# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_jmgy6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris(1,1,1,5,5,6,6,7,7,7-decafluoro-2,4-heptanedionate)mono(5-nitro-1,10-phenanthroline) ytterbium(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H10 F30 N3 O8 Yb' _chemical_formula_sum 'C33 H10 F30 N3 O8 Yb' _chemical_formula_weight 1319.48 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0391(3) _cell_length_b 25.3149(7) _cell_length_c 18.4810(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.213(2) _cell_angle_gamma 90.00 _cell_volume 4176.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7433 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 28.13 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2532 _exptl_absorpt_coefficient_mu 2.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2000)' _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 95198 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 30.23 _reflns_number_total 12348 _reflns_number_gt 9195 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material SHELXL-97 _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^)+(0.0301P)^2^+13.2194P] 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 12348 _refine_ls_number_parameters 886 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.009 _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 0.259485(17) 0.359842(6) 0.141479(11) 0.02986(5) Uani 1 1 d . . . F1A F 0.2785(9) 0.4874(3) -0.1042(5) 0.085(2) Uani 0.781(10) 1 d P A 1 F2A F 0.2297(8) 0.4065(2) -0.1194(3) 0.0819(18) Uani 0.781(10) 1 d P A 1 F3A F 0.4536(7) 0.4334(3) -0.0448(5) 0.096(2) Uani 0.781(10) 1 d P A 1 F1B F 0.331(3) 0.3944(7) -0.0894(13) 0.078(7) Uani 0.219(10) 1 d P A 2 F2B F 0.463(3) 0.4540(18) -0.043(2) 0.158(16) Uani 0.219(10) 1 d P A 2 F3B F 0.243(3) 0.4723(16) -0.1197(15) 0.122(15) Uani 0.219(10) 1 d P A 2 F4 F 0.0852(4) 0.56968(11) 0.05520(18) 0.0607(8) Uani 1 1 d . A . F5 F 0.0853(3) 0.53249(11) 0.1603(2) 0.0608(8) Uani 1 1 d . A . F6 F 0.3735(4) 0.59035(12) 0.1297(2) 0.0680(8) Uani 1 1 d . . . F7 F 0.2465(4) 0.62086(11) 0.1903(2) 0.0720(9) Uani 1 1 d . . . F8A F 0.3557(6) 0.5418(2) 0.2985(3) 0.1296(19) Uani 1 1 d . A . F9A F 0.5292(4) 0.58819(12) 0.2887(2) 0.0778(11) Uani 1 1 d . A . F10A F 0.4781(4) 0.51195(13) 0.2369(3) 0.1196(19) Uani 1 1 d . A . F11A F 0.5442(4) 0.23221(12) 0.0587(2) 0.0648(8) Uani 1 1 d . . . F12A F 0.6940(3) 0.25578(16) 0.1772(2) 0.0801(11) Uani 1 1 d . . . F13A F 0.5974(4) 0.17806(13) 0.1546(3) 0.0908(11) Uani 1 1 d . . . F14 F 0.2294(4) 0.14843(12) 0.2321(2) 0.0754(10) Uani 1 1 d . . . F15 F 0.1071(4) 0.21127(13) 0.25494(19) 0.0679(9) Uani 1 1 d . . . F16 F 0.0309(4) 0.16796(18) 0.0632(2) 0.0918(12) Uani 1 1 d . C . F17 F -0.0966(3) 0.21457(13) 0.1066(2) 0.0749(10) Uani 1 1 d . C . F18 F 0.0033(6) 0.08299(15) 0.1386(4) 0.140(2) Uani 1 1 d . . . F19 F -0.2081(5) 0.12010(19) 0.0738(3) 0.1114(16) Uani 1 1 d . . . F20 F -0.0908(4) 0.12721(16) 0.2011(3) 0.0940(13) Uani 1 1 d . . . F21A F 0.8012(4) 0.4199(4) 0.4079(3) 0.193(4) Uani 1 1 d . . . F22A F 0.8023(4) 0.37263(15) 0.3150(3) 0.0923(13) Uani 1 1 d . . . F23A F 0.7504(4) 0.45181(16) 0.2947(4) 0.141(3) Uani 1 1 d . . . F24 F 0.2023(6) 0.35135(17) 0.3828(3) 0.1262(17) Uani 1 1 d . . . F25 F 0.4233(6) 0.3743(2) 0.4719(2) 0.1254(18) Uani 1 1 d . . . F26 F 0.1284(8) 0.4491(3) 0.3407(3) 0.175(3) Uani 1 1 d . C . F27 F 0.3422(8) 0.47593(17) 0.4137(4) 0.164(2) Uani 1 1 d . C . F28A F 0.1601(16) 0.4062(5) 0.4988(9) 0.131(4) Uani 0.571(12) 1 d P B 1 F29A F 0.1096(11) 0.4847(5) 0.4637(6) 0.095(3) Uani 0.571(12) 1 d P B 1 F30A F 0.3339(14) 0.4610(6) 0.5407(7) 0.119(5) Uani 0.571(12) 1 d P B 1 F28B F 0.1007(16) 0.4183(11) 0.4611(12) 0.161(10) Uani 0.429(12) 1 d P B 2 F29B F 0.192(2) 0.4959(8) 0.4873(12) 0.134(7) Uani 0.429(12) 1 d P B 2 F30B F 0.3114(18) 0.4295(9) 0.5467(8) 0.127(8) Uani 0.429(12) 1 d P B 2 O1 O 0.3076(3) 0.39640(11) 0.04296(18) 0.0360(6) Uani 1 1 d . A . O2 O 0.2092(3) 0.44851(10) 0.13896(17) 0.0350(6) Uani 1 1 d . A . O3 O 0.4201(3) 0.29890(11) 0.13357(19) 0.0386(7) Uani 1 1 d . C . O4 O 0.1916(3) 0.27977(11) 0.17561(17) 0.0347(6) Uani 1 1 d . C . O5 O 0.4960(3) 0.38928(12) 0.22533(19) 0.0421(7) Uani 1 1 d . C . O6 O 0.2650(3) 0.37308(11) 0.26471(18) 0.0398(7) Uani 1 1 d . C . C1 C 0.3170(6) 0.4420(2) -0.0649(3) 0.0541(12) Uani 1 1 d . . . C2 C 0.2874(4) 0.44059(16) 0.0094(3) 0.0360(9) Uani 1 1 d . A . C3 C 0.2422(5) 0.48679(16) 0.0320(3) 0.0371(9) Uani 1 1 d . . . H3 H 0.2338 0.5179 0.0034 0.044 Uiso 1 1 calc R A . C4 C 0.2096(4) 0.48675(15) 0.0969(2) 0.0329(8) Uani 1 1 d . A . C5 C 0.1690(5) 0.54011(16) 0.1219(3) 0.0398(9) Uani 1 1 d . . . C6 C 0.3005(6) 0.57623(18) 0.1741(3) 0.0511(12) Uani 1 1 d . A . C7 C 0.4173(7) 0.5546(2) 0.2517(4) 0.0709(18) Uani 1 1 d . . . C8 C 0.5689(5) 0.22792(19) 0.1348(3) 0.0481(11) Uani 1 1 d . C . C9 C 0.4389(4) 0.25012(17) 0.1466(3) 0.0379(9) Uani 1 1 d . . . C10 C 0.3555(5) 0.21584(16) 0.1670(3) 0.0433(10) Uani 1 1 d . C . H10 H 0.3790 0.1800 0.1722 0.052 Uiso 1 1 calc R . . C11 C 0.2365(4) 0.23332(16) 0.1800(2) 0.0354(9) Uani 1 1 d . . . C12 C 0.1467(5) 0.19167(17) 0.2003(3) 0.0422(10) Uani 1 1 d . C . C13 C 0.0013(6) 0.1750(2) 0.1251(3) 0.0496(11) Uani 1 1 d . . . C14 C -0.0755(7) 0.1249(2) 0.1351(5) 0.0723(18) Uani 1 1 d . C . C15 C 0.7319(6) 0.4107(3) 0.3284(4) 0.080(2) Uani 1 1 d . C . C16 C 0.5650(5) 0.39803(18) 0.3000(3) 0.0477(12) Uani 1 1 d . . . C17 C 0.5115(6) 0.3975(2) 0.3561(3) 0.0544(13) Uani 1 1 d . C . H17 H 0.5753 0.4059 0.4100 0.065 Uiso 1 1 calc R . . C18 C 0.3633(6) 0.38469(17) 0.3337(3) 0.0455(11) Uani 1 1 d . . . C19 C 0.3115(7) 0.3864(2) 0.3997(3) 0.0582(14) Uani 1 1 d . C . C20 C 0.2484(8) 0.4390(3) 0.4084(4) 0.0699(16) Uani 1 1 d . . . C21 C 0.2103(7) 0.4469(3) 0.4785(4) 0.0700(17) Uani 1 1 d . B . N1A N -0.0057(10) 0.3712(3) 0.1107(5) 0.0250(17) Uani 0.553(4) 1 d P C 1 N2A N 0.0823(10) 0.3187(4) 0.0165(6) 0.028(2) Uani 0.553(4) 1 d P C 1 C26A C -0.1072(8) 0.3404(3) 0.0506(5) 0.0218(16) Uani 0.553(4) 1 d P C 1 C27A C -0.0638(9) 0.3115(3) -0.0009(5) 0.0203(16) Uani 0.553(4) 1 d P C 1 C28A C 0.1251(11) 0.2934(5) -0.0330(8) 0.038(3) Uani 0.553(4) 1 d P C 1 H28A H 0.2234 0.2980 -0.0240 0.045 Uiso 0.553(4) 1 calc PR C 1 C22A C -0.0476(10) 0.4001(4) 0.1559(6) 0.0328(18) Uani 0.553(4) 1 d P C 1 H22A H 0.0219 0.4222 0.1951 0.039 Uiso 0.553(4) 1 calc PR C 1 C23A C -0.1943(9) 0.3985(4) 0.1465(5) 0.0402(19) Uani 0.553(4) 1 d P C 1 H23A H -0.2206 0.4187 0.1800 0.048 Uiso 0.553(4) 1 calc PR C 1 C24A C -0.2961(11) 0.3676(4) 0.0889(7) 0.043(2) Uani 0.553(4) 1 d P C 1 H24A H -0.3935 0.3660 0.0826 0.051 Uiso 0.553(4) 1 calc PR C 1 C25A C -0.2565(9) 0.3381(4) 0.0392(6) 0.0323(17) Uani 0.553(4) 1 d P C 1 C29A C 0.0325(13) 0.2607(4) -0.0971(6) 0.042(2) Uani 0.553(4) 1 d P C 1 H29A H 0.0686 0.2436 -0.1292 0.050 Uiso 0.553(4) 1 calc PR C 1 C30A C -0.1117(13) 0.2543(4) -0.1114(6) 0.041(2) Uani 0.553(4) 1 d P C 1 H30A H -0.1748 0.2324 -0.1536 0.049 Uiso 0.553(4) 1 calc PR C 1 C31A C -0.1668(9) 0.2799(3) -0.0643(5) 0.0309(17) Uani 0.553(4) 1 d P C 1 C32A C -0.3163(12) 0.2769(4) -0.0731(7) 0.027(3) Uani 0.553(4) 1 d P C 1 C33A C -0.3589(8) 0.3065(3) -0.0240(6) 0.042(2) Uani 0.553(4) 1 d P C 1 H33A H -0.4581 0.3053 -0.0333 0.050 Uiso 0.553(4) 1 calc PR C 1 O7A O -0.4072(8) 0.2204(3) -0.1807(5) 0.072(2) Uani 0.553(4) 1 d P C 1 N3A N -0.4373(9) 0.2459(3) -0.1344(5) 0.057(2) Uani 0.553(4) 1 d P C 1 O8A O -0.5659(17) 0.2465(7) -0.1386(11) 0.077(5) Uani 0.553(4) 1 d P C 1 N1B N -0.0155(14) 0.3589(4) 0.0899(7) 0.028(2) Uani 0.447(4) 1 d P C 2 N2B N 0.1092(12) 0.3117(5) 0.0072(7) 0.023(2) Uani 0.447(4) 1 d P C 2 C26B C -0.1041(12) 0.3267(4) 0.0248(7) 0.026(2) Uani 0.447(4) 1 d P C 2 C27B C -0.0357(13) 0.3017(4) -0.0173(6) 0.026(2) Uani 0.447(4) 1 d P C 2 C28B C 0.1751(13) 0.2896(6) -0.0315(9) 0.031(3) Uani 0.447(4) 1 d P C 2 H28B H 0.2765 0.2962 -0.0133 0.038 Uiso 0.447(4) 1 calc PR C 2 C22B C -0.0772(14) 0.3836(4) 0.1301(7) 0.037(3) Uani 0.447(4) 1 d P C 2 H22B H -0.0163 0.4052 0.1734 0.045 Uiso 0.447(4) 1 calc PR C 2 C23B C -0.2329(15) 0.3790(5) 0.1112(8) 0.038(3) Uani 0.447(4) 1 d P C 2 H23B H -0.2725 0.3973 0.1406 0.046 Uiso 0.447(4) 1 calc PR C 2 C24B C -0.3194(12) 0.3466(4) 0.0485(7) 0.034(2) Uani 0.447(4) 1 d P C 2 H24B H -0.4194 0.3417 0.0359 0.041 Uiso 0.447(4) 1 calc PR C 2 C25B C -0.2616(10) 0.3206(4) 0.0025(7) 0.030(2) Uani 0.447(4) 1 d P C 2 C29B C 0.1021(13) 0.2568(5) -0.0986(7) 0.041(3) Uani 0.447(4) 1 d P C 2 H29B H 0.1511 0.2430 -0.1266 0.049 Uiso 0.447(4) 1 calc PR C 2 C30B C -0.0465(17) 0.2457(4) -0.1215(7) 0.039(3) Uani 0.447(4) 1 d P C 2 H30B H -0.0977 0.2221 -0.1640 0.047 Uiso 0.447(4) 1 calc PR C 2 C31B C -0.1203(12) 0.2689(4) -0.0824(7) 0.031(2) Uani 0.447(4) 1 d P C 2 C32B C -0.2735(11) 0.2604(4) -0.1032(6) 0.035(2) Uani 0.447(4) 1 d P C 2 H32B H -0.3298 0.2363 -0.1437 0.042 Uiso 0.447(4) 1 calc PR C 2 C33B C -0.3386(16) 0.2880(5) -0.0632(10) 0.027(3) Uani 0.447(4) 1 d P C 2 N3B N -0.5024(10) 0.2763(4) -0.0973(6) 0.046(2) Uani 0.447(4) 1 d P C 2 O7B O -0.5760(8) 0.3110(4) -0.0879(6) 0.067(3) Uani 0.447(4) 1 d P C 2 O8B O -0.5436(19) 0.2344(7) -0.1339(14) 0.060(4) Uani 0.447(4) 1 d P 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 0.02608(7) 0.02315(7) 0.03802(8) -0.00102(7) 0.01265(6) -0.00057(7) F1A 0.145(5) 0.062(3) 0.080(4) 0.029(3) 0.079(4) 0.028(3) F2A 0.116(4) 0.084(4) 0.052(3) -0.021(2) 0.044(3) -0.005(3) F3A 0.079(3) 0.145(6) 0.103(4) 0.058(4) 0.075(3) 0.055(4) F1B 0.150(19) 0.046(9) 0.078(13) -0.014(8) 0.084(13) -0.011(11) F2B 0.105(15) 0.30(4) 0.100(18) -0.06(2) 0.069(14) -0.13(2) F3B 0.082(13) 0.26(4) 0.038(10) 0.060(17) 0.039(10) 0.10(2) F4 0.0762(19) 0.0404(15) 0.0613(18) 0.0136(13) 0.0277(15) 0.0242(14) F5 0.0741(18) 0.0419(15) 0.094(2) 0.0066(14) 0.0620(17) 0.0121(14) F6 0.102(2) 0.0497(17) 0.077(2) 0.0025(15) 0.0622(19) -0.0100(16) F7 0.096(2) 0.0340(14) 0.086(2) -0.0122(15) 0.041(2) 0.0126(15) F8A 0.137(4) 0.172(5) 0.087(3) 0.069(3) 0.057(3) 0.001(4) F9A 0.084(2) 0.0487(18) 0.068(2) -0.0115(15) 0.0071(18) -0.0204(16) F10A 0.075(2) 0.0428(18) 0.146(4) -0.025(2) -0.032(2) 0.0176(17) F11A 0.086(2) 0.0608(18) 0.0669(19) 0.0064(15) 0.0520(17) 0.0124(16) F12A 0.0407(15) 0.106(3) 0.093(3) -0.015(2) 0.0299(16) 0.0093(17) F13A 0.119(2) 0.0574(18) 0.153(3) 0.0588(19) 0.111(2) 0.0554(18) F14 0.0615(18) 0.0577(18) 0.106(3) 0.0515(18) 0.0375(18) 0.0171(15) F15 0.094(2) 0.073(2) 0.0582(18) -0.0080(15) 0.0534(17) -0.0180(18) F16 0.096(2) 0.127(3) 0.069(2) -0.044(2) 0.052(2) -0.051(2) F17 0.0499(17) 0.066(2) 0.095(2) 0.0322(18) 0.0208(17) 0.0062(15) F18 0.125(4) 0.0370(19) 0.280(7) -0.019(3) 0.111(4) -0.017(2) F19 0.084(3) 0.118(3) 0.120(4) -0.020(3) 0.037(3) -0.059(3) F20 0.095(3) 0.098(3) 0.105(3) 0.025(2) 0.059(2) -0.027(2) F21A 0.046(2) 0.415(11) 0.092(3) -0.114(5) 0.008(2) -0.045(4) F22A 0.0498(18) 0.077(2) 0.143(4) 0.005(2) 0.038(2) 0.0208(17) F23A 0.0441(19) 0.057(2) 0.295(7) 0.001(3) 0.054(3) -0.0126(17) F24 0.214(4) 0.099(3) 0.126(3) -0.047(2) 0.129(3) -0.094(3) F25 0.141(4) 0.180(5) 0.054(2) 0.059(3) 0.043(2) 0.076(4) F26 0.232(6) 0.214(6) 0.053(3) 0.021(3) 0.042(3) 0.146(5) F27 0.320(6) 0.060(2) 0.257(5) -0.034(3) 0.257(5) -0.043(3) F28A 0.208(10) 0.102(7) 0.168(10) -0.010(7) 0.159(8) -0.038(8) F29A 0.095(6) 0.127(9) 0.081(6) 0.003(5) 0.055(5) 0.032(6) F30A 0.090(6) 0.192(13) 0.067(6) -0.065(7) 0.029(5) -0.050(7) F28B 0.086(8) 0.28(3) 0.152(15) -0.086(15) 0.089(8) -0.072(11) F29B 0.187(18) 0.121(11) 0.133(13) -0.036(9) 0.106(14) 0.016(13) F30B 0.097(10) 0.24(2) 0.038(5) 0.009(10) 0.026(6) 0.034(12) O1 0.0389(14) 0.0285(13) 0.0456(16) -0.0041(12) 0.0237(13) -0.0026(11) O2 0.0429(14) 0.0259(13) 0.0426(16) 0.0016(11) 0.0249(13) 0.0001(11) O3 0.0358(14) 0.0271(13) 0.0527(18) -0.0003(12) 0.0201(13) 0.0004(11) O4 0.0332(13) 0.0290(13) 0.0397(15) 0.0005(11) 0.0148(12) 0.0010(11) O5 0.0317(14) 0.0386(16) 0.0475(18) -0.0093(13) 0.0108(13) -0.0034(12) O6 0.0438(15) 0.0327(15) 0.0404(16) -0.0009(12) 0.0172(13) -0.0029(12) C1 0.070(3) 0.052(3) 0.056(3) 0.003(2) 0.043(3) 0.010(3) C2 0.0338(18) 0.035(2) 0.039(2) -0.0020(16) 0.0166(17) -0.0055(16) C3 0.046(2) 0.0291(19) 0.039(2) 0.0040(16) 0.0218(18) 0.0020(17) C4 0.0347(18) 0.0249(17) 0.039(2) -0.0016(15) 0.0172(17) -0.0001(15) C5 0.047(2) 0.031(2) 0.048(2) 0.0046(17) 0.027(2) 0.0081(18) C6 0.068(3) 0.029(2) 0.056(3) -0.002(2) 0.028(2) 0.005(2) C7 0.076(4) 0.039(3) 0.072(4) 0.001(3) 0.011(3) -0.003(3) C8 0.050(2) 0.040(2) 0.060(3) 0.011(2) 0.031(2) 0.014(2) C9 0.0348(19) 0.035(2) 0.043(2) 0.0026(17) 0.0168(18) 0.0060(17) C10 0.054(2) 0.0267(19) 0.058(3) 0.0053(18) 0.033(2) 0.0091(18) C11 0.0357(19) 0.0314(19) 0.035(2) 0.0052(16) 0.0122(17) -0.0020(16) C12 0.048(2) 0.035(2) 0.045(2) 0.0108(18) 0.023(2) 0.0044(18) C13 0.055(3) 0.046(3) 0.057(3) -0.006(2) 0.033(2) -0.012(2) C14 0.067(4) 0.048(3) 0.105(5) 0.002(3) 0.043(4) -0.014(3) C15 0.037(3) 0.101(5) 0.084(4) -0.053(4) 0.011(3) -0.004(3) C16 0.0296(19) 0.040(2) 0.057(3) -0.013(2) 0.005(2) 0.0005(18) C17 0.050(3) 0.056(3) 0.039(3) -0.007(2) 0.004(2) 0.006(2) C18 0.058(3) 0.030(2) 0.042(2) 0.0085(18) 0.017(2) 0.006(2) C19 0.081(4) 0.048(3) 0.043(3) 0.011(2) 0.026(3) 0.000(3) C20 0.099(4) 0.066(4) 0.055(3) 0.003(3) 0.044(3) 0.008(3) C21 0.072(4) 0.094(5) 0.049(3) -0.010(3) 0.032(3) -0.011(4) N1A 0.030(3) 0.026(4) 0.024(4) -0.004(3) 0.017(3) 0.007(3) N2A 0.036(4) 0.027(4) 0.030(4) -0.006(3) 0.021(3) 0.004(3) C26A 0.021(3) 0.022(4) 0.018(4) 0.006(3) 0.005(3) -0.004(3) C27A 0.027(3) 0.019(4) 0.016(3) -0.005(3) 0.011(3) -0.001(3) C28A 0.034(5) 0.033(5) 0.047(5) 0.005(4) 0.020(5) 0.004(4) C22A 0.032(4) 0.035(5) 0.036(4) 0.000(3) 0.020(3) 0.006(3) C23A 0.041(4) 0.052(5) 0.034(4) 0.008(4) 0.022(4) 0.013(4) C24A 0.034(5) 0.046(6) 0.047(6) 0.005(5) 0.018(4) 0.005(4) C25A 0.025(4) 0.034(4) 0.037(5) 0.012(3) 0.014(4) 0.000(3) C29A 0.060(6) 0.034(4) 0.040(5) -0.010(3) 0.030(5) -0.006(5) C30A 0.059(6) 0.033(5) 0.029(5) -0.006(4) 0.017(4) -0.007(4) C31A 0.041(4) 0.019(3) 0.025(4) 0.004(3) 0.008(3) -0.005(3) C32A 0.030(4) 0.015(4) 0.029(4) -0.004(3) 0.006(4) 0.003(3) C33A 0.020(3) 0.042(4) 0.051(5) 0.018(4) 0.007(3) -0.003(3) O7A 0.059(4) 0.058(4) 0.060(4) -0.021(4) -0.005(3) -0.013(3) N3A 0.053(5) 0.051(4) 0.034(4) 0.003(3) -0.007(3) -0.021(4) O8A 0.038(5) 0.112(12) 0.062(7) -0.013(7) 0.006(4) -0.013(6) N1B 0.040(5) 0.019(4) 0.031(5) -0.003(4) 0.021(4) 0.007(4) N2B 0.033(5) 0.019(4) 0.029(4) -0.008(3) 0.024(4) 0.001(3) C26B 0.032(5) 0.020(5) 0.023(5) -0.003(4) 0.012(4) 0.000(4) C27B 0.040(5) 0.020(5) 0.026(5) -0.001(3) 0.022(4) 0.006(4) C28B 0.033(6) 0.029(5) 0.039(6) -0.004(4) 0.022(5) 0.003(5) C22B 0.042(6) 0.024(5) 0.033(6) -0.005(4) 0.006(5) -0.002(4) C23B 0.046(7) 0.038(6) 0.029(6) -0.007(5) 0.016(6) 0.002(6) C24B 0.025(5) 0.032(5) 0.038(6) 0.007(4) 0.008(5) -0.001(4) C25B 0.027(4) 0.025(4) 0.032(5) 0.006(4) 0.008(4) 0.004(4) C29B 0.047(6) 0.042(6) 0.040(6) 0.005(4) 0.026(5) 0.005(5) C30B 0.061(8) 0.025(5) 0.026(5) -0.005(4) 0.015(5) -0.002(5) C31B 0.038(5) 0.030(6) 0.027(6) -0.005(4) 0.015(5) 0.003(4) C32B 0.038(5) 0.022(4) 0.035(5) -0.005(4) 0.008(4) -0.009(4) C33B 0.028(5) 0.015(6) 0.039(6) 0.002(4) 0.017(4) 0.008(4) N3B 0.037(4) 0.051(5) 0.043(5) 0.002(4) 0.012(4) -0.008(4) O7B 0.033(4) 0.071(6) 0.085(6) 0.001(5) 0.017(4) 0.007(4) O8B 0.034(7) 0.046(6) 0.078(9) -0.015(5) 0.006(6) -0.023(5) _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 O6 2.278(3) . ? Yb1 O1 2.283(3) . ? Yb1 O3 2.284(3) . ? Yb1 O5 2.287(3) . ? Yb1 O2 2.297(3) . ? Yb1 O4 2.316(3) . ? Yb1 N2A 2.413(10) . ? Yb1 N1A 2.471(9) . ? Yb1 N1B 2.475(13) . ? Yb1 N2B 2.549(11) . ? F1A C1 1.320(9) . ? F2A C1 1.334(8) . ? F3A C1 1.265(7) . ? F1B C1 1.318(17) . ? F2B C1 1.36(3) . ? F3B C1 1.22(3) . ? F4 C5 1.356(5) . ? F5 C5 1.339(5) . ? F6 C6 1.374(6) . ? F7 C6 1.345(5) . ? F8A C7 1.313(8) . ? F9A C7 1.323(6) . ? F10A C7 1.329(7) . ? F11A C8 1.317(6) . ? F12A C8 1.337(6) . ? F13A C8 1.309(5) . ? F14 C12 1.337(5) . ? F15 C12 1.337(5) . ? F16 C13 1.319(6) . ? F17 C13 1.333(6) . ? F18 C14 1.306(7) . ? F19 C14 1.300(7) . ? F20 C14 1.300(8) . ? F21A C15 1.326(8) . ? F22A C15 1.285(7) . ? F23A C15 1.269(9) . ? F24 C19 1.332(7) . ? F25 C19 1.328(6) . ? F26 C20 1.306(8) . ? F27 C20 1.299(8) . ? F28A C21 1.274(13) . ? F29A C21 1.327(13) . ? F30A C21 1.298(12) . ? F28B C21 1.230(18) . ? F29B C21 1.277(19) . ? F30B C21 1.281(15) . ? O1 C2 1.250(5) . ? O2 C4 1.243(5) . ? O3 C9 1.256(5) . ? O4 C11 1.248(5) . ? O5 C16 1.249(6) . ? O6 C18 1.239(5) . ? C1 C2 1.532(7) . ? C2 C3 1.387(6) . ? C3 C4 1.379(6) . ? C3 H3 0.9300 . ? C4 C5 1.542(6) . ? C5 C6 1.531(7) . ? C6 C7 1.480(8) . ? C8 C9 1.525(6) . ? C9 C10 1.373(6) . ? C10 C11 1.394(6) . ? C10 H10 0.9300 . ? C11 C12 1.542(6) . ? C12 C13 1.544(7) . ? C13 C14 1.540(7) . ? C15 C16 1.543(7) . ? C16 C17 1.369(8) . ? C17 C18 1.388(7) . ? C17 H17 0.9300 . ? C18 C19 1.530(7) . ? C19 C20 1.515(8) . ? C20 C21 1.523(8) . ? N1A C22A 1.316(11) . ? N1A C26A 1.358(10) . ? N2A C28A 1.338(13) . ? N2A C27A 1.363(12) . ? C26A C25A 1.417(12) . ? C26A C27A 1.418(11) . ? C27A C31A 1.405(10) . ? C28A C29A 1.397(16) . ? C28A H28A 0.9300 . ? C22A C23A 1.402(12) . ? C22A H22A 0.9300 . ? C23A C24A 1.340(14) . ? C23A H23A 0.9300 . ? C24A C25A 1.376(15) . ? C24A H24A 0.9300 . ? C25A C33A 1.402(12) . ? C29A C30A 1.357(15) . ? C29A H29A 0.9300 . ? C30A C31A 1.385(14) . ? C30A H30A 0.9300 . ? C31A C32A 1.437(15) . ? C32A C33A 1.385(13) . ? C32A N3A 1.456(12) . ? C33A H33A 0.9300 . ? O7A N3A 1.215(12) . ? N3A O8A 1.257(19) . ? N1B C22B 1.322(15) . ? N1B C26B 1.387(13) . ? N2B C28B 1.301(14) . ? N2B C27B 1.335(15) . ? C26B C27B 1.402(14) . ? C26B C25B 1.448(15) . ? C27B C31B 1.387(16) . ? C28B C29B 1.390(19) . ? C28B H28B 0.9300 . ? C22B C23B 1.442(19) . ? C22B H22B 0.9300 . ? C23B C24B 1.359(15) . ? C23B H23B 0.9300 . ? C24B C25B 1.395(16) . ? C24B H24B 0.9300 . ? C25B C33B 1.374(18) . ? C29B C30B 1.381(17) . ? C29B H29B 0.9300 . ? C30B C31B 1.382(16) . ? C30B H30B 0.9300 . ? C31B C32B 1.420(15) . ? C32B C33B 1.381(15) . ? C32B H32B 0.9300 . ? C33B N3B 1.497(17) . ? N3B O7B 1.211(12) . ? N3B O8B 1.22(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Yb1 O1 145.17(10) . . ? O6 Yb1 O3 117.93(11) . . ? O1 Yb1 O3 79.02(10) . . ? O6 Yb1 O5 74.43(11) . . ? O1 Yb1 O5 82.84(11) . . ? O3 Yb1 O5 73.67(10) . . ? O6 Yb1 O2 77.35(10) . . ? O1 Yb1 O2 73.28(10) . . ? O3 Yb1 O2 144.49(10) . . ? O5 Yb1 O2 81.13(10) . . ? O6 Yb1 O4 74.46(10) . . ? O1 Yb1 O4 140.18(10) . . ? O3 Yb1 O4 74.36(10) . . ? O5 Yb1 O4 116.37(10) . . ? O2 Yb1 O4 140.50(10) . . ? O6 Yb1 N2A 133.7(3) . . ? O1 Yb1 N2A 75.2(3) . . ? O3 Yb1 N2A 83.1(2) . . ? O5 Yb1 N2A 150.6(2) . . ? O2 Yb1 N2A 110.1(3) . . ? O4 Yb1 N2A 72.7(3) . . ? O6 Yb1 N1A 75.2(2) . . ? O1 Yb1 N1A 111.6(2) . . ? O3 Yb1 N1A 141.4(2) . . ? O5 Yb1 N1A 142.52(19) . . ? O2 Yb1 N1A 71.2(2) . . ? O4 Yb1 N1A 75.2(2) . . ? N2A Yb1 N1A 65.5(3) . . ? O6 Yb1 N1B 84.2(3) . . ? O1 Yb1 N1B 107.6(3) . . ? O3 Yb1 N1B 131.7(2) . . ? O5 Yb1 N1B 153.4(2) . . ? O2 Yb1 N1B 78.8(2) . . ? O4 Yb1 N1B 71.4(3) . . ? N2A Yb1 N1B 54.8(3) . . ? N1A Yb1 N1B 10.9(2) . . ? O6 Yb1 N2B 141.0(3) . . ? O1 Yb1 N2B 70.4(3) . . ? O3 Yb1 N2B 74.7(2) . . ? O5 Yb1 N2B 141.7(3) . . ? O2 Yb1 N2B 114.9(3) . . ? O4 Yb1 N2B 74.3(3) . . ? N2A Yb1 N2B 9.2(3) . . ? N1A Yb1 N2B 74.7(3) . . ? N1B Yb1 N2B 64.0(3) . . ? C2 O1 Yb1 135.5(3) . . ? C4 O2 Yb1 135.3(3) . . ? C9 O3 Yb1 134.5(3) . . ? C11 O4 Yb1 134.4(3) . . ? C16 O5 Yb1 133.3(3) . . ? C18 O6 Yb1 135.0(3) . . ? F3B C1 F3A 121.5(16) . . ? F3B C1 F1B 114.3(19) . . ? F3A C1 F1B 70.9(12) . . ? F3B C1 F1A 23(2) . . ? F3A C1 F1A 108.5(7) . . ? F1B C1 F1A 131.2(10) . . ? F3B C1 F2A 81.7(19) . . ? F3A C1 F2A 110.9(6) . . ? F1B C1 F2A 42.4(11) . . ? F1A C1 F2A 104.3(6) . . ? F3B C1 F2B 106(2) . . ? F3A C1 F2B 23(2) . . ? F1B C1 F2B 92(2) . . ? F1A C1 F2B 88.4(19) . . ? F2A C1 F2B 128.1(18) . . ? F3B C1 C2 117.7(14) . . ? F3A C1 C2 111.1(5) . . ? F1B C1 C2 112.4(9) . . ? F1A C1 C2 112.7(5) . . ? F2A C1 C2 109.3(5) . . ? F2B C1 C2 111.4(15) . . ? O1 C2 C3 127.3(4) . . ? O1 C2 C1 114.3(4) . . ? C3 C2 C1 118.4(4) . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? O2 C4 C3 127.9(4) . . ? O2 C4 C5 114.7(4) . . ? C3 C4 C5 117.4(4) . . ? F5 C5 F4 106.4(3) . . ? F5 C5 C6 108.8(4) . . ? F4 C5 C6 103.9(4) . . ? F5 C5 C4 110.4(3) . . ? F4 C5 C4 110.5(4) . . ? C6 C5 C4 116.2(4) . . ? F7 C6 F6 107.1(4) . . ? F7 C6 C7 108.4(4) . . ? F6 C6 C7 105.8(5) . . ? F7 C6 C5 108.8(4) . . ? F6 C6 C5 108.7(4) . . ? C7 C6 C5 117.5(4) . . ? F8A C7 F9A 111.3(6) . . ? F8A C7 F10A 109.5(5) . . ? F9A C7 F10A 105.5(5) . . ? F8A C7 C6 109.0(6) . . ? F9A C7 C6 111.8(5) . . ? F10A C7 C6 109.6(5) . . ? F13A C8 F11A 106.7(4) . . ? F13A C8 F12A 108.6(4) . . ? F11A C8 F12A 104.5(4) . . ? F13A C8 C9 114.1(4) . . ? F11A C8 C9 111.5(4) . . ? F12A C8 C9 111.0(4) . . ? O3 C9 C10 128.1(4) . . ? O3 C9 C8 113.5(4) . . ? C10 C9 C8 118.4(4) . . ? C9 C10 C11 121.7(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? O4 C11 C10 126.9(4) . . ? O4 C11 C12 115.2(4) . . ? C10 C11 C12 117.9(4) . . ? F14 C12 F15 108.2(4) . . ? F14 C12 C11 110.6(4) . . ? F15 C12 C11 109.8(4) . . ? F14 C12 C13 108.3(4) . . ? F15 C12 C13 107.2(4) . . ? C11 C12 C13 112.6(4) . . ? F16 C13 F17 108.1(5) . . ? F16 C13 C14 108.4(5) . . ? F17 C13 C14 107.4(4) . . ? F16 C13 C12 108.8(4) . . ? F17 C13 C12 108.0(4) . . ? C14 C13 C12 115.9(5) . . ? F20 C14 F19 108.0(6) . . ? F20 C14 F18 108.6(6) . . ? F19 C14 F18 108.9(6) . . ? F20 C14 C13 110.8(5) . . ? F19 C14 C13 110.0(5) . . ? F18 C14 C13 110.5(5) . . ? F23A C15 F22A 107.7(6) . . ? F23A C15 F21A 106.3(7) . . ? F22A C15 F21A 106.8(6) . . ? F23A C15 C16 112.5(5) . . ? F22A C15 C16 112.7(5) . . ? F21A C15 C16 110.5(6) . . ? O5 C16 C17 128.6(4) . . ? O5 C16 C15 112.4(5) . . ? C17 C16 C15 119.1(5) . . ? C16 C17 C18 121.0(4) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? O6 C18 C17 127.1(5) . . ? O6 C18 C19 115.2(5) . . ? C17 C18 C19 117.7(5) . . ? F25 C19 F24 108.0(5) . . ? F25 C19 C20 107.3(5) . . ? F24 C19 C20 105.7(5) . . ? F25 C19 C18 110.9(5) . . ? F24 C19 C18 109.8(4) . . ? C20 C19 C18 114.9(4) . . ? F27 C20 F26 104.5(6) . . ? F27 C20 C19 108.5(6) . . ? F26 C20 C19 108.6(5) . . ? F27 C20 C21 107.3(5) . . ? F26 C20 C21 108.0(6) . . ? C19 C20 C21 119.1(5) . . ? F28B C21 F28A 34.5(12) . . ? F28B C21 F29B 116.1(16) . . ? F28A C21 F29B 130.3(12) . . ? F28B C21 F30B 105.5(15) . . ? F28A C21 F30B 71.1(11) . . ? F29B C21 F30B 107.8(13) . . ? F28B C21 F30A 140.7(13) . . ? F28A C21 F30A 108.0(10) . . ? F29B C21 F30A 75.8(11) . . ? F30B C21 F30A 38.5(10) . . ? F28B C21 F29A 82.3(13) . . ? F28A C21 F29A 106.1(9) . . ? F29B C21 F29A 35.2(9) . . ? F30B C21 F29A 129.6(11) . . ? F30A C21 F29A 108.3(10) . . ? F28B C21 C20 104.0(11) . . ? F28A C21 C20 115.5(8) . . ? F29B C21 C20 110.1(10) . . ? F30B C21 C20 113.4(10) . . ? F30A C21 C20 106.1(8) . . ? F29A C21 C20 112.5(7) . . ? C22A N1A C26A 120.0(9) . . ? C22A N1A Yb1 122.8(6) . . ? C26A N1A Yb1 116.6(6) . . ? C28A N2A C27A 115.0(9) . . ? C28A N2A Yb1 122.2(7) . . ? C27A N2A Yb1 121.8(6) . . ? N1A C26A C25A 119.5(9) . . ? N1A C26A C27A 120.0(7) . . ? C25A C26A C27A 120.6(8) . . ? N2A C27A C31A 125.1(9) . . ? N2A C27A C26A 113.6(7) . . ? C31A C27A C26A 121.3(8) . . ? N2A C28A C29A 124.5(10) . . ? N2A C28A H28A 117.7 . . ? C29A C28A H28A 117.7 . . ? N1A C22A C23A 121.9(9) . . ? N1A C22A H22A 119.1 . . ? C23A C22A H22A 119.1 . . ? C24A C23A C22A 119.5(9) . . ? C24A C23A H23A 120.2 . . ? C22A C23A H23A 120.2 . . ? C23A C24A C25A 119.9(9) . . ? C23A C24A H24A 120.1 . . ? C25A C24A H24A 120.1 . . ? C24A C25A C33A 122.7(9) . . ? C24A C25A C26A 119.2(8) . . ? C33A C25A C26A 118.0(10) . . ? C30A C29A C28A 118.2(9) . . ? C30A C29A H29A 120.9 . . ? C28A C29A H29A 120.9 . . ? C29A C30A C31A 121.3(9) . . ? C29A C30A H30A 119.3 . . ? C31A C30A H30A 119.3 . . ? C30A C31A C27A 115.9(8) . . ? C30A C31A C32A 127.0(8) . . ? C27A C31A C32A 117.1(9) . . ? C33A C32A C31A 121.2(9) . . ? C33A C32A N3A 113.8(10) . . ? C31A C32A N3A 124.9(10) . . ? C32A C33A C25A 121.7(9) . . ? C32A C33A H33A 119.1 . . ? C25A C33A H33A 119.1 . . ? O7A N3A O8A 122.8(11) . . ? O7A N3A C32A 116.6(9) . . ? O8A N3A C32A 120.6(12) . . ? C22B N1B C26B 119.1(11) . . ? C22B N1B Yb1 120.4(8) . . ? C26B N1B Yb1 120.0(8) . . ? C28B N2B C27B 118.7(11) . . ? C28B N2B Yb1 121.2(9) . . ? C27B N2B Yb1 119.3(7) . . ? N1B C26B C27B 117.7(11) . . ? N1B C26B C25B 119.5(11) . . ? C27B C26B C25B 122.8(10) . . ? N2B C27B C31B 123.2(10) . . ? N2B C27B C26B 117.4(10) . . ? C31B C27B C26B 119.4(11) . . ? N2B C28B C29B 123.6(11) . . ? N2B C28B H28B 118.2 . . ? C29B C28B H28B 118.2 . . ? N1B C22B C23B 124.1(11) . . ? N1B C22B H22B 118.0 . . ? C23B C22B H22B 118.0 . . ? C24B C23B C22B 117.0(11) . . ? C24B C23B H23B 121.5 . . ? C22B C23B H23B 121.5 . . ? C23B C24B C25B 121.6(11) . . ? C23B C24B H24B 119.2 . . ? C25B C24B H24B 119.2 . . ? C33B C25B C24B 126.7(10) . . ? C33B C25B C26B 114.6(11) . . ? C24B C25B C26B 118.7(10) . . ? C30B C29B C28B 116.8(11) . . ? C30B C29B H29B 121.6 . . ? C28B C29B H29B 121.6 . . ? C31B C30B C29B 121.0(11) . . ? C31B C30B H30B 119.5 . . ? C29B C30B H30B 119.5 . . ? C30B C31B C27B 116.5(10) . . ? C30B C31B C32B 124.5(11) . . ? C27B C31B C32B 118.9(11) . . ? C33B C32B C31B 119.8(11) . . ? C33B C32B H32B 120.1 . . ? C31B C32B H32B 120.1 . . ? C25B C33B C32B 124.3(12) . . ? C25B C33B N3B 123.9(12) . . ? C32B C33B N3B 111.8(11) . . ? O7B N3B O8B 129.4(12) . . ? O7B N3B C33B 114.8(9) . . ? O8B N3B C33B 115.8(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Yb1 O1 C2 -42.2(4) . . . . ? O3 Yb1 O1 C2 -166.0(4) . . . . ? O5 Yb1 O1 C2 -91.4(4) . . . . ? O2 Yb1 O1 C2 -8.5(4) . . . . ? O4 Yb1 O1 C2 145.4(3) . . . . ? N2A Yb1 O1 C2 108.3(4) . . . . ? N1A Yb1 O1 C2 52.8(4) . . . . ? N1B Yb1 O1 C2 63.5(4) . . . . ? N2B Yb1 O1 C2 116.5(5) . . . . ? O6 Yb1 O2 C4 164.3(4) . . . . ? O1 Yb1 O2 C4 3.2(4) . . . . ? O3 Yb1 O2 C4 43.5(4) . . . . ? O5 Yb1 O2 C4 88.4(4) . . . . ? O4 Yb1 O2 C4 -150.5(3) . . . . ? N2A Yb1 O2 C4 -63.6(5) . . . . ? N1A Yb1 O2 C4 -117.3(4) . . . . ? N1B Yb1 O2 C4 -109.2(5) . . . . ? N2B Yb1 O2 C4 -55.1(5) . . . . ? O6 Yb1 O3 C9 60.8(4) . . . . ? O1 Yb1 O3 C9 -151.7(4) . . . . ? O5 Yb1 O3 C9 122.6(4) . . . . ? O2 Yb1 O3 C9 169.2(3) . . . . ? O4 Yb1 O3 C9 -1.6(4) . . . . ? N2A Yb1 O3 C9 -75.6(5) . . . . ? N1A Yb1 O3 C9 -40.8(6) . . . . ? N1B Yb1 O3 C9 -47.8(6) . . . . ? N2B Yb1 O3 C9 -79.3(5) . . . . ? O6 Yb1 O4 C11 -127.5(4) . . . . ? O1 Yb1 O4 C11 48.1(4) . . . . ? O3 Yb1 O4 C11 -1.8(4) . . . . ? O5 Yb1 O4 C11 -64.1(4) . . . . ? O2 Yb1 O4 C11 -173.4(3) . . . . ? N2A Yb1 O4 C11 85.7(4) . . . . ? N1A Yb1 O4 C11 154.2(4) . . . . ? N1B Yb1 O4 C11 143.5(5) . . . . ? N2B Yb1 O4 C11 76.3(4) . . . . ? O6 Yb1 O5 C16 7.6(4) . . . . ? O1 Yb1 O5 C16 161.0(4) . . . . ? O3 Yb1 O5 C16 -118.4(4) . . . . ? O2 Yb1 O5 C16 86.8(4) . . . . ? O4 Yb1 O5 C16 -55.7(4) . . . . ? N2A Yb1 O5 C16 -157.6(6) . . . . ? N1A Yb1 O5 C16 44.5(6) . . . . ? N1B Yb1 O5 C16 45.5(8) . . . . ? N2B Yb1 O5 C16 -153.8(6) . . . . ? O1 Yb1 O6 C18 -57.7(4) . . . . ? O3 Yb1 O6 C18 54.9(4) . . . . ? O5 Yb1 O6 C18 -6.5(4) . . . . ? O2 Yb1 O6 C18 -90.7(4) . . . . ? O4 Yb1 O6 C18 117.3(4) . . . . ? N2A Yb1 O6 C18 163.5(5) . . . . ? N1A Yb1 O6 C18 -164.3(4) . . . . ? N1B Yb1 O6 C18 -170.5(5) . . . . ? N2B Yb1 O6 C18 155.2(5) . . . . ? Yb1 O1 C2 C3 9.9(7) . . . . ? Yb1 O1 C2 C1 -170.1(3) . . . . ? F3B C1 C2 O1 148(2) . . . . ? F3A C1 C2 O1 -65.2(7) . . . . ? F1B C1 C2 O1 12.1(14) . . . . ? F1A C1 C2 O1 172.9(5) . . . . ? F2A C1 C2 O1 57.5(6) . . . . ? F2B C1 C2 O1 -90(2) . . . . ? F3B C1 C2 C3 -32(2) . . . . ? F3A C1 C2 C3 114.9(6) . . . . ? F1B C1 C2 C3 -167.9(14) . . . . ? F1A C1 C2 C3 -7.1(7) . . . . ? F2A C1 C2 C3 -122.5(5) . . . . ? F2B C1 C2 C3 90(2) . . . . ? O1 C2 C3 C4 -2.1(7) . . . . ? C1 C2 C3 C4 177.8(4) . . . . ? Yb1 O2 C4 C3 1.0(7) . . . . ? Yb1 O2 C4 C5 -178.8(3) . . . . ? C2 C3 C4 O2 -3.2(7) . . . . ? C2 C3 C4 C5 176.5(4) . . . . ? O2 C4 C5 F5 -24.9(5) . . . . ? C3 C4 C5 F5 155.3(4) . . . . ? O2 C4 C5 F4 -142.4(4) . . . . ? C3 C4 C5 F4 37.9(5) . . . . ? O2 C4 C5 C6 99.5(5) . . . . ? C3 C4 C5 C6 -80.2(5) . . . . ? F5 C5 C6 F7 -54.9(5) . . . . ? F4 C5 C6 F7 58.2(5) . . . . ? C4 C5 C6 F7 179.8(4) . . . . ? F5 C5 C6 F6 -171.2(3) . . . . ? F4 C5 C6 F6 -58.1(4) . . . . ? C4 C5 C6 F6 63.5(5) . . . . ? F5 C5 C6 C7 68.7(6) . . . . ? F4 C5 C6 C7 -178.2(5) . . . . ? C4 C5 C6 C7 -56.6(6) . . . . ? F7 C6 C7 F8A 63.4(6) . . . . ? F6 C6 C7 F8A 178.0(5) . . . . ? C5 C6 C7 F8A -60.4(7) . . . . ? F7 C6 C7 F9A -60.1(7) . . . . ? F6 C6 C7 F9A 54.5(6) . . . . ? C5 C6 C7 F9A 176.1(5) . . . . ? F7 C6 C7 F10A -176.8(5) . . . . ? F6 C6 C7 F10A -62.2(6) . . . . ? C5 C6 C7 F10A 59.4(7) . . . . ? Yb1 O3 C9 C10 4.2(7) . . . . ? Yb1 O3 C9 C8 -177.9(3) . . . . ? F13A C8 C9 O3 174.7(4) . . . . ? F11A C8 C9 O3 -64.3(5) . . . . ? F12A C8 C9 O3 51.8(5) . . . . ? F13A C8 C9 C10 -7.2(7) . . . . ? F11A C8 C9 C10 113.8(5) . . . . ? F12A C8 C9 C10 -130.2(5) . . . . ? O3 C9 C10 C11 -3.3(8) . . . . ? C8 C9 C10 C11 179.0(4) . . . . ? Yb1 O4 C11 C10 2.9(7) . . . . ? Yb1 O4 C11 C12 -175.9(3) . . . . ? C9 C10 C11 O4 -0.3(7) . . . . ? C9 C10 C11 C12 178.4(4) . . . . ? O4 C11 C12 F14 -157.6(4) . . . . ? C10 C11 C12 F14 23.5(6) . . . . ? O4 C11 C12 F15 -38.3(5) . . . . ? C10 C11 C12 F15 142.9(4) . . . . ? O4 C11 C12 C13 81.1(5) . . . . ? C10 C11 C12 C13 -97.8(5) . . . . ? F14 C12 C13 F16 -78.9(5) . . . . ? F15 C12 C13 F16 164.6(4) . . . . ? C11 C12 C13 F16 43.7(5) . . . . ? F14 C12 C13 F17 163.9(4) . . . . ? F15 C12 C13 F17 47.4(5) . . . . ? C11 C12 C13 F17 -73.4(5) . . . . ? F14 C12 C13 C14 43.5(6) . . . . ? F15 C12 C13 C14 -73.0(5) . . . . ? C11 C12 C13 C14 166.1(4) . . . . ? F16 C13 C14 F20 172.3(5) . . . . ? F17 C13 C14 F20 -71.1(6) . . . . ? C12 C13 C14 F20 49.7(7) . . . . ? F16 C13 C14 F19 -68.4(7) . . . . ? F17 C13 C14 F19 48.2(7) . . . . ? C12 C13 C14 F19 169.0(5) . . . . ? F16 C13 C14 F18 51.9(7) . . . . ? F17 C13 C14 F18 168.5(6) . . . . ? C12 C13 C14 F18 -70.7(7) . . . . ? Yb1 O5 C16 C17 -7.6(8) . . . . ? Yb1 O5 C16 C15 172.3(4) . . . . ? F23A C15 C16 O5 61.2(7) . . . . ? F22A C15 C16 O5 -60.8(8) . . . . ? F21A C15 C16 O5 179.9(6) . . . . ? F23A C15 C16 C17 -118.9(7) . . . . ? F22A C15 C16 C17 119.1(6) . . . . ? F21A C15 C16 C17 -0.2(9) . . . . ? O5 C16 C17 C18 1.9(8) . . . . ? C15 C16 C17 C18 -178.0(5) . . . . ? Yb1 O6 C18 C17 5.0(7) . . . . ? Yb1 O6 C18 C19 -176.9(3) . . . . ? C16 C17 C18 O6 -0.5(8) . . . . ? C16 C17 C18 C19 -178.5(4) . . . . ? O6 C18 C19 F25 150.7(5) . . . . ? C17 C18 C19 F25 -31.0(7) . . . . ? O6 C18 C19 F24 31.4(6) . . . . ? C17 C18 C19 F24 -150.3(5) . . . . ? O6 C18 C19 C20 -87.5(6) . . . . ? C17 C18 C19 C20 90.8(6) . . . . ? F25 C19 C20 F27 73.6(7) . . . . ? F24 C19 C20 F27 -171.3(5) . . . . ? C18 C19 C20 F27 -50.1(7) . . . . ? F25 C19 C20 F26 -173.4(6) . . . . ? F24 C19 C20 F26 -58.3(7) . . . . ? C18 C19 C20 F26 62.9(8) . . . . ? F25 C19 C20 C21 -49.3(8) . . . . ? F24 C19 C20 C21 65.7(7) . . . . ? C18 C19 C20 C21 -173.1(5) . . . . ? F27 C20 C21 F28B 166.8(14) . . . . ? F26 C20 C21 F28B 54.7(15) . . . . ? C19 C20 C21 F28B -69.6(15) . . . . ? F27 C20 C21 F28A -158.4(10) . . . . ? F26 C20 C21 F28A 89.4(11) . . . . ? C19 C20 C21 F28A -34.9(11) . . . . ? F27 C20 C21 F29B 41.7(13) . . . . ? F26 C20 C21 F29B -70.4(13) . . . . ? C19 C20 C21 F29B 165.3(12) . . . . ? F27 C20 C21 F30B -79.1(14) . . . . ? F26 C20 C21 F30B 168.8(13) . . . . ? C19 C20 C21 F30B 44.5(14) . . . . ? F27 C20 C21 F30A -38.7(11) . . . . ? F26 C20 C21 F30A -150.8(10) . . . . ? C19 C20 C21 F30A 84.8(10) . . . . ? F27 C20 C21 F29A 79.5(9) . . . . ? F26 C20 C21 F29A -32.6(10) . . . . ? C19 C20 C21 F29A -156.9(8) . . . . ? O6 Yb1 N1A C22A 29.2(8) . . . . ? O1 Yb1 N1A C22A -114.7(8) . . . . ? O3 Yb1 N1A C22A 145.6(6) . . . . ? O5 Yb1 N1A C22A -7.5(10) . . . . ? O2 Yb1 N1A C22A -52.2(8) . . . . ? O4 Yb1 N1A C22A 106.7(8) . . . . ? N2A Yb1 N1A C22A -175.8(9) . . . . ? N1B Yb1 N1A C22A 175(3) . . . . ? N2B Yb1 N1A C22A -175.9(9) . . . . ? O6 Yb1 N1A C26A -142.2(7) . . . . ? O1 Yb1 N1A C26A 73.9(7) . . . . ? O3 Yb1 N1A C26A -25.8(9) . . . . ? O5 Yb1 N1A C26A -178.9(5) . . . . ? O2 Yb1 N1A C26A 136.4(7) . . . . ? O4 Yb1 N1A C26A -64.7(7) . . . . ? N2A Yb1 N1A C26A 12.8(7) . . . . ? N1B Yb1 N1A C26A 4(2) . . . . ? N2B Yb1 N1A C26A 12.7(7) . . . . ? O6 Yb1 N2A C28A -147.7(9) . . . . ? O1 Yb1 N2A C28A 55.2(10) . . . . ? O3 Yb1 N2A C28A -25.2(10) . . . . ? O5 Yb1 N2A C28A 12.4(14) . . . . ? O2 Yb1 N2A C28A 120.8(10) . . . . ? O4 Yb1 N2A C28A -100.9(10) . . . . ? N1A Yb1 N2A C28A 177.9(11) . . . . ? N1B Yb1 N2A C28A 180.0(12) . . . . ? N2B Yb1 N2A C28A -2(3) . . . . ? O6 Yb1 N2A C27A 20.3(10) . . . . ? O1 Yb1 N2A C27A -136.8(9) . . . . ? O3 Yb1 N2A C27A 142.8(8) . . . . ? O5 Yb1 N2A C27A -179.6(5) . . . . ? O2 Yb1 N2A C27A -71.2(9) . . . . ? O4 Yb1 N2A C27A 67.1(8) . . . . ? N1A Yb1 N2A C27A -14.1(7) . . . . ? N1B Yb1 N2A C27A -12.0(7) . . . . ? N2B Yb1 N2A C27A 166(4) . . . . ? C22A N1A C26A C25A -2.5(13) . . . . ? Yb1 N1A C26A C25A 169.2(6) . . . . ? C22A N1A C26A C27A 176.6(8) . . . . ? Yb1 N1A C26A C27A -11.7(10) . . . . ? C28A N2A C27A C31A 0.8(15) . . . . ? Yb1 N2A C27A C31A -168.0(6) . . . . ? C28A N2A C27A C26A -177.6(9) . . . . ? Yb1 N2A C27A C26A 13.5(11) . . . . ? N1A C26A C27A N2A -0.5(12) . . . . ? C25A C26A C27A N2A 178.5(8) . . . . ? N1A C26A C27A C31A -179.0(8) . . . . ? C25A C26A C27A C31A 0.0(11) . . . . ? C27A N2A C28A C29A -1.5(17) . . . . ? Yb1 N2A C28A C29A 167.2(9) . . . . ? C26A N1A C22A C23A 3.0(14) . . . . ? Yb1 N1A C22A C23A -168.2(7) . . . . ? N1A C22A C23A C24A -1.4(14) . . . . ? C22A C23A C24A C25A -0.5(14) . . . . ? C23A C24A C25A C33A -177.6(9) . . . . ? C23A C24A C25A C26A 0.9(14) . . . . ? N1A C26A C25A C24A 0.6(12) . . . . ? C27A C26A C25A C24A -178.5(8) . . . . ? N1A C26A C25A C33A 179.2(8) . . . . ? C27A C26A C25A C33A 0.1(11) . . . . ? N2A C28A C29A C30A 0.9(17) . . . . ? C28A C29A C30A C31A 0.5(15) . . . . ? C29A C30A C31A C27A -1.2(13) . . . . ? C29A C30A C31A C32A 179.7(9) . . . . ? N2A C27A C31A C30A 0.5(13) . . . . ? C26A C27A C31A C30A 178.8(8) . . . . ? N2A C27A C31A C32A 179.7(9) . . . . ? C26A C27A C31A C32A -1.9(12) . . . . ? C30A C31A C32A C33A -177.0(9) . . . . ? C27A C31A C32A C33A 3.8(14) . . . . ? C30A C31A C32A N3A -0.2(16) . . . . ? C27A C31A C32A N3A -179.3(9) . . . . ? C31A C32A C33A C25A -3.9(15) . . . . ? N3A C32A C33A C25A 179.0(8) . . . . ? C24A C25A C33A C32A -179.6(10) . . . . ? C26A C25A C33A C32A 1.8(13) . . . . ? C33A C32A N3A O7A 177.9(9) . . . . ? C31A C32A N3A O7A 0.8(15) . . . . ? C33A C32A N3A O8A -1.5(16) . . . . ? C31A C32A N3A O8A -178.5(12) . . . . ? O6 Yb1 N1B C22B 25.0(10) . . . . ? O1 Yb1 N1B C22B -121.4(9) . . . . ? O3 Yb1 N1B C22B 147.7(8) . . . . ? O5 Yb1 N1B C22B -11.5(15) . . . . ? O2 Yb1 N1B C22B -53.2(9) . . . . ? O4 Yb1 N1B C22B 100.5(10) . . . . ? N2A Yb1 N1B C22B -177.9(12) . . . . ? N1A Yb1 N1B C22B -8.2(18) . . . . ? N2B Yb1 N1B C22B -178.3(11) . . . . ? O6 Yb1 N1B C26B -146.3(9) . . . . ? O1 Yb1 N1B C26B 67.3(9) . . . . ? O3 Yb1 N1B C26B -23.6(11) . . . . ? O5 Yb1 N1B C26B 177.2(6) . . . . ? O2 Yb1 N1B C26B 135.5(9) . . . . ? O4 Yb1 N1B C26B -70.7(9) . . . . ? N2A Yb1 N1B C26B 10.9(8) . . . . ? N1A Yb1 N1B C26B -179(3) . . . . ? N2B Yb1 N1B C26B 10.4(9) . . . . ? O6 Yb1 N2B C28B -142.1(10) . . . . ? O1 Yb1 N2B C28B 57.2(12) . . . . ? O3 Yb1 N2B C28B -26.4(11) . . . . ? O5 Yb1 N2B C28B 8.8(15) . . . . ? O2 Yb1 N2B C28B 117.0(12) . . . . ? O4 Yb1 N2B C28B -104.1(12) . . . . ? N2A Yb1 N2B C28B 177(4) . . . . ? N1A Yb1 N2B C28B 177.4(13) . . . . ? N1B Yb1 N2B C28B 179.3(14) . . . . ? O6 Yb1 N2B C27B 27.2(13) . . . . ? O1 Yb1 N2B C27B -133.5(10) . . . . ? O3 Yb1 N2B C27B 142.9(10) . . . . ? O5 Yb1 N2B C27B 178.1(7) . . . . ? O2 Yb1 N2B C27B -73.7(10) . . . . ? O4 Yb1 N2B C27B 65.2(10) . . . . ? N2A Yb1 N2B C27B -14(3) . . . . ? N1A Yb1 N2B C27B -13.3(9) . . . . ? N1B Yb1 N2B C27B -11.4(9) . . . . ? C22B N1B C26B C27B 179.2(11) . . . . ? Yb1 N1B C26B C27B -9.5(14) . . . . ? C22B N1B C26B C25B -0.2(17) . . . . ? Yb1 N1B C26B C25B 171.2(7) . . . . ? C28B N2B C27B C31B 0(2) . . . . ? Yb1 N2B C27B C31B -169.8(8) . . . . ? C28B N2B C27B C26B -179.0(12) . . . . ? Yb1 N2B C27B C26B 11.4(15) . . . . ? N1B C26B C27B N2B -1.5(16) . . . . ? C25B C26B C27B N2B 177.8(11) . . . . ? N1B C26B C27B C31B 179.7(10) . . . . ? C25B C26B C27B C31B -1.0(16) . . . . ? C27B N2B C28B C29B 1(2) . . . . ? Yb1 N2B C28B C29B 170.8(10) . . . . ? C26B N1B C22B C23B 0.5(19) . . . . ? Yb1 N1B C22B C23B -170.9(9) . . . . ? N1B C22B C23B C24B 0.8(19) . . . . ? C22B C23B C24B C25B -2.4(17) . . . . ? C23B C24B C25B C33B -178.4(12) . . . . ? C23B C24B C25B C26B 2.7(15) . . . . ? N1B C26B C25B C33B 179.6(11) . . . . ? C27B C26B C25B C33B 0.3(15) . . . . ? N1B C26B C25B C24B -1.3(15) . . . . ? C27B C26B C25B C24B 179.4(10) . . . . ? N2B C28B C29B C30B -3(2) . . . . ? C28B C29B C30B C31B 3.9(18) . . . . ? C29B C30B C31B C27B -2.9(17) . . . . ? C29B C30B C31B C32B 178.7(10) . . . . ? N2B C27B C31B C30B 1.0(18) . . . . ? C26B C27B C31B C30B 179.7(10) . . . . ? N2B C27B C31B C32B 179.5(11) . . . . ? C26B C27B C31B C32B -1.8(16) . . . . ? C30B C31B C32B C33B -176.3(12) . . . . ? C27B C31B C32B C33B 5.4(16) . . . . ? C24B C25B C33B C32B -175.5(12) . . . . ? C26B C25B C33B C32B 3.5(19) . . . . ? C24B C25B C33B N3B 1(2) . . . . ? C26B C25B C33B N3B -179.6(11) . . . . ? C31B C32B C33B C25B -6(2) . . . . ? C31B C32B C33B N3B 176.3(9) . . . . ? C25B C33B N3B O7B 28.6(18) . . . . ? C32B C33B N3B O7B -154.1(11) . . . . ? C25B C33B N3B O8B -154.8(17) . . . . ? C32B C33B N3B O8B 22(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.276 _refine_diff_density_min -1.484 _refine_diff_density_rms 0.112 _database_code_depnum_ccdc_archive 'CCDC 933187' ####################################################################### # # 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_ybtfac _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris(1,1,1-trifluoro-2,4-pentanedionate)mono(5-nitro-1,10-phenanthroline)ytterbium(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H19 F9 N3 O8 Yb' _chemical_formula_sum 'C27 H19 F9 N3 O8 Yb' _chemical_formula_weight 857.49 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' Yb Yb -0.3850 5.5486 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7806(16) _cell_length_b 14.750(2) _cell_length_c 23.952(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.101(5) _cell_angle_gamma 90.00 _cell_volume 3154.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5707 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 20.1 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 3.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2000)' _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56609 _diffrn_reflns_av_R_equivalents 0.1109 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 26.28 _reflns_number_total 6096 _reflns_number_gt 3130 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material SHELXL-97 _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^)+(0.1243P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6096 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1434 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.2096 _refine_ls_wR_factor_gt 0.1618 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _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 0.81305(6) 0.31215(3) 0.35733(2) 0.0656(2) Uani 1 1 d . . . F6 F 0.5874(17) 0.1561(10) 0.4768(6) 0.189(6) Uani 1 1 d . . . O6 O 0.9284(11) 0.1765(6) 0.3624(4) 0.088(3) Uani 1 1 d . . . O2 O 0.5734(10) 0.3317(5) 0.2896(4) 0.080(2) Uani 1 1 d . . . N2 N 0.8270(10) 0.4686(6) 0.3170(4) 0.065(2) Uani 1 1 d . . . O4 O 0.9725(10) 0.2961(6) 0.4561(4) 0.089(3) Uani 1 1 d . . . O5 O 0.6755(10) 0.2138(7) 0.3874(4) 0.089(2) Uani 1 1 d . . . N1 N 1.0689(11) 0.3620(7) 0.3653(4) 0.073(3) Uani 1 1 d . . . O1 O 0.8147(10) 0.2933(5) 0.2616(4) 0.081(2) Uani 1 1 d . . . O3 O 0.7330(9) 0.4101(5) 0.4119(3) 0.074(2) Uani 1 1 d . . . C12 C 0.7097(13) 0.5218(8) 0.2921(5) 0.067(3) Uani 1 1 d . . . H12 H 0.6255 0.5077 0.2992 0.080 Uiso 1 1 calc R . . C11 C 0.7009(13) 0.5982(8) 0.2557(6) 0.076(3) Uani 1 1 d . . . H11 H 0.6128 0.6314 0.2383 0.091 Uiso 1 1 calc R . . C26 C 0.720(2) 0.3180(9) 0.2100(7) 0.096(5) Uani 1 1 d . . . C3 C 1.3411(12) 0.4071(10) 0.3593(5) 0.082(4) Uani 1 1 d . . . H3 H 1.4322 0.4209 0.3577 0.098 Uiso 1 1 calc R . . C10 C 0.8240(13) 0.6221(9) 0.2466(6) 0.080(3) Uani 1 1 d . . . H10 H 0.8220 0.6732 0.2235 0.097 Uiso 1 1 calc R . . C4 C 1.2159(13) 0.4631(9) 0.3319(5) 0.077(3) Uani 1 1 d . . . C1 C 1.1864(15) 0.3112(9) 0.3922(6) 0.085(4) Uani 1 1 d . . . H1 H 1.1794 0.2607 0.4142 0.102 Uiso 1 1 calc R . . O8 O 1.4555(12) 0.5849(9) 0.3428(6) 0.140(4) Uani 1 1 d . . . C20 C 0.8315(19) 0.0808(10) 0.4131(6) 0.104(5) Uani 1 1 d . . . H20 H 0.8435 0.0247 0.4322 0.125 Uiso 1 1 calc R . . C8 C 0.9533(13) 0.5700(8) 0.2721(5) 0.067(3) Uani 1 1 d . . . N3 N 1.3495(14) 0.5749(9) 0.2943(7) 0.103(4) Uani 1 1 d . . . C7 C 1.0859(13) 0.5933(9) 0.2668(6) 0.084(4) Uani 1 1 d . . . H7 H 1.0892 0.6423 0.2429 0.100 Uiso 1 1 calc R . . C13 C 0.6785(18) 0.4987(11) 0.4816(7) 0.122(6) Uani 1 1 d . . . H13A H 0.6550 0.5471 0.4524 0.184 Uiso 1 1 calc R . . H13B H 0.7346 0.5221 0.5219 0.184 Uiso 1 1 calc R . . H13C H 0.5874 0.4718 0.4798 0.184 Uiso 1 1 calc R . . C9 C 0.9498(11) 0.4939(7) 0.3074(5) 0.062(3) Uani 1 1 d . . . C6 C 1.2079(14) 0.5433(9) 0.2969(6) 0.086(4) Uani 1 1 d . . . C16 C 0.9674(16) 0.3240(9) 0.5047(5) 0.083(4) Uani 1 1 d . . . C23 C 0.3412(16) 0.3551(12) 0.2064(8) 0.126(6) Uani 1 1 d . . . H23A H 0.2951 0.3085 0.2208 0.189 Uiso 1 1 calc R . . H23B H 0.3017 0.3532 0.1625 0.189 Uiso 1 1 calc R . . H23C H 0.3206 0.4133 0.2192 0.189 Uiso 1 1 calc R . . C19 C 0.9324(15) 0.1035(12) 0.3901(6) 0.089(4) Uani 1 1 d . . . C2 C 1.3235(15) 0.3306(9) 0.3889(7) 0.085(4) Uani 1 1 d . . . H2 H 1.4038 0.2911 0.4069 0.102 Uiso 1 1 calc R . . F9 F 0.777(2) 0.2418(10) 0.1364(7) 0.221(8) Uani 1 1 d . . . C5 C 1.0795(11) 0.4385(8) 0.3358(5) 0.062(3) Uani 1 1 d . . . F8 F 0.7274(17) 0.3775(10) 0.1186(5) 0.201(6) Uani 1 1 d . . . C14 C 0.7686(14) 0.4293(9) 0.4672(5) 0.078(3) Uani 1 1 d . . . O7 O 1.3515(11) 0.5946(9) 0.2468(6) 0.144(5) Uani 1 1 d . . . C22 C 0.595(2) 0.1017(13) 0.4357(9) 0.118(6) Uani 1 1 d . . . C15 C 0.8761(17) 0.3852(11) 0.5142(6) 0.105(5) Uani 1 1 d . . . H15 H 0.8875 0.3973 0.5540 0.126 Uiso 1 1 calc R . . C21 C 0.7127(18) 0.1332(10) 0.4107(6) 0.092(4) Uani 1 1 d . . . F5 F 0.4569(13) 0.1029(10) 0.3945(6) 0.187(6) Uani 1 1 d . . . F4 F 0.6256(15) 0.0214(9) 0.4612(7) 0.209(6) Uani 1 1 d . . . F7 F 0.9270(19) 0.3377(14) 0.1842(7) 0.231(8) Uani 1 1 d . . . C24 C 0.5041(16) 0.3404(9) 0.2318(6) 0.083(4) Uani 1 1 d . . . C18 C 1.0578(18) 0.0402(11) 0.3980(8) 0.132(6) Uani 1 1 d . . . H18A H 1.0184 -0.0194 0.3847 0.198 Uiso 1 1 calc R . . H18B H 1.1259 0.0382 0.4404 0.198 Uiso 1 1 calc R . . H18C H 1.1099 0.0610 0.3741 0.198 Uiso 1 1 calc R . . C25 C 0.5792(18) 0.3398(10) 0.1921(6) 0.094(4) Uani 1 1 d . . . H25 H 0.5254 0.3558 0.1514 0.113 Uiso 1 1 calc R . . C27 C 0.783(3) 0.3208(16) 0.1617(8) 0.131(7) Uani 1 1 d . . . F1 F 1.060(2) 0.1939(11) 0.5640(8) 0.266(11) Uani 1 1 d . . . F2 F 1.109(2) 0.3112(11) 0.6122(5) 0.247(9) Uani 1 1 d . . . F3 F 1.2129(16) 0.2761(17) 0.5604(7) 0.274(12) Uani 1 1 d . . . C17 C 1.087(3) 0.2774(15) 0.5594(7) 0.125(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.0755(4) 0.0698(4) 0.0500(3) 0.0004(2) 0.0241(2) 0.0054(3) F6 0.242(15) 0.235(14) 0.136(10) -0.015(10) 0.123(11) -0.050(12) O6 0.120(7) 0.080(6) 0.066(5) 0.004(5) 0.041(5) 0.010(5) O2 0.107(6) 0.067(5) 0.065(5) 0.000(4) 0.034(5) -0.002(4) N2 0.065(6) 0.065(6) 0.067(5) -0.006(5) 0.028(5) 0.000(5) O4 0.099(6) 0.105(7) 0.056(5) 0.010(4) 0.025(5) 0.021(5) O5 0.104(7) 0.087(6) 0.077(6) 0.013(5) 0.039(5) 0.006(5) N1 0.077(6) 0.076(7) 0.060(5) 0.004(5) 0.020(5) 0.012(6) O1 0.114(7) 0.076(6) 0.057(5) -0.007(4) 0.040(5) 0.002(5) O3 0.089(5) 0.075(6) 0.060(5) -0.001(4) 0.032(4) 0.003(4) C12 0.062(7) 0.073(8) 0.069(7) -0.001(6) 0.030(6) 0.004(6) C11 0.066(7) 0.072(8) 0.086(8) 0.003(7) 0.028(7) 0.008(6) C26 0.145(15) 0.086(10) 0.065(9) -0.007(7) 0.051(10) 0.000(10) C3 0.053(7) 0.100(11) 0.085(9) -0.013(7) 0.020(7) 0.022(7) C10 0.065(8) 0.085(9) 0.097(9) 0.024(7) 0.038(7) 0.004(7) C4 0.069(8) 0.088(10) 0.068(7) 0.001(7) 0.022(6) 0.005(7) C1 0.093(10) 0.087(10) 0.067(7) 0.019(7) 0.023(7) 0.014(8) O8 0.079(7) 0.195(13) 0.143(10) -0.029(9) 0.041(7) -0.022(8) C20 0.127(13) 0.072(10) 0.079(9) 0.014(7) 0.008(9) 0.031(10) C8 0.070(7) 0.069(8) 0.056(6) 0.001(6) 0.021(6) 0.000(6) N3 0.078(9) 0.114(10) 0.127(11) 0.032(9) 0.052(9) 0.017(7) C7 0.067(8) 0.092(10) 0.089(9) 0.022(7) 0.029(7) 0.017(7) C13 0.134(13) 0.134(14) 0.100(11) -0.031(10) 0.049(10) 0.025(11) C9 0.058(7) 0.059(7) 0.059(6) -0.002(5) 0.013(5) 0.007(5) C6 0.080(9) 0.093(10) 0.098(9) 0.010(8) 0.050(8) -0.002(8) C16 0.101(10) 0.090(10) 0.045(6) 0.008(6) 0.017(7) -0.012(8) C23 0.083(11) 0.128(14) 0.131(14) -0.007(12) 0.006(10) 0.013(10) C19 0.082(9) 0.119(13) 0.061(8) -0.001(8) 0.024(7) 0.003(9) C2 0.080(9) 0.078(10) 0.092(10) 0.009(7) 0.030(8) 0.010(7) F9 0.40(2) 0.167(12) 0.189(13) -0.043(10) 0.208(16) -0.026(13) C5 0.062(7) 0.065(7) 0.059(6) 0.007(6) 0.026(5) 0.008(6) F8 0.260(16) 0.241(15) 0.126(9) 0.087(10) 0.103(10) 0.053(12) C14 0.086(8) 0.088(9) 0.061(7) -0.014(7) 0.030(7) 0.002(7) O7 0.083(7) 0.205(14) 0.150(11) 0.076(10) 0.054(7) 0.025(7) C22 0.149(17) 0.108(14) 0.104(13) 0.044(11) 0.059(13) 0.015(12) C15 0.119(12) 0.131(13) 0.069(9) -0.021(9) 0.041(9) 0.022(10) C21 0.124(12) 0.082(11) 0.063(8) 0.014(7) 0.030(8) -0.022(9) F5 0.120(8) 0.265(16) 0.146(9) 0.051(9) 0.023(8) -0.041(9) F4 0.215(13) 0.169(11) 0.298(17) 0.125(12) 0.160(13) 0.036(9) F7 0.181(13) 0.42(3) 0.123(10) 0.005(12) 0.096(10) -0.023(14) C24 0.110(11) 0.068(8) 0.057(7) -0.001(6) 0.022(8) -0.010(7) C18 0.153(15) 0.114(13) 0.128(13) 0.020(11) 0.057(12) 0.071(12) C25 0.093(11) 0.107(11) 0.059(8) 0.007(7) 0.008(8) 0.013(9) C27 0.17(2) 0.16(2) 0.063(9) -0.003(11) 0.049(12) -0.010(15) F1 0.28(2) 0.183(15) 0.191(15) 0.111(12) -0.052(14) 0.004(12) F2 0.31(2) 0.288(19) 0.062(7) -0.025(8) -0.013(9) 0.094(13) F3 0.103(9) 0.51(3) 0.175(15) 0.179(18) 0.019(9) 0.065(13) C17 0.142(18) 0.125(15) 0.065(10) 0.019(10) 0.000(10) 0.009(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 Yb1 O4 2.252(8) . ? Yb1 O2 2.259(9) . ? Yb1 O6 2.276(9) . ? Yb1 O5 2.285(9) . ? Yb1 O3 2.289(7) . ? Yb1 O1 2.316(8) . ? Yb1 N2 2.527(9) . ? Yb1 N1 2.539(10) . ? F6 C22 1.29(2) . ? O6 C19 1.257(16) . ? O2 C24 1.276(14) . ? N2 C12 1.315(13) . ? N2 C9 1.364(13) . ? O4 C16 1.256(15) . ? O5 C21 1.301(16) . ? N1 C1 1.301(14) . ? N1 C5 1.358(13) . ? O1 C26 1.261(17) . ? O3 C14 1.257(12) . ? C12 C11 1.406(15) . ? C12 H12 0.9300 . ? C11 C10 1.354(15) . ? C11 H11 0.9300 . ? C26 C25 1.30(2) . ? C26 C27 1.52(2) . ? C3 C2 1.381(18) . ? C3 C4 1.398(16) . ? C3 H3 0.9300 . ? C10 C8 1.390(15) . ? C10 H10 0.9300 . ? C4 C5 1.422(15) . ? C4 C6 1.435(17) . ? C1 C2 1.404(18) . ? C1 H1 0.9300 . ? O8 N3 1.210(15) . ? C20 C19 1.35(2) . ? C20 C21 1.377(19) . ? C20 H20 0.9300 . ? C8 C7 1.397(16) . ? C8 C9 1.415(15) . ? N3 O7 1.181(15) . ? N3 C6 1.486(16) . ? C7 C6 1.336(16) . ? C7 H7 0.9300 . ? C13 C14 1.481(17) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C9 C5 1.426(14) . ? C16 C15 1.353(18) . ? C16 C17 1.52(2) . ? C23 C24 1.470(19) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C19 C18 1.491(18) . ? C2 H2 0.9300 . ? F9 C27 1.30(2) . ? F8 C27 1.27(2) . ? C14 C15 1.353(18) . ? C22 F5 1.30(2) . ? C22 F4 1.311(17) . ? C22 C21 1.57(2) . ? C15 H15 0.9300 . ? F7 C27 1.31(2) . ? C24 C25 1.420(19) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C25 H25 0.9300 . ? F1 C17 1.27(2) . ? F2 C17 1.29(2) . ? F3 C17 1.23(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Yb1 O2 146.9(3) . . ? O4 Yb1 O6 74.7(3) . . ? O2 Yb1 O6 119.8(3) . . ? O4 Yb1 O5 81.2(3) . . ? O2 Yb1 O5 74.7(3) . . ? O6 Yb1 O5 76.6(3) . . ? O4 Yb1 O3 73.7(3) . . ? O2 Yb1 O3 80.4(3) . . ? O6 Yb1 O3 143.4(3) . . ? O5 Yb1 O3 80.7(3) . . ? O4 Yb1 O1 138.2(3) . . ? O2 Yb1 O1 74.3(3) . . ? O6 Yb1 O1 75.1(3) . . ? O5 Yb1 O1 118.6(3) . . ? O3 Yb1 O1 141.5(3) . . ? O4 Yb1 N2 112.0(3) . . ? O2 Yb1 N2 79.1(3) . . ? O6 Yb1 N2 136.0(3) . . ? O5 Yb1 N2 146.2(3) . . ? O3 Yb1 N2 74.1(3) . . ? O1 Yb1 N2 73.0(3) . . ? O4 Yb1 N1 73.3(3) . . ? O2 Yb1 N1 136.0(3) . . ? O6 Yb1 N1 78.4(3) . . ? O5 Yb1 N1 148.1(3) . . ? O3 Yb1 N1 109.3(3) . . ? O1 Yb1 N1 72.8(3) . . ? N2 Yb1 N1 63.8(3) . . ? C19 O6 Yb1 133.5(9) . . ? C24 O2 Yb1 136.7(9) . . ? C12 N2 C9 115.3(9) . . ? C12 N2 Yb1 123.0(7) . . ? C9 N2 Yb1 120.2(7) . . ? C16 O4 Yb1 131.9(9) . . ? C21 O5 Yb1 128.2(9) . . ? C1 N1 C5 119.8(11) . . ? C1 N1 Yb1 121.0(9) . . ? C5 N1 Yb1 118.9(7) . . ? C26 O1 Yb1 129.5(9) . . ? C14 O3 Yb1 137.0(8) . . ? N2 C12 C11 125.4(10) . . ? N2 C12 H12 117.3 . . ? C11 C12 H12 117.3 . . ? C10 C11 C12 118.4(11) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? O1 C26 C25 130.6(14) . . ? O1 C26 C27 112.9(17) . . ? C25 C26 C27 116.5(16) . . ? C2 C3 C4 117.1(12) . . ? C2 C3 H3 121.5 . . ? C4 C3 H3 121.5 . . ? C11 C10 C8 119.7(11) . . ? C11 C10 H10 120.2 . . ? C8 C10 H10 120.2 . . ? C3 C4 C5 119.0(12) . . ? C3 C4 C6 126.1(12) . . ? C5 C4 C6 114.9(11) . . ? N1 C1 C2 121.7(12) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C19 C20 C21 126.0(14) . . ? C19 C20 H20 117.0 . . ? C21 C20 H20 117.0 . . ? C10 C8 C7 122.5(11) . . ? C10 C8 C9 117.5(10) . . ? C7 C8 C9 120.0(11) . . ? O7 N3 O8 123.4(14) . . ? O7 N3 C6 120.0(15) . . ? O8 N3 C6 116.4(14) . . ? C6 C7 C8 118.2(12) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C9 C8 123.7(10) . . ? N2 C9 C5 115.8(10) . . ? C8 C9 C5 120.4(10) . . ? C7 C6 C4 126.5(11) . . ? C7 C6 N3 116.5(12) . . ? C4 C6 N3 117.0(12) . . ? O4 C16 C15 130.8(13) . . ? O4 C16 C17 110.2(14) . . ? C15 C16 C17 119.0(14) . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O6 C19 C20 123.8(14) . . ? O6 C19 C18 116.8(14) . . ? C20 C19 C18 119.5(15) . . ? C3 C2 C1 121.2(13) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? N1 C5 C4 121.3(10) . . ? N1 C5 C9 118.9(10) . . ? C4 C5 C9 119.9(10) . . ? O3 C14 C15 123.8(12) . . ? O3 C14 C13 117.8(12) . . ? C15 C14 C13 118.2(11) . . ? F6 C22 F5 102.0(17) . . ? F6 C22 F4 106.1(16) . . ? F5 C22 F4 109.6(18) . . ? F6 C22 C21 112.6(17) . . ? F5 C22 C21 113.6(14) . . ? F4 C22 C21 112.2(15) . . ? C14 C15 C16 121.5(12) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? O5 C21 C20 127.9(13) . . ? O5 C21 C22 108.2(14) . . ? C20 C21 C22 123.9(14) . . ? O2 C24 C25 122.4(13) . . ? O2 C24 C23 118.1(14) . . ? C25 C24 C23 119.5(13) . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C26 C25 C24 123.1(13) . . ? C26 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? F8 C27 F9 106.8(16) . . ? F8 C27 F7 104(2) . . ? F9 C27 F7 101(2) . . ? F8 C27 C26 118(2) . . ? F9 C27 C26 112.2(18) . . ? F7 C27 C26 113.3(16) . . ? F3 C17 F1 103(2) . . ? F3 C17 F2 102.9(19) . . ? F1 C17 F2 104(2) . . ? F3 C17 C16 115.9(18) . . ? F1 C17 C16 113.7(17) . . ? F2 C17 C16 115.6(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Yb1 O6 C19 62.6(12) . . . . ? O2 Yb1 O6 C19 -85.1(12) . . . . ? O5 Yb1 O6 C19 -21.8(12) . . . . ? O3 Yb1 O6 C19 31.4(15) . . . . ? O1 Yb1 O6 C19 -146.7(13) . . . . ? N2 Yb1 O6 C19 168.6(11) . . . . ? N1 Yb1 O6 C19 138.2(12) . . . . ? O4 Yb1 O2 C24 179.2(10) . . . . ? O6 Yb1 O2 C24 -72.0(12) . . . . ? O5 Yb1 O2 C24 -136.3(12) . . . . ? O3 Yb1 O2 C24 140.8(11) . . . . ? O1 Yb1 O2 C24 -10.0(11) . . . . ? N2 Yb1 O2 C24 65.3(11) . . . . ? N1 Yb1 O2 C24 32.9(13) . . . . ? O4 Yb1 N2 C12 -124.1(8) . . . . ? O2 Yb1 N2 C12 23.3(8) . . . . ? O6 Yb1 N2 C12 145.3(8) . . . . ? O5 Yb1 N2 C12 -16.2(11) . . . . ? O3 Yb1 N2 C12 -59.6(8) . . . . ? O1 Yb1 N2 C12 100.1(8) . . . . ? N1 Yb1 N2 C12 178.9(9) . . . . ? O4 Yb1 N2 C9 70.8(8) . . . . ? O2 Yb1 N2 C9 -141.7(8) . . . . ? O6 Yb1 N2 C9 -19.8(9) . . . . ? O5 Yb1 N2 C9 178.7(7) . . . . ? O3 Yb1 N2 C9 135.3(8) . . . . ? O1 Yb1 N2 C9 -65.0(8) . . . . ? N1 Yb1 N2 C9 13.8(7) . . . . ? O2 Yb1 O4 C16 -28.3(14) . . . . ? O6 Yb1 O4 C16 -149.9(12) . . . . ? O5 Yb1 O4 C16 -71.5(12) . . . . ? O3 Yb1 O4 C16 11.3(11) . . . . ? O1 Yb1 O4 C16 164.9(10) . . . . ? N2 Yb1 O4 C16 76.1(12) . . . . ? N1 Yb1 O4 C16 127.9(12) . . . . ? O4 Yb1 O5 C21 -58.6(10) . . . . ? O2 Yb1 O5 C21 144.2(11) . . . . ? O6 Yb1 O5 C21 17.6(10) . . . . ? O3 Yb1 O5 C21 -133.4(11) . . . . ? O1 Yb1 O5 C21 82.1(11) . . . . ? N2 Yb1 O5 C21 -175.4(9) . . . . ? N1 Yb1 O5 C21 -21.6(14) . . . . ? O4 Yb1 N1 C1 50.2(9) . . . . ? O2 Yb1 N1 C1 -148.2(9) . . . . ? O6 Yb1 N1 C1 -27.1(9) . . . . ? O5 Yb1 N1 C1 11.9(12) . . . . ? O3 Yb1 N1 C1 115.6(9) . . . . ? O1 Yb1 N1 C1 -104.9(9) . . . . ? N2 Yb1 N1 C1 176.0(10) . . . . ? O4 Yb1 N1 C5 -136.2(8) . . . . ? O2 Yb1 N1 C5 25.3(10) . . . . ? O6 Yb1 N1 C5 146.4(8) . . . . ? O5 Yb1 N1 C5 -174.6(7) . . . . ? O3 Yb1 N1 C5 -70.8(8) . . . . ? O1 Yb1 N1 C5 68.6(8) . . . . ? N2 Yb1 N1 C5 -10.5(7) . . . . ? O4 Yb1 O1 C26 -168.5(11) . . . . ? O2 Yb1 O1 C26 18.9(11) . . . . ? O6 Yb1 O1 C26 146.4(12) . . . . ? O5 Yb1 O1 C26 81.1(12) . . . . ? O3 Yb1 O1 C26 -31.8(13) . . . . ? N2 Yb1 O1 C26 -64.2(11) . . . . ? N1 Yb1 O1 C26 -131.4(12) . . . . ? O4 Yb1 O3 C14 -4.2(11) . . . . ? O2 Yb1 O3 C14 155.1(12) . . . . ? O6 Yb1 O3 C14 27.1(14) . . . . ? O5 Yb1 O3 C14 79.2(12) . . . . ? O1 Yb1 O3 C14 -155.8(11) . . . . ? N2 Yb1 O3 C14 -123.6(12) . . . . ? N1 Yb1 O3 C14 -69.4(12) . . . . ? C9 N2 C12 C11 2.5(16) . . . . ? Yb1 N2 C12 C11 -163.2(9) . . . . ? N2 C12 C11 C10 -2.5(19) . . . . ? Yb1 O1 C26 C25 -20(2) . . . . ? Yb1 O1 C26 C27 161.2(11) . . . . ? C12 C11 C10 C8 1.5(19) . . . . ? C2 C3 C4 C5 0.0(17) . . . . ? C2 C3 C4 C6 -177.1(13) . . . . ? C5 N1 C1 C2 -3.5(19) . . . . ? Yb1 N1 C1 C2 170.0(10) . . . . ? C11 C10 C8 C7 -177.0(12) . . . . ? C11 C10 C8 C9 -0.8(18) . . . . ? C10 C8 C7 C6 174.6(13) . . . . ? C9 C8 C7 C6 -1.6(18) . . . . ? C12 N2 C9 C8 -1.7(15) . . . . ? Yb1 N2 C9 C8 164.5(8) . . . . ? C12 N2 C9 C5 177.9(9) . . . . ? Yb1 N2 C9 C5 -15.9(12) . . . . ? C10 C8 C9 N2 0.9(17) . . . . ? C7 C8 C9 N2 177.2(10) . . . . ? C10 C8 C9 C5 -178.7(11) . . . . ? C7 C8 C9 C5 -2.3(16) . . . . ? C8 C7 C6 C4 4(2) . . . . ? C8 C7 C6 N3 -175.0(12) . . . . ? C3 C4 C6 C7 174.6(13) . . . . ? C5 C4 C6 C7 -3(2) . . . . ? C3 C4 C6 N3 -6(2) . . . . ? C5 C4 C6 N3 176.7(12) . . . . ? O7 N3 C6 C7 -48(2) . . . . ? O8 N3 C6 C7 126.7(15) . . . . ? O7 N3 C6 C4 132.5(15) . . . . ? O8 N3 C6 C4 -52.5(19) . . . . ? Yb1 O4 C16 C15 -12(2) . . . . ? Yb1 O4 C16 C17 167.7(12) . . . . ? Yb1 O6 C19 C20 18(2) . . . . ? Yb1 O6 C19 C18 -160.9(10) . . . . ? C21 C20 C19 O6 -1(2) . . . . ? C21 C20 C19 C18 178.2(15) . . . . ? C4 C3 C2 C1 -1(2) . . . . ? N1 C1 C2 C3 3(2) . . . . ? C1 N1 C5 C4 2.0(16) . . . . ? Yb1 N1 C5 C4 -171.6(8) . . . . ? C1 N1 C5 C9 -179.2(11) . . . . ? Yb1 N1 C5 C9 7.2(13) . . . . ? C3 C4 C5 N1 -0.2(17) . . . . ? C6 C4 C5 N1 177.2(11) . . . . ? C3 C4 C5 C9 -179.0(10) . . . . ? C6 C4 C5 C9 -1.6(16) . . . . ? N2 C9 C5 N1 5.5(14) . . . . ? C8 C9 C5 N1 -174.9(10) . . . . ? N2 C9 C5 C4 -175.7(10) . . . . ? C8 C9 C5 C4 3.9(16) . . . . ? Yb1 O3 C14 C15 -4(2) . . . . ? Yb1 O3 C14 C13 -178.3(9) . . . . ? O3 C14 C15 C16 9(2) . . . . ? C13 C14 C15 C16 -176.9(15) . . . . ? O4 C16 C15 C14 -1(3) . . . . ? C17 C16 C15 C14 179.6(16) . . . . ? Yb1 O5 C21 C20 -13(2) . . . . ? Yb1 O5 C21 C22 168.7(10) . . . . ? C19 C20 C21 O5 -1(3) . . . . ? C19 C20 C21 C22 177.3(15) . . . . ? F6 C22 C21 O5 -59.0(19) . . . . ? F5 C22 C21 O5 56(2) . . . . ? F4 C22 C21 O5 -178.6(16) . . . . ? F6 C22 C21 C20 122.2(17) . . . . ? F5 C22 C21 C20 -122.5(18) . . . . ? F4 C22 C21 C20 3(3) . . . . ? Yb1 O2 C24 C25 -1(2) . . . . ? Yb1 O2 C24 C23 -178.0(10) . . . . ? O1 C26 C25 C24 1(3) . . . . ? C27 C26 C25 C24 179.9(15) . . . . ? O2 C24 C25 C26 10(2) . . . . ? C23 C24 C25 C26 -172.7(15) . . . . ? O1 C26 C27 F8 -150.4(18) . . . . ? C25 C26 C27 F8 30(3) . . . . ? O1 C26 C27 F9 85(2) . . . . ? C25 C26 C27 F9 -94(2) . . . . ? O1 C26 C27 F7 -29(3) . . . . ? C25 C26 C27 F7 152(2) . . . . ? O4 C16 C17 F3 49(3) . . . . ? C15 C16 C17 F3 -132(2) . . . . ? O4 C16 C17 F1 -70(3) . . . . ? C15 C16 C17 F1 109(2) . . . . ? O4 C16 C17 F2 169(2) . . . . ? C15 C16 C17 F2 -11(3) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.797 _refine_diff_density_min -2.675 _refine_diff_density_rms 0.188 _database_code_depnum_ccdc_archive 'CCDC 933188' ####################################################################### # # 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_ybtpmnitro _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris(1,1,1-trifluoro-5,5-dimethyl-2,4-hexanedionate)mono(5-nitro-1,10-phenanthroline) ytterbium(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H37 F9 N3 O8 Yb' _chemical_formula_sum 'C36 H37 F9 N3 O8 Yb' _chemical_formula_weight 983.73 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9036(3) _cell_length_b 22.3251(7) _cell_length_c 39.8599(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.782(2) _cell_angle_gamma 90.00 _cell_volume 8812.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3984 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 14.92 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3912 _exptl_absorpt_coefficient_mu 2.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.857 _exptl_absorpt_process_details (SADABS;Sheldrick,2003) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 148952 _diffrn_reflns_av_R_equivalents 0.1741 _diffrn_reflns_av_sigmaI/netI 0.1763 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.88 _reflns_number_total 16971 _reflns_number_gt 7034 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material SHELXL-97 _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^)+(0.0976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16971 _refine_ls_number_parameters 1011 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.2024 _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.2217 _refine_ls_wR_factor_gt 0.1815 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.962 _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 Yb2 Yb 0.14101(5) 0.61730(2) 0.410603(14) 0.0652(2) Uani 1 1 d . . . Yb1 Yb 0.76998(6) 1.10253(2) 0.333185(14) 0.0658(2) Uani 1 1 d . . . N1 N 0.5286(11) 1.0877(5) 0.3509(3) 0.082(3) Uani 1 1 d . . . N2 N 0.7354(12) 1.0258(4) 0.3775(3) 0.069(3) Uani 1 1 d . . . N3 N 0.210(2) 0.9571(11) 0.4139(5) 0.158(8) Uani 1 1 d . . . O1 O 0.1353(19) 0.9985(9) 0.4202(5) 0.207(9) Uani 1 1 d . . . O2 O 0.1952(18) 0.9095(8) 0.4234(6) 0.222(10) Uani 1 1 d . . . C1 C 0.4300(16) 1.1206(7) 0.3382(4) 0.096(5) Uani 1 1 d . . . H1 H 0.4478 1.1517 0.3233 0.115 Uiso 1 1 calc R . . C2 C 0.2955(16) 1.1073(9) 0.3478(5) 0.108(6) Uani 1 1 d . . . H2 H 0.2262 1.1309 0.3390 0.129 Uiso 1 1 calc R . . C3 C 0.263(2) 1.0646(10) 0.3680(5) 0.120(7) Uani 1 1 d . . . H3 H 0.1740 1.0575 0.3736 0.144 Uiso 1 1 calc R . . C4 C 0.3663(19) 1.0299(7) 0.3809(4) 0.089(5) Uani 1 1 d . . . C5 C 0.3458(17) 0.9780(9) 0.4034(4) 0.100(6) Uani 1 1 d . . . C6 C 0.4531(18) 0.9477(8) 0.4162(4) 0.124(7) Uani 1 1 d D . . H6 H 0.4360 0.9166 0.4310 0.148 Uiso 1 1 calc R . . C7 C 0.5880(19) 0.9597(9) 0.4085(4) 0.102(5) Uani 1 1 d D . . C8 C 0.704(3) 0.9303(8) 0.4211(4) 0.120(6) Uani 1 1 d . . . H8 H 0.6929 0.8971 0.4348 0.144 Uiso 1 1 calc R . . C9 C 0.830(2) 0.9482(8) 0.4141(5) 0.122(6) Uani 1 1 d . . . H9 H 0.9060 0.9305 0.4236 0.146 Uiso 1 1 calc R . . C10 C 0.8361(16) 0.9955(6) 0.3913(4) 0.092(5) Uani 1 1 d . . . H10 H 0.9224 1.0071 0.3851 0.110 Uiso 1 1 calc R . . C11 C 0.612(2) 1.0101(7) 0.3856(4) 0.087(4) Uani 1 1 d . . . C12 C 0.4983(15) 1.0432(7) 0.3714(4) 0.078(4) Uani 1 1 d . . . C13B C 1.0951(17) 0.9724(9) 0.3010(5) 0.101(5) Uani 1 1 d . . . F1B F 1.1779(8) 1.0152(5) 0.2912(2) 0.122(3) Uani 1 1 d . . . F2B F 1.1489(8) 0.9541(4) 0.3308(2) 0.124(3) Uani 1 1 d . . . F3B F 1.1175(9) 0.9253(5) 0.2807(2) 0.131(3) Uani 1 1 d . . . O4D O 0.0937(9) 0.5235(4) 0.4292(2) 0.095(3) Uani 1 1 d . A . O5D O 0.2685(8) 0.6053(4) 0.4579(2) 0.077(2) Uani 1 1 d . A . C13D C 0.0999(15) 0.4233(6) 0.4469(4) 0.097(5) Uani 1 1 d D A . C14D C 0.1462(13) 0.4891(5) 0.4500(3) 0.072(4) Uani 1 1 d . . . C15D C 0.2358(13) 0.5063(5) 0.4759(3) 0.079(4) Uani 1 1 d . A . H15D H 0.2604 0.4782 0.4921 0.095 Uiso 1 1 calc R . . C16D C 0.2866(12) 0.5613(6) 0.4782(3) 0.067(3) Uani 1 1 d . . . C17D C 0.3673(19) 0.5824(9) 0.5092(4) 0.100(5) Uani 1 1 d . A . C18D C -0.015(3) 0.4120(9) 0.4220(6) 0.268(18) Uani 1 1 d . . . H18A H -0.0934 0.4341 0.4287 0.402 Uiso 1 1 calc R A . H18B H -0.0359 0.3700 0.4215 0.402 Uiso 1 1 calc R . . H18C H 0.0116 0.4247 0.4001 0.402 Uiso 1 1 calc R . . C19D C 0.037(3) 0.4019(10) 0.4795(6) 0.270(17) Uani 1 1 d . . . H19A H -0.0329 0.4293 0.4859 0.404 Uiso 1 1 calc R A . H19B H 0.1050 0.4003 0.4969 0.404 Uiso 1 1 calc R . . H19C H -0.0009 0.3628 0.4762 0.404 Uiso 1 1 calc R . . C20D C 0.205(2) 0.3868(8) 0.4360(8) 0.285(17) Uani 1 1 d DU . . H20A H 0.2412 0.4028 0.4156 0.428 Uiso 1 1 calc R A . H20B H 0.1721 0.3470 0.4320 0.428 Uiso 1 1 calc R . . H20C H 0.2755 0.3856 0.4528 0.428 Uiso 1 1 calc R . . F1D F 0.3261(13) 0.6300(6) 0.5217(3) 0.167(5) Uani 1 1 d . . . F2D F 0.3739(11) 0.5408(5) 0.5320(2) 0.167(5) Uani 1 1 d . . . F3D F 0.4936(11) 0.5915(5) 0.4996(2) 0.151(4) Uani 1 1 d . . . O3E O 0.0353(8) 0.6883(4) 0.3794(2) 0.078(3) Uani 1 1 d . A . O4E O 0.2986(7) 0.6866(4) 0.3992(2) 0.068(2) Uani 1 1 d . A . C14E C 0.2962(15) 0.7371(6) 0.3841(3) 0.075(4) Uani 1 1 d . . . C15E C 0.1868(17) 0.7637(6) 0.3686(4) 0.096(5) Uani 1 1 d . A . H15E H 0.1987 0.8012 0.3589 0.115 Uiso 1 1 calc R . . C16E C 0.0552(14) 0.7368(7) 0.3665(3) 0.076(4) Uani 1 1 d . . . C17E C -0.0562(14) 0.7736(8) 0.3498(4) 0.087(4) Uani 1 1 d . A . C18E C -0.152(3) 0.7329(10) 0.3373(7) 0.254(17) Uani 1 1 d . . . H18D H -0.1107 0.7067 0.3214 0.382 Uiso 1 1 calc R A . H18E H -0.2247 0.7544 0.3265 0.382 Uiso 1 1 calc R . . H18F H -0.1875 0.7096 0.3555 0.382 Uiso 1 1 calc R . . C19E C -0.107(3) 0.8134(13) 0.3727(6) 0.33(3) Uani 1 1 d . . . H19D H -0.1314 0.7923 0.3927 0.501 Uiso 1 1 calc R A . H19E H -0.1861 0.8325 0.3633 0.501 Uiso 1 1 calc R . . H19F H -0.0405 0.8431 0.3780 0.501 Uiso 1 1 calc R . . C20E C -0.019(2) 0.8002(15) 0.3197(7) 0.32(2) Uani 1 1 d . . . H20D H 0.0161 0.7702 0.3049 0.474 Uiso 1 1 calc R A . H20E H 0.0491 0.8299 0.3240 0.474 Uiso 1 1 calc R . . H20F H -0.0965 0.8188 0.3094 0.474 Uiso 1 1 calc R . . O3F O 0.3064(8) 0.5639(4) 0.3854(2) 0.084(3) Uani 1 1 d . A . O4F O 0.0386(9) 0.5730(4) 0.3661(2) 0.086(3) Uani 1 1 d . A . C13F C 0.448(2) 0.5005(10) 0.3583(6) 0.142(9) Uani 1 1 d D A . C14F C 0.3101(17) 0.5271(7) 0.3625(4) 0.092(5) Uani 1 1 d . . . C15F C 0.2029(17) 0.5104(7) 0.3413(4) 0.097(5) Uani 1 1 d . A . H15F H 0.2195 0.4813 0.3252 0.116 Uiso 1 1 calc R . . C16F C 0.0686(16) 0.5350(7) 0.3426(4) 0.090(5) Uani 1 1 d . . . C17F C -0.0337(18) 0.5100(8) 0.3147(5) 0.148(9) Uani 1 1 d D A . C18F C 0.001(2) 0.5531(10) 0.2854(5) 0.175(9) Uani 1 1 d . . . H18G H 0.0878 0.5432 0.2768 0.263 Uiso 1 1 calc R A . H18H H 0.0013 0.5936 0.2935 0.263 Uiso 1 1 calc R . . H18I H -0.0663 0.5490 0.2679 0.263 Uiso 1 1 calc R . . C19F C -0.176(2) 0.5306(13) 0.3301(5) 0.254(16) Uani 1 1 d . . . H19G H -0.1956 0.5065 0.3494 0.381 Uiso 1 1 calc R A . H19H H -0.2462 0.5257 0.3135 0.381 Uiso 1 1 calc R . . H19I H -0.1706 0.5720 0.3366 0.381 Uiso 1 1 calc R . . C20F C -0.026(2) 0.4517(8) 0.3018(6) 0.224(14) Uani 1 1 d D . . H20G H -0.0487 0.4235 0.3190 0.337 Uiso 1 1 calc R A . H20H H 0.0636 0.4441 0.2942 0.337 Uiso 1 1 calc R . . H20I H -0.0890 0.4476 0.2833 0.337 Uiso 1 1 calc R . . F1F F 0.4905(13) 0.4742(6) 0.3840(3) 0.189(6) Uani 1 1 d . . . F2F F 0.5318(12) 0.5400(8) 0.3474(4) 0.232(9) Uani 1 1 d . . . F3F F 0.4454(14) 0.4569(8) 0.3348(4) 0.275(10) Uani 1 1 d D . . O3A O 0.9002(9) 1.1309(4) 0.3784(2) 0.082(3) Uani 1 1 d D . . O4A O 0.6835(9) 1.1934(4) 0.3497(2) 0.093(3) Uani 1 1 d D . . C13A C 1.0312(19) 1.1811(9) 0.4156(4) 0.132(8) Uani 1 1 d D . . C15A C 0.8311(14) 1.2310(6) 0.3885(4) 0.103(5) Uani 1 1 d D . . H15A H 0.8569 1.2649 0.4005 0.123 Uiso 1 1 calc R . . C14A C 0.9092(13) 1.1816(6) 0.3927(3) 0.085(4) Uani 1 1 d D . . C16A C 0.7188(15) 1.2364(6) 0.3684(4) 0.101(5) Uani 1 1 d D . . C17A C 0.6368(19) 1.2931(7) 0.3669(6) 0.129(7) Uani 1 1 d D . . C18A C 0.718(2) 1.3471(9) 0.3652(11) 0.31(2) Uani 1 1 d D . . H18J H 0.7953 1.3433 0.3799 0.462 Uiso 1 1 calc R . . H18K H 0.6653 1.3810 0.3719 0.462 Uiso 1 1 calc R . . H18L H 0.7482 1.3529 0.3426 0.462 Uiso 1 1 calc R . . C19A C 0.587(4) 1.3067(18) 0.3999(7) 0.37(3) Uani 1 1 d D . . H19J H 0.6613 1.3114 0.4153 0.555 Uiso 1 1 calc R . . H19K H 0.5300 1.2746 0.4073 0.555 Uiso 1 1 calc R . . H19L H 0.5354 1.3432 0.3990 0.555 Uiso 1 1 calc R . . C20A C 0.521(3) 1.2878(9) 0.3483(9) 0.32(2) Uani 1 1 d D . . H20J H 0.5428 1.2788 0.3255 0.481 Uiso 1 1 calc R . . H20K H 0.4714 1.3247 0.3492 0.481 Uiso 1 1 calc R . . H20L H 0.4668 1.2560 0.3573 0.481 Uiso 1 1 calc R . . F1A F 1.1443(13) 1.1889(9) 0.3997(4) 0.244(9) Uani 1 1 d D . . F2A F 1.0333(12) 1.2272(5) 0.4368(3) 0.160(4) Uani 1 1 d D . . F3A F 1.0373(16) 1.1386(6) 0.4349(4) 0.234(8) Uani 1 1 d D . . O3B O 0.6802(7) 1.0222(4) 0.3058(2) 0.069(2) Uani 1 1 d . . . O4B O 0.9460(8) 1.0397(4) 0.3224(2) 0.070(2) Uani 1 1 d . . . C14B C 0.9548(14) 0.9938(6) 0.3048(3) 0.070(4) Uani 1 1 d . . . C15B C 0.8578(12) 0.9581(6) 0.2900(3) 0.070(4) Uani 1 1 d . . . H15B H 0.8821 0.9230 0.2790 0.084 Uiso 1 1 calc R . . C16B C 0.7192(13) 0.9757(6) 0.2916(3) 0.065(4) Uani 1 1 d . . . C17B C 0.6100(14) 0.9349(7) 0.2757(4) 0.089(4) Uani 1 1 d . . . C18B C 0.535(2) 0.9132(10) 0.3040(5) 0.199(11) Uani 1 1 d . . . H18M H 0.5923 0.8875 0.3174 0.299 Uiso 1 1 calc R . . H18N H 0.4581 0.8910 0.2961 0.299 Uiso 1 1 calc R . . H18O H 0.5061 0.9465 0.3173 0.299 Uiso 1 1 calc R . . C19B C 0.6660(17) 0.8852(7) 0.2520(5) 0.141(7) Uani 1 1 d . . . H19M H 0.7131 0.9037 0.2338 0.212 Uiso 1 1 calc R . . H19N H 0.5925 0.8617 0.2432 0.212 Uiso 1 1 calc R . . H19O H 0.7270 0.8599 0.2644 0.212 Uiso 1 1 calc R . . C20B C 0.5098(18) 0.9739(8) 0.2565(6) 0.180(10) Uani 1 1 d . . . H20M H 0.5522 0.9900 0.2369 0.269 Uiso 1 1 calc R . . H20N H 0.4809 1.0062 0.2706 0.269 Uiso 1 1 calc R . . H20O H 0.4330 0.9503 0.2498 0.269 Uiso 1 1 calc R . . O4C O 0.6778(9) 1.1376(4) 0.2847(2) 0.086(3) Uani 1 1 d . . . O3C O 0.9282(9) 1.1640(4) 0.3112(3) 0.097(3) Uani 1 1 d . . . C13C C 1.046(3) 1.2432(15) 0.2864(8) 0.162(10) Uani 1 1 d . . . C14C C 0.9187(18) 1.2041(7) 0.2876(5) 0.098(5) Uani 1 1 d . . . C15C C 0.814(2) 1.2113(7) 0.2645(4) 0.111(6) Uani 1 1 d . . . H15C H 0.8214 1.2418 0.2487 0.133 Uiso 1 1 calc R . . C16C C 0.7010(16) 1.1760(7) 0.2637(4) 0.088(4) Uani 1 1 d . . . C17C C 0.6014(18) 1.1858(7) 0.2349(4) 0.100(5) Uani 1 1 d . . . C18C C 0.588(3) 1.2470(8) 0.2237(6) 0.215(13) Uani 1 1 d . . . H18P H 0.6753 1.2628 0.2186 0.322 Uiso 1 1 calc R . . H18Q H 0.5477 1.2706 0.2410 0.322 Uiso 1 1 calc R . . H18R H 0.5313 1.2482 0.2039 0.322 Uiso 1 1 calc R . . C19C C 0.473(2) 1.1633(17) 0.2416(5) 0.29(2) Uani 1 1 d . . . H19P H 0.4806 1.1226 0.2491 0.440 Uiso 1 1 calc R . . H19Q H 0.4185 1.1649 0.2215 0.440 Uiso 1 1 calc R . . H19R H 0.4320 1.1871 0.2587 0.440 Uiso 1 1 calc R . . C20C C 0.651(2) 1.1477(12) 0.2066(5) 0.218(13) Uani 1 1 d . . . H20P H 0.7400 1.1601 0.2007 0.327 Uiso 1 1 calc R . . H20Q H 0.5911 1.1521 0.1876 0.327 Uiso 1 1 calc R . . H20R H 0.6526 1.1065 0.2135 0.327 Uiso 1 1 calc R . . F1C F 1.082(2) 1.2621(10) 0.3148(5) 0.307(15) Uani 1 1 d . . . F2C F 1.0382(18) 1.2916(7) 0.2678(5) 0.257(10) Uani 1 1 d . . . F3C F 1.1432(18) 1.2169(9) 0.2734(7) 0.303(14) Uani 1 1 d . . . F1E F 0.4771(11) 0.7808(5) 0.4123(3) 0.150(4) Uani 1 1 d . . . F2E F 0.5298(10) 0.7273(6) 0.3708(3) 0.175(5) Uani 1 1 d . . . C13E C 0.4355(17) 0.7627(8) 0.3821(5) 0.105(6) Uani 1 1 d . A . F3E F 0.4364(11) 0.8130(5) 0.3640(3) 0.172(5) Uani 1 1 d . . . O1A O -0.4620(17) 0.8269(8) 0.4757(4) 0.083(6) Uiso 0.542(13) 1 d PD A 1 O2A O -0.5053(19) 0.7354(9) 0.4923(5) 0.102(7) Uiso 0.542(13) 1 d PD A 1 N1A N 0.101(3) 0.7143(12) 0.4541(6) 0.067(7) Uiso 0.542(13) 1 d P A 1 N2A N -0.095(3) 0.6258(14) 0.4299(7) 0.063(8) Uiso 0.542(13) 1 d P A 1 N3A N -0.436(2) 0.7772(12) 0.4798(7) 0.088(8) Uiso 0.542(13) 1 d PD A 1 C1A C 0.187(3) 0.7408(13) 0.4623(7) 0.053(8) Uiso 0.542(13) 1 d P A 1 H1A H 0.2736 0.7265 0.4582 0.063 Uiso 0.542(13) 1 calc PR A 1 C2A C 0.173(3) 0.7972(11) 0.4793(6) 0.069(7) Uiso 0.542(13) 1 d P A 1 H2A H 0.2458 0.8197 0.4869 0.082 Uiso 0.542(13) 1 calc PR A 1 C3A C 0.055(3) 0.8127(11) 0.4826(6) 0.058(7) Uiso 0.542(13) 1 d P A 1 H3A H 0.0430 0.8512 0.4910 0.070 Uiso 0.542(13) 1 calc PR A 1 C4A C -0.064(3) 0.7808(11) 0.4757(5) 0.037(5) Uiso 0.542(13) 1 d P A 1 C5A C -0.191(2) 0.7919(11) 0.4802(5) 0.066(7) Uiso 0.542(13) 1 d P A 1 H5A H -0.2149 0.8282 0.4900 0.079 Uiso 0.542(13) 1 calc PR A 1 C6A C -0.303(3) 0.7488(11) 0.4702(6) 0.052(8) Uiso 0.542(13) 1 d P A 1 C7A C -0.267(3) 0.7023(10) 0.4555(5) 0.059(7) Uiso 0.542(13) 1 d PD A 1 C8A C -0.370(2) 0.6561(9) 0.4432(5) 0.054(6) Uiso 0.542(13) 1 d P A 1 H8A H -0.4616 0.6616 0.4468 0.064 Uiso 0.542(13) 1 calc PR A 1 C9A C -0.320(5) 0.6015(19) 0.4250(11) 0.13(2) Uiso 0.542(13) 1 d P A 1 H9A H -0.3792 0.5730 0.4164 0.157 Uiso 0.542(13) 1 calc PR A 1 C10A C -0.195(3) 0.5961(10) 0.4220(5) 0.049(6) Uiso 0.542(13) 1 d P A 1 H10A H -0.1716 0.5608 0.4112 0.058 Uiso 0.542(13) 1 calc PR A 1 C11A C -0.140(2) 0.6816(10) 0.4467(5) 0.033(5) Uiso 0.542(13) 1 d PD A 1 C12A C -0.020(3) 0.7225(10) 0.4581(5) 0.042(6) Uiso 0.542(13) 1 d P A 1 O1B O -0.306(6) 0.826(3) 0.5121(15) 0.33(3) Uiso 0.458(13) 1 d PD A 2 O2B O -0.433(7) 0.790(3) 0.494(2) 0.33(4) Uiso 0.458(13) 1 d PD A 2 N1B N 0.073(2) 0.6923(10) 0.4480(5) 0.040(6) Uiso 0.458(13) 1 d P A 2 N2B N -0.091(4) 0.6031(17) 0.4233(9) 0.111(15) Uiso 0.458(13) 1 d P A 2 N3B N -0.323(7) 0.821(2) 0.4853(15) 0.23(2) Uiso 0.458(13) 1 d PD A 2 C1B C 0.182(10) 0.726(4) 0.461(2) 0.25(6) Uiso 0.458(13) 1 d PD A 2 H1B H 0.2743 0.7186 0.4617 0.302 Uiso 0.458(13) 1 calc PR A 2 C2B C 0.118(7) 0.771(3) 0.4728(14) 0.16(2) Uiso 0.458(13) 1 d PD A 2 H2B H 0.1790 0.8010 0.4779 0.195 Uiso 0.458(13) 1 calc PR A 2 C3B C -0.004(7) 0.789(3) 0.4800(14) 0.15(3) Uiso 0.458(13) 1 d PD A 2 H3B H -0.0255 0.8248 0.4910 0.182 Uiso 0.458(13) 1 calc PR A 2 C4B C -0.096(4) 0.7473(19) 0.4683(8) 0.082(10) Uiso 0.458(13) 1 d PD A 2 C5B C -0.253(4) 0.7556(19) 0.4734(11) 0.102(16) Uiso 0.458(13) 1 d PD A 2 C6B C -0.345(4) 0.6994(15) 0.4568(9) 0.112(14) Uiso 0.458(13) 1 d PD A 2 H6B H -0.4387 0.6992 0.4580 0.134 Uiso 0.458(13) 1 calc PR A 2 C7B C -0.274(3) 0.6530(14) 0.4412(10) 0.135(15) Uiso 0.458(13) 1 d PD A 2 C8B C -0.358(4) 0.6074(12) 0.4291(8) 0.050(10) Uiso 0.458(13) 1 d PD A 2 H8B H -0.4516 0.6125 0.4291 0.060 Uiso 0.458(13) 1 calc PR A 2 C9B C -0.302(4) 0.5533(19) 0.4168(10) 0.136(15) Uiso 0.458(13) 1 d PD A 2 H9B H -0.3525 0.5194 0.4115 0.164 Uiso 0.458(13) 1 calc PR A 2 C10B C -0.165(4) 0.5574(17) 0.4137(8) 0.097(11) Uiso 0.458(13) 1 d PD A 2 H10B H -0.1200 0.5252 0.4041 0.116 Uiso 0.458(13) 1 calc PR A 2 C11B C -0.136(3) 0.6440(14) 0.4368(6) 0.036(8) Uiso 0.458(13) 1 d PD A 2 C12B C -0.079(4) 0.6985(14) 0.4540(7) 0.058(8) Uiso 0.458(13) 1 d PD A 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 Yb2 0.0559(4) 0.0681(4) 0.0714(4) 0.0122(3) -0.0084(3) -0.0033(3) Yb1 0.0635(4) 0.0569(4) 0.0767(4) 0.0022(3) -0.0047(3) -0.0040(3) N1 0.065(8) 0.081(8) 0.099(9) -0.001(7) 0.007(7) -0.009(7) N2 0.052(7) 0.066(7) 0.089(8) 0.002(6) 0.006(6) -0.011(6) N3 0.17(2) 0.15(2) 0.153(16) 0.021(16) 0.068(14) -0.038(17) O1 0.154(17) 0.200(19) 0.27(2) -0.013(16) 0.050(14) -0.002(13) O2 0.166(15) 0.154(15) 0.35(3) 0.067(16) 0.099(15) -0.026(12) C1 0.070(11) 0.097(11) 0.120(13) -0.023(9) -0.022(10) 0.011(9) C2 0.051(11) 0.134(17) 0.138(16) -0.047(13) -0.012(10) 0.018(10) C3 0.089(15) 0.116(16) 0.155(19) -0.014(13) 0.022(13) -0.041(13) C4 0.090(14) 0.078(11) 0.101(12) -0.023(9) 0.033(11) -0.007(10) C5 0.083(13) 0.147(16) 0.069(11) -0.019(10) 0.004(9) -0.068(12) C6 0.17(2) 0.124(15) 0.077(12) -0.030(10) -0.030(14) -0.017(15) C7 0.082(13) 0.125(15) 0.099(13) -0.024(11) 0.008(10) -0.047(12) C8 0.150(19) 0.092(13) 0.117(15) 0.004(11) -0.020(15) 0.023(14) C9 0.123(17) 0.095(13) 0.148(17) 0.034(12) 0.016(13) 0.000(12) C10 0.088(12) 0.085(11) 0.102(12) 0.024(9) -0.010(9) -0.004(9) C11 0.116(15) 0.071(10) 0.074(10) -0.009(8) -0.006(10) -0.016(10) C12 0.061(11) 0.089(11) 0.085(11) -0.030(9) 0.031(9) -0.019(9) C13B 0.074(13) 0.124(15) 0.105(14) -0.011(12) -0.024(11) -0.003(11) F1B 0.065(6) 0.175(10) 0.125(8) -0.014(6) 0.017(5) -0.019(6) F2B 0.081(6) 0.154(8) 0.138(8) 0.000(7) -0.019(6) 0.029(5) F3B 0.091(7) 0.148(8) 0.155(9) -0.062(7) -0.007(6) 0.031(6) O4D 0.100(7) 0.084(7) 0.099(7) 0.031(6) -0.058(6) -0.026(5) O5D 0.075(6) 0.080(6) 0.076(6) 0.008(5) -0.006(5) -0.018(5) C13D 0.105(12) 0.062(10) 0.123(13) 0.023(9) 0.005(10) -0.023(9) C14D 0.073(9) 0.059(8) 0.083(10) 0.023(7) -0.012(8) -0.006(7) C15D 0.091(10) 0.046(8) 0.099(11) 0.021(7) -0.042(9) -0.013(7) C16D 0.058(8) 0.080(10) 0.064(9) 0.022(8) 0.006(7) 0.000(7) C17D 0.100(14) 0.141(16) 0.058(10) 0.021(11) -0.025(10) -0.043(12) C18D 0.38(4) 0.159(19) 0.26(3) 0.093(18) -0.23(3) -0.18(2) C19D 0.41(5) 0.19(3) 0.21(3) 0.07(2) 0.08(3) -0.14(3) C20D 0.36(4) 0.090(16) 0.41(4) -0.11(2) 0.05(3) -0.054(19) F1D 0.190(12) 0.171(11) 0.137(10) -0.077(9) -0.048(8) 0.006(9) F2D 0.217(12) 0.187(10) 0.094(7) 0.047(7) -0.079(7) -0.085(9) F3D 0.098(8) 0.241(12) 0.113(7) 0.028(7) -0.033(6) -0.053(8) O3E 0.078(6) 0.084(6) 0.073(6) 0.022(5) -0.002(5) -0.001(5) O4E 0.058(5) 0.069(6) 0.077(6) 0.005(5) 0.003(4) 0.000(4) C14E 0.086(11) 0.063(9) 0.076(10) 0.009(8) 0.022(8) -0.007(8) C15E 0.115(14) 0.061(9) 0.111(12) 0.024(8) -0.005(11) 0.017(9) C16E 0.058(10) 0.107(12) 0.064(9) 0.010(9) 0.009(7) 0.010(9) C17E 0.068(10) 0.118(13) 0.076(10) 0.028(10) -0.014(8) 0.006(9) C18E 0.23(3) 0.17(2) 0.36(4) 0.05(2) -0.22(3) 0.02(2) C19E 0.38(4) 0.41(4) 0.21(3) -0.15(3) -0.17(3) 0.35(4) C20E 0.102(18) 0.54(6) 0.30(3) 0.33(4) -0.015(19) 0.00(2) O3F 0.065(6) 0.071(6) 0.117(8) -0.014(6) 0.000(5) 0.009(5) O4F 0.071(6) 0.101(7) 0.087(7) -0.003(6) -0.018(5) 0.003(5) C13F 0.100(18) 0.143(19) 0.18(2) -0.083(18) -0.015(16) 0.080(15) C14F 0.108(14) 0.096(12) 0.073(11) -0.010(9) 0.010(10) 0.012(10) C15F 0.102(13) 0.112(12) 0.076(11) -0.017(9) 0.018(10) -0.009(11) C16F 0.076(12) 0.101(12) 0.093(12) 0.024(10) 0.033(9) 0.005(9) C17F 0.083(14) 0.28(3) 0.078(12) 0.010(16) -0.028(11) -0.049(16) C18F 0.16(2) 0.20(2) 0.16(2) -0.034(18) -0.073(17) -0.020(17) C19F 0.110(18) 0.46(5) 0.19(2) -0.13(3) -0.049(17) -0.09(2) C20F 0.25(3) 0.141(19) 0.28(3) -0.13(2) -0.06(2) -0.044(18) F1F 0.174(12) 0.204(13) 0.188(12) 0.004(10) -0.026(9) 0.127(10) F2F 0.080(10) 0.32(2) 0.302(19) 0.073(17) 0.073(10) 0.045(10) F3F 0.177(14) 0.33(2) 0.32(2) -0.150(18) -0.037(13) 0.159(15) O3A 0.096(7) 0.056(5) 0.094(7) 0.002(5) -0.008(5) -0.012(5) O4A 0.090(7) 0.079(7) 0.109(8) -0.004(6) -0.022(6) 0.005(5) C13A 0.19(2) 0.121(16) 0.082(13) -0.011(12) -0.029(14) -0.089(16) C15A 0.095(13) 0.069(10) 0.143(15) -0.035(10) -0.020(11) 0.010(9) C14A 0.091(12) 0.090(12) 0.072(10) -0.012(9) -0.003(8) -0.029(10) C16A 0.092(13) 0.081(12) 0.131(15) -0.004(11) -0.008(11) -0.003(10) C17A 0.099(14) 0.081(13) 0.21(2) -0.043(13) -0.041(14) 0.019(11) C18A 0.15(2) 0.081(17) 0.69(8) 0.02(3) -0.05(3) 0.028(16) C19A 0.48(7) 0.42(6) 0.22(3) -0.06(3) 0.08(4) 0.31(6) C20A 0.27(3) 0.115(19) 0.57(7) -0.12(3) -0.21(4) 0.12(2) F1A 0.109(10) 0.44(3) 0.181(13) -0.061(15) -0.021(9) -0.062(13) F2A 0.196(11) 0.133(9) 0.148(9) -0.034(7) -0.080(9) 0.002(7) F3A 0.280(18) 0.173(12) 0.244(16) 0.071(12) -0.166(14) -0.067(12) O3B 0.057(5) 0.069(6) 0.080(6) -0.015(5) -0.017(4) 0.002(4) O4B 0.064(6) 0.067(6) 0.079(6) -0.010(5) -0.009(4) -0.001(4) C14B 0.067(10) 0.080(10) 0.062(9) 0.004(8) -0.007(7) 0.019(8) C15B 0.039(8) 0.090(10) 0.082(9) -0.012(8) 0.000(7) 0.006(7) C16B 0.079(11) 0.051(8) 0.064(8) 0.014(7) -0.003(7) -0.020(7) C17B 0.060(10) 0.095(11) 0.113(12) 0.038(10) 0.031(9) -0.008(8) C18B 0.21(2) 0.25(3) 0.145(18) -0.055(18) 0.060(17) -0.15(2) C19B 0.106(14) 0.129(15) 0.188(19) -0.090(14) -0.016(13) -0.013(11) C20B 0.136(17) 0.137(17) 0.26(3) -0.046(17) -0.087(18) 0.010(14) O4C 0.095(7) 0.072(6) 0.091(7) 0.014(5) -0.014(6) -0.004(5) O3C 0.084(7) 0.091(7) 0.116(8) 0.031(6) 0.005(6) -0.022(6) C13C 0.099(19) 0.22(3) 0.16(2) 0.03(2) 0.004(17) -0.084(19) C14C 0.108(14) 0.071(11) 0.116(14) 0.001(10) 0.027(11) -0.029(10) C15C 0.122(16) 0.106(13) 0.103(13) 0.047(11) 0.003(12) -0.004(12) C16C 0.088(12) 0.069(10) 0.107(13) 0.000(9) -0.007(10) 0.006(9) C17C 0.102(14) 0.075(10) 0.122(14) 0.041(10) -0.002(11) 0.018(9) C18C 0.31(3) 0.118(16) 0.22(2) 0.020(16) -0.15(2) 0.055(18) C19C 0.069(15) 0.64(6) 0.17(2) 0.18(3) -0.015(14) 0.00(3) C20C 0.20(2) 0.33(3) 0.119(17) -0.06(2) -0.066(16) 0.12(2) F1C 0.33(3) 0.38(3) 0.209(16) 0.085(17) -0.077(17) -0.29(2) F2C 0.28(2) 0.193(14) 0.297(19) 0.140(15) -0.036(14) -0.112(14) F3C 0.129(13) 0.27(2) 0.52(4) 0.00(2) 0.157(19) -0.056(13) F1E 0.161(10) 0.156(9) 0.133(8) 0.036(7) -0.047(8) -0.087(8) F2E 0.065(7) 0.192(12) 0.269(15) -0.032(10) 0.052(8) -0.020(7) C13E 0.071(13) 0.110(14) 0.134(16) 0.056(13) -0.006(11) -0.036(11) F3E 0.164(10) 0.193(11) 0.158(9) 0.070(9) -0.023(7) -0.101(9) _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 Yb2 O4E 2.249(8) . ? Yb2 O4F 2.260(9) . ? Yb2 O3E 2.262(8) . ? Yb2 O3F 2.270(9) . ? Yb2 O5D 2.271(8) . ? Yb2 O4D 2.274(8) . ? Yb2 N1B 2.35(2) . ? Yb2 N2B 2.39(4) . ? Yb2 N2A 2.48(3) . ? Yb2 N1A 2.81(3) . ? Yb2 C11B 3.00(3) . ? Yb2 C1B 3.19(9) . ? Yb1 O4C 2.264(9) . ? Yb1 O3C 2.268(9) . ? Yb1 O3B 2.273(8) . ? Yb1 O4B 2.283(8) . ? Yb1 O3A 2.291(9) . ? Yb1 O4A 2.301(9) . ? Yb1 N2 2.486(10) . ? Yb1 N1 2.524(11) . ? N1 C1 1.319(16) . ? N1 C12 1.321(16) . ? N2 C11 1.313(17) . ? N2 C10 1.320(15) . ? N3 O2 1.14(2) . ? N3 O1 1.21(2) . ? N3 C5 1.49(2) . ? C1 C2 1.42(2) . ? C1 H1 0.9300 . ? C2 C3 1.29(2) . ? C2 H2 0.9300 . ? C3 C4 1.37(2) . ? C3 H3 0.9300 . ? C4 C12 1.398(18) . ? C4 C5 1.48(2) . ? C5 C6 1.35(2) . ? C6 C7 1.400(2) . ? C6 H6 0.9300 . ? C7 C8 1.41(2) . ? C7 C11 1.47(2) . ? C8 C9 1.34(2) . ? C8 H8 0.9300 . ? C9 C10 1.394(19) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.459(19) . ? C13B F1B 1.322(18) . ? C13B F3B 1.347(17) . ? C13B F2B 1.357(16) . ? C13B C14B 1.480(19) . ? O4D C14D 1.238(13) . ? O5D C16D 1.283(13) . ? C13D C20D 1.4001(10) . ? C13D C18D 1.52(2) . ? C13D C19D 1.52(2) . ? C13D C14D 1.544(17) . ? C14D C15D 1.405(15) . ? C15D C16D 1.329(15) . ? C15D H15D 0.9300 . ? C16D C17D 1.536(17) . ? C17D F1D 1.25(2) . ? C17D F2D 1.300(17) . ? C17D F3D 1.328(18) . ? C18D H18A 0.9600 . ? C18D H18B 0.9600 . ? C18D H18C 0.9600 . ? C19D H19A 0.9600 . ? C19D H19B 0.9600 . ? C19D H19C 0.9600 . ? C20D H20A 0.9600 . ? C20D H20B 0.9600 . ? C20D H20C 0.9600 . ? O3E C16E 1.216(15) . ? O4E C14E 1.277(13) . ? C14E C15E 1.376(17) . ? C14E C13E 1.496(19) . ? C15E C16E 1.437(18) . ? C15E H15E 0.9300 . ? C16E C17E 1.522(17) . ? C17E C19E 1.37(2) . ? C17E C20E 1.39(2) . ? C17E C18E 1.40(2) . ? C18E H18D 0.9600 . ? C18E H18E 0.9600 . ? C18E H18F 0.9600 . ? C19E H19D 0.9600 . ? C19E H19E 0.9600 . ? C19E H19F 0.9600 . ? C20E H20D 0.9600 . ? C20E H20E 0.9600 . ? C20E H20F 0.9600 . ? O3F C14F 1.232(15) . ? O4F C16F 1.300(16) . ? C13F F1F 1.25(2) . ? C13F F2F 1.29(3) . ? C13F F3F 1.3499(10) . ? C13F C14F 1.50(2) . ? C14F C15F 1.398(19) . ? C15F C16F 1.441(19) . ? C15F H15F 0.9300 . ? C16F C17F 1.60(2) . ? C17F C20F 1.401(2) . ? C17F C18F 1.55(2) . ? C17F C19F 1.61(2) . ? C18F H18G 0.9600 . ? C18F H18H 0.9600 . ? C18F H18I 0.9600 . ? C19F H19G 0.9600 . ? C19F H19H 0.9600 . ? C19F H19I 0.9600 . ? C20F H20G 0.9600 . ? C20F H20H 0.9600 . ? C20F H20I 0.9600 . ? O3A C14A 1.271(11) . ? O4A C16A 1.264(12) . ? C13A F3A 1.223(17) . ? C13A F1A 1.304(19) . ? C13A F2A 1.332(18) . ? C13A C14A 1.504(9) . ? C15A C14A 1.356(9) . ? C15A C16A 1.366(9) . ? C15A H15A 0.9300 . ? C16A C17A 1.504(9) . ? C17A C20A 1.36(2) . ? C17A C19A 1.44(3) . ? C17A C18A 1.45(2) . ? C18A H18J 0.9600 . ? C18A H18K 0.9600 . ? C18A H18L 0.9600 . ? C19A H19J 0.9600 . ? C19A H19K 0.9600 . ? C19A H19L 0.9600 . ? C20A H20J 0.9600 . ? C20A H20K 0.9600 . ? C20A H20L 0.9600 . ? O3B C16B 1.248(13) . ? O4B C14B 1.243(13) . ? C14B C15B 1.377(16) . ? C15B C16B 1.430(16) . ? C15B H15B 0.9300 . ? C16B C17B 1.544(17) . ? C17B C18B 1.439(19) . ? C17B C20B 1.52(2) . ? C17B C19B 1.563(19) . ? C18B H18M 0.9600 . ? C18B H18N 0.9600 . ? C18B H18O 0.9600 . ? C19B H19M 0.9600 . ? C19B H19N 0.9600 . ? C19B H19O 0.9600 . ? C20B H20M 0.9600 . ? C20B H20N 0.9600 . ? C20B H20O 0.9600 . ? O4C C16C 1.223(16) . ? O3C C14C 1.303(17) . ? C13C F3C 1.25(3) . ? C13C F1C 1.26(3) . ? C13C F2C 1.31(3) . ? C13C C14C 1.53(2) . ? C14C C15C 1.38(2) . ? C15C C16C 1.37(2) . ? C15C H15C 0.9300 . ? C16C C17C 1.518(19) . ? C17C C19C 1.39(2) . ? C17C C18C 1.44(2) . ? C17C C20C 1.50(2) . ? C18C H18P 0.9600 . ? C18C H18Q 0.9600 . ? C18C H18R 0.9600 . ? C19C H19P 0.9600 . ? C19C H19Q 0.9600 . ? C19C H19R 0.9600 . ? C20C H20P 0.9600 . ? C20C H20Q 0.9600 . ? C20C H20R 0.9600 . ? F1E C13E 1.331(19) . ? F2E C13E 1.31(2) . ? C13E F3E 1.333(16) . ? O1A N3A 1.15(3) . ? O2A N3A 1.26(3) . ? N1A C1A 1.09(4) . ? N1A C12A 1.22(3) . ? N2A C10A 1.22(4) . ? N2A C11A 1.48(4) . ? N3A C6A 1.51(3) . ? C1A C2A 1.44(4) . ? C1A H1A 0.9300 . ? C2A C3A 1.22(3) . ? C2A H2A 0.9300 . ? C3A C4A 1.40(4) . ? C3A H3A 0.9300 . ? C4A C5A 1.30(3) . ? C4A C12A 1.54(3) . ? C5A C6A 1.52(4) . ? C5A H5A 0.9300 . ? C6A C7A 1.25(3) . ? C7A C11A 1.39(3) . ? C7A C8A 1.53(3) . ? C8A C9A 1.50(4) . ? C8A H8A 0.9300 . ? C9A C10A 1.25(4) . ? C9A H9A 0.9300 . ? C10A H10A 0.9300 . ? C11A C12A 1.56(3) . ? O1B N3B 1.09(6) . ? O1B O2B 1.65(9) . ? O2B N3B 1.35(7) . ? N1B C1B 1.42(10) . ? N1B C12B 1.54(4) . ? N2B C11B 1.15(5) . ? N2B C10B 1.30(5) . ? N3B C5B 1.68(6) . ? C1B C2B 1.26(8) . ? C1B H1B 0.9300 . ? C2B C3B 1.32(6) . ? C2B H2B 0.9300 . ? C3B C4B 1.38(5) . ? C3B H3B 0.9300 . ? C4B C12B 1.24(5) . ? C4B C5B 1.58(5) . ? C5B C6B 1.68(5) . ? C6B C7B 1.400(10) . ? C6B H6B 0.9300 . ? C7B C8B 1.396(10) . ? C7B C11B 1.404(10) . ? C8B C9B 1.42(5) . ? C8B H8B 0.9300 . ? C9B C10B 1.37(4) . ? C9B H9B 0.9300 . ? C10B H10B 0.9300 . ? C11B C12B 1.50(4) . ? 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 O4E Yb2 O4F 116.6(3) . . ? O4E Yb2 O3E 74.0(3) . . ? O4F Yb2 O3E 71.1(3) . . ? O4E Yb2 O3F 76.4(3) . . ? O4F Yb2 O3F 75.1(3) . . ? O3E Yb2 O3F 117.1(3) . . ? O4E Yb2 O5D 82.5(3) . . ? O4F Yb2 O5D 147.0(3) . . ? O3E Yb2 O5D 141.9(3) . . ? O3F Yb2 O5D 84.8(3) . . ? O4E Yb2 O4D 147.9(3) . . ? O4F Yb2 O4D 76.2(3) . . ? O3E Yb2 O4D 136.8(3) . . ? O3F Yb2 O4D 79.3(3) . . ? O5D Yb2 O4D 74.6(3) . . ? O4E Yb2 N1B 81.0(6) . . ? O4F Yb2 N1B 133.0(6) . . ? O3E Yb2 N1B 73.5(5) . . ? O3F Yb2 N1B 150.4(6) . . ? O5D Yb2 N1B 73.5(5) . . ? O4D Yb2 N1B 112.8(6) . . ? O4E Yb2 N2B 144.0(9) . . ? O4F Yb2 N2B 71.6(10) . . ? O3E Yb2 N2B 76.6(9) . . ? O3F Yb2 N2B 136.7(10) . . ? O5D Yb2 N2B 109.6(9) . . ? O4D Yb2 N2B 66.7(9) . . ? N1B Yb2 N2B 71.0(11) . . ? O4E Yb2 N2A 132.1(7) . . ? O4F Yb2 N2A 82.0(7) . . ? O3E Yb2 N2A 71.6(6) . . ? O3F Yb2 N2A 150.1(7) . . ? O5D Yb2 N2A 105.5(6) . . ? O4D Yb2 N2A 76.7(7) . . ? N1B Yb2 N2A 57.9(9) . . ? N2B Yb2 N2A 13.4(11) . . ? O4E Yb2 N1A 72.5(6) . . ? O4F Yb2 N1A 139.2(6) . . ? O3E Yb2 N1A 74.4(5) . . ? O3F Yb2 N1A 142.0(7) . . ? O5D Yb2 N1A 70.1(6) . . ? O4D Yb2 N1A 118.5(5) . . ? N1B Yb2 N1A 9.0(8) . . ? N2B Yb2 N1A 80.0(11) . . ? N2A Yb2 N1A 66.8(9) . . ? O4E Yb2 C11B 124.9(6) . . ? O4F Yb2 C11B 87.6(6) . . ? O3E Yb2 C11B 68.6(5) . . ? O3F Yb2 C11B 157.6(6) . . ? O5D Yb2 C11B 103.5(5) . . ? O4D Yb2 C11B 82.9(6) . . ? N1B Yb2 C11B 50.8(8) . . ? N2B Yb2 C11B 20.8(10) . . ? N2A Yb2 C11B 7.5(10) . . ? N1A Yb2 C11B 59.6(8) . . ? O4E Yb2 C1B 61.3(18) . . ? O4F Yb2 C1B 152.2(17) . . ? O3E Yb2 C1B 82.4(17) . . ? O3F Yb2 C1B 126.5(18) . . ? O5D Yb2 C1B 59.9(17) . . ? O4D Yb2 C1B 121.4(17) . . ? N1B Yb2 C1B 24.0(18) . . ? N2B Yb2 C1B 95(2) . . ? N2A Yb2 C1B 81.8(19) . . ? N1A Yb2 C1B 15.5(18) . . ? C11B Yb2 C1B 74.8(19) . . ? O4C Yb1 O3C 74.6(3) . . ? O4C Yb1 O3B 73.3(3) . . ? O3C Yb1 O3B 124.0(3) . . ? O4C Yb1 O4B 110.6(3) . . ? O3C Yb1 O4B 76.4(3) . . ? O3B Yb1 O4B 73.7(3) . . ? O4C Yb1 O3A 142.4(3) . . ? O3C Yb1 O3A 75.7(3) . . ? O3B Yb1 O3A 143.9(3) . . ? O4B Yb1 O3A 84.0(3) . . ? O4C Yb1 O4A 78.0(3) . . ? O3C Yb1 O4A 80.7(3) . . ? O3B Yb1 O4A 133.4(3) . . ? O4B Yb1 O4A 152.1(3) . . ? O3A Yb1 O4A 74.9(3) . . ? O4C Yb1 N2 141.8(4) . . ? O3C Yb1 N2 142.5(4) . . ? O3B Yb1 N2 75.0(3) . . ? O4B Yb1 N2 79.8(3) . . ? O3A Yb1 N2 73.3(3) . . ? O4A Yb1 N2 110.4(3) . . ? O4C Yb1 N1 84.9(4) . . ? O3C Yb1 N1 148.2(4) . . ? O3B Yb1 N1 70.4(3) . . ? O4B Yb1 N1 134.5(3) . . ? O3A Yb1 N1 110.0(3) . . ? O4A Yb1 N1 71.2(4) . . ? N2 Yb1 N1 64.6(4) . . ? C1 N1 C12 118.9(14) . . ? C1 N1 Yb1 121.2(11) . . ? C12 N1 Yb1 119.7(10) . . ? C11 N2 C10 117.2(13) . . ? C11 N2 Yb1 119.8(10) . . ? C10 N2 Yb1 122.6(10) . . ? O2 N3 O1 124(2) . . ? O2 N3 C5 120(2) . . ? O1 N3 C5 112(2) . . ? N1 C1 C2 118.0(16) . . ? N1 C1 H1 121.0 . . ? C2 C1 H1 121.0 . . ? C3 C2 C1 124.2(18) . . ? C3 C2 H2 117.9 . . ? C1 C2 H2 117.9 . . ? C2 C3 C4 117.5(19) . . ? C2 C3 H3 121.2 . . ? C4 C3 H3 121.2 . . ? C3 C4 C12 118.0(17) . . ? C3 C4 C5 124.1(18) . . ? C12 C4 C5 117.9(17) . . ? C6 C5 C4 120.4(16) . . ? C6 C5 N3 116.4(18) . . ? C4 C5 N3 123.3(19) . . ? C5 C6 C7 124.7(19) . . ? C5 C6 H6 117.6 . . ? C7 C6 H6 117.6 . . ? C6 C7 C8 128(2) . . ? C6 C7 C11 116.5(19) . . ? C8 C7 C11 115.9(16) . . ? C9 C8 C7 122.9(19) . . ? C9 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? C8 C9 C10 114.4(18) . . ? C8 C9 H9 122.8 . . ? C10 C9 H9 122.8 . . ? N2 C10 C9 128.2(16) . . ? N2 C10 H10 115.9 . . ? C9 C10 H10 115.9 . . ? N2 C11 C12 119.0(14) . . ? N2 C11 C7 121.2(16) . . ? C12 C11 C7 119.8(17) . . ? N1 C12 C4 123.3(16) . . ? N1 C12 C11 116.1(14) . . ? C4 C12 C11 120.5(17) . . ? F1B C13B F3B 106.2(15) . . ? F1B C13B F2B 103.7(12) . . ? F3B C13B F2B 103.1(14) . . ? F1B C13B C14B 112.6(15) . . ? F3B C13B C14B 118.5(14) . . ? F2B C13B C14B 111.4(14) . . ? C14D O4D Yb2 134.6(8) . . ? C16D O5D Yb2 133.2(8) . . ? C20D C13D C18D 105(2) . . ? C20D C13D C19D 113.6(19) . . ? C18D C13D C19D 101.1(17) . . ? C20D C13D C14D 110.9(13) . . ? C18D C13D C14D 115.4(13) . . ? C19D C13D C14D 110.7(15) . . ? O4D C14D C15D 125.4(11) . . ? O4D C14D C13D 114.4(12) . . ? C15D C14D C13D 120.1(11) . . ? C16D C15D C14D 122.3(11) . . ? C16D C15D H15D 118.8 . . ? C14D C15D H15D 118.8 . . ? O5D C16D C15D 128.1(12) . . ? O5D C16D C17D 109.7(12) . . ? C15D C16D C17D 121.9(13) . . ? F1D C17D F2D 110.0(16) . . ? F1D C17D F3D 107.4(16) . . ? F2D C17D F3D 105.7(16) . . ? F1D C17D C16D 114.5(16) . . ? F2D C17D C16D 111.3(14) . . ? F3D C17D C16D 107.4(14) . . ? C13D C18D H18A 109.5 . . ? C13D C18D H18B 109.5 . . ? H18A C18D H18B 109.5 . . ? C13D C18D H18C 109.5 . . ? H18A C18D H18C 109.5 . . ? H18B C18D H18C 109.5 . . ? C13D C19D H19A 109.5 . . ? C13D C19D H19B 109.5 . . ? H19A C19D H19B 109.5 . . ? C13D C19D H19C 109.5 . . ? H19A C19D H19C 109.5 . . ? H19B C19D H19C 109.5 . . ? C13D C20D H20A 109.5 . . ? C13D C20D H20B 109.5 . . ? H20A C20D H20B 109.5 . . ? C13D C20D H20C 109.5 . . ? H20A C20D H20C 109.5 . . ? H20B C20D H20C 109.5 . . ? C16E O3E Yb2 141.2(9) . . ? C14E O4E Yb2 133.9(8) . . ? O4E C14E C15E 127.0(13) . . ? O4E C14E C13E 110.6(13) . . ? C15E C14E C13E 122.1(14) . . ? C14E C15E C16E 123.7(13) . . ? C14E C15E H15E 118.2 . . ? C16E C15E H15E 118.2 . . ? O3E C16E C15E 120.0(13) . . ? O3E C16E C17E 123.1(14) . . ? C15E C16E C17E 116.8(14) . . ? C19E C17E C20E 114(2) . . ? C19E C17E C18E 114(2) . . ? C20E C17E C18E 99.0(19) . . ? C19E C17E C16E 109.3(13) . . ? C20E C17E C16E 114.1(15) . . ? C18E C17E C16E 106.8(14) . . ? C17E C18E H18D 109.5 . . ? C17E C18E H18E 109.5 . . ? H18D C18E H18E 109.5 . . ? C17E C18E H18F 109.5 . . ? H18D C18E H18F 109.5 . . ? H18E C18E H18F 109.5 . . ? C17E C19E H19D 109.5 . . ? C17E C19E H19E 109.5 . . ? H19D C19E H19E 109.5 . . ? C17E C19E H19F 109.5 . . ? H19D C19E H19F 109.5 . . ? H19E C19E H19F 109.5 . . ? C17E C20E H20D 109.5 . . ? C17E C20E H20E 109.5 . . ? H20D C20E H20E 109.5 . . ? C17E C20E H20F 109.5 . . ? H20D C20E H20F 109.5 . . ? H20E C20E H20F 109.5 . . ? C14F O3F Yb2 135.1(10) . . ? C16F O4F Yb2 138.3(9) . . ? F1F C13F F2F 112.6(19) . . ? F1F C13F F3F 103.5(18) . . ? F2F C13F F3F 105(2) . . ? F1F C13F C14F 113(2) . . ? F2F C13F C14F 110.9(19) . . ? F3F C13F C14F 110.9(15) . . ? O3F C14F C15F 126.7(15) . . ? O3F C14F C13F 112.6(14) . . ? C15F C14F C13F 120.7(15) . . ? C14F C15F C16F 124.8(15) . . ? C14F C15F H15F 117.6 . . ? C16F C15F H15F 117.6 . . ? O4F C16F C15F 119.6(15) . . ? O4F C16F C17F 125.6(14) . . ? C15F C16F C17F 114.7(15) . . ? C20F C17F C18F 106.7(18) . . ? C20F C17F C16F 123.1(16) . . ? C18F C17F C16F 99.4(13) . . ? C20F C17F C19F 117.1(19) . . ? C18F C17F C19F 108.1(17) . . ? C16F C17F C19F 100.6(13) . . ? C17F C18F H18G 109.5 . . ? C17F C18F H18H 109.5 . . ? H18G C18F H18H 109.5 . . ? C17F C18F H18I 109.5 . . ? H18G C18F H18I 109.5 . . ? H18H C18F H18I 109.5 . . ? C17F C19F H19G 109.5 . . ? C17F C19F H19H 109.5 . . ? H19G C19F H19H 109.5 . . ? C17F C19F H19I 109.5 . . ? H19G C19F H19I 109.5 . . ? H19H C19F H19I 109.5 . . ? C17F C20F H20G 109.5 . . ? C17F C20F H20H 109.5 . . ? H20G C20F H20H 109.5 . . ? C17F C20F H20I 109.5 . . ? H20G C20F H20I 109.5 . . ? H20H C20F H20I 109.5 . . ? C14A O3A Yb1 129.4(8) . . ? C16A O4A Yb1 137.6(8) . . ? F3A C13A F1A 112(2) . . ? F3A C13A F2A 101.5(15) . . ? F1A C13A F2A 101.5(14) . . ? F3A C13A C14A 114.8(14) . . ? F1A C13A C14A 113.2(15) . . ? F2A C13A C14A 112.7(16) . . ? C14A C15A C16A 127.1(13) . . ? C14A C15A H15A 116.5 . . ? C16A C15A H15A 116.5 . . ? O3A C14A C15A 129.3(12) . . ? O3A C14A C13A 108.4(12) . . ? C15A C14A C13A 122.2(14) . . ? O4A C16A C15A 119.7(12) . . ? O4A C16A C17A 118.1(12) . . ? C15A C16A C17A 122.2(13) . . ? C20A C17A C19A 102(3) . . ? C20A C17A C18A 121(2) . . ? C19A C17A C18A 94(2) . . ? C20A C17A C16A 113.5(15) . . ? C19A C17A C16A 109(2) . . ? C18A C17A C16A 113.6(16) . . ? C17A C18A H18J 109.5 . . ? C17A C18A H18K 109.5 . . ? H18J C18A H18K 109.5 . . ? C17A C18A H18L 109.5 . . ? H18J C18A H18L 109.5 . . ? H18K C18A H18L 109.5 . . ? C17A C19A H19J 109.5 . . ? C17A C19A H19K 109.5 . . ? H19J C19A H19K 109.5 . . ? C17A C19A H19L 109.5 . . ? H19J C19A H19L 109.5 . . ? H19K C19A H19L 109.5 . . ? C17A C20A H20J 109.5 . . ? C17A C20A H20K 109.5 . . ? H20J C20A H20K 109.5 . . ? C17A C20A H20L 109.5 . . ? H20J C20A H20L 109.5 . . ? H20K C20A H20L 109.5 . . ? C16B O3B Yb1 138.9(8) . . ? C14B O4B Yb1 132.2(8) . . ? O4B C14B C15B 131.8(13) . . ? O4B C14B C13B 113.5(13) . . ? C15B C14B C13B 114.7(13) . . ? C14B C15B C16B 119.0(12) . . ? C14B C15B H15B 120.5 . . ? C16B C15B H15B 120.5 . . ? O3B C16B C15B 123.6(11) . . ? O3B C16B C17B 117.3(12) . . ? C15B C16B C17B 119.1(12) . . ? C18B C17B C20B 104.4(16) . . ? C18B C17B C16B 103.9(13) . . ? C20B C17B C16B 108.5(12) . . ? C18B C17B C19B 115.1(15) . . ? C20B C17B C19B 109.7(14) . . ? C16B C17B C19B 114.5(12) . . ? C17B C18B H18M 109.5 . . ? C17B C18B H18N 109.5 . . ? H18M C18B H18N 109.5 . . ? C17B C18B H18O 109.5 . . ? H18M C18B H18O 109.5 . . ? H18N C18B H18O 109.5 . . ? C17B C19B H19M 109.5 . . ? C17B C19B H19N 109.5 . . ? H19M C19B H19N 109.5 . . ? C17B C19B H19O 109.5 . . ? H19M C19B H19O 109.5 . . ? H19N C19B H19O 109.5 . . ? C17B C20B H20M 109.5 . . ? C17B C20B H20N 109.5 . . ? H20M C20B H20N 109.5 . . ? C17B C20B H20O 109.5 . . ? H20M C20B H20O 109.5 . . ? H20N C20B H20O 109.5 . . ? C16C O4C Yb1 138.5(10) . . ? C14C O3C Yb1 130.7(10) . . ? F3C C13C F1C 109(3) . . ? F3C C13C F2C 101(2) . . ? F1C C13C F2C 104(3) . . ? F3C C13C C14C 113(3) . . ? F1C C13C C14C 113(2) . . ? F2C C13C C14C 117(2) . . ? O3C C14C C15C 127.3(14) . . ? O3C C14C C13C 111.3(18) . . ? C15C C14C C13C 121.3(19) . . ? C16C C15C C14C 123.6(15) . . ? C16C C15C H15C 118.2 . . ? C14C C15C H15C 118.2 . . ? O4C C16C C15C 123.2(15) . . ? O4C C16C C17C 119.5(15) . . ? C15C C16C C17C 117.2(16) . . ? C19C C17C C18C 108.5(19) . . ? C19C C17C C20C 104(2) . . ? C18C C17C C20C 109.4(18) . . ? C19C C17C C16C 112.8(15) . . ? C18C C17C C16C 115.4(15) . . ? C20C C17C C16C 105.7(13) . . ? C17C C18C H18P 109.5 . . ? C17C C18C H18Q 109.5 . . ? H18P C18C H18Q 109.5 . . ? C17C C18C H18R 109.5 . . ? H18P C18C H18R 109.5 . . ? H18Q C18C H18R 109.5 . . ? C17C C19C H19P 109.5 . . ? C17C C19C H19Q 109.5 . . ? H19P C19C H19Q 109.5 . . ? C17C C19C H19R 109.5 . . ? H19P C19C H19R 109.5 . . ? H19Q C19C H19R 109.5 . . ? C17C C20C H20P 109.5 . . ? C17C C20C H20Q 109.5 . . ? H20P C20C H20Q 109.5 . . ? C17C C20C H20R 109.5 . . ? H20P C20C H20R 109.5 . . ? H20Q C20C H20R 109.5 . . ? F2E C13E F1E 106.3(15) . . ? F2E C13E F3E 108.3(16) . . ? F1E C13E F3E 103.3(15) . . ? F2E C13E C14E 116.8(16) . . ? F1E C13E C14E 109.9(16) . . ? F3E C13E C14E 111.4(14) . . ? C1A N1A C12A 130(3) . . ? C1A N1A Yb2 119(2) . . ? C12A N1A Yb2 110(2) . . ? C10A N2A C11A 109(3) . . ? C10A N2A Yb2 130(3) . . ? C11A N2A Yb2 119.3(17) . . ? O1A N3A O2A 130(3) . . ? O1A N3A C6A 124(2) . . ? O2A N3A C6A 105(2) . . ? N1A C1A C2A 122(3) . . ? N1A C1A H1A 118.8 . . ? C2A C1A H1A 118.8 . . ? C3A C2A C1A 114(3) . . ? C3A C2A H2A 123.2 . . ? C1A C2A H2A 123.2 . . ? C2A C3A C4A 129(2) . . ? C2A C3A H3A 115.4 . . ? C4A C3A H3A 115.4 . . ? C5A C4A C3A 134(2) . . ? C5A C4A C12A 120(3) . . ? C3A C4A C12A 106(2) . . ? C4A C5A C6A 123(3) . . ? C4A C5A H5A 118.3 . . ? C6A C5A H5A 118.3 . . ? C7A C6A N3A 137(3) . . ? C7A C6A C5A 116(3) . . ? N3A C6A C5A 108(2) . . ? C6A C7A C11A 132(3) . . ? C6A C7A C8A 121(3) . . ? C11A C7A C8A 107(2) . . ? C9A C8A C7A 119(3) . . ? C9A C8A H8A 120.7 . . ? C7A C8A H8A 120.7 . . ? C10A C9A C8A 117(4) . . ? C10A C9A H9A 121.4 . . ? C8A C9A H9A 121.4 . . ? N2A C10A C9A 136(4) . . ? N2A C10A H10A 112.2 . . ? C9A C10A H10A 112.2 . . ? C7A C11A N2A 132(2) . . ? C7A C11A C12A 115(2) . . ? N2A C11A C12A 113.2(18) . . ? N1A C12A C4A 118(2) . . ? N1A C12A C11A 128(2) . . ? C4A C12A C11A 114(2) . . ? N3B O1B O2B 54(4) . . ? N3B O2B O1B 41(3) . . ? C1B N1B C12B 129(4) . . ? C1B N1B Yb2 114(4) . . ? C12B N1B Yb2 116.9(17) . . ? C11B N2B C10B 123(4) . . ? C11B N2B Yb2 112(3) . . ? C10B N2B Yb2 125(3) . . ? O1B N3B O2B 85(6) . . ? O1B N3B C5B 109(6) . . ? O2B N3B C5B 89(4) . . ? C2B C1B N1B 100(8) . . ? C2B C1B Yb2 140(7) . . ? N1B C1B Yb2 42(3) . . ? C2B C1B H1B 130.1 . . ? N1B C1B H1B 130.1 . . ? Yb2 C1B H1B 88.9 . . ? C1B C2B C3B 143(9) . . ? C1B C2B H2B 108.6 . . ? C3B C2B H2B 108.6 . . ? C2B C3B C4B 108(6) . . ? C2B C3B H3B 126.0 . . ? C4B C3B H3B 126.0 . . ? C12B C4B C3B 132(5) . . ? C12B C4B C5B 107(4) . . ? C3B C4B C5B 121(5) . . ? C4B C5B C6B 113(3) . . ? C4B C5B N3B 123(4) . . ? C6B C5B N3B 122(4) . . ? C7B C6B C5B 117(3) . . ? C7B C6B H6B 121.5 . . ? C5B C6B H6B 121.5 . . ? C8B C7B C6B 113(3) . . ? C8B C7B C11B 116(3) . . ? C6B C7B C11B 131(3) . . ? C7B C8B C9B 120(3) . . ? C7B C8B H8B 119.8 . . ? C9B C8B H8B 119.8 . . ? C10B C9B C8B 112(4) . . ? C10B C9B H9B 124.2 . . ? C8B C9B H9B 124.2 . . ? N2B C10B C9B 125(4) . . ? N2B C10B H10B 117.5 . . ? C9B C10B H10B 117.5 . . ? N2B C11B C7B 124(3) . . ? N2B C11B C12B 136(4) . . ? C7B C11B C12B 101(3) . . ? N2B C11B Yb2 48(3) . . ? C7B C11B Yb2 166(2) . . ? C12B C11B Yb2 89.2(17) . . ? C4B C12B C11B 151(4) . . ? C4B C12B N1B 107(3) . . ? C11B C12B N1B 102(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4C Yb1 N1 C1 -26.4(10) . . . . ? O3C Yb1 N1 C1 23.1(14) . . . . ? O3B Yb1 N1 C1 -100.4(10) . . . . ? O4B Yb1 N1 C1 -140.4(9) . . . . ? O3A Yb1 N1 C1 118.0(10) . . . . ? O4A Yb1 N1 C1 52.6(10) . . . . ? N2 Yb1 N1 C1 177.3(11) . . . . ? O4C Yb1 N1 C12 148.4(10) . . . . ? O3C Yb1 N1 C12 -162.1(9) . . . . ? O3B Yb1 N1 C12 74.4(10) . . . . ? O4B Yb1 N1 C12 34.4(12) . . . . ? O3A Yb1 N1 C12 -67.1(10) . . . . ? O4A Yb1 N1 C12 -132.6(10) . . . . ? N2 Yb1 N1 C12 -7.8(9) . . . . ? O4C Yb1 N2 C11 -32.8(12) . . . . ? O3C Yb1 N2 C11 165.5(9) . . . . ? O3B Yb1 N2 C11 -67.5(10) . . . . ? O4B Yb1 N2 C11 -143.2(10) . . . . ? O3A Yb1 N2 C11 130.1(10) . . . . ? O4A Yb1 N2 C11 63.7(10) . . . . ? N1 Yb1 N2 C11 7.6(9) . . . . ? O4C Yb1 N2 C10 140.7(10) . . . . ? O3C Yb1 N2 C10 -21.0(13) . . . . ? O3B Yb1 N2 C10 106.0(10) . . . . ? O4B Yb1 N2 C10 30.3(10) . . . . ? O3A Yb1 N2 C10 -56.4(10) . . . . ? O4A Yb1 N2 C10 -122.8(10) . . . . ? N1 Yb1 N2 C10 -178.9(11) . . . . ? C12 N1 C1 C2 1(2) . . . . ? Yb1 N1 C1 C2 176.3(9) . . . . ? N1 C1 C2 C3 -1(2) . . . . ? C1 C2 C3 C4 0(3) . . . . ? C2 C3 C4 C12 0(3) . . . . ? C2 C3 C4 C5 -177.8(15) . . . . ? C3 C4 C5 C6 -177.3(16) . . . . ? C12 C4 C5 C6 5(2) . . . . ? C3 C4 C5 N3 1(2) . . . . ? C12 C4 C5 N3 -176.5(15) . . . . ? O2 N3 C5 C6 -22(3) . . . . ? O1 N3 C5 C6 138(2) . . . . ? O2 N3 C5 C4 159(2) . . . . ? O1 N3 C5 C4 -41(3) . . . . ? C4 C5 C6 C7 -3(2) . . . . ? N3 C5 C6 C7 178.3(16) . . . . ? C5 C6 C7 C8 179.4(16) . . . . ? C5 C6 C7 C11 2(2) . . . . ? C6 C7 C8 C9 -175.0(17) . . . . ? C11 C7 C8 C9 3(3) . . . . ? C7 C8 C9 C10 -5(3) . . . . ? C11 N2 C10 C9 0(2) . . . . ? Yb1 N2 C10 C9 -174.1(13) . . . . ? C8 C9 C10 N2 4(3) . . . . ? C10 N2 C11 C12 178.9(12) . . . . ? Yb1 N2 C11 C12 -7.2(16) . . . . ? C10 N2 C11 C7 -1.7(19) . . . . ? Yb1 N2 C11 C7 172.2(9) . . . . ? C6 C7 C11 N2 178.6(13) . . . . ? C8 C7 C11 N2 1(2) . . . . ? C6 C7 C11 C12 -2(2) . . . . ? C8 C7 C11 C12 179.9(13) . . . . ? C1 N1 C12 C4 -1(2) . . . . ? Yb1 N1 C12 C4 -176.4(10) . . . . ? C1 N1 C12 C11 -177.6(12) . . . . ? Yb1 N1 C12 C11 7.5(15) . . . . ? C3 C4 C12 N1 1(2) . . . . ? C5 C4 C12 N1 178.7(12) . . . . ? C3 C4 C12 C11 176.7(14) . . . . ? C5 C4 C12 C11 -5.4(19) . . . . ? N2 C11 C12 N1 -0.3(18) . . . . ? C7 C11 C12 N1 -179.7(12) . . . . ? N2 C11 C12 C4 -176.5(12) . . . . ? C7 C11 C12 C4 4.1(19) . . . . ? O4E Yb2 O4D C14D 32.3(17) . . . . ? O4F Yb2 O4D C14D 150.7(14) . . . . ? O3E Yb2 O4D C14D -167.9(12) . . . . ? O3F Yb2 O4D C14D 73.6(14) . . . . ? O5D Yb2 O4D C14D -13.9(13) . . . . ? N1B Yb2 O4D C14D -78.1(15) . . . . ? N2B Yb2 O4D C14D -133.7(17) . . . . ? N2A Yb2 O4D C14D -124.4(15) . . . . ? N1A Yb2 O4D C14D -70.4(15) . . . . ? C11B Yb2 O4D C14D -120.0(14) . . . . ? C1B Yb2 O4D C14D -53(2) . . . . ? O4E Yb2 O5D C16D -154.4(11) . . . . ? O4F Yb2 O5D C16D -25.5(14) . . . . ? O3E Yb2 O5D C16D 153.8(10) . . . . ? O3F Yb2 O5D C16D -77.4(11) . . . . ? O4D Yb2 O5D C16D 2.8(11) . . . . ? N1B Yb2 O5D C16D 122.9(12) . . . . ? N2B Yb2 O5D C16D 60.6(15) . . . . ? N2A Yb2 O5D C16D 73.9(13) . . . . ? N1A Yb2 O5D C16D 131.6(13) . . . . ? C11B Yb2 O5D C16D 81.4(12) . . . . ? C1B Yb2 O5D C16D 145(2) . . . . ? Yb2 O4D C14D C15D 19(2) . . . . ? Yb2 O4D C14D C13D -163.9(10) . . . . ? C20D C13D C14D O4D 112(2) . . . . ? C18D C13D C14D O4D -7(2) . . . . ? C19D C13D C14D O4D -121.4(18) . . . . ? C20D C13D C14D C15D -71(2) . . . . ? C18D C13D C14D C15D 169.7(18) . . . . ? C19D C13D C14D C15D 56(2) . . . . ? O4D C14D C15D C16D -9(2) . . . . ? C13D C14D C15D C16D 174.7(14) . . . . ? Yb2 O5D C16D C15D 3(2) . . . . ? Yb2 O5D C16D C17D -170.9(10) . . . . ? C14D C15D C16D O5D -2(2) . . . . ? C14D C15D C16D C17D 170.8(15) . . . . ? O5D C16D C17D F1D 47(2) . . . . ? C15D C16D C17D F1D -127.4(17) . . . . ? O5D C16D C17D F2D 172.5(15) . . . . ? C15D C16D C17D F2D -2(2) . . . . ? O5D C16D C17D F3D -72.3(18) . . . . ? C15D C16D C17D F3D 113.4(16) . . . . ? O4E Yb2 O3E C16E -4.3(14) . . . . ? O4F Yb2 O3E C16E -130.5(15) . . . . ? O3F Yb2 O3E C16E -69.3(15) . . . . ? O5D Yb2 O3E C16E 49.9(16) . . . . ? O4D Yb2 O3E C16E -173.2(13) . . . . ? N1B Yb2 O3E C16E 80.8(15) . . . . ? N2B Yb2 O3E C16E 154.7(18) . . . . ? N2A Yb2 O3E C16E 141.8(16) . . . . ? N1A Yb2 O3E C16E 71.5(16) . . . . ? C11B Yb2 O3E C16E 134.5(16) . . . . ? C1B Yb2 O3E C16E 58(2) . . . . ? O4F Yb2 O4E C14E 62.4(11) . . . . ? O3E Yb2 O4E C14E 3.8(11) . . . . ? O3F Yb2 O4E C14E 127.7(11) . . . . ? O5D Yb2 O4E C14E -145.9(11) . . . . ? O4D Yb2 O4E C14E 169.5(10) . . . . ? N1B Yb2 O4E C14E -71.5(12) . . . . ? N2B Yb2 O4E C14E -33(2) . . . . ? N2A Yb2 O4E C14E -41.7(14) . . . . ? N1A Yb2 O4E C14E -74.5(12) . . . . ? C11B Yb2 O4E C14E -44.6(13) . . . . ? C1B Yb2 O4E C14E -86(2) . . . . ? Yb2 O4E C14E C15E -3(2) . . . . ? Yb2 O4E C14E C13E -176.4(11) . . . . ? O4E C14E C15E C16E -1(2) . . . . ? C13E C14E C15E C16E 172.0(16) . . . . ? Yb2 O3E C16E C15E 3(2) . . . . ? Yb2 O3E C16E C17E -173.0(10) . . . . ? C14E C15E C16E O3E 1(2) . . . . ? C14E C15E C16E C17E 177.3(14) . . . . ? O3E C16E C17E C19E 94(2) . . . . ? C15E C16E C17E C19E -82(2) . . . . ? O3E C16E C17E C20E -138(2) . . . . ? C15E C16E C17E C20E 46(3) . . . . ? O3E C16E C17E C18E -29(2) . . . . ? C15E C16E C17E C18E 154.6(19) . . . . ? O4E Yb2 O3F C14F -130.6(14) . . . . ? O4F Yb2 O3F C14F -7.8(13) . . . . ? O3E Yb2 O3F C14F -66.9(14) . . . . ? O5D Yb2 O3F C14F 145.9(14) . . . . ? O4D Yb2 O3F C14F 70.6(13) . . . . ? N1B Yb2 O3F C14F -171.7(15) . . . . ? N2B Yb2 O3F C14F 33(2) . . . . ? N2A Yb2 O3F C14F 34(2) . . . . ? N1A Yb2 O3F C14F -166.4(14) . . . . ? C11B Yb2 O3F C14F 33(2) . . . . ? C1B Yb2 O3F C14F -168(2) . . . . ? O4E Yb2 O4F C16F 70.6(14) . . . . ? O3E Yb2 O4F C16F 130.7(14) . . . . ? O3F Yb2 O4F C16F 4.5(13) . . . . ? O5D Yb2 O4F C16F -49.7(16) . . . . ? O4D Yb2 O4F C16F -77.9(13) . . . . ? N1B Yb2 O4F C16F 173.7(14) . . . . ? N2B Yb2 O4F C16F -147.5(16) . . . . ? N2A Yb2 O4F C16F -156.0(15) . . . . ? N1A Yb2 O4F C16F 164.3(14) . . . . ? C11B Yb2 O4F C16F -161.1(14) . . . . ? C1B Yb2 O4F C16F 149(4) . . . . ? Yb2 O3F C14F C15F 7(2) . . . . ? Yb2 O3F C14F C13F -173.9(14) . . . . ? F1F C13F C14F O3F 59(2) . . . . ? F2F C13F C14F O3F -69(2) . . . . ? F3F C13F C14F O3F 175(2) . . . . ? F1F C13F C14F C15F -121.7(17) . . . . ? F2F C13F C14F C15F 110.7(18) . . . . ? F3F C13F C14F C15F -6(3) . . . . ? O3F C14F C15F C16F 1(3) . . . . ? C13F C14F C15F C16F -177.7(19) . . . . ? Yb2 O4F C16F C15F 0(2) . . . . ? Yb2 O4F C16F C17F 177.1(11) . . . . ? C14F C15F C16F O4F -4(2) . . . . ? C14F C15F C16F C17F 177.8(15) . . . . ? O4F C16F C17F C20F -146(2) . . . . ? C15F C16F C17F C20F 32(3) . . . . ? O4F C16F C17F C18F 97.0(18) . . . . ? C15F C16F C17F C18F -85.5(16) . . . . ? O4F C16F C17F C19F -14(2) . . . . ? C15F C16F C17F C19F 164.0(16) . . . . ? O4C Yb1 O3A C14A 31.4(14) . . . . ? O3C Yb1 O3A C14A 70.1(11) . . . . ? O3B Yb1 O3A C14A -160.8(10) . . . . ? O4B Yb1 O3A C14A 147.6(11) . . . . ? O4A Yb1 O3A C14A -13.9(11) . . . . ? N2 Yb1 O3A C14A -131.2(12) . . . . ? N1 Yb1 O3A C14A -77.0(12) . . . . ? O4C Yb1 O4A C16A -139.4(16) . . . . ? O3C Yb1 O4A C16A -63.3(15) . . . . ? O3B Yb1 O4A C16A 167.9(14) . . . . ? O4B Yb1 O4A C16A -27.9(19) . . . . ? O3A Yb1 O4A C16A 14.2(15) . . . . ? N2 Yb1 O4A C16A 79.6(16) . . . . ? N1 Yb1 O4A C16A 131.9(16) . . . . ? Yb1 O3A C14A C15A 11(2) . . . . ? Yb1 O3A C14A C13A -166.6(10) . . . . ? C16A C15A C14A O3A 3(3) . . . . ? C16A C15A C14A C13A -180.0(18) . . . . ? F3A C13A C14A O3A -51(2) . . . . ? F1A C13A C14A O3A 79(2) . . . . ? F2A C13A C14A O3A -166.6(14) . . . . ? F3A C13A C14A C15A 132(2) . . . . ? F1A C13A C14A C15A -98(2) . . . . ? F2A C13A C14A C15A 16(2) . . . . ? Yb1 O4A C16A C15A -8(3) . . . . ? Yb1 O4A C16A C17A 169.5(13) . . . . ? C14A C15A C16A O4A -5(3) . . . . ? C14A C15A C16A C17A 177.4(18) . . . . ? O4A C16A C17A C20A 9(3) . . . . ? C15A C16A C17A C20A -173(3) . . . . ? O4A C16A C17A C19A 122(3) . . . . ? C15A C16A C17A C19A -60(3) . . . . ? O4A C16A C17A C18A -134(3) . . . . ? C15A C16A C17A C18A 44(3) . . . . ? O4C Yb1 O3B C16B 112.5(12) . . . . ? O3C Yb1 O3B C16B 55.0(13) . . . . ? O4B Yb1 O3B C16B -5.5(11) . . . . ? O3A Yb1 O3B C16B -59.7(14) . . . . ? O4A Yb1 O3B C16B 166.8(11) . . . . ? N2 Yb1 O3B C16B -89.1(12) . . . . ? N1 Yb1 O3B C16B -157.0(13) . . . . ? O4C Yb1 O4B C14B -54.7(12) . . . . ? O3C Yb1 O4B C14B -122.2(11) . . . . ? O3B Yb1 O4B C14B 9.8(11) . . . . ? O3A Yb1 O4B C14B 161.1(11) . . . . ? O4A Yb1 O4B C14B -158.2(10) . . . . ? N2 Yb1 O4B C14B 87.0(11) . . . . ? N1 Yb1 O4B C14B 48.9(13) . . . . ? Yb1 O4B C14B C15B -13(2) . . . . ? Yb1 O4B C14B C13B 171.2(10) . . . . ? F1B C13B C14B O4B -51.0(18) . . . . ? F3B C13B C14B O4B -175.7(14) . . . . ? F2B C13B C14B O4B 65.0(18) . . . . ? F1B C13B C14B C15B 132.2(14) . . . . ? F3B C13B C14B C15B 7(2) . . . . ? F2B C13B C14B C15B -111.8(15) . . . . ? O4B C14B C15B C16B 5(2) . . . . ? C13B C14B C15B C16B -178.6(12) . . . . ? Yb1 O3B C16B C15B 2.4(19) . . . . ? Yb1 O3B C16B C17B -178.8(8) . . . . ? C14B C15B C16B O3B 0.3(19) . . . . ? C14B C15B C16B C17B -178.5(11) . . . . ? O3B C16B C17B C18B -66.0(17) . . . . ? C15B C16B C17B C18B 112.9(16) . . . . ? O3B C16B C17B C20B 44.7(17) . . . . ? C15B C16B C17B C20B -136.4(14) . . . . ? O3B C16B C17B C19B 167.6(12) . . . . ? C15B C16B C17B C19B -13.6(17) . . . . ? O3C Yb1 O4C C16C -10.8(14) . . . . ? O3B Yb1 O4C C16C -144.4(15) . . . . ? O4B Yb1 O4C C16C -79.5(15) . . . . ? O3A Yb1 O4C C16C 28.1(17) . . . . ? O4A Yb1 O4C C16C 72.7(15) . . . . ? N2 Yb1 O4C C16C -179.4(13) . . . . ? N1 Yb1 O4C C16C 144.6(15) . . . . ? O4C Yb1 O3C C14C 15.2(12) . . . . ? O3B Yb1 O3C C14C 72.1(13) . . . . ? O4B Yb1 O3C C14C 131.4(13) . . . . ? O3A Yb1 O3C C14C -141.5(13) . . . . ? O4A Yb1 O3C C14C -64.8(12) . . . . ? N2 Yb1 O3C C14C -176.4(11) . . . . ? N1 Yb1 O3C C14C -36.6(16) . . . . ? Yb1 O3C C14C C15C -15(2) . . . . ? Yb1 O3C C14C C13C 168.3(17) . . . . ? F3C C13C C14C O3C 76(3) . . . . ? F1C C13C C14C O3C -48(4) . . . . ? F2C C13C C14C O3C -168(3) . . . . ? F3C C13C C14C C15C -101(3) . . . . ? F1C C13C C14C C15C 135(3) . . . . ? F2C C13C C14C C15C 15(4) . . . . ? O3C C14C C15C C16C 1(3) . . . . ? C13C C14C C15C C16C 177(2) . . . . ? Yb1 O4C C16C C15C 4(3) . . . . ? Yb1 O4C C16C C17C -176.5(10) . . . . ? C14C C15C C16C O4C 5(3) . . . . ? C14C C15C C16C C17C -174.5(16) . . . . ? O4C C16C C17C C19C 20(3) . . . . ? C15C C16C C17C C19C -160(2) . . . . ? O4C C16C C17C C18C 145.5(18) . . . . ? C15C C16C C17C C18C -35(3) . . . . ? O4C C16C C17C C20C -93(2) . . . . ? C15C C16C C17C C20C 86.3(19) . . . . ? O4E C14E C13E F2E 50(2) . . . . ? C15E C14E C13E F2E -124.5(17) . . . . ? O4E C14E C13E F1E -71.4(18) . . . . ? C15E C14E C13E F1E 114.3(16) . . . . ? O4E C14E C13E F3E 174.8(15) . . . . ? C15E C14E C13E F3E 1(3) . . . . ? O4E Yb2 N1A C1A -31(2) . . . . ? O4F Yb2 N1A C1A -141.7(19) . . . . ? O3E Yb2 N1A C1A -109(2) . . . . ? O3F Yb2 N1A C1A 6(3) . . . . ? O5D Yb2 N1A C1A 57(2) . . . . ? O4D Yb2 N1A C1A 116(2) . . . . ? N1B Yb2 N1A C1A 168(6) . . . . ? N2B Yb2 N1A C1A 172(2) . . . . ? N2A Yb2 N1A C1A 175(2) . . . . ? C11B Yb2 N1A C1A 177(2) . . . . ? C1B Yb2 N1A C1A 11(8) . . . . ? O4E Yb2 N1A C12A 142.3(17) . . . . ? O4F Yb2 N1A C12A 32(2) . . . . ? O3E Yb2 N1A C12A 64.5(16) . . . . ? O3F Yb2 N1A C12A 178.8(13) . . . . ? O5D Yb2 N1A C12A -129.5(17) . . . . ? O4D Yb2 N1A C12A -70.7(17) . . . . ? N1B Yb2 N1A C12A -18(4) . . . . ? N2B Yb2 N1A C12A -14.3(18) . . . . ? N2A Yb2 N1A C12A -11.8(16) . . . . ? C11B Yb2 N1A C12A -9.4(15) . . . . ? C1B Yb2 N1A C12A -176(8) . . . . ? O4E Yb2 N2A C10A 142(2) . . . . ? O4F Yb2 N2A C10A 23(2) . . . . ? O3E Yb2 N2A C10A 96(2) . . . . ? O3F Yb2 N2A C10A -17(3) . . . . ? O5D Yb2 N2A C10A -124(2) . . . . ? O4D Yb2 N2A C10A -54(2) . . . . ? N1B Yb2 N2A C10A 178(3) . . . . ? N2B Yb2 N2A C10A -14(4) . . . . ? N1A Yb2 N2A C10A 176(3) . . . . ? C11B Yb2 N2A C10A 161(9) . . . . ? C1B Yb2 N2A C10A -179(3) . . . . ? O4E Yb2 N2A C11A -21(2) . . . . ? O4F Yb2 N2A C11A -139.6(16) . . . . ? O3E Yb2 N2A C11A -67.0(15) . . . . ? O3F Yb2 N2A C11A -179.8(10) . . . . ? O5D Yb2 N2A C11A 73.2(16) . . . . ? O4D Yb2 N2A C11A 142.8(16) . . . . ? N1B Yb2 N2A C11A 14.6(14) . . . . ? N2B Yb2 N2A C11A -177(7) . . . . ? N1A Yb2 N2A C11A 13.4(14) . . . . ? C11B Yb2 N2A C11A -2(6) . . . . ? C1B Yb2 N2A C11A 18(2) . . . . ? C12A N1A C1A C2A -4(4) . . . . ? Yb2 N1A C1A C2A 168.1(19) . . . . ? N1A C1A C2A C3A -2(4) . . . . ? C1A C2A C3A C4A 8(4) . . . . ? C2A C3A C4A C5A 175(3) . . . . ? C2A C3A C4A C12A -7(3) . . . . ? C3A C4A C5A C6A -180(2) . . . . ? C12A C4A C5A C6A 3(3) . . . . ? O1A N3A C6A C7A -134(3) . . . . ? O2A N3A C6A C7A 46(4) . . . . ? O1A N3A C6A C5A 42(3) . . . . ? O2A N3A C6A C5A -138(2) . . . . ? C4A C5A C6A C7A -4(3) . . . . ? C4A C5A C6A N3A 179(2) . . . . ? N3A C6A C7A C11A 177(3) . . . . ? C5A C6A C7A C11A 1(4) . . . . ? N3A C6A C7A C8A -2(4) . . . . ? C5A C6A C7A C8A -178.1(18) . . . . ? C6A C7A C8A C9A 179(3) . . . . ? C11A C7A C8A C9A 0(3) . . . . ? C7A C8A C9A C10A 2(5) . . . . ? C11A N2A C10A C9A -1(5) . . . . ? Yb2 N2A C10A C9A -165(4) . . . . ? C8A C9A C10A N2A -2(6) . . . . ? C6A C7A C11A N2A 178(3) . . . . ? C8A C7A C11A N2A -2(3) . . . . ? C6A C7A C11A C12A 2(3) . . . . ? C8A C7A C11A C12A -178.6(14) . . . . ? C10A N2A C11A C7A 3(3) . . . . ? Yb2 N2A C11A C7A 169.3(18) . . . . ? C10A N2A C11A C12A 179.4(18) . . . . ? Yb2 N2A C11A C12A -14(2) . . . . ? C1A N1A C12A C4A 4(4) . . . . ? Yb2 N1A C12A C4A -168.7(13) . . . . ? C1A N1A C12A C11A -178(2) . . . . ? Yb2 N1A C12A C11A 10(3) . . . . ? C5A C4A C12A N1A 179(2) . . . . ? C3A C4A C12A N1A 1(2) . . . . ? C5A C4A C12A C11A 1(3) . . . . ? C3A C4A C12A C11A -177.3(15) . . . . ? C7A C11A C12A N1A 179(2) . . . . ? N2A C11A C12A N1A 2(3) . . . . ? C7A C11A C12A C4A -3(2) . . . . ? N2A C11A C12A C4A -179.9(17) . . . . ? O4E Yb2 N1B C1B -33(4) . . . . ? O4F Yb2 N1B C1B -151(4) . . . . ? O3E Yb2 N1B C1B -109(4) . . . . ? O3F Yb2 N1B C1B 7(4) . . . . ? O5D Yb2 N1B C1B 52(4) . . . . ? O4D Yb2 N1B C1B 117(4) . . . . ? N2B Yb2 N1B C1B 170(4) . . . . ? N2A Yb2 N1B C1B 173(4) . . . . ? N1A Yb2 N1B C1B -15(7) . . . . ? C11B Yb2 N1B C1B 175(4) . . . . ? O4E Yb2 N1B C12B 145.4(16) . . . . ? O4F Yb2 N1B C12B 27.3(18) . . . . ? O3E Yb2 N1B C12B 69.6(15) . . . . ? O3F Yb2 N1B C12B -174.2(12) . . . . ? O5D Yb2 N1B C12B -129.8(16) . . . . ? O4D Yb2 N1B C12B -64.9(16) . . . . ? N2B Yb2 N1B C12B -11.6(17) . . . . ? N2A Yb2 N1B C12B -8.8(15) . . . . ? N1A Yb2 N1B C12B 164(6) . . . . ? C11B Yb2 N1B C12B -5.9(14) . . . . ? C1B Yb2 N1B C12B 179(5) . . . . ? O4E Yb2 N2B C11B -28(3) . . . . ? O4F Yb2 N2B C11B -139(3) . . . . ? O3E Yb2 N2B C11B -64(2) . . . . ? O3F Yb2 N2B C11B -180.0(16) . . . . ? O5D Yb2 N2B C11B 76(2) . . . . ? O4D Yb2 N2B C11B 139(3) . . . . ? N1B Yb2 N2B C11B 12(2) . . . . ? N2A Yb2 N2B C11B 2(4) . . . . ? N1A Yb2 N2B C11B 12(2) . . . . ? C1B Yb2 N2B C11B 17(3) . . . . ? O4E Yb2 N2B C10B 146(3) . . . . ? O4F Yb2 N2B C10B 36(3) . . . . ? O3E Yb2 N2B C10B 110(3) . . . . ? O3F Yb2 N2B C10B -6(4) . . . . ? O5D Yb2 N2B C10B -110(3) . . . . ? O4D Yb2 N2B C10B -47(3) . . . . ? N1B Yb2 N2B C10B -173(3) . . . . ? N2A Yb2 N2B C10B 176(8) . . . . ? N1A Yb2 N2B C10B -174(3) . . . . ? C11B Yb2 N2B C10B 174(5) . . . . ? C1B Yb2 N2B C10B -169(4) . . . . ? O2B O1B N3B C5B -87(5) . . . . ? O1B O2B N3B C5B 109(5) . . . . ? C12B N1B C1B C2B -14(9) . . . . ? Yb2 N1B C1B C2B 164(5) . . . . ? C12B N1B C1B Yb2 -178(5) . . . . ? O4E Yb2 C1B C2B 117(11) . . . . ? O4F Yb2 C1B C2B 24(13) . . . . ? O3E Yb2 C1B C2B 41(10) . . . . ? O3F Yb2 C1B C2B 159(9) . . . . ? O5D Yb2 C1B C2B -145(11) . . . . ? O4D Yb2 C1B C2B -100(10) . . . . ? N1B Yb2 C1B C2B -25(8) . . . . ? N2B Yb2 C1B C2B -35(10) . . . . ? N2A Yb2 C1B C2B -31(10) . . . . ? N1A Yb2 C1B C2B -17(6) . . . . ? C11B Yb2 C1B C2B -29(10) . . . . ? O4E Yb2 C1B N1B 142(5) . . . . ? O4F Yb2 C1B N1B 49(7) . . . . ? O3E Yb2 C1B N1B 66(4) . . . . ? O3F Yb2 C1B N1B -176(3) . . . . ? O5D Yb2 C1B N1B -120(4) . . . . ? O4D Yb2 C1B N1B -75(4) . . . . ? N2B Yb2 C1B N1B -10(4) . . . . ? N2A Yb2 C1B N1B -6(4) . . . . ? N1A Yb2 C1B N1B 8(4) . . . . ? C11B Yb2 C1B N1B -4(3) . . . . ? N1B C1B C2B C3B 13(14) . . . . ? Yb2 C1B C2B C3B 30(18) . . . . ? C1B C2B C3B C4B -8(13) . . . . ? C2B C3B C4B C12B 2(7) . . . . ? C2B C3B C4B C5B 179(4) . . . . ? C12B C4B C5B C6B -3(4) . . . . ? C3B C4B C5B C6B 179(3) . . . . ? C12B C4B C5B N3B -168(4) . . . . ? C3B C4B C5B N3B 13(6) . . . . ? O1B N3B C5B C4B -77(7) . . . . ? O2B N3B C5B C4B -161(5) . . . . ? O1B N3B C5B C6B 118(7) . . . . ? O2B N3B C5B C6B 34(6) . . . . ? C4B C5B C6B C7B 1(5) . . . . ? N3B C5B C6B C7B 167(4) . . . . ? C5B C6B C7B C8B 178(3) . . . . ? C5B C6B C7B C11B 0(6) . . . . ? C6B C7B C8B C9B -171(3) . . . . ? C11B C7B C8B C9B 7(5) . . . . ? C7B C8B C9B C10B -10(5) . . . . ? C11B N2B C10B C9B 3(6) . . . . ? Yb2 N2B C10B C9B -170(3) . . . . ? C8B C9B C10B N2B 5(5) . . . . ? C10B N2B C11B C7B -7(5) . . . . ? Yb2 N2B C11B C7B 167(3) . . . . ? C10B N2B C11B C12B 172(3) . . . . ? Yb2 N2B C11B C12B -14(4) . . . . ? C10B N2B C11B Yb2 -174(5) . . . . ? C8B C7B C11B N2B 2(5) . . . . ? C6B C7B C11B N2B 180(4) . . . . ? C8B C7B C11B C12B -177(3) . . . . ? C6B C7B C11B C12B 1(5) . . . . ? C8B C7B C11B Yb2 48(11) . . . . ? C6B C7B C11B Yb2 -135(8) . . . . ? O4E Yb2 C11B N2B 160(2) . . . . ? O4F Yb2 C11B N2B 39(2) . . . . ? O3E Yb2 C11B N2B 109(2) . . . . ? O3F Yb2 C11B N2B 0(3) . . . . ? O5D Yb2 C11B N2B -110(2) . . . . ? O4D Yb2 C11B N2B -37(2) . . . . ? N1B Yb2 C11B N2B -165(3) . . . . ? N2A Yb2 C11B N2B -3(8) . . . . ? N1A Yb2 C11B N2B -167(3) . . . . ? C1B Yb2 C11B N2B -163(3) . . . . ? O4E Yb2 C11B C7B 106(9) . . . . ? O4F Yb2 C11B C7B -15(10) . . . . ? O3E Yb2 C11B C7B 56(9) . . . . ? O3F Yb2 C11B C7B -54(10) . . . . ? O5D Yb2 C11B C7B -163(9) . . . . ? O4D Yb2 C11B C7B -91(10) . . . . ? N1B Yb2 C11B C7B 142(10) . . . . ? N2B Yb2 C11B C7B -54(10) . . . . ? N2A Yb2 C11B C7B -57(10) . . . . ? N1A Yb2 C11B C7B 140(10) . . . . ? C1B Yb2 C11B C7B 144(10) . . . . ? O4E Yb2 C11B C12B -29.8(15) . . . . ? O4F Yb2 C11B C12B -150.9(14) . . . . ? O3E Yb2 C11B C12B -80.4(14) . . . . ? O3F Yb2 C11B C12B 170.2(12) . . . . ? O5D Yb2 C11B C12B 60.5(14) . . . . ? O4D Yb2 C11B C12B 132.7(14) . . . . ? N1B Yb2 C11B C12B 5.4(13) . . . . ? N2B Yb2 C11B C12B 170(3) . . . . ? N2A Yb2 C11B C12B 167(8) . . . . ? N1A Yb2 C11B C12B 3.6(13) . . . . ? C1B Yb2 C11B C12B 7(2) . . . . ? C3B C4B C12B C11B -175(5) . . . . ? C5B C4B C12B C11B 7(7) . . . . ? C3B C4B C12B N1B -4(5) . . . . ? C5B C4B C12B N1B 178(2) . . . . ? N2B C11B C12B C4B 175(5) . . . . ? C7B C11B C12B C4B -6(6) . . . . ? Yb2 C11B C12B C4B 165(5) . . . . ? N2B C11B C12B N1B 4(4) . . . . ? C7B C11B C12B N1B -177(2) . . . . ? Yb2 C11B C12B N1B -6.6(15) . . . . ? C1B N1B C12B C4B 12(6) . . . . ? Yb2 N1B C12B C4B -166.1(19) . . . . ? C1B N1B C12B C11B -172(5) . . . . ? Yb2 N1B C12B C11B 9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.655 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.121 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 1 -0.046 0.500 0.000 331.9 105.7 2 -0.049 0.000 0.500 331.9 105.9 3 0.207 0.365 0.344 25.1 12.9 4 0.207 0.135 0.844 25.1 13.1 5 0.266 0.851 0.229 20.3 5.3 6 0.266 0.649 0.729 20.3 5.8 7 0.292 0.263 0.444 7.5 1.6 8 0.292 0.237 0.944 6.7 1.7 9 0.733 0.351 0.271 20.3 6.2 10 0.733 0.149 0.771 20.3 6.9 11 0.707 0.763 0.055 8.1 1.7 12 0.707 0.737 0.555 7.4 1.8 13 0.792 0.865 0.156 25.0 10.5 14 0.792 0.635 0.656 25.0 10.9 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 933189'