# 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_c100427h _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 Dy3 O25' _chemical_formula_weight 1270.98 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' Dy Dy -0.1892 4.4098 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1443(13) _cell_length_b 12.1037(16) _cell_length_c 14.857(2) _cell_angle_alpha 68.192(2) _cell_angle_beta 83.565(2) _cell_angle_gamma 74.557(2) _cell_volume 1632.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1085 _cell_measurement_theta_min 2.5105 _cell_measurement_theta_max 28.7933 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1202 _exptl_absorpt_coefficient_mu 6.907 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4912 _exptl_absorpt_correction_T_max 0.7239 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number 3908 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9324 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_unetI/netI 0.0980 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5685 _reflns_number_gt 4472 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR: the parameter to go anisotropic restraint to appointed atoms. SIMU: the parameter to set some atoms in limited range having the save shift parameters, and this parameter always is used with ISOR. SIMU 0.001 $o $c SIMU 0.005 0.005 C7 C2 C12 C5 C17 C19 O11 C22 o22 ISOR 0.005 0.005 C7 C2 C12 C5 C17 C19 O11 C22 o22 ; _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^)+(0.0335P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5685 _refine_ls_number_parameters 514 _refine_ls_number_restraints 360 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.052 _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 Dy1 Dy 1.24431(5) -0.52034(5) 0.89951(4) 0.01387(15) Uani 1 1 d . . . Dy2 Dy 0.35744(5) -0.02265(5) 0.78439(4) 0.01277(14) Uani 1 1 d . . . Dy3 Dy 0.48973(5) 0.28745(5) 0.54111(4) 0.01136(14) Uani 1 1 d . . . C1 C 1.0217(11) -0.2448(10) 0.7342(8) 0.0181(8) Uani 1 1 d U . . C2 C 0.9156(11) -0.2693(10) 0.8006(8) 0.0176(8) Uani 1 1 d U . . C3 C 0.8003(11) -0.1783(10) 0.7962(8) 0.0178(8) Uani 1 1 d U . . H3 H 0.7307 -0.1942 0.8420 0.021 Uiso 1 1 calc R . . C4 C 0.7848(12) -0.0625(10) 0.7249(8) 0.0184(8) Uani 1 1 d U . . C5 C 0.8924(11) -0.0411(10) 0.6598(8) 0.0188(9) Uani 1 1 d U . . H5 H 0.8839 0.0362 0.6119 0.023 Uiso 1 1 calc R . . C6 C 1.0105(12) -0.1292(10) 0.6634(8) 0.0186(9) Uani 1 1 d U . . H6 H 1.0817 -0.1121 0.6194 0.022 Uiso 1 1 calc R . . C7 C 1.2446(11) -0.2965(10) 0.6675(8) 0.0186(9) Uani 1 1 d U . . H7A H 1.2759 -0.2326 0.6770 0.022 Uiso 1 1 calc R . . H7B H 1.2078 -0.2650 0.6028 0.022 Uiso 1 1 calc R . . C8 C 1.3627(11) -0.4095(10) 0.6799(8) 0.0191(9) Uani 1 1 d U . . C9 C 0.9188(12) -0.3910(10) 0.8801(8) 0.0176(8) Uani 1 1 d U . . C10 C 0.6547(12) 0.0300(10) 0.7132(8) 0.0189(9) Uani 1 1 d U . . C11 C 0.1997(12) 0.0168(10) 1.0061(8) 0.0221(8) Uani 1 1 d U . . C12 C 0.1577(12) 0.1416(10) 0.9590(8) 0.0209(8) Uani 1 1 d U . . C13 C 0.0394(12) 0.2096(10) 0.9891(8) 0.0204(9) Uani 1 1 d U . . H13 H 0.0082 0.2934 0.9555 0.024 Uiso 1 1 calc R . . C14 C -0.0306(12) 0.1496(10) 1.0701(8) 0.0204(8) Uani 1 1 d U . . C15 C 0.0159(12) 0.0260(10) 1.1192(8) 0.0211(9) Uani 1 1 d U . . H15 H -0.0325 -0.0125 1.1736 0.025 Uiso 1 1 calc R . . C16 C 0.1315(12) -0.0423(11) 1.0902(8) 0.0217(9) Uani 1 1 d U . . H16 H 0.1636 -0.1255 1.1254 0.026 Uiso 1 1 calc R . . C17 C 0.3894(12) -0.1562(11) 1.0374(9) 0.0266(9) Uani 1 1 d U . . H17A H 0.3303 -0.2067 1.0782 0.032 Uiso 1 1 calc R . . H17B H 0.4357 -0.1325 1.0785 0.032 Uiso 1 1 calc R . . C18 C 0.4925(13) -0.2278(11) 0.9872(9) 0.0278(10) Uani 1 1 d U . . C19 C 0.2290(12) 0.2114(10) 0.8693(8) 0.0211(9) Uani 1 1 d U . . C20 C -0.1544(12) 0.2243(10) 1.1032(8) 0.0203(9) Uani 1 1 d U . . C21 C 0.1709(11) 0.3293(10) 0.4507(8) 0.0180(8) Uani 1 1 d U . . C22 C 0.1180(11) 0.2644(10) 0.5403(8) 0.0176(8) Uani 1 1 d U . . C23 C -0.0214(11) 0.2996(10) 0.5543(8) 0.0176(8) Uani 1 1 d U . . H23 H -0.0603 0.2559 0.6119 0.021 Uiso 1 1 calc R . . C24 C -0.1057(11) 0.3969(10) 0.4865(8) 0.0181(8) Uani 1 1 d U . . C25 C -0.0480(11) 0.4589(10) 0.3991(8) 0.0181(9) Uani 1 1 d U . . H25 H -0.1030 0.5251 0.3528 0.022 Uiso 1 1 calc R . . C26 C 0.0881(11) 0.4237(10) 0.3805(8) 0.0181(9) Uani 1 1 d U . . H26 H 0.1251 0.4632 0.3207 0.022 Uiso 1 1 calc R . . C27 C 0.3505(11) 0.2317(10) 0.3663(8) 0.0199(9) Uani 1 1 d U . . H27A H 0.3433 0.2893 0.3000 0.024 Uiso 1 1 calc R . . H27B H 0.2893 0.1790 0.3749 0.024 Uiso 1 1 calc R . . C28 C 0.4955(12) 0.1555(10) 0.3857(8) 0.0200(9) Uani 1 1 d U . . C29 C 0.2085(11) 0.1679(10) 0.6191(8) 0.0181(8) Uani 1 1 d U . . C30 C -0.2566(12) 0.4348(10) 0.5038(8) 0.0190(9) Uani 1 1 d U . . O1 O 1.1420(8) -0.3335(7) 0.7386(5) 0.0183(8) Uani 1 1 d U . . O2 O 1.4551(8) -0.4018(6) 0.6178(5) 0.0191(10) Uani 1 1 d U . . O3 O 1.3618(8) -0.5037(7) 0.7510(5) 0.0202(10) Uani 1 1 d U . . O4 O 1.0152(8) -0.4825(6) 0.8834(5) 0.0173(10) Uani 1 1 d U . . O5 O 0.8202(8) -0.3965(7) 0.9394(5) 0.0185(10) Uani 1 1 d U . . O6 O 0.5643(8) 0.0172(6) 0.7777(5) 0.0190(10) Uani 1 1 d U . . O7 O 0.6383(8) 0.1201(7) 0.6335(5) 0.0198(10) Uani 1 1 d U . . O8 O 0.3104(8) -0.0506(7) 0.9691(6) 0.0243(9) Uani 1 1 d U . . O9 O 0.5686(8) -0.3223(7) 1.0432(6) 0.0298(11) Uani 1 1 d U . . O10 O 0.4852(8) -0.1987(7) 0.8998(6) 0.0278(11) Uani 1 1 d U . . O11 O 0.2963(8) 0.1558(7) 0.8169(5) 0.0211(10) Uani 1 1 d U . . O12 O 0.2150(8) 0.3219(7) 0.8536(5) 0.0219(10) Uani 1 1 d U . . O13 O -0.1728(8) 0.3371(7) 1.0693(5) 0.0206(10) Uani 1 1 d U . . O14 O -0.2316(8) 0.1668(7) 1.1669(5) 0.0206(10) Uani 1 1 d U . . O15 O 0.3127(7) 0.2966(7) 0.4317(5) 0.0189(8) Uani 1 1 d U . . O16 O 0.5477(8) 0.1094(7) 0.3236(5) 0.0200(10) Uani 1 1 d U . . O17 O 0.5544(8) 0.1484(7) 0.4574(5) 0.0202(10) Uani 1 1 d U . . O18 O 0.3359(7) 0.1650(7) 0.6226(5) 0.0177(10) Uani 1 1 d U . . O19 O 0.1595(7) 0.0878(7) 0.6840(5) 0.0190(10) Uani 1 1 d U . . O20 O -0.3153(8) 0.3512(7) 0.5521(5) 0.0199(10) Uani 1 1 d U . . O21 O -0.3161(4) 0.5464(4) 0.4676(3) 0.0193(10) Uani 1 1 d U . . O22 O 1.4336(4) -0.4310(4) 0.8901(3) 0.054(3) Uani 1 1 d RU . . H22A H 1.3972 -0.3587 0.8891 0.065 Uiso 1 1 d R . . H22B H 1.5174 -0.4392 0.8733 0.065 Uiso 1 1 d R . . O23 O 0.4677(4) 0.2969(4) 0.7006(3) 0.0201(19) Uani 1 1 d R . . H23A H 0.4592 0.2325 0.7476 0.024 Uiso 1 1 d R . . H23B H 0.4183 0.3607 0.7099 0.024 Uiso 1 1 d R . . O24 O 0.6958(4) 0.4706(4) 0.8485(3) 0.137(7) Uani 1 1 d R . . H24A H 0.7500 0.4942 0.8730 0.205 Uiso 1 1 d R . . H24B H 0.7116 0.3928 0.8720 0.205 Uiso 1 1 d R . . O25 O 0.7176(15) 0.3336(15) 0.7478(10) 0.133(6) Uani 1 1 d . . . H25A H 0.6628 0.2899 0.7507 0.199 Uiso 1 1 d R . . H25B H 0.7238 0.3816 0.6895 0.199 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0140(3) 0.0113(3) 0.0120(3) -0.0026(2) 0.0045(2) -0.0005(2) Dy2 0.0125(3) 0.0117(3) 0.0120(3) -0.0035(2) 0.0043(2) -0.0024(2) Dy3 0.0090(3) 0.0123(3) 0.0096(3) -0.0018(2) 0.0032(2) -0.0020(2) C1 0.0174(14) 0.0166(15) 0.0156(14) -0.0022(12) 0.0030(12) -0.0029(12) C2 0.0174(14) 0.0163(15) 0.0152(14) -0.0027(12) 0.0021(12) -0.0029(12) C3 0.0173(15) 0.0164(16) 0.0155(15) -0.0027(13) 0.0020(13) -0.0027(13) C4 0.0173(15) 0.0169(15) 0.0160(14) -0.0022(13) 0.0021(13) -0.0024(13) C5 0.0175(15) 0.0170(16) 0.0163(15) -0.0017(13) 0.0025(14) -0.0025(13) C6 0.0175(15) 0.0169(16) 0.0161(15) -0.0018(13) 0.0029(14) -0.0026(13) C7 0.0177(16) 0.0169(16) 0.0158(15) -0.0017(14) 0.0051(14) -0.0037(14) C8 0.0181(17) 0.0171(17) 0.0162(17) -0.0014(15) 0.0059(15) -0.0038(15) C9 0.0177(16) 0.0164(16) 0.0150(15) -0.0029(14) 0.0020(14) -0.0027(13) C10 0.0173(16) 0.0173(17) 0.0165(16) -0.0020(14) 0.0017(14) -0.0017(14) C11 0.0235(15) 0.0197(14) 0.0196(14) -0.0060(13) 0.0041(13) -0.0029(12) C12 0.0229(14) 0.0187(14) 0.0194(14) -0.0068(12) 0.0048(12) -0.0041(12) C13 0.0225(15) 0.0183(15) 0.0192(15) -0.0068(13) 0.0044(14) -0.0048(13) C14 0.0223(15) 0.0183(15) 0.0194(15) -0.0065(13) 0.0044(13) -0.0051(13) C15 0.0227(16) 0.0188(16) 0.0196(16) -0.0060(14) 0.0043(14) -0.0045(14) C16 0.0231(16) 0.0193(15) 0.0197(16) -0.0058(14) 0.0040(14) -0.0037(14) C17 0.0258(17) 0.0235(17) 0.0208(16) -0.0031(14) 0.0036(15) 0.0014(14) C18 0.0262(18) 0.0247(18) 0.0207(17) -0.0019(16) 0.0036(16) 0.0026(15) C19 0.0231(15) 0.0184(15) 0.0199(15) -0.0071(13) 0.0058(13) -0.0041(13) C20 0.0222(17) 0.0182(16) 0.0196(17) -0.0064(14) 0.0046(14) -0.0057(14) C21 0.0157(14) 0.0195(16) 0.0187(15) -0.0067(13) 0.0015(13) -0.0052(12) C22 0.0153(14) 0.0189(15) 0.0184(14) -0.0059(13) 0.0016(13) -0.0057(12) C23 0.0152(15) 0.0188(16) 0.0183(15) -0.0057(14) 0.0012(14) -0.0057(13) C24 0.0155(15) 0.0193(16) 0.0186(15) -0.0052(14) 0.0008(14) -0.0054(13) C25 0.0155(16) 0.0194(17) 0.0186(16) -0.0056(14) 0.0010(14) -0.0052(14) C26 0.0157(16) 0.0195(17) 0.0187(16) -0.0061(14) 0.0013(14) -0.0052(14) C27 0.0178(17) 0.0212(17) 0.0200(17) -0.0080(15) 0.0018(15) -0.0033(14) C28 0.0184(18) 0.0210(18) 0.0202(18) -0.0089(15) 0.0017(16) -0.0030(15) C29 0.0153(16) 0.0194(17) 0.0184(16) -0.0048(14) 0.0021(14) -0.0060(14) C30 0.0161(16) 0.0198(17) 0.0191(17) -0.0043(15) 0.0002(15) -0.0053(14) O1 0.0175(15) 0.0167(15) 0.0157(15) -0.0018(13) 0.0042(13) -0.0033(13) O2 0.0180(19) 0.0172(19) 0.0161(18) -0.0011(16) 0.0059(17) -0.0042(17) O3 0.0188(19) 0.0178(19) 0.0168(18) -0.0010(16) 0.0066(17) -0.0031(17) O4 0.0178(18) 0.0161(18) 0.0151(17) -0.0034(16) 0.0014(16) -0.0031(15) O5 0.0182(18) 0.0169(18) 0.0152(17) -0.0024(16) 0.0027(16) -0.0019(16) O6 0.0171(18) 0.0175(18) 0.0169(18) -0.0019(16) 0.0015(16) -0.0019(16) O7 0.0177(18) 0.0181(19) 0.0167(18) -0.0015(16) 0.0018(16) -0.0004(16) O8 0.0249(16) 0.0213(16) 0.0202(15) -0.0048(14) 0.0038(14) -0.0006(13) O9 0.027(2) 0.026(2) 0.0215(19) -0.0004(18) 0.0040(18) 0.0042(17) O10 0.026(2) 0.025(2) 0.0202(19) -0.0016(18) 0.0034(18) 0.0027(17) O11 0.0235(17) 0.0185(17) 0.0197(17) -0.0075(15) 0.0063(15) -0.0040(15) O12 0.0237(18) 0.0184(17) 0.0209(17) -0.0066(15) 0.0067(16) -0.0039(15) O13 0.0226(19) 0.0181(18) 0.0199(19) -0.0064(16) 0.0049(17) -0.0055(16) O14 0.0220(19) 0.0185(18) 0.0200(18) -0.0061(16) 0.0048(17) -0.0061(16) O15 0.0166(15) 0.0203(16) 0.0193(16) -0.0074(14) 0.0020(14) -0.0043(13) O16 0.019(2) 0.021(2) 0.0203(19) -0.0097(17) 0.0019(18) -0.0030(17) O17 0.018(2) 0.021(2) 0.0203(19) -0.0086(17) 0.0014(17) -0.0027(17) O18 0.0150(18) 0.0193(19) 0.0180(18) -0.0048(16) 0.0021(16) -0.0065(16) O19 0.0154(18) 0.0200(19) 0.0190(18) -0.0036(16) 0.0024(16) -0.0061(16) O20 0.0163(18) 0.0205(19) 0.0196(19) -0.0027(17) 0.0000(17) -0.0055(16) O21 0.0166(18) 0.0197(19) 0.0196(19) -0.0045(17) 0.0001(17) -0.0051(16) O22 0.045(5) 0.051(4) 0.074(5) -0.029(4) 0.005(4) -0.016(4) O23 0.035(5) 0.007(4) 0.015(4) -0.002(4) -0.002(4) -0.002(4) O24 0.058(10) 0.170(16) 0.23(2) -0.136(15) -0.011(11) -0.011(10) O25 0.128(14) 0.231(19) 0.063(10) -0.063(12) 0.005(9) -0.069(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O4 2.268(7) . ? Dy1 O9 2.277(8) 2_747 ? Dy1 O5 2.319(7) 2_747 ? Dy1 O13 2.343(7) 2_657 ? Dy1 O12 2.349(7) 1_645 ? Dy1 O3 2.353(7) . ? Dy1 O22 2.410(4) . ? Dy1 O1 2.683(7) . ? Dy2 O16 2.230(7) 2_656 ? Dy2 O6 2.259(7) . ? Dy2 O14 2.288(7) 2_557 ? Dy2 O11 2.298(7) . ? Dy2 O10 2.340(8) . ? Dy2 O19 2.409(8) . ? Dy2 O18 2.604(7) . ? Dy2 O8 2.641(8) . ? Dy2 C29 2.898(12) . ? Dy3 O7 2.243(7) . ? Dy3 O21 2.266(4) 2_566 ? Dy3 O2 2.343(7) 2_756 ? Dy3 O20 2.347(7) 1_655 ? Dy3 O18 2.360(7) . ? Dy3 O17 2.365(7) . ? Dy3 O23 2.397(4) . ? Dy3 O15 2.508(7) . ? C1 O1 1.383(13) . ? C1 C6 1.388(15) . ? C1 C2 1.391(15) . ? C2 C3 1.365(15) . ? C2 C9 1.501(15) . ? C3 C4 1.388(14) . ? C3 H3 0.9300 . ? C4 C5 1.386(15) . ? C4 C10 1.465(15) . ? C5 C6 1.366(15) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.431(12) . ? C7 C8 1.526(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O3 1.235(12) . ? C8 O2 1.237(12) . ? C9 O5 1.255(12) . ? C9 O4 1.256(12) . ? C10 O6 1.245(12) . ? C10 O7 1.268(13) . ? C11 C12 1.375(15) . ? C11 O8 1.391(13) . ? C11 C16 1.400(15) . ? C12 C13 1.395(15) . ? C12 C19 1.512(15) . ? C13 C14 1.383(15) . ? C13 H13 0.9300 . ? C14 C15 1.372(14) . ? C14 C20 1.491(15) . ? C15 C16 1.371(15) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O8 1.407(13) . ? C17 C18 1.492(16) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O10 1.218(14) . ? C18 O9 1.250(13) . ? C19 O12 1.240(12) . ? C19 O11 1.244(12) . ? C20 O13 1.236(12) . ? C20 O14 1.277(13) . ? C21 C26 1.377(15) . ? C21 C22 1.402(15) . ? C21 O15 1.412(13) . ? C22 C23 1.380(15) . ? C22 C29 1.495(15) . ? C23 C24 1.381(15) . ? C23 H23 0.9300 . ? C24 C25 1.390(15) . ? C24 C30 1.499(15) . ? C25 C26 1.361(15) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 O15 1.426(12) . ? C27 C28 1.507(15) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O17 1.244(13) . ? C28 O16 1.248(12) . ? C29 O19 1.254(12) . ? C29 O18 1.290(12) . ? C30 O21 1.256(12) . ? C30 O20 1.256(12) . ? O2 Dy3 2.343(7) 2_756 ? O5 Dy1 2.319(7) 2_747 ? O9 Dy1 2.277(8) 2_747 ? O12 Dy1 2.349(7) 1_465 ? O13 Dy1 2.343(7) 2_657 ? O14 Dy2 2.288(7) 2_557 ? O16 Dy2 2.230(7) 2_656 ? O20 Dy3 2.347(7) 1_455 ? O21 Dy3 2.266(4) 2_566 ? O22 H22A 0.8495 . ? O22 H22B 0.8495 . ? O23 H23A 0.8483 . ? O23 H23B 0.8510 . ? O24 H24A 0.8499 . ? O24 H24B 0.8500 . ? O25 H25A 0.8516 . ? O25 H25B 0.8509 . ? 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 Dy1 O9 141.4(3) . 2_747 ? O4 Dy1 O5 79.9(3) . 2_747 ? O9 Dy1 O5 79.4(3) 2_747 2_747 ? O4 Dy1 O13 80.1(3) . 2_657 ? O9 Dy1 O13 128.4(3) 2_747 2_657 ? O5 Dy1 O13 82.3(2) 2_747 2_657 ? O4 Dy1 O12 75.2(3) . 1_645 ? O9 Dy1 O12 75.0(3) 2_747 1_645 ? O5 Dy1 O12 96.1(3) 2_747 1_645 ? O13 Dy1 O12 155.1(3) 2_657 1_645 ? O4 Dy1 O3 111.8(3) . . ? O9 Dy1 O3 81.8(3) 2_747 . ? O5 Dy1 O3 160.1(3) 2_747 . ? O13 Dy1 O3 114.9(3) 2_657 . ? O12 Dy1 O3 72.7(2) 1_645 . ? O4 Dy1 O22 145.5(2) . . ? O9 Dy1 O22 72.7(2) 2_747 . ? O5 Dy1 O22 109.3(2) 2_747 . ? O13 Dy1 O22 68.8(2) 2_657 . ? O12 Dy1 O22 133.8(2) 1_645 . ? O3 Dy1 O22 70.7(2) . . ? O4 Dy1 O1 65.4(2) . . ? O9 Dy1 O1 142.4(3) 2_747 . ? O5 Dy1 O1 138.1(2) 2_747 . ? O13 Dy1 O1 69.8(2) 2_657 . ? O12 Dy1 O1 96.8(2) 1_645 . ? O3 Dy1 O1 61.0(2) . . ? O22 Dy1 O1 89.40(19) . . ? O16 Dy2 O6 83.5(3) 2_656 . ? O16 Dy2 O14 85.3(3) 2_656 2_557 ? O6 Dy2 O14 147.3(3) . 2_557 ? O16 Dy2 O11 145.6(3) 2_656 . ? O6 Dy2 O11 79.5(3) . . ? O14 Dy2 O11 123.8(3) 2_557 . ? O16 Dy2 O10 85.9(3) 2_656 . ? O6 Dy2 O10 76.1(3) . . ? O14 Dy2 O10 72.6(3) 2_557 . ? O11 Dy2 O10 118.1(3) . . ? O16 Dy2 O19 90.6(3) 2_656 . ? O6 Dy2 O19 131.1(3) . . ? O14 Dy2 O19 79.5(3) 2_557 . ? O11 Dy2 O19 78.8(3) . . ? O10 Dy2 O19 152.0(3) . . ? O16 Dy2 O18 77.4(2) 2_656 . ? O6 Dy2 O18 79.8(2) . . ? O14 Dy2 O18 127.2(3) 2_557 . ? O11 Dy2 O18 70.3(2) . . ? O10 Dy2 O18 152.0(3) . . ? O19 Dy2 O18 51.7(2) . . ? O16 Dy2 O8 147.2(3) 2_656 . ? O6 Dy2 O8 95.1(3) . . ? O14 Dy2 O8 78.4(2) 2_557 . ? O11 Dy2 O8 64.6(2) . . ? O10 Dy2 O8 62.2(3) . . ? O19 Dy2 O8 113.8(2) . . ? O18 Dy2 O8 134.8(2) . . ? O16 Dy2 C29 84.1(3) 2_656 . ? O6 Dy2 C29 106.0(3) . . ? O14 Dy2 C29 103.2(3) 2_557 . ? O11 Dy2 C29 72.4(3) . . ? O10 Dy2 C29 169.4(3) . . ? O19 Dy2 C29 25.2(3) . . ? O18 Dy2 C29 26.4(3) . . ? O8 Dy2 C29 127.2(3) . . ? O7 Dy3 O21 148.2(2) . 2_566 ? O7 Dy3 O2 121.9(3) . 2_756 ? O21 Dy3 O2 85.9(2) 2_566 2_756 ? O7 Dy3 O20 73.6(3) . 1_655 ? O21 Dy3 O20 103.4(2) 2_566 1_655 ? O2 Dy3 O20 73.9(3) 2_756 1_655 ? O7 Dy3 O18 80.7(3) . . ? O21 Dy3 O18 87.5(2) 2_566 . ? O2 Dy3 O18 138.9(3) 2_756 . ? O20 Dy3 O18 146.8(3) 1_655 . ? O7 Dy3 O17 72.1(3) . . ? O21 Dy3 O17 135.9(2) 2_566 . ? O2 Dy3 O17 73.8(3) 2_756 . ? O20 Dy3 O17 107.6(3) 1_655 . ? O18 Dy3 O17 83.4(2) . . ? O7 Dy3 O23 73.9(2) . . ? O21 Dy3 O23 74.60(17) 2_566 . ? O2 Dy3 O23 140.0(2) 2_756 . ? O20 Dy3 O23 77.1(2) 1_655 . ? O18 Dy3 O23 75.8(2) . . ? O17 Dy3 O23 142.4(2) . . ? O7 Dy3 O15 127.5(2) . . ? O21 Dy3 O15 72.48(19) 2_566 . ? O2 Dy3 O15 72.4(2) 2_756 . ? O20 Dy3 O15 146.2(3) 1_655 . ? O18 Dy3 O15 67.0(2) . . ? O17 Dy3 O15 64.3(2) . . ? O23 Dy3 O15 130.5(2) . . ? O1 C1 C6 118.4(10) . . ? O1 C1 C2 121.1(10) . . ? C6 C1 C2 120.5(10) . . ? C3 C2 C1 119.4(11) . . ? C3 C2 C9 116.2(10) . . ? C1 C2 C9 124.3(10) . . ? C2 C3 C4 121.4(11) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 117.7(10) . . ? C5 C4 C10 121.0(10) . . ? C3 C4 C10 121.1(10) . . ? C6 C5 C4 122.5(11) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C1 118.5(11) . . ? C5 C6 H6 120.8 . . ? C1 C6 H6 120.8 . . ? O1 C7 C8 107.4(8) . . ? O1 C7 H7A 110.2 . . ? C8 C7 H7A 110.2 . . ? O1 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? O3 C8 O2 123.1(11) . . ? O3 C8 C7 118.9(10) . . ? O2 C8 C7 118.0(10) . . ? O5 C9 O4 122.8(10) . . ? O5 C9 C2 117.1(10) . . ? O4 C9 C2 120.1(10) . . ? O6 C10 O7 122.6(10) . . ? O6 C10 C4 120.9(10) . . ? O7 C10 C4 116.5(10) . . ? C12 C11 O8 119.5(10) . . ? C12 C11 C16 120.4(11) . . ? O8 C11 C16 120.1(10) . . ? C11 C12 C13 120.6(11) . . ? C11 C12 C19 123.0(11) . . ? C13 C12 C19 116.2(10) . . ? C14 C13 C12 118.4(11) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C15 C14 C13 120.5(11) . . ? C15 C14 C20 121.8(10) . . ? C13 C14 C20 117.7(10) . . ? C16 C15 C14 121.9(11) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C11 118.0(11) . . ? C15 C16 H16 121.0 . . ? C11 C16 H16 121.0 . . ? O8 C17 C18 110.3(10) . . ? O8 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? O8 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? O10 C18 O9 126.4(12) . . ? O10 C18 C17 118.8(11) . . ? O9 C18 C17 114.2(11) . . ? O12 C19 O11 124.8(11) . . ? O12 C19 C12 116.3(10) . . ? O11 C19 C12 119.0(10) . . ? O13 C20 O14 124.6(11) . . ? O13 C20 C14 117.9(10) . . ? O14 C20 C14 117.5(10) . . ? C26 C21 C22 121.7(11) . . ? C26 C21 O15 119.2(10) . . ? C22 C21 O15 119.1(10) . . ? C23 C22 C21 116.5(11) . . ? C23 C22 C29 121.5(10) . . ? C21 C22 C29 121.9(10) . . ? C22 C23 C24 122.8(11) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C23 C24 C25 118.4(11) . . ? C23 C24 C30 121.9(10) . . ? C25 C24 C30 119.6(11) . . ? C26 C25 C24 120.7(11) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C21 119.8(11) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? O15 C27 C28 109.2(9) . . ? O15 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? O15 C27 H27B 109.8 . . ? C28 C27 H27B 109.8 . . ? H27A C27 H27B 108.3 . . ? O17 C28 O16 125.8(11) . . ? O17 C28 C27 118.9(10) . . ? O16 C28 C27 115.2(10) . . ? O19 C29 O18 118.9(11) . . ? O19 C29 C22 119.3(10) . . ? O18 C29 C22 121.8(10) . . ? O19 C29 Dy2 55.0(6) . . ? O18 C29 Dy2 64.0(6) . . ? C22 C29 Dy2 173.8(8) . . ? O21 C30 O20 124.6(10) . . ? O21 C30 C24 118.3(9) . . ? O20 C30 C24 117.1(10) . . ? C1 O1 C7 115.9(8) . . ? C1 O1 Dy1 125.3(6) . . ? C7 O1 Dy1 113.3(6) . . ? C8 O2 Dy3 143.5(8) . 2_756 ? C8 O3 Dy1 127.7(7) . . ? C9 O4 Dy1 132.3(7) . . ? C9 O5 Dy1 145.1(7) . 2_747 ? C10 O6 Dy2 132.1(7) . . ? C10 O7 Dy3 145.2(7) . . ? C11 O8 C17 116.1(9) . . ? C11 O8 Dy2 125.9(7) . . ? C17 O8 Dy2 117.0(6) . . ? C18 O9 Dy1 160.4(8) . 2_747 ? C18 O10 Dy2 130.8(8) . . ? C19 O11 Dy2 147.2(7) . . ? C19 O12 Dy1 150.7(8) . 1_465 ? C20 O13 Dy1 146.2(7) . 2_657 ? C20 O14 Dy2 148.9(7) . 2_557 ? C21 O15 C27 115.0(8) . . ? C21 O15 Dy3 122.8(6) . . ? C27 O15 Dy3 119.3(6) . . ? C28 O16 Dy2 178.6(8) . 2_656 ? C28 O17 Dy3 125.3(7) . . ? C29 O18 Dy3 138.4(7) . . ? C29 O18 Dy2 89.6(6) . . ? Dy3 O18 Dy2 131.3(3) . . ? C29 O19 Dy2 99.8(7) . . ? C30 O20 Dy3 138.4(8) . 1_455 ? C30 O21 Dy3 153.2(6) . 2_566 ? Dy1 O22 H22A 105.0 . . ? Dy1 O22 H22B 141.1 . . ? H22A O22 H22B 111.1 . . ? Dy3 O23 H23A 117.3 . . ? Dy3 O23 H23B 119.8 . . ? H23A O23 H23B 110.7 . . ? H24A O24 H24B 109.5 . . ? H25A O25 H25B 109.5 . . ? 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 O1 C1 C2 C3 177.7(10) . . . . ? C6 C1 C2 C3 -0.6(17) . . . . ? O1 C1 C2 C9 -1.2(17) . . . . ? C6 C1 C2 C9 -179.5(10) . . . . ? C1 C2 C3 C4 2.1(17) . . . . ? C9 C2 C3 C4 -179.0(10) . . . . ? C2 C3 C4 C5 -2.0(16) . . . . ? C2 C3 C4 C10 172.5(10) . . . . ? C3 C4 C5 C6 0.5(17) . . . . ? C10 C4 C5 C6 -174.0(10) . . . . ? C4 C5 C6 C1 0.9(17) . . . . ? O1 C1 C6 C5 -179.2(10) . . . . ? C2 C1 C6 C5 -0.9(16) . . . . ? O1 C7 C8 O3 -8.9(14) . . . . ? O1 C7 C8 O2 171.0(10) . . . . ? C3 C2 C9 O5 -4.7(15) . . . . ? C1 C2 C9 O5 174.3(11) . . . . ? C3 C2 C9 O4 173.1(10) . . . . ? C1 C2 C9 O4 -7.9(17) . . . . ? C5 C4 C10 O6 -171.1(10) . . . . ? C3 C4 C10 O6 14.6(17) . . . . ? C5 C4 C10 O7 11.2(16) . . . . ? C3 C4 C10 O7 -163.1(10) . . . . ? O8 C11 C12 C13 173.8(10) . . . . ? C16 C11 C12 C13 -5.8(18) . . . . ? O8 C11 C12 C19 -1.8(18) . . . . ? C16 C11 C12 C19 178.5(11) . . . . ? C11 C12 C13 C14 3.2(17) . . . . ? C19 C12 C13 C14 179.1(10) . . . . ? C12 C13 C14 C15 -0.1(17) . . . . ? C12 C13 C14 C20 178.1(10) . . . . ? C13 C14 C15 C16 -0.3(18) . . . . ? C20 C14 C15 C16 -178.4(11) . . . . ? C14 C15 C16 C11 -2.2(17) . . . . ? C12 C11 C16 C15 5.3(18) . . . . ? O8 C11 C16 C15 -174.4(10) . . . . ? O8 C17 C18 O10 -9.4(16) . . . . ? O8 C17 C18 O9 178.8(10) . . . . ? C11 C12 C19 O12 -155.6(11) . . . . ? C13 C12 C19 O12 28.5(16) . . . . ? C11 C12 C19 O11 24.5(18) . . . . ? C13 C12 C19 O11 -151.3(11) . . . . ? C15 C14 C20 O13 164.3(11) . . . . ? C13 C14 C20 O13 -13.9(16) . . . . ? C15 C14 C20 O14 -13.6(17) . . . . ? C13 C14 C20 O14 168.3(11) . . . . ? C26 C21 C22 C23 0.4(16) . . . . ? O15 C21 C22 C23 -179.4(9) . . . . ? C26 C21 C22 C29 -175.6(10) . . . . ? O15 C21 C22 C29 4.6(16) . . . . ? C21 C22 C23 C24 -2.8(16) . . . . ? C29 C22 C23 C24 173.1(10) . . . . ? C22 C23 C24 C25 2.4(16) . . . . ? C22 C23 C24 C30 -179.1(10) . . . . ? C23 C24 C25 C26 0.6(16) . . . . ? C30 C24 C25 C26 -177.9(10) . . . . ? C24 C25 C26 C21 -3.0(16) . . . . ? C22 C21 C26 C25 2.5(16) . . . . ? O15 C21 C26 C25 -177.7(9) . . . . ? O15 C27 C28 O17 7.3(14) . . . . ? O15 C27 C28 O16 -169.3(9) . . . . ? C23 C22 C29 O19 26.2(16) . . . . ? C21 C22 C29 O19 -158.0(10) . . . . ? C23 C22 C29 O18 -153.5(10) . . . . ? C21 C22 C29 O18 22.2(16) . . . . ? C23 C22 C29 Dy2 5(8) . . . . ? C21 C22 C29 Dy2 -180(100) . . . . ? O16 Dy2 C29 O19 104.1(7) 2_656 . . . ? O6 Dy2 C29 O19 -174.5(6) . . . . ? O14 Dy2 C29 O19 20.3(7) 2_557 . . . ? O11 Dy2 C29 O19 -101.3(7) . . . . ? O10 Dy2 C29 O19 85.7(17) . . . . ? O18 Dy2 C29 O19 177.5(11) . . . . ? O8 Dy2 C29 O19 -65.0(7) . . . . ? O16 Dy2 C29 O18 -73.5(6) 2_656 . . . ? O6 Dy2 C29 O18 8.0(6) . . . . ? O14 Dy2 C29 O18 -157.2(6) 2_557 . . . ? O11 Dy2 C29 O18 81.1(6) . . . . ? O10 Dy2 C29 O18 -91.8(16) . . . . ? O19 Dy2 C29 O18 -177.5(11) . . . . ? O8 Dy2 C29 O18 117.5(6) . . . . ? O16 Dy2 C29 C22 127(7) 2_656 . . . ? O6 Dy2 C29 C22 -151(7) . . . . ? O14 Dy2 C29 C22 43(7) 2_557 . . . ? O11 Dy2 C29 C22 -78(7) . . . . ? O10 Dy2 C29 C22 109(7) . . . . ? O19 Dy2 C29 C22 23(7) . . . . ? O18 Dy2 C29 C22 -159(7) . . . . ? O8 Dy2 C29 C22 -42(7) . . . . ? C23 C24 C30 O21 147.7(10) . . . . ? C25 C24 C30 O21 -33.9(15) . . . . ? C23 C24 C30 O20 -33.9(16) . . . . ? C25 C24 C30 O20 144.5(11) . . . . ? C6 C1 O1 C7 -0.5(14) . . . . ? C2 C1 O1 C7 -178.8(10) . . . . ? C6 C1 O1 Dy1 151.3(8) . . . . ? C2 C1 O1 Dy1 -27.0(14) . . . . ? C8 C7 O1 C1 -175.6(8) . . . . ? C8 C7 O1 Dy1 29.2(10) . . . . ? O4 Dy1 O1 C1 42.5(7) . . . . ? O9 Dy1 O1 C1 -173.1(7) 2_747 . . . ? O5 Dy1 O1 C1 5.6(9) 2_747 . . . ? O13 Dy1 O1 C1 -45.7(7) 2_657 . . . ? O12 Dy1 O1 C1 112.7(8) 1_645 . . . ? O3 Dy1 O1 C1 178.6(8) . . . . ? O22 Dy1 O1 C1 -113.2(7) . . . . ? O4 Dy1 O1 C7 -165.1(7) . . . . ? O9 Dy1 O1 C7 -20.6(9) 2_747 . . . ? O5 Dy1 O1 C7 158.1(6) 2_747 . . . ? O13 Dy1 O1 C7 106.8(7) 2_657 . . . ? O12 Dy1 O1 C7 -94.9(7) 1_645 . . . ? O3 Dy1 O1 C7 -29.0(6) . . . . ? O22 Dy1 O1 C7 39.3(6) . . . . ? O3 C8 O2 Dy3 161.5(8) . . . 2_756 ? C7 C8 O2 Dy3 -18.4(18) . . . 2_756 ? O2 C8 O3 Dy1 157.4(8) . . . . ? C7 C8 O3 Dy1 -22.7(14) . . . . ? O4 Dy1 O3 C8 70.8(9) . . . . ? O9 Dy1 O3 C8 -146.8(9) 2_747 . . . ? O5 Dy1 O3 C8 -165.9(9) 2_747 . . . ? O13 Dy1 O3 C8 -18.1(10) 2_657 . . . ? O12 Dy1 O3 C8 136.4(9) 1_645 . . . ? O22 Dy1 O3 C8 -72.3(9) . . . . ? O1 Dy1 O3 C8 28.1(8) . . . . ? O5 C9 O4 Dy1 -121.2(10) . . . . ? C2 C9 O4 Dy1 61.1(14) . . . . ? O9 Dy1 O4 C9 151.9(9) 2_747 . . . ? O5 Dy1 O4 C9 93.3(10) 2_747 . . . ? O13 Dy1 O4 C9 9.5(10) 2_657 . . . ? O12 Dy1 O4 C9 -167.6(10) 1_645 . . . ? O3 Dy1 O4 C9 -103.5(10) . . . . ? O22 Dy1 O4 C9 -16.1(12) . . . . ? O1 Dy1 O4 C9 -62.7(9) . . . . ? O4 C9 O5 Dy1 39.8(19) . . . 2_747 ? C2 C9 O5 Dy1 -142.5(9) . . . 2_747 ? O7 C10 O6 Dy2 67.7(14) . . . . ? C4 C10 O6 Dy2 -109.8(11) . . . . ? O16 Dy2 O6 C10 25.9(10) 2_656 . . . ? O14 Dy2 O6 C10 96.5(11) 2_557 . . . ? O11 Dy2 O6 C10 -124.1(10) . . . . ? O10 Dy2 O6 C10 113.2(10) . . . . ? O19 Dy2 O6 C10 -59.1(10) . . . . ? O18 Dy2 O6 C10 -52.4(10) . . . . ? O8 Dy2 O6 C10 172.9(10) . . . . ? C29 Dy2 O6 C10 -56.0(10) . . . . ? O6 C10 O7 Dy3 -6(2) . . . . ? C4 C10 O7 Dy3 172.0(8) . . . . ? O21 Dy3 O7 C10 39.5(14) 2_566 . . . ? O2 Dy3 O7 C10 -173.1(12) 2_756 . . . ? O20 Dy3 O7 C10 128.5(13) 1_655 . . . ? O18 Dy3 O7 C10 -30.3(12) . . . . ? O17 Dy3 O7 C10 -116.3(13) . . . . ? O23 Dy3 O7 C10 47.5(12) . . . . ? O15 Dy3 O7 C10 -81.6(13) . . . . ? C12 C11 O8 C17 149.6(11) . . . . ? C16 C11 O8 C17 -30.7(15) . . . . ? C12 C11 O8 Dy2 -42.4(14) . . . . ? C16 C11 O8 Dy2 137.2(9) . . . . ? C18 C17 O8 C11 172.6(10) . . . . ? C18 C17 O8 Dy2 3.6(12) . . . . ? O16 Dy2 O8 C11 -152.4(7) 2_656 . . . ? O6 Dy2 O8 C11 121.7(8) . . . . ? O14 Dy2 O8 C11 -90.7(8) 2_557 . . . ? O11 Dy2 O8 C11 45.9(8) . . . . ? O10 Dy2 O8 C11 -167.0(9) . . . . ? O19 Dy2 O8 C11 -17.8(8) . . . . ? O18 Dy2 O8 C11 41.0(9) . . . . ? C29 Dy2 O8 C11 7.1(9) . . . . ? O16 Dy2 O8 C17 15.4(10) 2_656 . . . ? O6 Dy2 O8 C17 -70.5(7) . . . . ? O14 Dy2 O8 C17 77.1(7) 2_557 . . . ? O11 Dy2 O8 C17 -146.3(8) . . . . ? O10 Dy2 O8 C17 0.8(7) . . . . ? O19 Dy2 O8 C17 150.0(7) . . . . ? O18 Dy2 O8 C17 -151.2(7) . . . . ? C29 Dy2 O8 C17 175.0(7) . . . . ? O10 C18 O9 Dy1 37(3) . . . 2_747 ? C17 C18 O9 Dy1 -152(2) . . . 2_747 ? O9 C18 O10 Dy2 -176.7(9) . . . . ? C17 C18 O10 Dy2 12.6(17) . . . . ? O16 Dy2 O10 C18 -179.7(11) 2_656 . . . ? O6 Dy2 O10 C18 96.1(11) . . . . ? O14 Dy2 O10 C18 -93.3(11) 2_557 . . . ? O11 Dy2 O10 C18 26.3(12) . . . . ? O19 Dy2 O10 C18 -96.3(12) . . . . ? O18 Dy2 O10 C18 127.4(10) . . . . ? O8 Dy2 O10 C18 -7.5(10) . . . . ? C29 Dy2 O10 C18 -161.3(15) . . . . ? O12 C19 O11 Dy2 -172.3(8) . . . . ? C12 C19 O11 Dy2 8(2) . . . . ? O16 Dy2 O11 C19 165.3(13) 2_656 . . . ? O6 Dy2 O11 C19 -133.1(14) . . . . ? O14 Dy2 O11 C19 21.9(15) 2_557 . . . ? O10 Dy2 O11 C19 -65.2(15) . . . . ? O19 Dy2 O11 C19 91.0(14) . . . . ? O18 Dy2 O11 C19 144.1(15) . . . . ? O8 Dy2 O11 C19 -32.2(14) . . . . ? C29 Dy2 O11 C19 116.3(15) . . . . ? O11 C19 O12 Dy1 -118.5(14) . . . 1_465 ? C12 C19 O12 Dy1 61.7(19) . . . 1_465 ? O14 C20 O13 Dy1 37(2) . . . 2_657 ? C14 C20 O13 Dy1 -140.6(10) . . . 2_657 ? O13 C20 O14 Dy2 129.2(12) . . . 2_557 ? C14 C20 O14 Dy2 -53(2) . . . 2_557 ? C26 C21 O15 C27 -74.0(12) . . . . ? C22 C21 O15 C27 105.8(11) . . . . ? C26 C21 O15 Dy3 125.5(9) . . . . ? C22 C21 O15 Dy3 -54.7(12) . . . . ? C28 C27 O15 C21 -154.9(9) . . . . ? C28 C27 O15 Dy3 6.3(11) . . . . ? O7 Dy3 O15 C21 111.9(7) . . . . ? O21 Dy3 O15 C21 -39.8(7) 2_566 . . . ? O2 Dy3 O15 C21 -131.0(8) 2_756 . . . ? O20 Dy3 O15 C21 -127.8(7) 1_655 . . . ? O18 Dy3 O15 C21 55.1(7) . . . . ? O17 Dy3 O15 C21 148.9(8) . . . . ? O23 Dy3 O15 C21 10.7(8) . . . . ? O7 Dy3 O15 C27 -47.7(8) . . . . ? O21 Dy3 O15 C27 160.6(7) 2_566 . . . ? O2 Dy3 O15 C27 69.4(7) 2_756 . . . ? O20 Dy3 O15 C27 72.6(8) 1_655 . . . ? O18 Dy3 O15 C27 -104.5(7) . . . . ? O17 Dy3 O15 C27 -10.7(7) . . . . ? O23 Dy3 O15 C27 -148.9(6) . . . . ? O17 C28 O16 Dy2 54(31) . . . 2_656 ? C27 C28 O16 Dy2 -130(31) . . . 2_656 ? O16 C28 O17 Dy3 156.6(8) . . . . ? C27 C28 O17 Dy3 -19.6(14) . . . . ? O7 Dy3 O17 C28 166.2(9) . . . . ? O21 Dy3 O17 C28 4.4(10) 2_566 . . . ? O2 Dy3 O17 C28 -61.5(9) 2_756 . . . ? O20 Dy3 O17 C28 -128.2(9) 1_655 . . . ? O18 Dy3 O17 C28 83.9(9) . . . . ? O23 Dy3 O17 C28 140.2(8) . . . . ? O15 Dy3 O17 C28 16.4(8) . . . . ? O19 C29 O18 Dy3 -172.6(6) . . . . ? C22 C29 O18 Dy3 7.1(17) . . . . ? Dy2 C29 O18 Dy3 -170.3(10) . . . . ? O19 C29 O18 Dy2 -2.3(10) . . . . ? C22 C29 O18 Dy2 177.4(9) . . . . ? O7 Dy3 O18 C29 -172.2(10) . . . . ? O21 Dy3 O18 C29 37.5(10) 2_566 . . . ? O2 Dy3 O18 C29 -43.4(12) 2_756 . . . ? O20 Dy3 O18 C29 148.4(9) 1_655 . . . ? O17 Dy3 O18 C29 -99.3(10) . . . . ? O23 Dy3 O18 C29 112.2(10) . . . . ? O15 Dy3 O18 C29 -34.5(10) . . . . ? O7 Dy3 O18 Dy2 20.7(4) . . . . ? O21 Dy3 O18 Dy2 -129.6(4) 2_566 . . . ? O2 Dy3 O18 Dy2 149.6(3) 2_756 . . . ? O20 Dy3 O18 Dy2 -18.6(7) 1_655 . . . ? O17 Dy3 O18 Dy2 93.6(4) . . . . ? O23 Dy3 O18 Dy2 -54.9(4) . . . . ? O15 Dy3 O18 Dy2 158.4(5) . . . . ? O16 Dy2 O18 C29 102.3(6) 2_656 . . . ? O6 Dy2 O18 C29 -172.2(6) . . . . ? O14 Dy2 O18 C29 28.2(7) 2_557 . . . ? O11 Dy2 O18 C29 -89.8(6) . . . . ? O10 Dy2 O18 C29 157.0(6) . . . . ? O19 Dy2 O18 C29 1.3(6) . . . . ? O8 Dy2 O18 C29 -85.1(7) . . . . ? O16 Dy2 O18 Dy3 -86.3(4) 2_656 . . . ? O6 Dy2 O18 Dy3 -0.8(4) . . . . ? O14 Dy2 O18 Dy3 -160.3(3) 2_557 . . . ? O11 Dy2 O18 Dy3 81.6(4) . . . . ? O10 Dy2 O18 Dy3 -31.6(7) . . . . ? O19 Dy2 O18 Dy3 172.8(5) . . . . ? O8 Dy2 O18 Dy3 86.3(5) . . . . ? C29 Dy2 O18 Dy3 171.4(9) . . . . ? O18 C29 O19 Dy2 2.5(11) . . . . ? C22 C29 O19 Dy2 -177.2(8) . . . . ? O16 Dy2 O19 C29 -74.8(7) 2_656 . . . ? O6 Dy2 O19 C29 7.1(8) . . . . ? O14 Dy2 O19 C29 -159.9(7) 2_557 . . . ? O11 Dy2 O19 C29 72.3(7) . . . . ? O10 Dy2 O19 C29 -157.0(7) . . . . ? O18 Dy2 O19 C29 -1.4(6) . . . . ? O8 Dy2 O19 C29 127.9(6) . . . . ? O21 C30 O20 Dy3 46.8(17) . . . 1_455 ? C24 C30 O20 Dy3 -131.5(9) . . . 1_455 ? O20 C30 O21 Dy3 23(2) . . . 2_566 ? C24 C30 O21 Dy3 -158.6(8) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.288 _refine_diff_density_min -1.818 _refine_diff_density_rms 0.259 _database_code_depnum_ccdc_archive 'CCDC 946974' ####################################################################### # # 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_c100526k _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 Eu3 O25' _chemical_formula_weight 1239.36 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' Eu Eu -0.1578 3.6682 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.127(2) _cell_length_b 12.181(2) _cell_length_c 14.963(3) _cell_angle_alpha 68.50(3) _cell_angle_beta 84.11(3) _cell_angle_gamma 74.81(3) _cell_volume 1657.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1085 _cell_measurement_theta_min 2.5105 _cell_measurement_theta_max 28.7933 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 5.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5016 _exptl_absorpt_correction_T_max 0.5987 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number 3908 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9700 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_unetI/netI 0.0690 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5801 _reflns_number_gt 4731 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR: the parameter to go anisotropic restraint to appointed atoms. SIMU: the parameter to set some atoms in limited range having the save shift parameters, and this parameter always is used with ISOR. simu 0.001 c17 o8 o9 o11 c27 c1 c18 o22 isor 0.005 c17 o8 o9 o11 c27 c1 c18 o22 ; _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^)+(0.0364P)^2^+0.9051P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5801 _refine_ls_number_parameters 514 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.050 _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 Eu1 Eu 1.24524(4) -0.52008(3) 0.89992(3) 0.01397(12) Uani 1 1 d . . . Eu2 Eu 0.35702(4) -0.02267(3) 0.78447(3) 0.01293(12) Uani 1 1 d . . . Eu3 Eu 0.49152(4) 0.28762(3) 0.54304(3) 0.01133(11) Uani 1 1 d . . . C1 C 1.0217(9) -0.2450(7) 0.7353(6) 0.0169(19) Uani 1 1 d U . . C2 C 0.9166(8) -0.2704(7) 0.8021(6) 0.0124(18) Uani 1 1 d . . . C3 C 0.8001(8) -0.1778(7) 0.7961(6) 0.0148(18) Uani 1 1 d . . . H3 H 0.7297 -0.1925 0.8405 0.018 Uiso 1 1 calc R . . C4 C 0.7861(8) -0.0633(7) 0.7250(6) 0.0150(19) Uani 1 1 d . . . C5 C 0.8920(9) -0.0405(8) 0.6601(7) 0.025(2) Uani 1 1 d . . . H5 H 0.8835 0.0359 0.6126 0.030 Uiso 1 1 calc R . . C6 C 1.0096(9) -0.1299(8) 0.6654(7) 0.024(2) Uani 1 1 d . . . H6 H 1.0810 -0.1135 0.6222 0.029 Uiso 1 1 calc R . . C7 C 1.2453(8) -0.2999(7) 0.6695(6) 0.0176(19) Uani 1 1 d . . . H7A H 1.2792 -0.2371 0.6783 0.021 Uiso 1 1 calc R . . H7B H 1.2063 -0.2679 0.6058 0.021 Uiso 1 1 calc R . . C8 C 1.3605(9) -0.4090(7) 0.6787(6) 0.0172(19) Uani 1 1 d . . . C9 C 0.9177(9) -0.3912(7) 0.8810(6) 0.0165(19) Uani 1 1 d . . . C10 C 0.6568(8) 0.0311(7) 0.7148(6) 0.0152(19) Uani 1 1 d . . . C11 C 0.1992(9) 0.0172(7) 1.0068(6) 0.0177(19) Uani 1 1 d . . . C12 C 0.1567(9) 0.1410(7) 0.9577(6) 0.0172(19) Uani 1 1 d . . . C13 C 0.0426(9) 0.2067(7) 0.9907(6) 0.0179(19) Uani 1 1 d . . . H13 H 0.0156 0.2905 0.9595 0.021 Uiso 1 1 calc R . . C14 C -0.0323(8) 0.1516(7) 1.0687(6) 0.0169(19) Uani 1 1 d . . . C15 C 0.0154(9) 0.0288(7) 1.1182(6) 0.020(2) Uani 1 1 d . . . H15 H -0.0319 -0.0089 1.1726 0.024 Uiso 1 1 calc R . . C16 C 0.1310(9) -0.0396(7) 1.0894(6) 0.020(2) Uani 1 1 d . . . H16 H 0.1627 -0.1220 1.1245 0.024 Uiso 1 1 calc R . . C17 C 0.3860(10) -0.1574(8) 1.0372(7) 0.0285(10) Uani 1 1 d U . . H17A H 0.3245 -0.2060 1.0757 0.034 Uiso 1 1 calc R . . H17B H 0.4329 -0.1366 1.0799 0.034 Uiso 1 1 calc R . . C18 C 0.4885(10) -0.2299(8) 0.9883(7) 0.0292(10) Uani 1 1 d U . . C19 C 0.2277(9) 0.2114(7) 0.8708(6) 0.019(2) Uani 1 1 d . . . C20 C -0.1522(8) 0.2246(7) 1.1008(6) 0.0151(19) Uani 1 1 d . . . C21 C 0.1735(8) 0.3260(7) 0.4517(6) 0.0160(19) Uani 1 1 d . . . C22 C 0.1195(8) 0.2648(7) 0.5402(6) 0.0155(19) Uani 1 1 d . . . C23 C -0.0194(9) 0.2987(7) 0.5545(6) 0.022(2) Uani 1 1 d . . . H23 H -0.0588 0.2558 0.6111 0.027 Uiso 1 1 calc R . . C24 C -0.1019(8) 0.3965(7) 0.4853(6) 0.0159(19) Uani 1 1 d . . . C25 C -0.0451(9) 0.4564(7) 0.3995(6) 0.020(2) Uani 1 1 d . . . H25 H -0.0998 0.5223 0.3536 0.024 Uiso 1 1 calc R . . C26 C 0.0918(9) 0.4193(8) 0.3813(6) 0.021(2) Uani 1 1 d . . . H26 H 0.1290 0.4569 0.3219 0.025 Uiso 1 1 calc R . . C27 C 0.3525(10) 0.2298(9) 0.3690(7) 0.033(2) Uani 1 1 d U . . H27A H 0.3439 0.2870 0.3034 0.039 Uiso 1 1 calc R . . H27B H 0.2923 0.1765 0.3774 0.039 Uiso 1 1 calc R . . C28 C 0.4979(9) 0.1560(8) 0.3872(7) 0.022(2) Uani 1 1 d . . . C29 C 0.2078(8) 0.1672(7) 0.6194(6) 0.0168(19) Uani 1 1 d . . . C30 C -0.2545(9) 0.4354(8) 0.5034(6) 0.0170(19) Uani 1 1 d . . . O1 O 1.1414(6) -0.3330(5) 0.7408(4) 0.0181(13) Uani 1 1 d . . . O2 O 1.4508(6) -0.4014(5) 0.6163(4) 0.0209(14) Uani 1 1 d . . . O3 O 1.3576(6) -0.5038(5) 0.7492(4) 0.0254(15) Uani 1 1 d . . . O4 O 1.0124(6) -0.4811(5) 0.8822(4) 0.0183(13) Uani 1 1 d . . . O5 O 0.8190(6) -0.3941(5) 0.9391(4) 0.0193(13) Uani 1 1 d . . . O6 O 0.5663(6) 0.0171(5) 0.7786(4) 0.0191(13) Uani 1 1 d . . . O7 O 0.6431(6) 0.1203(5) 0.6360(4) 0.0275(15) Uani 1 1 d . . . O8 O 0.3095(6) -0.0496(5) 0.9698(4) 0.0265(10) Uani 1 1 d U . . O9 O 0.5630(7) -0.3232(5) 1.0446(5) 0.0315(11) Uani 1 1 d U . . O10 O 0.4867(7) -0.1981(5) 0.9005(4) 0.0300(16) Uani 1 1 d . . . O11 O 0.2974(6) 0.1555(5) 0.8196(4) 0.0259(15) Uani 1 1 d U . . O12 O 0.2158(7) 0.3200(5) 0.8548(5) 0.0287(16) Uani 1 1 d . . . O13 O -0.1739(6) 0.3369(5) 1.0663(4) 0.0222(14) Uani 1 1 d . . . O14 O -0.2298(6) 0.1687(5) 1.1658(4) 0.0243(15) Uani 1 1 d . . . O15 O 0.3132(5) 0.2945(5) 0.4339(4) 0.0151(13) Uani 1 1 d . . . O16 O 0.5480(6) 0.1103(5) 0.3255(4) 0.0245(15) Uani 1 1 d . . . O17 O 0.5551(6) 0.1472(5) 0.4583(4) 0.0197(14) Uani 1 1 d . . . O18 O 0.3336(6) 0.1642(5) 0.6240(4) 0.0171(13) Uani 1 1 d . . . O19 O 0.1557(6) 0.0898(5) 0.6826(5) 0.0291(16) Uani 1 1 d . . . O20 O -0.3137(6) 0.3561(5) 0.5544(4) 0.0249(15) Uani 1 1 d . . . O21 O -0.3132(4) 0.5467(3) 0.4671(2) 0.0224(14) Uani 1 1 d . . . O22 O 1.4364(4) -0.4308(3) 0.8896(2) 0.048(2) Uani 1 1 d RU . . H22A H 1.4000 -0.3585 0.8886 0.058 Uiso 1 1 d R . . H22B H 1.5203 -0.4389 0.8728 0.058 Uiso 1 1 d R . . O23 O 0.4706(4) 0.2971(3) 0.7001(2) 0.0248(15) Uani 1 1 d R . . H23A H 0.4620 0.2328 0.7471 0.030 Uiso 1 1 d R . . H23B H 0.4212 0.3610 0.7094 0.030 Uiso 1 1 d R . . O24 O 0.6986(4) 0.4709(3) 0.8480(2) 0.101(4) Uani 1 1 d R . . H24A H 0.7528 0.4945 0.8725 0.152 Uiso 1 1 d R . . H24B H 0.7145 0.3931 0.8715 0.152 Uiso 1 1 d R . . O25 O 0.7241(10) 0.3212(10) 0.7529(7) 0.090(3) Uani 1 1 d . . . H25A H 0.6692 0.2775 0.7559 0.135 Uiso 1 1 d R . . H25B H 0.7303 0.3692 0.6946 0.135 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0132(2) 0.0106(2) 0.0133(2) -0.00300(17) 0.00299(18) 0.00215(16) Eu2 0.0119(2) 0.0105(2) 0.0141(2) -0.00414(17) 0.00233(18) -0.00023(16) Eu3 0.0077(2) 0.0116(2) 0.0117(2) -0.00267(17) 0.00126(18) 0.00009(16) C1 0.013(4) 0.014(3) 0.019(4) -0.005(3) 0.000(3) 0.003(3) C2 0.007(4) 0.010(4) 0.018(5) -0.004(3) -0.002(4) 0.001(3) C3 0.012(5) 0.017(4) 0.013(5) -0.005(4) 0.002(4) -0.001(3) C4 0.010(5) 0.016(4) 0.019(5) -0.009(4) -0.007(4) 0.003(3) C5 0.019(5) 0.019(5) 0.028(6) 0.003(4) 0.001(4) -0.003(4) C6 0.014(5) 0.022(5) 0.028(6) 0.001(4) 0.000(4) -0.002(4) C7 0.015(5) 0.020(4) 0.014(5) -0.003(4) 0.005(4) -0.003(4) C8 0.021(5) 0.013(4) 0.017(5) -0.004(4) -0.004(4) -0.003(4) C9 0.016(5) 0.012(4) 0.019(5) -0.006(4) 0.001(4) -0.001(4) C10 0.012(5) 0.006(4) 0.025(5) -0.003(4) -0.006(4) 0.000(3) C11 0.017(5) 0.021(5) 0.020(5) -0.015(4) 0.000(4) -0.003(4) C12 0.021(5) 0.020(4) 0.016(5) -0.012(4) 0.000(4) -0.007(4) C13 0.017(5) 0.016(4) 0.024(5) -0.014(4) 0.004(4) -0.001(4) C14 0.011(5) 0.022(5) 0.021(5) -0.010(4) 0.004(4) -0.007(4) C15 0.018(5) 0.021(5) 0.017(5) -0.003(4) 0.007(4) -0.006(4) C16 0.016(5) 0.016(4) 0.028(6) -0.008(4) 0.005(4) -0.003(4) C17 0.0248(19) 0.0262(17) 0.0237(19) -0.0069(15) 0.0010(16) 0.0086(15) C18 0.0248(19) 0.0271(17) 0.0241(19) -0.0061(15) 0.0012(16) 0.0085(15) C19 0.012(5) 0.018(5) 0.025(5) -0.010(4) 0.003(4) 0.001(4) C20 0.014(5) 0.015(4) 0.018(5) -0.007(4) 0.000(4) -0.005(4) C21 0.009(5) 0.018(4) 0.028(5) -0.019(4) 0.002(4) -0.002(3) C22 0.012(5) 0.010(4) 0.019(5) -0.004(4) -0.002(4) 0.004(3) C23 0.023(5) 0.019(5) 0.022(5) -0.002(4) 0.003(4) -0.009(4) C24 0.014(5) 0.013(4) 0.022(5) -0.010(4) 0.001(4) -0.002(3) C25 0.015(5) 0.018(4) 0.025(5) -0.006(4) -0.005(4) -0.001(4) C26 0.010(5) 0.028(5) 0.019(5) -0.002(4) -0.002(4) -0.003(4) C27 0.030(4) 0.040(4) 0.033(4) -0.021(3) 0.003(4) -0.004(3) C28 0.021(5) 0.023(5) 0.022(5) -0.007(4) 0.000(4) -0.007(4) C29 0.008(5) 0.018(4) 0.019(5) -0.004(4) 0.003(4) 0.001(4) C30 0.018(5) 0.024(5) 0.013(5) -0.012(4) -0.005(4) -0.003(4) O1 0.013(3) 0.010(3) 0.021(3) -0.001(2) 0.008(3) 0.003(2) O2 0.018(4) 0.021(3) 0.017(3) -0.004(3) 0.009(3) 0.000(3) O3 0.034(4) 0.018(3) 0.017(3) 0.000(3) 0.008(3) -0.004(3) O4 0.019(4) 0.012(3) 0.020(3) -0.004(3) 0.000(3) -0.001(3) O5 0.020(4) 0.018(3) 0.012(3) 0.000(2) 0.007(3) 0.000(3) O6 0.006(3) 0.018(3) 0.030(4) -0.009(3) 0.000(3) 0.002(2) O7 0.022(4) 0.027(3) 0.018(4) -0.001(3) 0.000(3) 0.009(3) O8 0.024(2) 0.0242(18) 0.0228(19) -0.0083(16) 0.0003(17) 0.0080(16) O9 0.026(2) 0.0289(18) 0.025(2) -0.0043(16) 0.0019(17) 0.0096(16) O10 0.033(4) 0.024(3) 0.019(4) -0.002(3) 0.001(3) 0.008(3) O11 0.029(3) 0.020(3) 0.029(3) -0.014(2) 0.018(3) -0.005(2) O12 0.036(4) 0.018(3) 0.036(4) -0.015(3) 0.017(3) -0.012(3) O13 0.026(4) 0.014(3) 0.024(4) -0.006(3) 0.006(3) -0.003(3) O14 0.024(4) 0.024(3) 0.029(4) -0.011(3) 0.013(3) -0.014(3) O15 0.006(3) 0.023(3) 0.015(3) -0.010(3) 0.002(3) 0.001(2) O16 0.027(4) 0.028(3) 0.025(4) -0.020(3) 0.006(3) -0.005(3) O17 0.016(3) 0.017(3) 0.023(4) -0.007(3) -0.002(3) 0.002(2) O18 0.009(3) 0.019(3) 0.020(3) -0.005(3) -0.001(3) -0.001(2) O19 0.015(4) 0.028(4) 0.034(4) 0.002(3) 0.003(3) -0.007(3) O20 0.013(3) 0.026(3) 0.028(4) 0.002(3) 0.002(3) -0.011(3) O21 0.017(3) 0.014(3) 0.030(4) -0.004(3) -0.007(3) 0.003(3) O22 0.036(4) 0.043(3) 0.073(4) -0.028(3) 0.007(3) -0.015(3) O23 0.035(4) 0.016(3) 0.022(4) -0.007(3) 0.000(3) -0.004(3) O24 0.057(7) 0.136(10) 0.149(11) -0.098(9) 0.000(7) -0.019(7) O25 0.085(8) 0.128(9) 0.062(7) -0.027(6) 0.002(6) -0.045(7) _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 Eu1 O4 2.303(6) . ? Eu1 O9 2.309(6) 2_747 ? Eu1 O5 2.347(6) 2_747 ? Eu1 O12 2.377(5) 1_645 ? Eu1 O13 2.379(5) 2_657 ? Eu1 O3 2.384(6) . ? Eu1 O22 2.424(3) . ? Eu1 O1 2.692(6) . ? Eu1 H22A 2.7711 . ? Eu2 O16 2.280(6) 2_656 ? Eu2 O6 2.281(6) . ? Eu2 O14 2.326(6) 2_557 ? Eu2 O11 2.332(5) . ? Eu2 O10 2.363(6) . ? Eu2 O19 2.450(6) . ? Eu2 O18 2.613(6) . ? Eu2 O8 2.678(6) . ? Eu2 C29 2.912(8) . ? Eu3 O7 2.273(6) . ? Eu3 O21 2.297(3) 2_566 ? Eu3 O20 2.377(6) 1_655 ? Eu3 O2 2.379(6) 2_756 ? Eu3 O23 2.381(3) . ? Eu3 O17 2.407(5) . ? Eu3 O18 2.411(6) . ? Eu3 O15 2.522(5) . ? C1 O1 1.378(9) . ? C1 C6 1.392(11) . ? C1 C2 1.398(12) . ? C2 C3 1.386(10) . ? C2 C9 1.510(11) . ? C3 C4 1.392(11) . ? C3 H3 0.9300 . ? C4 C5 1.383(12) . ? C4 C10 1.478(11) . ? C5 C6 1.373(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.444(10) . ? C7 C8 1.494(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.234(10) . ? C8 O3 1.252(10) . ? C9 O4 1.248(9) . ? C9 O5 1.254(10) . ? C10 O6 1.250(10) . ? C10 O7 1.267(10) . ? C11 C12 1.383(11) . ? C11 C16 1.390(12) . ? C11 O8 1.394(10) . ? C12 C13 1.381(11) . ? C12 C19 1.502(12) . ? C13 C14 1.377(12) . ? C13 H13 0.9300 . ? C14 C15 1.379(11) . ? C14 C20 1.457(11) . ? C15 C16 1.378(11) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O8 1.413(10) . ? C17 C18 1.495(12) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O10 1.227(11) . ? C18 O9 1.244(11) . ? C19 O12 1.230(9) . ? C19 O11 1.252(9) . ? C20 O13 1.239(9) . ? C20 O14 1.291(10) . ? C21 C26 1.376(12) . ? C21 O15 1.390(9) . ? C21 C22 1.397(12) . ? C22 C23 1.377(12) . ? C22 C29 1.498(11) . ? C23 C24 1.393(11) . ? C23 H23 0.9300 . ? C24 C25 1.376(12) . ? C24 C30 1.519(12) . ? C25 C26 1.373(12) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 O15 1.429(10) . ? C27 C28 1.503(12) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O17 1.221(10) . ? C28 O16 1.246(10) . ? C29 O19 1.251(10) . ? C29 O18 1.274(9) . ? C30 O20 1.243(10) . ? C30 O21 1.261(9) . ? O2 Eu3 2.379(6) 2_756 ? O5 Eu1 2.347(6) 2_747 ? O9 Eu1 2.309(6) 2_747 ? O12 Eu1 2.377(5) 1_465 ? O13 Eu1 2.379(5) 2_657 ? O14 Eu2 2.326(6) 2_557 ? O16 Eu2 2.280(6) 2_656 ? O20 Eu3 2.377(6) 1_455 ? O21 Eu3 2.297(3) 2_566 ? O22 H22A 0.8561 . ? O22 H22B 0.8512 . ? O23 H23A 0.8574 . ? O23 H23B 0.8573 . ? O24 H24A 0.8484 . ? O24 H24B 0.8576 . ? O25 H25A 0.8523 . ? O25 H25B 0.8601 . ? 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 Eu1 O9 142.3(2) . 2_747 ? O4 Eu1 O5 80.2(2) . 2_747 ? O9 Eu1 O5 80.0(2) 2_747 2_747 ? O4 Eu1 O12 75.5(2) . 1_645 ? O9 Eu1 O12 74.6(2) 2_747 1_645 ? O5 Eu1 O12 94.9(2) 2_747 1_645 ? O4 Eu1 O13 80.24(19) . 2_657 ? O9 Eu1 O13 128.0(2) 2_747 2_657 ? O5 Eu1 O13 82.42(19) 2_747 2_657 ? O12 Eu1 O13 155.7(2) 1_645 2_657 ? O4 Eu1 O3 109.9(2) . . ? O9 Eu1 O3 81.9(2) 2_747 . ? O5 Eu1 O3 159.91(19) 2_747 . ? O12 Eu1 O3 72.0(2) 1_645 . ? O13 Eu1 O3 115.8(2) 2_657 . ? O4 Eu1 O22 145.23(15) . . ? O9 Eu1 O22 72.18(19) 2_747 . ? O5 Eu1 O22 110.32(16) 2_747 . ? O12 Eu1 O22 133.35(17) 1_645 . ? O13 Eu1 O22 69.03(17) 2_657 . ? O3 Eu1 O22 71.68(17) . . ? O4 Eu1 O1 64.97(18) . . ? O9 Eu1 O1 141.8(2) 2_747 . ? O5 Eu1 O1 138.20(18) 2_747 . ? O12 Eu1 O1 97.9(2) 1_645 . ? O13 Eu1 O1 69.98(18) 2_657 . ? O3 Eu1 O1 60.54(18) . . ? O22 Eu1 O1 88.83(14) . . ? O4 Eu1 H22A 128.3 . . ? O9 Eu1 H22A 88.4 2_747 . ? O5 Eu1 H22A 108.4 2_747 . ? O12 Eu1 H22A 148.4 1_645 . ? O13 Eu1 H22A 52.2 2_657 . ? O3 Eu1 H22A 79.5 . . ? O22 Eu1 H22A 17.4 . . ? O1 Eu1 H22A 79.1 . . ? O16 Eu2 O6 83.7(2) 2_656 . ? O16 Eu2 O14 85.5(2) 2_656 2_557 ? O6 Eu2 O14 146.9(2) . 2_557 ? O16 Eu2 O11 146.0(2) 2_656 . ? O6 Eu2 O11 79.2(2) . . ? O14 Eu2 O11 123.7(2) 2_557 . ? O16 Eu2 O10 86.4(2) 2_656 . ? O6 Eu2 O10 75.8(2) . . ? O14 Eu2 O10 72.4(2) 2_557 . ? O11 Eu2 O10 117.0(2) . . ? O16 Eu2 O19 90.4(2) 2_656 . ? O6 Eu2 O19 130.8(2) . . ? O14 Eu2 O19 80.3(2) 2_557 . ? O11 Eu2 O19 79.3(2) . . ? O10 Eu2 O19 152.7(2) . . ? O16 Eu2 O18 77.4(2) 2_656 . ? O6 Eu2 O18 80.08(19) . . ? O14 Eu2 O18 127.52(19) 2_557 . ? O11 Eu2 O18 70.91(19) . . ? O10 Eu2 O18 152.2(2) . . ? O19 Eu2 O18 51.07(19) . . ? O16 Eu2 O8 147.6(2) 2_656 . ? O6 Eu2 O8 95.2(2) . . ? O14 Eu2 O8 77.9(2) 2_557 . ? O11 Eu2 O8 63.78(19) . . ? O10 Eu2 O8 62.25(19) . . ? O19 Eu2 O8 113.6(2) . . ? O18 Eu2 O8 134.48(17) . . ? O16 Eu2 C29 83.7(2) 2_656 . ? O6 Eu2 C29 105.8(2) . . ? O14 Eu2 C29 103.9(2) 2_557 . ? O11 Eu2 C29 73.2(2) . . ? O10 Eu2 C29 169.6(2) . . ? O19 Eu2 C29 25.1(2) . . ? O18 Eu2 C29 25.9(2) . . ? O8 Eu2 C29 127.1(2) . . ? O7 Eu3 O21 148.67(17) . 2_566 ? O7 Eu3 O20 74.4(2) . 1_655 ? O21 Eu3 O20 103.11(16) 2_566 1_655 ? O7 Eu3 O2 121.2(2) . 2_756 ? O21 Eu3 O2 86.34(17) 2_566 2_756 ? O20 Eu3 O2 73.2(2) 1_655 2_756 ? O7 Eu3 O23 73.80(17) . . ? O21 Eu3 O23 75.25(13) 2_566 . ? O20 Eu3 O23 76.84(17) 1_655 . ? O2 Eu3 O23 140.02(15) 2_756 . ? O7 Eu3 O17 72.5(2) . . ? O21 Eu3 O17 134.71(16) 2_566 . ? O20 Eu3 O17 108.9(2) 1_655 . ? O2 Eu3 O17 73.58(19) 2_756 . ? O23 Eu3 O17 142.49(16) . . ? O7 Eu3 O18 81.2(2) . . ? O21 Eu3 O18 86.74(15) 2_566 . ? O20 Eu3 O18 147.52(19) 1_655 . ? O2 Eu3 O18 138.92(19) 2_756 . ? O23 Eu3 O18 75.96(15) . . ? O17 Eu3 O18 83.13(19) . . ? O7 Eu3 O15 127.2(2) . . ? O21 Eu3 O15 71.88(14) 2_566 . ? O20 Eu3 O15 146.12(19) 1_655 . ? O2 Eu3 O15 73.02(19) 2_756 . ? O23 Eu3 O15 130.53(15) . . ? O17 Eu3 O15 63.60(18) . . ? O18 Eu3 O15 66.35(18) . . ? O1 C1 C6 119.2(8) . . ? O1 C1 C2 120.0(7) . . ? C6 C1 C2 120.8(8) . . ? C3 C2 C1 118.0(7) . . ? C3 C2 C9 116.3(7) . . ? C1 C2 C9 125.7(7) . . ? C2 C3 C4 121.4(8) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 119.3(8) . . ? C5 C4 C10 119.9(8) . . ? C3 C4 C10 120.7(8) . . ? C6 C5 C4 120.5(8) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 119.9(9) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? O1 C7 C8 109.7(7) . . ? O1 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O1 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O2 C8 O3 124.0(8) . . ? O2 C8 C7 118.7(7) . . ? O3 C8 C7 117.3(8) . . ? O4 C9 O5 124.7(8) . . ? O4 C9 C2 118.6(8) . . ? O5 C9 C2 116.6(7) . . ? O6 C10 O7 124.1(8) . . ? O6 C10 C4 120.5(7) . . ? O7 C10 C4 115.3(8) . . ? C12 C11 C16 120.7(8) . . ? C12 C11 O8 118.4(8) . . ? C16 C11 O8 120.9(7) . . ? C13 C12 C11 118.7(8) . . ? C13 C12 C19 116.7(7) . . ? C11 C12 C19 124.6(8) . . ? C14 C13 C12 121.8(8) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 118.0(8) . . ? C13 C14 C20 119.9(8) . . ? C15 C14 C20 121.9(8) . . ? C16 C15 C14 122.0(8) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C11 118.5(8) . . ? C15 C16 H16 120.7 . . ? C11 C16 H16 120.7 . . ? O8 C17 C18 111.2(7) . . ? O8 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? O8 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? O10 C18 O9 126.9(9) . . ? O10 C18 C17 119.1(8) . . ? O9 C18 C17 113.8(8) . . ? O12 C19 O11 123.7(8) . . ? O12 C19 C12 118.2(7) . . ? O11 C19 C12 118.0(7) . . ? O13 C20 O14 122.8(8) . . ? O13 C20 C14 119.0(8) . . ? O14 C20 C14 118.2(7) . . ? C26 C21 O15 118.6(8) . . ? C26 C21 C22 121.6(8) . . ? O15 C21 C22 119.9(7) . . ? C23 C22 C21 117.8(8) . . ? C23 C22 C29 119.9(8) . . ? C21 C22 C29 122.3(8) . . ? C22 C23 C24 120.9(8) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 119.6(8) . . ? C25 C24 C30 120.0(8) . . ? C23 C24 C30 120.3(8) . . ? C26 C25 C24 120.4(8) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C21 119.4(9) . . ? C25 C26 H26 120.3 . . ? C21 C26 H26 120.3 . . ? O15 C27 C28 110.1(7) . . ? O15 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? O15 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.2 . . ? O17 C28 O16 126.6(9) . . ? O17 C28 C27 118.6(8) . . ? O16 C28 C27 114.8(8) . . ? O19 C29 O18 120.1(8) . . ? O19 C29 C22 119.2(7) . . ? O18 C29 C22 120.7(7) . . ? O19 C29 Eu2 56.3(4) . . ? O18 C29 Eu2 63.8(4) . . ? C22 C29 Eu2 174.7(6) . . ? O20 C30 O21 123.8(8) . . ? O20 C30 C24 118.2(7) . . ? O21 C30 C24 118.1(7) . . ? C1 O1 C7 116.7(6) . . ? C1 O1 Eu1 126.3(5) . . ? C7 O1 Eu1 112.5(4) . . ? C8 O2 Eu3 144.9(5) . 2_756 ? C8 O3 Eu1 127.8(5) . . ? C9 O4 Eu1 131.7(5) . . ? C9 O5 Eu1 144.3(5) . 2_747 ? C10 O6 Eu2 132.6(5) . . ? C10 O7 Eu3 143.9(6) . . ? C11 O8 C17 116.0(7) . . ? C11 O8 Eu2 126.4(5) . . ? C17 O8 Eu2 116.2(5) . . ? C18 O9 Eu1 158.5(7) . 2_747 ? C18 O10 Eu2 130.8(6) . . ? C19 O11 Eu2 147.1(6) . . ? C19 O12 Eu1 151.2(6) . 1_465 ? C20 O13 Eu1 145.2(6) . 2_657 ? C20 O14 Eu2 147.6(5) . 2_557 ? C21 O15 C27 115.4(6) . . ? C21 O15 Eu3 123.0(4) . . ? C27 O15 Eu3 118.9(5) . . ? C28 O16 Eu2 178.6(6) . 2_656 ? C28 O17 Eu3 125.2(5) . . ? C29 O18 Eu3 138.3(5) . . ? C29 O18 Eu2 90.2(5) . . ? Eu3 O18 Eu2 130.8(2) . . ? C29 O19 Eu2 98.6(5) . . ? C30 O20 Eu3 137.3(5) . 1_455 ? C30 O21 Eu3 152.5(5) . 2_566 ? Eu1 O22 H22A 105.0 . . ? Eu1 O22 H22B 141.2 . . ? H22A O22 H22B 111.2 . . ? Eu3 O23 H23A 117.4 . . ? Eu3 O23 H23B 119.9 . . ? H23A O23 H23B 110.7 . . ? H24A O24 H24B 109.5 . . ? H25A O25 H25B 109.9 . . ? 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 O1 C1 C2 C3 177.6(7) . . . . ? C6 C1 C2 C3 0.4(12) . . . . ? O1 C1 C2 C9 -2.8(12) . . . . ? C6 C1 C2 C9 180.0(8) . . . . ? C1 C2 C3 C4 1.1(12) . . . . ? C9 C2 C3 C4 -178.6(7) . . . . ? C2 C3 C4 C5 -1.4(12) . . . . ? C2 C3 C4 C10 175.0(7) . . . . ? C3 C4 C5 C6 0.3(13) . . . . ? C10 C4 C5 C6 -176.1(8) . . . . ? C4 C5 C6 C1 1.1(13) . . . . ? O1 C1 C6 C5 -178.7(8) . . . . ? C2 C1 C6 C5 -1.4(13) . . . . ? O1 C7 C8 O2 171.4(7) . . . . ? O1 C7 C8 O3 -7.5(10) . . . . ? C3 C2 C9 O4 171.4(7) . . . . ? C1 C2 C9 O4 -8.3(12) . . . . ? C3 C2 C9 O5 -6.1(11) . . . . ? C1 C2 C9 O5 174.3(7) . . . . ? C5 C4 C10 O6 -172.1(7) . . . . ? C3 C4 C10 O6 11.6(11) . . . . ? C5 C4 C10 O7 12.2(11) . . . . ? C3 C4 C10 O7 -164.2(7) . . . . ? C16 C11 C12 C13 -1.9(12) . . . . ? O8 C11 C12 C13 176.3(7) . . . . ? C16 C11 C12 C19 176.8(8) . . . . ? O8 C11 C12 C19 -5.0(12) . . . . ? C11 C12 C13 C14 -2.4(12) . . . . ? C19 C12 C13 C14 178.8(7) . . . . ? C12 C13 C14 C15 4.7(12) . . . . ? C12 C13 C14 C20 -179.8(7) . . . . ? C13 C14 C15 C16 -2.8(13) . . . . ? C20 C14 C15 C16 -178.1(7) . . . . ? C14 C15 C16 C11 -1.3(13) . . . . ? C12 C11 C16 C15 3.7(12) . . . . ? O8 C11 C16 C15 -174.4(7) . . . . ? O8 C17 C18 O10 -7.3(13) . . . . ? O8 C17 C18 O9 176.9(8) . . . . ? C13 C12 C19 O12 25.5(12) . . . . ? C11 C12 C19 O12 -153.2(8) . . . . ? C13 C12 C19 O11 -155.5(8) . . . . ? C11 C12 C19 O11 25.8(12) . . . . ? C13 C14 C20 O13 -10.2(12) . . . . ? C15 C14 C20 O13 165.1(8) . . . . ? C13 C14 C20 O14 171.3(7) . . . . ? C15 C14 C20 O14 -13.5(12) . . . . ? C26 C21 C22 C23 1.4(12) . . . . ? O15 C21 C22 C23 -179.8(7) . . . . ? C26 C21 C22 C29 -177.0(7) . . . . ? O15 C21 C22 C29 1.8(11) . . . . ? C21 C22 C23 C24 -4.3(12) . . . . ? C29 C22 C23 C24 174.1(7) . . . . ? C22 C23 C24 C25 3.3(12) . . . . ? C22 C23 C24 C30 -178.1(7) . . . . ? C23 C24 C25 C26 0.8(12) . . . . ? C30 C24 C25 C26 -177.8(7) . . . . ? C24 C25 C26 C21 -3.7(12) . . . . ? O15 C21 C26 C25 -176.3(7) . . . . ? C22 C21 C26 C25 2.5(12) . . . . ? O15 C27 C28 O17 9.3(12) . . . . ? O15 C27 C28 O16 -170.1(8) . . . . ? C23 C22 C29 O19 24.8(12) . . . . ? C21 C22 C29 O19 -156.9(8) . . . . ? C23 C22 C29 O18 -153.6(8) . . . . ? C21 C22 C29 O18 24.8(12) . . . . ? C23 C22 C29 Eu2 -5(6) . . . . ? C21 C22 C29 Eu2 174(6) . . . . ? O16 Eu2 C29 O19 104.6(5) 2_656 . . . ? O6 Eu2 C29 O19 -173.9(5) . . . . ? O14 Eu2 C29 O19 20.8(6) 2_557 . . . ? O11 Eu2 C29 O19 -100.6(5) . . . . ? O10 Eu2 C29 O19 88.4(14) . . . . ? O18 Eu2 C29 O19 178.6(8) . . . . ? O8 Eu2 C29 O19 -64.4(6) . . . . ? O16 Eu2 C29 O18 -74.0(5) 2_656 . . . ? O6 Eu2 C29 O18 7.5(5) . . . . ? O14 Eu2 C29 O18 -157.8(4) 2_557 . . . ? O11 Eu2 C29 O18 80.8(5) . . . . ? O10 Eu2 C29 O18 -90.2(13) . . . . ? O19 Eu2 C29 O18 -178.6(8) . . . . ? O8 Eu2 C29 O18 117.0(4) . . . . ? O16 Eu2 C29 C22 136(6) 2_656 . . . ? O6 Eu2 C29 C22 -143(6) . . . . ? O14 Eu2 C29 C22 52(6) 2_557 . . . ? O11 Eu2 C29 C22 -69(6) . . . . ? O10 Eu2 C29 C22 120(6) . . . . ? O19 Eu2 C29 C22 31(6) . . . . ? O18 Eu2 C29 C22 -150(6) . . . . ? O8 Eu2 C29 C22 -33(6) . . . . ? C25 C24 C30 O20 147.7(8) . . . . ? C23 C24 C30 O20 -30.9(11) . . . . ? C25 C24 C30 O21 -33.6(10) . . . . ? C23 C24 C30 O21 147.8(7) . . . . ? C6 C1 O1 C7 -2.6(11) . . . . ? C2 C1 O1 C7 -179.9(7) . . . . ? C6 C1 O1 Eu1 151.7(6) . . . . ? C2 C1 O1 Eu1 -25.7(10) . . . . ? C8 C7 O1 C1 -173.5(6) . . . . ? C8 C7 O1 Eu1 28.8(7) . . . . ? O4 Eu1 O1 C1 42.3(6) . . . . ? O9 Eu1 O1 C1 -172.7(5) 2_747 . . . ? O5 Eu1 O1 C1 5.8(7) 2_747 . . . ? O12 Eu1 O1 C1 112.2(6) 1_645 . . . ? O13 Eu1 O1 C1 -46.1(6) 2_657 . . . ? O3 Eu1 O1 C1 176.3(6) . . . . ? O22 Eu1 O1 C1 -114.1(6) . . . . ? O4 Eu1 O1 C7 -162.6(5) . . . . ? O9 Eu1 O1 C7 -17.6(6) 2_747 . . . ? O5 Eu1 O1 C7 160.9(4) 2_747 . . . ? O12 Eu1 O1 C7 -92.6(5) 1_645 . . . ? O13 Eu1 O1 C7 109.1(5) 2_657 . . . ? O3 Eu1 O1 C7 -28.5(5) . . . . ? O22 Eu1 O1 C7 41.0(5) . . . . ? O3 C8 O2 Eu3 160.9(6) . . . 2_756 ? C7 C8 O2 Eu3 -17.9(13) . . . 2_756 ? O2 C8 O3 Eu1 156.4(6) . . . . ? C7 C8 O3 Eu1 -24.7(10) . . . . ? O4 Eu1 O3 C8 73.4(7) . . . . ? O9 Eu1 O3 C8 -143.6(7) 2_747 . . . ? O5 Eu1 O3 C8 -168.9(6) 2_747 . . . ? O12 Eu1 O3 C8 140.0(7) 1_645 . . . ? O13 Eu1 O3 C8 -15.1(8) 2_657 . . . ? O22 Eu1 O3 C8 -69.7(7) . . . . ? O1 Eu1 O3 C8 29.6(6) . . . . ? O5 C9 O4 Eu1 -120.0(8) . . . . ? C2 C9 O4 Eu1 62.8(10) . . . . ? O9 Eu1 O4 C9 151.3(7) 2_747 . . . ? O5 Eu1 O4 C9 92.1(7) 2_747 . . . ? O12 Eu1 O4 C9 -170.2(8) 1_645 . . . ? O13 Eu1 O4 C9 8.2(7) 2_657 . . . ? O3 Eu1 O4 C9 -105.9(7) . . . . ? O22 Eu1 O4 C9 -19.6(9) . . . . ? O1 Eu1 O4 C9 -64.1(7) . . . . ? O4 C9 O5 Eu1 38.2(14) . . . 2_747 ? C2 C9 O5 Eu1 -144.6(7) . . . 2_747 ? O7 C10 O6 Eu2 67.4(10) . . . . ? C4 C10 O6 Eu2 -107.9(8) . . . . ? O16 Eu2 O6 C10 26.6(7) 2_656 . . . ? O14 Eu2 O6 C10 98.1(7) 2_557 . . . ? O11 Eu2 O6 C10 -123.9(7) . . . . ? O10 Eu2 O6 C10 114.4(7) . . . . ? O19 Eu2 O6 C10 -58.5(7) . . . . ? O18 Eu2 O6 C10 -51.7(7) . . . . ? O8 Eu2 O6 C10 174.0(7) . . . . ? C29 Eu2 O6 C10 -55.0(7) . . . . ? O6 C10 O7 Eu3 -6.5(15) . . . . ? C4 C10 O7 Eu3 169.1(6) . . . . ? O21 Eu3 O7 C10 39.6(11) 2_566 . . . ? O20 Eu3 O7 C10 129.2(10) 1_655 . . . ? O2 Eu3 O7 C10 -172.0(9) 2_756 . . . ? O23 Eu3 O7 C10 48.8(9) . . . . ? O17 Eu3 O7 C10 -114.6(10) . . . . ? O18 Eu3 O7 C10 -29.1(9) . . . . ? O15 Eu3 O7 C10 -80.2(10) . . . . ? C12 C11 O8 C17 153.6(8) . . . . ? C16 C11 O8 C17 -28.2(11) . . . . ? C12 C11 O8 Eu2 -40.8(10) . . . . ? C16 C11 O8 Eu2 137.3(7) . . . . ? C18 C17 O8 C11 172.0(7) . . . . ? C18 C17 O8 Eu2 5.0(10) . . . . ? O16 Eu2 O8 C11 -151.9(6) 2_656 . . . ? O6 Eu2 O8 C11 121.7(6) . . . . ? O14 Eu2 O8 C11 -91.1(6) 2_557 . . . ? O11 Eu2 O8 C11 46.4(6) . . . . ? O10 Eu2 O8 C11 -167.4(7) . . . . ? O19 Eu2 O8 C11 -17.4(6) . . . . ? O18 Eu2 O8 C11 40.4(7) . . . . ? C29 Eu2 O8 C11 7.3(7) . . . . ? O16 Eu2 O8 C17 13.6(8) 2_656 . . . ? O6 Eu2 O8 C17 -72.8(6) . . . . ? O14 Eu2 O8 C17 74.4(6) 2_557 . . . ? O11 Eu2 O8 C17 -148.1(6) . . . . ? O10 Eu2 O8 C17 -1.8(6) . . . . ? O19 Eu2 O8 C17 148.1(6) . . . . ? O18 Eu2 O8 C17 -154.1(6) . . . . ? C29 Eu2 O8 C17 172.8(6) . . . . ? O10 C18 O9 Eu1 33(3) . . . 2_747 ? C17 C18 O9 Eu1 -151.6(14) . . . 2_747 ? O9 C18 O10 Eu2 -178.1(7) . . . . ? C17 C18 O10 Eu2 6.7(14) . . . . ? O16 Eu2 O10 C18 -174.5(9) 2_656 . . . ? O6 Eu2 O10 C18 101.1(9) . . . . ? O14 Eu2 O10 C18 -88.2(9) 2_557 . . . ? O11 Eu2 O10 C18 31.3(9) . . . . ? O19 Eu2 O10 C18 -90.8(9) . . . . ? O18 Eu2 O10 C18 131.7(8) . . . . ? O8 Eu2 O10 C18 -2.8(8) . . . . ? C29 Eu2 O10 C18 -158.5(12) . . . . ? O12 C19 O11 Eu2 -170.3(7) . . . . ? C12 C19 O11 Eu2 10.7(15) . . . . ? O16 Eu2 O11 C19 162.3(10) 2_656 . . . ? O6 Eu2 O11 C19 -136.6(11) . . . . ? O14 Eu2 O11 C19 17.3(12) 2_557 . . . ? O10 Eu2 O11 C19 -68.8(11) . . . . ? O19 Eu2 O11 C19 87.9(11) . . . . ? O18 Eu2 O11 C19 140.2(11) . . . . ? O8 Eu2 O11 C19 -35.3(11) . . . . ? C29 Eu2 O11 C19 113.1(11) . . . . ? O11 C19 O12 Eu1 -118.4(11) . . . 1_465 ? C12 C19 O12 Eu1 60.6(15) . . . 1_465 ? O14 C20 O13 Eu1 39.6(14) . . . 2_657 ? C14 C20 O13 Eu1 -138.9(8) . . . 2_657 ? O13 C20 O14 Eu2 128.8(9) . . . 2_557 ? C14 C20 O14 Eu2 -52.7(14) . . . 2_557 ? C26 C21 O15 C27 -74.0(9) . . . . ? C22 C21 O15 C27 107.2(8) . . . . ? C26 C21 O15 Eu3 125.2(6) . . . . ? C22 C21 O15 Eu3 -53.6(8) . . . . ? C28 C27 O15 C21 -155.7(7) . . . . ? C28 C27 O15 Eu3 6.1(10) . . . . ? O7 Eu3 O15 C21 112.2(6) . . . . ? O21 Eu3 O15 C21 -39.5(5) 2_566 . . . ? O20 Eu3 O15 C21 -126.1(6) 1_655 . . . ? O2 Eu3 O15 C21 -131.2(6) 2_756 . . . ? O23 Eu3 O15 C21 11.3(6) . . . . ? O17 Eu3 O15 C21 149.1(6) . . . . ? O18 Eu3 O15 C21 55.0(5) . . . . ? O7 Eu3 O15 C27 -48.1(7) . . . . ? O21 Eu3 O15 C27 160.3(6) 2_566 . . . ? O20 Eu3 O15 C27 73.7(7) 1_655 . . . ? O2 Eu3 O15 C27 68.6(6) 2_756 . . . ? O23 Eu3 O15 C27 -149.0(6) . . . . ? O17 Eu3 O15 C27 -11.2(6) . . . . ? O18 Eu3 O15 C27 -105.3(6) . . . . ? O17 C28 O16 Eu2 31(27) . . . 2_656 ? C27 C28 O16 Eu2 -149(26) . . . 2_656 ? O16 C28 O17 Eu3 156.8(7) . . . . ? C27 C28 O17 Eu3 -22.5(11) . . . . ? O7 Eu3 O17 C28 168.3(7) . . . . ? O21 Eu3 O17 C28 6.9(8) 2_566 . . . ? O20 Eu3 O17 C28 -125.7(7) 1_655 . . . ? O2 Eu3 O17 C28 -60.5(7) 2_756 . . . ? O23 Eu3 O17 C28 141.4(6) . . . . ? O18 Eu3 O17 C28 85.4(7) . . . . ? O15 Eu3 O17 C28 18.4(6) . . . . ? O19 C29 O18 Eu3 -172.1(5) . . . . ? C22 C29 O18 Eu3 6.2(12) . . . . ? Eu2 C29 O18 Eu3 -170.7(7) . . . . ? O19 C29 O18 Eu2 -1.3(8) . . . . ? C22 C29 O18 Eu2 177.0(7) . . . . ? O7 Eu3 O18 C29 -171.9(8) . . . . ? O21 Eu3 O18 C29 37.1(8) 2_566 . . . ? O20 Eu3 O18 C29 146.6(7) 1_655 . . . ? O2 Eu3 O18 C29 -43.5(9) 2_756 . . . ? O23 Eu3 O18 C29 112.7(8) . . . . ? O17 Eu3 O18 C29 -98.6(8) . . . . ? O15 Eu3 O18 C29 -34.5(7) . . . . ? O7 Eu3 O18 Eu2 20.4(3) . . . . ? O21 Eu3 O18 Eu2 -130.6(3) 2_566 . . . ? O20 Eu3 O18 Eu2 -21.1(5) 1_655 . . . ? O2 Eu3 O18 Eu2 148.8(3) 2_756 . . . ? O23 Eu3 O18 Eu2 -55.0(3) . . . . ? O17 Eu3 O18 Eu2 93.6(3) . . . . ? O15 Eu3 O18 Eu2 157.8(3) . . . . ? O16 Eu2 O18 C29 101.7(5) 2_656 . . . ? O6 Eu2 O18 C29 -172.6(5) . . . . ? O14 Eu2 O18 C29 27.6(5) 2_557 . . . ? O11 Eu2 O18 C29 -90.7(5) . . . . ? O10 Eu2 O18 C29 157.3(5) . . . . ? O19 Eu2 O18 C29 0.8(5) . . . . ? O8 Eu2 O18 C29 -85.0(5) . . . . ? O16 Eu2 O18 Eu3 -86.4(3) 2_656 . . . ? O6 Eu2 O18 Eu3 -0.8(3) . . . . ? O14 Eu2 O18 Eu3 -160.5(3) 2_557 . . . ? O11 Eu2 O18 Eu3 81.2(3) . . . . ? O10 Eu2 O18 Eu3 -30.8(6) . . . . ? O19 Eu2 O18 Eu3 172.6(4) . . . . ? O8 Eu2 O18 Eu3 86.8(4) . . . . ? C29 Eu2 O18 Eu3 171.9(6) . . . . ? O18 C29 O19 Eu2 1.5(9) . . . . ? C22 C29 O19 Eu2 -176.9(6) . . . . ? O16 Eu2 O19 C29 -74.2(5) 2_656 . . . ? O6 Eu2 O19 C29 7.8(6) . . . . ? O14 Eu2 O19 C29 -159.5(5) 2_557 . . . ? O11 Eu2 O19 C29 73.3(5) . . . . ? O10 Eu2 O19 C29 -156.9(5) . . . . ? O18 Eu2 O19 C29 -0.8(5) . . . . ? O8 Eu2 O19 C29 128.3(5) . . . . ? O21 C30 O20 Eu3 54.1(12) . . . 1_455 ? C24 C30 O20 Eu3 -127.3(7) . . . 1_455 ? O20 C30 O21 Eu3 16.6(15) . . . 2_566 ? C24 C30 O21 Eu3 -162.1(6) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.278 _refine_diff_density_min -1.245 _refine_diff_density_rms 0.203 _database_code_depnum_ccdc_archive 'CCDC 946975' ####################################################################### # # 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_p100715a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 Gd3 O25' _chemical_formula_weight 1255.23 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1254(7) _cell_length_b 12.2074(9) _cell_length_c 14.8622(10) _cell_angle_alpha 68.646(7) _cell_angle_beta 84.590(6) _cell_angle_gamma 75.209(6) _cell_volume 1654.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1085 _cell_measurement_theta_min 2.5105 _cell_measurement_theta_max 28.7933 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1190 _exptl_absorpt_coefficient_mu 6.054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5303 _exptl_absorpt_correction_T_max 0.5827 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number 3908 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11496 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_unetI/netI 0.0360 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5831 _reflns_number_gt 5190 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^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 5831 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 1.24575(2) -0.518937(19) 0.899662(15) 0.01379(7) Uani 1 1 d . . . Gd2 Gd 0.35886(2) -0.022103(19) 0.785212(15) 0.01322(7) Uani 1 1 d . . . Gd3 Gd 0.49263(2) 0.288120(18) 0.543994(15) 0.01192(7) Uani 1 1 d . . . C1 C 1.0230(4) -0.2442(4) 0.7360(3) 0.0163(10) Uani 1 1 d . . . C2 C 0.9165(4) -0.2694(4) 0.8024(3) 0.0149(10) Uani 1 1 d . . . C3 C 0.8004(4) -0.1751(4) 0.7960(3) 0.0176(10) Uani 1 1 d . . . H3 H 0.7303 -0.1890 0.8407 0.021 Uiso 1 1 calc R . . C4 C 0.7876(4) -0.0627(4) 0.7253(3) 0.0139(9) Uani 1 1 d . . . C5 C 0.8940(4) -0.0393(4) 0.6609(3) 0.0205(11) Uani 1 1 d . . . H5 H 0.8858 0.0373 0.6138 0.025 Uiso 1 1 calc R . . C6 C 1.0122(5) -0.1285(4) 0.6657(3) 0.0202(10) Uani 1 1 d . . . H6 H 1.0836 -0.1118 0.6228 0.024 Uiso 1 1 calc R . . C7 C 1.2448(4) -0.2989(4) 0.6697(3) 0.0158(10) Uani 1 1 d . . . H7A H 1.2796 -0.2369 0.6793 0.019 Uiso 1 1 calc R . . H7B H 1.2051 -0.2662 0.6057 0.019 Uiso 1 1 calc R . . C8 C 1.3598(4) -0.4088(4) 0.6783(3) 0.0152(10) Uani 1 1 d . . . C9 C 0.9167(4) -0.3895(4) 0.8810(3) 0.0145(9) Uani 1 1 d . . . C10 C 0.6585(4) 0.0342(4) 0.7138(3) 0.0147(10) Uani 1 1 d . . . C11 C 0.1982(4) 0.0175(4) 1.0063(3) 0.0176(10) Uani 1 1 d . . . C12 C 0.1557(4) 0.1422(4) 0.9561(3) 0.0168(10) Uani 1 1 d . . . C13 C 0.0397(4) 0.2081(4) 0.9884(3) 0.0165(10) Uani 1 1 d . . . H13 H 0.0115 0.2912 0.9559 0.020 Uiso 1 1 calc R . . C14 C -0.0340(4) 0.1528(4) 1.0674(3) 0.0168(10) Uani 1 1 d . . . C15 C 0.0136(5) 0.0286(4) 1.1187(3) 0.0186(10) Uani 1 1 d . . . H15 H -0.0335 -0.0092 1.1733 0.022 Uiso 1 1 calc R . . C16 C 0.1300(4) -0.0387(4) 1.0892(3) 0.0196(10) Uani 1 1 d . . . H16 H 0.1621 -0.1206 1.1246 0.024 Uiso 1 1 calc R . . C17 C 0.3802(5) -0.1615(5) 1.0401(4) 0.0341(14) Uani 1 1 d . . . H17A H 0.3153 -0.2095 1.0728 0.041 Uiso 1 1 calc R . . H17B H 0.4231 -0.1455 1.0882 0.041 Uiso 1 1 calc R . . C18 C 0.4871(4) -0.2309(4) 0.9907(3) 0.0202(10) Uani 1 1 d . . . C19 C 0.2278(4) 0.2119(4) 0.8714(3) 0.0178(10) Uani 1 1 d . . . C20 C -0.1570(4) 0.2252(4) 1.1009(3) 0.0182(10) Uani 1 1 d . . . C21 C 0.1746(4) 0.3269(4) 0.4512(3) 0.0147(9) Uani 1 1 d . . . C22 C 0.1209(4) 0.2653(4) 0.5400(3) 0.0150(9) Uani 1 1 d . . . C23 C -0.0206(4) 0.2997(4) 0.5543(3) 0.0175(10) Uani 1 1 d . . . H23 H -0.0602 0.2568 0.6109 0.021 Uiso 1 1 calc R . . C24 C -0.1022(4) 0.3977(4) 0.4842(3) 0.0149(10) Uani 1 1 d . . . C25 C -0.0453(4) 0.4578(4) 0.3973(3) 0.0173(10) Uani 1 1 d . . . H25 H -0.0998 0.5232 0.3507 0.021 Uiso 1 1 calc R . . C26 C 0.0932(4) 0.4202(4) 0.3797(3) 0.0170(10) Uani 1 1 d . . . H26 H 0.1307 0.4576 0.3203 0.020 Uiso 1 1 calc R . . C27 C 0.3524(5) 0.2331(5) 0.3667(4) 0.0257(11) Uani 1 1 d . . . H27A H 0.3464 0.2916 0.3014 0.031 Uiso 1 1 calc R . . H27B H 0.2905 0.1820 0.3723 0.031 Uiso 1 1 calc R . . C28 C 0.4974(4) 0.1561(4) 0.3870(3) 0.0182(10) Uani 1 1 d . . . C29 C 0.2089(4) 0.1671(4) 0.6200(3) 0.0178(10) Uani 1 1 d . . . C30 C -0.2535(4) 0.4385(4) 0.5024(3) 0.0148(9) Uani 1 1 d . . . O1 O 1.1423(3) -0.3330(3) 0.7414(2) 0.0163(7) Uani 1 1 d . . . O2 O 1.4509(3) -0.4003(3) 0.6150(2) 0.0169(7) Uani 1 1 d . . . O3 O 1.3561(3) -0.5042(3) 0.7480(2) 0.0202(7) Uani 1 1 d . . . O4 O 1.0131(3) -0.4806(3) 0.8831(2) 0.0173(7) Uani 1 1 d . . . O5 O 0.8190(3) -0.3946(3) 0.9391(2) 0.0189(7) Uani 1 1 d . . . O6 O 0.5679(3) 0.0194(3) 0.7789(2) 0.0192(7) Uani 1 1 d . . . O7 O 0.6463(3) 0.1230(3) 0.6376(2) 0.0212(7) Uani 1 1 d . . . O8 O 0.3096(3) -0.0487(3) 0.9706(2) 0.0192(7) Uani 1 1 d . . . O9 O 0.5607(3) -0.3244(3) 1.0468(2) 0.0311(9) Uani 1 1 d . . . O10 O 0.4907(3) -0.1972(3) 0.9009(2) 0.0237(8) Uani 1 1 d . . . O11 O 0.3015(3) 0.1559(3) 0.8195(2) 0.0236(8) Uani 1 1 d . . . O12 O 0.2137(3) 0.3213(3) 0.8544(2) 0.0250(8) Uani 1 1 d . . . O13 O -0.1786(3) 0.3388(3) 1.0637(2) 0.0200(7) Uani 1 1 d . . . O14 O -0.2327(3) 0.1696(3) 1.1641(2) 0.0195(7) Uani 1 1 d . . . O15 O 0.3142(3) 0.2945(3) 0.4337(2) 0.0158(7) Uani 1 1 d . . . O16 O 0.5485(3) 0.1095(3) 0.3249(2) 0.0215(7) Uani 1 1 d . . . O17 O 0.5560(3) 0.1470(3) 0.4595(2) 0.0186(7) Uani 1 1 d . . . O18 O 0.3354(3) 0.1640(3) 0.6249(2) 0.0151(7) Uani 1 1 d . . . O19 O 0.1562(3) 0.0896(3) 0.6822(2) 0.0221(7) Uani 1 1 d . . . O20 O -0.3138(3) 0.3595(3) 0.5564(2) 0.0195(7) Uani 1 1 d . . . O21 O -0.3105(2) 0.5485(2) 0.46187(18) 0.0174(7) Uani 1 1 d . . . O22 O 1.4392(2) -0.4289(2) 0.88433(18) 0.0437(11) Uani 1 1 d R . . H22A H 1.4028 -0.3566 0.8833 0.052 Uiso 1 1 d R . . H22B H 1.5230 -0.4370 0.8675 0.052 Uiso 1 1 d R . . O23 O 0.4702(3) 0.2972(3) 0.7066(2) 0.0188(7) Uani 1 1 d . . . H23B H 0.4272 0.3649 0.7149 0.023 Uiso 1 1 d R . . H23A H 0.4268 0.2410 0.7341 0.023 Uiso 1 1 d R . . O24 O 0.7248(4) 0.3102(4) 0.7560(3) 0.0466(11) Uani 1 1 d . . . H24A H 0.6370 0.3191 0.7530 0.070 Uiso 1 1 d R . . H24B H 0.7627 0.3410 0.7006 0.070 Uiso 1 1 d R . . O25 O 0.6959(4) 0.4842(4) 0.8370(3) 0.0571(13) Uani 1 1 d . . . H25A H 0.7200 0.4270 0.8083 0.086 Uiso 1 1 d R . . H25B H 0.7560 0.4634 0.8839 0.086 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01374(12) 0.01144(12) 0.01259(12) -0.00263(9) 0.00142(9) 0.00030(9) Gd2 0.01310(12) 0.01109(11) 0.01323(12) -0.00315(9) 0.00201(9) -0.00149(9) Gd3 0.01028(11) 0.01142(11) 0.01150(12) -0.00223(9) 0.00113(9) -0.00127(8) C1 0.012(2) 0.015(2) 0.019(2) -0.005(2) 0.0006(19) 0.0006(18) C2 0.015(2) 0.014(2) 0.015(2) -0.0051(19) -0.0032(18) -0.0011(18) C3 0.016(2) 0.024(2) 0.013(2) -0.007(2) -0.0027(19) -0.0033(19) C4 0.014(2) 0.014(2) 0.012(2) -0.0029(19) -0.0004(18) -0.0034(18) C5 0.023(3) 0.013(2) 0.018(2) 0.002(2) -0.003(2) -0.0023(19) C6 0.016(2) 0.021(2) 0.022(3) -0.007(2) 0.005(2) -0.0025(19) C7 0.018(2) 0.014(2) 0.012(2) -0.0030(19) 0.0048(19) -0.0037(18) C8 0.019(2) 0.019(2) 0.012(2) -0.010(2) 0.0018(19) -0.0059(19) C9 0.010(2) 0.016(2) 0.017(2) -0.004(2) -0.0016(19) -0.0035(18) C10 0.015(2) 0.012(2) 0.017(2) -0.006(2) -0.005(2) -0.0021(18) C11 0.014(2) 0.019(2) 0.021(2) -0.009(2) -0.0015(19) -0.0018(19) C12 0.014(2) 0.022(2) 0.016(2) -0.009(2) 0.0029(19) -0.0049(19) C13 0.019(2) 0.014(2) 0.017(2) -0.006(2) 0.0003(19) -0.0040(18) C14 0.020(2) 0.017(2) 0.015(2) -0.006(2) -0.0008(19) -0.0050(19) C15 0.022(2) 0.020(2) 0.013(2) -0.003(2) 0.0023(19) -0.008(2) C16 0.017(2) 0.017(2) 0.021(2) -0.004(2) 0.000(2) -0.0020(19) C17 0.039(3) 0.029(3) 0.019(3) -0.004(2) -0.007(2) 0.015(2) C18 0.015(2) 0.016(2) 0.024(3) -0.003(2) -0.003(2) 0.0003(19) C19 0.016(2) 0.017(2) 0.020(2) -0.008(2) 0.0019(19) -0.0022(19) C20 0.020(2) 0.018(2) 0.018(2) -0.009(2) 0.001(2) -0.004(2) C21 0.009(2) 0.017(2) 0.022(2) -0.011(2) -0.0006(19) -0.0024(18) C22 0.012(2) 0.014(2) 0.019(2) -0.005(2) 0.0004(19) -0.0030(17) C23 0.018(2) 0.015(2) 0.016(2) -0.004(2) 0.0010(19) -0.0025(19) C24 0.012(2) 0.015(2) 0.019(2) -0.007(2) -0.0005(19) -0.0038(18) C25 0.015(2) 0.016(2) 0.019(2) -0.006(2) -0.0068(19) 0.0009(18) C26 0.021(2) 0.018(2) 0.014(2) -0.005(2) 0.0031(19) -0.0092(19) C27 0.020(3) 0.037(3) 0.027(3) -0.020(2) 0.001(2) -0.004(2) C28 0.020(2) 0.017(2) 0.019(2) -0.008(2) 0.007(2) -0.0098(19) C29 0.014(2) 0.018(2) 0.024(3) -0.010(2) 0.001(2) -0.0027(19) C30 0.012(2) 0.019(2) 0.015(2) -0.008(2) -0.0002(18) -0.0035(19) O1 0.0116(15) 0.0143(15) 0.0177(16) -0.0031(14) 0.0044(13) 0.0005(12) O2 0.0139(16) 0.0180(16) 0.0133(16) -0.0012(14) 0.0041(13) -0.0023(13) O3 0.0242(18) 0.0123(16) 0.0171(17) -0.0009(14) 0.0072(14) -0.0014(13) O4 0.0167(16) 0.0121(15) 0.0173(16) -0.0016(13) -0.0003(13) 0.0014(13) O5 0.0162(16) 0.0210(17) 0.0140(16) -0.0018(14) 0.0014(14) -0.0019(13) O6 0.0130(16) 0.0164(16) 0.0259(18) -0.0068(15) -0.0006(14) -0.0004(13) O7 0.0214(17) 0.0181(17) 0.0178(17) -0.0029(15) -0.0009(14) 0.0016(14) O8 0.0207(17) 0.0141(16) 0.0146(16) -0.0013(14) 0.0019(13) 0.0037(13) O9 0.0272(19) 0.028(2) 0.0205(18) -0.0005(16) 0.0002(15) 0.0122(16) O10 0.0242(18) 0.0217(18) 0.0155(17) -0.0017(15) 0.0035(14) 0.0024(14) O11 0.0304(19) 0.0164(16) 0.0214(17) -0.0069(15) 0.0109(15) -0.0043(14) O12 0.0294(19) 0.0179(17) 0.0296(19) -0.0121(16) 0.0136(15) -0.0085(14) O13 0.0194(17) 0.0150(16) 0.0233(18) -0.0060(15) 0.0020(14) -0.0021(13) O14 0.0204(17) 0.0180(16) 0.0219(17) -0.0083(15) 0.0099(14) -0.0094(14) O15 0.0102(15) 0.0226(16) 0.0163(16) -0.0098(14) 0.0052(13) -0.0040(13) O16 0.0227(17) 0.0235(18) 0.0234(18) -0.0152(16) 0.0052(14) -0.0058(14) O17 0.0176(16) 0.0190(17) 0.0189(17) -0.0090(14) 0.0014(14) -0.0008(13) O18 0.0122(16) 0.0151(15) 0.0135(15) -0.0009(13) -0.0024(13) -0.0009(12) O19 0.0140(16) 0.0224(17) 0.0217(17) 0.0033(15) 0.0017(14) -0.0074(14) O20 0.0156(16) 0.0209(17) 0.0182(17) -0.0017(15) 0.0002(13) -0.0058(13) O21 0.0150(16) 0.0169(16) 0.0198(17) -0.0078(14) -0.0040(13) 0.0006(13) O22 0.023(2) 0.041(2) 0.082(3) -0.043(2) 0.010(2) -0.0066(17) O23 0.0217(17) 0.0154(16) 0.0169(16) -0.0051(14) 0.0039(14) -0.0029(13) O24 0.044(2) 0.056(3) 0.035(2) -0.009(2) 0.0015(19) -0.015(2) O25 0.041(2) 0.072(3) 0.071(3) -0.041(3) 0.003(2) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O4 2.301(3) . ? Gd1 O9 2.324(3) 2_747 ? Gd1 O5 2.346(3) 2_747 ? Gd1 O13 2.374(3) 2_657 ? Gd1 O12 2.383(3) 1_645 ? Gd1 O3 2.386(3) . ? Gd1 O22 2.434(2) . ? Gd1 O1 2.673(3) . ? Gd2 O16 2.274(3) 2_656 ? Gd2 O6 2.285(3) . ? Gd2 O11 2.329(3) . ? Gd2 O14 2.334(3) 2_557 ? Gd2 O10 2.368(3) . ? Gd2 O19 2.461(3) . ? Gd2 O18 2.605(3) . ? Gd2 O8 2.667(3) . ? Gd2 C29 2.907(4) . ? Gd3 O7 2.277(3) . ? Gd3 O21 2.326(2) 2_566 ? Gd3 O2 2.361(3) 2_756 ? Gd3 O20 2.385(3) 1_655 ? Gd3 O17 2.411(3) . ? Gd3 O18 2.412(3) . ? Gd3 O23 2.446(3) . ? Gd3 O15 2.520(3) . ? C1 O1 1.388(5) . ? C1 C6 1.403(6) . ? C1 C2 1.407(6) . ? C2 C3 1.402(6) . ? C2 C9 1.506(6) . ? C3 C4 1.373(6) . ? C3 H3 0.9300 . ? C4 C5 1.387(6) . ? C4 C10 1.497(6) . ? C5 C6 1.385(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.440(5) . ? C7 C8 1.509(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.250(5) . ? C8 O3 1.252(5) . ? C9 O5 1.248(5) . ? C9 O4 1.271(5) . ? C10 O7 1.240(5) . ? C10 O6 1.264(5) . ? C11 C16 1.390(6) . ? C11 O8 1.393(5) . ? C11 C12 1.399(6) . ? C12 C13 1.396(6) . ? C12 C19 1.484(6) . ? C13 C14 1.381(6) . ? C13 H13 0.9300 . ? C14 C15 1.403(6) . ? C14 C20 1.490(6) . ? C15 C16 1.388(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O8 1.441(5) . ? C17 C18 1.505(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O9 1.243(5) . ? C18 O10 1.244(5) . ? C19 O12 1.239(5) . ? C19 O11 1.279(5) . ? C20 O13 1.259(5) . ? C20 O14 1.264(5) . ? C21 C26 1.382(6) . ? C21 O15 1.394(5) . ? C21 C22 1.398(6) . ? C22 C23 1.406(6) . ? C22 C29 1.504(6) . ? C23 C24 1.396(6) . ? C23 H23 0.9300 . ? C24 C25 1.388(6) . ? C24 C30 1.516(6) . ? C25 C26 1.391(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 O15 1.424(5) . ? C27 C28 1.517(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O17 1.236(5) . ? C28 O16 1.258(5) . ? C29 O19 1.250(5) . ? C29 O18 1.280(5) . ? C30 O21 1.257(5) . ? C30 O20 1.262(5) . ? O2 Gd3 2.361(3) 2_756 ? O5 Gd1 2.346(3) 2_747 ? O9 Gd1 2.324(3) 2_747 ? O12 Gd1 2.383(3) 1_465 ? O13 Gd1 2.374(3) 2_657 ? O14 Gd2 2.334(3) 2_557 ? O16 Gd2 2.274(3) 2_656 ? O20 Gd3 2.385(3) 1_455 ? O21 Gd3 2.326(2) 2_566 ? O22 H22A 0.8603 . ? O22 H22B 0.8533 . ? O23 H23B 0.8769 . ? O23 H23A 0.8650 . ? O24 H24A 0.8711 . ? O24 H24B 0.8694 . ? O25 H25A 0.9153 . ? O25 H25B 0.8910 . ? 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 Gd1 O9 142.45(12) . 2_747 ? O4 Gd1 O5 79.29(10) . 2_747 ? O9 Gd1 O5 81.02(11) 2_747 2_747 ? O4 Gd1 O13 80.67(11) . 2_657 ? O9 Gd1 O13 127.58(12) 2_747 2_657 ? O5 Gd1 O13 82.08(11) 2_747 2_657 ? O4 Gd1 O12 75.56(11) . 1_645 ? O9 Gd1 O12 74.34(13) 2_747 1_645 ? O5 Gd1 O12 94.12(11) 2_747 1_645 ? O13 Gd1 O12 156.22(11) 2_657 1_645 ? O4 Gd1 O3 110.18(11) . . ? O9 Gd1 O3 80.81(11) 2_747 . ? O5 Gd1 O3 159.44(10) 2_747 . ? O13 Gd1 O3 116.89(11) 2_657 . ? O12 Gd1 O3 71.71(11) 1_645 . ? O4 Gd1 O22 145.25(9) . . ? O9 Gd1 O22 72.19(11) 2_747 . ? O5 Gd1 O22 112.65(10) 2_747 . ? O13 Gd1 O22 69.54(9) 2_657 . ? O12 Gd1 O22 132.44(9) 1_645 . ? O3 Gd1 O22 70.42(10) . . ? O4 Gd1 O1 65.37(10) . . ? O9 Gd1 O1 141.10(10) 2_747 . ? O5 Gd1 O1 137.88(9) 2_747 . ? O13 Gd1 O1 70.64(10) 2_657 . ? O12 Gd1 O1 98.28(10) 1_645 . ? O3 Gd1 O1 60.94(9) . . ? O22 Gd1 O1 87.55(9) . . ? O16 Gd2 O6 83.99(11) 2_656 . ? O16 Gd2 O11 145.74(11) 2_656 . ? O6 Gd2 O11 78.64(11) . . ? O16 Gd2 O14 85.13(11) 2_656 2_557 ? O6 Gd2 O14 146.82(10) . 2_557 ? O11 Gd2 O14 124.37(11) . 2_557 ? O16 Gd2 O10 85.81(11) 2_656 . ? O6 Gd2 O10 75.88(11) . . ? O11 Gd2 O10 117.57(12) . . ? O14 Gd2 O10 72.13(11) 2_557 . ? O16 Gd2 O19 90.24(11) 2_656 . ? O6 Gd2 O19 130.50(11) . . ? O11 Gd2 O19 79.33(11) . . ? O14 Gd2 O19 80.71(11) 2_557 . ? O10 Gd2 O19 152.79(12) . . ? O16 Gd2 O18 77.71(10) 2_656 . ? O6 Gd2 O18 79.55(10) . . ? O11 Gd2 O18 70.27(10) . . ? O14 Gd2 O18 128.19(10) 2_557 . ? O10 Gd2 O18 151.65(10) . . ? O19 Gd2 O18 51.31(10) . . ? O16 Gd2 O8 147.76(10) 2_656 . ? O6 Gd2 O8 96.09(11) . . ? O11 Gd2 O8 64.20(10) . . ? O14 Gd2 O8 77.29(10) 2_557 . ? O10 Gd2 O8 63.22(10) . . ? O19 Gd2 O8 112.89(10) . . ? O18 Gd2 O8 134.17(9) . . ? O16 Gd2 C29 83.97(12) 2_656 . ? O6 Gd2 C29 105.44(12) . . ? O11 Gd2 C29 72.71(12) . . ? O14 Gd2 C29 104.45(12) 2_557 . ? O10 Gd2 C29 169.49(12) . . ? O19 Gd2 C29 25.21(11) . . ? O18 Gd2 C29 26.12(11) . . ? O8 Gd2 C29 126.36(10) . . ? O7 Gd3 O21 147.15(10) . 2_566 ? O7 Gd3 O2 120.80(10) . 2_756 ? O21 Gd3 O2 88.16(9) 2_566 2_756 ? O7 Gd3 O20 74.23(11) . 1_655 ? O21 Gd3 O20 102.99(9) 2_566 1_655 ? O2 Gd3 O20 73.44(10) 2_756 1_655 ? O7 Gd3 O17 72.41(11) . . ? O21 Gd3 O17 135.71(9) 2_566 . ? O2 Gd3 O17 73.76(10) 2_756 . ? O20 Gd3 O17 109.60(10) 1_655 . ? O7 Gd3 O18 81.79(10) . . ? O21 Gd3 O18 85.52(9) 2_566 . ? O2 Gd3 O18 138.72(10) 2_756 . ? O20 Gd3 O18 147.55(10) 1_655 . ? O17 Gd3 O18 82.78(10) . . ? O7 Gd3 O23 73.81(10) . . ? O21 Gd3 O23 73.73(9) 2_566 . ? O2 Gd3 O23 140.57(11) 2_756 . ? O20 Gd3 O23 76.92(10) 1_655 . ? O17 Gd3 O23 141.98(10) . . ? O18 Gd3 O23 75.61(10) . . ? O7 Gd3 O15 127.86(11) . . ? O21 Gd3 O15 72.32(9) 2_566 . ? O2 Gd3 O15 72.83(10) 2_756 . ? O20 Gd3 O15 146.07(10) 1_655 . ? O17 Gd3 O15 63.84(9) . . ? O18 Gd3 O15 66.38(10) . . ? O23 Gd3 O15 130.13(10) . . ? O1 C1 C6 119.2(4) . . ? O1 C1 C2 120.2(4) . . ? C6 C1 C2 120.6(4) . . ? C3 C2 C1 117.8(4) . . ? C3 C2 C9 116.7(4) . . ? C1 C2 C9 125.4(4) . . ? C4 C3 C2 121.7(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 C10 121.3(4) . . ? C5 C4 C10 118.9(4) . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 119.3(4) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? O1 C7 C8 109.3(3) . . ? O1 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O1 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? O2 C8 O3 123.9(4) . . ? O2 C8 C7 118.6(4) . . ? O3 C8 C7 117.4(4) . . ? O5 C9 O4 123.6(4) . . ? O5 C9 C2 117.6(4) . . ? O4 C9 C2 118.7(4) . . ? O7 C10 O6 124.3(4) . . ? O7 C10 C4 116.4(4) . . ? O6 C10 C4 119.3(4) . . ? C16 C11 O8 121.1(4) . . ? C16 C11 C12 120.7(4) . . ? O8 C11 C12 118.3(4) . . ? C13 C12 C11 118.7(4) . . ? C13 C12 C19 116.6(4) . . ? C11 C12 C19 124.7(4) . . ? C14 C13 C12 121.5(4) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 118.7(4) . . ? C13 C14 C20 120.5(4) . . ? C15 C14 C20 120.6(4) . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C11 119.4(4) . . ? C15 C16 H16 120.3 . . ? C11 C16 H16 120.3 . . ? O8 C17 C18 110.3(4) . . ? O8 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? O8 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? O9 C18 O10 125.5(4) . . ? O9 C18 C17 114.2(4) . . ? O10 C18 C17 120.1(4) . . ? O12 C19 O11 123.1(4) . . ? O12 C19 C12 118.5(4) . . ? O11 C19 C12 118.4(4) . . ? O13 C20 O14 124.2(4) . . ? O13 C20 C14 117.3(4) . . ? O14 C20 C14 118.5(4) . . ? C26 C21 O15 118.6(4) . . ? C26 C21 C22 121.9(4) . . ? O15 C21 C22 119.5(4) . . ? C21 C22 C23 117.7(4) . . ? C21 C22 C29 122.5(4) . . ? C23 C22 C29 119.7(4) . . ? C24 C23 C22 120.5(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.1(4) . . ? C25 C24 C30 119.6(4) . . ? C23 C24 C30 120.3(4) . . ? C24 C25 C26 120.0(4) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 119.6(4) . . ? C21 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? O15 C27 C28 109.7(4) . . ? O15 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? O15 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? O17 C28 O16 125.8(4) . . ? O17 C28 C27 118.7(4) . . ? O16 C28 C27 115.4(4) . . ? O19 C29 O18 120.7(4) . . ? O19 C29 C22 119.0(4) . . ? O18 C29 C22 120.4(4) . . ? O19 C29 Gd2 57.0(2) . . ? O18 C29 Gd2 63.7(2) . . ? C22 C29 Gd2 175.1(3) . . ? O21 C30 O20 124.5(4) . . ? O21 C30 C24 117.7(4) . . ? O20 C30 C24 117.7(4) . . ? C1 O1 C7 116.0(3) . . ? C1 O1 Gd1 126.5(2) . . ? C7 O1 Gd1 112.8(2) . . ? C8 O2 Gd3 145.0(3) . 2_756 ? C8 O3 Gd1 126.6(3) . . ? C9 O4 Gd1 132.3(3) . . ? C9 O5 Gd1 144.9(3) . 2_747 ? C10 O6 Gd2 132.6(3) . . ? C10 O7 Gd3 143.2(3) . . ? C11 O8 C17 115.4(3) . . ? C11 O8 Gd2 126.0(2) . . ? C17 O8 Gd2 116.0(2) . . ? C18 O9 Gd1 157.6(3) . 2_747 ? C18 O10 Gd2 129.4(3) . . ? C19 O11 Gd2 145.5(3) . . ? C19 O12 Gd1 150.2(3) . 1_465 ? C20 O13 Gd1 143.1(3) . 2_657 ? C20 O14 Gd2 148.4(3) . 2_557 ? C21 O15 C27 115.8(3) . . ? C21 O15 Gd3 122.6(2) . . ? C27 O15 Gd3 119.4(2) . . ? C28 O16 Gd2 179.0(3) . 2_656 ? C28 O17 Gd3 124.6(3) . . ? C29 O18 Gd3 138.1(3) . . ? C29 O18 Gd2 90.2(3) . . ? Gd3 O18 Gd2 130.97(11) . . ? C29 O19 Gd2 97.8(3) . . ? C30 O20 Gd3 136.4(3) . 1_455 ? C30 O21 Gd3 148.7(3) . 2_566 ? Gd1 O22 H22A 104.3 . . ? Gd1 O22 H22B 142.3 . . ? H22A O22 H22B 111.4 . . ? Gd3 O23 H23B 119.7 . . ? Gd3 O23 H23A 99.3 . . ? H23B O23 H23A 111.0 . . ? H24A O24 H24B 114.1 . . ? H25A O25 H25B 107.3 . . ? 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 O1 C1 C2 C3 177.6(4) . . . . ? C6 C1 C2 C3 -0.3(7) . . . . ? O1 C1 C2 C9 -1.8(7) . . . . ? C6 C1 C2 C9 -179.7(4) . . . . ? C1 C2 C3 C4 2.4(7) . . . . ? C9 C2 C3 C4 -178.1(4) . . . . ? C2 C3 C4 C5 -2.9(7) . . . . ? C2 C3 C4 C10 174.7(4) . . . . ? C3 C4 C5 C6 1.2(7) . . . . ? C10 C4 C5 C6 -176.5(4) . . . . ? C4 C5 C6 C1 0.9(7) . . . . ? O1 C1 C6 C5 -179.2(4) . . . . ? C2 C1 C6 C5 -1.3(7) . . . . ? O1 C7 C8 O2 171.8(4) . . . . ? O1 C7 C8 O3 -6.6(6) . . . . ? C3 C2 C9 O5 -5.1(6) . . . . ? C1 C2 C9 O5 174.3(4) . . . . ? C3 C2 C9 O4 172.7(4) . . . . ? C1 C2 C9 O4 -7.9(7) . . . . ? C3 C4 C10 O7 -166.2(4) . . . . ? C5 C4 C10 O7 11.5(6) . . . . ? C3 C4 C10 O6 11.1(7) . . . . ? C5 C4 C10 O6 -171.2(4) . . . . ? C16 C11 C12 C13 -2.8(7) . . . . ? O8 C11 C12 C13 176.6(4) . . . . ? C16 C11 C12 C19 175.2(4) . . . . ? O8 C11 C12 C19 -5.4(7) . . . . ? C11 C12 C13 C14 -0.9(7) . . . . ? C19 C12 C13 C14 -179.0(4) . . . . ? C12 C13 C14 C15 3.2(7) . . . . ? C12 C13 C14 C20 179.7(4) . . . . ? C13 C14 C15 C16 -2.0(7) . . . . ? C20 C14 C15 C16 -178.4(4) . . . . ? C14 C15 C16 C11 -1.6(7) . . . . ? O8 C11 C16 C15 -175.4(4) . . . . ? C12 C11 C16 C15 4.0(7) . . . . ? O8 C17 C18 O9 174.0(4) . . . . ? O8 C17 C18 O10 -10.3(7) . . . . ? C13 C12 C19 O12 23.8(6) . . . . ? C11 C12 C19 O12 -154.3(5) . . . . ? C13 C12 C19 O11 -156.2(4) . . . . ? C11 C12 C19 O11 25.8(7) . . . . ? C13 C14 C20 O13 -10.1(7) . . . . ? C15 C14 C20 O13 166.3(4) . . . . ? C13 C14 C20 O14 169.9(4) . . . . ? C15 C14 C20 O14 -13.7(7) . . . . ? C26 C21 C22 C23 1.2(7) . . . . ? O15 C21 C22 C23 -179.2(4) . . . . ? C26 C21 C22 C29 -177.5(4) . . . . ? O15 C21 C22 C29 2.2(7) . . . . ? C21 C22 C23 C24 -4.3(7) . . . . ? C29 C22 C23 C24 174.4(4) . . . . ? C22 C23 C24 C25 3.7(7) . . . . ? C22 C23 C24 C30 -176.7(4) . . . . ? C23 C24 C25 C26 0.2(7) . . . . ? C30 C24 C25 C26 -179.5(4) . . . . ? O15 C21 C26 C25 -177.1(4) . . . . ? C22 C21 C26 C25 2.6(7) . . . . ? C24 C25 C26 C21 -3.3(7) . . . . ? O15 C27 C28 O17 6.6(6) . . . . ? O15 C27 C28 O16 -171.4(4) . . . . ? C21 C22 C29 O19 -156.2(4) . . . . ? C23 C22 C29 O19 25.2(7) . . . . ? C21 C22 C29 O18 24.8(7) . . . . ? C23 C22 C29 O18 -153.9(4) . . . . ? C21 C22 C29 Gd2 170(4) . . . . ? C23 C22 C29 Gd2 -9(4) . . . . ? O16 Gd2 C29 O19 103.5(3) 2_656 . . . ? O6 Gd2 C29 O19 -174.4(3) . . . . ? O11 Gd2 C29 O19 -101.9(3) . . . . ? O14 Gd2 C29 O19 20.2(3) 2_557 . . . ? O10 Gd2 C29 O19 89.8(7) . . . . ? O18 Gd2 C29 O19 177.8(4) . . . . ? O8 Gd2 C29 O19 -64.5(3) . . . . ? O16 Gd2 C29 O18 -74.3(2) 2_656 . . . ? O6 Gd2 C29 O18 7.8(3) . . . . ? O11 Gd2 C29 O18 80.3(2) . . . . ? O14 Gd2 C29 O18 -157.7(2) 2_557 . . . ? O10 Gd2 C29 O18 -88.0(7) . . . . ? O19 Gd2 C29 O18 -177.8(4) . . . . ? O8 Gd2 C29 O18 117.6(2) . . . . ? O16 Gd2 C29 C22 139(4) 2_656 . . . ? O6 Gd2 C29 C22 -139(4) . . . . ? O11 Gd2 C29 C22 -66(4) . . . . ? O14 Gd2 C29 C22 56(4) 2_557 . . . ? O10 Gd2 C29 C22 125(4) . . . . ? O19 Gd2 C29 C22 36(4) . . . . ? O18 Gd2 C29 C22 -147(4) . . . . ? O8 Gd2 C29 C22 -29(4) . . . . ? C25 C24 C30 O21 -29.6(6) . . . . ? C23 C24 C30 O21 150.8(4) . . . . ? C25 C24 C30 O20 149.8(4) . . . . ? C23 C24 C30 O20 -29.8(6) . . . . ? C6 C1 O1 C7 -2.6(6) . . . . ? C2 C1 O1 C7 179.4(4) . . . . ? C6 C1 O1 Gd1 151.1(3) . . . . ? C2 C1 O1 Gd1 -26.8(6) . . . . ? C8 C7 O1 C1 -173.5(4) . . . . ? C8 C7 O1 Gd1 29.2(4) . . . . ? O4 Gd1 O1 C1 42.5(3) . . . . ? O9 Gd1 O1 C1 -172.3(3) 2_747 . . . ? O5 Gd1 O1 C1 6.8(4) 2_747 . . . ? O13 Gd1 O1 C1 -45.9(3) 2_657 . . . ? O12 Gd1 O1 C1 112.4(3) 1_645 . . . ? O3 Gd1 O1 C1 176.1(4) . . . . ? O22 Gd1 O1 C1 -115.0(3) . . . . ? O4 Gd1 O1 C7 -163.0(3) . . . . ? O9 Gd1 O1 C7 -17.8(4) 2_747 . . . ? O5 Gd1 O1 C7 161.3(3) 2_747 . . . ? O13 Gd1 O1 C7 108.6(3) 2_657 . . . ? O12 Gd1 O1 C7 -93.1(3) 1_645 . . . ? O3 Gd1 O1 C7 -29.5(3) . . . . ? O22 Gd1 O1 C7 39.4(3) . . . . ? O3 C8 O2 Gd3 158.9(3) . . . 2_756 ? C7 C8 O2 Gd3 -19.4(7) . . . 2_756 ? O2 C8 O3 Gd1 155.6(3) . . . . ? C7 C8 O3 Gd1 -26.1(6) . . . . ? O4 Gd1 O3 C8 75.2(4) . . . . ? O9 Gd1 O3 C8 -142.1(4) 2_747 . . . ? O5 Gd1 O3 C8 -170.2(3) 2_747 . . . ? O13 Gd1 O3 C8 -14.4(4) 2_657 . . . ? O12 Gd1 O3 C8 141.5(4) 1_645 . . . ? O22 Gd1 O3 C8 -67.8(4) . . . . ? O1 Gd1 O3 C8 30.6(3) . . . . ? O5 C9 O4 Gd1 -121.4(4) . . . . ? C2 C9 O4 Gd1 60.9(5) . . . . ? O9 Gd1 O4 C9 153.2(3) 2_747 . . . ? O5 Gd1 O4 C9 93.7(4) 2_747 . . . ? O13 Gd1 O4 C9 10.0(4) 2_657 . . . ? O12 Gd1 O4 C9 -169.2(4) 1_645 . . . ? O3 Gd1 O4 C9 -105.3(4) . . . . ? O22 Gd1 O4 C9 -20.8(5) . . . . ? O1 Gd1 O4 C9 -62.8(4) . . . . ? O4 C9 O5 Gd1 38.5(8) . . . 2_747 ? C2 C9 O5 Gd1 -143.8(4) . . . 2_747 ? O7 C10 O6 Gd2 70.1(6) . . . . ? C4 C10 O6 Gd2 -107.0(4) . . . . ? O16 Gd2 O6 C10 26.7(4) 2_656 . . . ? O11 Gd2 O6 C10 -123.6(4) . . . . ? O14 Gd2 O6 C10 98.2(4) 2_557 . . . ? O10 Gd2 O6 C10 113.9(4) . . . . ? O19 Gd2 O6 C10 -58.5(4) . . . . ? O18 Gd2 O6 C10 -51.9(4) . . . . ? O8 Gd2 O6 C10 174.3(4) . . . . ? C29 Gd2 O6 C10 -55.4(4) . . . . ? O6 C10 O7 Gd3 -11.4(8) . . . . ? C4 C10 O7 Gd3 165.7(3) . . . . ? O21 Gd3 O7 C10 43.0(6) 2_566 . . . ? O2 Gd3 O7 C10 -168.3(5) 2_756 . . . ? O20 Gd3 O7 C10 132.6(5) 1_655 . . . ? O17 Gd3 O7 C10 -110.3(5) . . . . ? O18 Gd3 O7 C10 -25.3(5) . . . . ? O23 Gd3 O7 C10 52.0(5) . . . . ? O15 Gd3 O7 C10 -76.7(5) . . . . ? C16 C11 O8 C17 -23.1(6) . . . . ? C12 C11 O8 C17 157.5(4) . . . . ? C16 C11 O8 Gd2 138.0(4) . . . . ? C12 C11 O8 Gd2 -41.4(5) . . . . ? C18 C17 O8 C11 173.3(4) . . . . ? C18 C17 O8 Gd2 10.3(6) . . . . ? O16 Gd2 O8 C11 -149.7(3) 2_656 . . . ? O6 Gd2 O8 C11 121.9(3) . . . . ? O11 Gd2 O8 C11 47.7(3) . . . . ? O14 Gd2 O8 C11 -91.1(3) 2_557 . . . ? O10 Gd2 O8 C11 -167.3(4) . . . . ? O19 Gd2 O8 C11 -17.0(4) . . . . ? O18 Gd2 O8 C11 40.6(4) . . . . ? C29 Gd2 O8 C11 7.6(4) . . . . ? O16 Gd2 O8 C17 11.3(4) 2_656 . . . ? O6 Gd2 O8 C17 -77.1(3) . . . . ? O11 Gd2 O8 C17 -151.4(4) . . . . ? O14 Gd2 O8 C17 69.9(3) 2_557 . . . ? O10 Gd2 O8 C17 -6.3(3) . . . . ? O19 Gd2 O8 C17 143.9(3) . . . . ? O18 Gd2 O8 C17 -158.4(3) . . . . ? C29 Gd2 O8 C17 168.6(3) . . . . ? O10 C18 O9 Gd1 30.6(13) . . . 2_747 ? C17 C18 O9 Gd1 -153.9(8) . . . 2_747 ? O9 C18 O10 Gd2 -179.6(4) . . . . ? C17 C18 O10 Gd2 5.2(7) . . . . ? O16 Gd2 O10 C18 -170.1(4) 2_656 . . . ? O6 Gd2 O10 C18 105.1(4) . . . . ? O11 Gd2 O10 C18 36.2(5) . . . . ? O14 Gd2 O10 C18 -83.9(4) 2_557 . . . ? O19 Gd2 O10 C18 -87.8(5) . . . . ? O18 Gd2 O10 C18 135.7(4) . . . . ? O8 Gd2 O10 C18 0.6(4) . . . . ? C29 Gd2 O10 C18 -156.4(6) . . . . ? O12 C19 O11 Gd2 -167.9(3) . . . . ? C12 C19 O11 Gd2 12.1(8) . . . . ? O16 Gd2 O11 C19 159.7(5) 2_656 . . . ? O6 Gd2 O11 C19 -139.3(5) . . . . ? O14 Gd2 O11 C19 14.5(6) 2_557 . . . ? O10 Gd2 O11 C19 -72.0(5) . . . . ? O19 Gd2 O11 C19 85.3(5) . . . . ? O18 Gd2 O11 C19 137.9(5) . . . . ? O8 Gd2 O11 C19 -36.7(5) . . . . ? C29 Gd2 O11 C19 110.4(5) . . . . ? O11 C19 O12 Gd1 -115.3(6) . . . 1_465 ? C12 C19 O12 Gd1 64.7(8) . . . 1_465 ? O14 C20 O13 Gd1 42.7(8) . . . 2_657 ? C14 C20 O13 Gd1 -137.4(4) . . . 2_657 ? O13 C20 O14 Gd2 128.1(5) . . . 2_557 ? C14 C20 O14 Gd2 -51.9(7) . . . 2_557 ? C26 C21 O15 C27 -71.9(5) . . . . ? C22 C21 O15 C27 108.4(5) . . . . ? C26 C21 O15 Gd3 125.0(4) . . . . ? C22 C21 O15 Gd3 -54.6(5) . . . . ? C28 C27 O15 C21 -154.8(4) . . . . ? C28 C27 O15 Gd3 8.9(5) . . . . ? O7 Gd3 O15 C21 113.4(3) . . . . ? O21 Gd3 O15 C21 -36.9(3) 2_566 . . . ? O2 Gd3 O15 C21 -130.5(3) 2_756 . . . ? O20 Gd3 O15 C21 -124.0(3) 1_655 . . . ? O17 Gd3 O15 C21 149.5(3) . . . . ? O18 Gd3 O15 C21 55.9(3) . . . . ? O23 Gd3 O15 C21 12.3(3) . . . . ? O7 Gd3 O15 C27 -49.1(3) . . . . ? O21 Gd3 O15 C27 160.6(3) 2_566 . . . ? O2 Gd3 O15 C27 67.0(3) 2_756 . . . ? O20 Gd3 O15 C27 73.5(4) 1_655 . . . ? O17 Gd3 O15 C27 -13.0(3) . . . . ? O18 Gd3 O15 C27 -106.6(3) . . . . ? O23 Gd3 O15 C27 -150.2(3) . . . . ? O17 C28 O16 Gd2 66(19) . . . 2_656 ? C27 C28 O16 Gd2 -116(18) . . . 2_656 ? O16 C28 O17 Gd3 156.9(3) . . . . ? C27 C28 O17 Gd3 -21.0(6) . . . . ? O7 Gd3 O17 C28 169.2(4) . . . . ? O21 Gd3 O17 C28 9.6(4) 2_566 . . . ? O2 Gd3 O17 C28 -60.2(3) 2_756 . . . ? O20 Gd3 O17 C28 -125.4(3) 1_655 . . . ? O18 Gd3 O17 C28 85.5(3) . . . . ? O23 Gd3 O17 C28 140.9(3) . . . . ? O15 Gd3 O17 C28 18.3(3) . . . . ? O19 C29 O18 Gd3 -172.6(3) . . . . ? C22 C29 O18 Gd3 6.4(7) . . . . ? Gd2 C29 O18 Gd3 -170.5(4) . . . . ? O19 C29 O18 Gd2 -2.1(4) . . . . ? C22 C29 O18 Gd2 176.9(4) . . . . ? O7 Gd3 O18 C29 -172.7(4) . . . . ? O21 Gd3 O18 C29 37.7(4) 2_566 . . . ? O2 Gd3 O18 C29 -44.4(5) 2_756 . . . ? O20 Gd3 O18 C29 144.9(4) 1_655 . . . ? O17 Gd3 O18 C29 -99.5(4) . . . . ? O23 Gd3 O18 C29 112.0(4) . . . . ? O15 Gd3 O18 C29 -35.0(4) . . . . ? O7 Gd3 O18 Gd2 19.99(16) . . . . ? O21 Gd3 O18 Gd2 -129.64(16) 2_566 . . . ? O2 Gd3 O18 Gd2 148.30(14) 2_756 . . . ? O20 Gd3 O18 Gd2 -22.4(3) 1_655 . . . ? O17 Gd3 O18 Gd2 93.17(16) . . . . ? O23 Gd3 O18 Gd2 -55.30(15) . . . . ? O15 Gd3 O18 Gd2 157.72(19) . . . . ? O16 Gd2 O18 C29 101.6(3) 2_656 . . . ? O6 Gd2 O18 C29 -172.4(3) . . . . ? O11 Gd2 O18 C29 -90.8(3) . . . . ? O14 Gd2 O18 C29 27.9(3) 2_557 . . . ? O10 Gd2 O18 C29 157.4(3) . . . . ? O19 Gd2 O18 C29 1.2(2) . . . . ? O8 Gd2 O18 C29 -84.0(3) . . . . ? O16 Gd2 O18 Gd3 -86.88(17) 2_656 . . . ? O6 Gd2 O18 Gd3 -0.82(16) . . . . ? O11 Gd2 O18 Gd3 80.74(17) . . . . ? O14 Gd2 O18 Gd3 -160.51(14) 2_557 . . . ? O10 Gd2 O18 Gd3 -31.0(3) . . . . ? O19 Gd2 O18 Gd3 172.8(2) . . . . ? O8 Gd2 O18 Gd3 87.52(18) . . . . ? C29 Gd2 O18 Gd3 171.6(3) . . . . ? O18 C29 O19 Gd2 2.3(5) . . . . ? C22 C29 O19 Gd2 -176.8(3) . . . . ? O16 Gd2 O19 C29 -75.2(3) 2_656 . . . ? O6 Gd2 O19 C29 7.1(3) . . . . ? O11 Gd2 O19 C29 72.0(3) . . . . ? O14 Gd2 O19 C29 -160.2(3) 2_557 . . . ? O10 Gd2 O19 C29 -156.5(3) . . . . ? O18 Gd2 O19 C29 -1.2(3) . . . . ? O8 Gd2 O19 C29 127.9(3) . . . . ? O21 C30 O20 Gd3 54.9(6) . . . 1_455 ? C24 C30 O20 Gd3 -124.4(4) . . . 1_455 ? O20 C30 O21 Gd3 20.7(8) . . . 2_566 ? C24 C30 O21 Gd3 -160.0(3) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.702 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 946976' ####################################################################### # # 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_p100710a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 Ho3 O25' _chemical_formula_weight 1278.27 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.191(2) _cell_length_b 12.122(2) _cell_length_c 14.884(3) _cell_angle_alpha 68.13(3) _cell_angle_beta 83.47(3) _cell_angle_gamma 74.45(3) _cell_volume 1643.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1085 _cell_measurement_theta_min 2.5105 _cell_measurement_theta_max 28.7933 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 7.261 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3245 _exptl_absorpt_correction_T_max 0.5305 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number 3908 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11349 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_unetI/netI 0.0350 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5784 _reflns_number_gt 5160 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR: the parameter to go anisotropic restraint to appointed atoms. SIMU: the parameter to set some atoms in limited range having the save shift parameters, and this parameter always is used with ISOR. simu 0.001 $c ISOR 0.005 0.001 C7 C8 C17 C18 c27 FREE Ho1 C9 ; _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^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5784 _refine_ls_number_parameters 514 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 1.24392(2) -0.52035(2) 0.899465(17) 0.01262(7) Uani 1 1 d . . . Ho2 Ho 0.35775(2) -0.02257(2) 0.784415(17) 0.01164(7) Uani 1 1 d . . . Ho3 Ho 0.48918(2) 0.28734(2) 0.540431(16) 0.01033(7) Uani 1 1 d . . . C1 C 1.0229(5) -0.2439(5) 0.7336(4) 0.0163(6) Uani 1 1 d U . . C2 C 0.9163(5) -0.2714(4) 0.8025(4) 0.0145(6) Uani 1 1 d U . . C3 C 0.8002(5) -0.1775(4) 0.7957(4) 0.0146(6) Uani 1 1 d U . . H3 H 0.7304 -0.1925 0.8412 0.017 Uiso 1 1 calc R . . C4 C 0.7836(5) -0.0622(5) 0.7238(4) 0.0156(6) Uani 1 1 d U . . C5 C 0.8895(5) -0.0390(5) 0.6581(4) 0.0187(6) Uani 1 1 d U . . H5 H 0.8805 0.0381 0.6101 0.022 Uiso 1 1 calc R . . C6 C 1.0075(5) -0.1282(5) 0.6628(4) 0.0188(6) Uani 1 1 d U . . H6 H 1.0775 -0.1109 0.6181 0.023 Uiso 1 1 calc R . . C7 C 1.2459(5) -0.2989(5) 0.6681(4) 0.0154(9) Uani 1 1 d U . . H7A H 1.2764 -0.2341 0.6765 0.019 Uiso 1 1 calc R . . H7B H 1.2096 -0.2686 0.6035 0.019 Uiso 1 1 calc R . . C8 C 1.3637(5) -0.4100(4) 0.6811(4) 0.0149(9) Uani 1 1 d U . . C9 C 0.9188(5) -0.3925(4) 0.8817(4) 0.0136(7) Uani 1 1 d U . . C10 C 0.6526(5) 0.0320(4) 0.7116(4) 0.0146(7) Uani 1 1 d U . . C11 C 0.2003(5) 0.0149(5) 1.0060(4) 0.0171(6) Uani 1 1 d U . . C12 C 0.1573(5) 0.1422(5) 0.9566(4) 0.0161(6) Uani 1 1 d U . . C13 C 0.0417(5) 0.2068(5) 0.9915(4) 0.0159(6) Uani 1 1 d U . . H13 H 0.0126 0.2912 0.9602 0.019 Uiso 1 1 calc R . . C14 C -0.0305(5) 0.1492(5) 1.0707(4) 0.0165(6) Uani 1 1 d U . . C15 C 0.0171(5) 0.0234(5) 1.1205(4) 0.0183(6) Uani 1 1 d U . . H15 H -0.0292 -0.0159 1.1757 0.022 Uiso 1 1 calc R . . C16 C 0.1320(5) -0.0430(5) 1.0886(4) 0.0188(6) Uani 1 1 d U . . H16 H 0.1636 -0.1266 1.1225 0.023 Uiso 1 1 calc R . . C17 C 0.3938(6) -0.1562(6) 1.0369(4) 0.0339(11) Uani 1 1 d U . . H17A H 0.3361 -0.2058 1.0805 0.041 Uiso 1 1 calc R . . H17B H 0.4430 -0.1313 1.0752 0.041 Uiso 1 1 calc R . . C18 C 0.4928(6) -0.2306(6) 0.9872(4) 0.0301(11) Uani 1 1 d U . . C19 C 0.2284(5) 0.2113(5) 0.8705(4) 0.0166(7) Uani 1 1 d U . . C20 C -0.1544(5) 0.2226(5) 1.1058(4) 0.0158(7) Uani 1 1 d U . . C21 C 0.1717(5) 0.3301(5) 0.4505(4) 0.0149(6) Uani 1 1 d U . . C22 C 0.1204(5) 0.2643(5) 0.5401(4) 0.0145(6) Uani 1 1 d U . . C23 C -0.0212(5) 0.2970(4) 0.5558(4) 0.0145(6) Uani 1 1 d U . . H23 H -0.0592 0.2522 0.6130 0.017 Uiso 1 1 calc R . . C24 C -0.1055(5) 0.3952(4) 0.4873(4) 0.0144(6) Uani 1 1 d U . . C25 C -0.0485(5) 0.4587(4) 0.3984(4) 0.0155(6) Uani 1 1 d U . . H25 H -0.1035 0.5245 0.3521 0.019 Uiso 1 1 calc R . . C26 C 0.0884(5) 0.4230(5) 0.3804(4) 0.0161(6) Uani 1 1 d U . . H26 H 0.1251 0.4620 0.3204 0.019 Uiso 1 1 calc R . . C27 C 0.3513(5) 0.2321(5) 0.3674(4) 0.0234(9) Uani 1 1 d U . . H27A H 0.3429 0.2897 0.3012 0.028 Uiso 1 1 calc R . . H27B H 0.2912 0.1787 0.3766 0.028 Uiso 1 1 calc R . . C28 C 0.4959(5) 0.1573(5) 0.3854(4) 0.0208(9) Uani 1 1 d U . . C29 C 0.2093(5) 0.1675(5) 0.6187(4) 0.0147(7) Uani 1 1 d U . . C30 C -0.2576(5) 0.4332(5) 0.5041(4) 0.0145(7) Uani 1 1 d U . . O1 O 1.1421(3) -0.3346(3) 0.7397(3) 0.0171(8) Uani 1 1 d . . . O2 O 1.4568(3) -0.4020(3) 0.6182(3) 0.0190(8) Uani 1 1 d . . . O3 O 1.3617(4) -0.5044(3) 0.7525(3) 0.0259(9) Uani 1 1 d . . . O4 O 1.0161(3) -0.4836(3) 0.8836(3) 0.0178(8) Uani 1 1 d . . . O5 O 0.8207(3) -0.3980(3) 0.9407(3) 0.0205(8) Uani 1 1 d . . . O6 O 0.5621(3) 0.0177(3) 0.7783(3) 0.0204(8) Uani 1 1 d . . . O7 O 0.6370(4) 0.1193(3) 0.6328(3) 0.0238(9) Uani 1 1 d . . . O8 O 0.3111(4) -0.0500(3) 0.9687(3) 0.0218(8) Uani 1 1 d . . . O9 O 0.5702(4) -0.3227(4) 1.0414(3) 0.0414(11) Uani 1 1 d . . . O10 O 0.4860(4) -0.1993(3) 0.8981(3) 0.0268(9) Uani 1 1 d . . . O11 O 0.2959(4) 0.1561(3) 0.8162(3) 0.0261(9) Uani 1 1 d . . . O12 O 0.2176(4) 0.3214(3) 0.8537(3) 0.0272(10) Uani 1 1 d . . . O13 O -0.1735(3) 0.3372(3) 1.0714(3) 0.0214(8) Uani 1 1 d . . . O14 O -0.2319(4) 0.1667(3) 1.1670(3) 0.0227(9) Uani 1 1 d . . . O15 O 0.3131(3) 0.2964(3) 0.4319(3) 0.0156(8) Uani 1 1 d . . . O16 O 0.5483(4) 0.1099(3) 0.3231(3) 0.0254(9) Uani 1 1 d . . . O17 O 0.5546(3) 0.1482(3) 0.4569(3) 0.0202(8) Uani 1 1 d . . . O18 O 0.3348(3) 0.1655(3) 0.6227(3) 0.0160(8) Uani 1 1 d . . . O19 O 0.1609(4) 0.0861(3) 0.6840(3) 0.0249(9) Uani 1 1 d . . . O20 O -0.3163(3) 0.3496(3) 0.5503(3) 0.0236(9) Uani 1 1 d . . . O21 O -0.3156(2) 0.54555(19) 0.46818(17) 0.0205(8) Uani 1 1 d . . . O22 O 1.4340(2) -0.43190(19) 0.89065(17) 0.0610(17) Uani 1 1 d R . . H22A H 1.3977 -0.3596 0.8896 0.073 Uiso 1 1 d R . . H22B H 1.5179 -0.4400 0.8738 0.073 Uiso 1 1 d R . . O23 O 0.4682(2) 0.29600(19) 0.70120(17) 0.0219(9) Uani 1 1 d R . . H23A H 0.4596 0.2317 0.7482 0.026 Uiso 1 1 d R . . H23B H 0.4188 0.3598 0.7105 0.026 Uiso 1 1 d R . . O24 O 0.6963(2) 0.46977(19) 0.84905(17) 0.158(4) Uani 1 1 d R . . H24A H 0.7505 0.4933 0.8736 0.237 Uiso 1 1 d R . . H24B H 0.7121 0.3920 0.8726 0.237 Uiso 1 1 d R . . O25 O 0.7173(7) 0.3407(9) 0.7459(6) 0.145(4) Uani 1 1 d . . . H25A H 0.6625 0.2970 0.7489 0.217 Uiso 1 1 d R . . H25B H 0.7236 0.3886 0.6877 0.217 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01148(13) 0.00948(13) 0.01312(13) -0.00339(10) 0.00245(9) 0.00151(9) Ho2 0.01033(13) 0.00941(13) 0.01348(13) -0.00429(10) 0.00283(9) -0.00063(9) Ho3 0.00683(12) 0.00989(13) 0.01166(13) -0.00259(10) 0.00206(9) -0.00055(9) C1 0.0122(12) 0.0144(12) 0.0192(13) -0.0045(11) 0.0019(11) -0.0011(10) C2 0.0111(11) 0.0135(12) 0.0182(13) -0.0055(10) 0.0008(10) -0.0023(10) C3 0.0112(12) 0.0135(12) 0.0181(13) -0.0056(11) 0.0008(10) -0.0020(10) C4 0.0123(11) 0.0135(12) 0.0192(13) -0.0049(10) 0.0007(10) -0.0018(10) C5 0.0134(12) 0.0154(12) 0.0209(13) -0.0021(11) 0.0022(11) -0.0005(10) C6 0.0133(12) 0.0157(12) 0.0207(13) -0.0023(11) 0.0033(11) -0.0002(11) C7 0.0137(18) 0.0157(18) 0.0151(19) -0.0046(15) 0.0054(15) -0.0044(15) C8 0.0135(18) 0.0152(18) 0.0152(19) -0.0049(16) 0.0051(15) -0.0049(15) C9 0.0102(13) 0.0133(14) 0.0175(15) -0.0061(12) 0.0001(12) -0.0026(12) C10 0.0122(14) 0.0125(14) 0.0192(15) -0.0062(12) -0.0007(12) -0.0025(12) C11 0.0171(12) 0.0160(12) 0.0199(13) -0.0097(11) 0.0030(11) -0.0039(11) C12 0.0167(12) 0.0156(12) 0.0195(12) -0.0104(10) 0.0032(10) -0.0051(10) C13 0.0167(12) 0.0153(12) 0.0193(12) -0.0099(11) 0.0032(10) -0.0057(10) C14 0.0171(12) 0.0158(12) 0.0191(12) -0.0093(10) 0.0032(10) -0.0049(10) C15 0.0181(12) 0.0167(12) 0.0201(13) -0.0079(11) 0.0036(11) -0.0039(11) C16 0.0183(12) 0.0169(12) 0.0207(13) -0.0077(11) 0.0034(11) -0.0034(11) C17 0.030(2) 0.032(2) 0.026(2) -0.0069(18) 0.0001(18) 0.0100(17) C18 0.027(2) 0.029(2) 0.025(2) -0.0080(18) -0.0003(17) 0.0064(17) C19 0.0170(14) 0.0158(14) 0.0199(15) -0.0103(12) 0.0035(12) -0.0046(12) C20 0.0167(14) 0.0159(14) 0.0183(14) -0.0097(12) 0.0026(12) -0.0053(12) C21 0.0101(12) 0.0143(12) 0.0197(13) -0.0061(11) 0.0009(10) -0.0026(10) C22 0.0096(11) 0.0138(11) 0.0194(12) -0.0061(10) 0.0013(9) -0.0022(9) C23 0.0099(11) 0.0135(12) 0.0195(12) -0.0059(10) 0.0007(10) -0.0024(10) C24 0.0101(11) 0.0136(11) 0.0194(12) -0.0060(10) -0.0002(9) -0.0024(9) C25 0.0107(12) 0.0145(12) 0.0199(13) -0.0053(11) -0.0004(10) -0.0021(10) C26 0.0110(12) 0.0150(12) 0.0201(13) -0.0051(11) 0.0007(10) -0.0018(10) C27 0.0190(19) 0.030(2) 0.024(2) -0.0160(18) 0.0031(17) -0.0036(17) C28 0.017(2) 0.028(2) 0.023(2) -0.0161(19) 0.0037(17) -0.0058(17) C29 0.0097(13) 0.0137(14) 0.0190(15) -0.0059(12) 0.0025(12) -0.0014(12) C30 0.0104(13) 0.0142(14) 0.0190(14) -0.0062(12) -0.0007(12) -0.0023(12) O1 0.0102(18) 0.0163(19) 0.018(2) -0.0029(16) 0.0062(15) 0.0007(15) O2 0.0119(19) 0.020(2) 0.019(2) -0.0049(17) 0.0079(16) -0.0010(16) O3 0.024(2) 0.015(2) 0.024(2) 0.0004(18) 0.0136(18) 0.0022(17) O4 0.0125(18) 0.0094(18) 0.028(2) -0.0050(17) -0.0017(16) 0.0017(14) O5 0.016(2) 0.019(2) 0.017(2) -0.0015(17) 0.0062(16) 0.0004(16) O6 0.0138(19) 0.020(2) 0.029(2) -0.0122(18) 0.0003(16) -0.0020(16) O7 0.019(2) 0.019(2) 0.025(2) -0.0020(18) -0.0027(17) 0.0019(16) O8 0.022(2) 0.015(2) 0.021(2) -0.0063(17) 0.0041(17) 0.0049(16) O9 0.036(3) 0.037(3) 0.024(2) -0.001(2) 0.000(2) 0.021(2) O10 0.028(2) 0.023(2) 0.019(2) -0.0046(19) 0.0038(18) 0.0042(18) O11 0.038(2) 0.015(2) 0.026(2) -0.0132(18) 0.0168(19) -0.0070(18) O12 0.031(2) 0.016(2) 0.039(3) -0.016(2) 0.0179(19) -0.0112(18) O13 0.021(2) 0.017(2) 0.026(2) -0.0104(18) 0.0079(17) -0.0029(16) O14 0.022(2) 0.020(2) 0.027(2) -0.0088(18) 0.0102(17) -0.0107(17) O15 0.0080(17) 0.020(2) 0.021(2) -0.0104(17) -0.0005(15) -0.0021(15) O16 0.028(2) 0.031(2) 0.026(2) -0.020(2) 0.0083(18) -0.0083(18) O17 0.0151(19) 0.021(2) 0.021(2) -0.0086(18) 0.0007(16) 0.0012(16) O18 0.0096(18) 0.0183(19) 0.017(2) -0.0033(16) 0.0009(15) -0.0036(15) O19 0.016(2) 0.024(2) 0.025(2) 0.0046(18) -0.0010(17) -0.0089(17) O20 0.014(2) 0.025(2) 0.028(2) -0.0049(19) 0.0028(17) -0.0072(17) O21 0.0127(19) 0.017(2) 0.031(2) -0.0117(18) -0.0012(16) 0.0027(15) O22 0.025(3) 0.056(3) 0.125(5) -0.061(4) -0.003(3) -0.003(2) O23 0.034(2) 0.013(2) 0.018(2) -0.0083(17) 0.0086(17) -0.0058(17) O24 0.067(5) 0.211(10) 0.259(12) -0.158(10) -0.002(6) -0.030(6) O25 0.102(6) 0.279(12) 0.085(6) -0.076(7) 0.019(5) -0.092(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O4 2.266(3) . ? Ho1 O9 2.277(4) 2_747 ? Ho1 O5 2.305(4) 2_747 ? Ho1 O13 2.329(3) 2_657 ? Ho1 O3 2.340(4) . ? Ho1 O12 2.347(3) 1_645 ? Ho1 O22 2.423(2) . ? Ho1 O1 2.668(4) . ? Ho2 O16 2.229(3) 2_656 ? Ho2 O6 2.248(3) . ? Ho2 O14 2.296(3) 2_557 ? Ho2 O11 2.296(3) . ? Ho2 O10 2.338(4) . ? Ho2 O19 2.406(4) . ? Ho2 O18 2.607(4) . ? Ho2 O8 2.639(4) . ? Ho2 C29 2.903(6) . ? Ho3 O7 2.247(4) . ? Ho3 O21 2.277(2) 2_566 ? Ho3 O20 2.340(3) 1_655 ? Ho3 O2 2.341(4) 2_756 ? Ho3 O17 2.368(3) . ? Ho3 O18 2.370(3) . ? Ho3 O23 2.417(2) . ? Ho3 O15 2.503(3) . ? C1 C6 1.386(7) . ? C1 O1 1.387(6) . ? C1 C2 1.425(6) . ? C2 C3 1.388(7) . ? C2 C9 1.497(7) . ? C3 C4 1.389(7) . ? C3 H3 0.9300 . ? C4 C5 1.384(7) . ? C4 C10 1.484(7) . ? C5 C6 1.373(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.445(5) . ? C7 C8 1.511(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O3 1.241(6) . ? C8 O2 1.251(5) . ? C9 O5 1.251(5) . ? C9 O4 1.264(6) . ? C10 O7 1.244(6) . ? C10 O6 1.271(6) . ? C11 O8 1.382(6) . ? C11 C16 1.383(7) . ? C11 C12 1.407(7) . ? C12 C13 1.392(6) . ? C12 C19 1.477(7) . ? C13 C14 1.373(7) . ? C13 H13 0.9300 . ? C14 C15 1.397(7) . ? C14 C20 1.501(7) . ? C15 C16 1.377(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O8 1.428(7) . ? C17 C18 1.489(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O9 1.233(7) . ? C18 O10 1.241(7) . ? C19 O12 1.239(6) . ? C19 O11 1.267(6) . ? C20 O14 1.255(6) . ? C20 O13 1.257(6) . ? C21 C26 1.375(7) . ? C21 C22 1.399(7) . ? C21 O15 1.414(6) . ? C22 C23 1.407(6) . ? C22 C29 1.489(7) . ? C23 C24 1.393(7) . ? C23 H23 0.9300 . ? C24 C25 1.409(7) . ? C24 C30 1.515(6) . ? C25 C26 1.372(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 O15 1.411(5) . ? C27 C28 1.503(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O17 1.235(6) . ? C28 O16 1.262(6) . ? C29 O19 1.264(6) . ? C29 O18 1.280(6) . ? C30 O20 1.252(6) . ? C30 O21 1.260(5) . ? O2 Ho3 2.341(4) 2_756 ? O5 Ho1 2.305(4) 2_747 ? O9 Ho1 2.277(4) 2_747 ? O12 Ho1 2.347(3) 1_465 ? O13 Ho1 2.329(3) 2_657 ? O14 Ho2 2.296(3) 2_557 ? O16 Ho2 2.229(3) 2_656 ? O20 Ho3 2.340(3) 1_455 ? O21 Ho3 2.277(2) 2_566 ? O22 H22A 0.8502 . ? O22 H22B 0.8527 . ? O23 H23A 0.8491 . ? O23 H23B 0.8520 . ? O24 H24A 0.8534 . ? O24 H24B 0.8506 . ? O25 H25A 0.8548 . ? O25 H25B 0.8517 . ? 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 Ho1 O9 141.06(15) . 2_747 ? O4 Ho1 O5 79.68(13) . 2_747 ? O9 Ho1 O5 79.02(14) 2_747 2_747 ? O4 Ho1 O13 80.53(12) . 2_657 ? O9 Ho1 O13 128.02(15) 2_747 2_657 ? O5 Ho1 O13 82.64(13) 2_747 2_657 ? O4 Ho1 O3 112.10(13) . . ? O9 Ho1 O3 82.16(14) 2_747 . ? O5 Ho1 O3 160.16(13) 2_747 . ? O13 Ho1 O3 114.31(12) 2_657 . ? O4 Ho1 O12 75.48(12) . 1_645 ? O9 Ho1 O12 74.99(15) 2_747 1_645 ? O5 Ho1 O12 96.46(13) 2_747 1_645 ? O13 Ho1 O12 155.74(13) 2_657 1_645 ? O3 Ho1 O12 72.45(12) . 1_645 ? O4 Ho1 O22 146.11(10) . . ? O9 Ho1 O22 72.26(13) 2_747 . ? O5 Ho1 O22 109.01(10) 2_747 . ? O13 Ho1 O22 68.70(10) 2_657 . ? O3 Ho1 O22 70.63(11) . . ? O12 Ho1 O22 133.10(10) 1_645 . ? O4 Ho1 O1 65.45(12) . . ? O9 Ho1 O1 143.20(13) 2_747 . ? O5 Ho1 O1 137.77(11) 2_747 . ? O13 Ho1 O1 69.25(12) 2_657 . ? O3 Ho1 O1 61.39(12) . . ? O12 Ho1 O1 97.03(13) 1_645 . ? O22 Ho1 O1 89.84(9) . . ? O16 Ho2 O6 84.13(13) 2_656 . ? O16 Ho2 O14 84.96(12) 2_656 2_557 ? O6 Ho2 O14 147.63(14) . 2_557 ? O16 Ho2 O11 145.70(14) 2_656 . ? O6 Ho2 O11 79.28(13) . . ? O14 Ho2 O11 123.76(12) 2_557 . ? O16 Ho2 O10 85.10(14) 2_656 . ? O6 Ho2 O10 76.07(14) . . ? O14 Ho2 O10 72.69(14) 2_557 . ? O11 Ho2 O10 119.03(14) . . ? O16 Ho2 O19 90.08(14) 2_656 . ? O6 Ho2 O19 131.37(13) . . ? O14 Ho2 O19 78.94(13) 2_557 . ? O11 Ho2 O19 79.08(14) . . ? O10 Ho2 O19 151.53(12) . . ? O16 Ho2 O18 77.68(13) 2_656 . ? O6 Ho2 O18 80.13(12) . . ? O14 Ho2 O18 126.77(12) 2_557 . ? O11 Ho2 O18 70.05(12) . . ? O10 Ho2 O18 151.86(11) . . ? O19 Ho2 O18 51.58(11) . . ? O16 Ho2 O8 147.13(13) 2_656 . ? O6 Ho2 O8 94.68(12) . . ? O14 Ho2 O8 78.64(12) 2_557 . ? O11 Ho2 O8 64.72(12) . . ? O10 Ho2 O8 62.94(12) . . ? O19 Ho2 O8 114.04(12) . . ? O18 Ho2 O8 134.62(10) . . ? O16 Ho2 C29 83.89(14) 2_656 . ? O6 Ho2 C29 106.08(14) . . ? O14 Ho2 C29 102.91(14) 2_557 . ? O11 Ho2 C29 72.37(14) . . ? O10 Ho2 C29 168.48(13) . . ? O19 Ho2 C29 25.42(12) . . ? O18 Ho2 C29 26.17(11) . . ? O8 Ho2 C29 127.37(12) . . ? O7 Ho3 O21 148.15(11) . 2_566 ? O7 Ho3 O20 73.60(13) . 1_655 ? O21 Ho3 O20 103.70(10) 2_566 1_655 ? O7 Ho3 O2 122.21(13) . 2_756 ? O21 Ho3 O2 85.66(11) 2_566 2_756 ? O20 Ho3 O2 73.74(13) 1_655 2_756 ? O7 Ho3 O17 71.88(13) . . ? O21 Ho3 O17 136.20(11) 2_566 . ? O20 Ho3 O17 106.86(12) 1_655 . ? O2 Ho3 O17 73.86(12) 2_756 . ? O7 Ho3 O18 80.68(13) . . ? O21 Ho3 O18 87.34(10) 2_566 . ? O20 Ho3 O18 146.91(13) 1_655 . ? O2 Ho3 O18 138.91(12) 2_756 . ? O17 Ho3 O18 83.87(11) . . ? O7 Ho3 O23 73.64(11) . . ? O21 Ho3 O23 74.83(10) 2_566 . ? O20 Ho3 O23 77.40(10) 1_655 . ? O2 Ho3 O23 139.97(10) 2_756 . ? O17 Ho3 O23 142.17(11) . . ? O18 Ho3 O23 75.61(9) . . ? O7 Ho3 O15 127.22(12) . . ? O21 Ho3 O15 72.60(9) 2_566 . ? O20 Ho3 O15 146.08(12) 1_655 . ? O2 Ho3 O15 72.36(12) 2_756 . ? O17 Ho3 O15 64.47(11) . . ? O18 Ho3 O15 66.92(12) . . ? O23 Ho3 O15 130.67(9) . . ? C6 C1 O1 121.1(4) . . ? C6 C1 C2 120.2(5) . . ? O1 C1 C2 118.7(4) . . ? C3 C2 C1 117.0(5) . . ? C3 C2 C9 117.2(4) . . ? C1 C2 C9 125.7(4) . . ? C2 C3 C4 122.8(5) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C5 C4 C3 118.4(5) . . ? C5 C4 C10 119.8(5) . . ? C3 C4 C10 121.6(4) . . ? C6 C5 C4 121.0(5) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 120.5(5) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? O1 C7 C8 108.2(4) . . ? O1 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O1 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? O3 C8 O2 123.7(5) . . ? O3 C8 C7 118.3(4) . . ? O2 C8 C7 118.0(4) . . ? O5 C9 O4 123.8(5) . . ? O5 C9 C2 117.3(4) . . ? O4 C9 C2 118.8(4) . . ? O7 C10 O6 124.0(5) . . ? O7 C10 C4 116.3(4) . . ? O6 C10 C4 119.7(5) . . ? O8 C11 C16 121.4(5) . . ? O8 C11 C12 117.9(4) . . ? C16 C11 C12 120.7(5) . . ? C13 C12 C11 118.0(5) . . ? C13 C12 C19 118.2(5) . . ? C11 C12 C19 123.8(4) . . ? C14 C13 C12 121.7(5) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 119.0(5) . . ? C13 C14 C20 119.9(5) . . ? C15 C14 C20 121.0(5) . . ? C16 C15 C14 120.7(5) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C11 119.8(5) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? O8 C17 C18 111.1(5) . . ? O8 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? O8 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? O9 C18 O10 126.3(5) . . ? O9 C18 C17 115.0(5) . . ? O10 C18 C17 118.6(6) . . ? O12 C19 O11 122.7(5) . . ? O12 C19 C12 118.5(4) . . ? O11 C19 C12 118.7(4) . . ? O14 C20 O13 124.2(5) . . ? O14 C20 C14 118.7(4) . . ? O13 C20 C14 117.1(4) . . ? C26 C21 C22 122.0(5) . . ? C26 C21 O15 119.8(4) . . ? C22 C21 O15 118.1(5) . . ? C21 C22 C23 117.1(5) . . ? C21 C22 C29 122.9(4) . . ? C23 C22 C29 120.0(5) . . ? C24 C23 C22 121.3(5) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 119.1(4) . . ? C23 C24 C30 121.9(5) . . ? C25 C24 C30 118.9(5) . . ? C26 C25 C24 119.8(5) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 120.4(5) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? O15 C27 C28 109.8(4) . . ? O15 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? O15 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? O17 C28 O16 125.3(5) . . ? O17 C28 C27 119.1(4) . . ? O16 C28 C27 115.6(5) . . ? O19 C29 O18 118.7(5) . . ? O19 C29 C22 120.1(4) . . ? O18 C29 C22 121.2(4) . . ? O19 C29 Ho2 54.8(3) . . ? O18 C29 Ho2 63.9(3) . . ? C22 C29 Ho2 174.1(3) . . ? O20 C30 O21 125.3(4) . . ? O20 C30 C24 117.1(4) . . ? O21 C30 C24 117.6(4) . . ? C1 O1 C7 115.3(4) . . ? C1 O1 Ho1 126.5(3) . . ? C7 O1 Ho1 112.7(3) . . ? C8 O2 Ho3 143.4(3) . 2_756 ? C8 O3 Ho1 127.8(3) . . ? C9 O4 Ho1 132.3(3) . . ? C9 O5 Ho1 145.3(3) . 2_747 ? C10 O6 Ho2 131.2(3) . . ? C10 O7 Ho3 144.9(3) . . ? C11 O8 C17 116.4(4) . . ? C11 O8 Ho2 126.2(3) . . ? C17 O8 Ho2 116.3(3) . . ? C18 O9 Ho1 162.3(4) . 2_747 ? C18 O10 Ho2 130.6(4) . . ? C19 O11 Ho2 146.6(3) . . ? C19 O12 Ho1 151.0(4) . 1_465 ? C20 O13 Ho1 147.0(3) . 2_657 ? C20 O14 Ho2 149.5(3) . 2_557 ? C27 O15 C21 115.5(3) . . ? C27 O15 Ho3 118.9(3) . . ? C21 O15 Ho3 122.8(3) . . ? C28 O16 Ho2 178.9(4) . 2_656 ? C28 O17 Ho3 124.4(3) . . ? C29 O18 Ho3 138.6(3) . . ? C29 O18 Ho2 89.9(3) . . ? Ho3 O18 Ho2 130.99(14) . . ? C29 O19 Ho2 99.8(3) . . ? C30 O20 Ho3 139.4(4) . 1_455 ? C30 O21 Ho3 152.9(3) . 2_566 ? Ho1 O22 H22A 104.8 . . ? Ho1 O22 H22B 141.4 . . ? H22A O22 H22B 111.1 . . ? Ho3 O23 H23A 117.4 . . ? Ho3 O23 H23B 119.5 . . ? H23A O23 H23B 110.7 . . ? H24A O24 H24B 109.5 . . ? H25A O25 H25B 109.4 . . ? 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 C6 C1 C2 C3 -0.9(7) . . . . ? O1 C1 C2 C3 178.3(4) . . . . ? C6 C1 C2 C9 179.2(5) . . . . ? O1 C1 C2 C9 -1.5(7) . . . . ? C1 C2 C3 C4 2.1(7) . . . . ? C9 C2 C3 C4 -178.0(4) . . . . ? C2 C3 C4 C5 -2.1(7) . . . . ? C2 C3 C4 C10 173.1(4) . . . . ? C3 C4 C5 C6 0.9(7) . . . . ? C10 C4 C5 C6 -174.4(5) . . . . ? C4 C5 C6 C1 0.1(8) . . . . ? O1 C1 C6 C5 -179.4(4) . . . . ? C2 C1 C6 C5 -0.1(8) . . . . ? O1 C7 C8 O3 -7.8(6) . . . . ? O1 C7 C8 O2 171.2(4) . . . . ? C3 C2 C9 O5 -5.4(7) . . . . ? C1 C2 C9 O5 174.5(4) . . . . ? C3 C2 C9 O4 172.3(4) . . . . ? C1 C2 C9 O4 -7.8(7) . . . . ? C5 C4 C10 O7 12.0(7) . . . . ? C3 C4 C10 O7 -163.1(4) . . . . ? C5 C4 C10 O6 -170.8(4) . . . . ? C3 C4 C10 O6 14.1(7) . . . . ? O8 C11 C12 C13 176.9(4) . . . . ? C16 C11 C12 C13 -2.2(7) . . . . ? O8 C11 C12 C19 -3.6(7) . . . . ? C16 C11 C12 C19 177.3(5) . . . . ? C11 C12 C13 C14 -0.9(7) . . . . ? C19 C12 C13 C14 179.6(4) . . . . ? C12 C13 C14 C15 3.2(7) . . . . ? C12 C13 C14 C20 179.9(4) . . . . ? C13 C14 C15 C16 -2.4(7) . . . . ? C20 C14 C15 C16 -179.1(5) . . . . ? C14 C15 C16 C11 -0.6(8) . . . . ? O8 C11 C16 C15 -176.2(4) . . . . ? C12 C11 C16 C15 3.0(7) . . . . ? O8 C17 C18 O9 178.4(5) . . . . ? O8 C17 C18 O10 -5.2(8) . . . . ? C13 C12 C19 O12 25.9(7) . . . . ? C11 C12 C19 O12 -153.5(5) . . . . ? C13 C12 C19 O11 -152.9(5) . . . . ? C11 C12 C19 O11 27.6(8) . . . . ? C13 C14 C20 O14 167.9(5) . . . . ? C15 C14 C20 O14 -15.5(7) . . . . ? C13 C14 C20 O13 -12.3(7) . . . . ? C15 C14 C20 O13 164.4(5) . . . . ? C26 C21 C22 C23 0.1(7) . . . . ? O15 C21 C22 C23 -178.1(4) . . . . ? C26 C21 C22 C29 -177.0(4) . . . . ? O15 C21 C22 C29 4.8(7) . . . . ? C21 C22 C23 C24 -3.5(7) . . . . ? C29 C22 C23 C24 173.7(4) . . . . ? C22 C23 C24 C25 3.4(7) . . . . ? C22 C23 C24 C30 -178.6(4) . . . . ? C23 C24 C25 C26 0.2(7) . . . . ? C30 C24 C25 C26 -177.8(4) . . . . ? C24 C25 C26 C21 -3.6(7) . . . . ? C22 C21 C26 C25 3.5(7) . . . . ? O15 C21 C26 C25 -178.4(4) . . . . ? O15 C27 C28 O17 8.8(7) . . . . ? O15 C27 C28 O16 -170.0(4) . . . . ? C21 C22 C29 O19 -157.9(5) . . . . ? C23 C22 C29 O19 25.1(7) . . . . ? C21 C22 C29 O18 23.1(7) . . . . ? C23 C22 C29 O18 -153.9(4) . . . . ? C21 C22 C29 Ho2 174(3) . . . . ? C23 C22 C29 Ho2 -3(3) . . . . ? O16 Ho2 C29 O19 103.2(3) 2_656 . . . ? O6 Ho2 C29 O19 -174.7(3) . . . . ? O14 Ho2 C29 O19 19.8(3) 2_557 . . . ? O11 Ho2 C29 O19 -101.9(3) . . . . ? O10 Ho2 C29 O19 86.0(7) . . . . ? O18 Ho2 C29 O19 177.6(5) . . . . ? O8 Ho2 C29 O19 -65.6(3) . . . . ? O16 Ho2 C29 O18 -74.4(3) 2_656 . . . ? O6 Ho2 C29 O18 7.6(3) . . . . ? O14 Ho2 C29 O18 -157.8(2) 2_557 . . . ? O11 Ho2 C29 O18 80.5(3) . . . . ? O10 Ho2 C29 O18 -91.6(7) . . . . ? O19 Ho2 C29 O18 -177.6(5) . . . . ? O8 Ho2 C29 O18 116.7(3) . . . . ? O16 Ho2 C29 C22 133(3) 2_656 . . . ? O6 Ho2 C29 C22 -145(3) . . . . ? O14 Ho2 C29 C22 50(3) 2_557 . . . ? O11 Ho2 C29 C22 -72(3) . . . . ? O10 Ho2 C29 C22 116(3) . . . . ? O19 Ho2 C29 C22 30(3) . . . . ? O18 Ho2 C29 C22 -152(3) . . . . ? O8 Ho2 C29 C22 -36(3) . . . . ? C23 C24 C30 O20 -35.1(7) . . . . ? C25 C24 C30 O20 142.9(5) . . . . ? C23 C24 C30 O21 147.0(4) . . . . ? C25 C24 C30 O21 -35.0(6) . . . . ? C6 C1 O1 C7 0.2(6) . . . . ? C2 C1 O1 C7 -179.1(4) . . . . ? C6 C1 O1 Ho1 151.9(4) . . . . ? C2 C1 O1 Ho1 -27.3(6) . . . . ? C8 C7 O1 C1 -176.3(4) . . . . ? C8 C7 O1 Ho1 28.1(4) . . . . ? O4 Ho1 O1 C1 43.4(3) . . . . ? O9 Ho1 O1 C1 -171.8(3) 2_747 . . . ? O5 Ho1 O1 C1 6.2(4) 2_747 . . . ? O13 Ho1 O1 C1 -45.4(3) 2_657 . . . ? O3 Ho1 O1 C1 179.5(4) . . . . ? O12 Ho1 O1 C1 113.9(3) 1_645 . . . ? O22 Ho1 O1 C1 -112.6(3) . . . . ? O4 Ho1 O1 C7 -164.2(3) . . . . ? O9 Ho1 O1 C7 -19.4(4) 2_747 . . . ? O5 Ho1 O1 C7 158.6(3) 2_747 . . . ? O13 Ho1 O1 C7 107.0(3) 2_657 . . . ? O3 Ho1 O1 C7 -28.1(3) . . . . ? O12 Ho1 O1 C7 -93.7(3) 1_645 . . . ? O22 Ho1 O1 C7 39.8(3) . . . . ? O3 C8 O2 Ho3 161.2(4) . . . 2_756 ? C7 C8 O2 Ho3 -17.7(7) . . . 2_756 ? O2 C8 O3 Ho1 157.6(3) . . . . ? C7 C8 O3 Ho1 -23.5(6) . . . . ? O4 Ho1 O3 C8 71.4(4) . . . . ? O9 Ho1 O3 C8 -146.2(4) 2_747 . . . ? O5 Ho1 O3 C8 -164.8(4) 2_747 . . . ? O13 Ho1 O3 C8 -17.9(5) 2_657 . . . ? O12 Ho1 O3 C8 137.1(4) 1_645 . . . ? O22 Ho1 O3 C8 -72.4(4) . . . . ? O1 Ho1 O3 C8 28.5(4) . . . . ? O5 C9 O4 Ho1 -120.7(4) . . . . ? C2 C9 O4 Ho1 61.8(6) . . . . ? O9 Ho1 O4 C9 149.6(4) 2_747 . . . ? O5 Ho1 O4 C9 91.8(5) 2_747 . . . ? O13 Ho1 O4 C9 7.6(4) 2_657 . . . ? O3 Ho1 O4 C9 -104.9(5) . . . . ? O12 Ho1 O4 C9 -168.7(5) 1_645 . . . ? O22 Ho1 O4 C9 -17.0(6) . . . . ? O1 Ho1 O4 C9 -63.8(4) . . . . ? O4 C9 O5 Ho1 40.5(8) . . . 2_747 ? C2 C9 O5 Ho1 -141.9(4) . . . 2_747 ? O7 C10 O6 Ho2 66.7(6) . . . . ? C4 C10 O6 Ho2 -110.3(5) . . . . ? O16 Ho2 O6 C10 26.8(4) 2_656 . . . ? O14 Ho2 O6 C10 97.7(5) 2_557 . . . ? O11 Ho2 O6 C10 -123.0(4) . . . . ? O10 Ho2 O6 C10 113.2(4) . . . . ? O19 Ho2 O6 C10 -58.1(5) . . . . ? O18 Ho2 O6 C10 -51.7(4) . . . . ? O8 Ho2 O6 C10 173.8(4) . . . . ? C29 Ho2 O6 C10 -55.1(4) . . . . ? O6 C10 O7 Ho3 -4.1(9) . . . . ? C4 C10 O7 Ho3 173.0(4) . . . . ? O21 Ho3 O7 C10 37.8(7) 2_566 . . . ? O20 Ho3 O7 C10 127.5(6) 1_655 . . . ? O2 Ho3 O7 C10 -174.6(5) 2_756 . . . ? O17 Ho3 O7 C10 -118.1(6) . . . . ? O18 Ho3 O7 C10 -31.5(6) . . . . ? O23 Ho3 O7 C10 46.1(5) . . . . ? O15 Ho3 O7 C10 -82.9(6) . . . . ? C16 C11 O8 C17 -31.4(7) . . . . ? C12 C11 O8 C17 149.5(5) . . . . ? C16 C11 O8 Ho2 136.1(4) . . . . ? C12 C11 O8 Ho2 -43.1(6) . . . . ? C18 C17 O8 C11 169.2(4) . . . . ? C18 C17 O8 Ho2 0.5(6) . . . . ? O16 Ho2 O8 C11 -150.6(3) 2_656 . . . ? O6 Ho2 O8 C11 123.0(3) . . . . ? O14 Ho2 O8 C11 -89.0(3) 2_557 . . . ? O11 Ho2 O8 C11 47.2(3) . . . . ? O10 Ho2 O8 C11 -165.3(4) . . . . ? O19 Ho2 O8 C11 -16.7(4) . . . . ? O18 Ho2 O8 C11 42.2(4) . . . . ? C29 Ho2 O8 C11 8.6(4) . . . . ? O16 Ho2 O8 C17 16.9(5) 2_656 . . . ? O6 Ho2 O8 C17 -69.6(4) . . . . ? O14 Ho2 O8 C17 78.4(4) 2_557 . . . ? O11 Ho2 O8 C17 -145.4(4) . . . . ? O10 Ho2 O8 C17 2.2(4) . . . . ? O19 Ho2 O8 C17 150.7(4) . . . . ? O18 Ho2 O8 C17 -150.3(3) . . . . ? C29 Ho2 O8 C17 176.1(3) . . . . ? O10 C18 O9 Ho1 34.2(19) . . . 2_747 ? C17 C18 O9 Ho1 -149.7(12) . . . 2_747 ? O9 C18 O10 Ho2 -175.0(4) . . . . ? C17 C18 O10 Ho2 9.0(8) . . . . ? O16 Ho2 O10 C18 -178.3(5) 2_656 . . . ? O6 Ho2 O10 C18 96.5(5) . . . . ? O14 Ho2 O10 C18 -92.1(5) 2_557 . . . ? O11 Ho2 O10 C18 27.4(5) . . . . ? O19 Ho2 O10 C18 -97.2(5) . . . . ? O18 Ho2 O10 C18 129.6(5) . . . . ? O8 Ho2 O10 C18 -6.2(5) . . . . ? C29 Ho2 O10 C18 -161.2(6) . . . . ? O12 C19 O11 Ho2 -174.4(4) . . . . ? C12 C19 O11 Ho2 4.4(10) . . . . ? O16 Ho2 O11 C19 166.3(6) 2_656 . . . ? O6 Ho2 O11 C19 -131.2(7) . . . . ? O14 Ho2 O11 C19 23.9(7) 2_557 . . . ? O10 Ho2 O11 C19 -63.9(7) . . . . ? O19 Ho2 O11 C19 92.6(7) . . . . ? O18 Ho2 O11 C19 145.5(7) . . . . ? O8 Ho2 O11 C19 -30.8(6) . . . . ? C29 Ho2 O11 C19 117.9(7) . . . . ? O11 C19 O12 Ho1 -122.8(6) . . . 1_465 ? C12 C19 O12 Ho1 58.4(9) . . . 1_465 ? O14 C20 O13 Ho1 38.8(9) . . . 2_657 ? C14 C20 O13 Ho1 -141.1(5) . . . 2_657 ? O13 C20 O14 Ho2 129.7(6) . . . 2_557 ? C14 C20 O14 Ho2 -50.5(9) . . . 2_557 ? C28 C27 O15 C21 -156.1(4) . . . . ? C28 C27 O15 Ho3 5.7(5) . . . . ? C26 C21 O15 C27 -72.7(6) . . . . ? C22 C21 O15 C27 105.5(5) . . . . ? C26 C21 O15 Ho3 126.3(4) . . . . ? C22 C21 O15 Ho3 -55.5(5) . . . . ? O7 Ho3 O15 C27 -48.0(4) . . . . ? O21 Ho3 O15 C27 160.4(4) 2_566 . . . ? O20 Ho3 O15 C27 71.6(4) 1_655 . . . ? O2 Ho3 O15 C27 69.5(3) 2_756 . . . ? O17 Ho3 O15 C27 -10.7(3) . . . . ? O18 Ho3 O15 C27 -105.0(4) . . . . ? O23 Ho3 O15 C27 -148.7(3) . . . . ? O7 Ho3 O15 C21 112.3(3) . . . . ? O21 Ho3 O15 C21 -39.3(3) 2_566 . . . ? O20 Ho3 O15 C21 -128.1(3) 1_655 . . . ? O2 Ho3 O15 C21 -130.2(3) 2_756 . . . ? O17 Ho3 O15 C21 149.6(4) . . . . ? O18 Ho3 O15 C21 55.3(3) . . . . ? O23 Ho3 O15 C21 11.6(4) . . . . ? O17 C28 O16 Ho2 50(18) . . . 2_656 ? C27 C28 O16 Ho2 -131(17) . . . 2_656 ? O16 C28 O17 Ho3 157.5(4) . . . . ? C27 C28 O17 Ho3 -21.2(7) . . . . ? O7 Ho3 O17 C28 166.6(4) . . . . ? O21 Ho3 O17 C28 4.8(5) 2_566 . . . ? O20 Ho3 O17 C28 -127.6(4) 1_655 . . . ? O2 Ho3 O17 C28 -60.7(4) 2_756 . . . ? O18 Ho3 O17 C28 84.5(4) . . . . ? O23 Ho3 O17 C28 141.4(4) . . . . ? O15 Ho3 O17 C28 17.1(4) . . . . ? O19 C29 O18 Ho3 -173.9(3) . . . . ? C22 C29 O18 Ho3 5.1(7) . . . . ? Ho2 C29 O18 Ho3 -171.7(4) . . . . ? O19 C29 O18 Ho2 -2.2(4) . . . . ? C22 C29 O18 Ho2 176.8(4) . . . . ? O7 Ho3 O18 C29 -170.6(5) . . . . ? O21 Ho3 O18 C29 39.0(4) 2_566 . . . ? O20 Ho3 O18 C29 150.3(4) 1_655 . . . ? O2 Ho3 O18 C29 -41.3(5) 2_756 . . . ? O17 Ho3 O18 C29 -98.0(5) . . . . ? O23 Ho3 O18 C29 114.0(5) . . . . ? O15 Ho3 O18 C29 -33.2(4) . . . . ? O7 Ho3 O18 Ho2 20.46(18) . . . . ? O21 Ho3 O18 Ho2 -129.92(17) 2_566 . . . ? O20 Ho3 O18 Ho2 -18.6(3) 1_655 . . . ? O2 Ho3 O18 Ho2 149.78(16) 2_756 . . . ? O17 Ho3 O18 Ho2 93.05(19) . . . . ? O23 Ho3 O18 Ho2 -54.91(16) . . . . ? O15 Ho3 O18 Ho2 157.9(2) . . . . ? O16 Ho2 O18 C29 101.4(3) 2_656 . . . ? O6 Ho2 O18 C29 -172.5(3) . . . . ? O14 Ho2 O18 C29 27.4(3) 2_557 . . . ? O11 Ho2 O18 C29 -90.5(3) . . . . ? O10 Ho2 O18 C29 154.9(3) . . . . ? O19 Ho2 O18 C29 1.3(3) . . . . ? O8 Ho2 O18 C29 -85.7(3) . . . . ? O16 Ho2 O18 Ho3 -85.92(19) 2_656 . . . ? O6 Ho2 O18 Ho3 0.16(17) . . . . ? O14 Ho2 O18 Ho3 -159.93(16) 2_557 . . . ? O11 Ho2 O18 Ho3 82.25(19) . . . . ? O10 Ho2 O18 Ho3 -32.3(3) . . . . ? O19 Ho2 O18 Ho3 174.0(2) . . . . ? O8 Ho2 O18 Ho3 87.0(2) . . . . ? C29 Ho2 O18 Ho3 172.7(4) . . . . ? O18 C29 O19 Ho2 2.4(5) . . . . ? C22 C29 O19 Ho2 -176.6(4) . . . . ? O16 Ho2 O19 C29 -75.5(3) 2_656 . . . ? O6 Ho2 O19 C29 6.8(4) . . . . ? O14 Ho2 O19 C29 -160.3(3) 2_557 . . . ? O11 Ho2 O19 C29 71.8(3) . . . . ? O10 Ho2 O19 C29 -155.3(3) . . . . ? O18 Ho2 O19 C29 -1.3(3) . . . . ? O8 Ho2 O19 C29 127.6(3) . . . . ? O21 C30 O20 Ho3 44.5(8) . . . 1_455 ? C24 C30 O20 Ho3 -133.2(4) . . . 1_455 ? O20 C30 O21 Ho3 23.3(9) . . . 2_566 ? C24 C30 O21 Ho3 -159.0(4) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.090 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.153 _database_code_depnum_ccdc_archive 'CCDC 946977' ####################################################################### # # 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_p110408n1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H13 O11 Pr' _chemical_formula_weight 450.11 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9671(4) _cell_length_b 9.1124(6) _cell_length_c 9.7614(5) _cell_angle_alpha 74.932(5) _cell_angle_beta 68.329(5) _cell_angle_gamma 69.519(5) _cell_volume 686.51(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3296 _cell_measurement_theta_min 2.5431 _cell_measurement_theta_max 29.1413 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 3.607 _exptl_absorpt_correction_type MULTI-scan _exptl_absorpt_correction_T_min 0.5324 _exptl_absorpt_correction_T_max 0.7143 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number 3908 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4329 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_unetI/netI 0.0646 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2401 _reflns_number_gt 2186 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^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 2401 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Pr1 Pr 0.22420(3) 0.54587(3) 0.52575(3) 0.01795(11) Uani 1 1 d . . . C1 C 0.4619(6) 0.1896(6) 0.2592(5) 0.0174(11) Uani 1 1 d . . . C2 C 0.5836(6) 0.2729(6) 0.2017(6) 0.0187(11) Uani 1 1 d . . . C3 C 0.6500(6) 0.3099(6) 0.0503(5) 0.0189(11) Uani 1 1 d . . . H3 H 0.7324 0.3622 0.0134 0.023 Uiso 1 1 calc R . . C4 C 0.5970(6) 0.2709(6) -0.0497(6) 0.0192(11) Uani 1 1 d . . . C5 C 0.4740(6) 0.1935(6) 0.0087(6) 0.0224(12) Uani 1 1 d . . . H5 H 0.4354 0.1685 -0.0562 0.027 Uiso 1 1 calc R . . C6 C 0.4068(6) 0.1525(7) 0.1594(6) 0.0268(13) Uani 1 1 d . . . H6 H 0.3246 0.1000 0.1952 0.032 Uiso 1 1 calc R . . C7 C 0.2755(6) 0.0848(6) 0.4755(6) 0.0210(11) Uani 1 1 d . . . H7A H 0.2760 0.0293 0.5748 0.025 Uiso 1 1 calc R . . H7B H 0.2826 0.0095 0.4175 0.025 Uiso 1 1 calc R . . C8 C 0.1136(6) 0.2160(6) 0.4860(5) 0.0187(11) Uani 1 1 d . . . C9 C 0.6357(6) 0.3268(6) 0.3054(5) 0.0182(11) Uani 1 1 d . . . C10 C 0.6679(6) 0.3141(6) -0.2115(6) 0.0211(12) Uani 1 1 d . . . O1 O 0.4168(4) 0.1446(4) 0.4080(4) 0.0235(8) Uani 1 1 d . . . O2 O -0.0133(4) 0.1837(4) 0.4938(4) 0.0280(9) Uani 1 1 d . . . O3 O 0.1117(4) 0.3533(4) 0.4898(4) 0.0306(9) Uani 1 1 d . . . O4 O 0.5270(4) 0.4034(4) 0.4063(4) 0.0246(9) Uani 1 1 d . . . O5 O 0.7882(4) 0.3019(5) 0.2845(4) 0.0298(10) Uani 1 1 d . . . O6 O 0.7620(4) 0.4040(5) -0.2592(4) 0.0276(9) Uani 1 1 d . . . O7 O 0.6373(4) 0.2612(4) -0.3028(4) 0.0238(8) Uani 1 1 d . . . O8 O 0.3202(4) 0.3140(5) 0.7014(4) 0.0360(10) Uani 1 1 d . . . H8A H 0.4276 0.2894 0.6798 0.043 Uiso 1 1 d R . . H8B H 0.2794 0.2381 0.7609 0.043 Uiso 1 1 d R . . O9 O -0.0113(4) 0.5175(5) 0.7698(4) 0.0395(11) Uani 1 1 d . . . H9A H -0.0956 0.4910 0.7768 0.047 Uiso 1 1 d R . . H9B H 0.0101 0.4869 0.8520 0.047 Uiso 1 1 d R . . O10 O 0.1271(6) 0.1352(6) 0.8938(6) 0.0706(16) Uani 1 1 d . . . H10A H 0.0638 0.1141 0.8599 0.085 Uiso 1 1 d R . . H10B H 0.1216 0.1046 0.9864 0.085 Uiso 1 1 d R . . O11 O 0.0329(5) 0.0255(5) 0.2078(5) 0.0459(11) Uani 1 1 d . . . H11A H -0.0484 0.1097 0.2252 0.055 Uiso 1 1 d R . . H11B H 0.0549 -0.0411 0.2808 0.055 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.01955(17) 0.02057(19) 0.01535(18) -0.00240(13) -0.00722(12) -0.00582(12) C1 0.016(2) 0.019(3) 0.015(3) -0.003(2) -0.004(2) -0.003(2) C2 0.016(2) 0.022(3) 0.020(3) -0.007(2) -0.008(2) -0.002(2) C3 0.018(2) 0.020(3) 0.018(3) -0.001(2) -0.005(2) -0.007(2) C4 0.025(3) 0.017(3) 0.015(3) 0.001(2) -0.009(2) -0.004(2) C5 0.024(3) 0.030(3) 0.019(3) -0.005(3) -0.011(2) -0.010(2) C6 0.024(3) 0.041(4) 0.021(3) 0.004(3) -0.007(2) -0.021(3) C7 0.019(3) 0.018(3) 0.018(3) 0.004(2) -0.003(2) -0.005(2) C8 0.025(3) 0.021(3) 0.011(3) -0.002(2) -0.008(2) -0.005(2) C9 0.029(3) 0.016(3) 0.013(3) 0.001(2) -0.010(2) -0.008(2) C10 0.018(3) 0.022(3) 0.021(3) -0.004(2) -0.006(2) -0.004(2) O1 0.0225(19) 0.033(2) 0.015(2) 0.0033(17) -0.0056(15) -0.0138(16) O2 0.0195(19) 0.028(2) 0.039(2) -0.0033(19) -0.0124(18) -0.0072(16) O3 0.039(2) 0.018(2) 0.037(2) -0.0028(19) -0.0167(19) -0.0064(17) O4 0.0241(19) 0.031(2) 0.023(2) -0.0115(18) -0.0052(17) -0.0088(17) O5 0.0170(19) 0.043(3) 0.034(2) -0.020(2) -0.0061(17) -0.0064(17) O6 0.032(2) 0.045(3) 0.015(2) -0.0022(18) -0.0074(17) -0.0238(19) O7 0.029(2) 0.025(2) 0.021(2) -0.0060(17) -0.0102(17) -0.0070(16) O8 0.025(2) 0.041(3) 0.039(3) 0.018(2) -0.0180(19) -0.0149(18) O9 0.029(2) 0.071(3) 0.027(2) -0.008(2) -0.0080(18) -0.024(2) O10 0.084(4) 0.086(4) 0.053(3) 0.020(3) -0.023(3) -0.057(3) O11 0.050(3) 0.036(3) 0.036(3) -0.002(2) -0.008(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O3 2.458(3) . ? Pr1 O8 2.465(4) . ? Pr1 O6 2.485(3) 2_665 ? Pr1 O4 2.530(3) . ? Pr1 O5 2.538(3) 2_666 ? Pr1 O2 2.539(4) 2_566 ? Pr1 O9 2.559(4) . ? Pr1 O7 2.629(4) 2_665 ? Pr1 O4 2.758(3) 2_666 ? Pr1 O3 2.875(3) 2_566 ? Pr1 C10 2.934(5) 2_665 ? Pr1 C9 3.031(4) 2_666 ? C1 O1 1.347(6) . ? C1 C6 1.396(6) . ? C1 C2 1.410(6) . ? C2 C3 1.373(7) . ? C2 C9 1.501(6) . ? C3 C4 1.394(6) . ? C3 H3 0.9300 . ? C4 C5 1.382(7) . ? C4 C10 1.471(7) . ? C5 C6 1.373(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.420(5) . ? C7 C8 1.512(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.244(5) . ? C8 O3 1.255(6) . ? C8 Pr1 3.070(5) 2_566 ? C9 O5 1.251(5) . ? C9 O4 1.257(6) . ? C9 Pr1 3.031(4) 2_666 ? C10 O6 1.263(6) . ? C10 O7 1.264(5) . ? C10 Pr1 2.934(5) 2_665 ? O2 Pr1 2.539(4) 2_566 ? O3 Pr1 2.875(3) 2_566 ? O4 Pr1 2.758(3) 2_666 ? O5 Pr1 2.538(3) 2_666 ? O6 Pr1 2.485(3) 2_665 ? O7 Pr1 2.629(4) 2_665 ? O8 H8A 0.8638 . ? O8 H8B 0.8726 . ? O9 H9A 0.8459 . ? O9 H9B 0.8481 . ? O10 H10A 0.8469 . ? O10 H10B 0.8626 . ? O11 H11A 0.8565 . ? O11 H11B 0.8431 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Pr1 O8 79.40(12) . . ? O3 Pr1 O6 72.39(12) . 2_665 ? O8 Pr1 O6 135.76(13) . 2_665 ? O3 Pr1 O4 94.86(11) . . ? O8 Pr1 O4 70.39(12) . . ? O6 Pr1 O4 78.70(12) 2_665 . ? O3 Pr1 O5 143.88(12) . 2_666 ? O8 Pr1 O5 82.93(13) . 2_666 ? O6 Pr1 O5 137.95(13) 2_665 2_666 ? O4 Pr1 O5 108.49(10) . 2_666 ? O3 Pr1 O2 107.53(11) . 2_566 ? O8 Pr1 O2 144.19(13) . 2_566 ? O6 Pr1 O2 78.01(12) 2_665 2_566 ? O4 Pr1 O2 140.71(12) . 2_566 ? O5 Pr1 O2 71.04(12) 2_666 2_566 ? O3 Pr1 O9 76.57(12) . . ? O8 Pr1 O9 68.69(13) . . ? O6 Pr1 O9 132.90(11) 2_665 . ? O4 Pr1 O9 139.06(13) . . ? O5 Pr1 O9 67.69(11) 2_666 . ? O2 Pr1 O9 78.67(13) 2_566 . ? O3 Pr1 O7 122.53(11) . 2_665 ? O8 Pr1 O7 136.38(11) . 2_665 ? O6 Pr1 O7 50.53(10) 2_665 2_665 ? O4 Pr1 O7 70.52(11) . 2_665 ? O5 Pr1 O7 91.69(11) 2_666 2_665 ? O2 Pr1 O7 70.23(11) 2_566 2_665 ? O9 Pr1 O7 147.10(12) . 2_665 ? O3 Pr1 O4 147.38(12) . 2_666 ? O8 Pr1 O4 72.57(11) . 2_666 ? O6 Pr1 O4 117.93(11) 2_665 2_666 ? O4 Pr1 O4 60.37(11) . 2_666 ? O5 Pr1 O4 48.41(10) 2_666 2_666 ? O2 Pr1 O4 104.95(10) 2_566 2_666 ? O9 Pr1 O4 107.38(10) . 2_666 ? O7 Pr1 O4 71.80(10) 2_665 2_666 ? O3 Pr1 O3 60.90(13) . 2_566 ? O8 Pr1 O3 121.98(12) . 2_566 ? O6 Pr1 O3 71.65(11) 2_665 2_566 ? O4 Pr1 O3 146.06(10) . 2_566 ? O5 Pr1 O3 104.56(10) 2_666 2_566 ? O2 Pr1 O3 47.20(10) 2_566 2_566 ? O9 Pr1 O3 62.46(11) . 2_566 ? O7 Pr1 O3 101.32(11) 2_665 2_566 ? O4 Pr1 O3 150.30(10) 2_666 2_566 ? O3 Pr1 C10 97.05(13) . 2_665 ? O8 Pr1 C10 140.25(13) . 2_665 ? O6 Pr1 C10 25.26(11) 2_665 2_665 ? O4 Pr1 C10 70.51(13) . 2_665 ? O5 Pr1 C10 116.33(13) 2_666 2_665 ? O2 Pr1 C10 74.94(13) 2_566 2_665 ? O9 Pr1 C10 149.52(13) . 2_665 ? O7 Pr1 C10 25.50(11) 2_665 2_665 ? O4 Pr1 C10 94.05(12) 2_666 2_665 ? O3 Pr1 C10 88.19(12) 2_566 2_665 ? O3 Pr1 C9 154.05(13) . 2_666 ? O8 Pr1 C9 76.00(13) . 2_666 ? O6 Pr1 C9 132.33(12) 2_665 2_666 ? O4 Pr1 C9 84.63(12) . 2_666 ? O5 Pr1 C9 23.93(12) 2_666 2_666 ? O2 Pr1 C9 88.18(12) 2_566 2_666 ? O9 Pr1 C9 86.84(12) . 2_666 ? O7 Pr1 C9 81.82(12) 2_665 2_666 ? O4 Pr1 C9 24.49(11) 2_666 2_666 ? O3 Pr1 C9 127.82(12) 2_566 2_666 ? C10 Pr1 C9 107.11(13) 2_665 2_666 ? O1 C1 C6 125.8(4) . . ? O1 C1 C2 115.5(4) . . ? C6 C1 C2 118.6(5) . . ? C3 C2 C1 119.8(4) . . ? C3 C2 C9 119.9(4) . . ? C1 C2 C9 120.2(4) . . ? C2 C3 C4 121.7(4) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 117.7(5) . . ? C5 C4 C10 121.5(4) . . ? C3 C4 C10 120.8(4) . . ? C6 C5 C4 122.0(4) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 120.1(4) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? O1 C7 C8 111.6(4) . . ? O1 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? O1 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? O2 C8 O3 122.4(5) . . ? O2 C8 C7 119.1(4) . . ? O3 C8 C7 118.5(4) . . ? O2 C8 Pr1 53.7(3) . 2_566 ? O3 C8 Pr1 69.2(3) . 2_566 ? C7 C8 Pr1 170.6(3) . 2_566 ? O5 C9 O4 120.8(4) . . ? O5 C9 C2 119.0(4) . . ? O4 C9 C2 120.1(4) . . ? O5 C9 Pr1 55.4(2) . 2_666 ? O4 C9 Pr1 65.5(2) . 2_666 ? C2 C9 Pr1 171.6(3) . 2_666 ? O6 C10 O7 119.8(5) . . ? O6 C10 C4 119.2(4) . . ? O7 C10 C4 121.0(4) . . ? O6 C10 Pr1 57.1(3) . 2_665 ? O7 C10 Pr1 63.6(3) . 2_665 ? C4 C10 Pr1 170.4(4) . 2_665 ? C1 O1 C7 118.0(4) . . ? C8 O2 Pr1 103.1(3) . 2_566 ? C8 O3 Pr1 153.7(3) . . ? C8 O3 Pr1 86.7(3) . 2_566 ? Pr1 O3 Pr1 119.10(13) . 2_566 ? C9 O4 Pr1 149.3(3) . . ? C9 O4 Pr1 90.0(3) . 2_666 ? Pr1 O4 Pr1 119.63(11) . 2_666 ? C9 O5 Pr1 100.7(3) . 2_666 ? C10 O6 Pr1 97.7(3) . 2_665 ? C10 O7 Pr1 90.9(3) . 2_665 ? Pr1 O8 H8A 109.8 . . ? Pr1 O8 H8B 135.3 . . ? H8A O8 H8B 112.2 . . ? Pr1 O9 H9A 123.6 . . ? Pr1 O9 H9B 120.0 . . ? H9A O9 H9B 109.5 . . ? H10A O10 H10B 119.9 . . ? H11A O11 H11B 118.5 . . ? 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 O1 C1 C2 C3 173.5(4) . . . . ? C6 C1 C2 C3 -2.6(8) . . . . ? O1 C1 C2 C9 -9.0(7) . . . . ? C6 C1 C2 C9 174.9(5) . . . . ? C1 C2 C3 C4 1.7(8) . . . . ? C9 C2 C3 C4 -175.8(5) . . . . ? C2 C3 C4 C5 0.2(7) . . . . ? C2 C3 C4 C10 179.0(5) . . . . ? C3 C4 C5 C6 -1.3(8) . . . . ? C10 C4 C5 C6 180.0(5) . . . . ? C4 C5 C6 C1 0.4(9) . . . . ? O1 C1 C6 C5 -174.1(5) . . . . ? C2 C1 C6 C5 1.6(8) . . . . ? O1 C7 C8 O2 155.9(4) . . . . ? O1 C7 C8 O3 -25.6(6) . . . . ? O1 C7 C8 Pr1 118(2) . . . 2_566 ? C3 C2 C9 O5 -49.4(7) . . . . ? C1 C2 C9 O5 133.0(5) . . . . ? C3 C2 C9 O4 126.6(5) . . . . ? C1 C2 C9 O4 -50.9(7) . . . . ? C3 C2 C9 Pr1 -4(3) . . . 2_666 ? C1 C2 C9 Pr1 179(2) . . . 2_666 ? C5 C4 C10 O6 170.0(5) . . . . ? C3 C4 C10 O6 -8.8(8) . . . . ? C5 C4 C10 O7 -10.8(8) . . . . ? C3 C4 C10 O7 170.5(5) . . . . ? C5 C4 C10 Pr1 105.4(19) . . . 2_665 ? C3 C4 C10 Pr1 -73(2) . . . 2_665 ? C6 C1 O1 C7 -14.8(7) . . . . ? C2 C1 O1 C7 169.5(4) . . . . ? C8 C7 O1 C1 -75.4(5) . . . . ? O3 C8 O2 Pr1 8.7(5) . . . 2_566 ? C7 C8 O2 Pr1 -172.9(4) . . . 2_566 ? O2 C8 O3 Pr1 161.3(5) . . . . ? C7 C8 O3 Pr1 -17.1(10) . . . . ? Pr1 C8 O3 Pr1 168.8(7) 2_566 . . . ? O2 C8 O3 Pr1 -7.5(5) . . . 2_566 ? C7 C8 O3 Pr1 174.1(4) . . . 2_566 ? O8 Pr1 O3 C8 -31.0(7) . . . . ? O6 Pr1 O3 C8 114.4(8) 2_665 . . . ? O4 Pr1 O3 C8 37.9(8) . . . . ? O5 Pr1 O3 C8 -93.1(8) 2_666 . . . ? O2 Pr1 O3 C8 -174.8(7) 2_566 . . . ? O9 Pr1 O3 C8 -101.5(8) . . . . ? O7 Pr1 O3 C8 107.9(7) 2_665 . . . ? O4 Pr1 O3 C8 -0.1(9) 2_666 . . . ? O3 Pr1 O3 C8 -167.2(9) 2_566 . . . ? C10 Pr1 O3 C8 108.9(8) 2_665 . . . ? C9 Pr1 O3 C8 -49.8(9) 2_666 . . . ? O8 Pr1 O3 Pr1 136.12(18) . . . 2_566 ? O6 Pr1 O3 Pr1 -78.39(16) 2_665 . . 2_566 ? O4 Pr1 O3 Pr1 -154.89(16) . . . 2_566 ? O5 Pr1 O3 Pr1 74.1(2) 2_666 . . 2_566 ? O2 Pr1 O3 Pr1 -7.59(19) 2_566 . . 2_566 ? O9 Pr1 O3 Pr1 65.72(16) . . . 2_566 ? O7 Pr1 O3 Pr1 -84.92(18) 2_665 . . 2_566 ? O4 Pr1 O3 Pr1 167.06(14) 2_666 . . 2_566 ? O3 Pr1 O3 Pr1 0.0 2_566 . . 2_566 ? C10 Pr1 O3 Pr1 -83.96(17) 2_665 . . 2_566 ? C9 Pr1 O3 Pr1 117.4(3) 2_666 . . 2_566 ? O5 C9 O4 Pr1 168.2(4) . . . . ? C2 C9 O4 Pr1 -7.8(10) . . . . ? Pr1 C9 O4 Pr1 165.2(7) 2_666 . . . ? O5 C9 O4 Pr1 2.9(5) . . . 2_666 ? C2 C9 O4 Pr1 -173.0(4) . . . 2_666 ? O3 Pr1 O4 C9 39.5(7) . . . . ? O8 Pr1 O4 C9 116.5(7) . . . . ? O6 Pr1 O4 C9 -31.4(7) 2_665 . . . ? O5 Pr1 O4 C9 -168.4(7) 2_666 . . . ? O2 Pr1 O4 C9 -86.0(7) 2_566 . . . ? O9 Pr1 O4 C9 114.6(7) . . . . ? O7 Pr1 O4 C9 -83.3(7) 2_665 . . . ? O4 Pr1 O4 C9 -162.9(8) 2_666 . . . ? O3 Pr1 O4 C9 -2.1(8) 2_566 . . . ? C10 Pr1 O4 C9 -56.2(7) 2_665 . . . ? C9 Pr1 O4 C9 -166.5(6) 2_666 . . . ? O3 Pr1 O4 Pr1 -157.52(16) . . . 2_666 ? O8 Pr1 O4 Pr1 -80.61(16) . . . 2_666 ? O6 Pr1 O4 Pr1 131.54(17) 2_665 . . 2_666 ? O5 Pr1 O4 Pr1 -5.5(2) 2_666 . . 2_666 ? O2 Pr1 O4 Pr1 76.9(2) 2_566 . . 2_666 ? O9 Pr1 O4 Pr1 -82.5(2) . . . 2_666 ? O7 Pr1 O4 Pr1 79.63(15) 2_665 . . 2_666 ? O4 Pr1 O4 Pr1 0.0 2_666 . . 2_666 ? O3 Pr1 O4 Pr1 160.86(14) 2_566 . . 2_666 ? C10 Pr1 O4 Pr1 106.71(18) 2_665 . . 2_666 ? C9 Pr1 O4 Pr1 -3.58(17) 2_666 . . 2_666 ? O4 C9 O5 Pr1 -3.2(6) . . . 2_666 ? C2 C9 O5 Pr1 172.8(4) . . . 2_666 ? O7 C10 O6 Pr1 11.0(5) . . . 2_665 ? C4 C10 O6 Pr1 -169.7(4) . . . 2_665 ? O6 C10 O7 Pr1 -10.3(5) . . . 2_665 ? C4 C10 O7 Pr1 170.4(4) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.942 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.145 _database_code_depnum_ccdc_archive 'CCDC 946978' ####################################################################### # # 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_p100325h _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 O25 Tb3' _chemical_formula_weight 1260.24 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1361(8) _cell_length_b 12.1778(10) _cell_length_c 14.8005(11) _cell_angle_alpha 68.768(7) _cell_angle_beta 84.392(6) _cell_angle_gamma 75.241(7) _cell_volume 1646.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1085 _cell_measurement_theta_min 2.5105 _cell_measurement_theta_max 28.7933 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 6.482 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.2941 _exptl_absorpt_correction_T_max 0.4431 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number 3908 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15193 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_unetI/netI 0.0359 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5777 _reflns_number_gt 5073 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR: the parameter to go anisotropic restraint to appointed atoms. SIMU: the parameter to set some atoms in limited range having the save shift parameters, and this parameter always is used with ISOR. ISOR 0.005 0.01 $C $O ISOR 0.005 0.01 C7 C3 C17 SIMU 0.005 0.01 1.7 $C $O FREE Tb2 C29 ; _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^)+(0.0292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5777 _refine_ls_number_parameters 517 _refine_ls_number_restraints 654 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0576 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 1.74593(2) -0.019022(19) 0.399736(15) 0.01310(7) Uani 1 1 d . . . Tb2 Tb 0.85932(2) 0.477951(19) 0.285631(15) 0.01310(7) Uani 1 1 d . . . Tb3 Tb 0.99211(2) 0.787881(19) 0.043502(15) 0.01076(6) Uani 1 1 d . . . C1 C 1.5240(4) 0.2559(4) 0.2354(3) 0.0157(9) Uani 1 1 d U . . C2 C 1.4172(4) 0.2300(4) 0.3028(3) 0.0144(9) Uani 1 1 d U . . C3 C 1.3008(4) 0.3245(4) 0.2962(3) 0.0119(9) Uani 1 1 d U . . H3 H 1.2304 0.3100 0.3409 0.014 Uiso 1 1 calc R . . C4 C 1.2872(4) 0.4382(4) 0.2256(3) 0.0135(8) Uani 1 1 d U . . C5 C 1.3934(5) 0.4611(4) 0.1603(3) 0.0190(10) Uani 1 1 d U . . H5 H 1.3851 0.5374 0.1126 0.023 Uiso 1 1 calc R . . C6 C 1.5115(5) 0.3721(4) 0.1650(3) 0.0198(10) Uani 1 1 d U . . H6 H 1.5826 0.3893 0.1216 0.024 Uiso 1 1 calc R . . C7 C 1.7466(4) 0.2002(4) 0.1692(3) 0.0141(9) Uani 1 1 d U . . H7A H 1.7808 0.2629 0.1784 0.017 Uiso 1 1 calc R . . H7B H 1.7077 0.2320 0.1049 0.017 Uiso 1 1 calc R . . C8 C 1.8611(4) 0.0907(4) 0.1788(3) 0.0143(9) Uani 1 1 d U . . C9 C 1.4183(4) 0.1096(4) 0.3814(3) 0.0139(9) Uani 1 1 d U . . C10 C 1.1579(4) 0.5336(4) 0.2141(3) 0.0141(9) Uani 1 1 d U . . C11 C 0.6986(5) 0.5166(4) 0.5072(3) 0.0195(9) Uani 1 1 d U . . C12 C 0.6560(5) 0.6426(4) 0.4562(3) 0.0180(9) Uani 1 1 d U . . C13 C 0.5385(4) 0.7084(4) 0.4887(3) 0.0176(9) Uani 1 1 d U . . H13 H 0.5091 0.7915 0.4560 0.021 Uiso 1 1 calc R . . C14 C 0.4659(5) 0.6517(4) 0.5683(3) 0.0163(9) Uani 1 1 d U . . C15 C 0.5140(5) 0.5273(4) 0.6193(3) 0.0195(10) Uani 1 1 d U . . H15 H 0.4669 0.4889 0.6739 0.023 Uiso 1 1 calc R . . C16 C 0.6295(5) 0.4617(4) 0.5894(3) 0.0222(10) Uani 1 1 d U . . H16 H 0.6614 0.3797 0.6248 0.027 Uiso 1 1 calc R . . C17 C 0.8820(5) 0.3382(5) 0.5400(4) 0.0311(11) Uani 1 1 d U . . H17A H 0.8171 0.2899 0.5728 0.037 Uiso 1 1 calc R . . H17B H 0.9246 0.3542 0.5883 0.037 Uiso 1 1 calc R . . C18 C 0.9882(5) 0.2694(4) 0.4905(3) 0.0198(9) Uani 1 1 d U . . C19 C 0.7273(5) 0.7115(4) 0.3714(3) 0.0181(9) Uani 1 1 d U . . C20 C 0.3421(5) 0.7251(4) 0.6007(3) 0.0177(9) Uani 1 1 d U . . C21 C 0.6736(4) 0.8275(4) -0.0495(3) 0.0141(8) Uani 1 1 d U . . C22 C 0.6215(4) 0.7652(4) 0.0398(3) 0.0142(8) Uani 1 1 d U . . C23 C 0.4801(4) 0.7995(4) 0.0539(3) 0.0155(9) Uani 1 1 d U . . H23 H 0.4407 0.7563 0.1108 0.019 Uiso 1 1 calc R . . C24 C 0.3972(4) 0.8970(4) -0.0157(3) 0.0133(8) Uani 1 1 d U . . C25 C 0.4547(4) 0.9574(4) -0.1021(3) 0.0159(9) Uani 1 1 d U . . H25 H 0.4005 1.0232 -0.1484 0.019 Uiso 1 1 calc R . . C26 C 0.5928(4) 0.9207(4) -0.1204(3) 0.0154(9) Uani 1 1 d U . . H26 H 0.6303 0.9586 -0.1800 0.018 Uiso 1 1 calc R . . C27 C 0.8520(5) 0.7328(5) -0.1344(3) 0.0218(10) Uani 1 1 d U . . H27A H 0.8456 0.7910 -0.2001 0.026 Uiso 1 1 calc R . . H27B H 0.7907 0.6809 -0.1281 0.026 Uiso 1 1 calc R . . C28 C 0.9983(5) 0.6567(4) -0.1141(3) 0.0164(9) Uani 1 1 d U . . C29 C 0.7090(5) 0.6680(4) 0.1190(3) 0.0160(9) Uani 1 1 d U . . C30 C 0.2454(4) 0.9382(4) 0.0027(3) 0.0136(8) Uani 1 1 d U . . O1 O 1.6430(3) 0.1663(3) 0.2414(2) 0.0160(7) Uani 1 1 d U . . O2 O 1.9531(3) 0.0988(3) 0.1157(2) 0.0156(7) Uani 1 1 d U . . O3 O 1.8576(3) -0.0044(3) 0.2491(2) 0.0209(7) Uani 1 1 d U . . O4 O 1.5141(3) 0.0197(3) 0.3841(2) 0.0153(7) Uani 1 1 d U . . O5 O 1.3190(3) 0.1042(3) 0.4399(2) 0.0171(7) Uani 1 1 d U . . O6 O 1.0672(3) 0.5189(3) 0.2800(2) 0.0180(7) Uani 1 1 d U . . O7 O 1.1452(3) 0.6229(3) 0.1364(2) 0.0192(7) Uani 1 1 d U . . O8 O 0.8117(3) 0.4508(3) 0.4708(2) 0.0205(7) Uani 1 1 d U . . O9 O 1.0615(3) 0.1747(3) 0.5466(2) 0.0313(9) Uani 1 1 d U . . O10 O 0.9914(3) 0.3032(3) 0.4002(2) 0.0248(8) Uani 1 1 d U . . O11 O 0.8018(3) 0.6563(3) 0.3191(2) 0.0228(8) Uani 1 1 d U . . O12 O 0.7146(3) 0.8225(3) 0.3534(2) 0.0238(8) Uani 1 1 d U . . O13 O 0.3215(3) 0.8399(3) 0.5638(2) 0.0201(7) Uani 1 1 d U . . O14 O 0.2664(3) 0.6691(3) 0.6646(2) 0.0226(7) Uani 1 1 d U . . O15 O 0.8139(3) 0.7953(3) -0.0665(2) 0.0144(6) Uani 1 1 d U . . O16 O 1.0493(3) 0.6090(3) -0.1757(2) 0.0201(7) Uani 1 1 d U . . O17 O 1.0560(3) 0.6477(3) -0.0409(2) 0.0174(7) Uani 1 1 d U . . O18 O 0.8365(3) 0.6635(3) 0.1249(2) 0.0146(7) Uani 1 1 d U . . O19 O 0.6582(3) 0.5884(3) 0.1830(2) 0.0233(8) Uani 1 1 d U . . O20 O 0.1841(3) 0.8587(3) 0.0554(2) 0.0194(7) Uani 1 1 d U . . O21 O 0.18915(18) 1.04756(17) -0.03791(14) 0.0149(7) Uani 1 1 d U . . O22 O 1.93749(18) 0.07283(17) 0.38605(14) 0.0468(12) Uani 1 1 d RU . . H22A H 2.0057 0.0279 0.3673 0.056 Uiso 1 1 d R . . H22B H 1.9624 0.1341 0.3884 0.056 Uiso 1 1 d R . . O23 O 0.97070(18) 0.79695(17) 0.20493(14) 0.0169(7) Uani 1 1 d RU . . H23A H 0.9256 0.7486 0.2431 0.020 Uiso 1 1 d R . . H23B H 0.9321 0.8680 0.2045 0.020 Uiso 1 1 d R . . O24 O 0.1949(4) 0.9833(4) 0.3372(3) 0.0635(14) Uani 1 1 d U . . H24A H 0.2368 0.9041 0.3527 0.095 Uiso 1 1 d R . . H24B H 0.2226 1.0104 0.3788 0.095 Uiso 1 1 d R . . O25 O 0.2273(5) 0.8111(4) 0.2550(3) 0.0591(13) Uani 1 1 d U . . H25A H 0.1486 0.7865 0.2637 0.089 Uiso 1 1 d R . . H25B H 0.2086 0.8899 0.2175 0.089 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01265(12) 0.01144(12) 0.01193(12) -0.00296(9) 0.00172(9) 0.00044(9) Tb2 0.01301(12) 0.01172(12) 0.01308(12) -0.00376(9) 0.00221(9) -0.00208(9) Tb3 0.00889(12) 0.01095(12) 0.01040(12) -0.00234(9) 0.00090(8) -0.00128(9) C1 0.0129(18) 0.0154(18) 0.0176(18) -0.0052(15) 0.0007(15) -0.0022(15) C2 0.0128(18) 0.0166(18) 0.0142(18) -0.0053(15) -0.0022(15) -0.0034(15) C3 0.0103(17) 0.0150(18) 0.0130(17) -0.0070(15) -0.0015(15) -0.0037(15) C4 0.0119(17) 0.0131(17) 0.0138(18) -0.0038(15) -0.0015(15) -0.0010(15) C5 0.017(2) 0.0160(19) 0.018(2) -0.0007(16) -0.0018(17) -0.0009(16) C6 0.017(2) 0.018(2) 0.019(2) -0.0014(17) 0.0015(17) -0.0025(17) C7 0.0117(17) 0.0175(18) 0.0140(18) -0.0052(15) 0.0040(15) -0.0071(15) C8 0.0167(18) 0.0165(18) 0.0125(18) -0.0078(15) 0.0021(15) -0.0058(15) C9 0.0126(18) 0.0153(18) 0.0141(18) -0.0063(15) 0.0006(15) -0.0024(15) C10 0.0161(18) 0.0111(17) 0.0164(18) -0.0053(15) -0.0034(16) -0.0034(15) C11 0.0181(19) 0.0210(19) 0.0200(18) -0.0090(16) 0.0001(16) -0.0032(16) C12 0.0190(18) 0.0190(18) 0.0188(18) -0.0097(15) -0.0002(16) -0.0047(16) C13 0.0163(19) 0.0183(19) 0.019(2) -0.0074(16) 0.0004(16) -0.0054(16) C14 0.0157(18) 0.0186(18) 0.0170(18) -0.0088(15) 0.0000(15) -0.0040(15) C15 0.020(2) 0.020(2) 0.018(2) -0.0076(17) 0.0027(17) -0.0037(17) C16 0.021(2) 0.020(2) 0.023(2) -0.0058(17) -0.0013(17) -0.0031(17) C17 0.030(2) 0.030(2) 0.023(2) -0.0068(17) -0.0031(17) 0.0064(18) C18 0.0166(18) 0.0204(19) 0.0191(18) -0.0058(16) -0.0008(16) -0.0001(16) C19 0.0199(18) 0.0175(18) 0.0184(18) -0.0082(15) 0.0025(16) -0.0051(16) C20 0.0152(18) 0.0207(18) 0.0203(18) -0.0102(16) -0.0004(16) -0.0052(16) C21 0.0107(17) 0.0163(18) 0.0172(18) -0.0076(15) -0.0014(15) -0.0033(15) C22 0.0135(17) 0.0137(17) 0.0163(18) -0.0058(15) -0.0004(15) -0.0039(15) C23 0.0153(19) 0.0156(19) 0.0157(19) -0.0043(16) 0.0021(16) -0.0068(16) C24 0.0109(17) 0.0155(18) 0.0157(18) -0.0083(15) -0.0013(15) -0.0023(15) C25 0.0131(18) 0.0159(19) 0.0185(19) -0.0051(16) -0.0043(16) -0.0030(16) C26 0.0132(19) 0.0187(19) 0.0146(19) -0.0052(16) -0.0005(16) -0.0054(16) C27 0.019(2) 0.029(2) 0.019(2) -0.0125(17) 0.0003(17) -0.0023(17) C28 0.0159(18) 0.0174(18) 0.0172(18) -0.0067(15) 0.0043(16) -0.0068(15) C29 0.0149(18) 0.0155(18) 0.0177(18) -0.0051(15) 0.0010(15) -0.0055(15) C30 0.0117(17) 0.0164(18) 0.0131(18) -0.0072(15) -0.0017(15) -0.0004(15) O1 0.0113(14) 0.0136(15) 0.0185(15) -0.0031(12) 0.0056(12) -0.0008(12) O2 0.0136(15) 0.0178(16) 0.0121(15) -0.0031(13) 0.0043(12) -0.0026(13) O3 0.0225(17) 0.0175(16) 0.0158(16) -0.0023(13) 0.0089(13) -0.0011(14) O4 0.0144(15) 0.0126(15) 0.0160(16) -0.0041(13) -0.0006(12) 0.0005(12) O5 0.0188(16) 0.0138(15) 0.0140(15) -0.0022(13) 0.0049(13) -0.0016(13) O6 0.0128(15) 0.0161(16) 0.0228(17) -0.0064(13) 0.0019(13) -0.0010(13) O7 0.0188(16) 0.0163(16) 0.0178(16) -0.0034(13) -0.0002(13) 0.0001(13) O8 0.0216(16) 0.0188(15) 0.0169(15) -0.0061(13) 0.0007(13) 0.0018(13) O9 0.0234(18) 0.0320(19) 0.0231(18) -0.0030(15) 0.0032(14) 0.0087(15) O10 0.0251(17) 0.0222(17) 0.0176(17) -0.0027(14) 0.0003(14) 0.0045(14) O11 0.0286(18) 0.0173(16) 0.0216(17) -0.0081(14) 0.0096(14) -0.0055(14) O12 0.0253(17) 0.0179(16) 0.0286(18) -0.0094(14) 0.0113(14) -0.0084(14) O13 0.0194(16) 0.0160(16) 0.0235(17) -0.0084(14) 0.0038(14) -0.0009(13) O14 0.0218(17) 0.0243(17) 0.0236(17) -0.0083(14) 0.0067(14) -0.0114(14) O15 0.0100(14) 0.0190(15) 0.0147(14) -0.0077(12) -0.0004(12) -0.0015(12) O16 0.0228(17) 0.0223(17) 0.0178(16) -0.0112(14) 0.0065(13) -0.0063(14) O17 0.0163(16) 0.0174(16) 0.0176(16) -0.0069(13) 0.0001(13) -0.0011(13) O18 0.0106(15) 0.0145(15) 0.0165(15) -0.0034(13) 0.0004(12) -0.0021(12) O19 0.0186(16) 0.0199(16) 0.0242(17) 0.0025(14) 0.0002(14) -0.0074(14) O20 0.0140(15) 0.0231(17) 0.0188(16) -0.0021(14) 0.0028(13) -0.0091(13) O21 0.0122(15) 0.0133(15) 0.0179(16) -0.0068(13) -0.0021(12) 0.0018(12) O22 0.026(2) 0.039(2) 0.092(3) -0.043(2) 0.010(2) -0.0102(18) O23 0.0207(17) 0.0110(16) 0.0175(17) -0.0052(14) 0.0022(14) -0.0016(14) O24 0.054(3) 0.072(3) 0.076(3) -0.039(3) 0.001(3) -0.016(3) O25 0.059(3) 0.060(3) 0.050(3) -0.011(2) -0.003(2) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O4 2.294(3) . ? Tb1 O9 2.315(3) 2_856 ? Tb1 O5 2.325(3) 2_856 ? Tb1 O13 2.353(3) 2_766 ? Tb1 O3 2.368(3) . ? Tb1 O12 2.369(3) 1_645 ? Tb1 O22 2.4347(19) . ? Tb1 O1 2.669(3) . ? Tb2 O16 2.254(3) 2_765 ? Tb2 O6 2.273(3) . ? Tb2 O11 2.320(3) . ? Tb2 O14 2.323(3) 2_666 ? Tb2 O10 2.361(3) . ? Tb2 O19 2.450(3) . ? Tb2 O18 2.601(3) . ? Tb2 O8 2.650(3) . ? Tb3 O7 2.272(3) . ? Tb3 O21 2.3307(18) 2_675 ? Tb3 O2 2.354(3) 2_865 ? Tb3 O20 2.365(3) 1_655 ? Tb3 O17 2.392(3) . ? Tb3 O18 2.399(3) . ? Tb3 O23 2.4177(18) . ? Tb3 O15 2.512(3) . ? C1 O1 1.391(5) . ? C1 C6 1.404(6) . ? C1 C2 1.415(6) . ? C2 C3 1.406(6) . ? C2 C9 1.504(6) . ? C3 C4 1.382(6) . ? C3 H3 0.9300 . ? C4 C5 1.388(6) . ? C4 C10 1.490(6) . ? C5 C6 1.383(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.447(5) . ? C7 C8 1.501(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.250(5) . ? C8 O3 1.251(5) . ? C9 O4 1.257(5) . ? C9 O5 1.260(5) . ? C10 O7 1.254(5) . ? C10 O6 1.270(5) . ? C11 C16 1.378(7) . ? C11 O8 1.403(5) . ? C11 C12 1.413(6) . ? C12 C13 1.405(6) . ? C12 C19 1.474(6) . ? C13 C14 1.381(6) . ? C13 H13 0.9300 . ? C14 C15 1.403(6) . ? C14 C20 1.492(6) . ? C15 C16 1.373(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O8 1.436(6) . ? C17 C18 1.493(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O10 1.247(5) . ? C18 O9 1.250(6) . ? C19 O12 1.253(5) . ? C19 O11 1.276(5) . ? C20 O14 1.266(5) . ? C20 O13 1.272(5) . ? C21 C26 1.375(6) . ? C21 C22 1.393(6) . ? C21 O15 1.400(5) . ? C22 C23 1.404(6) . ? C22 C29 1.493(6) . ? C23 C24 1.397(6) . ? C23 H23 0.9300 . ? C24 C25 1.382(6) . ? C24 C30 1.522(6) . ? C25 C26 1.388(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 O15 1.437(5) . ? C27 C28 1.527(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O17 1.238(5) . ? C28 O16 1.254(5) . ? C29 O19 1.262(5) . ? C29 O18 1.290(5) . ? C30 O21 1.249(5) . ? C30 O20 1.264(5) . ? O2 Tb3 2.354(3) 2_865 ? O5 Tb1 2.325(3) 2_856 ? O9 Tb1 2.315(3) 2_856 ? O12 Tb1 2.369(3) 1_465 ? O13 Tb1 2.353(3) 2_766 ? O14 Tb2 2.323(3) 2_666 ? O16 Tb2 2.255(3) 2_765 ? O20 Tb3 2.365(3) 1_455 ? O21 Tb3 2.3307(18) 2_675 ? O22 H22A 0.8567 . ? O22 H22B 0.8583 . ? O23 H23A 0.8491 . ? O23 H23B 0.8516 . ? O24 H24A 0.9016 . ? O24 H24B 0.8921 . ? O25 H25A 0.9036 . ? O25 H25B 0.8981 . ? 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 Tb1 O9 142.74(12) . 2_856 ? O4 Tb1 O5 79.06(11) . 2_856 ? O9 Tb1 O5 80.99(11) 2_856 2_856 ? O4 Tb1 O13 80.18(11) . 2_766 ? O9 Tb1 O13 127.51(12) 2_856 2_766 ? O5 Tb1 O13 81.98(11) 2_856 2_766 ? O4 Tb1 O3 110.91(11) . . ? O9 Tb1 O3 80.70(11) 2_856 . ? O5 Tb1 O3 159.50(11) 2_856 . ? O13 Tb1 O3 116.76(11) 2_766 . ? O4 Tb1 O12 75.89(11) . 1_645 ? O9 Tb1 O12 74.71(13) 2_856 1_645 ? O5 Tb1 O12 94.59(11) 2_856 1_645 ? O13 Tb1 O12 156.04(11) 2_766 1_645 ? O3 Tb1 O12 71.68(11) . 1_645 ? O4 Tb1 O22 144.59(9) . . ? O9 Tb1 O22 72.44(11) 2_856 . ? O5 Tb1 O22 111.98(9) 2_856 . ? O13 Tb1 O22 68.90(9) 2_766 . ? O3 Tb1 O22 70.79(9) . . ? O12 Tb1 O22 133.13(9) 1_645 . ? O4 Tb1 O1 65.34(10) . . ? O9 Tb1 O1 141.26(10) 2_856 . ? O5 Tb1 O1 137.74(10) 2_856 . ? O13 Tb1 O1 70.57(10) 2_766 . ? O3 Tb1 O1 61.19(10) . . ? O12 Tb1 O1 97.88(11) 1_645 . ? O22 Tb1 O1 87.76(8) . . ? O16 Tb2 O6 84.37(11) 2_765 . ? O16 Tb2 O11 145.49(11) 2_765 . ? O6 Tb2 O11 78.66(11) . . ? O16 Tb2 O14 84.76(11) 2_765 2_666 ? O6 Tb2 O14 146.70(11) . 2_666 ? O11 Tb2 O14 124.67(11) . 2_666 ? O16 Tb2 O10 85.54(11) 2_765 . ? O6 Tb2 O10 75.36(12) . . ? O11 Tb2 O10 118.16(12) . . ? O14 Tb2 O10 72.48(12) 2_666 . ? O16 Tb2 O19 89.97(11) 2_765 . ? O6 Tb2 O19 130.91(11) . . ? O11 Tb2 O19 79.21(12) . . ? O14 Tb2 O19 80.40(11) 2_666 . ? O10 Tb2 O19 152.80(11) . . ? O16 Tb2 O18 77.56(10) 2_765 . ? O6 Tb2 O18 79.92(10) . . ? O11 Tb2 O18 70.05(10) . . ? O14 Tb2 O18 127.85(11) 2_666 . ? O10 Tb2 O18 151.24(10) . . ? O19 Tb2 O18 51.37(10) . . ? O16 Tb2 O8 147.48(11) 2_765 . ? O6 Tb2 O8 95.47(10) . . ? O11 Tb2 O8 64.77(10) . . ? O14 Tb2 O8 77.68(11) 2_666 . ? O10 Tb2 O8 63.23(10) . . ? O19 Tb2 O8 113.38(10) . . ? O18 Tb2 O8 134.57(9) . . ? O7 Tb3 O21 147.39(9) . 2_675 ? O7 Tb3 O2 121.19(11) . 2_865 ? O21 Tb3 O2 87.43(9) 2_675 2_865 ? O7 Tb3 O20 74.20(11) . 1_655 ? O21 Tb3 O20 102.76(9) 2_675 1_655 ? O2 Tb3 O20 73.56(11) 2_865 1_655 ? O7 Tb3 O17 72.12(11) . . ? O21 Tb3 O17 136.07(9) 2_675 . ? O2 Tb3 O17 74.04(10) 2_865 . ? O20 Tb3 O17 109.21(10) 1_655 . ? O7 Tb3 O18 81.55(11) . . ? O21 Tb3 O18 86.08(8) 2_675 . ? O2 Tb3 O18 138.79(10) 2_865 . ? O20 Tb3 O18 147.37(10) 1_655 . ? O17 Tb3 O18 82.94(10) . . ? O7 Tb3 O23 73.83(9) . . ? O21 Tb3 O23 73.90(7) 2_675 . ? O2 Tb3 O23 140.27(9) 2_865 . ? O20 Tb3 O23 76.82(9) 1_655 . ? O17 Tb3 O23 141.93(9) . . ? O18 Tb3 O23 75.67(8) . . ? O7 Tb3 O15 128.11(11) . . ? O21 Tb3 O15 72.17(8) 2_675 . ? O2 Tb3 O15 72.55(10) 2_865 . ? O20 Tb3 O15 145.90(10) 1_655 . ? O17 Tb3 O15 64.40(10) . . ? O18 Tb3 O15 66.72(10) . . ? O23 Tb3 O15 130.20(8) . . ? O1 C1 C6 120.3(4) . . ? O1 C1 C2 119.4(4) . . ? C6 C1 C2 120.3(4) . . ? C3 C2 C1 117.4(4) . . ? C3 C2 C9 117.2(4) . . ? C1 C2 C9 125.3(4) . . ? C4 C3 C2 122.3(4) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 119.0(4) . . ? C3 C4 C10 121.5(4) . . ? C5 C4 C10 119.4(4) . . ? C6 C5 C4 121.0(4) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 119.9(4) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? O1 C7 C8 109.2(3) . . ? O1 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O1 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? O2 C8 O3 123.7(4) . . ? O2 C8 C7 118.5(4) . . ? O3 C8 C7 117.8(4) . . ? O4 C9 O5 123.4(4) . . ? O4 C9 C2 119.3(4) . . ? O5 C9 C2 117.3(4) . . ? O7 C10 O6 124.3(4) . . ? O7 C10 C4 116.2(4) . . ? O6 C10 C4 119.4(4) . . ? C16 C11 O8 121.9(4) . . ? C16 C11 C12 120.3(4) . . ? O8 C11 C12 117.8(4) . . ? C13 C12 C11 118.4(4) . . ? C13 C12 C19 116.9(4) . . ? C11 C12 C19 124.7(4) . . ? C14 C13 C12 120.9(4) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 119.1(4) . . ? C13 C14 C20 119.3(4) . . ? C15 C14 C20 121.6(4) . . ? C16 C15 C14 120.8(5) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C11 120.3(5) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? O8 C17 C18 110.4(4) . . ? O8 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? O8 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? O10 C18 O9 125.5(4) . . ? O10 C18 C17 119.9(4) . . ? O9 C18 C17 114.4(4) . . ? O12 C19 O11 121.7(4) . . ? O12 C19 C12 119.2(4) . . ? O11 C19 C12 119.1(4) . . ? O14 C20 O13 124.5(4) . . ? O14 C20 C14 117.9(4) . . ? O13 C20 C14 117.6(4) . . ? C26 C21 C22 122.5(4) . . ? C26 C21 O15 118.9(4) . . ? C22 C21 O15 118.5(4) . . ? C21 C22 C23 116.9(4) . . ? C21 C22 C29 123.0(4) . . ? C23 C22 C29 120.1(4) . . ? C24 C23 C22 121.4(4) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C25 C24 C23 119.2(4) . . ? C25 C24 C30 119.7(4) . . ? C23 C24 C30 121.1(4) . . ? C24 C25 C26 120.5(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C21 C26 C25 119.3(4) . . ? C21 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? O15 C27 C28 109.1(4) . . ? O15 C27 H27A 109.9 . . ? C28 C27 H27A 109.9 . . ? O15 C27 H27B 109.9 . . ? C28 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? O17 C28 O16 125.9(4) . . ? O17 C28 C27 118.9(4) . . ? O16 C28 C27 115.2(4) . . ? O19 C29 O18 118.5(4) . . ? O19 C29 C22 120.0(4) . . ? O18 C29 C22 121.5(4) . . ? O21 C30 O20 124.5(4) . . ? O21 C30 C24 117.7(4) . . ? O20 C30 C24 117.7(4) . . ? C1 O1 C7 115.8(3) . . ? C1 O1 Tb1 127.0(2) . . ? C7 O1 Tb1 112.5(2) . . ? C8 O2 Tb3 144.0(3) . 2_865 ? C8 O3 Tb1 126.8(3) . . ? C9 O4 Tb1 133.0(3) . . ? C9 O5 Tb1 144.7(3) . 2_856 ? C10 O6 Tb2 132.0(3) . . ? C10 O7 Tb3 143.2(3) . . ? C11 O8 C17 115.5(4) . . ? C11 O8 Tb2 125.5(3) . . ? C17 O8 Tb2 116.2(2) . . ? C18 O9 Tb1 157.7(3) . 2_856 ? C18 O10 Tb2 129.3(3) . . ? C19 O11 Tb2 144.7(3) . . ? C19 O12 Tb1 149.7(3) . 1_465 ? C20 O13 Tb1 143.5(3) . 2_766 ? C20 O14 Tb2 148.1(3) . 2_666 ? C21 O15 C27 115.0(3) . . ? C21 O15 Tb3 123.5(2) . . ? C27 O15 Tb3 119.2(2) . . ? C28 O16 Tb2 179.6(3) . 2_765 ? C28 O17 Tb3 124.6(3) . . ? C29 O18 Tb3 136.9(3) . . ? C29 O18 Tb2 91.1(3) . . ? Tb3 O18 Tb2 131.22(12) . . ? C29 O19 Tb2 99.0(3) . . ? C30 O20 Tb3 137.5(3) . 1_455 ? C30 O21 Tb3 148.7(2) . 2_675 ? Tb1 O22 H22A 106.0 . . ? Tb1 O22 H22B 145.3 . . ? H22A O22 H22B 108.4 . . ? Tb3 O23 H23A 112.9 . . ? Tb3 O23 H23B 111.7 . . ? H23A O23 H23B 107.6 . . ? H24A O24 H24B 107.9 . . ? H25A O25 H25B 107.3 . . ? 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 O1 C1 C2 C3 177.8(4) . . . . ? C6 C1 C2 C3 -0.2(6) . . . . ? O1 C1 C2 C9 -2.0(7) . . . . ? C6 C1 C2 C9 -179.9(4) . . . . ? C1 C2 C3 C4 1.6(6) . . . . ? C9 C2 C3 C4 -178.6(4) . . . . ? C2 C3 C4 C5 -1.6(6) . . . . ? C2 C3 C4 C10 174.2(4) . . . . ? C3 C4 C5 C6 0.0(7) . . . . ? C10 C4 C5 C6 -175.8(4) . . . . ? C4 C5 C6 C1 1.4(7) . . . . ? O1 C1 C6 C5 -179.2(4) . . . . ? C2 C1 C6 C5 -1.3(7) . . . . ? O1 C7 C8 O2 172.0(4) . . . . ? O1 C7 C8 O3 -6.7(5) . . . . ? C3 C2 C9 O4 173.0(4) . . . . ? C1 C2 C9 O4 -7.2(7) . . . . ? C3 C2 C9 O5 -4.7(6) . . . . ? C1 C2 C9 O5 175.1(4) . . . . ? C3 C4 C10 O7 -165.0(4) . . . . ? C5 C4 C10 O7 10.7(6) . . . . ? C3 C4 C10 O6 12.8(6) . . . . ? C5 C4 C10 O6 -171.5(4) . . . . ? C16 C11 C12 C13 -3.1(7) . . . . ? O8 C11 C12 C13 176.5(4) . . . . ? C16 C11 C12 C19 176.0(4) . . . . ? O8 C11 C12 C19 -4.4(7) . . . . ? C11 C12 C13 C14 -0.1(7) . . . . ? C19 C12 C13 C14 -179.3(4) . . . . ? C12 C13 C14 C15 2.4(7) . . . . ? C12 C13 C14 C20 179.6(4) . . . . ? C13 C14 C15 C16 -1.6(7) . . . . ? C20 C14 C15 C16 -178.8(4) . . . . ? C14 C15 C16 C11 -1.6(7) . . . . ? O8 C11 C16 C15 -175.7(4) . . . . ? C12 C11 C16 C15 4.0(7) . . . . ? O8 C17 C18 O10 -10.7(7) . . . . ? O8 C17 C18 O9 174.6(4) . . . . ? C13 C12 C19 O12 25.0(7) . . . . ? C11 C12 C19 O12 -154.1(5) . . . . ? C13 C12 C19 O11 -155.9(4) . . . . ? C11 C12 C19 O11 25.0(7) . . . . ? C13 C14 C20 O14 170.0(4) . . . . ? C15 C14 C20 O14 -12.9(7) . . . . ? C13 C14 C20 O13 -11.6(6) . . . . ? C15 C14 C20 O13 165.5(4) . . . . ? C26 C21 C22 C23 1.8(6) . . . . ? O15 C21 C22 C23 -179.5(4) . . . . ? C26 C21 C22 C29 -177.0(4) . . . . ? O15 C21 C22 C29 1.7(6) . . . . ? C21 C22 C23 C24 -4.4(6) . . . . ? C29 C22 C23 C24 174.5(4) . . . . ? C22 C23 C24 C25 3.0(6) . . . . ? C22 C23 C24 C30 -176.4(4) . . . . ? C23 C24 C25 C26 1.0(6) . . . . ? C30 C24 C25 C26 -179.6(4) . . . . ? C22 C21 C26 C25 2.1(7) . . . . ? O15 C21 C26 C25 -176.6(4) . . . . ? C24 C25 C26 C21 -3.5(7) . . . . ? O15 C27 C28 O17 7.6(6) . . . . ? O15 C27 C28 O16 -171.9(4) . . . . ? C21 C22 C29 O19 -156.2(4) . . . . ? C23 C22 C29 O19 25.0(6) . . . . ? C21 C22 C29 O18 24.7(7) . . . . ? C23 C22 C29 O18 -154.1(4) . . . . ? C25 C24 C30 O21 -28.7(6) . . . . ? C23 C24 C30 O21 150.8(4) . . . . ? C25 C24 C30 O20 149.1(4) . . . . ? C23 C24 C30 O20 -31.5(6) . . . . ? C6 C1 O1 C7 -2.4(6) . . . . ? C2 C1 O1 C7 179.6(4) . . . . ? C6 C1 O1 Tb1 151.2(3) . . . . ? C2 C1 O1 Tb1 -26.8(5) . . . . ? C8 C7 O1 C1 -174.0(3) . . . . ? C8 C7 O1 Tb1 28.7(4) . . . . ? O4 Tb1 O1 C1 42.3(3) . . . . ? O9 Tb1 O1 C1 -171.9(3) 2_856 . . . ? O5 Tb1 O1 C1 7.0(4) 2_856 . . . ? O13 Tb1 O1 C1 -45.6(3) 2_766 . . . ? O3 Tb1 O1 C1 176.8(3) . . . . ? O12 Tb1 O1 C1 112.8(3) 1_645 . . . ? O22 Tb1 O1 C1 -114.0(3) . . . . ? O4 Tb1 O1 C7 -163.4(3) . . . . ? O9 Tb1 O1 C7 -17.6(3) 2_856 . . . ? O5 Tb1 O1 C7 161.3(2) 2_856 . . . ? O13 Tb1 O1 C7 108.7(3) 2_766 . . . ? O3 Tb1 O1 C7 -28.9(2) . . . . ? O12 Tb1 O1 C7 -92.9(3) 1_645 . . . ? O22 Tb1 O1 C7 40.3(2) . . . . ? O3 C8 O2 Tb3 159.5(3) . . . 2_865 ? C7 C8 O2 Tb3 -19.2(7) . . . 2_865 ? O2 C8 O3 Tb1 155.7(3) . . . . ? C7 C8 O3 Tb1 -25.5(5) . . . . ? O4 Tb1 O3 C8 74.0(4) . . . . ? O9 Tb1 O3 C8 -142.8(4) 2_856 . . . ? O5 Tb1 O3 C8 -169.8(3) 2_856 . . . ? O13 Tb1 O3 C8 -15.3(4) 2_766 . . . ? O12 Tb1 O3 C8 140.4(4) 1_645 . . . ? O22 Tb1 O3 C8 -68.2(4) . . . . ? O1 Tb1 O3 C8 30.1(3) . . . . ? O5 C9 O4 Tb1 -122.4(4) . . . . ? C2 C9 O4 Tb1 60.1(5) . . . . ? O9 Tb1 O4 C9 153.2(4) 2_856 . . . ? O5 Tb1 O4 C9 94.4(4) 2_856 . . . ? O13 Tb1 O4 C9 10.8(4) 2_766 . . . ? O3 Tb1 O4 C9 -104.3(4) . . . . ? O12 Tb1 O4 C9 -168.0(4) 1_645 . . . ? O22 Tb1 O4 C9 -18.3(5) . . . . ? O1 Tb1 O4 C9 -62.3(4) . . . . ? O4 C9 O5 Tb1 39.0(7) . . . 2_856 ? C2 C9 O5 Tb1 -143.4(4) . . . 2_856 ? O7 C10 O6 Tb2 69.3(6) . . . . ? C4 C10 O6 Tb2 -108.3(4) . . . . ? O16 Tb2 O6 C10 26.7(4) 2_765 . . . ? O11 Tb2 O6 C10 -123.1(4) . . . . ? O14 Tb2 O6 C10 98.2(4) 2_666 . . . ? O10 Tb2 O6 C10 113.6(4) . . . . ? O19 Tb2 O6 C10 -58.3(4) . . . . ? O18 Tb2 O6 C10 -51.6(4) . . . . ? O8 Tb2 O6 C10 174.1(4) . . . . ? O6 C10 O7 Tb3 -10.3(8) . . . . ? C4 C10 O7 Tb3 167.4(3) . . . . ? O21 Tb3 O7 C10 42.4(6) 2_675 . . . ? O2 Tb3 O7 C10 -169.5(4) 2_865 . . . ? O20 Tb3 O7 C10 131.5(5) 1_655 . . . ? O17 Tb3 O7 C10 -111.7(5) . . . . ? O18 Tb3 O7 C10 -26.5(5) . . . . ? O23 Tb3 O7 C10 50.9(5) . . . . ? O15 Tb3 O7 C10 -77.9(5) . . . . ? C16 C11 O8 C17 -22.7(6) . . . . ? C12 C11 O8 C17 157.7(4) . . . . ? C16 C11 O8 Tb2 137.4(4) . . . . ? C12 C11 O8 Tb2 -42.2(5) . . . . ? C18 C17 O8 C11 172.7(4) . . . . ? C18 C17 O8 Tb2 10.6(5) . . . . ? O16 Tb2 O8 C11 -148.9(3) 2_765 . . . ? O6 Tb2 O8 C11 123.0(3) . . . . ? O11 Tb2 O8 C11 48.3(3) . . . . ? O14 Tb2 O8 C11 -90.0(3) 2_666 . . . ? O10 Tb2 O8 C11 -166.5(4) . . . . ? O19 Tb2 O8 C11 -16.3(4) . . . . ? O18 Tb2 O8 C11 41.7(4) . . . . ? O16 Tb2 O8 C17 11.1(4) 2_765 . . . ? O6 Tb2 O8 C17 -77.0(3) . . . . ? O11 Tb2 O8 C17 -151.7(4) . . . . ? O14 Tb2 O8 C17 70.0(3) 2_666 . . . ? O10 Tb2 O8 C17 -6.4(3) . . . . ? O19 Tb2 O8 C17 143.7(3) . . . . ? O18 Tb2 O8 C17 -158.2(3) . . . . ? O10 C18 O9 Tb1 33.4(13) . . . 2_856 ? C17 C18 O9 Tb1 -152.1(7) . . . 2_856 ? O9 C18 O10 Tb2 179.6(4) . . . . ? C17 C18 O10 Tb2 5.4(7) . . . . ? O16 Tb2 O10 C18 -170.1(4) 2_765 . . . ? O6 Tb2 O10 C18 104.6(4) . . . . ? O11 Tb2 O10 C18 36.3(4) . . . . ? O14 Tb2 O10 C18 -84.2(4) 2_666 . . . ? O19 Tb2 O10 C18 -88.9(5) . . . . ? O18 Tb2 O10 C18 136.1(4) . . . . ? O8 Tb2 O10 C18 0.5(4) . . . . ? O12 C19 O11 Tb2 -168.5(3) . . . . ? C12 C19 O11 Tb2 12.5(8) . . . . ? O16 Tb2 O11 C19 159.1(5) 2_765 . . . ? O6 Tb2 O11 C19 -138.8(6) . . . . ? O14 Tb2 O11 C19 15.0(6) 2_666 . . . ? O10 Tb2 O11 C19 -72.4(6) . . . . ? O19 Tb2 O11 C19 85.2(6) . . . . ? O18 Tb2 O11 C19 137.9(6) . . . . ? O8 Tb2 O11 C19 -37.2(5) . . . . ? O11 C19 O12 Tb1 -116.6(6) . . . 1_465 ? C12 C19 O12 Tb1 62.4(8) . . . 1_465 ? O14 C20 O13 Tb1 40.9(8) . . . 2_766 ? C14 C20 O13 Tb1 -137.4(4) . . . 2_766 ? O13 C20 O14 Tb2 128.4(5) . . . 2_666 ? C14 C20 O14 Tb2 -53.3(8) . . . 2_666 ? C26 C21 O15 C27 -72.6(5) . . . . ? C22 C21 O15 C27 108.6(4) . . . . ? C26 C21 O15 Tb3 124.8(4) . . . . ? C22 C21 O15 Tb3 -53.9(5) . . . . ? C28 C27 O15 C21 -155.4(4) . . . . ? C28 C27 O15 Tb3 8.0(5) . . . . ? O7 Tb3 O15 C21 113.2(3) . . . . ? O21 Tb3 O15 C21 -37.5(3) 2_675 . . . ? O2 Tb3 O15 C21 -130.4(3) 2_865 . . . ? O20 Tb3 O15 C21 -124.0(3) 1_655 . . . ? O17 Tb3 O15 C21 149.3(3) . . . . ? O18 Tb3 O15 C21 56.0(3) . . . . ? O23 Tb3 O15 C21 11.7(3) . . . . ? O7 Tb3 O15 C27 -48.6(3) . . . . ? O21 Tb3 O15 C27 160.7(3) 2_675 . . . ? O2 Tb3 O15 C27 67.7(3) 2_865 . . . ? O20 Tb3 O15 C27 74.2(4) 1_655 . . . ? O17 Tb3 O15 C27 -12.5(3) . . . . ? O18 Tb3 O15 C27 -105.8(3) . . . . ? O23 Tb3 O15 C27 -150.1(3) . . . . ? O17 C28 O16 Tb2 79(47) . . . 2_765 ? C27 C28 O16 Tb2 -102(47) . . . 2_765 ? O16 C28 O17 Tb3 157.7(3) . . . . ? C27 C28 O17 Tb3 -21.7(6) . . . . ? O7 Tb3 O17 C28 169.4(4) . . . . ? O21 Tb3 O17 C28 9.2(4) 2_675 . . . ? O2 Tb3 O17 C28 -59.4(3) 2_865 . . . ? O20 Tb3 O17 C28 -125.1(3) 1_655 . . . ? O18 Tb3 O17 C28 86.0(3) . . . . ? O23 Tb3 O17 C28 141.8(3) . . . . ? O15 Tb3 O17 C28 18.5(3) . . . . ? O19 C29 O18 Tb3 -172.8(3) . . . . ? C22 C29 O18 Tb3 6.4(7) . . . . ? O19 C29 O18 Tb2 -2.4(4) . . . . ? C22 C29 O18 Tb2 176.8(4) . . . . ? O7 Tb3 O18 C29 -172.4(4) . . . . ? O21 Tb3 O18 C29 37.8(4) 2_675 . . . ? O2 Tb3 O18 C29 -43.7(4) 2_865 . . . ? O20 Tb3 O18 C29 145.5(4) 1_655 . . . ? O17 Tb3 O18 C29 -99.5(4) . . . . ? O23 Tb3 O18 C29 112.2(4) . . . . ? O15 Tb3 O18 C29 -34.4(4) . . . . ? O7 Tb3 O18 Tb2 20.45(15) . . . . ? O21 Tb3 O18 Tb2 -129.29(15) 2_675 . . . ? O2 Tb3 O18 Tb2 149.13(14) 2_865 . . . ? O20 Tb3 O18 Tb2 -21.6(3) 1_655 . . . ? O17 Tb3 O18 Tb2 93.32(16) . . . . ? O23 Tb3 O18 Tb2 -54.93(14) . . . . ? O15 Tb3 O18 Tb2 158.45(18) . . . . ? O16 Tb2 O18 C29 101.5(3) 2_765 . . . ? O6 Tb2 O18 C29 -172.1(3) . . . . ? O11 Tb2 O18 C29 -90.6(3) . . . . ? O14 Tb2 O18 C29 28.3(3) 2_666 . . . ? O10 Tb2 O18 C29 156.9(3) . . . . ? O19 Tb2 O18 C29 1.4(2) . . . . ? O8 Tb2 O18 C29 -84.4(3) . . . . ? O16 Tb2 O18 Tb3 -87.24(17) 2_765 . . . ? O6 Tb2 O18 Tb3 -0.85(15) . . . . ? O11 Tb2 O18 Tb3 80.64(17) . . . . ? O14 Tb2 O18 Tb3 -160.40(14) 2_666 . . . ? O10 Tb2 O18 Tb3 -31.8(3) . . . . ? O19 Tb2 O18 Tb3 172.7(2) . . . . ? O8 Tb2 O18 Tb3 86.90(19) . . . . ? O18 C29 O19 Tb2 2.6(4) . . . . ? C22 C29 O19 Tb2 -176.6(3) . . . . ? O16 Tb2 O19 C29 -75.5(3) 2_765 . . . ? O6 Tb2 O19 C29 7.0(3) . . . . ? O11 Tb2 O19 C29 71.6(3) . . . . ? O14 Tb2 O19 C29 -160.2(3) 2_666 . . . ? O10 Tb2 O19 C29 -155.6(3) . . . . ? O18 Tb2 O19 C29 -1.4(2) . . . . ? O8 Tb2 O19 C29 127.8(3) . . . . ? O21 C30 O20 Tb3 52.9(6) . . . 1_455 ? C24 C30 O20 Tb3 -124.7(4) . . . 1_455 ? O20 C30 O21 Tb3 23.1(8) . . . 2_675 ? C24 C30 O21 Tb3 -159.3(3) . . . 2_675 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.627 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.137 _database_code_depnum_ccdc_archive 'CCDC 946979'