# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Yan Xu' _publ_contact_author_email yanxu@njut.edu.cn _publ_section_title ; Second Structural Directing Agent (SDA) Induce the Formation of 1D Organic Templated Terbium Sulfate ; loop_ _publ_author_name 'Yan Xu' 'Lei Zheng' 'Xinmin Qiu' 'Jie Fu' 'Yan Yuan' 'Dunru Zhu' # Attachment '- 1.CIF' data_zl-22 _database_code_depnum_ccdc_archive 'CCDC 802276' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H14 N O14 S3 Tb' _chemical_formula_weight 531.24 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' S S 0.1246 0.1234 '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 9.1889(14) _cell_length_b 9.3069(14) _cell_length_c 9.5114(14) _cell_angle_alpha 71.087(2) _cell_angle_beta 78.189(2) _cell_angle_gamma 79.218(2) _cell_volume 746.78(19) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3330 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 27.00 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 5.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5500 _exptl_absorpt_correction_T_max 0.6507 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5228 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2586 _reflns_number_gt 2407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.0440P] 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 2586 _refine_ls_number_parameters 208 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.474 _refine_ls_restrained_S_all 1.474 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb -0.05118(3) -0.89092(3) 0.74285(3) 0.01793(12) Uani 1 1 d . . . S1 S 0.20134(16) -1.02014(17) 0.54354(16) 0.0190(3) Uani 1 1 d . . . S2 S 0.11831(17) -0.80918(17) 0.94624(17) 0.0227(3) Uani 1 1 d . . . S3 S -0.25905(17) -0.59283(18) 0.6780(2) 0.0294(4) Uani 1 1 d . . . O1 O 0.1906(5) -1.0743(5) 0.4182(5) 0.0291(10) Uani 1 1 d . . . O2 O 0.3570(4) -1.0419(5) 0.5642(5) 0.0277(10) Uani 1 1 d . . . O3 O 0.1348(5) -0.8591(5) 0.5184(5) 0.0279(10) Uani 1 1 d . . . O4 O 0.1095(4) -1.1040(4) 0.6838(4) 0.0217(9) Uani 1 1 d . . . O5 O -0.2984(5) -0.7420(5) 0.7860(5) 0.0279(10) Uani 1 1 d . . . O6 O -0.0970(5) -0.6279(4) 0.6188(5) 0.0271(10) Uani 1 1 d . . . O7 O -0.2784(6) -0.4781(5) 0.7537(7) 0.0508(15) Uani 1 1 d . . . O8 O -0.3458(6) -0.5458(6) 0.5559(6) 0.0551(16) Uani 1 1 d . . . O9 O 0.1827(5) -0.8595(6) 0.8105(5) 0.0323(11) Uani 1 1 d . . . O10 O 0.1772(5) -0.9199(5) 1.0797(5) 0.0284(10) Uani 1 1 d . . . O11 O -0.0443(5) -0.8189(6) 0.9642(5) 0.0393(13) Uani 1 1 d . . . O12 O 0.1517(7) -0.6582(6) 0.9258(6) 0.0563(16) Uani 1 1 d . . . O1W O 0.0146(7) -1.3961(7) 0.7102(8) 0.0550(15) Uani 1 1 d D . . H1WA H -0.078(4) -1.388(11) 0.752(10) 0.082 Uiso 1 1 d D . . H1WB H 0.035(11) -1.305(5) 0.701(11) 0.082 Uiso 1 1 d D . . H1WC H 0.030(12) -1.435(10) 0.636(7) 0.082 Uiso 1 1 d D . . O2W O 0.4436(8) -0.7605(8) 0.5975(9) 0.0669(18) Uani 1 1 d D . . H2WA H 0.428(13) -0.665(5) 0.545(11) 0.100 Uiso 1 1 d D . . H2WB H 0.366(8) -0.785(13) 0.666(9) 0.100 Uiso 1 1 d D . . H2WC H 0.483(12) -0.835(9) 0.560(12) 0.100 Uiso 1 1 d D . . N1 N 0.3618(6) -0.2197(8) -0.1043(7) 0.0426(16) Uani 1 1 d . . . H1A H 0.3215 -0.2293 -0.0076 0.051 Uiso 1 1 calc R . . H1B H 0.3038 -0.1442 -0.1621 0.051 Uiso 1 1 calc R . . C1 C 0.5139(9) -0.1737(10) -0.1312(9) 0.053(2) Uani 1 1 d . . . H1C H 0.5067 -0.0792 -0.1083 0.080 Uiso 1 1 calc R . . H1D H 0.5571 -0.1602 -0.2347 0.080 Uiso 1 1 calc R . . H1E H 0.5762 -0.2520 -0.0679 0.080 Uiso 1 1 calc R . . C2 C 0.3579(10) -0.3610(10) -0.1350(10) 0.058(2) Uani 1 1 d . . . H2A H 0.2561 -0.3817 -0.1161 0.086 Uiso 1 1 calc R . . H2B H 0.4161 -0.4434 -0.0710 0.086 Uiso 1 1 calc R . . H2C H 0.3991 -0.3517 -0.2384 0.086 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 0.01722(17) 0.01910(18) 0.01814(18) -0.00701(12) -0.00178(11) -0.00237(11) S1 0.0166(7) 0.0224(8) 0.0198(8) -0.0089(6) -0.0027(6) -0.0024(6) S2 0.0270(8) 0.0209(8) 0.0217(8) -0.0030(6) -0.0072(6) -0.0087(6) S3 0.0224(8) 0.0213(8) 0.0434(10) -0.0074(7) -0.0086(7) 0.0000(6) O1 0.023(2) 0.044(3) 0.028(2) -0.023(2) -0.0063(19) 0.001(2) O2 0.018(2) 0.036(3) 0.033(2) -0.014(2) -0.0042(18) -0.0059(19) O3 0.029(2) 0.029(2) 0.025(2) -0.011(2) -0.0026(19) 0.0012(19) O4 0.025(2) 0.017(2) 0.020(2) -0.0022(17) 0.0010(17) -0.0053(17) O5 0.020(2) 0.031(3) 0.034(3) -0.015(2) -0.0036(19) -0.0002(18) O6 0.030(2) 0.012(2) 0.031(2) 0.0027(18) 0.0019(19) -0.0058(17) O7 0.035(3) 0.027(3) 0.091(4) -0.030(3) 0.010(3) -0.007(2) O8 0.053(3) 0.036(3) 0.065(4) 0.021(3) -0.035(3) -0.017(3) O9 0.028(2) 0.049(3) 0.021(2) -0.008(2) 0.0035(19) -0.019(2) O10 0.036(3) 0.025(2) 0.020(2) 0.0077(19) -0.0105(19) -0.013(2) O11 0.022(2) 0.069(4) 0.039(3) -0.036(3) -0.006(2) 0.002(2) O12 0.086(4) 0.028(3) 0.065(4) -0.004(3) -0.049(3) -0.010(3) O1W 0.062(4) 0.037(3) 0.065(4) -0.006(3) -0.011(3) -0.019(3) O2W 0.054(4) 0.053(4) 0.091(5) -0.034(4) 0.012(3) -0.003(3) N1 0.028(3) 0.059(4) 0.037(4) -0.014(3) -0.007(3) 0.005(3) C1 0.050(5) 0.051(5) 0.054(5) -0.001(4) -0.005(4) -0.021(4) C2 0.057(6) 0.058(6) 0.058(6) -0.016(5) -0.020(4) -0.001(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 Tb1 O1 2.318(4) 2_536 ? Tb1 O6 2.347(4) . ? Tb1 O10 2.307(4) 2_537 ? Tb1 O4 2.391(4) . ? Tb1 O11 2.423(4) . ? Tb1 O3 2.419(4) . ? Tb1 O9 2.458(4) . ? Tb1 O5 2.461(4) . ? Tb1 S1 3.0095(14) . ? Tb1 S3 3.0193(16) . ? Tb1 S2 3.0623(15) . ? S1 O2 1.451(4) . ? S1 O1 1.463(4) . ? S1 O3 1.470(4) . ? S1 O4 1.487(4) . ? S2 O12 1.437(5) . ? S2 O10 1.480(4) . ? S2 O11 1.485(5) . ? S2 O9 1.487(4) . ? S3 O7 1.438(5) . ? S3 O8 1.447(5) . ? S3 O5 1.492(5) . ? S3 O6 1.495(4) . ? O1 Tb1 2.318(4) 2_536 ? O10 Tb1 2.307(4) 2_537 ? O1W H1WA 0.87(2) . ? O1W H1WB 0.88(2) . ? O1W H1WC 0.87(2) . ? O2W H2WA 0.87(2) . ? O2W H2WB 0.87(2) . ? O2W H2WC 0.87(2) . ? N1 C2 1.444(10) . ? N1 C1 1.486(9) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? 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 Tb1 O6 86.37(16) 2_536 . ? O1 Tb1 O10 83.82(16) 2_536 2_537 ? O6 Tb1 O10 138.55(15) . 2_537 ? O1 Tb1 O4 82.48(14) 2_536 . ? O6 Tb1 O4 135.13(14) . . ? O10 Tb1 O4 83.17(14) 2_537 . ? O1 Tb1 O11 148.99(15) 2_536 . ? O6 Tb1 O11 86.74(17) . . ? O10 Tb1 O11 81.54(16) 2_537 . ? O4 Tb1 O11 122.40(15) . . ? O1 Tb1 O3 80.63(15) 2_536 . ? O6 Tb1 O3 77.31(14) . . ? O10 Tb1 O3 139.63(15) 2_537 . ? O4 Tb1 O3 58.05(14) . . ? O11 Tb1 O3 126.95(15) . . ? O1 Tb1 O9 153.27(15) 2_536 . ? O6 Tb1 O9 91.62(15) . . ? O10 Tb1 O9 113.98(15) 2_537 . ? O4 Tb1 O9 80.25(15) . . ? O11 Tb1 O9 57.12(14) . . ? O3 Tb1 O9 72.95(14) . . ? O1 Tb1 O5 74.65(14) 2_536 . ? O6 Tb1 O5 58.43(14) . . ? O10 Tb1 O5 80.14(15) 2_537 . ? O4 Tb1 O5 152.90(15) . . ? O11 Tb1 O5 76.00(14) . . ? O3 Tb1 O5 129.84(14) . . ? O9 Tb1 O5 126.16(14) . . ? O1 Tb1 S1 81.47(10) 2_536 . ? O6 Tb1 S1 106.18(10) . . ? O10 Tb1 S1 111.97(12) 2_537 . ? O4 Tb1 S1 29.20(9) . . ? O11 Tb1 S1 129.42(11) . . ? O3 Tb1 S1 28.89(10) . . ? O9 Tb1 S1 73.50(11) . . ? O5 Tb1 S1 151.97(10) . . ? O1 Tb1 S3 78.51(11) 2_536 . ? O6 Tb1 S3 29.05(11) . . ? O10 Tb1 S3 109.54(12) 2_537 . ? O4 Tb1 S3 155.64(10) . . ? O11 Tb1 S3 80.87(12) . . ? O3 Tb1 S3 103.50(11) . . ? O9 Tb1 S3 111.20(12) . . ? O5 Tb1 S3 29.40(11) . . ? S1 Tb1 S3 131.16(4) . . ? O1 Tb1 S2 173.90(11) 2_536 . ? O6 Tb1 S2 87.78(11) . . ? O10 Tb1 S2 99.47(11) 2_537 . ? O4 Tb1 S2 102.96(10) . . ? O11 Tb1 S2 28.49(11) . . ? O3 Tb1 S2 99.78(11) . . ? O9 Tb1 S2 28.68(10) . . ? O5 Tb1 S2 100.75(10) . . ? S1 Tb1 S2 101.87(4) . . ? S3 Tb1 S2 95.50(4) . . ? O2 S1 O1 109.6(2) . . ? O2 S1 O3 111.6(3) . . ? O1 S1 O3 110.9(3) . . ? O2 S1 O4 110.2(3) . . ? O1 S1 O4 110.3(3) . . ? O3 S1 O4 104.2(2) . . ? O2 S1 Tb1 122.81(18) . . ? O1 S1 Tb1 127.59(18) . . ? O3 S1 Tb1 52.67(17) . . ? O4 S1 Tb1 51.66(15) . . ? O12 S2 O10 110.5(3) . . ? O12 S2 O11 113.9(3) . . ? O10 S2 O11 108.1(3) . . ? O12 S2 O9 110.8(3) . . ? O10 S2 O9 109.9(3) . . ? O11 S2 O9 103.4(3) . . ? O12 S2 Tb1 124.9(2) . . ? O10 S2 Tb1 124.63(18) . . ? O11 S2 Tb1 51.08(17) . . ? O9 S2 Tb1 52.49(18) . . ? O7 S3 O8 111.9(3) . . ? O7 S3 O5 110.8(3) . . ? O8 S3 O5 110.3(3) . . ? O7 S3 O6 110.2(3) . . ? O8 S3 O6 109.6(3) . . ? O5 S3 O6 103.7(2) . . ? O7 S3 Tb1 126.1(2) . . ? O8 S3 Tb1 121.8(3) . . ? O5 S3 Tb1 54.09(16) . . ? O6 S3 Tb1 49.68(16) . . ? S1 O1 Tb1 150.8(3) . 2_536 ? S1 O3 Tb1 98.4(2) . . ? S1 O4 Tb1 99.14(19) . . ? S3 O5 Tb1 96.5(2) . . ? S3 O6 Tb1 101.3(2) . . ? S2 O9 Tb1 98.8(2) . . ? S2 O10 Tb1 125.3(2) . 2_537 ? S2 O11 Tb1 100.4(2) . . ? H1WA O1W H1WB 99(9) . . ? H1WA O1W H1WC 113(10) . . ? H1WB O1W H1WC 123(9) . . ? H2WA O2W H2WB 110(10) . . ? H2WA O2W H2WC 124(10) . . ? H2WB O2W H2WC 111(10) . . ? C2 N1 C1 114.7(6) . . ? C2 N1 H1A 108.6 . . ? C1 N1 H1A 108.6 . . ? C2 N1 H1B 108.6 . . ? C1 N1 H1B 108.6 . . ? H1A N1 H1B 107.6 . . ? N1 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.711 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.161 # Attachment '- 2.CIF' data_zl-32 _database_code_depnum_ccdc_archive 'CCDC 802277' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H76 N9 O50 S12 Tb5' _chemical_formula_weight 2398.20 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' S S 0.1246 0.1234 '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 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.6927(15) _cell_length_b 36.783(3) _cell_length_c 10.1514(8) _cell_angle_alpha 90.00 _cell_angle_beta 114.4180(10) _cell_angle_gamma 90.00 _cell_volume 7035.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 990 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 24.80 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4656 _exptl_absorpt_coefficient_mu 5.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5389 _exptl_absorpt_correction_T_max 0.6129 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25700 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6535 _reflns_number_gt 5761 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Since o21 o22 o23 o24 o21a o22a o23a o24a are disorder with the occupace factors of 0.5, the refinement is not stable. The thermal parameters of o21 o22 o23 o24 o21a o22a o23a o24a and distances of S-O, O...O were restrained. ; _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^)+(0.1020P)^2^+32.8689P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6535 _refine_ls_number_parameters 468 _refine_ls_number_restraints 185 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1545 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.315 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.5000 0.219006(11) 0.7500 0.02075(10) Uani 1 2 d S . . Tb2 Tb 0.256047(14) 0.192820(7) 0.50647(3) 0.01802(7) Uani 1 1 d . . . Tb3 Tb 0.140122(16) 0.030628(8) 0.48304(3) 0.02705(8) Uani 1 1 d . . . S1 S 0.13115(6) 0.23310(3) 0.55989(13) 0.0102(3) Uani 1 1 d . A . S2 S 0.05924(6) 0.03541(3) 0.13728(13) 0.0119(3) Uani 1 1 d . A . S3 S 0.15668(6) 0.24824(3) 0.17447(13) 0.0095(3) Uani 1 1 d . A . S4 S 0.20253(7) 0.11191(3) 0.51445(14) 0.0149(3) Uani 1 1 d . . . S5 S 0.40370(7) 0.15671(4) 0.53449(14) 0.0167(3) Uani 1 1 d . . . S6 S 0.25016(9) -0.02336(5) 0.36641(18) 0.0338(4) Uani 1 1 d D . . O1 O 0.20176(18) 0.27999(10) 0.2450(4) 0.0134(9) Uani 1 1 d . . . O2 O 0.18186(18) 0.25216(9) 0.5120(4) 0.0106(8) Uani 1 1 d . . . O3 O 0.1871(2) 0.21500(10) 0.2578(4) 0.0168(9) Uani 1 1 d . . . O4 O 0.0984(2) 0.06485(10) 0.2374(4) 0.0185(9) Uani 1 1 d . A . O5 O 0.05796(19) 0.23986(11) 0.4525(4) 0.0203(9) Uani 1 1 d U . . O6 O 0.39165(18) 0.17489(10) 0.6558(4) 0.0141(8) Uani 1 1 d U A . O7 O 0.0845(2) 0.25445(11) 0.1662(4) 0.0192(8) Uani 1 1 d U . . O8 O 0.1528(2) 0.24446(11) 0.0267(4) 0.0198(9) Uani 1 1 d U . . O9 O 0.2375(2) 0.07733(10) 0.5028(5) 0.0218(10) Uani 1 1 d . A . O10 O 0.0894(2) 0.02838(11) 0.0303(4) 0.0208(10) Uani 1 1 d . . . O11 O 0.14751(19) 0.19402(9) 0.5592(4) 0.0173(9) Uani 1 1 d . . . O12 O 0.3382(2) 0.16311(12) 0.4023(4) 0.0233(10) Uani 1 1 d U A . O13 O 0.2509(2) 0.13266(10) 0.6415(4) 0.0189(10) Uani 1 1 d . A . O14 O 0.13660(19) 0.10129(11) 0.5272(4) 0.0202(9) Uani 1 1 d . A . O15 O 0.1397(2) 0.24535(12) 0.7018(4) 0.0249(11) Uani 1 1 d . . . O16 O 0.0672(2) 0.00248(10) 0.2277(4) 0.0201(9) Uani 1 1 d U A . O17 O -0.01565(19) 0.04615(11) 0.0588(4) 0.0199(10) Uani 1 1 d . . . O18 O 0.1881(2) 0.13519(10) 0.3867(4) 0.0204(10) Uani 1 1 d . A . O19 O 0.4657(2) 0.17548(13) 0.5306(4) 0.0272(11) Uani 1 1 d . A . O20 O 0.4161(3) 0.11818(12) 0.5626(6) 0.0402(14) Uani 1 1 d . A . O21 O 0.2320(6) 0.0154(3) 0.3576(14) 0.068(3) Uani 0.50 1 d PDU A 1 O22 O 0.3264(5) -0.0063(4) 0.4292(15) 0.078(4) Uani 0.50 1 d PDU A 1 O23 O 0.2097(4) -0.0255(3) 0.4600(10) 0.051(3) Uani 0.50 1 d PDU A 1 O24 O 0.2822(5) -0.0588(2) 0.4075(12) 0.057(3) Uani 0.50 1 d PDU A 1 O21A O 0.2388(6) -0.0077(3) 0.2228(9) 0.064(3) Uani 0.50 1 d PDU . 2 O22A O 0.3185(5) -0.0365(3) 0.4448(11) 0.049(3) Uani 0.50 1 d PDU A 2 O23A O 0.2212(4) -0.0057(2) 0.4485(9) 0.030(2) Uani 0.50 1 d PDU A 2 O24A O 0.1951(6) -0.0507(3) 0.2679(12) 0.086(4) Uani 0.50 1 d PDU . 2 N1 N 0.2957(5) 0.0741(3) 0.2893(9) 0.109(3) Uani 1 1 d . . . H1D H 0.3063 0.0886 0.3670 0.131 Uiso 1 1 calc R . . H1E H 0.2753 0.0540 0.3055 0.131 Uiso 1 1 calc R . . N2 N 0.5034(6) 0.2428(4) 0.3227(12) 0.042(3) Uani 0.50 1 d P . . N3 N 0.2268(3) 0.19411(13) -0.0660(6) 0.0238(13) Uani 1 1 d . . . H3B H 0.2421 0.2018 -0.1323 0.029 Uiso 1 1 calc R . . H3C H 0.2032 0.2126 -0.0479 0.029 Uiso 1 1 calc R . . N4 N 0.0000 -0.06417(19) 0.2500 0.0275(19) Uani 1 2 d S . . H4C H 0.0072 -0.0498 0.3264 0.033 Uiso 1 1 d R . . N5 N 0.0000 0.1267(3) 0.2500 0.075(4) Uani 1 2 d S . . H5D H 0.0376 0.1124 0.2986 0.091 Uiso 1 1 d R . . N6 N 0.3731(4) -0.0871(2) 0.2911(8) 0.065(2) Uani 1 1 d . . . H6D H 0.3338 -0.0803 0.3016 0.077 Uiso 1 1 calc R . . H6E H 0.3590 -0.1018 0.2135 0.077 Uiso 1 1 calc R . . C1 C 0.3585(7) 0.0637(4) 0.2864(14) 0.094(4) Uani 1 1 d U . . H1A H 0.3883 0.0528 0.3773 0.141 Uiso 1 1 calc R . . H1B H 0.3819 0.0846 0.2697 0.141 Uiso 1 1 calc R . . H1C H 0.3495 0.0464 0.2100 0.141 Uiso 1 1 calc R . . C2 C 0.2439(5) 0.0921(3) 0.1706(10) 0.066(3) Uani 1 1 d U . . H2A H 0.2044 0.0983 0.1928 0.099 Uiso 1 1 calc R . . H2B H 0.2280 0.0765 0.0875 0.099 Uiso 1 1 calc R . . H2C H 0.2638 0.1139 0.1505 0.099 Uiso 1 1 calc R . . C3 C 0.5000 0.2102(4) 0.2500 0.065(4) Uani 1 2 d S . . C4 C 0.5000 0.2771(4) 0.2500 0.053(3) Uani 1 2 d S . . C5 C 0.1774(4) 0.1633(2) -0.1270(8) 0.042(2) Uani 1 1 d . . . H5A H 0.1383 0.1709 -0.2139 0.064 Uiso 1 1 calc R . . H5B H 0.1599 0.1553 -0.0579 0.064 Uiso 1 1 calc R . . H5C H 0.2019 0.1436 -0.1489 0.064 Uiso 1 1 calc R . . C6 C 0.2883(4) 0.1850(2) 0.0671(9) 0.044(2) Uani 1 1 d . . . H6A H 0.3179 0.2061 0.1017 0.067 Uiso 1 1 calc R . . H6B H 0.3149 0.1659 0.0481 0.067 Uiso 1 1 calc R . . H6C H 0.2726 0.1771 0.1391 0.067 Uiso 1 1 calc R . . C7 C -0.0647(4) -0.0860(2) 0.2196(10) 0.053(2) Uani 1 1 d . . . H7A H -0.1043 -0.0700 0.2001 0.080 Uiso 1 1 calc R . . H7B H -0.0579 -0.1008 0.3019 0.080 Uiso 1 1 calc R . . H7C H -0.0739 -0.1012 0.1369 0.080 Uiso 1 1 calc R . . C8 C 0.0153(6) 0.1478(3) 0.1508(14) 0.087(4) Uani 1 1 d . . . H8A H 0.0249 0.1321 0.0856 0.131 Uiso 1 1 calc R . . H8B H 0.0561 0.1627 0.2022 0.131 Uiso 1 1 calc R . . H8C H -0.0247 0.1630 0.0970 0.131 Uiso 1 1 calc R . . C9 C 0.4131(7) -0.1081(4) 0.4108(15) 0.097(4) Uani 1 1 d U . . H9A H 0.3845 -0.1276 0.4199 0.145 Uiso 1 1 calc R . . H9B H 0.4291 -0.0933 0.4962 0.145 Uiso 1 1 calc R . . H9C H 0.4534 -0.1178 0.3989 0.145 Uiso 1 1 calc R . . C10 C 0.4026(6) -0.0540(4) 0.2538(13) 0.088(3) Uani 1 1 d U . . H10A H 0.3669 -0.0428 0.1698 0.132 Uiso 1 1 calc R . . H10B H 0.4427 -0.0604 0.2340 0.132 Uiso 1 1 calc R . . H10C H 0.4174 -0.0373 0.3335 0.132 Uiso 1 1 calc R . . O1W O 0.4671(4) -0.0099(3) 0.5970(8) 0.089(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01348(16) 0.0274(2) 0.01956(17) 0.000 0.00506(14) 0.000 Tb2 0.01584(12) 0.01810(14) 0.01841(13) 0.00009(9) 0.00535(10) -0.00124(9) Tb3 0.02642(15) 0.02035(15) 0.03196(16) 0.00132(11) 0.00963(12) -0.00428(11) S1 0.0046(5) 0.0162(6) 0.0101(5) 0.0049(4) 0.0034(4) 0.0011(4) S2 0.0120(5) 0.0099(5) 0.0135(5) -0.0014(4) 0.0050(4) 0.0005(4) S3 0.0048(5) 0.0173(6) 0.0051(5) -0.0009(4) 0.0008(4) 0.0001(4) S4 0.0131(6) 0.0094(6) 0.0209(6) 0.0004(5) 0.0056(5) -0.0032(5) S5 0.0123(6) 0.0184(6) 0.0170(6) -0.0054(5) 0.0036(5) 0.0045(5) S6 0.0410(8) 0.0276(8) 0.0371(8) 0.0102(7) 0.0207(7) 0.0082(7) O1 0.0091(15) 0.0191(18) 0.0099(15) -0.0026(14) 0.0017(13) -0.0045(14) O2 0.0085(15) 0.0116(17) 0.0129(16) 0.0028(12) 0.0056(13) -0.0021(13) O3 0.0190(18) 0.0143(18) 0.0129(17) 0.0018(14) 0.0022(14) 0.0034(15) O4 0.0233(18) 0.0145(18) 0.0156(17) -0.0067(14) 0.0061(15) -0.0083(15) O5 0.0088(15) 0.0267(17) 0.0218(16) 0.0068(15) 0.0026(13) 0.0041(14) O6 0.0132(15) 0.0171(16) 0.0106(14) -0.0033(13) 0.0035(12) 0.0009(13) O7 0.0130(12) 0.0241(14) 0.0209(13) -0.0030(11) 0.0076(10) 0.0006(11) O8 0.0219(17) 0.0273(18) 0.0110(15) 0.0002(13) 0.0076(13) 0.0024(14) O9 0.0160(16) 0.0125(18) 0.042(2) 0.0034(16) 0.0171(15) 0.0038(15) O10 0.0221(18) 0.026(2) 0.0205(17) -0.0051(15) 0.0148(14) 0.0058(16) O11 0.0136(16) 0.0100(17) 0.030(2) 0.0049(14) 0.0105(15) -0.0002(13) O12 0.0202(17) 0.0305(19) 0.0168(16) -0.0058(14) 0.0053(13) 0.0012(15) O13 0.0192(18) 0.0139(18) 0.0150(18) 0.0027(15) -0.0016(15) -0.0061(15) O14 0.0182(17) 0.0174(19) 0.0299(19) -0.0018(15) 0.0149(15) -0.0033(15) O15 0.0231(19) 0.042(2) 0.0115(17) 0.0000(16) 0.0093(15) 0.0006(18) O16 0.0216(16) 0.0116(16) 0.0222(16) 0.0058(13) 0.0042(13) -0.0005(14) O17 0.0119(17) 0.026(2) 0.0195(18) 0.0027(16) 0.0040(14) 0.0064(15) O18 0.029(2) 0.0128(18) 0.0145(17) 0.0012(14) 0.0035(15) -0.0050(16) O19 0.0128(17) 0.047(3) 0.0233(19) -0.0153(18) 0.0087(15) -0.0060(18) O20 0.050(3) 0.016(2) 0.048(3) 0.001(2) 0.014(2) 0.008(2) O21 0.055(5) 0.074(5) 0.071(5) -0.010(4) 0.022(4) 0.009(4) O22 0.061(5) 0.100(7) 0.078(6) -0.015(5) 0.034(4) -0.002(5) O23 0.048(4) 0.071(5) 0.040(4) -0.001(4) 0.024(3) 0.026(4) O24 0.067(5) 0.057(5) 0.053(5) 0.009(4) 0.033(4) 0.033(4) O21A 0.068(5) 0.079(5) 0.032(4) -0.003(4) 0.007(4) 0.035(5) O22A 0.038(4) 0.066(5) 0.045(5) -0.004(4) 0.018(4) 0.020(4) O23A 0.029(4) 0.028(4) 0.036(4) -0.006(3) 0.016(3) 0.003(3) O24A 0.089(6) 0.091(6) 0.063(5) -0.033(5) 0.015(4) 0.040(5) N1 0.180(7) 0.115(8) 0.078(4) 0.036(5) 0.100(4) 0.030(7) N2 0.034(6) 0.067(8) 0.026(5) -0.013(5) 0.014(5) 0.008(6) N3 0.030(2) 0.025(3) 0.022(2) 0.0046(19) 0.0155(19) 0.001(2) N4 0.033(4) 0.016(3) 0.028(4) 0.000 0.007(3) 0.000 N5 0.047(6) 0.035(5) 0.130(11) 0.000 0.023(7) 0.000 N6 0.051(4) 0.089(6) 0.054(4) -0.024(4) 0.023(3) -0.029(4) C1 0.099(6) 0.095(6) 0.071(6) -0.021(5) 0.020(5) -0.001(5) C2 0.082(4) 0.072(5) 0.065(4) -0.015(4) 0.051(3) -0.007(4) C3 0.051(7) 0.066(9) 0.077(9) 0.000 0.026(6) 0.000 C4 0.041(5) 0.064(8) 0.064(7) 0.000 0.032(5) 0.000 C5 0.050(4) 0.041(4) 0.025(3) 0.003(3) 0.004(3) -0.010(3) C6 0.042(4) 0.044(4) 0.040(4) 0.008(3) 0.010(3) -0.002(4) C7 0.051(4) 0.043(4) 0.056(5) 0.003(4) 0.013(4) -0.021(4) C8 0.055(6) 0.076(7) 0.100(9) 0.012(7) 0.002(6) 0.015(6) C9 0.083(6) 0.096(6) 0.099(6) -0.015(5) 0.026(5) 0.025(5) C10 0.080(5) 0.106(6) 0.097(5) -0.033(5) 0.056(4) -0.020(5) O1W 0.071(5) 0.130(7) 0.057(4) -0.018(4) 0.018(4) -0.016(5) _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 O5 2.432(4) 8_556 ? Tb1 O5 2.432(4) 7_556 ? Tb1 O7 2.441(4) 8_556 ? Tb1 O7 2.441(4) 7_556 ? Tb1 O19 2.593(4) . ? Tb1 O19 2.593(4) 2_656 ? Tb1 O6 2.608(4) . ? Tb1 O6 2.608(4) 2_656 ? Tb1 S5 3.2254(13) . ? Tb1 S5 3.2254(13) 2_656 ? Tb2 O2 2.446(3) 7_556 ? Tb2 O3 2.469(3) . ? Tb2 O1 2.511(4) 7_556 ? Tb2 O11 2.515(4) . ? Tb2 O18 2.556(4) . ? Tb2 O12 2.587(4) . ? Tb2 O13 2.628(4) . ? Tb2 O6 2.663(3) . ? Tb2 O2 2.682(4) . ? Tb2 S4 3.1882(13) . ? Tb2 S1 3.2136(13) . ? Tb2 S5 3.2346(14) . ? Tb3 O23A 2.282(8) . ? Tb3 O17 2.497(4) 2 ? Tb3 O10 2.542(4) 6_556 ? Tb3 O23 2.583(10) . ? Tb3 O21A 2.588(9) 6_556 ? Tb3 O9 2.592(4) . ? Tb3 O4 2.601(4) . ? Tb3 O16 2.614(4) . ? Tb3 O14 2.644(4) . ? Tb3 O24A 2.735(12) 6_556 ? Tb3 O21 2.747(14) . ? Tb3 S2 3.2085(13) . ? S1 O15 1.448(4) . ? S1 O5 1.476(4) . ? S1 O11 1.478(4) . ? S1 O2 1.500(4) . ? S2 O17 1.473(4) . ? S2 O4 1.477(4) . ? S2 O10 1.482(4) . ? S2 O16 1.487(4) . ? S3 O3 1.472(4) . ? S3 O8 1.476(4) . ? S3 O7 1.480(4) . ? S3 O1 1.481(4) . ? S4 O14 1.475(4) . ? S4 O13 1.476(4) . ? S4 O18 1.478(4) . ? S4 O9 1.492(4) . ? S5 O20 1.447(5) . ? S5 O19 1.472(5) . ? S5 O12 1.479(4) . ? S5 O6 1.510(4) . ? S6 O23A 1.375(9) . ? S6 O22A 1.392(9) . ? S6 O24 1.444(9) . ? S6 O21 1.469(10) . ? S6 O21A 1.493(9) . ? S6 O23 1.506(10) . ? S6 O24A 1.538(10) . ? S6 O22 1.567(10) . ? O1 Tb2 2.511(4) 7_556 ? O2 Tb2 2.446(3) 7_556 ? O5 Tb1 2.432(4) 7_556 ? O7 Tb1 2.441(4) 7_556 ? O10 Tb3 2.542(4) 6 ? O17 Tb3 2.497(4) 2 ? O21A Tb3 2.588(9) 6 ? O24A Tb3 2.735(12) 6 ? N1 C1 1.367(17) . ? N1 C2 1.405(13) . ? N1 H1D 0.9000 . ? N1 H1E 0.9000 . ? N2 C3 1.397(18) . ? N2 N2 1.42(2) 2_655 ? N2 C4 1.446(18) . ? N3 C6 1.461(9) . ? N3 C5 1.481(9) . ? N3 H3B 0.9000 . ? N3 H3C 0.9000 . ? N4 C7 1.479(9) 2 ? N4 C7 1.479(9) . ? N4 H4C 0.9000 . ? N5 C8 1.407(14) . ? N5 C8 1.407(14) 2 ? N5 H5D 0.9001 . ? N6 C9 1.387(15) . ? N6 C10 1.479(15) . ? N6 H6D 0.9000 . ? N6 H6E 0.9000 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 N2 1.397(18) 2_655 ? C4 N2 1.446(18) 2_655 ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Tb1 O5 103.05(19) 8_556 7_556 ? O5 Tb1 O7 82.63(14) 8_556 8_556 ? O5 Tb1 O7 68.33(13) 7_556 8_556 ? O5 Tb1 O7 68.33(13) 8_556 7_556 ? O5 Tb1 O7 82.63(14) 7_556 7_556 ? O7 Tb1 O7 132.86(19) 8_556 7_556 ? O5 Tb1 O19 167.04(14) 8_556 . ? O5 Tb1 O19 78.10(14) 7_556 . ? O7 Tb1 O19 85.91(14) 8_556 . ? O7 Tb1 O19 124.41(13) 7_556 . ? O5 Tb1 O19 78.10(14) 8_556 2_656 ? O5 Tb1 O19 167.04(14) 7_556 2_656 ? O7 Tb1 O19 124.41(12) 8_556 2_656 ? O7 Tb1 O19 85.91(14) 7_556 2_656 ? O19 Tb1 O19 103.7(2) . 2_656 ? O5 Tb1 O6 138.22(13) 8_556 . ? O5 Tb1 O6 91.63(12) 7_556 . ? O7 Tb1 O6 138.76(13) 8_556 . ? O7 Tb1 O6 75.27(12) 7_556 . ? O19 Tb1 O6 54.01(13) . . ? O19 Tb1 O6 79.59(12) 2_656 . ? O5 Tb1 O6 91.63(12) 8_556 2_656 ? O5 Tb1 O6 138.22(13) 7_556 2_656 ? O7 Tb1 O6 75.27(12) 8_556 2_656 ? O7 Tb1 O6 138.76(13) 7_556 2_656 ? O19 Tb1 O6 79.59(12) . 2_656 ? O19 Tb1 O6 54.02(13) 2_656 2_656 ? O6 Tb1 O6 103.05(16) . 2_656 ? O5 Tb1 S5 164.97(11) 8_556 . ? O5 Tb1 S5 85.31(10) 7_556 . ? O7 Tb1 S5 112.23(10) 8_556 . ? O7 Tb1 S5 100.94(9) 7_556 . ? O19 Tb1 S5 26.57(10) . . ? O19 Tb1 S5 90.97(10) 2_656 . ? O6 Tb1 S5 27.49(9) . . ? O6 Tb1 S5 90.18(8) 2_656 . ? O5 Tb1 S5 85.31(10) 8_556 2_656 ? O5 Tb1 S5 164.97(11) 7_556 2_656 ? O7 Tb1 S5 100.94(9) 8_556 2_656 ? O7 Tb1 S5 112.23(10) 7_556 2_656 ? O19 Tb1 S5 90.97(10) . 2_656 ? O19 Tb1 S5 26.57(10) 2_656 2_656 ? O6 Tb1 S5 90.18(8) . 2_656 ? O6 Tb1 S5 27.49(9) 2_656 2_656 ? S5 Tb1 S5 89.46(5) . 2_656 ? O2 Tb2 O3 75.40(12) 7_556 . ? O2 Tb2 O1 76.82(12) 7_556 7_556 ? O3 Tb2 O1 135.20(12) . 7_556 ? O2 Tb2 O11 123.06(12) 7_556 . ? O3 Tb2 O11 91.28(13) . . ? O1 Tb2 O11 75.50(12) 7_556 . ? O2 Tb2 O18 148.50(13) 7_556 . ? O3 Tb2 O18 79.39(12) . . ? O1 Tb2 O18 134.64(13) 7_556 . ? O11 Tb2 O18 75.64(13) . . ? O2 Tb2 O12 82.14(13) 7_556 . ? O3 Tb2 O12 85.49(13) . . ? O1 Tb2 O12 124.38(12) 7_556 . ? O11 Tb2 O12 152.89(12) . . ? O18 Tb2 O12 77.31(14) . . ? O2 Tb2 O13 150.78(11) 7_556 . ? O3 Tb2 O13 132.87(11) . . ? O1 Tb2 O13 83.32(12) 7_556 . ? O11 Tb2 O13 70.81(12) . . ? O18 Tb2 O13 54.33(11) . . ? O12 Tb2 O13 91.89(14) . . ? O2 Tb2 O6 77.60(11) 7_556 . ? O3 Tb2 O6 133.75(13) . . ? O1 Tb2 O6 71.31(12) 7_556 . ? O11 Tb2 O6 134.97(12) . . ? O18 Tb2 O6 107.96(12) . . ? O12 Tb2 O6 53.99(11) . . ? O13 Tb2 O6 75.83(12) . . ? O2 Tb2 O2 69.61(14) 7_556 . ? O3 Tb2 O2 70.05(12) . . ? O1 Tb2 O2 67.61(11) 7_556 . ? O11 Tb2 O2 53.99(11) . . ? O18 Tb2 O2 118.54(12) . . ? O12 Tb2 O2 146.21(13) . . ? O13 Tb2 O2 121.80(13) . . ? O6 Tb2 O2 131.84(10) . . ? O2 Tb2 S4 166.77(9) 7_556 . ? O3 Tb2 S4 105.93(9) . . ? O1 Tb2 S4 109.06(9) 7_556 . ? O11 Tb2 S4 70.18(8) . . ? O18 Tb2 S4 27.07(9) . . ? O12 Tb2 S4 84.83(10) . . ? O13 Tb2 S4 27.29(8) . . ? O6 Tb2 S4 92.85(8) . . ? O2 Tb2 S4 123.45(8) . . ? O2 Tb2 S1 96.66(9) 7_556 . ? O3 Tb2 S1 81.67(10) . . ? O1 Tb2 S1 67.46(9) 7_556 . ? O11 Tb2 S1 26.48(8) . . ? O18 Tb2 S1 98.06(10) . . ? O12 Tb2 S1 166.97(9) . . ? O13 Tb2 S1 95.23(10) . . ? O6 Tb2 S1 138.57(8) . . ? O2 Tb2 S1 27.64(8) . . ? S4 Tb2 S1 96.55(3) . . ? O2 Tb2 S5 80.76(9) 7_556 . ? O3 Tb2 S5 110.56(10) . . ? O1 Tb2 S5 98.72(9) 7_556 . ? O11 Tb2 S5 151.96(9) . . ? O18 Tb2 S5 90.85(10) . . ? O12 Tb2 S5 26.58(8) . . ? O13 Tb2 S5 81.32(10) . . ? O6 Tb2 S5 27.55(8) . . ? O2 Tb2 S5 149.35(8) . . ? S4 Tb2 S5 86.55(4) . . ? S1 Tb2 S5 166.12(3) . . ? O23A Tb3 O17 151.6(2) . 2 ? O23A Tb3 O10 85.2(3) . 6_556 ? O17 Tb3 O10 75.52(13) 2 6_556 ? O23A Tb3 O23 17.4(3) . . ? O17 Tb3 O23 137.9(2) 2 . ? O10 Tb3 O23 67.9(2) 6_556 . ? O23A Tb3 O21A 67.0(3) . 6_556 ? O17 Tb3 O21A 126.3(3) 2 6_556 ? O10 Tb3 O21A 76.8(3) 6_556 6_556 ? O23 Tb3 O21A 64.7(3) . 6_556 ? O23A Tb3 O9 78.6(2) . . ? O17 Tb3 O9 125.17(13) 2 . ? O10 Tb3 O9 156.90(12) 6_556 . ? O23 Tb3 O9 95.3(2) . . ? O21A Tb3 O9 81.8(3) 6_556 . ? O23A Tb3 O4 96.3(2) . . ? O17 Tb3 O4 79.41(13) 2 . ? O10 Tb3 O4 126.52(12) 6_556 . ? O23 Tb3 O4 106.1(2) . . ? O21A Tb3 O4 151.6(3) 6_556 . ? O9 Tb3 O4 72.10(12) . . ? O23A Tb3 O16 77.0(2) . . ? O17 Tb3 O16 77.88(13) 2 . ? O10 Tb3 O16 74.64(12) 6_556 . ? O23 Tb3 O16 73.0(2) . . ? O21A Tb3 O16 135.3(2) 6_556 . ? O9 Tb3 O16 116.79(14) . . ? O4 Tb3 O16 54.16(11) . . ? O23A Tb3 O14 132.4(2) . . ? O17 Tb3 O14 72.86(12) 2 . ? O10 Tb3 O14 139.92(14) 6_556 . ? O23 Tb3 O14 149.0(2) . . ? O21A Tb3 O14 103.1(2) 6_556 . ? O9 Tb3 O14 53.87(12) . . ? O4 Tb3 O14 70.44(12) . . ? O16 Tb3 O14 120.83(12) . . ? O23A Tb3 O24A 108.0(3) . 6_556 ? O17 Tb3 O24A 93.8(3) 2 6_556 ? O10 Tb3 O24A 93.1(3) 6_556 6_556 ? O23 Tb3 O24A 107.9(3) . 6_556 ? O21A Tb3 O24A 43.2(3) 6_556 6_556 ? O9 Tb3 O24A 76.7(3) . 6_556 ? O4 Tb3 O24A 135.3(2) . 6_556 ? O16 Tb3 O24A 166.5(3) . 6_556 ? O14 Tb3 O24A 65.4(2) . 6_556 ? O23A Tb3 O21 27.9(3) . . ? O17 Tb3 O21 146.1(3) 2 . ? O10 Tb3 O21 109.4(2) 6_556 . ? O23 Tb3 O21 43.7(3) . . ? O21A Tb3 O21 86.6(3) 6_556 . ? O9 Tb3 O21 60.4(2) . . ? O4 Tb3 O21 70.9(3) . . ? O16 Tb3 O21 71.7(3) . . ? O14 Tb3 O21 110.6(2) . . ? O24A Tb3 O21 118.7(4) 6_556 . ? O23A Tb3 S2 87.0(2) . . ? O17 Tb3 S2 76.49(10) 2 . ? O10 Tb3 S2 100.61(9) 6_556 . ? O23 Tb3 S2 90.2(2) . . ? O21A Tb3 S2 154.0(2) 6_556 . ? O9 Tb3 S2 94.92(10) . . ? O4 Tb3 S2 26.96(8) . . ? O16 Tb3 S2 27.22(9) . . ? O14 Tb3 S2 95.34(9) . . ? O24A Tb3 S2 160.5(2) 6_556 . ? O21 Tb3 S2 69.6(2) . . ? O15 S1 O5 110.4(3) . . ? O15 S1 O11 111.9(3) . . ? O5 S1 O11 109.1(2) . . ? O15 S1 O2 111.2(2) . . ? O5 S1 O2 108.9(2) . . ? O11 S1 O2 105.1(2) . . ? O15 S1 Tb2 122.32(18) . . ? O5 S1 Tb2 127.17(18) . . ? O11 S1 Tb2 49.36(17) . . ? O2 S1 Tb2 56.06(14) . . ? O17 S2 O4 109.3(2) . . ? O17 S2 O10 108.6(2) . . ? O4 S2 O10 110.8(2) . . ? O17 S2 O16 112.1(2) . . ? O4 S2 O16 106.4(2) . . ? O10 S2 O16 109.7(2) . . ? O17 S2 Tb3 124.21(18) . . ? O4 S2 Tb3 52.96(15) . . ? O10 S2 Tb3 127.20(15) . . ? O16 S2 Tb3 53.53(15) . . ? O3 S3 O8 109.7(2) . . ? O3 S3 O7 110.0(2) . . ? O8 S3 O7 109.2(2) . . ? O3 S3 O1 110.1(2) . . ? O8 S3 O1 108.9(2) . . ? O7 S3 O1 109.0(2) . . ? O14 S4 O13 112.2(3) . . ? O14 S4 O18 111.8(2) . . ? O13 S4 O18 106.6(2) . . ? O14 S4 O9 106.1(2) . . ? O13 S4 O9 109.5(2) . . ? O18 S4 O9 110.7(3) . . ? O14 S4 Tb2 126.37(17) . . ? O13 S4 Tb2 54.72(15) . . ? O18 S4 Tb2 51.91(15) . . ? O9 S4 Tb2 127.48(17) . . ? O14 S4 Tb3 54.21(16) . . ? O13 S4 Tb3 131.74(16) . . ? O18 S4 Tb3 121.59(16) . . ? O9 S4 Tb3 52.32(16) . . ? Tb2 S4 Tb3 173.50(5) . . ? O20 S5 O19 112.3(3) . . ? O20 S5 O12 110.9(3) . . ? O19 S5 O12 112.5(3) . . ? O20 S5 O6 110.4(3) . . ? O19 S5 O6 104.7(2) . . ? O12 S5 O6 105.7(2) . . ? O20 S5 Tb1 123.5(2) . . ? O19 S5 Tb1 51.99(17) . . ? O12 S5 Tb1 125.42(18) . . ? O6 S5 Tb1 52.86(14) . . ? O20 S5 Tb2 120.3(2) . . ? O19 S5 Tb2 127.39(19) . . ? O12 S5 Tb2 51.49(18) . . ? O6 S5 Tb2 54.64(13) . . ? Tb1 S5 Tb2 93.68(4) . . ? O23A S6 O22A 114.4(6) . . ? O23A S6 O24 121.1(6) . . ? O22A S6 O24 44.3(6) . . ? O23A S6 O21 54.0(7) . . ? O22A S6 O21 123.1(7) . . ? O24 S6 O21 165.9(6) . . ? O23A S6 O21A 118.5(6) . . ? O22A S6 O21A 113.9(7) . . ? O24 S6 O21A 119.9(7) . . ? O21 S6 O21A 68.5(7) . . ? O23A S6 O23 31.5(5) . . ? O22A S6 O23 108.6(6) . . ? O24 S6 O23 94.5(6) . . ? O21 S6 O23 83.9(7) . . ? O21A S6 O23 137.1(6) . . ? O23A S6 O24A 108.1(6) . . ? O22A S6 O24A 116.8(7) . . ? O24 S6 O24A 74.2(6) . . ? O21 S6 O24A 119.5(6) . . ? O21A S6 O24A 80.9(6) . . ? O23 S6 O24A 85.4(6) . . ? O23A S6 O22 100.5(6) . . ? O22A S6 O22 45.0(7) . . ? O24 S6 O22 88.8(6) . . ? O21 S6 O22 79.9(6) . . ? O21A S6 O22 88.2(7) . . ? O23 S6 O22 119.5(7) . . ? O24A S6 O22 151.3(7) . . ? S3 O1 Tb2 133.5(2) . 7_556 ? S1 O2 Tb2 150.6(2) . 7_556 ? S1 O2 Tb2 96.30(16) . . ? Tb2 O2 Tb2 110.39(14) 7_556 . ? S3 O3 Tb2 142.3(2) . . ? S2 O4 Tb3 100.08(19) . . ? S1 O5 Tb1 136.5(3) . 7_556 ? S5 O6 Tb1 99.65(19) . . ? S5 O6 Tb2 97.80(15) . . ? Tb1 O6 Tb2 126.77(14) . . ? S3 O7 Tb1 153.4(2) . 7_556 ? S4 O9 Tb3 100.6(2) . . ? S2 O10 Tb3 128.3(2) . 6 ? S1 O11 Tb2 104.2(2) . . ? S5 O12 Tb2 101.9(2) . . ? S4 O13 Tb2 97.98(18) . . ? S4 O14 Tb3 98.9(2) . . ? S2 O16 Tb3 99.25(18) . . ? S2 O17 Tb3 144.2(3) . 2 ? S4 O18 Tb2 101.02(18) . . ? S5 O19 Tb1 101.4(2) . . ? S6 O21 Tb3 112.3(7) . . ? S6 O23 Tb3 119.4(6) . . ? S6 O21A Tb3 122.5(6) . 6 ? S6 O23A Tb3 154.5(5) . . ? S6 O24A Tb3 112.6(6) . 6 ? C1 N1 C2 120.6(10) . . ? C1 N1 H1D 107.2 . . ? C2 N1 H1D 107.2 . . ? C1 N1 H1E 107.2 . . ? C2 N1 H1E 107.2 . . ? H1D N1 H1E 106.8 . . ? C3 N2 N2 59.4(6) . 2_655 ? C3 N2 C4 119.9(10) . . ? N2 N2 C4 60.5(6) 2_655 . ? C6 N3 C5 113.5(5) . . ? C6 N3 H3B 108.9 . . ? C5 N3 H3B 108.9 . . ? C6 N3 H3C 108.9 . . ? C5 N3 H3C 108.9 . . ? H3B N3 H3C 107.7 . . ? C7 N4 C7 114.4(8) 2 . ? C7 N4 H4C 109.1 2 . ? C7 N4 H4C 108.1 . . ? C8 N5 C8 113.1(13) . 2 ? C8 N5 H5D 108.5 . . ? C8 N5 H5D 109.3 2 . ? C9 N6 C10 121.5(9) . . ? C9 N6 H6D 107.0 . . ? C10 N6 H6D 107.0 . . ? C9 N6 H6E 107.0 . . ? C10 N6 H6E 107.0 . . ? H6D N6 H6E 106.7 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 N2 61.3(13) . 2_655 ? N2 C4 N2 59.0(11) 2_655 . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 H7A 109.5 . . ? N4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N5 C8 H8A 109.5 . . ? N5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 H9A 109.5 . . ? N6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 H10A 109.5 . . ? N6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.540 _refine_diff_density_min -1.427 _refine_diff_density_rms 0.249