Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 200 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Dickins, Rachel S.' 'Love, Christine S.' 'Puschmann, Horst' _publ_contact_author_name 'Dr Rachel S Dickins' _publ_contact_author_address ; Department of Chemistry University of Durham South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email 'R.S.DICKINS@DURHAM.AC.UK' _publ_section_title ; Bidentate lactate binding in aqueous solution at a cationic, heptadentate lanthanide centre : X-ray, near-IR CD and NMR studies ; data_01srv057 _database_code_CSD 172449 _publ_requested_journal 'test' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H56 Ho N7 O6, 2(C F3 O3 S), C H4 O, 2(H2 O)' _chemical_formula_sum 'C44 H64 F6 Ho N7 O15 S2' _chemical_formula_weight 1274.09 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' 'Ho' 'Ho' -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.280(2) _cell_length_b 11.950(4) _cell_length_c 12.423(3) _cell_angle_alpha 64.82(2) _cell_angle_beta 76.837(19) _cell_angle_gamma 62.38(2) _cell_volume 1341.9(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6816 _cell_measurement_theta_min 4.463 _cell_measurement_theta_max 54.984 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 1.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67991 _exptl_absorpt_correction_T_max 0.80139 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (3s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _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 SMART CCD 1K area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 14284 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10965 _reflns_number_gt 10951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SMART-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(4) _refine_ls_number_reflns 10965 _refine_ls_number_parameters 694 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Ho1 Ho 0.2579(1) 0.4128(1) 0.1442(1) 0.01011(4) Uani 1 1 d . . . O1 O 0.1844(2) 0.2919(2) 0.0914(2) 0.0166(5) Uani 1 1 d . . . O2 O 0.0782(3) 0.3579(2) 0.2790(2) 0.0182(5) Uani 1 1 d . . . O3 O 0.1431(3) 0.1057(3) 0.1673(3) 0.0252(6) Uani 1 1 d . . . O11 O 0.0446(2) 0.5929(2) 0.0914(2) 0.0143(5) Uani 1 1 d . . . O21 O 0.2201(2) 0.4818(2) 0.3011(2) 0.0144(5) Uani 1 1 d . . . O31 O 0.3564(2) 0.1993(2) 0.2887(2) 0.0161(5) Uani 1 1 d . . . N1 N 0.2374(3) 0.5389(3) -0.0831(2) 0.0140(5) Uani 1 1 d . . . N2 N 0.2864(3) 0.6363(3) 0.0796(2) 0.0123(5) Uani 1 1 d . . . N3 N 0.4959(3) 0.3602(3) 0.2016(3) 0.0135(5) Uani 1 1 d . . . N4 N 0.4476(3) 0.2782(3) 0.0318(3) 0.0151(5) Uani 1 1 d . . . N11 N -0.1130(3) 0.7453(3) -0.0442(3) 0.0168(6) Uani 1 1 d . . . H11N H -0.1335 0.7799 -0.1192 0.020 Uiso 1 1 calc R . . N22 N 0.1740(3) 0.6356(3) 0.3804(3) 0.0162(6) Uani 1 1 d . . . H22N H 0.1625 0.7179 0.3688 0.019 Uiso 1 1 calc R . . N33 N 0.4995(3) 0.0415(3) 0.4364(3) 0.0162(6) Uani 1 1 d . . . H33N H 0.5724 0.0170 0.4707 0.019 Uiso 1 1 calc R . . C1 C 0.2843(4) 0.6500(3) -0.1262(3) 0.0163(6) Uani 1 1 d . . . H1A H 0.2488 0.7147 -0.2059 0.020 Uiso 1 1 calc R . . H1B H 0.3832 0.6100 -0.1346 0.020 Uiso 1 1 calc R . . C2 C 0.2407(3) 0.7275(3) -0.0435(3) 0.0151(6) Uani 1 1 d . . . H2A H 0.2775 0.7968 -0.0752 0.018 Uiso 1 1 calc R . . H2B H 0.1418 0.7755 -0.0413 0.018 Uiso 1 1 calc R . . C3 C 0.4300(4) 0.6065(3) 0.0837(3) 0.0122(7) Uani 1 1 d . . . H3A H 0.4350 0.6883 0.0808 0.015 Uiso 1 1 calc R . . H3B H 0.4792 0.5873 0.0122 0.015 Uiso 1 1 calc R . . C4 C 0.4986(3) 0.4864(3) 0.1944(3) 0.0154(6) Uani 1 1 d . . . H4A H 0.5926 0.4726 0.1922 0.018 Uiso 1 1 calc R . . H4B H 0.4526 0.5067 0.2662 0.018 Uiso 1 1 calc R . . C5 C 0.6027(3) 0.3048(3) 0.1180(3) 0.0158(6) Uani 1 1 d . . . H5A H 0.6908 0.2575 0.1547 0.019 Uiso 1 1 calc R . . H5B H 0.6054 0.3811 0.0438 0.019 Uiso 1 1 calc R . . C6 C 0.5791(3) 0.2064(3) 0.0876(3) 0.0172(7) Uani 1 1 d . . . H6A H 0.6512 0.1723 0.0321 0.021 Uiso 1 1 calc R . . H6B H 0.5800 0.1276 0.1609 0.021 Uiso 1 1 calc R . . C7 C 0.4578(4) 0.3519(4) -0.0983(3) 0.0190(7) Uani 1 1 d . . . H7A H 0.5072 0.2859 -0.1383 0.023 Uiso 1 1 calc R . . H7B H 0.5075 0.4076 -0.1146 0.023 Uiso 1 1 calc R . . C8 C 0.3178(3) 0.4431(4) -0.1464(3) 0.0175(7) Uani 1 1 d . . . H8A H 0.3246 0.4957 -0.2324 0.021 Uiso 1 1 calc R . . H8B H 0.2717 0.3860 -0.1366 0.021 Uiso 1 1 calc R . . C10 C 0.0945(3) 0.5945(3) -0.1075(3) 0.0152(6) Uani 1 1 d . . . H10A H 0.0753 0.5226 -0.1096 0.018 Uiso 1 1 calc R . . H10B H 0.0753 0.6696 -0.1863 0.018 Uiso 1 1 calc R . . C11 C 0.0057(4) 0.6465(3) -0.0134(3) 0.0124(6) Uani 1 1 d . . . C12 C -0.2138(3) 0.8019(3) 0.0385(3) 0.0166(7) Uani 1 1 d . . . H12 H -0.2276 0.7254 0.1076 0.020 Uiso 1 1 calc R . . C13 C -0.3452(4) 0.8970(4) -0.0250(4) 0.0271(8) Uani 1 1 d . . . H13A H -0.3341 0.9739 -0.0919 0.041 Uiso 1 1 calc R . . H13B H -0.4153 0.9306 0.0307 0.041 Uiso 1 1 calc R . . H13C H -0.3706 0.8475 -0.0549 0.041 Uiso 1 1 calc R . . C14 C -0.1655(3) 0.8721(3) 0.0850(3) 0.0167(7) Uani 1 1 d . . . C15 C -0.1820(4) 0.8511(4) 0.2061(3) 0.0205(7) Uani 1 1 d . . . H15 H -0.2216 0.7918 0.2596 0.025 Uiso 1 1 calc R . . C16 C -0.1399(4) 0.9176(4) 0.2478(4) 0.0287(9) Uani 1 1 d . . . H16 H -0.1510 0.9037 0.3300 0.034 Uiso 1 1 calc R . . C17 C -0.0818(4) 1.0047(4) 0.1695(5) 0.0311(10) Uani 1 1 d . . . H17 H -0.0530 1.0496 0.1984 0.037 Uiso 1 1 calc R . . C18 C -0.0659(4) 1.0256(4) 0.0501(5) 0.0312(10) Uani 1 1 d . . . H18 H -0.0256 1.0846 -0.0029 0.037 Uiso 1 1 calc R . . C19 C -0.1086(4) 0.9608(4) 0.0065(4) 0.0222(7) Uani 1 1 d . . . H19 H -0.0990 0.9768 -0.0761 0.027 Uiso 1 1 calc R . . C20 C 0.2039(3) 0.7031(3) 0.1645(3) 0.0149(6) Uani 1 1 d . . . H20A H 0.1113 0.7608 0.1366 0.018 Uiso 1 1 calc R . . H20B H 0.2407 0.7626 0.1673 0.018 Uiso 1 1 calc R . . C21 C 0.2015(3) 0.5987(3) 0.2888(3) 0.0145(6) Uani 1 1 d . . . C22 C 0.1622(4) 0.5418(3) 0.5016(3) 0.0171(7) Uani 1 1 d . . . H22 H 0.1078 0.4961 0.5001 0.021 Uiso 1 1 calc R . . C23 C 0.0881(4) 0.6242(4) 0.5819(4) 0.0234(8) Uani 1 1 d . . . H23A H 0.1400 0.6702 0.5838 0.035 Uiso 1 1 calc R . . H23B H 0.0773 0.5630 0.6627 0.035 Uiso 1 1 calc R . . H23C H -0.0002 0.6921 0.5505 0.035 Uiso 1 1 calc R . . C24 C 0.2998(4) 0.4333(4) 0.5470(3) 0.0181(7) Uani 1 1 d . . . C25 C 0.3221(4) 0.2963(4) 0.6033(3) 0.0235(8) Uani 1 1 d . . . H25 H 0.2507 0.2711 0.6133 0.028 Uiso 1 1 calc R . . C26 C 0.4470(5) 0.1970(4) 0.6446(4) 0.0280(9) Uani 1 1 d . . . H26 H 0.4611 0.1042 0.6818 0.034 Uiso 1 1 calc R . . C27 C 0.5513(4) 0.2329(4) 0.6318(4) 0.0285(8) Uani 1 1 d . . . H27 H 0.6366 0.1647 0.6610 0.034 Uiso 1 1 calc R . . C28 C 0.5315(4) 0.3686(4) 0.5762(4) 0.0276(8) Uani 1 1 d . . . H28 H 0.6032 0.3931 0.5673 0.033 Uiso 1 1 calc R . . C29 C 0.4067(4) 0.4678(4) 0.5339(3) 0.0215(7) Uani 1 1 d . . . H29 H 0.3934 0.5603 0.4956 0.026 Uiso 1 1 calc R . . C30 C 0.5178(4) 0.2578(3) 0.3244(3) 0.0158(6) Uani 1 1 d . . . H30A H 0.4795 0.3047 0.3815 0.019 Uiso 1 1 calc R . . H30B H 0.6152 0.2047 0.3367 0.019 Uiso 1 1 calc R . . C31 C 0.4532(4) 0.1609(3) 0.3488(3) 0.0144(6) Uani 1 1 d . . . C32 C 0.4338(4) -0.0530(3) 0.4793(3) 0.0181(7) Uani 1 1 d . . . H32 H 0.3426 -0.0009 0.4457 0.022 Uiso 1 1 calc R . . C33 C 0.4160(4) -0.0988(4) 0.6141(3) 0.0232(8) Uani 1 1 d . . . H33A H 0.5025 -0.1363 0.6487 0.035 Uiso 1 1 calc R . . H33B H 0.3814 -0.1688 0.6445 0.035 Uiso 1 1 calc R . . H33C H 0.3526 -0.0209 0.6358 0.035 Uiso 1 1 calc R . . C34 C 0.5111(4) -0.1678(4) 0.4327(3) 0.0201(7) Uani 1 1 d . . . C35 C 0.4715(4) -0.1550(4) 0.3277(3) 0.0240(8) Uani 1 1 d . . . H35 H 0.3995 -0.0742 0.2856 0.029 Uiso 1 1 calc R . . C36 C 0.5363(5) -0.2589(4) 0.2847(4) 0.0303(9) Uani 1 1 d . . . H36 H 0.5085 -0.2497 0.2136 0.036 Uiso 1 1 calc R . . C37 C 0.6416(5) -0.3763(4) 0.3452(4) 0.0319(9) Uani 1 1 d . . . H37 H 0.6855 -0.4483 0.3162 0.038 Uiso 1 1 calc R . . C38 C 0.6835(5) -0.3892(4) 0.4484(4) 0.0317(9) Uani 1 1 d . . . H38 H 0.7568 -0.4694 0.4893 0.038 Uiso 1 1 calc R . . C39 C 0.6182(4) -0.2848(4) 0.4917(4) 0.0245(8) Uani 1 1 d . . . H39 H 0.6471 -0.2937 0.5621 0.029 Uiso 1 1 calc R . . C41 C 0.1331(4) 0.2130(4) 0.1697(4) 0.0164(8) Uani 1 1 d . . . C42 C 0.0510(3) 0.2539(3) 0.2736(3) 0.0159(7) Uani 1 1 d . . . H42 H 0.0799 0.1726 0.3491 0.019 Uiso 1 1 calc R . . C43 C -0.0967(4) 0.3017(4) 0.2614(4) 0.0234(8) Uani 1 1 d . . . H43A H -0.1466 0.3216 0.3316 0.035 Uiso 1 1 calc R . . H43B H -0.1118 0.2304 0.2550 0.035 Uiso 1 1 calc R . . H43C H -0.1276 0.3842 0.1899 0.035 Uiso 1 1 calc R . . S1 S 0.74145(9) 0.58887(9) 0.85401(8) 0.01834(17) Uani 1 1 d . . . C1S C 0.8546(4) 0.4381(4) 0.8184(4) 0.0242(8) Uani 1 1 d . . . O1S1 O 0.7941(3) 0.6887(3) 0.7771(2) 0.0236(6) Uani 1 1 d . . . O2S1 O 0.7564(3) 0.5441(3) 0.9795(2) 0.0298(6) Uani 1 1 d . . . O3S1 O 0.6135(3) 0.6150(3) 0.8221(3) 0.0264(6) Uani 1 1 d . . . F1S1 F 0.8622(3) 0.4664(3) 0.7018(2) 0.0347(6) Uani 1 1 d . . . F2S1 F 0.9791(3) 0.3893(3) 0.8525(3) 0.0398(6) Uani 1 1 d . . . F3S1 F 0.8110(3) 0.3396(2) 0.8735(3) 0.0374(6) Uani 1 1 d . . . S2 S 0.98297(10) 0.00829(9) 0.61496(8) 0.02225(19) Uani 1 1 d . . . C2S C 0.9823(5) 0.1453(5) 0.6455(4) 0.0330(9) Uani 1 1 d . . . O1S2 O 0.8874(3) 0.0785(3) 0.5235(3) 0.0320(7) Uani 1 1 d . . . O2S2 O 1.1190(3) -0.0532(4) 0.5738(4) 0.0499(10) Uani 1 1 d . . . O3S2 O 0.9432(5) -0.0727(4) 0.7268(3) 0.0504(10) Uani 1 1 d . . . F1S2 F 1.0653(3) 0.0960(4) 0.7317(3) 0.0502(8) Uani 1 1 d . . . F2S2 F 0.8614(3) 0.2145(3) 0.6832(3) 0.0555(9) Uani 1 1 d . . . F3S2 F 1.0198(5) 0.2301(4) 0.5508(3) 0.0740(13) Uani 1 1 d . . . C1M C 0.3095(5) 0.0427(6) 0.9170(5) 0.0418(11) Uani 1 1 d . . . H1M1 H 0.2172 0.0868 0.8915 0.063 Uiso 1 1 calc R . . H1M2 H 0.3681 -0.0112 0.8689 0.063 Uiso 1 1 calc R . . H1M3 H 0.3389 0.1123 0.9063 0.063 Uiso 1 1 calc R . . O1M O 0.3154(4) -0.0417(3) 1.0360(3) 0.0404(8) Uani 1 1 d . . . H1M H 0.2793 0.0057 1.0783 0.061 Uiso 1 1 calc R . . O1W O 0.7365(3) 0.9248(3) 0.5570(3) 0.0300(7) Uani 1 1 d . . . O2W O 0.1514(3) 0.8808(3) 0.3698(3) 0.0306(7) Uani 1 1 d . . . H1W1 H 0.781(6) 0.965(6) 0.556(5) 0.046 Uiso 1 1 d . . . H1W2 H 0.760(6) 0.853(7) 0.612(6) 0.046 Uiso 1 1 d . . . H2W1 H 0.147(6) 0.955(7) 0.308(6) 0.046 Uiso 1 1 d . . . H2W2 H 0.142(6) 0.905(6) 0.421(6) 0.046 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 Ho1 0.01081(6) 0.00934(5) 0.00959(6) -0.00334(4) -0.00129(4) -0.00349(4) O1 0.0202(13) 0.0161(11) 0.0147(12) -0.0057(10) -0.0001(9) -0.0089(10) O2 0.0238(13) 0.0175(11) 0.0179(13) -0.0074(10) 0.0018(10) -0.0125(10) O3 0.0314(15) 0.0213(13) 0.0303(15) -0.0145(12) 0.0065(12) -0.0157(12) O11 0.0149(12) 0.0140(11) 0.0115(11) -0.0033(9) -0.0007(9) -0.0051(9) O21 0.0159(12) 0.0139(11) 0.0144(12) -0.0060(9) -0.0002(9) -0.0065(9) O31 0.0148(12) 0.0147(11) 0.0177(12) -0.0033(10) -0.0048(9) -0.0057(9) N1 0.0121(14) 0.0158(13) 0.0126(14) -0.0070(11) 0.0003(10) -0.0033(11) N2 0.0096(13) 0.0126(12) 0.0096(13) -0.0021(10) -0.0029(10) -0.0012(10) N3 0.0125(14) 0.0129(12) 0.0144(14) -0.0045(11) -0.0014(10) -0.0048(10) N4 0.0105(13) 0.0166(13) 0.0164(15) -0.0075(11) -0.0017(11) -0.0025(11) N11 0.0147(15) 0.0187(14) 0.0109(14) -0.0039(11) -0.0026(11) -0.0028(11) N22 0.0212(15) 0.0153(13) 0.0137(14) -0.0074(11) 0.0014(11) -0.0080(12) N33 0.0130(14) 0.0144(13) 0.0171(15) -0.0018(11) -0.0047(11) -0.0043(11) C1 0.0179(17) 0.0191(16) 0.0090(15) -0.0040(13) -0.0003(12) -0.0064(13) C2 0.0173(17) 0.0155(15) 0.0100(16) -0.0023(12) -0.0009(12) -0.0069(13) C3 0.0116(18) 0.0098(14) 0.0131(19) -0.0029(14) -0.0009(14) -0.0038(14) C4 0.0131(16) 0.0161(15) 0.0183(17) -0.0069(13) -0.0006(13) -0.0068(13) C5 0.0110(16) 0.0162(15) 0.0206(17) -0.0090(13) 0.0001(12) -0.0044(12) C6 0.0140(16) 0.0158(15) 0.0193(18) -0.0088(13) -0.0021(13) -0.0016(13) C7 0.0150(17) 0.0217(16) 0.0172(17) -0.0111(14) 0.0005(13) -0.0022(13) C8 0.0154(17) 0.0218(16) 0.0143(17) -0.0106(14) 0.0009(13) -0.0040(13) C10 0.0133(16) 0.0160(15) 0.0135(16) -0.0035(13) -0.0037(12) -0.0041(13) C11 0.0132(17) 0.0114(14) 0.0126(17) -0.0020(13) -0.0036(13) -0.0059(13) C12 0.0117(16) 0.0181(16) 0.0164(17) -0.0067(14) 0.0007(13) -0.0038(13) C13 0.0129(18) 0.030(2) 0.034(2) -0.0156(18) -0.0048(16) -0.0001(15) C14 0.0114(16) 0.0120(14) 0.0222(18) -0.0062(13) -0.0031(13) -0.0003(12) C15 0.0166(18) 0.0184(16) 0.0249(19) -0.0117(14) -0.0008(14) -0.0029(13) C16 0.019(2) 0.029(2) 0.038(3) -0.0208(19) -0.0083(17) 0.0000(16) C17 0.021(2) 0.0211(18) 0.057(3) -0.0229(19) -0.0119(19) -0.0009(15) C18 0.0143(19) 0.0143(17) 0.058(3) -0.0093(18) -0.0041(18) -0.0026(15) C19 0.0143(17) 0.0142(15) 0.027(2) -0.0046(14) -0.0017(14) 0.0002(13) C20 0.0176(17) 0.0112(14) 0.0144(16) -0.0049(13) 0.0006(12) -0.0053(12) C21 0.0127(16) 0.0165(15) 0.0142(16) -0.0059(13) -0.0021(12) -0.0050(12) C22 0.0223(18) 0.0182(16) 0.0127(16) -0.0077(13) 0.0021(13) -0.0093(14) C23 0.025(2) 0.0267(19) 0.017(2) -0.0114(16) 0.0038(15) -0.0089(16) C24 0.0212(18) 0.0225(17) 0.0122(17) -0.0088(14) 0.0010(13) -0.0089(14) C25 0.030(2) 0.0218(18) 0.0199(19) -0.0055(15) -0.0017(15) -0.0134(16) C26 0.037(2) 0.0222(19) 0.018(2) -0.0032(16) -0.0050(18) -0.0093(17) C27 0.029(2) 0.028(2) 0.020(2) -0.0079(16) -0.0061(16) -0.0034(16) C28 0.027(2) 0.033(2) 0.022(2) -0.0102(17) -0.0002(16) -0.0128(17) C29 0.027(2) 0.0234(17) 0.0162(18) -0.0071(14) 0.0018(14) -0.0132(15) C30 0.0191(17) 0.0146(15) 0.0134(16) -0.0029(13) -0.0061(13) -0.0063(13) C31 0.0154(18) 0.0151(15) 0.0128(17) -0.0060(13) 0.0020(14) -0.0067(14) C32 0.0155(17) 0.0172(16) 0.0210(18) -0.0040(14) -0.0020(13) -0.0087(13) C33 0.024(2) 0.0213(17) 0.0184(19) -0.0015(14) 0.0031(15) -0.0120(15) C34 0.0224(19) 0.0181(16) 0.0202(18) -0.0031(14) -0.0009(14) -0.0123(14) C35 0.025(2) 0.0288(19) 0.0207(19) -0.0043(15) -0.0017(15) -0.0174(16) C36 0.040(2) 0.035(2) 0.028(2) -0.0120(18) -0.0035(18) -0.024(2) C37 0.043(3) 0.030(2) 0.034(2) -0.0172(19) 0.0083(19) -0.0234(19) C38 0.037(2) 0.0181(18) 0.034(2) -0.0063(17) -0.0051(18) -0.0083(17) C39 0.030(2) 0.0166(17) 0.022(2) -0.0023(15) -0.0057(16) -0.0081(15) C41 0.014(2) 0.0180(17) 0.019(2) -0.0092(15) -0.0004(15) -0.0059(15) C42 0.0179(17) 0.0144(15) 0.0160(17) -0.0034(13) -0.0017(13) -0.0088(13) C43 0.0188(19) 0.0250(18) 0.028(2) -0.0117(16) -0.0010(15) -0.0083(15) S1 0.0191(4) 0.0185(4) 0.0152(4) -0.0032(3) -0.0010(3) -0.0086(3) C1S 0.0207(19) 0.0206(17) 0.030(2) -0.0061(16) -0.0021(15) -0.0097(15) O1S1 0.0315(15) 0.0231(13) 0.0164(13) -0.0040(11) -0.0005(11) -0.0149(12) O2S1 0.0395(17) 0.0334(15) 0.0168(14) -0.0050(12) -0.0003(12) -0.0197(14) O3S1 0.0197(14) 0.0303(14) 0.0247(15) -0.0065(12) -0.0023(11) -0.0097(11) F1S1 0.0407(15) 0.0370(13) 0.0308(14) -0.0189(11) 0.0065(11) -0.0173(12) F2S1 0.0233(13) 0.0321(13) 0.0549(18) -0.0136(13) -0.0092(12) -0.0034(10) F3S1 0.0425(16) 0.0229(12) 0.0479(16) -0.0102(11) 0.0022(12) -0.0188(11) S2 0.0261(5) 0.0213(4) 0.0195(5) -0.0067(4) -0.0024(4) -0.0101(4) C2S 0.045(3) 0.039(2) 0.029(2) -0.0153(19) 0.0026(19) -0.028(2) O1S2 0.0362(17) 0.0296(15) 0.0323(17) -0.0064(13) -0.0088(13) -0.0165(13) O2S2 0.0250(17) 0.078(3) 0.061(2) -0.052(2) -0.0022(16) -0.0089(17) O3S2 0.096(3) 0.044(2) 0.0234(17) -0.0064(15) 0.0049(18) -0.048(2) F1S2 0.062(2) 0.071(2) 0.0389(17) -0.0290(16) -0.0056(14) -0.0352(17) F2S2 0.057(2) 0.0421(17) 0.076(2) -0.0390(17) -0.0032(17) -0.0121(15) F3S2 0.157(4) 0.088(3) 0.0284(16) -0.0154(17) 0.013(2) -0.105(3) C1M 0.040(3) 0.048(3) 0.038(3) -0.017(2) 0.001(2) -0.019(2) O1M 0.042(2) 0.0301(16) 0.0385(19) -0.0154(14) 0.0125(15) -0.0101(14) O1W 0.0300(16) 0.0212(14) 0.0362(18) 0.0039(12) -0.0195(13) -0.0135(13) O2W 0.051(2) 0.0188(14) 0.0260(16) -0.0106(12) 0.0006(14) -0.0168(14) _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 Ho1 O21 2.308(2) . ? Ho1 O31 2.313(3) . ? Ho1 O1 2.317(2) . ? Ho1 O11 2.359(2) . ? Ho1 O2 2.469(3) . ? Ho1 N4 2.544(3) . ? Ho1 N1 2.578(3) . ? Ho1 N2 2.595(3) . ? Ho1 N3 2.653(3) . ? O1 C41 1.280(5) . ? O2 C42 1.441(4) . ? O3 C41 1.247(5) . ? O11 C11 1.260(4) . ? O21 C21 1.256(4) . ? O31 C31 1.255(4) . ? N1 C10 1.479(4) . ? N1 C8 1.493(4) . ? N1 C1 1.500(4) . ? N2 C20 1.482(4) . ? N2 C2 1.487(4) . ? N2 C3 1.496(5) . ? N3 C30 1.479(4) . ? N3 C4 1.486(4) . ? N3 C5 1.498(4) . ? N4 C6 1.483(4) . ? N4 C7 1.483(5) . ? N11 C11 1.310(5) . ? N11 C12 1.467(4) . ? N22 C21 1.314(4) . ? N22 C22 1.467(4) . ? N33 C31 1.319(5) . ? N33 C32 1.481(4) . ? C1 C2 1.520(4) . ? C3 C4 1.525(5) . ? C5 C6 1.520(4) . ? C7 C8 1.522(5) . ? C10 C11 1.504(5) . ? C12 C14 1.521(5) . ? C12 C13 1.522(5) . ? C14 C19 1.398(5) . ? C14 C15 1.398(5) . ? C15 C16 1.392(5) . ? C16 C17 1.393(7) . ? C17 C18 1.378(7) . ? C18 C19 1.396(6) . ? C20 C21 1.522(5) . ? C22 C24 1.523(5) . ? C22 C23 1.535(5) . ? C24 C25 1.398(5) . ? C24 C29 1.402(5) . ? C25 C26 1.384(6) . ? C26 C27 1.386(6) . ? C27 C28 1.392(6) . ? C28 C29 1.387(6) . ? C30 C31 1.533(5) . ? C32 C34 1.521(5) . ? C32 C33 1.521(5) . ? C34 C39 1.384(5) . ? C34 C35 1.399(5) . ? C35 C36 1.381(6) . ? C36 C37 1.381(7) . ? C37 C38 1.389(6) . ? C38 C39 1.388(6) . ? C41 C42 1.529(5) . ? C42 C43 1.512(5) . ? S1 O2S1 1.439(3) . ? S1 O3S1 1.441(3) . ? S1 O1S1 1.455(3) . ? S1 C1S 1.833(4) . ? C1S F1S1 1.332(5) . ? C1S F2S1 1.338(5) . ? C1S F3S1 1.339(4) . ? S2 O3S2 1.429(3) . ? S2 O1S2 1.437(3) . ? S2 O2S2 1.440(4) . ? S2 C2S 1.827(4) . ? C2S F3S2 1.322(5) . ? C2S F2S2 1.325(6) . ? C2S F1S2 1.334(5) . ? C1M O1M 1.387(6) . ? 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 O21 Ho1 O31 82.62(9) . . ? O21 Ho1 O1 136.50(8) . . ? O31 Ho1 O1 80.01(9) . . ? O21 Ho1 O11 82.34(9) . . ? O31 Ho1 O11 139.96(8) . . ? O1 Ho1 O11 85.94(9) . . ? O21 Ho1 O2 70.26(8) . . ? O31 Ho1 O2 71.98(9) . . ? O1 Ho1 O2 66.50(8) . . ? O11 Ho1 O2 68.03(9) . . ? O21 Ho1 N4 140.98(9) . . ? O31 Ho1 N4 76.01(9) . . ? O1 Ho1 N4 71.20(9) . . ? O11 Ho1 N4 133.74(9) . . ? O2 Ho1 N4 130.21(9) . . ? O21 Ho1 N1 133.81(9) . . ? O31 Ho1 N1 142.23(9) . . ? O1 Ho1 N1 77.20(9) . . ? O11 Ho1 N1 67.63(9) . . ? O2 Ho1 N1 123.52(9) . . ? N4 Ho1 N1 68.33(9) . . ? O21 Ho1 N2 67.93(9) . . ? O31 Ho1 N2 132.60(8) . . ? O1 Ho1 N2 146.09(9) . . ? O11 Ho1 N2 73.38(8) . . ? O2 Ho1 N2 125.65(8) . . ? N4 Ho1 N2 104.11(9) . . ? N1 Ho1 N2 70.23(9) . . ? O21 Ho1 N3 73.57(9) . . ? O31 Ho1 N3 67.09(9) . . ? O1 Ho1 N3 132.36(9) . . ? O11 Ho1 N3 140.99(8) . . ? O2 Ho1 N3 127.78(9) . . ? N4 Ho1 N3 68.14(9) . . ? N1 Ho1 N3 108.70(9) . . ? N2 Ho1 N3 69.32(9) . . ? C41 O1 Ho1 120.9(2) . . ? C42 O2 Ho1 117.3(2) . . ? C11 O11 Ho1 121.3(2) . . ? C21 O21 Ho1 123.8(2) . . ? C31 O31 Ho1 125.1(2) . . ? C10 N1 C8 108.4(3) . . ? C10 N1 C1 111.1(3) . . ? C8 N1 C1 109.0(3) . . ? C10 N1 Ho1 106.7(2) . . ? C8 N1 Ho1 110.9(2) . . ? C1 N1 Ho1 110.70(19) . . ? C20 N2 C2 110.0(2) . . ? C20 N2 C3 109.8(3) . . ? C2 N2 C3 108.6(3) . . ? C20 N2 Ho1 107.05(19) . . ? C2 N2 Ho1 110.77(19) . . ? C3 N2 Ho1 110.65(19) . . ? C30 N3 C4 111.0(3) . . ? C30 N3 C5 110.2(3) . . ? C4 N3 C5 108.6(3) . . ? C30 N3 Ho1 106.55(19) . . ? C4 N3 Ho1 110.32(19) . . ? C5 N3 Ho1 110.18(19) . . ? C6 N4 C7 112.0(3) . . ? C6 N4 Ho1 113.9(2) . . ? C7 N4 Ho1 115.6(2) . . ? C11 N11 C12 124.1(3) . . ? C21 N22 C22 121.0(3) . . ? C31 N33 C32 122.7(3) . . ? N1 C1 C2 113.2(3) . . ? N2 C2 C1 112.2(3) . . ? N2 C3 C4 113.4(3) . . ? N3 C4 C3 111.0(3) . . ? N3 C5 C6 112.2(3) . . ? N4 C6 C5 108.8(3) . . ? N4 C7 C8 109.4(3) . . ? N1 C8 C7 111.4(3) . . ? N1 C10 C11 110.8(3) . . ? O11 C11 N11 122.2(3) . . ? O11 C11 C10 120.2(3) . . ? N11 C11 C10 117.5(3) . . ? N11 C12 C14 110.5(3) . . ? N11 C12 C13 108.4(3) . . ? C14 C12 C13 112.8(3) . . ? C19 C14 C15 119.9(3) . . ? C19 C14 C12 120.2(3) . . ? C15 C14 C12 119.9(3) . . ? C16 C15 C14 119.6(4) . . ? C15 C16 C17 120.3(4) . . ? C18 C17 C16 120.1(4) . . ? C17 C18 C19 120.4(4) . . ? C18 C19 C14 119.7(4) . . ? N2 C20 C21 111.2(3) . . ? O21 C21 N22 121.7(3) . . ? O21 C21 C20 119.6(3) . . ? N22 C21 C20 118.6(3) . . ? N22 C22 C24 110.6(3) . . ? N22 C22 C23 108.7(3) . . ? C24 C22 C23 111.8(3) . . ? C25 C24 C29 118.4(3) . . ? C25 C24 C22 120.5(3) . . ? C29 C24 C22 121.1(3) . . ? C26 C25 C24 120.9(4) . . ? C25 C26 C27 120.0(4) . . ? C26 C27 C28 120.2(4) . . ? C29 C28 C27 119.7(4) . . ? C28 C29 C24 120.8(4) . . ? N3 C30 C31 111.7(3) . . ? O31 C31 N33 122.8(3) . . ? O31 C31 C30 119.4(3) . . ? N33 C31 C30 117.7(3) . . ? N33 C32 C34 110.3(3) . . ? N33 C32 C33 108.6(3) . . ? C34 C32 C33 114.8(3) . . ? C39 C34 C35 119.1(4) . . ? C39 C34 C32 122.1(3) . . ? C35 C34 C32 118.8(3) . . ? C36 C35 C34 120.5(4) . . ? C35 C36 C37 119.9(4) . . ? C36 C37 C38 120.1(4) . . ? C39 C38 C37 119.9(4) . . ? C34 C39 C38 120.4(4) . . ? O3 C41 O1 125.2(4) . . ? O3 C41 C42 117.0(3) . . ? O1 C41 C42 117.8(3) . . ? O2 C42 C43 111.3(3) . . ? O2 C42 C41 109.0(3) . . ? C43 C42 C41 111.0(3) . . ? O2S1 S1 O3S1 114.98(18) . . ? O2S1 S1 O1S1 115.43(17) . . ? O3S1 S1 O1S1 115.00(17) . . ? O2S1 S1 C1S 103.74(19) . . ? O3S1 S1 C1S 102.32(18) . . ? O1S1 S1 C1S 102.75(17) . . ? F1S1 C1S F2S1 107.3(3) . . ? F1S1 C1S F3S1 108.2(3) . . ? F2S1 C1S F3S1 108.1(3) . . ? F1S1 C1S S1 111.3(3) . . ? F2S1 C1S S1 111.6(3) . . ? F3S1 C1S S1 110.2(3) . . ? O3S2 S2 O1S2 114.7(2) . . ? O3S2 S2 O2S2 116.2(3) . . ? O1S2 S2 O2S2 113.5(2) . . ? O3S2 S2 C2S 103.7(2) . . ? O1S2 S2 C2S 103.6(2) . . ? O2S2 S2 C2S 102.8(2) . . ? F3S2 C2S F2S2 109.0(4) . . ? F3S2 C2S F1S2 107.4(4) . . ? F2S2 C2S F1S2 106.5(4) . . ? F3S2 C2S S2 112.2(3) . . ? F2S2 C2S S2 110.5(3) . . ? F1S2 C2S S2 111.1(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.841 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.109 data_01srv045 _database_code_CSD 172450 _publ_requested_journal 'test' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H56 N7 O6 Yb, 2(C F3 O3 S), C H4 O, 2(H2 O)' _chemical_formula_sum 'C44 H64 F6 N7 O15 S2 Yb' _chemical_formula_weight 1282.18 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.287(2) _cell_length_b 11.9208(19) _cell_length_c 12.407(3) _cell_angle_alpha 64.712(16) _cell_angle_beta 77.152(15) _cell_angle_gamma 62.720(10) _cell_volume 1340.8(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6075 _cell_measurement_theta_min 5.543 _cell_measurement_theta_max 54.969 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas Not_measured _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 653 _exptl_absorpt_coefficient_mu 1.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.52009 _exptl_absorpt_correction_T_max 0.60319 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (10s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _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 SMART CCD 1K area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 15088 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11065 _reflns_number_gt 11036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SMART-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0392P)^2^+2.3228P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.018(5) _refine_ls_number_reflns 11065 _refine_ls_number_parameters 689 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _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 0.257680(6) 0.412270(6) 0.142060(6) 0.01058(5) Uani 1 1 d . . . N1 N 0.2371(4) 0.5341(4) -0.0838(3) 0.0153(8) Uani 1 1 d . . . N2 N 0.2848(4) 0.6355(4) 0.0765(3) 0.0131(7) Uani 1 1 d . . . N3 N 0.4935(4) 0.3602(4) 0.1996(3) 0.0148(8) Uani 1 1 d . . . N4 N 0.4451(4) 0.2753(4) 0.0332(3) 0.0164(8) Uani 1 1 d . . . N10 N 0.1717(4) 0.6362(4) 0.3759(3) 0.0167(8) Uani 1 1 d . . . H10N H 0.1587 0.7192 0.3640 0.020 Uiso 1 1 calc R . . N20 N -0.1135(4) 0.7410(4) -0.0444(3) 0.0190(8) Uani 1 1 d . . . H20N H -0.1353 0.7753 -0.1192 0.023 Uiso 1 1 calc R . . N30 N 0.4958(4) 0.0426(4) 0.4347(3) 0.0176(8) Uani 1 1 d . . . H30N H 0.5679 0.0178 0.4704 0.021 Uiso 1 1 calc R . . O10 O 0.0469(3) 0.5907(3) 0.0899(3) 0.0145(6) Uani 1 1 d . . . O20 O 0.2207(3) 0.4801(3) 0.2968(3) 0.0158(6) Uani 1 1 d . . . O30 O 0.3536(3) 0.2014(3) 0.2860(3) 0.0172(7) Uani 1 1 d . . . C1 C 0.2828(5) 0.6468(5) -0.1285(4) 0.0170(9) Uani 1 1 d . . . H1A H 0.2472 0.7105 -0.2086 0.020 Uiso 1 1 calc R . . H1B H 0.3814 0.6077 -0.1367 0.020 Uiso 1 1 calc R . . C2 C 0.2387(5) 0.7264(5) -0.0468(4) 0.0157(9) Uani 1 1 d . . . H2A H 0.2753 0.7962 -0.0793 0.019 Uiso 1 1 calc R . . H2B H 0.1402 0.7738 -0.0450 0.019 Uiso 1 1 calc R . . C3 C 0.4290(5) 0.6061(5) 0.0796(5) 0.0141(10) Uani 1 1 d . . . H3A H 0.4348 0.6883 0.0754 0.017 Uiso 1 1 calc R . . H3B H 0.4775 0.5856 0.0087 0.017 Uiso 1 1 calc R . . C4 C 0.4964(5) 0.4870(5) 0.1915(4) 0.0161(9) Uani 1 1 d . . . H4A H 0.5901 0.4733 0.1899 0.019 Uiso 1 1 calc R . . H4B H 0.4501 0.5079 0.2627 0.019 Uiso 1 1 calc R . . C5 C 0.6010(5) 0.3033(5) 0.1181(4) 0.0182(9) Uani 1 1 d . . . H5A H 0.6881 0.2558 0.1565 0.022 Uiso 1 1 calc R . . H5B H 0.6052 0.3789 0.0434 0.022 Uiso 1 1 calc R . . C6 C 0.5766(5) 0.2043(5) 0.0886(4) 0.0179(9) Uani 1 1 d . . . H6A H 0.6478 0.1705 0.0329 0.021 Uiso 1 1 calc R . . H6B H 0.5780 0.1252 0.1623 0.021 Uiso 1 1 calc R . . C7 C 0.4549(5) 0.3471(5) -0.0980(4) 0.0211(10) Uani 1 1 d . . . H7A H 0.5029 0.2798 -0.1366 0.025 Uiso 1 1 calc R . . H7B H 0.5054 0.4029 -0.1162 0.025 Uiso 1 1 calc R . . C8 C 0.3158(5) 0.4376(5) -0.1459(4) 0.0168(9) Uani 1 1 d . . . H8A H 0.3221 0.4898 -0.2324 0.020 Uiso 1 1 calc R . . H8B H 0.2692 0.3803 -0.1350 0.020 Uiso 1 1 calc R . . H9A H 0.0803 0.1729 0.3491 0.020 Uiso 1 1 d R . . C10 C 0.0937(4) 0.5908(5) -0.1077(4) 0.0167(9) Uani 1 1 d . . . H10A H 0.0736 0.5190 -0.1094 0.020 Uiso 1 1 calc R . . H10B H 0.0746 0.6659 -0.1869 0.020 Uiso 1 1 calc R . . C11 C 0.0056(5) 0.6433(5) -0.0141(4) 0.0142(9) Uani 1 1 d . . . C12 C -0.2132(5) 0.7969(5) 0.0398(4) 0.0173(9) Uani 1 1 d . . . H12A H -0.2261 0.7200 0.1096 0.021 Uiso 1 1 calc R . . C13 C -0.3448(5) 0.8916(6) -0.0243(5) 0.0272(12) Uani 1 1 d . . . H13A H -0.3712 0.8411 -0.0522 0.041 Uiso 1 1 calc R . . H13B H -0.3336 0.9679 -0.0926 0.041 Uiso 1 1 calc R . . H13C H -0.4139 0.9266 0.0309 0.041 Uiso 1 1 calc R . . C14 C -0.1656(5) 0.8693(5) 0.0846(4) 0.0172(9) Uani 1 1 d . . . C15 C -0.1809(5) 0.8496(5) 0.2046(5) 0.0232(10) Uani 1 1 d . . . H15A H -0.2195 0.7893 0.2588 0.028 Uiso 1 1 calc R . . C16 C -0.1400(5) 0.9180(6) 0.2462(6) 0.0286(12) Uani 1 1 d . . . H16A H -0.1506 0.9045 0.3283 0.034 Uiso 1 1 calc R . . C17 C -0.0838(5) 1.0056(6) 0.1661(6) 0.0326(13) Uani 1 1 d . . . H17A H -0.0561 1.0527 0.1938 0.039 Uiso 1 1 calc R . . C18 C -0.0674(5) 1.0254(5) 0.0462(6) 0.0310(13) Uani 1 1 d . . . H18A H -0.0272 1.0844 -0.0076 0.037 Uiso 1 1 calc R . . C19 C -0.1099(5) 0.9585(5) 0.0050(5) 0.0247(11) Uani 1 1 d . . . H19A H -0.1009 0.9736 -0.0775 0.030 Uiso 1 1 calc R . . C20 C 0.2025(5) 0.7034(5) 0.1605(4) 0.0161(9) Uani 1 1 d . . . H20B H 0.1103 0.7612 0.1320 0.019 Uiso 1 1 calc R . . H20C H 0.2397 0.7628 0.1634 0.019 Uiso 1 1 calc R . . C21 C 0.2004(4) 0.5985(5) 0.2841(4) 0.0145(9) Uani 1 1 d . . . C22 C 0.1611(5) 0.5407(5) 0.4983(4) 0.0178(9) Uani 1 1 d . . . H22A H 0.1081 0.4937 0.4962 0.021 Uiso 1 1 calc R . . C23 C 0.0854(6) 0.6216(6) 0.5783(5) 0.0255(11) Uani 1 1 d . . . H23A H -0.0020 0.6895 0.5453 0.038 Uiso 1 1 calc R . . H23B H 0.1363 0.6677 0.5824 0.038 Uiso 1 1 calc R . . H23C H 0.0733 0.5595 0.6586 0.038 Uiso 1 1 calc R . . C24 C 0.2977(5) 0.4335(5) 0.5442(4) 0.0205(10) Uani 1 1 d . . . C25 C 0.3202(6) 0.2962(5) 0.6000(4) 0.0238(11) Uani 1 1 d . . . H25A H 0.2496 0.2700 0.6093 0.029 Uiso 1 1 calc R . . C26 C 0.4467(6) 0.1967(6) 0.6425(5) 0.0280(12) Uani 1 1 d . . . H26A H 0.4613 0.1035 0.6797 0.034 Uiso 1 1 calc R . . C27 C 0.5501(6) 0.2332(6) 0.6305(5) 0.0287(12) Uani 1 1 d . . . H27A H 0.6355 0.1658 0.6597 0.034 Uiso 1 1 calc R . . C28 C 0.5279(6) 0.3697(6) 0.5751(5) 0.0284(12) Uani 1 1 d . . . H28A H 0.5987 0.3953 0.5666 0.034 Uiso 1 1 calc R . . C29 C 0.4035(5) 0.4693(5) 0.5318(4) 0.0222(10) Uani 1 1 d . . . H29A H 0.3901 0.5621 0.4937 0.027 Uiso 1 1 calc R . . C30 C 0.5143(5) 0.2594(5) 0.3232(4) 0.0161(9) Uani 1 1 d . . . H30B H 0.4747 0.3072 0.3795 0.019 Uiso 1 1 calc R . . H30C H 0.6111 0.2067 0.3371 0.019 Uiso 1 1 calc R . . C31 C 0.4510(5) 0.1632(4) 0.3461(4) 0.0131(9) Uani 1 1 d . . . C32 C 0.4301(5) -0.0522(5) 0.4761(4) 0.0217(10) Uani 1 1 d . . . H32A H 0.3397 -0.0001 0.4413 0.026 Uiso 1 1 calc R . . C33 C 0.4109(5) -0.0974(5) 0.6114(4) 0.0248(11) Uani 1 1 d . . . H33A H 0.3616 -0.0170 0.6329 0.037 Uiso 1 1 calc R . . H33B H 0.4982 -0.1502 0.6481 0.037 Uiso 1 1 calc R . . H33C H 0.3604 -0.1539 0.6402 0.037 Uiso 1 1 calc R . . C34 C 0.5075(5) -0.1664(5) 0.4302(4) 0.0220(10) Uani 1 1 d . . . C35 C 0.4688(6) -0.1550(6) 0.3256(5) 0.0276(12) Uani 1 1 d . . . H35A H 0.3963 -0.0747 0.2836 0.033 Uiso 1 1 calc R . . C36 C 0.5336(7) -0.2579(6) 0.2815(5) 0.0328(13) Uani 1 1 d . . . H36D H 0.5059 -0.2482 0.2099 0.039 Uiso 1 1 calc R . . C37 C 0.6394(7) -0.3757(6) 0.3428(5) 0.0344(14) Uani 1 1 d . . . H37A H 0.6835 -0.4476 0.3140 0.041 Uiso 1 1 calc R . . C38 C 0.6808(6) -0.3880(6) 0.4471(5) 0.0321(13) Uani 1 1 d . . . H38A H 0.7544 -0.4676 0.4879 0.039 Uiso 1 1 calc R . . C39 C 0.6155(6) -0.2853(5) 0.4911(5) 0.0265(11) Uani 1 1 d . . . H39A H 0.6434 -0.2951 0.5626 0.032 Uiso 1 1 calc R . . O1L O 0.1843(3) 0.2928(3) 0.0913(3) 0.0164(7) Uani 1 1 d . . . O2L O 0.1412(4) 0.1077(4) 0.1655(3) 0.0273(8) Uani 1 1 d . . . O3L O 0.0797(3) 0.3579(3) 0.2782(3) 0.0176(7) Uani 1 1 d . . . C1L C 0.1311(5) 0.2140(6) 0.1686(5) 0.0168(11) Uani 1 1 d . . . C2L C 0.0515(5) 0.2545(5) 0.2733(4) 0.0175(9) Uani 1 1 d . . . C3L C -0.0977(5) 0.3043(6) 0.2611(5) 0.0267(11) Uani 1 1 d . . . H3LA H -0.1467 0.3285 0.3294 0.040 Uiso 1 1 calc R . . H3LB H -0.1151 0.2320 0.2589 0.040 Uiso 1 1 calc R . . H3LC H -0.1273 0.3846 0.1873 0.040 Uiso 1 1 calc R . . S1 S 0.73831(13) 0.58854(12) 0.85199(10) 0.0198(2) Uani 1 1 d . . . O1A O 0.7526(4) 0.5438(4) 0.9783(3) 0.0310(9) Uani 1 1 d . . . O1B O 0.7925(4) 0.6873(4) 0.7761(3) 0.0248(8) Uani 1 1 d . . . O1C O 0.6102(4) 0.6160(4) 0.8194(3) 0.0278(8) Uani 1 1 d . . . C1S C 0.9807(7) 0.1434(6) 0.6437(5) 0.0341(13) Uani 1 1 d . . . F1A F 0.9747(3) 0.3873(4) 0.8520(4) 0.0436(9) Uani 1 1 d . . . F1B F 0.8592(4) 0.4658(4) 0.7000(3) 0.0371(8) Uani 1 1 d . . . F1C F 0.8067(4) 0.3391(3) 0.8709(3) 0.0391(8) Uani 1 1 d . . . S2 S 0.98004(14) 0.00608(13) 0.61404(11) 0.0243(3) Uani 1 1 d . . . O2A O 1.1156(4) -0.0566(6) 0.5738(5) 0.0521(14) Uani 1 1 d . . . O2B O 0.9396(6) -0.0741(5) 0.7257(4) 0.0512(13) Uani 1 1 d . . . O2C O 0.8847(4) 0.0776(4) 0.5212(4) 0.0323(9) Uani 1 1 d . . . C2S C 0.8506(5) 0.4367(5) 0.8172(5) 0.0264(11) Uani 1 1 d . . . F2A F 1.0627(5) 0.0926(5) 0.7321(4) 0.0528(11) Uani 1 1 d . . . F2B F 1.0192(7) 0.2277(6) 0.5501(4) 0.0776(18) Uani 1 1 d . . . F2C F 0.8597(5) 0.2129(5) 0.6817(5) 0.0604(12) Uani 1 1 d . . . O1M O 0.3137(5) -0.0420(4) 1.0364(4) 0.0409(11) Uani 1 1 d . . . H1M H 0.2780 0.0065 1.0776 0.049 Uiso 1 1 calc R . . C1M C 0.3091(7) 0.0420(7) 0.9149(5) 0.0390(14) Uani 1 1 d . . . H1M1 H 0.2159 0.0977 0.8918 0.058 Uiso 1 1 calc R . . H1M2 H 0.3550 -0.0146 0.8671 0.058 Uiso 1 1 calc R . . H1M3 H 0.3531 0.1015 0.9011 0.058 Uiso 1 1 calc R . . O1W O 0.7323(4) 0.9246(4) 0.5558(4) 0.0304(9) Uani 1 1 d D . . H1W1 H 0.756(7) 0.856(5) 0.621(4) 0.036 Uiso 1 1 d D . . H1W2 H 0.773(6) 0.972(6) 0.550(6) 0.036 Uiso 1 1 d D . . O2W O 0.1479(5) 0.8817(4) 0.3679(4) 0.0346(10) Uani 1 1 d D . . H2W1 H 0.122(7) 0.961(4) 0.315(5) 0.042 Uiso 1 1 d D . . H2W2 H 0.185(7) 0.929(7) 0.315(5) 0.042 Uiso 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 0.01145(8) 0.00963(7) 0.01027(7) -0.00388(5) -0.00126(5) -0.00350(5) N1 0.0131(19) 0.0165(19) 0.0160(18) -0.0072(15) -0.0028(14) -0.0038(15) N2 0.0162(19) 0.0122(17) 0.0121(17) -0.0055(14) -0.0011(14) -0.0058(15) N3 0.0172(19) 0.0149(18) 0.0122(17) -0.0052(15) 0.0001(14) -0.0065(16) N4 0.0120(18) 0.0182(19) 0.0167(18) -0.0084(16) -0.0027(15) -0.0017(16) N10 0.021(2) 0.0158(19) 0.0144(18) -0.0072(15) 0.0014(15) -0.0082(16) N20 0.019(2) 0.022(2) 0.0137(18) -0.0069(16) -0.0024(15) -0.0055(17) N30 0.0150(19) 0.0159(19) 0.0195(19) -0.0022(16) -0.0049(15) -0.0065(16) O10 0.0159(16) 0.0148(15) 0.0125(14) -0.0059(12) -0.0002(12) -0.0055(13) O20 0.0183(17) 0.0191(16) 0.0121(14) -0.0059(13) 0.0009(12) -0.0099(14) O30 0.0201(17) 0.0151(16) 0.0160(15) -0.0037(13) -0.0037(13) -0.0074(13) C1 0.016(2) 0.020(2) 0.0111(19) -0.0049(17) 0.0018(16) -0.0065(19) C2 0.019(2) 0.016(2) 0.013(2) -0.0002(17) -0.0033(17) -0.0108(19) C3 0.016(3) 0.011(2) 0.014(3) -0.004(2) 0.0005(19) -0.005(2) C4 0.016(2) 0.019(2) 0.016(2) -0.0061(18) 0.0000(17) -0.0092(19) C5 0.011(2) 0.021(2) 0.022(2) -0.0138(19) -0.0003(17) -0.0012(18) C6 0.013(2) 0.016(2) 0.023(2) -0.0086(19) -0.0042(18) -0.0017(18) C7 0.019(2) 0.023(2) 0.020(2) -0.011(2) -0.0013(19) -0.004(2) C8 0.016(2) 0.018(2) 0.014(2) -0.0087(18) 0.0005(17) -0.0023(18) C10 0.010(2) 0.020(2) 0.017(2) -0.0048(18) -0.0036(17) -0.0050(18) C11 0.016(2) 0.012(2) 0.015(2) -0.0033(18) 0.0000(18) -0.0083(19) C12 0.012(2) 0.017(2) 0.017(2) -0.0056(18) 0.0007(17) -0.0016(18) C13 0.017(3) 0.031(3) 0.031(3) -0.017(2) -0.004(2) -0.001(2) C14 0.015(2) 0.012(2) 0.020(2) -0.0062(18) -0.0023(18) -0.0013(18) C15 0.018(2) 0.022(2) 0.027(2) -0.011(2) -0.0023(19) -0.004(2) C16 0.018(3) 0.028(3) 0.038(3) -0.019(3) -0.008(2) 0.002(2) C17 0.018(3) 0.026(3) 0.062(4) -0.028(3) -0.009(3) -0.002(2) C18 0.013(2) 0.015(2) 0.059(4) -0.011(3) -0.003(2) -0.003(2) C19 0.015(2) 0.021(2) 0.030(3) -0.009(2) 0.001(2) -0.003(2) C20 0.016(2) 0.017(2) 0.013(2) -0.0053(17) 0.0018(17) -0.0060(18) C21 0.011(2) 0.018(2) 0.016(2) -0.0076(18) -0.0006(16) -0.0058(18) C22 0.021(2) 0.020(2) 0.014(2) -0.0068(18) 0.0016(18) -0.010(2) C23 0.030(3) 0.030(3) 0.019(3) -0.014(2) 0.006(2) -0.012(2) C24 0.028(3) 0.025(3) 0.013(2) -0.0108(19) 0.0028(19) -0.012(2) C25 0.027(3) 0.025(3) 0.020(2) -0.007(2) 0.001(2) -0.014(2) C26 0.040(3) 0.023(3) 0.016(2) -0.006(2) 0.000(2) -0.010(2) C27 0.027(3) 0.032(3) 0.022(3) -0.012(2) -0.003(2) -0.005(2) C28 0.024(3) 0.038(3) 0.022(2) -0.012(2) 0.000(2) -0.011(2) C29 0.026(3) 0.024(3) 0.019(2) -0.008(2) -0.0002(19) -0.012(2) C30 0.015(2) 0.014(2) 0.016(2) -0.0037(18) -0.0047(17) -0.0029(18) C31 0.013(2) 0.010(2) 0.012(2) -0.0055(17) 0.0001(18) -0.0010(18) C32 0.024(3) 0.018(2) 0.023(2) -0.0012(19) -0.0037(19) -0.013(2) C33 0.026(3) 0.020(2) 0.020(2) -0.002(2) 0.001(2) -0.009(2) C34 0.025(3) 0.021(2) 0.023(2) -0.002(2) -0.001(2) -0.018(2) C35 0.029(3) 0.031(3) 0.026(3) -0.003(2) -0.004(2) -0.020(2) C36 0.044(4) 0.043(3) 0.027(3) -0.013(3) 0.002(2) -0.032(3) C37 0.050(4) 0.031(3) 0.036(3) -0.021(3) 0.013(3) -0.027(3) C38 0.034(3) 0.024(3) 0.036(3) -0.009(2) -0.002(2) -0.012(2) C39 0.032(3) 0.022(3) 0.025(3) -0.004(2) -0.006(2) -0.012(2) O1L 0.0187(17) 0.0145(15) 0.0153(15) -0.0056(13) -0.0011(13) -0.0059(13) O2L 0.037(2) 0.0238(19) 0.0290(19) -0.0140(16) 0.0069(16) -0.0191(17) O3L 0.0212(17) 0.0181(16) 0.0158(15) -0.0056(13) 0.0012(13) -0.0114(14) C1L 0.014(3) 0.019(2) 0.016(3) -0.008(2) 0.000(2) -0.004(2) C2L 0.017(2) 0.015(2) 0.018(2) -0.0031(19) 0.0020(18) -0.0090(19) C3L 0.021(3) 0.031(3) 0.033(3) -0.014(2) -0.001(2) -0.012(2) S1 0.0221(6) 0.0204(6) 0.0154(5) -0.0038(4) -0.0013(4) -0.0100(5) O1A 0.040(2) 0.036(2) 0.0196(18) -0.0055(16) -0.0036(16) -0.0214(19) O1B 0.034(2) 0.0225(18) 0.0177(16) -0.0035(14) -0.0004(15) -0.0156(16) O1C 0.0225(19) 0.029(2) 0.0265(19) -0.0066(16) 0.0002(15) -0.0106(16) C1S 0.054(4) 0.031(3) 0.028(3) -0.010(2) -0.002(3) -0.026(3) F1A 0.0216(17) 0.035(2) 0.066(3) -0.0167(18) -0.0076(17) -0.0046(15) F1B 0.043(2) 0.041(2) 0.0351(18) -0.0245(16) 0.0100(15) -0.0193(17) F1C 0.044(2) 0.0220(16) 0.050(2) -0.0101(15) 0.0033(17) -0.0177(16) S2 0.0273(7) 0.0228(6) 0.0230(6) -0.0084(5) -0.0025(5) -0.0099(5) O2A 0.026(2) 0.081(4) 0.065(3) -0.053(3) -0.002(2) -0.010(2) O2B 0.096(4) 0.041(3) 0.028(2) -0.007(2) 0.004(2) -0.045(3) O2C 0.037(2) 0.031(2) 0.032(2) -0.0074(17) -0.0088(17) -0.0166(18) C2S 0.017(2) 0.025(3) 0.036(3) -0.009(2) -0.002(2) -0.009(2) F2A 0.068(3) 0.069(3) 0.045(2) -0.028(2) -0.008(2) -0.038(2) F2B 0.163(6) 0.096(4) 0.031(2) -0.018(2) 0.016(3) -0.113(4) F2C 0.061(3) 0.051(3) 0.084(3) -0.045(3) -0.005(2) -0.016(2) O1M 0.044(3) 0.031(2) 0.036(2) -0.0142(19) 0.0116(19) -0.010(2) C1M 0.039(4) 0.039(4) 0.032(3) -0.013(3) 0.000(3) -0.012(3) O1W 0.033(2) 0.025(2) 0.033(2) 0.0013(16) -0.0178(17) -0.0154(18) O2W 0.057(3) 0.023(2) 0.028(2) -0.0110(17) 0.002(2) -0.020(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 O20 2.275(3) . ? Yb1 O1L 2.278(3) . ? Yb1 O30 2.283(3) . ? Yb1 O10 2.339(3) . ? Yb1 O3L 2.461(3) . ? Yb1 N4 2.532(4) . ? Yb1 N1 2.553(4) . ? Yb1 N2 2.574(4) . ? Yb1 N3 2.633(4) . ? Yb1 C1L 3.156(6) . ? Yb1 C21 3.158(5) . ? Yb1 C31 3.175(4) . ? N1 C10 1.484(6) . ? N1 C8 1.491(6) . ? N1 C1 1.500(6) . ? N2 C20 1.485(6) . ? N2 C2 1.485(5) . ? N2 C3 1.506(7) . ? N3 C30 1.476(5) . ? N3 C4 1.487(6) . ? N3 C5 1.497(6) . ? N4 C6 1.482(6) . ? N4 C7 1.488(6) . ? N10 C21 1.321(6) . ? N10 C22 1.477(6) . ? N20 C11 1.311(6) . ? N20 C12 1.479(6) . ? N30 C31 1.327(6) . ? N30 C32 1.481(6) . ? O10 C11 1.259(6) . ? O20 C21 1.264(6) . ? O30 C31 1.259(6) . ? C1 C2 1.529(6) . ? C3 C4 1.522(7) . ? C5 C6 1.521(7) . ? C7 C8 1.515(6) . ? C10 C11 1.506(7) . ? C12 C14 1.519(7) . ? C12 C13 1.528(7) . ? C14 C15 1.388(7) . ? C14 C19 1.393(7) . ? C15 C16 1.398(8) . ? C16 C17 1.386(9) . ? C17 C18 1.386(9) . ? C18 C19 1.392(8) . ? C20 C21 1.513(6) . ? C22 C24 1.515(7) . ? C22 C23 1.527(7) . ? C24 C25 1.397(7) . ? C24 C29 1.400(7) . ? C25 C26 1.404(8) . ? C26 C27 1.382(9) . ? C27 C28 1.389(8) . ? C28 C29 1.390(7) . ? C30 C31 1.513(7) . ? C32 C34 1.514(8) . ? C32 C33 1.526(7) . ? C34 C35 1.394(7) . ? C34 C39 1.406(7) . ? C35 C36 1.383(9) . ? C36 C37 1.390(9) . ? C37 C38 1.399(8) . ? C38 C39 1.380(8) . ? O1L C1L 1.286(6) . ? O2L C1L 1.236(7) . ? O3L C2L 1.434(6) . ? C1L C2L 1.531(7) . ? C2L C3L 1.527(7) . ? S1 O1C 1.441(4) . ? S1 O1A 1.445(4) . ? S1 O1B 1.450(4) . ? S1 C2S 1.841(6) . ? C1S F2B 1.314(7) . ? C1S F2C 1.336(8) . ? C1S F2A 1.341(7) . ? C1S S2 1.829(6) . ? F1A C2S 1.338(6) . ? F1B C2S 1.334(7) . ? F1C C2S 1.327(6) . ? S2 O2B 1.425(5) . ? S2 O2A 1.442(5) . ? S2 O2C 1.443(4) . ? O1M C1M 1.406(7) . ? 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 O20 Yb1 O1L 136.03(12) . . ? O20 Yb1 O30 82.50(12) . . ? O1L Yb1 O30 79.86(11) . . ? O20 Yb1 O10 81.91(11) . . ? O1L Yb1 O10 86.05(11) . . ? O30 Yb1 O10 139.57(11) . . ? O20 Yb1 O3L 69.36(11) . . ? O1L Yb1 O3L 66.92(11) . . ? O30 Yb1 O3L 71.71(12) . . ? O10 Yb1 O3L 67.90(11) . . ? O20 Yb1 N4 141.01(12) . . ? O1L Yb1 N4 71.02(12) . . ? O30 Yb1 N4 75.41(12) . . ? O10 Yb1 N4 134.55(11) . . ? O3L Yb1 N4 129.97(12) . . ? O20 Yb1 N1 134.73(12) . . ? O1L Yb1 N1 76.58(12) . . ? O30 Yb1 N1 141.62(12) . . ? O10 Yb1 N1 68.26(12) . . ? O3L Yb1 N1 123.71(12) . . ? N4 Yb1 N1 68.48(12) . . ? O20 Yb1 N2 68.19(11) . . ? O1L Yb1 N2 145.91(11) . . ? O30 Yb1 N2 133.09(12) . . ? O10 Yb1 N2 72.93(12) . . ? O3L Yb1 N2 124.97(11) . . ? N4 Yb1 N2 105.04(13) . . ? N1 Yb1 N2 70.85(12) . . ? O20 Yb1 N3 73.81(12) . . ? O1L Yb1 N3 132.38(12) . . ? O30 Yb1 N3 67.16(12) . . ? O10 Yb1 N3 140.95(11) . . ? O3L Yb1 N3 127.26(11) . . ? N4 Yb1 N3 68.13(12) . . ? N1 Yb1 N3 109.03(12) . . ? N2 Yb1 N3 69.84(12) . . ? O20 Yb1 C1L 116.70(13) . . ? O1L Yb1 C1L 20.20(13) . . ? O30 Yb1 C1L 67.04(13) . . ? O10 Yb1 C1L 87.47(13) . . ? O3L Yb1 C1L 49.16(13) . . ? N4 Yb1 C1L 83.62(14) . . ? N1 Yb1 C1L 95.83(13) . . ? N2 Yb1 C1L 159.22(13) . . ? N3 Yb1 C1L 130.69(13) . . ? O20 Yb1 C21 19.44(12) . . ? O1L Yb1 C21 147.39(12) . . ? O30 Yb1 C21 100.54(12) . . ? O10 Yb1 C21 72.52(11) . . ? O3L Yb1 C21 82.10(11) . . ? N4 Yb1 C21 141.10(12) . . ? N1 Yb1 C21 115.58(12) . . ? N2 Yb1 C21 49.59(12) . . ? N3 Yb1 C21 74.65(12) . . ? C1L Yb1 C21 131.25(13) . . ? O20 Yb1 C31 73.43(12) . . ? O1L Yb1 C31 97.80(12) . . ? O30 Yb1 C31 18.99(12) . . ? O10 Yb1 C31 148.18(12) . . ? O3L Yb1 C31 84.51(12) . . ? N4 Yb1 C31 75.47(12) . . ? N1 Yb1 C31 143.42(12) . . ? N2 Yb1 C31 114.29(12) . . ? N3 Yb1 C31 49.01(13) . . ? C1L Yb1 C31 86.00(13) . . ? C21 Yb1 C31 88.78(11) . . ? C10 N1 C8 108.8(3) . . ? C10 N1 C1 110.1(4) . . ? C8 N1 C1 109.7(4) . . ? C10 N1 Yb1 106.4(3) . . ? C8 N1 Yb1 111.3(3) . . ? C1 N1 Yb1 110.5(3) . . ? C20 N2 C2 109.6(3) . . ? C20 N2 C3 110.3(4) . . ? C2 N2 C3 108.4(4) . . ? C20 N2 Yb1 107.4(3) . . ? C2 N2 Yb1 110.8(3) . . ? C3 N2 Yb1 110.3(3) . . ? C30 N3 C4 110.6(3) . . ? C30 N3 C5 110.0(4) . . ? C4 N3 C5 108.6(4) . . ? C30 N3 Yb1 106.5(3) . . ? C4 N3 Yb1 110.1(3) . . ? C5 N3 Yb1 111.0(3) . . ? C6 N4 C7 111.8(4) . . ? C6 N4 Yb1 114.4(3) . . ? C7 N4 Yb1 115.6(3) . . ? C21 N10 C22 120.8(4) . . ? C11 N20 C12 123.8(4) . . ? C31 N30 C32 123.0(4) . . ? C11 O10 Yb1 121.6(3) . . ? C21 O20 Yb1 123.8(3) . . ? C31 O30 Yb1 124.8(3) . . ? N1 C1 C2 113.3(4) . . ? N2 C2 C1 111.6(4) . . ? N2 C3 C4 112.8(4) . . ? N3 C4 C3 110.8(4) . . ? N3 C5 C6 111.8(4) . . ? N4 C6 C5 109.0(4) . . ? N4 C7 C8 109.2(4) . . ? N1 C8 C7 111.4(4) . . ? N1 C10 C11 111.5(4) . . ? O10 C11 N20 122.6(5) . . ? O10 C11 C10 119.4(4) . . ? N20 C11 C10 118.0(4) . . ? O10 C11 Yb1 38.7(2) . . ? N20 C11 Yb1 161.2(3) . . ? C10 C11 Yb1 80.7(2) . . ? N20 C12 C14 110.9(4) . . ? N20 C12 C13 107.8(4) . . ? C14 C12 C13 112.2(4) . . ? C15 C14 C19 119.7(5) . . ? C15 C14 C12 120.0(4) . . ? C19 C14 C12 120.2(4) . . ? C14 C15 C16 120.4(5) . . ? C17 C16 C15 119.2(6) . . ? C16 C17 C18 120.8(5) . . ? C17 C18 C19 119.8(5) . . ? C18 C19 C14 120.0(5) . . ? N2 C20 C21 110.4(4) . . ? O20 C21 N10 121.9(4) . . ? O20 C21 C20 120.0(4) . . ? N10 C21 C20 118.1(4) . . ? O20 C21 Yb1 36.8(2) . . ? N10 C21 Yb1 158.5(3) . . ? C20 C21 Yb1 83.2(3) . . ? N10 C22 C24 111.0(4) . . ? N10 C22 C23 109.0(4) . . ? C24 C22 C23 112.3(4) . . ? C25 C24 C29 118.7(5) . . ? C25 C24 C22 120.3(5) . . ? C29 C24 C22 121.1(5) . . ? C24 C25 C26 120.4(5) . . ? C27 C26 C25 120.5(5) . . ? C26 C27 C28 119.2(5) . . ? C27 C28 C29 120.9(5) . . ? C28 C29 C24 120.3(5) . . ? N3 C30 C31 110.7(4) . . ? O30 C31 N30 121.8(5) . . ? O30 C31 C30 119.9(4) . . ? N30 C31 C30 118.2(4) . . ? O30 C31 Yb1 36.2(2) . . ? N30 C31 Yb1 157.7(4) . . ? C30 C31 Yb1 83.7(2) . . ? N30 C32 C34 110.2(4) . . ? N30 C32 C33 108.0(4) . . ? C34 C32 C33 115.2(4) . . ? C35 C34 C39 118.7(5) . . ? C35 C34 C32 119.1(5) . . ? C39 C34 C32 122.2(5) . . ? C36 C35 C34 121.5(5) . . ? C35 C36 C37 119.5(5) . . ? C36 C37 C38 119.8(5) . . ? C39 C38 C37 120.6(6) . . ? C38 C39 C34 120.0(5) . . ? C1L O1L Yb1 122.1(3) . . ? C2L O3L Yb1 116.9(3) . . ? O2L C1L O1L 124.9(5) . . ? O2L C1L C2L 117.9(5) . . ? O1L C1L C2L 117.1(4) . . ? O2L C1L Yb1 150.9(4) . . ? O1L C1L Yb1 37.7(2) . . ? C2L C1L Yb1 84.1(3) . . ? O3L C2L C3L 110.7(4) . . ? O3L C2L C1L 109.3(4) . . ? C3L C2L C1L 110.8(4) . . ? O1C S1 O1A 114.8(2) . . ? O1C S1 O1B 115.3(2) . . ? O1A S1 O1B 115.0(2) . . ? O1C S1 C2S 102.7(2) . . ? O1A S1 C2S 103.9(3) . . ? O1B S1 C2S 102.7(2) . . ? F2B C1S F2C 109.4(6) . . ? F2B C1S F2A 107.7(5) . . ? F2C C1S F2A 105.8(5) . . ? F2B C1S S2 112.8(4) . . ? F2C C1S S2 110.3(4) . . ? F2A C1S S2 110.5(4) . . ? O2B S2 O2A 116.2(4) . . ? O2B S2 O2C 114.9(3) . . ? O2A S2 O2C 113.5(3) . . ? O2B S2 C1S 103.8(3) . . ? O2A S2 C1S 103.0(3) . . ? O2C S2 C1S 103.2(3) . . ? F1C C2S F1B 108.3(5) . . ? F1C C2S F1A 108.2(4) . . ? F1B C2S F1A 106.7(5) . . ? F1C C2S S1 110.6(4) . . ? F1B C2S S1 111.1(4) . . ? F1A C2S S1 111.8(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.937 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.095