# Electronic Supplementary Material (ESI) for CrystEngComm # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'C33 H24 O12 Pr' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C33 H22 O11 Pr, H2 O' _chemical_formula_sum 'C33 H24 O12 Pr' _chemical_formula_weight 753.43 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.442(2) _cell_length_b 11.545(2) _cell_length_c 14.071(3) _cell_angle_alpha 102.208(2) _cell_angle_beta 110.9310(10) _cell_angle_gamma 100.5360(10) _cell_volume 1485.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4340 _cell_measurement_theta_min 2.7448 _cell_measurement_theta_max 27.5126 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 754 _exptl_absorpt_coefficient_mu 1.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6846 _exptl_absorpt_correction_T_max 0.7485 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12314 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5313 _reflns_number_gt 4998 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+4.2368P] 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 5313 _refine_ls_number_parameters 415 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 1.001 _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 Pr1 Pr 0.615285(18) 0.562735(14) 0.660546(13) 0.01311(7) Uani 1 1 d . . . C1 C 0.8007(4) 0.7875(3) 0.8232(3) 0.0219(7) Uani 1 1 d . . . C2 C 0.9029(4) 0.8995(3) 0.9133(3) 0.0217(7) Uani 1 1 d . . . C3 C 0.8936(4) 0.9216(3) 1.0113(3) 0.0234(8) Uani 1 1 d . . . H3 H 0.8216 0.8685 1.0186 0.028 Uiso 1 1 calc R . . C4 C 1.0101(4) 0.9785(3) 0.9010(3) 0.0216(7) Uani 1 1 d . . . C5 C 1.0190(4) 0.9636(3) 0.7941(3) 0.0251(8) Uani 1 1 d . . . C6 C 1.1349(5) 0.9150(3) 0.7768(3) 0.0300(9) Uani 1 1 d . . . C7 C 1.2580(5) 0.9176(4) 0.8597(4) 0.0397(10) Uani 1 1 d . . . H7 H 1.2674 0.9435 0.9297 0.048 Uiso 1 1 calc R . . C8 C 1.3680(7) 0.8816(5) 0.8389(5) 0.0587(14) Uani 1 1 d . . . H8 H 1.4517 0.8862 0.8952 0.070 Uiso 1 1 calc R . . C9 C 1.3533(6) 0.8392(5) 0.7356(5) 0.0575(14) Uani 1 1 d U . . H9 H 1.4270 0.8152 0.7221 0.069 Uiso 1 1 calc R . . C10 C 1.2317(6) 0.8323(5) 0.6536(5) 0.0574(14) Uani 1 1 d U . . H10 H 1.2213 0.8013 0.5838 0.069 Uiso 1 1 calc R . . C11 C 1.1211(6) 0.8715(4) 0.6723(4) 0.0475(12) Uani 1 1 d . . . H11 H 1.0390 0.8684 0.6154 0.057 Uiso 1 1 calc R . . C12 C 0.4839(4) 0.7433(3) 0.4953(3) 0.0180(7) Uani 1 1 d . . . C13 C 0.4874(4) 0.8762(3) 0.4977(3) 0.0174(7) Uani 1 1 d . . . C14 C 0.6051(4) 0.9699(3) 0.5759(3) 0.0190(7) Uani 1 1 d . . . H14 H 0.6756 0.9503 0.6273 0.023 Uiso 1 1 calc R . . C15 C 0.3813(4) 0.9066(3) 0.4219(3) 0.0179(7) Uani 1 1 d . . . C16 C 0.2444(4) 0.8112(3) 0.3420(3) 0.0202(7) Uani 1 1 d . . . C17 C 0.2118(4) 0.7852(3) 0.2262(3) 0.0234(8) Uani 1 1 d . . . C18 C 0.3163(5) 0.8245(4) 0.1917(3) 0.0390(10) Uani 1 1 d . . . H18 H 0.4069 0.8732 0.2411 0.047 Uiso 1 1 calc R . . C19 C 0.2859(6) 0.7914(6) 0.0841(4) 0.0566(14) Uani 1 1 d . . . H19 H 0.3566 0.8169 0.0613 0.068 Uiso 1 1 calc R . . C20 C 0.1509(6) 0.7207(5) 0.0103(4) 0.0546(14) Uani 1 1 d . . . H20 H 0.1311 0.6983 -0.0621 0.066 Uiso 1 1 calc R . . C21 C 0.0464(6) 0.6836(4) 0.0432(4) 0.0479(12) Uani 1 1 d . . . H21 H -0.0447 0.6370 -0.0069 0.058 Uiso 1 1 calc R . . C22 C 0.0756(5) 0.7151(4) 0.1509(3) 0.0336(9) Uani 1 1 d . . . H22 H 0.0041 0.6894 0.1730 0.040 Uiso 1 1 calc R . . C23 C 0.7015(4) 0.4906(3) 0.4276(3) 0.0177(7) Uani 1 1 d . . . C24 C 0.8569(4) 0.4998(3) 0.4651(3) 0.0187(7) Uani 1 1 d . . . C25 C 0.9260(4) 0.4788(3) 0.5609(3) 0.0219(7) Uani 1 1 d . . . H25 H 0.8758 0.4642 0.6020 0.026 Uiso 1 1 calc R . . C26 C 0.9314(4) 0.5212(3) 0.4024(3) 0.0199(7) Uani 1 1 d . . . C27 C 0.8677(4) 0.5455(4) 0.2969(3) 0.0265(8) Uani 1 1 d . . . C28 C 0.8035(4) 0.6496(4) 0.2902(4) 0.0319(9) Uani 1 1 d . . . C29 C 0.7277(5) 0.6595(5) 0.1892(4) 0.0471(12) Uani 1 1 d . . . H29 H 0.7173 0.6012 0.1282 0.057 Uiso 1 1 calc R . . C30 C 0.6686(7) 0.7563(5) 0.1809(5) 0.0596(14) Uani 1 1 d U . . H30 H 0.6170 0.7626 0.1139 0.072 Uiso 1 1 calc R . . C31 C 0.6851(7) 0.8411(6) 0.2687(5) 0.0601(14) Uani 1 1 d U . . H31 H 0.6447 0.9059 0.2611 0.072 Uiso 1 1 calc R . . C32 C 0.7608(7) 0.8362(5) 0.3716(6) 0.0664(17) Uani 1 1 d . . . H32 H 0.7717 0.8963 0.4318 0.080 Uiso 1 1 calc R . . C33 C 0.8194(5) 0.7369(4) 0.3802(5) 0.0453(11) Uani 1 1 d . . . H33 H 0.8694 0.7299 0.4472 0.054 Uiso 1 1 calc R . . O1 O 0.8310(3) 0.7487(2) 0.7462(2) 0.0281(6) Uani 1 1 d . . . O2 O 0.6886(3) 0.7326(2) 0.8292(2) 0.0297(6) Uani 1 1 d . . . O3 O 0.9379(3) 0.9965(3) 0.7269(2) 0.0393(7) Uani 1 1 d . . . O4 O 0.5406(3) 0.7239(2) 0.58307(19) 0.0230(5) Uani 1 1 d . . . O5 O 0.5733(3) 0.3370(2) 0.5952(2) 0.0255(6) Uani 1 1 d . . . O6 O 0.1625(3) 0.7579(3) 0.3732(2) 0.0336(6) Uani 1 1 d . . . O7 O 0.3781(3) 0.5539(2) 0.6698(2) 0.0244(5) Uani 1 1 d . . . O8 O 0.6528(2) 0.5263(2) 0.49653(19) 0.0200(5) Uani 1 1 d . . . O9 O 0.8758(3) 0.4824(3) 0.2193(2) 0.0418(8) Uani 1 1 d . . . O1W O 0.5925(3) 0.4599(3) 0.8020(3) 0.0405(7) Uani 1 1 d . . . H1WA H 0.5598 0.4987 0.8421 0.049 Uiso 1 1 d R . . H1WB H 0.5447 0.3842 0.7797 0.049 Uiso 1 1 d R . . O2W O 0.8433(3) 0.5184(3) 0.7713(2) 0.0325(6) Uani 1 1 d . . . H2WA H 0.9301 0.5574 0.7902 0.039 Uiso 1 1 d R . . H2WB H 0.8323 0.4431 0.7409 0.039 Uiso 1 1 d R . . O3W O 0.4976(6) 0.6381(5) 0.9145(4) 0.0804(13) Uani 1 1 d . . . H3WA H 0.5733 0.6784 0.9131 0.097 Uiso 1 1 d R . . H3WB H 0.4315 0.6182 0.8522 0.097 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 0.01151(11) 0.00965(10) 0.01388(11) 0.00114(7) 0.00245(8) 0.00161(7) C1 0.0204(18) 0.0152(16) 0.0201(18) -0.0008(14) 0.0031(15) 0.0003(14) C2 0.0183(18) 0.0151(16) 0.0224(18) -0.0011(13) 0.0042(15) 0.0002(13) C3 0.0207(18) 0.0181(17) 0.0239(18) 0.0004(14) 0.0080(16) -0.0026(14) C4 0.0194(18) 0.0171(16) 0.0213(17) -0.0001(14) 0.0053(15) 0.0022(14) C5 0.025(2) 0.0172(16) 0.0227(19) -0.0002(14) 0.0067(16) -0.0047(14) C6 0.037(2) 0.0189(17) 0.033(2) 0.0046(16) 0.0185(19) 0.0030(16) C7 0.044(3) 0.044(3) 0.040(2) 0.018(2) 0.020(2) 0.022(2) C8 0.061(4) 0.060(3) 0.075(4) 0.029(3) 0.035(3) 0.037(3) C9 0.0580(16) 0.0567(16) 0.0601(16) 0.0144(10) 0.0273(11) 0.0189(10) C10 0.0592(16) 0.0577(16) 0.0569(16) 0.0128(10) 0.0284(11) 0.0159(10) C11 0.058(3) 0.042(3) 0.036(2) -0.003(2) 0.024(2) 0.005(2) C12 0.0152(17) 0.0108(15) 0.0246(18) 0.0047(13) 0.0053(15) 0.0029(12) C13 0.0207(18) 0.0108(15) 0.0179(16) 0.0042(13) 0.0053(15) 0.0039(13) C14 0.0192(18) 0.0126(15) 0.0197(17) 0.0057(13) 0.0014(15) 0.0047(13) C15 0.0187(17) 0.0123(15) 0.0175(16) 0.0025(12) 0.0035(14) 0.0031(13) C16 0.0194(18) 0.0131(15) 0.0222(18) 0.0045(13) 0.0023(15) 0.0048(13) C17 0.0237(19) 0.0165(16) 0.0225(18) 0.0038(14) 0.0022(16) 0.0061(14) C18 0.030(2) 0.049(3) 0.029(2) 0.0078(19) 0.0071(19) 0.005(2) C19 0.056(3) 0.079(4) 0.038(3) 0.016(3) 0.024(3) 0.017(3) C20 0.070(4) 0.059(3) 0.021(2) 0.003(2) 0.010(2) 0.016(3) C21 0.051(3) 0.039(3) 0.028(2) -0.0002(19) -0.003(2) 0.003(2) C22 0.030(2) 0.027(2) 0.028(2) 0.0054(16) -0.0004(18) 0.0004(17) C23 0.0163(17) 0.0153(15) 0.0245(18) 0.0090(13) 0.0101(15) 0.0044(13) C24 0.0141(17) 0.0190(16) 0.0218(17) 0.0044(13) 0.0071(14) 0.0043(13) C25 0.0170(18) 0.0287(18) 0.0245(18) 0.0110(15) 0.0115(15) 0.0076(14) C26 0.0160(17) 0.0225(17) 0.0214(17) 0.0070(14) 0.0077(15) 0.0055(13) C27 0.0125(17) 0.040(2) 0.027(2) 0.0141(17) 0.0070(15) 0.0056(15) C28 0.0177(19) 0.040(2) 0.046(2) 0.027(2) 0.0146(18) 0.0090(16) C29 0.029(2) 0.063(3) 0.058(3) 0.043(3) 0.014(2) 0.014(2) C30 0.0585(17) 0.0595(17) 0.0612(17) 0.0242(10) 0.0221(11) 0.0155(10) C31 0.0587(17) 0.0585(17) 0.0639(17) 0.0234(10) 0.0230(11) 0.0170(10) C32 0.066(4) 0.038(3) 0.106(5) 0.019(3) 0.050(4) 0.013(3) C33 0.044(3) 0.036(2) 0.065(3) 0.023(2) 0.026(3) 0.013(2) O1 0.0232(14) 0.0228(13) 0.0258(14) -0.0058(11) 0.0092(11) -0.0050(11) O2 0.0240(14) 0.0252(13) 0.0257(14) -0.0063(11) 0.0103(12) -0.0092(11) O3 0.0365(17) 0.0460(18) 0.0291(16) 0.0133(14) 0.0057(14) 0.0107(14) O4 0.0272(14) 0.0146(11) 0.0216(13) 0.0066(10) 0.0032(11) 0.0060(10) O5 0.0356(15) 0.0103(11) 0.0215(13) 0.0014(10) 0.0041(12) 0.0054(10) O6 0.0280(15) 0.0316(15) 0.0321(15) 0.0114(12) 0.0076(13) -0.0044(12) O7 0.0150(12) 0.0348(14) 0.0189(13) 0.0050(11) 0.0048(11) 0.0052(11) O8 0.0159(12) 0.0209(12) 0.0235(13) 0.0045(10) 0.0101(10) 0.0040(9) O9 0.0400(18) 0.065(2) 0.0228(15) 0.0113(14) 0.0127(14) 0.0226(16) O1W 0.0466(19) 0.0403(17) 0.0476(19) 0.0249(15) 0.0265(16) 0.0142(14) O2W 0.0233(14) 0.0305(14) 0.0385(16) 0.0093(12) 0.0064(13) 0.0101(11) O3W 0.091(3) 0.088(3) 0.062(3) 0.016(2) 0.040(3) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O8 2.440(2) . ? Pr1 O4 2.457(2) . ? Pr1 O5 2.472(2) . ? Pr1 O2 2.500(2) . ? Pr1 O7 2.511(2) . ? Pr1 O1 2.517(2) . ? Pr1 O2W 2.548(3) . ? Pr1 O1W 2.581(3) . ? Pr1 O8 2.710(2) 2_666 ? Pr1 C23 2.977(3) 2_666 ? C1 O1 1.251(4) . ? C1 O2 1.266(5) . ? C1 C2 1.502(5) . ? C2 C3 1.389(5) . ? C2 C4 1.395(5) . ? C3 C4 1.398(5) 2_777 ? C3 H3 0.9300 . ? C4 C3 1.398(5) 2_777 ? C4 C5 1.516(5) . ? C5 O3 1.206(5) . ? C5 C6 1.496(6) . ? C6 C7 1.383(7) . ? C6 C11 1.394(6) . ? C7 C8 1.393(7) . ? C7 H7 0.9300 . ? C8 C9 1.374(8) . ? C8 H8 0.9300 . ? C9 C10 1.352(8) . ? C9 H9 0.9300 . ? C10 C11 1.402(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O4 1.253(4) . ? C12 O5 1.261(4) 2_666 ? C12 C13 1.521(4) . ? C13 C14 1.391(5) . ? C13 C15 1.394(5) . ? C14 C15 1.400(5) 2_676 ? C14 H14 0.9300 . ? C15 C14 1.400(5) 2_676 ? C15 C16 1.507(5) . ? C16 O6 1.222(5) . ? C16 C17 1.490(5) . ? C17 C18 1.387(6) . ? C17 C22 1.393(5) . ? C18 C19 1.380(7) . ? C18 H18 0.9300 . ? C19 C20 1.381(8) . ? C19 H19 0.9300 . ? C20 C21 1.364(8) . ? C20 H20 0.9300 . ? C21 C22 1.386(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O7 1.250(4) 2_666 ? C23 O8 1.277(4) . ? C23 C24 1.492(5) . ? C23 Pr1 2.977(3) 2_666 ? C24 C25 1.380(5) . ? C24 C26 1.398(5) . ? C25 C26 1.391(5) 2_766 ? C25 H25 0.9300 . ? C26 C25 1.391(5) 2_766 ? C26 C27 1.505(5) . ? C27 O9 1.217(5) . ? C27 C28 1.484(6) . ? C28 C33 1.377(7) . ? C28 C29 1.398(6) . ? C29 C30 1.378(8) . ? C29 H29 0.9300 . ? C30 C31 1.338(8) . ? C30 H30 0.9300 . ? C31 C32 1.399(9) . ? C31 H31 0.9300 . ? C32 C33 1.402(7) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? O5 C12 1.261(4) 2_666 ? O7 C23 1.250(4) 2_666 ? O8 Pr1 2.710(2) 2_666 ? O1W H1WA 0.8499 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8497 . ? O3W H3WA 0.8501 . ? O3W H3WB 0.8501 . ? 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 O8 Pr1 O4 74.96(8) . . ? O8 Pr1 O5 74.49(8) . . ? O4 Pr1 O5 136.31(8) . . ? O8 Pr1 O2 139.20(8) . . ? O4 Pr1 O2 81.02(9) . . ? O5 Pr1 O2 140.87(9) . . ? O8 Pr1 O7 124.95(8) . . ? O4 Pr1 O7 76.65(9) . . ? O5 Pr1 O7 96.45(9) . . ? O2 Pr1 O7 79.20(8) . . ? O8 Pr1 O1 89.43(8) . . ? O4 Pr1 O1 74.07(9) . . ? O5 Pr1 O1 135.49(9) . . ? O2 Pr1 O1 52.04(8) . . ? O7 Pr1 O1 125.82(8) . . ? O8 Pr1 O2W 95.50(9) . . ? O4 Pr1 O2W 139.51(9) . . ? O5 Pr1 O2W 73.99(9) . . ? O2 Pr1 O2W 81.86(10) . . ? O7 Pr1 O2W 134.86(9) . . ? O1 Pr1 O2W 66.46(9) . . ? O8 Pr1 O1W 142.53(9) . . ? O4 Pr1 O1W 140.25(9) . . ? O5 Pr1 O1W 69.26(10) . . ? O2 Pr1 O1W 72.93(10) . . ? O7 Pr1 O1W 69.45(9) . . ? O1 Pr1 O1W 109.84(10) . . ? O2W Pr1 O1W 65.91(10) . . ? O8 Pr1 O8 76.03(8) . 2_666 ? O4 Pr1 O8 68.76(8) . 2_666 ? O5 Pr1 O8 74.06(8) . 2_666 ? O2 Pr1 O8 124.60(8) . 2_666 ? O7 Pr1 O8 49.84(8) . 2_666 ? O1 Pr1 O8 142.42(8) . 2_666 ? O2W Pr1 O8 148.06(8) . 2_666 ? O1W Pr1 O8 102.24(9) . 2_666 ? O8 Pr1 C23 100.73(9) . 2_666 ? O4 Pr1 C23 69.71(9) . 2_666 ? O5 Pr1 C23 86.22(9) . 2_666 ? O2 Pr1 C23 101.18(9) . 2_666 ? O7 Pr1 C23 24.50(9) . 2_666 ? O1 Pr1 C23 138.06(9) . 2_666 ? O2W Pr1 C23 150.01(9) . 2_666 ? O1W Pr1 C23 86.26(10) . 2_666 ? O8 Pr1 C23 25.40(8) 2_666 2_666 ? O8 Pr1 Pr1 40.36(6) . 2_666 ? O4 Pr1 Pr1 66.57(6) . 2_666 ? O5 Pr1 Pr1 69.89(6) . 2_666 ? O2 Pr1 Pr1 146.49(7) . 2_666 ? O7 Pr1 Pr1 85.05(6) . 2_666 ? O1 Pr1 Pr1 121.53(6) . 2_666 ? O2W Pr1 Pr1 128.60(7) . 2_666 ? O1W Pr1 Pr1 128.19(8) . 2_666 ? O8 Pr1 Pr1 35.66(5) 2_666 2_666 ? C23 Pr1 Pr1 60.59(7) 2_666 2_666 ? O1 C1 O2 121.9(3) . . ? O1 C1 C2 119.2(3) . . ? O2 C1 C2 118.8(3) . . ? C3 C2 C4 119.9(3) . . ? C3 C2 C1 119.3(3) . . ? C4 C2 C1 120.8(3) . . ? C2 C3 C4 121.6(3) . 2_777 ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 2_777 . ? C2 C4 C3 118.6(3) . 2_777 ? C2 C4 C5 122.0(3) . . ? C3 C4 C5 119.4(3) 2_777 . ? O3 C5 C6 121.3(4) . . ? O3 C5 C4 119.8(4) . . ? C6 C5 C4 118.8(3) . . ? C7 C6 C11 118.7(4) . . ? C7 C6 C5 123.0(4) . . ? C11 C6 C5 118.1(4) . . ? C6 C7 C8 120.4(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 120.3(6) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.0(6) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.8(5) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C6 C11 C10 119.7(5) . . ? C6 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? O4 C12 O5 125.9(3) . 2_666 ? O4 C12 C13 117.1(3) . . ? O5 C12 C13 117.0(3) 2_666 . ? C14 C13 C15 119.3(3) . . ? C14 C13 C12 118.1(3) . . ? C15 C13 C12 122.5(3) . . ? C13 C14 C15 120.7(3) . 2_676 ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 2_676 . ? C13 C15 C14 120.0(3) . 2_676 ? C13 C15 C16 121.9(3) . . ? C14 C15 C16 117.9(3) 2_676 . ? O6 C16 C17 121.6(3) . . ? O6 C16 C15 119.6(3) . . ? C17 C16 C15 118.9(3) . . ? C18 C17 C22 119.2(4) . . ? C18 C17 C16 121.3(3) . . ? C22 C17 C16 119.5(4) . . ? C19 C18 C17 120.1(4) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.3(5) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 120.2(5) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.3(4) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C17 120.1(4) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? O7 C23 O8 121.7(3) 2_666 . ? O7 C23 C24 119.5(3) 2_666 . ? O8 C23 C24 118.7(3) . . ? O7 C23 Pr1 56.39(17) 2_666 2_666 ? O8 C23 Pr1 65.56(18) . 2_666 ? C24 C23 Pr1 172.5(2) . 2_666 ? C25 C24 C26 119.5(3) . . ? C25 C24 C23 118.9(3) . . ? C26 C24 C23 121.6(3) . . ? C24 C25 C26 121.9(3) . 2_766 ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 2_766 . ? C25 C26 C24 118.7(3) 2_766 . ? C25 C26 C27 117.1(3) 2_766 . ? C24 C26 C27 124.2(3) . . ? O9 C27 C28 121.1(4) . . ? O9 C27 C26 119.1(4) . . ? C28 C27 C26 119.8(3) . . ? C33 C28 C29 119.9(4) . . ? C33 C28 C27 121.7(4) . . ? C29 C28 C27 118.4(4) . . ? C30 C29 C28 119.5(5) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C31 C30 C29 120.3(6) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 122.5(6) . . ? C30 C31 H31 118.7 . . ? C32 C31 H31 118.7 . . ? C31 C32 C33 117.2(6) . . ? C31 C32 H32 121.4 . . ? C33 C32 H32 121.4 . . ? C28 C33 C32 120.6(5) . . ? C28 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C1 O1 Pr1 92.8(2) . . ? C1 O2 Pr1 93.2(2) . . ? C12 O4 Pr1 141.9(2) . . ? C12 O5 Pr1 135.2(2) 2_666 . ? C23 O7 Pr1 99.1(2) 2_666 . ? C23 O8 Pr1 161.2(2) . . ? C23 O8 Pr1 89.0(2) . 2_666 ? Pr1 O8 Pr1 103.97(8) . 2_666 ? Pr1 O1W H1WA 113.1 . . ? Pr1 O1W H1WB 117.2 . . ? H1WA O1W H1WB 107.4 . . ? Pr1 O2W H2WA 129.5 . . ? Pr1 O2W H2WB 104.4 . . ? H2WA O2W H2WB 107.5 . . ? H3WA O3W H3WB 107.4 . . ? 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 O1 C1 C2 C3 -160.8(4) . . . . ? O2 C1 C2 C3 16.8(5) . . . . ? O1 C1 C2 C4 16.6(5) . . . . ? O2 C1 C2 C4 -165.8(4) . . . . ? C4 C2 C3 C4 -0.2(6) . . . 2_777 ? C1 C2 C3 C4 177.3(3) . . . 2_777 ? C3 C2 C4 C3 0.2(6) . . . 2_777 ? C1 C2 C4 C3 -177.2(3) . . . 2_777 ? C3 C2 C4 C5 -175.9(3) . . . . ? C1 C2 C4 C5 6.8(5) . . . . ? C2 C4 C5 O3 76.2(5) . . . . ? C3 C4 C5 O3 -99.8(4) 2_777 . . . ? C2 C4 C5 C6 -107.4(4) . . . . ? C3 C4 C5 C6 76.6(4) 2_777 . . . ? O3 C5 C6 C7 156.2(4) . . . . ? C4 C5 C6 C7 -20.1(5) . . . . ? O3 C5 C6 C11 -20.1(6) . . . . ? C4 C5 C6 C11 163.6(4) . . . . ? C11 C6 C7 C8 2.3(7) . . . . ? C5 C6 C7 C8 -174.0(4) . . . . ? C6 C7 C8 C9 -2.2(8) . . . . ? C7 C8 C9 C10 0.0(9) . . . . ? C8 C9 C10 C11 1.9(9) . . . . ? C7 C6 C11 C10 -0.4(7) . . . . ? C5 C6 C11 C10 176.1(4) . . . . ? C9 C10 C11 C6 -1.7(8) . . . . ? O4 C12 C13 C14 33.3(5) . . . . ? O5 C12 C13 C14 -145.4(3) 2_666 . . . ? O4 C12 C13 C15 -149.9(3) . . . . ? O5 C12 C13 C15 31.4(5) 2_666 . . . ? C15 C13 C14 C15 -0.9(6) . . . 2_676 ? C12 C13 C14 C15 175.9(3) . . . 2_676 ? C14 C13 C15 C14 0.9(6) . . . 2_676 ? C12 C13 C15 C14 -175.8(3) . . . 2_676 ? C14 C13 C15 C16 -173.9(3) . . . . ? C12 C13 C15 C16 9.4(5) . . . . ? C13 C15 C16 O6 62.9(5) . . . . ? C14 C15 C16 O6 -112.1(4) 2_676 . . . ? C13 C15 C16 C17 -117.7(4) . . . . ? C14 C15 C16 C17 67.4(4) 2_676 . . . ? O6 C16 C17 C18 -165.8(4) . . . . ? C15 C16 C17 C18 14.8(5) . . . . ? O6 C16 C17 C22 11.2(5) . . . . ? C15 C16 C17 C22 -168.3(3) . . . . ? C22 C17 C18 C19 -1.7(7) . . . . ? C16 C17 C18 C19 175.3(4) . . . . ? C17 C18 C19 C20 1.0(8) . . . . ? C18 C19 C20 C21 0.4(9) . . . . ? C19 C20 C21 C22 -0.9(8) . . . . ? C20 C21 C22 C17 0.2(7) . . . . ? C18 C17 C22 C21 1.1(6) . . . . ? C16 C17 C22 C21 -175.9(4) . . . . ? O7 C23 C24 C25 -143.0(3) 2_666 . . . ? O8 C23 C24 C25 35.6(5) . . . . ? O7 C23 C24 C26 32.7(5) 2_666 . . . ? O8 C23 C24 C26 -148.7(3) . . . . ? C26 C24 C25 C26 0.4(6) . . . 2_766 ? C23 C24 C25 C26 176.2(3) . . . 2_766 ? C25 C24 C26 C25 -0.4(6) . . . 2_766 ? C23 C24 C26 C25 -176.1(3) . . . 2_766 ? C25 C24 C26 C27 -179.8(3) . . . . ? C23 C24 C26 C27 4.5(5) . . . . ? C25 C26 C27 O9 53.8(5) 2_766 . . . ? C24 C26 C27 O9 -126.7(4) . . . . ? C25 C26 C27 C28 -122.8(4) 2_766 . . . ? C24 C26 C27 C28 56.6(5) . . . . ? O9 C27 C28 C33 -166.4(4) . . . . ? C26 C27 C28 C33 10.1(6) . . . . ? O9 C27 C28 C29 12.2(6) . . . . ? C26 C27 C28 C29 -171.2(4) . . . . ? C33 C28 C29 C30 -0.5(7) . . . . ? C27 C28 C29 C30 -179.2(4) . . . . ? C28 C29 C30 C31 0.9(8) . . . . ? C29 C30 C31 C32 -0.4(9) . . . . ? C30 C31 C32 C33 -0.4(9) . . . . ? C29 C28 C33 C32 -0.3(7) . . . . ? C27 C28 C33 C32 178.3(4) . . . . ? C31 C32 C33 C28 0.8(8) . . . . ? O2 C1 O1 Pr1 -2.4(4) . . . . ? C2 C1 O1 Pr1 175.2(3) . . . . ? O8 Pr1 O1 C1 166.8(2) . . . . ? O4 Pr1 O1 C1 92.2(2) . . . . ? O5 Pr1 O1 C1 -126.3(2) . . . . ? O2 Pr1 O1 C1 1.3(2) . . . . ? O7 Pr1 O1 C1 32.4(3) . . . . ? O2W Pr1 O1 C1 -97.0(2) . . . . ? O1W Pr1 O1 C1 -46.1(2) . . . . ? O8 Pr1 O1 C1 100.9(2) 2_666 . . . ? C23 Pr1 O1 C1 61.2(3) 2_666 . . . ? Pr1 Pr1 O1 C1 140.9(2) 2_666 . . . ? O1 C1 O2 Pr1 2.4(4) . . . . ? C2 C1 O2 Pr1 -175.2(3) . . . . ? O8 Pr1 O2 C1 -23.8(3) . . . . ? O4 Pr1 O2 C1 -78.0(2) . . . . ? O5 Pr1 O2 C1 117.0(2) . . . . ? O7 Pr1 O2 C1 -156.0(2) . . . . ? O1 Pr1 O2 C1 -1.3(2) . . . . ? O2W Pr1 O2 C1 65.1(2) . . . . ? O1W Pr1 O2 C1 132.4(2) . . . . ? O8 Pr1 O2 C1 -134.3(2) 2_666 . . . ? C23 Pr1 O2 C1 -145.1(2) 2_666 . . . ? Pr1 Pr1 O2 C1 -92.6(2) 2_666 . . . ? O5 C12 O4 Pr1 8.9(6) 2_666 . . . ? C13 C12 O4 Pr1 -169.6(2) . . . . ? O8 Pr1 O4 C12 33.3(4) . . . . ? O5 Pr1 O4 C12 -13.7(4) . . . . ? O2 Pr1 O4 C12 -180.0(4) . . . . ? O7 Pr1 O4 C12 -99.1(4) . . . . ? O1 Pr1 O4 C12 127.1(4) . . . . ? O2W Pr1 O4 C12 114.0(4) . . . . ? O1W Pr1 O4 C12 -130.9(4) . . . . ? O8 Pr1 O4 C12 -47.3(4) 2_666 . . . ? C23 Pr1 O4 C12 -74.5(4) 2_666 . . . ? Pr1 Pr1 O4 C12 -8.7(4) 2_666 . . . ? O8 Pr1 O5 C12 -37.9(3) . . . 2_666 ? O4 Pr1 O5 C12 9.3(4) . . . 2_666 ? O2 Pr1 O5 C12 167.4(3) . . . 2_666 ? O7 Pr1 O5 C12 86.7(3) . . . 2_666 ? O1 Pr1 O5 C12 -110.6(3) . . . 2_666 ? O2W Pr1 O5 C12 -138.4(3) . . . 2_666 ? O1W Pr1 O5 C12 151.8(4) . . . 2_666 ? O8 Pr1 O5 C12 41.7(3) 2_666 . . 2_666 ? C23 Pr1 O5 C12 64.3(3) 2_666 . . 2_666 ? Pr1 Pr1 O5 C12 4.3(3) 2_666 . . 2_666 ? O8 Pr1 O7 C23 9.6(2) . . . 2_666 ? O4 Pr1 O7 C23 70.2(2) . . . 2_666 ? O5 Pr1 O7 C23 -65.9(2) . . . 2_666 ? O2 Pr1 O7 C23 153.4(2) . . . 2_666 ? O1 Pr1 O7 C23 128.9(2) . . . 2_666 ? O2W Pr1 O7 C23 -139.7(2) . . . 2_666 ? O1W Pr1 O7 C23 -130.9(2) . . . 2_666 ? O8 Pr1 O7 C23 -3.11(18) 2_666 . . 2_666 ? Pr1 Pr1 O7 C23 3.2(2) 2_666 . . 2_666 ? O7 C23 O8 Pr1 139.8(5) 2_666 . . . ? C24 C23 O8 Pr1 -38.8(8) . . . . ? Pr1 C23 O8 Pr1 134.4(7) 2_666 . . . ? O7 C23 O8 Pr1 5.4(3) 2_666 . . 2_666 ? C24 C23 O8 Pr1 -173.2(3) . . . 2_666 ? O4 Pr1 O8 C23 156.1(7) . . . . ? O5 Pr1 O8 C23 -55.5(7) . . . . ? O2 Pr1 O8 C23 100.1(7) . . . . ? O7 Pr1 O8 C23 -142.6(7) . . . . ? O1 Pr1 O8 C23 82.4(7) . . . . ? O2W Pr1 O8 C23 16.2(7) . . . . ? O1W Pr1 O8 C23 -40.6(7) . . . . ? O8 Pr1 O8 C23 -132.5(7) 2_666 . . . ? C23 Pr1 O8 C23 -138.5(6) 2_666 . . . ? Pr1 Pr1 O8 C23 -132.5(7) 2_666 . . . ? O4 Pr1 O8 Pr1 -71.36(9) . . . 2_666 ? O5 Pr1 O8 Pr1 77.02(9) . . . 2_666 ? O2 Pr1 O8 Pr1 -127.39(12) . . . 2_666 ? O7 Pr1 O8 Pr1 -10.01(13) . . . 2_666 ? O1 Pr1 O8 Pr1 -145.01(9) . . . 2_666 ? O2W Pr1 O8 Pr1 148.71(9) . . . 2_666 ? O1W Pr1 O8 Pr1 91.97(15) . . . 2_666 ? O8 Pr1 O8 Pr1 0.0 2_666 . . 2_666 ? C23 Pr1 O8 Pr1 -5.96(10) 2_666 . . 2_666 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.308 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.134 _database_code_depnum_ccdc_archive 'CCDC 890964' ####################################################################### # # 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_14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H22 Er O11' _chemical_formula_sum 'C33 H22 Er O11' _chemical_formula_weight 761.77 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' Er Er -0.2586 4.9576 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1324(8) _cell_length_b 10.1905(9) _cell_length_c 15.5442(10) _cell_angle_alpha 96.333(2) _cell_angle_beta 97.155(3) _cell_angle_gamma 114.009(3) _cell_volume 1431.59(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4053 _cell_measurement_theta_min 2.2231 _cell_measurement_theta_max 27.4758 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 2.997 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.3650 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10186 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6325 _reflns_number_gt 5851 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1131P)^2^+1.7785P] 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 6325 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1956 _refine_ls_wR_factor_gt 0.1755 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 Er1 Er 0.44456(3) 0.63143(3) 0.588597(17) 0.02152(15) Uani 1 1 d . . . C1 C 0.5345(8) 0.9202(8) 0.6644(5) 0.0270(15) Uani 1 1 d . . . C2 C 0.5778(8) 0.4201(8) 0.6392(5) 0.0269(15) Uani 1 1 d . . . C3 C 0.5798(8) 1.0738(8) 0.7061(5) 0.0257(15) Uani 1 1 d . . . C4 C 0.5650(9) 1.1732(8) 0.6553(5) 0.0296(16) Uani 1 1 d . . . H4 H 0.5244 1.1422 0.5955 0.036 Uiso 1 1 calc R . . C5 C 0.6106(9) 0.3189(8) 0.6933(5) 0.0245(14) Uani 1 1 d . . . C6 C 0.6770(8) 0.3681(8) 0.7821(5) 0.0242(14) Uani 1 1 d . . . C7 C 0.6914(8) 1.2681(8) 0.8325(5) 0.0267(15) Uani 1 1 d . . . H7 H 0.7346 1.2997 0.8918 0.032 Uiso 1 1 calc R . . C8 C 0.6420(8) 1.1212(8) 0.7956(5) 0.0244(14) Uani 1 1 d . . . C9 C 0.7377(10) 0.5261(8) 0.8271(5) 0.0319(17) Uani 1 1 d . . . C10 C 0.8475(9) 0.6403(9) 0.7871(6) 0.0309(17) Uani 1 1 d . . . C11 C 0.8779(10) 0.7857(9) 0.8139(7) 0.041(2) Uani 1 1 d . . . H11 H 0.8324 0.8117 0.8568 0.049 Uiso 1 1 calc R . . C12 C 0.9777(12) 0.8934(10) 0.7756(8) 0.055(3) Uani 1 1 d . . . H12 H 0.9958 0.9906 0.7922 0.066 Uiso 1 1 calc R . . C13 C 1.0481(13) 0.8575(12) 0.7147(8) 0.054(3) Uani 1 1 d . . . H13 H 1.1150 0.9304 0.6907 0.065 Uiso 1 1 calc R . . C14 C 1.0212(12) 0.7148(12) 0.6884(7) 0.050(2) Uani 1 1 d . . . H14 H 1.0703 0.6911 0.6469 0.060 Uiso 1 1 calc R . . C15 C 0.9204(9) 0.6047(10) 0.7237(6) 0.0354(18) Uani 1 1 d . . . H15 H 0.9015 0.5078 0.7053 0.042 Uiso 1 1 calc R . . C16 C 0.6616(10) 1.0246(9) 0.8600(6) 0.0302(17) Uani 1 1 d . . . C17 C 0.5283(11) 0.9146(9) 0.8843(6) 0.0331(19) Uani 1 1 d . . . C18 C 0.5405(13) 0.8018(11) 0.9227(7) 0.048(3) Uani 1 1 d . . . H18 H 0.6300 0.7954 0.9316 0.058 Uiso 1 1 calc R . . C19 C 0.4193(15) 0.6993(14) 0.9474(8) 0.060(3) Uani 1 1 d . . . H19 H 0.4281 0.6249 0.9737 0.072 Uiso 1 1 calc R . . C20 C 0.2833(14) 0.7064(13) 0.9332(7) 0.055(3) Uani 1 1 d . . . H20 H 0.2009 0.6356 0.9480 0.066 Uiso 1 1 calc R . . C21 C 0.2742(12) 0.8203(13) 0.8970(7) 0.056(3) Uani 1 1 d . . . H21 H 0.1856 0.8288 0.8896 0.067 Uiso 1 1 calc R . . C22 C 0.3964(10) 0.9236(11) 0.8711(7) 0.044(2) Uani 1 1 d . . . H22 H 0.3880 0.9984 0.8450 0.053 Uiso 1 1 calc R . . C23 C 0.7494(8) 0.7244(8) 0.5029(5) 0.0252(14) Uani 1 1 d . . . C24 C 0.8815(8) 0.8671(8) 0.5007(5) 0.0270(15) Uani 1 1 d . . . C25 C 0.9040(9) 0.9925(8) 0.5572(5) 0.0271(16) Uani 1 1 d . . . H25 H 0.8398 0.9876 0.5959 0.032 Uiso 1 1 calc R . . C26 C 0.9786(7) 0.8740(7) 0.4430(5) 0.0234(14) Uani 1 1 d . . . C27 C 0.9697(8) 0.7504(8) 0.3774(5) 0.0275(16) Uani 1 1 d . . . C28 C 0.8939(9) 0.7311(8) 0.2847(5) 0.0309(16) Uani 1 1 d . . . C29 C 0.9567(11) 0.6977(10) 0.2167(6) 0.040(2) Uani 1 1 d . . . H29 H 1.0420 0.6842 0.2294 0.048 Uiso 1 1 calc R . . C30 C 0.8950(12) 0.6843(12) 0.1308(6) 0.050(2) Uani 1 1 d . . . H30 H 0.9400 0.6649 0.0856 0.060 Uiso 1 1 calc R . . C31 C 0.7656(12) 0.6998(11) 0.1113(6) 0.051(3) Uani 1 1 d . . . H31 H 0.7217 0.6877 0.0530 0.061 Uiso 1 1 calc R . . C32 C 0.7021(11) 0.7334(11) 0.1790(7) 0.048(2) Uani 1 1 d . . . H32 H 0.6154 0.7444 0.1665 0.057 Uiso 1 1 calc R . . C33 C 0.7676(9) 0.7506(9) 0.2656(6) 0.0364(18) Uani 1 1 d . . . H33 H 0.7261 0.7756 0.3111 0.044 Uiso 1 1 calc R . . O1 O 0.5736(7) 0.8387(6) 0.7067(3) 0.0316(12) Uani 1 1 d . . . O2 O 0.4579(8) 0.8711(6) 0.5876(4) 0.0459(16) Uani 1 1 d . . . O3 O 0.4235(8) 0.5998(6) 0.4417(3) 0.0384(14) Uani 1 1 d . . . O4 O 0.5471(6) 0.5159(6) 0.6779(4) 0.0282(11) Uani 1 1 d . . . O5 O 0.7068(9) 0.5535(7) 0.8965(4) 0.0489(17) Uani 1 1 d . . . O6 O 0.7856(8) 1.0460(8) 0.8918(5) 0.0472(17) Uani 1 1 d . . . O7 O 0.6793(7) 0.7283(6) 0.5610(4) 0.0358(13) Uani 1 1 d . . . O8 O 0.7293(6) 0.6159(5) 0.4466(4) 0.0305(12) Uani 1 1 d . . . O9 O 1.0379(8) 0.6794(7) 0.3961(4) 0.0408(15) Uani 1 1 d . . . O1W O 0.1972(7) 0.6102(8) 0.5355(5) 0.0467(18) Uani 1 1 d . . . H1WA H 0.1185 0.5408 0.5421 0.056 Uiso 1 1 d R . . H1WB H 0.1724 0.6667 0.5080 0.056 Uiso 1 1 d R . . O2W O 0.3156(7) 0.6015(7) 0.7117(4) 0.0394(14) Uani 1 1 d . . . H2WA H 0.3316 0.6681 0.7550 0.047 Uiso 1 1 d R . . H2WB H 0.2250 0.5430 0.7032 0.047 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 Er1 0.0274(2) 0.0160(2) 0.0204(2) 0.00484(15) 0.00400(14) 0.00829(15) C1 0.033(4) 0.022(3) 0.024(4) 0.002(3) 0.006(3) 0.010(3) C2 0.029(3) 0.018(3) 0.032(4) 0.011(3) 0.008(3) 0.005(3) C3 0.029(3) 0.020(3) 0.027(4) 0.002(3) 0.007(3) 0.009(3) C4 0.045(4) 0.016(3) 0.024(4) 0.003(3) 0.002(3) 0.010(3) C5 0.039(4) 0.019(3) 0.018(3) 0.007(3) 0.010(3) 0.013(3) C6 0.029(3) 0.021(3) 0.023(3) 0.005(3) 0.004(3) 0.011(3) C7 0.033(4) 0.033(4) 0.018(3) 0.008(3) 0.004(3) 0.017(3) C8 0.028(3) 0.023(3) 0.026(4) 0.009(3) 0.008(3) 0.013(3) C9 0.047(5) 0.022(4) 0.029(4) 0.006(3) 0.008(3) 0.016(3) C10 0.028(4) 0.027(4) 0.037(4) 0.008(3) 0.004(3) 0.010(3) C11 0.043(5) 0.026(4) 0.049(5) 0.002(4) 0.009(4) 0.012(4) C12 0.059(6) 0.015(4) 0.079(8) 0.005(4) 0.005(6) 0.008(4) C13 0.057(6) 0.040(6) 0.060(7) 0.020(5) 0.011(5) 0.013(5) C14 0.049(5) 0.051(6) 0.053(6) 0.017(5) 0.016(5) 0.021(5) C15 0.038(4) 0.033(4) 0.036(5) 0.007(4) 0.007(4) 0.015(4) C16 0.043(4) 0.021(4) 0.028(4) 0.009(3) 0.004(3) 0.014(3) C17 0.051(5) 0.026(4) 0.025(4) 0.009(3) 0.001(3) 0.019(4) C18 0.068(7) 0.042(5) 0.047(6) 0.024(5) 0.011(5) 0.031(5) C19 0.073(8) 0.056(7) 0.061(7) 0.038(6) 0.031(6) 0.024(6) C20 0.062(7) 0.049(6) 0.034(5) 0.010(5) 0.013(5) 0.003(5) C21 0.046(5) 0.064(7) 0.053(6) 0.016(6) 0.017(5) 0.015(5) C22 0.031(4) 0.051(5) 0.058(6) 0.022(5) 0.012(4) 0.021(4) C23 0.027(3) 0.023(3) 0.025(4) 0.010(3) 0.009(3) 0.007(3) C24 0.027(3) 0.021(3) 0.031(4) 0.008(3) 0.007(3) 0.007(3) C25 0.028(4) 0.023(4) 0.028(4) 0.004(3) 0.008(3) 0.008(3) C26 0.020(3) 0.017(3) 0.032(4) 0.006(3) 0.007(3) 0.004(3) C27 0.029(4) 0.021(3) 0.030(4) 0.005(3) 0.007(3) 0.007(3) C28 0.037(4) 0.017(3) 0.032(4) 0.002(3) 0.003(3) 0.006(3) C29 0.045(5) 0.038(5) 0.041(5) 0.010(4) 0.020(4) 0.017(4) C30 0.063(6) 0.051(6) 0.035(5) -0.002(4) 0.019(5) 0.024(5) C31 0.066(6) 0.048(6) 0.029(5) 0.014(4) 0.000(4) 0.017(5) C32 0.043(5) 0.046(5) 0.053(6) 0.019(5) 0.010(4) 0.015(4) C33 0.036(4) 0.034(4) 0.041(5) 0.006(4) 0.009(4) 0.016(4) O1 0.054(3) 0.024(3) 0.021(3) 0.006(2) 0.007(2) 0.022(3) O2 0.069(4) 0.023(3) 0.039(3) -0.004(3) -0.005(3) 0.020(3) O3 0.065(4) 0.028(3) 0.013(2) 0.008(2) 0.001(2) 0.012(3) O4 0.032(3) 0.025(3) 0.033(3) 0.010(2) 0.003(2) 0.017(2) O5 0.082(5) 0.033(3) 0.031(3) 0.003(3) 0.018(3) 0.022(3) O6 0.046(4) 0.044(4) 0.050(4) 0.018(3) 0.001(3) 0.018(3) O7 0.048(3) 0.020(3) 0.031(3) 0.001(2) 0.010(3) 0.007(2) O8 0.043(3) 0.016(2) 0.027(3) 0.001(2) 0.007(2) 0.007(2) O9 0.049(4) 0.043(4) 0.039(3) 0.005(3) 0.007(3) 0.029(3) O1W 0.036(3) 0.046(4) 0.066(5) 0.022(4) 0.009(3) 0.022(3) O2W 0.038(3) 0.034(3) 0.039(3) -0.002(3) 0.017(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O3 2.241(5) . ? Er1 O7 2.292(6) . ? Er1 O4 2.322(5) . ? Er1 O8 2.366(5) 2_666 ? Er1 O2 2.392(6) . ? Er1 O1 2.417(6) . ? Er1 O2W 2.427(6) . ? Er1 O1W 2.452(6) . ? C1 O2 1.264(10) . ? C1 O1 1.266(9) . ? C1 C3 1.482(10) . ? C2 O3 1.249(9) 2_666 ? C2 O4 1.256(9) . ? C2 C5 1.511(9) . ? C3 C4 1.395(10) . ? C3 C8 1.397(10) . ? C4 C5 1.395(10) 1_565 ? C4 H4 0.9300 . ? C5 C4 1.395(10) 1_545 ? C5 C6 1.396(10) . ? C6 C7 1.394(9) 1_545 ? C6 C9 1.516(10) . ? C7 C6 1.394(10) 1_565 ? C7 C8 1.396(10) . ? C7 H7 0.9300 . ? C8 C16 1.529(10) . ? C9 O5 1.196(10) . ? C9 C10 1.502(11) . ? C10 C11 1.387(11) . ? C10 C15 1.403(12) . ? C11 C12 1.404(14) . ? C11 H11 0.9300 . ? C12 C13 1.358(17) . ? C12 H12 0.9300 . ? C13 C14 1.370(15) . ? C13 H13 0.9300 . ? C14 C15 1.395(13) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O6 1.213(11) . ? C16 C17 1.487(13) . ? C17 C22 1.368(12) . ? C17 C18 1.394(13) . ? C18 C19 1.381(16) . ? C18 H18 0.9300 . ? C19 C20 1.401(18) . ? C19 H19 0.9300 . ? C20 C21 1.375(16) . ? C20 H20 0.9300 . ? C21 C22 1.401(14) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O7 1.223(9) . ? C23 O8 1.261(9) . ? C23 C24 1.532(10) . ? C24 C25 1.386(11) . ? C24 C26 1.398(11) . ? C25 C26 1.397(10) 2_776 ? C25 H25 0.9300 . ? C26 C25 1.397(10) 2_776 ? C26 C27 1.496(10) . ? C27 O9 1.220(10) . ? C27 C28 1.497(11) . ? C28 C33 1.375(11) . ? C28 C29 1.379(12) . ? C29 C30 1.370(14) . ? C29 H29 0.9300 . ? C30 C31 1.384(15) . ? C30 H30 0.9300 . ? C31 C32 1.381(14) . ? C31 H31 0.9300 . ? C32 C33 1.383(13) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? O3 C2 1.249(9) 2_666 ? O8 Er1 2.366(5) 2_666 ? O1W H1WA 0.8518 . ? O1W H1WB 0.8501 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? 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 Er1 O7 73.6(2) . . ? O3 Er1 O4 123.8(2) . . ? O7 Er1 O4 80.6(2) . . ? O3 Er1 O8 81.1(2) . 2_666 ? O7 Er1 O8 127.3(2) . 2_666 ? O4 Er1 O8 76.42(19) . 2_666 ? O3 Er1 O2 88.9(2) . . ? O7 Er1 O2 85.3(2) . . ? O4 Er1 O2 137.9(2) . . ? O8 Er1 O2 140.2(2) 2_666 . ? O3 Er1 O1 134.2(2) . . ? O7 Er1 O1 76.8(2) . . ? O4 Er1 O1 83.81(18) . . ? O8 Er1 O1 144.35(19) 2_666 . ? O2 Er1 O1 54.30(19) . . ? O3 Er1 O2W 146.2(2) . . ? O7 Er1 O2W 140.1(2) . . ? O4 Er1 O2W 75.2(2) . . ? O8 Er1 O2W 76.8(2) 2_666 . ? O2 Er1 O2W 91.9(2) . . ? O1 Er1 O2W 69.6(2) . . ? O3 Er1 O1W 76.1(3) . . ? O7 Er1 O1W 141.7(2) . . ? O4 Er1 O1W 136.6(2) . . ? O8 Er1 O1W 68.9(2) 2_666 . ? O2 Er1 O1W 71.3(2) . . ? O1 Er1 O1W 110.1(2) . . ? O2W Er1 O1W 72.3(2) . . ? O3 Er1 C1 112.6(2) . . ? O7 Er1 C1 80.3(2) . . ? O4 Er1 C1 110.9(2) . . ? O8 Er1 C1 152.3(2) 2_666 . ? O2 Er1 C1 27.1(2) . . ? O1 Er1 C1 27.19(19) . . ? O2W Er1 C1 79.4(2) . . ? O1W Er1 C1 90.5(2) . . ? O2 C1 O1 120.4(7) . . ? O2 C1 C3 120.6(7) . . ? O1 C1 C3 119.1(7) . . ? O2 C1 Er1 59.6(4) . . ? O1 C1 Er1 60.7(4) . . ? C3 C1 Er1 178.7(6) . . ? O3 C2 O4 123.7(7) 2_666 . ? O3 C2 C5 118.6(7) 2_666 . ? O4 C2 C5 117.6(7) . . ? C4 C3 C8 119.5(7) . . ? C4 C3 C1 119.9(7) . . ? C8 C3 C1 120.5(7) . . ? C3 C4 C5 120.5(7) . 1_565 ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 1_565 . ? C4 C5 C6 120.3(6) 1_545 . ? C4 C5 C2 119.2(6) 1_545 . ? C6 C5 C2 120.3(6) . . ? C7 C6 C5 118.8(7) 1_545 . ? C7 C6 C9 117.5(6) 1_545 . ? C5 C6 C9 123.6(6) . . ? C6 C7 C8 121.2(7) 1_565 . ? C6 C7 H7 119.4 1_565 . ? C8 C7 H7 119.4 . . ? C7 C8 C3 119.6(6) . . ? C7 C8 C16 114.9(7) . . ? C3 C8 C16 125.5(7) . . ? O5 C9 C10 122.5(8) . . ? O5 C9 C6 119.0(7) . . ? C10 C9 C6 118.2(7) . . ? C11 C10 C15 119.0(8) . . ? C11 C10 C9 118.9(8) . . ? C15 C10 C9 122.1(7) . . ? C10 C11 C12 119.6(9) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 120.8(9) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 120.4(11) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 120.2(10) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C10 120.0(9) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? O6 C16 C17 123.1(8) . . ? O6 C16 C8 118.2(8) . . ? C17 C16 C8 118.5(7) . . ? C22 C17 C18 120.0(10) . . ? C22 C17 C16 121.6(8) . . ? C18 C17 C16 118.5(9) . . ? C19 C18 C17 119.9(11) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 120.7(11) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 118.6(11) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C20 C21 C22 120.9(11) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C17 C22 C21 120.0(9) . . ? C17 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? O7 C23 O8 127.9(7) . . ? O7 C23 C24 116.1(7) . . ? O8 C23 C24 116.0(7) . . ? C25 C24 C26 119.5(7) . . ? C25 C24 C23 118.7(7) . . ? C26 C24 C23 121.8(7) . . ? C24 C25 C26 121.1(8) . 2_776 ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 2_776 . ? C25 C26 C24 119.4(7) 2_776 . ? C25 C26 C27 114.1(7) 2_776 . ? C24 C26 C27 126.5(6) . . ? O9 C27 C26 120.6(7) . . ? O9 C27 C28 120.8(8) . . ? C26 C27 C28 118.0(7) . . ? C33 C28 C29 119.3(8) . . ? C33 C28 C27 122.3(8) . . ? C29 C28 C27 118.4(8) . . ? C30 C29 C28 120.7(9) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 120.0(9) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 119.6(9) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 119.9(10) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C28 C33 C32 120.4(9) . . ? C28 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C1 O1 Er1 92.1(4) . . ? C1 O2 Er1 93.3(5) . . ? C2 O3 Er1 174.6(6) 2_666 . ? C2 O4 Er1 116.3(5) . . ? C23 O7 Er1 141.5(5) . . ? C23 O8 Er1 134.9(5) . 2_666 ? Er1 O1W H1WA 123.9 . . ? Er1 O1W H1WB 128.8 . . ? H1WA O1W H1WB 107.3 . . ? Er1 O2W H2WA 125.5 . . ? Er1 O2W H2WB 119.5 . . ? H2WA O2W H2WB 107.4 . . ? 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 O3 Er1 C1 O2 31.0(6) . . . . ? O7 Er1 C1 O2 98.6(6) . . . . ? O4 Er1 C1 O2 174.5(5) . . . . ? O8 Er1 C1 O2 -84.7(7) 2_666 . . . ? O1 Er1 C1 O2 178.5(8) . . . . ? O2W Er1 C1 O2 -115.9(6) . . . . ? O1W Er1 C1 O2 -44.1(6) . . . . ? O3 Er1 C1 O1 -147.5(5) . . . . ? O7 Er1 C1 O1 -79.9(5) . . . . ? O4 Er1 C1 O1 -4.0(5) . . . . ? O8 Er1 C1 O1 96.8(6) 2_666 . . . ? O2 Er1 C1 O1 -178.5(8) . . . . ? O2W Er1 C1 O1 65.6(5) . . . . ? O1W Er1 C1 O1 137.4(5) . . . . ? O2 C1 C3 C4 -13.3(12) . . . . ? O1 C1 C3 C4 166.7(7) . . . . ? O2 C1 C3 C8 168.9(8) . . . . ? O1 C1 C3 C8 -11.1(11) . . . . ? C8 C3 C4 C5 -0.5(12) . . . 1_565 ? C1 C3 C4 C5 -178.4(7) . . . 1_565 ? O3 C2 C5 C4 -33.0(11) 2_666 . . 1_545 ? O4 C2 C5 C4 143.9(7) . . . 1_545 ? O3 C2 C5 C6 151.2(8) 2_666 . . . ? O4 C2 C5 C6 -31.8(11) . . . . ? C4 C5 C6 C7 -2.5(12) 1_545 . . 1_545 ? C2 C5 C6 C7 173.2(7) . . . 1_545 ? C4 C5 C6 C9 176.3(7) 1_545 . . . ? C2 C5 C6 C9 -8.0(12) . . . . ? C6 C7 C8 C3 1.4(11) 1_565 . . . ? C6 C7 C8 C16 -178.3(7) 1_565 . . . ? C4 C3 C8 C7 -1.4(11) . . . . ? C1 C3 C8 C7 176.5(7) . . . . ? C4 C3 C8 C16 178.3(8) . . . . ? C1 C3 C8 C16 -3.8(12) . . . . ? C7 C6 C9 O5 -48.9(11) 1_545 . . . ? C5 C6 C9 O5 132.3(9) . . . . ? C7 C6 C9 C10 124.7(8) 1_545 . . . ? C5 C6 C9 C10 -54.2(11) . . . . ? O5 C9 C10 C11 -21.9(13) . . . . ? C6 C9 C10 C11 164.8(8) . . . . ? O5 C9 C10 C15 158.0(9) . . . . ? C6 C9 C10 C15 -15.2(11) . . . . ? C15 C10 C11 C12 1.5(14) . . . . ? C9 C10 C11 C12 -178.5(9) . . . . ? C10 C11 C12 C13 -2.0(16) . . . . ? C11 C12 C13 C14 1.0(18) . . . . ? C12 C13 C14 C15 0.3(17) . . . . ? C13 C14 C15 C10 -0.7(15) . . . . ? C11 C10 C15 C14 -0.2(13) . . . . ? C9 C10 C15 C14 179.8(8) . . . . ? C7 C8 C16 O6 -66.0(11) . . . . ? C3 C8 C16 O6 114.3(10) . . . . ? C7 C8 C16 C17 110.8(9) . . . . ? C3 C8 C16 C17 -68.9(11) . . . . ? O6 C16 C17 C22 158.4(10) . . . . ? C8 C16 C17 C22 -18.2(13) . . . . ? O6 C16 C17 C18 -20.5(15) . . . . ? C8 C16 C17 C18 162.9(9) . . . . ? C22 C17 C18 C19 -0.1(17) . . . . ? C16 C17 C18 C19 178.9(9) . . . . ? C17 C18 C19 C20 0.9(19) . . . . ? C18 C19 C20 C21 -2.2(19) . . . . ? C19 C20 C21 C22 2.8(18) . . . . ? C18 C17 C22 C21 0.6(16) . . . . ? C16 C17 C22 C21 -178.3(9) . . . . ? C20 C21 C22 C17 -2.0(17) . . . . ? O7 C23 C24 C25 -6.5(10) . . . . ? O8 C23 C24 C25 175.9(7) . . . . ? O7 C23 C24 C26 174.0(7) . . . . ? O8 C23 C24 C26 -3.6(10) . . . . ? C26 C24 C25 C26 0.6(12) . . . 2_776 ? C23 C24 C25 C26 -179.0(7) . . . 2_776 ? C25 C24 C26 C25 -0.5(12) . . . 2_776 ? C23 C24 C26 C25 179.0(7) . . . 2_776 ? C25 C24 C26 C27 -179.2(7) . . . . ? C23 C24 C26 C27 0.3(11) . . . . ? C25 C26 C27 O9 86.9(9) 2_776 . . . ? C24 C26 C27 O9 -94.3(10) . . . . ? C25 C26 C27 C28 -84.1(9) 2_776 . . . ? C24 C26 C27 C28 94.7(9) . . . . ? O9 C27 C28 C33 149.2(8) . . . . ? C26 C27 C28 C33 -39.8(11) . . . . ? O9 C27 C28 C29 -33.2(11) . . . . ? C26 C27 C28 C29 137.8(8) . . . . ? C33 C28 C29 C30 0.2(14) . . . . ? C27 C28 C29 C30 -177.5(8) . . . . ? C28 C29 C30 C31 -2.0(16) . . . . ? C29 C30 C31 C32 2.1(16) . . . . ? C30 C31 C32 C33 -0.3(15) . . . . ? C29 C28 C33 C32 1.6(13) . . . . ? C27 C28 C33 C32 179.2(8) . . . . ? C31 C32 C33 C28 -1.6(14) . . . . ? O2 C1 O1 Er1 -1.5(8) . . . . ? C3 C1 O1 Er1 178.5(6) . . . . ? O3 Er1 O1 C1 43.8(6) . . . . ? O7 Er1 O1 C1 94.5(5) . . . . ? O4 Er1 O1 C1 176.3(5) . . . . ? O8 Er1 O1 C1 -127.6(5) 2_666 . . . ? O2 Er1 O1 C1 0.8(5) . . . . ? O2W Er1 O1 C1 -107.2(5) . . . . ? O1W Er1 O1 C1 -46.1(5) . . . . ? O1 C1 O2 Er1 1.5(8) . . . . ? C3 C1 O2 Er1 -178.5(6) . . . . ? O3 Er1 O2 C1 -151.6(6) . . . . ? O7 Er1 O2 C1 -78.0(5) . . . . ? O4 Er1 O2 C1 -7.7(7) . . . . ? O8 Er1 O2 C1 133.6(5) 2_666 . . . ? O1 Er1 O2 C1 -0.9(5) . . . . ? O2W Er1 O2 C1 62.2(5) . . . . ? O1W Er1 O2 C1 132.7(6) . . . . ? O3 C2 O4 Er1 10.8(10) 2_666 . . . ? C5 C2 O4 Er1 -166.0(5) . . . . ? O3 Er1 O4 C2 -7.4(6) . . . . ? O7 Er1 O4 C2 -70.3(5) . . . . ? O8 Er1 O4 C2 62.0(5) 2_666 . . . ? O2 Er1 O4 C2 -142.3(5) . . . . ? O1 Er1 O4 C2 -147.9(5) . . . . ? O2W Er1 O4 C2 141.7(6) . . . . ? O1W Er1 O4 C2 99.3(6) . . . . ? C1 Er1 O4 C2 -146.0(5) . . . . ? O8 C23 O7 Er1 -36.3(13) . . . . ? C24 C23 O7 Er1 146.4(6) . . . . ? O3 Er1 O7 C23 -19.7(8) . . . . ? O4 Er1 O7 C23 109.8(8) . . . . ? O8 Er1 O7 C23 45.1(9) 2_666 . . . ? O2 Er1 O7 C23 -110.0(8) . . . . ? O1 Er1 O7 C23 -164.4(9) . . . . ? O2W Er1 O7 C23 162.8(7) . . . . ? O1W Er1 O7 C23 -58.5(9) . . . . ? C1 Er1 O7 C23 -136.8(9) . . . . ? O7 C23 O8 Er1 2.5(13) . . . 2_666 ? C24 C23 O8 Er1 179.7(5) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.529 _refine_diff_density_min -4.068 _refine_diff_density_rms 0.327 _database_code_depnum_ccdc_archive 'CCDC 890965' ####################################################################### # # 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_11 #TrackingRef '11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H22 Ho O11' _chemical_formula_sum 'C33 H22 Ho O11' _chemical_formula_weight 759.44 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' Ho Ho -0.2175 4.6783 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1326(5) _cell_length_b 10.1834(4) _cell_length_c 15.5265(8) _cell_angle_alpha 96.308(4) _cell_angle_beta 97.128(4) _cell_angle_gamma 113.890(4) _cell_volume 1430.69(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3175 _cell_measurement_theta_min 2.7494 _cell_measurement_theta_max 29.1846 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 750 _exptl_absorpt_coefficient_mu 2.831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98405 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9423 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0945 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5591 _reflns_number_gt 4764 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 5591 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.44449(3) 0.63135(2) 0.588462(18) 0.01862(8) Uani 1 1 d . . . C1 C 0.4221(5) 0.5789(5) 0.3596(4) 0.0212(13) Uani 1 1 d . . . C2 C 0.5344(6) 0.9190(5) 0.6638(4) 0.0249(13) Uani 1 1 d . . . C3 C 0.3870(5) 0.6793(5) 0.3061(4) 0.0199(12) Uani 1 1 d . . . C4 C 0.5665(5) 1.1749(5) 0.6560(4) 0.0273(14) Uani 1 1 d . . . H4 H 0.5252 1.1438 0.5964 0.033 Uiso 1 1 calc R . . C5 C 0.5815(5) 1.0752(5) 0.7072(4) 0.0225(13) Uani 1 1 d . . . C6 C 0.6415(5) 1.1218(5) 0.7963(4) 0.0218(13) Uani 1 1 d . . . C7 C 0.3064(5) 0.7313(5) 0.1678(4) 0.0239(13) Uani 1 1 d . . . H7 H 0.2603 0.6989 0.1090 0.029 Uiso 1 1 calc R . . C8 C 0.3218(5) 0.6317(5) 0.2182(4) 0.0209(13) Uani 1 1 d . . . C9 C 0.6631(6) 1.0242(5) 0.8590(4) 0.0286(15) Uani 1 1 d . . . C10 C 0.5282(6) 0.9146(5) 0.8836(4) 0.0302(15) Uani 1 1 d . . . C11 C 0.3956(6) 0.9232(6) 0.8718(4) 0.0390(17) Uani 1 1 d . . . H11 H 0.3871 0.9987 0.8464 0.047 Uiso 1 1 calc R . . C12 C 0.2745(7) 0.8214(7) 0.8971(5) 0.0508(19) Uani 1 1 d . . . H12 H 0.1854 0.8288 0.8898 0.061 Uiso 1 1 calc R . . C13 C 0.2884(8) 0.7092(7) 0.9332(5) 0.054(2) Uani 1 1 d . . . H13 H 0.2071 0.6390 0.9492 0.065 Uiso 1 1 calc R . . C14 C 0.4188(8) 0.6990(6) 0.9458(5) 0.055(2) Uani 1 1 d . . . H14 H 0.4255 0.6214 0.9695 0.065 Uiso 1 1 calc R . . C15 C 0.5409(7) 0.8027(6) 0.9239(5) 0.0426(18) Uani 1 1 d . . . H15 H 0.6313 0.7987 0.9357 0.051 Uiso 1 1 calc R . . C16 C 0.2587(6) 0.4739(5) 0.1722(4) 0.0256(13) Uani 1 1 d . . . C17 C 0.1525(6) 0.3607(5) 0.2125(4) 0.0235(13) Uani 1 1 d . . . C18 C 0.1223(6) 0.2153(6) 0.1860(5) 0.0404(17) Uani 1 1 d . . . H18 H 0.1682 0.1893 0.1433 0.048 Uiso 1 1 calc R . . C19 C 0.0235(7) 0.1093(6) 0.2233(5) 0.050(2) Uani 1 1 d . . . H19 H 0.0051 0.0122 0.2059 0.060 Uiso 1 1 calc R . . C20 C -0.0470(7) 0.1429(6) 0.2844(5) 0.046(2) Uani 1 1 d . . . H20 H -0.1139 0.0693 0.3080 0.056 Uiso 1 1 calc R . . C21 C -0.0198(6) 0.2859(6) 0.3117(5) 0.0408(17) Uani 1 1 d . . . H21 H -0.0689 0.3097 0.3533 0.049 Uiso 1 1 calc R . . C22 C 0.0813(6) 0.3944(6) 0.2767(4) 0.0334(15) Uani 1 1 d . . . H22 H 0.1020 0.4915 0.2965 0.040 Uiso 1 1 calc R . . C23 C 0.7539(5) 0.7257(5) 0.5028(4) 0.0216(13) Uani 1 1 d . . . C24 C 0.8826(5) 0.8666(5) 0.5002(4) 0.0201(12) Uani 1 1 d . . . C25 C 0.9040(5) 0.9906(5) 0.5575(4) 0.0226(13) Uani 1 1 d . . . H25 H 0.8400 0.9848 0.5965 0.027 Uiso 1 1 calc R . . C26 C 0.9784(5) 0.8745(5) 0.4426(4) 0.0189(12) Uani 1 1 d . . . C27 C 0.9695(6) 0.7504(5) 0.3763(4) 0.0258(14) Uani 1 1 d . . . C28 C 0.8954(6) 0.7326(5) 0.2844(4) 0.0259(14) Uani 1 1 d . . . C29 C 0.9554(7) 0.6970(6) 0.2162(4) 0.0351(16) Uani 1 1 d . . . H29 H 1.0392 0.6807 0.2280 0.042 Uiso 1 1 calc R . . C30 C 0.8918(8) 0.6853(6) 0.1293(5) 0.0511(19) Uani 1 1 d . . . H30 H 0.9359 0.6664 0.0834 0.061 Uiso 1 1 calc R . . C31 C 0.7644(8) 0.7016(6) 0.1117(5) 0.0484(19) Uani 1 1 d . . . H31 H 0.7203 0.6917 0.0537 0.058 Uiso 1 1 calc R . . C32 C 0.7015(7) 0.7328(6) 0.1801(5) 0.0412(18) Uani 1 1 d . . . H32 H 0.6133 0.7411 0.1678 0.049 Uiso 1 1 calc R . . C33 C 0.7672(6) 0.7517(5) 0.2660(4) 0.0322(15) Uani 1 1 d . . . H33 H 0.7262 0.7772 0.3117 0.039 Uiso 1 1 calc R . . O1 O 0.4522(4) 0.4839(3) 0.3203(3) 0.0273(10) Uani 1 1 d . . . O2 O 0.4234(4) 0.5975(4) 0.4408(3) 0.0336(10) Uani 1 1 d . . . O3 O 0.4601(4) 0.8712(4) 0.5871(3) 0.0381(11) Uani 1 1 d . . . O4 O 0.5740(4) 0.8388(3) 0.7074(3) 0.0281(10) Uani 1 1 d . . . O5 O 0.7845(4) 1.0440(4) 0.8919(3) 0.0419(12) Uani 1 1 d . . . O6 O 0.2907(5) 0.4458(4) 0.1026(3) 0.0459(12) Uani 1 1 d . . . O7 O 0.7323(4) 0.6163(3) 0.4471(3) 0.0259(9) Uani 1 1 d . . . O8 O 0.6780(4) 0.7290(3) 0.5608(3) 0.0285(10) Uani 1 1 d . . . O9 O 1.0395(4) 0.6793(4) 0.3956(3) 0.0402(11) Uani 1 1 d . . . O1W O 0.1983(4) 0.6119(4) 0.5336(3) 0.0443(12) Uani 1 1 d . . . H1WA H 0.1383 0.5383 0.5512 0.053 Uiso 1 1 d R . . H1WB H 0.1512 0.6323 0.4920 0.053 Uiso 1 1 d R . . O2W O 0.3149(4) 0.6035(4) 0.7094(3) 0.0392(11) Uani 1 1 d . . . H2WA H 0.2764 0.5153 0.7175 0.047 Uiso 1 1 d R . . H2WB H 0.3122 0.6565 0.7558 0.047 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 0.02179(14) 0.01309(12) 0.02011(16) 0.00324(10) 0.00474(11) 0.00623(9) C1 0.019(3) 0.012(3) 0.021(4) 0.002(3) -0.002(3) -0.003(2) C2 0.026(3) 0.018(3) 0.028(4) 0.001(3) 0.007(3) 0.006(2) C3 0.022(3) 0.017(3) 0.018(3) 0.003(2) 0.002(3) 0.006(2) C4 0.030(3) 0.024(3) 0.026(4) 0.003(3) 0.005(3) 0.008(2) C5 0.025(3) 0.018(3) 0.029(4) 0.010(3) 0.008(3) 0.011(2) C6 0.028(3) 0.017(3) 0.022(4) 0.006(3) 0.005(3) 0.010(2) C7 0.033(3) 0.024(3) 0.013(3) 0.004(3) 0.004(3) 0.011(2) C8 0.024(3) 0.013(2) 0.027(4) 0.005(3) 0.009(3) 0.009(2) C9 0.041(4) 0.018(3) 0.029(4) 0.011(3) 0.004(3) 0.013(2) C10 0.040(4) 0.020(3) 0.030(4) 0.007(3) 0.007(3) 0.012(3) C11 0.039(4) 0.045(4) 0.041(5) 0.021(4) 0.013(3) 0.021(3) C12 0.041(4) 0.067(5) 0.043(5) 0.016(4) 0.012(4) 0.019(3) C13 0.054(5) 0.048(4) 0.036(5) 0.009(4) 0.016(4) -0.005(3) C14 0.076(5) 0.035(4) 0.054(6) 0.029(4) 0.023(4) 0.017(4) C15 0.055(4) 0.035(3) 0.047(5) 0.023(4) 0.014(4) 0.023(3) C16 0.034(3) 0.024(3) 0.019(4) 0.001(3) -0.002(3) 0.014(2) C17 0.022(3) 0.020(3) 0.026(4) -0.004(3) -0.002(3) 0.010(2) C18 0.042(4) 0.025(3) 0.058(5) 0.001(3) 0.016(4) 0.017(3) C19 0.055(5) 0.021(3) 0.067(6) 0.008(4) 0.007(4) 0.011(3) C20 0.039(4) 0.030(4) 0.067(6) 0.023(4) 0.015(4) 0.006(3) C21 0.030(3) 0.044(4) 0.049(5) 0.009(4) 0.014(3) 0.015(3) C22 0.042(4) 0.023(3) 0.038(4) 0.003(3) 0.011(3) 0.015(3) C23 0.016(3) 0.018(3) 0.028(4) 0.009(3) 0.005(3) 0.004(2) C24 0.020(3) 0.011(2) 0.024(4) 0.001(2) 0.006(3) 0.002(2) C25 0.017(3) 0.022(3) 0.022(4) -0.006(3) 0.004(3) 0.004(2) C26 0.020(3) 0.015(2) 0.022(3) 0.000(2) 0.002(2) 0.009(2) C27 0.028(3) 0.015(3) 0.029(4) 0.004(3) 0.010(3) 0.002(2) C28 0.030(3) 0.016(3) 0.032(4) 0.004(3) 0.009(3) 0.010(2) C29 0.041(4) 0.036(3) 0.035(4) 0.010(3) 0.013(3) 0.021(3) C30 0.074(5) 0.043(4) 0.034(5) 0.004(4) 0.018(4) 0.021(4) C31 0.064(5) 0.048(4) 0.029(5) 0.007(4) 0.007(4) 0.020(4) C32 0.036(4) 0.039(4) 0.044(5) 0.009(4) -0.005(4) 0.014(3) C33 0.033(3) 0.026(3) 0.036(4) 0.005(3) 0.014(3) 0.008(3) O1 0.029(2) 0.0222(19) 0.033(3) 0.0070(19) 0.0054(19) 0.0126(16) O2 0.049(3) 0.026(2) 0.022(3) 0.006(2) 0.004(2) 0.0119(18) O3 0.059(3) 0.021(2) 0.028(3) -0.004(2) -0.012(2) 0.0184(19) O4 0.045(2) 0.0212(19) 0.024(3) 0.0062(18) 0.006(2) 0.0193(17) O5 0.036(3) 0.037(2) 0.054(4) 0.016(2) -0.001(2) 0.0176(19) O6 0.074(3) 0.026(2) 0.033(3) -0.002(2) 0.021(3) 0.015(2) O7 0.027(2) 0.0130(18) 0.029(3) 0.0005(18) 0.0084(19) -0.0005(15) O8 0.025(2) 0.0208(19) 0.034(3) 0.0044(19) 0.013(2) 0.0014(15) O9 0.048(3) 0.035(2) 0.043(3) 0.000(2) 0.001(2) 0.027(2) O1W 0.041(3) 0.055(3) 0.047(3) 0.017(2) 0.005(2) 0.030(2) O2W 0.045(3) 0.028(2) 0.040(3) -0.003(2) 0.021(2) 0.0093(18) _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 O2 2.250(4) . ? Ho1 O8 2.283(3) . ? Ho1 O1 2.339(3) 2_666 ? Ho1 O7 2.380(3) 2_666 ? Ho1 O3 2.386(3) . ? Ho1 O2W 2.399(4) . ? Ho1 O4 2.427(4) . ? Ho1 O1W 2.454(4) . ? Ho1 C2 2.757(5) . ? C1 O1 1.248(6) . ? C1 O2 1.252(7) . ? C1 C3 1.506(6) . ? C2 O3 1.255(6) . ? C2 O4 1.268(5) . ? C2 C5 1.510(7) . ? C3 C8 1.380(7) . ? C3 C4 1.395(7) 2_676 ? C4 C3 1.395(7) 2_676 ? C4 C5 1.399(6) . ? C4 H4 0.9300 . ? C5 C6 1.387(8) . ? C6 C7 1.389(7) 2_676 ? C6 C9 1.523(6) . ? C7 C6 1.389(7) 2_676 ? C7 C8 1.392(6) . ? C7 H7 0.9300 . ? C8 C16 1.518(7) . ? C9 O5 1.198(6) . ? C9 C10 1.499(7) . ? C10 C11 1.372(7) . ? C10 C15 1.401(6) . ? C11 C12 1.383(8) . ? C11 H11 0.9300 . ? C12 C13 1.375(8) . ? C12 H12 0.9300 . ? C13 C14 1.359(8) . ? C13 H13 0.9300 . ? C14 C15 1.373(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O6 1.205(7) . ? C16 C17 1.483(7) . ? C17 C18 1.386(7) . ? C17 C22 1.392(8) . ? C18 C19 1.382(8) . ? C18 H18 0.9300 . ? C19 C20 1.350(10) . ? C19 H19 0.9300 . ? C20 C21 1.374(8) . ? C20 H20 0.9300 . ? C21 C22 1.385(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O7 1.258(7) . ? C23 O8 1.260(7) . ? C23 C24 1.506(6) . ? C24 C25 1.384(7) . ? C24 C26 1.385(7) . ? C25 C26 1.408(6) 2_776 ? C25 H25 0.9300 . ? C26 C25 1.408(6) 2_776 ? C26 C27 1.504(8) . ? C27 O9 1.235(6) . ? C27 C28 1.484(8) . ? C28 C29 1.370(8) . ? C28 C33 1.389(7) . ? C29 C30 1.390(9) . ? C29 H29 0.9300 . ? C30 C31 1.366(9) . ? C30 H30 0.9300 . ? C31 C32 1.375(10) . ? C31 H31 0.9300 . ? C32 C33 1.370(8) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? O1 Ho1 2.339(3) 2_666 ? O7 Ho1 2.380(3) 2_666 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8501 . ? O2W H2WA 0.8530 . ? O2W H2WB 0.8624 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ho1 O8 73.63(14) . . ? O2 Ho1 O1 123.79(14) . 2_666 ? O8 Ho1 O1 81.02(12) . 2_666 ? O2 Ho1 O7 80.66(13) . 2_666 ? O8 Ho1 O7 128.26(12) . 2_666 ? O1 Ho1 O7 77.24(12) 2_666 2_666 ? O2 Ho1 O3 89.31(14) . . ? O8 Ho1 O3 84.30(13) . . ? O1 Ho1 O3 137.29(13) 2_666 . ? O7 Ho1 O3 140.01(12) 2_666 . ? O2 Ho1 O2W 145.64(13) . . ? O8 Ho1 O2W 140.62(14) . . ? O1 Ho1 O2W 75.68(13) 2_666 . ? O7 Ho1 O2W 76.68(13) 2_666 . ? O3 Ho1 O2W 91.69(14) . . ? O2 Ho1 O4 134.84(12) . . ? O8 Ho1 O4 76.57(14) . . ? O1 Ho1 O4 83.16(12) 2_666 . ? O7 Ho1 O4 144.21(13) 2_666 . ? O3 Ho1 O4 54.39(12) . . ? O2W Ho1 O4 69.55(13) . . ? O2 Ho1 O1W 75.60(15) . . ? O8 Ho1 O1W 140.75(13) . . ? O1 Ho1 O1W 137.25(12) 2_666 . ? O7 Ho1 O1W 68.51(12) 2_666 . ? O3 Ho1 O1W 71.50(13) . . ? O2W Ho1 O1W 72.22(14) . . ? O4 Ho1 O1W 110.42(13) . . ? O2 Ho1 C2 113.08(15) . . ? O8 Ho1 C2 79.86(14) . . ? O1 Ho1 C2 110.48(15) 2_666 . ? O7 Ho1 C2 151.86(14) 2_666 . ? O3 Ho1 C2 27.03(13) . . ? O2W Ho1 C2 79.19(15) . . ? O4 Ho1 C2 27.38(13) . . ? O1W Ho1 C2 90.49(14) . . ? O1 C1 O2 123.7(5) . . ? O1 C1 C3 117.6(5) . . ? O2 C1 C3 118.7(5) . . ? O3 C2 O4 121.4(5) . . ? O3 C2 C5 121.1(4) . . ? O4 C2 C5 117.5(5) . . ? O3 C2 Ho1 59.8(3) . . ? O4 C2 Ho1 61.6(3) . . ? C5 C2 Ho1 178.4(4) . . ? C8 C3 C4 120.0(4) . 2_676 ? C8 C3 C1 120.6(5) . . ? C4 C3 C1 119.1(5) 2_676 . ? C3 C4 C5 120.4(6) 2_676 . ? C3 C4 H4 119.8 2_676 . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.5(5) . . ? C6 C5 C2 121.2(4) . . ? C4 C5 C2 119.3(5) . . ? C5 C6 C7 119.3(4) . 2_676 ? C5 C6 C9 124.6(5) . . ? C7 C6 C9 116.0(5) 2_676 . ? C6 C7 C8 121.3(5) 2_676 . ? C6 C7 H7 119.3 2_676 . ? C8 C7 H7 119.3 . . ? C3 C8 C7 119.3(5) . . ? C3 C8 C16 124.1(4) . . ? C7 C8 C16 116.6(5) . . ? O5 C9 C10 122.4(4) . . ? O5 C9 C6 120.1(5) . . ? C10 C9 C6 117.3(5) . . ? C11 C10 C15 119.0(5) . . ? C11 C10 C9 122.9(4) . . ? C15 C10 C9 118.0(5) . . ? C10 C11 C12 121.0(5) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 118.7(6) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C14 C13 C12 121.2(6) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 120.4(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C10 119.5(6) . . ? C14 C15 H15 120.2 . . ? C10 C15 H15 120.2 . . ? O6 C16 C17 122.4(5) . . ? O6 C16 C8 119.2(5) . . ? C17 C16 C8 118.4(5) . . ? C18 C17 C22 118.1(5) . . ? C18 C17 C16 119.4(6) . . ? C22 C17 C16 122.5(5) . . ? C19 C18 C17 119.7(6) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 121.8(6) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 C21 119.9(6) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 119.4(6) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C17 121.1(5) . . ? C21 C22 H22 119.4 . . ? C17 C22 H22 119.4 . . ? O7 C23 O8 126.2(4) . . ? O7 C23 C24 117.1(5) . . ? O8 C23 C24 116.7(5) . . ? C25 C24 C26 119.8(4) . . ? C25 C24 C23 118.3(5) . . ? C26 C24 C23 121.9(5) . . ? C24 C25 C26 120.8(5) . 2_776 ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 2_776 . ? C24 C26 C25 119.4(5) . 2_776 ? C24 C26 C27 126.2(4) . . ? C25 C26 C27 114.4(5) 2_776 . ? O9 C27 C28 121.2(5) . . ? O9 C27 C26 120.2(5) . . ? C28 C27 C26 117.9(4) . . ? C29 C28 C33 119.3(6) . . ? C29 C28 C27 119.0(5) . . ? C33 C28 C27 121.6(6) . . ? C28 C29 C30 120.4(6) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C31 C30 C29 119.8(7) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 119.8(7) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C33 C32 C31 120.8(6) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C28 119.7(6) . . ? C32 C33 H33 120.1 . . ? C28 C33 H33 120.1 . . ? C1 O1 Ho1 115.3(3) . 2_666 ? C1 O2 Ho1 175.2(4) . . ? C2 O3 Ho1 93.2(3) . . ? C2 O4 Ho1 91.0(3) . . ? C23 O7 Ho1 135.4(3) . 2_666 ? C23 O8 Ho1 143.0(4) . . ? Ho1 O1W H1WA 106.2 . . ? Ho1 O1W H1WB 141.2 . . ? H1WA O1W H1WB 108.4 . . ? Ho1 O2W H2WA 112.5 . . ? Ho1 O2W H2WB 138.7 . . ? H2WA O2W H2WB 106.5 . . ? 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 O2 Ho1 C2 O3 30.2(4) . . . . ? O8 Ho1 C2 O3 97.4(4) . . . . ? O1 Ho1 C2 O3 173.7(3) 2_666 . . . ? O7 Ho1 C2 O3 -84.8(5) 2_666 . . . ? O2W Ho1 C2 O3 -116.1(4) . . . . ? O4 Ho1 C2 O3 177.7(5) . . . . ? O1W Ho1 C2 O3 -44.3(4) . . . . ? O2 Ho1 C2 O4 -147.5(3) . . . . ? O8 Ho1 C2 O4 -80.3(3) . . . . ? O1 Ho1 C2 O4 -4.0(3) 2_666 . . . ? O7 Ho1 C2 O4 97.4(4) 2_666 . . . ? O3 Ho1 C2 O4 -177.7(5) . . . . ? O2W Ho1 C2 O4 66.1(3) . . . . ? O1W Ho1 C2 O4 137.9(3) . . . . ? O1 C1 C3 C8 30.6(7) . . . . ? O2 C1 C3 C8 -151.3(5) . . . . ? O1 C1 C3 C4 -143.5(5) . . . 2_676 ? O2 C1 C3 C4 34.6(7) . . . 2_676 ? C3 C4 C5 C6 0.8(8) 2_676 . . . ? C3 C4 C5 C2 -178.2(5) 2_676 . . . ? O3 C2 C5 C6 169.0(5) . . . . ? O4 C2 C5 C6 -11.8(8) . . . . ? O3 C2 C5 C4 -12.1(8) . . . . ? O4 C2 C5 C4 167.2(5) . . . . ? C4 C5 C6 C7 -3.8(8) . . . 2_676 ? C2 C5 C6 C7 175.2(5) . . . 2_676 ? C4 C5 C6 C9 179.7(5) . . . . ? C2 C5 C6 C9 -1.3(8) . . . . ? C4 C3 C8 C7 1.5(8) 2_676 . . . ? C1 C3 C8 C7 -172.5(5) . . . . ? C4 C3 C8 C16 -175.9(5) 2_676 . . . ? C1 C3 C8 C16 10.0(8) . . . . ? C6 C7 C8 C3 1.5(8) 2_676 . . . ? C6 C7 C8 C16 179.2(5) 2_676 . . . ? C5 C6 C9 O5 114.1(7) . . . . ? C7 C6 C9 O5 -62.4(8) 2_676 . . . ? C5 C6 C9 C10 -71.6(8) . . . . ? C7 C6 C9 C10 111.8(6) 2_676 . . . ? O5 C9 C10 C11 156.8(7) . . . . ? C6 C9 C10 C11 -17.4(9) . . . . ? O5 C9 C10 C15 -20.2(9) . . . . ? C6 C9 C10 C15 165.6(6) . . . . ? C15 C10 C11 C12 -1.6(10) . . . . ? C9 C10 C11 C12 -178.6(6) . . . . ? C10 C11 C12 C13 -1.0(11) . . . . ? C11 C12 C13 C14 1.4(12) . . . . ? C12 C13 C14 C15 1.0(12) . . . . ? C13 C14 C15 C10 -3.7(11) . . . . ? C11 C10 C15 C14 4.0(10) . . . . ? C9 C10 C15 C14 -178.9(6) . . . . ? C3 C8 C16 O6 -131.6(6) . . . . ? C7 C8 C16 O6 50.8(7) . . . . ? C3 C8 C16 C17 52.0(7) . . . . ? C7 C8 C16 C17 -125.5(5) . . . . ? O6 C16 C17 C18 20.2(8) . . . . ? C8 C16 C17 C18 -163.5(5) . . . . ? O6 C16 C17 C22 -160.0(6) . . . . ? C8 C16 C17 C22 16.3(7) . . . . ? C22 C17 C18 C19 0.1(8) . . . . ? C16 C17 C18 C19 180.0(5) . . . . ? C17 C18 C19 C20 1.1(10) . . . . ? C18 C19 C20 C21 -0.8(11) . . . . ? C19 C20 C21 C22 -0.7(9) . . . . ? C20 C21 C22 C17 2.0(9) . . . . ? C18 C17 C22 C21 -1.6(8) . . . . ? C16 C17 C22 C21 178.5(5) . . . . ? O7 C23 C24 C25 176.4(4) . . . . ? O8 C23 C24 C25 -3.5(7) . . . . ? O7 C23 C24 C26 -3.6(7) . . . . ? O8 C23 C24 C26 176.5(5) . . . . ? C26 C24 C25 C26 0.6(8) . . . 2_776 ? C23 C24 C25 C26 -179.4(4) . . . 2_776 ? C25 C24 C26 C25 -0.6(8) . . . 2_776 ? C23 C24 C26 C25 179.4(4) . . . 2_776 ? C25 C24 C26 C27 -179.6(5) . . . . ? C23 C24 C26 C27 0.4(8) . . . . ? C24 C26 C27 O9 -94.1(7) . . . . ? C25 C26 C27 O9 86.8(6) 2_776 . . . ? C24 C26 C27 C28 95.7(6) . . . . ? C25 C26 C27 C28 -83.4(6) 2_776 . . . ? O9 C27 C28 C29 -31.2(7) . . . . ? C26 C27 C28 C29 138.9(5) . . . . ? O9 C27 C28 C33 149.1(5) . . . . ? C26 C27 C28 C33 -40.8(7) . . . . ? C33 C28 C29 C30 2.3(8) . . . . ? C27 C28 C29 C30 -177.4(5) . . . . ? C28 C29 C30 C31 -3.5(9) . . . . ? C29 C30 C31 C32 1.4(9) . . . . ? C30 C31 C32 C33 1.8(9) . . . . ? C31 C32 C33 C28 -3.0(8) . . . . ? C29 C28 C33 C32 0.9(7) . . . . ? C27 C28 C33 C32 -179.4(4) . . . . ? O2 C1 O1 Ho1 -11.1(6) . . . 2_666 ? C3 C1 O1 Ho1 166.9(3) . . . 2_666 ? O1W Ho1 O2 C1 -179(100) . . . . ? C2 Ho1 O2 C1 97(4) . . . . ? O4 C2 O3 Ho1 2.3(6) . . . . ? C5 C2 O3 Ho1 -178.4(4) . . . . ? O2 Ho1 O3 C2 -152.4(4) . . . . ? O8 Ho1 O3 C2 -78.8(3) . . . . ? O1 Ho1 O3 C2 -8.7(4) 2_666 . . . ? O7 Ho1 O3 C2 133.0(3) 2_666 . . . ? O2W Ho1 O3 C2 61.9(3) . . . . ? O4 Ho1 O3 C2 -1.3(3) . . . . ? O1W Ho1 O3 C2 132.5(4) . . . . ? O3 C2 O4 Ho1 -2.3(6) . . . . ? C5 C2 O4 Ho1 178.5(4) . . . . ? O2 Ho1 O4 C2 44.1(4) . . . . ? O8 Ho1 O4 C2 93.9(3) . . . . ? O1 Ho1 O4 C2 176.2(3) 2_666 . . . ? O7 Ho1 O4 C2 -126.9(3) 2_666 . . . ? O3 Ho1 O4 C2 1.3(3) . . . . ? O2W Ho1 O4 C2 -106.5(3) . . . . ? O1W Ho1 O4 C2 -45.7(3) . . . . ? O8 C23 O7 Ho1 1.1(8) . . . 2_666 ? C24 C23 O7 Ho1 -178.8(3) . . . 2_666 ? O7 C23 O8 Ho1 -33.1(9) . . . . ? C24 C23 O8 Ho1 146.8(4) . . . . ? O2 Ho1 O8 C23 -21.1(5) . . . . ? O1 Ho1 O8 C23 108.2(5) 2_666 . . . ? O7 Ho1 O8 C23 42.3(6) 2_666 . . . ? O3 Ho1 O8 C23 -112.1(5) . . . . ? O2W Ho1 O8 C23 162.2(5) . . . . ? O4 Ho1 O8 C23 -166.8(5) . . . . ? O1W Ho1 O8 C23 -60.8(6) . . . . ? C2 Ho1 O8 C23 -139.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.563 _refine_diff_density_min -1.154 _refine_diff_density_rms 0.150 _database_code_depnum_ccdc_archive 'CCDC 890966' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'C33 H24 Nd O12' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C33 H22 Nd O11, H2 O' _chemical_formula_sum 'C33 H24 Nd O12' _chemical_formula_weight 756.76 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' Nd Nd -0.1943 3.0179 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4475(11) _cell_length_b 11.5142(6) _cell_length_c 14.0367(16) _cell_angle_alpha 102.313(7) _cell_angle_beta 110.938(10) _cell_angle_gamma 100.587(6) _cell_volume 1476.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4745 _cell_measurement_theta_min 2.9113 _cell_measurement_theta_max 29.1687 _exptl_crystal_description block _exptl_crystal_colour Light-purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7004 _exptl_absorpt_correction_T_max 0.7588 _exptl_absorpt_process_details 'CrysAlis (Oxford Diffraction, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10184 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0755 _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 -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5757 _reflns_number_gt 5015 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^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 5757 _refine_ls_number_parameters 415 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.038 _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 Nd1 Nd 0.61470(2) 0.56307(2) 0.659936(17) 0.01410(9) Uani 1 1 d . . . C1 C 0.7995(5) 0.7871(4) 0.8223(4) 0.0219(10) Uani 1 1 d . . . C2 C 0.9029(5) 0.8997(4) 0.9129(3) 0.0218(10) Uani 1 1 d . . . C3 C 1.1067(5) 1.0782(4) 0.9888(4) 0.0253(11) Uani 1 1 d . . . H3 H 1.1792 1.1312 0.9818 0.030 Uiso 1 1 calc R . . C4 C 1.0110(5) 0.9793(4) 0.9013(3) 0.0217(10) Uani 1 1 d . . . C5 C 1.0199(5) 0.9643(4) 0.7941(4) 0.0254(11) Uani 1 1 d . . . C6 C 1.1351(6) 0.9150(4) 0.7767(4) 0.0290(12) Uani 1 1 d . . . C7 C 1.2578(7) 0.9173(6) 0.8601(5) 0.0421(15) Uani 1 1 d . . . H7 H 1.2669 0.9433 0.9303 0.051 Uiso 1 1 calc R . . C8 C 1.3675(8) 0.8811(6) 0.8395(6) 0.0592(19) Uani 1 1 d . . . H8 H 1.4511 0.8855 0.8959 0.071 Uiso 1 1 calc R . . C9 C 1.3524(8) 0.8386(6) 0.7356(5) 0.0549(17) Uani 1 1 d U . . H9 H 1.4258 0.8142 0.7219 0.066 Uiso 1 1 calc R . . C10 C 1.2324(8) 0.8324(6) 0.6542(6) 0.0555(17) Uani 1 1 d U . . H10 H 1.2221 0.8017 0.5842 0.067 Uiso 1 1 calc R . . C11 C 1.1219(7) 0.8716(5) 0.6732(5) 0.0481(16) Uani 1 1 d . . . H11 H 1.0397 0.8684 0.6160 0.058 Uiso 1 1 calc R . . C12 C 0.7005(5) 0.4909(4) 0.4282(3) 0.0175(9) Uani 1 1 d . . . C13 C 0.8564(5) 0.5000(4) 0.4651(3) 0.0195(10) Uani 1 1 d . . . C14 C 0.9268(5) 0.4795(4) 0.5617(3) 0.0224(10) Uani 1 1 d . . . H14 H 0.8773 0.4657 0.6036 0.027 Uiso 1 1 calc R . . C15 C 0.9314(5) 0.5209(4) 0.4021(4) 0.0213(10) Uani 1 1 d . . . C16 C 0.8663(5) 0.5444(5) 0.2961(4) 0.0265(11) Uani 1 1 d . . . C17 C 0.8024(6) 0.6491(5) 0.2892(4) 0.0326(12) Uani 1 1 d . . . C18 C 0.8188(7) 0.7367(5) 0.3792(5) 0.0467(15) Uani 1 1 d . . . H18 H 0.8696 0.7310 0.4467 0.056 Uiso 1 1 calc R . . C19 C 0.7579(8) 0.8362(6) 0.3687(7) 0.070(2) Uani 1 1 d . . . H19 H 0.7675 0.8967 0.4284 0.084 Uiso 1 1 calc R . . C20 C 0.6836(8) 0.8398(7) 0.2659(6) 0.065(2) Uani 1 1 d U . . H20 H 0.6427 0.9043 0.2577 0.078 Uiso 1 1 calc R . . C21 C 0.6684(8) 0.7570(7) 0.1802(6) 0.0640(19) Uani 1 1 d U . . H21 H 0.6176 0.7637 0.1130 0.077 Uiso 1 1 calc R . . C22 C 0.7273(6) 0.6593(6) 0.1884(5) 0.0474(16) Uani 1 1 d . . . H22 H 0.7169 0.6008 0.1270 0.057 Uiso 1 1 calc R . . C23 C 0.4835(5) 0.7423(4) 0.4949(3) 0.0189(10) Uani 1 1 d . . . C24 C 0.4869(5) 0.8750(4) 0.4975(3) 0.0174(9) Uani 1 1 d . . . C25 C 0.6055(5) 0.9704(4) 0.5754(3) 0.0205(10) Uani 1 1 d . . . H25 H 0.6766 0.9510 0.6265 0.025 Uiso 1 1 calc R . . C26 C 0.3805(5) 0.9064(4) 0.4217(3) 0.0182(10) Uani 1 1 d . . . C27 C 0.2437(5) 0.8106(4) 0.3421(4) 0.0210(10) Uani 1 1 d . . . C28 C 0.2107(5) 0.7843(4) 0.2263(4) 0.0242(11) Uani 1 1 d . . . C29 C 0.3155(6) 0.8249(5) 0.1914(4) 0.0365(13) Uani 1 1 d . . . H29 H 0.4059 0.8746 0.2408 0.044 Uiso 1 1 calc R . . C30 C 0.2849(8) 0.7913(7) 0.0841(5) 0.0574(18) Uani 1 1 d . . . H30 H 0.3556 0.8159 0.0610 0.069 Uiso 1 1 calc R . . C31 C 0.1492(8) 0.7210(6) 0.0104(5) 0.0532(18) Uani 1 1 d . . . H31 H 0.1291 0.6995 -0.0623 0.064 Uiso 1 1 calc R . . C32 C 0.0440(7) 0.6825(6) 0.0428(4) 0.0480(17) Uani 1 1 d . . . H32 H -0.0474 0.6360 -0.0073 0.058 Uiso 1 1 calc R . . C33 C 0.0753(6) 0.7137(5) 0.1508(4) 0.0333(13) Uani 1 1 d . . . H33 H 0.0046 0.6869 0.1732 0.040 Uiso 1 1 calc R . . O1 O 0.8298(4) 0.7484(3) 0.7452(3) 0.0286(8) Uani 1 1 d . . . O2 O 0.6871(4) 0.7321(3) 0.8276(2) 0.0296(8) Uani 1 1 d . . . O3 O 0.9384(4) 0.9978(4) 0.7275(3) 0.0389(9) Uani 1 1 d . . . O4 O 0.6209(3) 0.4465(3) 0.3313(2) 0.0250(7) Uani 1 1 d . . . O5 O 0.6524(3) 0.5257(3) 0.4975(2) 0.0200(7) Uani 1 1 d . . . O6 O 0.8754(4) 0.4800(4) 0.2192(3) 0.0430(10) Uani 1 1 d . . . O7 O 0.5726(4) 0.3382(3) 0.5950(2) 0.0247(8) Uani 1 1 d . . . O8 O 0.5399(4) 0.7230(3) 0.5830(2) 0.0235(7) Uani 1 1 d . . . O9 O 0.1620(4) 0.7563(3) 0.3723(3) 0.0337(8) Uani 1 1 d . . . O1W O 0.8415(4) 0.5195(3) 0.7696(3) 0.0330(9) Uani 1 1 d . . . H1WB H 0.9311 0.5474 0.7894 0.040 Uiso 1 1 d R . . H1WA H 0.8203 0.4408 0.7475 0.040 Uiso 1 1 d R . . O2W O 0.5931(4) 0.4602(3) 0.8002(3) 0.0395(9) Uani 1 1 d . . . H2WA H 0.5597 0.5010 0.8388 0.047 Uiso 1 1 d R . . H2WB H 0.5422 0.3852 0.7758 0.047 Uiso 1 1 d R . . O3W O 0.5024(7) 0.3609(5) 0.0855(4) 0.0866(17) Uani 1 1 d . . . H3WA H 0.4264 0.3224 0.0884 0.104 Uiso 1 1 d R . . H3WB H 0.5715 0.3697 0.1450 0.104 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 Nd1 0.01350(14) 0.01361(14) 0.01267(13) 0.00340(9) 0.00268(9) 0.00438(10) C1 0.018(3) 0.018(2) 0.021(2) 0.0015(19) 0.0019(19) 0.002(2) C2 0.018(3) 0.018(2) 0.020(2) -0.0007(19) 0.0026(19) 0.001(2) C3 0.022(3) 0.022(2) 0.026(2) 0.005(2) 0.008(2) 0.001(2) C4 0.020(3) 0.020(2) 0.020(2) 0.0018(19) 0.0060(19) 0.005(2) C5 0.023(3) 0.020(2) 0.023(2) 0.000(2) 0.006(2) -0.001(2) C6 0.035(3) 0.022(3) 0.030(3) 0.005(2) 0.017(2) 0.003(2) C7 0.050(4) 0.051(4) 0.039(3) 0.019(3) 0.022(3) 0.030(3) C8 0.059(5) 0.059(4) 0.073(5) 0.026(4) 0.029(4) 0.038(4) C9 0.0550(19) 0.0546(19) 0.0568(19) 0.0152(11) 0.0251(12) 0.0175(11) C10 0.0563(19) 0.0563(19) 0.0551(19) 0.0137(11) 0.0264(12) 0.0152(11) C11 0.053(4) 0.051(4) 0.034(3) -0.002(3) 0.021(3) 0.010(3) C12 0.021(3) 0.016(2) 0.021(2) 0.0125(19) 0.010(2) 0.0053(19) C13 0.016(2) 0.025(2) 0.017(2) 0.0071(19) 0.0049(18) 0.006(2) C14 0.020(3) 0.030(3) 0.021(2) 0.010(2) 0.012(2) 0.009(2) C15 0.020(3) 0.028(3) 0.021(2) 0.011(2) 0.0095(19) 0.010(2) C16 0.012(2) 0.042(3) 0.025(3) 0.014(2) 0.005(2) 0.006(2) C17 0.023(3) 0.041(3) 0.045(3) 0.024(3) 0.018(2) 0.012(2) C18 0.046(4) 0.042(3) 0.062(4) 0.024(3) 0.026(3) 0.017(3) C19 0.068(6) 0.042(4) 0.111(7) 0.017(4) 0.054(5) 0.014(4) C20 0.064(2) 0.064(2) 0.067(2) 0.0232(11) 0.0255(12) 0.0182(11) C21 0.063(2) 0.064(2) 0.065(2) 0.0239(11) 0.0248(12) 0.0172(11) C22 0.028(3) 0.066(4) 0.057(4) 0.044(3) 0.011(3) 0.017(3) C23 0.021(3) 0.015(2) 0.023(2) 0.011(2) 0.008(2) 0.006(2) C24 0.020(3) 0.016(2) 0.016(2) 0.0057(18) 0.0053(18) 0.0065(19) C25 0.026(3) 0.017(2) 0.019(2) 0.0086(18) 0.007(2) 0.010(2) C26 0.021(3) 0.017(2) 0.016(2) 0.0063(18) 0.0059(18) 0.0084(19) C27 0.020(3) 0.016(2) 0.024(2) 0.0063(19) 0.004(2) 0.009(2) C28 0.026(3) 0.021(2) 0.022(2) 0.008(2) 0.004(2) 0.008(2) C29 0.029(3) 0.046(3) 0.023(3) 0.007(2) 0.004(2) 0.003(3) C30 0.055(5) 0.086(5) 0.039(3) 0.019(4) 0.027(3) 0.022(4) C31 0.067(5) 0.059(4) 0.022(3) 0.005(3) 0.010(3) 0.018(4) C32 0.051(4) 0.041(3) 0.025(3) 0.004(3) -0.008(3) 0.007(3) C33 0.031(3) 0.032(3) 0.025(3) 0.005(2) 0.001(2) 0.004(2) O1 0.027(2) 0.0244(18) 0.0238(17) -0.0031(14) 0.0095(15) -0.0019(15) O2 0.025(2) 0.0277(19) 0.0240(17) -0.0043(15) 0.0107(15) -0.0060(16) O3 0.038(2) 0.048(2) 0.0282(19) 0.0152(18) 0.0082(17) 0.014(2) O4 0.0169(18) 0.0339(19) 0.0195(16) 0.0058(14) 0.0043(14) 0.0061(15) O5 0.0155(17) 0.0246(17) 0.0231(16) 0.0088(14) 0.0096(13) 0.0074(14) O6 0.045(3) 0.066(3) 0.0224(19) 0.0128(19) 0.0150(17) 0.025(2) O7 0.035(2) 0.0162(16) 0.0184(16) 0.0038(13) 0.0051(14) 0.0090(15) O8 0.034(2) 0.0169(16) 0.0195(16) 0.0101(13) 0.0062(15) 0.0122(15) O9 0.028(2) 0.037(2) 0.0291(18) 0.0138(16) 0.0070(16) -0.0020(17) O1W 0.021(2) 0.038(2) 0.0333(19) 0.0105(16) 0.0014(15) 0.0137(17) O2W 0.048(3) 0.039(2) 0.043(2) 0.0235(18) 0.0240(19) 0.0146(19) O3W 0.099(5) 0.094(4) 0.068(3) 0.022(3) 0.042(3) 0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O5 2.414(3) . ? Nd1 O8 2.437(3) . ? Nd1 O7 2.453(3) . ? Nd1 O2 2.476(3) . ? Nd1 O4 2.491(3) 2_666 ? Nd1 O1 2.502(3) . ? Nd1 O1W 2.529(3) . ? Nd1 O2W 2.557(3) . ? Nd1 O5 2.701(3) 2_666 ? Nd1 C1 2.845(4) . ? Nd1 C12 2.962(5) 2_666 ? C1 O1 1.249(5) . ? C1 O2 1.263(6) . ? C1 C2 1.505(6) . ? C2 C3 1.392(7) 2_777 ? C2 C4 1.399(7) . ? C3 C4 1.383(6) . ? C3 C2 1.392(7) 2_777 ? C3 H3 0.9300 . ? C4 C5 1.516(6) . ? C5 O3 1.205(6) . ? C5 C6 1.495(7) . ? C6 C11 1.378(7) . ? C6 C7 1.385(8) . ? C7 C8 1.390(8) . ? C7 H7 0.9300 . ? C8 C9 1.376(9) . ? C8 H8 0.9300 . ? C9 C10 1.338(9) . ? C9 H9 0.9300 . ? C10 C11 1.403(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O4 1.241(5) . ? C12 O5 1.272(5) . ? C12 C13 1.498(6) . ? C12 Nd1 2.962(5) 2_666 ? C13 C14 1.387(6) . ? C13 C15 1.403(6) . ? C14 C15 1.385(6) 2_766 ? C14 H14 0.9300 . ? C15 C14 1.385(6) 2_766 ? C15 C16 1.506(6) . ? C16 O6 1.218(6) . ? C16 C17 1.485(7) . ? C17 C18 1.371(8) . ? C17 C22 1.395(8) . ? C18 C19 1.418(9) . ? C18 H18 0.9300 . ? C19 C20 1.387(11) . ? C19 H19 0.9300 . ? C20 C21 1.304(9) . ? C20 H20 0.9300 . ? C21 C22 1.385(9) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O7 1.252(5) 2_666 ? C23 O8 1.253(5) . ? C23 C24 1.515(6) . ? C24 C25 1.399(6) . ? C24 C26 1.401(6) . ? C25 C26 1.390(6) 2_676 ? C25 H25 0.9300 . ? C26 C25 1.390(6) 2_676 ? C26 C27 1.504(6) . ? C27 O9 1.213(6) . ? C27 C28 1.485(6) . ? C28 C33 1.387(7) . ? C28 C29 1.397(7) . ? C29 C30 1.371(8) . ? C29 H29 0.9300 . ? C30 C31 1.382(9) . ? C30 H30 0.9300 . ? C31 C32 1.370(9) . ? C31 H31 0.9300 . ? C32 C33 1.379(7) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? O4 Nd1 2.491(3) 2_666 ? O5 Nd1 2.701(3) 2_666 ? O7 C23 1.252(5) 2_666 ? O1W H1WB 0.8500 . ? O1W H1WA 0.8501 . ? O2W H2WA 0.8496 . ? O2W H2WB 0.8489 . ? O3W H3WA 0.8539 . ? O3W H3WB 0.8571 . ? 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 O5 Nd1 O8 75.44(10) . . ? O5 Nd1 O7 74.32(10) . . ? O8 Nd1 O7 136.34(10) . . ? O5 Nd1 O2 139.43(11) . . ? O8 Nd1 O2 80.96(11) . . ? O7 Nd1 O2 140.79(11) . . ? O5 Nd1 O4 125.06(10) . 2_666 ? O8 Nd1 O4 76.51(11) . 2_666 ? O7 Nd1 O4 96.21(11) . 2_666 ? O2 Nd1 O4 79.25(11) . 2_666 ? O5 Nd1 O1 89.33(10) . . ? O8 Nd1 O1 74.33(11) . . ? O7 Nd1 O1 135.34(11) . . ? O2 Nd1 O1 52.32(10) . . ? O4 Nd1 O1 126.20(10) 2_666 . ? O5 Nd1 O1W 94.93(10) . . ? O8 Nd1 O1W 139.51(12) . . ? O7 Nd1 O1W 74.01(11) . . ? O2 Nd1 O1W 82.08(11) . . ? O4 Nd1 O1W 135.17(11) 2_666 . ? O1 Nd1 O1W 66.20(12) . . ? O5 Nd1 O2W 141.87(11) . . ? O8 Nd1 O2W 140.45(11) . . ? O7 Nd1 O2W 68.88(11) . . ? O2 Nd1 O2W 73.14(11) . . ? O4 Nd1 O2W 69.75(11) 2_666 . ? O1 Nd1 O2W 109.89(12) . . ? O1W Nd1 O2W 65.91(12) . . ? O5 Nd1 O5 76.07(10) . 2_666 ? O8 Nd1 O5 68.42(10) . 2_666 ? O7 Nd1 O5 74.22(10) . 2_666 ? O2 Nd1 O5 124.46(10) . 2_666 ? O4 Nd1 O5 49.78(9) 2_666 2_666 ? O1 Nd1 O5 142.29(11) . 2_666 ? O1W Nd1 O5 148.23(10) . 2_666 ? O2W Nd1 O5 102.57(11) . 2_666 ? O5 Nd1 C1 114.66(12) . . ? O8 Nd1 C1 76.85(12) . . ? O7 Nd1 C1 145.22(12) . . ? O2 Nd1 C1 26.31(12) . . ? O4 Nd1 C1 103.41(12) 2_666 . ? O1 Nd1 C1 26.03(12) . . ? O1W Nd1 C1 71.80(12) . . ? O2W Nd1 C1 91.25(13) . . ? O5 Nd1 C1 139.75(11) 2_666 . ? O5 Nd1 C12 100.90(11) . 2_666 ? O8 Nd1 C12 69.60(11) . 2_666 ? O7 Nd1 C12 86.09(12) . 2_666 ? O2 Nd1 C12 101.13(12) . 2_666 ? O4 Nd1 C12 24.41(10) 2_666 2_666 ? O1 Nd1 C12 138.34(11) . 2_666 ? O1W Nd1 C12 150.18(12) . 2_666 ? O2W Nd1 C12 86.45(12) . 2_666 ? O5 Nd1 C12 25.43(10) 2_666 2_666 ? C1 Nd1 C12 122.12(13) . 2_666 ? O5 Nd1 Nd1 40.55(7) . 2_666 ? O8 Nd1 Nd1 66.62(7) . 2_666 ? O7 Nd1 Nd1 69.89(7) . 2_666 ? O2 Nd1 Nd1 146.48(9) . 2_666 ? O4 Nd1 Nd1 84.91(7) 2_666 2_666 ? O1 Nd1 Nd1 121.53(8) . 2_666 ? O1W Nd1 Nd1 128.38(7) . 2_666 ? O2W Nd1 Nd1 128.07(9) . 2_666 ? O5 Nd1 Nd1 35.52(6) 2_666 2_666 ? C1 Nd1 Nd1 139.56(10) . 2_666 ? C12 Nd1 Nd1 60.54(8) 2_666 2_666 ? O1 C1 O2 121.8(4) . . ? O1 C1 C2 118.8(4) . . ? O2 C1 C2 119.4(4) . . ? O1 C1 Nd1 61.5(2) . . ? O2 C1 Nd1 60.3(2) . . ? C2 C1 Nd1 175.6(3) . . ? C3 C2 C4 119.7(4) 2_777 . ? C3 C2 C1 118.9(4) 2_777 . ? C4 C2 C1 121.4(4) . . ? C4 C3 C2 121.6(5) . 2_777 ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 2_777 . ? C3 C4 C2 118.7(4) . . ? C3 C4 C5 119.5(4) . . ? C2 C4 C5 121.7(4) . . ? O3 C5 C6 122.0(5) . . ? O3 C5 C4 119.2(4) . . ? C6 C5 C4 118.7(4) . . ? C11 C6 C7 118.8(5) . . ? C11 C6 C5 118.3(5) . . ? C7 C6 C5 122.8(4) . . ? C6 C7 C8 120.2(6) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 120.1(7) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 120.1(7) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.8(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C6 C11 C10 119.9(6) . . ? C6 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? O4 C12 O5 121.6(4) . . ? O4 C12 C13 119.4(4) . . ? O5 C12 C13 119.0(4) . . ? O4 C12 Nd1 56.1(2) . 2_666 ? O5 C12 Nd1 65.8(2) . 2_666 ? C13 C12 Nd1 172.2(3) . 2_666 ? C14 C13 C15 118.9(4) . . ? C14 C13 C12 118.8(4) . . ? C15 C13 C12 122.2(4) . . ? C15 C14 C13 122.0(4) 2_766 . ? C15 C14 H14 119.0 2_766 . ? C13 C14 H14 119.0 . . ? C14 C15 C13 119.1(4) 2_766 . ? C14 C15 C16 117.4(4) 2_766 . ? C13 C15 C16 123.6(4) . . ? O6 C16 C17 121.9(5) . . ? O6 C16 C15 118.0(4) . . ? C17 C16 C15 120.0(4) . . ? C18 C17 C22 119.7(6) . . ? C18 C17 C16 121.7(5) . . ? C22 C17 C16 118.6(5) . . ? C17 C18 C19 119.6(7) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 117.5(7) . . ? C20 C19 H19 121.3 . . ? C18 C19 H19 121.3 . . ? C21 C20 C19 123.0(8) . . ? C21 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? C20 C21 C22 120.6(7) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C17 119.5(7) . . ? C21 C22 H22 120.2 . . ? C17 C22 H22 120.2 . . ? O7 C23 O8 125.7(4) 2_666 . ? O7 C23 C24 117.3(4) 2_666 . ? O8 C23 C24 117.0(4) . . ? C25 C24 C26 118.4(4) . . ? C25 C24 C23 118.5(4) . . ? C26 C24 C23 123.0(4) . . ? C26 C25 C24 121.5(4) 2_676 . ? C26 C25 H25 119.3 2_676 . ? C24 C25 H25 119.3 . . ? C25 C26 C24 120.1(4) 2_676 . ? C25 C26 C27 118.2(4) 2_676 . ? C24 C26 C27 121.4(4) . . ? O9 C27 C28 120.8(4) . . ? O9 C27 C26 120.5(4) . . ? C28 C27 C26 118.7(4) . . ? C33 C28 C29 118.9(4) . . ? C33 C28 C27 119.9(5) . . ? C29 C28 C27 121.2(4) . . ? C30 C29 C28 119.9(5) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.1(6) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 120.9(5) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C33 119.2(6) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C32 C33 C28 121.0(5) . . ? C32 C33 H33 119.5 . . ? C28 C33 H33 119.5 . . ? C1 O1 Nd1 92.5(3) . . ? C1 O2 Nd1 93.4(3) . . ? C12 O4 Nd1 99.5(3) . 2_666 ? C12 O5 Nd1 162.1(3) . . ? C12 O5 Nd1 88.8(2) . 2_666 ? Nd1 O5 Nd1 103.93(10) . 2_666 ? C23 O7 Nd1 135.4(3) 2_666 . ? C23 O8 Nd1 141.8(3) . . ? Nd1 O1W H1WB 138.3 . . ? Nd1 O1W H1WA 102.7 . . ? H1WB O1W H1WA 107.4 . . ? Nd1 O2W H2WA 110.5 . . ? Nd1 O2W H2WB 115.7 . . ? H2WA O2W H2WB 107.8 . . ? H3WA O3W H3WB 106.4 . . ? 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 O5 Nd1 C1 O1 -14.2(3) . . . . ? O8 Nd1 C1 O1 -81.1(3) . . . . ? O7 Nd1 C1 O1 83.9(3) . . . . ? O2 Nd1 C1 O1 -177.4(5) . . . . ? O4 Nd1 C1 O1 -153.6(3) 2_666 . . . ? O1W Nd1 C1 O1 72.9(3) . . . . ? O2W Nd1 C1 O1 137.0(3) . . . . ? O5 Nd1 C1 O1 -111.8(3) 2_666 . . . ? C12 Nd1 C1 O1 -136.4(3) 2_666 . . . ? Nd1 Nd1 C1 O1 -55.6(3) 2_666 . . . ? O5 Nd1 C1 O2 163.2(3) . . . . ? O8 Nd1 C1 O2 96.2(3) . . . . ? O7 Nd1 C1 O2 -98.8(3) . . . . ? O4 Nd1 C1 O2 23.8(3) 2_666 . . . ? O1 Nd1 C1 O2 177.4(5) . . . . ? O1W Nd1 C1 O2 -109.8(3) . . . . ? O2W Nd1 C1 O2 -45.7(3) . . . . ? O5 Nd1 C1 O2 65.6(3) 2_666 . . . ? C12 Nd1 C1 O2 40.9(3) 2_666 . . . ? Nd1 Nd1 C1 O2 121.8(3) 2_666 . . . ? O1 C1 C2 C3 -161.0(5) . . . 2_777 ? O2 C1 C2 C3 16.8(7) . . . 2_777 ? O1 C1 C2 C4 16.6(7) . . . . ? O2 C1 C2 C4 -165.6(5) . . . . ? C2 C3 C4 C2 -0.4(8) 2_777 . . . ? C2 C3 C4 C5 175.8(4) 2_777 . . . ? C3 C2 C4 C3 0.4(8) 2_777 . . . ? C1 C2 C4 C3 -177.2(4) . . . . ? C3 C2 C4 C5 -175.8(4) 2_777 . . . ? C1 C2 C4 C5 6.7(7) . . . . ? C3 C4 C5 O3 -100.0(6) . . . . ? C2 C4 C5 O3 76.1(6) . . . . ? C3 C4 C5 C6 76.6(6) . . . . ? C2 C4 C5 C6 -107.3(5) . . . . ? O3 C5 C6 C11 -20.0(8) . . . . ? C4 C5 C6 C11 163.5(5) . . . . ? O3 C5 C6 C7 156.4(6) . . . . ? C4 C5 C6 C7 -20.1(7) . . . . ? C11 C6 C7 C8 2.5(9) . . . . ? C5 C6 C7 C8 -173.8(5) . . . . ? C6 C7 C8 C9 -2.2(10) . . . . ? C7 C8 C9 C10 0.2(11) . . . . ? C8 C9 C10 C11 1.6(11) . . . . ? C7 C6 C11 C10 -0.8(9) . . . . ? C5 C6 C11 C10 175.7(5) . . . . ? C9 C10 C11 C6 -1.2(10) . . . . ? O4 C12 C13 C14 -143.4(4) . . . . ? O5 C12 C13 C14 34.5(6) . . . . ? O4 C12 C13 C15 32.6(6) . . . . ? O5 C12 C13 C15 -149.4(4) . . . . ? C15 C13 C14 C15 -0.1(8) . . . 2_766 ? C12 C13 C14 C15 176.1(4) . . . 2_766 ? C14 C13 C15 C14 0.1(7) . . . 2_766 ? C12 C13 C15 C14 -176.0(4) . . . 2_766 ? C14 C13 C15 C16 -179.9(5) . . . . ? C12 C13 C15 C16 4.1(7) . . . . ? C14 C15 C16 O6 53.0(7) 2_766 . . . ? C13 C15 C16 O6 -127.0(5) . . . . ? C14 C15 C16 C17 -122.8(5) 2_766 . . . ? C13 C15 C16 C17 57.1(7) . . . . ? O6 C16 C17 C18 -166.1(5) . . . . ? C15 C16 C17 C18 9.6(8) . . . . ? O6 C16 C17 C22 12.2(8) . . . . ? C15 C16 C17 C22 -172.1(5) . . . . ? C22 C17 C18 C19 0.6(9) . . . . ? C16 C17 C18 C19 178.9(6) . . . . ? C17 C18 C19 C20 -0.1(10) . . . . ? C18 C19 C20 C21 -0.3(12) . . . . ? C19 C20 C21 C22 0.1(12) . . . . ? C20 C21 C22 C17 0.5(11) . . . . ? C18 C17 C22 C21 -0.9(9) . . . . ? C16 C17 C22 C21 -179.2(5) . . . . ? O7 C23 C24 C25 -144.4(4) 2_666 . . . ? O8 C23 C24 C25 34.1(6) . . . . ? O7 C23 C24 C26 31.9(7) 2_666 . . . ? O8 C23 C24 C26 -149.5(4) . . . . ? C26 C24 C25 C26 -0.4(7) . . . 2_676 ? C23 C24 C25 C26 176.1(4) . . . 2_676 ? C25 C24 C26 C25 0.4(7) . . . 2_676 ? C23 C24 C26 C25 -175.9(4) . . . 2_676 ? C25 C24 C26 C27 -174.1(4) . . . . ? C23 C24 C26 C27 9.5(7) . . . . ? C25 C26 C27 O9 -112.2(5) 2_676 . . . ? C24 C26 C27 O9 62.4(6) . . . . ? C25 C26 C27 C28 67.7(5) 2_676 . . . ? C24 C26 C27 C28 -117.6(5) . . . . ? O9 C27 C28 C33 11.4(7) . . . . ? C26 C27 C28 C33 -168.6(4) . . . . ? O9 C27 C28 C29 -165.8(5) . . . . ? C26 C27 C28 C29 14.2(7) . . . . ? C33 C28 C29 C30 -2.1(8) . . . . ? C27 C28 C29 C30 175.1(5) . . . . ? C28 C29 C30 C31 2.2(10) . . . . ? C29 C30 C31 C32 -0.8(11) . . . . ? C30 C31 C32 C33 -0.7(10) . . . . ? C31 C32 C33 C28 0.8(9) . . . . ? C29 C28 C33 C32 0.6(8) . . . . ? C27 C28 C33 C32 -176.7(5) . . . . ? O2 C1 O1 Nd1 -2.7(5) . . . . ? C2 C1 O1 Nd1 175.0(4) . . . . ? O5 Nd1 O1 C1 167.1(3) . . . . ? O8 Nd1 O1 C1 92.1(3) . . . . ? O7 Nd1 O1 C1 -126.2(3) . . . . ? O2 Nd1 O1 C1 1.5(3) . . . . ? O4 Nd1 O1 C1 32.4(3) 2_666 . . . ? O1W Nd1 O1 C1 -97.2(3) . . . . ? O2W Nd1 O1 C1 -46.5(3) . . . . ? O5 Nd1 O1 C1 101.3(3) 2_666 . . . ? C12 Nd1 O1 C1 61.4(3) 2_666 . . . ? Nd1 Nd1 O1 C1 141.1(3) 2_666 . . . ? O1 C1 O2 Nd1 2.7(5) . . . . ? C2 C1 O2 Nd1 -175.0(4) . . . . ? O5 Nd1 O2 C1 -23.8(4) . . . . ? O8 Nd1 O2 C1 -78.6(3) . . . . ? O7 Nd1 O2 C1 116.9(3) . . . . ? O4 Nd1 O2 C1 -156.5(3) 2_666 . . . ? O1 Nd1 O2 C1 -1.5(3) . . . . ? O1W Nd1 O2 C1 64.5(3) . . . . ? O2W Nd1 O2 C1 131.6(3) . . . . ? O5 Nd1 O2 C1 -134.5(3) 2_666 . . . ? C12 Nd1 O2 C1 -145.6(3) 2_666 . . . ? Nd1 Nd1 O2 C1 -93.2(3) 2_666 . . . ? O5 C12 O4 Nd1 -5.4(5) . . . 2_666 ? C13 C12 O4 Nd1 172.5(3) . . . 2_666 ? O4 C12 O5 Nd1 140.7(7) . . . . ? C13 C12 O5 Nd1 -37.1(11) . . . . ? Nd1 C12 O5 Nd1 135.9(9) 2_666 . . . ? O4 C12 O5 Nd1 4.9(4) . . . 2_666 ? C13 C12 O5 Nd1 -173.0(4) . . . 2_666 ? O8 Nd1 O5 C12 154.9(9) . . . . ? O7 Nd1 O5 C12 -57.0(9) . . . . ? O2 Nd1 O5 C12 98.5(9) . . . . ? O4 Nd1 O5 C12 -143.6(9) 2_666 . . . ? O1 Nd1 O5 C12 80.9(9) . . . . ? O1W Nd1 O5 C12 14.9(9) . . . . ? O2W Nd1 O5 C12 -41.5(10) . . . . ? O5 Nd1 O5 C12 -134.2(10) 2_666 . . . ? C1 Nd1 O5 C12 87.1(9) . . . . ? C12 Nd1 O5 C12 -139.7(9) 2_666 . . . ? Nd1 Nd1 O5 C12 -134.2(10) 2_666 . . . ? O8 Nd1 O5 Nd1 -70.91(11) . . . 2_666 ? O7 Nd1 O5 Nd1 77.21(12) . . . 2_666 ? O2 Nd1 O5 Nd1 -127.35(15) . . . 2_666 ? O4 Nd1 O5 Nd1 -9.37(16) 2_666 . . 2_666 ? O1 Nd1 O5 Nd1 -144.88(12) . . . 2_666 ? O1W Nd1 O5 Nd1 149.07(12) . . . 2_666 ? O2W Nd1 O5 Nd1 92.70(18) . . . 2_666 ? O5 Nd1 O5 Nd1 0.0 2_666 . . 2_666 ? C1 Nd1 O5 Nd1 -138.71(12) . . . 2_666 ? C12 Nd1 O5 Nd1 -5.54(13) 2_666 . . 2_666 ? O5 Nd1 O7 C23 -37.6(4) . . . 2_666 ? O8 Nd1 O7 C23 10.1(5) . . . 2_666 ? O2 Nd1 O7 C23 167.7(4) . . . 2_666 ? O4 Nd1 O7 C23 87.1(4) 2_666 . . 2_666 ? O1 Nd1 O7 C23 -110.1(4) . . . 2_666 ? O1W Nd1 O7 C23 -137.6(4) . . . 2_666 ? O2W Nd1 O7 C23 152.5(5) . . . 2_666 ? O5 Nd1 O7 C23 42.0(4) 2_666 . . 2_666 ? C1 Nd1 O7 C23 -148.5(4) . . . 2_666 ? C12 Nd1 O7 C23 64.8(4) 2_666 . . 2_666 ? Nd1 Nd1 O7 C23 4.8(4) 2_666 . . 2_666 ? O7 C23 O8 Nd1 9.2(8) 2_666 . . . ? C24 C23 O8 Nd1 -169.2(3) . . . . ? O5 Nd1 O8 C23 32.9(5) . . . . ? O7 Nd1 O8 C23 -14.6(6) . . . . ? O2 Nd1 O8 C23 179.6(5) . . . . ? O4 Nd1 O8 C23 -99.4(5) 2_666 . . . ? O1 Nd1 O8 C23 126.3(5) . . . . ? O1W Nd1 O8 C23 113.2(5) . . . . ? O2W Nd1 O8 C23 -131.2(5) . . . . ? O5 Nd1 O8 C23 -47.6(5) 2_666 . . . ? C1 Nd1 O8 C23 153.1(5) . . . . ? C12 Nd1 O8 C23 -74.9(5) 2_666 . . . ? Nd1 Nd1 O8 C23 -9.1(5) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.611 _refine_diff_density_min -1.148 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 890967' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'C33 H24 O12 Sm' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C33 H22 O11 Sm, H2 O' _chemical_formula_sum 'C33 H24 O12 Sm' _chemical_formula_weight 762.87 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4130(11) _cell_length_b 11.4804(18) _cell_length_c 14.1232(19) _cell_angle_alpha 102.540(6) _cell_angle_beta 111.1880(10) _cell_angle_gamma 100.429(3) _cell_volume 1472.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4337 _cell_measurement_theta_min 2.1124 _cell_measurement_theta_max 27.4971 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 2.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6713 _exptl_absorpt_correction_T_max 0.7473 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9983 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5280 _reflns_number_gt 4802 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^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 5280 _refine_ls_number_parameters 415 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.084 _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 Sm1 Sm 0.61423(2) 0.563373(19) 0.658870(17) 0.01420(10) Uani 1 1 d . . . C1 C 0.7988(5) 0.7872(4) 0.8197(4) 0.0205(10) Uani 1 1 d . . . C2 C 0.9018(5) 0.8992(4) 0.9121(4) 0.0222(10) Uani 1 1 d . . . C3 C 1.1081(5) 1.0792(4) 0.9901(4) 0.0236(10) Uani 1 1 d . . . H3A H 1.1812 1.1325 0.9839 0.028 Uiso 1 1 calc R . . C4 C 1.0109(5) 0.9794(4) 0.9013(4) 0.0232(10) Uani 1 1 d . . . C5 C 1.0203(5) 0.9650(4) 0.7944(4) 0.0253(11) Uani 1 1 d . . . C6 C 1.1362(6) 0.9153(5) 0.7777(5) 0.0296(12) Uani 1 1 d . . . C7 C 1.2600(7) 0.9187(6) 0.8610(5) 0.0401(14) Uani 1 1 d . . . H7A H 1.2702 0.9464 0.9310 0.048 Uiso 1 1 calc R . . C8 C 1.3691(8) 0.8810(7) 0.8401(7) 0.059(2) Uani 1 1 d . . . H8A H 1.4528 0.8845 0.8964 0.071 Uiso 1 1 calc R . . C9 C 1.3541(8) 0.8389(7) 0.7380(6) 0.0575(19) Uani 1 1 d U . . H9A H 1.4287 0.8157 0.7251 0.069 Uiso 1 1 calc R . . C10 C 1.2294(8) 0.8302(7) 0.6531(7) 0.0586(19) Uani 1 1 d U . . H10A H 1.2176 0.7968 0.5833 0.070 Uiso 1 1 calc R . . C11 C 1.1216(8) 0.8721(6) 0.6735(5) 0.0477(16) Uani 1 1 d . . . H11A H 1.0395 0.8712 0.6171 0.057 Uiso 1 1 calc R . . C12 C 0.7006(5) 0.4918(4) 0.4300(4) 0.0183(10) Uani 1 1 d . . . C13 C 0.8562(5) 0.5001(4) 0.4652(4) 0.0198(10) Uani 1 1 d . . . C14 C 0.9288(5) 0.4806(4) 0.5623(4) 0.0210(10) Uani 1 1 d . . . H14A H 0.8803 0.4680 0.6048 0.025 Uiso 1 1 calc R . . C15 C 0.9301(5) 0.5206(5) 0.4029(4) 0.0214(10) Uani 1 1 d . . . C16 C 0.8643(5) 0.5424(5) 0.2962(4) 0.0268(11) Uani 1 1 d . . . C17 C 0.8008(5) 0.6484(5) 0.2893(5) 0.0320(13) Uani 1 1 d . . . C18 C 0.8182(7) 0.7372(6) 0.3796(6) 0.0424(15) Uani 1 1 d . . . H18A H 0.8693 0.7303 0.4465 0.051 Uiso 1 1 calc R . . C19 C 0.7596(9) 0.8383(7) 0.3722(8) 0.070(2) Uani 1 1 d . . . H19A H 0.7707 0.8993 0.4323 0.084 Uiso 1 1 calc R . . C20 C 0.6820(8) 0.8409(7) 0.2660(6) 0.0580(19) Uani 1 1 d U . . H20A H 0.6405 0.9053 0.2573 0.070 Uiso 1 1 calc R . . C21 C 0.6664(8) 0.7550(7) 0.1790(6) 0.0551(18) Uani 1 1 d U . . H21A H 0.6160 0.7612 0.1117 0.066 Uiso 1 1 calc R . . C22 C 0.7245(6) 0.6578(6) 0.1882(6) 0.0449(16) Uani 1 1 d . . . H22A H 0.7133 0.5980 0.1273 0.054 Uiso 1 1 calc R . . C23 C 0.4832(5) 0.7416(4) 0.4953(4) 0.0179(9) Uani 1 1 d . . . C24 C 0.4875(5) 0.8755(4) 0.4977(4) 0.0177(9) Uani 1 1 d . . . C25 C 0.6047(5) 0.9711(4) 0.5755(4) 0.0212(10) Uani 1 1 d . . . H25A H 0.6753 0.9517 0.6272 0.025 Uiso 1 1 calc R . . C26 C 0.3796(5) 0.9047(4) 0.4211(4) 0.0189(9) Uani 1 1 d . . . C27 C 0.2423(5) 0.8084(4) 0.3416(4) 0.0205(10) Uani 1 1 d . . . C28 C 0.2091(5) 0.7818(4) 0.2257(4) 0.0242(11) Uani 1 1 d . . . C29 C 0.0721(6) 0.7109(5) 0.1492(4) 0.0348(13) Uani 1 1 d . . . H29A H 0.0002 0.6850 0.1707 0.042 Uiso 1 1 calc R . . C30 C 0.0427(7) 0.6792(6) 0.0429(5) 0.0469(17) Uani 1 1 d . . . H30A H -0.0484 0.6301 -0.0072 0.056 Uiso 1 1 calc R . . C31 C 0.1469(8) 0.7193(6) 0.0093(5) 0.0533(18) Uani 1 1 d . . . H31A H 0.1259 0.6981 -0.0631 0.064 Uiso 1 1 calc R . . C32 C 0.2820(8) 0.7909(8) 0.0834(6) 0.0588(19) Uani 1 1 d . . . H32A H 0.3529 0.8172 0.0610 0.071 Uiso 1 1 calc R . . C33 C 0.3127(6) 0.8239(6) 0.1909(4) 0.0370(13) Uani 1 1 d . . . H33A H 0.4033 0.8746 0.2404 0.044 Uiso 1 1 calc R . . O1 O 0.8289(4) 0.7484(3) 0.7430(3) 0.0284(8) Uani 1 1 d . . . O2 O 0.6857(4) 0.7311(3) 0.8250(3) 0.0298(8) Uani 1 1 d . . . O3 O 0.9399(4) 1.0000(4) 0.7282(3) 0.0395(10) Uani 1 1 d . . . O4 O 0.6532(3) 0.5279(3) 0.5000(3) 0.0224(7) Uani 1 1 d . . . O5 O 0.6189(3) 0.4482(3) 0.3332(3) 0.0246(7) Uani 1 1 d . . . O6 O 0.8719(5) 0.4788(4) 0.2190(3) 0.0441(10) Uani 1 1 d . . . O7 O 0.5719(4) 0.3405(3) 0.5947(3) 0.0250(8) Uani 1 1 d . . . O8 O 0.5402(3) 0.7233(3) 0.5839(3) 0.0216(7) Uani 1 1 d . . . O9 O 0.1614(4) 0.7538(3) 0.3715(3) 0.0341(9) Uani 1 1 d . . . O1W O 0.8402(4) 0.5205(3) 0.7664(3) 0.0312(8) Uani 1 1 d . . . H1WB H 0.9262 0.5611 0.7802 0.037 Uiso 1 1 d R . . H1WA H 0.8335 0.4435 0.7402 0.037 Uiso 1 1 d R . . O2W O 0.5933(4) 0.4615(4) 0.7972(3) 0.0392(10) Uani 1 1 d . . . H2WA H 0.5694 0.3841 0.7927 0.047 Uiso 1 1 d R . . H2WB H 0.5736 0.5002 0.8471 0.047 Uiso 1 1 d R . . O3W O 0.5010(7) 0.6402(6) 0.9148(5) 0.0778(17) Uani 1 1 d . . . H3WA H 0.5623 0.7006 0.9150 0.093 Uiso 1 1 d R . . H3WB H 0.4397 0.6055 0.8503 0.093 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 Sm1 0.01339(14) 0.01069(14) 0.01388(14) 0.00090(10) 0.00269(10) 0.00255(9) C1 0.021(2) 0.013(2) 0.018(2) -0.0009(19) 0.001(2) 0.0028(19) C2 0.017(2) 0.015(2) 0.022(2) -0.0023(19) 0.0005(19) -0.0005(19) C3 0.023(3) 0.019(2) 0.020(2) -0.003(2) 0.007(2) 0.001(2) C4 0.023(3) 0.015(2) 0.022(2) -0.004(2) 0.005(2) 0.003(2) C5 0.023(3) 0.018(2) 0.023(3) -0.002(2) 0.004(2) -0.002(2) C6 0.038(3) 0.016(2) 0.037(3) 0.006(2) 0.019(3) 0.006(2) C7 0.046(4) 0.040(3) 0.038(3) 0.011(3) 0.019(3) 0.020(3) C8 0.053(4) 0.060(5) 0.079(6) 0.030(4) 0.031(4) 0.034(4) C9 0.058(2) 0.057(2) 0.059(2) 0.0163(11) 0.0261(12) 0.0169(11) C10 0.059(2) 0.059(2) 0.058(2) 0.0154(11) 0.0268(12) 0.0169(11) C11 0.060(4) 0.041(4) 0.035(3) -0.003(3) 0.024(3) 0.006(3) C12 0.019(2) 0.017(2) 0.021(2) 0.009(2) 0.010(2) 0.0057(19) C13 0.019(2) 0.018(2) 0.019(2) 0.0018(19) 0.007(2) 0.0039(19) C14 0.018(2) 0.027(3) 0.021(2) 0.007(2) 0.011(2) 0.006(2) C15 0.018(2) 0.026(3) 0.018(2) 0.006(2) 0.0058(19) 0.007(2) C16 0.014(2) 0.041(3) 0.024(3) 0.013(2) 0.006(2) 0.007(2) C17 0.018(3) 0.039(3) 0.046(3) 0.026(3) 0.013(2) 0.009(2) C18 0.037(3) 0.036(3) 0.059(4) 0.022(3) 0.020(3) 0.013(3) C19 0.073(6) 0.039(4) 0.106(7) 0.017(4) 0.050(5) 0.011(4) C20 0.057(2) 0.057(2) 0.060(2) 0.0200(11) 0.0235(12) 0.0167(11) C21 0.055(2) 0.055(2) 0.056(2) 0.0204(11) 0.0216(12) 0.0151(11) C22 0.029(3) 0.057(4) 0.058(4) 0.041(4) 0.013(3) 0.016(3) C23 0.017(2) 0.013(2) 0.021(2) 0.004(2) 0.0054(19) 0.0050(18) C24 0.020(2) 0.013(2) 0.017(2) 0.0021(19) 0.0058(19) 0.0046(18) C25 0.024(3) 0.014(2) 0.019(2) 0.0017(19) 0.003(2) 0.008(2) C26 0.025(2) 0.010(2) 0.018(2) 0.0013(18) 0.007(2) 0.0052(18) C27 0.023(2) 0.012(2) 0.022(2) 0.004(2) 0.005(2) 0.0049(19) C28 0.027(3) 0.017(2) 0.021(2) 0.003(2) 0.002(2) 0.008(2) C29 0.026(3) 0.033(3) 0.029(3) 0.009(3) -0.002(2) 0.001(2) C30 0.049(4) 0.033(3) 0.027(3) -0.005(3) -0.006(3) 0.002(3) C31 0.071(5) 0.055(4) 0.023(3) 0.004(3) 0.011(3) 0.022(4) C32 0.054(4) 0.083(6) 0.037(4) 0.015(4) 0.019(3) 0.017(4) C33 0.029(3) 0.044(3) 0.025(3) 0.002(3) 0.006(2) 0.004(3) O1 0.0261(19) 0.0215(18) 0.0244(19) -0.0059(15) 0.0086(16) -0.0037(15) O2 0.0254(19) 0.0257(19) 0.0250(19) -0.0052(16) 0.0099(16) -0.0068(15) O3 0.035(2) 0.048(3) 0.029(2) 0.012(2) 0.0059(18) 0.0125(19) O4 0.0180(17) 0.0213(17) 0.0274(18) 0.0046(15) 0.0105(14) 0.0062(14) O5 0.0170(17) 0.0325(19) 0.0215(18) 0.0065(16) 0.0053(14) 0.0086(15) O6 0.045(3) 0.065(3) 0.027(2) 0.011(2) 0.0162(19) 0.026(2) O7 0.0327(19) 0.0105(16) 0.0216(17) -0.0001(14) 0.0037(15) 0.0047(14) O8 0.0248(18) 0.0131(16) 0.0209(17) 0.0057(14) 0.0026(14) 0.0061(14) O9 0.027(2) 0.032(2) 0.033(2) 0.0115(18) 0.0066(17) -0.0020(16) O1W 0.0219(19) 0.030(2) 0.037(2) 0.0079(18) 0.0075(17) 0.0103(16) O2W 0.048(2) 0.035(2) 0.048(2) 0.023(2) 0.027(2) 0.0161(19) O3W 0.094(4) 0.083(4) 0.056(3) 0.015(3) 0.042(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O4 2.385(3) . ? Sm1 O8 2.420(3) . ? Sm1 O7 2.420(3) . ? Sm1 O5 2.451(3) 2_666 ? Sm1 O2 2.455(4) . ? Sm1 O1 2.488(3) . ? Sm1 O1W 2.500(3) . ? Sm1 O2W 2.537(4) . ? Sm1 O4 2.700(3) 2_666 ? Sm1 C1 2.824(5) . ? Sm1 C12 2.942(5) 2_666 ? C1 O1 1.247(6) . ? C1 O2 1.272(6) . ? C1 C2 1.506(6) . ? C2 C3 1.394(7) 2_777 ? C2 C4 1.403(7) . ? C3 C2 1.394(7) 2_777 ? C3 C4 1.396(7) . ? C3 H3A 0.9300 . ? C4 C5 1.522(7) . ? C5 O3 1.206(6) . ? C5 C6 1.496(8) . ? C6 C7 1.383(8) . ? C6 C11 1.389(8) . ? C7 C8 1.389(9) . ? C7 H7A 0.9300 . ? C8 C9 1.359(11) . ? C8 H8A 0.9300 . ? C9 C10 1.382(10) . ? C9 H9A 0.9300 . ? C10 C11 1.395(10) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 O5 1.246(6) . ? C12 O4 1.281(6) . ? C12 C13 1.491(6) . ? C12 Sm1 2.942(5) 2_666 ? C13 C15 1.392(6) . ? C13 C14 1.396(7) . ? C14 C15 1.374(7) 2_766 ? C14 H14A 0.9300 . ? C15 C14 1.374(7) 2_766 ? C15 C16 1.511(6) . ? C16 O6 1.211(7) . ? C16 C17 1.491(8) . ? C17 C18 1.378(9) . ? C17 C22 1.399(8) . ? C18 C19 1.412(10) . ? C18 H18A 0.9300 . ? C19 C20 1.434(12) . ? C19 H19A 0.9300 . ? C20 C21 1.334(10) . ? C20 H20A 0.9300 . ? C21 C22 1.371(9) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 O8 1.259(6) . ? C23 O7 1.261(6) 2_666 ? C23 C24 1.522(6) . ? C24 C25 1.387(7) . ? C24 C26 1.400(7) . ? C25 C26 1.394(6) 2_676 ? C25 H25A 0.9300 . ? C26 C25 1.394(6) 2_676 ? C26 C27 1.502(7) . ? C27 O9 1.209(6) . ? C27 C28 1.493(7) . ? C28 C33 1.391(8) . ? C28 C29 1.396(7) . ? C29 C30 1.367(8) . ? C29 H29A 0.9300 . ? C30 C31 1.378(10) . ? C30 H30A 0.9300 . ? C31 C32 1.376(10) . ? C31 H31A 0.9300 . ? C32 C33 1.381(9) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? O4 Sm1 2.700(3) 2_666 ? O5 Sm1 2.451(3) 2_666 ? O7 C23 1.261(6) 2_666 ? O1W H1WB 0.8600 . ? O1W H1WA 0.8600 . ? O2W H2WA 0.8600 . ? O2W H2WB 0.8601 . ? O3W H3WA 0.8530 . ? O3W H3WB 0.8520 . ? 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 Sm1 O8 75.39(11) . . ? O4 Sm1 O7 74.94(11) . . ? O8 Sm1 O7 136.64(11) . . ? O4 Sm1 O5 125.45(11) . 2_666 ? O8 Sm1 O5 77.09(11) . 2_666 ? O7 Sm1 O5 95.50(12) . 2_666 ? O4 Sm1 O2 139.17(11) . . ? O8 Sm1 O2 80.86(12) . . ? O7 Sm1 O2 140.48(12) . . ? O5 Sm1 O2 79.34(12) 2_666 . ? O4 Sm1 O1 88.42(11) . . ? O8 Sm1 O1 73.86(11) . . ? O7 Sm1 O1 135.47(12) . . ? O5 Sm1 O1 126.83(12) 2_666 . ? O2 Sm1 O1 52.90(11) . . ? O4 Sm1 O1W 94.46(12) . . ? O8 Sm1 O1W 139.12(12) . . ? O7 Sm1 O1W 74.10(12) . . ? O5 Sm1 O1W 135.15(12) 2_666 . ? O2 Sm1 O1W 82.27(13) . . ? O1 Sm1 O1W 66.26(12) . . ? O4 Sm1 O2W 142.28(12) . . ? O8 Sm1 O2W 140.33(12) . . ? O7 Sm1 O2W 68.82(13) . . ? O5 Sm1 O2W 69.38(12) 2_666 . ? O2 Sm1 O2W 72.80(13) . . ? O1 Sm1 O2W 110.18(12) . . ? O1W Sm1 O2W 66.18(12) . . ? O4 Sm1 O4 75.94(11) . 2_666 ? O8 Sm1 O4 69.02(10) . 2_666 ? O7 Sm1 O4 73.59(11) . 2_666 ? O5 Sm1 O4 50.33(11) 2_666 2_666 ? O2 Sm1 O4 125.05(11) . 2_666 ? O1 Sm1 O4 142.23(11) . 2_666 ? O1W Sm1 O4 147.67(11) . 2_666 ? O2W Sm1 O4 102.78(12) . 2_666 ? O4 Sm1 C1 113.91(13) . . ? O8 Sm1 C1 76.42(12) . . ? O7 Sm1 C1 145.38(13) . . ? O5 Sm1 C1 103.88(13) 2_666 . ? O2 Sm1 C1 26.74(13) . . ? O1 Sm1 C1 26.18(13) . . ? O1W Sm1 C1 71.90(13) . . ? O2W Sm1 C1 91.37(14) . . ? O4 Sm1 C1 140.30(12) 2_666 . ? O4 Sm1 C12 101.04(12) . 2_666 ? O8 Sm1 C12 69.88(11) . 2_666 ? O7 Sm1 C12 85.68(12) . 2_666 ? O5 Sm1 C12 24.63(12) 2_666 2_666 ? O2 Sm1 C12 101.28(13) . 2_666 ? O1 Sm1 C12 138.55(12) . 2_666 ? O1W Sm1 C12 150.37(12) . 2_666 ? O2W Sm1 C12 86.56(12) . 2_666 ? O4 Sm1 C12 25.78(11) 2_666 2_666 ? C1 Sm1 C12 122.46(14) . 2_666 ? O4 Sm1 Sm1 40.74(8) . 2_666 ? O8 Sm1 Sm1 66.99(8) . 2_666 ? O7 Sm1 Sm1 69.85(8) . 2_666 ? O5 Sm1 Sm1 85.13(8) 2_666 2_666 ? O2 Sm1 Sm1 146.72(9) . 2_666 ? O1 Sm1 Sm1 121.03(8) . 2_666 ? O1W Sm1 Sm1 127.93(9) . 2_666 ? O2W Sm1 Sm1 128.24(10) . 2_666 ? O4 Sm1 Sm1 35.20(7) 2_666 2_666 ? C1 Sm1 Sm1 139.33(10) . 2_666 ? C12 Sm1 Sm1 60.53(9) 2_666 2_666 ? O1 C1 O2 121.8(4) . . ? O1 C1 C2 119.9(4) . . ? O2 C1 C2 118.2(4) . . ? O1 C1 Sm1 61.7(2) . . ? O2 C1 Sm1 60.2(2) . . ? C2 C1 Sm1 174.6(3) . . ? C3 C2 C4 119.9(4) 2_777 . ? C3 C2 C1 119.8(4) 2_777 . ? C4 C2 C1 120.3(5) . . ? C2 C3 C4 121.6(5) 2_777 . ? C2 C3 H3A 119.2 2_777 . ? C4 C3 H3A 119.2 . . ? C3 C4 C2 118.5(5) . . ? C3 C4 C5 119.5(4) . . ? C2 C4 C5 121.9(4) . . ? O3 C5 C6 121.8(5) . . ? O3 C5 C4 119.6(5) . . ? C6 C5 C4 118.5(4) . . ? C7 C6 C11 119.3(6) . . ? C7 C6 C5 122.9(5) . . ? C11 C6 C5 117.6(5) . . ? C6 C7 C8 120.0(6) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 120.3(7) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 120.9(8) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C9 C10 C11 119.1(8) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C6 C11 C10 120.2(7) . . ? C6 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? O5 C12 O4 121.3(4) . . ? O5 C12 C13 119.3(4) . . ? O4 C12 C13 119.4(4) . . ? O5 C12 Sm1 55.1(2) . 2_666 ? O4 C12 Sm1 66.5(2) . 2_666 ? C13 C12 Sm1 171.3(3) . 2_666 ? C15 C13 C14 118.7(4) . . ? C15 C13 C12 122.7(4) . . ? C14 C13 C12 118.5(4) . . ? C15 C14 C13 121.9(4) 2_766 . ? C15 C14 H14A 119.0 2_766 . ? C13 C14 H14A 119.0 . . ? C14 C15 C13 119.4(4) 2_766 . ? C14 C15 C16 116.6(4) 2_766 . ? C13 C15 C16 124.0(4) . . ? O6 C16 C17 120.8(5) . . ? O6 C16 C15 119.6(5) . . ? C17 C16 C15 119.4(5) . . ? C18 C17 C22 120.1(6) . . ? C18 C17 C16 121.4(5) . . ? C22 C17 C16 118.4(6) . . ? C17 C18 C19 121.0(7) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C18 C19 C20 115.6(8) . . ? C18 C19 H19A 122.2 . . ? C20 C19 H19A 122.2 . . ? C21 C20 C19 123.0(8) . . ? C21 C20 H20A 118.5 . . ? C19 C20 H20A 118.5 . . ? C20 C21 C22 120.3(7) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C21 C22 C17 119.9(7) . . ? C21 C22 H22A 120.0 . . ? C17 C22 H22A 120.0 . . ? O8 C23 O7 125.6(4) . 2_666 ? O8 C23 C24 116.7(4) . . ? O7 C23 C24 117.7(4) 2_666 . ? C25 C24 C26 119.0(4) . . ? C25 C24 C23 119.0(4) . . ? C26 C24 C23 122.0(4) . . ? C24 C25 C26 122.3(4) . 2_676 ? C24 C25 H25A 118.9 . . ? C26 C25 H25A 118.9 2_676 . ? C25 C26 C24 118.7(4) 2_676 . ? C25 C26 C27 118.9(4) 2_676 . ? C24 C26 C27 122.1(4) . . ? O9 C27 C28 121.2(4) . . ? O9 C27 C26 120.4(4) . . ? C28 C27 C26 118.4(4) . . ? C33 C28 C29 118.4(5) . . ? C33 C28 C27 121.7(5) . . ? C29 C28 C27 119.9(5) . . ? C30 C29 C28 120.6(6) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C31 120.5(6) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C32 C31 C30 119.8(6) . . ? C32 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? C31 C32 C33 120.2(7) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C32 C33 C28 120.5(6) . . ? C32 C33 H33A 119.8 . . ? C28 C33 H33A 119.8 . . ? C1 O1 Sm1 92.2(3) . . ? C1 O2 Sm1 93.0(3) . . ? C12 O4 Sm1 162.2(3) . . ? C12 O4 Sm1 87.7(3) . 2_666 ? Sm1 O4 Sm1 104.06(11) . 2_666 ? C12 O5 Sm1 100.3(3) . 2_666 ? C23 O7 Sm1 135.9(3) 2_666 . ? C23 O8 Sm1 141.0(3) . . ? Sm1 O1W H1WB 126.0 . . ? Sm1 O1W H1WA 108.5 . . ? H1WB O1W H1WA 105.6 . . ? Sm1 O2W H2WA 130.5 . . ? Sm1 O2W H2WB 119.3 . . ? H2WA O2W H2WB 105.6 . . ? H3WA O3W H3WB 106.9 . . ? 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 O4 Sm1 C1 O1 -14.0(3) . . . . ? O8 Sm1 C1 O1 -81.0(3) . . . . ? O7 Sm1 C1 O1 84.1(4) . . . . ? O5 Sm1 C1 O1 -153.7(3) 2_666 . . . ? O2 Sm1 C1 O1 -177.7(5) . . . . ? O1W Sm1 C1 O1 72.8(3) . . . . ? O2W Sm1 C1 O1 137.2(3) . . . . ? O4 Sm1 C1 O1 -110.8(3) 2_666 . . . ? C12 Sm1 C1 O1 -136.0(3) 2_666 . . . ? Sm1 Sm1 C1 O1 -54.9(3) 2_666 . . . ? O4 Sm1 C1 O2 163.7(3) . . . . ? O8 Sm1 C1 O2 96.7(3) . . . . ? O7 Sm1 C1 O2 -98.2(3) . . . . ? O5 Sm1 C1 O2 23.9(3) 2_666 . . . ? O1 Sm1 C1 O2 177.7(5) . . . . ? O1W Sm1 C1 O2 -109.5(3) . . . . ? O2W Sm1 C1 O2 -45.2(3) . . . . ? O4 Sm1 C1 O2 66.9(3) 2_666 . . . ? C12 Sm1 C1 O2 41.6(3) 2_666 . . . ? Sm1 Sm1 C1 O2 122.7(3) 2_666 . . . ? O1 C1 C2 C3 -160.8(5) . . . 2_777 ? O2 C1 C2 C3 15.9(7) . . . 2_777 ? O1 C1 C2 C4 16.9(7) . . . . ? O2 C1 C2 C4 -166.4(5) . . . . ? C2 C3 C4 C2 -0.5(8) 2_777 . . . ? C2 C3 C4 C5 175.9(5) 2_777 . . . ? C3 C2 C4 C3 0.5(8) 2_777 . . . ? C1 C2 C4 C3 -177.3(4) . . . . ? C3 C2 C4 C5 -175.8(5) 2_777 . . . ? C1 C2 C4 C5 6.5(7) . . . . ? C3 C4 C5 O3 -99.3(6) . . . . ? C2 C4 C5 O3 76.9(7) . . . . ? C3 C4 C5 C6 76.7(6) . . . . ? C2 C4 C5 C6 -107.1(6) . . . . ? O3 C5 C6 C7 154.7(5) . . . . ? C4 C5 C6 C7 -21.2(7) . . . . ? O3 C5 C6 C11 -20.6(8) . . . . ? C4 C5 C6 C11 163.5(5) . . . . ? C11 C6 C7 C8 0.9(9) . . . . ? C5 C6 C7 C8 -174.4(6) . . . . ? C6 C7 C8 C9 -0.9(11) . . . . ? C7 C8 C9 C10 -1.5(12) . . . . ? C8 C9 C10 C11 3.7(11) . . . . ? C7 C6 C11 C10 1.4(9) . . . . ? C5 C6 C11 C10 176.9(6) . . . . ? C9 C10 C11 C6 -3.7(10) . . . . ? O5 C12 C13 C15 32.1(7) . . . . ? O4 C12 C13 C15 -148.9(5) . . . . ? O5 C12 C13 C14 -144.8(5) . . . . ? O4 C12 C13 C14 34.3(6) . . . . ? C15 C13 C14 C15 -0.9(8) . . . 2_766 ? C12 C13 C14 C15 176.1(4) . . . 2_766 ? C14 C13 C15 C14 0.9(8) . . . 2_766 ? C12 C13 C15 C14 -176.0(4) . . . 2_766 ? C14 C13 C15 C16 179.8(5) . . . . ? C12 C13 C15 C16 2.9(8) . . . . ? C14 C15 C16 O6 52.2(7) 2_766 . . . ? C13 C15 C16 O6 -126.7(6) . . . . ? C14 C15 C16 C17 -123.1(5) 2_766 . . . ? C13 C15 C16 C17 58.0(7) . . . . ? O6 C16 C17 C18 -166.1(5) . . . . ? C15 C16 C17 C18 9.2(7) . . . . ? O6 C16 C17 C22 12.7(7) . . . . ? C15 C16 C17 C22 -172.1(5) . . . . ? C22 C17 C18 C19 0.2(9) . . . . ? C16 C17 C18 C19 178.9(5) . . . . ? C17 C18 C19 C20 0.3(10) . . . . ? C18 C19 C20 C21 -0.8(11) . . . . ? C19 C20 C21 C22 0.7(11) . . . . ? C20 C21 C22 C17 -0.1(10) . . . . ? C18 C17 C22 C21 -0.3(8) . . . . ? C16 C17 C22 C21 -179.1(5) . . . . ? O8 C23 C24 C25 33.3(6) . . . . ? O7 C23 C24 C25 -144.3(5) 2_666 . . . ? O8 C23 C24 C26 -149.5(4) . . . . ? O7 C23 C24 C26 33.0(7) 2_666 . . . ? C26 C24 C25 C26 -1.3(8) . . . 2_676 ? C23 C24 C25 C26 176.0(4) . . . 2_676 ? C25 C24 C26 C25 1.2(8) . . . 2_676 ? C23 C24 C26 C25 -176.0(4) . . . 2_676 ? C25 C24 C26 C27 -173.4(4) . . . . ? C23 C24 C26 C27 9.4(7) . . . . ? C25 C26 C27 O9 -113.0(5) 2_676 . . . ? C24 C26 C27 O9 61.6(7) . . . . ? C25 C26 C27 C28 67.3(6) 2_676 . . . ? C24 C26 C27 C28 -118.1(5) . . . . ? O9 C27 C28 C33 -166.5(5) . . . . ? C26 C27 C28 C33 13.2(7) . . . . ? O9 C27 C28 C29 12.1(8) . . . . ? C26 C27 C28 C29 -168.2(5) . . . . ? C33 C28 C29 C30 2.8(8) . . . . ? C27 C28 C29 C30 -175.9(5) . . . . ? C28 C29 C30 C31 -1.6(10) . . . . ? C29 C30 C31 C32 0.6(11) . . . . ? C30 C31 C32 C33 -0.9(11) . . . . ? C31 C32 C33 C28 2.1(11) . . . . ? C29 C28 C33 C32 -3.0(9) . . . . ? C27 C28 C33 C32 175.6(6) . . . . ? O2 C1 O1 Sm1 -2.4(5) . . . . ? C2 C1 O1 Sm1 174.1(4) . . . . ? O4 Sm1 O1 C1 167.2(3) . . . . ? O8 Sm1 O1 C1 92.0(3) . . . . ? O7 Sm1 O1 C1 -126.3(3) . . . . ? O5 Sm1 O1 C1 32.4(3) 2_666 . . . ? O2 Sm1 O1 C1 1.3(3) . . . . ? O1W Sm1 O1 C1 -97.2(3) . . . . ? O2W Sm1 O1 C1 -46.4(3) . . . . ? O4 Sm1 O1 C1 102.8(3) 2_666 . . . ? C12 Sm1 O1 C1 62.3(3) 2_666 . . . ? Sm1 Sm1 O1 C1 141.5(3) 2_666 . . . ? O1 C1 O2 Sm1 2.4(5) . . . . ? C2 C1 O2 Sm1 -174.1(4) . . . . ? O4 Sm1 O2 C1 -23.2(4) . . . . ? O8 Sm1 O2 C1 -77.9(3) . . . . ? O7 Sm1 O2 C1 117.9(3) . . . . ? O5 Sm1 O2 C1 -156.4(3) 2_666 . . . ? O1 Sm1 O2 C1 -1.3(3) . . . . ? O1W Sm1 O2 C1 64.7(3) . . . . ? O2W Sm1 O2 C1 132.1(3) . . . . ? O4 Sm1 O2 C1 -134.1(3) 2_666 . . . ? C12 Sm1 O2 C1 -145.1(3) 2_666 . . . ? Sm1 Sm1 O2 C1 -92.8(3) 2_666 . . . ? O5 C12 O4 Sm1 138.1(8) . . . . ? C13 C12 O4 Sm1 -40.9(12) . . . . ? Sm1 C12 O4 Sm1 132.0(10) 2_666 . . . ? O5 C12 O4 Sm1 6.1(4) . . . 2_666 ? C13 C12 O4 Sm1 -172.9(4) . . . 2_666 ? O8 Sm1 O4 C12 158.3(10) . . . . ? O7 Sm1 O4 C12 -53.6(10) . . . . ? O5 Sm1 O4 C12 -139.6(10) 2_666 . . . ? O2 Sm1 O4 C12 101.9(10) . . . . ? O1 Sm1 O4 C12 84.6(10) . . . . ? O1W Sm1 O4 C12 18.6(10) . . . . ? O2W Sm1 O4 C12 -37.3(11) . . . . ? O4 Sm1 O4 C12 -130.1(10) 2_666 . . . ? C1 Sm1 O4 C12 90.7(10) . . . . ? C12 Sm1 O4 C12 -136.0(9) 2_666 . . . ? Sm1 Sm1 O4 C12 -130.1(10) 2_666 . . . ? O8 Sm1 O4 Sm1 -71.57(12) . . . 2_666 ? O7 Sm1 O4 Sm1 76.46(12) . . . 2_666 ? O5 Sm1 O4 Sm1 -9.54(18) 2_666 . . 2_666 ? O2 Sm1 O4 Sm1 -128.00(16) . . . 2_666 ? O1 Sm1 O4 Sm1 -145.30(13) . . . 2_666 ? O1W Sm1 O4 Sm1 148.67(12) . . . 2_666 ? O2W Sm1 O4 Sm1 92.8(2) . . . 2_666 ? O4 Sm1 O4 Sm1 0.0 2_666 . . 2_666 ? C1 Sm1 O4 Sm1 -139.17(12) . . . 2_666 ? C12 Sm1 O4 Sm1 -5.96(14) 2_666 . . 2_666 ? O4 C12 O5 Sm1 -6.8(5) . . . 2_666 ? C13 C12 O5 Sm1 172.2(3) . . . 2_666 ? O4 Sm1 O7 C23 -36.8(4) . . . 2_666 ? O8 Sm1 O7 C23 11.5(5) . . . 2_666 ? O5 Sm1 O7 C23 88.5(4) 2_666 . . 2_666 ? O2 Sm1 O7 C23 168.4(4) . . . 2_666 ? O1 Sm1 O7 C23 -108.5(4) . . . 2_666 ? O1W Sm1 O7 C23 -136.0(5) . . . 2_666 ? O2W Sm1 O7 C23 153.9(5) . . . 2_666 ? O4 Sm1 O7 C23 42.7(4) 2_666 . . 2_666 ? C1 Sm1 O7 C23 -147.2(4) . . . 2_666 ? C12 Sm1 O7 C23 65.9(4) 2_666 . . 2_666 ? Sm1 Sm1 O7 C23 5.7(4) 2_666 . . 2_666 ? O7 C23 O8 Sm1 8.5(8) 2_666 . . . ? C24 C23 O8 Sm1 -168.8(3) . . . . ? O4 Sm1 O8 C23 33.3(5) . . . . ? O7 Sm1 O8 C23 -14.9(5) . . . . ? O5 Sm1 O8 C23 -99.1(5) 2_666 . . . ? O2 Sm1 O8 C23 179.8(5) . . . . ? O1 Sm1 O8 C23 125.9(5) . . . . ? O1W Sm1 O8 C23 113.0(5) . . . . ? O2W Sm1 O8 C23 -131.8(5) . . . . ? O4 Sm1 O8 C23 -47.0(5) 2_666 . . . ? C1 Sm1 O8 C23 152.9(5) . . . . ? C12 Sm1 O8 C23 -74.5(5) 2_666 . . . ? Sm1 Sm1 O8 C23 -9.0(4) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.304 _refine_diff_density_min -0.980 _refine_diff_density_rms 0.180 _database_code_depnum_ccdc_archive 'CCDC 890968' ####################################################################### # # 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_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'C33 H24 Eu O12' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C33 H22 Eu O11, H2 O' _chemical_formula_sum 'C33 H24 Eu O12' _chemical_formula_weight 764.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3979(6) _cell_length_b 11.4388(6) _cell_length_c 14.1007(8) _cell_angle_alpha 102.635(5) _cell_angle_beta 111.321(5) _cell_angle_gamma 100.381(5) _cell_volume 1460.95(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3924 _cell_measurement_theta_min 2.7577 _cell_measurement_theta_max 29.1302 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 2.216 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.99255 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlis (Oxford Diffraction, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9693 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0669 _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 2.76 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5710 _reflns_number_gt 4947 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^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 5710 _refine_ls_number_parameters 415 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.037 _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 0.61396(2) 0.563440(19) 0.658491(16) 0.01448(7) Uani 1 1 d . . . C1 C 0.7982(5) 0.7874(4) 0.8196(3) 0.0220(10) Uani 1 1 d . . . C2 C 0.9013(5) 0.8988(4) 0.9113(3) 0.0226(10) Uani 1 1 d . . . C3 C 0.8924(5) 0.9212(4) 1.0095(3) 0.0247(10) Uani 1 1 d . . . H3 H 0.8193 0.8676 1.0156 0.030 Uiso 1 1 calc R . . C4 C 1.0119(5) 0.9802(4) 0.9024(3) 0.0211(10) Uani 1 1 d . . . C5 C 1.0201(5) 0.9658(4) 0.7952(4) 0.0264(11) Uani 1 1 d . . . C6 C 1.1365(5) 0.9153(4) 0.7788(4) 0.0288(11) Uani 1 1 d . . . C7 C 1.2595(6) 0.9176(5) 0.8607(5) 0.0434(14) Uani 1 1 d . . . H7 H 1.2691 0.9438 0.9308 0.052 Uiso 1 1 calc R . . C8 C 1.3710(7) 0.8814(6) 0.8409(5) 0.0557(17) Uani 1 1 d . . . H8 H 1.4559 0.8866 0.8973 0.067 Uiso 1 1 calc R . . C9 C 1.3531(7) 0.8379(6) 0.7365(5) 0.0534(15) Uani 1 1 d U . . H9 H 1.4265 0.8131 0.7226 0.064 Uiso 1 1 calc R . . C10 C 1.2310(7) 0.8307(6) 0.6541(5) 0.0539(15) Uani 1 1 d U . . H10 H 1.2194 0.7985 0.5840 0.065 Uiso 1 1 calc R . . C11 C 1.1215(7) 0.8716(5) 0.6738(4) 0.0468(15) Uani 1 1 d . . . H11 H 1.0389 0.8698 0.6170 0.056 Uiso 1 1 calc R . . C12 C 0.7007(5) 0.4923(4) 0.4304(3) 0.0178(9) Uani 1 1 d . . . C13 C 0.8570(5) 0.5014(4) 0.4669(3) 0.0190(9) Uani 1 1 d . . . C14 C 0.9289(5) 0.4821(4) 0.5626(3) 0.0205(10) Uani 1 1 d . . . H14 H 0.8805 0.4705 0.6053 0.025 Uiso 1 1 calc R . . C15 C 0.9297(5) 0.5205(4) 0.4024(3) 0.0209(10) Uani 1 1 d . . . C16 C 0.8629(5) 0.5426(4) 0.2961(4) 0.0264(11) Uani 1 1 d . . . C17 C 0.7992(5) 0.6476(5) 0.2881(4) 0.0306(11) Uani 1 1 d . . . C18 C 0.8174(6) 0.7367(5) 0.3785(5) 0.0458(14) Uani 1 1 d . . . H18 H 0.8689 0.7310 0.4459 0.055 Uiso 1 1 calc R . . C19 C 0.7562(8) 0.8390(6) 0.3682(6) 0.067(2) Uani 1 1 d . . . H19 H 0.7664 0.9012 0.4275 0.080 Uiso 1 1 calc R . . C20 C 0.6808(7) 0.8391(6) 0.2641(5) 0.0610(17) Uani 1 1 d U . . H20 H 0.6397 0.9039 0.2548 0.073 Uiso 1 1 calc R . . C21 C 0.6640(7) 0.7539(6) 0.1782(5) 0.0607(17) Uani 1 1 d U . . H21 H 0.6117 0.7587 0.1106 0.073 Uiso 1 1 calc R . . C22 C 0.7240(6) 0.6574(6) 0.1886(5) 0.0458(14) Uani 1 1 d . . . H22 H 0.7138 0.5978 0.1276 0.055 Uiso 1 1 calc R . . C23 C 0.4838(5) 0.7407(4) 0.4959(3) 0.0202(9) Uani 1 1 d . . . C24 C 0.4873(5) 0.8754(4) 0.4980(3) 0.0180(9) Uani 1 1 d . . . C25 C 0.6053(5) 0.9705(4) 0.5764(3) 0.0200(9) Uani 1 1 d . . . H25 H 0.6759 0.9510 0.6284 0.024 Uiso 1 1 calc R . . C26 C 0.3793(5) 0.9045(4) 0.4211(3) 0.0184(9) Uani 1 1 d . . . C27 C 0.2428(5) 0.8080(4) 0.3416(3) 0.0221(10) Uani 1 1 d . . . C28 C 0.2084(5) 0.7815(4) 0.2254(3) 0.0245(10) Uani 1 1 d . . . C29 C 0.3134(6) 0.8238(5) 0.1919(4) 0.0401(13) Uani 1 1 d . . . H29 H 0.4046 0.8737 0.2418 0.048 Uiso 1 1 calc R . . C30 C 0.2807(7) 0.7907(6) 0.0832(5) 0.0557(17) Uani 1 1 d . . . H30 H 0.3508 0.8179 0.0603 0.067 Uiso 1 1 calc R . . C31 C 0.1467(8) 0.7189(6) 0.0099(4) 0.0551(17) Uani 1 1 d . . . H31 H 0.1263 0.6971 -0.0626 0.066 Uiso 1 1 calc R . . C32 C 0.0410(7) 0.6780(5) 0.0418(4) 0.0488(15) Uani 1 1 d . . . H32 H -0.0505 0.6296 -0.0087 0.059 Uiso 1 1 calc R . . C33 C 0.0728(6) 0.7099(4) 0.1501(4) 0.0331(12) Uani 1 1 d . . . H33 H 0.0018 0.6828 0.1722 0.040 Uiso 1 1 calc R . . O1 O 0.6846(3) 0.7308(3) 0.8237(2) 0.0283(7) Uani 1 1 d . . . O2 O 0.8287(3) 0.7486(3) 0.7427(2) 0.0291(8) Uani 1 1 d . . . O3 O 0.9402(4) 1.0001(3) 0.7284(3) 0.0404(9) Uani 1 1 d . . . O4 O 0.6536(3) 0.5284(3) 0.5009(2) 0.0215(7) Uani 1 1 d . . . O5 O 0.6181(3) 0.4487(3) 0.3339(2) 0.0255(7) Uani 1 1 d . . . O6 O 0.8698(4) 0.4772(4) 0.2190(3) 0.0448(10) Uani 1 1 d . . . O7 O 0.5395(3) 0.7228(3) 0.5843(2) 0.0215(7) Uani 1 1 d . . . O8 O 0.4289(3) 0.6589(3) 0.4055(2) 0.0234(7) Uani 1 1 d . . . O9 O 0.1611(4) 0.7525(3) 0.3715(3) 0.0344(8) Uani 1 1 d . . . O1W O 0.5954(4) 0.4624(3) 0.7967(3) 0.0379(9) Uani 1 1 d . . . H1WA H 0.5532 0.3854 0.7812 0.045 Uiso 1 1 d R . . H1WB H 0.5567 0.5042 0.8302 0.045 Uiso 1 1 d R . . O2W O 0.8398(4) 0.5216(3) 0.7653(3) 0.0344(8) Uani 1 1 d . . . H2WA H 0.9252 0.5372 0.7698 0.041 Uiso 1 1 d R . . H2WB H 0.8191 0.4500 0.7732 0.041 Uiso 1 1 d R . . O3W O 0.4990(6) 0.3613(4) 0.0865(4) 0.0823(15) Uani 1 1 d . . . H3WA H 0.4232 0.3205 0.0878 0.099 Uiso 1 1 d R . . H3WB H 0.5704 0.3610 0.1406 0.099 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 0.01354(12) 0.01169(11) 0.01429(11) 0.00203(8) 0.00319(9) 0.00263(9) C1 0.016(3) 0.017(2) 0.022(2) 0.0027(19) 0.000(2) 0.001(2) C2 0.017(3) 0.019(2) 0.021(2) 0.0006(19) 0.001(2) 0.002(2) C3 0.023(3) 0.020(2) 0.025(2) 0.004(2) 0.009(2) 0.000(2) C4 0.021(3) 0.017(2) 0.023(2) 0.0039(19) 0.008(2) 0.004(2) C5 0.025(3) 0.020(2) 0.023(2) -0.002(2) 0.008(2) -0.004(2) C6 0.034(3) 0.024(3) 0.026(3) 0.003(2) 0.013(3) 0.005(2) C7 0.056(4) 0.042(3) 0.046(3) 0.015(3) 0.032(3) 0.022(3) C8 0.050(4) 0.056(4) 0.076(5) 0.029(4) 0.029(4) 0.032(4) C9 0.0532(17) 0.0528(18) 0.0556(17) 0.0141(10) 0.0245(11) 0.0178(11) C10 0.0549(18) 0.0541(18) 0.0535(17) 0.0128(10) 0.0256(12) 0.0155(10) C11 0.052(4) 0.043(3) 0.038(3) 0.001(3) 0.020(3) 0.009(3) C12 0.012(2) 0.017(2) 0.022(2) 0.0070(19) 0.006(2) 0.0002(19) C13 0.019(3) 0.018(2) 0.021(2) 0.0067(19) 0.009(2) 0.008(2) C14 0.021(3) 0.023(2) 0.020(2) 0.0075(19) 0.011(2) 0.007(2) C15 0.019(3) 0.023(2) 0.022(2) 0.0076(19) 0.009(2) 0.008(2) C16 0.015(3) 0.040(3) 0.027(3) 0.017(2) 0.009(2) 0.007(2) C17 0.020(3) 0.038(3) 0.040(3) 0.023(3) 0.013(2) 0.006(2) C18 0.044(4) 0.043(3) 0.061(4) 0.026(3) 0.025(3) 0.016(3) C19 0.070(5) 0.038(4) 0.103(6) 0.012(4) 0.056(5) 0.010(4) C20 0.0597(19) 0.0600(19) 0.0633(19) 0.0226(11) 0.0240(12) 0.0171(11) C21 0.0602(19) 0.0606(19) 0.0615(19) 0.0238(11) 0.0238(12) 0.0153(11) C22 0.030(3) 0.057(4) 0.052(4) 0.034(3) 0.009(3) 0.012(3) C23 0.019(3) 0.016(2) 0.024(2) 0.0077(19) 0.007(2) 0.005(2) C24 0.021(3) 0.013(2) 0.017(2) 0.0032(18) 0.007(2) 0.0030(19) C25 0.022(3) 0.018(2) 0.018(2) 0.0071(18) 0.004(2) 0.008(2) C26 0.022(3) 0.016(2) 0.015(2) 0.0046(17) 0.004(2) 0.008(2) C27 0.020(3) 0.014(2) 0.026(2) 0.0052(19) 0.002(2) 0.007(2) C28 0.026(3) 0.020(2) 0.020(2) 0.0023(19) 0.002(2) 0.009(2) C29 0.034(3) 0.044(3) 0.034(3) 0.010(3) 0.010(3) 0.005(3) C30 0.059(5) 0.078(5) 0.032(3) 0.018(3) 0.022(4) 0.019(4) C31 0.072(5) 0.060(4) 0.021(3) 0.003(3) 0.012(3) 0.020(4) C32 0.051(4) 0.041(3) 0.026(3) 0.001(3) -0.006(3) 0.006(3) C33 0.031(3) 0.030(3) 0.026(3) 0.008(2) 0.001(2) 0.006(2) O1 0.024(2) 0.0262(18) 0.0232(17) -0.0037(14) 0.0100(16) -0.0046(15) O2 0.027(2) 0.0293(18) 0.0228(17) -0.0028(14) 0.0117(16) 0.0001(16) O3 0.038(2) 0.049(2) 0.030(2) 0.0155(18) 0.0075(19) 0.013(2) O4 0.0197(18) 0.0202(16) 0.0266(17) 0.0051(13) 0.0134(15) 0.0050(14) O5 0.0199(19) 0.0353(19) 0.0194(17) 0.0081(14) 0.0060(15) 0.0089(15) O6 0.050(3) 0.064(3) 0.0252(19) 0.0125(18) 0.0166(19) 0.027(2) O7 0.0251(19) 0.0165(16) 0.0191(16) 0.0069(13) 0.0036(15) 0.0073(14) O8 0.030(2) 0.0133(15) 0.0175(16) 0.0015(13) 0.0020(15) 0.0048(14) O9 0.029(2) 0.031(2) 0.0334(19) 0.0117(16) 0.0079(17) -0.0054(16) O1W 0.045(2) 0.034(2) 0.044(2) 0.0208(17) 0.022(2) 0.0151(19) O2W 0.027(2) 0.034(2) 0.044(2) 0.0155(17) 0.0122(18) 0.0127(17) O3W 0.093(4) 0.091(4) 0.065(3) 0.021(3) 0.043(3) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O4 2.367(2) . ? Eu1 O7 2.403(3) . ? Eu1 O8 2.403(3) 2_666 ? Eu1 O5 2.435(3) 2_666 ? Eu1 O1 2.435(3) . ? Eu1 O2 2.480(3) . ? Eu1 O2W 2.481(3) . ? Eu1 O1W 2.519(3) . ? Eu1 O4 2.695(3) 2_666 ? C1 O2 1.251(5) . ? C1 O1 1.267(5) . ? C1 C2 1.491(6) . ? C2 C3 1.392(6) . ? C2 C4 1.405(6) . ? C3 C4 1.375(6) 2_777 ? C3 H3 0.9300 . ? C4 C3 1.375(6) 2_777 ? C4 C5 1.520(6) . ? C5 O3 1.200(5) . ? C5 C6 1.500(6) . ? C6 C7 1.367(7) . ? C6 C11 1.395(6) . ? C7 C8 1.397(7) . ? C7 H7 0.9300 . ? C8 C9 1.378(8) . ? C8 H8 0.9300 . ? C9 C10 1.348(8) . ? C9 H9 0.9300 . ? C10 C11 1.398(7) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O5 1.240(5) . ? C12 O4 1.282(4) . ? C12 C13 1.491(6) . ? C12 Eu1 2.932(4) 2_666 ? C13 C14 1.372(6) . ? C13 C15 1.405(5) . ? C14 C15 1.379(6) 2_766 ? C14 H14 0.9300 . ? C15 C14 1.379(6) 2_766 ? C15 C16 1.504(6) . ? C16 O6 1.212(5) . ? C16 C17 1.479(6) . ? C17 C18 1.374(7) . ? C17 C22 1.377(7) . ? C18 C19 1.438(8) . ? C18 H18 0.9300 . ? C19 C20 1.391(9) . ? C19 H19 0.9300 . ? C20 C21 1.310(8) . ? C20 H20 0.9300 . ? C21 C22 1.372(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O7 1.250(5) . ? C23 O8 1.258(5) . ? C23 C24 1.527(5) . ? C24 C25 1.385(6) . ? C24 C26 1.399(6) . ? C25 C26 1.400(5) 2_676 ? C25 H25 0.9300 . ? C26 C25 1.400(5) 2_676 ? C26 C27 1.492(6) . ? C27 O9 1.219(5) . ? C27 C28 1.490(6) . ? C28 C33 1.379(7) . ? C28 C29 1.390(6) . ? C29 C30 1.389(7) . ? C29 H29 0.9300 . ? C30 C31 1.362(9) . ? C30 H30 0.9300 . ? C31 C32 1.376(8) . ? C31 H31 0.9300 . ? C32 C33 1.386(7) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? O4 Eu1 2.695(3) 2_666 ? O5 Eu1 2.435(3) 2_666 ? O8 Eu1 2.403(3) 2_666 ? O1W H1WA 0.8499 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8510 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8501 . ? 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 O7 75.65(9) . . ? O4 Eu1 O8 75.16(9) . 2_666 ? O7 Eu1 O8 136.68(10) . 2_666 ? O4 Eu1 O5 125.72(10) . 2_666 ? O7 Eu1 O5 77.01(10) . 2_666 ? O8 Eu1 O5 95.18(10) 2_666 2_666 ? O4 Eu1 O1 139.00(10) . . ? O7 Eu1 O1 80.61(10) . . ? O8 Eu1 O1 140.50(10) 2_666 . ? O5 Eu1 O1 79.27(10) 2_666 . ? O4 Eu1 O2 88.10(10) . . ? O7 Eu1 O2 73.96(10) . . ? O8 Eu1 O2 135.58(10) 2_666 . ? O5 Eu1 O2 127.03(10) 2_666 . ? O1 Eu1 O2 53.08(9) . . ? O4 Eu1 O2W 94.02(10) . . ? O7 Eu1 O2W 138.96(11) . . ? O8 Eu1 O2W 74.38(11) 2_666 . ? O5 Eu1 O2W 135.38(10) 2_666 . ? O1 Eu1 O2W 82.45(10) . . ? O2 Eu1 O2W 65.97(11) . . ? O4 Eu1 O1W 142.20(10) . . ? O7 Eu1 O1W 140.35(9) . . ? O8 Eu1 O1W 68.75(10) 2_666 . ? O5 Eu1 O1W 69.67(10) 2_666 . ? O1 Eu1 O1W 72.75(10) . . ? O2 Eu1 O1W 109.90(11) . . ? O2W Eu1 O1W 66.10(10) . . ? O4 Eu1 O4 76.15(10) . 2_666 ? O7 Eu1 O4 68.97(9) . 2_666 ? O8 Eu1 O4 73.44(9) 2_666 2_666 ? O5 Eu1 O4 50.37(9) 2_666 2_666 ? O1 Eu1 O4 124.95(9) . 2_666 ? O2 Eu1 O4 142.23(9) . 2_666 ? O2W Eu1 O4 147.78(10) . 2_666 ? O1W Eu1 O4 103.20(10) . 2_666 ? O4 Eu1 C1 113.80(11) . . ? O7 Eu1 C1 76.42(11) . . ? O8 Eu1 C1 145.47(11) 2_666 . ? O5 Eu1 C1 103.88(11) 2_666 . ? O1 Eu1 C1 26.71(10) . . ? O2 Eu1 C1 26.38(10) . . ? O2W Eu1 C1 71.80(11) . . ? O1W Eu1 C1 91.06(12) . . ? O4 Eu1 C1 140.31(10) 2_666 . ? O4 Eu1 C12 101.39(11) . 2_666 ? O7 Eu1 C12 69.86(10) . 2_666 ? O8 Eu1 C12 85.43(11) 2_666 2_666 ? O5 Eu1 C12 24.55(10) 2_666 2_666 ? O1 Eu1 C12 101.12(11) . 2_666 ? O2 Eu1 C12 138.70(10) . 2_666 ? O2W Eu1 C12 150.56(11) . 2_666 ? O1W Eu1 C12 86.84(11) . 2_666 ? O4 Eu1 C12 25.90(9) 2_666 2_666 ? C1 Eu1 C12 122.42(11) . 2_666 ? O4 Eu1 Eu1 40.97(7) . 2_666 ? O7 Eu1 Eu1 67.08(7) . 2_666 ? O8 Eu1 Eu1 69.85(7) 2_666 2_666 ? O5 Eu1 Eu1 85.17(7) 2_666 2_666 ? O1 Eu1 Eu1 146.58(8) . 2_666 ? O2 Eu1 Eu1 120.94(7) . 2_666 ? O2W Eu1 Eu1 127.80(7) . 2_666 ? O1W Eu1 Eu1 128.54(9) . 2_666 ? O4 Eu1 Eu1 35.18(5) 2_666 2_666 ? C1 Eu1 Eu1 139.39(9) . 2_666 ? C12 Eu1 Eu1 60.64(8) 2_666 2_666 ? O2 C1 O1 121.4(4) . . ? O2 C1 C2 119.3(4) . . ? O1 C1 C2 119.2(4) . . ? O2 C1 Eu1 61.8(2) . . ? O1 C1 Eu1 59.7(2) . . ? C2 C1 Eu1 174.7(3) . . ? C3 C2 C4 118.6(4) . . ? C3 C2 C1 119.9(4) . . ? C4 C2 C1 121.5(4) . . ? C4 C3 C2 122.2(4) 2_777 . ? C4 C3 H3 118.9 2_777 . ? C2 C3 H3 118.9 . . ? C3 C4 C2 119.1(4) 2_777 . ? C3 C4 C5 119.9(4) 2_777 . ? C2 C4 C5 120.8(4) . . ? O3 C5 C6 121.5(4) . . ? O3 C5 C4 120.5(4) . . ? C6 C5 C4 117.9(4) . . ? C7 C6 C11 118.8(4) . . ? C7 C6 C5 123.7(4) . . ? C11 C6 C5 117.3(5) . . ? C6 C7 C8 121.1(5) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 118.9(6) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C10 C9 C8 121.1(5) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 120.1(5) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C6 C11 C10 119.9(6) . . ? C6 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? O5 C12 O4 121.0(4) . . ? O5 C12 C13 120.3(3) . . ? O4 C12 C13 118.7(4) . . ? O5 C12 Eu1 54.6(2) . 2_666 ? O4 C12 Eu1 66.6(2) . 2_666 ? C13 C12 Eu1 171.7(3) . 2_666 ? C14 C13 C15 119.3(4) . . ? C14 C13 C12 119.0(4) . . ? C15 C13 C12 121.6(4) . . ? C13 C14 C15 122.3(4) . 2_766 ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 2_766 . ? C14 C15 C13 118.5(4) 2_766 . ? C14 C15 C16 117.3(3) 2_766 . ? C13 C15 C16 124.3(4) . . ? O6 C16 C17 120.9(4) . . ? O6 C16 C15 118.6(4) . . ? C17 C16 C15 120.4(4) . . ? C18 C17 C22 119.9(5) . . ? C18 C17 C16 120.8(5) . . ? C22 C17 C16 119.3(5) . . ? C17 C18 C19 119.6(6) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 115.9(6) . . ? C20 C19 H19 122.0 . . ? C18 C19 H19 122.0 . . ? C21 C20 C19 124.2(6) . . ? C21 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? C20 C21 C22 119.6(7) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C17 120.8(6) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? O7 C23 O8 126.0(4) . . ? O7 C23 C24 116.7(4) . . ? O8 C23 C24 117.2(4) . . ? C25 C24 C26 119.5(4) . . ? C25 C24 C23 118.2(4) . . ? C26 C24 C23 122.2(4) . . ? C24 C25 C26 121.4(4) . 2_676 ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 2_676 . ? C24 C26 C25 119.1(4) . 2_676 ? C24 C26 C27 122.0(4) . . ? C25 C26 C27 118.7(4) 2_676 . ? O9 C27 C28 120.9(4) . . ? O9 C27 C26 120.4(4) . . ? C28 C27 C26 118.8(4) . . ? C33 C28 C29 119.5(4) . . ? C33 C28 C27 119.8(4) . . ? C29 C28 C27 120.7(4) . . ? C30 C29 C28 119.4(5) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C31 C30 C29 120.4(5) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.8(5) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C31 C32 C33 119.2(6) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C28 C33 C32 120.7(5) . . ? C28 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C1 O1 Eu1 93.5(2) . . ? C1 O2 Eu1 91.9(3) . . ? C12 O4 Eu1 162.7(3) . . ? C12 O4 Eu1 87.5(2) . 2_666 ? Eu1 O4 Eu1 103.85(10) . 2_666 ? C12 O5 Eu1 100.8(2) . 2_666 ? C23 O7 Eu1 140.6(3) . . ? C23 O8 Eu1 135.6(3) . 2_666 ? Eu1 O1W H1WA 123.2 . . ? Eu1 O1W H1WB 106.6 . . ? H1WA O1W H1WB 107.4 . . ? Eu1 O2W H2WA 135.6 . . ? Eu1 O2W H2WB 109.0 . . ? H2WA O2W H2WB 107.4 . . ? H3WA O3W H3WB 107.4 . . ? 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 O4 Eu1 C1 O2 -13.9(3) . . . . ? O7 Eu1 C1 O2 -81.2(2) . . . . ? O8 Eu1 C1 O2 84.6(3) 2_666 . . . ? O5 Eu1 C1 O2 -153.9(2) 2_666 . . . ? O1 Eu1 C1 O2 -177.3(4) . . . . ? O2W Eu1 C1 O2 72.4(2) . . . . ? O1W Eu1 C1 O2 136.8(2) . . . . ? O4 Eu1 C1 O2 -110.9(2) 2_666 . . . ? C12 Eu1 C1 O2 -136.3(2) 2_666 . . . ? Eu1 Eu1 C1 O2 -55.0(3) 2_666 . . . ? O4 Eu1 C1 O1 163.5(2) . . . . ? O7 Eu1 C1 O1 96.1(2) . . . . ? O8 Eu1 C1 O1 -98.1(3) 2_666 . . . ? O5 Eu1 C1 O1 23.4(3) 2_666 . . . ? O2 Eu1 C1 O1 177.3(4) . . . . ? O2W Eu1 C1 O1 -110.2(3) . . . . ? O1W Eu1 C1 O1 -45.9(2) . . . . ? O4 Eu1 C1 O1 66.5(3) 2_666 . . . ? C12 Eu1 C1 O1 41.1(3) 2_666 . . . ? Eu1 Eu1 C1 O1 122.3(2) 2_666 . . . ? O2 C1 C2 C3 -160.7(4) . . . . ? O1 C1 C2 C3 16.1(6) . . . . ? O2 C1 C2 C4 16.7(6) . . . . ? O1 C1 C2 C4 -166.4(4) . . . . ? C4 C2 C3 C4 -0.1(7) . . . 2_777 ? C1 C2 C3 C4 177.5(4) . . . 2_777 ? C3 C2 C4 C3 0.1(7) . . . 2_777 ? C1 C2 C4 C3 -177.5(4) . . . 2_777 ? C3 C2 C4 C5 -175.5(4) . . . . ? C1 C2 C4 C5 6.9(6) . . . . ? C3 C4 C5 O3 -99.2(6) 2_777 . . . ? C2 C4 C5 O3 76.4(6) . . . . ? C3 C4 C5 C6 77.0(5) 2_777 . . . ? C2 C4 C5 C6 -107.4(5) . . . . ? O3 C5 C6 C7 155.1(5) . . . . ? C4 C5 C6 C7 -21.0(7) . . . . ? O3 C5 C6 C11 -20.3(7) . . . . ? C4 C5 C6 C11 163.6(4) . . . . ? C11 C6 C7 C8 2.2(8) . . . . ? C5 C6 C7 C8 -173.1(5) . . . . ? C6 C7 C8 C9 -2.7(9) . . . . ? C7 C8 C9 C10 0.4(9) . . . . ? C8 C9 C10 C11 2.2(9) . . . . ? C7 C6 C11 C10 0.4(8) . . . . ? C5 C6 C11 C10 176.0(5) . . . . ? C9 C10 C11 C6 -2.6(9) . . . . ? O5 C12 C13 C14 -144.5(4) . . . . ? O4 C12 C13 C14 34.3(6) . . . . ? O5 C12 C13 C15 31.0(6) . . . . ? O4 C12 C13 C15 -150.2(4) . . . . ? C15 C13 C14 C15 -0.7(7) . . . 2_766 ? C12 C13 C14 C15 174.9(4) . . . 2_766 ? C14 C13 C15 C14 0.6(7) . . . 2_766 ? C12 C13 C15 C14 -174.8(4) . . . 2_766 ? C14 C13 C15 C16 -180.0(4) . . . . ? C12 C13 C15 C16 4.6(6) . . . . ? C14 C15 C16 O6 52.2(6) 2_766 . . . ? C13 C15 C16 O6 -127.2(5) . . . . ? C14 C15 C16 C17 -123.7(4) 2_766 . . . ? C13 C15 C16 C17 57.0(6) . . . . ? O6 C16 C17 C18 -166.6(5) . . . . ? C15 C16 C17 C18 9.2(7) . . . . ? O6 C16 C17 C22 11.8(7) . . . . ? C15 C16 C17 C22 -172.5(4) . . . . ? C22 C17 C18 C19 0.6(8) . . . . ? C16 C17 C18 C19 179.0(5) . . . . ? C17 C18 C19 C20 0.2(8) . . . . ? C18 C19 C20 C21 -0.2(10) . . . . ? C19 C20 C21 C22 -0.5(10) . . . . ? C20 C21 C22 C17 1.4(9) . . . . ? C18 C17 C22 C21 -1.4(8) . . . . ? C16 C17 C22 C21 -179.8(5) . . . . ? O7 C23 C24 C25 34.2(5) . . . . ? O8 C23 C24 C25 -144.0(4) . . . . ? O7 C23 C24 C26 -148.8(4) . . . . ? O8 C23 C24 C26 33.0(5) . . . . ? C26 C24 C25 C26 -1.5(6) . . . 2_676 ? C23 C24 C25 C26 175.6(3) . . . 2_676 ? C25 C24 C26 C25 1.5(6) . . . 2_676 ? C23 C24 C26 C25 -175.5(3) . . . 2_676 ? C25 C24 C26 C27 -173.7(4) . . . . ? C23 C24 C26 C27 9.3(5) . . . . ? C24 C26 C27 O9 61.6(5) . . . . ? C25 C26 C27 O9 -113.6(4) 2_676 . . . ? C24 C26 C27 C28 -118.6(4) . . . . ? C25 C26 C27 C28 66.2(5) 2_676 . . . ? O9 C27 C28 C33 11.3(6) . . . . ? C26 C27 C28 C33 -168.5(4) . . . . ? O9 C27 C28 C29 -166.1(4) . . . . ? C26 C27 C28 C29 14.1(6) . . . . ? C33 C28 C29 C30 -1.5(7) . . . . ? C27 C28 C29 C30 175.9(4) . . . . ? C28 C29 C30 C31 0.8(8) . . . . ? C29 C30 C31 C32 0.3(9) . . . . ? C30 C31 C32 C33 -0.6(9) . . . . ? C29 C28 C33 C32 1.2(7) . . . . ? C27 C28 C33 C32 -176.2(4) . . . . ? C31 C32 C33 C28 -0.1(8) . . . . ? O2 C1 O1 Eu1 2.8(4) . . . . ? C2 C1 O1 Eu1 -174.0(3) . . . . ? O4 Eu1 O1 C1 -23.4(3) . . . . ? O7 Eu1 O1 C1 -78.4(3) . . . . ? O8 Eu1 O1 C1 118.1(3) 2_666 . . . ? O5 Eu1 O1 C1 -156.8(3) 2_666 . . . ? O2 Eu1 O1 C1 -1.5(2) . . . . ? O2W Eu1 O1 C1 64.1(3) . . . . ? O1W Eu1 O1 C1 131.3(3) . . . . ? O4 Eu1 O1 C1 -134.4(2) 2_666 . . . ? C12 Eu1 O1 C1 -145.6(2) 2_666 . . . ? Eu1 Eu1 O1 C1 -93.1(3) 2_666 . . . ? O1 C1 O2 Eu1 -2.7(4) . . . . ? C2 C1 O2 Eu1 174.0(3) . . . . ? O4 Eu1 O2 C1 167.3(2) . . . . ? O7 Eu1 O2 C1 91.7(2) . . . . ? O8 Eu1 O2 C1 -126.3(2) 2_666 . . . ? O5 Eu1 O2 C1 32.4(3) 2_666 . . . ? O1 Eu1 O2 C1 1.5(2) . . . . ? O2W Eu1 O2 C1 -97.4(3) . . . . ? O1W Eu1 O2 C1 -46.7(3) . . . . ? O4 Eu1 O2 C1 103.0(3) 2_666 . . . ? C12 Eu1 O2 C1 62.2(3) 2_666 . . . ? Eu1 Eu1 O2 C1 141.6(2) 2_666 . . . ? O5 C12 O4 Eu1 137.3(8) . . . . ? C13 C12 O4 Eu1 -41.5(11) . . . . ? Eu1 C12 O4 Eu1 131.4(9) 2_666 . . . ? O5 C12 O4 Eu1 5.9(4) . . . 2_666 ? C13 C12 O4 Eu1 -172.9(3) . . . 2_666 ? O7 Eu1 O4 C12 159.1(9) . . . . ? O8 Eu1 O4 C12 -53.3(9) 2_666 . . . ? O5 Eu1 O4 C12 -139.0(9) 2_666 . . . ? O1 Eu1 O4 C12 102.5(9) . . . . ? O2 Eu1 O4 C12 85.1(9) . . . . ? O2W Eu1 O4 C12 19.4(9) . . . . ? O1W Eu1 O4 C12 -35.7(10) . . . . ? O4 Eu1 O4 C12 -129.5(9) 2_666 . . . ? C1 Eu1 O4 C12 91.2(9) . . . . ? C12 Eu1 O4 C12 -135.4(9) 2_666 . . . ? Eu1 Eu1 O4 C12 -129.5(9) 2_666 . . . ? O7 Eu1 O4 Eu1 -71.43(10) . . . 2_666 ? O8 Eu1 O4 Eu1 76.21(10) 2_666 . . 2_666 ? O5 Eu1 O4 Eu1 -9.45(15) 2_666 . . 2_666 ? O1 Eu1 O4 Eu1 -128.00(14) . . . 2_666 ? O2 Eu1 O4 Eu1 -145.36(10) . . . 2_666 ? O2W Eu1 O4 Eu1 148.89(11) . . . 2_666 ? O1W Eu1 O4 Eu1 93.78(17) . . . 2_666 ? O4 Eu1 O4 Eu1 0.0 2_666 . . 2_666 ? C1 Eu1 O4 Eu1 -139.25(11) . . . 2_666 ? C12 Eu1 O4 Eu1 -5.89(11) 2_666 . . 2_666 ? O4 C12 O5 Eu1 -6.7(4) . . . 2_666 ? C13 C12 O5 Eu1 172.1(3) . . . 2_666 ? O8 C23 O7 Eu1 9.6(7) . . . . ? C24 C23 O7 Eu1 -168.4(3) . . . . ? O4 Eu1 O7 C23 32.5(4) . . . . ? O8 Eu1 O7 C23 -16.5(5) 2_666 . . . ? O5 Eu1 O7 C23 -100.2(4) 2_666 . . . ? O1 Eu1 O7 C23 178.8(4) . . . . ? O2 Eu1 O7 C23 124.6(4) . . . . ? O2W Eu1 O7 C23 111.9(4) . . . . ? O1W Eu1 O7 C23 -133.3(4) . . . . ? O4 Eu1 O7 C23 -48.0(4) 2_666 . . . ? C1 Eu1 O7 C23 151.8(4) . . . . ? C12 Eu1 O7 C23 -75.6(4) 2_666 . . . ? Eu1 Eu1 O7 C23 -10.0(4) 2_666 . . . ? O7 C23 O8 Eu1 2.5(7) . . . 2_666 ? C24 C23 O8 Eu1 -179.5(2) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.113 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.124 _database_code_depnum_ccdc_archive 'CCDC 890969' ####################################################################### # # 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_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H22 Gd O11, H2 O' _chemical_formula_sum 'C33 H24 Gd O12' _chemical_formula_weight 769.77 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' Gd Gd -0.1653 3.9035 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4002(6) _cell_length_b 11.4239(6) _cell_length_c 14.1035(8) _cell_angle_alpha 102.7800(10) _cell_angle_beta 111.3540(10) _cell_angle_gamma 100.2750(10) _cell_volume 1458.80(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4490 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.05 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 2.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6268 _exptl_absorpt_correction_T_max 0.6779 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7988 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5612 _reflns_number_gt 5191 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+1.6785P] 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 5612 _refine_ls_number_parameters 415 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.052 _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 0.613372(17) 0.563779(14) 0.658266(12) 0.01465(6) Uani 1 1 d . . . C1 C 0.7972(4) 0.7860(3) 0.8192(3) 0.0222(8) Uani 1 1 d . . . C2 C 0.9010(4) 0.8994(3) 0.9110(3) 0.0233(8) Uani 1 1 d . . . C3 C 1.1080(4) 1.0789(3) 0.9906(3) 0.0251(8) Uani 1 1 d . . . H3 H 1.1809 1.1329 0.9845 0.030 Uiso 1 1 calc R . . C4 C 1.0115(4) 0.9792(3) 0.9017(3) 0.0229(8) Uani 1 1 d . . . C5 C 1.0211(4) 0.9648(3) 0.7955(3) 0.0262(8) Uani 1 1 d . . . C6 C 1.1363(5) 0.9153(4) 0.7779(3) 0.0302(9) Uani 1 1 d . . . C7 C 1.2600(5) 0.9174(4) 0.8614(4) 0.0416(11) Uani 1 1 d . . . H7 H 1.2688 0.9428 0.9314 0.050 Uiso 1 1 calc R . . C8 C 1.3716(6) 0.8816(5) 0.8415(5) 0.0575(14) Uani 1 1 d . . . H8 H 1.4562 0.8869 0.8982 0.069 Uiso 1 1 calc R . . C9 C 1.3558(6) 0.8387(5) 0.7378(5) 0.0579(14) Uani 1 1 d U . . H9 H 1.4296 0.8138 0.7244 0.070 Uiso 1 1 calc R . . C10 C 1.2325(6) 0.8323(5) 0.6543(5) 0.0587(14) Uani 1 1 d U . . H10 H 1.2220 0.8014 0.5843 0.070 Uiso 1 1 calc R . . C11 C 1.1217(6) 0.8718(5) 0.6732(4) 0.0490(13) Uani 1 1 d . . . H11 H 1.0388 0.8689 0.6162 0.059 Uiso 1 1 calc R . . C12 C 0.4846(4) 0.7407(3) 0.4961(3) 0.0186(7) Uani 1 1 d . . . C13 C 0.4871(4) 0.8742(3) 0.4980(3) 0.0196(7) Uani 1 1 d . . . C14 C 0.6057(4) 0.9708(3) 0.5765(3) 0.0209(7) Uani 1 1 d . . . H14 H 0.6768 0.9520 0.6286 0.025 Uiso 1 1 calc R . . C15 C 0.3803(4) 0.9048(3) 0.4217(3) 0.0197(7) Uani 1 1 d . . . C16 C 0.2418(4) 0.8068(3) 0.3407(3) 0.0223(8) Uani 1 1 d . . . C17 C 0.2083(4) 0.7807(3) 0.2252(3) 0.0247(8) Uani 1 1 d . . . C18 C 0.0715(5) 0.7090(4) 0.1493(3) 0.0380(10) Uani 1 1 d . . . H18 H 0.0006 0.6821 0.1714 0.046 Uiso 1 1 calc R . . C19 C 0.0395(6) 0.6771(5) 0.0416(4) 0.0503(13) Uani 1 1 d . . . H19 H -0.0523 0.6286 -0.0086 0.060 Uiso 1 1 calc R . . C20 C 0.1443(7) 0.7177(5) 0.0083(4) 0.0574(15) Uani 1 1 d . . . H20 H 0.1230 0.6967 -0.0644 0.069 Uiso 1 1 calc R . . C21 C 0.2804(7) 0.7892(6) 0.0830(4) 0.0602(15) Uani 1 1 d . . . H21 H 0.3511 0.8155 0.0605 0.072 Uiso 1 1 calc R . . C22 C 0.3119(5) 0.8218(5) 0.1904(3) 0.0408(11) Uani 1 1 d . . . H22 H 0.4032 0.8717 0.2402 0.049 Uiso 1 1 calc R . . C23 C 0.7005(4) 0.4929(3) 0.4315(3) 0.0186(7) Uani 1 1 d . . . C24 C 0.8562(4) 0.5019(3) 0.4666(3) 0.0209(7) Uani 1 1 d . . . C25 C 0.9299(4) 0.4830(4) 0.5636(3) 0.0259(8) Uani 1 1 d . . . H25 H 0.8820 0.4712 0.6066 0.031 Uiso 1 1 calc R . . C26 C 0.9283(4) 0.5190(3) 0.4017(3) 0.0233(8) Uani 1 1 d . . . C27 C 0.8615(4) 0.5408(4) 0.2952(3) 0.0297(9) Uani 1 1 d . . . C28 C 0.7981(4) 0.6465(4) 0.2878(4) 0.0366(10) Uani 1 1 d . . . C29 C 0.8154(6) 0.7372(5) 0.3769(5) 0.0506(13) Uani 1 1 d . . . H29 H 0.8666 0.7317 0.4445 0.061 Uiso 1 1 calc R . . C30 C 0.7575(7) 0.8380(6) 0.3682(5) 0.0716(17) Uani 1 1 d U . . H30 H 0.7697 0.9002 0.4284 0.086 Uiso 1 1 calc R . . C31 C 0.6814(7) 0.8407(6) 0.2658(5) 0.0671(16) Uani 1 1 d U . . H31 H 0.6406 0.9060 0.2579 0.080 Uiso 1 1 calc R . . C32 C 0.6639(7) 0.7547(6) 0.1784(5) 0.0644(15) Uani 1 1 d U . . H32 H 0.6118 0.7608 0.1113 0.077 Uiso 1 1 calc R . . C33 C 0.7228(5) 0.6555(5) 0.1867(5) 0.0532(14) Uani 1 1 d . . . H33 H 0.7122 0.5959 0.1254 0.064 Uiso 1 1 calc R . . O1 O 0.6837(3) 0.7312(2) 0.8228(2) 0.0287(6) Uani 1 1 d . . . O2 O 0.8276(3) 0.7472(2) 0.7420(2) 0.0308(6) Uani 1 1 d . . . O3 O 0.9403(3) 0.9997(3) 0.7282(2) 0.0413(7) Uani 1 1 d . . . O4 O 0.4296(3) 0.6583(2) 0.40547(19) 0.0253(6) Uani 1 1 d . . . O5 O 0.5397(3) 0.7226(2) 0.58474(19) 0.0227(5) Uani 1 1 d . . . O6 O 0.1620(3) 0.7528(3) 0.3719(2) 0.0363(7) Uani 1 1 d . . . O7 O 0.6179(3) 0.4487(3) 0.3346(2) 0.0256(6) Uani 1 1 d . . . O8 O 0.6541(3) 0.5282(2) 0.5021(2) 0.0224(5) Uani 1 1 d . . . O9 O 0.8697(4) 0.4758(3) 0.2187(2) 0.0483(8) Uani 1 1 d . . . O1W O 0.8379(3) 0.5210(3) 0.7647(2) 0.0354(7) Uani 1 1 d . . . H1WA H 0.9285 0.5365 0.7803 0.042 Uiso 1 1 d R . . H1WB H 0.7996 0.4453 0.7221 0.042 Uiso 1 1 d R . . O2W O 0.5944(3) 0.4638(3) 0.7960(2) 0.0411(7) Uani 1 1 d . . . H2WB H 0.6210 0.3991 0.8038 0.049 Uiso 1 1 d R . . H2WA H 0.5708 0.4865 0.8474 0.049 Uiso 1 1 d R . . O3W O 0.5015(6) 0.6406(5) 0.9139(4) 0.0888(15) Uani 1 1 d . . . H3WA H 0.5767 0.6824 0.9120 0.107 Uiso 1 1 d R . . H3WB H 0.4412 0.6023 0.8489 0.107 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 0.01386(10) 0.01125(9) 0.01418(9) 0.00129(6) 0.00293(7) 0.00244(6) C1 0.0202(19) 0.0169(17) 0.0190(18) 0.0006(14) 0.0012(15) 0.0020(15) C2 0.0182(18) 0.0199(18) 0.0218(18) -0.0014(15) 0.0042(15) 0.0014(15) C3 0.0186(19) 0.0233(19) 0.0237(19) -0.0010(15) 0.0065(16) -0.0011(15) C4 0.0202(19) 0.0214(18) 0.0201(18) -0.0005(15) 0.0062(15) 0.0033(15) C5 0.025(2) 0.0190(18) 0.0235(19) -0.0007(15) 0.0064(17) -0.0018(16) C6 0.036(2) 0.025(2) 0.030(2) 0.0048(17) 0.0172(19) 0.0048(17) C7 0.047(3) 0.045(3) 0.044(3) 0.018(2) 0.025(2) 0.022(2) C8 0.054(3) 0.056(3) 0.076(4) 0.026(3) 0.032(3) 0.033(3) C9 0.0579(16) 0.0573(16) 0.0603(16) 0.0152(10) 0.0274(11) 0.0188(10) C10 0.0603(17) 0.0590(17) 0.0579(16) 0.0137(10) 0.0287(11) 0.0171(10) C11 0.057(3) 0.045(3) 0.040(3) -0.002(2) 0.026(3) 0.008(2) C12 0.0169(17) 0.0148(17) 0.0234(18) 0.0068(14) 0.0068(15) 0.0052(14) C13 0.0222(19) 0.0138(16) 0.0201(17) 0.0041(14) 0.0068(15) 0.0049(14) C14 0.0236(19) 0.0127(16) 0.0200(17) 0.0045(14) 0.0024(15) 0.0053(14) C15 0.0232(19) 0.0137(16) 0.0187(17) 0.0035(13) 0.0067(15) 0.0034(14) C16 0.0209(19) 0.0123(16) 0.0260(19) 0.0055(14) 0.0022(16) 0.0038(14) C17 0.027(2) 0.0190(18) 0.0216(19) 0.0042(15) 0.0035(16) 0.0074(16) C18 0.034(2) 0.030(2) 0.031(2) 0.0065(18) -0.0018(19) 0.0014(19) C19 0.048(3) 0.042(3) 0.030(2) 0.000(2) -0.007(2) 0.004(2) C20 0.073(4) 0.063(4) 0.021(2) 0.005(2) 0.008(3) 0.019(3) C21 0.064(4) 0.079(4) 0.038(3) 0.012(3) 0.026(3) 0.020(3) C22 0.035(2) 0.052(3) 0.025(2) 0.005(2) 0.0077(19) 0.005(2) C23 0.0195(18) 0.0168(17) 0.0211(18) 0.0070(14) 0.0095(15) 0.0052(14) C24 0.0187(18) 0.0204(18) 0.0216(18) 0.0031(15) 0.0082(15) 0.0055(15) C25 0.023(2) 0.032(2) 0.026(2) 0.0105(17) 0.0125(17) 0.0062(17) C26 0.0206(19) 0.0252(19) 0.0215(18) 0.0055(15) 0.0069(16) 0.0069(16) C27 0.020(2) 0.045(2) 0.024(2) 0.0122(18) 0.0087(17) 0.0081(18) C28 0.026(2) 0.046(3) 0.050(3) 0.031(2) 0.019(2) 0.012(2) C29 0.054(3) 0.040(3) 0.072(4) 0.027(3) 0.033(3) 0.020(2) C30 0.0714(19) 0.0702(19) 0.0736(19) 0.0220(11) 0.0313(12) 0.0201(11) C31 0.0653(18) 0.0657(18) 0.0701(18) 0.0242(11) 0.0264(11) 0.0191(11) C32 0.0637(18) 0.0642(18) 0.0653(18) 0.0260(11) 0.0243(11) 0.0171(10) C33 0.038(3) 0.071(4) 0.063(3) 0.046(3) 0.021(3) 0.015(3) O1 0.0225(14) 0.0258(14) 0.0245(14) -0.0039(11) 0.0077(12) -0.0050(11) O2 0.0261(15) 0.0283(15) 0.0255(14) -0.0068(12) 0.0111(12) -0.0032(12) O3 0.0358(18) 0.052(2) 0.0308(16) 0.0136(15) 0.0076(14) 0.0140(15) O4 0.0328(15) 0.0138(12) 0.0189(13) 0.0004(10) 0.0032(11) 0.0047(11) O5 0.0271(14) 0.0157(12) 0.0210(13) 0.0066(10) 0.0044(11) 0.0073(11) O6 0.0310(16) 0.0338(16) 0.0347(16) 0.0133(13) 0.0083(14) -0.0040(13) O7 0.0177(13) 0.0345(15) 0.0235(14) 0.0082(12) 0.0081(11) 0.0069(11) O8 0.0200(13) 0.0209(13) 0.0280(14) 0.0075(11) 0.0120(11) 0.0063(10) O9 0.052(2) 0.070(2) 0.0258(16) 0.0134(16) 0.0161(15) 0.0285(19) O1W 0.0258(15) 0.0356(16) 0.0364(16) 0.0083(13) 0.0044(13) 0.0116(13) O2W 0.056(2) 0.0397(18) 0.0439(18) 0.0244(15) 0.0291(17) 0.0204(16) O3W 0.099(4) 0.092(4) 0.068(3) 0.015(3) 0.040(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O8 2.354(2) . ? Gd1 O5 2.388(2) . ? Gd1 O4 2.395(2) 2_666 ? Gd1 O7 2.424(2) 2_666 ? Gd1 O1 2.425(2) . ? Gd1 O2 2.465(3) . ? Gd1 O1W 2.475(3) . ? Gd1 O2W 2.509(3) . ? Gd1 O8 2.699(3) 2_666 ? Gd1 H1WB 2.5686 . ? C1 O2 1.252(4) . ? C1 O1 1.258(4) . ? C1 C2 1.503(5) . ? C2 C3 1.396(5) 2_777 ? C2 C4 1.400(5) . ? C3 C4 1.386(5) . ? C3 C2 1.396(5) 2_777 ? C3 H3 0.9300 . ? C4 C5 1.512(5) . ? C5 O3 1.213(5) . ? C5 C6 1.487(6) . ? C6 C7 1.384(6) . ? C6 C11 1.391(6) . ? C7 C8 1.395(6) . ? C7 H7 0.9300 . ? C8 C9 1.373(8) . ? C8 H8 0.9300 . ? C9 C10 1.366(8) . ? C9 H9 0.9300 . ? C10 C11 1.400(7) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O5 1.253(4) . ? C12 O4 1.261(4) . ? C12 C13 1.515(5) . ? C13 C14 1.394(5) . ? C13 C15 1.395(5) . ? C14 C15 1.395(5) 2_676 ? C14 H14 0.9300 . ? C15 C14 1.395(5) 2_676 ? C15 C16 1.515(5) . ? C16 O6 1.211(5) . ? C16 C17 1.482(5) . ? C17 C22 1.388(6) . ? C17 C18 1.389(6) . ? C18 C19 1.376(6) . ? C18 H18 0.9300 . ? C19 C20 1.382(8) . ? C19 H19 0.9300 . ? C20 C21 1.379(8) . ? C20 H20 0.9300 . ? C21 C22 1.374(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O7 1.243(4) . ? C23 O8 1.276(4) . ? C23 C24 1.488(5) . ? C23 Gd1 2.924(4) 2_666 ? C24 C25 1.390(5) . ? C24 C26 1.402(5) . ? C25 C26 1.381(5) 2_766 ? C25 H25 0.9300 . ? C26 C25 1.381(5) 2_766 ? C26 C27 1.505(5) . ? C27 O9 1.207(5) . ? C27 C28 1.481(6) . ? C28 C29 1.371(7) . ? C28 C33 1.393(6) . ? C29 C30 1.400(8) . ? C29 H29 0.9300 . ? C30 C31 1.381(8) . ? C30 H30 0.9300 . ? C31 C32 1.325(8) . ? C31 H31 0.9300 . ? C32 C33 1.388(8) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? O4 Gd1 2.395(2) 2_666 ? O7 Gd1 2.424(2) 2_666 ? O8 Gd1 2.699(2) 2_666 ? O1W H1WA 0.8600 . ? O1W H1WB 0.8601 . ? O2W H2WB 0.8499 . ? O2W H2WA 0.8499 . ? O3W H3WA 0.8535 . ? O3W H3WB 0.8549 . ? 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 O8 Gd1 O5 75.94(8) . . ? O8 Gd1 O4 75.15(9) . 2_666 ? O5 Gd1 O4 136.81(8) . 2_666 ? O8 Gd1 O7 125.96(9) . 2_666 ? O5 Gd1 O7 77.16(9) . 2_666 ? O4 Gd1 O7 94.92(9) 2_666 2_666 ? O8 Gd1 O1 138.91(9) . . ? O5 Gd1 O1 80.48(9) . . ? O4 Gd1 O1 140.50(9) 2_666 . ? O7 Gd1 O1 79.44(9) 2_666 . ? O8 Gd1 O2 87.77(9) . . ? O5 Gd1 O2 74.09(9) . . ? O4 Gd1 O2 135.32(9) 2_666 . ? O7 Gd1 O2 127.53(9) 2_666 . ? O1 Gd1 O2 53.29(9) . . ? O8 Gd1 O1W 93.67(9) . . ? O5 Gd1 O1W 139.11(10) . . ? O4 Gd1 O1W 74.16(9) 2_666 . ? O7 Gd1 O1W 135.26(9) 2_666 . ? O1 Gd1 O1W 82.66(10) . . ? O2 Gd1 O1W 65.97(10) . . ? O8 Gd1 O2W 142.17(9) . . ? O5 Gd1 O2W 140.16(9) . . ? O4 Gd1 O2W 68.81(9) 2_666 . ? O7 Gd1 O2W 69.49(9) 2_666 . ? O1 Gd1 O2W 72.69(10) . . ? O2 Gd1 O2W 109.89(10) . . ? O1W Gd1 O2W 66.09(10) . . ? O8 Gd1 O8 76.25(9) . 2_666 ? O5 Gd1 O8 68.97(8) . 2_666 ? O4 Gd1 O8 73.44(8) 2_666 2_666 ? O7 Gd1 O8 50.44(8) 2_666 2_666 ? O1 Gd1 O8 125.05(8) . 2_666 ? O2 Gd1 O8 142.26(9) . 2_666 ? O1W Gd1 O8 147.54(9) . 2_666 ? O2W Gd1 O8 103.35(9) . 2_666 ? O8 Gd1 C23 101.49(9) . 2_666 ? O5 Gd1 C23 70.08(9) . 2_666 ? O4 Gd1 C23 85.10(9) 2_666 2_666 ? O7 Gd1 C23 24.68(9) 2_666 2_666 ? O1 Gd1 C23 101.42(9) . 2_666 ? O2 Gd1 C23 139.27(9) . 2_666 ? O1W Gd1 C23 150.25(10) . 2_666 ? O2W Gd1 C23 86.78(10) . 2_666 ? O8 Gd1 C23 25.83(8) 2_666 2_666 ? O8 Gd1 Gd1 41.19(6) . 2_666 ? O5 Gd1 Gd1 67.24(6) . 2_666 ? O4 Gd1 Gd1 69.83(6) 2_666 2_666 ? O7 Gd1 Gd1 85.15(6) 2_666 2_666 ? O1 Gd1 Gd1 146.62(7) . 2_666 ? O2 Gd1 Gd1 120.87(6) . 2_666 ? O1W Gd1 Gd1 127.58(7) . 2_666 ? O2W Gd1 Gd1 128.59(8) . 2_666 ? O8 Gd1 Gd1 35.06(5) 2_666 2_666 ? C23 Gd1 Gd1 60.49(7) 2_666 2_666 ? O8 Gd1 H1WB 85.6 . . ? O5 Gd1 H1WB 151.2 . . ? O4 Gd1 H1WB 54.8 2_666 . ? O7 Gd1 H1WB 131.6 2_666 . ? O1 Gd1 H1WB 100.4 . . ? O2 Gd1 H1WB 83.4 . . ? O1W Gd1 H1WB 19.5 . . ? O2W Gd1 H1WB 64.6 . . ? O8 Gd1 H1WB 128.1 2_666 . ? C23 Gd1 H1WB 136.4 2_666 . ? Gd1 Gd1 H1WB 111.9 2_666 . ? O2 C1 O1 121.8(3) . . ? O2 C1 C2 119.0(3) . . ? O1 C1 C2 119.3(3) . . ? C3 C2 C4 119.4(3) 2_777 . ? C3 C2 C1 119.1(3) 2_777 . ? C4 C2 C1 121.4(3) . . ? C4 C3 C2 121.8(4) . 2_777 ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 2_777 . ? C3 C4 C2 118.8(3) . . ? C3 C4 C5 119.5(3) . . ? C2 C4 C5 121.6(3) . . ? O3 C5 C6 120.9(4) . . ? O3 C5 C4 119.9(4) . . ? C6 C5 C4 119.1(3) . . ? C7 C6 C11 119.1(4) . . ? C7 C6 C5 122.7(4) . . ? C11 C6 C5 118.1(4) . . ? C6 C7 C8 120.6(5) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C7 119.7(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 120.4(6) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.5(5) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C6 C11 C10 119.6(5) . . ? C6 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? O5 C12 O4 125.9(3) . . ? O5 C12 C13 117.0(3) . . ? O4 C12 C13 117.1(3) . . ? C14 C13 C15 118.4(3) . . ? C14 C13 C12 118.3(3) . . ? C15 C13 C12 123.2(3) . . ? C13 C14 C15 121.3(3) . 2_676 ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 2_676 . ? C14 C15 C13 120.3(3) 2_676 . ? C14 C15 C16 118.2(3) 2_676 . ? C13 C15 C16 121.4(3) . . ? O6 C16 C17 122.1(3) . . ? O6 C16 C15 119.4(3) . . ? C17 C16 C15 118.5(3) . . ? C22 C17 C18 118.7(4) . . ? C22 C17 C16 121.8(4) . . ? C18 C17 C16 119.5(4) . . ? C19 C18 C17 120.8(5) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 119.7(5) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 120.0(5) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.3(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C17 120.5(5) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? O7 C23 O8 121.5(3) . . ? O7 C23 C24 119.5(3) . . ? O8 C23 C24 119.0(3) . . ? O7 C23 Gd1 54.52(18) . 2_666 ? O8 C23 Gd1 67.18(19) . 2_666 ? C24 C23 Gd1 171.1(2) . 2_666 ? C25 C24 C26 118.8(3) . . ? C25 C24 C23 118.7(3) . . ? C26 C24 C23 122.3(3) . . ? C26 C25 C24 122.2(3) 2_766 . ? C26 C25 H25 118.9 2_766 . ? C24 C25 H25 118.9 . . ? C25 C26 C24 118.9(3) 2_766 . ? C25 C26 C27 116.8(3) 2_766 . ? C24 C26 C27 124.3(3) . . ? O9 C27 C28 121.4(4) . . ? O9 C27 C26 118.5(4) . . ? C28 C27 C26 120.0(3) . . ? C29 C28 C33 119.4(5) . . ? C29 C28 C27 122.2(4) . . ? C33 C28 C27 118.4(5) . . ? C28 C29 C30 121.3(5) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C31 C30 C29 116.8(6) . . ? C31 C30 H30 121.6 . . ? C29 C30 H30 121.6 . . ? C32 C31 C30 123.1(6) . . ? C32 C31 H31 118.4 . . ? C30 C31 H31 118.4 . . ? C31 C32 C33 120.3(6) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C32 C33 C28 119.1(6) . . ? C32 C33 H33 120.5 . . ? C28 C33 H33 120.5 . . ? C1 O1 Gd1 93.3(2) . . ? C1 O2 Gd1 91.6(2) . . ? C12 O4 Gd1 135.7(2) . 2_666 ? C12 O5 Gd1 140.5(2) . . ? C23 O7 Gd1 100.8(2) . 2_666 ? C23 O8 Gd1 163.6(2) . . ? C23 O8 Gd1 87.0(2) . 2_666 ? Gd1 O8 Gd1 103.75(9) . 2_666 ? Gd1 O1W H1WA 143.8 . . ? Gd1 O1W H1WB 86.4 . . ? H1WA O1W H1WB 105.6 . . ? Gd1 O2W H2WB 124.0 . . ? Gd1 O2W H2WA 131.7 . . ? H2WB O2W H2WA 104.1 . . ? H3WA O3W H3WB 106.8 . . ? 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 O2 C1 C2 C3 -160.7(4) . . . 2_777 ? O1 C1 C2 C3 17.8(5) . . . 2_777 ? O2 C1 C2 C4 15.5(5) . . . . ? O1 C1 C2 C4 -166.0(4) . . . . ? C2 C3 C4 C2 0.8(6) 2_777 . . . ? C2 C3 C4 C5 176.3(3) 2_777 . . . ? C3 C2 C4 C3 -0.8(6) 2_777 . . . ? C1 C2 C4 C3 -177.0(3) . . . . ? C3 C2 C4 C5 -176.2(3) 2_777 . . . ? C1 C2 C4 C5 7.6(6) . . . . ? C3 C4 C5 O3 -99.5(5) . . . . ? C2 C4 C5 O3 75.9(5) . . . . ? C3 C4 C5 C6 76.7(5) . . . . ? C2 C4 C5 C6 -108.0(4) . . . . ? O3 C5 C6 C7 155.8(4) . . . . ? C4 C5 C6 C7 -20.3(6) . . . . ? O3 C5 C6 C11 -20.6(6) . . . . ? C4 C5 C6 C11 163.3(4) . . . . ? C11 C6 C7 C8 2.9(7) . . . . ? C5 C6 C7 C8 -173.4(4) . . . . ? C6 C7 C8 C9 -3.0(8) . . . . ? C7 C8 C9 C10 0.9(9) . . . . ? C8 C9 C10 C11 1.3(9) . . . . ? C7 C6 C11 C10 -0.7(7) . . . . ? C5 C6 C11 C10 175.8(4) . . . . ? C9 C10 C11 C6 -1.4(8) . . . . ? O5 C12 C13 C14 34.9(5) . . . . ? O4 C12 C13 C14 -143.9(3) . . . . ? O5 C12 C13 C15 -148.6(3) . . . . ? O4 C12 C13 C15 32.6(5) . . . . ? C15 C13 C14 C15 -1.1(6) . . . 2_676 ? C12 C13 C14 C15 175.5(3) . . . 2_676 ? C14 C13 C15 C14 1.1(6) . . . 2_676 ? C12 C13 C15 C14 -175.4(3) . . . 2_676 ? C14 C13 C15 C16 -174.0(3) . . . . ? C12 C13 C15 C16 9.5(5) . . . . ? C14 C15 C16 O6 -113.5(4) 2_676 . . . ? C13 C15 C16 O6 61.7(5) . . . . ? C14 C15 C16 C17 66.1(4) 2_676 . . . ? C13 C15 C16 C17 -118.7(4) . . . . ? O6 C16 C17 C22 -165.9(4) . . . . ? C15 C16 C17 C22 14.4(5) . . . . ? O6 C16 C17 C18 11.4(6) . . . . ? C15 C16 C17 C18 -168.3(3) . . . . ? C22 C17 C18 C19 1.2(6) . . . . ? C16 C17 C18 C19 -176.2(4) . . . . ? C17 C18 C19 C20 -0.5(7) . . . . ? C18 C19 C20 C21 0.3(8) . . . . ? C19 C20 C21 C22 -0.8(9) . . . . ? C20 C21 C22 C17 1.5(8) . . . . ? C18 C17 C22 C21 -1.7(7) . . . . ? C16 C17 C22 C21 175.7(4) . . . . ? O7 C23 C24 C25 -144.7(4) . . . . ? O8 C23 C24 C25 33.5(5) . . . . ? O7 C23 C24 C26 30.3(5) . . . . ? O8 C23 C24 C26 -151.5(3) . . . . ? C26 C24 C25 C26 0.2(6) . . . 2_766 ? C23 C24 C25 C26 175.4(3) . . . 2_766 ? C25 C24 C26 C25 -0.2(6) . . . 2_766 ? C23 C24 C26 C25 -175.2(3) . . . 2_766 ? C25 C24 C26 C27 -179.8(4) . . . . ? C23 C24 C26 C27 5.2(6) . . . . ? C25 C26 C27 O9 51.8(5) 2_766 . . . ? C24 C26 C27 O9 -128.6(4) . . . . ? C25 C26 C27 C28 -123.3(4) 2_766 . . . ? C24 C26 C27 C28 56.2(5) . . . . ? O9 C27 C28 C29 -165.5(5) . . . . ? C26 C27 C28 C29 9.5(6) . . . . ? O9 C27 C28 C33 12.2(6) . . . . ? C26 C27 C28 C33 -172.8(4) . . . . ? C33 C28 C29 C30 0.7(8) . . . . ? C27 C28 C29 C30 178.4(5) . . . . ? C28 C29 C30 C31 0.6(9) . . . . ? C29 C30 C31 C32 -1.0(10) . . . . ? C30 C31 C32 C33 0.1(10) . . . . ? C31 C32 C33 C28 1.2(8) . . . . ? C29 C28 C33 C32 -1.7(7) . . . . ? C27 C28 C33 C32 -179.4(4) . . . . ? O2 C1 O1 Gd1 3.6(4) . . . . ? C2 C1 O1 Gd1 -174.8(3) . . . . ? O8 Gd1 O1 C1 -23.7(3) . . . . ? O5 Gd1 O1 C1 -79.1(2) . . . . ? O4 Gd1 O1 C1 117.4(2) 2_666 . . . ? O7 Gd1 O1 C1 -157.7(2) 2_666 . . . ? O2 Gd1 O1 C1 -1.9(2) . . . . ? O1W Gd1 O1 C1 63.5(2) . . . . ? O2W Gd1 O1 C1 130.6(2) . . . . ? O8 Gd1 O1 C1 -134.9(2) 2_666 . . . ? C23 Gd1 O1 C1 -146.4(2) 2_666 . . . ? Gd1 Gd1 O1 C1 -93.8(2) 2_666 . . . ? O1 C1 O2 Gd1 -3.5(4) . . . . ? C2 C1 O2 Gd1 174.9(3) . . . . ? O8 Gd1 O2 C1 167.8(2) . . . . ? O5 Gd1 O2 C1 91.8(2) . . . . ? O4 Gd1 O2 C1 -126.0(2) 2_666 . . . ? O7 Gd1 O2 C1 32.5(3) 2_666 . . . ? O1 Gd1 O2 C1 2.0(2) . . . . ? O1W Gd1 O2 C1 -97.1(2) . . . . ? O2W Gd1 O2 C1 -46.4(2) . . . . ? O8 Gd1 O2 C1 103.9(2) 2_666 . . . ? C23 Gd1 O2 C1 62.8(3) 2_666 . . . ? Gd1 Gd1 O2 C1 142.1(2) 2_666 . . . ? O5 C12 O4 Gd1 2.3(6) . . . 2_666 ? C13 C12 O4 Gd1 -179.1(2) . . . 2_666 ? O4 C12 O5 Gd1 10.1(6) . . . . ? C13 C12 O5 Gd1 -168.6(2) . . . . ? O8 Gd1 O5 C12 32.3(4) . . . . ? O4 Gd1 O5 C12 -17.0(4) 2_666 . . . ? O7 Gd1 O5 C12 -100.4(4) 2_666 . . . ? O1 Gd1 O5 C12 178.4(4) . . . . ? O2 Gd1 O5 C12 124.0(4) . . . . ? O1W Gd1 O5 C12 111.4(4) . . . . ? O2W Gd1 O5 C12 -133.9(4) . . . . ? O8 Gd1 O5 C12 -48.1(4) 2_666 . . . ? C23 Gd1 O5 C12 -75.7(4) 2_666 . . . ? Gd1 Gd1 O5 C12 -10.3(3) 2_666 . . . ? O8 C23 O7 Gd1 -6.0(4) . . . 2_666 ? C24 C23 O7 Gd1 172.2(3) . . . 2_666 ? O7 C23 O8 Gd1 137.0(7) . . . . ? C24 C23 O8 Gd1 -41.2(10) . . . . ? Gd1 C23 O8 Gd1 131.7(8) 2_666 . . . ? O7 C23 O8 Gd1 5.3(3) . . . 2_666 ? C24 C23 O8 Gd1 -172.9(3) . . . 2_666 ? O5 Gd1 O8 C23 158.7(8) . . . . ? O4 Gd1 O8 C23 -53.7(8) 2_666 . . . ? O7 Gd1 O8 C23 -138.9(8) 2_666 . . . ? O1 Gd1 O8 C23 101.9(8) . . . . ? O2 Gd1 O8 C23 84.6(8) . . . . ? O1W Gd1 O8 C23 18.8(8) . . . . ? O2W Gd1 O8 C23 -35.7(9) . . . . ? O8 Gd1 O8 C23 -129.9(9) 2_666 . . . ? C23 Gd1 O8 C23 -135.4(8) 2_666 . . . ? Gd1 Gd1 O8 C23 -129.9(9) 2_666 . . . ? O5 Gd1 O8 Gd1 -71.36(9) . . . 2_666 ? O4 Gd1 O8 Gd1 76.20(9) 2_666 . . 2_666 ? O7 Gd1 O8 Gd1 -9.06(13) 2_666 . . 2_666 ? O1 Gd1 O8 Gd1 -128.23(12) . . . 2_666 ? O2 Gd1 O8 Gd1 -145.52(10) . . . 2_666 ? O1W Gd1 O8 Gd1 148.74(10) . . . 2_666 ? O2W Gd1 O8 Gd1 94.16(16) . . . 2_666 ? O8 Gd1 O8 Gd1 0.0 2_666 . . 2_666 ? C23 Gd1 O8 Gd1 -5.53(10) 2_666 . . 2_666 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.212 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 890970' ####################################################################### # # 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_10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C34 H21 N2 O7 Tb' _chemical_formula_sum 'C34 H21 N2 O7 Tb' _chemical_formula_weight 728.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9617(6) _cell_length_b 12.6849(5) _cell_length_c 19.6998(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.951(3) _cell_angle_gamma 90.00 _cell_volume 2843.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6463 _cell_measurement_theta_min 2.1735 _cell_measurement_theta_max 27.5010 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2500 _exptl_crystal_size_mid 0.2100 _exptl_crystal_size_min 0.1800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 2.542 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21744 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6508 _reflns_number_gt 5765 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+9.0570P] 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 6508 _refine_ls_number_parameters 397 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.076 _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 Tb1 Tb 0.507269(19) 0.602042(16) 0.568362(11) 0.02582(9) Uani 1 1 d . . . C1 C 0.6323(5) 0.5057(4) 0.6965(3) 0.0335(10) Uani 1 1 d . . . C2 C 0.6964(4) 0.4543(4) 0.7660(3) 0.0324(10) Uani 1 1 d . . . C3 C 0.6434(5) 0.3690(4) 0.7882(3) 0.0344(10) Uani 1 1 d . . . H3 H 0.5682 0.3487 0.7610 0.041 Uiso 1 1 calc R . . C4 C 0.8073(4) 0.4876(4) 0.8086(3) 0.0347(10) Uani 1 1 d . . . C5 C 0.8723(5) 0.5847(5) 0.7946(3) 0.0409(12) Uani 1 1 d . . . C6 C 0.8200(5) 0.6909(5) 0.7989(3) 0.0455(13) Uani 1 1 d . . . C7 C 0.7233(6) 0.7042(5) 0.8225(3) 0.0529(15) Uani 1 1 d . . . H7 H 0.6881 0.6458 0.8360 0.063 Uiso 1 1 calc R . . C8 C 0.6783(7) 0.8047(6) 0.8262(4) 0.070(2) Uani 1 1 d . . . H8 H 0.6138 0.8134 0.8426 0.083 Uiso 1 1 calc R . . C9 C 0.7285(8) 0.8895(7) 0.8058(5) 0.074(2) Uani 1 1 d U . . H9 H 0.6967 0.9561 0.8072 0.089 Uiso 1 1 calc R . . C10 C 0.8242(8) 0.8793(7) 0.7834(5) 0.070(2) Uani 1 1 d U . . H10 H 0.8581 0.9390 0.7704 0.084 Uiso 1 1 calc R . . C11 C 0.8733(7) 0.7784(5) 0.7794(3) 0.0592(18) Uani 1 1 d . . . H11 H 0.9392 0.7711 0.7642 0.071 Uiso 1 1 calc R . . C12 C 0.6332(5) 0.2293(4) 0.8744(3) 0.0345(10) Uani 1 1 d . . . C13 C 0.7002(5) 0.3138(4) 0.8498(3) 0.0338(10) Uani 1 1 d . . . C14 C 0.8131(5) 0.3434(4) 0.8905(3) 0.0355(11) Uani 1 1 d . . . C15 C 0.8649(5) 0.4313(5) 0.8702(3) 0.0387(11) Uani 1 1 d . . . H15 H 0.9391 0.4529 0.8983 0.046 Uiso 1 1 calc R . . C16 C 0.8839(5) 0.2901(5) 0.9587(3) 0.0398(12) Uani 1 1 d . . . C17 C 0.9625(5) 0.2028(4) 0.9527(3) 0.0363(11) Uani 1 1 d . . . C18 C 1.0428(5) 0.1625(5) 1.0146(3) 0.0469(13) Uani 1 1 d . . . H18 H 1.0473 0.1907 1.0589 0.056 Uiso 1 1 calc R . . C19 C 1.1157(6) 0.0803(6) 1.0095(5) 0.067(2) Uani 1 1 d . . . H19 H 1.1688 0.0527 1.0505 0.080 Uiso 1 1 calc R . . C20 C 1.1100(7) 0.0399(6) 0.9447(4) 0.0648(18) Uani 1 1 d U . . H20 H 1.1585 -0.0162 0.9420 0.078 Uiso 1 1 calc R . . C21 C 1.0333(6) 0.0807(6) 0.8827(4) 0.0599(18) Uani 1 1 d . . . H21 H 1.0321 0.0537 0.8386 0.072 Uiso 1 1 calc R . . C22 C 0.9590(5) 0.1612(5) 0.8866(3) 0.0466(13) Uani 1 1 d . . . H22 H 0.9063 0.1881 0.8451 0.056 Uiso 1 1 calc R . . C23 C 0.3091(6) 0.7052(6) 0.4153(4) 0.0626(18) Uani 1 1 d . . . H23 H 0.2685 0.6453 0.4216 0.075 Uiso 1 1 calc R . . C24 C 0.2547(7) 0.7731(8) 0.3584(4) 0.079(2) Uani 1 1 d . . . H24 H 0.1798 0.7584 0.3279 0.095 Uiso 1 1 calc R . . C25 C 0.3134(7) 0.8601(7) 0.3489(4) 0.072(2) Uani 1 1 d . . . H25 H 0.2787 0.9062 0.3116 0.087 Uiso 1 1 calc R . . C26 C 0.4251(7) 0.8810(5) 0.3945(4) 0.0566(17) Uani 1 1 d . . . C27 C 0.4751(5) 0.8088(4) 0.4491(3) 0.0403(12) Uani 1 1 d . . . C28 C 0.5884(5) 0.8278(4) 0.4994(3) 0.0395(12) Uani 1 1 d . . . C29 C 0.6502(6) 0.9206(5) 0.4924(4) 0.0534(16) Uani 1 1 d . . . C30 C 0.5962(7) 0.9925(7) 0.4364(4) 0.070(2) Uani 1 1 d U . . H30 H 0.6360 1.0539 0.4321 0.084 Uiso 1 1 calc R . . C31 C 0.4916(7) 0.9749(7) 0.3904(4) 0.069(2) Uani 1 1 d U . . H31 H 0.4598 1.0239 0.3546 0.083 Uiso 1 1 calc R . . C32 C 0.7607(7) 0.9363(5) 0.5423(4) 0.0637(19) Uani 1 1 d . . . H32 H 0.8037 0.9964 0.5396 0.076 Uiso 1 1 calc R . . C33 C 0.8056(6) 0.8648(6) 0.5945(4) 0.0599(17) Uani 1 1 d . . . H33 H 0.8794 0.8749 0.6275 0.072 Uiso 1 1 calc R . . C34 C 0.7390(6) 0.7751(5) 0.5982(3) 0.0488(14) Uani 1 1 d . . . H34 H 0.7701 0.7264 0.6344 0.059 Uiso 1 1 calc R . . N1 N 0.4146(4) 0.7222(4) 0.4603(2) 0.0427(11) Uani 1 1 d . . . N2 N 0.6339(4) 0.7570(3) 0.5524(2) 0.0377(9) Uani 1 1 d . . . O1 O 0.5251(3) 0.4862(3) 0.6682(2) 0.0489(10) Uani 1 1 d . . . O2 O 0.6880(3) 0.5656(3) 0.66712(19) 0.0396(8) Uani 1 1 d . . . O3 O 0.9675(4) 0.5727(4) 0.7860(3) 0.0599(12) Uani 1 1 d . . . O4 O 0.6858(3) 0.1590(3) 0.9174(2) 0.0431(9) Uani 1 1 d . . . O5 O 0.5225(4) 0.2360(3) 0.8530(2) 0.0519(11) Uani 1 1 d . . . O6 O 0.8815(5) 0.3247(4) 1.0160(2) 0.0656(14) Uani 1 1 d . . . O7 O 0.6036(3) 0.5270(3) 0.49783(19) 0.0345(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.03186(14) 0.02198(14) 0.02244(13) -0.00066(7) 0.00667(9) -0.00388(8) C1 0.042(3) 0.029(2) 0.028(2) 0.0033(19) 0.008(2) -0.003(2) C2 0.036(2) 0.032(2) 0.028(2) 0.0015(19) 0.0084(19) 0.002(2) C3 0.040(3) 0.034(2) 0.029(2) 0.003(2) 0.009(2) 0.001(2) C4 0.035(2) 0.036(3) 0.033(2) 0.002(2) 0.010(2) 0.005(2) C5 0.039(3) 0.048(3) 0.033(3) 0.006(2) 0.006(2) -0.006(2) C6 0.053(3) 0.038(3) 0.034(3) 0.003(2) -0.003(2) -0.008(3) C7 0.053(3) 0.045(3) 0.053(4) -0.005(3) 0.006(3) 0.001(3) C8 0.076(5) 0.055(4) 0.067(5) -0.009(4) 0.006(4) 0.009(4) C9 0.075(2) 0.073(2) 0.074(2) -0.0007(10) 0.0211(12) 0.0007(10) C10 0.071(2) 0.068(2) 0.070(2) 0.0011(10) 0.0194(11) -0.0018(10) C11 0.069(4) 0.050(4) 0.047(3) 0.003(3) 0.000(3) -0.019(3) C12 0.044(3) 0.031(2) 0.030(2) 0.0046(19) 0.013(2) 0.001(2) C13 0.041(3) 0.030(2) 0.032(2) 0.004(2) 0.013(2) 0.005(2) C14 0.039(3) 0.038(3) 0.032(2) 0.007(2) 0.014(2) 0.011(2) C15 0.032(3) 0.045(3) 0.035(3) 0.006(2) 0.005(2) 0.005(2) C16 0.047(3) 0.041(3) 0.031(2) 0.003(2) 0.011(2) 0.008(2) C17 0.038(3) 0.038(3) 0.034(2) 0.003(2) 0.013(2) 0.006(2) C18 0.041(3) 0.054(4) 0.041(3) 0.002(3) 0.005(2) 0.011(3) C19 0.045(4) 0.071(5) 0.073(5) 0.002(4) 0.000(3) 0.024(3) C20 0.064(2) 0.064(2) 0.066(2) -0.0017(10) 0.0198(11) 0.0021(10) C21 0.056(4) 0.065(4) 0.065(4) -0.024(4) 0.028(3) -0.003(3) C22 0.045(3) 0.053(3) 0.042(3) -0.005(3) 0.013(2) 0.001(3) C23 0.057(4) 0.062(4) 0.056(4) 0.015(3) -0.001(3) -0.009(3) C24 0.060(4) 0.096(6) 0.061(5) 0.022(4) -0.011(4) 0.000(4) C25 0.075(5) 0.078(5) 0.057(4) 0.038(4) 0.011(4) 0.015(4) C26 0.074(5) 0.048(4) 0.053(4) 0.019(3) 0.028(4) 0.010(3) C27 0.050(3) 0.022(2) 0.048(3) 0.012(2) 0.014(2) 0.005(2) C28 0.049(3) 0.030(3) 0.045(3) 0.005(2) 0.023(2) -0.002(2) C29 0.066(4) 0.035(3) 0.072(4) 0.009(3) 0.040(4) -0.007(3) C30 0.071(2) 0.069(2) 0.071(2) 0.0026(10) 0.0230(11) -0.0013(10) C31 0.070(2) 0.069(2) 0.069(2) 0.0029(10) 0.0224(11) 0.0001(10) C32 0.070(5) 0.042(3) 0.092(5) 0.001(4) 0.044(4) -0.022(3) C33 0.053(4) 0.055(4) 0.073(5) -0.001(4) 0.021(3) -0.023(3) C34 0.053(3) 0.041(3) 0.051(3) 0.000(3) 0.013(3) -0.015(3) N1 0.042(2) 0.042(3) 0.040(2) 0.010(2) 0.006(2) -0.003(2) N2 0.045(2) 0.032(2) 0.037(2) 0.0000(18) 0.0136(19) -0.0069(18) O1 0.040(2) 0.058(3) 0.040(2) 0.0197(19) 0.0000(17) -0.0131(18) O2 0.041(2) 0.042(2) 0.0338(18) 0.0111(16) 0.0087(16) -0.0074(16) O3 0.044(2) 0.072(3) 0.068(3) 0.011(3) 0.024(2) -0.004(2) O4 0.047(2) 0.039(2) 0.045(2) 0.0185(17) 0.0159(18) 0.0085(17) O5 0.042(2) 0.052(2) 0.060(3) 0.030(2) 0.0122(19) 0.0035(18) O6 0.094(4) 0.067(3) 0.035(2) 0.001(2) 0.020(2) 0.039(3) O7 0.0328(17) 0.0340(18) 0.0380(18) -0.0120(15) 0.0127(15) -0.0102(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 Tb1 O7 2.252(3) 3_666 ? Tb1 O7 2.270(3) . ? Tb1 O5 2.400(4) 2_656 ? Tb1 O1 2.411(4) . ? Tb1 O2 2.465(4) . ? Tb1 O4 2.517(4) 2_656 ? Tb1 N2 2.560(4) . ? Tb1 N1 2.574(4) . ? C1 O1 1.255(6) . ? C1 O2 1.263(6) . ? C1 C2 1.496(7) . ? C2 C3 1.391(7) . ? C2 C4 1.398(7) . ? C3 C13 1.385(7) . ? C3 H3 0.9300 . ? C4 C15 1.395(7) . ? C4 C5 1.527(7) . ? C5 O3 1.212(7) . ? C5 C6 1.498(8) . ? C6 C7 1.384(9) . ? C6 C11 1.392(9) . ? C7 C8 1.395(10) . ? C7 H7 0.9300 . ? C8 C9 1.352(12) . ? C8 H8 0.9300 . ? C9 C10 1.354(12) . ? C9 H9 0.9300 . ? C10 C11 1.420(11) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O4 1.256(6) . ? C12 O5 1.262(7) . ? C12 C13 1.506(7) . ? C12 Tb1 2.804(5) 2_646 ? C13 C14 1.394(8) . ? C14 C15 1.393(8) . ? C14 C16 1.509(7) . ? C15 H15 0.9300 . ? C16 O6 1.220(7) . ? C16 C17 1.480(7) . ? C17 C22 1.395(8) . ? C17 C18 1.396(8) . ? C18 C19 1.382(9) . ? C18 H18 0.9300 . ? C19 C20 1.357(11) . ? C19 H19 0.9300 . ? C20 C21 1.382(11) . ? C20 H20 0.9300 . ? C21 C22 1.371(9) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 N1 1.318(8) . ? C23 C24 1.405(10) . ? C23 H23 0.9300 . ? C24 C25 1.352(12) . ? C24 H24 0.9300 . ? C25 C26 1.387(11) . ? C25 H25 0.9300 . ? C26 C27 1.400(8) . ? C26 C31 1.448(11) . ? C27 N1 1.370(7) . ? C27 C28 1.432(8) . ? C28 N2 1.357(7) . ? C28 C29 1.419(8) . ? C29 C32 1.398(11) . ? C29 C30 1.424(10) . ? C30 C31 1.317(11) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.353(11) . ? C32 H32 0.9300 . ? C33 C34 1.404(8) . ? C33 H33 0.9300 . ? C34 N2 1.323(8) . ? C34 H34 0.9300 . ? O4 Tb1 2.517(4) 2_646 ? O5 Tb1 2.400(4) 2_646 ? O7 Tb1 2.252(3) 3_666 ? 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 O7 Tb1 O7 70.13(14) 3_666 . ? O7 Tb1 O5 135.28(13) 3_666 2_656 ? O7 Tb1 O5 153.76(13) . 2_656 ? O7 Tb1 O1 85.26(14) 3_666 . ? O7 Tb1 O1 108.03(15) . . ? O5 Tb1 O1 84.17(17) 2_656 . ? O7 Tb1 O2 122.51(13) 3_666 . ? O7 Tb1 O2 85.26(13) . . ? O5 Tb1 O2 83.78(14) 2_656 . ? O1 Tb1 O2 53.60(12) . . ? O7 Tb1 O4 82.91(12) 3_666 2_656 ? O7 Tb1 O4 147.70(12) . 2_656 ? O5 Tb1 O4 53.15(13) 2_656 2_656 ? O1 Tb1 O4 86.42(14) . 2_656 ? O2 Tb1 O4 125.24(13) . 2_656 ? O7 Tb1 N2 138.76(13) 3_666 . ? O7 Tb1 N2 79.36(13) . . ? O5 Tb1 N2 75.35(15) 2_656 . ? O1 Tb1 N2 131.42(14) . . ? O2 Tb1 N2 80.37(13) . . ? O4 Tb1 N2 113.05(14) 2_656 . ? O7 Tb1 N1 85.69(15) 3_666 . ? O7 Tb1 N1 84.99(15) . . ? O5 Tb1 N1 90.17(16) 2_656 . ? O1 Tb1 N1 160.47(15) . . ? O2 Tb1 N1 144.36(14) . . ? O4 Tb1 N1 75.31(15) 2_656 . ? N2 Tb1 N1 64.15(15) . . ? O7 Tb1 C1 105.15(14) 3_666 . ? O7 Tb1 C1 97.96(14) . . ? O5 Tb1 C1 82.58(16) 2_656 . ? O1 Tb1 C1 26.70(13) . . ? O2 Tb1 C1 26.92(13) . . ? O4 Tb1 C1 106.22(14) 2_656 . ? N2 Tb1 C1 105.99(15) . . ? N1 Tb1 C1 169.14(15) . . ? O7 Tb1 C12 109.40(14) 3_666 2_656 ? O7 Tb1 C12 165.35(14) . 2_656 ? O5 Tb1 C12 26.64(14) 2_656 2_656 ? O1 Tb1 C12 86.35(16) . 2_656 ? O2 Tb1 C12 106.18(14) . 2_656 ? O4 Tb1 C12 26.61(13) 2_656 2_656 ? N2 Tb1 C12 93.34(15) . 2_656 ? N1 Tb1 C12 80.40(15) . 2_656 ? C1 Tb1 C12 96.25(15) . 2_656 ? O7 Tb1 Tb1 35.22(9) 3_666 3_666 ? O7 Tb1 Tb1 34.91(8) . 3_666 ? O5 Tb1 Tb1 169.25(10) 2_656 3_666 ? O1 Tb1 Tb1 98.02(11) . 3_666 ? O2 Tb1 Tb1 106.04(10) . 3_666 ? O4 Tb1 Tb1 116.32(8) 2_656 3_666 ? N2 Tb1 Tb1 110.14(10) . 3_666 ? N1 Tb1 Tb1 84.30(11) . 3_666 ? C1 Tb1 Tb1 104.12(10) . 3_666 ? C12 Tb1 Tb1 142.70(11) 2_656 3_666 ? O1 C1 O2 121.7(5) . . ? O1 C1 C2 119.1(4) . . ? O2 C1 C2 119.2(5) . . ? O1 C1 Tb1 59.6(3) . . ? O2 C1 Tb1 62.1(3) . . ? C2 C1 Tb1 178.4(4) . . ? C3 C2 C4 119.1(5) . . ? C3 C2 C1 118.1(4) . . ? C4 C2 C1 122.8(5) . . ? C13 C3 C2 121.4(5) . . ? C13 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C15 C4 C2 119.4(5) . . ? C15 C4 C5 115.3(5) . . ? C2 C4 C5 125.3(5) . . ? O3 C5 C6 123.2(6) . . ? O3 C5 C4 118.4(5) . . ? C6 C5 C4 118.1(5) . . ? C7 C6 C11 119.8(6) . . ? C7 C6 C5 122.4(5) . . ? C11 C6 C5 117.9(6) . . ? C6 C7 C8 120.3(7) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 119.9(8) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 121.2(9) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C11 120.6(8) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C6 C11 C10 118.2(7) . . ? C6 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? O4 C12 O5 122.0(5) . . ? O4 C12 C13 121.1(5) . . ? O5 C12 C13 116.8(4) . . ? O4 C12 Tb1 63.8(3) . 2_646 ? O5 C12 Tb1 58.5(3) . 2_646 ? C13 C12 Tb1 169.6(4) . 2_646 ? C3 C13 C14 119.7(5) . . ? C3 C13 C12 118.5(5) . . ? C14 C13 C12 121.6(4) . . ? C15 C14 C13 119.2(5) . . ? C15 C14 C16 115.9(5) . . ? C13 C14 C16 124.8(5) . . ? C14 C15 C4 121.0(5) . . ? C14 C15 H15 119.5 . . ? C4 C15 H15 119.5 . . ? O6 C16 C17 122.7(5) . . ? O6 C16 C14 119.7(5) . . ? C17 C16 C14 117.4(4) . . ? C22 C17 C18 119.4(5) . . ? C22 C17 C16 121.4(5) . . ? C18 C17 C16 119.2(5) . . ? C19 C18 C17 119.5(6) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 120.3(7) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 121.1(7) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 119.6(7) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C17 120.0(6) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? N1 C23 C24 123.3(7) . . ? N1 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C25 C24 C23 118.6(7) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C25 C26 120.3(7) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 118.1(6) . . ? C25 C26 C31 123.9(7) . . ? C27 C26 C31 118.0(7) . . ? N1 C27 C26 121.8(6) . . ? N1 C27 C28 117.3(5) . . ? C26 C27 C28 120.7(5) . . ? N2 C28 C29 121.7(6) . . ? N2 C28 C27 119.4(5) . . ? C29 C28 C27 118.9(5) . . ? C32 C29 C28 117.3(6) . . ? C32 C29 C30 123.9(6) . . ? C28 C29 C30 118.7(7) . . ? C31 C30 C29 122.1(8) . . ? C31 C30 H30 118.9 . . ? C29 C30 H30 118.9 . . ? C30 C31 C26 121.5(8) . . ? C30 C31 H31 119.2 . . ? C26 C31 H31 119.2 . . ? C33 C32 C29 120.4(6) . . ? C33 C32 H32 119.8 . . ? C29 C32 H32 119.8 . . ? C32 C33 C34 119.0(7) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? N2 C34 C33 122.7(6) . . ? N2 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? C23 N1 C27 117.8(5) . . ? C23 N1 Tb1 122.6(4) . . ? C27 N1 Tb1 119.6(4) . . ? C34 N2 C28 118.8(5) . . ? C34 N2 Tb1 121.5(4) . . ? C28 N2 Tb1 119.4(4) . . ? C1 O1 Tb1 93.7(3) . . ? C1 O2 Tb1 90.9(3) . . ? C12 O4 Tb1 89.6(3) . 2_646 ? C12 O5 Tb1 94.9(3) . 2_646 ? Tb1 O7 Tb1 109.87(14) 3_666 . ? 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 O7 Tb1 C1 O1 -43.2(4) 3_666 . . . ? O7 Tb1 C1 O1 -114.7(3) . . . . ? O5 Tb1 C1 O1 91.8(4) 2_656 . . . ? O2 Tb1 C1 O1 -177.3(5) . . . . ? O4 Tb1 C1 O1 43.7(4) 2_656 . . . ? N2 Tb1 C1 O1 164.2(3) . . . . ? N1 Tb1 C1 O1 140.2(8) . . . . ? C12 Tb1 C1 O1 68.9(4) 2_656 . . . ? Tb1 Tb1 C1 O1 -79.6(3) 3_666 . . . ? O7 Tb1 C1 O2 134.1(3) 3_666 . . . ? O7 Tb1 C1 O2 62.7(3) . . . . ? O5 Tb1 C1 O2 -90.9(3) 2_656 . . . ? O1 Tb1 C1 O2 177.3(5) . . . . ? O4 Tb1 C1 O2 -139.0(3) 2_656 . . . ? N2 Tb1 C1 O2 -18.5(3) . . . . ? N1 Tb1 C1 O2 -42.4(10) . . . . ? C12 Tb1 C1 O2 -113.8(3) 2_656 . . . ? Tb1 Tb1 C1 O2 97.7(3) 3_666 . . . ? O1 C1 C2 C3 14.8(7) . . . . ? O2 C1 C2 C3 -163.6(5) . . . . ? O1 C1 C2 C4 -166.1(5) . . . . ? O2 C1 C2 C4 15.5(8) . . . . ? C4 C2 C3 C13 -2.8(8) . . . . ? C1 C2 C3 C13 176.3(5) . . . . ? C3 C2 C4 C15 3.4(8) . . . . ? C1 C2 C4 C15 -175.7(5) . . . . ? C3 C2 C4 C5 -174.8(5) . . . . ? C1 C2 C4 C5 6.1(8) . . . . ? C15 C4 C5 O3 61.5(7) . . . . ? C2 C4 C5 O3 -120.2(6) . . . . ? C15 C4 C5 C6 -113.0(6) . . . . ? C2 C4 C5 C6 65.2(7) . . . . ? O3 C5 C6 C7 -167.0(6) . . . . ? C4 C5 C6 C7 7.3(8) . . . . ? O3 C5 C6 C11 11.9(9) . . . . ? C4 C5 C6 C11 -173.8(5) . . . . ? C11 C6 C7 C8 0.6(9) . . . . ? C5 C6 C7 C8 179.5(6) . . . . ? C6 C7 C8 C9 0.8(11) . . . . ? C7 C8 C9 C10 -1.7(13) . . . . ? C8 C9 C10 C11 1.1(14) . . . . ? C7 C6 C11 C10 -1.1(9) . . . . ? C5 C6 C11 C10 180.0(6) . . . . ? C9 C10 C11 C6 0.2(11) . . . . ? C2 C3 C13 C14 -0.3(8) . . . . ? C2 C3 C13 C12 174.1(5) . . . . ? O4 C12 C13 C3 161.0(5) . . . . ? O5 C12 C13 C3 -22.7(7) . . . . ? Tb1 C12 C13 C3 -83(2) 2_646 . . . ? O4 C12 C13 C14 -24.7(8) . . . . ? O5 C12 C13 C14 151.6(5) . . . . ? Tb1 C12 C13 C14 91(2) 2_646 . . . ? C3 C13 C14 C15 2.9(8) . . . . ? C12 C13 C14 C15 -171.3(5) . . . . ? C3 C13 C14 C16 179.6(5) . . . . ? C12 C13 C14 C16 5.4(8) . . . . ? C13 C14 C15 C4 -2.4(8) . . . . ? C16 C14 C15 C4 -179.4(5) . . . . ? C2 C4 C15 C14 -0.8(8) . . . . ? C5 C4 C15 C14 177.6(5) . . . . ? C15 C14 C16 O6 82.6(7) . . . . ? C13 C14 C16 O6 -94.2(8) . . . . ? C15 C14 C16 C17 -91.9(6) . . . . ? C13 C14 C16 C17 91.3(7) . . . . ? O6 C16 C17 C22 176.7(6) . . . . ? C14 C16 C17 C22 -9.0(8) . . . . ? O6 C16 C17 C18 -4.3(9) . . . . ? C14 C16 C17 C18 170.0(5) . . . . ? C22 C17 C18 C19 -1.6(10) . . . . ? C16 C17 C18 C19 179.4(6) . . . . ? C17 C18 C19 C20 0.7(12) . . . . ? C18 C19 C20 C21 1.1(13) . . . . ? C19 C20 C21 C22 -2.1(12) . . . . ? C20 C21 C22 C17 1.1(11) . . . . ? C18 C17 C22 C21 0.6(9) . . . . ? C16 C17 C22 C21 179.7(6) . . . . ? N1 C23 C24 C25 0.2(14) . . . . ? C23 C24 C25 C26 0.3(14) . . . . ? C24 C25 C26 C27 1.1(13) . . . . ? C24 C25 C26 C31 -176.7(9) . . . . ? C25 C26 C27 N1 -3.2(10) . . . . ? C31 C26 C27 N1 174.7(6) . . . . ? C25 C26 C27 C28 -177.8(7) . . . . ? C31 C26 C27 C28 0.2(10) . . . . ? N1 C27 C28 N2 4.3(8) . . . . ? C26 C27 C28 N2 179.1(6) . . . . ? N1 C27 C28 C29 -175.7(5) . . . . ? C26 C27 C28 C29 -0.8(9) . . . . ? N2 C28 C29 C32 0.3(9) . . . . ? C27 C28 C29 C32 -179.8(6) . . . . ? N2 C28 C29 C30 -178.8(6) . . . . ? C27 C28 C29 C30 1.2(9) . . . . ? C32 C29 C30 C31 -179.9(8) . . . . ? C28 C29 C30 C31 -0.9(11) . . . . ? C29 C30 C31 C26 0.2(13) . . . . ? C25 C26 C31 C30 178.0(8) . . . . ? C27 C26 C31 C30 0.2(11) . . . . ? C28 C29 C32 C33 0.3(11) . . . . ? C30 C29 C32 C33 179.3(7) . . . . ? C29 C32 C33 C34 -0.6(12) . . . . ? C32 C33 C34 N2 0.4(11) . . . . ? C24 C23 N1 C27 -2.2(11) . . . . ? C24 C23 N1 Tb1 176.4(7) . . . . ? C26 C27 N1 C23 3.7(9) . . . . ? C28 C27 N1 C23 178.4(6) . . . . ? C26 C27 N1 Tb1 -175.0(5) . . . . ? C28 C27 N1 Tb1 -0.2(7) . . . . ? O7 Tb1 N1 C23 28.4(6) 3_666 . . . ? O7 Tb1 N1 C23 98.8(6) . . . . ? O5 Tb1 N1 C23 -107.0(6) 2_656 . . . ? O1 Tb1 N1 C23 -34.2(8) . . . . ? O2 Tb1 N1 C23 173.5(5) . . . . ? O4 Tb1 N1 C23 -55.4(6) 2_656 . . . ? N2 Tb1 N1 C23 179.4(6) . . . . ? C1 Tb1 N1 C23 -154.9(8) . . . . ? C12 Tb1 N1 C23 -82.1(6) 2_656 . . . ? Tb1 Tb1 N1 C23 63.8(6) 3_666 . . . ? O7 Tb1 N1 C27 -152.9(4) 3_666 . . . ? O7 Tb1 N1 C27 -82.6(4) . . . . ? O5 Tb1 N1 C27 71.6(4) 2_656 . . . ? O1 Tb1 N1 C27 144.4(5) . . . . ? O2 Tb1 N1 C27 -7.9(6) . . . . ? O4 Tb1 N1 C27 123.3(4) 2_656 . . . ? N2 Tb1 N1 C27 -2.0(4) . . . . ? C1 Tb1 N1 C27 23.7(11) . . . . ? C12 Tb1 N1 C27 96.5(4) 2_656 . . . ? Tb1 Tb1 N1 C27 -117.6(4) 3_666 . . . ? C33 C34 N2 C28 0.1(9) . . . . ? C33 C34 N2 Tb1 -173.9(5) . . . . ? C29 C28 N2 C34 -0.5(8) . . . . ? C27 C28 N2 C34 179.6(5) . . . . ? C29 C28 N2 Tb1 173.7(4) . . . . ? C27 C28 N2 Tb1 -6.3(7) . . . . ? O7 Tb1 N2 C34 -134.6(4) 3_666 . . . ? O7 Tb1 N2 C34 -92.2(5) . . . . ? O5 Tb1 N2 C34 80.7(5) 2_656 . . . ? O1 Tb1 N2 C34 12.5(5) . . . . ? O2 Tb1 N2 C34 -5.3(4) . . . . ? O4 Tb1 N2 C34 119.0(5) 2_656 . . . ? N1 Tb1 N2 C34 178.2(5) . . . . ? C1 Tb1 N2 C34 3.1(5) . . . . ? C12 Tb1 N2 C34 100.6(5) 2_656 . . . ? Tb1 Tb1 N2 C34 -109.0(4) 3_666 . . . ? O7 Tb1 N2 C28 51.4(5) 3_666 . . . ? O7 Tb1 N2 C28 93.8(4) . . . . ? O5 Tb1 N2 C28 -93.2(4) 2_656 . . . ? O1 Tb1 N2 C28 -161.5(4) . . . . ? O2 Tb1 N2 C28 -179.3(4) . . . . ? O4 Tb1 N2 C28 -54.9(4) 2_656 . . . ? N1 Tb1 N2 C28 4.2(4) . . . . ? C1 Tb1 N2 C28 -170.9(4) . . . . ? C12 Tb1 N2 C28 -73.4(4) 2_656 . . . ? Tb1 Tb1 N2 C28 77.1(4) 3_666 . . . ? O2 C1 O1 Tb1 -2.8(6) . . . . ? C2 C1 O1 Tb1 178.8(4) . . . . ? O7 Tb1 O1 C1 138.5(3) 3_666 . . . ? O7 Tb1 O1 C1 71.1(4) . . . . ? O5 Tb1 O1 C1 -85.1(3) 2_656 . . . ? O2 Tb1 O1 C1 1.5(3) . . . . ? O4 Tb1 O1 C1 -138.4(3) 2_656 . . . ? N2 Tb1 O1 C1 -20.5(4) . . . . ? N1 Tb1 O1 C1 -158.9(4) . . . . ? C12 Tb1 O1 C1 -111.7(3) 2_656 . . . ? Tb1 Tb1 O1 C1 105.5(3) 3_666 . . . ? O1 C1 O2 Tb1 2.7(5) . . . . ? C2 C1 O2 Tb1 -178.9(4) . . . . ? O7 Tb1 O2 C1 -55.2(3) 3_666 . . . ? O7 Tb1 O2 C1 -118.0(3) . . . . ? O5 Tb1 O2 C1 85.8(3) 2_656 . . . ? O1 Tb1 O2 C1 -1.5(3) . . . . ? O4 Tb1 O2 C1 50.5(4) 2_656 . . . ? N2 Tb1 O2 C1 162.0(3) . . . . ? N1 Tb1 O2 C1 167.4(3) . . . . ? C12 Tb1 O2 C1 71.3(3) 2_656 . . . ? Tb1 Tb1 O2 C1 -89.7(3) 3_666 . . . ? O5 C12 O4 Tb1 -6.5(5) . . . 2_646 ? C13 C12 O4 Tb1 169.6(4) . . . 2_646 ? O4 C12 O5 Tb1 6.8(6) . . . 2_646 ? C13 C12 O5 Tb1 -169.4(4) . . . 2_646 ? O7 Tb1 O7 Tb1 0.0 3_666 . . 3_666 ? O5 Tb1 O7 Tb1 -167.4(3) 2_656 . . 3_666 ? O1 Tb1 O7 Tb1 77.88(17) . . . 3_666 ? O2 Tb1 O7 Tb1 127.11(16) . . . 3_666 ? O4 Tb1 O7 Tb1 -35.2(3) 2_656 . . 3_666 ? N2 Tb1 O7 Tb1 -151.82(18) . . . 3_666 ? N1 Tb1 O7 Tb1 -87.22(17) . . . 3_666 ? C1 Tb1 O7 Tb1 103.30(17) . . . 3_666 ? C12 Tb1 O7 Tb1 -90.8(5) 2_656 . . 3_666 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.920 _refine_diff_density_min -1.337 _refine_diff_density_rms 0.337 _database_code_depnum_ccdc_archive 'CCDC 890971' ####################################################################### # # 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_11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H20 Dy N2 O7' _chemical_formula_sum 'C34 H20 Dy N2 O7' _chemical_formula_weight 731.02 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9684(6) _cell_length_b 12.6499(4) _cell_length_c 19.6347(17) _cell_angle_alpha 90.00 _cell_angle_beta 108.000(6) _cell_angle_gamma 90.00 _cell_volume 2827.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4844 _cell_measurement_theta_min 3.2144 _cell_measurement_theta_max 29.1508 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 2.698 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.96576 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlis (Oxford Diffraction, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10757 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4737 _reflns_number_gt 3822 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+1.8875P] 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 4737 _refine_ls_number_parameters 397 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.043 _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 Dy1 Dy 0.507710(19) 0.398114(16) 0.568040(12) 0.02573(9) Uani 1 1 d . . . C1 C 0.6321(4) 0.4935(4) 0.6959(3) 0.0329(12) Uani 1 1 d . . . C2 C 0.3693(5) 0.2714(4) 0.6255(3) 0.0350(12) Uani 1 1 d . . . C3 C 0.6955(4) 0.5463(4) 0.7655(3) 0.0304(11) Uani 1 1 d . . . C4 C 0.6422(4) 0.6308(4) 0.7878(3) 0.0329(12) Uani 1 1 d . . . H4 H 0.5668 0.6507 0.7605 0.039 Uiso 1 1 calc R . . C5 C 0.3013(4) 0.1873(4) 0.6497(3) 0.0312(11) Uani 1 1 d . . . C6 C 0.1884(4) 0.1575(4) 0.6098(3) 0.0346(12) Uani 1 1 d . . . C7 C 0.8627(4) 0.5710(4) 0.8692(3) 0.0379(13) Uani 1 1 d . . . H7 H 0.9375 0.5507 0.8972 0.045 Uiso 1 1 calc R . . C8 C 0.8076(4) 0.5134(4) 0.8086(3) 0.0341(12) Uani 1 1 d . . . C9 C 0.8718(5) 0.4171(4) 0.7937(3) 0.0394(13) Uani 1 1 d . . . C10 C 0.8191(5) 0.3107(4) 0.7985(3) 0.0424(14) Uani 1 1 d . . . C11 C 0.7244(5) 0.2960(5) 0.8226(3) 0.0546(17) Uani 1 1 d . . . H11 H 0.6895 0.3542 0.8367 0.065 Uiso 1 1 calc R . . C12 C 0.6794(6) 0.1951(5) 0.8262(4) 0.068(2) Uani 1 1 d . . . H12 H 0.6153 0.1857 0.8429 0.082 Uiso 1 1 calc R . . C13 C 0.7309(6) 0.1105(6) 0.8049(4) 0.072(2) Uani 1 1 d U . . H13 H 0.7001 0.0432 0.8059 0.087 Uiso 1 1 calc R . . C14 C 0.8243(6) 0.1223(6) 0.7826(4) 0.070(2) Uani 1 1 d U . . H14 H 0.8583 0.0630 0.7692 0.084 Uiso 1 1 calc R . . C15 C 0.8731(6) 0.2236(5) 0.7789(3) 0.0575(18) Uani 1 1 d . . . H15 H 0.9391 0.2314 0.7638 0.069 Uiso 1 1 calc R . . C16 C 0.1176(4) 0.2118(4) 0.5408(3) 0.0365(13) Uani 1 1 d . . . C17 C 0.0380(4) 0.2983(4) 0.5471(3) 0.0331(12) Uani 1 1 d . . . C18 C 0.0412(5) 0.3395(4) 0.6126(3) 0.0443(14) Uani 1 1 d . . . H18 H 0.0944 0.3128 0.6542 0.053 Uiso 1 1 calc R . . C19 C -0.0333(5) 0.4194(5) 0.6168(4) 0.0577(17) Uani 1 1 d U . . H19 H -0.0317 0.4464 0.6611 0.069 Uiso 1 1 calc R . . C20 C -0.1104(5) 0.4593(5) 0.5553(4) 0.0617(17) Uani 1 1 d U . . H20 H -0.1595 0.5149 0.5581 0.074 Uiso 1 1 calc R . . C21 C -0.1160(5) 0.4192(5) 0.4909(4) 0.0570(17) Uani 1 1 d U . . H21 H -0.1698 0.4463 0.4497 0.068 Uiso 1 1 calc R . . C22 C -0.0418(5) 0.3378(4) 0.4858(3) 0.0464(15) Uani 1 1 d . . . H22 H -0.0458 0.3099 0.4413 0.056 Uiso 1 1 calc R . . C23 C 0.3091(5) 0.2948(5) 0.4161(3) 0.0604(19) Uani 1 1 d . . . H23 H 0.2687 0.3551 0.4221 0.072 Uiso 1 1 calc R . . C24 C 0.2547(6) 0.2264(6) 0.3597(4) 0.076(2) Uani 1 1 d . . . H24 H 0.1794 0.2404 0.3296 0.091 Uiso 1 1 calc R . . C25 C 0.3141(6) 0.1388(6) 0.3497(4) 0.070(2) Uani 1 1 d . . . H25 H 0.2801 0.0930 0.3119 0.084 Uiso 1 1 calc R . . C26 C 0.4244(6) 0.1186(5) 0.3956(4) 0.0541(17) Uani 1 1 d . . . C27 C 0.4758(5) 0.1912(4) 0.4506(3) 0.0419(14) Uani 1 1 d . . . C28 C 0.5890(5) 0.1720(4) 0.4999(3) 0.0373(13) Uani 1 1 d . . . C29 C 0.6507(5) 0.0807(4) 0.4931(4) 0.0476(15) Uani 1 1 d . . . C30 C 0.5965(6) 0.0070(6) 0.4377(4) 0.0683(19) Uani 1 1 d U . . H30 H 0.6359 -0.0551 0.4341 0.082 Uiso 1 1 calc R . . C31 C 0.4924(6) 0.0246(6) 0.3918(4) 0.0692(19) Uani 1 1 d U . . H31 H 0.4611 -0.0245 0.3556 0.083 Uiso 1 1 calc R . . C32 C 0.7617(6) 0.0645(5) 0.5426(4) 0.0613(19) Uani 1 1 d . . . H32 H 0.8050 0.0045 0.5397 0.074 Uiso 1 1 calc R . . C33 C 0.8055(5) 0.1366(5) 0.5947(4) 0.0580(18) Uani 1 1 d . . . H33 H 0.8791 0.1266 0.6282 0.070 Uiso 1 1 calc R . . C34 C 0.7402(5) 0.2256(4) 0.5980(3) 0.0461(15) Uani 1 1 d . . . H34 H 0.7724 0.2750 0.6339 0.055 Uiso 1 1 calc R . . N1 N 0.4147(4) 0.2782(3) 0.4612(2) 0.0393(11) Uani 1 1 d . . . N2 N 0.6342(4) 0.2443(3) 0.5528(2) 0.0361(11) Uani 1 1 d . . . O1 O 0.6877(3) 0.4348(3) 0.66624(18) 0.0365(8) Uani 1 1 d . . . O2 O 0.5248(3) 0.5132(3) 0.66764(19) 0.0462(10) Uani 1 1 d . . . O3 O 0.4793(3) 0.2640(3) 0.6460(2) 0.0475(10) Uani 1 1 d . . . O4 O 0.3162(3) 0.3419(3) 0.5825(2) 0.0414(9) Uani 1 1 d . . . O5 O 0.9663(3) 0.4285(3) 0.7859(2) 0.0576(11) Uani 1 1 d . . . O6 O 0.1203(4) 0.1772(3) 0.4841(2) 0.0633(13) Uani 1 1 d . . . O7 O 0.3969(3) 0.5263(2) 0.50205(18) 0.0326(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.03201(14) 0.02171(13) 0.02252(14) 0.00052(10) 0.00704(10) 0.00393(10) C1 0.040(3) 0.027(3) 0.028(3) 0.000(2) 0.006(2) 0.004(2) C2 0.051(3) 0.026(3) 0.032(3) 0.004(2) 0.019(3) 0.006(2) C3 0.038(3) 0.026(3) 0.028(3) -0.005(2) 0.012(2) -0.003(2) C4 0.036(3) 0.032(3) 0.028(3) -0.001(2) 0.007(2) -0.002(2) C5 0.042(3) 0.024(2) 0.031(3) 0.000(2) 0.016(2) 0.004(2) C6 0.043(3) 0.032(3) 0.030(3) 0.002(2) 0.013(2) 0.011(2) C7 0.032(3) 0.041(3) 0.037(3) -0.007(2) 0.005(2) -0.002(2) C8 0.038(3) 0.038(3) 0.028(3) -0.003(2) 0.013(2) -0.002(2) C9 0.037(3) 0.047(3) 0.029(3) -0.006(2) 0.003(2) 0.008(2) C10 0.051(3) 0.038(3) 0.031(3) -0.005(2) 0.001(3) 0.009(3) C11 0.054(4) 0.042(4) 0.060(4) 0.005(3) 0.006(3) 0.005(3) C12 0.067(4) 0.061(4) 0.065(5) 0.007(4) 0.003(4) -0.010(4) C13 0.074(2) 0.070(2) 0.071(2) 0.0003(10) 0.0200(11) -0.0006(10) C14 0.072(2) 0.068(2) 0.069(2) -0.0009(10) 0.0192(11) 0.0022(10) C15 0.068(4) 0.048(4) 0.044(4) -0.006(3) 0.000(3) 0.015(3) C16 0.044(3) 0.034(3) 0.031(3) 0.006(2) 0.012(3) 0.009(2) C17 0.036(3) 0.034(3) 0.029(3) 0.005(2) 0.011(2) 0.002(2) C18 0.040(3) 0.052(4) 0.042(4) 0.000(3) 0.014(3) 0.007(3) C19 0.0577(18) 0.0584(19) 0.0578(19) -0.0031(10) 0.0189(11) 0.0000(10) C20 0.0601(19) 0.0615(19) 0.0634(19) -0.0015(10) 0.0193(11) 0.0021(10) C21 0.0557(18) 0.0570(18) 0.0574(19) 0.0006(10) 0.0162(10) 0.0023(10) C22 0.044(3) 0.047(3) 0.041(4) -0.001(3) 0.004(3) 0.008(3) C23 0.061(4) 0.057(4) 0.047(4) -0.011(3) -0.006(3) 0.007(3) C24 0.056(4) 0.097(6) 0.055(5) -0.021(4) -0.009(4) -0.004(4) C25 0.077(5) 0.076(5) 0.052(4) -0.034(4) 0.015(4) -0.020(4) C26 0.069(4) 0.048(4) 0.053(4) -0.020(3) 0.029(4) -0.012(3) C27 0.052(3) 0.030(3) 0.047(4) -0.011(3) 0.020(3) -0.004(2) C28 0.047(3) 0.031(3) 0.041(3) -0.007(2) 0.025(3) 0.004(2) C29 0.060(4) 0.032(3) 0.062(4) -0.007(3) 0.034(3) 0.003(3) C30 0.069(2) 0.067(2) 0.069(2) -0.0025(10) 0.0226(11) 0.0014(10) C31 0.070(2) 0.069(2) 0.070(2) -0.0030(10) 0.0227(11) -0.0006(10) C32 0.069(4) 0.037(3) 0.090(5) 0.001(3) 0.042(4) 0.022(3) C33 0.054(4) 0.052(4) 0.069(5) 0.003(3) 0.021(3) 0.022(3) C34 0.049(3) 0.043(3) 0.046(4) -0.002(3) 0.013(3) 0.009(3) N1 0.046(3) 0.040(3) 0.030(2) -0.007(2) 0.009(2) 0.004(2) N2 0.040(2) 0.029(2) 0.039(3) 0.001(2) 0.012(2) 0.0067(19) O1 0.0410(19) 0.0387(19) 0.029(2) -0.0095(16) 0.0101(17) 0.0074(16) O2 0.043(2) 0.053(2) 0.035(2) -0.0169(18) 0.0008(18) 0.0105(18) O3 0.039(2) 0.048(2) 0.054(3) 0.0236(19) 0.0109(19) 0.0032(17) O4 0.046(2) 0.035(2) 0.045(2) 0.0171(17) 0.0152(18) 0.0081(17) O5 0.042(2) 0.067(3) 0.067(3) -0.006(2) 0.022(2) 0.005(2) O6 0.095(3) 0.063(3) 0.033(2) 0.004(2) 0.022(2) 0.038(2) O7 0.0312(17) 0.0349(19) 0.0323(19) 0.0116(15) 0.0108(15) 0.0074(15) _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 O7 2.238(3) . ? Dy1 O7 2.254(3) 3_666 ? Dy1 O3 2.379(4) . ? Dy1 O2 2.395(3) . ? Dy1 O1 2.450(3) . ? Dy1 O4 2.499(4) . ? Dy1 N2 2.539(4) . ? Dy1 N1 2.549(4) . ? C1 O1 1.255(6) . ? C1 O2 1.256(6) . ? C1 C3 1.498(7) . ? C2 O3 1.256(6) . ? C2 O4 1.257(6) . ? C2 C5 1.502(7) . ? C3 C4 1.384(7) . ? C3 C8 1.410(6) . ? C4 C5 1.400(7) 2_656 ? C4 H4 0.9300 . ? C5 C6 1.389(7) . ? C5 C4 1.400(7) 2_646 ? C6 C7 1.377(7) 2_646 ? C6 C16 1.521(7) . ? C7 C6 1.377(7) 2_656 ? C7 C8 1.378(7) . ? C7 H7 0.9300 . ? C8 C9 1.516(7) . ? C9 O5 1.196(7) . ? C9 C10 1.502(8) . ? C10 C11 1.369(9) . ? C10 C15 1.391(8) . ? C11 C12 1.396(8) . ? C11 H11 0.9300 . ? C12 C13 1.365(10) . ? C12 H12 0.9300 . ? C13 C14 1.328(10) . ? C13 H13 0.9300 . ? C14 C15 1.420(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O6 1.206(6) . ? C16 C17 1.480(7) . ? C17 C18 1.376(8) . ? C17 C22 1.379(7) . ? C18 C19 1.367(8) . ? C18 H18 0.9300 . ? C19 C20 1.369(8) . ? C19 H19 0.9300 . ? C20 C21 1.344(9) . ? C20 H20 0.9300 . ? C21 C22 1.384(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 N1 1.316(7) . ? C23 C24 1.398(8) . ? C23 H23 0.9300 . ? C24 C25 1.363(10) . ? C24 H24 0.9300 . ? C25 C26 1.374(9) . ? C25 H25 0.9300 . ? C26 C27 1.406(8) . ? C26 C31 1.456(9) . ? C27 N1 1.372(7) . ? C27 C28 1.422(7) . ? C28 N2 1.365(6) . ? C28 C29 1.399(7) . ? C29 C32 1.397(8) . ? C29 C30 1.427(9) . ? C30 C31 1.312(8) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.351(9) . ? C32 H32 0.9300 . ? C33 C34 1.383(8) . ? C33 H33 0.9300 . ? C34 N2 1.326(6) . ? C34 H34 0.9300 . ? O7 Dy1 2.254(3) 3_666 ? 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 O7 Dy1 O7 70.15(13) . 3_666 ? O7 Dy1 O3 135.45(12) . . ? O7 Dy1 O3 153.54(12) 3_666 . ? O7 Dy1 O2 85.30(12) . . ? O7 Dy1 O2 108.02(13) 3_666 . ? O3 Dy1 O2 84.32(14) . . ? O7 Dy1 O1 122.54(11) . . ? O7 Dy1 O1 84.98(12) 3_666 . ? O3 Dy1 O1 83.93(12) . . ? O2 Dy1 O1 53.85(12) . . ? O7 Dy1 O4 82.64(11) . . ? O7 Dy1 O4 147.74(11) 3_666 . ? O3 Dy1 O4 53.51(11) . . ? O2 Dy1 O4 85.97(13) . . ? O1 Dy1 O4 125.33(12) . . ? O7 Dy1 N2 139.07(14) . . ? O7 Dy1 N2 79.63(13) 3_666 . ? O3 Dy1 N2 74.83(14) . . ? O2 Dy1 N2 131.17(12) . . ? O1 Dy1 N2 80.02(12) . . ? O4 Dy1 N2 113.37(12) . . ? O7 Dy1 N1 85.68(13) . . ? O7 Dy1 N1 85.66(14) 3_666 . ? O3 Dy1 N1 89.57(14) . . ? O2 Dy1 N1 159.86(14) . . ? O1 Dy1 N1 144.53(12) . . ? O4 Dy1 N1 75.04(14) . . ? N2 Dy1 N1 64.64(13) . . ? O7 Dy1 Dy1 35.23(9) . 3_666 ? O7 Dy1 Dy1 34.93(7) 3_666 3_666 ? O3 Dy1 Dy1 169.35(8) . 3_666 ? O2 Dy1 Dy1 98.04(10) . 3_666 ? O1 Dy1 Dy1 105.89(9) . 3_666 ? O4 Dy1 Dy1 116.14(7) . 3_666 ? N2 Dy1 Dy1 110.45(10) . 3_666 ? N1 Dy1 Dy1 84.71(10) . 3_666 ? O1 C1 O2 121.9(4) . . ? O1 C1 C3 119.7(4) . . ? O2 C1 C3 118.4(5) . . ? O3 C2 O4 122.0(5) . . ? O3 C2 C5 117.5(4) . . ? O4 C2 C5 120.3(5) . . ? C4 C3 C8 119.0(4) . . ? C4 C3 C1 118.6(4) . . ? C8 C3 C1 122.4(4) . . ? C3 C4 C5 121.8(5) . 2_656 ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 2_656 . ? C6 C5 C4 118.6(5) . 2_646 ? C6 C5 C2 122.7(5) . . ? C4 C5 C2 118.5(4) 2_646 . ? C7 C6 C5 119.4(5) 2_646 . ? C7 C6 C16 116.6(4) 2_646 . ? C5 C6 C16 123.9(5) . . ? C6 C7 C8 122.7(5) 2_656 . ? C6 C7 H7 118.6 2_656 . ? C8 C7 H7 118.6 . . ? C7 C8 C3 118.4(5) . . ? C7 C8 C9 117.1(4) . . ? C3 C8 C9 124.5(4) . . ? O5 C9 C10 123.2(5) . . ? O5 C9 C8 118.9(5) . . ? C10 C9 C8 117.4(5) . . ? C11 C10 C15 119.5(6) . . ? C11 C10 C9 123.5(5) . . ? C15 C10 C9 116.9(6) . . ? C10 C11 C12 121.0(6) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 118.9(8) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 121.2(7) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 121.4(7) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C10 C15 C14 117.9(7) . . ? C10 C15 H15 121.1 . . ? C14 C15 H15 121.1 . . ? O6 C16 C17 123.1(5) . . ? O6 C16 C6 119.4(5) . . ? C17 C16 C6 117.1(5) . . ? C18 C17 C22 119.4(5) . . ? C18 C17 C16 121.6(5) . . ? C22 C17 C16 119.0(5) . . ? C19 C18 C17 120.4(5) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 119.6(7) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C21 C20 C19 121.0(6) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 120.2(6) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C17 C22 C21 119.5(6) . . ? C17 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? N1 C23 C24 123.3(6) . . ? N1 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C25 C24 C23 118.8(6) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 119.6(6) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 119.1(6) . . ? C25 C26 C31 123.8(6) . . ? C27 C26 C31 117.1(6) . . ? N1 C27 C26 120.9(5) . . ? N1 C27 C28 118.4(5) . . ? C26 C27 C28 120.6(5) . . ? N2 C28 C29 121.9(5) . . ? N2 C28 C27 118.2(4) . . ? C29 C28 C27 119.8(5) . . ? C32 C29 C28 118.1(5) . . ? C32 C29 C30 123.0(6) . . ? C28 C29 C30 118.8(6) . . ? C31 C30 C29 121.7(7) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 C26 122.0(7) . . ? C30 C31 H31 119.0 . . ? C26 C31 H31 119.0 . . ? C33 C32 C29 119.4(5) . . ? C33 C32 H32 120.3 . . ? C29 C32 H32 120.3 . . ? C32 C33 C34 119.5(6) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? N2 C34 C33 123.5(6) . . ? N2 C34 H34 118.3 . . ? C33 C34 H34 118.3 . . ? C23 N1 C27 118.2(5) . . ? C23 N1 Dy1 122.9(4) . . ? C27 N1 Dy1 118.9(3) . . ? C34 N2 C28 117.6(4) . . ? C34 N2 Dy1 122.6(3) . . ? C28 N2 Dy1 119.6(3) . . ? C1 O1 Dy1 90.8(3) . . ? C1 O2 Dy1 93.4(3) . . ? C2 O3 Dy1 94.9(3) . . ? C2 O4 Dy1 89.3(3) . . ? Dy1 O7 Dy1 109.85(13) . 3_666 ? 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 C3 C4 163.1(5) . . . . ? O2 C1 C3 C4 -14.1(7) . . . . ? O1 C1 C3 C8 -16.3(8) . . . . ? O2 C1 C3 C8 166.5(5) . . . . ? C8 C3 C4 C5 2.8(8) . . . 2_656 ? C1 C3 C4 C5 -176.7(5) . . . 2_656 ? O3 C2 C5 C6 -150.9(5) . . . . ? O4 C2 C5 C6 24.5(8) . . . . ? O3 C2 C5 C4 23.8(7) . . . 2_646 ? O4 C2 C5 C4 -160.8(5) . . . 2_646 ? C4 C5 C6 C7 -2.8(8) 2_646 . . 2_646 ? C2 C5 C6 C7 171.8(5) . . . 2_646 ? C4 C5 C6 C16 -179.8(5) 2_646 . . . ? C2 C5 C6 C16 -5.1(8) . . . . ? C6 C7 C8 C3 1.6(8) 2_656 . . . ? C6 C7 C8 C9 -177.3(5) 2_656 . . . ? C4 C3 C8 C7 -3.8(8) . . . . ? C1 C3 C8 C7 175.7(5) . . . . ? C4 C3 C8 C9 175.0(5) . . . . ? C1 C3 C8 C9 -5.6(8) . . . . ? C7 C8 C9 O5 -59.8(8) . . . . ? C3 C8 C9 O5 121.5(6) . . . . ? C7 C8 C9 C10 113.0(6) . . . . ? C3 C8 C9 C10 -65.8(7) . . . . ? O5 C9 C10 C11 165.3(6) . . . . ? C8 C9 C10 C11 -7.1(8) . . . . ? O5 C9 C10 C15 -12.9(8) . . . . ? C8 C9 C10 C15 174.7(5) . . . . ? C15 C10 C11 C12 -1.5(9) . . . . ? C9 C10 C11 C12 -179.6(5) . . . . ? C10 C11 C12 C13 -0.4(10) . . . . ? C11 C12 C13 C14 1.7(11) . . . . ? C12 C13 C14 C15 -1.1(11) . . . . ? C11 C10 C15 C14 2.1(8) . . . . ? C9 C10 C15 C14 -179.7(5) . . . . ? C13 C14 C15 C10 -0.8(10) . . . . ? C7 C6 C16 O6 -83.2(7) 2_646 . . . ? C5 C6 C16 O6 93.8(7) . . . . ? C7 C6 C16 C17 90.0(6) 2_646 . . . ? C5 C6 C16 C17 -92.9(6) . . . . ? O6 C16 C17 C18 -176.8(6) . . . . ? C6 C16 C17 C18 10.2(8) . . . . ? O6 C16 C17 C22 3.7(8) . . . . ? C6 C16 C17 C22 -169.3(5) . . . . ? C22 C17 C18 C19 -0.5(9) . . . . ? C16 C17 C18 C19 179.9(5) . . . . ? C17 C18 C19 C20 -0.9(9) . . . . ? C18 C19 C20 C21 1.7(10) . . . . ? C19 C20 C21 C22 -1.2(10) . . . . ? C18 C17 C22 C21 1.0(8) . . . . ? C16 C17 C22 C21 -179.4(5) . . . . ? C20 C21 C22 C17 -0.2(10) . . . . ? N1 C23 C24 C25 -1.2(12) . . . . ? C23 C24 C25 C26 1.2(12) . . . . ? C24 C25 C26 C27 -2.5(11) . . . . ? C24 C25 C26 C31 176.7(8) . . . . ? C25 C26 C27 N1 3.7(10) . . . . ? C31 C26 C27 N1 -175.5(6) . . . . ? C25 C26 C27 C28 179.0(6) . . . . ? C31 C26 C27 C28 -0.2(9) . . . . ? N1 C27 C28 N2 -3.7(8) . . . . ? C26 C27 C28 N2 -179.2(6) . . . . ? N1 C27 C28 C29 176.2(6) . . . . ? C26 C27 C28 C29 0.8(9) . . . . ? N2 C28 C29 C32 0.0(9) . . . . ? C27 C28 C29 C32 -179.9(6) . . . . ? N2 C28 C29 C30 178.2(6) . . . . ? C27 C28 C29 C30 -1.8(9) . . . . ? C32 C29 C30 C31 -179.6(7) . . . . ? C28 C29 C30 C31 2.4(11) . . . . ? C29 C30 C31 C26 -1.8(11) . . . . ? C25 C26 C31 C30 -178.4(7) . . . . ? C27 C26 C31 C30 0.8(11) . . . . ? C28 C29 C32 C33 -0.1(10) . . . . ? C30 C29 C32 C33 -178.1(7) . . . . ? C29 C32 C33 C34 -0.4(11) . . . . ? C32 C33 C34 N2 1.0(11) . . . . ? C24 C23 N1 C27 2.3(10) . . . . ? C24 C23 N1 Dy1 -176.3(6) . . . . ? C26 C27 N1 C23 -3.5(9) . . . . ? C28 C27 N1 C23 -178.9(5) . . . . ? C26 C27 N1 Dy1 175.2(5) . . . . ? C28 C27 N1 Dy1 -0.3(7) . . . . ? O7 Dy1 N1 C23 -28.2(5) . . . . ? O7 Dy1 N1 C23 -98.6(5) 3_666 . . . ? O3 Dy1 N1 C23 107.4(5) . . . . ? O2 Dy1 N1 C23 35.4(7) . . . . ? O1 Dy1 N1 C23 -173.7(4) . . . . ? O4 Dy1 N1 C23 55.3(5) . . . . ? N2 Dy1 N1 C23 -179.2(5) . . . . ? Dy1 Dy1 N1 C23 -63.6(5) 3_666 . . . ? O7 Dy1 N1 C27 153.2(4) . . . . ? O7 Dy1 N1 C27 82.8(4) 3_666 . . . ? O3 Dy1 N1 C27 -71.2(4) . . . . ? O2 Dy1 N1 C27 -143.2(4) . . . . ? O1 Dy1 N1 C27 7.7(6) . . . . ? O4 Dy1 N1 C27 -123.3(4) . . . . ? N2 Dy1 N1 C27 2.2(4) . . . . ? Dy1 Dy1 N1 C27 117.8(4) 3_666 . . . ? C33 C34 N2 C28 -1.0(9) . . . . ? C33 C34 N2 Dy1 173.3(5) . . . . ? C29 C28 N2 C34 0.5(8) . . . . ? C27 C28 N2 C34 -179.6(5) . . . . ? C29 C28 N2 Dy1 -174.0(4) . . . . ? C27 C28 N2 Dy1 5.9(7) . . . . ? O7 Dy1 N2 C34 133.9(4) . . . . ? O7 Dy1 N2 C34 91.5(4) 3_666 . . . ? O3 Dy1 N2 C34 -81.5(4) . . . . ? O2 Dy1 N2 C34 -13.5(5) . . . . ? O1 Dy1 N2 C34 4.8(4) . . . . ? O4 Dy1 N2 C34 -119.5(4) . . . . ? N1 Dy1 N2 C34 -178.4(5) . . . . ? Dy1 Dy1 N2 C34 108.2(4) 3_666 . . . ? O7 Dy1 N2 C28 -51.9(5) . . . . ? O7 Dy1 N2 C28 -94.3(4) 3_666 . . . ? O3 Dy1 N2 C28 92.7(4) . . . . ? O2 Dy1 N2 C28 160.8(4) . . . . ? O1 Dy1 N2 C28 179.0(4) . . . . ? O4 Dy1 N2 C28 54.7(4) . . . . ? N1 Dy1 N2 C28 -4.2(4) . . . . ? Dy1 Dy1 N2 C28 -77.6(4) 3_666 . . . ? O2 C1 O1 Dy1 -3.3(5) . . . . ? C3 C1 O1 Dy1 179.6(4) . . . . ? O7 Dy1 O1 C1 55.9(3) . . . . ? O7 Dy1 O1 C1 118.5(3) 3_666 . . . ? O3 Dy1 O1 C1 -85.6(3) . . . . ? O2 Dy1 O1 C1 1.8(3) . . . . ? O4 Dy1 O1 C1 -49.5(3) . . . . ? N2 Dy1 O1 C1 -161.2(3) . . . . ? N1 Dy1 O1 C1 -166.2(3) . . . . ? Dy1 Dy1 O1 C1 90.2(3) 3_666 . . . ? O1 C1 O2 Dy1 3.4(5) . . . . ? C3 C1 O2 Dy1 -179.5(4) . . . . ? O7 Dy1 O2 C1 -138.6(3) . . . . ? O7 Dy1 O2 C1 -71.2(3) 3_666 . . . ? O3 Dy1 O2 C1 84.8(3) . . . . ? O1 Dy1 O2 C1 -1.8(3) . . . . ? O4 Dy1 O2 C1 138.5(3) . . . . ? N2 Dy1 O2 C1 20.7(4) . . . . ? N1 Dy1 O2 C1 157.8(4) . . . . ? Dy1 Dy1 O2 C1 -105.7(3) 3_666 . . . ? O4 C2 O3 Dy1 -6.0(6) . . . . ? C5 C2 O3 Dy1 169.3(4) . . . . ? O7 Dy1 O3 C2 15.0(4) . . . . ? O7 Dy1 O3 C2 -147.8(3) 3_666 . . . ? O2 Dy1 O3 C2 92.4(3) . . . . ? O1 Dy1 O3 C2 146.5(3) . . . . ? O4 Dy1 O3 C2 3.2(3) . . . . ? N2 Dy1 O3 C2 -132.2(3) . . . . ? N1 Dy1 O3 C2 -68.4(3) . . . . ? Dy1 Dy1 O3 C2 -11.0(8) 3_666 . . . ? O3 C2 O4 Dy1 5.7(5) . . . . ? C5 C2 O4 Dy1 -169.5(4) . . . . ? O7 Dy1 O4 C2 -174.9(3) . . . . ? O7 Dy1 O4 C2 152.9(3) 3_666 . . . ? O3 Dy1 O4 C2 -3.2(3) . . . . ? O2 Dy1 O4 C2 -89.1(3) . . . . ? O1 Dy1 O4 C2 -49.9(3) . . . . ? N2 Dy1 O4 C2 44.4(3) . . . . ? N1 Dy1 O4 C2 97.7(3) . . . . ? Dy1 Dy1 O4 C2 173.9(3) 3_666 . . . ? O7 Dy1 O7 Dy1 0.0 3_666 . . 3_666 ? O3 Dy1 O7 Dy1 -171.92(15) . . . 3_666 ? O2 Dy1 O7 Dy1 111.08(15) . . . 3_666 ? O1 Dy1 O7 Dy1 70.08(18) . . . 3_666 ? O4 Dy1 O7 Dy1 -162.39(16) . . . 3_666 ? N2 Dy1 O7 Dy1 -44.9(2) . . . 3_666 ? N1 Dy1 O7 Dy1 -86.94(16) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.179 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 890972' ####################################################################### # # 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_12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C34 H21 Er N2 O7' _chemical_formula_sum 'C34 H21 Er N2 O7' _chemical_formula_weight 736.79 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0185(4) _cell_length_b 12.6199(5) _cell_length_c 19.5860(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.006(3) _cell_angle_gamma 90.00 _cell_volume 2825.16(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6272 _cell_measurement_theta_min 2.3555 _cell_measurement_theta_max 27.4894 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 3.026 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7409 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14264 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0941 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4328 _reflns_number_gt 3132 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.869 Explanation: This alarm has arisen due to the weak diffraction of the crystal. ; _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^)+(0.0034P)^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 4328 _refine_ls_number_parameters 397 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0476 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.908 _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 Er1 Er 0.508502(18) 0.398517(15) 0.567600(10) 0.02573(8) Uani 1 1 d . . . C1 C 0.6304(5) 0.4934(3) 0.6948(2) 0.0303(11) Uani 1 1 d . . . C2 C 0.6930(4) 0.5468(3) 0.7651(2) 0.0304(11) Uani 1 1 d . . . C3 C 0.6390(4) 0.6312(3) 0.7869(2) 0.0330(12) Uani 1 1 d . . . H3 H 0.5637 0.6504 0.7596 0.040 Uiso 1 1 calc R . . C4 C 0.6959(4) 0.6884(3) 0.8496(2) 0.0312(11) Uani 1 1 d . . . C5 C 0.8089(4) 0.6594(4) 0.8903(2) 0.0319(11) Uani 1 1 d . . . C6 C 0.8597(4) 0.5726(4) 0.8692(2) 0.0365(12) Uani 1 1 d . . . H6 H 0.9342 0.5520 0.8971 0.044 Uiso 1 1 calc R . . C7 C 0.8036(4) 0.5145(4) 0.8073(2) 0.0328(11) Uani 1 1 d . . . C8 C 0.3719(5) 0.2720(4) 0.6256(2) 0.0336(12) Uani 1 1 d . . . C9 C 0.8792(4) 0.7138(4) 0.9589(3) 0.0373(13) Uani 1 1 d . . . C10 C 0.9600(4) 0.7998(4) 0.9533(2) 0.0320(11) Uani 1 1 d . . . C11 C 0.9557(5) 0.8408(4) 0.8868(3) 0.0459(14) Uani 1 1 d . . . H11 H 0.9014 0.8150 0.8453 0.055 Uiso 1 1 calc R . . C12 C 1.0334(5) 0.9213(4) 0.8825(3) 0.0592(17) Uani 1 1 d . . . H12 H 1.0335 0.9480 0.8383 0.071 Uiso 1 1 calc R . . C13 C 1.1108(6) 0.9605(5) 0.9462(3) 0.0679(18) Uani 1 1 d U . . H13 H 1.1601 1.0166 0.9445 0.082 Uiso 1 1 calc R . . C14 C 1.1149(5) 0.9185(5) 1.0092(3) 0.0627(17) Uani 1 1 d . . . H14 H 1.1689 0.9440 1.0509 0.075 Uiso 1 1 calc R . . C15 C 1.0413(4) 0.8389(4) 1.0136(3) 0.0453(14) Uani 1 1 d . . . H15 H 1.0461 0.8105 1.0582 0.054 Uiso 1 1 calc R . . C16 C 0.8694(5) 0.4187(4) 0.7936(2) 0.0386(13) Uani 1 1 d . . . C17 C 0.8199(5) 0.3114(4) 0.7973(3) 0.0407(13) Uani 1 1 d . . . C18 C 0.8718(6) 0.2229(5) 0.7790(3) 0.0608(18) Uani 1 1 d . . . H18 H 0.9384 0.2298 0.7648 0.073 Uiso 1 1 calc R . . C19 C 0.8237(6) 0.1225(5) 0.7820(3) 0.0691(19) Uani 1 1 d U . . H19 H 0.8578 0.0637 0.7680 0.083 Uiso 1 1 calc R . . C20 C 0.7337(6) 0.1092(6) 0.8036(4) 0.0737(19) Uani 1 1 d U . . H20 H 0.7042 0.0413 0.8046 0.088 Uiso 1 1 calc R . . C21 C 0.6801(6) 0.1944(5) 0.8255(3) 0.075(2) Uani 1 1 d . . . H21 H 0.6159 0.1844 0.8418 0.090 Uiso 1 1 calc R . . C22 C 0.7257(5) 0.2967(4) 0.8224(3) 0.0514(15) Uani 1 1 d . . . H22 H 0.6919 0.3549 0.8375 0.062 Uiso 1 1 calc R . . C23 C 0.7388(5) 0.2280(4) 0.5974(3) 0.0461(14) Uani 1 1 d . . . H23 H 0.7694 0.2767 0.6341 0.055 Uiso 1 1 calc R . . C24 C 0.8070(5) 0.1393(4) 0.5938(3) 0.0569(16) Uani 1 1 d . . . H24 H 0.8816 0.1313 0.6262 0.068 Uiso 1 1 calc R . . C25 C 0.7627(6) 0.0657(4) 0.5425(3) 0.0591(17) Uani 1 1 d . . . H25 H 0.8058 0.0055 0.5397 0.071 Uiso 1 1 calc R . . C26 C 0.6511(5) 0.0811(4) 0.4936(3) 0.0505(15) Uani 1 1 d . . . C27 C 0.5946(5) 0.0078(5) 0.4375(3) 0.0624(17) Uani 1 1 d U . . H27 H 0.6335 -0.0544 0.4333 0.075 Uiso 1 1 calc R . . C28 C 0.4906(5) 0.0248(5) 0.3919(3) 0.0623(17) Uani 1 1 d U . . H28 H 0.4583 -0.0252 0.3564 0.075 Uiso 1 1 calc R . . C29 C 0.4252(6) 0.1189(4) 0.3954(3) 0.0544(16) Uani 1 1 d . . . C30 C 0.3110(6) 0.1414(5) 0.3501(3) 0.075(2) Uani 1 1 d . . . H30 H 0.2744 0.0947 0.3133 0.090 Uiso 1 1 calc R . . C31 C 0.2557(6) 0.2278(6) 0.3594(3) 0.072(2) Uani 1 1 d . . . H31 H 0.1815 0.2436 0.3286 0.087 Uiso 1 1 calc R . . C32 C 0.3113(5) 0.2960(5) 0.4169(3) 0.0544(16) Uani 1 1 d . . . H32 H 0.2710 0.3560 0.4237 0.065 Uiso 1 1 calc R . . C33 C 0.4763(4) 0.1922(4) 0.4506(3) 0.0364(13) Uani 1 1 d . . . C34 C 0.5870(5) 0.1738(4) 0.4997(3) 0.0364(12) Uani 1 1 d . . . N1 N 0.6357(4) 0.2466(3) 0.5528(2) 0.0362(10) Uani 1 1 d . . . N2 N 0.4157(4) 0.2798(3) 0.4612(2) 0.0391(10) Uani 1 1 d . . . O1 O 0.6863(3) 0.4353(2) 0.66542(16) 0.0361(8) Uani 1 1 d . . . O2 O 0.5231(3) 0.5120(3) 0.66686(16) 0.0439(9) Uani 1 1 d . . . O3 O 0.3190(3) 0.3446(2) 0.58304(17) 0.0408(9) Uani 1 1 d . . . O4 O 0.4824(3) 0.2643(3) 0.64551(19) 0.0456(9) Uani 1 1 d . . . O5 O 0.9652(3) 0.4297(3) 0.7854(2) 0.0623(11) Uani 1 1 d . . . O6 O 0.8765(4) 0.6794(3) 1.01624(19) 0.0623(12) Uani 1 1 d . . . O7 O 0.6029(3) 0.4749(2) 0.49752(16) 0.0298(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.03414(14) 0.02064(12) 0.02184(12) 0.00055(9) 0.00784(10) 0.00395(10) C1 0.042(3) 0.021(2) 0.028(3) 0.000(2) 0.009(2) -0.001(2) C2 0.045(3) 0.026(3) 0.021(2) -0.0041(19) 0.011(2) -0.005(2) C3 0.042(3) 0.027(3) 0.029(3) 0.002(2) 0.010(2) 0.001(2) C4 0.043(3) 0.021(3) 0.030(3) -0.003(2) 0.011(3) -0.005(2) C5 0.034(3) 0.037(3) 0.026(3) -0.007(2) 0.012(2) -0.011(2) C6 0.037(3) 0.034(3) 0.034(3) -0.008(2) 0.003(2) -0.002(2) C7 0.038(3) 0.031(3) 0.028(3) -0.002(2) 0.009(2) -0.004(2) C8 0.051(4) 0.027(3) 0.028(3) -0.001(2) 0.020(3) 0.003(2) C9 0.045(3) 0.031(3) 0.035(3) -0.007(2) 0.012(3) -0.004(3) C10 0.036(3) 0.028(3) 0.032(3) -0.003(2) 0.009(2) -0.006(2) C11 0.048(4) 0.045(3) 0.044(3) 0.001(2) 0.013(3) -0.003(3) C12 0.061(4) 0.067(4) 0.060(4) 0.025(3) 0.034(3) 0.003(3) C13 0.066(2) 0.068(2) 0.069(2) 0.0026(10) 0.0206(11) -0.0021(10) C14 0.044(4) 0.073(5) 0.060(4) -0.005(3) -0.001(3) -0.016(3) C15 0.038(3) 0.050(4) 0.041(3) 0.000(3) 0.003(3) -0.010(3) C16 0.039(3) 0.050(4) 0.022(3) -0.001(2) 0.004(2) 0.009(3) C17 0.049(4) 0.035(3) 0.027(3) -0.003(2) -0.006(3) 0.009(3) C18 0.075(5) 0.058(4) 0.043(4) -0.003(3) 0.008(3) 0.018(4) C19 0.071(2) 0.066(2) 0.068(2) -0.0017(10) 0.0188(11) 0.0019(10) C20 0.075(2) 0.071(2) 0.073(2) -0.0003(10) 0.0197(11) -0.0003(10) C21 0.077(5) 0.076(5) 0.052(4) 0.009(3) -0.009(4) -0.018(4) C22 0.056(4) 0.040(3) 0.048(4) 0.002(3) 0.002(3) 0.003(3) C23 0.050(4) 0.041(3) 0.044(3) -0.003(3) 0.010(3) 0.016(3) C24 0.065(4) 0.050(4) 0.064(4) 0.006(3) 0.032(3) 0.022(3) C25 0.075(5) 0.038(4) 0.074(4) 0.002(3) 0.037(4) 0.024(3) C26 0.065(4) 0.038(3) 0.061(4) -0.014(3) 0.037(3) 0.001(3) C27 0.0639(19) 0.0609(19) 0.0631(19) -0.0039(10) 0.0205(11) 0.0016(10) C28 0.0642(19) 0.0613(19) 0.0621(19) -0.0043(10) 0.0208(11) 0.0006(10) C29 0.073(4) 0.046(4) 0.053(4) -0.019(3) 0.034(3) -0.008(3) C30 0.080(5) 0.081(5) 0.055(4) -0.037(4) 0.007(4) -0.015(4) C31 0.053(4) 0.093(6) 0.055(4) -0.022(4) -0.007(4) 0.000(4) C32 0.049(4) 0.055(4) 0.046(3) -0.011(3) -0.004(3) 0.005(3) C33 0.040(3) 0.023(3) 0.043(3) -0.011(2) 0.008(3) -0.003(2) C34 0.054(4) 0.026(3) 0.037(3) -0.005(2) 0.024(3) -0.002(3) N1 0.052(3) 0.022(2) 0.039(3) -0.0007(17) 0.020(2) 0.007(2) N2 0.048(3) 0.036(2) 0.030(2) -0.0072(18) 0.006(2) 0.002(2) O1 0.039(2) 0.038(2) 0.0289(18) -0.0098(14) 0.0077(17) 0.0067(16) O2 0.039(2) 0.053(2) 0.034(2) -0.0149(16) 0.0023(17) 0.0110(18) O3 0.046(2) 0.037(2) 0.042(2) 0.0170(16) 0.0181(18) 0.0071(18) O4 0.043(2) 0.042(2) 0.051(2) 0.0210(17) 0.0122(19) 0.0031(18) O5 0.050(3) 0.073(3) 0.070(3) -0.012(2) 0.028(2) 0.007(2) O6 0.091(3) 0.065(3) 0.030(2) 0.0004(19) 0.017(2) -0.033(2) O7 0.0345(18) 0.0250(17) 0.0323(17) 0.0099(13) 0.0136(15) 0.0087(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 Er1 O7 2.218(3) 3_666 ? Er1 O7 2.250(3) . ? Er1 O4 2.365(3) . ? Er1 O2 2.377(3) . ? Er1 O1 2.433(3) . ? Er1 O3 2.484(3) . ? Er1 N1 2.524(4) . ? Er1 N2 2.529(4) . ? C1 O1 1.248(5) . ? C1 O2 1.257(5) . ? C1 C2 1.509(6) . ? C2 C3 1.381(6) . ? C2 C7 1.392(6) . ? C3 C4 1.406(6) . ? C3 H3 0.9300 . ? C4 C5 1.395(6) . ? C4 C8 1.502(6) 2_656 ? C5 C6 1.379(6) . ? C5 C9 1.512(6) . ? C6 C7 1.399(6) . ? C6 H6 0.9300 . ? C7 C16 1.513(7) . ? C8 O4 1.266(6) . ? C8 O3 1.270(5) . ? C8 C4 1.502(7) 2_646 ? C9 O6 1.214(6) . ? C9 C10 1.482(7) . ? C10 C15 1.371(6) . ? C10 C11 1.387(7) . ? C11 C12 1.400(7) . ? C11 H11 0.9300 . ? C12 C13 1.396(7) . ? C12 H12 0.9300 . ? C13 C14 1.331(8) . ? C13 H13 0.9300 . ? C14 C15 1.359(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O5 1.218(6) . ? C16 C17 1.489(7) . ? C17 C18 1.379(7) . ? C17 C22 1.380(8) . ? C18 C19 1.401(8) . ? C18 H18 0.9300 . ? C19 C20 1.289(9) . ? C19 H19 0.9300 . ? C20 C21 1.388(9) . ? C20 H20 0.9300 . ? C21 C22 1.411(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 N1 1.298(6) . ? C23 C24 1.402(7) . ? C23 H23 0.9300 . ? C24 C25 1.351(7) . ? C24 H24 0.9300 . ? C25 C26 1.399(7) . ? C25 H25 0.9300 . ? C26 C34 1.426(7) . ? C26 C27 1.437(7) . ? C27 C28 1.309(7) . ? C27 H27 0.9300 . ? C28 C29 1.438(8) . ? C28 H28 0.9300 . ? C29 C33 1.410(7) . ? C29 C30 1.414(8) . ? C30 C31 1.318(8) . ? C30 H30 0.9300 . ? C31 C32 1.411(7) . ? C31 H31 0.9300 . ? C32 N2 1.302(6) . ? C32 H32 0.9300 . ? C33 N2 1.375(6) . ? C33 C34 1.400(6) . ? C34 N1 1.376(6) . ? O7 Er1 2.218(3) 3_666 ? 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 O7 Er1 O7 70.70(12) 3_666 . ? O7 Er1 O4 135.25(12) 3_666 . ? O7 Er1 O4 153.24(12) . . ? O7 Er1 O2 85.12(11) 3_666 . ? O7 Er1 O2 108.48(12) . . ? O4 Er1 O2 83.97(13) . . ? O7 Er1 O1 122.85(11) 3_666 . ? O7 Er1 O1 85.01(11) . . ? O4 Er1 O1 83.57(11) . . ? O2 Er1 O1 54.27(11) . . ? O7 Er1 O3 81.60(11) 3_666 . ? O7 Er1 O3 147.78(10) . . ? O4 Er1 O3 54.23(11) . . ? O2 Er1 O3 84.51(12) . . ? O1 Er1 O3 124.86(11) . . ? O7 Er1 N1 139.54(12) 3_666 . ? O7 Er1 N1 79.49(12) . . ? O4 Er1 N1 74.69(13) . . ? O2 Er1 N1 131.10(12) . . ? O1 Er1 N1 79.63(12) . . ? O3 Er1 N1 114.62(12) . . ? O7 Er1 N2 85.34(12) 3_666 . ? O7 Er1 N2 85.87(12) . . ? O4 Er1 N2 89.71(13) . . ? O2 Er1 N2 158.95(13) . . ? O1 Er1 N2 144.91(12) . . ? O3 Er1 N2 75.56(13) . . ? N1 Er1 N2 65.41(13) . . ? O7 Er1 Er1 35.64(8) 3_666 3_666 ? O7 Er1 Er1 35.05(7) . 3_666 ? O4 Er1 Er1 169.58(9) . 3_666 ? O2 Er1 Er1 98.28(9) . 3_666 ? O1 Er1 Er1 106.04(8) . 3_666 ? O3 Er1 Er1 115.69(7) . 3_666 ? N1 Er1 Er1 110.51(9) . 3_666 ? N2 Er1 Er1 84.61(9) . 3_666 ? O1 C1 O2 122.3(4) . . ? O1 C1 C2 119.8(4) . . ? O2 C1 C2 117.9(4) . . ? C3 C2 C7 119.8(4) . . ? C3 C2 C1 118.5(4) . . ? C7 C2 C1 121.7(4) . . ? C2 C3 C4 121.2(5) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 C8 121.9(4) . 2_656 ? C3 C4 C8 118.5(4) . 2_656 ? C6 C5 C4 118.7(4) . . ? C6 C5 C9 116.7(4) . . ? C4 C5 C9 124.5(4) . . ? C5 C6 C7 122.5(5) . . ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C2 C7 C6 118.4(4) . . ? C2 C7 C16 125.8(4) . . ? C6 C7 C16 115.8(4) . . ? O4 C8 O3 121.5(4) . . ? O4 C8 C4 117.9(4) . 2_646 ? O3 C8 C4 120.5(5) . 2_646 ? O6 C9 C10 122.4(4) . . ? O6 C9 C5 119.5(4) . . ? C10 C9 C5 117.7(4) . . ? C15 C10 C11 119.0(5) . . ? C15 C10 C9 120.5(4) . . ? C11 C10 C9 120.5(4) . . ? C10 C11 C12 119.7(5) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 118.4(5) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C14 C13 C12 120.7(6) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 121.0(6) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C10 121.1(5) . . ? C14 C15 H15 119.5 . . ? C10 C15 H15 119.5 . . ? O5 C16 C17 121.2(5) . . ? O5 C16 C7 119.9(5) . . ? C17 C16 C7 118.6(4) . . ? C18 C17 C22 118.1(5) . . ? C18 C17 C16 120.3(6) . . ? C22 C17 C16 121.6(5) . . ? C17 C18 C19 119.7(7) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 122.1(7) . . ? C20 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C19 C20 C21 121.2(7) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C22 118.2(7) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? C17 C22 C21 120.7(6) . . ? C17 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? N1 C23 C24 124.2(5) . . ? N1 C23 H23 117.9 . . ? C24 C23 H23 117.9 . . ? C25 C24 C23 119.0(6) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 119.1(5) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C25 C26 C34 119.0(5) . . ? C25 C26 C27 124.1(5) . . ? C34 C26 C27 116.9(6) . . ? C28 C27 C26 122.8(6) . . ? C28 C27 H27 118.6 . . ? C26 C27 H27 118.6 . . ? C27 C28 C29 121.6(6) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C33 C29 C30 117.2(5) . . ? C33 C29 C28 117.6(6) . . ? C30 C29 C28 125.1(5) . . ? C31 C30 C29 120.8(6) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 118.7(6) . . ? C30 C31 H31 120.7 . . ? C32 C31 H31 120.7 . . ? N2 C32 C31 123.9(6) . . ? N2 C32 H32 118.1 . . ? C31 C32 H32 118.1 . . ? N2 C33 C34 117.7(4) . . ? N2 C33 C29 121.2(5) . . ? C34 C33 C29 120.9(5) . . ? N1 C34 C33 120.0(4) . . ? N1 C34 C26 119.8(5) . . ? C33 C34 C26 120.2(5) . . ? C23 N1 C34 118.8(4) . . ? C23 N1 Er1 123.1(3) . . ? C34 N1 Er1 117.6(3) . . ? C32 N2 C33 118.1(4) . . ? C32 N2 Er1 123.0(3) . . ? C33 N2 Er1 118.8(3) . . ? C1 O1 Er1 90.5(3) . . ? C1 O2 Er1 92.9(3) . . ? C8 O3 Er1 89.2(3) . . ? C8 O4 Er1 94.7(3) . . ? Er1 O7 Er1 109.30(12) 3_666 . ? 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 162.9(4) . . . . ? O2 C1 C2 C3 -15.2(7) . . . . ? O1 C1 C2 C7 -15.7(7) . . . . ? O2 C1 C2 C7 166.1(4) . . . . ? C7 C2 C3 C4 2.8(7) . . . . ? C1 C2 C3 C4 -175.9(4) . . . . ? C2 C3 C4 C5 0.1(7) . . . . ? C2 C3 C4 C8 -173.8(4) . . . 2_656 ? C3 C4 C5 C6 -2.4(7) . . . . ? C8 C4 C5 C6 171.3(4) 2_656 . . . ? C3 C4 C5 C9 -179.5(4) . . . . ? C8 C4 C5 C9 -5.8(7) 2_656 . . . ? C4 C5 C6 C7 1.9(7) . . . . ? C9 C5 C6 C7 179.2(4) . . . . ? C3 C2 C7 C6 -3.3(7) . . . . ? C1 C2 C7 C6 175.3(4) . . . . ? C3 C2 C7 C16 174.9(4) . . . . ? C1 C2 C7 C16 -6.4(7) . . . . ? C5 C6 C7 C2 1.0(7) . . . . ? C5 C6 C7 C16 -177.4(4) . . . . ? C6 C5 C9 O6 -83.6(6) . . . . ? C4 C5 C9 O6 93.6(6) . . . . ? C6 C5 C9 C10 89.2(6) . . . . ? C4 C5 C9 C10 -93.7(6) . . . . ? O6 C9 C10 C15 4.6(8) . . . . ? C5 C9 C10 C15 -168.0(5) . . . . ? O6 C9 C10 C11 -176.4(5) . . . . ? C5 C9 C10 C11 11.0(7) . . . . ? C15 C10 C11 C12 -0.4(8) . . . . ? C9 C10 C11 C12 -179.4(5) . . . . ? C10 C11 C12 C13 -2.2(9) . . . . ? C11 C12 C13 C14 3.5(10) . . . . ? C12 C13 C14 C15 -2.3(10) . . . . ? C13 C14 C15 C10 -0.4(10) . . . . ? C11 C10 C15 C14 1.7(8) . . . . ? C9 C10 C15 C14 -179.2(5) . . . . ? C2 C7 C16 O5 121.4(6) . . . . ? C6 C7 C16 O5 -60.4(6) . . . . ? C2 C7 C16 C17 -64.5(6) . . . . ? C6 C7 C16 C17 113.8(5) . . . . ? O5 C16 C17 C18 -11.5(8) . . . . ? C7 C16 C17 C18 174.4(4) . . . . ? O5 C16 C17 C22 165.0(5) . . . . ? C7 C16 C17 C22 -9.1(7) . . . . ? C22 C17 C18 C19 4.0(8) . . . . ? C16 C17 C18 C19 -179.3(5) . . . . ? C17 C18 C19 C20 -2.2(10) . . . . ? C18 C19 C20 C21 -0.3(11) . . . . ? C19 C20 C21 C22 1.0(10) . . . . ? C18 C17 C22 C21 -3.4(8) . . . . ? C16 C17 C22 C21 180.0(4) . . . . ? C20 C21 C22 C17 1.0(8) . . . . ? N1 C23 C24 C25 -2.3(9) . . . . ? C23 C24 C25 C26 1.3(8) . . . . ? C24 C25 C26 C34 -0.5(8) . . . . ? C24 C25 C26 C27 -179.3(6) . . . . ? C25 C26 C27 C28 -179.2(5) . . . . ? C34 C26 C27 C28 2.0(9) . . . . ? C26 C27 C28 C29 -0.3(10) . . . . ? C27 C28 C29 C33 -0.9(9) . . . . ? C27 C28 C29 C30 -177.5(6) . . . . ? C33 C29 C30 C31 0.3(10) . . . . ? C28 C29 C30 C31 176.9(7) . . . . ? C29 C30 C31 C32 -2.0(11) . . . . ? C30 C31 C32 N2 1.3(11) . . . . ? C30 C29 C33 N2 2.2(8) . . . . ? C28 C29 C33 N2 -174.7(5) . . . . ? C30 C29 C33 C34 177.3(5) . . . . ? C28 C29 C33 C34 0.3(8) . . . . ? N2 C33 C34 N1 -5.3(7) . . . . ? C29 C33 C34 N1 179.5(5) . . . . ? N2 C33 C34 C26 176.6(5) . . . . ? C29 C33 C34 C26 1.4(8) . . . . ? C25 C26 C34 N1 0.5(7) . . . . ? C27 C26 C34 N1 179.4(5) . . . . ? C25 C26 C34 C33 178.6(5) . . . . ? C27 C26 C34 C33 -2.5(8) . . . . ? C24 C23 N1 C34 2.3(8) . . . . ? C24 C23 N1 Er1 174.4(4) . . . . ? C33 C34 N1 C23 -179.5(5) . . . . ? C26 C34 N1 C23 -1.4(7) . . . . ? C33 C34 N1 Er1 8.0(6) . . . . ? C26 C34 N1 Er1 -173.9(4) . . . . ? O7 Er1 N1 C23 134.8(4) 3_666 . . . ? O7 Er1 N1 C23 92.1(4) . . . . ? O4 Er1 N1 C23 -80.8(4) . . . . ? O2 Er1 N1 C23 -13.3(5) . . . . ? O1 Er1 N1 C23 5.3(4) . . . . ? O3 Er1 N1 C23 -118.4(4) . . . . ? N2 Er1 N1 C23 -177.6(4) . . . . ? Er1 Er1 N1 C23 108.7(4) 3_666 . . . ? O7 Er1 N1 C34 -53.0(4) 3_666 . . . ? O7 Er1 N1 C34 -95.7(3) . . . . ? O4 Er1 N1 C34 91.4(3) . . . . ? O2 Er1 N1 C34 158.9(3) . . . . ? O1 Er1 N1 C34 177.5(3) . . . . ? O3 Er1 N1 C34 53.8(3) . . . . ? N2 Er1 N1 C34 -5.4(3) . . . . ? Er1 Er1 N1 C34 -79.1(3) 3_666 . . . ? C31 C32 N2 C33 1.1(9) . . . . ? C31 C32 N2 Er1 -176.7(5) . . . . ? C34 C33 N2 C32 -178.1(5) . . . . ? C29 C33 N2 C32 -2.9(8) . . . . ? C34 C33 N2 Er1 -0.1(6) . . . . ? C29 C33 N2 Er1 175.1(4) . . . . ? O7 Er1 N2 C32 -28.0(4) 3_666 . . . ? O7 Er1 N2 C32 -98.9(4) . . . . ? O4 Er1 N2 C32 107.5(4) . . . . ? O2 Er1 N2 C32 35.3(6) . . . . ? O1 Er1 N2 C32 -174.2(4) . . . . ? O3 Er1 N2 C32 54.5(4) . . . . ? N1 Er1 N2 C32 -179.3(5) . . . . ? Er1 Er1 N2 C32 -63.8(4) 3_666 . . . ? O7 Er1 N2 C33 154.1(4) 3_666 . . . ? O7 Er1 N2 C33 83.2(4) . . . . ? O4 Er1 N2 C33 -70.4(4) . . . . ? O2 Er1 N2 C33 -142.6(4) . . . . ? O1 Er1 N2 C33 7.9(5) . . . . ? O3 Er1 N2 C33 -123.4(4) . . . . ? N1 Er1 N2 C33 2.8(3) . . . . ? Er1 Er1 N2 C33 118.3(4) 3_666 . . . ? O2 C1 O1 Er1 -2.5(5) . . . . ? C2 C1 O1 Er1 179.4(4) . . . . ? O7 Er1 O1 C1 55.3(3) 3_666 . . . ? O7 Er1 O1 C1 118.4(3) . . . . ? O4 Er1 O1 C1 -85.8(3) . . . . ? O2 Er1 O1 C1 1.4(3) . . . . ? O3 Er1 O1 C1 -48.5(3) . . . . ? N1 Er1 O1 C1 -161.4(3) . . . . ? N2 Er1 O1 C1 -166.0(3) . . . . ? Er1 Er1 O1 C1 90.1(3) 3_666 . . . ? O1 C1 O2 Er1 2.6(5) . . . . ? C2 C1 O2 Er1 -179.3(4) . . . . ? O7 Er1 O2 C1 -138.4(3) 3_666 . . . ? O7 Er1 O2 C1 -70.7(3) . . . . ? O4 Er1 O2 C1 85.0(3) . . . . ? O1 Er1 O2 C1 -1.4(3) . . . . ? O3 Er1 O2 C1 139.6(3) . . . . ? N1 Er1 O2 C1 21.4(3) . . . . ? N2 Er1 O2 C1 158.2(3) . . . . ? Er1 Er1 O2 C1 -105.2(3) 3_666 . . . ? O4 C8 O3 Er1 6.3(4) . . . . ? C4 C8 O3 Er1 -170.0(4) 2_646 . . . ? O7 Er1 O3 C8 -175.9(3) 3_666 . . . ? O7 Er1 O3 C8 153.5(3) . . . . ? O4 Er1 O3 C8 -3.5(2) . . . . ? O2 Er1 O3 C8 -90.1(3) . . . . ? O1 Er1 O3 C8 -51.5(3) . . . . ? N1 Er1 O3 C8 43.0(3) . . . . ? N2 Er1 O3 C8 96.8(3) . . . . ? Er1 Er1 O3 C8 173.4(2) 3_666 . . . ? O3 C8 O4 Er1 -6.7(5) . . . . ? C4 C8 O4 Er1 169.8(4) 2_646 . . . ? O7 Er1 O4 C8 14.3(4) 3_666 . . . ? O7 Er1 O4 C8 -149.0(3) . . . . ? O2 Er1 O4 C8 91.1(3) . . . . ? O1 Er1 O4 C8 145.8(3) . . . . ? O3 Er1 O4 C8 3.6(3) . . . . ? N1 Er1 O4 C8 -133.3(3) . . . . ? N2 Er1 O4 C8 -68.8(3) . . . . ? Er1 Er1 O4 C8 -11.9(7) 3_666 . . . ? O7 Er1 O7 Er1 0.0 3_666 . . 3_666 ? O4 Er1 O7 Er1 167.6(2) . . . 3_666 ? O2 Er1 O7 Er1 -77.76(15) . . . 3_666 ? O1 Er1 O7 Er1 -127.42(13) . . . 3_666 ? O3 Er1 O7 Er1 32.2(3) . . . 3_666 ? N1 Er1 O7 Er1 152.23(16) . . . 3_666 ? N2 Er1 O7 Er1 86.50(15) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 0.824 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.080 _database_code_depnum_ccdc_archive 'CCDC 890973' ####################################################################### # # 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_13 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C34 H21 N2 O7 Yb' _chemical_formula_sum 'C34 H21 N2 O7 Yb' _chemical_formula_weight 742.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0745(18) _cell_length_b 12.584(2) _cell_length_c 19.537(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.000(7) _cell_angle_gamma 90.00 _cell_volume 2823.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7230 _cell_measurement_theta_min 1.9546 _cell_measurement_theta_max 32.1081 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2400 _exptl_crystal_size_mid 0.2200 _exptl_crystal_size_min 0.1800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 3.368 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6927 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14966 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4368 _reflns_number_gt 3298 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.877 Explanation: This alarm has arisen due to the weak diffraction of the crystal. ; _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^)+(0.0058P)^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 4368 _refine_ls_number_parameters 397 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.49100(2) 0.60100(2) 0.432972(14) 0.02628(12) Uani 1 1 d . . . C1 C 0.3707(6) 0.5046(5) 0.3059(3) 0.0318(16) Uani 1 1 d . . . C2 C 0.3087(6) 0.4522(5) 0.2348(3) 0.0311(16) Uani 1 1 d . . . C3 C 0.1999(6) 0.4835(5) 0.1934(3) 0.0320(16) Uani 1 1 d . . . C4 C 0.1433(6) 0.4259(6) 0.1318(4) 0.0377(17) Uani 1 1 d . . . C5 C 0.8064(6) 0.8376(5) 0.3896(3) 0.0312(16) Uani 1 1 d . . . C6 C 0.6935(6) 0.8095(5) 0.3497(3) 0.0296(15) Uani 1 1 d . . . C7 C 0.6375(6) 0.8666(5) 0.2867(3) 0.0347(17) Uani 1 1 d . . . H7 H 0.5630 0.8467 0.2589 0.042 Uiso 1 1 calc R . . C8 C 0.1348(7) 0.5810(6) 0.2074(4) 0.0409(19) Uani 1 1 d . . . C9 C 0.1816(7) 0.6873(6) 0.2024(4) 0.046(2) Uani 1 1 d . . . C10 C 0.2756(7) 0.7031(6) 0.1777(4) 0.052(2) Uani 1 1 d . . . H10 H 0.3097 0.6448 0.1629 0.062 Uiso 1 1 calc R . . H4 H 0.0675 0.4458 0.1047 0.062 Uiso 1 1 d R . . C11 C 0.3210(9) 0.8041(8) 0.1743(5) 0.073(3) Uani 1 1 d U . . H11 H 0.3845 0.8144 0.1576 0.087 Uiso 1 1 calc R . . C12 C 0.2687(9) 0.8867(8) 0.1964(5) 0.077(3) Uani 1 1 d U . . H12 H 0.3005 0.9541 0.1967 0.092 Uiso 1 1 calc R . . C13 C 0.1718(8) 0.8769(7) 0.2181(5) 0.067(3) Uani 1 1 d U . . H13 H 0.1361 0.9364 0.2301 0.080 Uiso 1 1 calc R . . C14 C 0.1280(8) 0.7754(7) 0.2219(4) 0.058(2) Uani 1 1 d . . . H14 H 0.0631 0.7663 0.2373 0.070 Uiso 1 1 calc R . . C15 C 0.8763(6) 0.7844(6) 0.4594(4) 0.0406(18) Uani 1 1 d . . . C16 C 0.9589(6) 0.6988(5) 0.4532(3) 0.0333(16) Uani 1 1 d . . . C17 C 1.0383(6) 0.6603(6) 0.5133(4) 0.047(2) Uani 1 1 d . . . H17 H 1.0409 0.6886 0.5577 0.056 Uiso 1 1 calc R . . C18 C 1.1141(7) 0.5819(6) 0.5108(5) 0.056(2) Uani 1 1 d U . . H18 H 1.1683 0.5568 0.5526 0.067 Uiso 1 1 calc R . . C19 C 1.1085(8) 0.5414(8) 0.4461(4) 0.070(3) Uani 1 1 d U . . H19 H 1.1592 0.4868 0.4438 0.085 Uiso 1 1 calc R . . C20 C 1.0298(7) 0.5784(7) 0.3824(5) 0.060(2) Uani 1 1 d U . . H20 H 1.0294 0.5507 0.3382 0.073 Uiso 1 1 calc R . . C21 C 0.9528(7) 0.6565(6) 0.3864(4) 0.0451(19) Uani 1 1 d . . . H21 H 0.8971 0.6809 0.3449 0.054 Uiso 1 1 calc R . . C22 C 0.6264(6) 0.7250(5) 0.3752(4) 0.0349(17) Uani 1 1 d . . . C23 C 0.6879(7) 0.7022(6) 0.5825(4) 0.051(2) Uani 1 1 d . . . H23 H 0.7276 0.6419 0.5756 0.061 Uiso 1 1 calc R . . C24 C 0.7446(9) 0.7713(8) 0.6403(5) 0.074(3) Uani 1 1 d . . . H24 H 0.8194 0.7565 0.6702 0.089 Uiso 1 1 calc R . . C25 C 0.6885(10) 0.8568(8) 0.6503(5) 0.079(3) Uani 1 1 d . . . H25 H 0.7240 0.9025 0.6882 0.095 Uiso 1 1 calc R . . C26 C 0.5720(8) 0.8811(6) 0.6032(4) 0.051(2) Uani 1 1 d . . . C27 C 0.5098(8) 0.9741(7) 0.6082(4) 0.064(2) Uani 1 1 d U . . H27 H 0.5422 1.0227 0.6448 0.077 Uiso 1 1 calc R . . C28 C 0.4065(8) 0.9933(7) 0.5619(4) 0.062(2) Uani 1 1 d U . . H28 H 0.3699 1.0574 0.5648 0.074 Uiso 1 1 calc R . . C29 C 0.3486(8) 0.9183(6) 0.5068(4) 0.052(2) Uani 1 1 d . . . C30 C 0.2357(8) 0.9330(6) 0.4575(5) 0.061(3) Uani 1 1 d . . . H30 H 0.1922 0.9927 0.4607 0.073 Uiso 1 1 calc R . . C31 C 0.1920(7) 0.8594(6) 0.4059(4) 0.055(2) Uani 1 1 d . . . H31 H 0.1181 0.8674 0.3731 0.066 Uiso 1 1 calc R . . C32 C 0.2620(6) 0.7695(6) 0.4032(4) 0.0434(19) Uani 1 1 d . . . H32 H 0.2315 0.7201 0.3668 0.052 Uiso 1 1 calc R . . C33 C 0.4117(6) 0.8258(5) 0.5002(4) 0.0359(17) Uani 1 1 d . . . C34 C 0.5245(6) 0.8062(5) 0.5505(4) 0.0353(17) Uani 1 1 d . . . N1 N 0.5823(5) 0.7186(5) 0.5382(3) 0.0380(14) Uani 1 1 d . . . N2 N 0.3637(5) 0.7512(4) 0.4469(3) 0.0330(13) Uani 1 1 d . . . O1 O 0.3147(4) 0.5625(4) 0.3359(2) 0.0395(12) Uani 1 1 d . . . O2 O 0.4794(4) 0.4883(4) 0.3349(2) 0.0463(13) Uani 1 1 d . . . O3 O 0.5155(4) 0.7354(4) 0.3556(3) 0.0440(13) Uani 1 1 d . . . O4 O 0.6794(4) 0.6530(4) 0.4175(2) 0.0393(12) Uani 1 1 d . . . O5 O 0.8730(5) 0.8183(4) 0.5156(3) 0.0593(16) Uani 1 1 d . . . O6 O 0.0368(5) 0.5676(5) 0.2157(3) 0.0647(16) Uani 1 1 d . . . O7 O 0.3982(4) 0.5242(3) 0.5024(2) 0.0342(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.0345(2) 0.02103(18) 0.02393(19) 0.00082(11) 0.01001(16) 0.00403(12) C1 0.045(5) 0.017(4) 0.034(4) -0.002(3) 0.012(4) 0.005(3) C2 0.040(4) 0.025(4) 0.031(4) -0.001(3) 0.014(4) 0.001(3) C3 0.034(4) 0.032(4) 0.029(4) -0.004(3) 0.009(3) -0.003(3) C4 0.034(4) 0.041(5) 0.038(4) 0.002(3) 0.010(4) -0.002(3) C5 0.031(4) 0.037(4) 0.027(4) 0.005(3) 0.012(3) 0.010(3) C6 0.045(4) 0.019(4) 0.028(4) 0.004(3) 0.015(3) 0.004(3) C7 0.044(4) 0.028(4) 0.034(4) 0.001(3) 0.015(4) -0.002(3) C8 0.042(5) 0.055(5) 0.022(4) -0.004(3) 0.004(4) 0.012(4) C9 0.059(5) 0.040(5) 0.027(4) -0.007(3) -0.003(4) 0.008(4) C10 0.049(5) 0.044(5) 0.057(5) 0.000(4) 0.008(5) -0.008(4) C11 0.073(3) 0.072(3) 0.072(3) 0.0005(10) 0.0215(13) -0.0002(10) C12 0.078(3) 0.076(3) 0.076(3) 0.0003(10) 0.0223(13) -0.0003(10) C13 0.068(3) 0.066(3) 0.066(3) -0.0008(10) 0.0195(13) 0.0013(10) C14 0.066(6) 0.061(6) 0.038(5) 0.002(4) 0.003(5) 0.025(5) C15 0.050(5) 0.036(4) 0.038(4) 0.002(3) 0.018(4) 0.004(4) C16 0.032(4) 0.038(4) 0.031(4) -0.002(3) 0.013(4) 0.003(3) C17 0.034(4) 0.056(5) 0.046(5) 0.003(4) 0.007(4) 0.013(4) C18 0.056(2) 0.056(2) 0.056(2) 0.0001(10) 0.0167(12) 0.0009(10) C19 0.070(3) 0.070(3) 0.071(3) -0.0011(10) 0.0219(13) 0.0012(10) C20 0.061(3) 0.061(3) 0.060(3) -0.0014(10) 0.0191(12) 0.0004(10) C21 0.048(5) 0.042(5) 0.046(5) 0.005(4) 0.016(4) 0.010(4) C22 0.048(5) 0.030(4) 0.033(4) -0.003(3) 0.022(4) 0.001(3) C23 0.054(5) 0.043(5) 0.050(5) -0.014(4) 0.006(4) 0.004(4) C24 0.069(7) 0.088(8) 0.050(6) -0.019(5) -0.004(5) 0.001(6) C25 0.107(9) 0.079(8) 0.055(6) -0.044(6) 0.031(6) -0.025(7) C26 0.068(6) 0.035(5) 0.050(5) -0.016(4) 0.020(5) -0.003(4) C27 0.065(3) 0.064(3) 0.064(3) -0.0022(10) 0.0202(12) 0.0005(10) C28 0.063(3) 0.061(3) 0.062(3) -0.0020(10) 0.0195(12) 0.0010(10) C29 0.072(6) 0.042(5) 0.054(5) -0.013(4) 0.038(5) -0.001(4) C30 0.077(7) 0.033(5) 0.086(7) -0.002(4) 0.046(6) 0.020(5) C31 0.045(5) 0.050(5) 0.072(6) -0.005(4) 0.019(5) 0.014(4) C32 0.044(5) 0.041(5) 0.045(5) 0.002(4) 0.013(4) 0.014(4) C33 0.050(5) 0.029(4) 0.036(4) -0.003(3) 0.024(4) -0.004(3) C34 0.041(4) 0.022(4) 0.042(4) -0.008(3) 0.010(4) 0.001(3) N1 0.040(4) 0.038(4) 0.034(3) 0.001(3) 0.009(3) 0.006(3) N2 0.045(4) 0.018(3) 0.040(3) 0.002(2) 0.019(3) 0.005(3) O1 0.042(3) 0.043(3) 0.034(3) -0.016(2) 0.013(3) 0.002(2) O2 0.052(4) 0.049(3) 0.035(3) -0.016(2) 0.009(3) 0.014(3) O3 0.041(3) 0.041(3) 0.051(3) 0.023(2) 0.016(3) 0.006(2) O4 0.043(3) 0.035(3) 0.045(3) 0.018(2) 0.022(3) 0.012(2) O5 0.085(4) 0.062(4) 0.032(3) -0.004(3) 0.019(3) 0.027(3) O6 0.058(4) 0.066(4) 0.076(4) -0.013(3) 0.029(4) 0.006(3) O7 0.035(3) 0.033(3) 0.036(3) 0.008(2) 0.013(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O7 2.196(4) 3_666 ? Yb1 O7 2.229(4) . ? Yb1 O3 2.347(4) . ? Yb1 O2 2.353(4) . ? Yb1 O1 2.422(5) . ? Yb1 O4 2.474(5) . ? Yb1 N1 2.496(6) . ? Yb1 N2 2.504(5) . ? C1 O1 1.255(8) . ? C1 O2 1.275(8) . ? C1 C2 1.512(9) . ? C2 C3 1.370(9) . ? C2 C7 1.388(9) 2_645 ? C3 C4 1.390(9) . ? C3 C8 1.527(9) . ? C4 C5 1.391(9) 2_645 ? C4 H4 0.9385 . ? C5 C6 1.391(9) . ? C5 C4 1.391(9) 2_655 ? C5 C15 1.519(9) . ? C6 C7 1.405(8) . ? C6 C22 1.511(9) . ? C7 C2 1.388(9) 2_655 ? C7 H7 0.9300 . ? C8 O6 1.255(9) . ? C8 C9 1.467(11) . ? C9 C10 1.378(11) . ? C9 C14 1.394(10) . ? C10 C11 1.394(11) . ? C10 H10 0.9300 . ? C11 C12 1.353(13) . ? C11 H11 0.9300 . ? C12 C13 1.368(13) . ? C12 H12 0.9300 . ? C13 C14 1.393(12) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O5 1.190(8) . ? C15 C16 1.498(10) . ? C16 C17 1.355(9) . ? C16 C21 1.390(9) . ? C17 C18 1.357(10) . ? C17 H17 0.9300 . ? C18 C19 1.345(10) . ? C18 H18 0.9300 . ? C19 C20 1.391(11) . ? C19 H19 0.9300 . ? C20 C21 1.372(11) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 O4 1.259(8) . ? C22 O3 1.280(8) . ? C23 N1 1.317(9) . ? C23 C24 1.422(11) . ? C23 H23 0.9300 . ? C24 C25 1.319(13) . ? C24 H24 0.9300 . ? C25 C26 1.456(13) . ? C25 H25 0.9300 . ? C26 C34 1.384(10) . ? C26 C27 1.410(11) . ? C27 C28 1.317(11) . ? C27 H27 0.9300 . ? C28 C29 1.440(11) . ? C28 H28 0.9300 . ? C29 C30 1.417(11) . ? C29 C33 1.419(10) . ? C30 C31 1.350(10) . ? C30 H30 0.9300 . ? C31 C32 1.423(10) . ? C31 H31 0.9300 . ? C32 N2 1.282(8) . ? C32 H32 0.9300 . ? C33 N2 1.388(8) . ? C33 C34 1.433(9) . ? C34 N1 1.365(8) . ? O7 Yb1 2.196(4) 3_666 ? 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 O7 Yb1 O7 70.78(17) 3_666 . ? O7 Yb1 O3 135.36(16) 3_666 . ? O7 Yb1 O3 153.03(16) . . ? O7 Yb1 O2 84.73(17) 3_666 . ? O7 Yb1 O2 108.64(17) . . ? O3 Yb1 O2 84.14(18) . . ? O7 Yb1 O1 122.59(17) 3_666 . ? O7 Yb1 O1 84.53(16) . . ? O3 Yb1 O1 83.97(17) . . ? O2 Yb1 O1 54.90(16) . . ? O7 Yb1 O4 80.81(15) 3_666 . ? O7 Yb1 O4 147.50(15) . . ? O3 Yb1 O4 55.03(15) . . ? O2 Yb1 O4 83.44(17) . . ? O1 Yb1 O4 125.15(15) . . ? O7 Yb1 N1 85.20(18) 3_666 . ? O7 Yb1 N1 86.15(18) . . ? O3 Yb1 N1 89.51(18) . . ? O2 Yb1 N1 158.14(19) . . ? O1 Yb1 N1 145.18(17) . . ? O4 Yb1 N1 75.82(17) . . ? O7 Yb1 N2 139.86(17) 3_666 . ? O7 Yb1 N2 79.62(16) . . ? O3 Yb1 N2 74.33(17) . . ? O2 Yb1 N2 131.27(18) . . ? O1 Yb1 N2 79.38(17) . . ? O4 Yb1 N2 115.61(17) . . ? N1 Yb1 N2 65.95(19) . . ? O7 Yb1 Yb1 35.69(11) 3_666 3_666 ? O7 Yb1 Yb1 35.09(11) . 3_666 ? O3 Yb1 Yb1 169.69(12) . 3_666 ? O2 Yb1 Yb1 98.14(13) . 3_666 ? O1 Yb1 Yb1 105.60(12) . 3_666 ? O4 Yb1 Yb1 115.08(10) . 3_666 ? N1 Yb1 Yb1 84.70(13) . 3_666 ? N2 Yb1 Yb1 110.74(12) . 3_666 ? O1 C1 O2 121.0(6) . . ? O1 C1 C2 119.8(6) . . ? O2 C1 C2 119.2(6) . . ? C3 C2 C7 119.9(6) . 2_645 ? C3 C2 C1 121.9(6) . . ? C7 C2 C1 118.1(6) 2_645 . ? C2 C3 C4 119.1(6) . . ? C2 C3 C8 125.4(6) . . ? C4 C3 C8 115.5(6) . . ? C3 C4 C5 122.2(7) . 2_645 ? C3 C4 H4 118.8 . . ? C5 C4 H4 119.0 2_645 . ? C6 C5 C4 118.6(6) . 2_655 ? C6 C5 C15 124.6(6) . . ? C4 C5 C15 116.7(6) 2_655 . ? C5 C6 C7 119.0(6) . . ? C5 C6 C22 121.8(6) . . ? C7 C6 C22 119.1(6) . . ? C2 C7 C6 121.2(7) 2_655 . ? C2 C7 H7 119.4 2_655 . ? C6 C7 H7 119.4 . . ? O6 C8 C9 122.0(7) . . ? O6 C8 C3 118.3(7) . . ? C9 C8 C3 119.4(7) . . ? C10 C9 C14 118.9(8) . . ? C10 C9 C8 122.1(7) . . ? C14 C9 C8 119.0(8) . . ? C9 C10 C11 121.8(9) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 117.1(10) . . ? C12 C11 H11 121.4 . . ? C10 C11 H11 121.4 . . ? C11 C12 C13 123.9(10) . . ? C11 C12 H12 118.1 . . ? C13 C12 H12 118.1 . . ? C12 C13 C14 118.3(10) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C13 C14 C9 119.9(9) . . ? C13 C14 H14 120.1 . . ? C9 C14 H14 120.1 . . ? O5 C15 C16 123.0(7) . . ? O5 C15 C5 120.1(7) . . ? C16 C15 C5 116.4(6) . . ? C17 C16 C21 119.6(7) . . ? C17 C16 C15 119.9(6) . . ? C21 C16 C15 120.5(6) . . ? C16 C17 C18 122.3(7) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C19 C18 C17 118.0(9) . . ? C19 C18 H18 121.0 . . ? C17 C18 H18 121.0 . . ? C18 C19 C20 122.4(10) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C21 C20 C19 118.5(8) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C20 C21 C16 119.1(7) . . ? C20 C21 H21 120.4 . . ? C16 C21 H21 120.4 . . ? O4 C22 O3 122.8(6) . . ? O4 C22 C6 120.4(6) . . ? O3 C22 C6 116.6(6) . . ? N1 C23 C24 123.9(8) . . ? N1 C23 H23 118.0 . . ? C24 C23 H23 118.0 . . ? C25 C24 C23 118.2(9) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? C24 C25 C26 121.2(8) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C34 C26 C27 120.7(8) . . ? C34 C26 C25 115.2(7) . . ? C27 C26 C25 124.2(8) . . ? C28 C27 C26 121.0(9) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 122.1(9) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C30 C29 C33 118.4(7) . . ? C30 C29 C28 124.5(8) . . ? C33 C29 C28 117.1(8) . . ? C31 C30 C29 119.4(7) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 118.3(8) . . ? C30 C31 H31 120.9 . . ? C32 C31 H31 120.9 . . ? N2 C32 C31 125.1(7) . . ? N2 C32 H32 117.4 . . ? C31 C32 H32 117.4 . . ? N2 C33 C29 120.8(7) . . ? N2 C33 C34 119.0(6) . . ? C29 C33 C34 120.2(7) . . ? N1 C34 C26 124.4(7) . . ? N1 C34 C33 116.6(6) . . ? C26 C34 C33 118.7(7) . . ? C23 N1 C34 117.0(6) . . ? C23 N1 Yb1 122.7(5) . . ? C34 N1 Yb1 120.3(4) . . ? C32 N2 C33 118.1(6) . . ? C32 N2 Yb1 123.8(5) . . ? C33 N2 Yb1 117.6(5) . . ? C1 O1 Yb1 90.7(4) . . ? C1 O2 Yb1 93.4(4) . . ? C22 O3 Yb1 93.6(4) . . ? C22 O4 Yb1 88.3(4) . . ? Yb1 O7 Yb1 109.22(17) 3_666 . ? 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 15.0(10) . . . . ? O2 C1 C2 C3 -165.6(6) . . . . ? O1 C1 C2 C7 -161.8(6) . . . 2_645 ? O2 C1 C2 C7 17.6(9) . . . 2_645 ? C7 C2 C3 C4 2.6(10) 2_645 . . . ? C1 C2 C3 C4 -174.2(6) . . . . ? C7 C2 C3 C8 -175.0(6) 2_645 . . . ? C1 C2 C3 C8 8.2(10) . . . . ? C2 C3 C4 C5 -0.4(10) . . . 2_645 ? C8 C3 C4 C5 177.4(6) . . . 2_645 ? C4 C5 C6 C7 4.2(9) 2_655 . . . ? C15 C5 C6 C7 178.7(6) . . . . ? C4 C5 C6 C22 -171.0(6) 2_655 . . . ? C15 C5 C6 C22 3.6(10) . . . . ? C5 C6 C7 C2 -2.1(10) . . . 2_655 ? C22 C6 C7 C2 173.2(6) . . . 2_655 ? C2 C3 C8 O6 -122.1(8) . . . . ? C4 C3 C8 O6 60.3(9) . . . . ? C2 C3 C8 C9 64.9(9) . . . . ? C4 C3 C8 C9 -112.7(7) . . . . ? O6 C8 C9 C10 -165.3(7) . . . . ? C3 C8 C9 C10 7.4(11) . . . . ? O6 C8 C9 C14 13.3(11) . . . . ? C3 C8 C9 C14 -173.9(6) . . . . ? C14 C9 C10 C11 2.5(12) . . . . ? C8 C9 C10 C11 -178.9(7) . . . . ? C9 C10 C11 C12 -0.1(13) . . . . ? C10 C11 C12 C13 -3.2(15) . . . . ? C11 C12 C13 C14 3.8(15) . . . . ? C12 C13 C14 C9 -1.2(13) . . . . ? C10 C9 C14 C13 -1.9(11) . . . . ? C8 C9 C14 C13 179.5(7) . . . . ? C6 C5 C15 O5 -91.5(10) . . . . ? C4 C5 C15 O5 83.2(9) 2_655 . . . ? C6 C5 C15 C16 96.3(8) . . . . ? C4 C5 C15 C16 -89.1(8) 2_655 . . . ? O5 C15 C16 C17 -3.3(12) . . . . ? C5 C15 C16 C17 168.7(7) . . . . ? O5 C15 C16 C21 175.0(8) . . . . ? C5 C15 C16 C21 -13.0(10) . . . . ? C21 C16 C17 C18 0.8(12) . . . . ? C15 C16 C17 C18 179.1(7) . . . . ? C16 C17 C18 C19 -0.4(13) . . . . ? C17 C18 C19 C20 1.1(14) . . . . ? C18 C19 C20 C21 -2.1(14) . . . . ? C19 C20 C21 C16 2.5(12) . . . . ? C17 C16 C21 C20 -1.9(12) . . . . ? C15 C16 C21 C20 179.9(7) . . . . ? C5 C6 C22 O4 -25.3(9) . . . . ? C7 C6 C22 O4 159.6(6) . . . . ? C5 C6 C22 O3 150.0(6) . . . . ? C7 C6 C22 O3 -25.2(9) . . . . ? N1 C23 C24 C25 0.0(15) . . . . ? C23 C24 C25 C26 -0.7(15) . . . . ? C24 C25 C26 C34 2.8(14) . . . . ? C24 C25 C26 C27 -176.1(10) . . . . ? C34 C26 C27 C28 -1.7(13) . . . . ? C25 C26 C27 C28 177.1(8) . . . . ? C26 C27 C28 C29 3.9(13) . . . . ? C27 C28 C29 C30 177.4(8) . . . . ? C27 C28 C29 C33 -5.4(12) . . . . ? C33 C29 C30 C31 -0.3(11) . . . . ? C28 C29 C30 C31 177.0(8) . . . . ? C29 C30 C31 C32 -0.1(12) . . . . ? C30 C31 C32 N2 1.2(12) . . . . ? C30 C29 C33 N2 -0.4(10) . . . . ? C28 C29 C33 N2 -177.8(6) . . . . ? C30 C29 C33 C34 -177.9(7) . . . . ? C28 C29 C33 C34 4.6(10) . . . . ? C27 C26 C34 N1 174.4(8) . . . . ? C25 C26 C34 N1 -4.5(12) . . . . ? C27 C26 C34 C33 1.1(11) . . . . ? C25 C26 C34 C33 -177.8(7) . . . . ? N2 C33 C34 N1 5.9(9) . . . . ? C29 C33 C34 N1 -176.5(7) . . . . ? N2 C33 C34 C26 179.7(6) . . . . ? C29 C33 C34 C26 -2.7(10) . . . . ? C24 C23 N1 C34 -1.5(12) . . . . ? C24 C23 N1 Yb1 176.2(7) . . . . ? C26 C34 N1 C23 4.0(11) . . . . ? C33 C34 N1 C23 177.4(6) . . . . ? C26 C34 N1 Yb1 -173.8(6) . . . . ? C33 C34 N1 Yb1 -0.3(8) . . . . ? O7 Yb1 N1 C23 28.3(6) 3_666 . . . ? O7 Yb1 N1 C23 99.3(6) . . . . ? O3 Yb1 N1 C23 -107.4(6) . . . . ? O2 Yb1 N1 C23 -34.6(9) . . . . ? O1 Yb1 N1 C23 173.9(5) . . . . ? O4 Yb1 N1 C23 -53.5(6) . . . . ? N2 Yb1 N1 C23 179.6(6) . . . . ? Yb1 Yb1 N1 C23 64.1(6) 3_666 . . . ? O7 Yb1 N1 C34 -154.1(5) 3_666 . . . ? O7 Yb1 N1 C34 -83.1(5) . . . . ? O3 Yb1 N1 C34 70.3(5) . . . . ? O2 Yb1 N1 C34 143.1(5) . . . . ? O1 Yb1 N1 C34 -8.4(7) . . . . ? O4 Yb1 N1 C34 124.2(5) . . . . ? N2 Yb1 N1 C34 -2.8(5) . . . . ? Yb1 Yb1 N1 C34 -118.3(5) 3_666 . . . ? C31 C32 N2 C33 -1.8(11) . . . . ? C31 C32 N2 Yb1 -174.0(6) . . . . ? C29 C33 N2 C32 1.4(9) . . . . ? C34 C33 N2 C32 179.0(6) . . . . ? C29 C33 N2 Yb1 174.0(5) . . . . ? C34 C33 N2 Yb1 -8.4(7) . . . . ? O7 Yb1 N2 C32 -134.4(5) 3_666 . . . ? O7 Yb1 N2 C32 -91.8(6) . . . . ? O3 Yb1 N2 C32 81.2(5) . . . . ? O2 Yb1 N2 C32 14.0(6) . . . . ? O1 Yb1 N2 C32 -5.5(5) . . . . ? O4 Yb1 N2 C32 118.6(5) . . . . ? N1 Yb1 N2 C32 177.8(6) . . . . ? Yb1 Yb1 N2 C32 -108.3(5) 3_666 . . . ? O7 Yb1 N2 C33 53.5(5) 3_666 . . . ? O7 Yb1 N2 C33 96.1(4) . . . . ? O3 Yb1 N2 C33 -91.0(4) . . . . ? O2 Yb1 N2 C33 -158.2(4) . . . . ? O1 Yb1 N2 C33 -177.6(4) . . . . ? O4 Yb1 N2 C33 -53.6(5) . . . . ? N1 Yb1 N2 C33 5.7(4) . . . . ? Yb1 Yb1 N2 C33 79.6(4) 3_666 . . . ? O2 C1 O1 Yb1 2.3(7) . . . . ? C2 C1 O1 Yb1 -178.3(5) . . . . ? O7 Yb1 O1 C1 -55.7(4) 3_666 . . . ? O7 Yb1 O1 C1 -118.7(4) . . . . ? O3 Yb1 O1 C1 85.8(4) . . . . ? O2 Yb1 O1 C1 -1.3(4) . . . . ? O4 Yb1 O1 C1 47.0(5) . . . . ? N1 Yb1 O1 C1 166.2(4) . . . . ? N2 Yb1 O1 C1 160.9(4) . . . . ? Yb1 Yb1 O1 C1 -90.3(4) 3_666 . . . ? O1 C1 O2 Yb1 -2.3(7) . . . . ? C2 C1 O2 Yb1 178.2(5) . . . . ? O7 Yb1 O2 C1 137.8(4) 3_666 . . . ? O7 Yb1 O2 C1 70.2(4) . . . . ? O3 Yb1 O2 C1 -85.5(4) . . . . ? O1 Yb1 O2 C1 1.3(4) . . . . ? O4 Yb1 O2 C1 -140.8(4) . . . . ? N1 Yb1 O2 C1 -159.3(5) . . . . ? N2 Yb1 O2 C1 -22.3(5) . . . . ? Yb1 Yb1 O2 C1 104.7(4) 3_666 . . . ? O4 C22 O3 Yb1 5.4(7) . . . . ? C6 C22 O3 Yb1 -169.7(5) . . . . ? O7 Yb1 O3 C22 -12.5(5) 3_666 . . . ? O7 Yb1 O3 C22 150.6(4) . . . . ? O2 Yb1 O3 C22 -88.9(4) . . . . ? O1 Yb1 O3 C22 -144.1(4) . . . . ? O4 Yb1 O3 C22 -2.8(4) . . . . ? N1 Yb1 O3 C22 70.1(4) . . . . ? N2 Yb1 O3 C22 135.2(4) . . . . ? Yb1 Yb1 O3 C22 14.4(10) 3_666 . . . ? O3 C22 O4 Yb1 -5.1(6) . . . . ? C6 C22 O4 Yb1 169.8(5) . . . . ? O7 Yb1 O4 C22 176.0(4) 3_666 . . . ? O7 Yb1 O4 C22 -155.0(4) . . . . ? O3 Yb1 O4 C22 2.9(4) . . . . ? O2 Yb1 O4 C22 90.3(4) . . . . ? O1 Yb1 O4 C22 52.4(4) . . . . ? N1 Yb1 O4 C22 -96.7(4) . . . . ? N2 Yb1 O4 C22 -42.6(4) . . . . ? Yb1 Yb1 O4 C22 -173.8(3) 3_666 . . . ? O7 Yb1 O7 Yb1 0.0 3_666 . . 3_666 ? O3 Yb1 O7 Yb1 -167.6(3) . . . 3_666 ? O2 Yb1 O7 Yb1 77.3(2) . . . 3_666 ? O1 Yb1 O7 Yb1 127.3(2) . . . 3_666 ? O4 Yb1 O7 Yb1 -30.5(4) . . . 3_666 ? N1 Yb1 O7 Yb1 -86.3(2) . . . 3_666 ? N2 Yb1 O7 Yb1 -152.5(2) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.877 _refine_diff_density_max 0.952 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.107 _database_code_depnum_ccdc_archive 'CCDC 890974' ####################################################################### # # 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_y _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'C33 H24 O12 Tb' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C33 H22 O11 Tb, H2 O' _chemical_formula_sum 'C33 H24 O12 Tb' _chemical_formula_weight 771.44 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3248(19) _cell_length_b 11.3302(18) _cell_length_c 14.087(3) _cell_angle_alpha 102.938(14) _cell_angle_beta 111.170(17) _cell_angle_gamma 100.561(14) _cell_volume 1433.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3751 _cell_measurement_theta_min 2.9482 _cell_measurement_theta_max 29.4129 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 766 _exptl_absorpt_coefficient_mu 2.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94398 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlis (Oxford Diffraction, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9427 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 26.25 _reflns_number_total 5739 _reflns_number_gt 5190 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0245P)^2^+1.0965P] 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 5739 _refine_ls_number_parameters 415 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 1.008 _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 Tb1 Tb 0.112647(19) 0.063955(17) 0.657762(15) 0.01420(7) Uani 1 1 d . . . C1 C -0.0159(4) 0.2393(4) 0.4954(3) 0.0176(9) Uani 1 1 d . . . C2 C -0.0123(4) 0.3737(4) 0.4975(3) 0.0161(9) Uani 1 1 d . . . C3 C 0.1061(4) 0.4713(4) 0.5765(3) 0.0201(9) Uani 1 1 d . . . H3 H 0.1773 0.4524 0.6287 0.024 Uiso 1 1 calc R . . C4 C -0.1209(4) 0.4037(4) 0.4207(3) 0.0194(9) Uani 1 1 d . . . C5 C -0.2575(4) 0.3065(4) 0.3410(3) 0.0206(9) Uani 1 1 d . . . C6 C -0.2931(5) 0.2791(4) 0.2249(4) 0.0239(10) Uani 1 1 d . . . C7 C -0.1894(5) 0.3215(5) 0.1907(4) 0.0394(13) Uani 1 1 d . . . H7 H -0.0971 0.3719 0.2403 0.047 Uiso 1 1 calc R . . C8 C -0.2234(7) 0.2888(7) 0.0824(5) 0.0548(17) Uani 1 1 d . . . H8 H -0.1527 0.3163 0.0596 0.066 Uiso 1 1 calc R . . C9 C -0.3589(7) 0.2169(7) 0.0083(5) 0.0563(17) Uani 1 1 d . . . H9 H -0.3807 0.1964 -0.0646 0.068 Uiso 1 1 calc R . . C10 C -0.4631(6) 0.1749(6) 0.0416(5) 0.0512(16) Uani 1 1 d . . . H10 H -0.5553 0.1245 -0.0084 0.061 Uiso 1 1 calc R . . C11 C -0.4304(5) 0.2075(5) 0.1488(4) 0.0348(12) Uani 1 1 d . . . H11 H -0.5022 0.1810 0.1709 0.042 Uiso 1 1 calc R . . C12 C 0.2000(4) -0.0066(4) 0.4333(4) 0.0188(9) Uani 1 1 d . . . C13 C 0.3562(4) 0.0020(4) 0.4675(3) 0.0177(9) Uani 1 1 d . . . C14 C 0.4272(4) 0.0185(4) 0.4016(4) 0.0215(9) Uani 1 1 d . . . C15 C 0.4307(4) -0.0158(4) 0.5640(4) 0.0227(10) Uani 1 1 d . . . H15 H 0.3830 -0.0265 0.6076 0.027 Uiso 1 1 calc R . . C16 C 0.3593(5) 0.0396(5) 0.2954(4) 0.0308(12) Uani 1 1 d . . . C17 C 0.2972(5) 0.1464(5) 0.2876(4) 0.0318(12) Uani 1 1 d . . . C18 C 0.3158(6) 0.2371(5) 0.3780(5) 0.0463(15) Uani 1 1 d . . . H18 H 0.3673 0.2320 0.4457 0.056 Uiso 1 1 calc R . . C19 C 0.2560(8) 0.3382(7) 0.3671(6) 0.0679(19) Uani 1 1 d U . . H19 H 0.2675 0.4014 0.4270 0.081 Uiso 1 1 calc R . . C20 C 0.1804(7) 0.3406(7) 0.2656(7) 0.0641(18) Uani 1 1 d U . . H20 H 0.1406 0.4070 0.2580 0.077 Uiso 1 1 calc R . . C21 C 0.1608(7) 0.2527(7) 0.1771(6) 0.0633(19) Uani 1 1 d U . . H21 H 0.1077 0.2576 0.1096 0.076 Uiso 1 1 calc R . . C22 C 0.2201(5) 0.1550(7) 0.1869(5) 0.0547(18) Uani 1 1 d . . . H22 H 0.2088 0.0940 0.1257 0.066 Uiso 1 1 calc R . . C23 C 0.2975(4) 0.2861(4) 0.8189(4) 0.0219(9) Uani 1 1 d . . . C24 C 0.4008(4) 0.3984(4) 0.9108(4) 0.0225(9) Uani 1 1 d . . . C25 C 0.3912(5) 0.4219(4) 1.0091(4) 0.0246(10) Uani 1 1 d . . . H25 H 0.3159 0.3687 1.0145 0.029 Uiso 1 1 calc R . . C26 C 0.5120(4) 0.4801(4) 0.9022(4) 0.0223(9) Uani 1 1 d . . . C27 C 0.5217(5) 0.4633(4) 0.7959(4) 0.0249(10) Uani 1 1 d . . . C28 C 0.6367(5) 0.4141(4) 0.7788(4) 0.0293(11) Uani 1 1 d . . . C29 C 0.6245(6) 0.3694(5) 0.6746(4) 0.0437(14) Uani 1 1 d . . . H29 H 0.5415 0.3665 0.6173 0.052 Uiso 1 1 calc R . . C30 C 0.7331(7) 0.3294(6) 0.6548(5) 0.0570(17) Uani 1 1 d U . . H30 H 0.7219 0.2970 0.5846 0.068 Uiso 1 1 calc R . . C31 C 0.8568(7) 0.3375(6) 0.7385(6) 0.0537(16) Uani 1 1 d U . . H31 H 0.9320 0.3136 0.7256 0.064 Uiso 1 1 calc R . . C32 C 0.8709(7) 0.3806(6) 0.8412(6) 0.0567(16) Uani 1 1 d U . . H32 H 0.9557 0.3855 0.8980 0.068 Uiso 1 1 calc R . . C33 C 0.7610(6) 0.4170(5) 0.8622(5) 0.0415(13) Uani 1 1 d . . . H33 H 0.7707 0.4436 0.9325 0.050 Uiso 1 1 calc R . . O1 O 0.0395(3) 0.2221(3) 0.5853(2) 0.0196(6) Uani 1 1 d . . . O2 O -0.0692(3) 0.1577(3) 0.4061(2) 0.0237(7) Uani 1 1 d . . . O3 O -0.3388(3) 0.2507(3) 0.3715(3) 0.0326(8) Uani 1 1 d . . . O4 O 0.1551(3) 0.0286(3) 0.5045(2) 0.0194(6) Uani 1 1 d . . . O5 O 0.1170(3) -0.0493(3) 0.3364(2) 0.0260(7) Uani 1 1 d . . . O6 O 0.3655(4) -0.0278(4) 0.2185(3) 0.0527(11) Uani 1 1 d . . . O7 O 0.3268(3) 0.2453(3) 0.7416(3) 0.0328(8) Uani 1 1 d . . . O8 O 0.1820(3) 0.2312(3) 0.8209(2) 0.0272(7) Uani 1 1 d . . . O9 O 0.4397(4) 0.4986(4) 0.7281(3) 0.0434(9) Uani 1 1 d . . . O1W O 0.3380(4) 0.0220(3) 0.7625(3) 0.0398(9) Uani 1 1 d . . . H1WA H 0.4252 0.0574 0.7752 0.048 Uiso 1 1 d R . . H1WB H 0.3382 -0.0413 0.7855 0.048 Uiso 1 1 d R . . O2W O 0.0985(4) -0.0344(4) 0.7963(3) 0.0451(10) Uani 1 1 d . . . H2WA H 0.0563 -0.1130 0.7641 0.054 Uiso 1 1 d R . . H2WB H 0.0808 -0.0143 0.8512 0.054 Uiso 1 1 d R . . O3W O 0.9975(6) 0.8584(5) 0.0861(4) 0.0905(17) Uani 1 1 d . . . H3WA H 1.0581 0.8987 0.1505 0.109 Uiso 1 1 d R . . H3WB H 0.9216 0.8167 0.0879 0.109 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 0.01332(12) 0.01168(12) 0.01320(12) 0.00171(9) 0.00286(9) 0.00201(8) C1 0.016(2) 0.014(2) 0.020(2) 0.003(2) 0.0073(18) 0.0015(17) C2 0.018(2) 0.011(2) 0.017(2) 0.0026(18) 0.0063(18) 0.0043(16) C3 0.018(2) 0.016(2) 0.018(2) 0.0048(19) 0.0001(18) 0.0052(17) C4 0.017(2) 0.016(2) 0.018(2) 0.0043(19) 0.0024(18) 0.0019(17) C5 0.022(2) 0.013(2) 0.020(2) 0.003(2) 0.0007(19) 0.0082(18) C6 0.030(3) 0.018(2) 0.021(2) 0.008(2) 0.006(2) 0.0100(19) C7 0.029(3) 0.052(4) 0.024(3) 0.006(3) 0.004(2) 0.004(3) C8 0.054(4) 0.083(5) 0.039(4) 0.024(4) 0.027(3) 0.024(4) C9 0.068(5) 0.073(5) 0.018(3) 0.004(3) 0.010(3) 0.028(4) C10 0.042(3) 0.047(4) 0.028(3) 0.000(3) -0.013(3) -0.001(3) C11 0.028(3) 0.033(3) 0.026(3) 0.005(2) -0.002(2) 0.002(2) C12 0.013(2) 0.016(2) 0.024(3) 0.007(2) 0.0059(19) 0.0013(17) C13 0.016(2) 0.017(2) 0.022(2) 0.0059(19) 0.0098(18) 0.0044(17) C14 0.019(2) 0.023(2) 0.024(2) 0.009(2) 0.0093(19) 0.0061(18) C15 0.016(2) 0.030(3) 0.024(2) 0.010(2) 0.0105(19) 0.0062(19) C16 0.024(3) 0.048(3) 0.030(3) 0.022(3) 0.015(2) 0.013(2) C17 0.022(3) 0.038(3) 0.044(3) 0.023(3) 0.017(2) 0.010(2) C18 0.046(3) 0.035(3) 0.071(4) 0.031(3) 0.028(3) 0.014(3) C19 0.071(4) 0.052(3) 0.086(4) 0.021(3) 0.041(3) 0.015(3) C20 0.045(3) 0.059(4) 0.092(4) 0.040(3) 0.021(3) 0.017(3) C21 0.048(3) 0.066(4) 0.077(4) 0.048(3) 0.013(3) 0.014(3) C22 0.027(3) 0.087(5) 0.058(4) 0.049(4) 0.010(3) 0.017(3) C23 0.016(2) 0.020(2) 0.022(2) 0.003(2) 0.0038(19) 0.0012(18) C24 0.016(2) 0.018(2) 0.020(2) -0.0045(19) 0.0009(18) -0.0005(17) C25 0.018(2) 0.024(2) 0.023(3) 0.004(2) 0.007(2) -0.0031(18) C26 0.018(2) 0.020(2) 0.021(2) -0.001(2) 0.0052(19) 0.0030(18) C27 0.022(2) 0.024(2) 0.021(2) 0.000(2) 0.008(2) 0.0016(19) C28 0.033(3) 0.022(3) 0.032(3) 0.006(2) 0.016(2) 0.002(2) C29 0.051(4) 0.037(3) 0.030(3) -0.004(3) 0.016(3) 0.001(3) C30 0.075(4) 0.051(3) 0.054(3) 0.005(3) 0.045(3) 0.015(3) C31 0.060(3) 0.042(3) 0.073(4) 0.014(3) 0.041(3) 0.023(2) C32 0.052(3) 0.056(3) 0.068(4) 0.020(3) 0.025(3) 0.031(3) C33 0.048(3) 0.045(3) 0.042(3) 0.016(3) 0.024(3) 0.026(3) O1 0.0242(16) 0.0136(15) 0.0168(16) 0.0071(13) 0.0030(13) 0.0053(12) O2 0.0282(17) 0.0125(15) 0.0205(17) 0.0005(14) 0.0029(14) 0.0041(13) O3 0.0262(18) 0.0312(19) 0.0289(19) 0.0114(17) 0.0049(15) -0.0064(15) O4 0.0179(15) 0.0206(16) 0.0239(17) 0.0070(14) 0.0125(13) 0.0075(12) O5 0.0185(16) 0.0328(19) 0.0224(18) 0.0036(16) 0.0075(14) 0.0059(14) O6 0.060(3) 0.081(3) 0.026(2) 0.018(2) 0.019(2) 0.036(2) O7 0.0229(18) 0.032(2) 0.0277(19) -0.0080(16) 0.0090(15) -0.0026(15) O8 0.0247(17) 0.0254(17) 0.0196(17) -0.0026(15) 0.0081(14) -0.0053(14) O9 0.037(2) 0.063(3) 0.028(2) 0.017(2) 0.0082(17) 0.0172(19) O1W 0.0304(19) 0.044(2) 0.046(2) 0.020(2) 0.0115(17) 0.0150(17) O2W 0.061(3) 0.043(2) 0.035(2) 0.020(2) 0.0213(19) 0.013(2) O3W 0.103(4) 0.093(4) 0.070(4) 0.016(3) 0.046(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O4 2.319(3) . ? Tb1 O1 2.363(3) . ? Tb1 O2 2.366(3) 2_556 ? Tb1 O5 2.379(3) 2_556 ? Tb1 O8 2.398(3) . ? Tb1 O7 2.422(3) . ? Tb1 O1W 2.461(3) . ? Tb1 O2W 2.488(3) . ? Tb1 O4 2.696(3) 2_556 ? Tb1 C12 2.891(4) 2_556 ? Tb1 Tb1 3.9597(12) 2_556 ? C1 O2 1.238(5) . ? C1 O1 1.264(5) . ? C1 C2 1.510(5) . ? C2 C3 1.388(6) . ? C2 C4 1.404(5) . ? C3 C4 1.386(6) 2_566 ? C3 H3 0.9300 . ? C4 C3 1.386(6) 2_566 ? C4 C5 1.482(6) . ? C5 O3 1.214(5) . ? C5 C6 1.484(6) . ? C6 C7 1.378(6) . ? C6 C11 1.382(6) . ? C7 C8 1.378(7) . ? C7 H7 0.9300 . ? C8 C9 1.364(8) . ? C8 H8 0.9300 . ? C9 C10 1.371(8) . ? C9 H9 0.9300 . ? C10 C11 1.366(7) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O5 1.240(5) . ? C12 O4 1.266(5) . ? C12 C13 1.484(6) . ? C12 Tb1 2.891(4) 2_556 ? C13 C15 1.380(6) . ? C13 C14 1.397(5) . ? C14 C15 1.377(6) 2_656 ? C14 C16 1.500(6) . ? C15 C14 1.377(6) 2_656 ? C15 H15 0.9300 . ? C16 O6 1.208(6) . ? C16 C17 1.477(7) . ? C17 C18 1.371(8) . ? C17 C22 1.390(7) . ? C18 C19 1.410(8) . ? C18 H18 0.9300 . ? C19 C20 1.369(9) . ? C19 H19 0.9300 . ? C20 C21 1.333(10) . ? C20 H20 0.9300 . ? C21 C22 1.369(9) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O7 1.247(5) . ? C23 O8 1.253(5) . ? C23 C24 1.483(6) . ? C24 C25 1.393(6) . ? C24 C26 1.397(6) . ? C25 C26 1.365(6) 2_667 ? C25 H25 0.9300 . ? C26 C25 1.365(6) 2_667 ? C26 C27 1.509(6) . ? C27 O9 1.225(5) . ? C27 C28 1.472(6) . ? C28 C33 1.380(7) . ? C28 C29 1.392(7) . ? C29 C30 1.377(8) . ? C29 H29 0.9300 . ? C30 C31 1.361(9) . ? C30 H30 0.9300 . ? C31 C32 1.364(9) . ? C31 H31 0.9300 . ? C32 C33 1.379(7) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? O2 Tb1 2.366(3) 2_556 ? O4 Tb1 2.696(3) 2_556 ? O5 Tb1 2.379(3) 2_556 ? O1W H1WA 0.8501 . ? O1W H1WB 0.8501 . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? 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 O1 76.22(10) . . ? O4 Tb1 O2 75.03(10) . 2_556 ? O1 Tb1 O2 136.67(10) . 2_556 ? O4 Tb1 O5 126.04(10) . 2_556 ? O1 Tb1 O5 77.23(10) . 2_556 ? O2 Tb1 O5 94.52(11) 2_556 2_556 ? O4 Tb1 O8 138.91(10) . . ? O1 Tb1 O8 80.46(10) . . ? O2 Tb1 O8 140.58(10) 2_556 . ? O5 Tb1 O8 79.70(11) 2_556 . ? O4 Tb1 O7 87.66(11) . . ? O1 Tb1 O7 74.83(11) . . ? O2 Tb1 O7 134.80(11) 2_556 . ? O5 Tb1 O7 128.34(11) 2_556 . ? O8 Tb1 O7 53.50(10) . . ? O4 Tb1 O1W 92.85(11) . . ? O1 Tb1 O1W 138.96(11) . . ? O2 Tb1 O1W 74.21(11) 2_556 . ? O5 Tb1 O1W 135.78(11) 2_556 . ? O8 Tb1 O1W 83.05(12) . . ? O7 Tb1 O1W 65.17(12) . . ? O4 Tb1 O2W 141.89(11) . . ? O1 Tb1 O2W 140.63(11) . . ? O2 Tb1 O2W 69.19(12) 2_556 . ? O5 Tb1 O2W 70.55(11) 2_556 . ? O8 Tb1 O2W 72.17(12) . . ? O7 Tb1 O2W 108.38(12) . . ? O1W Tb1 O2W 65.44(11) . . ? O4 Tb1 O4 75.94(10) . 2_556 ? O1 Tb1 O4 68.47(9) . 2_556 ? O2 Tb1 O4 73.55(9) 2_556 2_556 ? O5 Tb1 O4 50.70(9) 2_556 2_556 ? O8 Tb1 O4 125.20(10) . 2_556 ? O7 Tb1 O4 142.34(10) . 2_556 ? O1W Tb1 O4 147.62(11) . 2_556 ? O2W Tb1 O4 105.24(10) . 2_556 ? O4 Tb1 C12 101.30(11) . 2_556 ? O1 Tb1 C12 69.61(10) . 2_556 ? O2 Tb1 C12 85.10(11) 2_556 2_556 ? O5 Tb1 C12 24.88(11) 2_556 2_556 ? O8 Tb1 C12 101.59(12) . 2_556 ? O7 Tb1 C12 139.76(12) . 2_556 ? O1W Tb1 C12 151.02(11) . 2_556 ? O2W Tb1 C12 88.51(11) . 2_556 ? O4 Tb1 C12 25.90(10) 2_556 2_556 ? O4 Tb1 Tb1 41.33(7) . 2_556 ? O1 Tb1 Tb1 67.09(7) . 2_556 ? O2 Tb1 Tb1 69.88(7) 2_556 2_556 ? O5 Tb1 Tb1 85.03(8) 2_556 2_556 ? O8 Tb1 Tb1 146.49(8) . 2_556 ? O7 Tb1 Tb1 120.99(8) . 2_556 ? O1W Tb1 Tb1 127.15(9) . 2_556 ? O2W Tb1 Tb1 129.77(9) . 2_556 ? O4 Tb1 Tb1 34.62(6) 2_556 2_556 ? C12 Tb1 Tb1 60.16(9) 2_556 2_556 ? O2 C1 O1 126.6(4) . . ? O2 C1 C2 117.0(3) . . ? O1 C1 C2 116.4(4) . . ? C3 C2 C4 118.7(4) . . ? C3 C2 C1 118.5(3) . . ? C4 C2 C1 122.8(4) . . ? C2 C3 C4 121.6(4) . 2_566 ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 2_566 . ? C3 C4 C2 119.7(4) 2_566 . ? C3 C4 C5 118.3(3) 2_566 . ? C2 C4 C5 121.8(4) . . ? O3 C5 C4 119.7(4) . . ? O3 C5 C6 121.0(4) . . ? C4 C5 C6 119.3(4) . . ? C7 C6 C11 118.5(4) . . ? C7 C6 C5 120.9(4) . . ? C11 C6 C5 120.5(4) . . ? C6 C7 C8 119.7(5) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 121.1(5) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.7(5) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 119.6(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C6 121.4(5) . . ? C10 C11 H11 119.3 . . ? C6 C11 H11 119.3 . . ? O5 C12 O4 121.9(4) . . ? O5 C12 C13 119.3(4) . . ? O4 C12 C13 118.7(4) . . ? O5 C12 Tb1 53.8(2) . 2_556 ? O4 C12 Tb1 68.4(2) . 2_556 ? C13 C12 Tb1 170.5(3) . 2_556 ? C15 C13 C14 119.0(4) . . ? C15 C13 C12 118.8(3) . . ? C14 C13 C12 122.0(4) . . ? C15 C14 C13 118.2(4) 2_656 . ? C15 C14 C16 117.4(4) 2_656 . ? C13 C14 C16 124.4(4) . . ? C14 C15 C13 122.8(4) 2_656 . ? C14 C15 H15 118.6 2_656 . ? C13 C15 H15 118.6 . . ? O6 C16 C17 121.2(4) . . ? O6 C16 C14 118.1(4) . . ? C17 C16 C14 120.5(5) . . ? C18 C17 C22 119.9(5) . . ? C18 C17 C16 121.0(4) . . ? C22 C17 C16 119.1(6) . . ? C17 C18 C19 119.2(6) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 118.0(7) . . ? C20 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? C21 C20 C19 123.5(7) . . ? C21 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? C20 C21 C22 119.0(6) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C21 C22 C17 120.4(7) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? O7 C23 O8 120.4(4) . . ? O7 C23 C24 120.3(4) . . ? O8 C23 C24 119.3(4) . . ? C25 C24 C26 118.6(4) . . ? C25 C24 C23 120.1(4) . . ? C26 C24 C23 121.2(4) . . ? C26 C25 C24 122.6(4) 2_667 . ? C26 C25 H25 118.7 2_667 . ? C24 C25 H25 118.7 . . ? C25 C26 C24 118.7(4) 2_667 . ? C25 C26 C27 120.6(4) 2_667 . ? C24 C26 C27 120.6(4) . . ? O9 C27 C28 121.2(4) . . ? O9 C27 C26 119.2(4) . . ? C28 C27 C26 119.4(4) . . ? C33 C28 C29 118.1(5) . . ? C33 C28 C27 122.9(5) . . ? C29 C28 C27 118.9(5) . . ? C30 C29 C28 121.2(6) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C31 C30 C29 119.6(6) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C32 C31 C30 120.1(6) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 120.9(6) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C28 120.0(5) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C1 O1 Tb1 139.9(3) . . ? C1 O2 Tb1 135.6(2) . 2_556 ? C12 O4 Tb1 164.6(3) . . ? C12 O4 Tb1 85.7(2) . 2_556 ? Tb1 O4 Tb1 104.06(10) . 2_556 ? C12 O5 Tb1 101.3(3) . 2_556 ? C23 O7 Tb1 92.5(3) . . ? C23 O8 Tb1 93.5(3) . . ? Tb1 O1W H1WA 129.5 . . ? Tb1 O1W H1WB 122.6 . . ? H1WA O1W H1WB 107.4 . . ? Tb1 O2W H2WA 107.0 . . ? Tb1 O2W H2WB 135.8 . . ? H2WA O2W H2WB 107.4 . . ? H3WA O3W H3WB 107.6 . . ? 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 O2 C1 C2 C3 -143.8(4) . . . . ? O1 C1 C2 C3 34.4(5) . . . . ? O2 C1 C2 C4 33.7(6) . . . . ? O1 C1 C2 C4 -148.1(4) . . . . ? C4 C2 C3 C4 -1.6(7) . . . 2_566 ? C1 C2 C3 C4 176.0(4) . . . 2_566 ? C3 C2 C4 C3 1.5(7) . . . 2_566 ? C1 C2 C4 C3 -176.0(4) . . . 2_566 ? C3 C2 C4 C5 -173.5(4) . . . . ? C1 C2 C4 C5 9.0(6) . . . . ? C3 C4 C5 O3 -113.6(5) 2_566 . . . ? C2 C4 C5 O3 61.5(6) . . . . ? C3 C4 C5 C6 66.2(5) 2_566 . . . ? C2 C4 C5 C6 -118.7(4) . . . . ? O3 C5 C6 C7 -166.3(5) . . . . ? C4 C5 C6 C7 13.9(6) . . . . ? O3 C5 C6 C11 12.1(6) . . . . ? C4 C5 C6 C11 -167.7(4) . . . . ? C11 C6 C7 C8 -1.9(8) . . . . ? C5 C6 C7 C8 176.5(5) . . . . ? C6 C7 C8 C9 1.2(10) . . . . ? C7 C8 C9 C10 -0.8(10) . . . . ? C8 C9 C10 C11 1.1(10) . . . . ? C9 C10 C11 C6 -2.0(9) . . . . ? C7 C6 C11 C10 2.4(8) . . . . ? C5 C6 C11 C10 -176.1(5) . . . . ? O5 C12 C13 C15 -146.5(4) . . . . ? O4 C12 C13 C15 32.7(6) . . . . ? Tb1 C12 C13 C15 -104.6(16) 2_556 . . . ? O5 C12 C13 C14 28.8(6) . . . . ? O4 C12 C13 C14 -152.0(4) . . . . ? Tb1 C12 C13 C14 70.8(17) 2_556 . . . ? C15 C13 C14 C15 0.2(7) . . . 2_656 ? C12 C13 C14 C15 -175.1(4) . . . 2_656 ? C15 C13 C14 C16 -179.6(4) . . . . ? C12 C13 C14 C16 5.1(7) . . . . ? C14 C13 C15 C14 -0.3(8) . . . 2_656 ? C12 C13 C15 C14 175.2(4) . . . 2_656 ? C15 C14 C16 O6 52.2(7) 2_656 . . . ? C13 C14 C16 O6 -127.9(5) . . . . ? C15 C14 C16 C17 -122.9(5) 2_656 . . . ? C13 C14 C16 C17 56.9(6) . . . . ? O6 C16 C17 C18 -167.0(5) . . . . ? C14 C16 C17 C18 8.0(7) . . . . ? O6 C16 C17 C22 12.4(7) . . . . ? C14 C16 C17 C22 -172.6(4) . . . . ? C22 C17 C18 C19 0.0(7) . . . . ? C16 C17 C18 C19 179.4(5) . . . . ? C17 C18 C19 C20 0.5(8) . . . . ? C18 C19 C20 C21 -0.1(10) . . . . ? C19 C20 C21 C22 -0.7(10) . . . . ? C20 C21 C22 C17 1.2(9) . . . . ? C18 C17 C22 C21 -0.9(8) . . . . ? C16 C17 C22 C21 179.7(5) . . . . ? O7 C23 C24 C25 -160.8(4) . . . . ? O8 C23 C24 C25 17.7(6) . . . . ? O7 C23 C24 C26 17.0(7) . . . . ? O8 C23 C24 C26 -164.5(4) . . . . ? C26 C24 C25 C26 -1.4(7) . . . 2_667 ? C23 C24 C25 C26 176.4(4) . . . 2_667 ? C25 C24 C26 C25 1.4(7) . . . 2_667 ? C23 C24 C26 C25 -176.5(4) . . . 2_667 ? C25 C24 C26 C27 -176.4(4) . . . . ? C23 C24 C26 C27 5.7(6) . . . . ? C25 C26 C27 O9 -100.5(5) 2_667 . . . ? C24 C26 C27 O9 77.3(6) . . . . ? C25 C26 C27 C28 74.7(6) 2_667 . . . ? C24 C26 C27 C28 -107.5(5) . . . . ? O9 C27 C28 C33 155.4(5) . . . . ? C26 C27 C28 C33 -19.7(7) . . . . ? O9 C27 C28 C29 -20.6(7) . . . . ? C26 C27 C28 C29 164.2(4) . . . . ? C33 C28 C29 C30 -0.1(8) . . . . ? C27 C28 C29 C30 176.1(5) . . . . ? C28 C29 C30 C31 -2.2(9) . . . . ? C29 C30 C31 C32 2.4(10) . . . . ? C30 C31 C32 C33 -0.3(10) . . . . ? C31 C32 C33 C28 -2.1(9) . . . . ? C29 C28 C33 C32 2.2(8) . . . . ? C27 C28 C33 C32 -173.8(5) . . . . ? O2 C1 O1 Tb1 9.9(7) . . . . ? C2 C1 O1 Tb1 -168.1(3) . . . . ? O4 Tb1 O1 C1 32.3(4) . . . . ? O2 Tb1 O1 C1 -17.4(4) 2_556 . . . ? O5 Tb1 O1 C1 -100.3(4) 2_556 . . . ? O8 Tb1 O1 C1 178.2(4) . . . . ? O7 Tb1 O1 C1 123.6(4) . . . . ? O1W Tb1 O1 C1 110.5(4) . . . . ? O2W Tb1 O1 C1 -135.8(4) . . . . ? O4 Tb1 O1 C1 -47.8(4) 2_556 . . . ? C12 Tb1 O1 C1 -75.6(4) 2_556 . . . ? Tb1 Tb1 O1 C1 -10.4(4) 2_556 . . . ? O1 C1 O2 Tb1 2.8(7) . . . 2_556 ? C2 C1 O2 Tb1 -179.1(2) . . . 2_556 ? O5 C12 O4 Tb1 136.2(9) . . . . ? C13 C12 O4 Tb1 -43.0(12) . . . . ? Tb1 C12 O4 Tb1 130.1(10) 2_556 . . . ? O5 C12 O4 Tb1 6.1(4) . . . 2_556 ? C13 C12 O4 Tb1 -173.1(3) . . . 2_556 ? O1 Tb1 O4 C12 161.0(10) . . . . ? O2 Tb1 O4 C12 -51.7(10) 2_556 . . . ? O5 Tb1 O4 C12 -136.4(10) 2_556 . . . ? O8 Tb1 O4 C12 103.8(10) . . . . ? O7 Tb1 O4 C12 86.1(10) . . . . ? O1W Tb1 O4 C12 21.1(10) . . . . ? O2W Tb1 O4 C12 -31.2(11) . . . . ? O4 Tb1 O4 C12 -128.1(11) 2_556 . . . ? C12 Tb1 O4 C12 -133.5(10) 2_556 . . . ? Tb1 Tb1 O4 C12 -128.1(11) 2_556 . . . ? O1 Tb1 O4 Tb1 -70.84(10) . . . 2_556 ? O2 Tb1 O4 Tb1 76.39(11) 2_556 . . 2_556 ? O5 Tb1 O4 Tb1 -8.23(16) 2_556 . . 2_556 ? O8 Tb1 O4 Tb1 -128.10(14) . . . 2_556 ? O7 Tb1 O4 Tb1 -145.79(11) . . . 2_556 ? O1W Tb1 O4 Tb1 149.22(11) . . . 2_556 ? O2W Tb1 O4 Tb1 96.88(17) . . . 2_556 ? O4 Tb1 O4 Tb1 0.0 2_556 . . 2_556 ? C12 Tb1 O4 Tb1 -5.35(12) 2_556 . . 2_556 ? O4 C12 O5 Tb1 -7.0(4) . . . 2_556 ? C13 C12 O5 Tb1 172.1(3) . . . 2_556 ? O8 C23 O7 Tb1 -3.8(4) . . . . ? C24 C23 O7 Tb1 174.7(3) . . . . ? O4 Tb1 O7 C23 167.8(3) . . . . ? O1 Tb1 O7 C23 91.4(3) . . . . ? O2 Tb1 O7 C23 -126.1(3) 2_556 . . . ? O5 Tb1 O7 C23 31.8(3) 2_556 . . . ? O8 Tb1 O7 C23 2.1(2) . . . . ? O1W Tb1 O7 C23 -98.0(3) . . . . ? O2W Tb1 O7 C23 -47.5(3) . . . . ? O4 Tb1 O7 C23 104.6(3) 2_556 . . . ? C12 Tb1 O7 C23 63.0(3) 2_556 . . . ? Tb1 Tb1 O7 C23 142.1(2) 2_556 . . . ? O7 C23 O8 Tb1 3.9(4) . . . . ? C24 C23 O8 Tb1 -174.6(3) . . . . ? O4 Tb1 O8 C23 -24.3(3) . . . . ? O1 Tb1 O8 C23 -80.3(2) . . . . ? O2 Tb1 O8 C23 116.6(3) 2_556 . . . ? O5 Tb1 O8 C23 -158.9(3) 2_556 . . . ? O7 Tb1 O8 C23 -2.1(2) . . . . ? O1W Tb1 O8 C23 62.0(2) . . . . ? O2W Tb1 O8 C23 128.4(3) . . . . ? O4 Tb1 O8 C23 -135.2(2) 2_556 . . . ? C12 Tb1 O8 C23 -147.0(2) 2_556 . . . ? Tb1 Tb1 O8 C23 -94.6(3) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.071 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.133 _database_code_depnum_ccdc_archive 'CCDC 936978'