# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_la9 _database_code_depnum_ccdc_archive 'CCDC 889301' #TrackingRef 'web_deposit_cif_file_0_GaryGuillet_1349826934.gg6a.cif' # # xray code for La9 is gg6a # _audit_update_record ; 2012-09-24 # Formatted by publCIF ; _vrf_CHEMW03_I ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: the solvent area, which included three ether and three methanol molecules, were removed using Platon/Squeeze. ; _vrf_DENSD01_I ; PROBLEM: The ratio of the submitted crystal density and that RESPONSE: Density calculated using full crystal contents but not solvents ; _vrf_PLAT046_I ; PROBLEM: Reported Z, MW and D(calc) are Inconsistent .... 1.339 RESPONSE: All caused by removing solvents from the refinemt but not in the cell contents. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C103 H97 N16 O6 La1, N6 O18 La1, 6(CH4O), 3(C4H10O)' _chemical_formula_sum 'C121 H151 La2 N21 O33' _chemical_formula_weight 2705.45 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.2537(10) _cell_length_b 18.390(1) _cell_length_c 20.7899(12) _cell_angle_alpha 74.209(1) _cell_angle_beta 89.492(1) _cell_angle_gamma 87.577(1) _cell_volume 6709.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9229 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description blocks _exptl_crystal_colour clear _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2804 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6939 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40185 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 22967 _reflns_number_gt 20200 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT (Bruker, 2008)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The following restraints were employed in the final refinement model. La9 eadp o7 o8 o9 o10 o11 o12 o13 o14 o15 o16 o17 o18 o19 o20 o21 o22 o23 o24 eadp o7' o8' o9' o10' o11' o12' o13' o14' eadp o15' o16' o17' o18' o19' o20' o21' o22' o23' o24' eadp n16 n17 n18 n19 n20 n21 eadp n16' n17' n18' n19' n20' n21' DFIX 1.54 0.005 C76' C77' C76' C78' C76' C79' DFIX 2.54 0.005 C77' C78' C77' C79' C79' C78' DFIX 1.54 0.005 C76" C77" C76" C79" C76" C78" DFIX 2.54 0.005 C77" C79" C77" C78" C79" C78" ; _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^)+(0.0576P)^2^+8.4495P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22967 _refine_ls_number_parameters 1144 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 La1 La 0.251618(8) 0.228305(8) 0.418925(8) 0.01455(6) Uani 1 1 d . . . O1 O 0.20604(11) 0.31515(11) 0.31127(10) 0.0210(4) Uani 1 1 d . . . O2 O 0.26690(11) 0.13182(11) 0.3583(1) 0.0197(4) Uani 1 1 d . . . O3 O 0.36907(11) 0.26631(12) 0.36890(11) 0.0233(4) Uani 1 1 d . . . O4 O 0.19752(12) 0.27657(12) 0.15063(10) 0.0227(4) Uani 1 1 d . . . O5 O 0.37214(11) 0.12996(11) 0.22571(10) 0.0224(4) Uani 1 1 d . . . O6 O 0.39284(12) 0.36337(12) 0.17672(11) 0.0259(5) Uani 1 1 d . D . N1 N 0.11006(13) 0.22411(13) 0.38545(11) 0.0166(5) Uani 1 1 d . . . N2 N 0.33328(12) 0.10179(13) 0.47567(11) 0.0158(5) Uani 1 1 d . . . N3 N 0.29830(14) 0.36350(13) 0.42312(12) 0.0194(5) Uani 1 1 d . . . N4 N 0.16429(13) 0.12873(13) 0.49915(12) 0.0182(5) Uani 1 1 d . . . N5 N 0.31214(13) 0.20793(13) 0.54233(12) 0.0196(5) Uani 1 1 d . . . N6 N 0.17003(13) 0.31542(14) 0.47977(12) 0.0201(5) Uani 1 1 d . . . N7 N 0.18947(13) 0.09360(13) 0.56068(12) 0.0188(5) Uani 1 1 d . . . N8 N 0.29046(14) 0.25617(14) 0.57741(13) 0.0228(5) Uani 1 1 d . . . N9 N 0.11465(14) 0.28211(14) 0.51804(13) 0.0232(5) Uani 1 1 d . F . N10 N 0.04646(13) 0.08223(13) 0.52810(12) 0.0183(5) Uani 1 1 d . . . N11 N 0.37362(13) 0.12772(14) 0.63726(12) 0.0203(5) Uani 1 1 d . . . N12 N 0.15616(14) 0.42228(14) 0.52213(12) 0.0221(5) Uani 1 1 d . . . N13 N 0.12457(13) 0.35942(13) 0.22674(12) 0.0191(5) Uani 1 1 d . . . H13C H 0.0778 0.3664 0.2159 0.023 Uiso 1 1 calc R . . N14 N 0.30956(13) 0.02406(13) 0.33695(12) 0.0200(5) Uani 1 1 d . . . H14C H 0.3321 -0.0205 0.3528 0.024 Uiso 1 1 calc R . . N15 N 0.44199(14) 0.35600(15) 0.30898(12) 0.0239(6) Uani 1 1 d . . . H15A H 0.4567 0.4025 0.3016 0.029 Uiso 1 1 calc R . . C1 C 0.34373(16) 0.25566(16) 0.11561(15) 0.0200(6) Uani 1 1 d . . . H1A H 0.3287 0.2570 0.1617 0.024 Uiso 1 1 calc R . . C2 C 0.28227(16) 0.21925(16) 0.08851(14) 0.0196(6) Uani 1 1 d . . . C3 C 0.29460(17) 0.17169(17) 0.04734(15) 0.0227(6) Uani 1 1 d . E . H3A H 0.3434 0.1630 0.0340 0.027 Uiso 1 1 calc R . . C4 C 0.23765(19) 0.13626(17) 0.02489(15) 0.0256(7) Uani 1 1 d . . . C5 C 0.16710(19) 0.15094(18) 0.04437(16) 0.0287(7) Uani 1 1 d . E . H5A H 0.1278 0.1272 0.0297 0.034 Uiso 1 1 calc R . . C6 C 0.15126(17) 0.19928(18) 0.08477(15) 0.0256(7) Uani 1 1 d . . . C7 C 0.21000(17) 0.23259(16) 0.10645(14) 0.0205(6) Uani 1 1 d . E . C12 C 0.07374(19) 0.2128(2) 0.10504(19) 0.0365(8) Uani 1 1 d . E . H12A H 0.0731 0.2475 0.1334 0.055 Uiso 1 1 calc R . . H12B H 0.0537 0.1646 0.1299 0.055 Uiso 1 1 calc R . . H12C H 0.0439 0.2350 0.0650 0.055 Uiso 1 1 calc R . . C13 C 0.17829(17) 0.35517(16) 0.12063(14) 0.0215(6) Uani 1 1 d . . . H13A H 0.1290 0.3609 0.0999 0.026 Uiso 1 1 calc R . . H13B H 0.2143 0.3777 0.0858 0.026 Uiso 1 1 calc R . . C14 C 0.17893(17) 0.39310(17) 0.17600(14) 0.0227(6) Uani 1 1 d . . . H14A H 0.2283 0.3868 0.1965 0.027 Uiso 1 1 calc R . . H14B H 0.1672 0.4479 0.1579 0.027 Uiso 1 1 calc R . . C15 C 0.14250(16) 0.31928(15) 0.28754(14) 0.0179(6) Uani 1 1 d . . . C16 C 0.08351(16) 0.27538(16) 0.33036(14) 0.0175(6) Uani 1 1 d . . . C17 C 0.00946(17) 0.28637(17) 0.31574(15) 0.0224(6) Uani 1 1 d . . . H17A H -0.0077 0.3245 0.2776 0.027 Uiso 1 1 calc R . . C18 C -0.03943(17) 0.24018(18) 0.35823(15) 0.0242(7) Uani 1 1 d . . . H18A H -0.0906 0.2466 0.3495 0.029 Uiso 1 1 calc R . . C19 C -0.01288(16) 0.18495(17) 0.41330(15) 0.0219(6) Uani 1 1 d . . . H19A H -0.0451 0.1516 0.4421 0.026 Uiso 1 1 calc R . . C20 C 0.06255(16) 0.17949(16) 0.42547(14) 0.0173(6) Uani 1 1 d . . . C21 C 0.09299(15) 0.12631(15) 0.48722(14) 0.0165(6) Uani 1 1 d . . . C22 C 0.07080(16) 0.04380(15) 0.58805(14) 0.0178(6) Uani 1 1 d . . . C23 C 0.14342(16) 0.05594(15) 0.60640(14) 0.0178(6) Uani 1 1 d . . . C24 C 0.01942(16) -0.00814(16) 0.63121(14) 0.0190(6) Uani 1 1 d . . . C25 C -0.05586(16) 0.00259(17) 0.61498(15) 0.0204(6) Uani 1 1 d . . . H25A H -0.0720 0.0423 0.5775 0.025 Uiso 1 1 calc R . . C26 C -0.10623(17) -0.04452(17) 0.65353(15) 0.0231(6) Uani 1 1 d . . . H26A H -0.1568 -0.0370 0.6423 0.028 Uiso 1 1 calc R . . C27 C -0.08341(17) -0.10275(17) 0.70846(16) 0.0241(6) Uani 1 1 d . . . H27A H -0.1183 -0.1343 0.7353 0.029 Uiso 1 1 calc R . . C28 C -0.00918(18) -0.11459(17) 0.72394(16) 0.0251(7) Uani 1 1 d . . . H28A H 0.0067 -0.1548 0.7611 0.030 Uiso 1 1 calc R . . C29 C 0.04171(17) -0.06812(17) 0.68557(15) 0.0223(6) Uani 1 1 d . . . H29A H 0.0924 -0.0771 0.6963 0.027 Uiso 1 1 calc R . . C30 C 0.17319(16) 0.03130(16) 0.67537(15) 0.0206(6) Uani 1 1 d . . . C31 C 0.23124(17) -0.02204(17) 0.69159(16) 0.0236(6) Uani 1 1 d . . . H31A H 0.2536 -0.0415 0.6580 0.028 Uiso 1 1 calc R . . C32 C 0.25632(18) -0.04677(18) 0.75716(17) 0.0284(7) Uani 1 1 d . . . H32A H 0.2946 -0.0847 0.7688 0.034 Uiso 1 1 calc R . . C33 C 0.2257(2) -0.0163(2) 0.80528(17) 0.0348(8) Uani 1 1 d . . . H33A H 0.2436 -0.0327 0.8499 0.042 Uiso 1 1 calc R . . C34 C 0.1687(2) 0.0383(2) 0.78918(17) 0.0349(8) Uani 1 1 d . . . H34A H 0.1482 0.0595 0.8225 0.042 Uiso 1 1 calc R . . C35 C 0.14182(18) 0.06167(18) 0.72410(16) 0.0263(7) Uani 1 1 d . . . H35A H 0.1023 0.0982 0.7130 0.032 Uiso 1 1 calc R . . C36 C 0.41688(16) 0.21054(16) 0.12305(15) 0.0204(6) Uani 1 1 d . . . C37 C 0.47425(17) 0.22947(16) 0.07777(15) 0.0214(6) Uani 1 1 d . . . H37A H 0.4661 0.2684 0.0375 0.026 Uiso 1 1 calc R . . C38 C 0.54343(17) 0.19294(16) 0.08969(15) 0.0217(6) Uani 1 1 d . A . C39 C 0.55471(17) 0.13845(17) 0.14998(16) 0.0240(6) Uani 1 1 d . . . H39A H 0.6020 0.1143 0.1596 0.029 Uiso 1 1 calc R . . C40 C 0.49903(18) 0.11778(17) 0.19709(16) 0.0250(7) Uani 1 1 d . . . C41 C 0.42947(16) 0.15144(16) 0.18108(15) 0.0204(6) Uani 1 1 d . . . C42 C 0.60600(17) 0.21960(18) 0.03964(16) 0.0257(7) Uani 1 1 d . . . C43 C 0.6787(7) 0.1697(7) 0.0626(7) 0.001(4) Uiso 0.31(3) 1 d P A 1 H43A H 0.6721 0.1183 0.0588 0.002 Uiso 0.31(3) 1 calc PR A 1 H43B H 0.6897 0.1676 0.1091 0.002 Uiso 0.31(3) 1 calc PR A 1 H43C H 0.7194 0.1921 0.0339 0.002 Uiso 0.31(3) 1 calc PR A 1 C44 C 0.5834(5) 0.2040(9) -0.0273(5) 0.012(3) Uiso 0.31(3) 1 d P A 1 H44A H 0.5749 0.1500 -0.0196 0.018 Uiso 0.31(3) 1 calc PR A 1 H44B H 0.6226 0.2187 -0.0602 0.018 Uiso 0.31(3) 1 calc PR A 1 H44C H 0.5383 0.2336 -0.0443 0.018 Uiso 0.31(3) 1 calc PR A 1 C45 C 0.6176(8) 0.2983(8) 0.0278(10) 0.032(4) Uiso 0.31(3) 1 d P A 1 H45A H 0.6106 0.3236 -0.0198 0.048 Uiso 0.31(3) 1 calc PR A 1 H45B H 0.6676 0.3052 0.0411 0.048 Uiso 0.31(3) 1 calc PR A 1 H45C H 0.5824 0.3201 0.0540 0.048 Uiso 0.31(3) 1 calc PR A 1 C43' C 0.6747(7) 0.1724(7) 0.0546(7) 0.058(4) Uiso 0.69(3) 1 d P A 2 H43D H 0.6661 0.1216 0.0505 0.087 Uiso 0.69(3) 1 calc PR A 2 H43E H 0.6907 0.1690 0.1002 0.087 Uiso 0.69(3) 1 calc PR A 2 H43F H 0.7128 0.1954 0.0229 0.087 Uiso 0.69(3) 1 calc PR A 2 C44' C 0.5843(4) 0.2297(8) -0.0320(4) 0.047(2) Uiso 0.69(3) 1 d P A 2 H44D H 0.5727 0.1807 -0.0385 0.071 Uiso 0.69(3) 1 calc PR A 2 H44E H 0.6249 0.2508 -0.0614 0.071 Uiso 0.69(3) 1 calc PR A 2 H44F H 0.5411 0.2644 -0.0428 0.071 Uiso 0.69(3) 1 calc PR A 2 C45' C 0.6245(3) 0.3012(3) 0.0453(4) 0.0298(18) Uiso 0.69(3) 1 d P A 2 H45D H 0.6370 0.2982 0.0917 0.045 Uiso 0.69(3) 1 calc PR A 2 H45E H 0.5817 0.3358 0.0313 0.045 Uiso 0.69(3) 1 calc PR A 2 H45F H 0.6662 0.3198 0.0163 0.045 Uiso 0.69(3) 1 calc PR A 2 C46 C 0.5141(2) 0.0658(2) 0.26591(17) 0.0365(8) Uani 1 1 d . . . H46A H 0.4684 0.0583 0.2915 0.055 Uiso 1 1 calc R . . H46B H 0.5496 0.0884 0.2890 0.055 Uiso 1 1 calc R . . H46C H 0.5342 0.0169 0.2619 0.055 Uiso 1 1 calc R . . C47 C 0.33909(17) 0.06320(17) 0.21796(15) 0.0230(6) Uani 1 1 d . . . H47A H 0.3761 0.0209 0.2250 0.028 Uiso 1 1 calc R . . H47B H 0.3184 0.0728 0.1724 0.028 Uiso 1 1 calc R . . C48 C 0.27918(17) 0.04381(18) 0.26935(15) 0.0229(6) Uani 1 1 d . . . H48A H 0.2440 0.0876 0.2634 0.027 Uiso 1 1 calc R . . H48B H 0.2523 0.0007 0.2628 0.027 Uiso 1 1 calc R . . C49 C 0.30433(15) 0.07085(16) 0.37501(14) 0.0180(6) Uani 1 1 d . . . C50 C 0.34377(15) 0.04983(16) 0.44085(14) 0.0174(6) Uani 1 1 d . . . C51 C 0.38634(17) -0.01648(17) 0.46551(15) 0.0234(6) Uani 1 1 d . . . H51A H 0.3935 -0.0516 0.4397 0.028 Uiso 1 1 calc R . . C52 C 0.41806(18) -0.03055(17) 0.52813(16) 0.0263(7) Uani 1 1 d . . . H52A H 0.4471 -0.0755 0.5460 0.032 Uiso 1 1 calc R . . C53 C 0.40692(17) 0.02177(17) 0.56422(15) 0.0240(6) Uani 1 1 d . . . H53A H 0.4281 0.0132 0.6074 0.029 Uiso 1 1 calc R . . C54 C 0.36437(15) 0.08713(16) 0.53664(14) 0.0181(6) Uani 1 1 d . . . C55 C 0.34886(16) 0.14413(16) 0.57399(15) 0.0196(6) Uani 1 1 d . . . C56 C 0.35543(17) 0.17714(17) 0.67146(15) 0.0232(6) Uani 1 1 d . B . C57 C 0.30833(18) 0.24109(17) 0.64172(15) 0.0236(6) Uani 1 1 d . B . C58 C 0.38990(18) 0.16323(18) 0.73868(15) 0.0262(7) Uani 1 1 d . . . C59 C 0.40133(18) 0.08887(18) 0.77716(16) 0.0269(7) Uani 1 1 d . B . H59A H 0.3835 0.0485 0.7621 0.032 Uiso 1 1 calc R . . C60 C 0.4388(2) 0.0735(2) 0.83743(17) 0.0367(8) Uani 1 1 d . . . H60A H 0.4468 0.0228 0.8636 0.044 Uiso 1 1 calc R B . C61 C 0.4644(2) 0.1324(2) 0.85945(19) 0.0453(10) Uani 1 1 d . B . H61A H 0.4956 0.1217 0.8975 0.054 Uiso 0.51(4) 1 calc PR B 1 H61B H 0.4842 0.1228 0.9032 0.054 Uiso 0.49(4) 1 d PR B 2 C64 C 0.2738(2) 0.29367(18) 0.67715(16) 0.0300(7) Uani 1 1 d . . . C65 C 0.2355(2) 0.2665(2) 0.73578(18) 0.0434(10) Uani 1 1 d . C . H65A H 0.2271 0.2144 0.7547 0.052 Uiso 0.46(3) 1 calc PR C 1 H65B H 0.2418 0.2142 0.7580 0.052 Uiso 0.54(3) 1 d PR C 2 C70 C 0.35297(16) 0.33784(16) 0.07546(15) 0.0215(6) Uani 1 1 d . D . C71 C 0.33531(16) 0.36360(17) 0.00832(15) 0.0232(6) Uani 1 1 d . D . H71A H 0.3183 0.3287 -0.0139 0.028 Uiso 1 1 calc R . . C72 C 0.3416(2) 0.43864(19) -0.02771(17) 0.0328(8) Uani 1 1 d . . . C75 C 0.37902(18) 0.38874(17) 0.10837(16) 0.0267(7) Uani 1 1 d . . . C73 C 0.3610(4) 0.4896(3) 0.0108(3) 0.0222(15) Uiso 0.626(17) 1 d P D 1 H73A H 0.3612 0.5422 -0.0111 0.027 Uiso 0.626(17) 1 calc PR D 1 C74 C 0.3795(4) 0.4653(3) 0.0791(3) 0.0215(15) Uiso 0.626(17) 1 d P D 1 C80 C 0.4010(4) 0.5221(3) 0.1149(3) 0.0296(17) Uiso 0.626(17) 1 d P D 1 H80A H 0.4136 0.4960 0.1614 0.044 Uiso 0.626(17) 1 calc PR D 1 H80B H 0.3600 0.5585 0.1139 0.044 Uiso 0.626(17) 1 calc PR D 1 H80C H 0.4436 0.5489 0.0927 0.044 Uiso 0.626(17) 1 calc PR D 1 C73' C 0.3820(8) 0.4844(6) -0.0028(6) 0.030(3) Uiso 0.374(17) 1 d P D 2 H73B H 0.3987 0.5304 -0.0311 0.036 Uiso 0.374(17) 1 calc PR D 2 C74' C 0.3990(8) 0.4631(6) 0.0655(6) 0.030(3) Uiso 0.374(17) 1 d P D 2 C80' C 0.4311(8) 0.5181(6) 0.1011(6) 0.035(3) Uiso 0.374(17) 1 d P D 2 H80D H 0.4402 0.5662 0.0683 0.053 Uiso 0.374(17) 1 calc PR D 2 H80E H 0.4773 0.4961 0.1231 0.053 Uiso 0.374(17) 1 calc PR D 2 H80F H 0.3963 0.5267 0.1347 0.053 Uiso 0.374(17) 1 calc PR D 2 C76 C 0.3157(9) 0.4652(6) -0.0986(5) 0.016(3) Uiso 0.48(3) 1 d P D 1 C77 C 0.2332(8) 0.4610(9) -0.1015(7) 0.033(3) Uiso 0.48(3) 1 d P D 1 H77A H 0.2193 0.4090 -0.0809 0.050 Uiso 0.48(3) 1 calc PR D 1 H77B H 0.2171 0.4767 -0.1483 0.050 Uiso 0.48(3) 1 calc PR D 1 H77C H 0.2100 0.4947 -0.0773 0.050 Uiso 0.48(3) 1 calc PR D 1 C78 C 0.3532(7) 0.4138(10) -0.1416(7) 0.029(3) Uiso 0.48(3) 1 d P D 1 H78A H 0.3444 0.3605 -0.1201 0.043 Uiso 0.48(3) 1 calc PR D 1 H78B H 0.4061 0.4213 -0.1444 0.043 Uiso 0.48(3) 1 calc PR D 1 H78C H 0.3321 0.4282 -0.1867 0.043 Uiso 0.48(3) 1 calc PR D 1 C79 C 0.3302(11) 0.5492(6) -0.1326(7) 0.024(3) Uiso 0.48(3) 1 d P D 1 H79A H 0.3051 0.5812 -0.1077 0.036 Uiso 0.48(3) 1 calc PR D 1 H79B H 0.3116 0.5629 -0.1786 0.036 Uiso 0.48(3) 1 calc PR D 1 H79C H 0.3830 0.5568 -0.1330 0.036 Uiso 0.48(3) 1 calc PR D 1 C76' C 0.3279(8) 0.4569(7) -0.1117(8) 0.019(4) Uiso 0.26(2) 1 d PD D 2 C77' C 0.2442(8) 0.4499(8) -0.1127(9) 0.021(4) Uiso 0.26(2) 1 d PD D 2 H77D H 0.2269 0.4630 -0.1591 0.031 Uiso 0.26(2) 1 calc PR D 2 H77E H 0.2205 0.4845 -0.0896 0.031 Uiso 0.26(2) 1 calc PR D 2 H77F H 0.2318 0.3978 -0.0901 0.031 Uiso 0.26(2) 1 calc PR D 2 C78' C 0.3674(10) 0.4008(10) -0.1448(11) 0.050(7) Uiso 0.26(2) 1 d PD D 2 H78D H 0.3568 0.4158 -0.1928 0.074 Uiso 0.26(2) 1 calc PR D 2 H78E H 0.3502 0.3498 -0.1248 0.074 Uiso 0.26(2) 1 calc PR D 2 H78F H 0.4204 0.4010 -0.1377 0.074 Uiso 0.26(2) 1 calc PR D 2 C79' C 0.3495(11) 0.5386(7) -0.1454(9) 0.028(4) Uiso 0.26(2) 1 d PD D 2 H79D H 0.3393 0.5508 -0.1934 0.042 Uiso 0.26(2) 1 calc PR D 2 H79E H 0.4019 0.5433 -0.1382 0.042 Uiso 0.26(2) 1 calc PR D 2 H79F H 0.3209 0.5736 -0.1259 0.042 Uiso 0.26(2) 1 calc PR D 2 C76" C 0.3046(9) 0.4703(8) -0.0978(8) 0.048(12) Uiso 0.26(3) 1 d PD D 3 C77" C 0.2250(7) 0.4453(10) -0.0970(9) 0.021(5) Uiso 0.26(3) 1 d PD D 3 H77G H 0.2243 0.3901 -0.0811 0.031 Uiso 0.26(3) 1 calc PR D 3 H77H H 0.2045 0.4623 -0.1422 0.031 Uiso 0.26(3) 1 calc PR D 3 H77I H 0.1956 0.4677 -0.0670 0.031 Uiso 0.26(3) 1 calc PR D 3 C78" C 0.3539(8) 0.4314(13) -0.1403(10) 0.029(5) Uiso 0.26(3) 1 d PD D 3 H78G H 0.3490 0.3766 -0.1248 0.044 Uiso 0.26(3) 1 calc PR D 3 H78H H 0.4051 0.4434 -0.1358 0.044 Uiso 0.26(3) 1 calc PR D 3 H78I H 0.3389 0.4496 -0.1873 0.044 Uiso 0.26(3) 1 calc PR D 3 C79" C 0.3079(18) 0.5570(8) -0.1229(11) 0.048(6) Uiso 0.26(3) 1 d PD D 3 H79G H 0.3592 0.5713 -0.1265 0.072 Uiso 0.26(3) 1 calc PR D 3 H79H H 0.2823 0.5801 -0.0913 0.072 Uiso 0.26(3) 1 calc PR D 3 H79I H 0.2842 0.5748 -0.1669 0.072 Uiso 0.26(3) 1 calc PR D 3 C81 C 0.46930(17) 0.34920(18) 0.19494(15) 0.0246(7) Uani 1 1 d . . . H81A H 0.4945 0.3975 0.1863 0.030 Uiso 1 1 calc R D . H81B H 0.4936 0.3179 0.1684 0.030 Uiso 1 1 calc R . . C82 C 0.47273(17) 0.30809(19) 0.26849(15) 0.0271(7) Uani 1 1 d . D . H82A H 0.4449 0.2614 0.2769 0.033 Uiso 1 1 calc R . . H82B H 0.5244 0.2934 0.2817 0.033 Uiso 1 1 calc R . . C83 C 0.39325(16) 0.33150(17) 0.35582(14) 0.0214(6) Uani 1 1 d . . . C84 C 0.36293(17) 0.38480(17) 0.39422(15) 0.0227(6) Uani 1 1 d . . . C85 C 0.39707(19) 0.4481(2) 0.40151(17) 0.0316(7) Uani 1 1 d . . . H85A H 0.4437 0.4608 0.3821 0.038 Uiso 1 1 calc R . . C86 C 0.3621(2) 0.4927(2) 0.43760(18) 0.0368(8) Uani 1 1 d . . . H86A H 0.3846 0.5361 0.4434 0.044 Uiso 1 1 calc R . . C87 C 0.29352(19) 0.47304(18) 0.46527(17) 0.0293(7) Uani 1 1 d . . . H87A H 0.2676 0.5036 0.4888 0.035 Uiso 1 1 calc R . . C88 C 0.26391(17) 0.40732(17) 0.45749(15) 0.0225(6) Uani 1 1 d . . . C89 C 0.19317(17) 0.38004(16) 0.48876(15) 0.0211(6) Uani 1 1 d . . . C90 C 0.09581(17) 0.39448(17) 0.55374(15) 0.0225(6) Uani 1 1 d . F . C91 C 0.08048(18) 0.31765(17) 0.55840(16) 0.0250(7) Uani 1 1 d . . . C92 C 0.04652(18) 0.44623(16) 0.57913(15) 0.0232(6) Uani 1 1 d . . . C93 C 0.0750(2) 0.51077(18) 0.59066(17) 0.0298(7) Uani 1 1 d . F . H93A H 0.1256 0.5202 0.5836 0.036 Uiso 1 1 calc R . . C94 C 0.0287(2) 0.5614(2) 0.61260(18) 0.0358(8) Uani 1 1 d . . . H94A H 0.0480 0.6052 0.6210 0.043 Uiso 1 1 calc R F . C95 C -0.0454(2) 0.54792(19) 0.62221(17) 0.0342(8) Uani 1 1 d . F . H95A H -0.0765 0.5822 0.6377 0.041 Uiso 1 1 calc R . . C96 C -0.07412(19) 0.48483(18) 0.60941(16) 0.0291(7) Uani 1 1 d . . . H96A H -0.1250 0.4761 0.6156 0.035 Uiso 1 1 calc R F . C97 C -0.02827(18) 0.43427(17) 0.58741(15) 0.0252(7) Uani 1 1 d . F . H97A H -0.0480 0.3913 0.5780 0.030 Uiso 1 1 calc R . . C8 C 0.2455(8) 0.0885(5) -0.0230(4) 0.021(3) Uiso 0.50(4) 1 d P E 1 C9 C 0.3145(9) 0.0360(5) -0.0014(5) 0.032(3) Uiso 0.50(4) 1 d P E 1 H9A H 0.3567 0.0666 0.0006 0.047 Uiso 0.50(4) 1 calc PR E 1 H9B H 0.3242 0.0068 -0.0338 0.047 Uiso 0.50(4) 1 calc PR E 1 H9C H 0.3064 0.0012 0.0428 0.047 Uiso 0.50(4) 1 calc PR E 1 C10 C 0.2537(7) 0.1394(6) -0.0946(4) 0.024(3) Uiso 0.50(4) 1 d P E 1 H10A H 0.2098 0.1726 -0.1069 0.036 Uiso 0.50(4) 1 calc PR E 1 H10B H 0.2599 0.1079 -0.1256 0.036 Uiso 0.50(4) 1 calc PR E 1 H10C H 0.2967 0.1701 -0.0969 0.036 Uiso 0.50(4) 1 calc PR E 1 C11 C 0.1807(8) 0.0381(7) -0.0247(5) 0.034(3) Uiso 0.50(4) 1 d P E 1 H11A H 0.1359 0.0699 -0.0376 0.051 Uiso 0.50(4) 1 calc PR E 1 H11B H 0.1742 0.0032 0.0198 0.051 Uiso 0.50(4) 1 calc PR E 1 H11C H 0.1907 0.0091 -0.0572 0.051 Uiso 0.50(4) 1 calc PR E 1 C8' C 0.2626(8) 0.0820(6) -0.0203(5) 0.027(3) Uiso 0.50(4) 1 d P E 2 C9' C 0.3354(9) 0.0404(6) -0.0026(5) 0.033(3) Uiso 0.50(4) 1 d P E 2 H9'A H 0.3456 0.0085 -0.0327 0.050 Uiso 0.50(4) 1 calc PR E 2 H9'B H 0.3341 0.0087 0.0437 0.050 Uiso 0.50(4) 1 calc PR E 2 H9'C H 0.3740 0.0769 -0.0071 0.050 Uiso 0.50(4) 1 calc PR E 2 C10' C 0.2708(10) 0.1323(7) -0.0918(6) 0.042(4) Uiso 0.50(4) 1 d P E 2 H10D H 0.2859 0.1009 -0.1213 0.063 Uiso 0.50(4) 1 calc PR E 2 H10E H 0.3081 0.1694 -0.0926 0.063 Uiso 0.50(4) 1 calc PR E 2 H10F H 0.2238 0.1587 -0.1072 0.063 Uiso 0.50(4) 1 calc PR E 2 C11' C 0.2004(9) 0.0249(7) -0.0165(5) 0.032(3) Uiso 0.50(4) 1 d P E 2 H11D H 0.2140 -0.0096 -0.0436 0.049 Uiso 0.50(4) 1 calc PR E 2 H11E H 0.1545 0.0528 -0.0335 0.049 Uiso 0.50(4) 1 calc PR E 2 H11F H 0.1938 -0.0043 0.0301 0.049 Uiso 0.50(4) 1 calc PR E 2 C66 C 0.2106(8) 0.3228(6) 0.7643(5) 0.035(3) Uiso 0.46(3) 1 d P C 1 H66A H 0.1910 0.3087 0.8082 0.042 Uiso 0.46(3) 1 calc PR C 1 C67 C 0.2133(7) 0.4019(6) 0.7296(6) 0.026(3) Uiso 0.46(3) 1 d P C 1 H67A H 0.1882 0.4382 0.7477 0.032 Uiso 0.46(3) 1 calc PR C 1 C68 C 0.2508(7) 0.4256(5) 0.6717(5) 0.021(3) Uiso 0.46(3) 1 d P C 1 H68A H 0.2537 0.4782 0.6507 0.025 Uiso 0.46(3) 1 calc PR C 1 C69 C 0.2853(7) 0.3734(5) 0.6426(5) 0.020(3) Uiso 0.46(3) 1 d P C 1 H69A H 0.3142 0.3882 0.6033 0.024 Uiso 0.46(3) 1 calc PR C 1 C66' C 0.1878(8) 0.3119(6) 0.7657(4) 0.040(3) Uiso 0.54(3) 1 d P C 2 H66B H 0.1546 0.2901 0.8004 0.048 Uiso 0.54(3) 1 calc PR C 2 C67' C 0.1929(7) 0.3882(5) 0.7414(5) 0.034(2) Uiso 0.54(3) 1 d P C 2 H67B H 0.1688 0.4209 0.7640 0.041 Uiso 0.54(3) 1 calc PR C 2 C68' C 0.2324(6) 0.4183(5) 0.6847(5) 0.028(2) Uiso 0.54(3) 1 d P C 2 H68B H 0.2344 0.4715 0.6669 0.034 Uiso 0.54(3) 1 calc PR C 2 C69' C 0.2696(6) 0.3694(5) 0.6537(5) 0.027(3) Uiso 0.54(3) 1 d P C 2 H69B H 0.2939 0.3913 0.6128 0.032 Uiso 0.54(3) 1 calc PR C 2 C62 C 0.4445(8) 0.2084(5) 0.8256(6) 0.028(3) Uiso 0.51(4) 1 d P B 1 H62A H 0.4566 0.2484 0.8439 0.034 Uiso 0.51(4) 1 calc PR B 1 C63 C 0.4069(9) 0.2235(5) 0.7653(5) 0.025(3) Uiso 0.51(4) 1 d P B 1 H63A H 0.3927 0.2740 0.7420 0.030 Uiso 0.51(4) 1 calc PR B 1 C62' C 0.4627(10) 0.2051(6) 0.8160(7) 0.037(3) Uiso 0.49(4) 1 d P B 2 H62B H 0.4884 0.2438 0.8273 0.044 Uiso 0.49(4) 1 calc PR B 2 C63' C 0.4245(9) 0.2211(5) 0.7573(6) 0.027(3) Uiso 0.49(4) 1 d P B 2 H63B H 0.4213 0.2714 0.7291 0.033 Uiso 0.49(4) 1 calc PR B 2 C98 C 0.0202(5) 0.2722(4) 0.5984(4) 0.021(2) Uiso 0.495(13) 1 d P F 1 C99 C 0.0229(5) 0.2651(5) 0.6680(4) 0.032(2) Uiso 0.495(13) 1 d P F 1 H99A H 0.0596 0.2898 0.6852 0.039 Uiso 0.495(13) 1 calc PR F 1 C100 C -0.0284(7) 0.2217(7) 0.7124(5) 0.047(2) Uiso 0.495(13) 1 d P F 1 H10G H -0.0262 0.2158 0.7592 0.056 Uiso 0.495(13) 1 calc PR F 1 C101 C -0.0807(6) 0.1890(6) 0.6852(7) 0.052(3) Uiso 0.495(13) 1 d P F 1 H10H H -0.1170 0.1614 0.7136 0.062 Uiso 0.495(13) 1 calc PR F 1 C102 C -0.0833(5) 0.1942(5) 0.6163(5) 0.039(2) Uiso 0.495(13) 1 d P F 1 H10I H -0.1199 0.1690 0.5994 0.046 Uiso 0.495(13) 1 calc PR F 1 C103 C -0.0328(4) 0.2359(4) 0.5734(5) 0.0277(19) Uiso 0.495(13) 1 d P F 1 H10J H -0.0346 0.2396 0.5270 0.033 Uiso 0.495(13) 1 calc PR F 1 C200 C 0.0360(4) 0.2725(4) 0.6140(4) 0.0177(19) Uiso 0.505(13) 1 d P F 2 C300 C 0.0408(5) 0.2783(5) 0.6786(4) 0.0263(19) Uiso 0.505(13) 1 d P F 2 H30A H 0.0766 0.3083 0.6906 0.032 Uiso 0.505(13) 1 calc PR F 2 C400 C -0.0071(5) 0.2398(5) 0.7246(4) 0.038(2) Uiso 0.505(13) 1 d P F 2 H40A H -0.0044 0.2429 0.7694 0.046 Uiso 0.505(13) 1 calc PR F 2 C500 C -0.0598(6) 0.1958(5) 0.7073(5) 0.038(2) Uiso 0.505(13) 1 d P F 2 H50A H -0.0926 0.1703 0.7408 0.045 Uiso 0.505(13) 1 calc PR F 2 C600 C -0.0665(5) 0.1880(4) 0.6449(5) 0.037(2) Uiso 0.505(13) 1 d P F 2 H60B H -0.1030 0.1582 0.6339 0.045 Uiso 0.505(13) 1 calc PR F 2 C700 C -0.0160(4) 0.2267(4) 0.5969(4) 0.0238(18) Uiso 0.505(13) 1 d P F 2 H70A H -0.0173 0.2215 0.5527 0.029 Uiso 0.505(13) 1 calc PR F 2 La2 La 0.294004(15) 0.718328(15) 0.607850(16) 0.01406(8) Uiso 0.70 1 d PG G 1 O7 O 0.30172(5) 0.81505(3) 0.67273(4) 0.0382(2) Uiso 0.70 1 d PG G 1 O8 O 0.34941(4) 0.69799(5) 0.72654(2) 0.0382(2) Uiso 0.70 1 d PG G 1 O9 O 0.34797(7) 0.78737(7) 0.77537(4) 0.0382(2) Uiso 0.70 1 d PG G 1 O10 O 0.19323(3) 0.69405(5) 0.69615(3) 0.0382(2) Uiso 0.70 1 d PG G 1 O11 O 0.25022(5) 0.59236(3) 0.68508(3) 0.0382(2) Uiso 0.70 1 d PG G 1 O12 O 0.15407(6) 0.58097(6) 0.74830(5) 0.0382(2) Uiso 0.70 1 d PG G 1 O13 O 0.39711(4) 0.60705(4) 0.64035(4) 0.0382(2) Uiso 0.70 1 d PG G 1 O14 O 0.32105(5) 0.58993(3) 0.56734(4) 0.0382(2) Uiso 0.70 1 d PG G 1 O15 O 0.40690(7) 0.50448(4) 0.60885(6) 0.0382(2) Uiso 0.70 1 d PG G 1 O16 O 0.23503(4) 0.72944(5) 0.48962(2) 0.0382(2) Uiso 0.70 1 d PG G 1 O17 O 0.17162(3) 0.66464(5) 0.57163(4) 0.0382(2) Uiso 0.70 1 d PG G 1 O18 O 0.15304(6) 0.65465(7) 0.47030(5) 0.0382(2) Uiso 0.70 1 d PG G 1 O19 O 0.42573(3) 0.78388(5) 0.59224(4) 0.0382(2) Uiso 0.70 1 d PG G 1 O20 O 0.39698(3) 0.73512(5) 0.51456(3) 0.0382(2) Uiso 0.70 1 d PG G 1 O21 O 0.50072(4) 0.79399(8) 0.51338(6) 0.0382(2) Uiso 0.70 1 d PG G 1 O22 O 0.18632(4) 0.82546(4) 0.58100(4) 0.0382(2) Uiso 0.70 1 d PG G 1 O23 O 0.28808(5) 0.85835(2) 0.53032(3) 0.0382(2) Uiso 0.70 1 d PG G 1 O24 O 0.19152(7) 0.93791(4) 0.51144(6) 0.0382(2) Uiso 0.70 1 d PG G 1 N16 N 0.33358(5) 0.76913(5) 0.72410(3) 0.0280(4) Uiso 0.70 1 d PG G 1 N17 N 0.19921(5) 0.62095(5) 0.71129(4) 0.0280(4) Uiso 0.70 1 d PG G 1 N18 N 0.37702(5) 0.56699(3) 0.60446(5) 0.0280(4) Uiso 0.70 1 d PG G 1 N19 N 0.18519(4) 0.67922(5) 0.51289(4) 0.0280(4) Uiso 0.70 1 d PG G 1 N20 N 0.44225(3) 0.77144(6) 0.54188(5) 0.0280(4) Uiso 0.70 1 d PG G 1 N21 N 0.22057(5) 0.87457(3) 0.53988(4) 0.0280(4) Uiso 0.70 1 d PG G 1 La2' La 0.29678(4) 0.72273(4) 0.58883(4) 0.0266(2) Uiso 0.30 1 d PG H 2 O7' O 0.30234(10) 0.80728(8) 0.69057(7) 0.0169(5) Uiso 0.30 1 d PG H 2 O8' O 0.34877(8) 0.70493(9) 0.71377(5) 0.0169(5) Uiso 0.30 1 d PG H 2 O9' O 0.33220(14) 0.76847(14) 0.79547(7) 0.0169(5) Uiso 0.30 1 d PG H 2 O10' O 0.19385(8) 0.69345(10) 0.71066(6) 0.0169(5) Uiso 0.30 1 d PG H 2 O11' O 0.24649(10) 0.58889(7) 0.69907(7) 0.0169(5) Uiso 0.30 1 d PG H 2 O12' O 0.15036(13) 0.58887(13) 0.76299(9) 0.0169(5) Uiso 0.30 1 d PG H 2 O13' O 0.40320(7) 0.61601(8) 0.62582(8) 0.0169(5) Uiso 0.30 1 d PG H 2 O14' O 0.32556(9) 0.60063(6) 0.55031(7) 0.0169(5) Uiso 0.30 1 d PG H 2 O15' O 0.41201(13) 0.51809(9) 0.58159(11) 0.0249(5) Uiso 0.30 1 d PG H 2 O16' O 0.25201(8) 0.72068(9) 0.47410(5) 0.0249(5) Uiso 0.30 1 d PG H 2 O17' O 0.18298(7) 0.65455(9) 0.55979(8) 0.0249(5) Uiso 0.30 1 d PG H 2 O18' O 0.17959(12) 0.63786(13) 0.45536(9) 0.0249(5) Uiso 0.30 1 d PG H 2 O19' O 0.42524(6) 0.77688(10) 0.59552(8) 0.0249(5) Uiso 0.30 1 d PG H 2 O20' O 0.39696(7) 0.75040(9) 0.49917(6) 0.0249(5) Uiso 0.30 1 d PG H 2 O21' O 0.49251(9) 0.81075(14) 0.49520(11) 0.0249(5) Uiso 0.30 1 d PG H 2 O22' O 0.28887(10) 0.85774(5) 0.51238(7) 0.0249(5) Uiso 0.30 1 d PG H 2 O23' O 0.18481(7) 0.82031(8) 0.56296(8) 0.0249(5) Uiso 0.30 1 d PG H 2 O24' O 0.19508(14) 0.93231(8) 0.48892(10) 0.0249(5) Uiso 0.30 1 d PG H 2 N16' N 0.32740(11) 0.75610(11) 0.74115(6) 0.0208(7) Uiso 0.30 1 d PG H 2 N17' N 0.19343(10) 0.62126(10) 0.72592(7) 0.0208(7) Uiso 0.30 1 d PG H 2 N18' N 0.37766(10) 0.57612(7) 0.58439(9) 0.0208(7) Uiso 0.30 1 d PG H 2 N19' N 0.20336(8) 0.67409(10) 0.49241(7) 0.0208(7) Uiso 0.30 1 d PG H 2 N20' N 0.44185(6) 0.77995(11) 0.52612(9) 0.0208(7) Uiso 0.30 1 d PG H 2 N21' N 0.22416(10) 0.87492(6) 0.51871(8) 0.0208(7) Uiso 0.30 1 d PG H 2 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 La1 0.01354(9) 0.01299(9) 0.01723(9) -0.00432(6) 0.00031(6) -0.00046(6) O1 0.0197(11) 0.0208(10) 0.0206(10) -0.0024(8) -0.0004(8) -0.0014(8) O2 0.0204(11) 0.0171(10) 0.0224(10) -0.0071(8) -0.0004(8) 0.0007(8) O3 0.0185(11) 0.0224(11) 0.0294(11) -0.0071(9) 0.0043(9) -0.0051(9) O4 0.0262(11) 0.0229(11) 0.0184(10) -0.0056(8) 0.0012(9) 0.0049(9) O5 0.0244(11) 0.0166(10) 0.0266(11) -0.0063(8) 0.0051(9) -0.0042(8) O6 0.0238(11) 0.0275(11) 0.0273(11) -0.0088(9) -0.0081(9) 0.0009(9) N1 0.0179(12) 0.0154(11) 0.0171(12) -0.0058(9) 0.0001(10) 0.0017(9) N2 0.0141(12) 0.0159(11) 0.0173(12) -0.0039(9) 0.0020(9) -0.0032(9) N3 0.0216(13) 0.0185(12) 0.0176(12) -0.0036(10) -0.0021(10) -0.0034(10) N4 0.0164(12) 0.0146(11) 0.0228(12) -0.0042(10) -0.0016(10) 0.0022(9) N5 0.0209(13) 0.0177(12) 0.0210(12) -0.0062(10) 0.0003(10) -0.0033(10) N6 0.0182(13) 0.0189(12) 0.0240(13) -0.0074(10) 0.0001(10) 0.0003(10) N7 0.0178(12) 0.0153(12) 0.0227(12) -0.0042(10) -0.0001(10) 0.0005(10) N8 0.0260(14) 0.0179(12) 0.0252(13) -0.0069(10) -0.0028(11) -0.001(1) N9 0.0203(13) 0.0195(12) 0.0314(14) -0.0098(11) 0.0047(11) -0.0006(10) N10 0.0174(12) 0.0164(12) 0.0217(12) -0.0059(10) 0.0014(10) -0.0016(10) N11 0.0196(13) 0.0214(12) 0.0193(12) -0.0042(10) -0.0015(10) -0.0034(10) N12 0.0262(14) 0.0181(12) 0.0220(13) -0.0057(10) -0.0018(11) 0.0017(11) N13 0.0159(12) 0.0216(12) 0.0190(12) -0.0046(10) 0.001(1) 0.0013(10) N14 0.0206(13) 0.0149(12) 0.0252(13) -0.0068(10) 0.0021(10) -0.0007(10) N15 0.0184(13) 0.0287(14) 0.0236(13) -0.0047(11) -0.0005(11) -0.0065(11) C1 0.0191(15) 0.0198(14) 0.0223(14) -0.0080(12) -0.0020(12) 0.0014(12) C2 0.0210(15) 0.0180(14) 0.0180(14) -0.0014(11) 0.0005(12) -0.0032(12) C3 0.0245(16) 0.0209(15) 0.0221(15) -0.0051(12) 0.0035(12) -0.0011(12) C4 0.0365(19) 0.0203(15) 0.0192(15) -0.0031(12) -0.0007(13) -0.0065(13) C5 0.0321(18) 0.0276(17) 0.0258(16) -0.0044(13) -0.0037(14) -0.0119(14) C6 0.0225(16) 0.0271(16) 0.0241(16) -0.0011(13) -0.0002(13) -0.0055(13) C7 0.0254(16) 0.0179(14) 0.0168(14) -0.0026(11) 0.0013(12) -0.0003(12) C12 0.0249(18) 0.043(2) 0.043(2) -0.0121(17) 0.0033(15) -0.0066(15) C13 0.0225(16) 0.0209(15) 0.0188(14) -0.0019(12) 0.0002(12) 0.0026(12) C14 0.0247(16) 0.0218(15) 0.0196(14) -0.0024(12) 0.0022(12) -0.0009(12) C15 0.0214(15) 0.0134(13) 0.0202(14) -0.0075(11) 0.0012(12) 0.0029(11) C16 0.0191(15) 0.0171(14) 0.0184(14) -0.0089(11) 0.0010(11) 0.0024(11) C17 0.0230(16) 0.0220(15) 0.0216(15) -0.0058(12) -0.0015(12) 0.0046(12) C18 0.0148(15) 0.0302(17) 0.0272(16) -0.0075(13) -0.0006(12) 0.0007(13) C19 0.0191(15) 0.0262(16) 0.0208(15) -0.0069(12) 0.0025(12) -0.0016(12) C20 0.0173(14) 0.0173(14) 0.0191(14) -0.0080(11) 0.0006(11) 0.0005(11) C21 0.0161(14) 0.0150(13) 0.0207(14) -0.0084(11) 0.0031(11) -0.0023(11) C22 0.0185(15) 0.0148(13) 0.0215(14) -0.0075(11) 0.0012(12) 0.0011(11) C23 0.0186(15) 0.0133(13) 0.0217(14) -0.0054(11) 0.0022(12) 0.0009(11) C24 0.0200(15) 0.0179(14) 0.0207(14) -0.0074(12) 0.0008(12) -0.0040(12) C25 0.0203(15) 0.0203(14) 0.0213(14) -0.0066(12) -0.0012(12) -0.0014(12) C26 0.0182(15) 0.0254(16) 0.0273(16) -0.0097(13) 0.0025(12) -0.0032(12) C27 0.0241(16) 0.0223(15) 0.0275(16) -0.0090(13) 0.0081(13) -0.0071(13) C28 0.0277(17) 0.0201(15) 0.0259(16) -0.0034(12) 0.0034(13) -0.0028(13) C29 0.0173(15) 0.0226(15) 0.0263(16) -0.0051(12) -0.0008(12) -0.0009(12) C30 0.0204(15) 0.0172(14) 0.0236(15) -0.0037(12) 0.0002(12) -0.0053(12) C31 0.0191(15) 0.0232(15) 0.0289(16) -0.0076(13) -0.0029(13) -0.0015(12) C32 0.0239(17) 0.0268(16) 0.0333(18) -0.0063(14) -0.0083(14) 0.0015(13) C33 0.038(2) 0.039(2) 0.0277(17) -0.0100(15) -0.0127(15) -0.0011(16) C34 0.044(2) 0.0363(19) 0.0290(18) -0.0174(15) -0.0037(15) 0.0028(16) C35 0.0285(17) 0.0244(16) 0.0267(16) -0.0089(13) -0.0060(13) 0.0044(13) C36 0.0191(15) 0.0174(14) 0.0262(15) -0.0082(12) -0.0018(12) -0.0008(12) C37 0.0248(16) 0.0178(14) 0.0213(15) -0.0049(12) -0.0032(12) 0.0002(12) C38 0.0231(16) 0.0176(14) 0.0269(16) -0.0103(12) -0.0014(13) -0.0023(12) C39 0.0197(15) 0.0212(15) 0.0310(17) -0.0077(13) -0.0025(13) 0.0025(12) C40 0.0272(17) 0.0166(14) 0.0288(16) -0.0027(12) -0.0006(13) 0.0020(12) C41 0.0211(15) 0.0171(14) 0.0246(15) -0.0083(12) 0.0019(12) -0.0020(12) C42 0.0217(16) 0.0287(17) 0.0267(16) -0.0076(13) 0.0013(13) -0.0005(13) C46 0.0305(19) 0.0362(19) 0.0327(18) 0.0063(15) 0.0015(15) 0.0084(15) C47 0.0264(16) 0.0197(15) 0.0249(15) -0.0093(12) 0.0017(13) -0.0028(12) C48 0.0226(16) 0.0252(16) 0.0242(15) -0.0122(13) 0.0006(12) -0.0034(13) C49 0.0164(14) 0.0169(14) 0.0213(14) -0.0056(11) 0.0050(11) -0.0044(11) C50 0.0133(14) 0.0165(14) 0.0218(14) -0.0039(11) 0.0051(11) -0.0053(11) C51 0.0243(16) 0.0168(14) 0.0279(16) -0.0041(12) 0.0024(13) 0.0010(12) C52 0.0281(17) 0.0190(15) 0.0291(17) -0.0029(13) 0.0003(13) 0.0057(13) C53 0.0227(16) 0.0240(15) 0.0227(15) -0.0020(12) -0.0016(12) -0.0009(13) C54 0.0155(14) 0.0179(14) 0.0200(14) -0.0030(11) 0.0015(11) -0.0035(11) C55 0.0151(14) 0.0205(14) 0.0222(15) -0.0032(12) -0.0004(12) -0.0057(12) C56 0.0241(16) 0.0222(15) 0.0226(15) -0.0039(12) -0.0043(13) -0.0072(12) C57 0.0295(17) 0.0205(15) 0.0212(15) -0.0057(12) -0.0014(13) -0.0062(13) C58 0.0278(17) 0.0264(16) 0.0241(16) -0.0061(13) -0.0071(13) -0.0022(13) C59 0.0297(18) 0.0272(16) 0.0256(16) -0.0100(13) -0.0037(13) -0.0024(14) C60 0.044(2) 0.0357(19) 0.0286(18) -0.0051(15) -0.0090(16) 0.0009(16) C61 0.055(3) 0.050(2) 0.0317(19) -0.0117(17) -0.0237(18) -0.0031(19) C64 0.041(2) 0.0245(16) 0.0265(17) -0.0110(13) -0.0125(15) 0.0026(14) C65 0.066(3) 0.036(2) 0.0288(19) -0.0118(16) -0.0019(18) 0.0134(19) C70 0.0164(15) 0.0184(14) 0.0289(16) -0.0056(12) -0.0015(12) 0.0016(12) C71 0.0188(15) 0.0226(15) 0.0283(16) -0.0070(13) -0.0033(12) -0.0022(12) C72 0.0339(19) 0.0270(17) 0.0337(18) -0.0005(14) -0.0122(15) -0.0060(14) C75 0.0251(17) 0.0219(15) 0.0317(17) -0.0052(13) -0.0112(14) 0.0026(13) C81 0.0197(16) 0.0316(17) 0.0226(15) -0.0066(13) -0.0029(12) -0.0048(13) C82 0.0191(16) 0.0331(17) 0.0256(16) -0.0024(13) 0.0018(13) 0.0032(13) C83 0.0149(14) 0.0266(16) 0.0208(14) -0.0028(12) -0.0059(12) -0.0031(12) C84 0.0224(16) 0.0237(15) 0.0216(15) -0.0047(12) -0.0008(12) -0.0056(12) C85 0.0310(18) 0.0352(18) 0.0307(17) -0.0108(15) 0.0040(14) -0.0163(15) C86 0.048(2) 0.0288(18) 0.0380(19) -0.0131(15) 0.0044(17) -0.0206(16) C87 0.0373(19) 0.0211(16) 0.0319(17) -0.0106(13) 0.0027(15) -0.0073(14) C88 0.0268(16) 0.0193(15) 0.0211(15) -0.0048(12) -0.0014(12) -0.0013(12) C89 0.0241(16) 0.0142(14) 0.0248(15) -0.0052(12) -0.0028(12) 0.0012(12) C90 0.0281(17) 0.0192(15) 0.0208(15) -0.0071(12) -0.0031(13) 0.0041(13) C91 0.0277(17) 0.0192(15) 0.0284(16) -0.0074(13) 0.0034(13) 0.0023(13) C92 0.0322(18) 0.0173(14) 0.0204(14) -0.0067(12) -0.0026(13) 0.0055(13) C93 0.0347(19) 0.0251(16) 0.0327(18) -0.0134(14) -0.0017(15) 0.0020(14) C94 0.044(2) 0.0274(17) 0.043(2) -0.0228(16) -0.0005(17) 0.0049(16) C95 0.042(2) 0.0278(17) 0.0358(19) -0.0152(15) 0.0006(16) 0.0118(15) C96 0.0282(18) 0.0270(17) 0.0323(17) -0.0094(14) -0.0012(14) 0.0067(14) C97 0.0331(18) 0.0193(15) 0.0237(15) -0.0078(12) -0.0044(13) 0.0053(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 La1 O3 2.420(2) . ? La1 O2 2.4463(19) . ? La1 O1 2.4954(19) . ? La1 N3 2.686(2) . ? La1 N4 2.686(2) . ? La1 N1 2.692(2) . ? La1 N6 2.693(2) . ? La1 N2 2.697(2) . ? La1 N5 2.727(2) . ? O1 C15 1.256(4) . ? O2 C49 1.254(3) . ? O3 C83 1.253(4) . ? O4 C7 1.391(4) . ? O4 C13 1.439(3) . ? O5 C41 1.389(4) . ? O5 C47 1.438(3) . ? O6 C75 1.392(4) . ? O6 C81 1.444(4) . ? N1 C20 1.339(4) . ? N1 C16 1.349(4) . ? N2 C54 1.347(4) . ? N2 C50 1.354(4) . ? N3 C84 1.343(4) . ? N3 C88 1.348(4) . ? N4 C21 1.332(4) . ? N4 N7 1.342(3) . ? N5 C55 1.334(4) . ? N5 N8 1.339(3) . ? N6 C89 1.338(4) . ? N6 N9 1.343(4) . ? N7 C23 1.329(4) . ? N8 C57 1.330(4) . ? N9 C91 1.332(4) . ? N10 C22 1.324(4) . ? N10 C21 1.331(4) . ? N11 C56 1.328(4) . ? N11 C55 1.345(4) . ? N12 C90 1.326(4) . ? N12 C89 1.335(4) . ? N13 C15 1.315(4) . ? N13 C14 1.469(4) . ? N13 H13C 0.8800 . ? N14 C49 1.318(4) . ? N14 C48 1.461(4) . ? N14 H14C 0.8800 . ? N15 C83 1.312(4) . ? N15 C82 1.467(4) . ? N15 H15A 0.8800 . ? C1 C2 1.518(4) . ? C1 C36 1.528(4) . ? C1 C70 1.530(4) . ? C1 H1A 1.0000 . ? C2 C3 1.391(4) . ? C2 C7 1.398(4) . ? C3 C4 1.398(4) . ? C3 H3A 0.9500 . ? C4 C5 1.384(5) . ? C4 C8 1.500(9) . ? C4 C8' 1.597(11) . ? C5 C6 1.400(5) . ? C5 H5A 0.9500 . ? C6 C7 1.394(4) . ? C6 C12 1.503(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.500(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.506(4) . ? C16 C17 1.382(4) . ? C17 C18 1.393(4) . ? C17 H17A 0.9500 . ? C18 C19 1.383(4) . ? C18 H18A 0.9500 . ? C19 C20 1.397(4) . ? C19 H19A 0.9500 . ? C20 C21 1.482(4) . ? C22 C23 1.426(4) . ? C22 C24 1.480(4) . ? C23 C30 1.482(4) . ? C24 C29 1.397(4) . ? C24 C25 1.411(4) . ? C25 C26 1.384(4) . ? C25 H25A 0.9500 . ? C26 C27 1.389(4) . ? C26 H26A 0.9500 . ? C27 C28 1.390(5) . ? C27 H27A 0.9500 . ? C28 C29 1.383(4) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C35 1.392(4) . ? C30 C31 1.392(4) . ? C31 C32 1.389(4) . ? C31 H31A 0.9500 . ? C32 C33 1.377(5) . ? C32 H32A 0.9500 . ? C33 C34 1.392(5) . ? C33 H33A 0.9500 . ? C34 C35 1.391(5) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.392(4) . ? C36 C41 1.400(4) . ? C37 C38 1.397(4) . ? C37 H37A 0.9500 . ? C38 C39 1.386(4) . ? C38 C42 1.541(4) . ? C39 C40 1.396(5) . ? C39 H39A 0.9500 . ? C40 C41 1.391(4) . ? C40 C46 1.509(4) . ? C42 C45 1.425(15) . ? C42 C43' 1.480(13) . ? C42 C44' 1.504(8) . ? C42 C44 1.559(10) . ? C42 C43 1.582(13) . ? C42 C45' 1.587(8) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C43' H43D 0.9800 . ? C43' H43E 0.9800 . ? C43' H43F 0.9800 . ? C44' H44D 0.9800 . ? C44' H44E 0.9800 . ? C44' H44F 0.9800 . ? C45' H45D 0.9800 . ? C45' H45E 0.9800 . ? C45' H45F 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.506(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.499(4) . ? C50 C51 1.393(4) . ? C51 C52 1.384(4) . ? C51 H51A 0.9500 . ? C52 C53 1.380(4) . ? C52 H52A 0.9500 . ? C53 C54 1.389(4) . ? C53 H53A 0.9500 . ? C54 C55 1.482(4) . ? C56 C57 1.426(4) . ? C56 C58 1.491(4) . ? C57 C64 1.484(4) . ? C58 C59 1.392(4) . ? C58 C63' 1.402(10) . ? C58 C63 1.412(9) . ? C59 C60 1.387(5) . ? C59 H59A 0.9500 . ? C60 C61 1.384(5) . ? C60 H60A 0.9500 . ? C61 C62' 1.394(11) . ? C61 C62 1.416(10) . ? C61 H61A 0.9500 . ? C61 H61B 0.9502 . ? C64 C69' 1.344(9) . ? C64 C65 1.381(5) . ? C64 C69 1.469(10) . ? C65 C66 1.385(10) . ? C65 C66' 1.433(10) . ? C65 H65A 0.9500 . ? C65 H65B 0.9500 . ? C70 C71 1.383(4) . ? C70 C75 1.401(4) . ? C71 C72 1.388(4) . ? C71 H71A 0.9500 . ? C72 C73' 1.349(11) . ? C72 C73 1.444(7) . ? C72 C76 1.495(10) . ? C72 C76" 1.563(14) . ? C72 C76' 1.704(15) . ? C75 C74 1.374(6) . ? C75 C74' 1.473(12) . ? C73 C74 1.407(8) . ? C73 H73A 0.9500 . ? C74 C80 1.504(8) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C73' C74' 1.400(15) . ? C73' H73B 0.9500 . ? C74' C80' 1.543(14) . ? C80' H80D 0.9800 . ? C80' H80E 0.9800 . ? C80' H80F 0.9800 . ? C76 C77 1.512(15) . ? C76 C79 1.548(9) . ? C76 C78 1.599(18) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C76' C77' 1.540(5) . ? C76' C78' 1.540(5) . ? C76' C79' 1.541(5) . ? C77' H77D 0.9800 . ? C77' H77E 0.9800 . ? C77' H77F 0.9800 . ? C78' H78D 0.9800 . ? C78' H78E 0.9800 . ? C78' H78F 0.9800 . ? C79' H79D 0.9800 . ? C79' H79E 0.9800 . ? C79' H79F 0.9800 . ? C76" C77" 1.540(5) . ? C76" C79" 1.541(5) . ? C76" C78" 1.541(5) . ? C77" H77G 0.9800 . ? C77" H77H 0.9800 . ? C77" H77I 0.9800 . ? C78" H78G 0.9800 . ? C78" H78H 0.9800 . ? C78" H78I 0.9800 . ? C79" H79G 0.9800 . ? C79" H79H 0.9800 . ? C79" H79I 0.9800 . ? C81 C82 1.511(4) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.509(4) . ? C84 C85 1.388(4) . ? C85 C86 1.387(5) . ? C85 H85A 0.9500 . ? C86 C87 1.392(5) . ? C86 H86A 0.9500 . ? C87 C88 1.394(4) . ? C87 H87A 0.9500 . ? C88 C89 1.484(4) . ? C90 C91 1.429(4) . ? C90 C92 1.479(4) . ? C91 C200 1.484(7) . ? C91 C98 1.511(8) . ? C92 C97 1.394(5) . ? C92 C93 1.395(4) . ? C93 C94 1.395(5) . ? C93 H93A 0.9500 . ? C94 C95 1.388(5) . ? C94 H94A 0.9500 . ? C95 C96 1.384(5) . ? C95 H95A 0.9500 . ? C96 C97 1.390(4) . ? C96 H96A 0.9500 . ? C97 H97A 0.9500 . ? C8 C10 1.537(12) . ? C8 C11 1.539(12) . ? C8 C9 1.547(13) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C8' C9' 1.503(14) . ? C8' C10' 1.531(15) . ? C8' C11' 1.566(13) . ? C9' H9'A 0.9800 . ? C9' H9'B 0.9800 . ? C9' H9'C 0.9800 . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C66 C67 1.440(13) . ? C66 H66A 0.9500 . ? C67 C68 1.355(13) . ? C67 H67A 0.9500 . ? C68 C69 1.394(12) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? C66' C67' 1.363(12) . ? C66' H66B 0.9500 . ? C67' C68' 1.370(13) . ? C67' H67B 0.9500 . ? C68' C69' 1.393(12) . ? C68' H68B 0.9500 . ? C69' H69B 0.9500 . ? C62 C63 1.390(12) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? C62' C63' 1.366(13) . ? C62' H62B 0.9500 . ? C63' H63B 0.9500 . ? C98 C103 1.381(12) . ? C98 C99 1.417(11) . ? C99 C100 1.419(14) . ? C99 H99A 0.9500 . ? C100 C101 1.355(16) . ? C100 H10G 0.9500 . ? C101 C102 1.410(15) . ? C101 H10H 0.9500 . ? C102 C103 1.380(11) . ? C102 H10I 0.9500 . ? C103 H10J 0.9500 . ? C200 C300 1.379(11) . ? C200 C700 1.406(10) . ? C300 C400 1.360(11) . ? C300 H30A 0.9500 . ? C400 C500 1.394(13) . ? C400 H40A 0.9500 . ? C500 C600 1.350(13) . ? C500 H50A 0.9500 . ? C600 C700 1.415(11) . ? C600 H60B 0.9500 . ? C700 H70A 0.9500 . ? La2 O7 2.5167 . ? La2 O10 2.5527 . ? La2 O11 2.5869 . ? La2 O8 2.6003 . ? La2 O23 2.6383 . ? La2 O16 2.6453 . ? La2 O20 2.6549 . ? La2 O13 2.6703 . ? La2 O22 2.6740 . ? La2 O17 2.6746 . ? La2 O19 2.7127 . ? La2 O14 2.7396 . ? O7 N16 1.2925 . ? O8 N16 1.3153 . ? O9 N16 1.2347 . ? O10 N17 1.2947 . ? O11 N17 1.2434 . ? O12 N17 1.2424 . ? O13 N18 1.2493 . ? O14 N18 1.2717 . ? O15 N18 1.2321 . ? O16 N19 1.3170 . ? O17 N19 1.2029 . ? O18 N19 1.2577 . ? O19 N20 1.1654 . ? O20 N20 1.3087 . ? O21 N20 1.2469 . ? O22 N21 1.2471 . ? O23 N21 1.2821 . ? O24 N21 1.2515 . ? La2' O16' 2.5387 . ? La2' O22' 2.5569 . ? La2' O20' 2.5652 . ? La2' O19' 2.6054 . ? La2' O14' 2.6137 . ? La2' O23' 2.6213 . ? La2' O17' 2.6280 . ? La2' O13' 2.6644 . ? La2' O8' 2.7034 . ? La2' O7' 2.9511 . ? La2' N19' 2.9819 . ? La2' N21' 3.0357 . ? O7' N16' 1.2784 . ? O8' N16' 1.2721 . ? O9' N16' 1.2158 . ? O10' N17' 1.2786 . ? O11' N17' 1.3139 . ? O12' N17' 1.1601 . ? O13' N18' 1.3701 . ? O14' N18' 1.1881 . ? O15' N18' 1.2296 . ? O16' N19' 1.2443 . ? O17' N19' 1.3992 . ? O18' N19' 1.2391 . ? O19' N20' 1.4581 . ? O20' N20' 1.2215 . ? O21' N20' 1.1936 . ? O22' N21' 1.2252 . ? O23' N21' 1.3846 . ? O24' N21' 1.1755 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 La1 O2 82.70(7) . . ? O3 La1 O1 81.74(7) . . ? O2 La1 O1 86.50(7) . . ? O3 La1 N3 62.21(7) . . ? O2 La1 N3 142.65(7) . . ? O1 La1 N3 76.69(7) . . ? O3 La1 N4 152.44(7) . . ? O2 La1 N4 84.37(7) . . ? O1 La1 N4 121.63(7) . . ? N3 La1 N4 132.82(7) . . ? O3 La1 N1 140.86(7) . . ? O2 La1 N1 82.35(7) . . ? O1 La1 N1 61.42(7) . . ? N3 La1 N1 116.35(7) . . ? N4 La1 N1 60.24(7) . . ? O3 La1 N6 122.09(7) . . ? O2 La1 N6 152.86(7) . . ? O1 La1 N6 86.56(7) . . ? N3 La1 N6 59.90(7) . . ? N4 La1 N6 77.10(7) . . ? N1 La1 N6 71.30(7) . . ? O3 La1 N2 80.59(7) . . ? O2 La1 N2 61.65(7) . . ? O1 La1 N2 145.16(7) . . ? N3 La1 N2 119.68(7) . . ? N4 La1 N2 71.86(7) . . ? N1 La1 N2 122.17(7) . . ? N6 La1 N2 128.22(7) . . ? O3 La1 N5 89.40(7) . . ? O2 La1 N5 121.29(7) . . ? O1 La1 N5 149.61(7) . . ? N3 La1 N5 73.47(7) . . ? N4 La1 N5 76.77(7) . . ? N1 La1 N5 129.04(7) . . ? N6 La1 N5 73.66(7) . . ? N2 La1 N5 59.66(7) . . ? C15 O1 La1 126.77(18) . . ? C49 O2 La1 127.99(18) . . ? C83 O3 La1 126.12(19) . . ? C7 O4 C13 115.8(2) . . ? C41 O5 C47 111.6(2) . . ? C75 O6 C81 115.1(2) . . ? C20 N1 C16 118.1(2) . . ? C20 N1 La1 122.59(18) . . ? C16 N1 La1 118.82(18) . . ? C54 N2 C50 117.9(2) . . ? C54 N2 La1 123.96(18) . . ? C50 N2 La1 118.10(17) . . ? C84 N3 C88 118.7(3) . . ? C84 N3 La1 117.46(19) . . ? C88 N3 La1 123.57(19) . . ? C21 N4 N7 118.0(2) . . ? C21 N4 La1 122.72(18) . . ? N7 N4 La1 117.25(17) . . ? C55 N5 N8 118.5(2) . . ? C55 N5 La1 122.21(18) . . ? N8 N5 La1 117.61(17) . . ? C89 N6 N9 117.9(2) . . ? C89 N6 La1 122.90(19) . . ? N9 N6 La1 116.53(17) . . ? C23 N7 N4 119.3(2) . . ? C57 N8 N5 119.7(3) . . ? C91 N9 N6 119.3(3) . . ? C22 N10 C21 117.7(2) . . ? C56 N11 C55 116.5(3) . . ? C90 N12 C89 117.4(3) . . ? C15 N13 C14 123.1(3) . . ? C15 N13 H13C 118.4 . . ? C14 N13 H13C 118.4 . . ? C49 N14 C48 122.1(2) . . ? C49 N14 H14C 119.0 . . ? C48 N14 H14C 119.0 . . ? C83 N15 C82 121.9(3) . . ? C83 N15 H15A 119.0 . . ? C82 N15 H15A 119.0 . . ? C2 C1 C36 113.8(2) . . ? C2 C1 C70 112.3(2) . . ? C36 C1 C70 110.9(2) . . ? C2 C1 H1A 106.4 . . ? C36 C1 H1A 106.4 . . ? C70 C1 H1A 106.4 . . ? C3 C2 C7 118.1(3) . . ? C3 C2 C1 122.9(3) . . ? C7 C2 C1 119.0(3) . . ? C2 C3 C4 122.2(3) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C5 C4 C3 117.5(3) . . ? C5 C4 C8 116.7(6) . . ? C3 C4 C8 125.6(6) . . ? C5 C4 C8' 127.4(6) . . ? C3 C4 C8' 115.1(6) . . ? C8 C4 C8' 11.6(5) . . ? C4 C5 C6 122.8(3) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C7 C6 C5 117.5(3) . . ? C7 C6 C12 121.7(3) . . ? C5 C6 C12 120.7(3) . . ? O4 C7 C6 119.6(3) . . ? O4 C7 C2 118.4(3) . . ? C6 C7 C2 121.9(3) . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 C14 106.3(2) . . ? O4 C13 H13A 110.5 . . ? C14 C13 H13A 110.5 . . ? O4 C13 H13B 110.5 . . ? C14 C13 H13B 110.5 . . ? H13A C13 H13B 108.7 . . ? N13 C14 C13 109.5(2) . . ? N13 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? N13 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? O1 C15 N13 123.5(3) . . ? O1 C15 C16 118.6(2) . . ? N13 C15 C16 117.9(3) . . ? N1 C16 C17 122.8(3) . . ? N1 C16 C15 113.1(2) . . ? C17 C16 C15 124.1(3) . . ? C16 C17 C18 118.5(3) . . ? C16 C17 H17A 120.8 . . ? C18 C17 H17A 120.8 . . ? C19 C18 C17 119.5(3) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C18 C19 C20 118.2(3) . . ? C18 C19 H19A 120.9 . . ? C20 C19 H19A 120.9 . . ? N1 C20 C19 122.9(3) . . ? N1 C20 C21 116.7(2) . . ? C19 C20 C21 120.3(3) . . ? N10 C21 N4 124.9(3) . . ? N10 C21 C20 117.6(2) . . ? N4 C21 C20 117.5(2) . . ? N10 C22 C23 118.1(3) . . ? N10 C22 C24 116.8(3) . . ? C23 C22 C24 125.1(3) . . ? N7 C23 C22 120.4(3) . . ? N7 C23 C30 114.8(3) . . ? C22 C23 C30 124.8(3) . . ? C29 C24 C25 118.6(3) . . ? C29 C24 C22 123.6(3) . . ? C25 C24 C22 117.8(3) . . ? C26 C25 C24 120.1(3) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C25 C26 C27 120.6(3) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C26 C27 C28 119.6(3) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C28 C29 C24 120.7(3) . . ? C28 C29 H29A 119.7 . . ? C24 C29 H29A 119.7 . . ? C35 C30 C31 120.2(3) . . ? C35 C30 C23 119.1(3) . . ? C31 C30 C23 120.7(3) . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? C33 C32 C31 120.0(3) . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 C34 120.6(3) . . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 119.7 . . ? C35 C34 C33 119.8(3) . . ? C35 C34 H34A 120.1 . . ? C33 C34 H34A 120.1 . . ? C34 C35 C30 119.6(3) . . ? C34 C35 H35A 120.2 . . ? C30 C35 H35A 120.2 . . ? C37 C36 C41 118.0(3) . . ? C37 C36 C1 123.2(3) . . ? C41 C36 C1 118.5(3) . . ? C36 C37 C38 122.0(3) . . ? C36 C37 H37A 119.0 . . ? C38 C37 H37A 119.0 . . ? C39 C38 C37 117.8(3) . . ? C39 C38 C42 122.3(3) . . ? C37 C38 C42 119.6(3) . . ? C38 C39 C40 122.3(3) . . ? C38 C39 H39A 118.9 . . ? C40 C39 H39A 118.9 . . ? C41 C40 C39 118.1(3) . . ? C41 C40 C46 120.0(3) . . ? C39 C40 C46 121.7(3) . . ? O5 C41 C40 119.6(3) . . ? O5 C41 C36 118.9(3) . . ? C40 C41 C36 121.4(3) . . ? C45 C42 C43' 112.9(8) . . ? C45 C42 C44' 91.9(8) . . ? C43' C42 C44' 109.6(6) . . ? C45 C42 C38 112.3(7) . . ? C43' C42 C38 114.5(6) . . ? C44' C42 C38 113.5(4) . . ? C45 C42 C44 108.9(8) . . ? C43' C42 C44 100.3(6) . . ? C44' C42 C44 17.0(4) . . ? C38 C42 C44 106.9(5) . . ? C45 C42 C43 112.0(8) . . ? C43' C42 C43 5.4(9) . . ? C44' C42 C43 115.0(6) . . ? C38 C42 C43 110.9(5) . . ? C44 C42 C43 105.4(7) . . ? C45 C42 C45' 14.1(8) . . ? C43' C42 C45' 106.7(6) . . ? C44' C42 C45' 106.0(5) . . ? C38 C42 C45' 105.8(3) . . ? C44 C42 C45' 122.9(6) . . ? C43 C42 C45' 104.6(5) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C43' H43D 109.5 . . ? C42 C43' H43E 109.5 . . ? H43D C43' H43E 109.5 . . ? C42 C43' H43F 109.5 . . ? H43D C43' H43F 109.5 . . ? H43E C43' H43F 109.5 . . ? C42 C44' H44D 109.5 . . ? C42 C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C42 C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? C42 C45' H45D 109.5 . . ? C42 C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? C42 C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? C40 C46 H46A 109.5 . . ? C40 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C40 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O5 C47 C48 107.3(2) . . ? O5 C47 H47A 110.2 . . ? C48 C47 H47A 110.2 . . ? O5 C47 H47B 110.2 . . ? C48 C47 H47B 110.2 . . ? H47A C47 H47B 108.5 . . ? N14 C48 C47 110.8(2) . . ? N14 C48 H48A 109.5 . . ? C47 C48 H48A 109.5 . . ? N14 C48 H48B 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 108.1 . . ? O2 C49 N14 122.2(3) . . ? O2 C49 C50 119.0(2) . . ? N14 C49 C50 118.8(3) . . ? N2 C50 C51 122.2(3) . . ? N2 C50 C49 113.2(2) . . ? C51 C50 C49 124.6(3) . . ? C52 C51 C50 119.1(3) . . ? C52 C51 H51A 120.4 . . ? C50 C51 H51A 120.4 . . ? C53 C52 C51 119.0(3) . . ? C53 C52 H52A 120.5 . . ? C51 C52 H52A 120.5 . . ? C52 C53 C54 119.1(3) . . ? C52 C53 H53A 120.4 . . ? C54 C53 H53A 120.4 . . ? N2 C54 C53 122.6(3) . . ? N2 C54 C55 116.0(2) . . ? C53 C54 C55 121.4(3) . . ? N5 C55 N11 125.0(3) . . ? N5 C55 C54 117.8(3) . . ? N11 C55 C54 117.2(3) . . ? N11 C56 C57 119.6(3) . . ? N11 C56 C58 116.3(3) . . ? C57 C56 C58 124.0(3) . . ? N8 C57 C56 119.9(3) . . ? N8 C57 C64 114.6(3) . . ? C56 C57 C64 125.5(3) . . ? C59 C58 C63' 119.1(5) . . ? C59 C58 C63 119.8(4) . . ? C63' C58 C63 14.9(5) . . ? C59 C58 C56 118.6(3) . . ? C63' C58 C56 120.9(5) . . ? C63 C58 C56 121.5(4) . . ? C60 C59 C58 120.1(3) . . ? C60 C59 H59A 120.0 . . ? C58 C59 H59A 120.0 . . ? C61 C60 C59 119.9(3) . . ? C61 C60 H60A 120.1 . . ? C59 C60 H60A 120.1 . . ? C60 C61 C62' 119.2(5) . . ? C60 C61 C62 120.5(4) . . ? C62' C61 C62 16.3(5) . . ? C60 C61 H61A 119.8 . . ? C62' C61 H61A 118.4 . . ? C62 C61 H61A 119.8 . . ? C60 C61 H61B 120.1 . . ? C62' C61 H61B 120.7 . . ? C62 C61 H61B 117.4 . . ? H61A C61 H61B 14.5 . . ? C69' C64 C65 113.7(6) . . ? C69' C64 C69 14.0(5) . . ? C65 C64 C69 126.7(6) . . ? C69' C64 C57 125.2(6) . . ? C65 C64 C57 120.8(3) . . ? C69 C64 C57 112.5(6) . . ? C64 C65 C66 113.3(6) . . ? C64 C65 C66' 124.6(5) . . ? C66 C65 C66' 19.0(5) . . ? C64 C65 H65A 123.4 . . ? C66 C65 H65A 123.4 . . ? C66' C65 H65A 110.1 . . ? C64 C65 H65B 117.5 . . ? C66 C65 H65B 126.2 . . ? C66' C65 H65B 117.9 . . ? H65A C65 H65B 16.8 . . ? C71 C70 C75 119.1(3) . . ? C71 C70 C1 122.2(3) . . ? C75 C70 C1 118.6(3) . . ? C70 C71 C72 122.3(3) . . ? C70 C71 H71A 118.9 . . ? C72 C71 H71A 118.9 . . ? C73' C72 C71 119.6(5) . . ? C73' C72 C73 20.1(5) . . ? C71 C72 C73 115.6(3) . . ? C73' C72 C76 119.2(6) . . ? C71 C72 C76 120.3(4) . . ? C73 C72 C76 123.1(5) . . ? C73' C72 C76" 119.4(7) . . ? C71 C72 C76" 121.0(5) . . ? C73 C72 C76" 120.1(6) . . ? C76 C72 C76" 7.9(9) . . ? C73' C72 C76' 120.6(7) . . ? C71 C72 C76' 115.1(5) . . ? C73 C72 C76' 129.2(5) . . ? C76 C72 C76' 12.6(7) . . ? C76" C72 C76' 20.4(7) . . ? C74 C75 O6 117.5(4) . . ? C74 C75 C70 122.7(3) . . ? O6 C75 C70 118.8(3) . . ? C74 C75 C74' 18.2(5) . . ? O6 C75 C74' 124.5(5) . . ? C70 C75 C74' 116.2(5) . . ? C74 C73 C72 123.3(5) . . ? C74 C73 H73A 118.3 . . ? C72 C73 H73A 118.3 . . ? C75 C74 C73 116.2(5) . . ? C75 C74 C80 124.0(5) . . ? C73 C74 C80 119.8(5) . . ? C74 C80 H80A 109.5 . . ? C74 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C74 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C72 C73' C74' 118.9(9) . . ? C72 C73' H73B 120.5 . . ? C74' C73' H73B 120.5 . . ? C73' C74' C75 120.7(9) . . ? C73' C74' C80' 122.5(10) . . ? C75 C74' C80' 116.5(8) . . ? C74' C80' H80D 109.5 . . ? C74' C80' H80E 109.5 . . ? H80D C80' H80E 109.5 . . ? C74' C80' H80F 109.5 . . ? H80D C80' H80F 109.5 . . ? H80E C80' H80F 109.5 . . ? C72 C76 C77 110.2(9) . . ? C72 C76 C79 113.8(6) . . ? C77 C76 C79 104.2(10) . . ? C72 C76 C78 110.1(10) . . ? C77 C76 C78 109.3(7) . . ? C79 C76 C78 109.1(9) . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C76 C79 H79A 109.5 . . ? C76 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C76 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C77' C76' C78' 111.1(5) . . ? C77' C76' C79' 111.1(5) . . ? C78' C76' C79' 110.9(5) . . ? C77' C76' C72 99.6(8) . . ? C78' C76' C72 115.1(10) . . ? C79' C76' C72 108.6(8) . . ? C76' C77' H77D 109.5 . . ? C76' C77' H77E 109.5 . . ? H77D C77' H77E 109.5 . . ? C76' C77' H77F 109.5 . . ? H77D C77' H77F 109.5 . . ? H77E C77' H77F 109.5 . . ? C76' C78' H78D 109.5 . . ? C76' C78' H78E 109.5 . . ? H78D C78' H78E 109.5 . . ? C76' C78' H78F 109.5 . . ? H78D C78' H78F 109.5 . . ? H78E C78' H78F 109.5 . . ? C76' C79' H79D 109.5 . . ? C76' C79' H79E 109.5 . . ? H79D C79' H79E 109.5 . . ? C76' C79' H79F 109.5 . . ? H79D C79' H79F 109.5 . . ? H79E C79' H79F 109.5 . . ? C77" C76" C79" 110.9(5) . . ? C77" C76" C78" 111.0(5) . . ? C79" C76" C78" 111.0(5) . . ? C77" C76" C72 111.2(10) . . ? C79" C76" C72 111.7(10) . . ? C78" C76" C72 100.6(11) . . ? C76" C77" H77G 109.5 . . ? C76" C77" H77H 109.5 . . ? H77G C77" H77H 109.5 . . ? C76" C77" H77I 109.5 . . ? H77G C77" H77I 109.5 . . ? H77H C77" H77I 109.5 . . ? C76" C78" H78G 109.5 . . ? C76" C78" H78H 109.5 . . ? H78G C78" H78H 109.5 . . ? C76" C78" H78I 109.5 . . ? H78G C78" H78I 109.5 . . ? H78H C78" H78I 109.5 . . ? C76" C79" H79G 109.5 . . ? C76" C79" H79H 109.5 . . ? H79G C79" H79H 109.5 . . ? C76" C79" H79I 109.5 . . ? H79G C79" H79I 109.5 . . ? H79H C79" H79I 109.5 . . ? O6 C81 C82 107.4(2) . . ? O6 C81 H81A 110.2 . . ? C82 C81 H81A 110.2 . . ? O6 C81 H81B 110.2 . . ? C82 C81 H81B 110.2 . . ? H81A C81 H81B 108.5 . . ? N15 C82 C81 110.9(3) . . ? N15 C82 H82A 109.4 . . ? C81 C82 H82A 109.4 . . ? N15 C82 H82B 109.4 . . ? C81 C82 H82B 109.4 . . ? H82A C82 H82B 108.0 . . ? O3 C83 N15 122.9(3) . . ? O3 C83 C84 118.3(3) . . ? N15 C83 C84 118.8(3) . . ? N3 C84 C85 122.2(3) . . ? N3 C84 C83 112.4(3) . . ? C85 C84 C83 125.4(3) . . ? C86 C85 C84 119.0(3) . . ? C86 C85 H85A 120.5 . . ? C84 C85 H85A 120.5 . . ? C85 C86 C87 119.3(3) . . ? C85 C86 H86A 120.3 . . ? C87 C86 H86A 120.3 . . ? C86 C87 C88 118.2(3) . . ? C86 C87 H87A 120.9 . . ? C88 C87 H87A 120.9 . . ? N3 C88 C87 122.5(3) . . ? N3 C88 C89 115.9(3) . . ? C87 C88 C89 121.6(3) . . ? N12 C89 N6 124.5(3) . . ? N12 C89 C88 118.2(3) . . ? N6 C89 C88 117.2(3) . . ? N12 C90 C91 118.3(3) . . ? N12 C90 C92 117.7(3) . . ? C91 C90 C92 123.9(3) . . ? N9 C91 C90 119.8(3) . . ? N9 C91 C200 118.3(4) . . ? C90 C91 C200 121.2(4) . . ? N9 C91 C98 112.6(4) . . ? C90 C91 C98 127.0(4) . . ? C200 C91 C98 16.7(3) . . ? C97 C92 C93 119.7(3) . . ? C97 C92 C90 121.2(3) . . ? C93 C92 C90 118.9(3) . . ? C92 C93 C94 119.6(3) . . ? C92 C93 H93A 120.2 . . ? C94 C93 H93A 120.2 . . ? C95 C94 C93 120.1(3) . . ? C95 C94 H94A 120.0 . . ? C93 C94 H94A 120.0 . . ? C96 C95 C94 120.5(3) . . ? C96 C95 H95A 119.8 . . ? C94 C95 H95A 119.8 . . ? C95 C96 C97 119.7(3) . . ? C95 C96 H96A 120.2 . . ? C97 C96 H96A 120.2 . . ? C96 C97 C92 120.4(3) . . ? C96 C97 H97A 119.8 . . ? C92 C97 H97A 119.8 . . ? C4 C8 C10 109.8(6) . . ? C4 C8 C11 115.3(7) . . ? C10 C8 C11 106.3(7) . . ? C4 C8 C9 106.8(7) . . ? C10 C8 C9 111.0(8) . . ? C11 C8 C9 107.7(7) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9' C8' C10' 105.7(9) . . ? C9' C8' C11' 110.5(8) . . ? C10' C8' C11' 110.8(8) . . ? C9' C8' C4 115.6(8) . . ? C10' C8' C4 107.0(7) . . ? C11' C8' C4 107.2(7) . . ? C8' C9' H9'A 109.5 . . ? C8' C9' H9'B 109.5 . . ? H9'A C9' H9'B 109.5 . . ? C8' C9' H9'C 109.5 . . ? H9'A C9' H9'C 109.5 . . ? H9'B C9' H9'C 109.5 . . ? C8' C10' H10D 109.5 . . ? C8' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C8' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C8' C11' H11D 109.5 . . ? C8' C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C8' C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C65 C66 C67 122.3(8) . . ? C65 C66 H66A 118.8 . . ? C67 C66 H66A 118.8 . . ? C68 C67 C66 121.2(8) . . ? C68 C67 H67A 119.4 . . ? C66 C67 H67A 119.4 . . ? C67 C68 C69 120.5(8) . . ? C67 C68 H68A 119.7 . . ? C69 C68 H68A 119.7 . . ? C68 C69 C64 115.1(9) . . ? C68 C69 H69A 122.5 . . ? C64 C69 H69A 122.5 . . ? C67' C66' C65 115.9(8) . . ? C67' C66' H66B 122.0 . . ? C65 C66' H66B 122.0 . . ? C66' C67' C68' 120.7(8) . . ? C66' C67' H67B 119.6 . . ? C68' C67' H67B 119.6 . . ? C67' C68' C69' 118.8(8) . . ? C67' C68' H68B 120.6 . . ? C69' C68' H68B 120.6 . . ? C64 C69' C68' 125.0(9) . . ? C64 C69' H69B 117.5 . . ? C68' C69' H69B 117.5 . . ? C63 C62 C61 118.9(7) . . ? C63 C62 H62A 120.5 . . ? C61 C62 H62A 120.5 . . ? C62 C63 C58 119.7(7) . . ? C62 C63 H63A 120.2 . . ? C58 C63 H63A 120.2 . . ? C63' C62' C61 120.6(8) . . ? C63' C62' H62B 119.7 . . ? C61 C62' H62B 119.7 . . ? C62' C63' C58 119.9(8) . . ? C62' C63' H63B 120.1 . . ? C58 C63' H63B 120.1 . . ? C103 C98 C99 119.5(7) . . ? C103 C98 C91 125.8(7) . . ? C99 C98 C91 114.6(7) . . ? C98 C99 C100 121.2(9) . . ? C98 C99 H99A 119.4 . . ? C100 C99 H99A 119.4 . . ? C101 C100 C99 117.1(9) . . ? C101 C100 H10G 121.5 . . ? C99 C100 H10G 121.5 . . ? C100 C101 C102 122.5(10) . . ? C100 C101 H10H 118.8 . . ? C102 C101 H10H 118.8 . . ? C103 C102 C101 120.1(9) . . ? C103 C102 H10I 119.9 . . ? C101 C102 H10I 119.9 . . ? C102 C103 C98 119.6(8) . . ? C102 C103 H10J 120.2 . . ? C98 C103 H10J 120.2 . . ? C300 C200 C700 120.6(7) . . ? C300 C200 C91 122.8(6) . . ? C700 C200 C91 116.5(6) . . ? C400 C300 C200 118.3(8) . . ? C400 C300 H30A 120.9 . . ? C200 C300 H30A 120.9 . . ? C300 C400 C500 121.1(8) . . ? C300 C400 H40A 119.4 . . ? C500 C400 H40A 119.4 . . ? C600 C500 C400 122.9(9) . . ? C600 C500 H50A 118.6 . . ? C400 C500 H50A 118.6 . . ? C500 C600 C700 116.5(8) . . ? C500 C600 H60B 121.8 . . ? C700 C600 H60B 121.8 . . ? C200 C700 C600 120.6(7) . . ? C200 C700 H70A 119.7 . . ? C600 C700 H70A 119.7 . . ? O7 La2 O10 72.0 . . ? O7 La2 O11 110.0 . . ? O10 La2 O11 49.9 . . ? O7 La2 O8 52.9 . . ? O10 La2 O8 69.4 . . ? O11 La2 O8 70.8 . . ? O7 La2 O23 67.3 . . ? O10 La2 O23 112.7 . . ? O11 La2 O23 159.5 . . ? O8 La2 O23 116.5 . . ? O7 La2 O16 130.4 . . ? O10 La2 O16 109.0 . . ? O11 La2 O16 105.4 . . ? O8 La2 O16 176.1 . . ? O23 La2 O16 67.3 . . ? O7 La2 O20 111.6 . . ? O10 La2 O20 176.3 . . ? O11 La2 O20 126.9 . . ? O8 La2 O20 112.0 . . ? O23 La2 O20 69.9 . . ? O16 La2 O20 69.4 . . ? O7 La2 O13 114.0 . . ? O10 La2 O13 109.4 . . ? O11 La2 O13 65.1 . . ? O8 La2 O13 66.0 . . ? O23 La2 O13 135.3 . . ? O16 La2 O13 111.9 . . ? O20 La2 O13 68.7 . . ? O7 La2 O22 65.7 . . ? O10 La2 O22 67.4 . . ? O11 La2 O22 111.9 . . ? O8 La2 O22 112.5 . . ? O23 La2 O22 47.8 . . ? O16 La2 O22 69.4 . . ? O20 La2 O22 114.4 . . ? O13 La2 O22 176.8 . . ? O7 La2 O17 126.6 . . ? O10 La2 O17 65.2 . . ? O11 La2 O17 63.1 . . ? O8 La2 O17 129.2 . . ? O23 La2 O17 101.3 . . ? O16 La2 O17 47.8 . . ? O20 La2 O17 112.1 . . ? O13 La2 O17 109.3 . . ? O22 La2 O17 69.3 . . ? O7 La2 O19 68.1 . . ? O10 La2 O19 136.3 . . ? O11 La2 O19 132.5 . . ? O8 La2 O19 72.8 . . ? O23 La2 O19 66.7 . . ? O16 La2 O19 110.0 . . ? O20 La2 O19 46.7 . . ? O13 La2 O19 72.8 . . ? O22 La2 O19 109.6 . . ? O17 La2 O19 157.5 . . ? O7 La2 O14 160.9 . . ? O10 La2 O14 109.0 . . ? O11 La2 O14 62.6 . . ? O8 La2 O14 108.8 . . ? O23 La2 O14 126.2 . . ? O16 La2 O14 68.1 . . ? O20 La2 O14 67.3 . . ? O13 La2 O14 47.0 . . ? O22 La2 O14 133.0 . . ? O17 La2 O14 67.6 . . ? O19 La2 O14 103.1 . . ? N16 O7 La2 94.8 . . ? N16 O8 La2 90.5 . . ? N17 O10 La2 96.4 . . ? N17 O11 La2 96.1 . . ? N18 O13 La2 99.5 . . ? N18 O14 La2 95.5 . . ? N19 O16 La2 94.9 . . ? N19 O17 La2 96.5 . . ? N20 O19 La2 97.9 . . ? N20 O20 La2 96.8 . . ? N21 O22 La2 97.2 . . ? N21 O23 La2 98.0 . . ? O9 N16 O7 122.9 . . ? O9 N16 O8 115.2 . . ? O7 N16 O8 121.8 . . ? O9 N16 La2 176.4 . . ? O7 N16 La2 59.0 . . ? O8 N16 La2 62.8 . . ? O12 N17 O11 121.3 . . ? O12 N17 O10 121.4 . . ? O11 N17 O10 117.3 . . ? O12 N17 La2 172.5 . . ? O11 N17 La2 59.4 . . ? O10 N17 La2 58.1 . . ? O15 N18 O13 120.9 . . ? O15 N18 O14 120.9 . . ? O13 N18 O14 117.9 . . ? O17 N19 O18 126.2 . . ? O17 N19 O16 117.5 . . ? O18 N19 O16 116.2 . . ? O17 N19 La2 60.5 . . ? O18 N19 La2 166.6 . . ? O16 N19 La2 59.7 . . ? O19 N20 O21 121.0 . . ? O19 N20 O20 118.6 . . ? O21 N20 O20 120.3 . . ? O22 N21 O24 121.7 . . ? O22 N21 O23 116.8 . . ? O24 N21 O23 121.4 . . ? O16' La2' O22' 70.7 . . ? O16' La2' O20' 66.7 . . ? O22' La2' O20' 66.2 . . ? O16' La2' O19' 117.2 . . ? O22' La2' O19' 74.5 . . ? O20' La2' O19' 51.7 . . ? O16' La2' O14' 62.1 . . ? O22' La2' O14' 125.5 . . ? O20' La2' O14' 71.2 . . ? O19' La2' O14' 103.9 . . ? O16' La2' O23' 75.1 . . ? O22' La2' O23' 50.4 . . ? O20' La2' O23' 113.6 . . ? O19' La2' O23' 116.8 . . ? O14' La2' O23' 130.9 . . ? O16' La2' O17' 52.1 . . ? O22' La2' O17' 106.4 . . ? O20' La2' O17' 115.3 . . ? O19' La2' O17' 165.9 . . ? O14' La2' O17' 63.8 . . ? O23' La2' O17' 71.5 . . ? O16' La2' O13' 107.8 . . ? O22' La2' O13' 135.0 . . ? O20' La2' O13' 72.2 . . ? O19' La2' O13' 66.7 . . ? O14' La2' O13' 49.4 . . ? O23' La2' O13' 174.3 . . ? O17' La2' O13' 106.0 . . ? O16' La2' O8' 172.3 . . ? O22' La2' O8' 116.6 . . ? O20' La2' O8' 113.1 . . ? O19' La2' O8' 64.7 . . ? O14' La2' O8' 110.3 . . ? O23' La2' O8' 111.2 . . ? O17' La2' O8' 124.6 . . ? O13' La2' O8' 65.6 . . ? O16' La2' O7' 147.1 . . ? O22' La2' O7' 80.6 . . ? O20' La2' O7' 115.9 . . ? O19' La2' O7' 67.7 . . ? O14' La2' O7' 150.7 . . ? O23' La2' O7' 74.4 . . ? O17' La2' O7' 126.3 . . ? O13' La2' O7' 103.8 . . ? O8' La2' O7' 40.4 . . ? O16' La2' N19' 24.4 . . ? O22' La2' N19' 89.3 . . ? O20' La2' N19' 88.3 . . ? O19' La2' N19' 140.0 . . ? O14' La2' N19' 56.7 . . ? O23' La2' N19' 74.4 . . ? O17' La2' N19' 28.0 . . ? O13' La2' N19' 106.0 . . ? O8' La2' N19' 151.1 . . ? O7' La2' N19' 146.2 . . ? O16' La2' N21' 70.3 . . ? O22' La2' N21' 23.4 . . ? O20' La2' N21' 87.9 . . ? O19' La2' N21' 94.5 . . ? O14' La2' N21' 132.3 . . ? O23' La2' N21' 27.1 . . ? O17' La2' N21' 89.8 . . ? O13' La2' N21' 158.4 . . ? O8' La2' N21' 117.3 . . ? O7' La2' N21' 76.9 . . ? N19' La2' N21' 81.1 . . ? N16' O7' La2' 101.4 . . ? N16' O8' La2' 115.0 . . ? N18' O13' La2' 92.2 . . ? N18' O14' La2' 99.4 . . ? N19' O16' La2' 98.2 . . ? N19' O17' La2' 90.2 . . ? N20' O19' La2' 92.5 . . ? N20' O20' La2' 100.8 . . ? N21' O22' La2' 100.8 . . ? N21' O23' La2' 93.4 . . ? O9' N16' O8' 137.7 . . ? O9' N16' O7' 120.8 . . ? O8' N16' O7' 101.0 . . ? O12' N17' O10' 120.5 . . ? O12' N17' O11' 124.6 . . ? O10' N17' O11' 114.8 . . ? O14' N18' O15' 122.5 . . ? O14' N18' O13' 119.0 . . ? O15' N18' O13' 118.3 . . ? O14' N18' La2' 58.0 . . ? O15' N18' La2' 178.1 . . ? O13' N18' La2' 61.1 . . ? O18' N19' O16' 122.1 . . ? O18' N19' O17' 119.1 . . ? O16' N19' O17' 118.2 . . ? O18' N19' La2' 162.0 . . ? O16' N19' La2' 57.4 . . ? O17' N19' La2' 61.8 . . ? O21' N20' O20' 120.4 . . ? O21' N20' O19' 125.2 . . ? O20' N20' O19' 114.3 . . ? O21' N20' La2' 170.2 . . ? O20' N20' La2' 56.0 . . ? O19' N20' La2' 58.9 . . ? O24' N21' O22' 124.2 . . ? O24' N21' O23' 120.4 . . ? O22' N21' O23' 115.3 . . ? O24' N21' La2' 176.5 . . ? O22' N21' La2' 55.8 . . ? O23' N21' La2' 59.5 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.800 _refine_diff_density_min -1.233 _refine_diff_density_rms 0.081 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.003 0.000 1824 539 ' ' 2 0.500 0.000 0.000 21 4 ' ' _platon_squeeze_details ; ; data_er9 _database_code_depnum_ccdc_archive 'CCDC 889302' #TrackingRef 'web_deposit_cif_file_0_GaryGuillet_1349827043.gg9.cif' # # xray code for Er9 is gg9 # _vrf_CHEMW03_I ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: the solvent area, which included five ether and three methanol molecules, were removed using Platon/Squeeze. ; _vrf_THETM01_I ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Small crystal did not diffract to higher resolution ; _vrf_PLAT023_I ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.50 Deg. RESPONSE: Small crystal did not diffract to higher resolution ; _vrf_PLAT043_I ; PROBLEM: Check Reported Molecular Weight ................ 2460.97 RESPONSE: Solvents removed by SQUEEZE, see above ; _vrf_PLAT044_I ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: Density calculated using full crystal contents but not solvents ; _vrf_PLAT602_I ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: those are partial disordered atoms ; _audit_update_record ; 2012-09-24 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C103 H97 N15 O6 Er1, 3(NO3), 5(C4H10O1), 3(CH4O1)' _chemical_formula_sum 'C126 H159 Er N18 O23' _chemical_formula_weight 2460.97 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 21.310(2) _cell_length_b 21.575(2) _cell_length_c 25.924(2) _cell_angle_alpha 82.036(2) _cell_angle_beta 86.5700(10) _cell_angle_gamma 84.9750(10) _cell_volume 11744.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9795 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description blocks _exptl_crystal_colour clear _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5172 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 54385 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.79 _diffrn_reflns_theta_max 22.50 _reflns_number_total 30261 _reflns_number_gt 22824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT (Bruker, 2008)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The following restraints were employed in the final refinement model. Er9 isor 0.1 c84 c85 c86 c87 c88 isor 0.1 c49a c15a c83a eadp c84 c85 c86 c87 c88 eadp c49a c15a c83a dfix 1.54 c8a c9a c8a c10a c8a c11a dfix 2.60 c9a c10a c9a c11a c10a c11a dfix 1.54 c8a c9b c8a c10b c8a c11b dfix 2.60 c9b c10b c9b c11b c10b c11b dfix 1.54 c8 c9 c8 c10 c8 c11 dfix 2.60 c9 c10 c9 c11 c10 c11 dfix 1.54 c8 c9' c8 c10' c8 c11' dfix 2.60 c9' c10' c9' c11' c10' c11' dfix 1.54 c76a c77a c76a c77b c76a c78a c76a c78b c76a c79a c76a c79b dfix 2.60 c77a c78a c77a c79a c79a c78a dfix 2.60 c77b c78b c77b c79b c79b c78b dfix 1.24 n16 o9 n16 o8 n16 o7 dfix 2.15 o7 o8 o7 o9 o8 o9 dfix 1.24 n21 o22 n21 o23 n21 o24 dfix 2.15 o22 o23 o22 o24 o23 o24 ; _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^)+(0.0902P)^2^+10.7703P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 30261 _refine_ls_number_parameters 2393 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1521 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 1.051237(12) 0.509984(12) 0.768977(11) 0.02500(10) Uani 1 1 d . . . N1 N 0.9804(2) 0.5733(2) 0.82603(19) 0.0270(12) Uani 1 1 d . . . N2 N 1.0380(2) 0.5163(2) 0.67398(19) 0.0258(11) Uani 1 1 d . . . N3 N 1.1409(2) 0.4442(2) 0.81061(19) 0.0258(11) Uani 1 1 d . . . N4 N 1.0286(2) 0.6248(2) 0.73438(19) 0.0264(12) Uani 1 1 d . . . N5 N 1.1481(2) 0.5295(2) 0.7097(2) 0.0303(12) Uani 1 1 d . . . N6 N 1.1213(2) 0.5645(2) 0.82008(19) 0.0289(12) Uani 1 1 d . . . N7 N 1.0480(2) 0.6480(2) 0.6858(2) 0.0316(12) Uani 1 1 d . . . N8 N 1.2053(2) 0.5265(2) 0.7295(2) 0.0341(13) Uani 1 1 d . . . N9 N 1.1052(2) 0.6241(2) 0.8292(2) 0.0335(13) Uani 1 1 d . . . N10 N 0.9816(2) 0.7260(2) 0.74880(19) 0.0283(12) Uani 1 1 d . . . N11 N 1.1918(2) 0.5551(2) 0.6241(2) 0.0306(12) Uani 1 1 d . . . N12 N 1.2100(2) 0.5592(2) 0.87226(19) 0.0292(12) Uani 1 1 d . . . N13 N 0.9512(2) 0.4396(2) 0.9179(2) 0.0316(12) Uani 1 1 d . . . H13E H 0.9285 0.4581 0.9418 0.038 Uiso 1 1 calc R . . N14 N 0.8845(2) 0.4616(2) 0.6936(2) 0.0292(12) Uani 1 1 d . . . H14E H 0.8767 0.4570 0.6614 0.035 Uiso 1 1 calc R . . N15 N 1.0911(2) 0.3047(2) 0.7712(2) 0.0410(14) Uani 1 1 d . . . H15A H 1.1210 0.2771 0.7840 0.049 Uiso 1 1 calc R . . O1 O 1.01299(19) 0.45351(19) 0.84485(16) 0.0329(10) Uani 1 1 d . . . O2 O 0.94880(17) 0.49717(18) 0.74733(16) 0.0291(10) Uani 1 1 d . . . O3 O 1.05907(18) 0.40743(19) 0.75117(16) 0.0310(10) Uani 1 1 d . . . O4 O 0.8720(2) 0.3622(2) 0.87666(17) 0.0379(11) Uani 1 1 d . . . O5 O 0.86202(18) 0.3325(2) 0.72372(19) 0.0416(12) Uani 1 1 d . . . O6 O 0.9934(2) 0.2530(2) 0.8363(2) 0.0493(13) Uani 1 1 d . . . C1 C 0.8620(3) 0.2594(3) 0.8232(3) 0.0369(16) Uani 1 1 d . . . H1A H 0.8927 0.2916 0.8116 0.044 Uiso 1 1 calc R . . C2 C 0.8034(3) 0.2945(3) 0.8463(3) 0.0352(16) Uani 1 1 d . . . C3 C 0.7424(3) 0.2785(3) 0.8418(3) 0.0469(19) Uani 1 1 d . . . H3A H 0.7364 0.2439 0.8242 0.056 Uiso 1 1 calc R . . C4 C 0.6900(3) 0.3114(4) 0.8621(3) 0.057(2) Uani 1 1 d . A . C5 C 0.6999(4) 0.3629(4) 0.8864(3) 0.061(2) Uani 1 1 d . . . H5A H 0.6643 0.3868 0.8994 0.074 Uiso 1 1 calc R . . C6 C 0.7595(3) 0.3808(3) 0.8923(3) 0.0468(19) Uani 1 1 d . . . C7 C 0.8116(3) 0.3449(3) 0.8731(3) 0.0366(16) Uani 1 1 d . . . C8 C 0.6224(3) 0.2931(4) 0.8555(3) 0.072(3) Uani 1 1 d D . . C9 C 0.6139(8) 0.2928(8) 0.7966(4) 0.073(4) Uiso 0.550(12) 1 d PD A 1 H9A H 0.6327 0.2530 0.7862 0.109 Uiso 0.550(12) 1 calc PR A 1 H9B H 0.6348 0.3277 0.7765 0.109 Uiso 0.550(12) 1 calc PR A 1 H9C H 0.5689 0.2974 0.7899 0.109 Uiso 0.550(12) 1 calc PR A 1 C10 C 0.6213(8) 0.2227(6) 0.8831(6) 0.073(4) Uiso 0.550(12) 1 d PD A 1 H10A H 0.6628 0.2082 0.8964 0.109 Uiso 0.550(12) 1 calc PR A 1 H10B H 0.6108 0.1958 0.8578 0.109 Uiso 0.550(12) 1 calc PR A 1 H10C H 0.5895 0.2206 0.9121 0.109 Uiso 0.550(12) 1 calc PR A 1 C11 C 0.5726(7) 0.3357(7) 0.8802(6) 0.073(4) Uiso 0.550(12) 1 d PD A 1 H11A H 0.5653 0.3193 0.9170 0.109 Uiso 0.550(12) 1 calc PR A 1 H11B H 0.5333 0.3375 0.8621 0.109 Uiso 0.550(12) 1 calc PR A 1 H11C H 0.5871 0.3780 0.8774 0.109 Uiso 0.550(12) 1 calc PR A 1 C9' C 0.6199(11) 0.2378(8) 0.8258(8) 0.099(6) Uiso 0.450(12) 1 d PD A 2 H9'A H 0.6413 0.2003 0.8451 0.149 Uiso 0.450(12) 1 calc PR A 2 H9'B H 0.6411 0.2469 0.7913 0.149 Uiso 0.450(12) 1 calc PR A 2 H9'C H 0.5759 0.2305 0.8218 0.149 Uiso 0.450(12) 1 calc PR A 2 C10' C 0.5883(11) 0.2819(10) 0.9116(6) 0.099(6) Uiso 0.450(12) 1 d PD A 2 H10D H 0.6080 0.2440 0.9315 0.149 Uiso 0.450(12) 1 calc PR A 2 H10E H 0.5436 0.2768 0.9082 0.149 Uiso 0.450(12) 1 calc PR A 2 H10F H 0.5923 0.3181 0.9299 0.149 Uiso 0.450(12) 1 calc PR A 2 C11' C 0.5867(11) 0.3552(8) 0.8251(8) 0.099(6) Uiso 0.450(12) 1 d PD A 2 H11D H 0.6158 0.3885 0.8180 0.149 Uiso 0.450(12) 1 calc PR A 2 H11E H 0.5503 0.3693 0.8467 0.149 Uiso 0.450(12) 1 calc PR A 2 H11F H 0.5722 0.3457 0.7921 0.149 Uiso 0.450(12) 1 calc PR A 2 C12 C 0.7694(4) 0.4391(3) 0.9171(3) 0.058(2) Uani 1 1 d . . . H12A H 0.7285 0.4583 0.9285 0.087 Uiso 1 1 calc R . . H12B H 0.7903 0.4693 0.8914 0.087 Uiso 1 1 calc R . . H12C H 0.7957 0.4273 0.9471 0.087 Uiso 1 1 calc R . . C13 C 0.8978(3) 0.3427(3) 0.9269(3) 0.0358(16) Uani 1 1 d . . . H13A H 0.9038 0.2964 0.9338 0.043 Uiso 1 1 calc R . . H13B H 0.8690 0.3579 0.9547 0.043 Uiso 1 1 calc R . . C14 C 0.9603(3) 0.3711(3) 0.9253(3) 0.0357(16) Uani 1 1 d . . . H14A H 0.9813 0.3565 0.9584 0.043 Uiso 1 1 calc R . . H14B H 0.9879 0.3569 0.8964 0.043 Uiso 1 1 calc R . . C15 C 0.9749(3) 0.4747(3) 0.8782(2) 0.0268(14) Uani 1 1 d . . . C16 C 0.9573(3) 0.5446(3) 0.8712(2) 0.0284(14) Uani 1 1 d . . . C17 C 0.9201(3) 0.5763(3) 0.9056(3) 0.0463(18) Uani 1 1 d . . . H17A H 0.9034 0.5545 0.9371 0.056 Uiso 1 1 calc R . . C18 C 0.9070(4) 0.6409(4) 0.8938(3) 0.058(2) Uani 1 1 d . . . H18A H 0.8814 0.6640 0.9170 0.069 Uiso 1 1 calc R . . C19 C 0.9321(3) 0.6706(3) 0.8478(3) 0.0401(17) Uani 1 1 d . . . H19A H 0.9252 0.7148 0.8391 0.048 Uiso 1 1 calc R . . C20 C 0.9672(3) 0.6356(3) 0.8148(2) 0.0332(15) Uani 1 1 d . . . C21 C 0.9952(2) 0.6634(3) 0.7633(2) 0.0237(14) Uani 1 1 d . . . C22 C 1.0036(3) 0.7498(3) 0.7017(2) 0.0295(15) Uani 1 1 d . . . C23 C 1.0348(3) 0.7083(3) 0.6682(3) 0.0328(15) Uani 1 1 d . . . C24 C 0.9918(3) 0.8183(3) 0.6881(3) 0.0354(16) Uani 1 1 d . . . C25 C 0.9389(3) 0.8483(3) 0.7104(3) 0.0371(16) Uani 1 1 d . . . H25A H 0.9117 0.8248 0.7344 0.045 Uiso 1 1 calc R . . C26 C 0.9258(3) 0.9128(3) 0.6978(3) 0.0428(18) Uani 1 1 d . . . H26A H 0.8886 0.9329 0.7122 0.051 Uiso 1 1 calc R . . C27 C 0.9667(4) 0.9483(3) 0.6641(3) 0.055(2) Uani 1 1 d . . . H27A H 0.9582 0.9924 0.6560 0.066 Uiso 1 1 calc R . . C28 C 1.0193(5) 0.9182(3) 0.6429(3) 0.068(3) Uani 1 1 d . . . H28A H 1.0473 0.9422 0.6200 0.082 Uiso 1 1 calc R . . C29 C 1.0327(4) 0.8543(3) 0.6536(3) 0.058(2) Uani 1 1 d . . . H29A H 1.0692 0.8346 0.6379 0.070 Uiso 1 1 calc R . . C30 C 1.0521(4) 0.7242(3) 0.6118(3) 0.051(2) Uani 1 1 d . . . C31 C 1.0080(4) 0.7542(3) 0.5773(3) 0.056(2) Uani 1 1 d . . . H31A H 0.9682 0.7696 0.5910 0.067 Uiso 1 1 calc R . . C32 C 1.0200(6) 0.7626(4) 0.5233(4) 0.099(4) Uani 1 1 d . . . H32A H 0.9905 0.7847 0.5000 0.119 Uiso 1 1 calc R . . C33 C 1.0800(7) 0.7354(5) 0.5055(4) 0.116(5) Uani 1 1 d . . . H33A H 1.0887 0.7359 0.4691 0.139 Uiso 1 1 calc R . . C34 C 1.1257(7) 0.7086(5) 0.5395(5) 0.123(5) Uani 1 1 d . . . H34A H 1.1663 0.6949 0.5262 0.147 Uiso 1 1 calc R . . C35 C 1.1121(5) 0.7018(4) 0.5929(4) 0.079(3) Uani 1 1 d . . . H35A H 1.1427 0.6825 0.6165 0.095 Uiso 1 1 calc R . . C36 C 0.8460(3) 0.2330(3) 0.7741(3) 0.0352(16) Uani 1 1 d . . . C37 C 0.8301(3) 0.1708(3) 0.7762(3) 0.0333(15) Uani 1 1 d . . . H37A H 0.8325 0.1438 0.8083 0.040 Uiso 1 1 calc R . . C38 C 0.8109(3) 0.1476(3) 0.7327(3) 0.0335(16) Uani 1 1 d . . . C39 C 0.8086(3) 0.1881(3) 0.6863(3) 0.0374(16) Uani 1 1 d . . . H39A H 0.7952 0.1732 0.6563 0.045 Uiso 1 1 calc R . . C40 C 0.8252(3) 0.2504(3) 0.6815(3) 0.0383(17) Uani 1 1 d . . . C41 C 0.8429(3) 0.2712(3) 0.7266(3) 0.0383(17) Uani 1 1 d . . . C42 C 0.7904(3) 0.0802(3) 0.7383(3) 0.0379(17) Uani 1 1 d . . . C43 C 0.8308(4) 0.0346(3) 0.7748(3) 0.061(2) Uani 1 1 d . . . H43A H 0.8747 0.0334 0.7612 0.092 Uiso 1 1 calc R . . H43B H 0.8157 -0.0074 0.7774 0.092 Uiso 1 1 calc R . . H43C H 0.8281 0.0483 0.8094 0.092 Uiso 1 1 calc R . . C44 C 0.7220(3) 0.0807(4) 0.7605(3) 0.061(2) Uani 1 1 d . . . H44A H 0.7081 0.0382 0.7642 0.092 Uiso 1 1 calc R . . H44B H 0.6947 0.1089 0.7369 0.092 Uiso 1 1 calc R . . H44C H 0.7195 0.0954 0.7948 0.092 Uiso 1 1 calc R . . C45 C 0.7916(4) 0.0562(3) 0.6854(3) 0.051(2) Uani 1 1 d . . . H45A H 0.8347 0.0555 0.6699 0.076 Uiso 1 1 calc R . . H45B H 0.7634 0.0841 0.6623 0.076 Uiso 1 1 calc R . . H45C H 0.7775 0.0137 0.6902 0.076 Uiso 1 1 calc R . . C46 C 0.8258(4) 0.2906(3) 0.6294(3) 0.054(2) Uani 1 1 d . . . H46A H 0.8117 0.2670 0.6031 0.082 Uiso 1 1 calc R . . H46B H 0.8687 0.3024 0.6197 0.082 Uiso 1 1 calc R . . H46C H 0.7973 0.3285 0.6314 0.082 Uiso 1 1 calc R . . C47 C 0.8122(3) 0.3810(3) 0.7250(3) 0.0398(17) Uani 1 1 d . . . H47A H 0.7799 0.3682 0.7525 0.048 Uiso 1 1 calc R . . H47B H 0.7920 0.3890 0.6910 0.048 Uiso 1 1 calc R . . C48 C 0.8400(3) 0.4399(3) 0.7361(3) 0.0362(16) Uani 1 1 d . . . H48A H 0.8057 0.4732 0.7400 0.043 Uiso 1 1 calc R . . H48B H 0.8620 0.4309 0.7692 0.043 Uiso 1 1 calc R . . C49 C 0.9351(3) 0.4874(3) 0.7020(2) 0.0289(15) Uani 1 1 d . . . C50 C 0.9803(3) 0.5071(3) 0.6577(2) 0.0302(15) Uani 1 1 d . . . C51 C 0.9658(3) 0.5187(3) 0.6051(3) 0.0435(18) Uani 1 1 d . . . H51A H 0.9247 0.5134 0.5948 0.052 Uiso 1 1 calc R . . C52 C 1.0121(3) 0.5380(4) 0.5685(3) 0.0456(18) Uani 1 1 d . . . H52A H 1.0029 0.5466 0.5326 0.055 Uiso 1 1 calc R . . C53 C 1.0726(3) 0.5450(3) 0.5840(3) 0.0394(17) Uani 1 1 d . . . H53A H 1.1054 0.5577 0.5593 0.047 Uiso 1 1 calc R . . C54 C 1.0828(3) 0.5325(3) 0.6373(2) 0.0270(14) Uani 1 1 d . . . C55 C 1.1449(3) 0.5390(3) 0.6585(2) 0.0234(14) Uani 1 1 d . . . C56 C 1.2491(3) 0.5565(3) 0.6427(3) 0.0319(15) Uani 1 1 d . . . C57 C 1.2561(3) 0.5360(3) 0.6975(3) 0.0324(15) Uani 1 1 d . . . C58 C 1.2984(3) 0.5814(3) 0.6049(2) 0.0316(15) Uani 1 1 d . . . C59 C 1.2898(3) 0.5818(3) 0.5521(3) 0.0350(16) Uani 1 1 d . . . H59A H 1.2535 0.5653 0.5415 0.042 Uiso 1 1 calc R . . C60 C 1.3338(3) 0.6061(3) 0.5149(3) 0.0426(17) Uani 1 1 d . . . H60A H 1.3276 0.6067 0.4788 0.051 Uiso 1 1 calc R . . C61 C 1.3868(4) 0.6294(4) 0.5307(3) 0.054(2) Uani 1 1 d . . . H61A H 1.4173 0.6455 0.5054 0.065 Uiso 1 1 calc R . . C62 C 1.3958(3) 0.6296(3) 0.5835(3) 0.050(2) Uani 1 1 d . . . H62A H 1.4323 0.6459 0.5939 0.060 Uiso 1 1 calc R . . C63 C 1.3514(3) 0.6059(3) 0.6207(3) 0.0388(17) Uani 1 1 d . . . H63A H 1.3571 0.6065 0.6567 0.047 Uiso 1 1 calc R . . C64 C 1.3165(3) 0.5228(3) 0.7241(3) 0.0376(17) Uani 1 1 d . . . C65 C 1.3621(3) 0.4787(3) 0.7068(3) 0.0480(19) Uani 1 1 d . . . H65A H 1.3549 0.4585 0.6777 0.058 Uiso 1 1 calc R . . C66 C 1.4182(3) 0.4646(4) 0.7327(4) 0.059(2) Uani 1 1 d . . . H66A H 1.4495 0.4349 0.7210 0.070 Uiso 1 1 calc R . . C67 C 1.4280(4) 0.4933(4) 0.7747(4) 0.062(2) Uani 1 1 d . . . H67A H 1.4665 0.4842 0.7920 0.075 Uiso 1 1 calc R . . C68 C 1.3817(4) 0.5360(4) 0.7924(3) 0.055(2) Uani 1 1 d . . . H68A H 1.3883 0.5549 0.8224 0.066 Uiso 1 1 calc R . . C69 C 1.3266(3) 0.5512(3) 0.7671(3) 0.0401(17) Uani 1 1 d . . . H69A H 1.2957 0.5811 0.7790 0.048 Uiso 1 1 calc R . . C70 C 0.8939(3) 0.2122(3) 0.8648(3) 0.0377(17) Uani 1 1 d . . . C71 C 0.8611(3) 0.1722(3) 0.8993(3) 0.0393(17) Uani 1 1 d . . . H71A H 0.8169 0.1727 0.8960 0.047 Uiso 1 1 calc R . . C72 C 0.8885(4) 0.1304(3) 0.9394(3) 0.0494(19) Uani 1 1 d . . . C73 C 0.9531(4) 0.1333(4) 0.9448(3) 0.056(2) Uani 1 1 d . . . H73A H 0.9732 0.1058 0.9718 0.067 Uiso 1 1 calc R . . C74 C 0.9889(3) 0.1745(4) 0.9124(3) 0.054(2) Uani 1 1 d . . . C75 C 0.9591(3) 0.2119(3) 0.8710(3) 0.0450(19) Uani 1 1 d . . . C76 C 0.8490(4) 0.0845(4) 0.9751(3) 0.063(2) Uani 1 1 d . . . C77 C 0.7958(4) 0.1208(5) 1.0036(3) 0.075(3) Uani 1 1 d . . . H77A H 0.8139 0.1471 1.0259 0.112 Uiso 1 1 calc R . . H77B H 0.7696 0.0910 1.0252 0.112 Uiso 1 1 calc R . . H77C H 0.7697 0.1474 0.9780 0.112 Uiso 1 1 calc R . . C78 C 0.8202(5) 0.0426(4) 0.9404(3) 0.082(3) Uani 1 1 d . . . H78A H 0.7944 0.0128 0.9623 0.123 Uiso 1 1 calc R . . H78B H 0.8542 0.0194 0.9221 0.123 Uiso 1 1 calc R . . H78C H 0.7938 0.0689 0.9149 0.123 Uiso 1 1 calc R . . C79 C 0.8873(5) 0.0413(4) 1.0154(4) 0.090(3) Uani 1 1 d . . . H79A H 0.9051 0.0664 1.0388 0.136 Uiso 1 1 calc R . . H79B H 0.9215 0.0178 0.9976 0.136 Uiso 1 1 calc R . . H79C H 0.8598 0.0118 1.0357 0.136 Uiso 1 1 calc R . . C80 C 1.0577(3) 0.1804(4) 0.9199(4) 0.077(3) Uani 1 1 d . . . H80A H 1.0738 0.2122 0.8929 0.116 Uiso 1 1 calc R . . H80B H 1.0816 0.1399 0.9175 0.116 Uiso 1 1 calc R . . H80C H 1.0624 0.1929 0.9544 0.116 Uiso 1 1 calc R . . C81 C 1.0123(3) 0.2292(3) 0.7877(3) 0.0452(19) Uani 1 1 d . . . H81A H 0.9757 0.2130 0.7736 0.054 Uiso 1 1 calc R . . H81B H 1.0454 0.1942 0.7937 0.054 Uiso 1 1 calc R . . C82 C 1.0370(3) 0.2811(3) 0.7491(3) 0.047(2) Uani 1 1 d . . . H82A H 1.0505 0.2652 0.7159 0.057 Uiso 1 1 calc R . . H82B H 1.0035 0.3156 0.7421 0.057 Uiso 1 1 calc R . . C83 C 1.0973(3) 0.3645(3) 0.7729(2) 0.0293(15) Uani 1 1 d . . . C84 C 1.1494(3) 0.3841(3) 0.8026(2) 0.0302(6) Uani 1 1 d U . . C85 C 1.1997(3) 0.3442(3) 0.8213(2) 0.0302(6) Uani 1 1 d U . . H85A H 1.2044 0.3016 0.8151 0.036 Uiso 1 1 calc R . . C86 C 1.2434(3) 0.3687(3) 0.8496(2) 0.0302(6) Uani 1 1 d U . . H86A H 1.2788 0.3429 0.8628 0.036 Uiso 1 1 calc R . . C87 C 1.2344(3) 0.4301(3) 0.8579(2) 0.0302(6) Uani 1 1 d U . . H87A H 1.2630 0.4476 0.8775 0.036 Uiso 1 1 calc R . . C88 C 1.1816(3) 0.4669(3) 0.8365(2) 0.0302(6) Uani 1 1 d U . . C89 C 1.1714(3) 0.5330(3) 0.8433(2) 0.0281(14) Uani 1 1 d . . . C90 C 1.1963(3) 0.6183(3) 0.8797(2) 0.0290(15) Uani 1 1 d . . . C91 C 1.1395(3) 0.6505(3) 0.8601(2) 0.0319(15) Uani 1 1 d . . . C92 C 1.2412(3) 0.6465(3) 0.9096(3) 0.0376(16) Uani 1 1 d . . . C93 C 1.2770(4) 0.6080(4) 0.9463(3) 0.059(2) Uani 1 1 d . . . H93A H 1.2720 0.5643 0.9524 0.071 Uiso 1 1 calc R . . C94 C 1.3203(5) 0.6333(5) 0.9745(4) 0.083(3) Uani 1 1 d . . . H94A H 1.3453 0.6069 0.9991 0.100 Uiso 1 1 calc R . . C95 C 1.3261(4) 0.6974(5) 0.9658(4) 0.073(3) Uani 1 1 d . . . H95A H 1.3539 0.7152 0.9859 0.087 Uiso 1 1 calc R . . C96 C 1.2930(4) 0.7348(4) 0.9296(4) 0.063(2) Uani 1 1 d . . . H96A H 1.2986 0.7784 0.9237 0.076 Uiso 1 1 calc R . . C97 C 1.2504(3) 0.7102(3) 0.9006(3) 0.0496(19) Uani 1 1 d . . . H97A H 1.2277 0.7370 0.8746 0.060 Uiso 1 1 calc R . . C98 C 1.1108(3) 0.7130(3) 0.8713(3) 0.0421(18) Uani 1 1 d . . . C99 C 1.1010(3) 0.7247(4) 0.9230(3) 0.054(2) Uani 1 1 d . . . H99A H 1.1147 0.6940 0.9508 0.065 Uiso 1 1 calc R . . C100 C 1.0708(4) 0.7821(4) 0.9332(4) 0.072(3) Uani 1 1 d . . . H10G H 1.0632 0.7905 0.9682 0.086 Uiso 1 1 calc R . . C101 C 1.0518(5) 0.8275(4) 0.8915(5) 0.091(3) Uani 1 1 d . . . H10H H 1.0312 0.8665 0.8985 0.109 Uiso 1 1 calc R . . C102 C 1.0626(4) 0.8162(4) 0.8420(4) 0.070(3) Uani 1 1 d . . . H10I H 1.0499 0.8474 0.8142 0.084 Uiso 1 1 calc R . . C103 C 1.0926(3) 0.7587(3) 0.8310(3) 0.0487(19) Uani 1 1 d . . . H10J H 1.1003 0.7511 0.7959 0.058 Uiso 1 1 calc R . . Er2 Er 0.372315(12) 0.998574(12) 0.707909(11) 0.02756(10) Uani 1 1 d . . . O1A O 0.45716(18) 0.97605(19) 0.65033(17) 0.0324(10) Uani 1 1 d . . . O2A O 0.44282(19) 0.93886(19) 0.76448(17) 0.0357(10) Uani 1 1 d . . . O3A O 0.35849(19) 0.89720(18) 0.69209(17) 0.0336(10) Uani 1 1 d . . . O4A O 0.52514(18) 0.8003(2) 0.59849(18) 0.0412(11) Uani 1 1 d . . . O5A O 0.6086(3) 0.8359(2) 0.7346(3) 0.0683(17) Uani 1 1 d . . . O6A O 0.44870(19) 0.7486(2) 0.73129(19) 0.0418(12) Uani 1 1 d . . . N1A N 0.3441(2) 1.0050(2) 0.6164(2) 0.0311(12) Uani 1 1 d . . . N2A N 0.4600(2) 1.0568(2) 0.7322(2) 0.0332(13) Uani 1 1 d . . . N3A N 0.3053(2) 0.9371(2) 0.77610(19) 0.0287(12) Uani 1 1 d . . . N4A N 0.2571(2) 1.0292(2) 0.6897(2) 0.0309(12) Uani 1 1 d . . . N5A N 0.3713(2) 1.1127(2) 0.6703(2) 0.0288(12) Uani 1 1 d . . . N6A N 0.3324(2) 1.0528(2) 0.7859(2) 0.0302(12) Uani 1 1 d . . . N7A N 0.2129(2) 1.0311(2) 0.72841(19) 0.0268(12) Uani 1 1 d . . . N8A N 0.3293(2) 1.1386(2) 0.6355(2) 0.0311(12) Uani 1 1 d . . . N9A N 0.3504(2) 1.1101(2) 0.7904(2) 0.0321(12) Uani 1 1 d . . . N10A N 0.1791(2) 1.0578(2) 0.62670(19) 0.0279(12) Uani 1 1 d . . . N11A N 0.4188(2) 1.2094(2) 0.6634(2) 0.0333(13) Uani 1 1 d . . . N12A N 0.2702(2) 1.0506(2) 0.8654(2) 0.0316(12) Uani 1 1 d . . . N13A N 0.4937(2) 0.9326(2) 0.5789(2) 0.0377(14) Uani 1 1 d . . . H13F H 0.4872 0.9276 0.5465 0.045 Uiso 1 1 calc R . . N14A N 0.5371(3) 0.9196(3) 0.7988(3) 0.0608(19) Uani 1 1 d . . . H14F H 0.5697 0.9355 0.8098 0.073 Uiso 1 1 calc R . . N15A N 0.3251(2) 0.8001(2) 0.7125(2) 0.0357(13) Uani 1 1 d . . . H15B H 0.2984 0.7764 0.7315 0.043 Uiso 1 1 calc R . . C1A C 0.5754(3) 0.7313(3) 0.6915(3) 0.0408(17) Uani 1 1 d . . . H1AA H 0.5500 0.7727 0.6880 0.049 Uiso 1 1 calc R . . C2A C 0.5656(3) 0.7015(3) 0.6426(3) 0.0383(17) Uani 1 1 d . . . C3A C 0.5808(3) 0.6364(3) 0.6419(3) 0.050(2) Uani 1 1 d . . . H3AA H 0.5948 0.6111 0.6726 0.059 Uiso 1 1 calc R . . C4A C 0.5756(3) 0.6083(4) 0.5966(4) 0.050(2) Uani 1 1 d . B . C5A C 0.5560(3) 0.6463(4) 0.5530(3) 0.053(2) Uani 1 1 d . . . H5AA H 0.5543 0.6285 0.5217 0.064 Uiso 1 1 calc R . . C6A C 0.5384(3) 0.7104(4) 0.5525(3) 0.048(2) Uani 1 1 d . . . C7A C 0.5444(3) 0.7373(3) 0.5979(3) 0.0382(17) Uani 1 1 d . . . C8A C 0.5934(4) 0.5368(4) 0.5987(4) 0.079(3) Uani 1 1 d D . . C9A C 0.5717(9) 0.5077(12) 0.5524(6) 0.062(5) Uiso 0.403(17) 1 d PD B 1 H9AA H 0.5269 0.5004 0.5580 0.093 Uiso 0.403(17) 1 calc PR B 1 H9AB H 0.5964 0.4677 0.5497 0.093 Uiso 0.403(17) 1 calc PR B 1 H9AC H 0.5780 0.5364 0.5202 0.093 Uiso 0.403(17) 1 calc PR B 1 C10A C 0.6616(6) 0.5205(10) 0.6118(8) 0.062(5) Uiso 0.403(17) 1 d PD B 1 H10K H 0.6638 0.5042 0.6489 0.093 Uiso 0.403(17) 1 calc PR B 1 H10L H 0.6848 0.5583 0.6041 0.093 Uiso 0.403(17) 1 calc PR B 1 H10M H 0.6804 0.4886 0.5908 0.093 Uiso 0.403(17) 1 calc PR B 1 C11A C 0.5496(9) 0.5044(10) 0.6490(6) 0.062(5) Uiso 0.403(17) 1 d PD B 1 H11G H 0.5058 0.5222 0.6463 0.093 Uiso 0.403(17) 1 calc PR B 1 H11H H 0.5658 0.5131 0.6816 0.093 Uiso 0.403(17) 1 calc PR B 1 H11I H 0.5513 0.4590 0.6487 0.093 Uiso 0.403(17) 1 calc PR B 1 C9B C 0.5510(8) 0.5128(11) 0.5587(7) 0.095(4) Uiso 0.597(17) 1 d PD B 2 H9BA H 0.5079 0.5101 0.5738 0.143 Uiso 0.597(17) 1 calc PR B 2 H9BB H 0.5683 0.4712 0.5512 0.143 Uiso 0.597(17) 1 calc PR B 2 H9BC H 0.5505 0.5422 0.5263 0.143 Uiso 0.597(17) 1 calc PR B 2 C10B C 0.6636(6) 0.5380(9) 0.5686(7) 0.095(4) Uiso 0.597(17) 1 d PD B 2 H10N H 0.6614 0.5675 0.5363 0.143 Uiso 0.597(17) 1 calc PR B 2 H10O H 0.6777 0.4959 0.5604 0.143 Uiso 0.597(17) 1 calc PR B 2 H10P H 0.6936 0.5514 0.5913 0.143 Uiso 0.597(17) 1 calc PR B 2 C11B C 0.5961(9) 0.4996(9) 0.6502(5) 0.095(4) Uiso 0.597(17) 1 d PD B 2 H11J H 0.5536 0.4993 0.6670 0.143 Uiso 0.597(17) 1 calc PR B 2 H11K H 0.6238 0.5181 0.6717 0.143 Uiso 0.597(17) 1 calc PR B 2 H11L H 0.6125 0.4565 0.6466 0.143 Uiso 0.597(17) 1 calc PR B 2 C12A C 0.5114(4) 0.7498(4) 0.5044(3) 0.056(2) Uani 1 1 d . . . H12D H 0.5021 0.7933 0.5113 0.084 Uiso 1 1 calc R . . H12E H 0.4726 0.7329 0.4961 0.084 Uiso 1 1 calc R . . H12F H 0.5423 0.7487 0.4749 0.084 Uiso 1 1 calc R . . C13A C 0.5725(3) 0.8438(3) 0.5816(3) 0.0409(17) Uani 1 1 d . . . H13C H 0.5770 0.8507 0.5430 0.049 Uiso 1 1 calc R . . H13D H 0.6138 0.8267 0.5953 0.049 Uiso 1 1 calc R . . C14A C 0.5515(3) 0.9048(3) 0.6022(3) 0.0413(17) Uani 1 1 d . . . H14C H 0.5446 0.8970 0.6405 0.050 Uiso 1 1 calc R . . H14D H 0.5849 0.9343 0.5940 0.050 Uiso 1 1 calc R . . C15A C 0.4498(3) 0.9656(3) 0.6052(3) 0.0321(9) Uani 1 1 d U . . C16A C 0.3887(3) 0.9890(3) 0.5805(2) 0.0312(15) Uani 1 1 d . . . C17A C 0.3783(3) 0.9941(4) 0.5276(3) 0.051(2) Uani 1 1 d . . . H17B H 0.4113 0.9832 0.5034 0.062 Uiso 1 1 calc R . . C18A C 0.3196(3) 1.0153(4) 0.5113(3) 0.052(2) Uani 1 1 d . . . H18B H 0.3113 1.0192 0.4754 0.063 Uiso 1 1 calc R . . C19A C 0.2717(3) 1.0313(3) 0.5474(3) 0.0405(17) Uani 1 1 d . . . H19B H 0.2305 1.0460 0.5369 0.049 Uiso 1 1 calc R . . C20A C 0.2867(3) 1.0247(3) 0.5993(2) 0.0305(15) Uani 1 1 d . . . C21A C 0.2366(3) 1.0373(3) 0.6409(2) 0.0262(14) Uani 1 1 d . . . C22A C 0.1517(3) 1.0457(3) 0.7174(2) 0.0291(15) Uani 1 1 d . . . C23A C 0.1356(3) 1.0637(3) 0.6648(2) 0.0275(14) Uani 1 1 d . . . C24A C 0.0727(3) 1.0906(3) 0.6479(2) 0.0297(15) Uani 1 1 d . . . C25A C 0.0543(3) 1.0819(3) 0.5989(3) 0.0330(15) Uani 1 1 d . . . H25B H 0.0818 1.0594 0.5766 0.040 Uiso 1 1 calc R . . C26A C -0.0050(3) 1.1068(3) 0.5830(3) 0.0387(17) Uani 1 1 d . . . H26B H -0.0181 1.1007 0.5498 0.046 Uiso 1 1 calc R . . C27A C -0.0452(3) 1.1404(3) 0.6152(3) 0.0390(17) Uani 1 1 d . . . H27B H -0.0857 1.1570 0.6040 0.047 Uiso 1 1 calc R . . C28A C -0.0270(3) 1.1498(3) 0.6630(3) 0.0401(17) Uani 1 1 d . . . H28B H -0.0546 1.1730 0.6848 0.048 Uiso 1 1 calc R . . C29A C 0.0325(3) 1.1252(3) 0.6798(3) 0.0316(15) Uani 1 1 d . . . H29B H 0.0455 1.1320 0.7128 0.038 Uiso 1 1 calc R . . C30A C 0.1075(3) 1.0354(3) 0.7633(2) 0.0281(14) Uani 1 1 d . . . C31A C 0.0558(3) 1.0011(3) 0.7612(3) 0.0359(16) Uani 1 1 d . . . H31B H 0.0484 0.9852 0.7299 0.043 Uiso 1 1 calc R . . C32A C 0.0146(3) 0.9897(3) 0.8049(3) 0.0453(18) Uani 1 1 d . . . H32B H -0.0203 0.9656 0.8032 0.054 Uiso 1 1 calc R . . C33A C 0.0240(4) 1.0130(3) 0.8496(3) 0.051(2) Uani 1 1 d . . . H33B H -0.0047 1.0057 0.8788 0.062 Uiso 1 1 calc R . . C34A C 0.0754(3) 1.0473(3) 0.8527(3) 0.0414(17) Uani 1 1 d . . . H34B H 0.0820 1.0630 0.8842 0.050 Uiso 1 1 calc R . . C35A C 0.1172(3) 1.0588(3) 0.8098(3) 0.0379(16) Uani 1 1 d . . . H35B H 0.1523 1.0824 0.8120 0.045 Uiso 1 1 calc R . . C36A C 0.6455(3) 0.7452(3) 0.6940(3) 0.0466(19) Uani 1 1 d . . . C37A C 0.6953(3) 0.7054(3) 0.6791(3) 0.0416(18) Uani 1 1 d . . . H37B H 0.6867 0.6700 0.6635 0.050 Uiso 1 1 calc R . . C38A C 0.7577(3) 0.7151(3) 0.6858(3) 0.049(2) Uani 1 1 d . . . C39A C 0.7685(3) 0.7703(4) 0.7048(4) 0.077(3) Uani 1 1 d . C . H39B H 0.8109 0.7789 0.7085 0.093 Uiso 1 1 calc R . . C40A C 0.7207(4) 0.8132(4) 0.7185(5) 0.085(3) Uani 1 1 d . . . C41A C 0.6581(4) 0.7976(3) 0.7162(4) 0.067(3) Uani 1 1 d . C . C42A C 0.8124(3) 0.6660(4) 0.6774(3) 0.051(2) Uani 1 1 d . . . C43A C 0.7923(3) 0.6144(4) 0.6489(3) 0.058(2) Uani 1 1 d . . . H43D H 0.7787 0.6327 0.6142 0.087 Uiso 1 1 calc R . . H43E H 0.7572 0.5943 0.6687 0.087 Uiso 1 1 calc R . . H43F H 0.8279 0.5831 0.6454 0.087 Uiso 1 1 calc R . . C44A C 0.8352(4) 0.6382(4) 0.7319(3) 0.067(2) Uani 1 1 d . . . H44D H 0.8005 0.6189 0.7529 0.101 Uiso 1 1 calc R . . H44E H 0.8494 0.6717 0.7492 0.101 Uiso 1 1 calc R . . H44F H 0.8703 0.6063 0.7282 0.101 Uiso 1 1 calc R . . C45A C 0.8674(4) 0.6970(5) 0.6458(4) 0.074(3) Uani 1 1 d . . . H45D H 0.8541 0.7141 0.6108 0.111 Uiso 1 1 calc R . . H45E H 0.9032 0.6657 0.6432 0.111 Uiso 1 1 calc R . . H45F H 0.8800 0.7311 0.6634 0.111 Uiso 1 1 calc R . . C46A C 0.7246(8) 0.8700(8) 0.7568(7) 0.057(4) Uiso 0.50 1 d P C 1 H46D H 0.7081 0.8555 0.7921 0.086 Uiso 0.50 1 calc PR C 1 H46E H 0.6994 0.9079 0.7424 0.086 Uiso 0.50 1 calc PR C 1 H46F H 0.7686 0.8795 0.7580 0.086 Uiso 0.50 1 calc PR C 1 C46B C 0.7375(7) 0.8767(7) 0.7252(6) 0.045(4) Uiso 0.50 1 d P C 2 H46G H 0.7551 0.8972 0.6920 0.068 Uiso 0.50 1 calc PR C 2 H46H H 0.7689 0.8732 0.7518 0.068 Uiso 0.50 1 calc PR C 2 H46I H 0.6997 0.9017 0.7361 0.068 Uiso 0.50 1 calc PR C 2 C47A C 0.5972(4) 0.8198(4) 0.7892(4) 0.072(3) Uani 1 1 d . . . H47C H 0.6313 0.8339 0.8080 0.086 Uiso 1 1 calc R . . H47D H 0.5975 0.7736 0.7977 0.086 Uiso 1 1 calc R . . C48A C 0.5344(4) 0.8499(3) 0.8068(4) 0.072(3) Uani 1 1 d . . . H48C H 0.5005 0.8382 0.7865 0.087 Uiso 1 1 calc R . . H48D H 0.5252 0.8351 0.8441 0.087 Uiso 1 1 calc R . . C49A C 0.4923(3) 0.9582(3) 0.7757(3) 0.0321(9) Uani 1 1 d U . . C50A C 0.5013(3) 1.0246(3) 0.7659(3) 0.0353(16) Uani 1 1 d . . . C51A C 0.5489(3) 1.0556(3) 0.7844(3) 0.0473(19) Uani 1 1 d . . . H51B H 0.5794 1.0329 0.8065 0.057 Uiso 1 1 calc R . . C52A C 0.5508(3) 1.1195(4) 0.7699(3) 0.053(2) Uani 1 1 d . . . H52B H 0.5815 1.1413 0.7836 0.064 Uiso 1 1 calc R . . C53A C 0.5085(3) 1.1519(3) 0.7359(3) 0.0438(18) Uani 1 1 d . . . H53B H 0.5100 1.1957 0.7252 0.053 Uiso 1 1 calc R . . C54A C 0.4634(3) 1.1184(3) 0.7175(2) 0.0300(15) Uani 1 1 d . . . C55A C 0.4158(3) 1.1483(3) 0.6819(2) 0.0300(15) Uani 1 1 d . . . C56A C 0.3777(3) 1.2347(3) 0.6289(3) 0.0334(16) Uani 1 1 d . . . C57A C 0.3328(3) 1.1977(3) 0.6131(2) 0.0329(15) Uani 1 1 d . . . C58A C 0.3841(3) 1.3033(3) 0.6104(3) 0.0397(17) Uani 1 1 d . . . C59A C 0.4437(4) 1.3255(3) 0.6138(3) 0.052(2) Uani 1 1 d . . . H59B H 0.4784 1.2977 0.6258 0.062 Uiso 1 1 calc R . . C60A C 0.4505(4) 1.3898(4) 0.5990(3) 0.062(2) Uani 1 1 d . . . H60B H 0.4905 1.4052 0.6010 0.074 Uiso 1 1 calc R . . C61A C 0.4010(5) 1.4308(4) 0.5817(3) 0.068(2) Uani 1 1 d . . . H61B H 0.4067 1.4742 0.5721 0.082 Uiso 1 1 calc R . . C62A C 0.3442(5) 1.4093(4) 0.5783(3) 0.065(2) Uani 1 1 d . . . H62B H 0.3097 1.4375 0.5664 0.078 Uiso 1 1 calc R . . C63A C 0.3360(4) 1.3450(3) 0.5925(3) 0.056(2) Uani 1 1 d . . . H63B H 0.2958 1.3303 0.5895 0.067 Uiso 1 1 calc R . . C64A C 0.2852(3) 1.2170(3) 0.5729(3) 0.0389(17) Uani 1 1 d . . . C65A C 0.3023(4) 1.2401(3) 0.5214(3) 0.054(2) Uani 1 1 d . . . H65B H 0.3451 1.2463 0.5114 0.064 Uiso 1 1 calc R . . C66A C 0.2564(6) 1.2537(4) 0.4851(4) 0.080(3) Uani 1 1 d . . . H66B H 0.2675 1.2689 0.4499 0.096 Uiso 1 1 calc R . . C67A C 0.1928(5) 1.2447(4) 0.5008(4) 0.078(3) Uani 1 1 d . . . H67B H 0.1612 1.2545 0.4760 0.094 Uiso 1 1 calc R . . C68A C 0.1764(4) 1.2224(4) 0.5505(4) 0.064(2) Uani 1 1 d . . . H68B H 0.1335 1.2165 0.5605 0.077 Uiso 1 1 calc R . . C69A C 0.2216(3) 1.2082(3) 0.5862(3) 0.0455(18) Uani 1 1 d . . . H69B H 0.2097 1.1920 0.6210 0.055 Uiso 1 1 calc R . . C70A C 0.5512(3) 0.6936(3) 0.7410(3) 0.0467(19) Uani 1 1 d . . . C71A C 0.5902(4) 0.6489(3) 0.7706(3) 0.056(2) Uani 1 1 d . . . H71B H 0.6330 0.6420 0.7589 0.067 Uiso 1 1 calc R . . C72A C 0.5693(4) 0.6139(4) 0.8169(3) 0.057(2) Uani 1 1 d . D . C73A C 0.5075(4) 0.6285(4) 0.8345(3) 0.060(2) Uani 1 1 d . . . H73B H 0.4925 0.6070 0.8668 0.072 Uiso 1 1 calc R . . C74A C 0.4664(3) 0.6735(4) 0.8069(3) 0.052(2) Uani 1 1 d . . . C75A C 0.4886(3) 0.7037(3) 0.7592(3) 0.048(2) Uani 1 1 d . . . C76A C 0.6153(4) 0.5640(4) 0.8469(3) 0.073(3) Uani 1 1 d D . . C79A C 0.6441(19) 0.6015(19) 0.8877(14) 0.135(17) Uiso 0.30 1 d PD D 1 H79D H 0.6098 0.6244 0.9059 0.202 Uiso 0.30 1 calc PR D 1 H79E H 0.6726 0.6312 0.8692 0.202 Uiso 0.30 1 calc PR D 1 H79F H 0.6674 0.5717 0.9132 0.202 Uiso 0.30 1 calc PR D 1 C77A C 0.576(2) 0.5112(17) 0.8776(15) 0.14(2) Uiso 0.30 1 d PD D 1 H77D H 0.5517 0.5276 0.9068 0.212 Uiso 0.30 1 calc PR D 1 H77E H 0.6043 0.4752 0.8909 0.212 Uiso 0.30 1 calc PR D 1 H77F H 0.5467 0.4979 0.8541 0.212 Uiso 0.30 1 calc PR D 1 C78A C 0.6685(14) 0.5359(17) 0.8119(13) 0.110(14) Uiso 0.30 1 d PD D 1 H78D H 0.7073 0.5562 0.8148 0.165 Uiso 0.30 1 calc PR D 1 H78E H 0.6563 0.5430 0.7756 0.165 Uiso 0.30 1 calc PR D 1 H78F H 0.6757 0.4907 0.8232 0.165 Uiso 0.30 1 calc PR D 1 C79B C 0.6705(6) 0.5996(7) 0.8632(6) 0.085(4) Uiso 0.70 1 d PD D 2 H79G H 0.6539 0.6285 0.8877 0.128 Uiso 0.70 1 calc PR D 2 H79H H 0.6896 0.6235 0.8322 0.128 Uiso 0.70 1 calc PR D 2 H79I H 0.7025 0.5692 0.8799 0.128 Uiso 0.70 1 calc PR D 2 C77B C 0.5812(6) 0.5273(7) 0.8941(5) 0.068(4) Uiso 0.70 1 d PD D 2 H77G H 0.5644 0.5563 0.9183 0.102 Uiso 0.70 1 calc PR D 2 H77H H 0.6111 0.4954 0.9118 0.102 Uiso 0.70 1 calc PR D 2 H77I H 0.5465 0.5068 0.8821 0.102 Uiso 0.70 1 calc PR D 2 C78B C 0.6416(6) 0.5171(6) 0.8077(4) 0.065(3) Uiso 0.70 1 d PD D 2 H78G H 0.6064 0.5020 0.7917 0.097 Uiso 0.70 1 calc PR D 2 H78H H 0.6661 0.4814 0.8265 0.097 Uiso 0.70 1 calc PR D 2 H78I H 0.6688 0.5388 0.7804 0.097 Uiso 0.70 1 calc PR D 2 C80A C 0.4015(4) 0.6902(4) 0.8283(3) 0.065(2) Uani 1 1 d . . . H80D H 0.3802 0.7228 0.8037 0.098 Uiso 1 1 calc R . . H80E H 0.4040 0.7058 0.8617 0.098 Uiso 1 1 calc R . . H80F H 0.3776 0.6528 0.8334 0.098 Uiso 1 1 calc R . . C81A C 0.4112(3) 0.7213(3) 0.6968(3) 0.0405(17) Uani 1 1 d . . . H81C H 0.3877 0.6874 0.7167 0.049 Uiso 1 1 calc R . . H81D H 0.4387 0.7033 0.6696 0.049 Uiso 1 1 calc R . . C82A C 0.3661(3) 0.7733(3) 0.6725(3) 0.0382(17) Uani 1 1 d . . . H82C H 0.3902 0.8065 0.6523 0.046 Uiso 1 1 calc R . . H82D H 0.3400 0.7566 0.6480 0.046 Uiso 1 1 calc R . . C83A C 0.3272(3) 0.8592(3) 0.7209(3) 0.0321(9) Uani 1 1 d U . . C84A C 0.2909(3) 0.8798(3) 0.7677(2) 0.0314(15) Uani 1 1 d . . . C85A C 0.2468(4) 0.8477(3) 0.7992(3) 0.0467(19) Uani 1 1 d . . . H85B H 0.2366 0.8077 0.7925 0.056 Uiso 1 1 calc R . . C86A C 0.2177(4) 0.8740(3) 0.8405(3) 0.0478(19) Uani 1 1 d . . . H86B H 0.1864 0.8525 0.8618 0.057 Uiso 1 1 calc R . . C87A C 0.2336(3) 0.9317(3) 0.8513(3) 0.0409(17) Uani 1 1 d . . . H87B H 0.2152 0.9498 0.8806 0.049 Uiso 1 1 calc R . . C88A C 0.2774(3) 0.9617(3) 0.8175(2) 0.0288(15) Uani 1 1 d . . . C89A C 0.2941(3) 1.0257(3) 0.8235(2) 0.0289(15) Uani 1 1 d . . . C90A C 0.2861(3) 1.1089(3) 0.8697(2) 0.0316(15) Uani 1 1 d . . . C91A C 0.3285(3) 1.1378(3) 0.8317(3) 0.0306(15) Uani 1 1 d . . . C92A C 0.2573(3) 1.1380(3) 0.9148(3) 0.0353(16) Uani 1 1 d . . . C93A C 0.2525(4) 1.1020(3) 0.9635(3) 0.052(2) Uani 1 1 d . . . H93B H 0.2672 1.0588 0.9676 0.063 Uiso 1 1 calc R . . C94A C 0.2264(5) 1.1291(4) 1.0058(3) 0.072(3) Uani 1 1 d . . . H94B H 0.2235 1.1045 1.0391 0.086 Uiso 1 1 calc R . . C95A C 0.2046(4) 1.1916(4) 1.0003(3) 0.061(2) Uani 1 1 d . . . H95B H 0.1882 1.2104 1.0299 0.074 Uiso 1 1 calc R . . C96A C 0.2069(3) 1.2267(3) 0.9515(3) 0.0489(19) Uani 1 1 d . . . H96B H 0.1896 1.2690 0.9471 0.059 Uiso 1 1 calc R . . C97A C 0.2346(3) 1.2000(3) 0.9087(3) 0.0363(16) Uani 1 1 d . . . H97B H 0.2377 1.2247 0.8755 0.044 Uiso 1 1 calc R . . C98A C 0.3540(3) 1.1999(3) 0.8326(3) 0.0356(16) Uani 1 1 d . . . C99A C 0.3803(3) 1.2144(3) 0.8772(3) 0.0455(18) Uani 1 1 d . . . H99B H 0.3801 1.1855 0.9084 0.055 Uiso 1 1 calc R . . C104 C 0.4065(3) 1.2712(4) 0.8755(4) 0.054(2) Uani 1 1 d . . . H10Q H 0.4238 1.2818 0.9058 0.065 Uiso 1 1 calc R . . C105 C 0.4072(3) 1.3121(4) 0.8303(4) 0.058(2) Uani 1 1 d . . . H10R H 0.4253 1.3509 0.8296 0.069 Uiso 1 1 calc R . . C106 C 0.3827(3) 1.2985(3) 0.7861(3) 0.052(2) Uani 1 1 d . . . H10S H 0.3844 1.3275 0.7550 0.062 Uiso 1 1 calc R . . C107 C 0.3552(3) 1.2421(3) 0.7867(3) 0.0389(17) Uani 1 1 d . . . H10T H 0.3375 1.2325 0.7563 0.047 Uiso 1 1 calc R . . N16 N 0.5140(5) 0.8901(7) 0.4383(5) 0.0695(15) Uiso 0.60 1 d PD E 1 O7 O 0.4711(5) 0.9074(5) 0.4721(4) 0.0695(15) Uiso 0.60 1 d PD E 1 O8 O 0.5678(4) 0.8789(5) 0.4452(4) 0.0695(15) Uiso 0.60 1 d PD E 1 N16' N 0.4863(9) 0.8887(10) 0.4356(9) 0.0695(15) Uiso 0.40 1 d P E 2 O7' O 0.4195(7) 0.8947(7) 0.4512(6) 0.0695(15) Uiso 0.40 1 d P E 2 O8' O 0.5044(8) 0.9225(7) 0.4693(6) 0.0695(15) Uiso 0.40 1 d P E 2 O9 O 0.4896(3) 0.8749(3) 0.3991(2) 0.086(2) Uani 1 1 d D . . N17 N 0.8469(4) 0.4297(3) 0.5609(3) 0.0652(19) Uani 1 1 d . . . O10 O 0.8275(2) 0.4553(2) 0.60146(19) 0.0503(13) Uani 1 1 d . . . O11 O 0.9036(4) 0.4245(4) 0.5466(3) 0.110(3) Uani 1 1 d . . . O12 O 0.8076(4) 0.4109(3) 0.5339(3) 0.116(3) Uani 1 1 d . . . N18 N 0.8043(3) 0.8087(3) 0.2572(2) 0.0396(14) Uani 1 1 d . . . O13 O 0.8094(2) 0.7950(2) 0.21142(18) 0.0383(11) Uani 1 1 d . . . O14 O 0.8521(2) 0.8111(2) 0.28273(19) 0.0465(12) Uani 1 1 d . . . O15 O 0.7520(2) 0.8241(3) 0.2769(2) 0.0690(16) Uani 1 1 d . . . N19 N 0.0927(6) 0.5283(6) -0.0383(4) 0.098(3) Uani 1 1 d . . . O16 O 0.0594(6) 0.5797(6) -0.0438(4) 0.163(5) Uani 1 1 d . . . O17 O 0.1293(3) 0.5254(3) -0.0041(2) 0.0626(16) Uani 1 1 d . . . O18 O 0.0894(4) 0.4946(6) -0.0688(4) 0.161(5) Uani 1 1 d . . . N20 N 0.7910(3) 0.2964(3) 0.2714(3) 0.0606(19) Uani 1 1 d . . . O19 O 0.7508(3) 0.3151(3) 0.3112(3) 0.0886(14) Uani 1 1 d . F 1 O20 O 0.7578(3) 0.2916(3) 0.2351(3) 0.0886(14) Uani 1 1 d . F . O21 O 0.8275(6) 0.2411(6) 0.2873(5) 0.026(3) Uiso 0.30 1 d P F 1 O21' O 0.8219(6) 0.3377(7) 0.2760(5) 0.047(3) Uiso 0.40 1 d P F 2 O21" O 0.8437(8) 0.3016(8) 0.2765(6) 0.042(4) Uiso 0.30 1 d P F 3 N21 N 0.6659(9) -0.0575(11) 0.8663(8) 0.117(2) Uiso 0.50 1 d PD G 1 O22 O 0.6155(7) -0.0426(9) 0.8863(6) 0.117(2) Uiso 0.50 1 d PD G 1 O23 O 0.6710(8) -0.0602(10) 0.8179(6) 0.117(2) Uiso 0.50 1 d PD G 1 O24 O 0.7164(8) -0.0474(10) 0.8867(7) 0.117(2) Uiso 0.50 1 d PD G 1 N21' N 0.6665(12) -0.0274(11) 0.8646(10) 0.117(2) Uiso 0.50 1 d P H 2 O22' O 0.6298(8) 0.0086(9) 0.8863(7) 0.117(2) Uiso 0.50 1 d P H 2 O23' O 0.6516(9) -0.0554(11) 0.8359(8) 0.117(2) Uiso 0.50 1 d P H 2 O24' O 0.7285(10) -0.0309(10) 0.8791(8) 0.117(2) Uiso 0.50 1 d P H 2 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 Er1 0.02071(16) 0.02087(17) 0.03432(18) -0.00668(12) -0.00385(12) -0.00029(12) N1 0.024(3) 0.021(3) 0.037(3) -0.006(2) -0.002(2) 0.002(2) N2 0.021(3) 0.025(3) 0.032(3) -0.006(2) -0.005(2) 0.001(2) N3 0.021(3) 0.015(3) 0.044(3) -0.008(2) -0.005(2) -0.007(2) N4 0.027(3) 0.021(3) 0.031(3) -0.005(2) 0.001(2) -0.004(2) N5 0.027(3) 0.029(3) 0.036(3) -0.010(2) -0.005(2) -0.003(2) N6 0.026(3) 0.021(3) 0.040(3) -0.005(2) -0.002(2) -0.003(2) N7 0.038(3) 0.023(3) 0.034(3) -0.006(2) 0.009(2) -0.006(2) N8 0.022(3) 0.041(3) 0.042(3) -0.014(3) -0.008(3) 0.001(2) N9 0.040(3) 0.023(3) 0.038(3) -0.005(2) -0.004(3) -0.011(3) N10 0.023(3) 0.026(3) 0.035(3) -0.006(2) 0.001(2) 0.002(2) N11 0.033(3) 0.022(3) 0.038(3) -0.012(2) 0.000(3) -0.001(2) N12 0.028(3) 0.025(3) 0.036(3) -0.002(2) -0.001(2) -0.008(2) N13 0.028(3) 0.030(3) 0.039(3) -0.007(3) -0.003(2) -0.004(2) N14 0.015(3) 0.032(3) 0.043(3) -0.007(2) -0.005(2) -0.007(2) N15 0.028(3) 0.021(3) 0.076(4) -0.017(3) -0.015(3) 0.009(2) O1 0.030(2) 0.032(3) 0.035(3) 0.001(2) -0.003(2) -0.004(2) O2 0.023(2) 0.027(2) 0.038(3) -0.0081(19) -0.0005(19) -0.0015(18) O3 0.025(2) 0.022(2) 0.049(3) -0.011(2) -0.011(2) 0.000(2) O4 0.037(3) 0.037(3) 0.040(3) -0.003(2) -0.009(2) -0.006(2) O5 0.019(2) 0.029(3) 0.078(3) -0.010(2) 0.003(2) -0.006(2) O6 0.027(2) 0.043(3) 0.087(4) -0.040(3) 0.004(2) -0.009(2) C1 0.030(4) 0.026(4) 0.057(4) -0.012(3) 0.002(3) -0.005(3) C2 0.032(4) 0.027(4) 0.047(4) -0.008(3) -0.001(3) -0.001(3) C3 0.034(4) 0.048(5) 0.067(5) -0.034(4) -0.001(4) -0.008(3) C4 0.034(4) 0.062(5) 0.082(6) -0.040(5) -0.009(4) -0.002(4) C5 0.042(5) 0.067(6) 0.084(6) -0.040(5) -0.016(4) 0.009(4) C6 0.042(4) 0.047(5) 0.057(5) -0.023(4) -0.008(4) -0.007(4) C7 0.029(4) 0.036(4) 0.048(4) -0.008(3) -0.010(3) -0.007(3) C8 0.036(4) 0.088(7) 0.104(7) -0.054(6) -0.009(4) -0.010(4) C12 0.053(5) 0.041(5) 0.086(6) -0.029(4) -0.016(4) 0.007(4) C13 0.038(4) 0.025(4) 0.044(4) 0.000(3) -0.004(3) -0.004(3) C14 0.033(4) 0.035(4) 0.038(4) 0.001(3) -0.005(3) -0.007(3) C15 0.028(3) 0.032(4) 0.021(3) -0.005(3) -0.003(3) -0.008(3) C16 0.025(3) 0.026(4) 0.034(4) -0.003(3) -0.002(3) -0.001(3) C17 0.055(5) 0.036(4) 0.042(4) 0.003(3) 0.008(4) 0.008(4) C18 0.074(6) 0.045(5) 0.048(5) -0.004(4) 0.012(4) 0.012(4) C19 0.048(4) 0.029(4) 0.040(4) -0.006(3) 0.006(3) 0.015(3) C20 0.037(4) 0.032(4) 0.031(4) -0.006(3) -0.006(3) 0.003(3) C21 0.017(3) 0.029(4) 0.026(3) -0.010(3) -0.004(3) 0.003(3) C22 0.036(4) 0.012(3) 0.041(4) -0.008(3) -0.002(3) -0.002(3) C23 0.032(4) 0.022(4) 0.045(4) -0.010(3) 0.006(3) -0.004(3) C24 0.041(4) 0.023(4) 0.044(4) -0.011(3) 0.002(3) -0.001(3) C25 0.029(4) 0.030(4) 0.052(4) -0.007(3) -0.006(3) 0.001(3) C26 0.037(4) 0.027(4) 0.065(5) -0.012(4) -0.005(4) 0.004(3) C27 0.081(6) 0.022(4) 0.063(5) -0.009(4) -0.005(5) -0.005(4) C28 0.111(8) 0.023(5) 0.072(6) -0.010(4) 0.025(5) -0.030(5) C29 0.062(5) 0.035(5) 0.078(6) -0.015(4) 0.031(4) -0.014(4) C30 0.079(6) 0.021(4) 0.051(5) -0.005(4) 0.026(4) -0.010(4) C31 0.103(7) 0.026(4) 0.036(4) 0.000(3) 0.017(4) -0.006(4) C32 0.177(12) 0.053(6) 0.054(6) 0.011(5) 0.032(7) 0.011(7) C33 0.203(14) 0.067(7) 0.062(7) 0.004(6) 0.061(9) 0.015(8) C34 0.168(12) 0.061(7) 0.103(9) 0.038(6) 0.087(9) 0.052(7) C35 0.095(7) 0.042(5) 0.086(7) 0.007(5) 0.053(6) 0.006(5) C36 0.019(3) 0.037(4) 0.053(5) -0.019(4) 0.004(3) -0.005(3) C37 0.025(3) 0.031(4) 0.043(4) -0.004(3) 0.004(3) -0.001(3) C38 0.022(3) 0.033(4) 0.048(4) -0.016(3) 0.010(3) -0.007(3) C39 0.023(3) 0.045(5) 0.044(4) -0.008(4) 0.004(3) -0.004(3) C40 0.028(4) 0.033(4) 0.056(5) -0.015(3) 0.008(3) -0.006(3) C41 0.024(3) 0.032(4) 0.059(5) -0.006(4) 0.006(3) -0.006(3) C42 0.032(4) 0.026(4) 0.059(5) -0.019(3) 0.005(3) -0.004(3) C43 0.073(6) 0.037(5) 0.080(6) -0.020(4) -0.024(5) -0.008(4) C44 0.049(5) 0.046(5) 0.092(6) -0.019(4) 0.016(4) -0.020(4) C45 0.060(5) 0.031(4) 0.066(5) -0.019(4) -0.005(4) -0.013(4) C46 0.067(5) 0.041(5) 0.054(5) -0.005(4) 0.012(4) -0.011(4) C47 0.027(4) 0.032(4) 0.062(5) -0.012(3) -0.003(3) -0.005(3) C48 0.035(4) 0.031(4) 0.044(4) -0.008(3) 0.000(3) -0.005(3) C49 0.034(4) 0.015(3) 0.038(4) -0.009(3) -0.014(3) 0.012(3) C50 0.027(4) 0.023(4) 0.041(4) -0.006(3) -0.002(3) -0.001(3) C51 0.036(4) 0.056(5) 0.044(4) -0.011(4) -0.010(3) -0.016(4) C52 0.042(4) 0.065(5) 0.031(4) -0.008(4) -0.005(3) -0.007(4) C53 0.031(4) 0.048(5) 0.042(4) -0.016(3) -0.002(3) -0.005(3) C54 0.030(4) 0.018(3) 0.033(4) -0.011(3) -0.005(3) 0.008(3) C55 0.025(3) 0.013(3) 0.033(4) -0.007(3) -0.001(3) 0.000(3) C56 0.029(4) 0.023(4) 0.046(4) -0.014(3) -0.001(3) -0.001(3) C57 0.023(3) 0.034(4) 0.043(4) -0.009(3) 0.004(3) -0.009(3) C58 0.029(4) 0.026(4) 0.040(4) -0.007(3) 0.000(3) -0.002(3) C59 0.028(4) 0.023(4) 0.056(5) -0.012(3) -0.002(3) -0.005(3) C60 0.038(4) 0.046(4) 0.045(4) -0.008(3) 0.003(3) -0.010(3) C61 0.054(5) 0.046(5) 0.066(6) -0.016(4) 0.014(4) -0.024(4) C62 0.048(5) 0.051(5) 0.058(5) -0.021(4) 0.008(4) -0.027(4) C63 0.032(4) 0.042(4) 0.047(4) -0.020(3) -0.001(3) -0.005(3) C64 0.022(3) 0.042(4) 0.047(4) 0.007(3) -0.004(3) -0.012(3) C65 0.032(4) 0.045(5) 0.066(5) -0.007(4) -0.003(4) -0.002(4) C66 0.030(4) 0.047(5) 0.096(7) 0.004(5) -0.017(4) 0.000(4) C67 0.035(4) 0.056(5) 0.094(7) 0.006(5) -0.025(4) -0.012(4) C68 0.049(5) 0.055(5) 0.062(5) -0.003(4) -0.014(4) -0.016(4) C69 0.033(4) 0.039(4) 0.047(4) 0.002(3) -0.006(3) -0.006(3) C70 0.028(4) 0.037(4) 0.054(4) -0.022(4) -0.003(3) -0.010(3) C71 0.038(4) 0.040(4) 0.043(4) -0.017(4) -0.005(3) 0.001(3) C72 0.063(5) 0.042(5) 0.047(5) -0.023(4) -0.011(4) 0.005(4) C73 0.061(5) 0.043(5) 0.068(6) -0.024(4) -0.018(4) 0.008(4) C74 0.040(4) 0.046(5) 0.084(6) -0.041(5) -0.029(4) 0.014(4) C75 0.032(4) 0.035(4) 0.074(5) -0.031(4) 0.002(4) -0.004(3) C76 0.087(6) 0.051(5) 0.051(5) 0.001(4) -0.010(5) -0.012(5) C77 0.086(7) 0.086(7) 0.054(5) -0.016(5) 0.013(5) -0.014(6) C78 0.127(9) 0.063(6) 0.063(6) -0.006(5) -0.002(6) -0.053(6) C79 0.144(10) 0.066(7) 0.060(6) -0.003(5) -0.015(6) -0.009(6) C80 0.040(5) 0.079(7) 0.128(8) -0.063(6) -0.031(5) 0.010(4) C81 0.024(4) 0.031(4) 0.088(6) -0.027(4) -0.008(4) -0.007(3) C82 0.020(3) 0.029(4) 0.098(6) -0.024(4) -0.022(4) 0.004(3) C83 0.024(3) 0.020(4) 0.045(4) -0.010(3) 0.001(3) -0.003(3) C84 0.0217(14) 0.0279(16) 0.0419(17) -0.0065(13) -0.0017(12) -0.0045(12) C85 0.0217(14) 0.0279(16) 0.0419(17) -0.0065(13) -0.0017(12) -0.0045(12) C86 0.0217(14) 0.0279(16) 0.0419(17) -0.0065(13) -0.0017(12) -0.0045(12) C87 0.0217(14) 0.0279(16) 0.0419(17) -0.0065(13) -0.0017(12) -0.0045(12) C88 0.0217(14) 0.0279(16) 0.0419(17) -0.0065(13) -0.0017(12) -0.0045(12) C89 0.023(3) 0.032(4) 0.028(3) 0.006(3) -0.006(3) -0.003(3) C90 0.028(3) 0.027(4) 0.033(4) -0.006(3) -0.002(3) -0.006(3) C91 0.031(4) 0.027(4) 0.039(4) -0.004(3) 0.000(3) -0.006(3) C92 0.032(4) 0.036(4) 0.048(4) -0.009(3) -0.007(3) -0.006(3) C93 0.064(5) 0.053(5) 0.064(5) -0.003(4) -0.021(4) -0.024(4) C94 0.093(7) 0.078(7) 0.086(7) -0.004(5) -0.052(6) -0.028(6) C95 0.072(6) 0.084(7) 0.073(6) -0.022(5) -0.023(5) -0.032(6) C96 0.058(5) 0.055(5) 0.086(7) -0.023(5) -0.007(5) -0.027(4) C97 0.045(4) 0.037(5) 0.069(5) -0.009(4) -0.014(4) -0.008(4) C98 0.040(4) 0.031(4) 0.059(5) -0.012(4) -0.013(4) -0.009(3) C99 0.048(5) 0.047(5) 0.073(6) -0.030(4) -0.015(4) 0.003(4) C100 0.077(6) 0.055(6) 0.092(7) -0.043(5) -0.023(5) 0.012(5) C101 0.109(8) 0.046(6) 0.131(10) -0.057(7) -0.036(7) 0.012(6) C102 0.077(6) 0.025(5) 0.113(8) -0.016(5) -0.042(6) 0.003(4) C103 0.043(4) 0.037(5) 0.070(5) -0.009(4) -0.016(4) -0.011(4) Er2 0.02016(16) 0.02018(17) 0.04323(19) -0.00707(13) -0.00472(13) -0.00006(12) O1A 0.021(2) 0.024(2) 0.053(3) -0.014(2) -0.001(2) 0.0023(18) O2A 0.027(2) 0.027(2) 0.052(3) -0.003(2) -0.009(2) 0.0035(19) O3A 0.032(2) 0.017(2) 0.053(3) -0.008(2) -0.006(2) 0.0015(19) O4A 0.018(2) 0.040(3) 0.065(3) -0.010(2) 0.004(2) 0.001(2) O5A 0.067(4) 0.034(3) 0.108(5) -0.018(3) -0.047(4) 0.017(3) O6A 0.030(2) 0.027(3) 0.071(3) -0.015(2) -0.015(2) 0.006(2) N1A 0.020(3) 0.026(3) 0.047(3) -0.009(2) 0.000(2) 0.000(2) N2A 0.024(3) 0.033(3) 0.045(3) -0.012(3) -0.003(2) -0.004(2) N3A 0.030(3) 0.020(3) 0.036(3) -0.003(2) -0.005(2) 0.002(2) N4A 0.031(3) 0.019(3) 0.041(3) -0.005(2) 0.002(3) 0.003(2) N5A 0.020(3) 0.024(3) 0.042(3) -0.007(2) 0.001(2) 0.002(2) N6A 0.029(3) 0.019(3) 0.043(3) -0.004(2) 0.001(2) -0.004(2) N7A 0.021(3) 0.020(3) 0.039(3) -0.006(2) -0.002(2) 0.003(2) N8A 0.027(3) 0.026(3) 0.039(3) -0.003(2) -0.004(2) 0.006(2) N9A 0.033(3) 0.020(3) 0.044(3) -0.005(2) -0.006(3) -0.002(2) N10A 0.019(3) 0.024(3) 0.039(3) -0.001(2) -0.002(2) 0.004(2) N11A 0.030(3) 0.024(3) 0.046(3) -0.006(3) 0.004(3) -0.007(2) N12A 0.033(3) 0.020(3) 0.042(3) -0.004(2) -0.004(2) -0.004(2) N13A 0.024(3) 0.039(3) 0.053(4) -0.022(3) -0.006(3) 0.007(2) N14A 0.050(4) 0.034(4) 0.102(5) -0.015(4) -0.037(4) 0.006(3) N15A 0.030(3) 0.023(3) 0.057(4) -0.012(3) -0.007(3) -0.002(2) C1A 0.026(4) 0.025(4) 0.071(5) -0.009(4) -0.011(3) 0.007(3) C2A 0.018(3) 0.026(4) 0.075(5) -0.020(4) -0.002(3) -0.003(3) C3A 0.020(4) 0.043(5) 0.085(6) -0.008(4) 0.000(4) 0.001(3) C4A 0.028(4) 0.047(5) 0.083(6) -0.035(5) 0.014(4) -0.012(4) C5A 0.041(4) 0.061(6) 0.065(6) -0.032(5) 0.022(4) -0.020(4) C6A 0.024(4) 0.052(5) 0.071(6) -0.022(4) 0.013(4) -0.010(3) C7A 0.009(3) 0.036(4) 0.073(5) -0.018(4) 0.000(3) 0.000(3) C8A 0.048(5) 0.058(6) 0.143(9) -0.058(6) -0.001(5) 0.003(4) C12A 0.048(5) 0.062(5) 0.060(5) -0.012(4) 0.008(4) -0.016(4) C13A 0.020(3) 0.031(4) 0.071(5) -0.011(4) 0.004(3) 0.002(3) C14A 0.019(3) 0.044(4) 0.062(5) -0.020(4) 0.000(3) 0.005(3) C15A 0.0167(19) 0.029(2) 0.053(3) -0.0158(19) -0.0037(17) -0.0013(17) C16A 0.022(3) 0.030(4) 0.041(4) -0.009(3) 0.002(3) 0.008(3) C17A 0.032(4) 0.071(6) 0.053(5) -0.027(4) 0.006(4) 0.008(4) C18A 0.038(4) 0.082(6) 0.035(4) -0.020(4) 0.000(3) 0.020(4) C19A 0.026(4) 0.048(5) 0.047(4) -0.013(4) -0.006(3) 0.007(3) C20A 0.024(4) 0.027(4) 0.041(4) -0.007(3) 0.008(3) -0.008(3) C21A 0.029(4) 0.018(3) 0.031(4) -0.005(3) -0.011(3) 0.012(3) C22A 0.025(3) 0.017(3) 0.045(4) -0.005(3) -0.001(3) 0.001(3) C23A 0.025(3) 0.016(3) 0.041(4) -0.007(3) 0.001(3) 0.000(3) C24A 0.024(3) 0.022(3) 0.043(4) 0.002(3) -0.002(3) -0.007(3) C25A 0.029(4) 0.024(4) 0.045(4) 0.002(3) -0.001(3) -0.009(3) C26A 0.033(4) 0.036(4) 0.044(4) 0.008(3) -0.012(3) -0.004(3) C27A 0.022(3) 0.038(4) 0.054(5) 0.007(3) -0.006(3) -0.002(3) C28A 0.023(4) 0.036(4) 0.059(5) 0.000(3) -0.002(3) 0.002(3) C29A 0.023(3) 0.031(4) 0.040(4) -0.003(3) -0.004(3) -0.003(3) C30A 0.022(3) 0.019(3) 0.040(4) 0.001(3) -0.001(3) 0.005(3) C31A 0.026(4) 0.037(4) 0.042(4) 0.001(3) -0.002(3) 0.003(3) C32A 0.038(4) 0.032(4) 0.062(5) 0.003(4) 0.006(4) -0.001(3) C33A 0.047(5) 0.037(5) 0.061(5) 0.004(4) 0.013(4) 0.018(4) C34A 0.054(5) 0.029(4) 0.037(4) -0.003(3) 0.005(3) 0.010(4) C35A 0.035(4) 0.027(4) 0.048(4) 0.000(3) -0.003(3) 0.009(3) C36A 0.040(4) 0.021(4) 0.079(5) -0.001(4) -0.021(4) -0.002(3) C37A 0.031(4) 0.020(4) 0.075(5) -0.005(3) -0.015(3) 0.000(3) C38A 0.035(4) 0.023(4) 0.084(6) 0.009(4) -0.020(4) -0.001(3) C39A 0.027(4) 0.038(5) 0.166(10) -0.006(5) -0.039(5) 0.005(4) C40A 0.054(5) 0.030(5) 0.180(11) -0.018(6) -0.058(6) -0.004(4) C41A 0.051(5) 0.026(4) 0.125(8) -0.014(5) -0.043(5) 0.016(4) C42A 0.034(4) 0.052(5) 0.060(5) 0.010(4) -0.003(4) 0.001(4) C43A 0.034(4) 0.050(5) 0.089(6) -0.008(4) -0.014(4) 0.004(4) C44A 0.044(5) 0.074(6) 0.071(6) 0.012(5) -0.002(4) 0.028(4) C45A 0.043(5) 0.096(7) 0.086(7) -0.006(5) 0.001(4) -0.024(5) C47A 0.054(5) 0.026(4) 0.139(10) -0.020(5) -0.050(6) 0.018(4) C48A 0.067(6) 0.030(5) 0.121(8) -0.004(5) -0.052(6) 0.011(4) C49A 0.0167(19) 0.029(2) 0.053(3) -0.0158(19) -0.0037(17) -0.0013(17) C50A 0.021(3) 0.028(4) 0.057(4) -0.007(3) -0.010(3) 0.008(3) C51A 0.036(4) 0.031(4) 0.079(6) -0.013(4) -0.023(4) -0.001(3) C52A 0.024(4) 0.051(5) 0.092(6) -0.030(4) -0.022(4) 0.000(3) C53A 0.035(4) 0.033(4) 0.068(5) -0.014(4) -0.004(4) -0.013(3) C54A 0.021(3) 0.023(4) 0.047(4) -0.009(3) -0.003(3) 0.001(3) C55A 0.021(3) 0.024(4) 0.046(4) -0.013(3) 0.006(3) 0.000(3) C56A 0.034(4) 0.025(4) 0.042(4) -0.013(3) 0.012(3) 0.000(3) C57A 0.036(4) 0.020(4) 0.040(4) -0.006(3) 0.001(3) 0.007(3) C58A 0.051(4) 0.017(4) 0.049(4) -0.007(3) 0.006(3) 0.007(3) C59A 0.049(5) 0.039(5) 0.068(5) -0.006(4) 0.010(4) -0.019(4) C60A 0.076(6) 0.035(5) 0.077(6) -0.014(4) 0.008(5) -0.019(5) C61A 0.103(8) 0.028(5) 0.074(6) -0.004(4) -0.002(5) -0.016(5) C62A 0.089(7) 0.028(5) 0.077(6) -0.010(4) -0.021(5) 0.010(4) C63A 0.067(5) 0.030(5) 0.072(6) -0.009(4) -0.011(4) 0.000(4) C64A 0.047(4) 0.019(4) 0.051(5) -0.009(3) -0.007(3) 0.007(3) C65A 0.068(5) 0.041(5) 0.049(5) -0.004(4) -0.006(4) 0.009(4) C66A 0.134(10) 0.045(5) 0.054(6) 0.010(4) -0.018(6) 0.017(6) C67A 0.089(8) 0.060(6) 0.085(8) -0.005(5) -0.033(6) 0.009(5) C68A 0.073(6) 0.045(5) 0.071(6) 0.008(4) -0.033(5) 0.006(4) C69A 0.059(5) 0.024(4) 0.053(5) -0.005(3) -0.017(4) 0.005(3) C70A 0.033(4) 0.025(4) 0.085(6) -0.014(4) -0.012(4) -0.001(3) C71A 0.039(4) 0.036(5) 0.095(7) -0.010(4) -0.019(4) 0.002(4) C72A 0.048(5) 0.051(5) 0.071(6) -0.001(4) -0.010(4) -0.005(4) C73A 0.059(5) 0.049(5) 0.069(6) 0.002(4) -0.005(4) -0.009(4) C74A 0.039(4) 0.044(5) 0.075(6) -0.011(4) -0.002(4) -0.011(4) C75A 0.042(5) 0.031(4) 0.077(6) -0.016(4) -0.013(4) -0.008(4) C76A 0.068(6) 0.062(6) 0.086(7) 0.006(5) -0.024(5) -0.004(5) C80A 0.068(6) 0.063(6) 0.067(6) -0.010(5) -0.003(5) -0.013(5) C81A 0.034(4) 0.024(4) 0.067(5) -0.018(3) -0.008(3) -0.003(3) C82A 0.037(4) 0.023(4) 0.060(5) -0.022(3) -0.001(3) -0.003(3) C83A 0.0167(19) 0.029(2) 0.053(3) -0.0158(19) -0.0037(17) -0.0013(17) C84A 0.030(3) 0.022(4) 0.043(4) -0.005(3) -0.008(3) -0.003(3) C85A 0.069(5) 0.019(4) 0.056(5) -0.012(3) -0.002(4) -0.012(4) C86A 0.065(5) 0.028(4) 0.053(5) -0.007(3) 0.012(4) -0.026(4) C87A 0.048(4) 0.031(4) 0.044(4) -0.003(3) 0.002(3) -0.013(3) C88A 0.029(3) 0.023(4) 0.035(4) -0.002(3) -0.003(3) -0.006(3) C89A 0.026(3) 0.018(3) 0.044(4) -0.003(3) -0.009(3) -0.002(3) C90A 0.030(3) 0.023(4) 0.043(4) -0.003(3) -0.014(3) 0.002(3) C91A 0.024(3) 0.020(3) 0.048(4) -0.002(3) -0.007(3) 0.001(3) C92A 0.034(4) 0.028(4) 0.046(4) -0.010(3) -0.008(3) -0.007(3) C93A 0.087(6) 0.025(4) 0.043(5) -0.001(4) -0.005(4) 0.002(4) C94A 0.128(8) 0.047(6) 0.041(5) -0.008(4) 0.001(5) -0.009(5) C95A 0.094(7) 0.038(5) 0.054(5) -0.018(4) -0.004(5) 0.004(4) C96A 0.054(5) 0.037(4) 0.058(5) -0.012(4) -0.007(4) -0.003(4) C97A 0.032(4) 0.033(4) 0.045(4) -0.005(3) -0.006(3) -0.007(3) C98A 0.023(3) 0.026(4) 0.058(5) -0.009(3) 0.005(3) -0.002(3) C99A 0.032(4) 0.040(4) 0.067(5) -0.012(4) -0.004(4) -0.009(3) C104 0.042(4) 0.040(5) 0.087(6) -0.023(5) -0.013(4) -0.010(4) C105 0.032(4) 0.039(5) 0.105(7) -0.022(5) 0.004(4) -0.008(4) C106 0.044(4) 0.032(4) 0.075(6) -0.001(4) 0.013(4) -0.002(4) C107 0.029(4) 0.025(4) 0.063(5) -0.010(4) 0.004(3) -0.001(3) O9 0.092(5) 0.108(6) 0.058(4) -0.027(4) 0.010(4) 0.005(4) N17 0.083(6) 0.060(5) 0.054(5) -0.006(4) -0.020(4) -0.012(4) O10 0.054(3) 0.056(3) 0.043(3) -0.012(3) -0.007(2) -0.004(3) O11 0.093(6) 0.106(6) 0.142(7) -0.055(5) 0.040(5) -0.044(5) O12 0.178(8) 0.078(5) 0.102(6) -0.010(4) -0.094(6) -0.009(5) N18 0.028(3) 0.032(3) 0.059(4) -0.007(3) -0.003(3) -0.001(3) O13 0.040(3) 0.030(3) 0.047(3) -0.013(2) -0.006(2) 0.006(2) O14 0.036(3) 0.043(3) 0.062(3) -0.014(2) -0.009(2) -0.002(2) O15 0.035(3) 0.093(5) 0.082(4) -0.033(4) -0.004(3) 0.011(3) N19 0.129(10) 0.103(8) 0.064(6) -0.012(6) 0.015(6) -0.040(7) O16 0.207(12) 0.166(11) 0.119(8) 0.028(8) -0.073(8) -0.057(9) O17 0.057(3) 0.097(5) 0.043(3) -0.021(3) 0.002(3) -0.039(3) O18 0.107(6) 0.292(14) 0.121(7) -0.125(9) 0.036(5) -0.104(8) N20 0.067(5) 0.054(5) 0.061(5) -0.010(4) 0.026(4) -0.024(4) O19 0.104(4) 0.070(3) 0.096(4) -0.017(3) -0.027(3) -0.012(3) O20 0.104(4) 0.070(3) 0.096(4) -0.017(3) -0.027(3) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.310(4) . ? Er1 O3 2.312(4) . ? Er1 O2 2.335(4) . ? Er1 N2 2.479(5) . ? Er1 N3 2.486(5) . ? Er1 N1 2.503(5) . ? Er1 N6 2.519(5) . ? Er1 N5 2.529(5) . ? Er1 N4 2.530(5) . ? N1 C16 1.335(8) . ? N1 C20 1.343(8) . ? N2 C54 1.342(7) . ? N2 C50 1.363(7) . ? N3 C88 1.296(7) . ? N3 C84 1.336(7) . ? N4 C21 1.329(7) . ? N4 N7 1.344(7) . ? N5 C55 1.317(8) . ? N5 N8 1.344(7) . ? N6 C89 1.341(7) . ? N6 N9 1.350(7) . ? N7 C23 1.330(8) . ? N8 C57 1.337(8) . ? N9 C91 1.329(8) . ? N10 C22 1.332(8) . ? N10 C21 1.361(8) . ? N11 C55 1.336(7) . ? N11 C56 1.343(8) . ? N12 C90 1.320(8) . ? N12 C89 1.354(7) . ? N13 C15 1.294(7) . ? N13 C14 1.462(8) . ? N13 H13E 0.8800 . ? N14 C49 1.300(7) . ? N14 C48 1.464(8) . ? N14 H14E 0.8800 . ? N15 C83 1.316(8) . ? N15 C82 1.475(8) . ? N15 H15A 0.8800 . ? O1 C15 1.256(7) . ? O2 C49 1.277(7) . ? O3 C83 1.271(7) . ? O4 C7 1.384(7) . ? O4 C13 1.438(7) . ? O5 C41 1.410(8) . ? O5 C47 1.424(8) . ? O6 C75 1.394(9) . ? O6 C81 1.450(8) . ? C1 C70 1.524(10) . ? C1 C36 1.532(9) . ? C1 C2 1.537(9) . ? C1 H1A 1.0000 . ? C2 C3 1.389(9) . ? C2 C7 1.397(9) . ? C3 C4 1.387(10) . ? C3 H3A 0.9500 . ? C4 C5 1.387(10) . ? C4 C8 1.553(10) . ? C5 C6 1.384(10) . ? C5 H5A 0.9500 . ? C6 C7 1.402(9) . ? C6 C12 1.525(9) . ? C8 C9' 1.512(14) . ? C8 C11 1.514(12) . ? C8 C9 1.549(12) . ? C8 C10' 1.583(14) . ? C8 C10 1.587(12) . ? C8 C11' 1.612(14) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C9' H9'A 0.9800 . ? C9' H9'B 0.9800 . ? C9' H9'C 0.9800 . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.510(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.511(9) . ? C16 C17 1.373(9) . ? C17 C18 1.391(10) . ? C17 H17A 0.9500 . ? C18 C19 1.376(10) . ? C18 H18A 0.9500 . ? C19 C20 1.365(9) . ? C19 H19A 0.9500 . ? C20 C21 1.497(9) . ? C22 C23 1.427(8) . ? C22 C24 1.475(9) . ? C23 C30 1.487(10) . ? C24 C25 1.384(9) . ? C24 C29 1.414(9) . ? C25 C26 1.394(9) . ? C25 H25A 0.9500 . ? C26 C27 1.397(10) . ? C26 H26A 0.9500 . ? C27 C28 1.371(11) . ? C27 H27A 0.9500 . ? C28 C29 1.375(11) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.390(11) . ? C30 C35 1.410(11) . ? C31 C32 1.398(11) . ? C31 H31A 0.9500 . ? C32 C33 1.437(16) . ? C32 H32A 0.9500 . ? C33 C34 1.386(18) . ? C33 H33A 0.9500 . ? C34 C35 1.389(14) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C41 1.384(10) . ? C36 C37 1.406(9) . ? C37 C38 1.391(9) . ? C37 H37A 0.9500 . ? C38 C39 1.388(9) . ? C38 C42 1.539(9) . ? C39 C40 1.406(9) . ? C39 H39A 0.9500 . ? C40 C41 1.392(9) . ? C40 C46 1.499(10) . ? C42 C43 1.516(10) . ? C42 C45 1.528(9) . ? C42 C44 1.535(9) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.517(8) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.494(9) . ? C50 C51 1.400(9) . ? C51 C52 1.378(9) . ? C51 H51A 0.9500 . ? C52 C53 1.401(9) . ? C52 H52A 0.9500 . ? C53 C54 1.396(9) . ? C53 H53A 0.9500 . ? C54 C55 1.489(8) . ? C56 C57 1.441(9) . ? C56 C58 1.478(9) . ? C57 C64 1.482(9) . ? C58 C59 1.390(9) . ? C58 C63 1.393(9) . ? C59 C60 1.387(9) . ? C59 H59A 0.9500 . ? C60 C61 1.381(10) . ? C60 H60A 0.9500 . ? C61 C62 1.392(10) . ? C61 H61A 0.9500 . ? C62 C63 1.388(9) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? C64 C69 1.381(9) . ? C64 C65 1.396(10) . ? C65 C66 1.397(10) . ? C65 H65A 0.9500 . ? C66 C67 1.359(11) . ? C66 H66A 0.9500 . ? C67 C68 1.392(11) . ? C67 H67A 0.9500 . ? C68 C69 1.371(10) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? C70 C71 1.361(9) . ? C70 C75 1.407(9) . ? C71 C72 1.398(10) . ? C71 H71A 0.9500 . ? C72 C73 1.398(11) . ? C72 C76 1.531(11) . ? C73 C74 1.384(11) . ? C73 H73A 0.9500 . ? C74 C75 1.399(11) . ? C74 C80 1.510(10) . ? C76 C79 1.526(12) . ? C76 C77 1.534(12) . ? C76 C78 1.546(11) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.504(10) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.510(8) . ? C84 C85 1.382(9) . ? C85 C86 1.400(8) . ? C85 H85A 0.9500 . ? C86 C87 1.367(8) . ? C86 H86A 0.9500 . ? C87 C88 1.414(9) . ? C87 H87A 0.9500 . ? C88 C89 1.457(9) . ? C90 C91 1.426(9) . ? C90 C92 1.486(8) . ? C91 C98 1.490(9) . ? C92 C93 1.390(10) . ? C92 C97 1.391(9) . ? C93 C94 1.400(10) . ? C93 H93A 0.9500 . ? C94 C95 1.385(12) . ? C94 H94A 0.9500 . ? C95 C96 1.341(12) . ? C95 H95A 0.9500 . ? C96 C97 1.396(10) . ? C96 H96A 0.9500 . ? C97 H97A 0.9500 . ? C98 C103 1.382(10) . ? C98 C99 1.397(10) . ? C99 C100 1.395(11) . ? C99 H99A 0.9500 . ? C100 C101 1.408(14) . ? C100 H10G 0.9500 . ? C101 C102 1.343(13) . ? C101 H10H 0.9500 . ? C102 C103 1.403(11) . ? C102 H10I 0.9500 . ? C103 H10J 0.9500 . ? Er2 O3A 2.327(4) . ? Er2 O1A 2.336(4) . ? Er2 O2A 2.339(4) . ? Er2 N1A 2.463(5) . ? Er2 N2A 2.498(5) . ? Er2 N3A 2.510(5) . ? Er2 N5A 2.518(5) . ? Er2 N6A 2.539(5) . ? Er2 N4A 2.541(5) . ? O1A C15A 1.242(7) . ? O2A C49A 1.231(7) . ? O3A C83A 1.241(7) . ? O4A C7A 1.387(8) . ? O4A C13A 1.446(7) . ? O5A C41A 1.386(10) . ? O5A C47A 1.421(11) . ? O6A C75A 1.385(9) . ? O6A C81A 1.448(7) . ? N1A C20A 1.341(8) . ? N1A C16A 1.347(8) . ? N2A C54A 1.338(8) . ? N2A C50A 1.356(8) . ? N3A C88A 1.346(8) . ? N3A C84A 1.351(7) . ? N4A N7A 1.338(7) . ? N4A C21A 1.346(7) . ? N5A N8A 1.341(7) . ? N5A C55A 1.345(7) . ? N6A C89A 1.339(8) . ? N6A N9A 1.348(7) . ? N7A C22A 1.352(7) . ? N8A C57A 1.331(8) . ? N9A C91A 1.337(8) . ? N10A C21A 1.321(7) . ? N10A C23A 1.327(7) . ? N11A C56A 1.318(8) . ? N11A C55A 1.345(8) . ? N12A C89A 1.331(8) . ? N12A C90A 1.351(8) . ? N13A C15A 1.337(8) . ? N13A C14A 1.451(8) . ? N13A H13F 0.8800 . ? N14A C49A 1.325(8) . ? N14A C48A 1.493(9) . ? N14A H14F 0.8800 . ? N15A C83A 1.329(8) . ? N15A C82A 1.464(8) . ? N15A H15B 0.8800 . ? C1A C70A 1.510(10) . ? C1A C2A 1.529(9) . ? C1A C36A 1.557(9) . ? C1A H1AA 1.0000 . ? C2A C7A 1.377(10) . ? C2A C3A 1.416(9) . ? C3A C4A 1.407(10) . ? C3A H3AA 0.9500 . ? C4A C5A 1.364(11) . ? C4A C8A 1.550(11) . ? C5A C6A 1.398(11) . ? C5A H5AA 0.9500 . ? C6A C7A 1.400(10) . ? C6A C12A 1.520(11) . ? C8A C11B 1.462(13) . ? C8A C10A 1.513(13) . ? C8A C9A 1.539(14) . ? C8A C9B 1.582(13) . ? C8A C10B 1.647(13) . ? C8A C11A 1.667(14) . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C10A H10K 0.9800 . ? C10A H10L 0.9800 . ? C10A H10M 0.9800 . ? C11A H11G 0.9800 . ? C11A H11H 0.9800 . ? C11A H11I 0.9800 . ? C9B H9BA 0.9800 . ? C9B H9BB 0.9800 . ? C9B H9BC 0.9800 . ? C10B H10N 0.9800 . ? C10B H10O 0.9800 . ? C10B H10P 0.9800 . ? C11B H11J 0.9800 . ? C11B H11K 0.9800 . ? C11B H11L 0.9800 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A C14A 1.510(9) . ? C13A H13C 0.9900 . ? C13A H13D 0.9900 . ? C14A H14C 0.9900 . ? C14A H14D 0.9900 . ? C15A C16A 1.502(8) . ? C16A C17A 1.390(9) . ? C17A C18A 1.365(10) . ? C17A H17B 0.9500 . ? C18A C19A 1.396(9) . ? C18A H18B 0.9500 . ? C19A C20A 1.385(9) . ? C19A H19B 0.9500 . ? C20A C21A 1.508(8) . ? C22A C23A 1.419(9) . ? C22A C30A 1.477(8) . ? C23A C24A 1.480(8) . ? C24A C25A 1.392(9) . ? C24A C29A 1.396(9) . ? C25A C26A 1.392(9) . ? C25A H25B 0.9500 . ? C26A C27A 1.389(9) . ? C26A H26B 0.9500 . ? C27A C28A 1.366(9) . ? C27A H27B 0.9500 . ? C28A C29A 1.401(9) . ? C28A H28B 0.9500 . ? C29A H29B 0.9500 . ? C30A C31A 1.388(8) . ? C30A C35A 1.402(9) . ? C31A C32A 1.399(9) . ? C31A H31B 0.9500 . ? C32A C33A 1.357(10) . ? C32A H32B 0.9500 . ? C33A C34A 1.386(10) . ? C33A H33B 0.9500 . ? C34A C35A 1.393(9) . ? C34A H34B 0.9500 . ? C35A H35B 0.9500 . ? C36A C37A 1.377(10) . ? C36A C41A 1.391(10) . ? C37A C38A 1.389(9) . ? C37A H37B 0.9500 . ? C38A C39A 1.392(11) . ? C38A C42A 1.530(10) . ? C39A C40A 1.379(12) . ? C39A H39B 0.9500 . ? C40A C41A 1.410(11) . ? C40A C46B 1.482(16) . ? C40A C46A 1.691(18) . ? C42A C43A 1.523(10) . ? C42A C45A 1.539(10) . ? C42A C44A 1.546(10) . ? C43A H43D 0.9800 . ? C43A H43E 0.9800 . ? C43A H43F 0.9800 . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? C45A H45D 0.9800 . ? C45A H45E 0.9800 . ? C45A H45F 0.9800 . ? C46A H46D 0.9800 . ? C46A H46E 0.9800 . ? C46A H46F 0.9800 . ? C46B H46G 0.9800 . ? C46B H46H 0.9800 . ? C46B H46I 0.9800 . ? C47A C48A 1.510(12) . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? C48A H48C 0.9900 . ? C48A H48D 0.9900 . ? C49A C50A 1.448(9) . ? C50A C51A 1.404(9) . ? C51A C52A 1.381(10) . ? C51A H51B 0.9500 . ? C52A C53A 1.375(10) . ? C52A H52B 0.9500 . ? C53A C54A 1.395(9) . ? C53A H53B 0.9500 . ? C54A C55A 1.458(9) . ? C56A C57A 1.412(9) . ? C56A C58A 1.506(9) . ? C57A C64A 1.488(9) . ? C58A C63A 1.363(10) . ? C58A C59A 1.408(10) . ? C59A C60A 1.404(10) . ? C59A H59B 0.9500 . ? C60A C61A 1.373(12) . ? C60A H60B 0.9500 . ? C61A C62A 1.344(12) . ? C61A H61B 0.9500 . ? C62A C63A 1.409(11) . ? C62A H62B 0.9500 . ? C63A H63B 0.9500 . ? C64A C65A 1.398(10) . ? C64A C69A 1.402(10) . ? C65A C66A 1.382(12) . ? C65A H65B 0.9500 . ? C66A C67A 1.413(13) . ? C66A H66B 0.9500 . ? C67A C68A 1.347(13) . ? C67A H67B 0.9500 . ? C68A C69A 1.363(10) . ? C68A H68B 0.9500 . ? C69A H69B 0.9500 . ? C70A C71A 1.393(10) . ? C70A C75A 1.399(10) . ? C71A C72A 1.397(11) . ? C71A H71B 0.9500 . ? C72A C73A 1.393(11) . ? C72A C76A 1.549(11) . ? C73A C74A 1.399(11) . ? C73A H73B 0.9500 . ? C74A C75A 1.392(11) . ? C74A C80A 1.492(11) . ? C76A C77B 1.542(12) . ? C76A C78A 1.542(17) . ? C76A C79B 1.570(12) . ? C76A C77A 1.574(18) . ? C76A C78B 1.577(12) . ? C76A C79A 1.598(17) . ? C79A H79D 0.9800 . ? C79A H79E 0.9800 . ? C79A H79F 0.9800 . ? C77A H77D 0.9800 . ? C77A H77E 0.9800 . ? C77A H77F 0.9800 . ? C78A H78D 0.9800 . ? C78A H78E 0.9800 . ? C78A H78F 0.9800 . ? C79B H79G 0.9800 . ? C79B H79H 0.9800 . ? C79B H79I 0.9800 . ? C77B H77G 0.9800 . ? C77B H77H 0.9800 . ? C77B H77I 0.9800 . ? C78B H78G 0.9800 . ? C78B H78H 0.9800 . ? C78B H78I 0.9800 . ? C80A H80D 0.9800 . ? C80A H80E 0.9800 . ? C80A H80F 0.9800 . ? C81A C82A 1.507(9) . ? C81A H81C 0.9900 . ? C81A H81D 0.9900 . ? C82A H82C 0.9900 . ? C82A H82D 0.9900 . ? C83A C84A 1.498(9) . ? C84A C85A 1.377(9) . ? C85A C86A 1.369(10) . ? C85A H85B 0.9500 . ? C86A C87A 1.389(9) . ? C86A H86B 0.9500 . ? C87A C88A 1.382(9) . ? C87A H87B 0.9500 . ? C88A C89A 1.486(8) . ? C90A C91A 1.414(9) . ? C90A C92A 1.478(9) . ? C91A C98A 1.493(8) . ? C92A C97A 1.373(9) . ? C92A C93A 1.391(10) . ? C93A C94A 1.380(11) . ? C93A H93B 0.9500 . ? C94A C95A 1.377(11) . ? C94A H94B 0.9500 . ? C95A C96A 1.382(11) . ? C95A H95B 0.9500 . ? C96A C97A 1.395(9) . ? C96A H96B 0.9500 . ? C97A H97B 0.9500 . ? C98A C107 1.393(9) . ? C98A C99A 1.399(9) . ? C99A C104 1.385(10) . ? C99A H99B 0.9500 . ? C104 C105 1.366(11) . ? C104 H10Q 0.9500 . ? C105 C106 1.364(11) . ? C105 H10R 0.9500 . ? C106 C107 1.395(9) . ? C106 H10S 0.9500 . ? C107 H10T 0.9500 . ? N16 O8 1.169(11) . ? N16 O9 1.264(12) . ? N16 O7 1.296(13) . ? N16' O9 1.03(2) . ? N16' O8' 1.31(3) . ? N16' O7' 1.46(2) . ? N17 O11 1.244(9) . ? N17 O12 1.250(9) . ? N17 O10 1.285(8) . ? N18 O15 1.236(7) . ? N18 O14 1.256(7) . ? N18 O13 1.259(7) . ? N19 O18 1.156(11) . ? N19 O17 1.207(12) . ? N19 O16 1.258(14) . ? N20 O21" 1.156(17) . ? N20 O21' 1.177(13) . ? N20 O20 1.231(9) . ? N20 O19 1.381(9) . ? N20 O21 1.392(14) . ? N21 O22 1.201(15) . ? N21 O23 1.262(16) . ? N21 O24 1.276(16) . ? N21' O23' 1.10(3) . ? N21' O22' 1.22(2) . ? N21' O24' 1.39(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O3 75.81(15) . . ? O1 Er1 O2 78.72(14) . . ? O3 Er1 O2 77.49(13) . . ? O1 Er1 N2 137.47(15) . . ? O3 Er1 N2 74.08(15) . . ? O2 Er1 N2 65.97(14) . . ? O1 Er1 N3 71.78(15) . . ? O3 Er1 N3 66.53(14) . . ? O2 Er1 N3 137.74(14) . . ? N2 Er1 N3 120.52(15) . . ? O1 Er1 N1 65.36(16) . . ? O3 Er1 N1 135.54(15) . . ? O2 Er1 N1 74.55(14) . . ? N2 Er1 N1 122.35(16) . . ? N3 Er1 N1 117.03(16) . . ? O1 Er1 N6 90.79(15) . . ? O3 Er1 N6 130.05(15) . . ? O2 Er1 N6 147.40(15) . . ? N2 Er1 N6 131.69(15) . . ? N3 Er1 N6 63.58(15) . . ? N1 Er1 N6 73.03(15) . . ? O1 Er1 N5 144.89(16) . . ? O3 Er1 N5 89.01(15) . . ? O2 Er1 N5 129.20(15) . . ? N2 Er1 N5 63.23(15) . . ? N3 Er1 N5 73.14(16) . . ? N1 Er1 N5 135.39(15) . . ? N6 Er1 N5 74.88(15) . . ? O1 Er1 N4 129.30(15) . . ? O3 Er1 N4 146.84(15) . . ? O2 Er1 N4 86.27(14) . . ? N2 Er1 N4 72.93(15) . . ? N3 Er1 N4 135.93(14) . . ? N1 Er1 N4 63.98(16) . . ? N6 Er1 N4 76.65(15) . . ? N5 Er1 N4 79.08(16) . . ? C16 N1 C20 118.2(5) . . ? C16 N1 Er1 118.6(4) . . ? C20 N1 Er1 123.2(4) . . ? C54 N2 C50 117.5(5) . . ? C54 N2 Er1 124.1(4) . . ? C50 N2 Er1 118.2(4) . . ? C88 N3 C84 119.3(5) . . ? C88 N3 Er1 122.6(4) . . ? C84 N3 Er1 118.0(4) . . ? C21 N4 N7 118.2(5) . . ? C21 N4 Er1 120.6(4) . . ? N7 N4 Er1 121.1(3) . . ? C55 N5 N8 117.8(5) . . ? C55 N5 Er1 121.5(4) . . ? N8 N5 Er1 120.5(4) . . ? C89 N6 N9 118.7(5) . . ? C89 N6 Er1 120.7(4) . . ? N9 N6 Er1 120.3(4) . . ? C23 N7 N4 120.0(5) . . ? C57 N8 N5 119.7(5) . . ? C91 N9 N6 119.8(5) . . ? C22 N10 C21 116.7(5) . . ? C55 N11 C56 117.2(5) . . ? C90 N12 C89 118.3(5) . . ? C15 N13 C14 123.6(5) . . ? C15 N13 H13E 118.2 . . ? C14 N13 H13E 118.2 . . ? C49 N14 C48 121.8(5) . . ? C49 N14 H14E 119.1 . . ? C48 N14 H14E 119.1 . . ? C83 N15 C82 123.8(5) . . ? C83 N15 H15A 118.1 . . ? C82 N15 H15A 118.1 . . ? C15 O1 Er1 125.9(4) . . ? C49 O2 Er1 123.1(4) . . ? C83 O3 Er1 123.5(4) . . ? C7 O4 C13 113.9(5) . . ? C41 O5 C47 115.4(4) . . ? C75 O6 C81 113.3(5) . . ? C70 C1 C36 115.7(5) . . ? C70 C1 C2 111.1(5) . . ? C36 C1 C2 110.5(5) . . ? C70 C1 H1A 106.3 . . ? C36 C1 H1A 106.3 . . ? C2 C1 H1A 106.3 . . ? C3 C2 C7 118.2(6) . . ? C3 C2 C1 123.1(6) . . ? C7 C2 C1 118.8(5) . . ? C4 C3 C2 122.3(6) . . ? C4 C3 H3A 118.8 . . ? C2 C3 H3A 118.8 . . ? C5 C4 C3 117.7(6) . . ? C5 C4 C8 121.2(7) . . ? C3 C4 C8 121.0(6) . . ? C6 C5 C4 122.5(7) . . ? C6 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? C5 C6 C7 118.1(6) . . ? C5 C6 C12 121.7(7) . . ? C7 C6 C12 120.1(6) . . ? O4 C7 C2 118.6(6) . . ? O4 C7 C6 120.1(5) . . ? C2 C7 C6 121.0(6) . . ? C9' C8 C11 133.8(12) . . ? C9' C8 C9 50.9(9) . . ? C11 C8 C9 112.9(9) . . ? C9' C8 C4 114.4(11) . . ? C11 C8 C4 111.8(8) . . ? C9 C8 C4 108.1(8) . . ? C9' C8 C10' 112.2(11) . . ? C11 C8 C10' 51.6(9) . . ? C9 C8 C10' 144.0(12) . . ? C4 C8 C10' 107.8(10) . . ? C9' C8 C10 56.9(10) . . ? C11 C8 C10 111.1(9) . . ? C9 C8 C10 107.5(8) . . ? C4 C8 C10 105.1(8) . . ? C10' C8 C10 62.6(10) . . ? C9' C8 C11' 110.5(11) . . ? C11 C8 C11' 55.3(9) . . ? C9 C8 C11' 63.7(10) . . ? C4 C8 C11' 104.9(11) . . ? C10' C8 C11' 106.4(10) . . ? C10 C8 C11' 150.0(12) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C9' H9'A 109.5 . . ? C8 C9' H9'B 109.5 . . ? H9'A C9' H9'B 109.5 . . ? C8 C9' H9'C 109.5 . . ? H9'A C9' H9'C 109.5 . . ? H9'B C9' H9'C 109.5 . . ? C8 C10' H10D 109.5 . . ? C8 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C8 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C8 C11' H11D 109.5 . . ? C8 C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C8 C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 C14 106.5(5) . . ? O4 C13 H13A 110.4 . . ? C14 C13 H13A 110.4 . . ? O4 C13 H13B 110.4 . . ? C14 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? N13 C14 C13 110.6(5) . . ? N13 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? N13 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O1 C15 N13 123.1(6) . . ? O1 C15 C16 117.3(5) . . ? N13 C15 C16 119.6(5) . . ? N1 C16 C17 122.3(6) . . ? N1 C16 C15 112.4(5) . . ? C17 C16 C15 125.3(6) . . ? C16 C17 C18 119.2(6) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? C19 C18 C17 118.4(7) . . ? C19 C18 H18A 120.8 . . ? C17 C18 H18A 120.8 . . ? C20 C19 C18 119.1(7) . . ? C20 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? N1 C20 C19 122.9(6) . . ? N1 C20 C21 114.1(5) . . ? C19 C20 C21 123.0(6) . . ? N4 C21 N10 125.2(5) . . ? N4 C21 C20 117.8(5) . . ? N10 C21 C20 116.9(5) . . ? N10 C22 C23 119.0(5) . . ? N10 C22 C24 115.8(5) . . ? C23 C22 C24 125.2(6) . . ? N7 C23 C22 120.5(6) . . ? N7 C23 C30 112.9(5) . . ? C22 C23 C30 126.5(6) . . ? C25 C24 C29 119.2(6) . . ? C25 C24 C22 118.6(6) . . ? C29 C24 C22 122.3(6) . . ? C24 C25 C26 120.1(6) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C27 120.5(7) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C28 C27 C26 118.7(7) . . ? C28 C27 H27A 120.7 . . ? C26 C27 H27A 120.7 . . ? C27 C28 C29 122.1(7) . . ? C27 C28 H28A 118.9 . . ? C29 C28 H28A 118.9 . . ? C28 C29 C24 119.4(7) . . ? C28 C29 H29A 120.3 . . ? C24 C29 H29A 120.3 . . ? C31 C30 C35 120.3(8) . . ? C31 C30 C23 120.9(7) . . ? C35 C30 C23 118.4(8) . . ? C30 C31 C32 122.5(9) . . ? C30 C31 H31A 118.8 . . ? C32 C31 H31A 118.8 . . ? C31 C32 C33 115.5(10) . . ? C31 C32 H32A 122.3 . . ? C33 C32 H32A 122.3 . . ? C34 C33 C32 122.4(9) . . ? C34 C33 H33A 118.8 . . ? C32 C33 H33A 118.8 . . ? C33 C34 C35 120.0(10) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C34 C35 C30 119.0(10) . . ? C34 C35 H35A 120.5 . . ? C30 C35 H35A 120.5 . . ? C41 C36 C37 117.7(6) . . ? C41 C36 C1 120.7(6) . . ? C37 C36 C1 121.4(6) . . ? C38 C37 C36 122.2(6) . . ? C38 C37 H37A 118.9 . . ? C36 C37 H37A 118.9 . . ? C39 C38 C37 117.3(6) . . ? C39 C38 C42 122.9(6) . . ? C37 C38 C42 119.7(6) . . ? C38 C39 C40 123.1(6) . . ? C38 C39 H39A 118.4 . . ? C40 C39 H39A 118.4 . . ? C41 C40 C39 116.7(6) . . ? C41 C40 C46 122.8(6) . . ? C39 C40 C46 120.5(6) . . ? C36 C41 C40 122.9(6) . . ? C36 C41 O5 117.9(6) . . ? C40 C41 O5 119.1(6) . . ? C43 C42 C45 109.0(6) . . ? C43 C42 C44 108.1(7) . . ? C45 C42 C44 107.2(6) . . ? C43 C42 C38 112.4(5) . . ? C45 C42 C38 111.5(6) . . ? C44 C42 C38 108.4(5) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C40 C46 H46A 109.5 . . ? C40 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C40 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O5 C47 C48 108.2(5) . . ? O5 C47 H47A 110.1 . . ? C48 C47 H47A 110.1 . . ? O5 C47 H47B 110.1 . . ? C48 C47 H47B 110.1 . . ? H47A C47 H47B 108.4 . . ? N14 C48 C47 110.3(5) . . ? N14 C48 H48A 109.6 . . ? C47 C48 H48A 109.6 . . ? N14 C48 H48B 109.6 . . ? C47 C48 H48B 109.6 . . ? H48A C48 H48B 108.1 . . ? O2 C49 N14 122.9(6) . . ? O2 C49 C50 117.0(5) . . ? N14 C49 C50 120.1(5) . . ? N2 C50 C51 122.1(6) . . ? N2 C50 C49 112.5(5) . . ? C51 C50 C49 125.3(5) . . ? C52 C51 C50 118.8(6) . . ? C52 C51 H51A 120.6 . . ? C50 C51 H51A 120.6 . . ? C51 C52 C53 120.1(6) . . ? C51 C52 H52A 120.0 . . ? C53 C52 H52A 120.0 . . ? C54 C53 C52 117.2(6) . . ? C54 C53 H53A 121.4 . . ? C52 C53 H53A 121.4 . . ? N2 C54 C53 124.0(5) . . ? N2 C54 C55 113.8(5) . . ? C53 C54 C55 122.1(6) . . ? N5 C55 N11 126.2(5) . . ? N5 C55 C54 116.8(5) . . ? N11 C55 C54 116.9(5) . . ? N11 C56 C57 117.5(5) . . ? N11 C56 C58 116.2(6) . . ? C57 C56 C58 126.3(5) . . ? N8 C57 C56 120.2(5) . . ? N8 C57 C64 113.6(6) . . ? C56 C57 C64 126.2(5) . . ? C59 C58 C63 119.9(6) . . ? C59 C58 C56 118.1(5) . . ? C63 C58 C56 122.0(6) . . ? C60 C59 C58 120.5(6) . . ? C60 C59 H59A 119.7 . . ? C58 C59 H59A 119.7 . . ? C61 C60 C59 119.4(7) . . ? C61 C60 H60A 120.3 . . ? C59 C60 H60A 120.3 . . ? C60 C61 C62 120.7(7) . . ? C60 C61 H61A 119.7 . . ? C62 C61 H61A 119.7 . . ? C63 C62 C61 119.9(6) . . ? C63 C62 H62A 120.0 . . ? C61 C62 H62A 120.0 . . ? C62 C63 C58 119.6(6) . . ? C62 C63 H63A 120.2 . . ? C58 C63 H63A 120.2 . . ? C69 C64 C65 119.9(6) . . ? C69 C64 C57 120.6(6) . . ? C65 C64 C57 119.3(6) . . ? C64 C65 C66 119.7(7) . . ? C64 C65 H65A 120.2 . . ? C66 C65 H65A 120.2 . . ? C67 C66 C65 119.9(8) . . ? C67 C66 H66A 120.0 . . ? C65 C66 H66A 120.0 . . ? C66 C67 C68 120.0(7) . . ? C66 C67 H67A 120.0 . . ? C68 C67 H67A 120.0 . . ? C69 C68 C67 120.9(7) . . ? C69 C68 H68A 119.6 . . ? C67 C68 H68A 119.6 . . ? C68 C69 C64 119.5(7) . . ? C68 C69 H69A 120.2 . . ? C64 C69 H69A 120.2 . . ? C71 C70 C75 117.3(7) . . ? C71 C70 C1 122.5(6) . . ? C75 C70 C1 120.0(6) . . ? C70 C71 C72 123.9(7) . . ? C70 C71 H71A 118.0 . . ? C72 C71 H71A 118.0 . . ? C73 C72 C71 116.4(7) . . ? C73 C72 C76 122.7(7) . . ? C71 C72 C76 120.9(7) . . ? C74 C73 C72 122.8(8) . . ? C74 C73 H73A 118.6 . . ? C72 C73 H73A 118.6 . . ? C73 C74 C75 117.5(7) . . ? C73 C74 C80 122.9(8) . . ? C75 C74 C80 119.6(8) . . ? O6 C75 C74 119.9(6) . . ? O6 C75 C70 118.1(7) . . ? C74 C75 C70 121.8(7) . . ? C79 C76 C72 113.5(8) . . ? C79 C76 C77 108.7(7) . . ? C72 C76 C77 110.1(7) . . ? C79 C76 C78 107.4(7) . . ? C72 C76 C78 107.7(6) . . ? C77 C76 C78 109.3(8) . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C76 C79 H79A 109.5 . . ? C76 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C76 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C74 C80 H80A 109.5 . . ? C74 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C74 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O6 C81 C82 109.4(5) . . ? O6 C81 H81A 109.8 . . ? C82 C81 H81A 109.8 . . ? O6 C81 H81B 109.8 . . ? C82 C81 H81B 109.8 . . ? H81A C81 H81B 108.3 . . ? N15 C82 C81 108.7(6) . . ? N15 C82 H82A 109.9 . . ? C81 C82 H82A 109.9 . . ? N15 C82 H82B 109.9 . . ? C81 C82 H82B 109.9 . . ? H82A C82 H82B 108.3 . . ? O3 C83 N15 121.8(5) . . ? O3 C83 C84 117.9(5) . . ? N15 C83 C84 120.3(6) . . ? N3 C84 C85 122.9(5) . . ? N3 C84 C83 112.8(5) . . ? C85 C84 C83 124.2(5) . . ? C84 C85 C86 117.7(6) . . ? C84 C85 H85A 121.2 . . ? C86 C85 H85A 121.2 . . ? C87 C86 C85 119.3(6) . . ? C87 C86 H86A 120.3 . . ? C85 C86 H86A 120.3 . . ? C86 C87 C88 118.2(5) . . ? C86 C87 H87A 120.9 . . ? C88 C87 H87A 120.9 . . ? N3 C88 C87 122.5(6) . . ? N3 C88 C89 117.5(5) . . ? C87 C88 C89 120.0(5) . . ? N6 C89 N12 123.5(6) . . ? N6 C89 C88 115.6(5) . . ? N12 C89 C88 120.8(5) . . ? N12 C90 C91 118.9(5) . . ? N12 C90 C92 116.9(5) . . ? C91 C90 C92 124.2(6) . . ? N9 C91 C90 120.3(6) . . ? N9 C91 C98 112.8(5) . . ? C90 C91 C98 127.0(5) . . ? C93 C92 C97 118.7(6) . . ? C93 C92 C90 119.4(6) . . ? C97 C92 C90 121.8(6) . . ? C92 C93 C94 120.6(8) . . ? C92 C93 H93A 119.7 . . ? C94 C93 H93A 119.7 . . ? C95 C94 C93 118.9(9) . . ? C95 C94 H94A 120.6 . . ? C93 C94 H94A 120.6 . . ? C96 C95 C94 121.1(8) . . ? C96 C95 H95A 119.4 . . ? C94 C95 H95A 119.4 . . ? C95 C96 C97 120.7(8) . . ? C95 C96 H96A 119.6 . . ? C97 C96 H96A 119.6 . . ? C92 C97 C96 120.0(7) . . ? C92 C97 H97A 120.0 . . ? C96 C97 H97A 120.0 . . ? C103 C98 C99 120.1(7) . . ? C103 C98 C91 120.3(7) . . ? C99 C98 C91 119.6(7) . . ? C100 C99 C98 119.2(8) . . ? C100 C99 H99A 120.4 . . ? C98 C99 H99A 120.4 . . ? C99 C100 C101 119.7(9) . . ? C99 C100 H10G 120.2 . . ? C101 C100 H10G 120.2 . . ? C102 C101 C100 120.6(8) . . ? C102 C101 H10H 119.7 . . ? C100 C101 H10H 119.7 . . ? C101 C102 C103 120.5(9) . . ? C101 C102 H10I 119.8 . . ? C103 C102 H10I 119.8 . . ? C98 C103 C102 120.0(8) . . ? C98 C103 H10J 120.0 . . ? C102 C103 H10J 120.0 . . ? O3A Er2 O1A 76.48(14) . . ? O3A Er2 O2A 78.50(14) . . ? O1A Er2 O2A 78.62(15) . . ? O3A Er2 N1A 72.48(15) . . ? O1A Er2 N1A 65.77(15) . . ? O2A Er2 N1A 138.09(15) . . ? O3A Er2 N2A 137.23(15) . . ? O1A Er2 N2A 74.62(15) . . ? O2A Er2 N2A 65.41(16) . . ? N1A Er2 N2A 121.05(17) . . ? O3A Er2 N3A 65.24(15) . . ? O1A Er2 N3A 136.45(15) . . ? O2A Er2 N3A 74.27(15) . . ? N1A Er2 N3A 117.52(16) . . ? N2A Er2 N3A 121.31(16) . . ? O3A Er2 N5A 146.13(16) . . ? O1A Er2 N5A 89.38(15) . . ? O2A Er2 N5A 129.21(15) . . ? N1A Er2 N5A 73.65(16) . . ? N2A Er2 N5A 63.81(16) . . ? N3A Er2 N5A 134.11(15) . . ? O3A Er2 N6A 128.74(15) . . ? O1A Er2 N6A 147.14(15) . . ? O2A Er2 N6A 86.01(15) . . ? N1A Er2 N6A 135.86(16) . . ? N2A Er2 N6A 72.58(16) . . ? N3A Er2 N6A 63.55(15) . . ? N5A Er2 N6A 78.08(16) . . ? O3A Er2 N4A 89.05(15) . . ? O1A Er2 N4A 129.58(16) . . ? O2A Er2 N4A 145.71(16) . . ? N1A Er2 N4A 63.81(16) . . ? N2A Er2 N4A 133.72(16) . . ? N3A Er2 N4A 71.51(16) . . ? N5A Er2 N4A 76.40(15) . . ? N6A Er2 N4A 77.11(16) . . ? C15A O1A Er2 122.4(4) . . ? C49A O2A Er2 122.8(4) . . ? C83A O3A Er2 124.9(4) . . ? C7A O4A C13A 115.8(4) . . ? C41A O5A C47A 110.9(6) . . ? C75A O6A C81A 111.9(5) . . ? C20A N1A C16A 116.7(5) . . ? C20A N1A Er2 124.2(4) . . ? C16A N1A Er2 119.1(4) . . ? C54A N2A C50A 120.3(5) . . ? C54A N2A Er2 122.6(4) . . ? C50A N2A Er2 116.8(4) . . ? C88A N3A C84A 118.5(5) . . ? C88A N3A Er2 122.7(4) . . ? C84A N3A Er2 118.3(4) . . ? N7A N4A C21A 116.5(5) . . ? N7A N4A Er2 121.4(4) . . ? C21A N4A Er2 121.7(4) . . ? N8A N5A C55A 118.0(5) . . ? N8A N5A Er2 121.3(3) . . ? C55A N5A Er2 120.6(4) . . ? C89A N6A N9A 118.2(5) . . ? C89A N6A Er2 121.8(4) . . ? N9A N6A Er2 120.0(4) . . ? N4A N7A C22A 120.0(5) . . ? C57A N8A N5A 120.2(5) . . ? C91A N9A N6A 118.9(5) . . ? C21A N10A C23A 116.5(5) . . ? C56A N11A C55A 117.5(5) . . ? C89A N12A C90A 116.5(5) . . ? C15A N13A C14A 121.8(6) . . ? C15A N13A H13F 119.1 . . ? C14A N13A H13F 119.1 . . ? C49A N14A C48A 122.4(6) . . ? C49A N14A H14F 118.8 . . ? C48A N14A H14F 118.8 . . ? C83A N15A C82A 121.7(5) . . ? C83A N15A H15B 119.1 . . ? C82A N15A H15B 119.1 . . ? C70A C1A C2A 113.0(5) . . ? C70A C1A C36A 112.2(6) . . ? C2A C1A C36A 110.9(6) . . ? C70A C1A H1AA 106.8 . . ? C2A C1A H1AA 106.8 . . ? C36A C1A H1AA 106.8 . . ? C7A C2A C3A 118.4(7) . . ? C7A C2A C1A 121.3(6) . . ? C3A C2A C1A 120.2(7) . . ? C4A C3A C2A 121.6(8) . . ? C4A C3A H3AA 119.2 . . ? C2A C3A H3AA 119.2 . . ? C5A C4A C3A 117.5(7) . . ? C5A C4A C8A 123.9(7) . . ? C3A C4A C8A 118.6(8) . . ? C4A C5A C6A 122.9(7) . . ? C4A C5A H5AA 118.5 . . ? C6A C5A H5AA 118.5 . . ? C5A C6A C7A 118.4(8) . . ? C5A C6A C12A 121.2(7) . . ? C7A C6A C12A 120.4(7) . . ? C2A C7A O4A 119.7(6) . . ? C2A C7A C6A 121.2(7) . . ? O4A C7A C6A 119.0(7) . . ? C11B C8A C10A 70.8(10) . . ? C11B C8A C9A 119.8(14) . . ? C10A C8A C9A 115.7(11) . . ? C11B C8A C4A 117.2(10) . . ? C10A C8A C4A 111.0(9) . . ? C9A C8A C4A 114.6(12) . . ? C11B C8A C9B 116.0(11) . . ? C10A C8A C9B 132.1(12) . . ? C9A C8A C9B 17.3(11) . . ? C4A C8A C9B 106.5(10) . . ? C11B C8A C10B 111.3(10) . . ? C10A C8A C10B 41.6(8) . . ? C9A C8A C10B 87.3(10) . . ? C4A C8A C10B 99.9(8) . . ? C9B C8A C10B 103.9(9) . . ? C11B C8A C11A 36.1(9) . . ? C10A C8A C11A 106.9(10) . . ? C9A C8A C11A 103.1(10) . . ? C4A C8A C11A 104.3(9) . . ? C9B C8A C11A 91.2(10) . . ? C10B C8A C11A 146.4(11) . . ? C8A C9A H9AA 109.5 . . ? C8A C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C8A C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C8A C10A H10K 109.5 . . ? C8A C10A H10L 109.5 . . ? H10K C10A H10L 109.5 . . ? C8A C10A H10M 109.5 . . ? H10K C10A H10M 109.5 . . ? H10L C10A H10M 109.5 . . ? C8A C11A H11G 109.5 . . ? C8A C11A H11H 109.5 . . ? H11G C11A H11H 109.5 . . ? C8A C11A H11I 109.5 . . ? H11G C11A H11I 109.5 . . ? H11H C11A H11I 109.5 . . ? C8A C9B H9BA 109.5 . . ? C8A C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? C8A C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? C8A C10B H10N 109.5 . . ? C8A C10B H10O 109.5 . . ? H10N C10B H10O 109.5 . . ? C8A C10B H10P 109.5 . . ? H10N C10B H10P 109.5 . . ? H10O C10B H10P 109.5 . . ? C8A C11B H11J 109.5 . . ? C8A C11B H11K 109.5 . . ? H11J C11B H11K 109.5 . . ? C8A C11B H11L 109.5 . . ? H11J C11B H11L 109.5 . . ? H11K C11B H11L 109.5 . . ? C6A C12A H12D 109.5 . . ? C6A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C6A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? O4A C13A C14A 107.7(5) . . ? O4A C13A H13C 110.2 . . ? C14A C13A H13C 110.2 . . ? O4A C13A H13D 110.2 . . ? C14A C13A H13D 110.2 . . ? H13C C13A H13D 108.5 . . ? N13A C14A C13A 110.4(5) . . ? N13A C14A H14C 109.6 . . ? C13A C14A H14C 109.6 . . ? N13A C14A H14D 109.6 . . ? C13A C14A H14D 109.6 . . ? H14C C14A H14D 108.1 . . ? O1A C15A N13A 122.1(6) . . ? O1A C15A C16A 118.6(5) . . ? N13A C15A C16A 119.3(6) . . ? N1A C16A C17A 123.4(6) . . ? N1A C16A C15A 111.2(5) . . ? C17A C16A C15A 125.4(6) . . ? C18A C17A C16A 118.3(6) . . ? C18A C17A H17B 120.8 . . ? C16A C17A H17B 120.8 . . ? C17A C18A C19A 120.1(7) . . ? C17A C18A H18B 119.9 . . ? C19A C18A H18B 119.9 . . ? C20A C19A C18A 117.3(6) . . ? C20A C19A H19B 121.4 . . ? C18A C19A H19B 121.4 . . ? N1A C20A C19A 124.1(6) . . ? N1A C20A C21A 115.5(5) . . ? C19A C20A C21A 120.3(5) . . ? N10A C21A N4A 126.5(5) . . ? N10A C21A C20A 118.8(5) . . ? N4A C21A C20A 114.6(5) . . ? N7A C22A C23A 119.4(5) . . ? N7A C22A C30A 113.7(5) . . ? C23A C22A C30A 126.7(5) . . ? N10A C23A C22A 119.6(5) . . ? N10A C23A C24A 115.3(5) . . ? C22A C23A C24A 125.1(5) . . ? C25A C24A C29A 120.1(6) . . ? C25A C24A C23A 119.0(6) . . ? C29A C24A C23A 120.9(6) . . ? C26A C25A C24A 119.0(6) . . ? C26A C25A H25B 120.5 . . ? C24A C25A H25B 120.5 . . ? C27A C26A C25A 120.7(6) . . ? C27A C26A H26B 119.6 . . ? C25A C26A H26B 119.6 . . ? C28A C27A C26A 120.4(6) . . ? C28A C27A H27B 119.8 . . ? C26A C27A H27B 119.8 . . ? C27A C28A C29A 119.8(6) . . ? C27A C28A H28B 120.1 . . ? C29A C28A H28B 120.1 . . ? C24A C29A C28A 119.9(6) . . ? C24A C29A H29B 120.0 . . ? C28A C29A H29B 120.0 . . ? C31A C30A C35A 118.9(6) . . ? C31A C30A C22A 119.9(6) . . ? C35A C30A C22A 121.2(5) . . ? C30A C31A C32A 120.4(6) . . ? C30A C31A H31B 119.8 . . ? C32A C31A H31B 119.8 . . ? C33A C32A C31A 120.4(7) . . ? C33A C32A H32B 119.8 . . ? C31A C32A H32B 119.8 . . ? C32A C33A C34A 120.3(7) . . ? C32A C33A H33B 119.8 . . ? C34A C33A H33B 119.8 . . ? C33A C34A C35A 120.2(7) . . ? C33A C34A H34B 119.9 . . ? C35A C34A H34B 119.9 . . ? C34A C35A C30A 119.9(6) . . ? C34A C35A H35B 120.1 . . ? C30A C35A H35B 120.1 . . ? C37A C36A C41A 118.7(6) . . ? C37A C36A C1A 123.0(6) . . ? C41A C36A C1A 118.1(7) . . ? C36A C37A C38A 122.7(6) . . ? C36A C37A H37B 118.6 . . ? C38A C37A H37B 118.6 . . ? C37A C38A C39A 116.6(7) . . ? C37A C38A C42A 122.7(6) . . ? C39A C38A C42A 120.4(6) . . ? C40A C39A C38A 123.2(7) . . ? C40A C39A H39B 118.4 . . ? C38A C39A H39B 118.4 . . ? C39A C40A C41A 117.6(7) . . ? C39A C40A C46B 117.9(9) . . ? C41A C40A C46B 123.5(9) . . ? C39A C40A C46A 127.7(8) . . ? C41A C40A C46A 111.2(9) . . ? C46B C40A C46A 30.0(7) . . ? O5A C41A C36A 119.6(7) . . ? O5A C41A C40A 119.8(7) . . ? C36A C41A C40A 120.5(8) . . ? C43A C42A C38A 111.8(6) . . ? C43A C42A C45A 108.8(7) . . ? C38A C42A C45A 110.4(6) . . ? C43A C42A C44A 110.5(7) . . ? C38A C42A C44A 107.0(6) . . ? C45A C42A C44A 108.3(6) . . ? C42A C43A H43D 109.5 . . ? C42A C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C42A C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? C42A C44A H44D 109.5 . . ? C42A C44A H44E 109.5 . . ? H44D C44A H44E 109.5 . . ? C42A C44A H44F 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? C42A C45A H45D 109.5 . . ? C42A C45A H45E 109.5 . . ? H45D C45A H45E 109.5 . . ? C42A C45A H45F 109.5 . . ? H45D C45A H45F 109.5 . . ? H45E C45A H45F 109.5 . . ? C40A C46A H46D 109.5 . . ? C40A C46A H46E 109.5 . . ? H46D C46A H46E 109.5 . . ? C40A C46A H46F 109.5 . . ? H46D C46A H46F 109.5 . . ? H46E C46A H46F 109.5 . . ? C40A C46B H46G 109.5 . . ? C40A C46B H46H 109.5 . . ? H46G C46B H46H 109.5 . . ? C40A C46B H46I 109.5 . . ? H46G C46B H46I 109.5 . . ? H46H C46B H46I 109.5 . . ? O5A C47A C48A 110.7(7) . . ? O5A C47A H47C 109.5 . . ? C48A C47A H47C 109.5 . . ? O5A C47A H47D 109.5 . . ? C48A C47A H47D 109.5 . . ? H47C C47A H47D 108.1 . . ? N14A C48A C47A 108.8(7) . . ? N14A C48A H48C 109.9 . . ? C47A C48A H48C 109.9 . . ? N14A C48A H48D 109.9 . . ? C47A C48A H48D 109.9 . . ? H48C C48A H48D 108.3 . . ? O2A C49A N14A 121.3(6) . . ? O2A C49A C50A 120.1(6) . . ? N14A C49A C50A 118.5(5) . . ? N2A C50A C51A 119.9(6) . . ? N2A C50A C49A 112.6(5) . . ? C51A C50A C49A 127.3(6) . . ? C52A C51A C50A 119.1(6) . . ? C52A C51A H51B 120.4 . . ? C50A C51A H51B 120.4 . . ? C53A C52A C51A 120.5(6) . . ? C53A C52A H52B 119.7 . . ? C51A C52A H52B 119.7 . . ? C52A C53A C54A 117.9(7) . . ? C52A C53A H53B 121.0 . . ? C54A C53A H53B 121.0 . . ? N2A C54A C53A 122.2(6) . . ? N2A C54A C55A 115.4(5) . . ? C53A C54A C55A 122.4(6) . . ? N11A C55A N5A 124.3(6) . . ? N11A C55A C54A 118.3(5) . . ? N5A C55A C54A 117.4(5) . . ? N11A C56A C57A 119.8(6) . . ? N11A C56A C58A 114.0(6) . . ? C57A C56A C58A 126.2(6) . . ? N8A C57A C56A 119.9(6) . . ? N8A C57A C64A 112.7(5) . . ? C56A C57A C64A 127.3(6) . . ? C63A C58A C59A 118.5(7) . . ? C63A C58A C56A 124.5(7) . . ? C59A C58A C56A 117.0(6) . . ? C60A C59A C58A 118.4(8) . . ? C60A C59A H59B 120.8 . . ? C58A C59A H59B 120.8 . . ? C61A C60A C59A 121.9(8) . . ? C61A C60A H60B 119.1 . . ? C59A C60A H60B 119.1 . . ? C62A C61A C60A 119.5(8) . . ? C62A C61A H61B 120.2 . . ? C60A C61A H61B 120.2 . . ? C61A C62A C63A 120.0(8) . . ? C61A C62A H62B 120.0 . . ? C63A C62A H62B 120.0 . . ? C58A C63A C62A 121.8(8) . . ? C58A C63A H63B 119.1 . . ? C62A C63A H63B 119.1 . . ? C65A C64A C69A 118.6(7) . . ? C65A C64A C57A 122.2(7) . . ? C69A C64A C57A 119.1(6) . . ? C66A C65A C64A 119.5(8) . . ? C66A C65A H65B 120.2 . . ? C64A C65A H65B 120.2 . . ? C65A C66A C67A 119.5(9) . . ? C65A C66A H66B 120.3 . . ? C67A C66A H66B 120.3 . . ? C68A C67A C66A 121.0(9) . . ? C68A C67A H67B 119.5 . . ? C66A C67A H67B 119.5 . . ? C67A C68A C69A 119.6(9) . . ? C67A C68A H68B 120.2 . . ? C69A C68A H68B 120.2 . . ? C68A C69A C64A 121.7(8) . . ? C68A C69A H69B 119.1 . . ? C64A C69A H69B 119.1 . . ? C71A C70A C75A 117.8(8) . . ? C71A C70A C1A 121.9(7) . . ? C75A C70A C1A 120.4(7) . . ? C70A C71A C72A 123.0(7) . . ? C70A C71A H71B 118.5 . . ? C72A C71A H71B 118.5 . . ? C73A C72A C71A 116.6(7) . . ? C73A C72A C76A 123.6(8) . . ? C71A C72A C76A 119.8(7) . . ? C72A C73A C74A 122.8(8) . . ? C72A C73A H73B 118.6 . . ? C74A C73A H73B 118.6 . . ? C75A C74A C73A 117.9(7) . . ? C75A C74A C80A 120.8(7) . . ? C73A C74A C80A 121.3(8) . . ? O6A C75A C74A 118.7(7) . . ? O6A C75A C70A 119.4(7) . . ? C74A C75A C70A 121.6(7) . . ? C77B C76A C78A 125.3(17) . . ? C77B C76A C72A 111.1(8) . . ? C78A C76A C72A 114.0(17) . . ? C77B C76A C79B 112.4(9) . . ? C78A C76A C79B 82.1(14) . . ? C72A C76A C79B 106.9(8) . . ? C77B C76A C77A 22.5(15) . . ? C78A C76A C77A 111.3(15) . . ? C72A C76A C77A 108(2) . . ? C79B C76A C77A 131.9(19) . . ? C77B C76A C78B 109.2(8) . . ? C78A C76A C78B 27.9(13) . . ? C72A C76A C78B 107.1(8) . . ? C79B C76A C78B 109.8(8) . . ? C77A C76A C78B 89.7(15) . . ? C77B C76A C79A 86.8(15) . . ? C78A C76A C79A 110.3(15) . . ? C72A C76A C79A 103.7(18) . . ? C79B C76A C79A 30.2(13) . . ? C77A C76A C79A 108.9(15) . . ? C78B C76A C79A 136.5(16) . . ? C76A C79A H79D 109.5 . . ? C76A C79A H79E 109.5 . . ? H79D C79A H79E 109.5 . . ? C76A C79A H79F 109.5 . . ? H79D C79A H79F 109.5 . . ? H79E C79A H79F 109.5 . . ? C76A C77A H77D 109.5 . . ? C76A C77A H77E 109.5 . . ? H77D C77A H77E 109.5 . . ? C76A C77A H77F 109.5 . . ? H77D C77A H77F 109.5 . . ? H77E C77A H77F 109.5 . . ? C76A C78A H78D 109.5 . . ? C76A C78A H78E 109.5 . . ? H78D C78A H78E 109.5 . . ? C76A C78A H78F 109.5 . . ? H78D C78A H78F 109.5 . . ? H78E C78A H78F 109.5 . . ? C76A C79B H79G 109.5 . . ? C76A C79B H79H 109.5 . . ? H79G C79B H79H 109.5 . . ? C76A C79B H79I 109.5 . . ? H79G C79B H79I 109.5 . . ? H79H C79B H79I 109.5 . . ? C76A C77B H77G 109.5 . . ? C76A C77B H77H 109.5 . . ? H77G C77B H77H 109.5 . . ? C76A C77B H77I 109.5 . . ? H77G C77B H77I 109.5 . . ? H77H C77B H77I 109.5 . . ? C76A C78B H78G 109.5 . . ? C76A C78B H78H 109.5 . . ? H78G C78B H78H 109.5 . . ? C76A C78B H78I 109.5 . . ? H78G C78B H78I 109.5 . . ? H78H C78B H78I 109.5 . . ? C74A C80A H80D 109.5 . . ? C74A C80A H80E 109.5 . . ? H80D C80A H80E 109.5 . . ? C74A C80A H80F 109.5 . . ? H80D C80A H80F 109.5 . . ? H80E C80A H80F 109.5 . . ? O6A C81A C82A 106.9(5) . . ? O6A C81A H81C 110.3 . . ? C82A C81A H81C 110.3 . . ? O6A C81A H81D 110.3 . . ? C82A C81A H81D 110.3 . . ? H81C C81A H81D 108.6 . . ? N15A C82A C81A 110.8(6) . . ? N15A C82A H82C 109.5 . . ? C81A C82A H82C 109.5 . . ? N15A C82A H82D 109.5 . . ? C81A C82A H82D 109.5 . . ? H82C C82A H82D 108.1 . . ? O3A C83A N15A 122.6(6) . . ? O3A C83A C84A 119.5(5) . . ? N15A C83A C84A 117.9(6) . . ? N3A C84A C85A 121.3(6) . . ? N3A C84A C83A 111.3(5) . . ? C85A C84A C83A 127.4(5) . . ? C86A C85A C84A 119.5(6) . . ? C86A C85A H85B 120.2 . . ? C84A C85A H85B 120.2 . . ? C85A C86A C87A 120.4(6) . . ? C85A C86A H86B 119.8 . . ? C87A C86A H86B 119.8 . . ? C88A C87A C86A 117.0(6) . . ? C88A C87A H87B 121.5 . . ? C86A C87A H87B 121.5 . . ? N3A C88A C87A 123.2(5) . . ? N3A C88A C89A 115.7(5) . . ? C87A C88A C89A 121.0(6) . . ? N12A C89A N6A 126.1(5) . . ? N12A C89A C88A 117.9(5) . . ? N6A C89A C88A 116.0(5) . . ? N12A C90A C91A 118.8(6) . . ? N12A C90A C92A 116.7(6) . . ? C91A C90A C92A 124.5(5) . . ? N9A C91A C90A 121.4(5) . . ? N9A C91A C98A 113.0(5) . . ? C90A C91A C98A 125.6(6) . . ? C97A C92A C93A 119.9(6) . . ? C97A C92A C90A 120.5(6) . . ? C93A C92A C90A 119.6(6) . . ? C94A C93A C92A 119.8(7) . . ? C94A C93A H93B 120.1 . . ? C92A C93A H93B 120.1 . . ? C95A C94A C93A 120.7(8) . . ? C95A C94A H94B 119.7 . . ? C93A C94A H94B 119.7 . . ? C94A C95A C96A 119.5(7) . . ? C94A C95A H95B 120.3 . . ? C96A C95A H95B 120.3 . . ? C95A C96A C97A 120.2(7) . . ? C95A C96A H96B 119.9 . . ? C97A C96A H96B 119.9 . . ? C92A C97A C96A 119.8(7) . . ? C92A C97A H97B 120.1 . . ? C96A C97A H97B 120.1 . . ? C107 C98A C99A 120.0(6) . . ? C107 C98A C91A 118.6(6) . . ? C99A C98A C91A 121.2(6) . . ? C104 C99A C98A 119.4(7) . . ? C104 C99A H99B 120.3 . . ? C98A C99A H99B 120.3 . . ? C105 C104 C99A 119.9(8) . . ? C105 C104 H10Q 120.1 . . ? C99A C104 H10Q 120.1 . . ? C106 C105 C104 121.7(7) . . ? C106 C105 H10R 119.2 . . ? C104 C105 H10R 119.2 . . ? C105 C106 C107 119.9(8) . . ? C105 C106 H10S 120.1 . . ? C107 C106 H10S 120.1 . . ? C98A C107 C106 119.1(7) . . ? C98A C107 H10T 120.4 . . ? C106 C107 H10T 120.4 . . ? O8 N16 O9 121.4(12) . . ? O8 N16 O7 126.2(12) . . ? O9 N16 O7 111.2(10) . . ? O9 N16' O8' 151(2) . . ? O9 N16' O7' 106.9(18) . . ? O8' N16' O7' 95.9(18) . . ? N16' O9 N16 28.2(12) . . ? O11 N17 O12 118.5(8) . . ? O11 N17 O10 122.1(7) . . ? O12 N17 O10 119.4(8) . . ? O15 N18 O14 118.2(6) . . ? O15 N18 O13 120.4(6) . . ? O14 N18 O13 121.2(5) . . ? O18 N19 O17 129.3(14) . . ? O18 N19 O16 117.7(14) . . ? O17 N19 O16 112.4(11) . . ? O21" N20 O21' 43.7(9) . . ? O21" N20 O20 136.6(10) . . ? O21' N20 O20 128.0(9) . . ? O21" N20 O19 114.5(10) . . ? O21' N20 O19 88.5(8) . . ? O20 N20 O19 106.6(7) . . ? O21" N20 O21 64.1(11) . . ? O21' N20 O21 106.2(10) . . ? O20 N20 O21 112.6(8) . . ? O19 N20 O21 112.2(8) . . ? O22 N21 O23 119.9(18) . . ? O22 N21 O24 119.8(17) . . ? O23 N21 O24 115.0(16) . . ? O23' N21' O22' 123(3) . . ? O23' N21' O24' 122(3) . . ? O22' N21' O24' 115(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.929 _refine_diff_density_min -1.785 _refine_diff_density_rms 0.106 data_yb9 _database_code_depnum_ccdc_archive 'CCDC 889303' #TrackingRef 'web_deposit_cif_file_0_GaryGuillet_1349827139.gg4.cif' # # xray code for Yb9 is gg4 # _vrf_CHEMW03_I ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: the solvent area, which included three ether and six methanol molecules, were removed using Platon/Squeeze. ; _vrf_THETM01_I ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Small crystal did not diffract to higher resolution ; _vrf_PLAT023_I ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 18.76 Deg. RESPONSE: Small crystal did not diffract to higher resolution ; _vrf_PLAT043_I ; PROBLEM: Check Reported Molecular Weight ................ 2739.65 RESPONSE: Solvents removed by SQUEEZE, see above ; _vrf_PLAT044_I ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: Density calculated using full crystal contents but not solvents ; _vrf_PLAT201_I ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 11 RESPONSE: those are partial disordered atoms ; _vrf_PLAT241_I ; PROBLEM: Check High Ueq as Compared to Neighbors for O723 RESPONSE: disordered atoms could not be modeled by resolving disorders ; _vrf_PLAT602_I ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure RESPONSE: The solvents contributions were reomved by Platon/Squeeze ; _audit_update_record ; 2012-09-24 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C103 H97 N15 O6 Yb1, (C2H6N4O14Yb1), 2(NO3), 3(C4H10O1), 3(CH4O1)' _chemical_formula_sum 'C120 H145 N21 O32 Yb2' _chemical_formula_weight 2739.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.6026(14) _cell_length_b 17.8227(15) _cell_length_c 20.5821(17) _cell_angle_alpha 81.5270(10) _cell_angle_beta 81.6540(10) _cell_angle_gamma 88.4920(10) _cell_volume 6318.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9864 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description blocks _exptl_crystal_colour clear _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 1.555 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18759 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 18.76 _reflns_number_total 9683 _reflns_number_gt 8278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT (Bruker, 2008)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The following restraints were employed in the final refinement model. Yb9 dfix 2.30 yb2 o731 dfix 1.54 c8 c9 c8 c10 c8 c11 dfix 1.54 c8 c9' c8 c10' c8 c11' dfix 1.54 c8 c9" c8 c10" c8 c11" dfix 1.54 c76 c77' c76 c78' c76 c79' dfix 2.54 c9 c10 c9 c11 c10 c11 dfix 2.54 c9' c10' c9 c11' c10' c11' dfix 2.54 c9" c10" c9" c11" c10" c11" dfix 2.54 c77' c78' c77' c79' c78' c79' eadp c9' c10' c11' eadp c9 c10 c11 eadp c9" c10" c11" eadp c16 c17 c18 c19 c20 ; _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^)+(0.0921P)^2^+19.5697P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9683 _refine_ls_number_parameters 1355 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.26933(2) 0.75322(2) 0.506791(19) 0.0259(2) Uani 1 1 d . . . O1 O 0.3141(3) 0.6692(4) 0.5881(3) 0.0306(15) Uani 1 1 d . . . O2 O 0.1722(3) 0.7543(4) 0.5956(3) 0.0327(15) Uani 1 1 d . . . O3 O 0.3167(4) 0.8345(3) 0.5670(3) 0.0246(14) Uani 1 1 d . . . O4 O 0.2345(4) 0.6428(3) 0.7772(3) 0.0420(17) Uani 1 1 d . . . O5 O 0.1613(4) 0.8551(4) 0.7634(4) 0.055(2) Uani 1 1 d . . . O6 O 0.3880(3) 0.7990(3) 0.7387(3) 0.0354(16) Uani 1 1 d . . . N1 N 0.2059(4) 0.6278(4) 0.5274(4) 0.0270(18) Uani 1 1 d . . . N2 N 0.1891(4) 0.8688(4) 0.4993(4) 0.0273(19) Uani 1 1 d . . . N3 N 0.4109(4) 0.7647(4) 0.4855(4) 0.0260(18) Uani 1 1 d . . . N4 N 0.1683(4) 0.7359(5) 0.4350(4) 0.0289(19) Uani 1 1 d . . . N5 N 0.3040(5) 0.8487(4) 0.4031(4) 0.0299(19) Uani 1 1 d . . . N6 N 0.3375(5) 0.6779(4) 0.4218(4) 0.0307(19) Uani 1 1 d . . . N7 N 0.1608(4) 0.7885(4) 0.3827(4) 0.0310(19) Uani 1 1 d . . . N8 N 0.3577(5) 0.8349(4) 0.3525(5) 0.036(2) Uani 1 1 d . . . N9 N 0.2966(4) 0.6448(4) 0.3836(4) 0.0293(19) Uani 1 1 d . . . N10 N 0.0804(4) 0.6552(4) 0.4029(4) 0.0311(19) Uani 1 1 d . . . N11 N 0.2774(5) 0.9691(4) 0.3435(5) 0.036(2) Uani 1 1 d . . . N12 N 0.4540(4) 0.6515(4) 0.3535(4) 0.0329(19) Uani 1 1 d . . . N13 N 0.2995(4) 0.5685(4) 0.6686(4) 0.0334(19) Uani 1 1 d . . . H13C H 0.2816 0.5221 0.6804 0.040 Uiso 1 1 calc R . . N14 N 0.0877(4) 0.8181(4) 0.6613(5) 0.041(2) Uani 1 1 d . . . H14C H 0.0562 0.8572 0.6615 0.049 Uiso 1 1 calc R . . N15 N 0.4121(4) 0.8835(4) 0.6109(4) 0.0279(19) Uani 1 1 d . . . H15A H 0.4615 0.8940 0.6049 0.033 Uiso 1 1 calc R . . C1 C 0.2609(5) 0.7685(5) 0.8386(5) 0.034(2) Uani 1 1 d . . . H1A H 0.2620 0.7693 0.7898 0.040 Uiso 1 1 calc R . . C2 C 0.2028(5) 0.7076(5) 0.8715(5) 0.037(3) Uani 1 1 d . . . C3 C 0.1569(6) 0.7135(6) 0.9318(5) 0.038(3) Uani 1 1 d . . . H3A H 0.1658 0.7541 0.9549 0.046 Uiso 1 1 calc R . . C4 C 0.0991(6) 0.6628(6) 0.9591(5) 0.046(3) Uani 1 1 d . A . C5 C 0.0869(6) 0.6054(6) 0.9218(6) 0.059(3) Uani 1 1 d . . . H5A H 0.0464 0.5705 0.9385 0.071 Uiso 1 1 calc R . . C6 C 0.1307(7) 0.5974(6) 0.8623(6) 0.052(3) Uani 1 1 d . . . C7 C 0.1904(6) 0.6473(6) 0.8383(5) 0.035(2) Uani 1 1 d . . . C8 C 0.0505(5) 0.6656(6) 1.0260(5) 0.066(4) Uani 1 1 d D . . C9 C -0.0347(8) 0.6606(14) 1.0237(11) 0.079(4) Uiso 0.60 1 d PD A 1 H9A H -0.0654 0.6613 1.0673 0.118 Uiso 0.60 1 d PR A 1 H9B H -0.0499 0.6173 1.0042 0.118 Uiso 0.60 1 d PR A 1 H9C H -0.0432 0.7078 0.9946 0.118 Uiso 0.60 1 d PR A 1 C10 C 0.0706(12) 0.5831(9) 1.0694(10) 0.079(4) Uiso 0.60 1 d PD A 1 H10A H 0.0421 0.5780 1.1144 0.118 Uiso 0.60 1 d PR A 1 H10B H 0.1257 0.5772 1.0718 0.118 Uiso 0.60 1 d PR A 1 H10C H 0.0539 0.5438 1.0459 0.118 Uiso 0.60 1 d PR A 1 C11 C 0.0765(11) 0.7239(10) 1.0617(11) 0.079(4) Uiso 0.60 1 d PD A 1 H11A H 0.0436 0.7217 1.1047 0.118 Uiso 0.60 1 d PR A 1 H11B H 0.0711 0.7737 1.0354 0.118 Uiso 0.60 1 d PR A 1 H11C H 0.1301 0.7158 1.0688 0.118 Uiso 0.60 1 d PR A 1 C9' C -0.017(4) 0.721(4) 1.014(4) 0.033(15) Uiso 0.10 1 d PD A 2 H9'A H -0.0453 0.7214 1.0582 0.050 Uiso 0.10 1 d PR A 2 H9'B H -0.0241 0.6712 0.9996 0.050 Uiso 0.10 1 d PR A 2 H9'C H -0.0365 0.7608 0.9824 0.050 Uiso 0.10 1 d PR A 2 C10' C 0.021(5) 0.587(2) 1.062(4) 0.033(15) Uiso 0.10 1 d PD A 2 H10D H -0.0018 0.5764 1.1083 0.050 Uiso 0.10 1 d PR A 2 H10E H 0.0761 0.5950 1.0583 0.050 Uiso 0.10 1 d PR A 2 H10F H 0.0112 0.5448 1.0387 0.050 Uiso 0.10 1 d PR A 2 C11' C 0.074(3) 0.714(4) 1.075(3) 0.033(15) Uiso 0.10 1 d PD A 2 H11D H 0.0436 0.7190 1.1176 0.050 Uiso 0.10 1 d PR A 2 H11E H 0.0668 0.7589 1.0426 0.050 Uiso 0.10 1 d PR A 2 H11F H 0.1282 0.7077 1.0796 0.050 Uiso 0.10 1 d PR A 2 C9" C 0.017(2) 0.7533(12) 1.0196(17) 0.056(6) Uiso 0.30 1 d PD A 3 H9"A H -0.0161 0.7652 1.0592 0.084 Uiso 0.30 1 d PR A 3 H9"B H -0.0128 0.7554 0.9828 0.084 Uiso 0.30 1 d PR A 3 H9"C H 0.0590 0.7903 1.0075 0.084 Uiso 0.30 1 d PR A 3 C11" C 0.1017(15) 0.6625(19) 1.0801(14) 0.056(6) Uiso 0.30 1 d PD A 3 H11G H 0.0701 0.6632 1.1233 0.084 Uiso 0.30 1 d PR A 3 H11H H 0.1358 0.7066 1.0703 0.084 Uiso 0.30 1 d PR A 3 H11I H 0.1326 0.6159 1.0813 0.084 Uiso 0.30 1 d PR A 3 C10" C -0.0200(16) 0.6159(18) 1.0458(17) 0.056(6) Uiso 0.30 1 d PD A 3 H10G H -0.0466 0.6215 1.0901 0.084 Uiso 0.30 1 d PR A 3 H10H H 0.0020 0.5647 1.0464 0.084 Uiso 0.30 1 d PR A 3 H10I H -0.0566 0.6239 1.0138 0.084 Uiso 0.30 1 d PR A 3 C12 C 0.1135(7) 0.5362(7) 0.8224(6) 0.075(4) Uani 1 1 d . . . H12A H 0.0699 0.5059 0.8465 0.112 Uiso 1 1 calc R . . H12B H 0.1587 0.5033 0.8159 0.112 Uiso 1 1 calc R . . H12C H 0.1010 0.5599 0.7792 0.112 Uiso 1 1 calc R . . C13 C 0.3015(6) 0.5952(5) 0.7810(5) 0.039(3) Uani 1 1 d . . . H13A H 0.2860 0.5423 0.7989 0.047 Uiso 1 1 calc R . . H13B H 0.3340 0.6131 0.8109 0.047 Uiso 1 1 calc R . . C14 C 0.3453(6) 0.5980(5) 0.7133(4) 0.037(3) Uani 1 1 d . . . H14A H 0.3600 0.6511 0.6954 0.044 Uiso 1 1 calc R . . H14B H 0.3929 0.5676 0.7156 0.044 Uiso 1 1 calc R . . C15 C 0.2833(5) 0.6057(6) 0.6129(5) 0.028(2) Uani 1 1 d . . . C16 C 0.2260(5) 0.5764(5) 0.5772(5) 0.0357(11) Uani 1 1 d . . . C17 C 0.1940(5) 0.5030(5) 0.5910(5) 0.0357(11) Uani 1 1 d . . . H17A H 0.2091 0.4668 0.6254 0.043 Uiso 1 1 calc R . . C18 C 0.1408(5) 0.4853(5) 0.5535(4) 0.0357(11) Uani 1 1 d . . . H18A H 0.1197 0.4357 0.5614 0.043 Uiso 1 1 calc R . . C19 C 0.1173(5) 0.5380(5) 0.5048(4) 0.0357(11) Uani 1 1 d . . . H19A H 0.0787 0.5267 0.4799 0.043 Uiso 1 1 calc R . . C20 C 0.1525(5) 0.6094(5) 0.4932(5) 0.0357(11) Uani 1 1 d . . . C21 C 0.1323(5) 0.6700(5) 0.4410(4) 0.027(2) Uani 1 1 d . . . C22 C 0.0678(5) 0.7064(6) 0.3526(5) 0.031(2) Uani 1 1 d . . . C23 C 0.1152(5) 0.7741(5) 0.3393(5) 0.027(2) Uani 1 1 d . . . C24 C 0.0069(5) 0.6955(6) 0.3136(5) 0.031(2) Uani 1 1 d . . . C25 C -0.0098(6) 0.6214(6) 0.3086(5) 0.042(3) Uani 1 1 d . . . H25A H 0.0173 0.5809 0.3306 0.051 Uiso 1 1 calc R . . C26 C -0.0658(7) 0.6060(7) 0.2714(5) 0.053(3) Uani 1 1 d . . . H26A H -0.0763 0.5549 0.2679 0.064 Uiso 1 1 calc R . . C27 C -0.1059(7) 0.6629(8) 0.2402(6) 0.066(4) Uani 1 1 d . . . H27A H -0.1430 0.6521 0.2136 0.079 Uiso 1 1 calc R . . C28 C -0.0921(7) 0.7368(8) 0.2476(6) 0.069(4) Uani 1 1 d . . . H28A H -0.1206 0.7772 0.2271 0.083 Uiso 1 1 calc R . . C29 C -0.0355(6) 0.7521(6) 0.2857(5) 0.051(3) Uani 1 1 d . . . H29A H -0.0272 0.8029 0.2919 0.061 Uiso 1 1 calc R . . C30 C 0.1190(5) 0.8320(6) 0.2785(5) 0.031(2) Uani 1 1 d . . . C31 C 0.1327(6) 0.8092(6) 0.2159(6) 0.048(3) Uani 1 1 d . . . H31A H 0.1400 0.7569 0.2121 0.057 Uiso 1 1 calc R . . C32 C 0.1355(7) 0.8617(7) 0.1600(5) 0.058(3) Uani 1 1 d . . . H32A H 0.1464 0.8464 0.1173 0.070 Uiso 1 1 calc R . . C33 C 0.1225(7) 0.9368(6) 0.1663(6) 0.059(3) Uani 1 1 d . . . H33A H 0.1222 0.9732 0.1277 0.071 Uiso 1 1 calc R . . C34 C 0.1098(5) 0.9599(6) 0.2278(5) 0.041(3) Uani 1 1 d . . . H34A H 0.1020 1.0122 0.2314 0.049 Uiso 1 1 calc R . . C35 C 0.1086(5) 0.9089(6) 0.2827(5) 0.030(2) Uani 1 1 d . . . H35A H 0.1005 0.9254 0.3250 0.036 Uiso 1 1 calc R . . C36 C 0.2363(5) 0.8478(6) 0.8516(5) 0.036(3) Uani 1 1 d . . . C37 C 0.2664(6) 0.8835(6) 0.8969(5) 0.041(3) Uani 1 1 d . . . H37A H 0.3016 0.8561 0.9225 0.049 Uiso 1 1 calc R . . C38 C 0.2480(6) 0.9577(6) 0.9070(6) 0.050(3) Uani 1 1 d . B . C39 C 0.1969(7) 0.9950(7) 0.8677(7) 0.072(4) Uani 1 1 d . . . H39A H 0.1829 1.0456 0.8735 0.086 Uiso 1 1 calc R . . C40 C 0.1643(7) 0.9625(8) 0.8194(7) 0.073(4) Uani 1 1 d . . . C41 C 0.1864(6) 0.8874(7) 0.8138(6) 0.049(3) Uani 1 1 d . . . C42 C 0.2855(6) 0.9965(6) 0.9545(6) 0.060(3) Uani 1 1 d . . . C43 C 0.2681(14) 1.0832(13) 0.9475(12) 0.063(7) Uiso 0.50 1 d P B 1 H43A H 0.3017 1.1095 0.9092 0.095 Uiso 0.50 1 calc PR B 1 H43B H 0.2772 1.1025 0.9878 0.095 Uiso 0.50 1 calc PR B 1 H43C H 0.2143 1.0921 0.9410 0.095 Uiso 0.50 1 calc PR B 1 C44 C 0.3770(10) 0.9933(12) 0.9350(9) 0.037(5) Uiso 0.50 1 d P B 1 H44A H 0.3916 0.9455 0.9181 0.055 Uiso 0.50 1 calc PR B 1 H44B H 0.4015 0.9962 0.9744 0.055 Uiso 0.50 1 calc PR B 1 H44C H 0.3937 1.0360 0.9007 0.055 Uiso 0.50 1 calc PR B 1 C45 C 0.2575(15) 0.9564(14) 1.0206(11) 0.060(7) Uiso 0.50 1 d P B 1 H45A H 0.2787 0.9048 1.0251 0.090 Uiso 0.50 1 calc PR B 1 H45B H 0.2013 0.9540 1.0266 0.090 Uiso 0.50 1 calc PR B 1 H45C H 0.2737 0.9835 1.0544 0.090 Uiso 0.50 1 calc PR B 1 C43' C 0.230(2) 1.059(2) 0.9862(18) 0.131(12) Uiso 0.50 1 d P B 2 H43D H 0.2185 1.0984 0.9510 0.196 Uiso 0.50 1 calc PR B 2 H43E H 0.2564 1.0810 1.0178 0.196 Uiso 0.50 1 calc PR B 2 H43F H 0.1828 1.0343 1.0094 0.196 Uiso 0.50 1 calc PR B 2 C44' C 0.351(2) 1.034(2) 0.9194(16) 0.114(11) Uiso 0.50 1 d P B 2 H44D H 0.3861 0.9970 0.8995 0.170 Uiso 0.50 1 calc PR B 2 H44E H 0.3771 1.0581 0.9498 0.170 Uiso 0.50 1 calc PR B 2 H44F H 0.3365 1.0724 0.8843 0.170 Uiso 0.50 1 calc PR B 2 C45' C 0.3021(17) 0.9420(16) 1.0219(13) 0.082(9) Uiso 0.50 1 d P B 2 H45D H 0.3342 0.8989 1.0100 0.124 Uiso 0.50 1 calc PR B 2 H45E H 0.2533 0.9233 1.0476 0.124 Uiso 0.50 1 calc PR B 2 H45F H 0.3289 0.9710 1.0485 0.124 Uiso 0.50 1 calc PR B 2 C46 C 0.1112(8) 1.0074(8) 0.7763(8) 0.109(5) Uani 1 1 d . . . H46A H 0.0946 0.9752 0.7464 0.163 Uiso 1 1 calc R . . H46B H 0.1385 1.0516 0.7502 0.163 Uiso 1 1 calc R . . H46C H 0.0663 1.0243 0.8046 0.163 Uiso 1 1 calc R . . C47 C 0.0904(6) 0.8134(6) 0.7783(5) 0.046(3) Uani 1 1 d . . . H47A H 0.0461 0.8488 0.7817 0.055 Uiso 1 1 calc R . . H47B H 0.0887 0.7793 0.8210 0.055 Uiso 1 1 calc R . . C48 C 0.0872(5) 0.7679(6) 0.7225(5) 0.048(3) Uani 1 1 d . . . H48A H 0.1320 0.7332 0.7191 0.058 Uiso 1 1 calc R . . H48B H 0.0400 0.7369 0.7316 0.058 Uiso 1 1 calc R . . C49 C 0.1318(6) 0.8106(6) 0.6042(5) 0.033(3) Uani 1 1 d . . . C50 C 0.1341(6) 0.8760(5) 0.5496(5) 0.032(2) Uani 1 1 d . . . C51 C 0.0867(5) 0.9402(7) 0.5488(6) 0.046(3) Uani 1 1 d . . . H51A H 0.0465 0.9440 0.5844 0.055 Uiso 1 1 calc R . . C52 C 0.0989(6) 0.9982(6) 0.4959(6) 0.045(3) Uani 1 1 d . . . H52A H 0.0675 1.0425 0.4948 0.054 Uiso 1 1 calc R . . C53 C 0.1564(6) 0.9910(6) 0.4455(5) 0.039(3) Uani 1 1 d . . . H53A H 0.1658 1.0302 0.4087 0.047 Uiso 1 1 calc R . . C54 C 0.2009(5) 0.9263(6) 0.4482(5) 0.028(2) Uani 1 1 d . . . C55 C 0.2649(5) 0.9139(6) 0.3960(5) 0.030(2) Uani 1 1 d . . . C56 C 0.3330(6) 0.9576(6) 0.2941(6) 0.037(3) Uani 1 1 d . . . C57 C 0.3700(6) 0.8857(6) 0.2976(6) 0.037(3) Uani 1 1 d . . . C58 C 0.3513(7) 1.0200(6) 0.2387(5) 0.041(3) Uani 1 1 d . . . C59 C 0.2909(7) 1.0671(7) 0.2196(6) 0.057(3) Uani 1 1 d . . . H59A H 0.2402 1.0575 0.2418 0.068 Uiso 1 1 calc R . . C60 C 0.3043(10) 1.1277(7) 0.1685(7) 0.077(4) Uani 1 1 d . . . H60A H 0.2632 1.1598 0.1564 0.092 Uiso 1 1 calc R . . C61 C 0.3773(11) 1.1407(8) 0.1356(7) 0.081(4) Uani 1 1 d . . . H61A H 0.3866 1.1805 0.0993 0.098 Uiso 1 1 calc R . . C62 C 0.4375(9) 1.0955(8) 0.1554(6) 0.072(4) Uani 1 1 d . . . H62A H 0.4882 1.1060 0.1335 0.087 Uiso 1 1 calc R . . C63 C 0.4252(7) 1.0351(6) 0.2069(6) 0.050(3) Uani 1 1 d . . . H63A H 0.4670 1.0047 0.2200 0.061 Uiso 1 1 calc R . . C64 C 0.4241(7) 0.8628(6) 0.2425(6) 0.046(3) Uani 1 1 d . . . C65 C 0.4039(7) 0.8678(6) 0.1795(7) 0.057(3) Uani 1 1 d . . . H65A H 0.3542 0.8858 0.1720 0.068 Uiso 1 1 calc R . . C66 C 0.4541(10) 0.8471(7) 0.1279(7) 0.074(4) Uani 1 1 d . . . H66A H 0.4399 0.8514 0.0847 0.089 Uiso 1 1 calc R . . C67 C 0.5238(9) 0.8208(7) 0.1392(7) 0.066(3) Uani 1 1 d . . . H67A H 0.5585 0.8062 0.1034 0.079 Uiso 1 1 calc R . . C68 C 0.5469(8) 0.8141(6) 0.2015(8) 0.071(4) Uani 1 1 d . . . H68A H 0.5966 0.7955 0.2085 0.085 Uiso 1 1 calc R . . C69 C 0.4942(8) 0.8357(6) 0.2544(6) 0.056(3) Uani 1 1 d . . . H69A H 0.5079 0.8313 0.2978 0.067 Uiso 1 1 calc R . . C70 C 0.3428(6) 0.7474(5) 0.8520(5) 0.031(2) Uani 1 1 d . . . C71 C 0.3598(6) 0.7127(5) 0.9128(5) 0.036(2) Uani 1 1 d . . . H71A H 0.3190 0.7022 0.9485 0.043 Uiso 1 1 calc R . . C72 C 0.4340(6) 0.6926(5) 0.9238(5) 0.036(3) Uani 1 1 d . C . C73 C 0.4919(6) 0.7064(5) 0.8708(5) 0.034(2) Uani 1 1 d . . . H73A H 0.5430 0.6920 0.8771 0.041 Uiso 1 1 calc R . . C74 C 0.4779(6) 0.7408(5) 0.8084(5) 0.035(3) Uani 1 1 d . . . C75 C 0.4044(6) 0.7631(5) 0.8008(5) 0.029(2) Uani 1 1 d . . . C76 C 0.4527(6) 0.6573(5) 0.9922(5) 0.049(3) Uani 1 1 d D . . C77 C 0.4282(12) 0.7111(12) 1.0375(10) 0.072(6) Uiso 0.60 1 d P C 1 H77A H 0.4609 0.7561 1.0259 0.109 Uiso 0.60 1 calc PR C 1 H77B H 0.4326 0.6876 1.0830 0.109 Uiso 0.60 1 calc PR C 1 H77C H 0.3747 0.7258 1.0344 0.109 Uiso 0.60 1 calc PR C 1 C78 C 0.5329(11) 0.6288(13) 0.9921(10) 0.077(6) Uiso 0.60 1 d P C 1 H78A H 0.5687 0.6713 0.9780 0.116 Uiso 0.60 1 calc PR C 1 H78B H 0.5433 0.5915 0.9613 0.116 Uiso 0.60 1 calc PR C 1 H78C H 0.5397 0.6048 1.0369 0.116 Uiso 0.60 1 calc PR C 1 C79 C 0.3976(10) 0.5831(10) 1.0173(9) 0.056(5) Uiso 0.60 1 d P C 1 H79A H 0.4084 0.5589 1.0610 0.083 Uiso 0.60 1 calc PR C 1 H79B H 0.4078 0.5469 0.9855 0.083 Uiso 0.60 1 calc PR C 1 H79C H 0.3437 0.5989 1.0205 0.083 Uiso 0.60 1 calc PR C 1 C77' C 0.3872(11) 0.6665(15) 1.0497(11) 0.058(8) Uiso 0.40 1 d PD C 2 H77D H 0.3892 0.7174 1.0619 0.087 Uiso 0.40 1 calc PR C 2 H77E H 0.3935 0.6285 1.0881 0.087 Uiso 0.40 1 calc PR C 2 H77F H 0.3375 0.6594 1.0352 0.087 Uiso 0.40 1 calc PR C 2 C78' C 0.5258(11) 0.6993(14) 1.0084(13) 0.062(8) Uiso 0.40 1 d PD C 2 H78D H 0.5380 0.7442 0.9751 0.093 Uiso 0.40 1 calc PR C 2 H78E H 0.5699 0.6645 1.0075 0.093 Uiso 0.40 1 calc PR C 2 H78F H 0.5141 0.7148 1.0525 0.093 Uiso 0.40 1 calc PR C 2 C79' C 0.4753(15) 0.5733(10) 0.9925(15) 0.081(10) Uiso 0.40 1 d PD C 2 H79D H 0.5296 0.5696 0.9741 0.122 Uiso 0.40 1 calc PR C 2 H79E H 0.4437 0.5500 0.9655 0.122 Uiso 0.40 1 calc PR C 2 H79F H 0.4671 0.5468 1.0382 0.122 Uiso 0.40 1 calc PR C 2 C80 C 0.5424(6) 0.7534(6) 0.7494(5) 0.049(3) Uani 1 1 d . . . H80A H 0.5214 0.7784 0.7101 0.074 Uiso 1 1 calc R . . H80B H 0.5648 0.7043 0.7405 0.074 Uiso 1 1 calc R . . H80C H 0.5821 0.7854 0.7597 0.074 Uiso 1 1 calc R . . C81 C 0.3923(5) 0.8808(5) 0.7303(4) 0.031(2) Uani 1 1 d . . . H81A H 0.4460 0.8969 0.7291 0.038 Uiso 1 1 calc R . . H81B H 0.3600 0.9006 0.7677 0.038 Uiso 1 1 calc R . . C82 C 0.3642(5) 0.9100(5) 0.6667(4) 0.028(2) Uani 1 1 d . . . H82A H 0.3108 0.8930 0.6685 0.033 Uiso 1 1 calc R . . H82B H 0.3641 0.9661 0.6604 0.033 Uiso 1 1 calc R . . C83 C 0.3864(6) 0.8445(5) 0.5686(4) 0.027(2) Uani 1 1 d . . . C84 C 0.4449(5) 0.8093(5) 0.5205(5) 0.030(2) Uani 1 1 d . . . C85 C 0.5229(6) 0.8195(6) 0.5113(5) 0.042(3) Uani 1 1 d . . . H85A H 0.5457 0.8508 0.5366 0.050 Uiso 1 1 calc R . . C86 C 0.5676(6) 0.7832(6) 0.4642(5) 0.046(3) Uani 1 1 d . . . H86A H 0.6216 0.7906 0.4561 0.056 Uiso 1 1 calc R . . C87 C 0.5340(6) 0.7362(5) 0.4290(5) 0.038(3) Uani 1 1 d . . . H87A H 0.5642 0.7094 0.3978 0.045 Uiso 1 1 calc R . . C88 C 0.4552(6) 0.7293(5) 0.4406(5) 0.029(2) Uani 1 1 d . . . C89 C 0.4134(6) 0.6836(5) 0.4035(5) 0.030(2) Uani 1 1 d . . . C90 C 0.4134(6) 0.6172(5) 0.3177(5) 0.029(2) Uani 1 1 d . . . C91 C 0.3323(6) 0.6184(5) 0.3298(5) 0.032(2) Uani 1 1 d . . . C92 C 0.4578(6) 0.5779(6) 0.2652(5) 0.038(3) Uani 1 1 d . . . C93 C 0.5267(6) 0.6063(6) 0.2321(5) 0.039(3) Uani 1 1 d . . . H93A H 0.5463 0.6509 0.2436 0.047 Uiso 1 1 calc R . . C94 C 0.5684(6) 0.5716(7) 0.1824(5) 0.050(3) Uani 1 1 d . . . H94A H 0.6151 0.5932 0.1591 0.060 Uiso 1 1 calc R . . C95 C 0.5417(7) 0.5054(7) 0.1670(5) 0.053(3) Uani 1 1 d . . . H95A H 0.5702 0.4815 0.1328 0.064 Uiso 1 1 calc R . . C96 C 0.4743(7) 0.4736(6) 0.2007(6) 0.050(3) Uani 1 1 d . . . H96A H 0.4573 0.4270 0.1909 0.060 Uiso 1 1 calc R . . C97 C 0.4314(6) 0.5096(6) 0.2487(5) 0.043(3) Uani 1 1 d . . . H97A H 0.3839 0.4886 0.2709 0.052 Uiso 1 1 calc R . . C98 C 0.2799(6) 0.5942(6) 0.2874(5) 0.037(3) Uani 1 1 d . . . C99 C 0.2888(6) 0.6197(6) 0.2206(6) 0.046(3) Uani 1 1 d . . . H99A H 0.3299 0.6530 0.2014 0.055 Uiso 1 1 calc R . . C100 C 0.2394(7) 0.5979(7) 0.1808(6) 0.058(3) Uani 1 1 d . . . H10J H 0.2462 0.6167 0.1347 0.070 Uiso 1 1 calc R . . C101 C 0.1802(8) 0.5489(8) 0.2080(7) 0.069(4) Uani 1 1 d . . . H10K H 0.1469 0.5327 0.1804 0.083 Uiso 1 1 calc R . . C102 C 0.1694(6) 0.5237(6) 0.2746(7) 0.059(3) Uani 1 1 d . . . H10L H 0.1279 0.4905 0.2931 0.070 Uiso 1 1 calc R . . C103 C 0.2173(6) 0.5455(6) 0.3153(5) 0.041(3) Uani 1 1 d . . . H10M H 0.2088 0.5281 0.3617 0.049 Uiso 1 1 calc R . . Yb2 Yb 0.13328(3) 0.26426(3) 1.41613(2) 0.0511(2) Uani 1 1 d D D . O30 O 0.2373(4) 0.1839(4) 1.4080(3) 0.0504(18) Uani 1 1 d . D . O31 O 0.1949(5) 0.3143(5) 1.4902(5) 0.087(3) Uani 1 1 d . D . C999 C 0.2063(13) 0.2873(9) 1.5604(13) 0.181(11) Uani 1 1 d . D 1 H99B H 0.2368 0.3244 1.5760 0.272 Uiso 1 1 calc R D 1 H99C H 0.2333 0.2384 1.5628 0.272 Uiso 1 1 calc R D 1 H99D H 0.1562 0.2813 1.5885 0.272 Uiso 1 1 calc R D 1 C104 C 0.3006(6) 0.1857(7) 1.3542(5) 0.061(3) Uani 1 1 d . . . H10N H 0.3366 0.1443 1.3649 0.091 Uiso 1 1 calc R D . H10O H 0.3272 0.2344 1.3481 0.091 Uiso 1 1 calc R . . H10P H 0.2809 0.1795 1.3132 0.091 Uiso 1 1 calc R . . N700 N 0.0498(6) 0.1865(6) 1.5335(5) 0.060(3) Uani 1 1 d D . . O701 O 0.0239(5) 0.2446(5) 1.5023(4) 0.069(2) Uani 1 1 d D D . O702 O 0.1196(5) 0.1693(4) 1.5118(3) 0.0545(19) Uani 1 1 d D D . O703 O 0.0149(5) 0.1470(5) 1.5805(4) 0.078(3) Uani 1 1 d D . . N710 N 0.0290(6) 0.3764(7) 1.3771(6) 0.074(3) Uani 1 1 d D . . O711 O 0.0296(4) 0.3127(5) 1.3615(4) 0.076(3) Uani 1 1 d D D . O712 O 0.0752(6) 0.3880(4) 1.4171(4) 0.074(2) Uani 1 1 d D D . O713 O -0.0116(5) 0.4286(5) 1.3562(5) 0.097(3) Uani 1 1 d D . . O723 O 0.2946(7) 0.3770(6) 1.2708(7) 0.136(4) Uani 1 1 d . . . N720 N 0.2300(14) 0.3447(10) 1.3187(10) 0.056(5) Uiso 0.60 1 d P D 1 O721 O 0.1831(10) 0.3146(9) 1.3031(8) 0.093(5) Uiso 0.60 1 d P D 1 O722 O 0.2468(12) 0.3491(11) 1.3759(11) 0.111(7) Uiso 0.60 1 d P D 1 O621 O 0.1959(13) 0.3360(11) 1.3448(12) 0.059(6) Uiso 0.40 1 d P D 2 O622 O 0.3109(16) 0.3857(16) 1.3744(13) 0.113(8) Uiso 0.40 1 d P D 2 N620 N 0.267(2) 0.3609(19) 1.337(2) 0.082(10) Uiso 0.40 1 d P D 2 N730 N 0.0921(5) 0.1491(6) 1.3315(5) 0.061(3) Uani 1 1 d D . . O732 O 0.0711(4) 0.1588(4) 1.3904(5) 0.067(2) Uani 1 1 d D D . O731 O 0.1361(7) 0.2088(7) 1.3088(5) 0.080(3) Uiso 0.70 1 d PD D 1 O733 O 0.0638(7) 0.1092(7) 1.3016(6) 0.054(4) Uiso 0.70 1 d PD D 1 O633 O 0.0464(11) 0.0879(12) 1.3252(11) 0.019(6) Uiso 0.30 1 d P D 2 O634 O 0.1556(12) 0.1500(12) 1.2900(10) 0.039(5) Uiso 0.30 1 d P D 2 N800 N 0.4441(5) 0.9954(6) 0.4049(4) 0.041(2) Uani 1 1 d D . . O801 O 0.4938(5) 0.9547(4) 0.3792(4) 0.072(2) Uani 1 1 d D . . O802 O 0.3964(4) 0.9669(4) 0.4548(4) 0.0557(19) Uani 1 1 d D . . O803 O 0.4389(3) 1.0640(4) 0.3849(3) 0.0401(17) Uani 1 1 d D . . N810 N 0.2957(5) 0.3651(7) 0.7171(7) 0.074(3) Uani 1 1 d D . . O811 O 0.3166(6) 0.3673(7) 0.6576(6) 0.112(4) Uani 1 1 d D . . O812 O 0.3007(6) 0.3030(6) 0.7557(6) 0.122(4) Uani 1 1 d D . . O813 O 0.2709(4) 0.4202(5) 0.7414(4) 0.056(2) Uani 1 1 d 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 0.0287(3) 0.0125(3) 0.0378(3) -0.0060(2) -0.0070(2) -0.00054(19) O1 0.035(4) 0.016(4) 0.043(4) -0.004(3) -0.012(3) 0.001(3) O2 0.033(4) 0.016(4) 0.050(4) -0.006(3) -0.009(3) 0.009(3) O3 0.020(4) 0.019(4) 0.037(4) -0.010(3) -0.006(3) -0.002(3) O4 0.062(5) 0.026(4) 0.039(5) -0.009(3) -0.007(4) 0.008(4) O5 0.038(5) 0.053(5) 0.068(5) 0.006(4) -0.005(4) -0.001(4) O6 0.052(4) 0.019(4) 0.038(5) -0.012(3) -0.003(3) -0.009(3) N1 0.030(4) 0.008(4) 0.045(5) -0.004(4) -0.011(4) -0.005(3) N2 0.028(5) 0.013(5) 0.042(5) -0.002(5) -0.010(5) -0.003(4) N3 0.024(4) 0.009(4) 0.046(5) -0.004(4) -0.007(5) -0.007(4) N4 0.032(5) 0.017(5) 0.043(6) -0.013(5) -0.013(4) -0.004(4) N5 0.031(5) 0.011(5) 0.050(6) -0.001(4) -0.018(5) -0.001(4) N6 0.031(6) 0.014(5) 0.049(5) -0.011(4) -0.006(5) -0.003(4) N7 0.039(5) 0.019(5) 0.036(5) -0.002(5) -0.011(4) 0.009(4) N8 0.037(5) 0.026(6) 0.047(6) -0.008(6) -0.005(5) -0.004(4) N9 0.035(5) 0.009(4) 0.045(5) -0.007(4) -0.005(5) -0.004(4) N10 0.028(5) 0.020(5) 0.048(5) -0.011(5) -0.007(4) -0.001(4) N11 0.042(6) 0.020(6) 0.051(6) -0.011(6) -0.018(5) -0.004(4) N12 0.045(5) 0.019(5) 0.039(5) -0.012(4) -0.008(5) 0.004(4) N13 0.051(5) 0.016(5) 0.034(5) -0.002(4) -0.008(4) -0.009(4) N14 0.036(5) 0.032(6) 0.052(6) -0.005(5) -0.003(5) 0.011(4) N15 0.026(4) 0.016(4) 0.043(5) -0.004(4) -0.008(4) -0.005(4) C1 0.041(7) 0.020(7) 0.038(6) -0.002(5) -0.002(5) -0.007(5) C2 0.046(7) 0.024(7) 0.040(7) -0.002(6) -0.008(6) -0.001(5) C3 0.045(7) 0.031(7) 0.040(7) -0.008(5) -0.004(6) -0.012(6) C4 0.049(7) 0.050(8) 0.040(7) -0.013(6) -0.006(6) -0.013(6) C5 0.065(8) 0.051(8) 0.058(9) -0.005(7) 0.004(7) -0.036(6) C6 0.075(8) 0.030(7) 0.054(8) -0.010(6) -0.011(7) -0.020(7) C7 0.051(7) 0.019(7) 0.035(7) -0.003(6) -0.009(6) -0.001(6) C8 0.049(7) 0.096(10) 0.055(8) -0.016(7) 0.002(6) -0.031(7) C12 0.102(10) 0.052(8) 0.073(9) -0.018(7) -0.007(7) -0.035(7) C13 0.062(7) 0.021(6) 0.038(7) -0.008(5) -0.017(6) 0.000(6) C14 0.058(7) 0.023(6) 0.033(7) -0.008(5) -0.013(6) -0.005(5) C15 0.039(6) 0.011(7) 0.034(7) -0.009(5) -0.004(5) 0.008(5) C16 0.048(3) 0.016(3) 0.045(3) -0.005(2) -0.011(2) -0.006(2) C17 0.048(3) 0.016(3) 0.045(3) -0.005(2) -0.011(2) -0.006(2) C18 0.048(3) 0.016(3) 0.045(3) -0.005(2) -0.011(2) -0.006(2) C19 0.048(3) 0.016(3) 0.045(3) -0.005(2) -0.011(2) -0.006(2) C20 0.048(3) 0.016(3) 0.045(3) -0.005(2) -0.011(2) -0.006(2) C21 0.021(5) 0.020(7) 0.041(6) -0.011(5) -0.003(5) -0.005(5) C22 0.030(6) 0.019(7) 0.044(7) -0.006(6) -0.006(5) 0.001(6) C23 0.015(5) 0.028(7) 0.040(7) -0.013(6) 0.000(5) 0.015(5) C24 0.035(6) 0.022(7) 0.041(6) -0.012(5) -0.011(5) -0.010(6) C25 0.045(7) 0.046(9) 0.040(6) -0.010(5) -0.015(6) -0.006(6) C26 0.073(8) 0.039(8) 0.050(7) -0.002(6) -0.014(7) -0.026(7) C27 0.064(8) 0.064(10) 0.073(9) 0.004(8) -0.032(7) -0.040(8) C28 0.061(8) 0.057(10) 0.097(10) 0.008(7) -0.055(8) -0.010(7) C29 0.054(7) 0.026(7) 0.072(8) 0.005(6) -0.017(7) -0.005(6) C30 0.024(5) 0.030(8) 0.038(7) -0.002(6) -0.008(4) 0.002(5) C31 0.067(8) 0.025(7) 0.054(8) -0.020(7) -0.005(6) 0.004(5) C32 0.098(9) 0.041(9) 0.034(8) -0.003(7) -0.006(6) -0.005(7) C33 0.094(9) 0.024(9) 0.053(9) 0.008(6) -0.009(6) -0.002(6) C34 0.067(7) 0.022(7) 0.033(7) -0.003(7) -0.008(5) 0.007(5) C35 0.031(6) 0.018(7) 0.045(7) -0.011(6) -0.006(5) 0.003(5) C36 0.027(6) 0.039(8) 0.041(7) -0.011(6) 0.003(5) -0.005(6) C37 0.046(7) 0.022(8) 0.047(7) 0.002(6) 0.012(6) 0.000(5) C38 0.043(7) 0.026(8) 0.076(8) -0.011(7) 0.005(6) -0.001(6) C39 0.064(9) 0.032(8) 0.121(11) -0.020(8) -0.008(8) 0.002(7) C40 0.053(8) 0.044(10) 0.117(12) 0.002(8) -0.017(8) 0.007(7) C41 0.046(7) 0.046(9) 0.054(8) -0.013(7) -0.001(7) -0.002(7) C42 0.066(8) 0.027(7) 0.086(9) -0.029(7) 0.015(7) -0.003(6) C46 0.088(10) 0.053(9) 0.199(17) -0.021(10) -0.070(11) 0.018(8) C47 0.043(7) 0.042(7) 0.048(7) -0.007(6) 0.006(5) 0.007(6) C48 0.030(6) 0.052(8) 0.060(8) -0.008(7) 0.000(5) 0.012(5) C49 0.026(6) 0.022(8) 0.049(8) 0.002(7) -0.013(6) -0.015(6) C50 0.022(6) 0.021(7) 0.057(8) -0.017(6) -0.006(6) 0.002(5) C51 0.022(6) 0.046(8) 0.068(8) -0.017(7) 0.003(5) -0.003(6) C52 0.038(7) 0.019(7) 0.076(8) -0.004(7) -0.007(7) -0.003(5) C53 0.036(7) 0.020(7) 0.061(8) 0.004(5) -0.013(7) -0.009(6) C54 0.020(6) 0.021(7) 0.048(7) -0.007(6) -0.015(6) -0.002(6) C55 0.034(7) 0.019(7) 0.038(7) 0.008(6) -0.014(6) -0.018(6) C56 0.045(7) 0.016(8) 0.054(8) -0.006(6) -0.020(7) -0.011(6) C57 0.045(7) 0.020(8) 0.047(8) -0.003(7) -0.013(6) -0.014(6) C58 0.069(9) 0.017(7) 0.043(7) -0.001(6) -0.024(7) -0.011(7) C59 0.076(9) 0.040(8) 0.056(8) -0.001(7) -0.019(7) -0.030(7) C60 0.113(13) 0.045(9) 0.075(10) 0.022(8) -0.044(9) -0.025(8) C61 0.132(14) 0.052(10) 0.062(9) 0.010(7) -0.032(11) -0.039(11) C62 0.111(12) 0.054(9) 0.051(8) -0.004(8) 0.001(8) -0.047(9) C63 0.074(10) 0.023(7) 0.056(8) -0.008(7) -0.008(7) -0.017(6) C64 0.060(9) 0.022(6) 0.054(10) 0.001(6) -0.007(7) -0.012(6) C65 0.074(9) 0.042(8) 0.057(9) -0.015(6) -0.008(8) -0.009(6) C66 0.093(11) 0.060(9) 0.076(11) -0.026(8) -0.013(10) -0.017(8) C67 0.092(12) 0.045(8) 0.058(10) -0.019(6) 0.008(8) -0.007(7) C68 0.083(10) 0.026(7) 0.097(12) 0.006(7) -0.004(10) -0.008(6) C69 0.065(9) 0.043(8) 0.054(8) -0.005(6) 0.011(8) -0.004(7) C70 0.047(7) 0.011(5) 0.036(7) -0.005(5) -0.006(6) -0.006(5) C71 0.046(8) 0.026(6) 0.033(7) -0.003(5) 0.001(5) -0.004(5) C72 0.053(8) 0.020(6) 0.035(7) -0.001(5) -0.011(7) 0.000(5) C73 0.044(7) 0.019(6) 0.038(7) 0.002(5) -0.009(6) 0.003(5) C74 0.048(8) 0.008(6) 0.052(8) -0.017(5) -0.006(6) 0.001(5) C75 0.051(8) 0.013(6) 0.025(7) -0.007(5) -0.005(6) -0.002(5) C76 0.067(8) 0.031(7) 0.051(7) -0.006(6) -0.013(6) 0.002(6) C80 0.047(7) 0.048(7) 0.048(7) 0.002(5) 0.001(6) 0.003(5) C81 0.045(6) 0.014(7) 0.036(6) -0.002(5) -0.010(5) -0.006(4) C82 0.030(5) 0.014(5) 0.039(6) -0.007(5) 0.005(5) -0.005(4) C83 0.038(8) 0.007(6) 0.034(6) -0.001(5) -0.006(6) -0.001(5) C84 0.021(7) 0.027(6) 0.043(6) -0.005(5) -0.005(5) -0.001(5) C85 0.040(8) 0.037(7) 0.055(7) -0.021(6) -0.013(6) 0.000(6) C86 0.029(6) 0.051(7) 0.067(7) -0.039(7) -0.006(6) 0.017(6) C87 0.049(9) 0.023(6) 0.046(7) -0.020(5) -0.009(6) 0.002(5) C88 0.019(7) 0.025(6) 0.042(6) -0.013(5) 0.000(5) 0.004(5) C89 0.044(8) 0.010(6) 0.038(7) -0.006(5) -0.012(6) 0.002(5) C90 0.039(8) 0.017(6) 0.029(6) -0.007(5) 0.003(6) 0.007(5) C91 0.047(8) 0.009(6) 0.040(7) -0.014(5) -0.003(6) 0.006(5) C92 0.041(8) 0.020(7) 0.053(7) -0.003(6) -0.014(6) 0.001(6) C93 0.042(7) 0.037(7) 0.043(7) -0.019(6) -0.010(6) 0.003(6) C94 0.049(7) 0.063(9) 0.039(7) -0.010(7) -0.002(6) 0.007(7) C95 0.068(9) 0.062(10) 0.037(7) -0.029(7) -0.016(7) 0.034(7) C96 0.068(9) 0.037(7) 0.049(7) -0.019(6) -0.011(7) 0.019(7) C97 0.054(7) 0.033(7) 0.041(7) -0.002(6) -0.003(6) 0.003(6) C98 0.039(7) 0.034(7) 0.043(8) -0.024(6) -0.003(6) 0.007(6) C99 0.051(7) 0.046(7) 0.043(8) -0.010(6) -0.009(6) -0.003(6) C100 0.057(8) 0.059(8) 0.056(8) -0.006(7) -0.002(7) -0.013(7) C101 0.085(11) 0.083(10) 0.051(9) -0.027(8) -0.032(8) 0.015(9) C102 0.042(7) 0.044(8) 0.097(12) -0.029(8) -0.013(7) -0.010(6) C103 0.039(7) 0.035(7) 0.050(7) -0.023(6) 0.008(6) -0.002(6) Yb2 0.0571(4) 0.0291(3) 0.0644(4) -0.0085(3) 0.0009(3) 0.0085(3) O30 0.047(4) 0.050(5) 0.050(4) -0.004(4) 0.005(4) -0.006(3) O31 0.083(6) 0.063(6) 0.123(8) -0.042(6) -0.008(6) -0.009(5) C999 0.22(2) 0.060(12) 0.31(3) -0.074(16) -0.14(2) 0.024(13) C104 0.055(7) 0.058(8) 0.063(8) 0.003(6) -0.001(7) -0.003(6) N700 0.047(8) 0.064(9) 0.066(8) -0.031(7) 0.024(6) 0.002(7) O701 0.078(6) 0.044(6) 0.081(6) -0.008(5) 0.002(5) 0.019(5) O702 0.063(6) 0.037(5) 0.059(5) -0.003(4) 0.005(4) -0.007(4) O703 0.082(6) 0.061(6) 0.072(6) -0.008(5) 0.047(5) -0.003(5) N710 0.053(7) 0.058(10) 0.096(9) 0.015(8) -0.001(6) 0.036(7) O711 0.077(6) 0.017(5) 0.135(8) -0.014(5) -0.010(5) 0.014(4) O712 0.098(7) 0.037(5) 0.085(6) -0.015(4) -0.004(5) 0.019(5) O713 0.078(6) 0.058(7) 0.139(8) 0.011(6) 0.007(6) 0.022(6) O723 0.140(10) 0.069(7) 0.187(13) -0.010(7) 0.006(9) 0.022(7) N730 0.030(6) 0.075(8) 0.079(8) -0.004(7) -0.017(6) -0.002(5) O732 0.064(5) 0.063(6) 0.085(6) -0.038(5) -0.021(5) 0.027(4) N800 0.043(6) 0.031(7) 0.053(6) -0.004(6) -0.016(5) -0.015(6) O801 0.077(6) 0.039(5) 0.100(7) -0.032(5) 0.002(5) 0.008(5) O802 0.052(5) 0.037(5) 0.074(5) 0.011(4) -0.012(5) -0.009(4) O803 0.039(4) 0.020(5) 0.060(5) 0.004(4) -0.013(3) -0.004(3) N810 0.060(7) 0.039(9) 0.141(13) -0.036(10) -0.047(8) 0.008(6) O811 0.095(7) 0.157(11) 0.110(8) -0.097(8) -0.034(7) 0.034(7) O812 0.118(8) 0.035(6) 0.226(13) -0.003(7) -0.093(8) 0.006(5) O813 0.070(5) 0.028(5) 0.071(5) -0.003(4) -0.017(4) -0.008(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 O3 2.286(6) . ? Yb1 O1 2.290(6) . ? Yb1 O2 2.317(6) . ? Yb1 N2 2.465(7) . ? Yb1 N3 2.475(7) . ? Yb1 N1 2.477(6) . ? Yb1 N6 2.510(7) . ? Yb1 N4 2.523(7) . ? Yb1 N5 2.535(8) . ? Yb1 C49 3.161(13) . ? Yb1 C83 3.172(11) . ? Yb1 C15 3.188(11) . ? O1 C15 1.271(11) . ? O2 C49 1.235(11) . ? O3 C83 1.250(10) . ? O4 C7 1.391(11) . ? O4 C13 1.439(11) . ? O5 C41 1.388(12) . ? O5 C47 1.441(11) . ? O6 C75 1.407(10) . ? O6 C81 1.445(10) . ? N1 C20 1.328(11) . ? N1 C16 1.352(11) . ? N2 C50 1.328(11) . ? N2 C54 1.354(11) . ? N3 C88 1.342(11) . ? N3 C84 1.352(11) . ? N4 C21 1.330(11) . ? N4 N7 1.339(10) . ? N5 C55 1.337(12) . ? N5 N8 1.347(10) . ? N6 C89 1.336(11) . ? N6 N9 1.346(10) . ? N7 C23 1.341(11) . ? N8 C57 1.334(12) . ? N9 C91 1.333(11) . ? N10 C22 1.315(11) . ? N10 C21 1.343(11) . ? N11 C56 1.340(12) . ? N11 C55 1.346(12) . ? N12 C90 1.318(11) . ? N12 C89 1.355(11) . ? N13 C15 1.303(11) . ? N13 C14 1.467(11) . ? N13 H13C 0.8800 . ? N14 C49 1.333(12) . ? N14 C48 1.431(12) . ? N14 H14C 0.8800 . ? N15 C83 1.325(11) . ? N15 C82 1.453(11) . ? N15 H15A 0.8800 . ? C1 C36 1.517(13) . ? C1 C2 1.525(13) . ? C1 C70 1.534(13) . ? C1 H1A 1.0000 . ? C2 C7 1.393(13) . ? C2 C3 1.394(13) . ? C3 C4 1.378(13) . ? C3 H3A 0.9500 . ? C4 C5 1.405(14) . ? C4 C8 1.517(14) . ? C5 C6 1.374(15) . ? C5 H5A 0.9500 . ? C6 C7 1.381(14) . ? C6 C12 1.519(15) . ? C8 C11 1.476(14) . ? C8 C9 1.513(14) . ? C8 C11' 1.51(2) . ? C8 C10" 1.516(17) . ? C8 C11" 1.526(17) . ? C8 C10' 1.54(2) . ? C8 C9' 1.55(2) . ? C8 C9" 1.649(17) . ? C8 C10 1.663(15) . ? C8 H9'B 1.4879 . ? C8 H10E 1.4279 . ? C9 H9A 0.9799 . ? C9 H9B 0.9801 . ? C9 H9C 0.9800 . ? C9 H9'A 1.3741 . ? C9 H9'B 0.5149 . ? C9 H10G 1.4286 . ? C9 H10I 0.8332 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 1.4000 . ? C10 H10E 0.2954 . ? C10 H10F 1.5214 . ? C10 H11I 1.3223 . ? C10 H10H 1.4213 . ? C11 H11A 0.9800 . ? C11 H11B 0.9799 . ? C11 H11C 0.9800 . ? C11 H11D 1.2018 . ? C11 H11E 0.7171 . ? C11 H11F 1.0482 . ? C11 H9"C 1.5598 . ? C11 H11G 1.5331 . ? C11 H11H 1.1121 . ? C9' H9A 1.5784 . ? C9' H9C 0.7071 . ? C9' H9'A 0.9800 . ? C9' H9'B 0.9799 . ? C9' H9'C 0.9801 . ? C9' H9"A 1.3202 . ? C9' H9"B 0.8168 . ? C10' H10A 1.1914 . ? C10' H10C 1.0221 . ? C10' H10D 0.9799 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C10' H10G 1.4076 . ? C10' H10H 0.6639 . ? C11' H11A 0.7826 . ? C11' H11B 1.2468 . ? C11' H11C 0.9835 . ? C11' H11D 0.9799 . ? C11' H11E 0.9801 . ? C11' H11F 0.9800 . ? C11' H11G 1.2394 . ? C11' H11H 1.0887 . ? C9" H9C 1.5434 . ? C9" H11B 1.1310 . ? C9" H9'A 1.3461 . ? C9" H9'C 1.2932 . ? C9" H11E 1.0652 . ? C9" H9"A 0.9800 . ? C9" H9"B 0.9800 . ? C9" H9"C 0.9800 . ? C11" H11A 1.5380 . ? C11" H11C 1.0639 . ? C11" H10E 1.4498 . ? C11" H11F 0.9385 . ? C11" H11G 0.9800 . ? C11" H11H 0.9800 . ? C11" H11I 0.9800 . ? C10" H9A 1.2079 . ? C10" H9B 1.0643 . ? C10" H9'B 1.2743 . ? C10" H10D 1.4472 . ? C10" H10F 1.3872 . ? C10" H10G 0.9802 . ? C10" H10H 0.9800 . ? C10" H10I 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.486(12) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.478(13) . ? C16 C17 1.412(13) . ? C17 C18 1.367(12) . ? C17 H17A 0.9500 . ? C18 C19 1.373(12) . ? C18 H18A 0.9500 . ? C19 C20 1.403(13) . ? C19 H19A 0.9500 . ? C20 C21 1.483(13) . ? C22 C23 1.455(13) . ? C22 C24 1.463(13) . ? C23 C30 1.494(13) . ? C24 C29 1.349(13) . ? C24 C25 1.381(13) . ? C25 C26 1.389(14) . ? C25 H25A 0.9500 . ? C26 C27 1.357(15) . ? C26 H26A 0.9500 . ? C27 C28 1.379(16) . ? C27 H27A 0.9500 . ? C28 C29 1.408(14) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C35 1.392(12) . ? C30 C31 1.393(13) . ? C31 C32 1.369(14) . ? C31 H31A 0.9500 . ? C32 C33 1.373(15) . ? C32 H32A 0.9500 . ? C33 C34 1.375(14) . ? C33 H33A 0.9500 . ? C34 C35 1.340(12) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C41 1.370(14) . ? C36 C37 1.374(13) . ? C37 C38 1.391(14) . ? C37 H37A 0.9500 . ? C38 C39 1.388(16) . ? C38 C42 1.510(15) . ? C39 C40 1.416(17) . ? C39 H39A 0.9500 . ? C40 C41 1.401(16) . ? C40 C46 1.513(17) . ? C42 C44' 1.40(3) . ? C42 C45 1.46(2) . ? C42 C43 1.56(3) . ? C42 C43' 1.60(4) . ? C42 C44 1.60(2) . ? C42 C45' 1.63(3) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C43' H43D 0.9800 . ? C43' H43E 0.9800 . ? C43' H43F 0.9800 . ? C44' H44D 0.9800 . ? C44' H44E 0.9800 . ? C44' H44F 0.9800 . ? C45' H45D 0.9800 . ? C45' H45E 0.9800 . ? C45' H45F 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.509(14) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.491(14) . ? C50 C51 1.398(13) . ? C51 C52 1.384(14) . ? C51 H51A 0.9500 . ? C52 C53 1.359(14) . ? C52 H52A 0.9500 . ? C53 C54 1.376(13) . ? C53 H53A 0.9500 . ? C54 C55 1.475(13) . ? C56 C57 1.419(14) . ? C56 C58 1.477(14) . ? C57 C64 1.471(14) . ? C58 C63 1.382(14) . ? C58 C59 1.403(14) . ? C59 C60 1.391(16) . ? C59 H59A 0.9500 . ? C60 C61 1.371(18) . ? C60 H60A 0.9500 . ? C61 C62 1.386(18) . ? C61 H61A 0.9500 . ? C62 C63 1.392(15) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? C64 C69 1.356(14) . ? C64 C65 1.384(14) . ? C65 C66 1.368(16) . ? C65 H65A 0.9500 . ? C66 C67 1.341(16) . ? C66 H66A 0.9500 . ? C67 C68 1.389(16) . ? C67 H67A 0.9500 . ? C68 C69 1.417(16) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? C70 C71 1.381(12) . ? C70 C75 1.401(13) . ? C71 C72 1.387(13) . ? C71 H71A 0.9500 . ? C72 C73 1.378(13) . ? C72 C76 1.533(13) . ? C73 C74 1.392(13) . ? C73 H73A 0.9500 . ? C74 C75 1.367(12) . ? C74 C80 1.533(13) . ? C76 C77 1.45(2) . ? C76 C78 1.49(2) . ? C76 C79' 1.538(16) . ? C76 C77' 1.551(15) . ? C76 C78' 1.605(16) . ? C76 C79 1.64(2) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C77' H77D 0.9800 . ? C77' H77E 0.9800 . ? C77' H77F 0.9800 . ? C78' H78D 0.9800 . ? C78' H78E 0.9800 . ? C78' H78F 0.9800 . ? C79' H79D 0.9800 . ? C79' H79E 0.9800 . ? C79' H79F 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.484(12) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.512(13) . ? C84 C85 1.372(12) . ? C85 C86 1.384(13) . ? C85 H85A 0.9500 . ? C86 C87 1.380(13) . ? C86 H86A 0.9500 . ? C87 C88 1.379(12) . ? C87 H87A 0.9500 . ? C88 C89 1.472(13) . ? C90 C91 1.413(13) . ? C90 C92 1.490(13) . ? C91 C98 1.472(13) . ? C92 C93 1.372(13) . ? C92 C97 1.417(13) . ? C93 C94 1.382(14) . ? C93 H93A 0.9500 . ? C94 C95 1.376(15) . ? C94 H94A 0.9500 . ? C95 C96 1.375(15) . ? C95 H95A 0.9500 . ? C96 C97 1.380(14) . ? C96 H96A 0.9500 . ? C97 H97A 0.9500 . ? C98 C99 1.371(13) . ? C98 C103 1.420(13) . ? C99 C100 1.377(14) . ? C99 H99A 0.9500 . ? C100 C101 1.378(16) . ? C100 H10J 0.9500 . ? C101 C102 1.366(15) . ? C101 H10K 0.9500 . ? C102 C103 1.373(14) . ? C102 H10L 0.9500 . ? C103 H10M 0.9500 . ? Yb2 O621 2.01(2) . ? Yb2 O30 2.296(7) . ? Yb2 O31 2.286(9) . ? Yb2 O711 2.360(8) . ? Yb2 O732 2.362(8) . ? Yb2 O702 2.388(7) . ? Yb2 O712 2.408(8) . ? Yb2 O721 2.413(16) . ? Yb2 O701 2.415(8) . ? Yb2 O722 2.50(2) . ? Yb2 O731 2.543(10) . ? Yb2 N720 2.70(2) . ? O30 C104 1.451(12) . ? O31 C999 1.50(2) . ? C999 H99B 0.9800 . ? C999 H99C 0.9800 . ? C999 H99D 0.9800 . ? C104 H10N 0.9800 . ? C104 H10O 0.9800 . ? C104 H10P 0.9800 . ? N700 O703 1.206(10) . ? N700 O701 1.248(10) . ? N700 O702 1.291(9) . ? N710 O711 1.223(10) . ? N710 O713 1.225(10) . ? N710 O712 1.278(10) . ? O723 N620 1.37(4) . ? O723 N720 1.46(3) . ? N720 O721 1.11(2) . ? N720 O722 1.27(3) . ? O621 N620 1.31(5) . ? O622 N620 1.30(4) . ? N730 O733 1.170(11) . ? N730 O732 1.252(10) . ? N730 O634 1.30(2) . ? N730 O731 1.319(11) . ? N730 O633 1.41(2) . ? N800 O801 1.232(9) . ? N800 O803 1.238(9) . ? N800 O802 1.278(9) . ? N810 O813 1.209(10) . ? N810 O811 1.222(11) . ? N810 O812 1.272(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Yb1 O1 79.1(2) . . ? O3 Yb1 O2 77.9(2) . . ? O1 Yb1 O2 77.5(2) . . ? O3 Yb1 N2 72.7(2) . . ? O1 Yb1 N2 137.6(2) . . ? O2 Yb1 N2 66.3(3) . . ? O3 Yb1 N3 66.3(2) . . ? O1 Yb1 N3 74.3(2) . . ? O2 Yb1 N3 137.7(2) . . ? N2 Yb1 N3 119.5(2) . . ? O3 Yb1 N1 137.9(2) . . ? O1 Yb1 N1 66.0(2) . . ? O2 Yb1 N1 72.4(2) . . ? N2 Yb1 N1 118.9(2) . . ? N3 Yb1 N1 121.4(2) . . ? O3 Yb1 N6 130.3(3) . . ? O1 Yb1 N6 89.0(2) . . ? O2 Yb1 N6 146.1(2) . . ? N2 Yb1 N6 133.3(3) . . ? N3 Yb1 N6 64.0(3) . . ? N1 Yb1 N6 73.8(2) . . ? O3 Yb1 N4 144.7(2) . . ? O1 Yb1 N4 129.8(3) . . ? O2 Yb1 N4 88.5(2) . . ? N2 Yb1 N4 72.0(2) . . ? N3 Yb1 N4 133.8(2) . . ? N1 Yb1 N4 63.8(3) . . ? N6 Yb1 N4 76.5(2) . . ? O3 Yb1 N5 89.0(2) . . ? O1 Yb1 N5 146.3(2) . . ? O2 Yb1 N5 130.9(3) . . ? N2 Yb1 N5 64.6(3) . . ? N3 Yb1 N5 72.0(2) . . ? N1 Yb1 N5 133.0(2) . . ? N6 Yb1 N5 74.8(3) . . ? N4 Yb1 N5 75.5(2) . . ? O3 Yb1 C49 71.4(2) . . ? O1 Yb1 C49 94.1(2) . . ? O2 Yb1 C49 19.2(2) . . ? N2 Yb1 C49 47.4(3) . . ? N3 Yb1 C49 137.6(2) . . ? N1 Yb1 C49 87.8(2) . . ? N6 Yb1 C49 158.2(2) . . ? N4 Yb1 C49 85.0(2) . . ? N5 Yb1 C49 112.0(3) . . ? O3 Yb1 C83 18.8(2) . . ? O1 Yb1 C83 73.7(2) . . ? O2 Yb1 C83 94.4(2) . . ? N2 Yb1 C83 87.5(2) . . ? N3 Yb1 C83 47.6(2) . . ? N1 Yb1 C83 139.4(2) . . ? N6 Yb1 C83 111.6(3) . . ? N4 Yb1 C83 156.2(2) . . ? N5 Yb1 C83 84.9(2) . . ? C49 Yb1 C83 90.0(2) . . ? O3 Yb1 C15 95.1(2) . . ? O1 Yb1 C15 19.2(2) . . ? O2 Yb1 C15 70.5(2) . . ? N2 Yb1 C15 136.6(3) . . ? N3 Yb1 C15 90.3(2) . . ? N1 Yb1 C15 47.2(2) . . ? N6 Yb1 C15 86.6(2) . . ? N4 Yb1 C15 110.9(3) . . ? N5 Yb1 C15 158.5(3) . . ? C49 Yb1 C15 89.3(2) . . ? C83 Yb1 C15 92.2(2) . . ? C15 O1 Yb1 124.6(6) . . ? C49 O2 Yb1 122.8(6) . . ? C83 O3 Yb1 125.0(5) . . ? C7 O4 C13 114.1(7) . . ? C41 O5 C47 118.2(7) . . ? C75 O6 C81 113.8(6) . . ? C20 N1 C16 118.8(7) . . ? C20 N1 Yb1 123.5(6) . . ? C16 N1 Yb1 117.6(5) . . ? C50 N2 C54 118.9(8) . . ? C50 N2 Yb1 118.0(6) . . ? C54 N2 Yb1 123.1(6) . . ? C88 N3 C84 118.6(7) . . ? C88 N3 Yb1 123.1(6) . . ? C84 N3 Yb1 118.3(6) . . ? C21 N4 N7 118.9(7) . . ? C21 N4 Yb1 120.9(6) . . ? N7 N4 Yb1 119.1(6) . . ? C55 N5 N8 117.8(8) . . ? C55 N5 Yb1 119.3(7) . . ? N8 N5 Yb1 122.8(6) . . ? C89 N6 N9 117.8(7) . . ? C89 N6 Yb1 121.0(6) . . ? N9 N6 Yb1 119.5(6) . . ? N4 N7 C23 118.9(7) . . ? C57 N8 N5 119.8(8) . . ? C91 N9 N6 119.7(7) . . ? C22 N10 C21 118.8(8) . . ? C56 N11 C55 117.6(8) . . ? C90 N12 C89 115.9(8) . . ? C15 N13 C14 125.0(8) . . ? C15 N13 H13C 117.5 . . ? C14 N13 H13C 117.5 . . ? C49 N14 C48 125.7(8) . . ? C49 N14 H14C 117.1 . . ? C48 N14 H14C 117.1 . . ? C83 N15 C82 124.2(7) . . ? C83 N15 H15A 117.9 . . ? C82 N15 H15A 117.9 . . ? C36 C1 C2 113.5(8) . . ? C36 C1 C70 113.9(8) . . ? C2 C1 C70 112.4(7) . . ? C36 C1 H1A 105.4 . . ? C2 C1 H1A 105.4 . . ? C70 C1 H1A 105.4 . . ? C7 C2 C3 118.5(9) . . ? C7 C2 C1 119.5(9) . . ? C3 C2 C1 121.8(9) . . ? C4 C3 C2 122.6(9) . . ? C4 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? C3 C4 C5 116.2(9) . . ? C3 C4 C8 123.9(9) . . ? C5 C4 C8 119.9(10) . . ? C6 C5 C4 123.1(10) . . ? C6 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? C5 C6 C7 118.6(9) . . ? C5 C6 C12 121.3(11) . . ? C7 C6 C12 120.1(11) . . ? C6 C7 C2 120.7(9) . . ? C6 C7 O4 120.5(9) . . ? C2 C7 O4 118.5(9) . . ? C11 C8 C9 117.6(13) . . ? C11 C8 C11' 11(4) . . ? C9 C8 C11' 116(2) . . ? C11 C8 C4 112.8(11) . . ? C9 C8 C4 113.2(11) . . ? C11' C8 C4 121(3) . . ? C11 C8 C10" 127.8(17) . . ? C9 C8 C10" 34.9(12) . . ? C11' C8 C10" 119(3) . . ? C4 C8 C10" 119.2(15) . . ? C11 C8 C11" 47.1(13) . . ? C9 C8 C11" 136.0(16) . . ? C11' C8 C11" 39(3) . . ? C4 C8 C11" 110.2(14) . . ? C10" C8 C11" 113.7(15) . . ? C11 C8 C10' 123(3) . . ? C9 C8 C10' 70(3) . . ? C11' C8 C10' 111(2) . . ? C4 C8 C10' 114(3) . . ? C10" C8 C10' 36(3) . . ? C11" C8 C10' 86(3) . . ? C11 C8 C9' 85(4) . . ? C9 C8 C9' 42(3) . . ? C11' C8 C9' 90(4) . . ? C4 C8 C9' 107(3) . . ? C10" C8 C9' 76(3) . . ? C11" C8 C9' 128(4) . . ? C10' C8 C9' 111(2) . . ? C11 C8 C9" 56.6(13) . . ? C9 C8 C9" 73.5(13) . . ? C11' C8 C9" 64(3) . . ? C4 C8 C9" 103.4(14) . . ? C10" C8 C9" 105.0(13) . . ? C11" C8 C9" 103.3(13) . . ? C10' C8 C9" 136(3) . . ? C9' C8 C9" 32(3) . . ? C11 C8 C10 105.2(11) . . ? C9 C8 C10 103.3(10) . . ? C11' C8 C10 95(3) . . ? C4 C8 C10 102.7(10) . . ? C10" C8 C10 68.5(14) . . ? C11" C8 C10 59.6(13) . . ? C10' C8 C10 33(3) . . ? C9' C8 C10 142(3) . . ? C9" C8 C10 152.7(15) . . ? C11 C8 H9'B 122.4 . . ? C9 C8 H9'B 19.7 . . ? C11' C8 H9'B 125.2 . . ? C4 C8 H9'B 95.1 . . ? C10" C8 H9'B 50.2 . . ? C11" C8 H9'B 154.7 . . ? C10' C8 H9'B 84.4 . . ? C9' C8 H9'B 37.6 . . ? C9" C8 H9'B 68.8 . . ? C10 C8 H9'B 116.7 . . ? C11 C8 H10E 105.4 . . ? C9 C8 H10E 108.7 . . ? C11' C8 H10E 96.1 . . ? C4 C8 H10E 96.7 . . ? C10" C8 H10E 73.8 . . ? C11" C8 H10E 58.7 . . ? C10' C8 H10E 38.3 . . ? C9' C8 H10E 148.0 . . ? C9" C8 H10E 157.1 . . ? C10 C8 H10E 6.7 . . ? H9'B C8 H10E 120.7 . . ? C8 C9 H9A 112.5 . . ? C8 C9 H9B 114.7 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 100.8 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C9 H9'A 88.3 . . ? H9A C9 H9'A 53.5 . . ? H9B C9 H9'A 156.5 . . ? H9C C9 H9'A 68.3 . . ? C8 C9 H9'B 77.4 . . ? H9A C9 H9'B 155.6 . . ? H9B C9 H9'B 84.1 . . ? H9C C9 H9'B 46.1 . . ? H9'A C9 H9'B 106.7 . . ? C8 C9 H10G 90.9 . . ? H9A C9 H10G 37.1 . . ? H9B C9 H10G 94.1 . . ? H9C C9 H10G 145.7 . . ? H9'A C9 H10G 80.1 . . ? H9'B C9 H10G 166.1 . . ? C8 C9 H10I 125.3 . . ? H9A C9 H10I 96.7 . . ? H9B C9 H10I 13.4 . . ? H9C C9 H10I 111.9 . . ? H9'A C9 H10I 143.8 . . ? H9'B C9 H10I 94.7 . . ? H10G C9 H10I 85.8 . . ? C8 C10 H10A 110.6 . . ? C8 C10 H10B 111.7 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 106.0 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C10 H10D 94.4 . . ? H10A C10 H10D 33.9 . . ? H10B C10 H10D 142.8 . . ? H10C C10 H10D 86.9 . . ? C8 C10 H10E 34.1 . . ? H10A C10 H10E 139.9 . . ? H10B C10 H10E 82.2 . . ? H10C C10 H10E 101.6 . . ? H10D C10 H10E 128.3 . . ? C8 C10 H10F 89.6 . . ? H10A C10 H10F 96.5 . . ? H10B C10 H10F 136.4 . . ? H10C C10 H10F 27.0 . . ? H10D C10 H10F 66.3 . . ? H10E C10 H10F 100.2 . . ? C8 C10 H11I 87.0 . . ? H10A C10 H11I 97.9 . . ? H10B C10 H11I 34.7 . . ? H10C C10 H11I 142.4 . . ? H10D C10 H11I 128.1 . . ? H10E C10 H11I 69.5 . . ? H10F C10 H11I 165.5 . . ? C8 C10 H10H 79.1 . . ? H10A C10 H10H 88.4 . . ? H10B C10 H10H 152.5 . . ? H10C C10 H10H 43.4 . . ? H10D C10 H10H 55.4 . . ? H10E C10 H10H 97.6 . . ? H10F C10 H10H 16.3 . . ? H11I C10 H10H 166.0 . . ? C8 C11 H11A 108.5 . . ? C8 C11 H11B 108.4 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 111.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C11 H11D 111.7 . . ? H11A C11 H11D 7.4 . . ? H11B C11 H11D 113.6 . . ? H11C C11 H11D 102.1 . . ? C8 C11 H11E 103.5 . . ? H11A C11 H11E 105.5 . . ? H11B C11 H11E 8.3 . . ? H11C C11 H11E 117.8 . . ? H11D C11 H11E 110.5 . . ? C8 C11 H11F 111.0 . . ? H11A C11 H11F 97.8 . . ? H11B C11 H11F 120.8 . . ? H11C C11 H11F 13.3 . . ? H11D C11 H11F 90.4 . . ? H11E C11 H11F 129.1 . . ? C8 C11 H9"C 93.1 . . ? H11A C11 H9"C 115.5 . . ? H11B C11 H9"C 15.3 . . ? H11C C11 H9"C 117.4 . . ? H11D C11 H9"C 121.1 . . ? H11E C11 H9"C 12.2 . . ? H11F C11 H9"C 130.1 . . ? C8 C11 H11G 87.2 . . ? H11A C11 H11G 49.5 . . ? H11B C11 H11G 158.0 . . ? H11C C11 H11G 77.3 . . ? H11D C11 H11G 44.8 . . ? H11E C11 H11G 155.0 . . ? H11F C11 H11G 64.2 . . ? H9"C C11 H11G 163.7 . . ? C8 C11 H11H 105.1 . . ? H11A C11 H11H 109.0 . . ? H11B C11 H11H 116.1 . . ? H11C C11 H11H 7.6 . . ? H11D C11 H11H 101.6 . . ? H11E C11 H11H 124.4 . . ? H11F C11 H11H 11.3 . . ? H9"C C11 H11H 122.9 . . ? H11G C11 H11H 72.5 . . ? C8 C9' H9A 84.1 . . ? C8 C9' H9C 114.7 . . ? H9A C9' H9C 78.9 . . ? C8 C9' H9'A 103.4 . . ? H9A C9' H9'A 44.6 . . ? H9C C9' H9'A 106.4 . . ? C8 C9' H9'B 67.9 . . ? H9A C9' H9'B 65.0 . . ? H9C C9' H9'B 47.6 . . ? H9'A C9' H9'B 109.5 . . ? C8 C9' H9'C 145.4 . . ? H9A C9' H9'C 127.5 . . ? H9C C9' H9'C 66.1 . . ? H9'A C9' H9'C 109.5 . . ? H9'B C9' H9'C 109.5 . . ? C8 C9' H9"A 102.4 . . ? H9A C9' H9"A 89.0 . . ? H9C C9' H9"A 139.2 . . ? H9'A C9' H9"A 46.0 . . ? H9'B C9' H9"A 152.6 . . ? H9'C C9' H9"A 92.9 . . ? C8 C9' H9"B 121.2 . . ? H9A C9' H9"B 152.9 . . ? H9C C9' H9"B 81.3 . . ? H9'A C9' H9"B 126.8 . . ? H9'B C9' H9"B 113.0 . . ? H9'C C9' H9"B 25.5 . . ? H9"A C9' H9"B 94.0 . . ? C8 C10' H10A 107.0 . . ? C8 C10' H10C 112.3 . . ? H10A C10' H10C 92.3 . . ? C8 C10' H10D 125.1 . . ? H10A C10' H10D 41.9 . . ? H10C C10' H10D 112.5 . . ? C8 C10' H10E 64.5 . . ? H10A C10' H10E 67.6 . . ? H10C C10' H10E 65.2 . . ? H10D C10' H10E 109.5 . . ? C8 C10' H10F 124.3 . . ? H10A C10' H10F 121.8 . . ? H10C C10' H10F 46.2 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C8 C10' H10G 90.4 . . ? H10A C10' H10G 88.9 . . ? H10C C10' H10G 155.7 . . ? H10D C10' H10G 55.3 . . ? H10E C10' H10G 136.5 . . ? H10F C10' H10G 114.0 . . ? C8 C10' H10H 121.5 . . ? H10A C10' H10H 131.3 . . ? H10C C10' H10H 67.0 . . ? H10D C10' H10H 104.3 . . ? H10E C10' H10H 128.9 . . ? H10F C10' H10H 20.8 . . ? H10G C10' H10H 94.3 . . ? C8 C11' H11A 119.1 . . ? C8 C11' H11B 93.1 . . ? H11A C11' H11B 101.7 . . ? C8 C11' H11C 108.5 . . ? H11A C11' H11C 129.6 . . ? H11B C11' H11C 90.9 . . ? C8 C11' H11D 124.6 . . ? H11A C11' H11D 11.3 . . ? H11B C11' H11D 109.9 . . ? H11C C11' H11D 120.2 . . ? C8 C11' H11E 88.8 . . ? H11A C11' H11E 100.4 . . ? H11B C11' H11E 5.9 . . ? H11C C11' H11E 96.0 . . ? H11D C11' H11E 109.5 . . ? C8 C11' H11F 112.5 . . ? H11A C11' H11F 119.9 . . ? H11B C11' H11F 104.1 . . ? H11C C11' H11F 14.3 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C8 C11' H11G 97.4 . . ? H11A C11' H11G 66.0 . . ? H11B C11' H11G 166.7 . . ? H11C C11' H11G 93.5 . . ? H11D C11' H11G 57.2 . . ? H11E C11' H11G 166.4 . . ? H11F C11' H11G 79.4 . . ? C8 C11' H11H 103.9 . . ? H11A C11' H11H 130.6 . . ? H11B C11' H11H 98.8 . . ? H11C C11' H11H 8.8 . . ? H11D C11' H11H 120.2 . . ? H11E C11' H11H 103.7 . . ? H11F C11' H11H 10.7 . . ? H11G C11' H11H 86.6 . . ? C8 C9" H9C 75.3 . . ? C8 C9" H11B 90.8 . . ? H9C C9" H11B 165.4 . . ? C8 C9" H9'A 83.8 . . ? H9C C9" H9'A 55.7 . . ? H11B C9" H9'A 128.3 . . ? C8 C9" H9'C 110.0 . . ? H9C C9" H9'C 37.8 . . ? H11B C9" H9'C 151.7 . . ? H9'A C9" H9'C 74.6 . . ? C8 C9" H11E 79.1 . . ? H9C C9" H11E 153.9 . . ? H11B C9" H11E 14.8 . . ? H9'A C9" H11E 117.3 . . ? H9'C C9" H11E 166.4 . . ? C8 C9" H9"A 114.4 . . ? H9C C9" H9"A 96.0 . . ? H11B C9" H9"A 93.9 . . ? H9'A C9" H9"A 44.9 . . ? H9'C C9" H9"A 94.6 . . ? H11E C9" H9"A 90.6 . . ? C8 C9" H9"B 102.4 . . ? H9C C9" H9"B 39.0 . . ? H11B C9" H9"B 144.8 . . ? H9'A C9" H9"B 86.0 . . ? H9'C C9" H9"B 14.9 . . ? H11E C9" H9"B 156.6 . . ? H9"A C9" H9"B 109.5 . . ? C8 C9" H9"C 111.4 . . ? H9C C9" H9"C 146.4 . . ? H11B C9" H9"C 35.9 . . ? H9'A C9" H9"C 154.3 . . ? H9'C C9" H9"C 116.1 . . ? H11E C9" H9"C 50.3 . . ? H9"A C9" H9"C 109.5 . . ? H9"B C9" H9"C 109.5 . . ? C8 C11" H11A 82.2 . . ? C8 C11" H11C 103.1 . . ? H11A C11" H11C 73.4 . . ? C8 C11" H10E 57.3 . . ? H11A C11" H10E 120.8 . . ? H11C C11" H10E 149.7 . . ? C8 C11" H11F 114.2 . . ? H11A C11" H11F 71.7 . . ? H11C C11" H11F 12.1 . . ? H10E C11" H11F 160.2 . . ? C8 C11" H11G 109.9 . . ? H11A C11" H11G 49.3 . . ? H11C C11" H11G 105.6 . . ? H10E C11" H11G 103.2 . . ? H11F C11" H11G 96.5 . . ? C8 C11" H11H 109.1 . . ? H11A C11" H11H 82.0 . . ? H11C C11" H11H 9.6 . . ? H10E C11" H11H 147.3 . . ? H11F C11" H11H 13.0 . . ? H11G C11" H11H 109.5 . . ? C8 C11" H11I 109.4 . . ? H11A C11" H11I 158.8 . . ? H11C C11" H11I 119.0 . . ? H10E C11" H11I 58.1 . . ? H11F C11" H11I 116.5 . . ? H11G C11" H11I 109.5 . . ? H11H C11" H11I 109.5 . . ? C8 C10" H9A 99.8 . . ? C8 C10" H9B 109.1 . . ? H9A C10" H9B 89.3 . . ? C8 C10" H9'B 63.8 . . ? H9A C10" H9'B 72.3 . . ? H9B C10" H9'B 53.0 . . ? C8 C10" H10D 99.0 . . ? H9A C10" H10D 98.5 . . ? H9B C10" H10D 149.1 . . ? H9'B C10" H10D 157.5 . . ? C8 C10" H10F 101.3 . . ? H9A C10" H10F 156.8 . . ? H9B C10" H10F 92.9 . . ? H9'B C10" H10F 126.5 . . ? H10D C10" H10F 68.7 . . ? C8 C10" H10G 112.5 . . ? H9A C10" H10G 45.8 . . ? H9B C10" H10G 122.1 . . ? H9'B C10" H10G 117.4 . . ? H10D C10" H10G 53.6 . . ? H10F C10" H10G 115.7 . . ? C8 C10" H10H 102.3 . . ? H9A C10" H10H 152.4 . . ? H9B C10" H10H 98.7 . . ? H9'B C10" H10H 133.0 . . ? H10D C10" H10H 62.0 . . ? H10F C10" H10H 6.8 . . ? H10G C10" H10H 109.5 . . ? C8 C10" H10I 113.4 . . ? H9A C10" H10I 75.9 . . ? H9B C10" H10I 13.6 . . ? H9'B C10" H10I 51.5 . . ? H10D C10" H10I 147.6 . . ? H10F C10" H10I 104.2 . . ? H10G C10" H10I 109.5 . . ? H10H C10" H10I 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 C14 108.7(7) . . ? O4 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? O4 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N13 C14 C13 111.0(8) . . ? N13 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? N13 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? O1 C15 N13 121.8(8) . . ? O1 C15 C16 117.5(8) . . ? N13 C15 C16 120.7(9) . . ? O1 C15 Yb1 36.2(4) . . ? N13 C15 Yb1 155.1(6) . . ? C16 C15 Yb1 82.2(6) . . ? N1 C16 C17 121.1(8) . . ? N1 C16 C15 113.0(8) . . ? C17 C16 C15 126.0(9) . . ? C18 C17 C16 118.5(8) . . ? C18 C17 H17A 120.7 . . ? C16 C17 H17A 120.7 . . ? C17 C18 C19 121.0(8) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C18 C19 C20 117.3(8) . . ? C18 C19 H19A 121.4 . . ? C20 C19 H19A 121.4 . . ? N1 C20 C19 123.2(8) . . ? N1 C20 C21 115.1(8) . . ? C19 C20 C21 121.7(8) . . ? N4 C21 N10 124.6(8) . . ? N4 C21 C20 116.7(8) . . ? N10 C21 C20 118.8(9) . . ? N10 C22 C23 117.2(8) . . ? N10 C22 C24 120.5(9) . . ? C23 C22 C24 122.3(10) . . ? N7 C23 C22 120.5(8) . . ? N7 C23 C30 114.3(8) . . ? C22 C23 C30 125.1(9) . . ? C29 C24 C25 119.1(9) . . ? C29 C24 C22 124.4(9) . . ? C25 C24 C22 116.5(9) . . ? C24 C25 C26 120.3(10) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C27 C26 C25 121.0(10) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C26 C27 C28 118.9(10) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.5 . . ? C27 C28 C29 119.9(10) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C24 C29 C28 120.7(10) . . ? C24 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C35 C30 C31 118.7(9) . . ? C35 C30 C23 121.5(9) . . ? C31 C30 C23 119.8(9) . . ? C32 C31 C30 120.3(9) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C31 C32 C33 119.2(10) . . ? C31 C32 H32A 120.4 . . ? C33 C32 H32A 120.4 . . ? C32 C33 C34 120.9(10) . . ? C32 C33 H33A 119.6 . . ? C34 C33 H33A 119.6 . . ? C35 C34 C33 120.1(9) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C30 120.8(9) . . ? C34 C35 H35A 119.6 . . ? C30 C35 H35A 119.6 . . ? C41 C36 C37 118.6(10) . . ? C41 C36 C1 119.1(9) . . ? C37 C36 C1 122.2(9) . . ? C36 C37 C38 123.3(10) . . ? C36 C37 H37A 118.4 . . ? C38 C37 H37A 118.4 . . ? C39 C38 C37 115.7(10) . . ? C39 C38 C42 122.3(10) . . ? C37 C38 C42 121.8(11) . . ? C38 C39 C40 124.4(11) . . ? C38 C39 H39A 117.8 . . ? C40 C39 H39A 117.8 . . ? C41 C40 C39 115.0(11) . . ? C41 C40 C46 123.4(13) . . ? C39 C40 C46 121.6(13) . . ? C36 C41 O5 119.5(10) . . ? C36 C41 C40 123.1(11) . . ? O5 C41 C40 117.2(11) . . ? C44' C42 C45 140(2) . . ? C44' C42 C38 108.4(16) . . ? C45 C42 C38 105.3(12) . . ? C44' C42 C43 72.7(18) . . ? C45 C42 C43 112.9(15) . . ? C38 C42 C43 112.5(12) . . ? C44' C42 C43' 108(2) . . ? C45 C42 C43' 77.8(17) . . ? C38 C42 C43' 112.3(15) . . ? C43 C42 C43' 37.4(14) . . ? C44' C42 C44 33.5(14) . . ? C45 C42 C44 113.8(15) . . ? C38 C42 C44 109.3(10) . . ? C43 C42 C44 103.1(14) . . ? C43' C42 C44 131.5(17) . . ? C44' C42 C45' 113(2) . . ? C45 C42 C45' 30.2(12) . . ? C38 C42 C45' 115.0(13) . . ? C43 C42 C45' 126.3(15) . . ? C43' C42 C45' 100.0(18) . . ? C44 C42 C45' 83.8(14) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C43' H43D 109.5 . . ? C42 C43' H43E 109.5 . . ? H43D C43' H43E 109.5 . . ? C42 C43' H43F 109.5 . . ? H43D C43' H43F 109.5 . . ? H43E C43' H43F 109.5 . . ? C42 C44' H44D 109.5 . . ? C42 C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C42 C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? C42 C45' H45D 109.5 . . ? C42 C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? C42 C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? C40 C46 H46A 109.5 . . ? C40 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C40 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O5 C47 C48 107.2(8) . . ? O5 C47 H47A 110.3 . . ? C48 C47 H47A 110.3 . . ? O5 C47 H47B 110.3 . . ? C48 C47 H47B 110.3 . . ? H47A C47 H47B 108.5 . . ? N14 C48 C47 109.7(9) . . ? N14 C48 H48A 109.7 . . ? C47 C48 H48A 109.7 . . ? N14 C48 H48B 109.7 . . ? C47 C48 H48B 109.7 . . ? H48A C48 H48B 108.2 . . ? O2 C49 N14 123.4(9) . . ? O2 C49 C50 119.3(10) . . ? N14 C49 C50 117.2(10) . . ? O2 C49 Yb1 38.0(5) . . ? N14 C49 Yb1 158.4(7) . . ? C50 C49 Yb1 82.0(6) . . ? N2 C50 C51 121.0(9) . . ? N2 C50 C49 112.6(9) . . ? C51 C50 C49 126.3(11) . . ? C52 C51 C50 119.5(9) . . ? C52 C51 H51A 120.3 . . ? C50 C51 H51A 120.3 . . ? C53 C52 C51 119.0(9) . . ? C53 C52 H52A 120.5 . . ? C51 C52 H52A 120.5 . . ? C52 C53 C54 119.3(9) . . ? C52 C53 H53A 120.3 . . ? C54 C53 H53A 120.3 . . ? N2 C54 C53 122.2(9) . . ? N2 C54 C55 114.8(9) . . ? C53 C54 C55 123.0(10) . . ? N5 C55 N11 125.2(9) . . ? N5 C55 C54 118.2(9) . . ? N11 C55 C54 116.6(10) . . ? N11 C56 C57 118.1(9) . . ? N11 C56 C58 118.1(10) . . ? C57 C56 C58 123.8(11) . . ? N8 C57 C56 121.0(9) . . ? N8 C57 C64 116.1(9) . . ? C56 C57 C64 122.9(11) . . ? C63 C58 C59 119.2(10) . . ? C63 C58 C56 122.9(11) . . ? C59 C58 C56 117.8(11) . . ? C60 C59 C58 120.8(11) . . ? C60 C59 H59A 119.6 . . ? C58 C59 H59A 119.6 . . ? C61 C60 C59 119.5(13) . . ? C61 C60 H60A 120.2 . . ? C59 C60 H60A 120.2 . . ? C60 C61 C62 119.8(12) . . ? C60 C61 H61A 120.1 . . ? C62 C61 H61A 120.1 . . ? C61 C62 C63 121.3(12) . . ? C61 C62 H62A 119.3 . . ? C63 C62 H62A 119.3 . . ? C58 C63 C62 119.2(11) . . ? C58 C63 H63A 120.4 . . ? C62 C63 H63A 120.4 . . ? C69 C64 C65 120.1(11) . . ? C69 C64 C57 119.0(10) . . ? C65 C64 C57 120.9(12) . . ? C66 C65 C64 121.2(12) . . ? C66 C65 H65A 119.4 . . ? C64 C65 H65A 119.4 . . ? C67 C66 C65 118.9(12) . . ? C67 C66 H66A 120.5 . . ? C65 C66 H66A 120.5 . . ? C66 C67 C68 122.3(12) . . ? C66 C67 H67A 118.8 . . ? C68 C67 H67A 118.9 . . ? C67 C68 C69 118.0(12) . . ? C67 C68 H68A 121.0 . . ? C69 C68 H68A 121.0 . . ? C64 C69 C68 119.4(12) . . ? C64 C69 H69A 120.3 . . ? C68 C69 H69A 120.3 . . ? C71 C70 C75 117.2(9) . . ? C71 C70 C1 123.2(9) . . ? C75 C70 C1 119.5(9) . . ? C70 C71 C72 122.5(9) . . ? C70 C71 H71A 118.7 . . ? C72 C71 H71A 118.7 . . ? C73 C72 C71 117.7(8) . . ? C73 C72 C76 120.1(9) . . ? C71 C72 C76 122.1(9) . . ? C72 C73 C74 122.0(9) . . ? C72 C73 H73A 119.0 . . ? C74 C73 H73A 119.0 . . ? C75 C74 C73 118.2(9) . . ? C75 C74 C80 120.3(9) . . ? C73 C74 C80 121.5(9) . . ? C74 C75 C70 122.1(9) . . ? C74 C75 O6 119.9(9) . . ? C70 C75 O6 117.8(9) . . ? C77 C76 C78 115.7(13) . . ? C77 C76 C72 107.1(11) . . ? C78 C76 C72 114.2(11) . . ? C77 C76 C79' 140.7(15) . . ? C78 C76 C79' 56.5(12) . . ? C72 C76 C79' 110.7(13) . . ? C77 C76 C77' 41.4(11) . . ? C78 C76 C77' 131.8(14) . . ? C72 C76 C77' 113.5(12) . . ? C79' C76 C77' 110.7(13) . . ? C77 C76 C78' 69.8(12) . . ? C78 C76 C78' 51.4(11) . . ? C72 C76 C78' 109.2(12) . . ? C79' C76 C78' 106.5(12) . . ? C77' C76 C78' 105.9(12) . . ? C77 C76 C79 105.9(12) . . ? C78 C76 C79 105.9(12) . . ? C72 C76 C79 107.4(9) . . ? C79' C76 C79 52.4(11) . . ? C77' C76 C79 64.9(11) . . ? C78' C76 C79 142.7(13) . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C76 C79 H79A 109.5 . . ? C76 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C76 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C76 C77' H77D 109.5 . . ? C76 C77' H77E 109.5 . . ? H77D C77' H77E 109.5 . . ? C76 C77' H77F 109.5 . . ? H77D C77' H77F 109.5 . . ? H77E C77' H77F 109.5 . . ? C76 C78' H78D 109.5 . . ? C76 C78' H78E 109.5 . . ? H78D C78' H78E 109.5 . . ? C76 C78' H78F 109.5 . . ? H78D C78' H78F 109.5 . . ? H78E C78' H78F 109.5 . . ? C76 C79' H79D 109.5 . . ? C76 C79' H79E 109.5 . . ? H79D C79' H79E 109.5 . . ? C76 C79' H79F 109.5 . . ? H79D C79' H79F 109.5 . . ? H79E C79' H79F 109.5 . . ? C74 C80 H80A 109.5 . . ? C74 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C74 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O6 C81 C82 107.2(7) . . ? O6 C81 H81A 110.3 . . ? C82 C81 H81A 110.3 . . ? O6 C81 H81B 110.3 . . ? C82 C81 H81B 110.3 . . ? H81A C81 H81B 108.5 . . ? N15 C82 C81 111.3(7) . . ? N15 C82 H82A 109.4 . . ? C81 C82 H82A 109.4 . . ? N15 C82 H82B 109.4 . . ? C81 C82 H82B 109.4 . . ? H82A C82 H82B 108.0 . . ? O3 C83 N15 123.6(8) . . ? O3 C83 C84 118.5(8) . . ? N15 C83 C84 117.9(9) . . ? O3 C83 Yb1 36.2(4) . . ? N15 C83 Yb1 158.6(7) . . ? C84 C83 Yb1 82.7(6) . . ? N3 C84 C85 122.1(8) . . ? N3 C84 C83 111.4(8) . . ? C85 C84 C83 126.5(9) . . ? C84 C85 C86 118.5(9) . . ? C84 C85 H85A 120.8 . . ? C86 C85 H85A 120.8 . . ? C87 C86 C85 120.2(9) . . ? C87 C86 H86A 119.9 . . ? C85 C86 H86A 119.9 . . ? C88 C87 C86 118.0(9) . . ? C88 C87 H87A 121.0 . . ? C86 C87 H87A 121.0 . . ? N3 C88 C87 122.6(8) . . ? N3 C88 C89 115.1(9) . . ? C87 C88 C89 122.3(9) . . ? N6 C89 N12 125.3(8) . . ? N6 C89 C88 116.6(9) . . ? N12 C89 C88 118.1(10) . . ? N12 C90 C91 120.6(8) . . ? N12 C90 C92 116.2(9) . . ? C91 C90 C92 123.2(10) . . ? N9 C91 C90 119.8(8) . . ? N9 C91 C98 113.8(9) . . ? C90 C91 C98 126.5(9) . . ? C93 C92 C97 118.0(9) . . ? C93 C92 C90 120.6(9) . . ? C97 C92 C90 121.4(10) . . ? C92 C93 C94 121.7(10) . . ? C92 C93 H93A 119.1 . . ? C94 C93 H93A 119.2 . . ? C95 C94 C93 119.5(10) . . ? C95 C94 H94A 120.3 . . ? C93 C94 H94A 120.3 . . ? C96 C95 C94 120.6(10) . . ? C96 C95 H95A 119.7 . . ? C94 C95 H95A 119.7 . . ? C95 C96 C97 119.9(10) . . ? C95 C96 H96A 120.0 . . ? C97 C96 H96A 120.0 . . ? C96 C97 C92 120.3(10) . . ? C96 C97 H97A 119.9 . . ? C92 C97 H97A 119.9 . . ? C99 C98 C103 118.5(9) . . ? C99 C98 C91 121.0(10) . . ? C103 C98 C91 120.5(10) . . ? C98 C99 C100 121.3(10) . . ? C98 C99 H99A 119.4 . . ? C100 C99 H99A 119.4 . . ? C101 C100 C99 119.9(11) . . ? C101 C100 H10J 120.1 . . ? C99 C100 H10J 120.1 . . ? C102 C101 C100 119.9(11) . . ? C102 C101 H10K 120.1 . . ? C100 C101 H10K 120.1 . . ? C101 C102 C103 121.2(11) . . ? C101 C102 H10L 119.4 . . ? C103 C102 H10L 119.4 . . ? C102 C103 C98 119.3(10) . . ? C102 C103 H10M 120.4 . . ? C98 C103 H10M 120.4 . . ? O621 Yb2 O30 86.1(6) . . ? O621 Yb2 O31 86.6(7) . . ? O30 Yb2 O31 84.6(3) . . ? O621 Yb2 O711 83.8(6) . . ? O30 Yb2 O711 142.9(3) . . ? O31 Yb2 O711 130.1(3) . . ? O621 Yb2 O732 121.3(7) . . ? O30 Yb2 O732 81.9(2) . . ? O31 Yb2 O732 147.8(3) . . ? O711 Yb2 O732 73.3(3) . . ? O621 Yb2 O702 152.7(6) . . ? O30 Yb2 O702 71.5(3) . . ? O31 Yb2 O702 76.1(3) . . ? O711 Yb2 O702 123.5(3) . . ? O732 Yb2 O702 71.9(3) . . ? O621 Yb2 O712 72.7(6) . . ? O30 Yb2 O712 152.8(3) . . ? O31 Yb2 O712 77.4(3) . . ? O711 Yb2 O712 53.0(3) . . ? O732 Yb2 O712 123.6(3) . . ? O702 Yb2 O712 122.3(3) . . ? O621 Yb2 O721 25.3(7) . . ? O30 Yb2 O721 84.3(4) . . ? O31 Yb2 O721 111.5(5) . . ? O711 Yb2 O721 71.6(4) . . ? O732 Yb2 O721 96.1(5) . . ? O702 Yb2 O721 154.1(4) . . ? O712 Yb2 O721 83.5(4) . . ? O621 Yb2 O701 148.4(6) . . ? O30 Yb2 O701 124.1(3) . . ? O31 Yb2 O701 87.4(3) . . ? O711 Yb2 O701 76.6(3) . . ? O732 Yb2 O701 76.5(3) . . ? O702 Yb2 O701 52.9(3) . . ? O712 Yb2 O701 75.7(3) . . ? O721 Yb2 O701 148.2(4) . . ? O621 Yb2 O722 28.8(7) . . ? O30 Yb2 O722 74.9(5) . . ? O31 Yb2 O722 59.7(6) . . ? O711 Yb2 O722 108.7(5) . . ? O732 Yb2 O722 141.7(5) . . ? O702 Yb2 O722 126.1(5) . . ? O712 Yb2 O722 78.4(5) . . ? O721 Yb2 O722 52.1(6) . . ? O701 Yb2 O722 141.8(5) . . ? O621 Yb2 O731 73.7(7) . . ? O30 Yb2 O731 72.8(3) . . ? O31 Yb2 O731 150.7(3) . . ? O711 Yb2 O731 70.1(3) . . ? O732 Yb2 O731 47.8(3) . . ? O702 Yb2 O731 112.5(3) . . ? O712 Yb2 O731 115.5(3) . . ? O721 Yb2 O731 49.0(5) . . ? O701 Yb2 O731 120.7(3) . . ? O722 Yb2 O731 95.7(6) . . ? O621 Yb2 N720 7.6(7) . . ? O30 Yb2 N720 78.6(4) . . ? O31 Yb2 N720 87.5(5) . . ? O711 Yb2 N720 89.0(5) . . ? O732 Yb2 N720 118.0(5) . . ? O702 Yb2 N720 147.0(5) . . ? O712 Yb2 N720 80.3(4) . . ? O721 Yb2 N720 24.2(5) . . ? O701 Yb2 N720 156.0(4) . . ? O722 Yb2 N720 27.9(7) . . ? O731 Yb2 N720 70.2(5) . . ? C104 O30 Yb2 128.0(6) . . ? C999 O31 Yb2 133.0(9) . . ? O31 C999 H99B 109.5 . . ? O31 C999 H99C 109.5 . . ? H99B C999 H99C 109.5 . . ? O31 C999 H99D 109.5 . . ? H99B C999 H99D 109.5 . . ? H99C C999 H99D 109.5 . . ? O30 C104 H10N 109.5 . . ? O30 C104 H10O 109.5 . . ? H10N C104 H10O 109.5 . . ? O30 C104 H10P 109.5 . . ? H10N C104 H10P 109.5 . . ? H10O C104 H10P 109.5 . . ? O703 N700 O701 125.4(9) . . ? O703 N700 O702 119.8(10) . . ? O701 N700 O702 114.9(9) . . ? O703 N700 Yb2 173.6(7) . . ? O701 N700 Yb2 58.1(5) . . ? O702 N700 Yb2 57.1(5) . . ? N700 O701 Yb2 95.9(6) . . ? N700 O702 Yb2 95.9(6) . . ? O711 N710 O713 124.2(12) . . ? O711 N710 O712 116.6(9) . . ? O713 N710 O712 119.2(12) . . ? O711 N710 Yb2 57.2(5) . . ? O713 N710 Yb2 174.4(8) . . ? O712 N710 Yb2 59.6(5) . . ? N710 O711 Yb2 96.9(7) . . ? N710 O712 Yb2 93.1(6) . . ? N620 O723 N720 35.6(14) . . ? O721 N720 O722 131(3) . . ? O721 N720 O723 121(2) . . ? O722 N720 O723 107(2) . . ? O721 N720 Yb2 63.4(15) . . ? O722 N720 Yb2 67.6(16) . . ? O723 N720 Yb2 168.0(12) . . ? N720 O721 Yb2 92.4(16) . . ? N720 O722 Yb2 84.5(18) . . ? N620 O621 Yb2 133(2) . . ? O622 N620 O621 136(4) . . ? O622 N620 O723 112(3) . . ? O621 N620 O723 110(3) . . ? O622 N620 Yb2 113(3) . . ? O621 N620 Yb2 28.6(17) . . ? O723 N620 Yb2 134(2) . . ? O733 N730 O732 126.7(11) . . ? O733 N730 O634 90.6(14) . . ? O732 N730 O634 138.3(12) . . ? O733 N730 O731 128.8(12) . . ? O732 N730 O731 101.8(9) . . ? O634 N730 O731 54.2(10) . . ? O733 N730 O633 25.8(9) . . ? O732 N730 O633 102.2(12) . . ? O634 N730 O633 109.9(15) . . ? O731 N730 O633 154.6(14) . . ? O733 N730 Yb2 168.6(8) . . ? O732 N730 Yb2 46.4(5) . . ? O634 N730 Yb2 99.4(10) . . ? O731 N730 Yb2 55.6(6) . . ? O633 N730 Yb2 148.5(11) . . ? N730 O732 Yb2 111.0(7) . . ? N730 O731 Yb2 99.1(7) . . ? O801 N800 O803 122.4(9) . . ? O801 N800 O802 119.7(9) . . ? O803 N800 O802 117.9(9) . . ? O813 N810 O811 122.5(11) . . ? O813 N810 O812 118.0(12) . . ? O811 N810 O812 119.4(11) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 18.76 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.032 _refine_diff_density_min -1.037 _refine_diff_density_rms 0.103 data_yb10 _database_code_depnum_ccdc_archive 'CCDC 889304' #TrackingRef 'web_deposit_cif_file_0_GaryGuillet_1349827231.gg22.cif' # # xray code for Yb10 is gg22 # _audit_update_record ; 2012-09-20 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C112 H112 N15 O6 Yb1, 3(NO3), 4.5(C4H10O1), 3(CH4O)' _chemical_formula_sum 'C133 H169 N18 O22.50 Yb' _chemical_formula_weight 2552.90 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 cubic _symmetry_space_group_name_H-M P213 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 23.7722(9) _cell_length_b 23.7722(9) _cell_length_c 23.7722(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13434.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2785 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5372 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8000 _exptl_absorpt_correction_T_max 0.9258 _exptl_absorpt_process_details 'based on measured indexed crystal faces, Bruker SHELXTL v6.14 (Bruker 2008)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5536 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 1 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5536 _reflns_number_gt 4483 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT (Bruker, 2008)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The following restraints were employed in the final refinement model. yb10 adp n200 o200 o220 o210 eadp n100 o100 o120 o110 dfix 1.24 n100 o100 n100 o110 n100 o120 dfix 2.15 o100 o110 o100 o120 o110 o120 dfix 1.24 n200 o200 n200 o210 n200 o220 dfix 2.15 o200 o210 o200 o220 o210 o220 eadp c9 c10 c11 eadp c9' c10' c11' eadp c9" c10" c11" dfix 1.54 c8 c9 c8 c10 c8 c11 dfix 2.54 c9 c10 c9 c11 c10 c11 dfix 1.54 c8 c9' c8 c10' c8 c11' dfix 2.54 c9' c10' c9' c11' c10' c11' dfix 1.54 c8 c9" c8 c10" c8 c11" dfix 2.54 c9" c10" c9" c11" c10" c11" eadp c13 c14 c15 eadp c13' c14' c15' dfix 1.54 c12 c13 c12 c14 c12 c15 dfix 2.54 c13 c14 c13 c15 c14 c15 dfix 1.54 c12 c13' c12 c14' c12 c15' dfix 2.54 c13' c14' c13' c15' c14' c15' ; _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^)+(0.1312P)^2^+0.7417P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.406(17) _refine_ls_number_reflns 5536 _refine_ls_number_parameters 421 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.008 _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 -0.886554(11) -0.113446(11) -0.613446(11) 0.04654(17) Uani 1 3 d S . . O1 O -0.95542(18) -0.01616(19) -0.41347(19) 0.0467(10) Uani 1 1 d . . . O2 O -0.8679(2) -0.0504(2) -0.5437(2) 0.0510(11) Uani 1 1 d . . . N1 N -0.8399(2) -0.1553(3) -0.5305(2) 0.0496(12) Uani 1 1 d . . . N2 N -0.8658(2) -0.2173(2) -0.6183(2) 0.0479(11) Uani 1 1 d . . . N3 N -0.8686(2) -0.2439(2) -0.6683(3) 0.0494(13) Uani 1 1 d . . . N4 N -0.8282(3) -0.2986(3) -0.5749(3) 0.0576(15) Uani 1 1 d . . . N5 N -0.8441(3) -0.0264(3) -0.4548(3) 0.0560(14) Uani 1 1 d . . . C1 C -1.0470(3) 0.0470(3) -0.4530(3) 0.044(2) Uani 1 3 d S . . H1A H -1.0227 0.0227 -0.4773 0.053 Uiso 1 3 calc SR . . C2 C -1.0470(3) 0.0193(3) -0.3947(3) 0.0455(14) Uani 1 1 d . . . C3 C -1.0016(3) -0.0139(3) -0.3790(3) 0.0479(14) Uani 1 1 d . . . C4 C -1.0051(3) -0.0454(3) -0.3281(3) 0.0514(15) Uani 1 1 d . A . C5 C -1.0490(3) -0.0368(3) -0.2941(3) 0.0545(16) Uani 1 1 d . . . H5A H -1.0493 -0.0561 -0.2591 0.065 Uiso 1 1 calc R . . C6 C -1.0957(3) -0.0008(3) -0.3065(3) 0.0552(17) Uani 1 1 d . B . C7 C -1.0932(3) 0.0248(3) -0.3588(3) 0.0464(14) Uani 1 1 d . . . H7A H -1.1242 0.0470 -0.3708 0.056 Uiso 1 1 calc R . . C8 C -0.9596(3) -0.0905(3) -0.3104(3) 0.0629(19) Uani 1 1 d D . . C9 C -0.9210(12) -0.1146(13) -0.3576(10) 0.089(4) Uiso 0.50 1 d PD A 1 H9A H -0.8952 -0.0852 -0.3706 0.133 Uiso 0.50 1 calc PR A 1 H9B H -0.9443 -0.1275 -0.3891 0.133 Uiso 0.50 1 calc PR A 1 H9C H -0.8993 -0.1464 -0.3427 0.133 Uiso 0.50 1 calc PR A 1 C10 C -0.9861(9) -0.1400(8) -0.2778(9) 0.089(4) Uiso 0.50 1 d PD A 1 H10A H -0.9765 -0.1369 -0.2378 0.133 Uiso 0.50 1 calc PR A 1 H10B H -0.9717 -0.1756 -0.2926 0.133 Uiso 0.50 1 calc PR A 1 H10C H -1.0271 -0.1389 -0.2821 0.133 Uiso 0.50 1 calc PR A 1 C11 C -0.9201(9) -0.0560(9) -0.2696(9) 0.089(4) Uiso 0.50 1 d PD A 1 H11A H -0.9050 -0.0232 -0.2895 0.133 Uiso 0.50 1 calc PR A 1 H11B H -0.8890 -0.0800 -0.2570 0.133 Uiso 0.50 1 calc PR A 1 H11C H -0.9418 -0.0434 -0.2369 0.133 Uiso 0.50 1 calc PR A 1 C9' C -0.9498(13) -0.1346(11) -0.3578(9) 0.063(4) Uiso 0.25 1 d PD A 2 H9'A H -0.9247 -0.1187 -0.3864 0.095 Uiso 0.25 1 calc PR A 2 H9'B H -0.9859 -0.1444 -0.3751 0.095 Uiso 0.25 1 calc PR A 2 H9'C H -0.9326 -0.1684 -0.3418 0.095 Uiso 0.25 1 calc PR A 2 C10' C -0.9741(13) -0.1217(12) -0.2551(9) 0.063(4) Uiso 0.25 1 d PD A 2 H10D H -0.9597 -0.1002 -0.2230 0.095 Uiso 0.25 1 calc PR A 2 H10E H -0.9568 -0.1591 -0.2555 0.095 Uiso 0.25 1 calc PR A 2 H10F H -1.0150 -0.1255 -0.2519 0.095 Uiso 0.25 1 calc PR A 2 C11' C -0.9040(10) -0.0571(11) -0.3035(12) 0.063(4) Uiso 0.25 1 d PD A 2 H11D H -0.9078 -0.0203 -0.3216 0.095 Uiso 0.25 1 calc PR A 2 H11E H -0.8731 -0.0780 -0.3212 0.095 Uiso 0.25 1 calc PR A 2 H11F H -0.8959 -0.0520 -0.2634 0.095 Uiso 0.25 1 calc PR A 2 C9" C -0.9169(12) -0.1096(15) -0.3555(11) 0.044(3) Uiso 0.25 1 d PD A 3 H9"A H -0.8924 -0.0779 -0.3655 0.067 Uiso 0.25 1 calc PR A 3 H9"B H -0.9372 -0.1224 -0.3891 0.067 Uiso 0.25 1 calc PR A 3 H9"C H -0.8940 -0.1405 -0.3407 0.067 Uiso 0.25 1 calc PR A 3 C10" C -0.9986(9) -0.1460(9) -0.3017(10) 0.044(3) Uiso 0.25 1 d PD A 3 H10G H -1.0202 -0.1531 -0.3361 0.067 Uiso 0.25 1 calc PR A 3 H10H H -1.0245 -0.1398 -0.2703 0.067 Uiso 0.25 1 calc PR A 3 H10I H -0.9747 -0.1785 -0.2936 0.067 Uiso 0.25 1 calc PR A 3 C11" C -0.9325(10) -0.0806(11) -0.2530(7) 0.044(3) Uiso 0.25 1 d PD A 3 H11G H -0.9088 -0.0469 -0.2546 0.067 Uiso 0.25 1 calc PR A 3 H11H H -0.9094 -0.1132 -0.2428 0.067 Uiso 0.25 1 calc PR A 3 H11I H -0.9620 -0.0753 -0.2246 0.067 Uiso 0.25 1 calc PR A 3 C12 C -1.1450(3) 0.0089(3) -0.2669(3) 0.0631(19) Uiso 1 1 d D . . C13 C -1.1480(11) 0.0702(5) -0.2516(9) 0.068(3) Uiso 0.50 1 d PD B 1 H13A H -1.1495 0.0929 -0.2860 0.102 Uiso 0.50 1 calc PR B 1 H13B H -1.1146 0.0806 -0.2298 0.102 Uiso 0.50 1 calc PR B 1 H13C H -1.1819 0.0771 -0.2291 0.102 Uiso 0.50 1 calc PR B 1 C14 C -1.2001(9) -0.0067(9) -0.3002(9) 0.068(3) Uiso 0.50 1 d PD B 1 H14A H -1.2035 0.0176 -0.3333 0.102 Uiso 0.50 1 calc PR B 1 H14B H -1.2329 -0.0014 -0.2758 0.102 Uiso 0.50 1 calc PR B 1 H14C H -1.1982 -0.0461 -0.3122 0.102 Uiso 0.50 1 calc PR B 1 C15 C -1.1440(8) -0.0310(7) -0.2135(7) 0.068(3) Uiso 0.50 1 d PD B 1 H15A H -1.1382 -0.0700 -0.2255 0.102 Uiso 0.50 1 calc PR B 1 H15B H -1.1799 -0.0281 -0.1934 0.102 Uiso 0.50 1 calc PR B 1 H15C H -1.1133 -0.0196 -0.1884 0.102 Uiso 0.50 1 calc PR B 1 C13' C -1.1543(12) 0.0752(6) -0.2628(10) 0.077(4) Uiso 0.50 1 d PD B 2 H13D H -1.1543 0.0914 -0.3007 0.115 Uiso 0.50 1 calc PR B 2 H13E H -1.1238 0.0920 -0.2407 0.115 Uiso 0.50 1 calc PR B 2 H13F H -1.1904 0.0829 -0.2445 0.115 Uiso 0.50 1 calc PR B 2 C14' C -1.1986(9) -0.0156(10) -0.2910(10) 0.077(4) Uiso 0.50 1 d PD B 2 H14D H -1.2084 0.0043 -0.3258 0.115 Uiso 0.50 1 calc PR B 2 H14E H -1.2291 -0.0114 -0.2637 0.115 Uiso 0.50 1 calc PR B 2 H14F H -1.1929 -0.0556 -0.2992 0.115 Uiso 0.50 1 calc PR B 2 C15' C -1.1323(9) -0.0121(8) -0.2070(7) 0.077(4) Uiso 0.50 1 d PD B 2 H15D H -1.1144 0.0180 -0.1853 0.115 Uiso 0.50 1 calc PR B 2 H15E H -1.1069 -0.0446 -0.2089 0.115 Uiso 0.50 1 calc PR B 2 H15F H -1.1674 -0.0233 -0.1885 0.115 Uiso 0.50 1 calc PR B 2 C16 C -0.9153(3) 0.0274(3) -0.4049(3) 0.0502(15) Uani 1 1 d . . . H16A H -0.8953 0.0213 -0.3689 0.060 Uiso 1 1 calc R . . H16B H -0.9346 0.0643 -0.4029 0.060 Uiso 1 1 calc R . . C17 C -0.8743(3) 0.0274(3) -0.4521(3) 0.0547(16) Uani 1 1 d . . . H17A H -0.8944 0.0339 -0.4880 0.066 Uiso 1 1 calc R . . H17B H -0.8470 0.0585 -0.4468 0.066 Uiso 1 1 calc R . . C18 C -0.8467(3) -0.0619(3) -0.4963(3) 0.0490(14) Uani 1 1 d . . . C19 C -0.8261(3) -0.1215(3) -0.4872(3) 0.0550(17) Uani 1 1 d . . . C20 C -0.7977(4) -0.1399(4) -0.4390(4) 0.072(2) Uani 1 1 d . . . H20A H -0.7901 -0.1156 -0.4082 0.087 Uiso 1 1 calc R . . C21 C -0.7818(7) -0.1949(5) -0.4388(4) 0.113(5) Uani 1 1 d . . . H21A H -0.7593 -0.2086 -0.4088 0.136 Uiso 1 1 calc R . . C22 C -0.7973(5) -0.2309(4) -0.4808(4) 0.080(3) Uani 1 1 d . . . H22A H -0.7888 -0.2699 -0.4786 0.096 Uiso 1 1 calc R . . C23 C -0.8256(4) -0.2090(3) -0.5269(3) 0.0568(17) Uani 1 1 d . . . C24 C -0.8402(3) -0.2436(3) -0.5764(3) 0.0508(15) Uani 1 1 d . . . C25 C -0.8362(3) -0.3267(3) -0.6221(4) 0.0585(18) Uani 1 1 d . . . C26 C -0.8500(3) -0.2964(3) -0.6718(3) 0.0529(16) Uani 1 1 d . . . C27 C -0.8428(3) -0.3200(3) -0.7303(3) 0.0562(17) Uani 1 1 d . . . C28 C -0.8841(4) -0.3093(3) -0.7707(4) 0.072(2) Uani 1 1 d . . . H28A H -0.9166 -0.2878 -0.7619 0.087 Uiso 1 1 calc R . . C29 C -0.8761(5) -0.3308(4) -0.8233(4) 0.087(3) Uani 1 1 d . . . H29A H -0.9060 -0.3273 -0.8496 0.104 Uiso 1 1 calc R . . C30 C -0.8291(6) -0.3566(5) -0.8406(4) 0.102(4) Uani 1 1 d . . . H30A H -0.8240 -0.3676 -0.8787 0.123 Uiso 1 1 calc R . . C31 C -0.7864(6) -0.3670(5) -0.7984(4) 0.091(3) Uani 1 1 d . . . H31A H -0.7535 -0.3875 -0.8081 0.110 Uiso 1 1 calc R . . C32 C -0.7930(4) -0.3470(4) -0.7435(3) 0.065(2) Uani 1 1 d . . . H32A H -0.7642 -0.3518 -0.7161 0.078 Uiso 1 1 calc R . . C33 C -0.8328(3) -0.3895(3) -0.6193(3) 0.0613(17) Uani 1 1 d . . . C34 C -0.8675(4) -0.4233(4) -0.6525(5) 0.086(3) Uani 1 1 d . . . H34A H -0.8924 -0.4078 -0.6797 0.103 Uiso 1 1 calc R . . C35 C -0.8637(6) -0.4793(4) -0.6437(7) 0.117(5) Uani 1 1 d . . . H35A H -0.8879 -0.5027 -0.6653 0.141 Uiso 1 1 calc R . . C36 C -0.8289(6) -0.5051(4) -0.6072(6) 0.097(3) Uani 1 1 d . . . H36A H -0.8299 -0.5447 -0.6024 0.116 Uiso 1 1 calc R . . C37 C -0.7928(6) -0.4732(5) -0.5778(5) 0.098(4) Uani 1 1 d . . . H37A H -0.7656 -0.4903 -0.5541 0.117 Uiso 1 1 calc R . . C38 C -0.7956(4) -0.4133(4) -0.5823(4) 0.071(2) Uani 1 1 d . . . H38A H -0.7718 -0.3902 -0.5599 0.085 Uiso 1 1 calc R . . N100 N -1.0084(8) -0.3620(7) -0.7417(7) 0.136(3) Uiso 0.70 1 d PD C 1 O100 O -1.0325(7) -0.3484(7) -0.7868(6) 0.136(3) Uiso 0.70 1 d PD C 1 O110 O -1.0052(7) -0.3289(6) -0.7009(6) 0.136(3) Uiso 0.70 1 d PD C 1 O120 O -0.9764(7) -0.4023(6) -0.7377(6) 0.136(3) Uiso 0.70 1 d PD C 1 N200 N -0.9993(12) -0.3210(17) -0.6308(13) 0.142(7) Uiso 0.30 1 d PD D 2 O200 O -0.9640(12) -0.3020(16) -0.5965(14) 0.142(7) Uiso 0.30 1 d PD D 2 O210 O -0.9863(15) -0.3484(17) -0.6741(13) 0.142(7) Uiso 0.30 1 d PD D 2 O220 O -1.0459(11) -0.3328(16) -0.6074(14) 0.142(7) Uiso 0.30 1 d PD D 2 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 0.04654(17) 0.04654(17) 0.04654(17) -0.00023(12) 0.00023(12) 0.00023(12) O1 0.041(2) 0.049(2) 0.049(2) 0.000(2) 0.0025(19) -0.0030(19) O2 0.050(2) 0.052(3) 0.050(3) -0.001(2) -0.002(2) -0.006(2) N1 0.048(3) 0.059(3) 0.042(3) 0.001(2) 0.007(2) 0.004(3) N2 0.044(2) 0.052(3) 0.047(3) -0.002(3) -0.003(2) -0.002(2) N3 0.042(3) 0.038(3) 0.068(4) 0.004(2) -0.007(2) -0.003(2) N4 0.068(4) 0.048(3) 0.057(3) 0.005(3) 0.007(3) 0.016(3) N5 0.052(3) 0.067(4) 0.049(3) -0.007(3) 0.001(3) 0.005(3) C1 0.044(2) 0.044(2) 0.044(2) 0.000(3) 0.000(3) 0.000(3) C2 0.046(3) 0.044(3) 0.046(3) 0.002(3) 0.004(3) -0.005(2) C3 0.044(3) 0.051(3) 0.048(4) -0.010(3) -0.008(3) 0.002(3) C4 0.059(4) 0.044(3) 0.051(4) 0.002(3) -0.006(3) -0.003(3) C5 0.062(4) 0.053(4) 0.049(4) 0.005(3) -0.005(3) -0.004(3) C6 0.053(4) 0.062(4) 0.050(4) -0.002(3) 0.003(3) -0.006(3) C7 0.046(3) 0.045(3) 0.048(3) 0.001(3) 0.002(3) -0.006(3) C8 0.059(4) 0.069(5) 0.060(4) 0.012(4) 0.001(3) 0.006(4) C16 0.047(3) 0.055(4) 0.049(3) -0.011(3) -0.008(3) -0.003(3) C17 0.057(4) 0.049(3) 0.058(4) 0.000(3) 0.002(3) 0.001(3) C18 0.045(3) 0.051(3) 0.051(4) -0.002(3) -0.001(3) 0.005(3) C19 0.054(4) 0.069(5) 0.042(3) -0.006(3) 0.002(3) 0.003(3) C20 0.087(6) 0.078(5) 0.052(4) 0.002(4) -0.012(4) 0.020(5) C21 0.189(13) 0.093(7) 0.057(5) -0.011(5) -0.047(7) 0.053(8) C22 0.107(7) 0.071(5) 0.062(5) 0.006(4) -0.013(5) 0.025(5) C23 0.071(5) 0.057(4) 0.042(3) 0.000(3) 0.005(3) 0.004(4) C24 0.056(4) 0.050(3) 0.047(3) 0.006(3) 0.009(3) 0.007(3) C25 0.054(4) 0.049(4) 0.072(5) 0.012(3) 0.001(4) -0.005(3) C26 0.048(4) 0.042(3) 0.069(4) 0.002(3) -0.003(3) -0.003(3) C27 0.052(4) 0.043(3) 0.074(5) -0.002(3) -0.016(3) -0.002(3) C28 0.069(5) 0.058(4) 0.090(6) -0.006(4) -0.032(5) -0.011(4) C29 0.102(8) 0.081(6) 0.077(6) -0.017(5) -0.044(6) 0.002(6) C30 0.151(11) 0.099(8) 0.056(5) -0.022(5) -0.041(6) -0.007(8) C31 0.131(9) 0.078(6) 0.065(5) -0.002(5) -0.007(6) 0.019(6) C32 0.072(5) 0.069(5) 0.054(4) -0.010(4) -0.009(4) 0.007(4) C33 0.066(4) 0.046(3) 0.072(4) 0.009(4) 0.012(4) 0.009(3) C34 0.076(5) 0.053(4) 0.128(9) 0.019(5) -0.011(6) -0.004(4) C35 0.135(11) 0.049(5) 0.168(13) -0.012(7) -0.027(10) -0.004(6) C36 0.120(9) 0.046(4) 0.125(9) 0.005(6) -0.009(8) 0.007(5) C37 0.108(8) 0.092(7) 0.093(8) 0.038(6) 0.004(7) 0.033(7) C38 0.080(5) 0.063(5) 0.069(5) 0.011(4) 0.002(4) 0.016(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 O2 2.279(5) 7_344 ? Yb1 O2 2.279(5) 10_453 ? Yb1 O2 2.279(5) . ? Yb1 N1 2.472(6) 7_344 ? Yb1 N1 2.472(6) 10_453 ? Yb1 N1 2.472(6) . ? Yb1 N2 2.521(6) . ? Yb1 N2 2.521(6) 7_344 ? Yb1 N2 2.521(6) 10_453 ? Yb1 C18 3.186(7) . ? Yb1 C18 3.186(7) 7_344 ? Yb1 C18 3.186(7) 10_453 ? O1 C3 1.370(8) . ? O1 C16 1.424(8) . ? O2 C18 1.263(8) . ? N1 C23 1.323(10) . ? N1 C19 1.346(9) . ? N2 C24 1.323(9) . ? N2 N3 1.346(8) . ? N3 C26 1.328(9) . ? N4 C25 1.320(10) . ? N4 C24 1.339(9) . ? N5 C18 1.299(9) . ? N5 C17 1.469(9) . ? C1 C2 1.535(7) 10_453 ? C1 C2 1.535(7) 7_344 ? C1 C2 1.535(7) . ? C1 H1A 1.0000 . ? C2 C3 1.390(9) . ? C2 C7 1.396(9) . ? C3 C4 1.423(10) . ? C4 C5 1.336(11) . ? C4 C8 1.582(10) . ? C5 C6 1.432(11) . ? C5 H5A 0.9500 . ? C6 C7 1.386(10) . ? C6 C12 1.521(11) . ? C7 H7A 0.9500 . ? C8 C11" 1.528(15) . ? C8 C10 1.544(14) . ? C8 C9" 1.544(16) . ? C8 C10' 1.547(15) . ? C8 C11' 1.550(16) . ? C8 C9' 1.556(16) . ? C8 C9 1.558(15) . ? C8 C11 1.580(14) . ? C8 C10" 1.626(15) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C9' H9'A 0.9800 . ? C9' H9'B 0.9800 . ? C9' H9'C 0.9800 . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C9" H9"A 0.9800 . ? C9" H9"B 0.9800 . ? C9" H9"C 0.9800 . ? C10" H10G 0.9800 . ? C10" H10H 0.9800 . ? C10" H10I 0.9800 . ? C11" H11G 0.9800 . ? C11" H11H 0.9800 . ? C11" H11I 0.9800 . ? C12 C13 1.504(14) . ? C12 C14' 1.513(15) . ? C12 C15' 1.541(14) . ? C12 C14 1.574(14) . ? C12 C15 1.586(13) . ? C12 C13' 1.593(15) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C13' H13D 0.9800 . ? C13' H13E 0.9800 . ? C13' H13F 0.9800 . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? C15' H15D 0.9800 . ? C15' H15E 0.9800 . ? C15' H15F 0.9800 . ? C16 C17 1.486(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.514(11) . ? C19 C20 1.402(11) . ? C20 C21 1.360(14) . ? C20 H20A 0.9500 . ? C21 C22 1.367(14) . ? C21 H21A 0.9500 . ? C22 C23 1.387(11) . ? C22 H22A 0.9500 . ? C23 C24 1.478(10) . ? C25 C26 1.423(11) . ? C25 C33 1.495(10) . ? C26 C27 1.509(11) . ? C27 C32 1.383(12) . ? C27 C28 1.397(11) . ? C28 C29 1.364(14) . ? C28 H28A 0.9500 . ? C29 C30 1.339(16) . ? C29 H29A 0.9500 . ? C30 C31 1.449(16) . ? C30 H30A 0.9500 . ? C31 C32 1.398(13) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.370(12) . ? C33 C34 1.396(13) . ? C34 C35 1.352(14) . ? C34 H34A 0.9500 . ? C35 C36 1.348(18) . ? C35 H35A 0.9500 . ? C36 C37 1.342(17) . ? C36 H36A 0.9500 . ? C37 C38 1.429(14) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? N100 O120 1.228(14) . ? N100 O110 1.251(13) . ? N100 O100 1.255(13) . ? N200 O200 1.254(15) . ? N200 O210 1.256(15) . ? N200 O220 1.271(18) . ? 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 77.93(19) 7_344 10_453 ? O2 Yb1 O2 77.93(19) 7_344 . ? O2 Yb1 O2 77.93(19) 10_453 . ? O2 Yb1 N1 66.24(19) 7_344 7_344 ? O2 Yb1 N1 73.96(18) 10_453 7_344 ? O2 Yb1 N1 138.03(18) . 7_344 ? O2 Yb1 N1 138.03(18) 7_344 10_453 ? O2 Yb1 N1 66.24(19) 10_453 10_453 ? O2 Yb1 N1 73.96(18) . 10_453 ? N1 Yb1 N1 119.904(14) 7_344 10_453 ? O2 Yb1 N1 73.96(18) 7_344 . ? O2 Yb1 N1 138.03(18) 10_453 . ? O2 Yb1 N1 66.24(19) . . ? N1 Yb1 N1 119.905(14) 7_344 . ? N1 Yb1 N1 119.903(14) 10_453 . ? O2 Yb1 N2 88.97(17) 7_344 . ? O2 Yb1 N2 146.36(17) 10_453 . ? O2 Yb1 N2 129.78(18) . . ? N1 Yb1 N2 72.41(18) 7_344 . ? N1 Yb1 N2 133.00(18) 10_453 . ? N1 Yb1 N2 63.55(19) . . ? O2 Yb1 N2 129.78(18) 7_344 7_344 ? O2 Yb1 N2 88.97(17) 10_453 7_344 ? O2 Yb1 N2 146.36(17) . 7_344 ? N1 Yb1 N2 63.54(19) 7_344 7_344 ? N1 Yb1 N2 72.41(18) 10_453 7_344 ? N1 Yb1 N2 133.00(18) . 7_344 ? N2 Yb1 N2 75.8(2) . 7_344 ? O2 Yb1 N2 146.36(17) 7_344 10_453 ? O2 Yb1 N2 129.78(18) 10_453 10_453 ? O2 Yb1 N2 88.97(18) . 10_453 ? N1 Yb1 N2 133.00(18) 7_344 10_453 ? N1 Yb1 N2 63.54(19) 10_453 10_453 ? N1 Yb1 N2 72.41(18) . 10_453 ? N2 Yb1 N2 75.8(2) . 10_453 ? N2 Yb1 N2 75.8(2) 7_344 10_453 ? O2 Yb1 C18 73.53(18) 7_344 . ? O2 Yb1 C18 94.90(17) 10_453 . ? O2 Yb1 C18 18.77(18) . . ? N1 Yb1 C18 139.62(18) 7_344 . ? N1 Yb1 C18 88.03(18) 10_453 . ? N1 Yb1 C18 47.50(19) . . ? N2 Yb1 C18 111.05(18) . . ? N2 Yb1 C18 156.57(18) 7_344 . ? N2 Yb1 C18 84.12(17) 10_453 . ? O2 Yb1 C18 18.77(18) 7_344 7_344 ? O2 Yb1 C18 73.53(18) 10_453 7_344 ? O2 Yb1 C18 94.91(17) . 7_344 ? N1 Yb1 C18 47.50(19) 7_344 7_344 ? N1 Yb1 C18 139.62(18) 10_453 7_344 ? N1 Yb1 C18 88.03(18) . 7_344 ? N2 Yb1 C18 84.12(17) . 7_344 ? N2 Yb1 C18 111.04(18) 7_344 7_344 ? N2 Yb1 C18 156.57(18) 10_453 7_344 ? C18 Yb1 C18 92.17(17) . 7_344 ? O2 Yb1 C18 94.90(17) 7_344 10_453 ? O2 Yb1 C18 18.77(18) 10_453 10_453 ? O2 Yb1 C18 73.53(18) . 10_453 ? N1 Yb1 C18 88.03(18) 7_344 10_453 ? N1 Yb1 C18 47.50(19) 10_453 10_453 ? N1 Yb1 C18 139.62(18) . 10_453 ? N2 Yb1 C18 156.57(18) . 10_453 ? N2 Yb1 C18 84.12(17) 7_344 10_453 ? N2 Yb1 C18 111.04(18) 10_453 10_453 ? C18 Yb1 C18 92.17(17) . 10_453 ? C18 Yb1 C18 92.17(17) 7_344 10_453 ? C3 O1 C16 115.0(5) . . ? C18 O2 Yb1 125.7(4) . . ? C23 N1 C19 117.7(6) . . ? C23 N1 Yb1 123.7(5) . . ? C19 N1 Yb1 118.5(5) . . ? C24 N2 N3 117.8(6) . . ? C24 N2 Yb1 121.1(4) . . ? N3 N2 Yb1 119.3(4) . . ? C26 N3 N2 118.7(6) . . ? C25 N4 C24 116.2(6) . . ? C18 N5 C17 125.1(6) . . ? C2 C1 C2 112.8(4) 10_453 7_344 ? C2 C1 C2 112.8(4) 10_453 . ? C2 C1 C2 112.8(4) 7_344 . ? C2 C1 H1A 105.9 10_453 . ? C2 C1 H1A 105.9 7_344 . ? C2 C1 H1A 105.9 . . ? C3 C2 C7 120.0(6) . . ? C3 C2 C1 119.1(6) . . ? C7 C2 C1 120.8(6) . . ? O1 C3 C2 118.9(6) . . ? O1 C3 C4 122.4(6) . . ? C2 C3 C4 118.7(6) . . ? C5 C4 C3 118.8(7) . . ? C5 C4 C8 118.4(6) . . ? C3 C4 C8 122.8(6) . . ? C4 C5 C6 124.8(7) . . ? C4 C5 H5A 117.6 . . ? C6 C5 H5A 117.6 . . ? C7 C6 C5 114.5(7) . . ? C7 C6 C12 121.4(7) . . ? C5 C6 C12 124.1(7) . . ? C6 C7 C2 122.7(7) . . ? C6 C7 H7A 118.6 . . ? C2 C7 H7A 118.6 . . ? C11" C8 C10 80.8(12) . . ? C11" C8 C9" 112.9(14) . . ? C10 C8 C9" 113.2(18) . . ? C11" C8 C10' 53.8(13) . . ? C10 C8 C10' 28.0(11) . . ? C9" C8 C10' 126.6(19) . . ? C11" C8 C11' 57.8(14) . . ? C10 C8 C11' 133.3(14) . . ? C9" C8 C11' 70.4(16) . . ? C10' C8 C11' 110.3(13) . . ? C11" C8 C9' 133.5(16) . . ? C10 C8 C9' 85.0(13) . . ? C9" C8 C9' 37.0(16) . . ? C10' C8 C9' 109.0(13) . . ? C11' C8 C9' 107.1(12) . . ? C11" C8 C9 116.9(18) . . ? C10 C8 C9 108.8(12) . . ? C9" C8 C9 6.0(18) . . ? C10' C8 C9 124.5(19) . . ? C11' C8 C9 76.3(14) . . ? C9' C8 C9 31.0(13) . . ? C11" C8 C11 28.4(10) . . ? C10 C8 C11 109.3(11) . . ? C9" C8 C11 100.9(15) . . ? C10' C8 C11 82.0(13) . . ? C11' C8 C11 33.1(12) . . ? C9' C8 C11 134.9(14) . . ? C9 C8 C11 106.5(12) . . ? C11" C8 C4 114.9(11) . . ? C10 C8 C4 111.7(10) . . ? C9" C8 C4 117.6(16) . . ? C10' C8 C4 113.5(13) . . ? C11' C8 C4 105.3(13) . . ? C9' C8 C4 111.5(13) . . ? C9 C8 C4 117.4(15) . . ? C11 C8 C4 102.6(10) . . ? C11" C8 C10" 104.7(11) . . ? C10 C8 C10" 23.8(10) . . ? C9" C8 C10" 103.0(12) . . ? C10' C8 C10" 51.4(13) . . ? C11' C8 C10" 152.7(15) . . ? C9' C8 C10" 68.3(14) . . ? C9 C8 C10" 97.4(15) . . ? C11 C8 C10" 133.1(12) . . ? C4 C8 C10" 101.1(10) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C9' H9'A 109.5 . . ? C8 C9' H9'B 109.5 . . ? H9'A C9' H9'B 109.5 . . ? C8 C9' H9'C 109.5 . . ? H9'A C9' H9'C 109.5 . . ? H9'B C9' H9'C 109.5 . . ? C8 C10' H10D 109.5 . . ? C8 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C8 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C8 C11' H11D 109.5 . . ? C8 C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C8 C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C8 C9" H9"A 109.5 . . ? C8 C9" H9"B 109.5 . . ? H9"A C9" H9"B 109.5 . . ? C8 C9" H9"C 109.5 . . ? H9"A C9" H9"C 109.5 . . ? H9"B C9" H9"C 109.5 . . ? C8 C10" H10G 109.5 . . ? C8 C10" H10H 109.5 . . ? H10G C10" H10H 109.5 . . ? C8 C10" H10I 109.5 . . ? H10G C10" H10I 109.5 . . ? H10H C10" H10I 109.5 . . ? C8 C11" H11G 109.5 . . ? C8 C11" H11H 109.5 . . ? H11G C11" H11H 109.5 . . ? C8 C11" H11I 109.5 . . ? H11G C11" H11I 109.5 . . ? H11H C11" H11I 109.5 . . ? C13 C12 C14' 115.2(16) . . ? C13 C12 C6 109.5(11) . . ? C14' C12 C6 110.9(12) . . ? C13 C12 C15' 95.8(11) . . ? C14' C12 C15' 113.0(11) . . ? C6 C12 C15' 111.8(10) . . ? C13 C12 C14 108.1(11) . . ? C14' C12 C14 11.1(13) . . ? C6 C12 C14 107.2(11) . . ? C15' C12 C14 123.5(12) . . ? C13 C12 C15 112.8(10) . . ? C14' C12 C15 94.9(12) . . ? C6 C12 C15 113.1(9) . . ? C15' C12 C15 20.2(9) . . ? C14 C12 C15 105.8(10) . . ? C13 C12 C13' 11.7(12) . . ? C14' C12 C13' 106.7(11) . . ? C6 C12 C13' 107.1(12) . . ? C15' C12 C13' 107.0(10) . . ? C14 C12 C13' 98.6(14) . . ? C15 C12 C13' 123.0(12) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C13' H13D 109.5 . . ? C12 C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? C12 C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? C12 C14' H14D 109.5 . . ? C12 C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C12 C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C12 C15' H15D 109.5 . . ? C12 C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C12 C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? O1 C16 C17 109.3(5) . . ? O1 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? O1 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? N5 C17 C16 110.7(6) . . ? N5 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? O2 C18 N5 123.7(6) . . ? O2 C18 C19 117.3(6) . . ? N5 C18 C19 118.9(6) . . ? O2 C18 Yb1 35.5(3) . . ? N5 C18 Yb1 158.0(5) . . ? C19 C18 Yb1 82.0(4) . . ? N1 C19 C20 123.7(7) . . ? N1 C19 C18 111.8(6) . . ? C20 C19 C18 124.4(7) . . ? C21 C20 C19 115.9(8) . . ? C21 C20 H20A 122.1 . . ? C19 C20 H20A 122.1 . . ? C20 C21 C22 121.7(9) . . ? C20 C21 H21A 119.2 . . ? C22 C21 H21A 119.2 . . ? C21 C22 C23 118.2(8) . . ? C21 C22 H22A 120.9 . . ? C23 C22 H22A 120.9 . . ? N1 C23 C22 122.6(7) . . ? N1 C23 C24 115.1(6) . . ? C22 C23 C24 122.3(7) . . ? N2 C24 N4 125.4(7) . . ? N2 C24 C23 116.4(6) . . ? N4 C24 C23 118.1(6) . . ? N4 C25 C26 118.8(6) . . ? N4 C25 C33 117.4(7) . . ? C26 C25 C33 123.7(7) . . ? N3 C26 C25 120.0(7) . . ? N3 C26 C27 116.5(7) . . ? C25 C26 C27 123.4(6) . . ? C32 C27 C28 122.0(8) . . ? C32 C27 C26 118.5(6) . . ? C28 C27 C26 119.2(7) . . ? C29 C28 C27 117.7(9) . . ? C29 C28 H28A 121.1 . . ? C27 C28 H28A 121.1 . . ? C30 C29 C28 124.7(9) . . ? C30 C29 H29A 117.7 . . ? C28 C29 H29A 117.7 . . ? C29 C30 C31 116.8(9) . . ? C29 C30 H30A 121.6 . . ? C31 C30 H30A 121.6 . . ? C32 C31 C30 120.7(11) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C27 C32 C31 117.7(9) . . ? C27 C32 H32A 121.1 . . ? C31 C32 H32A 121.1 . . ? C38 C33 C34 120.5(8) . . ? C38 C33 C25 118.4(8) . . ? C34 C33 C25 121.1(7) . . ? C35 C34 C33 116.1(11) . . ? C35 C34 H34A 121.9 . . ? C33 C34 H34A 121.9 . . ? C36 C35 C34 126.1(12) . . ? C36 C35 H35A 117.0 . . ? C34 C35 H35A 117.0 . . ? C37 C36 C35 118.2(10) . . ? C37 C36 H36A 120.9 . . ? C35 C36 H36A 120.9 . . ? C36 C37 C38 119.6(10) . . ? C36 C37 H37A 120.2 . . ? C38 C37 H37A 120.2 . . ? C33 C38 C37 119.3(10) . . ? C33 C38 H38A 120.3 . . ? C37 C38 H38A 120.3 . . ? O120 N100 O110 113.0(14) . . ? O120 N100 O100 123.3(15) . . ? O110 N100 O100 121.9(15) . . ? O200 N200 O210 124(2) . . ? O200 N200 O220 112.3(19) . . ? O210 N200 O220 117(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.434 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.094 data_yb11 _database_code_depnum_ccdc_archive 'CCDC 889305' #TrackingRef 'web_deposit_cif_file_0_GaryGuillet_1349827473.gg2.cif' # # xray code for yb11 is gg2 # _vrf_CHEMW03_I ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: the solvent area, which included two and a half pentane and three ethanol molecules, were removed using Platon/Squeeze. ; _vrf_PLAT201_I ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 26 RESPONSE: All disordered partial atoms were refined isotropically. ; _audit_update_record ; 2012-09-24 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C118 H127 N16 O6 Yb1, 3(CO3F3S), 2.5(C5H12), 3(C2H6O)' _chemical_formula_sum 'C139 H175 F9 N15 O18 S3 Yb' _chemical_formula_weight 2784.16 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.8807(3) _cell_length_b 20.2373(4) _cell_length_c 24.8721(6) _cell_angle_alpha 95.009(2) _cell_angle_beta 101.027(2) _cell_angle_gamma 107.138(1) _cell_volume 6942.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9468 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 28.00 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2914 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7383 _exptl_absorpt_correction_T_max 0.8827 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 125559 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0939 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 31899 _reflns_number_gt 22963 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT (Bruker, 2008)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The following restraints were employed in the final refinement model. yb11 dfix 1.54 c31' c30 c32' c30 c33' c30 dfix 1.54 c25 c26' c25 c27' c25 c28' dfix 2.54 c31' c32' c31' c33' c32' c33' dfix 1.54 c30 c31' c30 c32' c30 c33' c33' c34' dfix 1.54 c33' c34' c33 c34 dfix 2.60 c34' c30 c34 c30 dfix 2.60 c35' c39' eadp c34 c34' eadp c26' c27' c28' c29' As is frequently observed within crystal structures, the triflate anions were heavily disordered requiring restraints to accomodate the roation of both the CF3 and SO3 moieties. Additionally, there was significant disorder in both the tbutyl groups as well as rocking motion within the platform moiety of the structure. Both these disorders required restraints to achieve a proper model. ; _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^)+(0.0504P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 31899 _refine_ls_number_parameters 1365 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.922 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 1.206904(10) 0.434449(7) 0.264427(6) 0.01844(4) Uani 1 1 d . . . O4 O 1.04534(15) 0.40178(11) 0.26422(9) 0.0222(5) Uani 1 1 d . . . O5 O 1.13336(15) 0.35099(11) 0.18690(8) 0.0193(5) Uani 1 1 d . . . O6 O 1.18201(15) 0.33006(11) 0.29875(8) 0.0195(5) Uani 1 1 d . . . N1 N 1.01401(18) 0.30829(13) 0.10928(11) 0.0203(6) Uani 1 1 d . . . H1B H 0.9823 0.3183 0.0791 0.024 Uiso 1 1 calc R . . N2 N 0.91903(19) 0.38256(14) 0.30563(12) 0.0268(6) Uani 1 1 d . . . H2A H 0.8989 0.3958 0.3346 0.032 Uiso 1 1 calc R . . N3 N 1.19914(18) 0.22274(13) 0.30142(11) 0.0199(6) Uani 1 1 d . . . H3A H 1.2384 0.1979 0.2994 0.024 Uiso 1 1 calc R . . N4 N 1.12976(17) 0.47939(13) 0.18560(11) 0.0188(6) Uani 1 1 d . . . N5 N 1.22491(19) 0.56424(13) 0.28065(11) 0.0210(6) Uani 1 1 d . . . N6 N 1.28421(19) 0.60707(13) 0.32614(11) 0.0212(6) Uani 1 1 d . . . N7 N 1.19817(19) 0.66097(14) 0.24106(11) 0.0235(6) Uani 1 1 d . . . N8 N 1.17290(19) 0.46123(13) 0.35588(11) 0.0201(6) Uani 1 1 d . . . N9 N 1.35199(19) 0.48835(13) 0.34260(11) 0.0215(6) Uani 1 1 d . . . N10 N 1.43761(19) 0.51796(14) 0.33049(11) 0.0228(6) Uani 1 1 d . . . N11 N 1.4148(2) 0.54268(14) 0.43624(11) 0.0240(6) Uani 1 1 d . . . N12 N 1.32711(18) 0.37399(13) 0.25219(10) 0.0190(6) Uani 1 1 d . . . N13 N 1.33610(18) 0.49361(13) 0.21473(10) 0.0196(6) Uani 1 1 d . . . N14 N 1.34168(19) 0.55663(13) 0.20034(11) 0.0217(6) Uani 1 1 d . . . N15 N 1.47947(19) 0.49693(14) 0.18500(11) 0.0241(6) Uani 1 1 d . . . C50 C 1.0531(2) 0.12102(16) 0.27679(12) 0.0199(7) Uani 1 1 d . . . H50A H 1.0949 0.0909 0.2768 0.024 Uiso 1 1 calc R . . H50B H 0.9945 0.0957 0.2890 0.024 Uiso 1 1 calc R . . C51 C 1.1067(2) 0.18922(16) 0.31535(13) 0.0209(7) Uani 1 1 d . . . H51A H 1.0670 0.2209 0.3121 0.025 Uiso 1 1 calc R . . H51B H 1.1183 0.1801 0.3541 0.025 Uiso 1 1 calc R . . C52 C 1.2270(2) 0.28781(17) 0.29174(12) 0.0187(7) Uani 1 1 d . . . C53 C 1.3167(2) 0.31221(16) 0.26941(12) 0.0181(6) Uani 1 1 d . . . C54 C 1.3814(2) 0.27567(18) 0.26633(14) 0.0250(7) Uani 1 1 d . . . H54A H 1.3712 0.2313 0.2783 0.030 Uiso 1 1 calc R . . C55 C 1.4613(2) 0.30537(19) 0.24533(15) 0.0311(8) Uani 1 1 d . . . H55A H 1.5081 0.2823 0.2440 0.037 Uiso 1 1 calc R . . C56 C 1.4722(2) 0.36880(18) 0.22639(14) 0.0264(8) Uani 1 1 d . . . H56A H 1.5261 0.3897 0.2114 0.032 Uiso 1 1 calc R . . C57 C 1.4032(2) 0.40139(16) 0.22967(12) 0.0202(7) Uani 1 1 d . . . C58 C 1.4071(2) 0.46832(17) 0.20921(13) 0.0213(7) Uani 1 1 d . . . C59 C 1.4832(2) 0.55792(17) 0.16779(13) 0.0235(7) Uani 1 1 d . . . C60 C 1.4141(2) 0.59032(17) 0.17896(13) 0.0225(7) Uani 1 1 d . . . C61 C 1.55984(14) 0.58690(12) 0.13749(9) 0.0277(8) Uani 1 1 d G . . C62 C 1.54564(13) 0.62801(13) 0.09676(9) 0.0317(8) Uani 1 1 d G . . H62A H 1.4864 0.6378 0.0878 0.038 Uiso 1 1 calc R . . C63 C 1.61818(17) 0.65480(12) 0.06920(9) 0.0370(9) Uani 1 1 d G . . H63A H 1.6085 0.6829 0.0414 0.044 Uiso 1 1 calc R . . C64 C 1.70491(15) 0.64049(13) 0.08237(10) 0.0405(10) Uani 1 1 d G . . H64A H 1.7545 0.6588 0.0635 0.049 Uiso 1 1 calc R . . C65 C 1.71911(13) 0.59938(14) 0.12311(11) 0.0427(10) Uani 1 1 d G . . H65A H 1.7784 0.5896 0.1321 0.051 Uiso 1 1 calc R . . C66 C 1.64657(16) 0.57259(13) 0.15067(9) 0.0383(9) Uani 1 1 d G . . H66A H 1.6563 0.5445 0.1785 0.046 Uiso 1 1 calc R . . C67 C 1.41329(17) 0.6613(1) 0.16846(10) 0.0307(8) Uani 1 1 d G . . C68 C 1.48872(16) 0.72112(14) 0.19467(10) 0.0481(11) Uani 1 1 d G . . H68A H 1.5436 0.7172 0.2192 0.058 Uiso 1 1 calc R . . C69 C 1.4838(2) 0.78673(11) 0.18503(13) 0.0668(15) Uani 1 1 d G . . H69A H 1.5353 0.8276 0.2030 0.080 Uiso 1 1 calc R . . C70 C 1.4034(3) 0.79251(10) 0.14917(13) 0.0677(16) Uani 1 1 d G . . H70A H 1.4000 0.8373 0.1426 0.081 Uiso 1 1 calc R . . C71 C 1.3280(2) 0.73269(15) 0.12295(11) 0.0494(12) Uani 1 1 d G . . H71A H 1.2731 0.7366 0.0984 0.059 Uiso 1 1 calc R . . C72 C 1.33292(16) 0.66708(11) 0.1326(1) 0.0363(9) Uani 1 1 d G . . H72A H 1.2814 0.6262 0.1147 0.044 Uiso 1 1 calc R . . C73 C 0.8052(2) 0.26508(17) 0.28024(17) 0.0323(9) Uani 1 1 d . . . H73A H 0.7745 0.2734 0.3111 0.039 Uiso 1 1 calc R . . H73B H 0.7554 0.2316 0.2498 0.039 Uiso 1 1 calc R . . C74 C 0.8484(2) 0.33294(17) 0.26012(15) 0.0295(8) Uani 1 1 d . . . H74A H 0.8800 0.3243 0.2298 0.035 Uiso 1 1 calc R . . H74B H 0.7968 0.3526 0.2454 0.035 Uiso 1 1 calc R . . C75 C 1.0115(2) 0.40885(16) 0.30595(14) 0.0240(7) Uani 1 1 d . . . C76 C 1.0806(2) 0.44713(16) 0.35970(14) 0.0249(7) Uani 1 1 d . . . C77 C 1.0556(3) 0.46400(19) 0.40887(16) 0.0364(9) Uani 1 1 d . . . H77A H 0.9897 0.4536 0.4105 0.044 Uiso 1 1 calc R . . C78 C 1.1279(3) 0.4961(2) 0.45524(16) 0.0406(10) Uani 1 1 d . . . H78A H 1.1125 0.5086 0.4892 0.049 Uiso 1 1 calc R . . C79 C 1.2236(3) 0.51000(18) 0.45190(15) 0.0331(9) Uani 1 1 d . . . H79A H 1.2746 0.5313 0.4836 0.040 Uiso 1 1 calc R . . C80 C 1.2427(2) 0.49218(16) 0.40161(13) 0.0236(7) Uani 1 1 d . . . C81 C 1.3419(2) 0.50830(16) 0.39294(13) 0.0224(7) Uani 1 1 d . . . C82 C 1.5021(2) 0.56773(16) 0.42588(13) 0.0216(7) Uani 1 1 d . . . C83 C 1.5099(2) 0.56166(17) 0.36920(13) 0.0221(7) Uani 1 1 d . A . C84 C 1.58430(13) 0.59972(11) 0.47375(7) 0.0237(7) Uani 1 1 d G . . C85 C 1.56694(12) 0.62690(12) 0.52259(9) 0.0279(8) Uani 1 1 d G . . H85A H 1.5028 0.6233 0.5251 0.033 Uiso 1 1 calc R . . C86 C 1.64343(16) 0.65941(12) 0.56779(7) 0.0318(8) Uani 1 1 d G . . H86A H 1.6316 0.6780 0.6012 0.038 Uiso 1 1 calc R . . C87 C 1.73729(13) 0.66473(12) 0.56414(7) 0.0339(9) Uani 1 1 d G . . H87A H 1.7896 0.6869 0.5950 0.041 Uiso 1 1 calc R . . C88 C 1.75466(12) 0.63755(13) 0.51531(9) 0.0360(9) Uani 1 1 d G . . H88A H 1.8188 0.6412 0.5128 0.043 Uiso 1 1 calc R . . C89 C 1.67816(15) 0.60504(12) 0.47011(7) 0.0324(8) Uani 1 1 d G . . H89A H 1.6900 0.5865 0.4367 0.039 Uiso 1 1 calc R . . C90 C 1.5914(2) 0.6050(2) 0.34911(14) 0.0295(8) Uani 1 1 d . . . C91 C 1.6234(3) 0.6771(2) 0.36558(17) 0.0414(10) Uani 1 1 d . A . H91A H 1.5942 0.7011 0.3880 0.050 Uiso 0.501(19) 1 calc PR A 1 H91B H 1.5938 0.6938 0.3921 0.050 Uiso 0.499(19) 1 d PR A 2 C92 C 1.7067(9) 0.7113(7) 0.3443(5) 0.056(4) Uiso 0.501(19) 1 d P A 1 H92A H 1.7321 0.7609 0.3523 0.068 Uiso 0.501(19) 1 calc PR A 1 C93 C 1.7507(8) 0.6782(6) 0.3140(4) 0.050(3) Uiso 0.501(19) 1 d P A 1 H93A H 1.8058 0.7044 0.3021 0.060 Uiso 0.501(19) 1 calc PR A 1 C94 C 1.7160(7) 0.6052(7) 0.2997(4) 0.045(3) Uiso 0.501(19) 1 d P A 1 H94A H 1.7472 0.5828 0.2775 0.053 Uiso 0.501(19) 1 calc PR A 1 C95 C 1.6366(6) 0.5646(6) 0.3173(4) 0.028(2) Uiso 0.501(19) 1 d P A 1 H95A H 1.6137 0.5150 0.3094 0.033 Uiso 0.501(19) 1 calc PR A 1 C92' C 1.6909(8) 0.7268(6) 0.3489(5) 0.042(3) Uiso 0.499(19) 1 d P A 2 H92B H 1.7083 0.7749 0.3636 0.050 Uiso 0.499(19) 1 calc PR A 2 C93' C 1.7331(8) 0.7037(7) 0.3095(4) 0.051(3) Uiso 0.499(19) 1 d P A 2 H93B H 1.7779 0.7366 0.2946 0.061 Uiso 0.499(19) 1 calc PR A 2 C94' C 1.7103(7) 0.6335(7) 0.2920(4) 0.047(3) Uiso 0.499(19) 1 d P A 2 H94B H 1.7444 0.6165 0.2683 0.057 Uiso 0.499(19) 1 calc PR A 2 C95' C 1.6342(6) 0.5867(6) 0.3102(3) 0.027(2) Uiso 0.499(19) 1 d P A 2 H95B H 1.6121 0.5390 0.2935 0.033 Uiso 0.499(19) 1 calc PR A 2 C96 C 0.8864(2) 0.19702(16) 0.09907(13) 0.0224(7) Uani 1 1 d . . . H96A H 0.8624 0.1992 0.0595 0.027 Uiso 1 1 calc R . . H96B H 0.8731 0.1472 0.1038 0.027 Uiso 1 1 calc R . . C97 C 0.9934(2) 0.23508(16) 0.11669(14) 0.0223(7) Uani 1 1 d . . . H97A H 1.0171 0.2321 0.1561 0.027 Uiso 1 1 calc R . . H97B H 1.0278 0.2126 0.0943 0.027 Uiso 1 1 calc R . . C98 C 1.0779(2) 0.36037(16) 0.14560(13) 0.0189(7) Uani 1 1 d . . . C99 C 1.0809(2) 0.43398(16) 0.13898(13) 0.0198(7) Uani 1 1 d . . . C100 C 1.0362(2) 0.45492(17) 0.09223(14) 0.0267(8) Uani 1 1 d . . . H10A H 1.0015 0.4220 0.0599 0.032 Uiso 1 1 calc R . . C101 C 1.0435(3) 0.52473(18) 0.09402(15) 0.0294(8) Uani 1 1 d . . . H10B H 1.0156 0.5407 0.0622 0.035 Uiso 1 1 calc R . . C102 C 1.0913(2) 0.57136(18) 0.14202(14) 0.0268(8) Uani 1 1 d . . . H10C H 1.0950 0.6192 0.1443 0.032 Uiso 1 1 calc R . . C103 C 1.1336(2) 0.54636(17) 0.18664(13) 0.0222(7) Uani 1 1 d . . . C104 C 1.1885(2) 0.59321(16) 0.23896(13) 0.0200(7) Uani 1 1 d . . . C105 C 1.2526(2) 0.70430(17) 0.28669(14) 0.0242(7) Uani 1 1 d . . . C106 C 1.3026(2) 0.67587(17) 0.32926(13) 0.0227(7) Uani 1 1 d . . . C107 C 1.25748(18) 0.77871(9) 0.28877(10) 0.0291(8) Uani 1 1 d G . . C108 C 1.24817(18) 0.80501(12) 0.23893(8) 0.0341(9) Uani 1 1 d G . . H10D H 1.2388 0.7755 0.2051 0.041 Uiso 1 1 calc R . . C109 C 1.2526(2) 0.87454(12) 0.23857(10) 0.0464(11) Uani 1 1 d G . . H10E H 1.2462 0.8925 0.2045 0.056 Uiso 1 1 calc R . . C110 C 1.2663(2) 0.91777(9) 0.28805(12) 0.0605(14) Uani 1 1 d G . . H11A H 1.2693 0.9653 0.2878 0.073 Uiso 1 1 calc R . . C111 C 1.2756(2) 0.89147(12) 0.33789(10) 0.0628(15) Uani 1 1 d G . . H11B H 1.2850 0.9210 0.3717 0.075 Uiso 1 1 calc R . . C112 C 1.2712(2) 0.82194(13) 0.33825(8) 0.0445(11) Uani 1 1 d G . . H11C H 1.2776 0.8040 0.3723 0.053 Uiso 1 1 calc R . . C113 C 1.37802(14) 0.71866(11) 0.37832(7) 0.0250(7) Uani 1 1 d G . . C114 C 1.45451(16) 0.77330(12) 0.37068(7) 0.0327(8) Uani 1 1 d G . . H11D H 1.4576 0.7838 0.3345 0.039 Uiso 1 1 calc R . . C115 C 1.52654(14) 0.81257(11) 0.41605(10) 0.0415(10) Uani 1 1 d G . . H11E H 1.5788 0.8499 0.4108 0.050 Uiso 1 1 calc R . . C116 C 1.52208(16) 0.79719(12) 0.46905(8) 0.0423(10) Uani 1 1 d G . . H11F H 1.5713 0.8240 0.5001 0.051 Uiso 1 1 calc R . . C117 C 1.44559(19) 0.74255(12) 0.47669(7) 0.0425(10) Uani 1 1 d G . . H11G H 1.4425 0.7320 0.5129 0.051 Uiso 1 1 calc R . . C118 C 1.37356(15) 0.70328(10) 0.43133(9) 0.0348(9) Uani 1 1 d G . . H11H H 1.3213 0.6659 0.4365 0.042 Uiso 1 1 calc R . . O1 O 1.02688(14) 0.13765(10) 0.22219(8) 0.0190(5) Uani 1 1 d . . . O2 O 0.88269(16) 0.23741(12) 0.2989(1) 0.0303(6) Uani 1 1 d . . . O3 O 0.83820(15) 0.22972(11) 0.13282(10) 0.0254(5) Uani 1 1 d . . . C1 C 0.8335(2) 0.12933(17) 0.20712(13) 0.0215(7) Uani 1 1 d . C . H1A H 0.8865 0.1747 0.2112 0.026 Uiso 1 1 calc R . . C2 C 0.8641(2) 0.07276(16) 0.17760(13) 0.0203(7) Uani 1 1 d . . . C3 C 0.9626(2) 0.08043(15) 0.18424(13) 0.0176(6) Uani 1 1 d . . . C4 C 0.9941(2) 0.03426(16) 0.15354(13) 0.0202(7) Uani 1 1 d . . . C5 C 0.9231(2) -0.02545(17) 0.12195(14) 0.0247(7) Uani 1 1 d . . . H5A H 0.9432 -0.0595 0.1031 0.030 Uiso 1 1 calc R . . C6 C 0.8245(2) -0.03754(18) 0.11671(14) 0.0263(8) Uani 1 1 d . B . C7 C 0.7973(2) 0.01455(17) 0.14334(13) 0.0241(7) Uani 1 1 d . . . H7A H 0.7307 0.0099 0.1378 0.029 Uiso 1 1 calc R . . C14 C 0.7421(2) 0.13773(18) 0.17246(15) 0.0279(8) Uani 1 1 d . . . C15 C 0.7475(2) 0.18726(19) 0.13635(16) 0.0328(9) Uani 1 1 d . C . C20 C 1.0996(2) 0.04426(17) 0.14992(13) 0.0226(7) Uani 1 1 d . . . C21 C 1.1698(2) 0.11927(17) 0.17159(14) 0.0272(8) Uani 1 1 d . . . H21A H 1.1474 0.1524 0.1505 0.041 Uiso 1 1 calc R . . H21B H 1.2346 0.1215 0.1670 0.041 Uiso 1 1 calc R . . H21C H 1.1720 0.1315 0.2109 0.041 Uiso 1 1 calc R . . C22 C 1.1365(3) -0.00624(19) 0.18386(16) 0.0341(9) Uani 1 1 d . . . H22A H 1.0929 -0.0541 0.1708 0.051 Uiso 1 1 calc R . . H22B H 1.1386 0.0067 0.2231 0.051 Uiso 1 1 calc R . . H22C H 1.2015 -0.0034 0.1794 0.051 Uiso 1 1 calc R . . C23 C 1.1038(2) 0.02691(19) 0.08921(14) 0.0303(8) Uani 1 1 d . . . H23A H 1.1716 0.0323 0.0877 0.036 Uiso 1 1 calc R . . H23B H 1.0653 -0.0227 0.0754 0.036 Uiso 1 1 calc R . . C24 C 1.0665(3) 0.0727(2) 0.05038(15) 0.0380(9) Uani 1 1 d . . . H24A H 1.0714 0.0586 0.0126 0.057 Uiso 1 1 calc R . . H24B H 1.1053 0.1219 0.0630 0.057 Uiso 1 1 calc R . . H24C H 0.9988 0.0668 0.0507 0.057 Uiso 1 1 calc R . . C25 C 0.7471(3) -0.10396(19) 0.08289(15) 0.0342(9) Uani 1 1 d D . . C26 C 0.7009(6) -0.0867(4) 0.0294(3) 0.0483(19) Uiso 0.60 1 d P B 1 H26A H 0.6681 -0.0526 0.0371 0.072 Uiso 0.60 1 calc PR B 1 H26B H 0.6537 -0.1294 0.0069 0.072 Uiso 0.60 1 calc PR B 1 H26C H 0.7505 -0.0668 0.0093 0.072 Uiso 0.60 1 calc PR B 1 C27 C 0.7974(5) -0.1608(4) 0.0626(3) 0.0365(17) Uiso 0.60 1 d P B 1 H27A H 0.8440 -0.1661 0.0941 0.055 Uiso 0.60 1 calc PR B 1 H27B H 0.8306 -0.1442 0.0336 0.055 Uiso 0.60 1 calc PR B 1 H27C H 0.7475 -0.2060 0.0479 0.055 Uiso 0.60 1 calc PR B 1 C28 C 0.6788(6) -0.1397(5) 0.1154(3) 0.037(2) Uiso 0.60 1 d P B 1 H28A H 0.6266 -0.1788 0.0905 0.045 Uiso 0.60 1 calc PR B 1 H28B H 0.6489 -0.1063 0.1298 0.045 Uiso 0.60 1 calc PR B 1 C29 C 0.7279(5) -0.1697(4) 0.1659(3) 0.0373(17) Uiso 0.60 1 d P B 1 H29A H 0.6793 -0.1919 0.1860 0.056 Uiso 0.60 1 calc PR B 1 H29B H 0.7794 -0.1314 0.1910 0.056 Uiso 0.60 1 calc PR B 1 H29C H 0.7552 -0.2045 0.1519 0.056 Uiso 0.60 1 calc PR B 1 C26' C 0.6650(8) -0.0805(6) 0.0456(5) 0.0542(18) Uiso 0.40 1 d PD B 2 H26D H 0.6482 -0.0459 0.0682 0.081 Uiso 0.40 1 calc PR B 2 H26E H 0.6076 -0.1215 0.0308 0.081 Uiso 0.40 1 calc PR B 2 H26F H 0.6891 -0.0599 0.0148 0.081 Uiso 0.40 1 calc PR B 2 C27' C 0.7780(9) -0.1477(6) 0.0472(5) 0.0542(18) Uiso 0.40 1 d PD B 2 H27D H 0.7599 -0.1398 0.0089 0.081 Uiso 0.40 1 calc PR B 2 H27E H 0.7469 -0.1968 0.0499 0.081 Uiso 0.40 1 calc PR B 2 H27F H 0.8482 -0.1364 0.0584 0.081 Uiso 0.40 1 calc PR B 2 C28' C 0.6954(11) -0.1470(8) 0.1254(6) 0.0542(18) Uiso 0.40 1 d PD B 2 H28C H 0.6716 -0.1163 0.1483 0.065 Uiso 0.40 1 calc PR B 2 H28D H 0.6392 -0.1867 0.1045 0.065 Uiso 0.40 1 calc PR B 2 C29' C 0.7660(9) -0.1750(7) 0.1635(5) 0.0542(18) Uiso 0.40 1 d P B 2 H29D H 0.7324 -0.2019 0.1888 0.081 Uiso 0.40 1 calc PR B 2 H29E H 0.8207 -0.1357 0.1850 0.081 Uiso 0.40 1 calc PR B 2 H29F H 0.7896 -0.2053 0.1408 0.081 Uiso 0.40 1 calc PR B 2 C16 C 0.6648(6) 0.2080(5) 0.1184(4) 0.034(2) Uiso 0.475(5) 1 d P C 1 C17 C 0.5755(6) 0.1649(4) 0.1271(4) 0.0302(18) Uiso 0.475(5) 1 d P C 1 H17A H 0.5176 0.1728 0.1099 0.036 Uiso 0.475(5) 1 calc PR C 1 C18 C 0.5692(5) 0.1117(4) 0.1596(3) 0.0242(17) Uiso 0.475(5) 1 d P C 1 C19 C 0.6533(5) 0.1017(4) 0.1861(4) 0.0182(19) Uiso 0.475(5) 1 d P C 1 H19A H 0.6522 0.0711 0.2130 0.022 Uiso 0.475(5) 1 calc PR C 1 C35 C 0.6655(6) 0.2681(5) 0.0843(4) 0.032(2) Uiso 0.475(5) 1 d P C 1 C36 C 0.7065(9) 0.2585(7) 0.0332(5) 0.055(4) Uiso 0.475(5) 1 d P C 1 H36A H 0.6962 0.2935 0.0093 0.067 Uiso 0.475(5) 1 calc PR C 1 H36B H 0.7770 0.2679 0.0454 0.067 Uiso 0.475(5) 1 calc PR C 1 C37 C 0.5634(8) 0.2707(6) 0.0594(5) 0.072(3) Uiso 0.475(5) 1 d P C 1 H37A H 0.5684 0.3086 0.0371 0.107 Uiso 0.475(5) 1 calc PR C 1 H37B H 0.5321 0.2790 0.0895 0.107 Uiso 0.475(5) 1 calc PR C 1 H37C H 0.5249 0.2260 0.0359 0.107 Uiso 0.475(5) 1 calc PR C 1 C38 C 0.7217(9) 0.3362(6) 0.1198(5) 0.050(3) Uiso 0.475(5) 1 d P C 1 H38A H 0.7875 0.3361 0.1351 0.076 Uiso 0.475(5) 1 calc PR C 1 H38B H 0.6905 0.3432 0.1502 0.076 Uiso 0.475(5) 1 calc PR C 1 H38C H 0.7242 0.3740 0.0976 0.076 Uiso 0.475(5) 1 calc PR C 1 C39 C 0.6620(8) 0.1870(5) -0.0004(5) 0.066(3) Uiso 0.475(5) 1 d P C 1 H39A H 0.6915 0.1844 -0.0322 0.099 Uiso 0.475(5) 1 calc PR C 1 H39B H 0.5924 0.1778 -0.0136 0.099 Uiso 0.475(5) 1 calc PR C 1 H39C H 0.6730 0.1520 0.0227 0.099 Uiso 0.475(5) 1 calc PR C 1 C40 C 0.4694(5) 0.0681(4) 0.1669(3) 0.0254(17) Uiso 0.475(5) 1 d P C 1 C41 C 0.4287(6) 0.1162(4) 0.1968(3) 0.036(2) Uiso 0.475(5) 1 d P C 1 H41A H 0.4715 0.1364 0.2334 0.053 Uiso 0.475(5) 1 calc PR C 1 H41B H 0.3645 0.0898 0.2012 0.053 Uiso 0.475(5) 1 calc PR C 1 H41C H 0.4237 0.1539 0.1754 0.053 Uiso 0.475(5) 1 calc PR C 1 C42 C 0.4761(6) 0.0108(4) 0.2020(4) 0.0286(19) Uiso 0.475(5) 1 d P C 1 H42A H 0.5212 0.0318 0.2378 0.043 Uiso 0.475(5) 1 calc PR C 1 H42B H 0.4992 -0.0229 0.1827 0.043 Uiso 0.475(5) 1 calc PR C 1 H42C H 0.4121 -0.0132 0.2081 0.043 Uiso 0.475(5) 1 calc PR C 1 C43 C 0.3989(6) 0.0378(4) 0.1096(3) 0.034(2) Uiso 0.475(5) 1 d P C 1 H43A H 0.3879 0.0772 0.0912 0.041 Uiso 0.475(5) 1 calc PR C 1 H43B H 0.3361 0.0091 0.1155 0.041 Uiso 0.475(5) 1 calc PR C 1 C44 C 0.4346(6) -0.0081(5) 0.0696(4) 0.028(2) Uiso 0.475(5) 1 d P C 1 H44A H 0.3863 -0.0251 0.0344 0.043 Uiso 0.475(5) 1 calc PR C 1 H44B H 0.4439 -0.0481 0.0868 0.043 Uiso 0.475(5) 1 calc PR C 1 H44C H 0.4960 0.0201 0.0626 0.043 Uiso 0.475(5) 1 calc PR C 1 C16' C 0.6621(5) 0.1920(4) 0.0988(3) 0.0207(16) Uiso 0.525(5) 1 d P C 2 C17' C 0.5745(5) 0.1448(3) 0.1019(3) 0.0245(15) Uiso 0.525(5) 1 d P C 2 H17B H 0.5172 0.1478 0.0792 0.029 Uiso 0.525(5) 1 calc PR C 2 C18' C 0.5654(5) 0.0937(4) 0.1361(3) 0.0260(16) Uiso 0.525(5) 1 d P C 2 C19' C 0.6501(5) 0.0909(4) 0.1693(3) 0.0222(18) Uiso 0.525(5) 1 d P C 2 H19B H 0.6453 0.0546 0.1915 0.027 Uiso 0.525(5) 1 calc PR C 2 C35' C 0.6642(5) 0.2534(3) 0.0660(3) 0.0175(16) Uiso 0.525(5) 1 d PD C 2 C36' C 0.6946(6) 0.3212(5) 0.1081(4) 0.028(2) Uiso 0.525(5) 1 d P C 2 H36C H 0.7603 0.3279 0.1302 0.034 Uiso 0.525(5) 1 calc PR C 2 H36D H 0.6992 0.3609 0.0869 0.034 Uiso 0.525(5) 1 calc PR C 2 C37' C 0.5646(5) 0.2448(4) 0.0292(3) 0.0314(17) Uiso 0.525(5) 1 d P C 2 H37D H 0.5436 0.2016 0.0025 0.047 Uiso 0.525(5) 1 calc PR C 2 H37E H 0.5690 0.2849 0.0092 0.047 Uiso 0.525(5) 1 calc PR C 2 H37F H 0.5178 0.2424 0.0524 0.047 Uiso 0.525(5) 1 calc PR C 2 C38' C 0.7357(6) 0.2642(5) 0.0281(3) 0.030(2) Uiso 0.525(5) 1 d P C 2 H38D H 0.7184 0.2221 0.0007 0.045 Uiso 0.525(5) 1 calc PR C 2 H38E H 0.8012 0.2732 0.0504 0.045 Uiso 0.525(5) 1 calc PR C 2 H38F H 0.7333 0.3043 0.0091 0.045 Uiso 0.525(5) 1 calc PR C 2 C39' C 0.6312(5) 0.3263(4) 0.1481(3) 0.0319(17) Uiso 0.525(5) 1 d PD C 2 H39D H 0.6588 0.3717 0.1723 0.048 Uiso 0.525(5) 1 calc PR C 2 H39E H 0.6274 0.2886 0.1706 0.048 Uiso 0.525(5) 1 calc PR C 2 H39F H 0.5663 0.3220 0.1272 0.048 Uiso 0.525(5) 1 calc PR C 2 C40' C 0.4655(5) 0.0451(4) 0.1386(3) 0.0355(18) Uiso 0.525(5) 1 d P C 2 C41' C 0.4043(7) 0.0885(5) 0.1528(4) 0.065(3) Uiso 0.525(5) 1 d P C 2 H41D H 0.4008 0.1208 0.1259 0.097 Uiso 0.525(5) 1 calc PR C 2 H41E H 0.4332 0.1153 0.1901 0.097 Uiso 0.525(5) 1 calc PR C 2 H41F H 0.3391 0.0578 0.1517 0.097 Uiso 0.525(5) 1 calc PR C 2 C42' C 0.4717(6) -0.0059(4) 0.1806(3) 0.0327(19) Uiso 0.525(5) 1 d P C 2 H42D H 0.5112 -0.0342 0.1708 0.049 Uiso 0.525(5) 1 calc PR C 2 H42E H 0.4066 -0.0367 0.1797 0.049 Uiso 0.525(5) 1 calc PR C 2 H42F H 0.5011 0.0207 0.2179 0.049 Uiso 0.525(5) 1 calc PR C 2 C43' C 0.4125(8) 0.0038(6) 0.0839(5) 0.063(3) Uiso 0.525(5) 1 d P C 2 H43C H 0.4018 0.0365 0.0579 0.076 Uiso 0.525(5) 1 calc PR C 2 H43D H 0.3483 -0.0257 0.0874 0.076 Uiso 0.525(5) 1 calc PR C 2 C44' C 0.4613(9) -0.0429(7) 0.0589(5) 0.091(4) Uiso 0.525(5) 1 d P C 2 H44D H 0.4211 -0.0677 0.0227 0.137 Uiso 0.525(5) 1 calc PR C 2 H44E H 0.4701 -0.0769 0.0835 0.137 Uiso 0.525(5) 1 calc PR C 2 H44F H 0.5244 -0.0144 0.0543 0.137 Uiso 0.525(5) 1 calc PR C 2 S1 S 0.7310(3) 0.43873(18) 0.3580(2) 0.0331(11) Uiso 0.363(9) 1 d P D 1 O13 O 0.8087(6) 0.4107(5) 0.3772(4) 0.034(2) Uiso 0.363(9) 1 d P D 1 O14 O 0.7455(7) 0.5064(5) 0.3865(5) 0.060(3) Uiso 0.363(9) 1 d P D 1 O15 O 0.6983(8) 0.4256(5) 0.3001(4) 0.041(3) Uiso 0.363(9) 1 d P D 1 C900 C 0.6342(10) 0.3863(7) 0.3780(5) 0.035(3) Uiso 0.363(9) 1 d P D 1 F1 F 0.6465(5) 0.3841(5) 0.4341(3) 0.041(2) Uiso 0.363(9) 1 d P D 1 F2 F 0.6031(6) 0.3199(4) 0.3536(3) 0.043(2) Uiso 0.363(9) 1 d P D 1 F3 F 0.5596(5) 0.4127(5) 0.3649(3) 0.047(2) Uiso 0.363(9) 1 d P D 1 S1' S 0.74824(17) 0.43378(10) 0.37417(13) 0.0310(6) Uiso 0.637(9) 1 d P D 2 F1' F 0.5608(3) 0.3865(3) 0.37356(18) 0.0492(13) Uiso 0.637(9) 1 d P D 2 F2' F 0.6551(3) 0.3584(3) 0.43903(16) 0.0404(12) Uiso 0.637(9) 1 d P D 2 F3' F 0.6252(4) 0.3058(3) 0.35589(19) 0.0480(14) Uiso 0.637(9) 1 d P D 2 O13' O 0.8237(4) 0.4047(3) 0.3931(2) 0.0361(14) Uiso 0.637(9) 1 d P D 2 O14' O 0.7540(3) 0.4968(3) 0.4087(2) 0.0415(14) Uiso 0.637(9) 1 d P D 2 O15' O 0.7256(5) 0.4354(3) 0.3157(3) 0.0491(17) Uiso 0.637(9) 1 d P D 2 C910 C 0.6409(5) 0.3678(4) 0.3864(3) 0.0342(19) Uiso 0.637(9) 1 d P D 2 S3 S 0.36996(19) 0.13152(11) 0.36301(8) 0.0325(5) Uiso 0.541(4) 1 d P E 1 O7 O 0.3432(5) 0.0783(4) 0.3992(3) 0.0637(18) Uiso 0.541(4) 1 d P E 1 O8 O 0.2897(6) 0.1146(4) 0.3119(3) 0.032(2) Uiso 0.541(4) 1 d P E 1 O9 O 0.4026(4) 0.2019(3) 0.3897(2) 0.0501(16) Uiso 0.541(4) 1 d P E 1 F7 F 0.4486(5) 0.0547(4) 0.3114(3) 0.095(2) Uiso 0.541(4) 1 d P E 1 F8 F 0.5025(4) 0.1602(3) 0.3074(3) 0.0793(18) Uiso 0.541(4) 1 d P E 1 F9 F 0.5437(6) 0.1266(4) 0.3844(3) 0.116(3) Uiso 0.541(4) 1 d P E 1 C901 C 0.4766(7) 0.1141(6) 0.3397(5) 0.060(2) Uiso 0.541(4) 1 d P E 1 S3' S 0.3293(2) 0.11493(12) 0.36474(9) 0.0279(6) Uiso 0.459(4) 1 d P E 2 O7' O 0.3024(7) 0.1205(5) 0.3066(4) 0.031(3) Uiso 0.459(4) 1 d P E 2 O8' O 0.2905(6) 0.0495(4) 0.3834(3) 0.057(2) Uiso 0.459(4) 1 d P E 2 O9' O 0.3336(5) 0.1760(4) 0.3999(3) 0.062(2) Uiso 0.459(4) 1 d P E 2 F7' F 0.4608(4) 0.0610(3) 0.3393(3) 0.0469(15) Uiso 0.459(4) 1 d P E 2 F8' F 0.5003(5) 0.1774(4) 0.3479(3) 0.076(2) Uiso 0.459(4) 1 d P E 2 F9' F 0.5057(4) 0.1248(3) 0.4188(3) 0.0594(17) Uiso 0.459(4) 1 d P E 2 C911 C 0.4527(6) 0.1190(4) 0.3662(4) 0.0301(19) Uiso 0.459(4) 1 d P E 2 S2 S 1.0131(3) 0.29637(12) 0.95971(8) 0.0224(7) Uiso 0.623(14) 1 d P F 1 F4 F 0.9786(5) 0.1715(3) 0.9015(2) 0.0487(17) Uiso 0.623(14) 1 d P F 1 F5 F 0.8595(3) 0.2039(3) 0.8946(2) 0.0493(16) Uiso 0.623(14) 1 d P F 1 F6 F 0.9133(5) 0.1652(3) 0.9667(2) 0.0571(17) Uiso 0.623(14) 1 d P F 1 O10 O 1.0312(5) 0.3321(3) 0.9156(2) 0.0377(15) Uiso 0.623(14) 1 d P F 1 O11 O 0.9503(4) 0.3190(3) 0.9893(2) 0.0284(15) Uiso 0.623(14) 1 d P F 1 O12 O 1.0899(5) 0.2863(3) 0.9986(3) 0.0452(19) Uiso 0.623(14) 1 d P F 1 S2' S 0.9913(5) 0.2902(3) 0.96078(17) 0.0400(13) Uiso 0.377(14) 1 d P F 2 O12' O 1.0987(7) 0.2932(5) 0.9864(4) 0.033(3) Uiso 0.377(14) 1 d P F 2 O10' O 0.9947(11) 0.3215(6) 0.9089(5) 0.060(3) Uiso 0.377(14) 1 d P F 2 O11' O 0.9322(7) 0.3079(5) 0.9952(4) 0.027(2) Uiso 0.377(14) 1 d P F 2 F5' F 0.8424(6) 0.1840(5) 0.9110(4) 0.052(3) Uiso 0.377(14) 1 d P F 2 F4' F 0.9434(7) 0.1641(4) 0.9767(3) 0.040(2) Uiso 0.377(14) 1 d P F 2 F6' F 0.9978(7) 0.1841(5) 0.8969(4) 0.045(3) Uiso 0.377(14) 1 d P F 2 C902 C 0.9401(3) 0.2037(2) 0.93157(18) 0.0424(10) Uiso 1 1 d . . . C8 C 0.8247(2) 0.11448(17) 0.26600(14) 0.0233(7) Uani 1 1 d . . . C9 C 0.8535(2) 0.16917(17) 0.31071(15) 0.0281(8) Uani 1 1 d . C . C10 C 0.8607(3) 0.15606(19) 0.36536(16) 0.0348(9) Uani 1 1 d . . . C11 C 0.8304(3) 0.0861(2) 0.37278(16) 0.0380(9) Uani 1 1 d . C . H11I H 0.8333 0.0762 0.4096 0.046 Uiso 1 1 calc R . . C12 C 0.7964(3) 0.03028(18) 0.33003(15) 0.0305(8) Uani 1 1 d . . . C13 C 0.7953(2) 0.04595(18) 0.27645(14) 0.0256(7) Uani 1 1 d . C . H13A H 0.7738 0.0087 0.2462 0.031 Uiso 1 1 calc R . . C30 C 0.9022(3) 0.2120(2) 0.41834(18) 0.0531(12) Uani 1 1 d D C . C31 C 0.9211(6) 0.1838(4) 0.4695(3) 0.059(2) Uiso 0.610(8) 1 d P C 1 H31A H 0.9682 0.1589 0.4677 0.089 Uiso 0.610(8) 1 calc PR C 1 H31B H 0.8609 0.1513 0.4745 0.089 Uiso 0.610(8) 1 calc PR C 1 H31C H 0.9471 0.2221 0.5009 0.089 Uiso 0.610(8) 1 calc PR C 1 C32 C 0.9882(7) 0.2661(5) 0.4137(4) 0.071(3) Uiso 0.610(8) 1 d P C 1 H32A H 1.0404 0.2459 0.4130 0.106 Uiso 0.610(8) 1 calc PR C 1 H32B H 1.0078 0.3034 0.4455 0.106 Uiso 0.610(8) 1 calc PR C 1 H32C H 0.9745 0.2853 0.3794 0.106 Uiso 0.610(8) 1 calc PR C 1 C33 C 0.8259(6) 0.2551(5) 0.4204(4) 0.073(3) Uiso 0.610(8) 1 d PD C 1 H33A H 0.8505 0.2924 0.4531 0.087 Uiso 0.610(8) 1 calc PR C 1 H33B H 0.8179 0.2774 0.3867 0.087 Uiso 0.610(8) 1 calc PR C 1 C34 C 0.7363(8) 0.2084(8) 0.4235(7) 0.126(4) Uiso 0.610(8) 1 d PD C 1 H34A H 0.6895 0.2337 0.4239 0.189 Uiso 0.610(8) 1 calc PR C 1 H34B H 0.7443 0.1876 0.4576 0.189 Uiso 0.610(8) 1 calc PR C 1 H34C H 0.7128 0.1713 0.3913 0.189 Uiso 0.610(8) 1 calc PR C 1 C31' C 0.9968(9) 0.1867(7) 0.4544(6) 0.076(5) Uiso 0.390(8) 1 d PD C 2 H31D H 1.0195 0.1601 0.4281 0.115 Uiso 0.390(8) 1 calc PR C 2 H31E H 0.9738 0.1575 0.4815 0.115 Uiso 0.390(8) 1 calc PR C 2 H31F H 1.0501 0.2284 0.4737 0.115 Uiso 0.390(8) 1 calc PR C 2 C32' C 0.9563(7) 0.2864(4) 0.4130(4) 0.026(2) Uiso 0.390(8) 1 d PD C 2 H32D H 1.0216 0.2893 0.4090 0.039 Uiso 0.390(8) 1 calc PR C 2 H32E H 0.9604 0.3180 0.4462 0.039 Uiso 0.390(8) 1 calc PR C 2 H32F H 0.9220 0.3000 0.3803 0.039 Uiso 0.390(8) 1 calc PR C 2 C33' C 0.8404(8) 0.2017(7) 0.4591(5) 0.077(5) Uiso 0.390(8) 1 d PD C 2 H33C H 0.8765 0.2281 0.4962 0.093 Uiso 0.390(8) 1 calc PR C 2 H33D H 0.8134 0.1516 0.4620 0.093 Uiso 0.390(8) 1 calc PR C 2 C34' C 0.7597(13) 0.2320(13) 0.4329(11) 0.126(4) Uiso 0.390(8) 1 d PD C 2 H34D H 0.7134 0.2285 0.4566 0.189 Uiso 0.390(8) 1 calc PR C 2 H34E H 0.7261 0.2053 0.3960 0.189 Uiso 0.390(8) 1 calc PR C 2 H34F H 0.7889 0.2812 0.4295 0.189 Uiso 0.390(8) 1 calc PR C 2 C45 C 0.7632(3) -0.04637(19) 0.33884(16) 0.0370(9) Uani 1 1 d . C . C46 C 0.7751(3) -0.0540(2) 0.40060(18) 0.0521(12) Uani 1 1 d . . . H46A H 0.7350 -0.0310 0.4170 0.078 Uiso 1 1 calc R C . H46B H 0.8430 -0.0320 0.4199 0.078 Uiso 1 1 calc R . . H46C H 0.7549 -0.1037 0.4043 0.078 Uiso 1 1 calc R . . C47 C 0.8287(4) -0.0835(2) 0.3170(2) 0.0596(13) Uani 1 1 d . . . H47A H 0.8237 -0.0808 0.2775 0.089 Uiso 1 1 calc R C . H47B H 0.8082 -0.1326 0.3223 0.089 Uiso 1 1 calc R . . H47C H 0.8957 -0.0606 0.3374 0.089 Uiso 1 1 calc R . . C48 C 0.6587(3) -0.0820(2) 0.30731(19) 0.0504(11) Uani 1 1 d . . . H48A H 0.6555 -0.0817 0.2672 0.060 Uiso 1 1 calc R C . H48B H 0.6393 -0.1315 0.3133 0.060 Uiso 1 1 calc R . . C49 C 0.5863(3) -0.0495(3) 0.3232(2) 0.0723(17) Uani 1 1 d . C . H49A H 0.5217 -0.0757 0.3007 0.108 Uiso 1 1 calc R . . H49B H 0.6036 -0.0008 0.3166 0.108 Uiso 1 1 calc R . . H49C H 0.5868 -0.0511 0.3625 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01928(7) 0.01731(7) 0.01631(7) 0.00141(5) 0.00294(5) 0.00326(5) O4 0.0204(12) 0.0253(12) 0.0217(12) 0.0027(10) 0.0075(10) 0.0071(10) O5 0.0204(11) 0.0207(12) 0.0141(11) 0.0025(9) 0.0001(9) 0.0048(9) O6 0.0208(11) 0.0199(12) 0.0171(11) 0.0007(9) 0.0033(9) 0.0066(9) N1 0.0194(14) 0.0187(14) 0.0186(14) 0.0026(11) -0.0006(11) 0.0028(11) N2 0.0239(15) 0.0192(15) 0.0360(17) -0.0015(13) 0.0145(13) 0.0017(12) N3 0.0166(13) 0.0171(14) 0.0227(15) 0.0024(11) 0.0012(11) 0.0028(11) N4 0.0161(13) 0.0177(14) 0.0208(14) 0.0025(11) 0.0036(11) 0.0034(11) N5 0.0245(15) 0.0175(14) 0.0192(14) 0.0024(11) 0.0059(11) 0.0035(11) N6 0.0236(14) 0.0184(14) 0.0192(14) 0.0012(11) 0.0045(11) 0.0037(11) N7 0.0242(15) 0.0186(15) 0.0254(16) 0.0030(12) 0.0028(12) 0.0053(12) N8 0.0231(14) 0.0153(13) 0.0184(14) 0.0021(11) 0.0045(11) 0.0012(11) N9 0.0252(15) 0.0206(14) 0.0166(14) 0.0006(11) 0.0040(11) 0.0051(12) N10 0.0252(15) 0.0239(15) 0.0190(14) 0.0025(12) 0.0031(12) 0.0090(12) N11 0.0303(16) 0.0182(14) 0.0183(14) -0.0014(11) 0.0018(12) 0.0035(12) N12 0.0203(14) 0.0198(14) 0.0123(13) -0.0004(11) -0.0008(10) 0.0031(11) N13 0.0183(14) 0.0221(14) 0.0161(13) 0.0048(11) 0.0016(11) 0.0039(11) N14 0.0236(14) 0.0198(14) 0.0179(14) 0.0024(11) 0.0028(11) 0.0026(12) N15 0.0206(14) 0.0288(16) 0.0186(14) 0.0018(12) 0.0040(11) 0.0022(12) C50 0.0169(16) 0.0195(16) 0.0196(17) 0.0043(13) -0.0002(13) 0.0025(13) C51 0.0194(16) 0.0213(17) 0.0184(16) 0.0023(13) 0.0026(13) 0.0025(13) C52 0.0168(16) 0.0238(17) 0.0090(15) -0.0012(13) -0.0042(12) 0.0025(13) C53 0.0175(16) 0.0181(16) 0.0125(15) -0.0009(12) -0.0020(12) 0.0009(13) C54 0.0247(18) 0.0233(18) 0.0268(19) 0.0049(15) 0.0045(14) 0.0076(14) C55 0.0258(19) 0.037(2) 0.034(2) 0.0055(17) 0.0054(16) 0.0166(16) C56 0.0234(18) 0.032(2) 0.0241(18) 0.0027(15) 0.0090(14) 0.0071(15) C57 0.0196(16) 0.0229(17) 0.0137(15) -0.0016(13) 0.0019(12) 0.0026(13) C58 0.0201(17) 0.0245(18) 0.0152(16) 0.0005(13) 0.0013(13) 0.0032(14) C59 0.0236(17) 0.0256(18) 0.0150(16) 0.0004(14) 0.0015(13) 0.0010(14) C60 0.0232(17) 0.0218(17) 0.0165(16) 0.0007(13) 0.0038(13) -0.0004(14) C61 0.0283(19) 0.0291(19) 0.0225(18) 0.0035(15) 0.0075(15) 0.0036(15) C62 0.032(2) 0.034(2) 0.027(2) 0.0061(16) 0.0109(16) 0.0045(16) C63 0.043(2) 0.040(2) 0.031(2) 0.0097(18) 0.0186(18) 0.0094(18) C64 0.041(2) 0.040(2) 0.043(2) 0.0075(19) 0.0271(19) 0.0042(19) C65 0.032(2) 0.052(3) 0.050(3) 0.015(2) 0.0188(19) 0.0135(19) C66 0.032(2) 0.047(2) 0.039(2) 0.0153(19) 0.0144(18) 0.0102(18) C67 0.042(2) 0.0235(19) 0.0274(19) 0.0051(15) 0.0227(17) 0.0024(16) C68 0.055(3) 0.034(2) 0.045(3) 0.000(2) 0.017(2) -0.004(2) C69 0.092(4) 0.026(2) 0.071(4) -0.004(2) 0.041(3) -0.009(2) C70 0.116(5) 0.035(3) 0.074(4) 0.020(3) 0.059(4) 0.029(3) C71 0.082(3) 0.041(3) 0.049(3) 0.020(2) 0.039(2) 0.035(2) C72 0.049(2) 0.031(2) 0.037(2) 0.0117(18) 0.0202(19) 0.0175(18) C73 0.0225(18) 0.0203(18) 0.054(2) 0.0019(17) 0.0138(17) 0.0050(15) C74 0.0218(18) 0.0212(18) 0.041(2) -0.0016(16) 0.0058(16) 0.0024(14) C75 0.0228(17) 0.0148(16) 0.033(2) 0.0027(14) 0.0060(15) 0.0041(14) C76 0.0306(19) 0.0158(17) 0.0284(19) 0.0023(14) 0.0141(15) 0.0032(14) C77 0.035(2) 0.031(2) 0.039(2) -0.0039(17) 0.0193(18) -0.0005(17) C78 0.048(2) 0.041(2) 0.028(2) -0.0024(18) 0.0202(19) 0.0027(19) C79 0.038(2) 0.029(2) 0.0238(19) -0.0025(16) 0.0081(16) -0.0015(16) C80 0.0326(19) 0.0172(17) 0.0209(17) 0.0046(14) 0.0090(14) 0.0055(14) C81 0.0295(18) 0.0154(16) 0.0201(17) 0.0029(13) 0.0041(14) 0.0049(14) C82 0.0271(18) 0.0178(16) 0.0195(17) -0.0001(13) -0.0001(14) 0.0107(14) C83 0.0242(17) 0.0224(17) 0.0196(17) -0.0008(14) 0.0015(14) 0.0106(14) C84 0.0311(19) 0.0190(17) 0.0185(17) 0.0018(13) -0.0010(14) 0.0085(14) C85 0.0289(19) 0.031(2) 0.0216(18) -0.0001(15) 0.0034(15) 0.0083(15) C86 0.040(2) 0.032(2) 0.0168(18) -0.0042(15) 0.0015(15) 0.0079(17) C87 0.033(2) 0.039(2) 0.0210(19) -0.0016(16) -0.0048(15) 0.0080(17) C88 0.030(2) 0.053(3) 0.025(2) 0.0017(18) -0.0002(16) 0.0181(18) C89 0.036(2) 0.041(2) 0.0208(18) -0.0038(16) -0.0019(15) 0.0206(18) C90 0.0224(18) 0.044(2) 0.0177(17) 0.0014(16) -0.0014(14) 0.0082(16) C91 0.036(2) 0.045(3) 0.040(2) 0.018(2) 0.0079(18) 0.0042(19) C96 0.0191(16) 0.0188(17) 0.0237(18) 0.0030(14) 0.0010(13) 0.0001(13) C97 0.0205(17) 0.0188(17) 0.0241(18) 0.0016(14) 0.0002(13) 0.0046(13) C98 0.0150(15) 0.0241(17) 0.0171(16) 0.0016(13) 0.0066(13) 0.0037(13) C99 0.0186(16) 0.0191(17) 0.0198(17) 0.0013(13) 0.0032(13) 0.0045(13) C100 0.0274(18) 0.0242(18) 0.0228(18) 0.0031(15) -0.0021(14) 0.0046(15) C101 0.035(2) 0.0265(19) 0.0259(19) 0.0094(16) -0.0001(15) 0.0106(16) C102 0.0259(18) 0.0227(18) 0.029(2) 0.0055(15) 0.0012(15) 0.0070(15) C103 0.0194(16) 0.0223(17) 0.0223(17) 0.0032(14) 0.0020(13) 0.0047(13) C104 0.0195(16) 0.0183(17) 0.0221(17) 0.0029(14) 0.0068(13) 0.0045(13) C105 0.0256(18) 0.0233(18) 0.0234(18) 0.0032(14) 0.0065(14) 0.0070(14) C106 0.0250(17) 0.0203(17) 0.0224(17) 0.0032(14) 0.0078(14) 0.0049(14) C107 0.0254(18) 0.0200(18) 0.035(2) 0.0002(15) -0.0039(15) 0.0045(14) C108 0.031(2) 0.026(2) 0.043(2) 0.0114(17) 0.0029(17) 0.0079(16) C109 0.044(2) 0.028(2) 0.060(3) 0.016(2) -0.005(2) 0.0095(19) C110 0.059(3) 0.024(2) 0.081(4) 0.004(2) -0.025(3) 0.015(2) C111 0.081(4) 0.031(2) 0.058(3) -0.017(2) -0.028(3) 0.026(2) C112 0.054(3) 0.031(2) 0.040(2) -0.0065(18) -0.015(2) 0.0203(19) C113 0.0307(19) 0.0197(17) 0.0219(18) 0.0025(14) 0.0004(14) 0.0076(14) C114 0.036(2) 0.028(2) 0.0256(19) 0.0037(16) -0.0023(16) 0.0028(16) C115 0.033(2) 0.035(2) 0.042(2) 0.0061(19) -0.0049(18) -0.0017(17) C116 0.049(3) 0.029(2) 0.035(2) 0.0008(18) -0.0132(19) 0.0070(19) C117 0.067(3) 0.030(2) 0.024(2) 0.0043(17) -0.0027(19) 0.014(2) C118 0.049(2) 0.0169(18) 0.031(2) 0.0032(15) 0.0046(18) 0.0015(16) O1 0.0166(11) 0.0172(11) 0.0191(11) 0.0014(9) -0.0003(9) 0.0024(9) O2 0.0270(13) 0.0220(13) 0.0397(15) 0.0041(11) 0.0080(11) 0.0043(10) O3 0.0185(12) 0.0213(12) 0.0349(14) 0.0074(10) 0.007(1) 0.0027(9) C1 0.0158(16) 0.0230(17) 0.0248(18) 0.0085(14) 0.0024(13) 0.0050(13) C2 0.0183(16) 0.0212(17) 0.0207(17) 0.0078(14) 0.0031(13) 0.0045(13) C3 0.0142(15) 0.0145(15) 0.0189(16) 0.0033(13) -0.0003(12) -0.0007(12) C4 0.0179(16) 0.0195(17) 0.0215(17) 0.0053(13) 0.0029(13) 0.0039(13) C5 0.0252(18) 0.0215(17) 0.0248(18) 0.0013(14) 0.0053(14) 0.0045(14) C6 0.0210(17) 0.0261(19) 0.0225(18) 0.0040(15) 0.0011(14) -0.0043(14) C7 0.0169(16) 0.0264(18) 0.0239(18) 0.0070(15) 0.0017(13) 0.0005(14) C14 0.0185(17) 0.0248(18) 0.042(2) 0.0119(16) 0.0063(15) 0.0077(14) C15 0.0186(18) 0.030(2) 0.050(2) 0.0188(18) 0.0061(16) 0.0044(15) C20 0.0189(16) 0.0243(18) 0.0248(18) -0.0006(14) 0.0034(13) 0.0092(14) C21 0.0189(17) 0.0300(19) 0.0294(19) 0.0001(15) 0.0040(14) 0.0050(14) C22 0.0269(19) 0.032(2) 0.041(2) 0.0060(18) 0.0004(16) 0.0106(16) C23 0.0195(17) 0.035(2) 0.032(2) -0.0034(16) 0.0056(15) 0.0048(15) C24 0.039(2) 0.041(2) 0.025(2) 0.0006(17) 0.0054(17) 0.0017(18) C25 0.028(2) 0.031(2) 0.028(2) -0.0013(16) 0.0005(16) -0.0084(16) C8 0.0197(17) 0.0220(17) 0.0309(19) 0.0064(15) 0.0097(14) 0.0073(14) C9 0.0264(18) 0.0217(18) 0.037(2) 0.0044(16) 0.0104(16) 0.0070(15) C10 0.038(2) 0.032(2) 0.036(2) 0.0030(17) 0.0158(17) 0.0096(17) C11 0.047(2) 0.040(2) 0.030(2) 0.0087(18) 0.0153(18) 0.0129(19) C12 0.032(2) 0.027(2) 0.036(2) 0.0091(17) 0.0127(16) 0.0102(16) C13 0.0213(17) 0.0244(18) 0.031(2) 0.0029(15) 0.0089(15) 0.0061(14) C30 0.069(3) 0.042(3) 0.039(3) -0.006(2) 0.023(2) 0.001(2) C45 0.046(2) 0.029(2) 0.041(2) 0.0152(18) 0.0196(19) 0.0113(18) C46 0.062(3) 0.041(3) 0.047(3) 0.019(2) 0.013(2) 0.003(2) C47 0.077(3) 0.043(3) 0.079(4) 0.026(3) 0.039(3) 0.031(3) C48 0.053(3) 0.038(2) 0.053(3) 0.019(2) 0.010(2) 0.001(2) C49 0.046(3) 0.067(3) 0.116(5) 0.057(3) 0.028(3) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O4 2.297(2) . ? Yb1 O6 2.303(2) . ? Yb1 O5 2.303(2) . ? Yb1 N4 2.461(3) . ? Yb1 N8 2.472(3) . ? Yb1 N12 2.494(3) . ? Yb1 N9 2.503(3) . ? Yb1 N13 2.543(2) . ? Yb1 N5 2.548(3) . ? O4 C75 1.252(4) . ? O5 C98 1.255(4) . ? O6 C52 1.252(4) . ? N1 C98 1.321(4) . ? N1 C97 1.458(4) . ? N1 H1B 0.8800 . ? N2 C75 1.320(4) . ? N2 C74 1.456(4) . ? N2 H2A 0.8800 . ? N3 C52 1.318(4) . ? N3 C51 1.465(4) . ? N3 H3A 0.8800 . ? N4 C103 1.337(4) . ? N4 C99 1.347(4) . ? N5 C104 1.338(4) . ? N5 N6 1.344(4) . ? N6 C106 1.330(4) . ? N7 C105 1.330(4) . ? N7 C104 1.331(4) . ? N8 C76 1.342(4) . ? N8 C80 1.344(4) . ? N9 C81 1.332(4) . ? N9 N10 1.342(4) . ? N10 C83 1.327(4) . ? N11 C82 1.333(4) . ? N11 C81 1.341(4) . ? N12 C53 1.333(4) . ? N12 C57 1.353(4) . ? N13 C58 1.327(4) . ? N13 N14 1.338(3) . ? N14 C60 1.326(4) . ? N15 C59 1.331(4) . ? N15 C58 1.341(4) . ? C50 O1 1.437(4) . ? C50 C51 1.513(4) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.509(4) . ? C53 C54 1.384(4) . ? C54 C55 1.385(5) . ? C54 H54A 0.9500 . ? C55 C56 1.381(5) . ? C55 H55A 0.9500 . ? C56 C57 1.385(4) . ? C56 H56A 0.9500 . ? C57 C58 1.477(4) . ? C59 C60 1.429(5) . ? C59 C61 1.491(3) . ? C60 C67 1.485(4) . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C62 H62A 0.9500 . ? C63 C64 1.3900 . ? C63 H63A 0.9500 . ? C64 C65 1.3900 . ? C64 H64A 0.9500 . ? C65 C66 1.3900 . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C67 C68 1.3900 . ? C67 C72 1.3900 . ? C68 C69 1.3900 . ? C68 H68A 0.9500 . ? C69 C70 1.3900 . ? C69 H69A 0.9500 . ? C70 C71 1.3900 . ? C70 H70A 0.9500 . ? C71 C72 1.3900 . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? C73 O2 1.442(4) . ? C73 C74 1.508(5) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.506(5) . ? C76 C77 1.388(5) . ? C77 C78 1.376(5) . ? C77 H77A 0.9500 . ? C78 C79 1.388(5) . ? C78 H78A 0.9500 . ? C79 C80 1.376(5) . ? C79 H79A 0.9500 . ? C80 C81 1.476(5) . ? C82 C83 1.434(4) . ? C82 C84 1.474(3) . ? C83 C90 1.473(5) . ? C84 C85 1.3900 . ? C84 C89 1.3900 . ? C85 C86 1.3900 . ? C85 H85A 0.9500 . ? C86 C87 1.3900 . ? C86 H86A 0.9500 . ? C87 C88 1.3900 . ? C87 H87A 0.9500 . ? C88 C89 1.3900 . ? C88 H88A 0.9500 . ? C89 H89A 0.9500 . ? C90 C95' 1.338(9) . ? C90 C91 1.392(5) . ? C90 C95 1.470(9) . ? C91 C92' 1.351(11) . ? C91 C92 1.452(13) . ? C91 H91A 0.9500 . ? C91 H91B 0.9501 . ? C92 C93 1.344(16) . ? C92 H92A 0.9500 . ? C93 C94 1.402(14) . ? C93 H93A 0.9500 . ? C94 C95 1.397(12) . ? C94 H94A 0.9500 . ? C95 H95A 0.9500 . ? C92' C93' 1.378(16) . ? C92' H92B 0.9500 . ? C93' C94' 1.371(15) . ? C93' H93B 0.9500 . ? C94' C95' 1.423(12) . ? C94' H94B 0.9500 . ? C95' H95B 0.9500 . ? C96 O3 1.438(4) . ? C96 C97 1.508(4) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.502(4) . ? C99 C100 1.389(4) . ? C100 C101 1.381(5) . ? C100 H10A 0.9500 . ? C101 C102 1.380(5) . ? C101 H10B 0.9500 . ? C102 C103 1.379(4) . ? C102 H10C 0.9500 . ? C103 C104 1.477(4) . ? C105 C106 1.437(4) . ? C105 C107 1.482(4) . ? C106 C113 1.489(4) . ? C107 C108 1.3900 . ? C107 C112 1.3900 . ? C108 C109 1.3900 . ? C108 H10D 0.9500 . ? C109 C110 1.3900 . ? C109 H10E 0.9500 . ? C110 C111 1.3900 . ? C110 H11A 0.9500 . ? C111 C112 1.3900 . ? C111 H11B 0.9500 . ? C112 H11C 0.9500 . ? C113 C114 1.3900 . ? C113 C118 1.3900 . ? C114 C115 1.3900 . ? C114 H11D 0.9500 . ? C115 C116 1.3900 . ? C115 H11E 0.9500 . ? C116 C117 1.3900 . ? C116 H11F 0.9500 . ? C117 C118 1.3900 . ? C117 H11G 0.9500 . ? C118 H11H 0.9500 . ? O1 C3 1.399(3) . ? O2 C9 1.396(4) . ? O3 C15 1.394(4) . ? C1 C14 1.528(4) . ? C1 C2 1.532(4) . ? C1 C8 1.543(4) . ? C1 H1A 1.0000 . ? C2 C7 1.383(4) . ? C2 C3 1.403(4) . ? C3 C4 1.395(4) . ? C4 C5 1.400(4) . ? C4 C20 1.543(4) . ? C5 C6 1.393(4) . ? C5 H5A 0.9500 . ? C6 C7 1.394(5) . ? C6 C25 1.536(5) . ? C7 H7A 0.9500 . ? C14 C15 1.398(5) . ? C14 C19' 1.400(8) . ? C14 C19 1.428(8) . ? C15 C16 1.420(9) . ? C15 C16' 1.459(7) . ? C20 C23 1.538(5) . ? C20 C22 1.537(5) . ? C20 C21 1.547(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.534(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27' 1.428(11) . ? C25 C28 1.481(9) . ? C25 C26 1.495(8) . ? C25 C28' 1.595(13) . ? C25 C26' 1.601(10) . ? C25 C27 1.639(8) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.589(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C26' H26D 0.9800 . ? C26' H26E 0.9800 . ? C26' H26F 0.9800 . ? C27' H27D 0.9800 . ? C27' H27E 0.9800 . ? C27' H27F 0.9800 . ? C28' C29' 1.545(19) . ? C28' H28C 0.9900 . ? C28' H28D 0.9900 . ? C29' H29D 0.9800 . ? C29' H29E 0.9800 . ? C29' H29F 0.9800 . ? C16 C17 1.425(11) . ? C16 C35 1.541(12) . ? C17 C18 1.395(10) . ? C17 H17A 0.9500 . ? C18 C19 1.378(10) . ? C18 C40 1.541(10) . ? C19 H19A 0.9500 . ? C35 C38 1.485(14) . ? C35 C36 1.533(15) . ? C35 C37 1.545(14) . ? C36 C39 1.498(15) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.504(11) . ? C40 C42 1.526(10) . ? C40 C43 1.551(11) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.571(12) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C16' C17' 1.391(9) . ? C16' C35' 1.540(9) . ? C17' C18' 1.388(9) . ? C17' H17B 0.9500 . ? C18' C19' 1.389(10) . ? C18' C40' 1.539(10) . ? C19' H19B 0.9500 . ? C35' C38' 1.532(11) . ? C35' C37' 1.539(9) . ? C35' C36' 1.546(11) . ? C36' C39' 1.512(10) . ? C36' H36C 0.9900 . ? C36' H36D 0.9900 . ? C37' H37D 0.9800 . ? C37' H37E 0.9800 . ? C37' H37F 0.9800 . ? C38' H38D 0.9800 . ? C38' H38E 0.9800 . ? C38' H38F 0.9800 . ? C39' H39D 0.9800 . ? C39' H39E 0.9800 . ? C39' H39F 0.9800 . ? C40' C43' 1.474(13) . ? C40' C41' 1.506(12) . ? C40' C42' 1.539(10) . ? C41' H41D 0.9800 . ? C41' H41E 0.9800 . ? C41' H41F 0.9800 . ? C42' H42D 0.9800 . ? C42' H42E 0.9800 . ? C42' H42F 0.9800 . ? C43' C44' 1.511(15) . ? C43' H43C 0.9900 . ? C43' H43D 0.9900 . ? C44' H44D 0.9800 . ? C44' H44E 0.9800 . ? C44' H44F 0.9800 . ? S1 O15 1.404(10) . ? S1 O14 1.422(10) . ? S1 O13 1.453(10) . ? S1 C900 1.707(14) . ? C900 F2 1.332(15) . ? C900 F3 1.366(16) . ? C900 F1 1.377(15) . ? S1' O15' 1.434(7) . ? S1' O13' 1.437(5) . ? S1' O14' 1.445(5) . ? S1' C910 1.851(8) . ? F1' C910 1.343(9) . ? F2' C910 1.324(8) . ? F3' C910 1.341(9) . ? S3 O9 1.418(6) . ? S3 O7 1.478(7) . ? S3 O8 1.504(9) . ? S3 C901 1.903(10) . ? F7 C901 1.249(12) . ? F8 C901 1.305(11) . ? F9 C901 1.294(11) . ? S3' O9' 1.428(7) . ? S3' O8' 1.435(7) . ? S3' O7' 1.448(10) . ? S3' C911 1.808(9) . ? F7' C911 1.346(10) . ? F8' C911 1.352(10) . ? F9' C911 1.368(10) . ? S2 O10 1.392(5) . ? S2 O12 1.427(7) . ? S2 O11 1.442(6) . ? S2 C902 1.862(5) . ? F4 C902 1.269(7) . ? F5 C902 1.366(6) . ? F6 C902 1.265(6) . ? S2' O11' 1.433(10) . ? S2' O10' 1.489(11) . ? S2' O12' 1.584(12) . ? S2' C902 1.718(6) . ? F5' C902 1.368(8) . ? F4' C902 1.437(9) . ? F6' C902 1.435(11) . ? C8 C13 1.390(4) . ? C8 C9 1.403(5) . ? C9 C10 1.398(5) . ? C10 C11 1.394(5) . ? C10 C30 1.555(5) . ? C11 C12 1.382(5) . ? C11 H11I 0.9500 . ? C12 C13 1.395(5) . ? C12 C45 1.532(5) . ? C13 H13A 0.9500 . ? C30 C32 1.450(9) . ? C30 C31 1.454(8) . ? C30 C33' 1.482(9) . ? C30 C32' 1.514(8) . ? C30 C33 1.627(10) . ? C30 C31' 1.753(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.410(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C31' H31D 0.9800 . ? C31' H31E 0.9800 . ? C31' H31F 0.9800 . ? C32' H32D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? C33' C34' 1.565(13) . ? C33' H33C 0.9900 . ? C33' H33D 0.9900 . ? C34' H34D 0.9800 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? C45 C48 1.526(6) . ? C45 C47 1.539(6) . ? C45 C46 1.539(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.511(6) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Yb1 O6 77.39(7) . . ? O4 Yb1 O5 75.23(7) . . ? O6 Yb1 O5 76.10(7) . . ? O4 Yb1 N4 73.83(8) . . ? O6 Yb1 N4 137.32(8) . . ? O5 Yb1 N4 66.57(8) . . ? O4 Yb1 N8 66.00(8) . . ? O6 Yb1 N8 76.27(8) . . ? O5 Yb1 N8 136.20(8) . . ? N4 Yb1 N8 117.89(8) . . ? O4 Yb1 N12 136.63(8) . . ? O6 Yb1 N12 65.71(8) . . ? O5 Yb1 N12 74.49(8) . . ? N4 Yb1 N12 119.73(8) . . ? N8 Yb1 N12 122.13(8) . . ? O4 Yb1 N9 130.31(8) . . ? O6 Yb1 N9 89.19(8) . . ? O5 Yb1 N9 147.35(8) . . ? N4 Yb1 N9 133.48(8) . . ? N8 Yb1 N9 64.35(8) . . ? N12 Yb1 N9 72.90(8) . . ? O4 Yb1 N13 145.64(8) . . ? O6 Yb1 N13 129.03(8) . . ? O5 Yb1 N13 89.32(8) . . ? N4 Yb1 N13 71.86(8) . . ? N8 Yb1 N13 134.41(8) . . ? N12 Yb1 N13 63.34(8) . . ? N9 Yb1 N13 77.45(8) . . ? O4 Yb1 N5 92.54(8) . . ? O6 Yb1 N5 148.19(8) . . ? O5 Yb1 N5 130.91(8) . . ? N4 Yb1 N5 64.35(8) . . ? N8 Yb1 N5 72.09(8) . . ? N12 Yb1 N5 130.82(8) . . ? N9 Yb1 N5 74.35(8) . . ? N13 Yb1 N5 74.47(8) . . ? C75 O4 Yb1 125.0(2) . . ? C98 O5 Yb1 123.0(2) . . ? C52 O6 Yb1 124.75(19) . . ? C98 N1 C97 123.3(3) . . ? C98 N1 H1B 118.4 . . ? C97 N1 H1B 118.4 . . ? C75 N2 C74 123.7(3) . . ? C75 N2 H2A 118.2 . . ? C74 N2 H2A 118.2 . . ? C52 N3 C51 123.9(3) . . ? C52 N3 H3A 118.1 . . ? C51 N3 H3A 118.1 . . ? C103 N4 C99 118.4(3) . . ? C103 N4 Yb1 123.5(2) . . ? C99 N4 Yb1 118.1(2) . . ? C104 N5 N6 118.0(3) . . ? C104 N5 Yb1 119.2(2) . . ? N6 N5 Yb1 121.76(19) . . ? C106 N6 N5 119.8(3) . . ? C105 N7 C104 118.1(3) . . ? C76 N8 C80 118.3(3) . . ? C76 N8 Yb1 118.7(2) . . ? C80 N8 Yb1 123.0(2) . . ? C81 N9 N10 117.3(3) . . ? C81 N9 Yb1 120.5(2) . . ? N10 N9 Yb1 118.54(18) . . ? C83 N10 N9 119.9(3) . . ? C82 N11 C81 117.0(3) . . ? C53 N12 C57 118.4(3) . . ? C53 N12 Yb1 118.4(2) . . ? C57 N12 Yb1 123.2(2) . . ? C58 N13 N14 117.8(3) . . ? C58 N13 Yb1 121.5(2) . . ? N14 N13 Yb1 120.04(19) . . ? C60 N14 N13 120.1(3) . . ? C59 N15 C58 117.1(3) . . ? O1 C50 C51 107.6(2) . . ? O1 C50 H50A 110.2 . . ? C51 C50 H50A 110.2 . . ? O1 C50 H50B 110.2 . . ? C51 C50 H50B 110.2 . . ? H50A C50 H50B 108.5 . . ? N3 C51 C50 110.3(3) . . ? N3 C51 H51A 109.6 . . ? C50 C51 H51A 109.6 . . ? N3 C51 H51B 109.6 . . ? C50 C51 H51B 109.6 . . ? H51A C51 H51B 108.1 . . ? O6 C52 N3 123.7(3) . . ? O6 C52 C53 118.1(3) . . ? N3 C52 C53 118.2(3) . . ? N12 C53 C54 122.9(3) . . ? N12 C53 C52 112.0(3) . . ? C54 C53 C52 125.1(3) . . ? C55 C54 C53 118.4(3) . . ? C55 C54 H54A 120.8 . . ? C53 C54 H54A 120.8 . . ? C56 C55 C54 119.4(3) . . ? C56 C55 H55A 120.3 . . ? C54 C55 H55A 120.3 . . ? C55 C56 C57 118.7(3) . . ? C55 C56 H56A 120.6 . . ? C57 C56 H56A 120.6 . . ? N12 C57 C56 122.1(3) . . ? N12 C57 C58 115.1(3) . . ? C56 C57 C58 122.8(3) . . ? N13 C58 N15 125.6(3) . . ? N13 C58 C57 116.6(3) . . ? N15 C58 C57 117.8(3) . . ? N15 C59 C60 118.4(3) . . ? N15 C59 C61 116.7(3) . . ? C60 C59 C61 124.9(3) . . ? N14 C60 C59 120.4(3) . . ? N14 C60 C67 113.5(3) . . ? C59 C60 C67 126.1(3) . . ? C62 C61 C66 120.0 . . ? C62 C61 C59 120.91(19) . . ? C66 C61 C59 119.09(19) . . ? C61 C62 C63 120.0 . . ? C61 C62 H62A 120.0 . . ? C63 C62 H62A 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H63A 120.0 . . ? C62 C63 H63A 120.0 . . ? C63 C64 C65 120.0 . . ? C63 C64 H64A 120.0 . . ? C65 C64 H64A 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 H65A 120.0 . . ? C64 C65 H65A 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66A 120.0 . . ? C61 C66 H66A 120.0 . . ? C68 C67 C72 120.0 . . ? C68 C67 C60 121.8(2) . . ? C72 C67 C60 118.2(2) . . ? C67 C68 C69 120.0 . . ? C67 C68 H68A 120.0 . . ? C69 C68 H68A 120.0 . . ? C70 C69 C68 120.0 . . ? C70 C69 H69A 120.0 . . ? C68 C69 H69A 120.0 . . ? C69 C70 C71 120.0 . . ? C69 C70 H70A 120.0 . . ? C71 C70 H70A 120.0 . . ? C72 C71 C70 120.0 . . ? C72 C71 H71A 120.0 . . ? C70 C71 H71A 120.0 . . ? C71 C72 C67 120.0 . . ? C71 C72 H72A 120.0 . . ? C67 C72 H72A 120.0 . . ? O2 C73 C74 107.3(3) . . ? O2 C73 H73A 110.3 . . ? C74 C73 H73A 110.3 . . ? O2 C73 H73B 110.3 . . ? C74 C73 H73B 110.3 . . ? H73A C73 H73B 108.5 . . ? N2 C74 C73 109.8(3) . . ? N2 C74 H74A 109.7 . . ? C73 C74 H74A 109.7 . . ? N2 C74 H74B 109.7 . . ? C73 C74 H74B 109.7 . . ? H74A C74 H74B 108.2 . . ? O4 C75 N2 123.4(3) . . ? O4 C75 C76 118.2(3) . . ? N2 C75 C76 118.4(3) . . ? N8 C76 C77 122.2(3) . . ? N8 C76 C75 111.7(3) . . ? C77 C76 C75 126.1(3) . . ? C78 C77 C76 118.8(3) . . ? C78 C77 H77A 120.6 . . ? C76 C77 H77A 120.6 . . ? C77 C78 C79 119.4(3) . . ? C77 C78 H78A 120.3 . . ? C79 C78 H78A 120.3 . . ? C80 C79 C78 118.4(3) . . ? C80 C79 H79A 120.8 . . ? C78 C79 H79A 120.8 . . ? N8 C80 C79 122.9(3) . . ? N8 C80 C81 114.5(3) . . ? C79 C80 C81 122.6(3) . . ? N9 C81 N11 125.0(3) . . ? N9 C81 C80 117.5(3) . . ? N11 C81 C80 117.4(3) . . ? N11 C82 C83 118.0(3) . . ? N11 C82 C84 117.5(3) . . ? C83 C82 C84 124.6(3) . . ? N10 C83 C82 119.8(3) . . ? N10 C83 C90 115.7(3) . . ? C82 C83 C90 124.3(3) . . ? C85 C84 C89 120.0 . . ? C85 C84 C82 118.78(18) . . ? C89 C84 C82 121.19(18) . . ? C84 C85 C86 120.0 . . ? C84 C85 H85A 120.0 . . ? C86 C85 H85A 120.0 . . ? C87 C86 C85 120.0 . . ? C87 C86 H86A 120.0 . . ? C85 C86 H86A 120.0 . . ? C88 C87 C86 120.0 . . ? C88 C87 H87A 120.0 . . ? C86 C87 H87A 120.0 . . ? C87 C88 C89 120.0 . . ? C87 C88 H88A 120.0 . . ? C89 C88 H88A 120.0 . . ? C88 C89 C84 120.0 . . ? C88 C89 H89A 120.0 . . ? C84 C89 H89A 120.0 . . ? C95' C90 C91 111.4(6) . . ? C95' C90 C95 20.0(4) . . ? C91 C90 C95 126.7(5) . . ? C95' C90 C83 129.1(5) . . ? C91 C90 C83 118.9(3) . . ? C95 C90 C83 114.1(5) . . ? C92' C91 C90 128.8(7) . . ? C92' C91 C92 18.6(7) . . ? C90 C91 C92 111.7(7) . . ? C92' C91 H91A 106.7 . . ? C90 C91 H91A 124.2 . . ? C92 C91 H91A 124.2 . . ? C92' C91 H91B 115.6 . . ? C90 C91 H91B 115.7 . . ? C92 C91 H91B 132.0 . . ? H91A C91 H91B 11.2 . . ? C93 C92 C91 125.0(11) . . ? C93 C92 H92A 117.5 . . ? C91 C92 H92A 117.5 . . ? C92 C93 C94 120.5(10) . . ? C92 C93 H93A 119.8 . . ? C94 C93 H93A 119.8 . . ? C95 C94 C93 121.5(9) . . ? C95 C94 H94A 119.3 . . ? C93 C94 H94A 119.3 . . ? C94 C95 C90 114.6(8) . . ? C94 C95 H95A 122.7 . . ? C90 C95 H95A 122.7 . . ? C91 C92' C93' 116.4(9) . . ? C91 C92' H92B 121.8 . . ? C93' C92' H92B 121.8 . . ? C94' C93' C92' 120.(1) . . ? C94' C93' H93B 120.0 . . ? C92' C93' H93B 120.0 . . ? C93' C94' C95' 118.0(9) . . ? C93' C94' H94B 121.0 . . ? C95' C94' H94B 121.0 . . ? C90 C95' C94' 124.8(8) . . ? C90 C95' H95B 117.6 . . ? C94' C95' H95B 117.6 . . ? O3 C96 C97 108.6(3) . . ? O3 C96 H96A 110.0 . . ? C97 C96 H96A 110.0 . . ? O3 C96 H96B 110.0 . . ? C97 C96 H96B 110.0 . . ? H96A C96 H96B 108.4 . . ? N1 C97 C96 110.5(3) . . ? N1 C97 H97A 109.6 . . ? C96 C97 H97A 109.6 . . ? N1 C97 H97B 109.6 . . ? C96 C97 H97B 109.6 . . ? H97A C97 H97B 108.1 . . ? O5 C98 N1 122.9(3) . . ? O5 C98 C99 118.3(3) . . ? N1 C98 C99 118.7(3) . . ? N4 C99 C100 122.1(3) . . ? N4 C99 C98 111.9(3) . . ? C100 C99 C98 126.0(3) . . ? C101 C100 C99 118.3(3) . . ? C101 C100 H10A 120.9 . . ? C99 C100 H10A 120.9 . . ? C100 C101 C102 120.1(3) . . ? C100 C101 H10B 120.0 . . ? C102 C101 H10B 120.0 . . ? C103 C102 C101 118.0(3) . . ? C103 C102 H10C 121.0 . . ? C101 C102 H10C 121.0 . . ? N4 C103 C102 123.2(3) . . ? N4 C103 C104 115.5(3) . . ? C102 C103 C104 121.4(3) . . ? N7 C104 N5 125.0(3) . . ? N7 C104 C103 117.6(3) . . ? N5 C104 C103 117.4(3) . . ? N7 C105 C106 117.9(3) . . ? N7 C105 C107 116.6(3) . . ? C106 C105 C107 125.4(3) . . ? N6 C106 C105 120.4(3) . . ? N6 C106 C113 115.2(3) . . ? C105 C106 C113 124.4(3) . . ? C108 C107 C112 120.0 . . ? C108 C107 C105 117.67(19) . . ? C112 C107 C105 122.33(19) . . ? C107 C108 C109 120.0 . . ? C107 C108 H10D 120.0 . . ? C109 C108 H10D 120.0 . . ? C108 C109 C110 120.0 . . ? C108 C109 H10E 120.0 . . ? C110 C109 H10E 120.0 . . ? C111 C110 C109 120.0 . . ? C111 C110 H11A 120.0 . . ? C109 C110 H11A 120.0 . . ? C112 C111 C110 120.0 . . ? C112 C111 H11B 120.0 . . ? C110 C111 H11B 120.0 . . ? C111 C112 C107 120.0 . . ? C111 C112 H11C 120.0 . . ? C107 C112 H11C 120.0 . . ? C114 C113 C118 120.0 . . ? C114 C113 C106 119.48(18) . . ? C118 C113 C106 120.51(18) . . ? C115 C114 C113 120.0 . . ? C115 C114 H11D 120.0 . . ? C113 C114 H11D 120.0 . . ? C114 C115 C116 120.0 . . ? C114 C115 H11E 120.0 . . ? C116 C115 H11E 120.0 . . ? C117 C116 C115 120.0 . . ? C117 C116 H11F 120.0 . . ? C115 C116 H11F 120.0 . . ? C118 C117 C116 120.0 . . ? C118 C117 H11G 120.0 . . ? C116 C117 H11G 120.0 . . ? C117 C118 C113 120.0 . . ? C117 C118 H11H 120.0 . . ? C113 C118 H11H 120.0 . . ? C3 O1 C50 113.4(2) . . ? C9 O2 C73 115.0(2) . . ? C15 O3 C96 114.8(3) . . ? C14 C1 C2 111.4(3) . . ? C14 C1 C8 113.3(3) . . ? C2 C1 C8 110.2(2) . . ? C14 C1 H1A 107.2 . . ? C2 C1 H1A 107.2 . . ? C8 C1 H1A 107.2 . . ? C7 C2 C3 118.6(3) . . ? C7 C2 C1 121.9(3) . . ? C3 C2 C1 119.6(3) . . ? C4 C3 O1 122.3(3) . . ? C4 C3 C2 121.4(3) . . ? O1 C3 C2 116.3(3) . . ? C3 C4 C5 116.8(3) . . ? C3 C4 C20 125.9(3) . . ? C5 C4 C20 117.3(3) . . ? C6 C5 C4 123.4(3) . . ? C6 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? C5 C6 C7 116.8(3) . . ? C5 C6 C25 123.0(3) . . ? C7 C6 C25 120.1(3) . . ? C2 C7 C6 122.3(3) . . ? C2 C7 H7A 118.9 . . ? C6 C7 H7A 118.9 . . ? C15 C14 C19' 116.2(4) . . ? C15 C14 C19 121.9(4) . . ? C19' C14 C19 17.9(4) . . ? C15 C14 C1 121.0(3) . . ? C19' C14 C1 122.2(4) . . ? C19 C14 C1 116.3(4) . . ? O3 C15 C14 118.8(3) . . ? O3 C15 C16 119.9(4) . . ? C14 C15 C16 118.3(4) . . ? O3 C15 C16' 118.7(4) . . ? C14 C15 C16' 122.3(4) . . ? C16 C15 C16' 21.9(4) . . ? C23 C20 C22 108.9(3) . . ? C23 C20 C4 109.7(3) . . ? C22 C20 C4 108.5(3) . . ? C23 C20 C21 106.8(3) . . ? C22 C20 C21 108.2(3) . . ? C4 C20 C21 114.6(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C20 114.2(3) . . ? C24 C23 H23A 108.7 . . ? C20 C23 H23A 108.7 . . ? C24 C23 H23B 108.7 . . ? C20 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27' C25 C28 116.6(7) . . ? C27' C25 C26 83.2(7) . . ? C28 C25 C26 114.9(5) . . ? C27' C25 C6 117.0(6) . . ? C28 C25 C6 112.5(4) . . ? C26 C25 C6 109.1(4) . . ? C27' C25 C28' 110.9(8) . . ? C28 C25 C28' 13.8(7) . . ? C26 C25 C28' 128.0(7) . . ? C6 C25 C28' 107.5(7) . . ? C27' C25 C26' 107.8(8) . . ? C28 C25 C26' 91.4(6) . . ? C26 C25 C26' 28.0(5) . . ? C6 C25 C26' 107.8(5) . . ? C28' C25 C26' 105.1(8) . . ? C27' C25 C27 19.8(6) . . ? C28 C25 C27 106.4(5) . . ? C26 C25 C27 103.0(4) . . ? C6 C25 C27 110.5(4) . . ? C28' C25 C27 97.3(7) . . ? C26' C25 C27 126.6(6) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 C29 113.6(5) . . ? C25 C28 H28A 108.8 . . ? C29 C28 H28A 108.8 . . ? C25 C28 H28B 108.8 . . ? C29 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C26' H26D 109.5 . . ? C25 C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C25 C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C25 C27' H27D 109.5 . . ? C25 C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C25 C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? C29' C28' C25 110.9(10) . . ? C29' C28' H28C 109.5 . . ? C25 C28' H28C 109.4 . . ? C29' C28' H28D 109.4 . . ? C25 C28' H28D 109.4 . . ? H28C C28' H28D 108.0 . . ? C28' C29' H29D 109.5 . . ? C28' C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C28' C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? C15 C16 C17 117.0(7) . . ? C15 C16 C35 123.1(7) . . ? C17 C16 C35 119.5(7) . . ? C18 C17 C16 123.0(7) . . ? C18 C17 H17A 118.5 . . ? C16 C17 H17A 118.5 . . ? C19 C18 C17 118.6(7) . . ? C19 C18 C40 122.0(7) . . ? C17 C18 C40 119.3(6) . . ? C18 C19 C14 119.1(7) . . ? C18 C19 H19A 120.4 . . ? C14 C19 H19A 120.4 . . ? C38 C35 C36 110.8(9) . . ? C38 C35 C16 109.8(8) . . ? C36 C35 C16 111.2(8) . . ? C38 C35 C37 108.2(9) . . ? C36 C35 C37 103.4(9) . . ? C16 C35 C37 113.3(8) . . ? C39 C36 C35 113.6(10) . . ? C39 C36 H36A 108.8 . . ? C35 C36 H36A 108.8 . . ? C39 C36 H36B 108.8 . . ? C35 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C42 107.3(6) . . ? C41 C40 C18 108.1(6) . . ? C42 C40 C18 112.1(6) . . ? C41 C40 C43 107.1(6) . . ? C42 C40 C43 111.7(6) . . ? C18 C40 C43 110.3(6) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 C44 114.6(7) . . ? C40 C43 H43A 108.6 . . ? C44 C43 H43A 108.6 . . ? C40 C43 H43B 108.6 . . ? C44 C43 H43B 108.6 . . ? H43A C43 H43B 107.6 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C17' C16' C15 115.7(5) . . ? C17' C16' C35' 120.4(6) . . ? C15 C16' C35' 122.9(5) . . ? C18' C17' C16' 124.3(6) . . ? C18' C17' H17B 117.9 . . ? C16' C17' H17B 117.9 . . ? C19' C18' C17' 116.8(6) . . ? C19' C18' C40' 122.1(6) . . ? C17' C18' C40' 121.1(6) . . ? C18' C19' C14 124.6(6) . . ? C18' C19' H19B 117.7 . . ? C14 C19' H19B 117.7 . . ? C38' C35' C37' 106.8(6) . . ? C38' C35' C16' 114.4(6) . . ? C37' C35' C16' 112.1(5) . . ? C38' C35' C36' 107.3(6) . . ? C37' C35' C36' 108.1(6) . . ? C16' C35' C36' 107.9(6) . . ? C39' C36' C35' 118.1(7) . . ? C39' C36' H36C 107.8 . . ? C35' C36' H36C 107.8 . . ? C39' C36' H36D 107.8 . . ? C35' C36' H36D 107.8 . . ? H36C C36' H36D 107.1 . . ? C35' C37' H37D 109.5 . . ? C35' C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? C35' C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? C35' C38' H38D 109.5 . . ? C35' C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? C35' C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? C36' C39' H39D 109.5 . . ? C36' C39' H39E 109.5 . . ? H39D C39' H39E 109.5 . . ? C36' C39' H39F 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? C43' C40' C41' 104.9(8) . . ? C43' C40' C42' 108.3(7) . . ? C41' C40' C42' 110.1(7) . . ? C43' C40' C18' 111.3(7) . . ? C41' C40' C18' 109.3(7) . . ? C42' C40' C18' 112.6(6) . . ? C40' C41' H41D 109.5 . . ? C40' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? C40' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? C40' C42' H42D 109.5 . . ? C40' C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? C40' C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? C40' C43' C44' 115.5(9) . . ? C40' C43' H43C 108.4 . . ? C44' C43' H43C 108.4 . . ? C40' C43' H43D 108.4 . . ? C44' C43' H43D 108.4 . . ? H43C C43' H43D 107.5 . . ? C43' C44' H44D 109.5 . . ? C43' C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C43' C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? O15 S1 O14 118.9(6) . . ? O15 S1 O13 112.7(6) . . ? O14 S1 O13 113.3(6) . . ? O15 S1 C900 101.4(6) . . ? O14 S1 C900 103.8(6) . . ? O13 S1 C900 104.3(6) . . ? F2 C900 F3 107.3(11) . . ? F2 C900 F1 105.9(10) . . ? F3 C900 F1 104.8(10) . . ? F2 C900 S1 114.8(9) . . ? F3 C900 S1 107.8(9) . . ? F1 C900 S1 115.6(9) . . ? O15' S1' O13' 115.5(3) . . ? O15' S1' O14' 114.9(3) . . ? O13' S1' O14' 114.4(3) . . ? O15' S1' C910 104.4(4) . . ? O13' S1' C910 101.9(3) . . ? O14' S1' C910 103.4(3) . . ? F2' C910 F3' 107.0(6) . . ? F2' C910 F1' 108.7(6) . . ? F3' C910 F1' 108.2(6) . . ? F2' C910 S1' 110.4(5) . . ? F3' C910 S1' 110.3(5) . . ? F1' C910 S1' 112.1(5) . . ? O9 S3 O7 115.1(4) . . ? O9 S3 O8 115.4(4) . . ? O7 S3 O8 108.5(4) . . ? O9 S3 C901 107.0(4) . . ? O7 S3 C901 103.5(4) . . ? O8 S3 C901 106.3(5) . . ? F7 C901 F9 118.2(10) . . ? F7 C901 F8 107.9(9) . . ? F9 C901 F8 109.9(9) . . ? F7 C901 S3 109.1(7) . . ? F9 C901 S3 105.5(8) . . ? F8 C901 S3 105.5(7) . . ? O9' S3' O8' 115.6(4) . . ? O9' S3' O7' 112.1(5) . . ? O8' S3' O7' 119.4(5) . . ? O9' S3' C911 106.7(4) . . ? O8' S3' C911 102.9(4) . . ? O7' S3' C911 96.8(5) . . ? F7' C911 F8' 111.7(7) . . ? F7' C911 F9' 103.7(7) . . ? F8' C911 F9' 103.6(7) . . ? F7' C911 S3' 113.6(6) . . ? F8' C911 S3' 111.0(6) . . ? F9' C911 S3' 112.5(6) . . ? O10 S2 O12 120.9(4) . . ? O10 S2 O11 113.6(3) . . ? O12 S2 O11 109.1(4) . . ? O10 S2 C902 108.6(3) . . ? O12 S2 C902 100.2(3) . . ? O11 S2 C902 101.9(3) . . ? O11' S2' O10' 117.8(6) . . ? O11' S2' O12' 121.0(6) . . ? O10' S2' O12' 105.8(6) . . ? O11' S2' C902 108.9(5) . . ? O10' S2' C902 98.5(5) . . ? O12' S2' C902 101.3(4) . . ? F6 C902 F4 107.3(5) . . ? F6 C902 F5 108.0(4) . . ? F4 C902 F5 101.9(5) . . ? F6 C902 F5' 81.3(5) . . ? F4 C902 F5' 110.5(6) . . ? F5 C902 F5' 26.7(4) . . ? F6 C902 F6' 118.9(6) . . ? F4 C902 F6' 13.9(5) . . ? F5 C902 F6' 103.6(5) . . ? F5' C902 F6' 118.0(6) . . ? F6 C902 F4' 19.0(4) . . ? F4 C902 F4' 97.9(5) . . ? F5 C902 F4' 126.8(5) . . ? F5' C902 F4' 100.1(6) . . ? F6' C902 F4' 106.9(5) . . ? F6 C902 S2' 111.8(4) . . ? F4 C902 S2' 123.7(4) . . ? F5 C902 S2' 102.7(3) . . ? F5' C902 S2' 114.0(4) . . ? F6' C902 S2' 110.3(5) . . ? F4' C902 S2' 106.1(4) . . ? F6 C902 S2 116.1(4) . . ? F4 C902 S2 114.8(4) . . ? F5 C902 S2 107.7(3) . . ? F5' C902 S2 121.8(4) . . ? F6' C902 S2 101.5(5) . . ? F4' C902 S2 107.6(4) . . ? S2' C902 S2 9.1(2) . . ? C13 C8 C9 118.6(3) . . ? C13 C8 C1 120.1(3) . . ? C9 C8 C1 121.0(3) . . ? O2 C9 C10 121.0(3) . . ? O2 C9 C8 117.3(3) . . ? C10 C9 C8 121.4(3) . . ? C11 C10 C9 116.6(3) . . ? C11 C10 C30 117.3(3) . . ? C9 C10 C30 126.0(3) . . ? C12 C11 C10 124.2(3) . . ? C12 C11 H11I 117.9 . . ? C10 C11 H11I 117.9 . . ? C11 C12 C13 117.0(3) . . ? C11 C12 C45 123.6(3) . . ? C13 C12 C45 119.4(3) . . ? C8 C13 C12 121.9(3) . . ? C8 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C32 C30 C31 110.0(6) . . ? C32 C30 C33' 134.8(8) . . ? C31 C30 C33' 54.3(5) . . ? C32 C30 C32' 27.7(4) . . ? C31 C30 C32' 121.7(6) . . ? C33' C30 C32' 117.9(7) . . ? C32 C30 C10 111.5(5) . . ? C31 C30 C10 114.3(4) . . ? C33' C30 C10 113.4(7) . . ? C32' C30 C10 118.8(5) . . ? C32 C30 C33 102.3(6) . . ? C31 C30 C33 110.8(5) . . ? C33' C30 C33 59.3(6) . . ? C32' C30 C33 74.6(5) . . ? C10 C30 C33 107.2(5) . . ? C32 C30 C31' 76.3(6) . . ? C31 C30 C31' 44.3(5) . . ? C33' C30 C31' 98.5(6) . . ? C32' C30 C31' 100.5(6) . . ? C10 C30 C31' 102.7(6) . . ? C33 C30 C31' 148.0(6) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C30 109.0(8) . . ? C34 C33 H33A 109.9 . . ? C30 C33 H33A 109.9 . . ? C34 C33 H33B 109.9 . . ? C30 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C31' H31D 109.5 . . ? C30 C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? C30 C31' H31F 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? C30 C32' H32D 109.5 . . ? C30 C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? C30 C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C30 C33' C34' 101.4(10) . . ? C30 C33' H33C 111.5 . . ? C34' C33' H33C 111.5 . . ? C30 C33' H33D 111.5 . . ? C34' C33' H33D 111.5 . . ? H33C C33' H33D 109.3 . . ? C33' C34' H34D 109.5 . . ? C33' C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C33' C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C48 C45 C12 110.0(3) . . ? C48 C45 C47 109.5(4) . . ? C12 C45 C47 108.5(3) . . ? C48 C45 C46 110.7(3) . . ? C12 C45 C46 112.3(3) . . ? C47 C45 C46 105.6(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C45 115.4(4) . . ? C49 C48 H48A 108.4 . . ? C45 C48 H48A 108.4 . . ? C49 C48 H48B 108.4 . . ? C45 C48 H48B 108.4 . . ? H48A C48 H48B 107.5 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.980 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.090 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.010 -0.010 0.490 1542 358 ' ' 2 0.196 0.937 0.986 9 1 ' ' 3 0.803 0.063 0.014 9 1 ' ' _platon_squeeze_details ; ; data_yb5 _database_code_depnum_ccdc_archive 'CCDC 889306' #TrackingRef 'web_deposit_cif_file_0_GaryGuillet_1349827554.gg17.cif' # # xray code for Yb5 is gg17 # # Although an Alert_A was not generated, we report that one # disordered MTBEsolvent molecule was disordered and it # contributed was remove by Platon/Squeeze. # # _audit_update_record ; 2012-09-24 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C87 H93 N15 O3 Yb1, 3(CO3F3S), (C5H12O1)' _chemical_formula_sum 'C95 H105 F9 N15 O13 S3 Yb' _chemical_formula_weight 2105.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -7.2108 4.4329 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 24.8539(6) _cell_length_b 13.9870(3) _cell_length_c 28.8206(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.791(1) _cell_angle_gamma 90.00 _cell_volume 9687.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 507 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4332 _exptl_absorpt_coefficient_mu 3.120 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6562 _exptl_absorpt_correction_T_max 0.8584 _exptl_absorpt_process_details 'based on measured indexed crystal faces, Bruker SHELXTL v6.14 (Bruker 2008)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37661 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 66.50 _reflns_number_total 12824 _reflns_number_gt 12386 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT (Bruker, 2008)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The following restraints were employed in the final refinement model. yb5 DFIX 1.37 c88 f1 c88 f2 c88 f3 dfix 2.19 f1 f2 f1 f3 f2 f3 dfix 1.37 c89' f4' c89' f5' c89' f6' dfix 2.19 f4' f5' f4' f6' f5' f6' eadp o4' o5' o6' eadp f1' f2' f3' eadp f7 f8 f9 eadp c88 c88' ; _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^)+(0.0136P)^2^+14.6460P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.008(5) _refine_ls_number_reflns 12824 _refine_ls_number_parameters 1139 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.057 _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 0.938863(5) 0.219472(10) 0.665259(5) 0.01506(5) Uani 1 1 d . . . O1 O 0.95101(10) 0.33418(18) 0.61473(8) 0.0204(5) Uani 1 1 d . . . O2 O 0.96854(10) 0.13058(17) 0.60970(8) 0.0186(5) Uani 1 1 d . . . O3 O 0.8572(1) 0.20316(17) 0.60771(9) 0.0204(5) Uani 1 1 d . . . N1 N 0.94683(12) 0.4776(2) 0.58000(11) 0.0205(6) Uani 1 1 d . . . N2 N 0.88285(12) 0.3646(2) 0.66559(10) 0.0183(6) Uani 1 1 d . . . N3 N 0.87998(12) 0.2153(2) 0.72239(10) 0.0194(6) Uani 1 1 d . . . N4 N 0.88044(13) 0.1385(2) 0.74995(11) 0.0213(6) Uani 1 1 d . . . N5 N 0.81684(13) 0.2951(2) 0.75813(11) 0.0223(6) Uani 1 1 d . . . N6 N 1.03268(13) 0.0474(2) 0.58440(11) 0.0239(7) Uani 1 1 d . . . N7 N 1.03886(11) 0.2340(2) 0.67051(10) 0.0160(6) Uani 1 1 d . . . N8 N 0.99116(12) 0.3186(2) 0.73268(10) 0.0182(6) Uani 1 1 d . . . N9 N 0.96687(12) 0.3562(2) 0.76502(11) 0.0187(6) Uani 1 1 d . . . N10 N 1.07749(12) 0.3890(2) 0.77240(11) 0.0193(6) Uani 1 1 d . . . N11 N 0.77480(13) 0.1351(2) 0.57440(11) 0.0228(7) Uani 1 1 d . . . N12 N 0.89798(12) 0.0559(2) 0.65875(10) 0.0181(6) Uani 1 1 d . . . N13 N 0.98962(12) 0.1012(2) 0.72503(10) 0.0182(6) Uani 1 1 d . . . N14 N 1.03775(12) 0.1259(2) 0.75657(11) 0.0189(6) Uani 1 1 d . . . N15 N 0.99765(12) -0.0571(2) 0.75485(11) 0.0196(6) Uani 1 1 d . . . C1 C 0.97615(18) 0.4006(3) 0.51012(16) 0.0285(8) Uani 1 1 d . . . H1A H 0.9568 0.4506 0.4870 0.034 Uiso 1 1 calc R . . C2 C 0.9367(2) 0.3163(3) 0.50656(16) 0.0359(10) Uani 1 1 d . . . H2A H 0.9032 0.3368 0.5158 0.054 Uiso 1 1 calc R . . H2B H 0.9552 0.2653 0.5281 0.054 Uiso 1 1 calc R . . H2C H 0.9264 0.2925 0.4735 0.054 Uiso 1 1 calc R . . C3 C 1.02914(19) 0.3716(4) 0.49580(18) 0.0422(11) Uani 1 1 d . . . H3A H 1.0538 0.4271 0.4985 0.063 Uiso 1 1 calc R . . H3B H 1.0193 0.3484 0.4626 0.063 Uiso 1 1 calc R . . H3C H 1.0482 0.3208 0.5172 0.063 Uiso 1 1 calc R . . C4 C 0.99327(15) 0.4460(3) 0.55993(13) 0.0229(8) Uani 1 1 d . . . H4A H 1.0161 0.3993 0.5824 0.028 Uiso 1 1 calc R . . H4B H 1.0171 0.5021 0.5585 0.028 Uiso 1 1 calc R . . C5 C 0.91328(16) 0.6140(3) 0.52387(14) 0.0258(8) Uani 1 1 d . . . H5A H 0.9403 0.5935 0.5054 0.031 Uiso 1 1 calc R . . C6 C 0.85684(17) 0.5693(3) 0.50015(13) 0.0272(8) Uani 1 1 d . . . H6A H 0.8600 0.4994 0.5017 0.041 Uiso 1 1 calc R . . H6B H 0.8450 0.5895 0.4665 0.041 Uiso 1 1 calc R . . H6C H 0.8293 0.5902 0.5170 0.041 Uiso 1 1 calc R . . C7 C 0.90990(19) 0.7229(3) 0.52215(18) 0.0378(10) Uani 1 1 d . . . H7A H 0.9466 0.7499 0.5373 0.057 Uiso 1 1 calc R . . H7B H 0.8829 0.7447 0.5394 0.057 Uiso 1 1 calc R . . H7C H 0.8981 0.7440 0.4887 0.057 Uiso 1 1 calc R . . C8 C 0.93575(17) 0.5816(3) 0.57566(15) 0.0277(8) Uani 1 1 d . . . H8A H 0.9707 0.6166 0.5900 0.033 Uiso 1 1 calc R . . H8B H 0.9085 0.5984 0.5941 0.033 Uiso 1 1 calc R . . C9 C 0.92935(14) 0.4163(3) 0.60772(12) 0.0186(7) Uani 1 1 d . . . C10 C 0.88295(15) 0.4331(3) 0.63283(13) 0.0214(7) Uani 1 1 d . . . C11 C 0.84245(19) 0.5032(3) 0.62270(15) 0.0317(9) Uani 1 1 d . . . H11A H 0.8405 0.5471 0.5972 0.038 Uiso 1 1 calc R . . C12 C 0.80437(19) 0.5080(3) 0.65085(17) 0.0375(10) Uani 1 1 d . . . H12A H 0.7771 0.5571 0.6455 0.045 Uiso 1 1 calc R . . C13 C 0.80648(17) 0.4410(3) 0.68653(15) 0.0309(9) Uani 1 1 d . . . H13A H 0.7821 0.4448 0.7070 0.037 Uiso 1 1 calc R . . C14 C 0.84514(15) 0.3681(3) 0.69150(13) 0.0222(7) Uani 1 1 d . . . C15 C 0.84717(14) 0.2882(3) 0.72589(12) 0.0189(7) Uani 1 1 d . . . C16 C 0.85085(15) 0.1389(3) 0.78259(13) 0.0216(7) Uani 1 1 d . . . C17 C 0.82017(14) 0.2227(3) 0.78865(12) 0.0209(7) Uani 1 1 d . . . C18 C 0.85104(19) 0.0473(3) 0.80870(15) 0.0311(9) Uani 1 1 d . . . C19 C 0.8023(2) 0.0083(3) 0.81536(16) 0.0347(9) Uani 1 1 d . . . H19A H 0.7680 0.0412 0.8041 0.042 Uiso 1 1 calc R . . C20 C 0.8040(3) -0.0793(4) 0.8386(2) 0.0508(13) Uani 1 1 d . . . H20A H 0.7708 -0.1056 0.8438 0.061 Uiso 1 1 calc R . . C21 C 0.8535(3) -0.1283(4) 0.8542(2) 0.0551(15) Uani 1 1 d . . . H21A H 0.8543 -0.1882 0.8699 0.066 Uiso 1 1 calc R . . C22 C 0.9017(2) -0.0903(4) 0.84709(17) 0.0482(13) Uani 1 1 d . . . H22A H 0.9358 -0.1243 0.8577 0.058 Uiso 1 1 calc R . . C23 C 0.9011(2) -0.0022(4) 0.82440(16) 0.0354(10) Uani 1 1 d . . . H23A H 0.9345 0.0241 0.8197 0.042 Uiso 1 1 calc R . . C24 C 0.79300(16) 0.2355(3) 0.82820(14) 0.0248(8) Uani 1 1 d . . . C25 C 0.81899(16) 0.2037(3) 0.87481(14) 0.0267(8) Uani 1 1 d . . . H25A H 0.8534 0.1704 0.8807 0.032 Uiso 1 1 calc R . . C26 C 0.7944(2) 0.2211(3) 0.91237(18) 0.0318(12) Uani 1 1 d . . . H26A H 0.8124 0.2007 0.9440 0.038 Uiso 1 1 calc R . . C27 C 0.7444(2) 0.2677(3) 0.90381(16) 0.0355(10) Uani 1 1 d . . . H27A H 0.7274 0.2787 0.9294 0.043 Uiso 1 1 calc R . . C28 C 0.7186(2) 0.2987(4) 0.85816(19) 0.0435(12) Uani 1 1 d . . . H28A H 0.6836 0.3299 0.8522 0.052 Uiso 1 1 calc R . . C29 C 0.74374(19) 0.2844(3) 0.82075(16) 0.0356(10) Uani 1 1 d . . . H29A H 0.7266 0.3088 0.7897 0.043 Uiso 1 1 calc R . . C30 C 0.95267(18) 0.0418(3) 0.51081(14) 0.0290(9) Uani 1 1 d . . . H30A H 0.9355 0.0994 0.5217 0.035 Uiso 1 1 calc R . . C31 C 0.90636(19) -0.0235(3) 0.48353(15) 0.0354(10) Uani 1 1 d . . . H31A H 0.8835 -0.0438 0.5049 0.053 Uiso 1 1 calc R . . H31B H 0.9226 -0.0798 0.4721 0.053 Uiso 1 1 calc R . . H31C H 0.8831 0.0111 0.4561 0.053 Uiso 1 1 calc R . . C32 C 0.9903(2) 0.0746(4) 0.47914(16) 0.0397(11) Uani 1 1 d . . . H32A H 1.0198 0.1158 0.4979 0.060 Uiso 1 1 calc R . . H32B H 0.9681 0.1104 0.4516 0.060 Uiso 1 1 calc R . . H32C H 1.0069 0.0187 0.4677 0.060 Uiso 1 1 calc R . . C33 C 0.98652(16) -0.0119(3) 0.55523(14) 0.0251(8) Uani 1 1 d . . . H33A H 0.9615 -0.0310 0.5754 0.030 Uiso 1 1 calc R . . H33B H 1.0022 -0.0708 0.5448 0.030 Uiso 1 1 calc R . . C34 C 1.09933(18) -0.0779(3) 0.62743(17) 0.036(1) Uani 1 1 d . . . H34A H 1.0683 -0.1250 0.6173 0.043 Uiso 1 1 calc R . . C35 C 1.1007(3) -0.0427(4) 0.67796(19) 0.0577(15) Uani 1 1 d . . . H35A H 1.1072 -0.0969 0.7002 0.086 Uiso 1 1 calc R . . H35B H 1.0650 -0.0126 0.6778 0.086 Uiso 1 1 calc R . . H35C H 1.1308 0.0041 0.6883 0.086 Uiso 1 1 calc R . . C36 C 1.1537(2) -0.1270(4) 0.6263(2) 0.0475(12) Uani 1 1 d . . . H36A H 1.1518 -0.1485 0.5936 0.071 Uiso 1 1 calc R . . H36B H 1.1597 -0.1822 0.6480 0.071 Uiso 1 1 calc R . . H36C H 1.1846 -0.0819 0.6367 0.071 Uiso 1 1 calc R . . C37 C 1.08894(16) 0.0051(3) 0.59197(15) 0.0293(9) Uani 1 1 d . . . H37A H 1.1171 0.0555 0.6039 0.035 Uiso 1 1 calc R . . H37B H 1.0938 -0.0176 0.5608 0.035 Uiso 1 1 calc R . . C38 C 1.01905(16) 0.1194(3) 0.60910(13) 0.0193(7) Uani 1 1 d . . . C39 C 1.05898(15) 0.1928(3) 0.63619(12) 0.0186(7) Uani 1 1 d . . . C40 C 1.10838(17) 0.2246(3) 0.62687(15) 0.0276(8) Uani 1 1 d . . . H40A H 1.1208 0.1989 0.6009 0.033 Uiso 1 1 calc R . . C41 C 1.13892(17) 0.2941(3) 0.65611(15) 0.0304(9) Uani 1 1 d . . . H41A H 1.1729 0.3161 0.6505 0.036 Uiso 1 1 calc R . . C42 C 1.12020(17) 0.3317(3) 0.69350(15) 0.0292(9) Uani 1 1 d . . . H42A H 1.1417 0.3772 0.7149 0.035 Uiso 1 1 calc R . . C43 C 1.06924(15) 0.3010(2) 0.69878(12) 0.0184(7) Uani 1 1 d . . . C44 C 1.04428(14) 0.3400(2) 0.73626(13) 0.0172(7) Uani 1 1 d . . . C45 C 0.99632(14) 0.4090(2) 0.80069(12) 0.0173(7) Uani 1 1 d . . . C46 C 1.05480(15) 0.4226(2) 0.80607(12) 0.0177(7) Uani 1 1 d . . . C47 C 0.96321(15) 0.4513(3) 0.83195(13) 0.0223(8) Uani 1 1 d . . . C48 C 0.92945(19) 0.3925(3) 0.85121(16) 0.0338(10) Uani 1 1 d . . . H48A H 0.9288 0.3255 0.8456 0.041 Uiso 1 1 calc R . . C49 C 0.8964(2) 0.4322(4) 0.87887(16) 0.0413(11) Uani 1 1 d . . . H49A H 0.8734 0.3919 0.8922 0.050 Uiso 1 1 calc R . . C50 C 0.89683(19) 0.5283(4) 0.88691(16) 0.0371(10) Uani 1 1 d . . . H50A H 0.8742 0.5547 0.9058 0.045 Uiso 1 1 calc R . . C51 C 0.93011(19) 0.5872(3) 0.86767(16) 0.0359(10) Uani 1 1 d . . . H51A H 0.9303 0.6542 0.8733 0.043 Uiso 1 1 calc R . . C52 C 0.96345(17) 0.5490(3) 0.84006(14) 0.0288(9) Uani 1 1 d . . . H52A H 0.9863 0.5897 0.8268 0.035 Uiso 1 1 calc R . . C53 C 1.09460(15) 0.4670(3) 0.84793(13) 0.0208(7) Uani 1 1 d . . . C54 C 1.08732(16) 0.4634(3) 0.89393(14) 0.0250(8) Uani 1 1 d . . . H54A H 1.0543 0.4366 0.8993 0.030 Uiso 1 1 calc R . . C55 C 1.12828(17) 0.4990(3) 0.93241(14) 0.0292(9) Uani 1 1 d . . . H55A H 1.1239 0.4944 0.9641 0.035 Uiso 1 1 calc R . . C56 C 1.17544(17) 0.5412(3) 0.92421(15) 0.0328(9) Uani 1 1 d . . . H56A H 1.2030 0.5669 0.9504 0.039 Uiso 1 1 calc R . . C57 C 1.18275(16) 0.5463(3) 0.87841(15) 0.0313(9) Uani 1 1 d . . . H57A H 1.2151 0.5757 0.8730 0.038 Uiso 1 1 calc R . . C58 C 1.14261(17) 0.5082(3) 0.84018(14) 0.0270(8) Uani 1 1 d . . . H58A H 1.1479 0.5102 0.8087 0.032 Uiso 1 1 calc R . . C59 C 0.77699(19) 0.2599(4) 0.51253(17) 0.0401(11) Uani 1 1 d . . . H59A H 0.8183 0.2672 0.5235 0.048 Uiso 1 1 calc R . . C60 C 0.7509(2) 0.3572(4) 0.4944(2) 0.0538(14) Uani 1 1 d . . . H60A H 0.7602 0.4040 0.5205 0.081 Uiso 1 1 calc R . . H60B H 0.7104 0.3504 0.4835 0.081 Uiso 1 1 calc R . . H60C H 0.7655 0.3790 0.4677 0.081 Uiso 1 1 calc R . . C61 C 0.7630(3) 0.1855(4) 0.47277(19) 0.0500(13) Uani 1 1 d . . . H61A H 0.7805 0.1245 0.4848 0.075 Uiso 1 1 calc R . . H61B H 0.7769 0.2069 0.4456 0.075 Uiso 1 1 calc R . . H61C H 0.7225 0.1771 0.4623 0.075 Uiso 1 1 calc R . . C62 C 0.75493(16) 0.2304(3) 0.55489(15) 0.0284(9) Uani 1 1 d . . . H62A H 0.7664 0.2786 0.5807 0.034 Uiso 1 1 calc R . . H62B H 0.7138 0.2298 0.5448 0.034 Uiso 1 1 calc R . . C63 C 0.69553(17) 0.0818(3) 0.60624(16) 0.0332(9) Uani 1 1 d . . . H63A H 0.6822 0.1495 0.6024 0.040 Uiso 1 1 calc R . . C64 C 0.7299(2) 0.0670(5) 0.65824(19) 0.0587(16) Uani 1 1 d . . . H64A H 0.7617 0.1110 0.6652 0.088 Uiso 1 1 calc R . . H64B H 0.7435 0.0010 0.6624 0.088 Uiso 1 1 calc R . . H64C H 0.7066 0.0797 0.6803 0.088 Uiso 1 1 calc R . . C65 C 0.64502(19) 0.0150(4) 0.59303(19) 0.0427(11) Uani 1 1 d . . . H65A H 0.6241 0.0271 0.5598 0.064 Uiso 1 1 calc R . . H65B H 0.6210 0.0268 0.6146 0.064 Uiso 1 1 calc R . . H65C H 0.6577 -0.0516 0.5962 0.064 Uiso 1 1 calc R . . C66 C 0.73116(15) 0.0631(3) 0.57112(14) 0.0259(8) Uani 1 1 d . . . H66A H 0.7486 -0.0008 0.5777 0.031 Uiso 1 1 calc R . . H66B H 0.7069 0.0624 0.5380 0.031 Uiso 1 1 calc R . . C67 C 0.82778(15) 0.1290(3) 0.59962(13) 0.0192(7) Uani 1 1 d . . . C68 C 0.85595(15) 0.0370(3) 0.62011(13) 0.0187(7) Uani 1 1 d . . . C69 C 0.84628(16) -0.0538(3) 0.60104(13) 0.0235(8) Uani 1 1 d . . . H69A H 0.8182 -0.0648 0.5723 0.028 Uiso 1 1 calc R . . C70 C 0.87872(17) -0.1289(3) 0.62495(15) 0.0279(8) Uani 1 1 d . . . H70A H 0.8728 -0.1920 0.6125 0.033 Uiso 1 1 calc R . . C71 C 0.91938(16) -0.1118(3) 0.66663(14) 0.0251(8) Uani 1 1 d . . . H71A H 0.9407 -0.1625 0.6843 0.030 Uiso 1 1 calc R . . C72 C 0.92791(14) -0.0172(3) 0.68178(12) 0.0186(7) Uani 1 1 d . . . C73 C 0.97480(14) 0.0096(3) 0.72293(12) 0.0174(7) Uani 1 1 d . . . C74 C 1.06607(15) 0.0605(3) 0.78646(12) 0.0192(7) Uani 1 1 d . . . C75 C 1.04199(15) -0.0314(3) 0.78937(13) 0.0204(7) Uani 1 1 d . . . C76 C 1.12317(16) 0.0902(3) 0.81221(13) 0.0239(8) Uani 1 1 d . . . C77 C 1.13222(18) 0.1811(3) 0.83221(15) 0.0305(9) Uani 1 1 d . . . H77A H 1.1016 0.2224 0.8313 0.037 Uiso 1 1 calc R . . C78 C 1.1859(2) 0.2117(3) 0.85354(17) 0.0414(11) Uani 1 1 d . . . H78A H 1.1922 0.2735 0.8676 0.050 Uiso 1 1 calc R . . C79 C 1.2306(2) 0.1514(4) 0.85424(19) 0.0476(12) Uani 1 1 d . . . H79A H 1.2674 0.1724 0.8685 0.057 Uiso 1 1 calc R . . C80 C 1.22165(19) 0.0611(4) 0.8342(2) 0.0457(12) Uani 1 1 d . . . H80A H 1.2523 0.0201 0.8348 0.055 Uiso 1 1 calc R . . C81 C 1.16794(18) 0.0303(3) 0.81330(16) 0.0347(9) Uani 1 1 d . . . H81A H 1.1618 -0.0319 0.7997 0.042 Uiso 1 1 calc R . . C82 C 1.06102(15) -0.0974(3) 0.82969(13) 0.0224(7) Uani 1 1 d . . . C83 C 1.08167(16) -0.0618(3) 0.87619(14) 0.0260(8) Uani 1 1 d . . . H83A H 1.0859 0.0052 0.8813 0.031 Uiso 1 1 calc R . . C84 C 1.09594(18) -0.1234(3) 0.91466(15) 0.0301(9) Uani 1 1 d . . . H84A H 1.1083 -0.0990 0.9464 0.036 Uiso 1 1 calc R . . C85 C 1.0921(2) -0.2218(3) 0.90676(18) 0.0316(12) Uani 1 1 d . . . H85A H 1.1028 -0.2644 0.9332 0.038 Uiso 1 1 calc R . . C86 C 1.07307(18) -0.2574(3) 0.86114(15) 0.0306(9) Uani 1 1 d . . . H86A H 1.0715 -0.3245 0.8561 0.037 Uiso 1 1 calc R . . C87 C 1.05607(16) -0.1961(3) 0.82237(15) 0.0269(8) Uani 1 1 d . . . H87A H 1.0412 -0.2210 0.7911 0.032 Uiso 1 1 calc R . . S3 S 0.06498(5) 0.72015(9) 0.49570(4) 0.0395(2) Uani 1 1 d . . . O10 O 0.03320(14) 0.6344(2) 0.48268(13) 0.0422(7) Uani 1 1 d . . . O11 O 0.05055(17) 0.7780(3) 0.53126(13) 0.0601(11) Uani 1 1 d . . . O12 O 0.12203(15) 0.7084(3) 0.49936(16) 0.0589(10) Uani 1 1 d . . . F7 F 0.0499(2) 0.7508(3) 0.40234(16) 0.0828(7) Uani 1 1 d . . . F8 F 0.0681(2) 0.8768(3) 0.44726(15) 0.0828(7) Uani 1 1 d . . . F9 F -0.0128(2) 0.8110(3) 0.43256(15) 0.0828(7) Uani 1 1 d . . . C90 C 0.0393(2) 0.7950(3) 0.44194(19) 0.0414(11) Uani 1 1 d . . . S1 S 0.75067(4) 0.75416(8) 0.56020(4) 0.0202(2) Uiso 0.80 1 d PD A 1 O4 O 0.7524(2) 0.8130(4) 0.51876(19) 0.0334(11) Uiso 0.80 1 d PD A 1 O5 O 0.80014(14) 0.7000(3) 0.57925(13) 0.0237(9) Uiso 0.80 1 d PD A 1 O6 O 0.72757(16) 0.8005(3) 0.59547(14) 0.0320(9) Uiso 0.80 1 d PD A 1 F1 F 0.71282(12) 0.6145(2) 0.50007(10) 0.0304(6) Uiso 0.80 1 d PD A 1 F2 F 0.69862(13) 0.5959(2) 0.57000(11) 0.0383(7) Uiso 0.80 1 d PD A 1 F3 F 0.64870(13) 0.6959(2) 0.52064(11) 0.0355(7) Uiso 0.80 1 d PD A 1 C88 C 0.70050(19) 0.6610(4) 0.53605(17) 0.027(1) Uiso 0.80 1 d PD A 1 S1' S 0.7460(2) 0.7268(4) 0.58886(19) 0.0317(11) Uiso 0.20 1 d PD B 2 O4' O 0.7078(6) 0.6570(11) 0.6004(6) 0.046(3) Uiso 0.20 1 d PD B 2 O5' O 0.7998(6) 0.6913(15) 0.5920(8) 0.046(3) Uiso 0.20 1 d PD B 2 O6' O 0.7424(8) 0.8225(11) 0.6060(7) 0.046(3) Uiso 0.20 1 d PD B 2 F1' F 0.6612(7) 0.7758(15) 0.5192(7) 0.076(4) Uiso 0.20 1 d PD B 2 F2' F 0.7101(8) 0.6703(14) 0.4968(7) 0.076(4) Uiso 0.20 1 d PD B 2 F3' F 0.7436(11) 0.8160(19) 0.513(1) 0.076(4) Uiso 0.20 1 d PD B 2 C88' C 0.7152(6) 0.7492(11) 0.5255(5) 0.027(1) Uiso 0.20 1 d PD B 2 S2 S 1.0055(2) -0.39073(18) 0.70675(9) 0.0177(9) Uiso 0.424(12) 1 d P C 1 O7 O 1.0178(5) -0.3895(7) 0.7579(3) 0.025(3) Uiso 0.424(12) 1 d P C 1 O8 O 0.9637(4) -0.3253(6) 0.6832(3) 0.031(2) Uiso 0.424(12) 1 d P C 1 O9 O 0.9978(4) -0.4829(5) 0.6872(3) 0.022(2) Uiso 0.424(12) 1 d P C 1 F4 F 1.0793(5) -0.2520(8) 0.7126(4) 0.072(3) Uiso 0.424(12) 1 d P C 1 F5 F 1.1154(5) -0.3879(12) 0.7139(4) 0.074(3) Uiso 0.424(12) 1 d P C 1 F6 F 1.0651(4) -0.3342(5) 0.6470(3) 0.045(2) Uiso 0.424(12) 1 d P C 1 C89 C 1.0681(6) -0.3397(9) 0.6939(4) 0.032(3) Uiso 0.424(12) 1 d P C 1 S2' S 1.0202(2) -0.38780(17) 0.70903(9) 0.0313(8) Uiso 0.576(12) 1 d P C 2 O7' O 1.0305(4) -0.3940(5) 0.7598(3) 0.031(2) Uiso 0.576(12) 1 d P C 2 O8' O 0.9848(4) -0.3098(5) 0.6859(2) 0.0440(18) Uiso 0.576(12) 1 d P C 2 O9' O 1.0125(4) -0.4787(5) 0.6832(2) 0.0318(19) Uiso 0.576(12) 1 d P C 2 F4' F 1.1038(3) -0.2752(4) 0.7259(2) 0.0548(18) Uiso 0.576(12) 1 d PD C 2 F5' F 1.1222(2) -0.4272(5) 0.71726(19) 0.0457(16) Uiso 0.576(12) 1 d PD C 2 F6' F 1.0867(4) -0.3381(5) 0.6566(2) 0.064(2) Uiso 0.576(12) 1 d PD C 2 C89' C 1.0878(5) -0.3551(6) 0.7023(3) 0.036(2) Uiso 0.576(12) 1 d PD C 2 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 0.01545(8) 0.01355(8) 0.01674(8) 0.00014(9) 0.00513(5) -0.00002(9) O1 0.0247(14) 0.0183(14) 0.0202(12) 0.0034(10) 0.0092(10) 0.0007(10) O2 0.0194(13) 0.0188(13) 0.0187(12) -0.0026(9) 0.0068(9) 0.0004(9) O3 0.0190(13) 0.0173(13) 0.0222(13) -0.0006(10) 0.0003(9) -0.0029(10) N1 0.0217(16) 0.0182(16) 0.0221(15) 0.0019(12) 0.0066(12) 0.0014(12) N2 0.0166(15) 0.0208(16) 0.0167(14) 0.0005(11) 0.0031(11) 0.0014(11) N3 0.0200(15) 0.0179(15) 0.0199(14) 0.0006(12) 0.0046(11) -0.0036(12) N4 0.0260(17) 0.0172(16) 0.0234(16) 0.0034(12) 0.0112(13) 0.0012(12) N5 0.0190(15) 0.0237(17) 0.0258(16) -0.0010(12) 0.0089(12) 0.0015(12) N6 0.0233(17) 0.0232(17) 0.0279(17) -0.0077(13) 0.0116(12) -0.0028(12) N7 0.0141(14) 0.0157(15) 0.0185(14) 0.0004(11) 0.0048(10) 0.0019(11) N8 0.0197(16) 0.0165(15) 0.0184(15) -0.0006(11) 0.0049(11) 0.0018(11) N9 0.0185(15) 0.0169(15) 0.0219(15) 0.0009(11) 0.0071(11) 0.0006(11) N10 0.0201(15) 0.0164(15) 0.0221(15) -0.0023(11) 0.0067(11) -0.0019(11) N11 0.0177(15) 0.0238(17) 0.0257(16) 0.0032(12) 0.0032(12) -0.0019(12) N12 0.0183(15) 0.0199(16) 0.0174(14) -0.0020(11) 0.0069(11) 0.0007(11) N13 0.0149(15) 0.0185(16) 0.0209(15) -0.0029(11) 0.0041(11) -0.0005(11) N14 0.0172(15) 0.0185(16) 0.0206(16) -0.0015(12) 0.0042(12) -0.0029(11) N15 0.0209(15) 0.0146(15) 0.0243(15) -0.0010(11) 0.0077(12) 0.0006(11) C1 0.032(2) 0.025(2) 0.033(2) 0.0069(16) 0.0169(17) 0.0029(16) C2 0.041(3) 0.032(2) 0.035(2) -0.0061(18) 0.0130(18) -0.0058(18) C3 0.033(3) 0.056(3) 0.042(3) -0.001(2) 0.0185(19) 0.003(2) C4 0.0207(19) 0.024(2) 0.0257(19) 0.0076(15) 0.0093(14) -0.0007(14) C5 0.029(2) 0.023(2) 0.029(2) 0.0077(15) 0.0140(15) 0.0045(15) C6 0.032(2) 0.030(2) 0.0220(19) 0.0037(15) 0.0107(15) 0.0077(16) C7 0.038(2) 0.027(2) 0.049(3) 0.0148(19) 0.0119(19) 0.0053(18) C8 0.028(2) 0.018(2) 0.037(2) 0.0014(15) 0.0074(16) -0.0021(15) C9 0.0197(18) 0.0185(19) 0.0182(17) 0.0008(13) 0.0060(13) -0.0005(13) C10 0.0237(19) 0.0200(19) 0.0207(18) 0.0003(14) 0.0061(14) 0.0015(14) C11 0.034(2) 0.034(2) 0.028(2) 0.0060(17) 0.0090(17) 0.0092(18) C12 0.037(2) 0.037(3) 0.042(2) 0.0148(19) 0.0169(19) 0.0195(19) C13 0.029(2) 0.033(2) 0.034(2) 0.0071(17) 0.0147(16) 0.0110(17) C14 0.0188(18) 0.027(2) 0.0210(18) -0.0007(14) 0.0061(13) 0.0007(14) C15 0.0155(17) 0.0207(19) 0.0204(17) -0.0032(14) 0.0042(12) -0.0031(13) C16 0.0204(18) 0.023(2) 0.0228(18) 0.0004(14) 0.0076(13) -0.0002(14) C17 0.0177(17) 0.0239(19) 0.0214(17) -0.0004(14) 0.0057(13) -0.0033(14) C18 0.044(3) 0.026(2) 0.030(2) 0.0053(16) 0.0210(18) 0.0029(17) C19 0.043(3) 0.027(2) 0.042(2) 0.0010(18) 0.0238(19) -0.0009(17) C20 0.075(4) 0.029(3) 0.064(3) 0.006(2) 0.047(3) -0.005(2) C21 0.095(4) 0.031(3) 0.056(3) 0.020(2) 0.050(3) 0.015(3) C22 0.073(4) 0.040(3) 0.038(3) 0.018(2) 0.027(2) 0.026(2) C23 0.044(3) 0.035(3) 0.033(2) 0.0082(19) 0.0192(19) 0.015(2) C24 0.027(2) 0.0182(19) 0.034(2) -0.0008(15) 0.0180(15) -0.0034(14) C25 0.025(2) 0.031(2) 0.027(2) -0.0053(15) 0.0104(15) -0.0087(15) C26 0.040(3) 0.034(3) 0.024(2) -0.0073(17) 0.0128(18) -0.0151(19) C27 0.050(3) 0.027(2) 0.038(2) -0.0009(18) 0.027(2) -0.0037(19) C28 0.040(3) 0.041(3) 0.058(3) 0.010(2) 0.030(2) 0.017(2) C29 0.033(2) 0.044(3) 0.036(2) 0.0156(19) 0.0200(18) 0.0116(19) C30 0.036(2) 0.024(2) 0.027(2) -0.0011(16) 0.0091(17) -0.0039(17) C31 0.043(3) 0.032(2) 0.029(2) -0.0029(17) 0.0056(18) -0.0059(19) C32 0.054(3) 0.039(3) 0.028(2) -0.0029(18) 0.0129(19) -0.012(2) C33 0.030(2) 0.0203(19) 0.0267(19) -0.0070(15) 0.0099(15) -0.0048(15) C34 0.029(2) 0.028(2) 0.050(3) -0.0028(19) 0.0081(18) 0.0052(17) C35 0.090(4) 0.045(3) 0.040(3) 0.009(2) 0.019(3) 0.025(3) C36 0.035(3) 0.042(3) 0.065(3) -0.006(2) 0.010(2) 0.010(2) C37 0.026(2) 0.026(2) 0.039(2) -0.0116(17) 0.0149(16) -0.0003(15) C38 0.025(2) 0.0201(19) 0.0160(17) 0.0037(14) 0.0103(14) 0.0012(14) C39 0.0194(18) 0.0193(19) 0.0195(17) 0.0013(13) 0.0091(13) 0.0022(13) C40 0.032(2) 0.024(2) 0.033(2) -0.0037(16) 0.0182(16) -0.0022(16) C41 0.027(2) 0.028(2) 0.041(2) -0.0076(17) 0.0195(17) -0.0115(16) C42 0.028(2) 0.028(2) 0.036(2) -0.0074(17) 0.0152(16) -0.0072(16) C43 0.0224(18) 0.0153(18) 0.0184(17) -0.0009(13) 0.0071(13) -0.0012(13) C44 0.0191(18) 0.0118(17) 0.0217(17) -0.0017(13) 0.0070(13) -0.0027(13) C45 0.0198(18) 0.0139(17) 0.0181(17) -0.0017(13) 0.0047(13) -0.0003(13) C46 0.0227(18) 0.0145(17) 0.0158(16) 0.0032(13) 0.0049(13) 0.0002(13) C47 0.0206(18) 0.028(2) 0.0190(18) -0.0034(14) 0.0053(13) -0.0020(14) C48 0.037(2) 0.034(2) 0.037(2) -0.0133(18) 0.0214(19) -0.0117(18) C49 0.041(3) 0.053(3) 0.035(2) -0.015(2) 0.0195(19) -0.017(2) C50 0.035(2) 0.048(3) 0.031(2) -0.0085(19) 0.0146(18) 0.0044(19) C51 0.043(3) 0.033(2) 0.035(2) -0.0041(18) 0.0157(18) 0.0086(18) C52 0.031(2) 0.028(2) 0.029(2) -0.0047(16) 0.0099(16) 0.0019(16) C53 0.0226(19) 0.0159(18) 0.0226(18) -0.0028(13) 0.0033(14) 0.0008(13) C54 0.025(2) 0.022(2) 0.027(2) 0.0021(15) 0.0054(15) -0.0005(14) C55 0.034(2) 0.031(2) 0.0204(19) 0.0001(15) 0.0037(15) 0.0059(16) C56 0.028(2) 0.038(2) 0.027(2) -0.0106(17) -0.0032(15) 0.0000(17) C57 0.019(2) 0.036(2) 0.037(2) -0.0115(18) 0.0037(16) -0.0073(16) C58 0.029(2) 0.028(2) 0.0258(19) -0.0089(15) 0.0093(15) -0.0055(16) C59 0.031(2) 0.040(3) 0.044(3) 0.017(2) -0.0020(18) -0.0092(18) C60 0.057(3) 0.040(3) 0.052(3) 0.017(2) -0.009(2) -0.010(2) C61 0.068(4) 0.047(3) 0.037(3) 0.014(2) 0.017(2) 0.005(2) C62 0.0191(19) 0.024(2) 0.038(2) 0.0085(17) -0.0001(15) 0.0006(15) C63 0.025(2) 0.034(2) 0.041(2) 0.0032(18) 0.0101(17) -0.0026(17) C64 0.037(3) 0.104(5) 0.037(3) 0.008(3) 0.012(2) -0.006(3) C65 0.025(2) 0.041(3) 0.064(3) 0.004(2) 0.016(2) -0.0090(18) C66 0.0166(18) 0.023(2) 0.035(2) 0.0027(15) 0.0016(14) -0.0039(14) C67 0.0171(18) 0.022(2) 0.0172(18) -0.0003(14) 0.0027(13) 0.0003(14) C68 0.0197(18) 0.0157(18) 0.0196(18) -0.0007(13) 0.0033(13) -0.0008(13) C69 0.0229(19) 0.024(2) 0.0215(19) -0.0012(14) 0.0022(14) -0.0023(14) C70 0.029(2) 0.019(2) 0.034(2) -0.0054(15) 0.0046(16) -0.0007(15) C71 0.027(2) 0.019(2) 0.027(2) 0.0014(15) 0.0042(17) -0.0001(13) C72 0.0174(17) 0.0203(19) 0.0181(17) 0.0010(13) 0.0045(13) -0.0013(13) C73 0.0178(18) 0.0164(18) 0.0190(17) -0.0009(13) 0.0065(13) 0.0008(13) C74 0.0212(18) 0.0163(18) 0.0197(17) -0.0005(13) 0.0043(13) 0.0013(13) C75 0.0198(18) 0.0182(19) 0.0233(18) -0.0019(14) 0.0059(14) 0.0033(13) C76 0.0228(19) 0.022(2) 0.0226(19) 0.0049(14) -0.0014(14) -0.0024(14) C77 0.035(2) 0.024(2) 0.027(2) 0.0052(16) -0.0031(17) -0.0042(16) C78 0.042(3) 0.033(3) 0.041(3) -0.0014(19) -0.0040(19) -0.0143(19) C79 0.028(2) 0.052(3) 0.053(3) -0.001(2) -0.007(2) -0.009(2) C80 0.024(2) 0.046(3) 0.058(3) 0.000(2) -0.005(2) 0.0025(19) C81 0.028(2) 0.032(2) 0.040(2) 0.0021(18) 0.0008(17) -0.0002(17) C82 0.0212(19) 0.022(2) 0.0240(19) 0.0026(14) 0.0065(14) 0.0005(14) C83 0.028(2) 0.022(2) 0.030(2) 0.0011(15) 0.0099(15) 0.0036(15) C84 0.035(2) 0.029(2) 0.025(2) 0.0016(16) 0.0058(16) 0.0020(16) C85 0.030(3) 0.036(3) 0.028(2) 0.0157(18) 0.0055(18) 0.0045(18) C86 0.031(2) 0.025(2) 0.035(2) 0.0047(16) 0.0065(16) -0.0002(16) C87 0.025(2) 0.022(2) 0.031(2) 0.0029(15) 0.0030(15) 0.0004(14) S3 0.0336(6) 0.0362(6) 0.0483(6) -0.0058(5) 0.0095(4) 0.0003(4) O10 0.0429(19) 0.0354(18) 0.0523(19) -0.0049(15) 0.0193(14) -0.0071(14) O11 0.056(2) 0.078(3) 0.044(2) -0.0161(19) 0.0082(16) 0.012(2) O12 0.035(2) 0.054(3) 0.085(3) -0.011(2) 0.0121(18) 0.0006(16) F7 0.115(2) 0.0615(14) 0.0816(16) 0.0169(11) 0.0423(13) 0.0255(13) F8 0.115(2) 0.0615(14) 0.0816(16) 0.0169(11) 0.0423(13) 0.0255(13) F9 0.115(2) 0.0615(14) 0.0816(16) 0.0169(11) 0.0423(13) 0.0255(13) C90 0.062(3) 0.022(2) 0.053(3) 0.0055(19) 0.036(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.238(2) . ? Yb1 O3 2.281(2) . ? Yb1 O2 2.293(2) . ? Yb1 N7 2.459(3) . ? Yb1 N2 2.462(3) . ? Yb1 N3 2.467(3) . ? Yb1 N8 2.469(3) . ? Yb1 N13 2.487(3) . ? Yb1 N12 2.490(3) . ? Yb1 C67 3.184(4) . ? Yb1 C9 3.191(4) . ? Yb1 C38 3.194(4) . ? O1 C9 1.262(5) . ? O2 C38 1.270(5) . ? O3 C67 1.256(5) . ? N1 C9 1.319(5) . ? N1 C8 1.480(5) . ? N1 C4 1.484(5) . ? N2 C14 1.340(5) . ? N2 C10 1.346(5) . ? N3 C15 1.326(5) . ? N3 N4 1.334(4) . ? N4 C16 1.334(5) . ? N5 C17 1.331(5) . ? N5 C15 1.341(5) . ? N6 C38 1.326(5) . ? N6 C37 1.482(5) . ? N6 C33 1.489(5) . ? N7 C43 1.340(5) . ? N7 C39 1.347(5) . ? N8 C44 1.332(5) . ? N8 N9 1.340(4) . ? N9 C45 1.325(5) . ? N10 C46 1.326(5) . ? N10 C44 1.340(5) . ? N11 C67 1.334(5) . ? N11 C66 1.466(5) . ? N11 C62 1.481(5) . ? N12 C72 1.337(5) . ? N12 C68 1.344(5) . ? N13 C73 1.331(5) . ? N13 N14 1.349(4) . ? N14 C74 1.328(5) . ? N15 C73 1.331(5) . ? N15 C75 1.332(5) . ? C1 C2 1.520(6) . ? C1 C4 1.528(6) . ? C1 C3 1.532(6) . ? C1 H1A 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C8 1.523(6) . ? C5 C7 1.524(6) . ? C5 C6 1.529(6) . ? C5 H5A 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.528(5) . ? C10 C11 1.381(6) . ? C11 C12 1.396(6) . ? C11 H11A 0.9500 . ? C12 C13 1.383(6) . ? C12 H12A 0.9500 . ? C13 C14 1.382(6) . ? C13 H13A 0.9500 . ? C14 C15 1.487(5) . ? C16 C17 1.433(5) . ? C16 C18 1.485(5) . ? C17 C24 1.477(5) . ? C18 C19 1.386(6) . ? C18 C23 1.393(6) . ? C19 C20 1.393(7) . ? C19 H19A 0.9500 . ? C20 C21 1.380(8) . ? C20 H20A 0.9500 . ? C21 C22 1.373(9) . ? C21 H21A 0.9500 . ? C22 C23 1.393(7) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C29 1.371(6) . ? C24 C25 1.405(6) . ? C25 C26 1.394(6) . ? C25 H25A 0.9500 . ? C26 C27 1.370(8) . ? C26 H26A 0.9500 . ? C27 C28 1.377(7) . ? C27 H27A 0.9500 . ? C28 C29 1.391(6) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.521(6) . ? C30 C32 1.534(6) . ? C30 C33 1.536(6) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C36 1.524(6) . ? C34 C37 1.525(6) . ? C34 C35 1.529(7) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.502(5) . ? C39 C40 1.395(6) . ? C40 C41 1.380(6) . ? C40 H40A 0.9500 . ? C41 C42 1.382(6) . ? C41 H41A 0.9500 . ? C42 C43 1.382(6) . ? C42 H42A 0.9500 . ? C43 C44 1.481(5) . ? C45 C46 1.434(5) . ? C45 C47 1.489(5) . ? C46 C53 1.487(5) . ? C47 C52 1.386(6) . ? C47 C48 1.388(6) . ? C48 C49 1.397(6) . ? C48 H48A 0.9500 . ? C49 C50 1.365(7) . ? C49 H49A 0.9500 . ? C50 C51 1.380(7) . ? C50 H50A 0.9500 . ? C51 C52 1.394(6) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 C54 1.384(6) . ? C53 C58 1.394(6) . ? C54 C55 1.392(6) . ? C54 H54A 0.9500 . ? C55 C56 1.385(7) . ? C55 H55A 0.9500 . ? C56 C57 1.379(6) . ? C56 H56A 0.9500 . ? C57 C58 1.390(6) . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? C59 C62 1.517(6) . ? C59 C61 1.522(8) . ? C59 C60 1.540(7) . ? C59 H59A 1.0000 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C66 1.528(6) . ? C63 C65 1.533(6) . ? C63 C64 1.538(7) . ? C63 H63A 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.511(5) . ? C68 C69 1.380(5) . ? C69 C70 1.395(6) . ? C69 H69A 0.9500 . ? C70 C71 1.379(6) . ? C70 H70A 0.9500 . ? C71 C72 1.393(5) . ? C71 H71A 0.9500 . ? C72 C73 1.483(5) . ? C74 C75 1.430(5) . ? C74 C76 1.483(5) . ? C75 C82 1.464(5) . ? C76 C81 1.387(6) . ? C76 C77 1.391(6) . ? C77 C78 1.387(6) . ? C77 H77A 0.9500 . ? C78 C79 1.389(8) . ? C78 H78A 0.9500 . ? C79 C80 1.384(8) . ? C79 H79A 0.9500 . ? C80 C81 1.386(6) . ? C80 H80A 0.9500 . ? C81 H81A 0.9500 . ? C82 C87 1.398(6) . ? C82 C83 1.399(6) . ? C83 C84 1.377(6) . ? C83 H83A 0.9500 . ? C84 C85 1.394(7) . ? C84 H84A 0.9500 . ? C85 C86 1.373(7) . ? C85 H85A 0.9500 . ? C86 C87 1.386(6) . ? C86 H86A 0.9500 . ? C87 H87A 0.9500 . ? S3 O12 1.405(4) . ? S3 O11 1.421(4) . ? S3 O10 1.432(3) . ? S3 C90 1.843(5) . ? F7 C90 1.381(6) . ? F8 C90 1.338(7) . ? F9 C90 1.275(7) . ? S1 O5 1.429(3) . ? S1 O6 1.443(4) . ? S1 O4 1.460(5) . ? S1 C88 1.815(5) . ? F1 C88 1.325(6) . ? F2 C88 1.346(6) . ? F3 C88 1.342(6) . ? S1' O5' 1.407(14) . ? S1' O6' 1.437(14) . ? S1' O4' 1.458(13) . ? S1' C88' 1.817(13) . ? F1' C88' 1.359(17) . ? F2' C88' 1.366(17) . ? F3' C88' 1.277(18) . ? S2 O9 1.401(8) . ? S2 O8 1.420(9) . ? S2 O7 1.427(9) . ? S2 C89 1.831(13) . ? F4 C89 1.341(15) . ? F5 C89 1.350(17) . ? F6 C89 1.339(13) . ? S2' O7' 1.423(8) . ? S2' O8' 1.452(7) . ? S2' O9' 1.460(7) . ? S2' C89' 1.800(11) . ? F4' C89' 1.316(9) . ? F5' C89' 1.321(12) . ? F6' C89' 1.334(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O3 80.88(9) . . ? O1 Yb1 O2 79.25(9) . . ? O3 Yb1 O2 79.82(9) . . ? O1 Yb1 N7 71.26(9) . . ? O3 Yb1 N7 138.65(9) . . ? O2 Yb1 N7 65.65(9) . . ? O1 Yb1 N2 65.30(9) . . ? O3 Yb1 N2 71.72(9) . . ? O2 Yb1 N2 137.11(9) . . ? N7 Yb1 N2 119.66(10) . . ? O1 Yb1 N3 130.76(9) . . ? O3 Yb1 N3 85.04(9) . . ? O2 Yb1 N3 143.57(9) . . ? N7 Yb1 N3 136.31(9) . . ? N2 Yb1 N3 65.47(10) . . ? O1 Yb1 N8 88.75(10) . . ? O3 Yb1 N8 145.1(1) . . ? O2 Yb1 N8 130.96(9) . . ? N7 Yb1 N8 65.45(10) . . ? N2 Yb1 N8 73.66(9) . . ? N3 Yb1 N8 76.76(10) . . ? O1 Yb1 N13 142.99(9) . . ? O3 Yb1 N13 129.56(9) . . ? O2 Yb1 N13 85.77(9) . . ? N7 Yb1 N13 71.73(9) . . ? N2 Yb1 N13 137.12(10) . . ? N3 Yb1 N13 78.71(10) . . ? N8 Yb1 N13 75.9(1) . . ? O1 Yb1 N12 136.85(9) . . ? O3 Yb1 N12 65.36(9) . . ? O2 Yb1 N12 69.34(9) . . ? N7 Yb1 N12 117.85(9) . . ? N2 Yb1 N12 122.48(10) . . ? N3 Yb1 N12 74.23(10) . . ? N8 Yb1 N12 134.23(10) . . ? N13 Yb1 N12 64.3(1) . . ? O1 Yb1 C67 97.98(9) . . ? O3 Yb1 C67 18.66(9) . . ? O2 Yb1 C67 75.77(9) . . ? N7 Yb1 C67 141.16(10) . . ? N2 Yb1 C67 85.67(9) . . ? N3 Yb1 C67 79.34(10) . . ? N8 Yb1 C67 153.27(10) . . ? N13 Yb1 C67 110.91(10) . . ? N12 Yb1 C67 46.76(10) . . ? O1 Yb1 C9 17.83(9) . . ? O3 Yb1 C9 76.96(9) . . ? O2 Yb1 C9 95.69(9) . . ? N7 Yb1 C9 84.27(9) . . ? N2 Yb1 C9 47.48(9) . . ? N3 Yb1 C9 112.93(10) . . ? N8 Yb1 C9 83.05(9) . . ? N13 Yb1 C9 152.98(9) . . ? N12 Yb1 C9 141.12(9) . . ? C67 Yb1 C9 95.51(9) . . ? O1 Yb1 C38 77.25(9) . . ? O3 Yb1 C38 98.18(9) . . ? O2 Yb1 C38 19.03(9) . . ? N7 Yb1 C38 46.84(10) . . ? N2 Yb1 C38 142.18(9) . . ? N3 Yb1 C38 151.76(10) . . ? N8 Yb1 C38 111.95(10) . . ? N13 Yb1 C38 77.73(9) . . ? N12 Yb1 C38 81.63(9) . . ? C67 Yb1 C38 94.78(10) . . ? C9 Yb1 C38 95.04(9) . . ? C9 O1 Yb1 129.3(2) . . ? C38 O2 Yb1 124.9(2) . . ? C67 O3 Yb1 125.8(2) . . ? C9 N1 C8 127.4(3) . . ? C9 N1 C4 116.9(3) . . ? C8 N1 C4 113.9(3) . . ? C14 N2 C10 119.4(3) . . ? C14 N2 Yb1 120.6(2) . . ? C10 N2 Yb1 118.8(2) . . ? C15 N3 N4 119.1(3) . . ? C15 N3 Yb1 120.9(2) . . ? N4 N3 Yb1 120.0(2) . . ? C16 N4 N3 119.6(3) . . ? C17 N5 C15 116.8(3) . . ? C38 N6 C37 125.7(3) . . ? C38 N6 C33 117.4(3) . . ? C37 N6 C33 115.1(3) . . ? C43 N7 C39 119.2(3) . . ? C43 N7 Yb1 119.9(2) . . ? C39 N7 Yb1 118.6(2) . . ? C44 N8 N9 118.1(3) . . ? C44 N8 Yb1 120.0(2) . . ? N9 N8 Yb1 121.8(2) . . ? C45 N9 N8 120.0(3) . . ? C46 N10 C44 117.2(3) . . ? C67 N11 C66 127.0(3) . . ? C67 N11 C62 116.8(3) . . ? C66 N11 C62 115.1(3) . . ? C72 N12 C68 118.5(3) . . ? C72 N12 Yb1 120.0(2) . . ? C68 N12 Yb1 117.3(2) . . ? C73 N13 N14 117.7(3) . . ? C73 N13 Yb1 121.6(2) . . ? N14 N13 Yb1 120.2(2) . . ? C74 N14 N13 119.5(3) . . ? C73 N15 C75 116.9(3) . . ? C2 C1 C4 114.0(3) . . ? C2 C1 C3 111.1(4) . . ? C4 C1 C3 108.1(4) . . ? C2 C1 H1A 107.8 . . ? C4 C1 H1A 107.8 . . ? C3 C1 H1A 107.8 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C1 115.6(3) . . ? N1 C4 H4A 108.4 . . ? C1 C4 H4A 108.4 . . ? N1 C4 H4B 108.4 . . ? C1 C4 H4B 108.4 . . ? H4A C4 H4B 107.4 . . ? C8 C5 C7 109.4(3) . . ? C8 C5 C6 112.4(3) . . ? C7 C5 C6 110.9(3) . . ? C8 C5 H5A 108.0 . . ? C7 C5 H5A 108.0 . . ? C6 C5 H5A 108.0 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C5 112.9(3) . . ? N1 C8 H8A 109.0 . . ? C5 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C5 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? O1 C9 N1 119.7(3) . . ? O1 C9 C10 114.0(3) . . ? N1 C9 C10 126.3(3) . . ? O1 C9 Yb1 32.88(16) . . ? N1 C9 Yb1 152.1(3) . . ? C10 C9 Yb1 81.5(2) . . ? N2 C10 C11 121.5(3) . . ? N2 C10 C9 111.0(3) . . ? C11 C10 C9 127.3(3) . . ? C10 C11 C12 118.5(4) . . ? C10 C11 H11A 120.8 . . ? C12 C11 H11A 120.8 . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C14 C13 C12 118.0(4) . . ? C14 C13 H13A 121.0 . . ? C12 C13 H13A 121.0 . . ? N2 C14 C13 122.4(4) . . ? N2 C14 C15 115.7(3) . . ? C13 C14 C15 121.8(3) . . ? N3 C15 N5 125.0(3) . . ? N3 C15 C14 116.4(3) . . ? N5 C15 C14 118.6(3) . . ? N4 C16 C17 119.8(3) . . ? N4 C16 C18 115.0(3) . . ? C17 C16 C18 125.2(3) . . ? N5 C17 C16 119.2(3) . . ? N5 C17 C24 117.0(3) . . ? C16 C17 C24 123.8(3) . . ? C19 C18 C23 119.9(4) . . ? C19 C18 C16 121.3(4) . . ? C23 C18 C16 118.7(4) . . ? C18 C19 C20 119.5(5) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C21 C20 C19 120.6(5) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C22 C21 C20 119.9(5) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.4(5) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C23 C18 119.6(5) . . ? C22 C23 H23A 120.2 . . ? C18 C23 H23A 120.2 . . ? C29 C24 C25 118.8(4) . . ? C29 C24 C17 120.4(4) . . ? C25 C24 C17 120.7(4) . . ? C26 C25 C24 120.1(4) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C27 C26 C25 120.1(5) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C28 120.0(4) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C27 C28 C29 120.3(4) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C24 C29 C28 120.6(4) . . ? C24 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C31 C30 C32 111.6(4) . . ? C31 C30 C33 108.6(3) . . ? C32 C30 C33 110.8(4) . . ? C31 C30 H30A 108.6 . . ? C32 C30 H30A 108.6 . . ? C33 C30 H30A 108.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N6 C33 C30 112.2(3) . . ? N6 C33 H33A 109.2 . . ? C30 C33 H33A 109.2 . . ? N6 C33 H33B 109.2 . . ? C30 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C36 C34 C37 109.2(4) . . ? C36 C34 C35 111.1(4) . . ? C37 C34 C35 110.6(4) . . ? C36 C34 H34A 108.6 . . ? C37 C34 H34A 108.6 . . ? C35 C34 H34A 108.6 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N6 C37 C34 113.2(3) . . ? N6 C37 H37A 108.9 . . ? C34 C37 H37A 108.9 . . ? N6 C37 H37B 108.9 . . ? C34 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? O2 C38 N6 119.4(3) . . ? O2 C38 C39 115.6(3) . . ? N6 C38 C39 125.0(3) . . ? O2 C38 Yb1 36.07(16) . . ? N6 C38 Yb1 152.0(3) . . ? C39 C38 Yb1 81.5(2) . . ? N7 C39 C40 121.0(3) . . ? N7 C39 C38 110.8(3) . . ? C40 C39 C38 128.0(3) . . ? C41 C40 C39 118.7(4) . . ? C41 C40 H40A 120.6 . . ? C39 C40 H40A 120.6 . . ? C40 C41 C42 120.1(4) . . ? C40 C41 H41A 119.9 . . ? C42 C41 H41A 119.9 . . ? C43 C42 C41 117.9(4) . . ? C43 C42 H42A 121.0 . . ? C41 C42 H42A 121.0 . . ? N7 C43 C42 122.7(3) . . ? N7 C43 C44 115.2(3) . . ? C42 C43 C44 122.2(3) . . ? N8 C44 N10 125.2(3) . . ? N8 C44 C43 116.9(3) . . ? N10 C44 C43 117.8(3) . . ? N9 C45 C46 120.1(3) . . ? N9 C45 C47 114.2(3) . . ? C46 C45 C47 125.7(3) . . ? N10 C46 C45 118.8(3) . . ? N10 C46 C53 115.0(3) . . ? C45 C46 C53 126.1(3) . . ? C52 C47 C48 119.6(4) . . ? C52 C47 C45 120.9(3) . . ? C48 C47 C45 119.4(4) . . ? C47 C48 C49 119.8(4) . . ? C47 C48 H48A 120.1 . . ? C49 C48 H48A 120.1 . . ? C50 C49 C48 120.6(4) . . ? C50 C49 H49A 119.7 . . ? C48 C49 H49A 119.7 . . ? C49 C50 C51 120.0(4) . . ? C49 C50 H50A 120.0 . . ? C51 C50 H50A 120.0 . . ? C50 C51 C52 120.3(4) . . ? C50 C51 H51A 119.8 . . ? C52 C51 H51A 119.8 . . ? C47 C52 C51 119.8(4) . . ? C47 C52 H52A 120.1 . . ? C51 C52 H52A 120.1 . . ? C54 C53 C58 119.7(3) . . ? C54 C53 C46 122.6(3) . . ? C58 C53 C46 117.5(3) . . ? C53 C54 C55 120.1(4) . . ? C53 C54 H54A 119.9 . . ? C55 C54 H54A 119.9 . . ? C56 C55 C54 119.7(4) . . ? C56 C55 H55A 120.2 . . ? C54 C55 H55A 120.2 . . ? C57 C56 C55 120.6(4) . . ? C57 C56 H56A 119.7 . . ? C55 C56 H56A 119.7 . . ? C56 C57 C58 119.7(4) . . ? C56 C57 H57A 120.1 . . ? C58 C57 H57A 120.1 . . ? C57 C58 C53 120.1(4) . . ? C57 C58 H58A 119.9 . . ? C53 C58 H58A 119.9 . . ? C62 C59 C61 111.1(4) . . ? C62 C59 C60 107.8(5) . . ? C61 C59 C60 110.7(4) . . ? C62 C59 H59A 109.1 . . ? C61 C59 H59A 109.1 . . ? C60 C59 H59A 109.1 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N11 C62 C59 113.4(4) . . ? N11 C62 H62A 108.9 . . ? C59 C62 H62A 108.9 . . ? N11 C62 H62B 108.9 . . ? C59 C62 H62B 108.9 . . ? H62A C62 H62B 107.7 . . ? C66 C63 C65 107.9(4) . . ? C66 C63 C64 110.5(4) . . ? C65 C63 C64 112.1(4) . . ? C66 C63 H63A 108.7 . . ? C65 C63 H63A 108.7 . . ? C64 C63 H63A 108.7 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N11 C66 C63 112.6(3) . . ? N11 C66 H66A 109.1 . . ? C63 C66 H66A 109.1 . . ? N11 C66 H66B 109.1 . . ? C63 C66 H66B 109.1 . . ? H66A C66 H66B 107.8 . . ? O3 C67 N11 119.7(3) . . ? O3 C67 C68 116.2(3) . . ? N11 C67 C68 124.2(3) . . ? O3 C67 Yb1 35.51(16) . . ? N11 C67 Yb1 152.1(3) . . ? C68 C67 Yb1 82.02(19) . . ? N12 C68 C69 122.0(3) . . ? N12 C68 C67 109.9(3) . . ? C69 C68 C67 127.7(3) . . ? C68 C69 C70 118.5(3) . . ? C68 C69 H69A 120.8 . . ? C70 C69 H69A 120.8 . . ? C71 C70 C69 120.2(4) . . ? C71 C70 H70A 119.9 . . ? C69 C70 H70A 119.9 . . ? C70 C71 C72 117.2(4) . . ? C70 C71 H71A 121.4 . . ? C72 C71 H71A 121.4 . . ? N12 C72 C71 123.4(3) . . ? N12 C72 C73 115.3(3) . . ? C71 C72 C73 121.1(3) . . ? N13 C73 N15 125.4(3) . . ? N13 C73 C72 115.5(3) . . ? N15 C73 C72 119.0(3) . . ? N14 C74 C75 119.8(3) . . ? N14 C74 C76 114.4(3) . . ? C75 C74 C76 125.7(3) . . ? N15 C75 C74 118.5(3) . . ? N15 C75 C82 117.4(3) . . ? C74 C75 C82 123.9(3) . . ? C81 C76 C77 119.9(4) . . ? C81 C76 C74 120.1(4) . . ? C77 C76 C74 119.7(4) . . ? C78 C77 C76 120.1(4) . . ? C78 C77 H77A 120.0 . . ? C76 C77 H77A 120.0 . . ? C77 C78 C79 119.6(5) . . ? C77 C78 H78A 120.2 . . ? C79 C78 H78A 120.2 . . ? C80 C79 C78 120.4(4) . . ? C80 C79 H79A 119.8 . . ? C78 C79 H79A 119.8 . . ? C79 C80 C81 120.0(5) . . ? C79 C80 H80A 120.0 . . ? C81 C80 H80A 120.0 . . ? C80 C81 C76 120.0(4) . . ? C80 C81 H81A 120.0 . . ? C76 C81 H81A 120.0 . . ? C87 C82 C83 119.5(3) . . ? C87 C82 C75 120.3(3) . . ? C83 C82 C75 120.1(3) . . ? C84 C83 C82 120.3(4) . . ? C84 C83 H83A 119.8 . . ? C82 C83 H83A 119.8 . . ? C83 C84 C85 119.6(4) . . ? C83 C84 H84A 120.2 . . ? C85 C84 H84A 120.2 . . ? C86 C85 C84 120.5(4) . . ? C86 C85 H85A 119.8 . . ? C84 C85 H85A 119.8 . . ? C85 C86 C87 120.5(4) . . ? C85 C86 H86A 119.7 . . ? C87 C86 H86A 119.7 . . ? C86 C87 C82 119.5(4) . . ? C86 C87 H87A 120.3 . . ? C82 C87 H87A 120.3 . . ? O12 S3 O11 116.6(2) . . ? O12 S3 O10 113.6(2) . . ? O11 S3 O10 116.2(3) . . ? O12 S3 C90 104.8(3) . . ? O11 S3 C90 100.7(2) . . ? O10 S3 C90 101.9(2) . . ? F9 C90 F8 111.0(4) . . ? F9 C90 F7 107.5(5) . . ? F8 C90 F7 105.6(4) . . ? F9 C90 S3 113.2(3) . . ? F8 C90 S3 109.2(4) . . ? F7 C90 S3 110.0(3) . . ? O5 S1 O6 115.2(2) . . ? O5 S1 O4 114.2(3) . . ? O6 S1 O4 115.0(3) . . ? O5 S1 C88 101.9(2) . . ? O6 S1 C88 103.6(2) . . ? O4 S1 C88 104.6(2) . . ? F1 C88 F3 108.3(4) . . ? F1 C88 F2 107.1(4) . . ? F3 C88 F2 106.1(4) . . ? F1 C88 S1 112.3(3) . . ? F3 C88 S1 111.9(3) . . ? F2 C88 S1 110.8(3) . . ? O5' S1' O6' 116.6(12) . . ? O5' S1' O4' 114.4(11) . . ? O6' S1' O4' 116.4(11) . . ? O5' S1' C88' 106.(1) . . ? O6' S1' C88' 97.9(9) . . ? O4' S1' C88' 102.3(8) . . ? F3' C88' F1' 111.1(18) . . ? F3' C88' F2' 113.1(19) . . ? F1' C88' F2' 101.7(15) . . ? F3' C88' S1' 106.8(15) . . ? F1' C88' S1' 109.4(12) . . ? F2' C88' S1' 114.8(13) . . ? O9 S2 O8 113.1(5) . . ? O9 S2 O7 113.5(5) . . ? O8 S2 O7 115.0(5) . . ? O9 S2 C89 108.2(6) . . ? O8 S2 C89 102.0(6) . . ? O7 S2 C89 103.6(6) . . ? F6 C89 F4 107.8(10) . . ? F6 C89 F5 106.1(10) . . ? F4 C89 F5 102.5(11) . . ? F6 C89 S2 113.4(9) . . ? F4 C89 S2 112.1(9) . . ? F5 C89 S2 114.3(9) . . ? O7' S2' O8' 116.5(4) . . ? O7' S2' O9' 115.9(4) . . ? O8' S2' O9' 115.8(4) . . ? O7' S2' C89' 101.4(5) . . ? O8' S2' C89' 103.5(5) . . ? O9' S2' C89' 99.8(4) . . ? F4' C89' F5' 113.3(10) . . ? F4' C89' F6' 106.7(7) . . ? F5' C89' F6' 107.8(8) . . ? F4' C89' S2' 109.1(7) . . ? F5' C89' S2' 108.4(6) . . ? F6' C89' S2' 111.6(8) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.747 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.060 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.312 0.216 0.744 155 36 ' ' 2 0.812 0.284 0.244 155 36 ' ' 3 0.812 0.716 0.744 155 36 ' ' 4 0.312 0.784 0.244 155 36 ' ' _platon_squeeze_details ; ; data_yb12 _database_code_depnum_ccdc_archive 'CCDC 889307' #TrackingRef 'web_deposit_cif_file_0_GaryGuillet_1349827628.gg20.cif' # # xray code for Yb12 is gg20 # _vrf_PLAT214_I ; PROBLEM: Atom O8 (Anion/Solvent) ADP max/min Ratio 8.7 prola RESPONSE: Disorder could not be resolved. ; _audit_update_record ; 2012-09-24 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C105 H69 N21 Yb1, 3(CO3F3S), 3(CH4O1), 1(H2O)' _chemical_formula_sum 'C111 H83 F9 N21 O13 S3 Yb' _chemical_formula_weight 2359.20 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6476(9) _cell_length_b 16.3938(10) _cell_length_c 23.0054(14) _cell_angle_alpha 88.0360(10) _cell_angle_beta 89.2040(10) _cell_angle_gamma 82.5580(10) _cell_volume 5100.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9936 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description colorless _exptl_crystal_colour blocks _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2398 _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7824 _exptl_absorpt_correction_T_max 0.8859 _exptl_absorpt_process_details 'based on measured indexed crystal faces, Bruker SHELXTL v6.14 (Bruker 2008)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II DUO' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 66581 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 23419 _reflns_number_gt 20270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT (Bruker, 2008)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The following restraints were employed in the final refinement model. yb12 eadp o7' o8' o9' f7' f8' f9' s3' c118 dfix 1.902 0.02 s3' c118 dfix 1.462 0.02 s3' o7' s3' o8' s3' o9' dfix 1.341 0.02 c118 f7' c118 f8' c118 f9' dfix 2.633 0.02 c118 o7' c118 o8' c118 o9' dfix 2.748 0.02 s3' f7' s3' f8' s3' f9' ; _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^)+(0.0496P)^2^+1.7613P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23419 _refine_ls_number_parameters 1451 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.005 _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 0.260965(8) 1.097572(6) 0.267119(4) 0.01196(4) Uani 1 1 d . . . N1 N 0.27488(15) 1.08499(12) 0.16045(8) 0.0132(4) Uani 1 1 d . . . N2 N 0.37718(15) 1.18417(12) 0.21877(9) 0.0145(4) Uani 1 1 d . . . N3 N 0.43181(15) 1.22963(12) 0.24985(9) 0.0157(4) Uani 1 1 d . . . N4 N 0.44962(16) 1.22782(13) 0.13076(9) 0.0171(4) Uani 1 1 d . . . N5 N 0.16980(15) 0.98933(12) 0.22536(8) 0.0136(4) Uani 1 1 d . . . N6 N 0.11195(15) 0.93349(12) 0.14083(9) 0.0149(4) Uani 1 1 d . . . N7 N 0.13162(15) 0.93228(12) 0.25892(9) 0.0151(4) Uani 1 1 d . . . N8 N 0.09413(15) 1.11012(12) 0.30997(8) 0.0135(4) Uani 1 1 d . . . N9 N 0.24103(16) 1.00188(12) 0.34917(9) 0.0165(4) Uani 1 1 d . . . N10 N 0.31097(17) 0.93695(13) 0.35747(9) 0.0193(5) Uani 1 1 d . . . N11 N 0.13479(17) 0.94547(13) 0.41736(9) 0.0174(4) Uani 1 1 d . . . N12 N 0.14195(15) 1.20519(12) 0.22103(8) 0.0136(4) Uani 1 1 d . . . N13 N 0.16863(16) 1.25007(12) 0.17468(8) 0.0149(4) Uani 1 1 d . . . N14 N -0.01667(16) 1.28310(12) 0.22375(9) 0.0150(4) Uani 1 1 d . . . N15 N 0.40602(15) 1.09492(12) 0.32914(8) 0.0144(4) Uani 1 1 d . . . N16 N 0.39586(16) 0.98444(12) 0.24678(8) 0.0147(4) Uani 1 1 d . . . N17 N 0.39381(16) 0.93341(12) 0.20242(9) 0.0160(4) Uani 1 1 d . . . N18 N 0.54418(16) 0.90798(13) 0.28127(9) 0.0180(4) Uani 1 1 d . . . N19 N 0.25319(15) 1.21425(12) 0.33409(8) 0.0149(4) Uani 1 1 d . . . N20 N 0.17351(16) 1.27158(12) 0.33783(9) 0.0157(4) Uani 1 1 d . . . N21 N 0.33722(16) 1.28335(13) 0.40312(9) 0.0175(4) Uani 1 1 d . . . C1 C 0.22064(18) 1.03749(15) 0.13165(10) 0.0154(5) Uani 1 1 d . . . C2 C 0.2178(2) 1.03639(17) 0.07140(11) 0.0236(6) Uani 1 1 d . . . H2A H 0.1771 1.0028 0.0525 0.028 Uiso 1 1 calc R . . C3 C 0.2754(2) 1.08523(19) 0.03965(12) 0.0303(7) Uani 1 1 d . . . H3A H 0.2747 1.0861 -0.0017 0.036 Uiso 1 1 calc R . . C4 C 0.3343(2) 1.13287(18) 0.06832(11) 0.0252(6) Uani 1 1 d . . . H4A H 0.3761 1.1656 0.0473 0.030 Uiso 1 1 calc R . . C5 C 0.33098(19) 1.13179(15) 0.12864(10) 0.0160(5) Uani 1 1 d . . . C6 C 0.38989(18) 1.18378(15) 0.16154(10) 0.0152(5) Uani 1 1 d . . . C7 C 0.50231(18) 1.27410(15) 0.16058(11) 0.0168(5) Uani 1 1 d . . . C8 C 0.49504(19) 1.27277(15) 0.22255(11) 0.0168(5) Uani 1 1 d . . . C9 C 0.16455(18) 0.98353(14) 0.16800(10) 0.0146(5) Uani 1 1 d . . . C10 C 0.06522(18) 0.88201(15) 0.17330(10) 0.0153(5) Uani 1 1 d . . . C11 C 0.08430(18) 0.87624(15) 0.23449(11) 0.0154(5) Uani 1 1 d . . . C12 C 0.5608(2) 1.32706(16) 0.12386(11) 0.0192(5) Uani 1 1 d . . . C13 C 0.6497(2) 1.29457(18) 0.09843(11) 0.0231(6) Uani 1 1 d . . . H13A H 0.6785 1.2402 0.1086 0.028 Uiso 1 1 calc R . . C14 C 0.6960(2) 1.3418(2) 0.05824(12) 0.0289(6) Uani 1 1 d . . . H14A H 0.7578 1.3205 0.0417 0.035 Uiso 1 1 calc R . . C15 C 0.6521(3) 1.4201(2) 0.04214(13) 0.0346(7) Uani 1 1 d . . . H15A H 0.6823 1.4512 0.0130 0.042 Uiso 1 1 calc R . . C16 C 0.5652(3) 1.45311(19) 0.06791(14) 0.0339(7) Uani 1 1 d . . . H16A H 0.5367 1.5075 0.0575 0.041 Uiso 1 1 calc R . . C17 C 0.5187(2) 1.40670(17) 0.10947(13) 0.0270(6) Uani 1 1 d . . . H17A H 0.4589 1.4294 0.1277 0.032 Uiso 1 1 calc R . . C18 C 0.5527(2) 1.32005(16) 0.26040(11) 0.0191(5) Uani 1 1 d . . . C19 C 0.6537(2) 1.32031(17) 0.25268(11) 0.0223(6) Uani 1 1 d . . . H19A H 0.6875 1.2899 0.2224 0.027 Uiso 1 1 calc R . . C20 C 0.7056(2) 1.36511(18) 0.28926(11) 0.0262(6) Uani 1 1 d . . . H20A H 0.7748 1.3652 0.2840 0.031 Uiso 1 1 calc R . . C21 C 0.6561(2) 1.40940(17) 0.33332(12) 0.0266(6) Uani 1 1 d . . . H21A H 0.6913 1.4405 0.3580 0.032 Uiso 1 1 calc R . . C22 C 0.5555(2) 1.40852(17) 0.34161(12) 0.0260(6) Uani 1 1 d . . . H22A H 0.5219 1.4387 0.3721 0.031 Uiso 1 1 calc R . . C23 C 0.5036(2) 1.36376(16) 0.30553(11) 0.0221(6) Uani 1 1 d . . . H23A H 0.4347 1.3628 0.3115 0.027 Uiso 1 1 calc R . . C24 C -0.00603(19) 0.83861(15) 0.14287(11) 0.0168(5) Uani 1 1 d . . . C25 C 0.0047(2) 0.82923(16) 0.08284(11) 0.0212(5) Uani 1 1 d . . . H25A H 0.0603 0.8468 0.0631 0.025 Uiso 1 1 calc R . . C26 C -0.0645(2) 0.79468(17) 0.05181(12) 0.0251(6) Uani 1 1 d . . . H26A H -0.0560 0.7879 0.0111 0.030 Uiso 1 1 calc R . . C27 C -0.1461(2) 0.77006(17) 0.08022(13) 0.0253(6) Uani 1 1 d . . . H27A H -0.1942 0.7469 0.0589 0.030 Uiso 1 1 calc R . . C28 C -0.1581(2) 0.77901(16) 0.13974(12) 0.0228(6) Uani 1 1 d . . . H28A H -0.2144 0.7619 0.1590 0.027 Uiso 1 1 calc R . . C29 C -0.08844(19) 0.81273(15) 0.17112(11) 0.0192(5) Uani 1 1 d . . . H29A H -0.0966 0.8183 0.2119 0.023 Uiso 1 1 calc R . . C30 C 0.05979(19) 0.80830(15) 0.27423(11) 0.0169(5) Uani 1 1 d . . . C31 C 0.0868(2) 0.72709(16) 0.25855(12) 0.0216(5) Uani 1 1 d . . . H31A H 0.1163 0.7158 0.2216 0.026 Uiso 1 1 calc R . . C32 C 0.0707(2) 0.66261(17) 0.29671(13) 0.0262(6) Uani 1 1 d . . . H32A H 0.0900 0.6072 0.2862 0.031 Uiso 1 1 calc R . . C33 C 0.0261(2) 0.67973(18) 0.35035(12) 0.0271(6) Uani 1 1 d . . . H33A H 0.0151 0.6358 0.3766 0.032 Uiso 1 1 calc R . . C34 C -0.0024(2) 0.76022(18) 0.36577(12) 0.0257(6) Uani 1 1 d . . . H34A H -0.0341 0.7713 0.4022 0.031 Uiso 1 1 calc R . . C35 C 0.0151(2) 0.82487(16) 0.32816(11) 0.0210(5) Uani 1 1 d . . . H35A H -0.0032 0.8802 0.3391 0.025 Uiso 1 1 calc R . . C36 C 0.07074(19) 1.05868(14) 0.35347(10) 0.0151(5) Uani 1 1 d . . . C37 C -0.0246(2) 1.05705(15) 0.37443(11) 0.0197(5) Uani 1 1 d . . . H37A H -0.0379 1.0206 0.4057 0.024 Uiso 1 1 calc R . . C38 C -0.0999(2) 1.10985(16) 0.34857(11) 0.0221(6) Uani 1 1 d . . . H38A H -0.1665 1.1087 0.3609 0.026 Uiso 1 1 calc R . . C39 C -0.0777(2) 1.16446(15) 0.30459(11) 0.0190(5) Uani 1 1 d . . . H39A H -0.1284 1.2019 0.2868 0.023 Uiso 1 1 calc R . . C40 C 0.02011(19) 1.16321(14) 0.28713(10) 0.0146(5) Uani 1 1 d . . . C41 C 0.15328(19) 0.99902(15) 0.37507(10) 0.0154(5) Uani 1 1 d . . . C42 C 0.2919(2) 0.87593(16) 0.39359(11) 0.0213(5) Uani 1 1 d . . . C43 C 0.2064(2) 0.88469(15) 0.42975(11) 0.0185(5) Uani 1 1 d . . . C44 C 0.04947(18) 1.21989(14) 0.24083(10) 0.0134(5) Uani 1 1 d . . . C45 C 0.01115(18) 1.33181(15) 0.18094(10) 0.0148(5) Uani 1 1 d . . . C46 C 0.10389(18) 1.31056(15) 0.15270(10) 0.0148(5) Uani 1 1 d . . . C47 C 0.3608(2) 0.79824(18) 0.38821(12) 0.0280(6) Uani 1 1 d . . . C48 C 0.4615(3) 0.7950(2) 0.39462(14) 0.0379(8) Uani 1 1 d . . . H48A H 0.4900 0.8424 0.4048 0.045 Uiso 1 1 calc R . . C49 C 0.5221(3) 0.7185(2) 0.38560(14) 0.0404(8) Uani 1 1 d . . . H49A H 0.5914 0.7138 0.3912 0.048 Uiso 1 1 calc R . . C50 C 0.4799(3) 0.6528(2) 0.36899(14) 0.0421(9) Uani 1 1 d . . . H50A H 0.5215 0.6029 0.3622 0.051 Uiso 1 1 calc R . . C51 C 0.3803(3) 0.6548(2) 0.36156(14) 0.0387(8) Uani 1 1 d . . . H51A H 0.3530 0.6077 0.3496 0.046 Uiso 1 1 calc R . . C52 C 0.1907(2) 0.83050(15) 0.48035(11) 0.0220(6) Uani 1 1 d . . . C53 C 0.2706(2) 0.79195(16) 0.51283(11) 0.0248(6) Uani 1 1 d . . . H53A H 0.3363 0.7996 0.5021 0.030 Uiso 1 1 calc R . . C54 C 0.2527(3) 0.74209(16) 0.56124(12) 0.0317(7) Uani 1 1 d . . . H54A H 0.3063 0.7172 0.5843 0.038 Uiso 1 1 calc R . . C55 C 0.1579(3) 0.72890(17) 0.57573(12) 0.0339(8) Uani 1 1 d . . . H55A H 0.1468 0.6927 0.6076 0.041 Uiso 1 1 calc R . . C56 C 0.0782(3) 0.76812(18) 0.54412(12) 0.0327(7) Uani 1 1 d . . . H56A H 0.0128 0.7592 0.5546 0.039 Uiso 1 1 calc R . . C57 C 0.0947(2) 0.82033(17) 0.49722(11) 0.0257(6) Uani 1 1 d . . . H57A H 0.0403 0.8491 0.4766 0.031 Uiso 1 1 calc R . . C58 C 0.13607(19) 1.34972(15) 0.09812(10) 0.0160(5) Uani 1 1 d . . . C59 C 0.2348(2) 1.36072(15) 0.09027(11) 0.0199(5) Uani 1 1 d . . . H59A H 0.2806 1.3453 0.1207 0.024 Uiso 1 1 calc R . . C60 C 0.2667(2) 1.39415(17) 0.03817(12) 0.0240(6) Uani 1 1 d . . . H60A H 0.3344 1.4008 0.0327 0.029 Uiso 1 1 calc R . . C61 C 0.1994(2) 1.41781(17) -0.00577(11) 0.0259(6) Uani 1 1 d . . . H61A H 0.2209 1.4417 -0.0411 0.031 Uiso 1 1 calc R . . C62 C 0.1011(2) 1.40684(16) 0.00162(11) 0.0236(6) Uani 1 1 d . . . H62A H 0.0556 1.4228 -0.0288 0.028 Uiso 1 1 calc R . . C63 C 0.0686(2) 1.37278(15) 0.05320(11) 0.0188(5) Uani 1 1 d . . . H63A H 0.0012 1.3651 0.0581 0.023 Uiso 1 1 calc R . . C64 C -0.05659(19) 1.40787(15) 0.16842(10) 0.0164(5) Uani 1 1 d . . . C65 C -0.0203(2) 1.48314(16) 0.16077(11) 0.0200(5) Uani 1 1 d . . . H65A H 0.0489 1.4853 0.1599 0.024 Uiso 1 1 calc R . . C66 C -0.0858(2) 1.55515(16) 0.15449(11) 0.0237(6) Uani 1 1 d . . . H66A H -0.0615 1.6068 0.1500 0.028 Uiso 1 1 calc R . . C67 C -0.1863(2) 1.55153(17) 0.15476(11) 0.0240(6) Uani 1 1 d . . . H67A H -0.2308 1.6008 0.1502 0.029 Uiso 1 1 calc R . . C68 C -0.2228(2) 1.47663(17) 0.16156(11) 0.0230(6) Uani 1 1 d . . . H68A H -0.2921 1.4747 0.1615 0.028 Uiso 1 1 calc R . . C69 C -0.1580(2) 1.40462(16) 0.16843(11) 0.0195(5) Uani 1 1 d . . . H69A H -0.1827 1.3532 0.1731 0.023 Uiso 1 1 calc R . . C70 C 0.41273(19) 1.15376(15) 0.36745(11) 0.0178(5) Uani 1 1 d . . . C71 C 0.4942(2) 1.15457(18) 0.40283(13) 0.0296(7) Uani 1 1 d . . . H71A H 0.4964 1.1973 0.4295 0.036 Uiso 1 1 calc R . . C72 C 0.5719(2) 1.0920(2) 0.39852(15) 0.0398(9) Uani 1 1 d . . . H72A H 0.6283 1.0908 0.4225 0.048 Uiso 1 1 calc R . . C73 C 0.5666(2) 1.03132(19) 0.35896(14) 0.0321(7) Uani 1 1 d . . . H73A H 0.6192 0.9878 0.3550 0.039 Uiso 1 1 calc R . . C74 C 0.48284(19) 1.03519(15) 0.32508(11) 0.0184(5) Uani 1 1 d . . . C75 C 0.47451(19) 0.97316(15) 0.28144(10) 0.0155(5) Uani 1 1 d . . . C76 C 0.53772(19) 0.85263(15) 0.24134(10) 0.0163(5) Uani 1 1 d . . . C77 C 0.46534(19) 0.87081(15) 0.19708(11) 0.0162(5) Uani 1 1 d . . . C78 C 0.32899(19) 1.22019(15) 0.36889(10) 0.0151(5) Uani 1 1 d . . . C79 C 0.17454(19) 1.33357(15) 0.37368(10) 0.0155(5) Uani 1 1 d . . . C80 C 0.26196(19) 1.34271(15) 0.40515(10) 0.0155(5) Uani 1 1 d . . . C81 C 0.6042(2) 0.77427(15) 0.24923(10) 0.0183(5) Uani 1 1 d . . . C82 C 0.6948(2) 0.77537(17) 0.27640(11) 0.0219(6) Uani 1 1 d . . . H82A H 0.7156 0.8263 0.2860 0.026 Uiso 1 1 calc R . . C83 C 0.7545(2) 0.70232(18) 0.28936(12) 0.0268(6) Uani 1 1 d . . . H83A H 0.8168 0.7032 0.3070 0.032 Uiso 1 1 calc R . . C84 C 0.7235(2) 0.62801(17) 0.27662(12) 0.0269(6) Uani 1 1 d . . . H84A H 0.7642 0.5779 0.2860 0.032 Uiso 1 1 calc R . . C85 C 0.6328(2) 0.62630(17) 0.25009(12) 0.0255(6) Uani 1 1 d . . . H85A H 0.6115 0.5751 0.2418 0.031 Uiso 1 1 calc R . . C86 C 0.5736(2) 0.69922(16) 0.23577(11) 0.0209(5) Uani 1 1 d . . . H86A H 0.5123 0.6981 0.2169 0.025 Uiso 1 1 calc R . . C87 C 0.4649(2) 0.82492(16) 0.14264(11) 0.0196(5) Uani 1 1 d . . . C88 C 0.3768(2) 0.8068(2) 0.11979(14) 0.0340(7) Uani 1 1 d . . . H88A H 0.3160 0.8233 0.1392 0.041 Uiso 1 1 calc R . . C89 C 0.3781(3) 0.7646(2) 0.06844(16) 0.0471(10) Uani 1 1 d . . . H89A H 0.3178 0.7523 0.0528 0.057 Uiso 1 1 calc R . . C90 C 0.4668(3) 0.7402(2) 0.03983(14) 0.0408(8) Uani 1 1 d . . . H90A H 0.4673 0.7112 0.0048 0.049 Uiso 1 1 calc R . . C91 C 0.5539(2) 0.75831(18) 0.06236(12) 0.0287(6) Uani 1 1 d . . . H91A H 0.6145 0.7416 0.0428 0.034 Uiso 1 1 calc R . . C92 C 0.5538(2) 0.80065(16) 0.11341(11) 0.0220(6) Uani 1 1 d . . . H92A H 0.6142 0.8132 0.1286 0.026 Uiso 1 1 calc R . . C93 C 0.27797(19) 1.41471(15) 0.43942(11) 0.0177(5) Uani 1 1 d . . . C94 C 0.3473(2) 1.40241(17) 0.48382(12) 0.0272(6) Uani 1 1 d . . . H94A H 0.3794 1.3486 0.4926 0.033 Uiso 1 1 calc R . . C95 C 0.3697(3) 1.46801(19) 0.51515(13) 0.0349(7) Uani 1 1 d . . . H95A H 0.4173 1.4592 0.5452 0.042 Uiso 1 1 calc R . . C96 C 0.3229(2) 1.54642(18) 0.50263(13) 0.0301(7) Uani 1 1 d . . . H96A H 0.3385 1.5915 0.5241 0.036 Uiso 1 1 calc R . . C97 C 0.2537(2) 1.55941(16) 0.45921(12) 0.0236(6) Uani 1 1 d . . . H97A H 0.2209 1.6133 0.4513 0.028 Uiso 1 1 calc R . . C98 C 0.2317(2) 1.49433(16) 0.42702(11) 0.0195(5) Uani 1 1 d . . . H98A H 0.1850 1.5039 0.3965 0.023 Uiso 1 1 calc R . . C99 C 0.08024(19) 1.38909(15) 0.37698(11) 0.0169(5) Uani 1 1 d . . . C100 C 0.0356(2) 1.40832(16) 0.43065(11) 0.0207(5) Uani 1 1 d . . . H10A H 0.0663 1.3863 0.4656 0.025 Uiso 1 1 calc R . . C101 C -0.0537(2) 1.45965(17) 0.43302(13) 0.0245(6) Uani 1 1 d . . . H10B H -0.0838 1.4729 0.4696 0.029 Uiso 1 1 calc R . . C102 C -0.0987(2) 1.49149(17) 0.38210(13) 0.0256(6) Uani 1 1 d . . . H10C H -0.1599 1.5264 0.3838 0.031 Uiso 1 1 calc R . . C103 C -0.0549(2) 1.47267(17) 0.32870(13) 0.0248(6) Uani 1 1 d . . . H10D H -0.0859 1.4948 0.2939 0.030 Uiso 1 1 calc R . . C104 C 0.0344(2) 1.42138(16) 0.32611(11) 0.0198(5) Uani 1 1 d . . . H10E H 0.0642 1.4083 0.2895 0.024 Uiso 1 1 calc R . . C105 C 0.3210(3) 0.72755(18) 0.37206(13) 0.0336(7) Uani 1 1 d . . . H10F H 0.2514 0.7300 0.3683 0.040 Uiso 1 1 calc R . . O900 O 0.7368(2) 0.07328(17) 0.24122(13) 0.0553(7) Uani 1 1 d . . . H900 H 0.7585 0.0997 0.2130 0.083 Uiso 1 1 calc R . . C900 C 0.7950(3) -0.0059(2) 0.24763(19) 0.0517(10) Uani 1 1 d . . . H90B H 0.8639 -0.0011 0.2370 0.078 Uiso 1 1 calc R . . H90C H 0.7693 -0.0447 0.2221 0.078 Uiso 1 1 calc R . . H90D H 0.7917 -0.0260 0.2881 0.078 Uiso 1 1 calc R . . O700 O 0.1234(2) 0.64369(17) 0.13088(12) 0.0593(8) Uani 1 1 d . . . H700 H 0.1419 0.6044 0.1542 0.089 Uiso 1 1 calc R . . O800 O 0.5676(2) 0.0547(2) 0.18277(14) 0.0656(9) Uani 1 1 d . . . H800 H 0.6171 0.0661 0.2005 0.098 Uiso 1 1 calc R . . C800 C 0.5944(3) 0.0347(2) 0.1262(2) 0.0563(11) Uani 1 1 d . . . H80A H 0.6156 0.0828 0.1056 0.084 Uiso 1 1 calc R . . H80B H 0.5377 0.0177 0.1063 0.084 Uiso 1 1 calc R . . H80C H 0.6489 -0.0105 0.1267 0.084 Uiso 1 1 calc R . . C700 C 0.1502(3) 0.6210(3) 0.07401(17) 0.0566(11) Uani 1 1 d . . . H70A H 0.1212 0.6639 0.0464 0.085 Uiso 1 1 calc R . . H70B H 0.1258 0.5689 0.0660 0.085 Uiso 1 1 calc R . . H70C H 0.2223 0.6143 0.0699 0.085 Uiso 1 1 calc R . . S1 S 0.91192(5) 0.15211(4) 0.12501(3) 0.02444(15) Uani 1 1 d . . . O1 O 0.9347(2) 0.21930(14) 0.08823(10) 0.0445(6) Uani 1 1 d . . . O2 O 0.99295(17) 0.10722(15) 0.15642(10) 0.0425(6) Uani 1 1 d . . . O3 O 0.82304(15) 0.17023(12) 0.15940(9) 0.0293(5) Uani 1 1 d . . . F1 F 0.85094(16) 0.01168(11) 0.10106(9) 0.0437(5) Uani 1 1 d . . . F2 F 0.95467(15) 0.05276(12) 0.03904(8) 0.0434(5) Uani 1 1 d . . . F3 F 0.80458(16) 0.11108(12) 0.04013(8) 0.0467(5) Uani 1 1 d . . . C106 C 0.8792(2) 0.07804(18) 0.07382(12) 0.0281(6) Uani 1 1 d . . . S2 S 0.27956(5) 0.47804(5) 0.23478(3) 0.02716(15) Uani 1 1 d . . . O4 O 0.33206(16) 0.40604(13) 0.20944(9) 0.0329(5) Uani 1 1 d . . . O5 O 0.28256(19) 0.48014(16) 0.29685(10) 0.0464(6) Uani 1 1 d . . . O6 O 0.18497(17) 0.50739(16) 0.20957(11) 0.0459(6) Uani 1 1 d . . . F4 F 0.31523(18) 0.63197(13) 0.22883(11) 0.0624(7) Uani 1 1 d . . . F5 F 0.3571(2) 0.56495(14) 0.15200(11) 0.0676(7) Uani 1 1 d . . . F6 F 0.44461(17) 0.54263(15) 0.22946(14) 0.0722(8) Uani 1 1 d . . . C107 C 0.3528(3) 0.5595(2) 0.21019(18) 0.0463(9) Uani 1 1 d . . . S3 S 0.78932(8) 0.90453(5) 0.49212(4) 0.01867(19) Uani 0.70 1 d P A 1 O7 O 0.7131(3) 0.97340(19) 0.49554(15) 0.0401(8) Uani 0.70 1 d P A 1 O8 O 0.8141(4) 0.8626(3) 0.54708(12) 0.0257(7) Uani 0.70 1 d P A 1 O9 O 0.8750(2) 0.9143(3) 0.45360(17) 0.0348(9) Uani 0.70 1 d P A 1 F7 F 0.64395(19) 0.81422(17) 0.48055(11) 0.0307(6) Uani 0.70 1 d P A 1 F8 F 0.7842(3) 0.75615(17) 0.45308(12) 0.0309(6) Uani 0.70 1 d P A 1 F9 F 0.7063(2) 0.85229(16) 0.39992(9) 0.0330(6) Uani 0.70 1 d P A 1 C108 C 0.7284(3) 0.8288(2) 0.45451(14) 0.0153(7) Uani 0.70 1 d P A 1 S3' S 0.8051(6) 0.9208(4) 0.4462(4) 0.1225(18) Uani 0.30 1 d PD B 2 O7' O 0.7557(13) 0.9953(8) 0.4674(8) 0.1225(18) Uani 0.30 1 d PD B 2 O8' O 0.7519(12) 0.8907(9) 0.3917(6) 0.1225(18) Uani 0.30 1 d PD B 2 O9' O 0.9060(11) 0.9074(14) 0.4500(11) 0.1225(18) Uani 0.30 1 d PD B 2 F7' F 0.6549(10) 0.8454(8) 0.4919(7) 0.1225(18) Uani 0.30 1 d PD B 2 F8' F 0.7920(14) 0.7633(8) 0.4718(8) 0.1225(18) Uani 0.30 1 d PD B 2 F9' F 0.8049(17) 0.8611(13) 0.5500(7) 0.1225(18) Uani 0.30 1 d PD B 2 C118 C 0.7594(13) 0.8432(9) 0.4996(7) 0.1225(18) Uani 0.30 1 d PD B 2 O600 O 0.4656(7) 0.9593(6) 0.4719(4) 0.110(3) Uiso 0.50 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 0.01382(6) 0.00994(5) 0.01229(5) 0.00049(3) -0.00259(4) -0.00210(4) N1 0.0140(10) 0.0108(9) 0.0150(9) -0.0005(7) -0.0015(8) -0.0019(8) N2 0.0141(10) 0.0124(10) 0.0174(10) 0.0005(8) -0.0032(8) -0.0029(8) N3 0.0152(10) 0.0129(10) 0.0196(10) 0.0001(8) -0.0033(8) -0.0040(8) N4 0.0157(11) 0.0174(10) 0.0188(10) 0.0023(8) -0.0016(8) -0.0055(9) N5 0.0136(10) 0.0132(10) 0.0145(9) -0.0007(7) -0.0011(8) -0.0036(8) N6 0.0168(11) 0.0131(10) 0.0156(10) -0.0015(8) -0.0030(8) -0.0037(8) N7 0.0167(11) 0.0125(10) 0.0163(10) 0.0000(8) -0.0005(8) -0.0033(8) N8 0.0182(11) 0.0105(9) 0.0122(9) -0.0007(7) -0.0026(8) -0.0034(8) N9 0.0209(11) 0.0138(10) 0.0150(10) 0.0021(8) -0.0067(8) -0.0034(9) N10 0.0213(12) 0.0156(10) 0.0209(11) 0.0045(8) -0.0071(9) -0.0029(9) N11 0.0253(12) 0.0137(10) 0.0139(10) 0.0011(8) -0.0033(8) -0.0052(9) N12 0.0171(11) 0.0119(10) 0.0122(9) 0.0007(7) -0.0013(8) -0.0032(8) N13 0.0187(11) 0.0133(10) 0.0127(9) 0.0016(7) -0.0014(8) -0.0030(8) N14 0.0169(11) 0.0131(10) 0.0152(10) -0.0002(8) -0.0022(8) -0.0024(8) N15 0.0168(11) 0.0116(10) 0.0148(9) -0.0004(7) -0.0038(8) -0.0020(8) N16 0.0187(11) 0.0110(10) 0.0145(9) -0.0018(7) -0.0025(8) -0.0020(8) N17 0.0186(11) 0.0135(10) 0.0157(10) -0.0016(8) -0.0015(8) -0.0010(8) N18 0.0179(11) 0.0160(10) 0.0195(10) -0.0016(8) -0.0040(8) 0.0012(9) N19 0.0159(11) 0.0138(10) 0.0151(9) 0.0006(8) -0.0027(8) -0.0020(8) N20 0.0171(11) 0.0132(10) 0.0166(10) -0.0008(8) 0.0000(8) -0.0009(8) N21 0.0214(11) 0.0149(10) 0.0165(10) -0.0023(8) -0.0035(8) -0.0025(9) C1 0.0166(12) 0.0137(11) 0.0158(11) -0.0006(9) -0.0016(9) -0.0018(10) C2 0.0304(15) 0.0263(14) 0.0169(12) -0.0013(10) -0.0049(11) -0.0129(12) C3 0.0445(19) 0.0356(17) 0.0148(12) -0.0002(11) -0.0023(12) -0.0200(14) C4 0.0331(16) 0.0277(15) 0.0179(12) 0.0015(11) 0.0003(11) -0.0165(13) C5 0.0177(13) 0.0143(12) 0.0168(11) 0.0006(9) -0.0004(9) -0.0048(10) C6 0.0148(12) 0.0125(11) 0.0179(11) 0.0019(9) -0.0019(9) -0.0004(9) C7 0.0143(12) 0.0156(12) 0.0206(12) 0.0014(9) -0.0028(10) -0.0028(10) C8 0.0155(12) 0.0146(12) 0.0205(12) 0.0016(9) -0.0038(10) -0.0024(10) C9 0.0137(12) 0.0114(11) 0.0185(11) -0.0001(9) -0.0024(9) -0.0007(9) C10 0.0153(12) 0.0118(11) 0.0183(11) -0.0018(9) -0.0019(9) 0.0005(9) C11 0.0143(12) 0.0126(11) 0.0192(12) -0.0014(9) 0.0003(9) -0.0012(9) C12 0.0197(13) 0.0229(13) 0.0167(12) -0.0004(10) -0.0038(10) -0.0092(11) C13 0.0213(14) 0.0262(14) 0.0228(13) -0.0003(11) -0.0035(11) -0.0071(12) C14 0.0235(15) 0.0429(18) 0.0234(14) -0.0049(12) 0.0037(11) -0.0155(13) C15 0.046(2) 0.0372(18) 0.0261(15) 0.0047(13) -0.0002(14) -0.0255(15) C16 0.0437(19) 0.0248(15) 0.0348(16) 0.0084(12) -0.0029(14) -0.0122(14) C17 0.0267(15) 0.0224(14) 0.0320(15) 0.0005(11) 0.0008(12) -0.0044(12) C18 0.0247(14) 0.0165(12) 0.0176(12) 0.0047(9) -0.0057(10) -0.0088(11) C19 0.0251(14) 0.0258(14) 0.0173(12) 0.0048(10) -0.0044(10) -0.0097(12) C20 0.0280(15) 0.0337(16) 0.0204(13) 0.0083(11) -0.0069(11) -0.0187(13) C21 0.0385(17) 0.0235(14) 0.0207(13) 0.0072(11) -0.0133(12) -0.0156(13) C22 0.0371(17) 0.0197(13) 0.0222(13) 0.0002(10) -0.0063(12) -0.0068(12) C23 0.0254(15) 0.0187(13) 0.0235(13) 0.0028(10) -0.0051(11) -0.0078(11) C24 0.0173(13) 0.0119(11) 0.0214(12) -0.0024(9) -0.0045(10) -0.0016(10) C25 0.0226(14) 0.0201(13) 0.0222(13) -0.0025(10) -0.0014(11) -0.0073(11) C26 0.0312(16) 0.0235(14) 0.0219(13) -0.0047(11) -0.0058(11) -0.0066(12) C27 0.0244(15) 0.0204(13) 0.0327(15) -0.0045(11) -0.0101(12) -0.0064(11) C28 0.0176(13) 0.0195(13) 0.0320(14) -0.0011(11) -0.0016(11) -0.0045(11) C29 0.0197(13) 0.0157(12) 0.0220(12) -0.0006(10) -0.0021(10) -0.0015(10) C30 0.0168(13) 0.0168(12) 0.0180(12) 0.0009(9) -0.0036(10) -0.0057(10) C31 0.0230(14) 0.0202(13) 0.0221(13) -0.0008(10) 0.0000(11) -0.0039(11) C32 0.0262(15) 0.0166(13) 0.0360(15) 0.0031(11) -0.0042(12) -0.0046(11) C33 0.0298(16) 0.0253(14) 0.0280(14) 0.0106(11) -0.0060(12) -0.0132(12) C34 0.0299(16) 0.0317(15) 0.0183(12) 0.0000(11) -0.0001(11) -0.0146(13) C35 0.0243(14) 0.0193(13) 0.0211(12) -0.0031(10) -0.0013(11) -0.0083(11) C36 0.0215(13) 0.0116(11) 0.0128(11) -0.0016(9) -0.0016(9) -0.0032(10) C37 0.0288(15) 0.0152(12) 0.0151(11) 0.0007(9) 0.0058(10) -0.0038(11) C38 0.0203(14) 0.0203(13) 0.0249(13) -0.0004(10) 0.0065(11) -0.0011(11) C39 0.0198(13) 0.0160(12) 0.0206(12) 0.0001(10) 0.0015(10) 0.0001(10) C40 0.0201(13) 0.0112(11) 0.0125(11) -0.0007(9) -0.0004(9) -0.0014(10) C41 0.0225(13) 0.0124(11) 0.0121(11) -0.0012(9) -0.0032(9) -0.0047(10) C42 0.0249(14) 0.0187(13) 0.0204(12) 0.0057(10) -0.0071(11) -0.0047(11) C43 0.0270(14) 0.0140(12) 0.0158(11) 0.0004(9) -0.0059(10) -0.0071(10) C44 0.0168(12) 0.0126(11) 0.0113(10) -0.0014(8) -0.0028(9) -0.0034(9) C45 0.0161(12) 0.0152(12) 0.0133(11) -0.0003(9) -0.0041(9) -0.0021(10) C46 0.0172(12) 0.0133(11) 0.0143(11) -0.0002(9) -0.0032(9) -0.0027(10) C47 0.0304(16) 0.0260(15) 0.0250(14) 0.0121(11) 0.0026(12) 0.0022(12) C48 0.0354(18) 0.0384(18) 0.0374(17) 0.0164(14) -0.0037(14) -0.0001(15) C49 0.0273(17) 0.058(2) 0.0335(17) 0.0093(15) 0.0018(14) 0.0011(16) C50 0.059(2) 0.0319(18) 0.0337(17) 0.0109(14) 0.0023(16) -0.0006(17) C51 0.053(2) 0.0288(16) 0.0332(17) 0.0035(13) 0.0083(15) -0.0019(15) C52 0.0399(17) 0.0121(12) 0.0153(12) 0.0013(9) -0.0066(11) -0.0084(11) C53 0.0416(18) 0.0143(12) 0.0177(12) -0.0005(10) -0.0053(12) -0.0005(12) C54 0.062(2) 0.0131(13) 0.0178(13) -0.0009(10) -0.0085(13) 0.0041(13) C55 0.073(3) 0.0144(13) 0.0149(13) 0.0031(10) -0.0010(14) -0.0099(14) C56 0.055(2) 0.0237(15) 0.0222(14) 0.0015(11) 0.0000(13) -0.0177(14) C57 0.0416(18) 0.0195(13) 0.0180(12) 0.0020(10) -0.0051(12) -0.0116(12) C58 0.0209(13) 0.0121(11) 0.0146(11) 0.0004(9) 0.0002(10) -0.0009(10) C59 0.0226(14) 0.0165(12) 0.0200(12) 0.0020(10) -0.0014(10) -0.0014(11) C60 0.0253(15) 0.0232(14) 0.0243(13) 0.0011(11) 0.0039(11) -0.0075(12) C61 0.0391(17) 0.0243(14) 0.0155(12) 0.0038(10) 0.0024(11) -0.0099(13) C62 0.0342(16) 0.0207(13) 0.0166(12) 0.0025(10) -0.0059(11) -0.0062(12) C63 0.0227(14) 0.0157(12) 0.0180(12) 0.0009(9) -0.0021(10) -0.0025(10) C64 0.0198(13) 0.0163(12) 0.0121(11) 0.0028(9) -0.0010(9) 0.0005(10) C65 0.0219(14) 0.0184(13) 0.0198(12) 0.0020(10) 0.0001(10) -0.0035(11) C66 0.0331(16) 0.0156(13) 0.0211(13) 0.0029(10) 0.0020(11) 0.0002(11) C67 0.0279(15) 0.0214(13) 0.0193(12) 0.0035(10) 0.0019(11) 0.0084(12) C68 0.0181(13) 0.0286(15) 0.0205(13) 0.0011(11) -0.0012(10) 0.0036(11) C69 0.0227(14) 0.0189(13) 0.0167(12) 0.0008(10) -0.0004(10) -0.0024(11) C70 0.0201(13) 0.0147(12) 0.0185(12) -0.0024(9) -0.0041(10) -0.0012(10) C71 0.0293(16) 0.0247(15) 0.0338(15) -0.0144(12) -0.0161(13) 0.0050(12) C72 0.0313(17) 0.0358(18) 0.050(2) -0.0201(15) -0.0266(15) 0.0106(14) C73 0.0267(16) 0.0273(15) 0.0402(17) -0.0158(13) -0.0167(13) 0.0102(13) C74 0.0198(13) 0.0145(12) 0.0206(12) -0.0027(9) -0.0053(10) 0.0003(10) C75 0.0170(12) 0.0125(11) 0.0170(11) 0.0006(9) -0.0024(9) -0.0018(10) C76 0.0154(12) 0.0159(12) 0.0176(11) -0.0011(9) -0.0008(9) -0.0017(10) C77 0.0156(12) 0.0129(11) 0.0203(12) -0.0010(9) -0.0025(10) -0.0020(10) C78 0.0179(13) 0.0120(11) 0.0154(11) 0.0001(9) -0.0014(9) -0.0026(10) C79 0.0190(13) 0.0131(11) 0.0144(11) 0.0014(9) -0.0008(9) -0.0032(10) C80 0.0194(13) 0.0132(11) 0.0140(11) -0.0004(9) -0.0005(9) -0.0021(10) C81 0.0217(13) 0.0170(12) 0.0146(11) -0.0020(9) -0.0017(10) 0.0042(10) C82 0.0215(14) 0.0236(14) 0.0198(12) -0.0019(10) -0.0039(10) 0.0011(11) C83 0.0208(14) 0.0337(16) 0.0232(13) -0.0027(11) -0.0061(11) 0.0076(12) C84 0.0301(16) 0.0248(14) 0.0215(13) 0.0002(11) -0.0011(11) 0.0130(12) C85 0.0330(16) 0.0172(13) 0.0242(13) -0.0030(10) 0.0012(12) 0.0055(12) C86 0.0219(14) 0.0194(13) 0.0201(12) -0.0026(10) -0.0020(10) 0.0030(11) C87 0.0222(14) 0.0167(12) 0.0187(12) -0.0027(10) -0.0060(10) 0.0031(10) C88 0.0235(15) 0.0410(18) 0.0373(17) -0.0196(14) -0.0063(13) 0.0013(14) C89 0.0310(18) 0.062(2) 0.049(2) -0.0335(18) -0.0136(16) 0.0007(17) C90 0.041(2) 0.050(2) 0.0311(16) -0.0233(15) -0.0093(14) 0.0039(16) C91 0.0320(17) 0.0301(15) 0.0219(13) -0.0054(11) -0.0006(12) 0.0049(13) C92 0.0224(14) 0.0230(14) 0.0200(12) -0.0026(10) -0.0047(10) 0.0004(11) C93 0.0202(13) 0.0155(12) 0.0182(12) -0.0040(9) 0.0004(10) -0.0043(10) C94 0.0355(17) 0.0185(13) 0.0270(14) -0.0054(11) -0.0106(12) 0.0004(12) C95 0.046(2) 0.0271(16) 0.0321(16) -0.0100(13) -0.0158(14) -0.0036(14) C96 0.0389(18) 0.0218(14) 0.0311(15) -0.0129(12) -0.0037(13) -0.0063(13) C97 0.0279(15) 0.0146(12) 0.0287(14) -0.0024(10) 0.0050(11) -0.0045(11) C98 0.0197(13) 0.0173(12) 0.0218(12) -0.0001(10) 0.0010(10) -0.0038(10) C99 0.0159(12) 0.0131(11) 0.0224(12) -0.0036(9) -0.0009(10) -0.0041(10) C100 0.0219(14) 0.0193(13) 0.0220(13) -0.0028(10) 0.0005(10) -0.0059(11) C101 0.0210(14) 0.0233(14) 0.0308(14) -0.0080(11) 0.0070(11) -0.0075(11) C102 0.0155(13) 0.0190(13) 0.0425(16) -0.0079(12) 0.0011(12) -0.0017(11) C103 0.0203(14) 0.0227(14) 0.0313(14) -0.0027(11) -0.0071(11) -0.0014(11) C104 0.0190(13) 0.0199(13) 0.0207(12) -0.0047(10) -0.0023(10) -0.0015(11) C105 0.044(2) 0.0229(15) 0.0323(16) 0.0042(12) 0.0090(14) -0.0001(14) O900 0.0613(18) 0.0452(15) 0.0594(18) 0.0013(13) 0.0167(14) -0.0092(14) C900 0.054(2) 0.0344(19) 0.067(3) -0.0131(18) 0.001(2) -0.0037(18) O700 0.074(2) 0.0523(17) 0.0471(15) -0.0024(13) 0.0052(15) 0.0075(15) O800 0.0479(17) 0.067(2) 0.077(2) 0.0334(17) 0.0090(15) 0.0000(16) C800 0.040(2) 0.042(2) 0.084(3) 0.015(2) 0.013(2) 0.0016(18) C700 0.058(3) 0.064(3) 0.044(2) -0.0072(19) 0.0058(19) 0.003(2) S1 0.0230(4) 0.0249(3) 0.0259(3) -0.0084(3) -0.0025(3) -0.0025(3) O1 0.0588(17) 0.0357(13) 0.0431(13) -0.0059(10) 0.0107(12) -0.0211(12) O2 0.0314(13) 0.0495(14) 0.0436(13) -0.0228(11) -0.0147(10) 0.0126(11) O3 0.0291(11) 0.0292(11) 0.0279(10) -0.0045(8) 0.0022(9) 0.0035(9) F1 0.0587(13) 0.0267(10) 0.0487(11) -0.0058(8) 0.0012(10) -0.0155(9) F2 0.0496(12) 0.0463(12) 0.0342(10) -0.0197(9) 0.0083(9) -0.0014(10) F3 0.0507(13) 0.0477(12) 0.0408(11) -0.0102(9) -0.0253(10) 0.0021(10) C106 0.0310(16) 0.0278(15) 0.0260(14) -0.0073(12) -0.0025(12) -0.0041(13) S2 0.0210(3) 0.0347(4) 0.0259(3) -0.0057(3) -0.0033(3) -0.0027(3) O4 0.0341(12) 0.0328(12) 0.0316(11) -0.0067(9) -0.0053(9) -0.0019(10) O5 0.0490(15) 0.0597(16) 0.0282(12) -0.0040(11) 0.0025(11) 0.0027(13) O6 0.0238(12) 0.0595(16) 0.0534(15) -0.0120(12) -0.0110(11) 0.0023(11) F4 0.0682(16) 0.0305(11) 0.0872(18) -0.0097(11) -0.0019(14) 0.0004(11) F5 0.0836(19) 0.0499(14) 0.0624(15) 0.0184(11) 0.0266(13) 0.0096(13) F6 0.0349(12) 0.0478(14) 0.136(2) 0.0036(15) -0.0110(14) -0.0144(11) C107 0.042(2) 0.0338(19) 0.062(2) -0.0052(17) -0.0025(18) 0.0007(16) S3 0.0329(5) 0.0141(4) 0.0105(4) 0.0016(3) -0.0043(4) -0.0088(4) O7 0.058(2) 0.0207(16) 0.0394(18) -0.0097(13) -0.0164(16) 0.0063(15) O8 0.045(2) 0.0323(16) 0.0039(11) 0.0042(11) -0.0118(12) -0.0187(15) O9 0.0206(18) 0.047(2) 0.0399(18) 0.0142(16) -0.0053(16) -0.0196(19) F7 0.0218(12) 0.0415(17) 0.0317(13) -0.0055(11) 0.0004(10) -0.0143(12) F8 0.0347(15) 0.0162(12) 0.0417(16) -0.0049(11) 0.0027(13) -0.0027(11) F9 0.0573(18) 0.0332(14) 0.0107(10) 0.0013(9) -0.0137(11) -0.0138(12) C108 0.0228(19) 0.0150(17) 0.0080(14) -0.0033(12) -0.0033(13) -0.0004(14) S3' 0.115(4) 0.083(3) 0.164(5) -0.002(3) 0.002(4) 0.010(3) O7' 0.115(4) 0.083(3) 0.164(5) -0.002(3) 0.002(4) 0.010(3) O8' 0.115(4) 0.083(3) 0.164(5) -0.002(3) 0.002(4) 0.010(3) O9' 0.115(4) 0.083(3) 0.164(5) -0.002(3) 0.002(4) 0.010(3) F7' 0.115(4) 0.083(3) 0.164(5) -0.002(3) 0.002(4) 0.010(3) F8' 0.115(4) 0.083(3) 0.164(5) -0.002(3) 0.002(4) 0.010(3) F9' 0.115(4) 0.083(3) 0.164(5) -0.002(3) 0.002(4) 0.010(3) C118 0.115(4) 0.083(3) 0.164(5) -0.002(3) 0.002(4) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N9 2.448(2) . ? Yb1 N15 2.451(2) . ? Yb1 N8 2.455(2) . ? Yb1 N12 2.460(2) . ? Yb1 N1 2.4723(19) . ? Yb1 N19 2.488(2) . ? Yb1 N2 2.489(2) . ? Yb1 N16 2.490(2) . ? Yb1 N5 2.518(2) . ? N1 C1 1.339(3) . ? N1 C5 1.345(3) . ? N2 C6 1.326(3) . ? N2 N3 1.348(3) . ? N3 C8 1.324(3) . ? N4 C7 1.324(3) . ? N4 C6 1.337(3) . ? N5 C9 1.330(3) . ? N5 N7 1.344(3) . ? N6 C10 1.327(3) . ? N6 C9 1.334(3) . ? N7 C11 1.333(3) . ? N8 C40 1.345(3) . ? N8 C36 1.348(3) . ? N9 C41 1.336(3) . ? N9 N10 1.345(3) . ? N10 C42 1.328(3) . ? N11 C43 1.329(3) . ? N11 C41 1.331(3) . ? N12 C44 1.331(3) . ? N12 N13 1.348(3) . ? N13 C46 1.331(3) . ? N14 C45 1.329(3) . ? N14 C44 1.335(3) . ? N15 C70 1.341(3) . ? N15 C74 1.343(3) . ? N16 C75 1.336(3) . ? N16 N17 1.344(3) . ? N17 C77 1.329(3) . ? N18 C76 1.325(3) . ? N18 C75 1.335(3) . ? N19 C78 1.332(3) . ? N19 N20 1.346(3) . ? N20 C79 1.332(3) . ? N21 C80 1.322(3) . ? N21 C78 1.339(3) . ? C1 C2 1.388(3) . ? C1 C9 1.475(3) . ? C2 C3 1.379(4) . ? C2 H2A 0.9500 . ? C3 C4 1.379(4) . ? C3 H3A 0.9500 . ? C4 C5 1.387(3) . ? C4 H4A 0.9500 . ? C5 C6 1.478(3) . ? C7 C8 1.427(3) . ? C7 C12 1.488(4) . ? C8 C18 1.483(3) . ? C10 C11 1.433(3) . ? C10 C24 1.474(3) . ? C11 C30 1.485(3) . ? C12 C17 1.388(4) . ? C12 C13 1.390(4) . ? C13 C14 1.384(4) . ? C13 H13A 0.9500 . ? C14 C15 1.385(5) . ? C14 H14A 0.9500 . ? C15 C16 1.373(5) . ? C15 H15A 0.9500 . ? C16 C17 1.398(4) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.388(4) . ? C18 C23 1.396(4) . ? C19 C20 1.394(4) . ? C19 H19A 0.9500 . ? C20 C21 1.384(4) . ? C20 H20A 0.9500 . ? C21 C22 1.386(4) . ? C21 H21A 0.9500 . ? C22 C23 1.386(4) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C29 1.397(4) . ? C24 C25 1.399(4) . ? C25 C26 1.381(4) . ? C25 H25A 0.9500 . ? C26 C27 1.381(4) . ? C26 H26A 0.9500 . ? C27 C28 1.387(4) . ? C27 H27A 0.9500 . ? C28 C29 1.384(4) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.393(4) . ? C30 C35 1.394(4) . ? C31 C32 1.388(4) . ? C31 H31A 0.9500 . ? C32 C33 1.390(4) . ? C32 H32A 0.9500 . ? C33 C34 1.383(4) . ? C33 H33A 0.9500 . ? C34 C35 1.388(4) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.384(4) . ? C36 C41 1.473(3) . ? C37 C38 1.382(4) . ? C37 H37A 0.9500 . ? C38 C39 1.384(4) . ? C38 H38A 0.9500 . ? C39 C40 1.387(4) . ? C39 H39A 0.9500 . ? C40 C44 1.475(3) . ? C42 C43 1.418(4) . ? C42 C47 1.490(4) . ? C43 C52 1.470(3) . ? C45 C46 1.423(3) . ? C45 C64 1.475(3) . ? C46 C58 1.478(3) . ? C47 C48 1.379(4) . ? C47 C105 1.405(4) . ? C48 C49 1.430(5) . ? C48 H48A 0.9500 . ? C49 C50 1.354(5) . ? C49 H49A 0.9500 . ? C50 C51 1.369(5) . ? C50 H50A 0.9500 . ? C51 C105 1.379(4) . ? C51 H51A 0.9500 . ? C52 C57 1.391(4) . ? C52 C53 1.399(4) . ? C53 C54 1.397(4) . ? C53 H53A 0.9500 . ? C54 C55 1.373(5) . ? C54 H54A 0.9500 . ? C55 C56 1.391(5) . ? C55 H55A 0.9500 . ? C56 C57 1.388(4) . ? C56 H56A 0.9500 . ? C57 H57A 0.9500 . ? C58 C59 1.391(4) . ? C58 C63 1.403(3) . ? C59 C60 1.389(4) . ? C59 H59A 0.9500 . ? C60 C61 1.387(4) . ? C60 H60A 0.9500 . ? C61 C62 1.384(4) . ? C61 H61A 0.9500 . ? C62 C63 1.386(4) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? C64 C69 1.391(4) . ? C64 C65 1.393(4) . ? C65 C66 1.390(4) . ? C65 H65A 0.9500 . ? C66 C67 1.379(4) . ? C66 H66A 0.9500 . ? C67 C68 1.387(4) . ? C67 H67A 0.9500 . ? C68 C69 1.386(4) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? C70 C71 1.389(4) . ? C70 C78 1.474(3) . ? C71 C72 1.382(4) . ? C71 H71A 0.9500 . ? C72 C73 1.381(4) . ? C72 H72A 0.9500 . ? C73 C74 1.386(4) . ? C73 H73A 0.9500 . ? C74 C75 1.469(3) . ? C76 C77 1.426(3) . ? C76 C81 1.480(3) . ? C77 C87 1.483(3) . ? C79 C80 1.431(3) . ? C79 C99 1.480(3) . ? C80 C93 1.482(3) . ? C81 C82 1.397(4) . ? C81 C86 1.395(4) . ? C82 C83 1.384(4) . ? C82 H82A 0.9500 . ? C83 C84 1.382(4) . ? C83 H83A 0.9500 . ? C84 C85 1.391(4) . ? C84 H84A 0.9500 . ? C85 C86 1.386(4) . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? C87 C88 1.389(4) . ? C87 C92 1.397(4) . ? C88 C89 1.388(4) . ? C88 H88A 0.9500 . ? C89 C90 1.389(5) . ? C89 H89A 0.9500 . ? C90 C91 1.374(4) . ? C90 H90A 0.9500 . ? C91 C92 1.384(4) . ? C91 H91A 0.9500 . ? C92 H92A 0.9500 . ? C93 C94 1.394(4) . ? C93 C98 1.397(3) . ? C94 C95 1.384(4) . ? C94 H94A 0.9500 . ? C95 C96 1.382(4) . ? C95 H95A 0.9500 . ? C96 C97 1.376(4) . ? C96 H96A 0.9500 . ? C97 C98 1.386(4) . ? C97 H97A 0.9500 . ? C98 H98A 0.9500 . ? C99 C104 1.391(4) . ? C99 C100 1.397(3) . ? C100 C101 1.390(4) . ? C100 H10A 0.9500 . ? C101 C102 1.385(4) . ? C101 H10B 0.9500 . ? C102 C103 1.386(4) . ? C102 H10C 0.9500 . ? C103 C104 1.390(4) . ? C103 H10D 0.9500 . ? C104 H10E 0.9500 . ? C105 H10F 0.9500 . ? O900 C900 1.436(4) . ? O900 H900 0.8400 . ? C900 H90B 0.9800 . ? C900 H90C 0.9800 . ? C900 H90D 0.9800 . ? O700 C700 1.403(4) . ? O700 H700 0.8400 . ? O800 C800 1.386(5) . ? O800 H800 0.8400 . ? C800 H80A 0.9800 . ? C800 H80B 0.9800 . ? C800 H80C 0.9800 . ? C700 H70A 0.9800 . ? C700 H70B 0.9800 . ? C700 H70C 0.9800 . ? S1 O1 1.429(2) . ? S1 O2 1.436(2) . ? S1 O3 1.443(2) . ? S1 C106 1.821(3) . ? F1 C106 1.334(4) . ? F2 C106 1.328(3) . ? F3 C106 1.334(3) . ? S2 O5 1.431(2) . ? S2 O4 1.436(2) . ? S2 O6 1.441(2) . ? S2 C107 1.839(4) . ? F4 C107 1.316(4) . ? F5 C107 1.340(5) . ? F6 C107 1.326(4) . ? S3 O7 1.436(3) . ? S3 O8 1.441(3) . ? S3 O9 1.479(3) . ? S3 C108 1.829(4) . ? F7 C108 1.336(5) . ? F8 C108 1.329(5) . ? F9 C108 1.328(4) . ? S3' O9' 1.369(14) . ? S3' O7' 1.416(13) . ? S3' O8' 1.581(14) . ? S3' C118 1.897(13) . ? F7' C118 1.434(16) . ? F8' C118 1.490(16) . ? F9' C118 1.382(16) . ? 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 N9 Yb1 N15 72.65(7) . . ? N9 Yb1 N8 65.32(7) . . ? N15 Yb1 N8 120.49(7) . . ? N9 Yb1 N12 130.70(7) . . ? N15 Yb1 N12 135.72(7) . . ? N8 Yb1 N12 65.39(7) . . ? N9 Yb1 N1 134.73(7) . . ? N15 Yb1 N1 122.33(7) . . ? N8 Yb1 N1 117.17(6) . . ? N12 Yb1 N1 71.52(6) . . ? N9 Yb1 N19 90.73(7) . . ? N15 Yb1 N19 65.51(7) . . ? N8 Yb1 N19 74.69(7) . . ? N12 Yb1 N19 76.03(6) . . ? N1 Yb1 N19 134.49(6) . . ? N9 Yb1 N2 144.07(7) . . ? N15 Yb1 N2 71.68(7) . . ? N8 Yb1 N2 140.20(6) . . ? N12 Yb1 N2 80.08(7) . . ? N1 Yb1 N2 65.39(7) . . ? N19 Yb1 N2 78.40(7) . . ? N9 Yb1 N16 78.91(7) . . ? N15 Yb1 N16 65.77(7) . . ? N8 Yb1 N16 136.91(7) . . ? N12 Yb1 N16 143.64(6) . . ? N1 Yb1 N16 72.21(6) . . ? N19 Yb1 N16 131.09(7) . . ? N2 Yb1 N16 82.83(7) . . ? N9 Yb1 N5 75.61(7) . . ? N15 Yb1 N5 134.68(6) . . ? N8 Yb1 N5 71.54(6) . . ? N12 Yb1 N5 89.59(7) . . ? N1 Yb1 N5 64.58(6) . . ? N19 Yb1 N5 146.23(7) . . ? N2 Yb1 N5 129.64(6) . . ? N16 Yb1 N5 77.11(7) . . ? C1 N1 C5 117.4(2) . . ? C1 N1 Yb1 121.72(16) . . ? C5 N1 Yb1 120.64(15) . . ? C6 N2 N3 118.3(2) . . ? C6 N2 Yb1 120.31(16) . . ? N3 N2 Yb1 121.36(15) . . ? C8 N3 N2 119.4(2) . . ? C7 N4 C6 116.7(2) . . ? C9 N5 N7 117.6(2) . . ? C9 N5 Yb1 119.80(16) . . ? N7 N5 Yb1 122.40(14) . . ? C10 N6 C9 117.8(2) . . ? C11 N7 N5 119.9(2) . . ? C40 N8 C36 117.2(2) . . ? C40 N8 Yb1 121.10(16) . . ? C36 N8 Yb1 121.36(16) . . ? C41 N9 N10 117.8(2) . . ? C41 N9 Yb1 121.34(16) . . ? N10 N9 Yb1 118.28(16) . . ? C42 N10 N9 118.8(2) . . ? C43 N11 C41 116.8(2) . . ? C44 N12 N13 118.4(2) . . ? C44 N12 Yb1 120.87(15) . . ? N13 N12 Yb1 120.71(15) . . ? C46 N13 N12 119.1(2) . . ? C45 N14 C44 116.6(2) . . ? C70 N15 C74 117.5(2) . . ? C70 N15 Yb1 121.45(16) . . ? C74 N15 Yb1 121.05(16) . . ? C75 N16 N17 117.8(2) . . ? C75 N16 Yb1 118.94(15) . . ? N17 N16 Yb1 123.29(15) . . ? C77 N17 N16 119.5(2) . . ? C76 N18 C75 117.3(2) . . ? C78 N19 N20 117.8(2) . . ? C78 N19 Yb1 119.73(16) . . ? N20 N19 Yb1 122.43(15) . . ? C79 N20 N19 119.6(2) . . ? C80 N21 C78 117.7(2) . . ? N1 C1 C2 123.2(2) . . ? N1 C1 C9 115.8(2) . . ? C2 C1 C9 120.9(2) . . ? C3 C2 C1 118.4(2) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 118.4(3) . . ? C3 C4 H4A 120.8 . . ? C5 C4 H4A 120.8 . . ? N1 C5 C4 123.1(2) . . ? N1 C5 C6 116.2(2) . . ? C4 C5 C6 120.7(2) . . ? N2 C6 N4 125.7(2) . . ? N2 C6 C5 117.2(2) . . ? N4 C6 C5 117.0(2) . . ? N4 C7 C8 119.4(2) . . ? N4 C7 C12 114.3(2) . . ? C8 C7 C12 126.2(2) . . ? N3 C8 C7 120.4(2) . . ? N3 C8 C18 115.5(2) . . ? C7 C8 C18 124.1(2) . . ? N5 C9 N6 125.2(2) . . ? N5 C9 C1 117.2(2) . . ? N6 C9 C1 117.5(2) . . ? N6 C10 C11 118.0(2) . . ? N6 C10 C24 116.1(2) . . ? C11 C10 C24 125.8(2) . . ? N7 C11 C10 119.9(2) . . ? N7 C11 C30 115.3(2) . . ? C10 C11 C30 124.7(2) . . ? C17 C12 C13 120.4(3) . . ? C17 C12 C7 118.3(2) . . ? C13 C12 C7 120.8(2) . . ? C14 C13 C12 119.7(3) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 120.5(3) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C12 C17 C16 119.3(3) . . ? C12 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C19 C18 C23 119.7(2) . . ? C19 C18 C8 121.7(2) . . ? C23 C18 C8 118.6(2) . . ? C18 C19 C20 120.2(3) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C22 C23 C18 119.9(3) . . ? C22 C23 H23A 120.1 . . ? C18 C23 H23A 120.1 . . ? C29 C24 C25 118.9(2) . . ? C29 C24 C10 122.1(2) . . ? C25 C24 C10 118.8(2) . . ? C26 C25 C24 120.8(3) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C27 C26 C25 119.7(3) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 120.3(3) . . ? C26 C27 H27A 119.8 . . ? C28 C27 H27A 119.8 . . ? C29 C28 C27 120.2(3) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C28 C29 C24 120.1(2) . . ? C28 C29 H29A 120.0 . . ? C24 C29 H29A 120.0 . . ? C31 C30 C35 119.8(2) . . ? C31 C30 C11 119.3(2) . . ? C35 C30 C11 120.8(2) . . ? C32 C31 C30 120.3(3) . . ? C32 C31 H31A 119.8 . . ? C30 C31 H31A 119.8 . . ? C33 C32 C31 119.4(3) . . ? C33 C32 H32A 120.3 . . ? C31 C32 H32A 120.3 . . ? C34 C33 C32 120.5(3) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C33 C34 C35 120.2(3) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C34 C35 C30 119.7(2) . . ? C34 C35 H35A 120.2 . . ? C30 C35 H35A 120.2 . . ? N8 C36 C37 123.4(2) . . ? N8 C36 C41 115.2(2) . . ? C37 C36 C41 121.2(2) . . ? C38 C37 C36 118.2(2) . . ? C38 C37 H37A 120.9 . . ? C36 C37 H37A 120.9 . . ? C37 C38 C39 119.6(3) . . ? C37 C38 H38A 120.2 . . ? C39 C38 H38A 120.2 . . ? C38 C39 C40 118.4(2) . . ? C38 C39 H39A 120.8 . . ? C40 C39 H39A 120.8 . . ? N8 C40 C39 123.1(2) . . ? N8 C40 C44 115.4(2) . . ? C39 C40 C44 121.5(2) . . ? N11 C41 N9 125.1(2) . . ? N11 C41 C36 118.2(2) . . ? N9 C41 C36 116.6(2) . . ? N10 C42 C43 120.5(2) . . ? N10 C42 C47 114.7(2) . . ? C43 C42 C47 124.5(2) . . ? N11 C43 C42 118.4(2) . . ? N11 C43 C52 117.1(2) . . ? C42 C43 C52 124.5(2) . . ? N12 C44 N14 125.3(2) . . ? N12 C44 C40 116.6(2) . . ? N14 C44 C40 118.0(2) . . ? N14 C45 C46 119.4(2) . . ? N14 C45 C64 115.9(2) . . ? C46 C45 C64 124.6(2) . . ? N13 C46 C45 120.1(2) . . ? N13 C46 C58 114.8(2) . . ? C45 C46 C58 125.1(2) . . ? C48 C47 C105 119.6(3) . . ? C48 C47 C42 122.5(3) . . ? C105 C47 C42 117.8(3) . . ? C47 C48 C49 118.3(3) . . ? C47 C48 H48A 120.9 . . ? C49 C48 H48A 120.9 . . ? C50 C49 C48 119.6(3) . . ? C50 C49 H49A 120.2 . . ? C48 C49 H49A 120.2 . . ? C49 C50 C51 123.2(3) . . ? C49 C50 H50A 118.4 . . ? C51 C50 H50A 118.4 . . ? C50 C51 C105 117.6(3) . . ? C50 C51 H51A 121.2 . . ? C105 C51 H51A 121.2 . . ? C57 C52 C53 119.9(2) . . ? C57 C52 C43 119.2(2) . . ? C53 C52 C43 120.9(3) . . ? C54 C53 C52 119.3(3) . . ? C54 C53 H53A 120.4 . . ? C52 C53 H53A 120.4 . . ? C55 C54 C53 120.4(3) . . ? C55 C54 H54A 119.8 . . ? C53 C54 H54A 119.8 . . ? C54 C55 C56 120.5(3) . . ? C54 C55 H55A 119.8 . . ? C56 C55 H55A 119.8 . . ? C57 C56 C55 119.7(3) . . ? C57 C56 H56A 120.1 . . ? C55 C56 H56A 120.1 . . ? C56 C57 C52 120.1(3) . . ? C56 C57 H57A 120.0 . . ? C52 C57 H57A 120.0 . . ? C59 C58 C63 119.7(2) . . ? C59 C58 C46 119.7(2) . . ? C63 C58 C46 120.5(2) . . ? C60 C59 C58 120.3(2) . . ? C60 C59 H59A 119.9 . . ? C58 C59 H59A 119.9 . . ? C61 C60 C59 119.7(3) . . ? C61 C60 H60A 120.1 . . ? C59 C60 H60A 120.1 . . ? C62 C61 C60 120.4(2) . . ? C62 C61 H61A 119.8 . . ? C60 C61 H61A 119.8 . . ? C61 C62 C63 120.4(2) . . ? C61 C62 H62A 119.8 . . ? C63 C62 H62A 119.8 . . ? C62 C63 C58 119.5(3) . . ? C62 C63 H63A 120.2 . . ? C58 C63 H63A 120.2 . . ? C69 C64 C65 120.1(2) . . ? C69 C64 C45 119.2(2) . . ? C65 C64 C45 120.5(2) . . ? C66 C65 C64 119.7(3) . . ? C66 C65 H65A 120.1 . . ? C64 C65 H65A 120.1 . . ? C67 C66 C65 119.9(3) . . ? C67 C66 H66A 120.1 . . ? C65 C66 H66A 120.1 . . ? C66 C67 C68 120.7(2) . . ? C66 C67 H67A 119.7 . . ? C68 C67 H67A 119.7 . . ? C69 C68 C67 119.8(3) . . ? C69 C68 H68A 120.1 . . ? C67 C68 H68A 120.1 . . ? C68 C69 C64 119.8(3) . . ? C68 C69 H69A 120.1 . . ? C64 C69 H69A 120.1 . . ? N15 C70 C71 122.9(2) . . ? N15 C70 C78 116.0(2) . . ? C71 C70 C78 121.1(2) . . ? C72 C71 C70 118.7(3) . . ? C72 C71 H71A 120.7 . . ? C70 C71 H71A 120.7 . . ? C73 C72 C71 119.1(3) . . ? C73 C72 H72A 120.4 . . ? C71 C72 H72A 120.4 . . ? C72 C73 C74 118.6(3) . . ? C72 C73 H73A 120.7 . . ? C74 C73 H73A 120.7 . . ? N15 C74 C73 123.2(2) . . ? N15 C74 C75 116.1(2) . . ? C73 C74 C75 120.7(2) . . ? N18 C75 N16 125.1(2) . . ? N18 C75 C74 117.2(2) . . ? N16 C75 C74 117.7(2) . . ? N18 C76 C77 118.5(2) . . ? N18 C76 C81 115.7(2) . . ? C77 C76 C81 125.7(2) . . ? N17 C77 C76 120.2(2) . . ? N17 C77 C87 115.7(2) . . ? C76 C77 C87 124.0(2) . . ? N19 C78 N21 125.3(2) . . ? N19 C78 C70 117.3(2) . . ? N21 C78 C70 117.3(2) . . ? N20 C79 C80 120.5(2) . . ? N20 C79 C99 114.4(2) . . ? C80 C79 C99 125.1(2) . . ? N21 C80 C79 118.4(2) . . ? N21 C80 C93 115.7(2) . . ? C79 C80 C93 125.9(2) . . ? C82 C81 C86 119.7(2) . . ? C82 C81 C76 118.7(2) . . ? C86 C81 C76 121.3(2) . . ? C83 C82 C81 120.1(3) . . ? C83 C82 H82A 120.0 . . ? C81 C82 H82A 120.0 . . ? C84 C83 C82 120.1(3) . . ? C84 C83 H83A 119.9 . . ? C82 C83 H83A 119.9 . . ? C83 C84 C85 120.2(2) . . ? C83 C84 H84A 119.9 . . ? C85 C84 H84A 119.9 . . ? C86 C85 C84 120.1(3) . . ? C86 C85 H85A 119.9 . . ? C84 C85 H85A 119.9 . . ? C85 C86 C81 119.8(3) . . ? C85 C86 H86A 120.1 . . ? C81 C86 H86A 120.1 . . ? C88 C87 C92 119.5(2) . . ? C88 C87 C77 120.8(2) . . ? C92 C87 C77 119.8(2) . . ? C87 C88 C89 119.8(3) . . ? C87 C88 H88A 120.1 . . ? C89 C88 H88A 120.1 . . ? C90 C89 C88 120.4(3) . . ? C90 C89 H89A 119.8 . . ? C88 C89 H89A 119.8 . . ? C91 C90 C89 119.8(3) . . ? C91 C90 H90A 120.1 . . ? C89 C90 H90A 120.1 . . ? C90 C91 C92 120.4(3) . . ? C90 C91 H91A 119.8 . . ? C92 C91 H91A 119.8 . . ? C91 C92 C87 120.1(3) . . ? C91 C92 H92A 119.9 . . ? C87 C92 H92A 119.9 . . ? C94 C93 C98 118.9(2) . . ? C94 C93 C80 117.8(2) . . ? C98 C93 C80 123.2(2) . . ? C95 C94 C93 120.5(3) . . ? C95 C94 H94A 119.7 . . ? C93 C94 H94A 119.7 . . ? C96 C95 C94 119.9(3) . . ? C96 C95 H95A 120.0 . . ? C94 C95 H95A 120.0 . . ? C97 C96 C95 120.2(3) . . ? C97 C96 H96A 119.9 . . ? C95 C96 H96A 119.9 . . ? C96 C97 C98 120.3(3) . . ? C96 C97 H97A 119.8 . . ? C98 C97 H97A 119.8 . . ? C97 C98 C93 120.1(2) . . ? C97 C98 H98A 120.0 . . ? C93 C98 H98A 120.0 . . ? C104 C99 C100 119.5(2) . . ? C104 C99 C79 119.8(2) . . ? C100 C99 C79 120.8(2) . . ? C101 C100 C99 120.1(3) . . ? C101 C100 H10A 120.0 . . ? C99 C100 H10A 120.0 . . ? C102 C101 C100 120.0(3) . . ? C102 C101 H10B 120.0 . . ? C100 C101 H10B 120.0 . . ? C101 C102 C103 120.3(3) . . ? C101 C102 H10C 119.9 . . ? C103 C102 H10C 119.9 . . ? C102 C103 C104 120.0(3) . . ? C102 C103 H10D 120.0 . . ? C104 C103 H10D 120.0 . . ? C103 C104 C99 120.2(2) . . ? C103 C104 H10E 119.9 . . ? C99 C104 H10E 119.9 . . ? C51 C105 C47 121.7(3) . . ? C51 C105 H10F 119.2 . . ? C47 C105 H10F 119.2 . . ? C900 O900 H900 109.5 . . ? O900 C900 H90B 109.5 . . ? O900 C900 H90C 109.5 . . ? H90B C900 H90C 109.5 . . ? O900 C900 H90D 109.5 . . ? H90B C900 H90D 109.5 . . ? H90C C900 H90D 109.5 . . ? C700 O700 H700 109.5 . . ? C800 O800 H800 109.5 . . ? O800 C800 H80A 109.5 . . ? O800 C800 H80B 109.5 . . ? H80A C800 H80B 109.5 . . ? O800 C800 H80C 109.5 . . ? H80A C800 H80C 109.5 . . ? H80B C800 H80C 109.5 . . ? O700 C700 H70A 109.5 . . ? O700 C700 H70B 109.5 . . ? H70A C700 H70B 109.5 . . ? O700 C700 H70C 109.5 . . ? H70A C700 H70C 109.5 . . ? H70B C700 H70C 109.5 . . ? O1 S1 O2 116.37(16) . . ? O1 S1 O3 114.08(14) . . ? O2 S1 O3 114.01(14) . . ? O1 S1 C106 103.36(14) . . ? O2 S1 C106 103.40(13) . . ? O3 S1 C106 103.34(13) . . ? F2 C106 F1 107.7(2) . . ? F2 C106 F3 107.4(2) . . ? F1 C106 F3 107.4(3) . . ? F2 C106 S1 111.5(2) . . ? F1 C106 S1 111.7(2) . . ? F3 C106 S1 111.0(2) . . ? O5 S2 O4 115.71(14) . . ? O5 S2 O6 114.99(15) . . ? O4 S2 O6 115.61(14) . . ? O5 S2 C107 103.74(17) . . ? O4 S2 C107 102.59(15) . . ? O6 S2 C107 101.22(17) . . ? F4 C107 F6 108.4(3) . . ? F4 C107 F5 107.8(3) . . ? F6 C107 F5 107.8(3) . . ? F4 C107 S2 111.9(3) . . ? F6 C107 S2 110.0(3) . . ? F5 C107 S2 110.8(3) . . ? O7 S3 O8 114.5(3) . . ? O7 S3 O9 117.4(2) . . ? O8 S3 O9 114.6(3) . . ? O7 S3 C108 102.85(19) . . ? O8 S3 C108 102.1(2) . . ? O9 S3 C108 102.4(2) . . ? F9 C108 F8 107.3(3) . . ? F9 C108 F7 106.7(3) . . ? F8 C108 F7 105.6(3) . . ? F9 C108 S3 112.4(3) . . ? F8 C108 S3 111.9(3) . . ? F7 C108 S3 112.5(2) . . ? O9' S3' O7' 117.9(14) . . ? O9' S3' O8' 120.1(14) . . ? O7' S3' O8' 112.3(11) . . ? O9' S3' C118 105.0(10) . . ? O7' S3' C118 100.8(9) . . ? O8' S3' C118 95.1(8) . . ? F9' C118 F7' 125.7(18) . . ? F9' C118 F8' 118.9(17) . . ? F7' C118 F8' 98.3(14) . . ? F9' C118 S3' 101.0(11) . . ? F7' C118 S3' 108.1(10) . . ? F8' C118 S3' 102.7(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.904 _refine_diff_density_min -1.056 _refine_diff_density_rms 0.085