# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jaume Veciana' _publ_contact_author_email VECIANAJ@ICMAB.ES _publ_section_title ; A three-dimensional lanthanide-organic radical open-framework ; loop_ _publ_author_name 'Jaume Veciana' 'Angela Datcu' 'Inhar Imaz' 'Daniel Maspoch' 'Nans Roques' 'Concepcio Rovira' ; J.-P.Sutter ; # Attachment 'B802196A Veciana_CIF1corr3.cif' data_nr121a_2 _database_code_depnum_ccdc_archive 'CCDC 676448' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H19 Cl12 N3 O9 Tb' _chemical_formula_sum 'C31 H19 Cl12 N3 O9 Tb' _chemical_formula_weight 1161.82 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' 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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I41/a _symmetry_space_group_name_Hall -I4ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 27.920(5) _cell_length_b 27.920(5) _cell_length_c 46.940(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 36591(10) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description octahedra _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9072.0 _exptl_absorpt_coefficient_mu 3.290 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.987 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device_type ADSCq210rCCD-HUBER _diffrn_measurement_method 'f\ scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85111 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 19.77 _reflns_number_total 3083 _reflns_number_gt 3083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CCD Server Software Huber' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'shelxl-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 ( Farrugia, 1997) and Diamond 2.1e' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+93.7159P] 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 SHELXL _refine_ls_extinction_coef 0.00039(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6422 _refine_ls_number_parameters 510 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.262 _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 C1 C 1.2312(4) 0.0855(5) 0.2088(2) 0.083(3) Uani 1 1 d . . . C2 C 1.1826(3) 0.0805(3) 0.1947(2) 0.064(2) Uani 1 1 d . . . C3 C 1.1443(4) 0.0594(3) 0.20894(18) 0.063(2) Uani 1 1 d . . . C4 C 1.1006(3) 0.0555(3) 0.1966(2) 0.061(2) Uani 1 1 d . . . C5 C 1.0918(3) 0.0721(3) 0.16844(18) 0.051(2) Uani 1 1 d . . . C6 C 1.1304(3) 0.0914(3) 0.15375(16) 0.050(2) Uani 1 1 d . . . C7 C 1.1748(3) 0.0958(3) 0.1672(2) 0.064(2) Uani 1 1 d . . . C8 C 1.0432(3) 0.0693(3) 0.15557(17) 0.072(3) Uani 1 1 d . . . C9 C 0.8749(3) 0.1307(3) 0.2189(2) 0.058(2) Uani 1 1 d . . . C10 C 0.9180(3) 0.1155(3) 0.20166(16) 0.052(2) Uani 1 1 d . . . C11 C 0.9201(3) 0.0713(3) 0.18853(17) 0.056(2) Uani 1 1 d . . . C12 C 0.9595(3) 0.0564(3) 0.17405(15) 0.052(2) Uani 1 1 d . . . C13 C 1.0013(3) 0.0853(3) 0.17191(15) 0.053(2) Uani 1 1 d . . . C14 C 0.9987(3) 0.1297(3) 0.18555(16) 0.052(2) Uani 1 1 d . . . C15 C 0.9572(3) 0.1443(3) 0.19966(14) 0.049(2) Uani 1 1 d . . . C16 C 1.0065(4) 0.0001(3) 0.04170(19) 0.056(2) Uani 1 1 d . . . C17 C 1.0177(3) 0.0183(3) 0.07128(17) 0.053(2) Uani 1 1 d . . . C18 C 1.0001(3) 0.0622(3) 0.07994(16) 0.051(2) Uani 1 1 d . . . C19 C 1.0097(3) 0.0803(3) 0.10660(19) 0.053(2) Uani 1 1 d . . . C20 C 1.0360(3) 0.0529(3) 0.12656(17) 0.054(2) Uani 1 1 d . . . C21 C 1.0539(3) 0.0076(3) 0.11707(18) 0.057(2) Uani 1 1 d . . . C22 C 1.0443(3) -0.0090(3) 0.09012(19) 0.050(2) Uani 1 1 d . . . C23 C 0.8561(4) 0.2656(5) 0.25978(16) 0.069(3) Uani 1 1 d . . . H23 H 0.8258 0.2779 0.2560 0.083 Uiso 1 1 calc R . . C24 C 0.9384(4) 0.2818(4) 0.2712(2) 0.098(3) Uani 1 1 d . . . H24A H 0.9480 0.2973 0.2885 0.148 Uiso 1 1 calc R . . H24B H 0.9601 0.2904 0.2562 0.148 Uiso 1 1 calc R . . H24C H 0.9390 0.2477 0.2738 0.148 Uiso 1 1 calc R . . C25 C 0.8797(4) 0.3465(3) 0.2605(2) 0.085(3) Uani 1 1 d . . . H25A H 0.8992 0.3598 0.2457 0.127 Uiso 1 1 calc R . . H25B H 0.8862 0.3629 0.2781 0.127 Uiso 1 1 calc R . . H25C H 0.8465 0.3504 0.2557 0.127 Uiso 1 1 calc R . . C26 C 0.7661(3) 0.0967(4) 0.1990(3) 0.089(3) Uani 1 1 d . . . H26 H 0.7770 0.1220 0.1879 0.106 Uiso 1 1 calc R . . C27 C 0.7501(4) 0.0548(4) 0.1541(2) 0.107(3) Uani 1 1 d . . . H27A H 0.7674 0.0267 0.1483 0.160 Uiso 1 1 calc R . . H27B H 0.7649 0.0827 0.1460 0.160 Uiso 1 1 calc R . . H27C H 0.7176 0.0526 0.1477 0.160 Uiso 1 1 calc R . . C28 C 0.7410(6) 0.0134(5) 0.2014(3) 0.166(6) Uani 1 1 d . . . H28A H 0.7077 0.0052 0.1997 0.250 Uiso 1 1 calc R . . H28B H 0.7486 0.0187 0.2211 0.250 Uiso 1 1 calc R . . H28C H 0.7603 -0.0122 0.1941 0.250 Uiso 1 1 calc R . . C29 C 0.8376(5) 0.1455(11) 0.3177(4) 0.277(17) Uani 1 1 d . . . H29 H 0.8318 0.1783 0.3180 0.332 Uiso 1 1 calc R . . C30 C 0.8461(12) 0.0785(7) 0.3445(6) 0.343(18) Uani 1 1 d D . . H30D H 0.8407 0.0654 0.3259 0.515 Uiso 0.50 1 calc PR . . H30E H 0.8217 0.0674 0.3573 0.515 Uiso 0.50 1 calc PR . . H30F H 0.8769 0.0685 0.3513 0.515 Uiso 0.50 1 calc PR . . C31 C 0.8441(7) 0.1455(12) 0.3716(6) 0.60(5) Uani 1 1 d D . . H31D H 0.8352 0.1784 0.3743 0.902 Uiso 0.50 1 calc PR . . H31E H 0.8755 0.1403 0.3794 0.902 Uiso 0.50 1 calc PR . . H31F H 0.8215 0.1252 0.3812 0.902 Uiso 0.50 1 calc PR . . N1 N 0.8903(3) 0.2968(3) 0.26370(14) 0.067(2) Uani 1 1 d . . . N2A N 0.7509(3) 0.0583(4) 0.1847(2) 0.100(3) Uani 1 1 d . . . N3 N 0.8444(3) 0.1349(6) 0.3429(3) 0.149(4) Uani 1 1 d D . . O1 O 1.2379(2) 0.1230(2) 0.22275(13) 0.0814(18) Uani 1 1 d . . . O2 O 1.2587(3) 0.0518(3) 0.20564(16) 0.107(2) Uani 1 1 d . . . O3 O 0.8476(2) 0.1614(2) 0.20897(11) 0.0591(14) Uani 1 1 d . . . O4 O 0.8694(2) 0.1135(2) 0.24291(14) 0.0716(17) Uani 1 1 d . . . O5 O 0.9673(2) -0.0203(2) 0.03836(11) 0.0659(15) Uani 1 1 d . . . O6 O 1.0378(2) 0.00644(18) 0.02316(12) 0.0599(14) Uani 1 1 d . . . O7 O 0.85996(19) 0.2204(2) 0.26065(10) 0.0641(15) Uani 1 1 d . . . H7 H 0.8907 0.2089 0.2640 0.077 Uiso 1 1 calc R . . O8 O 0.7676(2) 0.1031(2) 0.22463(17) 0.090(2) Uani 1 1 d . . . O9 O 0.8352(2) 0.1365(2) 0.29677(14) 0.0810(19) Uani 1 1 d . . . Cl1 Cl 1.15409(10) 0.03809(9) 0.24304(5) 0.0901(8) Uani 1 1 d . . . Cl2 Cl 1.05539(8) 0.02616(9) 0.21507(5) 0.0801(7) Uani 1 1 d . . . Cl3 Cl 1.12325(7) 0.11428(7) 0.12020(4) 0.0624(6) Uani 1 1 d . . . Cl4 Cl 1.22187(7) 0.12247(9) 0.14892(5) 0.0798(7) Uani 1 1 d . . . Cl5 Cl 0.86995(8) 0.03411(7) 0.19123(5) 0.0721(7) Uani 1 1 d . . . Cl6 Cl 0.96032(7) -0.00135(7) 0.16019(5) 0.0702(7) Uani 1 1 d . . . Cl7 Cl 1.04658(7) 0.16874(7) 0.18288(4) 0.0616(6) Uani 1 1 d . . . Cl8 Cl 0.95622(7) 0.20114(7) 0.21497(4) 0.0677(7) Uani 1 1 d . . . Cl9 Cl 0.96514(7) 0.09578(7) 0.05689(4) 0.0607(6) Uani 1 1 d . . . Cl10 Cl 0.99255(7) 0.13720(7) 0.11534(4) 0.0602(6) Uani 1 1 d . . . Cl11 Cl 1.08478(8) -0.02855(8) 0.14036(4) 0.0722(7) Uani 1 1 d . . . Cl12 Cl 1.06481(8) -0.06390(7) 0.07896(4) 0.0716(7) Uani 1 1 d . . . Tb1 Tb 0.800274(15) 0.160818(14) 0.254870(8) 0.0601(3) 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 C1 0.065(7) 0.083(8) 0.101(8) 0.015(7) -0.025(6) 0.013(7) C2 0.069(7) 0.060(6) 0.062(7) -0.004(5) -0.023(6) 0.007(5) C3 0.075(7) 0.056(5) 0.058(6) -0.001(4) -0.034(6) 0.003(5) C4 0.073(7) 0.058(5) 0.050(7) -0.018(4) 0.001(5) -0.005(5) C5 0.057(6) 0.056(5) 0.041(6) -0.022(4) -0.007(5) 0.006(5) C6 0.042(5) 0.059(5) 0.050(6) -0.010(4) -0.004(5) 0.000(4) C7 0.060(6) 0.060(5) 0.070(7) -0.009(5) -0.002(5) -0.004(5) C8 0.055(6) 0.120(8) 0.040(6) -0.038(5) 0.004(5) 0.000(5) C9 0.071(7) 0.045(5) 0.057(7) 0.001(5) 0.011(6) 0.006(5) C10 0.043(6) 0.064(7) 0.048(5) 0.007(5) 0.022(4) 0.005(6) C11 0.069(7) 0.049(6) 0.049(5) -0.007(4) 0.005(5) 0.011(5) C12 0.065(6) 0.052(5) 0.040(5) -0.019(4) 0.005(4) 0.008(6) C13 0.062(7) 0.065(6) 0.031(5) -0.009(4) -0.005(4) 0.005(6) C14 0.052(6) 0.066(6) 0.039(5) -0.005(4) 0.000(4) -0.010(5) C15 0.066(6) 0.058(5) 0.023(5) -0.004(4) 0.009(4) 0.011(6) C16 0.063(7) 0.059(6) 0.045(7) -0.014(5) 0.009(6) -0.006(5) C17 0.054(5) 0.068(6) 0.036(6) -0.024(5) 0.004(4) -0.015(5) C18 0.059(5) 0.066(6) 0.029(6) -0.021(4) -0.002(4) -0.007(5) C19 0.036(5) 0.068(5) 0.054(6) -0.010(5) 0.000(4) 0.005(4) C20 0.036(5) 0.078(6) 0.047(6) -0.024(5) 0.004(4) -0.009(5) C21 0.044(5) 0.075(6) 0.051(7) -0.006(5) -0.006(4) 0.005(5) C22 0.057(5) 0.056(5) 0.037(6) -0.014(5) -0.003(4) 0.001(4) C23 0.089(8) 0.072(8) 0.045(6) -0.005(5) 0.031(5) 0.009(8) C24 0.088(9) 0.111(8) 0.096(8) -0.016(6) -0.006(6) -0.004(7) C25 0.107(8) 0.064(7) 0.084(7) -0.004(5) 0.030(6) -0.009(6) C26 0.066(7) 0.063(8) 0.137(12) -0.011(8) 0.016(7) -0.011(6) C27 0.128(9) 0.124(9) 0.069(9) -0.012(6) 0.007(6) -0.031(7) C28 0.225(16) 0.158(13) 0.116(11) -0.032(10) 0.064(11) -0.069(12) C29 0.096(10) 0.69(5) 0.049(12) 0.035(18) -0.027(10) 0.047(17) C30 0.47(5) 0.28(3) 0.29(3) 0.04(3) -0.09(3) 0.00(3) C31 0.121(15) 1.45(14) 0.23(3) -0.41(5) -0.001(16) 0.10(4) N1 0.075(6) 0.065(6) 0.062(5) -0.013(4) 0.020(4) -0.022(6) N2A 0.099(6) 0.094(7) 0.106(9) -0.018(6) 0.050(5) -0.038(6) N3 0.079(6) 0.270(15) 0.098(10) 0.010(9) 0.011(6) 0.016(8) O1 0.097(5) 0.077(4) 0.070(4) -0.009(4) -0.033(3) -0.014(4) O2 0.076(5) 0.097(5) 0.148(7) -0.019(5) -0.061(4) 0.013(5) O3 0.064(4) 0.063(4) 0.051(4) -0.007(3) 0.020(3) 0.007(3) O4 0.092(4) 0.067(4) 0.056(4) 0.017(3) 0.029(3) 0.011(3) O5 0.072(4) 0.076(4) 0.050(4) -0.027(3) 0.004(3) -0.010(4) O6 0.067(4) 0.071(4) 0.043(4) -0.024(3) -0.005(3) 0.004(3) O7 0.066(4) 0.072(5) 0.054(4) -0.007(3) 0.021(3) 0.001(4) O8 0.104(5) 0.093(5) 0.074(5) -0.018(4) 0.043(4) -0.021(4) O9 0.099(5) 0.100(5) 0.044(5) 0.008(3) 0.012(4) 0.012(4) Cl1 0.115(2) 0.0917(18) 0.0636(17) 0.0102(12) -0.0308(13) 0.0048(16) Cl2 0.0834(16) 0.0989(17) 0.0580(15) 0.0037(12) 0.0026(12) -0.0024(14) Cl3 0.0622(13) 0.0787(14) 0.0464(14) -0.0032(10) -0.0064(10) 0.0053(11) Cl4 0.0633(14) 0.0927(17) 0.0835(17) -0.0003(13) -0.0109(12) -0.0152(13) Cl5 0.0696(15) 0.0604(14) 0.0862(16) -0.0075(11) 0.0253(12) -0.0119(12) Cl6 0.0722(14) 0.0653(14) 0.0730(15) -0.0215(11) 0.0072(11) 0.0056(12) Cl7 0.0584(13) 0.0763(15) 0.0500(13) -0.0122(10) 0.0030(9) -0.0081(12) Cl8 0.0744(15) 0.0620(14) 0.0668(15) -0.0179(11) 0.0141(11) -0.0028(12) Cl9 0.0635(13) 0.0729(14) 0.0458(13) -0.0158(10) -0.0087(10) 0.0106(11) Cl10 0.0655(13) 0.0666(13) 0.0486(13) -0.0235(10) -0.0007(10) 0.0060(11) Cl11 0.0764(15) 0.0876(16) 0.0527(14) -0.0071(11) -0.0089(11) 0.0174(13) Cl12 0.0889(16) 0.0664(14) 0.0594(15) -0.0183(11) -0.0042(11) 0.0165(13) Tb1 0.0709(4) 0.0593(4) 0.0501(4) -0.00125(19) 0.0271(2) 0.0001(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 C1 O2 1.225(11) . ? C1 O1 1.248(12) . ? C1 C2 1.517(13) . ? C2 C7 1.374(11) . ? C2 C3 1.393(12) . ? C3 C4 1.354(11) . ? C3 Cl1 1.730(9) . ? C4 C5 1.423(11) . ? C4 Cl2 1.736(9) . ? C5 C6 1.388(10) . ? C5 C8 1.486(11) . ? C6 C7 1.398(11) . ? C6 Cl3 1.711(8) . ? C7 Cl4 1.739(9) . ? C8 C20 1.450(11) . ? C8 C13 1.468(11) . ? C9 O4 1.237(9) . ? C9 O3 1.237(9) . ? C9 C10 1.509(11) . ? C9 Tb1 2.812(9) . ? C10 C15 1.361(10) . ? C10 C11 1.383(10) . ? C11 C12 1.356(10) . ? C11 Cl5 1.748(8) . ? C12 C13 1.423(10) . ? C12 Cl6 1.740(8) . ? C13 C14 1.399(10) . ? C14 C15 1.396(10) . ? C14 Cl7 1.729(8) . ? C15 Cl8 1.743(8) . ? C16 O5 1.244(9) . ? C16 O6 1.246(9) . ? C16 C17 1.511(11) . ? C17 C18 1.382(10) . ? C17 C22 1.384(10) . ? C18 C19 1.376(10) . ? C18 Cl9 1.733(8) . ? C19 C20 1.414(11) . ? C19 Cl10 1.710(8) . ? C20 C21 1.431(11) . ? C21 C22 1.374(11) . ? C21 Cl11 1.720(8) . ? C22 Cl12 1.718(8) . ? C23 O7 1.270(11) . ? C23 N1 1.305(11) . ? C23 H23 0.9300 . ? C24 N1 1.450(11) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N1 1.426(11) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O8 1.216(13) . ? C26 N2A 1.334(12) . ? C26 H26 0.9300 . ? C27 N2A 1.440(12) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N2A 1.504(15) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O9 1.018(18) . ? C29 N3 1.230(18) . ? C29 H29 0.9300 . ? C30 N3 1.57(3) . ? C30 H30D 0.9600 . ? C30 H30E 0.9600 . ? C30 H30F 0.9600 . ? C31 N3 1.38(2) . ? C31 H31D 0.9600 . ? C31 H31E 0.9600 . ? C31 H31F 0.9600 . ? O1 Tb1 2.291(6) 14 ? O3 Tb1 2.527(5) . ? O4 Tb1 2.405(5) . ? O5 Tb1 2.378(6) 8_554 ? O6 Tb1 2.299(6) 16_645 ? O7 Tb1 2.369(6) . ? O7 H7 0.9300 . ? O8 Tb1 2.333(8) . ? O9 Tb1 2.298(7) . ? Tb1 O1 2.291(6) 14_455 ? Tb1 O6 2.299(6) 15_665 ? Tb1 O5 2.378(6) 3_545 ? 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 C1 O1 127.9(9) . . ? O2 C1 C2 115.8(10) . . ? O1 C1 C2 116.3(10) . . ? C7 C2 C3 117.3(7) . . ? C7 C2 C1 121.7(9) . . ? C3 C2 C1 121.0(9) . . ? C4 C3 C2 121.4(8) . . ? C4 C3 Cl1 120.7(8) . . ? C2 C3 Cl1 118.0(7) . . ? C3 C4 C5 121.8(8) . . ? C3 C4 Cl2 118.7(8) . . ? C5 C4 Cl2 119.4(7) . . ? C6 C5 C4 117.0(7) . . ? C6 C5 C8 121.8(8) . . ? C4 C5 C8 121.2(8) . . ? C5 C6 C7 119.8(7) . . ? C5 C6 Cl3 120.8(6) . . ? C7 C6 Cl3 119.1(7) . . ? C2 C7 C6 122.6(8) . . ? C2 C7 Cl4 118.4(7) . . ? C6 C7 Cl4 119.0(7) . . ? C20 C8 C13 118.4(7) . . ? C20 C8 C5 121.7(7) . . ? C13 C8 C5 119.9(7) . . ? O4 C9 O3 122.3(8) . . ? O4 C9 C10 118.6(9) . . ? O3 C9 C10 119.0(8) . . ? O4 C9 Tb1 58.3(4) . . ? O3 C9 Tb1 64.0(4) . . ? C10 C9 Tb1 174.9(7) . . ? C15 C10 C11 117.4(7) . . ? C15 C10 C9 120.9(8) . . ? C11 C10 C9 121.6(8) . . ? C12 C11 C10 122.1(7) . . ? C12 C11 Cl5 120.3(7) . . ? C10 C11 Cl5 117.6(7) . . ? C11 C12 C13 121.9(7) . . ? C11 C12 Cl6 118.8(7) . . ? C13 C12 Cl6 119.1(7) . . ? C14 C13 C12 115.3(7) . . ? C14 C13 C8 123.4(8) . . ? C12 C13 C8 121.3(8) . . ? C15 C14 C13 121.2(7) . . ? C15 C14 Cl7 119.5(7) . . ? C13 C14 Cl7 119.1(7) . . ? C10 C15 C14 122.0(7) . . ? C10 C15 Cl8 119.7(7) . . ? C14 C15 Cl8 118.3(7) . . ? O5 C16 O6 126.5(8) . . ? O5 C16 C17 116.8(8) . . ? O6 C16 C17 116.7(8) . . ? C18 C17 C22 119.4(7) . . ? C18 C17 C16 119.7(8) . . ? C22 C17 C16 120.9(8) . . ? C19 C18 C17 121.6(7) . . ? C19 C18 Cl9 118.6(6) . . ? C17 C18 Cl9 119.8(6) . . ? C18 C19 C20 120.4(7) . . ? C18 C19 Cl10 120.3(7) . . ? C20 C19 Cl10 119.2(6) . . ? C19 C20 C21 116.9(7) . . ? C19 C20 C8 121.6(8) . . ? C21 C20 C8 121.4(8) . . ? C22 C21 C20 121.2(7) . . ? C22 C21 Cl11 119.0(7) . . ? C20 C21 Cl11 119.7(7) . . ? C21 C22 C17 120.4(7) . . ? C21 C22 Cl12 121.2(7) . . ? C17 C22 Cl12 118.4(6) . . ? O7 C23 N1 126.8(9) . . ? O7 C23 H23 116.6 . . ? N1 C23 H23 116.6 . . ? N1 C24 H24A 109.5 . . ? N1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O8 C26 N2A 128.8(11) . . ? O8 C26 H26 115.6 . . ? N2A C26 H26 115.6 . . ? N2A C27 H27A 109.5 . . ? N2A C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2A C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2A C28 H28A 109.5 . . ? N2A C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N2A C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O9 C29 N3 151(3) . . ? O9 C29 H29 104.3 . . ? N3 C29 H29 104.3 . . ? N3 C30 H30D 109.5 . . ? N3 C30 H30E 109.5 . . ? H30D C30 H30E 109.5 . . ? N3 C30 H30F 109.5 . . ? H30D C30 H30F 109.5 . . ? H30E C30 H30F 109.5 . . ? N3 C31 H31D 109.5 . . ? N3 C31 H31E 109.5 . . ? H31D C31 H31E 109.5 . . ? N3 C31 H31F 109.5 . . ? H31D C31 H31F 109.5 . . ? H31E C31 H31F 109.5 . . ? C23 N1 C25 118.9(9) . . ? C23 N1 C24 121.2(8) . . ? C25 N1 C24 119.9(9) . . ? C26 N2A C27 124.2(10) . . ? C26 N2A C28 117.8(10) . . ? C27 N2A C28 117.4(9) . . ? C29 N3 C31 152(2) . . ? C29 N3 C30 107(2) . . ? C31 N3 C30 99.6(13) . . ? C1 O1 Tb1 137.8(6) . 14 ? C9 O3 Tb1 89.9(5) . . ? C9 O4 Tb1 95.7(5) . . ? C16 O5 Tb1 145.9(5) . 8_554 ? C16 O6 Tb1 155.9(5) . 16_645 ? C23 O7 Tb1 129.5(7) . . ? C23 O7 H7 115.3 . . ? Tb1 O7 H7 115.3 . . ? C26 O8 Tb1 135.8(6) . . ? C29 O9 Tb1 141.4(14) . . ? O1 Tb1 O9 78.1(2) 14_455 . ? O1 Tb1 O6 98.4(2) 14_455 15_665 ? O9 Tb1 O6 154.19(19) . 15_665 ? O1 Tb1 O8 70.4(2) 14_455 . ? O9 Tb1 O8 118.8(2) . . ? O6 Tb1 O8 82.8(2) 15_665 . ? O1 Tb1 O7 143.63(19) 14_455 . ? O9 Tb1 O7 79.1(2) . . ? O6 Tb1 O7 90.1(2) 15_665 . ? O8 Tb1 O7 146.00(19) . . ? O1 Tb1 O5 74.6(2) 14_455 3_545 ? O9 Tb1 O5 77.3(2) . 3_545 ? O6 Tb1 O5 77.14(19) 15_665 3_545 ? O8 Tb1 O5 136.3(2) . 3_545 ? O7 Tb1 O5 72.96(18) . 3_545 ? O1 Tb1 O4 117.6(2) 14_455 . ? O9 Tb1 O4 72.3(2) . . ? O6 Tb1 O4 129.52(19) 15_665 . ? O8 Tb1 O4 78.0(2) . . ? O7 Tb1 O4 81.3(2) . . ? O5 Tb1 O4 143.2(2) 3_545 . ? O1 Tb1 O3 142.27(19) 14_455 . ? O9 Tb1 O3 120.6(2) . . ? O6 Tb1 O3 77.7(2) 15_665 . ? O8 Tb1 O3 71.92(18) . . ? O7 Tb1 O3 74.08(16) . . ? O5 Tb1 O3 138.03(18) 3_545 . ? O4 Tb1 O3 52.1(2) . . ? O1 Tb1 C9 134.5(2) 14_455 . ? O9 Tb1 C9 96.4(3) . . ? O6 Tb1 C9 103.7(3) 15_665 . ? O8 Tb1 C9 73.6(2) . . ? O7 Tb1 C9 76.0(2) . . ? O5 Tb1 C9 148.9(2) 3_545 . ? O4 Tb1 C9 26.0(2) . . ? O3 Tb1 C9 26.1(2) . . ? _diffrn_measured_fraction_theta_max 0.774 _diffrn_reflns_theta_full 19.77 _diffrn_measured_fraction_theta_full 0.774 _refine_diff_density_max 0.555 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.073 # Attachment 'B802196A Veciana_CIF2corr3.cif' data_nr140a_2 _database_code_depnum_ccdc_archive 'CCDC 676449' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H17 Cl12 N2 O9 Tb' _chemical_formula_sum 'C28 H17 Cl12 N2 O9 Tb' _chemical_formula_weight 1109.74 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' 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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I41/a _symmetry_space_group_name_Hall -I4ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 28.486(5) _cell_length_b 28.486(5) _cell_length_c 46.678(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 37877(10) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description octahedra _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8640 _exptl_absorpt_coefficient_mu 3.170 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.987 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device_type ADSCq210rCCD-HUBER _diffrn_measurement_method 'f\ scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32374 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 20.17 _reflns_number_total 3389 _reflns_number_gt 3389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CCD Server Software Huber' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'shelxl-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 ( Farrugia, 1997) and Diamond 2.1e' _computing_publication_material 'shelxl-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the high disorder observed around C1-o1-o2 poistions these atoms were only refined isotropically.C1, O1, and O2 were refined isotropically with restraints, and that the resulting Uiso values for those atoms are large. However, even though the crystals of 2 were immersed in paratone and measured at 150 K, they showed high instability due to the fast solvent removal from its channel-like framework that should induce large tensions in the crystals, and therefore, should also induce agitations in the structure. In fact, for example, when crystals of 2 were measured at room temperature, a continuous degradation and lost of the diffraction peaks were observed. We believe that this could be one of the reasons of why it is so difficult to detect the C1-O1-O2 carboxylate group, and therefore, the high large Uiso values finally obtained. H atoms in the anion were refined using a riding model (HFIX33 for C25 and HFIX137 for other methyl groups). ; _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^)+(0.1604P)^2^+91.4081P] 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 SHELXL _refine_ls_extinction_coef 0.00132(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8994 _refine_ls_number_parameters 465 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2645 _refine_ls_wR_factor_gt 0.2433 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 0.79547(2) 0.16387(2) 0.254157(13) 0.1433(5) Uani 1 1 d . . . C2 C 1.1781(5) 0.0934(4) 0.1980(5) 0.213(9) Uani 1 1 d D . . C3 C 1.1425(5) 0.0684(5) 0.2119(3) 0.155(5) Uani 1 1 d . . . C4 C 1.1000(4) 0.0610(4) 0.1993(3) 0.120(3) Uani 1 1 d . . . C5 C 1.0903(4) 0.0758(4) 0.1719(2) 0.110(3) Uani 1 1 d . . . C6 C 1.1269(5) 0.0969(4) 0.1576(2) 0.115(3) Uani 1 1 d . . . C7 C 1.1709(4) 0.1051(4) 0.1702(3) 0.132(4) Uani 1 1 d . . . C8 C 1.0424(4) 0.0697(7) 0.1595(3) 0.220(10) Uani 1 1 d . . . H8 H 1.0392 0.0378 0.1670 0.264 Uiso 1 1 calc R . . C9 C 0.8732(5) 0.1365(4) 0.2211(3) 0.126(4) Uani 1 1 d . . . C10 C 0.9177(4) 0.1188(4) 0.2043(2) 0.113(3) Uani 1 1 d . . . C11 C 0.9198(4) 0.0749(4) 0.1926(2) 0.114(3) Uani 1 1 d . . . C12 C 0.9600(5) 0.0600(4) 0.1782(2) 0.115(3) Uani 1 1 d . . . C13 C 1.0004(4) 0.0871(4) 0.17517(19) 0.109(3) Uani 1 1 d . . . C14 C 0.9986(4) 0.1318(4) 0.1879(2) 0.106(3) Uani 1 1 d . . . C15 C 0.9579(4) 0.1472(3) 0.2024(2) 0.109(3) Uani 1 1 d . . . C16 C 1.0051(6) 0.0041(5) 0.0435(3) 0.133(4) Uani 1 1 d . . . C17 C 1.0150(4) 0.0214(4) 0.0730(2) 0.120(3) Uani 1 1 d . . . C18 C 1.0006(3) 0.0644(4) 0.0820(2) 0.110(3) Uani 1 1 d . . . C19 C 1.0111(4) 0.0812(4) 0.1092(2) 0.112(3) Uani 1 1 d . . . C20 C 1.0353(4) 0.0546(4) 0.1290(2) 0.115(3) Uani 1 1 d . . . C21 C 1.0511(4) 0.0115(5) 0.1200(2) 0.135(4) Uani 1 1 d . . . C22 C 1.0400(4) -0.0050(4) 0.0916(2) 0.131(4) Uani 1 1 d . . . C23 C 0.8537(6) 0.2596(9) 0.2612(3) 0.172(7) Uani 1 1 d . . . H23 H 0.8279 0.2731 0.2545 0.202 Uiso 1 1 d D . . C24 C 0.9327(9) 0.2682(11) 0.2780(6) 0.306(16) Uani 1 1 d . . . H24A H 0.9391 0.2776 0.2973 0.458 Uiso 1 1 calc R . . H24B H 0.9582 0.2776 0.2658 0.458 Uiso 1 1 calc R . . H24C H 0.9292 0.2347 0.2772 0.458 Uiso 1 1 calc R . . C25 C 0.8871(8) 0.3426(8) 0.2662(5) 0.261(11) Uani 1 1 d . . . H25A H 0.8554 0.3512 0.2615 0.391 Uiso 1 1 calc R . . H25B H 0.9079 0.3535 0.2515 0.391 Uiso 1 1 calc R . . H25C H 0.8957 0.3565 0.2842 0.391 Uiso 1 1 calc R . . C26 C 0.7698(7) 0.1019(8) 0.1957(6) 0.239(10) Uani 1 1 d . . . H26 H 0.7847 0.1236 0.1847 0.303 Uiso 1 1 d D . . C27 C 0.7571(9) 0.0603(9) 0.1498(5) 0.291(13) Uani 1 1 d . . . H27A H 0.7742 0.0872 0.1431 0.437 Uiso 1 1 calc R . . H27B H 0.7269 0.0592 0.1407 0.437 Uiso 1 1 calc R . . H27C H 0.7743 0.0323 0.1452 0.437 Uiso 1 1 calc R . . N2A N 0.7510(6) 0.0635(7) 0.1811(5) 0.259(9) Uani 1 1 d . . . N1 N 0.8906(7) 0.2900(6) 0.2685(3) 0.189(5) Uani 1 1 d . . . O1 O 1.2281(6) 0.1295(6) 0.2258(3) 0.334(14) Uiso 1 1 d . . . O2 O 1.2493(9) 0.0811(10) 0.2038(6) 0.400(14) Uiso 1 1 d D . . O3 O 0.8476(3) 0.1641(3) 0.20856(19) 0.139(3) Uani 1 1 d . . . O4 O 0.8658(4) 0.1215(3) 0.2445(2) 0.169(4) Uani 1 1 d . . . O5 O 0.9662(4) -0.0157(3) 0.04072(17) 0.151(3) Uani 1 1 d . . . O6 O 1.0354(4) 0.0090(3) 0.0243(2) 0.161(4) Uani 1 1 d . . . O7 O 0.8539(4) 0.2188(4) 0.2628(2) 0.159(4) Uani 1 1 d . . . O8 O 0.7658(4) 0.1069(4) 0.2213(2) 0.191(5) Uani 1 1 d . . . O9 O 0.8375(5) 0.1296(5) 0.2976(3) 0.356(11) Uani 1 1 d D . . H9A H 0.8192 0.1281 0.3112 0.535 Uiso 1 1 calc R . . Cl1 Cl 1.15424(18) 0.04925(18) 0.24659(10) 0.222(2) Uani 1 1 d . . . Cl2 Cl 1.05925(13) 0.03083(13) 0.21908(8) 0.1639(13) Uani 1 1 d . . . Cl3 Cl 1.11937(11) 0.11727(12) 0.12228(6) 0.1391(10) Uani 1 1 d . . . Cl4 Cl 1.21430(13) 0.13292(16) 0.15099(10) 0.1843(15) Uani 1 1 d . . . Cl5 Cl 0.87107(13) 0.03974(12) 0.19454(9) 0.1681(14) Uani 1 1 d . . . Cl6 Cl 0.95896(12) 0.00313(11) 0.16463(8) 0.1561(12) Uani 1 1 d . . . Cl7 Cl 1.04419(9) 0.16999(11) 0.18561(6) 0.1266(9) Uani 1 1 d . . . Cl8 Cl 0.95628(12) 0.20219(10) 0.21749(7) 0.1442(11) Uani 1 1 d . . . Cl9 Cl 0.96993(11) 0.09915(10) 0.05821(6) 0.1350(11) Uani 1 1 d . . . Cl10 Cl 0.99451(10) 0.13807(10) 0.11746(6) 0.1354(10) Uani 1 1 d . . . Cl11 Cl 1.08138(14) -0.02597(14) 0.14283(7) 0.1687(14) Uani 1 1 d . . . Cl12 Cl 1.05979(15) -0.06048(12) 0.08157(8) 0.1753(15) Uani 1 1 d . . . C1 C 1.2143(7) 0.1033(9) 0.2110(6) 0.68(7) Uiso 1 1 d D . . C28 C 0.7287(19) 0.0269(16) 0.1941(8) 0.69(6) Uani 1 1 d . . . H28A H 0.7187 0.0047 0.1799 1.037 Uiso 1 1 calc R . . H28B H 0.7019 0.0384 0.2044 1.037 Uiso 1 1 calc R . . H28C H 0.7499 0.0119 0.2072 1.037 Uiso 1 1 calc R . . H9 H 0.8394 0.1522 0.3097 2.000 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.1673(7) 0.1448(6) 0.1180(6) -0.0293(4) 0.0807(4) -0.0312(4) C2 0.147(13) 0.27(2) 0.218(19) 0.074(16) -0.131(14) -0.025(13) C3 0.155(11) 0.165(11) 0.145(11) 0.043(9) -0.051(10) -0.036(9) C4 0.127(9) 0.121(8) 0.112(9) -0.008(6) -0.027(7) -0.018(6) C5 0.109(8) 0.131(8) 0.089(7) -0.031(6) -0.014(6) 0.010(6) C6 0.139(10) 0.113(7) 0.093(7) -0.008(6) -0.022(7) 0.024(7) C7 0.108(8) 0.138(9) 0.150(10) 0.003(8) -0.044(8) -0.005(6) C8 0.100(8) 0.42(3) 0.135(10) -0.173(15) -0.033(8) 0.043(11) C9 0.156(12) 0.100(8) 0.120(11) 0.002(7) 0.022(9) -0.018(8) C10 0.135(9) 0.118(8) 0.085(6) -0.009(6) 0.017(6) -0.012(7) C11 0.133(9) 0.102(7) 0.108(7) -0.013(6) 0.010(7) -0.012(6) C12 0.131(9) 0.118(8) 0.096(7) -0.030(6) -0.012(6) 0.010(7) C13 0.110(8) 0.143(9) 0.074(6) -0.032(6) -0.013(5) 0.006(7) C14 0.115(8) 0.132(8) 0.072(6) -0.012(6) 0.002(5) -0.003(6) C15 0.143(9) 0.102(7) 0.081(6) -0.010(5) 0.007(6) -0.011(7) C16 0.161(13) 0.130(10) 0.107(10) -0.053(8) -0.033(9) 0.020(9) C17 0.147(9) 0.117(8) 0.096(7) -0.051(7) -0.041(7) 0.024(7) C18 0.126(8) 0.119(8) 0.084(6) -0.039(6) -0.022(5) 0.012(6) C19 0.111(7) 0.119(8) 0.106(8) -0.055(7) -0.003(6) 0.015(6) C20 0.111(7) 0.140(9) 0.093(7) -0.046(7) -0.018(6) 0.017(6) C21 0.126(8) 0.173(11) 0.105(8) -0.032(8) -0.032(6) 0.026(8) C22 0.153(9) 0.137(9) 0.105(8) -0.055(7) -0.024(7) 0.027(7) C23 0.179(14) 0.229(19) 0.108(9) -0.047(13) 0.077(9) -0.059(17) C24 0.21(2) 0.39(4) 0.32(3) -0.17(3) 0.03(2) -0.01(2) C25 0.33(3) 0.22(2) 0.24(2) -0.032(17) 0.09(2) -0.08(2) C26 0.208(18) 0.216(19) 0.29(3) -0.11(2) 0.064(19) -0.041(14) C27 0.30(3) 0.35(3) 0.22(2) -0.11(2) 0.08(2) -0.08(2) C28 0.93(11) 0.72(8) 0.42(5) -0.32(5) 0.46(6) -0.64(9) N2A 0.220(15) 0.282(19) 0.27(2) -0.151(18) 0.101(14) -0.073(14) N1 0.215(16) 0.205(15) 0.149(10) -0.057(10) 0.080(11) -0.035(13) O3 0.146(7) 0.147(7) 0.126(6) -0.008(5) 0.044(5) -0.017(5) O4 0.233(10) 0.155(7) 0.121(6) 0.001(6) 0.051(7) -0.024(7) O5 0.184(8) 0.161(7) 0.108(5) -0.066(5) -0.034(6) 0.020(6) O6 0.199(9) 0.162(7) 0.120(7) -0.085(6) -0.060(6) 0.043(7) O7 0.192(9) 0.152(7) 0.132(7) -0.042(7) 0.060(6) -0.024(7) O8 0.193(9) 0.216(10) 0.164(8) -0.071(8) 0.103(8) -0.056(7) O9 0.244(14) 0.63(4) 0.192(12) 0.082(17) 0.070(11) 0.038(18) Cl1 0.236(5) 0.237(5) 0.193(4) 0.099(3) -0.109(4) -0.054(4) Cl2 0.167(3) 0.182(3) 0.142(3) -0.005(2) -0.014(2) -0.033(2) Cl3 0.154(2) 0.166(3) 0.0978(18) -0.0174(17) -0.0157(16) 0.0201(19) Cl4 0.136(3) 0.209(4) 0.208(4) 0.038(3) -0.018(3) -0.018(2) Cl5 0.176(3) 0.129(2) 0.200(3) -0.027(2) 0.043(3) -0.040(2) Cl6 0.165(3) 0.133(2) 0.170(3) -0.056(2) -0.017(2) 0.012(2) Cl7 0.120(2) 0.159(2) 0.1006(17) -0.0256(16) -0.0013(14) -0.0240(17) Cl8 0.162(3) 0.121(2) 0.150(2) -0.0365(18) 0.034(2) -0.0215(18) Cl9 0.159(2) 0.141(2) 0.1047(19) -0.0436(16) -0.0227(17) 0.0394(18) Cl10 0.143(2) 0.140(2) 0.123(2) -0.0719(18) -0.0021(17) 0.0105(17) Cl11 0.183(3) 0.204(3) 0.120(2) -0.024(2) -0.047(2) 0.046(3) Cl12 0.228(4) 0.148(3) 0.150(3) -0.057(2) -0.047(3) 0.058(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 O6 2.223(14) 15_665 ? Tb1 O7 2.320(12) . ? Tb1 O1 2.349(9) 14_455 ? Tb1 O4 2.383(11) . ? Tb1 O8 2.388(11) . ? Tb1 O5 2.419(9) 3_545 ? Tb1 O9 2.551(16) . ? Tb1 O3 2.595(7) . ? Tb1 C9 2.808(14) . ? C2 C1 1.23(3) . ? C2 C7 1.35(2) . ? C2 C3 1.399(15) . ? C3 C4 1.361(15) . ? C3 Cl1 1.739(14) . ? C4 C5 1.378(15) . ? C4 Cl2 1.714(12) . ? C5 C6 1.376(14) . ? C5 C8 1.490(14) . ? C6 C7 1.407(15) . ? C6 Cl3 1.760(11) . ? C7 Cl4 1.721(13) . ? C8 C13 1.486(14) . ? C8 C20 1.504(14) . ? C8 H8 0.9800 . ? C9 O4 1.189(14) . ? C9 O3 1.222(14) . ? C9 C10 1.575(17) . ? C10 C11 1.366(13) . ? C10 C15 1.406(13) . ? C11 C12 1.395(14) . ? C11 Cl5 1.714(11) . ? C12 C13 1.391(14) . ? C12 Cl6 1.740(10) . ? C13 C14 1.407(13) . ? C14 C15 1.413(13) . ? C14 Cl7 1.696(10) . ? C15 Cl8 1.719(10) . ? C16 O6 1.252(15) . ? C16 O5 1.251(15) . ? C16 C17 1.489(16) . ? C17 C22 1.352(14) . ? C17 C18 1.359(13) . ? C18 C19 1.390(13) . ? C18 Cl9 1.723(10) . ? C19 C20 1.378(14) . ? C19 Cl10 1.733(10) . ? C20 C21 1.373(14) . ? C21 C22 1.437(15) . ? C21 Cl11 1.739(12) . ? C22 Cl12 1.744(11) . ? C23 O7 1.16(2) . ? C23 N1 1.40(2) . ? C23 H23 0.8900 . ? C24 N1 1.42(3) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N1 1.50(2) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O8 1.21(3) . ? C26 N2A 1.40(2) . ? C27 N2A 1.47(2) . ? C26 H26 0.9100 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N2A C28 1.36(3) . ? O5 Tb1 2.419(9) 8_554 ? O6 Tb1 2.223(14) 16_645 ? O9 H9A 0.8200 . ? O9 H9 0.857 . ? C1 O1 1.09(2) . ? C1 O2 1.226(17) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? O1 O2 1.82(3) . ? O1 Tb1 2.349(9) 14 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Tb1 O7 90.1(4) 15_665 . ? O6 Tb1 O1 97.4(7) 15_665 14_455 ? O7 Tb1 O1 143.0(4) . 14_455 ? O6 Tb1 O4 127.5(3) 15_665 . ? O7 Tb1 O4 76.8(3) . . ? O1 Tb1 O4 123.4(6) 14_455 . ? O6 Tb1 O8 83.8(4) 15_665 . ? O7 Tb1 O8 145.4(3) . . ? O1 Tb1 O8 71.6(3) 14_455 . ? O4 Tb1 O8 80.3(4) . . ? O6 Tb1 O5 81.8(3) 15_665 3_545 ? O7 Tb1 O5 73.4(3) . 3_545 ? O1 Tb1 O5 71.9(3) 14_455 3_545 ? O4 Tb1 O5 137.8(3) . 3_545 ? O8 Tb1 O5 138.4(3) . 3_545 ? O6 Tb1 O9 160.9(3) 15_665 . ? O7 Tb1 O9 77.5(4) . . ? O1 Tb1 O9 84.6(7) 14_455 . ? O4 Tb1 O9 64.1(4) . . ? O8 Tb1 O9 114.7(4) . . ? O5 Tb1 O9 80.7(4) 3_545 . ? O6 Tb1 O3 77.0(3) 15_665 . ? O7 Tb1 O3 74.3(3) . . ? O1 Tb1 O3 142.7(3) 14_455 . ? O4 Tb1 O3 50.5(3) . . ? O8 Tb1 O3 71.2(3) . . ? O5 Tb1 O3 141.0(3) 3_545 . ? O9 Tb1 O3 112.6(4) . . ? O6 Tb1 C9 102.7(4) 15_665 . ? O7 Tb1 C9 73.5(3) . . ? O1 Tb1 C9 138.3(4) 14_455 . ? O4 Tb1 C9 24.8(3) . . ? O8 Tb1 C9 74.8(3) . . ? O5 Tb1 C9 146.6(3) 3_545 . ? O9 Tb1 C9 87.7(5) . . ? O3 Tb1 C9 25.7(3) . . ? C1 C2 C7 122.7(14) . . ? C1 C2 C3 119.8(15) . . ? C7 C2 C3 117.5(7) . . ? C4 C3 C2 121.4(11) . . ? C4 C3 Cl1 121.6(12) . . ? C2 C3 Cl1 116.9(9) . . ? C3 C4 C5 122.3(11) . . ? C3 C4 Cl2 116.6(10) . . ? C5 C4 Cl2 121.1(9) . . ? C6 C5 C4 115.6(9) . . ? C6 C5 C8 123.8(12) . . ? C4 C5 C8 120.6(13) . . ? C5 C6 C7 123.0(10) . . ? C5 C6 Cl3 120.4(9) . . ? C7 C6 Cl3 116.5(11) . . ? C2 C7 C6 119.7(10) . . ? C2 C7 Cl4 120.3(7) . . ? C6 C7 Cl4 119.9(10) . . ? C13 C8 C5 120.5(8) . . ? C13 C8 C20 116.9(9) . . ? C5 C8 C20 121.6(10) . . ? C13 C8 H8 93.3 . . ? C5 C8 H8 93.3 . . ? C20 C8 H8 93.3 . . ? O4 C9 O3 124.5(14) . . ? O4 C9 C10 119.0(14) . . ? O3 C9 C10 116.5(12) . . ? O4 C9 Tb1 57.2(8) . . ? O3 C9 Tb1 67.3(7) . . ? C10 C9 Tb1 176.1(11) . . ? C11 C10 C15 117.8(10) . . ? C11 C10 C9 121.9(10) . . ? C15 C10 C9 120.2(10) . . ? C10 C11 C12 120.5(10) . . ? C10 C11 Cl5 118.5(9) . . ? C12 C11 Cl5 120.9(9) . . ? C13 C12 C11 124.0(9) . . ? C13 C12 Cl6 119.6(9) . . ? C11 C12 Cl6 116.3(10) . . ? C12 C13 C14 115.5(9) . . ? C12 C13 C8 122.1(12) . . ? C14 C13 C8 122.4(12) . . ? C13 C14 C15 120.8(9) . . ? C13 C14 Cl7 121.8(8) . . ? C15 C14 Cl7 117.3(8) . . ? C10 C15 C14 121.4(9) . . ? C10 C15 Cl8 118.5(9) . . ? C14 C15 Cl8 120.1(9) . . ? O6 C16 O5 125.8(12) . . ? O6 C16 C17 119.6(14) . . ? O5 C16 C17 114.5(14) . . ? C22 C17 C18 117.6(9) . . ? C22 C17 C16 120.7(10) . . ? C18 C17 C16 121.7(11) . . ? C17 C18 C19 121.6(9) . . ? C17 C18 Cl9 118.2(7) . . ? C19 C18 Cl9 120.1(8) . . ? C20 C19 C18 122.1(9) . . ? C20 C19 Cl10 120.2(8) . . ? C18 C19 Cl10 117.7(9) . . ? C21 C20 C19 116.7(8) . . ? C21 C20 C8 120.2(12) . . ? C19 C20 C8 123.0(11) . . ? C20 C21 C22 120.1(10) . . ? C20 C21 Cl11 121.5(9) . . ? C22 C21 Cl11 118.3(10) . . ? C17 C22 C21 121.7(10) . . ? C17 C22 Cl12 120.0(8) . . ? C21 C22 Cl12 118.2(10) . . ? O7 C23 N1 127(2) . . ? N1 C24 H24A 109.5 . . ? N1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O8 C26 N2A 123(2) . . ? N2A C27 H27A 109.5 . . ? N2A C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2A C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C28 N2A C26 124(2) . . ? C28 N2A C27 116.8(19) . . ? C26 N2A C27 119(2) . . ? C23 N1 C24 116(2) . . ? C23 N1 C25 123(2) . . ? C24 N1 C25 121(2) . . ? C9 O3 Tb1 86.9(8) . . ? C9 O4 Tb1 98.1(10) . . ? C16 O5 Tb1 141.1(9) . 8_554 ? C16 O6 Tb1 158.2(9) . 16_645 ? C23 O7 Tb1 131.1(14) . . ? C26 O8 Tb1 133.0(12) . . ? Tb1 O9 H9A 109.5 . . ? Tb1 O9 H9 105.3 . . ? H9A O9 H9 64.7 . . ? O1 C1 O2 104(2) . . ? O1 C1 C2 140(3) . . ? O2 C1 C2 115(2) . . ? N2A C28 H28A 109.5 . . ? N2A C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N2A C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C1 O1 O2 40.9(13) . . ? C1 O1 Tb1 146(2) . 14 ? O2 O1 Tb1 105.7(15) . 14 ? C1 O2 O1 35.6(10) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 20.17 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.958 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.096