# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C176 H162 N22 O22 Yb6, C2 H6 O, 3(C H4 O), 5(O)' _chemical_formula_sum 'C181 H180 N22 O31 Yb6' _chemical_formula_weight 4197.71 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.599(3) _cell_length_b 15.498(3) _cell_length_c 24.333(5) _cell_angle_alpha 97.48(3) _cell_angle_beta 95.15(5) _cell_angle_gamma 117.74(3) _cell_volume 4759.5(23) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15608 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.51 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 2.988 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.6464 _exptl_absorpt_correction_T_max 0.7960 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25711 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16498 _reflns_number_gt 12492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _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. Restraints: ISOR was applied to all non-hydrogen atoms to allow their Uij components approximate to isotropic behavior. Hydrogen atoms of water molecules were not added. ; _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^)+(0.0165P)^2^+289.2896P] 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 16498 _refine_ls_number_parameters 1123 _refine_ls_number_restraints 755 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0986 _refine_ls_wR_factor_ref 0.2285 _refine_ls_wR_factor_gt 0.2127 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.001 _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 Yb1 Yb 0.25124(5) 0.57431(5) 0.75806(3) 0.01968(19) Uani 1 1 d U . . Yb2 Yb -0.03549(5) 0.39433(5) 0.71347(3) 0.01795(18) Uani 1 1 d U . . Yb3 Yb -0.32524(5) 0.29035(5) 0.66985(3) 0.02087(19) Uani 1 1 d U . . N1 N 0.4312(13) 0.5948(12) 0.9932(7) 0.041(4) Uani 1 1 d U . . H1A H 0.4709 0.5987 1.0228 0.050 Uiso 1 1 calc R . . N2 N 0.4789(11) 0.5974(11) 0.8800(6) 0.031(3) Uani 1 1 d U . . H2B H 0.4334 0.5835 0.8506 0.037 Uiso 1 1 calc R . . N3 N 0.3190(10) 0.6681(11) 0.6818(6) 0.025(3) Uani 1 1 d U . . N4 N 0.3724(11) 0.5316(11) 0.7158(6) 0.029(3) Uani 1 1 d U . . N5 N 0.0131(10) 0.5375(10) 0.6664(6) 0.021(3) Uani 1 1 d U . . N6 N -0.0926(11) 0.5087(10) 0.7590(6) 0.025(3) Uani 1 1 d U . . N7 N -0.0125(10) 0.2891(11) 0.7735(6) 0.027(3) Uani 1 1 d U . . N8 N -0.0471(11) 0.2479(10) 0.6576(6) 0.026(3) Uani 1 1 d U . . N9 N -0.3994(11) 0.3460(11) 0.7479(6) 0.031(3) Uani 1 1 d U . . N10 N -0.4489(11) 0.1496(11) 0.7089(6) 0.031(3) Uani 1 1 d U . . N11 N -0.4708(11) 0.1312(11) 0.5121(6) 0.029(3) Uani 1 1 d U . . H11A H -0.4526 0.1528 0.5479 0.034 Uiso 1 1 calc R . . O1 O 0.5557(13) 0.7029(12) 1.0877(7) 0.060(4) Uani 1 1 d U . . H1B H 0.5983 0.7228 1.1169 0.089 Uiso 1 1 calc R . . O2 O 0.3982(9) 0.6799(9) 0.8169(5) 0.031(3) Uani 1 1 d U . . O3 O 0.2154(9) 0.6967(9) 0.7700(5) 0.031(3) Uani 1 1 d U . . O4 O 0.2778(9) 0.4763(8) 0.8090(5) 0.027(3) Uani 1 1 d U . . O5 O 0.1308(8) 0.4456(8) 0.6885(5) 0.022(2) Uani 1 1 d U . . O6 O -0.1992(8) 0.3028(8) 0.7389(4) 0.022(2) Uani 1 1 d U . . O7 O 0.0918(9) 0.4965(8) 0.7869(5) 0.025(3) Uani 1 1 d U . . O8 O -0.1660(8) 0.3440(8) 0.6385(4) 0.019(2) Uani 1 1 d U . . O9 O -0.2921(10) 0.4410(9) 0.6640(5) 0.031(3) Uani 1 1 d U . . O10 O -0.3439(9) 0.1498(8) 0.6190(5) 0.026(3) Uani 1 1 d U . . O11 O -0.4583(9) 0.2529(8) 0.6009(5) 0.026(3) Uani 1 1 d U . . C1 C 0.5355(16) 0.7755(15) 1.0770(8) 0.039(5) Uani 1 1 d U . . C2 C 0.5857(19) 0.8671(17) 1.1143(10) 0.052(6) Uani 1 1 d U . . H2A H 0.6340 0.8779 1.1456 0.063 Uiso 1 1 calc R . . C3 C 0.5634(19) 0.9406(19) 1.1043(10) 0.057(6) Uani 1 1 d U . . H3A H 0.5950 1.0002 1.1302 0.069 Uiso 1 1 calc R . . C4 C 0.4957(19) 0.9300(18) 1.0571(10) 0.056(6) Uani 1 1 d U . . H4A H 0.4846 0.9824 1.0502 0.068 Uiso 1 1 calc R . . C5 C 0.4445(18) 0.8377(16) 1.0201(9) 0.046(5) Uani 1 1 d U . . H5A H 0.3963 0.8276 0.9890 0.055 Uiso 1 1 calc R . . C6 C 0.4648(16) 0.7602(15) 1.0293(8) 0.039(5) Uani 1 1 d U . . C7 C 0.4131(15) 0.6653(14) 0.9884(8) 0.035(4) Uani 1 1 d U . . H7A H 0.3652 0.6574 0.9577 0.043 Uiso 1 1 calc R . . C8 C 0.3855(17) 0.5077(16) 0.9495(9) 0.044(5) Uani 1 1 d U . . H8A H 0.3214 0.5001 0.9288 0.053 Uiso 1 1 calc R . . H8B H 0.3679 0.4493 0.9659 0.053 Uiso 1 1 calc R . . C9 C 0.4632(16) 0.5166(15) 0.9092(9) 0.040(5) Uani 1 1 d U . . H9A H 0.5297 0.5301 0.9302 0.048 Uiso 1 1 calc R . . H9B H 0.4357 0.4548 0.8822 0.048 Uiso 1 1 calc R . . C10 C 0.5530(14) 0.6863(15) 0.8936(7) 0.037(5) Uani 1 1 d DU . . H10A H 0.6077 0.6965 0.9209 0.044 Uiso 1 1 calc R . . C11 C 0.5653(14) 0.7711(13) 0.8739(7) 0.031(4) Uani 1 1 d U . . C12 C 0.6583(19) 0.8638(18) 0.8937(10) 0.057(6) Uani 1 1 d U . . H12A H 0.7132 0.8670 0.9180 0.068 Uiso 1 1 calc R . . C13 C 0.6676(18) 0.9468(18) 0.8777(10) 0.053(6) Uani 1 1 d U . . H13A H 0.7277 1.0074 0.8917 0.064 Uiso 1 1 calc R . . C14 C 0.5861(16) 0.9416(15) 0.8396(9) 0.041(5) Uani 1 1 d U . . H14A H 0.5935 0.9986 0.8275 0.050 Uiso 1 1 calc R . . C15 C 0.4954(16) 0.8529(14) 0.8203(8) 0.036(5) Uani 1 1 d U . . H15A H 0.4406 0.8513 0.7968 0.044 Uiso 1 1 calc R . . C16 C 0.4846(14) 0.7658(14) 0.8354(7) 0.031(4) Uani 1 1 d U . . C17 C 0.2257(14) 0.7747(13) 0.7506(8) 0.030(4) Uani 1 1 d U . . C18 C 0.1915(17) 0.8364(15) 0.7778(9) 0.045(5) Uani 1 1 d U . . H18A H 0.1639 0.8218 0.8104 0.054 Uiso 1 1 calc R . . C19 C 0.1968(16) 0.9205(15) 0.7580(9) 0.040(5) Uani 1 1 d U . . H19A H 0.1718 0.9596 0.7763 0.048 Uiso 1 1 calc R . . C20 C 0.2420(16) 0.9421(15) 0.7088(9) 0.041(5) Uani 1 1 d U . . H20A H 0.2452 0.9960 0.6945 0.049 Uiso 1 1 calc R . . C21 C 0.2819(16) 0.8854(15) 0.6811(9) 0.043(5) Uani 1 1 d U . . H21A H 0.3128 0.9020 0.6495 0.052 Uiso 1 1 calc R . . C22 C 0.2738(14) 0.8023(13) 0.7023(8) 0.031(4) Uani 1 1 d U . . C23 C 0.3204(14) 0.7494(13) 0.6730(7) 0.029(4) Uani 1 1 d U . . H23A H 0.3555 0.7771 0.6444 0.035 Uiso 1 1 calc R . . C24 C 0.3759(13) 0.6319(14) 0.6466(7) 0.027(4) Uani 1 1 d U . . H24A H 0.4203 0.6836 0.6276 0.033 Uiso 1 1 calc R . . H24B H 0.3261 0.5748 0.6182 0.033 Uiso 1 1 calc R . . C25 C 0.4423(14) 0.6033(14) 0.6831(8) 0.033(4) Uani 1 1 d U . . H25A H 0.4742 0.5728 0.6600 0.039 Uiso 1 1 calc R . . H25B H 0.4978 0.6618 0.7086 0.039 Uiso 1 1 calc R . . C26 C 0.3732(15) 0.4479(15) 0.7135(8) 0.038(5) Uani 1 1 d U . . H26A H 0.4143 0.4361 0.6897 0.045 Uiso 1 1 calc R . . C27 C 0.3163(14) 0.3710(14) 0.7444(8) 0.031(4) Uani 1 1 d U . . C28 C 0.3049(16) 0.2783(15) 0.7274(9) 0.042(5) Uani 1 1 d U . . H28A H 0.3294 0.2658 0.6950 0.050 Uiso 1 1 calc R . . C29 C 0.2596(17) 0.2047(17) 0.7560(10) 0.048(5) Uani 1 1 d U . . H29A H 0.2519 0.1420 0.7432 0.058 Uiso 1 1 calc R . . C30 C 0.2250(16) 0.2235(16) 0.8045(9) 0.044(5) Uani 1 1 d U . . H30A H 0.1962 0.1740 0.8254 0.052 Uiso 1 1 calc R . . C31 C 0.2324(14) 0.3137(14) 0.8223(8) 0.031(4) Uani 1 1 d U . . H31A H 0.2090 0.3245 0.8555 0.037 Uiso 1 1 calc R . . C32 C 0.2743(13) 0.3912(13) 0.7922(8) 0.028(4) Uani 1 1 d U . . C33 C 0.1326(12) 0.4335(12) 0.6324(7) 0.022(4) Uani 1 1 d U . . C34 C 0.1708(13) 0.3734(14) 0.6080(8) 0.030(4) Uani 1 1 d U . . H34A H 0.1953 0.3412 0.6300 0.036 Uiso 1 1 calc R . . C35 C 0.1723(14) 0.3615(14) 0.5504(8) 0.034(4) Uani 1 1 d U . . H35A H 0.1936 0.3179 0.5337 0.041 Uiso 1 1 calc R . . C36 C 0.1430(16) 0.4133(16) 0.5185(9) 0.042(5) Uani 1 1 d U . . H36A H 0.1492 0.4089 0.4807 0.051 Uiso 1 1 calc R . . C37 C 0.1042(13) 0.4721(13) 0.5422(7) 0.028(4) Uani 1 1 d U . . H37A H 0.0810 0.5044 0.5196 0.033 Uiso 1 1 calc R . . C38 C 0.0987(13) 0.4845(13) 0.5992(7) 0.024(4) Uani 1 1 d U . . C39 C 0.0516(12) 0.5455(13) 0.6223(7) 0.025(4) Uani 1 1 d U . . H39A H 0.0508 0.5927 0.6025 0.030 Uiso 1 1 calc R . . C40 C -0.0368(14) 0.5973(13) 0.6818(7) 0.030(4) Uani 1 1 d U . . H40A H -0.1066 0.5667 0.6595 0.036 Uiso 1 1 calc R . . H40B H 0.0036 0.6629 0.6733 0.036 Uiso 1 1 calc R . . C41 C -0.0449(15) 0.6074(14) 0.7438(8) 0.035(4) Uani 1 1 d U . . H41A H 0.0245 0.6490 0.7662 0.042 Uiso 1 1 calc R . . H41B H -0.0875 0.6389 0.7516 0.042 Uiso 1 1 calc R . . C42 C -0.1357(13) 0.4985(13) 0.8022(7) 0.029(4) Uani 1 1 d U . . H42A H -0.1392 0.5529 0.8209 0.034 Uiso 1 1 calc R . . C43 C -0.1801(13) 0.4081(13) 0.8248(7) 0.027(4) Uani 1 1 d U . . C44 C -0.1988(15) 0.4130(16) 0.8815(8) 0.040(5) Uani 1 1 d U . . H44A H -0.1862 0.4736 0.9019 0.047 Uiso 1 1 calc R . . C45 C -0.2337(17) 0.3335(17) 0.9066(9) 0.048(5) Uani 1 1 d U . . H45A H -0.2437 0.3402 0.9438 0.057 Uiso 1 1 calc R . . C46 C -0.2551(16) 0.2400(16) 0.8765(8) 0.042(5) Uani 1 1 d U . . H46A H -0.2777 0.1849 0.8936 0.050 Uiso 1 1 calc R . . C47 C -0.2413(14) 0.2323(15) 0.8202(8) 0.033(4) Uani 1 1 d U . . H47A H -0.2566 0.1706 0.8000 0.039 Uiso 1 1 calc R . . C48 C -0.2063(12) 0.3119(13) 0.7933(7) 0.022(4) Uani 1 1 d U . . C49 C 0.0883(14) 0.4959(14) 0.8428(7) 0.030(4) Uani 1 1 d U . . C50 C 0.1243(14) 0.5858(14) 0.8811(7) 0.031(4) Uani 1 1 d U . . H50A H 0.1485 0.6452 0.8682 0.037 Uiso 1 1 calc R . . C51 C 0.1238(17) 0.5860(17) 0.9374(9) 0.044(5) Uani 1 1 d U . . H51A H 0.1473 0.6459 0.9622 0.053 Uiso 1 1 calc R . . C52 C 0.0897(15) 0.5008(16) 0.9576(8) 0.042(5) Uani 1 1 d U . . H52A H 0.0911 0.5019 0.9960 0.050 Uiso 1 1 calc R . . C53 C 0.0529(15) 0.4123(16) 0.9199(8) 0.039(5) Uani 1 1 d U . . H53A H 0.0356 0.3544 0.9337 0.047 Uiso 1 1 calc R . . C54 C 0.0409(15) 0.4070(13) 0.8633(7) 0.031(4) Uani 1 1 d U . . C55 C 0.0136(14) 0.3098(14) 0.8278(8) 0.034(4) Uani 1 1 d U . . H55A H 0.0153 0.2610 0.8457 0.040 Uiso 1 1 calc R . . C56 C -0.0460(16) 0.1877(15) 0.7446(9) 0.041(5) Uani 1 1 d U . . H56A H -0.1220 0.1486 0.7384 0.050 Uiso 1 1 calc R . . H56B H -0.0168 0.1564 0.7673 0.050 Uiso 1 1 calc R . . C57 C -0.0066(16) 0.1937(15) 0.6887(8) 0.037(5) Uani 1 1 d U . . H57A H 0.0696 0.2283 0.6950 0.045 Uiso 1 1 calc R . . H57B H -0.0314 0.1274 0.6672 0.045 Uiso 1 1 calc R . . C58 C -0.0708(13) 0.2207(13) 0.6047(7) 0.028(4) Uani 1 1 d U . . H58A H -0.0543 0.1730 0.5887 0.034 Uiso 1 1 calc R . . C59 C -0.1220(13) 0.2570(12) 0.5655(7) 0.023(4) Uani 1 1 d U . . C60 C -0.1295(16) 0.2231(15) 0.5071(8) 0.039(5) Uani 1 1 d U . . H60A H -0.0982 0.1853 0.4953 0.047 Uiso 1 1 calc R . . C61 C -0.1826(15) 0.2468(15) 0.4695(8) 0.039(5) Uani 1 1 d U . . H61A H -0.1896 0.2235 0.4313 0.047 Uiso 1 1 calc R . . C62 C -0.2278(15) 0.3062(14) 0.4870(8) 0.037(5) Uani 1 1 d U . . H62A H -0.2634 0.3232 0.4605 0.044 Uiso 1 1 calc R . . C63 C -0.2189(15) 0.3396(15) 0.5443(8) 0.036(4) Uani 1 1 d U . . H63A H -0.2488 0.3792 0.5551 0.043 Uiso 1 1 calc R . . C64 C -0.1681(13) 0.3167(12) 0.5854(7) 0.026(4) Uani 1 1 d U . . C65 C -0.3006(14) 0.5164(14) 0.6871(8) 0.033(4) Uani 1 1 d U . . C66 C -0.2705(16) 0.6001(16) 0.6623(10) 0.047(5) Uani 1 1 d U . . H66A H -0.2528 0.5985 0.6266 0.056 Uiso 1 1 calc R . . C67 C -0.2669(15) 0.6870(15) 0.6912(9) 0.041(5) Uani 1 1 d U . . H67A H -0.2410 0.7436 0.6754 0.050 Uiso 1 1 calc R . . C68 C -0.3002(17) 0.6905(17) 0.7416(9) 0.047(5) Uani 1 1 d U . . H68A H -0.2975 0.7482 0.7603 0.057 Uiso 1 1 calc R . . C69 C -0.3371(16) 0.6071(16) 0.7634(10) 0.046(5) Uani 1 1 d U . . H69A H -0.3618 0.6079 0.7973 0.055 Uiso 1 1 calc R . . C70 C -0.3401(14) 0.5179(14) 0.7370(8) 0.032(4) Uani 1 1 d U . . C71 C -0.3887(15) 0.4320(15) 0.7631(8) 0.039(5) Uani 1 1 d U . . H71A H -0.4156 0.4413 0.7952 0.047 Uiso 1 1 calc R . . C72 C -0.4575(15) 0.2730(14) 0.7796(8) 0.036(5) Uani 1 1 d U . . H72A H -0.5049 0.2910 0.7972 0.043 Uiso 1 1 calc R . . H72B H -0.4095 0.2712 0.8091 0.043 Uiso 1 1 calc R . . C73 C -0.5213(15) 0.1693(14) 0.7412(7) 0.033(4) Uani 1 1 d U . . H73A H -0.5522 0.1190 0.7638 0.040 Uiso 1 1 calc R . . H73B H -0.5775 0.1672 0.7156 0.040 Uiso 1 1 calc R . . C74 C -0.4500(14) 0.0675(14) 0.7088(7) 0.029(4) Uani 1 1 d U . . H74A H -0.4944 0.0264 0.7304 0.034 Uiso 1 1 calc R . . C75 C -0.3900(14) 0.0296(13) 0.6787(7) 0.028(4) Uani 1 1 d U . . C76 C -0.3860(17) -0.0524(16) 0.6922(9) 0.044(5) Uani 1 1 d U . . H76A H -0.4195 -0.0806 0.7211 0.053 Uiso 1 1 calc R . . C77 C -0.3341(17) -0.0932(16) 0.6642(9) 0.046(5) Uani 1 1 d U . . H77A H -0.3310 -0.1481 0.6737 0.055 Uiso 1 1 calc R . . C78 C -0.2878(13) -0.0514(13) 0.6227(7) 0.028(4) Uani 1 1 d U . . H78A H -0.2520 -0.0786 0.6036 0.034 Uiso 1 1 calc R . . C79 C -0.2900(13) 0.0285(13) 0.6065(7) 0.026(4) Uani 1 1 d U . . H79A H -0.2584 0.0527 0.5763 0.032 Uiso 1 1 calc R . . C80 C -0.3395(13) 0.0745(13) 0.6352(7) 0.028(4) Uani 1 1 d U . . C81 C -0.4954(12) 0.2923(12) 0.5672(7) 0.023(4) Uani 1 1 d U . . C82 C -0.5145(13) 0.3709(13) 0.5877(8) 0.028(4) Uani 1 1 d U . . H82A H -0.4972 0.3985 0.6260 0.033 Uiso 1 1 calc R . . C83 C -0.5586(16) 0.4061(15) 0.5511(9) 0.040(5) Uani 1 1 d U . . H83A H -0.5707 0.4579 0.5652 0.048 Uiso 1 1 calc R . . C84 C -0.5859(15) 0.3685(14) 0.4943(8) 0.037(5) Uani 1 1 d U . . H84A H -0.6182 0.3932 0.4711 0.044 Uiso 1 1 calc R . . C85 C -0.5662(14) 0.2966(13) 0.4723(8) 0.031(4) Uani 1 1 d U . . H85A H -0.5832 0.2725 0.4337 0.037 Uiso 1 1 calc R . . C86 C -0.5193(13) 0.2569(13) 0.5079(7) 0.027(4) Uani 1 1 d U . . C87 C -0.5051(13) 0.1769(13) 0.4838(7) 0.028(4) Uani 1 1 d U . . H87A H -0.5218 0.1564 0.4449 0.034 Uiso 1 1 calc R . . C88 C -0.4596(13) 0.0455(12) 0.4891(7) 0.026(4) Uani 1 1 d U . . H88A H -0.3888 0.0576 0.5014 0.039 Uiso 1 1 calc R . . H88B H -0.4731 0.0331 0.4483 0.039 Uiso 1 1 calc R . . C89 C 0.026(3) 0.072(2) 0.3474(16) 0.038(9) Uani 0.50 1 d PDU . . H89A H -0.0282 0.0490 0.3152 0.057 Uiso 0.50 1 calc PR . . H89B H 0.0066 0.0238 0.3711 0.057 Uiso 0.50 1 calc PR . . H89C H 0.0906 0.0826 0.3352 0.057 Uiso 0.50 1 calc PR . . C90 C 0.042(3) 0.172(2) 0.3808(17) 0.051(11) Uani 0.50 1 d PDU . . H90A H -0.0086 0.1604 0.4062 0.061 Uiso 0.50 1 calc PR . . H90B H 0.0358 0.2134 0.3558 0.061 Uiso 0.50 1 calc PR . . O13 O 0.351(3) 0.060(3) 0.6004(18) 0.100 Uiso 0.50 1 d PD . . H13B H 0.3407 0.0594 0.6330 0.120 Uiso 0.50 1 calc PR . . C92 C 0.8486(14) 0.777(2) 1.0066(12) 0.069(7) Uani 1 1 d DU . . H92A H 0.8793 0.7357 1.0128 0.083 Uiso 1 1 calc R . . H92B H 0.8775 0.8336 1.0371 0.083 Uiso 1 1 calc R . . H92C H 0.8637 0.7999 0.9719 0.104 Uiso 1 1 calc R . . O12 O 0.155(2) 0.217(2) 0.4133(13) 0.061(9) Uani 0.50 1 d PDU . . H12B H 0.1710 0.2704 0.4334 0.091 Uiso 0.50 1 calc PR . . C91 C 0.260(3) 0.063(3) 0.5642(18) 0.051(11) Uani 0.50 1 d PDU . . H91B H 0.2003 0.0415 0.5828 0.061 Uiso 0.50 1 calc PR . . H91C H 0.2418 0.0206 0.5281 0.061 Uiso 0.50 1 calc PR . . H91A H 0.2826 0.1303 0.5592 0.061 Uiso 0.50 1 calc PR . . O14 O 0.7299(13) 0.7182(17) 1.0034(8) 0.100 Uiso 1 1 d D . . H14 H 0.7058 0.6683 0.9787 0.120 Uiso 1 1 calc R . . O15 O 0.1222(19) 0.0677(17) 0.5100(10) 0.040(6) Uani 0.55 1 d PU . . O15' O 0.079(2) 0.090(2) 0.4457(13) 0.042(7) Uani 0.45 1 d PU . . O16 O 0.991(4) 0.938(4) 1.095(2) 0.145(17) Uani 0.60 1 d PU . . O16' O 0.800(5) 1.111(5) 1.037(3) 0.12(2) Uani 0.40 1 d PU . . O17 O 1.120(6) 0.956(6) 1.011(3) 0.08(2) Uani 0.25 1 d PU . . O17' O 1.043(7) 1.040(7) 1.167(4) 0.10(3) Uani 0.25 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.0185(4) 0.0195(4) 0.0215(4) 0.0023(3) -0.0005(3) 0.0107(3) Yb2 0.0167(3) 0.0193(4) 0.0186(4) 0.0013(3) 0.0007(3) 0.0103(3) Yb3 0.0184(4) 0.0216(4) 0.0222(4) -0.0015(3) -0.0009(3) 0.0114(3) N1 0.046(8) 0.042(8) 0.034(7) 0.010(6) 0.000(6) 0.020(6) N2 0.028(6) 0.037(7) 0.031(7) 0.004(5) -0.007(5) 0.021(6) N3 0.014(6) 0.027(7) 0.026(6) -0.002(5) -0.003(5) 0.007(5) N4 0.027(6) 0.027(7) 0.036(7) 0.005(5) 0.003(5) 0.017(5) N5 0.014(6) 0.021(6) 0.031(6) 0.008(5) 0.002(5) 0.010(5) N6 0.021(6) 0.023(6) 0.035(7) 0.002(5) 0.007(5) 0.015(5) N7 0.017(6) 0.029(7) 0.031(7) 0.006(5) -0.001(5) 0.008(5) N8 0.028(6) 0.023(6) 0.030(7) 0.003(5) 0.008(5) 0.015(5) N9 0.026(6) 0.033(7) 0.035(7) 0.001(5) 0.000(5) 0.018(6) N10 0.025(6) 0.030(7) 0.033(7) -0.002(5) -0.001(5) 0.013(5) N11 0.030(6) 0.026(7) 0.026(6) -0.007(5) 0.000(5) 0.014(5) O1 0.071(8) 0.061(8) 0.056(8) 0.013(6) -0.008(6) 0.043(7) O2 0.028(6) 0.028(6) 0.029(6) 0.005(5) -0.004(4) 0.009(5) O3 0.032(6) 0.027(6) 0.042(6) 0.015(5) 0.010(5) 0.018(5) O4 0.030(6) 0.021(5) 0.037(6) 0.009(5) 0.005(5) 0.016(5) O5 0.021(5) 0.027(6) 0.025(5) 0.006(4) 0.003(4) 0.016(4) O6 0.021(5) 0.025(5) 0.018(5) 0.002(4) 0.002(4) 0.011(4) O7 0.024(5) 0.025(6) 0.027(5) 0.007(4) 0.007(4) 0.012(4) O8 0.021(5) 0.018(5) 0.019(5) 0.000(4) -0.003(4) 0.013(4) O9 0.035(6) 0.026(6) 0.034(6) 0.004(5) 0.001(5) 0.018(5) O10 0.023(5) 0.023(6) 0.032(6) 0.002(4) 0.002(4) 0.012(5) O11 0.025(5) 0.025(6) 0.032(6) -0.001(4) -0.004(4) 0.018(5) C1 0.040(8) 0.038(8) 0.037(8) 0.008(6) 0.004(6) 0.017(7) C2 0.055(9) 0.052(9) 0.056(9) 0.008(7) 0.009(7) 0.032(7) C3 0.061(10) 0.056(10) 0.058(10) 0.005(7) 0.018(8) 0.031(8) C4 0.064(10) 0.052(9) 0.062(10) 0.015(7) 0.015(8) 0.034(8) C5 0.053(9) 0.044(9) 0.044(9) 0.014(7) 0.003(7) 0.027(7) C6 0.041(8) 0.040(8) 0.036(8) 0.010(6) 0.012(6) 0.018(7) C7 0.033(8) 0.036(8) 0.039(8) 0.011(6) 0.000(6) 0.018(6) C8 0.046(9) 0.041(8) 0.047(9) 0.015(7) 0.002(7) 0.022(7) C9 0.042(8) 0.036(8) 0.045(8) 0.011(7) -0.009(6) 0.023(7) C10 0.033(8) 0.037(8) 0.039(8) 0.003(6) -0.001(6) 0.018(7) C11 0.030(7) 0.025(7) 0.030(7) 0.003(6) -0.004(6) 0.010(6) C12 0.049(9) 0.059(10) 0.060(10) 0.015(8) 0.001(7) 0.025(7) C13 0.048(9) 0.044(9) 0.060(9) 0.007(7) -0.001(7) 0.019(7) C14 0.039(8) 0.033(8) 0.047(8) 0.010(7) 0.003(7) 0.013(7) C15 0.042(8) 0.031(8) 0.035(8) 0.011(6) 0.001(6) 0.017(6) C16 0.032(8) 0.029(8) 0.030(7) 0.006(6) 0.007(6) 0.013(6) C17 0.029(7) 0.026(7) 0.037(8) 0.004(6) 0.005(6) 0.014(6) C18 0.052(9) 0.033(8) 0.053(9) 0.010(7) 0.013(7) 0.023(7) C19 0.042(8) 0.035(8) 0.047(9) -0.002(6) -0.007(7) 0.026(7) C20 0.044(8) 0.028(8) 0.051(9) 0.007(7) -0.003(7) 0.018(7) C21 0.043(8) 0.039(8) 0.047(9) 0.015(7) -0.001(7) 0.020(7) C22 0.033(8) 0.027(7) 0.031(7) 0.006(6) -0.004(6) 0.014(6) C23 0.027(7) 0.031(8) 0.027(7) 0.009(6) 0.000(6) 0.012(6) C24 0.021(7) 0.031(8) 0.030(7) 0.005(6) 0.008(6) 0.013(6) C25 0.028(7) 0.036(8) 0.037(8) 0.004(6) 0.009(6) 0.019(6) C26 0.038(8) 0.039(8) 0.038(8) -0.002(6) 0.007(6) 0.022(7) C27 0.028(7) 0.033(8) 0.041(8) 0.005(6) 0.000(6) 0.024(6) C28 0.041(8) 0.038(8) 0.049(9) 0.002(7) 0.001(7) 0.024(7) C29 0.051(9) 0.044(9) 0.060(9) 0.002(7) 0.009(7) 0.033(7) C30 0.042(8) 0.040(8) 0.056(9) 0.018(7) 0.000(7) 0.025(7) C31 0.029(7) 0.032(8) 0.036(8) 0.008(6) -0.002(6) 0.018(6) C32 0.022(7) 0.021(7) 0.039(8) 0.004(6) 0.001(6) 0.010(6) C33 0.019(7) 0.024(7) 0.024(7) 0.006(6) 0.001(5) 0.009(6) C34 0.025(7) 0.033(8) 0.034(8) 0.006(6) -0.001(6) 0.016(6) C35 0.028(7) 0.038(8) 0.041(8) 0.006(6) 0.009(6) 0.020(6) C36 0.044(8) 0.045(9) 0.035(8) 0.011(7) 0.013(7) 0.018(7) C37 0.022(7) 0.031(8) 0.026(7) 0.004(6) 0.000(6) 0.011(6) C38 0.022(7) 0.025(7) 0.028(7) 0.008(6) 0.001(5) 0.013(6) C39 0.019(7) 0.029(7) 0.029(7) 0.008(6) 0.004(6) 0.012(6) C40 0.031(7) 0.026(7) 0.036(8) 0.008(6) 0.008(6) 0.015(6) C41 0.033(8) 0.037(8) 0.041(8) 0.006(6) 0.010(6) 0.022(6) C42 0.026(7) 0.026(7) 0.034(8) -0.001(6) -0.001(6) 0.016(6) C43 0.025(7) 0.031(8) 0.020(7) -0.004(6) -0.002(6) 0.012(6) C44 0.037(8) 0.043(8) 0.038(8) 0.002(7) 0.005(6) 0.021(7) C45 0.045(9) 0.054(9) 0.038(8) 0.013(7) 0.007(7) 0.018(7) C46 0.041(8) 0.044(9) 0.033(8) 0.011(7) 0.010(6) 0.012(7) C47 0.025(7) 0.039(8) 0.034(8) 0.007(6) 0.001(6) 0.016(6) C48 0.018(6) 0.030(7) 0.020(7) 0.004(6) 0.008(5) 0.011(6) C49 0.033(7) 0.034(8) 0.024(7) 0.003(6) 0.001(6) 0.019(6) C50 0.030(7) 0.033(8) 0.026(7) -0.001(6) 0.000(6) 0.015(6) C51 0.046(9) 0.048(9) 0.037(8) 0.002(7) 0.004(7) 0.023(7) C52 0.035(8) 0.057(9) 0.031(8) 0.008(7) 0.008(6) 0.019(7) C53 0.040(8) 0.045(9) 0.037(8) 0.010(7) 0.001(6) 0.024(7) C54 0.037(5) 0.028(5) 0.022(5) 0.002(4) 0.008(4) 0.011(4) C55 0.026(7) 0.034(8) 0.035(8) 0.016(6) 0.003(6) 0.008(6) C56 0.036(8) 0.039(8) 0.046(8) 0.008(7) 0.000(6) 0.018(7) C57 0.037(8) 0.037(8) 0.042(8) 0.008(6) 0.005(6) 0.022(7) C58 0.025(7) 0.024(7) 0.036(8) -0.007(6) 0.010(6) 0.014(6) C59 0.024(7) 0.020(7) 0.021(7) 0.002(5) 0.009(6) 0.006(6) C60 0.039(8) 0.039(8) 0.035(8) 0.007(6) 0.008(6) 0.016(7) C61 0.041(8) 0.037(8) 0.030(8) 0.000(6) 0.005(6) 0.014(7) C62 0.039(8) 0.037(8) 0.026(7) 0.014(6) -0.003(6) 0.012(6) C63 0.034(8) 0.036(8) 0.033(8) 0.008(6) 0.001(6) 0.013(6) C64 0.025(7) 0.017(7) 0.030(7) 0.001(6) -0.001(6) 0.008(6) C65 0.026(7) 0.029(8) 0.046(8) 0.002(6) -0.001(6) 0.017(6) C66 0.040(8) 0.044(9) 0.061(9) 0.016(7) -0.002(7) 0.023(7) C67 0.034(8) 0.033(8) 0.058(9) 0.005(7) 0.000(7) 0.018(7) C68 0.047(9) 0.044(9) 0.057(9) -0.003(7) -0.002(7) 0.032(7) C69 0.042(8) 0.048(9) 0.056(9) -0.002(7) 0.002(7) 0.032(7) C70 0.027(7) 0.027(8) 0.041(8) 0.001(6) -0.003(6) 0.017(6) C71 0.034(8) 0.045(9) 0.040(8) -0.002(7) 0.004(6) 0.025(7) C72 0.032(8) 0.040(8) 0.035(8) -0.001(6) 0.011(6) 0.018(6) C73 0.039(8) 0.037(8) 0.025(7) 0.004(6) 0.008(6) 0.019(6) C74 0.026(7) 0.031(8) 0.026(7) 0.002(6) 0.000(6) 0.014(6) C75 0.029(7) 0.026(7) 0.035(8) 0.005(6) 0.005(6) 0.018(6) C76 0.047(9) 0.044(9) 0.044(9) 0.013(7) 0.004(7) 0.025(7) C77 0.052(9) 0.040(8) 0.057(9) 0.015(7) -0.003(7) 0.031(7) C78 0.028(7) 0.029(7) 0.035(8) -0.003(6) -0.003(6) 0.023(6) C79 0.020(7) 0.033(8) 0.026(7) -0.003(6) -0.005(5) 0.016(6) C80 0.025(7) 0.025(7) 0.030(7) 0.007(6) 0.003(6) 0.009(6) C81 0.016(6) 0.018(7) 0.031(7) 0.006(6) -0.001(5) 0.005(5) C82 0.022(7) 0.028(7) 0.032(7) 0.000(6) -0.003(6) 0.013(6) C83 0.039(8) 0.039(8) 0.049(9) 0.009(7) 0.011(7) 0.024(7) C84 0.034(8) 0.029(8) 0.043(8) 0.011(6) 0.002(6) 0.012(6) C85 0.027(7) 0.030(8) 0.034(8) 0.008(6) 0.000(6) 0.013(6) C86 0.022(7) 0.030(7) 0.032(7) 0.006(6) 0.003(6) 0.015(6) C87 0.027(7) 0.027(7) 0.026(7) 0.004(6) -0.001(6) 0.011(6) C88 0.029(7) 0.026(7) 0.027(7) 0.001(6) 0.000(6) 0.018(6) C89 0.037(12) 0.039(12) 0.043(12) 0.008(9) -0.006(8) 0.023(9) C90 0.057(14) 0.048(14) 0.055(14) 0.016(9) 0.014(9) 0.030(10) C92 0.065(10) 0.074(11) 0.071(11) 0.030(8) 0.005(8) 0.033(8) O12 0.064(12) 0.050(11) 0.059(12) 0.002(8) 0.018(9) 0.022(8) C91 0.056(14) 0.043(14) 0.048(14) 0.013(9) -0.001(9) 0.021(10) O15 0.048(9) 0.032(9) 0.047(10) -0.006(7) -0.006(7) 0.030(8) O15' 0.040(10) 0.039(11) 0.052(11) 0.001(8) 0.008(8) 0.024(8) O16 0.140(19) 0.144(19) 0.143(19) 0.028(10) 0.038(10) 0.060(12) O16' 0.12(2) 0.13(2) 0.12(2) 0.024(11) 0.019(10) 0.058(14) O17 0.08(2) 0.08(2) 0.09(2) 0.011(11) 0.012(11) 0.043(14) O17' 0.10(3) 0.10(3) 0.10(3) 0.017(11) 0.016(11) 0.046(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O3 2.184(12) . ? Yb1 O2 2.214(12) . ? Yb1 O4 2.224(11) . ? Yb1 O5 2.294(11) . ? Yb1 O7 2.295(11) . ? Yb1 N4 2.422(14) . ? Yb1 N3 2.496(14) . ? Yb1 C49 3.198(18) . ? Yb1 Yb2 3.743(2) . ? Yb2 O7 2.253(12) . ? Yb2 O8 2.278(10) . ? Yb2 O6 2.332(11) . ? Yb2 O5 2.343(11) . ? Yb2 N8 2.414(14) . ? Yb2 N7 2.439(14) . ? Yb2 N5 2.467(13) . ? Yb2 N6 2.468(13) . ? Yb2 C33 3.174(16) . ? Yb2 C48 3.189(15) . ? Yb2 Yb3 3.7442(16) . ? Yb3 O9 2.181(12) . ? Yb3 O10 2.244(11) . ? Yb3 O11 2.246(11) . ? Yb3 O6 2.296(11) . ? Yb3 O8 2.316(11) . ? Yb3 N10 2.470(16) . ? Yb3 N9 2.517(15) . ? Yb3 C64 3.138(18) . ? N1 C7 1.25(2) . ? N1 C8 1.44(3) . ? N1 H1A 0.8600 . ? N2 C10 1.27(2) . ? N2 C9 1.46(2) . ? N2 H2B 0.8600 . ? N3 C23 1.30(2) . ? N3 C24 1.47(2) . ? N4 C26 1.30(2) . ? N4 C25 1.49(2) . ? N5 C39 1.25(2) . ? N5 C40 1.45(2) . ? N6 C42 1.26(2) . ? N6 C41 1.47(2) . ? N7 C55 1.30(2) . ? N7 C56 1.46(2) . ? N8 C58 1.26(2) . ? N8 C57 1.47(2) . ? N9 C71 1.27(2) . ? N9 C72 1.43(2) . ? N10 C74 1.26(2) . ? N10 C73 1.49(2) . ? N11 C87 1.27(2) . ? N11 C88 1.46(2) . ? N11 H11A 0.8600 . ? O1 C1 1.34(2) . ? O1 H1B 0.8200 . ? O2 C16 1.32(2) . ? O3 C17 1.30(2) . ? O4 C32 1.31(2) . ? O5 C33 1.357(19) . ? O6 C48 1.332(19) . ? O7 C49 1.37(2) . ? O8 C64 1.30(2) . ? O9 C65 1.29(2) . ? O10 C80 1.31(2) . ? O11 C81 1.301(19) . ? C1 C2 1.40(3) . ? C1 C6 1.40(3) . ? C2 C3 1.37(3) . ? C2 H2A 0.9300 . ? C3 C4 1.38(3) . ? C3 H3A 0.9300 . ? C4 C5 1.40(3) . ? C4 H4A 0.9300 . ? C5 C6 1.40(3) . ? C5 H5A 0.9300 . ? C6 C7 1.48(3) . ? C7 H7A 0.9300 . ? C8 C9 1.53(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.40(3) . ? C10 H10A 0.9300 . ? C11 C16 1.40(2) . ? C11 C12 1.42(3) . ? C12 C13 1.34(3) . ? C12 H12A 0.9300 . ? C13 C14 1.40(3) . ? C13 H13A 0.9300 . ? C14 C15 1.37(3) . ? C14 H14A 0.9300 . ? C15 C16 1.39(3) . ? C15 H15A 0.9300 . ? C17 C18 1.39(3) . ? C17 C22 1.43(3) . ? C18 C19 1.42(3) . ? C18 H18A 0.9300 . ? C19 C20 1.42(3) . ? C19 H19A 0.9300 . ? C20 C21 1.40(3) . ? C20 H20A 0.9300 . ? C21 C22 1.41(3) . ? C21 H21A 0.9300 . ? C22 C23 1.45(3) . ? C23 H23A 0.9300 . ? C24 C25 1.51(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.45(3) . ? C26 H26A 0.9300 . ? C27 C28 1.37(3) . ? C27 C32 1.43(3) . ? C28 C29 1.35(3) . ? C28 H28A 0.9300 . ? C29 C30 1.37(3) . ? C29 H29A 0.9300 . ? C30 C31 1.36(3) . ? C30 H30A 0.9300 . ? C31 C32 1.41(3) . ? C31 H31A 0.9300 . ? C33 C34 1.39(2) . ? C33 C38 1.41(2) . ? C34 C35 1.39(3) . ? C34 H34A 0.9300 . ? C35 C36 1.36(3) . ? C35 H35A 0.9300 . ? C36 C37 1.37(3) . ? C36 H36A 0.9300 . ? C37 C38 1.39(2) . ? C37 H37A 0.9300 . ? C38 C39 1.49(2) . ? C39 H39A 0.9300 . ? C40 C41 1.52(3) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.45(3) . ? C42 H42A 0.9300 . ? C43 C44 1.43(3) . ? C43 C48 1.44(2) . ? C44 C45 1.35(3) . ? C44 H44A 0.9300 . ? C45 C46 1.41(3) . ? C45 H45A 0.9300 . ? C46 C47 1.40(3) . ? C46 H46A 0.9300 . ? C47 C48 1.38(2) . ? C47 H47A 0.9300 . ? C49 C50 1.41(3) . ? C49 C54 1.41(3) . ? C50 C51 1.37(3) . ? C50 H50A 0.9300 . ? C51 C52 1.35(3) . ? C51 H51A 0.9300 . ? C52 C53 1.38(3) . ? C52 H52A 0.9300 . ? C53 C54 1.36(3) . ? C53 H53A 0.9300 . ? C54 C55 1.49(3) . ? C55 H55A 0.9300 . ? C56 C57 1.52(3) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.48(2) . ? C58 H58A 0.9300 . ? C59 C60 1.43(2) . ? C59 C64 1.44(2) . ? C60 C61 1.34(3) . ? C60 H60A 0.9300 . ? C61 C62 1.41(3) . ? C61 H61A 0.9300 . ? C62 C63 1.40(3) . ? C62 H62A 0.9300 . ? C63 C64 1.37(2) . ? C63 H63A 0.9300 . ? C65 C70 1.39(3) . ? C65 C66 1.40(3) . ? C66 C67 1.41(3) . ? C66 H66A 0.9300 . ? C67 C68 1.36(3) . ? C67 H67A 0.9300 . ? C68 C69 1.35(3) . ? C68 H68A 0.9300 . ? C69 C70 1.43(3) . ? C69 H69A 0.9300 . ? C70 C71 1.45(3) . ? C71 H71A 0.9300 . ? C72 C73 1.54(3) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.46(2) . ? C74 H74A 0.9300 . ? C75 C76 1.38(3) . ? C75 C80 1.42(2) . ? C76 C77 1.37(3) . ? C76 H76A 0.9300 . ? C77 C78 1.34(3) . ? C77 H77A 0.9300 . ? C78 C79 1.36(2) . ? C78 H78A 0.9300 . ? C79 C80 1.40(2) . ? C79 H79A 0.9300 . ? C81 C82 1.41(2) . ? C81 C86 1.42(2) . ? C82 C83 1.36(3) . ? C82 H82A 0.9300 . ? C83 C84 1.37(3) . ? C83 H83A 0.9300 . ? C84 C85 1.33(3) . ? C84 H84A 0.9300 . ? C85 C86 1.42(2) . ? C85 H85A 0.9300 . ? C86 C87 1.41(2) . ? C87 H87A 0.9300 . ? C88 C88 1.56(3) 2_456 ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C89 C90 1.548(10) . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 O12 1.549(10) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? O13 C91 1.551(10) . ? O13 H13B 0.8200 . ? C92 O14 1.525(10) . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? O12 H12B 0.8200 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C91 H91A 0.9600 . ? O14 H14 0.8200 . ? O15 O15' 1.77(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Yb1 O2 84.1(5) . . ? O3 Yb1 O4 138.5(4) . . ? O2 Yb1 O4 77.4(4) . . ? O3 Yb1 O5 111.4(4) . . ? O2 Yb1 O5 162.6(4) . . ? O4 Yb1 O5 94.4(4) . . ? O3 Yb1 O7 80.1(4) . . ? O2 Yb1 O7 122.8(4) . . ? O4 Yb1 O7 79.4(4) . . ? O5 Yb1 O7 69.6(4) . . ? O3 Yb1 N4 139.5(5) . . ? O2 Yb1 N4 80.7(5) . . ? O4 Yb1 N4 73.5(5) . . ? O5 Yb1 N4 82.3(4) . . ? O7 Yb1 N4 139.0(5) . . ? O3 Yb1 N3 74.3(5) . . ? O2 Yb1 N3 90.0(4) . . ? O4 Yb1 N3 141.4(4) . . ? O5 Yb1 N3 86.9(4) . . ? O7 Yb1 N3 135.7(4) . . ? N4 Yb1 N3 68.4(5) . . ? O3 Yb1 C49 81.5(5) . . ? O2 Yb1 C49 101.6(4) . . ? O4 Yb1 C49 66.7(4) . . ? O5 Yb1 C49 88.9(4) . . ? O7 Yb1 C49 21.8(4) . . ? N4 Yb1 C49 138.4(5) . . ? N3 Yb1 C49 151.9(4) . . ? O3 Yb1 Yb2 89.8(3) . . ? O2 Yb1 Yb2 157.0(3) . . ? O4 Yb1 Yb2 93.1(3) . . ? O5 Yb1 Yb2 36.6(3) . . ? O7 Yb1 Yb2 34.3(3) . . ? N4 Yb1 Yb2 117.0(4) . . ? N3 Yb1 Yb2 109.6(3) . . ? C49 Yb1 Yb2 55.5(3) . . ? O7 Yb2 O8 158.9(4) . . ? O7 Yb2 O6 113.7(4) . . ? O8 Yb2 O6 69.6(4) . . ? O7 Yb2 O5 69.4(4) . . ? O8 Yb2 O5 113.5(4) . . ? O6 Yb2 O5 164.2(4) . . ? O7 Yb2 N8 125.9(4) . . ? O8 Yb2 N8 73.5(4) . . ? O6 Yb2 N8 92.1(4) . . ? O5 Yb2 N8 74.7(4) . . ? O7 Yb2 N7 73.2(4) . . ? O8 Yb2 N7 126.3(4) . . ? O6 Yb2 N7 74.6(4) . . ? O5 Yb2 N7 92.3(4) . . ? N8 Yb2 N7 69.2(5) . . ? O7 Yb2 N5 88.6(4) . . ? O8 Yb2 N5 73.8(4) . . ? O6 Yb2 N5 124.9(4) . . ? O5 Yb2 N5 69.8(4) . . ? N8 Yb2 N5 115.4(5) . . ? N7 Yb2 N5 158.2(4) . . ? O7 Yb2 N6 73.0(4) . . ? O8 Yb2 N6 89.6(4) . . ? O6 Yb2 N6 70.4(4) . . ? O5 Yb2 N6 124.1(4) . . ? N8 Yb2 N6 159.2(5) . . ? N7 Yb2 N6 114.4(5) . . ? N5 Yb2 N6 69.5(5) . . ? O7 Yb2 C33 91.1(4) . . ? O8 Yb2 C33 90.9(4) . . ? O6 Yb2 C33 153.4(4) . . ? O5 Yb2 C33 22.7(4) . . ? N8 Yb2 C33 64.3(5) . . ? N7 Yb2 C33 105.5(4) . . ? N5 Yb2 C33 62.2(4) . . ? N6 Yb2 C33 129.3(5) . . ? O7 Yb2 C48 92.2(4) . . ? O8 Yb2 C48 90.1(4) . . ? O6 Yb2 C48 21.6(4) . . ? O5 Yb2 C48 154.5(4) . . ? N8 Yb2 C48 104.9(5) . . ? N7 Yb2 C48 64.8(5) . . ? N5 Yb2 C48 129.1(4) . . ? N6 Yb2 C48 62.3(5) . . ? C33 Yb2 C48 168.3(4) . . ? O7 Yb2 Yb1 35.0(3) . . ? O8 Yb2 Yb1 139.6(3) . . ? O6 Yb2 Yb1 148.5(3) . . ? O5 Yb2 Yb1 35.7(3) . . ? N8 Yb2 Yb1 106.3(3) . . ? N7 Yb2 Yb1 88.1(3) . . ? N5 Yb2 Yb1 70.1(3) . . ? N6 Yb2 Yb1 94.4(3) . . ? C33 Yb2 Yb1 56.3(3) . . ? C48 Yb2 Yb1 127.0(3) . . ? O7 Yb2 Yb3 138.8(3) . . ? O8 Yb2 Yb3 35.7(3) . . ? O6 Yb2 Yb3 35.7(3) . . ? O5 Yb2 Yb3 149.2(3) . . ? N8 Yb2 Yb3 89.4(3) . . ? N7 Yb2 Yb3 106.8(3) . . ? N5 Yb2 Yb3 94.7(3) . . ? N6 Yb2 Yb3 69.9(3) . . ? C33 Yb2 Yb3 126.5(3) . . ? C48 Yb2 Yb3 54.7(3) . . ? Yb1 Yb2 Yb3 161.61(3) . . ? O9 Yb3 O10 142.2(4) . . ? O9 Yb3 O11 81.3(4) . . ? O10 Yb3 O11 78.5(4) . . ? O9 Yb3 O6 107.4(4) . . ? O10 Yb3 O6 94.0(4) . . ? O11 Yb3 O6 171.2(4) . . ? O9 Yb3 O8 81.2(4) . . ? O10 Yb3 O8 77.5(4) . . ? O11 Yb3 O8 112.6(4) . . ? O6 Yb3 O8 69.6(4) . . ? O9 Yb3 N10 138.6(5) . . ? O10 Yb3 N10 72.1(5) . . ? O11 Yb3 N10 87.9(5) . . ? O6 Yb3 N10 85.4(4) . . ? O8 Yb3 N10 139.0(4) . . ? O9 Yb3 N9 73.7(5) . . ? O10 Yb3 N9 139.9(5) . . ? O11 Yb3 N9 96.1(4) . . ? O6 Yb3 N9 86.7(4) . . ? O8 Yb3 N9 138.3(4) . . ? N10 Yb3 N9 67.9(5) . . ? O9 Yb3 C64 85.6(5) . . ? O10 Yb3 C64 63.9(4) . . ? O11 Yb3 C64 92.7(4) . . ? O6 Yb3 C64 88.0(4) . . ? O8 Yb3 C64 21.5(4) . . ? N10 Yb3 C64 135.0(5) . . ? N9 Yb3 C64 155.9(5) . . ? O9 Yb3 Yb2 87.1(3) . . ? O10 Yb3 Yb2 92.9(3) . . ? O11 Yb3 Yb2 147.4(3) . . ? O6 Yb3 Yb2 36.3(3) . . ? O8 Yb3 Yb2 35.1(2) . . ? N10 Yb3 Yb2 119.7(3) . . ? N9 Yb3 Yb2 109.8(3) . . ? C64 Yb3 Yb2 55.9(3) . . ? C7 N1 C8 120.0(17) . . ? C7 N1 H1A 120.0 . . ? C8 N1 H1A 120.0 . . ? C10 N2 C9 126.4(15) . . ? C10 N2 H2B 116.8 . . ? C9 N2 H2B 116.8 . . ? C23 N3 C24 116.3(15) . . ? C23 N3 Yb1 128.7(12) . . ? C24 N3 Yb1 114.6(10) . . ? C26 N4 C25 117.6(15) . . ? C26 N4 Yb1 125.8(13) . . ? C25 N4 Yb1 116.0(10) . . ? C39 N5 C40 118.3(14) . . ? C39 N5 Yb2 124.3(12) . . ? C40 N5 Yb2 114.5(10) . . ? C42 N6 C41 118.0(15) . . ? C42 N6 Yb2 125.0(12) . . ? C41 N6 Yb2 114.5(10) . . ? C55 N7 C56 117.9(16) . . ? C55 N7 Yb2 127.0(13) . . ? C56 N7 Yb2 114.6(11) . . ? C58 N8 C57 117.2(15) . . ? C58 N8 Yb2 127.3(12) . . ? C57 N8 Yb2 114.8(11) . . ? C71 N9 C72 116.6(16) . . ? C71 N9 Yb3 127.2(14) . . ? C72 N9 Yb3 116.3(11) . . ? C74 N10 C73 117.3(16) . . ? C74 N10 Yb3 126.9(12) . . ? C73 N10 Yb3 115.4(11) . . ? C87 N11 C88 125.6(15) . . ? C87 N11 H11A 117.2 . . ? C88 N11 H11A 117.2 . . ? C1 O1 H1B 109.5 . . ? C16 O2 Yb1 154.9(11) . . ? C17 O3 Yb1 143.5(11) . . ? C32 O4 Yb1 129.1(11) . . ? C33 O5 Yb1 127.6(10) . . ? C33 O5 Yb2 115.6(9) . . ? Yb1 O5 Yb2 107.6(4) . . ? C48 O6 Yb3 123.3(9) . . ? C48 O6 Yb2 118.4(9) . . ? Yb3 O6 Yb2 108.0(4) . . ? C49 O7 Yb2 127.4(10) . . ? C49 O7 Yb1 119.5(10) . . ? Yb2 O7 Yb1 110.8(5) . . ? C64 O8 Yb2 130.0(10) . . ? C64 O8 Yb3 117.7(10) . . ? Yb2 O8 Yb3 109.2(4) . . ? C65 O9 Yb3 144.1(12) . . ? C80 O10 Yb3 130.2(11) . . ? C81 O11 Yb3 142.7(10) . . ? O1 C1 C2 119.2(19) . . ? O1 C1 C6 120.7(19) . . ? C2 C1 C6 120(2) . . ? C3 C2 C1 119(2) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 123(2) . . ? C2 C3 H3A 118.6 . . ? C4 C3 H3A 118.6 . . ? C3 C4 C5 118(2) . . ? C3 C4 H4A 121.2 . . ? C5 C4 H4A 121.2 . . ? C4 C5 C6 121(2) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C1 C6 C5 119.0(19) . . ? C1 C6 C7 121.2(19) . . ? C5 C6 C7 119.8(18) . . ? N1 C7 C6 122.7(18) . . ? N1 C7 H7A 118.6 . . ? C6 C7 H7A 118.6 . . ? N1 C8 C9 109.9(17) . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? N2 C9 C8 108.8(16) . . ? N2 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? N2 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C11 130.1(15) . . ? N2 C10 H10A 114.9 . . ? C11 C10 H10A 114.9 . . ? C10 C11 C16 119.9(16) . . ? C10 C11 C12 120.6(17) . . ? C16 C11 C12 119.6(18) . . ? C13 C12 C11 121(2) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C12 C13 C14 120(2) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C15 C14 C13 120(2) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 121.0(18) . . ? C14 C15 H15A 119.5 . . ? C16 C15 H15A 119.5 . . ? O2 C16 C15 121.6(17) . . ? O2 C16 C11 119.8(16) . . ? C15 C16 C11 118.5(17) . . ? O3 C17 C18 120.1(17) . . ? O3 C17 C22 122.6(16) . . ? C18 C17 C22 117.3(17) . . ? C17 C18 C19 123(2) . . ? C17 C18 H18A 118.4 . . ? C19 C18 H18A 118.4 . . ? C18 C19 C20 116.9(19) . . ? C18 C19 H19A 121.6 . . ? C20 C19 H19A 121.6 . . ? C21 C20 C19 122.6(19) . . ? C21 C20 H20A 118.7 . . ? C19 C20 H20A 118.7 . . ? C20 C21 C22 118(2) . . ? C20 C21 H21A 121.0 . . ? C22 C21 H21A 121.0 . . ? C21 C22 C17 121.9(18) . . ? C21 C22 C23 115.1(18) . . ? C17 C22 C23 123.0(16) . . ? N3 C23 C22 127.7(17) . . ? N3 C23 H23A 116.2 . . ? C22 C23 H23A 116.2 . . ? N3 C24 C25 109.4(14) . . ? N3 C24 H24A 109.8 . . ? C25 C24 H24A 109.8 . . ? N3 C24 H24B 109.8 . . ? C25 C24 H24B 109.8 . . ? H24A C24 H24B 108.2 . . ? N4 C25 C24 107.8(14) . . ? N4 C25 H25A 110.1 . . ? C24 C25 H25A 110.1 . . ? N4 C25 H25B 110.1 . . ? C24 C25 H25B 110.1 . . ? H25A C25 H25B 108.5 . . ? N4 C26 C27 126.4(17) . . ? N4 C26 H26A 116.8 . . ? C27 C26 H26A 116.8 . . ? C28 C27 C32 120.2(18) . . ? C28 C27 C26 118.6(18) . . ? C32 C27 C26 121.2(16) . . ? C29 C28 C27 122(2) . . ? C29 C28 H28A 118.8 . . ? C27 C28 H28A 118.8 . . ? C28 C29 C30 119(2) . . ? C28 C29 H29A 120.6 . . ? C30 C29 H29A 120.6 . . ? C31 C30 C29 121(2) . . ? C31 C30 H30A 119.6 . . ? C29 C30 H30A 119.6 . . ? C30 C31 C32 122.2(19) . . ? C30 C31 H31A 118.9 . . ? C32 C31 H31A 118.9 . . ? O4 C32 C31 121.3(17) . . ? O4 C32 C27 123.4(16) . . ? C31 C32 C27 115.2(16) . . ? O5 C33 C34 120.2(15) . . ? O5 C33 C38 119.8(15) . . ? C34 C33 C38 119.9(16) . . ? O5 C33 Yb2 41.7(7) . . ? C34 C33 Yb2 131.4(12) . . ? C38 C33 Yb2 95.8(10) . . ? C33 C34 C35 119.8(17) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C36 C35 C34 120.4(18) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C35 C36 C37 119.9(19) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 C38 121.7(17) . . ? C36 C37 H37A 119.2 . . ? C38 C37 H37A 119.2 . . ? C37 C38 C33 118.1(16) . . ? C37 C38 C39 119.4(15) . . ? C33 C38 C39 122.4(15) . . ? N5 C39 C38 124.4(16) . . ? N5 C39 H39A 117.8 . . ? C38 C39 H39A 117.8 . . ? N5 C40 C41 111.6(14) . . ? N5 C40 H40A 109.3 . . ? C41 C40 H40A 109.3 . . ? N5 C40 H40B 109.3 . . ? C41 C40 H40B 109.3 . . ? H40A C40 H40B 108.0 . . ? N6 C41 C40 109.9(15) . . ? N6 C41 H41A 109.7 . . ? C40 C41 H41A 109.7 . . ? N6 C41 H41B 109.7 . . ? C40 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? N6 C42 C43 124.7(16) . . ? N6 C42 H42A 117.6 . . ? C43 C42 H42A 117.6 . . ? C44 C43 C48 117.1(17) . . ? C44 C43 C42 119.3(16) . . ? C48 C43 C42 123.6(15) . . ? C45 C44 C43 123(2) . . ? C45 C44 H44A 118.6 . . ? C43 C44 H44A 118.6 . . ? C44 C45 C46 120(2) . . ? C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C47 C46 C45 118.3(19) . . ? C47 C46 H46A 120.8 . . ? C45 C46 H46A 120.8 . . ? C48 C47 C46 123.0(19) . . ? C48 C47 H47A 118.5 . . ? C46 C47 H47A 118.5 . . ? O6 C48 C47 122.6(16) . . ? O6 C48 C43 118.8(15) . . ? C47 C48 C43 118.6(15) . . ? O6 C48 Yb2 40.0(7) . . ? C47 C48 Yb2 133.8(12) . . ? C43 C48 Yb2 95.6(10) . . ? O7 C49 C50 119.9(16) . . ? O7 C49 C54 122.1(16) . . ? C50 C49 C54 117.8(16) . . ? O7 C49 Yb1 38.6(7) . . ? C50 C49 Yb1 98.9(12) . . ? C54 C49 Yb1 133.8(12) . . ? C51 C50 C49 120.2(19) . . ? C51 C50 H50A 119.9 . . ? C49 C50 H50A 119.9 . . ? C52 C51 C50 121(2) . . ? C52 C51 H51A 119.3 . . ? C50 C51 H51A 119.3 . . ? C51 C52 C53 118.5(19) . . ? C51 C52 H52A 120.8 . . ? C53 C52 H52A 120.8 . . ? C54 C53 C52 122.2(19) . . ? C54 C53 H53A 118.9 . . ? C52 C53 H53A 118.9 . . ? C53 C54 C49 118.4(17) . . ? C53 C54 C55 116.5(17) . . ? C49 C54 C55 121.3(15) . . ? N7 C55 C54 124.1(17) . . ? N7 C55 H55A 118.0 . . ? C54 C55 H55A 118.0 . . ? N7 C56 C57 107.7(16) . . ? N7 C56 H56A 110.2 . . ? C57 C56 H56A 110.2 . . ? N7 C56 H56B 110.2 . . ? C57 C56 H56B 110.2 . . ? H56A C56 H56B 108.5 . . ? N8 C57 C56 108.0(15) . . ? N8 C57 H57A 110.1 . . ? C56 C57 H57A 110.1 . . ? N8 C57 H57B 110.1 . . ? C56 C57 H57B 110.1 . . ? H57A C57 H57B 108.4 . . ? N8 C58 C59 126.8(15) . . ? N8 C58 H58A 116.6 . . ? C59 C58 H58A 116.6 . . ? C60 C59 C64 122.2(16) . . ? C60 C59 C58 116.0(16) . . ? C64 C59 C58 121.6(14) . . ? C61 C60 C59 118.8(19) . . ? C61 C60 H60A 120.6 . . ? C59 C60 H60A 120.6 . . ? C60 C61 C62 121.0(18) . . ? C60 C61 H61A 119.5 . . ? C62 C61 H61A 119.5 . . ? C63 C62 C61 119.5(18) . . ? C63 C62 H62A 120.2 . . ? C61 C62 H62A 120.2 . . ? C64 C63 C62 123.1(19) . . ? C64 C63 H63A 118.5 . . ? C62 C63 H63A 118.5 . . ? O8 C64 C63 121.9(16) . . ? O8 C64 C59 122.7(15) . . ? C63 C64 C59 115.3(16) . . ? O8 C64 Yb3 40.8(7) . . ? C63 C64 Yb3 96.4(12) . . ? C59 C64 Yb3 132.1(11) . . ? O9 C65 C70 122.0(17) . . ? O9 C65 C66 120.8(19) . . ? C70 C65 C66 117.2(18) . . ? C65 C66 C67 121(2) . . ? C65 C66 H66A 119.7 . . ? C67 C66 H66A 119.7 . . ? C68 C67 C66 122(2) . . ? C68 C67 H67A 119.0 . . ? C66 C67 H67A 119.0 . . ? C69 C68 C67 117(2) . . ? C69 C68 H68A 121.3 . . ? C67 C68 H68A 121.3 . . ? C68 C69 C70 123(2) . . ? C68 C69 H69A 118.4 . . ? C70 C69 H69A 118.4 . . ? C65 C70 C69 119.1(19) . . ? C65 C70 C71 123.7(17) . . ? C69 C70 C71 117.1(19) . . ? N9 C71 C70 128.6(19) . . ? N9 C71 H71A 115.7 . . ? C70 C71 H71A 115.7 . . ? N9 C72 C73 110.7(15) . . ? N9 C72 H72A 109.5 . . ? C73 C72 H72A 109.5 . . ? N9 C72 H72B 109.5 . . ? C73 C72 H72B 109.5 . . ? H72A C72 H72B 108.1 . . ? N10 C73 C72 108.3(15) . . ? N10 C73 H73A 110.0 . . ? C72 C73 H73A 110.0 . . ? N10 C73 H73B 110.0 . . ? C72 C73 H73B 110.0 . . ? H73A C73 H73B 108.4 . . ? N10 C74 C75 127.6(17) . . ? N10 C74 H74A 116.2 . . ? C75 C74 H74A 116.2 . . ? C76 C75 C80 120.6(17) . . ? C76 C75 C74 118.9(17) . . ? C80 C75 C74 120.4(16) . . ? C77 C76 C75 122(2) . . ? C77 C76 H76A 119.2 . . ? C75 C76 H76A 119.2 . . ? C78 C77 C76 117.6(19) . . ? C78 C77 H77A 121.2 . . ? C76 C77 H77A 121.2 . . ? C77 C78 C79 124.1(17) . . ? C77 C78 H78A 118.0 . . ? C79 C78 H78A 118.0 . . ? C78 C79 C80 120.2(17) . . ? C78 C79 H79A 119.9 . . ? C80 C79 H79A 119.9 . . ? O10 C80 C79 120.4(16) . . ? O10 C80 C75 123.5(16) . . ? C79 C80 C75 115.9(16) . . ? O11 C81 C82 121.6(15) . . ? O11 C81 C86 121.1(15) . . ? C82 C81 C86 117.3(15) . . ? C83 C82 C81 119.5(17) . . ? C83 C82 H82A 120.3 . . ? C81 C82 H82A 120.3 . . ? C82 C83 C84 122.9(19) . . ? C82 C83 H83A 118.6 . . ? C84 C83 H83A 118.6 . . ? C85 C84 C83 120.3(19) . . ? C85 C84 H84A 119.9 . . ? C83 C84 H84A 119.9 . . ? C84 C85 C86 120.0(18) . . ? C84 C85 H85A 120.0 . . ? C86 C85 H85A 120.0 . . ? C87 C86 C81 121.2(16) . . ? C87 C86 C85 118.6(16) . . ? C81 C86 C85 120.0(16) . . ? N11 C87 C86 123.9(17) . . ? N11 C87 H87A 118.1 . . ? C86 C87 H87A 118.1 . . ? N11 C88 C88 107.5(17) . 2_456 ? N11 C88 H88A 110.2 . . ? C88 C88 H88A 110.2 2_456 . ? N11 C88 H88B 110.2 . . ? C88 C88 H88B 110.2 2_456 . ? H88A C88 H88B 108.5 . . ? C90 C89 H89A 109.5 . . ? C90 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C90 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C89 C90 O12 101(3) . . ? C89 C90 H90A 111.5 . . ? O12 C90 H90A 111.5 . . ? C89 C90 H90B 111.5 . . ? O12 C90 H90B 111.5 . . ? H90A C90 H90B 109.3 . . ? C91 O13 H13B 109.5 . . ? O14 C92 H92A 109.5 . . ? O14 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? O14 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C90 O12 H12B 109.5 . . ? O13 C91 H91B 109.5 . . ? O13 C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? O13 C91 H91A 109.5 . . ? H91B C91 H91A 109.5 . . ? H91C C91 H91A 109.5 . . ? C92 O14 H14 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.957 _refine_diff_density_min -3.353 _refine_diff_density_rms 0.278 _database_code_depnum_ccdc_archive 'CCDC 950238' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C64 H58 N8 O10 Yb3), 5(C H4 O), 5.52(O)' _chemical_formula_sum 'C261 H252 N32 O50.52 Yb12' _chemical_formula_weight 6721.43 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 TETRAGONAL _symmetry_space_group_name_H-M I4(1)/a _symmetry_space_group_name_Hall -I4ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 26.773(4) _cell_length_b 26.773(4) _cell_length_c 45.788(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 32821(9) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 19057 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13144.6 _exptl_absorpt_coefficient_mu 3.444 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5920 _exptl_absorpt_correction_T_max 0.7245 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14337 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14337 _reflns_number_gt 10816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _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. Restraints: ISOR was applied to all non-hydrogen atoms to allow their Uij components approximate to isotropic behavior, and the benzyle C1-C6 was fixed. Hydrogen atoms of water molecules were not added. ; _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^)+(0.0987P)^2^+548.4625P] 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 14337 _refine_ls_number_parameters 808 _refine_ls_number_restraints 587 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.2059 _refine_ls_wR_factor_gt 0.1785 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.020 _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 0.26437(2) 0.557611(19) 0.893996(10) 0.05922(15) Uani 1 1 d U . . Yb2 Yb 0.24802(2) 0.493793(19) 0.965740(9) 0.06255(16) Uani 1 1 d U . . Yb3 Yb 0.27295(2) 0.43409(2) 1.038024(10) 0.06615(17) Uani 1 1 d U . . O1 O 0.3505(4) 0.4609(4) 1.0379(2) 0.090(3) Uani 1 1 d U . . O2 O 0.1983(3) 0.4554(3) 1.05519(15) 0.065(2) Uani 1 1 d U . . O3 O 0.2453(3) 0.4178(3) 0.99151(16) 0.068(2) Uani 1 1 d U . . O4 O 0.2319(3) 0.5669(3) 0.93976(13) 0.0616(19) Uani 1 1 d U . . O5 O 0.2604(3) 0.5087(3) 1.01428(14) 0.068(2) Uani 1 1 d U . . O6 O 0.2623(3) 0.4816(3) 0.91802(13) 0.0550(17) Uani 1 1 d U . . O7 O 0.1917(3) 0.5278(3) 0.87784(16) 0.0604(19) Uani 1 1 d U . . O8 O 0.3459(3) 0.5365(4) 0.89280(18) 0.075(2) Uani 1 1 d U . . O9 O 0.2795(3) 0.5549(3) 0.84461(16) 0.065(2) Uani 1 1 d U . . H9A H 0.2529 0.5541 0.8358 0.098 Uiso 1 1 calc R . . O10 O 0.2914(3) 0.4426(3) 1.08721(14) 0.0594(19) Uani 1 1 d U . . H10A H 0.2655 0.4415 1.0967 0.089 Uiso 1 1 calc R . . N1 N 0.3273(4) 0.3622(5) 1.0326(2) 0.080(3) Uani 1 1 d DU . . N2 N 0.2308(5) 0.3567(4) 1.0542(2) 0.074(3) Uani 1 1 d U . . N3 N 0.3314(5) 0.4503(5) 0.9623(2) 0.083(3) Uani 1 1 d U . . N4 N 0.3230(5) 0.5536(4) 0.9689(2) 0.076(3) Uani 1 1 d U . . N5 N 0.2134(4) 0.6316(4) 0.8818(2) 0.068(3) Uani 1 1 d U . . N6 N 0.3138(4) 0.6368(4) 0.8978(2) 0.072(3) Uani 1 1 d U . . N7 N 0.1766(4) 0.4502(4) 0.94575(19) 0.070(3) Uani 1 1 d U . . N8 N 0.1697(4) 0.5249(3) 0.98639(13) 0.067(3) Uani 1 1 d U . . C1 C 0.3982(3) 0.4481(3) 1.03686(13) 0.093(4) Uani 1 1 d RU . . C2 C 0.4348(3) 0.4848(3) 1.03843(13) 0.104(5) Uani 1 1 d RU . . H2A H 0.4273 0.5159 1.0463 0.124 Uiso 1 1 calc R . . C3 C 0.4828(3) 0.4750(3) 1.02825(12) 0.154 Uiso 1 1 d R . . H3A H 0.5073 0.4995 1.0293 0.185 Uiso 1 1 calc R . . C4 C 0.4941(4) 0.4284(3) 1.01651(12) 0.152 Uiso 1 1 d R . . H4A H 0.5262 0.4218 1.0097 0.182 Uiso 1 1 calc R . . C5 C 0.4574(3) 0.3917(3) 1.01493(12) 0.159 Uiso 1 1 d RD . . H5A H 0.4650 0.3606 1.0071 0.191 Uiso 1 1 calc R . . C6 C 0.4095(3) 0.4015(3) 1.02510(12) 0.144(8) Uani 1 1 d RDU . . C7 C 0.3738(4) 0.3623(6) 1.0323(5) 0.159(9) Uani 1 1 d DU . . H7A H 0.3882 0.3321 1.0377 0.191 Uiso 1 1 calc R . . C8 C 0.3034(5) 0.3120(5) 1.0348(3) 0.080(4) Uani 1 1 d DU . . H8A H 0.3282 0.2867 1.0394 0.096 Uiso 1 1 calc R . . H8B H 0.2873 0.3032 1.0166 0.096 Uiso 1 1 calc R . . C9 C 0.2649(6) 0.3159(6) 1.0593(3) 0.099(5) Uani 1 1 d DU . . H9B H 0.2463 0.2849 1.0606 0.119 Uiso 1 1 calc R . . H9C H 0.2820 0.3210 1.0778 0.119 Uiso 1 1 calc R . . C10 C 0.1849(7) 0.3495(6) 1.0570(3) 0.090(4) Uani 1 1 d U . . H10B H 0.1749 0.3173 1.0617 0.108 Uiso 1 1 calc R . . C11 C 0.1463(6) 0.3862(7) 1.0535(4) 0.096(5) Uani 1 1 d DU . . C12 C 0.0963(6) 0.3672(9) 1.0537(5) 0.133(7) Uani 1 1 d DU . . H12A H 0.0893 0.3337 1.0569 0.159 Uiso 1 1 calc R . . C13 C 0.0587(8) 0.4023(9) 1.0489(5) 0.130(7) Uani 1 1 d U . . H13A H 0.0270 0.3902 1.0445 0.156 Uiso 1 1 calc R . . C14 C 0.0640(8) 0.4487(9) 1.0499(4) 0.119(6) Uani 1 1 d U . . H14A H 0.0366 0.4701 1.0499 0.143 Uiso 1 1 calc R . . C15 C 0.1104(5) 0.4663(7) 1.0509(3) 0.087(4) Uani 1 1 d U . . H15A H 0.1152 0.5006 1.0499 0.105 Uiso 1 1 calc R . . C16 C 0.1529(5) 0.4351(5) 1.0533(2) 0.065(3) Uani 1 1 d U . . C17 C 0.2521(6) 0.3772(4) 0.9762(2) 0.069(3) Uani 1 1 d U . . C18 C 0.2185(7) 0.3396(5) 0.9746(3) 0.092(4) Uani 1 1 d DU . . H18A H 0.1887 0.3428 0.9849 0.110 Uiso 1 1 calc R . . C19 C 0.2264(7) 0.2948(5) 0.9576(3) 0.094(4) Uani 1 1 d DU . . H19A H 0.2009 0.2715 0.9554 0.112 Uiso 1 1 calc R . . C20 C 0.2678(8) 0.2877(7) 0.9460(3) 0.105(5) Uani 1 1 d U . . H20A H 0.2740 0.2574 0.9367 0.126 Uiso 1 1 calc R . . C21 C 0.3025(8) 0.3213(7) 0.9464(4) 0.110(5) Uani 1 1 d U . . H21A H 0.3323 0.3137 0.9370 0.132 Uiso 1 1 calc R . . C22 C 0.2989(6) 0.3699(5) 0.9604(3) 0.073(3) Uani 1 1 d U . . C23 C 0.3362(7) 0.4079(7) 0.9586(3) 0.095(4) Uani 1 1 d U . . H23A H 0.3682 0.3972 0.9540 0.114 Uiso 1 1 calc R . . C24 C 0.3738(6) 0.4829(7) 0.9586(4) 0.101(5) Uani 1 1 d U . . H24A H 0.3771 0.4921 0.9382 0.121 Uiso 1 1 calc R . . H24B H 0.4041 0.4659 0.9646 0.121 Uiso 1 1 calc R . . C25 C 0.3662(7) 0.5304(7) 0.9774(4) 0.106(5) Uani 1 1 d U . . H25A H 0.3641 0.5213 0.9979 0.127 Uiso 1 1 calc R . . H25B H 0.3944 0.5528 0.9749 0.127 Uiso 1 1 calc R . . C26 C 0.3143(6) 0.6019(6) 0.9730(3) 0.078(4) Uani 1 1 d U . . H26A H 0.3417 0.6202 0.9794 0.094 Uiso 1 1 calc R . . C27 C 0.2737(6) 0.6280(5) 0.9696(2) 0.068(3) Uani 1 1 d U . . C28 C 0.2669(7) 0.6761(6) 0.9843(4) 0.099(5) Uani 1 1 d U . . H28A H 0.2924 0.6897 0.9955 0.119 Uiso 1 1 calc R . . C29 C 0.2231(8) 0.7005(7) 0.9813(4) 0.109(5) Uani 1 1 d U . . H29A H 0.2215 0.7320 0.9898 0.131 Uiso 1 1 calc R . . C30 C 0.1804(8) 0.6846(7) 0.9671(4) 0.114(6) Uani 1 1 d U . . H30A H 0.1510 0.7031 0.9671 0.137 Uiso 1 1 calc R . . C31 C 0.1847(6) 0.6388(5) 0.9529(3) 0.080(4) Uani 1 1 d U . . H31A H 0.1576 0.6266 0.9424 0.096 Uiso 1 1 calc R . . C32 C 0.2284(6) 0.6111(5) 0.9541(3) 0.077(4) Uani 1 1 d U . . C33 C 0.2503(6) 0.5511(4) 1.0283(2) 0.070(3) Uani 1 1 d U . . C34 C 0.2881(6) 0.5696(6) 1.0470(3) 0.082(4) Uani 1 1 d U . . H34A H 0.3191 0.5543 1.0489 0.099 Uiso 1 1 calc R . . C35 C 0.2742(7) 0.6156(6) 1.0634(3) 0.087(4) Uani 1 1 d U . . H35A H 0.2969 0.6289 1.0767 0.104 Uiso 1 1 calc R . . C36 C 0.2333(8) 0.6367(7) 1.0601(4) 0.103(5) Uani 1 1 d U . . H36A H 0.2282 0.6662 1.0704 0.124 Uiso 1 1 calc R . . C37 C 0.1910(7) 0.6192(5) 1.0408(3) 0.089(4) Uani 1 1 d U . . H37A H 0.1601 0.6348 1.0393 0.106 Uiso 1 1 calc R . . C38 C 0.2052(6) 0.5753(5) 1.0254(3) 0.074(3) Uani 1 1 d U . . C39 C 0.1646(5) 0.5558(5) 1.0069(2) 0.071(3) Uani 1 1 d U . . H39A H 0.1325 0.5672 1.0107 0.085 Uiso 1 1 calc R . . C40 C 0.1240(5) 0.5116(5) 0.9697(3) 0.076(4) Uani 1 1 d U . . H40A H 0.1219 0.5310 0.9518 0.091 Uiso 1 1 calc R . . H40B H 0.0943 0.5175 0.9813 0.091 Uiso 1 1 calc R . . C41 C 0.1296(6) 0.4563(7) 0.9628(4) 0.104(5) Uani 1 1 d U . . H41A H 0.1313 0.4371 0.9807 0.124 Uiso 1 1 calc R . . H41B H 0.1013 0.4447 0.9515 0.124 Uiso 1 1 calc R . . C42 C 0.1767(6) 0.4181(5) 0.9240(3) 0.078(4) Uani 1 1 d U . . H42A H 0.1477 0.3995 0.9214 0.094 Uiso 1 1 calc R . . C43 C 0.2168(5) 0.4083(4) 0.9036(2) 0.058(3) Uani 1 1 d U . . C44 C 0.2146(6) 0.3677(5) 0.8867(3) 0.071(3) Uani 1 1 d U . . H44A H 0.1877 0.3461 0.8888 0.085 Uiso 1 1 calc R . . C45 C 0.2508(7) 0.3569(5) 0.8663(3) 0.089(4) Uani 1 1 d U . . H45A H 0.2469 0.3294 0.8542 0.107 Uiso 1 1 calc R . . C46 C 0.2922(6) 0.3859(5) 0.8637(3) 0.075(4) Uani 1 1 d U . . H46A H 0.3172 0.3785 0.8502 0.089 Uiso 1 1 calc R . . C47 C 0.2954(5) 0.4271(4) 0.8820(2) 0.061(3) Uani 1 1 d U . . H47A H 0.3236 0.4474 0.8809 0.074 Uiso 1 1 calc R . . C48 C 0.2573(6) 0.4395(5) 0.9025(3) 0.077(4) Uani 1 1 d U . . C49 C 0.1458(5) 0.5416(5) 0.8834(2) 0.062(3) Uani 1 1 d U . . C50 C 0.1104(5) 0.5061(5) 0.8855(2) 0.068(3) Uani 1 1 d U . . H50A H 0.1186 0.4728 0.8824 0.082 Uiso 1 1 calc R . . C51 C 0.0584(6) 0.5199(7) 0.8928(3) 0.088(4) Uani 1 1 d U . . H51A H 0.0341 0.4955 0.8953 0.105 Uiso 1 1 calc R . . C52 C 0.0476(6) 0.5669(7) 0.8957(4) 0.096(5) Uani 1 1 d U . . H52A H 0.0159 0.5758 0.9022 0.116 Uiso 1 1 calc R . . C53 C 0.0839(7) 0.6063(8) 0.8890(4) 0.110(5) Uani 1 1 d U . . H53A H 0.0744 0.6396 0.8873 0.132 Uiso 1 1 calc R . . C54 C 0.1319(5) 0.5916(5) 0.8856(3) 0.071(3) Uani 1 1 d U . . C55 C 0.1664(5) 0.6327(5) 0.8812(3) 0.072(3) Uani 1 1 d U . . H55A H 0.1521 0.6637 0.8775 0.086 Uiso 1 1 calc R . . C56 C 0.2422(6) 0.6791(5) 0.8780(3) 0.085(4) Uani 1 1 d U . . H56A H 0.2204 0.7076 0.8811 0.101 Uiso 1 1 calc R . . H56B H 0.2557 0.6810 0.8584 0.101 Uiso 1 1 calc R . . C57 C 0.2849(5) 0.6801(5) 0.9003(3) 0.073(3) Uani 1 1 d U . . H57A H 0.3056 0.7092 0.8970 0.087 Uiso 1 1 calc R . . H57B H 0.2712 0.6823 0.9199 0.087 Uiso 1 1 calc R . . C58 C 0.3613(7) 0.6360(8) 0.8941(5) 0.137(9) Uani 1 1 d DU . . H58A H 0.3756 0.6656 0.9006 0.164 Uiso 1 1 calc R . . C59 C 0.3995 0.6023 0.8826 0.132 Uani 1 1 d DU . . C60 C 0.4476 0.6191 0.8768 0.156 Uani 1 1 d U . . H60A H 0.4537 0.6531 0.8747 0.187 Uiso 1 1 calc R . . C61 C 0.4866 0.5851 0.8742 0.156 Uani 1 1 d U . . H61A H 0.5188 0.5964 0.8703 0.187 Uiso 1 1 calc R . . C62 C 0.4775 0.5343 0.8774 0.142 Uani 1 1 d U . . H62A H 0.5035 0.5116 0.8757 0.171 Uiso 1 1 calc R . . C63 C 0.4294 0.5175 0.8832 0.092 Uani 1 1 d U . . H63A H 0.4233 0.4835 0.8854 0.111 Uiso 1 1 calc R . . C64 C 0.3904 0.5515 0.8858 0.079 Uani 1 1 d U . . O11 O 0.0102(10) 0.4136(12) 0.9169(6) 0.171(12) Uani 0.50 1 d PDU . . H11A H 0.0249 0.3905 0.9088 0.256 Uiso 0.50 1 calc PR . . C65 C -0.0307(9) 0.3922(10) 0.9372(5) 0.070(6) Uani 0.50 1 d PDU . . H65A H -0.0153 0.3763 0.9537 0.084 Uiso 0.50 1 calc PR . . H65B H -0.0504 0.3681 0.9267 0.084 Uiso 0.50 1 calc PR . . H65C H -0.0519 0.4188 0.9439 0.105 Uiso 0.50 1 calc PR . . O12 O 0.458(3) 0.354(3) 0.9090(15) 0.18(3) Uani 0.25 1 d PDU . . H12B H 0.4595 0.3232 0.9079 0.264 Uiso 0.25 1 calc PR . . C66 C 0.466(4) 0.376(4) 0.8782(18) 0.19(5) Uani 0.25 1 d PDU . . H66A H 0.4521 0.4096 0.8777 0.289 Uiso 0.25 1 calc PR . . H66B H 0.4491 0.3561 0.8639 0.289 Uiso 0.25 1 calc PR . . H66C H 0.5008 0.3778 0.8738 0.289 Uiso 0.25 1 calc PR . . O13 O 0.504(3) 0.601(3) 1.0535(15) 0.18(3) Uani 0.25 1 d PDU . . H13B H 0.4984 0.5799 1.0412 0.265 Uiso 0.25 1 calc PR . . C67 C 0.466(3) 0.644(3) 1.051(2) 0.15(3) Uani 0.25 1 d PDU . . H67A H 0.4786 0.6736 1.0603 0.232 Uiso 0.25 1 calc PR . . H67B H 0.4351 0.6344 1.0599 0.232 Uiso 0.25 1 calc PR . . H67C H 0.4600 0.6514 1.0306 0.232 Uiso 0.25 1 calc PR . . O14 O 0.416(3) 0.240(4) 1.079(2) 0.25(4) Uani 0.25 1 d PDU . . H14B H 0.3901 0.2326 1.0705 0.377 Uiso 0.25 1 calc PR . . C68 C 0.462(3) 0.228(3) 1.0596(17) 0.14(3) Uani 0.25 1 d PDU . . H68A H 0.4618 0.2497 1.0431 0.203 Uiso 0.25 1 calc PR . . H68B H 0.4594 0.1937 1.0530 0.203 Uiso 0.25 1 calc PR . . H68C H 0.4917 0.2321 1.0706 0.203 Uiso 0.25 1 calc PR . . O15 O 0.0674(15) 0.3422(14) 0.9042(8) 0.087(11) Uani 0.25 1 d PU . . O16 O -0.0018(18) 0.430(2) 0.9749(11) 0.117(15) Uani 0.25 1 d PU . . O17 O 0.0914(18) 0.2736(18) 0.9863(10) 0.110(14) Uani 0.25 1 d PU . . O18 O 0.008(3) 0.714(3) 0.8612(14) 0.18(3) Uani 0.25 1 d PU . . O19 O 0.0624(19) 0.358(2) 0.8578(11) 0.115(14) Uani 0.25 1 d PU . . O20 O 0.046(4) 0.744(4) 0.936(2) 0.12(3) Uani 0.13 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.0908(4) 0.0528(3) 0.0341(2) 0.00164(19) 0.0118(2) 0.0012(3) Yb2 0.0994(4) 0.0614(3) 0.0268(2) 0.00171(18) 0.0000(2) -0.0211(3) Yb3 0.0856(4) 0.0841(4) 0.0288(2) 0.0047(2) -0.0046(2) -0.0327(3) O1 0.088(6) 0.119(7) 0.064(5) -0.006(5) 0.013(4) -0.036(5) O2 0.061(4) 0.089(5) 0.044(4) 0.019(4) -0.004(3) -0.024(4) O3 0.091(5) 0.069(4) 0.046(4) 0.004(3) -0.012(4) -0.031(4) O4 0.103(5) 0.056(4) 0.026(3) -0.011(3) 0.007(3) -0.002(4) O5 0.090(5) 0.080(5) 0.034(3) 0.000(3) 0.003(3) -0.030(4) O6 0.077(4) 0.053(4) 0.035(3) -0.006(3) -0.005(3) 0.008(3) O7 0.063(4) 0.057(4) 0.061(4) -0.005(3) 0.011(4) 0.007(3) O8 0.070(5) 0.090(5) 0.064(5) 0.001(4) 0.018(4) 0.006(4) O9 0.073(5) 0.069(4) 0.054(4) -0.001(3) 0.010(3) 0.003(4) O10 0.058(4) 0.084(5) 0.037(3) -0.001(3) -0.002(3) -0.004(4) N1 0.082(6) 0.099(7) 0.059(5) 0.021(5) -0.007(5) -0.008(6) N2 0.095(7) 0.084(6) 0.042(4) -0.002(4) -0.005(5) -0.025(6) N3 0.120(8) 0.076(6) 0.053(5) 0.008(5) -0.012(5) 0.014(6) N4 0.094(7) 0.087(6) 0.045(5) 0.018(5) 0.006(5) -0.026(6) N5 0.083(6) 0.070(6) 0.052(5) -0.004(4) 0.017(5) 0.006(5) N6 0.076(6) 0.076(6) 0.065(5) 0.010(5) 0.002(5) -0.003(5) N7 0.097(6) 0.074(6) 0.040(4) 0.012(4) 0.003(4) -0.020(5) N8 0.086(6) 0.078(6) 0.038(4) -0.001(4) 0.004(4) -0.025(5) C1 0.082(8) 0.126(9) 0.070(7) 0.014(7) -0.001(6) -0.029(7) C2 0.084(8) 0.117(9) 0.110(9) 0.009(7) 0.004(7) -0.018(7) C6 0.113(10) 0.154(11) 0.165(11) 0.029(9) -0.004(8) -0.011(8) C7 0.159(12) 0.150(12) 0.168(12) 0.029(9) -0.011(9) 0.016(9) C8 0.092(8) 0.089(7) 0.060(6) -0.003(6) -0.005(6) 0.002(6) C9 0.122(9) 0.103(8) 0.072(7) 0.005(6) 0.007(7) -0.033(7) C10 0.103(8) 0.096(8) 0.072(7) -0.005(6) 0.011(6) -0.051(7) C11 0.089(8) 0.104(8) 0.094(8) -0.015(7) 0.010(7) -0.040(7) C12 0.144(10) 0.125(10) 0.129(10) -0.014(8) 0.008(8) -0.027(8) C13 0.116(10) 0.140(10) 0.133(10) -0.022(8) -0.008(8) -0.015(8) C14 0.106(9) 0.133(10) 0.118(9) 0.003(8) 0.005(8) -0.008(8) C15 0.072(7) 0.113(8) 0.076(7) 0.003(6) -0.021(6) -0.019(7) C16 0.071(6) 0.095(7) 0.030(4) 0.020(5) 0.002(4) -0.021(6) C17 0.102(8) 0.064(6) 0.041(5) 0.004(5) -0.005(5) -0.034(6) C18 0.124(9) 0.087(7) 0.064(6) 0.016(6) -0.017(7) -0.017(7) C19 0.121(9) 0.078(7) 0.082(7) 0.018(6) -0.026(7) -0.019(7) C20 0.135(9) 0.112(9) 0.069(7) -0.006(6) -0.003(7) -0.013(8) C21 0.134(9) 0.118(9) 0.077(8) 0.005(7) -0.001(7) 0.006(8) C22 0.095(8) 0.074(7) 0.051(6) 0.000(5) -0.006(6) 0.002(6) C23 0.112(9) 0.098(8) 0.074(7) 0.008(7) -0.013(7) -0.010(7) C24 0.092(8) 0.126(9) 0.084(8) 0.027(7) 0.008(6) -0.024(7) C25 0.112(9) 0.122(9) 0.084(8) -0.005(7) 0.013(7) -0.032(8) C26 0.097(8) 0.083(7) 0.055(6) -0.012(6) 0.007(6) -0.041(6) C27 0.096(8) 0.063(6) 0.044(5) -0.009(5) 0.011(5) -0.020(6) C28 0.116(9) 0.095(8) 0.087(8) -0.007(7) 0.011(7) -0.029(7) C29 0.136(10) 0.108(9) 0.083(8) -0.004(7) 0.024(8) -0.008(8) C30 0.126(10) 0.116(9) 0.101(9) -0.007(7) 0.027(8) -0.006(8) C31 0.108(8) 0.072(7) 0.061(6) -0.008(5) 0.022(6) 0.014(6) C32 0.113(8) 0.064(6) 0.055(6) 0.001(5) 0.025(6) -0.006(6) C33 0.123(8) 0.058(6) 0.028(4) -0.004(4) 0.016(5) -0.003(6) C34 0.088(7) 0.093(7) 0.065(6) 0.003(6) 0.022(6) -0.025(6) C35 0.113(8) 0.089(7) 0.058(6) -0.006(6) 0.002(6) -0.032(7) C36 0.134(9) 0.101(8) 0.075(7) -0.002(7) 0.009(7) -0.026(8) C37 0.125(9) 0.078(7) 0.063(6) -0.017(6) 0.025(6) 0.009(7) C38 0.112(8) 0.064(6) 0.047(5) 0.018(5) 0.008(6) -0.004(6) C39 0.085(7) 0.089(7) 0.040(5) 0.000(5) 0.027(5) -0.025(6) C40 0.090(7) 0.082(7) 0.054(6) -0.013(6) 0.005(5) -0.008(6) C41 0.093(8) 0.124(9) 0.095(8) 0.011(7) -0.020(7) -0.019(7) C42 0.099(8) 0.071(7) 0.065(6) 0.006(6) -0.014(6) -0.019(6) C43 0.076(6) 0.047(5) 0.051(5) -0.007(4) -0.021(5) -0.013(5) C44 0.104(8) 0.061(6) 0.047(5) 0.008(5) -0.005(6) -0.002(6) C45 0.127(9) 0.072(7) 0.068(7) -0.009(6) -0.021(7) 0.015(7) C46 0.092(7) 0.058(6) 0.074(7) 0.002(5) 0.002(6) 0.010(6) C47 0.105(7) 0.047(5) 0.032(5) 0.003(4) 0.004(5) 0.012(5) C48 0.122(8) 0.067(6) 0.042(5) 0.007(5) -0.003(5) 0.007(6) C49 0.065(6) 0.076(7) 0.044(5) 0.011(5) 0.022(5) 0.000(5) C50 0.074(6) 0.090(7) 0.042(5) -0.022(5) -0.019(5) -0.005(6) C51 0.080(7) 0.102(8) 0.082(7) -0.011(7) -0.006(6) -0.018(7) C52 0.079(7) 0.106(9) 0.104(8) -0.020(7) 0.003(6) -0.007(7) C53 0.090(8) 0.118(9) 0.123(9) -0.011(8) 0.000(7) 0.003(7) C54 0.067(6) 0.070(7) 0.075(7) -0.013(5) 0.002(5) 0.000(5) C55 0.074(7) 0.086(7) 0.056(6) 0.005(5) -0.002(5) 0.003(6) C56 0.098(8) 0.064(6) 0.092(7) 0.014(6) 0.015(7) -0.007(6) C57 0.083(7) 0.064(6) 0.072(6) -0.009(5) 0.010(6) -0.006(6) C58 0.129(11) 0.136(11) 0.146(12) -0.011(9) 0.001(9) -0.022(9) C59 0.119 0.137 0.141 -0.008 0.010 0.002 C60 0.146 0.152 0.169 0.000 0.007 -0.011 C61 0.157 0.158 0.154 -0.002 0.001 0.004 C62 0.127 0.149 0.151 -0.008 0.001 0.017 C63 0.066 0.111 0.101 -0.009 0.001 -0.008 C64 0.066 0.086 0.084 0.001 0.014 0.014 O11 0.176(14) 0.166(14) 0.170(14) 0.012(9) -0.019(10) -0.013(9) C65 0.075(10) 0.074(10) 0.060(9) 0.020(8) -0.011(8) -0.003(8) O12 0.17(3) 0.18(3) 0.18(3) -0.003(10) 0.005(10) 0.007(10) C66 0.19(5) 0.19(5) 0.20(5) 0.001(10) -0.001(10) 0.006(10) O13 0.18(3) 0.18(3) 0.18(3) -0.002(10) 0.003(10) 0.002(10) C67 0.15(4) 0.16(4) 0.15(4) 0.001(10) 0.005(10) -0.003(10) O14 0.25(4) 0.25(4) 0.25(4) 0.011(10) -0.003(10) 0.002(10) C68 0.14(3) 0.13(3) 0.14(3) -0.004(10) -0.002(10) 0.003(10) O15 0.090(13) 0.081(13) 0.090(13) -0.013(9) 0.012(9) -0.013(9) O16 0.110(17) 0.127(17) 0.115(17) 0.007(10) 0.006(10) -0.003(10) O17 0.105(16) 0.116(16) 0.108(16) -0.004(10) -0.001(10) 0.001(10) O18 0.18(3) 0.18(3) 0.18(3) 0.006(10) -0.006(10) 0.010(10) O19 0.114(17) 0.122(17) 0.109(17) -0.002(10) -0.006(10) -0.002(10) O20 0.12(3) 0.12(3) 0.12(3) 0.001(10) -0.001(10) -0.001(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 Yb1 O7 2.231(8) . ? Yb1 O8 2.254(9) . ? Yb1 O4 2.282(6) . ? Yb1 O9 2.299(7) . ? Yb1 O6 2.313(7) . ? Yb1 N5 2.470(11) . ? Yb1 N6 2.505(11) . ? Yb1 C48 3.192(13) . ? Yb1 Yb2 3.7286(9) . ? Yb2 O6 2.242(6) . ? Yb2 O5 2.282(7) . ? Yb2 O4 2.331(7) . ? Yb2 O3 2.354(8) . ? Yb2 N7 2.421(11) . ? Yb2 N8 2.447(10) . ? Yb2 N3 2.523(13) . ? Yb2 N4 2.571(11) . ? Yb2 C17 3.161(12) . ? Yb2 Yb3 3.7356(9) . ? Yb3 O1 2.198(10) . ? Yb3 O2 2.222(8) . ? Yb3 O3 2.297(7) . ? Yb3 O5 2.298(8) . ? Yb3 O10 2.317(6) . ? Yb3 N1 2.426(12) . ? Yb3 N2 2.472(11) . ? O1 C1 1.322(13) . ? O2 C16 1.334(14) . ? O3 C17 1.306(14) . ? O4 C32 1.357(15) . ? O5 C33 1.332(13) . ? O6 C48 1.340(14) . ? O7 C49 1.306(14) . ? O8 C64 1.297(9) . ? O9 H9A 0.8200 . ? O10 H10A 0.8200 . ? N1 C7 1.243(9) . ? N1 C8 1.493(18) . ? N2 C10 1.249(19) . ? N2 C9 1.45(2) . ? N3 C23 1.154(18) . ? N3 C24 1.44(2) . ? N4 C26 1.330(18) . ? N4 C25 1.37(2) . ? N5 C55 1.258(16) . ? N5 C56 1.497(17) . ? N6 C58 1.282(19) . ? N6 C57 1.400(16) . ? N7 C42 1.316(16) . ? N7 C41 1.49(2) . ? N8 C39 1.256(14) . ? N8 C40 1.486(16) . ? C1 C2 1.391(2) . ? C1 C6 1.391(2) . ? C2 C3 1.391(2) . ? C2 H2A 0.9300 . ? C3 C4 1.391(2) . ? C3 H3A 0.9300 . ? C4 C5 1.391(2) . ? C4 H4A 0.9300 . ? C5 C6 1.391(2) . ? C5 H5A 0.9300 . ? C6 C7 1.459(9) . ? C7 H7A 0.9300 . ? C8 C9 1.526(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.43(2) . ? C10 H10B 0.9300 . ? C11 C16 1.32(2) . ? C11 C12 1.433(10) . ? C12 C13 1.39(3) . ? C12 H12A 0.9300 . ? C13 C14 1.25(3) . ? C13 H13A 0.9300 . ? C14 C15 1.33(2) . ? C14 H14A 0.9300 . ? C15 C16 1.41(2) . ? C15 H15A 0.9300 . ? C17 C18 1.350(19) . ? C17 C22 1.46(2) . ? C18 C19 1.445(9) . ? C18 H18A 0.9300 . ? C19 C20 1.24(2) . ? C19 H19A 0.9300 . ? C20 C21 1.29(2) . ? C20 H20A 0.9300 . ? C21 C22 1.45(2) . ? C21 H21A 0.9300 . ? C22 C23 1.43(2) . ? C23 H23A 0.9300 . ? C24 C25 1.55(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.30(2) . ? C26 H26A 0.9300 . ? C27 C28 1.46(2) . ? C27 C32 1.47(2) . ? C28 C29 1.35(3) . ? C28 H28A 0.9300 . ? C29 C30 1.38(3) . ? C29 H29A 0.9300 . ? C30 C31 1.39(2) . ? C30 H30A 0.9300 . ? C31 C32 1.39(2) . ? C31 H31A 0.9300 . ? C33 C38 1.38(2) . ? C33 C34 1.42(2) . ? C34 C35 1.49(2) . ? C34 H34A 0.9300 . ? C35 C36 1.24(2) . ? C35 H35A 0.9300 . ? C36 C37 1.51(2) . ? C36 H36A 0.9300 . ? C37 C38 1.422(18) . ? C37 H37A 0.9300 . ? C38 C39 1.476(18) . ? C39 H39A 0.9300 . ? C40 C41 1.52(2) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.445(19) . ? C42 H42A 0.9300 . ? C43 C44 1.335(16) . ? C43 C48 1.370(18) . ? C44 C45 1.38(2) . ? C44 H44A 0.9300 . ? C45 C46 1.36(2) . ? C45 H45A 0.9300 . ? C46 C47 1.389(17) . ? C46 H46A 0.9300 . ? C47 C48 1.424(18) . ? C47 H47A 0.9300 . ? C49 C50 1.347(17) . ? C49 C54 1.393(18) . ? C50 C51 1.48(2) . ? C50 H50A 0.9300 . ? C51 C52 1.30(2) . ? C51 H51A 0.9300 . ? C52 C53 1.47(2) . ? C52 H52A 0.9300 . ? C53 C54 1.35(2) . ? C53 H53A 0.9300 . ? C54 C55 1.453(19) . ? C55 H55A 0.9300 . ? C56 C57 1.53(2) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.461(10) . ? C58 H58A 0.9300 . ? C59 C64 1.3899 . ? C59 C60 1.3900 . ? C60 C61 1.3902 . ? C60 H60A 0.9300 . ? C61 C62 1.3899 . ? C61 H61A 0.9300 . ? C62 C63 1.3899 . ? C62 H62A 0.9300 . ? C63 C64 1.3901 . ? C63 H63A 0.9300 . ? O11 C65 1.548(10) . ? O11 H11A 0.8200 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? O12 C66 1.550(10) . ? O12 H12B 0.8200 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? O13 C67 1.548(10) . ? O13 H13B 0.8200 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? O14 C68 1.552(10) . ? O14 H14B 0.8200 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 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 O7 Yb1 O8 138.3(3) . . ? O7 Yb1 O4 90.6(3) . . ? O8 Yb1 O4 114.7(3) . . ? O7 Yb1 O9 79.4(3) . . ? O8 Yb1 O9 78.3(3) . . ? O4 Yb1 O9 166.9(3) . . ? O7 Yb1 O6 79.7(3) . . ? O8 Yb1 O6 79.4(3) . . ? O4 Yb1 O6 69.5(2) . . ? O9 Yb1 O6 116.4(3) . . ? O7 Yb1 N5 74.3(3) . . ? O8 Yb1 N5 136.9(4) . . ? O4 Yb1 N5 84.8(3) . . ? O9 Yb1 N5 84.3(3) . . ? O6 Yb1 N5 143.1(3) . . ? O7 Yb1 N6 141.9(3) . . ? O8 Yb1 N6 72.6(4) . . ? O4 Yb1 N6 92.6(3) . . ? O9 Yb1 N6 90.1(3) . . ? O6 Yb1 N6 136.4(3) . . ? N5 Yb1 N6 68.2(4) . . ? O7 Yb1 C48 68.5(3) . . ? O8 Yb1 C48 79.2(4) . . ? O4 Yb1 C48 88.5(3) . . ? O9 Yb1 C48 95.6(3) . . ? O6 Yb1 C48 21.5(3) . . ? N5 Yb1 C48 142.2(4) . . ? N6 Yb1 C48 149.4(4) . . ? O7 Yb1 Yb2 91.5(2) . . ? O8 Yb1 Yb2 91.2(2) . . ? O4 Yb1 Yb2 36.52(19) . . ? O9 Yb1 Yb2 150.8(2) . . ? O6 Yb1 Yb2 34.43(15) . . ? N5 Yb1 Yb2 120.2(2) . . ? N6 Yb1 Yb2 112.9(2) . . ? C48 Yb1 Yb2 55.4(2) . . ? O6 Yb2 O5 161.7(3) . . ? O6 Yb2 O4 69.9(2) . . ? O5 Yb2 O4 112.2(3) . . ? O6 Yb2 O3 111.6(3) . . ? O5 Yb2 O3 70.6(3) . . ? O4 Yb2 O3 167.5(3) . . ? O6 Yb2 N7 72.3(3) . . ? O5 Yb2 N7 124.6(3) . . ? O4 Yb2 N7 93.8(3) . . ? O3 Yb2 N7 75.4(3) . . ? O6 Yb2 N8 124.9(3) . . ? O5 Yb2 N8 71.9(3) . . ? O4 Yb2 N8 75.6(3) . . ? O3 Yb2 N8 94.3(3) . . ? N7 Yb2 N8 68.5(3) . . ? O6 Yb2 N3 73.9(3) . . ? O5 Yb2 N3 90.7(3) . . ? O4 Yb2 N3 121.3(3) . . ? O3 Yb2 N3 70.1(4) . . ? N7 Yb2 N3 116.9(4) . . ? N8 Yb2 N3 160.0(3) . . ? O6 Yb2 N4 90.7(3) . . ? O5 Yb2 N4 73.9(3) . . ? O4 Yb2 N4 69.6(3) . . ? O3 Yb2 N4 122.3(3) . . ? N7 Yb2 N4 159.8(3) . . ? N8 Yb2 N4 115.8(3) . . ? N3 Yb2 N4 66.4(4) . . ? O6 Yb2 C17 89.9(3) . . ? O5 Yb2 C17 91.1(3) . . ? O4 Yb2 C17 155.9(3) . . ? O3 Yb2 C17 21.7(3) . . ? N7 Yb2 C17 66.9(4) . . ? N8 Yb2 C17 107.9(3) . . ? N3 Yb2 C17 61.5(4) . . ? N4 Yb2 C17 125.4(4) . . ? O6 Yb2 Yb1 35.69(18) . . ? O5 Yb2 Yb1 139.54(19) . . ? O4 Yb2 Yb1 35.64(16) . . ? O3 Yb2 Yb1 147.30(19) . . ? N7 Yb2 Yb1 88.9(2) . . ? N8 Yb2 Yb1 106.56(17) . . ? N3 Yb2 Yb1 93.0(2) . . ? N4 Yb2 Yb1 70.9(2) . . ? C17 Yb2 Yb1 125.6(2) . . ? O6 Yb2 Yb3 140.46(18) . . ? O5 Yb2 Yb3 35.5(2) . . ? O4 Yb2 Yb3 147.63(15) . . ? O3 Yb2 Yb3 36.05(17) . . ? N7 Yb2 Yb3 105.6(2) . . ? N8 Yb2 Yb3 87.51(18) . . ? N3 Yb2 Yb3 72.5(2) . . ? N4 Yb2 Yb3 94.4(2) . . ? C17 Yb2 Yb3 55.7(2) . . ? Yb1 Yb2 Yb3 162.88(2) . . ? O1 Yb3 O2 140.1(3) . . ? O1 Yb3 O3 111.3(3) . . ? O2 Yb3 O3 95.0(3) . . ? O1 Yb3 O5 81.5(4) . . ? O2 Yb3 O5 79.2(3) . . ? O3 Yb3 O5 71.3(3) . . ? O1 Yb3 O10 76.7(3) . . ? O2 Yb3 O10 79.8(3) . . ? O3 Yb3 O10 171.4(3) . . ? O5 Yb3 O10 114.0(3) . . ? O1 Yb3 N1 72.0(4) . . ? O2 Yb3 N1 141.2(3) . . ? O3 Yb3 N1 87.0(3) . . ? O5 Yb3 N1 136.7(3) . . ? O10 Yb3 N1 92.8(3) . . ? O1 Yb3 N2 134.9(4) . . ? O2 Yb3 N2 72.5(4) . . ? O3 Yb3 N2 88.3(3) . . ? O5 Yb3 N2 143.4(4) . . ? O10 Yb3 N2 83.6(3) . . ? N1 Yb3 N2 68.9(4) . . ? O1 Yb3 Yb2 91.5(3) . . ? O2 Yb3 Yb2 92.46(18) . . ? O3 Yb3 Yb2 37.10(19) . . ? O5 Yb3 Yb2 35.21(17) . . ? O10 Yb3 Yb2 149.0(2) . . ? N1 Yb3 Yb2 110.8(2) . . ? N2 Yb3 Yb2 122.8(2) . . ? C1 O1 Yb3 145.8(8) . . ? C16 O2 Yb3 133.8(8) . . ? C17 O3 Yb3 127.7(8) . . ? C17 O3 Yb2 116.5(6) . . ? Yb3 O3 Yb2 106.8(3) . . ? C32 O4 Yb1 124.5(7) . . ? C32 O4 Yb2 119.8(7) . . ? Yb1 O4 Yb2 107.8(3) . . ? C33 O5 Yb2 126.0(7) . . ? C33 O5 Yb3 122.9(6) . . ? Yb2 O5 Yb3 109.3(3) . . ? C48 O6 Yb2 128.5(7) . . ? C48 O6 Yb1 119.4(6) . . ? Yb2 O6 Yb1 109.9(3) . . ? C49 O7 Yb1 130.8(8) . . ? C64 O8 Yb1 144.9(6) . . ? Yb1 O9 H9A 109.5 . . ? Yb3 O10 H10A 109.5 . . ? C7 N1 C8 115.6(12) . . ? C7 N1 Yb3 126.8(12) . . ? C8 N1 Yb3 116.7(8) . . ? C10 N2 C9 119.3(13) . . ? C10 N2 Yb3 127.5(11) . . ? C9 N2 Yb3 113.2(9) . . ? C23 N3 C24 119.5(17) . . ? C23 N3 Yb2 124.0(14) . . ? C24 N3 Yb2 115.1(10) . . ? C26 N4 C25 123.3(13) . . ? C26 N4 Yb2 118.5(10) . . ? C25 N4 Yb2 113.2(10) . . ? C55 N5 C56 119.6(12) . . ? C55 N5 Yb1 125.1(10) . . ? C56 N5 Yb1 115.0(9) . . ? C58 N6 C57 125.0(14) . . ? C58 N6 Yb1 120.1(12) . . ? C57 N6 Yb1 114.5(8) . . ? C42 N7 C41 118.1(12) . . ? C42 N7 Yb2 126.8(10) . . ? C41 N7 Yb2 114.6(9) . . ? C39 N8 C40 117.0(11) . . ? C39 N8 Yb2 127.2(8) . . ? C40 N8 Yb2 115.1(6) . . ? O1 C1 C2 119.7(6) . . ? O1 C1 C6 117.1(5) . . ? C2 C1 C6 120.0 . . ? C1 C2 C3 120.0 . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? 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 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C1 C6 C5 120.0 . . ? C1 C6 C7 114.6(8) . . ? C5 C6 C7 123.0(7) . . ? N1 C7 C6 131.2(15) . . ? N1 C7 H7A 114.4 . . ? C6 C7 H7A 114.4 . . ? N1 C8 C9 106.2(11) . . ? N1 C8 H8A 110.5 . . ? C9 C8 H8A 110.5 . . ? N1 C8 H8B 110.5 . . ? C9 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? N2 C9 C8 111.0(12) . . ? N2 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? N2 C9 H9C 109.4 . . ? C8 C9 H9C 109.4 . . ? H9B C9 H9C 108.0 . . ? N2 C10 C11 126.3(14) . . ? N2 C10 H10B 116.9 . . ? C11 C10 H10B 116.9 . . ? C16 C11 C12 118.3(18) . . ? C16 C11 C10 125.7(13) . . ? C12 C11 C10 115.6(17) . . ? C13 C12 C11 116(2) . . ? C13 C12 H12A 122.1 . . ? C11 C12 H12A 122.1 . . ? C14 C13 C12 126(2) . . ? C14 C13 H13A 117.2 . . ? C12 C13 H13A 117.2 . . ? C13 C14 C15 117(2) . . ? C13 C14 H14A 121.4 . . ? C15 C14 H14A 121.4 . . ? C14 C15 C16 123.1(18) . . ? C14 C15 H15A 118.5 . . ? C16 C15 H15A 118.5 . . ? C11 C16 O2 121.6(14) . . ? C11 C16 C15 118.6(14) . . ? O2 C16 C15 119.8(13) . . ? O3 C17 C18 123.8(14) . . ? O3 C17 C22 119.8(11) . . ? C18 C17 C22 116.4(12) . . ? O3 C17 Yb2 41.8(5) . . ? C18 C17 Yb2 134.7(11) . . ? C22 C17 Yb2 94.9(7) . . ? C17 C18 C19 123.4(15) . . ? C17 C18 H18A 118.3 . . ? C19 C18 H18A 118.3 . . ? C20 C19 C18 119.1(17) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.4 . . ? C19 C20 C21 122(2) . . ? C19 C20 H20A 119.0 . . ? C21 C20 H20A 119.0 . . ? C20 C21 C22 125(2) . . ? C20 C21 H21A 117.3 . . ? C22 C21 H21A 117.3 . . ? C23 C22 C21 124.6(16) . . ? C23 C22 C17 122.2(13) . . ? C21 C22 C17 113.3(14) . . ? N3 C23 C22 128.1(19) . . ? N3 C23 H23A 116.0 . . ? C22 C23 H23A 116.0 . . ? N3 C24 C25 109.2(14) . . ? N3 C24 H24A 109.8 . . ? C25 C24 H24A 109.8 . . ? N3 C24 H24B 109.8 . . ? C25 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? N4 C25 C24 108.8(14) . . ? N4 C25 H25A 109.9 . . ? C24 C25 H25A 109.9 . . ? N4 C25 H25B 109.9 . . ? C24 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? C27 C26 N4 130.7(13) . . ? C27 C26 H26A 114.7 . . ? N4 C26 H26A 114.7 . . ? C26 C27 C28 121.4(14) . . ? C26 C27 C32 125.4(12) . . ? C28 C27 C32 112.9(14) . . ? C29 C28 C27 119.2(17) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C28 C29 C30 128.1(19) . . ? C28 C29 H29A 116.0 . . ? C30 C29 H29A 116.0 . . ? C29 C30 C31 115.0(19) . . ? C29 C30 H30A 122.5 . . ? C31 C30 H30A 122.5 . . ? C32 C31 C30 121.4(17) . . ? C32 C31 H31A 119.3 . . ? C30 C31 H31A 119.3 . . ? O4 C32 C31 120.3(14) . . ? O4 C32 C27 116.5(13) . . ? C31 C32 C27 123.2(12) . . ? O5 C33 C38 122.4(13) . . ? O5 C33 C34 116.3(14) . . ? C38 C33 C34 121.3(12) . . ? C33 C34 C35 114.6(14) . . ? C33 C34 H34A 122.7 . . ? C35 C34 H34A 122.7 . . ? C36 C35 C34 122.2(16) . . ? C36 C35 H35A 118.9 . . ? C34 C35 H35A 118.9 . . ? C35 C36 C37 126.3(17) . . ? C35 C36 H36A 116.8 . . ? C37 C36 H36A 116.8 . . ? C38 C37 C36 110.2(15) . . ? C38 C37 H37A 124.9 . . ? C36 C37 H37A 124.9 . . ? C33 C38 C37 125.2(14) . . ? C33 C38 C39 122.2(12) . . ? C37 C38 C39 112.4(14) . . ? N8 C39 C38 125.7(13) . . ? N8 C39 H39A 117.2 . . ? C38 C39 H39A 117.2 . . ? N8 C40 C41 105.1(12) . . ? N8 C40 H40A 110.7 . . ? C41 C40 H40A 110.7 . . ? N8 C40 H40B 110.7 . . ? C41 C40 H40B 110.7 . . ? H40A C40 H40B 108.8 . . ? N7 C41 C40 107.4(13) . . ? N7 C41 H41A 110.2 . . ? C40 C41 H41A 110.2 . . ? N7 C41 H41B 110.2 . . ? C40 C41 H41B 110.2 . . ? H41A C41 H41B 108.5 . . ? N7 C42 C43 127.4(12) . . ? N7 C42 H42A 116.3 . . ? C43 C42 H42A 116.3 . . ? C44 C43 C48 120.6(13) . . ? C44 C43 C42 119.2(12) . . ? C48 C43 C42 120.2(10) . . ? C43 C44 C45 122.2(14) . . ? C43 C44 H44A 118.9 . . ? C45 C44 H44A 118.9 . . ? C46 C45 C44 121.0(13) . . ? C46 C45 H45A 119.5 . . ? C44 C45 H45A 119.5 . . ? C45 C46 C47 116.7(14) . . ? C45 C46 H46A 121.6 . . ? C47 C46 H46A 121.6 . . ? C46 C47 C48 122.6(13) . . ? C46 C47 H47A 118.7 . . ? C48 C47 H47A 118.7 . . ? O6 C48 C43 124.8(12) . . ? O6 C48 C47 118.4(13) . . ? C43 C48 C47 116.8(11) . . ? O6 C48 Yb1 39.1(5) . . ? C43 C48 Yb1 130.9(9) . . ? C47 C48 Yb1 96.2(8) . . ? O7 C49 C50 118.4(12) . . ? O7 C49 C54 122.6(11) . . ? C50 C49 C54 118.9(12) . . ? C49 C50 C51 120.2(13) . . ? C49 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? C52 C51 C50 118.5(15) . . ? C52 C51 H51A 120.8 . . ? C50 C51 H51A 120.8 . . ? C51 C52 C53 121.9(16) . . ? C51 C52 H52A 119.1 . . ? C53 C52 H52A 119.1 . . ? C54 C53 C52 116.3(17) . . ? C54 C53 H53A 121.8 . . ? C52 C53 H53A 121.8 . . ? C53 C54 C49 123.0(14) . . ? C53 C54 C55 113.6(15) . . ? C49 C54 C55 123.1(12) . . ? N5 C55 C54 128.1(14) . . ? N5 C55 H55A 116.0 . . ? C54 C55 H55A 116.0 . . ? N5 C56 C57 108.9(11) . . ? N5 C56 H56A 109.9 . . ? C57 C56 H56A 109.9 . . ? N5 C56 H56B 109.9 . . ? C57 C56 H56B 109.9 . . ? H56A C56 H56B 108.3 . . ? N6 C57 C56 110.0(11) . . ? N6 C57 H57A 109.7 . . ? C56 C57 H57A 109.7 . . ? N6 C57 H57B 109.7 . . ? C56 C57 H57B 109.7 . . ? H57A C57 H57B 108.2 . . ? N6 C58 C59 138.7(19) . . ? N6 C58 H58A 110.7 . . ? C59 C58 H58A 110.7 . . ? C64 C59 C60 120.0 . . ? C64 C59 C58 116.3(10) . . ? C60 C59 C58 121.2(10) . . ? C59 C60 C61 120.0 . . ? C59 C60 H60A 120.0 . . ? C61 C60 H60A 120.0 . . ? C62 C61 C60 120.0 . . ? C62 C61 H61A 120.0 . . ? C60 C61 H61A 120.0 . . ? C63 C62 C61 120.0 . . ? C63 C62 H62A 120.0 . . ? C61 C62 H62A 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63A 120.0 . . ? C64 C63 H63A 120.0 . . ? O8 C64 C59 119.3(4) . . ? O8 C64 C63 120.6(4) . . ? C59 C64 C63 120.0 . . ? C65 O11 H11A 109.5 . . ? O11 C65 H65A 109.5 . . ? O11 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? O11 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C66 O12 H12B 109.5 . . ? O12 C66 H66A 109.5 . . ? O12 C66 H66B 109.4 . . ? H66A C66 H66B 109.5 . . ? O12 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C67 O13 H13B 109.5 . . ? O13 C67 H67A 109.5 . . ? O13 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? O13 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C68 O14 H14B 109.5 . . ? O14 C68 H68A 109.4 . . ? O14 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? O14 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.305 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.181 _database_code_depnum_ccdc_archive 'CCDC 950239' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H68 N9 O13 Yb2, N O3' _chemical_formula_sum 'C66 H68 N10 O16 Yb2' _chemical_formula_weight 1603.38 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.211(4) _cell_length_b 10.184(2) _cell_length_c 29.121(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.33(3) _cell_angle_gamma 90.00 _cell_volume 6518(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 20261 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 2.929 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5651 _exptl_absorpt_correction_T_max 0.7389 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35005 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11313 _reflns_number_gt 10105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _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^)+(0.0204P)^2^+29.8058P] 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 11313 _refine_ls_number_parameters 847 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.002 _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 Yb1 Yb 0.900180(9) 0.19173(2) 0.774685(7) 0.02344(6) Uani 1 1 d . . . Yb2 Yb 0.697282(9) 0.864738(19) 0.491150(7) 0.02185(6) Uani 1 1 d . . . N1 N 0.89292(18) -0.0292(4) 0.80615(14) 0.0287(9) Uani 1 1 d . . . N2 N 0.87200(18) 0.0301(4) 0.71240(14) 0.0273(9) Uani 1 1 d . . . N3 N 0.7703(2) 0.3749(6) 0.6811(2) 0.0586(15) Uani 1 1 d . . . N4 N 0.8083(2) 0.6498(6) 0.60641(17) 0.0546(15) Uani 1 1 d . . . N5 N 0.72807(19) 1.0410(4) 0.54676(14) 0.0308(9) Uani 1 1 d . . . N6 N 0.72985(17) 1.0620(4) 0.45275(14) 0.0266(9) Uani 1 1 d . . . N7 N 0.51844(19) 0.8239(4) 0.50649(14) 0.0286(9) Uani 1 1 d . . . N8 N 0.50568(19) 0.5671(4) 0.59444(14) 0.0288(9) Uani 1 1 d . . . N9 N 1.0295(2) 0.1355(4) 0.78494(16) 0.0336(10) Uani 1 1 d . . . N10 N 0.3556(2) 0.6067(5) 0.44175(17) 0.0392(11) Uani 1 1 d . . . O1 O 0.88536(17) 0.2179(3) 0.84591(12) 0.0353(8) Uani 1 1 d . . . O2 O 0.91127(18) 0.2932(3) 0.70955(12) 0.0366(9) Uani 1 1 d . . . O3 O 0.80241(15) 0.2315(4) 0.75485(12) 0.0337(8) Uani 1 1 d . . . H3C H 0.8113 0.3097 0.7550 0.040 Uiso 1 1 calc R . . O4 O 0.78484(15) 0.7799(3) 0.52755(13) 0.0344(8) Uani 1 1 d . . . H4A H 0.7758 0.7029 0.5219 0.041 Uiso 1 1 calc R . . O5 O 0.65604(15) 0.8141(3) 0.55320(11) 0.0284(7) Uani 1 1 d . . . O6 O 0.71672(17) 0.8049(3) 0.42378(12) 0.0353(8) Uani 1 1 d . . . O7 O 0.60489(14) 0.9341(3) 0.46640(11) 0.0300(8) Uani 1 1 d . . . H7C H 0.5900 0.8896 0.4854 0.036 Uiso 1 1 calc R . . O8 O 0.5355(2) 0.5704(5) 0.68209(14) 0.0605(13) Uani 1 1 d . . . H8E H 0.5176 0.6348 0.6700 0.091 Uiso 1 1 calc R . . O9 O 1.00876(17) 0.2080(4) 0.81389(14) 0.0453(10) Uani 1 1 d . . . O10 O 0.99219(17) 0.0843(4) 0.75446(14) 0.0419(9) Uani 1 1 d . . . O11 O 1.08459(16) 0.1145(4) 0.78676(15) 0.0458(10) Uani 1 1 d . . . O12 O 0.91735(16) 0.4168(3) 0.78949(12) 0.0332(8) Uani 1 1 d . . . H12B H 0.8840 0.4462 0.7785 0.040 Uiso 1 1 calc R . . O13 O 0.66820(16) 0.6408(3) 0.48396(12) 0.0326(8) Uani 1 1 d . . . H13C H 0.6700 0.6178 0.5111 0.039 Uiso 1 1 calc R . . O14 O 0.3283(2) 0.4990(4) 0.43558(15) 0.0564(12) Uani 1 1 d . . . O15 O 0.38690(19) 0.6290(4) 0.47928(16) 0.0519(11) Uani 1 1 d . . . O16 O 0.3506(2) 0.6898(5) 0.41057(18) 0.0713(15) Uani 1 1 d . . . C1 C 0.8817(2) 0.1557(5) 0.88429(17) 0.0304(11) Uani 1 1 d . . . C2 C 0.8772(2) 0.2249(6) 0.92542(17) 0.0361(12) Uani 1 1 d . . . H2A H 0.8769 0.3162 0.9250 0.043 Uiso 1 1 calc R . . C3 C 0.8731(3) 0.1600(7) 0.9662(2) 0.0479(15) Uani 1 1 d . . . H3B H 0.8706 0.2080 0.9930 0.057 Uiso 1 1 calc R . . C4 C 0.8727(3) 0.0235(7) 0.9679(2) 0.0574(18) Uani 1 1 d . . . H4B H 0.8695 -0.0195 0.9956 0.069 Uiso 1 1 calc R . . C5 C 0.8769(3) -0.0462(7) 0.9289(2) 0.0536(17) Uani 1 1 d . . . H5A H 0.8765 -0.1374 0.9301 0.064 Uiso 1 1 calc R . . C6 C 0.8817(2) 0.0164(5) 0.88687(18) 0.0335(12) Uani 1 1 d . . . C7 C 0.8859(2) -0.0659(5) 0.84757(18) 0.0326(12) Uani 1 1 d . . . H7B H 0.8833 -0.1559 0.8524 0.039 Uiso 1 1 calc R . . C8 C 0.8938(2) -0.1353(5) 0.77159(17) 0.0310(11) Uani 1 1 d . . . H8B H 0.8810 -0.2177 0.7838 0.037 Uiso 1 1 calc R . . H8C H 0.9345 -0.1462 0.7638 0.037 Uiso 1 1 calc R . . C9 C 0.8502(2) -0.0947(5) 0.72917(19) 0.0354(12) Uani 1 1 d . . . H9A H 0.8488 -0.1613 0.7053 0.042 Uiso 1 1 calc R . . H9B H 0.8095 -0.0838 0.7371 0.042 Uiso 1 1 calc R . . C10 C 0.8797(2) 0.0347(5) 0.66998(17) 0.0302(11) Uani 1 1 d . . . H10A H 0.8675 -0.0388 0.6521 0.036 Uiso 1 1 calc R . . C11 C 0.9053(2) 0.1421(5) 0.64659(17) 0.0292(11) Uani 1 1 d . . . C12 C 0.9172(3) 0.1185(6) 0.60112(19) 0.0396(13) Uani 1 1 d . . . H12A H 0.9051 0.0392 0.5868 0.047 Uiso 1 1 calc R . . C13 C 0.9463(3) 0.2095(6) 0.5773(2) 0.0456(15) Uani 1 1 d . . . H13A H 0.9537 0.1921 0.5473 0.055 Uiso 1 1 calc R . . C14 C 0.9643(3) 0.3269(6) 0.59842(19) 0.0429(14) Uani 1 1 d . . . H14A H 0.9840 0.3890 0.5825 0.052 Uiso 1 1 calc R . . C15 C 0.9533(3) 0.3533(6) 0.64296(18) 0.0385(13) Uani 1 1 d . . . H15A H 0.9664 0.4327 0.6567 0.046 Uiso 1 1 calc R . . C16 C 0.9229(2) 0.2635(5) 0.66802(17) 0.0292(11) Uani 1 1 d . . . C17 C 0.7454(2) 0.2190(5) 0.75931(17) 0.0264(10) Uani 1 1 d . . . C18 C 0.7264(3) 0.1408(5) 0.7946(2) 0.0399(13) Uani 1 1 d . . . H18A H 0.7553 0.0981 0.8158 0.048 Uiso 1 1 calc R . . C19 C 0.6660(3) 0.1275(6) 0.7979(2) 0.0544(17) Uani 1 1 d . . . H19A H 0.6544 0.0744 0.8212 0.065 Uiso 1 1 calc R . . C20 C 0.6211(3) 0.1914(7) 0.7674(3) 0.0614(19) Uani 1 1 d . . . H20A H 0.5802 0.1824 0.7707 0.074 Uiso 1 1 calc R . . C21 C 0.6377(3) 0.2670(6) 0.7327(3) 0.0546(17) Uani 1 1 d . . . H21A H 0.6080 0.3082 0.7118 0.066 Uiso 1 1 calc R . . C22 C 0.7000(2) 0.2830(5) 0.7285(2) 0.0371(13) Uani 1 1 d . . . C23 C 0.7147(3) 0.3556(7) 0.6900(2) 0.0552(17) Uani 1 1 d . . . H23A H 0.6829 0.3919 0.6697 0.066 Uiso 1 1 calc R . . C24 C 0.7873(3) 0.4439(7) 0.6376(2) 0.063(2) Uani 1 1 d . . . H24A H 0.8271 0.4160 0.6315 0.075 Uiso 1 1 calc R . . H24B H 0.7575 0.4250 0.6106 0.075 Uiso 1 1 calc R . . C25 C 0.7873(3) 0.5812(7) 0.6488(2) 0.0588(18) Uani 1 1 d . . . H25A H 0.8153 0.5993 0.6769 0.071 Uiso 1 1 calc R . . H25B H 0.7469 0.6103 0.6532 0.071 Uiso 1 1 calc R . . C26 C 0.8649(3) 0.6746(6) 0.6016(2) 0.0492(16) Uani 1 1 d . . . H26A H 0.8947 0.6443 0.6250 0.059 Uiso 1 1 calc R . . C27 C 0.8851(2) 0.7427(5) 0.56468(18) 0.0302(11) Uani 1 1 d . . . C28 C 0.9483(2) 0.7611(6) 0.56448(19) 0.0394(13) Uani 1 1 d . . . H28A H 0.9759 0.7265 0.5885 0.047 Uiso 1 1 calc R . . C29 C 0.9693(3) 0.8285(6) 0.5297(2) 0.0449(14) Uani 1 1 d . . . H29A H 1.0108 0.8406 0.5300 0.054 Uiso 1 1 calc R . . C30 C 0.9277(3) 0.8795(6) 0.4936(2) 0.0422(14) Uani 1 1 d . . . H30A H 0.9420 0.9244 0.4695 0.051 Uiso 1 1 calc R . . C31 C 0.8667(2) 0.8646(5) 0.49280(16) 0.0291(11) Uani 1 1 d . . . H31A H 0.8402 0.9011 0.4685 0.035 Uiso 1 1 calc R . . C32 C 0.8428(2) 0.7955(5) 0.52787(18) 0.0277(11) Uani 1 1 d . . . C33 C 0.6655(2) 0.8356(5) 0.59794(16) 0.0282(11) Uani 1 1 d . . . C34 C 0.6420(2) 0.7470(6) 0.62797(17) 0.0315(11) Uani 1 1 d . . . H34A H 0.6211 0.6726 0.6158 0.038 Uiso 1 1 calc R . . C35 C 0.6495(2) 0.7696(6) 0.67554(19) 0.0375(13) Uani 1 1 d . . . H35A H 0.6341 0.7100 0.6951 0.045 Uiso 1 1 calc R . . C36 C 0.6801(2) 0.8812(6) 0.69402(18) 0.0406(14) Uani 1 1 d . . . H36A H 0.6845 0.8969 0.7258 0.049 Uiso 1 1 calc R . . C37 C 0.7035(2) 0.9677(6) 0.66555(19) 0.0403(13) Uani 1 1 d . . . H37A H 0.7237 1.0422 0.6782 0.048 Uiso 1 1 calc R . . C38 C 0.6978(2) 0.9465(5) 0.61730(17) 0.0325(12) Uani 1 1 d . . . C39 C 0.7239(2) 1.0444(5) 0.59025(18) 0.0323(12) Uani 1 1 d . . . H39A H 0.7395 1.1189 0.6062 0.039 Uiso 1 1 calc R . . C40 C 0.7579(3) 1.1541(5) 0.52879(19) 0.0364(12) Uani 1 1 d . . . H40A H 0.8006 1.1352 0.5282 0.044 Uiso 1 1 calc R . . H40B H 0.7550 1.2300 0.5485 0.044 Uiso 1 1 calc R . . C41 C 0.7264(3) 1.1819(5) 0.48024(19) 0.0358(12) Uani 1 1 d . . . H41A H 0.6842 1.2056 0.4809 0.043 Uiso 1 1 calc R . . H41B H 0.7462 1.2541 0.4667 0.043 Uiso 1 1 calc R . . C42 C 0.7467(2) 1.0769(5) 0.41252(18) 0.0300(11) Uani 1 1 d . . . H42A H 0.7559 1.1620 0.4043 0.036 Uiso 1 1 calc R . . C43 C 0.7527(2) 0.9763(5) 0.37927(16) 0.0288(11) Uani 1 1 d . . . C44 C 0.7739(3) 1.0124(6) 0.33771(19) 0.0414(13) Uani 1 1 d . . . H44A H 0.7856 1.0988 0.3337 0.050 Uiso 1 1 calc R . . C45 C 0.7776(3) 0.9229(7) 0.30329(19) 0.0464(15) Uani 1 1 d . . . H45A H 0.7917 0.9483 0.2761 0.056 Uiso 1 1 calc R . . C46 C 0.7603(3) 0.7944(6) 0.30929(19) 0.0442(14) Uani 1 1 d . . . H46A H 0.7614 0.7342 0.2854 0.053 Uiso 1 1 calc R . . C47 C 0.7415(2) 0.7538(6) 0.35000(18) 0.0381(13) Uani 1 1 d . . . H47A H 0.7319 0.6659 0.3537 0.046 Uiso 1 1 calc R . . C48 C 0.7364(2) 0.8432(5) 0.38604(18) 0.0300(11) Uani 1 1 d . . . C49 C 0.5644(2) 0.9519(4) 0.42953(16) 0.0241(10) Uani 1 1 d . . . C50 C 0.5797(2) 1.0182(5) 0.39074(17) 0.0313(11) Uani 1 1 d . . . H50A H 0.6192 1.0482 0.3906 0.038 Uiso 1 1 calc R . . C51 C 0.5359(2) 1.0389(6) 0.35269(18) 0.0371(13) Uani 1 1 d . . . H51A H 0.5463 1.0850 0.3274 0.045 Uiso 1 1 calc R . . C52 C 0.4767(2) 0.9926(6) 0.35109(18) 0.0381(13) Uani 1 1 d . . . H52A H 0.4483 1.0053 0.3247 0.046 Uiso 1 1 calc R . . C53 C 0.4608(2) 0.9280(5) 0.38884(18) 0.0326(12) Uani 1 1 d . . . H53A H 0.4212 0.8974 0.3881 0.039 Uiso 1 1 calc R . . C54 C 0.5038(2) 0.9075(5) 0.42884(16) 0.0257(10) Uani 1 1 d . . . C55 C 0.4834(2) 0.8475(5) 0.46778(16) 0.0269(10) Uani 1 1 d . . . H55A H 0.4426 0.8238 0.4654 0.032 Uiso 1 1 calc R . . C56 C 0.4971(2) 0.7626(5) 0.54677(17) 0.0297(11) Uani 1 1 d . . . H56A H 0.4535 0.7743 0.5447 0.036 Uiso 1 1 calc R . . H56B H 0.5163 0.8050 0.5750 0.036 Uiso 1 1 calc R . . C57 C 0.5123(2) 0.6166(5) 0.54876(17) 0.0315(11) Uani 1 1 d . . . H57A H 0.4850 0.5698 0.5253 0.038 Uiso 1 1 calc R . . H57B H 0.5536 0.6031 0.5427 0.038 Uiso 1 1 calc R . . C58 C 0.4689(2) 0.4725(5) 0.59838(17) 0.0293(11) Uani 1 1 d . . . H58A H 0.4465 0.4367 0.5719 0.035 Uiso 1 1 calc R . . C59 C 0.4616(2) 0.4202(5) 0.64360(17) 0.0306(11) Uani 1 1 d . . . C60 C 0.4212(3) 0.3177(5) 0.6474(2) 0.0417(13) Uani 1 1 d . . . H60A H 0.3978 0.2843 0.6209 0.050 Uiso 1 1 calc R . . C61 C 0.4155(3) 0.2649(6) 0.6905(2) 0.0488(15) Uani 1 1 d . . . H61A H 0.3889 0.1956 0.6930 0.059 Uiso 1 1 calc R . . C62 C 0.4499(3) 0.3166(7) 0.7297(2) 0.0508(17) Uani 1 1 d . . . H62A H 0.4465 0.2813 0.7586 0.061 Uiso 1 1 calc R . . C63 C 0.4890(3) 0.4193(7) 0.7262(2) 0.0498(16) Uani 1 1 d . . . H63A H 0.5113 0.4537 0.7530 0.060 Uiso 1 1 calc R . . C64 C 0.4955(2) 0.4719(6) 0.68423(19) 0.0389(13) Uani 1 1 d . . . C65 C 0.9396(3) 0.4860(5) 0.83115(18) 0.0380(13) Uani 1 1 d . . . H65A H 0.9405 0.5784 0.8248 0.057 Uiso 1 1 calc R . . H65B H 0.9800 0.4562 0.8427 0.057 Uiso 1 1 calc R . . H65C H 0.9133 0.4698 0.8540 0.057 Uiso 1 1 calc R . . C66 C 0.6947(3) 0.5414(5) 0.4584(2) 0.0524(17) Uani 1 1 d . . . H66A H 0.6745 0.4593 0.4615 0.079 Uiso 1 1 calc R . . H66B H 0.7372 0.5327 0.4703 0.079 Uiso 1 1 calc R . . H66C H 0.6903 0.5657 0.4262 0.079 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 0.02752(12) 0.02069(11) 0.02330(11) -0.00029(8) 0.00771(8) -0.00015(8) Yb2 0.02173(11) 0.02041(11) 0.02289(11) 0.00113(8) 0.00150(8) -0.00051(8) N1 0.027(2) 0.026(2) 0.033(2) 0.0008(18) 0.0029(17) 0.0010(17) N2 0.029(2) 0.022(2) 0.030(2) -0.0002(17) 0.0002(17) -0.0014(17) N3 0.040(3) 0.072(4) 0.062(4) 0.034(3) 0.003(3) -0.013(3) N4 0.040(3) 0.078(4) 0.040(3) 0.027(3) -0.012(2) -0.025(3) N5 0.036(2) 0.025(2) 0.031(2) -0.0024(18) 0.0019(18) -0.0033(18) N6 0.025(2) 0.024(2) 0.030(2) 0.0014(17) 0.0013(17) 0.0015(17) N7 0.034(2) 0.026(2) 0.027(2) 0.0016(17) 0.0102(18) 0.0020(18) N8 0.039(2) 0.024(2) 0.023(2) 0.0011(17) 0.0032(18) 0.0012(19) N9 0.036(3) 0.025(2) 0.043(3) 0.002(2) 0.015(2) -0.0012(19) N10 0.046(3) 0.033(3) 0.042(3) 0.012(2) 0.014(2) 0.012(2) O1 0.055(2) 0.0289(19) 0.0256(18) -0.0003(15) 0.0164(17) -0.0008(17) O2 0.059(2) 0.0277(19) 0.0252(18) -0.0001(15) 0.0131(17) -0.0055(17) O3 0.0294(19) 0.034(2) 0.038(2) 0.0049(16) 0.0072(16) 0.0001(15) O4 0.0285(19) 0.030(2) 0.044(2) 0.0083(16) 0.0014(16) -0.0004(15) O5 0.0302(18) 0.035(2) 0.0197(17) 0.0002(14) 0.0021(14) -0.0057(15) O6 0.052(2) 0.0242(19) 0.0323(19) -0.0007(15) 0.0166(17) -0.0062(16) O7 0.0225(17) 0.036(2) 0.0309(19) 0.0082(15) 0.0038(14) 0.0016(15) O8 0.070(3) 0.077(3) 0.032(2) 0.005(2) 0.000(2) -0.035(3) O9 0.037(2) 0.053(3) 0.043(2) -0.021(2) -0.0058(17) 0.0102(18) O10 0.033(2) 0.050(2) 0.045(2) -0.0185(19) 0.0106(18) -0.0059(18) O11 0.025(2) 0.041(2) 0.072(3) -0.001(2) 0.0098(19) 0.0018(17) O12 0.040(2) 0.0287(19) 0.0306(19) -0.0026(15) 0.0051(16) 0.0013(16) O13 0.042(2) 0.0245(18) 0.0328(19) -0.0001(15) 0.0126(16) -0.0029(15) O14 0.086(3) 0.029(2) 0.048(3) 0.0050(19) -0.011(2) -0.006(2) O15 0.049(3) 0.047(3) 0.059(3) 0.008(2) 0.005(2) -0.014(2) O16 0.081(4) 0.058(3) 0.077(3) 0.038(3) 0.016(3) 0.005(3) C1 0.020(2) 0.041(3) 0.031(3) 0.002(2) 0.006(2) 0.000(2) C2 0.031(3) 0.050(3) 0.027(3) -0.002(2) 0.004(2) 0.000(2) C3 0.041(3) 0.074(5) 0.030(3) -0.002(3) 0.011(3) 0.001(3) C4 0.070(5) 0.073(5) 0.029(3) 0.019(3) 0.005(3) 0.003(4) C5 0.076(5) 0.051(4) 0.036(3) 0.015(3) 0.014(3) -0.001(3) C6 0.031(3) 0.038(3) 0.031(3) 0.008(2) 0.005(2) -0.003(2) C7 0.028(3) 0.030(3) 0.039(3) 0.011(2) 0.000(2) 0.000(2) C8 0.038(3) 0.020(3) 0.034(3) 0.000(2) -0.001(2) -0.002(2) C9 0.040(3) 0.027(3) 0.037(3) 0.001(2) -0.001(2) -0.008(2) C10 0.028(3) 0.032(3) 0.027(3) -0.007(2) -0.007(2) 0.003(2) C11 0.025(3) 0.032(3) 0.029(3) 0.000(2) 0.002(2) 0.005(2) C12 0.043(3) 0.043(3) 0.033(3) -0.010(2) 0.007(2) 0.005(3) C13 0.048(4) 0.062(4) 0.030(3) -0.002(3) 0.017(3) 0.010(3) C14 0.041(3) 0.059(4) 0.031(3) 0.012(3) 0.014(2) -0.005(3) C15 0.046(3) 0.039(3) 0.030(3) -0.002(2) 0.005(2) -0.011(3) C16 0.031(3) 0.032(3) 0.026(3) -0.001(2) 0.007(2) -0.001(2) C17 0.027(3) 0.023(2) 0.029(3) -0.004(2) 0.002(2) -0.002(2) C18 0.043(3) 0.032(3) 0.047(3) 0.005(3) 0.011(3) -0.004(2) C19 0.060(4) 0.045(4) 0.064(4) 0.009(3) 0.029(4) -0.015(3) C20 0.035(4) 0.063(5) 0.091(6) 0.008(4) 0.023(4) -0.010(3) C21 0.033(3) 0.048(4) 0.083(5) 0.008(3) 0.008(3) -0.003(3) C22 0.028(3) 0.039(3) 0.043(3) 0.008(3) 0.001(2) -0.003(2) C23 0.042(4) 0.054(4) 0.065(4) 0.026(3) -0.006(3) -0.005(3) C24 0.076(5) 0.059(4) 0.045(4) -0.012(3) -0.018(3) 0.023(4) C25 0.046(4) 0.064(4) 0.062(4) -0.023(4) -0.012(3) 0.017(3) C26 0.034(3) 0.055(4) 0.053(4) 0.017(3) -0.011(3) -0.006(3) C27 0.028(3) 0.027(3) 0.034(3) 0.004(2) -0.001(2) 0.000(2) C28 0.031(3) 0.047(3) 0.038(3) 0.001(3) -0.004(2) 0.004(3) C29 0.025(3) 0.063(4) 0.048(3) -0.001(3) 0.009(3) -0.001(3) C30 0.039(3) 0.054(4) 0.036(3) 0.003(3) 0.014(3) -0.007(3) C31 0.028(3) 0.035(3) 0.022(2) 0.000(2) -0.006(2) 0.002(2) C32 0.026(3) 0.021(2) 0.036(3) -0.001(2) 0.006(2) 0.001(2) C33 0.023(2) 0.037(3) 0.025(3) -0.002(2) 0.0006(19) 0.006(2) C34 0.024(3) 0.043(3) 0.028(3) 0.000(2) 0.003(2) 0.002(2) C35 0.023(3) 0.056(4) 0.034(3) 0.004(3) 0.007(2) 0.006(2) C36 0.033(3) 0.064(4) 0.023(3) -0.003(3) 0.001(2) 0.003(3) C37 0.034(3) 0.047(3) 0.038(3) -0.016(3) -0.001(2) -0.001(3) C38 0.031(3) 0.036(3) 0.030(3) -0.005(2) 0.003(2) 0.005(2) C39 0.031(3) 0.027(3) 0.036(3) -0.009(2) -0.005(2) 0.000(2) C40 0.041(3) 0.027(3) 0.039(3) -0.005(2) 0.001(2) -0.010(2) C41 0.040(3) 0.019(3) 0.050(3) -0.002(2) 0.013(3) 0.000(2) C42 0.031(3) 0.022(3) 0.037(3) 0.006(2) 0.005(2) -0.002(2) C43 0.026(3) 0.035(3) 0.025(2) 0.005(2) 0.002(2) 0.002(2) C44 0.047(3) 0.043(3) 0.035(3) 0.010(3) 0.010(3) -0.005(3) C45 0.045(3) 0.071(4) 0.024(3) 0.006(3) 0.009(2) -0.006(3) C46 0.041(3) 0.063(4) 0.030(3) -0.008(3) 0.009(2) 0.000(3) C47 0.042(3) 0.041(3) 0.033(3) -0.006(2) 0.010(2) -0.005(3) C48 0.026(3) 0.030(3) 0.034(3) -0.002(2) 0.007(2) 0.000(2) C49 0.026(2) 0.019(2) 0.026(2) 0.0001(19) 0.000(2) 0.0079(19) C50 0.030(3) 0.036(3) 0.029(3) 0.002(2) 0.008(2) 0.003(2) C51 0.040(3) 0.042(3) 0.031(3) 0.010(2) 0.008(2) 0.007(3) C52 0.031(3) 0.050(4) 0.031(3) 0.006(3) -0.004(2) 0.008(2) C53 0.021(2) 0.042(3) 0.033(3) 0.004(2) -0.004(2) 0.003(2) C54 0.030(3) 0.023(2) 0.023(2) 0.0012(19) 0.002(2) 0.005(2) C55 0.025(2) 0.027(3) 0.028(3) 0.001(2) 0.001(2) 0.004(2) C56 0.037(3) 0.023(3) 0.032(3) 0.000(2) 0.014(2) 0.003(2) C57 0.038(3) 0.028(3) 0.030(3) 0.001(2) 0.010(2) 0.005(2) C58 0.033(3) 0.027(3) 0.028(3) -0.003(2) 0.003(2) 0.004(2) C59 0.035(3) 0.029(3) 0.030(3) 0.002(2) 0.010(2) 0.005(2) C60 0.053(4) 0.034(3) 0.040(3) -0.002(3) 0.013(3) 0.001(3) C61 0.050(4) 0.039(3) 0.062(4) 0.010(3) 0.025(3) -0.001(3) C62 0.048(4) 0.063(4) 0.047(4) 0.023(3) 0.024(3) 0.016(3) C63 0.040(3) 0.077(5) 0.032(3) 0.012(3) 0.006(3) 0.003(3) C64 0.037(3) 0.048(3) 0.033(3) 0.004(3) 0.009(2) 0.003(3) C65 0.048(3) 0.033(3) 0.032(3) -0.009(2) 0.003(2) -0.007(3) C66 0.074(4) 0.025(3) 0.065(4) 0.006(3) 0.033(4) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.163(3) . ? Yb1 O3 2.202(3) . ? Yb1 O2 2.205(3) . ? Yb1 O12 2.353(3) . ? Yb1 N1 2.443(4) . ? Yb1 N2 2.462(4) . ? Yb1 O10 2.463(4) . ? Yb1 O9 2.520(4) . ? Yb1 N9 2.901(4) . ? Yb2 O6 2.157(3) . ? Yb2 O7 2.191(3) . ? Yb2 O5 2.202(3) . ? Yb2 O4 2.248(3) . ? Yb2 O13 2.371(3) . ? Yb2 N5 2.448(4) . ? Yb2 N6 2.459(4) . ? N1 C7 1.294(6) . ? N1 C8 1.479(6) . ? N2 C10 1.272(6) . ? N2 C9 1.468(6) . ? N3 C23 1.311(8) . ? N3 C24 1.543(9) . ? N4 C26 1.310(7) . ? N4 C25 1.548(9) . ? N5 C39 1.284(6) . ? N5 C40 1.463(6) . ? N6 C42 1.289(6) . ? N6 C41 1.468(6) . ? N7 C55 1.296(6) . ? N7 C56 1.466(6) . ? N8 C58 1.279(6) . ? N8 C57 1.450(6) . ? N9 O11 1.236(6) . ? N9 O10 1.238(6) . ? N9 O9 1.257(5) . ? N10 O15 1.228(6) . ? N10 O16 1.235(6) . ? N10 O14 1.254(6) . ? O1 C1 1.297(6) . ? O2 C16 1.308(6) . ? O3 C17 1.298(6) . ? O3 H3C 0.8200 . ? O4 C32 1.296(6) . ? O4 H4A 0.8200 . ? O5 C33 1.308(6) . ? O6 C48 1.300(6) . ? O7 C49 1.310(6) . ? O7 H7C 0.8200 . ? O8 C64 1.347(7) . ? O8 H8E 0.8200 . ? O12 C65 1.428(6) . ? O12 H12B 0.8200 . ? O13 C66 1.433(6) . ? O13 H13C 0.8200 . ? C1 C2 1.406(7) . ? C1 C6 1.421(8) . ? C2 C3 1.372(8) . ? C2 H2A 0.9300 . ? C3 C4 1.391(10) . ? C3 H3B 0.9300 . ? C4 C5 1.353(9) . ? C4 H4B 0.9300 . ? C5 C6 1.398(7) . ? C5 H5A 0.9300 . ? C6 C7 1.432(8) . ? C7 H7B 0.9300 . ? C8 C9 1.513(7) . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.448(7) . ? C10 H10A 0.9300 . ? C11 C12 1.408(7) . ? C11 C16 1.415(7) . ? C12 C13 1.374(8) . ? C12 H12A 0.9300 . ? C13 C14 1.377(9) . ? C13 H13A 0.9300 . ? C14 C15 1.380(7) . ? C14 H14A 0.9300 . ? C15 C16 1.402(7) . ? C15 H15A 0.9300 . ? C17 C22 1.408(7) . ? C17 C18 1.412(7) . ? C18 C19 1.367(8) . ? C18 H18A 0.9300 . ? C19 C20 1.397(10) . ? C19 H19A 0.9300 . ? C20 C21 1.363(9) . ? C20 H20A 0.9300 . ? C21 C22 1.417(8) . ? C21 H21A 0.9300 . ? C22 C23 1.421(8) . ? C23 H23A 0.9300 . ? C24 C25 1.437(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.407(8) . ? C26 H26A 0.9300 . ? C27 C28 1.416(7) . ? C27 C32 1.425(7) . ? C28 C29 1.360(8) . ? C28 H28A 0.9300 . ? C29 C30 1.395(8) . ? C29 H29A 0.9300 . ? C30 C31 1.360(7) . ? C30 H30A 0.9300 . ? C31 C32 1.406(7) . ? C31 H31A 0.9300 . ? C33 C34 1.409(7) . ? C33 C38 1.411(7) . ? C34 C35 1.390(7) . ? C34 H34A 0.9300 . ? C35 C36 1.391(8) . ? C35 H35A 0.9300 . ? C36 C37 1.364(8) . ? C36 H36A 0.9300 . ? C37 C38 1.409(7) . ? C37 H37A 0.9300 . ? C38 C39 1.443(7) . ? C39 H39A 0.9300 . ? C40 C41 1.511(8) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.429(7) . ? C42 H42A 0.9300 . ? C43 C44 1.409(7) . ? C43 C48 1.425(7) . ? C44 C45 1.366(8) . ? C44 H44A 0.9300 . ? C45 C46 1.383(9) . ? C45 H45A 0.9300 . ? C46 C47 1.376(8) . ? C46 H46A 0.9300 . ? C47 C48 1.406(7) . ? C47 H47A 0.9300 . ? C49 C50 1.400(7) . ? C49 C54 1.418(7) . ? C50 C51 1.381(7) . ? C50 H50A 0.9300 . ? C51 C52 1.392(8) . ? C51 H51A 0.9300 . ? C52 C53 1.370(7) . ? C52 H52A 0.9300 . ? C53 C54 1.410(7) . ? C53 H53A 0.9300 . ? C54 C55 1.419(7) . ? C55 H55A 0.9300 . ? C56 C57 1.524(7) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.451(7) . ? C58 H58A 0.9300 . ? C59 C60 1.391(8) . ? C59 C64 1.410(8) . ? C60 C61 1.386(8) . ? C60 H60A 0.9300 . ? C61 C62 1.381(9) . ? C61 H61A 0.9300 . ? C62 C63 1.373(9) . ? C62 H62A 0.9300 . ? C63 C64 1.363(8) . ? C63 H63A 0.9300 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O3 86.99(14) . . ? O1 Yb1 O2 144.95(13) . . ? O3 Yb1 O2 85.24(14) . . ? O1 Yb1 O12 75.38(12) . . ? O3 Yb1 O12 89.79(13) . . ? O2 Yb1 O12 70.48(12) . . ? O1 Yb1 N1 74.12(13) . . ? O3 Yb1 N1 98.72(13) . . ? O2 Yb1 N1 140.88(13) . . ? O12 Yb1 N1 147.77(13) . . ? O1 Yb1 N2 136.96(13) . . ? O3 Yb1 N2 78.12(13) . . ? O2 Yb1 N2 74.21(13) . . ? O12 Yb1 N2 143.46(12) . . ? N1 Yb1 N2 68.71(13) . . ? O1 Yb1 O10 122.05(14) . . ? O3 Yb1 O10 147.10(13) . . ? O2 Yb1 O10 78.61(14) . . ? O12 Yb1 O10 110.99(13) . . ? N1 Yb1 O10 77.47(13) . . ? N2 Yb1 O10 70.01(13) . . ? O1 Yb1 O9 79.99(14) . . ? O3 Yb1 O9 161.69(13) . . ? O2 Yb1 O9 98.05(15) . . ? O12 Yb1 O9 74.56(13) . . ? N1 Yb1 O9 90.09(14) . . ? N2 Yb1 O9 120.15(12) . . ? O10 Yb1 O9 50.57(12) . . ? O1 Yb1 N9 102.21(14) . . ? O3 Yb1 N9 170.80(13) . . ? O2 Yb1 N9 87.07(14) . . ? O12 Yb1 N9 92.39(12) . . ? N1 Yb1 N9 84.13(12) . . ? N2 Yb1 N9 94.94(13) . . ? O10 Yb1 N9 25.02(12) . . ? O9 Yb1 N9 25.60(12) . . ? O6 Yb2 O7 95.35(14) . . ? O6 Yb2 O5 147.37(13) . . ? O7 Yb2 O5 82.20(12) . . ? O6 Yb2 O4 92.68(14) . . ? O7 Yb2 O4 169.70(12) . . ? O5 Yb2 O4 87.56(13) . . ? O6 Yb2 O13 74.70(12) . . ? O7 Yb2 O13 92.92(13) . . ? O5 Yb2 O13 72.95(12) . . ? O4 Yb2 O13 82.99(13) . . ? O6 Yb2 N5 137.33(13) . . ? O7 Yb2 N5 98.03(14) . . ? O5 Yb2 N5 74.84(13) . . ? O4 Yb2 N5 80.23(14) . . ? O13 Yb2 N5 144.11(13) . . ? O6 Yb2 N6 72.91(13) . . ? O7 Yb2 N6 84.85(13) . . ? O5 Yb2 N6 138.53(13) . . ? O4 Yb2 N6 103.72(13) . . ? O13 Yb2 N6 147.16(12) . . ? N5 Yb2 N6 68.23(13) . . ? C7 N1 C8 116.0(4) . . ? C7 N1 Yb1 129.7(4) . . ? C8 N1 Yb1 114.2(3) . . ? C10 N2 C9 116.9(4) . . ? C10 N2 Yb1 129.4(3) . . ? C9 N2 Yb1 113.2(3) . . ? C23 N3 C24 125.4(5) . . ? C26 N4 C25 125.2(5) . . ? C39 N5 C40 115.6(4) . . ? C39 N5 Yb2 128.3(3) . . ? C40 N5 Yb2 116.0(3) . . ? C42 N6 C41 116.3(4) . . ? C42 N6 Yb2 130.7(3) . . ? C41 N6 Yb2 112.9(3) . . ? C55 N7 C56 123.5(4) . . ? C58 N8 C57 119.7(4) . . ? O11 N9 O10 120.9(4) . . ? O11 N9 O9 121.9(5) . . ? O10 N9 O9 117.2(4) . . ? O11 N9 Yb1 176.3(4) . . ? O10 N9 Yb1 57.3(2) . . ? O9 N9 Yb1 60.0(2) . . ? O15 N10 O16 120.4(5) . . ? O15 N10 O14 119.3(4) . . ? O16 N10 O14 120.3(5) . . ? C1 O1 Yb1 143.4(3) . . ? C16 O2 Yb1 138.5(3) . . ? C17 O3 Yb1 153.5(3) . . ? C17 O3 H3C 109.5 . . ? Yb1 O3 H3C 87.1 . . ? C32 O4 Yb2 138.3(3) . . ? C32 O4 H4A 109.5 . . ? Yb2 O4 H4A 95.9 . . ? C33 O5 Yb2 138.8(3) . . ? C48 O6 Yb2 145.2(3) . . ? C49 O7 Yb2 144.4(3) . . ? C49 O7 H7C 109.5 . . ? Yb2 O7 H7C 92.8 . . ? C64 O8 H8E 109.5 . . ? N9 O9 Yb1 94.4(3) . . ? N9 O10 Yb1 97.7(3) . . ? C65 O12 Yb1 131.6(3) . . ? C65 O12 H12B 109.5 . . ? Yb1 O12 H12B 99.9 . . ? C66 O13 Yb2 126.7(3) . . ? C66 O13 H13C 109.5 . . ? Yb2 O13 H13C 102.4 . . ? O1 C1 C2 120.7(5) . . ? O1 C1 C6 122.2(5) . . ? C2 C1 C6 117.0(5) . . ? C3 C2 C1 121.2(6) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 120.9(6) . . ? C2 C3 H3B 119.5 . . ? C4 C3 H3B 119.5 . . ? C5 C4 C3 119.5(6) . . ? C5 C4 H4B 120.2 . . ? C3 C4 H4B 120.2 . . ? C4 C5 C6 121.2(6) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C5 C6 C1 120.1(5) . . ? C5 C6 C7 117.1(5) . . ? C1 C6 C7 122.8(5) . . ? N1 C7 C6 127.3(5) . . ? N1 C7 H7B 116.3 . . ? C6 C7 H7B 116.3 . . ? N1 C8 C9 106.6(4) . . ? N1 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? N1 C8 H8C 110.4 . . ? C9 C8 H8C 110.4 . . ? H8B C8 H8C 108.6 . . ? N2 C9 C8 107.7(4) . . ? N2 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? N2 C9 H9B 110.2 . . ? C8 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? N2 C10 C11 127.0(5) . . ? N2 C10 H10A 116.5 . . ? C11 C10 H10A 116.5 . . ? C12 C11 C16 119.1(5) . . ? C12 C11 C10 117.0(5) . . ? C16 C11 C10 123.8(4) . . ? C13 C12 C11 121.7(5) . . ? C13 C12 H12A 119.2 . . ? C11 C12 H12A 119.2 . . ? C12 C13 C14 119.2(5) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C13 C14 C15 120.6(5) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C14 C15 C16 121.7(5) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.2 . . ? O2 C16 C15 120.3(5) . . ? O2 C16 C11 122.0(4) . . ? C15 C16 C11 117.6(4) . . ? O3 C17 C22 120.6(4) . . ? O3 C17 C18 121.8(5) . . ? C22 C17 C18 117.6(5) . . ? C19 C18 C17 120.5(6) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C18 C19 C20 121.8(6) . . ? C18 C19 H19A 119.1 . . ? C20 C19 H19A 119.1 . . ? C21 C20 C19 119.3(6) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C20 C21 C22 120.1(6) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C17 C22 C21 120.6(5) . . ? C17 C22 C23 121.2(5) . . ? C21 C22 C23 117.9(5) . . ? N3 C23 C22 124.4(6) . . ? N3 C23 H23A 117.8 . . ? C22 C23 H23A 117.8 . . ? C25 C24 N3 104.4(6) . . ? C25 C24 H24A 110.9 . . ? N3 C24 H24A 110.9 . . ? C25 C24 H24B 110.9 . . ? N3 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? C24 C25 N4 104.3(6) . . ? C24 C25 H25A 110.9 . . ? N4 C25 H25A 110.9 . . ? C24 C25 H25B 110.9 . . ? N4 C25 H25B 110.9 . . ? H25A C25 H25B 108.9 . . ? N4 C26 C27 126.4(5) . . ? N4 C26 H26A 116.8 . . ? C27 C26 H26A 116.8 . . ? C26 C27 C28 119.6(5) . . ? C26 C27 C32 120.8(5) . . ? C28 C27 C32 119.5(5) . . ? C29 C28 C27 121.1(5) . . ? C29 C28 H28A 119.5 . . ? C27 C28 H28A 119.5 . . ? C28 C29 C30 119.3(5) . . ? C28 C29 H29A 120.4 . . ? C30 C29 H29A 120.4 . . ? C31 C30 C29 121.3(5) . . ? C31 C30 H30A 119.3 . . ? C29 C30 H30A 119.3 . . ? C30 C31 C32 121.5(5) . . ? C30 C31 H31A 119.2 . . ? C32 C31 H31A 119.2 . . ? O4 C32 C31 122.3(5) . . ? O4 C32 C27 120.4(4) . . ? C31 C32 C27 117.3(4) . . ? O5 C33 C34 119.4(5) . . ? O5 C33 C38 122.1(5) . . ? C34 C33 C38 118.5(5) . . ? C35 C34 C33 120.7(5) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C36 C35 C34 120.2(5) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C37 C36 C35 120.0(5) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 121.4(5) . . ? C36 C37 H37A 119.3 . . ? C38 C37 H37A 119.3 . . ? C37 C38 C33 119.2(5) . . ? C37 C38 C39 117.0(5) . . ? C33 C38 C39 123.8(5) . . ? N5 C39 C38 127.7(5) . . ? N5 C39 H39A 116.1 . . ? C38 C39 H39A 116.1 . . ? N5 C40 C41 108.1(4) . . ? N5 C40 H40A 110.1 . . ? C41 C40 H40A 110.1 . . ? N5 C40 H40B 110.1 . . ? C41 C40 H40B 110.1 . . ? H40A C40 H40B 108.4 . . ? N6 C41 C40 107.5(4) . . ? N6 C41 H41A 110.2 . . ? C40 C41 H41A 110.2 . . ? N6 C41 H41B 110.2 . . ? C40 C41 H41B 110.2 . . ? H41A C41 H41B 108.5 . . ? N6 C42 C43 126.8(5) . . ? N6 C42 H42A 116.6 . . ? C43 C42 H42A 116.6 . . ? C44 C43 C48 119.3(5) . . ? C44 C43 C42 118.1(5) . . ? C48 C43 C42 122.6(4) . . ? C45 C44 C43 121.3(5) . . ? C45 C44 H44A 119.3 . . ? C43 C44 H44A 119.3 . . ? C44 C45 C46 119.4(5) . . ? C44 C45 H45A 120.3 . . ? C46 C45 H45A 120.3 . . ? C47 C46 C45 121.2(5) . . ? C47 C46 H46A 119.4 . . ? C45 C46 H46A 119.4 . . ? C46 C47 C48 121.1(5) . . ? C46 C47 H47A 119.5 . . ? C48 C47 H47A 119.5 . . ? O6 C48 C47 120.7(5) . . ? O6 C48 C43 121.7(4) . . ? C47 C48 C43 117.6(5) . . ? O7 C49 C50 120.6(4) . . ? O7 C49 C54 120.4(4) . . ? C50 C49 C54 118.9(4) . . ? C51 C50 C49 119.7(5) . . ? C51 C50 H50A 120.1 . . ? C49 C50 H50A 120.1 . . ? C50 C51 C52 121.8(5) . . ? C50 C51 H51A 119.1 . . ? C52 C51 H51A 119.1 . . ? C53 C52 C51 119.2(5) . . ? C53 C52 H52A 120.4 . . ? C51 C52 H52A 120.4 . . ? C52 C53 C54 120.7(5) . . ? C52 C53 H53A 119.6 . . ? C54 C53 H53A 119.6 . . ? C53 C54 C55 117.9(4) . . ? C53 C54 C49 119.5(4) . . ? C55 C54 C49 122.6(4) . . ? N7 C55 C54 123.7(5) . . ? N7 C55 H55A 118.2 . . ? C54 C55 H55A 118.2 . . ? N7 C56 C57 110.5(4) . . ? N7 C56 H56A 109.5 . . ? C57 C56 H56A 109.5 . . ? N7 C56 H56B 109.5 . . ? C57 C56 H56B 109.5 . . ? H56A C56 H56B 108.1 . . ? N8 C57 C56 108.9(4) . . ? N8 C57 H57A 109.9 . . ? C56 C57 H57A 109.9 . . ? N8 C57 H57B 109.9 . . ? C56 C57 H57B 109.9 . . ? H57A C57 H57B 108.3 . . ? N8 C58 C59 121.0(5) . . ? N8 C58 H58A 119.5 . . ? C59 C58 H58A 119.5 . . ? C60 C59 C64 119.0(5) . . ? C60 C59 C58 120.4(5) . . ? C64 C59 C58 120.5(5) . . ? C61 C60 C59 120.5(6) . . ? C61 C60 H60A 119.7 . . ? C59 C60 H60A 119.7 . . ? C62 C61 C60 119.1(6) . . ? C62 C61 H61A 120.4 . . ? C60 C61 H61A 120.4 . . ? C63 C62 C61 120.7(6) . . ? C63 C62 H62A 119.7 . . ? C61 C62 H62A 119.7 . . ? C64 C63 C62 121.0(6) . . ? C64 C63 H63A 119.5 . . ? C62 C63 H63A 119.5 . . ? O8 C64 C63 119.4(5) . . ? O8 C64 C59 121.0(5) . . ? C63 C64 C59 119.5(6) . . ? O12 C65 H65A 109.5 . . ? O12 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? O12 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? O13 C66 H66A 109.5 . . ? O13 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O13 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.292 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.119 _database_code_depnum_ccdc_archive 'CCDC 950240'