# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Hiroyuki Furuta' _publ_contact_author_email hfuruta@cstf.kyushu-u.ac.jp _publ_section_title ; Confusion of Mobius aromaticity: Disruption of annulenic pathway in singly N-confused [28]hexaph ; _publ_author_name H.Furuta #============================================================================== # End of CIF #============================================================================== # Attachment '- cif_text_all.doc' #=========================================================================== #== data___NCHexaphyrin _database_code_depnum_ccdc_archive 'CCDC 846697' #TrackingRef '- cif_text_all.doc' #=========================================================================== #== # CHEMICAL DATA _chemical_formula_sum 'C66 H14 F30 N6 ' _chemical_formula_moiety 'C66 H14 F30 N6 ' _chemical_formula_weight 1460.83 _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_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.522(6) _cell_length_b 16.807(6) _cell_length_c 18.706(8) _cell_angle_alpha 65.07(3) _cell_angle_beta 74.95(3) _cell_angle_gamma 77.85(4) _cell_volume 2878(2) _cell_formula_units_Z 2 _cell_measurement_temperature 50(2) _cell_measurement_reflns_used 5405 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 #--------------------------------------------------------------------------- #-- _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 0.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.889 _exptl_absorpt_correction_T_max 0.992 _exptl_special_details ; ? ; _diffrn_ambient_temperature 50(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\Ya _diffrn_radiation_source 'Rotating Anode (50 kV, 16 mA)' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury-8' _diffrn_measurement_method \Yw _diffrn_detector_area_resol_mean 14.7059 _diffrn_reflns_number 26350 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.54 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.985 #=========================================================================== #== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 and Platon squeeze' _computing_publication_material 'CrystalStructure 3.8.2' _computing_molecular_graphics ? #=========================================================================== #== _reflns_number_total 13096 _reflns_number_gt 8464 _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. Electron peaks due to solvent molecules are found with a disordered fashion. Therefore, the hexaphyrin molecule is refined with out the solvent moleculee by the PLATON Squeeze technique. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\Ys^2^(Fo^2^)+(0.0834P)^2^+6.1200P] 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 13096 _refine_ls_number_parameters 920 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1145 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2308 _refine_ls_wR_factor_gt 0.2075 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.385 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.096 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 -0.001 0.500 0.000 196 18 ' ' _platon_squeeze_details ; ; 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 0.4659(2) 0.15702(15) 0.60140(14) 0.0361(5) Uani 1 1 d . . . F2 F 0.6426(3) 0.02222(15) 0.58902(16) 0.0409(6) Uani 1 1 d . A . F3 F 0.8866(2) 0.05182(15) 0.49817(15) 0.0387(6) Uani 1 1 d . . . F4 F 0.9501(2) 0.21865(17) 0.41571(15) 0.0388(6) Uani 1 1 d . A . F5 F 0.7767(2) 0.35549(15) 0.43081(14) 0.0350(5) Uani 1 1 d . . . F6 F 0.7991(3) 0.42449(15) 0.25297(16) 0.0422(6) Uani 1 1 d . . . F7 F 0.9361(3) 0.28926(18) 0.21411(19) 0.0518(7) Uani 1 1 d . A . F8 F 0.8207(3) 0.20622(18) 0.1573(2) 0.0574(8) Uani 1 1 d . . . F9 F 0.5670(3) 0.25928(17) 0.13573(17) 0.0490(7) Uani 1 1 d . A . F10 F 0.4296(3) 0.39447(16) 0.17282(15) 0.0408(6) Uani 1 1 d . . . F11 F 0.6044(3) 0.8595(3) -0.00148(18) 0.0706(10) Uani 1 1 d . A . F12 F 0.6453(4) 0.9739(4) -0.1549(2) 0.1130(19) Uani 1 1 d . . . F13 F 0.4506(4) 1.0286(2) -0.24047(17) 0.0780(12) Uani 1 1 d . A . F14 F 0.2140(3) 0.96362(17) -0.17215(15) 0.0466(7) Uani 1 1 d . . . F15 F 0.1750(3) 0.84499(17) -0.02104(15) 0.0422(6) Uani 1 1 d . A . F16 F 0.1938(2) 0.95867(15) 0.31180(14) 0.0350(5) Uani 1 1 d . . . F17 F 0.0576(3) 1.10796(16) 0.32320(16) 0.0428(6) Uani 1 1 d . A . F18 F -0.2113(3) 1.13065(16) 0.34486(16) 0.0432(6) Uani 1 1 d . . . F19 F -0.3413(3) 1.00216(19) 0.35723(17) 0.0476(7) Uani 1 1 d . A . F20 F -0.2055(2) 0.85250(16) 0.34457(15) 0.0379(5) Uani 1 1 d . . . F21 F -0.0726(3) 0.64308(16) 0.72385(14) 0.0387(6) Uani 1 1 d . . . F22 F -0.2496(3) 0.75394(17) 0.77528(16) 0.0451(6) Uani 1 1 d . A . F23 F -0.4479(3) 0.84983(17) 0.69467(17) 0.0481(7) Uani 1 1 d . . . F24 F -0.4631(3) 0.83113(17) 0.56062(17) 0.0471(7) Uani 1 1 d . A . F25 F -0.2876(2) 0.71749(16) 0.50850(14) 0.0368(5) Uani 1 1 d . . . F26 F 0.1701(4) 0.40178(17) 0.86948(16) 0.0594(9) Uani 1 1 d . A . F27 F 0.1382(4) 0.29292(19) 1.02605(17) 0.0706(11) Uani 1 1 d . . . F28 F 0.0927(3) 0.12443(17) 1.07234(15) 0.0463(7) Uani 1 1 d . A . F29 F 0.0890(3) 0.06237(15) 0.96071(15) 0.0422(6) Uani 1 1 d . . . F30 F 0.1284(3) 0.16900(15) 0.80448(14) 0.0387(6) Uani 1 1 d . A . N1 N 0.3286(3) 0.3718(2) 0.62002(19) 0.0311(7) Uani 1 1 d . . . H1 H 0.2806 0.4134 0.5870 0.037 Uiso 0.48(2) 1 calc PR . . N2 N 0.5293(4) 0.3908(2) 0.3778(2) 0.0303(8) Uani 0.48(2) 1 d P A 1 N5 N 0.1298(4) 0.6548(3) 0.3856(2) 0.0355(9) Uani 0.48(2) 1 d P A 1 C8 C 0.4152(4) 0.5292(2) 0.3539(2) 0.0391(9) Uani 0.48(2) 1 d P A 1 H8 H 0.3765 0.5873 0.3265 0.047 Uiso 0.48(2) 1 calc PR A 1 C22 C -0.0103(4) 0.7338(2) 0.4575(2) 0.0308(8) Uani 0.48(2) 1 d P A 1 H22 H -0.0599 0.7812 0.4712 0.037 Uiso 0.48(2) 1 calc PR A 1 N2A N 0.4152(4) 0.5292(2) 0.3539(2) 0.0391(9) Uani 0.52(2) 1 d P A 2 N5A N -0.0103(4) 0.7338(2) 0.4575(2) 0.0308(8) Uani 0.52(2) 1 d P A 2 C8A C 0.5293(4) 0.3908(2) 0.3778(2) 0.0303(8) Uani 0.52(2) 1 d P A 2 H8A H 0.5780 0.3397 0.3701 0.036 Uiso 0.52(2) 1 calc PR A 2 C22A C 0.1298(4) 0.6548(3) 0.3856(2) 0.0355(9) Uani 0.52(2) 1 d P A 2 H22A H 0.1883 0.6415 0.3430 0.043 Uiso 0.52(2) 1 calc PR A 2 N3 N 0.4234(4) 0.6393(2) 0.17740(19) 0.0320(7) Uani 1 1 d . A . H3A H 0.3758 0.6453 0.2214 0.038 Uiso 0.52(2) 1 calc PR . . N4 N 0.2317(3) 0.7764(2) 0.21233(19) 0.0307(7) Uani 1 1 d . A . H4 H 0.2558 0.7208 0.2411 0.037 Uiso 0.48(2) 1 calc PR . . N6 N 0.0719(3) 0.4757(2) 0.6435(2) 0.0310(7) Uani 1 1 d . A . H6 H 0.1404 0.4840 0.6034 0.037 Uiso 0.52(2) 1 calc PR . . C1 C 0.2955(4) 0.3354(2) 0.7016(2) 0.0309(8) Uani 1 1 d . A . C2 C 0.4051(4) 0.2762(3) 0.7336(2) 0.0321(8) Uani 1 1 d . . . H2 H 0.4092 0.2453 0.7889 0.039 Uiso 1 1 calc R . . C3 C 0.5008(4) 0.2722(3) 0.6717(2) 0.0335(9) Uani 1 1 d . . . H3 H 0.5846 0.2375 0.6749 0.040 Uiso 1 1 calc R . . C4 C 0.4527(4) 0.3304(3) 0.5989(2) 0.0316(8) Uani 1 1 d . . . C5 C 0.5148(4) 0.3354(2) 0.5222(2) 0.0303(8) Uani 1 1 d . A . C6 C 0.4842(4) 0.3996(3) 0.4490(2) 0.0313(8) Uani 1 1 d . . . C7 C 0.4087(4) 0.4880(3) 0.4325(3) 0.0362(9) Uani 1 1 d . A . H7 H 0.3630 0.5113 0.4717 0.043 Uiso 1 1 calc R B 1 C9 C 0.4918(4) 0.4692(3) 0.3184(2) 0.0323(8) Uani 1 1 d . . . C10 C 0.5291(4) 0.4866(2) 0.2376(2) 0.0319(8) Uani 1 1 d . A . C11 C 0.5043(4) 0.5656(3) 0.1723(2) 0.0342(9) Uani 1 1 d . . . C12 C 0.5624(5) 0.5823(3) 0.0913(2) 0.0365(9) Uani 1 1 d . A . H12 H 0.6214 0.5416 0.0717 0.044 Uiso 1 1 calc R . . C13 C 0.5195(4) 0.6666(3) 0.0462(2) 0.0354(9) Uani 1 1 d . . . H13 H 0.5435 0.6964 -0.0104 0.043 Uiso 1 1 calc R A . C14 C 0.4313(4) 0.7015(3) 0.1008(2) 0.0326(8) Uani 1 1 d . A . C15 C 0.3627(4) 0.7863(3) 0.0801(2) 0.0336(9) Uani 1 1 d . . . C16 C 0.2743(4) 0.8212(2) 0.1312(2) 0.0309(8) Uani 1 1 d . A . C17 C 0.2096(4) 0.9101(3) 0.1072(2) 0.0346(9) Uani 1 1 d . . . H17 H 0.2203 0.9545 0.0544 0.042 Uiso 1 1 calc R A . C18 C 0.1309(4) 0.9188(3) 0.1737(2) 0.0346(9) Uani 1 1 d . A . H18 H 0.0765 0.9707 0.1765 0.041 Uiso 1 1 calc R . . C19 C 0.1447(4) 0.8351(3) 0.2397(2) 0.0294(8) Uani 1 1 d . . . C20 C 0.0759(4) 0.8199(2) 0.3184(2) 0.0287(8) Uani 1 1 d . A . C21 C 0.0660(4) 0.7402(3) 0.3844(2) 0.0300(8) Uani 1 1 d . . . C23 C -0.0019(4) 0.6460(2) 0.5073(2) 0.0307(8) Uani 1 1 d . . . C24 C 0.0878(4) 0.5988(3) 0.4606(2) 0.0335(9) Uani 1 1 d . A . H24 H 0.1129 0.5368 0.4807 0.040 Uiso 1 1 calc R C 1 C25 C -0.0722(4) 0.6135(2) 0.5858(2) 0.0310(8) Uani 1 1 d . A . C26 C -0.0464(4) 0.5288(2) 0.6443(2) 0.0314(8) Uani 1 1 d . . . C27 C -0.1349(4) 0.4881(3) 0.7188(2) 0.0343(9) Uani 1 1 d . A . H27 H -0.2243 0.5097 0.7341 0.041 Uiso 1 1 calc R . . C28 C -0.0672(4) 0.4136(3) 0.7630(2) 0.0341(9) Uani 1 1 d . . . H28 H -0.1002 0.3727 0.8151 0.041 Uiso 1 1 calc R A . C29 C 0.0629(4) 0.4074(2) 0.7171(2) 0.0300(8) Uani 1 1 d . A . C30 C 0.1694(4) 0.3475(3) 0.7463(2) 0.0308(8) Uani 1 1 d . . . C31 C 0.6149(4) 0.2612(2) 0.5177(2) 0.0309(8) Uani 1 1 d . . . C32 C 0.5860(4) 0.1744(3) 0.5571(2) 0.0311(8) Uani 1 1 d . A . C33 C 0.6750(4) 0.1045(3) 0.5511(2) 0.0330(9) Uani 1 1 d . . . C34 C 0.7980(4) 0.1197(3) 0.5046(3) 0.0341(9) Uani 1 1 d . A . C35 C 0.8298(4) 0.2044(3) 0.4640(3) 0.0347(9) Uani 1 1 d . . . C36 C 0.7406(4) 0.2736(3) 0.4705(2) 0.0318(8) Uani 1 1 d . A . C37 C 0.6097(5) 0.4129(3) 0.2153(3) 0.0367(9) Uani 1 1 d . . . C38 C 0.7392(5) 0.3845(3) 0.2252(3) 0.0370(9) Uani 1 1 d . A . C39 C 0.8109(5) 0.3156(3) 0.2051(3) 0.0424(11) Uani 1 1 d . . . C40 C 0.7527(5) 0.2731(3) 0.1759(3) 0.0436(11) Uani 1 1 d . A . C41 C 0.6251(5) 0.2999(3) 0.1652(3) 0.0417(10) Uani 1 1 d . . . C42 C 0.5557(4) 0.3688(3) 0.1848(3) 0.0368(9) Uani 1 1 d . A . C43 C 0.3892(4) 0.8476(3) -0.0065(2) 0.0342(9) Uani 1 1 d . A . C44 C 0.5055(5) 0.8826(4) -0.0433(3) 0.0496(12) Uani 1 1 d . . . C45 C 0.5295(6) 0.9410(4) -0.1217(3) 0.0636(17) Uani 1 1 d . A . C46 C 0.4304(6) 0.9700(3) -0.1649(3) 0.0517(13) Uani 1 1 d . . . C47 C 0.3124(5) 0.9366(3) -0.1303(3) 0.0388(10) Uani 1 1 d . A . C48 C 0.2930(4) 0.8756(3) -0.0525(2) 0.0330(8) Uani 1 1 d . . . C49 C -0.0024(4) 0.9006(3) 0.3292(2) 0.0308(8) Uani 1 1 d . . . C50 C 0.0617(4) 0.9672(3) 0.3241(2) 0.0322(8) Uani 1 1 d . A . C51 C -0.0074(5) 1.0444(3) 0.3295(3) 0.0354(9) Uani 1 1 d . . . C52 C -0.1419(4) 1.0555(3) 0.3401(2) 0.0350(9) Uani 1 1 d . A . C53 C -0.2093(4) 0.9899(3) 0.3477(3) 0.0380(10) Uani 1 1 d . . . C54 C -0.1385(4) 0.9132(3) 0.3415(2) 0.0323(8) Uani 1 1 d . A . C55 C -0.1734(4) 0.6742(3) 0.6144(2) 0.0313(8) Uani 1 1 d . . . C56 C -0.1701(4) 0.6872(3) 0.6825(2) 0.0329(9) Uani 1 1 d . A . C57 C -0.2581(4) 0.7453(3) 0.7095(3) 0.0362(9) Uani 1 1 d . . . C58 C -0.3580(5) 0.7941(3) 0.6680(3) 0.0406(10) Uani 1 1 d . A . C59 C -0.3659(4) 0.7837(3) 0.6006(3) 0.0383(9) Uani 1 1 d . . . C60 C -0.2754(4) 0.7257(3) 0.5742(2) 0.0331(8) Uani 1 1 d . A . C61 C 0.1477(4) 0.2892(3) 0.8328(2) 0.0312(8) Uani 1 1 d . A . C62 C 0.1492(5) 0.3179(3) 0.8914(3) 0.0404(10) Uani 1 1 d . . . C63 C 0.1311(5) 0.2637(3) 0.9713(3) 0.0445(11) Uani 1 1 d . A . C64 C 0.1108(4) 0.1774(3) 0.9942(2) 0.0361(9) Uani 1 1 d . . . C65 C 0.1086(4) 0.1467(2) 0.9382(2) 0.0320(8) Uani 1 1 d . A . C66 C 0.1286(4) 0.2011(3) 0.8590(2) 0.0314(8) 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 0.0366(13) 0.0288(12) 0.0339(12) -0.0047(10) -0.0062(10) -0.0019(9) F2 0.0498(15) 0.0231(11) 0.0452(14) -0.0073(10) -0.0146(12) -0.0009(10) F3 0.0406(14) 0.0338(13) 0.0436(14) -0.0192(11) -0.0150(11) 0.0093(10) F4 0.0335(13) 0.0459(14) 0.0397(13) -0.0207(11) -0.0047(10) -0.0047(10) F5 0.0398(13) 0.0299(12) 0.0334(12) -0.0074(10) -0.0103(10) -0.0067(10) F6 0.0503(16) 0.0300(12) 0.0532(16) -0.0174(11) -0.0244(13) 0.0019(11) F7 0.0531(17) 0.0409(15) 0.072(2) -0.0295(14) -0.0331(15) 0.0148(12) F8 0.075(2) 0.0413(15) 0.072(2) -0.0361(15) -0.0375(17) 0.0197(14) F9 0.0675(19) 0.0356(14) 0.0570(17) -0.0233(13) -0.0305(15) 0.0016(12) F10 0.0475(15) 0.0334(13) 0.0434(14) -0.0129(11) -0.0181(12) -0.0009(11) F11 0.0545(19) 0.109(3) 0.0363(15) -0.0008(16) -0.0176(14) -0.0329(18) F12 0.108(3) 0.178(5) 0.0408(18) 0.009(2) -0.014(2) -0.104(3) F13 0.128(3) 0.071(2) 0.0296(15) 0.0135(14) -0.0281(18) -0.056(2) F14 0.0660(18) 0.0424(14) 0.0337(13) -0.0108(11) -0.0272(13) 0.0024(12) F15 0.0457(15) 0.0488(15) 0.0307(12) -0.0108(11) -0.0118(11) -0.0068(12) F16 0.0366(13) 0.0326(12) 0.0363(13) -0.0121(10) -0.0077(10) -0.0069(10) F17 0.0575(17) 0.0307(13) 0.0439(14) -0.0151(11) -0.0112(12) -0.0092(11) F18 0.0541(16) 0.0355(13) 0.0448(15) -0.0209(11) -0.0205(12) 0.0100(11) F19 0.0366(14) 0.0572(17) 0.0590(17) -0.0344(14) -0.0176(13) 0.0097(12) F20 0.0373(13) 0.0407(13) 0.0432(14) -0.0218(11) -0.0096(11) -0.0058(10) F21 0.0460(15) 0.0377(13) 0.0346(13) -0.0122(10) -0.0180(11) -0.0004(11) F22 0.0565(17) 0.0447(15) 0.0416(14) -0.0230(12) -0.0089(12) -0.0088(12) F23 0.0473(16) 0.0409(14) 0.0558(17) -0.0253(13) -0.0040(13) 0.0017(12) F24 0.0400(15) 0.0447(15) 0.0543(16) -0.0175(13) -0.0215(13) 0.0113(11) F25 0.0383(13) 0.0395(13) 0.0326(12) -0.0116(10) -0.0142(10) -0.0006(10) F26 0.123(3) 0.0266(13) 0.0345(14) -0.0069(11) -0.0299(16) -0.0132(15) F27 0.147(3) 0.0377(15) 0.0321(14) -0.0106(12) -0.0334(18) -0.0070(18) F28 0.0615(18) 0.0365(14) 0.0269(12) 0.0007(10) -0.0111(12) -0.0020(12) F29 0.0524(16) 0.0248(12) 0.0429(14) -0.0017(10) -0.0155(12) -0.0082(10) F30 0.0576(16) 0.0295(12) 0.0327(12) -0.0113(10) -0.0151(11) -0.0063(11) N1 0.0350(18) 0.0303(17) 0.0263(16) -0.0098(13) -0.0094(14) 0.0016(13) N2 0.037(2) 0.0242(17) 0.0269(17) -0.0053(14) -0.0097(15) -0.0023(14) N5 0.042(2) 0.035(2) 0.0294(19) -0.0112(16) -0.0103(16) -0.0044(16) C8 0.045(2) 0.0275(19) 0.040(2) -0.0052(16) -0.0171(18) -0.0013(16) C22 0.0352(19) 0.0281(18) 0.0273(17) -0.0081(14) -0.0093(15) -0.0015(14) N2A 0.045(2) 0.0275(19) 0.040(2) -0.0052(16) -0.0171(18) -0.0013(16) N5A 0.0352(19) 0.0281(18) 0.0273(17) -0.0081(14) -0.0093(15) -0.0015(14) C8A 0.037(2) 0.0242(17) 0.0269(17) -0.0053(14) -0.0097(15) -0.0023(14) C22A 0.042(2) 0.035(2) 0.0294(19) -0.0112(16) -0.0103(16) -0.0044(16) N3 0.047(2) 0.0236(16) 0.0237(15) -0.0061(13) -0.0127(14) -0.0004(14) N4 0.0380(19) 0.0269(16) 0.0239(15) -0.0082(13) -0.0058(14) -0.0009(13) N6 0.0411(19) 0.0229(15) 0.0271(16) -0.0052(13) -0.0129(14) -0.0016(13) C1 0.041(2) 0.0255(18) 0.0259(18) -0.0082(15) -0.0115(16) -0.0007(16) C2 0.043(2) 0.032(2) 0.0201(17) -0.0069(15) -0.0112(16) -0.0003(16) C3 0.041(2) 0.028(2) 0.030(2) -0.0081(16) -0.0144(17) 0.0022(16) C4 0.038(2) 0.0247(18) 0.0301(19) -0.0084(15) -0.0106(17) -0.0004(15) C5 0.034(2) 0.0250(18) 0.0309(19) -0.0075(15) -0.0134(16) 0.0006(15) C6 0.037(2) 0.0269(19) 0.0259(18) -0.0054(15) -0.0108(16) -0.0001(16) C7 0.035(2) 0.027(2) 0.044(2) -0.0112(18) -0.0104(18) 0.0008(16) C9 0.039(2) 0.0243(18) 0.0283(19) -0.0051(15) -0.0083(17) -0.0026(16) C10 0.043(2) 0.0230(18) 0.032(2) -0.0105(16) -0.0150(17) -0.0001(16) C11 0.045(2) 0.0255(19) 0.033(2) -0.0110(16) -0.0130(18) -0.0003(16) C12 0.048(3) 0.031(2) 0.032(2) -0.0145(17) -0.0120(18) 0.0027(17) C13 0.046(2) 0.034(2) 0.0254(19) -0.0098(16) -0.0114(17) -0.0001(17) C14 0.040(2) 0.030(2) 0.0248(18) -0.0065(15) -0.0124(16) 0.0006(16) C15 0.042(2) 0.0279(19) 0.0279(19) -0.0065(16) -0.0147(17) 0.0022(16) C16 0.039(2) 0.0255(18) 0.0245(18) -0.0032(15) -0.0105(16) -0.0037(15) C17 0.049(2) 0.0251(19) 0.0241(18) -0.0018(15) -0.0133(17) -0.0014(17) C18 0.047(2) 0.0242(19) 0.031(2) -0.0061(16) -0.0164(18) 0.0003(16) C19 0.034(2) 0.0273(19) 0.0263(18) -0.0089(15) -0.0097(16) -0.0016(15) C20 0.032(2) 0.0254(18) 0.0285(19) -0.0097(15) -0.0083(15) -0.0017(15) C21 0.035(2) 0.032(2) 0.0247(18) -0.0104(15) -0.0113(16) 0.0004(15) C23 0.039(2) 0.0233(18) 0.0287(19) -0.0041(15) -0.0146(16) -0.0031(15) C24 0.039(2) 0.034(2) 0.0289(19) -0.0128(16) -0.0114(17) 0.0006(17) C25 0.036(2) 0.0244(18) 0.032(2) -0.0057(15) -0.0149(17) -0.0011(15) C26 0.044(2) 0.0247(18) 0.0249(18) -0.0035(15) -0.0136(17) -0.0062(16) C27 0.041(2) 0.032(2) 0.0270(19) -0.0082(16) -0.0076(17) -0.0032(17) C28 0.044(2) 0.030(2) 0.0252(18) -0.0066(16) -0.0081(17) -0.0051(17) C29 0.037(2) 0.0266(19) 0.0250(18) -0.0069(15) -0.0086(16) -0.0039(15) C30 0.039(2) 0.0264(19) 0.0281(19) -0.0087(15) -0.0077(16) -0.0072(15) C31 0.036(2) 0.0256(19) 0.0271(18) -0.0064(15) -0.0065(16) -0.0025(15) C32 0.031(2) 0.0265(19) 0.0302(19) -0.0063(15) -0.0075(16) 0.0009(15) C33 0.040(2) 0.0233(18) 0.035(2) -0.0091(16) -0.0142(18) 0.0019(16) C34 0.035(2) 0.030(2) 0.039(2) -0.0158(17) -0.0147(18) 0.0070(16) C35 0.033(2) 0.038(2) 0.036(2) -0.0163(18) -0.0100(17) -0.0007(17) C36 0.040(2) 0.0273(19) 0.0278(19) -0.0089(15) -0.0102(17) -0.0016(16) C37 0.053(3) 0.0232(19) 0.039(2) -0.0116(17) -0.022(2) 0.0024(17) C38 0.048(3) 0.0252(19) 0.042(2) -0.0121(17) -0.019(2) 0.0001(17) C39 0.046(3) 0.029(2) 0.057(3) -0.018(2) -0.028(2) 0.0111(18) C40 0.054(3) 0.027(2) 0.054(3) -0.017(2) -0.025(2) 0.0104(19) C41 0.062(3) 0.028(2) 0.042(2) -0.0154(18) -0.022(2) -0.0020(19) C42 0.044(2) 0.0244(19) 0.042(2) -0.0100(17) -0.0180(19) 0.0023(16) C43 0.041(2) 0.031(2) 0.0247(19) -0.0043(16) -0.0083(17) -0.0052(17) C44 0.047(3) 0.062(3) 0.034(2) -0.002(2) -0.018(2) -0.017(2) C45 0.071(4) 0.083(4) 0.032(2) 0.002(3) -0.012(2) -0.049(3) C46 0.077(4) 0.047(3) 0.028(2) 0.004(2) -0.022(2) -0.026(3) C47 0.062(3) 0.027(2) 0.030(2) -0.0061(16) -0.025(2) -0.0018(18) C48 0.041(2) 0.0257(19) 0.032(2) -0.0066(16) -0.0124(17) -0.0045(16) C49 0.036(2) 0.030(2) 0.0276(19) -0.0129(16) -0.0081(16) -0.0021(16) C50 0.036(2) 0.030(2) 0.0301(19) -0.0111(16) -0.0097(16) -0.0003(16) C51 0.049(3) 0.028(2) 0.032(2) -0.0118(16) -0.0149(18) -0.0017(17) C52 0.048(2) 0.031(2) 0.0290(19) -0.0169(17) -0.0129(18) 0.0080(17) C53 0.037(2) 0.041(2) 0.044(2) -0.025(2) -0.0163(19) 0.0087(18) C54 0.038(2) 0.029(2) 0.037(2) -0.0173(17) -0.0148(17) 0.0004(16) C55 0.032(2) 0.0294(19) 0.0310(19) -0.0084(16) -0.0093(16) -0.0037(15) C56 0.038(2) 0.0285(19) 0.032(2) -0.0073(16) -0.0129(17) -0.0049(16) C57 0.040(2) 0.034(2) 0.038(2) -0.0152(18) -0.0089(18) -0.0057(17) C58 0.041(2) 0.030(2) 0.051(3) -0.0191(19) -0.007(2) 0.0014(17) C59 0.036(2) 0.034(2) 0.044(2) -0.0107(18) -0.0169(19) 0.0015(17) C60 0.035(2) 0.029(2) 0.034(2) -0.0112(16) -0.0119(17) 0.0020(16) C61 0.037(2) 0.0262(19) 0.0308(19) -0.0111(16) -0.0100(16) -0.0003(15) C62 0.070(3) 0.0209(19) 0.028(2) -0.0028(16) -0.015(2) -0.0063(18) C63 0.076(3) 0.032(2) 0.028(2) -0.0100(17) -0.022(2) -0.001(2) C64 0.045(2) 0.028(2) 0.0234(18) 0.0018(15) -0.0100(17) -0.0010(17) C65 0.035(2) 0.0229(18) 0.033(2) -0.0027(15) -0.0090(17) -0.0056(15) C66 0.040(2) 0.0262(19) 0.0292(19) -0.0098(15) -0.0117(17) -0.0024(16) _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 C32 1.333(5) . ? F2 C33 1.334(5) . ? F3 C34 1.340(4) . ? F4 C35 1.351(5) . ? F5 C36 1.342(5) . ? F6 C38 1.329(5) . ? F7 C39 1.329(5) . ? F8 C40 1.326(5) . ? F9 C41 1.348(5) . ? F10 C42 1.352(5) . ? F11 C44 1.358(5) . ? F12 C45 1.333(6) . ? F13 C46 1.332(5) . ? F14 C47 1.347(5) . ? F15 C48 1.337(5) . ? F16 C50 1.336(5) . ? F17 C51 1.335(5) . ? F18 C52 1.344(4) . ? F19 C53 1.336(5) . ? F20 C54 1.332(4) . ? F21 C56 1.345(4) . ? F22 C57 1.326(5) . ? F23 C58 1.341(5) . ? F24 C59 1.340(5) . ? F25 C60 1.334(5) . ? F26 C62 1.342(5) . ? F27 C63 1.333(5) . ? F28 C64 1.340(4) . ? F29 C65 1.343(4) . ? F30 C66 1.341(4) . ? N1 C1 1.360(5) . ? N1 C4 1.388(5) . ? N1 H1 0.8800 . ? N2 C6 1.352(5) . ? N2 C9 1.379(5) . ? N5 C24 1.337(5) . ? N5 C21 1.444(5) . ? C8 C7 1.324(6) . ? C8 C9 1.433(6) . ? C8 H8 0.9500 . ? C22 C21 1.367(5) . ? C22 C23 1.371(5) . ? C22 H22 0.9500 . ? N3 C14 1.365(5) . ? N3 C11 1.371(5) . ? N3 H3A 0.8800 . ? N4 C19 1.370(5) . ? N4 C16 1.377(5) . ? N4 H4 0.8800 . ? N6 C29 1.367(5) . ? N6 C26 1.370(5) . ? N6 H6 0.8800 . ? C1 C30 1.398(6) . ? C1 C2 1.434(5) . ? C2 C3 1.338(6) . ? C2 H2 0.9500 . ? C3 C4 1.447(5) . ? C3 H3 0.9500 . ? C4 C5 1.389(6) . ? C5 C6 1.407(5) . ? C5 C31 1.469(5) . ? C6 C7 1.476(5) . ? C7 H7 0.9500 . ? C9 C10 1.375(6) . ? C10 C11 1.405(5) . ? C10 C37 1.497(6) . ? C11 C12 1.408(6) . ? C12 C13 1.359(6) . ? C12 H12 0.9500 . ? C13 C14 1.426(6) . ? C13 H13 0.9500 . ? C14 C15 1.396(5) . ? C15 C16 1.380(6) . ? C15 C43 1.498(5) . ? C16 C17 1.436(5) . ? C17 C18 1.351(6) . ? C17 H17 0.9500 . ? C18 C19 1.437(5) . ? C18 H18 0.9500 . ? C19 C20 1.402(5) . ? C20 C21 1.388(5) . ? C20 C49 1.494(5) . ? C23 C25 1.391(6) . ? C23 C24 1.457(6) . ? C24 H24 0.9500 . ? C25 C26 1.406(5) . ? C25 C55 1.471(6) . ? C26 C27 1.439(6) . ? C27 C28 1.347(6) . ? C27 H27 0.9500 . ? C28 C29 1.423(6) . ? C28 H28 0.9500 . ? C29 C30 1.396(6) . ? C30 C61 1.482(5) . ? C31 C32 1.389(5) . ? C31 C36 1.389(6) . ? C32 C33 1.363(5) . ? C33 C34 1.365(6) . ? C34 C35 1.368(6) . ? C35 C36 1.360(6) . ? C37 C42 1.378(6) . ? C37 C38 1.378(6) . ? C38 C39 1.379(6) . ? C39 C40 1.368(6) . ? C40 C41 1.362(7) . ? C41 C42 1.367(6) . ? C43 C44 1.357(6) . ? C43 C48 1.376(6) . ? C44 C45 1.370(6) . ? C45 C46 1.367(7) . ? C46 C47 1.358(7) . ? C47 C48 1.374(6) . ? C49 C54 1.376(6) . ? C49 C50 1.382(6) . ? C50 C51 1.377(6) . ? C51 C52 1.361(6) . ? C52 C53 1.373(6) . ? C53 C54 1.382(5) . ? C55 C56 1.390(6) . ? C55 C60 1.395(5) . ? C56 C57 1.363(6) . ? C57 C58 1.380(6) . ? C58 C59 1.368(6) . ? C59 C60 1.368(6) . ? C61 C62 1.375(6) . ? C61 C66 1.391(5) . ? C62 C63 1.370(6) . ? C63 C64 1.375(6) . ? C64 C65 1.355(6) . ? C65 C66 1.360(5) . ? 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 106.7(3) . . ? C1 N1 H1 126.6 . . ? C4 N1 H1 126.6 . . ? C6 N2 C9 107.9(3) . . ? C24 N5 C21 104.1(4) . . ? C7 C8 C9 106.8(3) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? C21 C22 C23 107.2(4) . . ? C21 C22 H22 126.4 . . ? C23 C22 H22 126.4 . . ? C14 N3 C11 106.6(3) . . ? C14 N3 H3A 126.7 . . ? C11 N3 H3A 126.7 . . ? C19 N4 C16 106.8(3) . . ? C19 N4 H4 126.6 . . ? C16 N4 H4 126.6 . . ? C29 N6 C26 106.7(3) . . ? C29 N6 H6 126.7 . . ? C26 N6 H6 126.7 . . ? N1 C1 C30 124.8(4) . . ? N1 C1 C2 109.6(4) . . ? C30 C1 C2 125.4(4) . . ? C3 C2 C1 107.8(3) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? C2 C3 C4 107.2(4) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N1 C4 C5 126.3(4) . . ? N1 C4 C3 108.4(4) . . ? C5 C4 C3 124.8(4) . . ? C4 C5 C6 126.9(4) . . ? C4 C5 C31 116.0(3) . . ? C6 C5 C31 116.8(4) . . ? N2 C6 C5 123.6(4) . . ? N2 C6 C7 107.2(3) . . ? C5 C6 C7 129.1(4) . . ? C8 C7 C6 108.5(4) . . ? C8 C7 H7 125.7 . . ? C6 C7 H7 125.7 . . ? C10 C9 N2 124.0(4) . . ? C10 C9 C8 126.4(4) . . ? N2 C9 C8 109.6(4) . . ? C9 C10 C11 128.6(4) . . ? C9 C10 C37 116.4(3) . . ? C11 C10 C37 115.0(4) . . ? N3 C11 C10 125.7(4) . . ? N3 C11 C12 109.3(3) . . ? C10 C11 C12 125.0(4) . . ? C13 C12 C11 108.1(4) . . ? C13 C12 H12 125.9 . . ? C11 C12 H12 125.9 . . ? C12 C13 C14 106.2(4) . . ? C12 C13 H13 126.9 . . ? C14 C13 H13 126.9 . . ? N3 C14 C15 124.5(4) . . ? N3 C14 C13 109.8(3) . . ? C15 C14 C13 125.7(4) . . ? C16 C15 C14 127.1(4) . . ? C16 C15 C43 115.6(3) . . ? C14 C15 C43 117.3(4) . . ? N4 C16 C15 125.8(4) . . ? N4 C16 C17 109.3(4) . . ? C15 C16 C17 124.9(4) . . ? C18 C17 C16 107.3(3) . . ? C18 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? C17 C18 C19 107.3(4) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? N4 C19 C20 127.7(3) . . ? N4 C19 C18 109.4(3) . . ? C20 C19 C18 122.9(4) . . ? C21 C20 C19 128.4(4) . . ? C21 C20 C49 117.5(4) . . ? C19 C20 C49 114.0(3) . . ? C22 C21 C20 122.5(4) . . ? C22 C21 N5 111.4(3) . . ? C20 C21 N5 126.0(4) . . ? C22 C23 C25 123.6(4) . . ? C22 C23 C24 106.7(4) . . ? C25 C23 C24 129.7(4) . . ? N5 C24 C23 110.7(4) . . ? N5 C24 H24 124.7 . . ? C23 C24 H24 124.7 . . ? C23 C25 C26 125.4(4) . . ? C23 C25 C55 118.6(3) . . ? C26 C25 C55 115.7(4) . . ? N6 C26 C25 125.5(4) . . ? N6 C26 C27 108.9(3) . . ? C25 C26 C27 125.2(4) . . ? C28 C27 C26 107.1(4) . . ? C28 C27 H27 126.4 . . ? C26 C27 H27 126.4 . . ? C27 C28 C29 107.4(4) . . ? C27 C28 H28 126.3 . . ? C29 C28 H28 126.3 . . ? N6 C29 C30 124.8(4) . . ? N6 C29 C28 109.7(3) . . ? C30 C29 C28 125.1(4) . . ? C29 C30 C1 126.4(4) . . ? C29 C30 C61 117.6(4) . . ? C1 C30 C61 116.0(3) . . ? C32 C31 C36 116.0(4) . . ? C32 C31 C5 121.5(4) . . ? C36 C31 C5 122.4(3) . . ? F1 C32 C33 117.4(4) . . ? F1 C32 C31 119.8(3) . . ? C33 C32 C31 122.8(4) . . ? F2 C33 C32 120.9(4) . . ? F2 C33 C34 119.9(4) . . ? C32 C33 C34 119.2(4) . . ? F3 C34 C33 120.0(4) . . ? F3 C34 C35 120.2(4) . . ? C33 C34 C35 119.8(4) . . ? F4 C35 C36 120.3(4) . . ? F4 C35 C34 119.1(4) . . ? C36 C35 C34 120.6(4) . . ? F5 C36 C35 118.7(4) . . ? F5 C36 C31 119.7(3) . . ? C35 C36 C31 121.6(4) . . ? C42 C37 C38 116.7(4) . . ? C42 C37 C10 120.7(4) . . ? C38 C37 C10 122.5(4) . . ? F6 C38 C37 120.4(4) . . ? F6 C38 C39 118.1(4) . . ? C37 C38 C39 121.5(4) . . ? F7 C39 C40 119.1(4) . . ? F7 C39 C38 121.0(4) . . ? C40 C39 C38 119.8(4) . . ? F8 C40 C41 119.9(4) . . ? F8 C40 C39 120.1(4) . . ? C41 C40 C39 120.0(4) . . ? F9 C41 C40 120.6(4) . . ? F9 C41 C42 119.9(4) . . ? C40 C41 C42 119.5(4) . . ? F10 C42 C41 118.1(4) . . ? F10 C42 C37 119.4(4) . . ? C41 C42 C37 122.5(4) . . ? C44 C43 C48 115.9(4) . . ? C44 C43 C15 122.7(4) . . ? C48 C43 C15 121.3(4) . . ? C43 C44 F11 119.4(4) . . ? C43 C44 C45 123.3(4) . . ? F11 C44 C45 117.3(4) . . ? F12 C45 C46 119.6(4) . . ? F12 C45 C44 121.0(5) . . ? C46 C45 C44 119.3(5) . . ? F13 C46 C47 120.6(4) . . ? F13 C46 C45 120.3(5) . . ? C47 C46 C45 119.2(4) . . ? F14 C47 C46 120.0(4) . . ? F14 C47 C48 119.9(4) . . ? C46 C47 C48 120.0(4) . . ? F15 C48 C47 117.8(4) . . ? F15 C48 C43 120.0(4) . . ? C47 C48 C43 122.1(4) . . ? C54 C49 C50 117.6(4) . . ? C54 C49 C20 122.1(4) . . ? C50 C49 C20 120.2(4) . . ? F16 C50 C51 118.2(4) . . ? F16 C50 C49 120.1(4) . . ? C51 C50 C49 121.6(4) . . ? F17 C51 C52 120.6(4) . . ? F17 C51 C50 120.1(4) . . ? C52 C51 C50 119.3(4) . . ? F18 C52 C51 120.3(4) . . ? F18 C52 C53 118.8(4) . . ? C51 C52 C53 120.8(4) . . ? F19 C53 C52 120.1(4) . . ? F19 C53 C54 120.7(4) . . ? C52 C53 C54 119.1(4) . . ? F20 C54 C49 120.4(3) . . ? F20 C54 C53 118.1(4) . . ? C49 C54 C53 121.5(4) . . ? C56 C55 C60 114.8(4) . . ? C56 C55 C25 121.7(4) . . ? C60 C55 C25 123.4(4) . . ? F21 C56 C57 116.5(4) . . ? F21 C56 C55 119.5(4) . . ? C57 C56 C55 124.0(4) . . ? F22 C57 C56 120.8(4) . . ? F22 C57 C58 120.3(4) . . ? C56 C57 C58 118.9(4) . . ? F23 C58 C59 120.5(4) . . ? F23 C58 C57 120.0(4) . . ? C59 C58 C57 119.5(4) . . ? F24 C59 C58 119.2(4) . . ? F24 C59 C60 120.3(4) . . ? C58 C59 C60 120.4(4) . . ? F25 C60 C59 118.3(3) . . ? F25 C60 C55 119.4(4) . . ? C59 C60 C55 122.3(4) . . ? C62 C61 C66 116.2(4) . . ? C62 C61 C30 122.3(4) . . ? C66 C61 C30 121.5(3) . . ? F26 C62 C63 118.8(4) . . ? F26 C62 C61 118.9(4) . . ? C63 C62 C61 122.3(4) . . ? F27 C63 C62 120.6(4) . . ? F27 C63 C64 120.1(4) . . ? C62 C63 C64 119.2(4) . . ? F28 C64 C65 120.6(4) . . ? F28 C64 C63 119.2(4) . . ? C65 C64 C63 120.2(4) . . ? F29 C65 C64 120.1(4) . . ? F29 C65 C66 120.1(4) . . ? C64 C65 C66 119.9(4) . . ? F30 C66 C65 118.9(3) . . ? F30 C66 C61 118.9(3) . . ? C65 C66 C61 122.2(4) . . ? 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 C30 -168.4(4) . . . . ? C4 N1 C1 C2 5.7(4) . . . . ? N1 C1 C2 C3 -4.1(5) . . . . ? C30 C1 C2 C3 170.0(4) . . . . ? C1 C2 C3 C4 0.8(5) . . . . ? C1 N1 C4 C5 167.9(4) . . . . ? C1 N1 C4 C3 -5.2(4) . . . . ? C2 C3 C4 N1 2.7(5) . . . . ? C2 C3 C4 C5 -170.5(4) . . . . ? N1 C4 C5 C6 18.7(7) . . . . ? C3 C4 C5 C6 -169.4(4) . . . . ? N1 C4 C5 C31 -155.5(4) . . . . ? C3 C4 C5 C31 16.5(6) . . . . ? C9 N2 C6 C5 -173.8(4) . . . . ? C9 N2 C6 C7 2.8(5) . . . . ? C4 C5 C6 N2 -165.9(4) . . . . ? C31 C5 C6 N2 8.2(6) . . . . ? C4 C5 C6 C7 18.4(7) . . . . ? C31 C5 C6 C7 -167.5(4) . . . . ? C9 C8 C7 C6 0.9(5) . . . . ? N2 C6 C7 C8 -2.3(5) . . . . ? C5 C6 C7 C8 174.0(4) . . . . ? C6 N2 C9 C10 174.9(4) . . . . ? C6 N2 C9 C8 -2.3(5) . . . . ? C7 C8 C9 C10 -176.3(4) . . . . ? C7 C8 C9 N2 0.8(5) . . . . ? N2 C9 C10 C11 -175.3(4) . . . . ? C8 C9 C10 C11 1.4(7) . . . . ? N2 C9 C10 C37 3.1(6) . . . . ? C8 C9 C10 C37 179.8(4) . . . . ? C14 N3 C11 C10 177.7(4) . . . . ? C14 N3 C11 C12 -0.4(5) . . . . ? C9 C10 C11 N3 -7.8(7) . . . . ? C37 C10 C11 N3 173.8(4) . . . . ? C9 C10 C11 C12 170.0(4) . . . . ? C37 C10 C11 C12 -8.4(6) . . . . ? N3 C11 C12 C13 0.9(5) . . . . ? C10 C11 C12 C13 -177.2(4) . . . . ? C11 C12 C13 C14 -1.1(5) . . . . ? C11 N3 C14 C15 179.7(4) . . . . ? C11 N3 C14 C13 -0.3(5) . . . . ? C12 C13 C14 N3 0.9(5) . . . . ? C12 C13 C14 C15 -179.1(4) . . . . ? N3 C14 C15 C16 -1.7(7) . . . . ? C13 C14 C15 C16 178.3(4) . . . . ? N3 C14 C15 C43 176.6(4) . . . . ? C13 C14 C15 C43 -3.4(6) . . . . ? C19 N4 C16 C15 -179.7(4) . . . . ? C19 N4 C16 C17 -1.1(4) . . . . ? C14 C15 C16 N4 -3.9(7) . . . . ? C43 C15 C16 N4 177.7(4) . . . . ? C14 C15 C16 C17 177.7(4) . . . . ? C43 C15 C16 C17 -0.7(6) . . . . ? N4 C16 C17 C18 1.1(5) . . . . ? C15 C16 C17 C18 179.7(4) . . . . ? C16 C17 C18 C19 -0.6(5) . . . . ? C16 N4 C19 C20 -179.9(4) . . . . ? C16 N4 C19 C18 0.8(4) . . . . ? C17 C18 C19 N4 -0.1(5) . . . . ? C17 C18 C19 C20 -179.5(4) . . . . ? N4 C19 C20 C21 -9.2(7) . . . . ? C18 C19 C20 C21 170.1(4) . . . . ? N4 C19 C20 C49 174.9(4) . . . . ? C18 C19 C20 C49 -5.8(6) . . . . ? C23 C22 C21 C20 177.4(4) . . . . ? C23 C22 C21 N5 -1.4(5) . . . . ? C19 C20 C21 C22 -176.6(4) . . . . ? C49 C20 C21 C22 -0.8(6) . . . . ? C19 C20 C21 N5 2.0(7) . . . . ? C49 C20 C21 N5 177.8(4) . . . . ? C24 N5 C21 C22 0.7(5) . . . . ? C24 N5 C21 C20 -178.1(4) . . . . ? C21 C22 C23 C25 -176.7(4) . . . . ? C21 C22 C23 C24 1.5(4) . . . . ? C21 N5 C24 C23 0.3(4) . . . . ? C22 C23 C24 N5 -1.2(5) . . . . ? C25 C23 C24 N5 176.9(4) . . . . ? C22 C23 C25 C26 -165.3(4) . . . . ? C24 C23 C25 C26 16.9(7) . . . . ? C22 C23 C25 C55 7.8(6) . . . . ? C24 C23 C25 C55 -169.9(4) . . . . ? C29 N6 C26 C25 169.1(4) . . . . ? C29 N6 C26 C27 -4.5(4) . . . . ? C23 C25 C26 N6 22.1(7) . . . . ? C55 C25 C26 N6 -151.3(4) . . . . ? C23 C25 C26 C27 -165.4(4) . . . . ? C55 C25 C26 C27 21.3(6) . . . . ? N6 C26 C27 C28 2.6(5) . . . . ? C25 C26 C27 C28 -171.0(4) . . . . ? C26 C27 C28 C29 0.3(5) . . . . ? C26 N6 C29 C30 -167.9(4) . . . . ? C26 N6 C29 C28 4.7(4) . . . . ? C27 C28 C29 N6 -3.2(5) . . . . ? C27 C28 C29 C30 169.5(4) . . . . ? N6 C29 C30 C1 -13.4(7) . . . . ? C28 C29 C30 C1 175.0(4) . . . . ? N6 C29 C30 C61 167.8(4) . . . . ? C28 C29 C30 C61 -3.7(6) . . . . ? N1 C1 C30 C29 -9.8(7) . . . . ? C2 C1 C30 C29 177.0(4) . . . . ? N1 C1 C30 C61 168.9(4) . . . . ? C2 C1 C30 C61 -4.2(6) . . . . ? C4 C5 C31 C32 53.5(5) . . . . ? C6 C5 C31 C32 -121.2(4) . . . . ? C4 C5 C31 C36 -130.4(4) . . . . ? C6 C5 C31 C36 54.9(5) . . . . ? C36 C31 C32 F1 -177.7(3) . . . . ? C5 C31 C32 F1 -1.3(6) . . . . ? C36 C31 C32 C33 0.7(6) . . . . ? C5 C31 C32 C33 177.0(4) . . . . ? F1 C32 C33 F2 -0.6(6) . . . . ? C31 C32 C33 F2 -179.0(4) . . . . ? F1 C32 C33 C34 178.3(4) . . . . ? C31 C32 C33 C34 -0.1(6) . . . . ? F2 C33 C34 F3 -1.1(6) . . . . ? C32 C33 C34 F3 180.0(4) . . . . ? F2 C33 C34 C35 178.2(4) . . . . ? C32 C33 C34 C35 -0.8(6) . . . . ? F3 C34 C35 F4 1.8(6) . . . . ? C33 C34 C35 F4 -177.4(4) . . . . ? F3 C34 C35 C36 -179.7(4) . . . . ? C33 C34 C35 C36 1.0(6) . . . . ? F4 C35 C36 F5 -2.8(6) . . . . ? C34 C35 C36 F5 178.8(4) . . . . ? F4 C35 C36 C31 178.0(4) . . . . ? C34 C35 C36 C31 -0.3(6) . . . . ? C32 C31 C36 F5 -179.6(3) . . . . ? C5 C31 C36 F5 4.1(6) . . . . ? C32 C31 C36 C35 -0.5(6) . . . . ? C5 C31 C36 C35 -176.8(4) . . . . ? C9 C10 C37 C42 108.5(5) . . . . ? C11 C10 C37 C42 -72.9(6) . . . . ? C9 C10 C37 C38 -70.3(6) . . . . ? C11 C10 C37 C38 108.3(5) . . . . ? C42 C37 C38 F6 178.8(4) . . . . ? C10 C37 C38 F6 -2.3(7) . . . . ? C42 C37 C38 C39 0.3(7) . . . . ? C10 C37 C38 C39 179.2(4) . . . . ? F6 C38 C39 F7 0.7(7) . . . . ? C37 C38 C39 F7 179.3(4) . . . . ? F6 C38 C39 C40 -179.7(4) . . . . ? C37 C38 C39 C40 -1.1(7) . . . . ? F7 C39 C40 F8 0.3(7) . . . . ? C38 C39 C40 F8 -179.3(4) . . . . ? F7 C39 C40 C41 -179.1(5) . . . . ? C38 C39 C40 C41 1.3(8) . . . . ? F8 C40 C41 F9 -0.1(7) . . . . ? C39 C40 C41 F9 179.3(4) . . . . ? F8 C40 C41 C42 179.9(4) . . . . ? C39 C40 C41 C42 -0.8(8) . . . . ? F9 C41 C42 F10 -0.6(7) . . . . ? C40 C41 C42 F10 179.4(4) . . . . ? F9 C41 C42 C37 179.9(4) . . . . ? C40 C41 C42 C37 0.0(7) . . . . ? C38 C37 C42 F10 -179.2(4) . . . . ? C10 C37 C42 F10 1.9(6) . . . . ? C38 C37 C42 C41 0.3(7) . . . . ? C10 C37 C42 C41 -178.6(4) . . . . ? C16 C15 C43 C44 108.1(5) . . . . ? C14 C15 C43 C44 -70.5(6) . . . . ? C16 C15 C43 C48 -68.4(5) . . . . ? C14 C15 C43 C48 113.0(5) . . . . ? C48 C43 C44 F11 178.8(5) . . . . ? C15 C43 C44 F11 2.1(8) . . . . ? C48 C43 C44 C45 -1.1(8) . . . . ? C15 C43 C44 C45 -177.8(5) . . . . ? C43 C44 C45 F12 179.6(6) . . . . ? F11 C44 C45 F12 -0.3(10) . . . . ? C43 C44 C45 C46 3.5(10) . . . . ? F11 C44 C45 C46 -176.4(6) . . . . ? F12 C45 C46 F13 2.0(10) . . . . ? C44 C45 C46 F13 178.2(6) . . . . ? F12 C45 C46 C47 -179.6(6) . . . . ? C44 C45 C46 C47 -3.4(10) . . . . ? F13 C46 C47 F14 -0.9(8) . . . . ? C45 C46 C47 F14 -179.3(5) . . . . ? F13 C46 C47 C48 179.5(5) . . . . ? C45 C46 C47 C48 1.1(8) . . . . ? F14 C47 C48 F15 0.1(6) . . . . ? C46 C47 C48 F15 179.7(4) . . . . ? F14 C47 C48 C43 -178.2(4) . . . . ? C46 C47 C48 C43 1.4(7) . . . . ? C44 C43 C48 F15 -179.6(4) . . . . ? C15 C43 C48 F15 -2.9(6) . . . . ? C44 C43 C48 C47 -1.3(7) . . . . ? C15 C43 C48 C47 175.4(4) . . . . ? C21 C20 C49 C54 -68.3(5) . . . . ? C19 C20 C49 C54 108.2(5) . . . . ? C21 C20 C49 C50 114.2(4) . . . . ? C19 C20 C49 C50 -69.4(5) . . . . ? C54 C49 C50 F16 -179.7(4) . . . . ? C20 C49 C50 F16 -2.0(6) . . . . ? C54 C49 C50 C51 -1.2(6) . . . . ? C20 C49 C50 C51 176.5(4) . . . . ? F16 C50 C51 F17 -0.6(6) . . . . ? C49 C50 C51 F17 -179.1(4) . . . . ? F16 C50 C51 C52 178.5(4) . . . . ? C49 C50 C51 C52 0.0(6) . . . . ? F17 C51 C52 F18 -0.3(6) . . . . ? C50 C51 C52 F18 -179.4(3) . . . . ? F17 C51 C52 C53 -179.1(4) . . . . ? C50 C51 C52 C53 1.7(6) . . . . ? F18 C52 C53 F19 1.9(6) . . . . ? C51 C52 C53 F19 -179.3(4) . . . . ? F18 C52 C53 C54 178.9(4) . . . . ? C51 C52 C53 C54 -2.2(6) . . . . ? C50 C49 C54 F20 177.9(3) . . . . ? C20 C49 C54 F20 0.3(6) . . . . ? C50 C49 C54 C53 0.7(6) . . . . ? C20 C49 C54 C53 -176.9(4) . . . . ? F19 C53 C54 F20 0.7(6) . . . . ? C52 C53 C54 F20 -176.3(4) . . . . ? F19 C53 C54 C49 178.0(4) . . . . ? C52 C53 C54 C49 1.0(6) . . . . ? C23 C25 C55 C56 -124.3(4) . . . . ? C26 C25 C55 C56 49.5(5) . . . . ? C23 C25 C55 C60 52.7(6) . . . . ? C26 C25 C55 C60 -133.5(4) . . . . ? C60 C55 C56 F21 -177.6(4) . . . . ? C25 C55 C56 F21 -0.4(6) . . . . ? C60 C55 C56 C57 -0.1(6) . . . . ? C25 C55 C56 C57 177.2(4) . . . . ? F21 C56 C57 F22 -2.8(6) . . . . ? C55 C56 C57 F22 179.6(4) . . . . ? F21 C56 C57 C58 178.3(4) . . . . ? C55 C56 C57 C58 0.7(7) . . . . ? F22 C57 C58 F23 -0.8(6) . . . . ? C56 C57 C58 F23 178.2(4) . . . . ? F22 C57 C58 C59 -179.4(4) . . . . ? C56 C57 C58 C59 -0.5(7) . . . . ? F23 C58 C59 F24 1.3(7) . . . . ? C57 C58 C59 F24 179.9(4) . . . . ? F23 C58 C59 C60 -178.9(4) . . . . ? C57 C58 C59 C60 -0.2(7) . . . . ? F24 C59 C60 F25 -0.5(6) . . . . ? C58 C59 C60 F25 179.7(4) . . . . ? F24 C59 C60 C55 -179.3(4) . . . . ? C58 C59 C60 C55 0.9(7) . . . . ? C56 C55 C60 F25 -179.5(4) . . . . ? C25 C55 C60 F25 3.3(6) . . . . ? C56 C55 C60 C59 -0.7(6) . . . . ? C25 C55 C60 C59 -177.9(4) . . . . ? C29 C30 C61 C62 -79.3(5) . . . . ? C1 C30 C61 C62 101.8(5) . . . . ? C29 C30 C61 C66 102.7(5) . . . . ? C1 C30 C61 C66 -76.2(5) . . . . ? C66 C61 C62 F26 178.6(4) . . . . ? C30 C61 C62 F26 0.5(7) . . . . ? C66 C61 C62 C63 -0.9(7) . . . . ? C30 C61 C62 C63 -179.0(4) . . . . ? F26 C62 C63 F27 -2.0(8) . . . . ? C61 C62 C63 F27 177.5(5) . . . . ? F26 C62 C63 C64 -179.5(5) . . . . ? C61 C62 C63 C64 0.0(8) . . . . ? F27 C63 C64 F28 2.7(7) . . . . ? C62 C63 C64 F28 -179.8(4) . . . . ? F27 C63 C64 C65 -177.5(4) . . . . ? C62 C63 C64 C65 -0.1(7) . . . . ? F28 C64 C65 F29 -0.4(6) . . . . ? C63 C64 C65 F29 179.9(4) . . . . ? F28 C64 C65 C66 -179.3(4) . . . . ? C63 C64 C65 C66 1.0(7) . . . . ? F29 C65 C66 F30 0.0(6) . . . . ? C64 C65 C66 F30 178.8(4) . . . . ? F29 C65 C66 C61 179.2(4) . . . . ? C64 C65 C66 C61 -1.9(7) . . . . ? C62 C61 C66 F30 -178.9(4) . . . . ? C30 C61 C66 F30 -0.8(6) . . . . ? C62 C61 C66 C65 1.8(6) . . . . ? C30 C61 C66 C65 180.0(4) . . . . ? #=========================================================================== #== # End of CIF #=========================================================================== #== data_shelxl _database_code_depnum_ccdc_archive 'CCDC 846698' #TrackingRef '- cif_text_all.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H16 F30 N6' _chemical_formula_sum 'C66 H16 F30 N6' _chemical_formula_weight 1462.85 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _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 13.3440(4) _cell_length_b 23.6138(7) _cell_length_c 19.8359(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.955(2) _cell_angle_gamma 90.00 _cell_volume 6190.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30288 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 68.2 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 1.417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8156 _exptl_absorpt_correction_T_max 0.8713 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\Ya _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \Yw _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70388 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 68.22 _reflns_number_total 11179 _reflns_number_gt 7420 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\Ys^2^(Fo^2^)+(0.1743P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11179 _refine_ls_number_parameters 1007 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.2735 _refine_ls_wR_factor_gt 0.2455 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1A F 0.4687(3) 0.71431(14) 1.11714(16) 0.0706(9) Uani 0.775(4) 1 d P A 1 F2A F 0.6202(2) 0.68393(14) 1.04798(18) 0.0828(11) Uani 0.775(4) 1 d P A 1 F3A F 0.7232(3) 0.76357(19) 0.9902(2) 0.0898(13) Uani 0.775(4) 1 d P A 1 F4A F 0.6829(3) 0.87558(19) 1.0081(2) 0.1061(14) Uani 0.775(4) 1 d P A 1 F5A F 0.5298(3) 0.90568(16) 1.0758(2) 0.0825(12) Uani 0.775(4) 1 d P A 1 F1B F 0.536(3) 0.7550(18) 1.095(2) 0.081(8) Uani 0.225(4) 1 d PU A 2 F2B F 0.6758(14) 0.7421(11) 1.0244(11) 0.130(7) Uani 0.225(4) 1 d PU A 2 F3B F 0.7161(10) 0.8401(9) 0.9614(8) 0.131(6) Uani 0.225(4) 1 d PU A 2 F4B F 0.6176(12) 0.9342(8) 0.9851(7) 0.127(6) Uani 0.225(4) 1 d PU A 2 F5B F 0.4663(11) 0.9366(6) 1.0626(7) 0.092(4) Uani 0.225(4) 1 d PU A 2 F6 F 0.39919(17) 0.68393(9) 0.95966(12) 0.0681(6) Uani 1 1 d . . . F7 F 0.55389(17) 0.69572(11) 0.88769(12) 0.0737(7) Uani 1 1 d . A . F8 F 0.53160(19) 0.76133(13) 0.77336(14) 0.0909(8) Uani 1 1 d . . . F9 F 0.3529(2) 0.81440(15) 0.73334(16) 0.1129(11) Uani 1 1 d . A . F10 F 0.20041(19) 0.80542(13) 0.80738(14) 0.0915(9) Uani 1 1 d . . . F11 F 0.02173(17) 0.52366(9) 0.93654(13) 0.0710(7) Uani 1 1 d . A . F12 F -0.04886(19) 0.42565(10) 0.88101(16) 0.0919(9) Uani 1 1 d . . . F13 F -0.2343(2) 0.42139(11) 0.80492(16) 0.0948(9) Uani 1 1 d . A . F14 F -0.3506(2) 0.51537(12) 0.79001(17) 0.1043(11) Uani 1 1 d . . . F15 F -0.28432(18) 0.61307(10) 0.84995(15) 0.0889(8) Uani 1 1 d . A . F16 F 0.03006(17) 0.65403(9) 1.21780(11) 0.0650(6) Uani 1 1 d . . . F17 F 0.0166(2) 0.63581(10) 1.34995(12) 0.0804(7) Uani 1 1 d . A . F18 F -0.1256(2) 0.69002(11) 1.41050(11) 0.0900(9) Uani 1 1 d . . . F19 F -0.2532(2) 0.76502(11) 1.33878(14) 0.0857(8) Uani 1 1 d . A . F20 F -0.24142(17) 0.78385(10) 1.20553(12) 0.0685(6) Uani 1 1 d . . . F21 F -0.2306(2) 0.93122(10) 1.17222(17) 0.0931(9) Uani 1 1 d . A . F22 F -0.3754(2) 1.00763(13) 1.1288(2) 0.1233(13) Uani 1 1 d . . . F23 F -0.3330(2) 1.09617(13) 1.0509(2) 0.1339(14) Uani 1 1 d . A . F24 F -0.1419(3) 1.10865(12) 1.01622(17) 0.1115(11) Uani 1 1 d . . . F25 F 0.0049(2) 1.03452(10) 1.06360(12) 0.0763(7) Uani 1 1 d . A . F26 F 0.2474(2) 0.92334(14) 1.43387(13) 0.0941(9) Uani 1 1 d . . . F27 F 0.3257(3) 0.98510(18) 1.54275(15) 0.1273(13) Uani 1 1 d . A . F28 F 0.4484(2) 1.07174(13) 1.53104(17) 0.1192(13) Uani 1 1 d . . . F29 F 0.5011(3) 1.09713(14) 1.4062(2) 0.1517(16) Uani 1 1 d . A . F30 F 0.4220(3) 1.03829(13) 1.29519(18) 0.1150(11) Uani 1 1 d . . . N1 N 0.3189(2) 0.87992(12) 1.21108(15) 0.0537(7) Uani 1 1 d . . . H1 H 0.2555 0.8748 1.1930 0.064 Uiso 1 1 calc R . . N2 N 0.3106(2) 0.78940(12) 1.02055(15) 0.0502(7) Uani 1 1 d . A . H2 H 0.3625 0.7938 0.9980 0.060 Uiso 1 1 calc R . . N3 N 0.0437(2) 0.69603(12) 0.93147(15) 0.0509(7) Uani 1 1 d . A . H3 H 0.0279 0.7147 0.9670 0.061 Uiso 1 1 calc R . . N4 N -0.0848(2) 0.69097(11) 1.02311(14) 0.0481(7) Uani 1 1 d . A . N5 N -0.0865(2) 0.80896(12) 1.05412(15) 0.0533(7) Uani 1 1 d . A . H5 H -0.1053 0.7887 1.0173 0.064 Uiso 1 1 calc R . . N6 N 0.1350(2) 0.92773(12) 1.21836(15) 0.0498(7) Uani 1 1 d . A . C1 C 0.3493(3) 0.91066(15) 1.26883(19) 0.0546(9) Uani 1 1 d . . . C2 C 0.4578(3) 0.90316(16) 1.2844(2) 0.0585(9) Uani 1 1 d . . . H2A H 0.4995 0.9170 1.3236 0.070 Uiso 1 1 calc R . . C3 C 0.4889(3) 0.87334(17) 1.2339(2) 0.0632(10) Uani 1 1 d . . . H3A H 0.5571 0.8636 1.2305 0.076 Uiso 1 1 calc R . . C4 C 0.4019(3) 0.85815(16) 1.1852(2) 0.0567(9) Uani 1 1 d . A . C5 C 0.3995(3) 0.82800(17) 1.12550(19) 0.0569(9) Uani 1 1 d . . . C6 C 0.3096(3) 0.80699(14) 1.08624(18) 0.0512(8) Uani 1 1 d . A . C7 C 0.2135(3) 0.79330(17) 1.1023(2) 0.0605(10) Uani 1 1 d . . . H7 H 0.1895 0.8008 1.1443 0.073 Uiso 1 1 calc R A . C8 C 0.1597(3) 0.76698(17) 1.0465(2) 0.0621(10) Uani 1 1 d . A . H8 H 0.0925 0.7531 1.0437 0.075 Uiso 1 1 calc R . . C9 C 0.2215(3) 0.76422(15) 0.99413(19) 0.0514(8) Uani 1 1 d . . . C10 C 0.2090(3) 0.73926(15) 0.92765(19) 0.0516(8) Uani 1 1 d . A . C11 C 0.1272(3) 0.70696(15) 0.90043(17) 0.0500(8) Uani 1 1 d . . . C12 C 0.1173(3) 0.67162(15) 0.84040(18) 0.0534(9) Uani 1 1 d . A . H12 H 0.1611 0.6717 0.8065 0.064 Uiso 1 1 calc R . . C13 C 0.0350(3) 0.63840(15) 0.84097(18) 0.0521(8) Uani 1 1 d . . . H13 H 0.0118 0.6105 0.8079 0.063 Uiso 1 1 calc R A . C14 C -0.0119(3) 0.65238(14) 0.90010(18) 0.0504(8) Uani 1 1 d . A . C15 C -0.0892(3) 0.62551(14) 0.92795(18) 0.0482(8) Uani 1 1 d . . . C16 C -0.1152(2) 0.64168(14) 0.99222(17) 0.0470(8) Uani 1 1 d . A . C17 C -0.1678(3) 0.60694(15) 1.03673(19) 0.0516(8) Uani 1 1 d . . . H17 H -0.1989 0.5713 1.0259 0.062 Uiso 1 1 calc R A . C18 C -0.1642(3) 0.63477(14) 1.09607(19) 0.0498(8) Uani 1 1 d . A . H18 H -0.1905 0.6221 1.1356 0.060 Uiso 1 1 calc R . . C19 C -0.1126(3) 0.68789(13) 1.08812(17) 0.0466(8) Uani 1 1 d . . . C20 C -0.0939(3) 0.73084(14) 1.13517(17) 0.0471(8) Uani 1 1 d . A . C21 C -0.0669(3) 0.78753(14) 1.11917(17) 0.0482(8) Uani 1 1 d . . . C22 C -0.0725(3) 0.86543(15) 1.05501(19) 0.0560(9) Uani 1 1 d . . . H22 H -0.0837 0.8898 1.0166 0.067 Uiso 1 1 calc R A . C23 C -0.0343(3) 0.83251(14) 1.16133(18) 0.0482(8) Uani 1 1 d . A . H23 H -0.0124 0.8303 1.2089 0.058 Uiso 1 1 calc R . . C24 C -0.0391(3) 0.88208(14) 1.12165(17) 0.0481(8) Uani 1 1 d . A . C25 C -0.0273(3) 0.93974(14) 1.14629(19) 0.0510(8) Uani 1 1 d . . . C26 C 0.0454(3) 0.95760(14) 1.19718(18) 0.0498(8) Uani 1 1 d . A . C27 C 0.0429(3) 1.00818(14) 1.23893(19) 0.0542(9) Uani 1 1 d . . . H27 H -0.0078 1.0367 1.2341 0.065 Uiso 1 1 calc R A . C28 C 0.1259(3) 1.00678(15) 1.2855(2) 0.0576(9) Uani 1 1 d . A . H28 H 0.1430 1.0328 1.3218 0.069 Uiso 1 1 calc R . . C29 C 0.1845(3) 0.95801(14) 1.26979(18) 0.0509(8) Uani 1 1 d . . . C30 C 0.2861(3) 0.94602(15) 1.29959(19) 0.0535(9) Uani 1 1 d . A . C31A C 0.4933(4) 0.8113(2) 1.0998(3) 0.0544(13) Uani 0.775(4) 1 d P A 1 C32A C 0.5175(12) 0.7503(8) 1.0958(11) 0.067(5) Uani 0.775(4) 1 d P A 1 C33A C 0.5981(4) 0.7389(2) 1.0564(3) 0.0641(14) Uani 0.775(4) 1 d P A 1 C34A C 0.6524(5) 0.7798(4) 1.0274(4) 0.0714(18) Uani 0.775(4) 1 d P A 1 C35A C 0.6296(5) 0.8350(3) 1.0363(4) 0.0750(17) Uani 0.775(4) 1 d P A 1 C36A C 0.5515(4) 0.8505(2) 1.0716(3) 0.0633(14) Uani 0.775(4) 1 d P A 1 C31B C 0.4939(13) 0.8380(10) 1.0867(10) 0.088(5) Uani 0.225(4) 1 d PGU A 2 C32B C 0.5479(15) 0.7887(9) 1.0787(11) 0.093(5) Uani 0.225(4) 1 d PGU A 2 C33B C 0.6230(15) 0.7885(10) 1.0366(13) 0.104(6) Uani 0.225(4) 1 d PGU A 2 C34B C 0.6441(13) 0.8376(11) 1.0025(10) 0.106(5) Uani 0.225(4) 1 d PGU A 2 C35B C 0.5900(14) 0.8869(10) 1.0105(9) 0.107(5) Uani 0.225(4) 1 d PGU A 2 C36B C 0.5149(13) 0.8871(9) 1.0526(11) 0.091(5) Uani 0.225(4) 1 d PGU A 2 C37 C 0.2943(3) 0.74502(15) 0.88623(19) 0.0530(9) Uani 1 1 d . . . C38 C 0.3866(3) 0.71733(16) 0.90463(19) 0.0550(9) Uani 1 1 d . A . C39 C 0.4666(3) 0.72303(18) 0.8683(2) 0.0621(10) Uani 1 1 d . . . C40 C 0.4546(3) 0.7557(2) 0.8091(2) 0.0715(12) Uani 1 1 d . A . C41 C 0.3640(3) 0.7831(2) 0.7900(2) 0.0763(13) Uani 1 1 d . . . C42 C 0.2867(3) 0.77737(19) 0.8280(2) 0.0675(11) Uani 1 1 d . A . C43 C -0.1292(3) 0.57132(14) 0.89530(18) 0.0521(8) Uani 1 1 d . A . C44 C -0.0714(3) 0.52230(15) 0.9021(2) 0.0554(9) Uani 1 1 d . . . C45 C -0.1072(3) 0.47198(16) 0.8735(2) 0.0659(11) Uani 1 1 d . A . C46 C -0.2000(3) 0.46996(17) 0.8340(2) 0.0662(11) Uani 1 1 d . . . C47 C -0.2584(3) 0.51784(18) 0.8265(2) 0.0699(12) Uani 1 1 d . A . C48 C -0.2242(3) 0.56725(16) 0.8579(2) 0.0611(10) Uani 1 1 d . . . C49 C -0.1043(3) 0.72006(14) 1.20768(17) 0.0477(8) Uani 1 1 d . . . C50 C -0.0411(3) 0.68257(15) 1.24592(18) 0.0530(9) Uani 1 1 d . A . C51 C -0.0471(3) 0.67269(17) 1.3145(2) 0.0619(10) Uani 1 1 d . . . C52 C -0.1182(3) 0.70023(18) 1.34435(19) 0.0631(10) Uani 1 1 d . A . C53 C -0.1827(3) 0.73886(17) 1.3090(2) 0.0631(10) Uani 1 1 d . . . C54 C -0.1759(3) 0.74766(15) 1.24059(19) 0.0550(9) Uani 1 1 d . A . C55 C -0.1093(3) 0.98056(15) 1.1189(2) 0.0577(9) Uani 1 1 d . A . C56 C -0.2066(3) 0.97438(17) 1.1339(3) 0.0734(12) Uani 1 1 d . . . C57 C -0.2822(4) 1.0136(2) 1.1118(3) 0.0944(17) Uani 1 1 d . A . C58 C -0.2600(4) 1.05825(19) 1.0727(3) 0.0966(18) Uani 1 1 d . . . C59 C -0.1632(4) 1.06453(19) 1.0548(3) 0.0892(16) Uani 1 1 d . A . C60 C -0.0896(3) 1.02628(17) 1.0788(2) 0.0664(11) Uani 1 1 d . . . C61 C 0.3310(3) 0.97966(16) 1.3604(2) 0.0605(10) Uani 1 1 d . . . C62 C 0.3082(3) 0.9655(2) 1.4254(2) 0.0687(11) Uani 1 1 d . A . C63 C 0.3498(4) 0.9974(3) 1.4824(3) 0.0849(15) Uani 1 1 d . . . C64 C 0.4101(4) 1.0412(2) 1.4766(3) 0.0941(19) Uani 1 1 d . A . C65 C 0.4363(4) 1.0556(2) 1.4136(4) 0.0951(17) Uani 1 1 d . . . C66 C 0.3942(4) 1.0235(2) 1.3572(3) 0.0849(14) Uani 1 1 d . A . 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 F1A 0.079(2) 0.0565(18) 0.078(2) 0.0033(15) 0.0184(17) 0.0065(16) F2A 0.072(2) 0.075(2) 0.101(3) -0.0136(19) 0.0127(18) 0.0196(17) F3A 0.058(2) 0.127(3) 0.088(3) -0.024(2) 0.0200(19) -0.0040(19) F4A 0.090(3) 0.105(3) 0.132(4) 0.004(3) 0.048(3) -0.022(2) F5A 0.078(3) 0.066(2) 0.106(3) 0.001(2) 0.022(2) -0.0092(18) F1B 0.067(14) 0.098(13) 0.083(14) -0.002(11) 0.028(11) -0.032(10) F2B 0.078(10) 0.193(17) 0.114(12) -0.040(12) -0.005(9) 0.052(11) F3B 0.072(8) 0.234(16) 0.089(9) -0.017(10) 0.022(7) 0.012(9) F4B 0.104(9) 0.189(15) 0.089(9) -0.006(10) 0.020(8) -0.067(10) F5B 0.094(9) 0.086(8) 0.096(9) -0.019(7) 0.017(7) -0.024(7) F6 0.0661(14) 0.0720(14) 0.0657(15) 0.0146(12) 0.0080(11) 0.0144(11) F7 0.0551(13) 0.0965(17) 0.0690(15) 0.0019(13) 0.0074(11) 0.0154(12) F8 0.0691(16) 0.129(2) 0.0801(18) 0.0210(16) 0.0300(14) 0.0095(14) F9 0.100(2) 0.155(3) 0.091(2) 0.063(2) 0.0398(17) 0.0362(19) F10 0.0722(16) 0.122(2) 0.0837(18) 0.0431(16) 0.0223(14) 0.0343(15) F11 0.0601(13) 0.0536(12) 0.0927(18) -0.0046(11) -0.0123(12) 0.0045(10) F12 0.0760(16) 0.0533(13) 0.140(2) -0.0225(14) -0.0066(16) 0.0119(11) F13 0.0802(17) 0.0675(15) 0.130(2) -0.0430(15) -0.0096(15) -0.0041(12) F14 0.0777(18) 0.0842(18) 0.135(3) -0.0368(17) -0.0408(17) 0.0048(14) F15 0.0735(16) 0.0597(14) 0.122(2) -0.0226(14) -0.0282(15) 0.0156(11) F16 0.0664(14) 0.0671(13) 0.0589(14) 0.0029(11) -0.0004(11) 0.0138(10) F17 0.1009(19) 0.0752(15) 0.0580(14) 0.0159(12) -0.0138(13) 0.0018(13) F18 0.143(3) 0.0863(18) 0.0427(13) 0.0052(12) 0.0207(15) -0.0173(16) F19 0.107(2) 0.0867(17) 0.0722(17) -0.0095(14) 0.0421(15) 0.0051(14) F20 0.0722(14) 0.0677(14) 0.0667(15) 0.0033(11) 0.0135(12) 0.0149(11) F21 0.0768(16) 0.0627(15) 0.144(3) 0.0207(16) 0.0294(17) 0.0057(12) F22 0.077(2) 0.0816(19) 0.209(4) 0.019(2) 0.012(2) 0.0071(15) F23 0.098(2) 0.0777(19) 0.208(4) 0.037(2) -0.043(2) 0.0104(16) F24 0.131(3) 0.0708(17) 0.118(2) 0.0376(16) -0.033(2) -0.0120(16) F25 0.1001(19) 0.0603(13) 0.0681(16) 0.0135(11) 0.0104(14) -0.0032(12) F26 0.0949(19) 0.129(2) 0.0577(15) -0.0131(15) 0.0073(14) -0.0197(18) F27 0.130(3) 0.191(4) 0.0572(18) -0.041(2) -0.0006(18) 0.014(2) F28 0.109(2) 0.109(2) 0.120(2) -0.069(2) -0.0519(19) 0.0376(17) F29 0.167(3) 0.083(2) 0.185(4) -0.022(2) -0.048(3) -0.046(2) F30 0.146(3) 0.0838(19) 0.110(3) -0.0002(18) -0.003(2) -0.0477(19) N1 0.0544(17) 0.0536(17) 0.0511(18) -0.0100(14) 0.0005(14) -0.0024(13) N2 0.0484(16) 0.0530(16) 0.0482(17) -0.0031(13) 0.0027(13) 0.0009(12) N3 0.0576(17) 0.0509(16) 0.0438(17) -0.0095(13) 0.0057(13) -0.0035(13) N4 0.0584(17) 0.0442(15) 0.0404(16) -0.0052(12) 0.0024(13) -0.0017(12) N5 0.070(2) 0.0490(16) 0.0373(16) -0.0031(13) -0.0049(14) -0.0069(13) N6 0.0507(16) 0.0485(15) 0.0490(17) -0.0027(13) 0.0025(13) -0.0040(12) C1 0.062(2) 0.0501(19) 0.050(2) -0.0035(16) -0.0001(17) -0.0024(16) C2 0.054(2) 0.064(2) 0.054(2) -0.0090(18) -0.0057(17) -0.0040(17) C3 0.056(2) 0.067(2) 0.064(3) -0.010(2) -0.0014(19) -0.0035(18) C4 0.052(2) 0.062(2) 0.055(2) -0.0078(18) 0.0015(17) 0.0008(16) C5 0.051(2) 0.067(2) 0.051(2) -0.0082(18) 0.0003(17) 0.0030(17) C6 0.053(2) 0.0515(19) 0.048(2) -0.0062(16) 0.0033(16) 0.0016(15) C7 0.062(2) 0.066(2) 0.053(2) -0.0145(19) 0.0101(18) -0.0095(18) C8 0.059(2) 0.072(2) 0.056(2) -0.0129(19) 0.0126(19) -0.0121(18) C9 0.056(2) 0.0510(19) 0.046(2) -0.0065(16) 0.0034(16) 0.0005(15) C10 0.052(2) 0.056(2) 0.046(2) 0.0004(16) 0.0047(16) 0.0033(15) C11 0.057(2) 0.0501(18) 0.0423(19) -0.0040(15) 0.0030(16) 0.0026(15) C12 0.061(2) 0.055(2) 0.043(2) -0.0004(16) 0.0049(16) 0.0063(16) C13 0.059(2) 0.052(2) 0.043(2) -0.0053(15) -0.0002(16) 0.0023(16) C14 0.058(2) 0.0463(18) 0.045(2) -0.0057(15) -0.0005(16) 0.0022(15) C15 0.0508(19) 0.0457(18) 0.046(2) -0.0069(15) 0.0005(15) 0.0001(14) C16 0.0472(18) 0.0435(17) 0.049(2) -0.0022(14) 0.0037(15) 0.0002(13) C17 0.0505(19) 0.0457(18) 0.057(2) -0.0022(16) 0.0025(16) -0.0031(14) C18 0.0520(19) 0.0476(18) 0.049(2) 0.0040(15) 0.0036(16) -0.0032(15) C19 0.0543(19) 0.0429(17) 0.0413(19) 0.0001(14) 0.0011(15) 0.0011(14) C20 0.0504(18) 0.0462(17) 0.0432(19) 0.0018(15) 0.0015(15) -0.0008(14) C21 0.0536(19) 0.0475(18) 0.0425(19) 0.0035(15) 0.0030(15) -0.0026(15) C22 0.071(2) 0.0454(19) 0.048(2) 0.0022(16) -0.0025(18) -0.0016(16) C23 0.056(2) 0.0468(18) 0.0398(19) -0.0002(14) 0.0011(15) -0.0025(15) C24 0.0534(19) 0.0444(18) 0.045(2) -0.0052(15) 0.0003(15) 0.0002(14) C25 0.055(2) 0.0471(19) 0.050(2) -0.0009(16) 0.0034(16) -0.0026(15) C26 0.056(2) 0.0455(18) 0.047(2) 0.0005(15) 0.0041(16) -0.0042(15) C27 0.067(2) 0.0403(17) 0.054(2) -0.0003(16) 0.0028(18) 0.0000(15) C28 0.066(2) 0.0483(19) 0.056(2) -0.0102(17) 0.0012(19) -0.0020(16) C29 0.059(2) 0.0462(18) 0.046(2) -0.0059(15) 0.0050(16) -0.0074(15) C30 0.055(2) 0.0510(19) 0.051(2) -0.0089(16) -0.0038(17) -0.0027(15) C31A 0.055(3) 0.060(3) 0.047(3) -0.009(2) 0.001(2) -0.002(3) C32A 0.038(5) 0.076(8) 0.085(9) -0.029(7) -0.001(5) 0.005(5) C33A 0.050(3) 0.075(4) 0.065(4) -0.011(3) 0.001(3) 0.006(2) C34A 0.053(4) 0.101(5) 0.061(4) -0.017(4) 0.011(3) -0.007(3) C35A 0.054(3) 0.087(4) 0.086(5) -0.002(4) 0.014(3) -0.008(3) C36A 0.064(3) 0.059(3) 0.066(4) -0.002(3) 0.004(3) -0.004(3) C31B 0.051(8) 0.135(12) 0.078(10) -0.020(10) 0.010(8) -0.033(9) C32B 0.055(8) 0.143(12) 0.080(9) -0.022(9) 0.010(7) -0.021(9) C33B 0.057(8) 0.164(12) 0.091(10) -0.026(10) 0.010(8) -0.007(9) C34B 0.055(8) 0.170(12) 0.094(9) -0.024(10) 0.014(8) -0.016(8) C35B 0.065(8) 0.162(12) 0.093(9) -0.019(9) 0.011(7) -0.028(8) C36B 0.054(8) 0.139(12) 0.082(9) -0.022(9) 0.017(7) -0.031(9) C37 0.054(2) 0.056(2) 0.050(2) -0.0011(17) 0.0078(17) 0.0007(15) C38 0.056(2) 0.059(2) 0.050(2) 0.0030(17) 0.0054(17) 0.0049(16) C39 0.053(2) 0.073(3) 0.059(2) -0.002(2) 0.0050(18) 0.0086(18) C40 0.060(2) 0.091(3) 0.067(3) 0.006(2) 0.019(2) 0.003(2) C41 0.072(3) 0.094(3) 0.065(3) 0.029(2) 0.018(2) 0.016(2) C42 0.060(2) 0.077(3) 0.065(3) 0.015(2) 0.009(2) 0.016(2) C43 0.061(2) 0.0472(18) 0.047(2) -0.0068(15) 0.0045(17) 0.0007(15) C44 0.052(2) 0.051(2) 0.059(2) -0.0061(17) -0.0045(17) 0.0003(15) C45 0.065(2) 0.050(2) 0.081(3) -0.0142(19) 0.002(2) 0.0083(17) C46 0.066(2) 0.053(2) 0.078(3) -0.025(2) 0.003(2) -0.0046(18) C47 0.059(2) 0.070(3) 0.073(3) -0.020(2) -0.016(2) 0.0023(19) C48 0.056(2) 0.049(2) 0.073(3) -0.0125(18) -0.0102(19) 0.0072(16) C49 0.056(2) 0.0471(18) 0.0400(19) -0.0009(15) 0.0075(15) -0.0024(15) C50 0.061(2) 0.054(2) 0.043(2) 0.0015(16) 0.0047(17) -0.0007(16) C51 0.080(3) 0.058(2) 0.044(2) 0.0078(17) -0.003(2) -0.0070(19) C52 0.086(3) 0.068(2) 0.035(2) -0.0006(18) 0.0075(19) -0.011(2) C53 0.081(3) 0.060(2) 0.053(2) -0.0051(18) 0.024(2) -0.0055(19) C54 0.062(2) 0.054(2) 0.049(2) -0.0026(16) 0.0095(18) -0.0014(16) C55 0.067(2) 0.0436(18) 0.058(2) 0.0016(17) -0.0075(19) -0.0014(16) C56 0.066(3) 0.052(2) 0.099(4) 0.010(2) -0.002(2) -0.0025(18) C57 0.062(3) 0.065(3) 0.150(5) 0.007(3) -0.005(3) -0.002(2) C58 0.079(3) 0.057(3) 0.139(5) 0.026(3) -0.038(3) -0.002(2) C59 0.100(4) 0.059(3) 0.096(4) 0.026(2) -0.030(3) -0.011(2) C60 0.078(3) 0.051(2) 0.065(3) 0.0025(18) -0.009(2) -0.0071(19) C61 0.059(2) 0.051(2) 0.067(3) -0.0157(18) -0.0091(19) 0.0046(16) C62 0.067(3) 0.079(3) 0.056(3) -0.026(2) -0.004(2) 0.008(2) C63 0.079(3) 0.106(4) 0.065(3) -0.025(3) -0.007(2) 0.024(3) C64 0.084(3) 0.076(3) 0.108(4) -0.047(3) -0.038(3) 0.028(3) C65 0.093(4) 0.064(3) 0.117(5) -0.019(3) -0.027(3) -0.009(3) C66 0.100(4) 0.072(3) 0.075(3) -0.006(3) -0.012(3) -0.011(3) _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 F1A C32A 1.18(2) . ? F2A C33A 1.347(6) . ? F3A C34A 1.334(8) . ? F4A C35A 1.358(7) . ? F5A C36A 1.340(7) . ? F1B C32B 0.88(5) . ? F2B C33B 1.34(2) . ? F3B C34B 1.346(18) . ? F4B C35B 1.30(2) . ? F5B C36B 1.36(2) . ? F6 C38 1.338(4) . ? F7 C39 1.340(4) . ? F8 C40 1.333(5) . ? F9 C41 1.336(5) . ? F10 C42 1.343(4) . ? F11 C44 1.333(4) . ? F12 C45 1.339(4) . ? F13 C46 1.336(4) . ? F14 C47 1.340(4) . ? F15 C48 1.343(4) . ? F16 C50 1.347(4) . ? F17 C51 1.346(4) . ? F18 C52 1.351(4) . ? F19 C53 1.330(5) . ? F20 C54 1.346(4) . ? F21 C56 1.336(5) . ? F22 C57 1.341(6) . ? F23 C58 1.349(5) . ? F24 C59 1.347(5) . ? F25 C60 1.351(5) . ? F26 C62 1.310(5) . ? F27 C63 1.315(6) . ? F28 C64 1.340(5) . ? F29 C65 1.329(6) . ? F30 C66 1.378(6) . ? N1 C1 1.369(4) . ? N1 C4 1.383(5) . ? N1 H1 0.8800 . ? N2 C9 1.367(4) . ? N2 C6 1.369(4) . ? N2 H2 0.8800 . ? N3 C14 1.368(4) . ? N3 C11 1.370(4) . ? N3 H3 0.8800 . ? N4 C16 1.351(4) . ? N4 C19 1.392(4) . ? N5 C22 1.346(4) . ? N5 C21 1.377(4) . ? N5 H5 0.8800 . ? N6 C29 1.343(4) . ? N6 C26 1.401(4) . ? C1 C30 1.386(5) . ? C1 C2 1.449(5) . ? C2 C3 1.336(5) . ? C2 H2A 0.9500 . ? C3 C4 1.449(5) . ? C3 H3A 0.9500 . ? C4 C5 1.378(5) . ? C5 C6 1.426(5) . ? C5 C31A 1.469(7) . ? C5 C31B 1.583(13) . ? C6 C7 1.401(5) . ? C7 C8 1.381(5) . ? C7 H7 0.9500 . ? C8 C9 1.414(5) . ? C8 H8 0.9500 . ? C9 C10 1.433(5) . ? C10 C11 1.379(5) . ? C10 C37 1.500(5) . ? C11 C12 1.445(5) . ? C12 C13 1.352(5) . ? C12 H12 0.9500 . ? C13 C14 1.442(5) . ? C13 H13 0.9500 . ? C14 C15 1.389(5) . ? C15 C16 1.419(5) . ? C15 C43 1.499(5) . ? C16 C17 1.455(5) . ? C17 C18 1.343(5) . ? C17 H17 0.9500 . ? C18 C19 1.450(5) . ? C18 H18 0.9500 . ? C19 C20 1.377(5) . ? C20 C21 1.433(5) . ? C20 C49 1.486(5) . ? C21 C23 1.384(4) . ? C22 C24 1.392(5) . ? C22 H22 0.9500 . ? C23 C24 1.407(5) . ? C23 H23 0.9500 . ? C24 C25 1.448(5) . ? C25 C26 1.366(5) . ? C25 C55 1.502(5) . ? C26 C27 1.456(5) . ? C27 C28 1.340(5) . ? C27 H27 0.9500 . ? C28 C29 1.450(5) . ? C28 H28 0.9500 . ? C29 C30 1.430(5) . ? C30 C61 1.498(5) . ? C31A C36A 1.376(7) . ? C31A C32A 1.482(18) . ? C32A C33A 1.44(2) . ? C33A C34A 1.378(9) . ? C34A C35A 1.357(10) . ? C35A C36A 1.384(8) . ? C31B C32B 1.3900 . ? C31B C36B 1.3900 . ? C32B C33B 1.3900 . ? C33B C34B 1.3900 . ? C34B C35B 1.3900 . ? C35B C36B 1.3900 . ? C37 C42 1.376(6) . ? C37 C38 1.398(5) . ? C38 C39 1.374(5) . ? C39 C40 1.396(6) . ? C40 C41 1.377(6) . ? C41 C42 1.366(6) . ? C43 C48 1.381(5) . ? C43 C44 1.387(5) . ? C44 C45 1.373(5) . ? C45 C46 1.372(6) . ? C46 C47 1.370(6) . ? C47 C48 1.371(5) . ? C49 C50 1.375(5) . ? C49 C54 1.391(5) . ? C50 C51 1.393(5) . ? C51 C52 1.352(6) . ? C52 C53 1.378(6) . ? C53 C54 1.388(5) . ? C55 C56 1.379(6) . ? C55 C60 1.388(5) . ? C56 C57 1.395(6) . ? C57 C58 1.365(7) . ? C58 C59 1.394(8) . ? C59 C60 1.370(6) . ? C61 C66 1.342(6) . ? C61 C62 1.406(6) . ? C62 C63 1.407(6) . ? C63 C64 1.324(8) . ? C64 C65 1.386(9) . ? C65 C66 1.403(7) . ? 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 110.3(3) . . ? C1 N1 H1 124.8 . . ? C4 N1 H1 124.8 . . ? C9 N2 C6 112.0(3) . . ? C9 N2 H2 124.0 . . ? C6 N2 H2 124.0 . . ? C14 N3 C11 111.2(3) . . ? C14 N3 H3 124.4 . . ? C11 N3 H3 124.4 . . ? C16 N4 C19 105.9(3) . . ? C22 N5 C21 110.1(3) . . ? C22 N5 H5 124.9 . . ? C21 N5 H5 124.9 . . ? C29 N6 C26 105.7(3) . . ? N1 C1 C30 124.0(3) . . ? N1 C1 C2 106.6(3) . . ? C30 C1 C2 129.0(3) . . ? C3 C2 C1 108.0(3) . . ? C3 C2 H2A 126.0 . . ? C1 C2 H2A 126.0 . . ? C2 C3 C4 109.1(4) . . ? C2 C3 H3A 125.5 . . ? C4 C3 H3A 125.5 . . ? C5 C4 N1 125.9(3) . . ? C5 C4 C3 128.5(4) . . ? N1 C4 C3 105.6(3) . . ? C4 C5 C6 124.6(3) . . ? C4 C5 C31A 121.1(4) . . ? C6 C5 C31A 114.2(4) . . ? C4 C5 C31B 114.5(8) . . ? C6 C5 C31B 116.9(8) . . ? C31A C5 C31B 25.5(9) . . ? N2 C6 C7 106.0(3) . . ? N2 C6 C5 120.5(3) . . ? C7 C6 C5 133.1(3) . . ? C8 C7 C6 108.2(3) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? C7 C8 C9 108.5(3) . . ? C7 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? N2 C9 C8 105.3(3) . . ? N2 C9 C10 121.1(3) . . ? C8 C9 C10 133.5(3) . . ? C11 C10 C9 125.0(3) . . ? C11 C10 C37 117.1(3) . . ? C9 C10 C37 117.8(3) . . ? N3 C11 C10 125.2(3) . . ? N3 C11 C12 105.9(3) . . ? C10 C11 C12 128.3(3) . . ? C13 C12 C11 108.0(3) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? C12 C13 C14 108.6(3) . . ? C12 C13 H13 125.7 . . ? C14 C13 H13 125.7 . . ? N3 C14 C15 123.3(3) . . ? N3 C14 C13 105.9(3) . . ? C15 C14 C13 130.4(3) . . ? C14 C15 C16 121.5(3) . . ? C14 C15 C43 117.2(3) . . ? C16 C15 C43 120.1(3) . . ? N4 C16 C15 122.9(3) . . ? N4 C16 C17 110.5(3) . . ? C15 C16 C17 126.3(3) . . ? C18 C17 C16 107.1(3) . . ? C18 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? C17 C18 C19 106.7(3) . . ? C17 C18 H18 126.6 . . ? C19 C18 H18 126.6 . . ? C20 C19 N4 122.9(3) . . ? C20 C19 C18 127.4(3) . . ? N4 C19 C18 109.7(3) . . ? C19 C20 C21 124.4(3) . . ? C19 C20 C49 119.8(3) . . ? C21 C20 C49 115.7(3) . . ? N5 C21 C23 106.7(3) . . ? N5 C21 C20 122.0(3) . . ? C23 C21 C20 130.6(3) . . ? N5 C22 C24 108.5(3) . . ? N5 C22 H22 125.7 . . ? C24 C22 H22 125.7 . . ? C21 C23 C24 108.3(3) . . ? C21 C23 H23 125.8 . . ? C24 C23 H23 125.8 . . ? C22 C24 C23 106.3(3) . . ? C22 C24 C25 126.3(3) . . ? C23 C24 C25 126.8(3) . . ? C26 C25 C24 124.9(3) . . ? C26 C25 C55 118.4(3) . . ? C24 C25 C55 116.2(3) . . ? C25 C26 N6 123.7(3) . . ? C25 C26 C27 127.1(3) . . ? N6 C26 C27 109.1(3) . . ? C28 C27 C26 106.9(3) . . ? C28 C27 H27 126.6 . . ? C26 C27 H27 126.6 . . ? C27 C28 C29 106.9(3) . . ? C27 C28 H28 126.5 . . ? C29 C28 H28 126.5 . . ? N6 C29 C30 123.2(3) . . ? N6 C29 C28 111.2(3) . . ? C30 C29 C28 125.3(3) . . ? C1 C30 C29 122.4(3) . . ? C1 C30 C61 118.3(3) . . ? C29 C30 C61 118.5(3) . . ? C36A C31A C5 121.1(5) . . ? C36A C31A C32A 119.6(10) . . ? C5 C31A C32A 118.8(9) . . ? F1A C32A C33A 123.4(13) . . ? F1A C32A C31A 123.0(13) . . ? C33A C32A C31A 113.2(16) . . ? F2A C33A C34A 119.1(6) . . ? F2A C33A C32A 116.0(9) . . ? C34A C33A C32A 124.9(10) . . ? F3A C34A C35A 122.4(6) . . ? F3A C34A C33A 118.9(7) . . ? C35A C34A C33A 118.7(7) . . ? C34A C35A F4A 119.1(6) . . ? C34A C35A C36A 121.1(6) . . ? F4A C35A C36A 119.8(6) . . ? F5A C36A C31A 119.4(5) . . ? F5A C36A C35A 118.2(5) . . ? C31A C36A C35A 122.4(5) . . ? C32B C31B C36B 120.0 . . ? C32B C31B C5 113.0(14) . . ? C36B C31B C5 126.1(14) . . ? F1B C32B C33B 113(3) . . ? F1B C32B C31B 127(3) . . ? C33B C32B C31B 120.0 . . ? F2B C33B C32B 123(2) . . ? F2B C33B C34B 116(2) . . ? C32B C33B C34B 120.0 . . ? F3B C34B C33B 122.8(19) . . ? F3B C34B C35B 117.2(19) . . ? C33B C34B C35B 120.0 . . ? F4B C35B C36B 119.7(18) . . ? F4B C35B C34B 119.8(18) . . ? C36B C35B C34B 120.0 . . ? F5B C36B C35B 119.2(15) . . ? F5B C36B C31B 120.7(15) . . ? C35B C36B C31B 120.0 . . ? C42 C37 C38 116.0(4) . . ? C42 C37 C10 122.5(3) . . ? C38 C37 C10 121.5(3) . . ? F6 C38 C39 117.8(3) . . ? F6 C38 C37 119.7(3) . . ? C39 C38 C37 122.5(4) . . ? F7 C39 C38 120.6(4) . . ? F7 C39 C40 120.0(4) . . ? C38 C39 C40 119.3(4) . . ? F8 C40 C41 121.3(4) . . ? F8 C40 C39 119.7(4) . . ? C41 C40 C39 119.0(4) . . ? F9 C41 C42 121.0(4) . . ? F9 C41 C40 118.8(4) . . ? C42 C41 C40 120.2(4) . . ? F10 C42 C41 117.6(4) . . ? F10 C42 C37 119.3(4) . . ? C41 C42 C37 123.0(4) . . ? C48 C43 C44 116.8(3) . . ? C48 C43 C15 122.5(3) . . ? C44 C43 C15 120.7(3) . . ? F11 C44 C45 118.6(3) . . ? F11 C44 C43 119.7(3) . . ? C45 C44 C43 121.7(4) . . ? F12 C45 C46 120.0(3) . . ? F12 C45 C44 119.9(4) . . ? C46 C45 C44 120.0(4) . . ? F13 C46 C47 120.4(4) . . ? F13 C46 C45 120.3(4) . . ? C47 C46 C45 119.3(3) . . ? F14 C47 C46 119.3(4) . . ? F14 C47 C48 120.4(4) . . ? C46 C47 C48 120.3(4) . . ? F15 C48 C47 118.4(3) . . ? F15 C48 C43 119.7(3) . . ? C47 C48 C43 121.8(3) . . ? C50 C49 C54 116.8(3) . . ? C50 C49 C20 120.8(3) . . ? C54 C49 C20 122.4(3) . . ? F16 C50 C49 120.5(3) . . ? F16 C50 C51 117.4(3) . . ? C49 C50 C51 122.2(4) . . ? F17 C51 C52 120.9(4) . . ? F17 C51 C50 120.1(4) . . ? C52 C51 C50 119.1(4) . . ? F18 C52 C51 119.3(4) . . ? F18 C52 C53 119.2(4) . . ? C51 C52 C53 121.5(4) . . ? F19 C53 C52 120.8(4) . . ? F19 C53 C54 120.7(4) . . ? C52 C53 C54 118.4(4) . . ? F20 C54 C53 118.3(3) . . ? F20 C54 C49 119.6(3) . . ? C53 C54 C49 122.1(4) . . ? C56 C55 C60 117.7(4) . . ? C56 C55 C25 120.9(3) . . ? C60 C55 C25 121.4(4) . . ? F21 C56 C55 120.7(4) . . ? F21 C56 C57 117.7(4) . . ? C55 C56 C57 121.5(4) . . ? F22 C57 C58 120.4(5) . . ? F22 C57 C56 120.4(5) . . ? C58 C57 C56 119.2(5) . . ? F23 C58 C57 119.4(5) . . ? F23 C58 C59 120.1(5) . . ? C57 C58 C59 120.5(4) . . ? F24 C59 C60 120.7(5) . . ? F24 C59 C58 120.2(4) . . ? C60 C59 C58 119.1(4) . . ? F25 C60 C59 118.3(4) . . ? F25 C60 C55 119.8(4) . . ? C59 C60 C55 121.9(5) . . ? C66 C61 C62 116.3(4) . . ? C66 C61 C30 123.7(4) . . ? C62 C61 C30 120.0(4) . . ? F26 C62 C61 120.9(3) . . ? F26 C62 C63 119.2(5) . . ? C61 C62 C63 119.9(5) . . ? F27 C63 C64 118.7(5) . . ? F27 C63 C62 119.6(6) . . ? C64 C63 C62 121.7(5) . . ? C63 C64 F28 121.3(7) . . ? C63 C64 C65 120.1(5) . . ? F28 C64 C65 118.6(6) . . ? F29 C65 C64 122.0(5) . . ? F29 C65 C66 120.4(7) . . ? C64 C65 C66 117.6(5) . . ? C61 C66 F30 119.1(4) . . ? C61 C66 C65 124.4(6) . . ? F30 C66 C65 116.5(5) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 68.22 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.701 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.080 #=========================================================================== #== # End of CIF #=========================================================================== #== #=========================================================================== #== data___PdNCHex _database_code_depnum_ccdc_archive 'CCDC 846699' #TrackingRef '- cif_text_all.doc' #=========================================================================== #== # CHEMICAL DATA _chemical_formula_sum 'C73 H30 F30 N6 Pd ' _chemical_formula_moiety 'C66 H14 F30 N6 Pd, C7 H16 ' _chemical_formula_weight 1667.43 _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_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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, -z' _cell_length_a 7.6108(2) _cell_length_b 17.3675(8) _cell_length_c 24.9638(11) _cell_angle_alpha 101.727(3) _cell_angle_beta 90.851(2) _cell_angle_gamma 93.498(2) _cell_volume 3223.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8471 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 #--------------------------------------------------------------------------- #-- _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 0.427 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_T_max 0.958 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\Ya _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury-8' _diffrn_measurement_method \Yw _diffrn_detector_area_resol_mean 14.7059 _diffrn_reflns_number 34080 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 #=========================================================================== #== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 and Platon squeeze' _computing_publication_material 'CrystalStructure 3.8.2' _computing_molecular_graphics ? #=========================================================================== #== _reflns_number_total 14684 _reflns_number_gt 12112 _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. Positional coordinates of hydrogen atoms in the hexaphyrin molecule are refined and their Biso values are riding to the connected atoms. The coordinates of solvent hydrogen atoms are placed at the calculated positions with the riding thermal factors. The bond lengths, bond angles, and thermal factors of the solvent heptane are restrained with DFIX, DANG, DELU, ISOR, and SIMU commands. There is a solvent accessible boid where no electron peak is found. Therefore, the structures are refined without the effect of an unknown molecule by the Platon squeeze technique. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\Ys^2^(Fo^2^)+(0.0723P)^2^+4.9988P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0038(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\Yl^3^/sin(2\Yq)]^-1/4^ _refine_ls_number_reflns 14684 _refine_ls_number_parameters 1062 _refine_ls_number_restraints 161 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.692 _refine_diff_density_min -1.263 _refine_diff_density_rms 0.104 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 -0.057 0.000 0.000 100 6 ' ' 2 0.264 0.095 0.400 9 1 ' ' 3 0.736 0.905 0.600 9 1 ' ' _platon_squeeze_details ; ; 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 Pd1 Pd 0.62786(3) 0.723940(14) 0.311015(10) 0.02614(10) Uani 1 1 d . . . F1 F 0.9120(3) 0.7535(2) 0.11249(11) 0.0570(7) Uani 1 1 d . . . F2 F 0.9038(4) 0.7862(2) 0.01195(12) 0.0715(9) Uani 1 1 d . . . F3 F 0.5997(5) 0.82933(18) -0.02932(10) 0.0664(9) Uani 1 1 d . . . F4 F 0.3032(5) 0.8303(2) 0.02848(13) 0.0802(11) Uani 1 1 d . . . F5 F 0.3096(3) 0.79653(19) 0.12930(11) 0.0564(7) Uani 1 1 d . . . F6 F 0.9894(3) 0.50769(15) 0.15231(9) 0.0423(5) Uani 1 1 d . . . F7 F 1.2314(3) 0.47434(18) 0.07590(11) 0.0522(7) Uani 1 1 d . . . F8 F 1.1350(4) 0.39456(17) -0.02645(11) 0.0544(7) Uani 1 1 d . . . F9 F 0.7897(4) 0.35293(17) -0.05246(10) 0.0574(7) Uani 1 1 d . . . F10 F 0.5439(3) 0.38758(16) 0.02234(10) 0.0482(6) Uani 1 1 d . . . F11 F -0.0344(4) 0.27100(15) 0.09975(10) 0.0485(6) Uani 1 1 d . . . F12 F -0.2387(4) 0.13696(17) 0.08071(12) 0.0658(9) Uani 1 1 d . . . F13 F -0.3169(5) 0.06222(18) 0.16302(15) 0.0769(10) Uani 1 1 d . . . F14 F -0.1944(5) 0.1252(2) 0.26601(14) 0.0797(11) Uani 1 1 d . . . F15 F 0.0052(4) 0.26098(17) 0.28675(11) 0.0613(8) Uani 1 1 d . . . F16 F 0.1410(4) 0.64119(17) 0.22020(10) 0.0520(7) Uani 1 1 d . . . F17 F 0.0720(4) 0.7885(2) 0.21379(14) 0.0745(10) Uani 1 1 d . . . F18 F 0.1229(5) 0.90668(18) 0.30247(19) 0.0896(12) Uani 1 1 d . . . F19 F 0.2234(4) 0.87475(16) 0.40038(15) 0.0709(9) Uani 1 1 d . . . F20 F 0.2794(3) 0.72712(15) 0.40905(10) 0.0455(6) Uani 1 1 d . . . F21 F 1.0801(3) 0.58950(14) 0.41861(9) 0.0403(5) Uani 1 1 d . . . F22 F 1.2446(3) 0.54910(16) 0.50332(11) 0.0497(6) Uani 1 1 d . . . F23 F 1.1046(4) 0.58091(16) 0.60451(10) 0.0529(7) Uani 1 1 d . . . F24 F 0.8006(4) 0.65551(16) 0.61939(9) 0.0530(7) Uani 1 1 d . . . F25 F 0.6429(4) 0.70216(17) 0.53505(10) 0.0501(6) Uani 1 1 d . . . F26 F 0.9741(4) 1.03333(16) 0.34101(13) 0.0640(8) Uani 1 1 d . . . F27 F 0.9905(4) 1.18620(15) 0.38868(12) 0.0602(8) Uani 1 1 d . . . F28 F 0.7491(4) 1.24230(14) 0.46210(13) 0.0590(7) Uani 1 1 d . . . F29 F 0.4949(5) 1.14277(19) 0.49014(18) 0.0891(13) Uani 1 1 d . . . F30 F 0.4743(4) 0.98907(17) 0.44167(16) 0.0756(10) Uani 1 1 d . . . N1 N 0.6582(4) 0.81986(16) 0.27834(12) 0.0274(6) Uani 1 1 d . . . N2 N 0.5933(4) 0.65267(17) 0.23453(11) 0.0263(6) Uani 1 1 d . . . N3 N 0.3694(4) 0.41673(18) 0.17756(13) 0.0320(7) Uani 1 1 d . . . H3 H 0.328(6) 0.466(3) 0.1904(18) 0.038 Uiso 1 1 d . . . N4 N 0.1995(4) 0.46213(18) 0.27146(13) 0.0301(6) Uani 1 1 d . . . H4 H 0.299(6) 0.456(3) 0.2702(18) 0.036 Uiso 1 1 d . . . N5 N 0.5585(4) 0.63821(16) 0.35200(11) 0.0252(6) Uani 1 1 d . . . N6 N 0.7200(4) 0.78679(17) 0.38310(12) 0.0286(6) Uani 1 1 d . . . C1 C 0.6671(5) 0.8960(2) 0.30741(14) 0.0303(7) Uani 1 1 d . . . C2 C 0.6400(6) 0.9479(2) 0.27101(16) 0.0357(8) Uani 1 1 d . . . H2 H 0.637(6) 1.005(3) 0.2807(18) 0.043 Uiso 1 1 d . . . C3 C 0.6197(6) 0.9035(2) 0.21995(16) 0.0352(8) Uani 1 1 d . . . H3A H 0.601(6) 0.921(3) 0.1845(19) 0.042 Uiso 1 1 d . . . C4 C 0.6269(5) 0.8231(2) 0.22432(14) 0.0280(7) Uani 1 1 d . . . C5 C 0.6166(5) 0.7580(2) 0.18123(14) 0.0289(7) Uani 1 1 d . . . C6 C 0.6114(5) 0.6790(2) 0.18480(14) 0.0276(7) Uani 1 1 d . . . C7 C 0.6234(5) 0.6130(2) 0.14148(15) 0.0293(7) Uani 1 1 d . . . H7 H 0.640(6) 0.618(3) 0.1032(18) 0.035 Uiso 1 1 d . . . C8 C 0.6117(5) 0.5459(2) 0.16385(15) 0.0295(7) Uani 1 1 d . . . C9 C 0.5924(5) 0.57419(19) 0.22135(14) 0.0268(7) Uani 1 1 d . . . H9 H 0.582(5) 0.545(2) 0.2501(17) 0.032 Uiso 1 1 d . . . C10 C 0.6237(5) 0.4645(2) 0.13440(14) 0.0283(7) Uani 1 1 d . . . C11 C 0.5111(5) 0.4043(2) 0.14341(15) 0.0312(7) Uani 1 1 d . . . C12 C 0.5047(6) 0.3204(2) 0.12233(16) 0.0362(8) Uani 1 1 d . . . H12 H 0.595(6) 0.295(3) 0.0958(19) 0.043 Uiso 1 1 d . . . C13 C 0.3589(6) 0.2865(2) 0.14149(17) 0.0373(8) Uani 1 1 d . . . H13 H 0.317(6) 0.231(3) 0.1360(18) 0.045 Uiso 1 1 d . . . C14 C 0.2665(5) 0.3472(2) 0.17639(15) 0.0322(8) Uani 1 1 d . . . C15 C 0.1144(5) 0.3427(2) 0.20526(15) 0.0308(7) Uani 1 1 d . . . C16 C 0.0693(5) 0.4107(2) 0.24512(14) 0.0300(7) Uani 1 1 d . . . C17 C -0.0900(5) 0.4469(2) 0.25763(15) 0.0332(8) Uani 1 1 d . . . H17 H -0.207(6) 0.423(3) 0.2460(18) 0.040 Uiso 1 1 d . . . C18 C -0.0481(5) 0.5226(2) 0.28729(15) 0.0334(8) Uani 1 1 d . . . H18 H -0.128(6) 0.564(3) 0.3006(18) 0.040 Uiso 1 1 d . . . C19 C 0.1343(5) 0.5329(2) 0.29533(14) 0.0273(7) Uani 1 1 d . . . C20 C 0.2549(5) 0.5975(2) 0.31770(13) 0.0267(7) Uani 1 1 d . . . C21 C 0.4154(5) 0.5838(2) 0.34085(14) 0.0271(7) Uani 1 1 d . . . C22 C 0.4409(5) 0.5229(2) 0.37122(15) 0.0312(7) Uani 1 1 d . . . H22 H 0.365(6) 0.478(3) 0.3715(17) 0.037 Uiso 1 1 d . . . C23 C 0.5856(5) 0.5459(2) 0.40432(15) 0.0318(7) Uani 1 1 d . . . H23 H 0.628(6) 0.520(3) 0.4323(18) 0.038 Uiso 1 1 d . . . C24 C 0.6534(5) 0.6206(2) 0.39361(13) 0.0256(7) Uani 1 1 d . . . C25 C 0.7733(5) 0.6749(2) 0.42702(14) 0.0289(7) Uani 1 1 d . . . C26 C 0.7901(5) 0.7545(2) 0.42396(14) 0.0281(7) Uani 1 1 d . . . C27 C 0.8705(5) 0.8178(2) 0.46523(15) 0.0332(8) Uani 1 1 d . . . H27 H 0.925(6) 0.812(3) 0.4992(18) 0.040 Uiso 1 1 d . . . C28 C 0.8399(5) 0.8864(2) 0.45010(15) 0.0353(8) Uani 1 1 d . . . H28 H 0.874(6) 0.940(3) 0.4704(18) 0.042 Uiso 1 1 d . . . C29 C 0.7502(5) 0.8666(2) 0.39717(15) 0.0311(7) Uani 1 1 d . . . C30 C 0.7121(5) 0.9186(2) 0.36383(15) 0.0314(7) Uani 1 1 d . . . C31 C 0.6118(5) 0.7748(2) 0.12413(14) 0.0303(7) Uani 1 1 d . . . C32 C 0.7601(6) 0.7723(2) 0.09297(16) 0.0375(8) Uani 1 1 d . . . C33 C 0.7575(6) 0.7898(3) 0.04136(17) 0.0469(10) Uani 1 1 d . . . C34 C 0.6022(7) 0.8108(3) 0.02051(15) 0.0445(10) Uani 1 1 d . . . C35 C 0.4521(7) 0.8119(3) 0.04972(18) 0.0489(11) Uani 1 1 d . . . C36 C 0.4583(6) 0.7934(2) 0.10091(16) 0.0383(9) Uani 1 1 d . . . C37 C 0.7557(5) 0.4477(2) 0.09114(15) 0.0304(7) Uani 1 1 d . . . C38 C 0.9349(5) 0.4698(2) 0.10238(15) 0.0329(8) Uani 1 1 d . . . C39 C 1.0613(5) 0.4520(2) 0.06372(17) 0.0375(8) Uani 1 1 d . . . C40 C 1.0122(6) 0.4114(2) 0.01159(17) 0.0401(9) Uani 1 1 d . . . C41 C 0.8386(6) 0.3901(2) -0.00140(16) 0.0408(9) Uani 1 1 d . . . C42 C 0.7132(5) 0.4084(2) 0.03783(16) 0.0370(8) Uani 1 1 d . . . C43 C -0.0048(5) 0.2707(2) 0.19410(15) 0.0336(8) Uani 1 1 d . . . C44 C -0.0705(6) 0.2362(2) 0.14182(16) 0.0368(8) Uani 1 1 d . . . C45 C -0.1767(6) 0.1676(2) 0.13154(18) 0.0451(10) Uani 1 1 d . . . C46 C -0.2172(7) 0.1298(3) 0.1729(2) 0.0524(12) Uani 1 1 d . . . C47 C -0.1567(7) 0.1619(3) 0.2251(2) 0.0547(12) Uani 1 1 d . . . C48 C -0.0529(6) 0.2314(3) 0.23535(17) 0.0448(10) Uani 1 1 d . . . C49 C 0.2118(5) 0.6782(2) 0.31470(15) 0.0309(7) Uani 1 1 d . . . C50 C 0.1554(5) 0.6972(3) 0.26607(18) 0.0405(9) Uani 1 1 d . . . C51 C 0.1236(6) 0.7728(3) 0.2614(2) 0.0484(11) Uani 1 1 d . . . C52 C 0.1488(7) 0.8326(3) 0.3066(3) 0.0595(14) Uani 1 1 d . . . C53 C 0.2009(6) 0.8168(2) 0.3564(2) 0.0488(11) Uani 1 1 d . . . C54 C 0.2301(5) 0.7401(2) 0.36022(17) 0.0367(8) Uani 1 1 d . . . C55 C 0.8597(5) 0.6500(2) 0.47423(14) 0.0295(7) Uani 1 1 d . . . C56 C 1.0113(5) 0.6095(2) 0.46806(15) 0.0319(7) Uani 1 1 d . . . C57 C 1.0965(5) 0.5870(2) 0.51116(16) 0.0360(8) Uani 1 1 d . . . C58 C 1.0246(6) 0.6033(2) 0.56236(16) 0.0386(9) Uani 1 1 d . . . C59 C 0.8706(6) 0.6416(2) 0.56989(14) 0.0368(9) Uani 1 1 d . . . C60 C 0.7921(5) 0.6645(2) 0.52588(15) 0.0343(8) Uani 1 1 d . . . C61 C 0.7235(5) 1.0051(2) 0.38922(15) 0.0338(8) Uani 1 1 d . . . C62 C 0.8535(6) 1.0582(2) 0.37748(16) 0.0376(8) Uani 1 1 d . . . C63 C 0.8612(6) 1.1374(2) 0.40149(16) 0.0389(9) Uani 1 1 d . . . C64 C 0.7401(6) 1.1657(2) 0.43850(19) 0.0433(10) Uani 1 1 d . . . C65 C 0.6123(7) 1.1151(3) 0.4531(2) 0.0542(12) Uani 1 1 d . . . C66 C 0.6039(6) 1.0361(3) 0.4275(2) 0.0492(11) Uani 1 1 d . . . C67 C 0.547(2) 0.2864(9) 0.3288(8) 0.135(5) Uani 0.755(14) 1 d PDU A 1 H67A H 0.5583 0.3097 0.3679 0.202 Uiso 0.755(14) 1 calc PR A 1 H67B H 0.4820 0.3207 0.3101 0.202 Uiso 0.755(14) 1 calc PR A 1 H67C H 0.6644 0.2806 0.3135 0.202 Uiso 0.755(14) 1 calc PR A 1 C68 C 0.4429(11) 0.2017(5) 0.3203(3) 0.111(2) Uani 0.755(14) 1 d PDU A 1 H68A H 0.5198 0.1632 0.3312 0.133 Uiso 0.755(14) 1 calc PR A 1 H68B H 0.3379 0.2048 0.3434 0.133 Uiso 0.755(14) 1 calc PR A 1 C69 C 0.3869(10) 0.1750(5) 0.2603(3) 0.101(2) Uani 0.755(14) 1 d PDU A 1 H69A H 0.4930 0.1708 0.2377 0.122 Uiso 0.755(14) 1 calc PR A 1 H69B H 0.3152 0.2152 0.2494 0.122 Uiso 0.755(14) 1 calc PR A 1 C70 C 0.2798(10) 0.0953(5) 0.2490(3) 0.0957(19) Uani 0.755(14) 1 d PDU A 1 H70A H 0.3495 0.0560 0.2619 0.115 Uiso 0.755(14) 1 calc PR A 1 H70B H 0.1712 0.1005 0.2704 0.115 Uiso 0.755(14) 1 calc PR A 1 C71 C 0.2294(11) 0.0651(5) 0.1891(4) 0.107(2) Uani 0.755(14) 1 d PDU A 1 H71A H 0.1576 0.1042 0.1768 0.128 Uiso 0.755(14) 1 calc PR A 1 H71B H 0.3384 0.0621 0.1678 0.128 Uiso 0.755(14) 1 calc PR A 1 C72 C 0.130(2) -0.0128(8) 0.1754(6) 0.114(4) Uani 0.755(14) 1 d PDU A 1 H72A H 0.0267 -0.0125 0.1990 0.137 Uiso 0.755(14) 1 calc PR A 1 H72B H 0.2062 -0.0540 0.1827 0.137 Uiso 0.755(14) 1 calc PR A 1 C73 C 0.0696(18) -0.0317(7) 0.1160(5) 0.137(5) Uani 0.755(14) 1 d PDU A 1 H73A H -0.0016 -0.0818 0.1084 0.206 Uiso 0.755(14) 1 calc PR A 1 H73B H 0.1724 -0.0358 0.0926 0.206 Uiso 0.755(14) 1 calc PR A 1 H73C H -0.0013 0.0103 0.1084 0.206 Uiso 0.755(14) 1 calc PR A 1 C67A C 0.523(5) 0.3274(19) 0.2940(15) 0.114(7) Uani 0.245(14) 1 d PDU A 2 H67D H 0.5457 0.3825 0.3129 0.171 Uiso 0.245(14) 1 calc PR A 2 H67E H 0.3974 0.3172 0.2842 0.171 Uiso 0.245(14) 1 calc PR A 2 H67F H 0.5920 0.3174 0.2607 0.171 Uiso 0.245(14) 1 calc PR A 2 C68A C 0.577(7) 0.272(2) 0.332(2) 0.118(5) Uani 0.245(14) 1 d PDU A 2 H68C H 0.6977 0.2551 0.3247 0.178 Uiso 0.245(14) 1 calc PR A 2 H68D H 0.5737 0.2993 0.3713 0.178 Uiso 0.245(14) 1 calc PR A 2 C69A C 0.4429(11) 0.2017(5) 0.3203(3) 0.111(2) Uani 0.245(14) 1 d PD A 2 H69C H 0.4931 0.1569 0.3328 0.133 Uiso 0.245(14) 1 calc PR A 2 H69D H 0.3369 0.2152 0.3418 0.133 Uiso 0.245(14) 1 calc PR A 2 C70A C 0.3869(10) 0.1750(5) 0.2603(3) 0.101(2) Uani 0.245(14) 1 d PD A 2 H70C H 0.4930 0.1708 0.2377 0.122 Uiso 0.245(14) 1 calc PR A 2 H70D H 0.3152 0.2152 0.2494 0.122 Uiso 0.245(14) 1 calc PR A 2 C71A C 0.2798(10) 0.0953(5) 0.2490(3) 0.0957(19) Uani 0.245(14) 1 d PD A 2 H71C H 0.3495 0.0560 0.2619 0.115 Uiso 0.245(14) 1 calc PR A 2 H71D H 0.1712 0.1005 0.2704 0.115 Uiso 0.245(14) 1 calc PR A 2 C72A C 0.2294(11) 0.0651(5) 0.1891(4) 0.107(2) Uani 0.245(14) 1 d PD A 2 H72C H 0.3342 0.0475 0.1682 0.128 Uiso 0.245(14) 1 calc PR A 2 H72D H 0.1797 0.1074 0.1734 0.128 Uiso 0.245(14) 1 calc PR A 2 C73A C 0.090(5) -0.005(2) 0.1857(18) 0.106(8) Uani 0.245(14) 1 d PDU A 2 H73D H -0.0028 0.0103 0.2118 0.127 Uiso 0.245(14) 1 calc PR A 2 H73E H 0.1464 -0.0504 0.1945 0.127 Uiso 0.245(14) 1 calc PR A 2 H73F H 0.0379 -0.0195 0.1486 0.127 Uiso 0.245(14) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03135(16) 0.02236(15) 0.02440(15) 0.00506(10) -0.00099(10) -0.00116(10) F1 0.0406(14) 0.087(2) 0.0467(15) 0.0192(14) 0.0037(11) 0.0092(14) F2 0.067(2) 0.102(3) 0.0490(17) 0.0239(16) 0.0255(14) -0.0025(18) F3 0.108(3) 0.0646(19) 0.0299(13) 0.0189(12) -0.0019(14) -0.0010(17) F4 0.076(2) 0.122(3) 0.0538(18) 0.0373(19) -0.0134(16) 0.033(2) F5 0.0410(14) 0.086(2) 0.0462(15) 0.0189(14) 0.0054(11) 0.0138(14) F6 0.0385(12) 0.0546(15) 0.0321(12) 0.0071(10) -0.0014(9) -0.0046(11) F7 0.0321(12) 0.0754(19) 0.0539(15) 0.0237(14) 0.0073(11) 0.0052(12) F8 0.0591(16) 0.0574(17) 0.0490(15) 0.0108(12) 0.0293(13) 0.0150(13) F9 0.0706(18) 0.0609(17) 0.0319(13) -0.0094(11) 0.0117(12) -0.0036(14) F10 0.0455(14) 0.0559(16) 0.0369(13) -0.0021(11) 0.0001(11) -0.0074(12) F11 0.0663(17) 0.0449(14) 0.0340(12) 0.0109(10) -0.0039(11) -0.0069(12) F12 0.085(2) 0.0491(16) 0.0560(17) 0.0026(13) -0.0299(16) -0.0194(15) F13 0.088(2) 0.0461(17) 0.092(2) 0.0189(16) -0.0258(19) -0.0367(16) F14 0.105(3) 0.068(2) 0.072(2) 0.0423(17) -0.0068(19) -0.0370(19) F15 0.085(2) 0.0606(18) 0.0376(14) 0.0188(12) -0.0111(13) -0.0276(15) F16 0.0625(17) 0.0572(16) 0.0369(13) 0.0147(11) -0.0118(12) -0.0044(13) F17 0.067(2) 0.088(2) 0.087(2) 0.059(2) -0.0067(17) 0.0164(17) F18 0.081(2) 0.0408(17) 0.160(4) 0.043(2) 0.024(2) 0.0240(16) F19 0.0624(19) 0.0348(15) 0.102(2) -0.0179(15) 0.0148(17) 0.0010(13) F20 0.0504(14) 0.0437(14) 0.0355(12) -0.0058(10) 0.0010(10) -0.0037(11) F21 0.0446(13) 0.0451(13) 0.0349(12) 0.0141(10) 0.0068(10) 0.0109(10) F22 0.0436(14) 0.0540(16) 0.0584(16) 0.0249(12) -0.0026(12) 0.0134(12) F23 0.0726(18) 0.0531(16) 0.0365(13) 0.0202(11) -0.0192(12) 0.0006(13) F24 0.080(2) 0.0530(16) 0.0259(12) 0.0083(10) 0.0040(12) 0.0052(14) F25 0.0547(15) 0.0603(17) 0.0390(13) 0.0126(11) 0.0119(11) 0.0214(13) F26 0.081(2) 0.0363(14) 0.0687(19) -0.0007(13) 0.0342(16) -0.0105(13) F27 0.077(2) 0.0322(13) 0.0659(18) 0.0024(12) 0.0190(15) -0.0186(13) F28 0.0698(19) 0.0252(12) 0.0753(19) -0.0039(12) 0.0033(15) -0.0018(12) F29 0.077(2) 0.0449(18) 0.131(3) -0.0182(19) 0.052(2) -0.0027(15) F30 0.0628(19) 0.0398(15) 0.114(3) -0.0051(16) 0.0382(19) -0.0143(13) N1 0.0361(16) 0.0207(13) 0.0255(14) 0.0067(11) -0.0022(12) -0.0021(11) N2 0.0302(15) 0.0245(14) 0.0244(14) 0.0064(11) 0.0003(11) -0.0007(11) N3 0.0354(16) 0.0233(14) 0.0350(16) 0.0011(12) 0.0097(13) -0.0017(12) N4 0.0267(15) 0.0272(15) 0.0347(16) 0.0028(12) 0.0013(13) -0.0005(12) N5 0.0311(15) 0.0224(13) 0.0226(13) 0.0066(10) -0.0016(11) -0.0013(11) N6 0.0389(16) 0.0211(14) 0.0261(14) 0.0068(11) -0.0052(12) -0.0014(12) C1 0.040(2) 0.0191(15) 0.0301(18) 0.0025(13) -0.0035(15) -0.0022(14) C2 0.050(2) 0.0230(17) 0.0343(19) 0.0082(14) -0.0045(17) -0.0011(16) C3 0.051(2) 0.0233(17) 0.0306(18) 0.0078(14) -0.0076(16) -0.0056(15) C4 0.0361(18) 0.0232(16) 0.0266(17) 0.0103(13) -0.0024(14) -0.0003(13) C5 0.0319(17) 0.0293(17) 0.0265(17) 0.0083(13) 0.0026(14) 0.0008(14) C6 0.0311(17) 0.0278(17) 0.0240(16) 0.0069(13) 0.0023(13) -0.0026(13) C7 0.0342(18) 0.0262(17) 0.0274(17) 0.0056(13) 0.0025(14) -0.0006(14) C8 0.0284(17) 0.0277(17) 0.0322(18) 0.0060(14) 0.0029(14) -0.0013(13) C9 0.0325(17) 0.0196(15) 0.0265(17) 0.0019(12) 0.0016(13) -0.0028(13) C10 0.0323(18) 0.0249(16) 0.0281(17) 0.0057(13) 0.0058(14) 0.0039(13) C11 0.0369(19) 0.0262(17) 0.0293(17) 0.0030(13) 0.0046(14) 0.0020(14) C12 0.044(2) 0.0244(18) 0.038(2) 0.0010(14) 0.0061(17) -0.0002(15) C13 0.046(2) 0.0256(18) 0.039(2) 0.0047(15) 0.0033(17) -0.0004(16) C14 0.041(2) 0.0246(17) 0.0300(18) 0.0041(13) 0.0008(15) -0.0021(14) C15 0.0341(18) 0.0260(17) 0.0305(18) 0.0032(13) 0.0010(14) -0.0035(14) C16 0.0346(18) 0.0266(17) 0.0281(17) 0.0068(13) -0.0017(14) -0.0060(14) C17 0.0295(18) 0.038(2) 0.0303(18) 0.0049(15) 0.0012(14) -0.0050(15) C18 0.0294(18) 0.037(2) 0.0315(19) 0.0028(15) -0.0004(14) -0.0004(15) C19 0.0290(17) 0.0278(17) 0.0249(16) 0.0058(13) 0.0034(13) -0.0009(13) C20 0.0315(17) 0.0262(16) 0.0218(15) 0.0036(12) 0.0018(13) 0.0008(13) C21 0.0289(17) 0.0242(16) 0.0270(16) 0.0051(13) -0.0011(13) -0.0065(13) C22 0.0382(19) 0.0238(17) 0.0325(18) 0.0082(14) 0.0037(15) 0.0011(14) C23 0.040(2) 0.0266(17) 0.0293(18) 0.0089(14) -0.0019(15) -0.0001(15) C24 0.0324(17) 0.0240(16) 0.0217(15) 0.0081(12) 0.0002(13) 0.0019(13) C25 0.0328(18) 0.0273(17) 0.0272(17) 0.0073(13) 0.0029(14) 0.0000(14) C26 0.0308(17) 0.0293(17) 0.0232(16) 0.0036(13) -0.0015(13) 0.0018(13) C27 0.039(2) 0.0287(18) 0.0306(18) 0.0046(14) -0.0042(15) -0.0034(15) C28 0.045(2) 0.0254(18) 0.0311(19) -0.0008(14) -0.0045(16) -0.0055(15) C29 0.0380(19) 0.0241(17) 0.0288(17) 0.0018(13) -0.0036(14) -0.0037(14) C30 0.0333(18) 0.0251(17) 0.0350(19) 0.0062(14) -0.0031(15) -0.0034(14) C31 0.0397(19) 0.0243(16) 0.0259(17) 0.0043(13) -0.0026(14) -0.0014(14) C32 0.043(2) 0.040(2) 0.0300(19) 0.0074(15) 0.0004(16) 0.0044(17) C33 0.058(3) 0.046(2) 0.035(2) 0.0076(18) 0.0117(19) -0.009(2) C34 0.074(3) 0.039(2) 0.0207(18) 0.0081(15) -0.0016(18) -0.001(2) C35 0.064(3) 0.053(3) 0.033(2) 0.0144(19) -0.008(2) 0.010(2) C36 0.043(2) 0.040(2) 0.0320(19) 0.0063(16) 0.0007(16) 0.0042(17) C37 0.0346(18) 0.0252(16) 0.0322(18) 0.0071(13) 0.0059(15) 0.0032(14) C38 0.037(2) 0.0318(18) 0.0306(18) 0.0085(14) 0.0012(15) 0.0037(15) C39 0.0334(19) 0.042(2) 0.041(2) 0.0164(17) 0.0065(16) 0.0066(16) C40 0.044(2) 0.040(2) 0.040(2) 0.0117(17) 0.0174(18) 0.0152(17) C41 0.054(3) 0.035(2) 0.0307(19) 0.0005(15) 0.0093(17) 0.0064(18) C42 0.039(2) 0.036(2) 0.0336(19) 0.0027(15) 0.0009(16) -0.0011(16) C43 0.039(2) 0.0284(18) 0.0333(19) 0.0080(14) -0.0011(15) -0.0042(15) C44 0.045(2) 0.0306(19) 0.035(2) 0.0083(15) -0.0026(16) -0.0024(16) C45 0.054(3) 0.032(2) 0.046(2) 0.0052(17) -0.016(2) -0.0051(18) C46 0.057(3) 0.036(2) 0.063(3) 0.013(2) -0.011(2) -0.016(2) C47 0.066(3) 0.050(3) 0.050(3) 0.024(2) -0.003(2) -0.020(2) C48 0.058(3) 0.040(2) 0.036(2) 0.0117(17) -0.0058(19) -0.0134(19) C49 0.0286(17) 0.0297(18) 0.0340(19) 0.0066(14) -0.0010(14) -0.0016(14) C50 0.036(2) 0.041(2) 0.046(2) 0.0166(18) -0.0052(17) -0.0025(17) C51 0.040(2) 0.047(3) 0.066(3) 0.028(2) 0.000(2) 0.0076(19) C52 0.047(3) 0.037(2) 0.104(4) 0.031(3) 0.012(3) 0.014(2) C53 0.035(2) 0.029(2) 0.076(3) -0.003(2) 0.012(2) 0.0005(16) C54 0.0306(18) 0.0324(19) 0.044(2) 0.0005(16) 0.0039(16) -0.0026(15) C55 0.0358(18) 0.0251(16) 0.0263(17) 0.0039(13) -0.0048(14) -0.0020(14) C56 0.0375(19) 0.0284(17) 0.0298(18) 0.0064(14) 0.0004(15) 0.0001(14) C57 0.036(2) 0.0337(19) 0.040(2) 0.0125(16) -0.0065(16) 0.0000(15) C58 0.053(2) 0.0314(19) 0.0314(19) 0.0106(15) -0.0158(17) -0.0069(17) C59 0.057(2) 0.0326(19) 0.0196(16) 0.0030(13) 0.0023(16) -0.0024(17) C60 0.041(2) 0.0338(19) 0.0285(18) 0.0063(14) 0.0021(15) 0.0016(16) C61 0.044(2) 0.0241(17) 0.0320(18) 0.0038(14) -0.0013(16) 0.0005(15) C62 0.049(2) 0.0286(18) 0.0331(19) 0.0029(15) 0.0037(17) -0.0023(16) C63 0.053(2) 0.0265(18) 0.036(2) 0.0070(15) -0.0016(17) -0.0099(16) C64 0.053(3) 0.0219(18) 0.052(2) 0.0019(16) -0.005(2) -0.0018(17) C65 0.052(3) 0.032(2) 0.071(3) -0.006(2) 0.014(2) 0.0025(19) C66 0.045(2) 0.031(2) 0.068(3) 0.004(2) 0.008(2) -0.0083(18) C67 0.089(7) 0.168(8) 0.131(8) -0.010(8) 0.029(6) 0.012(7) C68 0.098(4) 0.140(5) 0.094(4) 0.012(4) 0.015(4) 0.037(4) C69 0.075(4) 0.130(5) 0.099(4) 0.021(4) 0.011(3) 0.017(4) C70 0.081(4) 0.110(4) 0.106(4) 0.039(4) 0.004(3) 0.030(3) C71 0.090(4) 0.110(4) 0.123(4) 0.027(4) 0.001(4) 0.015(4) C72 0.105(6) 0.094(5) 0.144(6) 0.023(5) -0.001(5) 0.026(5) C73 0.134(9) 0.099(8) 0.154(8) -0.032(7) -0.011(8) 0.003(7) C67A 0.090(12) 0.142(12) 0.105(12) 0.013(9) 0.013(10) 0.005(11) C68A 0.102(8) 0.141(8) 0.109(7) 0.013(6) 0.011(7) 0.020(7) C69A 0.098(4) 0.140(5) 0.094(4) 0.012(4) 0.015(4) 0.037(4) C70A 0.075(4) 0.130(5) 0.099(4) 0.021(4) 0.011(3) 0.017(4) C71A 0.081(4) 0.110(4) 0.106(4) 0.039(4) 0.004(3) 0.030(3) C72A 0.090(4) 0.110(4) 0.123(4) 0.027(4) 0.001(4) 0.015(4) C73A 0.109(12) 0.080(11) 0.136(12) 0.037(10) 0.011(11) 0.019(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 Pd1 N6 1.998(3) . ? Pd1 N1 2.001(3) . ? Pd1 N5 2.020(3) . ? Pd1 N2 2.057(3) . ? F1 C32 1.333(5) . ? F2 C33 1.341(5) . ? F3 C34 1.347(4) . ? F4 C35 1.328(5) . ? F5 C36 1.343(5) . ? F6 C38 1.333(4) . ? F7 C39 1.340(5) . ? F8 C40 1.344(4) . ? F9 C41 1.342(5) . ? F10 C42 1.346(5) . ? F11 C44 1.337(4) . ? F12 C45 1.339(5) . ? F13 C46 1.335(5) . ? F14 C47 1.335(5) . ? F15 C48 1.339(5) . ? F16 C50 1.342(5) . ? F17 C51 1.333(5) . ? F18 C52 1.337(5) . ? F19 C53 1.331(5) . ? F20 C54 1.336(5) . ? F21 C56 1.337(4) . ? F22 C57 1.337(5) . ? F23 C58 1.344(4) . ? F24 C59 1.335(4) . ? F25 C60 1.344(5) . ? F26 C62 1.331(5) . ? F27 C63 1.344(5) . ? F28 C64 1.339(4) . ? F29 C65 1.335(6) . ? F30 C66 1.340(5) . ? N1 C1 1.369(4) . ? N1 C4 1.379(4) . ? N2 C9 1.335(4) . ? N2 C6 1.413(4) . ? N3 C11 1.385(5) . ? N3 C14 1.394(5) . ? N3 H3 0.93(5) . ? N4 C16 1.359(4) . ? N4 C19 1.377(5) . ? N4 H4 0.77(5) . ? N5 C24 1.352(4) . ? N5 C21 1.384(4) . ? N6 C29 1.364(4) . ? N6 C26 1.376(4) . ? C1 C30 1.414(5) . ? C1 C2 1.426(5) . ? C2 C3 1.350(5) . ? C2 H2 0.97(5) . ? C3 C4 1.427(5) . ? C3 H3A 1.01(5) . ? C4 C5 1.391(5) . ? C5 C6 1.392(5) . ? C5 C31 1.512(5) . ? C6 C7 1.415(5) . ? C7 C8 1.390(5) . ? C7 H7 0.99(4) . ? C8 C9 1.433(5) . ? C8 C10 1.463(5) . ? C9 H9 0.97(4) . ? C10 C11 1.367(5) . ? C10 C37 1.484(5) . ? C11 C12 1.444(5) . ? C12 C13 1.362(6) . ? C12 H12 1.02(5) . ? C13 C14 1.449(5) . ? C13 H13 0.98(5) . ? C14 C15 1.379(5) . ? C15 C16 1.444(5) . ? C15 C43 1.474(5) . ? C16 C17 1.410(5) . ? C17 C18 1.387(5) . ? C17 H17 0.97(5) . ? C18 C19 1.395(5) . ? C18 H18 0.99(5) . ? C19 C20 1.420(5) . ? C20 C21 1.398(5) . ? C20 C49 1.476(5) . ? C21 C22 1.440(5) . ? C22 C23 1.357(5) . ? C22 H22 0.94(5) . ? C23 C24 1.443(5) . ? C23 H23 0.97(4) . ? C24 C25 1.404(5) . ? C25 C26 1.399(5) . ? C25 C55 1.492(5) . ? C26 C27 1.443(5) . ? C27 C28 1.353(5) . ? C27 H27 0.97(5) . ? C28 C29 1.446(5) . ? C28 H28 0.98(5) . ? C29 C30 1.386(5) . ? C30 C61 1.504(5) . ? C31 C32 1.378(6) . ? C31 C36 1.382(5) . ? C32 C33 1.382(6) . ? C33 C34 1.383(7) . ? C34 C35 1.364(7) . ? C35 C36 1.380(6) . ? C37 C42 1.390(5) . ? C37 C38 1.402(5) . ? C38 C39 1.377(5) . ? C39 C40 1.382(6) . ? C40 C41 1.366(6) . ? C41 C42 1.382(6) . ? C43 C48 1.389(5) . ? C43 C44 1.392(5) . ? C44 C45 1.376(6) . ? C45 C46 1.362(7) . ? C46 C47 1.369(7) . ? C47 C48 1.378(6) . ? C49 C50 1.390(5) . ? C49 C54 1.395(5) . ? C50 C51 1.375(6) . ? C51 C52 1.372(8) . ? C52 C53 1.383(8) . ? C53 C54 1.386(6) . ? C55 C60 1.376(5) . ? C55 C56 1.382(5) . ? C56 C57 1.382(5) . ? C57 C58 1.381(6) . ? C58 C59 1.379(6) . ? C59 C60 1.382(5) . ? C61 C66 1.382(6) . ? C61 C62 1.387(5) . ? C62 C63 1.382(5) . ? C63 C64 1.356(6) . ? C64 C65 1.373(7) . ? C65 C66 1.387(6) . ? C67 C68 1.601(13) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.520(9) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.535(10) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.518(10) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.481(13) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.512(15) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C67A C68A 1.56(2) . ? C67A H67D 0.9800 . ? C67A H67E 0.9800 . ? C67A H67F 0.9800 . ? C68A H68C 0.9900 . ? C68A H68D 0.9900 . ? C73A H73D 0.9800 . ? C73A H73E 0.9800 . ? C73A H73F 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 N6 Pd1 N1 90.00(12) . . ? N6 Pd1 N5 86.23(11) . . ? N1 Pd1 N5 168.75(12) . . ? N6 Pd1 N2 166.57(12) . . ? N1 Pd1 N2 91.07(11) . . ? N5 Pd1 N2 95.06(11) . . ? C1 N1 C4 106.7(3) . . ? C1 N1 Pd1 125.0(2) . . ? C4 N1 Pd1 126.2(2) . . ? C9 N2 C6 105.9(3) . . ? C9 N2 Pd1 127.8(2) . . ? C6 N2 Pd1 124.6(2) . . ? C11 N3 C14 111.6(3) . . ? C11 N3 H3 123(3) . . ? C14 N3 H3 123(3) . . ? C16 N4 C19 111.1(3) . . ? C16 N4 H4 125(3) . . ? C19 N4 H4 123(3) . . ? C24 N5 C21 107.5(3) . . ? C24 N5 Pd1 125.1(2) . . ? C21 N5 Pd1 127.3(2) . . ? C29 N6 C26 108.3(3) . . ? C29 N6 Pd1 126.9(2) . . ? C26 N6 Pd1 124.1(2) . . ? N1 C1 C30 124.4(3) . . ? N1 C1 C2 109.3(3) . . ? C30 C1 C2 126.0(3) . . ? C3 C2 C1 107.5(3) . . ? C3 C2 H2 126(3) . . ? C1 C2 H2 127(3) . . ? C2 C3 C4 107.4(3) . . ? C2 C3 H3A 128(3) . . ? C4 C3 H3A 124(3) . . ? N1 C4 C5 124.5(3) . . ? N1 C4 C3 109.0(3) . . ? C5 C4 C3 126.3(3) . . ? C4 C5 C6 127.2(3) . . ? C4 C5 C31 116.5(3) . . ? C6 C5 C31 116.3(3) . . ? C5 C6 N2 123.5(3) . . ? C5 C6 C7 127.4(3) . . ? N2 C6 C7 109.1(3) . . ? C8 C7 C6 107.6(3) . . ? C8 C7 H7 130(3) . . ? C6 C7 H7 123(3) . . ? C7 C8 C9 105.1(3) . . ? C7 C8 C10 126.6(3) . . ? C9 C8 C10 128.3(3) . . ? N2 C9 C8 112.2(3) . . ? N2 C9 H9 119(2) . . ? C8 C9 H9 129(2) . . ? C11 C10 C8 122.2(3) . . ? C11 C10 C37 118.9(3) . . ? C8 C10 C37 118.8(3) . . ? C10 C11 N3 122.5(3) . . ? C10 C11 C12 131.9(3) . . ? N3 C11 C12 105.6(3) . . ? C13 C12 C11 108.7(3) . . ? C13 C12 H12 129(3) . . ? C11 C12 H12 122(3) . . ? C12 C13 C14 109.1(3) . . ? C12 C13 H13 130(3) . . ? C14 C13 H13 121(3) . . ? C15 C14 N3 124.0(3) . . ? C15 C14 C13 131.1(3) . . ? N3 C14 C13 104.9(3) . . ? C14 C15 C16 119.1(3) . . ? C14 C15 C43 120.7(3) . . ? C16 C15 C43 120.2(3) . . ? N4 C16 C17 106.4(3) . . ? N4 C16 C15 119.5(3) . . ? C17 C16 C15 133.0(3) . . ? C18 C17 C16 107.6(3) . . ? C18 C17 H17 127(3) . . ? C16 C17 H17 126(3) . . ? C17 C18 C19 108.5(3) . . ? C17 C18 H18 128(3) . . ? C19 C18 H18 123(3) . . ? N4 C19 C18 106.1(3) . . ? N4 C19 C20 118.8(3) . . ? C18 C19 C20 135.0(3) . . ? C21 C20 C19 119.7(3) . . ? C21 C20 C49 120.6(3) . . ? C19 C20 C49 119.6(3) . . ? N5 C21 C20 124.6(3) . . ? N5 C21 C22 108.0(3) . . ? C20 C21 C22 125.0(3) . . ? C23 C22 C21 107.5(3) . . ? C23 C22 H22 125(3) . . ? C21 C22 H22 127(3) . . ? C22 C23 C24 106.8(3) . . ? C22 C23 H23 126(3) . . ? C24 C23 H23 126(3) . . ? N5 C24 C25 123.3(3) . . ? N5 C24 C23 109.3(3) . . ? C25 C24 C23 126.2(3) . . ? C26 C25 C24 122.4(3) . . ? C26 C25 C55 118.4(3) . . ? C24 C25 C55 118.1(3) . . ? N6 C26 C25 125.7(3) . . ? N6 C26 C27 108.1(3) . . ? C25 C26 C27 126.0(3) . . ? C28 C27 C26 107.6(3) . . ? C28 C27 H27 127(3) . . ? C26 C27 H27 125(3) . . ? C27 C28 C29 107.2(3) . . ? C27 C28 H28 127(3) . . ? C29 C28 H28 125(3) . . ? N6 C29 C30 124.8(3) . . ? N6 C29 C28 108.6(3) . . ? C30 C29 C28 126.4(3) . . ? C29 C30 C1 124.5(3) . . ? C29 C30 C61 117.6(3) . . ? C1 C30 C61 117.9(3) . . ? C32 C31 C36 117.0(3) . . ? C32 C31 C5 121.6(3) . . ? C36 C31 C5 121.4(3) . . ? F1 C32 C31 120.2(3) . . ? F1 C32 C33 118.0(4) . . ? C31 C32 C33 121.8(4) . . ? F2 C33 C32 120.3(4) . . ? F2 C33 C34 120.5(4) . . ? C32 C33 C34 119.2(4) . . ? F3 C34 C35 120.1(4) . . ? F3 C34 C33 119.4(4) . . ? C35 C34 C33 120.5(4) . . ? F4 C35 C34 119.6(4) . . ? F4 C35 C36 121.3(5) . . ? C34 C35 C36 119.0(4) . . ? F5 C36 C35 117.9(4) . . ? F5 C36 C31 119.6(4) . . ? C35 C36 C31 122.5(4) . . ? C42 C37 C38 115.5(3) . . ? C42 C37 C10 123.4(3) . . ? C38 C37 C10 121.1(3) . . ? F6 C38 C39 117.3(4) . . ? F6 C38 C37 120.3(3) . . ? C39 C38 C37 122.4(4) . . ? F7 C39 C38 120.7(4) . . ? F7 C39 C40 119.6(4) . . ? C38 C39 C40 119.6(4) . . ? F8 C40 C41 120.3(4) . . ? F8 C40 C39 119.9(4) . . ? C41 C40 C39 119.9(4) . . ? F9 C41 C40 120.0(4) . . ? F9 C41 C42 120.1(4) . . ? C40 C41 C42 119.8(4) . . ? F10 C42 C41 117.2(3) . . ? F10 C42 C37 120.1(3) . . ? C41 C42 C37 122.7(4) . . ? C48 C43 C44 115.8(4) . . ? C48 C43 C15 121.5(3) . . ? C44 C43 C15 122.7(3) . . ? F11 C44 C45 117.8(4) . . ? F11 C44 C43 120.0(3) . . ? C45 C44 C43 122.3(4) . . ? F12 C45 C46 119.7(4) . . ? F12 C45 C44 120.2(4) . . ? C46 C45 C44 120.1(4) . . ? F13 C46 C45 120.4(4) . . ? F13 C46 C47 119.9(4) . . ? C45 C46 C47 119.7(4) . . ? F14 C47 C46 120.3(4) . . ? F14 C47 C48 119.6(4) . . ? C46 C47 C48 120.0(4) . . ? F15 C48 C47 118.6(4) . . ? F15 C48 C43 119.3(4) . . ? C47 C48 C43 122.1(4) . . ? C50 C49 C54 116.4(4) . . ? C50 C49 C20 121.9(3) . . ? C54 C49 C20 121.7(3) . . ? F16 C50 C51 117.3(4) . . ? F16 C50 C49 119.6(4) . . ? C51 C50 C49 123.0(4) . . ? F17 C51 C52 120.0(4) . . ? F17 C51 C50 121.0(5) . . ? C52 C51 C50 119.0(4) . . ? F18 C52 C51 119.8(5) . . ? F18 C52 C53 119.8(5) . . ? C51 C52 C53 120.4(4) . . ? F19 C53 C52 120.4(4) . . ? F19 C53 C54 120.0(5) . . ? C52 C53 C54 119.6(4) . . ? F20 C54 C53 117.8(4) . . ? F20 C54 C49 120.7(4) . . ? C53 C54 C49 121.5(4) . . ? C60 C55 C56 116.2(3) . . ? C60 C55 C25 122.3(3) . . ? C56 C55 C25 121.5(3) . . ? F21 C56 C55 119.9(3) . . ? F21 C56 C57 117.2(3) . . ? C55 C56 C57 122.9(4) . . ? F22 C57 C58 120.5(3) . . ? F22 C57 C56 120.7(4) . . ? C58 C57 C56 118.8(4) . . ? F23 C58 C59 120.4(4) . . ? F23 C58 C57 119.5(4) . . ? C59 C58 C57 120.0(3) . . ? F24 C59 C58 119.4(4) . . ? F24 C59 C60 121.5(4) . . ? C58 C59 C60 119.1(4) . . ? F25 C60 C55 119.9(3) . . ? F25 C60 C59 117.2(3) . . ? C55 C60 C59 122.9(4) . . ? C66 C61 C62 115.7(4) . . ? C66 C61 C30 120.8(4) . . ? C62 C61 C30 123.5(4) . . ? F26 C62 C63 117.9(4) . . ? F26 C62 C61 119.7(3) . . ? C63 C62 C61 122.4(4) . . ? F27 C63 C64 120.1(4) . . ? F27 C63 C62 119.8(4) . . ? C64 C63 C62 120.1(4) . . ? F28 C64 C63 119.9(4) . . ? F28 C64 C65 120.2(4) . . ? C63 C64 C65 119.9(4) . . ? F29 C65 C64 119.9(4) . . ? F29 C65 C66 120.9(4) . . ? C64 C65 C66 119.2(4) . . ? F30 C66 C61 119.8(4) . . ? F30 C66 C65 117.5(4) . . ? C61 C66 C65 122.7(4) . . ? C68 C67 H67A 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C68 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 C67 108.9(10) . . ? C69 C68 H68A 109.9 . . ? C67 C68 H68A 109.9 . . ? C69 C68 H68B 109.9 . . ? C67 C68 H68B 109.9 . . ? H68A C68 H68B 108.3 . . ? C68 C69 C70 112.3(7) . . ? C68 C69 H69A 109.2 . . ? C70 C69 H69A 109.2 . . ? C68 C69 H69B 109.2 . . ? C70 C69 H69B 109.2 . . ? H69A C69 H69B 107.9 . . ? C71 C70 C69 113.6(7) . . ? C71 C70 H70A 108.8 . . ? C69 C70 H70A 108.8 . . ? C71 C70 H70B 108.8 . . ? C69 C70 H70B 108.8 . . ? H70A C70 H70B 107.7 . . ? C72 C71 C70 116.0(9) . . ? C72 C71 H71A 108.3 . . ? C70 C71 H71A 108.3 . . ? C72 C71 H71B 108.3 . . ? C70 C71 H71B 108.3 . . ? H71A C71 H71B 107.4 . . ? C71 C72 C73 110.8(12) . . ? C71 C72 H72A 109.5 . . ? C73 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? C73 C72 H72B 109.5 . . ? H72A C72 H72B 108.1 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C68A C67A H67D 109.5 . . ? C68A C67A H67E 109.5 . . ? H67D C67A H67E 109.5 . . ? C68A C67A H67F 109.5 . . ? H67D C67A H67F 109.5 . . ? H67E C67A H67F 109.5 . . ? C67A C68A H68C 110.7 . . ? C67A C68A H68D 110.7 . . ? H68C C68A H68D 108.8 . . ? H73D C73A H73E 109.5 . . ? H73D C73A H73F 109.5 . . ? H73E C73A H73F 109.5 . . ? 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 N6 Pd1 N1 C1 -21.9(3) . . . . ? N5 Pd1 N1 C1 48.4(7) . . . . ? N2 Pd1 N1 C1 171.5(3) . . . . ? N6 Pd1 N1 C4 176.8(3) . . . . ? N5 Pd1 N1 C4 -112.9(6) . . . . ? N2 Pd1 N1 C4 10.2(3) . . . . ? N6 Pd1 N2 C9 73.7(6) . . . . ? N1 Pd1 N2 C9 168.1(3) . . . . ? N5 Pd1 N2 C9 -21.3(3) . . . . ? N6 Pd1 N2 C6 -89.0(5) . . . . ? N1 Pd1 N2 C6 5.4(3) . . . . ? N5 Pd1 N2 C6 176.0(3) . . . . ? N6 Pd1 N5 C24 -37.3(3) . . . . ? N1 Pd1 N5 C24 -108.0(6) . . . . ? N2 Pd1 N5 C24 129.3(3) . . . . ? N6 Pd1 N5 C21 147.7(3) . . . . ? N1 Pd1 N5 C21 77.0(6) . . . . ? N2 Pd1 N5 C21 -45.7(3) . . . . ? N1 Pd1 N6 C29 10.3(3) . . . . ? N5 Pd1 N6 C29 -159.1(3) . . . . ? N2 Pd1 N6 C29 104.9(5) . . . . ? N1 Pd1 N6 C26 -158.7(3) . . . . ? N5 Pd1 N6 C26 31.9(3) . . . . ? N2 Pd1 N6 C26 -64.1(6) . . . . ? C4 N1 C1 C30 -174.5(4) . . . . ? Pd1 N1 C1 C30 21.2(5) . . . . ? C4 N1 C1 C2 0.3(4) . . . . ? Pd1 N1 C1 C2 -164.1(3) . . . . ? N1 C1 C2 C3 -1.6(5) . . . . ? C30 C1 C2 C3 173.0(4) . . . . ? C1 C2 C3 C4 2.3(5) . . . . ? C1 N1 C4 C5 177.1(4) . . . . ? Pd1 N1 C4 C5 -18.8(5) . . . . ? C1 N1 C4 C3 1.2(4) . . . . ? Pd1 N1 C4 C3 165.2(3) . . . . ? C2 C3 C4 N1 -2.2(5) . . . . ? C2 C3 C4 C5 -178.0(4) . . . . ? N1 C4 C5 C6 9.5(6) . . . . ? C3 C4 C5 C6 -175.3(4) . . . . ? N1 C4 C5 C31 -170.1(3) . . . . ? C3 C4 C5 C31 5.2(6) . . . . ? C4 C5 C6 N2 8.4(6) . . . . ? C31 C5 C6 N2 -172.1(3) . . . . ? C4 C5 C6 C7 -171.3(4) . . . . ? C31 C5 C6 C7 8.3(6) . . . . ? C9 N2 C6 C5 179.5(3) . . . . ? Pd1 N2 C6 C5 -14.6(5) . . . . ? C9 N2 C6 C7 -0.8(4) . . . . ? Pd1 N2 C6 C7 165.1(2) . . . . ? C5 C6 C7 C8 -179.9(4) . . . . ? N2 C6 C7 C8 0.4(4) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C6 C7 C8 C10 -177.9(3) . . . . ? C6 N2 C9 C8 0.8(4) . . . . ? Pd1 N2 C9 C8 -164.5(2) . . . . ? C7 C8 C9 N2 -0.5(4) . . . . ? C10 C8 C9 N2 177.3(3) . . . . ? C7 C8 C10 C11 -136.1(4) . . . . ? C9 C8 C10 C11 46.4(6) . . . . ? C7 C8 C10 C37 40.4(5) . . . . ? C9 C8 C10 C37 -137.1(4) . . . . ? C8 C10 C11 N3 5.4(6) . . . . ? C37 C10 C11 N3 -171.1(3) . . . . ? C8 C10 C11 C12 -175.4(4) . . . . ? C37 C10 C11 C12 8.1(6) . . . . ? C14 N3 C11 C10 175.0(4) . . . . ? C14 N3 C11 C12 -4.4(4) . . . . ? C10 C11 C12 C13 -176.1(4) . . . . ? N3 C11 C12 C13 3.1(5) . . . . ? C11 C12 C13 C14 -0.8(5) . . . . ? C11 N3 C14 C15 -178.1(4) . . . . ? C11 N3 C14 C13 3.9(4) . . . . ? C12 C13 C14 C15 -179.6(4) . . . . ? C12 C13 C14 N3 -1.8(5) . . . . ? N3 C14 C15 C16 -9.1(6) . . . . ? C13 C14 C15 C16 168.4(4) . . . . ? N3 C14 C15 C43 168.4(4) . . . . ? C13 C14 C15 C43 -14.2(6) . . . . ? C19 N4 C16 C17 -6.5(4) . . . . ? C19 N4 C16 C15 162.8(3) . . . . ? C14 C15 C16 N4 -29.2(5) . . . . ? C43 C15 C16 N4 153.3(3) . . . . ? C14 C15 C16 C17 136.7(4) . . . . ? C43 C15 C16 C17 -40.7(6) . . . . ? N4 C16 C17 C18 5.4(4) . . . . ? C15 C16 C17 C18 -161.9(4) . . . . ? C16 C17 C18 C19 -2.4(4) . . . . ? C16 N4 C19 C18 5.1(4) . . . . ? C16 N4 C19 C20 -170.8(3) . . . . ? C17 C18 C19 N4 -1.5(4) . . . . ? C17 C18 C19 C20 173.4(4) . . . . ? N4 C19 C20 C21 -32.6(5) . . . . ? C18 C19 C20 C21 152.9(4) . . . . ? N4 C19 C20 C49 145.5(3) . . . . ? C18 C19 C20 C49 -29.0(6) . . . . ? C24 N5 C21 C20 153.5(3) . . . . ? Pd1 N5 C21 C20 -30.8(5) . . . . ? C24 N5 C21 C22 -9.6(4) . . . . ? Pd1 N5 C21 C22 166.1(2) . . . . ? C19 C20 C21 N5 164.1(3) . . . . ? C49 C20 C21 N5 -14.0(5) . . . . ? C19 C20 C21 C22 -35.6(5) . . . . ? C49 C20 C21 C22 146.3(4) . . . . ? N5 C21 C22 C23 6.8(4) . . . . ? C20 C21 C22 C23 -156.3(4) . . . . ? C21 C22 C23 C24 -1.4(4) . . . . ? C21 N5 C24 C25 -159.5(3) . . . . ? Pd1 N5 C24 C25 24.6(5) . . . . ? C21 N5 C24 C23 8.9(4) . . . . ? Pd1 N5 C24 C23 -167.0(2) . . . . ? C22 C23 C24 N5 -4.6(4) . . . . ? C22 C23 C24 C25 163.3(4) . . . . ? N5 C24 C25 C26 7.4(6) . . . . ? C23 C24 C25 C26 -159.0(4) . . . . ? N5 C24 C25 C55 175.4(3) . . . . ? C23 C24 C25 C55 9.0(5) . . . . ? C29 N6 C26 C25 174.3(4) . . . . ? Pd1 N6 C26 C25 -14.9(5) . . . . ? C29 N6 C26 C27 -0.9(4) . . . . ? Pd1 N6 C26 C27 169.9(3) . . . . ? C24 C25 C26 N6 -12.6(6) . . . . ? C55 C25 C26 N6 179.5(3) . . . . ? C24 C25 C26 C27 161.8(4) . . . . ? C55 C25 C26 C27 -6.2(6) . . . . ? N6 C26 C27 C28 3.1(4) . . . . ? C25 C26 C27 C28 -172.1(4) . . . . ? C26 C27 C28 C29 -3.9(5) . . . . ? C26 N6 C29 C30 174.1(4) . . . . ? Pd1 N6 C29 C30 3.7(6) . . . . ? C26 N6 C29 C28 -1.5(4) . . . . ? Pd1 N6 C29 C28 -171.9(3) . . . . ? C27 C28 C29 N6 3.4(5) . . . . ? C27 C28 C29 C30 -172.1(4) . . . . ? N6 C29 C30 C1 -12.1(6) . . . . ? C28 C29 C30 C1 162.6(4) . . . . ? N6 C29 C30 C61 169.3(4) . . . . ? C28 C29 C30 C61 -15.9(6) . . . . ? N1 C1 C30 C29 -1.1(6) . . . . ? C2 C1 C30 C29 -175.0(4) . . . . ? N1 C1 C30 C61 177.4(4) . . . . ? C2 C1 C30 C61 3.6(6) . . . . ? C4 C5 C31 C32 100.1(4) . . . . ? C6 C5 C31 C32 -79.5(5) . . . . ? C4 C5 C31 C36 -79.8(5) . . . . ? C6 C5 C31 C36 100.6(4) . . . . ? C36 C31 C32 F1 -178.9(4) . . . . ? C5 C31 C32 F1 1.2(6) . . . . ? C36 C31 C32 C33 1.7(6) . . . . ? C5 C31 C32 C33 -178.1(4) . . . . ? F1 C32 C33 F2 1.2(6) . . . . ? C31 C32 C33 F2 -179.5(4) . . . . ? F1 C32 C33 C34 -178.9(4) . . . . ? C31 C32 C33 C34 0.4(7) . . . . ? F2 C33 C34 F3 -1.3(7) . . . . ? C32 C33 C34 F3 178.7(4) . . . . ? F2 C33 C34 C35 177.9(4) . . . . ? C32 C33 C34 C35 -2.1(7) . . . . ? F3 C34 C35 F4 0.9(7) . . . . ? C33 C34 C35 F4 -178.3(4) . . . . ? F3 C34 C35 C36 -179.4(4) . . . . ? C33 C34 C35 C36 1.5(7) . . . . ? F4 C35 C36 F5 -1.6(7) . . . . ? C34 C35 C36 F5 178.7(4) . . . . ? F4 C35 C36 C31 -179.4(4) . . . . ? C34 C35 C36 C31 0.8(7) . . . . ? C32 C31 C36 F5 179.8(4) . . . . ? C5 C31 C36 F5 -0.3(6) . . . . ? C32 C31 C36 C35 -2.4(6) . . . . ? C5 C31 C36 C35 177.5(4) . . . . ? C11 C10 C37 C42 51.1(5) . . . . ? C8 C10 C37 C42 -125.5(4) . . . . ? C11 C10 C37 C38 -127.7(4) . . . . ? C8 C10 C37 C38 55.7(5) . . . . ? C42 C37 C38 F6 -180.0(3) . . . . ? C10 C37 C38 F6 -1.1(5) . . . . ? C42 C37 C38 C39 -1.7(6) . . . . ? C10 C37 C38 C39 177.2(3) . . . . ? F6 C38 C39 F7 -1.9(6) . . . . ? C37 C38 C39 F7 179.8(3) . . . . ? F6 C38 C39 C40 178.8(3) . . . . ? C37 C38 C39 C40 0.5(6) . . . . ? F7 C39 C40 F8 0.1(6) . . . . ? C38 C39 C40 F8 179.4(4) . . . . ? F7 C39 C40 C41 -178.5(4) . . . . ? C38 C39 C40 C41 0.8(6) . . . . ? F8 C40 C41 F9 -0.7(6) . . . . ? C39 C40 C41 F9 177.8(4) . . . . ? F8 C40 C41 C42 -179.3(4) . . . . ? C39 C40 C41 C42 -0.8(6) . . . . ? F9 C41 C42 F10 -0.1(6) . . . . ? C40 C41 C42 F10 178.5(4) . . . . ? F9 C41 C42 C37 -179.2(4) . . . . ? C40 C41 C42 C37 -0.6(7) . . . . ? C38 C37 C42 F10 -177.3(3) . . . . ? C10 C37 C42 F10 3.8(6) . . . . ? C38 C37 C42 C41 1.8(6) . . . . ? C10 C37 C42 C41 -177.1(4) . . . . ? C14 C15 C43 C48 124.6(5) . . . . ? C16 C15 C43 C48 -58.0(6) . . . . ? C14 C15 C43 C44 -52.9(6) . . . . ? C16 C15 C43 C44 124.6(4) . . . . ? C48 C43 C44 F11 178.4(4) . . . . ? C15 C43 C44 F11 -4.0(6) . . . . ? C48 C43 C44 C45 0.2(6) . . . . ? C15 C43 C44 C45 177.7(4) . . . . ? F11 C44 C45 F12 0.9(7) . . . . ? C43 C44 C45 F12 179.2(4) . . . . ? F11 C44 C45 C46 179.9(4) . . . . ? C43 C44 C45 C46 -1.8(7) . . . . ? F12 C45 C46 F13 0.5(8) . . . . ? C44 C45 C46 F13 -178.5(5) . . . . ? F12 C45 C46 C47 -178.7(5) . . . . ? C44 C45 C46 C47 2.3(8) . . . . ? F13 C46 C47 F14 1.2(8) . . . . ? C45 C46 C47 F14 -179.6(5) . . . . ? F13 C46 C47 C48 179.7(5) . . . . ? C45 C46 C47 C48 -1.1(8) . . . . ? F14 C47 C48 F15 -1.1(8) . . . . ? C46 C47 C48 F15 -179.5(5) . . . . ? F14 C47 C48 C43 177.9(5) . . . . ? C46 C47 C48 C43 -0.6(8) . . . . ? C44 C43 C48 F15 180.0(4) . . . . ? C15 C43 C48 F15 2.4(7) . . . . ? C44 C43 C48 C47 1.0(7) . . . . ? C15 C43 C48 C47 -176.5(5) . . . . ? C21 C20 C49 C50 128.5(4) . . . . ? C19 C20 C49 C50 -49.5(5) . . . . ? C21 C20 C49 C54 -49.6(5) . . . . ? C19 C20 C49 C54 132.3(4) . . . . ? C54 C49 C50 F16 177.6(3) . . . . ? C20 C49 C50 F16 -0.7(6) . . . . ? C54 C49 C50 C51 1.9(6) . . . . ? C20 C49 C50 C51 -176.3(4) . . . . ? F16 C50 C51 F17 3.3(6) . . . . ? C49 C50 C51 F17 179.1(4) . . . . ? F16 C50 C51 C52 -175.6(4) . . . . ? C49 C50 C51 C52 0.2(7) . . . . ? F17 C51 C52 F18 -0.6(7) . . . . ? C50 C51 C52 F18 178.3(4) . . . . ? F17 C51 C52 C53 179.4(4) . . . . ? C50 C51 C52 C53 -1.7(7) . . . . ? F18 C52 C53 F19 0.8(7) . . . . ? C51 C52 C53 F19 -179.2(4) . . . . ? F18 C52 C53 C54 -179.0(4) . . . . ? C51 C52 C53 C54 1.0(7) . . . . ? F19 C53 C54 F20 0.5(6) . . . . ? C52 C53 C54 F20 -179.6(4) . . . . ? F19 C53 C54 C49 -178.5(4) . . . . ? C52 C53 C54 C49 1.3(6) . . . . ? C50 C49 C54 F20 178.3(3) . . . . ? C20 C49 C54 F20 -3.4(6) . . . . ? C50 C49 C54 C53 -2.7(6) . . . . ? C20 C49 C54 C53 175.6(4) . . . . ? C26 C25 C55 C60 75.7(5) . . . . ? C24 C25 C55 C60 -92.8(4) . . . . ? C26 C25 C55 C56 -105.7(4) . . . . ? C24 C25 C55 C56 85.8(4) . . . . ? C60 C55 C56 F21 176.5(3) . . . . ? C25 C55 C56 F21 -2.1(5) . . . . ? C60 C55 C56 C57 -2.7(6) . . . . ? C25 C55 C56 C57 178.7(3) . . . . ? F21 C56 C57 F22 2.0(5) . . . . ? C55 C56 C57 F22 -178.7(3) . . . . ? F21 C56 C57 C58 -177.0(3) . . . . ? C55 C56 C57 C58 2.3(6) . . . . ? F22 C57 C58 F23 0.1(6) . . . . ? C56 C57 C58 F23 179.1(4) . . . . ? F22 C57 C58 C59 -179.2(4) . . . . ? C56 C57 C58 C59 -0.2(6) . . . . ? F23 C58 C59 F24 -0.7(6) . . . . ? C57 C58 C59 F24 178.6(4) . . . . ? F23 C58 C59 C60 179.4(4) . . . . ? C57 C58 C59 C60 -1.3(6) . . . . ? C56 C55 C60 F25 -178.6(3) . . . . ? C25 C55 C60 F25 0.1(6) . . . . ? C56 C55 C60 C59 1.1(6) . . . . ? C25 C55 C60 C59 179.8(4) . . . . ? F24 C59 C60 F25 0.6(6) . . . . ? C58 C59 C60 F25 -179.5(4) . . . . ? F24 C59 C60 C55 -179.1(4) . . . . ? C58 C59 C60 C55 0.8(6) . . . . ? C29 C30 C61 C66 -68.6(5) . . . . ? C1 C30 C61 C66 112.7(5) . . . . ? C29 C30 C61 C62 109.7(5) . . . . ? C1 C30 C61 C62 -68.9(5) . . . . ? C66 C61 C62 F26 -180.0(4) . . . . ? C30 C61 C62 F26 1.6(6) . . . . ? C66 C61 C62 C63 -1.5(6) . . . . ? C30 C61 C62 C63 -179.9(4) . . . . ? F26 C62 C63 F27 -1.6(6) . . . . ? C61 C62 C63 F27 179.8(4) . . . . ? F26 C62 C63 C64 179.4(4) . . . . ? C61 C62 C63 C64 0.8(7) . . . . ? F27 C63 C64 F28 0.3(7) . . . . ? C62 C63 C64 F28 179.3(4) . . . . ? F27 C63 C64 C65 -177.5(5) . . . . ? C62 C63 C64 C65 1.5(7) . . . . ? F28 C64 C65 F29 1.2(8) . . . . ? C63 C64 C65 F29 178.9(5) . . . . ? F28 C64 C65 C66 179.1(5) . . . . ? C63 C64 C65 C66 -3.1(8) . . . . ? C62 C61 C66 F30 -179.6(4) . . . . ? C30 C61 C66 F30 -1.1(7) . . . . ? C62 C61 C66 C65 -0.2(7) . . . . ? C30 C61 C66 C65 178.2(5) . . . . ? F29 C65 C66 F30 -0.2(8) . . . . ? C64 C65 C66 F30 -178.1(5) . . . . ? F29 C65 C66 C61 -179.6(5) . . . . ? C64 C65 C66 C61 2.5(8) . . . . ? C67 C68 C69 C70 -177.9(9) . . . . ? C68 C69 C70 C71 -177.2(7) . . . . ? C69 C70 C71 C72 178.3(10) . . . . ? C70 C71 C72 C73 173.3(10) . . . . ? #=========================================================================== #== # End of CIF #=========================================================================== #==