Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Henryk Kozlowski' 'Theodorine Bailly' 'Ramon Burgada' 'Joanna Galezowska' 'Rafal Janicki' 'Marc Lecouvey' 'Anna Mondry' _publ_contact_author_name 'Henryk Kozlowski' _publ_contact_author_address ; Faculty of Chemistry University of Wroclaw F Joliot-Curie 14 Wroclaw 50-383 POLAND ; _publ_contact_author_email HENRYKOZ@WCHUWR.CHEM.UNI.WROC.PL _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Co-ordination ability of trans-cyclohexane-1,2-diamine-N,N,N',N'-tetrakis-(methylenephosphonic acid) towards lanthanide(III) ions. ; # Attachment 'EUCDTMP.txt' data_eup _database_code_depnum_ccdc_archive 'CCDC 600968' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H124 Eu N20 O29.50 P4' _chemical_formula_weight 1345.19 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.982(9) _cell_length_b 13.280(12) _cell_length_c 17.569(15) _cell_angle_alpha 70.94(8) _cell_angle_beta 79.67(6) _cell_angle_gamma 71.97(7) _cell_volume 2712(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6493 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1438 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type 'analytical, from the crystal shape' _exptl_absorpt_correction_T_min 0.773 _exptl_absorpt_correction_T_max 0.868 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Kuma KM4 with a CCD counter' _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 18764 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.1086 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 28.55 _reflns_number_total 11872 _reflns_number_gt 8783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD ver. 1.171' _computing_cell_refinement 'CrysAlis RED ver. 1.171' _computing_data_reduction 'CrysAlis RED ver. 1.171' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11872 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1553 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu Eu 0.43117(2) 0.38924(3) 0.183262(18) 0.01665(10) Uani 1 d . . . P1 P 0.19472(12) 0.57667(13) 0.23111(9) 0.0168(3) Uani 1 d . . . P2 P 0.52894(12) 0.46867(13) 0.32202(9) 0.0184(3) Uani 1 d . . . P3 P 0.27553(13) 0.20954(13) 0.19556(9) 0.0192(3) Uani 1 d . . . P4 P 0.64078(13) 0.14435(14) 0.21913(10) 0.0225(4) Uani 1 d . . . O1 O 0.2906(3) 0.5525(3) 0.1676(2) 0.0197(9) Uani 1 d . . . O2 O 0.0861(3) 0.5829(3) 0.2060(2) 0.0199(9) Uani 1 d . . . O3 O 0.1924(3) 0.6774(3) 0.2546(3) 0.0230(9) Uani 1 d . . . O4 O 0.5493(3) 0.5784(3) 0.3154(2) 0.0224(9) Uani 1 d . . . O5 O 0.5479(3) 0.4421(4) 0.2406(2) 0.0259(10) Uani 1 d . . . O6 O 0.5937(3) 0.3734(4) 0.3866(3) 0.0239(10) Uani 1 d . . . O7 O 0.7502(3) 0.1306(4) 0.2469(3) 0.0274(10) Uani 1 d . . . O8 O 0.6440(3) 0.0533(4) 0.1839(3) 0.0270(10) Uani 1 d . . . O9 O 0.5942(3) 0.2579(4) 0.1614(3) 0.0255(10) Uani 1 d . . . O10 O 0.3009(4) 0.3205(4) 0.1560(3) 0.0386(13) Uani 1 d . . . O11 O 0.1689(3) 0.2191(4) 0.2481(3) 0.0293(11) Uani 1 d . . . O12 O 0.2812(3) 0.1474(3) 0.1346(2) 0.0218(9) Uani 1 d . . . C1 C 0.2235(4) 0.4542(5) 0.3191(4) 0.0183(12) Uani 1 d . . . H1A H 0.1852 0.4741 0.3671 0.022 Uiso 1 calc R . . H1B H 0.1951 0.3982 0.3127 0.022 Uiso 1 calc R . . C2 C 0.3842(4) 0.4865(5) 0.3507(4) 0.0174(12) Uani 1 d . . . H2A H 0.3705 0.4781 0.4083 0.021 Uiso 1 calc R . . H2B H 0.3451 0.5611 0.3227 0.021 Uiso 1 calc R . . C3 C 0.3638(5) 0.2978(4) 0.3964(3) 0.0186(13) Uani 1 d . . . H3 H 0.4391 0.2810 0.4087 0.022 Uiso 1 calc R . . C4 C 0.2911(5) 0.3023(5) 0.4759(3) 0.0215(13) Uani 1 d . . . H4A H 0.3030 0.3582 0.4951 0.026 Uiso 1 calc R . . H4B H 0.2155 0.3249 0.4646 0.026 Uiso 1 calc R . . C5 C 0.3120(5) 0.1921(5) 0.5432(3) 0.0240(14) Uani 1 d . . . H5A H 0.3851 0.1725 0.5592 0.029 Uiso 1 calc R . . H5B H 0.2611 0.1996 0.5900 0.029 Uiso 1 calc R . . C6 C 0.2992(5) 0.1028(6) 0.5142(4) 0.0276(15) Uani 1 d . . . H6A H 0.2248 0.1199 0.5016 0.033 Uiso 1 calc R . . H6B H 0.3148 0.0329 0.5564 0.033 Uiso 1 calc R . . C7 C 0.3767(5) 0.0930(5) 0.4389(4) 0.0201(13) Uani 1 d . . . H7A H 0.3677 0.0349 0.4207 0.024 Uiso 1 calc R . . H7B H 0.4510 0.0721 0.4526 0.024 Uiso 1 calc R . . C8 C 0.3564(5) 0.2024(5) 0.3692(3) 0.0167(12) Uani 1 d . . . H8 H 0.2816 0.2198 0.3558 0.020 Uiso 1 calc R . . C9 C 0.3908(5) 0.1282(5) 0.2532(3) 0.0204(13) Uani 1 d . . . H9A H 0.3714 0.0659 0.2941 0.025 Uiso 1 calc R . . H9B H 0.4502 0.0990 0.2174 0.025 Uiso 1 calc R . . C10 C 0.5453(5) 0.1375(5) 0.3100(4) 0.0229(14) Uani 1 d . . . H10A H 0.5527 0.0604 0.3401 0.027 Uiso 1 calc R . . H10B H 0.5653 0.1721 0.3439 0.027 Uiso 1 calc R . . N1 N 0.3411(4) 0.4058(4) 0.3318(3) 0.0166(10) Uani 1 d . . . N2 N 0.4297(4) 0.1916(4) 0.2939(3) 0.0169(10) Uani 1 d . . . C20 C 0.3607(5) 0.7955(5) 0.0410(4) 0.0225(13) Uani 1 d . . . C30 C 0.8023(5) 0.5045(5) 0.4080(4) 0.0237(14) Uani 1 d . . . C40 C 0.8206(5) 0.4204(6) 0.1275(4) 0.0298(15) Uani 1 d . . . C50 C 0.9924(5) 0.1670(5) 0.1276(4) 0.0232(14) Uani 1 d . . . C60 C 0.3883(5) 0.7632(5) 0.4068(4) 0.0267(15) Uani 1 d . . . C70 C 0.6456(6) 0.7190(6) 0.0856(6) 0.046(2) Uani 1 d . . . N71 N 0.6852(5) 0.7991(6) 0.0390(4) 0.0479(19) Uani 1 d . . . H71A H 0.6894 0.8130 -0.0126 0.058 Uiso 1 calc R . . H71B H 0.7072 0.8383 0.0598 0.058 Uiso 1 calc R . . N72 N 0.6119(7) 0.6587(9) 0.0563(12) 0.227(11) Uani 1 d . . . H72A H 0.6154 0.6712 0.0048 0.272 Uiso 1 calc R . . H72B H 0.5859 0.6060 0.0882 0.272 Uiso 1 calc R . . N73 N 0.6386(6) 0.7024(7) 0.1633(6) 0.095(4) Uani 1 d . . . H73A H 0.6113 0.6510 0.1957 0.114 Uiso 1 calc R . . H73B H 0.6612 0.7430 0.1824 0.114 Uiso 1 calc R . . N21 N 0.3294(4) 0.7267(4) 0.0147(3) 0.0232(12) Uani 1 d . . . H21A H 0.3377 0.7320 -0.0360 0.028 Uiso 1 calc R . . H21B H 0.3009 0.6771 0.0485 0.028 Uiso 1 calc R . . N22 N 0.3489(4) 0.7875(4) 0.1193(3) 0.0233(11) Uani 1 d . . . H22A H 0.3696 0.8318 0.1358 0.028 Uiso 1 calc R . . H22B H 0.3205 0.7381 0.1534 0.028 Uiso 1 calc R . . N23 N 0.4043(4) 0.8711(4) -0.0119(3) 0.0275(13) Uani 1 d . . . H23A H 0.4252 0.9156 0.0043 0.033 Uiso 1 calc R . . H23B H 0.4118 0.8759 -0.0625 0.033 Uiso 1 calc R . . N31 N 0.7628(4) 0.5735(5) 0.3404(3) 0.0293(13) Uani 1 d . . . H31A H 0.7947 0.6230 0.3110 0.035 Uiso 1 calc R . . H31B H 0.7050 0.5692 0.3256 0.035 Uiso 1 calc R . . N32 N 0.7506(4) 0.4286(5) 0.4537(3) 0.0289(13) Uani 1 d . . . H32A H 0.6924 0.4256 0.4385 0.035 Uiso 1 calc R . . H32B H 0.7756 0.3831 0.4980 0.035 Uiso 1 calc R . . N33 N 0.8916(4) 0.5091(5) 0.4327(3) 0.0290(13) Uani 1 d . . . H33A H 0.9247 0.5579 0.4042 0.035 Uiso 1 calc R . . H33B H 0.9161 0.4632 0.4771 0.035 Uiso 1 calc R . . N41 N 0.9090(4) 0.4487(6) 0.0900(4) 0.0389(16) Uani 1 d . . . H41A H 0.9556 0.4529 0.1172 0.047 Uiso 1 calc R . . H41B H 0.9202 0.4631 0.0383 0.047 Uiso 1 calc R . . N42 N 0.7495(5) 0.4151(5) 0.0828(5) 0.0444(17) Uani 1 d . . . H42A H 0.6909 0.3969 0.1059 0.053 Uiso 1 calc R . . H42B H 0.7626 0.4298 0.0312 0.053 Uiso 1 calc R . . N43 N 0.8030(5) 0.3986(5) 0.2057(4) 0.0429(16) Uani 1 d . . . H43A H 0.8494 0.4027 0.2332 0.052 Uiso 1 calc R . . H43B H 0.7450 0.3801 0.2299 0.052 Uiso 1 calc R . . N51 N 0.9985(4) 0.1603(5) 0.2042(3) 0.0309(13) Uani 1 d . . . H51A H 1.0558 0.1670 0.2180 0.037 Uiso 1 calc R . . H51B H 0.9451 0.1493 0.2398 0.037 Uiso 1 calc R . . N52 N 0.9039(4) 0.1574(5) 0.1065(4) 0.0319(14) Uani 1 d . . . H52A H 0.8997 0.1622 0.0571 0.038 Uiso 1 calc R . . H52B H 0.8506 0.1464 0.1421 0.038 Uiso 1 calc R . . N53 N 1.0749(4) 0.1839(5) 0.0736(3) 0.0293(13) Uani 1 d . . . H53A H 1.0714 0.1888 0.0240 0.035 Uiso 1 calc R . . H53B H 1.1321 0.1901 0.0879 0.035 Uiso 1 calc R . . N61 N 0.4617(4) 0.6774(4) 0.4473(3) 0.0275(12) Uani 1 d . . . H61A H 0.5092 0.6350 0.4223 0.033 Uiso 1 calc R . . H61B H 0.4620 0.6641 0.4986 0.033 Uiso 1 calc R . . N62 N 0.3898(4) 0.7815(5) 0.3279(3) 0.0257(12) Uani 1 d . . . H62A H 0.4379 0.7381 0.3040 0.031 Uiso 1 calc R . . H62B H 0.3428 0.8368 0.3006 0.031 Uiso 1 calc R . . N63 N 0.3169(5) 0.8295(5) 0.4457(3) 0.0313(13) Uani 1 d . . . H63A H 0.3185 0.8167 0.4968 0.038 Uiso 1 calc R . . H63B H 0.2689 0.8854 0.4198 0.038 Uiso 1 calc R . . OH1 O 0.5215(6) 0.5005(7) 0.0741(5) 0.0204(18) Uiso 0.50 d P . . OH2 O 0.4869(6) 0.4751(7) 0.0442(5) 0.0202(18) Uiso 0.50 d P . . OW1 O 0.4124(7) 0.4363(7) 0.0378(5) 0.0242(19) Uiso 0.50 d P . . OW2 O -0.0197(6) 0.7620(7) 0.0887(4) 0.101(3) Uani 1 d . . . OW3 O 0.0828(3) 0.8872(3) 0.1923(3) 0.0242(10) Uani 1 d . . . OW4 O 0.2296(4) 0.9571(4) 0.2380(3) 0.0312(11) Uani 1 d . . . OW5 O 0.9124(4) 0.7012(4) 0.2935(3) 0.0419(13) Uani 1 d . . . OW6 O 0.8897(3) -0.0807(4) 0.2955(3) 0.0281(10) Uani 1 d . . . OW7 O 0.0031(4) 0.3925(4) 0.2654(3) 0.0308(11) Uani 1 d . . . OW8 O 0.1295(4) 0.4885(4) 0.0796(3) 0.0347(12) Uani 1 d . . . OW9 O 0.7642(4) 0.2009(4) 0.3742(3) 0.0322(11) Uani 1 d . . . OW10 O 0.4485(4) -0.0326(4) 0.1099(3) 0.0411(13) Uani 1 d . . . OW11 O 0.7895(4) -0.0796(5) 0.0990(3) 0.0517(15) Uani 1 d . . . OW12 O 0.0022(4) 0.1271(4) 0.5654(3) 0.0402(13) Uani 1 d . . . OW13 O 0.9011(4) 0.0591(4) -0.0243(3) 0.0428(13) Uani 1 d . . . OW14 O 0.1170(5) 0.6687(4) 0.4132(3) 0.0515(15) Uani 1 d . . . OW15 O 0.8699(4) -0.0146(4) 0.6204(3) 0.0421(13) Uani 1 d . . . OW16 O -0.0303(4) 0.2086(4) 0.4017(3) 0.0385(12) Uani 1 d . . . OW17 O 0.5918(6) -0.1338(6) 0.2380(5) 0.083(2) Uani 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 Eu 0.01458(16) 0.01827(16) 0.01611(16) -0.00409(11) 0.00119(10) -0.00542(12) P1 0.0144(7) 0.0152(8) 0.0181(8) -0.0020(6) -0.0027(6) -0.0025(6) P2 0.0163(8) 0.0237(8) 0.0153(7) -0.0064(6) -0.0021(6) -0.0042(7) P3 0.0206(8) 0.0157(8) 0.0212(8) -0.0032(6) -0.0042(6) -0.0055(6) P4 0.0181(8) 0.0223(9) 0.0225(8) -0.0074(7) 0.0027(6) -0.0005(7) O1 0.019(2) 0.017(2) 0.018(2) -0.0004(17) -0.0010(16) -0.0026(18) O2 0.015(2) 0.022(2) 0.021(2) -0.0044(18) -0.0028(16) -0.0038(18) O3 0.029(2) 0.012(2) 0.030(2) -0.0047(18) -0.0103(19) -0.0032(18) O4 0.022(2) 0.021(2) 0.022(2) -0.0023(18) -0.0015(17) -0.0083(18) O5 0.014(2) 0.050(3) 0.021(2) -0.019(2) 0.0012(17) -0.010(2) O6 0.025(2) 0.023(2) 0.025(2) -0.0070(19) -0.0102(18) -0.0037(19) O7 0.014(2) 0.033(3) 0.032(3) -0.013(2) 0.0000(18) -0.0005(19) O8 0.028(2) 0.021(2) 0.028(2) -0.0100(19) 0.0014(19) -0.001(2) O9 0.020(2) 0.023(2) 0.021(2) -0.0013(19) 0.0020(18) 0.0032(19) O10 0.052(3) 0.018(2) 0.052(3) 0.002(2) -0.033(3) -0.015(2) O11 0.022(2) 0.037(3) 0.034(3) -0.021(2) -0.0011(19) -0.004(2) O12 0.022(2) 0.025(2) 0.021(2) -0.0075(18) 0.0022(17) -0.0113(19) C1 0.013(3) 0.017(3) 0.025(3) -0.007(2) 0.000(2) -0.004(2) C2 0.017(3) 0.018(3) 0.020(3) -0.006(2) -0.001(2) -0.008(2) C3 0.020(3) 0.008(3) 0.021(3) -0.002(2) 0.002(2) 0.000(2) C4 0.022(3) 0.024(3) 0.018(3) -0.008(3) 0.002(2) -0.006(3) C5 0.026(3) 0.028(4) 0.011(3) -0.003(3) 0.001(2) -0.002(3) C6 0.021(3) 0.028(4) 0.022(3) 0.007(3) 0.003(3) -0.007(3) C7 0.021(3) 0.013(3) 0.023(3) -0.003(2) -0.005(2) 0.000(2) C8 0.018(3) 0.010(3) 0.020(3) -0.002(2) 0.001(2) -0.006(2) C9 0.024(3) 0.021(3) 0.014(3) -0.005(2) 0.001(2) -0.005(3) C10 0.019(3) 0.024(3) 0.021(3) -0.005(3) -0.003(2) 0.000(3) N1 0.017(2) 0.014(2) 0.016(2) -0.003(2) 0.0001(19) -0.002(2) N2 0.016(2) 0.016(2) 0.016(2) -0.007(2) 0.0025(19) 0.000(2) C20 0.019(3) 0.015(3) 0.029(3) -0.002(3) -0.001(3) -0.003(3) C30 0.021(3) 0.030(4) 0.026(3) -0.015(3) 0.001(3) -0.008(3) C40 0.017(3) 0.023(4) 0.044(4) -0.010(3) -0.003(3) 0.001(3) C50 0.014(3) 0.028(4) 0.024(3) -0.004(3) -0.004(2) -0.002(3) C60 0.020(3) 0.023(3) 0.034(4) 0.001(3) -0.003(3) -0.009(3) C70 0.020(4) 0.028(4) 0.096(7) -0.030(5) -0.003(4) -0.003(3) N71 0.035(4) 0.083(6) 0.022(3) -0.012(3) 0.002(3) -0.018(4) N72 0.059(6) 0.119(9) 0.60(3) -0.251(16) -0.160(12) 0.066(6) N73 0.053(5) 0.062(6) 0.084(7) 0.044(5) 0.034(5) 0.013(4) N21 0.026(3) 0.020(3) 0.022(3) -0.003(2) 0.002(2) -0.010(2) N22 0.025(3) 0.020(3) 0.027(3) -0.006(2) -0.002(2) -0.009(2) N23 0.035(3) 0.028(3) 0.024(3) -0.005(2) 0.000(2) -0.020(3) N31 0.022(3) 0.037(3) 0.029(3) -0.006(3) -0.002(2) -0.013(3) N32 0.033(3) 0.035(3) 0.022(3) -0.003(2) -0.005(2) -0.019(3) N33 0.021(3) 0.036(3) 0.032(3) -0.011(3) -0.006(2) -0.008(3) N41 0.026(3) 0.068(5) 0.028(3) -0.009(3) -0.002(2) -0.025(3) N42 0.022(3) 0.037(4) 0.077(5) -0.012(3) -0.021(3) -0.007(3) N43 0.042(4) 0.042(4) 0.044(4) -0.013(3) 0.015(3) -0.020(3) N51 0.021(3) 0.040(4) 0.029(3) -0.010(3) 0.004(2) -0.009(3) N52 0.016(3) 0.047(4) 0.034(3) -0.014(3) -0.004(2) -0.005(3) N53 0.015(3) 0.041(4) 0.028(3) -0.009(3) 0.002(2) -0.006(3) N61 0.031(3) 0.028(3) 0.021(3) -0.001(2) -0.011(2) -0.005(3) N62 0.029(3) 0.026(3) 0.015(3) -0.002(2) -0.001(2) -0.003(2) N63 0.044(4) 0.025(3) 0.019(3) -0.001(2) 0.000(2) -0.010(3) OW2 0.105(6) 0.098(6) 0.035(4) -0.009(4) -0.019(4) 0.061(5) OW3 0.020(2) 0.022(2) 0.029(2) -0.0082(19) -0.0010(18) -0.0032(19) OW4 0.030(3) 0.028(3) 0.031(3) 0.004(2) -0.005(2) -0.013(2) OW5 0.026(3) 0.041(3) 0.064(4) -0.023(3) 0.015(2) -0.020(2) OW6 0.021(2) 0.026(3) 0.034(3) -0.008(2) 0.0001(19) -0.004(2) OW7 0.025(2) 0.027(3) 0.043(3) -0.013(2) 0.004(2) -0.011(2) OW8 0.035(3) 0.030(3) 0.039(3) -0.010(2) -0.021(2) 0.000(2) OW9 0.024(2) 0.029(3) 0.043(3) -0.013(2) -0.002(2) -0.005(2) OW10 0.036(3) 0.041(3) 0.057(3) -0.031(3) 0.012(2) -0.018(2) OW11 0.045(3) 0.050(4) 0.053(4) -0.024(3) 0.003(3) 0.003(3) OW12 0.030(3) 0.043(3) 0.048(3) -0.019(3) -0.007(2) -0.002(2) OW13 0.038(3) 0.045(3) 0.041(3) -0.012(3) -0.005(2) -0.004(3) OW14 0.070(4) 0.036(3) 0.033(3) -0.008(2) -0.015(3) 0.011(3) OW15 0.036(3) 0.042(3) 0.036(3) 0.002(2) -0.001(2) -0.010(3) OW16 0.041(3) 0.037(3) 0.034(3) -0.004(2) -0.008(2) -0.010(2) OW17 0.064(4) 0.060(5) 0.103(6) -0.010(4) 0.025(4) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu O1 2.334(5) . yes Eu O10 2.335(5) . yes Eu O5 2.340(4) . yes Eu O9 2.351(5) . yes Eu OH1 2.377(8) . yes Eu OH2 2.418(8) . yes Eu OW1 2.463(9) . yes Eu N1 2.710(5) . yes Eu N2 2.711(6) . yes Eu P1 3.469(4) . no Eu P4 3.489(4) . no Eu P2 3.505(3) . no P1 O3 1.514(5) . no P1 O2 1.522(4) . no P1 O1 1.545(4) . no P1 C1 1.835(6) . no P2 O4 1.525(5) . no P2 O6 1.530(5) . no P2 O5 1.543(5) . no P2 C2 1.817(6) . no P3 O11 1.515(5) . no P3 O10 1.521(5) . no P3 O12 1.531(5) . no P3 C9 1.806(6) . no P4 O8 1.515(5) . no P4 O7 1.523(5) . no P4 O9 1.525(5) . no P4 C10 1.833(6) . no C1 N1 1.489(7) . no C2 N1 1.497(7) . no C3 N1 1.493(7) . no C3 C8 1.525(8) . no C3 C4 1.547(8) . no C4 C5 1.533(8) . no C5 C6 1.497(9) . no C6 C7 1.527(9) . no C7 C8 1.548(8) . no C8 N2 1.505(7) . no C9 N2 1.503(8) . no C10 N2 1.484(7) . no C20 N23 1.321(7) . no C20 N22 1.329(8) . no C20 N21 1.337(8) . no C30 N31 1.316(8) . no C30 N33 1.332(8) . no C30 N32 1.344(8) . no C40 N43 1.301(9) . no C40 N41 1.314(8) . no C40 N42 1.345(9) . no C50 N53 1.320(8) . no C50 N52 1.323(8) . no C50 N51 1.334(8) . no C60 N61 1.324(8) . no C60 N62 1.324(8) . no C60 N63 1.328(9) . no C70 N72 1.291(11) . no C70 N71 1.298(10) . no C70 N73 1.301(13) . no OH1 OH2 0.942(10) . no OH2 OW1 1.264(11) . no OH2 OH2 1.499(16) 2_665 no 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 Eu O10 83.63(17) . . yes O1 Eu O5 96.89(17) . . yes O10 Eu O5 167.21(16) . . yes O1 Eu O9 162.22(14) . . yes O10 Eu O9 102.30(18) . . yes O5 Eu O9 81.04(17) . . yes O1 Eu OH1 83.6(2) . . yes O10 Eu OH1 119.1(2) . . yes O5 Eu OH1 73.6(2) . . yes O9 Eu OH1 78.9(2) . . yes O1 Eu OH2 83.9(2) . . yes O10 Eu OH2 96.8(2) . . yes O5 Eu OH2 96.0(2) . . yes O9 Eu OH2 78.8(2) . . yes OH1 Eu OH2 22.6(2) . . yes O1 Eu OW1 80.3(2) . . yes O10 Eu OW1 66.8(2) . . yes O5 Eu OW1 126.0(2) . . yes O9 Eu OW1 86.6(2) . . yes OH1 Eu OW1 52.4(3) . . yes OH2 Eu OW1 30.0(3) . . yes O1 Eu N1 71.44(16) . . yes O10 Eu N1 96.92(18) . . yes O5 Eu N1 71.33(15) . . yes O9 Eu N1 123.59(16) . . yes OH1 Eu N1 133.5(2) . . yes OH2 Eu N1 150.2(2) . . yes OW1 Eu N1 148.9(2) . . yes O1 Eu N2 126.26(15) . . yes O10 Eu N2 70.45(17) . . yes O5 Eu N2 99.45(17) . . yes O9 Eu N2 71.33(16) . . yes OH1 Eu N2 150.2(2) . . yes OH2 Eu N2 143.5(2) . . yes OW1 Eu N2 125.7(2) . . yes N1 Eu N2 66.30(16) . . yes O1 Eu P1 21.21(10) . . no O10 Eu P1 79.68(15) . . no O5 Eu P1 96.17(13) . . no O9 Eu P1 175.54(11) . . no OH1 Eu P1 103.7(2) . . no OH2 Eu P1 105.1(2) . . no OW1 Eu P1 97.8(2) . . no N1 Eu P1 52.01(12) . . no N2 Eu P1 105.87(13) . . no O1 Eu P4 176.49(10) . . no O10 Eu P4 97.81(14) . . no O5 Eu P4 80.99(14) . . no O9 Eu P4 20.41(11) . . no OH1 Eu P4 98.5(2) . . no OH2 Eu P4 99.1(2) . . no OW1 Eu P4 103.2(2) . . no N1 Eu P4 105.17(13) . . no N2 Eu P4 51.75(12) . . no P1 Eu P4 155.88(5) . . no O1 Eu P2 87.72(13) . . no O10 Eu P2 147.81(14) . . no O5 Eu P2 20.34(10) . . no O9 Eu P2 95.32(14) . . no OH1 Eu P2 90.5(2) . . no OH2 Eu P2 113.1(2) . . no OW1 Eu P2 141.8(2) . . no N1 Eu P2 51.05(11) . . no N2 Eu P2 90.46(13) . . no P1 Eu P2 81.13(8) . . no P4 Eu P2 89.38(9) . . no O3 P1 O2 112.9(2) . . no O3 P1 O1 111.1(2) . . no O2 P1 O1 113.0(2) . . no O3 P1 C1 109.0(3) . . no O2 P1 C1 106.0(3) . . no O1 P1 C1 104.3(3) . . no O3 P1 Eu 124.12(18) . . no O2 P1 Eu 120.68(18) . . no O1 P1 Eu 33.14(15) . . no C1 P1 Eu 71.2(2) . . no O4 P2 O6 111.5(2) . . no O4 P2 O5 113.6(3) . . no O6 P2 O5 111.4(3) . . no O4 P2 C2 105.6(3) . . no O6 P2 C2 109.7(3) . . no O5 P2 C2 104.7(3) . . no O4 P2 Eu 130.33(18) . . no O6 P2 Eu 115.22(19) . . no O5 P2 Eu 31.81(15) . . no C2 P2 Eu 73.9(2) . . no O11 P3 O10 112.6(3) . . no O11 P3 O12 111.6(2) . . no O10 P3 O12 112.7(3) . . no O11 P3 C9 112.3(3) . . no O10 P3 C9 103.1(3) . . no O12 P3 C9 103.8(3) . . no O11 P3 Eu 118.5(2) . . no O10 P3 Eu 30.74(18) . . no O12 P3 Eu 126.81(17) . . no C9 P3 Eu 73.2(2) . . no O8 P4 O7 112.0(3) . . no O8 P4 O9 110.8(3) . . no O7 P4 O9 113.9(3) . . no O8 P4 C10 109.6(3) . . no O7 P4 C10 105.5(3) . . no O9 P4 C10 104.5(3) . . no O8 P4 Eu 120.79(19) . . no O7 P4 Eu 124.7(2) . . no O9 P4 Eu 32.52(16) . . no C10 P4 Eu 72.0(2) . . no P1 O1 Eu 125.6(2) . . no P2 O5 Eu 127.8(2) . . no P4 O9 Eu 127.1(2) . . no P3 O10 Eu 129.8(3) . . no N1 C1 P1 114.0(4) . . no N1 C2 P2 113.2(4) . . no N1 C3 C8 112.9(5) . . no N1 C3 C4 112.8(5) . . no C8 C3 C4 110.1(5) . . no C5 C4 C3 114.0(5) . . no C6 C5 C4 110.1(5) . . no C5 C6 C7 109.9(5) . . no C6 C7 C8 112.2(5) . . no N2 C8 C3 112.1(4) . . no N2 C8 C7 112.3(5) . . no C3 C8 C7 111.1(5) . . no N2 C9 P3 113.9(4) . . no N2 C10 P4 114.4(4) . . no C1 N1 C3 113.0(4) . . no C1 N1 C2 109.8(4) . . no C3 N1 C2 110.3(5) . . no C1 N1 Eu 102.5(3) . . no C3 N1 Eu 113.3(3) . . no C2 N1 Eu 107.6(3) . . no C10 N2 C9 110.0(5) . . no C10 N2 C8 112.8(5) . . no C9 N2 C8 109.6(4) . . no C10 N2 Eu 104.6(3) . . no C9 N2 Eu 106.4(3) . . no C8 N2 Eu 113.2(3) . . no N23 C20 N22 120.4(6) . . no N23 C20 N21 119.1(6) . . no N22 C20 N21 120.5(5) . . no N31 C30 N33 121.4(6) . . no N31 C30 N32 119.2(6) . . no N33 C30 N32 119.4(6) . . no N43 C40 N41 120.4(7) . . no N43 C40 N42 121.4(7) . . no N41 C40 N42 118.2(7) . . no N53 C50 N52 120.7(6) . . no N53 C50 N51 119.5(6) . . no N52 C50 N51 119.9(6) . . no N61 C60 N62 118.6(6) . . no N61 C60 N63 119.5(6) . . no N62 C60 N63 121.8(6) . . no N72 C70 N71 121.4(13) . . no N72 C70 N73 120.6(13) . . no N71 C70 N73 117.9(8) . . no OH2 OH1 Eu 81.1(7) . . no OH1 OH2 OW1 151.0(10) . . no OH1 OH2 OH2 109.1(11) . 2_665 no OW1 OH2 OH2 97.6(9) . 2_665 no OH1 OH2 Eu 76.2(7) . . no OW1 OH2 Eu 76.9(5) . . no OH2 OH2 Eu 174.5(9) 2_665 . no OH2 OW1 Eu 73.1(5) . . no _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 28.55 _diffrn_measured_fraction_theta_full 0.859 _refine_diff_density_max 3.874 _refine_diff_density_min -1.784 _refine_diff_density_rms 0.166 # Attachment 'TbCDTMP.txt' data_tbp1 _database_code_depnum_ccdc_archive 'CCDC 600969' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H124 N20 O29.50 P4 Tb' _chemical_formula_weight 1352.15 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.026(9) _cell_length_b 13.241(9) _cell_length_c 17.530(13) _cell_angle_alpha 71.05(6) _cell_angle_beta 79.57(6) _cell_angle_gamma 72.00(7) _cell_volume 2709(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7138 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1442 _exptl_absorpt_coefficient_mu 1.525 _exptl_absorpt_correction_type 'analytical, from the shape' _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.817 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Kuma KM4 with a CCD counter' _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 18459 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.1144 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 28.44 _reflns_number_total 11761 _reflns_number_gt 8887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 software 1999' _computing_cell_refinement 'Kuma KM4 software 1999' _computing_data_reduction 'Kuma KM4 software 2000' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11761 _refine_ls_number_parameters 631 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1739 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.025 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb Tb 0.43212(2) 0.38758(3) 0.18242(2) 0.02002(11) Uani 1 d . . . P1 P 0.19717(12) 0.57503(13) 0.22931(10) 0.0179(3) Uani 1 d . . . P2 P 0.52947(13) 0.46612(15) 0.32122(10) 0.0219(4) Uani 1 d . . . P3 P 0.27670(14) 0.20951(14) 0.19567(11) 0.0234(4) Uani 1 d . . . P4 P 0.64064(14) 0.14420(16) 0.21828(11) 0.0280(4) Uani 1 d . . . O1 O 0.2924(3) 0.5483(4) 0.1665(3) 0.0206(9) Uani 1 d . . . O2 O 0.0881(3) 0.5827(4) 0.2052(3) 0.0226(10) Uani 1 d . . . O3 O 0.1953(4) 0.6779(4) 0.2512(3) 0.0250(10) Uani 1 d . . . O4 O 0.5516(4) 0.5747(4) 0.3132(3) 0.0273(11) Uani 1 d . . . O5 O 0.5482(4) 0.4378(5) 0.2404(3) 0.0344(13) Uani 1 d . . . O6 O 0.5928(4) 0.3716(4) 0.3872(3) 0.0283(11) Uani 1 d . . . O7 O 0.7500(4) 0.1310(5) 0.2453(3) 0.0340(12) Uani 1 d . . . O8 O 0.6439(4) 0.0521(4) 0.1835(3) 0.0328(12) Uani 1 d . . . O9 O 0.5927(4) 0.2582(4) 0.1608(3) 0.0291(12) Uani 1 d . . . O10 O 0.3028(5) 0.3199(4) 0.1559(4) 0.0404(14) Uani 1 d . . . O11 O 0.1702(4) 0.2195(5) 0.2482(3) 0.0360(13) Uani 1 d . . . O12 O 0.2816(4) 0.1466(4) 0.1347(3) 0.0262(10) Uani 1 d . . . C1 C 0.2226(5) 0.4549(5) 0.3192(4) 0.0200(13) Uani 1 d . . . H1A H 0.1857 0.4774 0.3667 0.024 Uiso 1 calc R . . H1B H 0.1924 0.3990 0.3145 0.024 Uiso 1 calc R . . C2 C 0.3840(5) 0.4868(6) 0.3490(4) 0.0215(14) Uani 1 d . . . H2A H 0.3692 0.4802 0.4064 0.026 Uiso 1 calc R . . H2B H 0.3461 0.5612 0.3196 0.026 Uiso 1 calc R . . C3 C 0.3626(5) 0.2976(5) 0.3975(4) 0.0204(13) Uani 1 d . . . H3 H 0.4375 0.2808 0.4100 0.024 Uiso 1 calc R . . C4 C 0.2907(5) 0.3017(6) 0.4763(4) 0.0271(15) Uani 1 d . . . H4A H 0.2155 0.3241 0.4649 0.032 Uiso 1 calc R . . H4B H 0.3019 0.3583 0.4953 0.032 Uiso 1 calc R . . C5 C 0.3107(6) 0.1918(6) 0.5449(4) 0.0262(16) Uani 1 d . . . H5A H 0.3828 0.1727 0.5619 0.031 Uiso 1 calc R . . H5B H 0.2586 0.1997 0.5911 0.031 Uiso 1 calc R . . C6 C 0.2996(6) 0.1022(5) 0.5149(4) 0.0258(15) Uani 1 d . . . H6A H 0.2255 0.1185 0.5026 0.031 Uiso 1 calc R . . H6B H 0.3159 0.0320 0.5568 0.031 Uiso 1 calc R . . C7 C 0.3765(6) 0.0933(5) 0.4389(4) 0.0248(15) Uani 1 d . . . H7A H 0.3677 0.0350 0.4205 0.030 Uiso 1 calc R . . H7B H 0.4507 0.0727 0.4523 0.030 Uiso 1 calc R . . C8 C 0.3557(5) 0.2023(5) 0.3701(4) 0.0176(13) Uani 1 d . . . H8 H 0.2812 0.2192 0.3568 0.021 Uiso 1 calc R . . C9 C 0.3919(6) 0.1284(6) 0.2536(4) 0.0262(15) Uani 1 d . . . H9A H 0.3724 0.0661 0.2947 0.031 Uiso 1 calc R . . H9B H 0.4511 0.0988 0.2178 0.031 Uiso 1 calc R . . C10 C 0.5460(5) 0.1361(6) 0.3104(4) 0.0260(15) Uani 1 d . . . H10A H 0.5533 0.0588 0.3401 0.031 Uiso 1 calc R . . H10B H 0.5658 0.1706 0.3445 0.031 Uiso 1 calc R . . N1 N 0.3415(4) 0.4048(4) 0.3308(3) 0.0201(11) Uani 1 d . . . N2 N 0.4301(4) 0.1910(4) 0.2935(3) 0.0186(11) Uani 1 d . . . C20 C 0.3616(5) 0.7948(5) 0.0409(4) 0.0218(14) Uani 1 d . . . C30 C 0.8016(6) 0.5015(6) 0.4080(4) 0.0284(15) Uani 1 d . . . C40 C 0.8199(6) 0.4211(6) 0.1283(5) 0.0341(18) Uani 1 d . . . C50 C 0.9926(5) 0.1673(6) 0.1280(5) 0.0318(17) Uani 1 d . . . C60 C 0.3894(6) 0.7626(7) 0.4059(5) 0.0330(17) Uani 1 d . . . C70 C 0.6447(12) 0.7137(12) 0.1009(9) 0.027(4) Uiso 0.50 d PD A 1 N71 N 0.6852(12) 0.7837(13) 0.0392(8) 0.033(4) Uiso 0.50 d PD A 1 H71A H 0.6849 0.7825 -0.0095 0.039 Uiso 0.50 calc PR A 1 H71B H 0.7119 0.8305 0.0479 0.039 Uiso 0.50 calc PR A 1 N72 N 0.6022(10) 0.6393(10) 0.0931(8) 0.036(3) Uiso 0.50 d PD A 1 H72A H 0.5998 0.6344 0.0457 0.044 Uiso 0.50 calc PR A 1 H72B H 0.5770 0.5958 0.1353 0.044 Uiso 0.50 calc PR A 1 N73 N 0.6450(12) 0.7195(13) 0.1758(8) 0.048(4) Uiso 0.50 d PD A 1 H73A H 0.6710 0.7678 0.1827 0.057 Uiso 0.50 calc PR A 1 H73B H 0.6191 0.6749 0.2168 0.057 Uiso 0.50 calc PR A 1 C80 C 0.6467(11) 0.7244(11) 0.0720(8) 0.021(3) Uiso 0.50 d PD B 2 N81 N 0.6211(9) 0.6743(9) 0.0269(7) 0.025(2) Uiso 0.50 d PD B 2 H81A H 0.5963 0.6174 0.0495 0.030 Uiso 0.50 calc PR B 2 H81B H 0.6292 0.6987 -0.0251 0.030 Uiso 0.50 calc PR B 2 N82 N 0.6343(10) 0.6872(11) 0.1528(8) 0.033(3) Uiso 0.50 d PD B 2 H82A H 0.6096 0.6303 0.1757 0.040 Uiso 0.50 calc PR B 2 H82B H 0.6512 0.7201 0.1818 0.040 Uiso 0.50 calc PR B 2 N83 N 0.6837(11) 0.8143(12) 0.0370(8) 0.027(4) Uiso 0.50 d PD B 2 H83A H 0.6908 0.8395 -0.0149 0.032 Uiso 0.50 calc PR B 2 H83B H 0.7003 0.8468 0.0664 0.032 Uiso 0.50 calc PR B 2 N21 N 0.3303(4) 0.7253(5) 0.0162(4) 0.0253(12) Uani 1 d . . . H21A H 0.3381 0.7296 -0.0344 0.030 Uiso 1 calc R . . H21B H 0.3023 0.6759 0.0508 0.030 Uiso 1 calc R . . N22 N 0.3503(5) 0.7880(5) 0.1201(4) 0.0266(13) Uani 1 d . . . H22A H 0.3226 0.7384 0.1549 0.032 Uiso 1 calc R . . H22B H 0.3706 0.8333 0.1359 0.032 Uiso 1 calc R . . N23 N 0.4050(5) 0.8716(5) -0.0118(4) 0.0304(14) Uani 1 d . . . H23A H 0.4131 0.8766 -0.0626 0.036 Uiso 1 calc R . . H23B H 0.4251 0.9164 0.0048 0.036 Uiso 1 calc R . . N31 N 0.7638(5) 0.5720(5) 0.3393(4) 0.0323(14) Uani 1 d . . . H31A H 0.7056 0.5696 0.3241 0.039 Uiso 1 calc R . . H31B H 0.7975 0.6201 0.3100 0.039 Uiso 1 calc R . . N32 N 0.7496(5) 0.4268(6) 0.4537(4) 0.0338(15) Uani 1 d . . . H32A H 0.6915 0.4241 0.4386 0.041 Uiso 1 calc R . . H32B H 0.7743 0.3813 0.4981 0.041 Uiso 1 calc R . . N33 N 0.8900(5) 0.5059(6) 0.4334(4) 0.0328(14) Uani 1 d . . . H33A H 0.9233 0.5548 0.4053 0.039 Uiso 1 calc R . . H33B H 0.9137 0.4598 0.4780 0.039 Uiso 1 calc R . . N41 N 0.9077(5) 0.4497(6) 0.0905(4) 0.0381(16) Uani 1 d . . . H41A H 0.9555 0.4516 0.1176 0.046 Uiso 1 calc R . . H41B H 0.9175 0.4665 0.0385 0.046 Uiso 1 calc R . . N42 N 0.7484(5) 0.4138(6) 0.0859(6) 0.054(2) Uani 1 d . . . H42A H 0.6921 0.3923 0.1106 0.065 Uiso 1 calc R . . H42B H 0.7586 0.4307 0.0339 0.065 Uiso 1 calc R . . N43 N 0.8049(6) 0.3956(6) 0.2071(5) 0.050(2) Uani 1 d . . . H43A H 0.8527 0.3975 0.2343 0.060 Uiso 1 calc R . . H43B H 0.7473 0.3769 0.2318 0.060 Uiso 1 calc R . . N51 N 0.9992(5) 0.1588(5) 0.2050(4) 0.0313(14) Uani 1 d . . . H51A H 0.9461 0.1473 0.2407 0.038 Uiso 1 calc R . . H51B H 1.0565 0.1649 0.2189 0.038 Uiso 1 calc R . . N52 N 0.9047(5) 0.1579(6) 0.1071(4) 0.0391(17) Uani 1 d . . . H52A H 0.8518 0.1464 0.1430 0.047 Uiso 1 calc R . . H52B H 0.9001 0.1633 0.0575 0.047 Uiso 1 calc R . . N53 N 1.0757(5) 0.1849(6) 0.0736(4) 0.0379(16) Uani 1 d . . . H53A H 1.0725 0.1903 0.0238 0.045 Uiso 1 calc R . . H53B H 1.1326 0.1908 0.0883 0.045 Uiso 1 calc R . . N61 N 0.4634(5) 0.6762(6) 0.4458(4) 0.0355(15) Uani 1 d . . . H61A H 0.4651 0.6634 0.4970 0.043 Uiso 1 calc R . . H61B H 0.5096 0.6332 0.4204 0.043 Uiso 1 calc R . . N62 N 0.3907(5) 0.7817(6) 0.3268(4) 0.0341(15) Uani 1 d . . . H62A H 0.3448 0.8381 0.2996 0.041 Uiso 1 calc R . . H62B H 0.4376 0.7376 0.3026 0.041 Uiso 1 calc R . . N63 N 0.3187(6) 0.8287(5) 0.4443(4) 0.0408(17) Uani 1 d . . . H63A H 0.2721 0.8855 0.4180 0.049 Uiso 1 calc R . . H63B H 0.3190 0.8151 0.4957 0.049 Uiso 1 calc R . . OH1 O 0.5233(7) 0.4953(7) 0.0737(5) 0.0196(18) Uiso 0.50 d P . . OH2 O 0.4860(7) 0.4745(8) 0.0457(6) 0.0220(19) Uiso 0.50 d P . . OW1 O 0.4143(7) 0.4343(8) 0.0360(6) 0.024(2) Uiso 0.50 d P . . OW2 O -0.0193(7) 0.7630(9) 0.0889(5) 0.111(4) Uani 1 d . . . OW3 O 0.0823(4) 0.8875(4) 0.1920(3) 0.0297(11) Uani 1 d . . . OW4 O 0.2298(4) 0.9573(4) 0.2380(3) 0.0319(12) Uani 1 d . . . OW5 O 0.9142(4) 0.6973(5) 0.2940(4) 0.0424(14) Uani 1 d . . . OW6 O 0.8897(4) -0.0820(4) 0.2940(3) 0.0357(13) Uani 1 d . . . OW7 O 0.0041(4) 0.3930(5) 0.2658(4) 0.0387(13) Uani 1 d . . . OW8 O 0.1302(5) 0.4879(5) 0.0782(4) 0.0408(14) Uani 1 d . . . OW9 O 0.7656(4) 0.2002(5) 0.3730(4) 0.0395(14) Uani 1 d . . . OW10 O 0.4493(4) -0.0329(5) 0.1109(4) 0.0413(14) Uani 1 d . . . OW11 O 0.7897(5) -0.0801(5) 0.0995(4) 0.0506(16) Uani 1 d . . . OW12 O 0.0032(5) 0.1251(5) 0.5680(4) 0.0466(15) Uani 1 d . . . OW13 O 0.9013(5) 0.0602(5) -0.0240(4) 0.0475(15) Uani 1 d . . . OW14 O 0.1227(6) 0.6709(5) 0.4108(4) 0.0537(18) Uani 1 d . . . OW15 O 0.8679(5) -0.0144(5) 0.6189(4) 0.0508(16) Uani 1 d . . . OW16 O -0.0294(5) 0.2094(5) 0.4015(4) 0.0465(15) Uani 1 d . . . OW17 O 0.5941(7) -0.1341(7) 0.2380(6) 0.094(3) Uani 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 Tb 0.01596(16) 0.02064(17) 0.01978(17) -0.00311(12) 0.00151(11) -0.00440(11) P1 0.0142(7) 0.0174(8) 0.0200(8) -0.0031(6) -0.0022(6) -0.0032(6) P2 0.0147(8) 0.0302(9) 0.0180(8) -0.0057(7) -0.0022(6) -0.0030(7) P3 0.0249(9) 0.0172(8) 0.0266(9) -0.0039(7) -0.0036(7) -0.0052(7) P4 0.0225(9) 0.0247(9) 0.0240(9) -0.0017(7) 0.0033(7) 0.0025(7) O1 0.019(2) 0.020(2) 0.022(2) -0.0034(19) -0.0011(18) -0.0055(18) O2 0.016(2) 0.023(2) 0.027(3) -0.004(2) -0.0023(18) -0.0062(18) O3 0.028(2) 0.017(2) 0.030(3) -0.004(2) -0.008(2) -0.0053(19) O4 0.019(2) 0.031(3) 0.028(3) -0.003(2) -0.0039(19) -0.008(2) O5 0.015(2) 0.070(4) 0.023(3) -0.021(3) 0.0021(19) -0.013(2) O6 0.023(2) 0.031(3) 0.029(3) -0.013(2) -0.010(2) 0.003(2) O7 0.020(2) 0.039(3) 0.033(3) -0.005(2) 0.001(2) -0.003(2) O8 0.036(3) 0.023(3) 0.031(3) -0.008(2) 0.003(2) 0.002(2) O9 0.023(2) 0.023(3) 0.024(3) -0.001(2) 0.0063(19) 0.0060(19) O10 0.051(3) 0.016(3) 0.060(4) 0.002(2) -0.034(3) -0.013(2) O11 0.026(3) 0.042(3) 0.043(3) -0.023(3) 0.001(2) -0.004(2) O12 0.029(3) 0.019(2) 0.031(3) -0.008(2) 0.002(2) -0.0093(19) C1 0.017(3) 0.019(3) 0.022(3) -0.003(3) -0.001(2) -0.005(2) C2 0.014(3) 0.023(3) 0.022(3) -0.004(3) 0.000(2) -0.002(2) C3 0.017(3) 0.018(3) 0.018(3) 0.001(3) 0.001(2) -0.002(2) C4 0.023(3) 0.037(4) 0.017(3) -0.008(3) 0.001(3) -0.004(3) C5 0.027(3) 0.035(4) 0.005(3) 0.004(3) -0.002(2) -0.001(3) C6 0.027(3) 0.017(3) 0.025(4) 0.001(3) 0.002(3) -0.005(3) C7 0.032(4) 0.013(3) 0.022(3) 0.001(3) -0.004(3) -0.002(3) C8 0.017(3) 0.019(3) 0.011(3) -0.001(2) 0.000(2) -0.002(2) C9 0.037(4) 0.017(3) 0.022(3) -0.006(3) 0.006(3) -0.008(3) C10 0.028(4) 0.017(3) 0.023(4) 0.001(3) 0.000(3) 0.000(3) N1 0.018(3) 0.017(3) 0.017(3) 0.000(2) 0.001(2) 0.002(2) N2 0.022(3) 0.013(2) 0.015(3) -0.002(2) 0.000(2) 0.000(2) C20 0.018(3) 0.015(3) 0.031(4) -0.004(3) 0.000(3) -0.004(2) C30 0.027(4) 0.032(4) 0.029(4) -0.016(3) 0.002(3) -0.007(3) C40 0.022(3) 0.021(4) 0.054(5) -0.003(3) -0.003(3) -0.007(3) C50 0.017(3) 0.034(4) 0.035(4) -0.001(3) -0.003(3) -0.001(3) C60 0.035(4) 0.033(4) 0.033(4) 0.001(3) -0.007(3) -0.021(3) N21 0.024(3) 0.027(3) 0.026(3) -0.009(2) 0.004(2) -0.011(2) N22 0.026(3) 0.027(3) 0.028(3) -0.006(3) 0.000(2) -0.012(2) N23 0.040(4) 0.028(3) 0.029(3) -0.006(3) 0.002(3) -0.022(3) N31 0.023(3) 0.036(4) 0.038(4) -0.006(3) -0.004(3) -0.012(3) N32 0.029(3) 0.043(4) 0.026(3) -0.004(3) -0.007(3) -0.009(3) N33 0.025(3) 0.040(4) 0.036(4) -0.012(3) -0.005(3) -0.011(3) N41 0.031(3) 0.048(4) 0.038(4) -0.003(3) -0.003(3) -0.025(3) N42 0.025(3) 0.042(4) 0.105(7) -0.020(4) -0.024(4) -0.013(3) N43 0.044(4) 0.047(5) 0.051(5) -0.007(4) 0.013(4) -0.016(4) N51 0.025(3) 0.036(4) 0.032(4) -0.010(3) 0.005(3) -0.011(3) N52 0.019(3) 0.055(4) 0.036(4) -0.006(3) 0.001(3) -0.008(3) N53 0.018(3) 0.058(5) 0.032(4) -0.005(3) -0.001(3) -0.012(3) N61 0.041(4) 0.041(4) 0.025(3) -0.003(3) -0.008(3) -0.015(3) N62 0.039(4) 0.033(4) 0.024(3) -0.003(3) -0.002(3) -0.008(3) N63 0.065(5) 0.025(3) 0.030(4) -0.003(3) -0.004(3) -0.013(3) OW2 0.090(6) 0.131(8) 0.039(4) -0.009(5) -0.011(4) 0.060(6) OW3 0.020(2) 0.021(2) 0.039(3) -0.003(2) -0.003(2) -0.0001(19) OW4 0.028(3) 0.026(3) 0.041(3) -0.006(2) -0.002(2) -0.010(2) OW5 0.029(3) 0.046(3) 0.059(4) -0.026(3) 0.015(3) -0.018(3) OW6 0.025(3) 0.026(3) 0.047(3) -0.006(2) 0.005(2) -0.003(2) OW7 0.032(3) 0.032(3) 0.054(4) -0.017(3) 0.008(3) -0.012(2) OW8 0.041(3) 0.035(3) 0.049(4) -0.012(3) -0.026(3) 0.000(2) OW9 0.027(3) 0.032(3) 0.054(4) -0.008(3) 0.001(2) -0.007(2) OW10 0.036(3) 0.041(3) 0.055(4) -0.029(3) 0.014(3) -0.017(3) OW11 0.044(3) 0.050(4) 0.063(4) -0.038(3) 0.002(3) -0.001(3) OW12 0.034(3) 0.055(4) 0.046(4) -0.017(3) -0.001(3) -0.004(3) OW13 0.036(3) 0.050(4) 0.047(4) -0.008(3) -0.011(3) 0.000(3) OW14 0.073(4) 0.046(4) 0.033(3) -0.015(3) -0.015(3) 0.006(3) OW15 0.051(4) 0.039(3) 0.043(4) 0.005(3) 0.005(3) -0.009(3) OW16 0.043(3) 0.042(4) 0.048(4) -0.005(3) -0.009(3) -0.008(3) OW17 0.077(6) 0.061(5) 0.124(8) -0.012(5) 0.030(5) -0.026(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb OH2 2.380(9) . yes Tb O1 2.307(5) . yes Tb O10 2.311(5) . yes Tb O9 2.317(5) . yes Tb O5 2.319(5) . yes Tb OH1 2.353(9) . yes Tb OW1 2.475(10) . yes Tb N2 2.702(6) . yes Tb N1 2.705(6) . yes P1 O2 1.519(5) . no P1 O3 1.522(5) . no P1 O1 1.537(5) . no P1 C1 1.833(7) . no P2 O4 1.510(6) . no P2 O6 1.533(5) . no P2 O5 1.539(5) . no P2 C2 1.826(6) . no P3 O11 1.514(5) . no P3 O10 1.516(5) . no P3 O12 1.537(5) . no P3 C9 1.812(8) . no P4 O8 1.518(6) . no P4 O7 1.523(6) . no P4 O9 1.530(5) . no P4 C10 1.841(7) . no C1 N1 1.506(8) . no C2 N1 1.500(9) . no C3 N1 1.502(8) . no C3 C8 1.521(9) . no C3 C4 1.529(9) . no C4 C5 1.540(10) . no C5 C6 1.499(10) . no C6 C7 1.529(9) . no C7 C8 1.535(8) . no C8 N2 1.528(8) . no C9 N2 1.477(9) . no C10 N2 1.496(8) . no C20 N21 1.324(9) . no C20 N23 1.328(8) . no C20 N22 1.345(9) . no C30 N31 1.328(10) . no C30 N32 1.335(10) . no C30 N33 1.331(9) . no C40 N43 1.303(11) . no C40 N41 1.312(9) . no C40 N42 1.336(11) . no C50 N52 1.315(10) . no C50 N51 1.334(10) . no C50 N53 1.332(9) . no C60 N63 1.314(11) . no C60 N62 1.325(10) . no C60 N61 1.331(10) . no C70 N71 1.324(16) . no C70 N72 1.323(14) . no C70 N73 1.340(15) . no C80 N81 1.323(14) . no C80 N82 1.337(14) . no C80 N83 1.341(14) . no OH1 OH2 0.901(11) . no OH2 OW1 1.268(13) . no OH2 OH2 1.546(18) 2_665 no 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 OH2 Tb O1 83.2(2) . . no OH2 Tb O10 97.3(3) . . no O1 Tb O10 82.64(18) . . no OH2 Tb O9 79.4(3) . . no O1 Tb O9 162.31(16) . . no O10 Tb O9 102.8(2) . . no OH2 Tb O5 96.2(3) . . no O1 Tb O5 98.27(19) . . no O10 Tb O5 166.5(2) . . no O9 Tb O5 80.3(2) . . no OH2 Tb OH1 21.9(3) . . no O1 Tb OH1 84.6(2) . . no O10 Tb OH1 119.1(3) . . no O9 Tb OH1 78.0(2) . . no O5 Tb OH1 74.3(3) . . no OH2 Tb OW1 30.2(3) . . no O1 Tb OW1 80.1(2) . . no O10 Tb OW1 67.1(3) . . no O9 Tb OW1 86.5(3) . . no O5 Tb OW1 126.4(3) . . no OH1 Tb OW1 52.1(3) . . no OH2 Tb N2 144.6(2) . . no O1 Tb N2 125.79(16) . . no O10 Tb N2 70.67(19) . . no O9 Tb N2 71.64(18) . . no O5 Tb N2 98.5(2) . . no OH1 Tb N2 149.6(2) . . no OW1 Tb N2 126.0(3) . . no OH2 Tb N1 149.3(3) . . no O1 Tb N1 71.48(17) . . no O10 Tb N1 96.4(2) . . no O9 Tb N1 123.73(17) . . no O5 Tb N1 71.35(17) . . no OH1 Tb N1 134.2(3) . . no OW1 Tb N1 148.9(2) . . no N2 Tb N1 66.04(17) . . no O2 P1 O3 111.8(3) . . no O2 P1 O1 113.7(3) . . no O3 P1 O1 111.3(3) . . no O2 P1 C1 105.6(3) . . no O3 P1 C1 108.9(3) . . no O1 P1 C1 105.0(3) . . no O4 P2 O6 111.1(3) . . no O4 P2 O5 113.3(3) . . no O6 P2 O5 112.0(3) . . no O4 P2 C2 105.8(3) . . no O6 P2 C2 110.0(3) . . no O5 P2 C2 104.2(3) . . no O11 P3 O10 112.9(3) . . no O11 P3 O12 111.2(3) . . no O10 P3 O12 112.8(3) . . no O11 P3 C9 112.4(3) . . no O10 P3 C9 102.7(3) . . no O12 P3 C9 104.2(3) . . no O8 P4 O7 111.9(3) . . no O8 P4 O9 111.1(3) . . no O7 P4 O9 114.2(3) . . no O8 P4 C10 109.1(3) . . no O7 P4 C10 105.6(3) . . no O9 P4 C10 104.5(3) . . no P1 O1 Tb 126.7(3) . . no P2 O5 Tb 128.4(3) . . no P4 O9 Tb 127.7(3) . . no P3 O10 Tb 129.9(3) . . no N1 C1 P1 112.8(4) . . no N1 C2 P2 112.5(4) . . no N1 C3 C8 111.4(5) . . no N1 C3 C4 114.5(5) . . no C8 C3 C4 110.2(5) . . no C3 C4 C5 114.9(6) . . no C6 C5 C4 109.1(6) . . no C5 C6 C7 110.6(6) . . no C6 C7 C8 112.3(5) . . no C3 C8 N2 112.4(5) . . no C3 C8 C7 111.1(5) . . no N2 C8 C7 111.8(5) . . no N2 C9 P3 114.2(4) . . no N2 C10 P4 113.4(4) . . no C3 N1 C2 109.9(5) . . no C3 N1 C1 112.4(5) . . no C2 N1 C1 108.6(5) . . no C3 N1 Tb 114.7(4) . . no C2 N1 Tb 107.2(4) . . no C1 N1 Tb 103.6(4) . . no C9 N2 C10 110.2(5) . . no C9 N2 C8 109.4(5) . . no C10 N2 C8 112.5(5) . . no C9 N2 Tb 106.2(4) . . no C10 N2 Tb 104.9(4) . . no C8 N2 Tb 113.4(3) . . no N21 C20 N23 120.7(7) . . no N21 C20 N22 120.2(6) . . no N23 C20 N22 119.1(6) . . no N31 C30 N32 120.2(7) . . no N31 C30 N33 120.8(7) . . no N32 C30 N33 118.9(7) . . no N43 C40 N41 120.1(8) . . no N43 C40 N42 120.3(8) . . no N41 C40 N42 119.6(8) . . no N52 C50 N51 119.7(7) . . no N52 C50 N53 121.2(7) . . no N51 C50 N53 119.1(7) . . no N63 C60 N62 121.2(7) . . no N63 C60 N61 120.3(8) . . no N62 C60 N61 118.5(8) . . no N71 C70 N72 123.9(14) . . no N71 C70 N73 118.2(12) . . no N72 C70 N73 117.9(13) . . no N81 C80 N82 120.4(11) . . no N81 C80 N83 120.2(12) . . no N82 C80 N83 119.4(11) . . no OH2 OH1 Tb 80.7(8) . . no OH1 OH2 OW1 155.8(12) . . no OH1 OH2 OH2 108.3(12) . 2_665 no OW1 OH2 OH2 95.4(10) . 2_665 no OH1 OH2 Tb 77.4(8) . . no OW1 OH2 Tb 79.0(6) . . no OH2 OH2 Tb 174.4(10) 2_665 . no OH2 OW1 Tb 70.7(6) . . no _diffrn_measured_fraction_theta_max 0.860 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.860 _refine_diff_density_max 4.415 _refine_diff_density_min -1.431 _refine_diff_density_rms 0.168