# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Nathaniel Rosi' _publ_contact_author_email NROSI@PITT.EDU _publ_section_title ; Near-infrared Emitting Ytterbium Metal-organic Frameworks with Tunable Excitation Properties ; loop_ _publ_author_name 'Nathaniel Rosi' 'Demetra A Chengelis-Czegan' 'Steven J Geib' 'Stephane Petoud' 'Jessica Szakos' ; K.A.White ; 'Matthias Zeller' # Attachment 'yb-pvdc-1.cif' data_Yb-PVDC-1 _database_code_depnum_ccdc_archive 'CCDC 698331' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common Yb-PVDC-1 _chemical_formula_moiety ? _chemical_formula_sum 'C39 H30 O10 Yb' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour yellow _diffrn_ambient_temperature 253(2) _chemical_formula_weight 831.67 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d d' _symmetry_int_tables_number 70 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 16.247(6) _cell_length_b 48.939(19) _cell_length_c 80.84(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 64280(43) _cell_formula_units_Z 32 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 2950 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 13.85 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13248 _exptl_absorpt_coefficient_mu 1.189 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7021 _exptl_absorpt_correction_T_max 0.7883 _exptl_absorpt_process_details 'Bruker Sadabs' _exptl_special_details ; An X-ray crystal structure was determined for C39H30O10Yb, Yb-PVDC-1, using a single crystal on a Bruker Smart Apex CCD diffractometer with graphite-monochromated MoKalpha (lambda= 0.71073 \%A) radiation. The parameters used during the collection of diffraction data are summarized in Table S1. The crystal was mounted in a glass capillary and placed in a cold N2 stream (253 K) for data collection. Unit-cell parameters and systematic absences indicated Yb-PVDC-1 crystallized in orthorhombic F ddd. Unit-cell dimensions were derived from the least-squares fit of the angular settings of 2973 reflections. Data were corrected for absorption using the Bruker program Sadabs. The crystal was very weakly diffracting with no observed intensities beyond 2?=46\%. The structure was solved via direct methods, which located Yb3+ and some of the remaining non-hydrogen atoms. Remaining non-hydrogen atoms were gradually found from several subsequent difference Fourier syntheses. All non-hydrogen atoms were refined anisotropically, although C(10) required an isotropic restraint (SHELXTL ISOR command) to avoid going non-positive definite. Idealized atom positions were calculated for all hydrogen atoms (d-(Cmethyl-H) = 0.96 \%A, d-Cphenyl-H)=0.93 \%A, U = 1.2Uiso of attached carbon). Calculations from Platon indicated solvent accessible voids accounting for 64.5% of the unit-cell volume (eight voids measuring 5175 \%A3 with 790 electrons each). We were unable to identify or model specific solvent molecules within the voids. The diffuse electron density was treated with the SQUEEZE routine from the PLATON software package. The large voids in the structure allow for considerable flexing and uncertainty in the positions of the framework atoms and this is evidenced in large atomic displacement parameters for many of the benzene carbons and a large number of atypical bond lengths and angles. It was necessary to constrain or restrain a number of bond lengths and angles in the structure in order get a stable refinement and chemically reasonable model. Phenyl rings were fit to rigid hexagons (dC-C = 1.39 \%A). For the linker phenyl ring located on the inversion center all 1,1 and 1,2 C-C distances were constrained (1.39 \%A for 1,1; 2.408 \%A for 1,2 distances); the symmetry operator was used to do this across the inversion center. Cphenyl-O distances were constrained to 1.36 \%A and O-Cmethyl distances at 1.42 \%A. Ethylene C=C distances were fixed at 1.31 \%A. All carbon and oxygen atoms were restrained to have similar ADP's as their neighbors (SIMU and DELU restraints with a standard deviation of 0.03 each). Chemically equivalent 1,1 and 1,2 C-C distances to the ethylene carbon atoms in all units were restrained to be the same within a standard deviation of 0.02 \%A. Numerous checkcif alerts are generated for high Rint values, unusual atomic displacement parameters. These are attributable to the uncertainty in the atomic positions and the low percentage of observed diffraction intensities. There is also a checkcif alert regarding the very large voids. The final Fourier map showed maximum and minimum peaks of 0.52 and -0.37 e-\%A-3, respectively, which were close to Yb(1). All computer programs used in the data collection and refinements are contained in the Bruker program packages SMART (vers. 5.625), SAINT (vers. 6.22), and SHELXTL (vers. 6.14) and Platon.[4] ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95070 _diffrn_reflns_av_R_equivalents 0.1522 _diffrn_reflns_av_sigmaI/netI 0.1168 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -89 _diffrn_reflns_limit_l_max 87 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 23.25 _reflns_number_total 11506 _reflns_number_gt 4841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^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 11506 _refine_ls_number_parameters 404 _refine_ls_number_restraints 455 _refine_ls_R_factor_all 0.1599 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.030 _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 Yb1 Yb -0.1250 0.8750 0.630321(5) 0.0880(2) Uani 1 2 d S . . Yb2 Yb 0.1250 0.909695(11) 0.6250 0.1100(3) Uani 1 2 d S . . O1 O 0.1476(4) 0.87457(14) 0.60858(6) 0.119(2) Uani 1 1 d U . . O2 O 0.2604(4) 0.85173(11) 0.61354(7) 0.1048(18) Uani 1 1 d U . . O3 O -0.0446(4) 0.67645(13) 0.39556(8) 0.138(2) Uani 1 1 d U . . O4 O 0.0706(4) 0.65251(13) 0.39859(6) 0.114(2) Uani 1 1 d U . . O5 O 0.2377(9) 0.7268(3) 0.52651(13) 0.351(7) Uani 1 1 d DU . . O6 O -0.0155(10) 0.7736(3) 0.48978(14) 0.335(7) Uani 1 1 d DU . . O7 O -0.1236(6) 0.90457(14) 0.60877(7) 0.146(3) Uani 1 1 d U . . O8 O 0.0030(5) 0.90563(18) 0.61164(7) 0.187(4) Uani 1 1 d U . . O9 O 0.1134(9) 0.9555(3) 0.50417(15) 0.294(6) Uani 1 1 d U . . O10 O 0.0770(7) 0.9564(2) 0.61628(14) 0.313(6) Uani 1 1 d . . . C1 C 0.1953(7) 0.8554(2) 0.60563(10) 0.102(3) Uani 1 1 d U . . C2 C 0.1757(4) 0.83639(13) 0.59204(6) 0.112(3) Uani 1 1 d GU . . C3 C 0.1025(4) 0.84064(13) 0.58350(8) 0.144(4) Uani 1 1 d GU . . H3A H 0.0660 0.8541 0.5870 0.172 Uiso 1 1 calc R . . C4 C 0.0840(4) 0.82482(15) 0.56971(8) 0.169(4) Uani 1 1 d GDU . . H4A H 0.0351 0.8277 0.5640 0.203 Uiso 1 1 calc R . . C5 C 0.1386(4) 0.80475(14) 0.56447(7) 0.169(4) Uani 1 1 d GU . . C6 C 0.2118(4) 0.80050(13) 0.57300(9) 0.171(4) Uani 1 1 d GDU . . H6A H 0.2483 0.7871 0.5695 0.206 Uiso 1 1 calc R . . C7 C 0.2303(4) 0.81631(15) 0.58679(8) 0.143(4) Uani 1 1 d GU . . H7A H 0.2792 0.8135 0.5925 0.172 Uiso 1 1 calc R . . C8 C 0.1204(7) 0.7906(3) 0.54903(15) 0.217(5) Uani 1 1 d DU . . H8A H 0.0686 0.7953 0.5451 0.261 Uiso 1 1 calc R . . C9 C 0.1567(8) 0.7731(3) 0.53920(15) 0.275(7) Uani 1 1 d DU . . H9A H 0.2086 0.7674 0.5426 0.330 Uiso 1 1 calc R . . C10 C 0.1282(6) 0.76140(17) 0.52379(9) 0.283(7) Uani 1 1 d GDU . . C11 C 0.1692(6) 0.73920(19) 0.51694(10) 0.292(7) Uani 1 1 d GDU . . C12 C 0.1446(6) 0.72885(17) 0.50171(10) 0.245(6) Uani 1 1 d GDU . . H12A H 0.1721 0.7140 0.4971 0.294 Uiso 1 1 calc R . . C13 C 0.0790(6) 0.7407(2) 0.49334(9) 0.258(6) Uani 1 1 d GDU . . C14 C 0.0379(6) 0.7629(2) 0.50019(11) 0.288(7) Uani 1 1 d GDU . . C15 C 0.0625(6) 0.77325(19) 0.51542(11) 0.274(7) Uani 1 1 d GDU . . H15A H 0.0351 0.7881 0.5200 0.329 Uiso 1 1 calc R . . C16 C 0.0552(9) 0.7317(3) 0.47692(15) 0.254(6) Uani 1 1 d DU . . H16A H 0.0145 0.7422 0.4719 0.305 Uiso 1 1 calc R . . C17 C 0.0820(9) 0.7112(3) 0.46807(16) 0.281(7) Uani 1 1 d DU . . H17A H 0.1227 0.7009 0.4733 0.337 Uiso 1 1 calc R . . C18 C 0.0608(5) 0.70149(17) 0.45203(7) 0.222(6) Uani 1 1 d GDU . . C19 C 0.0020(5) 0.71405(15) 0.44210(10) 0.239(6) Uani 1 1 d GDU . . H19A H -0.0264 0.7292 0.4460 0.286 Uiso 1 1 calc R . . C20 C -0.0141(4) 0.70391(17) 0.42638(9) 0.203(5) Uani 1 1 d GU . . H20A H -0.0534 0.7123 0.4197 0.243 Uiso 1 1 calc R . . C21 C 0.0284(5) 0.68121(17) 0.42058(7) 0.143(4) Uani 1 1 d GU . . C22 C 0.0872(5) 0.66865(14) 0.43050(9) 0.169(4) Uani 1 1 d GU . . H22A H 0.1156 0.6535 0.4266 0.202 Uiso 1 1 calc R . . C23 C 0.1033(5) 0.67879(16) 0.44623(8) 0.217(5) Uani 1 1 d GDU . . H23A H 0.1426 0.6704 0.4529 0.261 Uiso 1 1 calc R . . C24 C 0.0183(7) 0.6690(2) 0.40360(11) 0.120(3) Uani 1 1 d U . . C25 C -0.0561(9) 0.9111(3) 0.60352(12) 0.133(4) Uani 1 1 d U . . C26 C -0.0491(5) 0.92507(14) 0.58779(6) 0.120(3) Uani 1 1 d GU . . C27 C -0.1202(4) 0.93710(16) 0.58160(8) 0.153(4) Uani 1 1 d GU . . H27A H -0.1691 0.9360 0.5876 0.183 Uiso 1 1 calc R . . C28 C -0.1183(4) 0.95069(16) 0.56651(8) 0.192(5) Uani 1 1 d GDU . . H28A H -0.1659 0.9587 0.5624 0.231 Uiso 1 1 calc R . . C29 C -0.0452(4) 0.95225(16) 0.55760(7) 0.194(5) Uani 1 1 d GDU . . C30 C 0.0259(4) 0.94023(18) 0.56380(8) 0.207(5) Uani 1 1 d GDU . . H30A H 0.0747 0.9413 0.5578 0.249 Uiso 1 1 calc R . . C31 C 0.0240(4) 0.92664(16) 0.57889(8) 0.188(5) Uani 1 1 d GU . . H31A H 0.0715 0.9186 0.5830 0.226 Uiso 1 1 calc R . . C32 C -0.0466(6) 0.9672(3) 0.54126(14) 0.224(6) Uani 1 1 d DU . . H32A H -0.0964 0.9755 0.5387 0.269 Uiso 1 1 calc R . . C33 C 0.0115(8) 0.9702(3) 0.53022(13) 0.250(6) Uani 1 1 d DU . . H33A H 0.0629 0.9628 0.5325 0.300 Uiso 1 1 calc R . . C34 C 0.0010(8) 0.9848(3) 0.51432(11) 0.223(6) Uani 1 1 d DU . . C35 C -0.0537(7) 1.0067(2) 0.51318(10) 0.223(6) Uani 1 1 d DU . . H35A H -0.0880 1.0113 0.5220 0.268 Uiso 1 1 calc R . . C36 C 0.0552(9) 0.9787(3) 0.50153(13) 0.247(6) Uani 1 1 d DU . . C37 C 0.2631(12) 0.7026(3) 0.5148(3) 0.425(14) Uani 1 1 d DU . . H37A H 0.3086 0.6929 0.5196 0.637 Uiso 1 1 calc R . . H37B H 0.2790 0.7097 0.5042 0.637 Uiso 1 1 calc R . . H37C H 0.2173 0.6904 0.5135 0.637 Uiso 1 1 calc R . . C38 C 0.1665(12) 0.9551(5) 0.4883(2) 0.373(12) Uani 1 1 d U . . H38A H 0.2061 0.9406 0.4890 0.560 Uiso 1 1 calc R . . H38B H 0.1947 0.9723 0.4872 0.560 Uiso 1 1 calc R . . H38C H 0.1318 0.9523 0.4789 0.560 Uiso 1 1 calc R . . C39 C -0.0508(13) 0.7990(3) 0.5010(3) 0.377(12) Uani 1 1 d DU . . H39A H -0.0923 0.8087 0.4949 0.566 Uiso 1 1 calc R . . H39B H -0.0065 0.8112 0.5036 0.566 Uiso 1 1 calc R . . H39C H -0.0742 0.7920 0.5110 0.566 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.1193(4) 0.0996(4) 0.0451(3) 0.000 0.000 -0.0023(4) Yb2 0.1508(6) 0.0980(5) 0.0812(4) 0.000 0.0378(4) 0.000 O1 0.122(5) 0.147(6) 0.089(4) -0.035(4) -0.002(4) 0.018(5) O2 0.121(5) 0.122(5) 0.072(4) -0.028(3) -0.007(3) 0.011(4) O3 0.138(6) 0.145(6) 0.131(5) -0.064(4) -0.045(4) 0.039(5) O4 0.133(5) 0.151(6) 0.058(3) -0.026(3) -0.008(3) 0.029(4) O5 0.507(19) 0.396(16) 0.149(8) -0.034(9) -0.068(10) -0.055(13) O6 0.440(18) 0.382(16) 0.184(10) -0.130(10) -0.012(10) -0.047(12) O7 0.231(8) 0.143(5) 0.065(4) 0.019(4) 0.038(5) -0.003(6) O8 0.211(8) 0.293(9) 0.056(4) 0.029(5) -0.008(4) 0.131(7) O9 0.339(15) 0.331(15) 0.211(9) 0.098(10) -0.039(10) -0.021(11) O10 0.329(15) 0.273(12) 0.339(17) -0.002(10) 0.017(11) 0.026(10) C1 0.099(8) 0.137(8) 0.070(6) -0.030(6) -0.011(5) 0.000(7) C2 0.124(7) 0.136(8) 0.078(6) -0.040(5) -0.003(5) -0.004(6) C3 0.152(9) 0.194(10) 0.084(6) -0.055(6) -0.022(6) -0.005(7) C4 0.168(9) 0.207(11) 0.132(8) -0.085(8) -0.024(7) -0.010(8) C5 0.181(11) 0.208(11) 0.119(8) -0.068(7) -0.017(8) -0.053(9) C6 0.206(11) 0.157(9) 0.151(9) -0.090(8) 0.024(8) 0.008(8) C7 0.160(9) 0.151(9) 0.119(7) -0.069(6) -0.024(7) 0.018(7) C8 0.249(12) 0.239(14) 0.163(10) -0.066(9) 0.066(10) -0.083(11) C9 0.378(17) 0.285(17) 0.162(12) -0.037(10) 0.009(12) -0.066(14) C10 0.404(17) 0.340(16) 0.105(9) -0.049(10) -0.049(11) -0.130(12) C11 0.412(18) 0.300(15) 0.164(12) 0.005(11) -0.043(12) -0.102(12) C12 0.345(16) 0.311(14) 0.080(8) -0.062(9) -0.007(9) -0.173(11) C13 0.350(16) 0.310(15) 0.113(9) -0.085(10) -0.044(9) -0.125(11) C14 0.382(18) 0.320(16) 0.161(12) -0.122(12) -0.038(11) -0.069(12) C15 0.375(17) 0.337(16) 0.110(9) -0.085(11) 0.000(10) -0.151(12) C16 0.350(15) 0.277(16) 0.135(10) -0.074(9) 0.038(11) -0.113(13) C17 0.325(15) 0.357(18) 0.161(11) -0.081(11) 0.045(11) -0.135(14) C18 0.205(12) 0.349(15) 0.111(8) -0.121(9) -0.009(8) -0.094(11) C19 0.190(12) 0.348(14) 0.178(11) -0.188(11) 0.009(8) -0.031(10) C20 0.143(9) 0.281(13) 0.184(10) -0.149(9) -0.018(8) 0.026(9) C21 0.124(8) 0.203(10) 0.103(7) -0.076(7) -0.021(6) 0.015(7) C22 0.195(10) 0.229(11) 0.082(7) -0.056(7) -0.025(7) -0.005(8) C23 0.242(12) 0.293(15) 0.117(8) -0.049(9) -0.016(9) -0.038(11) C24 0.114(8) 0.158(9) 0.086(6) -0.043(6) -0.025(6) 0.023(7) C25 0.173(11) 0.158(9) 0.068(7) 0.024(6) 0.021(7) 0.057(9) C26 0.126(8) 0.169(8) 0.065(5) 0.046(5) 0.004(5) 0.019(7) C27 0.153(8) 0.209(10) 0.096(6) 0.067(6) 0.007(7) 0.004(8) C28 0.185(10) 0.264(12) 0.128(8) 0.088(8) 0.005(8) -0.002(10) C29 0.213(11) 0.267(11) 0.102(7) 0.114(8) -0.058(7) -0.066(10) C30 0.149(9) 0.374(15) 0.098(8) 0.088(9) 0.005(7) -0.032(10) C31 0.142(9) 0.333(13) 0.090(7) 0.072(8) -0.004(6) -0.015(10) C32 0.254(13) 0.273(13) 0.145(10) 0.096(10) -0.042(9) -0.111(11) C33 0.322(16) 0.290(14) 0.138(11) 0.086(10) -0.023(10) -0.095(13) C34 0.308(15) 0.230(14) 0.130(10) 0.121(9) -0.075(9) -0.080(11) C35 0.339(17) 0.229(15) 0.103(8) 0.109(9) -0.068(9) -0.107(11) C36 0.265(16) 0.297(17) 0.179(13) 0.090(13) -0.027(11) -0.042(12) C37 0.66(3) 0.165(15) 0.45(3) -0.126(16) 0.27(3) -0.016(18) C38 0.34(2) 0.58(3) 0.198(16) -0.08(2) 0.099(15) -0.03(2) C39 0.41(2) 0.26(2) 0.46(3) -0.073(19) 0.19(2) -0.006(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O4 2.185(6) 20_566 ? Yb1 O4 2.185(6) 31_566 ? Yb1 O2 2.239(6) 11_455 ? Yb1 O2 2.239(6) 12_465 ? Yb1 O7 2.265(6) 2_465 ? Yb1 O7 2.265(6) . ? Yb1 O8 2.975(9) 2_465 ? Yb1 O8 2.975(9) . ? Yb2 O1 2.202(6) 11_455 ? Yb2 O1 2.203(6) . ? Yb2 O8 2.266(9) 11_455 ? Yb2 O8 2.266(8) . ? Yb2 O3 2.267(6) 18_666 ? Yb2 O3 2.267(6) 20_566 ? Yb2 O10 2.517(12) . ? Yb2 O10 2.517(12) 11_455 ? O1 C1 1.239(10) . ? O2 C1 1.249(9) . ? O2 Yb1 2.239(6) 11_455 ? O3 C24 1.265(10) . ? O3 Yb2 2.267(6) 30_556 ? O4 C24 1.241(10) . ? O4 Yb1 2.185(6) 23_665 ? O5 C11 1.484(13) . ? O5 C37 1.571(15) . ? O6 C14 1.319(16) . ? O6 C39 1.642(14) . ? O7 C25 1.219(12) . ? O8 C25 1.195(12) . ? O9 C38 1.547(16) . ? O9 C36 1.494(14) . ? C1 C2 1.476(10) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C6 1.3900 . ? C5 C8 1.457(12) . ? C6 C7 1.3900 . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.3082(11) . ? C8 H8A 0.9300 . ? C9 C10 1.448(12) . ? C9 H9A 0.9300 . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 C16 1.450(11) . ? C14 C15 1.3900 . ? C15 H15A 0.9300 . ? C16 C17 1.3083(11) . ? C16 H16A 0.9300 . ? C17 C18 1.423(12) . ? C17 H17A 0.9300 . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C19 H19A 0.9300 . ? C20 C21 1.3900 . ? C20 H20A 0.9300 . ? C21 C22 1.3900 . ? C21 C24 1.506(10) . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.447(11) . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C27 H27A 0.9300 . ? C28 C29 1.3900 . ? C28 H28A 0.9300 . ? C29 C30 1.3900 . ? C29 C32 1.511(10) . ? C30 C31 1.3900 . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 C33 1.3086(11) . ? C32 H32A 0.9300 . ? C33 C34 1.479(11) . ? C33 H33A 0.9300 . ? C34 C35 1.394(8) . ? C34 C36 1.391(8) . ? C35 C36 1.389(8) 17_576 ? C35 H35A 0.9300 . ? C36 C35 1.389(8) 17_576 ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Yb1 O4 95.0(3) 20_566 31_566 ? O4 Yb1 O2 80.0(2) 20_566 11_455 ? O4 Yb1 O2 82.7(2) 31_566 11_455 ? O4 Yb1 O2 82.7(2) 20_566 12_465 ? O4 Yb1 O2 80.0(2) 31_566 12_465 ? O2 Yb1 O2 154.4(3) 11_455 12_465 ? O4 Yb1 O7 156.6(3) 20_566 2_465 ? O4 Yb1 O7 97.0(2) 31_566 2_465 ? O2 Yb1 O7 81.6(3) 11_455 2_465 ? O2 Yb1 O7 119.2(3) 12_465 2_465 ? O4 Yb1 O7 97.0(2) 20_566 . ? O4 Yb1 O7 156.6(3) 31_566 . ? O2 Yb1 O7 119.2(3) 11_455 . ? O2 Yb1 O7 81.6(3) 12_465 . ? O7 Yb1 O7 79.4(3) 2_465 . ? O4 Yb1 O8 159.4(2) 20_566 2_465 ? O4 Yb1 O8 75.5(2) 31_566 2_465 ? O2 Yb1 O8 116.0(2) 11_455 2_465 ? O2 Yb1 O8 77.7(2) 12_465 2_465 ? O7 Yb1 O8 44.0(2) 2_465 2_465 ? O7 Yb1 O8 86.5(3) . 2_465 ? O4 Yb1 O8 75.5(2) 20_566 . ? O4 Yb1 O8 159.4(2) 31_566 . ? O2 Yb1 O8 77.7(2) 11_455 . ? O2 Yb1 O8 116.0(2) 12_465 . ? O7 Yb1 O8 86.5(3) 2_465 . ? O7 Yb1 O8 44.0(2) . . ? O8 Yb1 O8 119.0(3) 2_465 . ? O1 Yb2 O1 77.4(3) 11_455 . ? O1 Yb2 O8 77.9(3) 11_455 11_455 ? O1 Yb2 O8 94.2(3) . 11_455 ? O1 Yb2 O8 94.2(3) 11_455 . ? O1 Yb2 O8 77.9(3) . . ? O8 Yb2 O8 169.9(4) 11_455 . ? O1 Yb2 O3 145.1(2) 11_455 18_666 ? O1 Yb2 O3 75.2(2) . 18_666 ? O8 Yb2 O3 82.9(2) 11_455 18_666 ? O8 Yb2 O3 100.7(2) . 18_666 ? O1 Yb2 O3 75.2(2) 11_455 20_566 ? O1 Yb2 O3 145.1(2) . 20_566 ? O8 Yb2 O3 100.7(2) 11_455 20_566 ? O8 Yb2 O3 82.9(2) . 20_566 ? O3 Yb2 O3 137.6(3) 18_666 20_566 ? O1 Yb2 O10 145.7(3) 11_455 . ? O1 Yb2 O10 126.3(3) . . ? O8 Yb2 O10 119.0(4) 11_455 . ? O8 Yb2 O10 71.0(3) . . ? O3 Yb2 O10 69.2(3) 18_666 . ? O3 Yb2 O10 72.4(3) 20_566 . ? O1 Yb2 O10 126.3(3) 11_455 11_455 ? O1 Yb2 O10 145.7(3) . 11_455 ? O8 Yb2 O10 71.1(4) 11_455 11_455 ? O8 Yb2 O10 119.0(3) . 11_455 ? O3 Yb2 O10 72.4(3) 18_666 11_455 ? O3 Yb2 O10 69.2(3) 20_566 11_455 ? O10 Yb2 O10 49.4(5) . 11_455 ? C1 O1 Yb2 144.1(6) . . ? C1 O2 Yb1 138.1(7) . 11_455 ? C24 O3 Yb2 137.6(6) . 30_556 ? C24 O4 Yb1 154.0(6) . 23_665 ? C11 O5 C37 101.1(9) . . ? C14 O6 C39 100.3(12) . . ? C25 O7 Yb1 116.5(8) . . ? C25 O8 Yb2 161.0(10) . . ? C25 O8 Yb1 80.3(8) . . ? Yb2 O8 Yb1 114.4(2) . . ? C38 O9 C36 104.0(12) . . ? O1 C1 O2 122.7(9) . . ? O1 C1 C2 119.1(9) . . ? O2 C1 C2 118.2(10) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 117.4(7) . . ? C7 C2 C1 122.4(7) . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 C8 117.9(4) . . ? C6 C5 C8 121.8(4) . . ? C7 C6 C5 120.0 . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? C9 C8 C5 137.7(11) . . ? C9 C8 H8A 111.1 . . ? C5 C8 H8A 111.2 . . ? C8 C9 C10 129.6(10) . . ? C8 C9 H9A 115.2 . . ? C10 C9 H9A 115.2 . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 119.9 . . ? C15 C10 C9 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 O5 121.9(7) . . ? C10 C11 O5 118.1(7) . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 C16 121.6(4) . . ? C14 C13 C16 118.3(4) . . ? O6 C14 C15 127.6(8) . . ? O6 C14 C13 111.9(8) . . ? C15 C14 C13 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 H15A 120.0 . . ? C10 C15 H15A 120.0 . . ? C17 C16 C13 130.1(10) . . ? C17 C16 H16A 114.9 . . ? C13 C16 H16A 114.9 . . ? C16 C17 C18 132.3(11) . . ? C16 C17 H17A 113.8 . . ? C18 C17 H17A 113.8 . . ? C19 C18 C23 120.0 . . ? C19 C18 C17 123.0(4) . . ? C23 C18 C17 116.9(4) . . ? C18 C19 C20 120.0 . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 C24 115.2(7) . . ? C20 C21 C24 124.7(7) . . ? C21 C22 C23 120.0 . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 H23A 120.0 . . ? C18 C23 H23A 120.0 . . ? O4 C24 O3 125.0(9) . . ? O4 C24 C21 118.7(9) . . ? O3 C24 C21 116.3(10) . . ? O8 C25 O7 118.2(11) . . ? O8 C25 C26 121.7(12) . . ? O7 C25 C26 120.1(11) . . ? C27 C26 C31 120.0 . . ? C27 C26 C25 116.8(7) . . ? C31 C26 C25 123.2(7) . . ? C26 C27 C28 120.0 . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 C32 122.2(4) . . ? C28 C29 C32 117.8(4) . . ? C29 C30 C31 120.0 . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 H31A 120.0 . . ? C26 C31 H31A 120.0 . . ? C33 C32 C29 129.8(9) . . ? C33 C32 H32A 115.1 . . ? C29 C32 H32A 115.1 . . ? C32 C33 C34 124.3(10) . . ? C32 C33 H33A 117.8 . . ? C34 C33 H33A 117.8 . . ? C35 C34 C36 121.3(7) . . ? C35 C34 C33 120.0(7) . . ? C36 C34 C33 118.0(7) . . ? C36 C35 C34 117.7(8) 17_576 . ? C36 C35 H35A 121.2 17_576 . ? C34 C35 H35A 121.2 . . ? C35 C36 C34 121.0(8) 17_576 . ? C35 C36 O9 121.8(10) 17_576 . ? C34 C36 O9 117.3(10) . . ? O5 C37 H37A 109.5 . . ? O5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O9 C38 H38A 109.5 . . ? O9 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O9 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O6 C39 H39A 109.5 . . ? O6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.522 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.063 # Attachment 'YB_PVDC_2_cif.txt' data_Yb-PVDC-2 _database_code_depnum_ccdc_archive 'CCDC 698332' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Yb-PVDC-2 _chemical_melting_point ? _chemical_formula_moiety 'C78 H60 O18 Yb2' _chemical_formula_sum 'C78 H60 O18 Yb2' _chemical_formula_weight 1631.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna _symmetry_space_group_name_Hall '-P 2a 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 16.0798(14) _cell_length_b 22.7096(19) _cell_length_c 38.484(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14053(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7858 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour amber _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 1.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.468 _exptl_absorpt_correction_T_max 0.543 _exptl_absorpt_process_details 'Apex2 v2.1-4 (Bruker, 2007)' _exptl_special_details ; An amber block-shaped crystal (0.45 x 0.5 x 0.45 mm) of Yb2(C26H20O6)3 was mounted in a glass capillary on a Bruker SMART APEX II CCD-based X-ray diffractometer equipped with a normal focus Mo-target X-ray tube (lambda = 0.71073A) operated at 2000 W power (45 kV and 35 mA). The X-ray intensities were measured at 298K. The detector was placed at a distance of 6.002 cm from the crystal. 1800 frames were collected with a scan width of 0.3 degrees in omega and phi with an exposure time of 10 s/frame. An initial unit cell was established using the Apex2 software proved to be ambiguous and thus 708 reflections were read in form several hundred frames and were exported into Cell-Now, resulting in a suggested I centered orthorhombic unit cell with the dimensions a = 16.063, b = 22.697, c = 38.454, alpha = 90.07, beta = 90.03, gamma = 89.93. 5.5% of the reflections were not consistent with an I centered lattice (versus 50% for e.g. a C-centered lattice), and the unit cell was integrated in this setting, a unit cell was assigned in XPREP and attempts were made to solve the structure. These attempts, however, failed, and thus the data were again integrated using a primitive orthorhombic instead of the I centered orthorhombic cell with the same metric parameters as that established by Cell_Now. Inspection in XPREP then also suggested an I-centered orthorhombic cell with I/sigma for reflections obeying I centering being 1.7 versus 5.2 for all reflections, but again the primitive cell was chosen instead. Based on systematic absences the space group Pnna was chosen and the data were cut off at a d-spacing of 0.75. The structure was then solved with the help of Patterson methods using the program XS, which revealed two Ytterbium atoms and some of the metal bound oxygen atoms. Using Fourier transform recycling additional possible oxygen atoms were identified during the next refinement cycles. Tentatively correct oxygen positions were chosen based on the Yb-O distances and angles. Successive improvement of the difference map then allowed for the identification of the aromatic rings bonded to the carboxylate groups, and the model was augmented to include all of the O2C-C6H4 groups. At this point it became obvious that the remainder of the linking molecules exhibit large vibrational motion with less than atomic resolution for the 2,5-dimethoxy phenylene units. The overall electron density nevertheless allowed for identification of the units as a whole and disorder for one of the two crystallographically independent linkers became obvious. The - caused by flip disorder of one of the two ethylene units - involves both etheylene units of this linker, the 2,5-dimethoxy phenylene and one of the carboxylate bonded aromatic rings, and the occupancy ratio refined to 0.63(1) to 0.37(1). The other linker - located on a crystallographical inversion center - showed no disorder but only very pronounced thermal motion. In order to obtain a chemically meaningful model and refinement a range of restraints was introduced at this point. For the benzene ring located on the inversion center all 1,1 and 1,2 C-C distances were restrained to be each the same (the respective symmetry operator was used to do this across the inversion center). All other benzene rings were restrained to resemble ideal hexagons with C-C distances of 1.39 Angstrom. All carbon atoms but the carboxylate ones were restrained to be isotropic within a standard deviation of 0.02 squared Angstroms, and all carbon and oxygen atoms were restrained to have similar ADPs as their neighbors (SIMU and DELU restraints with a standard deviation of 0.03 each). Chemically equivalent 1,1 and 1,2 C-C distances to the ethylene carbon atoms in all units were restrained to be the same within a standard deviation of 0.02 Angstrom. The methoxy units were restrained to have the same 1,1 and 1,2 distances in all units and to lie within the planes of the phenylene units they are bonded to. The carbon atoms C2a to C7a were set to have the same ADPs as their disordered counterparts C2b to C7b (which whom they significantely overlap). Application of these restraints did not cause any significant increase in R values or decrease in any other structure quality indicators, and none of the restraints applied had an error significantly larger than 0.1 Angstrom or Angstrom squared for bond distance and ADP restraints, respectively. The residual electron density in the voids between the inorganic-organic hybrid network did not exhibit any chemically meaningful pattern and was ignored during the refinement process. No correction was applied for the residual electron density. The two largest peaks exhibit electron densities of 2.44 and 1.89 electrons per cubic Angstrom. ; _diffrn_ambient_temperature 298(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 APEX2 CCD diffractometer' _diffrn_measurement_method '\w an \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 123644 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 28.29 _reflns_number_total 17435 _reflns_number_gt 9495 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2.1-4 (Bruker, 2007)' _computing_cell_refinement 'Apex2 v2.1-4' _computing_data_reduction 'Apex2 v2.1-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.1311P)^2^+49.4367P] 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 17435 _refine_ls_number_parameters 529 _refine_ls_number_restraints 1228 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.2528 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1524(5) 0.0756(3) 0.03048(17) 0.0481(17) Uani 1 1 d DU . . C2A C 0.183(2) 0.1165(11) 0.0583(6) 0.0549(19) Uani 0.371(11) 1 d PGDU A 1 C3A C 0.1305(16) 0.1298(10) 0.0859(7) 0.068(4) Uani 0.371(11) 1 d PGU A 1 H3AA H 0.0769 0.1144 0.0866 0.082 Uiso 0.371(11) 1 calc PR A 1 C4A C 0.1581(19) 0.1660(11) 0.1127(6) 0.084(4) Uani 0.371(11) 1 d PGU A 1 H4AA H 0.1230 0.1749 0.1311 0.100 Uiso 0.371(11) 1 calc PR A 1 C5A C 0.238(2) 0.1890(12) 0.1117(6) 0.089(3) Uani 0.371(11) 1 d PGDU A 1 C6A C 0.2906(17) 0.1757(13) 0.0841(8) 0.082(3) Uani 0.371(11) 1 d PGU A 1 H6AA H 0.3442 0.1911 0.0835 0.098 Uiso 0.371(11) 1 calc PR A 1 C7A C 0.263(2) 0.1395(13) 0.0574(6) 0.066(3) Uani 0.371(11) 1 d PGU A 1 H7AA H 0.2980 0.1306 0.0389 0.079 Uiso 0.371(11) 1 calc PR A 1 C8A C 0.2877(19) 0.2251(18) 0.1377(8) 0.101(6) Uani 0.371(11) 1 d PDU A 1 H8A H 0.3450 0.2288 0.1350 0.121 Uiso 0.371(11) 1 calc PR A 1 C9A C 0.2528(18) 0.2498(15) 0.1624(7) 0.098(6) Uani 0.371(11) 1 d PDU A 1 H9AA H 0.1950 0.2488 0.1626 0.117 Uiso 0.371(11) 1 calc PR A 1 C10A C 0.2935(15) 0.2808(13) 0.1915(5) 0.109(6) Uani 0.371(11) 1 d PGDU A 1 C11A C 0.3776(14) 0.2930(11) 0.1958(5) 0.115(6) Uani 0.371(11) 1 d PGDU A 1 C12A C 0.4054(14) 0.3205(13) 0.2259(6) 0.113(6) Uani 0.371(11) 1 d PGDU A 1 H12A H 0.4616 0.3286 0.2287 0.136 Uiso 0.371(11) 1 calc PR A 1 C13A C 0.3490(16) 0.3358(14) 0.2518(5) 0.107(6) Uani 0.371(11) 1 d PGDU A 1 C14A C 0.2649(15) 0.3236(12) 0.2475(5) 0.137(7) Uani 0.371(11) 1 d PGDU A 1 C15A C 0.2372(13) 0.2961(13) 0.2174(6) 0.120(7) Uani 0.371(11) 1 d PGDU A 1 H15A H 0.1809 0.2880 0.2146 0.144 Uiso 0.371(11) 1 calc PR A 1 O3A O 0.4492(18) 0.2796(16) 0.1722(7) 0.173(8) Uani 0.371(11) 1 d PDU A 1 O4A O 0.190(2) 0.3335(17) 0.2704(7) 0.193(9) Uani 0.371(11) 1 d PDU A 1 C16A C 0.524(3) 0.297(2) 0.2010(13) 0.185(12) Uani 0.371(11) 1 d PDU A 1 H16A H 0.5779 0.2886 0.1911 0.277 Uiso 0.371(11) 1 calc PR A 1 H16B H 0.5172 0.2744 0.2218 0.277 Uiso 0.371(11) 1 calc PR A 1 H16C H 0.5211 0.3383 0.2065 0.277 Uiso 0.371(11) 1 calc PR A 1 C17A C 0.104(2) 0.316(3) 0.2490(12) 0.212(16) Uani 0.371(11) 1 d PDU A 1 H17A H 0.0564 0.3241 0.2633 0.318 Uiso 0.371(11) 1 calc PR A 1 H17B H 0.1052 0.2754 0.2429 0.318 Uiso 0.371(11) 1 calc PR A 1 H17C H 0.1005 0.3397 0.2282 0.318 Uiso 0.371(11) 1 calc PR A 1 C18A C 0.381(2) 0.367(2) 0.2835(8) 0.105(7) Uani 0.371(11) 1 d PDU A 1 H18A H 0.3391 0.3766 0.2991 0.126 Uiso 0.371(11) 1 calc PR A 1 C19A C 0.451(2) 0.381(2) 0.2934(7) 0.107(7) Uani 0.371(11) 1 d PDU A 1 H19A H 0.4866 0.3847 0.2746 0.128 Uiso 0.371(11) 1 calc PR A 1 C2B C 0.1776(12) 0.1185(6) 0.0580(3) 0.0549(19) Uani 0.629(11) 1 d PGDU A 2 C3B C 0.1194(9) 0.1469(6) 0.0788(4) 0.068(4) Uani 0.629(11) 1 d PGU A 2 H3BA H 0.0629 0.1407 0.0751 0.082 Uiso 0.629(11) 1 calc PR A 2 C4B C 0.1455(11) 0.1847(6) 0.1050(3) 0.084(4) Uani 0.629(11) 1 d PGU A 2 H4BA H 0.1065 0.2037 0.1189 0.100 Uiso 0.629(11) 1 calc PR A 2 C5B C 0.2299(12) 0.1941(7) 0.1105(4) 0.089(3) Uani 0.629(11) 1 d PGDU A 2 C6B C 0.2882(10) 0.1657(8) 0.0897(5) 0.082(3) Uani 0.629(11) 1 d PGU A 2 H6BA H 0.3447 0.1720 0.0934 0.098 Uiso 0.629(11) 1 calc PR A 2 C7B C 0.2620(11) 0.1279(7) 0.0635(4) 0.066(3) Uani 0.629(11) 1 d PGU A 2 H7BA H 0.3010 0.1089 0.0496 0.079 Uiso 0.629(11) 1 calc PR A 2 C8B C 0.2506(11) 0.2298(10) 0.1426(5) 0.096(5) Uani 0.629(11) 1 d PDU A 2 H8BA H 0.2059 0.2429 0.1558 0.115 Uiso 0.629(11) 1 calc PR A 2 C9B C 0.3213(12) 0.2433(9) 0.1530(4) 0.106(5) Uani 0.629(11) 1 d PDU A 2 H9BA H 0.3656 0.2317 0.1390 0.127 Uiso 0.629(11) 1 calc PR A 2 C10B C 0.3429(11) 0.2760(7) 0.1853(3) 0.106(5) Uani 0.629(11) 1 d PGDU A 2 C11B C 0.4271(10) 0.2820(7) 0.1927(3) 0.134(5) Uani 0.629(11) 1 d PGDU A 2 C12B C 0.4523(8) 0.3120(8) 0.2224(4) 0.115(5) Uani 0.629(11) 1 d PGDU A 2 H12B H 0.5086 0.3160 0.2273 0.138 Uiso 0.629(11) 1 calc PR A 2 C13B C 0.3933(9) 0.3362(7) 0.2446(3) 0.102(5) Uani 0.629(11) 1 d PGDU A 2 C14B C 0.3091(8) 0.3302(7) 0.2372(3) 0.116(5) Uani 0.629(11) 1 d PGDU A 2 C15B C 0.2839(8) 0.3002(7) 0.2075(4) 0.119(5) Uani 0.629(11) 1 d PGDU A 2 H15B H 0.2276 0.2962 0.2026 0.143 Uiso 0.629(11) 1 calc PR A 2 O3B O 0.4927(14) 0.2550(10) 0.1720(5) 0.183(7) Uani 0.629(11) 1 d PDU A 2 O4B O 0.2471(12) 0.3542(9) 0.2588(5) 0.160(6) Uani 0.629(11) 1 d PDU A 2 C16B C 0.5873(19) 0.2802(16) 0.1755(9) 0.218(12) Uani 0.629(11) 1 d PDU A 2 H16D H 0.6246 0.2554 0.1626 0.327 Uiso 0.629(11) 1 calc PR A 2 H16E H 0.6034 0.2805 0.1995 0.327 Uiso 0.629(11) 1 calc PR A 2 H16F H 0.5897 0.3195 0.1664 0.327 Uiso 0.629(11) 1 calc PR A 2 C17B C 0.1582(18) 0.3352(17) 0.2392(8) 0.234(12) Uani 0.629(11) 1 d PDU A 2 H17D H 0.1120 0.3492 0.2527 0.351 Uiso 0.629(11) 1 calc PR A 2 H17E H 0.1553 0.2931 0.2373 0.351 Uiso 0.629(11) 1 calc PR A 2 H17F H 0.1564 0.3523 0.2164 0.351 Uiso 0.629(11) 1 calc PR A 2 C18B C 0.4155(14) 0.3567(12) 0.2803(5) 0.112(6) Uani 0.629(11) 1 d PDU A 2 H18B H 0.3716 0.3619 0.2957 0.134 Uiso 0.629(11) 1 calc PR A 2 C19B C 0.4855(14) 0.3674(12) 0.2914(4) 0.112(6) Uani 0.629(11) 1 d PDU A 2 H19B H 0.5320 0.3580 0.2782 0.134 Uiso 0.629(11) 1 calc PR A 2 C20 C 0.4960(8) 0.3959(6) 0.3268(3) 0.111(4) Uani 1 1 d DU . . C21 C 0.5768(9) 0.4068(7) 0.3326(3) 0.132(5) Uani 1 1 d U A . H21A H 0.6146 0.4011 0.3146 0.159 Uiso 1 1 calc R . . C22 C 0.6063(7) 0.4268(5) 0.3655(2) 0.098(3) Uani 1 1 d U . . H22A H 0.6624 0.4349 0.3689 0.118 Uiso 1 1 calc R A . C23 C 0.5495(5) 0.4338(4) 0.39211(19) 0.059(2) Uani 1 1 d U A . C24 C 0.4695(6) 0.4226(5) 0.3859(2) 0.081(3) Uani 1 1 d U . . H24A H 0.4309 0.4285 0.4035 0.098 Uiso 1 1 calc R A . C25 C 0.4429(7) 0.4026(6) 0.3542(3) 0.108(4) Uani 1 1 d U A . H25A H 0.3870 0.3933 0.3512 0.129 Uiso 1 1 calc R . . C26 C 0.5815(5) 0.4535(3) 0.42679(16) 0.0459(16) Uani 1 1 d U . . C27 C 0.6362(4) 0.5984(3) 0.47091(19) 0.0439(15) Uani 1 1 d U A . C28 C 0.6026(5) 0.65810(19) 0.47526(18) 0.072(2) Uani 1 1 d GU A . C29 C 0.5522(5) 0.6716(3) 0.50350(18) 0.091(3) Uani 1 1 d GU . . H29A H 0.5367 0.6422 0.5190 0.110 Uiso 1 1 calc R . . C30 C 0.5249(5) 0.7290(3) 0.5085(2) 0.122(4) Uani 1 1 d GU B . H30A H 0.4912 0.7381 0.5274 0.147 Uiso 1 1 calc R . . C31 C 0.5481(6) 0.7730(2) 0.4854(3) 0.136(5) Uani 1 1 d GDU . . C32 C 0.5985(6) 0.7595(2) 0.4571(2) 0.150(5) Uani 1 1 d GU B . H32A H 0.6141 0.7889 0.4416 0.180 Uiso 1 1 calc R . . C33 C 0.6258(5) 0.7021(3) 0.45208(18) 0.124(4) Uani 1 1 d GU . . H33A H 0.6595 0.6931 0.4332 0.149 Uiso 1 1 calc R B . C34 C 0.5256(11) 0.8357(5) 0.4945(5) 0.181(6) Uani 1 1 d DU B 1 H34A H 0.4861 0.8393 0.5120 0.217 Uiso 1 1 calc R B 1 C35 C 0.5505(12) 0.8826(5) 0.4828(6) 0.192(7) Uani 1 1 d DU B 1 H35A H 0.5923 0.8800 0.4662 0.231 Uiso 1 1 calc R B 1 C36 C 0.5225(13) 0.9432(5) 0.4917(5) 0.195(7) Uani 1 1 d DU B 1 C37 C 0.4716(14) 0.9543(6) 0.5195(5) 0.234(10) Uani 1 1 d DU . 1 H37A H 0.4494 0.9232 0.5323 0.351 Uiso 1 1 calc R . 1 C38 C 0.5464(16) 0.9888(7) 0.4715(6) 0.260(10) Uani 1 1 d DU . 1 C39 C 0.621(2) 1.0181(13) 0.4187(10) 0.393(19) Uani 1 1 d DU C 1 H39A H 0.6577 0.9999 0.4020 0.589 Uiso 1 1 calc R C 1 H39B H 0.6505 1.0493 0.4303 0.589 Uiso 1 1 calc R C 1 H39C H 0.5737 1.0339 0.4069 0.589 Uiso 1 1 calc R C 1 O9 O 0.5943(15) 0.9737(7) 0.4444(7) 0.327(10) Uani 1 1 d DU C 1 O1 O 0.2035(3) 0.0583(2) 0.00894(12) 0.0534(13) Uani 1 1 d U . . O2 O 0.0765(3) 0.0609(3) 0.03027(14) 0.0670(16) Uani 1 1 d U . . O5 O 0.6560(3) 0.4672(2) 0.43007(11) 0.0502(12) Uani 1 1 d U A . O6 O 0.5284(3) 0.4545(2) 0.45129(12) 0.0573(13) Uani 1 1 d U A . O7 O 0.6114(3) 0.5554(2) 0.48979(12) 0.0461(11) Uani 1 1 d U A . O8 O 0.6940(3) 0.5901(2) 0.44949(14) 0.0584(13) Uani 1 1 d U A . Yb1 Yb 0.7500 0.5000 0.467417(8) 0.02925(12) Uani 1 2 d S . . Yb2 Yb 0.5000 0.5000 0.5000 0.03212(12) Uani 1 2 d S . . 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 0.058(4) 0.052(4) 0.034(3) -0.015(3) -0.004(3) -0.004(3) C2A 0.060(4) 0.066(4) 0.038(3) -0.023(3) -0.008(3) -0.009(4) C3A 0.078(6) 0.076(7) 0.052(6) -0.024(5) -0.005(5) 0.003(6) C4A 0.103(7) 0.084(8) 0.065(6) -0.040(6) -0.003(5) 0.005(6) C5A 0.104(6) 0.095(6) 0.068(5) -0.045(4) -0.022(4) -0.009(5) C6A 0.085(5) 0.088(7) 0.071(6) -0.029(5) -0.023(5) -0.020(5) C7A 0.076(5) 0.073(7) 0.049(6) -0.019(5) -0.013(4) -0.011(5) C8A 0.108(12) 0.111(11) 0.084(10) -0.041(9) -0.019(10) -0.008(10) C9A 0.109(12) 0.103(11) 0.082(10) -0.039(9) -0.022(10) -0.011(11) C10A 0.126(11) 0.114(11) 0.088(10) -0.038(9) -0.037(10) -0.008(11) C11A 0.131(10) 0.127(10) 0.087(9) -0.047(9) -0.017(9) -0.001(10) C12A 0.135(11) 0.118(10) 0.087(10) -0.044(9) -0.023(9) -0.007(10) C13A 0.120(10) 0.114(10) 0.086(10) -0.037(9) -0.020(9) -0.014(10) C14A 0.147(10) 0.149(12) 0.116(11) -0.035(10) -0.011(10) -0.012(11) C15A 0.136(12) 0.125(12) 0.099(11) -0.027(10) -0.017(10) -0.019(11) O3A 0.199(15) 0.195(16) 0.125(13) -0.071(14) -0.008(13) 0.016(15) O4A 0.201(16) 0.218(18) 0.159(16) -0.043(16) 0.039(14) -0.018(17) C16A 0.164(15) 0.203(18) 0.188(18) -0.011(15) -0.021(14) -0.013(15) C17A 0.192(18) 0.23(2) 0.22(2) -0.004(17) 0.015(16) -0.026(17) C18A 0.110(12) 0.117(12) 0.088(11) -0.030(10) -0.020(10) -0.005(11) C19A 0.114(12) 0.128(13) 0.078(10) -0.041(10) -0.033(10) -0.004(11) C2B 0.060(4) 0.066(4) 0.038(3) -0.023(3) -0.008(3) -0.009(4) C3B 0.078(6) 0.076(7) 0.052(6) -0.024(5) -0.005(5) 0.003(6) C4B 0.103(7) 0.084(8) 0.065(6) -0.040(6) -0.003(5) 0.005(6) C5B 0.104(6) 0.095(6) 0.068(5) -0.045(4) -0.022(4) -0.009(5) C6B 0.085(5) 0.088(7) 0.071(6) -0.029(5) -0.023(5) -0.020(5) C7B 0.076(5) 0.073(7) 0.049(6) -0.019(5) -0.013(4) -0.011(5) C8B 0.108(10) 0.104(9) 0.076(8) -0.054(7) -0.013(8) -0.004(9) C9B 0.114(10) 0.116(10) 0.086(9) -0.042(8) -0.021(8) -0.023(9) C10B 0.120(9) 0.115(9) 0.083(8) -0.045(7) -0.026(8) -0.009(9) C11B 0.155(10) 0.156(10) 0.089(9) -0.059(8) -0.006(9) -0.002(9) C12B 0.145(10) 0.127(10) 0.073(8) -0.044(8) -0.008(8) 0.001(10) C13B 0.120(9) 0.114(9) 0.072(8) -0.043(7) -0.031(7) -0.016(8) C14B 0.133(9) 0.127(9) 0.088(8) -0.046(7) -0.029(8) -0.019(9) C15B 0.130(9) 0.128(10) 0.100(9) -0.035(8) -0.036(8) -0.015(9) O3B 0.199(13) 0.211(15) 0.140(11) -0.087(11) 0.032(12) 0.037(12) O4B 0.174(12) 0.179(13) 0.127(11) -0.084(10) -0.007(9) -0.040(10) C16B 0.200(15) 0.251(19) 0.203(18) -0.033(15) 0.004(15) 0.020(15) C17B 0.185(15) 0.261(19) 0.256(19) 0.023(16) -0.031(15) -0.026(15) C18B 0.121(11) 0.129(10) 0.085(8) -0.042(8) -0.030(8) -0.013(10) C19B 0.122(12) 0.140(12) 0.072(8) -0.042(8) -0.033(8) -0.006(10) C20 0.116(8) 0.158(9) 0.060(6) -0.045(6) -0.023(6) -0.023(7) C21 0.134(9) 0.219(12) 0.044(5) -0.059(7) 0.005(6) -0.031(9) C22 0.086(6) 0.164(10) 0.044(5) -0.049(6) 0.003(4) -0.020(7) C23 0.065(5) 0.075(5) 0.038(4) -0.027(4) -0.008(3) 0.000(4) C24 0.064(5) 0.120(8) 0.061(5) -0.033(5) -0.012(4) -0.010(5) C25 0.080(7) 0.163(10) 0.080(7) -0.040(7) -0.027(5) -0.021(7) C26 0.059(4) 0.050(4) 0.029(3) -0.011(3) -0.008(3) 0.007(3) C27 0.047(4) 0.030(3) 0.055(4) 0.003(3) -0.007(3) 0.006(3) C28 0.087(6) 0.031(4) 0.096(6) 0.003(4) 0.014(5) 0.016(4) C29 0.109(8) 0.046(5) 0.120(8) -0.009(5) 0.037(6) 0.011(5) C30 0.121(9) 0.066(7) 0.180(11) -0.015(7) 0.046(8) 0.026(7) C31 0.142(10) 0.052(6) 0.215(13) 0.002(7) 0.028(9) 0.035(7) C32 0.187(12) 0.055(6) 0.208(13) 0.055(8) 0.055(10) 0.034(7) C33 0.163(11) 0.046(5) 0.163(10) 0.028(6) 0.057(9) 0.007(6) C34 0.177(13) 0.064(7) 0.302(17) -0.020(9) 0.005(13) 0.039(9) C35 0.203(15) 0.054(7) 0.321(17) 0.000(10) 0.028(14) 0.031(9) C36 0.228(16) 0.049(7) 0.308(18) -0.013(9) 0.050(14) 0.047(9) C37 0.28(2) 0.066(9) 0.35(2) -0.009(12) 0.077(18) 0.033(12) C38 0.32(2) 0.076(9) 0.39(2) -0.019(12) 0.135(18) 0.054(13) C39 0.55(5) 0.16(2) 0.47(4) 0.05(2) 0.19(4) -0.05(3) O9 0.42(2) 0.107(10) 0.45(2) 0.014(13) 0.178(19) 0.050(13) O1 0.054(3) 0.062(3) 0.044(3) -0.023(2) 0.003(2) -0.005(3) O2 0.054(3) 0.086(4) 0.061(3) -0.030(3) 0.002(3) -0.019(3) O5 0.052(3) 0.065(3) 0.034(2) -0.012(2) -0.013(2) 0.004(3) O6 0.069(3) 0.067(3) 0.036(3) -0.015(2) 0.000(2) -0.004(3) O7 0.055(3) 0.036(2) 0.047(3) 0.001(2) -0.004(2) -0.004(2) O8 0.069(4) 0.046(3) 0.060(3) 0.010(2) 0.012(3) 0.010(3) Yb1 0.0360(2) 0.02731(18) 0.02443(18) 0.000 0.000 0.00202(17) Yb2 0.0335(2) 0.0332(2) 0.0297(2) -0.00162(17) -0.00199(12) 0.00434(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.232(8) . ? C1 O2 1.264(9) . ? C1 C2B 1.497(9) . ? C1 C2A 1.501(13) . ? C2A C3A 1.3900 . ? C2A C7A 1.3900 . ? C3A C4A 1.3900 . ? C3A H3AA 0.9300 . ? C4A C5A 1.3900 . ? C4A H4AA 0.9300 . ? C5A C6A 1.3900 . ? C5A C8A 1.518(16) . ? C6A C7A 1.3900 . ? C6A H6AA 0.9300 . ? C7A H7AA 0.9300 . ? C8A C9A 1.238(18) . ? C8A H8A 0.9300 . ? C9A C10A 1.478(15) . ? C9A H9AA 0.9300 . ? C10A C11A 1.3900 . ? C10A C15A 1.3900 . ? C11A C12A 1.3900 . ? C11A O3A 1.497(18) . ? C12A C13A 1.3900 . ? C12A H12A 0.9300 . ? C13A C14A 1.3900 . ? C13A C18A 1.498(15) . ? C14A C15A 1.3900 . ? C14A O4A 1.514(19) . ? C15A H15A 0.9300 . ? O3A C16A 1.69(2) . ? O4A C17A 1.65(2) . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C18A C19A 1.231(18) . ? C18A H18A 0.9300 . ? C19A C20 1.514(15) . ? C19A H19A 0.9300 . ? C2B C3B 1.3900 . ? C2B C7B 1.3900 . ? C3B C4B 1.3900 . ? C3B H3BA 0.9300 . ? C4B C5B 1.3900 . ? C4B H4BA 0.9300 . ? C5B C6B 1.3900 . ? C5B C8B 1.514(12) . ? C6B C7B 1.3900 . ? C6B H6BA 0.9300 . ? C7B H7BA 0.9300 . ? C8B C9B 1.244(15) . ? C8B H8BA 0.9300 . ? C9B C10B 1.490(12) . ? C9B H9BA 0.9300 . ? C10B C11B 1.3900 . ? C10B C15B 1.3900 . ? C11B C12B 1.3900 . ? C11B O3B 1.457(15) . ? C12B C13B 1.3900 . ? C12B H12B 0.9300 . ? C13B C14B 1.3900 . ? C13B C18B 1.493(13) . ? C14B C15B 1.3900 . ? C14B O4B 1.410(14) . ? C15B H15B 0.9300 . ? O3B C16B 1.63(2) . ? O4B C17B 1.67(2) . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? C18B C19B 1.228(16) . ? C18B H18B 0.9300 . ? C19B C20 1.518(13) . ? C19B H19B 0.9300 . ? C20 C21 1.341(16) . ? C20 C25 1.362(15) . ? C21 C22 1.426(12) . ? C21 H21A 0.9300 . ? C22 C23 1.383(11) . ? C22 H22A 0.9300 . ? C23 C24 1.332(11) . ? C23 C26 1.498(9) . ? C24 C25 1.373(12) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 O5 1.244(8) . ? C26 O6 1.273(8) . ? C27 O8 1.256(8) . ? C27 O7 1.280(8) . ? C27 C28 1.469(8) . ? C27 Yb1 2.891(7) . ? C28 C29 1.3900 . ? C28 C33 1.3900 . ? C29 C30 1.3900 . ? C29 H29A 0.9300 . ? C30 C31 1.3900 . ? C30 H30A 0.9300 . ? C31 C32 1.3900 . ? C31 C34 1.511(12) . ? C32 C33 1.3900 . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C35 1.222(15) . ? C34 H34A 0.9300 . ? C35 C36 1.488(13) . ? C35 H35A 0.9300 . ? C36 C38 1.353(14) . ? C36 C37 1.371(14) . ? C37 C38 1.370(14) 5_676 ? C37 H37A 0.9300 . ? C38 O9 1.34(2) . ? C38 C37 1.370(14) 5_676 ? C39 O9 1.48(3) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? O1 Yb1 2.206(5) 7_565 ? O2 Yb2 2.188(5) 3_545 ? O5 Yb1 2.215(4) . ? O6 Yb2 2.189(5) . ? O7 Yb2 2.224(5) . ? O7 Yb1 2.700(5) . ? O8 Yb1 2.339(5) . ? Yb1 O1 2.206(5) 8_666 ? Yb1 O1 2.206(5) 7_666 ? Yb1 O5 2.215(5) 2_665 ? Yb1 O8 2.339(5) 2_665 ? Yb1 O7 2.701(5) 2_665 ? Yb1 C27 2.891(7) 2_665 ? Yb1 Yb2 4.2110(3) . ? Yb1 Yb2 4.2110(3) 2_665 ? Yb2 O2 2.188(5) 3 ? Yb2 O2 2.188(5) 7_666 ? Yb2 O6 2.189(5) 5_666 ? Yb2 O7 2.224(5) 5_666 ? Yb2 Yb1 4.2110(4) 5_666 ? 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 C1 O2 123.8(6) . . ? O1 C1 C2B 120.2(10) . . ? O2 C1 C2B 116.0(9) . . ? O1 C1 C2A 117.3(14) . . ? O2 C1 C2A 118.9(14) . . ? C3A C2A C7A 120.0 . . ? C3A C2A C1 119(2) . . ? C7A C2A C1 121(2) . . ? C4A C3A C2A 120.0 . . ? C4A C3A H3AA 120.0 . . ? C2A C3A H3AA 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A H4AA 120.0 . . ? C3A C4A H4AA 120.0 . . ? C6A C5A C4A 120.0 . . ? C6A C5A C8A 108(2) . . ? C4A C5A C8A 132(2) . . ? C7A C6A C5A 120.0 . . ? C7A C6A H6AA 120.0 . . ? C5A C6A H6AA 120.0 . . ? C6A C7A C2A 120.0 . . ? C6A C7A H7AA 120.0 . . ? C2A C7A H7AA 120.0 . . ? C9A C8A C5A 121(2) . . ? C9A C8A H8A 119.6 . . ? C5A C8A H8A 119.6 . . ? C8A C9A C10A 127(2) . . ? C8A C9A H9AA 116.7 . . ? C10A C9A H9AA 116.7 . . ? C11A C10A C15A 120.0 . . ? C11A C10A C9A 128.0(18) . . ? C15A C10A C9A 112.0(18) . . ? C12A C11A C10A 120.0 . . ? C12A C11A O3A 110.4(13) . . ? C10A C11A O3A 129.6(13) . . ? C13A C12A C11A 120.0 . . ? C13A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? C12A C13A C14A 120.0 . . ? C12A C13A C18A 118(2) . . ? C14A C13A C18A 122(2) . . ? C15A C14A C13A 120.0 . . ? C15A C14A O4A 107.1(14) . . ? C13A C14A O4A 132.9(14) . . ? C14A C15A C10A 120.0 . . ? C14A C15A H15A 120.0 . . ? C10A C15A H15A 120.0 . . ? C11A O3A C16A 96(2) . . ? C14A O4A C17A 110.0(16) . . ? O3A C16A H16A 109.5 . . ? O3A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? O3A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? O4A C17A H17A 109.5 . . ? O4A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? O4A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C19A C18A C13A 134(3) . . ? C19A C18A H18A 113.1 . . ? C13A C18A H18A 113.1 . . ? C18A C19A C20 140(3) . . ? C18A C19A H19A 110.2 . . ? C20 C19A H19A 110.2 . . ? C3B C2B C7B 120.0 . . ? C3B C2B C1 121.8(12) . . ? C7B C2B C1 118.2(12) . . ? C2B C3B C4B 120.0 . . ? C2B C3B H3BA 120.0 . . ? C4B C3B H3BA 120.0 . . ? C3B C4B C5B 120.0 . . ? C3B C4B H4BA 120.0 . . ? C5B C4B H4BA 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B C8B 124.7(14) . . ? C4B C5B C8B 114.8(14) . . ? C7B C6B C5B 120.0 . . ? C7B C6B H6BA 120.0 . . ? C5B C6B H6BA 120.0 . . ? C6B C7B C2B 120.0 . . ? C6B C7B H7BA 120.0 . . ? C2B C7B H7BA 120.0 . . ? C9B C8B C5B 126.5(17) . . ? C9B C8B H8BA 116.7 . . ? C5B C8B H8BA 116.7 . . ? C8B C9B C10B 127.2(17) . . ? C8B C9B H9BA 116.4 . . ? C10B C9B H9BA 116.4 . . ? C11B C10B C15B 120.0 . . ? C11B C10B C9B 116.5(12) . . ? C15B C10B C9B 123.5(12) . . ? C12B C11B C10B 120.0 . . ? C12B C11B O3B 116.4(11) . . ? C10B C11B O3B 123.5(11) . . ? C11B C12B C13B 120.0 . . ? C11B C12B H12B 120.0 . . ? C13B C12B H12B 120.0 . . ? C14B C13B C12B 120.0 . . ? C14B C13B C18B 116.8(12) . . ? C12B C13B C18B 121.8(12) . . ? C13B C14B C15B 120.0 . . ? C13B C14B O4B 122.1(10) . . ? C15B C14B O4B 117.9(10) . . ? C14B C15B C10B 120.0 . . ? C14B C15B H15B 120.0 . . ? C10B C15B H15B 120.0 . . ? C11B O3B C16B 118.9(17) . . ? C14B O4B C17B 103.8(14) . . ? O3B C16B H16D 109.5 . . ? O3B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? O3B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? O4B C17B H17D 109.5 . . ? O4B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? O4B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C19B C18B C13B 127.0(17) . . ? C19B C18B H18B 116.5 . . ? C13B C18B H18B 116.5 . . ? C18B C19B C20 119.9(16) . . ? C18B C19B H19B 120.0 . . ? C20 C19B H19B 120.0 . . ? C21 C20 C25 117.4(9) . . ? C21 C20 C19A 130.2(19) . . ? C25 C20 C19A 112.3(18) . . ? C21 C20 C19B 109.5(13) . . ? C25 C20 C19B 132.1(13) . . ? C20 C21 C22 121.8(10) . . ? C20 C21 H21A 119.1 . . ? C22 C21 H21A 119.1 . . ? C23 C22 C21 118.4(10) . . ? C23 C22 H22A 120.8 . . ? C21 C22 H22A 120.8 . . ? C24 C23 C22 118.9(7) . . ? C24 C23 C26 123.2(7) . . ? C22 C23 C26 117.9(7) . . ? C23 C24 C25 121.6(9) . . ? C23 C24 H24A 119.2 . . ? C25 C24 H24A 119.2 . . ? C20 C25 C24 121.9(10) . . ? C20 C25 H25A 119.1 . . ? C24 C25 H25A 119.1 . . ? O5 C26 O6 124.5(6) . . ? O5 C26 C23 119.7(6) . . ? O6 C26 C23 115.7(7) . . ? O8 C27 O7 119.2(6) . . ? O8 C27 C28 119.0(6) . . ? O7 C27 C28 121.6(6) . . ? O8 C27 Yb1 52.1(3) . . ? O7 C27 Yb1 68.6(4) . . ? C28 C27 Yb1 162.0(5) . . ? C29 C28 C33 120.0 . . ? C29 C28 C27 120.5(5) . . ? C33 C28 C27 119.4(5) . . ? C30 C29 C28 120.0 . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 C34 122.0(9) . . ? C30 C31 C34 117.6(9) . . ? C33 C32 C31 120.0 . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 C28 120.0 . . ? C32 C33 H33A 120.0 . . ? C28 C33 H33A 120.0 . . ? C35 C34 C31 131.0(16) . . ? C35 C34 H34A 114.5 . . ? C31 C34 H34A 114.5 . . ? C34 C35 C36 128.4(17) . . ? C34 C35 H35A 115.8 . . ? C36 C35 H35A 115.8 . . ? C38 C36 C37 118.7(9) . . ? C38 C36 C35 119.3(16) . . ? C37 C36 C35 122.0(16) . . ? C38 C37 C36 119.8(11) 5_676 . ? C38 C37 H37A 120.1 5_676 . ? C36 C37 H37A 120.1 . . ? O9 C38 C36 114.6(17) . . ? O9 C38 C37 124.0(18) . 5_676 ? C36 C38 C37 121.1(12) . 5_676 ? O9 C39 H39A 109.5 . . ? O9 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O9 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 O9 C39 121(2) . . ? C1 O1 Yb1 154.8(5) . 7_565 ? C1 O2 Yb2 135.4(5) . 3_545 ? C26 O5 Yb1 143.8(4) . . ? C26 O6 Yb2 141.5(5) . . ? C27 O7 Yb2 141.5(4) . . ? C27 O7 Yb1 85.3(4) . . ? Yb2 O7 Yb1 117.21(18) . . ? C27 O8 Yb1 102.9(4) . . ? O1 Yb1 O1 87.2(3) 8_666 7_666 ? O1 Yb1 O5 92.13(19) 8_666 2_665 ? O1 Yb1 O5 154.56(18) 7_666 2_665 ? O1 Yb1 O5 154.56(18) 8_666 . ? O1 Yb1 O5 92.13(19) 7_666 . ? O5 Yb1 O5 99.1(3) 2_665 . ? O1 Yb1 O8 79.6(2) 8_666 . ? O1 Yb1 O8 127.48(19) 7_666 . ? O5 Yb1 O8 77.15(18) 2_665 . ? O5 Yb1 O8 80.77(19) . . ? O1 Yb1 O8 127.47(19) 8_666 2_665 ? O1 Yb1 O8 79.6(2) 7_666 2_665 ? O5 Yb1 O8 80.77(19) 2_665 2_665 ? O5 Yb1 O8 77.15(18) . 2_665 ? O8 Yb1 O8 145.7(3) . 2_665 ? O1 Yb1 O7 76.63(16) 8_666 . ? O1 Yb1 O7 76.67(16) 7_666 . ? O5 Yb1 O7 127.86(16) 2_665 . ? O5 Yb1 O7 78.47(16) . . ? O8 Yb1 O7 50.86(16) . . ? O8 Yb1 O7 145.02(17) 2_665 . ? O1 Yb1 O7 76.66(16) 8_666 2_665 ? O1 Yb1 O7 76.63(16) 7_666 2_665 ? O5 Yb1 O7 78.47(16) 2_665 2_665 ? O5 Yb1 O7 127.86(16) . 2_665 ? O8 Yb1 O7 145.02(17) . 2_665 ? O8 Yb1 O7 50.86(16) 2_665 2_665 ? O7 Yb1 O7 142.81(19) . 2_665 ? O1 Yb1 C27 73.54(19) 8_666 . ? O1 Yb1 C27 102.5(2) 7_666 . ? O5 Yb1 C27 101.7(2) 2_665 . ? O5 Yb1 C27 81.82(19) . . ? O8 Yb1 C27 25.07(18) . . ? O8 Yb1 C27 158.94(19) 2_665 . ? O7 Yb1 C27 26.19(17) . . ? O7 Yb1 C27 150.20(17) 2_665 . ? O1 Yb1 C27 102.5(2) 8_666 2_665 ? O1 Yb1 C27 73.54(19) 7_666 2_665 ? O5 Yb1 C27 81.82(19) 2_665 2_665 ? O5 Yb1 C27 101.7(2) . 2_665 ? O8 Yb1 C27 158.94(19) . 2_665 ? O8 Yb1 C27 25.07(18) 2_665 2_665 ? O7 Yb1 C27 150.19(17) . 2_665 ? O7 Yb1 C27 26.19(17) 2_665 2_665 ? C27 Yb1 C27 174.7(3) . 2_665 ? O1 Yb1 Yb2 96.18(13) 8_666 . ? O1 Yb1 Yb2 57.38(13) 7_666 . ? O5 Yb1 Yb2 147.67(13) 2_665 . ? O5 Yb1 Yb2 62.72(13) . . ? O8 Yb1 Yb2 73.76(13) . . ? O8 Yb1 Yb2 117.08(14) 2_665 . ? O7 Yb1 Yb2 28.02(10) . . ? O7 Yb1 Yb2 133.86(9) 2_665 . ? C27 Yb1 Yb2 51.83(15) . . ? C27 Yb1 Yb2 126.18(14) 2_665 . ? O1 Yb1 Yb2 57.38(13) 8_666 2_665 ? O1 Yb1 Yb2 96.18(13) 7_666 2_665 ? O5 Yb1 Yb2 62.71(13) 2_665 2_665 ? O5 Yb1 Yb2 147.66(13) . 2_665 ? O8 Yb1 Yb2 117.08(14) . 2_665 ? O8 Yb1 Yb2 73.76(13) 2_665 2_665 ? O7 Yb1 Yb2 133.86(9) . 2_665 ? O7 Yb1 Yb2 28.02(10) 2_665 2_665 ? C27 Yb1 Yb2 126.18(14) . 2_665 ? C27 Yb1 Yb2 51.83(15) 2_665 2_665 ? Yb2 Yb1 Yb2 145.352(9) . 2_665 ? O2 Yb2 O2 179.999(2) 3 7_666 ? O2 Yb2 O6 92.3(2) 3 5_666 ? O2 Yb2 O6 87.7(2) 7_666 5_666 ? O2 Yb2 O6 87.7(2) 3 . ? O2 Yb2 O6 92.3(2) 7_666 . ? O6 Yb2 O6 179.998(1) 5_666 . ? O2 Yb2 O7 90.0(2) 3 . ? O2 Yb2 O7 90.0(2) 7_666 . ? O6 Yb2 O7 92.97(18) 5_666 . ? O6 Yb2 O7 87.03(18) . . ? O2 Yb2 O7 90.0(2) 3 5_666 ? O2 Yb2 O7 90.0(2) 7_666 5_666 ? O6 Yb2 O7 87.04(18) 5_666 5_666 ? O6 Yb2 O7 92.96(18) . 5_666 ? O7 Yb2 O7 179.996(1) . 5_666 ? O2 Yb2 Yb1 67.78(15) 3 5_666 ? O2 Yb2 Yb1 112.22(15) 7_666 5_666 ? O6 Yb2 Yb1 63.01(14) 5_666 5_666 ? O6 Yb2 Yb1 116.99(14) . 5_666 ? O7 Yb2 Yb1 145.23(12) . 5_666 ? O7 Yb2 Yb1 34.78(12) 5_666 5_666 ? O2 Yb2 Yb1 112.22(15) 3 . ? O2 Yb2 Yb1 67.78(15) 7_666 . ? O6 Yb2 Yb1 116.99(14) 5_666 . ? O6 Yb2 Yb1 63.01(14) . . ? O7 Yb2 Yb1 34.77(12) . . ? O7 Yb2 Yb1 145.22(12) 5_666 . ? Yb1 Yb2 Yb1 180.0 5_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2A C3A -170.4(12) . . . . ? O2 C1 C2A C3A 10(2) . . . . ? C2B C1 C2A C3A 49(27) . . . . ? O1 C1 C2A C7A 7(2) . . . . ? O2 C1 C2A C7A -172.3(13) . . . . ? C2B C1 C2A C7A -133(29) . . . . ? C7A C2A C3A C4A 0.0 . . . . ? C1 C2A C3A C4A 178(2) . . . . ? C2A C3A C4A C5A 0.0 . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C3A C4A C5A C8A -175(4) . . . . ? C4A C5A C6A C7A 0.0 . . . . ? C8A C5A C6A C7A 176(3) . . . . ? C5A C6A C7A C2A 0.0 . . . . ? C3A C2A C7A C6A 0.0 . . . . ? C1 C2A C7A C6A -178(2) . . . . ? C6A C5A C8A C9A 170(4) . . . . ? C4A C5A C8A C9A -15(6) . . . . ? C5A C8A C9A C10A 173(4) . . . . ? C8A C9A C10A C11A 6(6) . . . . ? C8A C9A C10A C15A -171(4) . . . . ? C15A C10A C11A C12A 0.0 . . . . ? C9A C10A C11A C12A -177(3) . . . . ? C15A C10A C11A O3A 178(2) . . . . ? C9A C10A C11A O3A 1(4) . . . . ? C10A C11A C12A C13A 0.0 . . . . ? O3A C11A C12A C13A -178.7(18) . . . . ? C11A C12A C13A C14A 0.0 . . . . ? C11A C12A C13A C18A -179(3) . . . . ? C12A C13A C14A C15A 0.0 . . . . ? C18A C13A C14A C15A 179(4) . . . . ? C12A C13A C14A O4A 179(2) . . . . ? C18A C13A C14A O4A -2(4) . . . . ? C13A C14A C15A C10A 0.0 . . . . ? O4A C14A C15A C10A -179.2(18) . . . . ? C11A C10A C15A C14A 0.0 . . . . ? C9A C10A C15A C14A 178(3) . . . . ? C12A C11A O3A C16A 9(3) . . . . ? C10A C11A O3A C16A -170(3) . . . . ? C15A C14A O4A C17A -7(3) . . . . ? C13A C14A O4A C17A 174(3) . . . . ? C12A C13A C18A C19A -2(7) . . . . ? C14A C13A C18A C19A 179(5) . . . . ? C13A C18A C19A C20 -157(5) . . . . ? O1 C1 C2B C3B 168.4(8) . . . . ? O2 C1 C2B C3B -8.9(14) . . . . ? C2A C1 C2B C3B -151(29) . . . . ? O1 C1 C2B C7B -14.2(13) . . . . ? O2 C1 C2B C7B 168.5(8) . . . . ? C2A C1 C2B C7B 26(28) . . . . ? C7B C2B C3B C4B 0.0 . . . . ? C1 C2B C3B C4B 177.4(14) . . . . ? C2B C3B C4B C5B 0.0 . . . . ? C3B C4B C5B C6B 0.0 . . . . ? C3B C4B C5B C8B -172.5(18) . . . . ? C4B C5B C6B C7B 0.0 . . . . ? C8B C5B C6B C7B 171.7(19) . . . . ? C5B C6B C7B C2B 0.0 . . . . ? C3B C2B C7B C6B 0.0 . . . . ? C1 C2B C7B C6B -177.5(14) . . . . ? C6B C5B C8B C9B 7(3) . . . . ? C4B C5B C8B C9B 179(2) . . . . ? C5B C8B C9B C10B -177(2) . . . . ? C8B C9B C10B C11B 175(2) . . . . ? C8B C9B C10B C15B -5(3) . . . . ? C15B C10B C11B C12B 0.0 . . . . ? C9B C10B C11B C12B 179.9(17) . . . . ? C15B C10B C11B O3B 176.1(16) . . . . ? C9B C10B C11B O3B -4.0(19) . . . . ? C10B C11B C12B C13B 0.0 . . . . ? O3B C11B C12B C13B -176.4(14) . . . . ? C11B C12B C13B C14B 0.0 . . . . ? C11B C12B C13B C18B 166.0(19) . . . . ? C12B C13B C14B C15B 0.0 . . . . ? C18B C13B C14B C15B -166.7(18) . . . . ? C12B C13B C14B O4B -179.6(16) . . . . ? C18B C13B C14B O4B 14(2) . . . . ? C13B C14B C15B C10B 0.0 . . . . ? O4B C14B C15B C10B 179.6(15) . . . . ? C11B C10B C15B C14B 0.0 . . . . ? C9B C10B C15B C14B -179.9(18) . . . . ? C12B C11B O3B C16B -22(3) . . . . ? C10B C11B O3B C16B 162(2) . . . . ? C13B C14B O4B C17B -179.7(17) . . . . ? C15B C14B O4B C17B 1(2) . . . . ? C14B C13B C18B C19B -176(3) . . . . ? C12B C13B C18B C19B 17(4) . . . . ? C13B C18B C19B C20 172(2) . . . . ? C18A C19A C20 C21 174(5) . . . . ? C18A C19A C20 C25 -12(7) . . . . ? C18A C19A C20 C19B 136(11) . . . . ? C18B C19B C20 C21 -176(2) . . . . ? C18B C19B C20 C25 16(4) . . . . ? C18B C19B C20 C19A -26(5) . . . . ? C25 C20 C21 C22 -2(2) . . . . ? C19A C20 C21 C22 172(3) . . . . ? C19B C20 C21 C22 -172.2(16) . . . . ? C20 C21 C22 C23 1(2) . . . . ? C21 C22 C23 C24 -1.1(17) . . . . ? C21 C22 C23 C26 178.6(11) . . . . ? C22 C23 C24 C25 2.0(17) . . . . ? C26 C23 C24 C25 -177.5(10) . . . . ? C21 C20 C25 C24 3(2) . . . . ? C19A C20 C25 C24 -172(2) . . . . ? C19B C20 C25 C24 170.4(18) . . . . ? C23 C24 C25 C20 -3(2) . . . . ? C24 C23 C26 O5 -174.8(9) . . . . ? C22 C23 C26 O5 5.6(12) . . . . ? C24 C23 C26 O6 5.5(12) . . . . ? C22 C23 C26 O6 -174.1(9) . . . . ? O8 C27 C28 C29 -166.0(6) . . . . ? O7 C27 C28 C29 9.9(10) . . . . ? Yb1 C27 C28 C29 -110.6(15) . . . . ? O8 C27 C28 C33 10.0(9) . . . . ? O7 C27 C28 C33 -174.1(6) . . . . ? Yb1 C27 C28 C33 65.5(18) . . . . ? C33 C28 C29 C30 0.0 . . . . ? C27 C28 C29 C30 176.0(8) . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C29 C30 C31 C34 -172.6(11) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C34 C31 C32 C33 172.3(12) . . . . ? C31 C32 C33 C28 0.0 . . . . ? C29 C28 C33 C32 0.0 . . . . ? C27 C28 C33 C32 -176.1(8) . . . . ? C32 C31 C34 C35 -8(3) . . . . ? C30 C31 C34 C35 165(2) . . . . ? C31 C34 C35 C36 176.5(18) . . . . ? C34 C35 C36 C38 -168(3) . . . . ? C34 C35 C36 C37 11(4) . . . . ? C38 C36 C37 C38 -7(5) . . . 5_676 ? C35 C36 C37 C38 174(2) . . . 5_676 ? C37 C36 C38 O9 -178.3(18) . . . . ? C35 C36 C38 O9 0(4) . . . . ? C37 C36 C38 C37 7(5) . . . 5_676 ? C35 C36 C38 C37 -174(2) . . . 5_676 ? C36 C38 O9 C39 176(2) . . . . ? C37 C38 O9 C39 -9(5) 5_676 . . . ? O2 C1 O1 Yb1 -16.8(18) . . . 7_565 ? C2B C1 O1 Yb1 166.2(11) . . . 7_565 ? C2A C1 O1 Yb1 163.5(15) . . . 7_565 ? O1 C1 O2 Yb2 5.7(13) . . . 3_545 ? C2B C1 O2 Yb2 -177.1(8) . . . 3_545 ? C2A C1 O2 Yb2 -174.5(14) . . . 3_545 ? O6 C26 O5 Yb1 -1.9(14) . . . . ? C23 C26 O5 Yb1 178.4(6) . . . . ? O5 C26 O6 Yb2 29.0(13) . . . . ? C23 C26 O6 Yb2 -151.3(6) . . . . ? O8 C27 O7 Yb2 -116.7(7) . . . . ? C28 C27 O7 Yb2 67.4(10) . . . . ? Yb1 C27 O7 Yb2 -129.2(7) . . . . ? O8 C27 O7 Yb1 12.5(6) . . . . ? C28 C27 O7 Yb1 -163.4(7) . . . . ? O7 C27 O8 Yb1 -14.8(7) . . . . ? C28 C27 O8 Yb1 161.2(6) . . . . ? C26 O5 Yb1 O1 -45.2(11) . . . 8_666 ? C26 O5 Yb1 O1 42.7(9) . . . 7_666 ? C26 O5 Yb1 O5 -160.2(9) . . . 2_665 ? C26 O5 Yb1 O8 -85.0(9) . . . . ? C26 O5 Yb1 O8 121.5(9) . . . 2_665 ? C26 O5 Yb1 O7 -33.2(8) . . . . ? C26 O5 Yb1 O7 117.4(8) . . . 2_665 ? C26 O5 Yb1 C27 -59.6(8) . . . . ? C26 O5 Yb1 C27 116.3(8) . . . 2_665 ? C26 O5 Yb1 Yb2 -8.5(8) . . . . ? C26 O5 Yb1 Yb2 147.8(7) . . . 2_665 ? C27 O8 Yb1 O1 -73.4(5) . . . 8_666 ? C27 O8 Yb1 O1 4.8(5) . . . 7_666 ? C27 O8 Yb1 O5 -168.0(5) . . . 2_665 ? C27 O8 Yb1 O5 90.4(5) . . . . ? C27 O8 Yb1 O8 140.8(5) . . . 2_665 ? C27 O8 Yb1 O7 7.8(4) . . . . ? C27 O8 Yb1 O7 -121.1(4) . . . 2_665 ? C27 O8 Yb1 C27 -171.0(5) . . . 2_665 ? C27 O8 Yb1 Yb2 26.3(4) . . . . ? C27 O8 Yb1 Yb2 -118.1(4) . . . 2_665 ? C27 O7 Yb1 O1 79.8(4) . . . 8_666 ? Yb2 O7 Yb1 O1 -133.0(2) . . . 8_666 ? C27 O7 Yb1 O1 170.1(4) . . . 7_666 ? Yb2 O7 Yb1 O1 -42.8(2) . . . 7_666 ? C27 O7 Yb1 O5 -2.3(4) . . . 2_665 ? Yb2 O7 Yb1 O5 144.8(2) . . . 2_665 ? C27 O7 Yb1 O5 -94.9(4) . . . . ? Yb2 O7 Yb1 O5 52.2(2) . . . . ? C27 O7 Yb1 O8 -7.5(4) . . . . ? Yb2 O7 Yb1 O8 139.6(3) . . . . ? C27 O7 Yb1 O8 -141.5(4) . . . 2_665 ? Yb2 O7 Yb1 O8 5.7(4) . . . 2_665 ? C27 O7 Yb1 O7 125.0(4) . . . 2_665 ? Yb2 O7 Yb1 O7 -87.90(18) . . . 2_665 ? Yb2 O7 Yb1 C27 147.1(5) . . . . ? C27 O7 Yb1 C27 171.6(4) . . . 2_665 ? Yb2 O7 Yb1 C27 -41.2(4) . . . 2_665 ? C27 O7 Yb1 Yb2 -147.1(5) . . . . ? C27 O7 Yb1 Yb2 84.3(4) . . . 2_665 ? Yb2 O7 Yb1 Yb2 -128.52(14) . . . 2_665 ? O8 C27 Yb1 O1 100.7(5) . . . 8_666 ? O7 C27 Yb1 O1 -93.1(4) . . . 8_666 ? C28 C27 Yb1 O1 34.8(16) . . . 8_666 ? O8 C27 Yb1 O1 -176.1(4) . . . 7_666 ? O7 C27 Yb1 O1 -9.9(4) . . . 7_666 ? C28 C27 Yb1 O1 118.0(16) . . . 7_666 ? O8 C27 Yb1 O5 11.9(5) . . . 2_665 ? O7 C27 Yb1 O5 178.1(4) . . . 2_665 ? C28 C27 Yb1 O5 -53.9(16) . . . 2_665 ? O8 C27 Yb1 O5 -85.7(5) . . . . ? O7 C27 Yb1 O5 80.5(4) . . . . ? C28 C27 Yb1 O5 -151.6(16) . . . . ? O7 C27 Yb1 O8 166.2(7) . . . . ? C28 C27 Yb1 O8 -65.9(16) . . . . ? O8 C27 Yb1 O8 -82.7(9) . . . 2_665 ? O7 C27 Yb1 O8 83.5(7) . . . 2_665 ? C28 C27 Yb1 O8 -148.6(14) . . . 2_665 ? O8 C27 Yb1 O7 -166.2(7) . . . . ? C28 C27 Yb1 O7 127.9(18) . . . . ? O8 C27 Yb1 O7 99.1(5) . . . 2_665 ? O7 C27 Yb1 O7 -94.7(6) . . . 2_665 ? C28 C27 Yb1 O7 33.2(18) . . . 2_665 ? O8 C27 Yb1 Yb2 -147.3(5) . . . . ? O7 C27 Yb1 Yb2 18.9(3) . . . . ? C28 C27 Yb1 Yb2 146.9(17) . . . . ? O8 C27 Yb1 Yb2 76.6(5) . . . 2_665 ? O7 C27 Yb1 Yb2 -117.3(3) . . . 2_665 ? C28 C27 Yb1 Yb2 10.7(17) . . . 2_665 ? C26 O6 Yb2 O2 92.4(8) . . . 3 ? C26 O6 Yb2 O2 -87.6(8) . . . 7_666 ? C26 O6 Yb2 O7 2.2(8) . . . . ? C26 O6 Yb2 O7 -177.8(8) . . . 5_666 ? C26 O6 Yb2 Yb1 155.9(7) . . . 5_666 ? C26 O6 Yb2 Yb1 -24.1(7) . . . . ? C27 O7 Yb2 O2 -11.7(7) . . . 3 ? Yb1 O7 Yb2 O2 -131.5(2) . . . 3 ? C27 O7 Yb2 O2 168.3(7) . . . 7_666 ? Yb1 O7 Yb2 O2 48.5(2) . . . 7_666 ? C27 O7 Yb2 O6 -104.0(7) . . . 5_666 ? Yb1 O7 Yb2 O6 136.2(2) . . . 5_666 ? C27 O7 Yb2 O6 76.0(7) . . . . ? Yb1 O7 Yb2 O6 -43.8(2) . . . . ? C27 O7 Yb2 Yb1 -60.2(8) . . . 5_666 ? Yb1 O7 Yb2 Yb1 180.0 . . . 5_666 ? C27 O7 Yb2 Yb1 119.8(8) . . . . ? O1 Yb1 Yb2 O2 99.7(2) 8_666 . . 3 ? O1 Yb1 Yb2 O2 -177.6(2) 7_666 . . 3 ? O5 Yb1 Yb2 O2 -4.2(3) 2_665 . . 3 ? O5 Yb1 Yb2 O2 -65.3(2) . . . 3 ? O8 Yb1 Yb2 O2 22.5(2) . . . 3 ? O8 Yb1 Yb2 O2 -122.3(2) 2_665 . . 3 ? O7 Yb1 Yb2 O2 54.1(3) . . . 3 ? O7 Yb1 Yb2 O2 177.2(2) 2_665 . . 3 ? C27 Yb1 Yb2 O2 36.3(3) . . . 3 ? C27 Yb1 Yb2 O2 -149.9(3) 2_665 . . 3 ? Yb2 Yb1 Yb2 O2 136.89(18) 2_665 . . 3 ? O1 Yb1 Yb2 O2 -80.3(2) 8_666 . . 7_666 ? O1 Yb1 Yb2 O2 2.4(2) 7_666 . . 7_666 ? O5 Yb1 Yb2 O2 175.8(3) 2_665 . . 7_666 ? O5 Yb1 Yb2 O2 114.7(2) . . . 7_666 ? O8 Yb1 Yb2 O2 -157.5(2) . . . 7_666 ? O8 Yb1 Yb2 O2 57.7(2) 2_665 . . 7_666 ? O7 Yb1 Yb2 O2 -125.9(3) . . . 7_666 ? O7 Yb1 Yb2 O2 -2.8(2) 2_665 . . 7_666 ? C27 Yb1 Yb2 O2 -143.7(3) . . . 7_666 ? C27 Yb1 Yb2 O2 30.1(3) 2_665 . . 7_666 ? Yb2 Yb1 Yb2 O2 -43.11(18) 2_665 . . 7_666 ? O1 Yb1 Yb2 O6 -5.1(2) 8_666 . . 5_666 ? O1 Yb1 Yb2 O6 77.5(2) 7_666 . . 5_666 ? O5 Yb1 Yb2 O6 -109.1(3) 2_665 . . 5_666 ? O5 Yb1 Yb2 O6 -170.2(2) . . . 5_666 ? O8 Yb1 Yb2 O6 -82.4(2) . . . 5_666 ? O8 Yb1 Yb2 O6 132.8(2) 2_665 . . 5_666 ? O7 Yb1 Yb2 O6 -50.8(3) . . . 5_666 ? O7 Yb1 Yb2 O6 72.3(2) 2_665 . . 5_666 ? C27 Yb1 Yb2 O6 -68.6(2) . . . 5_666 ? C27 Yb1 Yb2 O6 105.2(2) 2_665 . . 5_666 ? Yb2 Yb1 Yb2 O6 32.01(16) 2_665 . . 5_666 ? O1 Yb1 Yb2 O6 174.9(2) 8_666 . . . ? O1 Yb1 Yb2 O6 -102.5(2) 7_666 . . . ? O5 Yb1 Yb2 O6 70.9(3) 2_665 . . . ? O5 Yb1 Yb2 O6 9.8(2) . . . . ? O8 Yb1 Yb2 O6 97.6(2) . . . . ? O8 Yb1 Yb2 O6 -47.2(2) 2_665 . . . ? O7 Yb1 Yb2 O6 129.2(3) . . . . ? O7 Yb1 Yb2 O6 -107.7(2) 2_665 . . . ? C27 Yb1 Yb2 O6 111.4(2) . . . . ? C27 Yb1 Yb2 O6 -74.8(2) 2_665 . . . ? Yb2 Yb1 Yb2 O6 -147.99(16) 2_665 . . . ? O1 Yb1 Yb2 O7 45.7(2) 8_666 . . . ? O1 Yb1 Yb2 O7 128.3(3) 7_666 . . . ? O5 Yb1 Yb2 O7 -58.3(3) 2_665 . . . ? O5 Yb1 Yb2 O7 -119.4(3) . . . . ? O8 Yb1 Yb2 O7 -31.5(2) . . . . ? O8 Yb1 Yb2 O7 -176.4(3) 2_665 . . . ? O7 Yb1 Yb2 O7 123.1(3) 2_665 . . . ? C27 Yb1 Yb2 O7 -17.7(3) . . . . ? C27 Yb1 Yb2 O7 156.1(3) 2_665 . . . ? Yb2 Yb1 Yb2 O7 82.8(2) 2_665 . . . ? O1 Yb1 Yb2 O7 -134.3(2) 8_666 . . 5_666 ? O1 Yb1 Yb2 O7 -51.7(3) 7_666 . . 5_666 ? O5 Yb1 Yb2 O7 121.7(3) 2_665 . . 5_666 ? O5 Yb1 Yb2 O7 60.6(3) . . . 5_666 ? O8 Yb1 Yb2 O7 148.5(2) . . . 5_666 ? O8 Yb1 Yb2 O7 3.6(3) 2_665 . . 5_666 ? O7 Yb1 Yb2 O7 180.0 . . . 5_666 ? O7 Yb1 Yb2 O7 -56.9(3) 2_665 . . 5_666 ? C27 Yb1 Yb2 O7 162.3(3) . . . 5_666 ? C27 Yb1 Yb2 O7 -23.9(3) 2_665 . . 5_666 ? Yb2 Yb1 Yb2 O7 -97.2(2) 2_665 . . 5_666 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.921 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.172 # start Validation Reply Form _vrf_PLAT220__js85_14m ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 8.86 Ratio RESPONSE: Please see the _exptl_special_details section of this cif file. ; _vrf_PLAT222__js85_14m ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.46 Ratio RESPONSE: Please see the _exptl_special_details section of this cif file. ; # end Validation Reply Form