# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_contact_author_name 'Prof Xian-He Bu' _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_address ; Chemistry Department Nankai University No.94 Weijin Road, Nankai District Tianjin 300071 CHINA ; _publ_section_title ; Lanthanide perchlorate complexes with 1,4-bis(phenylsulfinyl)butane: structure and luminescent properties ; loop_ _publ_author_name 'Xian-He Bu' 'Chun-ying Duan' 'Jian-Rong Li' 'Wong Keith Man-Chung' ; Vivian Wing-Wah Yam ; 'Ruo-Hua Zhang' #===END data_Complex_4 _database_code_depnum_ccdc_archive 'CCDC 200615' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H72 Cl3 O20 S8 Tb' _chemical_formula_weight 1682.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, -z' 'y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' _cell_length_a 14.449(4) _cell_length_b 14.449(4) _cell_length_c 17.537(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 3661.0(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 982 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.12 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 1.372 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.5946 _exptl_absorpt_correction_T_max 0.7730 _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 _diffrn_measurement_method 'Omig and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7638 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3215 _reflns_number_gt 2628 _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^)+(0.1160P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.496(14) _refine_ls_number_reflns 3215 _refine_ls_number_parameters 459 _refine_ls_number_restraints 645 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1709 _refine_ls_wR_factor_gt 0.1577 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 0.967 _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 0.5000 0.5000 0.5000 0.05388(6) Uani 1 4 d S . . S1 S 0.58674(17) 0.70409(18) 0.39749(12) 0.1333(7) Uani 0.50 1 d PDU A 1 S2 S 0.54500(19) 0.72093(19) 0.58680(12) 0.1347(8) Uani 0.50 1 d PDU A 1 O1 O 0.6041(5) 0.6017(5) 0.4085(4) 0.1304(11) Uani 0.50 1 d PU A 1 O2 O 0.5681(5) 0.6182(4) 0.5707(4) 0.1306(12) Uani 0.50 1 d PU A 1 C1 C 0.5999(2) 0.6674(2) 0.24588(12) 0.1260(12) Uani 0.50 1 d PDU A 1 H1A H 0.6434 0.6223 0.2583 0.151 Uiso 0.50 1 calc PR A 1 C2 C 0.5760(3) 0.68903(19) 0.17209(12) 0.1269(14) Uani 0.50 1 d PDU A 1 H2A H 0.5926 0.6472 0.1342 0.152 Uiso 0.50 1 calc PR A 1 C3 C 0.5295(2) 0.7674(2) 0.14969(13) 0.1259(14) Uani 0.50 1 d PDU A 1 H3A H 0.5311 0.7911 0.1004 0.151 Uiso 0.50 1 calc PR A 1 C4 C 0.4800(2) 0.8070(2) 0.20854(12) 0.1254(14) Uani 0.50 1 d PDU A 1 H4A H 0.4314 0.8462 0.1955 0.150 Uiso 0.50 1 calc PR A 1 C5 C 0.4966(2) 0.7933(2) 0.28519(13) 0.1221(14) Uani 0.50 1 d PDU A 1 H5A H 0.4719 0.8307 0.3233 0.147 Uiso 0.50 1 calc PR A 1 C6 C 0.5532(2) 0.7189(2) 0.29946(11) 0.1227(12) Uani 0.50 1 d PDU A 1 C7 C 0.6906(3) 0.7523(5) 0.41173(16) 0.1414(10) Uani 0.50 1 d PDU A 1 H7A H 0.7361 0.7083 0.3932 0.170 Uiso 0.50 1 calc PR A 1 H7B H 0.6939 0.8056 0.3782 0.170 Uiso 0.50 1 calc PR A 1 C8 C 0.7149(3) 0.7754(4) 0.46769(11) 0.1471(10) Uani 0.50 1 d PDU A 1 H8A H 0.7811 0.7643 0.4664 0.177 Uiso 0.50 1 calc PR A 1 H8B H 0.7079 0.8422 0.4661 0.177 Uiso 0.50 1 calc PR A 1 C9 C 0.6949(2) 0.7569(5) 0.52520(13) 0.1460(9) Uani 0.50 1 d PDU A 1 H9A H 0.7351 0.7083 0.5458 0.175 Uiso 0.50 1 calc PR A 1 C10 C 0.6425(2) 0.7767(5) 0.5658(2) 0.1438(12) Uani 0.50 1 d PDU A 1 H10A H 0.6235 0.8385 0.5509 0.173 Uiso 0.50 1 calc PR A 1 H10B H 0.6748 0.7837 0.6140 0.173 Uiso 0.50 1 calc PR A 1 C11 C 0.5468(4) 0.73301(16) 0.68948(10) 0.1266(12) Uani 0.50 1 d PDU A 1 C12 C 0.5130(4) 0.81205(17) 0.72357(12) 0.1249(14) Uani 0.50 1 d PDU A 1 H12A H 0.4941 0.8611 0.6929 0.150 Uiso 0.50 1 calc PR A 1 C13 C 0.5063(4) 0.82067(16) 0.80172(13) 0.1226(14) Uani 0.50 1 d PDU A 1 H13A H 0.5007 0.8780 0.8254 0.147 Uiso 0.50 1 calc PR A 1 C14 C 0.5085(3) 0.73928(16) 0.84275(14) 0.1259(14) Uani 0.50 1 d PDU A 1 H14A H 0.4800 0.7364 0.8902 0.151 Uiso 0.50 1 calc PR A 1 C15 C 0.5525(3) 0.66227(18) 0.81405(13) 0.1307(14) Uani 0.50 1 d PDU A 1 H15A H 0.5726 0.6147 0.8458 0.157 Uiso 0.50 1 calc PR A 1 C16 C 0.5656(4) 0.65880(17) 0.73629(13) 0.1296(12) Uani 0.50 1 d PDU A 1 H16A H 0.5879 0.6044 0.7146 0.156 Uiso 0.50 1 calc PR A 1 S1' S 0.71936(19) 0.54471(19) 0.41207(13) 0.1328(8) Uani 0.50 1 d PDU A 2 S2' S 0.70401(18) 0.58601(17) 0.60158(12) 0.1403(7) Uani 0.50 1 d PDU A 2 O1' O 0.6344(4) 0.5053(6) 0.4322(4) 0.1322(13) Uani 0.50 1 d PU A 2 O2' O 0.6136(4) 0.5732(4) 0.5763(3) 0.1272(12) Uani 0.50 1 d PU A 2 C1' C 0.67908(18) 0.5943(3) 0.24923(12) 0.1285(12) Uani 0.50 1 d PDU A 2 H1'A H 0.6325 0.6373 0.2586 0.154 Uiso 0.50 1 calc PR A 2 C2' C 0.70033(18) 0.5702(3) 0.17502(13) 0.1330(14) Uani 0.50 1 d PDU A 2 H2'A H 0.6616 0.5866 0.1349 0.160 Uiso 0.50 1 calc PR A 2 C3' C 0.78074(17) 0.5213(3) 0.16234(13) 0.1317(14) Uani 0.50 1 d PDU A 2 H3'A H 0.7947 0.5014 0.1132 0.158 Uiso 0.50 1 calc PR A 2 C4' C 0.84093(18) 0.5012(3) 0.22121(13) 0.1312(14) Uani 0.50 1 d PDU A 2 H4'A H 0.9029 0.4876 0.2125 0.157 Uiso 0.50 1 calc PR A 2 C5' C 0.80380(17) 0.5025(3) 0.29380(13) 0.1245(14) Uani 0.50 1 d PDU A 2 H5'A H 0.8312 0.4677 0.3323 0.149 Uiso 0.50 1 calc PR A 2 C6' C 0.72636(19) 0.5551(3) 0.30956(11) 0.1228(12) Uani 0.50 1 d PDU A 2 C7' C 0.7802(4) 0.6395(2) 0.4329(2) 0.1420(14) Uani 0.50 1 d PDU A 2 H7'A H 0.8397 0.6178 0.4512 0.170 Uiso 0.50 1 calc PR A 2 H7'B H 0.7920 0.6700 0.3846 0.170 Uiso 0.50 1 calc PR A 2 C8' C 0.7591(5) 0.6935(2) 0.47190(13) 0.1467(9) Uani 0.50 1 d PDU A 2 H8'A H 0.7123 0.7337 0.4488 0.176 Uiso 0.50 1 calc PR A 2 C9' C 0.7744(4) 0.7144(3) 0.52980(11) 0.1475(10) Uani 0.50 1 d PDU A 2 H9'A H 0.7639 0.7807 0.5297 0.177 Uiso 0.50 1 calc PR A 2 H9'B H 0.8408 0.7067 0.5342 0.177 Uiso 0.50 1 calc PR A 2 C10' C 0.7477(4) 0.6916(4) 0.58510(18) 0.1442(9) Uani 0.50 1 d PDU A 2 H10C H 0.6997 0.7354 0.5992 0.173 Uiso 0.50 1 calc PR A 2 H10D H 0.7976 0.7000 0.6214 0.173 Uiso 0.50 1 calc PR A 2 C11' C 0.73078(15) 0.5410(3) 0.69479(11) 0.1318(12) Uani 0.50 1 d PDU A 2 C12' C 0.81093(17) 0.5077(3) 0.72720(13) 0.1361(14) Uani 0.50 1 d PDU A 2 H12B H 0.8649 0.5014 0.6988 0.163 Uiso 0.50 1 calc PR A 2 C13' C 0.80827(17) 0.4842(3) 0.80325(13) 0.1379(14) Uani 0.50 1 d PDU A 2 H13B H 0.8547 0.4470 0.8236 0.165 Uiso 0.50 1 calc PR A 2 C14' C 0.73782(17) 0.5150(3) 0.84962(13) 0.1353(14) Uani 0.50 1 d PDU A 2 H14B H 0.7405 0.5066 0.9021 0.162 Uiso 0.50 1 calc PR A 2 C15' C 0.66342(18) 0.5586(4) 0.81643(13) 0.1369(14) Uani 0.50 1 d PDU A 2 H15B H 0.6178 0.5844 0.8472 0.164 Uiso 0.50 1 calc PR A 2 C16' C 0.65533(17) 0.5646(4) 0.73840(13) 0.1307(12) Uani 0.50 1 d PDU A 2 H16B H 0.6004 0.5841 0.7158 0.157 Uiso 0.50 1 calc PR A 2 Cl1 Cl 1.0000 0.5000 0.49834(12) 0.1004(4) Uani 1 2 d SDU . . O11 O 0.9777(4) 0.4822(5) 0.57470(18) 0.0986(12) Uani 0.253(3) 1 d PDU . 1 O12 O 1.0229(4) 0.5950(2) 0.4844(4) 0.1098(14) Uani 0.253(3) 1 d PDU . 1 O13 O 0.9260(3) 0.4779(5) 0.4467(3) 0.1053(10) Uani 0.253(3) 1 d PDU . 1 O14 O 1.0796(2) 0.4472(3) 0.4748(4) 0.1027(12) Uani 0.253(3) 1 d PDU . 1 O11' O 0.9214(2) 0.4484(3) 0.5250(3) 0.1025(12) Uani 0.247(3) 1 d PDU . 2 O12' O 0.9724(4) 0.5922(2) 0.4810(4) 0.1069(12) Uani 0.247(3) 1 d PDU . 2 O13' O 1.0331(4) 0.4573(4) 0.4306(2) 0.1045(12) Uani 0.247(3) 1 d PDU . 2 O14' O 1.0685(3) 0.4968(6) 0.5569(2) 0.0995(12) Uani 0.247(3) 1 d PDU . 2 Cl2 Cl 0.5000 0.5000 1.0000 0.2724(10) Uani 1 4 d SDU . . O21 O 0.5935(2) 0.5077(7) 1.0226(4) 0.270(2) Uiso 0.25 1 d PDU . . O23 O 0.5000 0.5000 0.91700(17) 0.269(2) Uiso 0.50 2 d SPDU . . O22 O 0.4462(3) 0.5785(3) 1.0210(4) 0.269(2) Uiso 0.25 1 d PDU . . O24 O 0.4570(4) 0.4161(2) 1.0221(4) 0.271(2) Uiso 0.25 1 d PDU . . 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 0.05699(7) 0.05699(7) 0.04766(10) 0.000 0.000 0.000 S1 0.1358(13) 0.1432(12) 0.1210(13) 0.0680(11) -0.0282(12) -0.0704(11) S2 0.1592(15) 0.1114(12) 0.1335(14) -0.0341(12) -0.0286(13) -0.0533(12) O1 0.1193(19) 0.145(2) 0.127(2) 0.0241(19) -0.0028(19) -0.0518(19) O2 0.152(2) 0.118(2) 0.122(2) -0.036(2) -0.047(2) -0.067(2) C1 0.115(2) 0.131(2) 0.133(2) 0.036(2) 0.012(2) -0.031(2) C2 0.115(2) 0.130(2) 0.136(2) 0.033(2) 0.014(2) -0.025(2) C3 0.116(2) 0.129(2) 0.132(3) 0.037(2) 0.003(2) -0.023(2) C4 0.117(2) 0.127(2) 0.132(3) 0.040(2) -0.003(2) -0.027(2) C5 0.112(2) 0.126(2) 0.128(2) 0.045(2) -0.004(2) -0.041(2) C6 0.116(2) 0.129(2) 0.122(2) 0.053(2) -0.009(2) -0.048(2) C7 0.1370(18) 0.1443(18) 0.1430(18) 0.0298(18) -0.0204(18) -0.0668(18) C8 0.1434(18) 0.1438(18) 0.1541(18) 0.0210(18) -0.0150(18) -0.0618(18) C9 0.1459(15) 0.1425(15) 0.1497(15) 0.0130(15) -0.0209(15) -0.0603(15) C10 0.152(2) 0.132(2) 0.147(2) 0.003(2) -0.018(2) -0.056(2) C11 0.134(2) 0.114(2) 0.131(2) -0.028(2) -0.031(2) -0.0583(19) C12 0.126(2) 0.118(2) 0.131(2) -0.026(2) -0.022(2) -0.061(2) C13 0.121(2) 0.120(2) 0.127(2) -0.027(2) -0.037(2) -0.063(2) C14 0.130(2) 0.121(2) 0.127(2) -0.033(2) -0.040(2) -0.052(2) C15 0.132(2) 0.125(2) 0.135(2) -0.023(2) -0.045(2) -0.045(2) C16 0.131(2) 0.127(2) 0.131(2) -0.018(2) -0.046(2) -0.048(2) S1' 0.1083(12) 0.1555(14) 0.1346(14) 0.0117(13) 0.0227(12) -0.0498(12) S2' 0.1433(12) 0.1464(14) 0.1313(13) 0.0319(12) -0.0753(11) -0.0772(11) O1' 0.113(2) 0.154(2) 0.130(2) 0.014(2) 0.019(2) -0.044(2) O2' 0.137(2) 0.131(2) 0.114(2) -0.006(2) -0.0805(18) -0.0780(18) C1' 0.110(2) 0.140(2) 0.136(2) 0.020(2) 0.025(2) -0.031(2) C2' 0.117(2) 0.144(3) 0.138(3) 0.017(2) 0.026(2) -0.033(2) C3' 0.118(2) 0.143(3) 0.135(3) 0.007(2) 0.032(2) -0.032(2) C4' 0.117(2) 0.137(3) 0.140(3) 0.007(2) 0.027(2) -0.030(2) C5' 0.108(2) 0.131(2) 0.135(3) 0.012(2) 0.028(2) -0.035(2) C6' 0.101(2) 0.137(2) 0.130(2) 0.013(2) 0.028(2) -0.040(2) C7' 0.124(2) 0.150(2) 0.151(3) 0.006(2) 0.003(2) -0.056(2) C8' 0.1408(15) 0.1476(15) 0.1516(15) 0.0182(15) -0.0121(15) -0.0603(15) C9' 0.1434(18) 0.1462(18) 0.1529(18) 0.0152(18) -0.0207(18) -0.0601(18) C10' 0.1464(16) 0.1403(16) 0.1458(16) 0.0189(16) -0.0271(16) -0.0658(16) C11' 0.131(2) 0.139(2) 0.125(2) 0.017(2) -0.064(2) -0.062(2) C12' 0.135(2) 0.144(2) 0.129(2) 0.017(2) -0.053(2) -0.051(2) C13' 0.135(2) 0.148(3) 0.131(3) 0.016(2) -0.051(2) -0.041(2) C14' 0.129(2) 0.148(3) 0.129(3) 0.009(2) -0.048(2) -0.040(2) C15' 0.128(2) 0.146(3) 0.137(3) 0.001(2) -0.046(2) -0.043(2) C16' 0.126(2) 0.135(2) 0.131(2) -0.002(2) -0.056(2) -0.052(2) Cl1 0.0713(5) 0.1265(7) 0.1035(7) 0.000 0.000 -0.0011(5) O11 0.071(2) 0.125(2) 0.100(2) 0.006(2) -0.006(2) -0.004(2) O12 0.082(2) 0.133(2) 0.115(3) 0.013(2) 0.000(2) -0.005(2) O13 0.0814(18) 0.1312(18) 0.1033(18) 0.0005(18) -0.0069(18) -0.0103(18) O14 0.076(2) 0.128(2) 0.105(2) -0.004(2) -0.002(2) 0.003(2) O11' 0.076(2) 0.130(2) 0.102(2) 0.004(2) 0.001(2) -0.008(2) O12' 0.080(2) 0.131(2) 0.109(2) 0.010(2) -0.009(2) -0.009(2) O13' 0.083(2) 0.129(2) 0.102(2) -0.003(2) -0.007(2) -0.001(2) O14' 0.075(2) 0.124(2) 0.100(2) 0.003(2) -0.004(2) -0.005(2) Cl2 0.2814(12) 0.2814(12) 0.2545(17) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1' 2.278(7) 4_566 ? Tb1 O1' 2.278(7) 3_656 ? Tb1 O1' 2.278(7) 2_665 ? Tb1 O1' 2.278(7) . ? Tb1 O2 2.328(6) . ? Tb1 O2 2.328(6) 2_665 ? Tb1 O2 2.328(6) 4_566 ? Tb1 O2 2.328(6) 3_656 ? Tb1 O2' 2.367(6) . ? Tb1 O2' 2.367(5) 4_566 ? Tb1 O2' 2.367(6) 2_665 ? Tb1 O2' 2.367(5) 3_656 ? S1 O1 1.512(8) . ? S1 C7 1.674(5) . ? S1 C6 1.799(3) . ? S2 O2 1.547(7) . ? S2 C10 1.664(5) . ? S2 C11 1.809(3) . ? C1 C2 1.376(3) . ? C1 C6 1.376(3) . ? C2 C3 1.375(4) . ? C3 C4 1.379(4) . ? C4 C5 1.380(3) . ? C5 C6 1.375(4) . ? C7 C8 1.094(4) . ? C7 C9 1.992(4) . ? C8 C9 1.083(4) . ? C8 C10 2.014(5) . ? C9 C10 1.078(4) . ? C11 C16 1.377(3) . ? C11 C12 1.379(4) . ? C12 C13 1.380(3) . ? C13 C14 1.379(3) . ? C14 C15 1.377(4) . ? C15 C16 1.378(3) . ? S1' O1' 1.399(7) . ? S1' C7' 1.668(5) . ? S1' C6' 1.807(3) . ? S2' O2' 1.392(6) . ? S2' C10' 1.676(6) . ? S2' C11' 1.801(3) . ? C1' C6' 1.381(3) . ? C1' C2' 1.382(3) . ? C2' C3' 1.378(4) . ? C3' C4' 1.381(3) . ? C4' C5' 1.382(3) . ? C5' C6' 1.381(4) . ? C7' C8' 1.081(4) . ? C7' C9' 2.016(5) . ? C8' C9' 1.082(4) . ? C8' C10' 1.992(4) . ? C9' C10' 1.095(4) . ? C11' C16' 1.375(3) . ? C11' C12' 1.376(3) . ? C12' C13' 1.377(3) . ? C13' C14' 1.377(4) . ? C14' C15' 1.375(4) . ? C15' C16' 1.376(3) . ? Cl1 O11 1.401(4) 2_765 ? Cl1 O11 1.401(4) . ? Cl1 O13' 1.421(4) . ? Cl1 O13' 1.421(4) 2_765 ? Cl1 O12' 1.423(4) 2_765 ? Cl1 O12' 1.423(4) . ? Cl1 O14' 1.427(4) . ? Cl1 O14' 1.427(4) 2_765 ? Cl1 O12 1.432(3) 2_765 ? Cl1 O12 1.432(3) . ? Cl1 O13 1.437(4) . ? Cl1 O13 1.437(4) 2_765 ? O11 O11 0.824(13) 2_765 ? O12 O13 1.445(8) 2_765 ? O12 O14 1.609(7) 2_765 ? O13 O14 1.192(9) 2_765 ? O13 O12 1.445(8) 2_765 ? O14 O13 1.192(9) 2_765 ? O14 O12 1.609(7) 2_765 ? O11' O14' 0.981(9) 2_765 ? O11' O12' 1.815(7) 2_765 ? O12' O13' 1.140(8) 2_765 ? O12' O11' 1.815(7) 2_765 ? O13' O12' 1.140(8) 2_765 ? O13' O13' 1.562(11) 2_765 ? O14' O11' 0.981(9) 2_765 ? Cl2 O21 1.412(4) 4_567 ? Cl2 O21 1.412(4) . ? Cl2 O21 1.412(4) 2_665 ? Cl2 O21 1.412(4) 3_657 ? Cl2 O24 1.416(4) 2_665 ? Cl2 O24 1.416(4) 3_657 ? Cl2 O24 1.416(4) . ? Cl2 O24 1.416(4) 4_567 ? Cl2 O22 1.423(4) 2_665 ? Cl2 O22 1.423(4) 3_657 ? Cl2 O22 1.423(4) . ? Cl2 O22 1.423(4) 4_567 ? O21 O22 1.037(11) 4_567 ? O21 O24 1.082(11) 3_657 ? O21 O24 1.321(9) 2_665 ? O21 O22 1.370(10) 2_665 ? O21 O23 1.720(6) 3_657 ? O23 O21 1.720(6) 4_567 ? O23 O21 1.720(6) 3_657 ? O23 O24 1.731(6) 3_657 ? O23 O24 1.731(6) 4_567 ? O23 O22 1.752(6) 4_567 ? O23 O22 1.752(6) 3_657 ? O22 O24 1.012(9) 4_567 ? O22 O21 1.037(11) 3_657 ? O22 O21 1.370(10) 2_665 ? O22 O24 1.401(8) 2_665 ? O22 O23 1.752(6) 3_657 ? O24 O22 1.012(9) 3_657 ? O24 O21 1.082(11) 4_567 ? O24 O21 1.321(9) 2_665 ? O24 O22 1.401(8) 2_665 ? O24 O23 1.731(6) 3_657 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1' Tb1 O1' 117.1(4) 4_566 3_656 ? O1' Tb1 O1' 105.81(18) 4_566 2_665 ? O1' Tb1 O1' 105.81(18) 3_656 2_665 ? O1' Tb1 O1' 105.81(18) 4_566 . ? O1' Tb1 O1' 105.81(18) 3_656 . ? O1' Tb1 O1' 117.1(4) 2_665 . ? O1' Tb1 O2 109.5(2) 4_566 . ? O1' Tb1 O2 27.3(3) 3_656 . ? O1' Tb1 O2 131.5(3) 2_665 . ? O1' Tb1 O2 83.9(3) . . ? O1' Tb1 O2 27.3(3) 4_566 2_665 ? O1' Tb1 O2 109.5(2) 3_656 2_665 ? O1' Tb1 O2 83.9(3) 2_665 2_665 ? O1' Tb1 O2 131.5(3) . 2_665 ? O2 Tb1 O2 115.7(3) . 2_665 ? O1' Tb1 O2 83.9(3) 4_566 4_566 ? O1' Tb1 O2 131.5(3) 3_656 4_566 ? O1' Tb1 O2 109.5(2) 2_665 4_566 ? O1' Tb1 O2 27.3(3) . 4_566 ? O2 Tb1 O2 106.46(15) . 4_566 ? O2 Tb1 O2 106.46(15) 2_665 4_566 ? O1' Tb1 O2 131.5(3) 4_566 3_656 ? O1' Tb1 O2 83.9(3) 3_656 3_656 ? O1' Tb1 O2 27.3(3) 2_665 3_656 ? O1' Tb1 O2 109.5(2) . 3_656 ? O2 Tb1 O2 106.46(15) . 3_656 ? O2 Tb1 O2 106.46(15) 2_665 3_656 ? O2 Tb1 O2 115.7(3) 4_566 3_656 ? O1' Tb1 O2' 93.6(2) 4_566 . ? O1' Tb1 O2' 49.3(2) 3_656 . ? O1' Tb1 O2' 154.3(2) 2_665 . ? O1' Tb1 O2' 71.9(2) . . ? O2 Tb1 O2' 22.8(2) . . ? O2 Tb1 O2' 108.6(2) 2_665 . ? O2 Tb1 O2' 88.9(2) 4_566 . ? O2 Tb1 O2' 128.4(2) 3_656 . ? O1' Tb1 O2' 71.9(2) 4_566 4_566 ? O1' Tb1 O2' 154.3(2) 3_656 4_566 ? O1' Tb1 O2' 93.6(2) 2_665 4_566 ? O1' Tb1 O2' 49.3(2) . 4_566 ? O2 Tb1 O2' 128.4(2) . 4_566 ? O2 Tb1 O2' 88.9(2) 2_665 4_566 ? O2 Tb1 O2' 22.8(2) 4_566 4_566 ? O2 Tb1 O2' 108.6(2) 3_656 4_566 ? O2' Tb1 O2' 108.64(14) . 4_566 ? O1' Tb1 O2' 49.3(2) 4_566 2_665 ? O1' Tb1 O2' 93.6(2) 3_656 2_665 ? O1' Tb1 O2' 71.9(2) 2_665 2_665 ? O1' Tb1 O2' 154.3(2) . 2_665 ? O2 Tb1 O2' 108.6(2) . 2_665 ? O2 Tb1 O2' 22.8(2) 2_665 2_665 ? O2 Tb1 O2' 128.4(2) 4_566 2_665 ? O2 Tb1 O2' 88.9(2) 3_656 2_665 ? O2' Tb1 O2' 111.1(3) . 2_665 ? O2' Tb1 O2' 108.64(14) 4_566 2_665 ? O1' Tb1 O2' 154.3(2) 4_566 3_656 ? O1' Tb1 O2' 71.9(2) 3_656 3_656 ? O1' Tb1 O2' 49.3(2) 2_665 3_656 ? O1' Tb1 O2' 93.6(2) . 3_656 ? O2 Tb1 O2' 88.9(2) . 3_656 ? O2 Tb1 O2' 128.4(2) 2_665 3_656 ? O2 Tb1 O2' 108.6(2) 4_566 3_656 ? O2 Tb1 O2' 22.8(2) 3_656 3_656 ? O2' Tb1 O2' 108.64(14) . 3_656 ? O2' Tb1 O2' 111.1(3) 4_566 3_656 ? O2' Tb1 O2' 108.64(14) 2_665 3_656 ? O1 S1 C7 103.8(4) . . ? O1 S1 C6 106.4(3) . . ? C7 S1 C6 109.6(2) . . ? O2 S2 C10 104.0(4) . . ? O2 S2 C11 105.7(3) . . ? C10 S2 C11 99.3(2) . . ? S1 O1 Tb1 121.8(4) . . ? S2 O2 Tb1 135.2(4) . . ? C2 C1 C6 113.3(2) . . ? C3 C2 C1 125.4(2) . . ? C2 C3 C4 112.4(2) . . ? C3 C4 C5 125.4(3) . . ? C6 C5 C4 113.1(2) . . ? C5 C6 C1 126.3(2) . . ? C5 C6 S1 115.28(19) . . ? C1 C6 S1 117.2(2) . . ? C8 C7 S1 123.3(4) . . ? C8 C7 C9 23.7(3) . . ? S1 C7 C9 101.0(2) . . ? C9 C8 C7 132.4(6) . . ? C9 C8 C10 21.2(3) . . ? C7 C8 C10 127.0(4) . . ? C10 C9 C8 137.5(7) . . ? C10 C9 C7 130.3(4) . . ? C8 C9 C7 23.9(3) . . ? C9 C10 S2 127.8(6) . . ? C9 C10 C8 21.3(3) . . ? S2 C10 C8 128.6(3) . . ? C16 C11 C12 117.1(2) . . ? C16 C11 S2 121.4(2) . . ? C12 C11 S2 120.4(2) . . ? C11 C12 C13 122.0(2) . . ? C14 C13 C12 116.1(2) . . ? C15 C14 C13 120.6(3) . . ? C14 C15 C16 117.0(3) . . ? C11 C16 C15 122.3(3) . . ? O1' S1' C7' 137.9(4) . . ? O1' S1' C6' 109.5(4) . . ? C7' S1' C6' 96.9(2) . . ? O2' S2' C10' 114.8(4) . . ? O2' S2' C11' 116.3(3) . . ? C10' S2' C11' 113.9(2) . . ? S1' O1' Tb1 153.4(5) . . ? S2' O2' Tb1 152.9(4) . . ? C6' C1' C2' 120.6(3) . . ? C3' C2' C1' 117.9(2) . . ? C2' C3' C4' 121.2(2) . . ? C3' C4' C5' 116.2(2) . . ? C6' C5' C4' 120.4(3) . . ? C5' C6' C1' 118.3(2) . . ? C5' C6' S1' 101.5(2) . . ? C1' C6' S1' 140.2(2) . . ? C8' C7' S1' 125.6(6) . . ? C8' C7' C9' 21.2(3) . . ? S1' C7' C9' 127.1(3) . . ? C7' C8' C9' 137.6(7) . . ? C7' C8' C10' 130.1(4) . . ? C9' C8' C10' 23.9(3) . . ? C8' C9' C10' 132.5(6) . . ? C8' C9' C7' 21.2(3) . . ? C10' C9' C7' 126.8(5) . . ? C9' C10' S2' 124.0(4) . . ? C9' C10' C8' 23.6(3) . . ? S2' C10' C8' 102.5(3) . . ? C16' C11' C12' 121.6(2) . . ? C16' C11' S2' 104.2(2) . . ? C12' C11' S2' 132.95(19) . . ? C11' C12' C13' 117.6(2) . . ? C12' C13' C14' 120.9(3) . . ? C15' C14' C13' 118.4(2) . . ? C14' C15' C16' 121.1(3) . . ? C11' C16' C15' 118.0(2) . . ? O11 Cl1 O11 34.2(5) 2_765 . ? O11 Cl1 O13' 143.2(4) 2_765 . ? O11 Cl1 O13' 142.8(4) . . ? O11 Cl1 O13' 142.8(4) 2_765 2_765 ? O11 Cl1 O13' 143.2(4) . 2_765 ? O13' Cl1 O13' 66.6(4) . 2_765 ? O11 Cl1 O12' 108.1(4) 2_765 2_765 ? O11 Cl1 O12' 95.5(4) . 2_765 ? O13' Cl1 O12' 47.2(4) . 2_765 ? O13' Cl1 O12' 108.8(4) 2_765 2_765 ? O11 Cl1 O12' 95.5(4) 2_765 . ? O11 Cl1 O12' 108.1(4) . . ? O13' Cl1 O12' 108.8(4) . . ? O13' Cl1 O12' 47.2(4) 2_765 . ? O12' Cl1 O12' 155.4(6) 2_765 . ? O11 Cl1 O14' 32.7(3) 2_765 . ? O11 Cl1 O14' 57.7(3) . . ? O13' Cl1 O14' 110.8(3) . . ? O13' Cl1 O14' 148.1(4) 2_765 . ? O12' Cl1 O14' 85.9(4) 2_765 . ? O12' Cl1 O14' 112.2(4) . . ? O11 Cl1 O14' 57.7(3) 2_765 2_765 ? O11 Cl1 O14' 32.7(3) . 2_765 ? O13' Cl1 O14' 148.1(4) . 2_765 ? O13' Cl1 O14' 110.8(3) 2_765 2_765 ? O12' Cl1 O14' 112.2(4) 2_765 2_765 ? O12' Cl1 O14' 85.9(4) . 2_765 ? O14' Cl1 O14' 87.9(4) . 2_765 ? O11 Cl1 O12 113.1(4) 2_765 2_765 ? O11 Cl1 O12 86.2(4) . 2_765 ? O13' Cl1 O12 61.2(4) . 2_765 ? O13' Cl1 O12 101.3(4) 2_765 2_765 ? O12' Cl1 O12 29.7(3) 2_765 2_765 ? O12' Cl1 O12 142.7(4) . 2_765 ? O14' Cl1 O12 104.6(4) . 2_765 ? O14' Cl1 O12 89.6(4) 2_765 2_765 ? O11 Cl1 O12 86.2(4) 2_765 . ? O11 Cl1 O12 113.1(4) . . ? O13' Cl1 O12 101.3(4) . . ? O13' Cl1 O12 61.2(4) 2_765 . ? O12' Cl1 O12 142.7(4) 2_765 . ? O12' Cl1 O12 29.7(3) . . ? O14' Cl1 O12 89.6(4) . . ? O14' Cl1 O12 104.6(4) 2_765 . ? O12 Cl1 O12 160.4(6) 2_765 . ? O11 Cl1 O13 144.5(3) 2_765 . ? O11 Cl1 O13 113.0(3) . . ? O13' Cl1 O13 68.1(3) . . ? O13' Cl1 O13 47.2(4) 2_765 . ? O12' Cl1 O13 82.3(4) 2_765 . ? O12' Cl1 O13 82.3(4) . . ? O14' Cl1 O13 164.2(4) . . ? O14' Cl1 O13 86.8(3) 2_765 . ? O12 Cl1 O13 60.5(4) 2_765 . ? O12 Cl1 O13 106.1(4) . . ? O11 Cl1 O13 113.0(3) 2_765 2_765 ? O11 Cl1 O13 144.5(3) . 2_765 ? O13' Cl1 O13 47.2(4) . 2_765 ? O13' Cl1 O13 68.1(3) 2_765 2_765 ? O12' Cl1 O13 82.3(4) 2_765 2_765 ? O12' Cl1 O13 82.3(4) . 2_765 ? O14' Cl1 O13 86.8(3) . 2_765 ? O14' Cl1 O13 164.2(4) 2_765 2_765 ? O12 Cl1 O13 106.1(4) 2_765 2_765 ? O12 Cl1 O13 60.5(4) . 2_765 ? O13 Cl1 O13 101.9(4) . 2_765 ? O11 O11 Cl1 72.9(3) 2_765 . ? Cl1 O12 O13 59.9(3) . 2_765 ? Cl1 O12 O14 56.2(2) . 2_765 ? O13 O12 O14 98.4(4) 2_765 2_765 ? O14 O13 Cl1 65.7(3) 2_765 . ? O14 O13 O12 120.5(5) 2_765 2_765 ? Cl1 O13 O12 59.6(3) . 2_765 ? O13 O14 Cl1 65.4(3) 2_765 . ? O13 O14 O12 109.0(4) 2_765 2_765 ? Cl1 O14 O12 55.7(2) . 2_765 ? O14' O11' Cl1 69.4(4) 2_765 . ? O14' O11' O12' 112.1(4) 2_765 2_765 ? Cl1 O11' O12' 50.28(18) . 2_765 ? O13' O12' Cl1 66.3(3) 2_765 . ? O13' O12' O11' 100.7(5) 2_765 2_765 ? Cl1 O12' O11' 51.0(2) . 2_765 ? O12' O13' Cl1 66.5(3) 2_765 . ? O12' O13' O13' 117.0(5) 2_765 2_765 ? Cl1 O13' O13' 56.7(2) . 2_765 ? O11' O14' Cl1 70.5(4) 2_765 . ? O21 Cl2 O21 94.52(16) 4_567 . ? O21 Cl2 O21 94.52(16) 4_567 2_665 ? O21 Cl2 O21 147.4(6) . 2_665 ? O21 Cl2 O21 147.4(6) 4_567 3_657 ? O21 Cl2 O21 94.52(16) . 3_657 ? O21 Cl2 O21 94.52(16) 2_665 3_657 ? O21 Cl2 O24 149.4(5) 4_567 2_665 ? O21 Cl2 O24 55.7(4) . 2_665 ? O21 Cl2 O24 114.2(5) 2_665 2_665 ? O21 Cl2 O24 45.0(4) 3_657 2_665 ? O21 Cl2 O24 55.7(4) 4_567 3_657 ? O21 Cl2 O24 45.0(4) . 3_657 ? O21 Cl2 O24 149.4(5) 2_665 3_657 ? O21 Cl2 O24 114.2(5) 3_657 3_657 ? O24 Cl2 O24 94.30(17) 2_665 3_657 ? O21 Cl2 O24 45.0(4) 4_567 . ? O21 Cl2 O24 114.2(5) . . ? O21 Cl2 O24 55.7(4) 2_665 . ? O21 Cl2 O24 149.4(5) 3_657 . ? O24 Cl2 O24 148.2(6) 2_665 . ? O24 Cl2 O24 94.30(16) 3_657 . ? O21 Cl2 O24 114.2(5) 4_567 4_567 ? O21 Cl2 O24 149.4(5) . 4_567 ? O21 Cl2 O24 45.0(4) 2_665 4_567 ? O21 Cl2 O24 55.7(4) 3_657 4_567 ? O24 Cl2 O24 94.30(16) 2_665 4_567 ? O24 Cl2 O24 148.2(6) 3_657 4_567 ? O24 Cl2 O24 94.30(17) . 4_567 ? O21 Cl2 O22 42.9(4) 4_567 2_665 ? O21 Cl2 O22 57.8(4) . 2_665 ? O21 Cl2 O22 112.8(4) 2_665 2_665 ? O21 Cl2 O22 151.4(4) 3_657 2_665 ? O24 Cl2 O22 111.8(3) 2_665 2_665 ? O24 Cl2 O22 41.7(4) 3_657 2_665 ? O24 Cl2 O22 59.1(3) . 2_665 ? O24 Cl2 O22 152.6(3) 4_567 2_665 ? O21 Cl2 O22 57.8(4) 4_567 3_657 ? O21 Cl2 O22 151.4(4) . 3_657 ? O21 Cl2 O22 42.9(4) 2_665 3_657 ? O21 Cl2 O22 112.8(4) 3_657 3_657 ? O24 Cl2 O22 152.6(3) 2_665 3_657 ? O24 Cl2 O22 111.8(3) 3_657 3_657 ? O24 Cl2 O22 41.7(4) . 3_657 ? O24 Cl2 O22 59.1(3) 4_567 3_657 ? O22 Cl2 O22 93.84(16) 2_665 3_657 ? O21 Cl2 O22 151.4(4) 4_567 . ? O21 Cl2 O22 112.8(4) . . ? O21 Cl2 O22 57.8(4) 2_665 . ? O21 Cl2 O22 42.9(4) 3_657 . ? O24 Cl2 O22 59.1(3) 2_665 . ? O24 Cl2 O22 152.6(3) 3_657 . ? O24 Cl2 O22 111.8(3) . . ? O24 Cl2 O22 41.7(4) 4_567 . ? O22 Cl2 O22 150.0(6) 2_665 . ? O22 Cl2 O22 93.84(16) 3_657 . ? O21 Cl2 O22 112.8(4) 4_567 4_567 ? O21 Cl2 O22 42.9(4) . 4_567 ? O21 Cl2 O22 151.4(4) 2_665 4_567 ? O21 Cl2 O22 57.8(4) 3_657 4_567 ? O24 Cl2 O22 41.7(4) 2_665 4_567 ? O24 Cl2 O22 59.1(3) 3_657 4_567 ? O24 Cl2 O22 152.6(3) . 4_567 ? O24 Cl2 O22 111.8(3) 4_567 4_567 ? O22 Cl2 O22 93.84(16) 2_665 4_567 ? O22 Cl2 O22 150.0(6) 3_657 4_567 ? O22 Cl2 O22 93.84(16) . 4_567 ? O22 O21 O24 82.8(7) 4_567 3_657 ? O22 O21 O24 49.0(6) 4_567 2_665 ? O24 O21 O24 119.3(6) 3_657 2_665 ? O22 O21 O22 118.7(6) 4_567 2_665 ? O24 O21 O22 46.9(6) 3_657 2_665 ? O24 O21 O22 121.7(4) 2_665 2_665 ? O22 O21 Cl2 69.1(4) 4_567 . ? O24 O21 Cl2 67.7(4) 3_657 . ? O24 O21 Cl2 62.3(3) 2_665 . ? O22 O21 Cl2 61.5(3) 2_665 . ? O22 O21 O23 109.3(5) 4_567 3_657 ? O24 O21 O23 107.6(5) 3_657 3_657 ? O24 O21 O23 67.9(4) 2_665 3_657 ? O22 O21 O23 68.0(4) 2_665 3_657 ? Cl2 O21 O23 54.31(17) . 3_657 ? Cl2 O23 O21 52.0(2) . 4_567 ? Cl2 O23 O21 52.0(2) . 3_657 ? O21 O23 O21 104.0(4) 4_567 3_657 ? Cl2 O23 O24 51.9(2) . 3_657 ? O21 O23 O24 45.0(4) 4_567 3_657 ? O21 O23 O24 87.0(4) 3_657 3_657 ? Cl2 O23 O24 51.9(2) . 4_567 ? O21 O23 O24 87.0(4) 4_567 4_567 ? O21 O23 O24 45.0(4) 3_657 4_567 ? O24 O23 O24 103.8(5) 3_657 4_567 ? Cl2 O23 O22 51.7(2) . 4_567 ? O21 O23 O22 85.7(3) 4_567 4_567 ? O21 O23 O22 46.5(4) 3_657 4_567 ? O24 O23 O22 47.4(3) 3_657 4_567 ? O24 O23 O22 84.9(3) 4_567 4_567 ? Cl2 O23 O22 51.7(2) . 3_657 ? O21 O23 O22 46.5(4) 4_567 3_657 ? O21 O23 O22 85.7(3) 3_657 3_657 ? O24 O23 O22 84.9(3) 3_657 3_657 ? O24 O23 O22 47.4(3) 4_567 3_657 ? O22 O23 O22 103.3(5) 4_567 3_657 ? O24 O22 O21 80.3(8) 4_567 3_657 ? O24 O22 O21 51.4(5) 4_567 2_665 ? O21 O22 O21 118.3(6) 3_657 2_665 ? O24 O22 O24 117.9(6) 4_567 2_665 ? O21 O22 O24 50.0(6) 3_657 2_665 ? O21 O22 O24 117.9(4) 2_665 2_665 ? O24 O22 Cl2 68.8(4) 4_567 . ? O21 O22 Cl2 68.0(4) 3_657 . ? O21 O22 Cl2 60.7(3) 2_665 . ? O24 O22 Cl2 60.2(3) 2_665 . ? O24 O22 O23 109.1(4) 4_567 3_657 ? O21 O22 O23 107.9(5) 3_657 3_657 ? O21 O22 O23 65.5(3) 2_665 3_657 ? O24 O22 O23 65.5(3) 2_665 3_657 ? Cl2 O22 O23 53.35(19) . 3_657 ? O22 O24 O21 81.7(8) 3_657 4_567 ? O22 O24 O21 50.7(5) 3_657 2_665 ? O21 O24 O21 119.0(6) 4_567 2_665 ? O22 O24 O22 118.1(6) 3_657 2_665 ? O21 O24 O22 47.2(6) 4_567 2_665 ? O21 O24 O22 120.3(4) 2_665 2_665 ? O22 O24 Cl2 69.5(4) 3_657 . ? O21 O24 Cl2 67.3(3) 4_567 . ? O21 O24 Cl2 62.0(3) 2_665 . ? O22 O24 Cl2 60.7(3) 2_665 . ? O22 O24 O23 110.0(4) 3_657 3_657 ? O21 O24 O23 107.1(5) 4_567 3_657 ? O21 O24 O23 67.1(4) 2_665 3_657 ? O22 O24 O23 67.1(4) 2_665 3_657 ? Cl2 O24 O23 53.99(19) . 3_657 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.053 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.099 #===END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 200616' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H72 Cl3 Eu O20 S8' _chemical_formula_weight 1676.01 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.488(2) _cell_length_b 14.488(2) _cell_length_c 17.490(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3671.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 894 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.13 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 1.260 _exptl_absorpt_correction_type MUlti-Scan _exptl_absorpt_correction_T_min 0.6975 _exptl_absorpt_correction_T_max 0.7810 _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 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9500 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3204 _reflns_number_gt 3070 _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^)+(0.1405P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(4) _refine_ls_number_reflns 3204 _refine_ls_number_parameters 459 _refine_ls_number_restraints 638 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1685 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.5000 0.5000 0.5000 0.0543(3) Uani 1 4 d S . . S1 S 0.5805(7) 0.7099(8) 0.4023(6) 0.132(3) Uani 0.50 1 d PDU A 1 S2 S 0.5371(11) 0.7209(11) 0.5872(8) 0.156(4) Uani 0.50 1 d PDU A 1 O1 O 0.579(3) 0.610(2) 0.4235(18) 0.126(5) Uani 0.50 1 d PU A 1 O2 O 0.515(3) 0.6303(18) 0.5713(14) 0.142(5) Uani 0.50 1 d PU A 1 C1 C 0.592(2) 0.668(2) 0.2468(17) 0.136(5) Uani 0.50 1 d PDU A 1 H1A H 0.6426 0.6313 0.2597 0.163 Uiso 0.50 1 calc PR A 1 C2 C 0.558(3) 0.666(2) 0.1746(18) 0.143(6) Uani 0.50 1 d PDU A 1 H2A H 0.5539 0.6121 0.1456 0.171 Uiso 0.50 1 calc PR A 1 C3 C 0.530(3) 0.750(2) 0.1491(11) 0.140(6) Uani 0.50 1 d PDU A 1 H3A H 0.5333 0.7623 0.0970 0.168 Uiso 0.50 1 calc PR A 1 C4 C 0.497(3) 0.815(2) 0.1972(19) 0.136(7) Uani 0.50 1 d PDU A 1 H4A H 0.4656 0.8670 0.1795 0.163 Uiso 0.50 1 calc PR A 1 C5 C 0.513(3) 0.801(2) 0.2726(19) 0.132(6) Uani 0.50 1 d PDU A 1 H5A H 0.4969 0.8474 0.3071 0.158 Uiso 0.50 1 calc PR A 1 C6 C 0.553(3) 0.723(3) 0.3000(10) 0.128(5) Uani 0.50 1 d PDU A 1 C7 C 0.685(2) 0.765(3) 0.4180(17) 0.147(4) Uani 0.50 1 d PDU A 1 H7A H 0.7326 0.7281 0.3944 0.176 Uiso 0.50 1 calc PR A 1 H7B H 0.6829 0.8236 0.3912 0.176 Uiso 0.50 1 calc PR A 1 C8 C 0.706(2) 0.779(3) 0.4775(14) 0.155(4) Uani 0.50 1 d PDU A 1 H8A H 0.7723 0.7752 0.4748 0.186 Uiso 0.50 1 calc PR A 1 H8B H 0.6921 0.8440 0.4832 0.186 Uiso 0.50 1 calc PR A 1 C9 C 0.6909(18) 0.752(3) 0.5346(17) 0.160(4) Uani 0.50 1 d PDU A 1 H9A H 0.6776 0.6874 0.5231 0.192 Uiso 0.50 1 calc PR A 1 H9B H 0.7521 0.7506 0.5570 0.192 Uiso 0.50 1 calc PR A 1 C10 C 0.648(2) 0.763(3) 0.585(2) 0.161(4) Uani 0.50 1 d PDU A 1 H10A H 0.6449 0.8286 0.5938 0.193 Uiso 0.50 1 calc PR A 1 H10B H 0.6805 0.7361 0.6284 0.193 Uiso 0.50 1 calc PR A 1 C11 C 0.544(3) 0.730(3) 0.6924(10) 0.146(5) Uani 0.50 1 d PDU A 1 C12 C 0.500(3) 0.811(3) 0.709(2) 0.147(7) Uani 0.50 1 d PDU A 1 H12A H 0.4691 0.8489 0.6737 0.177 Uiso 0.50 1 calc PR A 1 C13 C 0.508(4) 0.827(2) 0.786(2) 0.151(7) Uani 0.50 1 d PDU A 1 H13A H 0.5167 0.8872 0.8019 0.182 Uiso 0.50 1 calc PR A 1 C14 C 0.506(3) 0.759(3) 0.8403(13) 0.154(7) Uani 0.50 1 d PDU A 1 H14A H 0.4704 0.7567 0.8848 0.185 Uiso 0.50 1 calc PR A 1 C15 C 0.567(3) 0.695(2) 0.8134(19) 0.155(7) Uani 0.50 1 d PDU A 1 H15A H 0.6152 0.6758 0.8452 0.186 Uiso 0.50 1 calc PR A 1 C16 C 0.561(3) 0.658(2) 0.7414(19) 0.147(5) Uani 0.50 1 d PDU A 1 H16A H 0.5671 0.5958 0.7283 0.177 Uiso 0.50 1 calc PR A 1 S1' S 0.7181(8) 0.5517(9) 0.4137(6) 0.130(3) Uani 0.50 1 d PDU A 2 S2' S 0.6991(10) 0.5897(9) 0.6051(7) 0.152(3) Uani 0.50 1 d PDU A 2 O1' O 0.615(2) 0.557(3) 0.4314(16) 0.134(5) Uani 0.50 1 d PU A 2 O2' O 0.602(3) 0.596(3) 0.585(2) 0.138(5) Uani 0.50 1 d PU A 2 C1' C 0.680(2) 0.595(3) 0.2479(17) 0.138(5) Uani 0.50 1 d PDU A 2 H1'A H 0.6355 0.6397 0.2567 0.166 Uiso 0.50 1 calc PR A 2 C2' C 0.703(2) 0.572(3) 0.1751(19) 0.144(6) Uani 0.50 1 d PDU A 2 H2'A H 0.6663 0.5903 0.1339 0.173 Uiso 0.50 1 calc PR A 2 C3' C 0.781(3) 0.523(3) 0.1648(14) 0.144(6) Uani 0.50 1 d PDU A 2 H3'A H 0.7953 0.5010 0.1162 0.172 Uiso 0.50 1 calc PR A 2 C4' C 0.839(2) 0.503(3) 0.224(2) 0.140(6) Uani 0.50 1 d PDU A 2 H4'A H 0.9010 0.4910 0.2166 0.168 Uiso 0.50 1 calc PR A 2 C5' C 0.799(2) 0.503(3) 0.294(2) 0.131(6) Uani 0.50 1 d PDU A 2 H5'A H 0.8250 0.4688 0.3327 0.157 Uiso 0.50 1 calc PR A 2 C6' C 0.721(3) 0.552(3) 0.3081(9) 0.130(5) Uani 0.50 1 d PDU A 2 C7' C 0.781(2) 0.647(2) 0.431(2) 0.143(5) Uani 0.50 1 d PDU A 2 H7'A H 0.8429 0.6255 0.4439 0.172 Uiso 0.50 1 calc PR A 2 H7'B H 0.7863 0.6796 0.3832 0.172 Uiso 0.50 1 calc PR A 2 C8' C 0.763(3) 0.6983(18) 0.4743(14) 0.154(4) Uani 0.50 1 d PDU A 2 H8'A H 0.6968 0.7008 0.4687 0.185 Uiso 0.50 1 calc PR A 2 H8'B H 0.7852 0.7543 0.4499 0.185 Uiso 0.50 1 calc PR A 2 C9' C 0.771(3) 0.716(2) 0.5346(14) 0.160(4) Uani 0.50 1 d PDU A 2 H9'A H 0.7670 0.7830 0.5338 0.192 Uiso 0.50 1 calc PR A 2 H9'B H 0.8360 0.7032 0.5439 0.192 Uiso 0.50 1 calc PR A 2 C10' C 0.739(3) 0.6987(19) 0.5898(17) 0.157(4) Uani 0.50 1 d PDU A 2 H10C H 0.6880 0.7407 0.5975 0.188 Uiso 0.50 1 calc PR A 2 H10D H 0.7842 0.7118 0.6295 0.188 Uiso 0.50 1 calc PR A 2 C11' C 0.730(3) 0.547(3) 0.7009(12) 0.143(5) Uani 0.50 1 d PDU A 2 C12' C 0.808(2) 0.509(3) 0.7284(19) 0.143(6) Uani 0.50 1 d PDU A 2 H12B H 0.8599 0.4969 0.6982 0.171 Uiso 0.50 1 calc PR A 2 C13' C 0.805(2) 0.491(4) 0.8036(19) 0.143(7) Uani 0.50 1 d PDU A 2 H13B H 0.8549 0.4594 0.8245 0.172 Uiso 0.50 1 calc PR A 2 C14' C 0.736(2) 0.513(3) 0.8515(11) 0.140(7) Uani 0.50 1 d PDU A 2 H14B H 0.7358 0.4983 0.9032 0.168 Uiso 0.50 1 calc PR A 2 C15' C 0.667(2) 0.559(2) 0.8175(17) 0.140(6) Uani 0.50 1 d PDU A 2 H15B H 0.6226 0.5865 0.8491 0.169 Uiso 0.50 1 calc PR A 2 C16' C 0.655(2) 0.570(2) 0.7417(17) 0.140(5) Uani 0.50 1 d PDU A 2 H16B H 0.6010 0.5914 0.7197 0.168 Uiso 0.50 1 calc PR A 2 Cl1 Cl 1.0000 0.5000 0.5001(9) 0.1080(9) Uani 1 2 d SDU . . O11 O 0.970(2) 0.490(3) 0.5762(11) 0.109(4) Uani 0.220(10) 1 d PDU . 1 O12 O 1.047(2) 0.5856(14) 0.489(2) 0.115(4) Uani 0.220(10) 1 d PDU . 1 O13 O 0.9273(17) 0.492(3) 0.4453(18) 0.116(3) Uani 0.220(10) 1 d PDU . 1 O14 O 1.0653(19) 0.4279(19) 0.482(2) 0.115(4) Uani 0.220(10) 1 d PDU . 1 O11' O 0.9141(12) 0.470(2) 0.5335(16) 0.115(4) Uani 0.280(10) 1 d PDU . 2 O12' O 0.994(2) 0.5955(7) 0.4812(16) 0.115(4) Uani 0.280(10) 1 d PDU . 2 O13' O 1.014(2) 0.4478(17) 0.4327(13) 0.115(4) Uani 0.280(10) 1 d PDU . 2 O14' O 1.0704(16) 0.484(2) 0.5555(17) 0.113(3) Uani 0.280(10) 1 d PDU . 2 Cl2 Cl 0.5000 0.5000 1.0000 0.306(9) Uani 1 4 d SDU . . O21 O 0.5926(11) 0.50(3) 1.0260(18) 0.305(11) Uiso 0.25 1 d PDU . . O23 O 0.5000 0.5000 0.9176(5) 0.305(11) Uiso 0.50 2 d SPDU . . O22 O 0.45(2) 0.581(14) 1.0247(18) 0.305(11) Uiso 0.25 1 d PDU . . O24 O 0.45(2) 0.420(15) 1.0242(18) 0.304(11) Uiso 0.25 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0584(3) 0.0584(3) 0.0462(3) 0.000 0.000 0.000 S1 0.134(6) 0.135(5) 0.126(5) 0.066(4) -0.030(5) -0.070(5) S2 0.189(8) 0.145(6) 0.134(6) -0.027(5) -0.020(6) -0.079(6) O1 0.127(8) 0.138(9) 0.111(8) 0.060(7) -0.002(7) -0.068(8) O2 0.178(9) 0.139(8) 0.111(8) -0.031(7) -0.031(8) -0.080(8) C1 0.127(9) 0.143(9) 0.138(10) 0.037(9) -0.012(8) -0.024(8) C2 0.132(11) 0.152(11) 0.144(12) 0.027(10) -0.019(10) -0.016(11) C3 0.135(11) 0.151(12) 0.136(12) 0.035(11) -0.026(11) -0.016(11) C4 0.133(12) 0.145(12) 0.130(12) 0.034(11) -0.036(11) -0.023(11) C5 0.126(11) 0.143(11) 0.127(11) 0.037(10) -0.041(10) -0.031(10) C6 0.125(8) 0.136(9) 0.125(9) 0.050(8) -0.030(7) -0.045(8) C7 0.147(8) 0.154(8) 0.139(8) 0.028(7) -0.023(7) -0.066(7) C8 0.161(8) 0.159(8) 0.146(8) 0.013(8) -0.014(8) -0.061(8) C9 0.168(8) 0.163(8) 0.149(7) 0.003(7) -0.014(7) -0.065(7) C10 0.178(9) 0.161(8) 0.144(8) -0.003(8) -0.013(8) -0.071(8) C11 0.160(9) 0.146(9) 0.133(9) -0.021(8) -0.031(8) -0.071(9) C12 0.153(12) 0.154(12) 0.134(12) -0.013(11) -0.033(11) -0.058(11) C13 0.158(13) 0.158(13) 0.138(13) -0.014(11) -0.038(11) -0.048(12) C14 0.160(13) 0.160(13) 0.141(13) -0.018(11) -0.038(11) -0.041(12) C15 0.160(12) 0.159(12) 0.147(12) -0.011(11) -0.034(11) -0.046(11) C16 0.153(10) 0.152(10) 0.136(9) -0.011(8) -0.037(9) -0.058(9) S1' 0.099(4) 0.164(7) 0.126(6) 0.017(5) 0.028(4) -0.039(5) S2' 0.167(7) 0.171(7) 0.118(5) 0.029(5) -0.058(5) -0.084(6) O1' 0.121(8) 0.162(9) 0.119(8) 0.034(8) 0.025(7) -0.050(8) O2' 0.165(9) 0.144(9) 0.104(8) 0.001(8) -0.046(8) -0.084(8) C1' 0.123(9) 0.148(9) 0.145(10) 0.022(9) 0.013(8) -0.025(8) C2' 0.129(11) 0.149(11) 0.153(11) 0.024(11) 0.018(10) -0.030(10) C3' 0.131(11) 0.148(12) 0.152(12) 0.021(12) 0.030(11) -0.037(11) C4' 0.127(11) 0.144(12) 0.148(13) 0.018(11) 0.028(10) -0.042(11) C5' 0.117(10) 0.135(11) 0.140(11) 0.020(10) 0.027(10) -0.042(10) C6' 0.110(8) 0.147(9) 0.134(9) 0.016(8) 0.029(8) -0.036(8) C7' 0.128(8) 0.163(9) 0.138(9) 0.005(8) 0.007(8) -0.047(8) C8' 0.154(7) 0.163(8) 0.146(7) 0.014(7) -0.006(7) -0.059(7) C9' 0.165(8) 0.164(8) 0.151(8) 0.007(8) -0.017(8) -0.063(8) C10' 0.169(8) 0.162(8) 0.140(7) 0.012(7) -0.023(7) -0.074(7) C11' 0.154(9) 0.157(9) 0.119(9) 0.021(8) -0.051(8) -0.068(8) C12' 0.154(11) 0.155(12) 0.119(11) 0.024(10) -0.043(10) -0.060(11) C13' 0.151(12) 0.158(13) 0.121(12) 0.017(11) -0.042(11) -0.048(12) C14' 0.147(12) 0.153(12) 0.119(12) 0.012(11) -0.040(10) -0.045(12) C15' 0.143(11) 0.150(12) 0.129(11) 0.005(10) -0.037(10) -0.049(11) C16' 0.144(10) 0.149(10) 0.128(9) 0.005(8) -0.044(8) -0.059(9) Cl1 0.0807(16) 0.137(3) 0.106(2) 0.000 0.000 -0.0002(17) O11 0.086(7) 0.137(7) 0.104(7) 0.006(7) -0.003(6) -0.001(7) O12 0.092(7) 0.141(7) 0.113(7) 0.008(7) 0.002(7) -0.005(7) O13 0.094(6) 0.145(6) 0.110(6) 0.004(6) -0.002(6) -0.007(6) O14 0.092(7) 0.142(7) 0.110(7) -0.001(7) 0.001(6) 0.003(7) O11' 0.092(6) 0.143(7) 0.111(7) 0.003(6) 0.002(6) -0.007(6) O12' 0.090(7) 0.142(7) 0.112(7) 0.011(6) -0.003(6) -0.007(7) O13' 0.093(7) 0.144(7) 0.107(7) -0.001(7) -0.003(6) -0.002(7) O14' 0.092(6) 0.140(6) 0.108(6) 0.007(6) -0.002(6) -0.004(6) Cl2 0.312(9) 0.312(9) 0.293(10) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O1' 2.21(2) 4_656 ? Eu1 O1' 2.21(2) 2_665 ? Eu1 O1' 2.21(2) . ? Eu1 O1' 2.21(2) 3_566 ? Eu1 O2 2.27(2) . ? Eu1 O2 2.27(2) 4_656 ? Eu1 O2 2.27(2) 3_566 ? Eu1 O2 2.27(2) 2_665 ? Eu1 O1 2.38(3) 2_665 ? Eu1 O1 2.38(2) 4_656 ? Eu1 O1 2.38(3) . ? Eu1 O1 2.38(2) 3_566 ? S1 O1 1.49(4) . ? S1 C7 1.73(2) . ? S1 C6 1.843(13) . ? S2 O2 1.38(3) . ? S2 C10 1.72(2) . ? S2 C11 1.846(13) . ? C1 C6 1.354(10) . ? C1 C2 1.356(10) . ? C2 C3 1.356(10) . ? C3 C4 1.358(10) . ? C4 C5 1.356(10) . ? C5 C6 1.356(10) . ? C7 C8 1.102(16) . ? C8 C9 1.095(16) . ? C9 C10 1.092(17) . ? C11 C12 1.372(4) . ? C11 C16 1.374(8) . ? C12 C13 1.372(4) . ? C13 C14 1.372(4) . ? C14 C15 1.371(4) . ? C15 C16 1.372(4) . ? S1' O1' 1.52(3) . ? S1' C7' 1.68(2) . ? S1' C6' 1.846(13) . ? S2' O2' 1.45(4) . ? S2' C10' 1.70(2) . ? S2' C11' 1.841(13) . ? C1' C6' 1.356(10) . ? C1' C2' 1.356(10) . ? C2' C3' 1.354(10) . ? C3' C4' 1.356(10) . ? C4' C5' 1.354(10) . ? C5' C6' 1.354(10) . ? C7' C8' 1.089(17) . ? C8' C9' 1.092(17) . ? C9' C10' 1.100(16) . ? C11' C16' 1.344(9) . ? C11' C12' 1.345(9) . ? C12' C13' 1.343(9) . ? C13' C14' 1.347(9) . ? C14' C15' 1.345(9) . ? C15' C16' 1.344(9) . ? Cl1 O11 1.408(9) 2_765 ? Cl1 O11 1.408(9) . ? Cl1 O13' 1.414(9) . ? Cl1 O13' 1.414(9) 2_765 ? Cl1 O12' 1.425(9) . ? Cl1 O12' 1.425(9) 2_765 ? Cl1 O14' 1.427(9) . ? Cl1 O14' 1.427(9) 2_765 ? Cl1 O13 1.429(9) . ? Cl1 O13 1.429(9) 2_765 ? Cl1 O12 1.431(9) . ? Cl1 O12 1.431(9) 2_765 ? O11 O11 0.92(6) 2_765 ? O12 O13 1.41(5) 2_765 ? O12 O14 1.65(3) 2_765 ? O13 O14 1.33(5) 2_765 ? O13 O12 1.41(5) 2_765 ? O14 O13 1.33(5) 2_765 ? O14 O12 1.65(3) 2_765 ? O11' O14' 0.80(4) 2_765 ? O12' O13' 1.06(4) 2_765 ? O13' O12' 1.06(4) 2_765 ? O13' O13' 1.56(5) 2_765 ? O14' O11' 0.80(4) 2_765 ? Cl2 O21 1.417(10) 4_657 ? Cl2 O21 1.417(10) . ? Cl2 O21 1.417(10) 2_665 ? Cl2 O21 1.417(10) 3_567 ? Cl2 O22 1.423(10) 3_567 ? Cl2 O22 1.423(10) 4_657 ? Cl2 O22 1.423(10) . ? Cl2 O22 1.423(10) 2_665 ? Cl2 O24 1.425(10) 2_665 ? Cl2 O24 1.425(10) 3_567 ? Cl2 O24 1.425(10) . ? Cl2 O24 1.425(10) 4_657 ? O21 O24 1.13(4) 4_657 ? O21 O22 1.15(4) 3_567 ? O21 O22 1.33(4) 2_665 ? O21 O24 1.34(4) 2_665 ? O21 O23 1.66(3) 3_567 ? O23 O21 1.66(3) 4_657 ? O23 O21 1.66(3) 3_567 ? O23 O22 1.69(3) 3_567 ? O23 O22 1.69(3) 4_657 ? O23 O24 1.70(3) 3_567 ? O23 O24 1.70(3) 4_657 ? O22 O24 1.08(4) 3_567 ? O22 O21 1.15(4) 4_657 ? O22 O21 1.33(4) 2_665 ? O22 O24 1.39(4) 2_665 ? O22 O23 1.69(3) 3_567 ? O24 O22 1.08(4) 4_657 ? O24 O21 1.13(4) 3_567 ? O24 O21 1.34(4) 2_665 ? O24 O22 1.39(4) 2_665 ? O24 O23 1.70(3) 3_567 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1' Eu1 O1' 107.1(8) 4_656 2_665 ? O1' Eu1 O1' 107.1(8) 4_656 . ? O1' Eu1 O1' 114.4(16) 2_665 . ? O1' Eu1 O1' 114.4(16) 4_656 3_566 ? O1' Eu1 O1' 107.1(8) 2_665 3_566 ? O1' Eu1 O1' 107.1(7) . 3_566 ? O1' Eu1 O2 27.4(9) 4_656 . ? O1' Eu1 O2 132.7(10) 2_665 . ? O1' Eu1 O2 85.2(9) . . ? O1' Eu1 O2 107.1(10) 3_566 . ? O1' Eu1 O2 85.2(9) 4_656 4_656 ? O1' Eu1 O2 27.4(9) 2_665 4_656 ? O1' Eu1 O2 107.1(10) . 4_656 ? O1' Eu1 O2 132.7(10) 3_566 4_656 ? O2 Eu1 O2 107.5(6) . 4_656 ? O1' Eu1 O2 132.7(10) 4_656 3_566 ? O1' Eu1 O2 107.1(10) 2_665 3_566 ? O1' Eu1 O2 27.4(9) . 3_566 ? O1' Eu1 O2 85.2(9) 3_566 3_566 ? O2 Eu1 O2 107.5(6) . 3_566 ? O2 Eu1 O2 113.5(13) 4_656 3_566 ? O1' Eu1 O2 107.1(10) 4_656 2_665 ? O1' Eu1 O2 85.2(9) 2_665 2_665 ? O1' Eu1 O2 132.7(10) . 2_665 ? O1' Eu1 O2 27.4(9) 3_566 2_665 ? O2 Eu1 O2 113.5(13) . 2_665 ? O2 Eu1 O2 107.5(6) 4_656 2_665 ? O2 Eu1 O2 107.5(6) 3_566 2_665 ? O1' Eu1 O1 129.3(10) 4_656 2_665 ? O1' Eu1 O1 23.5(9) 2_665 2_665 ? O1' Eu1 O1 107.9(11) . 2_665 ? O1' Eu1 O1 88.6(10) 3_566 2_665 ? O2 Eu1 O1 156.0(10) . 2_665 ? O2 Eu1 O1 50.0(10) 4_656 2_665 ? O2 Eu1 O1 91.5(9) 3_566 2_665 ? O2 Eu1 O1 72.8(10) 2_665 2_665 ? O1' Eu1 O1 23.5(9) 4_656 4_656 ? O1' Eu1 O1 88.6(10) 2_665 4_656 ? O1' Eu1 O1 129.3(9) . 4_656 ? O1' Eu1 O1 107.9(11) 3_566 4_656 ? O2 Eu1 O1 50.0(10) . 4_656 ? O2 Eu1 O1 72.8(10) 4_656 4_656 ? O2 Eu1 O1 156.0(10) 3_566 4_656 ? O2 Eu1 O1 91.5(9) 2_665 4_656 ? O1 Eu1 O1 108.4(8) 2_665 4_656 ? O1' Eu1 O1 88.6(10) 4_656 . ? O1' Eu1 O1 107.9(11) 2_665 . ? O1' Eu1 O1 23.5(9) . . ? O1' Eu1 O1 129.3(10) 3_566 . ? O2 Eu1 O1 72.8(10) . . ? O2 Eu1 O1 91.5(9) 4_656 . ? O2 Eu1 O1 50.0(10) 3_566 . ? O2 Eu1 O1 156.0(10) 2_665 . ? O1 Eu1 O1 111.5(16) 2_665 . ? O1 Eu1 O1 108.4(8) 4_656 . ? O1' Eu1 O1 107.9(11) 4_656 3_566 ? O1' Eu1 O1 129.3(10) 2_665 3_566 ? O1' Eu1 O1 88.6(10) . 3_566 ? O1' Eu1 O1 23.5(9) 3_566 3_566 ? O2 Eu1 O1 91.5(9) . 3_566 ? O2 Eu1 O1 156.0(10) 4_656 3_566 ? O2 Eu1 O1 72.8(10) 3_566 3_566 ? O2 Eu1 O1 50.0(10) 2_665 3_566 ? O1 Eu1 O1 108.4(8) 2_665 3_566 ? O1 Eu1 O1 111.5(16) 4_656 3_566 ? O1 Eu1 O1 108.4(8) . 3_566 ? O1 S1 C7 115(2) . . ? O1 S1 C6 109.9(19) . . ? C7 S1 C6 107.2(18) . . ? O2 S2 C10 123(3) . . ? O2 S2 C11 106.3(19) . . ? C10 S2 C11 87.0(19) . . ? S1 O1 Eu1 143(3) . . ? S2 O2 Eu1 157(2) . . ? C6 C1 C2 120(3) . . ? C3 C2 C1 113(3) . . ? C2 C3 C4 122(3) . . ? C5 C4 C3 116(3) . . ? C4 C5 C6 123(3) . . ? C1 C6 C5 115(3) . . ? C1 C6 S1 121(2) . . ? C5 C6 S1 121(2) . . ? C8 C7 S1 118(2) . . ? C9 C8 C7 138(3) . . ? C10 C9 C8 143(4) . . ? C9 C10 S2 120(2) . . ? C12 C11 C16 127(3) . . ? C12 C11 S2 104(3) . . ? C16 C11 S2 125(3) . . ? C11 C12 C13 107(3) . . ? C12 C13 C14 124(3) . . ? C15 C14 C13 103(3) . . ? C14 C15 C16 122(3) . . ? C15 C16 C11 107(3) . . ? O1' S1' C7' 117(2) . . ? O1' S1' C6' 103.1(17) . . ? C7' S1' C6' 100(2) . . ? O2' S2' C10' 103(2) . . ? O2' S2' C11' 119(2) . . ? C10' S2' C11' 112(2) . . ? S1' O1' Eu1 146(2) . . ? S2' O2' Eu1 132(3) . . ? C6' C1' C2' 121(3) . . ? C3' C2' C1' 117(3) . . ? C2' C3' C4' 122(3) . . ? C5' C4' C3' 115(3) . . ? C6' C5' C4' 122(3) . . ? C5' C6' C1' 117(3) . . ? C5' C6' S1' 102(2) . . ? C1' C6' S1' 140(3) . . ? C8' C7' S1' 124(2) . . ? C7' C8' C9' 143(5) . . ? C8' C9' C10' 138(4) . . ? C9' C10' S2' 120(2) . . ? C16' C11' C12' 126(3) . . ? C16' C11' S2' 102(2) . . ? C12' C11' S2' 132(3) . . ? C13' C12' C11' 114(3) . . ? C12' C13' C14' 126(3) . . ? C15' C14' C13' 114(3) . . ? C16' C15' C14' 126(3) . . ? C11' C16' C15' 113(3) . . ? O11 Cl1 O11 38(2) 2_765 . ? O11 Cl1 O13' 142.8(16) 2_765 . ? O11 Cl1 O13' 141.1(18) . . ? O11 Cl1 O13' 141.1(18) 2_765 2_765 ? O11 Cl1 O13' 142.8(16) . 2_765 ? O13' Cl1 O13' 67(2) . 2_765 ? O11 Cl1 O12' 98.2(19) 2_765 . ? O11 Cl1 O12' 107(2) . . ? O13' Cl1 O12' 109.5(13) . . ? O13' Cl1 O12' 43.9(18) 2_765 . ? O11 Cl1 O12' 107(2) 2_765 2_765 ? O11 Cl1 O12' 98.2(19) . 2_765 ? O13' Cl1 O12' 43.9(18) . 2_765 ? O13' Cl1 O12' 109.5(13) 2_765 2_765 ? O12' Cl1 O12' 153(2) . 2_765 ? O11 Cl1 O14' 31.9(15) 2_765 . ? O11 Cl1 O14' 64(2) . . ? O13' Cl1 O14' 112.2(13) . . ? O13' Cl1 O14' 139.0(16) 2_765 . ? O12' Cl1 O14' 111.1(12) . . ? O12' Cl1 O14' 87.4(17) 2_765 . ? O11 Cl1 O14' 64(2) 2_765 2_765 ? O11 Cl1 O14' 31.9(15) . 2_765 ? O13' Cl1 O14' 139.0(16) . 2_765 ? O13' Cl1 O14' 112.2(12) 2_765 2_765 ? O12' Cl1 O14' 87.4(17) . 2_765 ? O12' Cl1 O14' 111.1(12) 2_765 2_765 ? O14' Cl1 O14' 94(3) . 2_765 ? O11 Cl1 O13 151(2) 2_765 . ? O11 Cl1 O13 113.3(14) . . ? O13' Cl1 O13 60(2) . . ? O13' Cl1 O13 51.6(18) 2_765 . ? O12' Cl1 O13 83.0(19) . . ? O12' Cl1 O13 79.0(18) 2_765 . ? O14' Cl1 O13 166(2) . . ? O14' Cl1 O13 86.7(15) 2_765 . ? O11 Cl1 O13 113.3(13) 2_765 2_765 ? O11 Cl1 O13 151(2) . 2_765 ? O13' Cl1 O13 51.6(18) . 2_765 ? O13' Cl1 O13 60(2) 2_765 2_765 ? O12' Cl1 O13 79.0(18) . 2_765 ? O12' Cl1 O13 83.0(19) 2_765 2_765 ? O14' Cl1 O13 86.7(15) . 2_765 ? O14' Cl1 O13 166(2) 2_765 2_765 ? O13 Cl1 O13 96(3) . 2_765 ? O11 Cl1 O12 84(3) 2_765 . ? O11 Cl1 O12 111.6(13) . . ? O13' Cl1 O12 106.2(18) . . ? O13' Cl1 O12 59.1(19) 2_765 . ? O12' Cl1 O12 32.2(13) . . ? O12' Cl1 O12 141.3(15) 2_765 . ? O14' Cl1 O12 84.1(18) . . ? O14' Cl1 O12 107.1(17) 2_765 . ? O13 Cl1 O12 109.1(13) . . ? O13 Cl1 O12 59(2) 2_765 . ? O11 Cl1 O12 111.6(13) 2_765 2_765 ? O11 Cl1 O12 84(3) . 2_765 ? O13' Cl1 O12 59.1(19) . 2_765 ? O13' Cl1 O12 106.2(18) 2_765 2_765 ? O12' Cl1 O12 141.3(15) . 2_765 ? O12' Cl1 O12 32.2(13) 2_765 2_765 ? O14' Cl1 O12 107.1(17) . 2_765 ? O14' Cl1 O12 84.1(18) 2_765 2_765 ? O13 Cl1 O12 59(2) . 2_765 ? O13 Cl1 O12 109.1(13) 2_765 2_765 ? O12 Cl1 O12 164(3) . 2_765 ? O11 O11 Cl1 70.9(12) 2_765 . ? O13 O12 Cl1 60.5(13) 2_765 . ? O13 O12 O14 97(2) 2_765 2_765 ? Cl1 O12 O14 55.4(8) . 2_765 ? O14 O13 O12 114(2) 2_765 2_765 ? O14 O13 Cl1 62.9(12) 2_765 . ? O12 O13 Cl1 60.6(12) 2_765 . ? O13 O14 Cl1 61.9(12) 2_765 . ? O13 O14 O12 102(2) 2_765 2_765 ? Cl1 O14 O12 54.7(8) . 2_765 ? O14' O11' Cl1 72.9(12) 2_765 . ? O13' O12' Cl1 67.5(12) 2_765 . ? O12' O13' Cl1 68.6(11) 2_765 . ? O12' O13' O13' 123.0(14) 2_765 2_765 ? Cl1 O13' O13' 56.5(12) . 2_765 ? O11' O14' Cl1 74.7(12) 2_765 . ? O21 Cl2 O21 95.9(9) 4_657 . ? O21 Cl2 O21 95.9(8) 4_657 2_665 ? O21 Cl2 O21 143(3) . 2_665 ? O21 Cl2 O21 143(3) 4_657 3_567 ? O21 Cl2 O21 95.9(8) . 3_567 ? O21 Cl2 O21 95.9(9) 2_665 3_567 ? O21 Cl2 O22 55.7(17) 4_657 3_567 ? O21 Cl2 O22 48(2) . 3_567 ? O21 Cl2 O22 150.5(16) 2_665 3_567 ? O21 Cl2 O22 111.6(14) 3_567 3_567 ? O21 Cl2 O22 111.6(14) 4_657 4_657 ? O21 Cl2 O22 150.5(16) . 4_657 ? O21 Cl2 O22 48(2) 2_665 4_657 ? O21 Cl2 O22 55.7(17) 3_567 4_657 ? O22 Cl2 O22 145(3) 3_567 4_657 ? O21 Cl2 O22 48(2) 4_657 . ? O21 Cl2 O22 111.6(14) . . ? O21 Cl2 O22 55.7(17) 2_665 . ? O21 Cl2 O22 150.5(16) 3_567 . ? O22 Cl2 O22 95.3(8) 3_567 . ? O22 Cl2 O22 95.3(8) 4_657 . ? O21 Cl2 O22 150.5(16) 4_657 2_665 ? O21 Cl2 O22 55.7(17) . 2_665 ? O21 Cl2 O22 111.6(14) 2_665 2_665 ? O21 Cl2 O22 48(2) 3_567 2_665 ? O22 Cl2 O22 95.3(8) 3_567 2_665 ? O22 Cl2 O22 95.3(8) 4_657 2_665 ? O22 Cl2 O22 145(3) . 2_665 ? O21 Cl2 O24 47(2) 4_657 2_665 ? O21 Cl2 O24 56.3(17) . 2_665 ? O21 Cl2 O24 111.3(14) 2_665 2_665 ? O21 Cl2 O24 151.0(16) 3_567 2_665 ? O22 Cl2 O24 44.8(19) 3_567 2_665 ? O22 Cl2 O24 152.9(15) 4_657 2_665 ? O22 Cl2 O24 58.5(17) . 2_665 ? O22 Cl2 O24 110.0(14) 2_665 2_665 ? O21 Cl2 O24 56.3(17) 4_657 3_567 ? O21 Cl2 O24 151.0(16) . 3_567 ? O21 Cl2 O24 47(2) 2_665 3_567 ? O21 Cl2 O24 111.3(14) 3_567 3_567 ? O22 Cl2 O24 110.0(14) 3_567 3_567 ? O22 Cl2 O24 58.5(17) 4_657 3_567 ? O22 Cl2 O24 44.8(19) . 3_567 ? O22 Cl2 O24 152.9(16) 2_665 3_567 ? O24 Cl2 O24 95.1(8) 2_665 3_567 ? O21 Cl2 O24 151.0(16) 4_657 . ? O21 Cl2 O24 111.3(14) . . ? O21 Cl2 O24 56.3(17) 2_665 . ? O21 Cl2 O24 47(2) 3_567 . ? O22 Cl2 O24 152.9(15) 3_567 . ? O22 Cl2 O24 44.8(19) 4_657 . ? O22 Cl2 O24 110.0(14) . . ? O22 Cl2 O24 58.5(17) 2_665 . ? O24 Cl2 O24 145(3) 2_665 . ? O24 Cl2 O24 95.1(8) 3_567 . ? O21 Cl2 O24 111.3(14) 4_657 4_657 ? O21 Cl2 O24 47(2) . 4_657 ? O21 Cl2 O24 151.0(16) 2_665 4_657 ? O21 Cl2 O24 56.3(17) 3_567 4_657 ? O22 Cl2 O24 58.5(17) 3_567 4_657 ? O22 Cl2 O24 110.0(14) 4_657 4_657 ? O22 Cl2 O24 152.9(16) . 4_657 ? O22 Cl2 O24 44.8(19) 2_665 4_657 ? O24 Cl2 O24 95.1(8) 2_665 4_657 ? O24 Cl2 O24 145(3) 3_567 4_657 ? O24 Cl2 O24 95.1(8) . 4_657 ? O24 O21 O22 75(2) 4_657 3_567 ? O24 O21 O22 52(3) 4_657 2_665 ? O22 O21 O22 116.5(15) 3_567 2_665 ? O24 O21 O24 116.3(15) 4_657 2_665 ? O22 O21 O24 51(2) 3_567 2_665 ? O22 O21 O24 122(2) 2_665 2_665 ? O24 O21 Cl2 67.0(12) 4_657 . ? O22 O21 Cl2 66.5(12) 3_567 . ? O22 O21 Cl2 62.4(10) 2_665 . ? O24 O21 Cl2 62.1(10) 2_665 . ? O24 O21 O23 109.9(15) 4_657 3_567 ? O22 O21 O23 109.4(15) 3_567 3_567 ? O22 O21 O23 67.7(19) 2_665 3_567 ? O24 O21 O23 67.8(19) 2_665 3_567 ? Cl2 O21 O23 55.0(8) . 3_567 ? Cl2 O23 O21 53.7(8) . 4_657 ? Cl2 O23 O21 53.7(8) . 3_567 ? O21 O23 O21 107.4(16) 4_657 3_567 ? Cl2 O23 O22 53.4(8) . 3_567 ? O21 O23 O22 46.6(13) 4_657 3_567 ? O21 O23 O22 88.9(14) 3_567 3_567 ? Cl2 O23 O22 53.4(8) . 4_657 ? O21 O23 O22 88.9(14) 4_657 4_657 ? O21 O23 O22 46.6(13) 3_567 4_657 ? O22 O23 O22 106.7(15) 3_567 4_657 ? Cl2 O23 O24 53.2(8) . 3_567 ? O21 O23 O24 47.0(13) 4_657 3_567 ? O21 O23 O24 88.4(14) 3_567 3_567 ? O22 O23 O24 87.0(14) 3_567 3_567 ? O22 O23 O24 48.5(13) 4_657 3_567 ? Cl2 O23 O24 53.2(8) . 4_657 ? O21 O23 O24 88.4(14) 4_657 4_657 ? O21 O23 O24 47.0(13) 3_567 4_657 ? O22 O23 O24 48.5(13) 3_567 4_657 ? O22 O23 O24 87.0(14) 4_657 4_657 ? O24 O23 O24 106.4(15) 3_567 4_657 ? O24 O22 O21 74(2) 3_567 4_657 ? O24 O22 O21 55(3) 3_567 2_665 ? O21 O22 O21 116.6(15) 4_657 2_665 ? O24 O22 O24 115.7(15) 3_567 2_665 ? O21 O22 O24 52(2) 4_657 2_665 ? O21 O22 O24 119(2) 2_665 2_665 ? O24 O22 Cl2 67.7(12) 3_567 . ? O21 O22 Cl2 65.9(12) 4_657 . ? O21 O22 Cl2 61.9(10) 2_665 . ? O24 O22 Cl2 60.8(10) 2_665 . ? O24 O22 O23 110.7(15) 3_567 3_567 ? O21 O22 O23 108.5(14) 4_657 3_567 ? O21 O22 O23 65.7(19) 2_665 3_567 ? O24 O22 O23 66.1(18) 2_665 3_567 ? Cl2 O22 O23 54.3(8) . 3_567 ? O22 O24 O21 74(2) 4_657 3_567 ? O22 O24 O21 55(3) 4_657 2_665 ? O21 O24 O21 116.5(15) 3_567 2_665 ? O22 O24 O22 115.8(15) 4_657 2_665 ? O21 O24 O22 53(2) 3_567 2_665 ? O21 O24 O22 119(2) 2_665 2_665 ? O22 O24 Cl2 67.5(12) 4_657 . ? O21 O24 Cl2 66.2(12) 3_567 . ? O21 O24 Cl2 61.5(10) 2_665 . ? O22 O24 Cl2 60.7(10) 2_665 . ? O22 O24 O23 110.4(15) 4_657 3_567 ? O21 O24 O23 108.7(14) 3_567 3_567 ? O21 O24 O23 65.2(19) 2_665 3_567 ? O22 O24 O23 65.4(18) 2_665 3_567 ? Cl2 O24 O23 54.1(8) . 3_567 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.259 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.113 #===END data_Complex_3 _database_code_depnum_ccdc_archive 'CCDC 200617' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H72 Cl3 Gd O20 S8' _chemical_formula_weight 1681.30 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, -z' 'y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' _cell_length_a 14.469(2) _cell_length_b 14.469(2) _cell_length_c 17.509(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3665.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1023 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 26.13 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1718 _exptl_absorpt_coefficient_mu 1.311 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.775787 _exptl_absorpt_correction_T_max 1.0000 _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 _diffrn_measurement_method 'omig and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7596 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3215 _reflns_number_gt 2950 _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^)+(0.1615P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.513(12) _refine_ls_number_reflns 3215 _refine_ls_number_parameters 459 _refine_ls_number_restraints 643 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.1902 _refine_ls_wR_factor_gt 0.1806 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.962 _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 Gd1 Gd 0.5000 0.5000 0.5000 0.05119(5) Uani 1 4 d S . . S1 S 0.57236(15) 0.71501(15) 0.40587(11) 0.0990(6) Uani 0.50 1 d PDU A 1 S2 S 0.52276(12) 0.7294(2) 0.59059(14) 0.1530(9) Uani 0.50 1 d PDU A 1 O1 O 0.5425(4) 0.6351(3) 0.4255(4) 0.0985(11) Uani 0.50 1 d PU A 1 O2 O 0.4728(7) 0.6361(4) 0.5722(4) 0.1393(16) Uani 0.50 1 d PU A 1 C1 C 0.5721(3) 0.64722(16) 0.25749(13) 0.1095(12) Uani 0.50 1 d PDU A 1 H1A H 0.5920 0.5898 0.2748 0.131 Uiso 0.50 1 calc PR A 1 C2 C 0.5529(3) 0.66937(18) 0.18307(13) 0.1111(14) Uani 0.50 1 d PDU A 1 H2A H 0.5706 0.6250 0.1475 0.133 Uiso 0.50 1 calc PR A 1 C3 C 0.5117(3) 0.74648(18) 0.15255(13) 0.1107(14) Uani 0.50 1 d PDU A 1 H3A H 0.4986 0.7556 0.1011 0.133 Uiso 0.50 1 calc PR A 1 C4 C 0.4931(4) 0.80792(19) 0.21017(12) 0.1073(14) Uani 0.50 1 d PDU A 1 H4A H 0.4703 0.8648 0.1941 0.129 Uiso 0.50 1 calc PR A 1 C5 C 0.5026(3) 0.79886(18) 0.28792(13) 0.0997(14) Uani 0.50 1 d PDU A 1 H5A H 0.4766 0.8374 0.3246 0.120 Uiso 0.50 1 calc PR A 1 C6 C 0.5570(3) 0.72330(17) 0.30211(11) 0.1005(12) Uani 0.50 1 d PDU A 1 C7 C 0.6669(3) 0.7737(5) 0.42919(9) 0.1125(14) Uani 0.50 1 d PDU A 1 H7A H 0.7173 0.7522 0.3973 0.135 Uiso 0.50 1 calc PR A 1 H7B H 0.6567 0.8383 0.4172 0.135 Uiso 0.50 1 calc PR A 1 C8 C 0.6905(3) 0.7682(2) 0.49489(7) 0.1299(10) Uani 0.50 1 d PDU A 1 H8A H 0.6822 0.8320 0.5103 0.156 Uiso 0.50 1 calc PR A 1 H8B H 0.7568 0.7621 0.4880 0.156 Uiso 0.50 1 calc PR A 1 C9 C 0.68230(15) 0.73083(18) 0.55594(9) 0.1379(9) Uani 0.50 1 d PDU A 1 H9A H 0.7114 0.7759 0.5891 0.166 Uiso 0.50 1 calc PR A 1 H9B H 0.7277 0.6818 0.5513 0.166 Uiso 0.50 1 calc PR A 1 C10 C 0.62806(10) 0.6958(2) 0.59951(10) 0.1432(9) Uani 0.50 1 d PDU A 1 H10A H 0.6481 0.7087 0.6513 0.172 Uiso 0.50 1 calc PR A 1 H10B H 0.6301 0.6294 0.5925 0.172 Uiso 0.50 1 calc PR A 1 C11 C 0.53831(17) 0.73801(11) 0.69476(8) 0.1476(12) Uani 0.50 1 d PDU A 1 C12 C 0.5096(3) 0.82024(12) 0.72559(8) 0.1477(15) Uani 0.50 1 d PDU A 1 H12A H 0.4964 0.8684 0.6921 0.177 Uiso 0.50 1 calc PR A 1 C13 C 0.4989(3) 0.83662(12) 0.80224(8) 0.1462(14) Uani 0.50 1 d PDU A 1 H13A H 0.4757 0.8919 0.8214 0.175 Uiso 0.50 1 calc PR A 1 C14 C 0.52541(16) 0.76460(11) 0.84810(10) 0.1493(15) Uani 0.50 1 d PDU A 1 H14A H 0.5037 0.7632 0.8981 0.179 Uiso 0.50 1 calc PR A 1 C15 C 0.58213(18) 0.69448(14) 0.82420(8) 0.1538(15) Uani 0.50 1 d PDU A 1 H15A H 0.6160 0.6577 0.8576 0.185 Uiso 0.50 1 calc PR A 1 C16 C 0.5844(3) 0.6835(2) 0.74645(8) 0.1510(15) Uani 0.50 1 d PDU A 1 H16A H 0.6199 0.6353 0.7272 0.181 Uiso 0.50 1 calc PR A 1 S1' S 0.71865(14) 0.55987(16) 0.40991(11) 0.0923(6) Uani 0.50 1 d PDU A 2 S2' S 0.6905(2) 0.60101(19) 0.61136(14) 0.1509(8) Uani 0.50 1 d PDU A 2 O1' O 0.5984(4) 0.5956(4) 0.4165(4) 0.0954(10) Uani 0.50 1 d PU A 2 O2' O 0.6067(5) 0.5882(6) 0.5777(4) 0.1373(13) Uani 0.50 1 d PU A 2 C1' C 0.67152(18) 0.5884(3) 0.24475(12) 0.1086(12) Uani 0.50 1 d PDU A 2 H1'A H 0.6226 0.6284 0.2546 0.130 Uiso 0.50 1 calc PR A 2 C2' C 0.68895(17) 0.5636(3) 0.17091(13) 0.1137(14) Uani 0.50 1 d PDU A 2 H2'A H 0.6464 0.5738 0.1320 0.136 Uiso 0.50 1 calc PR A 2 C3' C 0.77254(17) 0.5230(3) 0.15752(13) 0.1151(14) Uani 0.50 1 d PDU A 2 H3'A H 0.7902 0.5128 0.1072 0.138 Uiso 0.50 1 calc PR A 2 C4' C 0.83146(18) 0.4965(3) 0.21432(13) 0.1117(14) Uani 0.50 1 d PDU A 2 H4'A H 0.8903 0.4740 0.2040 0.134 Uiso 0.50 1 calc PR A 2 C5' C 0.79891(18) 0.5051(3) 0.28743(13) 0.1026(14) Uani 0.50 1 d PDU A 2 H5'A H 0.8297 0.4746 0.3266 0.123 Uiso 0.50 1 calc PR A 2 C6' C 0.72282(19) 0.5569(3) 0.30481(11) 0.0989(12) Uani 0.50 1 d PDU A 2 C7' C 0.7740(6) 0.6591(3) 0.42025(16) 0.1117(14) Uani 0.50 1 d PDU A 2 H7'A H 0.8367 0.6511 0.4016 0.134 Uiso 0.50 1 calc PR A 2 H7'B H 0.7444 0.7047 0.3879 0.134 Uiso 0.50 1 calc PR A 2 C8' C 0.7779(4) 0.6895(3) 0.48348(13) 0.1279(11) Uani 0.50 1 d PDU A 2 H8'A H 0.8341 0.7255 0.4777 0.153 Uiso 0.50 1 calc PR A 2 H8'B H 0.7985 0.6339 0.5092 0.153 Uiso 0.50 1 calc PR A 2 C9' C 0.7472(3) 0.7290(3) 0.53806(13) 0.1350(11) Uani 0.50 1 d PDU A 2 H9'A H 0.6970 0.7644 0.5158 0.162 Uiso 0.50 1 calc PR A 2 H9'B H 0.7950 0.7742 0.5486 0.162 Uiso 0.50 1 calc PR A 2 C10' C 0.7178(5) 0.7127(4) 0.60132(17) 0.1429(11) Uani 0.50 1 d PDU A 2 H10C H 0.6633 0.7502 0.6106 0.171 Uiso 0.50 1 calc PR A 2 H10D H 0.7641 0.7293 0.6390 0.171 Uiso 0.50 1 calc PR A 2 C11' C 0.74195(15) 0.5452(3) 0.69557(12) 0.1428(12) Uani 0.50 1 d PDU A 2 C12' C 0.81512(17) 0.5062(4) 0.73260(13) 0.1448(15) Uani 0.50 1 d PDU A 2 H12B H 0.8678 0.4886 0.7060 0.174 Uiso 0.50 1 calc PR A 2 C13' C 0.80911(17) 0.4938(4) 0.80973(13) 0.1443(15) Uani 0.50 1 d PDU A 2 H13B H 0.8574 0.4651 0.8355 0.173 Uiso 0.50 1 calc PR A 2 C14' C 0.73362(17) 0.5227(3) 0.84963(13) 0.1445(15) Uani 0.50 1 d PDU A 2 H14B H 0.7299 0.5140 0.9022 0.173 Uiso 0.50 1 calc PR A 2 C15' C 0.66363(18) 0.5648(4) 0.81077(13) 0.1459(15) Uani 0.50 1 d PDU A 2 H15B H 0.6168 0.5944 0.8377 0.175 Uiso 0.50 1 calc PR A 2 C16' C 0.66148(17) 0.5639(4) 0.73295(13) 0.1445(15) Uani 0.50 1 d PDU A 2 H16B H 0.6071 0.5756 0.7063 0.173 Uiso 0.50 1 calc PR A 2 Cl1 Cl 1.0000 0.5000 0.49934(12) 0.0903(3) Uani 1 2 d SDU . . O11 O 0.9699(4) 0.4912(6) 0.57513(18) 0.0954(12) Uani 0.255(3) 1 d PDU . 1 O12 O 1.0482(3) 0.5849(2) 0.4854(4) 0.0975(12) Uani 0.255(3) 1 d PDU . 1 O13 O 0.9269(3) 0.4933(6) 0.4444(2) 0.0952(10) Uani 0.255(3) 1 d PDU . 1 O14 O 1.0641(3) 0.4272(3) 0.4808(4) 0.0985(12) Uani 0.255(3) 1 d PDU . 1 O11' O 0.9148(2) 0.4692(5) 0.5323(3) 0.0977(12) Uani 0.245(3) 1 d PDU . 2 O12' O 0.9952(5) 0.5969(2) 0.4850(4) 0.0946(12) Uani 0.245(3) 1 d PDU . 2 O13' O 1.0135(5) 0.4532(4) 0.4293(2) 0.0982(12) Uani 0.245(3) 1 d PDU . 2 O14' O 1.0729(3) 0.4798(5) 0.5518(3) 0.0954(11) Uani 0.245(3) 1 d PDU . 2 Cl2 Cl 0.5000 0.5000 1.0000 0.2750(10) Uani 1 4 d SDU . . O21 O 0.5921(2) 0.5099(7) 1.0254(4) 0.273(2) Uiso 0.25 1 d PDU . . O23 O 0.5000 0.5000 0.91754(17) 0.274(2) Uiso 0.50 2 d SPDU . . O22 O 0.4437(3) 0.5756(3) 1.0228(4) 0.273(2) Uiso 0.25 1 d PDU . . O24 O 0.4601(4) 0.4149(2) 1.0234(4) 0.273(2) Uiso 0.25 1 d PDU . . 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 0.05380(6) 0.05380(6) 0.04596(9) 0.000 0.000 0.000 S1 0.0888(10) 0.0888(9) 0.1195(12) 0.0416(9) -0.0188(9) -0.0410(8) S2 0.2056(18) 0.1384(14) 0.1149(15) -0.0392(13) 0.0098(15) -0.0750(14) O1 0.102(2) 0.0855(18) 0.108(2) 0.0573(17) -0.006(2) -0.0392(18) O2 0.199(3) 0.118(3) 0.101(3) -0.067(2) 0.020(3) -0.060(3) C1 0.099(2) 0.101(2) 0.128(2) 0.026(2) 0.010(2) -0.016(2) C2 0.097(2) 0.106(2) 0.131(3) 0.021(2) 0.015(2) -0.020(2) C3 0.102(2) 0.106(2) 0.124(3) 0.030(2) 0.011(2) -0.020(2) C4 0.101(2) 0.095(2) 0.126(2) 0.031(2) 0.002(2) -0.030(2) C5 0.090(2) 0.088(2) 0.120(2) 0.036(2) -0.002(2) -0.032(2) C6 0.092(2) 0.092(2) 0.117(2) 0.035(2) -0.008(2) -0.0316(19) C7 0.116(2) 0.093(2) 0.129(2) 0.030(2) -0.027(2) -0.043(2) C8 0.1376(18) 0.1251(18) 0.1269(18) 0.0125(19) -0.0273(18) -0.0440(17) C9 0.1465(16) 0.1418(16) 0.1255(16) 0.0061(16) -0.0284(16) -0.0591(16) C10 0.1616(16) 0.1509(16) 0.1170(16) -0.0105(16) -0.0405(16) -0.0752(16) C11 0.193(2) 0.137(2) 0.113(2) -0.054(2) 0.010(2) -0.071(2) C12 0.187(3) 0.142(3) 0.115(2) -0.057(2) 0.017(3) -0.064(2) C13 0.182(3) 0.143(2) 0.114(2) -0.064(2) 0.011(3) -0.062(2) C14 0.186(3) 0.146(3) 0.116(2) -0.065(2) 0.006(3) -0.059(2) C15 0.193(3) 0.142(3) 0.126(3) -0.058(2) 0.005(3) -0.055(3) C16 0.195(3) 0.133(3) 0.125(3) -0.061(2) 0.010(3) -0.060(3) S1' 0.0649(9) 0.0982(11) 0.1140(13) 0.0088(10) 0.0217(9) -0.0161(9) S2' 0.1657(14) 0.1689(15) 0.1183(13) 0.0203(13) -0.0578(12) -0.0811(13) O1' 0.0852(18) 0.0921(18) 0.1090(19) 0.0398(17) 0.0043(17) -0.0354(17) O2' 0.146(2) 0.158(2) 0.108(2) 0.002(2) -0.062(2) -0.090(2) C1' 0.099(2) 0.103(2) 0.124(2) 0.015(2) 0.030(2) -0.008(2) C2' 0.111(2) 0.106(2) 0.125(2) 0.012(2) 0.039(2) -0.006(2) C3' 0.113(2) 0.108(2) 0.124(2) 0.007(2) 0.046(2) -0.014(2) C4' 0.106(2) 0.103(2) 0.126(2) 0.004(2) 0.048(2) -0.010(2) C5' 0.094(2) 0.095(2) 0.120(2) 0.011(2) 0.047(2) -0.015(2) C6' 0.084(2) 0.096(2) 0.117(2) 0.010(2) 0.0356(19) -0.0181(19) C7' 0.092(2) 0.121(2) 0.122(2) 0.001(2) -0.001(2) -0.027(2) C8' 0.1243(18) 0.1339(18) 0.1254(19) 0.0105(18) -0.0239(18) -0.0433(18) C9' 0.1385(18) 0.1387(18) 0.1278(18) 0.0039(18) -0.0332(18) -0.0585(18) C10' 0.1545(18) 0.1492(18) 0.1250(18) 0.0065(18) -0.0394(18) -0.0721(18) C11' 0.157(2) 0.160(2) 0.111(2) 0.013(2) -0.060(2) -0.065(2) C12' 0.159(3) 0.163(3) 0.112(2) 0.013(3) -0.055(2) -0.049(3) C13' 0.158(3) 0.163(3) 0.111(3) 0.010(3) -0.054(2) -0.038(3) C14' 0.158(3) 0.164(3) 0.111(3) 0.005(3) -0.054(2) -0.035(3) C15' 0.157(3) 0.164(3) 0.117(3) 0.003(3) -0.053(2) -0.034(3) C16' 0.157(3) 0.161(3) 0.115(3) 0.004(3) -0.060(2) -0.047(3) Cl1 0.0673(5) 0.1124(7) 0.0911(6) 0.000 0.000 -0.0001(5) O11 0.076(2) 0.113(2) 0.098(2) 0.006(2) -0.002(2) 0.000(2) O12 0.078(2) 0.116(2) 0.098(2) 0.007(2) 0.004(2) -0.001(2) O13 0.0749(18) 0.1170(18) 0.0937(18) 0.0046(18) -0.0014(18) -0.0026(18) O14 0.081(2) 0.117(2) 0.098(2) -0.002(2) 0.004(2) 0.004(2) O11' 0.076(2) 0.118(2) 0.099(2) 0.004(2) 0.002(2) -0.003(2) O12' 0.072(2) 0.116(2) 0.096(2) 0.012(2) -0.001(2) 0.000(2) O13' 0.079(2) 0.118(2) 0.098(2) -0.001(2) -0.002(2) -0.001(2) O14' 0.0762(18) 0.1139(18) 0.0960(18) 0.0053(18) 0.0007(18) -0.0007(18) Cl2 0.2813(13) 0.2813(13) 0.2624(18) 0.000 0.000 0.000 _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 O2 2.373(7) . ? Gd1 O2 2.373(7) 3_656 ? Gd1 O2 2.373(7) 4_566 ? Gd1 O2 2.373(7) 2_665 ? Gd1 O2' 2.421(7) . ? Gd1 O2' 2.421(7) 2_665 ? Gd1 O2' 2.421(7) 3_656 ? Gd1 O2' 2.421(7) 4_566 ? Gd1 O1 2.429(5) 4_566 ? Gd1 O1 2.429(5) 3_656 ? Gd1 O1 2.429(5) . ? Gd1 O1 2.429(5) 2_665 ? S1 O1 1.281(6) . ? S1 C7 1.660(5) . ? S1 C6 1.834(3) . ? S2 O2 1.564(8) . ? S2 C10 1.607(2) . ? S2 C11 1.842(3) . ? C1 C6 1.367(3) . ? C1 C2 1.370(3) . ? C2 C3 1.373(4) . ? C3 C4 1.371(3) . ? C4 C5 1.375(3) . ? C5 C6 1.370(4) . ? C7 C8 1.203(2) . ? C8 C9 1.204(2) . ? C9 C10 1.206(2) . ? C11 C12 1.371(2) . ? C11 C16 1.373(3) . ? C12 C13 1.3715(19) . ? C13 C14 1.370(2) . ? C14 C15 1.370(3) . ? C15 C16 1.371(2) . ? S1' C7' 1.655(6) . ? S1' O1' 1.818(6) . ? S1' C6' 1.842(3) . ? S2' O2' 1.361(8) . ? S2' C10' 1.673(6) . ? S2' C11' 1.839(4) . ? S2' C16' 2.236(4) . ? C1' C2' 1.365(3) . ? C1' C6' 1.365(3) . ? C2' C3' 1.365(4) . ? C3' C4' 1.365(3) . ? C4' C5' 1.370(3) . ? C5' C6' 1.366(4) . ? C7' C8' 1.193(4) . ? C8' C9' 1.199(4) . ? C9' C10' 1.210(4) . ? C11' C16' 1.363(3) . ? C11' C12' 1.363(4) . ? C12' C13' 1.365(3) . ? C13' C14' 1.362(4) . ? C14' C15' 1.364(4) . ? C15' C16' 1.363(3) . ? Cl1 O11 1.403(4) 2_765 ? Cl1 O11 1.403(4) . ? Cl1 O13' 1.415(4) . ? Cl1 O13' 1.415(4) 2_765 ? Cl1 O12' 1.426(3) . ? Cl1 O12' 1.426(3) 2_765 ? Cl1 O14' 1.428(4) . ? Cl1 O14' 1.428(4) 2_765 ? Cl1 O11' 1.432(4) 2_765 ? Cl1 O11' 1.432(4) . ? Cl1 O13 1.433(4) . ? Cl1 O13 1.433(4) 2_765 ? O11 O11 0.908(12) 2_765 ? O12 O13 1.388(9) 2_765 ? O12 O14 1.636(7) 2_765 ? O13 O14 1.322(9) 2_765 ? O13 O12 1.388(9) 2_765 ? O14 O13 1.322(9) 2_765 ? O14 O12 1.636(7) 2_765 ? O11' O14' 0.833(10) 2_765 ? O11' O12' 1.815(8) 2_765 ? O12' O13' 1.221(8) 2_765 ? O12' O11' 1.815(8) 2_765 ? O13' O12' 1.221(8) 2_765 ? O13' O13' 1.410(11) 2_765 ? O14' O11' 0.833(10) 2_765 ? Cl2 O21 1.413(4) 3_657 ? Cl2 O21 1.413(4) . ? Cl2 O21 1.413(4) 2_665 ? Cl2 O21 1.413(4) 4_567 ? Cl2 O24 1.420(4) 2_665 ? Cl2 O24 1.420(4) . ? Cl2 O24 1.420(4) 4_567 ? Cl2 O24 1.420(4) 3_657 ? Cl2 O22 1.421(4) 4_567 ? Cl2 O22 1.421(4) . ? Cl2 O22 1.421(4) 3_657 ? Cl2 O22 1.421(4) 2_665 ? O21 O22 1.106(11) 4_567 ? O21 O24 1.124(11) 3_657 ? O21 O24 1.324(10) 2_665 ? O21 O22 1.342(10) 2_665 ? O21 O23 1.672(6) 3_657 ? O23 O21 1.672(6) 3_657 ? O23 O21 1.672(6) 4_567 ? O23 O24 1.708(6) 4_567 ? O23 O24 1.708(6) 3_657 ? O23 O22 1.718(6) 4_567 ? O23 O22 1.718(6) 3_657 ? O22 O24 1.046(10) 4_567 ? O22 O21 1.106(11) 3_657 ? O22 O21 1.342(10) 2_665 ? O22 O24 1.400(8) 2_665 ? O22 O23 1.718(6) 3_657 ? O24 O22 1.046(10) 3_657 ? O24 O21 1.124(11) 4_567 ? O24 O21 1.324(10) 2_665 ? O24 O22 1.400(8) 2_665 ? O24 O23 1.708(6) 3_657 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O2 106.48(16) . 3_656 ? O2 Gd1 O2 106.48(17) . 4_566 ? O2 Gd1 O2 115.6(3) 3_656 4_566 ? O2 Gd1 O2 115.6(3) . 2_665 ? O2 Gd1 O2 106.48(16) 3_656 2_665 ? O2 Gd1 O2 106.48(16) 4_566 2_665 ? O2 Gd1 O2' 50.9(3) . . ? O2 Gd1 O2' 156.3(3) 3_656 . ? O2 Gd1 O2' 71.5(3) 4_566 . ? O2 Gd1 O2' 91.9(3) 2_665 . ? O2 Gd1 O2' 91.9(3) . 2_665 ? O2 Gd1 O2' 71.5(3) 3_656 2_665 ? O2 Gd1 O2' 156.3(3) 4_566 2_665 ? O2 Gd1 O2' 50.9(3) 2_665 2_665 ? O2' Gd1 O2' 111.6(4) . 2_665 ? O2 Gd1 O2' 71.5(3) . 3_656 ? O2 Gd1 O2' 50.9(3) 3_656 3_656 ? O2 Gd1 O2' 91.9(3) 4_566 3_656 ? O2 Gd1 O2' 156.3(3) 2_665 3_656 ? O2' Gd1 O2' 108.42(18) . 3_656 ? O2' Gd1 O2' 108.42(18) 2_665 3_656 ? O2 Gd1 O2' 156.3(3) . 4_566 ? O2 Gd1 O2' 91.9(3) 3_656 4_566 ? O2 Gd1 O2' 50.9(3) 4_566 4_566 ? O2 Gd1 O2' 71.5(3) 2_665 4_566 ? O2' Gd1 O2' 108.42(18) . 4_566 ? O2' Gd1 O2' 108.42(18) 2_665 4_566 ? O2' Gd1 O2' 111.6(4) 3_656 4_566 ? O2 Gd1 O1 93.3(3) . 4_566 ? O2 Gd1 O1 155.8(3) 3_656 4_566 ? O2 Gd1 O1 70.1(2) 4_566 4_566 ? O2 Gd1 O1 51.0(3) 2_665 4_566 ? O2' Gd1 O1 47.0(2) . 4_566 ? O2' Gd1 O1 94.5(2) 2_665 4_566 ? O2' Gd1 O1 152.5(2) 3_656 4_566 ? O2' Gd1 O1 73.5(2) 4_566 4_566 ? O2 Gd1 O1 51.0(3) . 3_656 ? O2 Gd1 O1 70.1(2) 3_656 3_656 ? O2 Gd1 O1 155.8(3) 4_566 3_656 ? O2 Gd1 O1 93.3(3) 2_665 3_656 ? O2' Gd1 O1 94.5(2) . 3_656 ? O2' Gd1 O1 47.0(2) 2_665 3_656 ? O2' Gd1 O1 73.5(2) 3_656 3_656 ? O2' Gd1 O1 152.5(2) 4_566 3_656 ? O1 Gd1 O1 115.1(3) 4_566 3_656 ? O2 Gd1 O1 70.1(2) . . ? O2 Gd1 O1 93.3(3) 3_656 . ? O2 Gd1 O1 51.0(3) 4_566 . ? O2 Gd1 O1 155.8(3) 2_665 . ? O2' Gd1 O1 73.5(2) . . ? O2' Gd1 O1 152.5(2) 2_665 . ? O2' Gd1 O1 47.0(2) 3_656 . ? O2' Gd1 O1 94.5(2) 4_566 . ? O1 Gd1 O1 106.75(14) 4_566 . ? O1 Gd1 O1 106.75(13) 3_656 . ? O2 Gd1 O1 155.8(3) . 2_665 ? O2 Gd1 O1 51.0(3) 3_656 2_665 ? O2 Gd1 O1 93.3(3) 4_566 2_665 ? O2 Gd1 O1 70.1(2) 2_665 2_665 ? O2' Gd1 O1 152.5(2) . 2_665 ? O2' Gd1 O1 73.5(2) 2_665 2_665 ? O2' Gd1 O1 94.5(2) 3_656 2_665 ? O2' Gd1 O1 47.0(2) 4_566 2_665 ? O1 Gd1 O1 106.75(13) 4_566 2_665 ? O1 Gd1 O1 106.75(14) 3_656 2_665 ? O1 Gd1 O1 115.1(3) . 2_665 ? O1 S1 C7 132.3(4) . . ? O1 S1 C6 106.5(3) . . ? C7 S1 C6 108.06(18) . . ? O2 S2 C10 101.4(4) . . ? O2 S2 C11 108.6(3) . . ? C10 S2 C11 78.95(13) . . ? S1 O1 Gd1 162.9(4) . . ? S2 O2 Gd1 138.5(5) . . ? C6 C1 C2 108.8(2) . . ? C1 C2 C3 130.4(2) . . ? C4 C3 C2 109.0(2) . . ? C3 C4 C5 130.3(3) . . ? C6 C5 C4 108.3(2) . . ? C1 C6 C5 129.1(3) . . ? C1 C6 S1 119.6(2) . . ? C5 C6 S1 107.54(18) . . ? C8 C7 S1 115.8(4) . . ? C7 C8 C9 148.3(4) . . ? C8 C9 C10 144.5(3) . . ? C9 C10 S2 115.4(2) . . ? C12 C11 C16 112.71(17) . . ? C12 C11 S2 114.32(15) . . ? C16 C11 S2 132.30(17) . . ? C11 C12 C13 124.70(16) . . ? C14 C13 C12 114.24(18) . . ? C13 C14 C15 123.48(19) . . ? C14 C15 C16 113.8(2) . . ? C15 C16 C11 125.2(2) . . ? C7' S1' O1' 102.1(3) . . ? C7' S1' C6' 96.52(19) . . ? O1' S1' C6' 95.8(2) . . ? O2' S2' C10' 107.2(4) . . ? O2' S2' C11' 130.3(4) . . ? C10' S2' C11' 114.4(3) . . ? O2' S2' C16' 102.2(4) . . ? C10' S2' C16' 112.1(2) . . ? C11' S2' C16' 37.51(12) . . ? S1' O1' Gd1 115.5(3) . . ? S2' O2' Gd1 152.0(5) . . ? C2' C1' C6' 122.8(3) . . ? C3' C2' C1' 116.1(2) . . ? C4' C3' C2' 123.3(2) . . ? C3' C4' C5' 116.2(2) . . ? C6' C5' C4' 122.4(3) . . ? C1' C6' C5' 116.7(2) . . ? C1' C6' S1' 138.1(2) . . ? C5' C6' S1' 105.17(19) . . ? C8' C7' S1' 116.4(4) . . ? C7' C8' C9' 153.9(6) . . ? C8' C9' C10' 140.1(5) . . ? C9' C10' S2' 111.6(4) . . ? C16' C11' C12' 121.2(2) . . ? C16' C11' S2' 87.2(2) . . ? C12' C11' S2' 151.3(2) . . ? C11' C12' C13' 118.4(2) . . ? C14' C13' C12' 121.2(3) . . ? C13' C14' C15' 118.5(2) . . ? C16' C15' C14' 120.8(3) . . ? C11' C16' C15' 117.5(2) . . ? C11' C16' S2' 55.24(16) . . ? C15' C16' S2' 161.0(4) . . ? O11 Cl1 O11 37.8(5) 2_765 . ? O11 Cl1 O13' 145.2(4) 2_765 . ? O11 Cl1 O13' 145.1(4) . . ? O11 Cl1 O13' 145.1(4) 2_765 2_765 ? O11 Cl1 O13' 145.2(4) . 2_765 ? O13' Cl1 O13' 59.8(4) . 2_765 ? O11 Cl1 O12' 95.3(5) 2_765 . ? O11 Cl1 O12' 103.9(5) . . ? O13' Cl1 O12' 109.0(4) . . ? O13' Cl1 O12' 50.9(4) 2_765 . ? O11 Cl1 O12' 103.9(5) 2_765 2_765 ? O11 Cl1 O12' 95.3(5) . 2_765 ? O13' Cl1 O12' 50.9(4) . 2_765 ? O13' Cl1 O12' 109.0(4) 2_765 2_765 ? O12' Cl1 O12' 159.7(6) . 2_765 ? O11 Cl1 O14' 35.0(3) 2_765 . ? O11 Cl1 O14' 66.6(3) . . ? O13' Cl1 O14' 111.0(4) . . ? O13' Cl1 O14' 139.2(4) 2_765 . ? O12' Cl1 O14' 110.5(4) . . ? O12' Cl1 O14' 82.9(4) 2_765 . ? O11 Cl1 O14' 66.6(3) 2_765 2_765 ? O11 Cl1 O14' 35.0(3) . 2_765 ? O13' Cl1 O14' 139.2(4) . 2_765 ? O13' Cl1 O14' 111.0(4) 2_765 2_765 ? O12' Cl1 O14' 82.9(4) . 2_765 ? O12' Cl1 O14' 110.5(4) 2_765 2_765 ? O14' Cl1 O14' 100.0(4) . 2_765 ? O11 Cl1 O11' 47.4(3) 2_765 2_765 ? O11 Cl1 O11' 85.1(4) . 2_765 ? O13' Cl1 O11' 112.3(4) . 2_765 ? O13' Cl1 O11' 108.6(4) 2_765 2_765 ? O12' Cl1 O11' 78.8(4) . 2_765 ? O12' Cl1 O11' 109.6(4) 2_765 2_765 ? O14' Cl1 O11' 33.9(4) . 2_765 ? O14' Cl1 O11' 108.2(3) 2_765 2_765 ? O11 Cl1 O11' 85.1(4) 2_765 . ? O11 Cl1 O11' 47.4(3) . . ? O13' Cl1 O11' 108.6(4) . . ? O13' Cl1 O11' 112.3(4) 2_765 . ? O12' Cl1 O11' 109.6(4) . . ? O12' Cl1 O11' 78.8(4) 2_765 . ? O14' Cl1 O11' 108.2(3) . . ? O14' Cl1 O11' 33.9(4) 2_765 . ? O11' Cl1 O11' 132.5(5) 2_765 . ? O11 Cl1 O13 150.5(3) 2_765 . ? O11 Cl1 O13 113.6(3) . . ? O13' Cl1 O13 59.2(4) . . ? O13' Cl1 O13 49.4(4) 2_765 . ? O12' Cl1 O13 85.0(4) . . ? O12' Cl1 O13 81.4(4) 2_765 . ? O14' Cl1 O13 164.3(5) . . ? O14' Cl1 O13 84.3(3) 2_765 . ? O11' Cl1 O13 157.9(4) 2_765 . ? O11' Cl1 O13 67.3(3) . . ? O11 Cl1 O13 113.6(3) 2_765 2_765 ? O11 Cl1 O13 150.5(3) . 2_765 ? O13' Cl1 O13 49.4(4) . 2_765 ? O13' Cl1 O13 59.2(4) 2_765 2_765 ? O12' Cl1 O13 81.4(4) . 2_765 ? O12' Cl1 O13 85.0(4) 2_765 2_765 ? O14' Cl1 O13 84.3(3) . 2_765 ? O14' Cl1 O13 164.3(5) 2_765 2_765 ? O11' Cl1 O13 67.3(3) 2_765 2_765 ? O11' Cl1 O13 157.9(4) . 2_765 ? O13 Cl1 O13 95.7(4) . 2_765 ? O11 O11 Cl1 71.1(2) 2_765 . ? O13 O12 Cl1 61.0(3) 2_765 . ? O13 O12 O14 98.4(4) 2_765 2_765 ? Cl1 O12 O14 55.5(2) . 2_765 ? O14 O13 O12 115.8(5) 2_765 2_765 ? O14 O13 Cl1 62.9(3) 2_765 . ? O12 O13 Cl1 61.1(3) 2_765 . ? O13 O14 Cl1 62.3(3) 2_765 . ? O13 O14 O12 102.4(4) 2_765 2_765 ? Cl1 O14 O12 55.1(2) . 2_765 ? O14' O11' Cl1 72.8(4) 2_765 . ? O14' O11' O12' 120.1(5) 2_765 2_765 ? Cl1 O11' O12' 50.5(2) . 2_765 ? O13' O12' Cl1 64.0(3) 2_765 . ? O13' O12' O11' 97.2(5) 2_765 2_765 ? Cl1 O12' O11' 50.7(3) . 2_765 ? O12' O13' O13' 122.8(4) 2_765 2_765 ? O12' O13' Cl1 65.0(3) 2_765 . ? O13' O13' Cl1 60.1(2) 2_765 . ? O11' O14' Cl1 73.3(4) 2_765 . ? O21 Cl2 O21 95.70(18) 3_657 . ? O21 Cl2 O21 95.70(18) 3_657 2_665 ? O21 Cl2 O21 143.3(6) . 2_665 ? O21 Cl2 O21 143.3(6) 3_657 4_567 ? O21 Cl2 O21 95.70(18) . 4_567 ? O21 Cl2 O21 95.70(18) 2_665 4_567 ? O21 Cl2 O24 46.7(4) 3_657 2_665 ? O21 Cl2 O24 55.7(5) . 2_665 ? O21 Cl2 O24 112.4(5) 2_665 2_665 ? O21 Cl2 O24 150.2(5) 4_567 2_665 ? O21 Cl2 O24 150.2(5) 3_657 . ? O21 Cl2 O24 112.4(5) . . ? O21 Cl2 O24 55.7(5) 2_665 . ? O21 Cl2 O24 46.7(4) 4_567 . ? O24 Cl2 O24 146.4(6) 2_665 . ? O21 Cl2 O24 55.7(5) 3_657 4_567 ? O21 Cl2 O24 150.2(5) . 4_567 ? O21 Cl2 O24 46.7(4) 2_665 4_567 ? O21 Cl2 O24 112.4(5) 4_567 4_567 ? O24 Cl2 O24 94.79(17) 2_665 4_567 ? O24 Cl2 O24 94.79(17) . 4_567 ? O21 Cl2 O24 112.4(5) 3_657 3_657 ? O21 Cl2 O24 46.7(4) . 3_657 ? O21 Cl2 O24 150.2(5) 2_665 3_657 ? O21 Cl2 O24 55.7(5) 4_567 3_657 ? O24 Cl2 O24 94.79(18) 2_665 3_657 ? O24 Cl2 O24 94.79(17) . 3_657 ? O24 Cl2 O24 146.4(6) 4_567 3_657 ? O21 Cl2 O22 56.5(4) 3_657 4_567 ? O21 Cl2 O22 45.9(4) . 4_567 ? O21 Cl2 O22 150.8(4) 2_665 4_567 ? O21 Cl2 O22 112.0(4) 4_567 4_567 ? O24 Cl2 O22 43.2(4) 2_665 4_567 ? O24 Cl2 O22 153.0(3) . 4_567 ? O24 Cl2 O22 110.6(3) 4_567 4_567 ? O24 Cl2 O22 59.0(3) 3_657 4_567 ? O21 Cl2 O22 45.9(4) 3_657 . ? O21 Cl2 O22 112.0(4) . . ? O21 Cl2 O22 56.5(4) 2_665 . ? O21 Cl2 O22 150.8(4) 4_567 . ? O24 Cl2 O22 59.0(3) 2_665 . ? O24 Cl2 O22 110.6(3) . . ? O24 Cl2 O22 43.2(4) 4_567 . ? O24 Cl2 O22 153.0(3) 3_657 . ? O22 Cl2 O22 94.54(17) 4_567 . ? O21 Cl2 O22 112.0(4) 3_657 3_657 ? O21 Cl2 O22 150.8(4) . 3_657 ? O21 Cl2 O22 45.9(4) 2_665 3_657 ? O21 Cl2 O22 56.5(4) 4_567 3_657 ? O24 Cl2 O22 153.0(3) 2_665 3_657 ? O24 Cl2 O22 43.2(4) . 3_657 ? O24 Cl2 O22 59.0(3) 4_567 3_657 ? O24 Cl2 O22 110.6(3) 3_657 3_657 ? O22 Cl2 O22 147.3(6) 4_567 3_657 ? O22 Cl2 O22 94.54(17) . 3_657 ? O21 Cl2 O22 150.8(4) 3_657 2_665 ? O21 Cl2 O22 56.5(4) . 2_665 ? O21 Cl2 O22 112.0(4) 2_665 2_665 ? O21 Cl2 O22 45.9(4) 4_567 2_665 ? O24 Cl2 O22 110.6(3) 2_665 2_665 ? O24 Cl2 O22 59.0(3) . 2_665 ? O24 Cl2 O22 153.0(3) 4_567 2_665 ? O24 Cl2 O22 43.2(4) 3_657 2_665 ? O22 Cl2 O22 94.54(17) 4_567 2_665 ? O22 Cl2 O22 147.3(6) . 2_665 ? O22 Cl2 O22 94.54(17) 3_657 2_665 ? O22 O21 O24 77.8(7) 4_567 3_657 ? O22 O21 O24 50.0(6) 4_567 2_665 ? O24 O21 O24 117.1(6) 3_657 2_665 ? O22 O21 O22 116.8(6) 4_567 2_665 ? O24 O21 O22 49.3(6) 3_657 2_665 ? O24 O21 O22 122.4(4) 2_665 2_665 ? O22 O21 Cl2 67.4(3) 4_567 . ? O24 O21 Cl2 67.0(4) 3_657 . ? O24 O21 Cl2 62.4(3) 2_665 . ? O22 O21 Cl2 62.1(3) 2_665 . ? O22 O21 O23 109.6(4) 4_567 3_657 ? O24 O21 O23 109.1(5) 3_657 3_657 ? O24 O21 O23 68.4(4) 2_665 3_657 ? O22 O21 O23 68.5(4) 2_665 3_657 ? Cl2 O21 O23 55.05(17) . 3_657 ? Cl2 O23 O21 53.3(2) . 3_657 ? Cl2 O23 O21 53.3(2) . 4_567 ? O21 O23 O21 106.6(5) 3_657 4_567 ? Cl2 O23 O24 52.8(2) . 4_567 ? O21 O23 O24 46.1(4) 3_657 4_567 ? O21 O23 O24 88.3(4) 4_567 4_567 ? Cl2 O23 O24 52.8(2) . 3_657 ? O21 O23 O24 88.3(4) 3_657 3_657 ? O21 O23 O24 46.1(4) 4_567 3_657 ? O24 O23 O24 105.5(5) 4_567 3_657 ? Cl2 O23 O22 52.6(2) . 4_567 ? O21 O23 O22 46.6(4) 3_657 4_567 ? O21 O23 O22 87.8(4) 4_567 4_567 ? O24 O23 O22 86.0(3) 4_567 4_567 ? O24 O23 O22 48.2(3) 3_657 4_567 ? Cl2 O23 O22 52.6(2) . 3_657 ? O21 O23 O22 87.8(4) 3_657 3_657 ? O21 O23 O22 46.6(4) 4_567 3_657 ? O24 O23 O22 48.2(3) 4_567 3_657 ? O24 O23 O22 86.0(3) 3_657 3_657 ? O22 O23 O22 105.1(5) 4_567 3_657 ? O24 O22 O21 75.9(7) 4_567 3_657 ? O24 O22 O21 54.5(5) 4_567 2_665 ? O21 O22 O21 117.4(6) 3_657 2_665 ? O24 O22 O24 116.7(6) 4_567 2_665 ? O21 O22 O24 51.7(6) 3_657 2_665 ? O21 O22 O24 118.3(4) 2_665 2_665 ? O24 O22 Cl2 68.3(4) 4_567 . ? O21 O22 Cl2 66.6(4) 3_657 . ? O21 O22 Cl2 61.4(3) 2_665 . ? O24 O22 Cl2 60.4(3) 2_665 . ? O24 O22 O23 110.2(4) 4_567 3_657 ? O21 O22 O23 108.3(5) 3_657 3_657 ? O21 O22 O23 64.9(3) 2_665 3_657 ? O24 O22 O23 65.5(3) 2_665 3_657 ? Cl2 O22 O23 53.77(19) . 3_657 ? O22 O24 O21 76.3(7) 3_657 4_567 ? O22 O24 O21 54.1(5) 3_657 2_665 ? O21 O24 O21 117.4(6) 4_567 2_665 ? O22 O24 O22 116.4(6) 3_657 2_665 ? O21 O24 O22 50.5(6) 4_567 2_665 ? O21 O24 O22 119.1(4) 2_665 2_665 ? O22 O24 Cl2 68.4(4) 3_657 . ? O21 O24 Cl2 66.3(3) 4_567 . ? O21 O24 Cl2 61.8(3) 2_665 . ? O22 O24 Cl2 60.5(3) 2_665 . ? O22 O24 O23 110.4(4) 3_657 3_657 ? O21 O24 O23 108.0(5) 4_567 3_657 ? O21 O24 O23 65.5(4) 2_665 3_657 ? O22 O24 O23 66.2(4) 2_665 3_657 ? Cl2 O24 O23 54.03(19) . 3_657 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.252 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.124 data_Complex_1 _database_code_depnum_ccdc_archive 'CCDC 221546' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H72 Cl3 La O20 S8' _chemical_formula_weight 1662.96 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.508(2) _cell_length_b 14.508(2) _cell_length_c 17.559(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3695.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 689 _cell_measurement_theta_min 3.6435 _cell_measurement_theta_max 18.5265 _exptl_crystal_description Colorless _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.981 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7708 _exptl_absorpt_correction_T_max 0.8926 _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 _diffrn_measurement_method 'Omig and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7785 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.96 _reflns_number_total 3236 _reflns_number_gt 2574 _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^)+(0.1955P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.54(2) _refine_ls_number_reflns 3236 _refine_ls_number_parameters 459 _refine_ls_number_restraints 657 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.2432 _refine_ls_wR_factor_gt 0.2195 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 0.953 _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 La1 La 0.5000 0.5000 0.5000 0.04992(7) Uani 1 4 d S . . S1 S 0.57697(18) 0.71474(19) 0.40134(12) 0.1113(7) Uani 0.50 1 d PDU A 1 S2 S 0.5354(2) 0.7305(3) 0.59025(14) 0.1521(9) Uani 0.50 1 d PDU A 1 O1 O 0.5461(5) 0.6364(4) 0.4258(4) 0.1040(12) Uani 0.50 1 d PU A 1 O2 O 0.4749(7) 0.6355(6) 0.5711(5) 0.1456(18) Uani 0.50 1 d PU A 1 C1 C 0.5721(4) 0.64144(15) 0.25676(14) 0.1197(12) Uani 0.50 1 d PDU A 1 H1A H 0.5864 0.5823 0.2734 0.144 Uiso 0.50 1 calc PR A 1 C2 C 0.5543(4) 0.67602(16) 0.18422(12) 0.1241(14) Uani 0.50 1 d PDU A 1 H2A H 0.5552 0.6282 0.1490 0.149 Uiso 0.50 1 calc PR A 1 C3 C 0.5355(4) 0.75918(19) 0.14713(12) 0.1245(14) Uani 0.50 1 d PDU A 1 H3A H 0.5422 0.7775 0.0967 0.149 Uiso 0.50 1 calc PR A 1 C4 C 0.5034(4) 0.80538(19) 0.21144(11) 0.1206(14) Uani 0.50 1 d PDU A 1 H4A H 0.4704 0.8572 0.1963 0.145 Uiso 0.50 1 calc PR A 1 C5 C 0.5039(3) 0.80039(19) 0.29074(13) 0.1119(14) Uani 0.50 1 d PDU A 1 H5A H 0.4752 0.8363 0.3277 0.134 Uiso 0.50 1 calc PR A 1 C6 C 0.5615(3) 0.72377(16) 0.29640(11) 0.1107(12) Uani 0.50 1 d PDU A 1 C7 C 0.6814(4) 0.7727(5) 0.42017(15) 0.1197(12) Uani 0.50 1 d PDU A 1 H7A H 0.7324 0.7424 0.3945 0.144 Uiso 0.50 1 calc PR A 1 H7B H 0.6782 0.8361 0.4029 0.144 Uiso 0.50 1 calc PR A 1 C8 C 0.6930(4) 0.7691(3) 0.49859(12) 0.1353(10) Uani 0.50 1 d PDU A 1 H8A H 0.6428 0.8081 0.5158 0.162 Uiso 0.50 1 calc PR A 1 H8B H 0.7478 0.8066 0.5052 0.162 Uiso 0.50 1 calc PR A 1 C9 C 0.7011(2) 0.7078(2) 0.55913(15) 0.1418(8) Uani 0.50 1 d PDU A 1 H9A H 0.7514 0.7331 0.5890 0.170 Uiso 0.50 1 calc PR A 1 H9B H 0.7258 0.6526 0.5357 0.170 Uiso 0.50 1 calc PR A 1 C10 C 0.6400(3) 0.6737(4) 0.6143(2) 0.1418(9) Uani 0.50 1 d PDU A 1 H10A H 0.6600 0.6898 0.6653 0.170 Uiso 0.50 1 calc PR A 1 H10B H 0.6336 0.6073 0.6106 0.170 Uiso 0.50 1 calc PR A 1 C11 C 0.5437(2) 0.73418(12) 0.69648(9) 0.1439(12) Uani 0.50 1 d PDU A 1 C12 C 0.5097(3) 0.81153(13) 0.73149(8) 0.1444(14) Uani 0.50 1 d PDU A 1 H12A H 0.4897 0.8584 0.6993 0.173 Uiso 0.50 1 calc PR A 1 C13 C 0.5014(3) 0.82831(11) 0.80808(8) 0.1409(14) Uani 0.50 1 d PDU A 1 H13A H 0.4888 0.8854 0.8298 0.169 Uiso 0.50 1 calc PR A 1 C14 C 0.51441(15) 0.74799(10) 0.84778(11) 0.1425(15) Uani 0.50 1 d PDU A 1 H14A H 0.4775 0.7361 0.8899 0.171 Uiso 0.50 1 calc PR A 1 C15 C 0.58010(15) 0.68458(15) 0.82746(8) 0.1472(15) Uani 0.50 1 d PDU A 1 H15A H 0.6160 0.6509 0.8614 0.177 Uiso 0.50 1 calc PR A 1 C16 C 0.5850(3) 0.6781(2) 0.74965(8) 0.1446(12) Uani 0.50 1 d PDU A 1 H16A H 0.6206 0.6301 0.7305 0.173 Uiso 0.50 1 calc PR A 1 S1' S 0.72370(18) 0.55760(18) 0.40899(12) 0.1025(7) Uani 0.50 1 d PDU A 2 S2' S 0.6943(2) 0.59991(19) 0.61241(9) 0.1510(8) Uani 0.50 1 d PDU A 2 O1' O 0.6017(5) 0.5940(5) 0.4138(4) 0.1042(11) Uani 0.50 1 d PU A 2 O2' O 0.6095(5) 0.5878(6) 0.5773(5) 0.1389(13) Uani 0.50 1 d PU A 2 C1' C 0.68285(19) 0.6031(2) 0.24484(12) 0.1179(12) Uani 0.50 1 d PDU A 2 H1'A H 0.6475 0.6553 0.2545 0.141 Uiso 0.50 1 calc PR A 2 C2' C 0.69522(18) 0.5715(3) 0.17240(13) 0.1208(14) Uani 0.50 1 d PDU A 2 H2'A H 0.6513 0.5819 0.1348 0.145 Uiso 0.50 1 calc PR A 2 C3' C 0.77418(17) 0.5240(3) 0.15686(13) 0.1206(14) Uani 0.50 1 d PDU A 2 H3'A H 0.7875 0.5072 0.1069 0.145 Uiso 0.50 1 calc PR A 2 C4' C 0.83369(18) 0.5008(3) 0.21377(12) 0.1172(14) Uani 0.50 1 d PDU A 2 H4'A H 0.8942 0.4834 0.2036 0.141 Uiso 0.50 1 calc PR A 2 C5' C 0.80028(17) 0.5043(3) 0.28648(13) 0.1113(14) Uani 0.50 1 d PDU A 2 H5'A H 0.8295 0.4715 0.3250 0.134 Uiso 0.50 1 calc PR A 2 C6' C 0.7241(2) 0.5558(3) 0.30267(11) 0.1079(12) Uani 0.50 1 d PDU A 2 C7' C 0.7710(6) 0.6710(4) 0.41081(15) 0.1193(12) Uani 0.50 1 d PDU A 2 H7'A H 0.8303 0.6728 0.3854 0.143 Uiso 0.50 1 calc PR A 2 H7'B H 0.7298 0.7147 0.3865 0.143 Uiso 0.50 1 calc PR A 2 C8' C 0.7800(4) 0.6897(3) 0.48784(12) 0.1340(10) Uani 0.50 1 d PDU A 2 H8'A H 0.8440 0.7086 0.4916 0.161 Uiso 0.50 1 calc PR A 2 H8'B H 0.7782 0.6286 0.5102 0.161 Uiso 0.50 1 calc PR A 2 C9' C 0.7382(3) 0.7432(3) 0.54369(13) 0.1407(10) Uani 0.50 1 d PDU A 2 H9'A H 0.6859 0.7708 0.5178 0.169 Uiso 0.50 1 calc PR A 2 H9'B H 0.7813 0.7932 0.5520 0.169 Uiso 0.50 1 calc PR A 2 C10' C 0.7047(5) 0.7234(4) 0.61643(18) 0.1452(10) Uani 0.50 1 d PDU A 2 H10C H 0.6455 0.7526 0.6254 0.174 Uiso 0.50 1 calc PR A 2 H10D H 0.7478 0.7425 0.6556 0.174 Uiso 0.50 1 calc PR A 2 C11' C 0.74061(15) 0.5475(3) 0.70131(11) 0.1418(12) Uani 0.50 1 d PDU A 2 C12' C 0.81403(17) 0.5069(4) 0.73469(12) 0.1412(14) Uani 0.50 1 d PDU A 2 H12B H 0.8641 0.4853 0.7068 0.169 Uiso 0.50 1 calc PR A 2 C13' C 0.80971(16) 0.4998(4) 0.81141(12) 0.1423(14) Uani 0.50 1 d PDU A 2 H13B H 0.8616 0.4782 0.8369 0.171 Uiso 0.50 1 calc PR A 2 C14' C 0.73504(16) 0.5220(4) 0.85346(13) 0.1436(14) Uani 0.50 1 d PDU A 2 H14B H 0.7327 0.5123 0.9058 0.172 Uiso 0.50 1 calc PR A 2 C15' C 0.66385(17) 0.5594(4) 0.81437(12) 0.1438(14) Uani 0.50 1 d PDU A 2 H15B H 0.6133 0.5803 0.8420 0.173 Uiso 0.50 1 calc PR A 2 C16' C 0.66142(16) 0.5684(4) 0.73789(9) 0.1426(12) Uani 0.50 1 d PDU A 2 H16B H 0.6088 0.5877 0.7121 0.171 Uiso 0.50 1 calc PR A 2 Cl1 Cl 1.0000 0.5000 0.50091(11) 0.0924(4) Uani 1 2 d SDU . . O11 O 0.9595(4) 0.4726(5) 0.5709(2) 0.0951(12) Uani 0.216(3) 1 d PDU . 1 O12 O 1.0471(4) 0.5853(2) 0.5136(5) 0.0971(12) Uani 0.216(3) 1 d PDU . 1 O13 O 0.9344(3) 0.5096(6) 0.4409(2) 0.0972(10) Uani 0.216(3) 1 d PDU . 1 O14 O 1.0664(3) 0.4329(3) 0.4766(4) 0.0977(12) Uani 0.216(3) 1 d PDU . 1 O11' O 0.9172(2) 0.4669(4) 0.5353(3) 0.0970(12) Uani 0.284(3) 1 d PDU . 2 O12' O 0.9914(5) 0.5968(2) 0.4859(4) 0.0976(12) Uani 0.284(3) 1 d PDU . 2 O13' O 1.0145(5) 0.4570(4) 0.42944(19) 0.0969(12) Uani 0.284(3) 1 d PDU . 2 O14' O 1.0745(3) 0.4853(5) 0.5525(2) 0.0975(10) Uani 0.284(3) 1 d PDU . 2 Cl2 Cl 0.5000 0.5000 1.0000 0.2784(10) Uani 1 4 d SDU . . O21 O 0.5909(2) 0.5161(6) 1.0259(4) 0.277(2) Uiso 0.25 1 d PDU . . O23 O 0.5000 0.5000 0.91803(17) 0.277(2) Uiso 0.50 2 d SPDU . . O22 O 0.4386(3) 0.5708(3) 1.0238(4) 0.277(2) Uiso 0.25 1 d PDU . . O24 O 0.4666(5) 0.4124(2) 1.0238(4) 0.277(2) Uiso 0.25 1 d PDU . . 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 0.05208(9) 0.05208(9) 0.04562(12) 0.000 0.000 0.000 S1 0.1110(12) 0.1128(12) 0.1101(12) 0.0464(10) -0.0188(11) -0.0499(10) S2 0.1919(17) 0.1435(16) 0.1208(15) -0.0263(14) -0.0179(15) -0.0747(15) O1 0.110(2) 0.102(2) 0.100(2) 0.0557(19) -0.010(2) -0.0518(19) O2 0.189(3) 0.133(3) 0.114(3) -0.037(3) -0.013(3) -0.065(3) C1 0.110(2) 0.126(2) 0.123(2) 0.028(2) 0.001(2) -0.017(2) C2 0.113(2) 0.130(2) 0.129(2) 0.026(2) 0.003(2) -0.014(2) C3 0.117(2) 0.130(3) 0.126(3) 0.033(2) 0.000(2) -0.015(2) C4 0.114(2) 0.124(2) 0.123(2) 0.034(2) 0.002(2) -0.023(2) C5 0.103(2) 0.120(2) 0.113(2) 0.036(2) -0.002(2) -0.029(2) C6 0.105(2) 0.118(2) 0.109(2) 0.041(2) -0.013(2) -0.034(2) C7 0.122(2) 0.124(2) 0.113(2) 0.022(2) -0.022(2) -0.058(2) C8 0.1435(18) 0.1438(18) 0.1185(18) 0.0129(18) -0.0310(18) -0.0645(17) C9 0.1547(15) 0.1532(15) 0.1176(15) 0.0097(15) -0.0387(15) -0.0773(15) C10 0.1607(16) 0.1527(16) 0.1118(16) -0.0031(16) -0.0478(16) -0.0833(16) C11 0.176(2) 0.145(2) 0.111(2) -0.033(2) -0.018(2) -0.065(2) C12 0.174(3) 0.150(3) 0.109(2) -0.037(2) -0.012(2) -0.052(2) C13 0.168(3) 0.147(3) 0.107(2) -0.042(2) -0.016(2) -0.049(2) C14 0.168(3) 0.149(3) 0.111(2) -0.037(2) -0.018(2) -0.048(3) C15 0.171(3) 0.152(3) 0.119(2) -0.025(2) -0.019(3) -0.047(3) C16 0.171(2) 0.146(2) 0.116(2) -0.026(2) -0.023(2) -0.057(2) S1' 0.0860(12) 0.1187(14) 0.1030(13) 0.0139(12) 0.0176(11) -0.0340(11) S2' 0.1654(13) 0.1694(14) 0.1183(13) 0.0166(13) -0.0563(12) -0.0830(12) O1' 0.0993(19) 0.1126(19) 0.1008(19) 0.0372(18) -0.0014(18) -0.0491(18) O2' 0.151(2) 0.159(2) 0.107(2) 0.010(2) -0.056(2) -0.094(2) C1' 0.111(2) 0.124(2) 0.119(2) 0.013(2) 0.020(2) -0.015(2) C2' 0.116(2) 0.124(2) 0.123(2) 0.011(2) 0.026(2) -0.014(2) C3' 0.117(2) 0.125(2) 0.120(2) 0.004(2) 0.033(2) -0.020(2) C4' 0.114(2) 0.121(2) 0.117(2) 0.005(2) 0.036(2) -0.025(2) C5' 0.107(2) 0.116(2) 0.111(2) 0.008(2) 0.033(2) -0.025(2) C6' 0.098(2) 0.118(2) 0.108(2) 0.009(2) 0.030(2) -0.026(2) C7' 0.114(2) 0.130(2) 0.114(2) 0.011(2) -0.010(2) -0.054(2) C8' 0.1384(18) 0.1452(18) 0.1184(18) 0.0138(18) -0.0282(18) -0.0654(17) C9' 0.1497(18) 0.1526(18) 0.1197(18) 0.0098(18) -0.0342(18) -0.0742(18) C10' 0.1597(18) 0.1567(18) 0.1193(18) 0.0079(18) -0.0421(18) -0.0819(18) C11' 0.160(2) 0.157(2) 0.108(2) 0.004(2) -0.053(2) -0.075(2) C12' 0.159(2) 0.159(3) 0.105(2) 0.001(2) -0.054(2) -0.066(2) C13' 0.160(3) 0.161(3) 0.106(2) -0.005(2) -0.052(2) -0.059(2) C14' 0.161(3) 0.160(3) 0.109(2) -0.002(2) -0.044(2) -0.055(2) C15' 0.161(3) 0.158(3) 0.113(2) -0.007(2) -0.038(2) -0.053(2) C16' 0.163(2) 0.152(2) 0.113(2) -0.010(2) -0.042(2) -0.060(2) Cl1 0.0701(6) 0.1089(7) 0.0982(7) 0.000 0.000 0.0007(6) O11 0.077(2) 0.110(2) 0.098(2) 0.006(2) -0.006(2) 0.005(2) O12 0.075(2) 0.112(2) 0.104(2) -0.001(2) -0.008(2) -0.001(2) O13 0.0783(18) 0.1129(18) 0.1003(18) 0.0023(18) -0.0055(18) -0.0001(18) O14 0.079(2) 0.112(2) 0.103(2) -0.001(2) -0.002(2) 0.002(2) O11' 0.076(2) 0.112(2) 0.103(2) 0.001(2) -0.001(2) -0.002(2) O12' 0.075(2) 0.113(2) 0.105(2) 0.006(2) -0.008(2) 0.002(2) O13' 0.075(2) 0.115(2) 0.100(2) -0.004(2) -0.005(2) -0.002(2) O14' 0.0792(18) 0.1112(18) 0.1019(18) 0.0036(18) -0.0074(18) 0.0017(18) Cl2 0.2834(12) 0.2834(12) 0.2684(17) 0.000 0.000 0.000 _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 O2 2.357(9) 4_656 ? La1 O2 2.357(9) . ? La1 O2 2.357(9) 2_665 ? La1 O2 2.357(9) 3_566 ? La1 O2' 2.447(8) . ? La1 O2' 2.447(8) 2_665 ? La1 O2' 2.447(8) 4_656 ? La1 O2' 2.447(8) 3_566 ? La1 O1 2.461(6) 2_665 ? La1 O1 2.461(6) 3_566 ? La1 O1 2.461(6) . ? La1 O1 2.461(6) 4_656 ? S1 O1 1.295(7) . ? S1 C7 1.764(6) . ? S1 C6 1.861(3) . ? S2 O2 1.669(10) . ? S2 C10 1.778(5) . ? S2 C11 1.870(3) . ? C1 C6 1.391(3) . ? C1 C2 1.393(3) . ? C2 C3 1.398(3) . ? C3 C4 1.393(4) . ? C4 C5 1.394(3) . ? C5 C6 1.394(4) . ? C7 C8 1.388(3) . ? C8 C9 1.391(4) . ? C9 C10 1.404(4) . ? C11 C12 1.372(2) . ? C11 C16 1.375(3) . ? C12 C13 1.3719(19) . ? C13 C14 1.371(2) . ? C14 C15 1.372(2) . ? C15 C16 1.3712(19) . ? S1' C7' 1.782(6) . ? S1' O1' 1.849(8) . ? S1' C6' 1.867(3) . ? S2' O2' 1.387(8) . ? S2' C10' 1.799(6) . ? S2' C11' 1.862(3) . ? C1' C6' 1.364(3) . ? C1' C2' 1.364(3) . ? C2' C3' 1.364(4) . ? C3' C4' 1.363(3) . ? C4' C5' 1.367(3) . ? C5' C6' 1.365(4) . ? C7' C8' 1.386(3) . ? C8' C9' 1.390(4) . ? C9' C10' 1.396(4) . ? C11' C16' 1.351(3) . ? C11' C12' 1.351(4) . ? C12' C13' 1.352(3) . ? C13' C14' 1.350(3) . ? C14' C15' 1.354(4) . ? C15' C16' 1.350(3) . ? Cl1 O13' 1.417(4) . ? Cl1 O13' 1.417(4) 2_765 ? Cl1 O11 1.418(4) 2_765 ? Cl1 O11 1.418(4) . ? Cl1 O13 1.426(4) . ? Cl1 O13 1.426(4) 2_765 ? Cl1 O14' 1.427(4) . ? Cl1 O14' 1.427(4) 2_765 ? Cl1 O11' 1.428(4) 2_765 ? Cl1 O11' 1.428(4) . ? Cl1 O12 1.432(4) . ? Cl1 O12 1.432(4) 2_765 ? O11 O12 1.314(9) 2_765 ? O11 O11 1.419(12) 2_765 ? O12 O11 1.314(9) 2_765 ? O12 O14 1.791(7) 2_765 ? O13 O14 1.043(9) 2_765 ? O14 O13 1.043(9) 2_765 ? O14 O12 1.791(7) 2_765 ? O11' O14' 0.767(10) 2_765 ? O12' O13' 1.265(8) 2_765 ? O13' O12' 1.265(8) 2_765 ? O13' O13' 1.316(11) 2_765 ? O14' O11' 0.767(10) 2_765 ? Cl2 O21 1.415(4) 2_665 ? Cl2 O21 1.415(4) . ? Cl2 O21 1.415(4) 4_657 ? Cl2 O21 1.415(4) 3_567 ? Cl2 O22 1.422(4) 4_657 ? Cl2 O22 1.422(4) 3_567 ? Cl2 O22 1.422(4) . ? Cl2 O22 1.422(4) 2_665 ? Cl2 O24 1.423(4) 2_665 ? Cl2 O24 1.423(4) 3_567 ? Cl2 O24 1.423(4) . ? Cl2 O24 1.423(4) 4_657 ? O21 O24 1.132(10) 4_657 ? O21 O22 1.132(10) 3_567 ? O21 O22 1.331(10) 2_665 ? O21 O24 1.332(9) 2_665 ? O21 O23 1.662(6) 3_567 ? O23 O21 1.662(6) 4_657 ? O23 O21 1.662(6) 3_567 ? O23 O22 1.700(6) 3_567 ? O23 O22 1.700(6) 4_657 ? O23 O24 1.700(6) 4_657 ? O23 O24 1.700(6) 3_567 ? O22 O24 1.067(10) 3_567 ? O22 O21 1.132(10) 4_657 ? O22 O21 1.331(10) 2_665 ? O22 O24 1.397(8) 2_665 ? O22 O23 1.700(6) 3_567 ? O24 O22 1.067(10) 4_657 ? O24 O21 1.132(10) 3_567 ? O24 O21 1.332(9) 2_665 ? O24 O22 1.397(8) 2_665 ? O24 O23 1.700(6) 3_567 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O2 106.3(2) 4_656 . ? O2 La1 O2 106.3(2) 4_656 2_665 ? O2 La1 O2 116.0(4) . 2_665 ? O2 La1 O2 116.0(4) 4_656 3_566 ? O2 La1 O2 106.3(2) . 3_566 ? O2 La1 O2 106.3(2) 2_665 3_566 ? O2 La1 O2' 156.3(3) 4_656 . ? O2 La1 O2' 51.1(3) . . ? O2 La1 O2' 92.3(3) 2_665 . ? O2 La1 O2' 70.9(3) 3_566 . ? O2 La1 O2' 70.9(3) 4_656 2_665 ? O2 La1 O2' 92.3(3) . 2_665 ? O2 La1 O2' 51.1(3) 2_665 2_665 ? O2 La1 O2' 156.3(3) 3_566 2_665 ? O2' La1 O2' 112.6(4) . 2_665 ? O2 La1 O2' 51.1(3) 4_656 4_656 ? O2 La1 O2' 70.9(3) . 4_656 ? O2 La1 O2' 156.3(3) 2_665 4_656 ? O2 La1 O2' 92.3(3) 3_566 4_656 ? O2' La1 O2' 107.94(19) . 4_656 ? O2' La1 O2' 107.94(19) 2_665 4_656 ? O2 La1 O2' 92.3(3) 4_656 3_566 ? O2 La1 O2' 156.3(3) . 3_566 ? O2 La1 O2' 70.9(3) 2_665 3_566 ? O2 La1 O2' 51.1(3) 3_566 3_566 ? O2' La1 O2' 107.94(19) . 3_566 ? O2' La1 O2' 107.94(19) 2_665 3_566 ? O2' La1 O2' 112.6(4) 4_656 3_566 ? O2 La1 O1 50.9(3) 4_656 2_665 ? O2 La1 O1 155.3(3) . 2_665 ? O2 La1 O1 69.6(3) 2_665 2_665 ? O2 La1 O1 94.1(3) 3_566 2_665 ? O2' La1 O1 152.7(3) . 2_665 ? O2' La1 O1 72.5(3) 2_665 2_665 ? O2' La1 O1 95.0(2) 4_656 2_665 ? O2' La1 O1 47.6(3) 3_566 2_665 ? O2 La1 O1 155.3(3) 4_656 3_566 ? O2 La1 O1 94.1(3) . 3_566 ? O2 La1 O1 50.9(3) 2_665 3_566 ? O2 La1 O1 69.6(3) 3_566 3_566 ? O2' La1 O1 47.6(3) . 3_566 ? O2' La1 O1 95.0(2) 2_665 3_566 ? O2' La1 O1 152.7(3) 4_656 3_566 ? O2' La1 O1 72.5(3) 3_566 3_566 ? O1 La1 O1 106.25(14) 2_665 3_566 ? O2 La1 O1 94.1(3) 4_656 . ? O2 La1 O1 69.6(3) . . ? O2 La1 O1 155.3(3) 2_665 . ? O2 La1 O1 50.9(3) 3_566 . ? O2' La1 O1 72.5(3) . . ? O2' La1 O1 152.7(3) 2_665 . ? O2' La1 O1 47.6(3) 4_656 . ? O2' La1 O1 95.0(2) 3_566 . ? O1 La1 O1 116.1(3) 2_665 . ? O1 La1 O1 106.25(15) 3_566 . ? O2 La1 O1 69.6(3) 4_656 4_656 ? O2 La1 O1 50.9(3) . 4_656 ? O2 La1 O1 94.1(3) 2_665 4_656 ? O2 La1 O1 155.3(3) 3_566 4_656 ? O2' La1 O1 95.0(2) . 4_656 ? O2' La1 O1 47.6(3) 2_665 4_656 ? O2' La1 O1 72.5(3) 4_656 4_656 ? O2' La1 O1 152.7(3) 3_566 4_656 ? O1 La1 O1 106.25(15) 2_665 4_656 ? O1 La1 O1 116.1(3) 3_566 4_656 ? O1 La1 O1 106.25(14) . 4_656 ? O1 S1 C7 130.8(4) . . ? O1 S1 C6 110.4(3) . . ? C7 S1 C6 104.8(2) . . ? O2 S2 C10 96.5(4) . . ? O2 S2 C11 105.0(4) . . ? C10 S2 C11 73.78(19) . . ? S1 O1 La1 167.2(5) . . ? S2 O2 La1 135.6(6) . . ? C6 C1 C2 97.3(2) . . ? C1 C2 C3 140.6(2) . . ? C4 C3 C2 95.9(2) . . ? C3 C4 C5 141.5(3) . . ? C6 C5 C4 96.6(2) . . ? C1 C6 C5 135.7(3) . . ? C1 C6 S1 114.94(19) . . ? C5 C6 S1 101.49(18) . . ? C8 C7 S1 105.8(4) . . ? C7 C8 C9 142.4(5) . . ? C8 C9 C10 134.4(4) . . ? C9 C10 S2 102.2(3) . . ? C12 C11 C16 109.65(17) . . ? C12 C11 S2 116.54(18) . . ? C16 C11 S2 133.5(2) . . ? C11 C12 C13 128.03(18) . . ? C14 C13 C12 109.60(16) . . ? C13 C14 C15 122.2(2) . . ? C16 C15 C14 109.9(2) . . ? C15 C16 C11 127.8(3) . . ? C7' S1' O1' 96.0(4) . . ? C7' S1' C6' 91.69(18) . . ? O1' S1' C6' 93.0(3) . . ? O2' S2' C10' 102.6(5) . . ? O2' S2' C11' 129.8(4) . . ? C10' S2' C11' 110.1(2) . . ? S1' O1' La1 115.8(3) . . ? S2' O2' La1 152.6(6) . . ? C6' C1' C2' 117.8(3) . . ? C1' C2' C3' 117.8(2) . . ? C4' C3' C2' 120.7(2) . . ? C3' C4' C5' 116.8(2) . . ? C6' C5' C4' 120.2(3) . . ? C1' C6' C5' 118.4(2) . . ? C1' C6' S1' 137.4(2) . . ? C5' C6' S1' 102.60(19) . . ? C8' C7' S1' 103.6(3) . . ? C7' C8' C9' 139.2(5) . . ? C8' C9' C10' 133.1(4) . . ? C9' C10' S2' 101.4(3) . . ? C16' C11' C12' 124.2(2) . . ? C16' C11' S2' 90.00(19) . . ? C12' C11' S2' 145.7(2) . . ? C11' C12' C13' 115.4(2) . . ? C14' C13' C12' 124.3(3) . . ? C13' C14' C15' 115.5(2) . . ? C16' C15' C14' 124.3(3) . . ? C15' C16' C11' 115.4(2) . . ? O13' Cl1 O13' 55.3(4) . 2_765 ? O13' Cl1 O11 146.0(4) . 2_765 ? O13' Cl1 O11 134.8(4) 2_765 2_765 ? O13' Cl1 O11 134.8(4) . . ? O13' Cl1 O11 146.0(4) 2_765 . ? O11 Cl1 O11 60.0(5) 2_765 . ? O13' Cl1 O13 59.2(4) . . ? O13' Cl1 O13 37.3(4) 2_765 . ? O11 Cl1 O13 152.7(4) 2_765 . ? O11 Cl1 O13 113.0(3) . . ? O13' Cl1 O13 37.3(4) . 2_765 ? O13' Cl1 O13 59.2(4) 2_765 2_765 ? O11 Cl1 O13 113.0(3) 2_765 2_765 ? O11 Cl1 O13 152.7(4) . 2_765 ? O13 Cl1 O13 84.8(4) . 2_765 ? O13' Cl1 O14' 112.6(4) . . ? O13' Cl1 O14' 137.8(4) 2_765 . ? O11 Cl1 O14' 34.7(4) 2_765 . ? O11 Cl1 O14' 73.9(3) . . ? O13 Cl1 O14' 171.6(3) . . ? O13 Cl1 O14' 87.1(2) 2_765 . ? O13' Cl1 O14' 137.8(4) . 2_765 ? O13' Cl1 O14' 112.6(4) 2_765 2_765 ? O11 Cl1 O14' 73.9(3) 2_765 2_765 ? O11 Cl1 O14' 34.7(4) . 2_765 ? O13 Cl1 O14' 87.1(2) . 2_765 ? O13 Cl1 O14' 171.6(3) 2_765 2_765 ? O14' Cl1 O14' 101.1(4) . 2_765 ? O13' Cl1 O11' 113.4(4) . 2_765 ? O13' Cl1 O11' 110.5(4) 2_765 2_765 ? O11 Cl1 O11' 36.0(3) 2_765 2_765 ? O11 Cl1 O11' 94.4(3) . 2_765 ? O13 Cl1 O11' 147.2(4) . 2_765 ? O13 Cl1 O11' 77.5(3) 2_765 2_765 ? O14' Cl1 O11' 31.2(4) . 2_765 ? O14' Cl1 O11' 108.6(3) 2_765 2_765 ? O13' Cl1 O11' 110.5(4) . . ? O13' Cl1 O11' 113.4(4) 2_765 . ? O11 Cl1 O11' 94.4(3) 2_765 . ? O11 Cl1 O11' 36.0(3) . . ? O13 Cl1 O11' 77.5(3) . . ? O13 Cl1 O11' 147.2(4) 2_765 . ? O14' Cl1 O11' 108.6(3) . . ? O14' Cl1 O11' 31.2(4) 2_765 . ? O11' Cl1 O11' 130.0(5) 2_765 . ? O13' Cl1 O12 116.6(4) . . ? O13' Cl1 O12 80.1(4) 2_765 . ? O11 Cl1 O12 54.9(4) 2_765 . ? O11 Cl1 O12 107.8(4) . . ? O13 Cl1 O12 110.4(4) . . ? O13 Cl1 O12 83.2(4) 2_765 . ? O14' Cl1 O12 70.6(4) . . ? O14' Cl1 O12 97.7(4) 2_765 . ? O11' Cl1 O12 40.6(3) 2_765 . ? O11' Cl1 O12 128.9(4) . . ? O13' Cl1 O12 80.1(4) . 2_765 ? O13' Cl1 O12 116.6(4) 2_765 2_765 ? O11 Cl1 O12 107.8(4) 2_765 2_765 ? O11 Cl1 O12 54.9(4) . 2_765 ? O13 Cl1 O12 83.2(4) . 2_765 ? O13 Cl1 O12 110.4(4) 2_765 2_765 ? O14' Cl1 O12 97.7(4) . 2_765 ? O14' Cl1 O12 70.6(4) 2_765 2_765 ? O11' Cl1 O12 128.9(4) 2_765 2_765 ? O11' Cl1 O12 40.6(3) . 2_765 ? O12 Cl1 O12 162.1(7) . 2_765 ? O12 O11 Cl1 63.1(3) 2_765 . ? O12 O11 O11 114.8(5) 2_765 2_765 ? Cl1 O11 O11 60.0(2) . 2_765 ? O11 O12 Cl1 62.0(3) 2_765 . ? O11 O12 O14 96.6(4) 2_765 2_765 ? Cl1 O12 O14 51.4(2) . 2_765 ? O14 O13 Cl1 69.0(4) 2_765 . ? O13 O14 Cl1 68.2(4) 2_765 . ? O13 O14 O12 109.0(4) 2_765 2_765 ? Cl1 O14 O12 51.28(18) . 2_765 ? O14' O11' Cl1 74.4(4) 2_765 . ? O13' O12' Cl1 62.9(3) 2_765 . ? O12' O13' O13' 124.4(4) 2_765 2_765 ? O12' O13' Cl1 64.4(3) 2_765 . ? O13' O13' Cl1 62.3(2) 2_765 . ? O11' O14' Cl1 74.5(5) 2_765 . ? O21 Cl2 O21 142.5(6) 2_665 . ? O21 Cl2 O21 95.94(17) 2_665 4_657 ? O21 Cl2 O21 95.94(17) . 4_657 ? O21 Cl2 O21 95.94(17) 2_665 3_567 ? O21 Cl2 O21 95.94(17) . 3_567 ? O21 Cl2 O21 142.5(6) 4_657 3_567 ? O21 Cl2 O22 47.0(4) 2_665 4_657 ? O21 Cl2 O22 150.6(4) . 4_657 ? O21 Cl2 O22 111.7(4) 4_657 4_657 ? O21 Cl2 O22 56.0(4) 3_567 4_657 ? O21 Cl2 O22 150.6(4) 2_665 3_567 ? O21 Cl2 O22 47.0(4) . 3_567 ? O21 Cl2 O22 56.0(4) 4_657 3_567 ? O21 Cl2 O22 111.7(4) 3_567 3_567 ? O22 Cl2 O22 145.8(6) 4_657 3_567 ? O21 Cl2 O22 56.0(4) 2_665 . ? O21 Cl2 O22 111.7(4) . . ? O21 Cl2 O22 47.0(4) 4_657 . ? O21 Cl2 O22 150.6(4) 3_567 . ? O22 Cl2 O22 94.97(17) 4_657 . ? O22 Cl2 O22 94.97(17) 3_567 . ? O21 Cl2 O22 111.7(4) 2_665 2_665 ? O21 Cl2 O22 56.0(4) . 2_665 ? O21 Cl2 O22 150.6(4) 4_657 2_665 ? O21 Cl2 O22 47.0(4) 3_567 2_665 ? O22 Cl2 O22 94.97(17) 4_657 2_665 ? O22 Cl2 O22 94.97(17) 3_567 2_665 ? O22 Cl2 O22 145.8(6) . 2_665 ? O21 Cl2 O24 111.7(4) 2_665 2_665 ? O21 Cl2 O24 56.0(4) . 2_665 ? O21 Cl2 O24 47.0(4) 4_657 2_665 ? O21 Cl2 O24 150.6(4) 3_567 2_665 ? O22 Cl2 O24 153.1(3) 4_657 2_665 ? O22 Cl2 O24 44.1(4) 3_567 2_665 ? O22 Cl2 O24 58.8(3) . 2_665 ? O22 Cl2 O24 110.2(3) 2_665 2_665 ? O21 Cl2 O24 47.0(4) 2_665 3_567 ? O21 Cl2 O24 150.6(4) . 3_567 ? O21 Cl2 O24 56.0(4) 4_657 3_567 ? O21 Cl2 O24 111.7(4) 3_567 3_567 ? O22 Cl2 O24 58.8(3) 4_657 3_567 ? O22 Cl2 O24 110.2(3) 3_567 3_567 ? O22 Cl2 O24 44.1(4) . 3_567 ? O22 Cl2 O24 153.1(3) 2_665 3_567 ? O24 Cl2 O24 94.97(17) 2_665 3_567 ? O21 Cl2 O24 56.0(4) 2_665 . ? O21 Cl2 O24 111.7(4) . . ? O21 Cl2 O24 150.6(4) 4_657 . ? O21 Cl2 O24 47.0(4) 3_567 . ? O22 Cl2 O24 44.1(4) 4_657 . ? O22 Cl2 O24 153.1(3) 3_567 . ? O22 Cl2 O24 110.2(3) . . ? O22 Cl2 O24 58.8(3) 2_665 . ? O24 Cl2 O24 145.8(6) 2_665 . ? O24 Cl2 O24 94.97(17) 3_567 . ? O21 Cl2 O24 150.6(4) 2_665 4_657 ? O21 Cl2 O24 47.0(4) . 4_657 ? O21 Cl2 O24 111.7(4) 4_657 4_657 ? O21 Cl2 O24 56.0(4) 3_567 4_657 ? O22 Cl2 O24 110.2(3) 4_657 4_657 ? O22 Cl2 O24 58.8(3) 3_567 4_657 ? O22 Cl2 O24 153.1(3) . 4_657 ? O22 Cl2 O24 44.1(4) 2_665 4_657 ? O24 Cl2 O24 94.97(17) 2_665 4_657 ? O24 Cl2 O24 145.8(6) 3_567 4_657 ? O24 Cl2 O24 94.97(17) . 4_657 ? O24 O21 O22 76.2(6) 4_657 3_567 ? O24 O21 O22 50.6(6) 4_657 2_665 ? O22 O21 O22 116.4(6) 3_567 2_665 ? O24 O21 O24 116.5(6) 4_657 2_665 ? O22 O21 O24 50.5(5) 3_567 2_665 ? O22 O21 O24 122.3(4) 2_665 2_665 ? O24 O21 Cl2 66.9(3) 4_657 . ? O22 O21 Cl2 66.8(3) 3_567 . ? O22 O21 Cl2 62.3(3) 2_665 . ? O24 O21 Cl2 62.3(3) 2_665 . ? O24 O21 O23 109.5(5) 4_657 3_567 ? O22 O21 O23 109.5(4) 3_567 3_567 ? O22 O21 O23 68.2(4) 2_665 3_567 ? O24 O21 O23 68.2(4) 2_665 3_567 ? Cl2 O21 O23 55.06(16) . 3_567 ? Cl2 O23 O21 53.7(2) . 4_657 ? Cl2 O23 O21 53.7(2) . 3_567 ? O21 O23 O21 107.4(4) 4_657 3_567 ? Cl2 O23 O22 53.1(2) . 3_567 ? O21 O23 O22 46.6(3) 4_657 3_567 ? O21 O23 O22 88.6(3) 3_567 3_567 ? Cl2 O23 O22 53.1(2) . 4_657 ? O21 O23 O22 88.6(3) 4_657 4_657 ? O21 O23 O22 46.6(3) 3_567 4_657 ? O22 O23 O22 106.2(5) 3_567 4_657 ? Cl2 O23 O24 53.1(2) . 4_657 ? O21 O23 O24 88.6(4) 4_657 4_657 ? O21 O23 O24 46.7(4) 3_567 4_657 ? O22 O23 O24 48.5(3) 3_567 4_657 ? O22 O23 O24 86.7(3) 4_657 4_657 ? Cl2 O23 O24 53.1(2) . 3_567 ? O21 O23 O24 46.7(4) 4_657 3_567 ? O21 O23 O24 88.6(4) 3_567 3_567 ? O22 O23 O24 86.7(3) 3_567 3_567 ? O22 O23 O24 48.5(3) 4_657 3_567 ? O24 O23 O24 106.2(5) 4_657 3_567 ? O24 O22 O21 74.5(7) 3_567 4_657 ? O24 O22 O21 55.0(5) 3_567 2_665 ? O21 O22 O21 116.9(5) 4_657 2_665 ? O24 O22 O24 116.0(5) 3_567 2_665 ? O21 O22 O24 51.9(6) 4_657 2_665 ? O21 O22 O24 118.8(4) 2_665 2_665 ? O24 O22 Cl2 68.0(4) 3_567 . ? O21 O22 Cl2 66.1(4) 4_657 . ? O21 O22 Cl2 61.7(3) 2_665 . ? O24 O22 Cl2 60.6(2) 2_665 . ? O24 O22 O23 110.5(4) 3_567 3_567 ? O21 O22 O23 108.4(5) 4_657 3_567 ? O21 O22 O23 65.2(3) 2_665 3_567 ? O24 O22 O23 65.8(3) 2_665 3_567 ? Cl2 O22 O23 54.02(18) . 3_567 ? O22 O24 O21 74.4(7) 4_657 3_567 ? O22 O24 O21 55.0(5) 4_657 2_665 ? O21 O24 O21 116.9(6) 3_567 2_665 ? O22 O24 O22 116.0(6) 4_657 2_665 ? O21 O24 O22 51.9(6) 3_567 2_665 ? O21 O24 O22 118.7(4) 2_665 2_665 ? O22 O24 Cl2 67.9(3) 4_657 . ? O21 O24 Cl2 66.1(3) 3_567 . ? O21 O24 Cl2 61.7(3) 2_665 . ? O22 O24 Cl2 60.6(3) 2_665 . ? O22 O24 O23 110.5(4) 4_657 3_567 ? O21 O24 O23 108.4(5) 3_567 3_567 ? O21 O24 O23 65.2(4) 2_665 3_567 ? O22 O24 O23 65.7(4) 2_665 3_567 ? Cl2 O24 O23 54.00(18) . 3_567 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.023 _refine_diff_density_min -1.181 _refine_diff_density_rms 0.132 #===END data_Complex_5 _database_code_depnum_ccdc_archive 'CCDC 221547' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H72 Cl3 O20 S8 Yb' _chemical_formula_weight 1697.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.426(2) _cell_length_b 14.426(2) _cell_length_c 17.487(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3639.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1002 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.98 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1730 _exptl_absorpt_coefficient_mu 1.694 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7104 _exptl_absorpt_correction_T_max 0.9643 _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 _diffrn_measurement_method 'Omig and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9250 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3195 _reflns_number_gt 3188 _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^)+(0.1625P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(3) _refine_ls_number_reflns 3195 _refine_ls_number_parameters 459 _refine_ls_number_restraints 643 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1647 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.5000 0.5000 0.5000 0.0532(2) Uani 1 4 d S . . S1 S 0.5696(5) 0.7139(4) 0.4073(4) 0.0860(15) Uani 0.50 1 d PDU A 1 S2 S 0.5122(11) 0.7316(7) 0.5887(6) 0.137(3) Uani 0.50 1 d PDU A 1 O1 O 0.5400(18) 0.6298(14) 0.4264(13) 0.097(3) Uani 0.50 1 d PU A 1 O2 O 0.474(2) 0.6340(16) 0.5719(12) 0.118(4) Uani 0.50 1 d PU A 1 C1 C 0.575(2) 0.6525(17) 0.2548(14) 0.102(4) Uani 0.50 1 d PDU A 1 H1A H 0.5997 0.5967 0.2720 0.122 Uiso 0.50 1 calc PR A 1 C2 C 0.556(2) 0.6652(19) 0.1794(15) 0.107(5) Uani 0.50 1 d PDU A 1 H2A H 0.5736 0.6203 0.1441 0.128 Uiso 0.50 1 calc PR A 1 C3 C 0.512(2) 0.743(2) 0.1550(11) 0.105(6) Uani 0.50 1 d PDU A 1 H3A H 0.4982 0.7511 0.1035 0.127 Uiso 0.50 1 calc PR A 1 C4 C 0.487(2) 0.8086(18) 0.2072(16) 0.101(6) Uani 0.50 1 d PDU A 1 H4A H 0.4585 0.8627 0.1909 0.121 Uiso 0.50 1 calc PR A 1 C5 C 0.505(2) 0.7957(16) 0.2830(17) 0.089(5) Uani 0.50 1 d PDU A 1 H5A H 0.4806 0.8363 0.3193 0.107 Uiso 0.50 1 calc PR A 1 C6 C 0.5575(17) 0.7225(15) 0.3047(8) 0.088(4) Uani 0.50 1 d PDU A 1 C7 C 0.6634(18) 0.7729(19) 0.4325(14) 0.104(4) Uani 0.50 1 d PDU A 1 H7A H 0.7150 0.7504 0.4021 0.125 Uiso 0.50 1 calc PR A 1 H7B H 0.6537 0.8374 0.4189 0.125 Uiso 0.50 1 calc PR A 1 C8 C 0.6856(19) 0.7697(18) 0.4988(14) 0.123(4) Uani 0.50 1 d PDU A 1 H8A H 0.6697 0.8318 0.5155 0.147 Uiso 0.50 1 calc PR A 1 H8B H 0.7527 0.7703 0.4946 0.147 Uiso 0.50 1 calc PR A 1 C9 C 0.6752(14) 0.727(3) 0.5571(13) 0.127(4) Uani 0.50 1 d PDU A 1 H9A H 0.7101 0.7639 0.5930 0.152 Uiso 0.50 1 calc PR A 1 H9B H 0.7142 0.6730 0.5477 0.152 Uiso 0.50 1 calc PR A 1 C10 C 0.6165(12) 0.6938(16) 0.5981(12) 0.120(3) Uani 0.50 1 d PDU A 1 H10A H 0.6353 0.7040 0.6507 0.144 Uiso 0.50 1 calc PR A 1 H10B H 0.6156 0.6273 0.5898 0.144 Uiso 0.50 1 calc PR A 1 C11 C 0.527(2) 0.744(2) 0.6911(9) 0.133(5) Uani 0.50 1 d PDU A 1 C12 C 0.508(3) 0.829(2) 0.7220(17) 0.127(6) Uani 0.50 1 d PDU A 1 H12A H 0.4986 0.8801 0.6903 0.152 Uiso 0.50 1 calc PR A 1 C13 C 0.502(3) 0.839(2) 0.7999(17) 0.124(7) Uani 0.50 1 d PDU A 1 H13A H 0.4808 0.8939 0.8215 0.149 Uiso 0.50 1 calc PR A 1 C14 C 0.528(3) 0.766(2) 0.8450(9) 0.129(7) Uani 0.50 1 d PDU A 1 H14A H 0.5087 0.7623 0.8957 0.155 Uiso 0.50 1 calc PR A 1 C15 C 0.582(3) 0.697(2) 0.8140(16) 0.135(7) Uani 0.50 1 d PDU A 1 H15A H 0.6191 0.6599 0.8446 0.162 Uiso 0.50 1 calc PR A 1 C16 C 0.580(3) 0.687(2) 0.7360(16) 0.136(6) Uani 0.50 1 d PDU A 1 H16A H 0.6151 0.6399 0.7134 0.163 Uiso 0.50 1 calc PR A 1 S1' S 0.7152(4) 0.5616(5) 0.4104(5) 0.0856(17) Uani 0.50 1 d PDU A 2 S2' S 0.6923(9) 0.5990(9) 0.6087(6) 0.130(3) Uani 0.50 1 d PDU A 2 O1' O 0.5991(15) 0.5857(17) 0.4251(15) 0.086(3) Uani 0.50 1 d PU A 2 O2' O 0.598(2) 0.602(2) 0.5848(15) 0.108(4) Uani 0.50 1 d PU A 2 C1' C 0.6713(18) 0.592(2) 0.2496(14) 0.104(4) Uani 0.50 1 d PDU A 2 H1'A H 0.6203 0.6297 0.2598 0.125 Uiso 0.50 1 calc PR A 2 C2' C 0.695(2) 0.570(2) 0.1766(15) 0.110(5) Uani 0.50 1 d PDU A 2 H2'A H 0.6578 0.5912 0.1367 0.132 Uiso 0.50 1 calc PR A 2 C3' C 0.771(2) 0.519(3) 0.1604(11) 0.111(6) Uani 0.50 1 d PDU A 2 H3'A H 0.7858 0.5028 0.1103 0.133 Uiso 0.50 1 calc PR A 2 C4' C 0.826(2) 0.492(3) 0.2194(16) 0.107(6) Uani 0.50 1 d PDU A 2 H4'A H 0.8823 0.4626 0.2090 0.128 Uiso 0.50 1 calc PR A 2 C5' C 0.8008(19) 0.506(2) 0.2934(17) 0.097(5) Uani 0.50 1 d PDU A 2 H5'A H 0.8350 0.4805 0.3335 0.116 Uiso 0.50 1 calc PR A 2 C6' C 0.7242(19) 0.558(2) 0.3072(9) 0.095(4) Uani 0.50 1 d PDU A 2 C7' C 0.7739(18) 0.6589(16) 0.4209(13) 0.102(4) Uani 0.50 1 d PDU A 2 H7'A H 0.8365 0.6477 0.4029 0.122 Uiso 0.50 1 calc PR A 2 H7'B H 0.7466 0.7045 0.3869 0.122 Uiso 0.50 1 calc PR A 2 C8' C 0.7796(17) 0.6934(18) 0.4828(13) 0.115(4) Uani 0.50 1 d PDU A 2 H8'A H 0.8298 0.7367 0.4738 0.138 Uiso 0.50 1 calc PR A 2 H8'B H 0.8084 0.6429 0.5107 0.138 Uiso 0.50 1 calc PR A 2 C9' C 0.741(2) 0.7322(15) 0.5345(14) 0.124(4) Uani 0.50 1 d PDU A 2 H9'A H 0.6857 0.7571 0.5102 0.149 Uiso 0.50 1 calc PR A 2 H9'B H 0.7801 0.7855 0.5440 0.149 Uiso 0.50 1 calc PR A 2 C10' C 0.713(3) 0.7121(14) 0.5979(13) 0.127(4) Uani 0.50 1 d PDU A 2 H10C H 0.6571 0.7465 0.6084 0.152 Uiso 0.50 1 calc PR A 2 H10D H 0.7596 0.7310 0.6351 0.152 Uiso 0.50 1 calc PR A 2 C11' C 0.734(3) 0.544(3) 0.6951(13) 0.120(5) Uani 0.50 1 d PDU A 2 C12' C 0.809(2) 0.507(3) 0.7299(19) 0.121(6) Uani 0.50 1 d PDU A 2 H12B H 0.8606 0.4895 0.7010 0.145 Uiso 0.50 1 calc PR A 2 C13' C 0.810(2) 0.496(4) 0.8069(19) 0.121(7) Uani 0.50 1 d PDU A 2 H13B H 0.8604 0.4678 0.8307 0.145 Uiso 0.50 1 calc PR A 2 C14' C 0.737(2) 0.525(3) 0.8494(12) 0.119(7) Uani 0.50 1 d PDU A 2 H14B H 0.7381 0.5192 0.9023 0.143 Uiso 0.50 1 calc PR A 2 C15' C 0.662(2) 0.562(3) 0.8144(16) 0.122(6) Uani 0.50 1 d PDU A 2 H15B H 0.6122 0.5839 0.8435 0.146 Uiso 0.50 1 calc PR A 2 C16' C 0.659(2) 0.568(3) 0.7369(17) 0.121(6) Uani 0.50 1 d PDU A 2 H16B H 0.6049 0.5886 0.7127 0.145 Uiso 0.50 1 calc PR A 2 Cl1 Cl 1.0000 0.5000 0.4984(8) 0.0900(8) Uani 1 2 d SDU . . O11 O 0.9745(17) 0.490(2) 0.5754(9) 0.093(4) Uani 0.267(11) 1 d PDU . 1 O12 O 1.039(2) 0.5893(12) 0.4827(16) 0.100(4) Uani 0.267(11) 1 d PDU . 1 O13 O 0.9233(14) 0.488(2) 0.4470(15) 0.093(3) Uani 0.267(11) 1 d PDU . 1 O14 O 1.0690(16) 0.4324(18) 0.4776(16) 0.095(4) Uani 0.267(11) 1 d PDU . 1 O11' O 0.9141(13) 0.463(2) 0.5259(17) 0.094(4) Uani 0.233(11) 1 d PDU . 2 O12' O 0.991(2) 0.5970(8) 0.4839(18) 0.094(4) Uani 0.233(11) 1 d PDU . 2 O13' O 1.024(2) 0.454(2) 0.4297(14) 0.098(4) Uani 0.233(11) 1 d PDU . 2 O14' O 1.0698(17) 0.485(3) 0.5554(17) 0.092(4) Uani 0.233(11) 1 d PDU . 2 Cl2 Cl 0.5000 0.5000 1.0000 0.269(9) Uani 1 4 d SDU . . O21 O 0.586(10) 0.53(3) 1.0256(19) 0.266(11) Uiso 0.25 1 d PDU . . O23 O 0.5000 0.5000 0.9175(6) 0.268(11) Uiso 0.50 2 d SPDU . . O22 O 0.426(17) 0.56(2) 1.0233(19) 0.267(11) Uiso 0.25 1 d PDU . . O24 O 0.48(3) 0.408(5) 1.0247(19) 0.268(11) Uiso 0.25 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.0558(3) 0.0558(3) 0.0480(3) 0.000 0.000 0.000 S1 0.072(3) 0.072(3) 0.115(4) 0.027(3) -0.012(3) -0.021(3) S2 0.193(8) 0.111(5) 0.106(5) -0.040(4) 0.006(5) -0.052(6) O1 0.094(7) 0.089(7) 0.109(7) 0.032(6) 0.010(7) -0.033(6) O2 0.166(9) 0.105(7) 0.084(7) -0.047(6) -0.004(7) -0.045(8) C1 0.086(7) 0.087(8) 0.132(9) 0.017(7) 0.002(7) -0.001(7) C2 0.090(9) 0.102(10) 0.129(10) 0.012(9) 0.007(9) -0.010(8) C3 0.094(10) 0.103(10) 0.119(11) 0.023(9) 0.001(9) -0.016(9) C4 0.090(10) 0.093(10) 0.119(11) 0.025(10) -0.006(9) -0.019(9) C5 0.077(9) 0.078(9) 0.113(10) 0.030(9) -0.008(8) -0.016(8) C6 0.076(7) 0.073(7) 0.114(8) 0.027(6) -0.007(6) -0.016(6) C7 0.111(8) 0.073(7) 0.128(8) 0.014(7) -0.021(7) -0.028(7) C8 0.137(7) 0.107(7) 0.125(7) 0.000(7) -0.020(7) -0.030(6) C9 0.145(8) 0.115(7) 0.119(7) -0.007(7) -0.017(7) -0.047(7) C10 0.150(7) 0.108(6) 0.101(6) -0.031(5) -0.027(6) -0.061(6) C11 0.170(10) 0.115(9) 0.113(9) -0.042(8) 0.013(8) -0.055(9) C12 0.154(12) 0.115(11) 0.111(11) -0.052(10) 0.017(10) -0.054(10) C13 0.143(13) 0.120(12) 0.109(12) -0.064(10) 0.011(11) -0.054(11) C14 0.144(14) 0.127(12) 0.116(12) -0.059(10) 0.009(11) -0.054(11) C15 0.153(13) 0.125(12) 0.129(12) -0.043(10) 0.009(11) -0.049(11) C16 0.163(12) 0.117(11) 0.128(11) -0.045(10) 0.017(10) -0.048(10) S1' 0.058(3) 0.086(4) 0.113(4) 0.014(3) 0.021(3) -0.004(2) S2' 0.151(6) 0.133(6) 0.106(5) 0.010(4) -0.042(4) -0.061(5) O1' 0.065(5) 0.085(6) 0.108(7) 0.017(6) 0.018(5) -0.032(5) O2' 0.142(8) 0.102(7) 0.081(6) -0.034(6) -0.032(6) -0.061(6) C1' 0.087(7) 0.092(8) 0.134(9) 0.008(8) 0.022(7) 0.002(7) C2' 0.098(9) 0.098(9) 0.134(11) 0.011(9) 0.029(9) 0.003(9) C3' 0.103(10) 0.101(10) 0.128(12) 0.005(10) 0.039(9) -0.003(9) C4' 0.095(10) 0.098(10) 0.127(12) -0.002(10) 0.035(10) 0.006(9) C5' 0.081(9) 0.092(10) 0.118(11) 0.002(9) 0.037(9) -0.003(9) C6' 0.072(6) 0.091(7) 0.121(8) 0.006(7) 0.032(6) -0.009(6) C7' 0.079(7) 0.107(8) 0.119(8) -0.004(7) -0.001(7) -0.019(7) C8' 0.111(8) 0.113(8) 0.122(8) 0.003(7) -0.019(7) -0.027(7) C9' 0.133(8) 0.115(7) 0.125(7) -0.007(7) -0.026(7) -0.045(7) C10' 0.145(7) 0.116(7) 0.119(7) -0.004(6) -0.025(6) -0.051(6) C11' 0.139(10) 0.114(9) 0.106(9) 0.006(8) -0.041(8) -0.043(8) C12' 0.140(12) 0.116(11) 0.108(11) 0.009(10) -0.035(10) -0.023(11) C13' 0.139(13) 0.118(12) 0.106(12) 0.002(11) -0.039(11) -0.010(12) C14' 0.135(13) 0.115(12) 0.106(11) -0.008(10) -0.042(10) -0.010(12) C15' 0.134(13) 0.115(12) 0.116(11) -0.010(10) -0.039(10) -0.013(11) C16' 0.136(12) 0.113(11) 0.113(10) -0.006(9) -0.045(9) -0.025(10) Cl1 0.0659(13) 0.115(2) 0.0888(19) 0.000 0.000 0.0000(13) O11 0.070(7) 0.114(7) 0.094(7) 0.008(7) -0.004(6) -0.003(7) O12 0.085(8) 0.118(8) 0.097(8) 0.017(7) 0.004(8) -0.007(8) O13 0.071(6) 0.119(6) 0.090(6) 0.004(6) -0.008(6) -0.004(6) O14 0.076(6) 0.117(7) 0.093(7) -0.011(6) 0.004(6) 0.008(7) O11' 0.069(6) 0.120(7) 0.093(7) 0.008(6) 0.001(6) -0.009(6) O12' 0.070(7) 0.118(7) 0.093(7) 0.014(6) -0.004(7) -0.002(7) O13' 0.078(7) 0.120(7) 0.094(7) -0.005(7) -0.005(6) 0.002(7) O14' 0.071(7) 0.115(7) 0.090(7) 0.004(7) -0.001(6) -0.001(7) Cl2 0.276(9) 0.276(9) 0.256(10) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1' 2.299(19) 4_656 ? Yb1 O1' 2.299(19) 2_665 ? Yb1 O1' 2.299(19) 3_566 ? Yb1 O1' 2.299(19) . ? Yb1 O2 2.34(2) 3_566 ? Yb1 O2 2.34(2) . ? Yb1 O2 2.34(2) 4_656 ? Yb1 O2 2.34(2) 2_665 ? Yb1 O1 2.344(16) 3_566 ? Yb1 O1 2.344(16) 2_665 ? Yb1 O1 2.344(16) . ? Yb1 O1 2.344(16) 4_656 ? S1 O1 1.328(18) . ? S1 C7 1.658(16) . ? S1 C6 1.807(14) . ? S2 O2 1.54(2) . ? S2 C10 1.608(5) . ? S2 C11 1.813(14) . ? C1 C6 1.358(9) . ? C1 C2 1.359(9) . ? C2 C3 1.359(9) . ? C3 C4 1.361(9) . ? C4 C5 1.362(9) . ? C5 C6 1.357(9) . ? C7 C8 1.204(5) . ? C8 C9 1.204(5) . ? C9 C10 1.206(5) . ? C11 C12 1.371(4) . ? C11 C16 1.374(8) . ? C12 C13 1.371(4) . ? C13 C14 1.371(4) . ? C14 C15 1.371(4) . ? C15 C16 1.372(4) . ? S1' C7' 1.650(16) . ? S1' O1' 1.73(2) . ? S1' C6' 1.810(14) . ? S2' O2' 1.42(4) . ? S2' C10' 1.671(17) . ? S2' C11' 1.808(14) . ? C1' C2' 1.358(9) . ? C1' C6' 1.358(9) . ? C2' C3' 1.360(9) . ? C3' C4' 1.359(9) . ? C4' C5' 1.360(9) . ? C5' C6' 1.357(9) . ? C7' C8' 1.195(8) . ? C8' C9' 1.202(8) . ? C9' C10' 1.211(8) . ? C11' C12' 1.356(8) . ? C11' C16' 1.357(8) . ? C12' C13' 1.358(8) . ? C13' C14' 1.357(8) . ? C14' C15' 1.356(8) . ? C15' C16' 1.358(8) . ? Cl1 O11 1.403(9) 2_765 ? Cl1 O11 1.403(9) . ? Cl1 O13' 1.414(9) 2_765 ? Cl1 O13' 1.414(9) . ? Cl1 O12' 1.429(9) . ? Cl1 O12' 1.429(9) 2_765 ? Cl1 O11' 1.430(9) 2_765 ? Cl1 O11' 1.430(9) . ? Cl1 O14' 1.433(9) . ? Cl1 O14' 1.433(9) 2_765 ? Cl1 O12 1.435(9) . ? Cl1 O12 1.435(9) 2_765 ? O11 O11 0.80(5) 2_765 ? O12 O13 1.39(4) 2_765 ? O12 O14 1.60(3) 2_765 ? O13 O14 1.27(4) 2_765 ? O13 O12 1.39(4) 2_765 ? O14 O13 1.27(4) 2_765 ? O14 O12 1.60(3) 2_765 ? O11' O14' 0.93(4) 2_765 ? O11' O12' 1.79(3) 2_765 ? O12' O13' 1.22(5) 2_765 ? O12' O11' 1.79(3) 2_765 ? O13' O12' 1.22(5) 2_765 ? O13' O13' 1.49(6) 2_765 ? O14' O11' 0.93(4) 2_765 ? Cl2 O21 1.416(10) . ? Cl2 O21 1.416(10) 4_657 ? Cl2 O21 1.416(10) 2_665 ? Cl2 O21 1.416(10) 3_567 ? Cl2 O24 1.417(10) 2_665 ? Cl2 O24 1.417(10) 4_657 ? Cl2 O24 1.417(10) . ? Cl2 O24 1.417(10) 3_567 ? Cl2 O22 1.424(10) 3_567 ? Cl2 O22 1.424(10) 2_665 ? Cl2 O22 1.424(10) . ? Cl2 O22 1.424(10) 4_657 ? O21 O22 1.10(5) 3_567 ? O21 O24 1.15(4) 4_657 ? O21 O24 1.31(4) 2_665 ? O21 O22 1.37(4) 2_665 ? O21 O23 1.67(3) 3_567 ? O23 O21 1.67(3) 4_657 ? O23 O21 1.67(3) 3_567 ? O23 O24 1.69(3) 4_657 ? O23 O24 1.69(3) 3_567 ? O23 O22 1.71(3) 3_567 ? O23 O22 1.71(3) 4_657 ? O22 O24 1.07(5) 3_567 ? O22 O21 1.10(5) 4_657 ? O22 O21 1.37(4) 2_665 ? O22 O24 1.38(4) 2_665 ? O22 O23 1.71(3) 3_567 ? O24 O22 1.07(5) 4_657 ? O24 O21 1.15(5) 3_567 ? O24 O21 1.31(4) 2_665 ? O24 O22 1.38(4) 2_665 ? O24 O23 1.69(3) 3_567 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1' Yb1 O1' 108.9(7) 4_656 2_665 ? O1' Yb1 O1' 110.5(13) 4_656 3_566 ? O1' Yb1 O1' 108.9(7) 2_665 3_566 ? O1' Yb1 O1' 108.9(7) 4_656 . ? O1' Yb1 O1' 110.5(13) 2_665 . ? O1' Yb1 O1' 108.9(7) 3_566 . ? O1' Yb1 O2 130.5(9) 4_656 3_566 ? O1' Yb1 O2 107.1(9) 2_665 3_566 ? O1' Yb1 O2 87.9(9) 3_566 3_566 ? O1' Yb1 O2 24.7(9) . 3_566 ? O1' Yb1 O2 24.7(9) 4_656 . ? O1' Yb1 O2 130.5(9) 2_665 . ? O1' Yb1 O2 107.1(9) 3_566 . ? O1' Yb1 O2 87.9(9) . . ? O2 Yb1 O2 106.8(6) 3_566 . ? O1' Yb1 O2 87.9(9) 4_656 4_656 ? O1' Yb1 O2 24.7(9) 2_665 4_656 ? O1' Yb1 O2 130.5(9) 3_566 4_656 ? O1' Yb1 O2 107.1(9) . 4_656 ? O2 Yb1 O2 114.9(13) 3_566 4_656 ? O2 Yb1 O2 106.8(6) . 4_656 ? O1' Yb1 O2 107.1(9) 4_656 2_665 ? O1' Yb1 O2 87.9(9) 2_665 2_665 ? O1' Yb1 O2 24.7(9) 3_566 2_665 ? O1' Yb1 O2 130.5(9) . 2_665 ? O2 Yb1 O2 106.8(6) 3_566 2_665 ? O2 Yb1 O2 114.9(13) . 2_665 ? O2 Yb1 O2 106.8(6) 4_656 2_665 ? O1' Yb1 O1 105.6(9) 4_656 3_566 ? O1' Yb1 O1 132.6(8) 2_665 3_566 ? O1' Yb1 O1 26.5(8) 3_566 3_566 ? O1' Yb1 O1 87.0(9) . 3_566 ? O2 Yb1 O1 71.0(8) 3_566 3_566 ? O2 Yb1 O1 92.2(8) . 3_566 ? O2 Yb1 O1 156.4(8) 4_656 3_566 ? O2 Yb1 O1 51.0(7) 2_665 3_566 ? O1' Yb1 O1 132.6(8) 4_656 2_665 ? O1' Yb1 O1 26.5(8) 2_665 2_665 ? O1' Yb1 O1 87.0(9) 3_566 2_665 ? O1' Yb1 O1 105.6(9) . 2_665 ? O2 Yb1 O1 92.2(8) 3_566 2_665 ? O2 Yb1 O1 156.4(8) . 2_665 ? O2 Yb1 O1 51.0(7) 4_656 2_665 ? O2 Yb1 O1 71.0(8) 2_665 2_665 ? O1 Yb1 O1 107.5(6) 3_566 2_665 ? O1' Yb1 O1 87.0(9) 4_656 . ? O1' Yb1 O1 105.6(9) 2_665 . ? O1' Yb1 O1 132.6(8) 3_566 . ? O1' Yb1 O1 26.5(8) . . ? O2 Yb1 O1 51.0(7) 3_566 . ? O2 Yb1 O1 71.0(8) . . ? O2 Yb1 O1 92.2(8) 4_656 . ? O2 Yb1 O1 156.4(8) 2_665 . ? O1 Yb1 O1 107.5(6) 3_566 . ? O1 Yb1 O1 113.4(12) 2_665 . ? O1' Yb1 O1 26.5(8) 4_656 4_656 ? O1' Yb1 O1 87.0(9) 2_665 4_656 ? O1' Yb1 O1 105.6(9) 3_566 4_656 ? O1' Yb1 O1 132.6(8) . 4_656 ? O2 Yb1 O1 156.4(8) 3_566 4_656 ? O2 Yb1 O1 51.0(7) . 4_656 ? O2 Yb1 O1 71.0(8) 4_656 4_656 ? O2 Yb1 O1 92.2(8) 2_665 4_656 ? O1 Yb1 O1 113.4(12) 3_566 4_656 ? O1 Yb1 O1 107.5(6) 2_665 4_656 ? O1 Yb1 O1 107.5(6) . 4_656 ? O1 S1 C7 131.6(15) . . ? O1 S1 C6 106.4(13) . . ? C7 S1 C6 107.9(12) . . ? O2 S2 C10 92.7(17) . . ? O2 S2 C11 108.7(16) . . ? C10 S2 C11 79.7(5) . . ? S1 O1 Yb1 161.2(16) . . ? S2 O2 Yb1 143.0(19) . . ? C6 C1 C2 119(2) . . ? C3 C2 C1 121(2) . . ? C2 C3 C4 119(2) . . ? C3 C4 C5 121(2) . . ? C6 C5 C4 119(2) . . ? C5 C6 C1 120(2) . . ? C5 C6 S1 112.6(17) . . ? C1 C6 S1 124.6(17) . . ? C8 C7 S1 117.0(16) . . ? C7 C8 C9 143(2) . . ? C8 C9 C10 143(2) . . ? C9 C10 S2 117.6(16) . . ? C12 C11 C16 115(3) . . ? C12 C11 S2 117(2) . . ? C16 C11 S2 124.9(19) . . ? C11 C12 C13 120(2) . . ? C14 C13 C12 118(2) . . ? C13 C14 C15 119(3) . . ? C14 C15 C16 118(3) . . ? C15 C16 C11 121(3) . . ? C7' S1' O1' 108.0(13) . . ? C7' S1' C6' 95.7(16) . . ? O1' S1' C6' 103.0(13) . . ? O2' S2' C10' 96.4(19) . . ? O2' S2' C11' 125(2) . . ? C10' S2' C11' 117(2) . . ? S1' O1' Yb1 125.4(13) . . ? S2' O2' Yb1 133.7(19) . . ? C2' C1' C6' 118(2) . . ? C1' C2' C3' 122(2) . . ? C4' C3' C2' 118(2) . . ? C3' C4' C5' 122(2) . . ? C6' C5' C4' 118(2) . . ? C5' C6' C1' 122(2) . . ? C5' C6' S1' 104.6(18) . . ? C1' C6' S1' 133.4(19) . . ? C8' C7' S1' 119.4(19) . . ? C7' C8' C9' 148(3) . . ? C8' C9' C10' 137(2) . . ? C9' C10' S2' 113.4(16) . . ? C12' C11' C16' 120(3) . . ? C12' C11' S2' 145(3) . . ? C16' C11' S2' 94(2) . . ? C11' C12' C13' 120(3) . . ? C14' C13' C12' 120(3) . . ? C15' C14' C13' 120(3) . . ? C14' C15' C16' 120(3) . . ? C11' C16' C15' 120(3) . . ? O11 Cl1 O11 33(2) 2_765 . ? O11 Cl1 O13' 146.1(18) 2_765 2_765 ? O11 Cl1 O13' 143.2(15) . 2_765 ? O11 Cl1 O13' 143.2(15) 2_765 . ? O11 Cl1 O13' 146.1(18) . . ? O13' Cl1 O13' 64(3) 2_765 . ? O11 Cl1 O12' 95.2(18) 2_765 . ? O11 Cl1 O12' 104.5(18) . . ? O13' Cl1 O12' 51(2) 2_765 . ? O13' Cl1 O12' 109.2(13) . . ? O11 Cl1 O12' 104.5(18) 2_765 2_765 ? O11 Cl1 O12' 95.2(18) . 2_765 ? O13' Cl1 O12' 109.2(13) 2_765 2_765 ? O13' Cl1 O12' 51(2) . 2_765 ? O12' Cl1 O12' 159(3) . 2_765 ? O11 Cl1 O11' 53.9(17) 2_765 2_765 ? O11 Cl1 O11' 86.8(14) . 2_765 ? O13' Cl1 O11' 109.1(13) 2_765 2_765 ? O13' Cl1 O11' 104.1(19) . 2_765 ? O12' Cl1 O11' 77.3(14) . 2_765 ? O12' Cl1 O11' 109.8(12) 2_765 2_765 ? O11 Cl1 O11' 86.8(14) 2_765 . ? O11 Cl1 O11' 53.9(17) . . ? O13' Cl1 O11' 104.1(19) 2_765 . ? O13' Cl1 O11' 109.1(13) . . ? O12' Cl1 O11' 109.8(12) . . ? O12' Cl1 O11' 77.3(14) 2_765 . ? O11' Cl1 O11' 141(2) 2_765 . ? O11 Cl1 O14' 33.3(14) 2_765 . ? O11 Cl1 O14' 60(2) . . ? O13' Cl1 O14' 146.4(18) 2_765 . ? O13' Cl1 O14' 110.4(13) . . ? O12' Cl1 O14' 109.5(13) . . ? O12' Cl1 O14' 85(2) 2_765 . ? O11' Cl1 O14' 37.9(17) 2_765 . ? O11' Cl1 O14' 108.7(13) . . ? O11 Cl1 O14' 60(2) 2_765 2_765 ? O11 Cl1 O14' 33.3(14) . 2_765 ? O13' Cl1 O14' 110.4(13) 2_765 2_765 ? O13' Cl1 O14' 146.4(18) . 2_765 ? O12' Cl1 O14' 85(2) . 2_765 ? O12' Cl1 O14' 109.5(13) 2_765 2_765 ? O11' Cl1 O14' 108.7(13) 2_765 2_765 ? O11' Cl1 O14' 37.9(17) . 2_765 ? O14' Cl1 O14' 92(3) . 2_765 ? O11 Cl1 O12 89.0(19) 2_765 . ? O11 Cl1 O12 112.6(13) . . ? O13' Cl1 O12 61.1(17) 2_765 . ? O13' Cl1 O12 99.0(17) . . ? O12' Cl1 O12 28.9(13) . . ? O12' Cl1 O12 143.8(14) 2_765 . ? O11' Cl1 O12 52.3(15) 2_765 . ? O11' Cl1 O12 137.7(15) . . ? O14' Cl1 O12 89.2(17) . . ? O14' Cl1 O12 106.3(16) 2_765 . ? O11 Cl1 O12 112.6(13) 2_765 2_765 ? O11 Cl1 O12 89.0(19) . 2_765 ? O13' Cl1 O12 99.0(17) 2_765 2_765 ? O13' Cl1 O12 61.1(17) . 2_765 ? O12' Cl1 O12 143.8(14) . 2_765 ? O12' Cl1 O12 28.9(13) 2_765 2_765 ? O11' Cl1 O12 137.7(15) 2_765 2_765 ? O11' Cl1 O12 52.3(16) . 2_765 ? O14' Cl1 O12 106.3(16) . 2_765 ? O14' Cl1 O12 89.2(17) 2_765 2_765 ? O12 Cl1 O12 158(2) . 2_765 ? O11 O11 Cl1 73.5(10) 2_765 . ? O13 O12 Cl1 61.1(10) 2_765 . ? O13 O12 O14 101.3(19) 2_765 2_765 ? Cl1 O12 O14 56.4(8) . 2_765 ? O14 O13 O12 120.2(16) 2_765 2_765 ? O14 O13 Cl1 64.0(10) 2_765 . ? O12 O13 Cl1 61.1(9) 2_765 . ? O13 O14 Cl1 63.6(10) 2_765 . ? O13 O14 O12 107(2) 2_765 2_765 ? Cl1 O14 O12 56.1(7) . 2_765 ? O14' O11' Cl1 71.2(13) 2_765 . ? O14' O11' O12' 115(2) 2_765 2_765 ? Cl1 O11' O12' 51.3(8) . 2_765 ? O13' O12' Cl1 63.9(13) 2_765 . ? O13' O12' O11' 99.1(17) 2_765 2_765 ? Cl1 O12' O11' 51.4(8) . 2_765 ? O12' O13' Cl1 65.2(12) 2_765 . ? O12' O13' O13' 117.0(19) 2_765 2_765 ? Cl1 O13' O13' 58.2(14) . 2_765 ? O11' O14' Cl1 70.9(11) 2_765 . ? O21 Cl2 O21 95.8(9) . 4_657 ? O21 Cl2 O21 143(3) . 2_665 ? O21 Cl2 O21 95.8(9) 4_657 2_665 ? O21 Cl2 O21 95.8(9) . 3_567 ? O21 Cl2 O21 143(3) 4_657 3_567 ? O21 Cl2 O21 95.8(9) 2_665 3_567 ? O21 Cl2 O24 55.0(18) . 2_665 ? O21 Cl2 O24 48(2) 4_657 2_665 ? O21 Cl2 O24 112.4(15) 2_665 2_665 ? O21 Cl2 O24 149.7(16) 3_567 2_665 ? O21 Cl2 O24 48(2) . 4_657 ? O21 Cl2 O24 112.4(15) 4_657 4_657 ? O21 Cl2 O24 149.7(16) 2_665 4_657 ? O21 Cl2 O24 55.0(18) 3_567 4_657 ? O24 Cl2 O24 95.3(8) 2_665 4_657 ? O21 Cl2 O24 112.4(15) . . ? O21 Cl2 O24 149.7(16) 4_657 . ? O21 Cl2 O24 55.0(18) 2_665 . ? O21 Cl2 O24 48(2) 3_567 . ? O24 Cl2 O24 145(3) 2_665 . ? O24 Cl2 O24 95.3(8) 4_657 . ? O21 Cl2 O24 149.7(16) . 3_567 ? O21 Cl2 O24 55.0(18) 4_657 3_567 ? O21 Cl2 O24 48(2) 2_665 3_567 ? O21 Cl2 O24 112.4(15) 3_567 3_567 ? O24 Cl2 O24 95.3(8) 2_665 3_567 ? O24 Cl2 O24 145(3) 4_657 3_567 ? O24 Cl2 O24 95.3(8) . 3_567 ? O21 Cl2 O22 46(2) . 3_567 ? O21 Cl2 O22 57.5(18) 4_657 3_567 ? O21 Cl2 O22 151.9(16) 2_665 3_567 ? O21 Cl2 O22 110.8(14) 3_567 3_567 ? O24 Cl2 O22 44(2) 2_665 3_567 ? O24 Cl2 O22 58.3(17) 4_657 3_567 ? O24 Cl2 O22 152.6(16) . 3_567 ? O24 Cl2 O22 110.5(14) 3_567 3_567 ? O21 Cl2 O22 57.5(18) . 2_665 ? O21 Cl2 O22 151.9(16) 4_657 2_665 ? O21 Cl2 O22 110.8(14) 2_665 2_665 ? O21 Cl2 O22 46(2) 3_567 2_665 ? O24 Cl2 O22 110.5(15) 2_665 2_665 ? O24 Cl2 O22 44(2) 4_657 2_665 ? O24 Cl2 O22 58.3(17) . 2_665 ? O24 Cl2 O22 152.6(16) 3_567 2_665 ? O22 Cl2 O22 94.7(8) 3_567 2_665 ? O21 Cl2 O22 110.8(14) . . ? O21 Cl2 O22 46(2) 4_657 . ? O21 Cl2 O22 57.5(18) 2_665 . ? O21 Cl2 O22 151.9(16) 3_567 . ? O24 Cl2 O22 58.3(17) 2_665 . ? O24 Cl2 O22 152.6(16) 4_657 . ? O24 Cl2 O22 110.5(15) . . ? O24 Cl2 O22 44(2) 3_567 . ? O22 Cl2 O22 94.7(8) 3_567 . ? O22 Cl2 O22 147(3) 2_665 . ? O21 Cl2 O22 151.9(16) . 4_657 ? O21 Cl2 O22 110.8(15) 4_657 4_657 ? O21 Cl2 O22 46(2) 2_665 4_657 ? O21 Cl2 O22 57.5(18) 3_567 4_657 ? O24 Cl2 O22 152.6(16) 2_665 4_657 ? O24 Cl2 O22 110.5(15) 4_657 4_657 ? O24 Cl2 O22 44(2) . 4_657 ? O24 Cl2 O22 58.3(17) 3_567 4_657 ? O22 Cl2 O22 147(3) 3_567 4_657 ? O22 Cl2 O22 94.7(8) 2_665 4_657 ? O22 Cl2 O22 94.7(8) . 4_657 ? O22 O21 O24 76(3) 3_567 4_657 ? O22 O21 O24 52(3) 3_567 2_665 ? O24 O21 O24 116.8(16) 4_657 2_665 ? O22 O21 O22 116.0(16) 3_567 2_665 ? O24 O21 O22 50(2) 4_657 2_665 ? O24 O21 O22 122(2) 2_665 2_665 ? O22 O21 Cl2 67.6(13) 3_567 . ? O24 O21 Cl2 66.1(12) 4_657 . ? O24 O21 Cl2 62.6(11) 2_665 . ? O22 O21 Cl2 61.5(10) 2_665 . ? O22 O21 O23 110.5(16) 3_567 3_567 ? O24 O21 O23 108.5(15) 4_657 3_567 ? O24 O21 O23 68(2) 2_665 3_567 ? O22 O21 O23 67.8(19) 2_665 3_567 ? Cl2 O21 O23 55.0(8) . 3_567 ? Cl2 O23 O21 53.5(8) . 4_657 ? Cl2 O23 O21 53.5(8) . 3_567 ? O21 O23 O21 107.0(16) 4_657 3_567 ? Cl2 O23 O24 53.2(8) . 4_657 ? O21 O23 O24 89.1(14) 4_657 4_657 ? O21 O23 O24 45.8(14) 3_567 4_657 ? Cl2 O23 O24 53.2(8) . 3_567 ? O21 O23 O24 45.8(14) 4_657 3_567 ? O21 O23 O24 89.1(14) 3_567 3_567 ? O24 O23 O24 106.3(16) 4_657 3_567 ? Cl2 O23 O22 52.8(8) . 3_567 ? O21 O23 O22 47.6(13) 4_657 3_567 ? O21 O23 O22 87.4(14) 3_567 3_567 ? O24 O23 O22 48.1(13) 4_657 3_567 ? O24 O23 O22 86.8(14) 3_567 3_567 ? Cl2 O23 O22 52.8(8) . 4_657 ? O21 O23 O22 87.4(14) 4_657 4_657 ? O21 O23 O22 47.6(13) 3_567 4_657 ? O24 O23 O22 86.8(14) 4_657 4_657 ? O24 O23 O22 48.1(13) 3_567 4_657 ? O22 O23 O22 105.7(16) 3_567 4_657 ? O24 O22 O21 74(3) 3_567 4_657 ? O24 O22 O21 55(3) 3_567 2_665 ? O21 O22 O21 116.5(15) 4_657 2_665 ? O24 O22 O24 116.2(16) 3_567 2_665 ? O21 O22 O24 54(3) 4_657 2_665 ? O21 O22 O24 118(2) 2_665 2_665 ? O24 O22 Cl2 67.4(12) 3_567 . ? O21 O22 Cl2 66.9(12) 4_657 . ? O21 O22 Cl2 61.0(10) 2_665 . ? O24 O22 Cl2 60.6(10) 2_665 . ? O24 O22 O23 109.8(15) 3_567 3_567 ? O21 O22 O23 109.3(15) 4_657 3_567 ? O21 O22 O23 64.6(19) 2_665 3_567 ? O24 O22 O23 65.0(19) 2_665 3_567 ? Cl2 O22 O23 53.8(8) . 3_567 ? O22 O24 O21 76(3) 4_657 3_567 ? O22 O24 O21 54(3) 4_657 2_665 ? O21 O24 O21 117.3(15) 3_567 2_665 ? O22 O24 O22 116.2(16) 4_657 2_665 ? O21 O24 O22 50(2) 3_567 2_665 ? O21 O24 O22 121(2) 2_665 2_665 ? O22 O24 Cl2 68.1(13) 4_657 . ? O21 O24 Cl2 66.0(12) 3_567 . ? O21 O24 Cl2 62.5(11) 2_665 . ? O22 O24 Cl2 61.1(10) 2_665 . ? O22 O24 O23 110.8(16) 4_657 3_567 ? O21 O24 O23 108.2(15) 3_567 3_567 ? O21 O24 O23 66(2) 2_665 3_567 ? O22 O24 O23 66.9(19) 2_665 3_567 ? Cl2 O24 O23 54.6(8) . 3_567 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.804 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.177