data_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H100 N4 O34 Tb4' _chemical_formula_weight 2153.20 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 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5188(5) _cell_length_b 13.3615(6) _cell_length_c 15.4902(7) _cell_angle_alpha 91.2730(10) _cell_angle_beta 109.4220(10) _cell_angle_gamma 96.1810(10) _cell_volume 2037.36(16) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 9130 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.52 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 3.516 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction, Siemens Industrial Automation Inc., Madison, Wisconsin, USA. ; _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 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12826 _diffrn_reflns_av_R_equivalents 0.0152 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8893 _reflns_number_gt 8210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+1.6157P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8893 _refine_ls_number_parameters 530 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.055 _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 O15 O 0.0629(2) 0.98919(16) 0.30515(15) 0.0228(4) Uani 1 1 d . . . O12 O -0.0964(3) 1.2326(2) 0.22216(19) 0.0382(6) Uani 1 1 d . . . O3 O -0.2713(3) 0.4997(2) 0.2812(2) 0.0438(7) Uani 1 1 d D . . C29 C 0.1519(3) 0.9595(2) 0.2747(2) 0.0239(6) Uani 1 1 d . . . O2 O -0.1192(4) 0.4925(3) 0.0176(2) 0.0520(8) Uani 1 1 d D . . C25 C -0.1833(3) 1.1772(2) 0.2448(2) 0.0270(7) Uani 1 1 d . . . C27 C -0.1035(4) 0.6773(2) 0.4640(3) 0.0291(7) Uani 1 1 d . . . C30 C 0.2007(4) 1.0220(3) 0.2106(3) 0.0362(8) Uani 1 1 d . . . H30A H 0.2644 1.0777 0.2447 0.054 Uiso 1 1 calc R . . H30B H 0.1249 1.0471 0.1664 0.054 Uiso 1 1 calc R . . H30C H 0.2441 0.9815 0.1795 0.054 Uiso 1 1 calc R . . C9 C -0.1698(4) 0.4759(3) 0.2453(3) 0.0406(9) Uani 1 1 d . . . H9A H -0.1590 0.4050 0.2519 0.049 Uiso 1 1 calc R . . H9B H -0.0840 0.5148 0.2804 0.049 Uiso 1 1 calc R . . C28 C -0.1557(6) 0.5951(3) 0.5130(3) 0.0521(12) Uani 1 1 d . . . H28A H -0.2436 0.6069 0.5141 0.078 Uiso 1 1 calc R . . H28B H -0.0941 0.5950 0.5747 0.078 Uiso 1 1 calc R . . H28C H -0.1627 0.5311 0.4814 0.078 Uiso 1 1 calc R . . C3 C -0.2731(4) 0.9649(3) 0.0454(3) 0.0436(10) Uani 1 1 d . . . H3 H -0.2729 1.0340 0.0390 0.052 Uiso 1 1 calc R . . C26 C -0.3297(4) 1.1763(4) 0.1882(4) 0.0594(14) Uani 1 1 d . . . H26A H -0.3769 1.1102 0.1862 0.089 Uiso 1 1 calc R . . H26B H -0.3368 1.1935 0.1271 0.089 Uiso 1 1 calc R . . H26C H -0.3692 1.2246 0.2150 0.089 Uiso 1 1 calc R . . C32 C 0.9241(7) 0.2388(6) 0.9512(5) 0.088(2) Uani 1 1 d . . . O21A O 0.7832(7) 0.2051(7) 0.9405(5) 0.069(3) Uani 0.513(9) 1 d P A 1 C34A C 0.5540(13) 0.2293(10) 0.8705(9) 0.078(4) Uiso 0.513(9) 1 d P A 1 O21B O 0.8038(9) 0.3066(6) 0.9382(5) 0.070(3) Uani 0.487(9) 1 d P A 2 C34B C 0.5700(17) 0.3032(12) 0.8502(11) 0.093(5) Uiso 0.487(9) 1 d P A 2 C33 C 0.6991(7) 0.2694(7) 0.8711(5) 0.106(3) Uani 1 1 d . . . C31 C 0.9837(9) 0.1726(7) 1.0165(5) 0.108(3) Uani 1 1 d . A . H1O H -0.428(5) 0.482(3) 0.1646(15) 0.050(14) Uiso 1 1 d D . . H3O H -0.234(6) 0.550(3) 0.318(4) 0.09(2) Uiso 1 1 d D . . H7O H 0.618(2) 1.150(3) 0.689(3) 0.046(13) Uiso 1 1 d D . . H8O H 0.063(6) 1.217(4) 0.306(4) 0.060(18) Uiso 1 1 d . . . H2O H -0.173(5) 0.449(4) -0.018(4) 0.08(2) Uiso 1 1 d D . . Tb1 Tb 0.033708(13) 1.083918(9) 0.428778(9) 0.01595(5) Uani 1 1 d . . . Tb2 Tb 0.024359(13) 0.812709(10) 0.364484(9) 0.01684(5) Uani 1 1 d . . . O8 O 0.1193(2) 1.20469(18) 0.34015(18) 0.0246(5) Uani 1 1 d . . . O10 O 0.0904(3) 0.66239(18) 0.30288(18) 0.0339(6) Uani 1 1 d . . . O11 O -0.1547(2) 1.12336(16) 0.31102(16) 0.0252(5) Uani 1 1 d . . . O5 O 0.11268(19) 1.08081(15) 0.59647(14) 0.0172(4) Uani 1 1 d . . . O4 O -0.1273(2) 0.79231(16) 0.21754(15) 0.0242(5) Uani 1 1 d . . . O16 O 0.1942(2) 0.87622(17) 0.29602(17) 0.0271(5) Uani 1 1 d . . . O7 O 0.5367(2) 1.15034(18) 0.66854(17) 0.0283(5) Uani 1 1 d D . . O6 O 0.12935(19) 0.93146(15) 0.48829(14) 0.0176(4) Uani 1 1 d . . . O14 O -0.0234(2) 0.75187(16) 0.50918(16) 0.0246(5) Uani 1 1 d . . . O13 O -0.1393(3) 0.67114(18) 0.37778(17) 0.0321(5) Uani 1 1 d . . . N1 N -0.2100(3) 0.60795(19) 0.13828(19) 0.0232(5) Uani 1 1 d . . . H1N H -0.1636 0.6455 0.1867 0.032(10) Uiso 1 1 calc R . . C6 C -0.2727(3) 0.7595(2) 0.0628(2) 0.0260(7) Uani 1 1 d . . . O9 O 0.2181(2) 0.72682(18) 0.43971(17) 0.0320(5) Uani 1 1 d . . . C8 C -0.2053(4) 0.4982(2) 0.1441(2) 0.0290(7) Uani 1 1 d . . . C21 C 0.2564(3) 1.0889(2) 0.6398(2) 0.0183(6) Uani 1 1 d . . . H21A H 0.2775 1.0490 0.6932 0.022 Uiso 1 1 calc R . . H21B H 0.2914 1.1586 0.6605 0.022 Uiso 1 1 calc R . . C20 C 0.2712(3) 0.9427(2) 0.5369(2) 0.0181(6) Uani 1 1 d . . . H20A H 0.3182 0.9224 0.4963 0.022 Uiso 1 1 calc R . . H20B H 0.2898 0.8987 0.5874 0.022 Uiso 1 1 calc R . . C1 C -0.1964(3) 0.8268(2) 0.1400(2) 0.0237(6) Uani 1 1 d . . . C11 C -0.3407(4) 0.4387(3) 0.0853(3) 0.0369(8) Uani 1 1 d . . . H11A H -0.3566 0.4514 0.0214 0.044 Uiso 1 1 calc R . . H11B H -0.3343 0.3672 0.0919 0.044 Uiso 1 1 calc R . . C24 C 0.3061(4) 0.6010(3) 0.3710(3) 0.0420(9) Uani 1 1 d . . . H24A H 0.3732 0.6385 0.3510 0.063 Uiso 1 1 calc R . . H24B H 0.2652 0.5427 0.3300 0.063 Uiso 1 1 calc R . . H24C H 0.3484 0.5802 0.4318 0.063 Uiso 1 1 calc R . . C16 C 0.4807(3) 1.2809(3) 0.3845(3) 0.0309(7) Uani 1 1 d . . . H16 H 0.5647 1.2710 0.4263 0.037 Uiso 1 1 calc R . . C13 C 0.2309(4) 1.3110(2) 0.2597(2) 0.0272(7) Uani 1 1 d . . . H13 H 0.1477 1.3215 0.2174 0.033 Uiso 1 1 calc R . . C19 C 0.3261(3) 1.0525(2) 0.5746(2) 0.0174(5) Uani 1 1 d . . . C22 C 0.4777(3) 1.0534(2) 0.6260(2) 0.0212(6) Uani 1 1 d . . . H22A H 0.4910 1.0041 0.6723 0.025 Uiso 1 1 calc R . . H22B H 0.5223 1.0347 0.5835 0.025 Uiso 1 1 calc R . . C10 C -0.0918(4) 0.4700(3) 0.1114(3) 0.0447(10) Uani 1 1 d . . . H10A H -0.0061 0.5073 0.1489 0.054 Uiso 1 1 calc R . . H10B H -0.0842 0.3986 0.1176 0.054 Uiso 1 1 calc R . . C18 C 0.3799(3) 1.1687(2) 0.4726(2) 0.0216(6) Uani 1 1 d . . . H18 H 0.4690 1.1669 0.5108 0.026 Uiso 1 1 calc R . . O1 O -0.4534(3) 0.4639(2) 0.1094(2) 0.0432(7) Uani 1 1 d D . . C23 C 0.1980(3) 0.6668(2) 0.3715(2) 0.0271(7) Uani 1 1 d . . . C2 C -0.2006(4) 0.9311(3) 0.1283(3) 0.0329(8) Uani 1 1 d . . . H2 H -0.1538 0.9773 0.1773 0.039 Uiso 1 1 calc R . . C7 C -0.2772(3) 0.6530(2) 0.0675(2) 0.0253(6) Uani 1 1 d . . . H7 H -0.3324 0.6130 0.0160 0.030 Uiso 1 1 calc R . . C12 C 0.2358(3) 1.2488(2) 0.3318(2) 0.0223(6) Uani 1 1 d . . . C17 C 0.3609(3) 1.2323(2) 0.3950(2) 0.0231(6) Uani 1 1 d . . . N2 N 0.2876(2) 1.11497(18) 0.49406(17) 0.0186(5) Uani 1 1 d . . . C14 C 0.3506(4) 1.3570(3) 0.2513(3) 0.0341(8) Uani 1 1 d . . . H14 H 0.3466 1.3982 0.2031 0.041 Uiso 1 1 calc R . . C5 C -0.3468(4) 0.7975(3) -0.0205(3) 0.0380(9) Uani 1 1 d . . . H5 H -0.3965 0.7529 -0.0702 0.046 Uiso 1 1 calc R . . C15 C 0.4756(4) 1.3428(3) 0.3134(3) 0.0360(8) Uani 1 1 d . . . H15 H 0.5551 1.3745 0.3074 0.043 Uiso 1 1 calc R . . C4 C -0.3469(4) 0.8986(3) -0.0296(3) 0.0483(11) Uani 1 1 d . . . H4 H -0.3957 0.9231 -0.0851 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O15 0.0191(10) 0.0288(11) 0.0208(11) 0.0006(9) 0.0075(9) 0.0020(9) O12 0.0257(13) 0.0435(14) 0.0441(16) 0.0245(12) 0.0088(12) 0.0045(11) O3 0.0501(17) 0.0406(15) 0.0353(15) -0.0032(12) 0.0150(13) -0.0183(13) C29 0.0204(15) 0.0296(16) 0.0210(15) -0.0033(13) 0.0088(13) -0.0039(13) O2 0.059(2) 0.0568(19) 0.0480(19) -0.0104(16) 0.0304(17) 0.0018(17) C25 0.0210(15) 0.0260(15) 0.0300(17) 0.0079(13) 0.0024(13) 0.0052(13) C27 0.0377(19) 0.0206(15) 0.0355(19) -0.0007(13) 0.0225(16) -0.0004(14) C30 0.042(2) 0.0387(19) 0.037(2) 0.0082(16) 0.0248(18) 0.0049(16) C9 0.047(2) 0.0264(17) 0.040(2) 0.0017(16) 0.0057(18) -0.0032(16) C28 0.085(3) 0.0279(18) 0.049(3) -0.0012(18) 0.036(3) -0.015(2) C3 0.043(2) 0.0286(17) 0.045(2) 0.0117(17) -0.0034(18) -0.0010(16) C26 0.024(2) 0.072(3) 0.070(3) 0.043(3) -0.001(2) 0.004(2) C32 0.082(4) 0.120(6) 0.081(5) -0.007(4) 0.049(4) 0.032(4) O21A 0.046(4) 0.104(7) 0.053(4) 0.001(4) 0.014(3) 0.002(4) O21B 0.083(6) 0.070(6) 0.054(5) -0.026(4) 0.023(4) 0.001(4) C33 0.066(4) 0.156(8) 0.077(5) -0.023(5) 0.002(4) 0.014(5) C31 0.116(6) 0.142(7) 0.070(4) -0.003(5) 0.046(5) -0.016(5) Tb1 0.01207(8) 0.01789(8) 0.01724(8) 0.00237(5) 0.00428(6) 0.00087(5) Tb2 0.01345(8) 0.01830(8) 0.01790(8) 0.00021(5) 0.00441(6) 0.00125(5) O8 0.0175(11) 0.0274(11) 0.0278(13) 0.0082(10) 0.0064(10) 0.0014(9) O10 0.0300(13) 0.0286(12) 0.0395(15) -0.0077(11) 0.0070(11) 0.0058(10) O11 0.0178(10) 0.0274(11) 0.0273(12) 0.0059(9) 0.0034(9) 0.0025(9) O5 0.0111(9) 0.0202(9) 0.0196(10) 0.0020(8) 0.0043(8) 0.0011(7) O4 0.0214(11) 0.0264(11) 0.0210(11) 0.0013(9) 0.0023(9) 0.0022(9) O16 0.0188(11) 0.0286(11) 0.0369(13) 0.0040(10) 0.0130(10) 0.0043(9) O7 0.0122(10) 0.0335(12) 0.0343(13) -0.0066(10) 0.0032(10) -0.0016(9) O6 0.0102(9) 0.0202(9) 0.0207(10) 0.0014(8) 0.0034(8) 0.0010(7) O14 0.0257(11) 0.0209(10) 0.0275(12) 0.0042(9) 0.0090(10) 0.0035(9) O13 0.0334(13) 0.0297(12) 0.0306(13) -0.0011(10) 0.0116(11) -0.0090(10) N1 0.0200(12) 0.0225(12) 0.0247(14) -0.0016(11) 0.0058(11) -0.0022(10) C6 0.0207(15) 0.0281(15) 0.0253(16) 0.0041(13) 0.0036(13) -0.0008(12) O9 0.0302(13) 0.0350(13) 0.0287(13) 0.0008(10) 0.0043(10) 0.0138(10) C8 0.0307(18) 0.0207(14) 0.0322(18) -0.0010(13) 0.0074(15) 0.0000(13) C21 0.0109(13) 0.0230(14) 0.0184(14) 0.0005(11) 0.0022(11) -0.0001(11) C20 0.0122(13) 0.0205(13) 0.0218(14) 0.0026(11) 0.0057(11) 0.0026(11) C1 0.0194(15) 0.0262(15) 0.0218(15) 0.0029(12) 0.0027(12) 0.0004(12) C11 0.039(2) 0.0289(17) 0.036(2) -0.0034(15) 0.0063(17) -0.0059(15) C24 0.037(2) 0.0331(18) 0.061(3) 0.0043(18) 0.019(2) 0.0148(16) C16 0.0219(16) 0.0350(17) 0.0369(19) 0.0064(15) 0.0127(15) -0.0015(14) C13 0.0296(17) 0.0255(15) 0.0282(17) 0.0062(13) 0.0121(14) 0.0027(13) C19 0.0104(12) 0.0206(13) 0.0191(14) 0.0013(11) 0.0031(11) -0.0005(10) C22 0.0120(13) 0.0261(15) 0.0242(15) 0.0000(12) 0.0045(11) 0.0017(11) C10 0.042(2) 0.039(2) 0.055(3) -0.0015(19) 0.016(2) 0.0122(18) C18 0.0136(13) 0.0237(14) 0.0254(16) -0.0004(12) 0.0045(12) 0.0004(11) O1 0.0294(14) 0.0582(18) 0.0357(16) -0.0036(14) 0.0090(12) -0.0135(12) C23 0.0242(16) 0.0215(14) 0.0395(19) 0.0056(14) 0.0148(15) 0.0053(12) C2 0.0298(18) 0.0251(16) 0.0341(19) 0.0030(14) -0.0006(15) -0.0010(14) C7 0.0199(15) 0.0277(15) 0.0249(16) -0.0013(13) 0.0052(13) -0.0028(12) C12 0.0211(15) 0.0208(14) 0.0259(16) 0.0017(12) 0.0097(13) 0.0006(12) C17 0.0216(15) 0.0223(14) 0.0263(16) 0.0015(12) 0.0106(13) -0.0008(12) N2 0.0158(11) 0.0208(11) 0.0185(12) 0.0003(10) 0.0052(10) 0.0008(9) C14 0.041(2) 0.0301(17) 0.037(2) 0.0113(15) 0.0213(17) 0.0008(15) C5 0.0344(19) 0.0387(19) 0.0266(18) 0.0039(15) -0.0056(15) -0.0056(16) C15 0.0290(18) 0.0373(18) 0.046(2) 0.0108(16) 0.0209(17) -0.0034(15) C4 0.046(2) 0.044(2) 0.036(2) 0.0155(18) -0.0092(19) -0.0018(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O15 C29 1.274(4) . ? O15 Tb1 2.394(2) . ? O15 Tb2 2.590(2) . ? O12 C25 1.260(4) . ? O3 C9 1.417(5) . ? C29 O16 1.253(4) . ? C29 C30 1.493(5) . ? C29 Tb2 2.894(3) . ? O2 C10 1.429(6) . ? C25 O11 1.239(4) . ? C25 C26 1.495(5) . ? C27 O13 1.260(4) . ? C27 O14 1.260(4) . ? C27 C28 1.506(5) . ? C27 Tb2 2.905(3) . ? C9 C8 1.530(5) . ? C3 C2 1.373(5) . ? C3 C4 1.394(6) . ? C32 C31 1.391(11) . ? C32 O21A 1.454(9) . ? C32 O21B 1.595(10) . ? O21A C33 1.500(11) . ? C34A C33 1.559(15) . ? O21B C33 1.280(10) . ? C34B C33 1.415(17) . ? Tb1 O11 2.323(2) . ? Tb1 O14 2.403(2) 2_576 ? Tb1 O8 2.430(2) . ? Tb1 O6 2.433(2) . ? Tb1 O5 2.453(2) . ? Tb1 O6 2.457(2) 2_576 ? Tb1 O5 2.4900(19) 2_576 ? Tb1 N2 2.505(2) . ? Tb1 Tb1 3.3643(3) 2_576 ? Tb1 Tb2 3.7178(2) 2_576 ? Tb1 Tb2 3.7190(2) . ? Tb2 O4 2.294(2) . ? Tb2 O5 2.3348(19) 2_576 ? Tb2 O6 2.344(2) . ? Tb2 O9 2.411(2) . ? Tb2 O16 2.451(2) . ? Tb2 O10 2.467(2) . ? Tb2 O13 2.477(2) . ? Tb2 O14 2.584(2) . ? Tb2 C23 2.791(3) . ? O8 C12 1.349(4) . ? O10 C23 1.264(4) . ? O5 C21 1.427(3) . ? O5 Tb2 2.3348(19) 2_576 ? O5 Tb1 2.4900(19) 2_576 ? O4 C1 1.303(4) . ? O7 C22 1.419(4) . ? O6 C20 1.420(3) . ? O6 Tb1 2.457(2) 2_576 ? O14 Tb1 2.403(2) 2_576 ? N1 C7 1.292(4) . ? N1 C8 1.476(4) . ? C6 C5 1.406(5) . ? C6 C7 1.423(4) . ? C6 C1 1.430(4) . ? O9 C23 1.257(4) . ? C8 C10 1.522(5) . ? C8 C11 1.534(5) . ? C21 C19 1.530(4) . ? C20 C19 1.543(4) . ? C1 C2 1.413(4) . ? C11 O1 1.426(5) . ? C24 C23 1.512(4) . ? C16 C15 1.382(5) . ? C16 C17 1.414(4) . ? C13 C14 1.387(5) . ? C13 C12 1.398(4) . ? C19 N2 1.484(4) . ? C19 C22 1.526(4) . ? C18 N2 1.282(4) . ? C18 C17 1.460(4) . ? C12 C17 1.398(5) . ? C14 C15 1.382(6) . ? C5 C4 1.361(5) . ? 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 C29 O15 Tb1 143.4(2) . . ? C29 O15 Tb2 90.42(19) . . ? Tb1 O15 Tb2 96.45(7) . . ? O16 C29 O15 119.7(3) . . ? O16 C29 C30 120.5(3) . . ? O15 C29 C30 119.8(3) . . ? O16 C29 Tb2 57.12(16) . . ? O15 C29 Tb2 63.48(16) . . ? C30 C29 Tb2 168.1(2) . . ? O11 C25 O12 123.9(3) . . ? O11 C25 C26 118.1(3) . . ? O12 C25 C26 118.0(3) . . ? O13 C27 O14 120.0(3) . . ? O13 C27 C28 119.9(3) . . ? O14 C27 C28 120.1(3) . . ? O13 C27 Tb2 57.92(16) . . ? O14 C27 Tb2 62.79(17) . . ? C28 C27 Tb2 170.8(3) . . ? O3 C9 C8 112.0(3) . . ? C2 C3 C4 121.8(3) . . ? C31 C32 O21A 97.7(7) . . ? C31 C32 O21B 133.9(6) . . ? O21A C32 O21B 52.4(5) . . ? C32 O21A C33 106.2(7) . . ? C33 O21B C32 110.0(7) . . ? O21B C33 C34B 123.8(10) . . ? O21B C33 O21A 57.6(6) . . ? C34B C33 O21A 136.6(10) . . ? O21B C33 C34A 129.4(9) . . ? C34B C33 C34A 41.3(7) . . ? O21A C33 C34A 100.5(8) . . ? O11 Tb1 O15 81.46(8) . . ? O11 Tb1 O14 82.40(8) . 2_576 ? O15 Tb1 O14 146.27(7) . 2_576 ? O11 Tb1 O8 73.67(8) . . ? O15 Tb1 O8 73.26(8) . . ? O14 Tb1 O8 73.85(8) 2_576 . ? O11 Tb1 O6 136.74(7) . . ? O15 Tb1 O6 71.87(7) . . ? O14 Tb1 O6 136.53(7) 2_576 . ? O8 Tb1 O6 126.74(8) . . ? O11 Tb1 O5 138.67(7) . . ? O15 Tb1 O5 135.91(7) . . ? O14 Tb1 O5 72.01(7) 2_576 . ? O8 Tb1 O5 126.17(8) . . ? O6 Tb1 O5 65.27(7) . . ? O11 Tb1 O6 82.10(7) . 2_576 ? O15 Tb1 O6 134.87(7) . 2_576 ? O14 Tb1 O6 71.13(7) 2_576 2_576 ? O8 Tb1 O6 139.51(7) . 2_576 ? O6 Tb1 O6 93.05(6) . 2_576 ? O5 Tb1 O6 59.36(6) . 2_576 ? O11 Tb1 O5 80.58(7) . 2_576 ? O15 Tb1 O5 71.62(7) . 2_576 ? O14 Tb1 O5 133.98(7) 2_576 2_576 ? O8 Tb1 O5 138.88(8) . 2_576 ? O6 Tb1 O5 59.17(6) . 2_576 ? O5 Tb1 O5 94.22(6) . 2_576 ? O6 Tb1 O5 64.37(6) 2_576 2_576 ? O11 Tb1 N2 143.72(8) . . ? O15 Tb1 N2 86.63(8) . . ? O14 Tb1 N2 89.14(8) 2_576 . ? O8 Tb1 N2 70.08(8) . . ? O6 Tb1 N2 68.89(7) . . ? O5 Tb1 N2 69.08(7) . . ? O6 Tb1 N2 128.17(7) 2_576 . ? O5 Tb1 N2 127.55(7) 2_576 . ? O11 Tb1 Tb1 115.24(5) . 2_576 ? O15 Tb1 Tb1 106.87(5) . 2_576 ? O14 Tb1 Tb1 106.78(5) 2_576 2_576 ? O8 Tb1 Tb1 171.08(6) . 2_576 ? O6 Tb1 Tb1 46.82(5) . 2_576 ? O5 Tb1 Tb1 47.57(5) . 2_576 ? O6 Tb1 Tb1 46.23(5) 2_576 2_576 ? O5 Tb1 Tb1 46.64(5) 2_576 2_576 ? N2 Tb1 Tb1 101.00(6) . 2_576 ? O11 Tb1 Tb2 102.13(6) . 2_576 ? O15 Tb1 Tb2 169.99(5) . 2_576 ? O14 Tb1 Tb2 43.70(5) 2_576 2_576 ? O8 Tb1 Tb2 116.67(6) . 2_576 ? O6 Tb1 Tb2 99.72(5) . 2_576 ? O5 Tb1 Tb2 37.92(4) . 2_576 ? O6 Tb1 Tb2 38.16(5) 2_576 2_576 ? O5 Tb1 Tb2 99.57(5) 2_576 2_576 ? N2 Tb1 Tb2 95.48(6) . 2_576 ? Tb1 Tb1 Tb2 63.121(5) 2_576 2_576 ? O11 Tb1 Tb2 100.11(6) . . ? O15 Tb1 Tb2 43.79(5) . . ? O14 Tb1 Tb2 169.73(5) 2_576 . ? O8 Tb1 Tb2 116.43(6) . . ? O6 Tb1 Tb2 38.02(5) . . ? O5 Tb1 Tb2 100.27(5) . . ? O6 Tb1 Tb2 99.22(5) 2_576 . ? O5 Tb1 Tb2 38.07(4) 2_576 . ? N2 Tb1 Tb2 94.42(5) . . ? Tb1 Tb1 Tb2 63.085(5) 2_576 . ? Tb2 Tb1 Tb2 126.207(4) 2_576 . ? O4 Tb2 O5 89.54(7) . 2_576 ? O4 Tb2 O6 143.26(7) . . ? O5 Tb2 O6 62.61(7) 2_576 . ? O4 Tb2 O9 130.86(8) . . ? O5 Tb2 O9 138.70(8) 2_576 . ? O6 Tb2 O9 82.55(7) . . ? O4 Tb2 O16 86.37(8) . . ? O5 Tb2 O16 121.57(7) 2_576 . ? O6 Tb2 O16 88.70(7) . . ? O9 Tb2 O16 75.87(8) . . ? O4 Tb2 O10 77.77(8) . . ? O5 Tb2 O10 159.51(8) 2_576 . ? O6 Tb2 O10 135.21(8) . . ? O9 Tb2 O10 53.45(8) . . ? O16 Tb2 O10 74.12(8) . . ? O4 Tb2 O13 78.53(8) . . ? O5 Tb2 O13 86.53(8) 2_576 . ? O6 Tb2 O13 119.88(7) . . ? O9 Tb2 O13 93.02(9) . . ? O16 Tb2 O13 148.11(8) . . ? O10 Tb2 O13 75.30(8) . . ? O4 Tb2 O14 125.60(8) . . ? O5 Tb2 O14 70.75(7) 2_576 . ? O6 Tb2 O14 69.82(7) . . ? O9 Tb2 O14 77.09(8) . . ? O16 Tb2 O14 147.31(8) . . ? O10 Tb2 O14 103.59(8) . . ? O13 Tb2 O14 51.03(8) . . ? O4 Tb2 O15 78.82(7) . . ? O5 Tb2 O15 70.75(7) 2_576 . ? O6 Tb2 O15 69.89(7) . . ? O9 Tb2 O15 119.11(8) . . ? O16 Tb2 O15 51.28(7) . . ? O10 Tb2 O15 121.27(8) . . ? O13 Tb2 O15 147.83(8) . . ? O14 Tb2 O15 133.50(7) . . ? O4 Tb2 C23 104.19(9) . . ? O5 Tb2 C23 162.48(9) 2_576 . ? O6 Tb2 C23 108.47(9) . . ? O9 Tb2 C23 26.71(9) . . ? O16 Tb2 C23 70.96(8) . . ? O10 Tb2 C23 26.91(9) . . ? O13 Tb2 C23 85.63(9) . . ? O14 Tb2 C23 92.21(8) . . ? O15 Tb2 C23 122.06(8) . . ? O4 Tb2 C29 79.27(9) . . ? O5 Tb2 C29 96.84(8) 2_576 . ? O6 Tb2 C29 80.81(8) . . ? O9 Tb2 C29 98.79(9) . . ? O16 Tb2 C29 25.43(8) . . ? O10 Tb2 C29 96.51(9) . . ? O13 Tb2 C29 157.51(9) . . ? O14 Tb2 C29 150.62(8) . . ? O15 Tb2 C29 26.11(8) . . ? C23 Tb2 C29 96.39(9) . . ? O4 Tb2 C27 103.02(9) . . ? O5 Tb2 C27 79.74(8) 2_576 . ? O6 Tb2 C27 95.39(8) . . ? O9 Tb2 C27 82.41(10) . . ? O16 Tb2 C27 157.19(9) . . ? O10 Tb2 C27 87.44(9) . . ? O13 Tb2 C27 25.52(9) . . ? O14 Tb2 C27 25.71(9) . . ? O15 Tb2 C27 150.44(8) . . ? C23 Tb2 C27 86.50(9) . . ? C29 Tb2 C27 175.80(9) . . ? C12 O8 Tb1 142.0(2) . . ? C23 O10 Tb2 91.01(19) . . ? C25 O11 Tb1 139.9(2) . . ? C21 O5 Tb2 123.52(17) . 2_576 ? C21 O5 Tb1 115.32(16) . . ? Tb2 O5 Tb1 101.86(7) 2_576 . ? C21 O5 Tb1 121.91(16) . 2_576 ? Tb2 O5 Tb1 100.80(7) 2_576 2_576 ? Tb1 O5 Tb1 85.78(6) . 2_576 ? C1 O4 Tb2 152.6(2) . . ? C29 O16 Tb2 97.46(18) . . ? C20 O6 Tb2 122.67(17) . . ? C20 O6 Tb1 116.14(16) . . ? Tb2 O6 Tb1 102.23(8) . . ? C20 O6 Tb1 120.52(17) . 2_576 ? Tb2 O6 Tb1 101.48(7) . 2_576 ? Tb1 O6 Tb1 86.95(6) . 2_576 ? C27 O14 Tb1 138.8(2) . 2_576 ? C27 O14 Tb2 91.51(19) . . ? Tb1 O14 Tb2 96.32(7) 2_576 . ? C27 O13 Tb2 96.6(2) . . ? C7 N1 C8 126.3(3) . . ? C5 C6 C7 118.0(3) . . ? C5 C6 C1 120.3(3) . . ? C7 C6 C1 121.6(3) . . ? C23 O9 Tb2 93.8(2) . . ? N1 C8 C10 108.5(3) . . ? N1 C8 C9 107.3(3) . . ? C10 C8 C9 108.4(3) . . ? N1 C8 C11 111.3(3) . . ? C10 C8 C11 109.8(3) . . ? C9 C8 C11 111.5(3) . . ? O5 C21 C19 111.5(2) . . ? O6 C20 C19 111.9(2) . . ? O4 C1 C2 122.2(3) . . ? O4 C1 C6 120.8(3) . . ? C2 C1 C6 117.0(3) . . ? O1 C11 C8 113.2(3) . . ? C15 C16 C17 121.3(3) . . ? C14 C13 C12 119.8(3) . . ? N2 C19 C22 116.7(2) . . ? N2 C19 C21 106.5(2) . . ? C22 C19 C21 109.8(2) . . ? N2 C19 C20 105.7(2) . . ? C22 C19 C20 106.3(2) . . ? C21 C19 C20 111.8(2) . . ? O7 C22 C19 110.8(2) . . ? O2 C10 C8 110.1(3) . . ? N2 C18 C17 127.3(3) . . ? O9 C23 O10 121.0(3) . . ? O9 C23 C24 119.2(3) . . ? O10 C23 C24 119.7(3) . . ? O9 C23 Tb2 59.53(16) . . ? O10 C23 Tb2 62.08(16) . . ? C24 C23 Tb2 170.8(2) . . ? C3 C2 C1 120.7(3) . . ? N1 C7 C6 124.6(3) . . ? O8 C12 C17 120.1(3) . . ? O8 C12 C13 119.7(3) . . ? C17 C12 C13 120.1(3) . . ? C12 C17 C16 118.4(3) . . ? C12 C17 C18 125.5(3) . . ? C16 C17 C18 116.1(3) . . ? C18 N2 C19 120.0(3) . . ? C18 N2 Tb1 134.8(2) . . ? C19 N2 Tb1 105.29(16) . . ? C15 C14 C13 121.2(3) . . ? C4 C5 C6 121.0(3) . . ? C16 C15 C14 119.1(3) . . ? C5 C4 C3 119.2(4) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 2.024 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.119 #===END data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H13 O7 Tb' _chemical_formula_weight 368.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/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 11.9785(10) _cell_length_b 11.9409(10) _cell_length_c 7.6080(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.424(2) _cell_angle_gamma 90.00 _cell_volume 1088.17(15) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2986 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.51 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 6.512 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.772 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; SADABS - G. M. Sheldrick, Area Detector Absoption Correction ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6713 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.53 _reflns_number_total 2464 _reflns_number_gt 2223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+1.0518P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2464 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0517 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 H6O H 0.752(4) 0.958(4) 0.910(6) 0.034(15) Uiso 1 1 d . . . Tb1 Tb 0.744224(13) 0.803497(13) 1.18725(2) 0.01240(6) Uani 1 1 d . . . O3 O 0.7413(2) 0.6000(2) 1.1642(3) 0.0193(5) Uani 1 1 d . . . O4 O 0.7176(2) 0.9516(2) 1.3846(3) 0.0176(5) Uani 1 1 d . . . O6 O 0.7636(2) 0.9668(2) 1.0017(4) 0.0179(5) Uani 1 1 d . . . C1 C 0.9353(3) 0.8218(3) 1.4088(5) 0.0159(7) Uani 1 1 d . . . O2 O 0.9334(2) 0.8730(2) 1.2679(3) 0.0214(6) Uani 1 1 d . . . O5 O 0.5499(2) 0.8637(2) 1.1227(3) 0.0197(5) Uani 1 1 d . . . O9 O 0.86154(18) 0.7529(2) 0.9422(3) 0.0146(5) Uani 1 1 d . . . C2 C 0.5532(3) 0.8304(3) 0.9689(5) 0.0154(7) Uani 1 1 d . . . O7 O 0.6364(2) 0.7706(2) 0.9193(3) 0.0153(5) Uani 1 1 d . . . C4 C 0.4628(3) 0.8584(3) 0.8389(5) 0.0224(8) Uani 1 1 d . . . H4A H 0.4055 0.9036 0.8964 0.034 Uiso 1 1 calc R . . H4B H 0.4293 0.7890 0.7942 0.034 Uiso 1 1 calc R . . H4C H 0.4947 0.9007 0.7410 0.034 Uiso 1 1 calc R . . C5 C 1.0218(3) 0.8474(3) 1.5476(5) 0.0256(9) Uani 1 1 d . . . H5A H 1.0771 0.8996 1.5000 0.038 Uiso 1 1 calc R . . H5B H 1.0591 0.7780 1.5836 0.038 Uiso 1 1 calc R . . H5C H 0.9856 0.8814 1.6496 0.038 Uiso 1 1 calc R . . C8 C 0.6756(4) 0.4153(3) 1.1044(5) 0.0271(9) Uani 1 1 d . . . H8A H 0.6025 0.4220 1.1605 0.041 Uiso 1 1 calc R . . H8B H 0.7296 0.3843 1.1886 0.041 Uiso 1 1 calc R . . H8C H 0.6695 0.3655 1.0023 0.041 Uiso 1 1 calc R . . C7 C 0.7145(3) 0.5302(3) 1.0450(4) 0.0147(7) Uani 1 1 d . . . C6 C 0.8354(4) 1.0607(3) 1.0243(6) 0.0298(9) Uani 1 1 d . . . H6A H 0.8523 1.0707 1.1496 0.045 Uiso 1 1 calc R . . H6B H 0.7985 1.1281 0.9788 0.045 Uiso 1 1 calc R . . H6C H 0.9049 1.0480 0.9602 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01646(10) 0.01324(10) 0.00751(10) -0.00010(6) -0.00011(6) -0.00058(7) O3 0.0306(15) 0.0160(13) 0.0112(12) -0.0004(10) -0.0004(10) -0.0011(11) O4 0.0300(14) 0.0155(12) 0.0074(12) 0.0011(9) 0.0004(10) -0.0007(10) O6 0.0270(15) 0.0141(13) 0.0127(14) 0.0003(11) -0.0013(11) -0.0042(10) C1 0.0165(17) 0.0165(17) 0.0146(18) -0.0021(14) 0.0009(14) 0.0024(14) O2 0.0246(14) 0.0254(14) 0.0141(13) 0.0017(11) 0.0008(10) -0.0085(11) O5 0.0215(13) 0.0230(14) 0.0147(13) -0.0009(11) 0.0024(10) 0.0069(11) O9 0.0137(12) 0.0145(12) 0.0157(13) -0.0001(10) 0.0002(9) 0.0022(10) C2 0.0171(17) 0.0130(17) 0.0161(18) 0.0008(13) 0.0013(14) -0.0023(13) O7 0.0178(12) 0.0158(12) 0.0122(12) -0.0012(10) -0.0012(10) 0.0026(10) C4 0.0207(19) 0.023(2) 0.023(2) -0.0034(16) -0.0071(15) 0.0031(15) C5 0.024(2) 0.024(2) 0.028(2) 0.0040(17) -0.0078(16) -0.0061(16) C8 0.044(2) 0.0200(19) 0.0175(19) 0.0004(16) 0.0028(17) -0.0096(18) C7 0.0184(18) 0.0128(16) 0.0130(17) -0.0007(13) 0.0003(13) 0.0025(13) C6 0.038(2) 0.023(2) 0.029(2) 0.0051(17) -0.0072(18) -0.0129(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O4 2.343(2) . ? Tb1 O7 2.366(2) 4_576 ? Tb1 O6 2.419(3) . ? Tb1 O9 2.419(2) . ? Tb1 O3 2.436(2) . ? Tb1 O7 2.437(2) . ? Tb1 O9 2.480(2) 4_576 ? Tb1 O5 2.482(2) . ? Tb1 O2 2.486(2) . ? Tb1 C2 2.836(4) . ? Tb1 C1 2.841(4) . ? Tb1 Tb1 4.0128(3) 4_575 ? O3 C7 1.271(4) . ? O4 C7 1.241(4) 4_576 ? O6 C6 1.423(4) . ? C1 O2 1.234(4) . ? C1 O9 1.282(4) 4_576 ? C1 C5 1.506(5) . ? O5 C2 1.237(4) . ? O9 C1 1.282(4) 4_575 ? O9 Tb1 2.480(2) 4_575 ? C2 O7 1.286(4) . ? C2 C4 1.498(5) . ? O7 Tb1 2.366(2) 4_575 ? C8 C7 1.519(5) . ? C7 O4 1.241(4) 4_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Tb1 O7 74.13(8) . 4_576 ? O4 Tb1 O6 77.27(9) . . ? O7 Tb1 O6 142.34(9) 4_576 . ? O4 Tb1 O9 139.88(8) . . ? O7 Tb1 O9 143.59(8) 4_576 . ? O6 Tb1 O9 72.12(9) . . ? O4 Tb1 O3 142.84(8) . . ? O7 Tb1 O3 70.94(8) 4_576 . ? O6 Tb1 O3 139.74(8) . . ? O9 Tb1 O3 72.76(8) . . ? O4 Tb1 O7 125.74(8) . . ? O7 Tb1 O7 105.97(8) 4_576 . ? O6 Tb1 O7 72.20(9) . . ? O9 Tb1 O7 67.81(8) . . ? O3 Tb1 O7 76.79(8) . . ? O4 Tb1 O9 77.45(8) . 4_576 ? O7 Tb1 O9 67.92(8) 4_576 4_576 ? O6 Tb1 O9 128.25(8) . 4_576 ? O9 Tb1 O9 101.88(7) . 4_576 ? O3 Tb1 O9 78.07(8) . 4_576 ? O7 Tb1 O9 154.70(8) . 4_576 ? O4 Tb1 O5 77.08(8) . . ? O7 Tb1 O5 74.91(8) 4_576 . ? O6 Tb1 O5 75.22(9) . . ? O9 Tb1 O5 117.98(8) . . ? O3 Tb1 O5 105.16(8) . . ? O7 Tb1 O5 52.48(8) . . ? O9 Tb1 O5 139.34(8) 4_576 . ? O4 Tb1 O2 73.62(9) . . ? O7 Tb1 O2 116.24(8) 4_576 . ? O6 Tb1 O2 77.52(9) . . ? O9 Tb1 O2 74.92(8) . . ? O3 Tb1 O2 111.30(8) . . ? O7 Tb1 O2 137.45(8) . . ? O9 Tb1 O2 52.22(8) 4_576 . ? O5 Tb1 O2 143.53(9) . . ? O4 Tb1 C2 100.19(9) . . ? O7 Tb1 C2 92.12(9) 4_576 . ? O6 Tb1 C2 69.35(9) . . ? O9 Tb1 C2 92.74(9) . . ? O3 Tb1 C2 93.41(9) . . ? O7 Tb1 C2 26.88(9) . . ? O9 Tb1 C2 159.87(9) 4_576 . ? O5 Tb1 C2 25.81(9) . . ? O2 Tb1 C2 146.82(9) . . ? O4 Tb1 C1 71.01(9) . . ? O7 Tb1 C1 91.58(9) 4_576 . ? O6 Tb1 C1 101.78(10) . . ? O9 Tb1 C1 90.37(9) . . ? O3 Tb1 C1 97.49(9) . . ? O7 Tb1 C1 158.17(9) . . ? O9 Tb1 C1 26.80(9) 4_576 . ? O5 Tb1 C1 147.72(9) . . ? O2 Tb1 C1 25.71(9) . . ? C2 Tb1 C1 169.09(10) . . ? O4 Tb1 Tb1 148.07(6) . 4_575 ? O7 Tb1 Tb1 126.30(6) 4_576 4_575 ? O6 Tb1 Tb1 72.71(7) . 4_575 ? O9 Tb1 Tb1 35.51(5) . 4_575 ? O3 Tb1 Tb1 67.31(5) . 4_575 ? O7 Tb1 Tb1 32.79(6) . 4_575 ? O9 Tb1 Tb1 130.62(5) 4_576 4_575 ? O5 Tb1 Tb1 84.91(6) . 4_575 ? O2 Tb1 Tb1 109.50(6) . 4_575 ? C2 Tb1 Tb1 59.10(7) . 4_575 ? C1 Tb1 Tb1 125.54(7) . 4_575 ? C7 O3 Tb1 135.1(2) . . ? C7 O4 Tb1 140.2(2) 4_576 . ? C6 O6 Tb1 128.7(2) . . ? O2 C1 O9 120.6(3) . 4_576 ? O2 C1 C5 121.1(3) . . ? O9 C1 C5 118.3(3) 4_576 . ? O2 C1 Tb1 60.87(18) . . ? O9 C1 Tb1 60.73(17) 4_576 . ? C5 C1 Tb1 168.3(3) . . ? C1 O2 Tb1 93.4(2) . . ? C2 O5 Tb1 93.3(2) . . ? C1 O9 Tb1 137.0(2) 4_575 . ? C1 O9 Tb1 92.5(2) 4_575 4_575 ? Tb1 O9 Tb1 109.97(9) . 4_575 ? O5 C2 O7 119.1(3) . . ? O5 C2 C4 121.7(3) . . ? O7 C2 C4 119.2(3) . . ? O5 C2 Tb1 60.89(18) . . ? O7 C2 Tb1 58.97(17) . . ? C4 C2 Tb1 171.0(3) . . ? C2 O7 Tb1 148.8(2) . 4_575 ? C2 O7 Tb1 94.1(2) . . ? Tb1 O7 Tb1 113.32(9) 4_575 . ? O4 C7 O3 125.3(3) 4_575 . ? O4 C7 C8 117.6(3) 4_575 . ? O3 C7 C8 117.2(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.110 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.129