# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dai-zheng Liao' _publ_contact_author_email maynk@nankai.edu.cn loop_ _publ_author_name 'Ya-Li Wang' 'Yuan-Yuan Gao' 'Yue Ma' 'Qing Wang' 'Licun Li' 'Dai-zheng Liao' # Attachment '- complex-3.cif' data_shelxlc _database_code_depnum_ccdc_archive 'CCDC 779494' #TrackingRef '- complex-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H45 F18 N4 O12 Tb' _chemical_formula_weight 1406.84 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 51.285(10) _cell_length_b 11.694(2) _cell_length_c 31.093(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.22(3) _cell_angle_gamma 90.00 _cell_volume 17263(6) _cell_formula_units_Z 12 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 23891 _cell_measurement_theta_min 1.7936 _cell_measurement_theta_max 27.9143 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8423 _exptl_absorpt_coefficient_mu 1.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 0.806 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 56639 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 60 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.01 _reflns_number_total 15209 _reflns_number_gt 13366 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Fluorine atoms in the CF3 groups were treated by disorder and these atoms were refined anisotropically with application of restraints on interatomic distances and thermal parameters (DFIX, ISOR and SIMU instructions in SHELXL). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+31.4165P] 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 SHELXL _refine_ls_extinction_coef 0.000282(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15209 _refine_ls_number_parameters 1235 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.005 _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 Tb1 Tb 1.0000 0.599520(18) 0.7500 0.02165(7) Uani 1 2 d S . . Tb2 Tb 0.833586(3) 0.857686(12) 0.924004(5) 0.01930(6) Uani 1 1 d . A . C1 C 0.85319(8) 0.4679(3) 0.93578(16) 0.0407(10) Uani 1 1 d . . . C2 C 0.83388(7) 0.5727(3) 0.92153(13) 0.0296(8) Uani 1 1 d . . . C3 C 0.80528(8) 0.5554(3) 0.89699(16) 0.0443(11) Uani 1 1 d . . . H3 H 0.7986 0.4813 0.8890 0.053 Uiso 1 1 calc R . . C4 C 0.78633(7) 0.6464(3) 0.88411(15) 0.0387(10) Uani 1 1 d . A . C5 C 0.75521(11) 0.6169(5) 0.8574(3) 0.089(2) Uani 1 1 d D . . C6 C 0.88753(7) 1.1361(3) 0.88712(13) 0.0310(8) Uani 1 1 d . . . C7 C 0.88285(6) 1.0361(3) 0.91514(12) 0.0225(7) Uani 1 1 d . A . C8 C 0.90489(7) 1.0036(3) 0.95521(12) 0.0256(7) Uani 1 1 d . . . H8 H 0.9221 1.0414 0.9638 0.031 Uiso 1 1 calc R . . C9 C 0.90183(6) 0.9153(3) 0.98298(11) 0.0215(7) Uani 1 1 d . A . C10 C 0.92657(7) 0.8872(3) 1.02808(13) 0.0286(8) Uani 1 1 d . . . C11 C 0.83996(8) 1.1852(3) 1.01407(14) 0.0371(9) Uani 1 1 d . . . C12 C 0.82767(7) 1.1121(3) 0.97018(13) 0.0284(8) Uani 1 1 d . A . C13 C 0.80703(8) 1.1588(3) 0.93119(14) 0.0336(9) Uani 1 1 d . . . H13 H 0.8011 1.2334 0.9324 0.040 Uiso 1 1 calc R . . C14 C 0.79511(7) 1.0968(3) 0.89048(13) 0.0301(8) Uani 1 1 d . A . C15 C 0.77517(9) 1.1622(3) 0.84790(17) 0.0498(11) Uani 1 1 d . . . C16 C 0.91663(9) 0.3938(4) 0.70389(15) 0.0450(10) Uani 1 1 d . . . C17 C 0.94623(7) 0.4263(3) 0.73781(13) 0.0304(8) Uani 1 1 d . . . C18 C 0.96023(8) 0.3457(3) 0.77100(14) 0.0380(9) Uani 1 1 d . . . H18 H 0.9507 0.2803 0.7738 0.046 Uiso 1 1 calc R . . C19 C 0.98813(8) 0.3599(3) 0.80011(13) 0.0332(8) Uani 1 1 d . . . C20 C 1.00237(9) 0.2663(3) 0.83639(15) 0.0453(11) Uani 1 1 d . . . C21 C 0.94850(9) 0.9391(3) 0.73521(16) 0.0394(10) Uani 1 1 d . . . C22 C 0.97517(7) 0.8670(3) 0.74365(12) 0.0287(8) Uani 1 1 d . B . C23 C 1.0000 0.9235(4) 0.7500 0.0371(13) Uani 1 2 d S . . H23 H 1.0000 1.0030 0.7500 0.045 Uiso 1 2 calc SR B . C24 C 0.65011(8) 1.1985(4) 0.86260(15) 0.0485(11) Uani 1 1 d . . . H24A H 0.6470 1.1616 0.8878 0.073 Uiso 1 1 calc R . . H24B H 0.6323 1.2166 0.8385 0.073 Uiso 1 1 calc R . . H24C H 0.6607 1.2675 0.8736 0.073 Uiso 1 1 calc R . . C25 C 0.69132(7) 1.0866(3) 0.87465(13) 0.0289(8) Uani 1 1 d . . . C26 C 0.70393(7) 1.0036(3) 0.85517(12) 0.0299(8) Uani 1 1 d . . . H26 H 0.6952 0.9832 0.8241 0.036 Uiso 1 1 calc R . . C27 C 0.72864(7) 0.9543(3) 0.88201(12) 0.0289(8) Uani 1 1 d . . . H27 H 0.7367 0.8998 0.8691 0.035 Uiso 1 1 calc R . . C28 C 0.74244(7) 0.9846(3) 0.92961(12) 0.0253(7) Uani 1 1 d . . . C29 C 0.73028(7) 1.0712(3) 0.94785(12) 0.0268(8) Uani 1 1 d . . . C30 C 0.70441(7) 1.1219(3) 0.91917(12) 0.0280(8) Uani 1 1 d . . . H30 H 0.6964 1.1794 0.9309 0.034 Uiso 1 1 calc R . . C31 C 0.76700(7) 0.9285(3) 0.95889(12) 0.0272(8) Uani 1 1 d . . . H31 H 0.7745 0.8700 0.9469 0.033 Uiso 1 1 calc R . . C32 C 0.78022(7) 0.9585(3) 1.00505(12) 0.0271(8) Uani 1 1 d . . . C33 C 0.76851(7) 1.0488(3) 1.02283(13) 0.0336(8) Uani 1 1 d . . . H33 H 0.7774 1.0719 1.0536 0.040 Uiso 1 1 calc R . . C34 C 0.74427(7) 1.1014(3) 0.99497(13) 0.0334(8) Uani 1 1 d . . . H34 H 0.7367 1.1589 1.0074 0.040 Uiso 1 1 calc R . . C35 C 0.80484(7) 0.8963(3) 1.03569(12) 0.0281(8) Uani 1 1 d . . . C36 C 0.86678(8) 0.7230(3) 1.05824(14) 0.0393(9) Uani 1 1 d . . . H36A H 0.8632 0.6754 1.0315 0.059 Uiso 1 1 calc R . . H36B H 0.8791 0.6836 1.0855 0.059 Uiso 1 1 calc R . . H36C H 0.8756 0.7928 1.0545 0.059 Uiso 1 1 calc R . . C37 C 0.83908(7) 0.7503(3) 1.06352(13) 0.0311(8) Uani 1 1 d . . . C38 C 0.82264(9) 0.6398(3) 1.06098(15) 0.0474(11) Uani 1 1 d . . . H38A H 0.8055 0.6569 1.0653 0.071 Uiso 1 1 calc R . . H38B H 0.8338 0.5884 1.0849 0.071 Uiso 1 1 calc R . . H38C H 0.8183 0.6048 1.0311 0.071 Uiso 1 1 calc R . . C39 C 0.86618(8) 0.9113(4) 1.11849(16) 0.0510(11) Uani 1 1 d . . . H39A H 0.8665 0.9493 1.0913 0.077 Uiso 1 1 calc R . . H39B H 0.8835 0.8700 1.1332 0.077 Uiso 1 1 calc R . . H39C H 0.8642 0.9669 1.1398 0.077 Uiso 1 1 calc R . . C40 C 0.84148(7) 0.8283(3) 1.10463(13) 0.0360(9) Uani 1 1 d . . . C41 C 0.84024(9) 0.7666(4) 1.14721(14) 0.0526(11) Uani 1 1 d . . . H41A H 0.8425 0.8212 1.1714 0.079 Uiso 1 1 calc R . . H41B H 0.8551 0.7110 1.1579 0.079 Uiso 1 1 calc R . . H41C H 0.8224 0.7290 1.1390 0.079 Uiso 1 1 calc R . . C42 C 1.01785(7) 0.7849(3) 1.03263(13) 0.0391(9) Uani 1 1 d . . . H42A H 1.0031 0.8013 1.0436 0.059 Uiso 1 1 calc R . . H42B H 1.0358 0.8000 1.0569 0.059 Uiso 1 1 calc R . . H42C H 1.0169 0.7059 1.0237 0.059 Uiso 1 1 calc R . . C43 C 0.98886(7) 0.8518(3) 0.95731(12) 0.0276(8) Uani 1 1 d . . . C44 C 0.98533(7) 0.9334(3) 0.92228(13) 0.0298(8) Uani 1 1 d . . . H44 H 1.0001 0.9820 0.9243 0.036 Uiso 1 1 calc R . . C45 C 0.96033(7) 0.9417(3) 0.88539(12) 0.0276(8) Uani 1 1 d . . . H45 H 0.9583 0.9949 0.8621 0.033 Uiso 1 1 calc R . . C46 C 0.93732(6) 0.8699(3) 0.88209(11) 0.0209(7) Uani 1 1 d . . . C47 C 0.94127(6) 0.7868(3) 0.91728(11) 0.0211(7) Uani 1 1 d . . . C48 C 0.96767(6) 0.7778(3) 0.95470(12) 0.0262(7) Uani 1 1 d . . . H48 H 0.9706 0.7220 0.9773 0.031 Uiso 1 1 calc R . . C49 C 0.91825(6) 0.7167(3) 0.91452(12) 0.0241(7) Uani 1 1 d . . . H49 H 0.9208 0.6593 0.9365 0.029 Uiso 1 1 calc R . . C50 C 0.89236(6) 0.7317(3) 0.88028(12) 0.0226(7) Uani 1 1 d . . . H50 H 0.8774 0.6859 0.8794 0.027 Uiso 1 1 calc R . . C51 C 0.88829(6) 0.8172(3) 0.84599(11) 0.0221(7) Uani 1 1 d . . . C52 C 0.91065(6) 0.8826(3) 0.84650(11) 0.0222(7) Uani 1 1 d . . . H52 H 0.9081 0.9358 0.8230 0.027 Uiso 1 1 calc R . . C53 C 0.86017(6) 0.8356(3) 0.81080(11) 0.0213(7) Uani 1 1 d . . . C54 C 0.81321(8) 0.8695(4) 0.69132(13) 0.0423(10) Uani 1 1 d . . . H54A H 0.8220 0.9187 0.6761 0.063 Uiso 1 1 calc R . . H54B H 0.7931 0.8785 0.6773 0.063 Uiso 1 1 calc R . . H54C H 0.8180 0.7914 0.6882 0.063 Uiso 1 1 calc R . . C55 C 0.82336(7) 0.9005(3) 0.74227(12) 0.0307(8) Uani 1 1 d . . . C56 C 0.82128(8) 1.0292(3) 0.74861(15) 0.0452(10) Uani 1 1 d . . . H56A H 0.8272 1.0464 0.7811 0.068 Uiso 1 1 calc R . . H56B H 0.8021 1.0535 0.7327 0.068 Uiso 1 1 calc R . . H56C H 0.8332 1.0686 0.7360 0.068 Uiso 1 1 calc R . . C57 C 0.80495(7) 0.7037(3) 0.75470(13) 0.0390(9) Uani 1 1 d . . . H57A H 0.8209 0.6730 0.7495 0.059 Uiso 1 1 calc R . . H57B H 0.7887 0.7014 0.7262 0.059 Uiso 1 1 calc R . . H57C H 0.8015 0.6590 0.7779 0.059 Uiso 1 1 calc R . . C58 C 0.81099(6) 0.8271(3) 0.77131(12) 0.0285(8) Uani 1 1 d . . . C59 C 0.78587(7) 0.8795(4) 0.77849(14) 0.0451(10) Uani 1 1 d . . . H59A H 0.7800 0.8299 0.7977 0.068 Uiso 1 1 calc R . . H59B H 0.7707 0.8890 0.7490 0.068 Uiso 1 1 calc R . . H59C H 0.7911 0.9526 0.7933 0.068 Uiso 1 1 calc R . . C60 C 0.83651(9) 0.3736(4) 0.78515(19) 0.0757(18) Uani 1 1 d . . . H60A H 0.8473 0.3064 0.7853 0.114 Uiso 1 1 calc R . . H60B H 0.8169 0.3590 0.7675 0.114 Uiso 1 1 calc R . . H60C H 0.8390 0.3932 0.8165 0.114 Uiso 1 1 calc R . . C61 C 0.87353(7) 0.4982(3) 0.78564(13) 0.0316(8) Uani 1 1 d . . . C62 C 0.88117(7) 0.5904(3) 0.76339(13) 0.0301(8) Uani 1 1 d . . . H62 H 0.8678 0.6243 0.7373 0.036 Uiso 1 1 calc R . . C63 C 0.90819(7) 0.6293(3) 0.78019(12) 0.0256(7) Uani 1 1 d . . . H63 H 0.9131 0.6896 0.7653 0.031 Uiso 1 1 calc R . . C64 C 0.92888(7) 0.5795(3) 0.81989(12) 0.0233(7) Uani 1 1 d . . . C65 C 0.92071(7) 0.4888(3) 0.84251(12) 0.0271(8) Uani 1 1 d . . . C66 C 0.89259(7) 0.4496(3) 0.82452(13) 0.0335(9) Uani 1 1 d . . . H66 H 0.8871 0.3904 0.8393 0.040 Uiso 1 1 calc R . . C67 C 0.95719(7) 0.6164(3) 0.83717(11) 0.0226(7) Uani 1 1 d . . . H67 H 0.9625 0.6756 0.8222 0.027 Uiso 1 1 calc R . . C68 C 0.97698(7) 0.5666(3) 0.87561(12) 0.0259(7) Uani 1 1 d . . . C69 C 0.96860(7) 0.4774(3) 0.89886(13) 0.0356(9) Uani 1 1 d . . . H69 H 0.9818 0.4441 0.9253 0.043 Uiso 1 1 calc R . . C70 C 0.94128(7) 0.4408(3) 0.88241(13) 0.0357(9) Uani 1 1 d . . . H70 H 0.9361 0.3826 0.8980 0.043 Uiso 1 1 calc R . . C71 C 1.00662(7) 0.6008(3) 0.89281(11) 0.0231(7) Uani 1 1 d . . . C72 C 1.06956(7) 0.6573(3) 0.87239(14) 0.0394(9) Uani 1 1 d . . . H72A H 1.0677 0.5784 0.8632 0.059 Uiso 1 1 calc R . . H72B H 1.0886 0.6723 0.8929 0.059 Uiso 1 1 calc R . . H72C H 1.0648 0.7050 0.8454 0.059 Uiso 1 1 calc R . . C73 C 1.04970(7) 0.6831(3) 0.89737(12) 0.0261(7) Uani 1 1 d . . . C74 C 1.04819(8) 0.8116(3) 0.90403(13) 0.0350(9) Uani 1 1 d . . . H74A H 1.0406 0.8483 0.8742 0.053 Uiso 1 1 calc R . . H74B H 1.0667 0.8405 0.9212 0.053 Uiso 1 1 calc R . . H74C H 1.0363 0.8268 0.9208 0.053 Uiso 1 1 calc R . . C75 C 1.06817(8) 0.4948(3) 0.94203(15) 0.0432(10) Uani 1 1 d . . . H75A H 1.0684 0.4516 0.9684 0.065 Uiso 1 1 calc R . . H75B H 1.0871 0.5044 0.9436 0.065 Uiso 1 1 calc R . . H75C H 1.0573 0.4547 0.9140 0.065 Uiso 1 1 calc R . . C76 C 1.05507(7) 0.6114(3) 0.94205(12) 0.0274(8) Uani 1 1 d . . . C77 C 1.07064(7) 0.6740(3) 0.98730(13) 0.0350(9) Uani 1 1 d . . . H77A H 1.0605 0.7421 0.9885 0.053 Uiso 1 1 calc R . . H77B H 1.0891 0.6943 0.9890 0.053 Uiso 1 1 calc R . . H77C H 1.0722 0.6253 1.0130 0.053 Uiso 1 1 calc R . . F1 F 0.87520(5) 0.47971(18) 0.92309(10) 0.0545(7) Uani 1 1 d . . . F2 F 0.84043(5) 0.37081(17) 0.91812(11) 0.0638(8) Uani 1 1 d . . . F3 F 0.86368(5) 0.4558(2) 0.98212(10) 0.0613(7) Uani 1 1 d . . . F4 F 0.7543(3) 0.581(2) 0.8136(5) 0.086(6) Uani 0.227(11) 1 d PDU A 1 F5 F 0.7396(3) 0.6809(12) 0.8496(6) 0.051(5) Uani 0.227(11) 1 d PU A 1 F6 F 0.7507(4) 0.508(2) 0.8763(7) 0.054(5) Uani 0.227(11) 1 d PU A 1 F4' F 0.74872(15) 0.5110(6) 0.8538(4) 0.116(4) Uani 0.773(11) 1 d P A 2 F6' F 0.74087(12) 0.6614(5) 0.8842(4) 0.154(5) Uani 0.773(11) 1 d PD A 2 F5' F 0.74396(16) 0.6738(8) 0.8192(3) 0.179(5) Uani 0.773(11) 1 d PU A 2 F7 F 0.87535(5) 1.1205(2) 0.84193(8) 0.0570(7) Uani 1 1 d . . . F8 F 0.91449(5) 1.1529(2) 0.89378(10) 0.0687(9) Uani 1 1 d . . . F9 F 0.87795(8) 1.2302(2) 0.89741(12) 0.0990(13) Uani 1 1 d . . . F10 F 0.95045(4) 0.93881(18) 1.03188(8) 0.0413(5) Uani 1 1 d . . . F11 F 0.93158(4) 0.77581(17) 1.03205(8) 0.0443(6) Uani 1 1 d . . . F12 F 0.92072(4) 0.9198(2) 1.06455(8) 0.0445(6) Uani 1 1 d . . . F13 F 0.86747(5) 1.1992(2) 1.02603(10) 0.0634(8) Uani 1 1 d . . . F14 F 0.82871(5) 1.28980(17) 1.00969(9) 0.0504(6) Uani 1 1 d . . . F15 F 0.83583(6) 1.13560(18) 1.04953(8) 0.0516(6) Uani 1 1 d . . . F16 F 0.75723(5) 1.0945(2) 0.81705(9) 0.0577(7) Uani 1 1 d . . . F17 F 0.78978(7) 1.2135(3) 0.82634(13) 0.1126(15) Uani 1 1 d . . . F18 F 0.76000(7) 1.2401(3) 0.85827(12) 0.1109(14) Uani 1 1 d . . . F19 F 0.91847(6) 0.3293(3) 0.67027(11) 0.0816(10) Uani 1 1 d . . . F20 F 0.90214(6) 0.3349(3) 0.72466(11) 0.0820(10) Uani 1 1 d . . . F21 F 0.90088(4) 0.4821(2) 0.68388(9) 0.0521(6) Uani 1 1 d . . . F22 F 1.01595(6) 0.3093(2) 0.87769(9) 0.0701(8) Uani 1 1 d . . . F23 F 1.01981(9) 0.2068(3) 0.82402(13) 0.1095(14) Uani 1 1 d . . . F24 F 0.98420(7) 0.1924(2) 0.84182(11) 0.0909(11) Uani 1 1 d . . . F25 F 0.9397(4) 0.9221(15) 0.7691(5) 0.076(4) Uani 0.61(4) 1 d P B 1 F26 F 0.9509(4) 1.0491(10) 0.7300(11) 0.089(5) Uani 0.61(4) 1 d P B 1 F27 F 0.9266(3) 0.9060(15) 0.6974(6) 0.094(5) Uani 0.61(4) 1 d P B 1 F26' F 0.9553(3) 1.0426(18) 0.7538(9) 0.068(5) Uani 0.39(4) 1 d PU B 2 F25' F 0.9334(6) 0.9016(18) 0.7563(13) 0.090(8) Uani 0.39(4) 1 d P B 2 F27' F 0.9355(7) 0.948(4) 0.6937(7) 0.108(11) Uani 0.39(4) 1 d P B 2 N1 N 0.82076(5) 0.8222(2) 1.02368(10) 0.0250(6) Uani 1 1 d . A . N2 N 0.81528(6) 0.8988(3) 1.08315(11) 0.0360(7) Uani 1 1 d . . . N3 N 0.83591(5) 0.8218(2) 0.81620(9) 0.0222(6) Uani 1 1 d . A . N4 N 0.85413(6) 0.8714(2) 0.76610(10) 0.0278(6) Uani 1 1 d . . . N5 N 1.02527(6) 0.5894(2) 0.93759(10) 0.0290(7) Uani 1 1 d . . . N6 N 1.02035(5) 0.6454(2) 0.86798(10) 0.0234(6) Uani 1 1 d . B . O1 O 0.84674(4) 0.66422(18) 0.93505(8) 0.0240(5) Uani 1 1 d . . . O2 O 0.79092(4) 0.75043(19) 0.89001(8) 0.0266(5) Uani 1 1 d . . . O3 O 0.85833(4) 0.99617(18) 0.89837(8) 0.0239(5) Uani 1 1 d . . . O4 O 0.88040(4) 0.85580(17) 0.97627(8) 0.0226(5) Uani 1 1 d . . . O5 O 0.83807(5) 1.01378(18) 0.97505(8) 0.0271(5) Uani 1 1 d . . . O6 O 0.79941(4) 0.99503(19) 0.88320(8) 0.0280(5) Uani 1 1 d . . . O7 O 0.83279(4) 0.78730(19) 0.85391(8) 0.0249(5) Uani 1 1 d . . . O8 O 0.87180(5) 0.8906(2) 0.74750(9) 0.0399(6) Uani 1 1 d . . . O9 O 0.81756(4) 0.79417(19) 0.98134(8) 0.0266(5) Uani 1 1 d . . . O10 O 0.80669(6) 0.9601(3) 1.10864(10) 0.0614(9) Uani 1 1 d . . . O11 O 0.66561(5) 1.1233(2) 0.84450(9) 0.0380(6) Uani 1 1 d . . . O12 O 1.01455(5) 0.8556(2) 0.99329(9) 0.0348(6) Uani 1 1 d . . . O13 O 0.84581(5) 0.4661(2) 0.76460(10) 0.0428(7) Uani 1 1 d . . . O14 O 0.95487(5) 0.52161(19) 0.73056(8) 0.0274(5) Uani 1 1 d . . . O15 O 1.00434(5) 0.44086(18) 0.80059(8) 0.0295(5) Uani 1 1 d . . . O16 O 0.97090(5) 0.76173(18) 0.74311(8) 0.0263(5) Uani 1 1 d . . . O17 O 1.00948(5) 0.67375(18) 0.82437(8) 0.0255(5) Uani 1 1 d . . . O18 O 1.01997(6) 0.5508(2) 0.97174(9) 0.0441(7) 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 Tb1 0.02138(12) 0.01902(12) 0.02224(13) 0.000 0.00562(9) 0.000 Tb2 0.01373(8) 0.02092(9) 0.02150(10) -0.00100(6) 0.00467(6) -0.00146(6) C1 0.034(2) 0.026(2) 0.062(3) 0.0014(19) 0.018(2) -0.0033(16) C2 0.0263(18) 0.0258(19) 0.038(2) -0.0006(15) 0.0134(16) -0.0012(14) C3 0.030(2) 0.0260(19) 0.068(3) -0.0067(19) 0.008(2) -0.0079(16) C4 0.0226(18) 0.033(2) 0.052(3) -0.0050(18) 0.0048(17) -0.0075(16) C5 0.029(3) 0.041(3) 0.165(8) -0.010(4) 0.001(4) -0.009(2) C6 0.0293(19) 0.0252(19) 0.033(2) 0.0036(15) 0.0050(16) -0.0037(15) C7 0.0222(16) 0.0177(16) 0.029(2) -0.0010(14) 0.0111(14) -0.0006(13) C8 0.0211(16) 0.0215(17) 0.033(2) -0.0031(14) 0.0091(15) -0.0065(13) C9 0.0176(15) 0.0200(16) 0.0243(19) -0.0047(13) 0.0051(13) 0.0003(13) C10 0.0212(17) 0.0261(18) 0.034(2) 0.0003(15) 0.0049(15) -0.0054(14) C11 0.042(2) 0.028(2) 0.046(3) -0.0122(18) 0.0223(19) -0.0089(17) C12 0.0284(18) 0.0261(18) 0.038(2) -0.0093(16) 0.0214(16) -0.0090(15) C13 0.036(2) 0.0194(17) 0.047(3) -0.0017(16) 0.0189(18) 0.0014(15) C14 0.0218(17) 0.0268(19) 0.041(2) 0.0021(16) 0.0117(16) 0.0028(14) C15 0.043(2) 0.036(2) 0.055(3) 0.007(2) 0.002(2) 0.0089(19) C16 0.044(2) 0.045(2) 0.041(3) -0.008(2) 0.011(2) -0.017(2) C17 0.0326(19) 0.033(2) 0.027(2) -0.0080(16) 0.0118(16) -0.0074(16) C18 0.045(2) 0.027(2) 0.038(2) 0.0006(16) 0.0111(18) -0.0152(17) C19 0.047(2) 0.0223(18) 0.030(2) 0.0014(15) 0.0144(17) 0.0003(16) C20 0.059(3) 0.026(2) 0.043(3) 0.0094(18) 0.010(2) -0.0023(19) C21 0.044(2) 0.027(2) 0.054(3) 0.0059(19) 0.026(2) 0.0101(18) C22 0.035(2) 0.028(2) 0.029(2) -0.0013(15) 0.0183(16) 0.0068(15) C23 0.045(3) 0.022(3) 0.056(4) 0.000 0.032(3) 0.000 C24 0.037(2) 0.070(3) 0.038(3) -0.001(2) 0.0146(19) 0.022(2) C25 0.0232(17) 0.0331(19) 0.030(2) 0.0017(15) 0.0103(15) 0.0009(15) C26 0.0292(18) 0.039(2) 0.023(2) -0.0042(15) 0.0116(15) -0.0036(16) C27 0.0271(18) 0.0321(19) 0.031(2) -0.0069(16) 0.0150(16) -0.0010(15) C28 0.0225(16) 0.0282(18) 0.027(2) -0.0033(15) 0.0112(14) -0.0044(14) C29 0.0284(18) 0.0241(17) 0.030(2) -0.0018(15) 0.0134(16) -0.0032(14) C30 0.0279(18) 0.0275(18) 0.032(2) -0.0024(15) 0.0150(15) 0.0012(14) C31 0.0222(17) 0.0301(18) 0.031(2) -0.0055(15) 0.0125(15) -0.0047(14) C32 0.0233(17) 0.0307(19) 0.026(2) -0.0036(15) 0.0082(15) -0.0052(14) C33 0.0333(19) 0.037(2) 0.026(2) -0.0107(16) 0.0059(16) -0.0041(16) C34 0.033(2) 0.031(2) 0.035(2) -0.0091(16) 0.0118(17) 0.0030(16) C35 0.0221(17) 0.0359(19) 0.026(2) -0.0036(15) 0.0091(15) -0.0049(15) C36 0.035(2) 0.052(2) 0.032(2) 0.0119(18) 0.0142(17) 0.0134(18) C37 0.0289(18) 0.035(2) 0.030(2) 0.0053(16) 0.0117(16) 0.0006(15) C38 0.060(3) 0.042(2) 0.043(3) 0.0105(19) 0.021(2) -0.009(2) C39 0.032(2) 0.054(3) 0.053(3) -0.011(2) 0.001(2) 0.0007(19) C40 0.0271(19) 0.049(2) 0.028(2) 0.0038(17) 0.0064(16) 0.0041(17) C41 0.049(3) 0.078(3) 0.029(2) 0.007(2) 0.012(2) 0.012(2) C42 0.0254(19) 0.052(2) 0.030(2) 0.0067(18) -0.0008(16) 0.0018(17) C43 0.0176(16) 0.0314(19) 0.031(2) -0.0013(15) 0.0057(14) 0.0025(14) C44 0.0213(17) 0.0282(18) 0.038(2) 0.0034(16) 0.0089(16) -0.0038(14) C45 0.0246(17) 0.0258(17) 0.032(2) 0.0080(15) 0.0101(15) 0.0009(14) C46 0.0190(15) 0.0207(16) 0.0241(18) -0.0002(13) 0.0093(13) 0.0007(13) C47 0.0187(15) 0.0230(17) 0.0207(18) -0.0012(13) 0.0065(13) 0.0023(13) C48 0.0214(16) 0.0278(18) 0.026(2) 0.0045(15) 0.0056(14) 0.0036(14) C49 0.0218(16) 0.0226(17) 0.027(2) 0.0037(14) 0.0079(14) 0.0021(13) C50 0.0187(16) 0.0226(16) 0.0270(19) 0.0019(14) 0.0092(14) 0.0004(13) C51 0.0181(15) 0.0253(17) 0.0224(18) -0.0035(14) 0.0069(13) 0.0008(13) C52 0.0222(16) 0.0228(16) 0.0214(18) 0.0035(14) 0.0079(13) 0.0022(13) C53 0.0187(15) 0.0222(16) 0.0210(18) -0.0013(13) 0.0051(13) 0.0019(13) C54 0.038(2) 0.058(3) 0.023(2) 0.0080(18) 0.0026(17) 0.0080(19) C55 0.0232(17) 0.036(2) 0.025(2) 0.0036(15) -0.0008(14) 0.0084(15) C56 0.041(2) 0.037(2) 0.047(3) 0.0060(19) 0.0042(19) 0.0115(18) C57 0.0263(19) 0.048(2) 0.031(2) -0.0060(18) -0.0024(16) -0.0120(17) C58 0.0148(15) 0.041(2) 0.0214(19) 0.0013(15) -0.0020(13) 0.0047(14) C59 0.0210(18) 0.075(3) 0.033(2) -0.001(2) 0.0034(16) 0.0138(19) C60 0.037(2) 0.078(3) 0.084(4) 0.040(3) -0.010(2) -0.030(2) C61 0.0233(17) 0.0305(19) 0.034(2) 0.0007(16) 0.0035(15) -0.0047(15) C62 0.0287(18) 0.0306(19) 0.027(2) 0.0035(15) 0.0062(15) 0.0040(15) C63 0.0277(18) 0.0255(17) 0.0225(19) 0.0036(14) 0.0084(14) 0.0018(14) C64 0.0258(17) 0.0208(16) 0.0225(19) -0.0003(13) 0.0085(14) 0.0011(13) C65 0.0267(17) 0.0237(17) 0.029(2) 0.0011(14) 0.0079(15) -0.0028(14) C66 0.0317(19) 0.0280(19) 0.035(2) 0.0053(16) 0.0062(17) -0.0053(15) C67 0.0274(17) 0.0181(16) 0.0228(18) 0.0024(13) 0.0101(14) 0.0009(13) C68 0.0273(17) 0.0241(17) 0.025(2) -0.0008(14) 0.0085(15) -0.0027(14) C69 0.0289(19) 0.033(2) 0.036(2) 0.0151(17) 0.0021(16) -0.0019(16) C70 0.034(2) 0.033(2) 0.033(2) 0.0156(17) 0.0053(17) -0.0067(16) C71 0.0257(17) 0.0189(16) 0.0213(18) 0.0010(13) 0.0050(14) 0.0001(13) C72 0.0255(19) 0.055(3) 0.038(2) -0.0081(19) 0.0127(17) -0.0026(17) C73 0.0218(16) 0.0286(18) 0.0245(19) -0.0022(15) 0.0048(14) -0.0022(14) C74 0.035(2) 0.0285(19) 0.037(2) 0.0003(16) 0.0082(17) -0.0071(16) C75 0.040(2) 0.032(2) 0.047(3) 0.0029(18) 0.0045(19) 0.0061(17) C76 0.0209(16) 0.0286(18) 0.026(2) -0.0002(15) 0.0012(14) 0.0003(14) C77 0.0277(18) 0.042(2) 0.029(2) -0.0023(17) 0.0029(16) -0.0025(16) F1 0.0450(14) 0.0321(12) 0.099(2) 0.0089(13) 0.0413(14) 0.0074(10) F2 0.0507(14) 0.0216(12) 0.120(3) -0.0117(13) 0.0328(16) -0.0049(10) F3 0.0582(16) 0.0497(15) 0.067(2) 0.0256(13) 0.0135(14) 0.0155(12) F4 0.049(7) 0.110(10) 0.075(9) -0.038(7) -0.004(6) -0.014(7) F5 0.015(5) 0.028(6) 0.083(9) 0.016(6) -0.014(6) -0.006(4) F6 0.023(7) 0.065(8) 0.071(9) -0.011(7) 0.013(7) -0.029(5) F4' 0.041(3) 0.040(3) 0.206(10) -0.012(5) -0.022(5) -0.0194(19) F6' 0.042(3) 0.083(4) 0.348(14) 0.000(6) 0.085(6) -0.014(3) F5' 0.085(5) 0.148(7) 0.176(8) 0.073(6) -0.096(5) -0.057(4) F7 0.0659(16) 0.0565(15) 0.0385(15) 0.0162(12) 0.0084(12) -0.0217(13) F8 0.0358(13) 0.0760(18) 0.080(2) 0.0412(15) 0.0050(13) -0.0204(12) F9 0.198(4) 0.0211(13) 0.134(3) 0.0224(15) 0.126(3) 0.0296(17) F10 0.0186(10) 0.0500(13) 0.0443(14) 0.0072(10) -0.0006(9) -0.0100(9) F11 0.0342(11) 0.0282(11) 0.0500(15) 0.0086(10) -0.0074(10) 0.0011(9) F12 0.0368(12) 0.0656(15) 0.0263(13) -0.0051(11) 0.0064(10) -0.0062(11) F13 0.0403(14) 0.0697(17) 0.077(2) -0.0419(15) 0.0189(13) -0.0225(12) F14 0.0757(17) 0.0270(12) 0.0575(17) -0.0133(11) 0.0353(14) -0.0044(11) F15 0.0812(18) 0.0397(13) 0.0378(15) -0.0091(11) 0.0267(13) -0.0160(12) F16 0.0419(13) 0.0546(15) 0.0555(17) 0.0036(13) -0.0055(12) 0.0193(12) F17 0.077(2) 0.127(3) 0.101(3) 0.081(2) -0.003(2) -0.021(2) F18 0.120(3) 0.081(2) 0.085(3) -0.0184(18) -0.014(2) 0.078(2) F19 0.0606(17) 0.093(2) 0.066(2) -0.0539(17) -0.0044(15) -0.0034(15) F20 0.0545(17) 0.097(2) 0.077(2) 0.0240(17) 0.0053(15) -0.0419(16) F21 0.0300(12) 0.0654(16) 0.0500(16) 0.0002(13) 0.0028(11) -0.0094(11) F22 0.089(2) 0.0458(15) 0.0433(17) 0.0138(12) -0.0113(14) -0.0070(14) F23 0.164(3) 0.073(2) 0.120(3) 0.057(2) 0.087(3) 0.080(2) F24 0.095(2) 0.0633(18) 0.080(2) 0.0431(16) -0.0054(18) -0.0371(17) F25 0.068(7) 0.124(11) 0.053(6) 0.020(4) 0.042(4) 0.042(6) F26 0.076(6) 0.033(4) 0.184(15) 0.040(7) 0.078(9) 0.022(4) F27 0.052(6) 0.100(7) 0.091(9) -0.043(6) -0.016(5) 0.045(5) F26' 0.057(5) 0.032(7) 0.110(9) -0.027(6) 0.025(6) 0.017(4) F25' 0.066(11) 0.039(6) 0.20(3) 0.038(10) 0.093(15) 0.023(6) F27' 0.085(14) 0.19(3) 0.035(7) 0.007(11) 0.002(9) 0.098(15) N1 0.0226(14) 0.0316(15) 0.0214(16) -0.0020(12) 0.0089(12) -0.0042(12) N2 0.0286(16) 0.0490(19) 0.0282(18) -0.0067(15) 0.0084(14) 0.0047(14) N3 0.0183(13) 0.0262(14) 0.0193(15) -0.0018(12) 0.0039(11) -0.0003(11) N4 0.0231(15) 0.0336(16) 0.0244(16) 0.0050(13) 0.0064(12) 0.0022(12) N5 0.0267(15) 0.0309(16) 0.0243(17) 0.0038(13) 0.0036(13) -0.0074(12) N6 0.0205(13) 0.0230(14) 0.0231(16) -0.0016(12) 0.0041(12) -0.0015(11) O1 0.0210(11) 0.0210(12) 0.0287(14) 0.0000(10) 0.0080(10) -0.0020(9) O2 0.0167(11) 0.0281(13) 0.0326(15) -0.0041(10) 0.0068(10) -0.0044(9) O3 0.0184(11) 0.0246(12) 0.0256(13) 0.0000(10) 0.0047(10) -0.0032(9) O4 0.0164(11) 0.0247(12) 0.0244(13) 0.0006(9) 0.0050(9) -0.0044(9) O5 0.0252(12) 0.0245(12) 0.0320(14) -0.0040(10) 0.0114(10) -0.0016(10) O6 0.0205(11) 0.0258(13) 0.0338(15) -0.0008(10) 0.0058(10) 0.0027(10) O7 0.0223(11) 0.0321(13) 0.0211(13) -0.0021(10) 0.0088(10) 0.0000(10) O8 0.0313(14) 0.0579(17) 0.0319(15) 0.0128(13) 0.0135(12) 0.0003(12) O9 0.0260(12) 0.0306(13) 0.0250(14) -0.0029(10) 0.0118(10) -0.0024(10) O10 0.0521(18) 0.097(2) 0.0309(18) -0.0156(17) 0.0110(14) 0.0252(17) O11 0.0290(13) 0.0530(16) 0.0299(15) -0.0016(12) 0.0086(11) 0.0111(12) O12 0.0199(12) 0.0409(15) 0.0337(15) 0.0057(11) -0.0011(10) -0.0023(10) O13 0.0239(13) 0.0445(16) 0.0473(18) 0.0150(13) -0.0011(12) -0.0087(11) O14 0.0272(12) 0.0269(13) 0.0269(14) -0.0007(10) 0.0090(10) -0.0052(10) O15 0.0337(13) 0.0211(12) 0.0307(15) 0.0024(10) 0.0087(11) -0.0038(10) O16 0.0298(12) 0.0199(12) 0.0295(14) 0.0011(10) 0.0115(11) 0.0023(10) O17 0.0288(12) 0.0272(12) 0.0190(13) 0.0008(10) 0.0076(10) -0.0019(10) O18 0.0426(15) 0.0553(17) 0.0289(16) 0.0110(13) 0.0072(12) -0.0108(13) _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 Tb1 O17 2.342(2) . ? Tb1 O17 2.342(2) 2_756 ? Tb1 O14 2.344(2) . ? Tb1 O14 2.344(2) 2_756 ? Tb1 O16 2.373(2) . ? Tb1 O16 2.373(2) 2_756 ? Tb1 O15 2.388(2) 2_756 ? Tb1 O15 2.388(2) . ? Tb2 O7 2.316(2) . ? Tb2 O4 2.336(2) . ? Tb2 O9 2.348(2) . ? Tb2 O1 2.349(2) . ? Tb2 O6 2.362(2) . ? Tb2 O5 2.372(2) . ? Tb2 O3 2.373(2) . ? Tb2 O2 2.394(2) . ? C1 F2 1.322(4) . ? C1 F1 1.336(4) . ? C1 F3 1.341(5) . ? C1 C2 1.531(5) . ? C2 O1 1.244(4) . ? C2 C3 1.388(5) . ? C3 C4 1.393(5) . ? C3 H3 0.9300 . ? C4 O2 1.240(4) . ? C4 C5 1.534(6) . ? C5 F5 1.056(15) . ? C5 F4' 1.276(9) . ? C5 F5' 1.293(10) . ? C5 F6' 1.403(8) . ? C5 F4 1.408(9) . ? C5 F6 1.45(3) . ? C6 F9 1.293(4) . ? C6 F7 1.317(4) . ? C6 F8 1.333(4) . ? C6 C7 1.531(5) . ? C7 O3 1.255(4) . ? C7 C8 1.382(5) . ? C8 C9 1.393(5) . ? C8 H8 0.9300 . ? C9 O4 1.250(4) . ? C9 C10 1.529(4) . ? C10 F11 1.324(4) . ? C10 F10 1.330(4) . ? C10 F12 1.334(4) . ? C11 F13 1.326(4) . ? C11 F15 1.331(4) . ? C11 F14 1.338(4) . ? C11 C12 1.530(5) . ? C12 O5 1.252(4) . ? C12 C13 1.385(5) . ? C13 C14 1.384(5) . ? C13 H13 0.9300 . ? C14 O6 1.247(4) . ? C14 C15 1.536(5) . ? C15 F16 1.314(5) . ? C15 F18 1.315(5) . ? C15 F17 1.323(5) . ? C16 F21 1.314(5) . ? C16 F19 1.321(5) . ? C16 F20 1.344(5) . ? C16 C17 1.533(5) . ? C17 O14 1.251(4) . ? C17 C18 1.381(5) . ? C18 C19 1.384(5) . ? C18 H18 0.9300 . ? C19 O15 1.256(4) . ? C19 C20 1.543(5) . ? C20 F23 1.301(5) . ? C20 F22 1.308(5) . ? C20 F24 1.327(5) . ? C21 F27' 1.21(2) . ? C21 F25' 1.27(2) . ? C21 F26 1.308(10) . ? C21 F25 1.309(12) . ? C21 F26' 1.329(16) . ? C21 F27 1.339(13) . ? C21 C22 1.543(5) . ? C22 O16 1.249(4) . ? C22 C23 1.381(4) . ? C23 C22 1.381(4) 2_756 ? C23 H23 0.9300 . ? C24 O11 1.435(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.354(5) . ? C25 O11 1.366(4) . ? C25 C26 1.422(5) . ? C26 C27 1.354(5) . ? C26 H26 0.9300 . ? C27 C28 1.423(5) . ? C27 H27 0.9300 . ? C28 C31 1.407(5) . ? C28 C29 1.416(5) . ? C29 C34 1.411(5) . ? C29 C30 1.418(5) . ? C30 H30 0.9300 . ? C31 C32 1.380(5) . ? C31 H31 0.9300 . ? C32 C33 1.426(5) . ? C32 C35 1.456(5) . ? C33 C34 1.364(5) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 N1 1.338(4) . ? C35 N2 1.366(5) . ? C36 C37 1.525(5) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N1 1.497(4) . ? C37 C38 1.529(5) . ? C37 C40 1.536(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.523(5) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 N2 1.501(5) . ? C40 C41 1.530(5) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 O12 1.433(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C48 1.367(5) . ? C43 O12 1.369(4) . ? C43 C44 1.407(5) . ? C44 C45 1.363(5) . ? C44 H44 0.9300 . ? C45 C46 1.420(4) . ? C45 H45 0.9300 . ? C46 C52 1.405(4) . ? C46 C47 1.419(4) . ? C47 C49 1.413(4) . ? C47 C48 1.417(4) . ? C48 H48 0.9300 . ? C49 C50 1.363(4) . ? C49 H49 0.9300 . ? C50 C51 1.418(4) . ? C50 H50 0.9300 . ? C51 C52 1.374(4) . ? C51 C53 1.459(4) . ? C52 H52 0.9300 . ? C53 N3 1.327(4) . ? C53 N4 1.370(4) . ? C54 C55 1.513(5) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 N4 1.507(4) . ? C55 C56 1.527(5) . ? C55 C58 1.545(5) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.525(5) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 N3 1.495(4) . ? C58 C59 1.517(5) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 O13 1.427(5) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C66 1.359(5) . ? C61 O13 1.374(4) . ? C61 C62 1.414(5) . ? C62 C63 1.361(5) . ? C62 H62 0.9300 . ? C63 C64 1.414(4) . ? C63 H63 0.9300 . ? C64 C67 1.412(4) . ? C64 C65 1.420(5) . ? C65 C70 1.406(5) . ? C65 C66 1.412(5) . ? C66 H66 0.9300 . ? C67 C68 1.371(5) . ? C67 H67 0.9300 . ? C68 C69 1.424(5) . ? C68 C71 1.463(4) . ? C69 C70 1.366(5) . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C71 N6 1.332(4) . ? C71 N5 1.365(4) . ? C72 C73 1.526(5) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 N6 1.502(4) . ? C73 C74 1.522(5) . ? C73 C76 1.556(5) . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 C76 1.520(5) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 N5 1.503(4) . ? C76 C77 1.518(5) . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? N1 O9 1.305(3) . ? N2 O10 1.265(4) . ? N3 O7 1.306(3) . ? N4 O8 1.266(4) . ? N5 O18 1.274(4) . ? N6 O17 1.299(3) . ? 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 O17 Tb1 O17 136.50(11) . 2_756 ? O17 Tb1 O14 102.40(8) . . ? O17 Tb1 O14 94.21(8) 2_756 . ? O17 Tb1 O14 94.21(8) . 2_756 ? O17 Tb1 O14 102.40(8) 2_756 2_756 ? O14 Tb1 O14 134.25(11) . 2_756 ? O17 Tb1 O16 71.43(8) . . ? O17 Tb1 O16 74.09(8) 2_756 . ? O14 Tb1 O16 76.20(8) . . ? O14 Tb1 O16 149.32(8) 2_756 . ? O17 Tb1 O16 74.09(8) . 2_756 ? O17 Tb1 O16 71.43(8) 2_756 2_756 ? O14 Tb1 O16 149.32(8) . 2_756 ? O14 Tb1 O16 76.20(8) 2_756 2_756 ? O16 Tb1 O16 73.83(11) . 2_756 ? O17 Tb1 O15 150.59(8) . 2_756 ? O17 Tb1 O15 72.83(8) 2_756 2_756 ? O14 Tb1 O15 72.00(8) . 2_756 ? O14 Tb1 O15 72.83(8) 2_756 2_756 ? O16 Tb1 O15 131.53(8) . 2_756 ? O16 Tb1 O15 125.42(8) 2_756 2_756 ? O17 Tb1 O15 72.83(8) . . ? O17 Tb1 O15 150.59(8) 2_756 . ? O14 Tb1 O15 72.83(8) . . ? O14 Tb1 O15 72.00(8) 2_756 . ? O16 Tb1 O15 125.42(8) . . ? O16 Tb1 O15 131.53(8) 2_756 . ? O15 Tb1 O15 78.02(11) 2_756 . ? O7 Tb2 O4 107.40(8) . . ? O7 Tb2 O9 135.69(8) . . ? O4 Tb2 O9 91.82(8) . . ? O7 Tb2 O1 72.37(8) . . ? O4 Tb2 O1 74.11(7) . . ? O9 Tb2 O1 75.41(8) . . ? O7 Tb2 O6 89.48(8) . . ? O4 Tb2 O6 137.64(8) . . ? O9 Tb2 O6 102.77(8) . . ? O1 Tb2 O6 147.92(8) . . ? O7 Tb2 O5 150.00(8) . . ? O4 Tb2 O5 74.20(8) . . ? O9 Tb2 O5 73.05(8) . . ? O1 Tb2 O5 133.91(8) . . ? O6 Tb2 O5 72.58(8) . . ? O7 Tb2 O3 75.39(8) . . ? O4 Tb2 O3 72.58(7) . . ? O9 Tb2 O3 148.86(8) . . ? O1 Tb2 O3 123.08(7) . . ? O6 Tb2 O3 74.82(8) . . ? O5 Tb2 O3 76.76(8) . . ? O7 Tb2 O2 73.17(8) . . ? O4 Tb2 O2 146.09(7) . . ? O9 Tb2 O2 69.24(8) . . ? O1 Tb2 O2 73.98(8) . . ? O6 Tb2 O2 75.54(8) . . ? O5 Tb2 O2 122.66(8) . . ? O3 Tb2 O2 136.45(8) . . ? F2 C1 F1 107.8(3) . . ? F2 C1 F3 106.9(3) . . ? F1 C1 F3 106.7(3) . . ? F2 C1 C2 113.8(3) . . ? F1 C1 C2 111.0(3) . . ? F3 C1 C2 110.4(3) . . ? O1 C2 C3 128.8(3) . . ? O1 C2 C1 112.8(3) . . ? C3 C2 C1 118.4(3) . . ? C2 C3 C4 121.6(3) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? O2 C4 C3 129.4(3) . . ? O2 C4 C5 113.6(3) . . ? C3 C4 C5 117.0(4) . . ? F5 C5 F4' 121.1(9) . . ? F5 C5 F5' 52.1(10) . . ? F4' C5 F5' 114.0(7) . . ? F5 C5 F6' 49.6(10) . . ? F4' C5 F6' 103.6(7) . . ? F5' C5 F6' 101.8(8) . . ? F5 C5 F4 103.9(14) . . ? F4' C5 F4 73.4(9) . . ? F5' C5 F4 54.7(9) . . ? F6' C5 F4 148.3(8) . . ? F5 C5 F6 119.4(14) . . ? F4' C5 F6 27.4(10) . . ? F5' C5 F6 137.5(9) . . ? F6' C5 F6 83.5(10) . . ? F4 C5 F6 100.2(13) . . ? F5 C5 C4 120.8(9) . . ? F4' C5 C4 116.7(5) . . ? F5' C5 C4 113.1(6) . . ? F6' C5 C4 105.6(5) . . ? F4 C5 C4 103.7(7) . . ? F6 C5 C4 105.6(9) . . ? F9 C6 F7 108.1(3) . . ? F9 C6 F8 107.8(3) . . ? F7 C6 F8 103.4(3) . . ? F9 C6 C7 110.7(3) . . ? F7 C6 C7 112.8(3) . . ? F8 C6 C7 113.7(3) . . ? O3 C7 C8 128.5(3) . . ? O3 C7 C6 113.3(3) . . ? C8 C7 C6 118.2(3) . . ? C7 C8 C9 121.1(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? O4 C9 C8 127.4(3) . . ? O4 C9 C10 113.9(3) . . ? C8 C9 C10 118.6(3) . . ? F11 C10 F10 107.4(3) . . ? F11 C10 F12 107.5(3) . . ? F10 C10 F12 106.9(3) . . ? F11 C10 C9 111.2(3) . . ? F10 C10 C9 113.6(3) . . ? F12 C10 C9 110.0(3) . . ? F13 C11 F15 107.9(4) . . ? F13 C11 F14 106.7(3) . . ? F15 C11 F14 106.6(3) . . ? F13 C11 C12 110.8(3) . . ? F15 C11 C12 110.8(3) . . ? F14 C11 C12 113.8(3) . . ? O5 C12 C13 128.2(3) . . ? O5 C12 C11 113.1(3) . . ? C13 C12 C11 118.7(3) . . ? C14 C13 C12 121.4(3) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? O6 C14 C13 128.2(3) . . ? O6 C14 C15 115.1(3) . . ? C13 C14 C15 116.6(3) . . ? F16 C15 F18 106.3(4) . . ? F16 C15 F17 106.1(4) . . ? F18 C15 F17 108.1(4) . . ? F16 C15 C14 112.6(3) . . ? F18 C15 C14 113.3(4) . . ? F17 C15 C14 110.0(3) . . ? F21 C16 F19 106.8(4) . . ? F21 C16 F20 106.1(4) . . ? F19 C16 F20 107.8(4) . . ? F21 C16 C17 113.8(3) . . ? F19 C16 C17 109.7(3) . . ? F20 C16 C17 112.3(3) . . ? O14 C17 C18 128.5(3) . . ? O14 C17 C16 115.0(3) . . ? C18 C17 C16 116.4(3) . . ? C17 C18 C19 121.5(3) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? O15 C19 C18 127.9(3) . . ? O15 C19 C20 113.4(3) . . ? C18 C19 C20 118.6(3) . . ? F23 C20 F22 109.0(4) . . ? F23 C20 F24 106.4(4) . . ? F22 C20 F24 105.3(4) . . ? F23 C20 C19 110.6(4) . . ? F22 C20 C19 112.0(3) . . ? F24 C20 C19 113.2(3) . . ? F27' C21 F25' 112.6(15) . . ? F27' C21 F26 79.8(14) . . ? F25' C21 F26 120.7(10) . . ? F27' C21 F25 130.7(17) . . ? F25' C21 F25 21.0(17) . . ? F26 C21 F25 109.1(10) . . ? F27' C21 F26' 109.4(15) . . ? F25' C21 F26' 101.5(12) . . ? F26 C21 F26' 30.4(7) . . ? F25 C21 F26' 84.3(11) . . ? F27' C21 F27 32(2) . . ? F25' C21 F27 83.1(14) . . ? F26 C21 F27 105.3(10) . . ? F25 C21 F27 103.4(10) . . ? F26' C21 F27 129.7(10) . . ? F27' C21 C22 108.9(11) . . ? F25' C21 C22 113.4(10) . . ? F26 C21 C22 116.1(6) . . ? F25 C21 C22 109.4(7) . . ? F26' C21 C22 110.8(7) . . ? F27 C21 C22 112.7(7) . . ? O16 C22 C23 128.4(3) . . ? O16 C22 C21 113.4(3) . . ? C23 C22 C21 118.2(3) . . ? C22 C23 C22 122.8(4) . 2_756 ? C22 C23 H23 118.6 . . ? C22 C23 H23 118.6 2_756 . ? O11 C24 H24A 109.5 . . ? O11 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O11 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 O11 125.6(3) . . ? C30 C25 C26 120.9(3) . . ? O11 C25 C26 113.5(3) . . ? C27 C26 C25 119.9(3) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 121.1(3) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C31 C28 C29 119.8(3) . . ? C31 C28 C27 121.9(3) . . ? C29 C28 C27 118.3(3) . . ? C34 C29 C28 117.8(3) . . ? C34 C29 C30 122.4(3) . . ? C28 C29 C30 119.7(3) . . ? C25 C30 C29 120.0(3) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C28 121.5(3) . . ? C32 C31 H31 119.3 . . ? C28 C31 H31 119.3 . . ? C31 C32 C33 118.5(3) . . ? C31 C32 C35 121.1(3) . . ? C33 C32 C35 120.3(3) . . ? C34 C33 C32 120.3(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C29 122.0(3) . . ? C33 C34 H34 119.0 . . ? C29 C34 H34 119.0 . . ? N1 C35 N2 106.5(3) . . ? N1 C35 C32 127.6(3) . . ? N2 C35 C32 125.8(3) . . ? C37 C36 H36A 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C37 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N1 C37 C36 110.3(3) . . ? N1 C37 C38 105.7(3) . . ? C36 C37 C38 109.6(3) . . ? N1 C37 C40 100.6(3) . . ? C36 C37 C40 115.4(3) . . ? C38 C37 C40 114.4(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N2 C40 C39 106.5(3) . . ? N2 C40 C41 108.7(3) . . ? C39 C40 C41 111.0(4) . . ? N2 C40 C37 100.3(3) . . ? C39 C40 C37 114.2(3) . . ? C41 C40 C37 115.1(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O12 C42 H42A 109.5 . . ? O12 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O12 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 O12 124.5(3) . . ? C48 C43 C44 121.1(3) . . ? O12 C43 C44 114.4(3) . . ? C45 C44 C43 120.3(3) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.7(3) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C52 C46 C47 119.5(3) . . ? C52 C46 C45 121.9(3) . . ? C47 C46 C45 118.5(3) . . ? C49 C47 C48 121.6(3) . . ? C49 C47 C46 118.5(3) . . ? C48 C47 C46 119.8(3) . . ? C43 C48 C47 119.6(3) . . ? C43 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C50 C49 C47 121.2(3) . . ? C50 C49 H49 119.4 . . ? C47 C49 H49 119.4 . . ? C49 C50 C51 120.1(3) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 119.9(3) . . ? C52 C51 C53 120.7(3) . . ? C50 C51 C53 119.4(3) . . ? C51 C52 C46 120.7(3) . . ? C51 C52 H52 119.7 . . ? C46 C52 H52 119.7 . . ? N3 C53 N4 107.6(3) . . ? N3 C53 C51 126.5(3) . . ? N4 C53 C51 125.9(3) . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N4 C55 C54 110.0(3) . . ? N4 C55 C56 105.7(3) . . ? C54 C55 C56 111.0(3) . . ? N4 C55 C58 99.9(3) . . ? C54 C55 C58 115.1(3) . . ? C56 C55 C58 114.0(3) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 H57A 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C58 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N3 C58 C59 110.7(3) . . ? N3 C58 C57 105.6(3) . . ? C59 C58 C57 110.9(3) . . ? N3 C58 C55 100.0(2) . . ? C59 C58 C55 114.9(3) . . ? C57 C58 C55 113.8(3) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O13 C60 H60A 109.5 . . ? O13 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O13 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C66 C61 O13 125.2(3) . . ? C66 C61 C62 121.0(3) . . ? O13 C61 C62 113.8(3) . . ? C63 C62 C61 119.8(3) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 121.1(3) . . ? C62 C63 H63 119.4 . . ? C64 C63 H63 119.4 . . ? C67 C64 C63 122.1(3) . . ? C67 C64 C65 119.6(3) . . ? C63 C64 C65 118.4(3) . . ? C70 C65 C66 122.2(3) . . ? C70 C65 C64 118.1(3) . . ? C66 C65 C64 119.7(3) . . ? C61 C66 C65 120.0(3) . . ? C61 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C68 C67 C64 121.1(3) . . ? C68 C67 H67 119.4 . . ? C64 C67 H67 119.4 . . ? C67 C68 C69 119.2(3) . . ? C67 C68 C71 121.7(3) . . ? C69 C68 C71 119.1(3) . . ? C70 C69 C68 120.2(3) . . ? C70 C69 H69 119.9 . . ? C68 C69 H69 119.9 . . ? C69 C70 C65 121.8(3) . . ? C69 C70 H70 119.1 . . ? C65 C70 H70 119.1 . . ? N6 C71 N5 108.0(3) . . ? N6 C71 C68 126.8(3) . . ? N5 C71 C68 125.2(3) . . ? C73 C72 H72A 109.5 . . ? C73 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C73 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N6 C73 C74 106.4(3) . . ? N6 C73 C72 109.9(3) . . ? C74 C73 C72 110.0(3) . . ? N6 C73 C76 100.5(2) . . ? C74 C73 C76 114.3(3) . . ? C72 C73 C76 114.9(3) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 H75A 109.5 . . ? C76 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C76 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N5 C76 C77 109.2(3) . . ? N5 C76 C75 106.3(3) . . ? C77 C76 C75 110.8(3) . . ? N5 C76 C73 100.3(2) . . ? C77 C76 C73 114.9(3) . . ? C75 C76 C73 114.3(3) . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? O9 N1 C35 125.9(3) . . ? O9 N1 C37 119.6(3) . . ? C35 N1 C37 113.0(3) . . ? O10 N2 C35 127.0(3) . . ? O10 N2 C40 119.9(3) . . ? C35 N2 C40 112.8(3) . . ? O7 N3 C53 126.2(3) . . ? O7 N3 C58 120.0(2) . . ? C53 N3 C58 112.8(3) . . ? O8 N4 C53 126.3(3) . . ? O8 N4 C55 122.2(3) . . ? C53 N4 C55 111.1(3) . . ? O18 N5 C71 126.6(3) . . ? O18 N5 C76 120.9(3) . . ? C71 N5 C76 111.9(3) . . ? O17 N6 C71 126.3(3) . . ? O17 N6 C73 119.7(3) . . ? C71 N6 C73 113.0(3) . . ? C2 O1 Tb2 133.9(2) . . ? C4 O2 Tb2 132.1(2) . . ? C7 O3 Tb2 133.9(2) . . ? C9 O4 Tb2 135.9(2) . . ? C12 O5 Tb2 134.1(2) . . ? C14 O6 Tb2 134.3(2) . . ? N3 O7 Tb2 140.41(19) . . ? N1 O9 Tb2 137.70(18) . . ? C25 O11 C24 117.2(3) . . ? C43 O12 C42 116.4(3) . . ? C61 O13 C60 117.0(3) . . ? C17 O14 Tb1 133.0(2) . . ? C19 O15 Tb1 132.9(2) . . ? C22 O16 Tb1 133.3(2) . . ? N6 O17 Tb1 141.50(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.371 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.085 # Attachment '- complex-5.cif' data_shelxle _database_code_depnum_ccdc_archive 'CCDC 779519' #TrackingRef '- complex-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H45 F18 Ho N4 O12' _chemical_formula_weight 1412.84 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.844(2) _cell_length_b 14.694(3) _cell_length_c 17.860(4) _cell_angle_alpha 97.57(3) _cell_angle_beta 93.51(3) _cell_angle_gamma 107.98(3) _cell_volume 2913.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11465 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.68 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 1.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.790 _exptl_absorpt_correction_T_max 0.838 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23245 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.1442 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10190 _reflns_number_gt 6644 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Fluorine atoms in the CF3 groups were treated by disorder and these atoms were refined anisotropically with application of restraints on interatomic distances and thermal parameters (DFIX, ISOR and SIMU instructions in SHELXL).The most disagreeable reflections of the compound were also omitted. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0081P)^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 10190 _refine_ls_number_parameters 813 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 0.852 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.001 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 Ho1 Ho 0.64599(2) 0.259178(17) 0.262139(16) 0.03912(8) Uani 1 1 d . A . C1 C 0.3189(5) 0.1603(4) 0.4012(4) 0.0632(17) Uani 1 1 d U . . C2 C 0.3796(4) 0.1675(3) 0.3284(3) 0.0392(13) Uani 1 1 d . . . C3 C 0.3105(4) 0.1366(4) 0.2584(4) 0.0587(16) Uani 1 1 d . . . H3 H 0.2285 0.1071 0.2568 0.070 Uiso 1 1 calc R . . C4 C 0.3610(5) 0.1487(4) 0.1911(3) 0.0517(13) Uani 1 1 d U A . C5 C 0.2753(7) 0.1112(6) 0.1171(5) 0.101(2) Uani 1 1 d DU . . C6 C 0.8399(6) 0.3777(5) 0.5068(4) 0.0687(18) Uani 1 1 d . . . C7 C 0.8286(5) 0.3324(3) 0.4240(3) 0.0505(15) Uani 1 1 d . A . C8 C 0.9314(4) 0.3196(4) 0.3946(4) 0.0573(16) Uani 1 1 d . . . H8 H 1.0033 0.3402 0.4258 0.069 Uiso 1 1 calc R . . C9 C 0.9274(4) 0.2772(4) 0.3206(4) 0.0485(15) Uani 1 1 d . A . C10 C 1.0445(5) 0.2695(5) 0.2916(5) 0.081(2) Uani 1 1 d . . . C11 C 0.9425(6) 0.5430(5) 0.2304(5) 0.085(2) Uani 1 1 d . . . C12 C 0.8512(5) 0.4421(4) 0.2035(4) 0.0508(15) Uani 1 1 d . A . C13 C 0.8551(4) 0.3957(4) 0.1321(4) 0.0578(16) Uani 1 1 d . . . H13 H 0.9100 0.4275 0.1014 0.069 Uiso 1 1 calc R . . C14 C 0.7795(5) 0.3024(4) 0.1044(3) 0.0504(15) Uani 1 1 d . A . C15 C 0.7948(6) 0.2558(5) 0.0244(4) 0.0715(19) Uani 1 1 d . . . C16 C 0.8875(6) 0.1570(4) 0.7766(4) 0.100(2) Uani 1 1 d . . . H16A H 0.9008 0.0957 0.7653 0.151 Uiso 1 1 calc R . . H16B H 0.8831 0.1714 0.8301 0.151 Uiso 1 1 calc R . . H16C H 0.9522 0.2068 0.7618 0.151 Uiso 1 1 calc R . . C17 C 0.7714(6) 0.1369(4) 0.6579(4) 0.0679(18) Uani 1 1 d . . . C18 C 0.8593(5) 0.1263(4) 0.6153(4) 0.0620(17) Uani 1 1 d . . . H18 H 0.9342 0.1325 0.6387 0.074 Uiso 1 1 calc R . . C19 C 0.8356(5) 0.1058(3) 0.5352(4) 0.0503(15) Uani 1 1 d . . . C20 C 0.7214(5) 0.0961(3) 0.4988(3) 0.0465(15) Uani 1 1 d . . . C21 C 0.6328(5) 0.1103(4) 0.5449(4) 0.0702(19) Uani 1 1 d . . . H21 H 0.5584 0.1071 0.5226 0.084 Uiso 1 1 calc R . . C22 C 0.6571(5) 0.1285(4) 0.6213(4) 0.0734(19) Uani 1 1 d . . . H22 H 0.5977 0.1358 0.6510 0.088 Uiso 1 1 calc R . . C23 C 0.9218(5) 0.0894(4) 0.4878(4) 0.0643(18) Uani 1 1 d . . . H23 H 0.9979 0.0970 0.5101 0.077 Uiso 1 1 calc R . . C24 C 0.8975(5) 0.0631(4) 0.4115(4) 0.0633(17) Uani 1 1 d . . . H24 H 0.9561 0.0516 0.3828 0.076 Uiso 1 1 calc R . . C25 C 0.7829(5) 0.0528(3) 0.3747(4) 0.0506(15) Uani 1 1 d . . . C26 C 0.6984(5) 0.0721(3) 0.4193(3) 0.0507(15) Uani 1 1 d . . . H26 H 0.6247 0.0691 0.3959 0.061 Uiso 1 1 calc R . . C27 C 0.7532(4) 0.0192(3) 0.2938(4) 0.0491(15) Uani 1 1 d . . . C28 C 0.7467(5) -0.1584(3) 0.1301(3) 0.081(2) Uani 1 1 d . . . H28A H 0.8220 -0.1699 0.1368 0.122 Uiso 1 1 calc R . . H28B H 0.7221 -0.1659 0.0768 0.122 Uiso 1 1 calc R . . H28C H 0.6880 -0.2042 0.1529 0.122 Uiso 1 1 calc R . . C29 C 0.7598(5) -0.0563(4) 0.1675(4) 0.0576(16) Uani 1 1 d . . . C30 C 0.8562(4) 0.0174(4) 0.1341(3) 0.0729(19) Uani 1 1 d . . . H30A H 0.8616 0.0817 0.1570 0.109 Uiso 1 1 calc R . . H30B H 0.8361 0.0098 0.0802 0.109 Uiso 1 1 calc R . . H30C H 0.9315 0.0072 0.1440 0.109 Uiso 1 1 calc R . . C31 C 0.5348(4) -0.1179(4) 0.1859(3) 0.0740(19) Uani 1 1 d . . . H31A H 0.5574 -0.1448 0.2283 0.111 Uiso 1 1 calc R . . H31B H 0.5114 -0.1670 0.1416 0.111 Uiso 1 1 calc R . . H31C H 0.4691 -0.0950 0.1968 0.111 Uiso 1 1 calc R . . C32 C 0.6409(5) -0.0335(3) 0.1714(3) 0.0531(15) Uani 1 1 d . . . C33 C 0.6066(5) 0.0132(4) 0.1061(3) 0.0685(18) Uani 1 1 d . . . H33A H 0.5364 0.0304 0.1157 0.103 Uiso 1 1 calc R . . H33B H 0.5908 -0.0319 0.0596 0.103 Uiso 1 1 calc R . . H33C H 0.6710 0.0703 0.1018 0.103 Uiso 1 1 calc R . . C34 C 0.7157(5) 0.3570(4) -0.2231(3) 0.0781(19) Uani 1 1 d . . . H34A H 0.7529 0.3244 -0.1910 0.117 Uiso 1 1 calc R . . H34B H 0.7419 0.3508 -0.2728 0.117 Uiso 1 1 calc R . . H34C H 0.6306 0.3283 -0.2268 0.117 Uiso 1 1 calc R . . C35 C 0.7228(5) 0.4765(4) -0.1183(4) 0.0597(16) Uani 1 1 d . . . C36 C 0.7855(5) 0.5705(4) -0.0805(4) 0.0670(18) Uani 1 1 d . . . H36 H 0.8379 0.6137 -0.1061 0.080 Uiso 1 1 calc R . . C37 C 0.7713(5) 0.5992(4) -0.0082(4) 0.0693(18) Uani 1 1 d . . . H37 H 0.8155 0.6615 0.0154 0.083 Uiso 1 1 calc R . . C38 C 0.6890(4) 0.5359(4) 0.0341(4) 0.0495(15) Uani 1 1 d . . . C39 C 0.6237(4) 0.4419(4) -0.0059(3) 0.0467(14) Uani 1 1 d . . . C40 C 0.6415(5) 0.4145(4) -0.0820(3) 0.0537(15) Uani 1 1 d . . . H40 H 0.5971 0.3534 -0.1078 0.064 Uiso 1 1 calc R . . C41 C 0.5417(4) 0.3793(4) 0.0342(3) 0.0515(15) Uani 1 1 d . . . H41 H 0.4957 0.3185 0.0088 0.062 Uiso 1 1 calc R . . C42 C 0.5276(4) 0.4047(4) 0.1084(3) 0.0479(15) Uani 1 1 d . . . H42 H 0.4732 0.3612 0.1327 0.057 Uiso 1 1 calc R . . C43 C 0.5954(4) 0.4968(3) 0.1485(3) 0.0422(13) Uani 1 1 d . . . C44 C 0.6732(4) 0.5604(3) 0.1094(3) 0.0522(15) Uani 1 1 d . . . H44 H 0.7165 0.6220 0.1348 0.063 Uiso 1 1 calc R . . C45 C 0.5839(4) 0.5222(4) 0.2277(4) 0.0500(15) Uani 1 1 d . . . C46 C 0.5926(5) 0.4737(4) 0.4198(3) 0.0764(19) Uani 1 1 d . . . H46A H 0.5458 0.4083 0.4228 0.115 Uiso 1 1 calc R . . H46B H 0.5940 0.5148 0.4665 0.115 Uiso 1 1 calc R . . H46C H 0.6726 0.4760 0.4113 0.115 Uiso 1 1 calc R . . C47 C 0.5374(5) 0.5086(4) 0.3542(3) 0.0598(16) Uani 1 1 d . . . C48 C 0.3991(4) 0.4761(4) 0.3519(3) 0.0670(18) Uani 1 1 d . . . H48A H 0.3661 0.4955 0.3086 0.101 Uiso 1 1 calc R . . H48B H 0.3774 0.5057 0.3975 0.101 Uiso 1 1 calc R . . H48C H 0.3686 0.4069 0.3481 0.101 Uiso 1 1 calc R . . C49 C 0.7297(5) 0.6587(4) 0.3811(4) 0.093(2) Uani 1 1 d . . . H49A H 0.7692 0.6121 0.3665 0.140 Uiso 1 1 calc R . . H49B H 0.7364 0.6731 0.4356 0.140 Uiso 1 1 calc R . . H49C H 0.7664 0.7169 0.3610 0.140 Uiso 1 1 calc R . . C50 C 0.5956(5) 0.6165(4) 0.3493(4) 0.0604(16) Uani 1 1 d . . . C51 C 0.5287(5) 0.6835(4) 0.3828(4) 0.084(2) Uani 1 1 d . . . H51A H 0.5707 0.7490 0.3769 0.126 Uiso 1 1 calc R . . H51B H 0.5236 0.6796 0.4357 0.126 Uiso 1 1 calc R . . H51C H 0.4497 0.6640 0.3566 0.126 Uiso 1 1 calc R . . F1 F 0.3225(3) 0.2468(2) 0.4361(2) 0.0817(10) Uani 1 1 d . . . F2 F 0.2014(3) 0.1071(2) 0.38981(19) 0.0759(10) Uani 1 1 d U . . F3 F 0.3684(3) 0.1216(2) 0.4516(2) 0.0876(12) Uani 1 1 d . . . F4 F 0.3023(7) 0.1715(6) 0.0657(5) 0.1128(17) Uani 0.587(5) 1 d PU A 1 F5 F 0.2872(7) 0.0272(6) 0.0830(5) 0.1134(17) Uani 0.587(5) 1 d PU A 1 F6 F 0.1609(7) 0.0929(7) 0.1248(5) 0.1102(18) Uani 0.587(5) 1 d PU A 1 F4' F 0.3238(9) 0.0909(10) 0.0548(6) 0.1133(18) Uani 0.413(5) 1 d PDU A 2 F5' F 0.1731(10) 0.0398(8) 0.1200(7) 0.1118(18) Uani 0.413(5) 1 d PDU A 2 F6' F 0.2370(10) 0.1863(7) 0.1001(6) 0.1110(18) Uani 0.413(5) 1 d PDU A 2 F7 F 0.8531(4) 0.4708(2) 0.5133(2) 0.1127(14) Uani 1 1 d . . . F8 F 0.9294(4) 0.3713(3) 0.5500(2) 0.1327(17) Uani 1 1 d . . . F9 F 0.7421(4) 0.3410(3) 0.5397(2) 0.1178(14) Uani 1 1 d . . . F10 F 1.1358(3) 0.3005(3) 0.3444(3) 0.151(2) Uani 1 1 d . . . F11 F 1.0372(3) 0.1790(3) 0.2725(3) 0.1219(16) Uani 1 1 d . . . F12 F 1.0718(4) 0.3115(4) 0.2362(3) 0.197(3) Uani 1 1 d . . . F13 F 1.0200(4) 0.5455(3) 0.2828(2) 0.1325(18) Uani 1 1 d . . . F14 F 1.0010(3) 0.5822(2) 0.1731(2) 0.1001(13) Uani 1 1 d . . . F15 F 0.8853(3) 0.6051(3) 0.2514(2) 0.1127(13) Uani 1 1 d U . . F16 F 0.8531(4) 0.1948(3) 0.0306(2) 0.1228(16) Uani 1 1 d . . . F17 F 0.8509(3) 0.3169(3) -0.0187(2) 0.1052(13) Uani 1 1 d . . . F18 F 0.6903(4) 0.2062(3) -0.0138(2) 0.1217(15) Uani 1 1 d . . . N1 N 0.5622(3) 0.4628(3) 0.2799(3) 0.0482(12) Uani 1 1 d . A . N2 N 0.5919(4) 0.6117(3) 0.2644(3) 0.0574(13) Uani 1 1 d . . . N3 N 0.6732(3) 0.0359(3) 0.2451(3) 0.0453(11) Uani 1 1 d . A . N4 N 0.7987(4) -0.0444(3) 0.2509(3) 0.0598(14) Uani 1 1 d . . . O1 O 0.4908(3) 0.2047(2) 0.34064(18) 0.0433(9) Uani 1 1 d . . . O2 O 0.4674(3) 0.1853(2) 0.18039(19) 0.0457(9) Uani 1 1 d . . . O3 O 0.7275(3) 0.3126(2) 0.3881(2) 0.0521(10) Uani 1 1 d . . . O4 O 0.8390(3) 0.2423(2) 0.2717(2) 0.0515(10) Uani 1 1 d . . . O5 O 0.7852(3) 0.4119(2) 0.2532(2) 0.0492(9) Uani 1 1 d . . . O6 O 0.7011(3) 0.2504(2) 0.1384(2) 0.0490(9) Uani 1 1 d . . . O7 O 0.5438(3) 0.3702(2) 0.2677(2) 0.0487(10) Uani 1 1 d . . . O8 O 0.6041(4) 0.6852(3) 0.2324(2) 0.0878(14) Uani 1 1 d . . . O9 O 0.6122(3) 0.0952(2) 0.2630(2) 0.0463(9) Uani 1 1 d . . . O10 O 0.8746(4) -0.0810(3) 0.2777(3) 0.1010(16) Uani 1 1 d . . . O11 O 0.7479(3) 0.4562(3) -0.1917(2) 0.0731(12) Uani 1 1 d . . . O12 O 0.7793(4) 0.1529(3) 0.7362(3) 0.0887(14) 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 Ho1 0.03706(13) 0.04027(13) 0.04172(17) 0.00551(11) 0.00534(11) 0.01502(10) C1 0.064(2) 0.063(4) 0.069(5) 0.012(4) 0.009(4) 0.028(2) C2 0.045(3) 0.034(3) 0.042(4) 0.005(3) 0.011(3) 0.016(3) C3 0.037(3) 0.068(4) 0.062(5) 0.005(4) 0.000(3) 0.008(3) C4 0.050(3) 0.057(3) 0.055(4) 0.017(2) 0.006(3) 0.024(3) C5 0.078(5) 0.133(5) 0.081(5) 0.011(4) -0.021(4) 0.026(5) C6 0.069(4) 0.076(5) 0.055(5) -0.003(4) -0.003(4) 0.021(4) C7 0.057(4) 0.036(3) 0.051(5) 0.007(3) -0.003(3) 0.005(3) C8 0.036(3) 0.063(4) 0.066(5) 0.003(4) 0.000(3) 0.011(3) C9 0.041(3) 0.048(3) 0.061(5) 0.013(3) 0.005(3) 0.019(3) C10 0.042(4) 0.080(5) 0.122(8) 0.015(5) 0.005(4) 0.022(4) C11 0.054(4) 0.060(4) 0.133(8) 0.014(5) 0.020(5) 0.007(4) C12 0.047(3) 0.039(3) 0.066(5) 0.004(3) 0.005(3) 0.015(3) C13 0.058(4) 0.052(4) 0.065(5) 0.015(4) 0.022(4) 0.014(3) C14 0.059(4) 0.056(4) 0.047(5) 0.016(3) 0.006(3) 0.030(3) C15 0.098(5) 0.068(4) 0.049(5) 0.005(4) 0.026(4) 0.025(4) C16 0.131(6) 0.103(5) 0.062(5) 0.000(4) -0.019(5) 0.041(5) C17 0.094(5) 0.065(4) 0.053(5) 0.006(4) -0.003(5) 0.040(4) C18 0.079(4) 0.061(4) 0.052(5) 0.005(3) -0.001(4) 0.035(3) C19 0.053(4) 0.046(3) 0.058(5) 0.009(3) 0.011(4) 0.022(3) C20 0.056(4) 0.046(3) 0.048(5) 0.014(3) 0.013(3) 0.028(3) C21 0.071(4) 0.075(4) 0.069(6) 0.006(4) -0.003(4) 0.034(4) C22 0.076(5) 0.095(5) 0.061(5) 0.004(4) 0.019(4) 0.046(4) C23 0.055(4) 0.068(4) 0.076(6) 0.013(4) -0.006(4) 0.029(3) C24 0.057(4) 0.068(4) 0.075(5) 0.020(4) 0.011(4) 0.031(3) C25 0.059(4) 0.046(3) 0.055(5) 0.014(3) 0.004(4) 0.027(3) C26 0.051(3) 0.054(3) 0.054(5) 0.018(3) 0.004(3) 0.024(3) C27 0.055(3) 0.043(3) 0.057(5) 0.014(3) 0.010(3) 0.024(3) C28 0.123(5) 0.055(4) 0.077(5) 0.005(4) 0.036(4) 0.041(4) C29 0.078(4) 0.047(3) 0.057(5) 0.012(3) 0.021(4) 0.030(3) C30 0.077(4) 0.072(4) 0.073(5) 0.017(4) 0.027(4) 0.021(3) C31 0.071(4) 0.058(4) 0.083(5) -0.001(4) 0.013(4) 0.010(3) C32 0.070(4) 0.034(3) 0.053(4) -0.002(3) 0.009(3) 0.017(3) C33 0.092(4) 0.063(4) 0.055(5) 0.004(3) 0.006(4) 0.034(4) C34 0.075(4) 0.100(5) 0.050(5) -0.010(4) 0.005(4) 0.023(4) C35 0.074(4) 0.066(4) 0.051(5) 0.014(4) 0.014(4) 0.036(4) C36 0.089(5) 0.067(4) 0.055(5) 0.025(4) 0.037(4) 0.026(4) C37 0.084(4) 0.040(3) 0.083(6) 0.015(4) 0.033(4) 0.011(3) C38 0.060(4) 0.043(3) 0.054(4) 0.014(3) 0.018(3) 0.023(3) C39 0.056(3) 0.051(3) 0.039(4) 0.016(3) 0.008(3) 0.022(3) C40 0.063(4) 0.053(4) 0.046(5) 0.005(3) 0.007(3) 0.020(3) C41 0.059(4) 0.048(3) 0.043(4) 0.010(3) 0.002(3) 0.010(3) C42 0.046(3) 0.049(3) 0.051(4) 0.021(3) 0.015(3) 0.012(3) C43 0.060(3) 0.040(3) 0.033(4) 0.008(3) 0.015(3) 0.023(3) C44 0.067(4) 0.034(3) 0.059(5) 0.009(3) 0.021(3) 0.018(3) C45 0.063(4) 0.044(3) 0.051(5) 0.009(3) 0.013(3) 0.028(3) C46 0.117(5) 0.099(5) 0.038(4) 0.014(4) 0.021(4) 0.066(4) C47 0.078(4) 0.066(4) 0.051(5) 0.018(3) 0.013(4) 0.041(4) C48 0.069(4) 0.077(4) 0.067(5) 0.015(4) 0.018(4) 0.036(3) C49 0.082(5) 0.089(5) 0.094(6) -0.018(4) 0.006(4) 0.022(4) C50 0.075(4) 0.059(4) 0.052(5) 0.001(3) 0.015(4) 0.031(3) C51 0.113(5) 0.082(4) 0.072(5) -0.009(4) 0.014(4) 0.061(4) F1 0.102(3) 0.087(2) 0.065(3) 0.002(2) 0.036(2) 0.041(2) F2 0.0699(12) 0.0807(13) 0.0741(13) 0.0127(9) 0.0122(9) 0.0188(9) F3 0.080(2) 0.127(3) 0.080(3) 0.061(3) 0.025(2) 0.048(2) F4 0.093(3) 0.157(4) 0.063(3) -0.006(3) -0.016(2) 0.017(3) F5 0.093(3) 0.151(4) 0.066(3) -0.023(3) -0.013(2) 0.016(3) F6 0.079(3) 0.157(4) 0.068(3) -0.014(3) -0.015(2) 0.017(3) F4' 0.093(3) 0.155(4) 0.064(3) -0.017(3) -0.012(2) 0.017(3) F5' 0.085(3) 0.153(4) 0.068(3) -0.017(3) -0.015(2) 0.013(3) F6' 0.088(3) 0.156(4) 0.066(3) -0.008(3) -0.019(2) 0.021(3) F7 0.160(4) 0.062(2) 0.093(3) -0.026(2) -0.017(3) 0.024(2) F8 0.146(4) 0.193(4) 0.067(3) -0.020(3) -0.043(3) 0.093(3) F9 0.126(3) 0.130(3) 0.065(3) -0.013(3) 0.031(3) 0.003(3) F10 0.046(2) 0.210(5) 0.176(5) -0.041(4) -0.007(3) 0.043(3) F11 0.082(3) 0.130(3) 0.162(5) -0.014(3) 0.031(3) 0.058(3) F12 0.126(4) 0.329(7) 0.251(7) 0.234(6) 0.137(4) 0.140(4) F13 0.104(3) 0.130(4) 0.104(4) 0.021(3) -0.034(3) -0.041(3) F14 0.095(3) 0.063(2) 0.120(4) 0.011(2) 0.037(3) -0.011(2) F15 0.1114(15) 0.1074(15) 0.1163(16) 0.0115(10) 0.0198(10) 0.0320(10) F16 0.205(4) 0.127(3) 0.092(4) 0.025(3) 0.055(3) 0.121(3) F17 0.157(4) 0.090(3) 0.076(3) 0.028(2) 0.059(3) 0.035(3) F18 0.123(3) 0.141(4) 0.066(3) -0.024(3) 0.013(3) 0.007(3) N1 0.058(3) 0.049(3) 0.046(3) 0.004(3) 0.014(3) 0.029(2) N2 0.080(3) 0.048(3) 0.054(4) 0.014(3) 0.019(3) 0.030(3) N3 0.050(3) 0.038(2) 0.051(3) 0.009(2) 0.009(2) 0.017(2) N4 0.075(3) 0.064(3) 0.059(4) 0.010(3) 0.011(3) 0.049(3) O1 0.0385(19) 0.0428(19) 0.046(3) 0.0053(18) 0.0064(18) 0.0096(16) O2 0.043(2) 0.052(2) 0.045(3) 0.0094(19) 0.0102(19) 0.0179(18) O3 0.045(2) 0.059(2) 0.050(3) 0.004(2) -0.0015(19) 0.0162(19) O4 0.039(2) 0.058(2) 0.059(3) 0.008(2) 0.004(2) 0.0198(18) O5 0.049(2) 0.046(2) 0.049(3) 0.005(2) 0.017(2) 0.0100(18) O6 0.053(2) 0.048(2) 0.042(3) 0.0089(19) 0.0077(19) 0.0095(18) O7 0.059(2) 0.042(2) 0.057(3) 0.0161(19) 0.020(2) 0.0280(18) O8 0.133(4) 0.056(3) 0.089(4) 0.021(3) 0.046(3) 0.040(3) O9 0.050(2) 0.0391(18) 0.057(3) 0.0060(18) 0.0101(19) 0.0233(17) O10 0.128(4) 0.123(4) 0.093(4) 0.018(3) 0.016(3) 0.097(3) O11 0.105(3) 0.082(3) 0.041(3) 0.010(3) 0.026(3) 0.039(3) O12 0.116(4) 0.105(3) 0.056(4) -0.003(3) 0.000(3) 0.061(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 Ho1 O7 2.308(3) . ? Ho1 O9 2.319(3) . ? Ho1 O3 2.327(4) . ? Ho1 O6 2.341(4) . ? Ho1 O2 2.361(3) . ? Ho1 O5 2.372(3) . ? Ho1 O4 2.372(3) . ? Ho1 O1 2.385(3) . ? C1 F3 1.324(6) . ? C1 F1 1.327(6) . ? C1 F2 1.357(6) . ? C1 C2 1.524(7) . ? C2 O1 1.253(5) . ? C2 C3 1.392(7) . ? C3 C4 1.382(7) . ? C3 H3 0.9300 . ? C4 O2 1.245(5) . ? C4 C5 1.542(8) . ? C5 F6 1.316(11) . ? C5 F4' 1.325(9) . ? C5 F4 1.343(11) . ? C5 F5' 1.344(9) . ? C5 F5 1.355(10) . ? C5 F6' 1.376(8) . ? C6 F8 1.307(6) . ? C6 F7 1.316(6) . ? C6 F9 1.326(7) . ? C6 C7 1.519(8) . ? C7 O3 1.253(5) . ? C7 C8 1.410(7) . ? C8 C9 1.376(7) . ? C8 H8 0.9300 . ? C9 O4 1.250(6) . ? C9 C10 1.541(8) . ? C10 F12 1.242(8) . ? C10 F11 1.302(7) . ? C10 F10 1.313(7) . ? C11 F13 1.259(7) . ? C11 F15 1.325(7) . ? C11 F14 1.362(8) . ? C11 C12 1.535(7) . ? C12 O5 1.252(6) . ? C12 C13 1.375(7) . ? C13 C14 1.390(7) . ? C13 H13 0.9300 . ? C14 O6 1.252(5) . ? C14 C15 1.548(8) . ? C15 F16 1.299(6) . ? C15 F17 1.310(6) . ? C15 F18 1.318(7) . ? C16 O12 1.412(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.360(7) . ? C17 O12 1.381(7) . ? C17 C22 1.428(7) . ? C18 C19 1.416(7) . ? C18 H18 0.9300 . ? C19 C23 1.421(7) . ? C19 C20 1.422(6) . ? C20 C26 1.407(7) . ? C20 C21 1.420(7) . ? C21 C22 1.350(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.355(7) . ? C23 H23 0.9300 . ? C24 C25 1.428(6) . ? C24 H24 0.9300 . ? C25 C26 1.389(7) . ? C25 C27 1.447(7) . ? C26 H26 0.9300 . ? C27 N3 1.346(6) . ? C27 N4 1.387(6) . ? C28 C29 1.517(6) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N4 1.503(7) . ? C29 C30 1.525(6) . ? C29 C32 1.548(7) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.532(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N3 1.504(6) . ? C32 C33 1.523(6) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 O11 1.415(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C40 1.367(7) . ? C35 O11 1.376(7) . ? C35 C36 1.405(7) . ? C36 C37 1.342(7) . ? C36 H36 0.9300 . ? C37 C38 1.450(7) . ? C37 H37 0.9300 . ? C38 C44 1.385(7) . ? C38 C39 1.424(7) . ? C39 C40 1.414(7) . ? C39 C41 1.417(6) . ? C40 H40 0.9300 . ? C41 C42 1.364(7) . ? C41 H41 0.9300 . ? C42 C43 1.412(6) . ? C42 H42 0.9300 . ? C43 C44 1.389(6) . ? C43 C45 1.441(7) . ? C44 H44 0.9300 . ? C45 N1 1.343(6) . ? C45 N2 1.362(6) . ? C46 C47 1.529(6) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 N1 1.494(6) . ? C47 C50 1.538(7) . ? C47 C48 1.554(6) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.555(7) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 N2 1.506(7) . ? C50 C51 1.530(7) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? N1 O7 1.296(4) . ? N2 O8 1.260(5) . ? N3 O9 1.314(4) . ? N4 O10 1.281(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Ho1 O9 140.19(10) . . ? O7 Ho1 O3 92.03(12) . . ? O9 Ho1 O3 97.04(12) . . ? O7 Ho1 O6 103.80(11) . . ? O9 Ho1 O6 92.85(12) . . ? O3 Ho1 O6 141.40(11) . . ? O7 Ho1 O2 73.61(11) . . ? O9 Ho1 O2 76.95(11) . . ? O3 Ho1 O2 144.89(11) . . ? O6 Ho1 O2 73.71(11) . . ? O7 Ho1 O5 72.55(11) . . ? O9 Ho1 O5 147.25(10) . . ? O3 Ho1 O5 78.96(12) . . ? O6 Ho1 O5 72.87(12) . . ? O2 Ho1 O5 124.07(11) . . ? O7 Ho1 O4 144.03(11) . . ? O9 Ho1 O4 75.14(11) . . ? O3 Ho1 O4 72.65(12) . . ? O6 Ho1 O4 74.08(12) . . ? O2 Ho1 O4 135.71(12) . . ? O5 Ho1 O4 72.64(11) . . ? O7 Ho1 O1 74.10(10) . . ? O9 Ho1 O1 72.09(11) . . ? O3 Ho1 O1 72.16(11) . . ? O6 Ho1 O1 145.87(11) . . ? O2 Ho1 O1 73.11(11) . . ? O5 Ho1 O1 134.47(11) . . ? O4 Ho1 O1 127.62(11) . . ? F3 C1 F1 106.1(5) . . ? F3 C1 F2 106.1(5) . . ? F1 C1 F2 105.2(5) . . ? F3 C1 C2 113.5(5) . . ? F1 C1 C2 111.5(5) . . ? F2 C1 C2 113.8(5) . . ? O1 C2 C3 127.5(5) . . ? O1 C2 C1 112.9(5) . . ? C3 C2 C1 119.6(5) . . ? C4 C3 C2 121.5(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? O2 C4 C3 129.7(5) . . ? O2 C4 C5 113.7(6) . . ? C3 C4 C5 116.7(5) . . ? F6 C5 F4' 127.4(9) . . ? F6 C5 F4 107.3(8) . . ? F4' C5 F4 57.3(7) . . ? F6 C5 F5' 36.4(6) . . ? F4' C5 F5' 109.7(10) . . ? F4 C5 F5' 128.8(9) . . ? F6 C5 F5 106.2(8) . . ? F4' C5 F5 48.6(7) . . ? F4 C5 F5 104.7(9) . . ? F5' C5 F5 72.2(7) . . ? F6 C5 F6' 69.1(6) . . ? F4' C5 F6' 101.4(9) . . ? F4 C5 F6' 46.4(6) . . ? F5' C5 F6' 103.5(9) . . ? F5 C5 F6' 140.4(9) . . ? F6 C5 C4 116.0(8) . . ? F4' C5 C4 116.1(7) . . ? F4 C5 C4 112.4(7) . . ? F5' C5 C4 116.7(8) . . ? F5 C5 C4 109.4(6) . . ? F6' C5 C4 107.5(7) . . ? F8 C6 F7 105.8(5) . . ? F8 C6 F9 106.9(6) . . ? F7 C6 F9 104.2(6) . . ? F8 C6 C7 115.5(5) . . ? F7 C6 C7 111.3(5) . . ? F9 C6 C7 112.4(5) . . ? O3 C7 C8 126.6(6) . . ? O3 C7 C6 115.4(5) . . ? C8 C7 C6 118.0(5) . . ? C9 C8 C7 121.2(5) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? O4 C9 C8 128.4(5) . . ? O4 C9 C10 113.4(6) . . ? C8 C9 C10 118.2(5) . . ? F12 C10 F11 108.2(8) . . ? F12 C10 F10 108.8(6) . . ? F11 C10 F10 101.9(6) . . ? F12 C10 C9 113.4(6) . . ? F11 C10 C9 110.5(5) . . ? F10 C10 C9 113.3(7) . . ? F13 C11 F15 110.5(8) . . ? F13 C11 F14 107.6(5) . . ? F15 C11 F14 101.8(5) . . ? F13 C11 C12 114.1(6) . . ? F15 C11 C12 109.2(5) . . ? F14 C11 C12 112.9(7) . . ? O5 C12 C13 128.9(5) . . ? O5 C12 C11 113.0(6) . . ? C13 C12 C11 118.0(6) . . ? C12 C13 C14 122.0(5) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? O6 C14 C13 126.6(6) . . ? O6 C14 C15 115.8(5) . . ? C13 C14 C15 117.6(6) . . ? F16 C15 F17 107.6(6) . . ? F16 C15 F18 106.9(6) . . ? F17 C15 F18 106.2(6) . . ? F16 C15 C14 109.7(5) . . ? F17 C15 C14 115.1(5) . . ? F18 C15 C14 110.9(5) . . ? O12 C16 H16A 109.5 . . ? O12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 O12 126.1(6) . . ? C18 C17 C22 119.8(6) . . ? O12 C17 C22 114.1(6) . . ? C17 C18 C19 119.4(6) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C23 122.0(6) . . ? C18 C19 C20 120.8(6) . . ? C23 C19 C20 117.1(6) . . ? C26 C20 C21 121.9(5) . . ? C26 C20 C19 119.9(5) . . ? C21 C20 C19 118.2(6) . . ? C22 C21 C20 119.8(6) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C17 121.9(6) . . ? C21 C22 H22 119.0 . . ? C17 C22 H22 119.0 . . ? C24 C23 C19 122.5(6) . . ? C24 C23 H23 118.7 . . ? C19 C23 H23 118.7 . . ? C23 C24 C25 120.6(6) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 118.0(6) . . ? C26 C25 C27 120.7(5) . . ? C24 C25 C27 121.2(6) . . ? C25 C26 C20 121.8(5) . . ? C25 C26 H26 119.1 . . ? C20 C26 H26 119.1 . . ? N3 C27 N4 105.0(5) . . ? N3 C27 C25 129.4(5) . . ? N4 C27 C25 125.4(5) . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 C28 109.6(4) . . ? N4 C29 C30 107.1(5) . . ? C28 C29 C30 110.3(5) . . ? N4 C29 C32 99.9(5) . . ? C28 C29 C32 114.7(5) . . ? C30 C29 C32 114.3(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C33 111.7(4) . . ? N3 C32 C31 104.8(4) . . ? C33 C32 C31 110.8(4) . . ? N3 C32 C29 98.5(4) . . ? C33 C32 C29 115.3(5) . . ? C31 C32 C29 114.6(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O11 C34 H34A 109.5 . . ? O11 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O11 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 O11 125.4(6) . . ? C40 C35 C36 119.4(6) . . ? O11 C35 C36 115.2(6) . . ? C37 C36 C35 121.4(6) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C36 C37 C38 121.8(6) . . ? C36 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C44 C38 C39 119.5(5) . . ? C44 C38 C37 124.5(5) . . ? C39 C38 C37 116.0(6) . . ? C40 C39 C41 122.8(5) . . ? C40 C39 C38 120.4(5) . . ? C41 C39 C38 116.9(5) . . ? C35 C40 C39 121.0(6) . . ? C35 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C42 C41 C39 122.7(5) . . ? C42 C41 H41 118.7 . . ? C39 C41 H41 118.7 . . ? C41 C42 C43 120.1(5) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 117.9(5) . . ? C44 C43 C45 121.9(5) . . ? C42 C43 C45 120.2(5) . . ? C38 C44 C43 122.7(5) . . ? C38 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? N1 C45 N2 106.3(5) . . ? N1 C45 C43 127.1(5) . . ? N2 C45 C43 126.6(5) . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N1 C47 C46 110.2(4) . . ? N1 C47 C50 100.6(4) . . ? C46 C47 C50 114.4(5) . . ? N1 C47 C48 105.5(5) . . ? C46 C47 C48 110.8(5) . . ? C50 C47 C48 114.3(4) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N2 C50 C51 110.7(5) . . ? N2 C50 C47 100.1(5) . . ? C51 C50 C47 115.1(5) . . ? N2 C50 C49 106.2(5) . . ? C51 C50 C49 109.5(5) . . ? C47 C50 C49 114.5(5) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O7 N1 C45 126.1(5) . . ? O7 N1 C47 119.3(4) . . ? C45 N1 C47 113.6(4) . . ? O8 N2 C45 124.5(5) . . ? O8 N2 C50 122.7(4) . . ? C45 N2 C50 112.7(4) . . ? O9 N3 C27 124.4(5) . . ? O9 N3 C32 120.8(4) . . ? C27 N3 C32 113.8(4) . . ? O10 N4 C27 124.2(5) . . ? O10 N4 C29 123.4(5) . . ? C27 N4 C29 112.0(4) . . ? C2 O1 Ho1 134.2(3) . . ? C4 O2 Ho1 133.7(4) . . ? C7 O3 Ho1 135.9(4) . . ? C9 O4 Ho1 132.9(4) . . ? C12 O5 Ho1 133.0(4) . . ? C14 O6 Ho1 135.6(4) . . ? N1 O7 Ho1 141.1(3) . . ? N3 O9 Ho1 134.3(2) . . ? C35 O11 C34 116.3(5) . . ? C17 O12 C16 117.5(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.018 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.074 # Attachment '- complex-6.cif' data_shelxlf _database_code_depnum_ccdc_archive 'CCDC 782331' #TrackingRef '- complex-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H45 Er F18 N4 O12' _chemical_formula_weight 1415.17 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' Er Er -0.2586 4.9576 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.778(2) _cell_length_b 14.717(3) _cell_length_c 17.644(3) _cell_angle_alpha 97.39(3) _cell_angle_beta 93.68(3) _cell_angle_gamma 107.89(3) _cell_volume 2868.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17103 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.72 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1410 _exptl_absorpt_coefficient_mu 1.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16506 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9992 _reflns_number_gt 8124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Fluorine atoms in the CF3 groups were treated by disorder and these atoms were refined anisotropically with application of restraints on interatomic distances and thermal parameters (DFIX, ISOR and SIMU instructions in SHELXL). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^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 9992 _refine_ls_number_parameters 841 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1601 _refine_ls_wR_factor_gt 0.1453 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.003 _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 Er1 Er 0.85416(3) 0.74258(2) 0.737819(17) 0.03498(13) Uani 1 1 d . A . C1 C 0.6134(12) 0.8431(9) 0.2236(6) 0.099(4) Uani 1 1 d . . . H1A H 0.6029 0.9056 0.2332 0.148 Uiso 1 1 calc R . . H1B H 0.5486 0.7963 0.2415 0.148 Uiso 1 1 calc R . . H1C H 0.6141 0.8252 0.1694 0.148 Uiso 1 1 calc R . . C2 C 0.7289(10) 0.8627(6) 0.3392(5) 0.066(2) Uani 1 1 d . . . C3 C 0.6418(9) 0.8748(6) 0.3836(5) 0.065(2) Uani 1 1 d . . . H3 H 0.5675 0.8708 0.3596 0.078 Uiso 1 1 calc R . . C4 C 0.6613(8) 0.8927(5) 0.4633(4) 0.0498(19) Uani 1 1 d . . . C5 C 0.5741(8) 0.9084(6) 0.5091(5) 0.059(2) Uani 1 1 d . . . H5 H 0.4976 0.9008 0.4863 0.071 Uiso 1 1 calc R . . C6 C 0.6004(8) 0.9348(6) 0.5865(5) 0.060(2) Uani 1 1 d . . . H6 H 0.5419 0.9464 0.6157 0.072 Uiso 1 1 calc R . . C7 C 0.7157(7) 0.9452(5) 0.6241(4) 0.0462(19) Uani 1 1 d . . . C8 C 0.8015(7) 0.9281(5) 0.5808(4) 0.0477(19) Uani 1 1 d . . . H8 H 0.8765 0.9332 0.6045 0.057 Uiso 1 1 calc R . . C9 C 0.7758(8) 0.9024(5) 0.4994(5) 0.050(2) Uani 1 1 d . . . C10 C 0.8650(8) 0.8880(6) 0.4524(5) 0.061(2) Uani 1 1 d . . . H10 H 0.9394 0.8905 0.4755 0.073 Uiso 1 1 calc R . . C11 C 0.8439(10) 0.8715(7) 0.3782(5) 0.074(3) Uani 1 1 d . . . H11 H 0.9049 0.8651 0.3491 0.089 Uiso 1 1 calc R . . C12 C 0.7429(7) 0.9797(5) 0.7040(5) 0.0477(19) Uani 1 1 d . . . C13 C 0.7394(8) 1.0573(5) 0.8313(4) 0.050(2) Uani 1 1 d . . . C14 C 0.7497(9) 1.1598(6) 0.8675(5) 0.066(3) Uani 1 1 d . . . H14A H 0.6722 1.1685 0.8623 0.100 Uiso 1 1 calc R . . H14B H 0.8045 1.2054 0.8418 0.100 Uiso 1 1 calc R . . H14C H 0.7788 1.1700 0.9210 0.100 Uiso 1 1 calc R . . C15 C 0.6447(8) 0.9840(6) 0.8661(5) 0.064(2) Uani 1 1 d . . . H15A H 0.6418 0.9199 0.8447 0.096 Uiso 1 1 calc R . . H15B H 0.5678 0.9920 0.8549 0.096 Uiso 1 1 calc R . . H15C H 0.6646 0.9938 0.9208 0.096 Uiso 1 1 calc R . . C16 C 0.8573(7) 1.0342(5) 0.8265(4) 0.0430(18) Uani 1 1 d . . . C17 C 0.8930(9) 0.9875(6) 0.8922(5) 0.063(2) Uani 1 1 d . . . H17A H 0.9610 0.9674 0.8807 0.094 Uiso 1 1 calc R . . H17B H 0.8271 0.9324 0.8985 0.094 Uiso 1 1 calc R . . H17C H 0.9135 1.0334 0.9387 0.094 Uiso 1 1 calc R . . C18 C 0.9632(8) 1.1188(6) 0.8121(5) 0.061(2) Uani 1 1 d . . . H18A H 0.9367 1.1524 0.7750 0.092 Uiso 1 1 calc R . . H18B H 1.0247 1.0948 0.7929 0.092 Uiso 1 1 calc R . . H18C H 0.9948 1.1623 0.8594 0.092 Uiso 1 1 calc R . . C19 C 0.4549(8) 0.7315(8) 0.7070(5) 0.072(3) Uani 1 1 d DU . . C20 C 0.5731(7) 0.7233(5) 0.6782(5) 0.0465(19) Uani 1 1 d . A . C21 C 0.5694(7) 0.6809(6) 0.6059(5) 0.056(2) Uani 1 1 d . . . H21 H 0.4970 0.6594 0.5744 0.067 Uiso 1 1 calc R A . C22 C 0.6705(7) 0.6684(5) 0.5771(4) 0.0458(18) Uani 1 1 d . A . C23 C 0.6603(9) 0.6221(7) 0.4915(5) 0.065(2) Uani 1 1 d . . . C24 C 1.1798(7) 0.8412(6) 0.5969(4) 0.0480(19) Uani 1 1 d . . . C25 C 1.1173(7) 0.8331(5) 0.6715(4) 0.0397(17) Uani 1 1 d . A . C26 C 1.1387(7) 0.8527(5) 0.8095(4) 0.0457(18) Uani 1 1 d . A . C27 C 1.2242(9) 0.8866(8) 0.8837(6) 0.075(3) Uani 1 1 d DU . . C28 C 1.1889(6) 0.8643(5) 0.7419(4) 0.0480(19) Uani 1 1 d . . . H28 H 1.2713 0.8932 0.7431 0.058 Uiso 1 1 calc R B . C29 C 0.7230(7) 0.6986(5) 0.8942(4) 0.0462(19) Uani 1 1 d . A . C30 C 0.7112(10) 0.7487(6) 0.9776(6) 0.068(3) Uani 1 1 d . . . C31 C 0.6455(7) 0.6067(5) 0.8687(4) 0.050(2) Uani 1 1 d . . . H31 H 0.5891 0.5765 0.8996 0.060 Uiso 1 1 calc R . . C32 C 0.6517(7) 0.5606(5) 0.7984(5) 0.053(2) Uani 1 1 d . A . C33 C 0.5593(10) 0.4589(6) 0.7702(7) 0.077(3) Uani 1 1 d . . . C34 C 0.7842(9) 0.6449(7) 1.2238(5) 0.076(3) Uani 1 1 d . . . H34A H 0.7545 0.6790 1.1885 0.113 Uiso 1 1 calc R . . H34B H 0.8700 0.6714 1.2330 0.113 Uiso 1 1 calc R . . H34C H 0.7502 0.6514 1.2714 0.113 Uiso 1 1 calc R . . C35 C 0.7763(8) 0.5232(6) 1.1176(4) 0.055(2) Uani 1 1 d . . . C36 C 0.7143(9) 0.4305(6) 1.0807(5) 0.067(3) Uani 1 1 d . . . H36 H 0.6603 0.3878 1.1061 0.080 Uiso 1 1 calc R . . C37 C 0.7320(8) 0.4023(6) 1.0084(5) 0.065(3) Uani 1 1 d . . . H37 H 0.6901 0.3397 0.9843 0.078 Uiso 1 1 calc R . . C38 C 0.8142(7) 0.4665(5) 0.9673(4) 0.0475(19) Uani 1 1 d . . . C39 C 0.8780(7) 0.5594(5) 1.0074(4) 0.0429(18) Uani 1 1 d . . . C40 C 0.8572(8) 0.5849(6) 1.0812(4) 0.053(2) Uani 1 1 d . . . H40 H 0.8997 0.6464 1.1073 0.064 Uiso 1 1 calc R . . C41 C 0.9601(7) 0.6235(5) 0.9678(4) 0.0476(19) Uani 1 1 d . . . H41 H 1.0061 0.6842 0.9937 0.057 Uiso 1 1 calc R . . C42 C 0.9732(7) 0.5978(5) 0.8919(4) 0.0478(19) Uani 1 1 d . . . H42 H 1.0259 0.6418 0.8667 0.057 Uiso 1 1 calc R . . C43 C 0.9073(7) 0.5051(5) 0.8520(4) 0.0392(17) Uani 1 1 d . . . C44 C 0.8286(7) 0.4403(5) 0.8890(4) 0.0473(19) Uani 1 1 d . . . H44 H 0.7848 0.3792 0.8627 0.057 Uiso 1 1 calc R . . C45 C 0.9208(7) 0.4817(5) 0.7734(4) 0.0430(18) Uani 1 1 d . . . C46 C 0.9051(8) 0.3860(6) 0.6493(5) 0.056(2) Uani 1 1 d . . . C47 C 0.7768(10) 0.3458(8) 0.6210(6) 0.090(3) Uani 1 1 d . . . H47A H 0.7364 0.3905 0.6394 0.136 Uiso 1 1 calc R . . H47B H 0.7428 0.2856 0.6393 0.136 Uiso 1 1 calc R . . H47C H 0.7674 0.3351 0.5658 0.136 Uiso 1 1 calc R . . C48 C 0.9759(10) 0.3220(7) 0.6180(5) 0.072(3) Uani 1 1 d . . . H48A H 0.9760 0.3209 0.5635 0.109 Uiso 1 1 calc R . . H48B H 0.9396 0.2576 0.6285 0.109 Uiso 1 1 calc R . . H48C H 1.0570 0.3470 0.6423 0.109 Uiso 1 1 calc R . . C49 C 1.1010(8) 0.5268(6) 0.6478(5) 0.064(2) Uani 1 1 d . . . H49A H 1.1337 0.5083 0.6923 0.096 Uiso 1 1 calc R . . H49B H 1.1316 0.5958 0.6506 0.096 Uiso 1 1 calc R . . H49C H 1.1236 0.4964 0.6023 0.096 Uiso 1 1 calc R . . C50 C 0.9654(8) 0.4952(6) 0.6445(4) 0.052(2) Uani 1 1 d . . . C51 C 0.9107(9) 0.5306(7) 0.5813(4) 0.072(3) Uani 1 1 d . . . H51A H 0.9533 0.5978 0.5819 0.108 Uiso 1 1 calc R . . H51B H 0.8282 0.5227 0.5881 0.108 Uiso 1 1 calc R . . H51C H 0.9152 0.4943 0.5330 0.108 Uiso 1 1 calc R . . F1 F 0.4060(16) 0.6594(18) 0.7409(14) 0.094(6) Uani 0.41(2) 1 d PU A 1 F2 F 0.470(3) 0.816(2) 0.7420(18) 0.092(7) Uani 0.41(2) 1 d PU A 1 F3 F 0.362(2) 0.679(2) 0.679(2) 0.117(7) Uani 0.41(2) 1 d PU A 1 F1' F 0.455(3) 0.8235(12) 0.7150(13) 0.087(5) Uani 0.59(2) 1 d PDU A 2 F2' F 0.3689(13) 0.7124(14) 0.6472(8) 0.089(4) Uani 0.59(2) 1 d PDU A 2 F3' F 0.4463(13) 0.7163(15) 0.7801(7) 0.098(5) Uani 0.59(2) 1 d PDU A 2 F4 F 0.5707(7) 0.6299(6) 0.4514(3) 0.126(3) Uani 1 1 d . A . F5 F 0.7569(6) 0.6586(5) 0.4606(3) 0.110(2) Uani 1 1 d . A . F6 F 0.6451(6) 0.5294(4) 0.4880(3) 0.103(2) Uani 1 1 d . A . F7 F 1.1294(5) 0.8793(4) 0.5487(3) 0.0830(17) Uani 1 1 d . . . F8 F 1.2957(4) 0.8927(4) 0.6094(3) 0.0780(16) Uani 1 1 d . . . F9 F 1.1765(5) 0.7542(4) 0.5648(3) 0.0800(16) Uani 1 1 d . . . F10 F 1.2421(18) 0.8112(14) 0.9111(10) 0.132(6) Uani 0.537(10) 1 d PU B 1 F11 F 1.1850(15) 0.8469(19) 0.9414(8) 0.123(6) Uani 0.537(10) 1 d PU B 1 F12 F 1.3294(14) 0.9475(12) 0.8789(11) 0.100(5) Uani 0.537(10) 1 d PU B 1 F10' F 1.3369(13) 0.8905(18) 0.8778(14) 0.112(6) Uani 0.463(10) 1 d PDU B 2 F11' F 1.1855(16) 0.9395(18) 0.9371(9) 0.110(6) Uani 0.463(10) 1 d PDU B 2 F12' F 1.2294(19) 0.9774(10) 0.9125(11) 0.123(7) Uani 0.463(10) 1 d PDU B 2 F13 F 0.6154(6) 0.3973(4) 0.7430(5) 0.132(3) Uani 1 1 d . . . F14 F 0.5035(5) 0.4220(4) 0.8279(4) 0.095(2) Uani 1 1 d . . . F15 F 0.4816(6) 0.4589(5) 0.7164(4) 0.120(3) Uani 1 1 d . . . F16 F 0.8151(7) 0.7972(5) 1.0157(3) 0.116(3) Uani 1 1 d . . . F17 F 0.6532(7) 0.6864(4) 1.0197(3) 0.104(2) Uani 1 1 d . . . F18 F 0.6504(8) 0.8075(5) 0.9695(4) 0.122(3) Uani 1 1 d . . . N1 N 0.6984(7) 1.0442(5) 0.7473(4) 0.0560(18) Uani 1 1 d . . . N2 N 0.8264(6) 0.9645(4) 0.7540(4) 0.0448(15) Uani 1 1 d . . . N3 N 0.9399(6) 0.5402(4) 0.7212(3) 0.0425(15) Uani 1 1 d . A . N4 N 0.9118(6) 0.3913(4) 0.7369(4) 0.0516(17) Uani 1 1 d . . . O1 O 0.7206(7) 0.8464(6) 0.2618(3) 0.090(2) Uani 1 1 d . . . O2 O 0.6225(7) 1.0797(5) 0.7194(4) 0.081(2) Uani 1 1 d . . . O3 O 0.8870(5) 0.9058(3) 0.7372(3) 0.0454(12) Uani 1 1 d . . . O4 O 0.7737(4) 0.6894(4) 0.6125(3) 0.0471(12) Uani 1 1 d . . . O5 O 0.6610(4) 0.7586(4) 0.7274(3) 0.0472(12) Uani 1 1 d . . . O6 O 0.9585(5) 0.6318(3) 0.7338(3) 0.0484(13) Uani 1 1 d . . . O7 O 0.8997(6) 0.3172(4) 0.7688(3) 0.0694(18) Uani 1 1 d . . . O8 O 0.8002(5) 0.7515(3) 0.8612(3) 0.0453(12) Uani 1 1 d . . . O9 O 0.7166(5) 0.5907(3) 0.7466(3) 0.0498(13) Uani 1 1 d . . . O10 O 0.7511(6) 0.5451(5) 1.1918(3) 0.0762(19) Uani 1 1 d . . . O11 O 1.0077(4) 0.7958(3) 0.6586(3) 0.0403(11) Uani 1 1 d . . . O12 O 1.0322(4) 0.8156(4) 0.8195(3) 0.0456(12) 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 Er1 0.0326(2) 0.03743(19) 0.0395(2) 0.00610(14) 0.00822(14) 0.01696(14) C1 0.138(12) 0.105(9) 0.055(6) 0.005(6) -0.011(7) 0.049(8) C2 0.086(7) 0.061(5) 0.063(6) 0.005(5) 0.008(5) 0.042(5) C3 0.069(6) 0.070(6) 0.071(6) 0.021(5) 0.010(5) 0.041(5) C4 0.059(5) 0.054(5) 0.050(5) 0.010(4) 0.006(4) 0.037(4) C5 0.056(5) 0.070(6) 0.061(5) 0.014(5) 0.009(4) 0.032(5) C6 0.062(6) 0.072(6) 0.068(6) 0.024(5) 0.023(5) 0.043(5) C7 0.049(5) 0.044(4) 0.055(5) 0.012(4) 0.010(4) 0.026(4) C8 0.043(5) 0.056(5) 0.052(5) 0.016(4) 0.010(4) 0.024(4) C9 0.058(5) 0.055(5) 0.058(5) 0.018(4) 0.018(4) 0.040(4) C10 0.061(6) 0.079(6) 0.054(5) 0.001(5) 0.008(4) 0.042(5) C11 0.079(7) 0.098(7) 0.064(6) 0.009(6) 0.017(5) 0.056(6) C12 0.049(5) 0.051(4) 0.059(5) 0.019(4) 0.024(4) 0.031(4) C13 0.068(6) 0.047(4) 0.040(4) 0.006(4) 0.015(4) 0.026(4) C14 0.093(7) 0.049(5) 0.060(5) -0.002(4) 0.018(5) 0.030(5) C15 0.064(6) 0.069(5) 0.064(5) 0.018(5) 0.023(5) 0.021(5) C16 0.059(5) 0.033(4) 0.039(4) 0.001(3) 0.008(4) 0.018(3) C17 0.081(7) 0.057(5) 0.055(5) 0.003(4) 0.008(5) 0.030(5) C18 0.064(6) 0.053(5) 0.059(5) 0.000(4) 0.010(5) 0.010(4) C19 0.049(5) 0.084(6) 0.087(6) 0.006(5) 0.014(5) 0.027(5) C20 0.034(4) 0.045(4) 0.064(5) 0.013(4) 0.003(4) 0.017(4) C21 0.032(4) 0.062(5) 0.070(6) 0.007(5) -0.005(4) 0.014(4) C22 0.052(5) 0.037(4) 0.049(4) 0.001(4) 0.006(4) 0.016(4) C23 0.065(6) 0.069(6) 0.057(5) 0.004(5) -0.006(5) 0.021(5) C24 0.040(5) 0.062(5) 0.049(4) 0.015(4) 0.014(4) 0.023(4) C25 0.037(4) 0.038(4) 0.051(4) 0.009(3) 0.016(4) 0.020(3) C26 0.037(4) 0.057(5) 0.039(4) -0.006(4) -0.003(3) 0.017(4) C27 0.057(6) 0.091(6) 0.070(6) 0.006(6) 0.002(5) 0.016(5) C28 0.024(4) 0.061(5) 0.051(5) -0.003(4) 0.007(3) 0.007(4) C29 0.053(5) 0.056(5) 0.040(4) 0.010(4) 0.014(4) 0.031(4) C30 0.100(8) 0.054(5) 0.067(6) 0.020(5) 0.037(6) 0.041(6) C31 0.055(5) 0.048(4) 0.045(4) 0.008(4) 0.016(4) 0.011(4) C32 0.042(5) 0.044(4) 0.079(6) 0.016(4) 0.018(4) 0.019(4) C33 0.070(7) 0.048(5) 0.101(8) 0.001(6) 0.040(7) -0.002(5) C34 0.076(7) 0.096(7) 0.048(5) -0.008(5) 0.010(5) 0.024(6) C35 0.072(6) 0.064(5) 0.044(4) 0.018(4) 0.022(4) 0.035(5) C36 0.082(7) 0.070(6) 0.069(6) 0.036(5) 0.044(5) 0.037(5) C37 0.077(7) 0.049(5) 0.071(6) 0.015(4) 0.035(5) 0.017(4) C38 0.056(5) 0.046(4) 0.058(5) 0.022(4) 0.025(4) 0.032(4) C39 0.050(5) 0.049(4) 0.037(4) 0.016(4) 0.008(3) 0.021(4) C40 0.068(6) 0.051(5) 0.044(4) 0.010(4) 0.008(4) 0.023(4) C41 0.046(5) 0.044(4) 0.050(5) 0.008(4) 0.000(4) 0.010(4) C42 0.049(5) 0.046(4) 0.055(5) 0.018(4) 0.016(4) 0.017(4) C43 0.047(4) 0.035(4) 0.046(4) 0.014(3) 0.015(4) 0.023(3) C44 0.067(5) 0.039(4) 0.044(4) 0.007(4) 0.015(4) 0.027(4) C45 0.047(5) 0.041(4) 0.048(4) 0.009(4) 0.015(4) 0.023(3) C46 0.067(6) 0.064(5) 0.049(5) 0.000(4) 0.016(4) 0.036(5) C47 0.085(8) 0.098(8) 0.076(7) -0.013(6) 0.012(6) 0.022(7) C48 0.099(8) 0.082(6) 0.051(5) -0.002(5) 0.017(5) 0.054(6) C49 0.065(6) 0.081(6) 0.071(6) 0.027(5) 0.043(5) 0.046(5) C50 0.070(6) 0.063(5) 0.040(4) 0.010(4) 0.018(4) 0.043(4) C51 0.089(7) 0.103(7) 0.042(5) 0.006(5) 0.004(5) 0.060(6) F1 0.055(9) 0.143(13) 0.099(13) 0.067(10) 0.025(9) 0.029(9) F2 0.049(9) 0.132(11) 0.094(16) -0.022(10) -0.002(11) 0.045(9) F3 0.040(8) 0.163(15) 0.137(15) 0.013(12) 0.025(11) 0.017(9) F1' 0.079(10) 0.113(8) 0.096(14) 0.019(8) 0.014(10) 0.066(6) F2' 0.036(6) 0.151(12) 0.096(9) 0.029(8) 0.007(6) 0.050(7) F3' 0.061(8) 0.175(13) 0.074(8) 0.051(8) 0.037(6) 0.044(8) F4 0.129(6) 0.195(8) 0.065(4) -0.018(4) -0.038(4) 0.095(6) F5 0.115(5) 0.128(5) 0.056(3) -0.011(4) 0.024(4) -0.001(4) F6 0.137(6) 0.064(4) 0.090(4) -0.025(3) -0.012(4) 0.027(4) F7 0.070(4) 0.132(5) 0.075(3) 0.063(4) 0.026(3) 0.051(3) F8 0.043(3) 0.102(4) 0.089(4) 0.028(3) 0.028(3) 0.013(3) F9 0.100(4) 0.084(4) 0.063(3) -0.004(3) 0.034(3) 0.040(3) F10 0.125(12) 0.155(12) 0.108(11) 0.037(9) -0.055(9) 0.040(9) F11 0.092(10) 0.182(14) 0.061(8) 0.025(10) -0.019(7) -0.002(11) F12 0.051(7) 0.140(12) 0.083(7) 0.017(10) -0.012(6) -0.004(8) F10' 0.047(7) 0.196(16) 0.087(9) -0.005(13) -0.007(6) 0.043(10) F11' 0.073(10) 0.176(14) 0.052(9) -0.042(10) 0.006(7) 0.022(11) F12' 0.104(12) 0.139(12) 0.081(11) -0.025(9) -0.003(9) -0.006(10) F13 0.105(5) 0.049(3) 0.220(8) -0.030(4) 0.076(6) -0.001(3) F14 0.087(4) 0.064(3) 0.120(5) 0.022(3) 0.042(4) -0.006(3) F15 0.092(5) 0.128(6) 0.088(4) 0.004(4) -0.029(4) -0.029(4) F16 0.116(6) 0.140(6) 0.058(3) -0.025(4) 0.003(4) 0.009(5) F17 0.159(6) 0.089(4) 0.067(4) 0.024(3) 0.058(4) 0.031(4) F18 0.202(8) 0.130(5) 0.094(4) 0.037(4) 0.071(5) 0.123(6) N1 0.066(5) 0.052(4) 0.066(4) 0.014(4) 0.023(4) 0.036(4) N2 0.049(4) 0.038(3) 0.058(4) 0.015(3) 0.020(3) 0.023(3) N3 0.050(4) 0.043(3) 0.046(4) 0.013(3) 0.019(3) 0.026(3) N4 0.063(5) 0.045(4) 0.056(4) 0.010(3) 0.026(4) 0.027(3) O1 0.125(7) 0.123(6) 0.039(3) -0.003(4) 0.000(4) 0.073(5) O2 0.103(5) 0.095(5) 0.079(4) 0.008(4) 0.009(4) 0.082(4) O3 0.049(3) 0.037(3) 0.060(3) 0.010(2) 0.012(3) 0.025(2) O4 0.037(3) 0.061(3) 0.048(3) 0.006(3) 0.005(2) 0.022(3) O5 0.034(3) 0.055(3) 0.058(3) 0.009(3) 0.010(3) 0.022(3) O6 0.056(3) 0.045(3) 0.060(3) 0.020(3) 0.016(3) 0.032(3) O7 0.106(5) 0.040(3) 0.075(4) 0.017(3) 0.037(4) 0.034(3) O8 0.047(3) 0.047(3) 0.044(3) 0.009(2) 0.013(3) 0.016(2) O9 0.049(3) 0.044(3) 0.059(3) 0.009(3) 0.019(3) 0.015(2) O10 0.099(5) 0.090(5) 0.057(4) 0.024(4) 0.038(4) 0.044(4) O11 0.029(3) 0.051(3) 0.045(3) 0.010(2) 0.010(2) 0.017(2) O12 0.039(3) 0.058(3) 0.039(3) 0.003(2) 0.001(2) 0.017(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 Er1 O4 2.288(5) . ? Er1 O8 2.306(5) . ? Er1 O3 2.314(4) . ? Er1 O6 2.321(5) . ? Er1 O12 2.336(5) . ? Er1 O9 2.354(5) . ? Er1 O5 2.357(5) . ? Er1 O11 2.361(4) . ? C1 O1 1.376(13) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.348(10) . ? C2 C3 1.370(12) . ? C2 C11 1.440(13) . ? C3 C4 1.387(11) . ? C3 H3 0.9300 . ? C4 C5 1.402(11) . ? C4 C9 1.412(11) . ? C5 C6 1.359(11) . ? C5 H5 0.9300 . ? C6 C7 1.427(11) . ? C6 H6 0.9300 . ? C7 C8 1.370(10) . ? C7 C12 1.417(11) . ? C8 C9 1.425(11) . ? C8 H8 0.9300 . ? C9 C10 1.429(11) . ? C10 C11 1.294(12) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 N2 1.369(10) . ? C12 N1 1.388(9) . ? C13 N1 1.500(10) . ? C13 C15 1.518(10) . ? C13 C14 1.525(10) . ? C13 C16 1.533(11) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N2 1.481(9) . ? C16 C17 1.520(11) . ? C16 C18 1.529(10) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 F3 1.16(3) . ? C19 F2 1.28(3) . ? C19 F1 1.28(2) . ? C19 F1' 1.342(10) . ? C19 F3' 1.342(9) . ? C19 F2' 1.354(9) . ? C19 C20 1.545(12) . ? C20 O5 1.238(9) . ? C20 C21 1.337(11) . ? C21 C22 1.377(11) . ? C21 H21 0.9300 . ? C22 O4 1.259(9) . ? C22 C23 1.557(11) . ? C23 F4 1.275(11) . ? C23 F5 1.289(10) . ? C23 F6 1.313(10) . ? C24 F7 1.286(9) . ? C24 F9 1.320(9) . ? C24 F8 1.330(9) . ? C24 C25 1.548(9) . ? C25 O11 1.230(8) . ? C25 C28 1.396(10) . ? C26 O12 1.239(8) . ? C26 C28 1.372(10) . ? C26 C27 1.526(12) . ? C27 F11 1.280(18) . ? C27 F12 1.303(18) . ? C27 F10' 1.322(10) . ? C27 F10 1.33(2) . ? C27 F11' 1.336(9) . ? C27 F12' 1.349(10) . ? C28 H28 0.9300 . ? C29 O8 1.234(8) . ? C29 C31 1.378(10) . ? C29 C30 1.592(11) . ? C30 F18 1.297(11) . ? C30 F16 1.301(12) . ? C30 F17 1.310(9) . ? C31 C32 1.352(10) . ? C31 H31 0.9300 . ? C32 O9 1.266(9) . ? C32 C33 1.553(12) . ? C33 F15 1.275(13) . ? C33 F14 1.332(10) . ? C33 F13 1.337(11) . ? C34 O10 1.426(10) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C40 1.357(11) . ? C35 O10 1.380(9) . ? C35 C36 1.384(12) . ? C36 C37 1.340(11) . ? C36 H36 0.9300 . ? C37 C38 1.435(10) . ? C37 H37 0.9300 . ? C38 C39 1.409(10) . ? C38 C44 1.423(10) . ? C39 C40 1.367(10) . ? C39 C41 1.418(10) . ? C40 H40 0.9300 . ? C41 C42 1.376(10) . ? C41 H41 0.9300 . ? C42 C43 1.412(10) . ? C42 H42 0.9300 . ? C43 C44 1.374(9) . ? C43 C45 1.416(10) . ? C44 H44 0.9300 . ? C45 N3 1.323(9) . ? C45 N4 1.372(9) . ? C46 C47 1.470(13) . ? C46 C48 1.514(11) . ? C46 N4 1.534(10) . ? C46 C50 1.560(11) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.515(12) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C51 1.481(11) . ? C50 N3 1.518(9) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? N1 O2 1.269(9) . ? N2 O3 1.297(7) . ? N3 O6 1.284(7) . ? N4 O7 1.264(8) . ? 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 O4 Er1 O8 141.56(18) . . ? O4 Er1 O3 97.55(18) . . ? O8 Er1 O3 92.42(17) . . ? O4 Er1 O6 92.28(18) . . ? O8 Er1 O6 103.36(18) . . ? O3 Er1 O6 140.27(18) . . ? O4 Er1 O12 144.70(18) . . ? O8 Er1 O12 73.73(18) . . ? O3 Er1 O12 76.90(18) . . ? O6 Er1 O12 73.10(19) . . ? O4 Er1 O9 78.62(18) . . ? O8 Er1 O9 73.34(17) . . ? O3 Er1 O9 147.47(19) . . ? O6 Er1 O9 72.22(18) . . ? O12 Er1 O9 124.06(18) . . ? O4 Er1 O5 72.59(18) . . ? O8 Er1 O5 74.37(19) . . ? O3 Er1 O5 75.15(18) . . ? O6 Er1 O5 144.07(18) . . ? O12 Er1 O5 136.10(18) . . ? O9 Er1 O5 72.90(18) . . ? O4 Er1 O11 71.86(17) . . ? O8 Er1 O11 146.05(18) . . ? O3 Er1 O11 72.55(17) . . ? O6 Er1 O11 74.26(17) . . ? O12 Er1 O11 73.27(17) . . ? O9 Er1 O11 133.79(17) . . ? O5 Er1 O11 127.39(17) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 127.0(10) . . ? O1 C2 C11 115.4(9) . . ? C3 C2 C11 117.6(9) . . ? C2 C3 C4 122.0(9) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C3 C4 C5 122.4(8) . . ? C3 C4 C9 118.8(8) . . ? C5 C4 C9 118.7(7) . . ? C6 C5 C4 120.6(9) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 121.6(8) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C8 C7 C12 120.8(8) . . ? C8 C7 C6 118.9(8) . . ? C12 C7 C6 120.1(7) . . ? C7 C8 C9 120.0(8) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C4 C9 C8 120.3(7) . . ? C4 C9 C10 118.5(8) . . ? C8 C9 C10 121.3(8) . . ? C11 C10 C9 121.0(9) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C2 122.1(9) . . ? C10 C11 H11 119.0 . . ? C2 C11 H11 119.0 . . ? N2 C12 N1 104.7(7) . . ? N2 C12 C7 127.8(7) . . ? N1 C12 C7 127.2(7) . . ? N1 C13 C15 107.0(7) . . ? N1 C13 C14 108.6(6) . . ? C15 C13 C14 110.3(7) . . ? N1 C13 C16 99.6(6) . . ? C15 C13 C16 113.7(7) . . ? C14 C13 C16 116.5(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C17 110.1(6) . . ? N2 C16 C18 105.6(6) . . ? C17 C16 C18 110.5(7) . . ? N2 C16 C13 100.1(6) . . ? C17 C16 C13 115.3(6) . . ? C18 C16 C13 114.2(6) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? F3 C19 F2 124(2) . . ? F3 C19 F1 63(2) . . ? F2 C19 F1 118(2) . . ? F3 C19 F1' 111(2) . . ? F2 C19 F1' 23.2(17) . . ? F1 C19 F1' 133.8(17) . . ? F3 C19 F3' 99(2) . . ? F2 C19 F3' 78.1(16) . . ? F1 C19 F3' 44.0(9) . . ? F1' C19 F3' 99.5(13) . . ? F3 C19 F2' 35.4(15) . . ? F2 C19 F2' 108.1(18) . . ? F1 C19 F2' 98.3(17) . . ? F1' C19 F2' 87.3(16) . . ? F3' C19 F2' 130.6(14) . . ? F3 C19 C20 121.3(16) . . ? F2 C19 C20 111(2) . . ? F1 C19 C20 110.0(12) . . ? F1' C19 C20 110.6(15) . . ? F3' C19 C20 112.4(9) . . ? F2' C19 C20 110.5(10) . . ? O5 C20 C21 128.4(8) . . ? O5 C20 C19 113.3(7) . . ? C21 C20 C19 118.3(8) . . ? C20 C21 C22 121.5(8) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? O4 C22 C21 127.5(7) . . ? O4 C22 C23 113.9(7) . . ? C21 C22 C23 118.5(8) . . ? F4 C23 F5 109.5(9) . . ? F4 C23 F6 107.3(8) . . ? F5 C23 F6 106.8(9) . . ? F4 C23 C22 112.3(9) . . ? F5 C23 C22 111.7(7) . . ? F6 C23 C22 109.1(7) . . ? F7 C24 F9 109.4(7) . . ? F7 C24 F8 107.7(6) . . ? F9 C24 F8 105.2(7) . . ? F7 C24 C25 111.8(7) . . ? F9 C24 C25 109.2(6) . . ? F8 C24 C25 113.3(7) . . ? O11 C25 C28 129.1(6) . . ? O11 C25 C24 112.6(7) . . ? C28 C25 C24 118.3(6) . . ? O12 C26 C28 129.0(7) . . ? O12 C26 C27 114.0(7) . . ? C28 C26 C27 116.9(7) . . ? F11 C27 F12 128.5(14) . . ? F11 C27 F10' 111.2(16) . . ? F12 C27 F10' 38.6(11) . . ? F11 C27 F10 49.7(12) . . ? F12 C27 F10 107.3(14) . . ? F10' C27 F10 71.6(15) . . ? F11 C27 F11' 63.2(13) . . ? F12 C27 F11' 99.7(14) . . ? F10' C27 F11' 126.4(15) . . ? F10 C27 F11' 110.5(16) . . ? F11 C27 F12' 97.2(15) . . ? F12 C27 F12' 69.2(13) . . ? F10' C27 F12' 105.2(16) . . ? F10 C27 F12' 136.7(15) . . ? F11' C27 F12' 35.8(11) . . ? F11 C27 C26 115.3(10) . . ? F12 C27 C26 116.0(12) . . ? F10' C27 C26 116.5(12) . . ? F10 C27 C26 110.4(10) . . ? F11' C27 C26 112.4(11) . . ? F12' C27 C26 109.1(12) . . ? C26 C28 C25 120.5(6) . . ? C26 C28 H28 119.7 . . ? C25 C28 H28 119.7 . . ? O8 C29 C31 129.8(7) . . ? O8 C29 C30 112.9(7) . . ? C31 C29 C30 117.2(7) . . ? F18 C30 F16 108.8(9) . . ? F18 C30 F17 107.2(8) . . ? F16 C30 F17 107.5(9) . . ? F18 C30 C29 108.2(8) . . ? F16 C30 C29 112.4(8) . . ? F17 C30 C29 112.6(7) . . ? C32 C31 C29 119.7(7) . . ? C32 C31 H31 120.1 . . ? C29 C31 H31 120.1 . . ? O9 C32 C31 129.8(7) . . ? O9 C32 C33 111.7(7) . . ? C31 C32 C33 118.2(7) . . ? F15 C33 F14 109.5(9) . . ? F15 C33 F13 107.1(10) . . ? F14 C33 F13 105.6(9) . . ? F15 C33 C32 112.9(9) . . ? F14 C33 C32 111.3(8) . . ? F13 C33 C32 110.1(8) . . ? O10 C34 H34A 109.5 . . ? O10 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O10 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 O10 124.4(8) . . ? C40 C35 C36 120.1(7) . . ? O10 C35 C36 115.5(7) . . ? C37 C36 C35 120.1(8) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 121.4(8) . . ? C36 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? C39 C38 C44 120.7(6) . . ? C39 C38 C37 117.0(7) . . ? C44 C38 C37 122.3(7) . . ? C40 C39 C38 119.6(7) . . ? C40 C39 C41 122.8(7) . . ? C38 C39 C41 117.6(6) . . ? C35 C40 C39 121.9(8) . . ? C35 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C42 C41 C39 121.3(7) . . ? C42 C41 H41 119.3 . . ? C39 C41 H41 119.3 . . ? C41 C42 C43 120.5(7) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 119.8(6) . . ? C44 C43 C45 121.1(7) . . ? C42 C43 C45 119.0(6) . . ? C43 C44 C38 120.0(7) . . ? C43 C44 H44 120.0 . . ? C38 C44 H44 120.0 . . ? N3 C45 N4 107.3(6) . . ? N3 C45 C43 127.5(6) . . ? N4 C45 C43 125.2(6) . . ? C47 C46 C48 112.3(8) . . ? C47 C46 N4 105.7(7) . . ? C48 C46 N4 108.7(7) . . ? C47 C46 C50 115.7(8) . . ? C48 C46 C50 113.7(7) . . ? N4 C46 C50 99.5(6) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C49 111.8(7) . . ? C51 C50 N3 109.6(6) . . ? C49 C50 N3 105.1(7) . . ? C51 C50 C46 114.6(8) . . ? C49 C50 C46 114.6(7) . . ? N3 C50 C46 99.9(6) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O2 N1 C12 123.4(7) . . ? O2 N1 C13 124.3(6) . . ? C12 N1 C13 112.0(7) . . ? O3 N2 C12 124.8(6) . . ? O3 N2 C16 121.5(6) . . ? C12 N2 C16 112.9(6) . . ? O6 N3 C45 126.0(6) . . ? O6 N3 C50 118.8(6) . . ? C45 N3 C50 114.1(6) . . ? O7 N4 C45 125.8(6) . . ? O7 N4 C46 121.9(6) . . ? C45 N4 C46 112.0(6) . . ? C2 O1 C1 116.2(9) . . ? N2 O3 Er1 134.9(4) . . ? C22 O4 Er1 134.8(5) . . ? C20 O5 Er1 132.7(5) . . ? N3 O6 Er1 140.5(5) . . ? C29 O8 Er1 134.3(5) . . ? C32 O9 Er1 132.1(5) . . ? C35 O10 C34 117.2(7) . . ? C25 O11 Er1 133.4(5) . . ? C26 O12 Er1 134.5(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.194 _refine_diff_density_min -3.142 _refine_diff_density_rms 0.177 # Attachment '- complex-7.cif' data_shelxlg _database_code_depnum_ccdc_archive 'CCDC 783309' #TrackingRef '- complex-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H45 F18 N4 O12 Tm1' _chemical_formula_weight 1416.84 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.768(2) _cell_length_b 14.695(3) _cell_length_c 17.642(3) _cell_angle_alpha 97.37(3) _cell_angle_beta 93.85(3) _cell_angle_gamma 108.19(3) _cell_volume 2855.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17424 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.74 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 1.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.747 _exptl_absorpt_correction_T_max 0.791 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16486 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9980 _reflns_number_gt 8505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Fluorine atoms in the CF3 groups were treated by disorder and these atoms were refined anisotropically with application of restraints on interatomic distances and thermal parameters (DFIX, ISOR and SIMU instructions in SHELXL). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^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 9980 _refine_ls_number_parameters 813 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.077 _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 F5 F 0.7184(17) 0.4741(12) 0.4132(10) 0.149(6) Uani 0.602(18) 1 d PU . . Tm1 Tm 0.35431(2) 0.242406(16) 0.237775(12) 0.03539(9) Uani 1 1 d . . . C1 C 0.6809(5) 0.3420(4) 0.0990(3) 0.0495(14) Uani 1 1 d . . . F1 F 0.6763(4) 0.2544(3) 0.0655(2) 0.0812(12) Uani 1 1 d . . . F2 F 0.6283(4) 0.3791(3) 0.0489(2) 0.0890(13) Uani 1 1 d . . . F3 F 0.7955(3) 0.3936(3) 0.1108(2) 0.0800(12) Uani 1 1 d . . . C2 C 0.7242(6) 0.3881(6) 0.3830(4) 0.073(2) Uani 1 1 d DU . . F4 F 0.8279(11) 0.4477(12) 0.3787(9) 0.116(5) Uani 0.602(18) 1 d PU . . F4' F 0.8373(12) 0.393(2) 0.3761(13) 0.104(6) Uani 0.398(18) 1 d PDU . . F5' F 0.6793(18) 0.428(2) 0.4400(8) 0.109(6) Uani 0.398(18) 1 d PDU . . F6' F 0.752(2) 0.3123(12) 0.4046(12) 0.119(6) Uani 0.398(18) 1 d PDU . . C3 C 0.1621(7) 0.1241(5) -0.0075(4) 0.072(2) Uani 1 1 d . . . C4 C -0.0434(6) 0.2327(6) 0.2080(5) 0.077(2) Uani 1 1 d . . . C5 C 0.2091(7) 0.2482(5) 0.4739(4) 0.0673(19) Uani 1 1 d . . . C6 C 0.0608(7) -0.0414(5) 0.2701(4) 0.073(2) Uani 1 1 d . . . C7 C 0.6175(5) 0.3325(4) 0.1726(3) 0.0396(12) Uani 1 1 d . . . C8 C 0.6892(5) 0.3632(4) 0.2422(3) 0.0504(14) Uani 1 1 d . . . H8 H 0.7721 0.3913 0.2435 0.060 Uiso 1 1 calc R . . C9 C 0.6379(5) 0.3522(4) 0.3098(3) 0.0462(14) Uani 1 1 d . . . C10 C 0.1502(5) 0.0609(4) 0.2952(4) 0.0494(14) Uani 1 1 d . . . C11 C 0.1471(5) 0.1070(4) 0.3674(3) 0.0547(15) Uani 1 1 d . . . H11 H 0.0923 0.0752 0.3986 0.066 Uiso 1 1 calc R . . C12 C 0.2240(5) 0.1997(4) 0.3945(3) 0.0483(14) Uani 1 1 d . . . C13 C 0.1706(5) 0.1691(4) 0.0772(3) 0.0468(14) Uani 1 1 d . . . C14 C 0.0681(5) 0.1816(4) 0.1048(3) 0.0564(16) Uani 1 1 d . . . H14 H -0.0043 0.1606 0.0728 0.068 Uiso 1 1 calc R . . C15 C 0.0729(5) 0.2247(4) 0.1787(3) 0.0495(14) Uani 1 1 d . . . C16 C 0.1072(7) 0.3382(6) -0.2779(4) 0.092(3) Uani 1 1 d . . . H16A H 0.0432 0.2935 -0.2572 0.138 Uiso 1 1 calc R . . H16B H 0.1062 0.3153 -0.3314 0.138 Uiso 1 1 calc R . . H16C H 0.0964 0.4008 -0.2721 0.138 Uiso 1 1 calc R . . C17 C 0.2272(7) 0.3632(5) -0.1597(3) 0.0645(18) Uani 1 1 d . . . C18 C 0.3411(6) 0.3704(5) -0.1241(4) 0.0698(19) Uani 1 1 d . . . H18 H 0.4008 0.3636 -0.1541 0.084 Uiso 1 1 calc R . . C19 C 0.3644(6) 0.3873(5) -0.0460(4) 0.0643(18) Uani 1 1 d . . . H19 H 0.4386 0.3888 -0.0232 0.077 Uiso 1 1 calc R . . C20 C 0.2768(5) 0.4026(4) 0.0009(3) 0.0499(14) Uani 1 1 d . . . C21 C 0.3010(5) 0.4269(4) 0.0809(3) 0.0476(14) Uani 1 1 d . . . H21 H 0.3755 0.4306 0.1049 0.057 Uiso 1 1 calc R . . C22 C 0.2158(5) 0.4453(4) 0.1241(3) 0.0465(14) Uani 1 1 d . . . C23 C 0.1006(5) 0.4354(4) 0.0873(3) 0.0587(16) Uani 1 1 d . . . H23 H 0.0421 0.4468 0.1164 0.070 Uiso 1 1 calc R . . C24 C 0.0755(6) 0.4095(5) 0.0103(3) 0.0580(16) Uani 1 1 d . . . H24 H -0.0011 0.4017 -0.0127 0.070 Uiso 1 1 calc R . . C25 C 0.1624(6) 0.3942(4) -0.0361(3) 0.0534(15) Uani 1 1 d . . . C26 C 0.1396(6) 0.3733(4) -0.1172(3) 0.0602(17) Uani 1 1 d . . . H26 H 0.0641 0.3666 -0.1413 0.072 Uiso 1 1 calc R . . C27 C 0.2456(5) 0.4808(4) 0.2061(3) 0.0447(13) Uani 1 1 d . . . C28 C 0.2410(6) 0.5580(4) 0.3313(3) 0.0499(14) Uani 1 1 d . . . C29 C 0.2543(7) 0.6597(4) 0.3696(4) 0.073(2) Uani 1 1 d . . . H29A H 0.2978 0.7059 0.3393 0.110 Uiso 1 1 calc R . . H29B H 0.2975 0.6720 0.4200 0.110 Uiso 1 1 calc R . . H29C H 0.1760 0.6658 0.3739 0.110 Uiso 1 1 calc R . . C30 C 0.1451(6) 0.4857(5) 0.3640(4) 0.0659(18) Uani 1 1 d . . . H30A H 0.0690 0.4950 0.3524 0.099 Uiso 1 1 calc R . . H30B H 0.1640 0.4942 0.4188 0.099 Uiso 1 1 calc R . . H30C H 0.1406 0.4213 0.3419 0.099 Uiso 1 1 calc R . . C31 C 0.3945(6) 0.4878(4) 0.3937(3) 0.0637(18) Uani 1 1 d . . . H31A H 0.3308 0.4294 0.3972 0.095 Uiso 1 1 calc R . . H31B H 0.4084 0.5322 0.4410 0.095 Uiso 1 1 calc R . . H31C H 0.4667 0.4727 0.3848 0.095 Uiso 1 1 calc R . . C32 C 0.4648(6) 0.6186(4) 0.3131(4) 0.0637(17) Uani 1 1 d . . . H32A H 0.5307 0.5959 0.3014 0.096 Uiso 1 1 calc R . . H32B H 0.4891 0.6670 0.3584 0.096 Uiso 1 1 calc R . . H32C H 0.4416 0.6463 0.2706 0.096 Uiso 1 1 calc R . . C33 C 0.2829(6) 0.1414(5) 0.7219(4) 0.076(2) Uani 1 1 d . . . H33A H 0.3690 0.1698 0.7278 0.115 Uiso 1 1 calc R . . H33B H 0.2538 0.1475 0.7711 0.115 Uiso 1 1 calc R . . H33C H 0.2480 0.1741 0.6880 0.115 Uiso 1 1 calc R . . C34 C 0.2770(6) 0.0227(5) 0.6172(3) 0.0567(16) Uani 1 1 d . . . C35 C 0.2129(6) -0.0718(5) 0.5798(4) 0.0685(19) Uani 1 1 d . . . H35 H 0.1594 -0.1153 0.6051 0.082 Uiso 1 1 calc R . . C36 C 0.2303(6) -0.0986(4) 0.5059(4) 0.0657(18) Uani 1 1 d . . . H36 H 0.1880 -0.1611 0.4811 0.079 Uiso 1 1 calc R . . C37 C 0.3109(5) -0.0342(4) 0.4654(3) 0.0469(14) Uani 1 1 d . . . C38 C 0.3277(5) -0.0593(4) 0.3886(3) 0.0472(14) Uani 1 1 d . . . H38 H 0.2846 -0.1208 0.3621 0.057 Uiso 1 1 calc R . . C39 C 0.4734(5) 0.0972(4) 0.3931(3) 0.0461(14) Uani 1 1 d . . . H39 H 0.5283 0.1412 0.3689 0.055 Uiso 1 1 calc R . . C40 C 0.4585(5) 0.1217(4) 0.4668(3) 0.0500(15) Uani 1 1 d . . . H40 H 0.5044 0.1827 0.4929 0.060 Uiso 1 1 calc R . . C41 C 0.3771(5) 0.0592(4) 0.5053(3) 0.0437(13) Uani 1 1 d . . . C42 C 0.3575(5) 0.0852(4) 0.5811(3) 0.0520(15) Uani 1 1 d . . . H42 H 0.4006 0.1468 0.6072 0.062 Uiso 1 1 calc R . . C43 C 0.4181(5) -0.0197(4) 0.2720(3) 0.0438(13) Uani 1 1 d . . . C44 C 0.4064(6) -0.1145(5) 0.1502(3) 0.0573(16) Uani 1 1 d . . . C45 C 0.4667(6) -0.0040(5) 0.1452(3) 0.0526(15) Uani 1 1 d . . . C46 C 0.4093(7) 0.0312(5) 0.0801(3) 0.071(2) Uani 1 1 d . . . H46A H 0.3271 0.0239 0.0877 0.107 Uiso 1 1 calc R . . H46B H 0.4119 -0.0064 0.0320 0.107 Uiso 1 1 calc R . . H46C H 0.4526 0.0983 0.0796 0.107 Uiso 1 1 calc R . . C47 C 0.6021(6) 0.0279(5) 0.1487(4) 0.0666(18) Uani 1 1 d . . . H47A H 0.6337 0.0975 0.1574 0.100 Uiso 1 1 calc R . . H47B H 0.6245 0.0033 0.1009 0.100 Uiso 1 1 calc R . . H47C H 0.6344 0.0032 0.1899 0.100 Uiso 1 1 calc R . . C48 C 0.4755(7) -0.1802(5) 0.1187(4) 0.076(2) Uani 1 1 d . . . H48A H 0.5566 -0.1564 0.1435 0.114 Uiso 1 1 calc R . . H48B H 0.4763 -0.1807 0.0643 0.114 Uiso 1 1 calc R . . H48C H 0.4371 -0.2448 0.1285 0.114 Uiso 1 1 calc R . . C49 C 0.2740(6) -0.1558(6) 0.1180(4) 0.088(2) Uani 1 1 d . . . H49A H 0.2400 -0.2193 0.1312 0.132 Uiso 1 1 calc R . . H49B H 0.2669 -0.1599 0.0630 0.132 Uiso 1 1 calc R . . H49C H 0.2317 -0.1142 0.1394 0.132 Uiso 1 1 calc R . . C56 C 0.3589(5) 0.5344(4) 0.3270(3) 0.0459(14) Uani 1 1 d . . . C68 C 0.4061(5) 0.0050(4) 0.3523(3) 0.0417(13) Uani 1 1 d . . . F7 F 0.1173(4) -0.1028(3) 0.2447(3) 0.130(2) Uani 1 1 d . . . O12 O 0.2192(5) 0.3458(4) -0.2378(2) 0.0847(15) Uani 1 1 d . . . F8 F -0.0193(5) -0.0403(4) 0.2162(3) 0.124(2) Uani 1 1 d . . . O11 O 0.1242(5) 0.5800(4) 0.2212(3) 0.0874(16) Uani 1 1 d . . . F9 F 0.0030(4) -0.0802(3) 0.3258(3) 0.0961(14) Uani 1 1 d . . . F10 F 0.1541(5) 0.1850(3) 0.5179(2) 0.1066(16) Uani 1 1 d . . . F11 F 0.3138(5) 0.2959(4) 0.5132(2) 0.1212(19) Uani 1 1 d . . . F12 F 0.1493(5) 0.3080(4) 0.4680(2) 0.1187(19) Uani 1 1 d . . . F13 F -0.0672(5) 0.1949(6) 0.2667(4) 0.192(4) Uani 1 1 d . . . F14 F -0.0363(4) 0.3243(4) 0.2262(3) 0.1172(18) Uani 1 1 d . . . F15 F -0.1356(4) 0.2024(5) 0.1551(3) 0.145(2) Uani 1 1 d . . . F16 F 0.0701(5) 0.1307(4) -0.0491(2) 0.128(2) Uani 1 1 d . . . F17 F 0.1459(4) 0.0296(3) -0.0114(2) 0.1055(15) Uani 1 1 d . . . F18 F 0.2588(5) 0.1590(4) -0.0391(2) 0.1145(18) Uani 1 1 d . . . N1 N 0.4088(4) -0.1098(3) 0.2350(3) 0.0514(12) Uani 1 1 d . . . N2 N 0.4390(4) 0.0401(3) 0.2204(2) 0.0432(11) Uani 1 1 d . . . N3 N 0.3264(4) 0.4643(3) 0.2537(2) 0.0415(10) Uani 1 1 d . . . N4 N 0.2003(5) 0.5429(4) 0.2479(3) 0.0558(13) Uani 1 1 d . . . O1 O 0.2508(4) 0.0425(4) 0.6905(2) 0.0759(13) Uani 1 1 d . . . O2 O 0.3978(5) -0.1826(3) 0.2665(3) 0.0769(14) Uani 1 1 d . . . O3 O 0.4587(3) 0.1334(3) 0.23351(19) 0.0452(9) Uani 1 1 d . . . O4 O 0.2166(3) 0.0911(3) 0.2458(2) 0.0499(9) Uani 1 1 d . . . O5 O 0.3015(3) 0.2520(3) 0.3606(2) 0.0460(9) Uani 1 1 d . . . O6 O 0.1624(3) 0.2591(3) 0.2291(2) 0.0490(9) Uani 1 1 d . . . O7 O 0.2734(3) 0.1890(3) 0.1129(2) 0.0470(9) Uani 1 1 d . . . O8 O 0.5067(3) 0.2948(2) 0.15965(18) 0.0406(8) Uani 1 1 d . . . O9 O 0.5317(3) 0.3156(3) 0.31997(18) 0.0435(9) Uani 1 1 d . . . O10 O 0.3877(3) 0.4054(2) 0.23683(19) 0.0426(9) Uani 1 1 d . . . F6 F 0.6912(14) 0.3387(14) 0.4365(7) 0.139(6) Uani 0.602(18) 1 d PU . . 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 F5 0.155(12) 0.159(11) 0.088(9) -0.052(8) -0.019(8) 0.019(9) Tm1 0.03548(16) 0.03546(14) 0.03864(14) 0.00499(9) 0.00547(9) 0.01640(10) C1 0.047(4) 0.050(4) 0.055(4) 0.013(3) 0.010(3) 0.017(3) F1 0.101(3) 0.081(3) 0.067(2) 0.000(2) 0.035(2) 0.035(2) F2 0.078(3) 0.136(4) 0.083(3) 0.070(3) 0.025(2) 0.054(3) F3 0.045(2) 0.107(3) 0.082(3) 0.023(2) 0.0214(18) 0.011(2) C2 0.058(5) 0.092(5) 0.057(4) 0.003(4) 0.004(3) 0.013(4) F4 0.067(7) 0.148(12) 0.091(6) 0.006(9) -0.019(5) -0.014(7) F4' 0.039(7) 0.193(16) 0.072(7) 0.000(12) -0.011(5) 0.039(9) F5' 0.084(9) 0.192(15) 0.038(7) -0.031(9) 0.003(6) 0.045(11) F6' 0.112(12) 0.156(11) 0.083(10) 0.018(9) -0.047(9) 0.048(9) C3 0.084(6) 0.061(5) 0.061(4) -0.006(3) -0.010(4) 0.020(4) C4 0.037(4) 0.096(6) 0.100(6) 0.016(5) 0.010(4) 0.026(4) C5 0.084(6) 0.064(4) 0.054(4) 0.010(3) 0.028(4) 0.021(4) C6 0.064(5) 0.065(5) 0.075(5) -0.004(4) 0.020(4) 0.005(4) C7 0.039(4) 0.037(3) 0.050(3) 0.009(2) 0.013(2) 0.020(3) C8 0.033(3) 0.061(4) 0.050(4) 0.001(3) 0.003(3) 0.009(3) C9 0.045(4) 0.052(4) 0.042(3) 0.001(3) -0.001(3) 0.021(3) C10 0.043(4) 0.040(3) 0.068(4) 0.010(3) 0.013(3) 0.016(3) C11 0.052(4) 0.050(4) 0.063(4) 0.016(3) 0.019(3) 0.012(3) C12 0.051(4) 0.050(4) 0.053(3) 0.016(3) 0.008(3) 0.026(3) C13 0.049(4) 0.036(3) 0.048(3) 0.006(2) -0.003(3) 0.006(3) C14 0.040(4) 0.061(4) 0.063(4) 0.002(3) -0.004(3) 0.014(3) C15 0.032(3) 0.049(4) 0.070(4) 0.014(3) 0.007(3) 0.015(3) C16 0.120(7) 0.110(6) 0.051(4) 0.000(4) -0.019(4) 0.055(5) C17 0.093(6) 0.068(4) 0.049(4) 0.004(3) 0.005(3) 0.052(4) C18 0.082(5) 0.091(5) 0.053(4) 0.006(3) 0.018(3) 0.052(4) C19 0.060(4) 0.079(5) 0.065(4) 0.007(3) 0.010(3) 0.040(4) C20 0.053(4) 0.049(4) 0.055(4) 0.011(3) 0.011(3) 0.026(3) C21 0.054(4) 0.044(3) 0.050(3) 0.009(3) 0.005(3) 0.024(3) C22 0.057(4) 0.039(3) 0.049(3) 0.014(2) 0.010(3) 0.020(3) C23 0.049(4) 0.072(4) 0.064(4) 0.012(3) 0.009(3) 0.030(3) C24 0.051(4) 0.074(4) 0.058(4) 0.012(3) 0.001(3) 0.034(3) C25 0.057(4) 0.047(4) 0.062(4) 0.012(3) 0.004(3) 0.024(3) C26 0.073(5) 0.056(4) 0.057(4) 0.005(3) -0.007(3) 0.033(4) C27 0.048(4) 0.045(3) 0.052(3) 0.014(3) 0.013(3) 0.026(3) C28 0.069(4) 0.041(3) 0.048(3) 0.010(3) 0.016(3) 0.028(3) C29 0.109(6) 0.040(4) 0.079(5) 0.005(3) 0.028(4) 0.035(4) C30 0.072(5) 0.060(4) 0.072(4) 0.013(3) 0.024(3) 0.026(4) C31 0.088(5) 0.061(4) 0.047(4) -0.002(3) 0.000(3) 0.037(4) C32 0.069(5) 0.044(4) 0.074(4) 0.003(3) 0.014(3) 0.013(3) C33 0.073(5) 0.096(6) 0.055(4) -0.007(4) 0.017(3) 0.026(4) C34 0.072(5) 0.067(4) 0.046(3) 0.012(3) 0.020(3) 0.040(4) C35 0.080(5) 0.069(5) 0.071(5) 0.028(4) 0.044(4) 0.032(4) C36 0.077(5) 0.045(4) 0.076(5) 0.012(3) 0.031(4) 0.015(3) C37 0.061(4) 0.036(3) 0.054(3) 0.016(3) 0.023(3) 0.023(3) C38 0.062(4) 0.034(3) 0.051(3) 0.009(2) 0.015(3) 0.022(3) C39 0.052(4) 0.042(3) 0.049(3) 0.017(3) 0.008(3) 0.017(3) C40 0.064(4) 0.040(3) 0.041(3) 0.009(2) 0.000(3) 0.011(3) C41 0.047(4) 0.046(3) 0.045(3) 0.012(3) 0.007(2) 0.023(3) C42 0.063(4) 0.056(4) 0.039(3) 0.005(3) 0.006(3) 0.024(3) C43 0.058(4) 0.036(3) 0.046(3) 0.013(2) 0.016(3) 0.023(3) C44 0.071(5) 0.058(4) 0.048(3) -0.002(3) 0.011(3) 0.031(3) C45 0.072(5) 0.067(4) 0.037(3) 0.012(3) 0.021(3) 0.043(3) C46 0.106(6) 0.082(5) 0.049(4) 0.014(3) 0.015(3) 0.062(4) C47 0.067(5) 0.081(5) 0.065(4) 0.015(3) 0.027(3) 0.037(4) C48 0.117(6) 0.077(5) 0.057(4) 0.003(3) 0.021(4) 0.064(5) C49 0.075(6) 0.095(6) 0.086(5) -0.014(4) 0.005(4) 0.026(4) C56 0.062(4) 0.031(3) 0.048(3) 0.004(2) 0.012(3) 0.020(3) C68 0.050(4) 0.039(3) 0.044(3) 0.013(2) 0.012(2) 0.022(3) F7 0.105(4) 0.049(3) 0.213(6) -0.028(3) 0.069(4) 0.001(2) O12 0.118(4) 0.106(4) 0.046(3) 0.002(2) 0.005(3) 0.065(3) F8 0.099(4) 0.119(4) 0.103(4) 0.020(3) -0.027(3) -0.029(3) O11 0.106(4) 0.101(4) 0.087(3) 0.008(3) 0.008(3) 0.081(3) F9 0.095(3) 0.062(3) 0.111(3) 0.015(2) 0.035(3) -0.009(2) F10 0.161(5) 0.091(3) 0.072(3) 0.025(2) 0.057(3) 0.033(3) F11 0.117(4) 0.146(5) 0.065(3) -0.028(3) 0.010(3) 0.011(3) F12 0.208(6) 0.129(4) 0.085(3) 0.035(3) 0.061(3) 0.132(4) F13 0.118(5) 0.332(10) 0.238(7) 0.210(7) 0.133(5) 0.145(6) F14 0.088(4) 0.116(4) 0.167(5) -0.003(3) 0.033(3) 0.066(3) F15 0.041(3) 0.200(6) 0.175(5) -0.044(4) -0.004(3) 0.044(3) F16 0.146(5) 0.183(5) 0.064(3) -0.016(3) -0.044(3) 0.093(4) F17 0.139(4) 0.068(3) 0.090(3) -0.028(2) -0.014(3) 0.026(3) F18 0.120(4) 0.127(4) 0.062(3) -0.012(2) 0.028(3) -0.002(3) N1 0.072(4) 0.037(3) 0.054(3) 0.008(2) 0.018(2) 0.029(2) N2 0.051(3) 0.046(3) 0.042(3) 0.007(2) 0.013(2) 0.027(2) N3 0.052(3) 0.032(2) 0.046(3) 0.0072(19) 0.009(2) 0.020(2) N4 0.070(4) 0.053(3) 0.061(3) 0.013(2) 0.013(2) 0.042(3) O1 0.101(4) 0.086(4) 0.055(3) 0.018(2) 0.035(2) 0.042(3) O2 0.122(4) 0.040(3) 0.079(3) 0.016(2) 0.038(3) 0.034(3) O3 0.056(3) 0.039(2) 0.052(2) 0.0162(17) 0.0147(17) 0.0267(18) O4 0.047(3) 0.046(2) 0.058(2) 0.0042(18) 0.0117(19) 0.0171(19) O5 0.052(3) 0.040(2) 0.047(2) 0.0078(17) 0.0082(18) 0.0158(19) O6 0.042(3) 0.053(2) 0.055(2) 0.0051(18) 0.0040(18) 0.0214(19) O7 0.043(2) 0.047(2) 0.049(2) -0.0014(17) 0.0006(17) 0.0177(19) O8 0.037(2) 0.045(2) 0.040(2) 0.0054(16) 0.0045(15) 0.0146(18) O9 0.039(2) 0.051(2) 0.040(2) 0.0037(16) 0.0039(16) 0.0157(19) O10 0.049(2) 0.035(2) 0.050(2) 0.0073(16) 0.0064(16) 0.0221(18) F6 0.104(9) 0.204(11) 0.061(6) 0.034(8) -0.028(5) -0.014(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F5 C2 1.331(15) . ? Tm1 O7 2.276(3) . ? Tm1 O5 2.294(4) . ? Tm1 O3 2.299(3) . ? Tm1 O10 2.306(3) . ? Tm1 O9 2.325(4) . ? Tm1 O8 2.335(4) . ? Tm1 O4 2.335(4) . ? Tm1 O6 2.344(4) . ? C1 F2 1.312(6) . ? C1 F3 1.311(6) . ? C1 F1 1.329(6) . ? C1 C7 1.541(7) . ? C2 F6 1.271(13) . ? C2 F4 1.274(13) . ? C2 F4' 1.325(10) . ? C2 F5' 1.320(9) . ? C2 F6' 1.347(9) . ? C2 C9 1.514(8) . ? C3 F18 1.289(8) . ? C3 F16 1.302(8) . ? C3 F17 1.334(8) . ? C3 C13 1.539(8) . ? C4 F13 1.245(9) . ? C4 F15 1.305(8) . ? C4 F14 1.318(9) . ? C4 C15 1.528(8) . ? C5 F12 1.295(8) . ? C5 F11 1.309(8) . ? C5 F10 1.327(7) . ? C5 C12 1.534(8) . ? C6 F8 1.299(8) . ? C6 F9 1.322(8) . ? C6 F7 1.329(8) . ? C6 C10 1.531(8) . ? C7 O8 1.239(6) . ? C7 C8 1.380(7) . ? C8 C9 1.378(7) . ? C8 H8 0.9300 . ? C9 O9 1.232(6) . ? C10 O4 1.242(6) . ? C10 C11 1.371(8) . ? C11 C12 1.382(8) . ? C11 H11 0.9300 . ? C12 O5 1.238(6) . ? C13 O7 1.256(6) . ? C13 C14 1.386(8) . ? C14 C15 1.363(8) . ? C14 H14 0.9300 . ? C15 O6 1.257(6) . ? C16 O12 1.419(8) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C26 1.348(9) . ? C17 O12 1.360(7) . ? C17 C18 1.408(9) . ? C18 C19 1.362(8) . ? C18 H18 0.9300 . ? C19 C20 1.417(8) . ? C19 H19 0.9300 . ? C20 C21 1.397(7) . ? C20 C25 1.418(8) . ? C21 C22 1.371(7) . ? C21 H21 0.9300 . ? C22 C23 1.419(8) . ? C22 C27 1.453(7) . ? C23 C24 1.349(8) . ? C23 H23 0.9300 . ? C24 C25 1.405(8) . ? C24 H24 0.9300 . ? C25 C26 1.414(8) . ? C26 H26 0.9300 . ? C27 N3 1.325(6) . ? C27 N4 1.359(6) . ? C28 N4 1.483(7) . ? C28 C30 1.495(8) . ? C28 C29 1.515(7) . ? C28 C56 1.537(8) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C56 1.532(7) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C56 1.517(8) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 O1 1.408(7) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C42 1.355(8) . ? C34 O1 1.364(6) . ? C34 C35 1.406(8) . ? C35 C36 1.361(8) . ? C35 H35 0.9300 . ? C36 C37 1.417(8) . ? C36 H36 0.9300 . ? C37 C38 1.402(7) . ? C37 C41 1.413(7) . ? C38 C68 1.358(7) . ? C38 H38 0.9300 . ? C39 C40 1.342(7) . ? C39 C68 1.409(7) . ? C39 H39 0.9300 . ? C40 C41 1.386(7) . ? C40 H40 0.9300 . ? C41 C42 1.397(7) . ? C42 H42 0.9300 . ? C43 N2 1.327(6) . ? C43 N1 1.367(6) . ? C43 C68 1.444(7) . ? C44 N1 1.487(7) . ? C44 C48 1.522(8) . ? C44 C49 1.523(9) . ? C44 C45 1.572(9) . ? C45 N2 1.503(6) . ? C45 C47 1.508(8) . ? C45 C46 1.520(8) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C56 N3 1.493(6) . ? O11 N4 1.279(6) . ? N1 O2 1.242(6) . ? N2 O3 1.305(5) . ? N3 O10 1.307(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 O7 Tm1 O5 141.72(14) . . ? O7 Tm1 O3 92.23(13) . . ? O5 Tm1 O3 103.74(12) . . ? O7 Tm1 O10 97.42(13) . . ? O5 Tm1 O10 92.36(12) . . ? O3 Tm1 O10 139.84(13) . . ? O7 Tm1 O9 145.12(13) . . ? O5 Tm1 O9 73.16(13) . . ? O3 Tm1 O9 73.01(13) . . ? O10 Tm1 O9 77.08(12) . . ? O7 Tm1 O8 71.93(13) . . ? O5 Tm1 O8 145.83(13) . . ? O3 Tm1 O8 73.54(12) . . ? O10 Tm1 O8 72.71(12) . . ? O9 Tm1 O8 73.59(12) . . ? O7 Tm1 O4 78.35(14) . . ? O5 Tm1 O4 73.75(13) . . ? O3 Tm1 O4 72.77(13) . . ? O10 Tm1 O4 147.38(13) . . ? O9 Tm1 O4 124.08(13) . . ? O8 Tm1 O4 133.52(12) . . ? O7 Tm1 O6 73.40(13) . . ? O5 Tm1 O6 73.69(13) . . ? O3 Tm1 O6 144.83(14) . . ? O10 Tm1 O6 74.86(13) . . ? O9 Tm1 O6 135.05(12) . . ? O8 Tm1 O6 128.09(13) . . ? O4 Tm1 O6 72.94(13) . . ? F2 C1 F3 107.9(5) . . ? F2 C1 F1 107.2(5) . . ? F3 C1 F1 105.7(5) . . ? F2 C1 C7 112.0(5) . . ? F3 C1 C7 114.5(5) . . ? F1 C1 C7 109.1(5) . . ? F6 C2 F4 127.7(11) . . ? F6 C2 F5 101.5(10) . . ? F4 C2 F5 75.4(15) . . ? F6 C2 F4' 106.7(18) . . ? F4 C2 F4' 37.5(11) . . ? F5 C2 F4' 110.5(17) . . ? F6 C2 F5' 63.0(11) . . ? F4 C2 F5' 106.6(17) . . ? F5 C2 F5' 39.8(10) . . ? F4' C2 F5' 129.2(14) . . ? F6 C2 F6' 48.3(9) . . ? F4 C2 F6' 101.7(17) . . ? F5 C2 F6' 140.2(11) . . ? F4' C2 F6' 66.5(19) . . ? F5' C2 F6' 109.0(14) . . ? F6 C2 C9 113.3(8) . . ? F4 C2 C9 117.3(9) . . ? F5 C2 C9 107.9(9) . . ? F4' C2 C9 116.0(11) . . ? F5' C2 C9 113.1(9) . . ? F6' C2 C9 108.4(8) . . ? F18 C3 F16 109.6(7) . . ? F18 C3 F17 105.6(7) . . ? F16 C3 F17 106.3(6) . . ? F18 C3 C13 113.5(6) . . ? F16 C3 C13 112.4(6) . . ? F17 C3 C13 108.9(6) . . ? F13 C4 F15 111.4(7) . . ? F13 C4 F14 106.4(8) . . ? F15 C4 F14 100.5(6) . . ? F13 C4 C15 113.3(6) . . ? F15 C4 C15 113.5(7) . . ? F14 C4 C15 110.8(6) . . ? F12 C5 F11 108.4(6) . . ? F12 C5 F10 108.2(6) . . ? F11 C5 F10 104.4(6) . . ? F12 C5 C12 111.4(6) . . ? F11 C5 C12 111.1(6) . . ? F10 C5 C12 113.1(6) . . ? F8 C6 F9 107.6(6) . . ? F8 C6 F7 109.6(7) . . ? F9 C6 F7 104.4(7) . . ? F8 C6 C10 109.8(6) . . ? F9 C6 C10 114.4(6) . . ? F7 C6 C10 110.8(6) . . ? O8 C7 C8 129.2(5) . . ? O8 C7 C1 113.4(5) . . ? C8 C7 C1 117.4(5) . . ? C9 C8 C7 119.9(5) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? O9 C9 C8 129.7(5) . . ? O9 C9 C2 114.5(5) . . ? C8 C9 C2 115.8(6) . . ? O4 C10 C11 128.6(6) . . ? O4 C10 C6 114.0(5) . . ? C11 C10 C6 117.4(6) . . ? C10 C11 C12 121.3(6) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? O5 C12 C11 127.6(6) . . ? O5 C12 C5 114.5(5) . . ? C11 C12 C5 117.8(6) . . ? O7 C13 C14 128.4(5) . . ? O7 C13 C3 113.2(5) . . ? C14 C13 C3 118.3(5) . . ? C15 C14 C13 120.2(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? O6 C15 C14 128.6(5) . . ? O6 C15 C4 112.9(6) . . ? C14 C15 C4 118.5(5) . . ? O12 C16 H16A 109.5 . . ? O12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C26 C17 O12 126.6(6) . . ? C26 C17 C18 120.7(6) . . ? O12 C17 C18 112.7(6) . . ? C19 C18 C17 120.5(6) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.8(6) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C25 120.1(5) . . ? C21 C20 C19 122.1(6) . . ? C25 C20 C19 117.8(5) . . ? C22 C21 C20 120.4(5) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 119.5(5) . . ? C21 C22 C27 120.2(5) . . ? C23 C22 C27 120.2(5) . . ? C24 C23 C22 120.4(6) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 121.6(6) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C26 122.0(6) . . ? C24 C25 C20 117.9(5) . . ? C26 C25 C20 120.1(6) . . ? C17 C26 C25 120.1(6) . . ? C17 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? N3 C27 N4 106.5(5) . . ? N3 C27 C22 127.5(5) . . ? N4 C27 C22 125.9(5) . . ? N4 C28 C30 105.4(5) . . ? N4 C28 C29 111.7(5) . . ? C30 C28 C29 109.9(5) . . ? N4 C28 C56 99.2(4) . . ? C30 C28 C56 114.3(5) . . ? C29 C28 C56 115.5(5) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C56 C31 H31A 109.5 . . ? C56 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C56 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C56 C32 H32A 109.5 . . ? C56 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C56 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O1 C33 H33A 109.5 . . ? O1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C42 C34 O1 125.4(6) . . ? C42 C34 C35 120.5(5) . . ? O1 C34 C35 114.1(6) . . ? C36 C35 C34 119.0(6) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 C37 122.0(6) . . ? C35 C36 H36 119.0 . . ? C37 C36 H36 119.0 . . ? C38 C37 C41 119.2(5) . . ? C38 C37 C36 123.0(5) . . ? C41 C37 C36 117.7(5) . . ? C68 C38 C37 120.8(5) . . ? C68 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C68 120.2(5) . . ? C40 C39 H39 119.9 . . ? C68 C39 H39 119.9 . . ? C39 C40 C41 122.2(5) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C40 C41 C42 122.7(5) . . ? C40 C41 C37 118.1(5) . . ? C42 C41 C37 119.2(5) . . ? C34 C42 C41 121.4(6) . . ? C34 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? N2 C43 N1 107.4(4) . . ? N2 C43 C68 126.6(5) . . ? N1 C43 C68 126.0(5) . . ? N1 C44 C48 110.0(5) . . ? N1 C44 C49 105.9(5) . . ? C48 C44 C49 110.7(5) . . ? N1 C44 C45 100.2(4) . . ? C48 C44 C45 114.8(5) . . ? C49 C44 C45 114.4(5) . . ? N2 C45 C47 106.3(5) . . ? N2 C45 C46 108.8(4) . . ? C47 C45 C46 112.4(5) . . ? N2 C45 C44 99.5(4) . . ? C47 C45 C44 114.3(5) . . ? C46 C45 C44 114.3(5) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N3 C56 C32 105.6(4) . . ? N3 C56 C31 110.9(4) . . ? C32 C56 C31 110.4(5) . . ? N3 C56 C28 99.5(4) . . ? C32 C56 C28 113.9(5) . . ? C31 C56 C28 115.4(5) . . ? C38 C68 C39 119.4(5) . . ? C38 C68 C43 120.4(5) . . ? C39 C68 C43 120.2(5) . . ? C17 O12 C16 116.1(6) . . ? O2 N1 C43 125.3(5) . . ? O2 N1 C44 122.0(4) . . ? C43 N1 C44 112.7(4) . . ? O3 N2 C43 126.4(4) . . ? O3 N2 C45 118.8(4) . . ? C43 N2 C45 113.5(4) . . ? O10 N3 C27 126.0(4) . . ? O10 N3 C56 120.9(4) . . ? C27 N3 C56 112.3(4) . . ? O11 N4 C27 125.3(5) . . ? O11 N4 C28 122.0(4) . . ? C27 N4 C28 112.4(4) . . ? C34 O1 C33 116.1(5) . . ? N2 O3 Tm1 140.0(3) . . ? C10 O4 Tm1 132.8(4) . . ? C12 O5 Tm1 134.9(4) . . ? C15 O6 Tm1 132.4(4) . . ? C13 O7 Tm1 135.0(4) . . ? C7 O8 Tm1 133.6(3) . . ? C9 O9 Tm1 133.9(3) . . ? N3 O10 Tm1 134.7(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.919 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.094 # Attachment '- complex-2.cif' data_shelxlb _database_code_depnum_ccdc_archive 'CCDC 783526' #TrackingRef '- complex-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H45 F18 Gd N4 O12' _chemical_formula_weight 1405.16 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.296(3) _cell_length_b 14.312(3) _cell_length_c 19.009(4) _cell_angle_alpha 100.89(3) _cell_angle_beta 103.92(3) _cell_angle_gamma 111.24(3) _cell_volume 2882.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26690 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.71 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1402 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23911 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10126 _reflns_number_gt 9474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Fluorine atoms in the CF3 groups and the carbon atoms in the naphthaline ring were treated by disorder and these atoms were refined anisotropically with application of restraints on interatomic distances and thermal parameters (DFIX, ISOR and SIMU instructions in SHELXL). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+3.3284P] 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 SHELXL _refine_ls_extinction_coef 0.0011(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10126 _refine_ls_number_parameters 898 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 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 Gd1 Gd 0.465868(14) 0.766747(12) 0.201554(8) 0.03399(8) Uani 1 1 d . A . C1 C -0.0108(5) 0.8450(5) -0.0179(3) 0.0798(16) Uani 1 1 d . . . H1A H -0.0454 0.8915 -0.0007 0.120 Uiso 1 1 calc R . . H1B H -0.0759 0.7755 -0.0439 0.120 Uiso 1 1 calc R . . H1C H 0.0307 0.8697 -0.0520 0.120 Uiso 1 1 calc R . . C2 C 0.0185(5) 0.8078(4) 0.1068(3) 0.0742(14) Uani 1 1 d . . . H2A H 0.0775 0.8058 0.1493 0.111 Uiso 1 1 calc R . . H2B H -0.0489 0.7391 0.0825 0.111 Uiso 1 1 calc R . . H2C H -0.0127 0.8571 0.1243 0.111 Uiso 1 1 calc R . . C3 C 0.0813(4) 0.8421(3) 0.0501(2) 0.0517(10) Uani 1 1 d . . . C4 C 0.1568(4) 0.7812(3) 0.0307(2) 0.0480(9) Uani 1 1 d . . . C5 C 0.1790(5) 0.7830(4) -0.0445(2) 0.0673(12) Uani 1 1 d . . . H5A H 0.2097 0.8541 -0.0465 0.101 Uiso 1 1 calc R . . H5B H 0.1025 0.7403 -0.0858 0.101 Uiso 1 1 calc R . . H5C H 0.2387 0.7557 -0.0486 0.101 Uiso 1 1 calc R . . C6 C 0.1119(5) 0.6708(4) 0.0371(3) 0.0701(13) Uani 1 1 d . . . H6A H 0.1643 0.6396 0.0240 0.105 Uiso 1 1 calc R . . H6B H 0.0282 0.6293 0.0030 0.105 Uiso 1 1 calc R . . H6C H 0.1146 0.6736 0.0884 0.105 Uiso 1 1 calc R . . C7 C 0.2942(4) 0.9491(3) 0.1170(2) 0.0468(9) Uani 1 1 d . . . C8 C 0.4110(5) 1.0396(4) 0.1630(3) 0.0682(14) Uani 1 1 d . . . C9 C 0.4177(7) 1.1216(4) 0.2176(3) 0.101(2) Uani 1 1 d D . . H9 H 0.3490 1.1266 0.2272 0.121 Uiso 1 1 calc R . . C10 C 0.5578(8) 1.2078(5) 0.2627(3) 0.097(2) Uani 1 1 d D . . C11 C 0.5518(10) 1.2735(9) 0.3156(7) 0.155(4) Uani 1 1 d U . . H11 H 0.4822 1.2743 0.3264 0.186 Uiso 1 1 calc R . . C12 C 0.6873(10) 1.3503(8) 0.3567(7) 0.163(4) Uani 1 1 d U . . H12 H 0.7021 1.4076 0.3962 0.196 Uiso 1 1 calc R . . C13 C 0.7946(9) 1.3462(6) 0.3428(6) 0.148(4) Uani 1 1 d . . . C14 C 1.0106(8) 1.4194(7) 0.4055(5) 0.138(3) Uani 1 1 d . . . H14A H 1.0043 1.3570 0.4194 0.207 Uiso 1 1 calc R . . H14B H 1.0757 1.4800 0.4453 0.207 Uiso 1 1 calc R . . H14C H 1.0290 1.4155 0.3591 0.207 Uiso 1 1 calc R . . C15 C 0.7856(9) 1.2725(7) 0.2878(5) 0.151(4) Uani 1 1 d DU . . H15 H 0.8537 1.2683 0.2768 0.181 Uiso 1 1 calc R . . C16 C 0.6458(6) 1.1893(6) 0.2404(4) 0.0883(17) Uani 1 1 d DU . . C17 C 0.6434(10) 1.1205(7) 0.1888(5) 0.131(3) Uani 1 1 d U . . H17 H 0.7118 1.1199 0.1763 0.157 Uiso 1 1 calc R . . C18 C 0.5199(5) 1.0430(5) 0.1519(4) 0.104(2) Uani 1 1 d . . . H18 H 0.5101 0.9855 0.1144 0.125 Uiso 1 1 calc R . . C19 C 0.5817(4) 0.7873(3) 0.0592(2) 0.0477(9) Uani 1 1 d . A . C20 C 0.6730(5) 0.8627(5) 0.0308(3) 0.0742(14) Uani 1 1 d DU . . F1 F 0.7848(17) 0.882(4) 0.0739(16) 0.165(11) Uani 0.49(5) 1 d P A 1 F2 F 0.670(4) 0.9503(16) 0.040(3) 0.135(9) Uani 0.49(5) 1 d P A 1 F3 F 0.667(3) 0.830(3) -0.0381(13) 0.142(11) Uani 0.49(5) 1 d P A 1 F1' F 0.7796(18) 0.9197(19) 0.0792(8) 0.117(8) Uani 0.51(5) 1 d P A 2 F2' F 0.624(3) 0.926(3) 0.009(2) 0.151(10) Uani 0.51(5) 1 d PD A 2 F3' F 0.687(3) 0.811(2) -0.0280(16) 0.130(8) Uani 0.51(5) 1 d P A 2 C21 C 0.4970(4) 0.6913(4) 0.0080(2) 0.0619(12) Uani 1 1 d . . . H21 H 0.4959 0.6767 -0.0421 0.074 Uiso 1 1 calc R A . C22 C 0.4132(4) 0.6157(3) 0.0281(2) 0.0518(10) Uani 1 1 d . A . C23 C 0.3275(6) 0.5091(5) -0.0329(3) 0.0860(18) Uani 1 1 d DU . . F4 F 0.2166(12) 0.4891(14) -0.0591(15) 0.110(7) Uani 0.44(3) 1 d P A 1 F5 F 0.264(4) 0.442(2) -0.0117(16) 0.26(2) Uani 0.44(3) 1 d P A 1 F6 F 0.371(3) 0.495(2) -0.0897(16) 0.174(13) Uani 0.44(3) 1 d P A 1 F4' F 0.245(2) 0.5287(18) -0.0814(13) 0.197(12) Uani 0.56(3) 1 d PD A 2 F5' F 0.3183(15) 0.4309(9) -0.0010(9) 0.128(6) Uani 0.56(3) 1 d PD A 2 F6' F 0.3778(15) 0.4701(14) -0.0737(10) 0.100(5) Uani 0.56(3) 1 d P A 2 C24 C 0.7409(4) 1.0715(4) 0.3999(3) 0.0631(12) Uani 1 1 d . . . C25 C 0.6139(4) 0.9943(3) 0.3424(2) 0.0466(9) Uani 1 1 d . A . C26 C 0.5122(4) 1.0008(3) 0.3580(2) 0.0565(11) Uani 1 1 d . . . H26 H 0.5248 1.0530 0.4005 0.068 Uiso 1 1 calc R . . C27 C 0.3925(4) 0.9318(3) 0.3121(2) 0.0489(9) Uani 1 1 d . A . C28 C 0.2858(5) 0.9459(5) 0.3340(3) 0.0744(14) Uani 1 1 d U . . F11 F 0.259(4) 0.898(4) 0.380(2) 0.171(12) Uani 0.48(3) 1 d P B 1 F12 F 0.3225(16) 1.0492(14) 0.3706(15) 0.122(7) Uani 0.48(3) 1 d P B 1 F10 F 0.1971(17) 0.931(3) 0.2795(9) 0.156(12) Uani 0.48(3) 1 d P B 1 F10' F 0.3156(12) 1.003(3) 0.4019(11) 0.160(13) Uani 0.52(3) 1 d P B 2 F11' F 0.225(2) 0.976(2) 0.2862(13) 0.137(9) Uani 0.52(3) 1 d P B 2 F12' F 0.1978(15) 0.8520(9) 0.3264(17) 0.113(6) Uani 0.52(3) 1 d P B 2 C29 C 0.4650(5) 0.7424(5) 0.4450(3) 0.0731(14) Uani 1 1 d . . . C30 C 0.4130(4) 0.7078(3) 0.3576(2) 0.0493(9) Uani 1 1 d . . . C31 C 0.2893(4) 0.6377(4) 0.3223(2) 0.0577(11) Uani 1 1 d . . . H31 H 0.2427 0.6117 0.3520 0.069 Uiso 1 1 calc R . . C32 C 0.2337(4) 0.6055(3) 0.2446(2) 0.0503(9) Uani 1 1 d . C . C33 C 0.0981(5) 0.5245(5) 0.2104(3) 0.0755(15) Uani 1 1 d DU . . F18 F 0.0531(12) 0.4812(18) 0.2546(6) 0.178(9) Uani 0.64(2) 1 d P C 1 F17 F 0.0881(9) 0.4471(10) 0.1524(9) 0.134(5) Uani 0.64(2) 1 d P C 1 F16 F 0.0309(11) 0.5656(13) 0.1797(11) 0.131(6) Uani 0.64(2) 1 d P C 1 F16' F 0.0813(12) 0.4336(10) 0.211(2) 0.123(12) Uani 0.36(2) 1 d P C 2 F17' F 0.0341(14) 0.5463(18) 0.2546(13) 0.136(11) Uani 0.36(2) 1 d PD C 2 F18' F 0.039(2) 0.520(3) 0.1452(15) 0.154(18) Uani 0.36(2) 1 d P C 2 C34 C 0.8580(5) 0.6815(5) 0.2494(3) 0.0799(16) Uani 1 1 d . . . H34A H 0.8360 0.6125 0.2552 0.120 Uiso 1 1 calc R . . H34B H 0.9458 0.7156 0.2598 0.120 Uiso 1 1 calc R . . H34C H 0.8150 0.6757 0.1983 0.120 Uiso 1 1 calc R . . C35 C 0.8217(3) 0.7463(3) 0.3052(2) 0.0472(9) Uani 1 1 d . . . C36 C 0.8559(5) 0.8548(4) 0.2973(3) 0.0767(15) Uani 1 1 d . . . H36A H 0.8214 0.8496 0.2450 0.115 Uiso 1 1 calc R . . H36B H 0.9446 0.8923 0.3140 0.115 Uiso 1 1 calc R . . H36C H 0.8238 0.8918 0.3279 0.115 Uiso 1 1 calc R . . C37 C 0.8710(6) 0.8329(4) 0.4469(3) 0.096(2) Uani 1 1 d . . . H37A H 0.7955 0.8411 0.4317 0.144 Uiso 1 1 calc R . . H37B H 0.9395 0.8962 0.4511 0.144 Uiso 1 1 calc R . . H37C H 0.8828 0.8197 0.4952 0.144 Uiso 1 1 calc R . . C38 C 0.9785(5) 0.7230(6) 0.4105(4) 0.097(2) Uani 1 1 d . . . H38A H 0.9921 0.7139 0.4601 0.145 Uiso 1 1 calc R . . H38B H 1.0483 0.7828 0.4116 0.145 Uiso 1 1 calc R . . H38C H 0.9688 0.6611 0.3745 0.145 Uiso 1 1 calc R . . C39 C 0.8634(4) 0.7404(4) 0.3874(3) 0.0594(11) Uani 1 1 d . . . C40 C 0.6509(3) 0.6212(3) 0.3227(2) 0.0433(8) Uani 1 1 d . . . C41 C 0.5303(3) 0.5341(3) 0.3038(2) 0.0425(8) Uani 1 1 d . . . C42 C 0.4882(4) 0.5045(3) 0.3601(2) 0.0491(9) Uani 1 1 d . . . H42 H 0.5354 0.5427 0.4107 0.059 Uiso 1 1 calc R . . C43 C 0.3753(4) 0.4174(3) 0.3427(2) 0.0452(9) Uani 1 1 d . . . C44 C 0.3300(5) 0.3864(4) 0.3997(3) 0.0723(14) Uani 1 1 d . . . H44 H 0.3743 0.4264 0.4504 0.087 Uiso 1 1 calc R . . C45 C 0.2241(5) 0.3001(5) 0.3826(3) 0.0805(16) Uani 1 1 d . . . H45 H 0.1957 0.2809 0.4212 0.097 Uiso 1 1 calc R . . C46 C 0.1555(4) 0.2382(4) 0.3055(3) 0.0649(12) Uani 1 1 d . . . C47 C -0.0232(6) 0.0871(5) 0.2216(4) 0.096(2) Uani 1 1 d . . . H47A H -0.0489 0.1277 0.1923 0.144 Uiso 1 1 calc R . . H47B H -0.0949 0.0311 0.2226 0.144 Uiso 1 1 calc R . . H47C H 0.0238 0.0579 0.1989 0.144 Uiso 1 1 calc R . . C48 C 0.1946(4) 0.2658(3) 0.2491(2) 0.0560(10) Uani 1 1 d . . . H48 H 0.1489 0.2247 0.1988 0.067 Uiso 1 1 calc R . . C49 C 0.3053(4) 0.3571(3) 0.2660(2) 0.0453(9) Uani 1 1 d . . . C50 C 0.3496(4) 0.3901(3) 0.2091(2) 0.0562(11) Uani 1 1 d . . . H50 H 0.3037 0.3521 0.1583 0.067 Uiso 1 1 calc R . . C51 C 0.4580(4) 0.4763(3) 0.2267(2) 0.0529(10) Uani 1 1 d . . . H51 H 0.4847 0.4973 0.1881 0.064 Uiso 1 1 calc R . . F7 F 0.8286(3) 1.0939(3) 0.3696(2) 0.1040(12) Uani 1 1 d . . . F8 F 0.7453(3) 1.1614(2) 0.4351(2) 0.1006(12) Uani 1 1 d . . . F9 F 0.7755(3) 1.0295(3) 0.4524(2) 0.1094(13) Uani 1 1 d . . . F13 F 0.5800(4) 0.7577(4) 0.47009(17) 0.1129(13) Uani 1 1 d . . . F14 F 0.4588(5) 0.8285(4) 0.47303(19) 0.152(2) Uani 1 1 d . . . F15 F 0.4069(5) 0.6720(4) 0.4740(2) 0.148(2) Uani 1 1 d . . . N1 N 0.1821(3) 0.9509(3) 0.0916(2) 0.0506(8) Uani 1 1 d . . . N2 N 0.2795(3) 0.8514(3) 0.09107(18) 0.0440(7) Uani 1 1 d . A . N3 N 0.7537(3) 0.6455(3) 0.3829(2) 0.0534(9) Uani 1 1 d . . . N4 N 0.6836(3) 0.6873(2) 0.28301(17) 0.0406(7) Uani 1 1 d . . . O1 O 0.7576(3) 0.6025(3) 0.43513(19) 0.0759(10) Uani 1 1 d . . . O2 O 0.6096(2) 0.6927(2) 0.22376(14) 0.0446(6) Uani 1 1 d . . . O3 O 0.0509(4) 0.1524(3) 0.2966(2) 0.0946(13) Uani 1 1 d . . . O4 O 0.4887(2) 0.7495(2) 0.32735(14) 0.0471(6) Uani 1 1 d . . . O5 O 0.2797(2) 0.6340(2) 0.19652(15) 0.0490(6) Uani 1 1 d . . . O6 O 0.3967(2) 0.6228(2) 0.08960(15) 0.0476(6) Uani 1 1 d . . . O7 O 0.5949(2) 0.8238(2) 0.12706(14) 0.0432(6) Uani 1 1 d . . . O8 O 0.3573(2) 0.8565(2) 0.25377(15) 0.0490(6) Uani 1 1 d . . . O9 O 0.6159(2) 0.9311(2) 0.28831(15) 0.0477(6) Uani 1 1 d . . . O10 O 0.3651(3) 0.8179(2) 0.10435(16) 0.0512(7) Uani 1 1 d . . . O11 O 0.1600(3) 1.0310(3) 0.1053(2) 0.0752(10) Uani 1 1 d . . . O12 O 0.9028(6) 1.4272(4) 0.3956(4) 0.171(3) 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 Gd1 0.03004(11) 0.03750(12) 0.02795(11) 0.00739(7) 0.00595(7) 0.01122(8) C1 0.060(3) 0.103(4) 0.076(3) 0.034(3) 0.002(3) 0.045(3) C2 0.062(3) 0.080(3) 0.081(3) 0.029(3) 0.034(3) 0.021(3) C3 0.041(2) 0.057(2) 0.055(2) 0.022(2) 0.0091(18) 0.0206(18) C4 0.043(2) 0.048(2) 0.046(2) 0.0164(17) 0.0027(17) 0.0171(17) C5 0.071(3) 0.075(3) 0.046(2) 0.012(2) 0.012(2) 0.028(3) C6 0.066(3) 0.054(3) 0.080(3) 0.026(2) 0.012(3) 0.021(2) C7 0.046(2) 0.048(2) 0.047(2) 0.0218(18) 0.0113(18) 0.0201(18) C8 0.069(3) 0.049(3) 0.066(3) 0.029(2) 0.002(2) 0.012(2) C9 0.125(5) 0.057(3) 0.074(4) 0.023(3) -0.003(4) 0.011(3) C10 0.171(7) 0.070(4) 0.066(3) 0.020(3) 0.029(4) 0.077(4) C11 0.173(7) 0.156(7) 0.197(8) 0.071(6) 0.076(6) 0.119(6) C12 0.118(6) 0.115(6) 0.193(8) 0.060(6) -0.027(5) 0.024(5) C13 0.117(7) 0.072(5) 0.173(9) 0.043(5) -0.035(6) 0.003(5) C14 0.104(6) 0.131(7) 0.122(7) 0.038(5) 0.006(5) 0.009(5) C15 0.153(7) 0.096(5) 0.124(6) 0.052(5) -0.015(5) -0.001(5) C16 0.094(4) 0.112(5) 0.098(4) 0.060(4) 0.049(3) 0.062(4) C17 0.167(7) 0.129(6) 0.129(6) 0.060(5) 0.077(5) 0.069(5) C18 0.044(3) 0.090(4) 0.145(6) 0.070(4) 0.001(3) -0.005(3) C19 0.042(2) 0.065(3) 0.042(2) 0.0224(19) 0.0169(17) 0.0253(19) C20 0.067(3) 0.090(4) 0.066(3) 0.030(3) 0.036(3) 0.022(3) F1 0.047(8) 0.26(3) 0.19(2) 0.108(18) 0.056(10) 0.042(13) F2 0.163(18) 0.083(8) 0.22(2) 0.080(12) 0.144(18) 0.048(11) F3 0.167(16) 0.157(19) 0.065(8) 0.051(10) 0.059(8) 0.010(11) F1' 0.075(11) 0.126(11) 0.071(8) 0.022(6) 0.023(6) -0.038(9) F2' 0.151(15) 0.19(2) 0.188(17) 0.159(18) 0.085(13) 0.084(15) F3' 0.140(13) 0.123(10) 0.131(17) 0.018(10) 0.118(14) 0.024(9) C21 0.060(3) 0.081(3) 0.035(2) 0.004(2) 0.019(2) 0.024(2) C22 0.041(2) 0.056(2) 0.043(2) -0.0048(18) 0.0068(18) 0.0180(18) C23 0.072(4) 0.081(4) 0.071(3) -0.021(3) 0.017(3) 0.022(3) F4 0.040(5) 0.070(10) 0.146(14) -0.040(8) -0.015(6) 0.009(5) F5 0.26(3) 0.13(2) 0.17(2) -0.080(14) 0.15(2) -0.126(18) F6 0.18(2) 0.133(17) 0.105(12) -0.063(11) 0.098(14) -0.027(12) F4' 0.128(13) 0.128(14) 0.188(17) -0.086(11) -0.094(12) 0.056(11) F5' 0.138(10) 0.051(6) 0.150(11) -0.014(5) 0.020(8) 0.031(7) F6' 0.092(7) 0.088(7) 0.092(8) -0.028(5) 0.016(6) 0.047(7) C24 0.053(3) 0.050(3) 0.060(3) -0.001(2) 0.004(2) 0.012(2) C25 0.044(2) 0.039(2) 0.040(2) 0.0041(16) 0.0056(17) 0.0084(16) C26 0.056(3) 0.057(2) 0.042(2) -0.0032(18) 0.0101(19) 0.023(2) C27 0.050(2) 0.051(2) 0.042(2) 0.0067(18) 0.0155(18) 0.0220(18) C28 0.065(3) 0.087(4) 0.066(3) 0.004(3) 0.027(3) 0.033(3) F11 0.16(2) 0.27(3) 0.20(3) 0.14(2) 0.15(2) 0.13(2) F12 0.106(8) 0.121(10) 0.126(13) -0.029(8) 0.044(9) 0.064(7) F10 0.065(7) 0.26(2) 0.084(10) -0.067(14) -0.024(7) 0.094(11) F10' 0.065(5) 0.25(2) 0.083(9) -0.068(13) 0.032(6) 0.031(11) F11' 0.140(15) 0.199(16) 0.19(2) 0.119(17) 0.100(15) 0.139(14) F12' 0.079(7) 0.107(8) 0.181(15) 0.051(9) 0.090(9) 0.036(6) C29 0.083(4) 0.096(4) 0.041(2) 0.019(3) 0.025(3) 0.036(3) C30 0.061(3) 0.059(2) 0.0340(19) 0.0157(18) 0.0181(19) 0.031(2) C31 0.056(3) 0.074(3) 0.049(2) 0.026(2) 0.027(2) 0.024(2) C32 0.045(2) 0.050(2) 0.054(2) 0.0195(19) 0.0188(19) 0.0154(18) C33 0.052(3) 0.082(4) 0.075(3) 0.033(3) 0.019(3) 0.006(3) F18 0.101(9) 0.216(18) 0.106(8) 0.092(11) 0.017(5) -0.060(10) F17 0.085(5) 0.099(7) 0.122(9) -0.009(6) 0.006(6) -0.025(5) F16 0.045(4) 0.169(10) 0.178(16) 0.082(10) 0.025(7) 0.040(6) F16' 0.062(7) 0.047(6) 0.22(3) 0.044(11) 0.013(13) 0.004(5) F17' 0.065(7) 0.127(14) 0.21(2) 0.020(12) 0.086(11) 0.026(8) F18' 0.058(12) 0.20(3) 0.101(14) 0.096(17) -0.026(9) -0.045(14) C34 0.050(3) 0.107(4) 0.067(3) 0.003(3) 0.017(2) 0.030(3) C35 0.0308(18) 0.055(2) 0.048(2) 0.0174(18) 0.0086(16) 0.0116(16) C36 0.052(3) 0.072(3) 0.089(4) 0.039(3) 0.013(3) 0.008(2) C37 0.113(5) 0.069(3) 0.062(3) 0.005(3) 0.028(3) 0.001(3) C38 0.042(3) 0.128(5) 0.102(5) 0.058(4) -0.001(3) 0.021(3) C39 0.041(2) 0.065(3) 0.051(2) 0.021(2) -0.0001(19) 0.0069(19) C40 0.0367(19) 0.047(2) 0.040(2) 0.0153(16) 0.0073(16) 0.0144(16) C41 0.040(2) 0.043(2) 0.0396(19) 0.0164(16) 0.0064(16) 0.0153(16) C42 0.048(2) 0.053(2) 0.0351(19) 0.0147(17) 0.0039(17) 0.0156(18) C43 0.046(2) 0.048(2) 0.0375(19) 0.0173(16) 0.0101(17) 0.0169(17) C44 0.071(3) 0.075(3) 0.042(2) 0.020(2) 0.013(2) 0.004(3) C45 0.077(3) 0.094(4) 0.053(3) 0.034(3) 0.028(3) 0.008(3) C46 0.056(3) 0.061(3) 0.061(3) 0.027(2) 0.015(2) 0.004(2) C47 0.079(4) 0.073(4) 0.092(4) 0.021(3) 0.023(3) -0.011(3) C48 0.054(2) 0.052(2) 0.045(2) 0.0115(18) 0.0113(19) 0.0098(19) C49 0.045(2) 0.044(2) 0.045(2) 0.0159(17) 0.0155(17) 0.0163(17) C50 0.057(3) 0.058(3) 0.035(2) 0.0091(18) 0.0127(19) 0.009(2) C51 0.048(2) 0.060(3) 0.039(2) 0.0153(18) 0.0138(18) 0.0106(19) F7 0.0498(17) 0.096(2) 0.103(3) -0.0149(19) 0.0177(17) -0.0086(16) F8 0.074(2) 0.0571(17) 0.110(3) -0.0313(17) -0.0053(18) 0.0140(15) F9 0.090(2) 0.092(2) 0.085(2) 0.0212(19) -0.0304(19) 0.0128(19) F13 0.093(3) 0.176(4) 0.0469(17) 0.025(2) 0.0009(17) 0.052(3) F14 0.248(6) 0.172(4) 0.0488(19) -0.008(2) 0.025(3) 0.141(4) F15 0.154(4) 0.189(5) 0.056(2) 0.060(3) 0.036(2) 0.015(3) N1 0.0514(19) 0.0514(19) 0.055(2) 0.0211(16) 0.0141(16) 0.0281(16) N2 0.0393(17) 0.0490(18) 0.0457(18) 0.0198(15) 0.0100(14) 0.0213(14) N3 0.0428(18) 0.058(2) 0.0485(19) 0.0249(16) 0.0021(15) 0.0134(16) N4 0.0310(15) 0.0486(17) 0.0373(16) 0.0151(13) 0.0060(13) 0.0144(13) O1 0.062(2) 0.086(2) 0.060(2) 0.0444(18) -0.0024(16) 0.0147(17) O2 0.0399(14) 0.0574(16) 0.0433(14) 0.0240(12) 0.0131(12) 0.0244(12) O3 0.077(2) 0.088(3) 0.076(2) 0.032(2) 0.024(2) -0.013(2) O4 0.0471(15) 0.0555(16) 0.0337(13) 0.0118(12) 0.0117(12) 0.0189(12) O5 0.0429(14) 0.0511(15) 0.0398(14) 0.0119(12) 0.0133(12) 0.0074(12) O6 0.0444(15) 0.0444(14) 0.0425(15) 0.0034(12) 0.0108(12) 0.0140(12) O7 0.0357(13) 0.0512(15) 0.0394(14) 0.0152(11) 0.0113(11) 0.0153(11) O8 0.0427(14) 0.0529(16) 0.0446(15) 0.0059(12) 0.0120(12) 0.0194(12) O9 0.0397(14) 0.0449(15) 0.0429(14) 0.0018(12) 0.0111(12) 0.0090(11) O10 0.0483(15) 0.0672(18) 0.0500(16) 0.0249(14) 0.0142(13) 0.0355(14) O11 0.085(2) 0.066(2) 0.098(3) 0.0330(19) 0.034(2) 0.0513(19) O12 0.100(4) 0.084(3) 0.215(7) -0.001(4) -0.051(4) 0.005(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 Gd1 O5 2.352(3) . ? Gd1 O10 2.357(3) . ? Gd1 O9 2.363(3) . ? Gd1 O2 2.365(3) . ? Gd1 O6 2.387(3) . ? Gd1 O7 2.402(3) . ? Gd1 O4 2.410(3) . ? Gd1 O8 2.411(3) . ? C1 C3 1.517(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.526(6) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 N1 1.500(5) . ? C3 C4 1.544(6) . ? C4 N2 1.496(5) . ? C4 C6 1.513(6) . ? C4 C5 1.521(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 N2 1.320(5) . ? C7 N1 1.359(5) . ? C7 C8 1.457(6) . ? C8 C9 1.375(9) . ? C8 C18 1.391(9) . ? C9 C10 1.604(9) . ? C9 H9 0.9300 . ? C10 C11 1.278(12) . ? C10 C16 1.343(9) . ? C11 C12 1.522(13) . ? C11 H11 0.9300 . ? C12 C13 1.426(16) . ? C12 H12 0.9300 . ? C13 C15 1.288(15) . ? C13 O12 1.386(9) . ? C14 O12 1.343(10) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.598(10) . ? C15 H15 0.9300 . ? C16 C17 1.238(10) . ? C17 C18 1.414(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 O7 1.244(5) . ? C19 C21 1.375(6) . ? C19 C20 1.533(6) . ? C20 F2 1.246(19) . ? C20 F1' 1.262(16) . ? C20 F3 1.28(2) . ? C20 F3' 1.301(19) . ? C20 F1 1.32(2) . ? C20 F2' 1.340(10) . ? C21 C22 1.384(6) . ? C21 H21 0.9300 . ? C22 O6 1.227(5) . ? C22 C23 1.537(6) . ? C23 F5 1.21(2) . ? C23 F4 1.236(18) . ? C23 F6' 1.270(15) . ? C23 F6 1.33(2) . ? C23 F4' 1.347(10) . ? C23 F5' 1.353(9) . ? C24 F8 1.308(5) . ? C24 F7 1.309(6) . ? C24 F9 1.323(6) . ? C24 C25 1.525(6) . ? C25 O9 1.247(5) . ? C25 C26 1.382(6) . ? C26 C27 1.381(6) . ? C26 H26 0.9300 . ? C27 O8 1.248(5) . ? C27 C28 1.536(6) . ? C28 F10 1.231(16) . ? C28 F11 1.250(15) . ? C28 F10' 1.278(13) . ? C28 F11' 1.281(16) . ? C28 F12' 1.341(12) . ? C28 F12 1.360(15) . ? C29 F14 1.283(7) . ? C29 F13 1.298(6) . ? C29 F15 1.308(6) . ? C29 C30 1.537(6) . ? C30 O4 1.240(5) . ? C30 C31 1.385(6) . ? C31 C32 1.376(6) . ? C31 H31 0.9300 . ? C32 O5 1.243(5) . ? C32 C33 1.530(6) . ? C33 F16' 1.241(13) . ? C33 F18 1.252(9) . ? C33 F18' 1.252(19) . ? C33 F16 1.271(14) . ? C33 F17' 1.350(9) . ? C33 F17 1.354(11) . ? C34 C35 1.530(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.501(6) . ? C35 N4 1.502(5) . ? C35 C39 1.552(6) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C39 1.529(8) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.502(7) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N3 1.499(5) . ? C40 N4 1.330(5) . ? C40 N3 1.364(5) . ? C40 C41 1.455(5) . ? C41 C42 1.369(5) . ? C41 C51 1.415(5) . ? C42 C43 1.399(5) . ? C42 H42 0.9300 . ? C43 C44 1.405(6) . ? C43 C49 1.412(5) . ? C44 C45 1.345(7) . ? C44 H44 0.9300 . ? C45 C46 1.421(7) . ? C45 H45 0.9300 . ? C46 C48 1.344(6) . ? C46 O3 1.365(5) . ? C47 O3 1.411(7) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.417(6) . ? C48 H48 0.9300 . ? C49 C50 1.405(6) . ? C50 C51 1.359(6) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? N1 O11 1.265(4) . ? N2 O10 1.297(4) . ? N3 O1 1.264(4) . ? N4 O2 1.300(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Gd1 O10 93.30(10) . . ? O5 Gd1 O9 136.70(9) . . ? O10 Gd1 O9 101.81(11) . . ? O5 Gd1 O2 103.82(10) . . ? O10 Gd1 O2 139.04(9) . . ? O9 Gd1 O2 90.82(10) . . ? O5 Gd1 O6 71.53(10) . . ? O10 Gd1 O6 76.20(10) . . ? O9 Gd1 O6 151.43(10) . . ? O2 Gd1 O6 74.57(10) . . ? O5 Gd1 O7 143.04(9) . . ? O10 Gd1 O7 69.77(9) . . ? O9 Gd1 O7 79.97(9) . . ? O2 Gd1 O7 74.48(9) . . ? O6 Gd1 O7 72.57(9) . . ? O5 Gd1 O4 71.87(10) . . ? O10 Gd1 O4 146.05(10) . . ? O9 Gd1 O4 73.18(10) . . ? O2 Gd1 O4 74.89(9) . . ? O6 Gd1 O4 124.05(10) . . ? O7 Gd1 O4 138.51(9) . . ? O5 Gd1 O8 74.02(10) . . ? O10 Gd1 O8 72.54(10) . . ? O9 Gd1 O8 72.41(9) . . ? O2 Gd1 O8 147.82(9) . . ? O6 Gd1 O8 131.31(9) . . ? O7 Gd1 O8 126.72(9) . . ? O4 Gd1 O8 74.02(10) . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C1 109.6(4) . . ? N1 C3 C2 106.0(4) . . ? C1 C3 C2 110.2(4) . . ? N1 C3 C4 101.4(3) . . ? C1 C3 C4 115.4(4) . . ? C2 C3 C4 113.3(4) . . ? N2 C4 C6 110.4(3) . . ? N2 C4 C5 105.5(3) . . ? C6 C4 C5 111.1(4) . . ? N2 C4 C3 99.4(3) . . ? C6 C4 C3 115.6(4) . . ? C5 C4 C3 113.7(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 N1 108.1(3) . . ? N2 C7 C8 125.9(4) . . ? N1 C7 C8 126.0(4) . . ? C9 C8 C18 118.6(6) . . ? C9 C8 C7 122.4(6) . . ? C18 C8 C7 119.0(5) . . ? C8 C9 C10 112.1(7) . . ? C8 C9 H9 123.9 . . ? C10 C9 H9 123.9 . . ? C11 C10 C16 137.9(9) . . ? C11 C10 C9 105.7(8) . . ? C16 C10 C9 116.2(6) . . ? C10 C11 C12 102.5(9) . . ? C10 C11 H11 128.8 . . ? C12 C11 H11 128.8 . . ? C13 C12 C11 128.9(11) . . ? C13 C12 H12 115.6 . . ? C11 C12 H12 115.6 . . ? C15 C13 O12 127.0(12) . . ? C15 C13 C12 121.3(9) . . ? O12 C13 C12 111.7(11) . . ? O12 C14 H14A 109.5 . . ? O12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 C16 113.2(10) . . ? C13 C15 H15 123.4 . . ? C16 C15 H15 123.4 . . ? C17 C16 C10 133.8(9) . . ? C17 C16 C15 110.1(8) . . ? C10 C16 C15 116.1(8) . . ? C16 C17 C18 109.1(9) . . ? C16 C17 H17 125.5 . . ? C18 C17 H17 125.5 . . ? C8 C18 C17 130.0(8) . . ? C8 C18 H18 115.0 . . ? C17 C18 H18 115.0 . . ? O7 C19 C21 128.8(4) . . ? O7 C19 C20 113.6(4) . . ? C21 C19 C20 117.5(4) . . ? F2 C20 F1' 80.5(18) . . ? F2 C20 F3 107.0(18) . . ? F1' C20 F3 116.6(16) . . ? F2 C20 F3' 125.1(15) . . ? F1' C20 F3' 107.5(14) . . ? F3 C20 F3' 20(2) . . ? F2 C20 F1 105.3(16) . . ? F1' C20 F1 25(2) . . ? F3 C20 F1 106.1(17) . . ? F3' C20 F1 91.0(17) . . ? F2 C20 F2' 28.5(19) . . ? F1' C20 F2' 107.9(15) . . ? F3 C20 F2' 87.7(17) . . ? F3' C20 F2' 108.0(16) . . ? F1 C20 F2' 132.1(17) . . ? F2 C20 C19 113.9(9) . . ? F1' C20 C19 115.3(8) . . ? F3 C20 C19 117.3(14) . . ? F3' C20 C19 110.6(13) . . ? F1 C20 C19 106.2(14) . . ? F2' C20 C19 107.2(12) . . ? C19 C21 C22 122.5(4) . . ? C19 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? O6 C22 C21 128.0(4) . . ? O6 C22 C23 114.1(4) . . ? C21 C22 C23 117.9(4) . . ? F5 C23 F4 68(3) . . ? F5 C23 F6' 109(2) . . ? F4 C23 F6' 120.0(14) . . ? F5 C23 F6 127(2) . . ? F4 C23 F6 109.3(18) . . ? F6' C23 F6 23(2) . . ? F5 C23 F4' 104(4) . . ? F4 C23 F4' 35.8(15) . . ? F6' C23 F4' 105.2(15) . . ? F6 C23 F4' 85.3(16) . . ? F5 C23 F5' 32(3) . . ? F4 C23 F5' 99.6(16) . . ? F6' C23 F5' 86.6(13) . . ? F6 C23 F5' 109(2) . . ? F4' C23 F5' 133.8(18) . . ? F5 C23 C22 116.2(11) . . ? F4 C23 C22 117.4(9) . . ? F6' C23 C22 116.1(9) . . ? F6 C23 C22 111.1(13) . . ? F4' C23 C22 104.9(10) . . ? F5' C23 C22 109.3(8) . . ? F8 C24 F7 106.7(4) . . ? F8 C24 F9 107.3(4) . . ? F7 C24 F9 105.0(5) . . ? F8 C24 C25 114.2(4) . . ? F7 C24 C25 113.1(4) . . ? F9 C24 C25 110.0(4) . . ? O9 C25 C26 128.5(4) . . ? O9 C25 C24 114.9(4) . . ? C26 C25 C24 116.6(4) . . ? C27 C26 C25 121.8(4) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? O8 C27 C26 128.4(4) . . ? O8 C27 C28 113.8(4) . . ? C26 C27 C28 117.8(4) . . ? F10 C28 F11 115.4(16) . . ? F10 C28 F10' 125.5(14) . . ? F11 C28 F10' 64.1(12) . . ? F10 C28 F11' 26.6(15) . . ? F11 C28 F11' 133.1(14) . . ? F10' C28 F11' 110.6(16) . . ? F10 C28 F12' 75.2(13) . . ? F11 C28 F12' 46.9(15) . . ? F10' C28 F12' 106.6(12) . . ? F11' C28 F12' 100.6(11) . . ? F10 C28 F12 100.0(13) . . ? F11 C28 F12 105.7(14) . . ? F10' C28 F12 42.5(13) . . ? F11' C28 F12 75.9(11) . . ? F12' C28 F12 138.4(9) . . ? F10 C28 C27 114.3(9) . . ? F11 C28 C27 110.9(9) . . ? F10' C28 C27 115.5(8) . . ? F11' C28 C27 112.4(10) . . ? F12' C28 C27 109.9(6) . . ? F12 C28 C27 109.5(9) . . ? F14 C29 F13 108.0(5) . . ? F14 C29 F15 108.3(5) . . ? F13 C29 F15 104.7(5) . . ? F14 C29 C30 110.4(5) . . ? F13 C29 C30 112.0(4) . . ? F15 C29 C30 113.1(5) . . ? O4 C30 C31 127.9(4) . . ? O4 C30 C29 114.4(4) . . ? C31 C30 C29 117.7(4) . . ? C32 C31 C30 121.7(4) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? O5 C32 C31 128.1(4) . . ? O5 C32 C33 113.8(4) . . ? C31 C32 C33 118.1(4) . . ? F16' C33 F18 56.2(11) . . ? F16' C33 F18' 108.0(16) . . ? F18 C33 F18' 126.2(10) . . ? F16' C33 F16 134.8(10) . . ? F18 C33 F16 109.7(12) . . ? F18' C33 F16 41.1(19) . . ? F16' C33 F17' 101.7(13) . . ? F18 C33 F17' 46.9(9) . . ? F18' C33 F17' 104.8(19) . . ? F16 C33 F17' 69.5(12) . . ? F16' C33 F17 53.6(14) . . ? F18 C33 F17 107.1(10) . . ? F18' C33 F17 64.4(18) . . ? F16 C33 F17 105.1(9) . . ? F17' C33 F17 141.1(9) . . ? F16' C33 C32 114.5(8) . . ? F18 C33 C32 116.2(6) . . ? F18' C33 C32 116.7(9) . . ? F16 C33 C32 110.0(8) . . ? F17' C33 C32 109.8(9) . . ? F17 C33 C32 108.1(6) . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N4 110.7(3) . . ? C36 C35 C34 110.3(4) . . ? N4 C35 C34 105.0(3) . . ? C36 C35 C39 116.1(4) . . ? N4 C35 C39 100.4(3) . . ? C34 C35 C39 113.3(4) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 H37A 109.5 . . ? C39 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C39 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N3 C39 C38 109.6(4) . . ? N3 C39 C37 106.4(4) . . ? C38 C39 C37 111.0(5) . . ? N3 C39 C35 100.4(3) . . ? C38 C39 C35 115.9(4) . . ? C37 C39 C35 112.6(4) . . ? N4 C40 N3 107.5(3) . . ? N4 C40 C41 126.9(3) . . ? N3 C40 C41 125.5(3) . . ? C42 C41 C51 119.5(4) . . ? C42 C41 C40 120.5(3) . . ? C51 C41 C40 120.0(4) . . ? C41 C42 C43 121.0(4) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C42 C43 C44 121.8(4) . . ? C42 C43 C49 119.6(4) . . ? C44 C43 C49 118.5(4) . . ? C45 C44 C43 121.4(4) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C44 C45 C46 119.9(4) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C48 C46 O3 125.8(4) . . ? C48 C46 C45 120.7(4) . . ? O3 C46 C45 113.5(4) . . ? O3 C47 H47A 109.5 . . ? O3 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O3 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 C49 120.2(4) . . ? C46 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C50 C49 C43 118.2(4) . . ? C50 C49 C48 122.5(4) . . ? C43 C49 C48 119.3(4) . . ? C51 C50 C49 121.6(4) . . ? C51 C50 H50 119.2 . . ? C49 C50 H50 119.2 . . ? C50 C51 C41 120.0(4) . . ? C50 C51 H51 120.0 . . ? C41 C51 H51 120.0 . . ? O11 N1 C7 126.0(4) . . ? O11 N1 C3 122.5(3) . . ? C7 N1 C3 111.2(3) . . ? O10 N2 C7 126.3(3) . . ? O10 N2 C4 119.3(3) . . ? C7 N2 C4 113.5(3) . . ? O1 N3 C40 125.9(3) . . ? O1 N3 C39 121.1(3) . . ? C40 N3 C39 112.6(3) . . ? O2 N4 C40 125.9(3) . . ? O2 N4 C35 120.7(3) . . ? C40 N4 C35 112.7(3) . . ? N4 O2 Gd1 136.3(2) . . ? C46 O3 C47 117.2(4) . . ? C30 O4 Gd1 132.8(3) . . ? C32 O5 Gd1 135.0(3) . . ? C22 O6 Gd1 133.5(3) . . ? C19 O7 Gd1 131.7(3) . . ? C27 O8 Gd1 131.9(3) . . ? C25 O9 Gd1 133.0(3) . . ? N2 O10 Gd1 138.1(2) . . ? C14 O12 C13 119.6(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.440 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.073 # Attachment '- complex-4.cif' data_shelxld _database_code_depnum_ccdc_archive 'CCDC 819316' #TrackingRef '- complex-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H45 Dy F18 N4 O12' _chemical_formula_weight 1410.41 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' Dy Dy -0.1892 4.4098 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.237(2) _cell_length_b 14.223(3) _cell_length_c 18.868(4) _cell_angle_alpha 100.82(3) _cell_angle_beta 104.15(3) _cell_angle_gamma 111.08(3) _cell_volume 2829.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18469 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.71 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1406 _exptl_absorpt_coefficient_mu 1.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.757 _exptl_absorpt_correction_T_max 0.817 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16457 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9892 _reflns_number_gt 8726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Fluorine atoms in the CF3 groups and the carbon atoms in the naphthaline ring were treated by disorder and these atoms were refined anisotropically with application of restraints on interatomic distances and thermal parameters (DFIX and ISOR instructions in SHELXL). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+2.8374P] 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 9892 _refine_ls_number_parameters 841 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7411(6) 1.0712(5) 0.3987(4) 0.0590(17) Uani 1 1 d . . . C2 C 0.2860(7) 0.9448(6) 0.3344(5) 0.071(2) Uani 1 1 d D . . C3 C 0.4672(7) 0.7443(7) 0.4446(4) 0.070(2) Uani 1 1 d . . . C4 C 0.1007(7) 0.5261(7) 0.2096(5) 0.069(2) Uani 1 1 d D . . C5 C 0.6736(7) 0.8627(7) 0.0330(4) 0.070(2) Uani 1 1 d . . . C6 C 0.3303(8) 0.5134(7) -0.0328(5) 0.082(2) Uani 1 1 d . . . C7 C 0.0811(5) 0.8422(5) 0.0500(3) 0.0498(14) Uani 1 1 d . . . C8 C -0.0117(7) 0.8439(7) -0.0187(4) 0.081(2) Uani 1 1 d . . . H8A H -0.0509 0.8870 -0.0016 0.121 Uiso 1 1 calc R . . H8B H -0.0739 0.7731 -0.0463 0.121 Uiso 1 1 calc R . . H8C H 0.0305 0.8726 -0.0516 0.121 Uiso 1 1 calc R . . C9 C 0.0183(6) 0.8087(6) 0.1070(4) 0.071(2) Uani 1 1 d . . . H9A H 0.0789 0.8115 0.1516 0.106 Uiso 1 1 calc R . . H9B H -0.0458 0.7377 0.0837 0.106 Uiso 1 1 calc R . . H9C H -0.0180 0.8556 0.1216 0.106 Uiso 1 1 calc R . . C10 C 0.1569(5) 0.7810(4) 0.0307(3) 0.0426(13) Uani 1 1 d . . . C11 C 0.1121(6) 0.6706(5) 0.0375(4) 0.0645(18) Uani 1 1 d . . . H11A H 0.1657 0.6394 0.0255 0.097 Uiso 1 1 calc R . . H11B H 0.0286 0.6285 0.0024 0.097 Uiso 1 1 calc R . . H11C H 0.1135 0.6735 0.0890 0.097 Uiso 1 1 calc R . . C12 C 0.1790(6) 0.7821(6) -0.0449(3) 0.0627(17) Uani 1 1 d . . . H12A H 0.2059 0.8529 -0.0483 0.094 Uiso 1 1 calc R . . H12B H 0.1030 0.7364 -0.0866 0.094 Uiso 1 1 calc R . . H12C H 0.2419 0.7578 -0.0476 0.094 Uiso 1 1 calc R . . C13 C 0.8202(5) 0.7462(4) 0.3039(3) 0.0429(13) Uani 1 1 d . . . C14 C 0.8541(6) 0.8549(6) 0.2963(4) 0.073(2) Uani 1 1 d . . . H14A H 0.8191 0.8499 0.2436 0.110 Uiso 1 1 calc R . . H14B H 0.9431 0.8926 0.3131 0.110 Uiso 1 1 calc R . . H14C H 0.8219 0.8918 0.3273 0.110 Uiso 1 1 calc R . . C15 C 0.8561(6) 0.6808(7) 0.2477(4) 0.078(2) Uani 1 1 d . . . H15A H 0.8439 0.6148 0.2579 0.117 Uiso 1 1 calc R . . H15B H 0.9420 0.7191 0.2537 0.117 Uiso 1 1 calc R . . H15C H 0.8048 0.6673 0.1961 0.117 Uiso 1 1 calc R . . C16 C 0.8627(5) 0.7398(5) 0.3858(4) 0.0596(17) Uani 1 1 d . . . C17 C 0.9795(6) 0.7224(7) 0.4094(5) 0.092(3) Uani 1 1 d . . . H17A H 0.9931 0.7128 0.4593 0.138 Uiso 1 1 calc R . . H17B H 1.0495 0.7829 0.4110 0.138 Uiso 1 1 calc R . . H17C H 0.9702 0.6606 0.3730 0.138 Uiso 1 1 calc R . . C18 C 0.8705(8) 0.8325(6) 0.4460(4) 0.092(3) Uani 1 1 d . . . H18A H 0.7935 0.8394 0.4317 0.139 Uiso 1 1 calc R . . H18B H 0.9375 0.8965 0.4492 0.139 Uiso 1 1 calc R . . H18C H 0.8855 0.8200 0.4950 0.139 Uiso 1 1 calc R . . C19 C 0.6509(5) 0.6214(4) 0.3218(3) 0.0409(12) Uani 1 1 d . . . C20 C 0.5310(5) 0.5355(4) 0.3033(3) 0.0417(13) Uani 1 1 d . . . C21 C 0.4566(5) 0.4772(5) 0.2260(3) 0.0481(14) Uani 1 1 d . . . H21 H 0.4822 0.4983 0.1867 0.058 Uiso 1 1 calc R . . C22 C 0.3488(6) 0.3912(5) 0.2086(3) 0.0542(16) Uani 1 1 d . . . H22 H 0.3025 0.3529 0.1574 0.065 Uiso 1 1 calc R . . C23 C 0.3047(5) 0.3582(4) 0.2656(3) 0.0409(12) Uani 1 1 d . . . C24 C 0.3765(5) 0.4186(4) 0.3432(3) 0.0428(13) Uani 1 1 d . . . C25 C 0.4893(5) 0.5053(4) 0.3600(3) 0.0451(13) Uani 1 1 d . . . H25 H 0.5374 0.5435 0.4110 0.054 Uiso 1 1 calc R . . C26 C 0.3327(6) 0.3879(6) 0.4005(4) 0.069(2) Uani 1 1 d . . . H26 H 0.3780 0.4276 0.4516 0.083 Uiso 1 1 calc R . . C27 C 0.2251(7) 0.3011(6) 0.3828(4) 0.078(2) Uani 1 1 d . . . H27 H 0.1969 0.2819 0.4217 0.093 Uiso 1 1 calc R . . C28 C 0.1571(6) 0.2410(5) 0.3072(4) 0.0624(18) Uani 1 1 d . . . C29 C 0.1950(5) 0.2682(5) 0.2490(3) 0.0530(15) Uani 1 1 d . . . H29 H 0.1480 0.2271 0.1984 0.064 Uiso 1 1 calc R . . C30 C -0.0221(7) 0.0888(6) 0.2231(5) 0.092(3) Uani 1 1 d . . . H30A H -0.0429 0.1304 0.1922 0.139 Uiso 1 1 calc R . . H30B H -0.0970 0.0363 0.2242 0.139 Uiso 1 1 calc R . . H30C H 0.0224 0.0546 0.2016 0.139 Uiso 1 1 calc R . . C31 C 0.4146(5) 0.7098(5) 0.3576(3) 0.0451(13) Uani 1 1 d . A . C32 C 0.2918(5) 0.6390(5) 0.3224(3) 0.0526(15) Uani 1 1 d . . . H32 H 0.2456 0.6121 0.3522 0.063 Uiso 1 1 calc R B . C33 C 0.2362(5) 0.6073(4) 0.2446(3) 0.0470(14) Uani 1 1 d . A . C34 C 0.3925(5) 0.9305(5) 0.3118(3) 0.0443(13) Uani 1 1 d . A . C35 C 0.5123(5) 1.0002(5) 0.3574(3) 0.0520(15) Uani 1 1 d . . . H35 H 0.5252 1.0531 0.4001 0.062 Uiso 1 1 calc R A . C36 C 0.6136(5) 0.9936(4) 0.3414(3) 0.0425(13) Uani 1 1 d . A . C37 C 0.5825(5) 0.7895(5) 0.0609(3) 0.0438(13) Uani 1 1 d . A . C38 C 0.4991(6) 0.6926(5) 0.0094(3) 0.0551(16) Uani 1 1 d . . . H38 H 0.4999 0.6771 -0.0406 0.066 Uiso 1 1 calc R . . C39 C 0.4147(5) 0.6178(5) 0.0292(3) 0.0481(14) Uani 1 1 d . A . C41 C 0.2935(5) 0.9490(5) 0.1177(3) 0.0446(13) Uani 1 1 d . . . C43 C 0.4101(6) 1.0391(5) 0.1629(4) 0.0615(18) Uani 1 1 d D . . C44 C 0.5200(7) 1.0433(7) 0.1523(5) 0.089(3) Uani 1 1 d DU . . H44 H 0.5119 0.9852 0.1156 0.107 Uiso 1 1 calc R . . C45 C 0.6389(12) 1.1218(9) 0.1885(7) 0.124(4) Uani 1 1 d U . . H45 H 0.7063 1.1213 0.1741 0.149 Uiso 1 1 calc R . . C46 C 0.6487(8) 1.1949(8) 0.2433(6) 0.092(3) Uani 1 1 d DU . . C47 C 0.5472(8) 1.2039(6) 0.2610(5) 0.092(3) Uani 1 1 d DU . . C48 C 0.4182(8) 1.1233(7) 0.2190(5) 0.095(3) Uani 1 1 d DU . . H48 H 0.3492 1.1281 0.2290 0.114 Uiso 1 1 calc R . . C49 C 0.5573(12) 1.2778(11) 0.3188(8) 0.153(5) Uani 1 1 d DU . . H49 H 0.4906 1.2818 0.3324 0.183 Uiso 1 1 calc R . . C50 C 0.6832(13) 1.3507(10) 0.3577(9) 0.158(5) Uani 1 1 d DU . . H50 H 0.6984 1.4083 0.3977 0.190 Uiso 1 1 calc R . . C51 C 0.7911(12) 1.3449(10) 0.3418(8) 0.130(4) Uani 1 1 d U . . C52 C 0.7799(11) 1.2717(11) 0.2853(8) 0.157(5) Uani 1 1 d DU . . H52 H 0.8469 1.2674 0.2722 0.189 Uiso 1 1 calc R . . C53 C 1.0099(10) 1.4200(9) 0.4041(6) 0.126(4) Uani 1 1 d . . . H53A H 1.0069 1.3604 0.4218 0.189 Uiso 1 1 calc R . . H53B H 1.0778 1.4832 0.4405 0.189 Uiso 1 1 calc R . . H53C H 1.0216 1.4100 0.3553 0.189 Uiso 1 1 calc R . . Dy Dy 0.46588(2) 0.767606(18) 0.201660(12) 0.03093(9) Uani 1 1 d . A . F1 F 0.8275(4) 1.0930(4) 0.3672(3) 0.0999(16) Uani 1 1 d . . . F2 F 0.7763(4) 1.0297(4) 0.4516(3) 0.1053(17) Uani 1 1 d . . . F3 F 0.7451(4) 1.1605(3) 0.4339(3) 0.0945(15) Uani 1 1 d . . . F4 F 0.3180(16) 0.999(4) 0.4045(14) 0.158(17) Uani 0.51(4) 1 d P A 1 F5 F 0.225(3) 0.977(3) 0.288(2) 0.143(13) Uani 0.51(4) 1 d P A 1 F6 F 0.197(2) 0.8504(9) 0.325(2) 0.102(8) Uani 0.51(4) 1 d PD A 1 F7 F 0.4610(7) 0.8298(5) 0.4732(3) 0.141(3) Uani 1 1 d . . . F8 F 0.5825(5) 0.7592(5) 0.4701(2) 0.1101(18) Uani 1 1 d . . . F9 F 0.4098(6) 0.6740(5) 0.4743(3) 0.141(3) Uani 1 1 d . . . F10 F 0.0327(14) 0.5689(15) 0.1807(12) 0.134(8) Uani 0.69(3) 1 d P B 1 F11 F 0.0557(16) 0.479(2) 0.2534(8) 0.186(11) Uani 0.69(3) 1 d P B 1 F12 F 0.0879(10) 0.4513(14) 0.1500(10) 0.129(6) Uani 0.69(3) 1 d P B 1 F13 F 0.7847(5) 0.9070(6) 0.0804(3) 0.152(3) Uani 1 1 d . . . F14 F 0.6783(6) 0.8221(5) -0.0319(3) 0.142(3) Uani 1 1 d . . . F15 F 0.6471(7) 0.9411(6) 0.0254(5) 0.167(3) Uani 1 1 d . . . F16 F 0.3803(5) 0.4810(4) -0.0784(3) 0.128(2) Uani 1 1 d . . . F17 F 0.2286(6) 0.5068(6) -0.0661(5) 0.213(5) Uani 1 1 d . . . F18 F 0.3054(8) 0.4345(5) -0.0019(4) 0.170(3) Uani 1 1 d . . . F4' F 0.3189(18) 1.0458(12) 0.371(2) 0.115(8) Uani 0.49(4) 1 d PD A 2 F5' F 0.198(2) 0.931(4) 0.2784(11) 0.154(17) Uani 0.49(4) 1 d P A 2 F6' F 0.260(5) 0.896(5) 0.381(3) 0.163(16) Uani 0.49(4) 1 d P A 2 F10' F 0.039(3) 0.523(4) 0.145(2) 0.14(2) Uani 0.31(3) 1 d P B 2 F11' F 0.0383(19) 0.548(2) 0.2545(17) 0.124(14) Uani 0.31(3) 1 d PD B 2 F12' F 0.0838(16) 0.4359(14) 0.209(3) 0.116(18) Uani 0.31(3) 1 d P B 2 N1 N 0.1814(4) 0.9503(4) 0.0912(3) 0.0491(12) Uani 1 1 d . . . N2 N 0.2801(4) 0.8515(4) 0.0916(2) 0.0392(10) Uani 1 1 d . . . N3 N 0.6824(4) 0.6884(3) 0.2825(2) 0.0387(10) Uani 1 1 d . . . N4 N 0.7542(4) 0.6450(4) 0.3816(3) 0.0500(12) Uani 1 1 d . . . O1 O 0.1590(5) 1.0303(4) 0.1055(3) 0.0775(14) Uani 1 1 d . . . O2 O 0.3658(3) 0.8184(3) 0.1049(2) 0.0464(9) Uani 1 1 d . . . O3 O 0.6080(3) 0.6939(3) 0.2232(2) 0.0389(8) Uani 1 1 d . . . O4 O 0.7583(4) 0.6025(4) 0.4341(3) 0.0761(15) Uani 1 1 d . . . O5 O 0.0526(5) 0.1543(4) 0.2976(3) 0.0897(18) Uani 1 1 d . . . O6 O 0.9011(8) 1.4292(6) 0.3969(5) 0.146(3) Uani 1 1 d U . . O7 O 0.6148(3) 0.9299(3) 0.2869(2) 0.0421(9) Uani 1 1 d . . . O8 O 0.3574(3) 0.8553(3) 0.2536(2) 0.0437(9) Uani 1 1 d . . . O9 O 0.5942(3) 0.8257(3) 0.12865(19) 0.0397(8) Uani 1 1 d . . . O10 O 0.3977(3) 0.6257(3) 0.0910(2) 0.0407(8) Uani 1 1 d . . . O11 O 0.4907(3) 0.7513(3) 0.32679(19) 0.0421(9) Uani 1 1 d . . . O12 O 0.2820(3) 0.6357(3) 0.1961(2) 0.0450(9) 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 C1 0.055(4) 0.046(4) 0.052(4) -0.003(3) 0.005(3) 0.013(3) C2 0.069(5) 0.078(6) 0.061(5) -0.002(5) 0.026(4) 0.034(5) C3 0.079(5) 0.092(6) 0.037(4) 0.016(4) 0.020(4) 0.037(4) C4 0.052(4) 0.073(6) 0.069(5) 0.028(4) 0.020(4) 0.009(4) C5 0.060(5) 0.086(6) 0.063(5) 0.028(4) 0.033(4) 0.019(4) C6 0.072(5) 0.068(6) 0.066(5) -0.019(4) 0.023(4) 0.007(4) C7 0.040(3) 0.058(4) 0.050(4) 0.021(3) 0.007(3) 0.022(3) C8 0.065(5) 0.105(7) 0.073(5) 0.039(5) 0.002(4) 0.046(4) C9 0.057(4) 0.075(5) 0.080(5) 0.026(4) 0.032(4) 0.020(4) C10 0.040(3) 0.040(3) 0.039(3) 0.012(2) 0.000(2) 0.015(2) C11 0.059(4) 0.044(4) 0.074(5) 0.020(3) 0.006(3) 0.013(3) C12 0.064(4) 0.071(5) 0.046(4) 0.012(3) 0.013(3) 0.027(4) C13 0.030(3) 0.047(3) 0.046(3) 0.015(3) 0.009(2) 0.011(2) C14 0.051(4) 0.068(5) 0.084(5) 0.036(4) 0.016(4) 0.007(3) C15 0.047(4) 0.103(6) 0.067(5) -0.001(4) 0.016(3) 0.029(4) C16 0.039(3) 0.061(4) 0.056(4) 0.021(3) 0.002(3) 0.005(3) C17 0.043(4) 0.115(7) 0.100(6) 0.059(6) -0.001(4) 0.018(4) C18 0.108(7) 0.067(5) 0.056(5) -0.001(4) 0.025(4) 0.000(5) C19 0.039(3) 0.039(3) 0.039(3) 0.013(2) 0.009(2) 0.013(2) C20 0.037(3) 0.041(3) 0.041(3) 0.013(3) 0.007(2) 0.013(2) C21 0.043(3) 0.053(4) 0.037(3) 0.014(3) 0.012(2) 0.009(3) C22 0.056(4) 0.050(4) 0.032(3) 0.006(3) 0.009(3) 0.004(3) C23 0.042(3) 0.036(3) 0.037(3) 0.011(2) 0.010(2) 0.011(2) C24 0.047(3) 0.044(3) 0.031(3) 0.015(2) 0.011(2) 0.014(3) C25 0.045(3) 0.045(3) 0.032(3) 0.009(2) 0.004(2) 0.012(3) C26 0.075(5) 0.068(5) 0.036(4) 0.015(3) 0.009(3) 0.005(4) C27 0.076(5) 0.087(6) 0.049(4) 0.028(4) 0.027(4) 0.004(4) C28 0.058(4) 0.054(4) 0.060(4) 0.027(3) 0.018(3) 0.004(3) C29 0.051(3) 0.047(4) 0.042(3) 0.009(3) 0.010(3) 0.006(3) C30 0.081(6) 0.060(5) 0.088(6) 0.011(4) 0.026(5) -0.014(4) C31 0.059(4) 0.050(4) 0.030(3) 0.012(3) 0.014(3) 0.027(3) C32 0.052(4) 0.067(4) 0.039(3) 0.022(3) 0.023(3) 0.019(3) C33 0.047(3) 0.039(3) 0.049(4) 0.013(3) 0.019(3) 0.011(3) C34 0.048(3) 0.050(4) 0.037(3) 0.008(3) 0.017(3) 0.023(3) C35 0.053(4) 0.049(4) 0.039(3) -0.007(3) 0.009(3) 0.019(3) C36 0.045(3) 0.030(3) 0.035(3) 0.004(2) 0.004(2) 0.006(2) C37 0.036(3) 0.062(4) 0.038(3) 0.021(3) 0.015(2) 0.022(3) C38 0.059(4) 0.068(4) 0.030(3) 0.001(3) 0.018(3) 0.023(3) C39 0.042(3) 0.045(4) 0.041(3) -0.007(3) 0.006(2) 0.016(3) C41 0.048(3) 0.044(4) 0.044(3) 0.020(3) 0.012(3) 0.021(3) C43 0.067(4) 0.042(4) 0.059(4) 0.026(3) 0.002(3) 0.013(3) C44 0.055(4) 0.071(5) 0.111(6) 0.043(4) 0.005(4) 0.002(3) C45 0.148(8) 0.118(7) 0.114(7) 0.059(6) 0.052(6) 0.050(6) C46 0.091(5) 0.106(6) 0.088(6) 0.052(5) 0.035(4) 0.038(5) C47 0.146(7) 0.056(5) 0.065(5) 0.012(4) 0.020(5) 0.047(5) C48 0.105(6) 0.068(5) 0.079(5) 0.035(4) 0.007(4) 0.011(4) C49 0.161(9) 0.137(8) 0.182(9) 0.055(7) 0.051(7) 0.088(7) C50 0.143(8) 0.114(8) 0.182(9) 0.060(7) -0.005(7) 0.047(7) C51 0.125(7) 0.091(7) 0.139(8) 0.053(6) 0.004(6) 0.026(5) C52 0.163(9) 0.132(8) 0.127(8) 0.066(7) 0.003(6) 0.027(6) C53 0.108(8) 0.114(9) 0.106(8) 0.023(7) 0.011(6) 0.013(7) Dy 0.02953(14) 0.03084(15) 0.02503(14) 0.00456(10) 0.00561(9) 0.00921(10) F1 0.048(2) 0.088(3) 0.101(3) -0.016(3) 0.019(2) -0.012(2) F2 0.088(3) 0.088(3) 0.079(3) 0.018(3) -0.029(2) 0.013(3) F3 0.073(3) 0.048(3) 0.106(3) -0.031(2) 0.000(2) 0.012(2) F4 0.069(8) 0.25(3) 0.077(13) -0.065(19) 0.025(8) 0.048(17) F5 0.17(2) 0.20(2) 0.21(3) 0.14(3) 0.14(2) 0.16(2) F6 0.071(9) 0.096(10) 0.150(19) 0.038(11) 0.074(11) 0.026(7) F7 0.234(7) 0.151(6) 0.046(3) -0.010(3) 0.025(3) 0.125(5) F8 0.090(3) 0.172(5) 0.041(2) 0.024(3) 0.001(2) 0.046(3) F9 0.147(5) 0.184(6) 0.051(3) 0.057(4) 0.034(3) 0.017(4) F10 0.043(6) 0.164(14) 0.187(19) 0.074(12) 0.022(9) 0.036(8) F11 0.122(12) 0.20(2) 0.098(10) 0.082(12) 0.014(7) -0.081(12) F12 0.081(6) 0.097(9) 0.112(11) -0.010(7) 0.008(6) -0.030(6) F13 0.061(3) 0.222(7) 0.103(4) 0.060(4) 0.027(3) -0.021(4) F14 0.157(5) 0.143(5) 0.098(4) 0.020(4) 0.096(4) 0.006(4) F15 0.212(7) 0.143(6) 0.268(9) 0.153(6) 0.181(7) 0.097(6) F16 0.116(4) 0.106(4) 0.101(4) -0.055(3) 0.041(3) 0.021(3) F17 0.090(4) 0.160(6) 0.228(8) -0.136(6) -0.087(5) 0.069(4) F18 0.202(8) 0.068(4) 0.147(6) -0.035(4) 0.067(6) -0.015(4) F4' 0.102(10) 0.120(12) 0.106(17) -0.034(11) 0.028(12) 0.068(9) F5' 0.069(9) 0.26(3) 0.081(13) -0.070(19) -0.028(10) 0.103(14) F6' 0.16(3) 0.27(4) 0.18(4) 0.14(3) 0.14(3) 0.14(3) F10' 0.057(17) 0.13(3) 0.13(3) 0.11(3) -0.042(15) -0.043(16) F11' 0.060(10) 0.099(19) 0.20(3) 0.019(16) 0.088(15) 0.007(11) F12' 0.043(9) 0.031(10) 0.23(5) 0.034(17) -0.003(18) -0.004(6) N1 0.051(3) 0.050(3) 0.058(3) 0.023(2) 0.017(2) 0.031(2) N2 0.041(2) 0.041(3) 0.038(3) 0.017(2) 0.0096(19) 0.020(2) N3 0.034(2) 0.045(3) 0.034(2) 0.014(2) 0.0082(19) 0.014(2) N4 0.041(3) 0.056(3) 0.044(3) 0.026(2) 0.004(2) 0.013(2) O1 0.087(4) 0.066(3) 0.102(4) 0.035(3) 0.033(3) 0.052(3) O2 0.045(2) 0.059(3) 0.044(2) 0.0218(19) 0.0114(17) 0.0313(19) O3 0.0366(19) 0.047(2) 0.036(2) 0.0182(17) 0.0114(16) 0.0195(16) O4 0.062(3) 0.084(4) 0.062(3) 0.042(3) -0.002(2) 0.014(2) O5 0.076(3) 0.079(4) 0.071(3) 0.027(3) 0.024(3) -0.015(3) O6 0.103(5) 0.088(5) 0.168(6) 0.009(4) -0.021(4) 0.014(4) O7 0.036(2) 0.039(2) 0.039(2) 0.0019(17) 0.0089(16) 0.0096(16) O8 0.041(2) 0.041(2) 0.040(2) 0.0005(18) 0.0108(16) 0.0148(17) O9 0.040(2) 0.047(2) 0.032(2) 0.0109(17) 0.0132(16) 0.0172(17) O10 0.043(2) 0.036(2) 0.034(2) 0.0030(16) 0.0095(16) 0.0126(16) O11 0.043(2) 0.045(2) 0.031(2) 0.0079(17) 0.0099(16) 0.0150(17) O12 0.044(2) 0.044(2) 0.034(2) 0.0094(17) 0.0132(17) 0.0062(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 F3 1.295(7) . ? C1 F1 1.306(8) . ? C1 F2 1.315(8) . ? C1 C36 1.520(8) . ? C2 F5' 1.23(2) . ? C2 F6' 1.248(19) . ? C2 F5 1.27(2) . ? C2 F4 1.282(17) . ? C2 F4' 1.334(10) . ? C2 F6 1.337(9) . ? C2 C34 1.533(8) . ? C3 F7 1.272(9) . ? C3 F8 1.296(8) . ? C3 F9 1.305(9) . ? C3 C31 1.519(8) . ? C4 F12' 1.219(19) . ? C4 F10' 1.25(3) . ? C4 F11 1.268(12) . ? C4 F10 1.275(17) . ? C4 F12 1.329(13) . ? C4 F11' 1.338(10) . ? C4 C33 1.523(9) . ? C5 F13 1.275(9) . ? C5 F14 1.276(8) . ? C5 F15 1.290(9) . ? C5 C37 1.504(8) . ? C6 F17 1.210(10) . ? C6 F16 1.278(8) . ? C6 F18 1.334(11) . ? C6 C39 1.516(9) . ? C7 N1 1.484(8) . ? C7 C8 1.509(8) . ? C7 C9 1.519(8) . ? C7 C10 1.542(8) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 N2 1.493(7) . ? C10 C11 1.508(8) . ? C10 C12 1.517(8) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N3 1.493(6) . ? C13 C14 1.495(8) . ? C13 C15 1.527(9) . ? C13 C16 1.536(8) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N4 1.485(7) . ? C16 C17 1.513(10) . ? C16 C18 1.527(10) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.324(7) . ? C19 N4 1.356(7) . ? C19 C20 1.437(7) . ? C20 C25 1.367(7) . ? C20 C21 1.414(8) . ? C21 C22 1.350(8) . ? C21 H21 0.9300 . ? C22 C23 1.400(7) . ? C22 H22 0.9300 . ? C23 C29 1.395(7) . ? C23 C24 1.417(7) . ? C24 C26 1.392(8) . ? C24 C25 1.393(7) . ? C25 H25 0.9300 . ? C26 C27 1.353(9) . ? C26 H26 0.9300 . ? C27 C28 1.382(9) . ? C27 H27 0.9300 . ? C28 C29 1.360(8) . ? C28 O5 1.363(7) . ? C29 H29 0.9300 . ? C30 O5 1.396(9) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 O11 1.245(6) . ? C31 C32 1.373(8) . ? C32 C33 1.365(8) . ? C32 H32 0.9300 . ? C33 O12 1.242(6) . ? C34 O8 1.238(6) . ? C34 C35 1.374(8) . ? C35 C36 1.376(8) . ? C35 H35 0.9300 . ? C36 O7 1.243(6) . ? C37 O9 1.238(6) . ? C37 C38 1.373(8) . ? C38 C39 1.374(8) . ? C38 H38 0.9300 . ? C39 O10 1.225(6) . ? C41 N2 1.317(7) . ? C41 N1 1.348(7) . ? C41 C43 1.444(8) . ? C43 C44 1.389(8) . ? C43 C48 1.398(11) . ? C44 C45 1.375(13) . ? C44 H44 0.9300 . ? C45 C46 1.270(13) . ? C45 H45 0.9300 . ? C46 C47 1.404(8) . ? C46 C52 1.480(9) . ? C47 C49 1.311(15) . ? C47 C48 1.476(8) . ? C48 H48 0.9300 . ? C49 C50 1.414(9) . ? C49 H49 0.9300 . ? C50 C51 1.450(18) . ? C50 H50 0.9300 . ? C51 C52 1.284(18) . ? C51 O6 1.420(13) . ? C52 H52 0.9300 . ? C53 O6 1.361(12) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? Dy O12 2.317(4) . ? Dy O7 2.320(4) . ? Dy O2 2.322(4) . ? Dy O3 2.327(3) . ? Dy O10 2.342(4) . ? Dy O9 2.366(3) . ? Dy O11 2.372(3) . ? Dy O8 2.376(4) . ? N1 O1 1.259(6) . ? N2 O2 1.286(5) . ? N3 O3 1.293(5) . ? N4 O4 1.254(6) . ? 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 F3 C1 F1 107.2(6) . . ? F3 C1 F2 107.0(6) . . ? F1 C1 F2 105.7(6) . . ? F3 C1 C36 114.0(6) . . ? F1 C1 C36 112.6(5) . . ? F2 C1 C36 109.8(5) . . ? F5' C2 F6' 117(2) . . ? F5' C2 F5 27.1(17) . . ? F6' C2 F5 133.2(17) . . ? F5' C2 F4 129.0(18) . . ? F6' C2 F4 62.3(14) . . ? F5 C2 F4 112(2) . . ? F5' C2 F4' 99.5(16) . . ? F6' C2 F4' 105.3(18) . . ? F5 C2 F4' 74.2(15) . . ? F4 C2 F4' 44.7(17) . . ? F5' C2 F6 75.0(16) . . ? F6' C2 F6 48(2) . . ? F5 C2 F6 100.2(14) . . ? F4 C2 F6 106.1(16) . . ? F4' C2 F6 137.2(12) . . ? F5' C2 C34 112.6(12) . . ? F6' C2 C34 110.3(11) . . ? F5 C2 C34 113.0(11) . . ? F4 C2 C34 114.4(12) . . ? F4' C2 C34 111.4(12) . . ? F6 C2 C34 109.7(8) . . ? F7 C3 F8 108.0(7) . . ? F7 C3 F9 107.7(7) . . ? F8 C3 F9 104.2(7) . . ? F7 C3 C31 110.8(6) . . ? F8 C3 C31 112.4(6) . . ? F9 C3 C31 113.3(7) . . ? F12' C4 F10' 108(2) . . ? F12' C4 F11 54.5(17) . . ? F10' C4 F11 125.0(15) . . ? F12' C4 F10 134.9(13) . . ? F10' C4 F10 41(3) . . ? F11 C4 F10 110.1(16) . . ? F12' C4 F12 55(2) . . ? F10' C4 F12 64(2) . . ? F11 C4 F12 106.2(13) . . ? F10 C4 F12 104.3(12) . . ? F12' C4 F11' 102(2) . . ? F10' C4 F11' 103(3) . . ? F11 C4 F11' 49.1(12) . . ? F10 C4 F11' 68.2(17) . . ? F12 C4 F11' 141.2(11) . . ? F12' C4 C33 114.9(11) . . ? F10' C4 C33 117.8(12) . . ? F11 C4 C33 116.3(8) . . ? F10 C4 C33 109.8(11) . . ? F12 C4 C33 109.5(7) . . ? F11' C4 C33 108.7(11) . . ? F13 C5 F14 107.0(7) . . ? F13 C5 F15 103.7(8) . . ? F14 C5 F15 105.3(7) . . ? F13 C5 C37 113.3(6) . . ? F14 C5 C37 115.9(7) . . ? F15 C5 C37 110.7(6) . . ? F17 C6 F16 112.9(8) . . ? F17 C6 F18 103.8(9) . . ? F16 C6 F18 98.7(8) . . ? F17 C6 C39 114.1(8) . . ? F16 C6 C39 115.4(6) . . ? F18 C6 C39 110.1(7) . . ? N1 C7 C8 110.2(5) . . ? N1 C7 C9 106.0(5) . . ? C8 C7 C9 110.0(6) . . ? N1 C7 C10 101.2(4) . . ? C8 C7 C10 115.1(6) . . ? C9 C7 C10 113.6(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 110.4(4) . . ? N2 C10 C12 105.5(5) . . ? C11 C10 C12 111.0(5) . . ? N2 C10 C7 99.4(4) . . ? C11 C10 C7 115.5(5) . . ? C12 C10 C7 113.9(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 110.3(5) . . ? N3 C13 C15 105.5(5) . . ? C14 C13 C15 110.6(6) . . ? N3 C13 C16 100.3(4) . . ? C14 C13 C16 116.1(5) . . ? C15 C13 C16 113.0(6) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 109.3(6) . . ? N4 C16 C18 106.4(5) . . ? C17 C16 C18 110.7(6) . . ? N4 C16 C13 100.6(4) . . ? C17 C16 C13 116.3(6) . . ? C18 C16 C13 112.5(6) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 N4 107.5(5) . . ? N3 C19 C20 126.8(5) . . ? N4 C19 C20 125.6(5) . . ? C25 C20 C21 118.7(5) . . ? C25 C20 C19 120.8(5) . . ? C21 C20 C19 120.4(5) . . ? C22 C21 C20 120.5(5) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 121.8(5) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C29 C23 C22 122.7(5) . . ? C29 C23 C24 119.3(5) . . ? C22 C23 C24 117.9(5) . . ? C26 C24 C25 122.0(5) . . ? C26 C24 C23 118.6(5) . . ? C25 C24 C23 119.4(5) . . ? C20 C25 C24 121.6(5) . . ? C20 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C27 C26 C24 120.9(6) . . ? C27 C26 H26 119.6 . . ? C24 C26 H26 119.6 . . ? C26 C27 C28 120.3(6) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 O5 124.6(6) . . ? C29 C28 C27 121.2(6) . . ? O5 C28 C27 114.2(5) . . ? C28 C29 C23 119.7(6) . . ? C28 C29 H29 120.2 . . ? C23 C29 H29 120.2 . . ? O5 C30 H30A 109.5 . . ? O5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O11 C31 C32 127.9(5) . . ? O11 C31 C3 114.3(5) . . ? C32 C31 C3 117.9(5) . . ? C33 C32 C31 121.5(5) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? O12 C33 C32 128.3(5) . . ? O12 C33 C4 113.2(5) . . ? C32 C33 C4 118.4(5) . . ? O8 C34 C35 128.4(5) . . ? O8 C34 C2 114.0(5) . . ? C35 C34 C2 117.6(5) . . ? C34 C35 C36 121.6(5) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? O7 C36 C35 128.4(5) . . ? O7 C36 C1 115.1(5) . . ? C35 C36 C1 116.5(5) . . ? O9 C37 C38 128.7(5) . . ? O9 C37 C5 114.3(5) . . ? C38 C37 C5 117.0(5) . . ? C37 C38 C39 122.2(5) . . ? C37 C38 H38 118.9 . . ? C39 C38 H38 118.9 . . ? O10 C39 C38 127.8(5) . . ? O10 C39 C6 115.6(6) . . ? C38 C39 C6 116.5(6) . . ? N2 C41 N1 108.1(5) . . ? N2 C41 C43 125.3(5) . . ? N1 C41 C43 126.6(6) . . ? C44 C43 C48 117.6(7) . . ? C44 C43 C41 120.0(7) . . ? C48 C43 C41 122.4(7) . . ? C45 C44 C43 128.8(10) . . ? C45 C44 H44 115.6 . . ? C43 C44 H44 115.6 . . ? C46 C45 C44 114.0(12) . . ? C46 C45 H45 123.0 . . ? C44 C45 H45 123.0 . . ? C45 C46 C47 124.2(10) . . ? C45 C46 C52 112.0(11) . . ? C47 C46 C52 123.8(11) . . ? C49 C47 C46 124.3(10) . . ? C49 C47 C48 113.7(10) . . ? C46 C47 C48 121.7(8) . . ? C43 C48 C47 113.2(8) . . ? C43 C48 H48 123.4 . . ? C47 C48 H48 123.4 . . ? C47 C49 C50 110.9(13) . . ? C47 C49 H49 124.5 . . ? C50 C49 H49 124.5 . . ? C49 C50 C51 126.8(15) . . ? C49 C50 H50 116.6 . . ? C51 C50 H50 116.6 . . ? C52 C51 O6 129.1(14) . . ? C52 C51 C50 121.5(13) . . ? O6 C51 C50 109.4(13) . . ? C51 C52 C46 112.5(14) . . ? C51 C52 H52 123.7 . . ? C46 C52 H52 123.7 . . ? O6 C53 H53A 109.5 . . ? O6 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O6 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O12 Dy O7 137.44(12) . . ? O12 Dy O2 93.35(14) . . ? O7 Dy O2 101.65(14) . . ? O12 Dy O3 103.63(13) . . ? O7 Dy O3 90.84(13) . . ? O2 Dy O3 138.72(12) . . ? O12 Dy O10 71.28(13) . . ? O7 Dy O10 150.93(13) . . ? O2 Dy O10 76.20(14) . . ? O3 Dy O10 74.26(13) . . ? O12 Dy O9 143.34(12) . . ? O7 Dy O9 78.94(13) . . ? O2 Dy O9 69.75(12) . . ? O3 Dy O9 74.47(12) . . ? O10 Dy O9 73.11(12) . . ? O12 Dy O11 72.47(13) . . ? O7 Dy O11 73.20(13) . . ? O2 Dy O11 146.37(13) . . ? O3 Dy O11 74.89(12) . . ? O10 Dy O11 124.24(13) . . ? O9 Dy O11 137.79(12) . . ? O12 Dy O8 73.86(13) . . ? O7 Dy O8 73.07(12) . . ? O2 Dy O8 72.82(13) . . ? O3 Dy O8 147.93(13) . . ? O10 Dy O8 131.17(12) . . ? O9 Dy O8 126.77(13) . . ? O11 Dy O8 73.95(13) . . ? O1 N1 C41 125.6(5) . . ? O1 N1 C7 122.3(5) . . ? C41 N1 C7 111.8(5) . . ? O2 N2 C41 126.6(5) . . ? O2 N2 C10 119.4(4) . . ? C41 N2 C10 113.2(4) . . ? O3 N3 C19 126.0(4) . . ? O3 N3 C13 120.7(4) . . ? C19 N3 C13 112.4(4) . . ? O4 N4 C19 125.7(5) . . ? O4 N4 C16 121.4(5) . . ? C19 N4 C16 112.4(4) . . ? N2 O2 Dy 137.9(3) . . ? N3 O3 Dy 136.2(3) . . ? C28 O5 C30 118.2(5) . . ? C53 O6 C51 117.0(10) . . ? C36 O7 Dy 132.9(3) . . ? C34 O8 Dy 131.7(3) . . ? C37 O9 Dy 131.8(3) . . ? C39 O10 Dy 133.9(4) . . ? C31 O11 Dy 132.5(4) . . ? C33 O12 Dy 134.6(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.412 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.108 data_shelxla _database_code_depnum_ccdc_archive 'CCDC 824913' #TrackingRef '- complex-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H45 F18 N4 O12 Pr' _chemical_formula_weight 1388.82 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.388(3) _cell_length_b 14.306(3) _cell_length_c 19.221(4) _cell_angle_alpha 100.93(3) _cell_angle_beta 103.76(3) _cell_angle_gamma 111.60(3) _cell_volume 2927.8(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26681 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.59 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.859 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24257 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10266 _reflns_number_gt 8690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Fluorine atoms in the CF3 groups and the carbon atoms in the naphthaline ring were treated by disorder and these atoms were refined anisotropically with application of restraints on thermal parameters (ISOR and SIMU instructions in SHELXL). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+5.0298P] 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 10266 _refine_ls_number_parameters 785 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1436 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.047 _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 Pr Pr 0.46702(2) 0.76468(2) 0.201090(15) 0.03881(12) Uani 1 1 d . . . O12 O 0.5961(3) 0.8191(3) 0.1231(2) 0.0495(9) Uani 1 1 d . . . O11 O 0.3958(3) 0.6178(3) 0.0864(2) 0.0539(10) Uani 1 1 d . . . O3 O 0.6129(3) 0.6885(3) 0.2255(2) 0.0512(9) Uani 1 1 d . . . O9 O 0.4848(4) 0.7449(3) 0.3285(2) 0.0547(10) Uani 1 1 d . . . O7 O 0.6176(3) 0.9335(3) 0.2919(2) 0.0555(10) Uani 1 1 d . . . O10 O 0.2760(3) 0.6291(3) 0.1979(2) 0.0553(10) Uani 1 1 d . . . O8 O 0.3582(3) 0.8590(3) 0.2553(2) 0.0541(10) Uani 1 1 d . . . N1 N 0.2796(4) 0.8524(4) 0.0900(3) 0.0480(11) Uani 1 1 d . . . O1 O 0.3649(4) 0.8177(3) 0.1030(2) 0.0576(10) Uani 1 1 d . . . N3 N 0.6857(4) 0.6835(4) 0.2847(2) 0.0477(11) Uani 1 1 d . . . N2 N 0.1848(4) 0.9526(4) 0.0914(3) 0.0556(12) Uani 1 1 d . . . C44 C 0.3051(5) 0.3533(4) 0.2657(3) 0.0491(13) Uani 1 1 d . . . F13 F 0.7456(4) 1.1624(3) 0.4389(3) 0.1142(18) Uani 1 1 d . . . O4 O 0.7556(4) 0.6006(4) 0.4365(3) 0.0843(15) Uani 1 1 d . . . N4 N 0.7535(4) 0.6438(4) 0.3847(3) 0.0584(13) Uani 1 1 d . . . O2 O 0.1631(4) 1.0330(4) 0.1062(3) 0.0799(14) Uani 1 1 d . . . C42 C 0.4598(5) 0.4721(5) 0.2282(3) 0.0553(15) Uani 1 1 d . . . H42 H 0.4877 0.4925 0.1902 0.066 Uiso 1 1 calc R . . C40 C 0.6523(5) 0.6179(4) 0.3240(3) 0.0474(13) Uani 1 1 d . . . C22 C 0.2960(5) 0.9507(5) 0.1165(3) 0.0507(14) Uani 1 1 d . . . C15 C 0.5797(5) 0.7828(5) 0.0555(3) 0.0534(14) Uani 1 1 d . . . C16 C 0.1582(5) 0.7824(4) 0.0307(3) 0.0532(14) Uani 1 1 d . . . C43 C 0.3521(6) 0.3873(5) 0.2104(3) 0.0638(17) Uani 1 1 d . . . H43 H 0.3069 0.3498 0.1599 0.077 Uiso 1 1 calc R . . C50 C 0.4872(5) 0.4997(5) 0.3599(3) 0.0542(14) Uani 1 1 d . . . H50 H 0.5333 0.5375 0.4102 0.065 Uiso 1 1 calc R . . F15 F 0.7730(5) 1.0296(4) 0.4549(3) 0.1203(19) Uani 1 1 d . . . C5 C 0.7412(6) 1.0739(5) 0.4032(4) 0.0683(18) Uani 1 1 d . . . C9 C 0.6146(5) 0.9962(4) 0.3452(3) 0.0530(14) Uani 1 1 d . . . C41 C 0.5316(5) 0.5308(4) 0.3048(3) 0.0476(13) Uani 1 1 d . . . C7 C 0.3927(5) 0.9329(5) 0.3128(3) 0.0533(14) Uani 1 1 d . . . C49 C 0.3740(5) 0.4122(5) 0.3417(3) 0.0510(13) Uani 1 1 d . . . F14 F 0.8288(4) 1.0965(4) 0.3750(3) 0.1174(18) Uani 1 1 d . . . C20 C 0.0207(7) 0.8092(6) 0.1068(4) 0.077(2) Uani 1 1 d . . . H20A H 0.0801 0.8104 0.1498 0.115 Uiso 1 1 calc R . . H20B H -0.0442 0.7389 0.0834 0.115 Uiso 1 1 calc R . . H20C H -0.0133 0.8566 0.1225 0.115 Uiso 1 1 calc R . . C13 C 0.4108(6) 0.6113(5) 0.0249(3) 0.0612(16) Uani 1 1 d . . . C17 C 0.1115(7) 0.6708(5) 0.0367(5) 0.079(2) Uani 1 1 d . . . H17A H 0.1639 0.6396 0.0245 0.119 Uiso 1 1 calc R . . H17B H 0.0288 0.6292 0.0022 0.119 Uiso 1 1 calc R . . H17C H 0.1125 0.6733 0.0871 0.119 Uiso 1 1 calc R . . F2 F 0.5735(5) 0.7518(5) 0.4696(2) 0.125(2) Uani 1 1 d . . . C21 C -0.0080(7) 0.8474(7) -0.0166(4) 0.087(2) Uani 1 1 d . . . H21A H -0.0506 0.8858 0.0008 0.130 Uiso 1 1 calc R . . H21B H -0.0666 0.7768 -0.0469 0.130 Uiso 1 1 calc R . . H21C H 0.0360 0.8820 -0.0463 0.130 Uiso 1 1 calc R . . F1 F 0.4542(8) 0.8232(6) 0.4719(3) 0.162(3) Uani 1 1 d . . . C12 C 0.2293(5) 0.6002(5) 0.2450(4) 0.0555(15) Uani 1 1 d . . . C34 C 0.8235(5) 0.7449(5) 0.3077(3) 0.0545(14) Uani 1 1 d . . . C10 C 0.4078(6) 0.7029(5) 0.3576(3) 0.0530(14) Uani 1 1 d . . . F3 F 0.4018(7) 0.6669(6) 0.4729(3) 0.163(3) Uani 1 1 d . . . C18 C 0.1788(7) 0.7838(6) -0.0443(3) 0.0729(19) Uani 1 1 d . . . H18A H 0.2085 0.8549 -0.0466 0.109 Uiso 1 1 calc R . . H18B H 0.1024 0.7401 -0.0847 0.109 Uiso 1 1 calc R . . H18C H 0.2384 0.7572 -0.0486 0.109 Uiso 1 1 calc R . . C23 C 0.5218(8) 1.0445(7) 0.1514(5) 0.099(2) Uani 1 1 d U . . H23 H 0.5128 0.9891 0.1127 0.118 Uiso 1 1 calc R . . C11 C 0.2848(6) 0.6336(5) 0.3220(4) 0.0628(16) Uani 1 1 d . . . H11 H 0.2376 0.6084 0.3512 0.075 Uiso 1 1 calc R . . C19 C 0.0830(5) 0.8435(5) 0.0508(3) 0.0562(15) Uani 1 1 d . . . F9 F 0.3702(6) 0.4718(5) -0.0812(4) 0.168(3) Uani 1 1 d . . . C47 C 0.2211(8) 0.2949(7) 0.3799(4) 0.091(3) Uani 1 1 d . . . H47 H 0.1917 0.2754 0.4177 0.109 Uiso 1 1 calc R . . F6 F 0.0288(5) 0.5483(7) 0.1688(5) 0.200(4) Uani 1 1 d . . . C31 C 0.6895(12) 1.3524(9) 0.3604(8) 0.143(3) Uani 1 1 d U . . H31 H 0.7058 1.4084 0.4012 0.172 Uiso 1 1 calc R . . O5 O 0.0471(5) 0.1478(5) 0.2937(3) 0.105(2) Uani 1 1 d . . . C45 C 0.1930(6) 0.2620(5) 0.2481(3) 0.0599(16) Uani 1 1 d . . . H45 H 0.1473 0.2220 0.1981 0.072 Uiso 1 1 calc R . . C8 C 0.5124(6) 1.0018(5) 0.3593(3) 0.0609(16) Uani 1 1 d . . . H8 H 0.5243 1.0537 0.4015 0.073 Uiso 1 1 calc R . . C4 C 0.6695(8) 0.8574(7) 0.0262(5) 0.084(2) Uani 1 1 d . . . C14 C 0.4945(6) 0.6872(6) 0.0045(4) 0.0677(18) Uani 1 1 d . . . H14 H 0.4927 0.6727 -0.0451 0.081 Uiso 1 1 calc R . . C51 C -0.0270(8) 0.0825(7) 0.2197(5) 0.107(3) Uani 1 1 d . . . H51A H -0.0475 0.1244 0.1900 0.160 Uiso 1 1 calc R . . H51B H -0.1012 0.0292 0.2204 0.160 Uiso 1 1 calc R . . H51C H 0.0173 0.0494 0.1981 0.160 Uiso 1 1 calc R . . C3 C 0.3227(8) 0.5073(8) -0.0367(6) 0.108(3) Uani 1 1 d . . . C24 C 0.4122(7) 1.0407(5) 0.1629(4) 0.0727(18) Uani 1 1 d U . . C2 C 0.0947(7) 0.5234(7) 0.2115(5) 0.094(3) Uani 1 1 d . . . F10 F 0.6735(7) 0.8149(6) -0.0379(4) 0.167(3) Uani 1 1 d . . . C35 C 0.8623(7) 0.6804(7) 0.2538(4) 0.097(3) Uani 1 1 d . . . H35A H 0.8272 0.6798 0.2033 0.145 Uiso 1 1 calc R . . H35B H 0.8333 0.6094 0.2561 0.145 Uiso 1 1 calc R . . H35C H 0.9505 0.7119 0.2681 0.145 Uiso 1 1 calc R . . C27 C 0.6496(10) 1.1907(8) 0.2426(6) 0.104(2) Uani 1 1 d U . . F7 F 0.2962(9) 0.4262(6) -0.0074(5) 0.213(5) Uani 1 1 d . . . C28 C 0.6405(11) 1.1203(9) 0.1903(7) 0.126(3) Uani 1 1 d U . . H28 H 0.7082 1.1185 0.1782 0.151 Uiso 1 1 calc R . . F8 F 0.2222(6) 0.4996(7) -0.0671(5) 0.247(6) Uani 1 1 d . . . C36 C 0.8570(7) 0.8535(6) 0.3003(5) 0.088(2) Uani 1 1 d . . . H36A H 0.8193 0.8483 0.2491 0.132 Uiso 1 1 calc R . . H36B H 0.9450 0.8906 0.3144 0.132 Uiso 1 1 calc R . . H36C H 0.8284 0.8911 0.3326 0.132 Uiso 1 1 calc R . . C25 C 0.4188(9) 1.1220(6) 0.2176(5) 0.097(2) Uani 1 1 d U . . H25 H 0.3505 1.1272 0.2269 0.117 Uiso 1 1 calc R . . C29 C 0.7937(12) 1.2729(9) 0.2889(7) 0.141(3) Uani 1 1 d U . . H29 H 0.8630 1.2703 0.2795 0.169 Uiso 1 1 calc R . . C46 C 0.1525(6) 0.2331(5) 0.3032(4) 0.0707(18) Uani 1 1 d . . . C48 C 0.3274(7) 0.3809(6) 0.3981(4) 0.078(2) Uani 1 1 d . . . H48 H 0.3710 0.4204 0.4484 0.094 Uiso 1 1 calc R . . F11 F 0.6450(8) 0.9358(6) 0.0199(5) 0.184(4) Uani 1 1 d . . . F16 F 0.3172(6) 1.0268(8) 0.3871(5) 0.238(6) Uani 1 1 d . . . F5 F 0.0806(6) 0.4372(6) 0.1741(8) 0.269(7) Uani 1 1 d . . . F18 F 0.2193(9) 0.8683(8) 0.3463(7) 0.241(6) Uani 1 1 d . . . C6 C 0.2879(7) 0.9482(7) 0.3345(4) 0.080(2) Uani 1 1 d . . . F17 F 0.2112(6) 0.9568(7) 0.2799(4) 0.159(3) Uani 1 1 d . . . F12 F 0.7810(5) 0.9011(7) 0.0722(4) 0.178(4) Uani 1 1 d . . . C32 C 0.5559(12) 1.2743(9) 0.3160(7) 0.135(3) Uani 1 1 d U . . H32 H 0.4865 1.2760 0.3258 0.162 Uiso 1 1 calc R . . C1 C 0.4591(8) 0.7380(7) 0.4438(4) 0.080(2) Uani 1 1 d . . . C26 C 0.5568(10) 1.2058(7) 0.2627(5) 0.098(2) Uani 1 1 d U . . F4 F 0.0399(7) 0.5000(10) 0.2569(5) 0.275(8) Uani 1 1 d . . . C30 C 0.7909(12) 1.3426(10) 0.3416(8) 0.133(3) Uani 1 1 d U . . O6 O 0.9061(8) 1.4270(6) 0.3970(6) 0.174(4) Uani 1 1 d . . . C37 C 0.8623(6) 0.7390(5) 0.3888(4) 0.0691(19) Uani 1 1 d . . . C39 C 0.9789(7) 0.7233(8) 0.4139(5) 0.109(3) Uani 1 1 d . . . H39A H 0.9918 0.7160 0.4635 0.163 Uiso 1 1 calc R . . H39B H 1.0482 0.7833 0.4146 0.163 Uiso 1 1 calc R . . H39C H 0.9703 0.6607 0.3795 0.163 Uiso 1 1 calc R . . C38 C 0.8674(10) 0.8321(6) 0.4471(4) 0.113(3) Uani 1 1 d . . . H38A H 0.7936 0.8411 0.4298 0.170 Uiso 1 1 calc R . . H38B H 0.9377 0.8955 0.4534 0.170 Uiso 1 1 calc R . . H38C H 0.8742 0.8178 0.4944 0.170 Uiso 1 1 calc R . . C33 C 1.0108(11) 1.4179(10) 0.4053(7) 0.150(5) Uani 1 1 d . . . H33A H 1.0020 1.3530 0.4158 0.225 Uiso 1 1 calc R . . H33B H 1.0760 1.4763 0.4462 0.225 Uiso 1 1 calc R . . H33C H 1.0301 1.4177 0.3598 0.225 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr 0.03580(17) 0.04433(18) 0.02939(16) 0.00759(11) 0.00640(11) 0.01473(13) O12 0.045(2) 0.058(2) 0.042(2) 0.0167(18) 0.0134(17) 0.0189(18) O11 0.049(2) 0.051(2) 0.049(2) 0.0045(18) 0.0137(18) 0.0166(19) O3 0.048(2) 0.068(2) 0.043(2) 0.0243(19) 0.0129(17) 0.030(2) O9 0.056(2) 0.062(2) 0.035(2) 0.0083(18) 0.0108(18) 0.021(2) O7 0.045(2) 0.056(2) 0.050(2) 0.0028(19) 0.0120(18) 0.0155(19) O10 0.050(2) 0.060(2) 0.044(2) 0.0141(19) 0.0145(18) 0.0129(19) O8 0.046(2) 0.060(2) 0.049(2) 0.0046(19) 0.0121(18) 0.0221(19) N1 0.046(3) 0.055(3) 0.046(3) 0.020(2) 0.011(2) 0.025(2) O1 0.058(2) 0.078(3) 0.053(2) 0.027(2) 0.0178(19) 0.044(2) N3 0.041(2) 0.057(3) 0.042(2) 0.018(2) 0.008(2) 0.020(2) N2 0.054(3) 0.054(3) 0.062(3) 0.024(2) 0.014(2) 0.028(2) C44 0.052(3) 0.052(3) 0.044(3) 0.017(3) 0.014(3) 0.025(3) F13 0.080(3) 0.069(3) 0.123(4) -0.040(3) -0.011(3) 0.020(2) O4 0.076(3) 0.088(3) 0.062(3) 0.040(3) -0.005(2) 0.016(3) N4 0.054(3) 0.060(3) 0.047(3) 0.021(2) 0.002(2) 0.017(2) O2 0.082(3) 0.069(3) 0.107(4) 0.032(3) 0.031(3) 0.050(3) C42 0.057(4) 0.066(4) 0.038(3) 0.016(3) 0.017(3) 0.020(3) C40 0.049(3) 0.046(3) 0.042(3) 0.014(2) 0.009(2) 0.019(3) C22 0.054(3) 0.054(3) 0.045(3) 0.022(3) 0.012(3) 0.024(3) C15 0.049(3) 0.075(4) 0.049(4) 0.028(3) 0.022(3) 0.032(3) C16 0.050(3) 0.053(3) 0.048(3) 0.017(3) 0.005(3) 0.020(3) C43 0.060(4) 0.067(4) 0.040(3) 0.010(3) 0.011(3) 0.009(3) C50 0.061(4) 0.056(3) 0.036(3) 0.011(3) 0.006(3) 0.023(3) F15 0.106(4) 0.098(3) 0.085(3) 0.018(3) -0.035(3) 0.014(3) C5 0.057(4) 0.059(4) 0.059(4) -0.002(3) 0.002(3) 0.015(3) C9 0.052(3) 0.045(3) 0.042(3) 0.005(3) 0.005(3) 0.012(3) C41 0.045(3) 0.051(3) 0.041(3) 0.015(2) 0.008(2) 0.018(3) C7 0.054(3) 0.060(4) 0.043(3) 0.010(3) 0.017(3) 0.024(3) C49 0.054(3) 0.057(3) 0.043(3) 0.018(3) 0.015(3) 0.025(3) F14 0.055(3) 0.112(4) 0.113(4) -0.016(3) 0.015(3) -0.007(3) C20 0.069(4) 0.078(5) 0.084(5) 0.026(4) 0.035(4) 0.027(4) C13 0.049(3) 0.069(4) 0.047(4) -0.010(3) 0.010(3) 0.023(3) C17 0.077(5) 0.056(4) 0.091(5) 0.024(4) 0.014(4) 0.023(4) F2 0.114(4) 0.197(6) 0.047(2) 0.027(3) 0.005(3) 0.067(4) C21 0.069(4) 0.107(6) 0.081(5) 0.033(4) -0.001(4) 0.050(4) F1 0.271(9) 0.182(6) 0.052(3) -0.007(3) 0.028(4) 0.154(6) C12 0.053(3) 0.055(3) 0.064(4) 0.025(3) 0.025(3) 0.023(3) C34 0.043(3) 0.063(4) 0.050(3) 0.016(3) 0.010(3) 0.019(3) C10 0.066(4) 0.062(4) 0.038(3) 0.018(3) 0.019(3) 0.033(3) F3 0.182(6) 0.199(7) 0.057(3) 0.058(4) 0.039(4) 0.019(5) C18 0.081(5) 0.085(5) 0.047(4) 0.016(3) 0.015(3) 0.037(4) C23 0.074(4) 0.095(4) 0.108(5) 0.051(4) 0.012(4) 0.019(3) C11 0.068(4) 0.080(4) 0.052(4) 0.029(3) 0.033(3) 0.033(4) C19 0.048(3) 0.062(4) 0.059(4) 0.023(3) 0.011(3) 0.027(3) F9 0.135(5) 0.154(5) 0.133(5) -0.076(4) 0.050(4) 0.032(4) C47 0.088(5) 0.115(7) 0.057(4) 0.039(4) 0.030(4) 0.020(5) F6 0.056(3) 0.257(9) 0.249(9) 0.167(8) 0.000(4) 0.015(4) C31 0.138(6) 0.115(5) 0.149(6) 0.040(5) 0.009(5) 0.050(5) O5 0.087(4) 0.102(4) 0.088(4) 0.040(3) 0.029(3) -0.005(3) C45 0.062(4) 0.057(4) 0.045(3) 0.011(3) 0.011(3) 0.015(3) C8 0.060(4) 0.059(4) 0.046(3) -0.005(3) 0.009(3) 0.024(3) C4 0.078(5) 0.104(6) 0.084(6) 0.043(5) 0.045(5) 0.035(5) C14 0.062(4) 0.089(5) 0.043(3) 0.009(3) 0.022(3) 0.026(4) C51 0.090(6) 0.078(5) 0.100(7) 0.019(5) 0.024(5) -0.009(5) C3 0.074(6) 0.087(6) 0.095(7) -0.039(5) 0.024(5) -0.001(5) C24 0.069(4) 0.064(3) 0.075(4) 0.034(3) 0.009(3) 0.021(3) C2 0.062(5) 0.083(6) 0.093(6) 0.042(5) 0.006(4) -0.010(4) F10 0.191(7) 0.170(6) 0.120(5) 0.031(4) 0.121(5) 0.021(5) C35 0.059(4) 0.130(7) 0.078(5) -0.003(5) 0.021(4) 0.033(5) C27 0.118(5) 0.102(4) 0.100(4) 0.051(4) 0.035(4) 0.047(4) F7 0.214(9) 0.098(5) 0.195(8) -0.057(5) 0.071(7) -0.021(5) C28 0.119(5) 0.119(5) 0.119(5) 0.048(4) 0.029(4) 0.032(4) F8 0.108(5) 0.184(7) 0.267(10) -0.150(7) -0.106(6) 0.084(5) C36 0.060(4) 0.087(5) 0.098(6) 0.046(5) 0.014(4) 0.011(4) C25 0.111(5) 0.075(4) 0.077(4) 0.029(3) 0.006(4) 0.023(4) C29 0.146(6) 0.121(5) 0.125(6) 0.058(5) 0.019(5) 0.034(5) C46 0.067(4) 0.061(4) 0.073(5) 0.025(4) 0.023(4) 0.013(3) C48 0.078(5) 0.085(5) 0.047(4) 0.022(3) 0.017(3) 0.011(4) F11 0.228(8) 0.165(6) 0.273(10) 0.158(7) 0.180(8) 0.101(6) F16 0.094(4) 0.298(10) 0.194(7) -0.145(7) 0.025(4) 0.074(5) F5 0.071(4) 0.099(5) 0.462(19) -0.058(8) -0.009(7) -0.017(4) F18 0.235(9) 0.227(9) 0.462(17) 0.203(11) 0.295(12) 0.156(8) C6 0.057(4) 0.100(6) 0.063(4) -0.002(4) 0.020(4) 0.026(4) F17 0.123(5) 0.267(9) 0.133(5) 0.042(5) 0.042(4) 0.141(6) F12 0.071(3) 0.261(9) 0.130(5) 0.073(5) 0.040(4) -0.014(4) C32 0.146(6) 0.115(5) 0.143(6) 0.036(4) 0.029(5) 0.069(4) C1 0.096(6) 0.106(6) 0.041(4) 0.022(4) 0.025(4) 0.045(5) C26 0.137(5) 0.074(4) 0.090(4) 0.027(3) 0.027(4) 0.059(3) F4 0.103(5) 0.412(16) 0.140(6) 0.123(9) 0.027(5) -0.078(7) C30 0.141(6) 0.107(5) 0.136(6) 0.052(5) 0.023(5) 0.045(5) O6 0.100(5) 0.094(5) 0.211(9) 0.002(5) -0.046(6) 0.002(4) C37 0.052(4) 0.073(4) 0.055(4) 0.022(3) -0.002(3) 0.010(3) C39 0.053(4) 0.137(8) 0.106(7) 0.056(6) -0.011(4) 0.023(5) C38 0.146(8) 0.075(5) 0.061(5) 0.001(4) 0.030(5) 0.000(5) C33 0.111(9) 0.141(10) 0.135(10) 0.045(8) 0.005(8) 0.010(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr O1 2.418(4) . ? Pr O10 2.424(4) . ? Pr O7 2.428(4) . ? Pr O3 2.432(4) . ? Pr O11 2.450(4) . ? Pr O12 2.464(4) . ? Pr O9 2.487(4) . ? Pr O8 2.490(4) . ? O12 C15 1.242(7) . ? O11 C13 1.232(7) . ? O3 N3 1.306(5) . ? O9 C10 1.242(7) . ? O7 C9 1.245(7) . ? O10 C12 1.240(7) . ? O8 C7 1.234(7) . ? N1 O1 1.317(6) . ? N1 C22 1.321(7) . ? N1 C16 1.486(7) . ? N3 C40 1.324(7) . ? N3 C34 1.507(7) . ? N2 O2 1.271(6) . ? N2 C22 1.359(7) . ? N2 C19 1.503(8) . ? C44 C49 1.409(8) . ? C44 C43 1.410(8) . ? C44 C45 1.422(8) . ? F13 C5 1.295(8) . ? O4 N4 1.267(6) . ? N4 C40 1.367(7) . ? N4 C37 1.496(8) . ? C42 C43 1.343(8) . ? C42 C41 1.423(8) . ? C42 H42 0.9300 . ? C40 C41 1.454(8) . ? C22 C24 1.454(9) . ? C15 C14 1.372(9) . ? C15 C4 1.532(9) . ? C16 C17 1.522(8) . ? C16 C18 1.524(9) . ? C16 C19 1.556(8) . ? C43 H43 0.9300 . ? C50 C41 1.378(8) . ? C50 C49 1.401(8) . ? C50 H50 0.9300 . ? F15 C5 1.335(8) . ? C5 F14 1.290(8) . ? C5 C9 1.534(8) . ? C9 C8 1.382(9) . ? C7 C8 1.389(8) . ? C7 C6 1.529(9) . ? C49 C48 1.415(9) . ? C20 C19 1.520(9) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C13 C14 1.390(9) . ? C13 C3 1.526(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? F2 C1 1.310(9) . ? C21 C19 1.528(8) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? F1 C1 1.265(9) . ? C12 C11 1.378(9) . ? C12 C2 1.508(9) . ? C34 C36 1.497(9) . ? C34 C35 1.536(9) . ? C34 C37 1.546(8) . ? C10 C11 1.381(9) . ? C10 C1 1.532(9) . ? F3 C1 1.313(9) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C23 C28 1.376(13) . ? C23 C24 1.410(11) . ? C23 H23 0.9300 . ? C11 H11 0.9300 . ? F9 C3 1.278(10) . ? C47 C48 1.339(10) . ? C47 C46 1.426(10) . ? C47 H47 0.9300 . ? F6 C2 1.214(10) . ? C31 C30 1.434(17) . ? C31 C32 1.523(16) . ? C31 H31 0.9300 . ? O5 C46 1.362(8) . ? O5 C51 1.409(10) . ? C45 C46 1.346(9) . ? C45 H45 0.9300 . ? C8 H8 0.9300 . ? C4 F11 1.284(10) . ? C4 F10 1.286(10) . ? C4 F12 1.286(10) . ? C14 H14 0.9300 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C3 F8 1.197(11) . ? C3 F7 1.352(14) . ? C24 C25 1.376(11) . ? C2 F5 1.230(12) . ? C2 F4 1.250(11) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C27 C28 1.231(14) . ? C27 C26 1.371(13) . ? C27 C29 1.631(15) . ? C28 H28 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C25 C26 1.582(13) . ? C25 H25 0.9300 . ? C29 C30 1.297(17) . ? C29 H29 0.9300 . ? C48 H48 0.9300 . ? F16 C6 1.230(9) . ? F18 C6 1.248(10) . ? C6 F17 1.295(10) . ? C32 C26 1.282(14) . ? C32 H32 0.9300 . ? C30 O6 1.466(14) . ? O6 C33 1.326(14) . ? C37 C39 1.522(10) . ? C37 C38 1.541(11) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? 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 O1 Pr O10 93.62(14) . . ? O1 Pr O7 102.22(14) . . ? O10 Pr O7 134.01(14) . . ? O1 Pr O3 140.14(13) . . ? O10 Pr O3 103.74(14) . . ? O7 Pr O3 91.11(13) . . ? O1 Pr O11 75.81(14) . . ? O10 Pr O11 72.88(14) . . ? O7 Pr O11 152.80(14) . . ? O3 Pr O11 75.56(13) . . ? O1 Pr O12 69.68(13) . . ? O10 Pr O12 142.61(13) . . ? O7 Pr O12 83.10(13) . . ? O3 Pr O12 75.01(12) . . ? O11 Pr O12 70.68(13) . . ? O1 Pr O9 145.01(14) . . ? O10 Pr O9 69.92(13) . . ? O7 Pr O9 72.68(14) . . ? O3 Pr O9 74.79(13) . . ? O11 Pr O9 124.28(13) . . ? O12 Pr O9 140.52(13) . . ? O1 Pr O8 72.49(13) . . ? O10 Pr O8 73.75(14) . . ? O7 Pr O8 70.59(13) . . ? O3 Pr O8 146.70(13) . . ? O11 Pr O8 131.67(13) . . ? O12 Pr O8 127.34(13) . . ? O9 Pr O8 73.27(13) . . ? C15 O12 Pr 132.0(4) . . ? C13 O11 Pr 133.8(4) . . ? N3 O3 Pr 136.5(3) . . ? C10 O9 Pr 133.2(4) . . ? C9 O7 Pr 133.9(4) . . ? C12 O10 Pr 136.2(4) . . ? C7 O8 Pr 132.4(4) . . ? O1 N1 C22 126.1(5) . . ? O1 N1 C16 118.9(4) . . ? C22 N1 C16 114.1(4) . . ? N1 O1 Pr 138.2(3) . . ? O3 N3 C40 126.1(5) . . ? O3 N3 C34 120.3(4) . . ? C40 N3 C34 113.2(4) . . ? O2 N2 C22 126.1(5) . . ? O2 N2 C19 121.9(5) . . ? C22 N2 C19 111.6(4) . . ? C49 C44 C43 117.9(5) . . ? C49 C44 C45 119.1(5) . . ? C43 C44 C45 123.0(5) . . ? O4 N4 C40 125.6(5) . . ? O4 N4 C37 121.9(5) . . ? C40 N4 C37 112.1(5) . . ? C43 C42 C41 120.4(6) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? N3 C40 N4 107.6(5) . . ? N3 C40 C41 126.6(5) . . ? N4 C40 C41 125.7(5) . . ? N1 C22 N2 107.6(5) . . ? N1 C22 C24 126.2(6) . . ? N2 C22 C24 126.2(6) . . ? O12 C15 C14 129.7(6) . . ? O12 C15 C4 113.9(6) . . ? C14 C15 C4 116.5(6) . . ? N1 C16 C17 110.7(5) . . ? N1 C16 C18 106.1(5) . . ? C17 C16 C18 111.0(6) . . ? N1 C16 C19 99.3(4) . . ? C17 C16 C19 114.9(6) . . ? C18 C16 C19 113.9(5) . . ? C42 C43 C44 122.2(6) . . ? C42 C43 H43 118.9 . . ? C44 C43 H43 118.9 . . ? C41 C50 C49 121.3(5) . . ? C41 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? F14 C5 F13 107.3(6) . . ? F14 C5 F15 104.8(6) . . ? F13 C5 F15 107.0(6) . . ? F14 C5 C9 113.5(6) . . ? F13 C5 C9 114.4(6) . . ? F15 C5 C9 109.3(6) . . ? O7 C9 C8 128.2(5) . . ? O7 C9 C5 114.7(6) . . ? C8 C9 C5 117.0(5) . . ? C50 C41 C42 118.6(5) . . ? C50 C41 C40 121.1(5) . . ? C42 C41 C40 120.2(5) . . ? O8 C7 C8 128.4(6) . . ? O8 C7 C6 114.3(5) . . ? C8 C7 C6 117.2(5) . . ? C50 C49 C44 119.6(5) . . ? C50 C49 C48 121.5(5) . . ? C44 C49 C48 118.9(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O11 C13 C14 128.3(6) . . ? O11 C13 C3 114.9(7) . . ? C14 C13 C3 116.8(7) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O10 C12 C11 127.5(6) . . ? O10 C12 C2 113.8(6) . . ? C11 C12 C2 118.6(6) . . ? C36 C34 N3 111.0(5) . . ? C36 C34 C35 110.9(6) . . ? N3 C34 C35 104.9(5) . . ? C36 C34 C37 116.0(6) . . ? N3 C34 C37 99.8(5) . . ? C35 C34 C37 113.1(6) . . ? O9 C10 C11 128.0(5) . . ? O9 C10 C1 113.6(6) . . ? C11 C10 C1 118.4(6) . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C28 C23 C24 127.9(11) . . ? C28 C23 H23 116.0 . . ? C24 C23 H23 116.0 . . ? C12 C11 C10 122.7(6) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? N2 C19 C20 106.6(5) . . ? N2 C19 C21 109.1(5) . . ? C20 C19 C21 110.7(6) . . ? N2 C19 C16 100.7(4) . . ? C20 C19 C16 113.8(5) . . ? C21 C19 C16 115.0(6) . . ? C48 C47 C46 120.7(7) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C30 C31 C32 122.3(12) . . ? C30 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C46 O5 C51 117.7(6) . . ? C46 C45 C44 120.5(6) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C9 C8 C7 122.5(5) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? F11 C4 F10 106.7(8) . . ? F11 C4 F12 103.8(9) . . ? F10 C4 F12 106.2(8) . . ? F11 C4 C15 111.5(7) . . ? F10 C4 C15 115.5(8) . . ? F12 C4 C15 112.3(7) . . ? C15 C14 C13 121.9(6) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? O5 C51 H51A 109.5 . . ? O5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? F8 C3 F9 114.4(10) . . ? F8 C3 F7 101.9(10) . . ? F9 C3 F7 95.8(10) . . ? F8 C3 C13 115.9(9) . . ? F9 C3 C13 115.3(7) . . ? F7 C3 C13 110.6(9) . . ? C25 C24 C23 118.9(8) . . ? C25 C24 C22 122.2(8) . . ? C23 C24 C22 118.8(7) . . ? F6 C2 F5 104.4(10) . . ? F6 C2 F4 104.0(11) . . ? F5 C2 F4 103.1(10) . . ? F6 C2 C12 116.2(7) . . ? F5 C2 C12 111.2(9) . . ? F4 C2 C12 116.5(8) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C28 C27 C26 128.2(12) . . ? C28 C27 C29 111.1(12) . . ? C26 C27 C29 120.7(11) . . ? C27 C28 C23 114.4(13) . . ? C27 C28 H28 122.8 . . ? C23 C28 H28 122.8 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C24 C25 C26 111.6(9) . . ? C24 C25 H25 124.2 . . ? C26 C25 H25 124.2 . . ? C30 C29 C27 105.2(13) . . ? C30 C29 H29 127.4 . . ? C27 C29 H29 127.4 . . ? C45 C46 O5 126.1(7) . . ? C45 C46 C47 120.1(6) . . ? O5 C46 C47 113.8(6) . . ? C47 C48 C49 120.7(6) . . ? C47 C48 H48 119.6 . . ? C49 C48 H48 119.6 . . ? F16 C6 F18 109.1(9) . . ? F16 C6 F17 103.5(9) . . ? F18 C6 F17 101.6(8) . . ? F16 C6 C7 116.9(7) . . ? F18 C6 C7 111.7(8) . . ? F17 C6 C7 112.7(7) . . ? C26 C32 C31 107.3(12) . . ? C26 C32 H32 126.3 . . ? C31 C32 H32 126.3 . . ? F1 C1 F2 108.2(8) . . ? F1 C1 F3 108.5(8) . . ? F2 C1 F3 102.7(7) . . ? F1 C1 C10 111.2(6) . . ? F2 C1 C10 112.5(6) . . ? F3 C1 C10 113.3(7) . . ? C32 C26 C27 133.2(12) . . ? C32 C26 C25 107.9(11) . . ? C27 C26 C25 118.8(9) . . ? C29 C30 C31 131.2(14) . . ? C29 C30 O6 120.2(14) . . ? C31 C30 O6 108.6(12) . . ? C33 O6 C30 119.7(11) . . ? N4 C37 C39 109.6(6) . . ? N4 C37 C38 105.7(6) . . ? C39 C37 C38 110.9(7) . . ? N4 C37 C34 101.3(4) . . ? C39 C37 C34 116.1(7) . . ? C38 C37 C34 112.2(6) . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O6 C33 H33A 109.5 . . ? O6 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O6 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.361 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.087 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 861122' #TrackingRef 'shelxl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H21 N2 O3' _chemical_formula_weight 313.37 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 29.00(2) _cell_length_b 11.358(8) _cell_length_c 20.024(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.977(9) _cell_angle_gamma 90.00 _cell_volume 6531(8) _cell_formula_units_Z 16 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 13677 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 27.91 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.983 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 41194 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.0843 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.01 _reflns_number_total 11306 _reflns_number_gt 8090 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+14.5013P] 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 SHELXL _refine_ls_extinction_coef 0.0099(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11306 _refine_ls_number_parameters 851 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1363 _refine_ls_R_factor_gt 0.1015 _refine_ls_wR_factor_ref 0.2550 _refine_ls_wR_factor_gt 0.2319 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.03359(9) 1.1791(2) 0.65213(13) 0.0352(7) Uani 1 1 d . . . C2B C 1.01731(17) 1.2816(4) 0.6918(2) 0.0458(5) Uani 0.685(6) 1 d PU A 2 H2BB H 0.9986 1.3338 0.6616 0.069 Uiso 0.685(6) 1 calc PR A 2 H2BC H 1.0439 1.3235 0.7139 0.069 Uiso 0.685(6) 1 calc PR A 2 H2BA H 0.9992 1.2523 0.7249 0.069 Uiso 0.685(6) 1 calc PR A 2 C3 C 1.05509(12) 1.2256(3) 0.59151(15) 0.0545(9) Uani 1 1 d . A . H3B H 1.0665 1.1608 0.5678 0.082 Uiso 1 1 calc R . . H3C H 1.0803 1.2779 0.6070 0.082 Uiso 1 1 calc R . . H3A H 1.0318 1.2674 0.5618 0.082 Uiso 1 1 calc R . . C4 C 1.06424(9) 1.0859(2) 0.69431(13) 0.0351(7) Uani 1 1 d . A . C5 C 1.05357(11) 1.0762(3) 0.76755(13) 0.0479(9) Uani 1 1 d . . . H5A H 1.0206 1.0689 0.7674 0.072 Uiso 1 1 calc R A . H5C H 1.0646 1.1456 0.7922 0.072 Uiso 1 1 calc R . . H5B H 1.0689 1.0082 0.7887 0.072 Uiso 1 1 calc R . . C6B C 1.11620(16) 1.0960(4) 0.6903(2) 0.0458(5) Uani 0.685(6) 1 d PU A 2 H6BB H 1.1328 1.0386 0.7194 0.069 Uiso 0.685(6) 1 calc PR A 2 H6BC H 1.1268 1.1735 0.7041 0.069 Uiso 0.685(6) 1 calc PR A 2 H6BA H 1.1217 1.0824 0.6447 0.069 Uiso 0.685(6) 1 calc PR A 2 C7 C 1.00186(9) 0.9876(2) 0.62760(12) 0.0341(7) Uani 1 1 d . . . C8 C 0.96981(9) 0.8924(2) 0.60570(12) 0.0360(7) Uani 1 1 d . A . C9 C 0.92143(9) 0.9115(3) 0.60418(13) 0.0410(8) Uani 1 1 d . . . H9 H 0.9109 0.9858 0.6142 0.049 Uiso 1 1 calc R A . C10 C 0.88975(10) 0.8224(3) 0.58817(14) 0.0426(8) Uani 1 1 d . A . H10 H 0.8581 0.8375 0.5870 0.051 Uiso 1 1 calc R . . C11 C 0.90481(9) 0.7074(2) 0.57332(12) 0.0324(7) Uani 1 1 d . . . C12 C 0.87270(9) 0.6136(2) 0.55809(12) 0.0346(7) Uani 1 1 d . A . H12 H 0.8410 0.6270 0.5571 0.042 Uiso 1 1 calc R . . C13 C 0.88850(9) 0.5031(2) 0.54485(13) 0.0351(7) Uani 1 1 d . . . C14 C 0.93656(10) 0.4819(3) 0.54677(13) 0.0389(7) Uani 1 1 d . A . H14 H 0.9470 0.4068 0.5382 0.047 Uiso 1 1 calc R . . C15 C 0.96786(9) 0.5716(2) 0.56126(12) 0.0358(7) Uani 1 1 d . . . H15 H 0.9995 0.5566 0.5625 0.043 Uiso 1 1 calc R A . C16 C 0.95286(9) 0.6869(2) 0.57444(11) 0.0318(7) Uani 1 1 d . A . C17 C 0.98531(10) 0.7801(2) 0.59088(12) 0.0360(7) Uani 1 1 d . . . H17 H 1.0170 0.7662 0.5918 0.043 Uiso 1 1 calc R A . C18 C 0.81190(10) 0.4201(3) 0.52819(16) 0.0498(9) Uani 1 1 d . . . H18B H 0.8008 0.4798 0.4960 0.075 Uiso 1 1 calc R A . H18C H 0.8053 0.4430 0.5721 0.075 Uiso 1 1 calc R . . H18A H 0.7965 0.3470 0.5155 0.075 Uiso 1 1 calc R . . C19 C 0.87064(9) 1.1000(2) 0.78553(13) 0.0336(7) Uani 1 1 d . . . C20 C 0.92318(9) 1.0953(3) 0.78508(16) 0.0477(9) Uani 1 1 d . . . H20B H 0.9363 1.0329 0.8140 0.072 Uiso 1 1 calc R . . H20C H 0.9368 1.1689 0.8009 0.072 Uiso 1 1 calc R . . H20A H 0.9295 1.0812 0.7400 0.072 Uiso 1 1 calc R . . C21 C 0.86084(12) 1.1070(3) 0.85847(14) 0.0501(9) Uani 1 1 d . . . H21A H 0.8278 1.1091 0.8592 0.075 Uiso 1 1 calc R . . H21C H 0.8748 1.1770 0.8792 0.075 Uiso 1 1 calc R . . H21B H 0.8738 1.0392 0.8829 0.075 Uiso 1 1 calc R . . C22 C 0.84387(9) 1.1927(2) 0.73690(13) 0.0351(7) Uani 1 1 d . . . C23 C 0.81820(10) 1.2864(3) 0.77148(15) 0.0463(8) Uani 1 1 d . . . H23B H 0.8026 1.3391 0.7382 0.069 Uiso 1 1 calc R . . H23C H 0.8401 1.3298 0.8025 0.069 Uiso 1 1 calc R . . H23A H 0.7957 1.2496 0.7955 0.069 Uiso 1 1 calc R . . C24 C 0.87300(10) 1.2504(3) 0.68804(15) 0.0489(9) Uani 1 1 d . . . H24B H 0.8876 1.1906 0.6644 0.073 Uiso 1 1 calc R . . H24C H 0.8965 1.2992 0.7128 0.073 Uiso 1 1 calc R . . H24A H 0.8532 1.2978 0.6563 0.073 Uiso 1 1 calc R . . C25 C 0.81509(9) 1.0007(2) 0.70680(13) 0.0339(7) Uani 1 1 d . . . C26 C 0.78891(8) 0.9064(2) 0.66911(12) 0.0321(7) Uani 1 1 d . . . C27 C 0.76915(9) 0.9250(3) 0.60082(13) 0.0377(7) Uani 1 1 d . . . H27 H 0.7722 0.9980 0.5808 0.045 Uiso 1 1 calc R . . C28 C 0.74568(9) 0.8360(3) 0.56441(13) 0.0361(7) Uani 1 1 d . . . H28 H 0.7329 0.8500 0.5199 0.043 Uiso 1 1 calc R . . C29 C 0.74038(8) 0.7237(3) 0.59266(12) 0.0338(7) Uani 1 1 d . . . C30 C 0.71606(10) 0.6318(3) 0.55592(14) 0.0419(8) Uani 1 1 d . . . H30 H 0.7029 0.6444 0.5115 0.050 Uiso 1 1 calc R . . C31 C 0.71165(10) 0.5249(3) 0.58479(13) 0.0411(8) Uani 1 1 d . . . C32 C 0.73235(9) 0.5030(3) 0.65222(13) 0.0383(7) Uani 1 1 d . . . H32 H 0.7293 0.4294 0.6715 0.046 Uiso 1 1 calc R . . C33 C 0.75639(9) 0.5891(3) 0.68826(13) 0.0362(7) Uani 1 1 d . . . H33 H 0.7704 0.5731 0.7320 0.043 Uiso 1 1 calc R . . C34 C 0.76083(9) 0.7048(3) 0.66071(12) 0.0337(7) Uani 1 1 d . . . C35 C 0.78453(9) 0.7964(3) 0.69751(12) 0.0354(7) Uani 1 1 d . . . H35 H 0.7976 0.7833 0.7420 0.043 Uiso 1 1 calc R . . C36 C 0.66224(13) 0.4496(3) 0.48800(17) 0.0707(12) Uani 1 1 d . . . H36C H 0.6839 0.4604 0.4563 0.106 Uiso 1 1 calc R . . H36B H 0.6430 0.5184 0.4883 0.106 Uiso 1 1 calc R . . H36A H 0.6430 0.3824 0.4751 0.106 Uiso 1 1 calc R . . C37 C 0.65737(9) 1.1098(2) 0.76566(14) 0.0378(7) Uani 1 1 d . . . C38 C 0.63321(10) 1.1714(3) 0.81874(14) 0.0471(8) Uani 1 1 d . . . H38A H 0.6099 1.2240 0.7970 0.071 Uiso 1 1 calc R . . H38C H 0.6557 1.2152 0.8485 0.071 Uiso 1 1 calc R . . H38B H 0.6188 1.1138 0.8441 0.071 Uiso 1 1 calc R . . C39 C 0.67801(10) 1.2020(3) 0.72324(16) 0.0510(9) Uani 1 1 d . . . H39B H 0.6989 1.1646 0.6965 0.076 Uiso 1 1 calc R . . H39C H 0.6948 1.2593 0.7523 0.076 Uiso 1 1 calc R . . H39A H 0.6534 1.2402 0.6941 0.076 Uiso 1 1 calc R . . C40 C 0.62800(10) 1.0120(3) 0.72513(14) 0.0411(8) Uani 1 1 d . . . C41 C 0.57569(10) 1.0192(3) 0.72712(16) 0.0475(9) Uani 1 1 d . . . H41B H 0.5636 1.0901 0.7051 0.071 Uiso 1 1 calc R . . H41C H 0.5699 1.0198 0.7732 0.071 Uiso 1 1 calc R . . H41A H 0.5606 0.9523 0.7043 0.071 Uiso 1 1 calc R . . C42 C 0.63729(13) 0.9984(4) 0.65206(15) 0.0648(11) Uani 1 1 d . . . H42A H 0.6202 0.9321 0.6318 0.097 Uiso 1 1 calc R . . H42C H 0.6700 0.9862 0.6514 0.097 Uiso 1 1 calc R . . H42B H 0.6275 1.0684 0.6272 0.097 Uiso 1 1 calc R . . C43 C 0.68795(9) 0.9203(2) 0.80076(13) 0.0340(7) Uani 1 1 d . . . C44 C 0.71764(9) 0.8284(3) 0.83439(12) 0.0354(7) Uani 1 1 d . . . C45 C 0.70531(9) 0.7104(2) 0.82810(13) 0.0353(7) Uani 1 1 d . . . H45 H 0.6771 0.6901 0.8028 0.042 Uiso 1 1 calc R . . C46 C 0.73425(9) 0.6203(2) 0.85895(12) 0.0339(7) Uani 1 1 d . . . C47 C 0.72207(9) 0.4997(3) 0.85108(14) 0.0397(7) Uani 1 1 d . . . H47 H 0.6941 0.4791 0.8252 0.048 Uiso 1 1 calc R . . C48 C 0.75039(9) 0.4135(3) 0.88061(13) 0.0385(7) Uani 1 1 d . . . H48 H 0.7417 0.3350 0.8745 0.046 Uiso 1 1 calc R . . C49 C 0.79324(9) 0.4427(3) 0.92082(12) 0.0369(7) Uani 1 1 d . . . C50 C 0.80607(9) 0.5585(2) 0.92957(13) 0.0352(7) Uani 1 1 d . . . H50 H 0.8338 0.5779 0.9564 0.042 Uiso 1 1 calc R . . C51 C 0.77723(9) 0.6489(2) 0.89790(12) 0.0332(7) Uani 1 1 d . . . C52 C 0.78991(10) 0.7701(3) 0.90415(13) 0.0385(7) Uani 1 1 d . . . H52 H 0.8181 0.7911 0.9294 0.046 Uiso 1 1 calc R . . C53 C 0.76164(9) 0.8551(3) 0.87403(13) 0.0369(7) Uani 1 1 d . . . H53 H 0.7710 0.9333 0.8791 0.044 Uiso 1 1 calc R . . C54 C 0.86237(11) 0.3716(3) 0.98833(16) 0.0553(9) Uani 1 1 d . . . H54A H 0.8822 0.4130 0.9617 0.083 Uiso 1 1 calc R . . H54B H 0.8768 0.2985 1.0037 0.083 Uiso 1 1 calc R . . H54C H 0.8575 0.4188 1.0265 0.083 Uiso 1 1 calc R . . C55 C 0.46840(9) 1.0961(3) 0.85958(14) 0.0403(8) Uani 1 1 d . . . C56B C 0.45074(15) 1.1213(4) 0.9277(2) 0.0458(5) Uani 0.685(6) 1 d PU A 2 H56B H 0.4253 1.1759 0.9208 0.069 Uiso 0.685(6) 1 calc PR A 2 H56C H 0.4756 1.1543 0.9588 0.069 Uiso 0.685(6) 1 calc PR A 2 H56A H 0.4404 1.0491 0.9458 0.069 Uiso 0.685(6) 1 calc PR A 2 C57 C 0.48362(11) 1.2036(3) 0.82367(18) 0.0585(10) Uani 1 1 d . A . H57A H 0.4981 1.1793 0.7856 0.088 Uiso 1 1 calc R . . H57C H 0.5055 1.2481 0.8541 0.088 Uiso 1 1 calc R . . H57B H 0.4570 1.2516 0.8085 0.088 Uiso 1 1 calc R . . C58 C 0.43604(10) 1.0115(3) 0.81415(14) 0.0426(8) Uani 1 1 d . A . C59 C 0.44053(12) 1.0226(3) 0.73873(15) 0.0549(10) Uani 1 1 d . . . H59A H 0.4240 0.9592 0.7143 0.082 Uiso 1 1 calc R A . H59C H 0.4728 1.0190 0.7328 0.082 Uiso 1 1 calc R . . H59B H 0.4276 1.0964 0.7219 0.082 Uiso 1 1 calc R . . C60 C 0.38522(10) 1.0150(3) 0.82308(18) 0.0573(10) Uani 1 1 d . . . H60B H 0.3733 1.0930 0.8138 0.086 Uiso 1 1 calc R A . H60C H 0.3819 0.9938 0.8686 0.086 Uiso 1 1 calc R . . H60A H 0.3681 0.9603 0.7925 0.086 Uiso 1 1 calc R . . C61 C 0.50035(9) 0.9028(3) 0.87061(12) 0.0368(7) Uani 1 1 d . . . C62 C 0.53228(9) 0.8053(2) 0.89184(13) 0.0355(7) Uani 1 1 d . A . C63 C 0.58063(10) 0.8251(3) 0.90053(14) 0.0427(8) Uani 1 1 d . . . H63 H 0.5920 0.8991 0.8915 0.051 Uiso 1 1 calc R A . C64 C 0.61138(10) 0.7357(3) 0.92233(15) 0.0451(8) Uani 1 1 d . A . H64 H 0.6432 0.7510 0.9278 0.054 Uiso 1 1 calc R . . C65 C 0.59606(10) 0.6228(3) 0.93647(13) 0.0388(7) Uani 1 1 d . . . C66 C 0.62723(10) 0.5310(3) 0.96124(14) 0.0411(8) Uani 1 1 d . A . H66 H 0.6591 0.5448 0.9684 0.049 Uiso 1 1 calc R . . C67 C 0.61016(11) 0.4223(3) 0.97449(14) 0.0475(9) Uani 1 1 d . . . C68 C 0.56206(11) 0.3974(3) 0.96094(17) 0.0557(10) Uani 1 1 d . A . H68 H 0.5512 0.3220 0.9681 0.067 Uiso 1 1 calc R . . C69 C 0.53163(11) 0.4842(3) 0.93738(16) 0.0491(9) Uani 1 1 d . . . H69 H 0.5000 0.4671 0.9289 0.059 Uiso 1 1 calc R A . C70 C 0.54702(10) 0.6004(3) 0.92549(14) 0.0402(8) Uani 1 1 d . A . C71 C 0.51587(10) 0.6929(3) 0.90338(13) 0.0398(8) Uani 1 1 d . . . H71 H 0.4840 0.6783 0.8965 0.048 Uiso 1 1 calc R A . C72 C 0.68643(10) 0.3501(3) 1.01955(16) 0.0543(9) Uani 1 1 d . . . H72A H 0.7000 0.3710 0.9801 0.081 Uiso 1 1 calc R A . H72B H 0.7011 0.2801 1.0392 0.081 Uiso 1 1 calc R . . H72C H 0.6909 0.4133 1.0517 0.081 Uiso 1 1 calc R . . N1 N 1.04603(7) 0.9749(2) 0.66068(10) 0.0341(6) Uani 1 1 d . A . N2 N 0.99261(8) 1.1045(2) 0.62365(11) 0.0369(6) Uani 1 1 d . A . N3 N 0.85062(7) 0.9855(2) 0.75688(11) 0.0358(6) Uani 1 1 d . . . N4 N 0.80848(7) 1.1169(2) 0.69497(11) 0.0373(6) Uani 1 1 d . . . N5 N 0.69650(8) 1.0377(2) 0.80292(12) 0.0409(6) Uani 1 1 d . . . N6 N 0.64702(7) 0.9028(2) 0.76026(11) 0.0363(6) Uani 1 1 d . . . N7 N 0.50973(8) 1.0187(2) 0.88149(11) 0.0393(6) Uani 1 1 d . A . N8 N 0.45658(8) 0.8939(2) 0.83641(12) 0.0416(6) Uani 1 1 d . A . O1 O 1.06788(7) 0.87689(17) 0.67220(11) 0.0474(6) Uani 1 1 d . . . O2 O 0.95550(7) 1.15183(19) 0.59258(11) 0.0518(6) Uani 1 1 d . . . O3 O 0.86765(7) 0.88721(17) 0.77999(10) 0.0465(6) Uani 1 1 d . . . O4 O 0.77696(7) 1.16415(19) 0.65203(10) 0.0517(6) Uani 1 1 d . . . O5 O 0.73198(7) 1.0898(2) 0.83636(13) 0.0658(7) Uani 1 1 d . . . O6 O 0.62635(7) 0.80426(19) 0.74599(11) 0.0549(6) Uani 1 1 d . . . O7 O 0.54720(7) 1.0624(2) 0.91430(11) 0.0545(6) Uani 1 1 d . . . O8 O 0.43575(7) 0.79712(19) 0.81718(11) 0.0545(6) Uani 1 1 d . . . O9 O 0.86090(7) 0.40599(17) 0.52977(10) 0.0419(5) Uani 1 1 d . A . O10 O 0.68750(8) 0.43106(19) 0.55448(10) 0.0534(6) Uani 1 1 d . . . O11 O 0.81832(7) 0.34827(18) 0.94807(10) 0.0452(6) Uani 1 1 d . . . O12 O 0.63679(8) 0.32879(19) 1.00093(11) 0.0555(6) Uani 1 1 d . A . C6A C 1.1161(4) 1.1012(10) 0.7040(5) 0.0458(5) Uani 0.315(6) 1 d PU A 1 H6AB H 1.1304 1.0397 0.7326 0.069 Uiso 0.315(6) 1 calc PR A 1 H6AC H 1.1240 1.1763 0.7246 0.069 Uiso 0.315(6) 1 calc PR A 1 H6AA H 1.1272 1.0976 0.6611 0.069 Uiso 0.315(6) 1 calc PR A 1 C2A C 1.0175(4) 1.2797(11) 0.6919(6) 0.0458(5) Uani 0.315(6) 1 d PU A 1 H2AB H 0.9991 1.3328 0.6620 0.069 Uiso 0.315(6) 1 calc PR A 1 H2AC H 1.0441 1.3206 0.7148 0.069 Uiso 0.315(6) 1 calc PR A 1 H2AA H 0.9991 1.2497 0.7245 0.069 Uiso 0.315(6) 1 calc PR A 1 C56A C 0.4502(4) 1.1649(9) 0.9152(5) 0.0458(5) Uani 0.315(6) 1 d PU A 1 H56E H 0.4306 1.2276 0.8959 0.069 Uiso 0.315(6) 1 calc PR A 1 H56F H 0.4760 1.1972 0.9449 0.069 Uiso 0.315(6) 1 calc PR A 1 H56D H 0.4326 1.1135 0.9402 0.069 Uiso 0.315(6) 1 calc PR A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0397(13) 0.0297(14) 0.0359(13) 0.0007(11) 0.0040(11) -0.0004(12) C2B 0.0474(10) 0.0355(11) 0.0541(11) -0.0036(9) 0.0049(9) 0.0038(9) C3 0.0651(19) 0.048(2) 0.0518(17) 0.0049(15) 0.0121(15) 0.0015(17) C4 0.0344(13) 0.0317(15) 0.0378(13) -0.0084(11) -0.0002(11) -0.0030(12) C5 0.0567(17) 0.0532(19) 0.0316(13) -0.0017(13) -0.0013(13) 0.0071(16) C6B 0.0474(10) 0.0355(11) 0.0541(11) -0.0036(9) 0.0049(9) 0.0038(9) C7 0.0415(14) 0.0297(14) 0.0293(12) -0.0077(11) -0.0014(11) 0.0088(12) C8 0.0426(14) 0.0337(15) 0.0291(12) -0.0034(11) -0.0041(11) 0.0071(12) C9 0.0402(14) 0.0370(16) 0.0425(14) -0.0091(13) -0.0064(12) 0.0084(13) C10 0.0375(14) 0.0447(17) 0.0426(14) -0.0095(13) -0.0056(12) 0.0122(13) C11 0.0347(13) 0.0355(15) 0.0253(11) -0.0011(11) -0.0023(10) 0.0076(12) C12 0.0324(12) 0.0397(16) 0.0308(12) -0.0022(12) 0.0011(10) 0.0072(12) C13 0.0390(13) 0.0292(14) 0.0365(13) -0.0033(12) 0.0036(11) 0.0019(12) C14 0.0442(14) 0.0310(15) 0.0414(14) -0.0032(12) 0.0057(12) 0.0080(13) C15 0.0311(13) 0.0379(16) 0.0374(13) -0.0060(12) 0.0012(11) 0.0063(12) C16 0.0409(13) 0.0307(14) 0.0229(11) -0.0038(10) 0.0017(10) 0.0035(12) C17 0.0385(13) 0.0369(15) 0.0306(12) -0.0054(11) -0.0024(11) 0.0063(12) C18 0.0405(15) 0.0404(18) 0.0672(19) -0.0017(15) 0.0029(14) -0.0006(14) C19 0.0338(13) 0.0241(13) 0.0416(13) -0.0053(11) 0.0006(11) -0.0012(11) C20 0.0319(14) 0.0385(17) 0.0700(19) -0.0009(15) -0.0029(14) -0.0008(13) C21 0.0655(19) 0.0457(18) 0.0368(14) -0.0017(14) -0.0015(14) 0.0039(16) C22 0.0287(12) 0.0340(15) 0.0406(13) -0.0005(12) -0.0018(11) -0.0020(12) C23 0.0454(16) 0.0356(16) 0.0555(17) -0.0062(14) -0.0016(14) 0.0036(14) C24 0.0487(16) 0.0491(19) 0.0470(15) 0.0076(15) -0.0005(13) -0.0112(15) C25 0.0265(12) 0.0363(15) 0.0381(13) -0.0012(12) 0.0009(10) 0.0016(12) C26 0.0230(11) 0.0361(15) 0.0367(12) -0.0034(12) 0.0022(10) -0.0020(11) C27 0.0338(13) 0.0405(16) 0.0383(13) 0.0020(12) 0.0033(11) 0.0002(12) C28 0.0338(13) 0.0414(16) 0.0315(12) 0.0003(12) -0.0009(10) 0.0015(12) C29 0.0268(12) 0.0415(16) 0.0332(12) -0.0073(12) 0.0038(10) -0.0034(12) C30 0.0425(15) 0.0439(17) 0.0367(13) -0.0056(13) -0.0039(12) 0.0000(14) C31 0.0410(14) 0.0449(18) 0.0363(13) -0.0088(13) 0.0018(12) -0.0018(13) C32 0.0333(13) 0.0393(16) 0.0413(14) -0.0031(13) 0.0021(11) -0.0058(12) C33 0.0368(13) 0.0397(16) 0.0312(12) -0.0023(12) 0.0016(11) -0.0034(12) C34 0.0295(12) 0.0382(15) 0.0339(12) -0.0049(12) 0.0065(10) -0.0047(12) C35 0.0308(12) 0.0451(17) 0.0293(12) -0.0016(12) 0.0006(10) -0.0029(12) C36 0.084(2) 0.058(2) 0.0588(19) -0.0003(17) -0.0297(18) -0.022(2) C37 0.0270(12) 0.0336(15) 0.0504(15) 0.0138(13) -0.0030(11) 0.0035(12) C38 0.0440(15) 0.0475(18) 0.0466(15) 0.0026(14) -0.0044(13) 0.0022(14) C39 0.0414(15) 0.0443(18) 0.0649(18) 0.0162(15) -0.0011(14) -0.0038(14) C40 0.0403(14) 0.0362(16) 0.0434(14) 0.0082(13) -0.0062(12) 0.0003(13) C41 0.0365(14) 0.0358(17) 0.0656(18) 0.0079(15) -0.0088(14) -0.0009(13) C42 0.080(2) 0.069(2) 0.0433(17) 0.0030(17) 0.0021(16) -0.002(2) C43 0.0313(12) 0.0311(15) 0.0385(13) 0.0025(12) 0.0009(11) 0.0006(12) C44 0.0331(13) 0.0420(16) 0.0309(12) 0.0008(12) 0.0032(10) 0.0017(12) C45 0.0314(13) 0.0308(15) 0.0426(14) -0.0062(12) 0.0007(11) -0.0005(12) C46 0.0348(13) 0.0340(15) 0.0328(12) 0.0016(11) 0.0048(10) 0.0038(12) C47 0.0337(13) 0.0411(16) 0.0427(14) -0.0016(13) -0.0003(11) 0.0027(13) C48 0.0436(14) 0.0287(15) 0.0427(14) 0.0030(12) 0.0041(12) -0.0004(12) C49 0.0383(13) 0.0402(16) 0.0323(12) 0.0034(12) 0.0047(11) 0.0085(13) C50 0.0342(13) 0.0340(15) 0.0361(13) 0.0006(12) -0.0002(11) 0.0013(12) C51 0.0366(13) 0.0347(15) 0.0284(11) 0.0016(11) 0.0049(10) 0.0032(12) C52 0.0372(14) 0.0363(16) 0.0395(14) -0.0042(12) -0.0030(11) 0.0005(12) C53 0.0374(14) 0.0301(15) 0.0415(14) -0.0009(12) -0.0003(11) -0.0019(12) C54 0.0528(17) 0.0438(19) 0.0614(18) 0.0029(16) -0.0194(15) 0.0097(15) C55 0.0359(14) 0.0395(17) 0.0428(14) -0.0044(13) -0.0036(12) 0.0007(13) C56B 0.0474(10) 0.0355(11) 0.0541(11) -0.0036(9) 0.0049(9) 0.0038(9) C57 0.0509(18) 0.0366(18) 0.081(2) 0.0066(17) -0.0159(17) 0.0004(15) C58 0.0391(14) 0.0389(17) 0.0472(15) 0.0004(13) -0.0033(12) -0.0032(13) C59 0.0594(19) 0.051(2) 0.0497(17) 0.0022(15) -0.0067(15) 0.0002(17) C60 0.0372(15) 0.052(2) 0.081(2) 0.0114(18) 0.0016(15) 0.0015(15) C61 0.0360(13) 0.0404(16) 0.0324(12) -0.0012(12) -0.0009(11) 0.0001(13) C62 0.0373(13) 0.0356(15) 0.0324(12) 0.0011(12) 0.0003(11) 0.0016(12) C63 0.0398(14) 0.0427(17) 0.0449(14) 0.0117(13) 0.0038(12) -0.0011(13) C64 0.0351(14) 0.0460(18) 0.0535(16) 0.0080(14) 0.0034(13) 0.0013(14) C65 0.0452(15) 0.0376(16) 0.0326(12) 0.0010(12) 0.0017(11) 0.0005(13) C66 0.0388(14) 0.0395(17) 0.0441(14) 0.0054(13) 0.0023(12) 0.0038(13) C67 0.0560(17) 0.0411(18) 0.0415(15) -0.0022(13) -0.0069(14) 0.0028(15) C68 0.0518(18) 0.0435(19) 0.0669(19) 0.0057(16) -0.0084(16) -0.0045(15) C69 0.0465(16) 0.0371(17) 0.0600(18) 0.0046(15) -0.0059(14) -0.0069(14) C70 0.0427(15) 0.0357(16) 0.0402(14) -0.0038(13) -0.0012(12) -0.0019(13) C71 0.0352(13) 0.0416(17) 0.0402(14) -0.0043(13) -0.0033(11) -0.0036(13) C72 0.0447(16) 0.058(2) 0.0586(18) 0.0071(16) 0.0018(14) 0.0107(16) N1 0.0330(11) 0.0293(12) 0.0373(11) -0.0035(10) -0.0042(9) 0.0040(10) N2 0.0354(11) 0.0336(13) 0.0385(11) -0.0015(10) -0.0061(9) 0.0065(10) N3 0.0302(11) 0.0347(13) 0.0401(11) 0.0002(10) -0.0032(9) 0.0001(10) N4 0.0300(11) 0.0356(13) 0.0430(12) -0.0002(11) -0.0058(9) 0.0019(10) N5 0.0319(11) 0.0333(13) 0.0537(13) 0.0106(11) -0.0067(10) -0.0001(10) N6 0.0348(11) 0.0290(12) 0.0430(12) 0.0005(10) -0.0017(10) 0.0038(10) N7 0.0357(11) 0.0351(13) 0.0435(12) -0.0040(11) -0.0071(10) -0.0046(10) N8 0.0390(12) 0.0348(13) 0.0478(12) -0.0042(11) -0.0051(10) -0.0043(11) O1 0.0434(11) 0.0284(11) 0.0649(12) -0.0035(10) -0.0122(10) 0.0076(9) O2 0.0489(11) 0.0370(12) 0.0628(12) -0.0049(10) -0.0161(10) 0.0118(10) O3 0.0476(11) 0.0255(10) 0.0601(12) 0.0051(9) -0.0149(9) 0.0004(9) O4 0.0421(10) 0.0469(13) 0.0582(12) 0.0037(10) -0.0215(9) 0.0080(10) O5 0.0460(12) 0.0399(13) 0.1004(17) 0.0063(12) -0.0288(12) -0.0105(10) O6 0.0438(11) 0.0360(12) 0.0773(14) -0.0037(11) -0.0187(10) -0.0015(10) O7 0.0392(10) 0.0491(13) 0.0678(13) -0.0040(11) -0.0187(10) -0.0107(10) O8 0.0465(11) 0.0377(12) 0.0723(13) -0.0091(11) -0.0165(10) -0.0050(10) O9 0.0426(10) 0.0307(11) 0.0519(11) -0.0017(9) 0.0043(9) -0.0009(9) O10 0.0674(13) 0.0426(12) 0.0437(10) -0.0048(10) -0.0156(10) -0.0139(11) O11 0.0487(11) 0.0340(11) 0.0482(11) 0.0049(9) -0.0095(9) 0.0047(9) O12 0.0553(12) 0.0390(12) 0.0662(13) 0.0014(11) -0.0122(11) 0.0093(10) C6A 0.0474(10) 0.0355(11) 0.0541(11) -0.0036(9) 0.0049(9) 0.0038(9) C2A 0.0474(10) 0.0355(11) 0.0541(11) -0.0036(9) 0.0049(9) 0.0038(9) C56A 0.0474(10) 0.0355(11) 0.0541(11) -0.0036(9) 0.0049(9) 0.0038(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2A 1.504(13) . ? C1 N2 1.506(3) . ? C1 C2B 1.521(6) . ? C1 C3 1.534(4) . ? C1 C4 1.554(4) . ? C2B H2BB 0.9600 . ? C2B H2BC 0.9600 . ? C2B H2BA 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3 H3A 0.9600 . ? C4 N1 1.491(3) . ? C4 C6A 1.501(11) . ? C4 C6B 1.524(5) . ? C4 C5 1.544(4) . ? C5 H5A 0.9600 . ? C5 H5C 0.9600 . ? C5 H5B 0.9600 . ? C6B H6BB 0.9600 . ? C6B H6BC 0.9600 . ? C6B H6BA 0.9600 . ? C7 N2 1.354(4) . ? C7 N1 1.366(3) . ? C7 C8 1.453(4) . ? C8 C17 1.398(4) . ? C8 C9 1.416(4) . ? C9 C10 1.374(4) . ? C9 H9 0.9300 . ? C10 C11 1.422(4) . ? C10 H10 0.9300 . ? C11 C16 1.410(4) . ? C11 C12 1.420(4) . ? C12 C13 1.375(4) . ? C12 H12 0.9300 . ? C13 O9 1.371(3) . ? C13 C14 1.409(4) . ? C14 C15 1.369(4) . ? C14 H14 0.9300 . ? C15 C16 1.416(4) . ? C15 H15 0.9300 . ? C16 C17 1.425(4) . ? C17 H17 0.9300 . ? C18 O9 1.426(4) . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C18 H18A 0.9600 . ? C19 N3 1.505(3) . ? C19 C20 1.526(4) . ? C19 C21 1.528(4) . ? C19 C22 1.564(4) . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C20 H20A 0.9600 . ? C21 H21A 0.9600 . ? C21 H21C 0.9600 . ? C21 H21B 0.9600 . ? C22 N4 1.503(3) . ? C22 C23 1.520(4) . ? C22 C24 1.526(4) . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C23 H23A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C24 H24A 0.9600 . ? C25 N3 1.345(3) . ? C25 N4 1.351(4) . ? C25 C26 1.461(4) . ? C26 C35 1.385(4) . ? C26 C27 1.423(4) . ? C27 C28 1.370(4) . ? C27 H27 0.9300 . ? C28 C29 1.412(4) . ? C28 H28 0.9300 . ? C29 C30 1.409(4) . ? C29 C34 1.425(4) . ? C30 C31 1.359(4) . ? C30 H30 0.9300 . ? C31 O10 1.370(4) . ? C31 C32 1.421(4) . ? C32 C33 1.350(4) . ? C32 H32 0.9300 . ? C33 C34 1.438(4) . ? C33 H33 0.9300 . ? C34 C35 1.399(4) . ? C35 H35 0.9300 . ? C36 O10 1.443(4) . ? C36 H36C 0.9600 . ? C36 H36B 0.9600 . ? C36 H36A 0.9600 . ? C37 N5 1.510(3) . ? C37 C38 1.522(4) . ? C37 C39 1.522(4) . ? C37 C40 1.558(4) . ? C38 H38A 0.9600 . ? C38 H38C 0.9600 . ? C38 H38B 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C39 H39A 0.9600 . ? C40 N6 1.493(4) . ? C40 C41 1.525(4) . ? C40 C42 1.532(4) . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C41 H41A 0.9600 . ? C42 H42A 0.9600 . ? C42 H42C 0.9600 . ? C42 H42B 0.9600 . ? C43 N5 1.356(4) . ? C43 N6 1.356(3) . ? C43 C44 1.457(4) . ? C44 C45 1.389(4) . ? C44 C53 1.438(4) . ? C45 C46 1.410(4) . ? C45 H45 0.9300 . ? C46 C51 1.413(4) . ? C46 C47 1.418(4) . ? C47 C48 1.359(4) . ? C47 H47 0.9300 . ? C48 C49 1.423(4) . ? C48 H48 0.9300 . ? C49 O11 1.366(3) . ? C49 C50 1.373(4) . ? C50 C51 1.417(4) . ? C50 H50 0.9300 . ? C51 C52 1.426(4) . ? C52 C53 1.353(4) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 O11 1.437(4) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 N7 1.502(4) . ? C55 C56A 1.514(11) . ? C55 C57 1.514(5) . ? C55 C58 1.547(4) . ? C55 C56B 1.549(5) . ? C56B H56B 0.9600 . ? C56B H56C 0.9600 . ? C56B H56A 0.9600 . ? C57 H57A 0.9600 . ? C57 H57C 0.9600 . ? C57 H57B 0.9600 . ? C58 N8 1.504(4) . ? C58 C60 1.509(4) . ? C58 C59 1.539(4) . ? C59 H59A 0.9600 . ? C59 H59C 0.9600 . ? C59 H59B 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C60 H60A 0.9600 . ? C61 N7 1.356(4) . ? C61 N8 1.360(3) . ? C61 C62 1.468(4) . ? C62 C71 1.394(4) . ? C62 C63 1.406(4) . ? C63 C64 1.382(4) . ? C63 H63 0.9300 . ? C64 C65 1.399(4) . ? C64 H64 0.9300 . ? C65 C66 1.423(4) . ? C65 C70 1.431(4) . ? C66 C67 1.369(4) . ? C66 H66 0.9300 . ? C67 O12 1.375(4) . ? C67 C68 1.412(5) . ? C68 C69 1.363(4) . ? C68 H68 0.9300 . ? C69 C70 1.424(4) . ? C69 H69 0.9300 . ? C70 C71 1.415(4) . ? C71 H71 0.9300 . ? C72 O12 1.456(4) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? N1 O1 1.285(3) . ? N2 O2 1.284(3) . ? N3 O3 1.281(3) . ? N4 O4 1.282(3) . ? N5 O5 1.291(3) . ? N6 O6 1.283(3) . ? N7 O7 1.288(3) . ? N8 O8 1.287(3) . ? C6A H6AB 0.9600 . ? C6A H6AC 0.9600 . ? C6A H6AA 0.9600 . ? C2A H2AB 0.9600 . ? C2A H2AC 0.9600 . ? C2A H2AA 0.9600 . ? C56A H56E 0.9600 . ? C56A H56F 0.9600 . ? C56A H56D 0.9600 . ? 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 C2A C1 N2 110.0(5) . . ? C2A C1 C2B 0.6(6) . . ? N2 C1 C2B 110.1(3) . . ? C2A C1 C3 110.4(5) . . ? N2 C1 C3 106.3(2) . . ? C2B C1 C3 109.8(3) . . ? C2A C1 C4 115.2(5) . . ? N2 C1 C4 100.6(2) . . ? C2B C1 C4 115.7(3) . . ? C3 C1 C4 113.6(2) . . ? C1 C2B H2BB 109.5 . . ? C1 C2B H2BC 109.5 . . ? H2BB C2B H2BC 109.5 . . ? C1 C2B H2BA 109.5 . . ? H2BB C2B H2BA 109.5 . . ? H2BC C2B H2BA 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C3 H3A 109.5 . . ? H3B C3 H3A 109.5 . . ? H3C C3 H3A 109.5 . . ? N1 C4 C6A 116.3(5) . . ? N1 C4 C6B 109.3(3) . . ? C6A C4 C6B 10.6(5) . . ? N1 C4 C5 105.3(2) . . ? C6A C4 C5 102.4(5) . . ? C6B C4 C5 112.7(3) . . ? N1 C4 C1 100.99(19) . . ? C6A C4 C1 118.6(5) . . ? C6B C4 C1 114.5(3) . . ? C5 C4 C1 112.9(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? H5C C5 H5B 109.5 . . ? C4 C6B H6BB 109.5 . . ? C4 C6B H6BC 109.5 . . ? H6BB C6B H6BC 109.5 . . ? C4 C6B H6BA 109.5 . . ? H6BB C6B H6BA 109.5 . . ? H6BC C6B H6BA 109.5 . . ? N2 C7 N1 107.3(2) . . ? N2 C7 C8 126.8(2) . . ? N1 C7 C8 125.8(2) . . ? C17 C8 C9 118.8(3) . . ? C17 C8 C7 122.1(3) . . ? C9 C8 C7 118.9(3) . . ? C10 C9 C8 121.4(3) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 120.7(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C16 C11 C12 119.8(2) . . ? C16 C11 C10 118.7(2) . . ? C12 C11 C10 121.5(2) . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? O9 C13 C12 125.2(2) . . ? O9 C13 C14 114.4(2) . . ? C12 C13 C14 120.3(3) . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 121.1(3) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C11 C16 C15 118.6(2) . . ? C11 C16 C17 120.0(2) . . ? C15 C16 C17 121.4(2) . . ? C8 C17 C16 120.4(3) . . ? C8 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? O9 C18 H18B 109.5 . . ? O9 C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O9 C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? N3 C19 C20 107.4(2) . . ? N3 C19 C21 107.2(2) . . ? C20 C19 C21 109.0(2) . . ? N3 C19 C22 102.3(2) . . ? C20 C19 C22 115.4(2) . . ? C21 C19 C22 114.7(2) . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C20 H20A 109.5 . . ? H20B C20 H20A 109.5 . . ? H20C C20 H20A 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? H21C C21 H21B 109.5 . . ? N4 C22 C23 108.4(2) . . ? N4 C22 C24 106.5(2) . . ? C23 C22 C24 109.9(3) . . ? N4 C22 C19 101.8(2) . . ? C23 C22 C19 114.8(2) . . ? C24 C22 C19 114.6(2) . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? H24C C24 H24A 109.5 . . ? N3 C25 N4 109.4(2) . . ? N3 C25 C26 125.5(3) . . ? N4 C25 C26 125.1(2) . . ? C35 C26 C27 118.7(2) . . ? C35 C26 C25 121.3(2) . . ? C27 C26 C25 119.9(2) . . ? C28 C27 C26 120.4(3) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 121.8(2) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C30 C29 C28 122.3(2) . . ? C30 C29 C34 120.0(3) . . ? C28 C29 C34 117.7(2) . . ? C31 C30 C29 120.7(3) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 O10 125.4(2) . . ? C30 C31 C32 120.5(3) . . ? O10 C31 C32 114.0(3) . . ? C33 C32 C31 120.0(3) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 121.6(2) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C29 120.0(3) . . ? C35 C34 C33 122.8(2) . . ? C29 C34 C33 117.2(2) . . ? C26 C35 C34 121.4(2) . . ? C26 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? O10 C36 H36C 109.5 . . ? O10 C36 H36B 109.5 . . ? H36C C36 H36B 109.5 . . ? O10 C36 H36A 109.5 . . ? H36C C36 H36A 109.5 . . ? H36B C36 H36A 109.5 . . ? N5 C37 C38 106.9(2) . . ? N5 C37 C39 108.8(2) . . ? C38 C37 C39 109.2(3) . . ? N5 C37 C40 100.9(2) . . ? C38 C37 C40 114.9(2) . . ? C39 C37 C40 115.4(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? H38C C38 H38B 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C39 H39A 109.5 . . ? H39B C39 H39A 109.5 . . ? H39C C39 H39A 109.5 . . ? N6 C40 C41 109.6(2) . . ? N6 C40 C42 105.3(3) . . ? C41 C40 C42 109.7(2) . . ? N6 C40 C37 102.0(2) . . ? C41 C40 C37 115.0(2) . . ? C42 C40 C37 114.4(3) . . ? C40 C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C41 H41A 109.5 . . ? H41B C41 H41A 109.5 . . ? H41C C41 H41A 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? H42C C42 H42B 109.5 . . ? N5 C43 N6 107.7(2) . . ? N5 C43 C44 126.6(2) . . ? N6 C43 C44 125.7(2) . . ? C45 C44 C53 116.8(2) . . ? C45 C44 C43 121.4(2) . . ? C53 C44 C43 121.7(3) . . ? C44 C45 C46 122.0(2) . . ? C44 C45 H45 119.0 . . ? C46 C45 H45 119.0 . . ? C45 C46 C51 120.1(3) . . ? C45 C46 C47 121.9(2) . . ? C51 C46 C47 118.0(2) . . ? C48 C47 C46 121.4(2) . . ? C48 C47 H47 119.3 . . ? C46 C47 H47 119.3 . . ? C47 C48 C49 120.4(3) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? O11 C49 C50 125.6(2) . . ? O11 C49 C48 114.7(3) . . ? C50 C49 C48 119.7(2) . . ? C49 C50 C51 120.3(2) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C46 C51 C50 120.1(3) . . ? C46 C51 C52 117.8(2) . . ? C50 C51 C52 122.1(2) . . ? C53 C52 C51 121.1(2) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C52 C53 C44 122.1(3) . . ? C52 C53 H53 118.9 . . ? C44 C53 H53 118.9 . . ? O11 C54 H54A 109.5 . . ? O11 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O11 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N7 C55 C56A 115.6(4) . . ? N7 C55 C57 109.7(2) . . ? C56A C55 C57 95.0(5) . . ? N7 C55 C58 101.7(2) . . ? C56A C55 C58 120.6(4) . . ? C57 C55 C58 114.5(2) . . ? N7 C55 C56B 101.5(2) . . ? C56A C55 C56B 20.8(4) . . ? C57 C55 C56B 115.1(3) . . ? C58 C55 C56B 112.6(3) . . ? C55 C56B H56B 109.5 . . ? C55 C56B H56C 109.5 . . ? H56B C56B H56C 109.5 . . ? C55 C56B H56A 109.5 . . ? H56B C56B H56A 109.5 . . ? H56C C56B H56A 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? H57C C57 H57B 109.5 . . ? N8 C58 C60 109.9(3) . . ? N8 C58 C59 106.2(2) . . ? C60 C58 C59 109.3(2) . . ? N8 C58 C55 101.2(2) . . ? C60 C58 C55 115.9(3) . . ? C59 C58 C55 113.5(3) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? H59C C59 H59B 109.5 . . ? C58 C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C58 C60 H60A 109.5 . . ? H60B C60 H60A 109.5 . . ? H60C C60 H60A 109.5 . . ? N7 C61 N8 107.8(2) . . ? N7 C61 C62 125.5(2) . . ? N8 C61 C62 126.7(3) . . ? C71 C62 C63 118.9(3) . . ? C71 C62 C61 121.5(2) . . ? C63 C62 C61 119.6(3) . . ? C64 C63 C62 120.7(3) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C63 C64 C65 121.9(3) . . ? C63 C64 H64 119.0 . . ? C65 C64 H64 119.0 . . ? C64 C65 C66 122.6(3) . . ? C64 C65 C70 117.9(3) . . ? C66 C65 C70 119.5(3) . . ? C67 C66 C65 119.9(3) . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C66 C67 O12 124.9(3) . . ? C66 C67 C68 121.2(3) . . ? O12 C67 C68 113.9(3) . . ? C69 C68 C67 119.7(3) . . ? C69 C68 H68 120.1 . . ? C67 C68 H68 120.1 . . ? C68 C69 C70 121.7(3) . . ? C68 C69 H69 119.1 . . ? C70 C69 H69 119.1 . . ? C71 C70 C69 122.6(3) . . ? C71 C70 C65 119.6(3) . . ? C69 C70 C65 117.8(3) . . ? C62 C71 C70 120.9(3) . . ? C62 C71 H71 119.5 . . ? C70 C71 H71 119.5 . . ? O12 C72 H72A 109.5 . . ? O12 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? O12 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O1 N1 C7 125.8(2) . . ? O1 N1 C4 121.1(2) . . ? C7 N1 C4 112.2(2) . . ? O2 N2 C7 125.8(2) . . ? O2 N2 C1 120.8(2) . . ? C7 N2 C1 113.0(2) . . ? O3 N3 C25 126.7(2) . . ? O3 N3 C19 120.4(2) . . ? C25 N3 C19 112.8(2) . . ? O4 N4 C25 126.7(2) . . ? O4 N4 C22 120.2(2) . . ? C25 N4 C22 113.1(2) . . ? O5 N5 C43 126.6(2) . . ? O5 N5 C37 119.9(2) . . ? C43 N5 C37 113.3(2) . . ? O6 N6 C43 127.2(2) . . ? O6 N6 C40 119.3(2) . . ? C43 N6 C40 113.3(2) . . ? O7 N7 C61 126.3(2) . . ? O7 N7 C55 120.4(2) . . ? C61 N7 C55 112.8(2) . . ? O8 N8 C61 125.5(2) . . ? O8 N8 C58 121.3(2) . . ? C61 N8 C58 112.8(2) . . ? C13 O9 C18 117.6(2) . . ? C31 O10 C36 117.3(2) . . ? C49 O11 C54 117.5(2) . . ? C67 O12 C72 116.9(3) . . ? C4 C6A H6AB 109.5 . . ? C4 C6A H6AC 109.5 . . ? C4 C6A H6AA 109.5 . . ? C1 C2A H2AB 109.5 . . ? C1 C2A H2AC 109.5 . . ? C1 C2A H2AA 109.5 . . ? C55 C56A H56E 109.5 . . ? C55 C56A H56F 109.5 . . ? C55 C56A H56D 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 C2A C1 C4 N1 140.4(6) . . . . ? N2 C1 C4 N1 22.2(2) . . . . ? C2B C1 C4 N1 140.7(3) . . . . ? C3 C1 C4 N1 -91.0(3) . . . . ? C2A C1 C4 C6A -91.4(8) . . . . ? N2 C1 C4 C6A 150.5(5) . . . . ? C2B C1 C4 C6A -91.0(6) . . . . ? C3 C1 C4 C6A 37.3(6) . . . . ? C2A C1 C4 C6B -102.3(6) . . . . ? N2 C1 C4 C6B 139.5(3) . . . . ? C2B C1 C4 C6B -102.0(4) . . . . ? C3 C1 C4 C6B 26.3(4) . . . . ? C2A C1 C4 C5 28.4(6) . . . . ? N2 C1 C4 C5 -89.8(3) . . . . ? C2B C1 C4 C5 28.8(4) . . . . ? C3 C1 C4 C5 157.1(2) . . . . ? N2 C7 C8 C17 158.3(3) . . . . ? N1 C7 C8 C17 -26.9(4) . . . . ? N2 C7 C8 C9 -26.5(4) . . . . ? N1 C7 C8 C9 148.3(3) . . . . ? C17 C8 C9 C10 -0.4(4) . . . . ? C7 C8 C9 C10 -175.7(2) . . . . ? C8 C9 C10 C11 0.7(4) . . . . ? C9 C10 C11 C16 -0.8(4) . . . . ? C9 C10 C11 C12 178.6(2) . . . . ? C16 C11 C12 C13 0.4(4) . . . . ? C10 C11 C12 C13 -179.1(2) . . . . ? C11 C12 C13 O9 179.8(2) . . . . ? C11 C12 C13 C14 0.4(4) . . . . ? O9 C13 C14 C15 180.0(2) . . . . ? C12 C13 C14 C15 -0.6(4) . . . . ? C13 C14 C15 C16 -0.1(4) . . . . ? C12 C11 C16 C15 -1.0(3) . . . . ? C10 C11 C16 C15 178.5(2) . . . . ? C12 C11 C16 C17 -178.9(2) . . . . ? C10 C11 C16 C17 0.6(3) . . . . ? C14 C15 C16 C11 0.9(4) . . . . ? C14 C15 C16 C17 178.7(2) . . . . ? C9 C8 C17 C16 0.1(4) . . . . ? C7 C8 C17 C16 175.3(2) . . . . ? C11 C16 C17 C8 -0.3(4) . . . . ? C15 C16 C17 C8 -178.1(2) . . . . ? N3 C19 C22 N4 7.7(2) . . . . ? C20 C19 C22 N4 124.0(2) . . . . ? C21 C19 C22 N4 -108.0(3) . . . . ? N3 C19 C22 C23 124.5(2) . . . . ? C20 C19 C22 C23 -119.2(3) . . . . ? C21 C19 C22 C23 8.9(3) . . . . ? N3 C19 C22 C24 -106.8(3) . . . . ? C20 C19 C22 C24 9.5(3) . . . . ? C21 C19 C22 C24 137.5(3) . . . . ? N3 C25 C26 C35 27.2(4) . . . . ? N4 C25 C26 C35 -155.4(3) . . . . ? N3 C25 C26 C27 -149.9(3) . . . . ? N4 C25 C26 C27 27.5(4) . . . . ? C35 C26 C27 C28 0.9(4) . . . . ? C25 C26 C27 C28 178.1(2) . . . . ? C26 C27 C28 C29 -0.2(4) . . . . ? C27 C28 C29 C30 179.5(3) . . . . ? C27 C28 C29 C34 -0.7(4) . . . . ? C28 C29 C30 C31 -180.0(3) . . . . ? C34 C29 C30 C31 0.3(4) . . . . ? C29 C30 C31 O10 177.7(3) . . . . ? C29 C30 C31 C32 -1.3(4) . . . . ? C30 C31 C32 C33 0.4(4) . . . . ? O10 C31 C32 C33 -178.7(3) . . . . ? C31 C32 C33 C34 1.5(4) . . . . ? C30 C29 C34 C35 -179.3(3) . . . . ? C28 C29 C34 C35 1.0(4) . . . . ? C30 C29 C34 C33 1.5(4) . . . . ? C28 C29 C34 C33 -178.2(2) . . . . ? C32 C33 C34 C35 178.3(3) . . . . ? C32 C33 C34 C29 -2.5(4) . . . . ? C27 C26 C35 C34 -0.6(4) . . . . ? C25 C26 C35 C34 -177.8(2) . . . . ? C29 C34 C35 C26 -0.3(4) . . . . ? C33 C34 C35 C26 178.8(3) . . . . ? N5 C37 C40 N6 15.5(3) . . . . ? C38 C37 C40 N6 -99.2(3) . . . . ? C39 C37 C40 N6 132.5(2) . . . . ? N5 C37 C40 C41 134.0(2) . . . . ? C38 C37 C40 C41 19.3(3) . . . . ? C39 C37 C40 C41 -109.0(3) . . . . ? N5 C37 C40 C42 -97.7(3) . . . . ? C38 C37 C40 C42 147.7(3) . . . . ? C39 C37 C40 C42 19.4(4) . . . . ? N5 C43 C44 C45 -179.6(3) . . . . ? N6 C43 C44 C45 -1.1(4) . . . . ? N5 C43 C44 C53 -1.4(4) . . . . ? N6 C43 C44 C53 177.1(3) . . . . ? C53 C44 C45 C46 0.1(4) . . . . ? C43 C44 C45 C46 178.4(2) . . . . ? C44 C45 C46 C51 0.2(4) . . . . ? C44 C45 C46 C47 -178.4(3) . . . . ? C45 C46 C47 C48 179.5(3) . . . . ? C51 C46 C47 C48 0.8(4) . . . . ? C46 C47 C48 C49 0.3(4) . . . . ? C47 C48 C49 O11 179.5(2) . . . . ? C47 C48 C49 C50 -0.2(4) . . . . ? O11 C49 C50 C51 179.2(2) . . . . ? C48 C49 C50 C51 -1.0(4) . . . . ? C45 C46 C51 C50 179.3(2) . . . . ? C47 C46 C51 C50 -2.1(4) . . . . ? C45 C46 C51 C52 -0.4(4) . . . . ? C47 C46 C51 C52 178.3(2) . . . . ? C49 C50 C51 C46 2.2(4) . . . . ? C49 C50 C51 C52 -178.2(3) . . . . ? C46 C51 C52 C53 0.3(4) . . . . ? C50 C51 C52 C53 -179.3(3) . . . . ? C51 C52 C53 C44 0.0(4) . . . . ? C45 C44 C53 C52 -0.2(4) . . . . ? C43 C44 C53 C52 -178.5(3) . . . . ? N7 C55 C58 N8 18.2(3) . . . . ? C56A C55 C58 N8 -111.2(5) . . . . ? C57 C55 C58 N8 136.4(3) . . . . ? C56B C55 C58 N8 -89.6(3) . . . . ? N7 C55 C58 C60 137.1(3) . . . . ? C56A C55 C58 C60 7.7(6) . . . . ? C57 C55 C58 C60 -104.7(3) . . . . ? C56B C55 C58 C60 29.3(4) . . . . ? N7 C55 C58 C59 -95.2(3) . . . . ? C56A C55 C58 C59 135.4(5) . . . . ? C57 C55 C58 C59 23.0(4) . . . . ? C56B C55 C58 C59 157.0(3) . . . . ? N7 C61 C62 C71 154.3(3) . . . . ? N8 C61 C62 C71 -26.2(4) . . . . ? N7 C61 C62 C63 -26.0(4) . . . . ? N8 C61 C62 C63 153.5(3) . . . . ? C71 C62 C63 C64 -2.2(4) . . . . ? C61 C62 C63 C64 178.2(3) . . . . ? C62 C63 C64 C65 0.1(4) . . . . ? C63 C64 C65 C66 -177.7(3) . . . . ? C63 C64 C65 C70 2.1(4) . . . . ? C64 C65 C66 C67 179.7(3) . . . . ? C70 C65 C66 C67 -0.1(4) . . . . ? C65 C66 C67 O12 -177.3(3) . . . . ? C65 C66 C67 C68 3.1(4) . . . . ? C66 C67 C68 C69 -3.3(5) . . . . ? O12 C67 C68 C69 177.1(3) . . . . ? C67 C68 C69 C70 0.4(5) . . . . ? C68 C69 C70 C71 -177.7(3) . . . . ? C68 C69 C70 C65 2.5(5) . . . . ? C64 C65 C70 C71 -2.3(4) . . . . ? C66 C65 C70 C71 177.5(3) . . . . ? C64 C65 C70 C69 177.6(3) . . . . ? C66 C65 C70 C69 -2.6(4) . . . . ? C63 C62 C71 C70 1.9(4) . . . . ? C61 C62 C71 C70 -178.4(2) . . . . ? C69 C70 C71 C62 -179.6(3) . . . . ? C65 C70 C71 C62 0.3(4) . . . . ? N2 C7 N1 O1 -177.5(2) . . . . ? C8 C7 N1 O1 6.9(4) . . . . ? N2 C7 N1 C4 13.3(3) . . . . ? C8 C7 N1 C4 -162.4(2) . . . . ? C6A C4 N1 O1 37.2(6) . . . . ? C6B C4 N1 O1 46.0(3) . . . . ? C5 C4 N1 O1 -75.3(3) . . . . ? C1 C4 N1 O1 167.0(2) . . . . ? C6A C4 N1 C7 -153.0(5) . . . . ? C6B C4 N1 C7 -144.2(3) . . . . ? C5 C4 N1 C7 94.5(3) . . . . ? C1 C4 N1 C7 -23.2(3) . . . . ? N1 C7 N2 O2 175.6(2) . . . . ? C8 C7 N2 O2 -8.8(4) . . . . ? N1 C7 N2 C1 3.4(3) . . . . ? C8 C7 N2 C1 179.0(2) . . . . ? C2A C1 N2 O2 48.3(6) . . . . ? C2B C1 N2 O2 47.7(4) . . . . ? C3 C1 N2 O2 -71.2(3) . . . . ? C4 C1 N2 O2 170.2(2) . . . . ? C2A C1 N2 C7 -139.1(5) . . . . ? C2B C1 N2 C7 -139.7(3) . . . . ? C3 C1 N2 C7 101.5(3) . . . . ? C4 C1 N2 C7 -17.1(3) . . . . ? N4 C25 N3 O3 -177.5(2) . . . . ? C26 C25 N3 O3 0.2(4) . . . . ? N4 C25 N3 C19 2.0(3) . . . . ? C26 C25 N3 C19 179.7(2) . . . . ? C20 C19 N3 O3 51.2(3) . . . . ? C21 C19 N3 O3 -65.9(3) . . . . ? C22 C19 N3 O3 173.1(2) . . . . ? C20 C19 N3 C25 -128.4(2) . . . . ? C21 C19 N3 C25 114.6(3) . . . . ? C22 C19 N3 C25 -6.4(3) . . . . ? N3 C25 N4 O4 -178.1(2) . . . . ? C26 C25 N4 O4 4.2(4) . . . . ? N3 C25 N4 C22 3.8(3) . . . . ? C26 C25 N4 C22 -173.9(2) . . . . ? C23 C22 N4 O4 52.9(3) . . . . ? C24 C22 N4 O4 -65.3(3) . . . . ? C19 C22 N4 O4 174.3(2) . . . . ? C23 C22 N4 C25 -128.9(2) . . . . ? C24 C22 N4 C25 112.9(3) . . . . ? C19 C22 N4 C25 -7.5(3) . . . . ? N6 C43 N5 O5 179.6(3) . . . . ? C44 C43 N5 O5 -1.7(5) . . . . ? N6 C43 N5 C37 4.6(3) . . . . ? C44 C43 N5 C37 -176.7(2) . . . . ? C38 C37 N5 O5 -68.3(3) . . . . ? C39 C37 N5 O5 49.5(3) . . . . ? C40 C37 N5 O5 171.3(2) . . . . ? C38 C37 N5 C43 107.2(3) . . . . ? C39 C37 N5 C43 -135.1(3) . . . . ? C40 C37 N5 C43 -13.3(3) . . . . ? N5 C43 N6 O6 -178.8(3) . . . . ? C44 C43 N6 O6 2.5(4) . . . . ? N5 C43 N6 C40 7.1(3) . . . . ? C44 C43 N6 C40 -171.6(2) . . . . ? C41 C40 N6 O6 48.2(3) . . . . ? C42 C40 N6 O6 -69.7(3) . . . . ? C37 C40 N6 O6 170.5(2) . . . . ? C41 C40 N6 C43 -137.2(2) . . . . ? C42 C40 N6 C43 104.8(3) . . . . ? C37 C40 N6 C43 -15.0(3) . . . . ? N8 C61 N7 O7 177.5(2) . . . . ? C62 C61 N7 O7 -2.9(4) . . . . ? N8 C61 N7 C55 6.0(3) . . . . ? C62 C61 N7 C55 -174.5(2) . . . . ? C56A C55 N7 O7 -55.8(6) . . . . ? C57 C55 N7 O7 50.2(3) . . . . ? C58 C55 N7 O7 171.8(2) . . . . ? C56B C55 N7 O7 -71.9(3) . . . . ? C56A C55 N7 C61 116.4(5) . . . . ? C57 C55 N7 C61 -137.7(3) . . . . ? C58 C55 N7 C61 -16.1(3) . . . . ? C56B C55 N7 C61 100.2(3) . . . . ? N7 C61 N8 O8 179.9(3) . . . . ? C62 C61 N8 O8 0.4(4) . . . . ? N7 C61 N8 C58 7.7(3) . . . . ? C62 C61 N8 C58 -171.9(3) . . . . ? C60 C58 N8 O8 47.3(4) . . . . ? C59 C58 N8 O8 -70.9(3) . . . . ? C55 C58 N8 O8 170.3(2) . . . . ? C60 C58 N8 C61 -140.1(3) . . . . ? C59 C58 N8 C61 101.7(3) . . . . ? C55 C58 N8 C61 -17.1(3) . . . . ? C12 C13 O9 C18 -0.6(4) . . . . ? C14 C13 O9 C18 178.8(2) . . . . ? C30 C31 O10 C36 -4.1(4) . . . . ? C32 C31 O10 C36 174.9(3) . . . . ? C50 C49 O11 C54 -1.3(4) . . . . ? C48 C49 O11 C54 179.0(2) . . . . ? C66 C67 O12 C72 3.7(4) . . . . ? C68 C67 O12 C72 -176.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.292 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.062