# 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 _publ_contact_author_name 'Ya-Wen Wang' _publ_contact_author_email YWWANG@LZU.EDU.CN _publ_section_title ; Synthesis, radii dependent self-assembly crystal structures and luminescent properties of rare earth (III) complexes with a tripodal salicylic derivative ; loop_ _publ_author_name 'Ya-Wen Wang' 'Wei Dou' 'Wei-Sheng Liu' 'Wenwu Qin' 'Ai-Jiang Zhang' 'Yanling Zhang' # Attachment 'complexes.cif' data_1 #TrackingRef 'complexes.cif' _database_code_depnum_ccdc_archive 'CCDC 731522' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H94 La2 N8 O28 S2' _chemical_formula_weight 1981.6 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' La La -0.2871 2.4523 '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' 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' H H 0.0000 0.0000 '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 14.721(3) _cell_length_b 14.825(3) _cell_length_c 15.953(3) _cell_angle_alpha 108.509(7) _cell_angle_beta 109.630(8) _cell_angle_gamma 91.613(8) _cell_volume 3074.0(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.59 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.856 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16928 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11314 _reflns_number_gt 8325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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. During the refinement, the restrains for the DMF solvent molecules: SIMU 0.02 0.04 3.8 C34 > C35 ISOR 0.02 C34 C35 ; _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^)+(0.0455P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11314 _refine_ls_number_parameters 555 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.014 _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 La1 La 0.387354(15) 0.416952(14) 0.872114(13) 0.04599(8) Uani 1 1 d . . . S1 S 0.45171(10) 0.13261(8) 1.28424(8) 0.0739(3) Uani 1 1 d . . . C1 C 0.8005(5) -0.0555(4) 1.2420(5) 0.135(2) Uani 1 1 d . . . H1A H 0.7817 -0.1049 1.1807 0.202 Uiso 1 1 calc R . . H1B H 0.8266 -0.0831 1.2904 0.202 Uiso 1 1 calc R . . H1C H 0.8490 -0.0069 1.2480 0.202 Uiso 1 1 calc R . . C2 C 0.7132(4) -0.0114(3) 1.2529(3) 0.0872(14) Uani 1 1 d . . . C3 C 0.7248(4) 0.0823(4) 1.3163(3) 0.1017(16) Uani 1 1 d . . . H3 H 0.7874 0.1154 1.3538 0.122 Uiso 1 1 calc R . . C4 C 0.6468(4) 0.1257(3) 1.3242(3) 0.0900(14) Uani 1 1 d . . . H4 H 0.6562 0.1878 1.3671 0.108 Uiso 1 1 calc R . . C5 C 0.5525(4) 0.0775(3) 1.2682(3) 0.0709(12) Uani 1 1 d . . . C6 C 0.5407(4) -0.0130(3) 1.2050(3) 0.0714(12) Uani 1 1 d . . . H6 H 0.4782 -0.0456 1.1663 0.086 Uiso 1 1 calc R . . C7 C 0.6197(4) -0.0565(3) 1.1980(3) 0.0840(14) Uani 1 1 d . . . H7 H 0.6097 -0.1185 1.1547 0.101 Uiso 1 1 calc R . . C8 C 0.4115(3) 0.2317(2) 1.1590(2) 0.0549(9) Uani 1 1 d . . . C9 C 0.4672(3) 0.1797(2) 1.0967(2) 0.0559(9) Uani 1 1 d . . . H9A H 0.4688 0.1141 1.0960 0.067 Uiso 1 1 calc R . . H9B H 0.4346 0.1777 1.0321 0.067 Uiso 1 1 calc R . . C10 C 0.6182(3) 0.1959(2) 1.0773(2) 0.0537(9) Uani 1 1 d . . . C11 C 0.6658(3) 0.1173(3) 1.0849(3) 0.0782(13) Uani 1 1 d . . . H11 H 0.6591 0.0870 1.1259 0.094 Uiso 1 1 calc R . . C12 C 0.7228(4) 0.0844(3) 1.0315(4) 0.0867(14) Uani 1 1 d . . . H12 H 0.7560 0.0332 1.0380 0.104 Uiso 1 1 calc R . . C13 C 0.7306(3) 0.1270(3) 0.9688(3) 0.0771(13) Uani 1 1 d . . . H13 H 0.7679 0.1040 0.9319 0.092 Uiso 1 1 calc R . . C14 C 0.6822(3) 0.2051(3) 0.9612(3) 0.0623(10) Uani 1 1 d . . . H14 H 0.6869 0.2337 0.9184 0.075 Uiso 1 1 calc R . . C15 C 0.6273(2) 0.2409(2) 1.0160(2) 0.0461(8) Uani 1 1 d . . . C16 C 0.5797(3) 0.3273(2) 1.0088(2) 0.0493(8) Uani 1 1 d . . . C17 C 0.4247(3) 0.3374(2) 1.1694(2) 0.0502(8) Uani 1 1 d . . . H17C H 0.4927 0.3655 1.2050 0.060 Uiso 1 1 calc R . . H17D H 0.4065 0.3432 1.1073 0.060 Uiso 1 1 calc R . . C18 C 0.2959(3) 0.4349(2) 1.1734(2) 0.0515(9) Uani 1 1 d . . . C19 C 0.2062(3) 0.4258(3) 1.1801(3) 0.0703(11) Uani 1 1 d . . . H19 H 0.1945 0.3905 1.2153 0.084 Uiso 1 1 calc R . . C20 C 0.1333(3) 0.4689(4) 1.1347(4) 0.0847(14) Uani 1 1 d . . . H20 H 0.0723 0.4625 1.1394 0.102 Uiso 1 1 calc R . . C21 C 0.1499(3) 0.5216(3) 1.0822(3) 0.0816(13) Uani 1 1 d . . . H21 H 0.1006 0.5503 1.0512 0.098 Uiso 1 1 calc R . . C22 C 0.2413(3) 0.5307(3) 1.0765(3) 0.0662(11) Uani 1 1 d . . . H22 H 0.2527 0.5651 1.0405 0.079 Uiso 1 1 calc R . . C23 C 0.3162(2) 0.4894(2) 1.1236(2) 0.0472(8) Uani 1 1 d . . . C24 C 0.4164(3) 0.5105(2) 1.1244(2) 0.0481(8) Uani 1 1 d . . . C25 C 0.3020(3) 0.1905(3) 1.1103(3) 0.0692(11) Uani 1 1 d . . . H25A H 0.2923 0.1216 1.0969 0.083 Uiso 1 1 calc R . . H25B H 0.2666 0.2208 1.1505 0.083 Uiso 1 1 calc R . . C26 C 0.1747(3) 0.2240(3) 0.9868(3) 0.0637(10) Uani 1 1 d . . . C27 C 0.1017(3) 0.1873(3) 1.0086(3) 0.0792(12) Uani 1 1 d . . . H27 H 0.1171 0.1532 1.0501 0.095 Uiso 1 1 calc R . . C28 C 0.0080(4) 0.2005(4) 0.9703(4) 0.1009(17) Uani 1 1 d . . . H28 H -0.0405 0.1744 0.9848 0.121 Uiso 1 1 calc R . . C29 C -0.0156(3) 0.2520(4) 0.9102(4) 0.1027(17) Uani 1 1 d . . . H29 H -0.0796 0.2619 0.8842 0.123 Uiso 1 1 calc R . . C30 C 0.0580(3) 0.2890(3) 0.8891(3) 0.0838(13) Uani 1 1 d . . . H30 H 0.0424 0.3242 0.8486 0.101 Uiso 1 1 calc R . . C31 C 0.1541(3) 0.2754(3) 0.9262(3) 0.0611(10) Uani 1 1 d . . . C32 C 0.2292(3) 0.3182(3) 0.8987(3) 0.0613(10) Uani 1 1 d . . . C33 C 0.4206(5) 0.2200(3) 0.7068(3) 0.0945(16) Uani 1 1 d . . . H33 H 0.4845 0.2352 0.7502 0.113 Uiso 1 1 calc R . . C34 C 0.4751(7) 0.0902(5) 0.6029(6) 0.189(3) Uani 1 1 d U . . H34A H 0.5377 0.1139 0.6530 0.284 Uiso 1 1 calc R . . H34B H 0.4792 0.0933 0.5450 0.284 Uiso 1 1 calc R . . H34C H 0.4554 0.0247 0.5945 0.284 Uiso 1 1 calc R . . C35 C 0.3064(7) 0.1201(5) 0.5566(5) 0.192(4) Uani 1 1 d U . . H35A H 0.3090 0.1116 0.4953 0.288 Uiso 1 1 calc R . . H35B H 0.2672 0.1690 0.5715 0.288 Uiso 1 1 calc R . . H35C H 0.2783 0.0607 0.5561 0.288 Uiso 1 1 calc R . . C36 C 0.2760(3) 0.5318(4) 0.7125(3) 0.0733(12) Uani 1 1 d . . . H36 H 0.3161 0.5870 0.7594 0.088 Uiso 1 1 calc R . . C37 C 0.2083(5) 0.6344(5) 0.6252(5) 0.159(3) Uani 1 1 d . . . H37A H 0.1471 0.6546 0.6260 0.191 Uiso 1 1 d R . . H37B H 0.2136 0.6289 0.5655 0.191 Uiso 1 1 d R . . H37C H 0.2608 0.6811 0.6757 0.191 Uiso 1 1 d R . . C38 C 0.1525(5) 0.4628(6) 0.5617(4) 0.148(3) Uani 1 1 d . . . H38A H 0.1756 0.4469 0.5099 0.178 Uiso 1 1 d R . . H38B H 0.0883 0.4797 0.5415 0.178 Uiso 1 1 d R . . H38C H 0.1505 0.4084 0.5816 0.178 Uiso 1 1 d R . . C39 C 0.4321(4) 0.5213(4) 0.5964(3) 0.0830(13) Uani 1 1 d . . . H39 H 0.4687 0.5154 0.6540 0.100 Uiso 1 1 calc R . . C40 C 0.3972(5) 0.3497(4) 0.5372(4) 0.138(2) Uani 1 1 d . . . H40A H 0.4374 0.3585 0.6015 0.207 Uiso 1 1 calc R . . H40B H 0.4255 0.3105 0.4948 0.207 Uiso 1 1 calc R . . H40C H 0.3331 0.3185 0.5233 0.207 Uiso 1 1 calc R . . C41 C 0.3356(4) 0.4435(4) 0.4328(3) 0.123(2) Uani 1 1 d . . . H41A H 0.3297 0.5087 0.4359 0.184 Uiso 1 1 calc R . . H41B H 0.2719 0.4072 0.4103 0.184 Uiso 1 1 calc R . . H41C H 0.3685 0.4153 0.3903 0.184 Uiso 1 1 calc R . . N1 N 0.4485(2) 0.2271(2) 1.2558(2) 0.0625(8) Uani 1 1 d . . . H1 H 0.4708 0.2812 1.3019 0.075 Uiso 1 1 calc R . . N2 N 0.2157(3) 0.5415(3) 0.6374(3) 0.0813(11) Uani 1 1 d . . . N3 N 0.4038(4) 0.1489(3) 0.6272(3) 0.1116(16) Uani 1 1 d . . . N4 N 0.3906(3) 0.4425(3) 0.5253(2) 0.0818(11) Uani 1 1 d . . . O1 O 0.3668(2) 0.0647(2) 1.2210(2) 0.0885(9) Uani 1 1 d . . . O2 O 0.4717(3) 0.1672(2) 1.3842(2) 0.0948(10) Uani 1 1 d . . . O3 O 0.56398(18) 0.22964(16) 1.13383(16) 0.0564(6) Uani 1 1 d . . . O4 O 0.51320(17) 0.31818(16) 0.93214(17) 0.0558(6) Uani 1 1 d . . . O5 O 0.61267(18) 0.40384(16) 1.07940(16) 0.0594(6) Uani 1 1 d . . . O6 O 0.36440(19) 0.38811(17) 1.21839(17) 0.0600(7) Uani 1 1 d . . . O7 O 0.48497(18) 0.55089(17) 1.20032(16) 0.0590(6) Uani 1 1 d . . . O8 O 0.42777(16) 0.48927(15) 1.04523(15) 0.0516(6) Uani 1 1 d . . . O9 O 0.2694(2) 0.2109(2) 1.02447(19) 0.0754(8) Uani 1 1 d . . . O10 O 0.31091(19) 0.28975(18) 0.91341(19) 0.0671(7) Uani 1 1 d . . . O11 O 0.20988(19) 0.3842(2) 0.8635(2) 0.0729(7) Uani 1 1 d . . . O12 O 0.3628(2) 0.26798(18) 0.73024(18) 0.0746(8) Uani 1 1 d . . . O13 O 0.2852(2) 0.4553(2) 0.72751(18) 0.0729(8) Uani 1 1 d . . . O14 O 0.4273(3) 0.6036(3) 0.5944(2) 0.0997(10) 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 La1 0.05005(13) 0.04187(12) 0.03539(11) 0.00777(8) 0.00803(9) 0.00362(8) S1 0.1093(9) 0.0578(6) 0.0649(7) 0.0279(5) 0.0378(7) 0.0158(6) C1 0.138(5) 0.121(5) 0.137(5) 0.036(4) 0.042(4) 0.073(4) C2 0.118(4) 0.062(3) 0.074(3) 0.023(2) 0.025(3) 0.030(3) C3 0.105(4) 0.080(3) 0.082(3) 0.010(3) 0.005(3) 0.019(3) C4 0.114(4) 0.065(3) 0.072(3) 0.011(2) 0.022(3) 0.025(3) C5 0.101(3) 0.048(2) 0.054(2) 0.0174(19) 0.015(2) 0.013(2) C6 0.100(3) 0.046(2) 0.058(2) 0.0163(19) 0.018(2) 0.012(2) C7 0.137(5) 0.048(2) 0.059(3) 0.017(2) 0.027(3) 0.019(3) C8 0.068(2) 0.048(2) 0.046(2) 0.0119(16) 0.0227(19) 0.0062(18) C9 0.070(3) 0.050(2) 0.046(2) 0.0143(17) 0.0202(19) 0.0095(18) C10 0.060(2) 0.045(2) 0.049(2) 0.0084(17) 0.0179(19) 0.0126(17) C11 0.106(4) 0.062(3) 0.076(3) 0.033(2) 0.034(3) 0.038(3) C12 0.093(4) 0.066(3) 0.093(3) 0.021(3) 0.027(3) 0.043(3) C13 0.060(3) 0.073(3) 0.079(3) 0.000(2) 0.025(2) 0.019(2) C14 0.064(2) 0.055(2) 0.057(2) 0.0030(18) 0.025(2) 0.0059(19) C15 0.049(2) 0.0432(18) 0.0383(18) 0.0078(15) 0.0126(16) 0.0085(15) C16 0.057(2) 0.046(2) 0.043(2) 0.0128(16) 0.0183(19) 0.0077(17) C17 0.059(2) 0.0454(19) 0.051(2) 0.0185(16) 0.0233(18) 0.0147(16) C18 0.057(2) 0.049(2) 0.045(2) 0.0096(17) 0.0204(18) 0.0137(17) C19 0.068(3) 0.075(3) 0.076(3) 0.024(2) 0.039(2) 0.013(2) C20 0.064(3) 0.095(3) 0.092(3) 0.016(3) 0.041(3) 0.010(3) C21 0.059(3) 0.086(3) 0.091(3) 0.023(3) 0.022(3) 0.030(2) C22 0.068(3) 0.060(2) 0.065(3) 0.016(2) 0.022(2) 0.012(2) C23 0.050(2) 0.0450(19) 0.0426(19) 0.0097(16) 0.0161(17) 0.0142(16) C24 0.060(2) 0.0382(18) 0.045(2) 0.0120(16) 0.0193(19) 0.0115(16) C25 0.078(3) 0.067(3) 0.065(3) 0.022(2) 0.030(2) 0.002(2) C26 0.054(3) 0.065(2) 0.063(3) 0.010(2) 0.022(2) -0.002(2) C27 0.063(3) 0.090(3) 0.078(3) 0.027(3) 0.021(2) -0.002(2) C28 0.078(4) 0.099(4) 0.124(5) 0.030(4) 0.044(4) -0.010(3) C29 0.049(3) 0.108(4) 0.136(5) 0.028(4) 0.029(3) -0.003(3) C30 0.064(3) 0.080(3) 0.096(3) 0.026(3) 0.020(3) 0.006(2) C31 0.053(2) 0.056(2) 0.062(2) 0.006(2) 0.020(2) -0.0008(18) C32 0.053(2) 0.054(2) 0.056(2) 0.0016(19) 0.012(2) -0.0020(19) C33 0.160(5) 0.059(3) 0.072(3) 0.015(2) 0.060(3) 0.006(3) C34 0.312(10) 0.119(5) 0.201(7) 0.030(5) 0.193(7) 0.064(6) C35 0.263(9) 0.132(6) 0.089(4) 0.000(4) -0.012(6) -0.006(6) C36 0.076(3) 0.083(3) 0.055(3) 0.026(2) 0.015(2) 0.017(2) C37 0.192(8) 0.188(7) 0.158(6) 0.125(6) 0.072(6) 0.085(6) C38 0.107(5) 0.241(9) 0.075(4) 0.061(5) 0.000(4) 0.025(5) C39 0.099(4) 0.078(3) 0.058(3) 0.011(2) 0.023(3) 0.007(3) C40 0.208(7) 0.080(4) 0.112(5) 0.015(3) 0.058(5) 0.021(4) C41 0.137(5) 0.147(5) 0.058(3) 0.021(3) 0.018(3) -0.016(4) N1 0.094(2) 0.0466(17) 0.0469(17) 0.0141(14) 0.0279(17) 0.0118(16) N2 0.076(3) 0.113(3) 0.059(2) 0.049(2) 0.012(2) 0.026(2) N3 0.207(5) 0.065(2) 0.076(3) 0.018(2) 0.072(3) 0.021(3) N4 0.101(3) 0.076(3) 0.059(2) 0.0062(19) 0.034(2) 0.000(2) O1 0.102(2) 0.0656(18) 0.101(2) 0.0334(17) 0.038(2) -0.0032(17) O2 0.154(3) 0.087(2) 0.072(2) 0.0428(17) 0.059(2) 0.044(2) O3 0.0674(16) 0.0505(14) 0.0499(14) 0.0121(11) 0.0244(13) 0.0122(12) O4 0.0571(15) 0.0474(14) 0.0483(14) 0.0119(11) 0.0057(13) 0.0097(11) O5 0.0773(17) 0.0451(14) 0.0428(13) 0.0115(11) 0.0092(13) 0.0113(12) O6 0.0789(18) 0.0628(16) 0.0503(14) 0.0235(12) 0.0335(14) 0.0219(14) O7 0.0618(16) 0.0648(16) 0.0380(13) 0.0079(12) 0.0133(13) -0.0023(13) O8 0.0603(15) 0.0497(13) 0.0389(13) 0.0088(10) 0.0175(12) 0.0009(11) O9 0.0607(18) 0.105(2) 0.0629(17) 0.0352(16) 0.0200(15) 0.0059(15) O10 0.0570(17) 0.0623(16) 0.0855(19) 0.0277(14) 0.0281(15) 0.0092(13) O11 0.0630(18) 0.0783(19) 0.0763(19) 0.0349(16) 0.0162(15) 0.0128(15) O12 0.105(2) 0.0491(16) 0.0500(15) -0.0004(12) 0.0204(16) 0.0118(15) O13 0.081(2) 0.0722(19) 0.0516(16) 0.0213(14) 0.0073(14) 0.0102(15) O14 0.121(3) 0.081(2) 0.073(2) 0.0200(18) 0.0133(19) 0.001(2) _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 La1 O8 2.472(2) . ? La1 O4 2.519(2) . ? La1 O5 2.520(2) 2_667 ? La1 O12 2.523(3) . ? La1 O10 2.535(3) . ? La1 O13 2.541(3) . ? La1 O11 2.593(3) . ? La1 O7 2.618(2) 2_667 ? La1 O8 2.700(2) 2_667 ? La1 C24 3.031(4) 2_667 ? La1 La1 4.2167(9) 2_667 ? S1 O1 1.426(3) . ? S1 O2 1.432(3) . ? S1 N1 1.601(3) . ? S1 C5 1.768(5) . ? C1 C2 1.494(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.369(7) . ? C2 C3 1.400(6) . ? C3 C4 1.355(6) . ? C3 H3 0.9300 . ? C4 C5 1.394(6) . ? C4 H4 0.9300 . ? C5 C6 1.363(5) . ? C6 C7 1.365(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.479(4) . ? C8 C17 1.522(5) . ? C8 C9 1.533(5) . ? C8 C25 1.542(5) . ? C9 O3 1.422(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.383(5) . ? C10 O3 1.387(4) . ? C10 C11 1.394(5) . ? C11 C12 1.381(6) . ? C11 H11 0.9300 . ? C12 C13 1.373(6) . ? C12 H12 0.9300 . ? C13 C14 1.393(5) . ? C13 H13 0.9300 . ? C14 C15 1.379(5) . ? C14 H14 0.9300 . ? C15 C16 1.495(5) . ? C16 O4 1.247(4) . ? C16 O5 1.258(4) . ? C17 O6 1.447(4) . ? C17 H17C 0.9700 . ? C17 H17D 0.9700 . ? C18 C19 1.367(5) . ? C18 O6 1.372(4) . ? C18 C23 1.386(5) . ? C19 C20 1.377(6) . ? C19 H19 0.9300 . ? C20 C21 1.384(6) . ? C20 H20 0.9300 . ? C21 C22 1.383(6) . ? C21 H21 0.9300 . ? C22 C23 1.389(5) . ? C22 H22 0.9300 . ? C23 C24 1.494(5) . ? C24 O7 1.236(4) . ? C24 O8 1.272(4) . ? C24 La1 3.031(4) 2_667 ? C25 O9 1.423(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O9 1.367(5) . ? C26 C31 1.375(5) . ? C26 C27 1.380(6) . ? C27 C28 1.357(6) . ? C27 H27 0.9300 . ? C28 C29 1.371(7) . ? C28 H28 0.9300 . ? C29 C30 1.384(7) . ? C29 H29 0.9300 . ? C30 C31 1.386(6) . ? C30 H30 0.9300 . ? C31 C32 1.511(5) . ? C32 O10 1.258(4) . ? C32 O11 1.269(5) . ? C33 O12 1.204(6) . ? C33 N3 1.308(5) . ? C33 H33 0.9300 . ? C34 N3 1.456(8) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N3 1.442(8) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O13 1.233(5) . ? C36 N2 1.283(5) . ? C36 H36 0.9300 . ? C37 N2 1.454(7) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 N2 1.405(7) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 O14 1.234(5) . ? C39 N4 1.296(5) . ? C39 H39 0.9300 . ? C40 N4 1.450(6) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 N4 1.429(6) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? N1 H1 0.8600 . ? O5 La1 2.520(2) 2_667 ? O7 La1 2.618(2) 2_667 ? O8 La1 2.700(2) 2_667 ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P-1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.005 -0.008 1147 314 ' ' _platon_squeeze_details ; ; 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 O8 La1 O4 78.95(8) . . ? O8 La1 O5 69.39(7) . 2_667 ? O4 La1 O5 131.64(8) . 2_667 ? O8 La1 O12 148.06(8) . . ? O4 La1 O12 75.02(9) . . ? O5 La1 O12 142.54(8) 2_667 . ? O8 La1 O10 75.82(8) . . ? O4 La1 O10 69.93(8) . . ? O5 La1 O10 131.30(8) 2_667 . ? O12 La1 O10 78.07(9) . . ? O8 La1 O13 135.47(8) . . ? O4 La1 O13 145.03(8) . . ? O5 La1 O13 71.46(8) 2_667 . ? O12 La1 O13 73.80(9) . . ? O10 La1 O13 117.78(9) . . ? O8 La1 O11 85.03(8) . . ? O4 La1 O11 120.68(9) . . ? O5 La1 O11 92.51(9) 2_667 . ? O12 La1 O11 92.53(10) . . ? O10 La1 O11 50.77(9) . . ? O13 La1 O11 76.27(9) . . ? O8 La1 O7 119.27(7) . 2_667 ? O4 La1 O7 79.85(8) . 2_667 ? O5 La1 O7 84.78(8) 2_667 2_667 ? O12 La1 O7 73.94(9) . 2_667 ? O10 La1 O7 143.08(8) . 2_667 ? O13 La1 O7 76.68(9) . 2_667 ? O11 La1 O7 152.23(8) . 2_667 ? O8 La1 O8 70.85(8) . 2_667 ? O4 La1 O8 65.66(7) . 2_667 ? O5 La1 O8 69.81(8) 2_667 2_667 ? O12 La1 O8 113.37(9) . 2_667 ? O10 La1 O8 128.20(8) . 2_667 ? O13 La1 O8 113.83(8) . 2_667 ? O11 La1 O8 153.76(8) . 2_667 ? O7 La1 O8 48.56(7) 2_667 2_667 ? O8 La1 C24 95.63(9) . 2_667 ? O4 La1 C24 69.85(8) . 2_667 ? O5 La1 C24 77.76(8) 2_667 2_667 ? O12 La1 C24 92.52(10) . 2_667 ? O10 La1 C24 139.77(9) . 2_667 ? O13 La1 C24 96.08(9) . 2_667 ? O11 La1 C24 169.25(9) . 2_667 ? O7 La1 C24 23.87(8) 2_667 2_667 ? O8 La1 C24 24.78(8) 2_667 2_667 ? O8 La1 La1 37.22(5) . 2_667 ? O4 La1 La1 67.90(5) . 2_667 ? O5 La1 La1 64.70(5) 2_667 2_667 ? O12 La1 La1 138.71(7) . 2_667 ? O10 La1 La1 104.62(6) . 2_667 ? O13 La1 La1 132.58(7) . 2_667 ? O11 La1 La1 121.57(6) . 2_667 ? O7 La1 La1 82.12(5) 2_667 2_667 ? O8 La1 La1 33.63(5) 2_667 2_667 ? C24 La1 La1 58.41(7) 2_667 2_667 ? O1 S1 O2 120.1(2) . . ? O1 S1 N1 109.19(18) . . ? O2 S1 N1 105.07(17) . . ? O1 S1 C5 106.3(2) . . ? O2 S1 C5 106.5(2) . . ? N1 S1 C5 109.37(18) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 117.1(5) . . ? C7 C2 C1 122.6(5) . . ? C3 C2 C1 120.2(5) . . ? C4 C3 C2 121.3(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 118.7(4) . . ? C6 C5 S1 121.8(4) . . ? C4 C5 S1 119.5(3) . . ? C5 C6 C7 120.7(4) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 121.9(4) . . ? C6 C7 H7 119.1 . . ? C2 C7 H7 119.1 . . ? N1 C8 C17 107.2(3) . . ? N1 C8 C9 113.6(3) . . ? C17 C8 C9 107.2(3) . . ? N1 C8 C25 109.7(3) . . ? C17 C8 C25 109.0(3) . . ? C9 C8 C25 109.9(3) . . ? O3 C9 C8 109.1(3) . . ? O3 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? O3 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C15 C10 O3 120.7(3) . . ? C15 C10 C11 120.4(3) . . ? O3 C10 C11 118.8(3) . . ? C12 C11 C10 119.8(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 120.4(4) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.3(4) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 121.2(4) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 118.8(3) . . ? C14 C15 C16 119.7(3) . . ? C10 C15 C16 121.5(3) . . ? O4 C16 O5 125.7(3) . . ? O4 C16 C15 117.2(3) . . ? O5 C16 C15 117.0(3) . . ? O6 C17 C8 109.7(3) . . ? O6 C17 H17C 109.7 . . ? C8 C17 H17C 109.7 . . ? O6 C17 H17D 109.7 . . ? C8 C17 H17D 109.7 . . ? H17C C17 H17D 108.2 . . ? C19 C18 O6 116.7(4) . . ? C19 C18 C23 121.2(4) . . ? O6 C18 C23 122.0(3) . . ? C18 C19 C20 119.8(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C21 120.6(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 C20 118.9(4) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 121.2(4) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C18 C23 C22 118.2(3) . . ? C18 C23 C24 122.5(3) . . ? C22 C23 C24 119.1(3) . . ? O7 C24 O8 121.5(3) . . ? O7 C24 C23 120.3(3) . . ? O8 C24 C23 118.1(3) . . ? O7 C24 La1 58.97(18) . 2_667 ? O8 C24 La1 62.87(18) . 2_667 ? C23 C24 La1 171.5(2) . 2_667 ? O9 C25 C8 105.9(3) . . ? O9 C25 H25A 110.5 . . ? C8 C25 H25A 110.5 . . ? O9 C25 H25B 110.5 . . ? C8 C25 H25B 110.5 . . ? H25A C25 H25B 108.7 . . ? O9 C26 C31 117.7(4) . . ? O9 C26 C27 121.6(4) . . ? C31 C26 C27 120.7(4) . . ? C28 C27 C26 120.9(5) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.3(5) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C30 118.5(5) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C29 C30 C31 122.4(5) . . ? C29 C30 H30 118.8 . . ? C31 C30 H30 118.8 . . ? C26 C31 C30 117.2(4) . . ? C26 C31 C32 124.3(4) . . ? C30 C31 C32 118.5(4) . . ? O10 C32 O11 121.0(4) . . ? O10 C32 C31 119.5(4) . . ? O11 C32 C31 119.5(4) . . ? O12 C33 N3 127.3(6) . . ? O12 C33 H33 116.4 . . ? N3 C33 H33 116.4 . . ? N3 C34 H34A 109.5 . . ? N3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O13 C36 N2 125.4(4) . . ? O13 C36 H36 117.3 . . ? N2 C36 H36 117.3 . . ? N2 C37 H37A 111.0 . . ? N2 C37 H37B 108.5 . . ? H37A C37 H37B 109.5 . . ? N2 C37 H37C 109.0 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N2 C38 H38A 109.3 . . ? N2 C38 H38B 109.3 . . ? H38A C38 H38B 109.5 . . ? N2 C38 H38C 109.9 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O14 C39 N4 125.7(5) . . ? O14 C39 H39 117.1 . . ? N4 C39 H39 117.1 . . ? N4 C40 H40A 109.5 . . ? N4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C8 N1 S1 127.2(2) . . ? C8 N1 H1 116.4 . . ? S1 N1 H1 116.4 . . ? C36 N2 C38 122.1(5) . . ? C36 N2 C37 122.2(5) . . ? C38 N2 C37 115.7(5) . . ? C33 N3 C35 119.7(6) . . ? C33 N3 C34 125.6(7) . . ? C35 N3 C34 114.6(5) . . ? C39 N4 C41 121.6(5) . . ? C39 N4 C40 120.8(5) . . ? C41 N4 C40 117.5(4) . . ? C10 O3 C9 114.4(3) . . ? C16 O4 La1 136.3(2) . . ? C16 O5 La1 141.9(2) . 2_667 ? C18 O6 C17 118.4(2) . . ? C24 O7 La1 97.2(2) . 2_667 ? C24 O8 La1 158.5(2) . . ? C24 O8 La1 92.3(2) . 2_667 ? La1 O8 La1 109.15(8) . 2_667 ? C26 O9 C25 119.9(3) . . ? C32 O10 La1 95.4(2) . . ? C32 O11 La1 92.4(2) . . ? C33 O12 La1 130.8(3) . . ? C36 O13 La1 132.1(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.648 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.062 #==END data_2 #TrackingRef 'complexes.cif' _database_code_depnum_ccdc_archive 'CCDC 731523' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H94 Eu2 N8 O28 S2' _chemical_formula_weight 2007.69 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 12.638(2) _cell_length_b 13.316(2) _cell_length_c 15.053(3) _cell_angle_alpha 82.070(10) _cell_angle_beta 66.800(10) _cell_angle_gamma 72.550(10) _cell_volume 2220.7(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 15.86 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.528 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7739 _exptl_absorpt_correction_T_max 0.9002 _exptl_absorpt_process_details 'SADABS (Sheldrick,1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.81 _diffrn_reflns_number 8455 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7798 _reflns_number_gt 6853 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0377P)^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 0.00063(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7798 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.003 _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 Eu Eu 0.824999(13) 0.528142(12) 0.591142(10) 0.02472(6) Uani 1 1 d . . . S S 1.24556(8) 0.17127(7) 0.92367(6) 0.0433(2) Uani 1 1 d . . . O1 O 1.1389(2) 0.1556(2) 0.99843(18) 0.0590(7) Uani 1 1 d . . . O2 O 1.3548(2) 0.0891(2) 0.9040(2) 0.0573(7) Uani 1 1 d . . . O3 O 1.1629(2) 0.42458(17) 0.76745(15) 0.0374(5) Uani 1 1 d . . . O4 O 0.94676(18) 0.58045(17) 0.65776(14) 0.0338(5) Uani 1 1 d . . . O5 O 1.14201(19) 0.51956(17) 0.56956(15) 0.0365(5) Uani 1 1 d . . . O6 O 1.1643(2) 0.15260(16) 0.66674(16) 0.0422(6) Uani 1 1 d . . . O7 O 1.00604(18) 0.39177(15) 0.53792(14) 0.0310(5) Uani 1 1 d . . . O8 O 1.18811(19) 0.28913(16) 0.47790(16) 0.0390(5) Uani 1 1 d . . . O9 O 0.9200(2) 0.26236(18) 0.83033(19) 0.0485(6) Uani 1 1 d . . . O10 O 0.8272(2) 0.42214(17) 0.73551(15) 0.0384(5) Uani 1 1 d . . . O11 O 0.7340(2) 0.38192(18) 0.65543(17) 0.0429(6) Uani 1 1 d . . . O12 O 0.63120(19) 0.58613(18) 0.57173(17) 0.0426(6) Uani 1 1 d . . . O13 O 0.6808(2) 0.64286(18) 0.72398(16) 0.0433(6) Uani 1 1 d . . . O14 O 1.4471(3) 0.1265(2) 0.6680(2) 0.0752(9) Uani 1 1 d . . . N1 N 1.2256(2) 0.1947(2) 0.82273(19) 0.0360(6) Uani 1 1 d . . . H1 H 1.2856 0.1671 0.7725 0.043 Uiso 1 1 calc R . . N2 N 0.4922(3) 0.6328(3) 0.5042(3) 0.0658(10) Uani 1 1 d . . . N3 N 0.6001(3) 0.7842(3) 0.8193(2) 0.0628(10) Uani 1 1 d . . . N4 N 1.5384(3) -0.0379(3) 0.6097(3) 0.0654(10) Uani 1 1 d . . . C1 C 1.3427(5) 0.5507(4) 1.0214(4) 0.0959(18) Uani 1 1 d . . . H1A H 1.2705 0.6070 1.0360 0.115 Uiso 1 1 calc R . . H1B H 1.4049 0.5707 0.9666 0.115 Uiso 1 1 calc R . . H1C H 1.3664 0.5362 1.0761 0.115 Uiso 1 1 calc R . . C2 C 1.3217(4) 0.4543(3) 0.9985(3) 0.0600(11) Uani 1 1 d . . . C3 C 1.2297(4) 0.4151(4) 1.0623(3) 0.0623(12) Uani 1 1 d . . . H3 H 1.1843 0.4463 1.1221 0.075 Uiso 1 1 calc R . . C4 C 1.2028(3) 0.3314(3) 1.0403(3) 0.0552(11) Uani 1 1 d . . . H4 H 1.1390 0.3073 1.0839 0.066 Uiso 1 1 calc R . . C5 C 1.2720(3) 0.2834(3) 0.9522(2) 0.0431(9) Uani 1 1 d . . . C6 C 1.3658(3) 0.3193(3) 0.8878(3) 0.0504(10) Uani 1 1 d . . . H6 H 1.4123 0.2866 0.8289 0.061 Uiso 1 1 calc R . . C7 C 1.3911(4) 0.4040(4) 0.9106(3) 0.0615(11) Uani 1 1 d . . . H7 H 1.4551 0.4279 0.8669 0.074 Uiso 1 1 calc R . . C8 C 1.1169(3) 0.2578(2) 0.8059(2) 0.0324(7) Uani 1 1 d . . . C9 C 1.0776(3) 0.3727(2) 0.8341(2) 0.0338(7) Uani 1 1 d . . . H9A H 0.9991 0.4065 0.8321 0.041 Uiso 1 1 calc R . . H9B H 1.0732 0.3769 0.8994 0.041 Uiso 1 1 calc R . . C10 C 1.1323(3) 0.5325(2) 0.7788(2) 0.0328(7) Uani 1 1 d . . . C11 C 1.1527(3) 0.5712(3) 0.8492(3) 0.0503(10) Uani 1 1 d . . . H11 H 1.1821 0.5250 0.8915 0.060 Uiso 1 1 calc R . . C12 C 1.1297(4) 0.6779(3) 0.8569(3) 0.0560(10) Uani 1 1 d . . . H12 H 1.1466 0.7035 0.9028 0.067 Uiso 1 1 calc R . . C13 C 1.0819(4) 0.7467(3) 0.7974(3) 0.0501(9) Uani 1 1 d . . . H13 H 1.0652 0.8189 0.8034 0.060 Uiso 1 1 calc R . . C14 C 1.0589(3) 0.7080(3) 0.7286(2) 0.0413(8) Uani 1 1 d . . . H14 H 1.0258 0.7549 0.6887 0.050 Uiso 1 1 calc R . . C15 C 1.0839(3) 0.6008(2) 0.7177(2) 0.0282(6) Uani 1 1 d . . . C16 C 1.0552(3) 0.5627(2) 0.6419(2) 0.0288(7) Uani 1 1 d . . . C17 C 1.1461(3) 0.2567(2) 0.6972(2) 0.0365(8) Uani 1 1 d . . . H17A H 1.0810 0.3054 0.6818 0.044 Uiso 1 1 calc R . . H17B H 1.2177 0.2799 0.6622 0.044 Uiso 1 1 calc R . . C18 C 1.0817(3) 0.1372(2) 0.6360(2) 0.0348(7) Uani 1 1 d . . . C19 C 1.0449(4) 0.0461(3) 0.6685(3) 0.0521(10) Uani 1 1 d . . . H19 H 1.0767 -0.0016 0.7088 0.063 Uiso 1 1 calc R . . C20 C 0.9612(4) 0.0262(3) 0.6413(3) 0.0654(12) Uani 1 1 d . . . H20 H 0.9376 -0.0354 0.6626 0.078 Uiso 1 1 calc R . . C21 C 0.9125(4) 0.0964(3) 0.5831(3) 0.0584(11) Uani 1 1 d . . . H21 H 0.8549 0.0832 0.5660 0.070 Uiso 1 1 calc R . . C22 C 0.9489(3) 0.1860(3) 0.5501(3) 0.0436(8) Uani 1 1 d . . . H22 H 0.9149 0.2335 0.5109 0.052 Uiso 1 1 calc R . . C23 C 1.0356(3) 0.2080(2) 0.5737(2) 0.0307(7) Uani 1 1 d . . . C24 C 1.0799(3) 0.3015(2) 0.5278(2) 0.0282(7) Uani 1 1 d . . . C25 C 1.0149(3) 0.2065(3) 0.8613(2) 0.0380(8) Uani 1 1 d . . . H25A H 1.0395 0.1326 0.8461 0.046 Uiso 1 1 calc R . . H25B H 0.9904 0.2126 0.9304 0.046 Uiso 1 1 calc R . . C26 C 0.8315(3) 0.2186(3) 0.8399(2) 0.0367(8) Uani 1 1 d . . . C27 C 0.8109(3) 0.1309(3) 0.8978(2) 0.0443(9) Uani 1 1 d . . . H27 H 0.8581 0.0994 0.9337 0.053 Uiso 1 1 calc R . . C28 C 0.7209(4) 0.0900(3) 0.9025(3) 0.0558(10) Uani 1 1 d . . . H28 H 0.7066 0.0318 0.9425 0.067 Uiso 1 1 calc R . . C29 C 0.6520(3) 0.1345(3) 0.8483(3) 0.0565(11) Uani 1 1 d . . . H29 H 0.5915 0.1066 0.8512 0.068 Uiso 1 1 calc R . . C30 C 0.6735(3) 0.2206(3) 0.7901(3) 0.0418(8) Uani 1 1 d . . . H30 H 0.6278 0.2498 0.7526 0.050 Uiso 1 1 calc R . . C31 C 0.7611(3) 0.2653(2) 0.7853(2) 0.0315(7) Uani 1 1 d . . . C32 C 0.7752(3) 0.3621(2) 0.7227(2) 0.0313(7) Uani 1 1 d . . . C33 C 0.6022(3) 0.6046(3) 0.5022(3) 0.0469(9) Uani 1 1 d . . . H33 H 0.6635 0.5982 0.4416 0.056 Uiso 1 1 calc R . . C34 C 0.4684(6) 0.6541(4) 0.4155(5) 0.121(3) Uani 1 1 d . . . H34A H 0.5424 0.6359 0.3609 0.145 Uiso 1 1 calc R . . H34B H 0.4294 0.7275 0.4112 0.145 Uiso 1 1 calc R . . H34C H 0.4176 0.6129 0.4157 0.145 Uiso 1 1 calc R . . C35 C 0.3939(4) 0.6442(5) 0.5935(5) 0.120(2) Uani 1 1 d . . . H35A H 0.4218 0.6140 0.6446 0.144 Uiso 1 1 calc R . . H35B H 0.3390 0.6088 0.5915 0.144 Uiso 1 1 calc R . . H35C H 0.3541 0.7176 0.6051 0.144 Uiso 1 1 calc R . . C36 C 0.6879(4) 0.7193(3) 0.7553(3) 0.0529(10) Uani 1 1 d . . . H36 H 0.7624 0.7327 0.7317 0.063 Uiso 1 1 calc R . . C37 C 0.6143(6) 0.8731(4) 0.8536(5) 0.117(2) Uani 1 1 d . . . H37A H 0.6950 0.8777 0.8207 0.141 Uiso 1 1 calc R . . H37B H 0.5968 0.8646 0.9219 0.141 Uiso 1 1 calc R . . H37C H 0.5604 0.9364 0.8412 0.141 Uiso 1 1 calc R . . C38 C 0.4843(5) 0.7669(5) 0.8600(5) 0.124(2) Uani 1 1 d . . . H38A H 0.4849 0.7068 0.8309 0.148 Uiso 1 1 calc R . . H38B H 0.4272 0.8279 0.8480 0.148 Uiso 1 1 calc R . . H38C H 0.4626 0.7543 0.9284 0.148 Uiso 1 1 calc R . . C39 C 1.4454(4) 0.0375(4) 0.6553(3) 0.0701(13) Uani 1 1 d . . . H39 H 1.3715 0.0228 0.6805 0.084 Uiso 1 1 calc R . . C40 C 1.6562(4) -0.0230(5) 0.5710(5) 0.110(2) Uani 1 1 d . . . H40A H 1.6852 -0.0217 0.5017 0.132 Uiso 1 1 calc R . . H40B H 1.7087 -0.0798 0.5928 0.132 Uiso 1 1 calc R . . H40C H 1.6536 0.0425 0.5928 0.132 Uiso 1 1 calc R . . C41 C 1.5273(5) -0.1386(4) 0.5925(4) 0.0925(17) Uani 1 1 d . . . H41A H 1.4457 -0.1410 0.6250 0.111 Uiso 1 1 calc R . . H41B H 1.5778 -0.1947 0.6168 0.111 Uiso 1 1 calc R . . H41C H 1.5511 -0.1464 0.5243 0.111 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 Eu 0.02356(9) 0.02446(9) 0.02413(9) 0.00110(5) -0.01011(6) -0.00273(6) S 0.0392(5) 0.0492(5) 0.0384(5) 0.0117(4) -0.0216(4) -0.0037(4) O1 0.0525(16) 0.079(2) 0.0419(15) 0.0213(14) -0.0203(13) -0.0191(14) O2 0.0513(16) 0.0492(16) 0.0686(18) 0.0117(13) -0.0358(14) 0.0031(13) O3 0.0411(13) 0.0304(12) 0.0378(12) -0.0005(10) -0.0157(11) -0.0042(10) O4 0.0286(12) 0.0431(13) 0.0306(11) -0.0031(10) -0.0114(9) -0.0092(10) O5 0.0328(12) 0.0437(13) 0.0306(12) -0.0064(10) -0.0149(10) -0.0005(10) O6 0.0579(15) 0.0260(12) 0.0439(13) 0.0000(10) -0.0281(12) -0.0010(11) O7 0.0331(12) 0.0258(11) 0.0294(11) 0.0012(9) -0.0124(9) -0.0010(9) O8 0.0301(12) 0.0309(12) 0.0407(13) 0.0055(10) -0.0056(10) 0.0001(10) O9 0.0445(14) 0.0405(14) 0.0729(17) 0.0211(12) -0.0383(13) -0.0164(12) O10 0.0551(15) 0.0339(12) 0.0357(12) 0.0101(10) -0.0247(11) -0.0196(11) O11 0.0463(14) 0.0433(14) 0.0499(14) 0.0153(11) -0.0297(12) -0.0186(11) O12 0.0334(13) 0.0478(14) 0.0478(14) -0.0015(11) -0.0235(11) -0.0012(11) O13 0.0446(14) 0.0405(14) 0.0385(13) -0.0077(11) -0.0127(11) -0.0032(11) O14 0.0602(19) 0.061(2) 0.079(2) -0.0208(17) -0.0008(16) -0.0068(16) N1 0.0333(15) 0.0351(15) 0.0339(15) 0.0007(12) -0.0151(12) 0.0016(12) N2 0.053(2) 0.054(2) 0.113(3) 0.008(2) -0.056(2) -0.0158(17) N3 0.071(2) 0.051(2) 0.052(2) -0.0184(17) -0.0222(19) 0.0110(18) N4 0.059(2) 0.056(2) 0.067(2) -0.0128(18) -0.0215(19) 0.0061(18) C1 0.078(4) 0.098(4) 0.119(5) -0.055(4) -0.043(3) -0.002(3) C2 0.045(2) 0.071(3) 0.070(3) -0.028(2) -0.037(2) 0.008(2) C3 0.050(3) 0.084(3) 0.042(2) -0.018(2) -0.024(2) 0.013(2) C4 0.047(2) 0.074(3) 0.035(2) -0.0034(19) -0.0185(18) 0.002(2) C5 0.0342(19) 0.058(2) 0.0345(18) -0.0001(16) -0.0188(16) -0.0011(17) C6 0.040(2) 0.065(3) 0.044(2) -0.0193(19) -0.0154(18) -0.0045(19) C7 0.040(2) 0.081(3) 0.062(3) -0.016(2) -0.018(2) -0.010(2) C8 0.0324(17) 0.0329(17) 0.0315(16) 0.0022(13) -0.0161(14) -0.0041(14) C9 0.0332(17) 0.0326(17) 0.0334(17) 0.0017(14) -0.0161(14) -0.0019(14) C10 0.0328(17) 0.0308(17) 0.0350(17) -0.0019(14) -0.0148(14) -0.0052(14) C11 0.062(2) 0.055(2) 0.047(2) -0.0043(18) -0.038(2) -0.0079(19) C12 0.070(3) 0.060(3) 0.055(2) -0.015(2) -0.032(2) -0.023(2) C13 0.064(3) 0.035(2) 0.055(2) -0.0082(17) -0.020(2) -0.0182(18) C14 0.049(2) 0.0321(18) 0.0409(19) -0.0020(15) -0.0178(17) -0.0066(16) C15 0.0261(15) 0.0316(17) 0.0261(15) -0.0012(13) -0.0080(13) -0.0085(13) C16 0.0322(18) 0.0263(16) 0.0264(16) 0.0022(13) -0.0126(14) -0.0048(13) C17 0.051(2) 0.0293(17) 0.0337(17) 0.0050(14) -0.0235(16) -0.0091(15) C18 0.0433(19) 0.0232(16) 0.0300(17) -0.0014(13) -0.0088(15) -0.0041(14) C19 0.076(3) 0.0273(18) 0.046(2) 0.0030(16) -0.017(2) -0.0124(19) C20 0.082(3) 0.041(2) 0.067(3) -0.006(2) -0.009(2) -0.032(2) C21 0.053(2) 0.057(3) 0.068(3) -0.022(2) -0.010(2) -0.026(2) C22 0.043(2) 0.041(2) 0.045(2) -0.0113(16) -0.0146(17) -0.0069(16) C23 0.0318(17) 0.0270(16) 0.0275(16) -0.0043(13) -0.0066(13) -0.0041(13) C24 0.0344(18) 0.0274(16) 0.0208(15) -0.0013(12) -0.0124(13) -0.0026(14) C25 0.0391(19) 0.0387(19) 0.0379(18) 0.0077(15) -0.0218(16) -0.0063(15) C26 0.0352(18) 0.0324(18) 0.0374(18) 0.0036(14) -0.0109(15) -0.0073(15) C27 0.046(2) 0.042(2) 0.041(2) 0.0151(16) -0.0171(17) -0.0117(17) C28 0.058(3) 0.041(2) 0.062(3) 0.0201(19) -0.018(2) -0.0199(19) C29 0.048(2) 0.045(2) 0.077(3) 0.014(2) -0.020(2) -0.0241(19) C30 0.0359(19) 0.041(2) 0.049(2) 0.0084(16) -0.0180(16) -0.0134(16) C31 0.0271(16) 0.0290(16) 0.0328(17) 0.0018(13) -0.0075(13) -0.0062(13) C32 0.0286(16) 0.0296(17) 0.0299(16) 0.0016(13) -0.0083(14) -0.0045(14) C33 0.046(2) 0.041(2) 0.066(2) 0.0077(18) -0.032(2) -0.0173(17) C34 0.161(6) 0.088(4) 0.199(7) 0.053(4) -0.160(6) -0.051(4) C35 0.042(3) 0.113(5) 0.189(7) -0.039(5) -0.026(4) -0.007(3) C36 0.056(2) 0.046(2) 0.051(2) -0.0023(19) -0.026(2) 0.0024(19) C37 0.155(6) 0.063(3) 0.147(6) -0.049(4) -0.093(5) 0.022(4) C38 0.091(5) 0.120(5) 0.107(5) -0.043(4) 0.015(4) -0.008(4) C39 0.052(3) 0.067(3) 0.074(3) -0.009(3) -0.015(2) 0.000(2) C40 0.057(3) 0.097(4) 0.136(5) -0.029(4) -0.002(3) 0.002(3) C41 0.114(5) 0.054(3) 0.108(4) -0.016(3) -0.058(4) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu O7 2.375(2) . ? Eu O10 2.428(2) . ? Eu O5 2.429(2) 2_766 ? Eu O4 2.431(2) . ? Eu O13 2.440(2) . ? Eu O11 2.449(2) . ? Eu O12 2.459(2) . ? Eu O8 2.495(2) 2_766 ? Eu O7 2.645(2) 2_766 ? Eu C32 2.802(3) . ? Eu C24 2.935(3) 2_766 ? Eu Eu 4.0833(8) 2_766 ? S O1 1.427(3) . ? S O2 1.432(3) . ? S N1 1.610(3) . ? S C5 1.765(4) . ? O3 C10 1.388(4) . ? O3 C9 1.432(4) . ? O4 C16 1.247(4) . ? O5 C16 1.253(3) . ? O5 Eu 2.429(2) 2_766 ? O6 C18 1.371(4) . ? O6 C17 1.444(4) . ? O7 C24 1.267(3) . ? O7 Eu 2.645(2) 2_766 ? O8 C24 1.245(4) . ? O8 Eu 2.495(2) 2_766 ? O9 C26 1.362(4) . ? O9 C25 1.420(4) . ? O10 C32 1.251(4) . ? O11 C32 1.276(4) . ? O12 C33 1.211(4) . ? O13 C36 1.219(4) . ? O14 C39 1.234(5) . ? N1 C8 1.477(4) . ? N2 C33 1.316(5) . ? N2 C35 1.414(7) . ? N2 C34 1.455(6) . ? N3 C36 1.311(5) . ? N3 C38 1.424(7) . ? N3 C37 1.439(6) . ? N4 C39 1.307(5) . ? N4 C40 1.435(6) . ? N4 C41 1.455(6) . ? C1 C2 1.495(6) . ? C2 C3 1.375(6) . ? C2 C7 1.395(5) . ? C3 C4 1.373(6) . ? C4 C5 1.384(5) . ? C5 C6 1.371(5) . ? C6 C7 1.379(5) . ? C8 C9 1.525(4) . ? C8 C17 1.531(4) . ? C8 C25 1.532(4) . ? C10 C11 1.379(4) . ? C10 C15 1.387(4) . ? C11 C12 1.374(5) . ? C12 C13 1.368(5) . ? C13 C14 1.377(5) . ? C14 C15 1.385(4) . ? C15 C16 1.513(4) . ? C18 C19 1.386(5) . ? C18 C23 1.402(4) . ? C19 C20 1.377(6) . ? C20 C21 1.369(6) . ? C21 C22 1.367(5) . ? C22 C23 1.393(5) . ? C23 C24 1.489(4) . ? C24 Eu 2.935(3) 2_766 ? C26 C27 1.384(4) . ? C26 C31 1.398(4) . ? C27 C28 1.376(5) . ? C28 C29 1.375(5) . ? C29 C30 1.370(5) . ? C30 C31 1.380(4) . ? C31 C32 1.501(4) . ? 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 Eu O10 75.29(7) . . ? O7 Eu O5 72.37(7) . 2_766 ? O10 Eu O5 131.66(7) . 2_766 ? O7 Eu O4 78.18(7) . . ? O10 Eu O4 70.85(7) . . ? O5 Eu O4 133.37(7) 2_766 . ? O7 Eu O13 145.88(7) . . ? O10 Eu O13 75.80(8) . . ? O5 Eu O13 141.66(8) 2_766 . ? O4 Eu O13 75.50(8) . . ? O7 Eu O11 83.81(8) . . ? O10 Eu O11 53.41(7) . . ? O5 Eu O11 87.96(8) 2_766 . ? O4 Eu O11 124.11(7) . . ? O13 Eu O11 93.26(8) . . ? O7 Eu O12 139.05(8) . . ? O10 Eu O12 115.41(8) . . ? O5 Eu O12 72.34(7) 2_766 . ? O4 Eu O12 142.54(7) . . ? O13 Eu O12 71.07(8) . . ? O11 Eu O12 74.84(8) . . ? O7 Eu O8 121.53(7) . 2_766 ? O10 Eu O8 142.87(8) . 2_766 ? O5 Eu O8 85.25(8) 2_766 2_766 ? O4 Eu O8 80.25(7) . 2_766 ? O13 Eu O8 74.74(8) . 2_766 ? O11 Eu O8 149.86(7) . 2_766 ? O12 Eu O8 75.12(8) . 2_766 ? O7 Eu O7 71.26(7) . 2_766 ? O10 Eu O7 129.19(7) . 2_766 ? O5 Eu O7 70.93(7) 2_766 2_766 ? O4 Eu O7 65.71(7) . 2_766 ? O13 Eu O7 115.61(7) . 2_766 ? O11 Eu O7 151.06(7) . 2_766 ? O12 Eu O7 115.00(7) . 2_766 ? O8 Eu O7 50.33(6) 2_766 2_766 ? O7 Eu C32 76.57(8) . . ? O10 Eu C32 26.45(8) . . ? O5 Eu C32 109.91(9) 2_766 . ? O4 Eu C32 97.05(8) . . ? O13 Eu C32 85.47(8) . . ? O11 Eu C32 27.06(8) . . ? O12 Eu C32 96.71(9) . . ? O8 Eu C32 160.09(8) 2_766 . ? O7 Eu C32 145.86(8) 2_766 . ? O7 Eu C24 96.83(8) . 2_766 ? O10 Eu C24 140.68(8) . 2_766 ? O5 Eu C24 78.61(8) 2_766 2_766 ? O4 Eu C24 69.82(8) . 2_766 ? O13 Eu C24 94.12(8) . 2_766 ? O11 Eu C24 165.61(8) . 2_766 ? O12 Eu C24 95.95(8) . 2_766 ? O8 Eu C24 24.86(7) 2_766 2_766 ? O7 Eu C24 25.57(7) 2_766 2_766 ? C32 Eu C24 166.45(8) . 2_766 ? O7 Eu Eu 37.84(5) . 2_766 ? O10 Eu Eu 105.17(6) . 2_766 ? O5 Eu Eu 67.18(5) 2_766 2_766 ? O4 Eu Eu 67.32(5) . 2_766 ? O13 Eu Eu 139.59(6) . 2_766 ? O11 Eu Eu 120.28(6) . 2_766 ? O12 Eu Eu 135.48(6) . 2_766 ? O8 Eu Eu 83.72(5) 2_766 2_766 ? O7 Eu Eu 33.42(4) 2_766 2_766 ? C32 Eu Eu 113.65(6) . 2_766 ? C24 Eu Eu 58.99(6) 2_766 2_766 ? O1 S O2 119.35(16) . . ? O1 S N1 109.25(15) . . ? O2 S N1 105.25(15) . . ? O1 S C5 107.67(17) . . ? O2 S C5 106.61(17) . . ? N1 S C5 108.26(15) . . ? C10 O3 C9 114.7(2) . . ? C16 O4 Eu 137.14(19) . . ? C16 O5 Eu 137.28(19) . 2_766 ? C18 O6 C17 117.8(2) . . ? C24 O7 Eu 161.1(2) . . ? C24 O7 Eu 90.10(17) . 2_766 ? Eu O7 Eu 108.74(7) . 2_766 ? C24 O8 Eu 97.75(18) . 2_766 ? C26 O9 C25 120.8(2) . . ? C32 O10 Eu 93.70(18) . . ? C32 O11 Eu 92.07(18) . . ? C33 O12 Eu 133.7(2) . . ? C36 O13 Eu 130.5(3) . . ? C8 N1 S 127.9(2) . . ? C33 N2 C35 120.3(4) . . ? C33 N2 C34 121.2(5) . . ? C35 N2 C34 118.4(4) . . ? C36 N3 C38 119.9(4) . . ? C36 N3 C37 123.3(5) . . ? C38 N3 C37 116.7(4) . . ? C39 N4 C40 120.8(4) . . ? C39 N4 C41 122.1(4) . . ? C40 N4 C41 117.1(4) . . ? C3 C2 C7 118.0(4) . . ? C3 C2 C1 120.7(4) . . ? C7 C2 C1 121.2(5) . . ? C4 C3 C2 122.0(4) . . ? C3 C4 C5 119.1(4) . . ? C6 C5 C4 120.3(4) . . ? C6 C5 S 119.0(3) . . ? C4 C5 S 120.5(3) . . ? C5 C6 C7 119.9(4) . . ? C6 C7 C2 120.7(4) . . ? N1 C8 C9 114.1(3) . . ? N1 C8 C17 106.8(3) . . ? C9 C8 C17 107.3(2) . . ? N1 C8 C25 109.1(2) . . ? C9 C8 C25 109.6(3) . . ? C17 C8 C25 109.8(3) . . ? O3 C9 C8 108.5(2) . . ? C11 C10 C15 120.4(3) . . ? C11 C10 O3 119.8(3) . . ? C15 C10 O3 119.8(3) . . ? C12 C11 C10 120.1(3) . . ? C13 C12 C11 120.3(3) . . ? C12 C13 C14 119.4(3) . . ? C13 C14 C15 121.4(3) . . ? C14 C15 C10 118.2(3) . . ? C14 C15 C16 119.2(3) . . ? C10 C15 C16 122.6(3) . . ? O4 C16 O5 127.4(3) . . ? O4 C16 C15 115.6(3) . . ? O5 C16 C15 117.0(3) . . ? O6 C17 C8 111.2(2) . . ? O6 C18 C19 117.0(3) . . ? O6 C18 C23 123.0(3) . . ? C19 C18 C23 120.0(3) . . ? C20 C19 C18 120.0(4) . . ? C21 C20 C19 120.5(4) . . ? C22 C21 C20 119.8(4) . . ? C21 C22 C23 121.6(4) . . ? C22 C23 C18 117.9(3) . . ? C22 C23 C24 119.0(3) . . ? C18 C23 C24 123.0(3) . . ? O8 C24 O7 121.3(3) . . ? O8 C24 C23 119.4(3) . . ? O7 C24 C23 119.2(3) . . ? O8 C24 Eu 57.38(15) . 2_766 ? O7 C24 Eu 64.33(15) . 2_766 ? C23 C24 Eu 171.1(2) . 2_766 ? O9 C25 C8 105.5(2) . . ? O9 C26 C27 123.6(3) . . ? O9 C26 C31 116.6(3) . . ? C27 C26 C31 119.8(3) . . ? C28 C27 C26 120.3(3) . . ? C29 C28 C27 120.4(3) . . ? C30 C29 C28 119.1(4) . . ? C29 C30 C31 122.0(3) . . ? C30 C31 C26 118.2(3) . . ? C30 C31 C32 118.4(3) . . ? C26 C31 C32 123.3(3) . . ? O10 C32 O11 120.4(3) . . ? O10 C32 C31 120.9(3) . . ? O11 C32 C31 118.8(3) . . ? O10 C32 Eu 59.85(15) . . ? O11 C32 Eu 60.87(16) . . ? C31 C32 Eu 173.5(2) . . ? O12 C33 N2 126.2(4) . . ? O13 C36 N3 125.9(4) . . ? O14 C39 N4 125.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Eu O4 C16 20.9(3) . . . . ? O10 Eu O4 C16 99.2(3) . . . . ? O5 Eu O4 C16 -30.6(3) 2_766 . . . ? O13 Eu O4 C16 178.9(3) . . . . ? O11 Eu O4 C16 94.9(3) . . . . ? O12 Eu O4 C16 -153.7(3) . . . . ? O8 Eu O4 C16 -104.4(3) 2_766 . . . ? O7 Eu O4 C16 -53.7(3) 2_766 . . . ? C32 Eu O4 C16 95.5(3) . . . . ? C24 Eu O4 C16 -81.0(3) 2_766 . . . ? Eu Eu O4 C16 -17.2(3) 2_766 . . . ? O10 Eu O7 C24 42.0(6) . . . . ? O5 Eu O7 C24 -101.6(6) 2_766 . . . ? O4 Eu O7 C24 115.0(6) . . . . ? O13 Eu O7 C24 74.9(6) . . . . ? O11 Eu O7 C24 -11.8(6) . . . . ? O12 Eu O7 C24 -70.0(6) . . . . ? O8 Eu O7 C24 -174.3(6) 2_766 . . . ? O7 Eu O7 C24 -176.9(6) 2_766 . . . ? C32 Eu O7 C24 14.7(6) . . . . ? C24 Eu O7 C24 -177.3(5) 2_766 . . . ? Eu Eu O7 C24 -176.9(6) 2_766 . . . ? O10 Eu O7 Eu -141.16(9) . . . 2_766 ? O5 Eu O7 Eu 75.27(8) 2_766 . . 2_766 ? O4 Eu O7 Eu -68.11(8) . . . 2_766 ? O13 Eu O7 Eu -108.24(13) . . . 2_766 ? O11 Eu O7 Eu 165.09(9) . . . 2_766 ? O12 Eu O7 Eu 106.85(11) . . . 2_766 ? O8 Eu O7 Eu 2.54(11) 2_766 . . 2_766 ? O7 Eu O7 Eu 0.0 2_766 . . 2_766 ? C32 Eu O7 Eu -168.42(10) . . . 2_766 ? C24 Eu O7 Eu -0.44(9) 2_766 . . 2_766 ? O7 Eu O10 C32 -89.34(19) . . . . ? O5 Eu O10 C32 -40.1(2) 2_766 . . . ? O4 Eu O10 C32 -171.7(2) . . . . ? O13 Eu O10 C32 108.99(19) . . . . ? O11 Eu O10 C32 3.87(17) . . . . ? O12 Eu O10 C32 48.4(2) . . . . ? O8 Eu O10 C32 147.37(17) 2_766 . . . ? O7 Eu O10 C32 -139.36(17) 2_766 . . . ? C24 Eu O10 C32 -172.07(17) 2_766 . . . ? Eu Eu O10 C32 -112.83(18) 2_766 . . . ? O7 Eu O11 C32 72.47(18) . . . . ? O10 Eu O11 C32 -3.79(17) . . . . ? O5 Eu O11 C32 144.95(19) 2_766 . . . ? O4 Eu O11 C32 1.3(2) . . . . ? O13 Eu O11 C32 -73.41(19) . . . . ? O12 Eu O11 C32 -142.8(2) . . . . ? O8 Eu O11 C32 -138.13(18) 2_766 . . . ? O7 Eu O11 C32 102.7(2) 2_766 . . . ? C24 Eu O11 C32 165.8(3) 2_766 . . . ? Eu Eu O11 C32 83.00(19) 2_766 . . . ? O7 Eu O12 C33 -52.5(4) . . . . ? O10 Eu O12 C33 -149.3(3) . . . . ? O5 Eu O12 C33 -20.9(3) 2_766 . . . ? O4 Eu O12 C33 119.4(3) . . . . ? O13 Eu O12 C33 147.5(3) . . . . ? O11 Eu O12 C33 -113.6(3) . . . . ? O8 Eu O12 C33 68.8(3) 2_766 . . . ? O7 Eu O12 C33 37.3(3) 2_766 . . . ? C32 Eu O12 C33 -129.7(3) . . . . ? C24 Eu O12 C33 55.1(3) 2_766 . . . ? Eu Eu O12 C33 4.4(4) 2_766 . . . ? O7 Eu O13 C36 73.5(3) . . . . ? O10 Eu O13 C36 106.3(3) . . . . ? O5 Eu O13 C36 -111.9(3) 2_766 . . . ? O4 Eu O13 C36 32.8(3) . . . . ? O11 Eu O13 C36 157.3(3) . . . . ? O12 Eu O13 C36 -130.0(3) . . . . ? O8 Eu O13 C36 -50.8(3) 2_766 . . . ? O7 Eu O13 C36 -20.6(3) 2_766 . . . ? C32 Eu O13 C36 131.3(3) . . . . ? C24 Eu O13 C36 -35.1(3) 2_766 . . . ? Eu Eu O13 C36 9.5(3) 2_766 . . . ? O1 S N1 C8 38.5(3) . . . . ? O2 S N1 C8 167.8(3) . . . . ? C5 S N1 C8 -78.5(3) . . . . ? C7 C2 C3 C4 -2.2(6) . . . . ? C1 C2 C3 C4 175.2(4) . . . . ? C2 C3 C4 C5 1.5(6) . . . . ? C3 C4 C5 C6 -0.2(5) . . . . ? C3 C4 C5 S 176.7(3) . . . . ? O1 S C5 C6 -175.7(3) . . . . ? O2 S C5 C6 55.1(3) . . . . ? N1 S C5 C6 -57.7(3) . . . . ? O1 S C5 C4 7.3(3) . . . . ? O2 S C5 C4 -121.9(3) . . . . ? N1 S C5 C4 125.3(3) . . . . ? C4 C5 C6 C7 -0.3(6) . . . . ? S C5 C6 C7 -177.2(3) . . . . ? C5 C6 C7 C2 -0.4(6) . . . . ? C3 C2 C7 C6 1.6(6) . . . . ? C1 C2 C7 C6 -175.7(4) . . . . ? S N1 C8 C9 60.5(4) . . . . ? S N1 C8 C17 178.9(2) . . . . ? S N1 C8 C25 -62.4(4) . . . . ? C10 O3 C9 C8 174.0(2) . . . . ? N1 C8 C9 O3 69.6(3) . . . . ? C17 C8 C9 O3 -48.6(3) . . . . ? C25 C8 C9 O3 -167.7(2) . . . . ? C9 O3 C10 C11 81.1(4) . . . . ? C9 O3 C10 C15 -100.5(3) . . . . ? C15 C10 C11 C12 -2.6(6) . . . . ? O3 C10 C11 C12 175.9(3) . . . . ? C10 C11 C12 C13 2.6(6) . . . . ? C11 C12 C13 C14 -1.0(6) . . . . ? C12 C13 C14 C15 -0.6(6) . . . . ? C13 C14 C15 C10 0.6(5) . . . . ? C13 C14 C15 C16 179.2(3) . . . . ? C11 C10 C15 C14 1.0(5) . . . . ? O3 C10 C15 C14 -177.4(3) . . . . ? C11 C10 C15 C16 -177.6(3) . . . . ? O3 C10 C15 C16 4.0(4) . . . . ? Eu O4 C16 O5 12.6(5) . . . . ? Eu O4 C16 C15 -169.31(19) . . . . ? Eu O5 C16 O4 13.5(5) 2_766 . . . ? Eu O5 C16 C15 -164.5(2) 2_766 . . . ? C14 C15 C16 O4 -68.5(4) . . . . ? C10 C15 C16 O4 110.1(3) . . . . ? C14 C15 C16 O5 109.8(3) . . . . ? C10 C15 C16 O5 -71.6(4) . . . . ? C18 O6 C17 C8 112.3(3) . . . . ? N1 C8 C17 O6 67.2(3) . . . . ? C9 C8 C17 O6 -170.1(3) . . . . ? C25 C8 C17 O6 -51.0(3) . . . . ? C17 O6 C18 C19 -136.6(3) . . . . ? C17 O6 C18 C23 44.1(4) . . . . ? O6 C18 C19 C20 179.3(3) . . . . ? C23 C18 C19 C20 -1.4(5) . . . . ? C18 C19 C20 C21 -0.9(6) . . . . ? C19 C20 C21 C22 1.3(6) . . . . ? C20 C21 C22 C23 0.4(6) . . . . ? C21 C22 C23 C18 -2.6(5) . . . . ? C21 C22 C23 C24 174.1(3) . . . . ? O6 C18 C23 C22 -177.7(3) . . . . ? C19 C18 C23 C22 3.0(5) . . . . ? O6 C18 C23 C24 5.7(5) . . . . ? C19 C18 C23 C24 -173.6(3) . . . . ? Eu O8 C24 O7 -7.4(3) 2_766 . . . ? Eu O8 C24 C23 170.3(2) 2_766 . . . ? Eu O7 C24 O8 -176.0(4) . . . . ? Eu O7 C24 O8 6.9(3) 2_766 . . . ? Eu O7 C24 C23 6.3(8) . . . . ? Eu O7 C24 C23 -170.8(2) 2_766 . . . ? Eu O7 C24 Eu 177.0(6) . . . 2_766 ? C22 C23 C24 O8 -120.2(3) . . . . ? C18 C23 C24 O8 56.3(4) . . . . ? C22 C23 C24 O7 57.5(4) . . . . ? C18 C23 C24 O7 -125.9(3) . . . . ? C22 C23 C24 Eu -53.8(15) . . . 2_766 ? C18 C23 C24 Eu 122.8(13) . . . 2_766 ? C26 O9 C25 C8 158.7(3) . . . . ? N1 C8 C25 O9 -171.7(3) . . . . ? C9 C8 C25 O9 62.6(3) . . . . ? C17 C8 C25 O9 -55.0(3) . . . . ? C25 O9 C26 C27 15.1(5) . . . . ? C25 O9 C26 C31 -163.4(3) . . . . ? O9 C26 C27 C28 -178.9(3) . . . . ? C31 C26 C27 C28 -0.5(5) . . . . ? C26 C27 C28 C29 1.3(6) . . . . ? C27 C28 C29 C30 -0.4(6) . . . . ? C28 C29 C30 C31 -1.2(6) . . . . ? C29 C30 C31 C26 1.9(5) . . . . ? C29 C30 C31 C32 -177.5(3) . . . . ? O9 C26 C31 C30 177.4(3) . . . . ? C27 C26 C31 C30 -1.0(5) . . . . ? O9 C26 C31 C32 -3.2(5) . . . . ? C27 C26 C31 C32 178.4(3) . . . . ? Eu O10 C32 O11 -6.9(3) . . . . ? Eu O10 C32 C31 172.5(2) . . . . ? Eu O11 C32 O10 6.9(3) . . . . ? Eu O11 C32 C31 -172.6(2) . . . . ? C30 C31 C32 O10 159.9(3) . . . . ? C26 C31 C32 O10 -19.6(5) . . . . ? C30 C31 C32 O11 -20.7(4) . . . . ? C26 C31 C32 O11 159.9(3) . . . . ? C30 C31 C32 Eu -106(2) . . . . ? C26 C31 C32 Eu 75(2) . . . . ? O7 Eu C32 O10 83.91(18) . . . . ? O5 Eu C32 O10 149.22(17) 2_766 . . . ? O4 Eu C32 O10 7.90(19) . . . . ? O13 Eu C32 O10 -66.86(18) . . . . ? O11 Eu C32 O10 -173.2(3) . . . . ? O12 Eu C32 O10 -137.17(18) . . . . ? O8 Eu C32 O10 -72.9(3) 2_766 . . . ? O7 Eu C32 O10 64.1(2) 2_766 . . . ? C24 Eu C32 O10 21.9(5) 2_766 . . . ? Eu Eu C32 O10 76.18(18) 2_766 . . . ? O7 Eu C32 O11 -102.93(19) . . . . ? O10 Eu C32 O11 173.2(3) . . . . ? O5 Eu C32 O11 -37.6(2) 2_766 . . . ? O4 Eu C32 O11 -178.94(18) . . . . ? O13 Eu C32 O11 106.30(19) . . . . ? O12 Eu C32 O11 35.99(19) . . . . ? O8 Eu C32 O11 100.2(3) 2_766 . . . ? O7 Eu C32 O11 -122.74(19) 2_766 . . . ? C24 Eu C32 O11 -164.9(3) 2_766 . . . ? Eu Eu C32 O11 -110.66(17) 2_766 . . . ? O7 Eu C32 C31 -14(2) . . . . ? O10 Eu C32 C31 -98(2) . . . . ? O5 Eu C32 C31 51(2) 2_766 . . . ? O4 Eu C32 C31 -90(2) . . . . ? O13 Eu C32 C31 -165(2) . . . . ? O11 Eu C32 C31 89(2) . . . . ? O12 Eu C32 C31 125(2) . . . . ? O8 Eu C32 C31 -171.0(19) 2_766 . . . ? O7 Eu C32 C31 -34(2) 2_766 . . . ? C24 Eu C32 C31 -76(2) 2_766 . . . ? Eu Eu C32 C31 -22(2) 2_766 . . . ? Eu O12 C33 N2 178.0(3) . . . . ? C35 N2 C33 O12 0.0(6) . . . . ? C34 N2 C33 O12 179.3(4) . . . . ? Eu O13 C36 N3 170.8(3) . . . . ? C38 N3 C36 O13 1.3(7) . . . . ? C37 N3 C36 O13 179.9(4) . . . . ? C40 N4 C39 O14 1.9(8) . . . . ? C41 N4 C39 O14 -175.9(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O14 0.86 1.99 2.830(4) 163.7 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.673 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.067 #==END data_3 #TrackingRef 'complexes.cif' _database_code_depnum_ccdc_archive 'CCDC 731524' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H44 Gd N3 O15 S' _chemical_formula_weight 972.07 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' Gd Gd -0.1653 3.9035 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.592(8) _cell_length_b 13.836(7) _cell_length_c 19.690(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.599(8) _cell_angle_gamma 90.00 _cell_volume 4200(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3834 _cell_measurement_theta_min 2.143 _cell_measurement_theta_max 25.591 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 1.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5798 _exptl_absorpt_correction_T_max 0.6569 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21430 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7348 _reflns_number_gt 4522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.0243P)^2^+14.4573P] 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 7348 _refine_ls_number_parameters 520 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _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 Gd1 Gd 0.63385(2) 0.90098(3) 0.592537(17) 0.03543(12) Uani 1 1 d . . . C1 C 0.6955(4) 0.9250(5) 0.4658(3) 0.0384(17) Uani 1 1 d . . . C2 C 0.7164(4) 0.9243(5) 0.3935(3) 0.0396(18) Uani 1 1 d . . . C3 C 0.7052(5) 1.0084(6) 0.3564(4) 0.058(2) Uani 1 1 d . . . H3 H 0.6846 1.0630 0.3763 0.070 Uiso 1 1 calc R . . C4 C 0.7239(6) 1.0136(6) 0.2896(4) 0.077(3) Uani 1 1 d . . . H4 H 0.7163 1.0711 0.2650 0.092 Uiso 1 1 calc R . . C5 C 0.7537(6) 0.9327(7) 0.2610(4) 0.067(3) Uani 1 1 d . . . H5 H 0.7661 0.9356 0.2163 0.081 Uiso 1 1 calc R . . C6 C 0.7656(5) 0.8477(6) 0.2961(4) 0.059(2) Uani 1 1 d . . . H6 H 0.7869 0.7936 0.2761 0.071 Uiso 1 1 calc R . . C7 C 0.7453(5) 0.8436(6) 0.3630(4) 0.048(2) Uani 1 1 d . . . C8 C 0.7724(5) 0.6722(5) 0.3702(4) 0.053(2) Uani 1 1 d . . . H8A H 0.8346 0.6700 0.3701 0.064 Uiso 1 1 calc R . . H8B H 0.7434 0.6663 0.3233 0.064 Uiso 1 1 calc R . . C9 C 0.5366(5) 0.7555(6) 0.5128(4) 0.048(2) Uani 1 1 d . . . C10 C 0.4817(3) 0.6809(4) 0.4708(3) 0.0461(19) Uani 1 1 d G . . C11 C 0.3938(3) 0.6782(4) 0.4761(3) 0.067(2) Uani 1 1 d G . . H11 H 0.3699 0.7251 0.5014 0.080 Uiso 1 1 calc R . . C12 C 0.3417(3) 0.6052(5) 0.4437(3) 0.082(3) Uani 1 1 d G . . H12 H 0.2829 0.6034 0.4473 0.098 Uiso 1 1 calc R . . C13 C 0.3774(4) 0.5350(4) 0.4059(3) 0.095(3) Uani 1 1 d G . . H13 H 0.3426 0.4862 0.3842 0.114 Uiso 1 1 calc R . . C14 C 0.4653(4) 0.5378(4) 0.4005(3) 0.098(4) Uani 1 1 d G . . H14 H 0.4892 0.4908 0.3752 0.118 Uiso 1 1 calc R . . C15 C 0.5174(3) 0.6107(5) 0.4330(3) 0.073(3) Uani 1 1 d G . . C26 C 0.9248(3) 0.6886(4) 0.5192(3) 0.0460(19) Uani 1 1 d G . . C27 C 0.9942(3) 0.6527(3) 0.4901(2) 0.052(2) Uani 1 1 d G . . H27 H 0.9958 0.5877 0.4783 0.063 Uiso 1 1 calc R . . C28 C 1.0613(3) 0.7138(4) 0.4786(2) 0.064(2) Uani 1 1 d G . . H28 H 1.1077 0.6898 0.4591 0.077 Uiso 1 1 calc R . . C29 C 1.0590(3) 0.8110(4) 0.4962(3) 0.060(2) Uani 1 1 d G . . C30 C 0.9896(4) 0.8470(3) 0.5253(3) 0.071(3) Uani 1 1 d G . . H30 H 0.9880 0.9120 0.5371 0.085 Uiso 1 1 calc R . . C31 C 0.9225(3) 0.7858(4) 0.5368(3) 0.063(2) Uani 1 1 d G . . H31 H 0.8761 0.8099 0.5563 0.076 Uiso 1 1 calc R . . C16 C 0.6473(5) 0.5643(7) 0.3962(5) 0.079(3) Uani 1 1 d . . . H16A H 0.6312 0.5606 0.3467 0.094 Uiso 1 1 calc R . . H16B H 0.6363 0.5020 0.4157 0.094 Uiso 1 1 calc R . . C17 C 0.7216(5) 0.4641(5) 0.1847(4) 0.0412(18) Uani 1 1 d . . . C18 C 0.7689(5) 0.3885(6) 0.2295(4) 0.0458(18) Uani 1 1 d . . . C19 C 0.7916(6) 0.3061(6) 0.1989(4) 0.070(3) Uani 1 1 d U . . H19 H 0.7765 0.2990 0.1517 0.084 Uiso 1 1 calc R . . C20 C 0.8366(7) 0.2324(8) 0.2364(5) 0.100(3) Uani 1 1 d U . . H20 H 0.8498 0.1758 0.2147 0.120 Uiso 1 1 calc R . . C21 C 0.8613(7) 0.2436(7) 0.3054(5) 0.095(3) Uani 1 1 d U . . H21 H 0.8936 0.1955 0.3305 0.114 Uiso 1 1 calc R . . C22 C 0.8388(6) 0.3252(6) 0.3377(4) 0.074(3) Uani 1 1 d U . . H22 H 0.8542 0.3313 0.3850 0.089 Uiso 1 1 calc R . . C23 C 0.7934(5) 0.3985(6) 0.3008(3) 0.0495(19) Uani 1 1 d . . . C24 C 0.7927(6) 0.4980(6) 0.3999(3) 0.058(2) Uani 1 1 d . . . H24A H 0.8549 0.5069 0.4110 0.070 Uiso 1 1 calc R . . H24B H 0.7755 0.4445 0.4267 0.070 Uiso 1 1 calc R . . C25 C 0.7444(4) 0.5908(6) 0.4144(3) 0.0441(18) Uani 1 1 d . . . C32 C 1.1367(6) 0.8744(7) 0.4902(5) 0.089(3) Uani 1 1 d . . . H32A H 1.1307 0.9353 0.5125 0.134 Uiso 1 1 d R . . H32B H 1.1402 0.8853 0.4426 0.134 Uiso 1 1 d R . . H32C H 1.1886 0.8427 0.5116 0.134 Uiso 1 1 d R . . C33 C 0.5461(8) 0.7694(9) 0.7034(6) 0.100(3) Uani 1 1 d U A . H33 H 0.6036 0.7440 0.7151 0.120 Uiso 1 1 d R . . C36 C 0.9158(8) -0.0665(10) 0.7047(7) 0.103(3) Uani 1 1 d U . . H36 H 0.8923 -0.0562 0.6590 0.124 Uiso 1 1 calc R . . C37 C 1.0126(8) -0.0132(10) 0.8030(6) 0.130(4) Uani 1 1 d U . . H37A H 0.9851 0.0340 0.8282 0.195 Uiso 1 1 calc R . . H37B H 1.0739 -0.0016 0.8093 0.195 Uiso 1 1 calc R . . H37C H 1.0017 -0.0767 0.8194 0.195 Uiso 1 1 calc R . . C38 C 1.0085(9) 0.0714(11) 0.6930(7) 0.158(4) Uani 1 1 d U . . H38A H 0.9713 0.0770 0.6497 0.236 Uiso 1 1 calc R . . H38B H 1.0667 0.0582 0.6852 0.236 Uiso 1 1 calc R . . H38C H 1.0075 0.1307 0.7181 0.236 Uiso 1 1 calc R . . C34A C 0.4954(16) 0.680(2) 0.8020(9) 0.097(9) Uani 0.469(19) 1 d PDU A 1 H34A H 0.5527 0.6872 0.8259 0.146 Uiso 0.469(19) 1 d PR A 1 H34B H 0.4817 0.6122 0.7949 0.146 Uiso 0.469(19) 1 d PR A 1 H34C H 0.4547 0.7082 0.8279 0.146 Uiso 0.469(19) 1 d PR A 1 C35A C 0.4072(12) 0.7209(18) 0.6909(10) 0.103(10) Uani 0.469(19) 1 d PDU A 1 H35A H 0.4102 0.7529 0.6485 0.154 Uiso 0.469(19) 1 d PR A 1 H35B H 0.3912 0.6539 0.6815 0.154 Uiso 0.469(19) 1 d PR A 1 H35C H 0.3632 0.7509 0.7135 0.154 Uiso 0.469(19) 1 d PR A 1 C34B C 0.5072(15) 0.6291(14) 0.7689(14) 0.124(10) Uani 0.531(19) 1 d PDU A 2 H34D H 0.5574 0.5995 0.7547 0.186 Uiso 0.531(19) 1 d PR A 2 H34E H 0.4574 0.5875 0.7547 0.186 Uiso 0.531(19) 1 d PR A 2 H34F H 0.5144 0.6365 0.8177 0.186 Uiso 0.531(19) 1 d PR A 2 C35B C 0.4207(15) 0.7781(15) 0.7515(15) 0.142(12) Uani 0.531(19) 1 d PDU A 2 H35D H 0.4160 0.8377 0.7269 0.213 Uiso 0.531(19) 1 d PR A 2 H35E H 0.3690 0.7407 0.7369 0.213 Uiso 0.531(19) 1 d PR A 2 H35F H 0.4260 0.7897 0.7999 0.213 Uiso 0.531(19) 1 d PR A 2 N1 N 0.7581(3) 0.6143(4) 0.4877(3) 0.0440(15) Uani 1 1 d . . . H1 H 0.7131 0.6342 0.5041 0.053 Uiso 1 1 calc R . . N2 N 0.4912(5) 0.7250(6) 0.7356(4) 0.080(2) Uani 1 1 d DU . . N3 N 0.9785(6) -0.0063(8) 0.7320(5) 0.102(3) Uani 1 1 d U . . O1 O 0.7362(3) 0.8736(4) 0.5113(2) 0.0533(15) Uani 1 1 d . . . O2 O 0.6350(3) 0.9795(4) 0.4788(2) 0.0492(13) Uani 1 1 d . . . O3 O 0.7490(4) 0.7597(4) 0.3994(2) 0.0681(17) Uani 1 1 d . . . O4 O 0.6091(3) 0.7332(4) 0.5445(3) 0.0578(15) Uani 1 1 d . . . O5 O 0.5061(3) 0.8383(4) 0.5155(3) 0.0582(15) Uani 1 1 d . . . O6 O 0.6013(4) 0.6323(5) 0.4216(3) 0.095(2) Uani 1 1 d . . . O7 O 0.6710(3) 0.5226(4) 0.2067(2) 0.0476(13) Uani 1 1 d . . . O8 O 0.7337(3) 0.4674(4) 0.1227(2) 0.0569(15) Uani 1 1 d . . . O9 O 0.7683(4) 0.4808(4) 0.3284(2) 0.0642(16) Uani 1 1 d . . . O10 O 0.8224(3) 0.6412(4) 0.6052(2) 0.0499(13) Uani 1 1 d . . . O11 O 0.8807(3) 0.5134(3) 0.5388(2) 0.0503(13) Uani 1 1 d . . . O12 O 0.5415(4) 0.8294(4) 0.6642(3) 0.0710(17) Uani 1 1 d . . . O13 O 0.5295(3) 1.0283(3) 0.5867(2) 0.0499(13) Uani 1 1 d . . . H2W H 0.5457 1.0730 0.5613 0.060 Uiso 1 1 d R A . H1W H 0.4757 1.0151 0.5800 0.060 Uiso 1 1 d R . . O14 O 0.7434(3) 0.8018(4) 0.6568(2) 0.0502(13) Uani 1 1 d . . . H3W H 0.7921 0.8221 0.6765 0.060 Uiso 1 1 d R A . H4W H 0.7465 0.7520 0.6321 0.060 Uiso 1 1 d R . . O15 O 0.8874(4) -0.1317(6) 0.7331(4) 0.104(3) Uani 1 1 d . . . S1 S 0.84589(11) 0.60809(14) 0.54166(8) 0.0406(4) 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 Gd1 0.03764(19) 0.0395(2) 0.02844(18) 0.00070(19) 0.00261(13) 0.00122(19) C1 0.035(4) 0.040(5) 0.036(4) -0.004(3) -0.004(3) -0.003(3) C2 0.045(4) 0.044(5) 0.031(4) 0.000(3) 0.006(3) 0.001(3) C3 0.087(6) 0.046(5) 0.043(5) 0.008(4) 0.017(4) 0.008(5) C4 0.132(9) 0.044(6) 0.061(6) 0.022(5) 0.033(6) 0.016(6) C5 0.094(7) 0.073(7) 0.040(5) 0.009(5) 0.026(5) 0.015(5) C6 0.085(6) 0.059(6) 0.036(5) 0.000(4) 0.021(4) 0.013(5) C7 0.068(5) 0.046(5) 0.032(4) 0.004(4) 0.013(4) 0.004(4) C8 0.074(6) 0.048(5) 0.039(4) -0.001(4) 0.015(4) 0.017(4) C9 0.044(5) 0.062(6) 0.037(4) 0.007(4) 0.001(4) -0.003(4) C10 0.039(4) 0.051(5) 0.045(4) 0.004(4) -0.006(3) -0.011(4) C11 0.049(5) 0.075(7) 0.073(6) -0.003(5) 0.000(4) -0.016(5) C12 0.050(5) 0.101(8) 0.091(7) -0.016(7) -0.002(5) -0.024(6) C13 0.086(8) 0.073(8) 0.116(9) -0.017(7) -0.014(7) -0.041(6) C14 0.067(7) 0.090(8) 0.124(9) -0.055(7) -0.031(6) -0.012(6) C15 0.048(5) 0.092(8) 0.074(6) -0.031(6) -0.007(4) -0.012(5) C26 0.043(4) 0.054(5) 0.038(4) -0.001(4) -0.001(3) 0.008(4) C27 0.056(5) 0.051(5) 0.051(5) -0.001(4) 0.011(4) 0.008(4) C28 0.053(5) 0.082(7) 0.060(5) 0.002(5) 0.014(4) 0.015(5) C29 0.059(6) 0.071(7) 0.049(5) 0.009(5) 0.002(4) 0.000(5) C30 0.066(6) 0.056(6) 0.095(7) -0.006(5) 0.024(5) -0.002(5) C31 0.054(5) 0.050(6) 0.088(6) -0.004(5) 0.021(5) 0.007(4) C16 0.061(6) 0.105(9) 0.064(6) -0.011(6) -0.010(5) 0.008(6) C17 0.043(4) 0.042(5) 0.038(4) 0.002(4) 0.004(4) -0.004(4) C18 0.056(5) 0.042(5) 0.039(4) 0.001(4) 0.008(3) 0.003(4) C19 0.103(6) 0.055(5) 0.052(5) 0.004(4) 0.009(4) 0.011(5) C20 0.151(8) 0.075(6) 0.071(6) -0.003(5) 0.010(6) 0.030(6) C21 0.137(7) 0.064(6) 0.078(6) 0.008(5) -0.002(6) 0.036(6) C22 0.111(6) 0.051(5) 0.053(5) 0.003(4) -0.007(5) 0.019(5) C23 0.077(5) 0.032(4) 0.036(4) -0.006(4) -0.003(4) 0.007(4) C24 0.089(6) 0.045(5) 0.034(4) -0.001(4) -0.011(4) 0.004(5) C25 0.051(4) 0.049(5) 0.029(4) -0.005(4) -0.002(3) 0.008(4) C32 0.080(7) 0.097(9) 0.095(8) 0.000(6) 0.029(6) -0.023(6) C33 0.099(3) 0.101(3) 0.100(3) 0.0015(10) 0.0146(11) -0.0011(10) C36 0.076(6) 0.122(6) 0.106(6) -0.013(5) -0.001(5) -0.002(5) C37 0.112(6) 0.149(7) 0.119(6) -0.027(6) -0.014(6) 0.008(6) C38 0.129(7) 0.168(8) 0.169(7) 0.012(7) 0.002(6) -0.015(6) C34A 0.106(12) 0.101(12) 0.084(11) 0.018(9) 0.009(8) -0.015(9) C35A 0.096(12) 0.106(13) 0.108(13) 0.021(9) 0.023(9) -0.019(9) C34B 0.128(12) 0.124(13) 0.125(13) 0.020(9) 0.035(9) -0.002(9) C35B 0.140(14) 0.140(14) 0.150(14) -0.005(9) 0.035(9) 0.000(9) N1 0.038(3) 0.053(4) 0.040(3) -0.002(3) 0.002(3) 0.008(3) N2 0.076(4) 0.089(5) 0.078(4) 0.034(4) 0.018(4) -0.022(4) N3 0.080(5) 0.121(6) 0.103(5) 0.001(5) 0.005(4) -0.002(4) O1 0.054(3) 0.074(4) 0.032(3) 0.005(3) 0.009(2) 0.029(3) O2 0.053(3) 0.061(4) 0.034(3) 0.003(3) 0.007(2) 0.020(3) O3 0.119(5) 0.052(4) 0.039(3) 0.003(3) 0.032(3) 0.022(3) O4 0.055(3) 0.047(3) 0.064(3) -0.012(3) -0.016(3) 0.004(3) O5 0.053(3) 0.050(4) 0.066(4) 0.004(3) -0.010(3) 0.007(3) O6 0.060(4) 0.114(6) 0.105(5) -0.063(5) -0.008(4) 0.008(4) O7 0.053(3) 0.061(4) 0.028(3) 0.004(2) 0.003(2) 0.010(3) O8 0.077(4) 0.063(4) 0.033(3) 0.010(3) 0.016(3) 0.025(3) O9 0.111(5) 0.045(4) 0.029(3) -0.004(3) -0.015(3) 0.019(3) O10 0.058(3) 0.058(3) 0.032(3) -0.004(2) -0.001(2) 0.012(3) O11 0.063(3) 0.041(3) 0.046(3) 0.002(2) 0.003(2) 0.017(3) O12 0.076(4) 0.078(5) 0.062(4) 0.019(3) 0.022(3) -0.020(3) O13 0.050(3) 0.054(3) 0.043(3) 0.000(3) 0.000(2) 0.016(3) O14 0.057(3) 0.051(3) 0.037(3) -0.001(2) -0.009(2) 0.011(3) O15 0.071(5) 0.126(7) 0.105(6) -0.009(5) -0.020(4) -0.009(4) S1 0.0451(10) 0.0439(12) 0.0317(9) 0.0011(9) 0.0017(8) 0.0109(9) _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 Gd1 O12 2.378(5) . ? Gd1 O13 2.389(4) . ? Gd1 O14 2.399(4) . ? Gd1 O8 2.411(5) 4_576 ? Gd1 O1 2.452(5) . ? Gd1 O5 2.473(5) . ? Gd1 O7 2.474(4) 4_576 ? Gd1 O2 2.491(5) . ? Gd1 O4 2.514(5) . ? Gd1 C17 2.812(7) 4_576 ? Gd1 C1 2.825(7) . ? Gd1 C9 2.846(8) . ? C1 O1 1.242(8) . ? C1 O2 1.264(8) . ? C1 C2 1.506(9) . ? C2 C3 1.371(9) . ? C2 C7 1.375(9) . ? C3 C4 1.390(10) . ? C3 H3 0.9300 . ? C4 C5 1.366(11) . ? C4 H4 0.9300 . ? C5 C6 1.362(10) . ? C5 H5 0.9300 . ? C6 C7 1.402(9) . ? C6 H6 0.9300 . ? C7 O3 1.360(8) . ? C8 O3 1.411(8) . ? C8 C25 1.527(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O5 1.244(9) . ? C9 O4 1.247(8) . ? C9 C10 1.507(9) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 O6 1.391(8) . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C26 S1 1.765(4) . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 C32 1.516(9) . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C16 O6 1.326(10) . ? C16 C25 1.548(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O7 1.252(8) . ? C17 O8 1.262(8) . ? C17 C18 1.491(10) . ? C17 Gd1 2.812(7) 4_575 ? C18 C19 1.361(10) . ? C18 C23 1.406(9) . ? C19 C20 1.386(12) . ? C19 H19 0.9300 . ? C20 C21 1.364(12) . ? C20 H20 0.9300 . ? C21 C22 1.368(12) . ? C21 H21 0.9300 . ? C22 C23 1.380(10) . ? C22 H22 0.9300 . ? C23 O9 1.345(8) . ? C24 O9 1.422(8) . ? C24 C25 1.535(10) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N1 1.464(8) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 O12 1.129(12) . ? C33 N2 1.293(12) . ? C33 H33 0.9580 . ? C36 O15 1.182(13) . ? C36 N3 1.334(13) . ? C36 H36 0.9300 . ? C37 N3 1.422(12) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 N3 1.438(14) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C34A N2 1.441(14) . ? C34A H34A 0.9507 . ? C34A H34B 0.9668 . ? C34A H34C 0.9566 . ? C35A N2 1.465(14) . ? C35A H35A 0.9537 . ? C35A H35B 0.9699 . ? C35A H35C 0.9658 . ? C34B N2 1.484(14) . ? C34B H34D 0.9619 . ? C34B H34E 0.9734 . ? C34B H34F 0.9552 . ? C35B N2 1.397(15) . ? C35B H35D 0.9540 . ? C35B H35E 0.9647 . ? C35B H35F 0.9575 . ? N1 S1 1.604(5) . ? N1 H1 0.8600 . ? O7 Gd1 2.474(4) 4_575 ? O8 Gd1 2.411(5) 4_575 ? O10 S1 1.431(5) . ? O11 S1 1.422(5) . ? O13 H2W 0.8568 . ? O13 H1W 0.8506 . ? O14 H3W 0.8485 . ? O14 H4W 0.8480 . ? 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 O12 Gd1 O13 82.4(2) . . ? O12 Gd1 O14 83.99(19) . . ? O13 Gd1 O14 150.84(15) . . ? O12 Gd1 O8 126.45(18) . 4_576 ? O13 Gd1 O8 82.21(18) . 4_576 ? O14 Gd1 O8 85.40(18) . 4_576 ? O12 Gd1 O1 146.5(2) . . ? O13 Gd1 O1 125.98(16) . . ? O14 Gd1 O1 76.94(16) . . ? O8 Gd1 O1 79.56(17) 4_576 . ? O12 Gd1 O5 73.41(19) . . ? O13 Gd1 O5 75.47(18) . . ? O14 Gd1 O5 124.56(18) . . ? O8 Gd1 O5 147.87(18) 4_576 . ? O1 Gd1 O5 95.06(18) . . ? O12 Gd1 O7 73.70(18) . 4_576 ? O13 Gd1 O7 78.09(16) . 4_576 ? O14 Gd1 O7 73.38(16) . 4_576 ? O8 Gd1 O7 52.99(16) 4_576 4_576 ? O1 Gd1 O7 124.90(17) . 4_576 ? O5 Gd1 O7 139.93(17) . 4_576 ? O12 Gd1 O2 143.27(18) . . ? O13 Gd1 O2 74.43(16) . . ? O14 Gd1 O2 128.54(16) . . ? O8 Gd1 O2 78.53(16) 4_576 . ? O1 Gd1 O2 52.28(15) . . ? O5 Gd1 O2 73.43(17) . . ? O7 Gd1 O2 126.74(17) 4_576 . ? O12 Gd1 O4 76.5(2) . . ? O13 Gd1 O4 126.72(17) . . ? O14 Gd1 O4 74.15(16) . . ? O8 Gd1 O4 147.88(18) 4_576 . ? O1 Gd1 O4 71.95(18) . . ? O5 Gd1 O4 51.79(17) . . ? O7 Gd1 O4 137.59(17) 4_576 . ? O2 Gd1 O4 94.94(17) . . ? O12 Gd1 C17 100.0(2) . 4_576 ? O13 Gd1 C17 78.65(18) . 4_576 ? O14 Gd1 C17 78.50(19) . 4_576 ? O8 Gd1 C17 26.57(18) 4_576 4_576 ? O1 Gd1 C17 102.8(2) . 4_576 ? O5 Gd1 C17 153.9(2) . 4_576 ? O7 Gd1 C17 26.42(17) 4_576 4_576 ? O2 Gd1 C17 102.8(2) . 4_576 ? O4 Gd1 C17 152.63(18) . 4_576 ? O12 Gd1 C1 152.81(19) . . ? O13 Gd1 C1 100.96(19) . . ? O14 Gd1 C1 102.92(19) . . ? O8 Gd1 C1 80.61(17) 4_576 . ? O1 Gd1 C1 26.00(16) . . ? O5 Gd1 C1 81.27(18) . . ? O7 Gd1 C1 133.49(18) 4_576 . ? O2 Gd1 C1 26.56(16) . . ? O4 Gd1 C1 80.20(19) . . ? C17 Gd1 C1 107.2(2) 4_576 . ? O12 Gd1 C9 73.3(2) . . ? O13 Gd1 C9 101.1(2) . . ? O14 Gd1 C9 99.5(2) . . ? O8 Gd1 C9 160.20(18) 4_576 . ? O1 Gd1 C9 82.9(2) . . ? O5 Gd1 C9 25.84(18) . . ? O7 Gd1 C9 146.79(19) 4_576 . ? O2 Gd1 C9 83.53(19) . . ? O4 Gd1 C9 25.95(19) . . ? C17 Gd1 C9 173.2(2) 4_576 . ? C1 Gd1 C9 79.6(2) . . ? O1 C1 O2 120.8(6) . . ? O1 C1 C2 121.2(6) . . ? O2 C1 C2 118.0(6) . . ? O1 C1 Gd1 60.0(4) . . ? O2 C1 Gd1 61.8(4) . . ? C2 C1 Gd1 169.7(5) . . ? C3 C2 C7 118.6(7) . . ? C3 C2 C1 118.0(6) . . ? C7 C2 C1 123.3(6) . . ? C2 C3 C4 121.3(8) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 118.7(8) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.8(8) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C7 118.7(8) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? O3 C7 C2 117.0(6) . . ? O3 C7 C6 122.1(7) . . ? C2 C7 C6 120.8(7) . . ? O3 C8 C25 106.8(6) . . ? O3 C8 H8A 110.4 . . ? C25 C8 H8A 110.4 . . ? O3 C8 H8B 110.4 . . ? C25 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? O5 C9 O4 122.0(7) . . ? O5 C9 C10 117.7(7) . . ? O4 C9 C10 120.3(7) . . ? O5 C9 Gd1 60.1(4) . . ? O4 C9 Gd1 62.0(4) . . ? C10 C9 Gd1 177.6(6) . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 117.5(5) . . ? C15 C10 C9 122.2(5) . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? O6 C15 C14 125.5(5) . . ? O6 C15 C10 113.4(5) . . ? C14 C15 C10 120.0 . . ? C27 C26 C31 120.0 . . ? C27 C26 S1 119.5(3) . . ? C31 C26 S1 120.2(3) . . ? C28 C27 C26 120.0 . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 C32 120.4(6) . . ? C28 C29 C32 119.3(6) . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? O6 C16 C25 108.1(7) . . ? O6 C16 H16A 110.1 . . ? C25 C16 H16A 110.1 . . ? O6 C16 H16B 110.1 . . ? C25 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? O7 C17 O8 120.3(7) . . ? O7 C17 C18 121.9(6) . . ? O8 C17 C18 117.8(7) . . ? O7 C17 Gd1 61.6(4) . 4_575 ? O8 C17 Gd1 58.7(4) . 4_575 ? C18 C17 Gd1 176.2(5) . 4_575 ? C19 C18 C23 118.4(7) . . ? C19 C18 C17 117.7(7) . . ? C23 C18 C17 123.9(7) . . ? C18 C19 C20 121.7(8) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 119.5(10) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 120.2(9) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.5(8) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? O9 C23 C22 124.5(7) . . ? O9 C23 C18 115.8(7) . . ? C22 C23 C18 119.7(7) . . ? O9 C24 C25 105.0(6) . . ? O9 C24 H24A 110.8 . . ? C25 C24 H24A 110.8 . . ? O9 C24 H24B 110.8 . . ? C25 C24 H24B 110.8 . . ? H24A C24 H24B 108.8 . . ? N1 C25 C24 111.5(5) . . ? N1 C25 C8 112.7(6) . . ? C24 C25 C8 108.7(6) . . ? N1 C25 C16 105.9(6) . . ? C24 C25 C16 104.4(7) . . ? C8 C25 C16 113.3(6) . . ? C29 C32 H32A 109.8 . . ? C29 C32 H32B 109.2 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.4 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O12 C33 N2 134.9(12) . . ? O12 C33 H33 113.2 . . ? N2 C33 H33 111.9 . . ? O15 C36 N3 126.1(13) . . ? O15 C36 H36 116.9 . . ? N3 C36 H36 116.9 . . ? N3 C37 H37A 109.5 . . ? N3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N3 C38 H38A 109.5 . . ? N3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C34A H34A 108.5 . . ? N2 C34A H34B 108.1 . . ? H34A C34A H34B 110.2 . . ? N2 C34A H34C 111.4 . . ? H34A C34A H34C 109.9 . . ? H34B C34A H34C 108.8 . . ? N2 C34A H34F 135.4 . . ? H34A C34A H34F 65.1 . . ? H34B C34A H34F 47.1 . . ? H34C C34A H34F 112.0 . . ? N2 C35A H35A 110.6 . . ? N2 C35A H35B 109.5 . . ? H35A C35A H35B 108.7 . . ? N2 C35A H35C 109.9 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 108.6 . . ? N2 C35A H35E 92.2 . . ? H35A C35A H35E 131.0 . . ? H35B C35A H35E 102.9 . . ? N2 C34B H34A 83.1 . . ? N2 C34B H34B 121.5 . . ? H34A C34B H34B 83.8 . . ? N2 C34B H34D 110.0 . . ? H34A C34B H34D 97.7 . . ? H34B C34B H34D 128.2 . . ? N2 C34B H34E 109.1 . . ? H34A C34B H34E 144.5 . . ? H34B C34B H34E 61.3 . . ? H34D C34B H34E 108.2 . . ? N2 C34B H34F 109.6 . . ? H34B C34B H34F 47.6 . . ? H34D C34B H34F 111.1 . . ? H34E C34B H34F 108.8 . . ? N2 C35B H35C 104.3 . . ? N2 C35B H35D 110.1 . . ? H35C C35B H35D 87.6 . . ? N2 C35B H35E 107.5 . . ? H35D C35B H35E 108.3 . . ? N2 C35B H35F 111.0 . . ? H35C C35B H35F 130.6 . . ? H35D C35B H35F 110.4 . . ? H35E C35B H35F 109.3 . . ? C25 N1 S1 128.6(5) . . ? C25 N1 H1 115.7 . . ? S1 N1 H1 115.7 . . ? C33 N2 C35B 117.4(13) . . ? C33 N2 C34A 134.9(12) . . ? C35B N2 C34A 87.4(15) . . ? C33 N2 C35A 108.8(11) . . ? C35B N2 C35A 59.5(13) . . ? C34A N2 C35A 116.3(12) . . ? C33 N2 C34B 124.2(13) . . ? C35B N2 C34B 117.1(13) . . ? C35A N2 C34B 107.8(15) . . ? C36 N3 C37 119.8(11) . . ? C36 N3 C38 121.9(11) . . ? C37 N3 C38 118.1(11) . . ? C1 O1 Gd1 94.0(4) . . ? C1 O2 Gd1 91.6(4) . . ? C7 O3 C8 120.8(6) . . ? C9 O4 Gd1 92.1(5) . . ? C9 O5 Gd1 94.1(4) . . ? C16 O6 C15 118.9(7) . . ? C17 O7 Gd1 92.0(4) . 4_575 ? C17 O8 Gd1 94.7(4) . 4_575 ? C23 O9 C24 119.4(6) . . ? C33 O12 Gd1 136.9(8) . . ? Gd1 O13 H2W 107.6 . . ? Gd1 O13 H1W 119.8 . . ? H2W O13 H1W 115.8 . . ? Gd1 O14 H3W 124.8 . . ? Gd1 O14 H4W 105.1 . . ? H3W O14 H4W 114.1 . . ? O11 S1 O10 118.6(3) . . ? O11 S1 N1 108.4(3) . . ? O10 S1 N1 104.9(3) . . ? O11 S1 C26 106.7(3) . . ? O10 S1 C26 107.2(3) . . ? N1 S1 C26 111.0(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.755 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.118 #==END data_4 #TrackingRef 'complexes.cif' _database_code_depnum_ccdc_archive 'CCDC 731525' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H44 N3 O15 S Tb' _chemical_formula_weight 973.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.608(8) _cell_length_b 13.829(7) _cell_length_c 19.631(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.558(8) _cell_angle_gamma 90.00 _cell_volume 4190(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3264 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 28.23 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 1.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5621 _exptl_absorpt_correction_T_max 0.6409 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20355 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7389 _reflns_number_gt 6246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.0585P)^2^+2.1782P] 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 7389 _refine_ls_number_parameters 544 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.633354(13) 0.900879(13) 0.592275(9) 0.03535(9) Uani 1 1 d . . . C1 C 0.6956(3) 0.9249(3) 0.4660(2) 0.0368(9) Uani 1 1 d . . . C2 C 0.7171(3) 0.9249(3) 0.3942(2) 0.0401(9) Uani 1 1 d . . . C3 C 0.7052(4) 1.0091(3) 0.3561(2) 0.0598(13) Uani 1 1 d . . . H3 H 0.6844 1.0639 0.3757 0.072 Uiso 1 1 calc R . . C4 C 0.7238(5) 1.0137(4) 0.2894(3) 0.0785(18) Uani 1 1 d . . . H4 H 0.7147 1.0708 0.2644 0.094 Uiso 1 1 calc R . . C5 C 0.7553(4) 0.9343(4) 0.2606(3) 0.0672(15) Uani 1 1 d . . . H5 H 0.7695 0.9380 0.2163 0.081 Uiso 1 1 calc R . . C6 C 0.7663(4) 0.8486(4) 0.2964(2) 0.0565(13) Uani 1 1 d . . . H6 H 0.7872 0.7944 0.2762 0.068 Uiso 1 1 calc R . . C7 C 0.7461(3) 0.8433(3) 0.3630(2) 0.0446(10) Uani 1 1 d . . . C8 C 0.7731(4) 0.6716(3) 0.3703(2) 0.0523(12) Uani 1 1 d . . . H8A H 0.8352 0.6687 0.3706 0.063 Uiso 1 1 calc R . . H8B H 0.7446 0.6664 0.3230 0.063 Uiso 1 1 calc R . . C9 C 0.5367(3) 0.7555(3) 0.5124(2) 0.0456(10) Uani 1 1 d . . . C10 C 0.4819(3) 0.6804(3) 0.4716(2) 0.0480(11) Uani 1 1 d . . . C11 C 0.3939(3) 0.6775(4) 0.4748(3) 0.0638(13) Uani 1 1 d . . . H11 H 0.3695 0.7253 0.4992 0.077 Uiso 1 1 calc R . . C12 C 0.3417(4) 0.6054(5) 0.4426(4) 0.0822(19) Uani 1 1 d . . . H12 H 0.2826 0.6045 0.4448 0.099 Uiso 1 1 calc R . . C13 C 0.3788(5) 0.5352(6) 0.4075(4) 0.099(2) Uani 1 1 d . . . H13 H 0.3450 0.4841 0.3879 0.119 Uiso 1 1 calc R . . C14 C 0.4643(4) 0.5390(5) 0.4005(4) 0.091(2) Uani 1 1 d . . . H14 H 0.4882 0.4920 0.3752 0.109 Uiso 1 1 calc R . . C15 C 0.5150(4) 0.6133(4) 0.4313(3) 0.0683(16) Uani 1 1 d . . . C16 C 0.6486(4) 0.5631(4) 0.3958(3) 0.0726(16) Uani 1 1 d . . . H16A H 0.6329 0.5572 0.3463 0.087 Uiso 1 1 calc R . . H16B H 0.6376 0.5017 0.4167 0.087 Uiso 1 1 calc R . . C17 C 0.7202(3) 0.4647(3) 0.1841(2) 0.0404(10) Uani 1 1 d . . . C18 C 0.7689(3) 0.3881(3) 0.2289(2) 0.0452(11) Uani 1 1 d . . . C19 C 0.7912(4) 0.3046(4) 0.1976(3) 0.0675(14) Uani 1 1 d U . . H19 H 0.7760 0.2975 0.1502 0.081 Uiso 1 1 calc R . . C20 C 0.8359(5) 0.2311(4) 0.2354(3) 0.0883(17) Uani 1 1 d U . . H20 H 0.8481 0.1738 0.2140 0.106 Uiso 1 1 calc R . . C21 C 0.8621(5) 0.2437(4) 0.3048(3) 0.0855(17) Uani 1 1 d U . . H21 H 0.8950 0.1962 0.3301 0.103 Uiso 1 1 calc R . . C22 C 0.8398(4) 0.3260(4) 0.3370(3) 0.0680(14) Uani 1 1 d U . . H22 H 0.8563 0.3333 0.3842 0.082 Uiso 1 1 calc R . . C23 C 0.7930(4) 0.3981(3) 0.2997(2) 0.0500(12) Uani 1 1 d . . . C24 C 0.7928(4) 0.4976(3) 0.3999(2) 0.0587(13) Uani 1 1 d . . . H24A H 0.8550 0.5068 0.4109 0.070 Uiso 1 1 calc R . . H24B H 0.7759 0.4439 0.4268 0.070 Uiso 1 1 calc R . . C25 C 0.7439(3) 0.5901(3) 0.4138(2) 0.0461(11) Uani 1 1 d . . . C26 C 0.9255(3) 0.6885(3) 0.5199(2) 0.0432(10) Uani 1 1 d . . . C27 C 0.9939(3) 0.6538(4) 0.4905(2) 0.0563(12) Uani 1 1 d . . . H27 H 0.9957 0.5889 0.4785 0.068 Uiso 1 1 calc R . . C28 C 1.0603(3) 0.7152(4) 0.4787(3) 0.0638(14) Uani 1 1 d . . . H28 H 1.1056 0.6914 0.4578 0.077 Uiso 1 1 calc R . . C29 C 1.0599(3) 0.8103(4) 0.4973(3) 0.0611(13) Uani 1 1 d . . . C30 C 0.9898(4) 0.8446(4) 0.5251(3) 0.0739(16) Uani 1 1 d . . . H30 H 0.9877 0.9098 0.5362 0.089 Uiso 1 1 calc R . . C31 C 0.9233(3) 0.7858(4) 0.5368(3) 0.0617(13) Uani 1 1 d . . . H31 H 0.8769 0.8108 0.5560 0.074 Uiso 1 1 calc R . . C32 C 1.1366(4) 0.8759(5) 0.4901(4) 0.091(2) Uani 1 1 d . . . H32A H 1.1814 0.8388 0.4739 0.136 Uiso 1 1 d R . . H32B H 1.1585 0.9036 0.5341 0.136 Uiso 1 1 d R . . H32C H 1.1182 0.9267 0.4579 0.136 Uiso 1 1 d R . . C33 C 0.5477(5) 0.7678(6) 0.7044(4) 0.097(2) Uani 1 1 d U A . H33 H 0.6039 0.7454 0.7173 0.116 Uiso 1 1 calc R . . C36 C 0.9160(4) -0.0670(7) 0.7044(4) 0.093(2) Uani 1 1 d . . . H36 H 0.8947 -0.0576 0.6581 0.112 Uiso 1 1 calc R . . C37 C 1.0136(5) -0.0145(8) 0.8021(4) 0.138(4) Uani 1 1 d . . . H37A H 0.9798 0.0240 0.8290 0.166 Uiso 1 1 calc R . . H37B H 1.0721 0.0089 0.8083 0.166 Uiso 1 1 calc R . . H37C H 1.0131 -0.0806 0.8168 0.166 Uiso 1 1 calc R . . C38 C 1.0075(9) 0.0713(9) 0.6938(7) 0.193(5) Uani 1 1 d U . . H38A H 1.0638 0.0567 0.6824 0.232 Uiso 1 1 calc R . . H38B H 1.0106 0.1293 0.7210 0.232 Uiso 1 1 calc R . . H38C H 0.9675 0.0807 0.6522 0.232 Uiso 1 1 calc R . . C34A C 0.4205(10) 0.7782(10) 0.7486(9) 0.140(7) Uani 0.595(14) 1 d PDU A 1 H34A H 0.4157 0.8354 0.7209 0.210 Uiso 0.595(14) 1 d PR A 1 H34B H 0.4247 0.7944 0.7959 0.210 Uiso 0.595(14) 1 d PR A 1 H34C H 0.3687 0.7394 0.7349 0.210 Uiso 0.595(14) 1 d PR A 1 C35A C 0.5093(11) 0.6298(10) 0.7706(9) 0.125(5) Uani 0.595(14) 1 d PDU A 1 H34D H 0.4082 0.7469 0.6427 0.188 Uiso 0.595(14) 1 d PR A 1 H34E H 0.3642 0.7549 0.7097 0.188 Uiso 0.595(14) 1 d PR A 1 H34F H 0.3862 0.6529 0.6817 0.188 Uiso 0.595(14) 1 d PR A 1 C34B C 0.4055(10) 0.7198(13) 0.6893(8) 0.095(6) Uani 0.405(14) 1 d PDU A 2 H35A H 0.5601 0.5992 0.7602 0.143 Uiso 0.405(14) 1 d PR A 2 H35B H 0.5161 0.6422 0.8202 0.143 Uiso 0.405(14) 1 d PR A 2 H35C H 0.4601 0.5872 0.7592 0.143 Uiso 0.405(14) 1 d PR A 2 C35B C 0.4959(12) 0.6811(13) 0.8006(7) 0.091(6) Uani 0.405(14) 1 d PDU A 2 H35D H 0.5534 0.6863 0.8252 0.136 Uiso 0.405(14) 1 d PR A 2 H35E H 0.4564 0.7153 0.8242 0.136 Uiso 0.405(14) 1 d PR A 2 H35F H 0.4784 0.6133 0.7972 0.136 Uiso 0.405(14) 1 d PR A 2 N1 N 0.7577(2) 0.6150(2) 0.48804(17) 0.0425(8) Uani 1 1 d . . . H1 H 0.7130 0.6356 0.5044 0.051 Uiso 1 1 calc R . . N2 N 0.4915(3) 0.7253(4) 0.7348(2) 0.0750(13) Uani 1 1 d DU . . N3 N 0.9783(4) -0.0082(5) 0.7326(3) 0.0973(17) Uani 1 1 d . . . O1 O 0.7354(2) 0.8730(2) 0.51174(15) 0.0523(8) Uani 1 1 d . . . O2 O 0.6353(2) 0.9794(2) 0.47902(14) 0.0497(8) Uani 1 1 d . . . O3 O 0.7498(3) 0.7598(2) 0.40017(15) 0.0672(11) Uani 1 1 d . . . O4 O 0.6093(2) 0.7332(2) 0.54507(17) 0.0581(9) Uani 1 1 d . . . O5 O 0.5062(2) 0.8387(2) 0.51511(17) 0.0590(9) Uani 1 1 d . . . O6 O 0.6017(3) 0.6330(3) 0.4198(2) 0.0855(13) Uani 1 1 d . . . O7 O 0.6704(2) 0.5227(2) 0.20665(14) 0.0483(7) Uani 1 1 d . . . O8 O 0.7324(2) 0.4678(2) 0.12192(15) 0.0561(9) Uani 1 1 d . . . O9 O 0.7679(3) 0.4810(2) 0.32823(15) 0.0651(10) Uani 1 1 d . . . O10 O 0.8221(2) 0.6416(2) 0.60574(14) 0.0496(8) Uani 1 1 d . . . O11 O 0.8797(2) 0.5125(2) 0.53927(15) 0.0508(8) Uani 1 1 d . . . O12 O 0.5418(2) 0.8295(3) 0.66348(18) 0.0671(10) Uani 1 1 d . . . O13 O 0.5299(2) 1.0270(2) 0.58711(14) 0.0491(7) Uani 1 1 d . . . H1W H 0.4763 1.0114 0.5795 0.059 Uiso 1 1 d R A . H2W H 0.5444 1.0737 0.5609 0.059 Uiso 1 1 d R . . O14 O 0.7413(2) 0.8012(2) 0.65672(14) 0.0490(7) Uani 1 1 d . . . H3W H 0.7829 0.8306 0.6814 0.059 Uiso 1 1 d R A . H4W H 0.7559 0.7490 0.6380 0.059 Uiso 1 1 d R . . O15 O 0.8847(3) -0.1313(4) 0.7335(3) 0.0985(15) Uani 1 1 d . . . S1 S 0.84570(7) 0.60826(7) 0.54186(5) 0.0402(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 Tb1 0.03748(14) 0.04041(13) 0.02772(12) 0.00098(7) 0.00339(8) 0.00102(8) C1 0.040(2) 0.037(2) 0.033(2) -0.0049(16) 0.0051(18) -0.0001(18) C2 0.044(2) 0.044(2) 0.033(2) 0.0022(17) 0.0074(18) 0.0030(19) C3 0.086(4) 0.049(3) 0.047(3) 0.005(2) 0.019(3) 0.011(3) C4 0.129(6) 0.060(3) 0.053(3) 0.021(3) 0.033(3) 0.019(3) C5 0.091(4) 0.077(3) 0.038(3) 0.009(2) 0.025(3) 0.007(3) C6 0.077(4) 0.059(3) 0.037(2) -0.005(2) 0.020(2) 0.007(3) C7 0.056(3) 0.048(2) 0.031(2) 0.0007(18) 0.0088(19) 0.003(2) C8 0.077(4) 0.045(2) 0.036(2) -0.0014(18) 0.012(2) 0.018(2) C9 0.046(3) 0.051(3) 0.039(2) 0.0035(19) 0.004(2) -0.008(2) C10 0.041(3) 0.049(3) 0.052(3) -0.003(2) -0.001(2) -0.006(2) C11 0.048(3) 0.073(3) 0.070(3) 0.000(3) 0.007(2) -0.007(3) C12 0.049(3) 0.104(5) 0.090(5) 0.002(4) 0.001(3) -0.026(3) C13 0.086(5) 0.089(5) 0.112(6) -0.018(4) -0.019(4) -0.043(4) C14 0.065(4) 0.086(4) 0.112(5) -0.046(4) -0.021(4) -0.002(3) C15 0.041(3) 0.085(4) 0.073(4) -0.023(3) -0.010(3) -0.012(3) C16 0.067(4) 0.076(4) 0.068(3) -0.017(3) -0.012(3) 0.008(3) C17 0.044(3) 0.045(2) 0.031(2) 0.0037(17) 0.0021(18) -0.004(2) C18 0.059(3) 0.039(2) 0.037(2) 0.0033(17) 0.006(2) 0.000(2) C19 0.091(3) 0.059(2) 0.052(2) 0.001(2) 0.006(2) 0.012(2) C20 0.115(3) 0.069(3) 0.080(3) -0.005(2) 0.008(3) 0.023(3) C21 0.109(3) 0.067(3) 0.075(3) 0.008(2) -0.002(3) 0.026(3) C22 0.087(3) 0.058(2) 0.055(2) 0.004(2) -0.003(2) 0.015(2) C23 0.070(3) 0.037(2) 0.040(2) 0.0011(18) 0.000(2) 0.002(2) C24 0.089(4) 0.046(2) 0.036(2) -0.0063(19) -0.009(2) 0.009(3) C25 0.051(3) 0.054(3) 0.030(2) -0.0022(17) -0.0039(19) 0.005(2) C26 0.037(2) 0.052(2) 0.038(2) 0.0010(18) -0.0023(18) 0.008(2) C27 0.057(3) 0.059(3) 0.055(3) -0.006(2) 0.014(2) 0.011(3) C28 0.048(3) 0.080(4) 0.066(3) 0.000(3) 0.017(2) 0.008(3) C29 0.054(3) 0.071(3) 0.058(3) 0.008(3) 0.007(2) 0.000(3) C30 0.069(4) 0.050(3) 0.104(5) -0.004(3) 0.019(3) 0.000(3) C31 0.052(3) 0.052(3) 0.084(4) -0.007(3) 0.018(3) 0.008(2) C32 0.073(4) 0.098(5) 0.105(5) 0.005(4) 0.028(4) -0.019(4) C33 0.076(3) 0.119(4) 0.093(3) 0.026(3) 0.006(3) -0.016(3) C36 0.056(4) 0.148(7) 0.072(4) -0.034(5) -0.004(3) 0.019(5) C37 0.078(5) 0.198(10) 0.126(7) -0.068(7) -0.027(5) 0.005(6) C38 0.186(6) 0.196(6) 0.196(6) 0.009(4) 0.024(4) -0.009(4) C34A 0.138(8) 0.140(8) 0.145(8) 0.002(4) 0.030(4) 0.000(4) C35A 0.128(7) 0.126(6) 0.124(6) 0.011(4) 0.025(4) -0.002(4) C34B 0.093(7) 0.098(7) 0.095(7) 0.008(4) 0.013(4) -0.009(4) C35B 0.095(7) 0.092(7) 0.086(7) 0.008(4) 0.014(4) -0.006(4) N1 0.039(2) 0.053(2) 0.0345(18) -0.0024(15) 0.0025(15) 0.0081(16) N2 0.072(3) 0.087(3) 0.069(2) 0.027(2) 0.020(2) -0.018(2) N3 0.062(3) 0.121(5) 0.105(4) -0.011(4) -0.002(3) -0.010(3) O1 0.059(2) 0.0667(19) 0.0322(15) 0.0097(14) 0.0113(14) 0.0245(17) O2 0.0547(19) 0.0616(19) 0.0336(15) 0.0043(13) 0.0099(13) 0.0187(16) O3 0.125(3) 0.0442(17) 0.0383(17) 0.0040(14) 0.0304(19) 0.0213(19) O4 0.050(2) 0.0520(18) 0.065(2) -0.0126(15) -0.0150(16) 0.0015(16) O5 0.059(2) 0.0469(19) 0.065(2) -0.0002(15) -0.0116(17) 0.0033(16) O6 0.065(3) 0.088(3) 0.096(3) -0.043(2) -0.013(2) 0.000(2) O7 0.0520(19) 0.0602(19) 0.0325(14) 0.0037(13) 0.0063(13) 0.0092(16) O8 0.071(2) 0.067(2) 0.0329(16) 0.0086(14) 0.0144(15) 0.0226(18) O9 0.111(3) 0.0466(18) 0.0310(15) -0.0048(13) -0.0116(17) 0.0157(19) O10 0.059(2) 0.0574(18) 0.0315(15) -0.0014(13) 0.0050(14) 0.0111(16) O11 0.058(2) 0.0474(17) 0.0454(16) 0.0007(13) 0.0008(14) 0.0161(15) O12 0.072(3) 0.070(2) 0.062(2) 0.0138(18) 0.0214(19) -0.0163(19) O13 0.0501(19) 0.0574(18) 0.0383(15) -0.0040(13) 0.0016(13) 0.0105(15) O14 0.057(2) 0.0529(17) 0.0345(15) -0.0018(13) -0.0016(13) 0.0104(15) O15 0.069(3) 0.131(4) 0.090(3) -0.009(3) -0.005(3) -0.017(3) S1 0.0446(6) 0.0431(6) 0.0315(5) 0.0000(4) 0.0013(4) 0.0092(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O12 2.359(3) . ? Tb1 O13 2.369(3) . ? Tb1 O14 2.388(3) . ? Tb1 O8 2.399(3) 4_576 ? Tb1 O1 2.436(3) . ? Tb1 O5 2.466(3) . ? Tb1 O7 2.471(3) 4_576 ? Tb1 O2 2.479(3) . ? Tb1 O4 2.504(3) . ? Tb1 C17 2.795(4) 4_576 ? C1 O1 1.242(5) . ? C1 O2 1.260(5) . ? C1 C2 1.498(6) . ? C2 C3 1.382(6) . ? C2 C7 1.391(6) . ? C3 C4 1.383(7) . ? C3 H3 0.9300 . ? C4 C5 1.361(8) . ? C4 H4 0.9300 . ? C5 C6 1.376(7) . ? C5 H5 0.9300 . ? C6 C7 1.391(6) . ? C6 H6 0.9300 . ? C7 O3 1.363(5) . ? C8 O3 1.424(5) . ? C8 C25 1.524(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O5 1.249(5) . ? C9 O4 1.255(5) . ? C9 C10 1.499(6) . ? C10 C15 1.369(7) . ? C10 C11 1.385(7) . ? C11 C12 1.381(8) . ? C11 H11 0.9300 . ? C12 C13 1.368(10) . ? C12 H12 0.9300 . ? C13 C14 1.363(10) . ? C13 H13 0.9300 . ? C14 C15 1.380(8) . ? C14 H14 0.9300 . ? C15 O6 1.431(7) . ? C16 O6 1.338(7) . ? C16 C25 1.524(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O7 1.244(5) . ? C17 O8 1.264(5) . ? C17 C18 1.508(6) . ? C17 Tb1 2.795(4) 4_575 ? C18 C19 1.376(7) . ? C18 C23 1.393(6) . ? C19 C20 1.384(8) . ? C19 H19 0.9300 . ? C20 C21 1.375(8) . ? C20 H20 0.9300 . ? C21 C22 1.372(8) . ? C21 H21 0.9300 . ? C22 C23 1.380(6) . ? C22 H22 0.9300 . ? C23 O9 1.358(5) . ? C24 O9 1.422(5) . ? C24 C25 1.536(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N1 1.481(5) . ? C26 C27 1.375(6) . ? C26 C31 1.388(6) . ? C26 S1 1.768(5) . ? C27 C28 1.385(7) . ? C27 H27 0.9300 . ? C28 C29 1.365(8) . ? C28 H28 0.9300 . ? C29 C30 1.377(8) . ? C29 C32 1.526(8) . ? C30 C31 1.364(8) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 O12 1.166(7) . ? C33 N2 1.275(8) . ? C33 H33 0.9300 . ? C36 O15 1.199(9) . ? C36 N3 1.325(9) . ? C36 H36 0.9300 . ? C37 N3 1.395(9) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 N3 1.450(13) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C34A N2 1.387(12) . ? C34A H34A 0.9576 . ? C34A H34B 0.9467 . ? C34A H34C 0.9750 . ? C35A N2 1.503(12) . ? C35A H35A 0.9491 . ? C35A H35B 0.9777 . ? C35A H35C 0.9666 . ? C34B N2 1.499(13) . ? C34B H34D 0.9957 . ? C34B H34E 0.9421 . ? C34B H34F 0.9772 . ? C35B N2 1.422(12) . ? C35B H35D 0.9564 . ? C35B H35E 0.9497 . ? C35B H35F 0.9757 . ? N1 S1 1.606(4) . ? N1 H1 0.8600 . ? O7 Tb1 2.471(3) 4_575 ? O8 Tb1 2.399(3) 4_575 ? O10 S1 1.435(3) . ? O11 S1 1.430(3) . ? O13 H1W 0.8565 . ? O13 H2W 0.8754 . ? O14 H3W 0.8540 . ? O14 H4W 0.8561 . ? 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 O12 Tb1 O13 82.23(13) . . ? O12 Tb1 O14 83.46(13) . . ? O13 Tb1 O14 150.48(10) . . ? O12 Tb1 O8 126.74(11) . 4_576 ? O13 Tb1 O8 82.15(13) . 4_576 ? O14 Tb1 O8 86.00(12) . 4_576 ? O12 Tb1 O1 146.13(12) . . ? O13 Tb1 O1 126.59(10) . . ? O14 Tb1 O1 76.98(11) . . ? O8 Tb1 O1 79.49(12) 4_576 . ? O12 Tb1 O5 73.42(13) . . ? O13 Tb1 O5 75.49(11) . . ? O14 Tb1 O5 124.32(11) . . ? O8 Tb1 O5 147.53(11) 4_576 . ? O1 Tb1 O5 95.18(13) . . ? O12 Tb1 O7 73.79(12) . 4_576 ? O13 Tb1 O7 77.86(10) . 4_576 ? O14 Tb1 O7 73.40(10) . 4_576 ? O8 Tb1 O7 53.20(10) 4_576 4_576 ? O1 Tb1 O7 124.78(11) . 4_576 ? O5 Tb1 O7 139.94(11) . 4_576 ? O12 Tb1 O2 143.55(12) . . ? O13 Tb1 O2 74.82(10) . . ? O14 Tb1 O2 128.77(10) . . ? O8 Tb1 O2 78.03(11) 4_576 . ? O1 Tb1 O2 52.46(10) . . ? O5 Tb1 O2 73.63(12) . . ? O7 Tb1 O2 126.55(11) 4_576 . ? O12 Tb1 O4 76.18(13) . . ? O13 Tb1 O4 127.05(11) . . ? O14 Tb1 O4 73.54(11) . . ? O8 Tb1 O4 147.78(12) 4_576 . ? O1 Tb1 O4 71.91(12) . . ? O5 Tb1 O4 52.20(10) . . ? O7 Tb1 O4 137.21(11) 4_576 . ? O2 Tb1 O4 95.44(11) . . ? O12 Tb1 C17 100.05(13) . 4_576 ? O13 Tb1 C17 78.46(12) . 4_576 ? O14 Tb1 C17 78.81(12) . 4_576 ? O8 Tb1 C17 26.80(11) 4_576 4_576 ? O1 Tb1 C17 102.87(13) . 4_576 ? O5 Tb1 C17 153.76(12) . 4_576 ? O7 Tb1 C17 26.41(11) 4_576 4_576 ? O2 Tb1 C17 102.58(12) . 4_576 ? O4 Tb1 C17 152.33(11) . 4_576 ? O1 C1 O2 120.5(4) . . ? O1 C1 C2 121.5(4) . . ? O2 C1 C2 118.0(4) . . ? C3 C2 C7 118.1(4) . . ? C3 C2 C1 118.6(4) . . ? C7 C2 C1 123.3(4) . . ? C2 C3 C4 121.4(5) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 119.7(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.5(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 119.8(5) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? O3 C7 C2 116.2(4) . . ? O3 C7 C6 123.4(4) . . ? C2 C7 C6 120.4(4) . . ? O3 C8 C25 106.6(4) . . ? O3 C8 H8A 110.4 . . ? C25 C8 H8A 110.4 . . ? O3 C8 H8B 110.4 . . ? C25 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? O5 C9 O4 121.7(4) . . ? O5 C9 C10 118.0(4) . . ? O4 C9 C10 120.2(4) . . ? C15 C10 C11 118.0(4) . . ? C15 C10 C9 122.9(4) . . ? C11 C10 C9 119.1(4) . . ? C12 C11 C10 121.4(6) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C13 C12 C11 118.5(6) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C14 C13 C12 121.2(6) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.4(6) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C10 C15 C14 121.1(6) . . ? C10 C15 O6 114.2(4) . . ? C14 C15 O6 124.5(6) . . ? O6 C16 C25 107.9(4) . . ? O6 C16 H16A 110.1 . . ? C25 C16 H16A 110.1 . . ? O6 C16 H16B 110.1 . . ? C25 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? O7 C17 O8 120.9(4) . . ? O7 C17 C18 122.3(4) . . ? O8 C17 C18 116.8(4) . . ? O7 C17 Tb1 62.1(2) . 4_575 ? O8 C17 Tb1 58.8(2) . 4_575 ? C18 C17 Tb1 175.5(3) . 4_575 ? C19 C18 C23 118.7(4) . . ? C19 C18 C17 118.0(4) . . ? C23 C18 C17 123.3(4) . . ? C18 C19 C20 121.2(5) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 119.3(6) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 120.2(6) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.4(5) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? O9 C23 C22 123.6(4) . . ? O9 C23 C18 116.4(4) . . ? C22 C23 C18 120.0(4) . . ? O9 C24 C25 103.9(3) . . ? O9 C24 H24A 111.0 . . ? C25 C24 H24A 111.0 . . ? O9 C24 H24B 111.0 . . ? C25 C24 H24B 111.0 . . ? H24A C24 H24B 109.0 . . ? N1 C25 C16 106.2(4) . . ? N1 C25 C8 111.6(4) . . ? C16 C25 C8 114.5(4) . . ? N1 C25 C24 111.4(3) . . ? C16 C25 C24 104.4(4) . . ? C8 C25 C24 108.6(4) . . ? C27 C26 C31 119.1(5) . . ? C27 C26 S1 120.2(4) . . ? C31 C26 S1 120.5(4) . . ? C26 C27 C28 120.3(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 120.8(5) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 118.2(5) . . ? C28 C29 C32 120.9(5) . . ? C30 C29 C32 120.9(5) . . ? C31 C30 C29 122.1(5) . . ? C31 C30 H30 118.9 . . ? C29 C30 H30 118.9 . . ? C30 C31 C26 119.4(5) . . ? C30 C31 H31 120.3 . . ? C26 C31 H31 120.3 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O12 C33 N2 132.1(7) . . ? O12 C33 H33 113.9 . . ? N2 C33 H33 113.9 . . ? O15 C36 N3 125.6(7) . . ? O15 C36 H36 117.2 . . ? N3 C36 H36 117.2 . . ? N3 C37 H37A 109.5 . . ? N3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N3 C38 H38A 109.5 . . ? N3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C34A H34A 108.8 . . ? N2 C34A H34B 112.1 . . ? H34A C34A H34B 110.5 . . ? N2 C34A H34C 108.0 . . ? H34A C34A H34C 107.7 . . ? H34B C34A H34C 109.6 . . ? N2 C34A H34E 106.4 . . ? H34A C34A H34E 82.0 . . ? H34B C34A H34E 131.9 . . ? N2 C35A H35A 113.2 . . ? N2 C35A H35B 107.3 . . ? H35A C35A H35B 108.8 . . ? N2 C35A H35C 110.0 . . ? H35A C35A H35C 109.7 . . ? H35B C35A H35C 107.7 . . ? N2 C35A H35D 84.5 . . ? H35A C35A H35D 94.6 . . ? H35C C35A H35D 142.3 . . ? N2 C35A H35F 118.2 . . ? H35A C35A H35F 128.5 . . ? H35B C35A H35F 52.0 . . ? H35C C35A H35F 55.9 . . ? H35D C35A H35F 86.4 . . ? N2 C34B H34C 91.8 . . ? N2 C34B H34D 111.8 . . ? H34C C34B H34D 135.4 . . ? N2 C34B H34E 109.2 . . ? H34D C34B H34E 108.8 . . ? N2 C34B H34F 111.5 . . ? H34C C34B H34F 99.3 . . ? H34D C34B H34F 105.7 . . ? H34E C34B H34F 109.8 . . ? N2 C35B H35B 141.0 . . ? N2 C35B H35C 85.4 . . ? H35B C35B H35C 75.6 . . ? N2 C35B H35D 109.9 . . ? H35B C35B H35D 58.3 . . ? H35C C35B H35D 123.5 . . ? N2 C35B H35E 106.3 . . ? H35B C35B H35E 112.7 . . ? H35C C35B H35E 116.9 . . ? H35D C35B H35E 110.2 . . ? N2 C35B H35F 112.0 . . ? H35B C35B H35F 53.5 . . ? H35D C35B H35F 109.8 . . ? H35E C35B H35F 108.5 . . ? C25 N1 S1 128.3(3) . . ? C25 N1 H1 115.9 . . ? S1 N1 H1 115.9 . . ? C33 N2 C34A 118.3(9) . . ? C33 N2 C35B 132.8(9) . . ? C34A N2 C35B 88.9(11) . . ? C33 N2 C34B 111.2(8) . . ? C34A N2 C34B 58.2(9) . . ? C35B N2 C34B 115.9(9) . . ? C33 N2 C35A 122.1(9) . . ? C34A N2 C35A 118.0(9) . . ? C34B N2 C35A 108.7(10) . . ? C36 N3 C37 121.9(8) . . ? C36 N3 C38 121.0(8) . . ? C37 N3 C38 116.9(8) . . ? C1 O1 Tb1 94.1(3) . . ? C1 O2 Tb1 91.6(2) . . ? C7 O3 C8 119.9(3) . . ? C9 O4 Tb1 92.1(3) . . ? C9 O5 Tb1 94.0(3) . . ? C16 O6 C15 119.8(5) . . ? C17 O7 Tb1 91.5(2) . 4_575 ? C17 O8 Tb1 94.4(3) . 4_575 ? C23 O9 C24 119.4(3) . . ? C33 O12 Tb1 136.2(5) . . ? Tb1 O13 H1W 117.7 . . ? Tb1 O13 H2W 109.5 . . ? H1W O13 H2W 114.5 . . ? Tb1 O14 H3W 116.3 . . ? Tb1 O14 H4W 118.1 . . ? H3W O14 H4W 114.6 . . ? O11 S1 O10 118.29(18) . . ? O11 S1 N1 108.40(18) . . ? O10 S1 N1 104.51(19) . . ? O11 S1 C26 107.1(2) . . ? O10 S1 C26 107.0(2) . . ? N1 S1 C26 111.58(19) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.499 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.115 #==END data_5 _database_code_depnum_ccdc_archive 'CCDC 731526' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H44 N3 O15 S Y' _chemical_formula_weight 903.73 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' Y Y -2.7962 3.5667 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.594(8) _cell_length_b 13.806(7) _cell_length_c 19.560(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.657(8) _cell_angle_gamma 90.00 _cell_volume 4163(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2484 _cell_measurement_theta_min 2.312 _cell_measurement_theta_max 25.411 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.522 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7722 _exptl_absorpt_correction_T_max 0.8758 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21655 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.1081 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7328 _reflns_number_gt 3736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.0329P)^2^+9.9120P] 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 7328 _refine_ls_number_parameters 545 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1346 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.985 _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 Y1 Y 0.63255(4) 0.90039(4) 0.59176(3) 0.03781(18) Uani 1 1 d . . 1 C1 C 0.6945(4) 0.9242(4) 0.4666(3) 0.0384(15) Uani 1 1 d . . 1 C2 C 0.7166(4) 0.9256(4) 0.3947(3) 0.0404(15) Uani 1 1 d . . 1 C3 C 0.7047(4) 1.0093(5) 0.3567(3) 0.0587(19) Uani 1 1 d . . 1 H3 H 0.6839 1.0641 0.3764 0.070 Uiso 1 1 calc R . 1 C4 C 0.7231(5) 1.0141(6) 0.2892(4) 0.077(2) Uani 1 1 d . . 1 H4 H 0.7130 1.0710 0.2637 0.092 Uiso 1 1 calc R . 1 C5 C 0.7562(5) 0.9345(5) 0.2608(4) 0.067(2) Uani 1 1 d . . 1 H5 H 0.7714 0.9382 0.2167 0.080 Uiso 1 1 calc R . 1 C6 C 0.7669(4) 0.8491(5) 0.2968(3) 0.0561(19) Uani 1 1 d . . 1 H6 H 0.7879 0.7948 0.2766 0.067 Uiso 1 1 calc R . 1 C7 C 0.7466(4) 0.8438(5) 0.3632(3) 0.0439(16) Uani 1 1 d . . 1 C8 C 0.7732(4) 0.6716(4) 0.3707(3) 0.0513(18) Uani 1 1 d . . 1 H8A H 0.8354 0.6687 0.3712 0.062 Uiso 1 1 calc R . 1 H8B H 0.7449 0.6666 0.3231 0.062 Uiso 1 1 calc R . 1 C9 C 0.5372(4) 0.7555(5) 0.5124(3) 0.0466(16) Uani 1 1 d . . 1 C10 C 0.4812(4) 0.6813(5) 0.4710(3) 0.0459(16) Uani 1 1 d . . 1 C11 C 0.3932(4) 0.6789(5) 0.4743(4) 0.062(2) Uani 1 1 d . . 1 H11 H 0.3683 0.7270 0.4981 0.074 Uiso 1 1 calc R . 1 C12 C 0.3426(5) 0.6056(7) 0.4425(4) 0.082(2) Uani 1 1 d . . 1 H12 H 0.2836 0.6042 0.4449 0.098 Uiso 1 1 calc R . 1 C13 C 0.3791(6) 0.5342(6) 0.4071(5) 0.088(3) Uani 1 1 d . . 1 H13 H 0.3453 0.4825 0.3882 0.105 Uiso 1 1 calc R . 1 C14 C 0.4651(6) 0.5390(6) 0.3995(4) 0.094(3) Uani 1 1 d . . 1 H14 H 0.4891 0.4930 0.3734 0.112 Uiso 1 1 calc R . 1 C15 C 0.5151(4) 0.6129(6) 0.4313(4) 0.068(2) Uani 1 1 d . . 1 C16 C 0.6480(5) 0.5641(6) 0.3957(4) 0.077(2) Uani 1 1 d . . 1 H16A H 0.6319 0.5600 0.3459 0.093 Uiso 1 1 calc R . 1 H16B H 0.6370 0.5017 0.4155 0.093 Uiso 1 1 calc R . 1 C17 C 0.7196(4) 0.4653(5) 0.1830(3) 0.0427(16) Uani 1 1 d . . 1 C18 C 0.7674(4) 0.3896(5) 0.2277(3) 0.0464(16) Uani 1 1 d . . 1 C19 C 0.7885(5) 0.3060(5) 0.1969(4) 0.071(2) Uani 1 1 d U . 1 H19 H 0.7713 0.2989 0.1495 0.085 Uiso 1 1 calc R . 1 C20 C 0.8342(5) 0.2317(6) 0.2327(4) 0.089(3) Uani 1 1 d U . 1 H20 H 0.8475 0.1756 0.2101 0.107 Uiso 1 1 calc R . 1 C21 C 0.8595(5) 0.2428(6) 0.3025(4) 0.087(3) Uani 1 1 d U . 1 H21 H 0.8902 0.1935 0.3277 0.104 Uiso 1 1 calc R . 1 C22 C 0.8401(5) 0.3261(5) 0.3357(4) 0.072(2) Uani 1 1 d U . 1 H22 H 0.8590 0.3339 0.3827 0.087 Uiso 1 1 calc R . 1 C23 C 0.7921(4) 0.3981(5) 0.2984(3) 0.0528(17) Uani 1 1 d . . 1 C24 C 0.7924(5) 0.4970(5) 0.3998(3) 0.062(2) Uani 1 1 d . . 1 H24A H 0.8546 0.5055 0.4117 0.075 Uiso 1 1 calc R . 1 H24B H 0.7743 0.4431 0.4261 0.075 Uiso 1 1 calc R . 1 C25 C 0.7441(4) 0.5894(5) 0.4135(3) 0.0460(16) Uani 1 1 d . . 1 C26 C 0.9259(4) 0.6878(5) 0.5206(3) 0.0443(16) Uani 1 1 d . . 1 C27 C 0.9947(4) 0.6531(5) 0.4908(3) 0.0565(19) Uani 1 1 d . . 1 H27 H 0.9967 0.5884 0.4781 0.068 Uiso 1 1 calc R . 1 C28 C 1.0605(4) 0.7157(6) 0.4800(4) 0.063(2) Uani 1 1 d . . 1 H28 H 1.1062 0.6920 0.4593 0.076 Uiso 1 1 calc R . 1 C29 C 1.0608(5) 0.8113(6) 0.4986(4) 0.0590(19) Uani 1 1 d . . 1 C30 C 0.9901(5) 0.8442(6) 0.5260(4) 0.077(2) Uani 1 1 d . . 1 H30 H 0.9878 0.9093 0.5377 0.093 Uiso 1 1 calc R . 1 C31 C 0.9227(5) 0.7848(5) 0.5369(4) 0.068(2) Uani 1 1 d . . 1 H31 H 0.8756 0.8097 0.5551 0.081 Uiso 1 1 calc R . 1 C32 C 1.1369(5) 0.8763(6) 0.4918(4) 0.088(3) Uani 1 1 d . . 1 H32A H 1.1864 0.8557 0.5237 0.132 Uiso 1 1 calc R . 1 H32B H 1.1227 0.9419 0.5019 0.132 Uiso 1 1 calc R . 1 H32C H 1.1500 0.8726 0.4454 0.132 Uiso 1 1 calc R . 1 C33 C 0.5471(6) 0.7685(7) 0.7041(5) 0.093(3) Uani 1 1 d U . 1 H33 H 0.6034 0.7465 0.7178 0.112 Uiso 1 1 calc R . 1 C36 C 0.9139(6) -0.0648(8) 0.7028(5) 0.087(3) Uani 1 1 d . A 1 H36 H 0.8906 -0.0527 0.6570 0.104 Uiso 1 1 calc R A 1 C37 C 1.0135(6) -0.0154(9) 0.8029(5) 0.150(5) Uani 1 1 d . A 1 H37A H 0.9962 0.0393 0.8280 0.226 Uiso 1 1 calc R A 1 H37B H 1.0756 -0.0173 0.8073 0.226 Uiso 1 1 calc R A 1 H37C H 0.9929 -0.0739 0.8215 0.226 Uiso 1 1 calc R A 1 C38 C 1.0054(8) 0.0714(9) 0.6930(7) 0.178(5) Uani 1 1 d U A 1 H38A H 0.9917 0.0566 0.6446 0.267 Uiso 1 1 calc R A 1 H38B H 1.0669 0.0803 0.7049 0.267 Uiso 1 1 calc R A 1 H38C H 0.9760 0.1297 0.7028 0.267 Uiso 1 1 calc R A 1 C34A C 0.4981(13) 0.6788(17) 0.7990(8) 0.110(8) Uani 0.486(15) 1 d PDU . 1 H34A H 0.5557 0.6860 0.8227 0.132 Uiso 0.486(15) 1 d PR . 1 H34B H 0.4857 0.6110 0.7907 0.132 Uiso 0.486(15) 1 d PR . 1 H34C H 0.4577 0.7040 0.8267 0.132 Uiso 0.486(15) 1 d PR . 1 C35A C 0.4048(10) 0.7193(16) 0.6894(9) 0.121(9) Uani 0.486(15) 1 d PDU . 1 H35A H 0.3905 0.6519 0.6786 0.145 Uiso 0.486(15) 1 d PR . 1 H35B H 0.4045 0.7549 0.6466 0.145 Uiso 0.486(15) 1 d PR . 1 H35C H 0.3615 0.7459 0.7136 0.145 Uiso 0.486(15) 1 d PR . 1 C34B C 0.5064(12) 0.6299(11) 0.7691(10) 0.104(7) Uani 0.514(15) 1 d PDU . 2 H34D H 0.5572 0.5991 0.7573 0.125 Uiso 0.514(15) 1 d PR . 2 H34E H 0.4572 0.5881 0.7543 0.125 Uiso 0.514(15) 1 d PR . 2 H34F H 0.5122 0.6391 0.8173 0.125 Uiso 0.514(15) 1 d PR . 2 C35B C 0.4196(11) 0.7803(12) 0.7475(11) 0.117(8) Uani 0.514(15) 1 d PDU . 2 H35D H 0.4166 0.8395 0.7214 0.140 Uiso 0.514(15) 1 d PR . 2 H35E H 0.3676 0.7425 0.7324 0.140 Uiso 0.514(15) 1 d PR . 2 H35F H 0.4226 0.7935 0.7954 0.140 Uiso 0.514(15) 1 d PR . 2 N1 N 0.7581(3) 0.6150(3) 0.4879(2) 0.0432(13) Uani 1 1 d . . 1 H1 H 0.7133 0.6364 0.5041 0.052 Uiso 1 1 calc R . 1 N2 N 0.4911(4) 0.7267(5) 0.7344(3) 0.079(2) Uani 1 1 d D . 1 N3 N 0.9780(5) -0.0070(6) 0.7327(4) 0.102(2) Uani 1 1 d . A 1 O1 O 0.7344(3) 0.8722(3) 0.5126(2) 0.0535(12) Uani 1 1 d . . 1 O2 O 0.6343(3) 0.9791(3) 0.47934(19) 0.0507(11) Uani 1 1 d . . 1 O3 O 0.7501(3) 0.7600(3) 0.4002(2) 0.0681(14) Uani 1 1 d . . 1 O4 O 0.6095(3) 0.7336(3) 0.5452(2) 0.0585(13) Uani 1 1 d . . 1 O5 O 0.5065(3) 0.8400(3) 0.5147(2) 0.0586(13) Uani 1 1 d . . 1 O6 O 0.6008(3) 0.6326(4) 0.4210(3) 0.0877(18) Uani 1 1 d . . 1 O7 O 0.6697(3) 0.5239(3) 0.20643(19) 0.0492(11) Uani 1 1 d . . 1 O8 O 0.7307(3) 0.4696(3) 0.1201(2) 0.0562(13) Uani 1 1 d . . 1 O9 O 0.7688(3) 0.4816(3) 0.3278(2) 0.0645(14) Uani 1 1 d . . 1 O10 O 0.8221(3) 0.6411(3) 0.60654(19) 0.0500(11) Uani 1 1 d . . 1 O11 O 0.8806(3) 0.5121(3) 0.5395(2) 0.0505(11) Uani 1 1 d . . 1 O12 O 0.5414(3) 0.8296(3) 0.6622(2) 0.0641(13) Uani 1 1 d . . 1 O13 O 0.5313(2) 1.0252(3) 0.58757(19) 0.0490(11) Uani 1 1 d . . 1 H1W H 0.5407 1.0697 0.5599 0.059 Uiso 1 1 d R . 1 H2W H 0.4806 1.0024 0.5826 0.059 Uiso 1 1 d R . 1 O14 O 0.7391(3) 0.8018(3) 0.65595(19) 0.0503(11) Uani 1 1 d . . 1 H3W H 0.7793 0.8289 0.6838 0.060 Uiso 1 1 d R . 1 H4W H 0.7497 0.7446 0.6416 0.060 Uiso 1 1 d R . 1 O15 O 0.8845(4) -0.1324(5) 0.7322(3) 0.097(2) Uani 1 1 d . A 1 S1 S 0.84553(10) 0.60808(12) 0.54216(8) 0.0439(4) Uani 1 1 d . . 1 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 Y1 0.0412(3) 0.0434(3) 0.0283(3) 0.0008(3) 0.0031(2) 0.0006(3) C1 0.040(4) 0.039(4) 0.034(4) -0.003(3) 0.002(3) -0.007(3) C2 0.044(4) 0.046(4) 0.032(3) 0.002(3) 0.006(3) 0.004(3) C3 0.077(5) 0.056(5) 0.046(4) 0.007(4) 0.020(4) 0.010(4) C4 0.113(7) 0.066(6) 0.056(5) 0.021(4) 0.025(5) 0.018(5) C5 0.093(6) 0.070(5) 0.042(4) 0.007(4) 0.028(4) 0.010(4) C6 0.072(5) 0.060(5) 0.040(4) -0.001(4) 0.021(4) 0.012(4) C7 0.052(4) 0.047(4) 0.032(4) 0.009(3) 0.003(3) 0.011(3) C8 0.076(5) 0.044(4) 0.034(4) -0.005(3) 0.009(3) 0.009(4) C9 0.049(4) 0.053(5) 0.036(4) 0.002(3) 0.004(3) -0.001(4) C10 0.041(4) 0.048(4) 0.045(4) -0.003(3) -0.004(3) -0.009(3) C11 0.047(5) 0.069(5) 0.066(5) -0.008(4) 0.001(4) -0.015(4) C12 0.053(5) 0.100(7) 0.088(6) 0.000(6) -0.004(4) -0.012(5) C13 0.071(6) 0.077(6) 0.104(7) -0.004(6) -0.023(5) -0.027(5) C14 0.067(6) 0.093(7) 0.113(7) -0.052(6) -0.016(5) -0.010(5) C15 0.041(4) 0.083(6) 0.074(5) -0.030(5) -0.011(4) -0.008(4) C16 0.064(5) 0.093(6) 0.065(5) -0.024(5) -0.022(4) 0.014(5) C17 0.041(4) 0.046(4) 0.039(4) 0.003(3) 0.001(3) -0.006(3) C18 0.059(4) 0.042(4) 0.037(4) 0.002(3) 0.003(3) 0.006(3) C19 0.084(4) 0.064(4) 0.063(4) 0.003(3) 0.007(3) 0.012(3) C20 0.110(5) 0.079(4) 0.076(4) -0.005(4) 0.007(4) 0.021(4) C21 0.106(5) 0.069(4) 0.081(4) 0.002(4) 0.000(4) 0.023(4) C22 0.087(4) 0.066(4) 0.059(4) -0.003(3) -0.006(3) 0.015(3) C23 0.066(5) 0.045(4) 0.045(4) -0.003(4) -0.002(3) 0.005(4) C24 0.098(6) 0.049(4) 0.034(4) -0.004(3) -0.012(4) 0.004(4) C25 0.050(4) 0.049(4) 0.035(4) -0.004(3) -0.008(3) 0.003(3) C26 0.044(4) 0.050(4) 0.039(4) 0.001(3) 0.004(3) 0.008(3) C27 0.055(5) 0.055(5) 0.059(5) -0.004(4) 0.008(4) 0.014(4) C28 0.049(5) 0.079(6) 0.066(5) -0.001(4) 0.021(4) 0.006(4) C29 0.056(5) 0.066(5) 0.055(5) 0.007(4) 0.008(4) -0.001(4) C30 0.076(6) 0.055(5) 0.104(7) -0.012(5) 0.021(5) 0.001(5) C31 0.054(5) 0.058(5) 0.095(6) -0.009(4) 0.025(4) 0.009(4) C32 0.082(6) 0.097(7) 0.090(6) -0.002(5) 0.030(5) -0.021(5) C33 0.081(4) 0.108(5) 0.090(5) 0.025(4) 0.007(4) -0.013(4) C36 0.055(6) 0.127(9) 0.074(7) -0.013(6) -0.005(5) 0.015(6) C37 0.090(8) 0.223(14) 0.121(9) -0.079(9) -0.042(7) 0.013(8) C38 0.168(7) 0.179(7) 0.184(7) 0.014(5) 0.020(5) -0.012(5) C34A 0.113(9) 0.112(9) 0.104(9) 0.010(5) 0.018(5) -0.011(5) C35A 0.118(10) 0.125(10) 0.121(10) 0.007(5) 0.020(5) -0.012(5) C34B 0.106(8) 0.103(8) 0.105(8) 0.010(5) 0.022(5) 0.000(5) C35B 0.114(9) 0.118(9) 0.121(9) -0.002(5) 0.027(5) 0.002(5) N1 0.041(3) 0.055(4) 0.033(3) 0.003(3) 0.004(2) 0.012(3) N2 0.073(5) 0.096(5) 0.071(5) 0.034(4) 0.016(4) -0.022(4) N3 0.062(5) 0.126(7) 0.112(7) -0.013(6) -0.002(5) -0.016(5) O1 0.064(3) 0.065(3) 0.033(2) 0.009(2) 0.010(2) 0.025(2) O2 0.055(3) 0.063(3) 0.035(2) 0.005(2) 0.008(2) 0.018(2) O3 0.124(4) 0.045(3) 0.041(3) 0.001(2) 0.029(3) 0.023(3) O4 0.051(3) 0.049(3) 0.069(3) -0.011(2) -0.013(3) 0.003(2) O5 0.063(3) 0.045(3) 0.060(3) 0.000(2) -0.013(2) 0.003(2) O6 0.061(4) 0.095(4) 0.101(4) -0.050(3) -0.008(3) 0.009(3) O7 0.054(3) 0.058(3) 0.036(2) 0.000(2) 0.008(2) 0.009(2) O8 0.076(3) 0.069(3) 0.024(2) 0.011(2) 0.012(2) 0.022(3) O9 0.108(4) 0.048(3) 0.031(3) -0.008(2) -0.014(2) 0.021(3) O10 0.059(3) 0.061(3) 0.030(2) -0.002(2) 0.005(2) 0.013(2) O11 0.060(3) 0.040(3) 0.051(3) -0.002(2) 0.005(2) 0.020(2) O12 0.062(3) 0.069(3) 0.064(3) 0.017(3) 0.018(3) -0.013(3) O13 0.048(3) 0.059(3) 0.039(2) 0.004(2) 0.004(2) 0.005(2) O14 0.064(3) 0.044(3) 0.039(3) 0.002(2) -0.004(2) 0.008(2) O15 0.080(4) 0.125(6) 0.080(5) -0.007(4) -0.004(3) -0.011(4) S1 0.0473(10) 0.0484(10) 0.0347(9) 0.0002(8) 0.0020(7) 0.0090(8) _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 Y1 O13 2.331(4) . ? Y1 O12 2.337(4) . ? Y1 O14 2.358(4) . ? Y1 O8 2.369(4) 4_576 ? Y1 O1 2.411(4) . ? Y1 O5 2.438(4) . ? Y1 O2 2.457(4) . ? Y1 O7 2.463(4) 4_576 ? Y1 O4 2.482(4) . ? Y1 C17 2.781(6) 4_576 ? C1 O1 1.242(6) . ? C1 O2 1.261(6) . ? C1 C2 1.498(8) . ? C2 C3 1.370(8) . ? C2 C7 1.400(8) . ? C3 C4 1.395(8) . ? C3 H3 0.9300 . ? C4 C5 1.368(9) . ? C4 H4 0.9300 . ? C5 C6 1.370(9) . ? C5 H5 0.9300 . ? C6 C7 1.385(8) . ? C6 H6 0.9300 . ? C7 O3 1.361(7) . ? C8 O3 1.420(7) . ? C8 C25 1.519(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O4 1.247(7) . ? C9 O5 1.264(7) . ? C9 C10 1.502(8) . ? C10 C15 1.377(9) . ? C10 C11 1.383(8) . ? C11 C12 1.373(9) . ? C11 H11 0.9300 . ? C12 C13 1.375(10) . ? C12 H12 0.9300 . ? C13 C14 1.373(10) . ? C13 H13 0.9300 . ? C14 C15 1.374(9) . ? C14 H14 0.9300 . ? C15 O6 1.408(8) . ? C16 O6 1.338(8) . ? C16 C25 1.528(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O7 1.256(7) . ? C17 O8 1.269(6) . ? C17 C18 1.489(8) . ? C17 Y1 2.781(6) 4_575 ? C18 C19 1.365(9) . ? C18 C23 1.383(8) . ? C19 C20 1.378(9) . ? C19 H19 0.9300 . ? C20 C21 1.372(10) . ? C20 H20 0.9300 . ? C21 C22 1.376(9) . ? C21 H21 0.9300 . ? C22 C23 1.384(9) . ? C22 H22 0.9300 . ? C23 O9 1.363(7) . ? C24 O9 1.417(7) . ? C24 C25 1.525(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N1 1.483(7) . ? C26 C31 1.379(8) . ? C26 C27 1.382(8) . ? C26 S1 1.766(6) . ? C27 C28 1.381(9) . ? C27 H27 0.9300 . ? C28 C29 1.369(9) . ? C28 H28 0.9300 . ? C29 C30 1.373(9) . ? C29 C32 1.510(9) . ? C30 C31 1.375(9) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 O12 1.171(9) . ? C33 N2 1.266(9) . ? C33 H33 0.9300 . ? C36 O15 1.221(10) . ? C36 N3 1.342(10) . ? C36 H36 0.9300 . ? C37 N3 1.406(11) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 N3 1.435(12) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C34A N2 1.416(13) . ? C34A H34A 0.9505 . ? C34A H34B 0.9659 . ? C34A H34C 0.9560 . ? C35A N2 1.497(13) . ? C35A H35A 0.9729 . ? C35A H35B 0.9697 . ? C35A H35C 0.9537 . ? C34B H34D 0.9564 . ? C34B H34E 0.9692 . ? C34B H34F 0.9425 . ? C35B H35D 0.9611 . ? C35B H35E 0.9725 . ? C35B H35F 0.9484 . ? N1 S1 1.600(5) . ? N1 H1 0.8600 . ? O7 Y1 2.463(4) 4_575 ? O8 Y1 2.369(4) 4_575 ? O10 S1 1.437(4) . ? O11 S1 1.438(4) . ? O13 H1W 0.8454 . ? O13 H2W 0.8423 . ? O14 H3W 0.8528 . ? O14 H4W 0.8635 . ? 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 O13 Y1 O12 82.02(16) . . ? O13 Y1 O14 149.86(13) . . ? O12 Y1 O14 83.51(16) . . ? O13 Y1 O8 81.87(15) . 4_576 ? O12 Y1 O8 127.44(15) . 4_576 ? O14 Y1 O8 86.23(15) . 4_576 ? O13 Y1 O1 127.25(14) . . ? O12 Y1 O1 145.97(16) . . ? O14 Y1 O1 76.66(14) . . ? O8 Y1 O1 78.91(15) 4_576 . ? O13 Y1 O5 75.64(15) . . ? O12 Y1 O5 73.50(16) . . ? O14 Y1 O5 124.75(15) . . ? O8 Y1 O5 146.73(15) 4_576 . ? O1 Y1 O5 95.48(16) . . ? O13 Y1 O2 74.93(14) . . ? O12 Y1 O2 143.33(15) . . ? O14 Y1 O2 129.07(14) . . ? O8 Y1 O2 77.31(14) 4_576 . ? O1 Y1 O2 53.10(13) . . ? O5 Y1 O2 73.39(15) . . ? O13 Y1 O7 77.50(13) . 4_576 ? O12 Y1 O7 73.85(15) . 4_576 ? O14 Y1 O7 73.12(14) . 4_576 ? O8 Y1 O7 53.88(13) 4_576 4_576 ? O1 Y1 O7 124.45(15) . 4_576 ? O5 Y1 O7 139.98(15) . 4_576 ? O2 Y1 O7 126.47(15) . 4_576 ? O13 Y1 O4 127.80(15) . . ? O12 Y1 O4 76.16(16) . . ? O14 Y1 O4 73.25(15) . . ? O8 Y1 O4 147.27(15) 4_576 . ? O1 Y1 O4 71.80(15) . . ? O5 Y1 O4 52.90(14) . . ? O2 Y1 O4 95.88(15) . . ? O7 Y1 O4 136.81(15) 4_576 . ? O13 Y1 C17 78.01(16) . 4_576 ? O12 Y1 C17 100.51(18) . 4_576 ? O14 Y1 C17 78.85(16) . 4_576 ? O8 Y1 C17 27.04(15) 4_576 4_576 ? O1 Y1 C17 102.39(17) . 4_576 ? O5 Y1 C17 153.53(16) . 4_576 ? O2 Y1 C17 102.06(17) . 4_576 ? O7 Y1 C17 26.84(14) 4_576 4_576 ? O4 Y1 C17 152.09(16) . 4_576 ? O1 C1 O2 120.8(5) . . ? O1 C1 C2 121.8(6) . . ? O2 C1 C2 117.5(5) . . ? C3 C2 C7 117.9(6) . . ? C3 C2 C1 119.3(6) . . ? C7 C2 C1 122.8(5) . . ? C2 C3 C4 121.6(7) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 119.3(7) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.4(6) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 120.1(6) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? O3 C7 C6 123.2(6) . . ? O3 C7 C2 116.2(5) . . ? C6 C7 C2 120.5(6) . . ? O3 C8 C25 107.7(5) . . ? O3 C8 H8A 110.2 . . ? C25 C8 H8A 110.2 . . ? O3 C8 H8B 110.2 . . ? C25 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? O4 C9 O5 121.6(6) . . ? O4 C9 C10 121.3(6) . . ? O5 C9 C10 117.1(6) . . ? C15 C10 C11 118.5(6) . . ? C15 C10 C9 122.0(6) . . ? C11 C10 C9 119.5(6) . . ? C12 C11 C10 120.2(7) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.2(7) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 120.3(8) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 118.9(8) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C14 C15 C10 121.6(7) . . ? C14 C15 O6 124.4(7) . . ? C10 C15 O6 113.7(6) . . ? O6 C16 C25 109.3(6) . . ? O6 C16 H16A 109.8 . . ? C25 C16 H16A 109.8 . . ? O6 C16 H16B 109.8 . . ? C25 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? O7 C17 O8 120.4(6) . . ? O7 C17 C18 121.3(6) . . ? O8 C17 C18 118.3(6) . . ? O7 C17 Y1 62.3(3) . 4_575 ? O8 C17 Y1 58.1(3) . 4_575 ? C18 C17 Y1 176.2(5) . 4_575 ? C19 C18 C23 117.7(6) . . ? C19 C18 C17 117.8(6) . . ? C23 C18 C17 124.6(6) . . ? C18 C19 C20 123.0(7) . . ? C18 C19 H19 118.5 . . ? C20 C19 H19 118.5 . . ? C21 C20 C19 118.2(8) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C20 C21 C22 120.8(8) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C23 119.4(7) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? O9 C23 C18 116.2(6) . . ? O9 C23 C22 122.9(6) . . ? C18 C23 C22 120.9(7) . . ? O9 C24 C25 103.8(5) . . ? O9 C24 H24A 111.0 . . ? C25 C24 H24A 111.0 . . ? O9 C24 H24B 111.0 . . ? C25 C24 H24B 111.0 . . ? H24A C24 H24B 109.0 . . ? N1 C25 C8 110.6(5) . . ? N1 C25 C24 111.7(5) . . ? C8 C25 C24 109.4(5) . . ? N1 C25 C16 105.7(5) . . ? C8 C25 C16 114.1(5) . . ? C24 C25 C16 105.2(6) . . ? C31 C26 C27 119.4(6) . . ? C31 C26 S1 119.9(5) . . ? C27 C26 S1 120.6(5) . . ? C28 C27 C26 119.4(7) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 122.3(7) . . ? C29 C28 H28 118.8 . . ? C27 C28 H28 118.8 . . ? C28 C29 C30 116.9(7) . . ? C28 C29 C32 121.4(7) . . ? C30 C29 C32 121.7(7) . . ? C29 C30 C31 122.7(7) . . ? C29 C30 H30 118.6 . . ? C31 C30 H30 118.6 . . ? C30 C31 C26 119.3(7) . . ? C30 C31 H31 120.4 . . ? C26 C31 H31 120.4 . . ? O12 C33 N2 132.2(9) . . ? O12 C33 H33 113.9 . . ? N2 C33 H33 113.9 . . ? O15 C36 N3 123.9(9) . . ? O15 C36 H36 118.0 . . ? N3 C36 H36 118.0 . . ? N2 C34A H34A 109.1 . . ? N2 C34A H34B 108.3 . . ? H34A C34A H34B 109.5 . . ? N2 C34A H34C 111.5 . . ? H34A C34A H34C 110.0 . . ? H34B C34A H34C 108.3 . . ? N2 C34A H34F 146.0 . . ? H34A C34A H34F 67.6 . . ? H34B C34A H34F 48.7 . . ? H34C C34A H34F 100.7 . . ? N2 C35A H35A 110.4 . . ? N2 C35A H35B 111.1 . . ? H35A C35A H35B 109.1 . . ? N2 C35A H35C 108.8 . . ? H35A C35A H35C 108.7 . . ? H35B C35A H35C 108.8 . . ? N2 C35A H35E 93.3 . . ? H35A C35A H35E 107.7 . . ? H35B C35A H35E 124.1 . . ? H34A C34B H34B 90.3 . . ? H34A C34B H34D 92.6 . . ? H34B C34B H34D 120.5 . . ? H34A C34B H34E 148.7 . . ? H34B C34B H34E 59.1 . . ? H34D C34B H34E 108.1 . . ? H34B C34B H34F 50.4 . . ? H34D C34B H34F 110.1 . . ? H34E C34B H34F 109.3 . . ? H35C C35B H35D 94.2 . . ? H35D C35B H35E 108.8 . . ? H35C C35B H35F 124.7 . . ? H35D C35B H35F 110.7 . . ? H35E C35B H35F 108.5 . . ? C25 N1 S1 128.4(4) . . ? C25 N1 H1 115.8 . . ? S1 N1 H1 115.8 . . ? C33 N2 C34A 131.6(11) . . ? C33 N2 C35A 112.2(9) . . ? C34A N2 C35A 115.9(11) . . ? C36 N3 C37 122.3(9) . . ? C36 N3 C38 118.4(10) . . ? C37 N3 C38 119.1(9) . . ? C1 O1 Y1 93.7(4) . . ? C1 O2 Y1 91.1(3) . . ? C7 O3 C8 120.5(5) . . ? C9 O4 Y1 91.9(4) . . ? C9 O5 Y1 93.6(4) . . ? C16 O6 C15 120.3(6) . . ? C17 O7 Y1 90.8(3) . 4_575 ? C17 O8 Y1 94.9(4) . 4_575 ? C23 O9 C24 120.0(5) . . ? C33 O12 Y1 136.5(6) . . ? Y1 O13 H1W 112.1 . . ? Y1 O13 H2W 110.2 . . ? H1W O13 H2W 116.7 . . ? Y1 O14 H3W 118.7 . . ? Y1 O14 H4W 120.6 . . ? H3W O14 H4W 116.7 . . ? O10 S1 O11 118.2(3) . . ? O10 S1 N1 105.0(2) . . ? O11 S1 N1 108.8(3) . . ? O10 S1 C26 107.1(3) . . ? O11 S1 C26 106.1(3) . . ? N1 S1 C26 111.7(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.923 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.083 #==END