# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2034 data_xf142 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H53 N4 O7 Yb' _chemical_formula_weight 1055.05 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)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.646(1) _cell_length_b 23.715(3) _cell_length_c 17.944(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.2(1) _cell_angle_gamma 90.00 _cell_volume 5239.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used '221 from 4 still frames' _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2148 _exptl_absorpt_coefficient_mu 1.838 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_T_max 1.092 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV/90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS IIc' _diffrn_measurement_method ; Data was collected to 0.82\%A with 88% completeness by taking 41 oscillation photos in the range of 0 - 164\%, \D\f = 4\%, 8 min. per frame. Crystal to detector distance is 78.098 mm, background level -80. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14941 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0927 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.53 _reflns_number_total 8594 _reflns_number_gt 7715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BioteX 1.0 (MSC, 1995)' _computing_cell_refinement 'BioteX 1.0 (MSC, 1995)' _computing_data_reduction 'BioteX 1.0 (MSC, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Siemens, 1990)' _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^)+(0.0908P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0034(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8594 _refine_ls_number_parameters 633 _refine_ls_number_restraints 335 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.061 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.418194(16) 0.378594(8) 0.489445(14) 0.05398(9) Uani 1 1 d . . . N1 N 0.2262(3) 0.37705(14) 0.4548(3) 0.0541(11) Uani 1 1 d D . . N2 N 0.3718(3) 0.28529(16) 0.5179(2) 0.0523(10) Uani 1 1 d D . . N3 N 0.5227(3) 0.32061(17) 0.4271(3) 0.0583(11) Uani 1 1 d D . . N4 N 0.3754(3) 0.40998(16) 0.3614(3) 0.0553(11) Uani 1 1 d D . . C1 C 0.1640(4) 0.4190(2) 0.4127(3) 0.0591(13) Uani 1 1 d D . . C2 C 0.0587(4) 0.4198(2) 0.4282(4) 0.0739(17) Uani 1 1 d D . . H2 H 0.0025 0.4443 0.4069 0.089 Uiso 1 1 calc R . . C3 C 0.0549(5) 0.3776(2) 0.4807(5) 0.0741(18) Uani 1 1 d D . . H3 H -0.0028 0.3688 0.5027 0.089 Uiso 1 1 calc R . . C4 C 0.1606(4) 0.3499(2) 0.4945(3) 0.0590(13) Uani 1 1 d D . . C5 C 0.1883(4) 0.3016(2) 0.5400(3) 0.0605(14) Uani 1 1 d D . . C6 C 0.2851(4) 0.2711(2) 0.5463(3) 0.0618(14) Uani 1 1 d D . . C7 C 0.3034(5) 0.2166(2) 0.5835(4) 0.0744(17) Uani 1 1 d D . . H7 H 0.2563 0.1979 0.6080 0.089 Uiso 1 1 calc R . . C8 C 0.4001(5) 0.1981(2) 0.5762(4) 0.0703(16) Uani 1 1 d D . . H8 H 0.4331 0.1643 0.5948 0.084 Uiso 1 1 calc R . . C9 C 0.4441(4) 0.2408(2) 0.5336(4) 0.0609(14) Uani 1 1 d D . . C10 C 0.5401(4) 0.2349(2) 0.5082(4) 0.0634(15) Uani 1 1 d D . . C11 C 0.5738(4) 0.2711(2) 0.4576(3) 0.0611(14) Uani 1 1 d D . . C12 C 0.6662(5) 0.2621(2) 0.4231(4) 0.0734(17) Uani 1 1 d D . . H12 H 0.7153 0.2324 0.4340 0.088 Uiso 1 1 calc R . . C13 C 0.6688(4) 0.3036(2) 0.3731(4) 0.0708(16) Uani 1 1 d D . . H13 H 0.7188 0.3079 0.3428 0.085 Uiso 1 1 calc R . . C14 C 0.5786(4) 0.3403(2) 0.3755(3) 0.0620(14) Uani 1 1 d D . . C15 C 0.5493(4) 0.3872(2) 0.3277(4) 0.0583(14) Uani 1 1 d D . . C16 C 0.4543(4) 0.4188(2) 0.3203(3) 0.0565(13) Uani 1 1 d D . . C17 C 0.4239(4) 0.4657(2) 0.2682(3) 0.0645(15) Uani 1 1 d D . . H17 H 0.4636 0.4803 0.2351 0.077 Uiso 1 1 calc R . . C18 C 0.3253(4) 0.4842(2) 0.2773(3) 0.0616(14) Uani 1 1 d D . . H18 H 0.2857 0.5143 0.2519 0.074 Uiso 1 1 calc R . . C19 C 0.2942(4) 0.4486(2) 0.3335(3) 0.0598(14) Uani 1 1 d D . . C20 C 0.1957(4) 0.4526(2) 0.3579(3) 0.0592(14) Uani 1 1 d D . . C21 C 0.1052(4) 0.2795(2) 0.5790(3) 0.0677(16) Uani 1 1 d D . . C22 C 0.1209(5) 0.2830(2) 0.6574(3) 0.0723(16) Uani 1 1 d D . . H22 H 0.1844 0.2993 0.6856 0.087 Uiso 1 1 calc R . . C23 C 0.0440(5) 0.2628(3) 0.6956(4) 0.084(2) Uani 1 1 d D . . H23 H 0.0559 0.2661 0.7485 0.101 Uiso 1 1 calc R . . C24 C -0.0482(5) 0.2385(3) 0.6549(5) 0.102(3) Uani 1 1 d D . . H24 H -0.0997 0.2248 0.6799 0.123 Uiso 1 1 calc R . . C25 C -0.0650(5) 0.2343(4) 0.5785(5) 0.113(3) Uani 1 1 d D . . H25 H -0.1293 0.2182 0.5511 0.136 Uiso 1 1 calc R . . C26 C 0.0110(5) 0.2533(3) 0.5390(4) 0.100(2) Uani 1 1 d D . . H26 H -0.0013 0.2485 0.4863 0.120 Uiso 1 1 calc R . . C27 C 0.6067(4) 0.1826(2) 0.5329(3) 0.0629(14) Uani 1 1 d D . . C28 C 0.6120(6) 0.1392(3) 0.4856(4) 0.093(2) Uani 1 1 d D . . H28 H 0.5721 0.1405 0.4352 0.112 Uiso 1 1 calc R . . C29 C 0.6766(7) 0.0919(3) 0.5113(5) 0.121(3) Uani 1 1 d D . . H29 H 0.6823 0.0631 0.4774 0.145 Uiso 1 1 calc R . . C30 C 0.7306(6) 0.0883(3) 0.5853(5) 0.105(3) Uani 1 1 d D . . H30 H 0.7698 0.0558 0.6027 0.125 Uiso 1 1 calc R . . C31 C 0.7285(6) 0.1310(2) 0.6342(4) 0.087(2) Uani 1 1 d D . . H31 H 0.7678 0.1287 0.6847 0.105 Uiso 1 1 calc R . . C32 C 0.6664(5) 0.1790(2) 0.6082(4) 0.0767(18) Uani 1 1 d D . . H32 H 0.6650 0.2087 0.6417 0.092 Uiso 1 1 calc R . . C33 C 0.6247(4) 0.4029(2) 0.2770(3) 0.0647(14) Uani 1 1 d D . . C34 C 0.5954(5) 0.3959(3) 0.1988(4) 0.0790(18) Uani 1 1 d D . . H34 H 0.5268 0.3820 0.1760 0.095 Uiso 1 1 calc R . . C35 C 0.6678(6) 0.4094(3) 0.1538(4) 0.095(2) Uani 1 1 d D . . H35 H 0.6474 0.4044 0.1010 0.114 Uiso 1 1 calc R . . C36 C 0.7681(6) 0.4298(4) 0.1863(5) 0.107(3) Uani 1 1 d D . . H36 H 0.8165 0.4383 0.1559 0.128 Uiso 1 1 calc R . . C37 C 0.7976(5) 0.4377(4) 0.2622(5) 0.107(3) Uani 1 1 d D . . H37 H 0.8655 0.4527 0.2839 0.128 Uiso 1 1 calc R . . C38 C 0.7283(4) 0.4238(3) 0.3083(4) 0.084(2) Uani 1 1 d D . . H38 H 0.7509 0.4285 0.3610 0.101 Uiso 1 1 calc R . . C39 C 0.1177(4) 0.4971(2) 0.3194(3) 0.0625(14) Uani 1 1 d D . . C40 C 0.0898(5) 0.5419(2) 0.3609(4) 0.086(2) Uani 1 1 d D . . H40 H 0.1194 0.5443 0.4133 0.103 Uiso 1 1 calc R . . C41 C 0.0179(6) 0.5833(3) 0.3248(5) 0.102(2) Uani 1 1 d D . . H41 H 0.0005 0.6133 0.3533 0.123 Uiso 1 1 calc R . . C42 C -0.0266(6) 0.5805(3) 0.2492(5) 0.108(3) Uani 1 1 d D . . H42 H -0.0750 0.6083 0.2259 0.130 Uiso 1 1 calc R . . C43 C -0.0013(6) 0.5374(3) 0.2070(5) 0.105(3) Uani 1 1 d D . . H43 H -0.0313 0.5361 0.1547 0.127 Uiso 1 1 calc R . . C44 C 0.0708(4) 0.4943(3) 0.2421(4) 0.0801(19) Uani 1 1 d D . . H44 H 0.0865 0.4642 0.2132 0.096 Uiso 1 1 calc R . . C45 C 0.4442(4) 0.5103(2) 0.5046(3) 0.0584(14) Uani 1 1 d . . . O1 O 0.3756(3) 0.47327(14) 0.5092(2) 0.0620(10) Uani 1 1 d . . . O2 O 0.4323(3) 0.56230(14) 0.5092(2) 0.0649(10) Uani 1 1 d . . . C46 C 0.2998(6) 0.4282(3) 0.6383(4) 0.094(2) Uani 1 1 d DU . . H46A H 0.2512 0.4415 0.5926 0.140 Uiso 1 1 calc R . . H46B H 0.3388 0.4595 0.6655 0.140 Uiso 1 1 calc R . . H46C H 0.2589 0.4097 0.6702 0.140 Uiso 1 1 calc R . . O3 O 0.3740(4) 0.38969(17) 0.6188(3) 0.0759(12) Uani 1 1 d DU . . C47 C 0.4488(7) 0.3686(5) 0.6804(5) 0.130(3) Uani 1 1 d DU . . H47A H 0.4572 0.3963 0.7211 0.156 Uiso 1 1 calc R . . H47B H 0.4171 0.3353 0.6979 0.156 Uiso 1 1 calc R . . C48 C 0.5482(7) 0.3547(5) 0.6732(5) 0.147(4) Uani 1 1 d DU . . H48A H 0.5645 0.3175 0.6954 0.177 Uiso 1 1 calc R . . H48B H 0.5990 0.3808 0.7041 0.177 Uiso 1 1 calc R . . O4 O 0.5693(3) 0.35376(18) 0.6007(3) 0.0784(12) Uani 1 1 d DU . . C49 C 0.6819(5) 0.3558(3) 0.6032(5) 0.092(2) Uani 1 1 d DU . . H49A H 0.6928 0.3553 0.5520 0.137 Uiso 1 1 calc R . . H49B H 0.7171 0.3236 0.6307 0.137 Uiso 1 1 calc R . . H49C H 0.7123 0.3897 0.6285 0.137 Uiso 1 1 calc R . . C50 C 0.8393(6) 0.2920(5) 0.8148(6) 0.140(4) Uani 1 1 d DU . . H50A H 0.8549 0.3224 0.7836 0.210 Uiso 1 1 calc R . . H50B H 0.8902 0.2619 0.8149 0.210 Uiso 1 1 calc R . . H50C H 0.8452 0.3051 0.8661 0.210 Uiso 1 1 calc R . . O5 O 0.7338(4) 0.2722(2) 0.7850(3) 0.1086(17) Uani 1 1 d DU . . C51 C 0.7032(6) 0.2289(3) 0.8274(5) 0.116(3) Uani 1 1 d DU . . H51A H 0.7198 0.2396 0.8810 0.139 Uiso 1 1 calc R . . H51B H 0.7450 0.1954 0.8223 0.139 Uiso 1 1 calc R . . C52 C 0.5889(7) 0.2160(4) 0.8033(6) 0.121(3) Uani 1 1 d DU . . H52A H 0.5704 0.2109 0.7482 0.145 Uiso 1 1 calc R . . H52B H 0.5749 0.1806 0.8265 0.145 Uiso 1 1 calc R . . O6 O 0.5236(4) 0.2566(3) 0.8223(4) 0.129(2) Uani 1 1 d DU . . C53 C 0.4136(7) 0.2419(5) 0.8097(7) 0.155(4) Uani 1 1 d DU . . H53A H 0.3738 0.2722 0.8260 0.233 Uiso 1 1 calc R . . H53B H 0.4062 0.2085 0.8383 0.233 Uiso 1 1 calc R . . H53C H 0.3853 0.2349 0.7562 0.233 Uiso 1 1 calc R . . C54 C 1.1331(13) -0.0720(17) 0.6267(16) 0.244(15) Uani 0.50 1 d PDU . . H54A H 1.1738 -0.0500 0.6684 0.366 Uiso 0.50 1 calc PR . . H54B H 1.1416 -0.0564 0.5791 0.366 Uiso 0.50 1 calc PR . . H54C H 1.1593 -0.1101 0.6313 0.366 Uiso 0.50 1 calc PR . . O7 O 1.0232(12) -0.0714(8) 0.6288(11) 0.206(7) Uani 0.50 1 d PDU . . C55 C 0.9563(13) -0.1035(10) 0.5763(13) 0.181(8) Uani 0.50 1 d PDU . . H55A H 0.9875 -0.1408 0.5766 0.217 Uiso 0.50 1 calc PR . . H55B H 0.9517 -0.0873 0.5260 0.217 Uiso 0.50 1 calc PR . . C56 C 0.8507(12) -0.1085(7) 0.5884(12) 0.148(6) Uani 0.50 1 d PDU . . H56A H 0.8191 -0.1439 0.5672 0.177 Uiso 0.50 1 calc PR . . H56B H 0.8541 -0.1088 0.6430 0.177 Uiso 0.50 1 calc PR . . O8 O 0.7873(11) -0.0655(6) 0.5555(10) 0.168(5) Uani 0.50 1 d PDU . . C57 C 0.6774(13) -0.0674(8) 0.5525(16) 0.179(9) Uani 0.50 1 d PDU . . H57A H 0.6438 -0.0333 0.5295 0.268 Uiso 0.50 1 calc PR . . H57B H 0.6661 -0.0708 0.6034 0.268 Uiso 0.50 1 calc PR . . H57C H 0.6458 -0.0992 0.5225 0.268 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.05349(14) 0.04360(14) 0.06369(17) 0.00139(9) 0.01097(11) -0.00137(8) N1 0.0430(19) 0.048(2) 0.070(3) 0.0048(18) 0.0094(19) -0.0007(15) N2 0.059(2) 0.0425(19) 0.055(2) 0.0042(18) 0.0102(19) -0.0087(17) N3 0.057(2) 0.047(2) 0.071(3) 0.002(2) 0.015(2) 0.0004(17) N4 0.056(2) 0.047(2) 0.061(3) 0.0028(19) 0.0109(19) 0.0006(17) C1 0.056(3) 0.056(3) 0.067(3) 0.007(3) 0.017(2) -0.001(2) C2 0.057(3) 0.073(3) 0.091(5) 0.021(3) 0.014(3) 0.015(3) C3 0.063(3) 0.080(4) 0.084(4) 0.018(3) 0.026(3) 0.004(2) C4 0.051(2) 0.054(3) 0.070(4) 0.004(3) 0.010(2) -0.001(2) C5 0.061(3) 0.054(3) 0.064(3) 0.004(3) 0.010(2) -0.009(2) C6 0.061(3) 0.049(3) 0.069(4) 0.003(2) 0.002(3) -0.004(2) C7 0.075(3) 0.054(3) 0.092(5) 0.012(3) 0.015(3) -0.011(3) C8 0.074(3) 0.052(3) 0.085(4) 0.008(3) 0.019(3) 0.003(3) C9 0.064(3) 0.044(2) 0.072(4) 0.002(2) 0.010(3) 0.002(2) C10 0.060(3) 0.049(3) 0.078(4) 0.007(3) 0.008(3) 0.005(2) C11 0.061(3) 0.048(3) 0.071(4) -0.005(3) 0.007(3) 0.006(2) C12 0.073(3) 0.070(3) 0.080(4) 0.012(3) 0.024(3) 0.017(3) C13 0.061(3) 0.075(4) 0.082(4) 0.007(3) 0.027(3) 0.009(3) C14 0.055(3) 0.065(3) 0.068(4) 0.003(3) 0.017(2) 0.002(2) C15 0.058(3) 0.052(3) 0.066(4) -0.001(2) 0.018(3) 0.001(2) C16 0.057(3) 0.051(3) 0.063(3) -0.002(2) 0.016(2) -0.008(2) C17 0.070(3) 0.056(3) 0.069(4) 0.007(3) 0.020(3) -0.008(2) C18 0.060(3) 0.057(3) 0.070(4) 0.008(3) 0.019(2) 0.001(2) C19 0.058(3) 0.048(3) 0.070(4) 0.005(2) 0.008(2) 0.001(2) C20 0.055(3) 0.054(3) 0.066(4) 0.005(3) 0.009(2) 0.002(2) C21 0.061(3) 0.057(3) 0.083(4) 0.013(3) 0.013(3) -0.003(2) C22 0.074(3) 0.064(3) 0.078(4) 0.008(3) 0.017(3) 0.003(3) C23 0.089(4) 0.076(4) 0.092(5) 0.018(4) 0.030(4) 0.005(3) C24 0.082(4) 0.102(5) 0.132(7) 0.035(5) 0.045(5) -0.002(4) C25 0.078(4) 0.148(7) 0.109(7) 0.026(6) 0.011(4) -0.043(4) C26 0.087(4) 0.131(6) 0.077(5) 0.016(4) 0.010(4) -0.038(4) C27 0.062(3) 0.055(3) 0.072(4) 0.017(3) 0.017(3) 0.008(2) C28 0.117(5) 0.075(4) 0.078(5) 0.000(4) 0.006(4) 0.028(4) C29 0.154(7) 0.071(5) 0.127(8) -0.009(5) 0.010(6) 0.030(5) C30 0.109(5) 0.068(4) 0.130(7) 0.013(4) 0.013(5) 0.031(4) C31 0.090(4) 0.068(4) 0.095(5) 0.027(4) 0.003(4) 0.009(3) C32 0.079(4) 0.064(3) 0.084(5) 0.013(3) 0.012(3) 0.001(3) C33 0.062(3) 0.061(3) 0.073(4) 0.002(3) 0.020(3) 0.010(2) C34 0.093(4) 0.072(3) 0.075(4) 0.001(3) 0.025(4) 0.002(3) C35 0.112(5) 0.100(5) 0.082(5) 0.005(4) 0.040(4) 0.012(4) C36 0.091(4) 0.122(6) 0.124(7) 0.019(6) 0.058(5) 0.007(5) C37 0.064(4) 0.140(7) 0.120(7) 0.007(6) 0.029(4) -0.015(4) C38 0.063(3) 0.097(4) 0.095(5) 0.009(4) 0.022(3) -0.011(3) C39 0.056(3) 0.057(3) 0.076(4) 0.015(3) 0.019(3) 0.004(2) C40 0.091(4) 0.076(4) 0.092(5) 0.010(4) 0.023(4) 0.020(3) C41 0.113(5) 0.079(4) 0.124(7) 0.022(4) 0.046(5) 0.038(4) C42 0.096(5) 0.096(5) 0.136(8) 0.042(5) 0.034(5) 0.037(4) C43 0.088(4) 0.114(6) 0.104(6) 0.048(5) 0.000(4) 0.011(4) C44 0.069(3) 0.071(4) 0.096(5) 0.022(4) 0.010(3) 0.007(3) C45 0.061(3) 0.041(2) 0.070(4) 0.001(2) 0.009(3) -0.004(2) O1 0.0637(19) 0.0465(18) 0.078(3) -0.0051(18) 0.0211(18) -0.0033(16) O2 0.066(2) 0.0455(19) 0.083(3) 0.0019(18) 0.0178(19) -0.0028(15) C46 0.111(5) 0.086(4) 0.095(5) -0.013(4) 0.047(4) 0.002(4) O3 0.096(3) 0.068(2) 0.063(3) 0.002(2) 0.017(2) 0.006(2) C47 0.117(6) 0.200(10) 0.069(5) 0.018(6) 0.016(4) 0.026(6) C48 0.145(6) 0.216(10) 0.080(5) 0.029(7) 0.023(5) 0.083(7) O4 0.072(2) 0.074(2) 0.081(3) 0.012(2) 0.000(2) -0.010(2) C49 0.074(3) 0.087(4) 0.103(6) 0.012(4) -0.001(3) -0.008(3) C50 0.080(4) 0.207(10) 0.130(8) 0.034(8) 0.017(5) 0.010(5) O5 0.090(3) 0.131(4) 0.104(4) 0.041(3) 0.020(3) 0.010(3) C51 0.115(4) 0.118(6) 0.117(7) 0.049(5) 0.028(5) 0.025(4) C52 0.128(5) 0.115(6) 0.127(7) 0.031(5) 0.043(5) -0.005(4) O6 0.093(3) 0.140(5) 0.153(6) 0.018(4) 0.027(4) -0.001(3) C53 0.100(5) 0.228(12) 0.138(9) 0.012(9) 0.026(6) -0.028(6) C54 0.199(11) 0.39(4) 0.14(2) 0.01(3) 0.025(17) -0.04(2) O7 0.219(10) 0.214(15) 0.201(16) -0.045(12) 0.081(12) -0.092(12) C55 0.211(9) 0.196(17) 0.131(17) -0.024(14) 0.029(13) -0.018(11) C56 0.217(9) 0.133(11) 0.090(12) 0.004(11) 0.027(12) -0.056(9) O8 0.215(9) 0.109(9) 0.193(14) -0.007(9) 0.077(11) -0.039(8) C57 0.218(11) 0.087(11) 0.25(3) -0.040(14) 0.084(19) -0.050(11) _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 O2 2.350(3) 3_666 ? Yb1 O1 2.355(3) . ? Yb1 N4 2.357(4) . ? Yb1 N3 2.359(4) . ? Yb1 N1 2.365(4) . ? Yb1 N2 2.374(4) . ? Yb1 O4 2.499(4) . ? Yb1 O3 2.522(5) . ? N1 C4 1.372(7) . ? N1 C1 1.381(6) . ? N2 C6 1.353(7) . ? N2 C9 1.381(6) . ? N3 C14 1.369(7) . ? N3 C11 1.392(6) . ? N4 C19 1.382(6) . ? N4 C16 1.385(7) . ? C1 C20 1.394(8) . ? C1 C2 1.421(8) . ? C2 C3 1.383(9) . ? C3 C4 1.459(8) . ? C4 C5 1.404(7) . ? C5 C6 1.403(7) . ? C5 C21 1.484(8) . ? C6 C7 1.448(7) . ? C7 C8 1.333(8) . ? C8 C9 1.454(8) . ? C9 C10 1.398(8) . ? C10 C11 1.385(8) . ? C10 C27 1.507(7) . ? C11 C12 1.458(9) . ? C12 C13 1.337(8) . ? C13 C14 1.442(7) . ? C14 C15 1.401(7) . ? C15 C16 1.396(7) . ? C15 C33 1.507(8) . ? C16 C17 1.446(7) . ? C17 C18 1.365(8) . ? C18 C19 1.438(8) . ? C19 C20 1.414(7) . ? C20 C39 1.501(7) . ? C21 C22 1.378(7) . ? C21 C26 1.389(7) . ? C22 C23 1.396(8) . ? C23 C24 1.355(8) . ? C24 C25 1.343(9) . ? C25 C26 1.393(8) . ? C27 C28 1.346(8) . ? C27 C32 1.393(7) . ? C28 C29 1.401(8) . ? C29 C30 1.350(9) . ? C30 C31 1.343(8) . ? C31 C32 1.401(7) . ? C33 C34 1.377(7) . ? C33 C38 1.394(7) . ? C34 C35 1.390(8) . ? C35 C36 1.360(8) . ? C36 C37 1.340(9) . ? C37 C38 1.374(8) . ? C39 C44 1.379(7) . ? C39 C40 1.389(7) . ? C40 C41 1.393(8) . ? C41 C42 1.347(9) . ? C42 C43 1.353(9) . ? C43 C44 1.419(7) . ? C45 O2 1.248(6) . ? C45 O1 1.250(6) . ? C45 C45 1.537(11) 3_666 ? C45 Yb1 3.147(5) 3_666 ? O2 Yb1 2.350(3) 3_666 ? C46 O3 1.409(7) . ? O3 C47 1.375(8) . ? C47 C48 1.335(10) . ? C48 O4 1.385(8) . ? O4 C49 1.415(7) . ? C50 O5 1.399(8) . ? O5 C51 1.386(8) . ? C51 C52 1.443(10) . ? C52 O6 1.362(9) . ? O6 C53 1.402(9) . ? C54 O7 1.399(14) . ? O7 C55 1.349(14) . ? C55 C56 1.406(16) . ? C56 O8 1.347(13) . ? O8 C57 1.379(13) . ? 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 O2 Yb1 O1 68.95(13) 3_666 . ? O2 Yb1 N4 80.00(14) 3_666 . ? O1 Yb1 N4 80.58(14) . . ? O2 Yb1 N3 79.38(14) 3_666 . ? O1 Yb1 N3 143.08(14) . . ? N4 Yb1 N3 75.57(15) . . ? O2 Yb1 N1 141.94(12) 3_666 . ? O1 Yb1 N1 78.35(12) . . ? N4 Yb1 N1 75.83(16) . . ? N3 Yb1 N1 121.27(15) . . ? O2 Yb1 N2 142.33(13) 3_666 . ? O1 Yb1 N2 141.27(16) . . ? N4 Yb1 N2 119.40(14) . . ? N3 Yb1 N2 75.60(15) . . ? N1 Yb1 N2 75.70(13) . . ? O2 Yb1 O4 70.47(13) 3_666 . ? O1 Yb1 O4 105.29(13) . . ? N4 Yb1 O4 144.75(15) . . ? N3 Yb1 O4 80.35(15) . . ? N1 Yb1 O4 139.32(16) . . ? N2 Yb1 O4 77.87(13) . . ? O2 Yb1 O3 106.00(14) 3_666 . ? O1 Yb1 O3 69.84(14) . . ? N4 Yb1 O3 144.49(14) . . ? N3 Yb1 O3 139.74(14) . . ? N1 Yb1 O3 79.25(16) . . ? N2 Yb1 O3 77.40(14) . . ? O4 Yb1 O3 65.11(15) . . ? C4 N1 C1 106.6(4) . . ? C4 N1 Yb1 125.2(3) . . ? C1 N1 Yb1 123.7(3) . . ? C6 N2 C9 106.8(4) . . ? C6 N2 Yb1 125.0(3) . . ? C9 N2 Yb1 124.8(3) . . ? C14 N3 C11 106.8(4) . . ? C14 N3 Yb1 123.6(3) . . ? C11 N3 Yb1 124.4(4) . . ? C19 N4 C16 105.8(4) . . ? C19 N4 Yb1 123.3(4) . . ? C16 N4 Yb1 122.3(3) . . ? N1 C1 C20 125.3(5) . . ? N1 C1 C2 110.2(5) . . ? C20 C1 C2 124.3(5) . . ? C3 C2 C1 107.6(5) . . ? C2 C3 C4 105.6(5) . . ? N1 C4 C5 125.8(5) . . ? N1 C4 C3 109.8(5) . . ? C5 C4 C3 124.4(5) . . ? C6 C5 C4 124.4(5) . . ? C6 C5 C21 118.6(4) . . ? C4 C5 C21 116.9(4) . . ? N2 C6 C5 127.5(5) . . ? N2 C6 C7 109.7(5) . . ? C5 C6 C7 122.8(5) . . ? C8 C7 C6 107.6(5) . . ? C7 C8 C9 107.0(5) . . ? N2 C9 C10 126.4(5) . . ? N2 C9 C8 108.9(5) . . ? C10 C9 C8 124.5(5) . . ? C11 C10 C9 124.8(5) . . ? C11 C10 C27 117.8(5) . . ? C9 C10 C27 117.2(5) . . ? C10 C11 N3 126.6(5) . . ? C10 C11 C12 125.8(5) . . ? N3 C11 C12 107.5(5) . . ? C13 C12 C11 108.8(5) . . ? C12 C13 C14 106.5(6) . . ? N3 C14 C15 125.4(5) . . ? N3 C14 C13 110.3(5) . . ? C15 C14 C13 124.2(5) . . ? C16 C15 C14 125.9(5) . . ? C16 C15 C33 117.3(5) . . ? C14 C15 C33 116.7(4) . . ? N4 C16 C15 125.2(5) . . ? N4 C16 C17 110.0(4) . . ? C15 C16 C17 124.8(5) . . ? C18 C17 C16 106.6(5) . . ? C17 C18 C19 107.3(5) . . ? N4 C19 C20 124.5(5) . . ? N4 C19 C18 110.1(5) . . ? C20 C19 C18 125.4(4) . . ? C1 C20 C19 126.5(5) . . ? C1 C20 C39 117.5(4) . . ? C19 C20 C39 115.9(5) . . ? C22 C21 C26 117.5(6) . . ? C22 C21 C5 120.5(5) . . ? C26 C21 C5 122.1(6) . . ? C21 C22 C23 121.8(5) . . ? C24 C23 C22 119.4(7) . . ? C25 C24 C23 119.9(7) . . ? C24 C25 C26 121.9(6) . . ? C21 C26 C25 119.5(6) . . ? C28 C27 C32 118.0(5) . . ? C28 C27 C10 123.4(5) . . ? C32 C27 C10 118.6(5) . . ? C27 C28 C29 121.0(6) . . ? C30 C29 C28 120.1(7) . . ? C31 C30 C29 120.8(6) . . ? C30 C31 C32 119.3(6) . . ? C27 C32 C31 120.8(6) . . ? C34 C33 C38 117.5(6) . . ? C34 C33 C15 121.7(5) . . ? C38 C33 C15 120.8(5) . . ? C33 C34 C35 120.3(6) . . ? C36 C35 C34 120.5(7) . . ? C37 C36 C35 120.1(7) . . ? C36 C37 C38 120.7(6) . . ? C37 C38 C33 120.9(7) . . ? C44 C39 C40 118.2(5) . . ? C44 C39 C20 121.0(5) . . ? C40 C39 C20 120.8(5) . . ? C39 C40 C41 120.6(6) . . ? C42 C41 C40 120.8(7) . . ? C41 C42 C43 120.2(7) . . ? C42 C43 C44 120.4(7) . . ? C39 C44 C43 119.7(6) . . ? O2 C45 O1 126.4(5) . . ? O2 C45 C45 116.6(5) . 3_666 ? O1 C45 C45 116.9(5) . 3_666 ? O2 C45 Yb1 40.9(2) . 3_666 ? O1 C45 Yb1 166.6(4) . 3_666 ? C45 C45 Yb1 75.8(4) 3_666 3_666 ? C45 O1 Yb1 118.3(3) . . ? C45 O2 Yb1 118.8(3) . 3_666 ? C47 O3 C46 114.2(6) . . ? C47 O3 Yb1 116.5(5) . . ? C46 O3 Yb1 126.6(4) . . ? C48 C47 O3 120.1(7) . . ? C47 C48 O4 118.9(7) . . ? C48 O4 C49 112.3(6) . . ? C48 O4 Yb1 118.0(4) . . ? C49 O4 Yb1 126.7(4) . . ? C51 O5 C50 113.6(6) . . ? O5 C51 C52 112.3(6) . . ? O6 C52 C51 113.4(8) . . ? C52 O6 C53 114.8(8) . . ? C55 O7 C54 116.4(18) . . ? O7 C55 C56 114.0(17) . . ? O8 C56 C55 111.0(16) . . ? C56 O8 C57 119.1(14) . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 25.53 _diffrn_measured_fraction_theta_full 0.877 _refine_diff_density_max 1.321 _refine_diff_density_min -2.325 _refine_diff_density_rms 0.134