Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Michael Scott' _publ_contact_author_address ; Department of Chemistry University of Florida P.O. Box 117200 Gainesville FL 32611 UNITED STATES OF AMERICA ; _publ_contact_author_email MJSCOTT@CHEM.UFL.EDU _publ_section_title ; Highly efficient binding of trivalent f-elements from acidic media with a C3-symmetric tripodal ligand containing diglycolamide arms ; loop_ _publ_author_name 'Michael Scott' 'Artem Gelis' 'Kornelia Matloka' 'Monica Regalbuto' 'George Vandegrift' data_Ybtripoddiamide _database_code_depnum_ccdc_archive 'CCDC 280073' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 5, Yb - tripod diamide' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H150 N9 O23 Yb' _chemical_formula_weight 1863.20 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 b-unique _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 71.172(5) _cell_length_b 12.8866(9) _cell_length_c 23.3365(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.4890(10) _cell_angle_gamma 90.00 _cell_volume 21338(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measurd' _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7912 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type 'Corrected by SADABS' _exptl_absorpt_correction_T_min 0.78239 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Corrected by SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens Smart CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69932 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -94 _diffrn_reflns_limit_h_max 79 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.03 _reflns_number_total 24823 _reflns_number_gt 18157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART' _computing_cell_refinement 'Bruker AXS SMART' _computing_data_reduction 'Bruker AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'Microsoft Word' _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. Two methanol solvate molecules were severely distorted and they were removed from the refinement with the Squeeze program in the Platon Program Package tert-pentyl groups were disordered and several carbon atoms were refined isotropically ; _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^)+(0.0944P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24823 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1471 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.011 _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 0.915751(2) 0.143270(10) 0.825322(6) 0.03731(6) Uani 1 1 d . . . O1 O 0.83846(3) 0.27290(16) 0.79872(9) 0.0379(5) Uani 1 1 d . . . O2 O 0.85282(3) 0.14764(15) 0.95593(10) 0.0351(5) Uani 1 1 d . . . O3 O 0.83877(3) -0.06062(18) 0.82516(11) 0.0426(5) Uani 1 1 d . . . O4 O 0.89339(3) 0.26632(16) 0.84374(9) 0.0374(5) Uani 1 1 d . . . O5 O 0.91108(3) 0.2780(2) 0.75338(10) 0.0460(6) Uani 1 1 d . . . O6 O 0.93355(4) 0.1308(2) 0.74686(13) 0.0573(7) Uani 1 1 d . . . O7 O 0.89771(3) 0.05980(17) 0.88881(11) 0.0430(5) Uani 1 1 d . . . O8 O 0.92286(3) 0.18588(18) 0.92726(10) 0.0429(5) Uani 1 1 d . . . O9 O 0.93832(3) 0.26853(18) 0.84625(10) 0.0437(5) Uani 1 1 d . . . O10 O 0.88876(3) 0.08962(19) 0.77294(10) 0.0455(6) Uani 1 1 d . . . O11 O 0.91578(3) -0.0365(2) 0.79634(15) 0.0626(8) Uani 1 1 d . . . O12 O 0.94131(3) 0.0415(2) 0.86237(13) 0.0557(7) Uani 1 1 d . . . N1 N 0.87239(4) 0.3933(2) 0.81642(13) 0.0426(6) Uani 1 1 d . . . H1A H 0.8700 0.4456 0.7927 0.051 Uiso 1 1 calc R . . N2 N 0.94433(6) 0.1698(5) 0.66206(17) 0.113(2) Uani 1 1 d . . . N3 N 0.88609(4) 0.0333(2) 0.97429(13) 0.0426(6) Uani 1 1 d . . . H3A H 0.8884 0.0374 1.0118 0.051 Uiso 1 1 calc R . . N4 N 0.96133(5) 0.3534(2) 0.89952(15) 0.0543(8) Uani 1 1 d . . . N5 N 0.86772(4) -0.0383(2) 0.74870(13) 0.0442(7) Uani 1 1 d . . . H5A H 0.8661 -0.1046 0.7409 0.053 Uiso 1 1 calc R . . N6 N 0.96189(5) -0.0926(3) 0.8617(3) 0.0987(18) Uani 1 1 d . . . C1 C 0.82239(4) 0.1254(2) 0.86883(14) 0.0329(6) Uani 1 1 d . . . H1B H 0.8359 0.1196 0.8606 0.039 Uiso 1 1 calc R . . C2 C 0.81157(5) 0.1708(2) 0.81514(14) 0.0362(7) Uani 1 1 d . . . C3 C 0.82026(5) 0.2427(2) 0.77995(14) 0.0394(7) Uani 1 1 d . . . C4 C 0.81147(6) 0.2744(3) 0.72741(16) 0.0515(9) Uani 1 1 d . . . C5 C 0.82034(8) 0.3437(4) 0.68245(19) 0.0717(14) Uani 1 1 d . . . C6 C 0.81190(13) 0.4567(4) 0.6895(3) 0.136(3) Uani 1 1 d . . . H6A H 0.7981 0.4529 0.6873 0.203 Uiso 1 1 calc R . . H6B H 0.8158 0.5016 0.6587 0.203 Uiso 1 1 calc R . . H6C H 0.8166 0.4854 0.7268 0.203 Uiso 1 1 calc R . . C7 C 0.84234(10) 0.3535(5) 0.6890(3) 0.108(2) Uani 1 1 d . . . H7A H 0.8480 0.2843 0.6938 0.161 Uiso 1 1 calc R . . H7B H 0.8461 0.3961 0.7227 0.161 Uiso 1 1 calc R . . H7C H 0.8467 0.3863 0.6545 0.161 Uiso 1 1 calc R . . C8 C 0.81580(13) 0.3042(6) 0.6225(2) 0.130(3) Uani 1 1 d . . . H8A H 0.8195 0.3562 0.5941 0.156 Uiso 1 1 calc R . . H8B H 0.8021 0.2911 0.6157 0.156 Uiso 1 1 calc R . . C9 C 0.82739(14) 0.1979(8) 0.6156(4) 0.164(3) Uiso 1 1 d . . . H9A H 0.8271 0.1792 0.5748 0.245 Uiso 1 1 calc R . . H9B H 0.8216 0.1423 0.6369 0.245 Uiso 1 1 calc R . . H9C H 0.8405 0.2078 0.6308 0.245 Uiso 1 1 calc R . . C10 C 0.79301(6) 0.2396(4) 0.71477(18) 0.0667(12) Uani 1 1 d . . . H10A H 0.7866 0.2624 0.6798 0.080 Uiso 1 1 calc R . . C11 C 0.78333(6) 0.1745(3) 0.74927(18) 0.0545(9) Uani 1 1 d . . . C12 C 0.76311(7) 0.1380(4) 0.7357(3) 0.0817(16) Uani 1 1 d . . . C13 C 0.75533(11) 0.1719(8) 0.6779(4) 0.174(5) Uani 1 1 d . . . H13A H 0.7651 0.1661 0.6507 0.261 Uiso 1 1 calc R . . H13B H 0.7512 0.2443 0.6798 0.261 Uiso 1 1 calc R . . H13C H 0.7446 0.1279 0.6652 0.261 Uiso 1 1 calc R . . C14 C 0.75106(9) 0.1717(8) 0.7847(4) 0.162(4) Uani 1 1 d . . . H14A H 0.7475 0.2447 0.7795 0.242 Uiso 1 1 calc R . . H14B H 0.7584 0.1631 0.8217 0.242 Uiso 1 1 calc R . . H14C H 0.7397 0.1287 0.7839 0.242 Uiso 1 1 calc R . . C15 C 0.76217(9) 0.0184(6) 0.7344(3) 0.118(2) Uani 1 1 d . . . H15A H 0.7673 -0.0090 0.7720 0.142 Uiso 1 1 calc R . . H15B H 0.7488 -0.0035 0.7285 0.142 Uiso 1 1 calc R . . C16 C 0.77259(12) -0.0262(6) 0.6894(4) 0.143(3) Uani 1 1 d . . . H16A H 0.7702 -0.1010 0.6870 0.215 Uiso 1 1 calc R . . H16B H 0.7861 -0.0142 0.6983 0.215 Uiso 1 1 calc R . . H16C H 0.7685 0.0064 0.6526 0.215 Uiso 1 1 calc R . . C17 C 0.79328(5) 0.1385(3) 0.79928(16) 0.0449(8) Uani 1 1 d . . . H17A H 0.7874 0.0907 0.8231 0.054 Uiso 1 1 calc R . . C18 C 0.82144(4) 0.1975(2) 0.92099(13) 0.0330(6) Uani 1 1 d . . . C19 C 0.83670(4) 0.2070(2) 0.96193(13) 0.0336(6) Uani 1 1 d . . . C20 C 0.83679(5) 0.2825(3) 1.00632(14) 0.0420(7) Uani 1 1 d . . . C21 C 0.85385(6) 0.3034(3) 1.04964(16) 0.0519(9) Uani 1 1 d . . . C22 C 0.85026(7) 0.3911(4) 1.0912(2) 0.0716(13) Uani 1 1 d . . . H22A H 0.8469 0.4543 1.0694 0.107 Uiso 1 1 calc R . . H22B H 0.8617 0.4037 1.1165 0.107 Uiso 1 1 calc R . . H22C H 0.8399 0.3717 1.1144 0.107 Uiso 1 1 calc R . . C23 C 0.87134(6) 0.3322(4) 1.0177(2) 0.0678(12) Uani 1 1 d . . . H23A H 0.8686 0.3944 0.9944 0.102 Uiso 1 1 calc R . . H23B H 0.8744 0.2746 0.9927 0.102 Uiso 1 1 calc R . . H23C H 0.8820 0.3458 1.0457 0.102 Uiso 1 1 calc R . . C24 C 0.85944(7) 0.2076(4) 1.08666(18) 0.0690(12) Uani 1 1 d . . . H24A H 0.8692 0.2283 1.1171 0.083 Uiso 1 1 calc R . . H24B H 0.8651 0.1553 1.0622 0.083 Uiso 1 1 calc R . . C25 C 0.84277(9) 0.1567(4) 1.1153(2) 0.0893(17) Uani 1 1 d . . . H25A H 0.8472 0.0945 1.1364 0.134 Uiso 1 1 calc R . . H25B H 0.8329 0.1374 1.0856 0.134 Uiso 1 1 calc R . . H25C H 0.8377 0.2061 1.1420 0.134 Uiso 1 1 calc R . . C26 C 0.82034(6) 0.3400(3) 1.00865(16) 0.0458(8) Uani 1 1 d . . . H26A H 0.8200 0.3910 1.0380 0.055 Uiso 1 1 calc R . . C27 C 0.80452(5) 0.3280(3) 0.97119(16) 0.0420(8) Uani 1 1 d . . . C28 C 0.78615(6) 0.3884(3) 0.9786(2) 0.0538(10) Uani 1 1 d . . . C29 C 0.77705(9) 0.4204(5) 0.9180(3) 0.105(2) Uani 1 1 d . . . H29A H 0.7657 0.4618 0.9225 0.158 Uiso 1 1 calc R . . H29B H 0.7736 0.3579 0.8956 0.158 Uiso 1 1 calc R . . H29C H 0.7861 0.4615 0.8979 0.158 Uiso 1 1 calc R . . C30 C 0.79014(7) 0.4929(3) 1.0067(3) 0.094(2) Uani 1 1 d . . . H30A H 0.7968 0.4827 1.0447 0.141 Uiso 1 1 calc R . . H30B H 0.7782 0.5292 1.0108 0.141 Uiso 1 1 calc R . . H30C H 0.7980 0.5343 0.9827 0.141 Uiso 1 1 calc R . . C31 C 0.77292(8) 0.3237(5) 1.0073(3) 0.102(2) Uani 1 1 d . . . H31A H 0.7693 0.2650 0.9814 0.122 Uiso 1 1 calc R . . H31B H 0.7614 0.3653 1.0113 0.122 Uiso 1 1 calc R . . C32 C 0.77908(9) 0.2787(6) 1.0663(3) 0.107(2) Uani 1 1 d . . . H32A H 0.7707 0.2215 1.0749 0.161 Uiso 1 1 calc R . . H32B H 0.7785 0.3329 1.0956 0.161 Uiso 1 1 calc R . . H32C H 0.7920 0.2528 1.0663 0.161 Uiso 1 1 calc R . . C33 C 0.80544(4) 0.2565(2) 0.92667(15) 0.0377(7) Uani 1 1 d . . . H33A H 0.7949 0.2480 0.8996 0.045 Uiso 1 1 calc R . . C34 C 0.81542(4) 0.0163(2) 0.88151(14) 0.0345(6) Uani 1 1 d . . . C35 C 0.82368(5) -0.0729(2) 0.85923(16) 0.0417(8) Uani 1 1 d . . . C36 C 0.81859(6) -0.1723(3) 0.8765(2) 0.0537(10) Uani 1 1 d . . . C37 C 0.82871(7) -0.2720(3) 0.8568(3) 0.0743(15) Uani 1 1 d . . . C38 C 0.84962(7) -0.2677(3) 0.8779(3) 0.0828(16) Uani 1 1 d . . . H38A H 0.8560 -0.3295 0.8646 0.124 Uiso 1 1 calc R . . H38B H 0.8509 -0.2654 0.9200 0.124 Uiso 1 1 calc R . . H38C H 0.8553 -0.2055 0.8625 0.124 Uiso 1 1 calc R . . C39 C 0.82048(11) -0.3696(3) 0.8854(4) 0.145(4) Uani 1 1 d . . . H39A H 0.8263 -0.4322 0.8708 0.217 Uiso 1 1 calc R . . H39B H 0.8068 -0.3722 0.8761 0.217 Uiso 1 1 calc R . . H39C H 0.8232 -0.3657 0.9271 0.217 Uiso 1 1 calc R . . C40 C 0.82649(7) -0.2846(4) 0.7907(3) 0.0792(16) Uani 1 1 d . . . H40A H 0.8348 -0.2332 0.7737 0.095 Uiso 1 1 calc R . . H40B H 0.8311 -0.3544 0.7811 0.095 Uiso 1 1 calc R . . C41 C 0.80685(9) -0.2720(6) 0.7624(4) 0.128(3) Uani 1 1 d . . . H41A H 0.8070 -0.2830 0.7209 0.192 Uiso 1 1 calc R . . H41B H 0.8023 -0.2018 0.7696 0.192 Uiso 1 1 calc R . . H41C H 0.7985 -0.3229 0.7783 0.192 Uiso 1 1 calc R . . C42 C 0.80431(6) -0.1799(3) 0.9134(2) 0.0568(11) Uani 1 1 d . . . H42A H 0.8007 -0.2470 0.9252 0.068 Uiso 1 1 calc R . . C43 C 0.79503(5) -0.0941(3) 0.93416(16) 0.0447(8) Uani 1 1 d . . . C44 C 0.77880(6) -0.1032(3) 0.9734(2) 0.0638(13) Uani 1 1 d . . . C45 C 0.77733(7) -0.2115(3) 0.9989(2) 0.0724(14) Uani 1 1 d . . . H45A H 0.7892 -0.2292 1.0208 0.109 Uiso 1 1 calc R . . H45B H 0.7748 -0.2620 0.9679 0.109 Uiso 1 1 calc R . . H45C H 0.7670 -0.2130 1.0245 0.109 Uiso 1 1 calc R . . C46 C 0.75860(9) -0.0817(6) 0.9273(4) 0.159(4) Uani 1 1 d . . . H46A H 0.7474 -0.0857 0.9491 0.239 Uiso 1 1 calc R . . H46B H 0.7578 -0.1347 0.8970 0.239 Uiso 1 1 calc R . . H46C H 0.7593 -0.0128 0.9098 0.239 Uiso 1 1 calc R . . C47 C 0.77802(15) -0.0203(5) 1.0160(5) 0.147(4) Uani 1 1 d . . . H47A H 0.7778 0.0487 0.9972 0.176 Uiso 1 1 calc R . . H47B H 0.7667 -0.0273 1.0376 0.176 Uiso 1 1 calc R . . C48 C 0.79423(15) -0.0326(9) 1.0520(4) 0.169(4) Uani 1 1 d . . . H48A H 0.7931 0.0075 1.0873 0.254 Uiso 1 1 calc R . . H48B H 0.8051 -0.0078 1.0326 0.254 Uiso 1 1 calc R . . H48C H 0.7959 -0.1062 1.0617 0.254 Uiso 1 1 calc R . . C49 C 0.80110(4) 0.0026(2) 0.91833(14) 0.0374(7) Uani 1 1 d . . . H49A H 0.7953 0.0623 0.9331 0.045 Uiso 1 1 calc R . . C50 C 0.83933(5) 0.3644(2) 0.83419(15) 0.0358(7) Uani 1 1 d . . . H50A H 0.8305 0.3579 0.8648 0.043 Uiso 1 1 calc R . . H50B H 0.8358 0.4263 0.8107 0.043 Uiso 1 1 calc R . . C51 C 0.85952(5) 0.3750(3) 0.86064(15) 0.0404(7) Uani 1 1 d . . . H51A H 0.8603 0.4334 0.8883 0.048 Uiso 1 1 calc R . . H51B H 0.8632 0.3108 0.8819 0.048 Uiso 1 1 calc R . . C52 C 0.88749(5) 0.3354(2) 0.80974(15) 0.0385(7) Uani 1 1 d . . . C53 C 0.89749(6) 0.3570(3) 0.7561(2) 0.0595(11) Uani 1 1 d . . . H53A H 0.8885 0.3554 0.7216 0.071 Uiso 1 1 calc R . . H53B H 0.9036 0.4260 0.7586 0.071 Uiso 1 1 calc R . . C54 C 0.92123(6) 0.2834(5) 0.70329(17) 0.0769(15) Uani 1 1 d . . . H54A H 0.9289 0.3476 0.7035 0.092 Uiso 1 1 calc R . . H54B H 0.9124 0.2830 0.6682 0.092 Uiso 1 1 calc R . . C55 C 0.93368(5) 0.1892(5) 0.70503(18) 0.0691(13) Uani 1 1 d . . . C56 C 0.95601(8) 0.0727(7) 0.6599(3) 0.126(3) Uani 1 1 d . . . H56A H 0.9623 0.0737 0.6230 0.151 Uiso 1 1 calc R . . C57 C 0.97113(7) 0.0736(6) 0.7082(3) 0.101(2) Uani 1 1 d . . . H57A H 0.9807 0.0216 0.7009 0.152 Uiso 1 1 calc R . . H57B H 0.9656 0.0572 0.7443 0.152 Uiso 1 1 calc R . . H57C H 0.9770 0.1424 0.7110 0.152 Uiso 1 1 calc R . . C58 C 0.94399(14) -0.0288(7) 0.6608(4) 0.161(3) Uiso 1 1 d . . . H58A H 0.9523 -0.0893 0.6599 0.241 Uiso 1 1 calc R . . H58B H 0.9349 -0.0302 0.6271 0.241 Uiso 1 1 calc R . . H58C H 0.9373 -0.0306 0.6959 0.241 Uiso 1 1 calc R . . C59 C 0.94409(14) 0.2278(8) 0.6099(4) 0.157(3) Uiso 1 1 d . . . H59A H 0.9350 0.2862 0.6134 0.189 Uiso 1 1 calc R . . C60 C 0.93515(18) 0.1528(8) 0.5594(5) 0.184(5) Uiso 1 1 d . . . H60A H 0.9218 0.1412 0.5645 0.276 Uiso 1 1 calc R . . H60B H 0.9418 0.0862 0.5610 0.276 Uiso 1 1 calc R . . H60C H 0.9364 0.1856 0.5220 0.276 Uiso 1 1 calc R . . C61 C 0.96252(16) 0.2749(9) 0.6008(5) 0.188(4) Uiso 1 1 d . . . H61A H 0.9650 0.3320 0.6280 0.283 Uiso 1 1 calc R . . H61B H 0.9623 0.3015 0.5614 0.283 Uiso 1 1 calc R . . H61C H 0.9724 0.2223 0.6068 0.283 Uiso 1 1 calc R . . C62 C 0.85189(4) 0.0409(2) 0.97442(15) 0.0386(7) Uani 1 1 d . . . H62A H 0.8399 0.0088 0.9589 0.046 Uiso 1 1 calc R . . H62B H 0.8526 0.0371 1.0169 0.046 Uiso 1 1 calc R . . C63 C 0.86840(4) -0.0146(2) 0.95190(17) 0.0417(8) Uani 1 1 d . . . H63A H 0.8682 -0.0884 0.9636 0.050 Uiso 1 1 calc R . . H63B H 0.8674 -0.0117 0.9094 0.050 Uiso 1 1 calc R . . C64 C 0.89869(4) 0.0704(2) 0.94182(16) 0.0393(7) Uani 1 1 d . . . C65 C 0.91515(5) 0.1275(3) 0.97133(17) 0.0484(9) Uani 1 1 d . . . H65A H 0.9109 0.1738 1.0017 0.058 Uiso 1 1 calc R . . H65B H 0.9246 0.0781 0.9890 0.058 Uiso 1 1 calc R . . C66 C 0.93947(5) 0.2418(3) 0.94679(16) 0.0484(8) Uani 1 1 d . . . H66A H 0.9490 0.1944 0.9655 0.058 Uiso 1 1 calc R . . H66B H 0.9365 0.2961 0.9747 0.058 Uiso 1 1 calc R . . C67 C 0.94652(5) 0.2895(3) 0.89395(15) 0.0416(8) Uani 1 1 d . . . C68 C 0.97151(7) 0.3735(4) 0.9559(2) 0.0698(13) Uani 1 1 d . . . H68A H 0.9656 0.3303 0.9852 0.084 Uiso 1 1 calc R . . C69 C 0.99167(7) 0.3421(5) 0.9562(3) 0.0927(19) Uani 1 1 d . . . H69A H 0.9925 0.2713 0.9411 0.139 Uiso 1 1 calc R . . H69B H 0.9975 0.3445 0.9956 0.139 Uiso 1 1 calc R . . H69C H 0.9983 0.3898 0.9319 0.139 Uiso 1 1 calc R . . C70 C 0.96963(9) 0.4873(5) 0.9730(3) 0.107(2) Uani 1 1 d . . . H70A H 0.9566 0.5099 0.9645 0.160 Uiso 1 1 calc R . . H70B H 0.9780 0.5299 0.9512 0.160 Uiso 1 1 calc R . . H70C H 0.9731 0.4951 1.0142 0.160 Uiso 1 1 calc R . . C71 C 0.96790(7) 0.4070(4) 0.8482(2) 0.0671(12) Uani 1 1 d . . . H71A H 0.9784 0.4541 0.8626 0.081 Uiso 1 1 calc R . . C72 C 0.97633(8) 0.3292(4) 0.8075(2) 0.0814(16) Uani 1 1 d . . . H72A H 0.9871 0.2937 0.8277 0.122 Uiso 1 1 calc R . . H72B H 0.9806 0.3662 0.7741 0.122 Uiso 1 1 calc R . . H72C H 0.9667 0.2780 0.7945 0.122 Uiso 1 1 calc R . . C73 C 0.95265(9) 0.4754(4) 0.8193(3) 0.0923(18) Uani 1 1 d . . . H73A H 0.9466 0.5154 0.8484 0.138 Uiso 1 1 calc R . . H73B H 0.9432 0.4319 0.7979 0.138 Uiso 1 1 calc R . . H73C H 0.9583 0.5230 0.7926 0.138 Uiso 1 1 calc R . . C74 C 0.83441(5) -0.0273(3) 0.76695(16) 0.0440(8) Uani 1 1 d . . . H74A H 0.8232 0.0188 0.7648 0.053 Uiso 1 1 calc R . . H74B H 0.8315 -0.0881 0.7419 0.053 Uiso 1 1 calc R . . C75 C 0.85120(5) 0.0303(3) 0.74723(16) 0.0440(8) Uani 1 1 d . . . H75A H 0.8482 0.0561 0.7076 0.053 Uiso 1 1 calc R . . H75B H 0.8540 0.0908 0.7725 0.053 Uiso 1 1 calc R . . C76 C 0.88516(5) -0.0031(3) 0.76147(16) 0.0457(8) Uani 1 1 d . . . C77 C 0.90053(5) -0.0813(4) 0.7618(2) 0.0715(14) Uani 1 1 d . . . H77A H 0.8966 -0.1477 0.7785 0.086 Uiso 1 1 calc R . . H77B H 0.9041 -0.0944 0.7223 0.086 Uiso 1 1 calc R . . C78 C 0.93169(6) -0.1026(4) 0.8050(3) 0.100(2) Uani 1 1 d . . . H78A H 0.9371 -0.1169 0.7680 0.120 Uiso 1 1 calc R . . H78B H 0.9280 -0.1694 0.8220 0.120 Uiso 1 1 calc R . . C79 C 0.94562(6) -0.0474(3) 0.8449(3) 0.0772(16) Uani 1 1 d . . . C80 C 0.97609(6) -0.0429(4) 0.9001(3) 0.0879(18) Uani 1 1 d . . . H80A H 0.9871 -0.0915 0.9023 0.105 Uiso 1 1 calc R . . C81 C 0.98346(6) 0.0573(4) 0.8775(2) 0.0750(13) Uani 1 1 d . . . H81A H 0.9870 0.0469 0.8382 0.113 Uiso 1 1 calc R . . H81B H 0.9946 0.0795 0.9020 0.113 Uiso 1 1 calc R . . H81C H 0.9737 0.1107 0.8777 0.113 Uiso 1 1 calc R . . C82 C 0.97012(10) -0.0384(6) 0.9586(4) 0.122(3) Uani 1 1 d . . . H82A H 0.9686 -0.1090 0.9731 0.183 Uiso 1 1 calc R . . H82B H 0.9581 -0.0016 0.9584 0.183 Uiso 1 1 calc R . . H82C H 0.9796 -0.0015 0.9834 0.183 Uiso 1 1 calc R . . C83 C 0.96669(8) -0.1986(5) 0.8395(6) 0.185(6) Uani 1 1 d . . . H83A H 0.9550 -0.2247 0.8174 0.222 Uiso 1 1 calc R . . C84 C 0.98202(12) -0.1900(6) 0.7958(5) 0.168(4) Uani 1 1 d . . . H84A H 0.9779 -0.1404 0.7656 0.253 Uiso 1 1 calc R . . H84B H 0.9839 -0.2582 0.7786 0.253 Uiso 1 1 calc R . . H84C H 0.9939 -0.1662 0.8157 0.253 Uiso 1 1 calc R . . C85 C 0.97091(11) -0.2745(5) 0.8890(6) 0.217(7) Uani 1 1 d . . . H85A H 0.9601 -0.2775 0.9125 0.325 Uiso 1 1 calc R . . H85B H 0.9821 -0.2511 0.9127 0.325 Uiso 1 1 calc R . . H85C H 0.9732 -0.3436 0.8735 0.325 Uiso 1 1 calc R . . N7 N 0.87649(5) 0.6435(2) 0.75093(14) 0.0499(8) Uani 1 1 d . . . O13 O 0.88935(9) 0.6335(4) 0.7880(3) 0.152(2) Uani 1 1 d . . . O14 O 0.87107(5) 0.7335(2) 0.73394(15) 0.0790(10) Uani 1 1 d . . . O15 O 0.86484(5) 0.5695(2) 0.74406(14) 0.0676(8) Uani 1 1 d . . . N8 N 0.97127(7) 0.2005(4) 1.0823(2) 0.0866(14) Uani 1 1 d . . . O16 O 0.9681(2) 0.1245(10) 1.0540(6) 0.287(6) Uiso 1 1 d . . . O17 O 0.97985(16) 0.1860(10) 1.1247(6) 0.307(6) Uani 1 1 d . . . O18 O 0.95812(11) 0.2531(6) 1.0789(2) 0.185(3) Uani 1 1 d . . . N9 N 0.89223(8) -0.0351(9) 1.1092(2) 0.130(3) Uani 1 1 d . . . O19 O 0.89871(8) -0.0806(7) 1.1539(2) 0.173(3) Uani 1 1 d . . . O20 O 0.87983(10) -0.0811(6) 1.0810(3) 0.168(3) Uani 1 1 d . . . O21 O 0.89743(9) 0.0442(5) 1.0935(2) 0.128(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.03034(8) 0.03593(9) 0.04631(10) -0.00729(6) 0.00715(6) -0.00651(5) O1 0.0434(12) 0.0295(11) 0.0420(12) -0.0063(9) 0.0114(10) -0.0069(9) O2 0.0337(11) 0.0339(11) 0.0385(12) 0.0029(9) 0.0077(9) 0.0024(8) O3 0.0349(12) 0.0397(12) 0.0557(14) -0.0082(11) 0.0191(10) -0.0014(10) O4 0.0418(12) 0.0323(11) 0.0384(12) 0.0007(9) 0.0055(9) -0.0013(9) O5 0.0381(13) 0.0605(15) 0.0406(13) 0.0035(11) 0.0108(10) -0.0058(11) O6 0.0393(14) 0.0758(19) 0.0589(18) -0.0219(15) 0.0170(12) -0.0099(12) O7 0.0358(12) 0.0336(12) 0.0603(16) 0.0013(11) 0.0081(11) -0.0053(9) O8 0.0367(12) 0.0430(13) 0.0483(14) 0.0054(11) 0.0005(10) -0.0129(10) O9 0.0431(13) 0.0434(13) 0.0442(13) -0.0009(11) 0.0016(10) -0.0159(10) O10 0.0375(12) 0.0500(15) 0.0499(14) -0.0171(11) 0.0093(10) -0.0126(11) O11 0.0315(13) 0.0510(15) 0.106(2) -0.0345(16) 0.0114(13) -0.0041(11) O12 0.0337(13) 0.0441(14) 0.090(2) -0.0021(14) 0.0084(13) -0.0038(11) N1 0.0420(16) 0.0344(14) 0.0515(17) 0.0090(13) 0.0046(13) -0.0016(12) N2 0.046(2) 0.255(7) 0.038(2) 0.007(3) 0.0139(17) 0.016(3) N3 0.0307(14) 0.0416(15) 0.0556(18) 0.0093(13) 0.0048(12) -0.0001(11) N4 0.0494(19) 0.061(2) 0.0521(19) -0.0025(15) -0.0001(15) -0.0274(15) N5 0.0336(14) 0.0452(16) 0.0552(18) -0.0185(13) 0.0138(13) -0.0113(12) N6 0.0345(19) 0.047(2) 0.215(6) 0.005(3) 0.012(3) 0.0037(16) C1 0.0308(15) 0.0291(15) 0.0395(17) -0.0012(12) 0.0073(13) -0.0014(11) C2 0.0384(17) 0.0319(15) 0.0386(17) -0.0039(13) 0.0056(13) -0.0026(12) C3 0.0473(19) 0.0319(16) 0.0390(17) -0.0048(13) 0.0039(14) -0.0068(13) C4 0.065(2) 0.045(2) 0.044(2) 0.0040(16) -0.0017(17) -0.0119(18) C5 0.086(3) 0.080(3) 0.046(2) 0.019(2) -0.012(2) -0.032(3) C6 0.224(9) 0.064(4) 0.121(6) 0.047(4) 0.031(6) -0.021(4) C7 0.103(5) 0.141(6) 0.081(4) 0.048(4) 0.024(4) -0.022(4) C8 0.192(8) 0.143(6) 0.053(3) 0.005(4) 0.005(4) -0.088(6) C10 0.074(3) 0.071(3) 0.051(2) 0.015(2) -0.020(2) -0.007(2) C11 0.044(2) 0.064(2) 0.054(2) 0.0062(19) -0.0050(17) -0.0070(18) C12 0.050(3) 0.108(5) 0.083(4) 0.021(3) -0.020(2) -0.016(3) C13 0.099(5) 0.247(10) 0.163(8) 0.088(8) -0.071(5) -0.090(6) C14 0.053(4) 0.295(12) 0.135(7) 0.008(7) -0.009(4) -0.036(5) C15 0.085(4) 0.161(7) 0.105(5) 0.006(5) -0.014(4) -0.056(4) C16 0.160(7) 0.143(7) 0.129(6) -0.046(5) 0.022(6) -0.072(6) C17 0.0438(19) 0.046(2) 0.0450(19) 0.0014(15) 0.0029(15) -0.0048(15) C18 0.0378(16) 0.0276(15) 0.0345(16) 0.0014(12) 0.0085(12) -0.0008(12) C19 0.0334(15) 0.0308(15) 0.0374(16) 0.0014(12) 0.0086(12) 0.0003(12) C20 0.0486(19) 0.0406(18) 0.0374(17) -0.0022(14) 0.0064(14) 0.0005(15) C21 0.056(2) 0.054(2) 0.045(2) -0.0098(17) -0.0012(17) 0.0022(18) C22 0.079(3) 0.077(3) 0.057(3) -0.029(2) -0.009(2) 0.008(3) C23 0.048(2) 0.089(3) 0.066(3) -0.022(2) -0.002(2) -0.011(2) C24 0.076(3) 0.084(3) 0.044(2) 0.000(2) -0.011(2) 0.010(2) C25 0.113(5) 0.106(4) 0.051(3) 0.013(3) 0.015(3) 0.005(3) C26 0.053(2) 0.0400(19) 0.046(2) -0.0095(15) 0.0130(16) 0.0030(15) C27 0.0421(19) 0.0358(16) 0.050(2) -0.0023(15) 0.0132(15) 0.0078(14) C28 0.045(2) 0.0414(19) 0.076(3) -0.0075(19) 0.0153(19) 0.0098(16) C29 0.085(4) 0.112(5) 0.120(5) -0.005(4) 0.006(4) 0.050(4) C30 0.063(3) 0.043(2) 0.182(6) -0.012(3) 0.038(3) 0.009(2) C31 0.068(3) 0.071(3) 0.174(7) 0.011(4) 0.055(4) 0.011(3) C32 0.103(5) 0.127(5) 0.098(5) 0.030(4) 0.039(4) 0.014(4) C33 0.0355(16) 0.0312(15) 0.0470(18) 0.0012(13) 0.0082(14) 0.0007(12) C34 0.0308(15) 0.0309(15) 0.0425(17) -0.0015(13) 0.0077(13) -0.0004(12) C35 0.0355(17) 0.0335(16) 0.058(2) -0.0087(15) 0.0176(15) -0.0018(13) C36 0.052(2) 0.0299(16) 0.083(3) -0.0082(18) 0.028(2) 0.0021(15) C37 0.071(3) 0.0304(19) 0.128(4) -0.005(2) 0.053(3) 0.0029(18) C38 0.079(3) 0.047(2) 0.126(5) -0.006(3) 0.032(3) 0.022(2) C39 0.151(6) 0.026(2) 0.276(11) -0.005(4) 0.140(7) 0.008(3) C40 0.063(3) 0.051(2) 0.127(5) -0.041(3) 0.030(3) -0.004(2) C41 0.086(4) 0.119(6) 0.179(7) -0.075(5) 0.006(4) -0.021(4) C42 0.060(2) 0.0240(15) 0.091(3) 0.0021(18) 0.032(2) -0.0030(16) C43 0.0430(19) 0.0339(17) 0.060(2) 0.0001(16) 0.0212(16) -0.0009(14) C44 0.066(3) 0.040(2) 0.092(3) 0.002(2) 0.048(3) -0.0034(19) C45 0.075(3) 0.052(2) 0.097(4) 0.019(2) 0.047(3) -0.005(2) C46 0.084(4) 0.134(6) 0.277(11) 0.076(7) 0.125(6) 0.028(4) C47 0.177(8) 0.076(4) 0.208(10) -0.004(5) 0.148(8) -0.013(5) C48 0.154(9) 0.209(11) 0.154(9) 0.032(8) 0.068(8) -0.005(9) C49 0.0351(16) 0.0313(15) 0.0474(19) -0.0019(13) 0.0132(14) 0.0034(12) C50 0.0433(18) 0.0235(14) 0.0411(17) -0.0013(12) 0.0061(14) -0.0016(12) C51 0.0419(18) 0.0375(17) 0.0415(18) -0.0012(14) 0.0020(14) -0.0003(13) C52 0.0383(17) 0.0324(16) 0.0445(18) 0.0036(13) 0.0020(14) -0.0088(13) C53 0.046(2) 0.071(3) 0.063(3) 0.028(2) 0.0151(19) 0.0029(18) C54 0.039(2) 0.152(5) 0.041(2) 0.019(3) 0.0111(17) -0.002(3) C55 0.0299(19) 0.134(4) 0.043(2) -0.017(3) 0.0048(16) -0.003(2) C56 0.060(3) 0.216(9) 0.107(5) -0.053(5) 0.039(3) 0.017(4) C57 0.058(3) 0.146(6) 0.104(4) -0.020(4) 0.027(3) 0.005(3) C62 0.0298(15) 0.0369(17) 0.0501(19) 0.0098(14) 0.0100(14) 0.0013(12) C63 0.0303(16) 0.0318(16) 0.064(2) 0.0044(15) 0.0113(15) 0.0012(12) C64 0.0349(16) 0.0290(15) 0.055(2) 0.0062(14) 0.0080(14) 0.0019(12) C65 0.0390(19) 0.054(2) 0.052(2) 0.0138(17) 0.0044(16) -0.0076(15) C66 0.0371(18) 0.052(2) 0.055(2) 0.0032(17) -0.0036(15) -0.0163(15) C67 0.0389(18) 0.0353(17) 0.050(2) -0.0029(14) -0.0004(15) -0.0113(14) C68 0.055(3) 0.091(3) 0.062(3) -0.010(2) -0.004(2) -0.034(2) C69 0.056(3) 0.136(5) 0.083(4) -0.012(3) -0.012(3) -0.023(3) C70 0.097(4) 0.123(5) 0.099(4) -0.050(4) -0.001(3) -0.045(4) C71 0.067(3) 0.064(3) 0.071(3) -0.002(2) 0.008(2) -0.038(2) C72 0.080(3) 0.096(4) 0.072(3) -0.012(3) 0.029(3) -0.044(3) C73 0.106(4) 0.067(3) 0.104(4) 0.032(3) 0.007(3) -0.032(3) C74 0.0361(17) 0.0456(19) 0.052(2) -0.0167(16) 0.0130(15) -0.0072(14) C75 0.0395(18) 0.0432(18) 0.051(2) -0.0094(15) 0.0120(15) -0.0051(14) C76 0.0432(19) 0.050(2) 0.047(2) -0.0201(16) 0.0189(15) -0.0131(15) C77 0.040(2) 0.064(3) 0.113(4) -0.049(3) 0.021(2) -0.0100(19) C78 0.037(2) 0.055(3) 0.209(7) -0.054(4) 0.012(3) 0.004(2) C79 0.031(2) 0.047(2) 0.155(5) -0.013(3) 0.021(2) -0.0025(17) C80 0.038(2) 0.063(3) 0.162(6) 0.028(3) 0.005(3) 0.002(2) C81 0.053(3) 0.060(3) 0.112(4) 0.002(3) 0.004(2) -0.009(2) C82 0.097(5) 0.111(5) 0.161(7) 0.046(5) 0.026(5) 0.014(4) C83 0.043(3) 0.079(5) 0.432(17) -0.088(7) 0.013(6) 0.016(3) C84 0.114(6) 0.118(6) 0.271(12) -0.104(7) -0.001(7) 0.033(5) C85 0.108(6) 0.041(3) 0.51(2) 0.037(7) 0.091(9) 0.016(4) N7 0.074(2) 0.0242(14) 0.0476(17) 0.0057(12) -0.0207(16) -0.0059(13) O13 0.131(5) 0.161(5) 0.153(5) 0.038(4) -0.050(4) -0.036(4) O14 0.113(3) 0.0372(15) 0.090(2) 0.0011(15) 0.027(2) -0.0060(16) O15 0.081(2) 0.0399(14) 0.079(2) 0.0086(14) -0.0105(16) -0.0118(14) N8 0.078(3) 0.096(4) 0.079(3) 0.023(3) -0.038(2) -0.016(3) O17 0.241(10) 0.319(13) 0.334(15) -0.013(11) -0.156(10) 0.009(10) O18 0.221(7) 0.234(8) 0.099(4) 0.037(4) 0.014(4) 0.093(7) N9 0.067(3) 0.288(11) 0.036(3) 0.016(4) 0.001(2) 0.010(5) O19 0.120(4) 0.332(9) 0.067(3) 0.063(4) 0.010(3) 0.052(5) O20 0.176(6) 0.200(6) 0.119(4) 0.059(4) -0.043(4) -0.049(5) O21 0.129(5) 0.172(6) 0.081(4) -0.025(3) -0.012(3) 0.053(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O10 2.301(2) . ? Yb1 O7 2.302(2) . ? Yb1 O9 2.303(2) . ? Yb1 O4 2.311(2) . ? Yb1 O6 2.312(3) . ? Yb1 O12 2.351(3) . ? Yb1 O11 2.413(2) . ? Yb1 O5 2.420(2) . ? Yb1 O8 2.455(2) . ? Yb1 C76 3.164(3) . ? Yb1 C52 3.192(3) . ? Yb1 C64 3.204(3) . ? O1 C3 1.390(4) . ? O1 C50 1.439(4) . ? O2 C19 1.395(4) . ? O2 C62 1.444(4) . ? O3 C35 1.394(4) . ? O3 C74 1.436(4) . ? O4 C52 1.243(4) . ? O5 C53 1.409(5) . ? O5 C54 1.423(4) . ? O6 C55 1.233(6) . ? O7 C64 1.241(4) . ? O8 C65 1.419(4) . ? O8 C66 1.428(4) . ? O9 C67 1.245(4) . ? O10 C76 1.247(4) . ? O11 C78 1.419(5) . ? O11 C77 1.423(5) . ? O12 C79 1.263(5) . ? N1 C52 1.328(4) . ? N1 C51 1.452(4) . ? N2 C55 1.327(5) . ? N2 C59 1.427(10) . ? N2 C56 1.505(10) . ? N3 C64 1.309(4) . ? N3 C63 1.461(4) . ? N4 C67 1.336(4) . ? N4 C68 1.475(6) . ? N4 C71 1.489(5) . ? N5 C76 1.333(4) . ? N5 C75 1.469(4) . ? N6 C79 1.327(6) . ? N6 C80 1.447(8) . ? N6 C83 1.510(7) . ? C1 C34 1.527(4) . ? C1 C2 1.534(5) . ? C1 C18 1.537(4) . ? C2 C17 1.389(5) . ? C2 C3 1.413(4) . ? C3 C4 1.393(5) . ? C4 C10 1.398(6) . ? C4 C5 1.550(5) . ? C5 C8 1.501(7) . ? C5 C7 1.566(9) . ? C5 C6 1.589(8) . ? C8 C9 1.613(12) . ? C10 C11 1.383(6) . ? C11 C17 1.396(5) . ? C11 C12 1.523(6) . ? C12 C13 1.482(9) . ? C12 C15 1.543(9) . ? C12 C14 1.544(10) . ? C15 C16 1.450(10) . ? C18 C33 1.384(4) . ? C18 C19 1.395(4) . ? C19 C20 1.420(4) . ? C20 C26 1.391(5) . ? C20 C21 1.541(5) . ? C21 C22 1.524(5) . ? C21 C24 1.542(6) . ? C21 C23 1.545(6) . ? C24 C25 1.552(7) . ? C26 C27 1.379(5) . ? C27 C33 1.394(5) . ? C27 C28 1.542(5) . ? C28 C31 1.460(7) . ? C28 C30 1.515(6) . ? C28 C29 1.563(8) . ? C31 C32 1.527(9) . ? C34 C49 1.395(4) . ? C34 C35 1.409(4) . ? C35 C36 1.399(5) . ? C36 C42 1.387(5) . ? C36 C37 1.559(5) . ? C37 C38 1.531(7) . ? C37 C40 1.548(8) . ? C37 C39 1.559(6) . ? C40 C41 1.507(8) . ? C42 C43 1.394(5) . ? C43 C49 1.379(4) . ? C43 C44 1.534(5) . ? C44 C47 1.463(9) . ? C44 C45 1.524(6) . ? C44 C46 1.749(10) . ? C47 C48 1.383(13) . ? C50 C51 1.525(5) . ? C52 C53 1.513(5) . ? C54 C55 1.502(7) . ? C56 C57 1.497(9) . ? C56 C58 1.565(11) . ? C59 C61 1.476(12) . ? C59 C60 1.616(14) . ? C62 C63 1.505(4) . ? C64 C65 1.503(5) . ? C66 C67 1.499(5) . ? C68 C69 1.490(7) . ? C68 C70 1.529(8) . ? C71 C73 1.515(8) . ? C71 C72 1.536(7) . ? C74 C75 1.509(4) . ? C76 C77 1.487(6) . ? C78 C79 1.487(7) . ? C80 C82 1.461(9) . ? C80 C81 1.505(6) . ? C83 C85 1.524(15) . ? C83 C84 1.555(13) . ? N7 O13 1.217(6) . ? N7 O15 1.266(4) . ? N7 O14 1.276(4) . ? N8 O17 1.136(10) . ? N8 O18 1.153(7) . ? N8 O16 1.193(13) . ? N9 O21 1.155(9) . ? N9 O20 1.213(9) . ? N9 O19 1.253(8) . ? 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 O10 Yb1 O7 73.56(9) . . ? O10 Yb1 O9 149.64(9) . . ? O7 Yb1 O9 127.31(8) . . ? O10 Yb1 O4 75.31(8) . . ? O7 Yb1 O4 76.93(8) . . ? O9 Yb1 O4 87.64(8) . . ? O10 Yb1 O6 92.57(9) . . ? O7 Yb1 O6 147.68(9) . . ? O9 Yb1 O6 78.47(9) . . ? O4 Yb1 O6 128.54(10) . . ? O10 Yb1 O12 128.13(9) . . ? O7 Yb1 O12 87.55(9) . . ? O9 Yb1 O12 78.81(9) . . ? O4 Yb1 O12 146.98(9) . . ? O6 Yb1 O12 78.25(11) . . ? O10 Yb1 O11 65.27(9) . . ? O7 Yb1 O11 75.20(9) . . ? O9 Yb1 O11 135.77(8) . . ? O4 Yb1 O11 136.59(8) . . ? O6 Yb1 O11 72.48(10) . . ? O12 Yb1 O11 63.28(9) . . ? O10 Yb1 O5 77.49(9) . . ? O7 Yb1 O5 136.76(8) . . ? O9 Yb1 O5 72.54(8) . . ? O4 Yb1 O5 65.01(8) . . ? O6 Yb1 O5 63.55(10) . . ? O12 Yb1 O5 135.68(8) . . ? O11 Yb1 O5 119.82(10) . . ? O10 Yb1 O8 133.01(8) . . ? O7 Yb1 O8 64.15(8) . . ? O9 Yb1 O8 63.27(8) . . ? O4 Yb1 O8 76.06(8) . . ? O6 Yb1 O8 134.31(9) . . ? O12 Yb1 O8 70.95(9) . . ? O11 Yb1 O8 118.79(10) . . ? O5 Yb1 O8 121.22(8) . . ? O10 Yb1 C76 19.20(10) . . ? O7 Yb1 C76 68.07(9) . . ? O9 Yb1 C76 163.90(9) . . ? O4 Yb1 C76 92.18(9) . . ? O6 Yb1 C76 89.16(9) . . ? O12 Yb1 C76 108.96(10) . . ? O11 Yb1 C76 46.48(9) . . ? O5 Yb1 C76 92.80(9) . . ? O8 Yb1 C76 132.20(8) . . ? O10 Yb1 C52 71.34(9) . . ? O7 Yb1 C52 93.29(8) . . ? O9 Yb1 C52 84.46(9) . . ? O4 Yb1 C52 18.57(8) . . ? O6 Yb1 C52 110.06(10) . . ? O12 Yb1 C52 159.49(9) . . ? O11 Yb1 C52 136.61(9) . . ? O5 Yb1 C52 46.64(8) . . ? O8 Yb1 C52 90.99(9) . . ? C76 Yb1 C52 90.25(9) . . ? O10 Yb1 C64 90.38(9) . . ? O7 Yb1 C64 18.07(9) . . ? O9 Yb1 C64 109.26(9) . . ? O4 Yb1 C64 74.39(8) . . ? O6 Yb1 C64 156.80(10) . . ? O12 Yb1 C64 81.85(9) . . ? O11 Yb1 C64 88.00(10) . . ? O5 Yb1 C64 139.32(8) . . ? O8 Yb1 C64 46.09(8) . . ? C76 Yb1 C64 86.12(9) . . ? C52 Yb1 C64 92.68(8) . . ? C3 O1 C50 114.0(2) . . ? C19 O2 C62 115.8(2) . . ? C35 O3 C74 117.0(3) . . ? C52 O4 Yb1 125.1(2) . . ? C53 O5 C54 113.4(3) . . ? C53 O5 Yb1 123.0(2) . . ? C54 O5 Yb1 123.6(3) . . ? C55 O6 Yb1 128.5(3) . . ? C64 O7 Yb1 126.8(2) . . ? C65 O8 C66 113.2(3) . . ? C65 O8 Yb1 121.4(2) . . ? C66 O8 Yb1 121.7(2) . . ? C67 O9 Yb1 127.7(2) . . ? C76 O10 Yb1 123.4(3) . . ? C78 O11 C77 113.6(3) . . ? C78 O11 Yb1 123.7(2) . . ? C77 O11 Yb1 122.1(2) . . ? C79 O12 Yb1 126.0(3) . . ? C52 N1 C51 123.6(3) . . ? C55 N2 C59 125.2(7) . . ? C55 N2 C56 122.1(6) . . ? C59 N2 C56 112.1(6) . . ? C64 N3 C63 123.9(3) . . ? C67 N4 C68 121.6(3) . . ? C67 N4 C71 120.2(3) . . ? C68 N4 C71 118.2(3) . . ? C76 N5 C75 122.1(3) . . ? C79 N6 C80 122.7(4) . . ? C79 N6 C83 120.7(5) . . ? C80 N6 C83 116.5(4) . . ? C34 C1 C2 111.0(3) . . ? C34 C1 C18 111.6(2) . . ? C2 C1 C18 111.5(2) . . ? C17 C2 C3 119.0(3) . . ? C17 C2 C1 120.2(3) . . ? C3 C2 C1 120.7(3) . . ? O1 C3 C4 122.6(3) . . ? O1 C3 C2 116.1(3) . . ? C4 C3 C2 121.1(3) . . ? C3 C4 C10 116.2(3) . . ? C3 C4 C5 125.9(4) . . ? C10 C4 C5 117.9(4) . . ? C8 C5 C4 111.5(4) . . ? C8 C5 C7 105.0(5) . . ? C4 C5 C7 116.0(4) . . ? C8 C5 C6 110.6(6) . . ? C4 C5 C6 106.4(4) . . ? C7 C5 C6 107.4(5) . . ? C5 C8 C9 107.9(7) . . ? C11 C10 C4 125.1(4) . . ? C10 C11 C17 116.4(4) . . ? C10 C11 C12 124.8(4) . . ? C17 C11 C12 118.7(4) . . ? C13 C12 C11 112.2(5) . . ? C13 C12 C15 105.3(6) . . ? C11 C12 C15 110.5(5) . . ? C13 C12 C14 113.6(7) . . ? C11 C12 C14 109.2(5) . . ? C15 C12 C14 105.6(6) . . ? C16 C15 C12 112.7(6) . . ? C2 C17 C11 121.8(3) . . ? C33 C18 C19 119.2(3) . . ? C33 C18 C1 119.7(3) . . ? C19 C18 C1 121.0(3) . . ? C18 C19 O2 119.0(3) . . ? C18 C19 C20 121.3(3) . . ? O2 C19 C20 119.5(3) . . ? C26 C20 C19 116.0(3) . . ? C26 C20 C21 120.2(3) . . ? C19 C20 C21 123.8(3) . . ? C22 C21 C20 112.6(3) . . ? C22 C21 C24 106.7(4) . . ? C20 C21 C24 112.5(3) . . ? C22 C21 C23 108.1(4) . . ? C20 C21 C23 110.4(3) . . ? C24 C21 C23 106.3(4) . . ? C21 C24 C25 114.0(4) . . ? C27 C26 C20 124.3(3) . . ? C26 C27 C33 117.6(3) . . ? C26 C27 C28 122.0(3) . . ? C33 C27 C28 120.4(3) . . ? C31 C28 C30 114.5(4) . . ? C31 C28 C27 110.2(4) . . ? C30 C28 C27 111.4(3) . . ? C31 C28 C29 109.2(5) . . ? C30 C28 C29 102.0(4) . . ? C27 C28 C29 109.1(4) . . ? C28 C31 C32 118.8(6) . . ? C18 C33 C27 121.4(3) . . ? C49 C34 C35 118.0(3) . . ? C49 C34 C1 120.0(3) . . ? C35 C34 C1 121.9(3) . . ? O3 C35 C36 119.8(3) . . ? O3 C35 C34 118.7(3) . . ? C36 C35 C34 121.1(3) . . ? C42 C36 C35 117.5(3) . . ? C42 C36 C37 120.2(3) . . ? C35 C36 C37 122.3(3) . . ? C38 C37 C40 110.2(4) . . ? C38 C37 C39 106.3(5) . . ? C40 C37 C39 109.2(5) . . ? C38 C37 C36 109.7(4) . . ? C40 C37 C36 111.5(4) . . ? C39 C37 C36 110.0(3) . . ? C41 C40 C37 116.4(4) . . ? C36 C42 C43 123.4(3) . . ? C49 C43 C42 117.2(3) . . ? C49 C43 C44 119.7(3) . . ? C42 C43 C44 123.1(3) . . ? C47 C44 C45 113.3(5) . . ? C47 C44 C43 114.8(4) . . ? C45 C44 C43 112.4(3) . . ? C47 C44 C46 103.3(6) . . ? C45 C44 C46 107.9(4) . . ? C43 C44 C46 104.0(4) . . ? C48 C47 C44 104.8(8) . . ? C43 C49 C34 122.6(3) . . ? O1 C50 C51 107.6(3) . . ? N1 C51 C50 110.7(3) . . ? O4 C52 N1 124.3(3) . . ? O4 C52 C53 120.2(3) . . ? N1 C52 C53 115.5(3) . . ? O4 C52 Yb1 36.31(15) . . ? N1 C52 Yb1 158.6(2) . . ? C53 C52 Yb1 84.5(2) . . ? O5 C53 C52 105.9(3) . . ? O5 C54 C55 105.9(4) . . ? O6 C55 N2 121.5(5) . . ? O6 C55 C54 118.3(3) . . ? N2 C55 C54 120.2(5) . . ? C57 C56 N2 109.6(6) . . ? C57 C56 C58 110.9(8) . . ? N2 C56 C58 113.0(6) . . ? N2 C59 C61 112.8(9) . . ? N2 C59 C60 106.7(8) . . ? C61 C59 C60 116.3(10) . . ? O2 C62 C63 107.0(2) . . ? N3 C63 C62 110.4(3) . . ? O7 C64 N3 123.3(3) . . ? O7 C64 C65 119.5(3) . . ? N3 C64 C65 117.2(3) . . ? O7 C64 Yb1 35.12(14) . . ? N3 C64 Yb1 157.0(3) . . ? C65 C64 Yb1 84.95(19) . . ? O8 C65 C64 105.0(3) . . ? O8 C66 C67 105.4(3) . . ? O9 C67 N4 122.1(3) . . ? O9 C67 C66 118.9(3) . . ? N4 C67 C66 119.0(3) . . ? N4 C68 C69 111.2(4) . . ? N4 C68 C70 110.7(4) . . ? C69 C68 C70 111.3(4) . . ? N4 C71 C73 111.7(4) . . ? N4 C71 C72 110.9(4) . . ? C73 C71 C72 113.8(5) . . ? O3 C74 C75 108.5(3) . . ? N5 C75 C74 110.4(3) . . ? O10 C76 N5 123.1(3) . . ? O10 C76 C77 120.7(3) . . ? N5 C76 C77 116.3(3) . . ? O10 C76 Yb1 37.37(18) . . ? N5 C76 Yb1 154.5(2) . . ? C77 C76 Yb1 85.6(2) . . ? O11 C77 C76 104.8(3) . . ? O11 C78 C79 106.7(3) . . ? O12 C79 N6 122.0(5) . . ? O12 C79 C78 118.0(4) . . ? N6 C79 C78 119.9(4) . . ? N6 C80 C82 110.9(5) . . ? N6 C80 C81 114.1(5) . . ? C82 C80 C81 115.3(6) . . ? N6 C83 C85 111.0(9) . . ? N6 C83 C84 110.5(7) . . ? C85 C83 C84 115.8(6) . . ? O13 N7 O15 117.3(4) . . ? O13 N7 O14 120.7(4) . . ? O15 N7 O14 117.8(3) . . ? O17 N8 O18 122.4(10) . . ? O17 N8 O16 114.3(10) . . ? O18 N8 O16 109.1(9) . . ? O21 N9 O20 119.9(7) . . ? O21 N9 O19 124.8(9) . . ? O20 N9 O19 115.3(10) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.653 _refine_diff_density_min -0.898 _refine_diff_density_rms 0.088 #===END data_Cetripoddiamide _database_code_depnum_ccdc_archive 'CCDC 280074' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 6, Ce - tripod diamide' _chemical_melting_point Unkown _chemical_formula_moiety ? _chemical_formula_sum 'C93 H168 Ce2 N12 O35' _chemical_formula_weight 2294.63 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'b unique' _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 19.075(2) _cell_length_b 13.2833(14) _cell_length_c 24.916(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.643(2) _cell_angle_gamma 90.00 _cell_volume 5907.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measurd' _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2412 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type 'Corrected by SADABS' _exptl_absorpt_correction_T_min 0.824646 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Corrected by SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Siemens Smart CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33661 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.1695 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.43 _reflns_number_total 22398 _reflns_number_gt 12522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART' _computing_cell_refinement 'Bruker AXS SMART' _computing_data_reduction 'Bruker AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'Microsoft Word' _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. Three methanol solvate molecules were severely distorted and they were removed from the refinement with the Squeeze program in the Platon Program Package tert-pentyl groups were disordered and several carbon atoms were refined isotropically An RSC reviewer did not like the long refined distances in two of the ethyl arms in the t-pentyl groups (C37-C38) and (C47-C48) so DFIX 1.6 was used to lock the separation. Hydrogen atoms have been omitted from the ether solvate. ; _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^)+(0.0920P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(17) _refine_ls_number_reflns 22398 _refine_ls_number_parameters 1195 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.1889 _refine_ls_wR_factor_gt 0.1666 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _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 Ce1 Ce 0.79933(3) -0.85637(4) 0.38124(2) 0.03071(16) Uani 1 1 d . . . O1 O 1.0534(5) -0.7076(6) 0.5458(4) 0.052(2) Uani 1 1 d . . . O2 O 1.1149(4) -0.7722(5) 0.4059(3) 0.0434(19) Uani 1 1 d . . . O3 O 1.0662(4) -1.0067(5) 0.5102(3) 0.0376(17) Uani 1 1 d . . . O4 O 0.8873(5) -0.7193(5) 0.4180(4) 0.048(2) Uani 1 1 d . . . O5 O 0.7714(4) -0.7309(5) 0.4510(3) 0.0389(18) Uani 1 1 d . . . O6 O 0.6936(5) -0.8874(6) 0.4111(4) 0.042(2) Uani 1 1 d . . . O7 O 0.9087(5) -0.8988(6) 0.3580(4) 0.049(2) Uani 1 1 d . . . O8 O 0.8117(4) -0.7801(5) 0.2912(3) 0.0421(19) Uani 1 1 d . . . O9 O 0.7047(5) -0.7327(6) 0.3245(4) 0.048(2) Uani 1 1 d . . . O10 O 0.8796(5) -0.9262(6) 0.4708(4) 0.043(2) Uani 1 1 d . . . O11 O 0.7936(5) -1.0467(5) 0.3933(4) 0.044(2) Uani 1 1 d . . . O12 O 0.7249(5) -0.9590(6) 0.2985(4) 0.048(2) Uani 1 1 d . . . N1 N 0.9375(5) -0.5855(6) 0.4740(4) 0.038(2) Uani 1 1 d . . . H1A H 0.9304 -0.5360 0.4937 0.046 Uiso 1 1 calc R . . N2 N 0.6023(7) -0.8524(8) 0.4442(5) 0.053(3) Uani 1 1 d . . . N3 N 0.9997(5) -0.8714(7) 0.3190(5) 0.045(3) Uani 1 1 d . . . H3A H 1.0100 -0.8456 0.2910 0.054 Uiso 1 1 calc R . . N4 N 0.6320(5) -0.6576(6) 0.2452(4) 0.039(2) Uani 1 1 d . . . N5 N 0.9329(5) -1.0561(7) 0.5333(4) 0.038(2) Uani 1 1 d . . . H5A H 0.9277 -1.1171 0.5429 0.046 Uiso 1 1 calc R . . N6 N 0.6677(6) -1.0918(7) 0.2497(4) 0.056(3) Uani 1 1 d . . . C1 C 1.1582(6) -0.8384(7) 0.5210(5) 0.040(3) Uani 1 1 d . . . H1B H 1.1056 -0.8348 0.4956 0.048 Uiso 1 1 calc R . . C2 C 1.1625(6) -0.8144(9) 0.5850(5) 0.045(3) Uani 1 1 d . . . C3 C 1.1100(8) -0.7493(9) 0.5929(5) 0.052(3) Uani 1 1 d . . . C4 C 1.1109(8) -0.7301(10) 0.6495(6) 0.066(4) Uani 1 1 d . . . C5 C 1.0464(12) -0.6741(12) 0.6619(7) 0.089(6) Uani 1 1 d . . . C6 C 0.9710(12) -0.712(2) 0.6267(10) 0.145(9) Uani 1 1 d . . . H6A H 0.9686 -0.7832 0.6324 0.217 Uiso 1 1 calc R . . H6B H 0.9618 -0.6986 0.5869 0.217 Uiso 1 1 calc R . . H6C H 0.9338 -0.6786 0.6380 0.217 Uiso 1 1 calc R . . C7 C 1.0548(14) -0.6777(15) 0.7249(9) 0.140(9) Uani 1 1 d . . . H7A H 1.1026 -0.6503 0.7478 0.210 Uiso 1 1 calc R . . H7B H 1.0515 -0.7462 0.7360 0.210 Uiso 1 1 calc R . . H7C H 1.0157 -0.6387 0.7307 0.210 Uiso 1 1 calc R . . C8 C 1.0453(15) -0.5548(16) 0.6481(11) 0.146(9) Uani 1 1 d . . . H8A H 1.0208 -0.5445 0.6072 0.175 Uiso 1 1 calc R . . H8B H 1.0159 -0.5202 0.6674 0.175 Uiso 1 1 calc R . . C9 C 1.1259(16) -0.5070(15) 0.6678(10) 0.147(10) Uani 1 1 d . . . H9A H 1.1220 -0.4365 0.6588 0.220 Uiso 1 1 calc R . . H9B H 1.1549 -0.5397 0.6483 0.220 Uiso 1 1 calc R . . H9C H 1.1501 -0.5156 0.7085 0.220 Uiso 1 1 calc R . . C10 C 1.1667(9) -0.7777(11) 0.6927(6) 0.068(4) Uani 1 1 d . . . H10A H 1.1674 -0.7684 0.7299 0.082 Uiso 1 1 calc R . . C11 C 1.2192(9) -0.8355(12) 0.6861(7) 0.078(5) Uani 1 1 d . . . C12 C 1.2823(10) -0.8919(12) 0.7341(6) 0.080(5) Uani 1 1 d . . . C13 C 1.290(2) -0.839(2) 0.7927(7) 0.25(2) Uani 1 1 d . . . H13A H 1.2451 -0.8498 0.8010 0.373 Uiso 1 1 calc R . . H13B H 1.2974 -0.7679 0.7897 0.373 Uiso 1 1 calc R . . H13C H 1.3320 -0.8666 0.8229 0.373 Uiso 1 1 calc R . . C14 C 1.3603(13) -0.871(2) 0.7306(9) 0.178(13) Uani 1 1 d . . . H14A H 1.3633 -0.9017 0.6965 0.267 Uiso 1 1 calc R . . H14B H 1.3983 -0.8992 0.7636 0.267 Uiso 1 1 calc R . . H14C H 1.3678 -0.7999 0.7294 0.267 Uiso 1 1 calc R . . C15 C 1.2765(18) -1.008(3) 0.7367(14) 0.207(13) Uiso 1 1 d . . . H15A H 1.3153 -1.0354 0.7704 0.248 Uiso 1 1 calc R . . H15B H 1.2806 -1.0396 0.7027 0.248 Uiso 1 1 calc R . . C16 C 1.1946(13) -1.0259(18) 0.7400(10) 0.139(8) Uiso 1 1 d . . . H16A H 1.1850 -1.0968 0.7405 0.209 Uiso 1 1 calc R . . H16B H 1.1575 -0.9958 0.7072 0.209 Uiso 1 1 calc R . . H16C H 1.1924 -0.9955 0.7743 0.209 Uiso 1 1 calc R . . C17 C 1.2155(6) -0.8575(9) 0.6310(4) 0.045(3) Uani 1 1 d . . . H17A H 1.2497 -0.9024 0.6253 0.054 Uiso 1 1 calc R . . C18 C 1.2019(6) -0.7575(8) 0.5024(4) 0.036(3) Uani 1 1 d . . . C19 C 1.1783(5) -0.7243(7) 0.4455(5) 0.034(2) Uani 1 1 d . . . C20 C 1.2128(8) -0.6442(10) 0.4280(5) 0.057(3) Uani 1 1 d . . . C21 C 1.1800(9) -0.5998(10) 0.3636(6) 0.067(4) Uani 1 1 d . . . C22 C 1.2243(11) -0.4984(9) 0.3626(7) 0.101(6) Uani 1 1 d . . . H22A H 1.2051 -0.4693 0.3249 0.151 Uiso 1 1 calc R . . H22B H 1.2766 -0.5131 0.3723 0.151 Uiso 1 1 calc R . . H22C H 1.2179 -0.4518 0.3899 0.151 Uiso 1 1 calc R . . C23 C 1.0967(11) -0.5741(14) 0.3480(7) 0.102(6) Uani 1 1 d . . . H23A H 1.0774 -0.5477 0.3097 0.153 Uiso 1 1 calc R . . H23B H 1.0912 -0.5247 0.3744 0.153 Uiso 1 1 calc R . . H23C H 1.0696 -0.6338 0.3503 0.153 Uiso 1 1 calc R . . C24 C 1.1930(10) -0.6673(10) 0.3225(5) 0.062(4) Uani 1 1 d . . . H24A H 1.1829 -0.6306 0.2869 0.074 Uiso 1 1 calc R . . H24B H 1.1566 -0.7214 0.3149 0.074 Uiso 1 1 calc R . . C25 C 1.2683(13) -0.7132(13) 0.3381(8) 0.109(7) Uani 1 1 d . . . H25A H 1.2698 -0.7562 0.3075 0.163 Uiso 1 1 calc R . . H25B H 1.2788 -0.7520 0.3725 0.163 Uiso 1 1 calc R . . H25C H 1.3052 -0.6610 0.3443 0.163 Uiso 1 1 calc R . . C26 C 1.2740(8) -0.6078(10) 0.4665(6) 0.060(3) Uani 1 1 d . . . H26A H 1.3004 -0.5592 0.4545 0.072 Uiso 1 1 calc R . . C27 C 1.3019(7) -0.6361(9) 0.5231(6) 0.056(3) Uani 1 1 d . . . C28 C 1.3761(12) -0.5949(14) 0.5683(7) 0.101(7) Uani 1 1 d . . . C29 C 1.4206(11) -0.5322(17) 0.5394(9) 0.132(8) Uani 1 1 d . . . H29A H 1.4665 -0.5097 0.5679 0.199 Uiso 1 1 calc R . . H29B H 1.3913 -0.4749 0.5208 0.199 Uiso 1 1 calc R . . H29C H 1.4316 -0.5727 0.5115 0.199 Uiso 1 1 calc R . . C30 C 1.4375(16) -0.6781(19) 0.5941(12) 0.23(2) Uani 1 1 d . . . H30A H 1.4819 -0.6476 0.6205 0.352 Uiso 1 1 calc R . . H30B H 1.4491 -0.7100 0.5637 0.352 Uiso 1 1 calc R . . H30C H 1.4190 -0.7275 0.6139 0.352 Uiso 1 1 calc R . . C31 C 1.3574(11) -0.5441(19) 0.6127(10) 0.140(9) Uani 1 1 d . . . H31A H 1.4035 -0.5232 0.6426 0.167 Uiso 1 1 calc R . . H31B H 1.3325 -0.5915 0.6296 0.167 Uiso 1 1 calc R . . C32 C 1.3079(13) -0.4535(17) 0.5924(12) 0.199(16) Uani 1 1 d . . . H32A H 1.2977 -0.4241 0.6241 0.299 Uiso 1 1 calc R . . H32B H 1.2617 -0.4735 0.5634 0.299 Uiso 1 1 calc R . . H32C H 1.3327 -0.4050 0.5767 0.299 Uiso 1 1 calc R . . C33 C 1.2621(6) -0.7111(8) 0.5401(5) 0.045(3) Uani 1 1 d . . . H33A H 1.2778 -0.7294 0.5786 0.054 Uiso 1 1 calc R . . C34 C 1.1866(5) -0.9425(8) 0.5174(4) 0.033(2) Uani 1 1 d . . . C35 C 1.1341(6) -1.0262(8) 0.5053(5) 0.041(3) Uani 1 1 d . . . C36 C 1.1566(7) -1.1202(8) 0.4912(6) 0.055(3) Uani 1 1 d . . . C37 C 1.1073(7) -1.2124(9) 0.4725(6) 0.064(4) Uani 1 1 d D . . C38 C 1.1248(8) -1.2897(11) 0.5296(10) 0.165(13) Uani 1 1 d D . . H38A H 1.0932 -1.3481 0.5186 0.247 Uiso 1 1 calc R . . H38B H 1.1146 -1.2549 0.5598 0.247 Uiso 1 1 calc R . . H38C H 1.1764 -1.3101 0.5427 0.247 Uiso 1 1 calc R . . C39 C 1.0238(7) -1.1911(10) 0.4519(7) 0.067(4) Uani 1 1 d . . . H39A H 1.0098 -1.1509 0.4177 0.101 Uiso 1 1 calc R . . H39B H 1.0120 -1.1555 0.4812 0.101 Uiso 1 1 calc R . . H39C H 0.9967 -1.2535 0.4437 0.101 Uiso 1 1 calc R . . C40 C 1.1326(19) -1.271(2) 0.4350(18) 0.214(18) Uani 1 1 d . . . H40A H 1.1857 -1.2854 0.4533 0.256 Uiso 1 1 calc R . . H40B H 1.1062 -1.3353 0.4274 0.256 Uiso 1 1 calc R . . C41 C 1.1199(16) -1.2198(17) 0.3821(11) 0.147(12) Uani 1 1 d . . . H41A H 1.1381 -1.2599 0.3578 0.221 Uiso 1 1 calc R . . H41B H 1.1459 -1.1565 0.3897 0.221 Uiso 1 1 calc R . . H41C H 1.0672 -1.2081 0.3635 0.221 Uiso 1 1 calc R . . C42 C 1.2327(8) -1.1300(8) 0.4965(7) 0.073(5) Uani 1 1 d . . . H42A H 1.2482 -1.1932 0.4889 0.088 Uiso 1 1 calc R . . C43 C 1.2871(7) -1.0532(9) 0.5121(6) 0.060(4) Uani 1 1 d . . . C44 C 1.3654(7) -1.0735(10) 0.5202(8) 0.072(5) Uani 1 1 d . . . C45 C 1.4146(15) -0.991(2) 0.5571(11) 0.166(10) Uiso 1 1 d . . . H45A H 1.4030 -0.9281 0.5372 0.249 Uiso 1 1 calc R . . H45B H 1.4663 -1.0074 0.5648 0.249 Uiso 1 1 calc R . . H45C H 1.4057 -0.9864 0.5926 0.249 Uiso 1 1 calc R . . C46 C 1.3804(17) -1.044(2) 0.4649(12) 0.200(13) Uiso 1 1 d . . . H46A H 1.3571 -0.9807 0.4510 0.301 Uiso 1 1 calc R . . H46B H 1.3600 -1.0949 0.4361 0.301 Uiso 1 1 calc R . . H46C H 1.4334 -1.0391 0.4733 0.301 Uiso 1 1 calc R . . C47 C 1.3955(17) -1.166(2) 0.5589(12) 0.177(12) Uiso 1 1 d D . . H47A H 1.4468 -1.1778 0.5617 0.212 Uiso 1 1 calc R . . H47B H 1.3664 -1.2246 0.5403 0.212 Uiso 1 1 calc R . . C48 C 1.393(3) -1.159(3) 0.6231(15) 0.28(2) Uiso 1 1 d D . . H48A H 1.4103 -1.2213 0.6428 0.427 Uiso 1 1 calc R . . H48B H 1.3432 -1.1454 0.6212 0.427 Uiso 1 1 calc R . . H48C H 1.4258 -1.1054 0.6434 0.427 Uiso 1 1 calc R . . C49 C 1.2575(6) -0.9585(9) 0.5202(5) 0.051(3) Uani 1 1 d . . . H49A H 1.2896 -0.9034 0.5280 0.061 Uiso 1 1 calc R . . C50 C 1.0737(7) -0.6128(8) 0.5233(5) 0.047(3) Uani 1 1 d . . . H50A H 1.1205 -0.6203 0.5165 0.056 Uiso 1 1 calc R . . H50B H 1.0787 -0.5577 0.5500 0.056 Uiso 1 1 calc R . . C51 C 1.0088(6) -0.5941(9) 0.4673(5) 0.043(3) Uani 1 1 d . . . H51A H 1.0185 -0.5327 0.4500 0.051 Uiso 1 1 calc R . . H51B H 1.0066 -0.6491 0.4411 0.051 Uiso 1 1 calc R . . C52 C 0.8818(6) -0.6503(8) 0.4513(4) 0.037(2) Uani 1 1 d . . . C53 C 0.8128(6) -0.6384(7) 0.4677(4) 0.038(2) Uani 1 1 d . . . H53A H 0.8270 -0.6275 0.5086 0.046 Uiso 1 1 calc R . . H53B H 0.7829 -0.5817 0.4476 0.046 Uiso 1 1 calc R . . C54 C 0.7042(6) -0.7284(8) 0.4611(5) 0.039(3) Uani 1 1 d . . . H54A H 0.6741 -0.6715 0.4416 0.046 Uiso 1 1 calc R . . H54B H 0.7136 -0.7227 0.5018 0.046 Uiso 1 1 calc R . . C55 C 0.6624(8) -0.8315(9) 0.4366(5) 0.039(3) Uani 1 1 d . . . C56 C 0.5656(7) -0.7871(10) 0.4749(5) 0.056(3) Uani 1 1 d . . . H56A H 0.5953 -0.7250 0.4844 0.067 Uiso 1 1 calc R . . C57 C 0.5738(9) -0.8360(12) 0.5307(6) 0.079(5) Uani 1 1 d . . . H57A H 0.6256 -0.8515 0.5510 0.118 Uiso 1 1 calc R . . H57B H 0.5449 -0.8969 0.5237 0.118 Uiso 1 1 calc R . . H57C H 0.5562 -0.7910 0.5534 0.118 Uiso 1 1 calc R . . C58 C 0.4853(7) -0.7551(12) 0.4388(7) 0.075(4) Uani 1 1 d . . . H58A H 0.4851 -0.7242 0.4039 0.112 Uiso 1 1 calc R . . H58B H 0.4673 -0.7080 0.4601 0.112 Uiso 1 1 calc R . . H58C H 0.4534 -0.8133 0.4297 0.112 Uiso 1 1 calc R . . C59 C 0.5649(6) -0.9518(8) 0.4255(6) 0.046(3) Uani 1 1 d . . . H59A H 0.5222 -0.9539 0.4386 0.055 Uiso 1 1 calc R . . C60 C 0.5320(8) -0.9636(11) 0.3593(6) 0.074(4) Uani 1 1 d . . . H60A H 0.5089 -1.0286 0.3498 0.111 Uiso 1 1 calc R . . H60B H 0.5715 -0.9576 0.3441 0.111 Uiso 1 1 calc R . . H60C H 0.4954 -0.9121 0.3433 0.111 Uiso 1 1 calc R . . C61 C 0.6133(8) -1.0395(11) 0.4526(7) 0.078(5) Uani 1 1 d . . . H61A H 0.5864 -1.1008 0.4387 0.117 Uiso 1 1 calc R . . H61B H 0.6267 -1.0359 0.4935 0.117 Uiso 1 1 calc R . . H61C H 0.6578 -1.0381 0.4431 0.117 Uiso 1 1 calc R . . C62 C 1.1284(7) -0.8697(8) 0.3825(5) 0.050(3) Uani 1 1 d . . . H62A H 1.1647 -0.9092 0.4122 0.060 Uiso 1 1 calc R . . H62B H 1.1474 -0.8589 0.3516 0.060 Uiso 1 1 calc R . . C63 C 1.0550(6) -0.9227(9) 0.3608(5) 0.050(3) Uani 1 1 d . . . H63A H 1.0621 -0.9876 0.3456 0.060 Uiso 1 1 calc R . . H63B H 1.0384 -0.9350 0.3928 0.060 Uiso 1 1 calc R . . C64 C 0.9300(7) -0.8598(8) 0.3200(5) 0.043(3) Uani 1 1 d . . . C65 C 0.8735(6) -0.7979(10) 0.2741(5) 0.052(3) Uani 1 1 d . . . H65A H 0.8957 -0.7345 0.2691 0.062 Uiso 1 1 calc R . . H65B H 0.8576 -0.8338 0.2379 0.062 Uiso 1 1 calc R . . C66 C 0.7511(7) -0.7266(9) 0.2492(5) 0.048(3) Uani 1 1 d . . . H66A H 0.7296 -0.7673 0.2150 0.058 Uiso 1 1 calc R . . H66B H 0.7693 -0.6643 0.2386 0.058 Uiso 1 1 calc R . . C67 C 0.6936(7) -0.7050(9) 0.2754(6) 0.042(3) Uani 1 1 d . . . C68 C 0.5739(8) -0.6297(9) 0.2701(6) 0.051(3) Uani 1 1 d . . . H68A H 0.5341 -0.5938 0.2402 0.062 Uiso 1 1 calc R . . C69 C 0.5393(9) -0.7221(11) 0.2849(7) 0.082(5) Uani 1 1 d . . . H69A H 0.5205 -0.7647 0.2518 0.123 Uiso 1 1 calc R . . H69B H 0.4989 -0.7029 0.2973 0.123 Uiso 1 1 calc R . . H69C H 0.5765 -0.7580 0.3152 0.123 Uiso 1 1 calc R . . C70 C 0.6046(9) -0.5593(10) 0.3194(6) 0.074(5) Uani 1 1 d . . . H70A H 0.6258 -0.5016 0.3077 0.111 Uiso 1 1 calc R . . H70B H 0.6426 -0.5929 0.3502 0.111 Uiso 1 1 calc R . . H70C H 0.5650 -0.5380 0.3322 0.111 Uiso 1 1 calc R . . C71 C 0.6175(8) -0.6239(9) 0.1859(5) 0.054(3) Uani 1 1 d . . . H71A H 0.6589 -0.6488 0.1749 0.064 Uiso 1 1 calc R . . C72 C 0.6208(9) -0.5074(9) 0.1852(6) 0.068(4) Uani 1 1 d . . . H72A H 0.6670 -0.4849 0.2133 0.101 Uiso 1 1 calc R . . H72B H 0.5795 -0.4802 0.1940 0.101 Uiso 1 1 calc R . . H72C H 0.6179 -0.4849 0.1479 0.101 Uiso 1 1 calc R . . C73 C 0.5464(8) -0.6641(9) 0.1428(6) 0.064(4) Uani 1 1 d . . . H73A H 0.5461 -0.7362 0.1452 0.097 Uiso 1 1 calc R . . H73B H 0.5433 -0.6444 0.1050 0.097 Uiso 1 1 calc R . . H73C H 0.5042 -0.6374 0.1506 0.097 Uiso 1 1 calc R . . C74 C 1.0670(6) -1.0295(9) 0.5671(5) 0.049(3) Uani 1 1 d . . . H74A H 1.1078 -0.9939 0.5955 0.059 Uiso 1 1 calc R . . H74B H 1.0743 -1.1011 0.5745 0.059 Uiso 1 1 calc R . . C75 C 0.9950(6) -0.9982(8) 0.5710(5) 0.038(3) Uani 1 1 d . . . H75A H 0.9970 -1.0062 0.6102 0.046 Uiso 1 1 calc R . . H75B H 0.9867 -0.9274 0.5611 0.046 Uiso 1 1 calc R . . C76 C 0.8840(6) -1.0212(8) 0.4850(5) 0.034(3) Uani 1 1 d . . . C77 C 0.8275(7) -1.0990(9) 0.4458(4) 0.052(3) Uani 1 1 d . . . H77A H 0.8534 -1.1587 0.4401 0.063 Uiso 1 1 calc R . . H77B H 0.7905 -1.1186 0.4622 0.063 Uiso 1 1 calc R . . C78 C 0.7457(7) -1.1124(8) 0.3517(4) 0.052(3) Uani 1 1 d . . . H78A H 0.7071 -1.1389 0.3647 0.062 Uiso 1 1 calc R . . H78B H 0.7740 -1.1684 0.3447 0.062 Uiso 1 1 calc R . . C79 C 0.7112(7) -1.0514(8) 0.2978(5) 0.041(3) Uani 1 1 d . . . C80 C 0.6318(8) -1.0332(10) 0.1970(5) 0.058(4) Uani 1 1 d . . . H80A H 0.5994 -1.0805 0.1689 0.069 Uiso 1 1 calc R . . C81 C 0.5804(10) -0.9524(12) 0.2054(6) 0.084(5) Uani 1 1 d . . . H81A H 0.5462 -0.9821 0.2213 0.127 Uiso 1 1 calc R . . H81B H 0.5526 -0.9222 0.1691 0.127 Uiso 1 1 calc R . . H81C H 0.6097 -0.9018 0.2310 0.127 Uiso 1 1 calc R . . C82 C 0.6891(12) -0.9969(10) 0.1719(6) 0.099(7) Uani 1 1 d . . . H82A H 0.7189 -1.0527 0.1681 0.149 Uiso 1 1 calc R . . H82B H 0.7208 -0.9472 0.1968 0.149 Uiso 1 1 calc R . . H82C H 0.6637 -0.9676 0.1349 0.149 Uiso 1 1 calc R . . C83 C 0.6520(10) -1.2032(10) 0.2451(7) 0.084(5) Uani 1 1 d . . . H83A H 0.6841 -1.2333 0.2813 0.100 Uiso 1 1 calc R . . C84 C 0.6725(17) -1.2499(11) 0.1997(9) 0.167(13) Uani 1 1 d . . . H84A H 0.7247 -1.2387 0.2068 0.250 Uiso 1 1 calc R . . H84B H 0.6432 -1.2209 0.1634 0.250 Uiso 1 1 calc R . . H84C H 0.6629 -1.3210 0.1989 0.250 Uiso 1 1 calc R . . C85 C 0.5677(14) -1.2237(16) 0.2401(9) 0.139(9) Uani 1 1 d . . . H85A H 0.5589 -1.1940 0.2723 0.209 Uiso 1 1 calc R . . H85B H 0.5591 -1.2950 0.2398 0.209 Uiso 1 1 calc R . . H85C H 0.5342 -1.1946 0.2053 0.209 Uiso 1 1 calc R . . Ce2 Ce 0.76227(3) -0.65822(5) 0.05730(3) 0.0440(2) Uani 1 1 d . . . N7 N 0.6316(7) -0.7757(8) 0.0599(5) 0.055(3) Uani 1 1 d . . . O13 O 0.6825(5) -0.7576(5) 0.1057(3) 0.0435(19) Uani 1 1 d . . . O14 O 0.6308(5) -0.7437(6) 0.0138(4) 0.060(2) Uani 1 1 d . . . O15 O 0.5768(5) -0.8337(7) 0.0601(4) 0.068(3) Uani 1 1 d . . . N8 N 0.6948(7) -0.6596(8) -0.0713(5) 0.057(3) Uani 1 1 d . . . O16 O 0.7386(6) -0.7256(6) -0.0448(4) 0.065(3) Uani 1 1 d . . . O17 O 0.6848(6) -0.5823(8) -0.0435(4) 0.065(3) Uani 1 1 d . . . O18 O 0.6614(7) -0.6666(7) -0.1240(5) 0.087(3) Uani 1 1 d . . . N9 N 0.6899(7) -0.4625(8) 0.0652(5) 0.061(3) Uani 1 1 d . . . O19 O 0.6554(5) -0.5448(7) 0.0641(4) 0.060(2) Uani 1 1 d . . . O20 O 0.7500(6) -0.4626(5) 0.0573(4) 0.051(2) Uani 1 1 d . . . O21 O 0.6573(7) -0.3810(7) 0.0686(5) 0.088(3) Uani 1 1 d . . . N10 N 0.8577(11) -0.5725(8) 0.1746(6) 0.072(4) Uani 1 1 d . . . O22 O 0.7894(6) -0.5933(6) 0.1612(4) 0.056(3) Uani 1 1 d . . . O23 O 0.8859(5) -0.5850(6) 0.1341(4) 0.062(2) Uani 1 1 d . . . O24 O 0.9024(7) -0.5476(9) 0.2216(5) 0.088(3) Uani 1 1 d . . . N11 N 0.9043(6) -0.6427(8) 0.0269(4) 0.048(3) Uani 1 1 d . . . O25 O 0.8561(5) -0.5726(6) 0.0140(4) 0.047(2) Uani 1 1 d . . . O26 O 0.8880(5) -0.7248(6) 0.0434(4) 0.053(2) Uani 1 1 d . . . O27 O 0.9679(6) -0.6293(7) 0.0213(5) 0.069(3) Uani 1 1 d . . . N12 N 0.8215(7) -0.8648(8) 0.1081(5) 0.057(3) Uani 1 1 d . . . O28 O 0.8398(5) -0.7866(6) 0.1367(4) 0.055(2) Uani 1 1 d . . . O29 O 0.7764(4) -0.8637(5) 0.0578(3) 0.0427(19) Uani 1 1 d . . . O30 O 0.8502(6) -0.9458(7) 0.1309(4) 0.075(3) Uani 1 1 d . . . O31 O 0.8576(6) -1.2800(8) 0.3119(5) 0.091(4) Uani 1 1 d . . . C86 C 0.8109(11) -1.4277(18) 0.3521(14) 0.173(14) Uani 1 1 d . . . C87 C 0.8527(16) -1.3964(14) 0.3163(15) 0.179(13) Uani 1 1 d . . . C88 C 0.9002(12) -1.2448(14) 0.2780(10) 0.113(7) Uani 1 1 d . . . C89 C 0.8925(11) -1.1333(17) 0.2811(9) 0.117(7) Uani 1 1 d . . . O32 O 0.9983(8) -0.8143(14) 0.2068(5) 0.134(5) Uani 1 1 d . . . C90 C 1.0372(11) -0.7418(17) 0.1862(9) 0.115(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0431(4) 0.0228(3) 0.0292(3) -0.0026(3) 0.0164(3) -0.0010(3) O1 0.051(5) 0.038(5) 0.069(6) 0.004(4) 0.022(5) -0.005(4) O2 0.046(5) 0.032(4) 0.054(5) 0.001(4) 0.020(4) 0.005(4) O3 0.030(4) 0.043(4) 0.042(4) -0.001(3) 0.014(3) 0.002(3) O4 0.070(6) 0.022(4) 0.068(6) -0.012(4) 0.044(5) -0.002(4) O5 0.042(5) 0.023(4) 0.055(5) 0.003(3) 0.021(4) -0.008(3) O6 0.042(6) 0.041(5) 0.048(5) -0.005(4) 0.021(4) -0.008(4) O7 0.070(6) 0.024(4) 0.055(5) 0.012(4) 0.025(5) -0.004(4) O8 0.060(6) 0.032(4) 0.039(4) 0.008(4) 0.023(4) 0.001(4) O9 0.064(6) 0.034(5) 0.047(5) 0.010(4) 0.022(5) 0.021(4) O10 0.038(5) 0.038(5) 0.052(5) -0.004(4) 0.014(4) -0.009(4) O11 0.071(6) 0.010(3) 0.055(6) 0.000(3) 0.029(5) -0.003(4) O12 0.071(6) 0.022(4) 0.050(5) -0.009(4) 0.021(5) -0.015(4) N1 0.037(6) 0.022(5) 0.055(6) -0.005(4) 0.017(5) -0.001(4) N2 0.056(8) 0.064(8) 0.047(7) -0.024(6) 0.027(6) -0.026(6) N3 0.019(6) 0.053(7) 0.057(7) 0.018(5) 0.006(5) -0.002(5) N4 0.043(6) 0.025(5) 0.049(6) 0.006(4) 0.017(5) 0.006(4) N5 0.030(5) 0.055(6) 0.036(5) -0.003(5) 0.019(5) -0.002(5) N6 0.096(9) 0.028(5) 0.026(5) -0.008(4) 0.000(6) -0.010(5) C1 0.045(7) 0.029(6) 0.047(6) 0.010(5) 0.016(5) 0.006(5) C2 0.022(6) 0.049(7) 0.065(8) -0.006(6) 0.015(6) -0.006(5) C3 0.062(9) 0.049(7) 0.031(6) -0.014(6) -0.002(6) -0.018(7) C4 0.072(10) 0.061(9) 0.080(10) 0.007(8) 0.045(9) 0.012(8) C5 0.139(17) 0.077(11) 0.080(11) 0.012(9) 0.076(12) 0.027(11) C6 0.091(17) 0.23(3) 0.122(18) -0.003(19) 0.043(14) 0.030(18) C7 0.22(3) 0.111(16) 0.16(2) -0.011(14) 0.16(2) 0.004(16) C8 0.20(3) 0.104(16) 0.19(2) -0.025(16) 0.14(2) 0.023(17) C9 0.24(3) 0.086(14) 0.17(2) 0.000(14) 0.14(2) -0.020(17) C10 0.081(12) 0.069(10) 0.059(9) 0.006(8) 0.030(9) -0.002(9) C11 0.067(10) 0.072(11) 0.067(10) 0.026(8) -0.012(8) -0.012(9) C12 0.083(12) 0.071(10) 0.065(10) 0.011(8) 0.001(9) -0.002(9) C13 0.36(5) 0.31(4) 0.029(10) 0.045(16) 0.009(17) 0.17(3) C14 0.112(19) 0.30(4) 0.106(17) 0.06(2) 0.023(15) 0.06(2) C17 0.048(7) 0.056(7) 0.036(6) 0.011(6) 0.020(6) 0.011(6) C18 0.024(6) 0.043(6) 0.038(6) -0.001(5) 0.006(5) 0.006(5) C19 0.012(5) 0.030(5) 0.054(7) -0.001(5) 0.006(5) 0.003(4) C20 0.073(9) 0.048(7) 0.047(7) 0.001(7) 0.019(7) 0.002(8) C21 0.086(12) 0.048(8) 0.058(9) 0.010(7) 0.015(8) -0.022(8) C22 0.182(19) 0.029(7) 0.097(12) 0.028(8) 0.057(13) -0.014(9) C23 0.129(16) 0.102(14) 0.090(12) 0.061(11) 0.056(12) 0.047(12) C24 0.092(12) 0.057(9) 0.034(7) 0.002(6) 0.019(7) -0.019(8) C25 0.18(2) 0.066(11) 0.108(14) -0.005(10) 0.091(15) -0.005(13) C26 0.070(9) 0.042(7) 0.065(9) 0.012(6) 0.018(8) -0.018(6) C27 0.064(8) 0.041(7) 0.069(9) -0.009(7) 0.030(7) -0.019(7) C28 0.147(18) 0.091(13) 0.065(10) -0.022(10) 0.037(11) -0.076(13) C29 0.101(16) 0.16(2) 0.128(16) -0.066(16) 0.031(13) -0.074(15) C30 0.20(3) 0.15(2) 0.21(3) -0.07(2) -0.11(2) 0.12(2) C31 0.086(15) 0.16(2) 0.16(2) -0.089(19) 0.032(14) -0.010(15) C32 0.129(19) 0.123(19) 0.25(3) -0.11(2) -0.06(2) 0.067(17) C33 0.030(6) 0.047(7) 0.048(7) 0.002(6) 0.000(6) -0.013(6) C34 0.021(6) 0.035(6) 0.045(6) 0.003(5) 0.015(5) -0.003(5) C35 0.037(7) 0.033(6) 0.051(7) 0.001(5) 0.013(6) -0.013(5) C36 0.052(8) 0.028(6) 0.098(10) 0.008(6) 0.041(8) 0.003(5) C37 0.046(8) 0.040(7) 0.123(12) -0.010(8) 0.051(9) -0.005(6) C38 0.023(8) 0.044(9) 0.40(4) 0.066(15) 0.048(14) -0.015(7) C39 0.046(8) 0.045(7) 0.099(11) -0.023(7) 0.010(8) -0.016(6) C40 0.17(3) 0.12(2) 0.39(6) -0.14(3) 0.15(4) -0.08(2) C41 0.14(2) 0.072(16) 0.16(2) -0.030(15) -0.026(19) 0.000(15) C42 0.088(11) 0.019(6) 0.141(14) -0.007(7) 0.074(10) 0.004(7) C43 0.049(8) 0.035(7) 0.107(11) 0.020(7) 0.042(8) 0.012(6) C44 0.034(8) 0.048(8) 0.140(15) 0.006(9) 0.040(9) -0.002(6) C49 0.036(7) 0.041(7) 0.074(9) 0.018(6) 0.018(6) -0.002(6) C50 0.047(8) 0.020(5) 0.078(9) -0.007(6) 0.029(7) -0.008(5) C51 0.044(7) 0.035(6) 0.054(8) -0.007(6) 0.022(6) -0.024(6) C52 0.037(6) 0.039(6) 0.038(6) 0.002(6) 0.017(5) 0.002(6) C53 0.053(7) 0.021(5) 0.043(6) -0.004(5) 0.021(5) -0.008(5) C54 0.037(7) 0.042(6) 0.047(7) 0.002(6) 0.028(6) 0.009(5) C55 0.056(9) 0.027(6) 0.047(8) 0.008(6) 0.033(7) -0.012(6) C56 0.048(8) 0.067(9) 0.058(8) -0.019(7) 0.024(7) -0.021(7) C57 0.088(11) 0.083(11) 0.087(11) -0.012(9) 0.058(10) -0.011(9) C58 0.029(8) 0.083(11) 0.110(13) 0.003(9) 0.020(8) 0.008(7) C59 0.023(6) 0.029(6) 0.093(10) 0.004(6) 0.030(7) -0.008(5) C60 0.064(10) 0.072(10) 0.085(11) -0.022(8) 0.025(8) -0.037(8) C61 0.071(11) 0.065(10) 0.089(11) 0.028(9) 0.018(9) -0.028(9) C62 0.062(8) 0.044(7) 0.046(7) 0.001(6) 0.021(6) 0.003(6) C63 0.032(7) 0.044(7) 0.066(9) 0.003(6) 0.006(6) -0.007(6) C64 0.064(9) 0.026(6) 0.037(6) 0.001(5) 0.015(6) -0.007(6) C65 0.027(7) 0.076(9) 0.056(8) 0.011(7) 0.020(6) 0.003(6) C66 0.053(8) 0.041(7) 0.046(7) 0.020(6) 0.012(6) 0.009(6) C67 0.037(8) 0.042(7) 0.050(8) -0.017(6) 0.020(7) -0.013(6) C68 0.061(9) 0.044(7) 0.065(9) 0.004(6) 0.043(8) 0.014(6) C69 0.089(12) 0.076(10) 0.109(13) 0.015(10) 0.071(11) 0.033(9) C70 0.106(13) 0.049(8) 0.087(11) -0.002(8) 0.058(10) 0.025(8) C71 0.064(9) 0.045(7) 0.056(8) 0.005(6) 0.026(7) 0.016(6) C72 0.092(11) 0.040(7) 0.070(9) 0.008(7) 0.027(8) 0.003(7) C73 0.074(11) 0.043(8) 0.072(10) 0.019(7) 0.020(8) 0.015(7) C74 0.038(7) 0.048(7) 0.053(8) 0.008(6) 0.005(6) -0.003(6) C75 0.023(6) 0.044(7) 0.044(7) 0.003(5) 0.009(5) -0.010(5) C76 0.030(6) 0.035(7) 0.029(6) 0.007(5) 0.000(5) -0.011(5) C77 0.075(10) 0.056(8) 0.020(6) 0.014(5) 0.011(6) 0.024(7) C78 0.069(9) 0.032(6) 0.026(6) -0.010(5) -0.019(6) -0.016(6) C79 0.046(7) 0.028(6) 0.044(7) -0.003(6) 0.010(6) -0.002(5) C80 0.064(9) 0.051(8) 0.042(8) -0.001(6) -0.002(7) 0.017(7) C81 0.113(14) 0.082(11) 0.039(8) -0.001(8) 0.004(9) 0.014(10) C82 0.22(2) 0.031(8) 0.071(10) 0.009(7) 0.080(13) 0.023(10) C83 0.105(14) 0.039(8) 0.083(11) -0.001(8) 0.003(10) -0.030(8) C84 0.39(4) 0.020(8) 0.128(17) -0.015(10) 0.13(2) 0.010(14) C85 0.19(2) 0.110(17) 0.110(16) -0.006(13) 0.042(17) -0.062(17) Ce2 0.0609(6) 0.0275(3) 0.0525(5) 0.0036(3) 0.0310(4) 0.0017(4) N7 0.072(9) 0.050(7) 0.053(7) 0.013(6) 0.033(7) 0.016(6) O13 0.057(6) 0.032(4) 0.044(5) -0.003(4) 0.021(4) -0.013(4) O14 0.066(6) 0.048(5) 0.075(6) 0.011(5) 0.039(5) 0.015(4) O15 0.064(6) 0.064(6) 0.082(6) -0.008(5) 0.033(5) -0.020(5) N8 0.096(9) 0.033(6) 0.050(7) 0.010(6) 0.035(6) 0.003(6) O16 0.107(8) 0.033(5) 0.054(6) 0.010(4) 0.027(6) 0.010(5) O17 0.099(9) 0.065(6) 0.037(5) 0.016(5) 0.032(6) 0.028(6) O18 0.136(10) 0.060(7) 0.069(7) 0.019(6) 0.040(7) 0.027(6) N9 0.069(8) 0.038(6) 0.092(9) 0.008(6) 0.050(7) 0.015(6) O19 0.065(6) 0.045(5) 0.084(7) 0.001(5) 0.043(5) 0.003(5) O20 0.067(7) 0.023(4) 0.083(6) 0.001(4) 0.050(5) 0.001(4) O21 0.134(10) 0.043(5) 0.122(9) 0.032(6) 0.086(8) 0.034(6) N10 0.155(15) 0.021(6) 0.064(9) -0.009(6) 0.070(11) 0.001(7) O22 0.061(6) 0.048(5) 0.082(7) 0.011(5) 0.052(6) 0.015(5) O23 0.084(7) 0.036(5) 0.079(6) -0.019(5) 0.044(6) -0.018(5) O24 0.101(9) 0.087(8) 0.076(8) -0.022(7) 0.032(7) -0.020(7) N11 0.043(7) 0.063(8) 0.047(7) -0.001(6) 0.027(6) 0.009(6) O25 0.057(6) 0.030(4) 0.070(6) 0.021(4) 0.043(5) 0.020(4) O26 0.078(6) 0.025(4) 0.061(5) 0.008(4) 0.031(5) -0.002(4) O27 0.064(7) 0.062(6) 0.097(8) 0.023(6) 0.049(6) 0.013(5) N12 0.090(9) 0.038(7) 0.057(7) 0.022(6) 0.043(7) 0.017(6) O28 0.069(7) 0.038(5) 0.055(6) -0.008(5) 0.020(5) -0.006(5) O29 0.058(5) 0.038(4) 0.036(4) 0.005(4) 0.021(4) -0.008(4) O30 0.090(8) 0.049(6) 0.079(7) 0.022(5) 0.022(6) 0.015(5) O31 0.088(8) 0.063(7) 0.119(9) -0.013(7) 0.034(7) 0.028(6) C86 0.071(14) 0.127(19) 0.31(4) 0.15(2) 0.055(18) 0.022(12) C87 0.16(2) 0.033(10) 0.31(4) -0.033(17) 0.05(3) -0.002(13) C88 0.138(18) 0.072(12) 0.19(2) -0.002(13) 0.131(18) -0.002(11) C89 0.112(15) 0.131(18) 0.133(17) -0.037(14) 0.073(14) -0.022(13) O32 0.111(11) 0.216(17) 0.081(9) 0.033(10) 0.043(8) -0.011(11) C90 0.090(15) 0.134(18) 0.127(17) 0.044(14) 0.046(13) 0.019(13) _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 Ce1 O10 2.403(9) . ? Ce1 O6 2.418(8) . ? Ce1 O7 2.420(9) . ? Ce1 O4 2.426(8) . ? Ce1 O12 2.461(8) . ? Ce1 O9 2.481(8) . ? Ce1 O8 2.547(7) . ? Ce1 O11 2.554(6) . ? Ce1 O5 2.596(7) . ? O1 C3 1.399(14) . ? O1 C50 1.484(13) . ? O2 C19 1.414(12) . ? O2 C62 1.480(13) . ? O3 C35 1.367(13) . ? O3 C74 1.445(13) . ? O4 C52 1.265(12) . ? O5 C54 1.390(11) . ? O5 C53 1.440(11) . ? O6 C55 1.255(15) . ? O7 C64 1.265(13) . ? O8 C65 1.409(12) . ? O8 C66 1.444(12) . ? O9 C67 1.221(14) . ? O10 C76 1.307(13) . ? O11 C78 1.415(12) . ? O11 C77 1.418(12) . ? O12 C79 1.253(13) . ? N1 C52 1.329(13) . ? N1 C51 1.431(14) . ? N2 C55 1.258(16) . ? N2 C56 1.485(16) . ? N2 C59 1.495(14) . ? N3 C64 1.348(16) . ? N3 C63 1.373(14) . ? N4 C67 1.313(15) . ? N4 C71 1.473(14) . ? N4 C68 1.494(14) . ? N5 C76 1.319(13) . ? N5 C75 1.447(13) . ? N6 C79 1.307(14) . ? N6 C80 1.472(15) . ? N6 C83 1.506(16) . ? C1 C34 1.500(14) . ? C1 C18 1.529(14) . ? C1 C2 1.598(15) . ? C2 C17 1.358(15) . ? C2 C3 1.391(17) . ? C3 C4 1.427(17) . ? C4 C10 1.372(19) . ? C4 C5 1.56(2) . ? C5 C6 1.48(3) . ? C5 C7 1.52(2) . ? C5 C8 1.62(3) . ? C8 C9 1.57(3) . ? C10 C11 1.32(2) . ? C11 C17 1.38(2) . ? C11 C12 1.56(2) . ? C12 C14 1.55(3) . ? C12 C15 1.56(3) . ? C12 C13 1.58(3) . ? C15 C16 1.61(3) . ? C18 C33 1.349(14) . ? C18 C19 1.400(14) . ? C19 C20 1.398(16) . ? C20 C26 1.314(18) . ? C20 C21 1.616(18) . ? C21 C24 1.45(2) . ? C21 C23 1.53(2) . ? C21 C22 1.594(18) . ? C24 C25 1.48(2) . ? C26 C27 1.372(18) . ? C27 C33 1.406(15) . ? C27 C28 1.56(2) . ? C28 C31 1.44(2) . ? C28 C29 1.54(2) . ? C28 C30 1.57(3) . ? C31 C32 1.50(3) . ? C34 C49 1.347(14) . ? C34 C35 1.454(14) . ? C35 C36 1.404(15) . ? C36 C42 1.417(18) . ? C36 C37 1.514(17) . ? C37 C40 1.43(3) . ? C37 C39 1.518(17) . ? C37 C38 1.689(16) . ? C40 C41 1.43(4) . ? C42 C43 1.408(18) . ? C43 C49 1.422(16) . ? C43 C44 1.460(17) . ? C44 C45 1.52(3) . ? C44 C47 1.55(3) . ? C44 C46 1.55(3) . ? C47 C48 1.616(19) . ? C50 C51 1.525(16) . ? C52 C53 1.517(14) . ? C54 C55 1.594(16) . ? C56 C57 1.492(19) . ? C56 C58 1.538(17) . ? C59 C61 1.491(18) . ? C59 C60 1.550(18) . ? C62 C63 1.487(16) . ? C64 C65 1.508(16) . ? C66 C67 1.489(16) . ? C68 C70 1.490(18) . ? C68 C69 1.501(18) . ? C71 C73 1.501(18) . ? C71 C72 1.549(16) . ? C74 C75 1.471(15) . ? C76 C77 1.562(16) . ? C78 C79 1.508(15) . ? C80 C82 1.52(2) . ? C80 C81 1.517(19) . ? C83 C84 1.46(2) . ? C83 C85 1.59(3) . ? Ce2 O16 2.582(9) . ? Ce2 O19 2.588(8) . ? Ce2 O22 2.601(9) . ? Ce2 O20 2.609(7) . ? Ce2 O13 2.610(7) . ? Ce2 O14 2.615(9) . ? Ce2 O17 2.625(9) . ? Ce2 O28 2.636(9) . ? Ce2 O23 2.643(9) . ? Ce2 O25 2.650(7) . ? Ce2 O26 2.691(9) . ? Ce2 O29 2.742(7) . ? N7 O14 1.221(12) . ? N7 O13 1.233(13) . ? N7 O15 1.300(13) . ? N8 O16 1.231(13) . ? N8 O18 1.244(14) . ? N8 O17 1.289(13) . ? N9 O20 1.231(13) . ? N9 O21 1.268(12) . ? N9 O19 1.271(13) . ? N10 O24 1.227(16) . ? N10 O22 1.258(17) . ? N10 O23 1.309(13) . ? N11 O26 1.244(12) . ? N11 O25 1.267(12) . ? N11 O27 1.280(14) . ? N12 O28 1.238(13) . ? N12 O29 1.246(13) . ? N12 O30 1.249(12) . ? O31 C88 1.442(19) . ? O31 C87 1.56(2) . ? C86 C87 1.45(4) . ? C88 C89 1.49(3) . ? O32 C90 1.42(2) . ? 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 O10 Ce1 O6 88.6(3) . . ? O10 Ce1 O7 79.1(3) . . ? O6 Ce1 O7 156.4(2) . . ? O10 Ce1 O4 79.0(3) . . ? O6 Ce1 O4 123.5(3) . . ? O7 Ce1 O4 74.1(3) . . ? O10 Ce1 O12 123.7(3) . . ? O6 Ce1 O12 82.3(3) . . ? O7 Ce1 O12 87.8(3) . . ? O4 Ce1 O12 148.2(3) . . ? O10 Ce1 O9 151.9(3) . . ? O6 Ce1 O9 76.7(3) . . ? O7 Ce1 O9 122.2(3) . . ? O4 Ce1 O9 89.2(3) . . ? O12 Ce1 O9 78.5(3) . . ? O10 Ce1 O8 138.1(3) . . ? O6 Ce1 O8 133.3(3) . . ? O7 Ce1 O8 61.7(3) . . ? O4 Ce1 O8 76.6(3) . . ? O12 Ce1 O8 71.9(3) . . ? O9 Ce1 O8 60.6(3) . . ? O10 Ce1 O11 63.1(3) . . ? O6 Ce1 O11 73.7(3) . . ? O7 Ce1 O11 82.8(3) . . ? O4 Ce1 O11 138.7(3) . . ? O12 Ce1 O11 60.9(3) . . ? O9 Ce1 O11 132.1(3) . . ? O8 Ce1 O11 121.3(2) . . ? O10 Ce1 O5 80.8(3) . . ? O6 Ce1 O5 60.9(2) . . ? O7 Ce1 O5 135.1(3) . . ? O4 Ce1 O5 62.8(2) . . ? O12 Ce1 O5 136.3(3) . . ? O9 Ce1 O5 71.1(3) . . ? O8 Ce1 O5 116.0(2) . . ? O11 Ce1 O5 122.0(2) . . ? C3 O1 C50 115.3(9) . . ? C19 O2 C62 116.4(8) . . ? C35 O3 C74 111.5(8) . . ? C52 O4 Ce1 125.8(7) . . ? C54 O5 C53 112.0(8) . . ? C54 O5 Ce1 123.8(6) . . ? C53 O5 Ce1 121.3(5) . . ? C55 O6 Ce1 130.5(8) . . ? C64 O7 Ce1 128.0(8) . . ? C65 O8 C66 113.8(8) . . ? C65 O8 Ce1 123.2(6) . . ? C66 O8 Ce1 122.4(6) . . ? C67 O9 Ce1 127.2(8) . . ? C76 O10 Ce1 125.7(7) . . ? C78 O11 C77 109.9(8) . . ? C78 O11 Ce1 124.6(6) . . ? C77 O11 Ce1 124.7(7) . . ? C79 O12 Ce1 127.7(8) . . ? C52 N1 C51 123.3(9) . . ? C55 N2 C56 124.6(11) . . ? C55 N2 C59 120.5(11) . . ? C56 N2 C59 114.7(10) . . ? C64 N3 C63 122.8(11) . . ? C67 N4 C71 122.3(10) . . ? C67 N4 C68 121.7(10) . . ? C71 N4 C68 115.9(9) . . ? C76 N5 C75 124.0(10) . . ? C79 N6 C80 123.1(10) . . ? C79 N6 C83 121.2(11) . . ? C80 N6 C83 115.7(10) . . ? C34 C1 C18 112.6(9) . . ? C34 C1 C2 110.5(8) . . ? C18 C1 C2 108.7(9) . . ? C17 C2 C3 120.0(11) . . ? C17 C2 C1 121.3(10) . . ? C3 C2 C1 118.7(10) . . ? C2 C3 O1 120.5(10) . . ? C2 C3 C4 119.6(12) . . ? O1 C3 C4 119.7(12) . . ? C10 C4 C3 115.4(12) . . ? C10 C4 C5 120.8(13) . . ? C3 C4 C5 123.0(14) . . ? C6 C5 C7 109.1(17) . . ? C6 C5 C4 113.0(15) . . ? C7 C5 C4 112.7(16) . . ? C6 C5 C8 105.6(19) . . ? C7 C5 C8 103.7(15) . . ? C4 C5 C8 112.2(14) . . ? C9 C8 C5 112.9(19) . . ? C11 C10 C4 125.7(14) . . ? C10 C11 C17 118.2(13) . . ? C10 C11 C12 126.9(16) . . ? C17 C11 C12 114.6(15) . . ? C14 C12 C15 105(2) . . ? C14 C12 C11 111.7(14) . . ? C15 C12 C11 117.7(17) . . ? C14 C12 C13 101.3(19) . . ? C15 C12 C13 113.0(19) . . ? C11 C12 C13 106.8(15) . . ? C12 C15 C16 103(2) . . ? C2 C17 C11 120.8(12) . . ? C33 C18 C19 116.9(10) . . ? C33 C18 C1 122.1(10) . . ? C19 C18 C1 120.9(9) . . ? C20 C19 C18 122.4(10) . . ? C20 C19 O2 120.4(10) . . ? C18 C19 O2 117.2(9) . . ? C26 C20 C19 116.7(11) . . ? C26 C20 C21 121.6(12) . . ? C19 C20 C21 121.8(12) . . ? C24 C21 C23 112.3(14) . . ? C24 C21 C22 106.8(13) . . ? C23 C21 C22 108.4(13) . . ? C24 C21 C20 112.0(12) . . ? C23 C21 C20 109.6(12) . . ? C22 C21 C20 107.6(12) . . ? C21 C24 C25 117.5(13) . . ? C20 C26 C27 124.9(12) . . ? C26 C27 C33 116.7(12) . . ? C26 C27 C28 124.7(12) . . ? C33 C27 C28 118.5(12) . . ? C31 C28 C29 115.6(17) . . ? C31 C28 C27 108.2(17) . . ? C29 C28 C27 111.1(13) . . ? C31 C28 C30 111.4(18) . . ? C29 C28 C30 97(2) . . ? C27 C28 C30 113.8(15) . . ? C28 C31 C32 114(2) . . ? C18 C33 C27 122.1(11) . . ? C49 C34 C35 119.7(10) . . ? C49 C34 C1 121.3(9) . . ? C35 C34 C1 118.8(9) . . ? O3 C35 C36 124.9(9) . . ? O3 C35 C34 116.1(9) . . ? C36 C35 C34 118.9(10) . . ? C35 C36 C42 116.9(11) . . ? C35 C36 C37 125.8(11) . . ? C42 C36 C37 117.3(10) . . ? C40 C37 C36 109.2(14) . . ? C40 C37 C39 115.9(19) . . ? C36 C37 C39 114.7(10) . . ? C40 C37 C38 102(2) . . ? C36 C37 C38 108.4(11) . . ? C39 C37 C38 105.7(10) . . ? C41 C40 C37 111(3) . . ? C43 C42 C36 126.1(10) . . ? C42 C43 C49 113.0(11) . . ? C42 C43 C44 121.5(11) . . ? C49 C43 C44 125.5(12) . . ? C43 C44 C45 109.6(15) . . ? C43 C44 C47 111.7(15) . . ? C45 C44 C47 100.4(18) . . ? C43 C44 C46 109.4(17) . . ? C45 C44 C46 95.1(17) . . ? C47 C44 C46 127.6(19) . . ? C44 C47 C48 116(3) . . ? C34 C49 C43 125.0(11) . . ? O1 C50 C51 104.3(9) . . ? N1 C51 C50 113.8(9) . . ? O4 C52 N1 120.6(9) . . ? O4 C52 C53 122.1(10) . . ? N1 C52 C53 117.3(9) . . ? O5 C53 C52 105.8(8) . . ? O5 C54 C55 106.2(8) . . ? O6 C55 N2 124.4(12) . . ? O6 C55 C54 116.1(10) . . ? N2 C55 C54 119.5(11) . . ? N2 C56 C57 108.2(11) . . ? N2 C56 C58 114.3(11) . . ? C57 C56 C58 114.9(12) . . ? C61 C59 N2 113.4(11) . . ? C61 C59 C60 110.9(12) . . ? N2 C59 C60 113.0(10) . . ? O2 C62 C63 106.6(9) . . ? N3 C63 C62 114.4(10) . . ? O7 C64 N3 123.1(11) . . ? O7 C64 C65 117.3(11) . . ? N3 C64 C65 119.6(10) . . ? O8 C65 C64 108.1(9) . . ? O8 C66 C67 107.5(9) . . ? O9 C67 N4 121.5(11) . . ? O9 C67 C66 119.1(12) . . ? N4 C67 C66 119.3(11) . . ? C70 C68 N4 111.4(11) . . ? C70 C68 C69 112.9(12) . . ? N4 C68 C69 110.7(9) . . ? N4 C71 C73 114.4(11) . . ? N4 C71 C72 108.7(10) . . ? C73 C71 C72 112.2(11) . . ? O3 C74 C75 108.6(9) . . ? N5 C75 C74 112.0(9) . . ? O10 C76 N5 123.0(10) . . ? O10 C76 C77 120.3(9) . . ? N5 C76 C77 116.7(9) . . ? O11 C77 C76 104.1(9) . . ? O11 C78 C79 106.7(9) . . ? O12 C79 N6 118.5(11) . . ? O12 C79 C78 119.3(10) . . ? N6 C79 C78 122.2(10) . . ? N6 C80 C82 111.1(12) . . ? N6 C80 C81 111.7(11) . . ? C82 C80 C81 115.3(12) . . ? C84 C83 N6 112.1(14) . . ? C84 C83 C85 113.9(17) . . ? N6 C83 C85 110.0(15) . . ? O16 Ce2 O19 113.4(3) . . ? O16 Ce2 O22 178.5(3) . . ? O19 Ce2 O22 68.1(3) . . ? O16 Ce2 O20 111.1(3) . . ? O19 Ce2 O20 49.3(3) . . ? O22 Ce2 O20 69.9(3) . . ? O16 Ce2 O13 110.6(3) . . ? O19 Ce2 O13 70.3(3) . . ? O22 Ce2 O13 69.6(3) . . ? O20 Ce2 O13 115.9(2) . . ? O16 Ce2 O14 68.4(3) . . ? O19 Ce2 O14 67.5(3) . . ? O22 Ce2 O14 112.4(3) . . ? O20 Ce2 O14 111.1(3) . . ? O13 Ce2 O14 48.8(3) . . ? O16 Ce2 O17 49.2(3) . . ? O19 Ce2 O17 69.4(3) . . ? O22 Ce2 O17 132.2(3) . . ? O20 Ce2 O17 66.2(3) . . ? O13 Ce2 O17 114.4(3) . . ? O14 Ce2 O17 68.7(3) . . ? O16 Ce2 O28 111.9(3) . . ? O19 Ce2 O28 125.0(3) . . ? O22 Ce2 O28 66.7(3) . . ? O20 Ce2 O28 132.2(3) . . ? O13 Ce2 O28 65.8(3) . . ? O14 Ce2 O28 103.4(3) . . ? O17 Ce2 O28 160.8(3) . . ? O16 Ce2 O23 130.0(3) . . ? O19 Ce2 O23 105.1(3) . . ? O22 Ce2 O23 49.0(3) . . ? O20 Ce2 O23 72.0(3) . . ? O13 Ce2 O23 111.6(3) . . ? O14 Ce2 O23 160.1(3) . . ? O17 Ce2 O23 127.5(3) . . ? O28 Ce2 O23 64.7(3) . . ? O16 Ce2 O25 69.9(3) . . ? O19 Ce2 O25 115.9(3) . . ? O22 Ce2 O25 109.7(3) . . ? O20 Ce2 O25 69.2(2) . . ? O13 Ce2 O25 173.2(3) . . ? O14 Ce2 O25 134.8(3) . . ? O17 Ce2 O25 71.2(3) . . ? O28 Ce2 O25 107.6(3) . . ? O23 Ce2 O25 65.1(3) . . ? O16 Ce2 O26 67.2(3) . . ? O19 Ce2 O26 163.4(3) . . ? O22 Ce2 O26 111.3(3) . . ? O20 Ce2 O26 114.3(3) . . ? O13 Ce2 O26 125.8(2) . . ? O14 Ce2 O26 124.9(3) . . ? O17 Ce2 O26 103.2(3) . . ? O28 Ce2 O26 66.1(3) . . ? O23 Ce2 O26 66.8(3) . . ? O25 Ce2 O26 47.8(2) . . ? O16 Ce2 O29 69.0(2) . . ? O19 Ce2 O29 131.1(2) . . ? O22 Ce2 O29 109.9(2) . . ? O20 Ce2 O29 179.5(3) . . ? O13 Ce2 O29 64.3(2) . . ? O14 Ce2 O29 69.4(2) . . ? O17 Ce2 O29 114.1(3) . . ? O28 Ce2 O29 47.5(2) . . ? O23 Ce2 O29 107.6(3) . . ? O25 Ce2 O29 110.4(2) . . ? O26 Ce2 O29 65.3(2) . . ? O14 N7 O13 123.3(12) . . ? O14 N7 O15 117.8(12) . . ? O13 N7 O15 118.9(10) . . ? O14 N7 Ce2 61.8(7) . . ? O13 N7 Ce2 61.6(6) . . ? O15 N7 Ce2 175.4(8) . . ? N7 O13 Ce2 93.8(7) . . ? N7 O14 Ce2 93.9(8) . . ? O16 N8 O18 120.7(11) . . ? O16 N8 O17 118.6(11) . . ? O18 N8 O17 120.7(11) . . ? O16 N8 Ce2 58.4(6) . . ? O18 N8 Ce2 173.6(9) . . ? O17 N8 Ce2 60.7(6) . . ? N8 O16 Ce2 97.6(7) . . ? N8 O17 Ce2 94.0(7) . . ? O20 N9 O21 121.3(11) . . ? O20 N9 O19 120.1(9) . . ? O21 N9 O19 118.2(11) . . ? O20 N9 Ce2 60.7(5) . . ? O21 N9 Ce2 178.1(9) . . ? O19 N9 Ce2 59.8(5) . . ? N9 O19 Ce2 95.0(6) . . ? N9 O20 Ce2 95.1(6) . . ? O24 N10 O22 128.3(12) . . ? O24 N10 O23 115.7(16) . . ? O22 N10 O23 115.9(13) . . ? N10 O22 Ce2 99.2(7) . . ? N10 O23 Ce2 95.8(9) . . ? O26 N11 O25 118.9(10) . . ? O26 N11 O27 121.0(10) . . ? O25 N11 O27 120.1(10) . . ? N11 O25 Ce2 96.7(6) . . ? N11 O26 Ce2 95.3(7) . . ? O28 N12 O29 121.6(10) . . ? O28 N12 O30 118.1(12) . . ? O29 N12 O30 120.3(12) . . ? N12 O28 Ce2 98.1(7) . . ? N12 O29 Ce2 92.8(6) . . ? C88 O31 C87 115.0(16) . . ? C86 C87 O31 113(2) . . ? O31 C88 C89 101.9(13) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.356 _refine_diff_density_min -2.257 _refine_diff_density_rms 0.120 #===END data_Ybtrisdiamide _database_code_depnum_ccdc_archive 'CCDC 280075' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 7, Yb - tris diamide' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H96 N9 O18 Yb' _chemical_formula_weight 1260.38 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 tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 16.9828(7) _cell_length_b 16.9828(7) _cell_length_c 24.3051(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7010.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measurd' _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2644 _exptl_absorpt_coefficient_mu 1.396 _exptl_absorpt_correction_type 'Corrected by SADABS' _exptl_absorpt_correction_T_min 0.818915 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Corrected by SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Siemens Smart CCD' _diffrn_measurement_method scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38856 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6165 _reflns_number_gt 4059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART' _computing_cell_refinement 'Bruker AXS SMART' _computing_data_reduction 'Bruker AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'Microsoft Word' _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. Two of the nitrate anions were severly disordered ; _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^)+(0.0719P)^2^+33.3107P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6165 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1993 _refine_ls_wR_factor_gt 0.1737 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 0.2500 0.7500 0.622542(19) 0.0496(2) Uani 1 2 d S . . O1 O 0.2500 0.7500 0.7228(3) 0.071(3) Uani 1 2 d S . . O2 O 0.3695(4) 0.7576(7) 0.6651(3) 0.062(2) Uani 1 1 d . . . O3 O 0.3258(6) 0.8084(5) 0.5542(3) 0.059(2) Uani 1 1 d . . . O4 O 0.3372(5) 0.6664(6) 0.5697(3) 0.063(2) Uani 1 1 d . . . O5 O 0.2555(7) 0.6176(5) 0.6496(3) 0.061(2) Uani 1 1 d . . . N1 N 0.4605(7) 0.7538(10) 0.7323(4) 0.083(3) Uani 1 1 d . . . N2 N 0.4210(8) 0.8240(8) 0.4932(5) 0.084(4) Uani 1 1 d . . . N3 N 0.2821(7) 0.4897(7) 0.6453(5) 0.074(3) Uani 1 1 d . . . C1 C 0.3181(6) 0.7560(10) 0.7558(4) 0.070(4) Uani 1 1 d . . . H1A H 0.3216 0.7120 0.7811 0.083 Uiso 1 1 calc R . . H1B H 0.3178 0.8046 0.7767 0.083 Uiso 1 1 calc R . . C2 C 0.3872(7) 0.7548(9) 0.7145(5) 0.060(3) Uani 1 1 d . . . C3 C 0.5279(8) 0.7495(17) 0.6939(7) 0.106(6) Uani 1 1 d . . . H3A H 0.5756 0.7462 0.7165 0.128 Uiso 1 1 calc R . . C4 C 0.5354(13) 0.8317(16) 0.6565(10) 0.157(12) Uani 1 1 d . . . H4A H 0.5805 0.8281 0.6329 0.236 Uiso 1 1 calc R . . H4B H 0.5412 0.8762 0.6806 0.236 Uiso 1 1 calc R . . H4C H 0.4887 0.8382 0.6347 0.236 Uiso 1 1 calc R . . C5 C 0.5245(11) 0.6784(13) 0.6617(9) 0.117(8) Uani 1 1 d . . . H5A H 0.5272 0.6335 0.6856 0.175 Uiso 1 1 calc R . . H5B H 0.5681 0.6772 0.6365 0.175 Uiso 1 1 calc R . . H5C H 0.4760 0.6770 0.6414 0.175 Uiso 1 1 calc R . . C6 C 0.4766(9) 0.7519(16) 0.7936(6) 0.108(6) Uani 1 1 d . . . H6A H 0.4263 0.7581 0.8128 0.129 Uiso 1 1 calc R . . C7 C 0.5285(14) 0.8219(15) 0.8082(9) 0.150(10) Uani 1 1 d . . . H7A H 0.5027 0.8697 0.7974 0.225 Uiso 1 1 calc R . . H7B H 0.5779 0.8175 0.7894 0.225 Uiso 1 1 calc R . . H7C H 0.5374 0.8226 0.8472 0.225 Uiso 1 1 calc R . . C8 C 0.5144(13) 0.6724(16) 0.8125(9) 0.142(9) Uani 1 1 d . . . H8A H 0.4754 0.6315 0.8113 0.213 Uiso 1 1 calc R . . H8B H 0.5339 0.6778 0.8494 0.213 Uiso 1 1 calc R . . H8C H 0.5571 0.6591 0.7883 0.213 Uiso 1 1 calc R . . C9 C 0.3758(8) 0.7803(9) 0.5271(6) 0.068(4) Uani 1 1 d . . . C10 C 0.3886(9) 0.6904(8) 0.5274(5) 0.077(5) Uani 1 1 d . . . H10A H 0.3742 0.6670 0.4924 0.092 Uiso 1 1 calc R . . H10B H 0.4428 0.6770 0.5358 0.092 Uiso 1 1 calc R . . C11 C 0.3397(7) 0.5829(8) 0.5754(5) 0.064(3) Uani 1 1 d . . . H11A H 0.3934 0.5651 0.5810 0.076 Uiso 1 1 calc R . . H11B H 0.3188 0.5576 0.5427 0.076 Uiso 1 1 calc R . . C12 C 0.2878(8) 0.5631(9) 0.6267(5) 0.064(3) Uani 1 1 d . . . C13 C 0.2389(10) 0.4714(11) 0.6968(6) 0.086(5) Uani 1 1 d . . . H13A H 0.2424 0.4143 0.7021 0.104 Uiso 1 1 calc R . . C14 C 0.1569(11) 0.4897(11) 0.6908(7) 0.104(6) Uani 1 1 d . . . H14A H 0.1408 0.4798 0.6536 0.156 Uiso 1 1 calc R . . H14B H 0.1484 0.5442 0.6995 0.156 Uiso 1 1 calc R . . H14C H 0.1266 0.4575 0.7154 0.156 Uiso 1 1 calc R . . C15 C 0.2738(11) 0.5078(10) 0.7458(6) 0.107(7) Uani 1 1 d . . . H15A H 0.2467 0.4896 0.7781 0.160 Uiso 1 1 calc R . . H15B H 0.2692 0.5640 0.7433 0.160 Uiso 1 1 calc R . . H15C H 0.3284 0.4936 0.7482 0.160 Uiso 1 1 calc R . . C16 C 0.3242(11) 0.4213(10) 0.6141(8) 0.098(5) Uani 1 1 d . . . H16A H 0.3495 0.4427 0.5811 0.117 Uiso 1 1 calc R . . C17 C 0.2690(12) 0.3613(10) 0.5979(8) 0.116(6) Uani 1 1 d . . . H17A H 0.2956 0.3223 0.5762 0.175 Uiso 1 1 calc R . . H17B H 0.2275 0.3847 0.5766 0.175 Uiso 1 1 calc R . . H17C H 0.2471 0.3370 0.6301 0.175 Uiso 1 1 calc R . . C18 C 0.3867(13) 0.3872(11) 0.6512(11) 0.137(8) Uani 1 1 d . . . H18A H 0.4301 0.3690 0.6293 0.206 Uiso 1 1 calc R . . H18B H 0.3650 0.3438 0.6715 0.206 Uiso 1 1 calc R . . H18C H 0.4046 0.4269 0.6763 0.206 Uiso 1 1 calc R . . C19 C 0.4081(10) 0.9137(12) 0.4913(6) 0.092(5) Uani 1 1 d . . . H19A H 0.4485 0.9353 0.4668 0.110 Uiso 1 1 calc R . . C20 C 0.3290(13) 0.9347(14) 0.4663(8) 0.144(9) Uani 1 1 d . . . H20A H 0.2989 0.9647 0.4923 0.215 Uiso 1 1 calc R . . H20B H 0.3010 0.8873 0.4572 0.215 Uiso 1 1 calc R . . H20C H 0.3371 0.9653 0.4336 0.215 Uiso 1 1 calc R . . C21 C 0.4245(11) 0.9462(10) 0.5483(8) 0.114(7) Uani 1 1 d . . . H21A H 0.4698 0.9202 0.5636 0.171 Uiso 1 1 calc R . . H21B H 0.3797 0.9372 0.5715 0.171 Uiso 1 1 calc R . . H21C H 0.4345 1.0017 0.5458 0.171 Uiso 1 1 calc R . . C22 C 0.4839(15) 0.7899(13) 0.4582(9) 0.159(12) Uani 1 1 d . . . H22A H 0.4771 0.7326 0.4586 0.190 Uiso 1 1 calc R . . C23 C 0.473(2) 0.8180(14) 0.3964(8) 0.205(16) Uani 1 1 d . . . H23A H 0.4424 0.7800 0.3766 0.307 Uiso 1 1 calc R . . H23B H 0.5241 0.8228 0.3794 0.307 Uiso 1 1 calc R . . H23C H 0.4472 0.8681 0.3958 0.307 Uiso 1 1 calc R . . C24 C 0.5617(15) 0.8067(13) 0.4801(12) 0.176(14) Uani 1 1 d . . . H24A H 0.5569 0.8397 0.5120 0.265 Uiso 1 1 calc R . . H24B H 0.5925 0.8333 0.4527 0.265 Uiso 1 1 calc R . . H24C H 0.5871 0.7583 0.4901 0.265 Uiso 1 1 calc R . . O6 O 0.2500 0.7500 0.4443(12) 0.193(9) Uiso 1 2 d S . . N25 N 0.2367(17) 0.7895(15) 0.4008(12) 0.097(8) Uiso 0.50 1 d P . . O6C O 0.299(2) 0.781(2) 0.3745(12) 0.171(13) Uiso 0.50 1 d P . . O6B O 0.182(2) 0.829(3) 0.3878(14) 0.176(13) Uiso 0.50 1 d P . . N4 N 0.919(2) 0.945(2) 0.5370(15) 0.123(11) Uiso 0.50 1 d P . . O7 O 0.843(2) 0.952(2) 0.5391(15) 0.176(14) Uiso 0.50 1 d P . . O8 O 0.951(3) 1.000(3) 0.5598(19) 0.25(2) Uiso 0.50 1 d P . . O9 O 0.9413(15) 0.9042(16) 0.5045(12) 0.124(9) Uiso 0.50 1 d P . . N5 N 0.7500 0.7500 0.7500 0.110(10) Uiso 1 4 d S . . O10 O 0.772(3) 0.782(2) 0.7081(18) 0.153(17) Uiso 0.38 1 d P . . O10B O 0.702(3) 0.792(3) 0.7309(17) 0.145(16) Uiso 0.38 1 d P . . N6 N 0.2500 1.2500 0.7500 0.079(7) Uiso 1 4 d S . . O11 O 0.241(3) 1.1892(17) 0.7760(12) 0.085(9) Uiso 0.38 1 d P . . O11B O 0.206(2) 1.193(2) 0.7677(13) 0.083(10) Uiso 0.38 1 d P . . 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 0.0516(5) 0.0627(5) 0.0346(3) 0.000 0.000 -0.0227(3) O1 0.033(6) 0.137(11) 0.044(5) 0.000 0.000 -0.018(6) O2 0.043(4) 0.095(7) 0.049(4) -0.013(6) -0.001(3) -0.014(5) O3 0.088(7) 0.047(5) 0.042(4) 0.014(4) 0.012(5) -0.018(4) O4 0.045(6) 0.089(8) 0.056(4) 0.013(5) 0.014(4) -0.025(4) O5 0.067(6) 0.072(6) 0.044(4) 0.005(4) -0.001(6) -0.027(6) N1 0.073(7) 0.113(9) 0.063(6) -0.029(9) -0.033(6) 0.003(8) N2 0.088(9) 0.096(10) 0.067(7) -0.021(7) 0.036(7) -0.018(7) N3 0.071(7) 0.053(7) 0.097(8) 0.011(6) -0.026(7) -0.018(6) C1 0.056(7) 0.108(11) 0.044(6) -0.023(8) -0.014(5) -0.001(7) C2 0.052(6) 0.060(7) 0.067(7) 0.022(8) -0.006(5) 0.001(6) C3 0.036(7) 0.19(2) 0.091(11) -0.010(18) -0.021(7) -0.034(13) C4 0.098(16) 0.24(3) 0.135(19) 0.09(2) -0.017(15) -0.048(17) C5 0.088(14) 0.146(19) 0.117(17) 0.053(14) 0.032(12) 0.058(13) C6 0.069(9) 0.185(19) 0.069(8) -0.029(15) -0.012(7) -0.020(13) C7 0.137(19) 0.20(3) 0.110(16) -0.083(17) -0.060(14) 0.021(17) C8 0.111(18) 0.21(3) 0.109(17) 0.017(17) -0.024(14) 0.021(17) C9 0.065(9) 0.083(10) 0.054(8) 0.013(7) 0.013(7) -0.016(7) C10 0.097(11) 0.085(11) 0.049(8) -0.037(7) 0.037(7) -0.038(8) C11 0.057(8) 0.078(9) 0.056(7) 0.000(7) 0.009(6) -0.024(7) C12 0.055(7) 0.072(9) 0.064(8) 0.022(7) -0.010(6) -0.012(6) C13 0.059(10) 0.133(14) 0.067(9) 0.015(9) -0.010(9) -0.026(10) C14 0.140(17) 0.100(13) 0.074(11) 0.027(9) 0.034(11) -0.024(12) C15 0.141(19) 0.104(12) 0.075(10) 0.048(9) -0.014(10) -0.031(12) C16 0.109(14) 0.061(10) 0.123(14) 0.008(10) -0.001(12) -0.009(9) C17 0.115(16) 0.086(11) 0.149(16) -0.019(12) -0.001(13) -0.013(11) C18 0.122(17) 0.086(13) 0.20(2) 0.001(15) -0.017(17) 0.023(12) C19 0.056(10) 0.127(17) 0.092(10) 0.023(12) 0.047(10) -0.028(7) C20 0.144(19) 0.18(2) 0.103(14) 0.109(15) -0.009(14) -0.031(16) C21 0.131(17) 0.067(11) 0.143(16) 0.000(11) 0.043(13) -0.034(11) C22 0.19(2) 0.126(17) 0.156(19) -0.038(14) 0.152(19) -0.053(16) C23 0.37(4) 0.15(2) 0.097(14) -0.012(15) 0.15(2) -0.07(2) C24 0.16(2) 0.094(15) 0.28(3) 0.040(18) 0.14(2) 0.009(15) _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 2.282(7) . ? Yb1 O2 2.282(7) 2_565 ? Yb1 O3 2.324(7) 2_565 ? Yb1 O3 2.324(7) . ? Yb1 O5 2.344(9) 2_565 ? Yb1 O5 2.344(9) . ? Yb1 O4 2.421(8) . ? Yb1 O4 2.421(8) 2_565 ? Yb1 O1 2.436(8) . ? Yb1 C9 3.195(14) 2_565 ? Yb1 C9 3.195(14) . ? O1 C1 1.412(11) . ? O1 C1 1.412(11) 2_565 ? O2 C2 1.239(12) . ? O3 C9 1.176(16) . ? O4 C10 1.409(13) . ? O4 C11 1.425(16) . ? O5 C12 1.211(16) . ? N1 C2 1.317(14) . ? N1 C3 1.478(18) . ? N1 C6 1.514(16) . ? N2 C9 1.348(16) . ? N2 C22 1.48(2) . ? N2 C19 1.54(2) . ? N3 C12 1.331(17) . ? N3 C13 1.483(18) . ? N3 C16 1.56(2) . ? C1 C2 1.544(15) . ? C3 C5 1.44(3) . ? C3 C4 1.67(3) . ? C6 C7 1.52(3) . ? C6 C8 1.56(3) . ? C9 C10 1.54(2) . ? C11 C12 1.564(16) . ? C13 C14 1.44(2) . ? C13 C15 1.47(2) . ? C16 C17 1.44(2) . ? C16 C18 1.51(3) . ? C19 C21 1.52(2) . ? C19 C20 1.52(2) . ? C22 C24 1.45(3) . ? C22 C23 1.59(3) . ? O6 N25 1.27(3) 2_565 ? O6 N25 1.27(3) . ? N25 O6B 1.18(4) . ? N25 O6C 1.24(4) . ? N25 N25 1.41(5) 2_565 ? N25 O6C 1.49(4) 2_565 ? O6C N25 1.49(4) 2_565 ? N4 O9 1.12(4) . ? N4 O8 1.22(5) . ? N4 O7 1.29(4) . ? N5 O10B 1.18(4) 7_577 ? N5 O10B 1.18(4) 2_665 ? N5 O10B 1.18(4) . ? N5 O10B 1.18(4) 8_757 ? N5 O10 1.22(4) 7_577 ? N5 O10 1.22(4) 2_665 ? N5 O10 1.22(4) . ? N5 O10 1.22(4) 8_757 ? O10 O10B 1.33(5) . ? O10 O10 1.34(8) 2_665 ? O10 O10B 1.45(5) 2_665 ? O10 O10B 1.54(5) 7_577 ? O10B O10 1.45(5) 2_665 ? O10B O10 1.54(5) 8_757 ? O10B O10B 1.79(7) 7_577 ? O10B O10B 1.79(7) 8_757 ? N6 O11 1.22(3) 8_767 ? N6 O11 1.22(3) 2_575 ? N6 O11 1.22(3) . ? N6 O11 1.22(3) 7_477 ? N6 O11B 1.30(3) 2_575 ? N6 O11B 1.30(3) 8_767 ? N6 O11B 1.30(3) . ? N6 O11B 1.30(3) 7_477 ? O11 O11B 0.63(5) . ? O11 O11B 1.57(4) 8_767 ? O11B O11 1.57(4) 7_477 ? 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 O2 126.1(4) . 2_565 ? O2 Yb1 O3 147.3(4) . 2_565 ? O2 Yb1 O3 78.9(3) 2_565 2_565 ? O2 Yb1 O3 78.9(3) . . ? O2 Yb1 O3 147.3(4) 2_565 . ? O3 Yb1 O3 88.7(4) 2_565 . ? O2 Yb1 O5 81.6(3) . 2_565 ? O2 Yb1 O5 83.8(3) 2_565 2_565 ? O3 Yb1 O5 126.0(4) 2_565 2_565 ? O3 Yb1 O5 79.2(3) . 2_565 ? O2 Yb1 O5 83.8(3) . . ? O2 Yb1 O5 81.6(3) 2_565 . ? O3 Yb1 O5 79.2(3) 2_565 . ? O3 Yb1 O5 126.0(4) . . ? O5 Yb1 O5 147.4(4) 2_565 . ? O2 Yb1 O4 74.3(3) . . ? O2 Yb1 O4 138.7(4) 2_565 . ? O3 Yb1 O4 73.1(3) 2_565 . ? O3 Yb1 O4 62.1(3) . . ? O5 Yb1 O4 137.4(4) 2_565 . ? O5 Yb1 O4 64.0(3) . . ? O2 Yb1 O4 138.7(4) . 2_565 ? O2 Yb1 O4 74.3(3) 2_565 2_565 ? O3 Yb1 O4 62.1(3) 2_565 2_565 ? O3 Yb1 O4 73.1(3) . 2_565 ? O5 Yb1 O4 64.0(3) 2_565 2_565 ? O5 Yb1 O4 137.4(4) . 2_565 ? O4 Yb1 O4 115.9(3) . 2_565 ? O2 Yb1 O1 63.03(18) . . ? O2 Yb1 O1 63.03(18) 2_565 . ? O3 Yb1 O1 135.64(19) 2_565 . ? O3 Yb1 O1 135.64(19) . . ? O5 Yb1 O1 73.72(18) 2_565 . ? O5 Yb1 O1 73.72(18) . . ? O4 Yb1 O1 122.04(17) . . ? O4 Yb1 O1 122.04(17) 2_565 . ? O2 Yb1 C9 158.9(3) . 2_565 ? O2 Yb1 C9 74.1(3) 2_565 2_565 ? O3 Yb1 C9 16.6(4) 2_565 2_565 ? O3 Yb1 C9 85.4(3) . 2_565 ? O5 Yb1 C9 109.3(4) 2_565 2_565 ? O5 Yb1 C9 94.3(4) . 2_565 ? O4 Yb1 C9 86.0(3) . 2_565 ? O4 Yb1 C9 45.6(4) 2_565 2_565 ? O1 Yb1 C9 136.5(2) . 2_565 ? O2 Yb1 C9 74.1(3) . . ? O2 Yb1 C9 158.9(3) 2_565 . ? O3 Yb1 C9 85.4(3) 2_565 . ? O3 Yb1 C9 16.6(4) . . ? O5 Yb1 C9 94.3(4) 2_565 . ? O5 Yb1 C9 109.3(4) . . ? O4 Yb1 C9 45.6(4) . . ? O4 Yb1 C9 86.0(3) 2_565 . ? O1 Yb1 C9 136.5(2) . . ? C9 Yb1 C9 86.9(5) 2_565 . ? C1 O1 C1 110.7(11) . 2_565 ? C1 O1 Yb1 124.7(5) . . ? C1 O1 Yb1 124.7(5) 2_565 . ? C2 O2 Yb1 130.8(7) . . ? C9 O3 Yb1 128.9(9) . . ? C10 O4 C11 109.9(9) . . ? C10 O4 Yb1 126.6(9) . . ? C11 O4 Yb1 123.4(7) . . ? C12 O5 Yb1 128.5(8) . . ? C2 N1 C3 121.7(10) . . ? C2 N1 C6 119.6(11) . . ? C3 N1 C6 118.6(11) . . ? C9 N2 C22 123.1(15) . . ? C9 N2 C19 118.8(12) . . ? C22 N2 C19 118.1(13) . . ? C12 N3 C13 121.3(14) . . ? C12 N3 C16 119.9(13) . . ? C13 N3 C16 118.7(13) . . ? O1 C1 C2 104.6(8) . . ? O2 C2 N1 123.2(11) . . ? O2 C2 C1 116.4(9) . . ? N1 C2 C1 120.3(10) . . ? C5 C3 N1 110.7(17) . . ? C5 C3 C4 114.0(15) . . ? N1 C3 C4 111(2) . . ? N1 C6 C7 108.6(17) . . ? N1 C6 C8 112.4(17) . . ? C7 C6 C8 111.6(14) . . ? O3 C9 N2 122.0(14) . . ? O3 C9 C10 120.0(11) . . ? N2 C9 C10 117.9(14) . . ? O3 C9 Yb1 34.5(6) . . ? N2 C9 Yb1 155.9(11) . . ? C10 C9 Yb1 86.1(7) . . ? O4 C10 C9 101.7(11) . . ? O4 C11 C12 105.9(10) . . ? O5 C12 N3 121.8(13) . . ? O5 C12 C11 117.2(12) . . ? N3 C12 C11 120.9(14) . . ? C14 C13 C15 112.5(17) . . ? C14 C13 N3 110.4(13) . . ? C15 C13 N3 113.4(13) . . ? C17 C16 C18 110.5(16) . . ? C17 C16 N3 111.2(15) . . ? C18 C16 N3 108.6(16) . . ? C21 C19 C20 116.3(18) . . ? C21 C19 N2 107.9(15) . . ? C20 C19 N2 111.8(14) . . ? C24 C22 N2 111.5(19) . . ? C24 C22 C23 113.0(18) . . ? N2 C22 C23 110(2) . . ? N25 O6 N25 68(3) 2_565 . ? O6B N25 O6C 126(4) . . ? O6B N25 O6 131(3) . . ? O6C N25 O6 103(3) . . ? O6B N25 N25 141(4) . 2_565 ? O6C N25 N25 68(3) . 2_565 ? O6 N25 N25 56.2(14) . 2_565 ? O6B N25 O6C 91(3) . 2_565 ? O6C N25 O6C 91(3) . 2_565 ? O6 N25 O6C 90(2) . 2_565 ? N25 N25 O6C 50.5(17) 2_565 2_565 ? N25 O6C N25 62(3) . 2_565 ? O9 N4 O8 130(5) . . ? O9 N4 O7 115(5) . . ? O8 N4 O7 111(5) . . ? O10B N5 O10B 98.9(15) 7_577 2_665 ? O10B N5 O10B 98.9(15) 7_577 . ? O10B N5 O10B 134(4) 2_665 . ? O10B N5 O10B 134(4) 7_577 8_757 ? O10B N5 O10B 98.9(15) 2_665 8_757 ? O10B N5 O10B 98.9(15) . 8_757 ? O10B N5 O10 67(3) 7_577 7_577 ? O10B N5 O10 80(2) 2_665 7_577 ? O10B N5 O10 146(3) . 7_577 ? O10B N5 O10 74(3) 8_757 7_577 ? O10B N5 O10 146(3) 7_577 2_665 ? O10B N5 O10 67(3) 2_665 2_665 ? O10B N5 O10 74(3) . 2_665 ? O10B N5 O10 80(2) 8_757 2_665 ? O10 N5 O10 134(2) 7_577 2_665 ? O10B N5 O10 80(2) 7_577 . ? O10B N5 O10 74(3) 2_665 . ? O10B N5 O10 67(3) . . ? O10B N5 O10 146(3) 8_757 . ? O10 N5 O10 134(2) 7_577 . ? O10 N5 O10 67(4) 2_665 . ? O10B N5 O10 74(3) 7_577 8_757 ? O10B N5 O10 146(3) 2_665 8_757 ? O10B N5 O10 80(2) . 8_757 ? O10B N5 O10 67(3) 8_757 8_757 ? O10 N5 O10 67(4) 7_577 8_757 ? O10 N5 O10 134(2) 2_665 8_757 ? O10 N5 O10 134(2) . 8_757 ? N5 O10 O10B 55(3) . . ? N5 O10 O10 56.7(18) . 2_665 ? O10B O10 O10 66(4) . 2_665 ? N5 O10 O10B 52(3) . 2_665 ? O10B O10 O10B 102(5) . 2_665 ? O10 O10 O10B 57(3) 2_665 2_665 ? N5 O10 O10B 49(2) . 7_577 ? O10B O10 O10B 77(3) . 7_577 ? O10 O10 O10B 105(3) 2_665 7_577 ? O10B O10 O10B 73(3) 2_665 7_577 ? N5 O10B O10 58(3) . . ? N5 O10B O10 54(3) . 2_665 ? O10 O10B O10 57(4) . 2_665 ? N5 O10B O10 51(2) . 8_757 ? O10 O10B O10 103(5) . 8_757 ? O10 O10B O10 97(4) 2_665 8_757 ? N5 O10B O10B 40.5(8) . 7_577 ? O10 O10B O10B 57(2) . 7_577 ? O10 O10B O10B 90(3) 2_665 7_577 ? O10 O10B O10B 51(2) 8_757 7_577 ? N5 O10B O10B 40.5(8) . 8_757 ? O10 O10B O10B 94(3) . 8_757 ? O10 O10B O10B 56(2) 2_665 8_757 ? O10 O10B O10B 46(3) 8_757 8_757 ? O10B O10B O10B 74(2) 7_577 8_757 ? O11 N6 O11 105.6(13) 8_767 2_575 ? O11 N6 O11 105.6(12) 8_767 . ? O11 N6 O11 118(3) 2_575 . ? O11 N6 O11 118(3) 8_767 7_477 ? O11 N6 O11 105.6(12) 2_575 7_477 ? O11 N6 O11 105.6(13) . 7_477 ? O11 N6 O11B 77.2(19) 8_767 2_575 ? O11 N6 O11B 29(2) 2_575 2_575 ? O11 N6 O11B 122.2(18) . 2_575 ? O11 N6 O11B 124(2) 7_477 2_575 ? O11 N6 O11B 29(2) 8_767 8_767 ? O11 N6 O11B 124(2) 2_575 8_767 ? O11 N6 O11B 77.2(19) . 8_767 ? O11 N6 O11B 122.2(18) 7_477 8_767 ? O11B N6 O11B 96.3(9) 2_575 8_767 ? O11 N6 O11B 124(2) 8_767 . ? O11 N6 O11B 122.2(18) 2_575 . ? O11 N6 O11B 29(2) . . ? O11 N6 O11B 77.2(19) 7_477 . ? O11B N6 O11B 141(3) 2_575 . ? O11B N6 O11B 96.3(9) 8_767 . ? O11 N6 O11B 122.2(18) 8_767 7_477 ? O11 N6 O11B 77.2(19) 2_575 7_477 ? O11 N6 O11B 124(2) . 7_477 ? O11 N6 O11B 29(2) 7_477 7_477 ? O11B N6 O11B 96.3(9) 2_575 7_477 ? O11B N6 O11B 141(3) 8_767 7_477 ? O11B N6 O11B 96.3(9) . 7_477 ? O11B O11 N6 83(5) . . ? O11B O11 O11B 116(5) . 8_767 ? N6 O11 O11B 53.6(18) . 8_767 ? O11 O11B N6 69(5) . . ? O11 O11B O11 117(6) . 7_477 ? N6 O11B O11 49.2(18) . 7_477 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.166 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.119 #===END