# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Hong-Feng Li' _publ_contact_author_email lhf4612@163.com _publ_section_title ; Highly Luminescent Bis-Diketone Lanthanide Complexes with Triple-Stranded Dinuclear Structure ; loop_ _publ_author_name 'Hong-Feng Li' 'Guangming Li' # Attachment '- Complex1.CIF' data_shelxl_c _database_code_depnum_ccdc_archive 'CCDC 833523' #TrackingRef '- Complex1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H46 Eu2 F18 O16' _chemical_formula_weight 1716.93 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' Eu Eu -0.1578 3.6682 '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' 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 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 20.417(4) _cell_length_b 21.521(4) _cell_length_c 17.649(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.76(3) _cell_angle_gamma 90.00 _cell_volume 6732(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour buff _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3384 _exptl_absorpt_coefficient_mu 1.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.760 _exptl_absorpt_process_details SADABS _exptl_special_details ; "dfix h8a o8 h8b o8 0.85" and "sadi h8a eu1 h8b eu1" commands have been added to defix the position of the H atoms. ; _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 SMART1000 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32099 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7681 _reflns_number_gt 6225 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT-plus _computing_data_reduction SAINT-plus _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_molecular_graphics SHELXL97 _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^)+(0.0895P)^2^+11.5786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7681 _refine_ls_number_parameters 458 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.163 _refine_ls_shift/su_mean 0.015 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 0.3975(4) 0.0597(3) 0.2901(4) 0.0739(16) Uani 1 1 d . . . C2 C 0.3315(3) 0.1036(3) 0.2684(3) 0.0576(12) Uani 1 1 d . . . C3 C 0.2782(3) 0.0845(3) 0.2898(3) 0.0590(12) Uani 1 1 d . . . H3A H 0.2819 0.0453 0.3137 0.071 Uiso 1 1 calc R . . C4 C 0.2175(3) 0.1245(2) 0.2756(3) 0.0532(11) Uani 1 1 d . . . C5 C 0.1666(3) 0.1081(2) 0.3110(3) 0.0518(10) Uani 1 1 d . . . C6 C 0.1407(3) 0.0489(2) 0.3111(4) 0.0617(12) Uani 1 1 d . . . H6 H 0.1552 0.0158 0.2888 0.074 Uiso 1 1 calc R . . C7 C 0.0928(3) 0.0390(3) 0.3446(4) 0.0670(14) Uani 1 1 d . . . H7 H 0.0736 -0.0006 0.3424 0.080 Uiso 1 1 calc R . . C8 C 0.0735(3) 0.0865(3) 0.3807(4) 0.0607(12) Uani 1 1 d . . . H8 H 0.0410 0.0789 0.4024 0.073 Uiso 1 1 calc R . . C9 C 0.1014(2) 0.1460(2) 0.3856(3) 0.0469(9) Uani 1 1 d . . . C10 C 0.1452(2) 0.1567(2) 0.3468(3) 0.0487(10) Uani 1 1 d . . . H10 H 0.1606 0.1970 0.3446 0.058 Uiso 1 1 calc R . . C11 C 0.0893(2) 0.1972(2) 0.4337(3) 0.0452(9) Uani 1 1 d . . . C12 C 0.0188(2) 0.2121(2) 0.4219(3) 0.0450(9) Uani 1 1 d . . . H12 H -0.0230 0.1891 0.3829 0.054 Uiso 1 1 calc R . . C13 C 0.0095(2) 0.26136(19) 0.4680(3) 0.0416(9) Uani 1 1 d . . . C14 C 0.0730(2) 0.2936(2) 0.5286(3) 0.0520(10) Uani 1 1 d . . . H14 H 0.0677 0.3261 0.5600 0.062 Uiso 1 1 calc R . . C15 C 0.1427(3) 0.2783(3) 0.5424(4) 0.0621(13) Uani 1 1 d . . . H15 H 0.1850 0.2994 0.5842 0.075 Uiso 1 1 calc R . . C16 C 0.1505(3) 0.2312(2) 0.4941(4) 0.0549(12) Uani 1 1 d . . . H16 H 0.1982 0.2222 0.5025 0.066 Uiso 1 1 calc R . . C17 C -0.0670(2) 0.2766(2) 0.4513(3) 0.0424(9) Uani 1 1 d . . . C18 C -0.0834(2) 0.3388(2) 0.4649(3) 0.0491(10) Uani 1 1 d . . . H18A H -0.0462 0.3689 0.4803 0.059 Uiso 1 1 calc R . . C19 C -0.1509(2) 0.3562(2) 0.4563(3) 0.0467(9) Uani 1 1 d . . . C20 C -0.1591(3) 0.4239(3) 0.4758(4) 0.0641(13) Uani 1 1 d . . . C21 C 0.4261(3) 0.3820(3) 0.3449(4) 0.0755(16) Uani 1 1 d . . . C22 C 0.3506(3) 0.3481(3) 0.3070(3) 0.0567(12) Uani 1 1 d . . . C23 C 0.2970(3) 0.3730(3) 0.3241(3) 0.0598(12) Uani 1 1 d . . . H23A H 0.3087 0.4081 0.3592 0.072 Uiso 1 1 calc R . . C24 C 0.2242(3) 0.3458(2) 0.2889(3) 0.0504(10) Uani 1 1 d . . . C25 C 0.1707(3) 0.3687(2) 0.3171(3) 0.0491(10) Uani 1 1 d . . . C26 C 0.0939(3) 0.3640(2) 0.2596(3) 0.0490(10) Uani 1 1 d . . . H26 H 0.0772 0.3467 0.2047 0.059 Uiso 1 1 calc R . . C27 C 0.0410(3) 0.3848(2) 0.2826(3) 0.0484(9) Uani 1 1 d . . . C28 C 0.0674(3) 0.4079(2) 0.3661(3) 0.0572(12) Uani 1 1 d . . . H28 H 0.0331 0.4207 0.3830 0.069 Uiso 1 1 calc R . . C29 C 0.1437(3) 0.4121(2) 0.4246(3) 0.0612(12) Uani 1 1 d . . . H29 H 0.1602 0.4274 0.4805 0.073 Uiso 1 1 calc R . . C30 C 0.1957(3) 0.3937(2) 0.4006(3) 0.0547(11) Uani 1 1 d . . . H30 H 0.2470 0.3979 0.4397 0.066 Uiso 1 1 calc R . . C31 C 0.1545(4) 0.1189(4) -0.0054(5) 0.101(3) Uani 1 1 d . . . H31A H 0.1062 0.1385 -0.0233 0.121 Uiso 1 1 calc R . . H31B H 0.1545 0.1053 -0.0578 0.121 Uiso 1 1 calc R . . C32 C 0.1618(7) 0.0653(6) 0.0470(7) 0.165(6) Uani 1 1 d . . . H32A H 0.1980 0.0372 0.0464 0.248 Uiso 1 1 calc R . . H32B H 0.1138 0.0449 0.0237 0.248 Uiso 1 1 calc R . . H32C H 0.1785 0.0782 0.1059 0.248 Uiso 1 1 calc R . . Eu1 Eu 0.249611(11) 0.237286(11) 0.164490(14) 0.04405(10) Uani 1 1 d D . . F1 F 0.4815(2) 0.3443(3) 0.3904(4) 0.173(3) Uani 1 1 d . . . F2 F 0.4392(3) 0.4028(3) 0.2873(4) 0.133(2) Uani 1 1 d . . . F3 F 0.4361(4) 0.4270(4) 0.3959(6) 0.220(5) Uani 1 1 d . . . F4 F -0.2202(3) 0.4485(2) 0.4111(4) 0.132(2) Uani 1 1 d . . . F5 F -0.1034(2) 0.45995(16) 0.4905(3) 0.0953(13) Uani 1 1 d . . . F6 F -0.1682(3) 0.4275(2) 0.5443(4) 0.129(2) Uani 1 1 d . . . F7 F 0.4595(3) 0.0831(4) 0.3406(7) 0.236(5) Uani 1 1 d . . . F8 F 0.4019(4) 0.0416(4) 0.2265(4) 0.188(3) Uani 1 1 d . . . F9 F 0.3959(5) 0.0077(4) 0.3256(8) 0.245(6) Uani 1 1 d . . . O1 O 0.3363(2) 0.15353(18) 0.2351(2) 0.0641(9) Uani 1 1 d . . . O2 O 0.20672(19) 0.17470(17) 0.2388(2) 0.0583(8) Uani 1 1 d . . . O3 O -0.11589(18) 0.23437(13) 0.4237(2) 0.0469(7) Uani 1 1 d . . . O4 O -0.21011(18) 0.32349(16) 0.4347(2) 0.0557(8) Uani 1 1 d . . . O5 O 0.34703(18) 0.30067(19) 0.2636(2) 0.0614(9) Uani 1 1 d . . . O6 O 0.20146(18) 0.30346(17) 0.2330(2) 0.0584(8) Uani 1 1 d . . . O7 O 0.2146(2) 0.1656(2) 0.0391(3) 0.0781(12) Uani 1 1 d . . . H71 H 0.2556 0.1531 0.0428 0.117 Uiso 1 1 d R . . O8 O 0.3430(3) 0.2424(2) 0.1125(3) 0.0747(12) Uani 1 1 d D . . H8A H 0.386(2) 0.223(3) 0.145(4) 0.112 Uiso 1 1 d D . . H8B H 0.329(3) 0.265(3) 0.065(3) 0.112 Uiso 1 1 d 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 0.069(4) 0.082(4) 0.073(4) 0.008(3) 0.037(3) 0.025(3) C2 0.056(3) 0.066(3) 0.050(2) -0.002(2) 0.026(2) 0.015(2) C3 0.063(3) 0.057(3) 0.062(3) 0.005(2) 0.035(2) 0.017(2) C4 0.060(3) 0.058(3) 0.045(2) 0.003(2) 0.028(2) 0.014(2) C5 0.060(3) 0.052(3) 0.050(2) 0.006(2) 0.032(2) 0.012(2) C6 0.076(3) 0.048(3) 0.070(3) -0.001(2) 0.043(3) 0.009(2) C7 0.083(4) 0.048(3) 0.078(4) -0.005(3) 0.046(3) -0.004(3) C8 0.061(3) 0.063(3) 0.072(3) 0.004(3) 0.044(3) 0.001(2) C9 0.044(2) 0.050(2) 0.049(2) 0.0019(18) 0.0245(18) 0.0047(18) C10 0.051(2) 0.047(2) 0.052(2) 0.0047(19) 0.0283(19) 0.0062(19) C11 0.044(2) 0.050(2) 0.045(2) 0.0016(17) 0.0245(17) 0.0032(17) C12 0.043(2) 0.048(2) 0.045(2) 0.0001(19) 0.0228(17) -0.0004(18) C13 0.040(2) 0.044(2) 0.041(2) -0.0016(16) 0.0201(17) -0.0013(16) C14 0.042(2) 0.055(3) 0.055(2) -0.015(2) 0.0211(18) -0.0037(19) C15 0.041(2) 0.067(3) 0.068(3) -0.021(3) 0.019(2) -0.008(2) C16 0.043(2) 0.062(3) 0.064(3) -0.005(2) 0.029(2) 0.0002(19) C17 0.038(2) 0.049(2) 0.041(2) -0.0009(17) 0.0201(16) -0.0005(17) C18 0.040(2) 0.048(2) 0.061(3) -0.008(2) 0.0272(19) -0.0034(18) C19 0.048(2) 0.043(2) 0.054(2) -0.0022(18) 0.0288(19) 0.0010(18) C20 0.065(3) 0.051(3) 0.090(4) 0.000(3) 0.049(3) 0.004(2) C21 0.058(3) 0.081(4) 0.085(4) -0.007(3) 0.033(3) -0.018(3) C22 0.047(2) 0.068(3) 0.054(3) 0.001(2) 0.024(2) -0.011(2) C23 0.056(3) 0.061(3) 0.064(3) -0.013(2) 0.030(2) -0.014(2) C24 0.056(2) 0.048(2) 0.048(2) -0.0014(19) 0.026(2) 0.0009(19) C25 0.057(3) 0.042(2) 0.054(2) -0.0019(19) 0.032(2) -0.0022(19) C26 0.056(2) 0.044(2) 0.052(2) -0.0047(19) 0.032(2) -0.0035(19) C27 0.057(2) 0.036(2) 0.058(2) 0.0006(18) 0.034(2) 0.0012(18) C28 0.066(3) 0.054(3) 0.063(3) -0.001(2) 0.041(2) 0.006(2) C29 0.072(3) 0.057(3) 0.055(3) -0.010(2) 0.032(2) 0.005(2) C30 0.059(3) 0.044(2) 0.057(3) -0.005(2) 0.027(2) 0.003(2) C31 0.060(4) 0.127(7) 0.097(5) -0.045(5) 0.025(3) -0.015(4) C32 0.210(12) 0.180(12) 0.097(6) 0.001(7) 0.070(7) -0.102(10) Eu1 0.03727(15) 0.05285(17) 0.04396(15) -0.00026(8) 0.02163(11) 0.00415(8) F1 0.056(2) 0.175(6) 0.197(6) 0.066(5) -0.006(3) -0.037(3) F2 0.121(4) 0.139(4) 0.151(5) 0.017(4) 0.077(4) -0.053(3) F3 0.152(5) 0.263(9) 0.300(9) -0.201(8) 0.154(6) -0.150(6) F4 0.100(3) 0.072(3) 0.170(5) 0.014(3) 0.026(3) 0.033(2) F5 0.091(2) 0.0487(18) 0.168(4) -0.019(2) 0.081(3) -0.0099(17) F6 0.216(6) 0.071(3) 0.185(5) -0.034(3) 0.164(5) -0.015(3) F7 0.083(3) 0.171(7) 0.308(10) -0.090(7) -0.013(5) 0.067(4) F8 0.199(6) 0.232(8) 0.146(5) -0.003(5) 0.096(5) 0.134(6) F9 0.249(8) 0.204(7) 0.423(13) 0.204(9) 0.273(10) 0.174(7) O1 0.062(2) 0.067(2) 0.074(2) 0.0116(19) 0.0417(18) 0.0199(17) O2 0.0600(19) 0.064(2) 0.065(2) 0.0146(17) 0.0416(17) 0.0175(16) O3 0.0377(16) 0.0464(18) 0.0565(18) -0.0034(13) 0.0234(14) -0.0016(11) O4 0.0487(17) 0.0561(19) 0.072(2) -0.0070(16) 0.0373(16) -0.0008(14) O5 0.0421(16) 0.079(3) 0.062(2) -0.0118(18) 0.0249(14) -0.0054(16) O6 0.0482(17) 0.064(2) 0.065(2) -0.0192(17) 0.0295(15) -0.0017(15) O7 0.0500(19) 0.096(3) 0.088(3) -0.035(2) 0.0336(19) -0.0070(19) O8 0.063(3) 0.111(4) 0.063(3) 0.004(2) 0.040(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 F8 1.233(8) . ? C1 F7 1.237(9) . ? C1 F9 1.291(9) . ? C1 C2 1.530(7) . ? C2 O1 1.253(7) . ? C2 C3 1.378(7) . ? C3 C4 1.424(6) . ? C3 H3A 0.9300 . ? C4 O2 1.223(6) . ? C4 C5 1.497(7) . ? C5 C6 1.381(7) . ? C5 C10 1.399(6) . ? C6 C7 1.387(8) . ? C6 H6 0.9300 . ? C7 C8 1.363(8) . ? C7 H7 0.9300 . ? C8 C9 1.386(7) . ? C8 H8 0.9300 . ? C9 C10 1.388(6) . ? C9 C11 1.485(6) . ? C10 H10 0.9300 . ? C11 C16 1.383(7) . ? C11 C12 1.385(6) . ? C12 C13 1.405(6) . ? C12 H12 0.9300 . ? C13 C14 1.389(6) . ? C13 C17 1.477(6) . ? C14 C15 1.360(7) . ? C14 H14 0.9300 . ? C15 C16 1.384(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O3 1.255(5) . ? C17 C18 1.428(6) . ? C18 C19 1.362(6) . ? C18 H18A 0.9300 . ? C19 O4 1.282(5) . ? C19 C20 1.525(7) . ? C20 F5 1.294(6) . ? C20 F4 1.314(7) . ? C20 F6 1.314(7) . ? C21 F2 1.255(8) . ? C21 F3 1.267(9) . ? C21 F1 1.297(8) . ? C21 C22 1.526(7) . ? C22 O5 1.257(6) . ? C22 C23 1.379(7) . ? C23 C24 1.421(7) . ? C23 H23A 0.9300 . ? C24 O6 1.250(6) . ? C24 C25 1.492(6) . ? C25 C26 1.385(7) . ? C25 C30 1.406(7) . ? C26 C27 1.402(6) . ? C26 H26 0.9300 . ? C27 C28 1.386(7) . ? C27 C27 1.489(9) 2 ? C28 C29 1.379(8) . ? C28 H28 0.9300 . ? C29 C30 1.381(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.440(13) . ? C31 O7 1.474(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? Eu1 O5 2.329(4) . ? Eu1 O2 2.333(3) . ? Eu1 O6 2.375(3) . ? Eu1 O3 2.379(3) 2 ? Eu1 O1 2.397(3) . ? Eu1 O4 2.399(3) 2 ? Eu1 O8 2.495(4) . ? Eu1 O7 2.494(4) . ? O3 Eu1 2.379(3) 2 ? O4 Eu1 2.399(3) 2 ? O7 H71 0.8499 . ? O8 H8A 0.878(19) . ? O8 H8B 0.875(19) . ? 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 F8 C1 F7 105.9(8) . . ? F8 C1 F9 101.4(8) . . ? F7 C1 F9 105.4(8) . . ? F8 C1 C2 114.9(5) . . ? F7 C1 C2 112.9(6) . . ? F9 C1 C2 115.1(6) . . ? O1 C2 C3 129.8(5) . . ? O1 C2 C1 112.4(5) . . ? C3 C2 C1 117.7(5) . . ? C2 C3 C4 120.5(5) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? O2 C4 C3 122.6(5) . . ? O2 C4 C5 116.7(4) . . ? C3 C4 C5 120.6(4) . . ? C6 C5 C10 118.9(4) . . ? C6 C5 C4 124.3(4) . . ? C10 C5 C4 116.8(4) . . ? C5 C6 C7 119.6(5) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C7 C6 120.9(5) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 121.1(5) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 117.9(4) . . ? C10 C9 C11 119.3(4) . . ? C8 C9 C11 122.8(4) . . ? C9 C10 C5 121.4(4) . . ? C9 C10 H10 119.3 . . ? C5 C10 H10 119.3 . . ? C16 C11 C12 117.9(4) . . ? C16 C11 C9 119.3(4) . . ? C12 C11 C9 122.8(4) . . ? C11 C12 C13 121.1(4) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 118.7(4) . . ? C14 C13 C17 122.2(4) . . ? C12 C13 C17 119.1(4) . . ? C15 C14 C13 120.6(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.9(5) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 121.7(5) . . ? C11 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? O3 C17 C18 122.5(4) . . ? O3 C17 C13 118.4(4) . . ? C18 C17 C13 119.1(4) . . ? C19 C18 C17 123.1(4) . . ? C19 C18 H18A 118.4 . . ? C17 C18 H18A 118.4 . . ? O4 C19 C18 129.4(4) . . ? O4 C19 C20 113.5(4) . . ? C18 C19 C20 117.1(4) . . ? F5 C20 F4 107.1(5) . . ? F5 C20 F6 107.0(5) . . ? F4 C20 F6 105.7(5) . . ? F5 C20 C19 115.7(4) . . ? F4 C20 C19 110.7(5) . . ? F6 C20 C19 110.2(5) . . ? F2 C21 F3 106.2(7) . . ? F2 C21 F1 104.7(6) . . ? F3 C21 F1 104.8(7) . . ? F2 C21 C22 113.0(5) . . ? F3 C21 C22 116.6(6) . . ? F1 C21 C22 110.7(6) . . ? O5 C22 C23 129.5(5) . . ? O5 C22 C21 113.3(5) . . ? C23 C22 C21 117.2(5) . . ? C22 C23 C24 121.1(5) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? O6 C24 C23 122.9(4) . . ? O6 C24 C25 117.2(4) . . ? C23 C24 C25 119.9(4) . . ? C26 C25 C30 119.1(4) . . ? C26 C25 C24 118.7(4) . . ? C30 C25 C24 122.2(4) . . ? C25 C26 C27 121.2(4) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 118.2(4) . . ? C28 C27 C27 121.0(5) . 2 ? C26 C27 C27 120.7(5) . 2 ? C29 C28 C27 121.2(5) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 120.4(5) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C25 119.8(5) . . ? C29 C30 H30 120.1 . . ? C25 C30 H30 120.1 . . ? C32 C31 O7 114.2(7) . . ? C32 C31 H31A 108.8 . . ? O7 C31 H31A 108.7 . . ? C32 C31 H31B 108.7 . . ? O7 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O5 Eu1 O2 109.57(13) . . ? O5 Eu1 O6 71.42(12) . . ? O2 Eu1 O6 72.17(14) . . ? O5 Eu1 O3 141.42(12) . 2 ? O2 Eu1 O3 73.96(12) . 2 ? O6 Eu1 O3 73.64(11) . 2 ? O5 Eu1 O1 85.12(14) . . ? O2 Eu1 O1 70.11(12) . . ? O6 Eu1 O1 124.86(13) . . ? O3 Eu1 O1 129.18(12) 2 . ? O5 Eu1 O4 86.99(13) . 2 ? O2 Eu1 O4 140.60(11) . 2 ? O6 Eu1 O4 80.43(12) . 2 ? O3 Eu1 O4 71.46(11) 2 2 ? O1 Eu1 O4 148.77(11) . 2 ? O5 Eu1 O8 74.13(15) . . ? O2 Eu1 O8 143.22(14) . . ? O6 Eu1 O8 138.24(15) . . ? O3 Eu1 O8 126.78(14) 2 . ? O1 Eu1 O8 73.90(14) . . ? O4 Eu1 O8 74.88(13) 2 . ? O5 Eu1 O7 142.24(12) . . ? O2 Eu1 O7 96.89(15) . . ? O6 Eu1 O7 144.53(12) . . ? O3 Eu1 O7 70.90(12) 2 . ? O1 Eu1 O7 78.98(14) . . ? O4 Eu1 O7 89.21(15) 2 . ? O8 Eu1 O7 68.63(15) . . ? C2 O1 Eu1 132.8(3) . . ? C4 O2 Eu1 142.1(3) . . ? C17 O3 Eu1 131.9(3) . 2 ? C19 O4 Eu1 124.5(3) . 2 ? C22 O5 Eu1 134.7(3) . . ? C24 O6 Eu1 138.8(3) . . ? C31 O7 Eu1 133.6(4) . . ? C31 O7 H71 110.6 . . ? Eu1 O7 H71 106.9 . . ? Eu1 O8 H8A 116(3) . . ? Eu1 O8 H8B 115(3) . . ? H8A O8 H8B 130(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H71 F6 0.85 2.32 3.086(6) 150.1 8 O7 H71 O4 0.85 2.39 2.936(5) 122.6 8 O8 H8B O7 0.875(19) 2.19(2) 3.056(7) 168(6) 7 O8 H8B O4 0.875(19) 2.78(8) 3.108(6) 104(6) 8 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.971 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.132 # Attachment '- 3.cif' data_shelxl_a _database_code_depnum_ccdc_archive 'CCDC 833524' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H50 F18 Nd2 O16' _chemical_formula_weight 1753.56 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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 11.1163(3) _cell_length_b 17.6881(5) _cell_length_c 18.9126(6) _cell_angle_alpha 93.2520(8) _cell_angle_beta 101.1120(8) _cell_angle_gamma 102.6610(7) _cell_volume 3541.19(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light purple' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 1.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.732 _exptl_absorpt_process_details SADABS _exptl_special_details ; "isor 0.01 f1 f2 f3 f1' f2' f3' isor 0.01 c1" have been used to define the elongate elipsoid parameters of the F and C atoms. "eadp f1 f1' eadp f2 f2'eadp f3 f3'" have been used to make the elipsoid parameter of the corresponding atoms to be equal. "dfix c1 f1 c1 f1' c1 f2 c1 f2' c1 f3 c1 f3' 1.35 sadi f1 f2 f2 f3 f3 f1 f1' f2' f2' f3' f3' f1'" have been used to define corresponding distances in the reasonable ranges. ; _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 SMART1000 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56721 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.46 _reflns_number_total 16073 _reflns_number_gt 10732 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT-plus _computing_data_reduction SAINT-plus _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_molecular_graphics SHELXL97 _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^)+(0.0675P)^2^+3.1745P] 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 16073 _refine_ls_number_parameters 954 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1510 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.025 _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 O1 O 0.4009(5) 0.1223(3) 0.1269(3) 0.0794(13) Uani 1 1 d . . . O2 O 0.5515(4) 0.2506(2) 0.21634(19) 0.0580(10) Uani 1 1 d . . . O3 O 0.6341(4) 0.7236(2) 0.3956(2) 0.0602(10) Uani 1 1 d . . . O4 O 0.6854(4) 0.8634(2) 0.4788(2) 0.0587(10) Uani 1 1 d . . . O5 O 0.7608(4) 0.1988(2) 0.1719(2) 0.0543(9) Uani 1 1 d . . . O6 O 0.7100(3) 0.3362(2) 0.12196(19) 0.0505(8) Uani 1 1 d . . . O7 O 0.5141(3) 0.7760(2) 0.26100(19) 0.0515(9) Uani 1 1 d . . . O8 O 0.3227(4) 0.8361(2) 0.2984(2) 0.0610(10) Uani 1 1 d . . . O9 O 0.4287(4) 0.1861(2) -0.0205(2) 0.0605(10) Uani 1 1 d . . . O10 O 0.4285(4) 0.2998(2) 0.0878(2) 0.0588(10) Uani 1 1 d . . . O11 O 0.3713(4) 0.6892(2) 0.3542(2) 0.0625(10) Uani 1 1 d . . . O12 O 0.3852(4) 0.7967(2) 0.4696(2) 0.0600(10) Uani 1 1 d . . . O13 O 0.7265(4) 0.2092(3) 0.0086(2) 0.0712(12) Uani 1 1 d . . . O14 O 0.6039(5) 0.0780(2) 0.0602(2) 0.0738(12) Uani 1 1 d . . . O15 O 0.6592(5) 0.9295(3) 0.3380(3) 0.0849(14) Uani 1 1 d . . . O16 O 0.4783(5) 0.9557(3) 0.4085(3) 0.0782(13) Uani 1 1 d . . . Nd1 Nd 0.50662(3) 0.818618(15) 0.379808(15) 0.04721(10) Uani 1 1 d . . . Nd2 Nd 0.56790(3) 0.212065(16) 0.095478(15) 0.04782(10) Uani 1 1 d . . . C1 C 0.2075(12) 0.0658(7) 0.1549(6) 0.153(4) Uani 1 1 d DU . . C2 C 0.3334(7) 0.1292(4) 0.1710(4) 0.085(2) Uani 1 1 d . . . C3 C 0.3530(7) 0.1838(4) 0.2303(4) 0.085(2) Uani 1 1 d . . . H3 H 0.2908 0.1815 0.2572 0.102 Uiso 1 1 calc R . . C4 C 0.4650(6) 0.2427(3) 0.2506(3) 0.0543(13) Uani 1 1 d . . . C5 C 0.4817(5) 0.2999(3) 0.3150(3) 0.0514(13) Uani 1 1 d . . . C6 C 0.4116(6) 0.2844(4) 0.3681(3) 0.0637(15) Uani 1 1 d . . . H6 H 0.3519 0.2376 0.3640 0.076 Uiso 1 1 calc R . . C7 C 0.4309(6) 0.3388(4) 0.4267(3) 0.0653(16) Uani 1 1 d . . . H7 H 0.3852 0.3281 0.4627 0.078 Uiso 1 1 calc R . . C8 C 0.5177(6) 0.4091(4) 0.4324(3) 0.0613(15) Uani 1 1 d . . . H8 H 0.5274 0.4461 0.4712 0.074 Uiso 1 1 calc R . . C9 C 0.5907(5) 0.4251(3) 0.3807(3) 0.0506(12) Uani 1 1 d . . . C10 C 0.5717(5) 0.3693(3) 0.3224(3) 0.0516(13) Uani 1 1 d . . . H10 H 0.6205 0.3787 0.2876 0.062 Uiso 1 1 calc R . . C11 C 0.6930(5) 0.4979(3) 0.3925(3) 0.0506(12) Uani 1 1 d . . . C12 C 0.8162(6) 0.4925(3) 0.3982(4) 0.0647(16) Uani 1 1 d . . . H12 H 0.8335 0.4439 0.3902 0.078 Uiso 1 1 calc R . . C13 C 0.9145(6) 0.5580(4) 0.4157(4) 0.077(2) Uani 1 1 d . . . H13 H 0.9971 0.5533 0.4190 0.093 Uiso 1 1 calc R . . C14 C 0.8908(6) 0.6304(3) 0.4283(4) 0.0656(16) Uani 1 1 d . . . H14 H 0.9574 0.6740 0.4421 0.079 Uiso 1 1 calc R . . C15 C 0.7681(5) 0.6380(3) 0.4205(3) 0.0504(12) Uani 1 1 d . . . C16 C 0.6706(5) 0.5717(3) 0.4025(3) 0.0531(13) Uani 1 1 d . . . H16 H 0.5878 0.5767 0.3969 0.064 Uiso 1 1 calc R . . C17 C 0.7378(5) 0.7157(3) 0.4315(3) 0.0518(13) Uani 1 1 d . . . C18 C 0.8197(5) 0.7749(3) 0.4830(3) 0.0557(14) Uani 1 1 d . . . H18 H 0.8986 0.7680 0.5045 0.067 Uiso 1 1 calc R . . C19 C 0.7865(5) 0.8427(3) 0.5026(3) 0.0516(13) Uani 1 1 d . . . C20 C 0.9279(6) 0.2106(4) 0.2696(4) 0.0670(16) Uani 1 1 d . . . C21 C 0.8415(5) 0.2478(3) 0.2178(3) 0.0490(12) Uani 1 1 d . . . C22 C 0.8610(5) 0.3280(3) 0.2251(3) 0.0546(13) Uani 1 1 d . . . H22 H 0.9228 0.3565 0.2634 0.066 Uiso 1 1 calc R . . C23 C 0.7912(5) 0.3685(3) 0.1769(3) 0.0456(11) Uani 1 1 d . . . C24 C 0.8094(5) 0.4547(3) 0.1911(3) 0.0485(12) Uani 1 1 d . . . C25 C 0.9213(5) 0.5034(3) 0.2297(3) 0.0601(15) Uani 1 1 d . . . H25 H 0.9902 0.4830 0.2475 0.072 Uiso 1 1 calc R . . C26 C 0.9297(6) 0.5820(3) 0.2414(4) 0.0704(18) Uani 1 1 d . . . H26 H 1.0048 0.6146 0.2669 0.084 Uiso 1 1 calc R . . C27 C 0.8277(6) 0.6134(3) 0.2156(3) 0.0624(15) Uani 1 1 d . . . H27 H 0.8348 0.6666 0.2242 0.075 Uiso 1 1 calc R . . C28 C 0.7148(5) 0.5654(3) 0.1772(3) 0.0478(12) Uani 1 1 d . . . C29 C 0.7072(5) 0.4860(3) 0.1647(3) 0.0469(12) Uani 1 1 d . . . H29 H 0.6327 0.4534 0.1385 0.056 Uiso 1 1 calc R . . C30 C 0.6057(5) 0.5981(3) 0.1478(3) 0.0479(12) Uani 1 1 d . . . C31 C 0.5369(6) 0.5739(3) 0.0769(3) 0.0563(14) Uani 1 1 d . . . H31 H 0.5588 0.5360 0.0491 0.068 Uiso 1 1 calc R . . C32 C 0.4378(5) 0.6050(3) 0.0475(3) 0.0565(14) Uani 1 1 d . . . H32 H 0.3944 0.5891 0.0000 0.068 Uiso 1 1 calc R . . C33 C 0.4034(5) 0.6596(3) 0.0887(3) 0.0533(13) Uani 1 1 d . . . H33 H 0.3360 0.6804 0.0688 0.064 Uiso 1 1 calc R . . C34 C 0.4670(5) 0.6842(3) 0.1592(3) 0.0447(11) Uani 1 1 d . . . C35 C 0.5686(5) 0.6538(3) 0.1881(3) 0.0481(12) Uani 1 1 d . . . H35 H 0.6127 0.6709 0.2353 0.058 Uiso 1 1 calc R . . C36 C 0.4311(5) 0.7408(3) 0.2078(3) 0.0503(12) Uani 1 1 d . . . C37 C 0.3055(5) 0.7513(3) 0.1940(3) 0.0563(14) Uani 1 1 d . . . H37 H 0.2496 0.7255 0.1522 0.068 Uiso 1 1 calc R . . C38 C 0.2636(5) 0.7976(4) 0.2396(3) 0.0580(14) Uani 1 1 d . . . C39 C 0.1272(7) 0.8039(5) 0.2184(4) 0.079(2) Uani 1 1 d . . . C40 C 0.2559(6) 0.1575(4) -0.1181(3) 0.0641(16) Uani 1 1 d . . . C41 C 0.3280(5) 0.2052(3) -0.0469(3) 0.0544(13) Uani 1 1 d . . . C42 C 0.2759(6) 0.2604(3) -0.0205(3) 0.0615(15) Uani 1 1 d . . . H42 H 0.2010 0.2680 -0.0476 0.074 Uiso 1 1 calc R . . C43 C 0.3300(6) 0.3071(3) 0.0462(3) 0.0564(14) Uani 1 1 d . . . C44 C 0.2708(5) 0.3703(3) 0.0696(3) 0.0538(13) Uani 1 1 d . . . C45 C 0.2040(6) 0.4089(4) 0.0200(3) 0.0631(15) Uani 1 1 d . . . H45 H 0.1912 0.3943 -0.0294 0.076 Uiso 1 1 calc R . . C46 C 0.1565(6) 0.4693(4) 0.0444(4) 0.0699(17) Uani 1 1 d . . . H46 H 0.1152 0.4967 0.0111 0.084 Uiso 1 1 calc R . . C47 C 0.1698(6) 0.4892(4) 0.1174(3) 0.0629(15) Uani 1 1 d . . . H47 H 0.1362 0.5294 0.1328 0.075 Uiso 1 1 calc R . . C48 C 0.2325(5) 0.4501(3) 0.1679(3) 0.0523(13) Uani 1 1 d . . . C49 C 0.2857(5) 0.3915(3) 0.1439(3) 0.0545(13) Uani 1 1 d . . . H49 H 0.3312 0.3663 0.1774 0.065 Uiso 1 1 calc R . . C50 C 0.2391(5) 0.4676(3) 0.2471(3) 0.0493(12) Uani 1 1 d . . . C51 C 0.2056(5) 0.4076(3) 0.2888(3) 0.0589(14) Uani 1 1 d . . . H51 H 0.1871 0.3563 0.2682 0.071 Uiso 1 1 calc R . . C52 C 0.1989(6) 0.4223(3) 0.3602(3) 0.0596(14) Uani 1 1 d . . . H52 H 0.1756 0.3811 0.3870 0.072 Uiso 1 1 calc R . . C53 C 0.2268(5) 0.4981(3) 0.3919(3) 0.0562(14) Uani 1 1 d . . . H53 H 0.2205 0.5081 0.4397 0.067 Uiso 1 1 calc R . . C54 C 0.2645(5) 0.5594(3) 0.3519(3) 0.0483(12) Uani 1 1 d . . . C55 C 0.2693(5) 0.5440(3) 0.2798(3) 0.0506(12) Uani 1 1 d . . . H55 H 0.2929 0.5851 0.2529 0.061 Uiso 1 1 calc R . . C56 C 0.3036(5) 0.6431(3) 0.3849(3) 0.0491(12) Uani 1 1 d . . . C57 C 0.2623(5) 0.6652(3) 0.4477(3) 0.0568(14) Uani 1 1 d . . . H57 H 0.2061 0.6285 0.4660 0.068 Uiso 1 1 calc R . . C58 C 0.3037(5) 0.7400(3) 0.4822(3) 0.0512(13) Uani 1 1 d . . . C59 C 0.2435(6) 0.7608(4) 0.5449(4) 0.0659(16) Uani 1 1 d . . . C60 C 0.8582(7) 0.2435(5) 0.0283(4) 0.098(3) Uani 1 1 d . . . H60A H 0.8990 0.2115 0.0595 0.147 Uiso 1 1 calc R . . H60B H 0.8718 0.2944 0.0532 0.147 Uiso 1 1 calc R . . H60C H 0.8926 0.2476 -0.0146 0.147 Uiso 1 1 calc R . . C61 C 0.6950(8) 0.1340(5) -0.0317(4) 0.092(2) Uani 1 1 d . . . H61A H 0.7558 0.1316 -0.0618 0.110 Uiso 1 1 calc R . . H61B H 0.6124 0.1259 -0.0633 0.110 Uiso 1 1 calc R . . C62 C 0.6943(8) 0.0716(4) 0.0172(5) 0.094(2) Uani 1 1 d . . . H62A H 0.6713 0.0209 -0.0106 0.113 Uiso 1 1 calc R . . H62B H 0.7772 0.0779 0.0480 0.113 Uiso 1 1 calc R . . C63 C 0.6014(9) 0.0229(5) 0.1131(5) 0.106(3) Uani 1 1 d . . . H63A H 0.5804 -0.0290 0.0891 0.158 Uiso 1 1 calc R . . H63B H 0.5393 0.0284 0.1408 0.158 Uiso 1 1 calc R . . H63C H 0.6828 0.0325 0.1450 0.158 Uiso 1 1 calc R . . C64 C 0.7781(8) 0.9176(5) 0.3269(4) 0.098(3) Uani 1 1 d . . . H64A H 0.8083 0.9521 0.2935 0.147 Uiso 1 1 calc R . . H64B H 0.7677 0.8646 0.3077 0.147 Uiso 1 1 calc R . . H64C H 0.8380 0.9281 0.3723 0.147 Uiso 1 1 calc R . . C65 C 0.6672(10) 1.0066(4) 0.3702(5) 0.110(3) Uani 1 1 d . . . H65A H 0.7079 1.0454 0.3427 0.132 Uiso 1 1 calc R . . H65B H 0.7163 1.0144 0.4195 0.132 Uiso 1 1 calc R . . C66 C 0.5358(11) 1.0143(5) 0.3699(6) 0.118(3) Uani 1 1 d . . . H66A H 0.5377 1.0653 0.3926 0.142 Uiso 1 1 calc R . . H66B H 0.4881 1.0088 0.3205 0.142 Uiso 1 1 calc R . . C67 C 0.3582(8) 0.9673(5) 0.4184(5) 0.101(3) Uani 1 1 d . . . H67A H 0.3704 1.0162 0.4467 0.151 Uiso 1 1 calc R . . H67B H 0.3190 0.9259 0.4431 0.151 Uiso 1 1 calc R . . H67C H 0.3049 0.9676 0.3720 0.151 Uiso 1 1 calc R . . C68 C 0.8779(6) 0.9008(4) 0.5622(4) 0.0644(16) Uani 1 1 d . . . F1 F 0.1687(12) 0.0500(7) 0.2196(5) 0.123(4) Uani 0.541(6) 1 d PDU . . F1' F 0.1221(13) 0.0685(9) 0.1914(7) 0.123(4) Uani 0.459(6) 1 d PDU . . F2 F 0.1931(11) 0.0070(6) 0.1151(6) 0.121(3) Uani 0.541(6) 1 d PDU . . F2' F 0.2593(11) -0.0035(6) 0.1662(7) 0.121(3) Uani 0.459(6) 1 d PDU . . F3' F 0.1563(12) 0.0579(10) 0.0846(6) 0.177(4) Uani 0.541(6) 1 d PDU . . F3 F 0.1116(14) 0.1047(8) 0.1177(8) 0.177(4) Uani 0.459(6) 1 d PDU . . F4 F 0.9936(4) 0.8904(3) 0.5747(3) 0.1071(16) Uani 1 1 d . . . F5 F 0.8405(5) 0.8972(3) 0.6237(2) 0.1192(18) Uani 1 1 d . . . F6 F 0.8866(4) 0.9727(2) 0.5461(3) 0.0995(14) Uani 1 1 d . . . F7 F 1.0166(6) 0.1948(4) 0.2403(3) 0.156(3) Uani 1 1 d . . . F8 F 0.8692(5) 0.1475(3) 0.2892(3) 0.163(3) Uani 1 1 d . . . F9 F 0.9908(5) 0.2550(2) 0.3293(2) 0.1047(15) Uani 1 1 d . . . F10 F 0.0630(5) 0.7638(5) 0.1593(3) 0.164(3) Uani 1 1 d . . . F11 F 0.1162(5) 0.8732(3) 0.2165(5) 0.179(3) Uani 1 1 d . . . F12 F 0.0642(4) 0.7788(4) 0.2678(3) 0.1269(19) Uani 1 1 d . . . F13 F 0.1857(5) 0.0917(3) -0.1065(3) 0.1135(16) Uani 1 1 d . . . F14 F 0.3342(4) 0.1373(2) -0.15744(19) 0.0847(11) Uani 1 1 d . . . F15 F 0.1842(5) 0.1935(3) -0.1612(2) 0.1095(17) Uani 1 1 d . . . F16 F 0.1684(5) 0.7004(2) 0.5649(3) 0.1115(17) Uani 1 1 d . . . F17 F 0.1750(4) 0.8106(3) 0.5267(2) 0.1044(15) Uani 1 1 d . . . F18 F 0.3281(4) 0.7942(3) 0.6033(2) 0.0936(13) 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 O1 0.095(3) 0.066(3) 0.075(3) -0.011(2) 0.040(3) 0.000(3) O2 0.062(2) 0.064(2) 0.045(2) -0.0075(18) 0.0139(18) 0.009(2) O3 0.068(2) 0.049(2) 0.060(2) -0.0069(18) -0.005(2) 0.026(2) O4 0.056(2) 0.049(2) 0.065(2) -0.0142(18) -0.0008(19) 0.0172(19) O5 0.059(2) 0.044(2) 0.059(2) 0.0000(17) 0.0018(18) 0.0213(18) O6 0.057(2) 0.0405(19) 0.053(2) -0.0012(16) 0.0043(17) 0.0156(17) O7 0.052(2) 0.052(2) 0.049(2) -0.0074(17) 0.0064(17) 0.0155(18) O8 0.056(2) 0.059(2) 0.069(3) -0.012(2) 0.0045(19) 0.028(2) O9 0.069(3) 0.063(2) 0.051(2) -0.0111(18) 0.0028(19) 0.032(2) O10 0.065(2) 0.064(2) 0.052(2) -0.0103(18) 0.0028(18) 0.036(2) O11 0.069(3) 0.042(2) 0.069(3) -0.0133(18) 0.023(2) -0.006(2) O12 0.067(2) 0.047(2) 0.065(2) -0.0112(18) 0.022(2) 0.008(2) O13 0.083(3) 0.076(3) 0.061(3) -0.006(2) 0.016(2) 0.035(3) O14 0.093(3) 0.049(2) 0.078(3) -0.003(2) 0.010(3) 0.023(2) O15 0.098(4) 0.065(3) 0.074(3) -0.004(2) 0.018(3) -0.015(3) O16 0.091(3) 0.049(2) 0.087(3) -0.008(2) 0.002(3) 0.020(2) Nd1 0.05096(18) 0.03833(16) 0.05007(17) -0.00748(12) 0.00826(13) 0.01085(13) Nd2 0.05675(19) 0.04306(17) 0.04396(16) -0.00560(12) 0.00656(13) 0.01846(14) C1 0.165(8) 0.149(8) 0.155(8) -0.024(6) 0.096(7) 0.014(7) C2 0.092(5) 0.052(4) 0.101(5) -0.024(4) 0.042(4) -0.016(4) C3 0.098(5) 0.063(4) 0.090(5) -0.021(4) 0.048(4) -0.009(4) C4 0.066(4) 0.041(3) 0.056(3) -0.004(2) 0.014(3) 0.015(3) C5 0.061(3) 0.047(3) 0.048(3) -0.002(2) 0.015(2) 0.015(3) C6 0.067(4) 0.058(4) 0.064(4) -0.002(3) 0.023(3) 0.004(3) C7 0.064(4) 0.068(4) 0.064(4) -0.007(3) 0.031(3) 0.004(3) C8 0.065(4) 0.076(4) 0.049(3) -0.007(3) 0.017(3) 0.029(3) C9 0.056(3) 0.046(3) 0.053(3) 0.001(2) 0.011(3) 0.020(3) C10 0.061(3) 0.048(3) 0.046(3) 0.001(2) 0.016(3) 0.012(3) C11 0.061(3) 0.045(3) 0.048(3) -0.001(2) 0.011(2) 0.019(3) C12 0.068(4) 0.042(3) 0.087(4) -0.002(3) 0.020(3) 0.018(3) C13 0.056(4) 0.059(4) 0.122(6) -0.001(4) 0.021(4) 0.024(3) C14 0.056(3) 0.047(3) 0.091(5) -0.006(3) 0.013(3) 0.013(3) C15 0.058(3) 0.042(3) 0.048(3) -0.001(2) 0.007(2) 0.011(3) C16 0.058(3) 0.056(3) 0.049(3) -0.002(2) 0.011(2) 0.024(3) C17 0.067(4) 0.044(3) 0.046(3) 0.002(2) 0.013(3) 0.016(3) C18 0.055(3) 0.049(3) 0.059(3) -0.004(3) 0.001(3) 0.015(3) C19 0.059(3) 0.046(3) 0.045(3) -0.004(2) 0.011(2) 0.006(3) C20 0.071(4) 0.050(3) 0.077(4) 0.016(3) 0.000(3) 0.019(3) C21 0.049(3) 0.046(3) 0.054(3) 0.004(2) 0.010(2) 0.016(3) C22 0.055(3) 0.050(3) 0.057(3) 0.005(3) 0.001(3) 0.016(3) C23 0.043(3) 0.040(3) 0.056(3) -0.002(2) 0.012(2) 0.014(2) C24 0.060(3) 0.043(3) 0.047(3) 0.001(2) 0.013(2) 0.022(3) C25 0.044(3) 0.045(3) 0.085(4) 0.002(3) 0.002(3) 0.010(3) C26 0.052(3) 0.047(3) 0.101(5) -0.001(3) -0.004(3) 0.007(3) C27 0.061(4) 0.040(3) 0.080(4) -0.002(3) 0.003(3) 0.013(3) C28 0.053(3) 0.045(3) 0.047(3) -0.001(2) 0.009(2) 0.016(3) C29 0.050(3) 0.044(3) 0.047(3) 0.000(2) 0.008(2) 0.014(2) C30 0.055(3) 0.039(3) 0.049(3) 0.000(2) 0.007(2) 0.014(2) C31 0.070(4) 0.051(3) 0.048(3) -0.007(2) 0.008(3) 0.022(3) C32 0.066(4) 0.061(3) 0.040(3) -0.004(2) -0.004(2) 0.026(3) C33 0.062(3) 0.052(3) 0.046(3) -0.003(2) 0.001(2) 0.023(3) C34 0.052(3) 0.038(3) 0.045(3) 0.001(2) 0.009(2) 0.014(2) C35 0.060(3) 0.042(3) 0.042(3) -0.002(2) 0.006(2) 0.017(3) C36 0.058(3) 0.053(3) 0.046(3) 0.005(2) 0.011(2) 0.026(3) C37 0.054(3) 0.060(3) 0.053(3) -0.005(3) 0.001(3) 0.021(3) C38 0.051(3) 0.062(4) 0.063(4) -0.001(3) 0.005(3) 0.027(3) C39 0.068(4) 0.091(5) 0.085(5) -0.006(4) 0.010(4) 0.043(4) C40 0.066(4) 0.056(4) 0.064(4) -0.009(3) -0.004(3) 0.021(3) C41 0.057(3) 0.056(3) 0.050(3) -0.002(3) 0.006(3) 0.020(3) C42 0.058(3) 0.063(4) 0.061(3) -0.011(3) -0.002(3) 0.025(3) C43 0.064(4) 0.052(3) 0.055(3) -0.004(3) 0.013(3) 0.020(3) C44 0.052(3) 0.052(3) 0.059(3) -0.007(3) 0.008(3) 0.022(3) C45 0.066(4) 0.067(4) 0.058(3) -0.005(3) 0.009(3) 0.026(3) C46 0.074(4) 0.079(4) 0.069(4) 0.010(3) 0.012(3) 0.046(4) C47 0.065(4) 0.054(3) 0.075(4) -0.004(3) 0.017(3) 0.026(3) C48 0.047(3) 0.047(3) 0.061(3) -0.006(3) 0.009(3) 0.012(3) C49 0.056(3) 0.050(3) 0.058(3) -0.006(3) 0.006(3) 0.023(3) C50 0.044(3) 0.043(3) 0.060(3) -0.007(2) 0.010(2) 0.013(2) C51 0.059(3) 0.042(3) 0.072(4) -0.008(3) 0.011(3) 0.011(3) C52 0.068(4) 0.044(3) 0.064(4) 0.002(3) 0.011(3) 0.010(3) C53 0.060(3) 0.051(3) 0.056(3) -0.006(3) 0.015(3) 0.011(3) C54 0.040(3) 0.042(3) 0.059(3) -0.008(2) 0.009(2) 0.008(2) C55 0.046(3) 0.039(3) 0.065(3) -0.004(2) 0.014(3) 0.007(2) C56 0.041(3) 0.039(3) 0.059(3) -0.009(2) 0.003(2) 0.002(2) C57 0.055(3) 0.046(3) 0.067(4) -0.008(3) 0.023(3) 0.003(3) C58 0.051(3) 0.048(3) 0.054(3) -0.008(2) 0.006(2) 0.017(3) C59 0.072(4) 0.057(4) 0.073(4) -0.007(3) 0.026(3) 0.017(3) C60 0.084(5) 0.138(8) 0.086(5) 0.005(5) 0.032(4) 0.045(5) C61 0.118(6) 0.092(5) 0.075(5) -0.016(4) 0.033(4) 0.041(5) C62 0.122(7) 0.078(5) 0.104(6) -0.005(4) 0.040(5) 0.057(5) C63 0.130(7) 0.065(5) 0.115(7) 0.016(5) 0.007(6) 0.026(5) C64 0.094(6) 0.110(7) 0.077(5) -0.009(4) 0.028(4) -0.010(5) C65 0.135(8) 0.052(4) 0.123(7) -0.004(4) 0.034(6) -0.020(5) C66 0.156(10) 0.067(5) 0.130(8) 0.003(5) 0.021(7) 0.032(6) C67 0.107(6) 0.092(6) 0.111(6) -0.027(5) 0.012(5) 0.059(5) C68 0.058(4) 0.061(4) 0.069(4) -0.007(3) 0.001(3) 0.017(3) F1 0.115(6) 0.110(5) 0.125(6) -0.026(4) 0.051(5) -0.024(4) F1' 0.115(6) 0.110(5) 0.125(6) -0.026(4) 0.051(5) -0.024(4) F2 0.134(6) 0.094(4) 0.117(5) -0.024(4) 0.049(4) -0.025(4) F2' 0.134(6) 0.094(4) 0.117(5) -0.024(4) 0.049(4) -0.025(4) F3' 0.142(6) 0.179(7) 0.183(7) -0.020(6) 0.031(5) -0.006(5) F3 0.142(6) 0.179(7) 0.183(7) -0.020(6) 0.031(5) -0.006(5) F4 0.074(3) 0.091(3) 0.132(4) -0.043(3) -0.027(2) 0.025(2) F5 0.142(4) 0.128(4) 0.063(3) -0.032(3) 0.019(3) -0.006(3) F6 0.097(3) 0.055(2) 0.121(4) -0.009(2) -0.020(3) 0.006(2) F7 0.156(5) 0.219(7) 0.140(5) 0.031(5) 0.022(4) 0.149(6) F8 0.142(5) 0.096(4) 0.187(6) 0.089(4) -0.075(4) -0.032(3) F9 0.118(4) 0.075(3) 0.093(3) 0.014(2) -0.039(3) 0.017(3) F10 0.082(3) 0.289(9) 0.113(4) -0.076(5) -0.026(3) 0.091(5) F11 0.078(3) 0.095(4) 0.365(11) 0.053(5) 0.007(5) 0.052(3) F12 0.073(3) 0.178(6) 0.132(4) 0.004(4) 0.031(3) 0.029(3) F13 0.117(4) 0.085(3) 0.111(4) -0.024(3) 0.021(3) -0.023(3) F14 0.104(3) 0.095(3) 0.056(2) -0.0163(19) 0.006(2) 0.040(2) F15 0.123(4) 0.104(3) 0.088(3) -0.034(2) -0.041(3) 0.065(3) F16 0.143(4) 0.076(3) 0.122(4) -0.015(3) 0.087(3) -0.006(3) F17 0.118(3) 0.120(4) 0.109(3) 0.011(3) 0.047(3) 0.079(3) F18 0.102(3) 0.107(3) 0.065(2) -0.024(2) 0.018(2) 0.020(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 O1 C2 1.243(8) . ? O1 Nd2 2.359(4) . ? O2 C4 1.247(7) . ? O2 Nd2 2.400(3) . ? O3 C17 1.260(7) . ? O3 Nd1 2.421(4) . ? O4 C19 1.266(7) . ? O4 Nd1 2.406(4) . ? O5 C21 1.258(6) . ? O5 Nd2 2.410(4) . ? O6 C23 1.252(6) . ? O6 Nd2 2.370(4) . ? O7 C36 1.253(6) . ? O7 Nd1 2.352(3) . ? O8 C38 1.252(7) . ? O8 Nd1 2.401(4) . ? O9 C41 1.259(6) . ? O9 Nd2 2.384(4) . ? O10 C43 1.255(7) . ? O10 Nd2 2.413(3) . ? O11 C56 1.233(6) . ? O11 Nd1 2.413(4) . ? O12 C58 1.263(7) . ? O12 Nd1 2.364(4) . ? O13 C60 1.423(9) . ? O13 C61 1.433(8) . ? O13 Nd2 2.638(4) . ? O14 C62 1.428(8) . ? O14 C63 1.436(9) . ? O14 Nd2 2.563(4) . ? O15 C64 1.435(9) . ? O15 C65 1.440(9) . ? O15 Nd1 2.566(5) . ? O16 C66 1.412(10) . ? O16 C67 1.441(8) . ? O16 Nd1 2.554(4) . ? C1 F2 1.211(11) . ? C1 F1' 1.285(12) . ? C1 F3' 1.327(12) . ? C1 F1 1.399(12) . ? C1 F2' 1.474(13) . ? C1 F3 1.481(14) . ? C1 C2 1.554(13) . ? C2 C3 1.388(9) . ? C3 C4 1.409(9) . ? C3 H3 0.9300 . ? C4 C5 1.495(7) . ? C5 C10 1.383(8) . ? C5 C6 1.389(8) . ? C6 C7 1.377(8) . ? C6 H6 0.9300 . ? C7 C8 1.381(8) . ? C7 H7 0.9300 . ? C8 C9 1.390(8) . ? C8 H8 0.9300 . ? C9 C10 1.389(7) . ? C9 C11 1.493(8) . ? C10 H10 0.9300 . ? C11 C12 1.378(8) . ? C11 C16 1.391(7) . ? C12 C13 1.382(9) . ? C12 H12 0.9300 . ? C13 C14 1.380(8) . ? C13 H13 0.9300 . ? C14 C15 1.379(8) . ? C14 H14 0.9300 . ? C15 C16 1.386(8) . ? C15 C17 1.499(7) . ? C16 H16 0.9300 . ? C17 C18 1.414(7) . ? C18 C19 1.380(7) . ? C18 H18 0.9300 . ? C19 C68 1.527(8) . ? C20 F8 1.276(8) . ? C20 F7 1.293(8) . ? C20 F9 1.318(7) . ? C20 C21 1.518(8) . ? C21 C22 1.383(7) . ? C22 C23 1.412(7) . ? C22 H22 0.9300 . ? C23 C24 1.493(7) . ? C24 C25 1.391(8) . ? C24 C29 1.391(7) . ? C25 C26 1.374(8) . ? C25 H25 0.9300 . ? C26 C27 1.387(8) . ? C26 H26 0.9300 . ? C27 C28 1.391(8) . ? C27 H27 0.9300 . ? C28 C29 1.393(7) . ? C28 C30 1.482(7) . ? C29 H29 0.9300 . ? C30 C35 1.391(7) . ? C30 C31 1.402(7) . ? C31 C32 1.374(7) . ? C31 H31 0.9300 . ? C32 C33 1.370(7) . ? C32 H32 0.9300 . ? C33 C34 1.379(7) . ? C33 H33 0.9300 . ? C34 C35 1.388(7) . ? C34 C36 1.490(7) . ? C35 H35 0.9300 . ? C36 C37 1.424(7) . ? C37 C38 1.369(7) . ? C37 H37 0.9300 . ? C38 C39 1.522(8) . ? C39 F11 1.260(9) . ? C39 F10 1.283(8) . ? C39 F12 1.313(9) . ? C40 F13 1.307(8) . ? C40 F15 1.317(7) . ? C40 F14 1.340(7) . ? C40 C41 1.525(8) . ? C41 C42 1.358(7) . ? C42 C43 1.417(7) . ? C42 H42 0.9300 . ? C43 C44 1.502(7) . ? C44 C45 1.388(8) . ? C44 C49 1.401(7) . ? C45 C46 1.385(8) . ? C45 H45 0.9300 . ? C46 C47 1.376(9) . ? C46 H46 0.9300 . ? C47 C48 1.380(8) . ? C47 H47 0.9300 . ? C48 C49 1.397(7) . ? C48 C50 1.497(7) . ? C49 H49 0.9300 . ? C50 C51 1.386(8) . ? C50 C55 1.395(7) . ? C51 C52 1.379(8) . ? C51 H51 0.9300 . ? C52 C53 1.381(7) . ? C52 H52 0.9300 . ? C53 C54 1.394(8) . ? C53 H53 0.9300 . ? C54 C55 1.388(7) . ? C54 C56 1.509(7) . ? C55 H55 0.9300 . ? C56 C57 1.418(7) . ? C57 C58 1.381(7) . ? C57 H57 0.9300 . ? C58 C59 1.534(8) . ? C59 F17 1.305(7) . ? C59 F18 1.318(7) . ? C59 F16 1.326(7) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C62 1.480(11) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.496(12) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 F5 1.309(8) . ? C68 F6 1.313(7) . ? C68 F4 1.318(7) . ? F1 F1' 0.805(19) . ? F1' F3 1.562(19) . ? F2 F2' 1.148(14) . ? F2 F3' 1.200(16) . ? F3' F3 1.251(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 Nd2 131.4(4) . . ? C4 O2 Nd2 135.6(4) . . ? C17 O3 Nd1 140.5(3) . . ? C19 O4 Nd1 136.0(3) . . ? C21 O5 Nd2 129.9(3) . . ? C23 O6 Nd2 133.0(3) . . ? C36 O7 Nd1 132.9(3) . . ? C38 O8 Nd1 129.5(3) . . ? C41 O9 Nd2 133.8(3) . . ? C43 O10 Nd2 137.5(3) . . ? C56 O11 Nd1 138.3(3) . . ? C58 O12 Nd1 134.7(3) . . ? C60 O13 C61 114.2(6) . . ? C60 O13 Nd2 124.3(4) . . ? C61 O13 Nd2 109.1(4) . . ? C62 O14 C63 111.6(6) . . ? C62 O14 Nd2 119.9(4) . . ? C63 O14 Nd2 117.9(4) . . ? C64 O15 C65 113.2(6) . . ? C64 O15 Nd1 119.1(5) . . ? C65 O15 Nd1 115.8(5) . . ? C66 O16 C67 110.6(6) . . ? C66 O16 Nd1 116.5(5) . . ? C67 O16 Nd1 120.4(4) . . ? O7 Nd1 O12 143.02(13) . . ? O7 Nd1 O8 71.11(12) . . ? O12 Nd1 O8 88.54(14) . . ? O7 Nd1 O4 125.84(13) . . ? O12 Nd1 O4 86.01(14) . . ? O8 Nd1 O4 152.37(12) . . ? O7 Nd1 O11 74.40(13) . . ? O12 Nd1 O11 70.89(13) . . ? O8 Nd1 O11 76.41(15) . . ? O4 Nd1 O11 126.54(14) . . ? O7 Nd1 O3 75.93(13) . . ? O12 Nd1 O3 103.61(14) . . ? O8 Nd1 O3 138.31(12) . . ? O4 Nd1 O3 69.16(12) . . ? O11 Nd1 O3 70.62(14) . . ? O7 Nd1 O16 119.76(15) . . ? O12 Nd1 O16 79.32(15) . . ? O8 Nd1 O16 71.09(14) . . ? O4 Nd1 O16 81.28(14) . . ? O11 Nd1 O16 136.00(15) . . ? O3 Nd1 O16 149.86(14) . . ? O7 Nd1 O15 74.15(14) . . ? O12 Nd1 O15 139.88(14) . . ? O8 Nd1 O15 94.66(16) . . ? O4 Nd1 O15 72.95(15) . . ? O11 Nd1 O15 148.52(14) . . ? O3 Nd1 O15 100.23(17) . . ? O16 Nd1 O15 64.23(17) . . ? O1 Nd2 O6 147.42(13) . . ? O1 Nd2 O9 81.98(16) . . ? O6 Nd2 O9 116.77(13) . . ? O1 Nd2 O2 70.94(14) . . ? O6 Nd2 O2 77.58(13) . . ? O9 Nd2 O2 135.55(13) . . ? O1 Nd2 O5 107.28(16) . . ? O6 Nd2 O5 71.37(12) . . ? O9 Nd2 O5 148.50(12) . . ? O2 Nd2 O5 74.91(13) . . ? O1 Nd2 O10 85.17(16) . . ? O6 Nd2 O10 77.26(13) . . ? O9 Nd2 O10 71.10(12) . . ? O2 Nd2 O10 72.07(13) . . ? O5 Nd2 O10 138.33(12) . . ? O1 Nd2 O14 75.27(16) . . ? O6 Nd2 O14 130.75(14) . . ? O9 Nd2 O14 82.20(13) . . ? O2 Nd2 O14 121.73(14) . . ? O5 Nd2 O14 71.74(13) . . ? O10 Nd2 O14 148.85(14) . . ? O1 Nd2 O13 136.49(14) . . ? O6 Nd2 O13 75.58(13) . . ? O9 Nd2 O13 78.37(14) . . ? O2 Nd2 O13 144.30(14) . . ? O5 Nd2 O13 74.49(13) . . ? O10 Nd2 O13 123.21(14) . . ? O14 Nd2 O13 63.91(15) . . ? F2 C1 F1' 117.0(13) . . ? F2 C1 F3' 56.2(8) . . ? F1' C1 F3' 109.4(12) . . ? F2 C1 F1 112.0(11) . . ? F1' C1 F1 34.6(9) . . ? F3' C1 F1 137.9(13) . . ? F2 C1 F2' 49.4(7) . . ? F1' C1 F2' 111.9(11) . . ? F3' C1 F2' 104.7(10) . . ? F1 C1 F2' 83.1(9) . . ? F2 C1 F3 103.6(11) . . ? F1' C1 F3 68.4(10) . . ? F3' C1 F3 52.6(8) . . ? F1 C1 F3 102.8(9) . . ? F2' C1 F3 151.4(12) . . ? F2 C1 C2 121.5(9) . . ? F1' C1 C2 120.8(11) . . ? F3' C1 C2 109.7(10) . . ? F1 C1 C2 109.6(10) . . ? F2' C1 C2 98.9(9) . . ? F3 C1 C2 105.1(10) . . ? O1 C2 C3 130.3(6) . . ? O1 C2 C1 112.7(6) . . ? C3 C2 C1 117.0(7) . . ? C2 C3 C4 121.5(6) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? O2 C4 C3 123.0(5) . . ? O2 C4 C5 117.6(5) . . ? C3 C4 C5 119.4(5) . . ? C10 C5 C6 119.6(5) . . ? C10 C5 C4 118.7(5) . . ? C6 C5 C4 121.8(5) . . ? C7 C6 C5 119.6(6) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 120.5(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 120.8(5) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 118.1(5) . . ? C10 C9 C11 122.4(5) . . ? C8 C9 C11 119.3(5) . . ? C5 C10 C9 121.4(5) . . ? C5 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C12 C11 C16 117.8(5) . . ? C12 C11 C9 119.3(5) . . ? C16 C11 C9 122.8(5) . . ? C11 C12 C13 121.0(5) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 120.3(6) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.0(6) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 118.9(5) . . ? C14 C15 C17 121.8(5) . . ? C16 C15 C17 119.2(5) . . ? C15 C16 C11 121.8(5) . . ? C15 C16 H16 119.1 . . ? C11 C16 H16 119.1 . . ? O3 C17 C18 122.6(5) . . ? O3 C17 C15 116.8(5) . . ? C18 C17 C15 120.6(5) . . ? C19 C18 C17 122.2(5) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? O4 C19 C18 128.3(5) . . ? O4 C19 C68 113.3(5) . . ? C18 C19 C68 118.3(5) . . ? F8 C20 F7 107.9(7) . . ? F8 C20 F9 106.7(6) . . ? F7 C20 F9 102.9(6) . . ? F8 C20 C21 112.5(6) . . ? F7 C20 C21 110.8(6) . . ? F9 C20 C21 115.3(5) . . ? O5 C21 C22 128.7(5) . . ? O5 C21 C20 112.9(5) . . ? C22 C21 C20 118.4(5) . . ? C21 C22 C23 122.8(5) . . ? C21 C22 H22 118.6 . . ? C23 C22 H22 118.6 . . ? O6 C23 C22 123.7(5) . . ? O6 C23 C24 116.1(4) . . ? C22 C23 C24 120.2(5) . . ? C25 C24 C29 119.6(5) . . ? C25 C24 C23 123.3(5) . . ? C29 C24 C23 117.1(5) . . ? C26 C25 C24 119.6(5) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 121.0(6) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C28 120.2(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C29 118.7(5) . . ? C27 C28 C30 121.0(5) . . ? C29 C28 C30 120.3(5) . . ? C24 C29 C28 121.0(5) . . ? C24 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C35 C30 C31 117.6(5) . . ? C35 C30 C28 122.3(5) . . ? C31 C30 C28 120.1(4) . . ? C32 C31 C30 121.4(5) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C33 C32 C31 119.6(5) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 121.0(5) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C33 C34 C35 119.1(4) . . ? C33 C34 C36 123.7(5) . . ? C35 C34 C36 117.1(4) . . ? C34 C35 C30 121.2(5) . . ? C34 C35 H35 119.4 . . ? C30 C35 H35 119.4 . . ? O7 C36 C37 122.8(5) . . ? O7 C36 C34 117.3(4) . . ? C37 C36 C34 119.9(5) . . ? C38 C37 C36 122.9(5) . . ? C38 C37 H37 118.6 . . ? C36 C37 H37 118.6 . . ? O8 C38 C37 128.5(5) . . ? O8 C38 C39 113.8(5) . . ? C37 C38 C39 117.6(5) . . ? F11 C39 F10 109.0(8) . . ? F11 C39 F12 102.8(7) . . ? F10 C39 F12 104.4(7) . . ? F11 C39 C38 113.3(7) . . ? F10 C39 C38 115.5(6) . . ? F12 C39 C38 110.8(6) . . ? F13 C40 F15 108.3(6) . . ? F13 C40 F14 105.2(5) . . ? F15 C40 F14 105.3(6) . . ? F13 C40 C41 111.1(6) . . ? F15 C40 C41 114.7(5) . . ? F14 C40 C41 111.6(5) . . ? O9 C41 C42 129.3(5) . . ? O9 C41 C40 113.6(5) . . ? C42 C41 C40 117.0(5) . . ? C41 C42 C43 123.2(5) . . ? C41 C42 H42 118.4 . . ? C43 C42 H42 118.4 . . ? O10 C43 C42 123.3(5) . . ? O10 C43 C44 116.6(5) . . ? C42 C43 C44 120.0(5) . . ? C45 C44 C49 119.4(5) . . ? C45 C44 C43 122.0(5) . . ? C49 C44 C43 118.7(5) . . ? C46 C45 C44 119.6(6) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C47 C46 C45 120.8(6) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C46 C47 C48 120.7(5) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C47 C48 C49 118.9(5) . . ? C47 C48 C50 120.9(5) . . ? C49 C48 C50 120.1(5) . . ? C48 C49 C44 120.5(5) . . ? C48 C49 H49 119.8 . . ? C44 C49 H49 119.8 . . ? C51 C50 C55 118.1(5) . . ? C51 C50 C48 120.2(5) . . ? C55 C50 C48 121.5(5) . . ? C52 C51 C50 121.5(5) . . ? C52 C51 H51 119.2 . . ? C50 C51 H51 119.2 . . ? C51 C52 C53 120.0(6) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C52 C53 C54 119.6(5) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C55 C54 C53 119.7(5) . . ? C55 C54 C56 118.3(5) . . ? C53 C54 C56 122.0(5) . . ? C54 C55 C50 120.9(5) . . ? C54 C55 H55 119.6 . . ? C50 C55 H55 119.6 . . ? O11 C56 C57 123.4(5) . . ? O11 C56 C54 116.4(5) . . ? C57 C56 C54 120.1(5) . . ? C58 C57 C56 121.5(5) . . ? C58 C57 H57 119.2 . . ? C56 C57 H57 119.2 . . ? O12 C58 C57 129.6(5) . . ? O12 C58 C59 112.6(5) . . ? C57 C58 C59 117.7(5) . . ? F17 C59 F18 106.1(5) . . ? F17 C59 F16 106.5(6) . . ? F18 C59 F16 106.9(6) . . ? F17 C59 C58 110.3(6) . . ? F18 C59 C58 112.5(5) . . ? F16 C59 C58 114.1(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 . . ? O13 C61 C62 111.0(6) . . ? O13 C61 H61A 109.4 . . ? C62 C61 H61A 109.4 . . ? O13 C61 H61B 109.4 . . ? C62 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? O14 C62 C61 107.0(6) . . ? O14 C62 H62A 110.3 . . ? C61 C62 H62A 110.3 . . ? O14 C62 H62B 110.3 . . ? C61 C62 H62B 110.3 . . ? H62A C62 H62B 108.6 . . ? O14 C63 H63A 109.5 . . ? O14 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? O14 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O15 C64 H64A 109.5 . . ? O15 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? O15 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O15 C65 C66 107.7(7) . . ? O15 C65 H65A 110.2 . . ? C66 C65 H65A 110.2 . . ? O15 C65 H65B 110.2 . . ? C66 C65 H65B 110.2 . . ? H65A C65 H65B 108.5 . . ? O16 C66 C65 108.6(7) . . ? O16 C66 H66A 110.0 . . ? C65 C66 H66A 110.0 . . ? O16 C66 H66B 110.0 . . ? C65 C66 H66B 110.0 . . ? H66A C66 H66B 108.4 . . ? O16 C67 H67A 109.5 . . ? O16 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? O16 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? F5 C68 F6 106.6(6) . . ? F5 C68 F4 107.0(6) . . ? F6 C68 F4 106.3(6) . . ? F5 C68 C19 111.4(5) . . ? F6 C68 C19 111.4(5) . . ? F4 C68 C19 113.7(5) . . ? F1' F1 C1 64.9(11) . . ? F1 F1' C1 80.5(13) . . ? F1 F1' F3 142.0(16) . . ? C1 F1' F3 61.8(8) . . ? F2' F2 F3' 142.0(12) . . ? F2' F2 C1 77.3(9) . . ? F3' F2 C1 66.8(8) . . ? F2 F2' C1 53.3(7) . . ? F2 F3' F3 120.0(12) . . ? F2 F3' C1 57.0(7) . . ? F3 F3' C1 70.0(9) . . ? F3' F3 C1 57.4(7) . . ? F3' F3 F1' 97.9(10) . . ? C1 F3 F1' 49.9(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.117 _refine_diff_density_min -1.691 _refine_diff_density_rms 0.113 # Attachment '- 4.cif' data_shelxl_b _database_code_depnum_ccdc_archive 'CCDC 833525' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H50 F18 O16 Yb2' _chemical_formula_weight 1811.16 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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 10.8884(3) _cell_length_b 17.7585(5) _cell_length_c 18.8929(5) _cell_angle_alpha 94.2940(7) _cell_angle_beta 101.7520(7) _cell_angle_gamma 103.4720(7) _cell_volume 3449.34(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 2.810 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.532 _exptl_absorpt_correction_T_max 0.620 _exptl_absorpt_process_details SADABS _exptl_special_details ; "isor 0.01 f1 f2 f3 f1' f2' f3' f4 f5 f7 f10 f11 f12" commands have been added to define the elongated elipsoid parameters of the F atoms. The residual electron density of 3.065 is ascribed to a ghost peak around Yb1 atom. ; _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 SMART1000 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34043 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.56 _reflns_number_total 15669 _reflns_number_gt 12312 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT-plus _computing_data_reduction SAINT-plus _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_molecular_graphics SHELXL97 _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^)+(0.0385P)^2^+35.5401P] 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 15669 _refine_ls_number_parameters 969 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1646 _refine_ls_wR_factor_gt 0.1538 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.081 _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 O1 O 0.3904(7) 0.1295(4) 0.1136(4) 0.0589(18) Uani 1 1 d . . . O2 O 0.5496(6) 0.2510(3) 0.2119(3) 0.0437(14) Uani 1 1 d . . . O3 O 0.6264(6) 0.7249(3) 0.3942(4) 0.0496(15) Uani 1 1 d . . . O4 O 0.6757(6) 0.8651(3) 0.4769(4) 0.0480(15) Uani 1 1 d . . . O5 O 0.7508(6) 0.1999(3) 0.1722(3) 0.0423(13) Uani 1 1 d . . . O6 O 0.7034(6) 0.3344(3) 0.1235(3) 0.0400(13) Uani 1 1 d . . . O7 O 0.5162(5) 0.7735(3) 0.2653(3) 0.0402(13) Uani 1 1 d . . . O8 O 0.3265(6) 0.8349(4) 0.3031(4) 0.0528(16) Uani 1 1 d . . . O9 O 0.4443(6) 0.1869(4) -0.0175(3) 0.0478(15) Uani 1 1 d . . . O10 O 0.4354(6) 0.2983(4) 0.0885(3) 0.0479(15) Uani 1 1 d . . . O11 O 0.3695(7) 0.6918(3) 0.3503(3) 0.0498(15) Uani 1 1 d . . . O12 O 0.3961(6) 0.8002(3) 0.4659(3) 0.0460(14) Uani 1 1 d . . . O13 O 0.7258(7) 0.2147(4) 0.0160(3) 0.0514(16) Uani 1 1 d . . . O14 O 0.5934(7) 0.0836(4) 0.0644(4) 0.0564(17) Uani 1 1 d . . . O15 O 0.6609(9) 0.9144(5) 0.3383(4) 0.073(2) Uani 1 1 d . . . O16 O 0.4841(8) 0.9472(4) 0.4090(4) 0.070(2) Uani 1 1 d . . . Yb1 Yb 0.50547(4) 0.815810(19) 0.37778(2) 0.03837(11) Uani 1 1 d . . . Yb2 Yb 0.56787(3) 0.214473(19) 0.097357(19) 0.03689(10) Uani 1 1 d . . . C1 C 0.180(2) 0.0751(10) 0.1305(12) 0.120(8) Uani 1 1 d . . . C2 C 0.3157(11) 0.1346(6) 0.1564(6) 0.060(3) Uani 1 1 d . . . C3 C 0.3388(11) 0.1865(6) 0.2166(7) 0.065(3) Uani 1 1 d . . . H3 H 0.2730 0.1843 0.2416 0.078 Uiso 1 1 calc R . . C4 C 0.4565(9) 0.2437(5) 0.2441(5) 0.0425(19) Uani 1 1 d . . . C5 C 0.4751(9) 0.2999(5) 0.3095(5) 0.045(2) Uani 1 1 d . . . C6 C 0.4056(10) 0.2825(6) 0.3626(6) 0.053(2) Uani 1 1 d . . . H6 H 0.3458 0.2344 0.3574 0.064 Uiso 1 1 calc R . . C7 C 0.4245(10) 0.3352(7) 0.4222(5) 0.058(3) Uani 1 1 d . . . H7 H 0.3789 0.3231 0.4581 0.070 Uiso 1 1 calc R . . C8 C 0.5124(11) 0.4073(6) 0.4290(5) 0.055(3) Uani 1 1 d . . . H8 H 0.5219 0.4441 0.4688 0.067 Uiso 1 1 calc R . . C9 C 0.5855(9) 0.4258(5) 0.3789(5) 0.0427(19) Uani 1 1 d . . . C10 C 0.5666(9) 0.3714(5) 0.3191(5) 0.0413(19) Uani 1 1 d . . . H10 H 0.6157 0.3827 0.2845 0.050 Uiso 1 1 calc R . . C11 C 0.6884(9) 0.4997(5) 0.3924(5) 0.0416(19) Uani 1 1 d . . . C12 C 0.8167(10) 0.4971(6) 0.4018(7) 0.062(3) Uani 1 1 d . . . H12 H 0.8362 0.4493 0.3939 0.074 Uiso 1 1 calc R . . C13 C 0.9148(11) 0.5632(7) 0.4225(8) 0.075(4) Uani 1 1 d . . . H13 H 1.0002 0.5594 0.4306 0.090 Uiso 1 1 calc R . . C14 C 0.8905(10) 0.6364(6) 0.4319(7) 0.061(3) Uani 1 1 d . . . H14 H 0.9586 0.6812 0.4438 0.073 Uiso 1 1 calc R . . C15 C 0.7633(9) 0.6414(5) 0.4233(5) 0.0424(19) Uani 1 1 d . . . C16 C 0.6642(9) 0.5734(5) 0.4021(5) 0.0437(19) Uani 1 1 d . . . H16 H 0.5787 0.5769 0.3941 0.052 Uiso 1 1 calc R . . C17 C 0.7308(9) 0.7179(5) 0.4329(5) 0.0430(19) Uani 1 1 d . . . C18 C 0.8144(9) 0.7789(5) 0.4857(5) 0.048(2) Uani 1 1 d . . . H18 H 0.8956 0.7738 0.5088 0.057 Uiso 1 1 calc R . . C19 C 0.7775(9) 0.8449(5) 0.5033(5) 0.046(2) Uani 1 1 d . . . C20 C 0.9175(9) 0.2110(5) 0.2737(6) 0.051(2) Uani 1 1 d . . . C21 C 0.8332(8) 0.2492(5) 0.2204(5) 0.0398(18) Uani 1 1 d . . . C22 C 0.8567(9) 0.3287(5) 0.2298(5) 0.0436(19) Uani 1 1 d . . . H22 H 0.9194 0.3573 0.2697 0.052 Uiso 1 1 calc R . . C23 C 0.7873(8) 0.3687(5) 0.1798(5) 0.0361(17) Uani 1 1 d . . . C24 C 0.8098(8) 0.4552(5) 0.1940(5) 0.0375(17) Uani 1 1 d . . . C25 C 0.9239(8) 0.5044(5) 0.2328(6) 0.050(2) Uani 1 1 d . . . H25 H 0.9942 0.4845 0.2509 0.060 Uiso 1 1 calc R . . C26 C 0.9348(10) 0.5834(5) 0.2451(7) 0.063(3) Uani 1 1 d . . . H26 H 1.0125 0.6162 0.2720 0.075 Uiso 1 1 calc R . . C27 C 0.8327(9) 0.6146(5) 0.2182(6) 0.051(2) Uani 1 1 d . . . H27 H 0.8415 0.6680 0.2270 0.061 Uiso 1 1 calc R . . C28 C 0.7159(8) 0.5655(5) 0.1778(5) 0.0388(18) Uani 1 1 d . . . C29 C 0.7061(8) 0.4862(5) 0.1659(5) 0.0372(17) Uani 1 1 d . . . H29 H 0.6290 0.4530 0.1388 0.045 Uiso 1 1 calc R . . C30 C 0.6051(9) 0.5982(5) 0.1478(5) 0.0414(19) Uani 1 1 d . . . C31 C 0.5368(10) 0.5739(5) 0.0783(5) 0.050(2) Uani 1 1 d . . . H31 H 0.5578 0.5351 0.0508 0.060 Uiso 1 1 calc R . . C32 C 0.4352(10) 0.6056(6) 0.0466(5) 0.049(2) Uani 1 1 d . . . H32 H 0.3923 0.5903 -0.0020 0.059 Uiso 1 1 calc R . . C33 C 0.4004(9) 0.6599(5) 0.0890(5) 0.045(2) Uani 1 1 d . . . H33 H 0.3319 0.6806 0.0692 0.054 Uiso 1 1 calc R . . C34 C 0.4660(8) 0.6838(4) 0.1601(4) 0.0357(17) Uani 1 1 d . . . C35 C 0.5707(8) 0.6537(4) 0.1895(4) 0.0362(17) Uani 1 1 d . . . H35 H 0.6173 0.6712 0.2372 0.043 Uiso 1 1 calc R . . C36 C 0.4307(9) 0.7402(5) 0.2091(5) 0.0394(18) Uani 1 1 d . . . C37 C 0.3060(9) 0.7533(5) 0.1943(5) 0.045(2) Uani 1 1 d . . . H37 H 0.2477 0.7288 0.1512 0.054 Uiso 1 1 calc R . . C38 C 0.2670(9) 0.8005(5) 0.2407(5) 0.047(2) Uani 1 1 d . . . C39 C 0.1301(11) 0.8133(8) 0.2195(7) 0.069(3) Uani 1 1 d . . . C40 C 0.2694(9) 0.1510(6) -0.1186(6) 0.053(2) Uani 1 1 d . . . C41 C 0.3397(8) 0.2017(5) -0.0470(5) 0.0420(19) Uani 1 1 d . . . C42 C 0.2803(9) 0.2554(5) -0.0216(5) 0.050(2) Uani 1 1 d . . . H42 H 0.2019 0.2597 -0.0496 0.060 Uiso 1 1 calc R . . C43 C 0.3352(9) 0.3047(5) 0.0460(5) 0.0417(19) Uani 1 1 d . . . C44 C 0.2724(8) 0.3654(5) 0.0678(5) 0.0428(19) Uani 1 1 d . . . C45 C 0.2001(9) 0.4011(6) 0.0176(5) 0.050(2) Uani 1 1 d . . . H45 H 0.1850 0.3843 -0.0319 0.060 Uiso 1 1 calc R . . C46 C 0.1507(11) 0.4609(6) 0.0401(6) 0.058(3) Uani 1 1 d . . . H46 H 0.1058 0.4858 0.0060 0.070 Uiso 1 1 calc R . . C47 C 0.1684(10) 0.4838(6) 0.1140(6) 0.053(2) Uani 1 1 d . . . H47 H 0.1357 0.5246 0.1294 0.064 Uiso 1 1 calc R . . C48 C 0.2331(8) 0.4472(5) 0.1647(5) 0.0417(19) Uani 1 1 d . . . C49 C 0.2873(8) 0.3891(5) 0.1413(5) 0.044(2) Uani 1 1 d . . . H49 H 0.3346 0.3656 0.1757 0.053 Uiso 1 1 calc R . . C50 C 0.2398(8) 0.4663(5) 0.2445(5) 0.0418(19) Uani 1 1 d . . . C51 C 0.2056(9) 0.4073(5) 0.2870(6) 0.048(2) Uani 1 1 d . . . H51 H 0.1850 0.3554 0.2666 0.058 Uiso 1 1 calc R . . C52 C 0.2020(10) 0.4243(5) 0.3570(6) 0.052(2) Uani 1 1 d . . . H52 H 0.1804 0.3839 0.3845 0.063 Uiso 1 1 calc R . . C53 C 0.2296(9) 0.5004(5) 0.3886(5) 0.045(2) Uani 1 1 d . . . H53 H 0.2232 0.5111 0.4365 0.055 Uiso 1 1 calc R . . C54 C 0.2669(7) 0.5611(5) 0.3492(5) 0.0389(18) Uani 1 1 d . . . C55 C 0.2701(8) 0.5437(5) 0.2769(5) 0.0404(18) Uani 1 1 d . . . H55 H 0.2926 0.5841 0.2496 0.049 Uiso 1 1 calc R . . C56 C 0.3063(8) 0.6449(5) 0.3817(5) 0.0392(18) Uani 1 1 d . . . C57 C 0.2724(9) 0.6674(5) 0.4468(6) 0.049(2) Uani 1 1 d . . . H57 H 0.2189 0.6305 0.4671 0.058 Uiso 1 1 calc R . . C58 C 0.3172(8) 0.7431(5) 0.4808(5) 0.0424(19) Uani 1 1 d . . . C59 C 0.2601(11) 0.7648(6) 0.5456(6) 0.060(3) Uani 1 1 d . . . C60 C 0.8631(11) 0.2511(8) 0.0375(7) 0.073(3) Uani 1 1 d . . . H60A H 0.9038 0.2233 0.0730 0.110 Uiso 1 1 calc R . . H60B H 0.8767 0.3043 0.0582 0.110 Uiso 1 1 calc R . . H60C H 0.9001 0.2501 -0.0045 0.110 Uiso 1 1 calc R . . C61 C 0.6994(13) 0.1383(6) -0.0246(6) 0.067(3) Uani 1 1 d . . . H61A H 0.7681 0.1363 -0.0498 0.081 Uiso 1 1 calc R . . H61B H 0.6184 0.1283 -0.0608 0.081 Uiso 1 1 calc R . . C62 C 0.6908(13) 0.0775(7) 0.0253(7) 0.072(3) Uani 1 1 d . . . H62A H 0.6687 0.0262 -0.0025 0.086 Uiso 1 1 calc R . . H62B H 0.7738 0.0848 0.0592 0.086 Uiso 1 1 calc R . . C63 C 0.5867(14) 0.0305(6) 0.1167(8) 0.081(4) Uani 1 1 d . . . H63A H 0.5624 -0.0220 0.0924 0.121 Uiso 1 1 calc R . . H63B H 0.5233 0.0376 0.1435 0.121 Uiso 1 1 calc R . . H63C H 0.6700 0.0398 0.1497 0.121 Uiso 1 1 calc R . . C64 C 0.7787(14) 0.9026(9) 0.3273(8) 0.097(5) Uani 1 1 d . . . H64A H 0.8093 0.9366 0.2939 0.145 Uiso 1 1 calc R . . H64B H 0.7661 0.8493 0.3074 0.145 Uiso 1 1 calc R . . H64C H 0.8415 0.9139 0.3730 0.145 Uiso 1 1 calc R . . C65 C 0.6762(18) 0.9948(7) 0.3696(9) 0.098(5) Uani 1 1 d . . . H65A H 0.7199 1.0313 0.3415 0.118 Uiso 1 1 calc R . . H65B H 0.7268 1.0044 0.4195 0.118 Uiso 1 1 calc R . . C66 C 0.543(2) 1.0035(7) 0.3671(10) 0.121(7) Uani 1 1 d . . . H66A H 0.5464 1.0559 0.3876 0.146 Uiso 1 1 calc R . . H66B H 0.4931 0.9943 0.3171 0.146 Uiso 1 1 calc R . . C67 C 0.3655(14) 0.9629(8) 0.4206(8) 0.097(5) Uani 1 1 d . . . H67A H 0.3826 1.0160 0.4424 0.146 Uiso 1 1 calc R . . H67B H 0.3308 0.9283 0.4524 0.146 Uiso 1 1 calc R . . H67C H 0.3040 0.9550 0.3747 0.146 Uiso 1 1 calc R . . C68 C 0.8724(11) 0.9059(6) 0.5643(6) 0.061(3) Uani 1 1 d . . . F1 F 0.1323(18) 0.0568(10) 0.1938(11) 0.087(5) Uani 0.56(3) 1 d PU . . F1' F 0.098(2) 0.0827(16) 0.1630(16) 0.094(7) Uani 0.44(3) 1 d PU . . F2 F 0.1750(16) 0.0153(10) 0.0961(11) 0.085(6) Uani 0.56(3) 1 d PU . . F2' F 0.220(3) 0.0016(13) 0.1358(18) 0.107(8) Uani 0.44(3) 1 d PU . . F3' F 0.141(3) 0.071(2) 0.0635(15) 0.154(10) Uani 0.56(3) 1 d PU . . F3 F 0.095(2) 0.1134(16) 0.0867(16) 0.117(9) Uani 0.44(3) 1 d PU . . F4 F 0.9874(7) 0.8960(5) 0.5818(5) 0.102(3) Uani 1 1 d U . . F5 F 0.8222(9) 0.9047(5) 0.6242(4) 0.108(3) Uani 1 1 d U . . F6 F 0.8835(7) 0.9774(4) 0.5487(4) 0.088(2) Uani 1 1 d . . . F7 F 1.0016(9) 0.1884(6) 0.2444(5) 0.119(3) Uani 1 1 d U . . F8 F 0.8502(9) 0.1509(5) 0.2949(6) 0.133(4) Uani 1 1 d . . . F9 F 0.9857(8) 0.2569(4) 0.3336(4) 0.089(2) Uani 1 1 d . . . F10 F 0.0596(8) 0.7724(7) 0.1569(5) 0.120(3) Uani 1 1 d U . . F11 F 0.1322(9) 0.8847(6) 0.2217(7) 0.133(4) Uani 1 1 d U . . F12 F 0.0612(8) 0.7885(6) 0.2657(5) 0.108(3) Uani 1 1 d U . . F13 F 0.2023(8) 0.0837(4) -0.1071(4) 0.095(3) Uani 1 1 d . . . F14 F 0.3536(6) 0.1350(4) -0.1556(3) 0.0665(17) Uani 1 1 d . . . F15 F 0.1933(8) 0.1845(5) -0.1616(4) 0.096(3) Uani 1 1 d . . . F16 F 0.1925(9) 0.7036(4) 0.5686(5) 0.101(3) Uani 1 1 d . . . F17 F 0.1850(8) 0.8100(5) 0.5280(4) 0.090(2) Uani 1 1 d . . . F18 F 0.3531(7) 0.8022(4) 0.6021(3) 0.079(2) 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 O1 0.068(5) 0.036(3) 0.060(4) -0.017(3) 0.015(4) -0.004(3) O2 0.041(3) 0.043(3) 0.044(3) -0.002(3) 0.007(3) 0.009(3) O3 0.056(4) 0.034(3) 0.053(4) -0.003(3) -0.005(3) 0.018(3) O4 0.045(3) 0.034(3) 0.058(4) -0.007(3) 0.001(3) 0.010(3) O5 0.044(3) 0.035(3) 0.046(3) 0.004(3) 0.001(3) 0.013(3) O6 0.047(3) 0.029(3) 0.043(3) -0.002(2) 0.004(3) 0.014(2) O7 0.037(3) 0.037(3) 0.044(3) -0.006(2) 0.004(3) 0.011(2) O8 0.044(3) 0.047(4) 0.064(4) -0.013(3) 0.001(3) 0.023(3) O9 0.055(4) 0.043(3) 0.047(4) -0.007(3) 0.009(3) 0.024(3) O10 0.044(3) 0.048(4) 0.048(3) -0.008(3) -0.003(3) 0.021(3) O11 0.061(4) 0.030(3) 0.050(4) -0.008(3) 0.012(3) -0.001(3) O12 0.048(3) 0.035(3) 0.051(4) -0.012(3) 0.013(3) 0.006(3) O13 0.056(4) 0.058(4) 0.044(3) 0.000(3) 0.009(3) 0.026(3) O14 0.069(4) 0.038(3) 0.064(4) -0.002(3) 0.007(4) 0.026(3) O15 0.082(6) 0.057(5) 0.060(5) 0.004(4) 0.008(4) -0.012(4) O16 0.095(6) 0.033(3) 0.073(5) -0.007(3) -0.004(4) 0.022(4) Yb1 0.0430(2) 0.02689(17) 0.0411(2) -0.00533(14) 0.00480(16) 0.00804(14) Yb2 0.0412(2) 0.02965(18) 0.0387(2) -0.00294(14) 0.00416(15) 0.01336(14) C1 0.125(15) 0.090(12) 0.136(16) -0.045(11) 0.088(14) -0.026(11) C2 0.059(6) 0.041(5) 0.076(7) -0.011(5) 0.032(6) -0.004(4) C3 0.060(6) 0.051(6) 0.082(8) -0.016(5) 0.041(6) -0.004(5) C4 0.042(5) 0.036(4) 0.050(5) 0.001(4) 0.013(4) 0.010(4) C5 0.058(5) 0.038(4) 0.044(5) -0.001(4) 0.013(4) 0.020(4) C6 0.049(5) 0.049(5) 0.061(6) 0.006(5) 0.020(5) 0.005(4) C7 0.060(6) 0.068(7) 0.046(5) -0.001(5) 0.024(5) 0.009(5) C8 0.083(7) 0.047(5) 0.041(5) -0.005(4) 0.019(5) 0.024(5) C9 0.046(5) 0.039(4) 0.043(5) 0.002(4) 0.003(4) 0.018(4) C10 0.048(5) 0.034(4) 0.044(5) 0.004(3) 0.017(4) 0.009(4) C11 0.048(5) 0.032(4) 0.045(5) 0.004(3) 0.009(4) 0.015(4) C12 0.050(6) 0.043(5) 0.096(8) 0.000(5) 0.020(6) 0.019(4) C13 0.048(6) 0.054(6) 0.116(11) -0.008(6) 0.005(6) 0.020(5) C14 0.045(5) 0.046(5) 0.087(8) -0.005(5) 0.006(5) 0.013(4) C15 0.049(5) 0.036(4) 0.039(4) -0.005(3) 0.003(4) 0.012(4) C16 0.048(5) 0.040(5) 0.049(5) 0.001(4) 0.015(4) 0.020(4) C17 0.050(5) 0.036(4) 0.043(5) 0.002(4) 0.011(4) 0.011(4) C18 0.045(5) 0.039(5) 0.056(5) 0.004(4) 0.004(4) 0.012(4) C19 0.051(5) 0.034(4) 0.044(5) -0.001(4) 0.004(4) 0.003(4) C20 0.048(5) 0.042(5) 0.058(6) 0.010(4) -0.004(5) 0.014(4) C21 0.037(4) 0.040(4) 0.047(5) 0.010(4) 0.011(4) 0.016(4) C22 0.041(4) 0.037(4) 0.049(5) 0.002(4) 0.003(4) 0.012(4) C23 0.035(4) 0.033(4) 0.045(4) 0.005(3) 0.014(4) 0.012(3) C24 0.034(4) 0.031(4) 0.046(5) -0.001(3) 0.005(4) 0.011(3) C25 0.034(4) 0.037(5) 0.075(7) 0.006(4) 0.001(4) 0.013(4) C26 0.043(5) 0.031(5) 0.101(9) -0.005(5) -0.002(5) 0.006(4) C27 0.045(5) 0.032(4) 0.068(6) -0.005(4) -0.001(4) 0.010(4) C28 0.045(5) 0.035(4) 0.041(4) 0.002(3) 0.012(4) 0.019(4) C29 0.034(4) 0.034(4) 0.043(4) 0.002(3) 0.007(3) 0.010(3) C30 0.045(5) 0.032(4) 0.043(5) 0.000(3) -0.004(4) 0.016(3) C31 0.062(6) 0.036(5) 0.048(5) -0.004(4) -0.003(4) 0.020(4) C32 0.065(6) 0.053(5) 0.026(4) -0.006(4) -0.004(4) 0.025(5) C33 0.048(5) 0.041(5) 0.045(5) 0.003(4) 0.000(4) 0.021(4) C34 0.045(4) 0.028(4) 0.034(4) 0.002(3) 0.007(3) 0.012(3) C35 0.038(4) 0.032(4) 0.037(4) -0.003(3) 0.003(3) 0.011(3) C36 0.050(5) 0.029(4) 0.041(4) 0.000(3) 0.007(4) 0.019(4) C37 0.042(5) 0.046(5) 0.042(5) -0.006(4) -0.004(4) 0.014(4) C38 0.040(4) 0.044(5) 0.052(5) -0.006(4) -0.003(4) 0.019(4) C39 0.055(6) 0.078(8) 0.079(8) -0.007(6) 0.004(6) 0.042(6) C40 0.047(5) 0.044(5) 0.057(6) -0.011(4) -0.008(4) 0.015(4) C41 0.037(4) 0.038(4) 0.043(5) -0.007(4) -0.001(4) 0.007(3) C42 0.049(5) 0.047(5) 0.054(5) -0.006(4) 0.003(4) 0.021(4) C43 0.044(5) 0.040(4) 0.042(5) -0.001(4) 0.007(4) 0.017(4) C44 0.040(4) 0.040(4) 0.046(5) -0.002(4) 0.007(4) 0.011(4) C45 0.046(5) 0.057(6) 0.047(5) -0.002(4) 0.003(4) 0.023(4) C46 0.063(6) 0.064(6) 0.053(6) 0.005(5) 0.004(5) 0.035(5) C47 0.057(6) 0.050(5) 0.064(6) 0.001(5) 0.020(5) 0.031(5) C48 0.036(4) 0.035(4) 0.052(5) -0.007(4) 0.007(4) 0.010(3) C49 0.033(4) 0.039(4) 0.052(5) -0.010(4) -0.010(4) 0.014(3) C50 0.028(4) 0.034(4) 0.062(6) -0.002(4) 0.006(4) 0.010(3) C51 0.041(5) 0.034(4) 0.063(6) -0.010(4) 0.006(4) 0.008(4) C52 0.059(6) 0.033(4) 0.066(6) 0.008(4) 0.019(5) 0.008(4) C53 0.042(5) 0.044(5) 0.044(5) -0.005(4) 0.004(4) 0.008(4) C54 0.026(4) 0.032(4) 0.054(5) -0.006(3) 0.002(3) 0.007(3) C55 0.036(4) 0.034(4) 0.048(5) -0.004(4) 0.006(4) 0.009(3) C56 0.030(4) 0.036(4) 0.045(5) -0.005(4) -0.003(3) 0.009(3) C57 0.038(4) 0.039(5) 0.067(6) -0.006(4) 0.021(4) 0.002(4) C58 0.037(4) 0.039(4) 0.048(5) -0.006(4) 0.004(4) 0.011(4) C59 0.067(7) 0.048(6) 0.072(7) -0.001(5) 0.034(6) 0.018(5) C60 0.057(7) 0.084(8) 0.085(9) 0.006(7) 0.030(6) 0.020(6) C61 0.085(8) 0.059(7) 0.064(7) -0.010(5) 0.023(6) 0.032(6) C62 0.086(8) 0.055(6) 0.076(8) -0.013(6) 0.011(7) 0.035(6) C63 0.095(9) 0.037(6) 0.106(10) 0.017(6) 0.014(8) 0.015(6) C64 0.083(10) 0.114(12) 0.066(8) -0.009(8) 0.016(7) -0.020(9) C65 0.130(14) 0.042(6) 0.099(11) 0.009(7) 0.025(10) -0.022(8) C66 0.19(2) 0.030(6) 0.136(15) 0.021(7) 0.020(14) 0.026(9) C67 0.107(11) 0.078(9) 0.104(11) -0.034(8) -0.008(9) 0.062(8) C68 0.058(6) 0.051(6) 0.063(7) -0.009(5) -0.006(5) 0.014(5) F1 0.080(8) 0.076(8) 0.094(9) 0.002(6) 0.034(7) -0.012(6) F1' 0.076(9) 0.099(11) 0.101(11) -0.006(8) 0.034(8) 0.005(7) F2 0.084(8) 0.065(8) 0.086(9) -0.021(6) 0.007(7) -0.001(6) F2' 0.110(11) 0.082(10) 0.121(12) 0.014(8) 0.031(9) 0.005(8) F3' 0.133(12) 0.161(13) 0.148(13) 0.000(9) 0.027(9) 0.009(9) F3 0.090(11) 0.111(12) 0.132(12) 0.008(9) -0.004(8) 0.020(8) F4 0.071(4) 0.089(5) 0.124(6) -0.026(4) -0.023(4) 0.025(4) F5 0.123(6) 0.111(6) 0.068(4) -0.025(4) 0.020(4) -0.002(5) F6 0.086(5) 0.041(3) 0.106(6) -0.008(3) -0.018(4) -0.003(3) F7 0.120(6) 0.153(7) 0.113(6) 0.019(5) 0.011(5) 0.105(6) F8 0.105(6) 0.085(5) 0.156(8) 0.082(6) -0.054(6) -0.029(5) F9 0.097(5) 0.070(4) 0.074(5) 0.016(4) -0.030(4) 0.015(4) F10 0.076(5) 0.178(7) 0.101(5) -0.030(5) -0.017(4) 0.070(5) F11 0.101(6) 0.113(6) 0.199(8) 0.031(6) 0.009(5) 0.071(5) F12 0.066(4) 0.144(7) 0.118(6) 0.009(5) 0.029(4) 0.028(4) F13 0.093(5) 0.067(4) 0.099(6) -0.029(4) 0.026(5) -0.021(4) F14 0.080(4) 0.082(4) 0.038(3) -0.012(3) 0.005(3) 0.036(4) F15 0.107(6) 0.105(6) 0.063(4) -0.034(4) -0.038(4) 0.067(5) F16 0.137(7) 0.061(4) 0.109(6) -0.014(4) 0.088(6) -0.009(4) F17 0.097(5) 0.116(6) 0.086(5) 0.007(4) 0.037(4) 0.070(5) F18 0.097(5) 0.084(5) 0.042(3) -0.021(3) 0.005(3) 0.014(4) _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 O1 C2 1.272(12) . ? O1 Yb2 2.248(7) . ? O2 C4 1.271(10) . ? O2 Yb2 2.274(6) . ? O3 C17 1.258(11) . ? O3 Yb1 2.310(6) . ? O4 C19 1.262(11) . ? O4 Yb1 2.301(6) . ? O5 C21 1.259(10) . ? O5 Yb2 2.275(6) . ? O6 C23 1.259(10) . ? O6 Yb2 2.245(6) . ? O7 C36 1.262(10) . ? O7 Yb1 2.235(6) . ? O8 C38 1.256(11) . ? O8 Yb1 2.272(6) . ? O9 C41 1.258(10) . ? O9 Yb2 2.258(6) . ? O10 C43 1.250(10) . ? O10 Yb2 2.294(6) . ? O11 C56 1.222(10) . ? O11 Yb1 2.304(6) . ? O12 C58 1.258(11) . ? O12 Yb1 2.233(6) . ? O13 C60 1.442(13) . ? O13 C61 1.444(12) . ? O13 Yb2 2.529(7) . ? O14 C63 1.417(13) . ? O14 C62 1.429(14) . ? O14 Yb2 2.454(6) . ? O15 C64 1.400(17) . ? O15 C65 1.463(16) . ? O15 Yb1 2.411(8) . ? O16 C67 1.438(15) . ? O16 C66 1.438(18) . ? O16 Yb1 2.439(7) . ? C1 F2 1.19(2) . ? C1 F1' 1.21(2) . ? C1 F3' 1.24(3) . ? C1 F1 1.43(3) . ? C1 F3 1.44(3) . ? C1 F2' 1.47(3) . ? C1 C2 1.562(19) . ? C2 C3 1.350(14) . ? C3 C4 1.410(13) . ? C3 H3 0.9300 . ? C4 C5 1.478(12) . ? C5 C6 1.385(13) . ? C5 C10 1.392(12) . ? C6 C7 1.358(14) . ? C6 H6 0.9300 . ? C7 C8 1.388(14) . ? C7 H7 0.9300 . ? C8 C9 1.367(13) . ? C8 H8 0.9300 . ? C9 C10 1.379(12) . ? C9 C11 1.480(12) . ? C10 H10 0.9300 . ? C11 C12 1.384(13) . ? C11 C16 1.400(11) . ? C12 C13 1.360(15) . ? C12 H12 0.9300 . ? C13 C14 1.391(14) . ? C13 H13 0.9300 . ? C14 C15 1.386(13) . ? C14 H14 0.9300 . ? C15 C16 1.388(12) . ? C15 C17 1.489(12) . ? C16 H16 0.9300 . ? C17 C18 1.416(12) . ? C18 C19 1.364(13) . ? C18 H18 0.9300 . ? C19 C68 1.542(13) . ? C20 F7 1.285(13) . ? C20 F8 1.286(12) . ? C20 F9 1.317(12) . ? C20 C21 1.527(12) . ? C21 C22 1.365(12) . ? C22 C23 1.424(12) . ? C22 H22 0.9300 . ? C23 C24 1.493(11) . ? C24 C25 1.369(12) . ? C24 C29 1.396(11) . ? C25 C26 1.377(12) . ? C25 H25 0.9300 . ? C26 C27 1.379(13) . ? C26 H26 0.9300 . ? C27 C28 1.396(12) . ? C27 H27 0.9300 . ? C28 C29 1.383(11) . ? C28 C30 1.488(11) . ? C29 H29 0.9300 . ? C30 C31 1.353(12) . ? C30 C35 1.381(11) . ? C31 C32 1.404(13) . ? C31 H31 0.9300 . ? C32 C33 1.375(12) . ? C32 H32 0.9300 . ? C33 C34 1.371(12) . ? C33 H33 0.9300 . ? C34 C35 1.402(11) . ? C34 C36 1.479(11) . ? C35 H35 0.9300 . ? C36 C37 1.408(12) . ? C37 C38 1.363(12) . ? C37 H37 0.9300 . ? C38 C39 1.536(13) . ? C39 F11 1.261(14) . ? C39 F12 1.298(15) . ? C39 F10 1.327(14) . ? C40 F13 1.306(12) . ? C40 F15 1.314(11) . ? C40 F14 1.328(12) . ? C40 C41 1.517(12) . ? C41 C42 1.380(12) . ? C42 C43 1.426(12) . ? C42 H42 0.9300 . ? C43 C44 1.479(11) . ? C44 C49 1.387(12) . ? C44 C45 1.394(13) . ? C45 C46 1.374(13) . ? C45 H45 0.9300 . ? C46 C47 1.386(14) . ? C46 H46 0.9300 . ? C47 C48 1.366(13) . ? C47 H47 0.9300 . ? C48 C49 1.389(11) . ? C48 C50 1.504(13) . ? C49 H49 0.9300 . ? C50 C51 1.396(13) . ? C50 C55 1.398(11) . ? C51 C52 1.345(14) . ? C51 H51 0.9300 . ? C52 C53 1.375(12) . ? C52 H52 0.9300 . ? C53 C54 1.386(13) . ? C53 H53 0.9300 . ? C54 C55 1.387(12) . ? C54 C56 1.495(11) . ? C55 H55 0.9300 . ? C56 C57 1.409(12) . ? C57 C58 1.376(12) . ? C57 H57 0.9300 . ? C58 C59 1.545(13) . ? C59 F17 1.288(13) . ? C59 F16 1.319(12) . ? C59 F18 1.320(13) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C62 1.484(17) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.49(2) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 F4 1.285(13) . ? C68 F6 1.308(13) . ? C68 F5 1.353(14) . ? F1 F1' 0.85(3) . ? F1' F3 1.58(4) . ? F2 F2' 0.89(3) . ? F2 F3' 1.30(4) . ? F3' F3 1.10(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 C2 O1 Yb2 131.6(6) . . ? C4 O2 Yb2 135.0(6) . . ? C17 O3 Yb1 139.6(6) . . ? C19 O4 Yb1 133.8(6) . . ? C21 O5 Yb2 128.8(5) . . ? C23 O6 Yb2 132.4(5) . . ? C36 O7 Yb1 132.8(5) . . ? C38 O8 Yb1 129.2(5) . . ? C41 O9 Yb2 132.9(6) . . ? C43 O10 Yb2 137.5(6) . . ? C56 O11 Yb1 137.6(6) . . ? C58 O12 Yb1 133.3(5) . . ? C60 O13 C61 111.6(8) . . ? C60 O13 Yb2 124.9(6) . . ? C61 O13 Yb2 110.0(6) . . ? C63 O14 C62 111.6(9) . . ? C63 O14 Yb2 118.2(7) . . ? C62 O14 Yb2 117.6(6) . . ? C64 O15 C65 111.2(11) . . ? C64 O15 Yb1 122.3(8) . . ? C65 O15 Yb1 115.8(8) . . ? C67 O16 C66 109.8(12) . . ? C67 O16 Yb1 123.1(7) . . ? C66 O16 Yb1 113.6(9) . . ? O12 Yb1 O7 146.7(2) . . ? O12 Yb1 O8 88.9(2) . . ? O7 Yb1 O8 74.8(2) . . ? O12 Yb1 O4 81.2(2) . . ? O7 Yb1 O4 127.3(2) . . ? O8 Yb1 O4 147.0(2) . . ? O12 Yb1 O11 73.7(2) . . ? O7 Yb1 O11 74.5(2) . . ? O8 Yb1 O11 77.5(2) . . ? O4 Yb1 O11 128.3(2) . . ? O12 Yb1 O3 102.7(2) . . ? O7 Yb1 O3 75.4(2) . . ? O8 Yb1 O3 140.8(2) . . ? O4 Yb1 O3 72.2(2) . . ? O11 Yb1 O3 70.4(2) . . ? O12 Yb1 O15 140.1(3) . . ? O7 Yb1 O15 71.6(2) . . ? O8 Yb1 O15 96.3(3) . . ? O4 Yb1 O15 73.1(3) . . ? O11 Yb1 O15 146.0(3) . . ? O3 Yb1 O15 97.9(3) . . ? O12 Yb1 O16 77.4(3) . . ? O7 Yb1 O16 121.5(2) . . ? O8 Yb1 O16 70.1(2) . . ? O4 Yb1 O16 77.1(2) . . ? O11 Yb1 O16 136.4(3) . . ? O3 Yb1 O16 148.8(2) . . ? O15 Yb1 O16 67.6(3) . . ? O6 Yb2 O1 149.0(2) . . ? O6 Yb2 O9 114.6(2) . . ? O1 Yb2 O9 78.9(3) . . ? O6 Yb2 O2 78.3(2) . . ? O1 Yb2 O2 74.3(2) . . ? O9 Yb2 O2 139.0(2) . . ? O6 Yb2 O5 74.7(2) . . ? O1 Yb2 O5 111.1(3) . . ? O9 Yb2 O5 144.7(2) . . ? O2 Yb2 O5 75.0(2) . . ? O6 Yb2 O10 75.0(2) . . ? O1 Yb2 O10 83.0(3) . . ? O9 Yb2 O10 74.0(2) . . ? O2 Yb2 O10 72.5(2) . . ? O5 Yb2 O10 139.2(2) . . ? O6 Yb2 O14 134.2(2) . . ? O1 Yb2 O14 73.7(3) . . ? O9 Yb2 O14 79.9(2) . . ? O2 Yb2 O14 120.1(2) . . ? O5 Yb2 O14 71.5(2) . . ? O10 Yb2 O14 147.8(2) . . ? O6 Yb2 O13 75.1(2) . . ? O1 Yb2 O13 135.8(2) . . ? O9 Yb2 O13 74.8(2) . . ? O2 Yb2 O13 144.4(2) . . ? O5 Yb2 O13 75.4(2) . . ? O10 Yb2 O13 121.5(2) . . ? O14 Yb2 O13 67.3(2) . . ? F2 C1 F1' 122.4(18) . . ? F2 C1 F3' 64(2) . . ? F1' C1 F3' 112(3) . . ? F2 C1 F1 107.6(19) . . ? F1' C1 F1 36.5(14) . . ? F3' C1 F1 140(2) . . ? F2 C1 F3 108(2) . . ? F1' C1 F3 72(3) . . ? F3' C1 F3 48(2) . . ? F1 C1 F3 109(2) . . ? F2 C1 F2' 37.2(13) . . ? F1' C1 F2' 116(2) . . ? F3' C1 F2' 101(3) . . ? F1 C1 F2' 84.1(18) . . ? F3 C1 F2' 144(2) . . ? F2 C1 C2 117.4(17) . . ? F1' C1 C2 116.9(16) . . ? F3' C1 C2 110.1(17) . . ? F1 C1 C2 107.7(16) . . ? F3 C1 C2 107.6(16) . . ? F2' C1 C2 99.6(19) . . ? O1 C2 C3 127.8(9) . . ? O1 C2 C1 112.8(9) . . ? C3 C2 C1 119.3(10) . . ? C2 C3 C4 124.1(9) . . ? C2 C3 H3 117.9 . . ? C4 C3 H3 117.9 . . ? O2 C4 C3 121.2(8) . . ? O2 C4 C5 117.1(8) . . ? C3 C4 C5 121.6(8) . . ? C6 C5 C10 119.1(8) . . ? C6 C5 C4 121.5(9) . . ? C10 C5 C4 119.4(8) . . ? C7 C6 C5 120.3(9) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 119.5(9) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 121.8(9) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 118.1(9) . . ? C8 C9 C11 120.1(8) . . ? C10 C9 C11 121.7(8) . . ? C9 C10 C5 121.1(8) . . ? C9 C10 H10 119.4 . . ? C5 C10 H10 119.4 . . ? C12 C11 C16 117.1(8) . . ? C12 C11 C9 119.4(8) . . ? C16 C11 C9 123.3(8) . . ? C13 C12 C11 121.1(9) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 121.6(10) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C15 C14 C13 119.0(10) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 118.7(8) . . ? C14 C15 C17 121.6(8) . . ? C16 C15 C17 119.6(8) . . ? C15 C16 C11 122.4(8) . . ? C15 C16 H16 118.8 . . ? C11 C16 H16 118.8 . . ? O3 C17 C18 122.4(8) . . ? O3 C17 C15 117.6(8) . . ? C18 C17 C15 120.0(8) . . ? C19 C18 C17 120.9(9) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? O4 C19 C18 130.0(8) . . ? O4 C19 C68 113.1(8) . . ? C18 C19 C68 116.9(9) . . ? F7 C20 F8 107.4(10) . . ? F7 C20 F9 105.0(9) . . ? F8 C20 F9 105.9(9) . . ? F7 C20 C21 111.1(9) . . ? F8 C20 C21 112.2(8) . . ? F9 C20 C21 114.8(8) . . ? O5 C21 C22 129.4(8) . . ? O5 C21 C20 112.3(7) . . ? C22 C21 C20 118.3(8) . . ? C21 C22 C23 121.5(8) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? O6 C23 C22 123.1(7) . . ? O6 C23 C24 116.7(7) . . ? C22 C23 C24 120.1(7) . . ? C25 C24 C29 119.2(8) . . ? C25 C24 C23 124.0(7) . . ? C29 C24 C23 116.8(7) . . ? C24 C25 C26 120.1(8) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C27 121.2(9) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C28 119.6(8) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 118.6(8) . . ? C29 C28 C30 121.0(8) . . ? C27 C28 C30 120.3(7) . . ? C28 C29 C24 121.2(8) . . ? C28 C29 H29 119.4 . . ? C24 C29 H29 119.4 . . ? C31 C30 C35 119.1(8) . . ? C31 C30 C28 119.7(8) . . ? C35 C30 C28 121.2(7) . . ? C30 C31 C32 121.8(8) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C33 C32 C31 118.6(8) . . ? C33 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? C34 C33 C32 120.5(8) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.7(7) . . ? C33 C34 C36 123.0(8) . . ? C35 C34 C36 117.3(7) . . ? C30 C35 C34 120.2(7) . . ? C30 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? O7 C36 C37 122.1(7) . . ? O7 C36 C34 116.8(7) . . ? C37 C36 C34 121.1(8) . . ? C38 C37 C36 122.7(8) . . ? C38 C37 H37 118.6 . . ? C36 C37 H37 118.6 . . ? O8 C38 C37 128.9(8) . . ? O8 C38 C39 111.7(8) . . ? C37 C38 C39 119.3(9) . . ? F11 C39 F12 103.9(11) . . ? F11 C39 F10 112.1(12) . . ? F12 C39 F10 102.7(11) . . ? F11 C39 C38 112.1(11) . . ? F12 C39 C38 111.5(10) . . ? F10 C39 C38 113.7(9) . . ? F13 C40 F15 109.7(9) . . ? F13 C40 F14 105.9(8) . . ? F15 C40 F14 106.6(9) . . ? F13 C40 C41 110.7(9) . . ? F15 C40 C41 113.0(8) . . ? F14 C40 C41 110.6(8) . . ? O9 C41 C42 128.6(8) . . ? O9 C41 C40 114.3(8) . . ? C42 C41 C40 117.0(8) . . ? C41 C42 C43 122.1(8) . . ? C41 C42 H42 118.9 . . ? C43 C42 H42 118.9 . . ? O10 C43 C42 122.1(8) . . ? O10 C43 C44 118.1(8) . . ? C42 C43 C44 119.7(8) . . ? C49 C44 C45 117.9(8) . . ? C49 C44 C43 119.0(8) . . ? C45 C44 C43 123.0(8) . . ? C46 C45 C44 121.1(9) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C46 C47 119.5(9) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? C48 C47 C46 120.8(8) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C49 119.1(9) . . ? C47 C48 C50 120.6(8) . . ? C49 C48 C50 120.1(8) . . ? C44 C49 C48 121.4(8) . . ? C44 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? C51 C50 C55 117.9(9) . . ? C51 C50 C48 120.9(8) . . ? C55 C50 C48 121.0(8) . . ? C52 C51 C50 121.2(8) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C51 C52 C53 121.0(9) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? C52 C53 C54 120.1(9) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 119.0(8) . . ? C55 C54 C56 118.3(8) . . ? C53 C54 C56 122.7(8) . . ? C54 C55 C50 120.8(8) . . ? C54 C55 H55 119.6 . . ? C50 C55 H55 119.6 . . ? O11 C56 C57 122.2(8) . . ? O11 C56 C54 117.4(8) . . ? C57 C56 C54 120.3(8) . . ? C58 C57 C56 121.0(9) . . ? C58 C57 H57 119.5 . . ? C56 C57 H57 119.5 . . ? O12 C58 C57 130.0(9) . . ? O12 C58 C59 112.8(7) . . ? C57 C58 C59 117.2(8) . . ? F17 C59 F16 107.6(10) . . ? F17 C59 F18 107.6(9) . . ? F16 C59 F18 106.6(10) . . ? F17 C59 C58 110.5(9) . . ? F16 C59 C58 113.3(8) . . ? F18 C59 C58 110.9(9) . . ? 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 . . ? O13 C61 C62 110.2(9) . . ? O13 C61 H61A 109.6 . . ? C62 C61 H61A 109.6 . . ? O13 C61 H61B 109.6 . . ? C62 C61 H61B 109.6 . . ? H61A C61 H61B 108.1 . . ? O14 C62 C61 108.9(9) . . ? O14 C62 H62A 109.9 . . ? C61 C62 H62A 109.9 . . ? O14 C62 H62B 109.9 . . ? C61 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? O14 C63 H63A 109.5 . . ? O14 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? O14 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O15 C64 H64A 109.5 . . ? O15 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? O15 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O15 C65 C66 106.1(11) . . ? O15 C65 H65A 110.5 . . ? C66 C65 H65A 110.5 . . ? O15 C65 H65B 110.5 . . ? C66 C65 H65B 110.5 . . ? H65A C65 H65B 108.7 . . ? O16 C66 C65 107.4(12) . . ? O16 C66 H66A 110.2 . . ? C65 C66 H66A 110.2 . . ? O16 C66 H66B 110.2 . . ? C65 C66 H66B 110.2 . . ? H66A C66 H66B 108.5 . . ? O16 C67 H67A 109.5 . . ? O16 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? O16 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? F4 C68 F6 107.4(10) . . ? F4 C68 F5 108.7(10) . . ? F6 C68 F5 104.1(10) . . ? F4 C68 C19 114.9(9) . . ? F6 C68 C19 112.6(9) . . ? F5 C68 C19 108.4(9) . . ? F1' F1 C1 58(2) . . ? F1 F1' C1 86(3) . . ? F1 F1' F3 146(3) . . ? C1 F1' F3 61(2) . . ? F2' F2 C1 89(2) . . ? F2' F2 F3' 147(3) . . ? C1 F2 F3' 60(2) . . ? F2 F2' C1 53.7(19) . . ? F3 F3' C1 76(3) . . ? F3 F3' F2 125(3) . . ? C1 F3' F2 55.7(18) . . ? F3' F3 C1 57(2) . . ? F3' F3 F1' 97(3) . . ? C1 F3 F1' 47.2(13) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.065 _refine_diff_density_min -1.474 _refine_diff_density_rms 0.179