# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2009 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'M. L. P. Reddy' _publ_contact_author_email MLPREDDY55@GMAIL.COM _publ_section_title ; 3-Phenyl-4-acyl-5-isoxazolonate complex of Tb3+ doped into poly-beta-hydroxybutyrate matrix as a promising light-conversion molecular device ; loop_ _publ_author_name 'M. L. P. Reddy' 'Silvanose Biju' 'Alan H. Cowley' 'Kalyan Vasudevan' # Attachment 'Compound 1.cif' data_sbkv099b _database_code_depnum_ccdc_archive 'CCDC 702914' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H34 N3 O11 Tb' _chemical_formula_sum 'C36 H34 N3 O11 Tb' _chemical_formula_weight 843.58 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 P21/c _symmetry_space_group_name_Hall -P2ybc 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 22.803(5) _cell_length_b 5.9919(12) _cell_length_c 26.097(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.27(3) _cell_angle_gamma 90.00 _cell_volume 3496.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8748 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 2.088 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14424 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.1013 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7991 _reflns_number_gt 5541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. Four water hydrogen atoms were not located. They should be located on the 2 bare oxygen atoms bound to the Terbium atom. ; _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^)+(0.0640P)^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 SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 7991 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7031(3) 0.4216(10) -0.0956(2) 0.0161(13) Uani 1 1 d . . . C2 C 0.7333(2) 0.2664(10) -0.1209(2) 0.0151(12) Uani 1 1 d . . . C3 C 0.7310(3) 0.3656(9) -0.1710(2) 0.0166(13) Uani 1 1 d . . . C4 C 0.7627(3) 0.0739(10) -0.0947(2) 0.0153(12) Uani 1 1 d . . . C5 C 0.8062(3) -0.0611(11) -0.1178(2) 0.0244(14) Uani 1 1 d . . . H5A H 0.8339 0.0401 -0.1298 0.029 Uiso 1 1 calc R . . H5B H 0.7845 -0.1395 -0.1482 0.029 Uiso 1 1 calc R . . C6 C 0.8417(3) -0.2288(12) -0.0816(2) 0.0302(16) Uani 1 1 d . . . H6A H 0.8632 -0.1539 -0.0511 0.045 Uiso 1 1 calc R . . H6B H 0.8694 -0.3034 -0.0991 0.045 Uiso 1 1 calc R . . H6C H 0.8150 -0.3364 -0.0713 0.045 Uiso 1 1 calc R . . C7 C 0.7544(3) 0.2914(10) -0.2175(2) 0.0170(13) Uani 1 1 d . . . C8 C 0.7882(3) 0.4429(11) -0.2403(2) 0.0213(14) Uani 1 1 d . . . H8 H 0.7973 0.5822 -0.2251 0.026 Uiso 1 1 calc R . . C9 C 0.8083(3) 0.3872(10) -0.2854(2) 0.0237(15) Uani 1 1 d . . . H9 H 0.8311 0.4885 -0.3002 0.028 Uiso 1 1 calc R . . C10 C 0.7947(3) 0.1840(10) -0.3083(2) 0.0233(15) Uani 1 1 d . . . H10 H 0.8078 0.1474 -0.3389 0.028 Uiso 1 1 calc R . . C11 C 0.7612(3) 0.0313(11) -0.2858(2) 0.0229(14) Uani 1 1 d . . . H11 H 0.7521 -0.1074 -0.3013 0.027 Uiso 1 1 calc R . . C12 C 0.7413(3) 0.0844(10) -0.2407(2) 0.0198(14) Uani 1 1 d . . . H12 H 0.7191 -0.0186 -0.2258 0.024 Uiso 1 1 calc R . . C13 C 0.8186(2) -0.1238(9) 0.08522(19) 0.0119(12) Uani 1 1 d . . . C14 C 0.8635(2) 0.0389(10) 0.0909(2) 0.0133(12) Uani 1 1 d . . . C15 C 0.9116(2) -0.0556(10) 0.1282(2) 0.0162(12) Uani 1 1 d . . . C16 C 0.8561(3) 0.2358(9) 0.0591(2) 0.0141(12) Uani 1 1 d . . . C17 C 0.9094(3) 0.3666(10) 0.0494(2) 0.0212(14) Uani 1 1 d . . . H17A H 0.8965 0.5135 0.0362 0.025 Uiso 1 1 calc R . . H17B H 0.9377 0.3858 0.0821 0.025 Uiso 1 1 calc R . . C18 C 0.9399(5) 0.2503(17) 0.0107(4) 0.092(4) Uani 1 1 d . . . H18A H 0.9578 0.1144 0.0258 0.139 Uiso 1 1 calc R . . H18B H 0.9703 0.3457 0.0020 0.139 Uiso 1 1 calc R . . H18C H 0.9110 0.2165 -0.0203 0.139 Uiso 1 1 calc R . . C19 C 0.9703(2) 0.0331(10) 0.1545(2) 0.0172(13) Uani 1 1 d . . . C20 C 1.0201(3) -0.1061(10) 0.1616(2) 0.0237(15) Uani 1 1 d . . . H20 H 1.0178 -0.2438 0.1449 0.028 Uiso 1 1 calc R . . C21 C 1.0736(3) -0.0399(12) 0.1938(2) 0.0286(16) Uani 1 1 d . . . H21 H 1.1067 -0.1336 0.1986 0.034 Uiso 1 1 calc R . . C22 C 1.0771(3) 0.1644(11) 0.2184(2) 0.0289(16) Uani 1 1 d . . . H22 H 1.1125 0.2072 0.2404 0.035 Uiso 1 1 calc R . . C23 C 1.0282(3) 0.3066(11) 0.2104(2) 0.0265(16) Uani 1 1 d . . . H23 H 1.0311 0.4456 0.2265 0.032 Uiso 1 1 calc R . . C24 C 0.9745(3) 0.2422(11) 0.1782(2) 0.0229(14) Uani 1 1 d . . . H24 H 0.9418 0.3382 0.1727 0.028 Uiso 1 1 calc R . . C25 C 0.5646(2) 0.2153(9) 0.0276(2) 0.0132(12) Uani 1 1 d . . . C26 C 0.5681(2) 0.1332(9) 0.0793(2) 0.0145(12) Uani 1 1 d . . . C27 C 0.5073(2) 0.1335(9) 0.0858(2) 0.0143(12) Uani 1 1 d . . . C28 C 0.6220(3) 0.0532(11) 0.1106(2) 0.0181(13) Uani 1 1 d . . . C29 C 0.6236(3) -0.0402(13) 0.1641(2) 0.0349(18) Uani 1 1 d . . . H29A H 0.5928 0.0296 0.1795 0.042 Uiso 1 1 calc R . . H29B H 0.6621 -0.0084 0.1862 0.042 Uiso 1 1 calc R . . C30 C 0.6134(4) -0.2938(14) 0.1606(3) 0.058(3) Uani 1 1 d . . . H30A H 0.5739 -0.3242 0.1413 0.086 Uiso 1 1 calc R . . H30B H 0.6177 -0.3545 0.1952 0.086 Uiso 1 1 calc R . . H30C H 0.6424 -0.3612 0.1432 0.086 Uiso 1 1 calc R . . C31 C 0.4798(2) 0.0624(11) 0.1301(2) 0.0184(13) Uani 1 1 d . . . C32 C 0.4788(3) 0.2051(11) 0.1717(2) 0.0293(16) Uani 1 1 d . . . H32 H 0.4972 0.3439 0.1727 0.035 Uiso 1 1 calc R . . C33 C 0.4505(4) 0.1425(12) 0.2117(3) 0.0399(19) Uani 1 1 d . . . H33 H 0.4495 0.2399 0.2393 0.048 Uiso 1 1 calc R . . C34 C 0.4241(3) -0.0627(13) 0.2108(2) 0.0289(16) Uani 1 1 d . . . H34 H 0.4056 -0.1049 0.2380 0.035 Uiso 1 1 calc R . . C35 C 0.4248(3) -0.2055(11) 0.1705(2) 0.0270(16) Uani 1 1 d . . . H35 H 0.4068 -0.3449 0.1703 0.032 Uiso 1 1 calc R . . C36 C 0.4520(3) -0.1448(11) 0.1296(2) 0.0232(14) Uani 1 1 d . . . H36 H 0.4518 -0.2423 0.1019 0.028 Uiso 1 1 calc R . . N1 N 0.7029(2) 0.5559(9) -0.17612(17) 0.0221(12) Uani 1 1 d . . . N2 N 0.8984(2) -0.2532(9) 0.14400(18) 0.0196(11) Uani 1 1 d . . . N3 N 0.4711(2) 0.2045(8) 0.04398(18) 0.0182(11) Uani 1 1 d . . . O1 O 0.69242(16) 0.4280(6) -0.04958(13) 0.0147(8) Uani 1 1 d . . . O2 O 0.75268(17) 0.0189(6) -0.05116(14) 0.0180(9) Uani 1 1 d . . . O3 O 0.76707(16) -0.1370(6) 0.05806(14) 0.0150(9) Uani 1 1 d . . . O4 O 0.80526(17) 0.2946(6) 0.03564(14) 0.0166(9) Uani 1 1 d . . . O5 O 0.60349(16) 0.2558(7) 0.00079(14) 0.0157(9) Uani 1 1 d . . . O6 O 0.66990(16) 0.0494(7) 0.09297(14) 0.0172(9) Uani 1 1 d . . . O7 O 0.68548(18) 0.5950(6) -0.12672(14) 0.0186(9) Uani 1 1 d . . . O8 O 0.83864(17) -0.3004(6) 0.11573(14) 0.0173(9) Uani 1 1 d . . . O9 O 0.50659(17) 0.2586(7) 0.00595(14) 0.0162(9) Uani 1 1 d . . . O10 O 0.70263(17) 0.4911(6) 0.06526(14) 0.0190(9) Uani 1 1 d . . . O11 O 0.65092(17) -0.1746(6) -0.01592(14) 0.0182(9) Uani 1 1 d . . . Tb1 Tb 0.705122(12) 0.15138(4) 0.015936(9) 0.01150(10) 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 0.016(3) 0.016(3) 0.016(3) 0.003(3) 0.004(2) -0.003(2) C2 0.018(3) 0.013(3) 0.015(3) -0.003(2) 0.006(2) -0.003(3) C3 0.020(3) 0.011(3) 0.020(3) -0.002(3) 0.006(2) -0.006(3) C4 0.019(3) 0.014(3) 0.013(3) -0.002(2) 0.004(2) -0.003(3) C5 0.027(4) 0.023(3) 0.025(3) -0.002(3) 0.010(3) 0.006(3) C6 0.029(4) 0.024(4) 0.039(4) -0.003(3) 0.008(3) 0.011(3) C7 0.021(3) 0.020(3) 0.009(3) -0.002(2) 0.000(2) 0.006(3) C8 0.027(3) 0.018(3) 0.020(3) -0.003(3) 0.006(3) 0.002(3) C9 0.032(4) 0.017(4) 0.023(3) 0.003(3) 0.009(3) -0.003(3) C10 0.031(4) 0.024(4) 0.016(3) -0.001(3) 0.008(3) 0.007(3) C11 0.029(4) 0.020(4) 0.019(3) -0.006(3) 0.003(3) -0.001(3) C12 0.026(3) 0.018(3) 0.017(3) 0.001(3) 0.007(3) -0.005(3) C13 0.015(3) 0.010(3) 0.011(3) -0.004(2) 0.005(2) -0.002(2) C14 0.012(3) 0.012(3) 0.017(3) 0.000(2) 0.006(2) -0.003(2) C15 0.018(3) 0.013(3) 0.018(3) -0.005(3) 0.005(2) 0.003(3) C16 0.019(3) 0.008(3) 0.017(3) -0.003(2) 0.007(3) 0.000(2) C17 0.021(3) 0.017(3) 0.025(3) 0.004(3) 0.001(3) -0.001(3) C18 0.100(9) 0.065(7) 0.142(10) -0.046(7) 0.097(8) -0.039(7) C19 0.018(3) 0.017(3) 0.015(3) 0.002(3) 0.003(2) -0.003(3) C20 0.027(4) 0.021(4) 0.022(3) 0.001(3) 0.004(3) 0.003(3) C21 0.016(3) 0.031(4) 0.037(4) 0.007(3) 0.003(3) 0.001(3) C22 0.019(3) 0.038(4) 0.026(3) 0.005(3) -0.005(3) -0.008(3) C23 0.031(4) 0.026(4) 0.020(3) -0.005(3) -0.001(3) -0.008(3) C24 0.026(3) 0.021(3) 0.021(3) 0.005(3) 0.002(3) 0.007(3) C25 0.014(3) 0.005(3) 0.021(3) -0.006(2) 0.002(2) 0.001(2) C26 0.013(3) 0.017(3) 0.014(3) 0.000(2) 0.005(2) -0.002(2) C27 0.013(3) 0.012(3) 0.019(3) -0.002(3) 0.006(2) -0.003(2) C28 0.017(3) 0.023(3) 0.015(3) -0.002(3) 0.006(2) -0.008(3) C29 0.018(3) 0.068(6) 0.020(3) 0.015(4) 0.006(3) 0.008(4) C30 0.052(5) 0.066(7) 0.063(5) 0.048(5) 0.033(4) 0.027(5) C31 0.015(3) 0.024(3) 0.017(3) 0.001(3) 0.002(2) 0.000(3) C32 0.035(4) 0.025(4) 0.032(4) -0.008(3) 0.016(3) -0.005(3) C33 0.052(5) 0.037(5) 0.036(4) -0.017(4) 0.023(4) -0.003(4) C34 0.022(4) 0.041(4) 0.026(3) 0.003(3) 0.013(3) -0.004(3) C35 0.020(3) 0.029(4) 0.031(4) 0.009(3) 0.003(3) -0.006(3) C36 0.024(3) 0.028(4) 0.019(3) -0.002(3) 0.006(3) -0.004(3) N1 0.036(3) 0.018(3) 0.016(2) 0.002(2) 0.013(2) 0.000(3) N2 0.018(3) 0.014(3) 0.023(3) 0.001(2) -0.004(2) -0.001(2) N3 0.018(3) 0.011(3) 0.028(3) 0.000(2) 0.008(2) 0.002(2) O1 0.016(2) 0.014(2) 0.0143(19) -0.0028(17) 0.0042(16) 0.0045(17) O2 0.022(2) 0.011(2) 0.021(2) 0.0008(17) 0.0039(18) 0.0033(17) O3 0.012(2) 0.013(2) 0.0192(19) -0.0005(17) 0.0018(16) -0.0025(17) O4 0.016(2) 0.012(2) 0.021(2) 0.0034(17) 0.0020(17) -0.0017(17) O5 0.016(2) 0.013(2) 0.019(2) 0.0008(18) 0.0056(18) -0.0019(18) O6 0.015(2) 0.020(2) 0.017(2) 0.0027(18) 0.0031(17) 0.0009(18) O7 0.029(2) 0.011(2) 0.017(2) 0.0046(17) 0.0103(18) 0.0035(17) O8 0.015(2) 0.014(2) 0.021(2) 0.0047(17) -0.0004(17) -0.0008(17) O9 0.013(2) 0.016(2) 0.019(2) 0.0004(18) 0.0026(17) 0.0001(17) O10 0.024(2) 0.013(2) 0.020(2) -0.0051(17) 0.0035(17) -0.0036(18) O11 0.015(2) 0.016(2) 0.023(2) -0.0048(18) 0.0013(17) -0.0012(17) Tb1 0.01163(15) 0.00981(15) 0.01313(15) 0.00053(12) 0.00262(10) -0.00025(12) _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 O1 1.273(7) . ? C1 O7 1.331(7) . ? C1 C2 1.397(8) . ? C2 C3 1.427(8) . ? C2 C4 1.438(8) . ? C3 N1 1.303(7) . ? C3 C7 1.485(8) . ? C4 O2 1.247(6) . ? C4 C5 1.496(8) . ? C5 C6 1.503(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C12 1.387(8) . ? C7 C8 1.398(8) . ? C8 C9 1.385(8) . ? C8 H8 0.9300 . ? C9 C10 1.365(8) . ? C9 H9 0.9300 . ? C10 C11 1.395(9) . ? C10 H10 0.9300 . ? C11 C12 1.378(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 O3 1.251(6) . ? C13 O8 1.349(6) . ? C13 C14 1.400(7) . ? C14 C16 1.432(8) . ? C14 C15 1.434(7) . ? C15 N2 1.308(8) . ? C15 C19 1.478(7) . ? C16 O4 1.252(6) . ? C16 C17 1.510(8) . ? C17 C18 1.503(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.392(8) . ? C19 C24 1.392(9) . ? C20 C21 1.395(8) . ? C20 H20 0.9300 . ? C21 C22 1.377(9) . ? C21 H21 0.9300 . ? C22 C23 1.387(9) . ? C22 H22 0.9300 . ? C23 C24 1.396(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O5 1.256(6) . ? C25 O9 1.358(6) . ? C25 C26 1.424(8) . ? C26 C28 1.418(8) . ? C26 C27 1.430(8) . ? C27 N3 1.304(7) . ? C27 C31 1.481(8) . ? C28 O6 1.266(7) . ? C28 C29 1.497(8) . ? C29 C30 1.537(11) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.386(8) . ? C31 C36 1.393(8) . ? C32 C33 1.381(9) . ? C32 H32 0.9300 . ? C33 C34 1.367(9) . ? C33 H33 0.9300 . ? C34 C35 1.358(9) . ? C34 H34 0.9300 . ? C35 C36 1.383(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? N1 O7 1.440(6) . ? N2 O8 1.445(6) . ? N3 O9 1.435(6) . ? O1 Tb1 2.358(4) . ? O2 Tb1 2.369(4) . ? O3 Tb1 2.363(4) . ? O4 Tb1 2.399(4) . ? O5 Tb1 2.358(4) . ? O6 Tb1 2.386(4) . ? O10 Tb1 2.415(4) . ? O11 Tb1 2.373(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O7 117.5(5) . . ? O1 C1 C2 132.0(5) . . ? O7 C1 C2 110.5(5) . . ? C1 C2 C3 102.8(5) . . ? C1 C2 C4 122.5(5) . . ? C3 C2 C4 134.4(5) . . ? N1 C3 C2 112.8(5) . . ? N1 C3 C7 115.2(5) . . ? C2 C3 C7 132.0(5) . . ? O2 C4 C2 119.6(5) . . ? O2 C4 C5 118.6(5) . . ? C2 C4 C5 121.8(5) . . ? C4 C5 C6 115.2(5) . . ? C4 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? C4 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 118.9(5) . . ? C12 C7 C3 122.9(5) . . ? C8 C7 C3 118.0(5) . . ? C9 C8 C7 120.5(6) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 120.2(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.7(6) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 120.6(6) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C7 120.0(6) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? O3 C13 O8 117.2(5) . . ? O3 C13 C14 133.7(5) . . ? O8 C13 C14 109.1(4) . . ? C13 C14 C16 120.8(5) . . ? C13 C14 C15 104.1(5) . . ? C16 C14 C15 134.9(5) . . ? N2 C15 C14 112.2(5) . . ? N2 C15 C19 115.0(5) . . ? C14 C15 C19 132.6(5) . . ? O4 C16 C14 120.5(5) . . ? O4 C16 C17 118.1(5) . . ? C14 C16 C17 121.2(5) . . ? C18 C17 C16 111.4(6) . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 119.7(5) . . ? C20 C19 C15 119.2(5) . . ? C24 C19 C15 120.5(5) . . ? C19 C20 C21 120.3(6) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 119.9(6) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.2(6) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 120.4(6) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 119.5(6) . . ? C19 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? O5 C25 O9 117.9(5) . . ? O5 C25 C26 132.8(5) . . ? O9 C25 C26 109.3(5) . . ? C28 C26 C25 123.0(5) . . ? C28 C26 C27 133.1(5) . . ? C25 C26 C27 103.6(5) . . ? N3 C27 C26 111.8(5) . . ? N3 C27 C31 116.9(5) . . ? C26 C27 C31 131.2(5) . . ? O6 C28 C26 120.6(5) . . ? O6 C28 C29 117.7(5) . . ? C26 C28 C29 121.6(5) . . ? C28 C29 C30 109.8(6) . . ? C28 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? C28 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 118.6(6) . . ? C32 C31 C27 120.6(6) . . ? C36 C31 C27 120.7(5) . . ? C33 C32 C31 120.5(6) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 119.9(6) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 120.6(6) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 120.4(6) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 120.0(6) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C3 N1 O7 105.5(4) . . ? C15 N2 O8 105.6(4) . . ? C27 N3 O9 107.6(4) . . ? C1 O1 Tb1 130.1(4) . . ? C4 O2 Tb1 141.0(4) . . ? C13 O3 Tb1 128.9(3) . . ? C16 O4 Tb1 139.1(4) . . ? C25 O5 Tb1 129.3(3) . . ? C28 O6 Tb1 139.3(3) . . ? C1 O7 N1 108.4(4) . . ? C13 O8 N2 108.9(4) . . ? C25 O9 N3 107.7(4) . . ? O5 Tb1 O1 73.41(13) . . ? O5 Tb1 O3 138.65(13) . . ? O1 Tb1 O3 145.99(13) . . ? O5 Tb1 O2 122.80(12) . . ? O1 Tb1 O2 73.06(13) . . ? O3 Tb1 O2 77.32(13) . . ? O5 Tb1 O11 74.46(13) . . ? O1 Tb1 O11 110.04(13) . . ? O3 Tb1 O11 77.54(13) . . ? O2 Tb1 O11 75.38(13) . . ? O5 Tb1 O6 74.19(13) . . ? O1 Tb1 O6 141.00(13) . . ? O3 Tb1 O6 71.92(13) . . ? O2 Tb1 O6 144.60(14) . . ? O11 Tb1 O6 81.17(13) . . ? O5 Tb1 O4 143.52(14) . . ? O1 Tb1 O4 83.16(12) . . ? O3 Tb1 O4 72.81(12) . . ? O2 Tb1 O4 74.00(13) . . ? O11 Tb1 O4 141.09(13) . . ? O6 Tb1 O4 111.96(12) . . ? O5 Tb1 O10 74.99(13) . . ? O1 Tb1 O10 77.39(13) . . ? O3 Tb1 O10 116.27(12) . . ? O2 Tb1 O10 137.56(13) . . ? O11 Tb1 O10 144.64(13) . . ? O6 Tb1 O10 73.73(14) . . ? O4 Tb1 O10 72.83(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -177.6(6) . . . . ? O7 C1 C2 C3 -0.7(6) . . . . ? O1 C1 C2 C4 -3.5(10) . . . . ? O7 C1 C2 C4 173.4(5) . . . . ? C1 C2 C3 N1 -0.4(7) . . . . ? C4 C2 C3 N1 -173.4(6) . . . . ? C1 C2 C3 C7 179.9(6) . . . . ? C4 C2 C3 C7 6.9(11) . . . . ? C1 C2 C4 O2 13.1(9) . . . . ? C3 C2 C4 O2 -175.0(6) . . . . ? C1 C2 C4 C5 -165.6(6) . . . . ? C3 C2 C4 C5 6.3(10) . . . . ? O2 C4 C5 C6 -9.9(8) . . . . ? C2 C4 C5 C6 168.8(6) . . . . ? N1 C3 C7 C12 -126.0(6) . . . . ? C2 C3 C7 C12 53.6(9) . . . . ? N1 C3 C7 C8 50.3(7) . . . . ? C2 C3 C7 C8 -130.1(6) . . . . ? C12 C7 C8 C9 0.0(8) . . . . ? C3 C7 C8 C9 -176.4(5) . . . . ? C7 C8 C9 C10 0.7(9) . . . . ? C8 C9 C10 C11 -0.8(9) . . . . ? C9 C10 C11 C12 0.4(9) . . . . ? C10 C11 C12 C7 0.3(9) . . . . ? C8 C7 C12 C11 -0.5(8) . . . . ? C3 C7 C12 C11 175.8(5) . . . . ? O3 C13 C14 C16 -4.2(10) . . . . ? O8 C13 C14 C16 174.2(5) . . . . ? O3 C13 C14 C15 -179.3(6) . . . . ? O8 C13 C14 C15 -1.0(6) . . . . ? C13 C14 C15 N2 -0.1(6) . . . . ? C16 C14 C15 N2 -174.2(6) . . . . ? C13 C14 C15 C19 -174.9(6) . . . . ? C16 C14 C15 C19 11.0(11) . . . . ? C13 C14 C16 O4 18.0(8) . . . . ? C15 C14 C16 O4 -168.6(6) . . . . ? C13 C14 C16 C17 -156.7(5) . . . . ? C15 C14 C16 C17 16.7(10) . . . . ? O4 C16 C17 C18 -99.4(8) . . . . ? C14 C16 C17 C18 75.4(8) . . . . ? N2 C15 C19 C20 45.1(8) . . . . ? C14 C15 C19 C20 -140.2(6) . . . . ? N2 C15 C19 C24 -126.0(6) . . . . ? C14 C15 C19 C24 48.7(9) . . . . ? C24 C19 C20 C21 2.1(9) . . . . ? C15 C19 C20 C21 -169.1(5) . . . . ? C19 C20 C21 C22 -0.3(9) . . . . ? C20 C21 C22 C23 -1.4(10) . . . . ? C21 C22 C23 C24 1.3(10) . . . . ? C20 C19 C24 C23 -2.2(9) . . . . ? C15 C19 C24 C23 168.9(6) . . . . ? C22 C23 C24 C19 0.5(9) . . . . ? O5 C25 C26 C28 -7.6(10) . . . . ? O9 C25 C26 C28 174.0(5) . . . . ? O5 C25 C26 C27 178.3(6) . . . . ? O9 C25 C26 C27 -0.2(6) . . . . ? C28 C26 C27 N3 -173.0(6) . . . . ? C25 C26 C27 N3 0.3(6) . . . . ? C28 C26 C27 C31 5.0(11) . . . . ? C25 C26 C27 C31 178.3(6) . . . . ? C25 C26 C28 O6 -0.8(9) . . . . ? C27 C26 C28 O6 171.4(6) . . . . ? C25 C26 C28 C29 -177.6(6) . . . . ? C27 C26 C28 C29 -5.4(10) . . . . ? O6 C28 C29 C30 -85.5(7) . . . . ? C26 C28 C29 C30 91.4(7) . . . . ? N3 C27 C31 C32 -98.9(7) . . . . ? C26 C27 C31 C32 83.2(8) . . . . ? N3 C27 C31 C36 78.0(7) . . . . ? C26 C27 C31 C36 -100.0(7) . . . . ? C36 C31 C32 C33 -0.2(10) . . . . ? C27 C31 C32 C33 176.7(6) . . . . ? C31 C32 C33 C34 1.0(11) . . . . ? C32 C33 C34 C35 -0.7(11) . . . . ? C33 C34 C35 C36 -0.3(10) . . . . ? C34 C35 C36 C31 1.0(9) . . . . ? C32 C31 C36 C35 -0.8(9) . . . . ? C27 C31 C36 C35 -177.7(5) . . . . ? C2 C3 N1 O7 1.2(6) . . . . ? C7 C3 N1 O7 -179.0(4) . . . . ? C14 C15 N2 O8 1.0(6) . . . . ? C19 C15 N2 O8 176.8(5) . . . . ? C26 C27 N3 O9 -0.2(6) . . . . ? C31 C27 N3 O9 -178.6(5) . . . . ? O7 C1 O1 Tb1 172.7(3) . . . . ? C2 C1 O1 Tb1 -10.6(9) . . . . ? C2 C4 O2 Tb1 -9.6(9) . . . . ? C5 C4 O2 Tb1 169.1(4) . . . . ? O8 C13 O3 Tb1 163.5(3) . . . . ? C14 C13 O3 Tb1 -18.2(9) . . . . ? C14 C16 O4 Tb1 -9.8(9) . . . . ? C17 C16 O4 Tb1 165.0(4) . . . . ? O9 C25 O5 Tb1 -168.3(3) . . . . ? C26 C25 O5 Tb1 13.4(9) . . . . ? C26 C28 O6 Tb1 1.9(10) . . . . ? C29 C28 O6 Tb1 178.8(4) . . . . ? O1 C1 O7 N1 178.8(5) . . . . ? C2 C1 O7 N1 1.5(6) . . . . ? C3 N1 O7 C1 -1.7(6) . . . . ? O3 C13 O8 N2 -179.7(4) . . . . ? C14 C13 O8 N2 1.6(6) . . . . ? C15 N2 O8 C13 -1.6(6) . . . . ? O5 C25 O9 N3 -178.7(5) . . . . ? C26 C25 O9 N3 0.0(6) . . . . ? C27 N3 O9 C25 0.1(6) . . . . ? C25 O5 Tb1 O1 -166.2(5) . . . . ? C25 O5 Tb1 O3 27.7(5) . . . . ? C25 O5 Tb1 O2 137.4(4) . . . . ? C25 O5 Tb1 O11 76.8(4) . . . . ? C25 O5 Tb1 O6 -8.2(4) . . . . ? C25 O5 Tb1 O4 -113.9(4) . . . . ? C25 O5 Tb1 O10 -85.2(4) . . . . ? C1 O1 Tb1 O5 -122.8(5) . . . . ? C1 O1 Tb1 O3 40.7(5) . . . . ? C1 O1 Tb1 O2 10.2(4) . . . . ? C1 O1 Tb1 O11 -56.7(5) . . . . ? C1 O1 Tb1 O6 -157.7(4) . . . . ? C1 O1 Tb1 O4 85.5(5) . . . . ? C1 O1 Tb1 O10 159.4(5) . . . . ? C13 O3 Tb1 O5 -139.5(4) . . . . ? C13 O3 Tb1 O1 64.8(5) . . . . ? C13 O3 Tb1 O2 94.7(4) . . . . ? C13 O3 Tb1 O11 172.3(5) . . . . ? C13 O3 Tb1 O6 -103.1(5) . . . . ? C13 O3 Tb1 O4 17.8(4) . . . . ? C13 O3 Tb1 O10 -42.4(5) . . . . ? C4 O2 Tb1 O5 56.1(6) . . . . ? C4 O2 Tb1 O1 -0.5(5) . . . . ? C4 O2 Tb1 O3 -163.5(6) . . . . ? C4 O2 Tb1 O11 116.2(6) . . . . ? C4 O2 Tb1 O6 166.4(5) . . . . ? C4 O2 Tb1 O4 -88.1(6) . . . . ? C4 O2 Tb1 O10 -48.3(6) . . . . ? C28 O6 Tb1 O5 1.5(6) . . . . ? C28 O6 Tb1 O1 36.3(7) . . . . ? C28 O6 Tb1 O3 -154.4(6) . . . . ? C28 O6 Tb1 O2 -123.5(6) . . . . ? C28 O6 Tb1 O11 -74.8(6) . . . . ? C28 O6 Tb1 O4 143.4(6) . . . . ? C28 O6 Tb1 O10 80.1(6) . . . . ? C16 O4 Tb1 O5 149.4(5) . . . . ? C16 O4 Tb1 O1 -160.8(6) . . . . ? C16 O4 Tb1 O3 -5.2(5) . . . . ? C16 O4 Tb1 O2 -86.6(6) . . . . ? C16 O4 Tb1 O11 -47.2(6) . . . . ? C16 O4 Tb1 O6 56.4(6) . . . . ? C16 O4 Tb1 O10 120.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.953 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.237 # end Validation Reply Form # Attachment 'HIBPI.cif' data_bijujan14 _database_code_depnum_ccdc_archive 'CCDC 703223' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H13 N O3' _chemical_formula_sum 'C13 H13 N O3' _chemical_formula_weight 231.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall -p2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.244(5) _cell_length_b 8.813(5) _cell_length_c 16.888(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 2417.7(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3859 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 23.2 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9412 _exptl_absorpt_correction_T_max 0.9722 _exptl_absorpt_process_details '(SADABS, 1999)' _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 axs kappa apex2 CCD diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13770 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.77 _reflns_number_total 3086 _reflns_number_gt 1643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_structure_solution 'SIR92 (Altomare etal., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 32 (Farrugia, 1997)' _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^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3086 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1269 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _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 0.91384(10) 0.41667(19) 0.27450(8) 0.0697(5) Uani 1 1 d . . . H1 H 0.9384 0.3213 0.2752 0.084 Uiso 1 1 calc R . . C2 C 0.86054(12) 0.4584(2) 0.33409(9) 0.0850(6) Uani 1 1 d . . . H2 H 0.8491 0.3912 0.3751 0.102 Uiso 1 1 calc R . . C3 C 0.82424(12) 0.5995(2) 0.33296(10) 0.0884(6) Uani 1 1 d . . . H3 H 0.7880 0.6274 0.3730 0.106 Uiso 1 1 calc R . . C4 C 0.84147(12) 0.6991(2) 0.27285(11) 0.0829(5) Uani 1 1 d . . . H4 H 0.8173 0.7948 0.2724 0.100 Uiso 1 1 calc R . . C5 C 0.89428(10) 0.65764(18) 0.21333(9) 0.0656(4) Uani 1 1 d . . . H5 H 0.9055 0.7253 0.1725 0.079 Uiso 1 1 calc R . . C6 C 0.93086(8) 0.51692(15) 0.21345(7) 0.0513(4) Uani 1 1 d . . . C7 C 0.98953(8) 0.47387(15) 0.15059(7) 0.0519(4) Uani 1 1 d . . . C8 C 1.06318(9) 0.3661(2) 0.05206(9) 0.0653(4) Uani 1 1 d . . . C9 C 0.98899(7) 0.34804(16) 0.09701(7) 0.0496(3) Uani 1 1 d . . . C10 C 0.93455(8) 0.23591(16) 0.07845(7) 0.0533(4) Uani 1 1 d . . . C11 C 0.85129(8) 0.21011(16) 0.11212(8) 0.0533(4) Uani 1 1 d . . . H11 H 0.8407 0.2892 0.1516 0.064 Uiso 1 1 calc R . . C12 C 0.78642(10) 0.2228(3) 0.04787(10) 0.0904(6) Uani 1 1 d . . . H12A H 0.7908 0.3200 0.0225 0.136 Uiso 1 1 calc R . . H12B H 0.7327 0.2125 0.0710 0.136 Uiso 1 1 calc R . . H12C H 0.7947 0.1440 0.0094 0.136 Uiso 1 1 calc R . . C13 C 0.84730(11) 0.0568(2) 0.15340(11) 0.0905(6) Uani 1 1 d . . . H13A H 0.8562 -0.0225 0.1154 0.136 Uiso 1 1 calc R . . H13B H 0.7941 0.0442 0.1773 0.136 Uiso 1 1 calc R . . H13C H 0.8890 0.0519 0.1936 0.136 Uiso 1 1 calc R . . N1 N 1.05405(9) 0.55838(15) 0.14068(8) 0.0770(4) Uani 1 1 d . . . O1 O 1.10183(6) 0.49182(16) 0.07726(7) 0.0835(4) Uani 1 1 d . . . O2 O 1.09032(7) 0.28742(17) -0.00216(6) 0.0895(4) Uani 1 1 d . . . O3 O 0.95424(8) 0.13724(14) 0.02233(7) 0.0833(4) Uani 1 1 d . . . H3A H 1.0065(13) 0.166(2) 0.0040(11) 0.110(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0941(12) 0.0640(10) 0.0511(9) 0.0054(7) -0.0019(8) 0.0077(9) C2 0.1130(14) 0.0945(15) 0.0476(9) 0.0046(9) 0.0056(9) -0.0020(12) C3 0.0961(13) 0.1072(16) 0.0619(11) -0.0260(10) 0.0121(10) 0.0030(12) C4 0.0906(13) 0.0701(11) 0.0881(12) -0.0158(10) 0.0054(10) 0.0109(10) C5 0.0734(10) 0.0548(9) 0.0687(9) 0.0000(8) -0.0039(8) 0.0004(8) C6 0.0605(8) 0.0476(8) 0.0459(7) -0.0025(6) -0.0095(6) -0.0048(6) C7 0.0553(8) 0.0503(8) 0.0501(8) 0.0078(6) -0.0084(6) -0.0043(7) C8 0.0506(8) 0.0857(12) 0.0596(9) 0.0084(8) 0.0009(7) 0.0024(8) C9 0.0432(7) 0.0597(8) 0.0458(7) 0.0018(6) 0.0008(6) 0.0029(6) C10 0.0495(8) 0.0584(9) 0.0520(7) -0.0089(7) 0.0015(6) 0.0098(7) C11 0.0493(8) 0.0562(9) 0.0543(7) -0.0109(7) 0.0032(6) -0.0007(6) C12 0.0547(10) 0.1354(18) 0.0810(11) 0.0043(12) -0.0061(8) 0.0057(10) C13 0.0923(12) 0.0794(13) 0.0997(13) 0.0167(11) 0.0088(10) -0.0014(10) N1 0.0757(9) 0.0757(10) 0.0796(9) 0.0008(8) 0.0041(7) -0.0209(7) O1 0.0643(7) 0.0984(9) 0.0880(8) 0.0092(7) 0.0113(6) -0.0223(7) O2 0.0610(7) 0.1327(12) 0.0749(7) -0.0065(7) 0.0210(6) 0.0098(7) O3 0.0681(7) 0.0925(9) 0.0892(8) -0.0437(7) 0.0175(7) 0.0006(6) _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 C2 1.378(2) . ? C1 C6 1.386(2) . ? C1 H1 0.9300 . ? C2 C3 1.377(3) . ? C2 H2 0.9300 . ? C3 C4 1.371(3) . ? C3 H3 0.9300 . ? C4 C5 1.371(2) . ? C4 H4 0.9300 . ? C5 C6 1.375(2) . ? C5 H5 0.9300 . ? C6 C7 1.4762(18) . ? C7 N1 1.2967(17) . ? C7 C9 1.4313(19) . ? C8 O2 1.2301(19) . ? C8 O1 1.343(2) . ? C8 C9 1.4333(19) . ? C9 C10 1.363(2) . ? C10 O3 1.3254(16) . ? C10 C11 1.4847(19) . ? C11 C12 1.517(2) . ? C11 C13 1.522(2) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? N1 O1 1.4469(17) . ? O3 H3A 0.94(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.91(16) . . ? C2 C1 H1 120.0 . . ? C6 C1 H1 120.0 . . ? C3 C2 C1 120.02(16) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.09(16) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.99(17) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.65(16) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 119.33(14) . . ? C5 C6 C7 120.65(13) . . ? C1 C6 C7 120.00(13) . . ? N1 C7 C9 111.62(12) . . ? N1 C7 C6 117.84(13) . . ? C9 C7 C6 130.53(12) . . ? O2 C8 O1 122.24(15) . . ? O2 C8 C9 129.28(17) . . ? O1 C8 C9 108.47(14) . . ? C10 C9 C7 135.34(12) . . ? C10 C9 C8 120.29(13) . . ? C7 C9 C8 104.11(13) . . ? O3 C10 C9 118.92(13) . . ? O3 C10 C11 113.16(13) . . ? C9 C10 C11 127.89(12) . . ? C10 C11 C12 110.35(11) . . ? C10 C11 C13 110.50(12) . . ? C12 C11 C13 111.33(14) . . ? C10 C11 H11 108.2 . . ? C12 C11 H11 108.2 . . ? C13 C11 H11 108.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 N1 O1 107.23(12) . . ? C8 O1 N1 108.56(12) . . ? C10 O3 H3A 106.3(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.0(3) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 0.6(3) . . . . ? C3 C4 C5 C6 -0.5(3) . . . . ? C4 C5 C6 C1 0.0(2) . . . . ? C4 C5 C6 C7 -178.26(14) . . . . ? C2 C1 C6 C5 0.2(2) . . . . ? C2 C1 C6 C7 178.50(13) . . . . ? C5 C6 C7 N1 57.66(18) . . . . ? C1 C6 C7 N1 -120.63(16) . . . . ? C5 C6 C7 C9 -123.81(16) . . . . ? C1 C6 C7 C9 57.90(19) . . . . ? N1 C7 C9 C10 -173.62(15) . . . . ? C6 C7 C9 C10 7.8(3) . . . . ? N1 C7 C9 C8 0.18(15) . . . . ? C6 C7 C9 C8 -178.41(13) . . . . ? O2 C8 C9 C10 -4.2(2) . . . . ? O1 C8 C9 C10 174.30(13) . . . . ? O2 C8 C9 C7 -179.17(16) . . . . ? O1 C8 C9 C7 -0.65(15) . . . . ? C7 C9 C10 O3 178.09(14) . . . . ? C8 C9 C10 O3 5.1(2) . . . . ? C7 C9 C10 C11 0.2(3) . . . . ? C8 C9 C10 C11 -172.84(13) . . . . ? O3 C10 C11 C12 -59.91(17) . . . . ? C9 C10 C11 C12 118.09(17) . . . . ? O3 C10 C11 C13 63.65(17) . . . . ? C9 C10 C11 C13 -118.36(16) . . . . ? C9 C7 N1 O1 0.33(16) . . . . ? C6 C7 N1 O1 179.12(10) . . . . ? O2 C8 O1 N1 179.51(13) . . . . ? C9 C8 O1 N1 0.87(16) . . . . ? C7 N1 O1 C8 -0.76(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3A O2 0.94(2) 1.74(2) 2.6094(19) 153.4(18) . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.150 _refine_diff_density_min -0.134 _refine_diff_density_rms 0.033 # Attachment 'Compound 2.cif' data_bijutbibp1 _database_code_depnum_ccdc_archive 'CCDC 703224' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H44 N3 O11 Tb' _chemical_formula_weight 913.71 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 P21/c 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 8.756(1) _cell_length_b 38.268(3) _cell_length_c 12.162(2) _cell_angle_alpha 90.000 _cell_angle_beta 96.327(8) _cell_angle_gamma 90.000 _cell_volume 4050.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8786 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 29.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 1.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5523 _exptl_absorpt_correction_T_max 0.6859 _exptl_absorpt_process_details 'SADABS(Bruker, 1999)' _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 axs kappa apex2 CCD Diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 55338 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 61 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 34.91 _reflns_number_total 16522 _reflns_number_gt 11700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_structure_solution 'SIR92 (Altornare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)' _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. The hydrogen atoms of the coordinating water molecule(H10A, H10B) and that of the hydroxyl group of the ethanol(H11A) were located in the difference Fourier map. Positional coordinates of these atoms were restrained during refinement such that their bond distances and angles with the parent oxygen atoms remain chemically meaningfull. The restraints were: (water)O10-H10A, O10-H10B = 0.85(0.01)A\%, H10A...H10B = 1.39A\%, (hydroxyl)O11-H11A = 0.9(0.01)A\%. ; _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^)+(0.0468P)^2^+2.4403P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00144(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16522 _refine_ls_number_parameters 525 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _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 0.7276(4) 0.17526(8) 0.2677(3) 0.0423(7) Uani 1 1 d . . . C2 C 0.8715(4) 0.16336(8) 0.2409(3) 0.0401(6) Uani 1 1 d . . . C3 C 0.8908(4) 0.12876(9) 0.2055(3) 0.0437(7) Uani 1 1 d . . . C4 C 1.0161(4) 0.17965(9) 0.2303(3) 0.0449(7) Uani 1 1 d . . . C5 C 1.0768(4) 0.21508(10) 0.2595(3) 0.0507(8) Uani 1 1 d . . . C6 C 1.1434(6) 0.22180(12) 0.3647(4) 0.0703(12) Uani 1 1 d . . . H6 H 1.1418 0.2049 0.4196 0.084 Uiso 1 1 calc R . . C7 C 1.2135(6) 0.25392(15) 0.3890(5) 0.0889(17) Uani 1 1 d . . . H7 H 1.2588 0.2585 0.4603 0.107 Uiso 1 1 calc R . . C8 C 1.2161(6) 0.27858(13) 0.3087(7) 0.0930(19) Uani 1 1 d . . . H8 H 1.2644 0.2999 0.3251 0.112 Uiso 1 1 calc R . . C9 C 1.1501(8) 0.27244(14) 0.2069(6) 0.0992(19) Uani 1 1 d . . . H9 H 1.1502 0.2897 0.1529 0.119 Uiso 1 1 calc R . . C10 C 1.0812(6) 0.24060(13) 0.1809(5) 0.0789(14) Uani 1 1 d . . . H10 H 1.0371 0.2364 0.1090 0.095 Uiso 1 1 calc R . . C11 C 0.6942(4) 0.21373(9) 0.2874(4) 0.0570(10) Uani 1 1 d . . . H11 H 0.7853 0.2276 0.2760 0.068 Uiso 1 1 calc R . . C12 C 0.6615(10) 0.21739(13) 0.4079(5) 0.116(3) Uani 1 1 d . . . H12A H 0.6328 0.2411 0.4217 0.174 Uiso 1 1 calc R . . H12B H 0.7521 0.2114 0.4561 0.174 Uiso 1 1 calc R . . H12C H 0.5792 0.2020 0.4216 0.174 Uiso 1 1 calc R . . C13 C 0.5619(7) 0.22610(13) 0.2099(7) 0.107(2) Uani 1 1 d . . . H13A H 0.5901 0.2262 0.1358 0.160 Uiso 1 1 calc R . . H13B H 0.5342 0.2493 0.2300 0.160 Uiso 1 1 calc R . . H13C H 0.4760 0.2107 0.2138 0.160 Uiso 1 1 calc R . . C14 C 0.6272(3) 0.03788(7) 0.0620(2) 0.0343(6) Uani 1 1 d . . . C15 C 0.6870(3) 0.01037(7) 0.1320(3) 0.0346(6) Uani 1 1 d . . . C16 C 0.6835(4) 0.01095(8) 0.2478(3) 0.0405(6) Uani 1 1 d . . . C17 C 0.7356(3) -0.01513(7) 0.0567(3) 0.0366(6) Uani 1 1 d . . . C18 C 0.8150(4) -0.04924(8) 0.0768(3) 0.0396(6) Uani 1 1 d . . . C19 C 0.7384(4) -0.07826(9) 0.1081(4) 0.0555(9) Uani 1 1 d . . . H19 H 0.6346 -0.0768 0.1176 0.067 Uiso 1 1 calc R . . C20 C 0.8156(5) -0.10961(10) 0.1255(4) 0.0628(11) Uani 1 1 d . . . H20 H 0.7638 -0.1291 0.1483 0.075 Uiso 1 1 calc R . . C21 C 0.9668(6) -0.11234(11) 0.1097(4) 0.0669(11) Uani 1 1 d . . . H21 H 1.0182 -0.1335 0.1220 0.080 Uiso 1 1 calc R . . C22 C 1.0421(5) -0.08379(13) 0.0758(5) 0.0757(14) Uani 1 1 d . . . H22 H 1.1446 -0.0856 0.0632 0.091 Uiso 1 1 calc R . . C23 C 0.9671(4) -0.05212(10) 0.0600(4) 0.0590(10) Uani 1 1 d . . . H23 H 1.0198 -0.0327 0.0378 0.071 Uiso 1 1 calc R . . C24 C 0.7122(5) -0.02104(10) 0.3192(3) 0.0559(9) Uani 1 1 d . . . H24 H 0.7782 -0.0371 0.2830 0.067 Uiso 1 1 calc R . . C25 C 0.5579(7) -0.03887(15) 0.3278(5) 0.0939(17) Uani 1 1 d . . . H25A H 0.4943 -0.0239 0.3668 0.141 Uiso 1 1 calc R . . H25B H 0.5745 -0.0605 0.3671 0.141 Uiso 1 1 calc R . . H25C H 0.5080 -0.0434 0.2549 0.141 Uiso 1 1 calc R . . C26 C 0.7893(7) -0.01253(14) 0.4321(4) 0.0862(16) Uani 1 1 d . . . H26A H 0.8888 -0.0027 0.4258 0.129 Uiso 1 1 calc R . . H26B H 0.8006 -0.0335 0.4757 0.129 Uiso 1 1 calc R . . H26C H 0.7280 0.0040 0.4672 0.129 Uiso 1 1 calc R . . C27 C 0.7014(4) 0.11222(8) 0.5165(3) 0.0423(7) Uani 1 1 d . . . C28 C 0.5656(3) 0.12932(8) 0.5408(3) 0.0393(6) Uani 1 1 d . . . C29 C 0.4291(4) 0.12718(9) 0.4691(3) 0.0465(8) Uani 1 1 d . . . C30 C 0.5225(4) 0.14816(9) 0.6336(3) 0.0471(8) Uani 1 1 d . . . C31 C 0.6138(4) 0.15909(9) 0.7388(3) 0.0473(7) Uani 1 1 d . . . C32 C 0.5810(5) 0.14553(13) 0.8380(4) 0.0687(12) Uani 1 1 d . . . H32 H 0.5065 0.1282 0.8389 0.082 Uiso 1 1 calc R . . C33 C 0.6580(6) 0.15743(18) 0.9375(4) 0.0864(17) Uani 1 1 d . . . H33 H 0.6339 0.1483 1.0043 0.104 Uiso 1 1 calc R . . C34 C 0.7674(6) 0.18218(13) 0.9363(4) 0.0715(13) Uani 1 1 d . . . H34 H 0.8188 0.1901 1.0026 0.086 Uiso 1 1 calc R . . C35 C 0.8032(5) 0.19565(10) 0.8386(4) 0.0600(10) Uani 1 1 d . . . H35 H 0.8798 0.2125 0.8383 0.072 Uiso 1 1 calc R . . C36 C 0.7257(5) 0.18429(9) 0.7403(3) 0.0548(9) Uani 1 1 d . . . H36 H 0.7495 0.1938 0.6740 0.066 Uiso 1 1 calc R . . C37 C 0.8420(4) 0.10936(11) 0.5995(3) 0.0559(10) Uani 1 1 d . . . H37 H 0.8178 0.1198 0.6692 0.067 Uiso 1 1 calc R . . C38 C 0.8814(10) 0.07186(17) 0.6207(6) 0.148(4) Uani 1 1 d . . . H38A H 0.7953 0.0601 0.6463 0.222 Uiso 1 1 calc R . . H38B H 0.9683 0.0702 0.6759 0.222 Uiso 1 1 calc R . . H38C H 0.9060 0.0612 0.5535 0.222 Uiso 1 1 calc R . . C39 C 0.9701(7) 0.1298(3) 0.5594(6) 0.162(4) Uani 1 1 d . . . H39A H 1.0541 0.1312 0.6170 0.244 Uiso 1 1 calc R . . H39B H 0.9347 0.1529 0.5394 0.244 Uiso 1 1 calc R . . H39C H 1.0037 0.1185 0.4959 0.244 Uiso 1 1 calc R . . C40 C 0.2206(11) 0.0493(3) 0.2913(7) 0.176(5) Uani 1 1 d . . . H40A H 0.2715 0.0359 0.3523 0.211 Uiso 1 1 calc R . . H40B H 0.1942 0.0716 0.3224 0.211 Uiso 1 1 calc R . . C41 C 0.0853(8) 0.0330(3) 0.2623(6) 0.147(4) Uani 1 1 d . . . H41A H 0.0436 0.0406 0.1899 0.221 Uiso 1 1 calc R . . H41B H 0.0146 0.0386 0.3146 0.221 Uiso 1 1 calc R . . H41C H 0.1016 0.0082 0.2616 0.221 Uiso 1 1 calc R . . N1 N 1.1127(4) 0.15817(9) 0.1941(4) 0.0670(10) Uani 1 1 d . . . N2 N 0.7110(3) -0.00500(7) -0.0456(2) 0.0421(6) Uani 1 1 d . . . N3 N 0.3790(4) 0.15701(12) 0.6224(3) 0.0737(11) Uani 1 1 d . . . O1 O 0.6180(3) 0.15480(6) 0.2694(2) 0.0530(6) Uani 1 1 d . . . O2 O 0.8059(3) 0.10301(6) 0.1966(2) 0.0522(6) Uani 1 1 d . . . O3 O 1.0343(3) 0.12543(8) 0.1761(3) 0.0699(9) Uani 1 1 d . . . O4 O 0.5665(2) 0.06627(5) 0.07938(18) 0.0396(5) Uani 1 1 d . . . O5 O 0.6459(3) 0.03820(6) 0.29461(19) 0.0493(6) Uani 1 1 d . . . O6 O 0.6407(3) 0.02877(6) -0.04426(19) 0.0416(5) Uani 1 1 d . . . O7 O 0.3951(3) 0.11364(7) 0.3773(2) 0.0501(6) Uani 1 1 d . . . O8 O 0.7076(3) 0.09813(7) 0.4244(2) 0.0534(6) Uani 1 1 d . . . O9 O 0.3169(3) 0.14368(9) 0.5170(3) 0.0715(9) Uani 1 1 d . . . O10 O 0.3800(3) 0.12636(7) 0.1248(2) 0.0504(6) Uani 1 1 d D . . O11 O 0.3319(3) 0.05666(7) 0.2235(2) 0.0568(7) Uani 1 1 d D . . Tb1 Tb 0.560380(16) 0.094468(4) 0.252436(13) 0.03897(6) Uani 1 1 d . . . H11A H 0.337(7) 0.0373(9) 0.183(4) 0.11(2) Uiso 1 1 d D . . H10A H 0.322(4) 0.1158(12) 0.076(3) 0.096(19) Uiso 1 1 d D . . H10B H 0.328(4) 0.1391(11) 0.164(3) 0.085(16) 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 C1 0.0402(16) 0.0347(14) 0.0530(18) -0.0064(13) 0.0097(13) -0.0024(12) C2 0.0352(15) 0.0356(14) 0.0500(18) -0.0091(12) 0.0076(12) -0.0051(12) C3 0.0350(15) 0.0446(16) 0.0529(19) -0.0119(14) 0.0108(13) -0.0013(13) C4 0.0404(16) 0.0441(17) 0.0510(18) -0.0047(14) 0.0090(13) -0.0053(14) C5 0.0415(18) 0.0483(18) 0.063(2) -0.0029(16) 0.0114(16) -0.0093(14) C6 0.073(3) 0.061(3) 0.075(3) -0.009(2) 0.001(2) -0.015(2) C7 0.077(3) 0.080(4) 0.109(4) -0.034(3) 0.004(3) -0.022(3) C8 0.072(3) 0.053(3) 0.159(6) -0.023(3) 0.035(4) -0.025(2) C9 0.108(5) 0.062(3) 0.132(5) 0.014(3) 0.035(4) -0.024(3) C10 0.090(4) 0.066(3) 0.082(3) 0.014(2) 0.015(3) -0.016(3) C11 0.049(2) 0.0316(15) 0.094(3) -0.0128(17) 0.0271(19) -0.0060(14) C12 0.206(8) 0.047(3) 0.106(4) -0.024(3) 0.073(5) -0.014(4) C13 0.080(4) 0.050(3) 0.184(6) -0.007(3) -0.018(4) 0.018(2) C14 0.0273(12) 0.0324(13) 0.0429(15) -0.0078(11) 0.0017(11) -0.0048(10) C15 0.0302(13) 0.0290(12) 0.0436(16) -0.0052(11) -0.0011(11) 0.0002(10) C16 0.0410(16) 0.0345(14) 0.0448(17) -0.0030(12) -0.0015(13) 0.0018(12) C17 0.0277(13) 0.0318(13) 0.0496(17) -0.0084(12) 0.0010(11) -0.0026(10) C18 0.0370(15) 0.0345(14) 0.0461(17) -0.0091(12) -0.0013(12) 0.0016(12) C19 0.0378(17) 0.0371(17) 0.090(3) -0.0028(17) 0.0007(17) -0.0006(14) C20 0.061(2) 0.0343(17) 0.090(3) 0.0014(18) -0.006(2) 0.0004(16) C21 0.077(3) 0.042(2) 0.080(3) -0.0017(19) 0.004(2) 0.0251(19) C22 0.055(2) 0.067(3) 0.109(4) 0.013(3) 0.027(2) 0.026(2) C23 0.0428(19) 0.0473(19) 0.088(3) 0.0101(19) 0.0128(18) 0.0086(15) C24 0.077(3) 0.0425(18) 0.0465(19) 0.0015(15) -0.0022(17) 0.0107(17) C25 0.111(5) 0.073(3) 0.100(4) 0.021(3) 0.019(3) -0.021(3) C26 0.123(5) 0.073(3) 0.056(3) 0.001(2) -0.019(3) 0.025(3) C27 0.0384(16) 0.0377(15) 0.0510(18) -0.0119(13) 0.0056(13) 0.0008(12) C28 0.0345(14) 0.0381(14) 0.0465(17) -0.0093(12) 0.0094(12) -0.0012(12) C29 0.0320(15) 0.0480(18) 0.061(2) -0.0115(15) 0.0129(14) -0.0004(13) C30 0.0413(17) 0.0460(17) 0.056(2) -0.0111(15) 0.0133(14) -0.0004(14) C31 0.0499(18) 0.0448(17) 0.0494(19) -0.0086(14) 0.0146(14) 0.0062(15) C32 0.060(3) 0.084(3) 0.064(3) 0.005(2) 0.017(2) -0.013(2) C33 0.076(3) 0.141(5) 0.044(2) 0.015(3) 0.014(2) 0.001(3) C34 0.076(3) 0.078(3) 0.057(3) -0.015(2) -0.005(2) 0.021(2) C35 0.072(3) 0.0371(17) 0.068(3) -0.0105(16) -0.002(2) 0.0027(17) C36 0.072(3) 0.0418(18) 0.051(2) -0.0010(15) 0.0082(18) -0.0031(17) C37 0.0413(18) 0.065(2) 0.059(2) -0.0228(18) -0.0071(16) 0.0123(17) C38 0.181(8) 0.093(4) 0.145(6) -0.046(4) -0.100(6) 0.080(5) C39 0.065(4) 0.320(13) 0.098(5) -0.009(6) -0.007(3) -0.079(6) C40 0.177(8) 0.214(10) 0.154(7) -0.080(7) 0.094(7) -0.129(8) C41 0.108(5) 0.216(10) 0.123(6) -0.016(6) 0.037(5) -0.078(6) N1 0.0413(17) 0.059(2) 0.104(3) -0.0215(19) 0.0234(17) -0.0132(15) N2 0.0408(14) 0.0329(12) 0.0525(16) -0.0099(11) 0.0043(12) 0.0008(10) N3 0.0504(19) 0.100(3) 0.072(2) -0.040(2) 0.0130(16) 0.008(2) O1 0.0391(12) 0.0344(11) 0.0878(19) -0.0114(11) 0.0167(12) -0.0019(10) O2 0.0406(12) 0.0398(12) 0.0779(17) -0.0244(11) 0.0142(12) -0.0074(10) O3 0.0425(14) 0.0626(17) 0.109(2) -0.0375(16) 0.0302(15) -0.0106(12) O4 0.0408(11) 0.0298(9) 0.0472(12) -0.0046(8) 0.0003(9) 0.0042(8) O5 0.0657(16) 0.0392(12) 0.0424(12) -0.0068(9) 0.0035(11) 0.0081(11) O6 0.0443(12) 0.0342(10) 0.0462(12) -0.0031(9) 0.0040(9) 0.0025(9) O7 0.0340(11) 0.0583(15) 0.0577(15) -0.0172(12) 0.0045(10) -0.0016(10) O8 0.0426(13) 0.0586(15) 0.0579(15) -0.0236(12) 0.0007(11) 0.0137(11) O9 0.0340(13) 0.106(2) 0.0752(19) -0.0377(17) 0.0097(12) 0.0081(14) O10 0.0435(13) 0.0446(13) 0.0625(16) -0.0080(11) 0.0039(12) 0.0080(11) O11 0.0537(15) 0.0538(15) 0.0654(17) -0.0177(13) 0.0174(12) -0.0187(12) Tb1 0.03363(8) 0.03200(8) 0.05147(10) -0.01002(6) 0.00558(6) 0.00045(6) _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 O1 1.241(4) . ? C1 C2 1.411(4) . ? C1 C11 1.525(4) . ? C2 C3 1.408(4) . ? C2 C4 1.430(5) . ? C3 O2 1.232(4) . ? C3 O3 1.350(4) . ? C4 N1 1.291(5) . ? C4 C5 1.485(5) . ? C5 C10 1.370(6) . ? C5 C6 1.370(6) . ? C6 C7 1.391(6) . ? C6 H6 0.9300 . ? C7 C8 1.360(9) . ? C7 H7 0.9300 . ? C8 C9 1.328(9) . ? C8 H8 0.9300 . ? C9 C10 1.381(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C13 1.488(7) . ? C11 C12 1.530(7) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 O4 1.238(3) . ? C14 O6 1.356(4) . ? C14 C15 1.418(4) . ? C15 C16 1.412(4) . ? C15 C17 1.435(4) . ? C16 O5 1.249(4) . ? C16 C24 1.507(5) . ? C17 N2 1.298(4) . ? C17 C18 1.486(4) . ? C18 C19 1.373(5) . ? C18 C23 1.375(5) . ? C19 C20 1.382(5) . ? C19 H19 0.9300 . ? C20 C21 1.363(6) . ? C20 H20 0.9300 . ? C21 C22 1.363(7) . ? C21 H21 0.9300 . ? C22 C23 1.382(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C26 1.498(6) . ? C24 C25 1.528(7) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O8 1.249(4) . ? C27 C28 1.417(4) . ? C27 C37 1.508(5) . ? C28 C29 1.402(5) . ? C28 C30 1.425(4) . ? C29 O7 1.237(4) . ? C29 O9 1.353(4) . ? C30 N3 1.294(5) . ? C30 C31 1.492(5) . ? C31 C32 1.372(6) . ? C31 C36 1.373(5) . ? C32 C33 1.395(7) . ? C32 H32 0.9300 . ? C33 C34 1.349(7) . ? C33 H33 0.9300 . ? C34 C35 1.363(7) . ? C34 H34 0.9300 . ? C35 C36 1.378(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.491(7) . ? C37 C39 1.493(8) . ? C37 H37 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.352(9) . ? C40 O11 1.373(7) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? N1 O3 1.434(4) . ? N2 O6 1.432(3) . ? N3 O9 1.430(5) . ? O1 Tb1 2.367(2) . ? O2 Tb1 2.347(3) . ? O4 Tb1 2.371(2) . ? O5 Tb1 2.319(2) . ? O7 Tb1 2.329(2) . ? O8 Tb1 2.337(3) . ? O10 Tb1 2.419(3) . ? O10 H10A 0.844(10) . ? O10 H10B 0.846(10) . ? O11 Tb1 2.463(3) . ? O11 H11A 0.892(10) . ? 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 O1 C1 C2 120.8(3) . . ? O1 C1 C11 116.4(3) . . ? C2 C1 C11 122.6(3) . . ? C3 C2 C1 121.0(3) . . ? C3 C2 C4 104.2(3) . . ? C1 C2 C4 134.6(3) . . ? O2 C3 O3 118.1(3) . . ? O2 C3 C2 133.4(3) . . ? O3 C3 C2 108.4(3) . . ? N1 C4 C2 111.9(3) . . ? N1 C4 C5 115.6(3) . . ? C2 C4 C5 132.3(3) . . ? C10 C5 C6 118.4(4) . . ? C10 C5 C4 121.4(4) . . ? C6 C5 C4 119.9(4) . . ? C5 C6 C7 119.8(5) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 120.1(5) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C7 120.4(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.2(6) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C5 C10 C9 121.0(5) . . ? C5 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C13 C11 C1 110.9(4) . . ? C13 C11 C12 111.3(5) . . ? C1 C11 C12 107.4(3) . . ? C13 C11 H11 109.1 . . ? C1 C11 H11 109.1 . . ? C12 C11 H11 109.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4 C14 O6 118.2(3) . . ? O4 C14 C15 133.3(3) . . ? O6 C14 C15 108.4(2) . . ? C16 C15 C14 122.7(3) . . ? C16 C15 C17 133.5(3) . . ? C14 C15 C17 103.7(3) . . ? O5 C16 C15 120.3(3) . . ? O5 C16 C24 116.8(3) . . ? C15 C16 C24 122.8(3) . . ? N2 C17 C15 112.3(3) . . ? N2 C17 C18 116.4(3) . . ? C15 C17 C18 131.2(3) . . ? C19 C18 C23 119.2(3) . . ? C19 C18 C17 121.5(3) . . ? C23 C18 C17 119.3(3) . . ? C18 C19 C20 120.0(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 120.8(4) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 119.4(4) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C23 120.5(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C18 C23 C22 120.2(4) . . ? C18 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C26 C24 C16 112.4(3) . . ? C26 C24 C25 110.3(4) . . ? C16 C24 C25 108.0(4) . . ? C26 C24 H24 108.7 . . ? C16 C24 H24 108.7 . . ? C25 C24 H24 108.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O8 C27 C28 120.5(3) . . ? O8 C27 C37 117.1(3) . . ? C28 C27 C37 122.4(3) . . ? C29 C28 C27 121.4(3) . . ? C29 C28 C30 103.9(3) . . ? C27 C28 C30 134.5(3) . . ? O7 C29 O9 118.0(3) . . ? O7 C29 C28 133.6(3) . . ? O9 C29 C28 108.4(3) . . ? N3 C30 C28 112.8(3) . . ? N3 C30 C31 116.1(3) . . ? C28 C30 C31 131.1(3) . . ? C32 C31 C36 118.2(4) . . ? C32 C31 C30 120.2(4) . . ? C36 C31 C30 121.5(3) . . ? C31 C32 C33 120.7(4) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 119.8(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.4(4) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 119.9(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C31 C36 C35 121.0(4) . . ? C31 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C38 C37 C39 113.1(6) . . ? C38 C37 C27 110.0(4) . . ? C39 C37 C27 109.3(4) . . ? C38 C37 H37 108.1 . . ? C39 C37 H37 108.1 . . ? C27 C37 H37 108.1 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 O11 126.6(7) . . ? C41 C40 H40A 105.7 . . ? O11 C40 H40A 105.7 . . ? C41 C40 H40B 105.7 . . ? O11 C40 H40B 105.7 . . ? H40A C40 H40B 106.1 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 N1 O3 106.7(3) . . ? C17 N2 O6 106.5(2) . . ? C30 N3 O9 105.7(3) . . ? C1 O1 Tb1 140.5(2) . . ? C3 O2 Tb1 130.4(2) . . ? C3 O3 N1 108.7(3) . . ? C14 O4 Tb1 127.1(2) . . ? C16 O5 Tb1 140.3(2) . . ? C14 O6 N2 109.0(2) . . ? C29 O7 Tb1 128.0(2) . . ? C27 O8 Tb1 138.9(2) . . ? C29 O9 N3 109.2(3) . . ? Tb1 O10 H10A 121(4) . . ? Tb1 O10 H10B 106(3) . . ? H10A O10 H10B 110.9(17) . . ? C40 O11 Tb1 130.8(4) . . ? C40 O11 H11A 104(4) . . ? Tb1 O11 H11A 118(4) . . ? O5 Tb1 O7 110.92(9) . . ? O5 Tb1 O8 74.03(8) . . ? O7 Tb1 O8 73.64(9) . . ? O5 Tb1 O2 84.82(9) . . ? O7 Tb1 O2 143.07(8) . . ? O8 Tb1 O2 79.53(10) . . ? O5 Tb1 O1 145.68(10) . . ? O7 Tb1 O1 77.15(9) . . ? O8 Tb1 O1 76.84(10) . . ? O2 Tb1 O1 72.32(8) . . ? O5 Tb1 O4 74.66(8) . . ? O7 Tb1 O4 143.01(8) . . ? O8 Tb1 O4 139.26(8) . . ? O2 Tb1 O4 72.28(8) . . ? O1 Tb1 O4 119.72(9) . . ? O5 Tb1 O10 141.49(9) . . ? O7 Tb1 O10 81.42(10) . . ? O8 Tb1 O10 143.19(8) . . ? O2 Tb1 O10 107.34(10) . . ? O1 Tb1 O10 71.44(9) . . ? O4 Tb1 O10 74.75(8) . . ? O5 Tb1 O11 73.94(10) . . ? O7 Tb1 O11 74.03(9) . . ? O8 Tb1 O11 121.49(10) . . ? O2 Tb1 O11 142.74(8) . . ? O1 Tb1 O11 138.36(9) . . ? O4 Tb1 O11 72.73(8) . . ? O10 Tb1 O11 75.05(10) . . ? 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 6.0(5) . . . . ? C11 C1 C2 C3 -169.4(4) . . . . ? O1 C1 C2 C4 179.0(4) . . . . ? C11 C1 C2 C4 3.6(6) . . . . ? C1 C2 C3 O2 -5.0(7) . . . . ? C4 C2 C3 O2 -179.8(4) . . . . ? C1 C2 C3 O3 174.4(3) . . . . ? C4 C2 C3 O3 -0.5(4) . . . . ? C3 C2 C4 N1 -0.4(5) . . . . ? C1 C2 C4 N1 -174.2(4) . . . . ? C3 C2 C4 C5 -175.9(4) . . . . ? C1 C2 C4 C5 10.3(7) . . . . ? N1 C4 C5 C10 84.1(5) . . . . ? C2 C4 C5 C10 -100.6(5) . . . . ? N1 C4 C5 C6 -89.6(5) . . . . ? C2 C4 C5 C6 85.7(6) . . . . ? C10 C5 C6 C7 -0.2(7) . . . . ? C4 C5 C6 C7 173.7(4) . . . . ? C5 C6 C7 C8 0.0(8) . . . . ? C6 C7 C8 C9 0.9(9) . . . . ? C7 C8 C9 C10 -1.5(10) . . . . ? C6 C5 C10 C9 -0.4(8) . . . . ? C4 C5 C10 C9 -174.2(5) . . . . ? C8 C9 C10 C5 1.3(9) . . . . ? O1 C1 C11 C13 -53.6(5) . . . . ? C2 C1 C11 C13 122.0(5) . . . . ? O1 C1 C11 C12 68.2(5) . . . . ? C2 C1 C11 C12 -116.2(5) . . . . ? O4 C14 C15 C16 1.3(5) . . . . ? O6 C14 C15 C16 -177.0(3) . . . . ? O4 C14 C15 C17 178.3(3) . . . . ? O6 C14 C15 C17 0.0(3) . . . . ? C14 C15 C16 O5 -9.9(5) . . . . ? C17 C15 C16 O5 174.2(3) . . . . ? C14 C15 C16 C24 165.5(3) . . . . ? C17 C15 C16 C24 -10.5(5) . . . . ? C16 C15 C17 N2 176.9(3) . . . . ? C14 C15 C17 N2 0.4(3) . . . . ? C16 C15 C17 C18 -6.9(5) . . . . ? C14 C15 C17 C18 176.6(3) . . . . ? N2 C17 C18 C19 -108.3(4) . . . . ? C15 C17 C18 C19 75.6(5) . . . . ? N2 C17 C18 C23 69.4(4) . . . . ? C15 C17 C18 C23 -106.7(4) . . . . ? C23 C18 C19 C20 2.0(6) . . . . ? C17 C18 C19 C20 179.7(4) . . . . ? C18 C19 C20 C21 -1.4(7) . . . . ? C19 C20 C21 C22 -0.3(7) . . . . ? C20 C21 C22 C23 1.5(8) . . . . ? C19 C18 C23 C22 -0.8(6) . . . . ? C17 C18 C23 C22 -178.5(4) . . . . ? C21 C22 C23 C18 -1.0(8) . . . . ? O5 C16 C24 C26 -37.2(5) . . . . ? C15 C16 C24 C26 147.3(4) . . . . ? O5 C16 C24 C25 84.8(4) . . . . ? C15 C16 C24 C25 -90.7(5) . . . . ? O8 C27 C28 C29 8.3(5) . . . . ? C37 C27 C28 C29 -170.2(4) . . . . ? O8 C27 C28 C30 -178.3(4) . . . . ? C37 C27 C28 C30 3.2(6) . . . . ? C27 C28 C29 O7 -3.7(6) . . . . ? C30 C28 C29 O7 -178.9(4) . . . . ? C27 C28 C29 O9 175.5(3) . . . . ? C30 C28 C29 O9 0.3(4) . . . . ? C29 C28 C30 N3 -0.4(5) . . . . ? C27 C28 C30 N3 -174.7(4) . . . . ? C29 C28 C30 C31 179.7(4) . . . . ? C27 C28 C30 C31 5.4(7) . . . . ? N3 C30 C31 C32 65.3(6) . . . . ? C28 C30 C31 C32 -114.9(5) . . . . ? N3 C30 C31 C36 -110.7(5) . . . . ? C28 C30 C31 C36 69.2(6) . . . . ? C36 C31 C32 C33 0.8(7) . . . . ? C30 C31 C32 C33 -175.3(4) . . . . ? C31 C32 C33 C34 -0.9(8) . . . . ? C32 C33 C34 C35 0.0(8) . . . . ? C33 C34 C35 C36 0.9(7) . . . . ? C32 C31 C36 C35 0.1(6) . . . . ? C30 C31 C36 C35 176.2(3) . . . . ? C34 C35 C36 C31 -1.0(6) . . . . ? O8 C27 C37 C38 -57.5(6) . . . . ? C28 C27 C37 C38 121.0(5) . . . . ? O8 C27 C37 C39 67.2(6) . . . . ? C28 C27 C37 C39 -114.2(6) . . . . ? C2 C4 N1 O3 1.0(5) . . . . ? C5 C4 N1 O3 177.3(3) . . . . ? C15 C17 N2 O6 -0.6(3) . . . . ? C18 C17 N2 O6 -177.4(2) . . . . ? C28 C30 N3 O9 0.3(5) . . . . ? C31 C30 N3 O9 -179.8(3) . . . . ? C2 C1 O1 Tb1 5.8(6) . . . . ? C11 C1 O1 Tb1 -178.5(3) . . . . ? O3 C3 O2 Tb1 173.3(3) . . . . ? C2 C3 O2 Tb1 -7.4(7) . . . . ? O2 C3 O3 N1 -179.4(4) . . . . ? C2 C3 O3 N1 1.1(4) . . . . ? C4 N1 O3 C3 -1.3(5) . . . . ? O6 C14 O4 Tb1 -169.26(18) . . . . ? C15 C14 O4 Tb1 12.5(5) . . . . ? C15 C16 O5 Tb1 3.6(5) . . . . ? C24 C16 O5 Tb1 -172.0(3) . . . . ? O4 C14 O6 N2 -179.0(2) . . . . ? C15 C14 O6 N2 -0.4(3) . . . . ? C17 N2 O6 C14 0.6(3) . . . . ? O9 C29 O7 Tb1 164.9(3) . . . . ? C28 C29 O7 Tb1 -15.9(6) . . . . ? C28 C27 O8 Tb1 8.4(6) . . . . ? C37 C27 O8 Tb1 -173.0(3) . . . . ? O7 C29 O9 N3 179.3(4) . . . . ? C28 C29 O9 N3 -0.1(5) . . . . ? C30 N3 O9 C29 -0.1(5) . . . . ? C41 C40 O11 Tb1 168.0(9) . . . . ? C16 O5 Tb1 O7 146.8(4) . . . . ? C16 O5 Tb1 O8 -148.3(4) . . . . ? C16 O5 Tb1 O2 -67.7(4) . . . . ? C16 O5 Tb1 O1 -115.3(4) . . . . ? C16 O5 Tb1 O4 5.3(4) . . . . ? C16 O5 Tb1 O10 43.8(4) . . . . ? C16 O5 Tb1 O11 81.4(4) . . . . ? C29 O7 Tb1 O5 84.5(3) . . . . ? C29 O7 Tb1 O8 19.3(3) . . . . ? C29 O7 Tb1 O2 -25.8(4) . . . . ? C29 O7 Tb1 O1 -60.5(3) . . . . ? C29 O7 Tb1 O4 176.6(3) . . . . ? C29 O7 Tb1 O10 -133.3(3) . . . . ? C29 O7 Tb1 O11 149.9(3) . . . . ? C27 O8 Tb1 O5 -136.1(4) . . . . ? C27 O8 Tb1 O7 -18.0(4) . . . . ? C27 O8 Tb1 O2 136.3(4) . . . . ? C27 O8 Tb1 O1 62.3(4) . . . . ? C27 O8 Tb1 O4 -177.2(3) . . . . ? C27 O8 Tb1 O10 31.3(5) . . . . ? C27 O8 Tb1 O11 -76.9(4) . . . . ? C3 O2 Tb1 O5 -143.0(3) . . . . ? C3 O2 Tb1 O7 -24.5(4) . . . . ? C3 O2 Tb1 O8 -68.3(3) . . . . ? C3 O2 Tb1 O1 11.1(3) . . . . ? C3 O2 Tb1 O4 141.5(4) . . . . ? C3 O2 Tb1 O10 74.4(4) . . . . ? C3 O2 Tb1 O11 162.3(3) . . . . ? C1 O1 Tb1 O5 38.9(5) . . . . ? C1 O1 Tb1 O7 147.3(4) . . . . ? C1 O1 Tb1 O8 71.4(4) . . . . ? C1 O1 Tb1 O2 -11.7(4) . . . . ? C1 O1 Tb1 O4 -68.3(4) . . . . ? C1 O1 Tb1 O10 -127.6(4) . . . . ? C1 O1 Tb1 O11 -165.7(4) . . . . ? C14 O4 Tb1 O5 -12.1(2) . . . . ? C14 O4 Tb1 O7 -116.7(2) . . . . ? C14 O4 Tb1 O8 28.8(3) . . . . ? C14 O4 Tb1 O2 77.3(2) . . . . ? C14 O4 Tb1 O1 133.9(2) . . . . ? C14 O4 Tb1 O10 -168.5(2) . . . . ? C14 O4 Tb1 O11 -89.7(2) . . . . ? C40 O11 Tb1 O5 97.2(8) . . . . ? C40 O11 Tb1 O7 -20.7(8) . . . . ? C40 O11 Tb1 O8 38.0(8) . . . . ? C40 O11 Tb1 O2 155.0(7) . . . . ? C40 O11 Tb1 O1 -68.7(8) . . . . ? C40 O11 Tb1 O4 175.8(8) . . . . ? C40 O11 Tb1 O10 -105.9(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11A N2 0.892(10) 2.09(3) 2.924(4) 156(5) 3_655 O10 H10B N1 0.846(10) 2.09(3) 2.847(4) 148(4) 1_455 _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.480 _refine_diff_density_min -1.148 _refine_diff_density_rms 0.124 _vrf_PLAT220_bijutbibp1 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.12 Ratio RESPONSE: Some of the the terminal carbons seems have mild unresolvable thermal disorder, which is making the Ueq(max)/Ueq(min ratio large. ; _vrf_PLAT241_bijutbibp1 ; PROBLEM: Check High Ueq as Compared to Neighbors for C40 RESPONSE: The carbons of the coordinating ethyl alcohol seems to have mild unresolvable thermal disorder. ; _vrf_PLAT242_bijutbibp1 ; PROBLEM: Check Low Ueq as Compared to Neighbors for O11 RESPONSE: The two methyl carbons seems to have mild unresolvable thermal disorder. ;