# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_coden_Cambridge 440 _publ_contact_author_name 'Colin L. Raston' _publ_contact_author_address ; School of Biomedical and Chemical Sciences University of Western Australia Crawley Perth WA 6909 Australia ; _publ_contact_author_phone '+61 89380 3045' _publ_contact_author_fax '+61 89380 1005' _publ_contact_author_email clraston@chem.uwa.edu.au _publ_requested_journal 'New J. Chem.' _publ_contact_letter ; The following 1 set of data is supplementary data for one of the crystal structures included in the paper, details of which are given below ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Hydrogen bonded arrays of a ytterbium(III) p-sulfonatocalix[6]arene complex ; loop_ _publ_author_name _publ_author_address 'Jerry L. Atwood' ; Department of Chemistry University of Missouri-Columbia Columbia Missouri 65211 USA ; 'Scott J. Dalgarno' ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Michaele J. Hardie' ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Colin L. Raston' ; School of Biomedical and Chemical Sciences University of Western Australia Crawley Perth WA 6909 Australia ; #================================================================= data_Yb[6]PyNOxide _database_code_depnum_ccdc_archive 'CCDC 222953' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Yb[6]PyNO _chemical_melting_point ? _chemical_formula_moiety 'C67 H95 N5 O49 S6 Yb2' _chemical_formula_sum 'C67 H95 N5 O49 S6 Yb2' _chemical_formula_weight 2292.92 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' 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 12.487(4) _cell_length_b 17.799(5) _cell_length_c 20.803(6) _cell_angle_alpha 113.601(4) _cell_angle_beta 91.155(5) _cell_angle_gamma 91.297(5) _cell_volume 4234(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 2.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4404 _exptl_absorpt_correction_T_max 0.7915 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37445 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.14 _reflns_number_total 18422 _reflns_number_gt 14123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+5.5208P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18422 _refine_ls_number_parameters 1197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1089 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.228049(16) 0.384385(12) -0.002222(11) 0.01879(6) Uani 1 1 d . . . Yb2 Yb 0.754602(18) -0.393274(13) -0.433707(13) 0.02673(7) Uani 1 1 d . . . S3 S 0.21684(9) 0.17201(7) -0.11842(6) 0.0182(2) Uani 1 1 d . . . S4 S 0.80377(9) 0.30106(7) -0.13892(7) 0.0204(3) Uani 1 1 d . . . S5 S 0.76184(10) 0.31537(7) -0.62717(7) 0.0218(3) Uani 1 1 d . . . S6 S 1.08687(9) 0.21601(7) 0.16687(6) 0.0181(2) Uani 1 1 d . . . S7 S 0.68836(9) -0.18096(7) -0.36078(6) 0.0195(2) Uani 1 1 d . . . S9 S 0.44859(11) 0.19289(9) -0.35927(7) 0.0315(3) Uani 1 1 d . . . O1 O 0.8682(3) 0.3517(2) -0.5983(2) 0.0314(9) Uani 1 1 d . . . O2 O 0.6790(3) 0.3515(2) -0.5767(2) 0.0310(9) Uani 1 1 d . . . O3 O 0.7402(3) 0.3184(2) -0.69515(19) 0.0307(9) Uani 1 1 d . . . O4 O 0.7793(3) -0.0361(2) -0.68544(19) 0.0239(8) Uani 1 1 d . . . O5 O 0.4565(4) 0.2730(3) -0.3581(2) 0.0492(11) Uani 1 1 d . . . O6 O 0.4723(4) 0.1923(3) -0.2914(2) 0.0535(13) Uani 1 1 d . . . O7 O 0.3482(3) 0.1517(3) -0.3889(2) 0.0480(11) Uani 1 1 d . . . O8 O 0.7979(3) 0.0151(2) -0.5366(2) 0.0280(9) Uani 1 1 d . . . O9 O 0.6618(3) -0.1804(2) -0.29264(18) 0.0252(8) Uani 1 1 d . . . O10 O 0.7437(3) -0.2564(2) -0.40314(18) 0.0242(8) Uani 1 1 d . . . O11 O 0.5984(3) -0.1675(2) -0.39924(19) 0.0282(8) Uani 1 1 d . . . O12 O 1.0151(3) 0.0803(2) -0.3069(2) 0.0271(9) Uani 1 1 d . . . O13 O 0.5690(3) -0.3778(2) -0.4207(3) 0.0458(11) Uani 1 1 d . . . O14 O 0.7237(3) -0.3377(2) -0.3131(2) 0.0364(9) Uani 1 1 d . . . O15 O 0.9179(3) -0.3606(2) -0.36794(19) 0.0325(9) Uani 1 1 d . . . O16 O 0.8827(3) -0.4963(2) -0.4938(2) 0.0367(10) Uani 1 1 d . . . O17 O 0.6717(3) -0.4780(2) -0.5421(2) 0.0373(10) Uani 1 1 d . . . O18 O 0.8583(3) -0.3609(2) -0.5114(2) 0.0369(10) Uani 1 1 d . . . O19 O 0.7098(3) -0.5001(2) -0.4060(2) 0.0422(11) Uani 1 1 d . . . O20 O 1.0515(3) 0.2420(2) 0.23849(18) 0.0297(8) Uani 1 1 d . . . O21 O 1.1136(3) 0.2851(2) 0.14849(18) 0.0237(8) Uani 1 1 d . . . O22 O 1.1728(3) 0.1580(2) 0.15049(19) 0.0278(8) Uani 1 1 d . . . O23 O 0.7088(3) 0.0393(2) -0.0069(2) 0.0224(8) Uani 1 1 d . . . O24 O 0.8875(3) 0.3388(2) -0.08469(19) 0.0265(8) Uani 1 1 d . . . O25 O 0.7020(3) 0.3416(2) -0.1175(2) 0.0296(9) Uani 1 1 d . . . O26 O 0.8337(3) 0.2955(2) -0.2075(2) 0.0325(9) Uani 1 1 d . . . O27 O 0.7049(3) -0.0330(2) -0.1584(2) 0.0205(8) Uani 1 1 d . . . O28 O 0.2760(2) 0.2480(2) -0.07429(17) 0.0203(7) Uani 1 1 d . . . O29 O 0.1317(3) 0.1524(2) -0.08081(19) 0.0259(8) Uani 1 1 d . . . O30 O 0.1774(3) 0.1775(2) -0.18267(19) 0.0291(8) Uani 1 1 d . . . O31 O 0.4970(3) -0.1099(2) -0.2020(2) 0.0240(9) Uani 1 1 d . . . O32 O 0.3345(3) 0.3917(2) -0.0874(2) 0.0311(9) Uani 1 1 d . . . O33 O 0.3475(3) 0.4967(2) 0.0556(2) 0.0334(9) Uani 1 1 d . . . O34 O 0.1614(3) 0.4569(2) 0.10906(18) 0.0267(8) Uani 1 1 d . . . O35 O 0.1025(3) 0.3022(2) 0.02359(18) 0.0260(8) Uani 1 1 d . . . O36 O 0.1049(3) 0.3363(2) -0.10162(18) 0.0248(8) Uani 1 1 d . . . O37 O 0.1382(3) 0.4937(2) -0.01193(19) 0.0268(8) Uani 1 1 d . . . O38 O 0.3552(3) 0.3499(2) 0.0589(2) 0.0358(10) Uani 1 1 d . . . O39A O 0.5462(4) 0.4977(3) 0.1148(3) 0.0220(12) Uiso 0.60 1 d P A 2 O39B O 0.5544(10) 0.4624(8) 0.0537(7) 0.058(3) Uiso 0.40 1 d P B 1 O40 O 0.9561(3) 0.4896(3) 0.1215(2) 0.0380(10) Uani 1 1 d . . . O41 O 0.7825(3) 0.7504(3) 0.2750(2) 0.0433(10) Uani 1 1 d . . . O42 O 0.4862(3) 0.2932(3) -0.1560(2) 0.0430(10) Uani 1 1 d . . . O43 O 0.5222(4) 0.4207(3) -0.2559(3) 0.0616(14) Uani 1 1 d . . . O44 O 0.7366(3) 0.4304(2) -0.2280(2) 0.0429(10) Uani 1 1 d . . . O45 O 0.4849(3) -0.2983(3) -0.2897(2) 0.0488(11) Uani 1 1 d . . . O46 O 1.0024(3) 0.2317(2) -0.2987(2) 0.0338(9) Uani 1 1 d . . . O47 O 0.5458(4) -0.3101(3) -0.5214(3) 0.0622(14) Uani 1 1 d . . . O48 O 0.5109(4) -0.4916(4) -0.6415(3) 0.0715(16) Uani 1 1 d . . . O49A O 0.6758(14) -0.4142(13) -0.2214(11) 0.052(5) Uani 0.40 1 d P C 3 O49B O 0.7312(14) -0.4127(12) -0.2302(9) 0.044(4) Uani 0.40 1 d P D 2 O49C O 0.787(2) -0.4231(16) -0.2478(13) 0.029(5) Uani 0.20 1 d P E 1 N1 N 0.8887(3) -0.2864(3) -0.5072(2) 0.0261(10) Uani 1 1 d . . . N2 N 0.7590(4) -0.5644(3) -0.4019(2) 0.0305(10) Uani 1 1 d . . . N3 N 0.3961(3) 0.2760(2) 0.0444(2) 0.0234(9) Uani 1 1 d . . . N4A N 0.6013(7) 0.4350(5) 0.1127(5) 0.0220(19) Uiso 0.60 1 d P A 2 N4B N 0.6056(11) 0.4204(9) 0.0867(8) 0.030(3) Uiso 0.40 1 d P B 1 N5 N 0.9097(3) 0.4966(3) 0.1805(2) 0.0270(10) Uani 1 1 d . . . C1 C 0.8549(4) 0.0824(3) -0.7019(2) 0.0185(10) Uani 1 1 d . . . C2 C 0.8488(4) 0.1653(3) -0.6835(2) 0.0180(10) Uani 1 1 d . . . H2 H 0.9022 0.1927 -0.6989 0.022 Uiso 1 1 calc R . . C3 C 0.7663(4) 0.2106(3) -0.6428(2) 0.0185(10) Uani 1 1 d . . . C4 C 0.6878(4) 0.1719(3) -0.6192(2) 0.0189(10) Uani 1 1 d . . . H4 H 0.6308 0.2023 -0.5925 0.023 Uiso 1 1 calc R . . C5 C 0.6931(4) 0.0886(3) -0.6350(2) 0.0182(10) Uani 1 1 d . . . C6 C 0.7765(4) 0.0445(3) -0.6753(2) 0.0196(10) Uani 1 1 d . . . C7 C 0.6092(4) 0.0447(3) -0.6085(2) 0.0194(10) Uani 1 1 d . . . H7A H 0.5367 0.0576 -0.6205 0.023 Uiso 1 1 calc R . . H7B H 0.6171 -0.0153 -0.6325 0.023 Uiso 1 1 calc R . . C8 C 0.6202(4) 0.0701(3) -0.5298(3) 0.0195(10) Uani 1 1 d . . . C9 C 0.5375(4) 0.1097(3) -0.4865(3) 0.0237(11) Uani 1 1 d . . . H9 H 0.4723 0.1179 -0.5067 0.028 Uiso 1 1 calc R . . C10 C 0.5492(4) 0.1373(3) -0.4142(3) 0.0256(11) Uani 1 1 d . . . C11 C 0.6447(4) 0.1278(3) -0.3842(3) 0.0261(11) Uani 1 1 d . . . H11 H 0.6531 0.1495 -0.3345 0.031 Uiso 1 1 calc R . . C12 C 0.7287(4) 0.0872(3) -0.4252(3) 0.0229(11) Uani 1 1 d . . . C13 C 0.7146(4) 0.0564(3) -0.4980(3) 0.0210(10) Uani 1 1 d . . . C14 C 0.8344(4) 0.0851(3) -0.3894(3) 0.0272(12) Uani 1 1 d . . . H14A H 0.8486 0.1396 -0.3508 0.033 Uiso 1 1 calc R . . H14B H 0.8916 0.0766 -0.4237 0.033 Uiso 1 1 calc R . . C15 C 0.8435(4) 0.0206(3) -0.3595(2) 0.0182(10) Uani 1 1 d . . . C16 C 0.7675(4) -0.0415(3) -0.3721(2) 0.0180(10) Uani 1 1 d . . . H16 H 0.7044 -0.0440 -0.3993 0.022 Uiso 1 1 calc R . . C17 C 0.7831(4) -0.1004(3) -0.3451(2) 0.0170(10) Uani 1 1 d . . . C18 C 0.8768(4) -0.0987(3) -0.3059(2) 0.0189(10) Uani 1 1 d . . . H18 H 0.8873 -0.1401 -0.2887 0.023 Uiso 1 1 calc R . . C19 C 0.9530(4) -0.0372(3) -0.2926(2) 0.0164(9) Uani 1 1 d . . . C20 C 0.9353(4) 0.0223(3) -0.3199(2) 0.0190(10) Uani 1 1 d . . . C21 C 1.0559(4) -0.0354(3) -0.2523(2) 0.0181(10) Uani 1 1 d . . . H21A H 1.0408 -0.0587 -0.2173 0.022 Uiso 1 1 calc R . . H21B H 1.0806 0.0225 -0.2263 0.022 Uiso 1 1 calc R . . C22 C 0.9825(4) -0.2522(3) -0.4751(3) 0.0293(12) Uani 1 1 d . . . H22 H 1.0265 -0.2810 -0.4555 0.035 Uiso 1 1 calc R . . C23 C 1.0157(5) -0.1762(4) -0.4704(3) 0.0329(13) Uani 1 1 d . . . H23 H 1.0824 -0.1524 -0.4477 0.039 Uiso 1 1 calc R . . C24 C 0.9528(5) -0.1352(4) -0.4983(3) 0.0363(14) Uani 1 1 d . . . H24 H 0.9747 -0.0823 -0.4949 0.044 Uiso 1 1 calc R . . C25 C 0.8572(5) -0.1707(4) -0.5315(3) 0.0394(15) Uani 1 1 d . . . H25 H 0.8128 -0.1425 -0.5514 0.047 Uiso 1 1 calc R . . C26 C 0.8259(5) -0.2469(4) -0.5357(3) 0.0341(13) Uani 1 1 d . . . H26 H 0.7599 -0.2718 -0.5588 0.041 Uiso 1 1 calc R . . C27 C 0.7049(5) -0.6366(3) -0.4260(3) 0.0328(13) Uani 1 1 d . . . H27 H 0.6352 -0.6418 -0.4467 0.039 Uiso 1 1 calc R . . C28 C 0.7511(5) -0.7034(4) -0.4204(3) 0.0395(15) Uani 1 1 d . . . H28 H 0.7136 -0.7550 -0.4378 0.047 Uiso 1 1 calc R . . C29 C 0.8508(5) -0.6954(4) -0.3900(3) 0.0404(15) Uani 1 1 d . . . H29 H 0.8824 -0.7409 -0.3850 0.048 Uiso 1 1 calc R . . C30 C 0.9050(5) -0.6208(4) -0.3666(3) 0.0413(15) Uani 1 1 d . . . H30 H 0.9752 -0.6149 -0.3463 0.050 Uiso 1 1 calc R . . C31 C 0.8580(5) -0.5549(4) -0.3726(3) 0.0411(15) Uani 1 1 d . . . H31 H 0.8951 -0.5031 -0.3563 0.049 Uiso 1 1 calc R . . C32 C 0.3448(4) -0.0435(3) -0.1477(2) 0.0152(9) Uani 1 1 d . . . C33 C 0.2795(4) 0.0231(3) -0.1277(2) 0.0177(10) Uani 1 1 d . . . H33 H 0.2151 0.0221 -0.1044 0.021 Uiso 1 1 calc R . . C34 C 0.3066(4) 0.0915(3) -0.1410(2) 0.0170(9) Uani 1 1 d . . . C35 C 0.4011(4) 0.0936(3) -0.1752(2) 0.0191(10) Uani 1 1 d . . . H35 H 0.4187 0.1403 -0.1847 0.023 Uiso 1 1 calc R . . C36 C 0.4691(3) 0.0286(3) -0.1953(2) 0.0156(9) Uani 1 1 d . . . C37 C 0.4398(3) -0.0401(3) -0.1819(2) 0.0155(9) Uani 1 1 d . . . C38 C 0.5696(3) 0.0301(3) -0.2354(2) 0.0156(9) Uani 1 1 d . . . H38A H 0.5897 -0.0273 -0.2626 0.019 Uiso 1 1 calc R . . H38B H 0.5516 0.0542 -0.2695 0.019 Uiso 1 1 calc R . . C39 C 0.6668(3) 0.0772(3) -0.1910(2) 0.0143(9) Uani 1 1 d . . . C40 C 0.6920(4) 0.1557(3) -0.1848(2) 0.0170(10) Uani 1 1 d . . . H40 H 0.6471 0.1804 -0.2077 0.020 Uiso 1 1 calc R . . C41 C 0.7810(4) 0.1993(3) -0.1461(2) 0.0169(9) Uani 1 1 d . . . C42 C 0.8495(3) 0.1638(3) -0.1137(2) 0.0167(9) Uani 1 1 d . . . H42 H 0.9114 0.1937 -0.0881 0.020 Uiso 1 1 calc R . . C43 C 0.8281(3) 0.0847(3) -0.1187(2) 0.0145(9) Uani 1 1 d . . . C44 C 0.7362(3) 0.0424(3) -0.1574(2) 0.0143(9) Uani 1 1 d . . . C45 C 0.9031(3) 0.0466(3) -0.0819(2) 0.0167(9) Uani 1 1 d . . . H45A H 0.9779 0.0535 -0.0941 0.020 Uiso 1 1 calc R . . H45B H 0.8858 -0.0129 -0.0993 0.020 Uiso 1 1 calc R . . C46 C 0.8943(4) 0.0853(3) -0.0021(2) 0.0148(9) Uani 1 1 d . . . C47 C 0.9827(3) 0.1256(3) 0.0404(2) 0.0162(9) Uani 1 1 d . . . H47 H 1.0492 0.1271 0.0195 0.019 Uiso 1 1 calc R . . C48 C 0.9758(4) 0.1638(3) 0.1130(2) 0.0165(9) Uani 1 1 d . . . C49 C 0.8774(4) 0.1620(3) 0.1432(3) 0.0191(10) Uani 1 1 d . . . H49 H 0.8714 0.1899 0.1926 0.023 Uiso 1 1 calc R . . C50 C 0.7883(3) 0.1206(3) 0.1029(2) 0.0160(9) Uani 1 1 d . . . C51 C 0.7987(4) 0.0816(3) 0.0302(2) 0.0166(9) Uani 1 1 d . . . C52 C 0.6833(4) 0.1211(3) 0.1378(3) 0.0195(10) Uani 1 1 d . . . H52A H 0.6252 0.1309 0.1093 0.023 Uiso 1 1 calc R . . H52B H 0.6859 0.1676 0.1844 0.023 Uiso 1 1 calc R . . C53 C 0.4752(4) 0.2502(3) -0.0017(3) 0.0302(12) Uani 1 1 d . . . H53 H 0.5014 0.2838 -0.0242 0.036 Uiso 1 1 calc R . . C54 C 0.5178(4) 0.1751(4) -0.0160(3) 0.0351(14) Uani 1 1 d . . . H54 H 0.5753 0.1575 -0.0472 0.042 Uiso 1 1 calc R . . C55 C 0.4780(5) 0.1257(4) 0.0142(3) 0.0381(15) Uani 1 1 d . . . H55 H 0.5055 0.0727 0.0031 0.046 Uiso 1 1 calc R . . C56 C 0.3976(5) 0.1538(4) 0.0609(3) 0.0375(14) Uani 1 1 d . . . H56 H 0.3700 0.1205 0.0832 0.045 Uiso 1 1 calc R . . C57 C 0.3571(4) 0.2286(3) 0.0756(3) 0.0317(13) Uani 1 1 d . . . H57 H 0.3012 0.2475 0.1080 0.038 Uiso 1 1 calc R . . C58A C 0.5856(10) 0.3971(8) 0.1565(7) 0.040(3) Uiso 0.60 1 d P A 2 H58A H 0.5303 0.4136 0.1895 0.049 Uiso 0.60 1 calc PR A 2 C58B C 0.5615(16) 0.4205(13) 0.1449(11) 0.051(5) Uiso 0.40 1 d P B 1 H58B H 0.5013 0.4519 0.1657 0.061 Uiso 0.40 1 calc PR B 1 C59A C 0.6509(13) 0.3339(9) 0.1529(8) 0.053(3) Uiso 0.60 1 d P A 2 H59A H 0.6411 0.3082 0.1847 0.064 Uiso 0.60 1 calc PR A 2 C59B C 0.6131(19) 0.3692(16) 0.1726(12) 0.062(6) Uiso 0.40 1 d P B 1 H59B H 0.5821 0.3626 0.2114 0.075 Uiso 0.40 1 calc PR B 1 C60A C 0.7268(10) 0.3085(8) 0.1063(8) 0.051(3) Uiso 0.60 1 d P A 2 H60A H 0.7720 0.2659 0.1054 0.061 Uiso 0.60 1 calc PR A 2 C60B C 0.6998(14) 0.3308(9) 0.1481(9) 0.029(3) Uiso 0.40 1 d P B 1 H60B H 0.7340 0.3016 0.1718 0.035 Uiso 0.40 1 calc PR B 1 C61A C 0.7403(9) 0.3447(7) 0.0584(6) 0.036(2) Uiso 0.60 1 d P A 2 H61A H 0.7922 0.3255 0.0232 0.044 Uiso 0.60 1 calc PR A 2 C61B C 0.7421(14) 0.3317(11) 0.0892(10) 0.042(4) Uiso 0.40 1 d P B 1 H61B H 0.8048 0.3029 0.0700 0.050 Uiso 0.40 1 calc PR B 1 C62A C 0.6777(9) 0.4076(7) 0.0635(6) 0.028(3) Uiso 0.60 1 d P A 2 H62A H 0.6873 0.4334 0.0318 0.034 Uiso 0.60 1 calc PR A 2 C62B C 0.6859(18) 0.3801(14) 0.0561(12) 0.052(6) Uiso 0.40 1 d P B 1 H62B H 0.7092 0.3810 0.0132 0.062 Uiso 0.40 1 calc PR B 1 C63 C 0.8376(4) 0.5548(3) 0.2096(3) 0.0337(13) Uani 1 1 d . . . H63 H 0.8209 0.5917 0.1884 0.040 Uiso 1 1 calc R . . C64 C 0.7881(5) 0.5612(4) 0.2696(3) 0.0443(16) Uani 1 1 d . . . H64 H 0.7370 0.6022 0.2899 0.053 Uiso 1 1 calc R . . C65 C 0.8127(5) 0.5076(5) 0.3008(4) 0.0532(18) Uani 1 1 d . . . H65 H 0.7790 0.5111 0.3424 0.064 Uiso 1 1 calc R . . C66 C 0.8867(5) 0.4496(4) 0.2700(4) 0.0463(16) Uani 1 1 d . . . H66 H 0.9048 0.4126 0.2908 0.056 Uiso 1 1 calc R . . C67 C 0.9348(5) 0.4437(4) 0.2101(3) 0.0355(13) Uani 1 1 d . . . H67 H 0.9857 0.4028 0.1892 0.043 Uiso 1 1 calc R . . H68 H 0.836(6) -0.046(4) -0.688(4) 0.06(2) Uiso 1 1 d . . . H69 H 0.777(4) -0.009(3) -0.573(3) 0.021(17) Uiso 1 1 d . . . H70 H 1.000(5) 0.121(4) -0.306(3) 0.032(18) Uiso 1 1 d . . . H71 H 0.541(4) -0.104(3) -0.212(3) 0.008(16) Uiso 1 1 d . . . H72 H 0.739(4) -0.058(3) -0.164(3) 0.004(16) Uiso 1 1 d . . . H73 H 0.718(4) 0.017(3) -0.040(3) 0.002(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01613(11) 0.01472(11) 0.02521(12) 0.00770(9) -0.00021(8) 0.00098(8) Yb2 0.02294(12) 0.01563(12) 0.03770(15) 0.00663(10) 0.00023(10) 0.00046(9) S3 0.0141(5) 0.0154(6) 0.0234(6) 0.0060(5) 0.0010(5) 0.0010(4) S4 0.0175(6) 0.0142(6) 0.0283(7) 0.0075(5) -0.0004(5) -0.0002(5) S5 0.0229(6) 0.0165(6) 0.0259(7) 0.0082(5) 0.0029(5) 0.0021(5) S6 0.0172(6) 0.0202(6) 0.0170(6) 0.0077(5) -0.0019(5) -0.0023(5) S7 0.0173(6) 0.0162(6) 0.0245(6) 0.0075(5) 0.0026(5) 0.0013(5) S9 0.0303(7) 0.0399(8) 0.0236(7) 0.0116(6) 0.0034(6) 0.0056(6) O1 0.0245(19) 0.0215(19) 0.041(2) 0.0052(17) -0.0021(17) -0.0022(15) O2 0.031(2) 0.0223(19) 0.039(2) 0.0110(17) 0.0126(17) 0.0072(16) O3 0.042(2) 0.024(2) 0.030(2) 0.0159(17) -0.0009(17) 0.0014(17) O4 0.024(2) 0.0180(18) 0.029(2) 0.0094(16) 0.0044(16) 0.0029(16) O5 0.060(3) 0.039(3) 0.043(3) 0.010(2) 0.020(2) 0.007(2) O6 0.051(3) 0.085(4) 0.029(2) 0.025(2) 0.009(2) 0.020(3) O7 0.029(2) 0.059(3) 0.049(3) 0.013(2) 0.007(2) 0.004(2) O8 0.023(2) 0.033(2) 0.029(2) 0.0137(19) -0.0010(17) 0.0078(17) O9 0.0257(19) 0.0220(18) 0.028(2) 0.0102(16) 0.0095(15) 0.0014(15) O10 0.0232(18) 0.0183(18) 0.029(2) 0.0071(15) 0.0048(15) 0.0030(14) O11 0.0221(18) 0.0244(19) 0.038(2) 0.0121(17) -0.0050(16) -0.0012(15) O12 0.0200(18) 0.022(2) 0.044(2) 0.0185(19) -0.0112(16) -0.0064(16) O13 0.022(2) 0.030(2) 0.080(3) 0.017(2) 0.000(2) -0.0013(17) O14 0.035(2) 0.029(2) 0.051(3) 0.022(2) 0.0090(19) 0.0059(17) O15 0.027(2) 0.030(2) 0.032(2) 0.0037(17) -0.0013(16) 0.0003(16) O16 0.031(2) 0.024(2) 0.044(2) 0.0030(18) -0.0073(18) 0.0058(16) O17 0.034(2) 0.030(2) 0.044(2) 0.0112(19) -0.0088(18) 0.0004(17) O18 0.043(2) 0.020(2) 0.040(2) 0.0040(18) 0.0137(19) -0.0027(17) O19 0.030(2) 0.023(2) 0.081(3) 0.028(2) 0.000(2) 0.0038(17) O20 0.0276(19) 0.040(2) 0.0164(18) 0.0070(17) -0.0024(15) -0.0097(17) O21 0.0268(19) 0.0188(18) 0.0260(19) 0.0103(15) -0.0061(15) -0.0056(14) O22 0.0216(18) 0.0249(19) 0.034(2) 0.0097(17) -0.0081(16) 0.0021(15) O23 0.0179(18) 0.027(2) 0.018(2) 0.0045(17) 0.0009(16) -0.0044(15) O24 0.0224(18) 0.0160(17) 0.037(2) 0.0064(16) -0.0057(16) -0.0026(14) O25 0.0209(18) 0.0170(18) 0.047(2) 0.0087(17) 0.0005(16) 0.0027(14) O26 0.039(2) 0.028(2) 0.037(2) 0.0194(18) 0.0051(18) -0.0025(17) O27 0.0199(19) 0.0148(19) 0.030(2) 0.0118(16) -0.0004(16) 0.0044(16) O28 0.0130(16) 0.0205(18) 0.0247(18) 0.0061(15) 0.0017(13) 0.0012(13) O29 0.0184(17) 0.0182(18) 0.040(2) 0.0105(16) 0.0108(16) 0.0031(14) O30 0.032(2) 0.025(2) 0.028(2) 0.0086(17) -0.0036(16) 0.0071(16) O31 0.0152(19) 0.024(2) 0.036(2) 0.0145(17) 0.0116(17) 0.0034(16) O32 0.0237(19) 0.028(2) 0.042(2) 0.0143(18) 0.0084(17) -0.0005(16) O33 0.0251(19) 0.0187(19) 0.050(2) 0.0075(18) -0.0063(17) -0.0030(15) O34 0.0287(19) 0.0233(19) 0.026(2) 0.0079(16) 0.0011(15) 0.0028(15) O35 0.0264(19) 0.0202(18) 0.030(2) 0.0087(16) 0.0059(16) -0.0013(15) O36 0.0246(18) 0.0222(18) 0.0259(19) 0.0082(16) -0.0024(15) 0.0003(15) O37 0.0307(19) 0.0188(18) 0.030(2) 0.0088(16) 0.0004(16) 0.0037(15) O38 0.038(2) 0.0148(18) 0.046(2) 0.0037(17) -0.0139(19) 0.0071(16) O40 0.032(2) 0.058(3) 0.028(2) 0.021(2) 0.0075(17) 0.0156(19) O41 0.030(2) 0.050(3) 0.052(3) 0.023(2) 0.008(2) 0.0061(19) O42 0.028(2) 0.045(3) 0.046(3) 0.008(2) 0.0060(19) 0.0000(19) O43 0.056(3) 0.050(3) 0.064(3) 0.008(3) -0.006(3) 0.002(2) O44 0.057(3) 0.034(2) 0.040(2) 0.018(2) -0.001(2) 0.000(2) O45 0.030(2) 0.052(3) 0.065(3) 0.024(3) 0.003(2) 0.000(2) O46 0.032(2) 0.026(2) 0.045(2) 0.0165(19) -0.0026(18) 0.0008(16) O47 0.080(4) 0.053(3) 0.052(3) 0.021(3) -0.021(3) -0.018(3) O48 0.071(4) 0.089(4) 0.056(3) 0.030(3) -0.009(3) 0.027(3) O49A 0.078(13) 0.049(8) 0.031(8) 0.016(6) 0.007(10) -0.003(11) O49B 0.056(14) 0.050(9) 0.026(10) 0.015(7) 0.001(10) -0.002(13) O49C 0.045(16) 0.028(12) 0.018(13) 0.015(10) 0.000(11) -0.007(12) N1 0.027(2) 0.023(2) 0.022(2) 0.0027(19) 0.0067(18) -0.0009(19) N2 0.030(2) 0.021(2) 0.042(3) 0.015(2) -0.001(2) -0.0009(19) N3 0.020(2) 0.015(2) 0.033(2) 0.0065(18) -0.0049(18) 0.0012(17) N5 0.026(2) 0.027(2) 0.028(2) 0.013(2) -0.0057(19) -0.0023(19) C1 0.014(2) 0.021(2) 0.019(2) 0.006(2) -0.0048(18) -0.0017(19) C2 0.021(2) 0.018(2) 0.015(2) 0.0067(19) 0.0003(19) -0.0001(19) C3 0.021(2) 0.018(2) 0.016(2) 0.007(2) 0.0005(19) 0.0027(19) C4 0.018(2) 0.022(2) 0.019(2) 0.010(2) 0.0014(19) 0.0052(19) C5 0.019(2) 0.021(2) 0.016(2) 0.009(2) 0.0003(19) -0.0016(19) C6 0.024(2) 0.017(2) 0.017(2) 0.007(2) -0.005(2) 0.001(2) C7 0.014(2) 0.026(3) 0.020(3) 0.011(2) -0.0021(19) -0.0019(19) C8 0.022(2) 0.014(2) 0.024(3) 0.010(2) 0.002(2) -0.0041(19) C9 0.022(3) 0.029(3) 0.023(3) 0.015(2) -0.004(2) -0.002(2) C10 0.022(3) 0.034(3) 0.024(3) 0.015(2) 0.001(2) 0.003(2) C11 0.023(3) 0.036(3) 0.023(3) 0.016(2) -0.001(2) -0.006(2) C12 0.022(3) 0.022(3) 0.032(3) 0.019(2) -0.003(2) -0.004(2) C13 0.020(2) 0.021(3) 0.026(3) 0.014(2) -0.001(2) 0.000(2) C14 0.023(3) 0.035(3) 0.035(3) 0.026(3) -0.007(2) -0.005(2) C15 0.017(2) 0.020(2) 0.019(2) 0.009(2) 0.0003(19) 0.0020(19) C16 0.017(2) 0.021(2) 0.015(2) 0.006(2) -0.0011(18) 0.0012(19) C17 0.017(2) 0.014(2) 0.019(2) 0.0046(19) 0.0023(19) -0.0021(18) C18 0.020(2) 0.021(2) 0.018(2) 0.009(2) 0.0055(19) 0.007(2) C19 0.017(2) 0.015(2) 0.017(2) 0.0050(19) 0.0073(18) 0.0086(18) C20 0.019(2) 0.020(2) 0.020(2) 0.009(2) 0.0036(19) 0.0004(19) C21 0.020(2) 0.019(2) 0.018(2) 0.010(2) -0.0010(19) 0.0003(19) C22 0.031(3) 0.032(3) 0.024(3) 0.010(2) -0.004(2) -0.002(2) C23 0.035(3) 0.037(3) 0.027(3) 0.013(3) 0.000(2) -0.007(3) C24 0.052(4) 0.030(3) 0.028(3) 0.012(3) 0.014(3) 0.000(3) C25 0.046(4) 0.042(4) 0.040(4) 0.026(3) 0.011(3) 0.017(3) C26 0.029(3) 0.048(4) 0.025(3) 0.014(3) 0.005(2) 0.007(3) C27 0.035(3) 0.031(3) 0.034(3) 0.016(3) -0.006(3) -0.010(2) C28 0.059(4) 0.026(3) 0.036(3) 0.016(3) 0.001(3) -0.001(3) C29 0.053(4) 0.035(3) 0.040(4) 0.022(3) 0.004(3) 0.015(3) C30 0.037(3) 0.042(4) 0.045(4) 0.017(3) -0.004(3) 0.007(3) C31 0.033(3) 0.032(3) 0.059(4) 0.021(3) -0.008(3) -0.003(3) C32 0.017(2) 0.016(2) 0.011(2) 0.0036(18) -0.0013(18) -0.0022(18) C33 0.016(2) 0.021(2) 0.016(2) 0.007(2) 0.0025(18) -0.0017(19) C34 0.015(2) 0.016(2) 0.017(2) 0.0030(19) -0.0010(18) 0.0011(18) C35 0.017(2) 0.018(2) 0.023(3) 0.009(2) -0.0008(19) -0.0016(19) C36 0.012(2) 0.020(2) 0.012(2) 0.0026(19) -0.0052(17) -0.0021(18) C37 0.013(2) 0.015(2) 0.016(2) 0.0049(19) -0.0009(18) 0.0009(18) C38 0.016(2) 0.015(2) 0.013(2) 0.0025(18) -0.0020(18) -0.0026(18) C39 0.009(2) 0.018(2) 0.014(2) 0.0036(19) 0.0051(17) 0.0009(17) C40 0.015(2) 0.020(2) 0.016(2) 0.007(2) 0.0047(18) 0.0045(19) C41 0.018(2) 0.015(2) 0.018(2) 0.0071(19) 0.0028(19) -0.0024(18) C42 0.012(2) 0.018(2) 0.018(2) 0.0038(19) 0.0019(18) -0.0005(18) C43 0.013(2) 0.016(2) 0.015(2) 0.0069(19) 0.0018(17) 0.0019(18) C44 0.014(2) 0.016(2) 0.012(2) 0.0046(18) 0.0027(17) 0.0009(18) C45 0.012(2) 0.018(2) 0.021(2) 0.009(2) 0.0003(18) 0.0011(18) C46 0.018(2) 0.014(2) 0.013(2) 0.0056(18) -0.0010(18) 0.0024(18) C47 0.011(2) 0.020(2) 0.019(2) 0.009(2) 0.0024(18) 0.0001(18) C48 0.018(2) 0.016(2) 0.018(2) 0.011(2) -0.0036(19) -0.0008(18) C49 0.023(2) 0.017(2) 0.020(3) 0.011(2) 0.001(2) 0.0021(19) C50 0.014(2) 0.015(2) 0.022(3) 0.010(2) 0.0023(19) 0.0028(18) C51 0.017(2) 0.016(2) 0.019(2) 0.010(2) -0.0022(19) 0.0012(18) C52 0.017(2) 0.020(2) 0.023(3) 0.010(2) 0.0026(19) 0.0019(19) C53 0.028(3) 0.036(3) 0.030(3) 0.017(3) -0.004(2) -0.002(2) C54 0.028(3) 0.045(4) 0.026(3) 0.008(3) -0.003(2) 0.013(3) C55 0.033(3) 0.025(3) 0.049(4) 0.009(3) -0.018(3) 0.005(2) C56 0.036(3) 0.030(3) 0.055(4) 0.026(3) -0.008(3) 0.000(3) C57 0.029(3) 0.033(3) 0.034(3) 0.014(3) 0.000(2) -0.004(2) C63 0.032(3) 0.030(3) 0.040(3) 0.015(3) 0.004(3) 0.008(2) C64 0.042(4) 0.050(4) 0.039(4) 0.016(3) 0.011(3) 0.008(3) C65 0.045(4) 0.077(5) 0.047(4) 0.036(4) 0.010(3) -0.003(4) C66 0.040(4) 0.058(4) 0.055(4) 0.039(4) 0.000(3) -0.005(3) C67 0.033(3) 0.034(3) 0.043(4) 0.019(3) -0.003(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O38 2.260(4) . ? Yb1 O32 2.279(4) . ? Yb1 O35 2.334(3) . ? Yb1 O34 2.335(4) . ? Yb1 O37 2.343(3) . ? Yb1 O33 2.353(3) . ? Yb1 O28 2.385(3) . ? Yb1 O36 2.402(3) . ? Yb2 O19 2.259(4) . ? Yb2 O10 2.267(3) . ? Yb2 O18 2.328(4) . ? Yb2 O14 2.343(4) . ? Yb2 O13 2.349(4) . ? Yb2 O17 2.354(4) . ? Yb2 O15 2.359(4) . ? Yb2 O16 2.421(4) . ? S3 O29 1.449(3) . ? S3 O30 1.456(4) . ? S3 O28 1.467(3) . ? S3 C34 1.757(5) . ? S4 O26 1.448(4) . ? S4 O24 1.460(4) . ? S4 O25 1.463(4) . ? S4 C41 1.773(5) . ? S5 O2 1.455(4) . ? S5 O3 1.457(4) . ? S5 O1 1.470(4) . ? S5 C3 1.763(5) . ? S6 O20 1.453(4) . ? S6 O22 1.455(4) . ? S6 O21 1.460(3) . ? S6 C48 1.758(5) . ? S7 O11 1.445(4) . ? S7 O9 1.459(4) . ? S7 O10 1.475(3) . ? S7 C17 1.760(5) . ? S9 O5 1.418(5) . ? S9 O7 1.434(4) . ? S9 O6 1.440(4) . ? S9 C10 1.753(5) . ? O4 C6 1.365(6) . ? O8 C13 1.364(6) . ? O12 C20 1.360(6) . ? O18 N1 1.338(5) . ? O19 N2 1.343(5) . ? O23 C51 1.373(6) . ? O27 C44 1.382(6) . ? O31 C37 1.366(6) . ? O38 N3 1.341(5) . ? O39A N4A 1.310(9) . ? O39B N4B 1.362(17) . ? O40 N5 1.330(6) . ? N1 C22 1.341(7) . ? N1 C26 1.342(7) . ? N2 C27 1.337(7) . ? N2 C31 1.345(7) . ? N3 C57 1.344(6) . ? N3 C53 1.347(7) . ? N4A C58A 1.349(16) . ? N4A C62A 1.363(14) . ? N4B C62B 1.27(3) . ? N4B C58B 1.34(2) . ? N5 C63 1.346(7) . ? N5 C67 1.355(7) . ? C1 C2 1.374(6) . ? C1 C6 1.417(7) . ? C1 C21 1.516(6) 2_754 ? C2 C3 1.398(6) . ? C3 C4 1.391(6) . ? C4 C5 1.388(6) . ? C5 C6 1.396(7) . ? C5 C7 1.530(6) . ? C7 C8 1.515(7) . ? C8 C9 1.392(7) . ? C8 C13 1.414(6) . ? C9 C10 1.385(7) . ? C10 C11 1.379(7) . ? C11 C12 1.389(7) . ? C12 C13 1.393(7) . ? C12 C14 1.511(6) . ? C14 C15 1.514(6) . ? C15 C16 1.379(6) . ? C15 C20 1.390(6) . ? C16 C17 1.388(6) . ? C17 C18 1.405(6) . ? C18 C19 1.372(7) . ? C19 C20 1.407(6) . ? C19 C21 1.512(6) . ? C21 C1 1.516(6) 2_754 ? C22 C23 1.370(7) . ? C23 C24 1.354(8) . ? C24 C25 1.372(8) . ? C25 C26 1.372(8) . ? C27 C28 1.377(8) . ? C28 C29 1.363(8) . ? C29 C30 1.373(9) . ? C30 C31 1.371(8) . ? C32 C33 1.380(6) . ? C32 C37 1.408(6) . ? C32 C52 1.511(6) 2_655 ? C33 C34 1.389(6) . ? C34 C35 1.398(6) . ? C35 C36 1.381(6) . ? C36 C37 1.401(6) . ? C36 C38 1.526(6) . ? C38 C39 1.523(6) . ? C39 C40 1.378(6) . ? C39 C44 1.404(6) . ? C40 C41 1.383(6) . ? C41 C42 1.388(6) . ? C42 C43 1.390(6) . ? C43 C44 1.403(6) . ? C43 C45 1.528(6) . ? C45 C46 1.529(6) . ? C46 C47 1.390(6) . ? C46 C51 1.395(6) . ? C47 C48 1.392(6) . ? C48 C49 1.397(6) . ? C49 C50 1.384(6) . ? C50 C51 1.398(6) . ? C50 C52 1.511(6) . ? C52 C32 1.511(6) 2_655 ? C53 C54 1.370(8) . ? C54 C55 1.361(8) . ? C55 C56 1.370(9) . ? C56 C57 1.354(8) . ? C58A C59A 1.38(2) . ? C58B C59B 1.42(3) . ? C59A C60A 1.32(2) . ? C59B C60B 1.29(3) . ? C60A C61A 1.396(17) . ? C60B C61B 1.35(3) . ? C61A C62A 1.350(16) . ? C61B C62B 1.48(3) . ? C63 C64 1.370(8) . ? C64 C65 1.386(9) . ? C65 C66 1.367(9) . ? C66 C67 1.363(9) . ? 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 O38 Yb1 O32 97.71(15) . . ? O38 Yb1 O35 89.75(14) . . ? O32 Yb1 O35 144.20(13) . . ? O38 Yb1 O34 83.11(13) . . ? O32 Yb1 O34 145.25(13) . . ? O35 Yb1 O34 70.28(12) . . ? O38 Yb1 O37 144.77(12) . . ? O32 Yb1 O37 85.46(13) . . ? O35 Yb1 O37 108.05(12) . . ? O34 Yb1 O37 75.22(12) . . ? O38 Yb1 O33 69.95(13) . . ? O32 Yb1 O33 74.62(14) . . ? O35 Yb1 O33 139.89(13) . . ? O34 Yb1 O33 73.12(13) . . ? O37 Yb1 O33 77.27(12) . . ? O38 Yb1 O28 73.49(12) . . ? O32 Yb1 O28 72.61(12) . . ? O35 Yb1 O28 76.17(11) . . ? O34 Yb1 O28 138.86(11) . . ? O37 Yb1 O28 139.37(12) . . ? O33 Yb1 O28 126.12(12) . . ? O38 Yb1 O36 146.08(12) . . ? O32 Yb1 O36 79.05(13) . . ? O35 Yb1 O36 75.56(12) . . ? O34 Yb1 O36 118.61(12) . . ? O37 Yb1 O36 69.07(12) . . ? O33 Yb1 O36 138.46(12) . . ? O28 Yb1 O36 73.36(11) . . ? O19 Yb2 O10 145.81(14) . . ? O19 Yb2 O18 140.97(14) . . ? O10 Yb2 O18 73.04(12) . . ? O19 Yb2 O14 73.68(15) . . ? O10 Yb2 O14 74.75(13) . . ? O18 Yb2 O14 137.55(13) . . ? O19 Yb2 O13 79.08(14) . . ? O10 Yb2 O13 79.35(13) . . ? O18 Yb2 O13 126.13(15) . . ? O14 Yb2 O13 72.73(15) . . ? O19 Yb2 O17 82.40(15) . . ? O10 Yb2 O17 115.81(13) . . ? O18 Yb2 O17 78.82(14) . . ? O14 Yb2 O17 141.16(14) . . ? O13 Yb2 O17 73.01(15) . . ? O19 Yb2 O15 95.01(14) . . ? O10 Yb2 O15 85.79(13) . . ? O18 Yb2 O15 81.50(14) . . ? O14 Yb2 O15 69.22(13) . . ? O13 Yb2 O15 141.58(15) . . ? O17 Yb2 O15 144.43(13) . . ? O19 Yb2 O16 75.62(14) . . ? O10 Yb2 O16 135.49(13) . . ? O18 Yb2 O16 66.43(14) . . ? O14 Yb2 O16 126.48(13) . . ? O13 Yb2 O16 140.48(14) . . ? O17 Yb2 O16 73.95(13) . . ? O15 Yb2 O16 71.08(13) . . ? O29 S3 O30 112.2(2) . . ? O29 S3 O28 111.8(2) . . ? O30 S3 O28 109.9(2) . . ? O29 S3 C34 106.6(2) . . ? O30 S3 C34 108.4(2) . . ? O28 S3 C34 107.7(2) . . ? O26 S4 O24 113.4(2) . . ? O26 S4 O25 112.2(2) . . ? O24 S4 O25 111.0(2) . . ? O26 S4 C41 107.0(2) . . ? O24 S4 C41 107.2(2) . . ? O25 S4 C41 105.5(2) . . ? O2 S5 O3 113.5(2) . . ? O2 S5 O1 111.2(2) . . ? O3 S5 O1 111.3(2) . . ? O2 S5 C3 107.8(2) . . ? O3 S5 C3 106.2(2) . . ? O1 S5 C3 106.4(2) . . ? O20 S6 O22 113.3(2) . . ? O20 S6 O21 112.6(2) . . ? O22 S6 O21 111.6(2) . . ? O20 S6 C48 105.6(2) . . ? O22 S6 C48 106.6(2) . . ? O21 S6 C48 106.4(2) . . ? O11 S7 O9 114.2(2) . . ? O11 S7 O10 111.6(2) . . ? O9 S7 O10 110.7(2) . . ? O11 S7 C17 107.4(2) . . ? O9 S7 C17 107.1(2) . . ? O10 S7 C17 105.3(2) . . ? O5 S9 O7 112.6(3) . . ? O5 S9 O6 112.1(3) . . ? O7 S9 O6 112.2(3) . . ? O5 S9 C10 106.1(3) . . ? O7 S9 C10 107.2(3) . . ? O6 S9 C10 106.0(3) . . ? S7 O10 Yb2 146.2(2) . . ? N1 O18 Yb2 128.0(3) . . ? N2 O19 Yb2 137.0(3) . . ? S3 O28 Yb1 135.13(18) . . ? N3 O38 Yb1 128.3(3) . . ? O18 N1 C22 119.7(5) . . ? O18 N1 C26 119.8(5) . . ? C22 N1 C26 120.4(5) . . ? C27 N2 O19 117.7(5) . . ? C27 N2 C31 121.9(5) . . ? O19 N2 C31 120.3(4) . . ? O38 N3 C57 119.6(4) . . ? O38 N3 C53 119.5(4) . . ? C57 N3 C53 121.0(5) . . ? O39A N4A C58A 123.2(10) . . ? O39A N4A C62A 117.6(9) . . ? C58A N4A C62A 119.2(10) . . ? C62B N4B C58B 126.6(17) . . ? C62B N4B O39B 116.4(17) . . ? C58B N4B O39B 116.8(15) . . ? O40 N5 C63 120.2(4) . . ? O40 N5 C67 119.1(5) . . ? C63 N5 C67 120.7(5) . . ? C2 C1 C6 117.4(4) . . ? C2 C1 C21 120.0(4) . 2_754 ? C6 C1 C21 122.6(4) . 2_754 ? C1 C2 C3 121.8(4) . . ? C4 C3 C2 120.1(4) . . ? C4 C3 S5 122.0(4) . . ? C2 C3 S5 117.8(4) . . ? C5 C4 C3 119.7(4) . . ? C4 C5 C6 119.4(4) . . ? C4 C5 C7 120.9(4) . . ? C6 C5 C7 119.7(4) . . ? O4 C6 C5 115.8(4) . . ? O4 C6 C1 122.6(4) . . ? C5 C6 C1 121.6(4) . . ? C8 C7 C5 111.8(4) . . ? C9 C8 C13 117.9(4) . . ? C9 C8 C7 120.4(4) . . ? C13 C8 C7 121.7(4) . . ? C10 C9 C8 120.8(5) . . ? C11 C10 C9 120.1(5) . . ? C11 C10 S9 118.8(4) . . ? C9 C10 S9 120.9(4) . . ? C10 C11 C12 121.2(5) . . ? C11 C12 C13 118.3(4) . . ? C11 C12 C14 118.7(5) . . ? C13 C12 C14 122.8(5) . . ? O8 C13 C12 116.7(4) . . ? O8 C13 C8 121.9(4) . . ? C12 C13 C8 121.4(5) . . ? C12 C14 C15 116.6(4) . . ? C16 C15 C20 118.6(4) . . ? C16 C15 C14 123.2(4) . . ? C20 C15 C14 118.1(4) . . ? C15 C16 C17 120.1(4) . . ? C16 C17 C18 120.9(4) . . ? C16 C17 S7 121.3(4) . . ? C18 C17 S7 117.8(3) . . ? C19 C18 C17 119.8(4) . . ? C18 C19 C20 118.4(4) . . ? C18 C19 C21 120.8(4) . . ? C20 C19 C21 120.7(4) . . ? O12 C20 C15 122.1(4) . . ? O12 C20 C19 115.7(4) . . ? C15 C20 C19 122.2(4) . . ? C19 C21 C1 113.8(4) . 2_754 ? N1 C22 C23 120.9(5) . . ? C24 C23 C22 119.4(5) . . ? C23 C24 C25 119.6(6) . . ? C26 C25 C24 119.8(5) . . ? N1 C26 C25 119.9(5) . . ? N2 C27 C28 119.5(5) . . ? C29 C28 C27 119.9(6) . . ? C28 C29 C30 119.3(5) . . ? C31 C30 C29 120.1(6) . . ? N2 C31 C30 119.2(5) . . ? C33 C32 C37 118.2(4) . . ? C33 C32 C52 123.1(4) . 2_655 ? C37 C32 C52 118.6(4) . 2_655 ? C32 C33 C34 120.9(4) . . ? C33 C34 C35 120.1(4) . . ? C33 C34 S3 118.8(3) . . ? C35 C34 S3 121.0(4) . . ? C36 C35 C34 120.7(4) . . ? C35 C36 C37 118.3(4) . . ? C35 C36 C38 120.2(4) . . ? C37 C36 C38 121.4(4) . . ? O31 C37 C36 124.3(4) . . ? O31 C37 C32 113.8(4) . . ? C36 C37 C32 121.8(4) . . ? C39 C38 C36 116.0(4) . . ? C40 C39 C44 117.4(4) . . ? C40 C39 C38 120.3(4) . . ? C44 C39 C38 122.2(4) . . ? C39 C40 C41 121.5(4) . . ? C40 C41 C42 120.4(4) . . ? C40 C41 S4 118.0(4) . . ? C42 C41 S4 121.6(4) . . ? C41 C42 C43 120.3(4) . . ? C42 C43 C44 118.0(4) . . ? C42 C43 C45 119.9(4) . . ? C44 C43 C45 122.1(4) . . ? O27 C44 C43 120.7(4) . . ? O27 C44 C39 116.8(4) . . ? C43 C44 C39 122.3(4) . . ? C43 C45 C46 112.5(4) . . ? C47 C46 C51 118.1(4) . . ? C47 C46 C45 120.2(4) . . ? C51 C46 C45 121.7(4) . . ? C46 C47 C48 121.3(4) . . ? C47 C48 C49 118.9(4) . . ? C47 C48 S6 121.5(4) . . ? C49 C48 S6 119.6(4) . . ? C50 C49 C48 121.5(4) . . ? C49 C50 C51 118.1(4) . . ? C49 C50 C52 119.6(4) . . ? C51 C50 C52 122.4(4) . . ? O23 C51 C46 122.5(4) . . ? O23 C51 C50 115.4(4) . . ? C46 C51 C50 122.1(4) . . ? C50 C52 C32 115.1(4) . 2_655 ? N3 C53 C54 119.5(5) . . ? C55 C54 C53 120.4(5) . . ? C54 C55 C56 118.6(5) . . ? C57 C56 C55 120.6(6) . . ? N3 C57 C56 119.9(5) . . ? N4A C58A C59A 119.4(12) . . ? N4B C58B C59B 113.6(18) . . ? C60A C59A C58A 121.4(13) . . ? C60B C59B C58B 124(2) . . ? C59A C60A C61A 119.7(12) . . ? C59B C60B C61B 120.7(17) . . ? C62A C61A C60A 118.3(10) . . ? C60B C61B C62B 116.6(17) . . ? C61A C62A N4A 121.9(10) . . ? N4B C62B C61B 118(2) . . ? N5 C63 C64 120.4(5) . . ? C63 C64 C65 119.8(6) . . ? C66 C65 C64 118.3(6) . . ? C67 C66 C65 121.2(6) . . ? N5 C67 C66 119.6(6) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.713 _refine_diff_density_min -1.466 _refine_diff_density_rms 0.133