Supplementary information (ESI) for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'CrystEngComm' _journal_coden_Cambridge 1350 _publ_contact_author_name 'Lin Xu' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 CHINA ; _publ_contact_author_email LINXU@NENU.EDU.CN _publ_section_title ; 1D lanthanide(III) complexes with disulfide ligand generated in site ; loop_ _publ_author_name 'Lin Xu.' 'Bo Bi.' 'Lihua Fan.' 'Fengyan Li.' 'Xizheng Liu.' data_1 _database_code_depnum_ccdc_archive 'CCDC 642851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H29 Dy N3 O10 S6' _chemical_formula_weight 874.36 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' Dy Dy -0.1892 4.4098 '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 7.8528(16) _cell_length_b 11.780(2) _cell_length_c 17.456(4) _cell_angle_alpha 93.85(3) _cell_angle_beta 94.70(3) _cell_angle_gamma 91.87(3) _cell_volume 1604.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15096 _cell_measurement_theta_min 6.03 _cell_measurement_theta_max 55.22 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 2.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4898 _exptl_absorpt_correction_T_max 0.6067 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type RAXIS-RAPID _diffrn_measurement_method w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15660 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7181 _reflns_number_gt 6632 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+1.4179P] 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 7181 _refine_ls_number_parameters 405 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.221 _refine_ls_restrained_S_all 1.221 _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 Dy1 Dy -0.218687(18) -0.412137(12) -0.244210(8) 0.02022(5) Uani 1 1 d . . . S1 S -0.02456(12) -0.07116(8) -0.03983(5) 0.0359(2) Uani 1 1 d . . . S2 S -0.32901(10) -0.83236(7) -0.24321(5) 0.02787(17) Uani 1 1 d . . . S3 S -0.33067(11) -1.00516(7) -0.25559(5) 0.02817(17) Uani 1 1 d . . . S4 S 0.09687(12) -0.19423(8) -0.25642(6) 0.03370(19) Uani 1 1 d . . . S5 S 0.03602(14) -0.51960(9) -0.09348(5) 0.0414(2) Uani 1 1 d . . . S6 S -0.16666(12) -0.55120(8) -0.42642(5) 0.03197(18) Uani 1 1 d . . . O1 O -0.1197(3) -0.2656(2) -0.13065(15) 0.0369(6) Uani 1 1 d . . . O1W O -0.7631(4) -0.4353(3) -0.38733(17) 0.0490(7) Uani 1 1 d D . . O2 O -0.3564(4) -0.3704(2) -0.12863(15) 0.0401(6) Uani 1 1 d . . . O3 O -0.5035(3) -0.4975(2) -0.27754(15) 0.0319(5) Uani 1 1 d . . . O4 O -0.3296(3) -0.6005(2) -0.20951(15) 0.0329(5) Uani 1 1 d . . . O5 O -0.3206(4) -1.3443(2) -0.37395(16) 0.0382(6) Uani 1 1 d . . . O6 O -0.3381(3) -1.2315(2) -0.27004(14) 0.0326(5) Uani 1 1 d . . . O7 O 0.0201(3) -0.3115(2) -0.28508(14) 0.0322(5) Uani 1 1 d . . . O8 O 0.0119(3) -0.4953(2) -0.17696(14) 0.0329(5) Uani 1 1 d . . . O9 O -0.1350(3) -0.5436(2) -0.33916(14) 0.0328(5) Uani 1 1 d . . . C1 C -0.2225(4) -0.1125(3) -0.00629(19) 0.0276(7) Uani 1 1 d . . . C2 C -0.3180(4) -0.2088(3) -0.03967(19) 0.0270(7) Uani 1 1 d . . . C3 C -0.4744(5) -0.2328(3) -0.0116(2) 0.0374(9) Uani 1 1 d . . . H3 H -0.5409 -0.2956 -0.0329 0.045 Uiso 1 1 calc R . . C4 C -0.5326(5) -0.1656(4) 0.0472(2) 0.0454(10) Uani 1 1 d . . . H4 H -0.6383 -0.1805 0.0656 0.054 Uiso 1 1 calc R . . C5 C -0.4283(5) -0.0753(4) 0.0776(2) 0.0423(9) Uani 1 1 d . . . H5 H -0.4652 -0.0303 0.1183 0.051 Uiso 1 1 calc R . . C6 C -0.2605(5) -0.2861(3) -0.10346(18) 0.0283(7) Uani 1 1 d . . . C7 C -0.5509(4) -0.8010(3) -0.25791(18) 0.0245(6) Uani 1 1 d . . . C8 C -0.5967(4) -0.6869(3) -0.25945(18) 0.0249(6) Uani 1 1 d . . . C9 C -0.7694(4) -0.6659(3) -0.2720(2) 0.0329(7) Uani 1 1 d . . . H9 H -0.8042 -0.5916 -0.2753 0.039 Uiso 1 1 calc R . . C10 C -0.8906(5) -0.7557(3) -0.2798(2) 0.0391(9) Uani 1 1 d . . . H10 H -1.0068 -0.7428 -0.2866 0.047 Uiso 1 1 calc R . . C11 C -0.8325(5) -0.8633(3) -0.2770(3) 0.0407(9) Uani 1 1 d . . . H11 H -0.9128 -0.9237 -0.2817 0.049 Uiso 1 1 calc R . . C12 C -0.4690(4) -0.5896(3) -0.24803(18) 0.0238(6) Uani 1 1 d . . . C13 C -0.3170(4) -1.1463(3) -0.38805(19) 0.0276(7) Uani 1 1 d . . . C14 C -0.3159(5) -1.0334(3) -0.35697(19) 0.0295(7) Uani 1 1 d . . . C15 C -0.2855(9) -0.9656(4) -0.4744(3) 0.0724(18) Uani 1 1 d . . . H15 H -0.2780 -0.9037 -0.5045 0.087 Uiso 1 1 calc R . . C16 C -0.2805(8) -1.0718(4) -0.5097(3) 0.0664(16) Uani 1 1 d . . . H16 H -0.2653 -1.0819 -0.5619 0.080 Uiso 1 1 calc R . . C17 C -0.2985(6) -1.1635(4) -0.4664(2) 0.0418(9) Uani 1 1 d . . . H17 H -0.2983 -1.2371 -0.4893 0.050 Uiso 1 1 calc R . . C18 C -0.3284(4) -1.2475(3) -0.3415(2) 0.0262(6) Uani 1 1 d . . . C19 C 0.2646(6) -0.2191(5) -0.1861(3) 0.0613(13) Uani 1 1 d . . . H19A H 0.2172 -0.2407 -0.1400 0.092 Uiso 1 1 calc R . . H19B H 0.3349 -0.1508 -0.1747 0.092 Uiso 1 1 calc R . . H19C H 0.3327 -0.2791 -0.2054 0.092 Uiso 1 1 calc R . . C20 C 0.2223(6) -0.1569(4) -0.3326(3) 0.0540(12) Uani 1 1 d . . . H20A H 0.1481 -0.1405 -0.3766 0.081 Uiso 1 1 calc R . . H20B H 0.2922 -0.2193 -0.3463 0.081 Uiso 1 1 calc R . . H20C H 0.2942 -0.0910 -0.3157 0.081 Uiso 1 1 calc R . . C21 C -0.0221(7) -0.6656(4) -0.0885(3) 0.0605(14) Uani 1 1 d . . . H21A H -0.1440 -0.6763 -0.0976 0.091 Uiso 1 1 calc R . . H21B H 0.0142 -0.6891 -0.0383 0.091 Uiso 1 1 calc R . . H21C H 0.0320 -0.7103 -0.1269 0.091 Uiso 1 1 calc R . . C22 C 0.2633(6) -0.5283(5) -0.0741(3) 0.0680(16) Uani 1 1 d . . . H22A H 0.3166 -0.4539 -0.0745 0.102 Uiso 1 1 calc R . . H22B H 0.3068 -0.5783 -0.1130 0.102 Uiso 1 1 calc R . . H22C H 0.2878 -0.5574 -0.0245 0.102 Uiso 1 1 calc R . . C23 C -0.0405(6) -0.6655(4) -0.4573(2) 0.0501(11) Uani 1 1 d . . . H23A H 0.0783 -0.6421 -0.4501 0.075 Uiso 1 1 calc R . . H23B H -0.0712 -0.6867 -0.5108 0.075 Uiso 1 1 calc R . . H23C H -0.0605 -0.7296 -0.4275 0.075 Uiso 1 1 calc R . . C24 C -0.3730(6) -0.6201(5) -0.4467(3) 0.0530(11) Uani 1 1 d . . . H24A H -0.4592 -0.5683 -0.4330 0.079 Uiso 1 1 calc R . . H24B H -0.3801 -0.6859 -0.4174 0.079 Uiso 1 1 calc R . . H24C H -0.3906 -0.6430 -0.5007 0.079 Uiso 1 1 calc R . . N1 N -0.2768(4) -0.0477(3) 0.05251(18) 0.0365(7) Uani 1 1 d . . . N2 N -0.6660(4) -0.8874(3) -0.2678(2) 0.0357(7) Uani 1 1 d . . . N3 N -0.3007(6) -0.9447(3) -0.39882(19) 0.0515(10) Uani 1 1 d . . . H1WB H -0.676(4) -0.456(4) -0.357(2) 0.058(15) Uiso 1 1 d D . . H1WA H -0.813(10) -0.418(7) -0.345(3) 0.13(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02172(8) 0.01399(7) 0.02437(8) -0.00082(5) 0.00063(5) -0.00047(5) S1 0.0350(5) 0.0325(5) 0.0389(5) -0.0145(4) 0.0145(4) -0.0110(4) S2 0.0235(4) 0.0206(4) 0.0391(4) -0.0031(3) 0.0041(3) 0.0008(3) S3 0.0371(4) 0.0190(4) 0.0294(4) 0.0014(3) 0.0070(3) 0.0054(3) S4 0.0321(4) 0.0247(4) 0.0434(5) -0.0044(4) 0.0059(4) -0.0059(3) S5 0.0544(6) 0.0383(5) 0.0305(4) 0.0048(4) -0.0064(4) 0.0060(4) S6 0.0391(5) 0.0275(4) 0.0289(4) -0.0030(3) 0.0031(4) 0.0040(3) O1 0.0338(14) 0.0376(15) 0.0378(14) -0.0119(11) 0.0091(11) -0.0042(11) O1W 0.0457(17) 0.064(2) 0.0377(15) 0.0045(14) 0.0004(14) 0.0120(15) O2 0.0522(17) 0.0308(14) 0.0361(14) -0.0109(11) 0.0133(12) -0.0158(12) O3 0.0295(12) 0.0201(12) 0.0453(14) 0.0054(10) -0.0031(11) -0.0029(9) O4 0.0306(13) 0.0198(12) 0.0469(14) 0.0037(10) -0.0053(11) -0.0038(9) O5 0.0503(16) 0.0187(12) 0.0444(15) -0.0020(11) -0.0022(12) 0.0053(11) O6 0.0423(14) 0.0205(12) 0.0370(13) 0.0049(10) 0.0088(11) 0.0086(10) O7 0.0313(13) 0.0264(13) 0.0381(13) -0.0042(10) 0.0075(11) -0.0084(10) O8 0.0343(13) 0.0350(14) 0.0292(12) 0.0054(10) -0.0033(10) 0.0051(10) O9 0.0396(14) 0.0277(13) 0.0298(12) -0.0058(10) -0.0010(11) 0.0076(10) C1 0.0306(17) 0.0257(17) 0.0258(15) -0.0026(13) 0.0033(13) -0.0028(13) C2 0.0319(17) 0.0236(17) 0.0249(15) -0.0006(12) 0.0023(13) -0.0020(13) C3 0.039(2) 0.038(2) 0.0326(18) -0.0081(15) 0.0072(16) -0.0145(16) C4 0.037(2) 0.052(3) 0.047(2) -0.0080(19) 0.0189(18) -0.0117(18) C5 0.046(2) 0.045(2) 0.036(2) -0.0117(17) 0.0183(17) -0.0059(18) C6 0.0396(19) 0.0223(17) 0.0220(15) -0.0022(12) 0.0007(14) -0.0009(13) C7 0.0225(15) 0.0219(16) 0.0293(16) 0.0004(12) 0.0051(13) -0.0010(12) C8 0.0258(16) 0.0209(16) 0.0281(15) -0.0008(12) 0.0058(13) -0.0024(12) C9 0.0258(17) 0.0266(18) 0.047(2) 0.0055(15) 0.0054(15) 0.0035(13) C10 0.0226(17) 0.038(2) 0.058(2) 0.0081(18) 0.0046(16) -0.0028(14) C11 0.0274(18) 0.032(2) 0.062(3) 0.0049(18) 0.0026(17) -0.0101(14) C12 0.0246(15) 0.0189(15) 0.0276(15) -0.0038(12) 0.0054(13) -0.0005(12) C13 0.0318(17) 0.0214(16) 0.0301(16) 0.0019(13) 0.0051(14) 0.0036(12) C14 0.0382(19) 0.0207(16) 0.0307(17) 0.0028(13) 0.0076(14) 0.0027(13) C15 0.139(6) 0.040(3) 0.042(2) 0.013(2) 0.027(3) -0.005(3) C16 0.120(5) 0.049(3) 0.033(2) 0.003(2) 0.026(3) -0.002(3) C17 0.059(3) 0.033(2) 0.0329(19) -0.0059(15) 0.0098(18) 0.0021(17) C18 0.0218(15) 0.0213(16) 0.0356(17) 0.0029(13) 0.0019(13) 0.0034(11) C19 0.047(3) 0.076(4) 0.055(3) -0.004(3) -0.014(2) -0.013(2) C20 0.063(3) 0.041(2) 0.059(3) 0.001(2) 0.022(2) -0.022(2) C21 0.067(3) 0.055(3) 0.057(3) 0.024(2) -0.016(2) -0.022(2) C22 0.054(3) 0.077(4) 0.069(3) 0.025(3) -0.030(3) -0.016(3) C23 0.061(3) 0.050(3) 0.038(2) -0.0141(19) 0.003(2) 0.021(2) C24 0.046(2) 0.071(3) 0.039(2) -0.011(2) 0.0008(19) -0.006(2) N1 0.0404(18) 0.0341(17) 0.0337(16) -0.0117(13) 0.0110(14) -0.0066(13) N2 0.0286(15) 0.0234(15) 0.0542(19) 0.0008(13) 0.0022(14) -0.0055(11) N3 0.096(3) 0.0265(18) 0.0342(17) 0.0054(14) 0.0170(19) -0.0028(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O9 2.340(2) . ? Dy1 O8 2.353(3) . ? Dy1 O7 2.370(2) . ? Dy1 O2 2.396(3) . ? Dy1 O6 2.409(2) 1_565 ? Dy1 O3 2.432(2) . ? Dy1 O4 2.488(2) . ? Dy1 O5 2.529(3) 1_565 ? Dy1 O1 2.591(3) . ? Dy1 C18 2.775(3) 1_565 ? Dy1 C12 2.816(3) . ? Dy1 C6 2.832(3) . ? S1 C1 1.770(3) . ? S1 S1 2.1094(18) 2 ? S2 C7 1.795(3) . ? S2 S3 2.0320(12) . ? S3 C14 1.793(3) . ? S4 O7 1.525(2) . ? S4 C19 1.771(5) . ? S4 C20 1.787(4) . ? S5 O8 1.502(3) . ? S5 C21 1.774(5) . ? S5 C22 1.796(5) . ? S6 O9 1.519(3) . ? S6 C23 1.779(4) . ? S6 C24 1.786(5) . ? O1 C6 1.261(4) . ? O1W H1WB 0.880(10) . ? O1W H1WA 0.886(10) . ? O2 C6 1.259(4) . ? O3 C12 1.259(4) . ? O4 C12 1.252(4) . ? O5 C18 1.244(4) . ? O5 Dy1 2.529(3) 1_545 ? O6 C18 1.258(4) . ? O6 Dy1 2.409(2) 1_545 ? C1 N1 1.344(4) . ? C1 C2 1.405(5) . ? C2 C3 1.387(5) . ? C2 C6 1.499(4) . ? C3 C4 1.371(5) . ? C3 H3 0.9300 . ? C4 C5 1.371(6) . ? C4 H4 0.9300 . ? C5 N1 1.339(5) . ? C5 H5 0.9300 . ? C7 N2 1.332(4) . ? C7 C8 1.404(5) . ? C8 C9 1.389(5) . ? C8 C12 1.491(4) . ? C9 C10 1.392(5) . ? C9 H9 0.9300 . ? C10 C11 1.363(6) . ? C10 H10 0.9300 . ? C11 N2 1.346(5) . ? C11 H11 0.9300 . ? C13 C17 1.389(5) . ? C13 C14 1.401(5) . ? C13 C18 1.491(4) . ? C14 N3 1.323(4) . ? C15 N3 1.341(6) . ? C15 C16 1.361(7) . ? C15 H15 0.9300 . ? C16 C17 1.369(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 Dy1 2.775(3) 1_545 ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 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 O9 Dy1 O8 78.81(9) . . ? O9 Dy1 O7 79.62(9) . . ? O8 Dy1 O7 77.87(9) . . ? O9 Dy1 O2 150.32(9) . . ? O8 Dy1 O2 92.40(10) . . ? O7 Dy1 O2 126.57(9) . . ? O9 Dy1 O6 124.22(9) . 1_565 ? O8 Dy1 O6 142.68(9) . 1_565 ? O7 Dy1 O6 78.44(9) . 1_565 ? O2 Dy1 O6 79.19(9) . 1_565 ? O9 Dy1 O3 84.80(9) . . ? O8 Dy1 O3 126.67(9) . . ? O7 Dy1 O3 147.59(9) . . ? O2 Dy1 O3 77.86(9) . . ? O6 Dy1 O3 87.36(9) 1_565 . ? O9 Dy1 O4 74.78(9) . . ? O8 Dy1 O4 73.94(9) . . ? O7 Dy1 O4 144.89(9) . . ? O2 Dy1 O4 75.56(9) . . ? O6 Dy1 O4 136.21(8) 1_565 . ? O3 Dy1 O4 52.78(8) . . ? O9 Dy1 O5 72.30(9) . 1_565 ? O8 Dy1 O5 143.15(9) . 1_565 ? O7 Dy1 O5 74.87(9) . 1_565 ? O2 Dy1 O5 123.81(10) . 1_565 ? O6 Dy1 O5 52.63(8) 1_565 1_565 ? O3 Dy1 O5 73.36(9) . 1_565 ? O4 Dy1 O5 118.22(9) . 1_565 ? O9 Dy1 O1 146.36(9) . . ? O8 Dy1 O1 74.87(9) . . ? O7 Dy1 O1 74.71(8) . . ? O2 Dy1 O1 52.22(8) . . ? O6 Dy1 O1 71.31(9) 1_565 . ? O3 Dy1 O1 127.94(9) . . ? O4 Dy1 O1 116.47(9) . . ? O5 Dy1 O1 119.99(9) 1_565 . ? O9 Dy1 C18 97.30(9) . 1_565 ? O8 Dy1 C18 147.78(9) . 1_565 ? O7 Dy1 C18 70.00(9) . 1_565 ? O2 Dy1 C18 104.59(10) . 1_565 ? O6 Dy1 C18 26.92(9) 1_565 1_565 ? O3 Dy1 C18 84.16(9) . 1_565 ? O4 Dy1 C18 136.41(9) . 1_565 ? O5 Dy1 C18 26.62(9) 1_565 1_565 ? O1 Dy1 C18 94.00(10) . 1_565 ? O9 Dy1 C12 76.86(9) . . ? O8 Dy1 C12 100.17(10) . . ? O7 Dy1 C12 156.30(9) . . ? O2 Dy1 C12 76.92(9) . . ? O6 Dy1 C12 112.85(9) 1_565 . ? O3 Dy1 C12 26.50(9) . . ? O4 Dy1 C12 26.39(9) . . ? O5 Dy1 C12 95.10(10) 1_565 . ? O1 Dy1 C12 128.03(9) . . ? C18 Dy1 C12 110.14(10) 1_565 . ? O9 Dy1 C6 164.63(10) . . ? O8 Dy1 C6 86.14(10) . . ? O7 Dy1 C6 100.37(9) . . ? O2 Dy1 C6 26.20(9) . . ? O6 Dy1 C6 70.31(9) 1_565 . ? O3 Dy1 C6 101.99(10) . . ? O4 Dy1 C6 98.20(9) . . ? O5 Dy1 C6 122.73(9) 1_565 . ? O1 Dy1 C6 26.41(9) . . ? C18 Dy1 C6 97.10(10) 1_565 . ? C12 Dy1 C6 103.06(10) . . ? C1 S1 S1 95.73(12) . 2 ? C7 S2 S3 103.50(11) . . ? C14 S3 S2 103.01(12) . . ? O7 S4 C19 105.7(2) . . ? O7 S4 C20 103.07(18) . . ? C19 S4 C20 98.9(2) . . ? O8 S5 C21 106.6(2) . . ? O8 S5 C22 104.5(2) . . ? C21 S5 C22 98.5(3) . . ? O9 S6 C23 104.11(18) . . ? O9 S6 C24 105.15(18) . . ? C23 S6 C24 98.5(2) . . ? C6 O1 Dy1 87.5(2) . . ? H1WB O1W H1WA 87(6) . . ? C6 O2 Dy1 96.6(2) . . ? C12 O3 Dy1 94.0(2) . . ? C12 O4 Dy1 91.55(19) . . ? C18 O5 Dy1 87.8(2) . 1_545 ? C18 O6 Dy1 92.97(19) . 1_545 ? S4 O7 Dy1 129.27(14) . . ? S5 O8 Dy1 129.36(15) . . ? S6 O9 Dy1 131.80(15) . . ? N1 C1 C2 121.7(3) . . ? N1 C1 S1 117.0(3) . . ? C2 C1 S1 121.4(2) . . ? C3 C2 C1 117.6(3) . . ? C3 C2 C6 118.7(3) . . ? C1 C2 C6 123.8(3) . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 117.1(3) . . ? C3 C4 H4 121.5 . . ? C5 C4 H4 121.5 . . ? N1 C5 C4 124.4(3) . . ? N1 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? O2 C6 O1 121.8(3) . . ? O2 C6 C2 118.2(3) . . ? O1 C6 C2 120.0(3) . . ? O2 C6 Dy1 57.17(17) . . ? O1 C6 Dy1 66.06(17) . . ? C2 C6 Dy1 166.5(2) . . ? N2 C7 C8 122.5(3) . . ? N2 C7 S2 118.5(3) . . ? C8 C7 S2 119.0(2) . . ? C9 C8 C7 117.4(3) . . ? C9 C8 C12 119.6(3) . . ? C7 C8 C12 122.9(3) . . ? C8 C9 C10 120.3(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 117.6(3) . . ? C11 C10 H10 121.2 . . ? C9 C10 H10 121.2 . . ? N2 C11 C10 124.0(3) . . ? N2 C11 H11 118.0 . . ? C10 C11 H11 118.0 . . ? O4 C12 O3 121.1(3) . . ? O4 C12 C8 119.7(3) . . ? O3 C12 C8 119.2(3) . . ? O4 C12 Dy1 62.06(16) . . ? O3 C12 Dy1 59.48(16) . . ? C8 C12 Dy1 173.3(2) . . ? C17 C13 C14 117.3(3) . . ? C17 C13 C18 118.7(3) . . ? C14 C13 C18 123.9(3) . . ? N3 C14 C13 123.1(3) . . ? N3 C14 S3 117.3(3) . . ? C13 C14 S3 119.6(2) . . ? N3 C15 C16 124.0(4) . . ? N3 C15 H15 118.0 . . ? C16 C15 H15 118.0 . . ? C15 C16 C17 118.4(4) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C16 C17 C13 119.8(4) . . ? C16 C17 H17 120.1 . . ? C13 C17 H17 120.1 . . ? O5 C18 O6 122.3(3) . . ? O5 C18 C13 119.0(3) . . ? O6 C18 C13 118.6(3) . . ? O5 C18 Dy1 65.62(19) . 1_545 ? O6 C18 Dy1 60.11(17) . 1_545 ? C13 C18 Dy1 158.1(2) . 1_545 ? S4 C19 H19A 109.5 . . ? S4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? S4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? S4 C20 H20A 109.5 . . ? S4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? S4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? S5 C21 H21A 109.5 . . ? S5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S5 C22 H22A 109.5 . . ? S5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S6 C23 H23A 109.5 . . ? S6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? S6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S6 C24 H24A 109.5 . . ? S6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C5 N1 C1 118.1(3) . . ? C7 N2 C11 118.2(3) . . ? C14 N3 C15 117.5(4) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.666 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.116 # Attachment 'Eu.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 642852' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H29 Eu N3 O10 S6' _chemical_formula_weight 863.82 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8341(3) _cell_length_b 11.8843(5) _cell_length_c 17.5342(8) _cell_angle_alpha 94.0870(10) _cell_angle_beta 94.6990(10) _cell_angle_gamma 91.9950(10) _cell_volume 1621.50(12) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 866 _exptl_absorpt_coefficient_mu 2.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5358 _exptl_absorpt_correction_T_max 0.8904 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10161 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0887 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7454 _reflns_number_gt 5512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0282P)^2^+4.1540P] 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 7454 _refine_ls_number_parameters 405 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Eu1 Eu 0.22011(4) 0.41156(3) 0.243838(19) 0.02468(10) Uani 1 1 d . . . O1 O 0.3589(6) 0.3689(4) 0.1271(3) 0.0438(12) Uani 1 1 d . . . O1W O 0.7661(8) 0.4350(5) 0.3863(3) 0.0540(14) Uani 1 1 d D . . O2 O 0.1251(6) 0.2658(4) 0.1294(3) 0.0388(11) Uani 1 1 d . . . O3 O 0.3225(6) 1.3427(4) 0.3739(3) 0.0413(12) Uani 1 1 d . . . O4 O 0.3407(6) 1.2286(3) 0.2701(3) 0.0344(10) Uani 1 1 d . . . O5 O 0.5067(5) 0.4993(3) 0.2776(3) 0.0345(11) Uani 1 1 d . . . O6 O 0.3348(5) 0.6009(3) 0.2087(3) 0.0371(11) Uani 1 1 d . . . O7 O 0.1386(6) 0.5431(4) 0.3400(2) 0.0366(11) Uani 1 1 d . . . O8 O -0.0190(5) 0.3083(3) 0.2847(3) 0.0349(11) Uani 1 1 d . . . O9 O -0.0138(5) 0.4957(4) 0.1762(3) 0.0353(11) Uani 1 1 d . . . S1 S 0.0257(2) 0.07122(15) 0.03959(11) 0.0396(4) Uani 1 1 d . . . S2 S 0.3300(2) 0.83212(13) 0.24380(10) 0.0313(4) Uani 1 1 d . . . S3 S 0.3306(2) 1.00434(13) 0.25599(10) 0.0315(4) Uani 1 1 d . . . S4 S 0.1686(2) 0.55172(14) 0.42772(10) 0.0363(4) Uani 1 1 d . . . S5 S -0.0397(3) 0.52072(16) 0.09296(11) 0.0443(5) Uani 1 1 d . . . S6 S -0.0989(2) 0.19285(14) 0.25612(11) 0.0384(4) Uani 1 1 d . . . N1 N 0.2772(7) 0.0455(5) -0.0532(3) 0.0375(14) Uani 1 1 d . . . N2 N 0.6641(7) 0.8879(4) 0.2685(3) 0.0364(13) Uani 1 1 d . . . N3 N 0.3021(9) 0.9442(5) 0.3986(4) 0.0521(17) Uani 1 1 d . . . C1 C 0.2242(8) 0.1106(5) 0.0048(3) 0.0293(14) Uani 1 1 d . . . C2 C 0.3219(8) 0.2071(5) 0.0393(4) 0.0305(14) Uani 1 1 d . . . C3 C 0.4737(9) 0.2310(6) 0.0105(4) 0.0405(17) Uani 1 1 d . . . H3 H 0.5387 0.2950 0.0302 0.049 Uiso 1 1 calc R . . C4 C 0.5344(10) 0.1612(6) -0.0483(4) 0.048(2) Uani 1 1 d . . . H4 H 0.6413 0.1743 -0.0661 0.058 Uiso 1 1 calc R . . C5 C 0.4272(9) 0.0724(6) -0.0780(4) 0.0439(18) Uani 1 1 d . . . H5 H 0.4628 0.0275 -0.1189 0.053 Uiso 1 1 calc R . . C6 C 0.2613(8) 0.2856(5) 0.1025(4) 0.0305(14) Uani 1 1 d . . . C7 C 0.3177(8) 1.0328(5) 0.3561(4) 0.0330(15) Uani 1 1 d . . . C8 C 0.3186(8) 1.1447(5) 0.3879(4) 0.0303(14) Uani 1 1 d . . . C9 C 0.2976(10) 1.1627(6) 0.4661(4) 0.0477(19) Uani 1 1 d . . . H9 H 0.2979 1.2361 0.4885 0.057 Uiso 1 1 calc R . . C10 C 0.2763(13) 1.0727(7) 0.5101(5) 0.067(3) Uani 1 1 d . . . H10 H 0.2584 1.0830 0.5619 0.080 Uiso 1 1 calc R . . C11 C 0.2829(15) 0.9661(8) 0.4735(5) 0.088(4) Uani 1 1 d . . . H11 H 0.2733 0.9048 0.5032 0.105 Uiso 1 1 calc R . . C12 C 0.3330(8) 1.2449(5) 0.3411(4) 0.0315(15) Uani 1 1 d . . . C13 C 0.5506(7) 0.8013(5) 0.2587(3) 0.0253(13) Uani 1 1 d . . . C14 C 0.5971(7) 0.6896(5) 0.2616(3) 0.0256(13) Uani 1 1 d . . . C15 C 0.7738(8) 0.6683(5) 0.2732(4) 0.0341(15) Uani 1 1 d . . . H15 H 0.8101 0.5948 0.2749 0.041 Uiso 1 1 calc R . . C16 C 0.8906(8) 0.7580(6) 0.2820(4) 0.0413(18) Uani 1 1 d . . . H16 H 1.0069 0.7463 0.2915 0.050 Uiso 1 1 calc R . . C17 C 0.8339(9) 0.8636(6) 0.2766(5) 0.0452(19) Uani 1 1 d . . . H17 H 0.9149 0.9231 0.2785 0.054 Uiso 1 1 calc R . . C18 C 0.4714(8) 0.5908(5) 0.2480(4) 0.0276(14) Uani 1 1 d . . . C19 C 0.0408(10) 0.6659(6) 0.4588(4) 0.050(2) Uani 1 1 d . . . H19A H -0.0783 0.6424 0.4515 0.075 Uiso 1 1 calc R . . H19B H 0.0608 0.7293 0.4292 0.075 Uiso 1 1 calc R . . H19C H 0.0714 0.6872 0.5121 0.075 Uiso 1 1 calc R . . C20 C 0.3707(9) 0.6212(7) 0.4480(4) 0.057(2) Uani 1 1 d . . . H20A H 0.4584 0.5709 0.4344 0.085 Uiso 1 1 calc R . . H20B H 0.3874 0.6443 0.5018 0.085 Uiso 1 1 calc R . . H20C H 0.3765 0.6865 0.4189 0.085 Uiso 1 1 calc R . . C21 C -0.2689(11) 0.5317(8) 0.0746(6) 0.083(3) Uani 1 1 d . . . H21A H -0.3242 0.4584 0.0750 0.124 Uiso 1 1 calc R . . H21B H -0.2938 0.5607 0.0253 0.124 Uiso 1 1 calc R . . H21C H -0.3105 0.5818 0.1137 0.124 Uiso 1 1 calc R . . C22 C 0.0193(11) 0.6655(7) 0.0886(5) 0.062(2) Uani 1 1 d . . . H22A H 0.1417 0.6759 0.0971 0.092 Uiso 1 1 calc R . . H22B H -0.0336 0.7097 0.1274 0.092 Uiso 1 1 calc R . . H22C H -0.0181 0.6892 0.0390 0.092 Uiso 1 1 calc R . . C23 C -0.2307(10) 0.1582(6) 0.3318(5) 0.056(2) Uani 1 1 d . . . H23A H -0.1587 0.1411 0.3761 0.083 Uiso 1 1 calc R . . H23B H -0.3048 0.0937 0.3145 0.083 Uiso 1 1 calc R . . H23C H -0.2987 0.2212 0.3449 0.083 Uiso 1 1 calc R . . C24 C -0.2689(11) 0.2190(8) 0.1861(5) 0.073(3) Uani 1 1 d . . . H24A H -0.2216 0.2393 0.1399 0.110 Uiso 1 1 calc R . . H24B H -0.3348 0.2795 0.2056 0.110 Uiso 1 1 calc R . . H24C H -0.3415 0.1520 0.1752 0.110 Uiso 1 1 calc R . . H1WA H 0.791(13) 0.398(7) 0.343(3) 0.10(4) Uiso 1 1 d D . . H1WB H 0.659(9) 0.457(17) 0.386(13) 0.35(12) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02570(16) 0.01913(15) 0.02862(17) -0.00045(12) 0.00137(12) -0.00077(11) O1 0.059(3) 0.029(2) 0.042(3) -0.012(2) 0.018(2) -0.016(2) O1W 0.053(3) 0.067(4) 0.042(3) -0.001(3) 0.002(3) 0.009(3) O2 0.034(3) 0.042(3) 0.039(3) -0.009(2) 0.011(2) -0.009(2) O3 0.055(3) 0.024(2) 0.042(3) -0.003(2) -0.007(2) 0.005(2) O4 0.041(3) 0.029(2) 0.035(3) 0.002(2) 0.011(2) 0.009(2) O5 0.029(2) 0.022(2) 0.052(3) 0.006(2) 0.000(2) -0.0029(18) O6 0.030(2) 0.026(2) 0.053(3) 0.005(2) -0.008(2) -0.0035(19) O7 0.043(3) 0.035(2) 0.030(3) -0.009(2) 0.003(2) 0.008(2) O8 0.034(2) 0.030(2) 0.039(3) -0.005(2) 0.004(2) -0.015(2) O9 0.031(2) 0.037(3) 0.037(3) 0.007(2) -0.002(2) 0.005(2) S1 0.0364(10) 0.0371(9) 0.0437(11) -0.0150(8) 0.0141(8) -0.0114(8) S2 0.0276(8) 0.0236(8) 0.0423(10) -0.0026(7) 0.0054(7) 0.0001(6) S3 0.0380(9) 0.0241(8) 0.0334(9) 0.0011(7) 0.0078(7) 0.0053(7) S4 0.0433(10) 0.0331(9) 0.0322(9) -0.0020(7) 0.0042(8) 0.0034(8) S5 0.0555(12) 0.0428(10) 0.0337(10) 0.0041(8) -0.0039(9) 0.0059(9) S6 0.0352(10) 0.0286(9) 0.0504(11) -0.0043(8) 0.0078(8) -0.0059(7) N1 0.033(3) 0.037(3) 0.041(3) -0.009(3) 0.016(3) -0.005(3) N2 0.031(3) 0.025(3) 0.051(4) -0.004(3) 0.004(3) -0.003(2) N3 0.089(5) 0.029(3) 0.041(4) 0.009(3) 0.016(4) -0.002(3) C1 0.037(4) 0.028(3) 0.023(3) 0.001(3) 0.003(3) -0.001(3) C2 0.041(4) 0.025(3) 0.025(3) 0.002(3) 0.004(3) -0.003(3) C3 0.036(4) 0.039(4) 0.046(4) -0.008(3) 0.013(3) -0.013(3) C4 0.049(5) 0.049(5) 0.047(5) 0.000(4) 0.013(4) -0.016(4) C5 0.054(5) 0.042(4) 0.034(4) -0.007(3) 0.011(4) -0.012(4) C6 0.042(4) 0.024(3) 0.026(3) 0.001(3) 0.009(3) -0.006(3) C7 0.035(4) 0.029(3) 0.037(4) 0.004(3) 0.010(3) 0.005(3) C8 0.030(3) 0.026(3) 0.035(4) 0.000(3) 0.005(3) 0.002(3) C9 0.071(5) 0.039(4) 0.031(4) -0.007(3) 0.009(4) -0.005(4) C10 0.118(8) 0.049(5) 0.036(5) 0.002(4) 0.029(5) -0.011(5) C11 0.174(11) 0.046(5) 0.043(5) 0.016(5) 0.011(6) -0.019(6) C12 0.023(3) 0.027(3) 0.046(4) 0.005(3) 0.003(3) 0.007(3) C13 0.027(3) 0.021(3) 0.028(3) -0.003(3) 0.005(3) -0.002(2) C14 0.027(3) 0.020(3) 0.030(3) -0.001(3) 0.004(3) -0.002(2) C15 0.025(3) 0.030(3) 0.048(4) 0.001(3) 0.008(3) 0.004(3) C16 0.018(3) 0.041(4) 0.066(5) 0.010(4) 0.007(3) 0.003(3) C17 0.029(4) 0.042(4) 0.064(5) 0.006(4) 0.000(4) -0.011(3) C18 0.021(3) 0.024(3) 0.038(4) -0.008(3) 0.012(3) -0.003(2) C19 0.060(5) 0.047(4) 0.043(5) -0.010(4) 0.011(4) 0.018(4) C20 0.040(4) 0.083(6) 0.044(5) -0.017(4) 0.006(4) -0.004(4) C21 0.078(7) 0.079(7) 0.084(7) 0.044(6) -0.049(6) -0.031(5) C22 0.059(5) 0.061(5) 0.064(6) 0.016(5) -0.002(4) -0.014(4) C23 0.055(5) 0.043(4) 0.073(6) 0.013(4) 0.033(4) -0.016(4) C24 0.064(6) 0.091(7) 0.056(6) 0.002(5) -0.031(5) -0.026(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 Eu1 O7 2.359(4) . ? Eu1 O9 2.388(4) . ? Eu1 O8 2.391(4) . ? Eu1 O1 2.426(5) . ? Eu1 O5 2.452(4) . ? Eu1 O4 2.459(4) 1_545 ? Eu1 O6 2.529(4) . ? Eu1 O3 2.555(5) 1_545 ? Eu1 O2 2.598(4) . ? Eu1 C12 2.824(6) 1_545 ? Eu1 C18 2.842(6) . ? Eu1 C6 2.851(6) . ? O1 C6 1.259(7) . ? O1W H1WA 0.889(10) . ? O1W H1WB 0.892(10) . ? O2 C6 1.224(7) . ? O3 C12 1.268(7) . ? O3 Eu1 2.555(5) 1_565 ? O4 C12 1.254(8) . ? O4 Eu1 2.459(4) 1_565 ? O5 C18 1.267(7) . ? O6 C18 1.239(7) . ? O7 S4 1.533(5) . ? O8 S6 1.521(4) . ? O9 S5 1.510(5) . ? S1 C1 1.776(6) . ? S1 S1 2.117(3) 2 ? S2 C13 1.781(6) . ? S2 S3 2.042(2) . ? S3 C7 1.775(7) . ? S4 C20 1.757(7) . ? S4 C19 1.795(7) . ? S5 C22 1.775(8) . ? S5 C21 1.809(9) . ? S6 C24 1.786(8) . ? S6 C23 1.808(7) . ? N1 C5 1.323(8) . ? N1 C1 1.337(8) . ? N2 C13 1.329(7) . ? N2 C17 1.369(8) . ? N3 C7 1.341(8) . ? N3 C11 1.343(10) . ? C1 C2 1.424(8) . ? C2 C3 1.358(8) . ? C2 C6 1.515(9) . ? C3 C4 1.400(10) . ? C3 H3 0.9300 . ? C4 C5 1.370(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.404(8) . ? C8 C9 1.396(9) . ? C8 C12 1.500(9) . ? C9 C10 1.377(10) . ? C9 H9 0.9300 . ? C10 C11 1.382(12) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 Eu1 2.824(6) 1_565 ? C13 C14 1.392(8) . ? C14 C15 1.417(8) . ? C14 C18 1.499(8) . ? C15 C16 1.371(8) . ? C15 H15 0.9300 . ? C16 C17 1.353(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 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 O7 Eu1 O9 79.17(15) . . ? O7 Eu1 O8 80.58(15) . . ? O9 Eu1 O8 78.74(15) . . ? O7 Eu1 O1 150.43(15) . . ? O9 Eu1 O1 92.38(16) . . ? O8 Eu1 O1 125.87(14) . . ? O7 Eu1 O5 83.80(15) . . ? O9 Eu1 O5 125.88(14) . . ? O8 Eu1 O5 147.49(15) . . ? O1 Eu1 O5 78.36(15) . . ? O7 Eu1 O4 123.75(15) . 1_545 ? O9 Eu1 O4 142.80(15) . 1_545 ? O8 Eu1 O4 77.29(15) . 1_545 ? O1 Eu1 O4 79.34(15) . 1_545 ? O5 Eu1 O4 88.21(14) . 1_545 ? O7 Eu1 O6 74.97(15) . . ? O9 Eu1 O6 73.90(14) . . ? O8 Eu1 O6 146.08(15) . . ? O1 Eu1 O6 75.45(15) . . ? O5 Eu1 O6 52.08(14) . . ? O4 Eu1 O6 136.20(14) 1_545 . ? O7 Eu1 O3 72.18(15) . 1_545 ? O9 Eu1 O3 143.17(16) . 1_545 ? O8 Eu1 O3 74.22(15) . 1_545 ? O1 Eu1 O3 123.74(16) . 1_545 ? O5 Eu1 O3 73.90(15) . 1_545 ? O4 Eu1 O3 52.23(14) 1_545 1_545 ? O6 Eu1 O3 118.62(14) . 1_545 ? O7 Eu1 O2 147.76(15) . . ? O9 Eu1 O2 75.53(15) . . ? O8 Eu1 O2 75.18(14) . . ? O1 Eu1 O2 51.12(14) . . ? O5 Eu1 O2 127.47(14) . . ? O4 Eu1 O2 71.09(15) 1_545 . ? O6 Eu1 O2 115.81(15) . . ? O3 Eu1 O2 119.73(14) 1_545 . ? O7 Eu1 C12 97.43(18) . 1_545 ? O9 Eu1 C12 148.14(16) . 1_545 ? O8 Eu1 C12 69.49(16) . 1_545 ? O1 Eu1 C12 104.08(18) . 1_545 ? O5 Eu1 C12 84.60(16) . 1_545 ? O4 Eu1 C12 26.32(16) 1_545 1_545 ? O6 Eu1 C12 136.31(16) . 1_545 ? O3 Eu1 C12 26.67(16) 1_545 1_545 ? O2 Eu1 C12 93.68(17) . 1_545 ? O7 Eu1 C18 76.17(16) . . ? O9 Eu1 C18 99.49(17) . . ? O8 Eu1 C18 156.57(16) . . ? O1 Eu1 C18 77.40(16) . . ? O5 Eu1 C18 26.39(15) . . ? O4 Eu1 C18 113.59(16) 1_545 . ? O6 Eu1 C18 25.83(15) . . ? O3 Eu1 C18 95.68(17) 1_545 . ? O2 Eu1 C18 127.40(16) . . ? C12 Eu1 C18 110.52(19) 1_545 . ? O7 Eu1 C6 164.99(17) . . ? O9 Eu1 C6 86.17(17) . . ? O8 Eu1 C6 99.84(16) . . ? O1 Eu1 C6 26.04(15) . . ? O5 Eu1 C6 102.48(17) . . ? O4 Eu1 C6 70.52(16) 1_545 . ? O6 Eu1 C6 97.95(16) . . ? O3 Eu1 C6 122.54(16) 1_545 . ? O2 Eu1 C6 25.43(14) . . ? C12 Eu1 C6 96.73(19) 1_545 . ? C18 Eu1 C6 103.36(17) . . ? C6 O1 Eu1 96.2(4) . . ? H1WA O1W H1WB 115(10) . . ? C6 O2 Eu1 88.9(4) . . ? C12 O3 Eu1 88.6(4) . 1_565 ? C12 O4 Eu1 93.3(4) . 1_565 ? C18 O5 Eu1 94.3(3) . . ? C18 O6 Eu1 91.3(4) . . ? S4 O7 Eu1 132.8(3) . . ? S6 O8 Eu1 130.6(3) . . ? S5 O9 Eu1 130.0(3) . . ? C1 S1 S1 95.3(2) . 2 ? C13 S2 S3 103.9(2) . . ? C7 S3 S2 103.0(2) . . ? O7 S4 C20 104.9(3) . . ? O7 S4 C19 104.7(3) . . ? C20 S4 C19 97.7(4) . . ? O9 S5 C22 106.7(3) . . ? O9 S5 C21 104.7(4) . . ? C22 S5 C21 97.8(4) . . ? O8 S6 C24 105.8(3) . . ? O8 S6 C23 103.2(3) . . ? C24 S6 C23 97.4(4) . . ? C5 N1 C1 117.7(6) . . ? C13 N2 C17 117.3(5) . . ? C7 N3 C11 117.3(6) . . ? N1 C1 C2 122.4(6) . . ? N1 C1 S1 117.3(5) . . ? C2 C1 S1 120.3(5) . . ? C3 C2 C1 117.0(6) . . ? C3 C2 C6 119.4(6) . . ? C1 C2 C6 123.5(6) . . ? C2 C3 C4 121.4(6) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 116.2(7) . . ? C5 C4 H4 121.9 . . ? C3 C4 H4 121.9 . . ? N1 C5 C4 125.2(7) . . ? N1 C5 H5 117.4 . . ? C4 C5 H5 117.4 . . ? O2 C6 O1 122.2(6) . . ? O2 C6 C2 120.6(5) . . ? O1 C6 C2 117.2(6) . . ? O2 C6 Eu1 65.7(3) . . ? O1 C6 Eu1 57.8(3) . . ? C2 C6 Eu1 165.2(5) . . ? N3 C7 C8 122.2(6) . . ? N3 C7 S3 117.5(5) . . ? C8 C7 S3 120.3(5) . . ? C9 C8 C7 118.2(6) . . ? C9 C8 C12 118.8(6) . . ? C7 C8 C12 123.0(6) . . ? C10 C9 C8 120.4(7) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 116.7(8) . . ? C9 C10 H10 121.7 . . ? C11 C10 H10 121.7 . . ? N3 C11 C10 125.2(8) . . ? N3 C11 H11 117.4 . . ? C10 C11 H11 117.4 . . ? O4 C12 O3 122.3(6) . . ? O4 C12 C8 118.8(6) . . ? O3 C12 C8 118.6(6) . . ? O4 C12 Eu1 60.4(3) . 1_565 ? O3 C12 Eu1 64.7(3) . 1_565 ? C8 C12 Eu1 157.2(4) . 1_565 ? N2 C13 C14 122.8(6) . . ? N2 C13 S2 117.6(4) . . ? C14 C13 S2 119.6(4) . . ? C13 C14 C15 118.0(5) . . ? C13 C14 C18 123.4(5) . . ? C15 C14 C18 118.5(5) . . ? C16 C15 C14 118.9(6) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C17 C16 C15 119.0(6) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 N2 123.7(6) . . ? C16 C17 H17 118.2 . . ? N2 C17 H17 118.2 . . ? O6 C18 O5 121.6(5) . . ? O6 C18 C14 119.2(5) . . ? O5 C18 C14 119.2(5) . . ? O6 C18 Eu1 62.8(3) . . ? O5 C18 Eu1 59.3(3) . . ? C14 C18 Eu1 171.8(4) . . ? S4 C19 H19A 109.5 . . ? S4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? S4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? S4 C20 H20A 109.5 . . ? S4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? S4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? S5 C21 H21A 109.5 . . ? S5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S5 C22 H22A 109.5 . . ? S5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S6 C23 H23A 109.5 . . ? S6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? S6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S6 C24 H24A 109.5 . . ? S6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.675 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.160 # Attachment 'Nd.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 642853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H27 N3 Nd O9 S6' _chemical_formula_weight 838.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Nd Nd -0.1943 3.0179 '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 7.7400(15) _cell_length_b 12.154(2) _cell_length_c 17.433(4) _cell_angle_alpha 73.85(3) _cell_angle_beta 88.22(3) _cell_angle_gamma 88.55(3) _cell_volume 1574.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12073 _cell_measurement_theta_min 6.26 _cell_measurement_theta_max 55.22 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 2.101 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.5714 _exptl_absorpt_correction_T_max 0.8174 _exptl_absorpt_process_details ; semi-empirical absorption based on psi-scan (North, et al. 1968) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type RAXIS-RAPID _diffrn_measurement_method w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15379 _diffrn_reflns_av_R_equivalents 0.0817 _diffrn_reflns_av_sigmaI/netI 0.1108 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7042 _reflns_number_gt 5515 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+4.5892P] 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 7042 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 0.17669(4) -0.26496(3) -0.257235(18) 0.02229(10) Uani 1 1 d . . . S1A S 0.2328(4) -0.3229(3) -0.44113(17) 0.0322(7) Uani 0.50 1 d P . . S1B S 0.0902(6) -0.3471(4) -0.4530(2) 0.0545(11) Uani 0.50 1 d P . . S2 S 0.31485(19) -0.68134(13) -0.26169(9) 0.0287(3) Uani 1 1 d . . . S3 S 0.3283(2) -0.84574(13) -0.26881(9) 0.0305(3) Uani 1 1 d . . . S4 S -0.2289(2) -0.08147(16) -0.28705(10) 0.0379(4) Uani 1 1 d . . . S5 S -0.0534(2) -0.46657(16) -0.09790(10) 0.0412(4) Uani 1 1 d . . . S6 S 0.0164(2) -0.05117(18) -0.03961(10) 0.0423(5) Uani 1 1 d . . . O1 O 0.3248(6) -0.3017(4) -0.1279(2) 0.0372(11) Uani 1 1 d . . . O2 O 0.0966(5) -0.1913(4) -0.1335(3) 0.0362(11) Uani 1 1 d . . . O3 O 0.2959(6) -0.4711(4) -0.2332(3) 0.0378(11) Uani 1 1 d . . . O4 O 0.4729(6) -0.3309(4) -0.2867(3) 0.0366(11) Uani 1 1 d . . . O5 O -0.0432(5) -0.3934(4) -0.1827(2) 0.0344(10) Uani 1 1 d . . . O6 O 0.0976(6) -0.3338(4) -0.3716(3) 0.0412(11) Uani 1 1 d . . . O7 O 0.3045(6) -1.0654(4) -0.2761(2) 0.0335(10) Uani 1 1 d . . . O8 O 0.2771(7) -1.1217(4) -0.3840(3) 0.0420(12) Uani 1 1 d . . . O9 O -0.0835(6) -0.1574(4) -0.3016(3) 0.0412(12) Uani 1 1 d . . . N1 N 0.2811(8) -0.0762(6) 0.0564(3) 0.0458(16) Uani 1 1 d . . . N2 N 0.3386(8) -0.7226(5) -0.4222(3) 0.0397(14) Uani 1 1 d . . . N3 N 0.6544(7) -0.7079(5) -0.2880(4) 0.0370(13) Uani 1 1 d . . . C1 C 0.2182(8) -0.1108(6) -0.0030(3) 0.0314(14) Uani 1 1 d . . . C2 C 0.3069(8) -0.1884(6) -0.0369(3) 0.0289(13) Uani 1 1 d . . . C3 C 0.4667(9) -0.2272(6) -0.0059(4) 0.0404(17) Uani 1 1 d . . . H3 H 0.5303 -0.2790 -0.0263 0.049 Uiso 1 1 calc R . . C4 C 0.5323(9) -0.1904(8) 0.0545(5) 0.054(2) Uani 1 1 d . . . H4 H 0.6405 -0.2158 0.0747 0.065 Uiso 1 1 calc R . . C5 C 0.4365(10) -0.1162(8) 0.0843(4) 0.053(2) Uani 1 1 d . . . H5 H 0.4805 -0.0920 0.1258 0.064 Uiso 1 1 calc R . . C6 C 0.2368(8) -0.2298(5) -0.1020(3) 0.0264(12) Uani 1 1 d . . . C7 C 0.8149(9) -0.6714(6) -0.2993(4) 0.0402(16) Uani 1 1 d . . . H7 H 0.9006 -0.7242 -0.3041 0.048 Uiso 1 1 calc R . . C8 C 0.5326(7) -0.6334(5) -0.2777(3) 0.0262(12) Uani 1 1 d . . . C9 C 0.5698(8) -0.5196(5) -0.2811(3) 0.0270(13) Uani 1 1 d . . . C10 C 0.7379(8) -0.4844(6) -0.2963(3) 0.0295(13) Uani 1 1 d . . . H10 H 0.7650 -0.4086 -0.3011 0.035 Uiso 1 1 calc R . . C11 C 0.8667(8) -0.5615(6) -0.3046(4) 0.0364(15) Uani 1 1 d . . . H11 H 0.9819 -0.5405 -0.3133 0.044 Uiso 1 1 calc R . . C12 C 0.4374(7) -0.4357(5) -0.2661(3) 0.0248(12) Uani 1 1 d . . . C13 C 0.3293(7) -0.8302(5) -0.3742(3) 0.0255(12) Uani 1 1 d . . . C14 C 0.3190(7) -0.9259(5) -0.4035(3) 0.0242(12) Uani 1 1 d . . . C15 C 0.3216(9) -0.9071(6) -0.4858(4) 0.0380(15) Uani 1 1 d . . . H15 H 0.3147 -0.9690 -0.5071 0.046 Uiso 1 1 calc R . . C16 C 0.3340(11) -0.7989(6) -0.5357(4) 0.0473(19) Uani 1 1 d . . . H16 H 0.3392 -0.7857 -0.5909 0.057 Uiso 1 1 calc R . . C17 C 0.3385(10) -0.7101(6) -0.5012(4) 0.0460(18) Uani 1 1 d . . . H17 H 0.3419 -0.6360 -0.5351 0.055 Uiso 1 1 calc R . . C18 C 0.3008(7) -1.0451(5) -0.3511(3) 0.0262(12) Uani 1 1 d . . . C19 C 0.1523(14) -0.2139(8) -0.5219(5) 0.066(3) Uani 1 1 d . . . C20 C -0.3210(9) -0.1517(7) -0.1919(5) 0.0502(19) Uani 1 1 d . . . H20A H -0.3831 -0.2174 -0.1955 0.075 Uiso 1 1 calc R . . H20B H -0.3989 -0.0999 -0.1749 0.075 Uiso 1 1 calc R . . H20C H -0.2307 -0.1757 -0.1540 0.075 Uiso 1 1 calc R . . C21 C -0.1269(10) 0.0323(7) -0.2609(5) 0.054(2) Uani 1 1 d . . . H21A H -0.0689 0.0803 -0.3072 0.081 Uiso 1 1 calc R . . H21B H -0.0444 0.0012 -0.2202 0.081 Uiso 1 1 calc R . . H21C H -0.2125 0.0769 -0.2412 0.081 Uiso 1 1 calc R . . C22A C 0.198(6) -0.437(3) -0.4806(18) 0.112(17) Uani 0.50 1 d P . . C22B C 0.270(4) -0.435(3) -0.4588(15) 0.085(12) Uani 0.50 1 d P . . C23 C 0.0116(12) -0.6063(7) -0.0983(5) 0.064(3) Uani 1 1 d . . . H23A H 0.1340 -0.6084 -0.1088 0.096 Uiso 1 1 calc R . . H23B H -0.0481 -0.6280 -0.1391 0.096 Uiso 1 1 calc R . . H23C H -0.0156 -0.6586 -0.0472 0.096 Uiso 1 1 calc R . . C24 C -0.2755(11) -0.4924(9) -0.0770(5) 0.073(3) Uani 1 1 d . . . H24A H -0.3336 -0.4228 -0.0744 0.109 Uiso 1 1 calc R . . H24B H -0.2899 -0.5496 -0.0268 0.109 Uiso 1 1 calc R . . H24C H -0.3240 -0.5190 -0.1185 0.109 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 Nd1 0.02906(17) 0.01439(16) 0.02448(16) -0.00749(11) 0.00291(12) -0.00105(11) S1A 0.0332(16) 0.044(2) 0.0244(14) -0.0169(13) -0.0034(13) 0.0028(14) S1B 0.076(3) 0.047(3) 0.047(2) -0.0230(18) -0.011(2) 0.002(2) S2 0.0307(7) 0.0224(8) 0.0372(8) -0.0148(6) -0.0026(6) -0.0041(6) S3 0.0434(9) 0.0199(8) 0.0280(7) -0.0055(6) -0.0050(7) -0.0056(6) S4 0.0359(8) 0.0412(11) 0.0370(8) -0.0120(7) -0.0082(7) 0.0132(7) S5 0.0543(10) 0.0359(10) 0.0300(8) -0.0034(7) 0.0056(8) -0.0095(8) S6 0.0411(9) 0.0553(12) 0.0432(9) -0.0349(9) -0.0172(8) 0.0178(8) O1 0.046(3) 0.035(3) 0.033(2) -0.014(2) -0.004(2) 0.010(2) O2 0.032(2) 0.043(3) 0.041(2) -0.023(2) -0.008(2) 0.006(2) O3 0.043(2) 0.017(2) 0.054(3) -0.012(2) 0.014(2) -0.0028(19) O4 0.040(2) 0.017(2) 0.051(3) -0.007(2) 0.005(2) 0.0009(18) O5 0.039(2) 0.036(3) 0.027(2) -0.0060(19) 0.0029(19) -0.0071(19) O6 0.054(3) 0.039(3) 0.036(2) -0.018(2) 0.001(2) -0.015(2) O7 0.048(3) 0.024(2) 0.029(2) -0.0058(18) -0.006(2) -0.0042(19) O8 0.072(3) 0.021(3) 0.035(2) -0.0112(19) 0.007(2) -0.008(2) O9 0.041(3) 0.044(3) 0.042(2) -0.020(2) -0.006(2) 0.013(2) N1 0.052(4) 0.054(4) 0.043(3) -0.034(3) -0.019(3) 0.021(3) N2 0.063(4) 0.020(3) 0.035(3) -0.006(2) -0.003(3) -0.001(3) N3 0.034(3) 0.020(3) 0.062(4) -0.020(3) 0.001(3) -0.002(2) C1 0.038(3) 0.030(4) 0.026(3) -0.008(2) -0.006(3) 0.007(3) C2 0.035(3) 0.030(4) 0.021(3) -0.007(2) -0.001(2) -0.001(3) C3 0.040(4) 0.045(5) 0.036(3) -0.013(3) -0.009(3) 0.016(3) C4 0.038(4) 0.082(7) 0.052(4) -0.034(4) -0.024(4) 0.022(4) C5 0.049(4) 0.075(6) 0.046(4) -0.034(4) -0.028(4) 0.015(4) C6 0.034(3) 0.024(3) 0.024(3) -0.011(2) 0.003(2) -0.003(2) C7 0.037(3) 0.029(4) 0.060(4) -0.021(3) 0.000(3) 0.005(3) C8 0.026(3) 0.021(3) 0.035(3) -0.012(2) -0.011(2) 0.004(2) C9 0.036(3) 0.018(3) 0.026(3) -0.005(2) -0.004(2) 0.005(2) C10 0.034(3) 0.023(3) 0.034(3) -0.011(2) -0.008(3) -0.003(2) C11 0.026(3) 0.027(4) 0.057(4) -0.014(3) 0.003(3) -0.002(3) C12 0.032(3) 0.018(3) 0.028(3) -0.013(2) 0.002(2) 0.003(2) C13 0.027(3) 0.018(3) 0.031(3) -0.004(2) 0.003(2) -0.005(2) C14 0.020(3) 0.025(3) 0.028(3) -0.007(2) -0.003(2) -0.005(2) C15 0.055(4) 0.026(4) 0.036(3) -0.014(3) 0.005(3) -0.009(3) C16 0.082(5) 0.030(4) 0.026(3) -0.003(3) 0.009(3) 0.001(4) C17 0.074(5) 0.026(4) 0.033(3) 0.001(3) 0.000(3) -0.003(3) C18 0.026(3) 0.020(3) 0.034(3) -0.008(2) -0.002(2) -0.004(2) C19 0.119(8) 0.035(5) 0.040(4) -0.004(4) -0.004(5) -0.004(5) C20 0.038(4) 0.048(5) 0.063(5) -0.014(4) 0.005(4) -0.007(3) C21 0.056(5) 0.031(4) 0.076(5) -0.017(4) -0.002(4) 0.004(3) C22A 0.24(5) 0.044(15) 0.048(14) -0.010(11) -0.015(18) 0.05(2) C22B 0.11(2) 0.081(18) 0.044(14) 0.007(14) 0.045(16) 0.047(17) C23 0.082(6) 0.046(5) 0.052(5) 0.002(4) 0.018(4) 0.009(4) C24 0.071(6) 0.067(7) 0.060(5) 0.010(5) 0.032(5) 0.004(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 Nd1 O9 2.401(4) . ? Nd1 O5 2.427(4) . ? Nd1 O6 2.466(5) . ? Nd1 O1 2.484(4) . ? Nd1 O4 2.495(4) . ? Nd1 O8 2.518(5) 1_565 ? Nd1 O3 2.574(4) . ? Nd1 O7 2.574(5) 1_565 ? Nd1 O2 2.607(4) . ? Nd1 C18 2.888(6) 1_565 ? Nd1 C12 2.890(5) . ? Nd1 C6 2.907(6) . ? S1A S1B 1.188(6) . ? S1A C22B 1.50(4) . ? S1A O6 1.555(6) . ? S1A C22A 1.74(4) . ? S1A C19 1.761(8) . ? S1B O6 1.474(6) . ? S1B C22A 1.53(4) . ? S1B C22B 1.75(3) . ? S1B C19 1.794(10) . ? S2 C8 1.785(6) . ? S2 S3 2.036(2) . ? S3 C13 1.793(6) . ? S4 O9 1.497(5) . ? S4 C20 1.777(8) . ? S4 C21 1.781(9) . ? S5 O5 1.499(4) . ? S5 C23 1.761(9) . ? S5 C24 1.764(9) . ? S6 C1 1.766(6) . ? S6 S6 2.106(3) 2 ? O1 C6 1.265(7) . ? O2 C6 1.251(7) . ? O3 C12 1.250(7) . ? O4 C12 1.259(7) . ? O7 C18 1.262(7) . ? O7 Nd1 2.574(5) 1_545 ? O8 C18 1.243(8) . ? O8 Nd1 2.518(5) 1_545 ? N1 C1 1.331(8) . ? N1 C5 1.340(8) . ? N2 C17 1.343(8) . ? N2 C13 1.345(7) . ? N3 C7 1.320(9) . ? N3 C8 1.333(7) . ? C1 C2 1.401(9) . ? C2 C3 1.384(8) . ? C2 C6 1.486(8) . ? C3 C4 1.368(10) . ? C3 H3 0.9300 . ? C4 C5 1.355(11) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C11 1.382(10) . ? C7 H7 0.9300 . ? C8 C9 1.405(9) . ? C9 C10 1.375(9) . ? C9 C12 1.495(8) . ? C10 C11 1.383(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 C14 1.400(9) . ? C14 C15 1.387(8) . ? C14 C18 1.490(8) . ? C15 C16 1.364(9) . ? C15 H15 0.9300 . ? C16 C17 1.375(11) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 Nd1 2.888(6) 1_545 ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22A C22B 0.68(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 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 O9 Nd1 O5 78.40(16) . . ? O9 Nd1 O6 77.32(16) . . ? O5 Nd1 O6 85.59(15) . . ? O9 Nd1 O1 129.95(15) . . ? O5 Nd1 O1 85.84(15) . . ? O6 Nd1 O1 148.65(16) . . ? O9 Nd1 O4 150.00(15) . . ? O5 Nd1 O4 123.26(15) . . ? O6 Nd1 O4 83.59(16) . . ? O1 Nd1 O4 76.15(15) . . ? O9 Nd1 O8 77.58(17) . 1_565 ? O5 Nd1 O8 149.78(15) . 1_565 ? O6 Nd1 O8 71.45(16) . 1_565 ? O1 Nd1 O8 123.87(16) . 1_565 ? O4 Nd1 O8 74.48(15) . 1_565 ? O9 Nd1 O3 138.89(17) . . ? O5 Nd1 O3 72.45(15) . . ? O6 Nd1 O3 72.18(16) . . ? O1 Nd1 O3 76.48(16) . . ? O4 Nd1 O3 51.21(14) . . ? O8 Nd1 O3 116.46(15) 1_565 . ? O9 Nd1 O7 83.51(16) . 1_565 ? O5 Nd1 O7 142.60(15) . 1_565 ? O6 Nd1 O7 121.97(15) . 1_565 ? O1 Nd1 O7 81.11(15) . 1_565 ? O4 Nd1 O7 87.31(15) . 1_565 ? O8 Nd1 O7 50.97(14) 1_565 1_565 ? O3 Nd1 O7 136.32(14) . 1_565 ? O9 Nd1 O2 79.38(14) . . ? O5 Nd1 O2 74.46(16) . . ? O6 Nd1 O2 151.90(15) . . ? O1 Nd1 O2 50.60(13) . . ? O4 Nd1 O2 123.87(14) . . ? O8 Nd1 O2 118.30(16) 1_565 . ? O3 Nd1 O2 118.42(15) . . ? O7 Nd1 O2 70.16(15) 1_565 . ? O9 Nd1 C18 76.40(17) . 1_565 ? O5 Nd1 C18 153.70(15) . 1_565 ? O6 Nd1 C18 96.08(17) . 1_565 ? O1 Nd1 C18 104.74(17) . 1_565 ? O4 Nd1 C18 82.92(15) . 1_565 ? O8 Nd1 C18 25.42(16) 1_565 1_565 ? O3 Nd1 C18 133.05(15) . 1_565 ? O7 Nd1 C18 25.90(15) 1_565 1_565 ? O2 Nd1 C18 93.51(17) . 1_565 ? O9 Nd1 C12 152.12(16) . . ? O5 Nd1 C12 98.04(17) . . ? O6 Nd1 C12 74.83(16) . . ? O1 Nd1 C12 76.61(15) . . ? O4 Nd1 C12 25.72(16) . . ? O8 Nd1 C12 94.69(16) 1_565 . ? O3 Nd1 C12 25.61(15) . . ? O7 Nd1 C12 112.56(16) 1_565 . ? O2 Nd1 C12 126.75(14) . . ? C18 Nd1 C12 107.76(17) 1_565 . ? O9 Nd1 C6 104.68(16) . . ? O5 Nd1 C6 82.85(16) . . ? O6 Nd1 C6 167.57(17) . . ? O1 Nd1 C6 25.64(15) . . ? O4 Nd1 C6 98.95(16) . . ? O8 Nd1 C6 120.97(17) 1_565 . ? O3 Nd1 C6 99.83(16) . . ? O7 Nd1 C6 70.41(15) 1_565 . ? O2 Nd1 C6 25.49(14) . . ? C18 Nd1 C6 96.31(18) 1_565 . ? C12 Nd1 C6 102.24(16) . . ? S1B S1A C22B 80.3(14) . . ? S1B S1A O6 63.4(3) . . ? C22B S1A O6 112.2(12) . . ? S1B S1A C22A 59.6(15) . . ? C22B S1A C22A 22.9(19) . . ? O6 S1A C22A 106.4(15) . . ? S1B S1A C19 72.0(4) . . ? C22B S1A C19 114.8(11) . . ? O6 S1A C19 105.7(4) . . ? C22A S1A C19 97.0(10) . . ? S1A S1B O6 70.6(3) . . ? S1A S1B C22A 78.4(18) . . ? O6 S1B C22A 122.9(11) . . ? S1A S1B C22B 57.7(15) . . ? O6 S1B C22B 103.5(10) . . ? C22A S1B C22B 23(2) . . ? S1A S1B C19 69.0(4) . . ? O6 S1B C19 107.8(4) . . ? C22A S1B C19 103.8(16) . . ? C22B S1B C19 101.8(12) . . ? C8 S2 S3 104.5(2) . . ? C13 S3 S2 103.6(2) . . ? O9 S4 C20 106.3(3) . . ? O9 S4 C21 104.9(3) . . ? C20 S4 C21 98.5(4) . . ? O5 S5 C23 107.2(3) . . ? O5 S5 C24 105.2(3) . . ? C23 S5 C24 97.9(5) . . ? C1 S6 S6 95.5(2) . 2 ? C6 O1 Nd1 96.2(3) . . ? C6 O2 Nd1 90.7(3) . . ? C12 O3 Nd1 91.5(3) . . ? C12 O4 Nd1 94.9(3) . . ? S5 O5 Nd1 132.1(3) . . ? S1B O6 S1A 46.1(3) . . ? S1B O6 Nd1 161.7(4) . . ? S1A O6 Nd1 118.1(3) . . ? C18 O7 Nd1 91.1(4) . 1_545 ? C18 O8 Nd1 94.2(4) . 1_545 ? S4 O9 Nd1 149.5(3) . . ? C1 N1 C5 118.6(6) . . ? C17 N2 C13 116.7(6) . . ? C7 N3 C8 117.1(6) . . ? N1 C1 C2 122.7(5) . . ? N1 C1 S6 116.6(5) . . ? C2 C1 S6 120.7(5) . . ? C3 C2 C1 116.3(6) . . ? C3 C2 C6 120.3(6) . . ? C1 C2 C6 123.3(5) . . ? C4 C3 C2 121.0(6) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C5 C4 C3 118.6(6) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.8(7) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? O2 C6 O1 120.0(5) . . ? O2 C6 C2 121.1(5) . . ? O1 C6 C2 118.9(5) . . ? O2 C6 Nd1 63.8(3) . . ? O1 C6 Nd1 58.2(3) . . ? C2 C6 Nd1 162.8(4) . . ? N3 C7 C11 125.7(6) . . ? N3 C7 H7 117.1 . . ? C11 C7 H7 117.1 . . ? N3 C8 C9 122.3(6) . . ? N3 C8 S2 117.8(5) . . ? C9 C8 S2 119.8(4) . . ? C10 C9 C8 118.3(5) . . ? C10 C9 C12 118.1(6) . . ? C8 C9 C12 123.5(6) . . ? C9 C10 C11 120.1(6) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C7 C11 C10 116.3(6) . . ? C7 C11 H11 121.8 . . ? C10 C11 H11 121.8 . . ? O3 C12 O4 121.8(5) . . ? O3 C12 C9 119.5(5) . . ? O4 C12 C9 118.7(5) . . ? O3 C12 Nd1 62.9(3) . . ? O4 C12 Nd1 59.3(3) . . ? C9 C12 Nd1 173.3(4) . . ? N2 C13 C14 122.7(5) . . ? N2 C13 S3 116.4(5) . . ? C14 C13 S3 120.9(4) . . ? C15 C14 C13 117.6(6) . . ? C15 C14 C18 119.1(6) . . ? C13 C14 C18 123.3(5) . . ? C16 C15 C14 120.7(7) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 117.4(6) . . ? C15 C16 H16 121.3 . . ? C17 C16 H16 121.3 . . ? N2 C17 C16 124.8(6) . . ? N2 C17 H17 117.6 . . ? C16 C17 H17 117.6 . . ? O8 C18 O7 122.1(6) . . ? O8 C18 C14 117.4(5) . . ? O7 C18 C14 120.5(6) . . ? O8 C18 Nd1 60.4(3) . 1_545 ? O7 C18 Nd1 63.0(3) . 1_545 ? C14 C18 Nd1 165.9(4) . 1_545 ? S1A C19 S1B 39.0(2) . . ? S4 C20 H20A 109.5 . . ? S4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? S4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? S4 C21 H21A 109.5 . . ? S4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22B C22A S1B 97(6) . . ? C22B C22A S1A 59(5) . . ? S1B C22A S1A 42.0(10) . . ? C22A C22B S1A 98(5) . . ? C22A C22B S1B 60(5) . . ? S1A C22B S1B 41.9(8) . . ? S5 C23 H23A 109.5 . . ? S5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? S5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S5 C24 H24A 109.5 . . ? S5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.745 _refine_diff_density_min -1.037 _refine_diff_density_rms 0.166