# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Koen Binnemans' 'S. Bellayer' 'Kris Driesen' 'Christiane G\"orller-Walrand' 'Jean Le Bideau' 'Kyra Lunstroot' 'Peter Nockemann' 'Kristof Van Hecke' 'Luc Van Meervelt' 'Lydie Viau' 'Andre Vioux' _publ_contact_author_name 'Prof Koen Binnemans ' _publ_contact_author_email KOEN.BINNEMANS@CHEM.KULEUVEN.BE _publ_section_title ; Lanthanide-Doped Luminescent Ionogels ; # Attachment 'wg150_Tbdpa.cif' data_wg150 _database_code_depnum_ccdc_archive 'CCDC 695447' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C5 H14 N O), C21 H9 N3 O12 Tb' _chemical_formula_sum 'C36 H51 N6 O15 Tb' _chemical_formula_weight 966.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -9.1472 9.1891 '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' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3 c' _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 10.4585(3) _cell_length_b 10.4585(3) _cell_length_c 69.627(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6595.5(4) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2964 _exptl_absorpt_coefficient_mu 8.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.124 _exptl_absorpt_correction_T_max 0.181 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18596 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -84 _diffrn_reflns_limit_l_max 84 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 70.88 _reflns_number_total 1414 _reflns_number_gt 1219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material Platon _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^)+(0.1315P)^2^+27.3311P] 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 1414 _refine_ls_number_parameters 180 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1832 _refine_ls_wR_factor_gt 0.1755 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.115 _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 Tb1 Tb 0.6667 0.3333 0.0833 0.03039(12) Uani 1 6 d S . . O1 O 0.6453(2) 0.1551(2) 0.05988(3) 0.0386(5) Uani 1 1 d . . . O2 O 0.5127(3) -0.0533(3) 0.04325(4) 0.0567(7) Uani 1 1 d . . . C1 C 0.5301(3) 0.0331(4) 0.05648(6) 0.0423(9) Uani 1 1 d . . . N1 N 0.6667 0.5721(3) 0.0833 0.0369(8) Uani 1 2 d S . . C2 C 0.4033(3) -0.0097(3) 0.07022(5) 0.0432(8) Uani 1 1 d . . . C3 C 0.2721(5) -0.1416(4) 0.06965(7) 0.0713(14) Uani 1 1 d . . . H3 H 0.2544 -0.2136 0.0601 0.086 Uiso 1 1 calc R . . C4 C 0.1675(5) -0.1659(5) 0.0833 0.092(4) Uani 1 2 d S . . H4 H 0.0766 -0.2567 0.0833 0.110 Uiso 1 2 calc SR . . N2 N 0.6667 0.3333 0.00304(8) 0.1662(15) Uani 1 3 d SDU . . O3 O 0.7206(16) 0.0637(7) 0.01601(17) 0.161(4) Uani 0.33 1 d PDU . . H3A H 0.6497 0.0353 0.0237 0.241 Uiso 0.33 1 calc PR . . C5 C 0.7864(5) 0.2907(7) 0.00069(12) 0.1785(16) Uani 0.33 1 d PDU . . H5A H 0.7596 0.2232 -0.0104 0.214 Uiso 0.33 1 calc PR . . H5B H 0.8803 0.3812 -0.0025 0.214 Uiso 0.33 1 calc PR . . C6 C 0.8140(12) 0.2175(8) 0.01776(16) 0.168(2) Uani 0.33 1 d PDU . . H6A H 0.9185 0.2422 0.0180 0.201 Uiso 0.33 1 calc PR . . H6B H 0.7927 0.2529 0.0299 0.201 Uiso 0.33 1 calc PR . . C7 C 0.5627(11) 0.2516(14) 0.01959(11) 0.166(3) Uani 0.33 1 d PDU . . H7A H 0.4914 0.1507 0.0156 0.249 Uiso 0.33 1 calc PR . . H7B H 0.5099 0.3031 0.0233 0.249 Uiso 0.33 1 calc PR . . H7C H 0.6197 0.2482 0.0305 0.249 Uiso 0.33 1 calc PR . . C8 C 0.7285(15) 0.4947(6) 0.00888(18) 0.181(3) Uani 0.33 1 d PDU . . H8A H 0.8126 0.5583 0.0006 0.272 Uiso 0.33 1 calc PR . . H8B H 0.7609 0.5078 0.0223 0.272 Uiso 0.33 1 calc PR . . H8C H 0.6515 0.5214 0.0074 0.272 Uiso 0.33 1 calc PR . . C9 C 0.5748(10) 0.3126(17) -0.01450(11) 0.173(4) Uani 0.33 1 d PDU . . H9A H 0.6205 0.4036 -0.0221 0.260 Uiso 0.33 1 calc PR . . H9B H 0.4754 0.2891 -0.0106 0.260 Uiso 0.33 1 calc PR . . H9C H 0.5686 0.2314 -0.0222 0.260 Uiso 0.33 1 calc PR . . N3 N 1.0438(7) -0.0239(9) 0.03295(13) 0.099(4) Uani 0.17 1 d PDU . . O4 O 0.7774(9) 0.0083(11) 0.02775(14) 0.050(3) Uani 0.17 1 d PDU . . H4A H 0.6998 0.0091 0.0306 0.074 Uiso 0.17 1 calc PR . . C10 C 0.9689(6) 0.0215(8) 0.04806(11) 0.097(4) Uani 0.17 1 d PDU . . H10A H 0.8966 -0.0681 0.0551 0.116 Uiso 0.17 1 calc PR . . H10B H 1.0446 0.0874 0.0574 0.116 Uiso 0.17 1 calc PR . . C11 C 0.8901(8) 0.0989(9) 0.04055(18) 0.090(5) Uani 0.17 1 d PDU . . H11A H 0.8473 0.1258 0.0514 0.107 Uiso 0.17 1 calc PR . . H11B H 0.9617 0.1910 0.0339 0.107 Uiso 0.17 1 calc PR . . C12 C 1.0000 0.0000 0.01236(13) 0.124(7) Uani 0.50 3 d SPDU . . H12A H 0.8974 -0.0754 0.0097 0.186 Uiso 0.17 1 calc PR . . H12B H 1.0651 -0.0078 0.0029 0.186 Uiso 0.17 1 calc PR . . H12C H 1.0101 0.0982 0.0116 0.186 Uiso 0.17 1 calc PR . . C13 C 1.0006(16) -0.1871(9) 0.0328(3) 0.112(9) Uani 0.17 1 d PDU . . H13A H 1.0052 -0.2188 0.0459 0.168 Uiso 0.17 1 calc PR . . H13B H 1.0690 -0.2005 0.0246 0.168 Uiso 0.17 1 calc PR . . H13C H 0.8998 -0.2465 0.0278 0.168 Uiso 0.17 1 calc PR . . C14 C 1.2117(9) 0.0620(18) 0.0326(3) 0.105(8) Uani 0.17 1 d PDU . . H14A H 1.2460 0.1616 0.0277 0.158 Uiso 0.17 1 calc PR . . H14B H 1.2479 0.0112 0.0243 0.158 Uiso 0.17 1 calc PR . . H14C H 1.2496 0.0684 0.0457 0.158 Uiso 0.17 1 calc PR . . 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 0.02960(15) 0.02960(15) 0.0320(2) 0.000 0.000 0.01480(8) O1 0.0414(8) 0.0331(8) 0.0395(10) -0.0047(7) -0.0028(8) 0.0174(7) O2 0.0699(11) 0.0405(11) 0.0493(14) -0.0108(10) -0.0041(12) 0.0198(10) C1 0.0513(14) 0.0374(13) 0.0394(17) 0.0034(13) -0.0059(11) 0.0231(10) N1 0.0403(18) 0.0331(12) 0.0398(17) 0.0047(7) 0.0095(14) 0.0202(9) C2 0.0418(13) 0.0326(12) 0.0484(16) -0.0022(12) -0.0059(13) 0.0134(10) C3 0.056(2) 0.0448(18) 0.086(3) -0.0140(19) 0.004(2) 0.0053(16) C4 0.055(3) 0.055(3) 0.123(8) -0.015(3) 0.015(3) -0.004(4) N2 0.2284(18) 0.2284(18) 0.042(3) 0.000 0.000 0.1142(9) O3 0.200(8) 0.220(3) 0.087(6) -0.004(4) 0.050(6) 0.124(5) C5 0.2288(18) 0.239(2) 0.066(4) 0.014(2) 0.024(2) 0.1155(16) C6 0.222(3) 0.221(3) 0.073(5) 0.017(3) 0.037(4) 0.119(3) C7 0.235(4) 0.238(5) 0.036(3) -0.008(4) 0.005(3) 0.127(5) C8 0.258(7) 0.236(2) 0.036(5) -0.022(4) 0.008(6) 0.113(3) C9 0.255(4) 0.208(8) 0.045(3) -0.001(4) -0.014(3) 0.108(4) N3 0.104(5) 0.074(5) 0.107(5) 0.008(5) -0.011(5) 0.035(5) O4 0.060(5) 0.043(5) 0.059(7) 0.004(5) 0.008(5) 0.035(4) C10 0.100(5) 0.071(5) 0.100(5) 0.004(5) -0.017(5) 0.028(5) C11 0.089(6) 0.069(6) 0.090(6) 0.001(6) -0.015(6) 0.025(6) C12 0.116(8) 0.116(8) 0.140(13) 0.000 0.000 0.058(4) C13 0.115(12) 0.071(11) 0.110(12) 0.017(11) -0.001(12) 0.017(11) C14 0.106(12) 0.086(10) 0.109(12) 0.020(11) -0.012(12) 0.037(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.403(2) 17_554 ? Tb1 O1 2.403(2) 16_544 ? Tb1 O1 2.403(2) 18_654 ? Tb1 O1 2.403(2) . ? Tb1 O1 2.403(2) 2_655 ? Tb1 O1 2.403(2) 3_665 ? Tb1 N1 2.497(3) 2_655 ? Tb1 N1 2.497(3) . ? Tb1 N1 2.497(3) 3_665 ? O1 C1 1.264(3) . ? O2 C1 1.239(5) . ? C1 C2 1.511(5) . ? N1 C2 1.344(4) 17_554 ? N1 C2 1.344(4) 3_665 ? C2 N1 1.344(4) 2_655 ? C2 C3 1.376(4) . ? C3 C4 1.375(5) . ? C3 H3 0.9500 . ? C4 C3 1.375(5) 16_544 ? C4 H4 0.9500 . ? N2 C9 1.501(7) 2_655 ? N2 C9 1.501(7) 3_665 ? N2 C9 1.501(7) . ? N2 C7 1.521(7) 2_655 ? N2 C7 1.521(7) . ? N2 C7 1.521(7) 3_665 ? N2 C8 1.530(6) 3_665 ? N2 C8 1.530(6) 2_655 ? N2 C8 1.530(6) . ? N2 C5 1.533(6) . ? N2 C5 1.533(6) 3_665 ? N2 C5 1.533(6) 2_655 ? O3 C6 1.409(8) . ? O3 H3A 0.8400 . ? C5 C6 1.517(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? N3 N3 1.076(15) 3_765 ? N3 N3 1.076(15) 2_645 ? N3 C10 1.180(10) 3_765 ? N3 C10 1.207(9) 2_645 ? N3 C10 1.522(8) . ? N3 C14 1.522(10) . ? N3 C13 1.532(11) . ? N3 C12 1.562(11) . ? N3 C11 1.674(12) 3_765 ? N3 C11 1.833(13) 2_645 ? N3 C13 1.956(16) 2_645 ? O4 C11 1.402(9) . ? O4 H4A 0.8400 . ? C10 C11 1.508(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O1 78.91(8) 17_554 16_544 ? O1 Tb1 O1 78.91(8) 17_554 18_654 ? O1 Tb1 O1 78.91(8) 16_544 18_654 ? O1 Tb1 O1 145.70(10) 17_554 . ? O1 Tb1 O1 128.51(9) 16_544 . ? O1 Tb1 O1 86.35(10) 18_654 . ? O1 Tb1 O1 86.35(10) 17_554 2_655 ? O1 Tb1 O1 145.70(10) 16_544 2_655 ? O1 Tb1 O1 128.51(9) 18_654 2_655 ? O1 Tb1 O1 78.89(8) . 2_655 ? O1 Tb1 O1 128.51(9) 17_554 3_665 ? O1 Tb1 O1 86.35(10) 16_544 3_665 ? O1 Tb1 O1 145.70(10) 18_654 3_665 ? O1 Tb1 O1 78.89(8) . 3_665 ? O1 Tb1 O1 78.89(8) 2_655 3_665 ? O1 Tb1 N1 136.83(5) 17_554 2_655 ? O1 Tb1 N1 64.25(4) 16_544 2_655 ? O1 Tb1 N1 72.85(5) 18_654 2_655 ? O1 Tb1 N1 64.26(4) . 2_655 ? O1 Tb1 N1 136.82(5) 2_655 2_655 ? O1 Tb1 N1 72.85(5) 3_665 2_655 ? O1 Tb1 N1 64.25(4) 17_554 . ? O1 Tb1 N1 72.85(5) 16_544 . ? O1 Tb1 N1 136.83(5) 18_654 . ? O1 Tb1 N1 136.82(5) . . ? O1 Tb1 N1 72.85(5) 2_655 . ? O1 Tb1 N1 64.26(4) 3_665 . ? N1 Tb1 N1 120.0 2_655 . ? O1 Tb1 N1 72.85(5) 17_554 3_665 ? O1 Tb1 N1 136.83(5) 16_544 3_665 ? O1 Tb1 N1 64.25(4) 18_654 3_665 ? O1 Tb1 N1 72.85(5) . 3_665 ? O1 Tb1 N1 64.26(4) 2_655 3_665 ? O1 Tb1 N1 136.82(5) 3_665 3_665 ? N1 Tb1 N1 120.0 2_655 3_665 ? N1 Tb1 N1 120.000(1) . 3_665 ? C1 O1 Tb1 125.6(2) . . ? O2 C1 O1 126.5(3) . . ? O2 C1 C2 117.9(3) . . ? O1 C1 C2 115.7(3) . . ? C2 N1 C2 119.8(4) 17_554 3_665 ? C2 N1 Tb1 120.08(18) 17_554 . ? C2 N1 Tb1 120.08(18) 3_665 . ? N1 C2 C3 121.6(4) 2_655 . ? N1 C2 C1 114.0(3) 2_655 . ? C3 C2 C1 124.5(3) . . ? C4 C3 C2 117.9(4) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C3 121.3(5) 16_544 . ? C3 C4 H4 119.3 16_544 . ? C3 C4 H4 119.3 . . ? C9 N2 C9 60.5(7) 2_655 3_665 ? C9 N2 C9 60.5(7) 2_655 . ? C9 N2 C9 60.5(7) 3_665 . ? C9 N2 C7 108.0(5) 2_655 2_655 ? C9 N2 C7 125.3(8) 3_665 2_655 ? C9 N2 C7 164.3(9) . 2_655 ? C9 N2 C7 125.3(8) 2_655 . ? C9 N2 C7 164.3(9) 3_665 . ? C9 N2 C7 108.0(5) . . ? C7 N2 C7 68.8(6) 2_655 . ? C9 N2 C7 164.3(9) 2_655 3_665 ? C9 N2 C7 108.0(5) 3_665 3_665 ? C9 N2 C7 125.3(8) . 3_665 ? C7 N2 C7 68.8(6) 2_655 3_665 ? C7 N2 C7 68.8(6) . 3_665 ? C9 N2 C8 73.1(6) 2_655 3_665 ? C9 N2 C8 105.2(8) 3_665 3_665 ? C9 N2 C8 132.6(9) . 3_665 ? C7 N2 C8 90.4(8) . 3_665 ? C7 N2 C8 102.0(7) 3_665 3_665 ? C9 N2 C8 105.2(8) 2_655 2_655 ? C9 N2 C8 132.6(9) 3_665 2_655 ? C9 N2 C8 73.1(6) . 2_655 ? C7 N2 C8 102.0(7) 2_655 2_655 ? C7 N2 C8 90.4(8) 3_665 2_655 ? C8 N2 C8 113.2(4) 3_665 2_655 ? C9 N2 C8 132.6(9) 2_655 . ? C9 N2 C8 73.1(6) 3_665 . ? C9 N2 C8 105.2(8) . . ? C7 N2 C8 90.4(8) 2_655 . ? C7 N2 C8 102.0(7) . . ? C8 N2 C8 113.2(4) 3_665 . ? C8 N2 C8 113.2(4) 2_655 . ? C9 N2 C5 55.1(5) 2_655 . ? C9 N2 C5 83.3(7) 3_665 . ? C9 N2 C5 115.3(7) . . ? C7 N2 C5 55.5(5) 2_655 . ? C7 N2 C5 112.1(7) . . ? C7 N2 C5 115.7(7) 3_665 . ? C8 N2 C5 127.9(6) 2_655 . ? C8 N2 C5 113.1(6) . . ? C9 N2 C5 83.3(7) 2_655 3_665 ? C9 N2 C5 115.3(7) 3_665 3_665 ? C9 N2 C5 55.1(5) . 3_665 ? C7 N2 C5 115.7(7) 2_655 3_665 ? C7 N2 C5 55.5(5) . 3_665 ? C7 N2 C5 112.1(7) 3_665 3_665 ? C8 N2 C5 113.1(6) 3_665 3_665 ? C8 N2 C5 127.9(6) . 3_665 ? C5 N2 C5 118.88(13) . 3_665 ? C9 N2 C5 115.3(7) 2_655 2_655 ? C9 N2 C5 55.1(5) 3_665 2_655 ? C9 N2 C5 83.3(7) . 2_655 ? C7 N2 C5 112.1(7) 2_655 2_655 ? C7 N2 C5 115.7(7) . 2_655 ? C7 N2 C5 55.5(5) 3_665 2_655 ? C8 N2 C5 127.9(6) 3_665 2_655 ? C8 N2 C5 113.1(6) 2_655 2_655 ? C5 N2 C5 118.88(13) . 2_655 ? C5 N2 C5 118.88(13) 3_665 2_655 ? C6 O3 H3A 109.5 . . ? C6 C5 N2 116.9(7) . . ? C6 C5 H5A 108.1 . . ? N2 C5 H5A 108.1 . . ? C6 C5 H5B 108.1 . . ? N2 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? O3 C6 C5 108.1(8) . . ? O3 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O3 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 N3 N3 60.000(1) 3_765 2_645 ? N3 N3 C10 84.7(6) 3_765 3_765 ? N3 N3 C10 64.5(6) 2_645 3_765 ? N3 N3 C10 61.9(5) 3_765 2_645 ? N3 N3 C10 83.4(5) 2_645 2_645 ? N3 N3 C10 52.0(4) 3_765 . ? N3 N3 C10 50.5(4) 2_645 . ? N3 N3 C14 158.9(11) 3_765 . ? N3 N3 C14 98.9(11) 2_645 . ? C10 N3 C14 86.6(9) 3_765 . ? C10 N3 C14 120.2(10) 2_645 . ? C10 N3 C14 116.7(9) . . ? N3 N3 C13 95.6(10) 3_765 . ? N3 N3 C13 155.6(10) 2_645 . ? C10 N3 C13 117.2(10) 3_765 . ? C10 N3 C13 85.1(9) 2_645 . ? C10 N3 C13 116.2(8) . . ? C14 N3 C13 105.5(10) . . ? N3 N3 C12 69.8(3) 3_765 . ? N3 N3 C12 69.8(3) 2_645 . ? C10 N3 C12 134.2(9) 3_765 . ? C10 N3 C12 131.7(7) 2_645 . ? C10 N3 C12 110.3(6) . . ? C14 N3 C12 103.6(8) . . ? C13 N3 C12 103.0(8) . . ? N3 N3 C11 136.5(8) 3_765 3_765 ? N3 N3 C11 80.4(9) 2_645 3_765 ? C10 N3 C11 60.9(5) 3_765 3_765 ? C10 N3 C11 98.7(8) 2_645 3_765 ? C10 N3 C11 89.8(6) . 3_765 ? C13 N3 C11 122.7(9) . 3_765 ? C12 N3 C11 114.7(6) . 3_765 ? N3 N3 C11 64.2(7) 3_765 2_645 ? N3 N3 C11 121.4(6) 2_645 2_645 ? C10 N3 C11 94.6(7) 3_765 2_645 ? C10 N3 C11 54.9(5) 2_645 2_645 ? C10 N3 C11 81.7(5) . 2_645 ? C14 N3 C11 135.9(10) . 2_645 ? C12 N3 C11 106.5(6) . 2_645 ? C11 N3 C11 138.2(9) 3_765 2_645 ? N3 N3 C13 111.2(8) 3_765 2_645 ? N3 N3 C13 51.2(8) 2_645 2_645 ? C10 N3 C13 68.0(7) 3_765 2_645 ? C10 N3 C13 107.7(8) 2_645 2_645 ? C10 N3 C13 82.7(6) . 2_645 ? C14 N3 C13 47.7(8) . 2_645 ? C13 N3 C13 153.2(6) . 2_645 ? C12 N3 C13 86.2(6) . 2_645 ? C11 N3 C13 162.6(8) 2_645 2_645 ? C11 O4 H4A 109.5 . . ? C11 C10 N3 115.6(8) . . ? C11 C10 H10A 108.4 . . ? N3 C10 H10A 108.4 . . ? C11 C10 H10B 108.4 . . ? N3 C10 H10B 108.4 . . ? H10A C10 H10B 107.4 . . ? O4 C11 C10 111.0(8) . . ? O4 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? O4 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 67.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.226 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.160 # Attachment 'wg172_Ybtta.cif' data_wg172 _database_code_depnum_ccdc_archive 'CCDC 695448' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H16 F12 O8 S4 Yb, C10 H19 N2, 0.04(C2 H8 O2)' _chemical_formula_sum 'C42.08 H35.32 F12 N2 O8.08 S4 Yb' _chemical_formula_weight 1227.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -7.2108 4.4329 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5623(4) _cell_length_b 19.6699(7) _cell_length_c 22.3920(9) _cell_angle_alpha 72.477(2) _cell_angle_beta 78.911(2) _cell_angle_gamma 81.305(2) _cell_volume 4741.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2433.7 _exptl_absorpt_coefficient_mu 6.197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.281 _exptl_absorpt_correction_T_max 0.538 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58800 _diffrn_reflns_av_R_equivalents 0.1058 _diffrn_reflns_av_sigmaI/netI 0.1005 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 71.78 _reflns_number_total 17984 _reflns_number_gt 13133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material Platon _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^)+(0.0440P)^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 17984 _refine_ls_number_parameters 1406 _refine_ls_number_restraints 461 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.973 _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 C1 C 0.1916(6) 0.8958(3) 0.4639(3) 0.0299(12) Uani 1 1 d . . . H1 H 0.2055 0.9256 0.4877 0.036 Uiso 1 1 calc R . . C2 C 0.0856(5) 0.8706(3) 0.4700(3) 0.0308(12) Uani 1 1 d . . . H2 H 0.0186 0.8813 0.4989 0.037 Uiso 1 1 calc R . . C3 C 0.0822(4) 0.8263(2) 0.4292(2) 0.0146(9) Uani 1 1 d . . . H3 H 0.0158 0.8046 0.4269 0.017 Uiso 1 1 calc R . . C4 C 0.2000(4) 0.8214(3) 0.3924(2) 0.0179(9) Uani 1 1 d . . . C5 C 0.2461(4) 0.7812(2) 0.3452(2) 0.0157(9) Uani 1 1 d . . . C6 C 0.1754(4) 0.7301(3) 0.3403(2) 0.0179(9) Uani 1 1 d . . . H6 H 0.1039 0.7212 0.3692 0.021 Uiso 1 1 calc R . . C7 C 0.2074(4) 0.6934(3) 0.2954(3) 0.0170(9) Uani 1 1 d . . . C8 C 0.1172(5) 0.6454(3) 0.2912(3) 0.0220(11) Uani 1 1 d . . . S2A S 0.2936(2) 0.52553(14) 0.42370(13) 0.0256(6) Uani 0.723(8) 1 d PDU A 1 C9A C 0.2595(8) 0.4706(5) 0.4979(3) 0.0252(19) Uani 0.723(8) 1 d PDU A 1 H9A H 0.2141 0.4312 0.5074 0.030 Uiso 0.723(8) 1 calc PR A 1 C10A C 0.3052(8) 0.4894(5) 0.5435(6) 0.0308(18) Uani 0.723(8) 1 d PDU A 1 H10A H 0.2964 0.4642 0.5873 0.037 Uiso 0.723(8) 1 calc PR A 1 C11A C 0.3666(14) 0.5515(8) 0.5154(5) 0.028(2) Uani 0.723(8) 1 d PDU A 1 H11A H 0.4021 0.5741 0.5383 0.034 Uiso 0.723(8) 1 calc PR A 1 C12A C 0.3682(6) 0.5750(3) 0.4499(4) 0.0214(13) Uani 0.723(8) 1 d PDU A 1 C11B C 0.314(2) 0.5261(13) 0.4319(15) 0.025(3) Uani 0.277(8) 1 d PDU A 2 H11B H 0.3080 0.5321 0.3888 0.030 Uiso 0.277(8) 1 calc PR A 2 C10B C 0.264(3) 0.4689(16) 0.4811(11) 0.025(3) Uani 0.277(8) 1 d PDU A 2 H10B H 0.2243 0.4329 0.4757 0.030 Uiso 0.277(8) 1 calc PR A 2 C9B C 0.2851(15) 0.4748(10) 0.5396(15) 0.025(3) Uani 0.277(8) 1 d PDU A 2 H9B H 0.2598 0.4429 0.5797 0.030 Uiso 0.277(8) 1 calc PR A 2 S2B S 0.3611(9) 0.5463(5) 0.5286(4) 0.0262(15) Uani 0.277(8) 1 d PDU A 2 C12B C 0.3712(11) 0.5734(6) 0.4493(6) 0.024(2) Uani 0.277(8) 1 d PDU A 2 C13 C 0.4302(4) 0.6342(2) 0.4047(2) 0.0186(10) Uani 1 1 d D . . C14 C 0.4832(5) 0.6791(3) 0.4286(3) 0.0232(11) Uani 1 1 d . A . H14 H 0.4707 0.6728 0.4731 0.028 Uiso 1 1 calc R . . C15 C 0.5530(4) 0.7318(3) 0.3891(3) 0.0204(10) Uani 1 1 d . . . C16 C 0.6216(5) 0.7666(4) 0.4231(3) 0.0308(13) Uani 1 1 d . A . C17 C 0.8468(5) 0.9739(3) 0.0830(3) 0.0269(11) Uani 1 1 d . . . H17 H 0.8493 1.0242 0.0661 0.032 Uiso 1 1 calc R . . C18 C 0.9407(5) 0.9253(3) 0.0724(3) 0.0293(12) Uani 1 1 d . . . H18 H 1.0138 0.9386 0.0467 0.035 Uiso 1 1 calc R . . C19 C 0.9180(5) 0.8517(3) 0.1040(2) 0.0236(11) Uani 1 1 d . . . H19 H 0.9729 0.8107 0.1031 0.028 Uiso 1 1 calc R . . C20 C 0.7975(4) 0.8509(3) 0.1373(3) 0.0190(10) Uani 1 1 d . . . C21 C 0.7327(4) 0.7896(3) 0.1757(2) 0.0169(9) Uani 1 1 d . . . C22 C 0.7941(4) 0.7193(3) 0.1836(3) 0.0202(10) Uani 1 1 d . . . H22 H 0.8711 0.7145 0.1601 0.024 Uiso 1 1 calc R . . C23 C 0.7471(4) 0.6587(3) 0.2235(3) 0.0173(10) Uani 1 1 d . . . C24 C 0.8271(5) 0.5871(3) 0.2310(3) 0.0232(11) Uani 1 1 d . . . C25 C 0.6985(5) 0.6038(3) 0.0075(3) 0.0309(12) Uani 1 1 d . . . H25 H 0.7583 0.5696 -0.0046 0.037 Uiso 1 1 calc R . . C26 C 0.6218(6) 0.6455(3) -0.0312(3) 0.0308(12) Uani 1 1 d . . . H26 H 0.6216 0.6433 -0.0730 0.037 Uiso 1 1 calc R . . C27 C 0.5425(5) 0.6925(3) -0.0018(3) 0.0224(10) Uani 1 1 d . . . H27 H 0.4828 0.7254 -0.0215 0.027 Uiso 1 1 calc R . . C28 C 0.5621(4) 0.6847(3) 0.0595(3) 0.0206(10) Uani 1 1 d . . . C29 C 0.4996(4) 0.7216(3) 0.1069(2) 0.0167(9) Uani 1 1 d . . . C30 C 0.4247(5) 0.7852(3) 0.0859(3) 0.0205(10) Uani 1 1 d . . . H30 H 0.4042 0.7972 0.0446 0.025 Uiso 1 1 calc R . . C31 C 0.3809(4) 0.8299(3) 0.1235(3) 0.0191(10) Uani 1 1 d . . . C32 C 0.3074(6) 0.8992(3) 0.0943(3) 0.0349(15) Uani 1 1 d . . . C33 C 0.5573(5) 0.4917(3) 0.3252(3) 0.0252(11) Uani 1 1 d . . . H33A H 0.6300 0.4602 0.3189 0.038 Uiso 1 1 calc R . . H33B H 0.5179 0.4755 0.3691 0.038 Uiso 1 1 calc R . . H33C H 0.5770 0.5409 0.3163 0.038 Uiso 1 1 calc R . . C34 C 0.4728(4) 0.5331(3) 0.2243(3) 0.0192(10) Uani 1 1 d . . . H34 H 0.5165 0.5733 0.2044 0.023 Uiso 1 1 calc R . . C35 C 0.3492(5) 0.4513(3) 0.2421(3) 0.0233(11) Uani 1 1 d . . . H35 H 0.2925 0.4247 0.2361 0.028 Uiso 1 1 calc R . . C36 C 0.4001(4) 0.4385(3) 0.2947(3) 0.0212(10) Uani 1 1 d . . . H36 H 0.3851 0.4014 0.3331 0.025 Uiso 1 1 calc R . . C37 C 0.3599(5) 0.5453(3) 0.1363(3) 0.0232(10) Uani 1 1 d . . . H37A H 0.3351 0.5085 0.1208 0.028 Uiso 1 1 calc R . . H37B H 0.4289 0.5656 0.1062 0.028 Uiso 1 1 calc R . . C38 C 0.2592(4) 0.6044(3) 0.1372(3) 0.0231(11) Uani 1 1 d . . . H38A H 0.2823 0.6407 0.1540 0.028 Uiso 1 1 calc R . . H38B H 0.1885 0.5840 0.1656 0.028 Uiso 1 1 calc R . . C39 C 0.2294(5) 0.6397(4) 0.0710(3) 0.0314(13) Uani 1 1 d . . . H39A H 0.1974 0.6046 0.0566 0.038 Uiso 1 1 calc R . . H39B H 0.3028 0.6543 0.0417 0.038 Uiso 1 1 calc R . . C40 C 0.1389(5) 0.7056(4) 0.0684(3) 0.0375(14) Uani 1 1 d . . . H40A H 0.1676 0.7386 0.0868 0.045 Uiso 1 1 calc R . . H40B H 0.0631 0.6903 0.0946 0.045 Uiso 1 1 calc R . . C41 C 0.1172(7) 0.7457(5) 0.0007(4) 0.057(2) Uani 1 1 d . . . H41A H 0.1943 0.7549 -0.0269 0.069 Uiso 1 1 calc R . . H41B H 0.0717 0.7926 0.0006 0.069 Uiso 1 1 calc R . . C42 C 0.0484(8) 0.7033(7) -0.0269(5) 0.081(4) Uani 1 1 d . . . H42A H 0.0982 0.6603 -0.0331 0.122 Uiso 1 1 calc R . . H42B H 0.0275 0.7336 -0.0677 0.122 Uiso 1 1 calc R . . H42C H -0.0240 0.6894 0.0026 0.122 Uiso 1 1 calc R . . C43 C 0.7571(6) 0.2821(4) 0.4350(3) 0.0358(14) Uani 1 1 d . . . H43 H 0.7720 0.2662 0.4776 0.043 Uiso 1 1 calc R . . C44 C 0.8270(5) 0.3243(3) 0.3876(4) 0.0336(14) Uani 1 1 d . . . H44 H 0.8953 0.3411 0.3940 0.040 Uiso 1 1 calc R . . C45 C 0.7904(4) 0.3416(2) 0.3278(2) 0.0097(8) Uani 1 1 d . . . H45 H 0.8294 0.3703 0.2892 0.012 Uiso 1 1 calc R . . C46 C 0.6818(4) 0.3078(3) 0.3354(2) 0.0160(9) Uani 1 1 d . . . C47 C 0.6068(4) 0.3095(2) 0.2887(2) 0.0155(9) Uani 1 1 d . . . C48 C 0.6439(4) 0.3453(3) 0.2243(3) 0.0190(10) Uani 1 1 d . . . H48 H 0.7159 0.3671 0.2127 0.023 Uiso 1 1 calc R . . C49 C 0.5777(4) 0.3492(3) 0.1778(2) 0.0156(9) Uani 1 1 d . . . C50 C 0.6279(5) 0.3867(3) 0.1092(3) 0.0219(10) Uani 1 1 d . . . S6A S 0.1020(2) 0.41767(10) 0.36526(11) 0.0248(6) Uani 0.777(7) 1 d PDU B 1 C51A C 0.0059(6) 0.4460(5) 0.4231(3) 0.0194(15) Uani 0.777(7) 1 d PDU B 1 H51A H -0.0365 0.4923 0.4160 0.023 Uiso 0.777(7) 1 calc PR B 1 C52A C -0.0042(8) 0.3942(4) 0.4819(4) 0.0246(15) Uani 0.777(7) 1 d PDU B 1 H52A H -0.0550 0.3998 0.5192 0.030 Uiso 0.777(7) 1 calc PR B 1 C53A C 0.0731(10) 0.3320(6) 0.4774(5) 0.023(2) Uani 0.777(7) 1 d PDU B 1 H53A H 0.0818 0.2908 0.5124 0.027 Uiso 0.777(7) 1 calc PR B 1 C54A C 0.1349(5) 0.3371(3) 0.4166(3) 0.0181(12) Uani 0.777(7) 1 d PDU B 1 C53B C 0.107(3) 0.4046(11) 0.3786(16) 0.021(3) Uani 0.223(7) 1 d PDU B 2 H53B H 0.1432 0.4196 0.3356 0.026 Uiso 0.223(7) 1 calc PR B 2 C52B C 0.022(3) 0.4512(19) 0.4062(14) 0.024(3) Uani 0.223(7) 1 d PDU B 2 H52B H -0.0080 0.4990 0.3872 0.029 Uiso 0.223(7) 1 calc PR B 2 C51B C -0.006(2) 0.4082(8) 0.4692(16) 0.021(3) Uani 0.223(7) 1 d PDU B 2 H51B H -0.0612 0.4268 0.4991 0.025 Uiso 0.223(7) 1 calc PR B 2 S6B S 0.0597(9) 0.3228(5) 0.4911(5) 0.0219(18) Uani 0.223(7) 1 d PDU B 2 C54B C 0.1343(10) 0.3354(8) 0.4172(7) 0.020(3) Uani 0.223(7) 1 d PDU B 2 C55 C 0.2192(4) 0.2832(3) 0.3920(2) 0.0170(9) Uani 1 1 d D . . C56 C 0.2420(4) 0.2133(3) 0.4338(3) 0.0186(10) Uani 1 1 d . B . H56 H 0.1999 0.2023 0.4759 0.022 Uiso 1 1 calc R . . C57 C 0.3229(4) 0.1610(3) 0.4154(3) 0.0172(10) Uani 1 1 d . . . C58 C 0.3458(5) 0.0908(3) 0.4667(3) 0.0231(11) Uani 1 1 d . B . C59 C -0.0711(5) 0.0439(3) 0.3996(3) 0.0278(12) Uani 1 1 d . . . H59 H -0.0880 -0.0005 0.4296 0.033 Uiso 1 1 calc R . . C60 C -0.1538(5) 0.0919(3) 0.3694(3) 0.0284(12) Uani 1 1 d . . . H60 H -0.2350 0.0842 0.3762 0.034 Uiso 1 1 calc R . . C61 C -0.1068(5) 0.1546(3) 0.3268(3) 0.0250(11) Uani 1 1 d . . . H61 H -0.1524 0.1933 0.3021 0.030 Uiso 1 1 calc R . . C62 C 0.0137(4) 0.1521(3) 0.3259(3) 0.0202(10) Uani 1 1 d . . . C63 C 0.0981(4) 0.2032(3) 0.2889(3) 0.0191(10) Uani 1 1 d . . . C64 C 0.0563(4) 0.2683(3) 0.2473(3) 0.0232(11) Uani 1 1 d . . . H64 H -0.0246 0.2752 0.2420 0.028 Uiso 1 1 calc R . . C65 C 0.1274(5) 0.3221(3) 0.2142(3) 0.0208(10) Uani 1 1 d . . . C66 C 0.0691(5) 0.3919(3) 0.1735(3) 0.0266(12) Uani 1 1 d . . . S8A S 0.22026(17) 0.19552(10) 0.08895(10) 0.0308(5) Uani 0.851(7) 1 d PDU C 1 C67A C 0.2184(6) 0.1602(4) 0.0284(3) 0.0370(15) Uani 0.851(7) 1 d PDU C 1 H67A H 0.1528 0.1674 0.0065 0.044 Uiso 0.851(7) 1 calc PR C 1 C68A C 0.3238(7) 0.1196(5) 0.0147(4) 0.0374(14) Uani 0.851(7) 1 d PDU C 1 H68A H 0.3389 0.0955 -0.0174 0.045 Uiso 0.851(7) 1 calc PR C 1 C69A C 0.4051(8) 0.1184(5) 0.0539(5) 0.0319(18) Uani 0.851(7) 1 d PDU C 1 H69A H 0.4822 0.0936 0.0514 0.038 Uiso 0.851(7) 1 calc PR C 1 C70A C 0.3606(5) 0.1577(3) 0.0971(3) 0.0232(11) Uani 0.851(7) 1 d PDU C 1 C69B C 0.249(2) 0.180(2) 0.0891(18) 0.032(3) Uani 0.149(7) 1 d PDU C 2 H69B H 0.2000 0.2115 0.1109 0.038 Uiso 0.149(7) 1 calc PR C 2 C68B C 0.212(2) 0.157(3) 0.043(2) 0.036(3) Uani 0.149(7) 1 d PDU C 2 H68B H 0.1363 0.1690 0.0293 0.043 Uiso 0.149(7) 1 calc PR C 2 C67B C 0.306(2) 0.1119(19) 0.0191(14) 0.035(3) Uani 0.149(7) 1 d PDU C 2 H67B H 0.3009 0.0903 -0.0128 0.042 Uiso 0.149(7) 1 calc PR C 2 S8B S 0.4285(13) 0.1007(8) 0.0539(8) 0.034(2) Uani 0.149(7) 1 d PDU C 2 C70B C 0.3633(19) 0.1532(10) 0.0994(7) 0.029(3) Uani 0.149(7) 1 d PDU C 2 C71 C 0.4184(4) 0.1700(3) 0.1459(2) 0.0202(10) Uani 1 1 d D . . C72 C 0.5410(5) 0.1500(3) 0.1463(3) 0.0218(10) Uani 1 1 d . C . H72 H 0.5870 0.1325 0.1131 0.026 Uiso 1 1 calc R . . C73 C 0.5947(4) 0.1558(3) 0.1940(3) 0.0195(10) Uani 1 1 d . . . C74 C 0.7288(5) 0.1381(3) 0.1896(3) 0.0249(11) Uani 1 1 d . C . C75 C 0.4339(5) -0.0053(3) 0.6500(3) 0.0279(12) Uani 1 1 d . . . H75A H 0.4550 0.0271 0.6077 0.042 Uiso 1 1 calc R . . H75B H 0.3496 0.0047 0.6653 0.042 Uiso 1 1 calc R . . H75C H 0.4497 -0.0550 0.6480 0.042 Uiso 1 1 calc R . . C76 C 0.6069(4) -0.0315(3) 0.7070(2) 0.0188(10) Uani 1 1 d . . . H76 H 0.6463 -0.0694 0.6904 0.023 Uiso 1 1 calc R . . C77 C 0.5647(5) 0.0495(3) 0.7602(3) 0.0214(10) Uani 1 1 d . . . H77 H 0.5707 0.0779 0.7868 0.026 Uiso 1 1 calc R . . C78 C 0.4767(5) 0.0553(3) 0.7270(3) 0.0237(11) Uani 1 1 d . . . H78 H 0.4074 0.0881 0.7269 0.028 Uiso 1 1 calc R . . C79 C 0.7591(4) -0.0292(3) 0.7719(3) 0.0213(10) Uani 1 1 d . . . H79A H 0.7936 -0.0749 0.7626 0.026 Uiso 1 1 calc R . . H79B H 0.7455 -0.0377 0.8184 0.026 Uiso 1 1 calc R . . C80 C 0.8451(4) 0.0266(3) 0.7418(3) 0.0206(10) Uani 1 1 d . . . H80A H 0.8116 0.0716 0.7524 0.025 Uiso 1 1 calc R . . H80B H 0.8558 0.0364 0.6951 0.025 Uiso 1 1 calc R . . C81 C 0.9661(5) 0.0026(3) 0.7641(4) 0.0311(13) Uani 1 1 d . . . H81A H 0.9967 -0.0444 0.7564 0.037 Uiso 1 1 calc R . . H81B H 0.9562 -0.0037 0.8103 0.037 Uiso 1 1 calc R . . C82 C 1.0571(5) 0.0568(3) 0.7297(3) 0.0317(13) Uani 1 1 d . . . H82A H 1.1363 0.0352 0.7402 0.038 Uiso 1 1 calc R . . H82B H 1.0608 0.0668 0.6834 0.038 Uiso 1 1 calc R . . C83 C 1.0283(5) 0.1267(3) 0.7471(3) 0.0258(11) Uani 1 1 d . . . H83A H 0.9483 0.1479 0.7377 0.031 Uiso 1 1 calc R . . H83B H 1.0272 0.1172 0.7932 0.031 Uiso 1 1 calc R . . C84 C 1.1168(5) 0.1796(3) 0.7114(3) 0.0326(13) Uani 1 1 d . . . H84A H 1.1961 0.1589 0.7207 0.049 Uiso 1 1 calc R . . H84B H 1.0957 0.2238 0.7245 0.049 Uiso 1 1 calc R . . H84C H 1.1161 0.1906 0.6657 0.049 Uiso 1 1 calc R . . F1 F 0.1692(3) 0.58088(16) 0.28791(17) 0.0268(7) Uani 1 1 d . . . F2 F 0.0281(3) 0.6354(2) 0.33950(18) 0.0338(8) Uani 1 1 d . . . F3 F 0.0689(3) 0.67504(19) 0.23781(18) 0.0307(7) Uani 1 1 d . . . F4 F 0.6325(3) 0.8356(2) 0.3925(2) 0.0415(9) Uani 1 1 d . . . F5 F 0.5745(5) 0.7635(4) 0.4817(2) 0.0751(19) Uani 1 1 d . . . F6 F 0.7323(3) 0.7344(2) 0.4234(2) 0.0430(9) Uani 1 1 d . . . F7 F 0.7734(3) 0.53820(16) 0.21826(17) 0.0270(7) Uani 1 1 d . . . F8 F 0.9306(3) 0.59250(18) 0.1929(2) 0.0373(9) Uani 1 1 d . . . F9 F 0.8478(3) 0.55989(19) 0.2906(2) 0.0393(9) Uani 1 1 d . . . F10 F 0.3565(9) 0.9544(3) 0.0939(5) 0.127(4) Uani 1 1 d . . . F11 F 0.2899(5) 0.9076(3) 0.0363(2) 0.0663(17) Uani 1 1 d . . . F12 F 0.2044(6) 0.9060(4) 0.1279(3) 0.106(3) Uani 1 1 d . . . F13 F 0.6489(3) 0.3410(2) 0.07412(17) 0.0360(8) Uani 1 1 d . . . F14 F 0.7267(3) 0.4171(2) 0.10246(18) 0.0383(8) Uani 1 1 d . . . F15 F 0.5484(3) 0.43952(19) 0.08272(17) 0.0355(8) Uani 1 1 d . . . F16 F 0.4561(3) 0.08200(17) 0.47828(18) 0.0321(7) Uani 1 1 d . . . F17 F 0.2742(3) 0.08501(19) 0.52270(17) 0.0359(8) Uani 1 1 d . . . F18 F 0.3318(3) 0.03424(17) 0.44772(18) 0.0327(7) Uani 1 1 d . . . F19 F 0.0728(6) 0.4454(3) 0.1967(4) 0.095(3) Uani 1 1 d . . . F20 F -0.0432(4) 0.3913(2) 0.1716(3) 0.0589(13) Uani 1 1 d . . . F21 F 0.1243(5) 0.4105(4) 0.1164(3) 0.096(3) Uani 1 1 d . . . F22 F 0.7813(3) 0.1956(2) 0.1829(2) 0.0414(9) Uani 1 1 d . . . F23 F 0.7787(3) 0.1118(2) 0.1408(2) 0.0457(10) Uani 1 1 d . . . F24 F 0.7581(3) 0.0898(2) 0.2426(2) 0.0448(10) Uani 1 1 d . . . N1 N 0.4777(4) 0.4895(2) 0.2820(2) 0.0214(9) Uani 1 1 d . . . N2 N 0.3963(4) 0.5106(2) 0.1991(2) 0.0222(9) Uani 1 1 d . . . N3 N 0.5043(4) 0.0055(2) 0.6933(2) 0.0200(8) Uani 1 1 d . . . N4 N 0.6450(4) -0.0063(2) 0.7478(2) 0.0183(8) Uani 1 1 d . . . O1 O 0.3452(3) 0.79485(18) 0.31222(17) 0.0165(7) Uani 1 1 d . A . O2 O 0.3005(3) 0.69280(18) 0.25504(17) 0.0165(7) Uani 1 1 d . A . O3 O 0.4356(3) 0.64122(18) 0.34640(17) 0.0184(7) Uani 1 1 d . A . O4 O 0.5724(3) 0.7541(2) 0.32969(18) 0.0210(7) Uani 1 1 d . A . O5 O 0.6277(3) 0.80237(18) 0.19998(18) 0.0187(7) Uani 1 1 d . A . O6 O 0.6471(3) 0.65176(18) 0.25697(18) 0.0178(7) Uani 1 1 d . A . O7 O 0.5197(3) 0.69571(18) 0.16295(16) 0.0173(7) Uani 1 1 d . A . O8 O 0.3935(3) 0.82436(18) 0.17951(18) 0.0185(7) Uani 1 1 d . A . O9 O 0.5128(3) 0.27980(18) 0.30875(17) 0.0156(7) Uani 1 1 d . B . O10 O 0.4805(3) 0.32421(19) 0.18335(17) 0.0182(7) Uani 1 1 d . B . O11 O 0.2665(3) 0.30319(18) 0.33524(17) 0.0167(7) Uani 1 1 d . B . O12 O 0.3832(3) 0.16106(18) 0.36255(18) 0.0194(7) Uani 1 1 d . B . O13 O 0.2056(3) 0.18639(18) 0.29682(18) 0.0176(7) Uani 1 1 d . B . O14 O 0.2365(3) 0.32535(18) 0.21302(18) 0.0182(7) Uani 1 1 d . B . O15 O 0.3525(3) 0.19810(19) 0.18562(18) 0.0200(7) Uani 1 1 d . B . O16 O 0.5469(3) 0.17315(19) 0.24449(19) 0.0200(7) Uani 1 1 d . B . S1 S 0.29626(12) 0.86882(8) 0.40960(7) 0.0291(3) Uani 1 1 d . . . S3 S 0.72621(12) 0.93614(7) 0.12912(7) 0.0290(3) Uani 1 1 d . . . S4 S 0.67588(12) 0.61938(7) 0.08021(6) 0.0258(3) Uani 1 1 d . . . S5 S 0.64141(13) 0.26017(8) 0.41201(7) 0.0326(3) Uani 1 1 d . . . S7 S 0.06688(11) 0.07333(7) 0.37679(6) 0.0235(2) Uani 1 1 d . . . Yb1 Yb 0.48034(2) 0.732156(13) 0.255001(12) 0.01387(7) Uani 1 1 d . . . Yb2 Yb 0.37645(2) 0.244946(13) 0.264471(12) 0.01362(7) Uani 1 1 d . . . O17 O -0.031(2) 0.5573(14) 0.0673(12) 0.035(7) Uani 0.159(12) 1 d PDU . . H17A H -0.0480 0.5219 0.0982 0.052 Uiso 0.159(12) 1 calc PR . . C85 C 0.009(3) 0.5346(17) 0.0123(13) 0.020(7) Uani 0.159(12) 1 d PDU . . H85A H -0.0285 0.5673 -0.0228 0.031 Uiso 0.159(12) 1 calc PR . . H85B H -0.0128 0.4861 0.0200 0.031 Uiso 0.159(12) 1 calc PR . . H85C H 0.0950 0.5346 0.0015 0.031 Uiso 0.159(12) 1 calc PR . . 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 0.043(3) 0.026(3) 0.020(3) -0.010(2) 0.002(2) -0.004(2) C2 0.035(3) 0.029(3) 0.026(3) -0.013(2) 0.010(2) -0.004(2) C3 0.020(2) 0.012(2) 0.014(2) -0.0077(18) -0.0063(19) 0.0039(17) C4 0.020(2) 0.018(2) 0.016(2) -0.003(2) -0.0019(19) -0.0058(18) C5 0.016(2) 0.015(2) 0.014(2) -0.0012(18) -0.0003(18) -0.0033(17) C6 0.022(2) 0.019(2) 0.012(2) -0.0023(19) -0.0032(19) -0.0057(18) C7 0.014(2) 0.018(2) 0.017(2) -0.0010(19) -0.0022(19) -0.0032(17) C8 0.020(2) 0.024(3) 0.025(3) -0.012(2) -0.002(2) -0.003(2) S2A 0.0253(11) 0.0294(10) 0.0222(13) -0.0059(8) -0.0004(8) -0.0104(8) C9A 0.020(3) 0.027(3) 0.025(4) -0.001(3) -0.001(3) -0.003(2) C10A 0.026(3) 0.037(4) 0.023(3) 0.005(3) -0.008(3) -0.005(3) C11A 0.025(3) 0.032(3) 0.022(4) 0.001(3) -0.003(3) -0.005(3) C12A 0.016(2) 0.025(3) 0.018(3) -0.001(2) -0.002(2) 0.002(2) C11B 0.020(4) 0.029(4) 0.022(4) -0.002(4) -0.003(4) -0.006(4) C10B 0.021(4) 0.028(4) 0.023(5) -0.004(4) 0.001(4) -0.004(4) C9B 0.020(5) 0.031(5) 0.025(5) -0.001(5) -0.009(5) -0.010(4) S2B 0.027(2) 0.034(3) 0.014(3) -0.003(2) -0.002(2) -0.004(2) C12B 0.021(4) 0.028(4) 0.020(4) -0.001(4) -0.002(4) -0.002(3) C13 0.015(2) 0.023(2) 0.016(3) -0.005(2) -0.0049(19) 0.0054(18) C14 0.023(2) 0.030(3) 0.016(3) -0.005(2) -0.004(2) -0.003(2) C15 0.013(2) 0.030(3) 0.019(3) -0.011(2) 0.0004(19) -0.0035(19) C16 0.026(3) 0.052(4) 0.020(3) -0.014(3) -0.004(2) -0.012(2) C17 0.031(3) 0.028(3) 0.021(3) -0.007(2) 0.003(2) -0.008(2) C18 0.025(3) 0.039(3) 0.020(3) -0.002(2) 0.003(2) -0.013(2) C19 0.038(3) 0.025(3) 0.008(2) -0.001(2) 0.001(2) -0.019(2) C20 0.016(2) 0.022(2) 0.017(2) -0.005(2) 0.0003(19) -0.0024(18) C21 0.017(2) 0.022(2) 0.014(2) -0.008(2) -0.0022(19) -0.0054(18) C22 0.012(2) 0.021(2) 0.029(3) -0.012(2) 0.0016(19) -0.0004(18) C23 0.015(2) 0.021(2) 0.019(3) -0.010(2) -0.0070(19) 0.0013(18) C24 0.017(2) 0.019(2) 0.035(3) -0.011(2) -0.005(2) 0.0016(19) C25 0.035(3) 0.029(3) 0.028(3) -0.014(3) 0.003(2) 0.001(2) C26 0.041(3) 0.035(3) 0.016(3) -0.009(2) -0.001(2) -0.006(3) C27 0.026(3) 0.022(2) 0.017(3) -0.007(2) 0.005(2) -0.004(2) C28 0.020(2) 0.020(2) 0.021(3) -0.008(2) 0.001(2) -0.0047(19) C29 0.014(2) 0.020(2) 0.015(2) -0.003(2) -0.0008(18) -0.0048(17) C30 0.023(2) 0.022(2) 0.015(2) -0.004(2) -0.002(2) 0.0004(19) C31 0.016(2) 0.020(2) 0.020(3) -0.002(2) -0.0051(19) -0.0030(18) C32 0.046(4) 0.030(3) 0.027(3) -0.011(3) -0.018(3) 0.019(3) C33 0.023(3) 0.024(3) 0.028(3) -0.007(2) -0.005(2) 0.000(2) C34 0.018(2) 0.018(2) 0.021(3) -0.005(2) 0.0003(19) -0.0053(18) C35 0.018(2) 0.019(2) 0.031(3) -0.010(2) 0.005(2) -0.0019(19) C36 0.016(2) 0.016(2) 0.028(3) -0.005(2) 0.005(2) -0.0025(18) C37 0.022(2) 0.028(3) 0.018(3) -0.006(2) 0.002(2) -0.003(2) C38 0.016(2) 0.031(3) 0.018(3) -0.007(2) 0.0026(19) 0.000(2) C39 0.028(3) 0.046(3) 0.019(3) -0.011(3) -0.003(2) 0.002(2) C40 0.024(3) 0.055(4) 0.024(3) -0.006(3) 0.003(2) 0.007(3) C41 0.038(4) 0.080(6) 0.029(4) 0.003(4) 0.001(3) 0.027(4) C42 0.051(5) 0.143(10) 0.051(6) -0.041(7) -0.031(5) 0.046(6) C43 0.046(4) 0.040(3) 0.025(3) -0.007(3) -0.018(3) -0.002(3) C44 0.023(3) 0.037(3) 0.051(4) -0.022(3) -0.018(3) 0.000(2) C45 0.012(2) 0.0095(19) 0.007(2) -0.0017(16) -0.0039(16) 0.0051(15) C46 0.014(2) 0.017(2) 0.016(2) -0.0033(19) -0.0017(18) -0.0019(17) C47 0.008(2) 0.016(2) 0.021(3) -0.006(2) 0.0002(18) -0.0017(16) C48 0.011(2) 0.027(2) 0.018(2) -0.005(2) 0.0039(18) -0.0049(18) C49 0.015(2) 0.017(2) 0.014(2) -0.0056(19) 0.0020(18) -0.0008(17) C50 0.019(2) 0.026(3) 0.017(3) -0.002(2) 0.000(2) -0.002(2) S6A 0.0218(8) 0.0191(10) 0.0255(13) -0.0017(7) 0.0046(8) 0.0026(7) C51A 0.016(3) 0.020(3) 0.019(4) -0.007(3) 0.010(2) -0.002(2) C52A 0.024(3) 0.027(3) 0.019(4) -0.003(3) 0.000(2) -0.004(3) C53A 0.021(3) 0.024(3) 0.023(4) -0.005(3) -0.004(3) -0.004(3) C54A 0.014(2) 0.022(2) 0.020(2) -0.008(2) -0.003(2) -0.002(2) C53B 0.017(4) 0.021(4) 0.023(4) -0.004(4) 0.001(4) -0.003(4) C52B 0.020(4) 0.021(4) 0.024(5) -0.003(4) 0.005(4) 0.001(4) C51B 0.020(4) 0.021(4) 0.020(5) -0.006(4) 0.000(4) -0.003(4) S6B 0.020(3) 0.023(3) 0.019(3) -0.003(3) 0.000(2) 0.001(2) C54B 0.017(4) 0.022(4) 0.020(4) -0.006(4) -0.002(4) -0.002(4) C55 0.014(2) 0.019(2) 0.019(3) -0.004(2) -0.0050(19) -0.0053(17) C56 0.016(2) 0.023(2) 0.019(2) -0.009(2) -0.0019(19) -0.0027(18) C57 0.016(2) 0.015(2) 0.023(3) -0.004(2) -0.008(2) -0.0058(17) C58 0.030(3) 0.017(2) 0.022(3) -0.003(2) -0.006(2) -0.003(2) C59 0.031(3) 0.028(3) 0.026(3) -0.013(2) 0.008(2) -0.012(2) C60 0.020(3) 0.032(3) 0.035(3) -0.015(3) 0.002(2) -0.009(2) C61 0.019(2) 0.023(3) 0.034(3) -0.011(2) 0.001(2) -0.0066(19) C62 0.019(2) 0.023(2) 0.020(3) -0.010(2) 0.000(2) -0.0002(19) C63 0.015(2) 0.025(3) 0.023(3) -0.016(2) -0.004(2) 0.0009(19) C64 0.012(2) 0.028(3) 0.030(3) -0.009(2) -0.006(2) 0.0009(19) C65 0.020(2) 0.025(3) 0.016(2) -0.006(2) -0.002(2) 0.0009(19) C66 0.015(2) 0.031(3) 0.030(3) -0.004(2) -0.005(2) 0.004(2) S8A 0.0324(10) 0.0318(10) 0.0330(10) -0.0095(8) -0.0189(8) 0.0004(7) C67A 0.047(3) 0.044(3) 0.026(3) -0.010(3) -0.017(3) -0.008(3) C68A 0.049(3) 0.041(3) 0.028(3) -0.012(3) -0.014(3) -0.006(3) C69A 0.042(3) 0.032(4) 0.025(3) -0.013(3) -0.006(3) -0.003(3) C70A 0.028(2) 0.024(2) 0.021(2) -0.007(2) -0.009(2) -0.005(2) C69B 0.039(4) 0.033(4) 0.027(4) -0.008(4) -0.013(4) -0.005(4) C68B 0.043(4) 0.039(4) 0.029(4) -0.009(4) -0.017(4) -0.004(4) C67B 0.045(4) 0.040(5) 0.027(4) -0.011(4) -0.015(4) -0.006(4) S8B 0.045(4) 0.037(5) 0.025(4) -0.011(4) -0.010(4) -0.009(4) C70B 0.037(4) 0.030(5) 0.024(4) -0.009(4) -0.009(4) -0.005(4) C71 0.023(2) 0.018(2) 0.021(3) -0.008(2) -0.003(2) -0.0052(19) C72 0.025(3) 0.022(2) 0.018(3) -0.008(2) -0.001(2) 0.002(2) C73 0.016(2) 0.019(2) 0.021(3) -0.005(2) -0.0016(19) 0.0021(18) C74 0.018(2) 0.029(3) 0.027(3) -0.010(2) -0.004(2) 0.006(2) C75 0.031(3) 0.028(3) 0.028(3) -0.010(2) -0.011(2) -0.001(2) C76 0.020(2) 0.016(2) 0.019(2) -0.005(2) 0.0047(19) -0.0061(18) C77 0.021(2) 0.018(2) 0.023(3) -0.006(2) 0.002(2) -0.0031(19) C78 0.020(2) 0.025(3) 0.023(3) -0.007(2) 0.002(2) -0.001(2) C79 0.020(2) 0.019(2) 0.024(3) -0.005(2) -0.005(2) 0.0012(19) C80 0.018(2) 0.019(2) 0.024(3) -0.002(2) -0.006(2) -0.0025(18) C81 0.021(3) 0.019(3) 0.056(4) -0.013(3) -0.014(3) 0.006(2) C82 0.015(2) 0.038(3) 0.044(4) -0.018(3) -0.002(2) 0.003(2) C83 0.021(2) 0.029(3) 0.026(3) -0.007(2) -0.002(2) 0.000(2) C84 0.023(3) 0.034(3) 0.037(3) 0.000(3) -0.006(2) -0.012(2) F1 0.0303(16) 0.0216(15) 0.0307(18) -0.0081(14) -0.0047(14) -0.0080(12) F2 0.0262(16) 0.048(2) 0.0326(19) -0.0193(17) 0.0084(14) -0.0216(14) F3 0.0236(16) 0.0411(19) 0.0331(19) -0.0141(16) -0.0142(14) -0.0006(13) F4 0.044(2) 0.040(2) 0.055(3) -0.028(2) -0.0150(19) -0.0099(16) F5 0.066(3) 0.154(6) 0.031(2) -0.050(3) 0.021(2) -0.076(3) F6 0.0273(18) 0.052(2) 0.050(2) 0.0005(19) -0.0224(17) -0.0119(16) F7 0.0214(15) 0.0212(15) 0.040(2) -0.0116(14) -0.0039(13) -0.0011(12) F8 0.0137(15) 0.0274(17) 0.064(3) -0.0133(17) 0.0076(15) 0.0008(12) F9 0.044(2) 0.0331(18) 0.042(2) -0.0089(17) -0.0243(18) 0.0122(15) F10 0.211(10) 0.027(3) 0.164(9) -0.006(4) -0.138(8) 0.021(4) F11 0.099(4) 0.067(3) 0.028(2) -0.021(2) -0.034(2) 0.055(3) F12 0.081(4) 0.143(6) 0.045(3) -0.004(3) -0.006(3) 0.088(4) F13 0.0397(19) 0.045(2) 0.0191(17) -0.0122(15) 0.0082(14) -0.0014(15) F14 0.0287(17) 0.054(2) 0.0248(18) 0.0018(16) 0.0032(14) -0.0174(15) F15 0.0318(18) 0.0357(18) 0.0259(18) 0.0046(15) -0.0009(14) 0.0047(14) F16 0.0346(18) 0.0265(16) 0.0341(19) -0.0008(14) -0.0193(15) 0.0019(13) F17 0.046(2) 0.0298(17) 0.0205(17) 0.0025(14) 0.0024(15) 0.0029(15) F18 0.049(2) 0.0186(15) 0.0309(19) -0.0031(14) -0.0115(16) -0.0071(14) F19 0.120(5) 0.038(3) 0.152(7) -0.038(4) -0.098(5) 0.037(3) F20 0.0225(19) 0.059(3) 0.073(3) 0.022(2) -0.019(2) -0.0040(17) F21 0.057(3) 0.114(5) 0.043(3) 0.041(3) 0.020(2) 0.048(3) F22 0.0198(16) 0.041(2) 0.067(3) -0.023(2) -0.0047(17) -0.0019(14) F23 0.0264(18) 0.068(3) 0.053(3) -0.042(2) -0.0041(17) 0.0137(17) F24 0.0269(18) 0.053(2) 0.042(2) -0.0034(19) -0.0085(17) 0.0185(17) N1 0.019(2) 0.018(2) 0.026(2) -0.0061(19) -0.0007(18) -0.0019(16) N2 0.019(2) 0.026(2) 0.022(2) -0.0102(19) 0.0031(17) -0.0052(17) N3 0.018(2) 0.017(2) 0.023(2) -0.0050(18) -0.0001(17) -0.0048(16) N4 0.017(2) 0.0170(19) 0.019(2) -0.0040(17) 0.0009(17) -0.0035(15) O1 0.0150(16) 0.0163(16) 0.0180(17) -0.0044(14) -0.0015(13) -0.0027(12) O2 0.0121(15) 0.0247(17) 0.0146(17) -0.0093(14) 0.0028(13) -0.0066(12) O3 0.0183(16) 0.0200(17) 0.0156(18) -0.0051(14) -0.0011(14) 0.0000(13) O4 0.0166(16) 0.0268(18) 0.0220(19) -0.0109(16) -0.0008(14) -0.0040(13) O5 0.0130(16) 0.0215(17) 0.0201(18) -0.0061(15) -0.0003(14) 0.0002(13) O6 0.0129(16) 0.0171(16) 0.0222(18) -0.0057(14) -0.0018(14) 0.0020(12) O7 0.0232(17) 0.0179(16) 0.0108(17) -0.0048(14) -0.0014(14) -0.0021(13) O8 0.0186(16) 0.0167(16) 0.0188(18) -0.0019(14) -0.0039(14) -0.0022(13) O9 0.0122(15) 0.0191(16) 0.0169(17) -0.0059(14) -0.0032(13) -0.0029(12) O10 0.0148(16) 0.0223(17) 0.0161(17) -0.0038(14) -0.0017(13) -0.0018(13) O11 0.0155(15) 0.0155(15) 0.0185(18) -0.0070(14) 0.0023(13) -0.0012(12) O12 0.0177(16) 0.0190(16) 0.0211(19) -0.0049(15) -0.0043(14) -0.0007(13) O13 0.0129(15) 0.0184(16) 0.0213(18) -0.0051(14) -0.0008(13) -0.0042(12) O14 0.0127(16) 0.0193(16) 0.0222(18) -0.0051(14) -0.0044(13) 0.0009(12) O15 0.0181(16) 0.0231(17) 0.0226(19) -0.0115(15) -0.0052(14) -0.0005(13) O16 0.0145(16) 0.0244(18) 0.0240(19) -0.0124(16) -0.0038(14) 0.0018(13) S1 0.0302(7) 0.0313(7) 0.0286(7) -0.0138(6) 0.0012(6) -0.0081(5) S3 0.0305(7) 0.0254(6) 0.0283(7) -0.0066(6) 0.0031(5) -0.0058(5) S4 0.0259(6) 0.0292(6) 0.0213(6) -0.0099(5) -0.0016(5) 0.0030(5) S5 0.0332(7) 0.0399(8) 0.0243(7) -0.0038(6) -0.0060(6) -0.0115(6) S7 0.0213(6) 0.0260(6) 0.0219(6) -0.0059(5) 0.0006(5) -0.0048(5) Yb1 0.01199(12) 0.01594(12) 0.01364(13) -0.00491(10) -0.00016(9) -0.00203(9) Yb2 0.01056(11) 0.01535(12) 0.01513(13) -0.00466(10) -0.00206(9) -0.00092(8) O17 0.035(10) 0.030(10) 0.037(11) -0.006(8) -0.013(8) 0.008(7) C85 0.021(8) 0.021(9) 0.022(9) -0.007(5) -0.009(5) 0.000(5) _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 C2 1.359(9) . ? C1 S1 1.689(6) . ? C1 H1 0.9500 . ? C2 C3 1.450(7) . ? C2 H2 0.9500 . ? C3 C4 1.456(7) . ? C3 H3 0.9500 . ? C4 C5 1.478(7) . ? C4 S1 1.719(5) . ? C5 O1 1.257(6) . ? C5 C6 1.428(7) . ? C6 C7 1.372(7) . ? C6 H6 0.9500 . ? C7 O2 1.267(6) . ? C7 C8 1.540(7) . ? C8 F2 1.332(7) . ? C8 F1 1.337(6) . ? C8 F3 1.349(7) . ? S2A C12A 1.681(7) . ? S2A C9A 1.696(7) . ? C9A C10A 1.399(8) . ? C9A H9A 0.9500 . ? C10A C11A 1.420(10) . ? C10A H10A 0.9500 . ? C11A C12A 1.396(9) . ? C11A H11A 0.9500 . ? C12A C13 1.469(7) . ? C11B C12B 1.402(10) . ? C11B C10B 1.417(10) . ? C11B H11B 0.9500 . ? C10B C9B 1.416(10) . ? C10B H10B 0.9500 . ? C9B S2B 1.701(10) . ? C9B H9B 0.9500 . ? S2B C12B 1.679(10) . ? C12B C13 1.470(9) . ? C13 O3 1.261(6) . ? C13 C14 1.420(7) . ? C14 C15 1.390(8) . ? C14 H14 0.9500 . ? C15 O4 1.256(7) . ? C15 C16 1.547(7) . ? C16 F5 1.306(8) . ? C16 F4 1.335(8) . ? C16 F6 1.340(7) . ? C17 C18 1.369(8) . ? C17 S3 1.691(6) . ? C17 H17 0.9500 . ? C18 C19 1.446(8) . ? C18 H18 0.9500 . ? C19 C20 1.447(8) . ? C19 H19 0.9500 . ? C20 C21 1.468(8) . ? C20 S3 1.727(5) . ? C21 O5 1.252(6) . ? C21 C22 1.433(7) . ? C22 C23 1.373(8) . ? C22 H22 0.9500 . ? C23 O6 1.253(7) . ? C23 C24 1.547(6) . ? C24 F8 1.326(7) . ? C24 F9 1.335(8) . ? C24 F7 1.343(6) . ? C25 C26 1.364(9) . ? C25 S4 1.710(6) . ? C25 H25 0.9500 . ? C26 C27 1.417(8) . ? C26 H26 0.9500 . ? C27 C28 1.394(8) . ? C27 H27 0.9500 . ? C28 C29 1.477(7) . ? C28 S4 1.721(5) . ? C29 O7 1.258(6) . ? C29 C30 1.417(7) . ? C30 C31 1.374(7) . ? C30 H30 0.9500 . ? C31 O8 1.260(7) . ? C31 C32 1.528(7) . ? C32 F12 1.292(10) . ? C32 F10 1.296(10) . ? C32 F11 1.312(8) . ? C33 N1 1.472(7) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 N2 1.323(7) . ? C34 N1 1.324(7) . ? C34 H34 0.9500 . ? C35 C36 1.357(8) . ? C35 N2 1.378(8) . ? C35 H35 0.9500 . ? C36 N1 1.376(7) . ? C36 H36 0.9500 . ? C37 N2 1.478(7) . ? C37 C38 1.517(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.517(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.531(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.533(10) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.551(15) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.345(11) . ? C43 S5 1.679(6) . ? C43 H43 0.9500 . ? C44 C45 1.411(8) . ? C44 H44 0.9500 . ? C45 C46 1.467(6) . ? C45 H45 0.9500 . ? C46 C47 1.473(6) . ? C46 S5 1.701(5) . ? C47 O9 1.253(6) . ? C47 C48 1.414(7) . ? C48 C49 1.385(7) . ? C48 H48 0.9500 . ? C49 O10 1.263(6) . ? C49 C50 1.531(7) . ? C50 F13 1.329(6) . ? C50 F14 1.331(7) . ? C50 F15 1.352(6) . ? S6A C54A 1.693(6) . ? S6A C51A 1.708(6) . ? C51A C52A 1.397(8) . ? C51A H51A 0.9500 . ? C52A C53A 1.421(9) . ? C52A H52A 0.9500 . ? C53A C54A 1.391(8) . ? C53A H53A 0.9500 . ? C54A C55 1.487(7) . ? C53B C54B 1.402(10) . ? C53B C52B 1.420(10) . ? C53B H53B 0.9500 . ? C52B C51B 1.414(10) . ? C52B H52B 0.9500 . ? C51B S6B 1.702(10) . ? C51B H51B 0.9500 . ? S6B C54B 1.676(10) . ? C54B C55 1.473(10) . ? C55 O11 1.252(7) . ? C55 C56 1.430(7) . ? C56 C57 1.386(7) . ? C56 H56 0.9500 . ? C57 O12 1.252(7) . ? C57 C58 1.533(7) . ? C58 F16 1.325(6) . ? C58 F17 1.346(7) . ? C58 F18 1.346(6) . ? C59 C60 1.361(9) . ? C59 S7 1.712(6) . ? C59 H59 0.9500 . ? C60 C61 1.421(9) . ? C60 H60 0.9500 . ? C61 C62 1.383(7) . ? C61 H61 0.9500 . ? C62 C63 1.460(8) . ? C62 S7 1.730(5) . ? C63 O13 1.269(6) . ? C63 C64 1.417(8) . ? C64 C65 1.379(8) . ? C64 H64 0.9500 . ? C65 O14 1.268(6) . ? C65 C66 1.540(7) . ? C66 F21 1.284(8) . ? C66 F20 1.309(7) . ? C66 F19 1.315(8) . ? S8A C70A 1.699(6) . ? S8A C67A 1.705(6) . ? C67A C68A 1.388(8) . ? C67A H67A 0.9500 . ? C68A C69A 1.399(8) . ? C68A H68A 0.9500 . ? C69A C70A 1.391(8) . ? C69A H69A 0.9500 . ? C70A C71 1.479(6) . ? C69B C70B 1.388(10) . ? C69B C68B 1.416(10) . ? C69B H69B 0.9500 . ? C68B C67B 1.416(10) . ? C68B H68B 0.9500 . ? C67B S8B 1.701(10) . ? C67B H67B 0.9500 . ? S8B C70B 1.667(10) . ? C70B C71 1.458(10) . ? C71 O15 1.259(6) . ? C71 C72 1.413(7) . ? C72 C73 1.374(7) . ? C72 H72 0.9500 . ? C73 O16 1.279(7) . ? C73 C74 1.527(7) . ? C74 F22 1.321(7) . ? C74 F23 1.340(7) . ? C74 F24 1.343(7) . ? C75 N3 1.457(7) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 N4 1.330(7) . ? C76 N3 1.333(7) . ? C76 H76 0.9500 . ? C77 C78 1.343(8) . ? C77 N4 1.384(6) . ? C77 H77 0.9500 . ? C78 N3 1.375(7) . ? C78 H78 0.9500 . ? C79 N4 1.477(6) . ? C79 C80 1.508(7) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.535(7) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 C82 1.540(9) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.512(8) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.509(8) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? O1 Yb1 2.281(3) . ? O2 Yb1 2.326(3) . ? O3 Yb1 2.307(4) . ? O4 Yb1 2.319(3) . ? O5 Yb1 2.282(4) . ? O6 Yb1 2.300(3) . ? O7 Yb1 2.324(3) . ? O8 Yb1 2.326(3) . ? O9 Yb2 2.297(3) . ? O10 Yb2 2.280(4) . ? O11 Yb2 2.306(3) . ? O12 Yb2 2.323(4) . ? O13 Yb2 2.322(3) . ? O14 Yb2 2.301(3) . ? O15 Yb2 2.300(3) . ? O16 Yb2 2.297(3) . ? O17 C85 1.405(10) . ? O17 H17A 0.8400 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 S1 113.1(4) . . ? C2 C1 H1 123.4 . . ? S1 C1 H1 123.4 . . ? C1 C2 C3 115.1(5) . . ? C1 C2 H2 122.5 . . ? C3 C2 H2 122.5 . . ? C2 C3 C4 106.9(4) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C3 C4 C5 129.4(4) . . ? C3 C4 S1 112.7(3) . . ? C5 C4 S1 117.8(4) . . ? O1 C5 C6 124.9(4) . . ? O1 C5 C4 117.1(4) . . ? C6 C5 C4 118.0(4) . . ? C7 C6 C5 122.2(5) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? O2 C7 C6 130.3(5) . . ? O2 C7 C8 112.9(4) . . ? C6 C7 C8 116.8(5) . . ? F2 C8 F1 107.5(5) . . ? F2 C8 F3 107.0(4) . . ? F1 C8 F3 106.5(4) . . ? F2 C8 C7 114.1(4) . . ? F1 C8 C7 111.5(4) . . ? F3 C8 C7 109.9(5) . . ? C12A S2A C9A 91.8(5) . . ? C10A C9A S2A 112.9(10) . . ? C10A C9A H9A 123.5 . . ? S2A C9A H9A 123.5 . . ? C9A C10A C11A 110.7(13) . . ? C9A C10A H10A 124.7 . . ? C11A C10A H10A 124.7 . . ? C12A C11A C10A 111.4(12) . . ? C12A C11A H11A 124.3 . . ? C10A C11A H11A 124.3 . . ? C11A C12A C13 126.8(8) . . ? C11A C12A S2A 113.1(8) . . ? C13 C12A S2A 120.1(5) . . ? C12B C11B C10B 117(3) . . ? C12B C11B H11B 121.3 . . ? C10B C11B H11B 121.3 . . ? C9B C10B C11B 108(3) . . ? C9B C10B H10B 125.9 . . ? C11B C10B H10B 125.9 . . ? C10B C9B S2B 111(3) . . ? C10B C9B H9B 124.4 . . ? S2B C9B H9B 124.4 . . ? C12B S2B C9B 95.8(13) . . ? C11B C12B C13 124.9(16) . . ? C11B C12B S2B 107.3(15) . . ? C13 C12B S2B 127.8(11) . . ? O3 C13 C14 123.6(5) . . ? O3 C13 C12A 117.7(5) . . ? C14 C13 C12A 118.7(5) . . ? O3 C13 C12B 117.1(7) . . ? C14 C13 C12B 119.3(8) . . ? C15 C14 C13 122.1(5) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? O4 C15 C14 130.2(5) . . ? O4 C15 C16 114.3(5) . . ? C14 C15 C16 115.5(5) . . ? F5 C16 F4 107.1(5) . . ? F5 C16 F6 107.9(6) . . ? F4 C16 F6 105.9(5) . . ? F5 C16 C15 114.4(5) . . ? F4 C16 C15 111.8(5) . . ? F6 C16 C15 109.4(5) . . ? C18 C17 S3 113.8(5) . . ? C18 C17 H17 123.1 . . ? S3 C17 H17 123.1 . . ? C17 C18 C19 113.6(5) . . ? C17 C18 H18 123.2 . . ? C19 C18 H18 123.2 . . ? C18 C19 C20 108.5(5) . . ? C18 C19 H19 125.7 . . ? C20 C19 H19 125.7 . . ? C19 C20 C21 129.4(4) . . ? C19 C20 S3 112.2(4) . . ? C21 C20 S3 118.5(4) . . ? O5 C21 C22 124.3(5) . . ? O5 C21 C20 117.8(4) . . ? C22 C21 C20 117.8(4) . . ? C23 C22 C21 123.1(5) . . ? C23 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? O6 C23 C22 129.6(4) . . ? O6 C23 C24 112.9(5) . . ? C22 C23 C24 117.4(5) . . ? F8 C24 F9 108.2(4) . . ? F8 C24 F7 106.8(4) . . ? F9 C24 F7 106.6(5) . . ? F8 C24 C23 113.8(5) . . ? F9 C24 C23 110.5(4) . . ? F7 C24 C23 110.6(4) . . ? C26 C25 S4 113.1(4) . . ? C26 C25 H25 123.4 . . ? S4 C25 H25 123.4 . . ? C25 C26 C27 112.0(5) . . ? C25 C26 H26 124.0 . . ? C27 C26 H26 124.0 . . ? C28 C27 C26 112.2(5) . . ? C28 C27 H27 123.9 . . ? C26 C27 H27 123.9 . . ? C27 C28 C29 130.2(5) . . ? C27 C28 S4 111.3(4) . . ? C29 C28 S4 118.5(4) . . ? O7 C29 C30 124.2(4) . . ? O7 C29 C28 117.6(4) . . ? C30 C29 C28 118.2(5) . . ? C31 C30 C29 122.0(5) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? O8 C31 C30 130.3(5) . . ? O8 C31 C32 112.5(4) . . ? C30 C31 C32 117.3(5) . . ? F12 C32 F10 103.6(7) . . ? F12 C32 F11 106.9(6) . . ? F10 C32 F11 107.5(7) . . ? F12 C32 C31 112.3(6) . . ? F10 C32 C31 110.5(5) . . ? F11 C32 C31 115.3(5) . . ? N1 C33 H33A 109.5 . . ? N1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N2 C34 N1 108.0(5) . . ? N2 C34 H34 126.0 . . ? N1 C34 H34 126.0 . . ? C36 C35 N2 106.2(5) . . ? C36 C35 H35 126.9 . . ? N2 C35 H35 126.9 . . ? C35 C36 N1 106.9(5) . . ? C35 C36 H36 126.6 . . ? N1 C36 H36 126.6 . . ? N2 C37 C38 113.3(4) . . ? N2 C37 H37A 108.9 . . ? C38 C37 H37A 108.9 . . ? N2 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? C37 C38 C39 110.7(4) . . ? C37 C38 H38A 109.5 . . ? C39 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C38 C39 C40 112.4(5) . . ? C38 C39 H39A 109.1 . . ? C40 C39 H39A 109.1 . . ? C38 C39 H39B 109.1 . . ? C40 C39 H39B 109.1 . . ? H39A C39 H39B 107.9 . . ? C39 C40 C41 112.6(5) . . ? C39 C40 H40A 109.1 . . ? C41 C40 H40A 109.1 . . ? C39 C40 H40B 109.1 . . ? C41 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? C40 C41 C42 112.6(8) . . ? C40 C41 H41A 109.1 . . ? C42 C41 H41A 109.1 . . ? C40 C41 H41B 109.1 . . ? C42 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 S5 113.8(5) . . ? C44 C43 H43 123.1 . . ? S5 C43 H43 123.1 . . ? C43 C44 C45 114.5(5) . . ? C43 C44 H44 122.8 . . ? C45 C44 H44 122.8 . . ? C44 C45 C46 108.3(5) . . ? C44 C45 H45 125.8 . . ? C46 C45 H45 125.8 . . ? C45 C46 C47 130.6(5) . . ? C45 C46 S5 111.3(3) . . ? C47 C46 S5 118.2(4) . . ? O9 C47 C48 124.0(4) . . ? O9 C47 C46 117.6(5) . . ? C48 C47 C46 118.3(4) . . ? C49 C48 C47 121.5(5) . . ? C49 C48 H48 119.3 . . ? C47 C48 H48 119.3 . . ? O10 C49 C48 128.9(5) . . ? O10 C49 C50 113.6(4) . . ? C48 C49 C50 117.4(4) . . ? F13 C50 F14 108.3(4) . . ? F13 C50 F15 106.3(4) . . ? F14 C50 F15 106.1(5) . . ? F13 C50 C49 110.6(4) . . ? F14 C50 C49 114.7(4) . . ? F15 C50 C49 110.5(4) . . ? C54A S6A C51A 91.9(4) . . ? C52A C51A S6A 113.3(7) . . ? C52A C51A H51A 123.4 . . ? S6A C51A H51A 123.4 . . ? C51A C52A C53A 109.6(10) . . ? C51A C52A H52A 125.2 . . ? C53A C52A H52A 125.2 . . ? C54A C53A C52A 113.4(10) . . ? C54A C53A H53A 123.3 . . ? C52A C53A H53A 123.3 . . ? C53A C54A C55 129.8(7) . . ? C53A C54A S6A 111.9(6) . . ? C55 C54A S6A 118.3(5) . . ? C54B C53B C52B 118(3) . . ? C54B C53B H53B 121.2 . . ? C52B C53B H53B 121.2 . . ? C51B C52B C53B 102(3) . . ? C51B C52B H52B 129.0 . . ? C53B C52B H52B 129.0 . . ? C52B C51B S6B 120(3) . . ? C52B C51B H51B 120.2 . . ? S6B C51B H51B 120.2 . . ? C54B S6B C51B 89.0(15) . . ? C53B C54B C55 121.0(17) . . ? C53B C54B S6B 111.8(17) . . ? C55 C54B S6B 127.2(12) . . ? O11 C55 C56 124.5(4) . . ? O11 C55 C54B 117.5(8) . . ? C56 C55 C54B 118.0(8) . . ? O11 C55 C54A 116.5(5) . . ? C56 C55 C54A 119.0(5) . . ? C57 C56 C55 122.6(5) . . ? C57 C56 H56 118.7 . . ? C55 C56 H56 118.7 . . ? O12 C57 C56 130.6(5) . . ? O12 C57 C58 112.6(4) . . ? C56 C57 C58 116.8(5) . . ? F16 C58 F17 107.0(4) . . ? F16 C58 F18 106.6(4) . . ? F17 C58 F18 106.2(5) . . ? F16 C58 C57 111.0(5) . . ? F17 C58 C57 114.9(4) . . ? F18 C58 C57 110.6(4) . . ? C60 C59 S7 111.8(5) . . ? C60 C59 H59 124.1 . . ? S7 C59 H59 124.1 . . ? C59 C60 C61 113.5(5) . . ? C59 C60 H60 123.2 . . ? C61 C60 H60 123.2 . . ? C62 C61 C60 111.5(5) . . ? C62 C61 H61 124.3 . . ? C60 C61 H61 124.3 . . ? C61 C62 C63 130.5(5) . . ? C61 C62 S7 111.4(4) . . ? C63 C62 S7 118.1(4) . . ? O13 C63 C64 123.9(5) . . ? O13 C63 C62 117.1(5) . . ? C64 C63 C62 119.0(4) . . ? C65 C64 C63 123.2(4) . . ? C65 C64 H64 118.4 . . ? C63 C64 H64 118.4 . . ? O14 C65 C64 130.2(5) . . ? O14 C65 C66 111.9(5) . . ? C64 C65 C66 117.9(5) . . ? F21 C66 F20 108.6(6) . . ? F21 C66 F19 105.2(7) . . ? F20 C66 F19 104.8(5) . . ? F21 C66 C65 112.6(5) . . ? F20 C66 C65 114.9(5) . . ? F19 C66 C65 110.1(5) . . ? C70A S8A C67A 91.8(3) . . ? C68A C67A S8A 112.2(5) . . ? C68A C67A H67A 123.9 . . ? S8A C67A H67A 123.9 . . ? C67A C68A C69A 111.7(6) . . ? C67A C68A H68A 124.1 . . ? C69A C68A H68A 124.1 . . ? C70A C69A C68A 112.6(6) . . ? C70A C69A H69A 123.7 . . ? C68A C69A H69A 123.7 . . ? C69A C70A C71 129.1(6) . . ? C69A C70A S8A 111.7(4) . . ? C71 C70A S8A 119.1(4) . . ? C70B C69B C68B 113.0(10) . . ? C70B C69B H69B 123.5 . . ? C68B C69B H69B 123.5 . . ? C67B C68B C69B 108.9(10) . . ? C67B C68B H68B 125.0 . . ? C69B C68B H68B 127.0 . . ? C68B C67B S8B 113.3(9) . . ? C68B C67B H67B 123.4 . . ? S8B C67B H67B 123.4 . . ? C70B S8B C67B 91.7(7) . . ? C69B C70B C71 122.0(17) . . ? C69B C70B S8B 113.2(9) . . ? C71 C70B S8B 124.7(15) . . ? O15 C71 C72 123.8(4) . . ? O15 C71 C70B 117.8(10) . . ? C72 C71 C70B 118.3(10) . . ? O15 C71 C70A 116.2(5) . . ? C72 C71 C70A 120.0(5) . . ? C73 C72 C71 120.9(5) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? O16 C73 C72 128.6(5) . . ? O16 C73 C74 112.9(4) . . ? C72 C73 C74 118.5(5) . . ? F22 C74 F23 106.8(5) . . ? F22 C74 F24 106.3(5) . . ? F23 C74 F24 107.1(4) . . ? F22 C74 C73 110.9(4) . . ? F23 C74 C73 113.8(4) . . ? F24 C74 C73 111.4(5) . . ? N3 C75 H75A 109.5 . . ? N3 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N3 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N4 C76 N3 108.6(4) . . ? N4 C76 H76 125.7 . . ? N3 C76 H76 125.7 . . ? C78 C77 N4 106.3(4) . . ? C78 C77 H77 126.8 . . ? N4 C77 H77 126.8 . . ? C77 C78 N3 108.2(4) . . ? C77 C78 H78 125.9 . . ? N3 C78 H78 125.9 . . ? N4 C79 C80 111.2(4) . . ? N4 C79 H79A 109.4 . . ? C80 C79 H79A 109.4 . . ? N4 C79 H79B 109.4 . . ? C80 C79 H79B 109.4 . . ? H79A C79 H79B 108.0 . . ? C79 C80 C81 112.2(4) . . ? C79 C80 H80A 109.2 . . ? C81 C80 H80A 109.2 . . ? C79 C80 H80B 109.2 . . ? C81 C80 H80B 109.2 . . ? H80A C80 H80B 107.9 . . ? C80 C81 C82 112.4(5) . . ? C80 C81 H81A 109.1 . . ? C82 C81 H81A 109.1 . . ? C80 C81 H81B 109.1 . . ? C82 C81 H81B 109.1 . . ? H81A C81 H81B 107.9 . . ? C83 C82 C81 113.2(5) . . ? C83 C82 H82A 108.9 . . ? C81 C82 H82A 108.9 . . ? C83 C82 H82B 108.9 . . ? C81 C82 H82B 108.9 . . ? H82A C82 H82B 107.8 . . ? C84 C83 C82 112.1(5) . . ? C84 C83 H83A 109.2 . . ? C82 C83 H83A 109.2 . . ? C84 C83 H83B 109.2 . . ? C82 C83 H83B 109.2 . . ? H83A C83 H83B 107.9 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C34 N1 C36 109.3(4) . . ? C34 N1 C33 126.3(5) . . ? C36 N1 C33 124.3(5) . . ? C34 N2 C35 109.6(5) . . ? C34 N2 C37 126.3(5) . . ? C35 N2 C37 124.0(4) . . ? C76 N3 C78 108.1(4) . . ? C76 N3 C75 125.8(4) . . ? C78 N3 C75 126.2(4) . . ? C76 N4 C77 108.8(4) . . ? C76 N4 C79 125.9(4) . . ? C77 N4 C79 125.1(4) . . ? C5 O1 Yb1 132.1(3) . . ? C7 O2 Yb1 127.2(3) . . ? C13 O3 Yb1 134.4(3) . . ? C15 O4 Yb1 129.8(3) . . ? C21 O5 Yb1 133.9(3) . . ? C23 O6 Yb1 129.6(3) . . ? C29 O7 Yb1 136.4(3) . . ? C31 O8 Yb1 131.9(3) . . ? C47 O9 Yb2 136.0(3) . . ? C49 O10 Yb2 132.6(3) . . ? C55 O11 Yb2 134.2(3) . . ? C57 O12 Yb2 129.6(3) . . ? C63 O13 Yb2 135.2(3) . . ? C65 O14 Yb2 131.4(4) . . ? C71 O15 Yb2 136.9(3) . . ? C73 O16 Yb2 130.5(3) . . ? C1 S1 C4 92.2(3) . . ? C17 S3 C20 91.9(3) . . ? C25 S4 C28 91.3(3) . . ? C43 S5 C46 92.2(3) . . ? C59 S7 C62 91.8(3) . . ? O1 Yb1 O5 108.83(12) . . ? O1 Yb1 O6 145.15(12) . . ? O5 Yb1 O6 76.73(12) . . ? O1 Yb1 O3 80.40(12) . . ? O5 Yb1 O3 141.72(12) . . ? O6 Yb1 O3 76.04(13) . . ? O1 Yb1 O4 71.76(12) . . ? O5 Yb1 O4 73.36(13) . . ? O6 Yb1 O4 77.50(12) . . ? O3 Yb1 O4 74.86(13) . . ? O1 Yb1 O7 144.09(11) . . ? O5 Yb1 O7 80.65(12) . . ? O6 Yb1 O7 70.15(12) . . ? O3 Yb1 O7 114.07(12) . . ? O4 Yb1 O7 142.27(12) . . ? O1 Yb1 O2 76.04(11) . . ? O5 Yb1 O2 147.31(12) . . ? O6 Yb1 O2 118.38(12) . . ? O3 Yb1 O2 70.54(12) . . ? O4 Yb1 O2 135.80(13) . . ? O7 Yb1 O2 78.45(12) . . ? O1 Yb1 O8 75.18(12) . . ? O5 Yb1 O8 74.24(12) . . ? O6 Yb1 O8 137.06(13) . . ? O3 Yb1 O8 142.43(12) . . ? O4 Yb1 O8 122.06(12) . . ? O7 Yb1 O8 74.44(12) . . ? O2 Yb1 O8 76.09(12) . . ? O10 Yb2 O9 74.15(12) . . ? O10 Yb2 O16 79.44(13) . . ? O9 Yb2 O16 75.86(11) . . ? O10 Yb2 O15 83.78(13) . . ? O9 Yb2 O15 144.40(12) . . ? O16 Yb2 O15 72.83(12) . . ? O10 Yb2 O14 74.39(12) . . ? O9 Yb2 O14 122.29(11) . . ? O16 Yb2 O14 141.05(13) . . ? O15 Yb2 O14 76.07(12) . . ? O10 Yb2 O11 109.84(12) . . ? O9 Yb2 O11 74.66(12) . . ? O16 Yb2 O11 144.96(12) . . ? O15 Yb2 O11 140.20(12) . . ? O14 Yb2 O11 72.40(12) . . ? O10 Yb2 O13 144.99(12) . . ? O9 Yb2 O13 138.88(13) . . ? O16 Yb2 O13 114.61(12) . . ? O15 Yb2 O13 71.47(13) . . ? O14 Yb2 O13 75.84(13) . . ? O11 Yb2 O13 77.71(12) . . ? O10 Yb2 O12 144.93(12) . . ? O9 Yb2 O12 74.50(12) . . ? O16 Yb2 O12 78.03(13) . . ? O15 Yb2 O12 114.28(13) . . ? O14 Yb2 O12 137.28(13) . . ? O11 Yb2 O12 76.19(12) . . ? O13 Yb2 O12 69.70(12) . . ? C85 O17 H17A 109.5 . . ? O17 C85 H85A 109.5 . . ? O17 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? O17 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 67.25 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.169 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.153