442 HKLF 4 REM 20100730 REM R1 = 0.0455 for 10180 Fo > 4sig(Fo) and 0.0547 for all 13133 data REM 810 parameters refined using 1 restraints END WGHT 0.0681 0.0000 REM Highest difference peak 0.240, deepest hole -0.233, 1-sigma level 0.039 Q1 1 0.1189 -0.5831 0.5481 11.00000 0.05 0.24 Q2 1 0.3495 0.4680 0.4469 11.00000 0.05 0.19 Q3 1 0.1583 -0.0077 0.5633 11.00000 0.05 0.18 Q4 1 0.0906 -0.5115 0.5170 11.00000 0.05 0.18 Q5 1 0.0618 0.2946 0.1913 11.00000 0.05 0.18 Q6 1 0.0714 0.1023 0.3820 11.00000 0.05 0.17 Q7 1 0.2445 1.1173 0.7776 11.00000 0.05 0.17 Q8 1 0.3828 -0.0648 0.4514 11.00000 0.05 0.17 Q9 1 0.4118 0.7581 0.7204 11.00000 0.05 0.16 Q10 1 0.1056 0.7933 0.3137 11.00000 0.05 0.16 Q11 1 0.4304 0.5219 0.6323 11.00000 0.05 0.16 Q12 1 0.1396 0.1843 0.4682 11.00000 0.05 0.16 Q13 1 0.2918 -0.2939 0.6093 11.00000 0.05 0.15 Q14 1 0.4462 0.7127 0.8340 11.00000 0.05 0.15 Q15 1 0.3369 0.9362 0.6535 11.00000 0.05 0.15 Q16 1 0.3699 0.6266 0.5531 11.00000 0.05 0.14 Q17 1 0.3585 0.4629 0.5478 11.00000 0.05 0.14 Q18 1 0.0914 0.3087 0.0522 11.00000 0.05 0.14 Q19 1 0.2709 0.2203 0.4223 11.00000 0.05 0.14 Q20 1 0.2050 0.2933 0.3780 11.00000 0.05 0.14 Q21 1 0.2013 0.6582 0.2424 11.00000 0.05 0.14 Q22 1 0.3580 -0.0357 0.4855 11.00000 0.05 0.14 Q23 1 0.2151 0.1508 0.3762 11.00000 0.05 0.14 Q24 1 0.3134 0.0302 0.3744 11.00000 0.05 0.14 Q25 1 0.1194 0.2413 0.4304 11.00000 0.05 0.14 ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.0090 0.0039 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0311 0.0180 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0727 0.0534 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 F1 F 0.38363(5) 0.68641(8) 0.80789(4) 0.0447(3) Uani 1 1 d . . . F2 F 0.47283(4) 0.78586(8) 0.83424(3) 0.0402(2) Uani 1 1 d . . . F3 F 0.22916(4) 0.43448(7) 0.46107(3) 0.0369(2) Uani 1 1 d . . . F4 F 0.29726(4) 0.47379(7) 0.43104(3) 0.0378(2) Uani 1 1 d . . . F5 F 0.21126(4) -0.01240(7) 0.57513(3) 0.0374(2) Uani 1 1 d . . . F6 F 0.26944(4) -0.05206(7) 0.53542(4) 0.0382(2) Uani 1 1 d . . . F7 F 0.11750(5) 0.27790(8) 0.21391(4) 0.0547(3) Uani 1 1 d . . . F8 F 0.03113(5) 0.38310(8) 0.18795(3) 0.0444(3) Uani 1 1 d . . . N1 N 0.41966(6) 0.72276(11) 0.74481(5) 0.0314(3) Uani 1 1 d . . . N2 N 0.37633(6) 0.87783(11) 0.77663(5) 0.0338(3) Uani 1 1 d . . . N3 N 0.33285(6) 0.49341(10) 0.52354(5) 0.0300(3) Uani 1 1 d . . . N4 N 0.31406(6) 0.30312(10) 0.48208(5) 0.0305(3) Uani 1 1 d . . . N5 N 0.16892(6) 0.03772(10) 0.48401(5) 0.0281(3) Uani 1 1 d . . . N6 N 0.17690(6) -0.16348(10) 0.51176(5) 0.0287(3) Uani 1 1 d . . . N7 N 0.08223(6) 0.31660(10) 0.27673(5) 0.0311(3) Uani 1 1 d . . . N8 N 0.12922(6) 0.46749(10) 0.24683(5) 0.0316(3) Uani 1 1 d . . . C1 C 0.44489(7) 0.62375(13) 0.73944(6) 0.0317(4) Uani 1 1 d . . . C2 C 0.44119(7) 0.62061(13) 0.68988(6) 0.0313(4) Uani 1 1 d . . . C3 C 0.41406(7) 0.72064(13) 0.66484(6) 0.0308(4) Uani 1 1 d . . . C4 C 0.40045(7) 0.78488(13) 0.69861(6) 0.0306(4) Uani 1 1 d . . . C5 C 0.37225(7) 0.88991(13) 0.69250(6) 0.0321(4) Uani 1 1 d . . . H5 H 0.3613 0.9283 0.6602 0.039 Uiso 1 1 calc R . . C6 C 0.36064(7) 0.93662(13) 0.73016(6) 0.0326(4) Uani 1 1 d . . . C7 C 0.32973(8) 1.03812(14) 0.73042(6) 0.0356(4) Uani 1 1 d . . . C8 C 0.32507(8) 1.03895(14) 0.77590(7) 0.0387(4) Uani 1 1 d . . . C9 C 0.35493(8) 0.93971(14) 0.80396(6) 0.0377(4) Uani 1 1 d . . . C10 C 0.33403(8) 0.60762(12) 0.53066(6) 0.0312(4) Uani 1 1 d . . . C11 C 0.37970(7) 0.63232(13) 0.58137(6) 0.0317(4) Uani 1 1 d . . . C12 C 0.40661(8) 0.53140(13) 0.60613(6) 0.0318(4) Uani 1 1 d . . . C13 C 0.37788(7) 0.44431(13) 0.56972(6) 0.0316(4) Uani 1 1 d . . . C14 C 0.39003(7) 0.32919(13) 0.57202(6) 0.0313(4) Uani 1 1 d . . . H14 H 0.4192 0.2977 0.6026 0.038 Uiso 1 1 calc R . . C15 C 0.35955(7) 0.26003(13) 0.52956(6) 0.0314(4) Uani 1 1 d . . . C16 C 0.36616(7) 0.14233(13) 0.52320(6) 0.0338(4) Uani 1 1 d . . . C17 C 0.32493(8) 0.11621(13) 0.47185(6) 0.0351(4) Uani 1 1 d . . . C18 C 0.29318(8) 0.21715(13) 0.44752(6) 0.0325(4) Uani 1 1 d . . . C19 C 0.46155(8) 0.54300(13) 0.65942(6) 0.0342(4) Uani 1 1 d . . . H19 H 0.4770 0.4696 0.6771 0.041 Uiso 1 1 calc R . . C20 C 0.50839(8) 0.61511(15) 0.64917(7) 0.0429(4) Uani 1 1 d . . . H20A H 0.5234 0.5740 0.6258 0.051 Uiso 1 1 calc R . . H20B H 0.5423 0.6301 0.6824 0.051 Uiso 1 1 calc R . . C21 C 0.47940(8) 0.72964(15) 0.62322(7) 0.0434(4) Uani 1 1 d . . . H21A H 0.4847 0.7387 0.5899 0.052 Uiso 1 1 calc R . . H21B H 0.5004 0.7926 0.6464 0.052 Uiso 1 1 calc R . . C22 C 0.40993(8) 0.73734(13) 0.61211(6) 0.0344(4) Uani 1 1 d . . . H22 H 0.3908 0.8100 0.5960 0.041 Uiso 1 1 calc R . . C23 C 0.47111(8) 0.53674(14) 0.78152(6) 0.0399(4) Uani 1 1 d . . . H23A H 0.4998 0.5729 0.8128 0.060 Uiso 0.748(19) 1 calc PR . . H23B H 0.4912 0.4785 0.7693 0.060 Uiso 0.748(19) 1 calc PR . . H23C H 0.4394 0.5022 0.7898 0.060 Uiso 0.748(19) 1 calc PR . . H23D H 0.4538 0.4628 0.7685 0.060 Uiso 0.252(19) 1 calc PR . . H23E H 0.4624 0.5572 0.8119 0.060 Uiso 0.252(19) 1 calc PR . . H23F H 0.5142 0.5335 0.7915 0.060 Uiso 0.252(19) 1 calc PR . . C24 C 0.30959(9) 1.12670(14) 0.68857(7) 0.0460(5) Uani 1 1 d . . . H24A H 0.2807 1.1780 0.6943 0.055 Uiso 1 1 calc R . . H24B H 0.2900 1.0908 0.6540 0.055 Uiso 1 1 calc R . . C25 C 0.36470(10) 1.19345(16) 0.69074(8) 0.0581(6) Uani 1 1 d . . . H25A H 0.3817 1.2340 0.7239 0.087 Uiso 1 1 calc R . . H25B H 0.3531 1.2475 0.6619 0.087 Uiso 1 1 calc R . . H25C H 0.3943 1.1412 0.6878 0.087 Uiso 1 1 calc R . . C26 C 0.29662(9) 1.12831(15) 0.79470(8) 0.0478(5) Uani 1 1 d . . . H26A H 0.2783 1.0946 0.8174 0.057 Uiso 1 1 calc R . . H26B H 0.2647 1.1636 0.7646 0.057 Uiso 1 1 calc R . . C27 C 0.34186(9) 1.22081(17) 0.82572(9) 0.0606(6) Uani 1 1 d . . . H27A H 0.3726 1.1868 0.8565 0.091 Uiso 1 1 calc R . . H27B H 0.3211 1.2797 0.8368 0.091 Uiso 1 1 calc R . . H27C H 0.3604 1.2540 0.8034 0.091 Uiso 1 1 calc R . . C28 C 0.36388(9) 0.90361(16) 0.85599(7) 0.0491(5) Uani 1 1 d . . . H28A H 0.3509 0.8252 0.8551 0.074 Uiso 0.711(10) 1 calc PR . . H28B H 0.3407 0.9517 0.8697 0.074 Uiso 0.711(10) 1 calc PR . . H28C H 0.4061 0.9094 0.8785 0.074 Uiso 0.711(10) 1 calc PR . . H28D H 0.3809 0.9657 0.8805 0.074 Uiso 0.289(10) 1 calc PR . . H28E H 0.3911 0.8392 0.8658 0.074 Uiso 0.289(10) 1 calc PR . . H28F H 0.3257 0.8815 0.8571 0.074 Uiso 0.289(10) 1 calc PR . . C29 C 0.29232(8) 0.68668(13) 0.48892(6) 0.0358(4) Uani 1 1 d . . . H29A H 0.3053 0.6920 0.4598 0.054 Uiso 1 1 calc R . . H29B H 0.2932 0.7617 0.5039 0.054 Uiso 1 1 calc R . . H29C H 0.2518 0.6569 0.4763 0.054 Uiso 1 1 calc R . . C30 C 0.41033(9) 0.06482(14) 0.56470(7) 0.0426(4) Uani 1 1 d . . . H30A H 0.4113 0.0881 0.5992 0.051 Uiso 1 1 calc R . . H30B H 0.3943 -0.0129 0.5583 0.051 Uiso 1 1 calc R . . C31 C 0.47421(9) 0.0612(2) 0.56816(8) 0.0615(6) Uani 1 1 d . . . H31A H 0.4744 0.0411 0.5341 0.092 Uiso 1 1 calc R . . H31B H 0.4966 0.0047 0.5940 0.092 Uiso 1 1 calc R . . H31C H 0.4926 0.1354 0.5786 0.092 Uiso 1 1 calc R . . C32 C 0.31397(9) 0.00306(14) 0.44560(7) 0.0440(5) Uani 1 1 d . . . H32A H 0.3197 -0.0565 0.4720 0.053 Uiso 1 1 calc R . . H32B H 0.2723 -0.0008 0.4202 0.053 Uiso 1 1 calc R . . C33 C 0.35332(11) -0.01807(17) 0.41879(8) 0.0630(6) Uani 1 1 d . . . H33A H 0.3462 0.0383 0.3913 0.095 Uiso 1 1 calc R . . H33B H 0.3457 -0.0936 0.4033 0.095 Uiso 1 1 calc R . . H33C H 0.3946 -0.0132 0.4436 0.095 Uiso 1 1 calc R . . C34 C 0.24300(8) 0.23015(14) 0.39314(6) 0.0367(4) Uani 1 1 d . . . H34A H 0.2049 0.2102 0.3950 0.055 Uiso 1 1 calc R . . H34B H 0.2507 0.1801 0.3684 0.055 Uiso 1 1 calc R . . H34C H 0.2415 0.3084 0.3815 0.055 Uiso 1 1 calc R . . C35 C 0.17237(7) 0.15303(12) 0.48459(6) 0.0289(3) Uani 1 1 d . . . C36 C 0.12601(7) 0.19422(12) 0.43675(6) 0.0289(3) Uani 1 1 d . . . C37 C 0.09354(7) 0.10277(12) 0.40681(6) 0.0294(3) Uani 1 1 d . . . C38 C 0.12001(7) 0.00469(13) 0.43593(6) 0.0288(3) Uani 1 1 d . . . C39 C 0.10258(7) -0.10746(12) 0.42508(6) 0.0305(4) Uani 1 1 d . . . H39 H 0.0721 -0.1272 0.3927 0.037 Uiso 1 1 calc R . . C40 C 0.13005(7) -0.19038(12) 0.46198(6) 0.0288(3) Uani 1 1 d . . . C41 C 0.11417(8) -0.30579(12) 0.46082(6) 0.0320(4) Uani 1 1 d . . . C42 C 0.15105(8) -0.34755(13) 0.51077(6) 0.0331(4) Uani 1 1 d . . . C43 C 0.18983(8) -0.25841(13) 0.54116(6) 0.0318(4) Uani 1 1 d . . . C44 C 0.05428(8) 0.21915(13) 0.27940(6) 0.0331(4) Uani 1 1 d . . . C45 C 0.05886(7) 0.21110(13) 0.32882(6) 0.0317(4) Uani 1 1 d . . . C46 C 0.09051(7) 0.30479(12) 0.35762(6) 0.0290(3) Uani 1 1 d . . . C47 C 0.10461(7) 0.37274(12) 0.32477(6) 0.0298(3) Uani 1 1 d . . . C48 C 0.13636(7) 0.47436(12) 0.33240(6) 0.0309(4) Uani 1 1 d . . . H48 H 0.1498 0.5095 0.3656 0.037 Uiso 1 1 calc R . . C49 C 0.14808(8) 0.52242(13) 0.29456(6) 0.0319(4) Uani 1 1 d . . . C50 C 0.18169(8) 0.62078(14) 0.29521(6) 0.0369(4) Uani 1 1 d . . . C51 C 0.18399(8) 0.62298(14) 0.24835(6) 0.0367(4) Uani 1 1 d . . . C52 C 0.15165(8) 0.52723(13) 0.21968(6) 0.0345(4) Uani 1 1 d . . . C53 C 0.09915(8) 0.30775(13) 0.41252(6) 0.0315(4) Uani 1 1 d . . . H53 H 0.1217 0.3750 0.4319 0.038 Uiso 1 1 calc R . . C54 C 0.03076(8) 0.30564(14) 0.40508(7) 0.0400(4) Uani 1 1 d . . . H54A H 0.0285 0.3054 0.4398 0.048 Uiso 1 1 calc R . . H54B H 0.0113 0.3754 0.3869 0.048 Uiso 1 1 calc R . . C55 C -0.00435(8) 0.20059(14) 0.37318(7) 0.0407(4) Uani 1 1 d . . . H55A H -0.0198 0.1549 0.3950 0.049 Uiso 1 1 calc R . . H55B H -0.0385 0.2263 0.3421 0.049 Uiso 1 1 calc R . . C56 C 0.03720(7) 0.12938(13) 0.35652(6) 0.0339(4) Uani 1 1 d . . . H56 H 0.0181 0.0614 0.3355 0.041 Uiso 1 1 calc R . . C57 C 0.21805(8) 0.21617(13) 0.53080(6) 0.0340(4) Uani 1 1 d . . . H57A H 0.2083 0.2068 0.5616 0.051 Uiso 1 1 calc R . . H57B H 0.2173 0.2965 0.5223 0.051 Uiso 1 1 calc R . . H57C H 0.2577 0.1856 0.5381 0.051 Uiso 1 1 calc R . . C58 C 0.06637(8) -0.36637(13) 0.41425(6) 0.0388(4) Uani 1 1 d . . . H58A H 0.0705 -0.3401 0.3821 0.047 Uiso 1 1 calc R . . H58B H 0.0756 -0.4480 0.4176 0.047 Uiso 1 1 calc R . . C59 C 0.00086(9) -0.35264(17) 0.40649(7) 0.0528(5) Uani 1 1 d . . . H59A H -0.0049 -0.3812 0.4372 0.079 Uiso 1 1 calc R . . H59B H -0.0243 -0.3952 0.3757 0.079 Uiso 1 1 calc R . . H59C H -0.0100 -0.2727 0.4016 0.079 Uiso 1 1 calc R . . C60 C 0.14864(10) -0.46401(13) 0.53033(7) 0.0470(5) Uani 1 1 d . . . H60A H 0.1414 -0.5189 0.5017 0.056 Uiso 1 1 calc R . . H60B H 0.1872 -0.4826 0.5585 0.056 Uiso 1 1 calc R . . C61 C 0.10099(10) -0.47243(19) 0.55018(9) 0.0706(7) Uani 1 1 d . . . H61A H 0.1103 -0.4235 0.5807 0.106 Uiso 1 1 calc R . . H61B H 0.0977 -0.5506 0.5601 0.106 Uiso 1 1 calc R . . H61C H 0.0633 -0.4487 0.5230 0.106 Uiso 1 1 calc R . . C62 C 0.23955(8) -0.26310(14) 0.59619(6) 0.0379(4) Uani 1 1 d . . . H62A H 0.2782 -0.2554 0.5936 0.057 Uiso 0.711(10) 1 calc PR . . H62B H 0.2378 -0.3354 0.6125 0.057 Uiso 0.711(10) 1 calc PR . . H62C H 0.2342 -0.2014 0.6174 0.057 Uiso 0.711(10) 1 calc PR . . H62D H 0.2219 -0.2728 0.6221 0.057 Uiso 0.289(10) 1 calc PR . . H62E H 0.2623 -0.1928 0.6031 0.057 Uiso 0.289(10) 1 calc PR . . H62F H 0.2660 -0.3267 0.5983 0.057 Uiso 0.289(10) 1 calc PR . . C63 C 0.02565(9) 0.13715(14) 0.23529(6) 0.0444(5) Uani 1 1 d . . . H63A H -0.0007 0.1782 0.2044 0.067 Uiso 0.711(10) 1 calc PR . . H63B H 0.0025 0.0816 0.2456 0.067 Uiso 0.711(10) 1 calc PR . . H63C H 0.0565 0.0984 0.2272 0.067 Uiso 0.711(10) 1 calc PR . . H63D H 0.0396 0.0606 0.2471 0.067 Uiso 0.289(10) 1 calc PR . . H63E H 0.0364 0.1572 0.2059 0.067 Uiso 0.289(10) 1 calc PR . . H63F H -0.0176 0.1404 0.2243 0.067 Uiso 0.289(10) 1 calc PR . . C64 C 0.20685(10) 0.70618(16) 0.33835(7) 0.0538(5) Uani 1 1 d U . . H64A H 0.2412 0.7452 0.3352 0.065 Uiso 1 1 calc R . . H64B H 0.2206 0.6680 0.3726 0.065 Uiso 1 1 calc R . . C65 C 0.15829(11) 0.7916(2) 0.33417(10) 0.0831(8) Uani 1 1 d U . . H65A H 0.1466 0.8323 0.3011 0.125 Uiso 1 1 calc R . . H65B H 0.1734 0.8453 0.3631 0.125 Uiso 1 1 calc R . . H65C H 0.1238 0.7520 0.3357 0.125 Uiso 1 1 calc R . . C66 C 0.21458(8) 0.70889(15) 0.22959(7) 0.0432(4) Uani 1 1 d . . . H66A H 0.2398 0.6711 0.2138 0.052 Uiso 1 1 calc R . . H66B H 0.2408 0.7544 0.2594 0.052 Uiso 1 1 calc R . . C67 C 0.16919(8) 0.78845(15) 0.18827(7) 0.0436(4) Uani 1 1 d . . . H67A H 0.1435 0.7436 0.1585 0.065 Uiso 1 1 calc R . . H67B H 0.1908 0.8442 0.1764 0.065 Uiso 1 1 calc R . . H67C H 0.1449 0.8273 0.2041 0.065 Uiso 1 1 calc R . . C68 C 0.14319(9) 0.48958(15) 0.16778(7) 0.0452(5) Uani 1 1 d . . . H68A H 0.1592 0.4132 0.1696 0.068 Uiso 0.711(10) 1 calc PR . . H68B H 0.1639 0.5408 0.1529 0.068 Uiso 0.711(10) 1 calc PR . . H68C H 0.1007 0.4892 0.1458 0.068 Uiso 0.711(10) 1 calc PR . . H68D H 0.1233 0.5489 0.1426 0.068 Uiso 0.289(10) 1 calc PR . . H68E H 0.1186 0.4214 0.1593 0.068 Uiso 0.289(10) 1 calc PR . . H68F H 0.1819 0.4729 0.1664 0.068 Uiso 0.289(10) 1 calc PR . . B1 B 0.41384(9) 0.76564(15) 0.79262(7) 0.0327(4) Uani 1 1 d . . . B2 B 0.29134(9) 0.42824(15) 0.47283(7) 0.0305(4) Uani 1 1 d . . . B3 B 0.20907(9) -0.04588(15) 0.52824(7) 0.0299(4) Uani 1 1 d . . . B4 B 0.08930(9) 0.35925(15) 0.22959(7) 0.0326(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 F(1) 0.0612(7) 0.0409(6) 0.0414(6) -0.0087(5) 0.0300(6) -0.0040(5) F(2) 0.0440(6) 0.0420(6) 0.0290(5) -0.0015(5) 0.0079(5) -0.0052(4) F(3) 0.0375(6) 0.0348(5) 0.0388(6) 0.0035(5) 0.0152(5) 0.0018(4) F(4) 0.0561(7) 0.0345(5) 0.0270(5) -0.0006(5) 0.0205(5) 0.0010(4) F(5) 0.0517(7) 0.0350(5) 0.0257(5) -0.0023(5) 0.0152(5) -0.0007(4) F(6) 0.0330(6) 0.0378(5) 0.0447(6) -0.0003(5) 0.0160(5) 0.0060(4) F(7) 0.0880(9) 0.0338(6) 0.0613(7) 0.0101(6) 0.0496(7) 0.0015(5) F(8) 0.0541(7) 0.0384(6) 0.0299(5) -0.0041(5) 0.0042(5) 0.0069(4) N(1) 0.0349(8) 0.0331(7) 0.0262(7) 0.0011(6) 0.0117(7) -0.0010(6) N(2) 0.0361(8) 0.0369(8) 0.0303(7) -0.0029(7) 0.0149(7) -0.0077(6) N(3) 0.0376(8) 0.0296(7) 0.0254(7) 0.0050(6) 0.0149(7) 0.0024(6) N(4) 0.0372(8) 0.0295(7) 0.0273(7) 0.0021(6) 0.0152(7) -0.0008(6) N(5) 0.0342(8) 0.0272(7) 0.0244(7) -0.0026(6) 0.0131(6) -0.0013(5) N(6) 0.0341(8) 0.0276(7) 0.0259(7) 0.0002(6) 0.0132(6) 0.0014(6) N(7) 0.0369(8) 0.0293(7) 0.0246(7) -0.0009(6) 0.0092(7) 0.0023(6) N(8) 0.0352(8) 0.0337(7) 0.0267(7) 0.0036(6) 0.0131(7) 0.0036(6) C(1) 0.0300(9) 0.0343(9) 0.0283(8) 0.0007(8) 0.0085(8) -0.0016(7) C(2) 0.0307(9) 0.0340(9) 0.0280(8) -0.0009(7) 0.0101(8) -0.0034(7) C(3) 0.0338(10) 0.0313(8) 0.0295(9) -0.0026(7) 0.0145(8) -0.0032(7) C(4) 0.0319(10) 0.0335(8) 0.0259(8) -0.0025(7) 0.0106(8) -0.0026(7) C(5) 0.0370(10) 0.0307(8) 0.0294(9) -0.0017(8) 0.0136(8) -0.0029(7) C(6) 0.0351(10) 0.0325(9) 0.0297(9) -0.0008(8) 0.0119(8) -0.0045(7) C(7) 0.0343(10) 0.0372(9) 0.0352(9) -0.0016(8) 0.0135(8) -0.0076(7) C(8) 0.0345(10) 0.0405(10) 0.0432(10) -0.0026(8) 0.0174(9) -0.0116(8) C(9) 0.0382(11) 0.0429(10) 0.0353(9) -0.0052(8) 0.0177(9) -0.0106(8) C(10) 0.0407(10) 0.0293(8) 0.0296(9) 0.0029(8) 0.0200(8) -0.0005(7) C(11) 0.0385(10) 0.0312(8) 0.0309(9) 0.0016(8) 0.0196(8) -0.0019(7) C(12) 0.0350(10) 0.0344(9) 0.0290(9) 0.0040(8) 0.0158(8) -0.0010(7) C(13) 0.0362(10) 0.0336(9) 0.0264(8) 0.0046(8) 0.0136(8) 0.0016(7) C(14) 0.0349(10) 0.0316(8) 0.0297(9) 0.0042(8) 0.0148(8) 0.0041(7) C(15) 0.0349(10) 0.0311(8) 0.0298(9) 0.0037(8) 0.0141(8) 0.0030(7) C(16) 0.0383(10) 0.0317(8) 0.0357(9) 0.0034(8) 0.0191(8) 0.0029(7) C(17) 0.0429(11) 0.0293(8) 0.0397(10) -0.0006(8) 0.0234(9) -0.0017(7) C(18) 0.0359(10) 0.0336(8) 0.0332(9) -0.0015(8) 0.0192(8) -0.0019(7) C(19) 0.0348(10) 0.0366(9) 0.0309(9) 0.0029(8) 0.0124(8) -0.0029(7) C(20) 0.0375(11) 0.0519(11) 0.0422(11) -0.0011(9) 0.0186(9) -0.0076(9) C(21) 0.0475(12) 0.0476(10) 0.0434(11) -0.0083(9) 0.0268(10) -0.0078(9) C(22) 0.0436(11) 0.0314(8) 0.0331(9) -0.0009(8) 0.0202(9) -0.0014(7) C(23) 0.0441(11) 0.0414(10) 0.0324(9) 0.0053(9) 0.0127(9) 0.0015(8) C(24) 0.0553(13) 0.0375(10) 0.0469(11) 0.0080(9) 0.0216(10) -0.0040(8) C(25) 0.0756(16) 0.0461(11) 0.0686(14) 0.0062(11) 0.0454(13) 0.0077(10) C(26) 0.0465(12) 0.0494(11) 0.0553(12) 0.0025(9) 0.0284(10) -0.0142(9) C(27) 0.0615(14) 0.0540(12) 0.0830(16) -0.0042(11) 0.0463(13) -0.0278(11) C(28) 0.0581(13) 0.0572(12) 0.0418(11) -0.0028(10) 0.0300(10) -0.0092(9) C(29) 0.0504(12) 0.0300(8) 0.0298(9) 0.0043(8) 0.0186(9) 0.0015(7) C(30) 0.0524(12) 0.0314(9) 0.0445(11) 0.0056(9) 0.0193(10) 0.0041(8) C(31) 0.0548(14) 0.0814(16) 0.0450(12) 0.0254(12) 0.0158(11) 0.0017(11) C(32) 0.0599(13) 0.0320(9) 0.0438(11) -0.0002(9) 0.0240(10) -0.0053(8) C(33) 0.0882(18) 0.0525(12) 0.0589(13) 0.0031(12) 0.0400(13) -0.0164(10) C(34) 0.0443(11) 0.0379(9) 0.0308(9) 0.0009(8) 0.0178(9) -0.0032(7) C(35) 0.0359(10) 0.0273(8) 0.0274(8) -0.0014(7) 0.0166(8) 0.0005(6) C(36) 0.0334(10) 0.0278(8) 0.0288(8) -0.0023(7) 0.0157(8) 0.0005(7) C(37) 0.0323(9) 0.0291(8) 0.0281(8) -0.0021(7) 0.0131(8) 0.0023(7) C(38) 0.0323(9) 0.0289(8) 0.0263(8) -0.0011(7) 0.0127(8) 0.0011(7) C(39) 0.0353(10) 0.0319(8) 0.0251(8) -0.0006(7) 0.0126(8) -0.0005(7) C(40) 0.0336(10) 0.0288(8) 0.0268(8) -0.0001(7) 0.0146(8) -0.0010(7) C(41) 0.0403(10) 0.0282(8) 0.0309(9) 0.0005(8) 0.0176(8) -0.0005(7) C(42) 0.0434(11) 0.0278(8) 0.0330(9) 0.0018(8) 0.0201(8) 0.0021(7) C(43) 0.0399(10) 0.0306(8) 0.0281(8) 0.0049(8) 0.0166(8) 0.0044(7) C(44) 0.0361(10) 0.0291(8) 0.0282(9) 0.0001(8) 0.0062(8) 0.0047(7) C(45) 0.0298(10) 0.0304(8) 0.0305(9) 0.0003(7) 0.0071(8) 0.0065(7) C(46) 0.0287(9) 0.0273(8) 0.0289(9) -0.0001(7) 0.0089(8) 0.0030(7) C(47) 0.0306(9) 0.0303(8) 0.0256(8) 0.0024(7) 0.0074(8) 0.0023(7) C(48) 0.0343(10) 0.0303(8) 0.0263(8) 0.0003(7) 0.0097(8) 0.0016(7) C(49) 0.0367(10) 0.0316(8) 0.0276(8) -0.0004(8) 0.0126(8) 0.0022(7) C(50) 0.0393(11) 0.0397(9) 0.0311(9) -0.0056(8) 0.0130(8) 0.0040(7) C(51) 0.0356(10) 0.0429(10) 0.0331(9) -0.0016(8) 0.0150(8) 0.0078(8) C(52) 0.0364(10) 0.0395(9) 0.0297(9) 0.0038(8) 0.0151(8) 0.0064(7) C(53) 0.0372(10) 0.0273(8) 0.0319(9) 0.0002(7) 0.0156(8) 0.0030(7) C(54) 0.0434(11) 0.0359(9) 0.0461(11) 0.0042(8) 0.0232(10) 0.0058(8) C(55) 0.0340(11) 0.0402(10) 0.0495(11) 0.0021(8) 0.0181(9) 0.0113(8) C(56) 0.0352(10) 0.0294(8) 0.0341(9) -0.0038(8) 0.0100(8) 0.0048(7) C(57) 0.0457(11) 0.0308(8) 0.0274(9) -0.0055(8) 0.0162(8) -0.0009(7) C(58) 0.0512(12) 0.0287(9) 0.0340(9) -0.0056(8) 0.0135(9) 0.0004(7) C(59) 0.0523(13) 0.0590(12) 0.0417(11) -0.0112(11) 0.0123(10) 0.0005(9) C(60) 0.0763(15) 0.0301(9) 0.0355(10) -0.0045(9) 0.0228(10) 0.0031(8) C(61) 0.0628(15) 0.0752(15) 0.0703(15) -0.0171(13) 0.0220(13) 0.0354(12) C(62) 0.0479(12) 0.0357(9) 0.0297(9) 0.0029(8) 0.0144(9) 0.0054(7) C(63) 0.0557(13) 0.0413(10) 0.0283(9) -0.0083(9) 0.0076(9) 0.0001(8) C(64) 0.0760(15) 0.0519(11) 0.0356(10) -0.0298(10) 0.0238(11) -0.0029(9) C(65) 0.105(2) 0.0762(15) 0.107(2) -0.0389(13) 0.0839(18) -0.0499(14) C(66) 0.0406(11) 0.0549(11) 0.0370(10) -0.0094(9) 0.0182(9) 0.0087(8) C(67) 0.0485(12) 0.0438(10) 0.0437(11) -0.0083(9) 0.0234(10) 0.0044(8) C(68) 0.0567(13) 0.0485(11) 0.0374(10) 0.0055(10) 0.0258(10) 0.0057(8) B(1) 0.0365(12) 0.0342(10) 0.0287(10) -0.0032(9) 0.0142(9) -0.0035(8) B(2) 0.0355(11) 0.0298(9) 0.0272(10) 0.0024(8) 0.0133(9) 0.0022(8) B(3) 0.0305(11) 0.0313(9) 0.0283(10) 0.0005(8) 0.0117(9) 0.0017(8) B(4) 0.0427(12) 0.0282(9) 0.0288(10) 0.0044(9) 0.0157(9) 0.0037(8) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 F(1) B(1) 1.360(3) yes . . F(2) B(1) 1.4777(19) yes . . F(3) B(2) 1.426(3) yes . . F(4) B(2) 1.340(3) yes . . F(5) B(3) 1.346(3) yes . . F(6) B(3) 1.411(3) yes . . F(7) B(4) 1.352(3) yes . . F(8) B(4) 1.472(2) yes . . N(1) C(1) 1.361(3) yes . . N(1) C(4) 1.397(2) yes . . N(1) B(1) 1.482(3) yes . . N(2) C(6) 1.387(2) yes . . N(2) C(9) 1.303(3) yes . . N(2) B(1) 1.579(3) yes . . N(3) C(10) 1.3677(19) yes . . N(3) C(13) 1.4516(18) yes . . N(3) B(2) 1.585(2) yes . . N(4) C(15) 1.4513(18) yes . . N(4) C(18) 1.359(2) yes . . N(4) B(2) 1.570(3) yes . . N(5) C(35) 1.3700(19) yes . . N(5) C(38) 1.4610(18) yes . . N(5) B(3) 1.589(2) yes . . N(6) C(40) 1.4506(18) yes . . N(6) C(43) 1.356(2) yes . . N(6) B(3) 1.579(3) yes . . N(7) C(44) 1.359(3) yes . . N(7) C(47) 1.402(2) yes . . N(7) B(4) 1.478(3) yes . . N(8) C(49) 1.389(2) yes . . N(8) C(52) 1.301(3) yes . . N(8) B(4) 1.571(3) yes . . C(1) C(2) 1.348(3) yes . . C(1) C(23) 1.506(3) yes . . C(2) C(3) 1.405(2) yes . . C(2) C(19) 1.463(3) yes . . C(3) C(4) 1.348(3) yes . . C(3) C(22) 1.446(3) yes . . C(4) C(5) 1.402(3) yes . . C(5) C(6) 1.310(3) yes . . C(6) C(7) 1.422(3) yes . . C(7) C(8) 1.314(3) yes . . C(7) C(24) 1.503(3) yes . . C(8) C(9) 1.445(3) yes . . C(8) C(26) 1.470(3) yes . . C(9) C(28) 1.444(3) yes . . C(10) C(11) 1.451(2) yes . . C(10) C(29) 1.533(2) yes . . C(11) C(12) 1.410(3) yes . . C(11) C(22) 1.530(2) yes . . C(12) C(13) 1.427(2) yes . . C(12) C(19) 1.575(2) yes . . C(13) C(14) 1.393(3) yes . . C(14) C(15) 1.394(2) yes . . C(15) C(16) 1.424(3) yes . . C(16) C(17) 1.428(2) yes . . C(16) C(30) 1.542(3) yes . . C(17) C(18) 1.445(3) yes . . C(17) C(32) 1.502(3) yes . . C(18) C(34) 1.543(2) yes . . C(19) C(20) 1.541(3) yes . . C(20) C(21) 1.572(3) yes . . C(21) C(22) 1.605(3) yes . . C(24) C(25) 1.542(4) yes . . C(26) C(27) 1.559(3) yes . . C(30) C(31) 1.526(4) yes . . C(32) C(33) 1.449(4) yes . . C(35) C(36) 1.4586(19) yes . . C(35) C(57) 1.533(2) yes . . C(36) C(37) 1.410(2) yes . . C(36) C(53) 1.535(2) yes . . C(37) C(38) 1.422(2) yes . . C(37) C(56) 1.5691(19) yes . . C(38) C(39) 1.394(2) yes . . C(39) C(40) 1.393(2) yes . . C(40) C(41) 1.420(2) yes . . C(41) C(42) 1.422(2) yes . . C(41) C(58) 1.546(2) yes . . C(42) C(43) 1.453(3) yes . . C(42) C(60) 1.494(3) yes . . C(43) C(62) 1.544(2) yes . . C(44) C(45) 1.340(3) yes . . C(44) C(63) 1.509(3) yes . . C(45) C(46) 1.413(2) yes . . C(45) C(56) 1.459(3) yes . . C(46) C(47) 1.359(3) yes . . C(46) C(53) 1.460(3) yes . . C(47) C(48) 1.404(2) yes . . C(48) C(49) 1.323(3) yes . . C(49) C(50) 1.423(3) yes . . C(50) C(51) 1.328(3) yes . . C(50) C(64) 1.508(3) yes . . C(51) C(52) 1.436(3) yes . . C(51) C(66) 1.473(3) yes . . C(52) C(68) 1.449(3) yes . . C(53) C(54) 1.602(3) yes . . C(54) C(55) 1.577(3) yes . . C(55) C(56) 1.524(3) yes . . C(58) C(59) 1.538(3) yes . . C(60) C(61) 1.472(4) yes . . C(64) C(65) 1.530(4) yes . . C(66) C(67) 1.567(3) yes . . C(5) H(5) 0.950 no . . C(14) H(14) 0.950 no . . C(19) H(19) 1.000 no . . C(20) H(20A) 0.990 no . . C(20) H(20B) 0.990 no . . C(21) H(21A) 0.990 no . . C(21) H(21B) 0.990 no . . C(22) H(22) 1.000 no . . C(23) H(23A) 0.980 no . . C(23) H(23B) 0.980 no . . C(23) H(23C) 0.980 no . . C(23) H(23D) 0.980 no . . C(23) H(23E) 0.980 no . . C(23) H(23F) 0.980 no . . C(24) H(24A) 0.990 no . . C(24) H(24B) 0.990 no . . C(25) H(25A) 0.980 no . . C(25) H(25B) 0.980 no . . C(25) H(25C) 0.980 no . . C(26) H(26A) 0.990 no . . C(26) H(26B) 0.990 no . . C(27) H(27A) 0.980 no . . C(27) H(27B) 0.980 no . . C(27) H(27C) 0.980 no . . C(28) H(28A) 0.980 no . . C(28) H(28B) 0.980 no . . C(28) H(28C) 0.980 no . . C(28) H(28D) 0.980 no . . C(28) H(28E) 0.980 no . . C(28) H(28F) 0.980 no . . C(29) H(29A) 0.980 no . . C(29) H(29B) 0.980 no . . C(29) H(29C) 0.980 no . . C(30) H(30A) 0.990 no . . C(30) H(30B) 0.990 no . . C(31) H(31A) 0.980 no . . C(31) H(31B) 0.980 no . . C(31) H(31C) 0.980 no . . C(32) H(32A) 0.990 no . . C(32) H(32B) 0.990 no . . C(33) H(33A) 0.980 no . . C(33) H(33B) 0.980 no . . C(33) H(33C) 0.980 no . . C(34) H(34A) 0.980 no . . C(34) H(34B) 0.980 no . . C(34) H(34C) 0.980 no . . C(39) H(39) 0.950 no . . C(48) H(48) 0.950 no . . C(53) H(53) 1.000 no . . C(54) H(54A) 0.990 no . . C(54) H(54B) 0.990 no . . C(55) H(55A) 0.990 no . . C(55) H(55B) 0.990 no . . C(56) H(56) 1.000 no . . C(57) H(57A) 0.980 no . . C(57) H(57B) 0.980 no . . C(57) H(57C) 0.980 no . . C(58) H(58A) 0.990 no . . C(58) H(58B) 0.990 no . . C(59) H(59A) 0.980 no . . C(59) H(59B) 0.980 no . . C(59) H(59C) 0.980 no . . C(60) H(60A) 0.990 no . . C(60) H(60B) 0.990 no . . C(61) H(61A) 0.980 no . . C(61) H(61B) 0.980 no . . C(61) H(61C) 0.980 no . . C(62) H(62A) 0.980 no . . C(62) H(62B) 0.980 no . . C(62) H(62C) 0.980 no . . C(62) H(62D) 0.980 no . . C(62) H(62E) 0.980 no . . C(62) H(62F) 0.980 no . . C(63) H(63A) 0.980 no . . C(63) H(63B) 0.980 no . . C(63) H(63C) 0.980 no . . C(63) H(63D) 0.980 no . . C(63) H(63E) 0.980 no . . C(63) H(63F) 0.980 no . . C(64) H(64A) 0.990 no . . C(64) H(64B) 0.990 no . . C(65) H(65A) 0.980 no . . C(65) H(65B) 0.980 no . . C(65) H(65C) 0.980 no . . C(66) H(66A) 0.990 no . . C(66) H(66B) 0.990 no . . C(67) H(67A) 0.980 no . . C(67) H(67B) 0.980 no . . C(67) H(67C) 0.980 no . . C(68) H(68A) 0.980 no . . C(68) H(68B) 0.980 no . . C(68) H(68C) 0.980 no . . C(68) H(68D) 0.980 no . . C(68) H(68E) 0.980 no . . C(68) H(68F) 0.980 no . . H(23A) H(23E) 0.924 no . . H(23A) H(23F) 0.924 no . . H(23B) H(23D) 0.924 no . . H(23B) H(23F) 0.924 no . . H(23C) H(23D) 0.924 no . . H(23C) H(23E) 0.924 no . . H(28A) H(28E) 0.924 no . . H(28A) H(28F) 0.924 no . . H(28B) H(28D) 0.924 no . . H(28B) H(28F) 0.924 no . . H(28C) H(28D) 0.924 no . . H(28C) H(28E) 0.924 no . . H(62A) H(62E) 0.924 no . . H(62A) H(62F) 0.924 no . . H(62B) H(62D) 0.924 no . . H(62B) H(62F) 0.924 no . . H(62C) H(62D) 0.924 no . . H(62C) H(62E) 0.924 no . . H(63A) H(63E) 0.924 no . . H(63A) H(63F) 0.924 no . . H(63B) H(63D) 0.924 no . . H(63B) H(63F) 0.924 no . . H(63C) H(63D) 0.924 no . . H(63C) H(63E) 0.924 no . . H(68A) H(68E) 0.924 no . . H(68A) H(68F) 0.924 no . . H(68B) H(68D) 0.924 no . . H(68B) H(68F) 0.924 no . . H(68C) H(68D) 0.924 no . . H(68C) H(68E) 0.924 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(1) N(1) C(4) 111.05(15) yes . . . C(1) N(1) B(1) 126.83(14) yes . . . C(4) N(1) B(1) 122.09(14) yes . . . C(6) N(2) C(9) 103.47(14) yes . . . C(6) N(2) B(1) 127.42(16) yes . . . C(9) N(2) B(1) 129.06(15) yes . . . C(10) N(3) C(13) 107.62(12) yes . . . C(10) N(3) B(2) 125.63(12) yes . . . C(13) N(3) B(2) 126.70(12) yes . . . C(15) N(4) C(18) 109.02(12) yes . . . C(15) N(4) B(2) 125.42(12) yes . . . C(18) N(4) B(2) 125.53(12) yes . . . C(35) N(5) C(38) 107.65(11) yes . . . C(35) N(5) B(3) 126.65(12) yes . . . C(38) N(5) B(3) 125.66(12) yes . . . C(40) N(6) C(43) 107.91(12) yes . . . C(40) N(6) B(3) 126.27(12) yes . . . C(43) N(6) B(3) 125.78(12) yes . . . C(44) N(7) C(47) 111.75(15) yes . . . C(44) N(7) B(4) 125.00(14) yes . . . C(47) N(7) B(4) 123.25(14) yes . . . C(49) N(8) C(52) 104.00(13) yes . . . C(49) N(8) B(4) 127.79(16) yes . . . C(52) N(8) B(4) 128.21(15) yes . . . N(1) C(1) C(2) 106.40(14) yes . . . N(1) C(1) C(23) 125.47(16) yes . . . C(2) C(1) C(23) 128.13(16) yes . . . C(1) C(2) C(3) 108.45(16) yes . . . C(1) C(2) C(19) 135.04(15) yes . . . C(3) C(2) C(19) 116.39(16) yes . . . C(2) C(3) C(4) 109.11(15) yes . . . C(2) C(3) C(22) 116.98(16) yes . . . C(4) C(3) C(22) 133.76(15) yes . . . N(1) C(4) C(3) 104.98(14) yes . . . N(1) C(4) C(5) 123.70(17) yes . . . C(3) C(4) C(5) 131.30(16) yes . . . C(4) C(5) C(6) 121.81(16) yes . . . N(2) C(6) C(5) 117.82(15) yes . . . N(2) C(6) C(7) 112.11(16) yes . . . C(5) C(6) C(7) 129.91(15) yes . . . C(6) C(7) C(8) 104.78(15) yes . . . C(6) C(7) C(24) 127.06(18) yes . . . C(8) C(7) C(24) 128.10(18) yes . . . C(7) C(8) C(9) 107.52(18) yes . . . C(7) C(8) C(26) 125.26(17) yes . . . C(9) C(8) C(26) 127.17(19) yes . . . N(2) C(9) C(8) 112.07(16) yes . . . N(2) C(9) C(28) 118.65(16) yes . . . C(8) C(9) C(28) 129.27(19) yes . . . N(3) C(10) C(11) 107.83(12) yes . . . N(3) C(10) C(29) 121.69(13) yes . . . C(11) C(10) C(29) 130.48(13) yes . . . C(10) C(11) C(12) 109.98(13) yes . . . C(10) C(11) C(22) 137.04(14) yes . . . C(12) C(11) C(22) 112.64(12) yes . . . C(11) C(12) C(13) 105.02(12) yes . . . C(11) C(12) C(19) 116.89(13) yes . . . C(13) C(12) C(19) 137.56(14) yes . . . N(3) C(13) C(12) 109.54(13) yes . . . N(3) C(13) C(14) 120.58(13) yes . . . C(12) C(13) C(14) 129.73(13) yes . . . C(13) C(14) C(15) 120.22(13) yes . . . N(4) C(15) C(14) 122.31(14) yes . . . N(4) C(15) C(16) 108.40(12) yes . . . C(14) C(15) C(16) 129.29(13) yes . . . C(15) C(16) C(17) 105.50(13) yes . . . C(15) C(16) C(30) 124.83(13) yes . . . C(17) C(16) C(30) 129.67(14) yes . . . C(16) C(17) C(18) 109.40(14) yes . . . C(16) C(17) C(32) 127.22(14) yes . . . C(18) C(17) C(32) 123.38(13) yes . . . N(4) C(18) C(17) 107.68(12) yes . . . N(4) C(18) C(34) 123.90(14) yes . . . C(17) C(18) C(34) 128.40(14) yes . . . C(2) C(19) C(12) 104.14(14) yes . . . C(2) C(19) C(20) 101.61(14) yes . . . C(12) C(19) C(20) 107.28(14) yes . . . C(19) C(20) C(21) 109.27(15) yes . . . C(20) C(21) C(22) 113.09(16) yes . . . C(3) C(22) C(11) 106.59(15) yes . . . C(3) C(22) C(21) 98.24(13) yes . . . C(11) C(22) C(21) 107.87(15) yes . . . C(7) C(24) C(25) 108.03(15) yes . . . C(8) C(26) C(27) 111.91(18) yes . . . C(16) C(30) C(31) 117.76(18) yes . . . C(17) C(32) C(33) 112.12(18) yes . . . N(5) C(35) C(36) 107.53(12) yes . . . N(5) C(35) C(57) 121.27(12) yes . . . C(36) C(35) C(57) 131.18(13) yes . . . C(35) C(36) C(37) 110.02(13) yes . . . C(35) C(36) C(53) 138.06(13) yes . . . C(37) C(36) C(53) 111.60(12) yes . . . C(36) C(37) C(38) 105.34(12) yes . . . C(36) C(37) C(56) 118.10(13) yes . . . C(38) C(37) C(56) 136.16(13) yes . . . N(5) C(38) C(37) 109.45(13) yes . . . N(5) C(38) C(39) 121.83(13) yes . . . C(37) C(38) C(39) 128.59(13) yes . . . C(38) C(39) C(40) 119.65(13) yes . . . N(6) C(40) C(39) 121.75(13) yes . . . N(6) C(40) C(41) 109.96(12) yes . . . C(39) C(40) C(41) 127.94(13) yes . . . C(40) C(41) C(42) 104.45(13) yes . . . C(40) C(41) C(58) 125.34(13) yes . . . C(42) C(41) C(58) 130.21(14) yes . . . C(41) C(42) C(43) 109.85(14) yes . . . C(41) C(42) C(60) 125.39(14) yes . . . C(43) C(42) C(60) 124.70(13) yes . . . N(6) C(43) C(42) 107.81(12) yes . . . N(6) C(43) C(62) 122.61(14) yes . . . C(42) C(43) C(62) 129.54(14) yes . . . N(7) C(44) C(45) 105.82(14) yes . . . N(7) C(44) C(63) 126.01(17) yes . . . C(45) C(44) C(63) 128.16(17) yes . . . C(44) C(45) C(46) 109.67(16) yes . . . C(44) C(45) C(56) 133.36(15) yes . . . C(46) C(45) C(56) 116.95(15) yes . . . C(45) C(46) C(47) 108.05(15) yes . . . C(45) C(46) C(53) 116.02(16) yes . . . C(47) C(46) C(53) 135.91(14) yes . . . N(7) C(47) C(46) 104.68(13) yes . . . N(7) C(47) C(48) 122.73(16) yes . . . C(46) C(47) C(48) 132.52(15) yes . . . C(47) C(48) C(49) 121.76(15) yes . . . N(8) C(49) C(48) 117.77(15) yes . . . N(8) C(49) C(50) 111.90(16) yes . . . C(48) C(49) C(50) 130.15(15) yes . . . C(49) C(50) C(51) 104.31(15) yes . . . C(49) C(50) C(64) 128.04(18) yes . . . C(51) C(50) C(64) 127.60(18) yes . . . C(50) C(51) C(52) 107.90(17) yes . . . C(50) C(51) C(66) 125.59(16) yes . . . C(52) C(51) C(66) 126.52(17) yes . . . N(8) C(52) C(51) 111.86(16) yes . . . N(8) C(52) C(68) 118.80(15) yes . . . C(51) C(52) C(68) 129.31(18) yes . . . C(36) C(53) C(46) 107.64(14) yes . . . C(36) C(53) C(54) 106.86(15) yes . . . C(46) C(53) C(54) 98.23(13) yes . . . C(53) C(54) C(55) 113.43(16) yes . . . C(54) C(55) C(56) 109.17(15) yes . . . C(37) C(56) C(45) 103.48(13) yes . . . C(37) C(56) C(55) 107.29(14) yes . . . C(45) C(56) C(55) 102.29(14) yes . . . C(41) C(58) C(59) 118.40(16) yes . . . C(42) C(60) C(61) 110.35(18) yes . . . C(50) C(64) C(65) 108.63(16) yes . . . C(51) C(66) C(67) 111.41(16) yes . . . F(1) B(1) F(2) 110.43(13) yes . . . F(1) B(1) N(1) 107.19(14) yes . . . F(1) B(1) N(2) 110.16(17) yes . . . F(2) B(1) N(1) 110.90(17) yes . . . F(2) B(1) N(2) 111.56(13) yes . . . N(1) B(1) N(2) 106.43(13) yes . . . F(3) B(2) F(4) 104.05(12) yes . . . F(3) B(2) N(3) 115.88(16) yes . . . F(3) B(2) N(4) 111.34(14) yes . . . F(4) B(2) N(3) 109.27(15) yes . . . F(4) B(2) N(4) 111.92(17) yes . . . N(3) B(2) N(4) 104.55(12) yes . . . F(5) B(3) F(6) 103.34(13) yes . . . F(5) B(3) N(5) 110.39(15) yes . . . F(5) B(3) N(6) 111.78(17) yes . . . F(6) B(3) N(5) 116.08(16) yes . . . F(6) B(3) N(6) 111.74(15) yes . . . N(5) B(3) N(6) 103.74(11) yes . . . F(7) B(4) F(8) 109.86(13) yes . . . F(7) B(4) N(7) 106.95(14) yes . . . F(7) B(4) N(8) 110.39(17) yes . . . F(8) B(4) N(7) 110.88(17) yes . . . F(8) B(4) N(8) 112.29(13) yes . . . N(7) B(4) N(8) 106.29(13) yes . . . C(4) C(5) H(5) 119.100 no . . . C(6) C(5) H(5) 119.095 no . . . C(13) C(14) H(14) 119.885 no . . . C(15) C(14) H(14) 119.898 no . . . C(2) C(19) H(19) 114.178 no . . . C(12) C(19) H(19) 114.196 no . . . C(20) C(19) H(19) 114.196 no . . . C(19) C(20) H(20A) 109.830 no . . . C(19) C(20) H(20B) 109.826 no . . . C(21) C(20) H(20A) 109.816 no . . . C(21) C(20) H(20B) 109.824 no . . . H(20A) C(20) H(20B) 108.257 no . . . C(20) C(21) H(21A) 108.963 no . . . C(20) C(21) H(21B) 108.963 no . . . C(22) C(21) H(21A) 108.976 no . . . C(22) C(21) H(21B) 108.961 no . . . H(21A) C(21) H(21B) 107.755 no . . . C(3) C(22) H(22) 114.237 no . . . C(11) C(22) H(22) 114.235 no . . . C(21) C(22) H(22) 114.251 no . . . C(1) C(23) H(23A) 109.464 no . . . C(1) C(23) H(23B) 109.463 no . . . C(1) C(23) H(23C) 109.472 no . . . C(1) C(23) H(23D) 109.470 no . . . C(1) C(23) H(23E) 109.472 no . . . C(1) C(23) H(23F) 109.468 no . . . H(23A) C(23) H(23B) 109.469 no . . . H(23A) C(23) H(23C) 109.476 no . . . H(23A) C(23) H(23D) 141.067 no . . . H(23A) C(23) H(23E) 56.249 no . . . H(23A) C(23) H(23F) 56.249 no . . . H(23B) C(23) H(23C) 109.484 no . . . H(23B) C(23) H(23D) 56.252 no . . . H(23B) C(23) H(23E) 141.064 no . . . H(23B) C(23) H(23F) 56.245 no . . . H(23C) C(23) H(23D) 56.262 no . . . H(23C) C(23) H(23E) 56.255 no . . . H(23C) C(23) H(23F) 141.060 no . . . H(23D) C(23) H(23E) 109.485 no . . . H(23D) C(23) H(23F) 109.466 no . . . H(23E) C(23) H(23F) 109.466 no . . . C(7) C(24) H(24A) 110.095 no . . . C(7) C(24) H(24B) 110.095 no . . . C(25) C(24) H(24A) 110.094 no . . . C(25) C(24) H(24B) 110.097 no . . . H(24A) C(24) H(24B) 108.429 no . . . C(24) C(25) H(25A) 109.477 no . . . C(24) C(25) H(25B) 109.455 no . . . C(24) C(25) H(25C) 109.470 no . . . H(25A) C(25) H(25B) 109.477 no . . . H(25A) C(25) H(25C) 109.480 no . . . H(25B) C(25) H(25C) 109.470 no . . . C(8) C(26) H(26A) 109.233 no . . . C(8) C(26) H(26B) 109.229 no . . . C(27) C(26) H(26A) 109.245 no . . . C(27) C(26) H(26B) 109.223 no . . . H(26A) C(26) H(26B) 107.911 no . . . C(26) C(27) H(27A) 109.459 no . . . C(26) C(27) H(27B) 109.465 no . . . C(26) C(27) H(27C) 109.485 no . . . H(27A) C(27) H(27B) 109.469 no . . . H(27A) C(27) H(27C) 109.479 no . . . H(27B) C(27) H(27C) 109.470 no . . . C(9) C(28) H(28A) 109.462 no . . . C(9) C(28) H(28B) 109.468 no . . . C(9) C(28) H(28C) 109.460 no . . . C(9) C(28) H(28D) 109.453 no . . . C(9) C(28) H(28E) 109.457 no . . . C(9) C(28) H(28F) 109.468 no . . . H(28A) C(28) H(28B) 109.492 no . . . H(28A) C(28) H(28C) 109.473 no . . . H(28A) C(28) H(28D) 141.085 no . . . H(28A) C(28) H(28E) 56.251 no . . . H(28A) C(28) H(28F) 56.261 no . . . H(28B) C(28) H(28C) 109.472 no . . . H(28B) C(28) H(28D) 56.256 no . . . H(28B) C(28) H(28E) 141.074 no . . . H(28B) C(28) H(28F) 56.261 no . . . H(28C) C(28) H(28D) 56.249 no . . . H(28C) C(28) H(28E) 56.251 no . . . H(28C) C(28) H(28F) 141.071 no . . . H(28D) C(28) H(28E) 109.476 no . . . H(28D) C(28) H(28F) 109.490 no . . . H(28E) C(28) H(28F) 109.482 no . . . C(10) C(29) H(29A) 109.474 no . . . C(10) C(29) H(29B) 109.480 no . . . C(10) C(29) H(29C) 109.475 no . . . H(29A) C(29) H(29B) 109.463 no . . . H(29A) C(29) H(29C) 109.461 no . . . H(29B) C(29) H(29C) 109.474 no . . . C(16) C(30) H(30A) 107.865 no . . . C(16) C(30) H(30B) 107.874 no . . . C(31) C(30) H(30A) 107.858 no . . . C(31) C(30) H(30B) 107.868 no . . . H(30A) C(30) H(30B) 107.178 no . . . C(30) C(31) H(31A) 109.465 no . . . C(30) C(31) H(31B) 109.477 no . . . C(30) C(31) H(31C) 109.476 no . . . H(31A) C(31) H(31B) 109.466 no . . . H(31A) C(31) H(31C) 109.462 no . . . H(31B) C(31) H(31C) 109.482 no . . . C(17) C(32) H(32A) 109.191 no . . . C(17) C(32) H(32B) 109.182 no . . . C(33) C(32) H(32A) 109.182 no . . . C(33) C(32) H(32B) 109.192 no . . . H(32A) C(32) H(32B) 107.885 no . . . C(32) C(33) H(33A) 109.469 no . . . C(32) C(33) H(33B) 109.470 no . . . C(32) C(33) H(33C) 109.474 no . . . H(33A) C(33) H(33B) 109.460 no . . . H(33A) C(33) H(33C) 109.476 no . . . H(33B) C(33) H(33C) 109.479 no . . . C(18) C(34) H(34A) 109.480 no . . . C(18) C(34) H(34B) 109.477 no . . . C(18) C(34) H(34C) 109.473 no . . . H(34A) C(34) H(34B) 109.476 no . . . H(34A) C(34) H(34C) 109.477 no . . . H(34B) C(34) H(34C) 109.445 no . . . C(38) C(39) H(39) 120.183 no . . . C(40) C(39) H(39) 120.171 no . . . C(47) C(48) H(48) 119.125 no . . . C(49) C(48) H(48) 119.113 no . . . C(36) C(53) H(53) 114.221 no . . . C(46) C(53) H(53) 114.235 no . . . C(54) C(53) H(53) 114.238 no . . . C(53) C(54) H(54A) 108.887 no . . . C(53) C(54) H(54B) 108.867 no . . . C(55) C(54) H(54A) 108.888 no . . . C(55) C(54) H(54B) 108.884 no . . . H(54A) C(54) H(54B) 107.727 no . . . C(54) C(55) H(55A) 109.847 no . . . C(54) C(55) H(55B) 109.855 no . . . C(56) C(55) H(55A) 109.844 no . . . C(56) C(55) H(55B) 109.835 no . . . H(55A) C(55) H(55B) 108.280 no . . . C(37) C(56) H(56) 114.190 no . . . C(45) C(56) H(56) 114.175 no . . . C(55) C(56) H(56) 114.187 no . . . C(35) C(57) H(57A) 109.464 no . . . C(35) C(57) H(57B) 109.473 no . . . C(35) C(57) H(57C) 109.483 no . . . H(57A) C(57) H(57B) 109.459 no . . . H(57A) C(57) H(57C) 109.462 no . . . H(57B) C(57) H(57C) 109.485 no . . . C(41) C(58) H(58A) 107.711 no . . . C(41) C(58) H(58B) 107.700 no . . . C(59) C(58) H(58A) 107.724 no . . . C(59) C(58) H(58B) 107.719 no . . . H(58A) C(58) H(58B) 107.088 no . . . C(58) C(59) H(59A) 109.480 no . . . C(58) C(59) H(59B) 109.457 no . . . C(58) C(59) H(59C) 109.464 no . . . H(59A) C(59) H(59B) 109.485 no . . . H(59A) C(59) H(59C) 109.466 no . . . H(59B) C(59) H(59C) 109.476 no . . . C(42) C(60) H(60A) 109.584 no . . . C(42) C(60) H(60B) 109.582 no . . . C(61) C(60) H(60A) 109.585 no . . . C(61) C(60) H(60B) 109.583 no . . . H(60A) C(60) H(60B) 108.117 no . . . C(60) C(61) H(61A) 109.466 no . . . C(60) C(61) H(61B) 109.466 no . . . C(60) C(61) H(61C) 109.452 no . . . H(61A) C(61) H(61B) 109.479 no . . . H(61A) C(61) H(61C) 109.487 no . . . H(61B) C(61) H(61C) 109.477 no . . . C(43) C(62) H(62A) 109.485 no . . . C(43) C(62) H(62B) 109.465 no . . . C(43) C(62) H(62C) 109.468 no . . . C(43) C(62) H(62D) 109.466 no . . . C(43) C(62) H(62E) 109.474 no . . . C(43) C(62) H(62F) 109.478 no . . . H(62A) C(62) H(62B) 109.469 no . . . H(62A) C(62) H(62C) 109.477 no . . . H(62A) C(62) H(62D) 141.049 no . . . H(62A) C(62) H(62E) 56.249 no . . . H(62A) C(62) H(62F) 56.265 no . . . H(62B) C(62) H(62C) 109.463 no . . . H(62B) C(62) H(62D) 56.249 no . . . H(62B) C(62) H(62E) 141.061 no . . . H(62B) C(62) H(62F) 56.235 no . . . H(62C) C(62) H(62D) 56.242 no . . . H(62C) C(62) H(62E) 56.263 no . . . H(62C) C(62) H(62F) 141.054 no . . . H(62D) C(62) H(62E) 109.473 no . . . H(62D) C(62) H(62F) 109.453 no . . . H(62E) C(62) H(62F) 109.483 no . . . C(44) C(63) H(63A) 109.468 no . . . C(44) C(63) H(63B) 109.473 no . . . C(44) C(63) H(63C) 109.475 no . . . C(44) C(63) H(63D) 109.467 no . . . C(44) C(63) H(63E) 109.472 no . . . C(44) C(63) H(63F) 109.470 no . . . H(63A) C(63) H(63B) 109.469 no . . . H(63A) C(63) H(63C) 109.476 no . . . H(63A) C(63) H(63D) 141.065 no . . . H(63A) C(63) H(63E) 56.246 no . . . H(63A) C(63) H(63F) 56.250 no . . . H(63B) C(63) H(63C) 109.466 no . . . H(63B) C(63) H(63D) 56.242 no . . . H(63B) C(63) H(63E) 141.055 no . . . H(63B) C(63) H(63F) 56.249 no . . . H(63C) C(63) H(63D) 56.258 no . . . H(63C) C(63) H(63E) 56.261 no . . . H(63C) C(63) H(63F) 141.055 no . . . H(63D) C(63) H(63E) 109.489 no . . . H(63D) C(63) H(63F) 109.465 no . . . H(63E) C(63) H(63F) 109.465 no . . . C(50) C(64) H(64A) 109.951 no . . . C(50) C(64) H(64B) 109.971 no . . . C(65) C(64) H(64A) 109.970 no . . . C(65) C(64) H(64B) 109.964 no . . . H(64A) C(64) H(64B) 108.350 no . . . C(64) C(65) H(65A) 109.462 no . . . C(64) C(65) H(65B) 109.464 no . . . C(64) C(65) H(65C) 109.463 no . . . H(65A) C(65) H(65B) 109.465 no . . . H(65A) C(65) H(65C) 109.479 no . . . H(65B) C(65) H(65C) 109.494 no . . . C(51) C(66) H(66A) 109.347 no . . . C(51) C(66) H(66B) 109.350 no . . . C(67) C(66) H(66A) 109.351 no . . . C(67) C(66) H(66B) 109.346 no . . . H(66A) C(66) H(66B) 107.972 no . . . C(66) C(67) H(67A) 109.469 no . . . C(66) C(67) H(67B) 109.482 no . . . C(66) C(67) H(67C) 109.466 no . . . H(67A) C(67) H(67B) 109.482 no . . . H(67A) C(67) H(67C) 109.465 no . . . H(67B) C(67) H(67C) 109.463 no . . . C(52) C(68) H(68A) 109.467 no . . . C(52) C(68) H(68B) 109.479 no . . . C(52) C(68) H(68C) 109.474 no . . . C(52) C(68) H(68D) 109.470 no . . . C(52) C(68) H(68E) 109.456 no . . . C(52) C(68) H(68F) 109.465 no . . . H(68A) C(68) H(68B) 109.475 no . . . H(68A) C(68) H(68C) 109.462 no . . . H(68A) C(68) H(68D) 141.064 no . . . H(68A) C(68) H(68E) 56.249 no . . . H(68A) C(68) H(68F) 56.247 no . . . H(68B) C(68) H(68C) 109.471 no . . . H(68B) C(68) H(68D) 56.255 no . . . H(68B) C(68) H(68E) 141.065 no . . . H(68B) C(68) H(68F) 56.263 no . . . H(68C) C(68) H(68D) 56.251 no . . . H(68C) C(68) H(68E) 56.248 no . . . H(68C) C(68) H(68F) 141.061 no . . . H(68D) C(68) H(68E) 109.475 no . . . H(68D) C(68) H(68F) 109.490 no . . . H(68E) C(68) H(68F) 109.471 no . . . C(23) H(23A) H(23E) 61.868 no . . . C(23) H(23A) H(23F) 61.884 no . . . H(23E) H(23A) H(23F) 120.001 no . . . C(23) H(23B) H(23D) 61.868 no . . . C(23) H(23B) H(23F) 61.875 no . . . H(23D) H(23B) H(23F) 119.994 no . . . C(23) H(23C) H(23D) 61.867 no . . . C(23) H(23C) H(23E) 61.859 no . . . H(23D) H(23C) H(23E) 119.978 no . . . C(28) H(28A) H(28E) 61.884 no . . . C(28) H(28A) H(28F) 61.867 no . . . H(28E) H(28A) H(28F) 120.004 no . . . C(28) H(28B) H(28D) 61.867 no . . . C(28) H(28B) H(28F) 61.863 no . . . H(28D) H(28B) H(28F) 119.988 no . . . C(28) H(28C) H(28D) 61.866 no . . . C(28) H(28C) H(28E) 61.875 no . . . H(28D) H(28C) H(28E) 120.001 no . . . C(62) H(62A) H(62E) 61.880 no . . . C(62) H(62A) H(62F) 61.870 no . . . H(62E) H(62A) H(62F) 120.002 no . . . C(62) H(62B) H(62D) 61.878 no . . . C(62) H(62B) H(62F) 61.876 no . . . H(62D) H(62B) H(62F) 120.003 no . . . C(62) H(62C) H(62D) 61.882 no . . . C(62) H(62C) H(62E) 61.866 no . . . H(62D) H(62C) H(62E) 119.999 no . . . C(63) H(63A) H(63E) 61.862 no . . . C(63) H(63A) H(63F) 61.870 no . . . H(63E) H(63A) H(63F) 119.983 no . . . C(63) H(63B) H(63D) 61.876 no . . . C(63) H(63B) H(63F) 61.876 no . . . H(63D) H(63B) H(63F) 120.006 no . . . C(63) H(63C) H(63D) 61.879 no . . . C(63) H(63C) H(63E) 61.869 no . . . H(63D) H(63C) H(63E) 120.001 no . . . C(63) H(63D) H(63B) 61.882 no . . . C(63) H(63D) H(63C) 61.864 no . . . H(63B) H(63D) H(63C) 119.993 no . . . C(63) H(63E) H(63A) 61.893 no . . . C(63) H(63E) H(63C) 61.869 no . . . H(63A) H(63E) H(63C) 120.011 no . . . C(63) H(63F) H(63A) 61.880 no . . . C(63) H(63F) H(63B) 61.875 no . . . H(63A) H(63F) H(63B) 120.005 no . . . C(68) H(68A) H(68E) 61.878 no . . . C(68) H(68A) H(68F) 61.869 no . . . H(68E) H(68A) H(68F) 120.005 no . . . C(68) H(68B) H(68D) 61.871 no . . . C(68) H(68B) H(68F) 61.864 no . . . H(68D) H(68B) H(68F) 119.992 no . . . C(68) H(68C) H(68D) 61.868 no . . . C(68) H(68C) H(68E) 61.877 no . . . H(68D) H(68C) H(68E) 120.005 no . . . C(62) H(62D) H(62B) 61.873 no . . . C(62) H(62D) H(62C) 61.876 no . . . H(62B) H(62D) H(62C) 120.002 no . . . C(62) H(62E) H(62A) 61.871 no . . . C(62) H(62E) H(62C) 61.871 no . . . H(62A) H(62E) H(62C) 119.989 no . . . C(62) H(62F) H(62A) 61.866 no . . . C(62) H(62F) H(62B) 61.888 no . . . H(62A) H(62F) H(62B) 120.004 no . . . C(28) H(28D) H(28B) 61.877 no . . . C(28) H(28D) H(28C) 61.886 no . . . H(28B) H(28D) H(28C) 120.011 no . . . C(28) H(28E) H(28A) 61.865 no . . . C(28) H(28E) H(28C) 61.874 no . . . H(28A) H(28E) H(28C) 119.993 no . . . C(28) H(28F) H(28A) 61.872 no . . . C(28) H(28F) H(28B) 61.877 no . . . H(28A) H(28F) H(28B) 120.003 no . . . C(68) H(68D) H(68B) 61.875 no . . . C(68) H(68D) H(68C) 61.881 no . . . H(68B) H(68D) H(68C) 120.001 no . . . C(68) H(68E) H(68A) 61.874 no . . . C(68) H(68E) H(68C) 61.875 no . . . H(68A) H(68E) H(68C) 119.995 no . . . C(68) H(68F) H(68A) 61.884 no . . . C(68) H(68F) H(68B) 61.873 no . . . H(68A) H(68F) H(68B) 120.003 no . . . C(23) H(23D) H(23B) 61.880 no . . . C(23) H(23D) H(23C) 61.870 no . . . H(23B) H(23D) H(23C) 120.003 no . . . C(23) H(23E) H(23A) 61.883 no . . . C(23) H(23E) H(23C) 61.886 no . . . H(23A) H(23E) H(23C) 120.022 no . . . C(23) H(23F) H(23A) 61.867 no . . . C(23) H(23F) H(23B) 61.879 no . . . H(23A) H(23F) H(23B) 120.003 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(1) N(1) C(4) C(3) 0.63(17) no . . . . C(1) N(1) C(4) C(5) 179.36(13) no . . . . C(4) N(1) C(1) C(2) -1.03(17) no . . . . C(4) N(1) C(1) C(23) 179.18(13) no . . . . C(1) N(1) B(1) F(1) -57.1(2) no . . . . C(1) N(1) B(1) F(2) 63.5(2) no . . . . C(1) N(1) B(1) N(2) -174.94(14) no . . . . B(1) N(1) C(1) C(2) -179.04(15) no . . . . B(1) N(1) C(1) C(23) 1.2(3) no . . . . C(4) N(1) B(1) F(1) 125.12(15) no . . . . C(4) N(1) B(1) F(2) -114.26(15) no . . . . C(4) N(1) B(1) N(2) 7.3(2) no . . . . B(1) N(1) C(4) C(3) 178.75(14) no . . . . B(1) N(1) C(4) C(5) -2.5(3) no . . . . C(6) N(2) C(9) C(8) 0.12(17) no . . . . C(6) N(2) C(9) C(28) -179.30(13) no . . . . C(9) N(2) C(6) C(5) -174.71(14) no . . . . C(9) N(2) C(6) C(7) 1.10(17) no . . . . C(6) N(2) B(1) F(1) -126.35(17) no . . . . C(6) N(2) B(1) F(2) 110.63(17) no . . . . C(6) N(2) B(1) N(1) -10.5(3) no . . . . B(1) N(2) C(6) C(5) 7.8(3) no . . . . B(1) N(2) C(6) C(7) -176.38(13) no . . . . C(9) N(2) B(1) F(1) 56.8(2) no . . . . C(9) N(2) B(1) F(2) -66.2(3) no . . . . C(9) N(2) B(1) N(1) 172.70(15) no . . . . B(1) N(2) C(9) C(8) 177.54(14) no . . . . B(1) N(2) C(9) C(28) -1.9(3) no . . . . C(10) N(3) C(13) C(12) 0.8(2) no . . . . C(10) N(3) C(13) C(14) -175.17(16) no . . . . C(13) N(3) C(10) C(11) -0.1(2) no . . . . C(13) N(3) C(10) C(29) 179.39(16) no . . . . C(10) N(3) B(2) F(3) -64.8(3) no . . . . C(10) N(3) B(2) F(4) 52.3(3) no . . . . C(10) N(3) B(2) N(4) 172.27(17) no . . . . B(2) N(3) C(10) C(11) -177.79(16) no . . . . B(2) N(3) C(10) C(29) 1.7(3) no . . . . C(13) N(3) B(2) F(3) 117.92(18) no . . . . C(13) N(3) B(2) F(4) -124.99(18) no . . . . C(13) N(3) B(2) N(4) -5.0(3) no . . . . B(2) N(3) C(13) C(12) 178.48(16) no . . . . B(2) N(3) C(13) C(14) 2.5(3) no . . . . C(15) N(4) C(18) C(17) -0.2(2) no . . . . C(15) N(4) C(18) C(34) 178.14(16) no . . . . C(18) N(4) C(15) C(14) 178.89(17) no . . . . C(18) N(4) C(15) C(16) -0.2(2) no . . . . C(15) N(4) B(2) F(3) -120.77(17) no . . . . C(15) N(4) B(2) F(4) 123.25(17) no . . . . C(15) N(4) B(2) N(3) 5.1(3) no . . . . B(2) N(4) C(15) C(14) -2.8(3) no . . . . B(2) N(4) C(15) C(16) 178.16(16) no . . . . C(18) N(4) B(2) F(3) 57.3(3) no . . . . C(18) N(4) B(2) F(4) -58.7(3) no . . . . C(18) N(4) B(2) N(3) -176.87(17) no . . . . B(2) N(4) C(18) C(17) -178.52(16) no . . . . B(2) N(4) C(18) C(34) -0.2(3) no . . . . C(35) N(5) C(38) C(37) 0.2(2) no . . . . C(35) N(5) C(38) C(39) -176.05(16) no . . . . C(38) N(5) C(35) C(36) -0.4(2) no . . . . C(38) N(5) C(35) C(57) 178.01(15) no . . . . C(35) N(5) B(3) F(5) 49.0(3) no . . . . C(35) N(5) B(3) F(6) -68.1(3) no . . . . C(35) N(5) B(3) N(6) 168.90(17) no . . . . B(3) N(5) C(35) C(36) -178.47(16) no . . . . B(3) N(5) C(35) C(57) -0.0(3) no . . . . C(38) N(5) B(3) F(5) -128.71(17) no . . . . C(38) N(5) B(3) F(6) 114.15(18) no . . . . C(38) N(5) B(3) N(6) -8.8(3) no . . . . B(3) N(5) C(38) C(37) 178.28(16) no . . . . B(3) N(5) C(38) C(39) 2.0(3) no . . . . C(40) N(6) C(43) C(42) -0.5(2) no . . . . C(40) N(6) C(43) C(62) 177.58(16) no . . . . C(43) N(6) C(40) C(39) 173.17(16) no . . . . C(43) N(6) C(40) C(41) -0.5(2) no . . . . C(40) N(6) B(3) F(5) 131.16(17) no . . . . C(40) N(6) B(3) F(6) -113.57(18) no . . . . C(40) N(6) B(3) N(5) 12.2(3) no . . . . B(3) N(6) C(40) C(39) -9.0(3) no . . . . B(3) N(6) C(40) C(41) 177.38(16) no . . . . C(43) N(6) B(3) F(5) -51.4(3) no . . . . C(43) N(6) B(3) F(6) 63.9(3) no . . . . C(43) N(6) B(3) N(5) -170.33(17) no . . . . B(3) N(6) C(43) C(42) -178.30(16) no . . . . B(3) N(6) C(43) C(62) -0.3(3) no . . . . C(44) N(7) C(47) C(46) 1.30(17) no . . . . C(44) N(7) C(47) C(48) 178.73(14) no . . . . C(47) N(7) C(44) C(45) -0.59(18) no . . . . C(47) N(7) C(44) C(63) -179.28(14) no . . . . C(44) N(7) B(4) F(7) -57.0(2) no . . . . C(44) N(7) B(4) F(8) 62.8(2) no . . . . C(44) N(7) B(4) N(8) -174.91(14) no . . . . B(4) N(7) C(44) C(45) 178.77(14) no . . . . B(4) N(7) C(44) C(63) 0.1(3) no . . . . C(47) N(7) B(4) F(7) 122.33(15) no . . . . C(47) N(7) B(4) F(8) -117.91(15) no . . . . C(47) N(7) B(4) N(8) 4.4(2) no . . . . B(4) N(7) C(47) C(46) -178.08(14) no . . . . B(4) N(7) C(47) C(48) -0.6(3) no . . . . C(49) N(8) C(52) C(51) -1.47(17) no . . . . C(49) N(8) C(52) C(68) 176.67(13) no . . . . C(52) N(8) C(49) C(48) -173.94(14) no . . . . C(52) N(8) C(49) C(50) 1.77(18) no . . . . C(49) N(8) B(4) F(7) -123.45(17) no . . . . C(49) N(8) B(4) F(8) 113.59(17) no . . . . C(49) N(8) B(4) N(7) -7.8(3) no . . . . B(4) N(8) C(49) C(48) 6.8(3) no . . . . B(4) N(8) C(49) C(50) -177.47(13) no . . . . C(52) N(8) B(4) F(7) 57.5(2) no . . . . C(52) N(8) B(4) F(8) -65.5(3) no . . . . C(52) N(8) B(4) N(7) 173.12(15) no . . . . B(4) N(8) C(52) C(51) 177.77(13) no . . . . B(4) N(8) C(52) C(68) -4.1(3) no . . . . N(1) C(1) C(2) C(3) 1.01(17) no . . . . N(1) C(1) C(2) C(19) 176.59(16) no . . . . C(23) C(1) C(2) C(3) -179.21(15) no . . . . C(23) C(1) C(2) C(19) -3.6(3) no . . . . C(1) C(2) C(3) C(4) -0.65(18) no . . . . C(1) C(2) C(3) C(22) 175.56(13) no . . . . C(1) C(2) C(19) C(12) 135.55(19) no . . . . C(1) C(2) C(19) C(20) -113.1(2) no . . . . C(3) C(2) C(19) C(12) -49.13(18) no . . . . C(3) C(2) C(19) C(20) 62.24(16) no . . . . C(19) C(2) C(3) C(4) -177.17(13) no . . . . C(19) C(2) C(3) C(22) -1.0(2) no . . . . C(2) C(3) C(4) N(1) 0.02(17) no . . . . C(2) C(3) C(4) C(5) -178.58(15) no . . . . C(2) C(3) C(22) C(11) 53.62(19) no . . . . C(2) C(3) C(22) C(21) -57.88(16) no . . . . C(4) C(3) C(22) C(11) -131.34(18) no . . . . C(4) C(3) C(22) C(21) 117.15(19) no . . . . C(22) C(3) C(4) N(1) -175.30(17) no . . . . C(22) C(3) C(4) C(5) 6.1(4) no . . . . N(1) C(4) C(5) C(6) -1.5(3) no . . . . C(3) C(4) C(5) C(6) 176.83(16) no . . . . C(4) C(5) C(6) N(2) -1.0(3) no . . . . C(4) C(5) C(6) C(7) -175.96(14) no . . . . N(2) C(6) C(7) C(8) -1.95(18) no . . . . N(2) C(6) C(7) C(24) 175.55(13) no . . . . C(5) C(6) C(7) C(8) 173.22(17) no . . . . C(5) C(6) C(7) C(24) -9.3(3) no . . . . C(6) C(7) C(8) C(9) 1.88(18) no . . . . C(6) C(7) C(8) C(26) 179.49(14) no . . . . C(6) C(7) C(24) C(25) -74.0(2) no . . . . C(8) C(7) C(24) C(25) 102.9(3) no . . . . C(24) C(7) C(8) C(9) -175.58(16) no . . . . C(24) C(7) C(8) C(26) 2.0(3) no . . . . C(7) C(8) C(9) N(2) -1.4(2) no . . . . C(7) C(8) C(9) C(28) 177.97(16) no . . . . C(7) C(8) C(26) C(27) -91.2(2) no . . . . C(9) C(8) C(26) C(27) 85.9(3) no . . . . C(26) C(8) C(9) N(2) -178.91(16) no . . . . C(26) C(8) C(9) C(28) 0.4(3) no . . . . N(3) C(10) C(11) C(12) -0.7(3) no . . . . N(3) C(10) C(11) C(22) 171.71(19) no . . . . C(29) C(10) C(11) C(12) 179.93(19) no . . . . C(29) C(10) C(11) C(22) -7.7(4) no . . . . C(10) C(11) C(12) C(13) 1.1(3) no . . . . C(10) C(11) C(12) C(19) 174.24(16) no . . . . C(10) C(11) C(22) C(3) 136.9(3) no . . . . C(10) C(11) C(22) C(21) -118.4(3) no . . . . C(12) C(11) C(22) C(3) -50.8(2) no . . . . C(12) C(11) C(22) C(21) 53.8(2) no . . . . C(22) C(11) C(12) C(13) -173.27(15) no . . . . C(22) C(11) C(12) C(19) -0.2(3) no . . . . C(11) C(12) C(13) N(3) -1.2(3) no . . . . C(11) C(12) C(13) C(14) 174.29(18) no . . . . C(11) C(12) C(19) C(2) 49.7(3) no . . . . C(11) C(12) C(19) C(20) -57.5(3) no . . . . C(13) C(12) C(19) C(2) -140.2(3) no . . . . C(13) C(12) C(19) C(20) 112.6(3) no . . . . C(19) C(12) C(13) N(3) -172.0(3) no . . . . C(19) C(12) C(13) C(14) 3.4(4) no . . . . N(3) C(13) C(14) C(15) 0.9(3) no . . . . C(12) C(13) C(14) C(15) -174.10(19) no . . . . C(13) C(14) C(15) N(4) -0.8(3) no . . . . C(13) C(14) C(15) C(16) 178.03(17) no . . . . N(4) C(15) C(16) C(17) 0.4(2) no . . . . N(4) C(15) C(16) C(30) 179.69(15) no . . . . C(14) C(15) C(16) C(17) -178.51(19) no . . . . C(14) C(15) C(16) C(30) 0.7(4) no . . . . C(15) C(16) C(17) C(18) -0.6(3) no . . . . C(15) C(16) C(17) C(32) -179.89(18) no . . . . C(15) C(16) C(30) C(31) -83.4(3) no . . . . C(17) C(16) C(30) C(31) 95.7(3) no . . . . C(30) C(16) C(17) C(18) -179.77(19) no . . . . C(30) C(16) C(17) C(32) 0.9(4) no . . . . C(16) C(17) C(18) N(4) 0.5(3) no . . . . C(16) C(17) C(18) C(34) -177.75(17) no . . . . C(16) C(17) C(32) C(33) -88.0(3) no . . . . C(18) C(17) C(32) C(33) 92.8(3) no . . . . C(32) C(17) C(18) N(4) 179.84(18) no . . . . C(32) C(17) C(18) C(34) 1.6(4) no . . . . C(2) C(19) C(20) C(21) -54.47(14) no . . . . C(12) C(19) C(20) C(21) 54.50(17) no . . . . C(19) C(20) C(21) C(22) -2.87(19) no . . . . C(20) C(21) C(22) C(3) 57.94(16) no . . . . C(20) C(21) C(22) C(11) -52.53(18) no . . . . N(5) C(35) C(36) C(37) 0.5(2) no . . . . N(5) C(35) C(36) C(53) 173.11(19) no . . . . C(57) C(35) C(36) C(37) -177.71(18) no . . . . C(57) C(35) C(36) C(53) -5.1(4) no . . . . C(35) C(36) C(37) C(38) -0.4(2) no . . . . C(35) C(36) C(37) C(56) 173.63(15) no . . . . C(35) C(36) C(53) C(46) 137.4(3) no . . . . C(35) C(36) C(53) C(54) -117.9(3) no . . . . C(37) C(36) C(53) C(46) -50.0(2) no . . . . C(37) C(36) C(53) C(54) 54.64(19) no . . . . C(53) C(36) C(37) C(38) -175.06(15) no . . . . C(53) C(36) C(37) C(56) -1.1(3) no . . . . C(36) C(37) C(38) N(5) 0.1(2) no . . . . C(36) C(37) C(38) C(39) 176.03(18) no . . . . C(36) C(37) C(56) C(45) 50.6(2) no . . . . C(36) C(37) C(56) C(55) -57.1(2) no . . . . C(38) C(37) C(56) C(45) -137.8(3) no . . . . C(38) C(37) C(56) C(55) 114.6(3) no . . . . C(56) C(37) C(38) N(5) -172.2(2) no . . . . C(56) C(37) C(38) C(39) 3.7(4) no . . . . N(5) C(38) C(39) C(40) 3.5(3) no . . . . C(37) C(38) C(39) C(40) -171.93(18) no . . . . C(38) C(39) C(40) N(6) -0.3(3) no . . . . C(38) C(39) C(40) C(41) 172.10(17) no . . . . N(6) C(40) C(41) C(42) 1.2(2) no . . . . N(6) C(40) C(41) C(58) -179.41(16) no . . . . C(39) C(40) C(41) C(42) -171.96(19) no . . . . C(39) C(40) C(41) C(58) 7.5(4) no . . . . C(40) C(41) C(42) C(43) -1.4(3) no . . . . C(40) C(41) C(42) C(60) 175.91(17) no . . . . C(40) C(41) C(58) C(59) -80.9(3) no . . . . C(42) C(41) C(58) C(59) 98.4(3) no . . . . C(58) C(41) C(42) C(43) 179.17(19) no . . . . C(58) C(41) C(42) C(60) -3.5(4) no . . . . C(41) C(42) C(43) N(6) 1.2(3) no . . . . C(41) C(42) C(43) C(62) -176.63(18) no . . . . C(41) C(42) C(60) C(61) -82.2(3) no . . . . C(43) C(42) C(60) C(61) 94.8(3) no . . . . C(60) C(42) C(43) N(6) -176.15(19) no . . . . C(60) C(42) C(43) C(62) 6.0(4) no . . . . N(7) C(44) C(45) C(46) -0.34(19) no . . . . N(7) C(44) C(45) C(56) 178.04(15) no . . . . C(63) C(44) C(45) C(46) 178.31(16) no . . . . C(63) C(44) C(45) C(56) -3.3(4) no . . . . C(44) C(45) C(46) C(47) 1.17(19) no . . . . C(44) C(45) C(46) C(53) -179.96(13) no . . . . C(44) C(45) C(56) C(37) 131.28(19) no . . . . C(44) C(45) C(56) C(55) -117.3(2) no . . . . C(46) C(45) C(56) C(37) -50.44(18) no . . . . C(46) C(45) C(56) C(55) 60.97(16) no . . . . C(56) C(45) C(46) C(47) -177.51(13) no . . . . C(56) C(45) C(46) C(53) 1.4(2) no . . . . C(45) C(46) C(47) N(7) -1.44(17) no . . . . C(45) C(46) C(47) C(48) -178.51(15) no . . . . C(45) C(46) C(53) C(36) 52.05(19) no . . . . C(45) C(46) C(53) C(54) -58.65(16) no . . . . C(47) C(46) C(53) C(36) -129.49(19) no . . . . C(47) C(46) C(53) C(54) 119.8(2) no . . . . C(53) C(46) C(47) N(7) -179.98(18) no . . . . C(53) C(46) C(47) C(48) 2.9(4) no . . . . N(7) C(47) C(48) C(49) -1.3(3) no . . . . C(46) C(47) C(48) C(49) 175.33(16) no . . . . C(47) C(48) C(49) N(8) -1.6(3) no . . . . C(47) C(48) C(49) C(50) -176.43(15) no . . . . N(8) C(49) C(50) C(51) -1.38(19) no . . . . N(8) C(49) C(50) C(64) 176.26(14) no . . . . C(48) C(49) C(50) C(51) 173.66(18) no . . . . C(48) C(49) C(50) C(64) -8.7(3) no . . . . C(49) C(50) C(51) C(52) 0.43(18) no . . . . C(49) C(50) C(51) C(66) -179.47(15) no . . . . C(49) C(50) C(64) C(65) -83.8(2) no . . . . C(51) C(50) C(64) C(65) 93.3(3) no . . . . C(64) C(50) C(51) C(52) -177.22(17) no . . . . C(64) C(50) C(51) C(66) 2.9(3) no . . . . C(50) C(51) C(52) N(8) 0.7(2) no . . . . C(50) C(51) C(52) C(68) -177.21(15) no . . . . C(50) C(51) C(66) C(67) -108.00(19) no . . . . C(52) C(51) C(66) C(67) 72.1(3) no . . . . C(66) C(51) C(52) N(8) -179.42(15) no . . . . C(66) C(51) C(52) C(68) 2.7(3) no . . . . C(36) C(53) C(54) C(55) -54.15(17) no . . . . C(46) C(53) C(54) C(55) 57.18(15) no . . . . C(53) C(54) C(55) C(56) -1.45(19) no . . . . C(54) C(55) C(56) C(37) 53.29(17) no . . . . C(54) C(55) C(56) C(45) -55.23(15) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 F(1) C(1) 2.937(3) no . . F(1) C(4) 3.429(3) no . . F(1) C(6) 3.5868(19) no . . F(1) C(9) 3.077(2) no . . F(1) C(23) 3.077(3) no . . F(1) C(28) 3.027(3) no . . F(2) C(1) 3.1200(19) no . . F(2) C(4) 3.4952(17) no . . F(2) C(6) 3.5995(16) no . . F(2) C(9) 3.233(2) no . . F(2) C(23) 3.292(2) no . . F(2) C(28) 3.262(3) no . . F(3) C(10) 3.2695(17) no . . F(3) C(18) 3.112(2) no . . F(3) C(29) 3.3170(18) no . . F(3) C(34) 3.172(2) no . . F(4) C(10) 3.0150(18) no . . F(4) C(18) 3.0857(18) no . . F(4) C(29) 3.0228(19) no . . F(4) C(34) 3.1840(19) no . . F(5) C(35) 3.0418(17) no . . F(5) C(43) 3.0495(18) no . . F(5) C(57) 3.0098(19) no . . F(5) C(62) 3.0577(19) no . . F(6) C(35) 3.3081(17) no . . F(6) C(43) 3.168(2) no . . F(6) C(57) 3.4041(19) no . . F(6) C(62) 3.258(2) no . . F(7) C(44) 2.893(3) no . . F(7) C(47) 3.412(3) no . . F(7) C(49) 3.5655(19) no . . F(7) C(52) 3.0599(19) no . . F(7) C(63) 3.034(3) no . . F(7) C(68) 2.995(3) no . . F(8) C(44) 3.0771(19) no . . F(8) C(47) 3.5290(17) no . . F(8) C(52) 3.218(2) no . . F(8) C(63) 3.225(2) no . . F(8) C(68) 3.254(3) no . . N(1) C(6) 2.868(2) no . . N(2) C(4) 2.696(3) no . . N(3) C(15) 2.834(2) no . . N(4) C(13) 2.8712(19) no . . N(5) C(40) 2.8542(19) no . . N(6) C(38) 2.8453(19) no . . N(7) C(49) 2.859(2) no . . N(8) C(47) 2.709(3) no . . C(1) C(20) 3.427(3) no . . C(1) C(22) 3.573(3) no . . C(2) C(11) 2.809(2) no . . C(2) C(21) 2.707(3) no . . C(3) C(12) 2.741(3) no . . C(3) C(20) 2.800(3) no . . C(3) B(1) 3.599(3) no . . C(4) C(11) 3.592(3) no . . C(4) C(19) 3.593(3) no . . C(4) C(21) 3.418(3) no . . C(5) C(8) 3.452(3) no . . C(5) C(9) 3.342(3) no . . C(5) C(22) 3.275(3) no . . C(5) C(24) 3.180(3) no . . C(5) B(1) 2.963(3) no . . C(6) C(25) 3.252(3) no . . C(6) C(28) 3.495(3) no . . C(7) C(27) 3.349(3) no . . C(8) C(25) 3.419(4) no . . C(9) C(27) 3.426(3) no . . C(10) C(14) 3.589(2) no . . C(11) C(20) 2.982(3) no . . C(12) C(21) 2.874(3) no . . C(14) C(19) 3.480(2) no . . C(14) C(30) 3.193(3) no . . C(14) B(2) 3.109(3) no . . C(15) C(31) 3.497(3) no . . C(16) C(33) 3.385(3) no . . C(18) C(33) 3.390(3) no . . C(19) C(22) 2.712(3) no . . C(19) C(23) 3.317(3) no . . C(22) C(29) 3.571(2) no . . C(23) B(1) 3.124(3) no . . C(24) C(26) 3.091(4) no . . C(26) C(28) 3.247(3) no . . C(28) B(1) 2.991(4) no . . C(29) B(2) 3.097(3) no . . C(30) C(32) 3.321(3) no . . C(32) C(34) 3.230(3) no . . C(34) B(2) 3.132(3) no . . C(36) C(45) 2.819(2) no . . C(36) C(55) 2.985(3) no . . C(37) C(44) 3.574(3) no . . C(37) C(46) 2.747(3) no . . C(37) C(54) 2.844(3) no . . C(39) C(43) 3.586(2) no . . C(39) C(56) 3.424(2) no . . C(39) C(58) 3.178(3) no . . C(39) B(3) 3.125(2) no . . C(40) C(59) 3.503(3) no . . C(41) C(61) 3.289(4) no . . C(43) C(61) 3.411(3) no . . C(44) C(53) 3.591(3) no . . C(44) C(55) 3.436(3) no . . C(45) C(54) 2.713(3) no . . C(45) B(4) 3.586(3) no . . C(46) C(55) 2.803(3) no . . C(47) C(54) 3.465(3) no . . C(47) C(56) 3.598(3) no . . C(48) C(51) 3.470(3) no . . C(48) C(52) 3.360(3) no . . C(48) C(53) 3.358(3) no . . C(48) C(64) 3.214(3) no . . C(48) B(4) 2.972(3) no . . C(49) C(65) 3.356(3) no . . C(49) C(68) 3.507(3) no . . C(50) C(67) 3.494(3) no . . C(51) C(65) 3.356(4) no . . C(52) C(67) 3.292(3) no . . C(53) C(56) 2.715(2) no . . C(56) C(63) 3.277(3) no . . C(57) B(3) 3.115(3) no . . C(58) C(60) 3.286(3) no . . C(60) C(62) 3.289(3) no . . C(62) B(3) 3.111(3) no . . C(63) B(4) 3.094(3) no . . C(64) C(66) 3.106(3) no . . C(66) C(68) 3.232(3) no . . C(68) B(4) 2.972(4) no . . F(2) C(14) 3.3952(16) no . 2_656 F(2) C(19) 3.4179(19) no . 2_656 F(3) C(48) 3.4509(16) no . . F(3) C(53) 3.293(2) no . . F(3) C(57) 3.310(2) no . . F(3) C(60) 3.459(3) no . 1_565 F(4) C(28) 3.429(3) no . 4_564 F(5) C(24) 3.5487(18) no . 1_545 F(5) C(68) 3.579(3) no . 4_555 F(6) C(16) 3.411(2) no . . F(6) C(17) 3.287(3) no . . F(6) C(29) 3.4857(19) no . 1_545 F(6) C(30) 3.501(3) no . . F(6) C(32) 3.157(3) no . . F(8) C(39) 3.5532(16) no . 2_555 F(8) C(56) 3.3543(18) no . 2_555 N(4) C(57) 3.296(3) no . . N(6) C(29) 3.591(3) no . 1_545 C(14) F(2) 3.3952(16) no . 2_646 C(15) C(57) 3.508(3) no . . C(16) F(6) 3.411(2) no . . C(17) F(6) 3.287(3) no . . C(18) C(35) 3.564(3) no . . C(18) C(57) 3.469(3) no . . C(19) F(2) 3.4179(19) no . 2_646 C(24) F(5) 3.5487(18) no . 1_565 C(28) F(4) 3.429(3) no . 4_565 C(29) F(6) 3.4857(19) no . 1_565 C(29) N(6) 3.591(3) no . 1_565 C(29) C(43) 3.409(3) no . 1_565 C(30) F(6) 3.501(3) no . . C(32) F(6) 3.157(3) no . . C(34) C(36) 3.536(3) no . . C(34) C(46) 3.575(3) no . . C(34) C(47) 3.595(3) no . . C(35) C(18) 3.564(3) no . . C(36) C(34) 3.536(3) no . . C(39) F(8) 3.5532(16) no . 2_545 C(39) C(65) 3.515(4) no . 1_545 C(43) C(29) 3.409(3) no . 1_545 C(46) C(34) 3.575(3) no . . C(47) C(34) 3.595(3) no . . C(48) F(3) 3.4509(16) no . . C(53) F(3) 3.293(2) no . . C(56) F(8) 3.3543(18) no . 2_545 C(57) F(3) 3.310(2) no . . C(57) N(4) 3.296(3) no . . C(57) C(15) 3.508(3) no . . C(57) C(18) 3.469(3) no . . C(60) F(3) 3.459(3) no . 1_545 C(65) C(39) 3.515(4) no . 1_565 C(68) F(5) 3.579(3) no . 4_554 F(1) H(23A) 3.0963 no . . F(1) H(23C) 2.7221 no . . F(1) H(28A) 2.4256 no . . F(1) H(28C) 3.2133 no . . F(1) H(28E) 2.3842 no . . F(1) H(28F) 3.2746 no . . F(1) H(23D) 3.5522 no . . F(1) H(23E) 2.4282 no . . F(2) H(23A) 2.7346 no . . F(2) H(23C) 3.5684 no . . F(2) H(28A) 3.2793 no . . F(2) H(28C) 2.8057 no . . F(2) H(28E) 2.5511 no . . F(2) H(23E) 2.7714 no . . F(2) H(23F) 3.5111 no . . F(3) H(29A) 3.5828 no . . F(3) H(29C) 2.6947 no . . F(3) H(34A) 3.1573 no . . F(3) H(34C) 2.7854 no . . F(4) H(29A) 2.6935 no . . F(4) H(29C) 2.9368 no . . F(4) H(34C) 2.4799 no . . F(5) H(57A) 2.6240 no . . F(5) H(57C) 2.9621 no . . F(5) H(62A) 3.2553 no . . F(5) H(62C) 2.4931 no . . F(5) H(62D) 3.3246 no . . F(5) H(62E) 2.4469 no . . F(6) H(57C) 2.8373 no . . F(6) H(62A) 2.8660 no . . F(6) H(62C) 3.2574 no . . F(6) H(62E) 2.5728 no . . F(7) H(63A) 3.0338 no . . F(7) H(63C) 2.7050 no . . F(7) H(63D) 3.5321 no . . F(7) H(63E) 2.3835 no . . F(7) H(68A) 2.4714 no . . F(7) H(68C) 3.0739 no . . F(7) H(68E) 2.2895 no . . F(7) H(68F) 3.3435 no . . F(8) H(63A) 2.6449 no . . F(8) H(63C) 3.5296 no . . F(8) H(63E) 2.7198 no . . F(8) H(63F) 3.4139 no . . F(8) H(68A) 3.3776 no . . F(8) H(68C) 2.7195 no . . F(8) H(68D) 3.5693 no . . F(8) H(68E) 2.5940 no . . N(1) H(5) 3.3058 no . . N(1) H(23A) 2.7757 no . . N(1) H(23B) 3.3147 no . . N(1) H(23C) 2.8601 no . . N(1) H(23D) 3.1953 no . . N(1) H(23E) 2.6320 no . . N(1) H(23F) 3.1201 no . . N(2) H(5) 3.1752 no . . N(2) H(28A) 2.5674 no . . N(2) H(28B) 3.1608 no . . N(2) H(28C) 2.6668 no . . N(2) H(28D) 3.0336 no . . N(2) H(28E) 2.4095 no . . N(2) H(28F) 2.9469 no . . N(3) H(14) 3.3297 no . . N(3) H(29A) 2.8678 no . . N(3) H(29B) 3.3096 no . . N(3) H(29C) 2.7191 no . . N(4) H(14) 3.3452 no . . N(4) H(34A) 3.0323 no . . N(4) H(34B) 3.2783 no . . N(4) H(34C) 2.6738 no . . N(5) H(39) 3.3511 no . . N(5) H(57A) 2.8282 no . . N(5) H(57B) 3.3136 no . . N(5) H(57C) 2.7426 no . . N(6) H(39) 3.3402 no . . N(6) H(62A) 2.8530 no . . N(6) H(62B) 3.3187 no . . N(6) H(62C) 2.7611 no . . N(6) H(62D) 3.1165 no . . N(6) H(62E) 2.6147 no . . N(6) H(62F) 3.1982 no . . N(7) H(48) 3.3050 no . . N(7) H(63A) 2.7732 no . . N(7) H(63B) 3.3172 no . . N(7) H(63C) 2.8847 no . . N(7) H(63D) 3.2125 no . . N(7) H(63E) 2.6470 no . . N(7) H(63F) 3.1127 no . . N(8) H(48) 3.1862 no . . N(8) H(68A) 2.6061 no . . N(8) H(68B) 3.1672 no . . N(8) H(68C) 2.6369 no . . N(8) H(68D) 3.0097 no . . N(8) H(68E) 2.4122 no . . N(8) H(68F) 2.9826 no . . C(1) H(19) 2.8314 no . . C(1) H(20B) 3.3330 no . . C(2) H(20A) 3.2084 no . . C(2) H(20B) 2.5595 no . . C(2) H(21B) 3.0124 no . . C(2) H(22) 3.3020 no . . C(2) H(23A) 3.2064 no . . C(2) H(23B) 2.6714 no . . C(2) H(23C) 3.1326 no . . C(2) H(23D) 2.8057 no . . C(2) H(23E) 3.3191 no . . C(2) H(23F) 2.8881 no . . C(3) H(5) 2.7597 no . . C(3) H(19) 3.3074 no . . C(3) H(20B) 3.1646 no . . C(3) H(21A) 3.1868 no . . C(3) H(21B) 2.5053 no . . C(4) H(21B) 3.2904 no . . C(4) H(22) 2.7900 no . . C(5) H(22) 3.0435 no . . C(5) H(24B) 3.0321 no . . C(5) H(25C) 3.0406 no . . C(6) H(24A) 3.3899 no . . C(6) H(24B) 2.8259 no . . C(6) H(25A) 3.5788 no . . C(6) H(25C) 2.9507 no . . C(7) H(5) 2.6981 no . . C(7) H(25A) 2.6869 no . . C(7) H(25B) 3.3133 no . . C(7) H(25C) 2.6154 no . . C(7) H(26A) 3.2013 no . . C(7) H(26B) 2.6102 no . . C(7) H(27C) 3.1738 no . . C(8) H(24A) 2.6729 no . . C(8) H(24B) 3.2222 no . . C(8) H(25A) 3.3026 no . . C(8) H(27A) 2.7275 no . . C(8) H(27B) 3.3409 no . . C(8) H(27C) 2.7066 no . . C(8) H(28A) 3.2570 no . . C(8) H(28B) 2.6963 no . . C(8) H(28C) 3.1713 no . . C(8) H(28D) 2.8309 no . . C(8) H(28E) 3.3695 no . . C(8) H(28F) 2.9268 no . . C(9) H(26A) 2.7502 no . . C(9) H(26B) 3.3527 no . . C(9) H(27A) 3.2290 no . . C(10) H(22) 3.0071 no . . C(11) H(19) 3.4027 no . . C(11) H(20A) 3.3121 no . . C(11) H(21A) 2.7844 no . . C(11) H(21B) 3.3836 no . . C(11) H(29A) 3.2400 no . . C(11) H(29B) 2.8177 no . . C(11) H(29C) 3.3655 no . . C(12) H(14) 2.7942 no . . C(12) H(20A) 2.7361 no . . C(12) H(20B) 3.3786 no . . C(12) H(21A) 3.2485 no . . C(12) H(22) 3.3264 no . . C(13) H(19) 3.0480 no . . C(14) H(19) 3.3223 no . . C(14) H(30A) 2.9516 no . . C(14) H(31C) 3.3522 no . . C(15) H(30A) 2.7592 no . . C(15) H(30B) 3.3637 no . . C(15) H(31C) 3.3432 no . . C(16) H(14) 2.7836 no . . C(16) H(31A) 2.8108 no . . C(16) H(31B) 3.4410 no . . C(16) H(31C) 2.8702 no . . C(16) H(32A) 2.7619 no . . C(16) H(32B) 3.3566 no . . C(16) H(33C) 3.1597 no . . C(17) H(30A) 3.3668 no . . C(17) H(30B) 2.8018 no . . C(17) H(31A) 3.4963 no . . C(17) H(33A) 2.6574 no . . C(17) H(33B) 3.2920 no . . C(17) H(33C) 2.6278 no . . C(17) H(34A) 3.0912 no . . C(17) H(34B) 2.8484 no . . C(17) H(34C) 3.4224 no . . C(18) H(32A) 3.3281 no . . C(18) H(32B) 2.6868 no . . C(18) H(33A) 3.1944 no . . C(19) H(14) 3.2812 no . . C(19) H(21A) 3.2088 no . . C(19) H(21B) 3.1723 no . . C(19) H(23B) 2.9600 no . . C(19) H(23D) 3.2582 no . . C(19) H(23F) 3.3942 no . . C(20) H(22) 3.5343 no . . C(21) H(19) 3.4411 no . . C(22) H(5) 3.0924 no . . C(22) H(20A) 3.2808 no . . C(22) H(20B) 3.3168 no . . C(22) H(29B) 3.2608 no . . C(23) H(19) 3.0692 no . . C(24) H(5) 2.9202 no . . C(24) H(26B) 2.7696 no . . C(24) H(27C) 3.3132 no . . C(25) H(5) 3.2507 no . . C(25) H(27C) 3.2605 no . . C(26) H(24A) 2.7321 no . . C(26) H(25A) 3.5968 no . . C(26) H(28B) 2.8584 no . . C(26) H(28D) 3.1388 no . . C(26) H(28F) 3.3371 no . . C(27) H(24A) 3.4116 no . . C(27) H(25A) 3.3368 no . . C(27) H(28B) 3.4228 no . . C(27) H(28D) 3.3557 no . . C(28) H(26A) 2.9867 no . . C(28) H(27A) 3.3658 no . . C(29) H(22) 3.3561 no . . C(30) H(14) 2.9355 no . . C(30) H(32A) 3.0345 no . . C(30) H(33C) 3.3708 no . . C(31) H(14) 3.4055 no . . C(31) H(33C) 3.3701 no . . C(32) H(30B) 2.9936 no . . C(32) H(34A) 3.4939 no . . C(32) H(34B) 2.9742 no . . C(33) H(31A) 3.4916 no . . C(33) H(34B) 3.3250 no . . C(34) H(32B) 2.8577 no . . C(34) H(33A) 3.4119 no . . C(35) H(53) 3.0348 no . . C(36) H(54A) 2.7523 no . . C(36) H(54B) 3.3738 no . . C(36) H(55A) 3.3224 no . . C(36) H(56) 3.4100 no . . C(36) H(57A) 3.2753 no . . C(36) H(57B) 2.8300 no . . C(36) H(57C) 3.3610 no . . C(37) H(39) 2.7770 no . . C(37) H(53) 3.3187 no . . C(37) H(54A) 3.2050 no . . C(37) H(55A) 2.7281 no . . C(37) H(55B) 3.3612 no . . C(38) H(56) 3.0134 no . . C(39) H(56) 3.2413 no . . C(39) H(58A) 2.9890 no . . C(39) H(59C) 3.2307 no . . C(40) H(58A) 2.7772 no . . C(40) H(58B) 3.3696 no . . C(40) H(59C) 3.3209 no . . C(41) H(39) 2.7622 no . . C(41) H(59A) 2.8650 no . . C(41) H(59B) 3.4601 no . . C(41) H(59C) 2.8635 no . . C(41) H(60A) 2.7465 no . . C(41) H(60B) 3.3502 no . . C(41) H(61C) 3.0126 no . . C(42) H(58A) 3.3556 no . . C(42) H(58B) 2.7998 no . . C(42) H(59A) 3.5805 no . . C(42) H(61A) 2.6628 no . . C(42) H(61B) 3.2820 no . . C(42) H(61C) 2.5907 no . . C(42) H(62A) 3.2583 no . . C(42) H(62B) 2.8089 no . . C(42) H(62C) 3.3572 no . . C(42) H(62D) 3.0390 no . . C(42) H(62E) 3.4585 no . . C(42) H(62F) 2.9292 no . . C(43) H(60A) 3.3389 no . . C(43) H(60B) 2.7077 no . . C(43) H(61A) 3.2362 no . . C(44) H(55B) 3.3532 no . . C(44) H(56) 2.7916 no . . C(45) H(53) 3.3106 no . . C(45) H(54B) 3.0357 no . . C(45) H(55A) 3.2031 no . . C(45) H(55B) 2.5497 no . . C(45) H(63A) 3.2190 no . . C(45) H(63B) 2.6750 no . . C(45) H(63C) 3.1085 no . . C(45) H(63D) 2.7853 no . . C(45) H(63E) 3.3112 no . . C(45) H(63F) 2.9080 no . . C(46) H(48) 2.7916 no . . C(46) H(54A) 3.1957 no . . C(46) H(54B) 2.5157 no . . C(46) H(55B) 3.1504 no . . C(46) H(56) 3.3171 no . . C(47) H(53) 2.8474 no . . C(47) H(54B) 3.3521 no . . C(48) H(53) 3.1559 no . . C(48) H(64B) 2.9965 no . . C(48) H(65C) 3.3122 no . . C(49) H(64A) 3.3819 no . . C(49) H(64B) 2.8039 no . . C(49) H(65C) 3.0990 no . . C(50) H(48) 2.7151 no . . C(50) H(65A) 2.6769 no . . C(50) H(65B) 3.3167 no . . C(50) H(65C) 2.6315 no . . C(50) H(66A) 3.1602 no . . C(50) H(66B) 2.5881 no . . C(50) H(67C) 3.3885 no . . C(51) H(64A) 2.6989 no . . C(51) H(64B) 3.2644 no . . C(51) H(65A) 3.1923 no . . C(51) H(67A) 2.7139 no . . C(51) H(67B) 3.3441 no . . C(51) H(67C) 2.7193 no . . C(51) H(68A) 3.2148 no . . C(51) H(68B) 2.6919 no . . C(51) H(68C) 3.2120 no . . C(51) H(68D) 2.8745 no . . C(51) H(68E) 3.3692 no . . C(51) H(68F) 2.8778 no . . C(52) H(66A) 2.8001 no . . C(52) H(66B) 3.3705 no . . C(52) H(67A) 3.0435 no . . C(52) H(67C) 3.5816 no . . C(53) H(48) 3.1955 no . . C(53) H(55A) 3.2952 no . . C(53) H(55B) 3.3135 no . . C(53) H(57B) 3.2961 no . . C(54) H(56) 3.4319 no . . C(55) H(53) 3.5397 no . . C(56) H(39) 3.2157 no . . C(56) H(54A) 3.1877 no . . C(56) H(54B) 3.1693 no . . C(56) H(63B) 2.9247 no . . C(56) H(63D) 3.1764 no . . C(56) H(63F) 3.3989 no . . C(57) H(53) 3.4138 no . . C(58) H(39) 2.9137 no . . C(58) H(60A) 3.0178 no . . C(58) H(61C) 3.2090 no . . C(59) H(39) 3.2924 no . . C(59) H(61C) 3.2116 no . . C(60) H(58B) 2.9548 no . . C(60) H(62B) 2.9064 no . . C(60) H(62D) 3.3666 no . . C(60) H(62F) 3.2005 no . . C(61) H(58B) 3.5098 no . . C(61) H(59A) 3.3839 no . . C(61) H(62B) 3.5107 no . . C(62) H(60B) 2.9108 no . . C(62) H(61A) 3.5659 no . . C(63) H(56) 3.0042 no . . C(64) H(48) 2.9626 no . . C(64) H(66B) 2.6922 no . . C(65) H(48) 3.4853 no . . C(65) H(66B) 3.4384 no . . C(65) H(67C) 3.5337 no . . C(66) H(64A) 2.7884 no . . C(66) H(65A) 3.3788 no . . C(66) H(68B) 2.8322 no . . C(66) H(68D) 3.2025 no . . C(66) H(68F) 3.2368 no . . C(67) H(65A) 3.4316 no . . C(67) H(68B) 3.0850 no . . C(67) H(68D) 3.1369 no . . C(68) H(66A) 3.0826 no . . C(68) H(67A) 3.0243 no . . B(1) H(23A) 3.0066 no . . B(1) H(23C) 3.1931 no . . B(1) H(28A) 2.8194 no . . B(1) H(28C) 3.0010 no . . B(1) H(28E) 2.4679 no . . B(1) H(28F) 3.5670 no . . B(1) H(23E) 2.7044 no . . B(2) H(29A) 3.1825 no . . B(2) H(29C) 2.8932 no . . B(2) H(34A) 3.5070 no . . B(2) H(34C) 2.7524 no . . B(3) H(57A) 3.1393 no . . B(3) H(57C) 2.9623 no . . B(3) H(62A) 3.1559 no . . B(3) H(62C) 2.9602 no . . B(3) H(62E) 2.6409 no . . B(4) H(63A) 2.9559 no . . B(4) H(63C) 3.1902 no . . B(4) H(63E) 2.6812 no . . B(4) H(68A) 2.8845 no . . B(4) H(68C) 2.8990 no . . B(4) H(68E) 2.4438 no . . H(5) H(22) 2.5841 no . . H(5) H(24B) 2.5573 no . . H(5) H(25C) 2.6719 no . . H(14) H(19) 2.8608 no . . H(14) H(30A) 2.4926 no . . H(14) H(31C) 2.8805 no . . H(19) H(20A) 2.4738 no . . H(19) H(20B) 2.4518 no . . H(19) H(23B) 2.4559 no . . H(19) H(23D) 2.8138 no . . H(19) H(23F) 3.0480 no . . H(20A) H(21A) 2.2306 no . . H(20A) H(21B) 2.7597 no . . H(20B) H(21A) 2.7314 no . . H(20B) H(21B) 2.2303 no . . H(20B) H(23F) 3.5514 no . . H(21A) H(22) 2.5106 no . . H(21B) H(22) 2.5033 no . . H(22) H(29B) 2.8016 no . . H(24A) H(25A) 2.3717 no . . H(24A) H(25B) 2.4202 no . . H(24A) H(25C) 2.8828 no . . H(24A) H(26A) 3.5887 no . . H(24A) H(26B) 2.1452 no . . H(24A) H(27C) 3.0414 no . . H(24B) H(25A) 2.8825 no . . H(24B) H(25B) 2.3689 no . . H(24B) H(25C) 2.4232 no . . H(24B) H(26B) 3.4765 no . . H(25A) H(26B) 3.5566 no . . H(25A) H(27C) 2.4742 no . . H(26A) H(27A) 2.3972 no . . H(26A) H(27B) 2.4017 no . . H(26A) H(27C) 2.8893 no . . H(26A) H(28B) 2.3668 no . . H(26A) H(28D) 2.8806 no . . H(26A) H(28F) 2.8219 no . . H(26B) H(27A) 2.8890 no . . H(26B) H(27B) 2.3855 no . . H(26B) H(27C) 2.4137 no . . H(27A) H(28B) 2.9566 no . . H(27A) H(28C) 3.3887 no . . H(27A) H(28D) 2.6946 no . . H(30A) H(31A) 2.8515 no . . H(30A) H(31B) 2.3617 no . . H(30A) H(31C) 2.3376 no . . H(30B) H(31A) 2.3881 no . . H(30B) H(31B) 2.3131 no . . H(30B) H(31C) 2.8497 no . . H(30B) H(32A) 2.4431 no . . H(30B) H(33C) 3.1938 no . . H(31A) H(33C) 2.5982 no . . H(32A) H(33A) 2.8045 no . . H(32A) H(33B) 2.2793 no . . H(32A) H(33C) 2.3151 no . . H(32B) H(33A) 2.2922 no . . H(32B) H(33B) 2.3021 no . . H(32B) H(33C) 2.8051 no . . H(32B) H(34A) 2.9269 no . . H(32B) H(34B) 2.5248 no . . H(33A) H(34B) 2.7449 no . . H(39) H(56) 2.7667 no . . H(39) H(58A) 2.5403 no . . H(39) H(59C) 2.7286 no . . H(48) H(53) 2.7209 no . . H(48) H(64B) 2.5104 no . . H(48) H(65C) 2.9937 no . . H(53) H(54A) 2.5094 no . . H(53) H(54B) 2.4942 no . . H(53) H(57B) 2.8478 no . . H(54A) H(55A) 2.2339 no . . H(54A) H(55B) 2.7415 no . . H(54B) H(55A) 2.7559 no . . H(54B) H(55B) 2.2338 no . . H(55A) H(56) 2.4519 no . . H(55B) H(56) 2.4424 no . . H(56) H(63B) 2.3946 no . . H(56) H(63C) 3.5141 no . . H(56) H(63D) 2.7087 no . . H(56) H(63F) 3.0234 no . . H(58A) H(59A) 2.8594 no . . H(58A) H(59B) 2.3446 no . . H(58A) H(59C) 2.3726 no . . H(58B) H(59A) 2.3716 no . . H(58B) H(59B) 2.3458 no . . H(58B) H(59C) 2.8592 no . . H(58B) H(60A) 2.4205 no . . H(58B) H(61C) 3.0625 no . . H(59A) H(61C) 2.4568 no . . H(60A) H(61A) 2.8245 no . . H(60A) H(61B) 2.2934 no . . H(60A) H(61C) 2.3558 no . . H(60B) H(61A) 2.3014 no . . H(60B) H(61B) 2.3472 no . . H(60B) H(61C) 2.8251 no . . H(60B) H(62A) 3.3877 no . . H(60B) H(62B) 2.3227 no . . H(60B) H(62D) 2.9802 no . . H(60B) H(62F) 2.5869 no . . H(61A) H(62B) 3.0714 no . . H(61A) H(62D) 3.0854 no . . H(64A) H(65A) 2.3683 no . . H(64A) H(65B) 2.3969 no . . H(64A) H(65C) 2.8730 no . . H(64A) H(66A) 3.4786 no . . H(64A) H(66B) 2.1085 no . . H(64B) H(65A) 2.8726 no . . H(64B) H(65B) 2.3640 no . . H(64B) H(65C) 2.4012 no . . H(64B) H(66B) 3.5240 no . . H(65A) H(66B) 3.0900 no . . H(65A) H(67C) 2.6850 no . . H(66A) H(67A) 2.4156 no . . H(66A) H(67B) 2.4010 no . . H(66A) H(67C) 2.8962 no . . H(66A) H(68A) 3.5872 no . . H(66A) H(68B) 2.5033 no . . H(66A) H(68D) 3.1231 no . . H(66A) H(68F) 2.7970 no . . H(66B) H(67A) 2.8962 no . . H(66B) H(67B) 2.4049 no . . H(66B) H(67C) 2.4115 no . . H(67A) H(68B) 2.4740 no . . H(67A) H(68C) 3.1679 no . . H(67A) H(68D) 2.3668 no . . H(67A) H(68F) 3.3276 no . . F(1) H(31C) 3.4771 no . 2_656 F(1) H(33B) 3.3216 no . 4_555 F(1) H(66B) 3.2926 no . 4_565 F(2) H(14) 2.5450 no . 2_656 F(2) H(19) 2.5790 no . 2_656 F(2) H(20A) 3.5845 no . 2_656 F(2) H(30A) 3.5898 no . 2_656 F(2) H(31C) 2.8628 no . 2_656 F(3) H(48) 2.7613 no . . F(3) H(53) 2.5295 no . . F(3) H(57B) 2.4599 no . . F(3) H(57C) 3.5552 no . . F(3) H(60A) 2.8394 no . 1_565 F(3) H(60B) 3.3953 no . 1_565 F(4) H(26A) 3.1218 no . 4_564 F(4) H(28B) 2.4937 no . 4_564 F(4) H(48) 3.3750 no . . F(4) H(64B) 3.0159 no . . F(4) H(28D) 2.9829 no . 4_564 F(4) H(28F) 2.9633 no . 4_564 F(5) H(5) 3.5787 no . 1_545 F(5) H(24B) 2.5986 no . 1_545 F(5) H(68A) 3.5359 no . 4_555 F(5) H(68B) 2.8409 no . 4_555 F(5) H(68D) 3.3822 no . 4_555 F(5) H(68F) 2.9332 no . 4_555 F(6) H(5) 3.3343 no . 1_545 F(6) H(22) 3.2307 no . 1_545 F(6) H(24B) 3.5689 no . 1_545 F(6) H(29B) 2.5256 no . 1_545 F(6) H(30B) 2.9024 no . . F(6) H(32A) 2.5098 no . . F(6) H(32B) 3.2905 no . . F(7) H(26B) 3.3859 no . 4_564 F(7) H(59B) 3.3507 no . 2_555 F(7) H(59C) 3.3257 no . 2_555 F(8) H(39) 2.6517 no . 2_555 F(8) H(56) 2.3943 no . 2_555 F(8) H(59C) 2.9836 no . 2_555 F(8) H(63B) 3.2895 no . 2_555 N(2) H(19) 3.4793 no . 2_656 N(2) H(20B) 3.5284 no . 2_656 N(2) H(66A) 3.1631 no . 4_565 N(2) H(66B) 3.5247 no . 4_565 N(4) H(57B) 2.9814 no . . N(4) H(57C) 2.8150 no . . N(5) H(34A) 3.5755 no . . N(6) H(29B) 3.0636 no . 1_545 N(6) H(29C) 3.2015 no . 1_545 N(8) H(26A) 3.4806 no . 4_564 N(8) H(26B) 3.5121 no . 4_564 N(8) H(63B) 3.5709 no . 2_555 C(3) H(62A) 3.1504 no . 1_565 C(3) H(62E) 3.5788 no . 1_565 C(3) H(62F) 3.4124 no . 1_565 C(4) H(23B) 3.3537 no . 2_656 C(4) H(62A) 3.3064 no . 1_565 C(4) H(62E) 3.4020 no . 1_565 C(4) H(23F) 3.5597 no . 2_656 C(5) H(23B) 3.2581 no . 2_656 C(5) H(62A) 3.3065 no . 1_565 C(5) H(62C) 3.3856 no . 1_565 C(5) H(66A) 3.5822 no . 4_565 C(5) H(62E) 3.0312 no . 1_565 C(5) H(23F) 3.1355 no . 2_656 C(6) H(20B) 3.5137 no . 2_656 C(6) H(66A) 3.0848 no . 4_565 C(6) H(23F) 3.5281 no . 2_656 C(7) H(20B) 3.3133 no . 2_656 C(7) H(66A) 3.2273 no . 4_565 C(7) H(68F) 3.3546 no . 4_565 C(8) H(20B) 3.1777 no . 2_656 C(8) H(66A) 3.2786 no . 4_565 C(9) H(20A) 3.2694 no . 2_656 C(9) H(20B) 3.2872 no . 2_656 C(9) H(66A) 3.2363 no . 4_565 C(9) H(66B) 3.4551 no . 4_565 C(10) H(62A) 3.0673 no . 1_565 C(10) H(62F) 3.0553 no . 1_565 C(11) H(62A) 2.9458 no . 1_565 C(11) H(62F) 3.0306 no . 1_565 C(14) H(25B) 3.1234 no . 1_545 C(14) H(57C) 3.4448 no . . C(15) H(57B) 3.4276 no . . C(15) H(57C) 2.7336 no . . C(16) H(57C) 2.8799 no . . C(17) H(57C) 3.0184 no . . C(18) H(27B) 3.4057 no . 4_564 C(18) H(57B) 3.4114 no . . C(18) H(57C) 2.9890 no . . C(20) H(27A) 3.0906 no . 2_646 C(20) H(27C) 3.3849 no . 2_646 C(20) H(28C) 3.4851 no . 2_646 C(20) H(28D) 3.5851 no . 2_646 C(21) H(27A) 3.4733 no . 2_646 C(21) H(31B) 3.4281 no . 1_565 C(22) H(30B) 3.2751 no . 1_565 C(22) H(62A) 3.0546 no . 1_565 C(22) H(62F) 3.4698 no . 1_565 C(23) H(21B) 3.4377 no . 2_646 C(23) H(25C) 3.3002 no . 2_646 C(23) H(30A) 3.5031 no . 2_656 C(23) H(31B) 3.2660 no . 2_656 C(24) H(57A) 3.5719 no . 1_565 C(24) H(68A) 3.5340 no . 4_565 C(24) H(68F) 3.1651 no . 4_565 C(25) H(14) 3.4413 no . 1_565 C(25) H(20B) 3.4624 no . 2_656 C(25) H(30A) 3.4057 no . 1_565 C(25) H(23F) 3.3844 no . 2_656 C(26) H(34B) 3.5239 no . 4_565 C(26) H(34C) 3.2737 no . 4_565 C(27) H(20A) 3.4983 no . 2_656 C(27) H(20B) 3.1154 no . 2_656 C(27) H(33A) 3.3701 no . 4_565 C(27) H(34B) 3.1310 no . 4_565 C(27) H(34C) 3.3866 no . 4_565 C(28) H(20A) 3.2917 no . 2_656 C(28) H(64A) 3.3297 no . 4_565 C(29) H(32A) 3.1923 no . 1_565 C(29) H(62A) 3.1388 no . 1_565 C(29) H(64B) 3.0351 no . . C(29) H(62F) 3.3504 no . 1_565 C(30) H(22) 3.2313 no . 1_545 C(30) H(23A) 3.2664 no . 2_646 C(31) H(23A) 3.1284 no . 2_646 C(31) H(33C) 3.3915 no . 3_656 C(31) H(23E) 3.0889 no . 2_646 C(32) H(29B) 3.4238 no . 1_545 C(33) H(27B) 3.5266 no . 4_564 C(34) H(26A) 3.3034 no . 4_564 C(34) H(27B) 2.9033 no . 4_564 C(35) H(34A) 2.9744 no . . C(36) H(34A) 2.6143 no . . C(37) H(34A) 3.1341 no . . C(38) H(65B) 3.3811 no . 1_545 C(39) H(65B) 2.9315 no . 1_545 C(39) H(65C) 3.1999 no . 1_545 C(40) H(29C) 3.3700 no . 1_545 C(40) H(65B) 3.3369 no . 1_545 C(40) H(65C) 3.5270 no . 1_545 C(41) H(29C) 3.2480 no . 1_545 C(42) H(29C) 2.9655 no . 1_545 C(43) H(29B) 3.0877 no . 1_545 C(43) H(29C) 2.9437 no . 1_545 C(45) H(34A) 3.3217 no . . C(46) H(34A) 2.8106 no . . C(46) H(34C) 3.4862 no . . C(46) H(58B) 3.4628 no . 1_565 C(47) H(34A) 3.1362 no . . C(47) H(34C) 3.1893 no . . C(47) H(63B) 3.5849 no . 2_555 C(48) H(34C) 3.1019 no . . C(48) H(58A) 3.3261 no . 1_565 C(48) H(58B) 3.3760 no . 1_565 C(48) H(63B) 3.4834 no . 2_555 C(48) H(63F) 3.3523 no . 2_555 C(49) H(26A) 3.2972 no . 4_564 C(49) H(63B) 3.4763 no . 2_555 C(49) H(63F) 3.3308 no . 2_555 C(50) H(26A) 3.3676 no . 4_564 C(50) H(28F) 3.2633 no . 4_564 C(51) H(26A) 3.4971 no . 4_564 C(52) H(26A) 3.5410 no . 4_564 C(52) H(26B) 3.4103 no . 4_564 C(52) H(55B) 3.5340 no . 2_555 C(53) H(34A) 3.0373 no . . C(53) H(58B) 2.9678 no . 1_565 C(53) H(60A) 3.0783 no . 1_565 C(54) H(58B) 3.0933 no . 1_565 C(55) H(67A) 3.2041 no . 2_545 C(55) H(67C) 3.5982 no . 2_545 C(55) H(68C) 3.3376 no . 2_545 C(55) H(68D) 3.2996 no . 2_545 C(57) H(24B) 3.5208 no . 1_545 C(57) H(60A) 3.5864 no . 1_565 C(58) H(48) 3.2068 no . 1_545 C(58) H(53) 3.3110 no . 1_545 C(58) H(54B) 3.3131 no . 1_545 C(58) H(63A) 3.1093 no . 2_545 C(58) H(63E) 3.3274 no . 2_545 C(58) H(63F) 3.5693 no . 2_545 C(58) H(65C) 3.3312 no . 1_545 C(59) H(54B) 3.2977 no . 1_545 C(59) H(61B) 3.1151 no . 3_546 C(59) H(63A) 3.1075 no . 2_545 C(59) H(63C) 3.4817 no . 2_545 C(59) H(63E) 2.9036 no . 2_545 C(60) H(53) 3.1926 no . 1_545 C(60) H(57B) 3.3500 no . 1_545 C(61) H(59A) 3.0462 no . 3_546 C(62) H(29B) 3.3179 no . 1_545 C(62) H(29C) 3.5906 no . 1_545 C(62) H(66A) 3.4500 no . 4_555 C(62) H(67A) 3.4229 no . 4_555 C(62) H(67B) 3.0635 no . 4_555 C(63) H(58A) 3.2132 no . 2_555 C(63) H(59B) 3.1000 no . 2_555 C(64) H(28A) 3.3860 no . 4_564 C(64) H(28B) 3.5703 no . 4_564 C(64) H(29A) 3.3091 no . . C(64) H(28F) 2.9338 no . 4_564 C(65) H(39) 3.2653 no . 1_565 C(65) H(58A) 3.3206 no . 1_565 C(66) H(62C) 3.3390 no . 4_554 C(66) H(62D) 3.1581 no . 4_554 C(67) H(55B) 3.0586 no . 2_555 C(67) H(61A) 3.2050 no . 4_554 C(67) H(62B) 3.2084 no . 4_554 C(67) H(62C) 3.1462 no . 4_554 C(67) H(62D) 2.6302 no . 4_554 C(68) H(55A) 3.4512 no . 2_555 B(1) H(19) 3.4542 no . 2_656 B(2) H(57B) 3.0877 no . . B(3) H(29B) 3.3116 no . 1_545 B(4) H(56) 3.4968 no . 2_555 H(5) F(5) 3.5787 no . 1_565 H(5) F(6) 3.3343 no . 1_565 H(5) H(23B) 3.4234 no . 2_656 H(5) H(30A) 3.0946 no . 1_565 H(5) H(30B) 3.3110 no . 1_565 H(5) H(62A) 3.0636 no . 1_565 H(5) H(62C) 3.2496 no . 1_565 H(5) H(62E) 2.7293 no . 1_565 H(5) H(23F) 3.0742 no . 2_656 H(14) F(2) 2.5450 no . 2_646 H(14) C(25) 3.4413 no . 1_545 H(14) H(25B) 2.7818 no . 1_545 H(14) H(25C) 3.2480 no . 1_545 H(19) F(2) 2.5790 no . 2_646 H(19) N(2) 3.4793 no . 2_646 H(19) B(1) 3.4542 no . 2_646 H(20A) F(2) 3.5845 no . 2_646 H(20A) C(9) 3.2694 no . 2_646 H(20A) C(27) 3.4983 no . 2_646 H(20A) C(28) 3.2917 no . 2_646 H(20A) H(27A) 2.7411 no . 2_646 H(20A) H(27C) 3.4878 no . 2_646 H(20A) H(28B) 3.5788 no . 2_646 H(20A) H(28C) 2.6350 no . 2_646 H(20A) H(28D) 2.7298 no . 2_646 H(20A) H(28E) 3.4338 no . 2_646 H(20B) N(2) 3.5284 no . 2_646 H(20B) C(6) 3.5137 no . 2_646 H(20B) C(7) 3.3133 no . 2_646 H(20B) C(8) 3.1777 no . 2_646 H(20B) C(9) 3.2872 no . 2_646 H(20B) C(25) 3.4624 no . 2_646 H(20B) C(27) 3.1154 no . 2_646 H(20B) H(25A) 2.8325 no . 2_646 H(20B) H(25C) 3.3385 no . 2_646 H(20B) H(27A) 2.7723 no . 2_646 H(20B) H(27C) 2.6911 no . 2_646 H(20B) H(28D) 3.5943 no . 2_646 H(21A) H(27A) 3.2751 no . 2_646 H(21A) H(30B) 3.5808 no . 1_565 H(21A) H(31B) 3.1667 no . 1_565 H(21B) C(23) 3.4377 no . 2_656 H(21B) H(23A) 3.5147 no . 2_656 H(21B) H(23B) 3.1677 no . 2_656 H(21B) H(23C) 3.0782 no . 2_656 H(21B) H(27A) 3.3755 no . 2_646 H(21B) H(27C) 3.1702 no . 2_646 H(21B) H(31B) 2.8919 no . 1_565 H(21B) H(23D) 2.9813 no . 2_656 H(21B) H(23E) 3.3478 no . 2_656 H(21B) H(23F) 3.4301 no . 2_656 H(22) F(6) 3.2307 no . 1_565 H(22) C(30) 3.2313 no . 1_565 H(22) H(30A) 3.3324 no . 1_565 H(22) H(30B) 2.3650 no . 1_565 H(22) H(31B) 3.4827 no . 1_565 H(22) H(32A) 3.5774 no . 1_565 H(22) H(62A) 2.8317 no . 1_565 H(22) H(62E) 3.2191 no . 1_565 H(22) H(62F) 3.4758 no . 1_565 H(23A) C(30) 3.2664 no . 2_656 H(23A) C(31) 3.1284 no . 2_656 H(23A) H(21B) 3.5147 no . 2_646 H(23A) H(25C) 2.7141 no . 2_646 H(23A) H(30A) 2.5766 no . 2_656 H(23A) H(31B) 2.6893 no . 2_656 H(23A) H(31C) 3.0487 no . 2_656 H(23B) C(4) 3.3537 no . 2_646 H(23B) C(5) 3.2581 no . 2_646 H(23B) H(5) 3.4234 no . 2_646 H(23B) H(21B) 3.1677 no . 2_646 H(23B) H(25C) 3.2227 no . 2_646 H(23C) H(21B) 3.0782 no . 2_646 H(23C) H(31B) 2.9990 no . 2_656 H(24A) H(57A) 3.4427 no . 1_565 H(24A) H(68A) 2.9782 no . 4_565 H(24A) H(68F) 2.8610 no . 4_565 H(24B) F(5) 2.5986 no . 1_565 H(24B) F(6) 3.5689 no . 1_565 H(24B) C(57) 3.5208 no . 1_565 H(24B) H(57A) 2.9198 no . 1_565 H(24B) H(57C) 3.2135 no . 1_565 H(24B) H(68A) 3.3875 no . 4_565 H(24B) H(68B) 3.4426 no . 4_565 H(24B) H(68F) 2.8947 no . 4_565 H(25A) H(20B) 2.8325 no . 2_656 H(25A) H(23D) 3.2115 no . 1_565 H(25B) C(14) 3.1234 no . 1_565 H(25B) H(14) 2.7818 no . 1_565 H(25B) H(30A) 3.2497 no . 1_565 H(25B) H(57A) 3.5922 no . 1_565 H(25B) H(57C) 3.4103 no . 1_565 H(25C) C(23) 3.3002 no . 2_656 H(25C) H(14) 3.2480 no . 1_565 H(25C) H(20B) 3.3385 no . 2_656 H(25C) H(23A) 2.7141 no . 2_656 H(25C) H(23B) 3.2227 no . 2_656 H(25C) H(30A) 2.7285 no . 1_565 H(25C) H(23F) 2.4404 no . 2_656 H(26A) F(4) 3.1218 no . 4_565 H(26A) N(8) 3.4806 no . 4_565 H(26A) C(34) 3.3034 no . 4_565 H(26A) C(49) 3.2972 no . 4_565 H(26A) C(50) 3.3676 no . 4_565 H(26A) C(51) 3.4971 no . 4_565 H(26A) C(52) 3.5410 no . 4_565 H(26A) H(34B) 3.2176 no . 4_565 H(26A) H(34C) 2.5577 no . 4_565 H(26B) F(7) 3.3859 no . 4_565 H(26B) N(8) 3.5121 no . 4_565 H(26B) C(52) 3.4103 no . 4_565 H(26B) H(34B) 3.5603 no . 4_565 H(26B) H(34C) 3.5261 no . 4_565 H(26B) H(68A) 3.0306 no . 4_565 H(26B) H(68F) 3.1470 no . 4_565 H(27A) C(20) 3.0906 no . 2_656 H(27A) C(21) 3.4733 no . 2_656 H(27A) H(20A) 2.7411 no . 2_656 H(27A) H(20B) 2.7723 no . 2_656 H(27A) H(21A) 3.2751 no . 2_656 H(27A) H(21B) 3.3755 no . 2_656 H(27A) H(33A) 3.5308 no . 4_565 H(27A) H(34B) 3.4974 no . 4_565 H(27A) H(34C) 3.5281 no . 4_565 H(27B) C(18) 3.4057 no . 4_565 H(27B) C(33) 3.5266 no . 4_565 H(27B) C(34) 2.9033 no . 4_565 H(27B) H(33A) 2.5732 no . 4_565 H(27B) H(34B) 2.2659 no . 4_565 H(27B) H(34C) 2.8780 no . 4_565 H(27C) C(20) 3.3849 no . 2_656 H(27C) H(20A) 3.4878 no . 2_656 H(27C) H(20B) 2.6911 no . 2_656 H(27C) H(21B) 3.1702 no . 2_656 H(27C) H(33A) 3.5804 no . 4_565 H(28A) C(64) 3.3860 no . 4_565 H(28A) H(29A) 3.5068 no . 4_565 H(28A) H(33B) 3.0820 no . 4_555 H(28A) H(64A) 2.6528 no . 4_565 H(28A) H(64B) 3.4013 no . 4_565 H(28A) H(66B) 3.1099 no . 4_565 H(28B) F(4) 2.4937 no . 4_565 H(28B) C(64) 3.5703 no . 4_565 H(28B) H(20A) 3.5788 no . 2_656 H(28B) H(29A) 3.4081 no . 4_565 H(28B) H(64A) 3.2370 no . 4_565 H(28B) H(64B) 3.2864 no . 4_565 H(28C) C(20) 3.4851 no . 2_656 H(28C) H(20A) 2.6350 no . 2_656 H(29A) C(64) 3.3091 no . . H(29A) H(28A) 3.5068 no . 4_564 H(29A) H(28B) 3.4081 no . 4_564 H(29A) H(32A) 3.0080 no . 1_565 H(29A) H(33B) 3.3340 no . 1_565 H(29A) H(64A) 3.2677 no . . H(29A) H(64B) 2.5227 no . . H(29A) H(28F) 3.2082 no . 4_564 H(29B) F(6) 2.5256 no . 1_565 H(29B) N(6) 3.0636 no . 1_565 H(29B) C(32) 3.4238 no . 1_565 H(29B) C(43) 3.0877 no . 1_565 H(29B) C(62) 3.3179 no . 1_565 H(29B) B(3) 3.3116 no . 1_565 H(29B) H(30B) 3.5553 no . 1_565 H(29B) H(32A) 2.5097 no . 1_565 H(29B) H(32B) 3.5638 no . 1_565 H(29B) H(62A) 2.6664 no . 1_565 H(29B) H(64B) 3.5679 no . . H(29B) H(62E) 3.1777 no . 1_565 H(29B) H(62F) 3.1302 no . 1_565 H(29C) N(6) 3.2015 no . 1_565 H(29C) C(40) 3.3700 no . 1_565 H(29C) C(41) 3.2480 no . 1_565 H(29C) C(42) 2.9655 no . 1_565 H(29C) C(43) 2.9437 no . 1_565 H(29C) C(62) 3.5906 no . 1_565 H(29C) H(48) 3.5800 no . . H(29C) H(62A) 3.2432 no . 1_565 H(29C) H(64B) 2.6899 no . . H(29C) H(62F) 3.2819 no . 1_565 H(30A) F(2) 3.5898 no . 2_646 H(30A) C(23) 3.5031 no . 2_646 H(30A) C(25) 3.4057 no . 1_545 H(30A) H(5) 3.0946 no . 1_545 H(30A) H(22) 3.3324 no . 1_545 H(30A) H(23A) 2.5766 no . 2_646 H(30A) H(25B) 3.2497 no . 1_545 H(30A) H(25C) 2.7285 no . 1_545 H(30A) H(23E) 3.1406 no . 2_646 H(30A) H(23F) 2.9521 no . 2_646 H(30B) F(6) 2.9024 no . . H(30B) C(22) 3.2751 no . 1_545 H(30B) H(5) 3.3110 no . 1_545 H(30B) H(21A) 3.5808 no . 1_545 H(30B) H(22) 2.3650 no . 1_545 H(30B) H(29B) 3.5553 no . 1_545 H(31A) H(31A) 2.8194 no . 3_656 H(31A) H(33C) 3.0310 no . 3_656 H(31B) C(21) 3.4281 no . 1_545 H(31B) C(23) 3.2660 no . 2_646 H(31B) H(21A) 3.1667 no . 1_545 H(31B) H(21B) 2.8919 no . 1_545 H(31B) H(22) 3.4827 no . 1_545 H(31B) H(23A) 2.6893 no . 2_646 H(31B) H(23C) 2.9990 no . 2_646 H(31B) H(33C) 3.2102 no . 3_656 H(31B) H(23D) 3.5745 no . 2_646 H(31B) H(23E) 2.4944 no . 2_646 H(31B) H(23F) 3.3187 no . 2_646 H(31C) F(1) 3.4771 no . 2_646 H(31C) F(2) 2.8628 no . 2_646 H(31C) H(23A) 3.0487 no . 2_646 H(31C) H(33C) 3.3744 no . 3_656 H(31C) H(28E) 3.5914 no . 2_646 H(31C) H(23E) 2.9590 no . 2_646 H(32A) F(6) 2.5098 no . . H(32A) C(29) 3.1923 no . 1_545 H(32A) H(22) 3.5774 no . 1_545 H(32A) H(29A) 3.0080 no . 1_545 H(32A) H(29B) 2.5097 no . 1_545 H(32B) F(6) 3.2905 no . . H(32B) H(29B) 3.5638 no . 1_545 H(32B) H(65B) 2.9530 no . 1_545 H(33A) C(27) 3.3701 no . 4_564 H(33A) H(27A) 3.5308 no . 4_564 H(33A) H(27B) 2.5732 no . 4_564 H(33A) H(27C) 3.5804 no . 4_564 H(33B) F(1) 3.3216 no . 4_554 H(33B) H(28A) 3.0820 no . 4_554 H(33B) H(29A) 3.3340 no . 1_545 H(33B) H(64A) 3.1658 no . 1_545 H(33B) H(28E) 3.4212 no . 4_554 H(33C) C(31) 3.3915 no . 3_656 H(33C) H(31A) 3.0310 no . 3_656 H(33C) H(31B) 3.2102 no . 3_656 H(33C) H(31C) 3.3744 no . 3_656 H(34A) N(5) 3.5755 no . . H(34A) C(35) 2.9744 no . . H(34A) C(36) 2.6143 no . . H(34A) C(37) 3.1341 no . . H(34A) C(45) 3.3217 no . . H(34A) C(46) 2.8106 no . . H(34A) C(47) 3.1362 no . . H(34A) C(53) 3.0373 no . . H(34A) H(53) 3.2599 no . . H(34A) H(57B) 3.5878 no . . H(34B) C(26) 3.5239 no . 4_564 H(34B) C(27) 3.1310 no . 4_564 H(34B) H(26A) 3.2176 no . 4_564 H(34B) H(26B) 3.5603 no . 4_564 H(34B) H(27A) 3.4974 no . 4_564 H(34B) H(27B) 2.2659 no . 4_564 H(34C) C(26) 3.2737 no . 4_564 H(34C) C(27) 3.3866 no . 4_564 H(34C) C(46) 3.4862 no . . H(34C) C(47) 3.1893 no . . H(34C) C(48) 3.1019 no . . H(34C) H(26A) 2.5577 no . 4_564 H(34C) H(26B) 3.5261 no . 4_564 H(34C) H(27A) 3.5281 no . 4_564 H(34C) H(27B) 2.8780 no . 4_564 H(34C) H(48) 3.1844 no . . H(39) F(8) 2.6517 no . 2_545 H(39) C(65) 3.2653 no . 1_545 H(39) H(63A) 3.4685 no . 2_545 H(39) H(65B) 2.9125 no . 1_545 H(39) H(65C) 2.7772 no . 1_545 H(48) F(3) 2.7613 no . . H(48) F(4) 3.3750 no . . H(48) C(58) 3.2068 no . 1_565 H(48) H(29C) 3.5800 no . . H(48) H(34C) 3.1844 no . . H(48) H(58A) 2.7975 no . 1_565 H(48) H(58B) 2.7670 no . 1_565 H(48) H(63F) 3.5835 no . 2_555 H(53) F(3) 2.5295 no . . H(53) C(58) 3.3110 no . 1_565 H(53) C(60) 3.1926 no . 1_565 H(53) H(34A) 3.2599 no . . H(53) H(58B) 2.3421 no . 1_565 H(53) H(60A) 2.2069 no . 1_565 H(54A) H(58B) 3.2892 no . 1_565 H(54A) H(60A) 3.3521 no . 1_565 H(54A) H(61A) 3.5042 no . 3_556 H(54A) H(61B) 3.5500 no . 1_565 H(54A) H(61C) 3.2840 no . 3_556 H(54B) C(58) 3.3131 no . 1_565 H(54B) C(59) 3.2977 no . 1_565 H(54B) H(58B) 2.5594 no . 1_565 H(54B) H(59A) 3.2986 no . 1_565 H(54B) H(59B) 2.8358 no . 1_565 H(54B) H(61A) 3.4685 no . 3_556 H(55A) C(68) 3.4512 no . 2_545 H(55A) H(67A) 2.9955 no . 2_545 H(55A) H(68B) 3.5177 no . 2_545 H(55A) H(68C) 2.7060 no . 2_545 H(55A) H(68D) 2.6508 no . 2_545 H(55B) C(52) 3.5340 no . 2_545 H(55B) C(67) 3.0586 no . 2_545 H(55B) H(67A) 2.5659 no . 2_545 H(55B) H(67C) 2.6922 no . 2_545 H(55B) H(68C) 3.2755 no . 2_545 H(55B) H(68D) 3.0966 no . 2_545 H(56) F(8) 2.3943 no . 2_545 H(56) B(4) 3.4968 no . 2_545 H(56) H(68C) 3.2538 no . 2_545 H(57A) C(24) 3.5719 no . 1_545 H(57A) H(24A) 3.4427 no . 1_545 H(57A) H(24B) 2.9198 no . 1_545 H(57A) H(25B) 3.5922 no . 1_545 H(57B) F(3) 2.4599 no . . H(57B) N(4) 2.9814 no . . H(57B) C(15) 3.4276 no . . H(57B) C(18) 3.4114 no . . H(57B) C(60) 3.3500 no . 1_565 H(57B) B(2) 3.0877 no . . H(57B) H(34A) 3.5878 no . . H(57B) H(60A) 2.7823 no . 1_565 H(57B) H(60B) 2.9994 no . 1_565 H(57C) F(3) 3.5552 no . . H(57C) N(4) 2.8150 no . . H(57C) C(14) 3.4448 no . . H(57C) C(15) 2.7336 no . . H(57C) C(16) 2.8799 no . . H(57C) C(17) 3.0184 no . . H(57C) C(18) 2.9890 no . . H(57C) H(24B) 3.2135 no . 1_545 H(57C) H(25B) 3.4103 no . 1_545 H(58A) C(48) 3.3261 no . 1_545 H(58A) C(63) 3.2132 no . 2_545 H(58A) C(65) 3.3206 no . 1_545 H(58A) H(48) 2.7975 no . 1_545 H(58A) H(63A) 2.3616 no . 2_545 H(58A) H(63B) 3.4300 no . 2_545 H(58A) H(63C) 3.4797 no . 2_545 H(58A) H(63E) 2.8052 no . 2_545 H(58A) H(63F) 2.7433 no . 2_545 H(58A) H(65B) 3.5294 no . 1_545 H(58A) H(65C) 2.4197 no . 1_545 H(58B) C(46) 3.4628 no . 1_545 H(58B) C(48) 3.3760 no . 1_545 H(58B) C(53) 2.9678 no . 1_545 H(58B) C(54) 3.0933 no . 1_545 H(58B) H(48) 2.7670 no . 1_545 H(58B) H(53) 2.3421 no . 1_545 H(58B) H(54A) 3.2892 no . 1_545 H(58B) H(54B) 2.5594 no . 1_545 H(58B) H(63A) 3.5103 no . 2_545 H(59A) C(61) 3.0462 no . 3_546 H(59A) H(54B) 3.2986 no . 1_545 H(59A) H(61A) 3.3532 no . 3_546 H(59A) H(61B) 2.4336 no . 3_546 H(59A) H(61C) 2.9242 no . 3_546 H(59B) F(7) 3.3507 no . 2_545 H(59B) C(63) 3.1000 no . 2_545 H(59B) H(54B) 2.8358 no . 1_545 H(59B) H(61A) 3.5336 no . 3_546 H(59B) H(61B) 3.0507 no . 3_546 H(59B) H(63A) 2.6741 no . 2_545 H(59B) H(63C) 2.6620 no . 2_545 H(59B) H(63D) 3.3316 no . 2_545 H(59B) H(63E) 2.2611 no . 2_545 H(59B) H(63F) 3.3412 no . 2_545 H(59C) F(7) 3.3257 no . 2_545 H(59C) F(8) 2.9836 no . 2_545 H(59C) H(61B) 3.4463 no . 3_546 H(59C) H(63A) 3.1171 no . 2_545 H(59C) H(63E) 2.9284 no . 2_545 H(59C) H(68E) 3.4246 no . 2_545 H(60A) F(3) 2.8394 no . 1_545 H(60A) C(53) 3.0783 no . 1_545 H(60A) C(57) 3.5864 no . 1_545 H(60A) H(53) 2.2069 no . 1_545 H(60A) H(54A) 3.3521 no . 1_545 H(60A) H(57B) 2.7823 no . 1_545 H(60B) F(3) 3.3953 no . 1_545 H(60B) H(57B) 2.9994 no . 1_545 H(61A) C(67) 3.2050 no . 4_555 H(61A) H(54A) 3.5042 no . 3_556 H(61A) H(54B) 3.4685 no . 3_556 H(61A) H(59A) 3.3532 no . 3_546 H(61A) H(59B) 3.5336 no . 3_546 H(61A) H(67A) 2.9235 no . 4_555 H(61A) H(67B) 2.7922 no . 4_555 H(61A) H(67C) 3.4012 no . 4_555 H(61B) C(59) 3.1151 no . 3_546 H(61B) H(54A) 3.5500 no . 1_545 H(61B) H(59A) 2.4336 no . 3_546 H(61B) H(59B) 3.0507 no . 3_546 H(61B) H(59C) 3.4463 no . 3_546 H(61C) H(54A) 3.2840 no . 3_556 H(61C) H(59A) 2.9242 no . 3_546 H(61C) H(61C) 3.1006 no . 3_546 H(62A) C(3) 3.1504 no . 1_545 H(62A) C(4) 3.3064 no . 1_545 H(62A) C(5) 3.3065 no . 1_545 H(62A) C(10) 3.0673 no . 1_545 H(62A) C(11) 2.9458 no . 1_545 H(62A) C(22) 3.0546 no . 1_545 H(62A) C(29) 3.1388 no . 1_545 H(62A) H(5) 3.0636 no . 1_545 H(62A) H(22) 2.8317 no . 1_545 H(62A) H(29B) 2.6664 no . 1_545 H(62A) H(29C) 3.2432 no . 1_545 H(62B) C(67) 3.2084 no . 4_555 H(62B) H(66A) 3.4127 no . 4_555 H(62B) H(67A) 3.2259 no . 4_555 H(62B) H(67B) 2.4627 no . 4_555 H(62C) C(5) 3.3856 no . 1_545 H(62C) C(66) 3.3390 no . 4_555 H(62C) C(67) 3.1462 no . 4_555 H(62C) H(5) 3.2496 no . 1_545 H(62C) H(66A) 2.6593 no . 4_555 H(62C) H(67A) 2.9025 no . 4_555 H(62C) H(67B) 2.8341 no . 4_555 H(62C) H(68B) 2.9765 no . 4_555 H(62C) H(68D) 3.5431 no . 4_555 H(62C) H(68F) 3.4912 no . 4_555 H(63A) C(58) 3.1093 no . 2_555 H(63A) C(59) 3.1075 no . 2_555 H(63A) H(39) 3.4685 no . 2_555 H(63A) H(58A) 2.3616 no . 2_555 H(63A) H(58B) 3.5103 no . 2_555 H(63A) H(59B) 2.6741 no . 2_555 H(63A) H(59C) 3.1171 no . 2_555 H(63A) H(65C) 2.9079 no . 2_545 H(63B) F(8) 3.2895 no . 2_545 H(63B) N(8) 3.5709 no . 2_545 H(63B) C(47) 3.5849 no . 2_545 H(63B) C(48) 3.4834 no . 2_545 H(63B) C(49) 3.4763 no . 2_545 H(63B) H(58A) 3.4300 no . 2_555 H(63C) C(59) 3.4817 no . 2_555 H(63C) H(58A) 3.4797 no . 2_555 H(63C) H(59B) 2.6620 no . 2_555 H(63D) H(59B) 3.3316 no . 2_555 H(63E) C(58) 3.3274 no . 2_555 H(63E) C(59) 2.9036 no . 2_555 H(63E) H(58A) 2.8052 no . 2_555 H(63E) H(59B) 2.2611 no . 2_555 H(63E) H(59C) 2.9284 no . 2_555 H(63F) C(48) 3.3523 no . 2_545 H(63F) C(49) 3.3308 no . 2_545 H(63F) C(58) 3.5693 no . 2_555 H(63F) H(48) 3.5835 no . 2_545 H(63F) H(58A) 2.7433 no . 2_555 H(63F) H(59B) 3.3412 no . 2_555 H(63F) H(65C) 2.8126 no . 2_545 H(64A) C(28) 3.3297 no . 4_564 H(64A) H(28A) 2.6528 no . 4_564 H(64A) H(28B) 3.2370 no . 4_564 H(64A) H(29A) 3.2677 no . . H(64A) H(33B) 3.1658 no . 1_565 H(64A) H(28E) 3.5667 no . 4_564 H(64A) H(28F) 2.4322 no . 4_564 H(64B) F(4) 3.0159 no . . H(64B) C(29) 3.0351 no . . H(64B) H(28A) 3.4013 no . 4_564 H(64B) H(28B) 3.2864 no . 4_564 H(64B) H(29A) 2.5227 no . . H(64B) H(29B) 3.5679 no . . H(64B) H(29C) 2.6899 no . . H(64B) H(28F) 2.8240 no . 4_564 H(65B) C(38) 3.3811 no . 1_565 H(65B) C(39) 2.9315 no . 1_565 H(65B) C(40) 3.3369 no . 1_565 H(65B) H(32B) 2.9530 no . 1_565 H(65B) H(39) 2.9125 no . 1_565 H(65B) H(58A) 3.5294 no . 1_565 H(65C) C(39) 3.1999 no . 1_565 H(65C) C(40) 3.5270 no . 1_565 H(65C) C(58) 3.3312 no . 1_565 H(65C) H(39) 2.7772 no . 1_565 H(65C) H(58A) 2.4197 no . 1_565 H(65C) H(63A) 2.9079 no . 2_555 H(65C) H(63F) 2.8126 no . 2_555 H(66A) N(2) 3.1631 no . 4_564 H(66A) C(5) 3.5822 no . 4_564 H(66A) C(6) 3.0848 no . 4_564 H(66A) C(7) 3.2273 no . 4_564 H(66A) C(8) 3.2786 no . 4_564 H(66A) C(9) 3.2363 no . 4_564 H(66A) C(62) 3.4500 no . 4_554 H(66A) H(62B) 3.4127 no . 4_554 H(66A) H(62C) 2.6593 no . 4_554 H(66A) H(62D) 2.7024 no . 4_554 H(66A) H(62E) 3.3444 no . 4_554 H(66B) F(1) 3.2926 no . 4_564 H(66B) N(2) 3.5247 no . 4_564 H(66B) C(9) 3.4551 no . 4_564 H(66B) H(28A) 3.1099 no . 4_564 H(66B) H(28F) 3.1501 no . 4_564 H(67A) C(55) 3.2041 no . 2_555 H(67A) C(62) 3.4229 no . 4_554 H(67A) H(55A) 2.9955 no . 2_555 H(67A) H(55B) 2.5659 no . 2_555 H(67A) H(61A) 2.9235 no . 4_554 H(67A) H(62B) 3.2259 no . 4_554 H(67A) H(62C) 2.9025 no . 4_554 H(67A) H(62D) 2.5126 no . 4_554 H(67B) C(62) 3.0635 no . 4_554 H(67B) H(61A) 2.7922 no . 4_554 H(67B) H(62B) 2.4627 no . 4_554 H(67B) H(62C) 2.8341 no . 4_554 H(67B) H(62D) 2.1132 no . 4_554 H(67B) H(62F) 3.3510 no . 4_554 H(67C) C(55) 3.5982 no . 2_555 H(67C) H(55B) 2.6922 no . 2_555 H(67C) H(61A) 3.4012 no . 4_554 H(67C) H(62D) 3.5331 no . 4_554 H(68A) F(5) 3.5359 no . 4_554 H(68A) C(24) 3.5340 no . 4_564 H(68A) H(24A) 2.9782 no . 4_564 H(68A) H(24B) 3.3875 no . 4_564 H(68A) H(26B) 3.0306 no . 4_564 H(68B) F(5) 2.8409 no . 4_554 H(68B) H(24B) 3.4426 no . 4_564 H(68B) H(55A) 3.5177 no . 2_555 H(68B) H(62C) 2.9765 no . 4_554 H(68B) H(62D) 3.3536 no . 4_554 H(68C) C(55) 3.3376 no . 2_555 H(68C) H(55A) 2.7060 no . 2_555 H(68C) H(55B) 3.2755 no . 2_555 H(68C) H(56) 3.2538 no . 2_555 H(62D) C(66) 3.1581 no . 4_555 H(62D) C(67) 2.6302 no . 4_555 H(62D) H(66A) 2.7024 no . 4_555 H(62D) H(67A) 2.5126 no . 4_555 H(62D) H(67B) 2.1132 no . 4_555 H(62D) H(67C) 3.5331 no . 4_555 H(62D) H(68B) 3.3536 no . 4_555 H(62E) C(3) 3.5788 no . 1_545 H(62E) C(4) 3.4020 no . 1_545 H(62E) C(5) 3.0312 no . 1_545 H(62E) H(5) 2.7293 no . 1_545 H(62E) H(22) 3.2191 no . 1_545 H(62E) H(29B) 3.1777 no . 1_545 H(62E) H(66A) 3.3444 no . 4_555 H(62F) C(3) 3.4124 no . 1_545 H(62F) C(10) 3.0553 no . 1_545 H(62F) C(11) 3.0306 no . 1_545 H(62F) C(22) 3.4698 no . 1_545 H(62F) C(29) 3.3504 no . 1_545 H(62F) H(22) 3.4758 no . 1_545 H(62F) H(29B) 3.1302 no . 1_545 H(62F) H(29C) 3.2819 no . 1_545 H(62F) H(67B) 3.3510 no . 4_555 H(28D) F(4) 2.9829 no . 4_565 H(28D) C(20) 3.5851 no . 2_656 H(28D) H(20A) 2.7298 no . 2_656 H(28D) H(20B) 3.5943 no . 2_656 H(28E) H(20A) 3.4338 no . 2_656 H(28E) H(31C) 3.5914 no . 2_656 H(28E) H(33B) 3.4212 no . 4_555 H(28E) H(64A) 3.5667 no . 4_565 H(28F) F(4) 2.9633 no . 4_565 H(28F) C(50) 3.2633 no . 4_565 H(28F) C(64) 2.9338 no . 4_565 H(28F) H(29A) 3.2082 no . 4_565 H(28F) H(64A) 2.4322 no . 4_565 H(28F) H(64B) 2.8240 no . 4_565 H(28F) H(66B) 3.1501 no . 4_565 H(68D) F(5) 3.3822 no . 4_554 H(68D) C(55) 3.2996 no . 2_555 H(68D) H(55A) 2.6508 no . 2_555 H(68D) H(55B) 3.0966 no . 2_555 H(68D) H(62C) 3.5431 no . 4_554 H(68E) H(59C) 3.4246 no . 2_555 H(68F) F(5) 2.9332 no . 4_554 H(68F) C(7) 3.3546 no . 4_564 H(68F) C(24) 3.1651 no . 4_564 H(68F) H(24A) 2.8610 no . 4_564 H(68F) H(24B) 2.8947 no . 4_564 H(68F) H(26B) 3.1470 no . 4_564 H(68F) H(62C) 3.4912 no . 4_554 H(23D) H(21B) 2.9813 no . 2_646 H(23D) H(25A) 3.2115 no . 1_545 H(23D) H(31B) 3.5745 no . 2_656 H(23E) C(31) 3.0889 no . 2_656 H(23E) H(21B) 3.3478 no . 2_646 H(23E) H(30A) 3.1406 no . 2_656 H(23E) H(31B) 2.4944 no . 2_656 H(23E) H(31C) 2.9590 no . 2_656 H(23F) C(4) 3.5597 no . 2_646 H(23F) C(5) 3.1355 no . 2_646 H(23F) C(6) 3.5281 no . 2_646 H(23F) C(25) 3.3844 no . 2_646 H(23F) H(5) 3.0742 no . 2_646 H(23F) H(21B) 3.4301 no . 2_646 H(23F) H(25C) 2.4404 no . 2_646 H(23F) H(30A) 2.9521 no . 2_656 H(23F) H(31B) 3.3187 no . 2_656 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================