# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Li-Wei Han' 'Jian Lu' 'Tian-Fu Liu' 'Shuiying Gao' 'Rong Cao' _publ_contact_author_name 'Cao, Rong' _publ_contact_author_email rcao@fjirsm.ac.cn data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 757674' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H25 N4 Nd O17 S2' _chemical_formula_weight 753.76 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' N N 0.0061 0.0033 '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' Nd Nd -0.1943 3.0179 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.311(4) _cell_length_b 14.432(7) _cell_length_c 24.230(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.479(10) _cell_angle_gamma 90.00 _cell_volume 2556(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description trunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 2.284 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.670 _exptl_absorpt_correction_T_max 0.710 _exptl_absorpt_process_details SADABS _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _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 ; Siemens SMART 1K CCD ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 19509 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5824 _reflns_number_gt 4267 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SADABS (University of Gottingen, 1996)' _computing_cell_refinement 'SADABS (University of Gottingen, 1996)' _computing_data_reduction 'SADABS (University of Gottingen, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5824 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2232 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.191 _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 Nd1 Nd 0.39587(7) 0.74131(3) 0.15923(2) 0.0344(2) Uani 1 1 d . . . S1 S -0.1551(4) -0.00867(15) 0.14368(12) 0.0458(7) Uani 1 1 d . . . S2 S 0.5790(3) 0.80340(16) -0.22978(10) 0.0391(6) Uani 1 1 d . . . N1 N 0.0903(10) 0.3552(4) 0.0549(3) 0.0322(16) Uani 1 1 d . . . N2 N 0.1195(11) 0.4272(5) 0.0928(3) 0.0369(17) Uani 1 1 d . . . N3 N 0.2820(10) 0.5136(5) -0.0357(3) 0.0350(17) Uani 1 1 d . . . N4 N 0.3550(10) 0.5954(5) -0.0318(3) 0.0352(17) Uani 1 1 d . . . O1W O 0.7094(11) 0.6782(6) 0.1389(3) 0.069(2) Uani 1 1 d . . . O1 O 0.1264(11) 0.3313(5) -0.0395(3) 0.054(2) Uani 1 1 d . . . O2 O 0.1821(10) 0.5943(5) 0.1453(3) 0.0497(18) Uani 1 1 d . . . O2W O 0.1160(11) 0.7835(5) 0.1059(4) 0.062(2) Uani 1 1 d . . . O3 O 0.3594(10) 0.6354(4) 0.0763(3) 0.0458(17) Uani 1 1 d . . . O3W O 0.6150(10) 0.8108(4) 0.2258(3) 0.0461(16) Uani 1 1 d . . . O4W O 0.4889(12) 0.6063(5) 0.2194(3) 0.062(2) Uani 1 1 d . . . O4 O -0.3409(11) 0.0059(5) 0.1591(4) 0.071(3) Uani 1 1 d . . . O5 O -0.1382(10) -0.0766(5) 0.1000(3) 0.055(2) Uani 1 1 d . . . O5W O 0.5270(11) 0.8310(5) 0.0791(3) 0.061(2) Uani 1 1 d . . . O6 O -0.0339(12) -0.0275(5) 0.1900(3) 0.061(2) Uani 1 1 d . . . O6W O 0.3339(9) 0.9131(4) 0.1754(3) 0.0472(19) Uani 1 1 d . . . O7W O 0.5757(15) 0.9741(6) 0.2860(4) 0.091(3) Uani 1 1 d . . . O7 O 0.6608(11) 0.8900(5) -0.2127(3) 0.056(2) Uani 1 1 d . . . O8 O 0.4015(9) 0.8151(5) -0.2577(3) 0.056(2) Uani 1 1 d . . . O9 O 0.7006(11) 0.7460(4) -0.2626(3) 0.0465(18) Uani 1 1 d . . . C1 C -0.0821(12) 0.0989(6) 0.1155(4) 0.036(2) Uani 1 1 d . . . C2 C -0.0809(12) 0.1774(6) 0.1490(4) 0.038(2) Uani 1 1 d . . . H2A H -0.1173 0.1729 0.1854 0.045 Uiso 1 1 calc R . . C3 C -0.0270(14) 0.2600(6) 0.1289(4) 0.039(2) Uani 1 1 d . . . H3A H -0.0273 0.3122 0.1514 0.047 Uiso 1 1 calc R . . C4 C 0.0292(12) 0.2672(5) 0.0746(4) 0.0327(19) Uani 1 1 d . . . C5 C 0.0300(17) 0.1898(7) 0.0412(4) 0.053(3) Uani 1 1 d . . . H5A H 0.0657 0.1944 0.0047 0.064 Uiso 1 1 calc R . . C6 C -0.0231(16) 0.1047(7) 0.0627(5) 0.051(3) Uani 1 1 d . . . H6A H -0.0182 0.0517 0.0409 0.062 Uiso 1 1 calc R . . C7 C 0.1413(12) 0.3804(6) 0.0036(4) 0.035(2) Uani 1 1 d . . . C8 C 0.2174(11) 0.4721(5) 0.0090(3) 0.0283(17) Uani 1 1 d . . . C9 C 0.1940(12) 0.4932(6) 0.0655(4) 0.0334(19) Uani 1 1 d . . . C10 C 0.2494(14) 0.5794(6) 0.0982(4) 0.036(2) Uani 1 1 d . . . C11 C 0.4187(12) 0.6405(6) -0.0789(4) 0.0330(19) Uani 1 1 d . . . C12 C 0.4831(14) 0.7303(6) -0.0730(4) 0.038(2) Uani 1 1 d . . . H12A H 0.4906 0.7574 -0.0382 0.046 Uiso 1 1 calc R . . C13 C 0.5358(15) 0.7793(6) -0.1183(4) 0.043(2) Uani 1 1 d . . . H13A H 0.5717 0.8408 -0.1146 0.051 Uiso 1 1 calc R . . C14 C 0.5357(12) 0.7373(6) -0.1696(4) 0.0324(19) Uani 1 1 d . . . C15 C 0.4743(14) 0.6463(6) -0.1753(4) 0.040(2) Uani 1 1 d . . . H15A H 0.4707 0.6187 -0.2100 0.047 Uiso 1 1 calc R . . C16 C 0.4184(13) 0.5968(6) -0.1298(4) 0.037(2) Uani 1 1 d . . . H16A H 0.3814 0.5354 -0.1333 0.045 Uiso 1 1 calc R . . O8W O 0.422(4) 0.972(6) 0.029(3) 0.61(7) 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 Nd1 0.0383(4) 0.0341(3) 0.0312(3) -0.00262(18) 0.0051(2) -0.0038(2) S1 0.0479(15) 0.0249(11) 0.0651(17) 0.0029(10) 0.0121(13) -0.0049(10) S2 0.0426(14) 0.0368(12) 0.0382(13) 0.0056(9) 0.0067(11) -0.0017(10) N1 0.039(4) 0.024(3) 0.034(4) -0.004(3) 0.003(3) -0.003(3) N2 0.047(5) 0.034(4) 0.030(4) 0.001(3) 0.002(4) -0.003(3) N3 0.045(5) 0.033(4) 0.028(4) 0.004(3) 0.000(3) 0.001(3) N4 0.029(4) 0.029(4) 0.049(5) 0.007(3) 0.009(3) -0.003(3) O1W 0.047(5) 0.110(7) 0.052(5) -0.007(5) 0.012(4) 0.005(4) O1 0.079(6) 0.047(4) 0.037(4) -0.010(3) 0.008(4) -0.014(4) O2 0.066(5) 0.047(4) 0.036(4) -0.009(3) 0.011(4) -0.015(3) O2W 0.053(5) 0.041(4) 0.091(6) -0.013(4) -0.024(4) 0.011(4) O3 0.057(5) 0.037(3) 0.043(4) -0.002(3) 0.006(3) -0.009(3) O3W 0.049(4) 0.042(4) 0.047(4) -0.001(3) -0.015(3) -0.003(3) O4W 0.083(6) 0.048(4) 0.054(5) 0.009(3) -0.005(4) 0.005(4) O4 0.047(5) 0.047(4) 0.119(8) 0.006(4) 0.032(5) -0.003(3) O5 0.066(5) 0.033(4) 0.066(5) -0.007(3) 0.006(4) -0.008(3) O5W 0.065(5) 0.066(5) 0.053(5) 0.010(4) 0.010(4) -0.027(4) O6 0.084(6) 0.035(4) 0.064(5) 0.006(3) 0.004(5) -0.003(4) O6W 0.046(4) 0.020(3) 0.077(5) 0.016(3) 0.027(4) 0.009(3) O7W 0.138(9) 0.072(6) 0.063(6) -0.006(4) -0.013(6) 0.052(6) O7 0.071(5) 0.041(4) 0.058(5) 0.000(3) 0.017(4) -0.013(4) O8 0.037(4) 0.082(6) 0.048(4) 0.023(4) -0.005(3) -0.001(4) O9 0.057(5) 0.040(4) 0.044(4) 0.005(3) 0.026(4) 0.005(3) C1 0.032(5) 0.032(4) 0.044(5) 0.004(4) 0.007(4) 0.003(4) C2 0.038(5) 0.035(5) 0.041(5) 0.008(4) 0.001(4) -0.006(4) C3 0.053(6) 0.028(4) 0.037(5) 0.001(3) 0.014(5) -0.007(4) C4 0.031(5) 0.018(4) 0.049(6) 0.006(3) 0.004(4) -0.005(3) C5 0.077(8) 0.051(6) 0.032(5) -0.010(4) 0.018(5) -0.012(5) C6 0.069(8) 0.033(5) 0.052(6) -0.001(4) 0.007(6) -0.007(5) C7 0.033(5) 0.033(4) 0.039(5) -0.008(4) 0.005(4) -0.003(4) C8 0.029(4) 0.027(4) 0.029(4) 0.008(3) 0.003(4) 0.003(3) C9 0.030(5) 0.036(4) 0.033(5) -0.002(3) -0.007(4) 0.000(4) C10 0.050(6) 0.026(4) 0.034(5) -0.001(3) 0.000(4) -0.005(4) C11 0.035(5) 0.034(4) 0.030(4) 0.002(3) 0.008(4) 0.000(4) C12 0.049(6) 0.038(5) 0.027(5) 0.006(4) 0.007(4) 0.001(4) C13 0.058(7) 0.036(5) 0.035(5) -0.002(4) 0.012(5) -0.009(5) C14 0.027(4) 0.039(5) 0.031(5) 0.001(3) 0.003(4) -0.003(4) C15 0.058(6) 0.031(4) 0.030(5) -0.003(3) 0.002(4) 0.003(4) C16 0.039(5) 0.031(4) 0.041(5) 0.001(4) -0.006(4) 0.001(4) O8W 0.20(4) 0.84(12) 0.78(14) -0.48(12) -0.22(6) 0.11(7) _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 Nd1 O9 2.409(7) 4_576 ? Nd1 O3W 2.458(7) . ? Nd1 O2W 2.468(8) . ? Nd1 O4W 2.517(7) . ? Nd1 O1W 2.527(8) . ? Nd1 O3 2.532(7) . ? Nd1 O5W 2.543(7) . ? Nd1 O6W 2.553(6) . ? Nd1 O2 2.651(7) . ? Nd1 C10 2.952(9) . ? S1 O4 1.433(8) . ? S1 O6 1.438(9) . ? S1 O5 1.449(7) . ? S1 C1 1.783(9) . ? S2 O7 1.441(7) . ? S2 O8 1.458(8) . ? S2 O9 1.464(7) . ? S2 C14 1.779(9) . ? N1 C7 1.355(11) . ? N1 N2 1.400(9) . ? N1 C4 1.433(10) . ? N2 C9 1.288(10) . ? N3 N4 1.299(10) . ? N3 C8 1.336(10) . ? N4 C11 1.404(11) . ? O1 C7 1.266(10) . ? O2 C10 1.272(11) . ? O3 C10 1.266(10) . ? O9 Nd1 2.409(7) 4_675 ? C1 C6 1.363(13) . ? C1 C2 1.394(13) . ? C2 C3 1.350(11) . ? C3 C4 1.392(13) . ? C4 C5 1.380(12) . ? C5 C6 1.393(13) . ? C7 C8 1.440(11) . ? C8 C9 1.416(11) . ? C9 C10 1.524(11) . ? C11 C16 1.384(12) . ? C11 C12 1.385(12) . ? C12 C13 1.370(12) . ? C13 C14 1.382(13) . ? C14 C15 1.393(12) . ? C15 C16 1.386(12) . ? O8W O8W 1.98(14) 3_675 ? 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 O9 Nd1 O3W 80.9(3) 4_576 . ? O9 Nd1 O2W 83.9(3) 4_576 . ? O3W Nd1 O2W 139.5(2) . . ? O9 Nd1 O4W 76.1(2) 4_576 . ? O3W Nd1 O4W 77.0(2) . . ? O2W Nd1 O4W 134.6(3) . . ? O9 Nd1 O1W 137.7(3) 4_576 . ? O3W Nd1 O1W 72.3(3) . . ? O2W Nd1 O1W 136.9(3) . . ? O4W Nd1 O1W 66.5(3) . . ? O9 Nd1 O3 128.1(2) 4_576 . ? O3W Nd1 O3 145.1(2) . . ? O2W Nd1 O3 70.4(2) . . ? O4W Nd1 O3 90.8(2) . . ? O1W Nd1 O3 72.9(3) . . ? O9 Nd1 O5W 143.6(2) 4_576 . ? O3W Nd1 O5W 92.4(2) . . ? O2W Nd1 O5W 78.3(3) . . ? O4W Nd1 O5W 137.3(3) . . ? O1W Nd1 O5W 70.9(3) . . ? O3 Nd1 O5W 74.6(2) . . ? O9 Nd1 O6W 72.21(19) 4_576 . ? O3W Nd1 O6W 67.5(2) . . ? O2W Nd1 O6W 72.1(2) . . ? O4W Nd1 O6W 135.2(3) . . ? O1W Nd1 O6W 123.0(3) . . ? O3 Nd1 O6W 133.8(2) . . ? O5W Nd1 O6W 72.2(2) . . ? O9 Nd1 O2 78.6(2) 4_576 . ? O3W Nd1 O2 141.5(2) . . ? O2W Nd1 O2 69.7(2) . . ? O4W Nd1 O2 66.7(3) . . ? O1W Nd1 O2 102.8(3) . . ? O3 Nd1 O2 50.68(19) . . ? O5W Nd1 O2 122.9(2) . . ? O6W Nd1 O2 133.7(2) . . ? O9 Nd1 C10 103.9(2) 4_576 . ? O3W Nd1 C10 150.9(2) . . ? O2W Nd1 C10 69.4(2) . . ? O4W Nd1 C10 76.5(3) . . ? O1W Nd1 C10 86.4(3) . . ? O3 Nd1 C10 25.2(2) . . ? O5W Nd1 C10 99.2(3) . . ? O6W Nd1 C10 141.5(3) . . ? O2 Nd1 C10 25.5(2) . . ? O4 S1 O6 113.2(6) . . ? O4 S1 O5 112.9(5) . . ? O6 S1 O5 112.3(5) . . ? O4 S1 C1 105.5(4) . . ? O6 S1 C1 106.2(5) . . ? O5 S1 C1 106.1(4) . . ? O7 S2 O8 113.0(5) . . ? O7 S2 O9 113.1(4) . . ? O8 S2 O9 111.1(5) . . ? O7 S2 C14 108.1(4) . . ? O8 S2 C14 105.6(4) . . ? O9 S2 C14 105.4(4) . . ? C7 N1 N2 111.1(6) . . ? C7 N1 C4 129.8(7) . . ? N2 N1 C4 118.9(7) . . ? C9 N2 N1 105.8(7) . . ? N4 N3 C8 120.1(8) . . ? N3 N4 C11 120.4(8) . . ? C10 O2 Nd1 90.5(5) . . ? C10 O3 Nd1 96.2(5) . . ? S2 O9 Nd1 139.9(4) . 4_675 ? C6 C1 C2 119.9(8) . . ? C6 C1 S1 121.2(7) . . ? C2 C1 S1 118.8(7) . . ? C3 C2 C1 120.4(9) . . ? C2 C3 C4 120.1(8) . . ? C5 C4 C3 120.1(8) . . ? C5 C4 N1 121.0(8) . . ? C3 C4 N1 118.9(7) . . ? C4 C5 C6 119.2(9) . . ? C1 C6 C5 120.2(9) . . ? O1 C7 N1 125.9(8) . . ? O1 C7 C8 128.0(8) . . ? N1 C7 C8 106.2(7) . . ? N3 C8 C9 137.9(8) . . ? N3 C8 C7 118.8(8) . . ? C9 C8 C7 103.3(7) . . ? N2 C9 C8 113.5(8) . . ? N2 C9 C10 116.6(8) . . ? C8 C9 C10 129.8(8) . . ? O3 C10 O2 122.1(8) . . ? O3 C10 C9 117.9(8) . . ? O2 C10 C9 120.0(8) . . ? O3 C10 Nd1 58.5(5) . . ? O2 C10 Nd1 63.9(5) . . ? C9 C10 Nd1 174.1(7) . . ? C16 C11 C12 120.8(8) . . ? C16 C11 N4 121.3(8) . . ? C12 C11 N4 117.9(8) . . ? C13 C12 C11 120.1(9) . . ? C12 C13 C14 120.0(9) . . ? C13 C14 C15 119.8(8) . . ? C13 C14 S2 120.4(7) . . ? C15 C14 S2 119.1(7) . . ? C16 C15 C14 120.5(8) . . ? C15 C16 C11 118.7(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.801 _refine_diff_density_min -2.040 _refine_diff_density_rms 0.210 data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 776693' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H31 Er N6 O16 S2' _chemical_formula_weight 938.97 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' Er Er -0.2586 4.9576 '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 9.886(6) _cell_length_b 13.7983(2) _cell_length_c 14.3256(3) _cell_angle_alpha 85.445(7) _cell_angle_beta 71.214(5) _cell_angle_gamma 72.885(6) _cell_volume 1767.87(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 938 _exptl_absorpt_coefficient_mu 2.573 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.773 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 173(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 ; Mercury ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13852 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7583 _reflns_number_gt 6285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. SIMU restrains the anisotropic displacement parameters of atoms of the sulfonate groups to be similar. DELU enforces the main directions of movement of covalently bonded atoms are same. The DFIX restrains the distances of atoms in the sulfonate groups to reasonable values. ; _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^)+(0.0877P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7583 _refine_ls_number_parameters 525 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.137 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.33766(3) 0.303696(18) 0.265605(17) 0.04329(14) Uani 1 1 d . . . S1' S 1.2629(8) -0.3384(5) 0.0846(7) 0.0564(16) Uani 0.506(15) 1 d P A -1 S1 S 1.2619(7) -0.3171(6) 0.1234(6) 0.0527(18) Uani 0.494(15) 1 d PD A 2 S2 S 0.15466(19) 0.30097(16) -0.47044(11) 0.0554(4) Uani 1 1 d . . . O1 O 0.8553(6) -0.0750(4) -0.2008(4) 0.0676(14) Uani 1 1 d . . . O1W O 0.1431(7) 0.4562(5) 0.3127(4) 0.097(2) Uani 1 1 d . . . O2 O 0.4707(5) 0.1931(3) 0.1346(3) 0.0508(11) Uani 1 1 d . . . O2W O 0.1609(7) 0.3140(5) 0.1813(5) 0.089(2) Uani 1 1 d . . . O3 O 0.3569(5) 0.2060(4) 0.0198(4) 0.0613(13) Uani 1 1 d . . . O3W O 0.2598(6) 0.1591(4) 0.3132(4) 0.0638(13) Uani 1 1 d . . . O4' O 1.3508(19) -0.2881(10) 0.1188(15) 0.091(6) Uani 0.506(15) 1 d P A -1 O4 O 1.2528(17) -0.2770(11) 0.2150(10) 0.098(6) Uani 0.494(15) 1 d P A 2 O4W O 0.4120(11) 0.4043(4) 0.1334(4) 0.118(3) Uani 1 1 d . . . O5' O 1.185(3) -0.393(2) 0.1594(16) 0.072(6) Uani 0.506(15) 1 d P A -1 O5 O 1.4061(13) -0.3317(13) 0.0527(11) 0.092(6) Uani 0.494(15) 1 d P A 2 O5W O -0.0226(14) 0.4886(8) 0.1416(12) 0.193(6) Uani 1 1 d . . . O6' O 1.3526(13) -0.4025(8) -0.0007(9) 0.081(5) Uani 0.506(15) 1 d P A -1 O6 O 1.211(4) -0.407(3) 0.134(3) 0.143(14) Uani 0.494(15) 1 d P A 2 O6W O 1.297(2) -0.5490(9) -0.0843(13) 0.269(11) Uani 1 1 d . . . O7 O 0.0620(12) 0.3985(9) -0.4425(6) 0.200(7) Uani 1 1 d D . . O7W O 0.8585(15) 0.029(3) -0.4125(18) 0.36(3) Uani 0.50 1 d P . . O7W' O 0.833(4) 0.175(4) -0.3550(18) 0.381(11) Uani 0.50 1 d P . . O8 O 0.0868(12) 0.2251(11) -0.4722(7) 0.194(7) Uani 1 1 d . . . O9 O 0.2631(6) 0.3015(4) -0.5636(3) 0.0635(13) Uani 1 1 d . . . N1 N 0.4574(5) 0.1583(4) -0.1680(4) 0.0421(11) Uani 1 1 d . . . N2 N 0.5845(6) 0.0845(4) -0.1834(4) 0.0448(11) Uani 1 1 d . . . N3 N 0.8007(6) -0.0330(4) -0.0364(4) 0.0500(13) Uani 1 1 d . . . N4 N 0.6942(6) 0.0357(4) 0.0329(4) 0.0443(11) Uani 1 1 d . . . N5 N 0.5658(6) 0.2004(5) 0.3021(4) 0.0580(15) Uani 1 1 d . . . N6 N 0.4781(8) 0.4064(5) 0.3184(5) 0.078(2) Uani 1 1 d . . . H2A H 0.4264 0.3755 0.2980 0.093 Uiso 1 1 calc R . . H3A H 0.8664 -0.0252 0.1228 0.093 Uiso 1 1 d R . . H5A H 1.0041 -0.1943 -0.1272 0.093 Uiso 1 1 d R . . H6A H 1.1919 -0.3044 -0.0716 0.093 Uiso 1 1 d R . . H12A H 0.4451 0.1723 -0.4776 0.093 Uiso 1 1 d R . . H13A H 0.5643 0.1166 -0.3604 0.093 Uiso 1 1 d R . . H15A H 0.2053 0.2797 -0.1512 0.093 Uiso 1 1 d R . . H16A H 0.0867 0.3404 -0.2680 0.093 Uiso 1 1 d R . . H17A H 0.5558 0.0688 0.2702 0.093 Uiso 1 1 d R . . H18A H 0.7496 -0.0329 0.3207 0.093 Uiso 1 1 d R . . H19A H 0.8913 0.0372 0.3712 0.093 Uiso 1 1 d R . . H21A H 0.9310 0.2047 0.4149 0.093 Uiso 1 1 d R . . H22A H 0.8586 0.3716 0.4391 0.093 Uiso 1 1 d R . . H24A H 0.6885 0.5380 0.4104 0.093 Uiso 1 1 d R . . H25A H 0.4817 0.6328 0.3651 0.093 Uiso 1 1 d R . . H26A H 0.3545 0.5437 0.3073 0.093 Uiso 1 1 d R . . C1 C 1.1331(8) -0.2371(6) 0.0595(7) 0.070(2) Uani 1 1 d . . . C2 C 1.0381(8) -0.1532(5) 0.1199(6) 0.064(2) Uani 1 1 d . A . C3 C 0.9292(8) -0.0842(5) 0.0837(6) 0.0558(16) Uani 1 1 d . . . C4 C 0.9147(7) -0.1008(4) -0.0057(5) 0.0490(15) Uani 1 1 d . A . C5 C 1.0120(10) -0.1836(6) -0.0658(7) 0.079(2) Uani 1 1 d . . . C6 C 1.1224(11) -0.2498(6) -0.0317(9) 0.090(3) Uani 1 1 d . A . C7 C 0.7762(7) -0.0238(5) -0.1252(5) 0.0489(15) Uani 1 1 d . . . C8 C 0.6369(7) 0.0588(4) -0.1089(5) 0.0457(14) Uani 1 1 d . . . C9 C 0.5952(7) 0.0907(4) -0.0087(5) 0.0434(13) Uani 1 1 d . . . C10 C 0.4631(7) 0.1703(5) 0.0546(5) 0.0449(13) Uani 1 1 d . . . C11 C 0.2533(6) 0.2601(5) -0.3848(4) 0.0418(13) Uani 1 1 d . . . C12 C 0.3954(8) 0.1935(5) -0.4117(4) 0.0506(15) Uani 1 1 d . . . C13 C 0.4658(7) 0.1599(5) -0.3421(5) 0.0518(15) Uani 1 1 d . . . C14 C 0.3950(7) 0.1899(4) -0.2442(4) 0.0404(12) Uani 1 1 d . . . C15 C 0.2537(7) 0.2574(5) -0.2186(4) 0.0503(15) Uani 1 1 d . . . C16 C 0.1825(7) 0.2929(5) -0.2874(4) 0.0488(14) Uani 1 1 d . . . C17 C 0.6087(9) 0.0997(6) 0.2951(6) 0.068(2) Uani 1 1 d . . . C18 C 0.7255(11) 0.0379(8) 0.3229(7) 0.085(3) Uani 1 1 d . . . C19 C 0.8043(11) 0.0805(9) 0.3544(8) 0.093(3) Uani 1 1 d . . . C20 C 0.7704(10) 0.1859(10) 0.3663(7) 0.086(3) Uani 1 1 d . . . C21 C 0.8432(13) 0.2408(14) 0.3992(11) 0.119(4) Uani 1 1 d . . . C22 C 0.8058(15) 0.3388(13) 0.4111(10) 0.115(4) Uani 1 1 d . . . C23 C 0.6793(14) 0.3996(10) 0.3819(9) 0.103(4) Uani 1 1 d . . . C24 C 0.631(2) 0.5046(15) 0.3868(11) 0.151(7) Uani 1 1 d . . . C25 C 0.511(2) 0.5600(9) 0.3579(12) 0.133(5) Uani 1 1 d . . . C26 C 0.4390(16) 0.5056(8) 0.3251(10) 0.110(4) Uani 1 1 d . . . C27 C 0.6006(10) 0.3517(8) 0.3438(6) 0.074(2) Uani 1 1 d . . . C28 C 0.6447(8) 0.2444(6) 0.3369(5) 0.0630(19) 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 Er1 0.0475(2) 0.04401(18) 0.02826(17) -0.00405(10) -0.01559(12) 0.00711(12) S1' 0.050(2) 0.043(2) 0.068(4) 0.006(2) -0.016(3) -0.0043(18) S1 0.045(2) 0.045(3) 0.054(3) 0.016(2) -0.012(3) 0.001(2) S2 0.0446(8) 0.0868(12) 0.0307(7) 0.0059(7) -0.0164(7) -0.0091(8) O1 0.064(3) 0.071(3) 0.056(3) -0.021(3) -0.014(3) -0.003(3) O1W 0.101(5) 0.080(4) 0.067(4) -0.025(3) -0.031(3) 0.049(3) O2 0.065(3) 0.045(2) 0.032(2) -0.0094(17) -0.016(2) 0.003(2) O2W 0.072(4) 0.099(4) 0.079(4) -0.022(3) -0.041(3) 0.024(3) O3 0.049(3) 0.075(3) 0.050(3) -0.013(2) -0.022(2) 0.008(2) O3W 0.080(3) 0.065(3) 0.047(3) -0.005(2) -0.014(2) -0.028(3) O4' 0.074(10) 0.067(8) 0.149(18) 0.021(9) -0.057(12) -0.026(7) O4 0.098(11) 0.095(9) 0.073(9) 0.004(7) -0.042(8) 0.029(8) O4W 0.231(9) 0.050(3) 0.045(3) 0.006(2) -0.024(4) -0.022(4) O5' 0.056(8) 0.060(11) 0.069(8) 0.033(7) -0.007(6) 0.007(7) O5 0.047(7) 0.111(12) 0.074(9) 0.013(8) -0.003(6) 0.021(7) O5W 0.167(10) 0.119(7) 0.297(16) -0.047(9) -0.145(11) 0.046(7) O6' 0.069(7) 0.058(6) 0.085(9) -0.004(6) -0.012(6) 0.014(5) O6 0.14(3) 0.051(11) 0.26(4) 0.05(2) -0.09(3) -0.035(16) O6W 0.45(3) 0.125(9) 0.33(2) -0.021(11) -0.32(2) 0.010(12) O7 0.201(10) 0.225(11) 0.069(5) -0.072(6) -0.085(6) 0.158(9) O7W 0.050(8) 0.51(5) 0.24(2) 0.33(3) 0.083(12) 0.115(16) O7W' 0.328(13) 0.90(3) 0.162(19) 0.31(3) -0.168(16) -0.512 O8 0.205(10) 0.362(16) 0.164(9) 0.181(10) -0.155(8) -0.240(12) O9 0.067(3) 0.089(4) 0.032(2) 0.001(2) -0.019(2) -0.015(3) N1 0.043(3) 0.047(3) 0.035(2) -0.003(2) -0.017(2) -0.004(2) N2 0.048(3) 0.046(3) 0.041(3) 0.004(2) -0.019(2) -0.010(2) N3 0.042(3) 0.042(3) 0.054(3) -0.011(2) -0.009(2) 0.000(2) N4 0.047(3) 0.037(2) 0.044(3) 0.000(2) -0.014(2) -0.007(2) N5 0.048(3) 0.075(4) 0.044(3) 0.005(3) -0.020(3) -0.001(3) N6 0.103(6) 0.069(4) 0.071(4) 0.016(3) -0.028(4) -0.042(4) C1 0.050(4) 0.049(4) 0.100(7) 0.030(4) -0.021(4) -0.009(3) C2 0.048(4) 0.054(4) 0.083(5) 0.022(4) -0.024(4) -0.007(3) C3 0.046(3) 0.047(3) 0.067(4) 0.004(3) -0.020(3) -0.002(3) C4 0.045(3) 0.035(3) 0.063(4) 0.009(3) -0.018(3) -0.007(3) C5 0.076(5) 0.052(4) 0.089(6) -0.015(4) -0.024(5) 0.010(4) C6 0.076(6) 0.056(4) 0.106(8) 0.009(5) -0.014(5) 0.011(4) C7 0.048(3) 0.041(3) 0.056(4) -0.010(3) -0.018(3) -0.005(3) C8 0.047(3) 0.045(3) 0.043(3) -0.003(2) -0.012(3) -0.012(3) C9 0.044(3) 0.040(3) 0.044(3) 0.000(2) -0.013(3) -0.010(2) C10 0.042(3) 0.051(3) 0.040(3) 0.004(3) -0.014(3) -0.010(3) C11 0.040(3) 0.054(3) 0.027(3) 0.003(2) -0.010(2) -0.009(3) C12 0.050(3) 0.066(4) 0.028(3) -0.002(3) -0.016(3) 0.000(3) C13 0.044(3) 0.062(4) 0.039(3) -0.001(3) -0.011(3) -0.002(3) C14 0.047(3) 0.045(3) 0.033(3) 0.002(2) -0.018(2) -0.012(2) C15 0.051(3) 0.060(4) 0.031(3) -0.007(3) -0.014(3) 0.001(3) C16 0.045(3) 0.061(4) 0.031(3) -0.004(3) -0.012(3) 0.000(3) C17 0.061(4) 0.066(4) 0.063(5) 0.005(4) -0.025(4) 0.009(4) C18 0.068(5) 0.101(7) 0.075(6) 0.008(5) -0.042(5) 0.011(5) C19 0.064(5) 0.097(7) 0.092(7) 0.019(6) -0.030(5) 0.016(5) C20 0.055(5) 0.159(10) 0.061(5) 0.021(6) -0.032(4) -0.044(6) C21 0.077(7) 0.183(14) 0.119(10) 0.015(10) -0.060(7) -0.042(9) C22 0.101(9) 0.173(13) 0.120(10) 0.017(10) -0.066(8) -0.078(10) C23 0.113(9) 0.112(8) 0.110(9) 0.027(7) -0.044(7) -0.068(7) C24 0.231(18) 0.197(16) 0.118(10) 0.054(11) -0.096(12) -0.164(16) C25 0.217(17) 0.081(7) 0.141(12) 0.034(7) -0.074(12) -0.091(10) C26 0.155(11) 0.072(6) 0.119(9) 0.028(6) -0.057(8) -0.045(7) C27 0.066(5) 0.118(7) 0.058(5) 0.030(5) -0.031(4) -0.049(5) C28 0.050(4) 0.085(5) 0.049(4) 0.012(4) -0.011(3) -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 Er1 O2 2.295(4) . ? Er1 O4W 2.311(6) . ? Er1 O9 2.318(4) 1_556 ? Er1 O3W 2.321(5) . ? Er1 O1W 2.365(5) . ? Er1 O2W 2.391(6) . ? Er1 N5 2.478(6) . ? Er1 N6 2.553(7) . ? S1' O5' 1.41(2) . ? S1' O6' 1.440(14) . ? S1' O4' 1.470(16) . ? S1' C1 1.701(10) . ? S1 O5 1.426(14) . ? S1 O4 1.430(17) . ? S1 O6 1.45(4) . ? S1 C1 1.856(11) . ? S2 O7 1.391(8) . ? S2 O8 1.406(9) . ? S2 O9 1.418(5) . ? S2 C11 1.764(6) . ? O1 C7 1.239(8) . ? O2 C10 1.243(8) . ? O3 C10 1.260(8) . ? O9 Er1 2.318(4) 1_554 ? N1 N2 1.330(7) . ? N1 C14 1.401(7) . ? N2 C8 1.312(8) . ? N3 C7 1.360(9) . ? N3 N4 1.371(7) . ? N3 C4 1.403(8) . ? N4 C9 1.325(8) . ? N5 C17 1.329(10) . ? N5 C28 1.343(10) . ? N6 C26 1.310(12) . ? N6 C27 1.368(11) . ? C1 C6 1.372(14) . ? C1 C2 1.403(11) . ? C2 C3 1.418(10) . ? C3 C4 1.377(11) . ? C4 C5 1.396(10) . ? C5 C6 1.397(13) . ? C7 C8 1.471(9) . ? C8 C9 1.427(8) . ? C9 C10 1.511(8) . ? C11 C12 1.384(9) . ? C11 C16 1.388(8) . ? C12 C13 1.370(9) . ? C13 C14 1.384(8) . ? C14 C15 1.382(9) . ? C15 C16 1.369(9) . ? C17 C18 1.372(11) . ? C18 C19 1.302(16) . ? C19 C20 1.404(16) . ? C20 C21 1.383(17) . ? C20 C28 1.437(12) . ? C21 C22 1.302(19) . ? C22 C23 1.451(18) . ? C23 C24 1.39(2) . ? C23 C27 1.404(14) . ? C24 C25 1.37(2) . ? C25 C26 1.374(18) . ? C27 C28 1.418(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Er1 O4W 74.85(18) . . ? O2 Er1 O9 138.90(18) . 1_556 ? O4W Er1 O9 142.0(2) . 1_556 ? O2 Er1 O3W 75.93(17) . . ? O4W Er1 O3W 144.5(2) . . ? O9 Er1 O3W 72.95(18) 1_556 . ? O2 Er1 O1W 142.00(19) . . ? O4W Er1 O1W 79.6(3) . . ? O9 Er1 O1W 76.3(2) 1_556 . ? O3W Er1 O1W 113.5(2) . . ? O2 Er1 O2W 76.72(18) . . ? O4W Er1 O2W 78.1(3) . . ? O9 Er1 O2W 119.7(2) 1_556 . ? O3W Er1 O2W 76.0(2) . . ? O1W Er1 O2W 70.8(2) . . ? O2 Er1 N5 73.61(18) . . ? O4W Er1 N5 107.0(3) . . ? O9 Er1 N5 76.70(19) 1_556 . ? O3W Er1 N5 83.3(2) . . ? O1W Er1 N5 141.8(2) . . ? O2W Er1 N5 147.1(2) . . ? O2 Er1 N6 116.9(2) . . ? O4W Er1 N6 73.9(3) . . ? O9 Er1 N6 73.8(2) 1_556 . ? O3W Er1 N6 138.6(2) . . ? O1W Er1 N6 81.3(3) . . ? O2W Er1 N6 143.4(2) . . ? N5 Er1 N6 65.5(2) . . ? O5' S1' O6' 110.8(13) . . ? O5' S1' O4' 112.9(18) . . ? O6' S1' O4' 111.9(10) . . ? O5' S1' C1 106.7(11) . . ? O6' S1' C1 112.7(8) . . ? O4' S1' C1 101.4(7) . . ? O5 S1 O4 112.0(13) . . ? O5 S1 O6 112(2) . . ? O4 S1 O6 113.8(19) . . ? O5 S1 C1 104.3(7) . . ? O4 S1 C1 115.7(7) . . ? O6 S1 C1 97.9(17) . . ? O7 S2 O8 117.5(8) . . ? O7 S2 O9 110.6(6) . . ? O8 S2 O9 108.6(6) . . ? O7 S2 C11 107.7(4) . . ? O8 S2 C11 105.4(4) . . ? O9 S2 C11 106.4(3) . . ? C10 O2 Er1 140.2(4) . . ? S2 O9 Er1 152.0(3) . 1_554 ? N2 N1 C14 120.6(5) . . ? C8 N2 N1 117.5(5) . . ? C7 N3 N4 112.9(5) . . ? C7 N3 C4 130.5(5) . . ? N4 N3 C4 116.6(6) . . ? C9 N4 N3 107.8(5) . . ? C17 N5 C28 117.4(7) . . ? C17 N5 Er1 121.9(5) . . ? C28 N5 Er1 120.5(5) . . ? C26 N6 C27 119.0(9) . . ? C26 N6 Er1 124.9(7) . . ? C27 N6 Er1 116.1(5) . . ? C6 C1 C2 120.9(7) . . ? C6 C1 S1' 109.9(8) . . ? C2 C1 S1' 129.1(9) . . ? C6 C1 S1 129.9(7) . . ? C2 C1 S1 109.2(8) . . ? S1' C1 S1 20.3(2) . . ? C1 C2 C3 117.2(8) . . ? C4 C3 C2 121.3(7) . . ? C3 C4 C5 120.8(7) . . ? C3 C4 N3 119.3(6) . . ? C5 C4 N3 119.9(7) . . ? C6 C5 C4 118.0(9) . . ? C1 C6 C5 121.8(8) . . ? O1 C7 N3 126.6(6) . . ? O1 C7 C8 129.5(7) . . ? N3 C7 C8 103.9(5) . . ? N2 C8 C9 136.9(6) . . ? N2 C8 C7 117.7(6) . . ? C9 C8 C7 105.4(6) . . ? N4 C9 C8 109.9(5) . . ? N4 C9 C10 117.7(5) . . ? C8 C9 C10 132.4(6) . . ? O2 C10 O3 127.2(6) . . ? O2 C10 C9 117.0(6) . . ? O3 C10 C9 115.8(6) . . ? C12 C11 C16 119.9(6) . . ? C12 C11 S2 121.7(4) . . ? C16 C11 S2 118.4(5) . . ? C13 C12 C11 119.9(6) . . ? C12 C13 C14 120.8(6) . . ? C15 C14 C13 118.7(6) . . ? C15 C14 N1 116.6(5) . . ? C13 C14 N1 124.7(6) . . ? C16 C15 C14 121.4(5) . . ? C15 C16 C11 119.3(6) . . ? N5 C17 C18 124.7(9) . . ? C19 C18 C17 117.9(10) . . ? C18 C19 C20 123.2(9) . . ? C21 C20 C19 129.2(11) . . ? C21 C20 C28 115.9(12) . . ? C19 C20 C28 114.8(9) . . ? C22 C21 C20 127.2(12) . . ? C21 C22 C23 117.9(10) . . ? C24 C23 C27 116.2(12) . . ? C24 C23 C22 124.1(12) . . ? C27 C23 C22 119.7(11) . . ? C25 C24 C23 122.7(11) . . ? C26 C25 C24 116.3(12) . . ? N6 C26 C25 124.5(13) . . ? N6 C27 C23 121.2(10) . . ? N6 C27 C28 119.7(7) . . ? C23 C27 C28 119.0(9) . . ? N5 C28 C27 117.9(7) . . ? N5 C28 C20 121.9(8) . . ? C27 C28 C20 120.3(8) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 1.306 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.124 data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 776694' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H31 N6 O16 S2 Tm' _chemical_formula_weight 940.64 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' Tm Tm -0.3139 5.2483 '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 9.860(6) _cell_length_b 13.7800(2) _cell_length_c 14.2998(3) _cell_angle_alpha 85.437(7) _cell_angle_beta 71.121(5) _cell_angle_gamma 72.855(6) _cell_volume 1756.42(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 2.726 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_T_max 0.761 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 173(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 ; Mercury ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 15280 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7964 _reflns_number_gt 6684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. SIMU restrains the anisotropic displacement parameters of atoms of the sulfonate groups to be similar. DELU enforces the main directions of movement of covalently bonded atoms are same. The DFIX restrains the distances of atoms in the sulfonate groups to reasonable values. ; _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^)+(0.0877P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0129(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7964 _refine_ls_number_parameters 525 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1477 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.068 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm1 Tm 0.33741(3) 0.30342(2) 0.26572(2) 0.04356(16) Uani 1 1 d . . . S1' S 1.2649(12) -0.3383(7) 0.0767(7) 0.047(2) Uani 0.343(10) 1 d P A -1 S1 S 1.2629(6) -0.3225(5) 0.1183(5) 0.0697(19) Uani 0.657(10) 1 d PD A 2 S2 S 0.1546(2) 0.30151(18) -0.47071(14) 0.0561(5) Uani 1 1 d . . . O1 O 0.8560(8) -0.0756(5) -0.2008(5) 0.0753(19) Uani 1 1 d . . . O1W O 0.1427(8) 0.4547(5) 0.3143(5) 0.093(2) Uani 1 1 d . . . O2 O 0.4710(6) 0.1928(4) 0.1352(4) 0.0504(12) Uani 1 1 d . . . O2W O 0.1601(8) 0.3114(6) 0.1848(6) 0.091(2) Uani 1 1 d . . . O3 O 0.3581(6) 0.2077(5) 0.0182(4) 0.0626(15) Uani 1 1 d . . . O3W O 0.2596(7) 0.1600(5) 0.3139(4) 0.0627(15) Uani 1 1 d . . . O4' O 1.3554(15) -0.4023(11) -0.0004(12) 0.051(4) Uani 0.343(10) 1 d P A -1 O4 O 1.221(3) -0.237(3) 0.332(2) 0.246(14) Uani 0.657(10) 1 d P A 2 O4W O 0.4114(12) 0.4042(5) 0.1342(5) 0.113(3) Uani 1 1 d . . . O5' O 1.255(2) -0.2749(13) 0.2118(13) 0.071(6) Uani 0.343(10) 1 d P A -1 O5 O 1.4055(14) -0.3289(13) 0.0572(13) 0.124(7) Uani 0.657(10) 1 d P A 2 O5W O 0.292(2) 0.4484(9) -0.0833(15) 0.273(12) Uani 1 1 d . . . O6' O 1.3447(19) -0.2860(12) 0.1239(17) 0.053(5) Uani 0.343(10) 1 d P A -1 O6 O 1.1899(9) -0.3966(6) 0.1536(7) 0.059(3) Uani 0.657(10) 1 d P A 2 O6W O -0.0247(14) 0.4866(8) 0.1431(12) 0.180(6) Uani 1 1 d . . . O7W' O 0.883(2) 0.102(2) 0.6229(16) 0.150(11) Uani 0.50 1 d P . . O7W O 0.850(2) -0.002(3) 0.572(2) 0.27(2) Uani 0.50 1 d P . . O7 O 0.0612(15) 0.4013(10) -0.4431(7) 0.219(9) Uani 1 1 d D . . O8 O 0.0838(14) 0.2283(12) -0.4708(8) 0.204(8) Uani 1 1 d . . . O9 O 0.2647(7) 0.3021(5) -0.5645(4) 0.0642(16) Uani 1 1 d . . . N1 N 0.4558(7) 0.1583(4) -0.1671(4) 0.0439(13) Uani 1 1 d . . . N2 N 0.5843(7) 0.0847(5) -0.1830(5) 0.0448(14) Uani 1 1 d . . . N3 N 0.8014(7) -0.0322(5) -0.0361(5) 0.0515(15) Uani 1 1 d . . . N4 N 0.6954(7) 0.0357(4) 0.0334(5) 0.0457(14) Uani 1 1 d . . . N5 N 0.5635(7) 0.2014(5) 0.3020(5) 0.0548(16) Uani 1 1 d . . . N6 N 0.4767(10) 0.4064(6) 0.3201(6) 0.081(3) Uani 1 1 d . . . H2A H 0.4269 0.3734 0.3000 0.097 Uiso 1 1 calc R . . H3A H 0.8625 -0.0278 0.1256 0.097 Uiso 1 1 d R . . H5A H 1.0086 -0.1941 -0.1265 0.097 Uiso 1 1 d R . . H6A H 1.1880 -0.3081 -0.0702 0.097 Uiso 1 1 d R . . H12A H 0.4442 0.1727 -0.4769 0.097 Uiso 1 1 d R . . H13A H 0.5674 0.1172 -0.3589 0.097 Uiso 1 1 d R . . H15A H 0.2044 0.2785 -0.1492 0.097 Uiso 1 1 d R . . H16A H 0.0881 0.3426 -0.2682 0.097 Uiso 1 1 d R . . H17A H 0.5541 0.0694 0.2715 0.097 Uiso 1 1 d R . . H18A H 0.7503 -0.0329 0.3188 0.097 Uiso 1 1 d R . . H19A H 0.8904 0.0375 0.3729 0.097 Uiso 1 1 d R . . H21A H 0.9236 0.2156 0.4248 0.097 Uiso 1 1 d R . . H22A H 0.8489 0.3841 0.4392 0.097 Uiso 1 1 d R . . H24A H 0.6658 0.5484 0.4162 0.097 Uiso 1 1 d R . . H25A H 0.4625 0.6373 0.3588 0.097 Uiso 1 1 d R . . H26A H 0.3448 0.5440 0.3064 0.097 Uiso 1 1 d R . . C1 C 1.1341(9) -0.2371(7) 0.0595(9) 0.075(3) Uani 1 1 d . . . C2 C 1.0370(9) -0.1521(7) 0.1210(8) 0.065(2) Uani 1 1 d . A . C3 C 0.9278(9) -0.0851(6) 0.0853(7) 0.058(2) Uani 1 1 d . . . C4 C 0.9164(8) -0.1011(5) -0.0063(7) 0.0510(19) Uani 1 1 d . A . C5 C 1.0139(11) -0.1844(7) -0.0650(9) 0.078(3) Uani 1 1 d . . . C6 C 1.1209(12) -0.2513(8) -0.0313(11) 0.090(4) Uani 1 1 d . A . C7 C 0.7753(8) -0.0238(6) -0.1243(6) 0.0496(18) Uani 1 1 d . . . C8 C 0.6367(8) 0.0592(5) -0.1099(6) 0.0460(16) Uani 1 1 d . . . C9 C 0.5945(8) 0.0907(5) -0.0087(6) 0.0471(16) Uani 1 1 d . . . C10 C 0.4622(8) 0.1723(6) 0.0538(6) 0.0456(16) Uani 1 1 d . . . C11 C 0.2515(7) 0.2613(5) -0.3847(5) 0.0393(14) Uani 1 1 d . . . C12 C 0.3944(9) 0.1943(6) -0.4115(6) 0.0535(19) Uani 1 1 d . . . C13 C 0.4671(8) 0.1603(6) -0.3412(6) 0.0531(19) Uani 1 1 d . . . C14 C 0.3942(8) 0.1906(5) -0.2442(5) 0.0414(15) Uani 1 1 d . . . C15 C 0.2528(8) 0.2575(6) -0.2173(5) 0.0493(17) Uani 1 1 d . . . C16 C 0.1825(8) 0.2939(6) -0.2879(5) 0.0514(18) Uani 1 1 d . . . C17 C 0.6073(10) 0.1010(7) 0.2958(7) 0.068(2) Uani 1 1 d . . . C18 C 0.7254(13) 0.0393(9) 0.3233(9) 0.095(4) Uani 1 1 d . . . C19 C 0.8051(12) 0.0804(11) 0.3552(10) 0.095(4) Uani 1 1 d . . . C20 C 0.7691(11) 0.1881(13) 0.3668(8) 0.097(4) Uani 1 1 d . . . C21 C 0.8381(17) 0.2498(18) 0.4031(13) 0.138(7) Uani 1 1 d . . . C22 C 0.797(2) 0.3489(17) 0.4109(14) 0.130(7) Uani 1 1 d . . . C23 C 0.6772(15) 0.4027(12) 0.3812(10) 0.102(4) Uani 1 1 d . . . C24 C 0.620(3) 0.5101(17) 0.3873(13) 0.160(9) Uani 1 1 d . . . C25 C 0.496(3) 0.5633(13) 0.3561(14) 0.153(8) Uani 1 1 d . . . C26 C 0.4301(18) 0.5088(9) 0.3249(10) 0.106(4) Uani 1 1 d . . . C27 C 0.5979(11) 0.3535(9) 0.3455(8) 0.074(3) Uani 1 1 d . . . C28 C 0.6416(10) 0.2473(8) 0.3366(7) 0.068(2) 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 Tm1 0.0472(2) 0.0447(2) 0.0287(2) -0.00316(12) -0.01580(14) 0.00688(13) S1' 0.051(4) 0.049(3) 0.035(4) 0.009(3) -0.011(4) -0.011(3) S1 0.048(2) 0.067(3) 0.069(4) 0.031(3) -0.011(3) 0.006(2) S2 0.0442(10) 0.0904(15) 0.0296(9) 0.0054(9) -0.0159(8) -0.0093(10) O1 0.070(4) 0.079(4) 0.060(4) -0.020(3) -0.009(3) -0.004(3) O1W 0.096(5) 0.079(4) 0.071(5) -0.025(3) -0.040(4) 0.045(4) O2 0.060(3) 0.049(3) 0.036(3) -0.006(2) -0.020(2) 0.000(2) O2W 0.080(5) 0.100(5) 0.082(5) -0.022(4) -0.049(4) 0.023(4) O3 0.050(3) 0.075(4) 0.053(4) -0.015(3) -0.023(3) 0.009(3) O3W 0.073(4) 0.071(4) 0.045(3) -0.004(3) -0.014(3) -0.026(3) O4' 0.033(7) 0.041(8) 0.056(10) -0.010(7) -0.006(7) 0.016(6) O4 0.150(19) 0.43(4) 0.22(3) 0.07(3) -0.075(18) -0.17(3) O4W 0.220(10) 0.047(4) 0.047(4) 0.009(3) -0.024(5) -0.022(5) O5' 0.076(12) 0.067(11) 0.042(10) -0.008(7) -0.033(9) 0.038(9) O5 0.057(7) 0.145(13) 0.116(13) 0.061(11) -0.015(8) 0.023(8) O5W 0.46(3) 0.113(10) 0.35(2) -0.009(12) -0.34(2) 0.006(14) O6' 0.026(8) 0.041(8) 0.089(15) -0.002(8) -0.021(9) -0.003(6) O6 0.063(5) 0.035(4) 0.079(7) 0.029(4) -0.032(5) -0.012(4) O6W 0.165(11) 0.113(8) 0.261(17) -0.024(9) -0.125(11) 0.033(7) O7W' 0.065(10) 0.22(3) 0.098(16) 0.081(18) 0.012(10) -0.003(15) O7W 0.071(12) 0.32(4) 0.22(3) 0.24(3) 0.052(15) 0.075(17) O7 0.210(11) 0.256(14) 0.073(6) -0.082(7) -0.090(7) 0.181(11) O8 0.221(12) 0.39(2) 0.161(10) 0.189(12) -0.158(10) -0.257(14) O9 0.072(4) 0.099(5) 0.022(3) 0.004(3) -0.018(3) -0.022(3) N1 0.046(3) 0.048(3) 0.037(3) 0.001(2) -0.021(3) -0.005(3) N2 0.047(3) 0.051(3) 0.042(3) 0.008(3) -0.020(3) -0.017(3) N3 0.046(3) 0.044(3) 0.058(4) -0.006(3) -0.012(3) -0.007(3) N4 0.048(3) 0.042(3) 0.042(3) 0.000(2) -0.014(3) -0.006(3) N5 0.043(3) 0.066(4) 0.048(4) 0.003(3) -0.015(3) -0.003(3) N6 0.115(7) 0.081(6) 0.068(6) 0.020(4) -0.036(5) -0.055(5) C1 0.047(5) 0.049(5) 0.109(9) 0.031(5) -0.012(5) -0.006(4) C2 0.050(4) 0.057(5) 0.090(7) 0.022(5) -0.033(5) -0.011(4) C3 0.051(4) 0.044(4) 0.069(6) 0.008(4) -0.019(4) -0.004(3) C4 0.042(4) 0.039(4) 0.067(5) 0.011(3) -0.017(4) -0.006(3) C5 0.072(6) 0.058(5) 0.085(8) -0.013(5) -0.013(6) 0.004(5) C6 0.069(6) 0.057(6) 0.115(10) 0.002(6) -0.015(7) 0.011(5) C7 0.041(4) 0.045(4) 0.060(5) -0.013(3) -0.015(4) -0.005(3) C8 0.049(4) 0.048(4) 0.044(4) -0.001(3) -0.018(3) -0.014(3) C9 0.046(4) 0.044(4) 0.047(4) 0.002(3) -0.011(3) -0.010(3) C10 0.040(4) 0.048(4) 0.043(4) 0.007(3) -0.014(3) -0.005(3) C11 0.039(3) 0.043(3) 0.034(3) 0.002(3) -0.013(3) -0.009(3) C12 0.055(4) 0.066(5) 0.033(4) -0.002(3) -0.015(3) -0.005(4) C13 0.042(4) 0.069(5) 0.034(4) -0.006(3) -0.009(3) 0.003(3) C14 0.046(4) 0.043(4) 0.036(4) 0.003(3) -0.017(3) -0.010(3) C15 0.050(4) 0.062(4) 0.029(4) -0.006(3) -0.013(3) -0.003(3) C16 0.047(4) 0.065(5) 0.029(4) -0.005(3) -0.009(3) 0.002(3) C17 0.056(5) 0.075(6) 0.054(5) 0.003(4) -0.016(4) 0.009(4) C18 0.069(7) 0.099(8) 0.091(9) 0.027(7) -0.033(6) 0.015(6) C19 0.057(6) 0.121(11) 0.085(9) 0.024(7) -0.028(6) 0.006(6) C20 0.052(5) 0.189(14) 0.056(6) 0.035(8) -0.026(5) -0.043(8) C21 0.082(9) 0.26(2) 0.106(12) 0.034(15) -0.062(9) -0.069(14) C22 0.119(13) 0.205(19) 0.123(13) 0.037(14) -0.067(11) -0.104(15) C23 0.102(9) 0.138(12) 0.098(10) 0.030(8) -0.046(8) -0.071(9) C24 0.27(2) 0.189(19) 0.103(12) 0.023(12) -0.058(14) -0.19(2) C25 0.29(3) 0.109(12) 0.126(14) 0.041(10) -0.103(16) -0.121(16) C26 0.171(13) 0.066(7) 0.109(10) 0.018(6) -0.065(10) -0.058(8) C27 0.059(5) 0.108(8) 0.068(6) 0.029(6) -0.030(5) -0.039(6) C28 0.050(5) 0.105(8) 0.042(5) 0.009(5) -0.012(4) -0.018(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 Tm1 O2 2.284(5) . ? Tm1 O9 2.298(5) 1_556 ? Tm1 O4W 2.300(6) . ? Tm1 O3W 2.303(6) . ? Tm1 O1W 2.349(6) . ? Tm1 O2W 2.362(7) . ? Tm1 N5 2.449(6) . ? Tm1 N6 2.554(8) . ? S1' O4' 1.358(17) . ? S1' O6' 1.53(2) . ? S1' C1 1.660(13) . ? S1' O5' 2.14(2) . ? S1 O5 1.376(14) . ? S1 O6 1.390(10) . ? S1 C1 1.832(11) . ? S2 O8 1.386(10) . ? S2 O7 1.414(10) . ? S2 O9 1.428(6) . ? S2 C11 1.753(7) . ? O1 C7 1.251(10) . ? O2 C10 1.255(9) . ? O3 C10 1.247(9) . ? O5' O6' 1.27(3) . ? O9 Tm1 2.298(5) 1_554 ? N1 N2 1.334(8) . ? N1 C14 1.407(9) . ? N2 C8 1.291(9) . ? N3 C7 1.357(11) . ? N3 N4 1.362(8) . ? N3 C4 1.408(10) . ? N4 C9 1.341(9) . ? N5 C17 1.323(11) . ? N5 C28 1.349(12) . ? N6 C27 1.348(12) . ? N6 C26 1.350(13) . ? C1 C6 1.381(17) . ? C1 C2 1.421(14) . ? C2 C3 1.402(11) . ? C3 C4 1.390(13) . ? C4 C5 1.389(12) . ? C5 C6 1.371(15) . ? C7 C8 1.467(10) . ? C8 C9 1.436(11) . ? C9 C10 1.519(10) . ? C11 C16 1.374(10) . ? C11 C12 1.387(10) . ? C12 C13 1.392(11) . ? C13 C14 1.373(10) . ? C14 C15 1.375(10) . ? C15 C16 1.385(10) . ? C17 C18 1.376(13) . ? C18 C19 1.297(19) . ? C19 C20 1.430(19) . ? C20 C21 1.45(2) . ? C20 C28 1.458(14) . ? C21 C22 1.31(2) . ? C22 C23 1.37(2) . ? C23 C27 1.399(16) . ? C23 C24 1.42(2) . ? C24 C25 1.41(3) . ? C25 C26 1.31(2) . ? C27 C28 1.402(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Tm1 O9 138.9(2) . 1_556 ? O2 Tm1 O4W 75.2(2) . . ? O9 Tm1 O4W 141.4(3) 1_556 . ? O2 Tm1 O3W 76.1(2) . . ? O9 Tm1 O3W 73.1(2) 1_556 . ? O4W Tm1 O3W 144.9(3) . . ? O2 Tm1 O1W 142.7(2) . . ? O9 Tm1 O1W 75.8(2) 1_556 . ? O4W Tm1 O1W 79.9(3) . . ? O3W Tm1 O1W 113.0(3) . . ? O2 Tm1 O2W 77.1(2) . . ? O9 Tm1 O2W 119.2(2) 1_556 . ? O4W Tm1 O2W 79.3(3) . . ? O3W Tm1 O2W 75.0(3) . . ? O1W Tm1 O2W 71.2(3) . . ? O2 Tm1 N5 73.5(2) . . ? O9 Tm1 N5 76.3(2) 1_556 . ? O4W Tm1 N5 107.1(3) . . ? O3W Tm1 N5 83.3(2) . . ? O1W Tm1 N5 141.4(3) . . ? O2W Tm1 N5 146.9(3) . . ? O2 Tm1 N6 117.3(2) . . ? O9 Tm1 N6 72.7(2) 1_556 . ? O4W Tm1 N6 74.2(3) . . ? O3W Tm1 N6 138.1(2) . . ? O1W Tm1 N6 81.0(3) . . ? O2W Tm1 N6 144.5(3) . . ? N5 Tm1 N6 65.5(3) . . ? O4' S1' O6' 115.3(12) . . ? O4' S1' C1 119.9(10) . . ? O6' S1' C1 99.3(9) . . ? O4' S1' O5' 143.9(11) . . ? O6' S1' O5' 35.8(10) . . ? C1 S1' O5' 91.6(8) . . ? O5 S1 O6 131.5(11) . . ? O5 S1 C1 106.9(7) . . ? O6 S1 C1 100.8(6) . . ? O8 S2 O7 116.5(10) . . ? O8 S2 O9 110.0(7) . . ? O7 S2 O9 109.9(7) . . ? O8 S2 C11 105.7(4) . . ? O7 S2 C11 107.5(5) . . ? O9 S2 C11 106.6(3) . . ? C10 O2 Tm1 138.8(5) . . ? O6' O5' S1' 44.9(10) . . ? O5' O6' S1' 99.3(15) . . ? S2 O9 Tm1 151.2(4) . 1_554 ? N2 N1 C14 120.4(6) . . ? C8 N2 N1 117.7(7) . . ? C7 N3 N4 113.1(6) . . ? C7 N3 C4 130.0(7) . . ? N4 N3 C4 116.9(7) . . ? C9 N4 N3 107.2(6) . . ? C17 N5 C28 117.7(8) . . ? C17 N5 Tm1 122.4(6) . . ? C28 N5 Tm1 119.7(6) . . ? C27 N6 C26 121.4(10) . . ? C27 N6 Tm1 116.8(7) . . ? C26 N6 Tm1 121.8(8) . . ? C6 C1 C2 120.8(9) . . ? C6 C1 S1' 106.4(9) . . ? C2 C1 S1' 132.6(10) . . ? C6 C1 S1 126.8(9) . . ? C2 C1 S1 112.3(9) . . ? S1' C1 S1 20.4(3) . . ? C3 C2 C1 116.9(10) . . ? C4 C3 C2 121.3(9) . . ? C3 C4 C5 120.5(8) . . ? C3 C4 N3 118.1(7) . . ? C5 C4 N3 121.4(9) . . ? C6 C5 C4 119.2(11) . . ? C5 C6 C1 121.3(10) . . ? O1 C7 N3 126.2(8) . . ? O1 C7 C8 128.7(8) . . ? N3 C7 C8 105.1(6) . . ? N2 C8 C9 136.8(7) . . ? N2 C8 C7 118.9(7) . . ? C9 C8 C7 104.2(7) . . ? N4 C9 C8 110.3(7) . . ? N4 C9 C10 118.0(7) . . ? C8 C9 C10 131.7(7) . . ? O3 C10 O2 129.0(7) . . ? O3 C10 C9 115.4(7) . . ? O2 C10 C9 115.6(7) . . ? C16 C11 C12 119.3(7) . . ? C16 C11 S2 119.4(5) . . ? C12 C11 S2 121.3(6) . . ? C11 C12 C13 120.4(7) . . ? C14 C13 C12 119.5(7) . . ? C13 C14 C15 120.3(7) . . ? C13 C14 N1 124.0(7) . . ? C15 C14 N1 115.7(6) . . ? C14 C15 C16 120.2(7) . . ? C11 C16 C15 120.3(7) . . ? N5 C17 C18 125.0(11) . . ? C19 C18 C17 119.2(12) . . ? C18 C19 C20 121.6(10) . . ? C19 C20 C21 131.3(13) . . ? C19 C20 C28 115.3(11) . . ? C21 C20 C28 113.4(14) . . ? C22 C21 C20 126.9(15) . . ? C21 C22 C23 118.4(15) . . ? C22 C23 C27 121.3(15) . . ? C22 C23 C24 124.1(15) . . ? C27 C23 C24 114.5(14) . . ? C25 C24 C23 122.7(13) . . ? C26 C25 C24 117.0(16) . . ? C25 C26 N6 123.1(16) . . ? N6 C27 C28 118.2(9) . . ? N6 C27 C23 121.2(12) . . ? C28 C27 C23 120.6(11) . . ? N5 C28 C27 119.7(8) . . ? N5 C28 C20 121.0(11) . . ? C27 C28 C20 119.3(11) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.285 _refine_diff_density_min -1.154 _refine_diff_density_rms 0.241 # Attachment '- 776695.CIF' data_compound_8 _database_code_depnum_ccdc_archive 'CCDC 776695' #TrackingRef '- 776695.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H31 N6 O16 S2 Yb' _chemical_formula_weight 944.75 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' Yb Yb -0.3850 5.5486 '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 9.848(6) _cell_length_b 13.7706(2) _cell_length_c 14.2740(3) _cell_angle_alpha 85.445(7) _cell_angle_beta 71.158(5) _cell_angle_gamma 72.811(6) _cell_volume 1749.92(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 942 _exptl_absorpt_coefficient_mu 2.874 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.507 _exptl_absorpt_correction_T_max 0.750 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 173(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 ; Mercury ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 15274 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7957 _reflns_number_gt 6827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. SIMU restrains the anisotropic displacement parameters of atoms of the sulfonate groups to be similar. DELU enforces the main directions of movement of covalently bonded atoms are same. The DFIX restrains the distances of atoms in the sulfonate groups to reasonable values. ; _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^)+(0.0877P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0070(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7957 _refine_ls_number_parameters 525 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1847 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.201 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.33686(4) 0.30311(2) 0.26582(2) 0.04399(17) Uani 1 1 d . . . S1' S 1.2631(9) -0.3382(6) 0.0835(9) 0.0566(19) Uani 0.513(19) 1 d P A -1 S1 S 1.2647(8) -0.3171(7) 0.1222(8) 0.051(2) Uani 0.487(19) 1 d PD A 2 S2 S 0.1542(2) 0.3021(2) -0.47107(15) 0.0568(6) Uani 1 1 d . . . O1W O 0.1410(9) 0.4528(6) 0.3141(6) 0.096(3) Uani 1 1 d . . . O2W O 0.1590(9) 0.3104(7) 0.1851(6) 0.089(3) Uani 1 1 d . . . O3W O 0.2582(8) 0.1603(5) 0.3133(5) 0.0637(17) Uani 1 1 d . . . O3 O 0.4710(7) 0.1931(4) 0.1354(4) 0.0507(14) Uani 1 1 d . . . O4' O 1.3562(15) -0.3998(12) -0.0037(12) 0.078(6) Uani 0.513(19) 1 d P A -1 O4 O 1.249(2) -0.2752(14) 0.2167(16) 0.098(8) Uani 0.487(19) 1 d P A 2 O4W O 0.4089(13) 0.4041(5) 0.1344(5) 0.110(4) Uani 1 1 d . . . O2 O 0.3570(7) 0.2069(5) 0.0200(5) 0.0651(18) Uani 1 1 d . . . O5' O 1.186(4) -0.394(3) 0.159(2) 0.073(8) Uani 0.513(19) 1 d P A -1 O5 O 1.4104(19) -0.333(2) 0.0511(14) 0.099(10) Uani 0.487(19) 1 d P A 2 O5W O 0.293(2) 0.4510(11) -0.0831(15) 0.246(11) Uani 1 1 d . . . O1 O 0.8566(9) -0.0770(6) -0.2003(5) 0.078(2) Uani 1 1 d . . . O6' O 1.350(3) -0.2882(14) 0.118(2) 0.097(9) Uani 0.513(19) 1 d P A -1 O6 O 1.209(6) -0.405(3) 0.131(4) 0.136(19) Uani 0.487(19) 1 d P A 2 O6W O -0.0236(15) 0.4859(10) 0.1442(12) 0.168(6) Uani 1 1 d . . . O7W' O 0.834(4) 0.172(4) 0.647(2) 0.32(3) Uani 0.50 1 d P . . O7W O 0.859(2) 0.027(3) 0.588(2) 0.38(4) Uani 0.50 1 d P . . O7 O 0.0594(15) 0.4004(11) -0.4436(7) 0.199(9) Uani 1 1 d D . . O8 O 0.0834(17) 0.2280(14) -0.4721(9) 0.202(9) Uani 1 1 d . . . O9 O 0.2637(7) 0.3013(6) -0.5646(4) 0.0615(17) Uani 1 1 d . . . N1 N 0.4564(7) 0.1589(5) -0.1674(5) 0.0447(15) Uani 1 1 d . . . N2 N 0.5847(8) 0.0839(5) -0.1835(5) 0.0475(15) Uani 1 1 d . . . N3 N 0.8035(8) -0.0329(5) -0.0359(6) 0.0549(18) Uani 1 1 d . . . N4 N 0.6951(7) 0.0362(5) 0.0332(5) 0.0456(15) Uani 1 1 d . . . N5 N 0.5619(8) 0.2022(6) 0.3018(5) 0.0556(18) Uani 1 1 d . . . N6 N 0.4741(11) 0.4047(8) 0.3172(7) 0.078(3) Uani 1 1 d . . . C1 C 1.1325(11) -0.2364(7) 0.0602(9) 0.068(3) Uani 1 1 d . . . C2 C 1.0382(11) -0.1543(8) 0.1178(9) 0.069(3) Uani 1 1 d . A . H2A H 1.0465 -0.1440 0.1805 0.083 Uiso 1 1 calc R . . C3 C 0.9286(11) -0.0850(7) 0.0837(8) 0.061(2) Uani 1 1 d . . . H3A H 0.8630 -0.0268 0.1228 0.073 Uiso 1 1 calc R A . C4 C 0.9169(10) -0.1017(6) -0.0059(7) 0.052(2) Uani 1 1 d . A . C5 C 1.0166(13) -0.1852(8) -0.0654(10) 0.084(4) Uani 1 1 d . . . H5A H 1.0105 -0.1950 -0.1289 0.101 Uiso 1 1 calc R A . C6 C 1.1216(14) -0.2520(8) -0.0321(12) 0.096(4) Uani 1 1 d . A . H6A H 1.1882 -0.3096 -0.0717 0.115 Uiso 1 1 calc R . . C7 C 0.7757(9) -0.0230(6) -0.1254(7) 0.0490(19) Uani 1 1 d . . . C8 C 0.6355(9) 0.0595(6) -0.1096(6) 0.0450(17) Uani 1 1 d . . . C9 C 0.5943(9) 0.0912(6) -0.0078(6) 0.0463(18) Uani 1 1 d . . . C10 C 0.4626(9) 0.1725(6) 0.0542(6) 0.0443(17) Uani 1 1 d . . . C11 C 0.2529(9) 0.2612(6) -0.3856(6) 0.0426(17) Uani 1 1 d . . . C12 C 0.3946(10) 0.1952(7) -0.4120(6) 0.050(2) Uani 1 1 d . . . H12A H 0.4449 0.1741 -0.4792 0.060 Uiso 1 1 calc R . . C13 C 0.4646(9) 0.1593(7) -0.3410(6) 0.0486(19) Uani 1 1 d . . . H13A H 0.5618 0.1123 -0.3594 0.058 Uiso 1 1 calc R . . C14 C 0.3938(9) 0.1913(6) -0.2441(5) 0.0421(16) Uani 1 1 d . . . C15 C 0.2531(9) 0.2573(6) -0.2181(6) 0.0471(19) Uani 1 1 d . . . H15A H 0.2035 0.2790 -0.1510 0.057 Uiso 1 1 calc R . . C16 C 0.1818(10) 0.2928(7) -0.2882(6) 0.0495(19) Uani 1 1 d . . . H16A H 0.0840 0.3390 -0.2694 0.059 Uiso 1 1 calc R . . C17 C 0.6055(11) 0.1012(9) 0.2955(8) 0.073(3) Uani 1 1 d . . . H17A H 0.5523 0.0690 0.2691 0.087 Uiso 1 1 calc R . . C18 C 0.7228(13) 0.0402(11) 0.3249(9) 0.086(4) Uani 1 1 d . . . H18A H 0.7451 -0.0317 0.3222 0.103 Uiso 1 1 calc R . . C19 C 0.8030(14) 0.0823(12) 0.3564(10) 0.090(4) Uani 1 1 d . . . H19A H 0.8876 0.0402 0.3727 0.108 Uiso 1 1 calc R . . C20 C 0.7667(13) 0.1901(13) 0.3669(9) 0.090(4) Uani 1 1 d . . . C21 C 0.8390(17) 0.2495(19) 0.4010(13) 0.126(7) Uani 1 1 d . . . H21A H 0.9249 0.2130 0.4190 0.152 Uiso 1 1 calc R . . C22 C 0.800(2) 0.3485(19) 0.4101(15) 0.131(8) Uani 1 1 d . . . H22A H 0.8520 0.3822 0.4357 0.157 Uiso 1 1 calc R . . C23 C 0.6783(18) 0.4012(13) 0.3804(11) 0.097(4) Uani 1 1 d . . . C24 C 0.627(3) 0.5047(18) 0.3862(13) 0.139(7) Uani 1 1 d . . . H24A H 0.6768 0.5404 0.4118 0.167 Uiso 1 1 calc R . . C25 C 0.508(3) 0.5593(12) 0.3574(15) 0.136(7) Uani 1 1 d . . . H25A H 0.4779 0.6315 0.3611 0.163 Uiso 1 1 calc R . . C26 C 0.432(2) 0.5067(10) 0.3221(11) 0.104(5) Uani 1 1 d . . . H26A H 0.3489 0.5439 0.3012 0.125 Uiso 1 1 calc R . . C27 C 0.5942(13) 0.3548(11) 0.3448(8) 0.077(3) Uani 1 1 d . . . C28 C 0.6403(10) 0.2455(9) 0.3368(7) 0.065(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 Yb1 0.0495(2) 0.0435(2) 0.0300(2) -0.00362(13) -0.01600(15) 0.00486(15) S1' 0.056(3) 0.043(3) 0.069(5) 0.002(3) -0.020(3) -0.011(2) S1 0.042(3) 0.041(3) 0.058(4) 0.009(3) -0.012(3) -0.002(2) S2 0.0475(11) 0.0881(17) 0.0324(10) 0.0048(10) -0.0171(9) -0.0118(11) O1W 0.102(6) 0.080(5) 0.065(5) -0.024(4) -0.031(4) 0.045(5) O2W 0.081(5) 0.091(6) 0.087(6) -0.023(4) -0.049(5) 0.018(4) O3W 0.081(4) 0.063(4) 0.047(4) -0.005(3) -0.013(3) -0.028(3) O3 0.062(3) 0.047(3) 0.031(3) -0.007(2) -0.011(3) 0.000(3) O4' 0.055(8) 0.072(10) 0.082(11) -0.003(8) -0.007(8) 0.003(7) O4 0.086(13) 0.079(12) 0.098(15) -0.011(10) -0.033(11) 0.030(10) O4W 0.218(11) 0.042(4) 0.040(4) 0.006(3) -0.016(5) -0.020(5) O2 0.059(4) 0.075(5) 0.053(4) -0.012(3) -0.022(3) 0.001(3) O5' 0.060(11) 0.066(15) 0.072(10) 0.036(9) -0.012(9) -0.006(9) O5 0.048(9) 0.14(2) 0.061(11) 0.024(12) 0.001(8) 0.020(10) O5W 0.40(3) 0.115(11) 0.29(2) -0.005(12) -0.28(2) 0.024(14) O1 0.073(5) 0.087(6) 0.057(4) -0.031(4) -0.007(4) -0.006(4) O6' 0.096(17) 0.061(11) 0.17(3) 0.032(13) -0.077(19) -0.034(11) O6 0.13(3) 0.049(16) 0.26(6) 0.05(3) -0.09(4) -0.042(19) O6W 0.162(11) 0.106(10) 0.248(17) -0.017(10) -0.123(12) 0.015(8) O7W' 0.32(4) 0.73(9) 0.15(2) 0.25(4) -0.16(3) -0.46(6) O7W 0.051(10) 0.55(6) 0.24(3) 0.35(4) 0.076(14) 0.12(2) O7 0.191(11) 0.229(14) 0.072(6) -0.078(8) -0.078(7) 0.155(11) O8 0.243(14) 0.39(2) 0.142(10) 0.177(13) -0.156(11) -0.269(17) O9 0.060(4) 0.101(5) 0.025(3) 0.001(3) -0.015(3) -0.025(4) N1 0.047(4) 0.050(4) 0.040(3) 0.001(3) -0.024(3) -0.006(3) N2 0.053(4) 0.045(4) 0.050(4) 0.007(3) -0.023(3) -0.015(3) N3 0.053(4) 0.044(4) 0.058(5) -0.007(3) -0.012(4) -0.005(3) N4 0.049(4) 0.040(4) 0.047(4) -0.002(3) -0.017(3) -0.009(3) N5 0.048(4) 0.066(5) 0.050(4) 0.005(3) -0.021(3) -0.008(4) N6 0.090(6) 0.082(7) 0.075(6) 0.021(5) -0.030(5) -0.044(6) C1 0.058(6) 0.043(5) 0.092(8) 0.031(5) -0.020(6) -0.012(4) C2 0.059(6) 0.057(6) 0.088(8) 0.018(5) -0.029(6) -0.011(5) C3 0.059(5) 0.044(5) 0.075(7) 0.008(4) -0.027(5) -0.006(4) C4 0.045(4) 0.037(4) 0.064(6) 0.011(4) -0.012(4) -0.004(3) C5 0.073(7) 0.057(6) 0.089(9) -0.016(6) -0.002(6) 0.006(5) C6 0.082(8) 0.042(6) 0.129(12) -0.001(6) -0.012(8) 0.011(5) C7 0.049(4) 0.040(4) 0.052(5) -0.005(3) -0.012(4) -0.008(3) C8 0.044(4) 0.043(4) 0.050(4) 0.002(3) -0.018(4) -0.012(3) C9 0.042(4) 0.044(4) 0.051(5) -0.004(3) -0.012(4) -0.009(3) C10 0.042(4) 0.048(4) 0.041(4) 0.007(3) -0.012(3) -0.012(3) C11 0.045(4) 0.050(4) 0.034(4) 0.002(3) -0.015(3) -0.014(3) C12 0.053(5) 0.062(5) 0.030(4) -0.006(3) -0.014(3) -0.006(4) C13 0.041(4) 0.063(5) 0.036(4) -0.007(3) -0.010(3) -0.004(4) C14 0.058(5) 0.041(4) 0.035(4) 0.007(3) -0.023(3) -0.016(3) C15 0.047(4) 0.057(5) 0.030(4) -0.007(3) -0.013(3) 0.000(4) C16 0.053(5) 0.055(5) 0.034(4) -0.002(3) -0.014(4) -0.006(4) C17 0.059(6) 0.080(7) 0.060(6) 0.000(5) -0.026(5) 0.017(5) C18 0.067(7) 0.090(9) 0.084(8) 0.008(6) -0.037(6) 0.016(6) C19 0.065(7) 0.103(11) 0.087(9) 0.020(7) -0.033(7) 0.000(7) C20 0.060(6) 0.157(14) 0.065(7) 0.024(8) -0.032(6) -0.039(8) C21 0.071(9) 0.24(2) 0.095(11) 0.031(15) -0.050(8) -0.057(13) C22 0.106(13) 0.20(2) 0.133(15) 0.019(16) -0.063(12) -0.094(15) C23 0.116(11) 0.107(11) 0.101(10) 0.020(8) -0.046(9) -0.073(10) C24 0.19(2) 0.18(2) 0.110(13) 0.004(13) -0.060(13) -0.121(18) C25 0.22(2) 0.071(10) 0.171(19) 0.036(10) -0.104(17) -0.081(13) C26 0.163(14) 0.059(7) 0.098(10) 0.015(6) -0.046(10) -0.043(9) C27 0.069(6) 0.121(10) 0.059(6) 0.029(6) -0.023(5) -0.059(7) C28 0.048(5) 0.096(8) 0.041(5) 0.011(5) -0.006(4) -0.018(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 Yb1 O3 2.277(5) . ? Yb1 O9 2.291(5) 1_556 ? Yb1 O4W 2.294(7) . ? Yb1 O3W 2.297(7) . ? Yb1 O1W 2.337(6) . ? Yb1 O2W 2.364(8) . ? Yb1 N5 2.431(7) . ? Yb1 N6 2.498(10) . ? S1' O4' 1.442(18) . ? S1' O5' 1.43(3) . ? S1' O6' 1.45(2) . ? S1' C1 1.693(12) . ? S1 O5 1.430(18) . ? S1 O6 1.45(4) . ? S1 O4 1.45(2) . ? S1 C1 1.856(13) . ? S2 O8 1.399(12) . ? S2 O7 1.400(10) . ? S2 O9 1.418(6) . ? S2 C11 1.755(8) . ? O3 C10 1.249(10) . ? O2 C10 1.242(10) . ? O1 C7 1.248(10) . ? O9 Yb1 2.291(5) 1_554 ? N1 N2 1.339(9) . ? N1 C14 1.405(9) . ? N2 C8 1.290(10) . ? N3 N4 1.374(9) . ? N3 C7 1.378(11) . ? N3 C4 1.396(11) . ? N4 C9 1.327(10) . ? N5 C28 1.330(13) . ? N5 C17 1.330(13) . ? N6 C27 1.343(15) . ? N6 C26 1.343(15) . ? C1 C2 1.360(15) . ? C1 C6 1.394(19) . ? C2 C3 1.403(13) . ? C3 C4 1.364(14) . ? C4 C5 1.399(13) . ? C5 C6 1.351(17) . ? C7 C8 1.469(11) . ? C8 C9 1.443(11) . ? C9 C10 1.509(11) . ? C11 C16 1.379(10) . ? C11 C12 1.371(11) . ? C12 C13 1.384(11) . ? C13 C14 1.373(10) . ? C14 C15 1.365(11) . ? C15 C16 1.381(11) . ? C17 C18 1.379(13) . ? C18 C19 1.304(19) . ? C19 C20 1.43(2) . ? C20 C21 1.43(2) . ? C20 C28 1.432(15) . ? C21 C22 1.31(3) . ? C22 C23 1.38(2) . ? C23 C27 1.410(17) . ? C23 C24 1.36(2) . ? C24 C25 1.36(3) . ? C25 C26 1.41(2) . ? C27 C28 1.440(17) . ? 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 O3 Yb1 O9 138.8(2) . 1_556 ? O3 Yb1 O4W 75.1(2) . . ? O9 Yb1 O4W 141.7(3) 1_556 . ? O3 Yb1 O3W 76.3(2) . . ? O9 Yb1 O3W 73.1(2) 1_556 . ? O4W Yb1 O3W 144.5(3) . . ? O3 Yb1 O1W 142.5(2) . . ? O9 Yb1 O1W 75.9(3) 1_556 . ? O4W Yb1 O1W 79.9(3) . . ? O3W Yb1 O1W 112.3(3) . . ? O3 Yb1 O2W 77.2(2) . . ? O9 Yb1 O2W 118.9(3) 1_556 . ? O4W Yb1 O2W 79.2(4) . . ? O3W Yb1 O2W 74.3(3) . . ? O1W Yb1 O2W 70.9(3) . . ? O3 Yb1 N5 73.5(2) . . ? O9 Yb1 N5 76.5(2) 1_556 . ? O4W Yb1 N5 107.4(3) . . ? O3W Yb1 N5 83.9(3) . . ? O1W Yb1 N5 141.8(3) . . ? O2W Yb1 N5 146.9(3) . . ? O3 Yb1 N6 116.7(3) . . ? O9 Yb1 N6 73.6(3) 1_556 . ? O4W Yb1 N6 73.8(3) . . ? O3W Yb1 N6 139.0(3) . . ? O1W Yb1 N6 81.6(4) . . ? O2W Yb1 N6 144.3(3) . . ? N5 Yb1 N6 65.5(3) . . ? O4' S1' O5' 112.1(18) . . ? O4' S1' O6' 110.6(13) . . ? O5' S1' O6' 113(2) . . ? O4' S1' C1 112.9(10) . . ? O5' S1' C1 107.1(16) . . ? O6' S1' C1 100.9(10) . . ? O5 S1 O6 112(3) . . ? O5 S1 O4 114.3(17) . . ? O6 S1 O4 114(2) . . ? O5 S1 C1 105.7(9) . . ? O6 S1 C1 95(2) . . ? O4 S1 C1 113.4(9) . . ? O8 S2 O7 115.7(10) . . ? O8 S2 O9 108.8(7) . . ? O7 S2 O9 111.1(7) . . ? O8 S2 C11 105.9(5) . . ? O7 S2 C11 108.5(5) . . ? O9 S2 C11 106.2(4) . . ? C10 O3 Yb1 138.9(5) . . ? S2 O9 Yb1 151.6(4) . 1_554 ? N2 N1 C14 120.3(6) . . ? C8 N2 N1 116.5(7) . . ? N4 N3 C7 111.4(7) . . ? N4 N3 C4 117.7(8) . . ? C7 N3 C4 130.9(8) . . ? C9 N4 N3 108.7(7) . . ? C28 N5 C17 116.8(9) . . ? C28 N5 Yb1 121.0(7) . . ? C17 N5 Yb1 121.9(7) . . ? C27 N6 C26 117.8(12) . . ? C27 N6 Yb1 118.4(8) . . ? C26 N6 Yb1 123.7(10) . . ? C2 C1 C6 120.7(10) . . ? C2 C1 S1' 131.0(11) . . ? C6 C1 S1' 108.0(10) . . ? C2 C1 S1 111.2(10) . . ? C6 C1 S1 128.1(10) . . ? S1' C1 S1 20.5(2) . . ? C1 C2 C3 119.4(12) . . ? C4 C3 C2 119.5(10) . . ? C3 C4 N3 117.9(8) . . ? C3 C4 C5 120.5(9) . . ? N3 C4 C5 121.6(10) . . ? C6 C5 C4 119.7(13) . . ? C5 C6 C1 120.1(11) . . ? O1 C7 N3 124.2(8) . . ? O1 C7 C8 130.4(9) . . ? N3 C7 C8 105.3(7) . . ? N2 C8 C9 138.0(8) . . ? N2 C8 C7 117.5(8) . . ? C9 C8 C7 104.5(7) . . ? N4 C9 C8 110.1(7) . . ? N4 C9 C10 118.7(7) . . ? C8 C9 C10 131.2(7) . . ? O2 C10 O3 128.4(8) . . ? O2 C10 C9 115.9(8) . . ? O3 C10 C9 115.6(7) . . ? C16 C11 C12 119.5(7) . . ? C16 C11 S2 118.4(6) . . ? C12 C11 S2 122.0(6) . . ? C13 C12 C11 120.2(7) . . ? C12 C13 C14 120.2(7) . . ? C15 C14 C13 119.5(7) . . ? C15 C14 N1 116.5(7) . . ? C13 C14 N1 124.0(7) . . ? C14 C15 C16 120.8(7) . . ? C15 C16 C11 119.9(8) . . ? N5 C17 C18 124.1(13) . . ? C19 C18 C17 119.4(14) . . ? C18 C19 C20 121.6(11) . . ? C21 C20 C19 129.7(14) . . ? C21 C20 C28 116.2(15) . . ? C19 C20 C28 114.1(12) . . ? C22 C21 C20 127.1(16) . . ? C21 C22 C23 116.1(17) . . ? C27 C23 C24 114.3(15) . . ? C27 C23 C22 124.2(16) . . ? C24 C23 C22 121.5(16) . . ? C25 C24 C23 123.3(16) . . ? C24 C25 C26 118.5(16) . . ? N6 C26 C25 121.0(16) . . ? N6 C27 C23 125.0(14) . . ? N6 C27 C28 117.1(10) . . ? C23 C27 C28 117.9(12) . . ? N5 C28 C20 124.0(12) . . ? N5 C28 C27 117.6(9) . . ? C20 C28 C27 118.4(12) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.319 _refine_diff_density_min -1.383 _refine_diff_density_rms 0.153