# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wuping Liao' _publ_contact_author_email WPLIAO@CIAC.JL.CN _publ_section_title ; Two MnII2LnIII4 (Ln = Gd, Eu) Hexanuclear Compounds of p-tert-butylsulfinylcalix[4]arene ; _publ_author_address ; State Key Lab of Rare Earth Resource Utilization Changchun Institute of Applied Chemistry CAS, Changchun 130022 P.R. China ; _publ_contact_author 'Prof Dr Wuping Liao' loop_ _publ_author_name 'Wuping Liao.' 'Yanfeng Bi.' 'Song Gao.' 'Deqian Li.' 'Xiu-Teng Wang.' ; Xiaofei Wqang ; 'Hongjie Zhang.' # Attachment 'compd-squeezed.cif' data_compound_1_squeeze _database_code_depnum_ccdc_archive 'CCDC 712755' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Gd4Mn2(C40H44O8S4)4(H2O)2 _chemical_melting_point ? _chemical_formula_moiety Gd4Mn2(C40H44O8S4)4(H2O)2 _chemical_formula_sum 'C160 H176 Gd4 Mn2 O34 S16' _chemical_formula_weight 3894.85 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.7575(6) _cell_length_b 19.7575(6) _cell_length_c 65.511(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25572.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 184(2) _cell_measurement_reflns_used 8608 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.44 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7880 _exptl_absorpt_coefficient_mu 1.295 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6528 _exptl_absorpt_correction_T_max 0.8294 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 184(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Apex CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 124362 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -71 _diffrn_reflns_limit_l_max 85 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.49 _reflns_number_total 14640 _reflns_number_gt 11870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (1998)' _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. In order to subtract the contribution from the disordered solvent molecules, the SQUEEZE command was used. All the non-hydrogen atoms were refined anisotropically. The sulfinyl oxygen atom (O5) was refined with two disordered sites (O5 and O5') both with the occupation factor being of 0.5 and the same displacement parameters. ; _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^)+(0.0759P)^2^+13.0252P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14640 _refine_ls_number_parameters 501 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1195 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.107 _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 -0.572616(7) -0.345273(7) 0.072636(2) 0.03645(6) Uani 1 1 d . . . Mn1 Mn -0.5000 -0.2500 0.037271(9) 0.03719(14) Uani 1 2 d S . . S1 S -0.58745(6) -0.18000(5) 0.006873(16) 0.0627(3) Uani 1 1 d . . . S2 S -0.74468(4) -0.31696(4) 0.064747(14) 0.04837(19) Uani 1 1 d . . . S3 S -0.61688(4) -0.16212(4) 0.124463(11) 0.04044(17) Uani 1 1 d . . . S4 S -0.49798(4) 0.00460(4) 0.066284(13) 0.04287(17) Uani 1 1 d . . . O1 O -0.60725(10) -0.26926(11) 0.04491(3) 0.0423(5) Uani 1 1 d . . . O2 O -0.62103(11) -0.25439(15) 0.08956(4) 0.0604(7) Uani 1 1 d . . . O3 O -0.53156(12) -0.13231(10) 0.08849(3) 0.0445(5) Uani 1 1 d . . . O4 O -0.50431(10) -0.14041(10) 0.04456(3) 0.0401(4) Uani 1 1 d . . . O5 O -0.5341(3) -0.2209(3) 0.00828(7) 0.0612(10) Uani 0.50 1 d P . . O5' O -0.5883(3) -0.1740(3) -0.01450(8) 0.0612(10) Uani 0.50 1 d P . . O6 O -0.68829(11) -0.36740(12) 0.06750(4) 0.0497(5) Uani 1 1 d . . . O7 O -0.64423(14) -0.14426(14) 0.14556(3) 0.0604(7) Uani 1 1 d . . . O8 O -0.43429(11) -0.03739(11) 0.06787(3) 0.0459(5) Uani 1 1 d . . . O9 O -0.5000 -0.2500 0.07137(4) 0.0389(6) Uani 1 2 d S . . C1 C -0.66358(17) -0.21198(17) 0.01758(5) 0.0466(7) Uani 1 1 d . . . C2 C -0.7223(2) -0.1965(2) 0.00676(6) 0.0621(10) Uani 1 1 d . . . H2A H -0.7189 -0.1706 -0.0054 0.075 Uiso 1 1 calc R . . C3 C -0.7850(2) -0.2177(2) 0.01322(7) 0.0723(12) Uani 1 1 d . . . C4 C -0.78662(19) -0.2541(2) 0.03098(7) 0.0658(11) Uani 1 1 d . . . H4A H -0.8293 -0.2694 0.0358 0.079 Uiso 1 1 calc R . . C5 C -0.72899(16) -0.27011(17) 0.04234(6) 0.0492(8) Uani 1 1 d . . . C6 C -0.74149(15) -0.25653(16) 0.08489(5) 0.0436(7) Uani 1 1 d . . . C7 C -0.80515(16) -0.23218(17) 0.09093(6) 0.0531(9) Uani 1 1 d . . . H7A H -0.8444 -0.2479 0.0840 0.064 Uiso 1 1 calc R . . C8 C -0.81255(16) -0.18568(17) 0.10672(7) 0.0554(9) Uani 1 1 d . . . C9 C -0.75461(17) -0.16636(17) 0.11682(6) 0.0512(8) Uani 1 1 d . . . H9A H -0.7582 -0.1367 0.1282 0.061 Uiso 1 1 calc R . . C10 C -0.69073(14) -0.18910(14) 0.11081(5) 0.0376(6) Uani 1 1 d . . . C11 C -0.60516(14) -0.08115(14) 0.11248(4) 0.0363(6) Uani 1 1 d . . . C12 C -0.63859(16) -0.02458(17) 0.12025(5) 0.0456(7) Uani 1 1 d . . . H12A H -0.6672 -0.0296 0.1318 0.055 Uiso 1 1 calc R . . C13 C -0.63097(17) 0.03895(16) 0.11146(6) 0.0478(7) Uani 1 1 d . . . C14 C -0.58673(16) 0.04356(16) 0.09522(6) 0.0472(7) Uani 1 1 d . . . H14A H -0.5795 0.0866 0.0891 0.057 Uiso 1 1 calc R . . C15 C -0.55213(15) -0.01231(15) 0.08733(5) 0.0400(6) Uani 1 1 d . . . C16 C -0.54365(15) -0.02495(15) 0.04470(5) 0.0407(6) Uani 1 1 d . . . C17 C -0.58112(16) 0.02741(17) 0.03542(5) 0.0479(8) Uani 1 1 d . . . H17A H -0.5804 0.0713 0.0413 0.058 Uiso 1 1 calc R . . C18 C -0.61888(16) 0.01632(18) 0.01794(6) 0.0514(8) Uani 1 1 d . . . C19 C -0.61761(17) -0.04830(18) 0.01029(5) 0.0492(8) Uani 1 1 d . . . H19A H -0.6430 -0.0578 -0.0017 0.059 Uiso 1 1 calc R . . C20 C -0.58123(16) -0.10038(16) 0.01917(5) 0.0440(7) Uani 1 1 d . . . C21 C -0.66284(15) -0.25141(16) 0.03549(5) 0.0423(7) Uani 1 1 d . . . C22 C -0.68190(14) -0.23494(16) 0.09472(5) 0.0394(6) Uani 1 1 d . . . C23 C -0.56133(15) -0.07788(14) 0.09567(4) 0.0359(6) Uani 1 1 d . . . C24 C -0.54102(14) -0.09135(15) 0.03678(5) 0.0386(6) Uani 1 1 d . . . C25 C -0.8482(3) -0.2022(4) 0.00036(11) 0.112(2) Uani 1 1 d . . . C26 C -0.88158(19) -0.1584(2) 0.11351(8) 0.0748(13) Uani 1 1 d . . . C27 C -0.6714(2) 0.09939(18) 0.11991(7) 0.0616(10) Uani 1 1 d . . . C28 C -0.65714(19) 0.0730(2) 0.00683(7) 0.0641(11) Uani 1 1 d . . . C29 C -0.8478(4) -0.1327(5) -0.00767(14) 0.167(3) Uani 1 1 d U . . H29A H -0.8922 -0.1221 -0.0135 0.250 Uiso 1 1 calc R . . H29B H -0.8131 -0.1286 -0.0183 0.250 Uiso 1 1 calc R . . H29C H -0.8378 -0.1009 0.0034 0.250 Uiso 1 1 calc R . . C30 C -0.8555(6) -0.2556(7) -0.01475(19) 0.268(6) Uani 1 1 d U . . H30D H -0.8191 -0.2518 -0.0249 0.402 Uiso 1 1 calc R . . H30E H -0.8994 -0.2511 -0.0216 0.402 Uiso 1 1 calc R . . H30F H -0.8529 -0.2997 -0.0080 0.402 Uiso 1 1 calc R . . C31 C -0.9114(3) -0.2072(5) 0.01309(15) 0.161(3) Uani 1 1 d U . . H31A H -0.9510 -0.1973 0.0046 0.242 Uiso 1 1 calc R . . H31B H -0.9090 -0.1745 0.0243 0.242 Uiso 1 1 calc R . . H31C H -0.9154 -0.2530 0.0187 0.242 Uiso 1 1 calc R . . C32 C -0.9378(2) -0.1806(4) 0.09863(14) 0.134(3) Uani 1 1 d . . . H32A H -0.9813 -0.1623 0.1032 0.202 Uiso 1 1 calc R . . H32B H -0.9401 -0.2301 0.0983 0.202 Uiso 1 1 calc R . . H32C H -0.9276 -0.1635 0.0849 0.202 Uiso 1 1 calc R . . C33 C -0.8977(3) -0.1842(3) 0.13459(12) 0.124(3) Uani 1 1 d . . . H33A H -0.8639 -0.1674 0.1443 0.186 Uiso 1 1 calc R . . H33B H -0.8971 -0.2338 0.1345 0.186 Uiso 1 1 calc R . . H33C H -0.9427 -0.1683 0.1387 0.186 Uiso 1 1 calc R . . C34 C -0.8801(2) -0.0814(2) 0.11341(9) 0.0845(15) Uani 1 1 d . . . H34A H -0.8467 -0.0654 0.1234 0.127 Uiso 1 1 calc R . . H34B H -0.9249 -0.0640 0.1170 0.127 Uiso 1 1 calc R . . H34C H -0.8676 -0.0653 0.0998 0.127 Uiso 1 1 calc R . . C35 C -0.7466(2) 0.0827(2) 0.11982(8) 0.0767(13) Uani 1 1 d . . . H35A H -0.7608 0.0713 0.1059 0.115 Uiso 1 1 calc R . . H35B H -0.7723 0.1219 0.1247 0.115 Uiso 1 1 calc R . . H35C H -0.7551 0.0440 0.1288 0.115 Uiso 1 1 calc R . . C36 C -0.6495(3) 0.1136(3) 0.14216(8) 0.0924(17) Uani 1 1 d . . . H36A H -0.6007 0.1225 0.1426 0.139 Uiso 1 1 calc R . . H36B H -0.6599 0.0742 0.1507 0.139 Uiso 1 1 calc R . . H36C H -0.6740 0.1532 0.1473 0.139 Uiso 1 1 calc R . . C37 C -0.6590(3) 0.1632(2) 0.10756(9) 0.0908(16) Uani 1 1 d . . . H37A H -0.6757 0.1567 0.0936 0.136 Uiso 1 1 calc R . . H37B H -0.6103 0.1728 0.1072 0.136 Uiso 1 1 calc R . . H37C H -0.6828 0.2013 0.1139 0.136 Uiso 1 1 calc R . . C38 C -0.6597(3) 0.1376(3) 0.01895(10) 0.114(2) Uani 1 1 d . . . H38A H -0.6856 0.1717 0.0114 0.171 Uiso 1 1 calc R . . H38B H -0.6135 0.1542 0.0212 0.171 Uiso 1 1 calc R . . H38C H -0.6815 0.1291 0.0321 0.171 Uiso 1 1 calc R . . C39 C -0.6225(3) 0.0845(3) -0.01345(10) 0.124(3) Uani 1 1 d . . . H39A H -0.6369 0.0496 -0.0232 0.185 Uiso 1 1 calc R . . H39B H -0.5733 0.0820 -0.0116 0.185 Uiso 1 1 calc R . . H39C H -0.6347 0.1293 -0.0187 0.185 Uiso 1 1 calc R . . C40 C -0.7306(2) 0.0519(3) 0.00320(11) 0.1037(19) Uani 1 1 d . . . H40A H -0.7317 0.0062 -0.0027 0.156 Uiso 1 1 calc R . . H40B H -0.7521 0.0837 -0.0063 0.156 Uiso 1 1 calc R . . H40C H -0.7551 0.0521 0.0162 0.156 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.03115(9) 0.04344(10) 0.03475(9) -0.00392(5) -0.00004(5) 0.00707(6) Mn1 0.0369(3) 0.0416(3) 0.0332(3) 0.000 0.000 0.0069(3) S1 0.0731(6) 0.0673(6) 0.0478(5) -0.0103(4) 0.0114(4) 0.0012(5) S2 0.0319(4) 0.0502(5) 0.0630(5) -0.0071(4) -0.0031(3) 0.0000(3) S3 0.0462(4) 0.0392(4) 0.0358(4) 0.0027(3) 0.0003(3) 0.0127(3) S4 0.0399(4) 0.0343(4) 0.0545(5) 0.0050(3) 0.0012(3) -0.0023(3) O1 0.0347(10) 0.0507(12) 0.0416(11) -0.0033(9) -0.0061(8) 0.0051(9) O2 0.0289(11) 0.094(2) 0.0581(15) -0.0317(13) 0.0033(10) 0.0057(11) O3 0.0566(13) 0.0316(10) 0.0453(12) 0.0017(8) 0.0131(10) 0.0091(9) O4 0.0424(11) 0.0387(11) 0.0392(11) 0.0046(8) -0.0015(9) 0.0071(9) O5 0.068(2) 0.073(2) 0.0418(19) -0.0034(16) 0.0006(16) 0.0203(19) O5' 0.068(2) 0.073(2) 0.0418(19) -0.0034(16) 0.0006(16) 0.0203(19) O6 0.0391(12) 0.0528(13) 0.0572(14) -0.0033(11) -0.0060(10) 0.0000(10) O7 0.0796(18) 0.0667(16) 0.0349(12) 0.0008(11) 0.0051(11) 0.0236(14) O8 0.0401(11) 0.0459(12) 0.0517(13) 0.0081(10) -0.0003(9) -0.0011(9) O9 0.0387(15) 0.0364(15) 0.0415(16) 0.000 0.000 0.0014(12) C1 0.0469(17) 0.0471(17) 0.0459(17) -0.0063(13) -0.0093(14) 0.0072(14) C2 0.056(2) 0.065(2) 0.065(2) -0.0014(18) -0.0221(18) 0.0129(18) C3 0.056(2) 0.076(3) 0.085(3) 0.007(2) -0.034(2) 0.008(2) C4 0.0392(18) 0.069(3) 0.089(3) -0.007(2) -0.0172(18) 0.0026(17) C5 0.0352(15) 0.0519(19) 0.061(2) -0.0075(15) -0.0111(14) 0.0080(14) C6 0.0321(14) 0.0436(16) 0.0551(19) 0.0006(14) 0.0068(13) 0.0036(12) C7 0.0290(15) 0.0478(18) 0.082(3) 0.0019(17) 0.0086(15) 0.0026(13) C8 0.0322(16) 0.0447(18) 0.089(3) 0.0036(17) 0.0170(16) 0.0074(14) C9 0.0464(18) 0.0458(18) 0.061(2) 0.0004(15) 0.0143(15) 0.0102(14) C10 0.0333(14) 0.0355(14) 0.0439(16) 0.0078(12) 0.0052(11) 0.0041(11) C11 0.0341(14) 0.0355(14) 0.0394(15) 0.0004(11) -0.0059(11) 0.0056(11) C12 0.0389(16) 0.0453(17) 0.0526(19) -0.0041(14) 0.0020(13) 0.0092(13) C13 0.0439(17) 0.0363(16) 0.063(2) -0.0090(14) 0.0004(15) 0.0064(13) C14 0.0410(16) 0.0326(15) 0.068(2) 0.0001(14) -0.0053(15) 0.0021(13) C15 0.0350(14) 0.0381(15) 0.0469(17) -0.0005(12) -0.0028(12) -0.0001(12) C16 0.0353(15) 0.0386(15) 0.0483(17) 0.0090(12) 0.0027(12) 0.0031(12) C17 0.0423(17) 0.0413(16) 0.060(2) 0.0167(14) 0.0061(14) 0.0072(13) C18 0.0403(17) 0.057(2) 0.057(2) 0.0221(16) 0.0047(14) 0.0108(15) C19 0.0434(17) 0.061(2) 0.0429(17) 0.0154(15) -0.0021(13) 0.0096(15) C20 0.0414(16) 0.0503(18) 0.0404(16) 0.0095(13) 0.0036(12) 0.0071(13) C21 0.0354(15) 0.0446(17) 0.0467(17) -0.0112(13) -0.0050(12) 0.0089(13) C22 0.0298(13) 0.0459(16) 0.0425(16) 0.0018(12) 0.0080(11) 0.0005(12) C23 0.0388(15) 0.0314(13) 0.0376(15) -0.0028(11) -0.0076(11) 0.0044(11) C24 0.0327(14) 0.0427(16) 0.0404(15) 0.0120(12) 0.0048(11) 0.0078(12) C25 0.061(3) 0.139(5) 0.137(5) 0.032(4) -0.050(3) 0.010(3) C26 0.0411(19) 0.058(2) 0.126(4) -0.002(2) 0.026(2) 0.0124(17) C27 0.056(2) 0.0409(18) 0.088(3) -0.0105(18) 0.0018(19) 0.0184(16) C28 0.052(2) 0.069(2) 0.071(3) 0.031(2) 0.0014(18) 0.0217(18) C29 0.105(5) 0.195(7) 0.200(7) 0.093(6) -0.053(5) 0.032(5) C30 0.243(8) 0.297(10) 0.263(9) -0.067(7) -0.209(7) 0.048(7) C31 0.076(4) 0.204(7) 0.203(7) 0.061(6) -0.058(4) 0.011(4) C32 0.035(2) 0.121(5) 0.248(9) -0.064(6) 0.016(3) 0.015(3) C33 0.087(4) 0.102(4) 0.183(7) 0.040(4) 0.088(4) 0.037(3) C34 0.056(2) 0.070(3) 0.128(4) -0.003(3) 0.021(3) 0.028(2) C35 0.059(2) 0.062(3) 0.110(4) -0.011(2) 0.009(2) 0.020(2) C36 0.099(4) 0.079(3) 0.099(4) -0.045(3) -0.011(3) 0.036(3) C37 0.101(4) 0.042(2) 0.130(5) 0.002(2) 0.025(3) 0.022(2) C38 0.138(5) 0.073(3) 0.131(5) 0.025(3) -0.031(4) 0.058(3) C39 0.123(5) 0.131(5) 0.116(5) 0.089(4) 0.041(4) 0.053(4) C40 0.063(3) 0.109(4) 0.139(5) 0.045(4) -0.016(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2 2.317(2) . ? Gd1 O8 2.343(2) 7_344 ? Gd1 O3 2.348(2) 7_344 ? Gd1 O6 2.351(2) . ? Gd1 O9 2.3682(2) . ? Gd1 O7 2.388(2) 12_566 ? Gd1 O4 2.402(2) 7_344 ? Gd1 O1 2.454(2) . ? Gd1 Mn1 3.3120(5) . ? Mn1 O5 2.096(5) . ? Mn1 O5 2.096(5) 7_344 ? Mn1 O1 2.210(2) . ? Mn1 O1 2.210(2) 7_344 ? Mn1 O4 2.219(2) 7_344 ? Mn1 O4 2.219(2) . ? Mn1 O9 2.234(3) . ? Mn1 Gd1 3.3122(5) 7_344 ? S1 O5 1.332(5) . ? S1 O5' 1.405(5) . ? S1 C20 1.772(4) . ? S1 C1 1.776(4) . ? S2 O6 1.506(2) . ? S2 C5 1.763(4) . ? S2 C6 1.781(3) . ? S3 O7 1.525(2) . ? S3 C10 1.793(3) . ? S3 C11 1.797(3) . ? S4 O8 1.511(2) . ? S4 C16 1.776(3) . ? S4 C15 1.777(3) . ? O1 C21 1.308(4) . ? O2 C22 1.307(3) . ? O3 C23 1.313(3) . ? O3 Gd1 2.347(2) 7_344 ? O4 C24 1.314(3) . ? O4 Gd1 2.403(2) 7_344 ? O5 O5 1.771(10) 7_344 ? O7 Gd1 2.388(2) 14_545 ? O8 Gd1 2.343(2) 7_344 ? O9 Gd1 2.3683(2) 7_344 ? C1 C2 1.393(5) . ? C1 C21 1.409(5) . ? C2 C3 1.375(6) . ? C2 H2A 0.9500 . ? C3 C4 1.369(6) . ? C3 C25 1.536(6) . ? C4 C5 1.397(5) . ? C4 H4A 0.9500 . ? C5 C21 1.430(5) . ? C6 C7 1.404(4) . ? C6 C22 1.408(4) . ? C7 C8 1.391(5) . ? C7 H7A 0.9500 . ? C8 C9 1.376(5) . ? C8 C26 1.533(5) . ? C9 C10 1.396(4) . ? C9 H9A 0.9500 . ? C10 C22 1.401(4) . ? C11 C12 1.395(4) . ? C11 C23 1.403(4) . ? C12 C13 1.389(5) . ? C12 H12A 0.9500 . ? C13 C14 1.380(5) . ? C13 C27 1.540(4) . ? C14 C15 1.397(4) . ? C14 H14A 0.9500 . ? C15 C23 1.417(4) . ? C16 C17 1.410(4) . ? C16 C24 1.412(4) . ? C17 C18 1.384(5) . ? C17 H17A 0.9500 . ? C18 C19 1.372(5) . ? C18 C28 1.535(4) . ? C19 C20 1.383(4) . ? C19 H19A 0.9500 . ? C20 C24 1.412(4) . ? C25 C30 1.453(12) . ? C25 C29 1.472(10) . ? C25 C31 1.505(10) . ? C26 C33 1.507(8) . ? C26 C34 1.520(6) . ? C26 C32 1.541(8) . ? C27 C37 1.518(6) . ? C27 C35 1.521(6) . ? C27 C36 1.547(6) . ? C28 C38 1.505(7) . ? C28 C39 1.511(6) . ? C28 C40 1.529(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30D 0.9800 . ? C30 H30E 0.9800 . ? C30 H30F 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? 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 O8 148.72(9) . 7_344 ? O2 Gd1 O3 107.25(8) . 7_344 ? O8 Gd1 O3 79.70(7) 7_344 7_344 ? O2 Gd1 O6 79.12(8) . . ? O8 Gd1 O6 81.58(8) 7_344 . ? O3 Gd1 O6 151.70(8) 7_344 . ? O2 Gd1 O9 69.57(7) . . ? O8 Gd1 O9 138.28(6) 7_344 . ? O3 Gd1 O9 68.55(6) 7_344 . ? O6 Gd1 O9 137.03(6) . . ? O2 Gd1 O7 77.48(10) . 12_566 ? O8 Gd1 O7 74.44(9) 7_344 12_566 ? O3 Gd1 O7 77.17(9) 7_344 12_566 ? O6 Gd1 O7 77.47(9) . 12_566 ? O9 Gd1 O7 121.22(9) . 12_566 ? O2 Gd1 O4 135.95(9) . 7_344 ? O8 Gd1 O4 75.20(7) 7_344 7_344 ? O3 Gd1 O4 76.21(7) 7_344 7_344 ? O6 Gd1 O4 118.92(8) . 7_344 ? O9 Gd1 O4 71.55(7) . 7_344 ? O7 Gd1 O4 142.50(9) 12_566 7_344 ? O2 Gd1 O1 76.40(9) . . ? O8 Gd1 O1 121.53(7) 7_344 . ? O3 Gd1 O1 133.42(7) 7_344 . ? O6 Gd1 O1 74.74(8) . . ? O9 Gd1 O1 69.92(7) . . ? O7 Gd1 O1 144.79(9) 12_566 . ? O4 Gd1 O1 71.45(7) 7_344 . ? O2 Gd1 Mn1 94.20(7) . . ? O8 Gd1 Mn1 116.34(6) 7_344 . ? O3 Gd1 Mn1 92.11(6) 7_344 . ? O6 Gd1 Mn1 115.26(6) . . ? O9 Gd1 Mn1 42.39(7) . . ? O7 Gd1 Mn1 163.55(6) 12_566 . ? O4 Gd1 Mn1 42.05(5) 7_344 . ? O1 Gd1 Mn1 41.86(5) . . ? O5 Mn1 O5 50.0(3) . 7_344 ? O5 Mn1 O1 86.83(16) . . ? O5 Mn1 O1 117.76(17) 7_344 . ? O5 Mn1 O1 117.76(17) . 7_344 ? O5 Mn1 O1 86.84(16) 7_344 7_344 ? O1 Mn1 O1 153.82(11) . 7_344 ? O5 Mn1 O4 118.39(16) . 7_344 ? O5 Mn1 O4 85.11(16) 7_344 7_344 ? O1 Mn1 O4 79.63(8) . 7_344 ? O1 Mn1 O4 94.73(8) 7_344 7_344 ? O5 Mn1 O4 85.11(16) . . ? O5 Mn1 O4 118.39(16) 7_344 . ? O1 Mn1 O4 94.73(8) . . ? O1 Mn1 O4 79.63(8) 7_344 . ? O4 Mn1 O4 155.13(11) 7_344 . ? O5 Mn1 O9 155.00(14) . . ? O5 Mn1 O9 155.00(14) 7_344 . ? O1 Mn1 O9 76.91(6) . . ? O1 Mn1 O9 76.91(6) 7_344 . ? O4 Mn1 O9 77.57(5) 7_344 . ? O4 Mn1 O9 77.57(5) . . ? O5 Mn1 Gd1 130.62(16) . . ? O5 Mn1 Gd1 128.10(16) 7_344 . ? O1 Mn1 Gd1 47.81(6) . . ? O1 Mn1 Gd1 110.77(6) 7_344 . ? O4 Mn1 Gd1 46.48(5) 7_344 . ? O4 Mn1 Gd1 112.79(6) . . ? O9 Mn1 Gd1 45.611(8) . . ? O5 Mn1 Gd1 128.10(16) . 7_344 ? O5 Mn1 Gd1 130.62(16) 7_344 7_344 ? O1 Mn1 Gd1 110.77(6) . 7_344 ? O1 Mn1 Gd1 47.81(6) 7_344 7_344 ? O4 Mn1 Gd1 112.79(6) 7_344 7_344 ? O4 Mn1 Gd1 46.48(5) . 7_344 ? O9 Mn1 Gd1 45.609(8) . 7_344 ? Gd1 Mn1 Gd1 91.220(16) . 7_344 ? O5 S1 O5' 97.4(3) . . ? O5 S1 C20 116.9(3) . . ? O5' S1 C20 112.2(2) . . ? O5 S1 C1 115.3(3) . . ? O5' S1 C1 114.5(3) . . ? C20 S1 C1 101.25(15) . . ? O6 S2 C5 108.50(15) . . ? O6 S2 C6 109.19(14) . . ? C5 S2 C6 105.00(16) . . ? O7 S3 C10 103.45(15) . . ? O7 S3 C11 103.63(14) . . ? C10 S3 C11 98.73(13) . . ? O8 S4 C16 107.29(14) . . ? O8 S4 C15 110.17(13) . . ? C16 S4 C15 104.48(14) . . ? C21 O1 Mn1 130.7(2) . . ? C21 O1 Gd1 138.4(2) . . ? Mn1 O1 Gd1 90.32(7) . . ? C22 O2 Gd1 137.0(2) . . ? C23 O3 Gd1 134.89(19) . 7_344 ? C24 O4 Mn1 131.1(2) . . ? C24 O4 Gd1 137.2(2) . 7_344 ? Mn1 O4 Gd1 91.47(7) . 7_344 ? S1 O5 O5 174.9(4) . 7_344 ? S1 O5 Mn1 118.9(3) . . ? O5 O5 Mn1 65.00(13) 7_344 . ? S2 O6 Gd1 127.83(14) . . ? S3 O7 Gd1 125.70(14) . 14_545 ? S4 O8 Gd1 126.95(13) . 7_344 ? Mn1 O9 Gd1 92.00(7) . . ? Mn1 O9 Gd1 92.01(7) . 7_344 ? Gd1 O9 Gd1 175.99(14) . 7_344 ? C2 C1 C21 123.6(3) . . ? C2 C1 S1 115.2(3) . . ? C21 C1 S1 121.1(2) . . ? C3 C2 C1 121.8(4) . . ? C3 C2 H2A 119.1 . . ? C1 C2 H2A 119.1 . . ? C4 C3 C2 116.3(3) . . ? C4 C3 C25 123.5(5) . . ? C2 C3 C25 120.2(5) . . ? C3 C4 C5 123.6(4) . . ? C3 C4 H4A 118.2 . . ? C5 C4 H4A 118.2 . . ? C4 C5 C21 121.3(4) . . ? C4 C5 S2 114.8(3) . . ? C21 C5 S2 123.9(2) . . ? C7 C6 C22 121.1(3) . . ? C7 C6 S2 114.0(3) . . ? C22 C6 S2 124.9(2) . . ? C8 C7 C6 122.0(3) . . ? C8 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? C9 C8 C7 117.0(3) . . ? C9 C8 C26 120.2(4) . . ? C7 C8 C26 122.8(4) . . ? C8 C9 C10 121.8(3) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C9 C10 C22 122.2(3) . . ? C9 C10 S3 119.9(3) . . ? C22 C10 S3 117.8(2) . . ? C12 C11 C23 122.8(3) . . ? C12 C11 S3 119.5(2) . . ? C23 C11 S3 117.6(2) . . ? C13 C12 C11 121.4(3) . . ? C13 C12 H12A 119.3 . . ? C11 C12 H12A 119.3 . . ? C14 C13 C12 116.6(3) . . ? C14 C13 C27 123.7(3) . . ? C12 C13 C27 119.7(3) . . ? C13 C14 C15 122.9(3) . . ? C13 C14 H14A 118.6 . . ? C15 C14 H14A 118.6 . . ? C14 C15 C23 121.1(3) . . ? C14 C15 S4 115.6(2) . . ? C23 C15 S4 123.2(2) . . ? C17 C16 C24 122.9(3) . . ? C17 C16 S4 111.6(3) . . ? C24 C16 S4 125.4(2) . . ? C18 C17 C16 121.6(3) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C19 C18 C17 116.1(3) . . ? C19 C18 C28 121.0(3) . . ? C17 C18 C28 122.9(4) . . ? C18 C19 C20 123.2(3) . . ? C18 C19 H19A 118.4 . . ? C20 C19 H19A 118.4 . . ? C19 C20 C24 122.8(3) . . ? C19 C20 S1 115.7(3) . . ? C24 C20 S1 121.5(2) . . ? O1 C21 C1 123.4(3) . . ? O1 C21 C5 123.3(3) . . ? C1 C21 C5 113.3(3) . . ? O2 C22 C10 120.0(3) . . ? O2 C22 C6 124.2(3) . . ? C10 C22 C6 115.8(3) . . ? O3 C23 C11 121.3(3) . . ? O3 C23 C15 123.6(3) . . ? C11 C23 C15 115.1(3) . . ? O4 C24 C16 124.3(3) . . ? O4 C24 C20 122.3(3) . . ? C16 C24 C20 113.4(3) . . ? C30 C25 C29 115.7(8) . . ? C30 C25 C31 104.3(8) . . ? C29 C25 C31 105.3(6) . . ? C30 C25 C3 108.1(6) . . ? C29 C25 C3 112.2(5) . . ? C31 C25 C3 110.9(6) . . ? C33 C26 C34 110.3(5) . . ? C33 C26 C8 109.6(4) . . ? C34 C26 C8 109.5(3) . . ? C33 C26 C32 109.3(5) . . ? C34 C26 C32 107.2(5) . . ? C8 C26 C32 111.0(4) . . ? C37 C27 C35 109.7(4) . . ? C37 C27 C13 111.6(4) . . ? C35 C27 C13 109.7(3) . . ? C37 C27 C36 107.8(4) . . ? C35 C27 C36 108.5(4) . . ? C13 C27 C36 109.5(3) . . ? C38 C28 C39 110.6(5) . . ? C38 C28 C40 106.4(4) . . ? C39 C28 C40 109.6(5) . . ? C38 C28 C18 112.6(4) . . ? C39 C28 C18 107.7(3) . . ? C40 C28 C18 110.0(3) . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30D 109.5 . . ? C25 C30 H30E 109.5 . . ? H30D C30 H30E 109.5 . . ? C25 C30 H30F 109.5 . . ? H30D C30 H30F 109.5 . . ? H30E C30 H30F 109.5 . . ? C25 C31 H31A 109.5 . . ? C25 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C25 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C26 C33 H33A 109.5 . . ? C26 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C26 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 H34A 109.5 . . ? C26 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C26 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C27 C35 H35A 109.5 . . ? C27 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C27 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C27 C36 H36A 109.5 . . ? C27 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C27 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C27 C37 H37A 109.5 . . ? C27 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C27 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C28 C38 H38A 109.5 . . ? C28 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C28 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C28 C39 H39A 109.5 . . ? C28 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C28 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C28 C40 H40A 109.5 . . ? C28 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C28 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.653 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.088 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.043 -0.002 -0.001 11687 3744 ' ' _platon_squeeze_details ; ; ###end data_compound_2_squeeze _database_code_depnum_ccdc_archive 'CCDC 712756' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Eu4Mn2(C40H44O8S4)4(H2O)2) _chemical_melting_point ? _chemical_formula_moiety '[Eu4Mn2(C40H44O8S4)4(H2O)2]' _chemical_formula_sum 'C160 H176 Eu4 Mn2 O34 S16' _chemical_formula_weight 3873.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mn Mn 0.3368 0.7283 '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 I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 19.6997(8) _cell_length_b 19.6997(8) _cell_length_c 65.255(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25324(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9473 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.79 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7864 _exptl_absorpt_coefficient_mu 1.251 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4882 _exptl_absorpt_correction_T_max 0.6955 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Apex CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 256781 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -85 _diffrn_reflns_limit_l_max 86 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.00 _reflns_number_total 15242 _reflns_number_gt 12512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (1998)' _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. In order to subtract the contribution from the disordered solvent molecules, the SQUEEZE command was used. All the non-hydrogen atoms were refined anisotropically. The sulfinyl oxygen atom (O5) was refined with two disordered sites (O5 and O5') both with the occupation factor being of 0.5 and the same displacement parameters. ; _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^)+(0.0755P)^2^+14.4712P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15242 _refine_ls_number_parameters 491 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.058 _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 Eu1 Eu 0.073660(7) 0.154541(8) 0.572365(2) 0.04114(6) Uani 1 1 d . . . Mn1 Mn 0.0000 0.2500 0.536974(9) 0.04218(14) Uani 1 2 d S . . S1 S 0.08758(6) 0.32043(6) 0.506330(16) 0.0689(3) Uani 1 1 d . . . S2 S 0.24643(4) 0.18462(4) 0.564446(14) 0.0534(2) Uani 1 1 d . . . S3 S 0.11698(4) 0.33887(4) 0.624416(11) 0.04442(17) Uani 1 1 d . . . S4 S -0.00233(4) 0.50569(4) 0.565989(13) 0.04832(18) Uani 1 1 d . . . O1 O 0.10772(10) 0.23184(11) 0.54458(3) 0.0463(5) Uani 1 1 d . . . O2 O 0.12183(11) 0.24637(15) 0.58941(4) 0.0651(7) Uani 1 1 d . . . O3 O 0.03158(11) 0.36823(10) 0.58829(3) 0.0478(5) Uani 1 1 d . . . O4 O 0.00347(10) 0.35990(11) 0.54409(3) 0.0450(5) Uani 1 1 d . . . O5 O 0.0340(3) 0.2795(3) 0.50765(7) 0.0660(10) Uani 0.50 1 d P . . O5' O 0.0887(3) 0.3271(3) 0.48523(8) 0.0660(10) Uani 0.50 1 d P . . O6 O 0.19048(11) 0.13349(12) 0.56733(4) 0.0543(5) Uani 1 1 d . . . O7 O 0.14418(15) 0.35697(13) 0.64558(3) 0.0670(7) Uani 1 1 d . . . O8 O -0.06617(11) 0.46366(11) 0.56763(3) 0.0504(5) Uani 1 1 d . . . O9 O 0.0000 0.2500 0.57110(4) 0.0437(6) Uani 1 2 d S . . C1 C 0.16425(17) 0.28912(17) 0.51703(5) 0.0533(8) Uani 1 1 d . . . C2 C 0.22265(19) 0.3046(2) 0.50615(6) 0.0650(10) Uani 1 1 d . . . H2A H 0.2189 0.3303 0.4939 0.078 Uiso 1 1 calc R . . C3 C 0.2855(2) 0.2842(2) 0.51252(7) 0.0757(12) Uani 1 1 d . . . C4 C 0.28799(18) 0.2477(2) 0.53045(7) 0.0679(10) Uani 1 1 d . . . H4A H 0.3309 0.2327 0.5353 0.081 Uiso 1 1 calc R . . C5 C 0.22967(16) 0.23152(17) 0.54202(6) 0.0541(8) Uani 1 1 d . . . C6 C 0.24250(15) 0.24494(16) 0.58465(5) 0.0482(7) Uani 1 1 d . . . C7 C 0.30639(16) 0.26934(17) 0.59078(6) 0.0569(8) Uani 1 1 d . . . H7A H 0.3458 0.2539 0.5838 0.068 Uiso 1 1 calc R . . C8 C 0.31347(16) 0.31548(17) 0.60679(7) 0.0613(10) Uani 1 1 d . . . C9 C 0.25474(17) 0.33483(15) 0.61701(6) 0.0529(8) Uani 1 1 d . . . H9A H 0.2580 0.3644 0.6285 0.064 Uiso 1 1 calc R . . C10 C 0.19131(14) 0.31181(14) 0.61083(5) 0.0416(6) Uani 1 1 d . . . C11 C 0.10499(14) 0.41991(14) 0.61242(4) 0.0401(6) Uani 1 1 d . . . C12 C 0.13860(16) 0.47613(16) 0.62016(5) 0.0483(7) Uani 1 1 d . . . H12A H 0.1671 0.4710 0.6318 0.058 Uiso 1 1 calc R . . C13 C 0.13159(16) 0.54001(15) 0.61125(6) 0.0502(7) Uani 1 1 d . . . C14 C 0.08674(15) 0.54485(15) 0.59496(5) 0.0491(7) Uani 1 1 d . . . H14A H 0.0790 0.5880 0.5889 0.059 Uiso 1 1 calc R . . C15 C 0.05240(14) 0.48840(14) 0.58709(5) 0.0420(6) Uani 1 1 d . . . C16 C 0.04367(15) 0.47571(16) 0.54435(5) 0.0474(7) Uani 1 1 d . . . C17 C 0.08098(16) 0.52750(18) 0.53508(5) 0.0535(8) Uani 1 1 d . . . H17A H 0.0798 0.5716 0.5409 0.064 Uiso 1 1 calc R . . C18 C 0.11957(16) 0.51704(19) 0.51772(6) 0.0567(8) Uani 1 1 d . . . C19 C 0.11854(17) 0.4522(2) 0.50988(5) 0.0562(8) Uani 1 1 d . . . H19A H 0.1444 0.4428 0.4979 0.067 Uiso 1 1 calc R . . C20 C 0.08134(16) 0.39970(17) 0.51865(5) 0.0501(7) Uani 1 1 d . . . C21 C 0.16371(15) 0.24967(16) 0.53507(5) 0.0485(7) Uani 1 1 d . . . C22 C 0.18290(14) 0.26629(16) 0.59457(5) 0.0432(6) Uani 1 1 d . . . C23 C 0.06138(14) 0.42325(14) 0.59556(4) 0.0403(6) Uani 1 1 d . . . C24 C 0.04095(15) 0.40948(16) 0.53635(5) 0.0449(7) Uani 1 1 d . . . C25 C 0.3485(3) 0.2993(4) 0.49960(10) 0.114(2) Uani 1 1 d . . . C26 C 0.3829(2) 0.3426(2) 0.61391(9) 0.0842(14) Uani 1 1 d . . . C27 C 0.17167(19) 0.60095(17) 0.61986(7) 0.0634(10) Uani 1 1 d . . . C28 C 0.15926(19) 0.5730(2) 0.50664(6) 0.0696(11) Uani 1 1 d . . . C29 C 0.3486(4) 0.3721(4) 0.49257(14) 0.167(3) Uani 1 1 d U . . H29A H 0.3097 0.3800 0.4835 0.251 Uiso 1 1 calc R . . H29B H 0.3907 0.3816 0.4851 0.251 Uiso 1 1 calc R . . H29C H 0.3454 0.4022 0.5045 0.251 Uiso 1 1 calc R . . C30 C 0.4115(4) 0.2927(5) 0.51206(15) 0.170(3) Uani 1 1 d U . . H30A H 0.4155 0.2460 0.5171 0.255 Uiso 1 1 calc R . . H30B H 0.4093 0.3240 0.5237 0.255 Uiso 1 1 calc R . . H30C H 0.4510 0.3037 0.5036 0.255 Uiso 1 1 calc R . . C31 C 0.3575(6) 0.2452(7) 0.4848(2) 0.284(6) Uani 1 1 d U . . H31A H 0.3182 0.2437 0.4756 0.426 Uiso 1 1 calc R . . H31B H 0.3616 0.2017 0.4919 0.426 Uiso 1 1 calc R . . H31C H 0.3987 0.2535 0.4767 0.426 Uiso 1 1 calc R . . C32 C 0.4388(2) 0.3207(3) 0.59895(14) 0.139(3) Uani 1 1 d . . . H32A H 0.4414 0.2710 0.5986 0.208 Uiso 1 1 calc R . . H32B H 0.4825 0.3392 0.6035 0.208 Uiso 1 1 calc R . . H32C H 0.4284 0.3380 0.5852 0.208 Uiso 1 1 calc R . . C33 C 0.3974(3) 0.3168(3) 0.63510(11) 0.134(3) Uani 1 1 d . . . H33A H 0.3991 0.2671 0.6349 0.201 Uiso 1 1 calc R . . H33B H 0.3614 0.3318 0.6444 0.201 Uiso 1 1 calc R . . H33C H 0.4411 0.3347 0.6398 0.201 Uiso 1 1 calc R . . C34 C 0.3816(2) 0.4196(2) 0.61356(9) 0.0872(14) Uani 1 1 d . . . H34A H 0.3466 0.4361 0.6230 0.131 Uiso 1 1 calc R . . H34B H 0.3713 0.4353 0.5996 0.131 Uiso 1 1 calc R . . H34C H 0.4259 0.4372 0.6178 0.131 Uiso 1 1 calc R . . C35 C 0.2472(2) 0.5838(2) 0.61976(8) 0.0799(13) Uani 1 1 d . . . H35A H 0.2620 0.5750 0.6057 0.120 Uiso 1 1 calc R . . H35B H 0.2552 0.5434 0.6282 0.120 Uiso 1 1 calc R . . H35C H 0.2730 0.6221 0.6254 0.120 Uiso 1 1 calc R . . C36 C 0.1593(3) 0.6646(2) 0.60744(9) 0.0907(15) Uani 1 1 d . . . H36A H 0.1731 0.6568 0.5932 0.136 Uiso 1 1 calc R . . H36B H 0.1859 0.7021 0.6132 0.136 Uiso 1 1 calc R . . H36C H 0.1109 0.6761 0.6079 0.136 Uiso 1 1 calc R . . C37 C 0.1494(3) 0.6150(3) 0.64212(8) 0.0947(16) Uani 1 1 d . . . H37A H 0.1008 0.6258 0.6424 0.142 Uiso 1 1 calc R . . H37B H 0.1753 0.6533 0.6476 0.142 Uiso 1 1 calc R . . H37C H 0.1578 0.5746 0.6505 0.142 Uiso 1 1 calc R . . C38 C 0.1614(3) 0.6376(3) 0.51859(10) 0.118(2) Uani 1 1 d . . . H38A H 0.1877 0.6716 0.5110 0.177 Uiso 1 1 calc R . . H38B H 0.1829 0.6294 0.5319 0.177 Uiso 1 1 calc R . . H38C H 0.1151 0.6544 0.5207 0.177 Uiso 1 1 calc R . . C39 C 0.2336(2) 0.5513(3) 0.50353(10) 0.1075(19) Uani 1 1 d . . . H39A H 0.2584 0.5876 0.4965 0.161 Uiso 1 1 calc R . . H39B H 0.2351 0.5098 0.4953 0.161 Uiso 1 1 calc R . . H39C H 0.2546 0.5427 0.5169 0.161 Uiso 1 1 calc R . . C40 C 0.1263(3) 0.5852(3) 0.48613(9) 0.121(2) Uani 1 1 d . . . H40A H 0.1511 0.6208 0.4788 0.181 Uiso 1 1 calc R . . H40B H 0.0791 0.5995 0.4882 0.181 Uiso 1 1 calc R . . H40C H 0.1272 0.5432 0.4781 0.181 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.03304(9) 0.05124(10) 0.03913(9) -0.00554(6) 0.00060(5) -0.00878(6) Mn1 0.0389(3) 0.0501(4) 0.0376(3) 0.000 0.000 -0.0095(3) S1 0.0730(6) 0.0802(7) 0.0535(5) -0.0113(4) -0.0108(4) -0.0033(5) S2 0.0346(4) 0.0558(5) 0.0697(5) -0.0078(4) 0.0036(3) -0.0013(3) S3 0.0518(4) 0.0415(4) 0.0400(4) 0.0025(3) -0.0012(3) -0.0136(3) S4 0.0415(4) 0.0403(4) 0.0631(5) 0.0078(3) -0.0010(3) 0.0023(3) O1 0.0361(10) 0.0569(13) 0.0459(11) -0.0052(9) 0.0053(8) -0.0078(9) O2 0.0296(10) 0.106(2) 0.0601(14) -0.0327(13) -0.0020(9) -0.0062(12) O3 0.0588(13) 0.0333(10) 0.0514(12) 0.0034(9) -0.0149(10) -0.0117(9) O4 0.0437(11) 0.0472(11) 0.0440(11) 0.0087(9) 0.0008(9) -0.0097(9) O5 0.068(2) 0.085(3) 0.0441(18) -0.0025(16) 0.0004(15) -0.0223(19) O5' 0.068(2) 0.085(3) 0.0441(18) -0.0025(16) 0.0004(15) -0.0223(19) O6 0.0401(11) 0.0610(14) 0.0616(13) -0.0052(11) 0.0045(10) -0.0039(10) O7 0.0923(19) 0.0700(16) 0.0386(11) 0.0003(11) -0.0079(12) -0.0291(14) O8 0.0390(11) 0.0518(13) 0.0605(13) 0.0100(10) -0.0010(9) 0.0008(9) O9 0.0432(15) 0.0398(15) 0.0483(16) 0.000 0.000 -0.0028(12) C1 0.0525(18) 0.0544(19) 0.0530(18) -0.0059(14) 0.0114(14) -0.0094(15) C2 0.060(2) 0.070(2) 0.065(2) 0.0010(18) 0.0224(17) -0.0161(18) C3 0.055(2) 0.084(3) 0.088(3) 0.006(2) 0.031(2) -0.011(2) C4 0.0401(18) 0.075(3) 0.089(3) -0.003(2) 0.0163(18) -0.0070(17) C5 0.0387(16) 0.0554(19) 0.068(2) -0.0079(16) 0.0101(14) -0.0079(14) C6 0.0364(15) 0.0457(16) 0.0624(19) 0.0012(14) -0.0077(13) -0.0039(12) C7 0.0328(15) 0.0483(18) 0.090(3) 0.0043(17) -0.0093(15) -0.0024(13) C8 0.0381(16) 0.0407(16) 0.105(3) 0.0021(17) -0.0217(17) -0.0056(13) C9 0.0507(18) 0.0362(15) 0.072(2) 0.0023(14) -0.0195(16) -0.0072(13) C10 0.0396(14) 0.0365(14) 0.0485(15) 0.0089(12) -0.0081(12) -0.0066(11) C11 0.0359(14) 0.0384(14) 0.0459(15) -0.0005(11) 0.0039(11) -0.0043(11) C12 0.0421(16) 0.0450(16) 0.0577(18) -0.0038(13) -0.0018(13) -0.0092(13) C13 0.0426(16) 0.0348(15) 0.073(2) -0.0091(14) 0.0054(15) -0.0081(12) C14 0.0422(16) 0.0332(14) 0.072(2) 0.0000(14) 0.0066(14) -0.0006(12) C15 0.0335(13) 0.0380(14) 0.0545(16) 0.0014(12) 0.0031(12) 0.0002(11) C16 0.0386(15) 0.0505(17) 0.0531(17) 0.0129(14) -0.0018(13) -0.0019(13) C17 0.0404(16) 0.0513(18) 0.069(2) 0.0185(15) -0.0081(14) -0.0079(13) C18 0.0407(16) 0.067(2) 0.063(2) 0.0257(17) -0.0057(14) -0.0117(15) C19 0.0446(17) 0.074(2) 0.0502(18) 0.0165(16) -0.0016(14) -0.0154(16) C20 0.0428(16) 0.0599(19) 0.0474(16) 0.0117(14) -0.0022(13) -0.0086(14) C21 0.0386(15) 0.0509(17) 0.0558(17) -0.0142(14) 0.0060(13) -0.0123(13) C22 0.0309(13) 0.0510(17) 0.0477(15) 0.0022(13) -0.0101(11) -0.0023(12) C23 0.0386(14) 0.0369(14) 0.0455(15) -0.0028(11) 0.0059(11) -0.0027(11) C24 0.0382(14) 0.0518(17) 0.0448(15) 0.0138(13) -0.0067(12) -0.0087(12) C25 0.059(3) 0.158(6) 0.126(5) 0.036(4) 0.045(3) -0.006(3) C26 0.047(2) 0.059(2) 0.147(4) 0.001(2) -0.038(2) -0.0108(17) C27 0.0533(19) 0.0416(17) 0.095(3) -0.0106(17) 0.0026(18) -0.0163(15) C28 0.054(2) 0.078(3) 0.076(2) 0.032(2) -0.0028(18) -0.0244(19) C29 0.101(4) 0.194(7) 0.206(7) 0.088(6) 0.050(4) -0.026(4) C30 0.092(4) 0.208(7) 0.210(7) 0.064(6) 0.065(5) -0.001(4) C31 0.251(8) 0.321(10) 0.278(9) -0.063(7) 0.213(7) -0.055(7) C32 0.035(2) 0.112(4) 0.269(9) -0.061(5) -0.025(3) -0.011(2) C33 0.099(4) 0.109(4) 0.194(7) 0.053(4) -0.101(4) -0.049(3) C34 0.059(2) 0.065(3) 0.137(4) -0.005(3) -0.021(3) -0.027(2) C35 0.061(2) 0.054(2) 0.125(4) -0.018(2) -0.008(2) -0.0172(18) C36 0.089(3) 0.045(2) 0.139(4) -0.004(2) -0.015(3) -0.021(2) C37 0.098(4) 0.076(3) 0.110(4) -0.042(3) 0.010(3) -0.033(3) C38 0.137(5) 0.084(3) 0.134(5) 0.029(3) 0.018(4) -0.061(3) C39 0.062(3) 0.127(5) 0.134(5) 0.043(4) 0.010(3) -0.024(3) C40 0.126(5) 0.126(5) 0.110(4) 0.078(4) -0.040(4) -0.049(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O2 2.326(2) . ? Eu1 O8 2.354(2) 2 ? Eu1 O6 2.361(2) . ? Eu1 O3 2.362(2) 2 ? Eu1 O9 2.3767(2) . ? Eu1 O7 2.393(2) 15_556 ? Eu1 O4 2.407(2) 2 ? Eu1 O1 2.461(2) . ? Eu1 Mn1 3.3129(5) . ? Eu1 S4 3.4801(8) 2 ? Eu1 S2 3.4932(8) . ? Eu1 S3 3.5116(8) 15_556 ? Mn1 O5 2.109(5) 2 ? Mn1 O5 2.109(5) . ? Mn1 O1 2.208(2) 2 ? Mn1 O1 2.209(2) . ? Mn1 O4 2.215(2) 2 ? Mn1 O4 2.215(2) . ? Mn1 O9 2.227(3) . ? Mn1 Eu1 3.3130(5) 2 ? S1 O5 1.330(5) . ? S1 O5' 1.383(5) . ? S1 C20 1.761(4) . ? S1 C1 1.775(4) . ? S2 O6 1.505(2) . ? S2 C5 1.762(4) . ? S2 C6 1.776(3) . ? S3 O7 1.524(2) . ? S3 C10 1.793(3) . ? S3 C11 1.794(3) . ? S3 Eu1 3.5113(8) 16_556 ? S4 O8 1.510(2) . ? S4 C16 1.779(3) . ? S4 C15 1.781(3) . ? S4 Eu1 3.4801(8) 2 ? O1 C21 1.314(4) . ? O2 C22 1.309(3) . ? O3 C23 1.321(3) . ? O3 Eu1 2.362(2) 2 ? O4 C24 1.324(3) . ? O4 Eu1 2.407(2) 2 ? O5 O5 1.775(10) 2 ? O7 Eu1 2.393(2) 16_556 ? O8 Eu1 2.354(2) 2 ? O9 Eu1 2.3767(2) 2 ? C1 C2 1.386(4) . ? C1 C21 1.411(5) . ? C2 C3 1.367(6) . ? C2 H2A 0.9500 . ? C3 C4 1.374(6) . ? C3 C25 1.530(5) . ? C4 C5 1.411(5) . ? C4 H4A 0.9500 . ? C5 C21 1.422(5) . ? C6 C22 1.405(4) . ? C6 C7 1.405(4) . ? C7 C8 1.392(5) . ? C7 H7A 0.9500 . ? C8 C9 1.389(5) . ? C8 C26 1.539(5) . ? C9 C10 1.389(4) . ? C9 H9A 0.9500 . ? C10 C22 1.399(4) . ? C11 C12 1.386(4) . ? C11 C23 1.398(4) . ? C12 C13 1.393(5) . ? C12 H12A 0.9500 . ? C13 C14 1.385(5) . ? C13 C27 1.543(4) . ? C14 C15 1.400(4) . ? C14 H14A 0.9500 . ? C15 C23 1.409(4) . ? C16 C17 1.395(4) . ? C16 C24 1.406(5) . ? C17 C18 1.379(5) . ? C17 H17A 0.9500 . ? C18 C19 1.376(5) . ? C18 C28 1.533(5) . ? C19 C20 1.390(4) . ? C19 H19A 0.9500 . ? C20 C24 1.416(4) . ? C25 C31 1.451(13) . ? C25 C30 1.489(10) . ? C25 C29 1.506(10) . ? C26 C33 1.500(8) . ? C26 C34 1.519(6) . ? C26 C32 1.535(8) . ? C27 C36 1.512(6) . ? C27 C35 1.527(6) . ? C27 C37 1.542(6) . ? C28 C38 1.494(8) . ? C28 C40 1.507(6) . ? C28 C39 1.539(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? 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 Eu1 O8 149.08(9) . 2 ? O2 Eu1 O6 78.78(8) . . ? O8 Eu1 O6 82.48(8) 2 . ? O2 Eu1 O3 107.18(7) . 2 ? O8 Eu1 O3 79.33(7) 2 2 ? O6 Eu1 O3 152.04(8) . 2 ? O2 Eu1 O9 69.53(7) . . ? O8 Eu1 O9 137.73(5) 2 . ? O6 Eu1 O9 136.81(6) . . ? O3 Eu1 O9 68.26(6) 2 . ? O2 Eu1 O7 77.41(10) . 15_556 ? O8 Eu1 O7 74.65(9) 2 15_556 ? O6 Eu1 O7 77.53(8) . 15_556 ? O3 Eu1 O7 77.29(9) 2 15_556 ? O9 Eu1 O7 120.99(9) . 15_556 ? O2 Eu1 O4 135.73(9) . 2 ? O8 Eu1 O4 75.10(7) 2 2 ? O6 Eu1 O4 119.19(7) . 2 ? O3 Eu1 O4 76.16(7) 2 2 ? O9 Eu1 O4 71.43(7) . 2 ? O7 Eu1 O4 142.72(9) 15_556 2 ? O2 Eu1 O1 76.11(8) . . ? O8 Eu1 O1 122.17(7) 2 . ? O6 Eu1 O1 74.95(8) . . ? O3 Eu1 O1 132.91(7) 2 . ? O9 Eu1 O1 69.60(7) . . ? O7 Eu1 O1 144.82(9) 15_556 . ? O4 Eu1 O1 71.36(7) 2 . ? O2 Eu1 Mn1 94.05(7) . . ? O8 Eu1 Mn1 116.27(5) 2 . ? O6 Eu1 Mn1 115.44(6) . . ? O3 Eu1 Mn1 91.72(6) 2 . ? O9 Eu1 Mn1 42.21(7) . . ? O7 Eu1 Mn1 163.14(6) 15_556 . ? O4 Eu1 Mn1 41.95(5) 2 . ? O1 Eu1 Mn1 41.81(5) . . ? O2 Eu1 S4 158.02(7) . 2 ? O8 Eu1 S4 20.22(5) 2 2 ? O6 Eu1 S4 102.57(6) . 2 ? O3 Eu1 S4 61.70(5) 2 2 ? O9 Eu1 S4 117.837(17) . 2 ? O7 Eu1 S4 81.46(7) 15_556 2 ? O4 Eu1 S4 63.02(5) 2 2 ? O1 Eu1 S4 125.68(5) . 2 ? Mn1 Eu1 S4 104.749(15) . 2 ? O2 Eu1 S2 62.70(5) . . ? O8 Eu1 S2 102.09(5) 2 . ? O6 Eu1 S2 19.89(6) . . ? O3 Eu1 S2 162.27(6) 2 . ? O9 Eu1 S2 117.10(2) . . ? O7 Eu1 S2 86.00(7) 15_556 . ? O4 Eu1 S2 121.44(5) 2 . ? O1 Eu1 S2 61.34(5) . . ? Mn1 Eu1 S2 103.141(17) . . ? S4 Eu1 S2 121.98(2) 2 . ? O2 Eu1 S3 65.55(7) . 15_556 ? O8 Eu1 S3 90.91(6) 2 15_556 ? O6 Eu1 S3 91.91(6) . 15_556 ? O3 Eu1 S3 67.47(6) 2 15_556 ? O9 Eu1 S3 100.48(7) . 15_556 ? O7 Eu1 S3 20.56(6) 15_556 15_556 ? O4 Eu1 S3 142.92(5) 2 15_556 ? O1 Eu1 S3 141.27(5) . 15_556 ? Mn1 Eu1 S3 142.688(15) . 15_556 ? S4 Eu1 S3 92.48(2) 2 15_556 ? S2 Eu1 S3 94.80(2) . 15_556 ? O5 Mn1 O5 49.8(3) 2 . ? O5 Mn1 O1 86.74(16) 2 2 ? O5 Mn1 O1 117.69(16) . 2 ? O5 Mn1 O1 117.69(16) 2 . ? O5 Mn1 O1 86.74(16) . . ? O1 Mn1 O1 154.02(11) 2 . ? O5 Mn1 O4 84.87(16) 2 2 ? O5 Mn1 O4 117.99(17) . 2 ? O1 Mn1 O4 94.68(8) 2 2 ? O1 Mn1 O4 79.88(8) . 2 ? O5 Mn1 O4 117.99(17) 2 . ? O5 Mn1 O4 84.88(16) . . ? O1 Mn1 O4 79.88(8) 2 . ? O1 Mn1 O4 94.68(8) . . ? O4 Mn1 O4 155.82(11) 2 . ? O5 Mn1 O9 155.11(13) 2 . ? O5 Mn1 O9 155.11(13) . . ? O1 Mn1 O9 77.01(5) 2 . ? O1 Mn1 O9 77.01(5) . . ? O4 Mn1 O9 77.91(5) 2 . ? O4 Mn1 O9 77.91(5) . . ? O5 Mn1 Eu1 127.96(16) 2 . ? O5 Mn1 Eu1 130.52(16) . . ? O1 Mn1 Eu1 110.87(6) 2 . ? O1 Mn1 Eu1 47.97(6) . . ? O4 Mn1 Eu1 46.59(5) 2 . ? O4 Mn1 Eu1 113.28(6) . . ? O9 Mn1 Eu1 45.805(8) . . ? O5 Mn1 Eu1 130.52(16) 2 2 ? O5 Mn1 Eu1 127.96(16) . 2 ? O1 Mn1 Eu1 47.97(6) 2 2 ? O1 Mn1 Eu1 110.86(6) . 2 ? O4 Mn1 Eu1 113.28(6) 2 2 ? O4 Mn1 Eu1 46.59(5) . 2 ? O9 Mn1 Eu1 45.805(8) . 2 ? Eu1 Mn1 Eu1 91.610(16) . 2 ? O5 S1 O5' 97.7(3) . . ? O5 S1 C20 116.9(3) . . ? O5' S1 C20 111.8(3) . . ? O5 S1 C1 116.0(3) . . ? O5' S1 C1 114.3(3) . . ? C20 S1 C1 100.84(16) . . ? O6 S2 C5 108.52(15) . . ? O6 S2 C6 108.84(14) . . ? C5 S2 C6 104.92(16) . . ? O6 S2 Eu1 32.26(9) . . ? C5 S2 Eu1 91.68(10) . . ? C6 S2 Eu1 87.78(10) . . ? O7 S3 C10 103.33(15) . . ? O7 S3 C11 103.51(14) . . ? C10 S3 C11 99.00(13) . . ? O7 S3 Eu1 33.48(10) . 16_556 ? C10 S3 Eu1 124.21(9) . 16_556 ? C11 S3 Eu1 119.45(10) . 16_556 ? O8 S4 C16 107.37(14) . . ? O8 S4 C15 110.15(13) . . ? C16 S4 C15 103.99(14) . . ? O8 S4 Eu1 32.61(8) . 2 ? C16 S4 Eu1 89.97(10) . 2 ? C15 S4 Eu1 88.77(10) . 2 ? C21 O1 Mn1 131.1(2) . . ? C21 O1 Eu1 138.0(2) . . ? Mn1 O1 Eu1 90.22(7) . . ? C22 O2 Eu1 137.0(2) . . ? C23 O3 Eu1 134.75(19) . 2 ? C24 O4 Mn1 131.2(2) . . ? C24 O4 Eu1 137.0(2) . 2 ? Mn1 O4 Eu1 91.47(7) . 2 ? S1 O5 O5 174.9(5) . 2 ? S1 O5 Mn1 118.6(3) . . ? O5 O5 Mn1 65.11(13) 2 . ? S2 O6 Eu1 127.86(14) . . ? S3 O7 Eu1 125.95(14) . 16_556 ? S4 O8 Eu1 127.17(12) . 2 ? Mn1 O9 Eu1 91.98(7) . . ? Mn1 O9 Eu1 91.98(7) . 2 ? Eu1 O9 Eu1 176.03(13) . 2 ? C2 C1 C21 123.7(3) . . ? C2 C1 S1 115.4(3) . . ? C21 C1 S1 120.9(2) . . ? C3 C2 C1 122.1(4) . . ? C3 C2 H2A 119.0 . . ? C1 C2 H2A 119.0 . . ? C2 C3 C4 116.5(3) . . ? C2 C3 C25 120.7(4) . . ? C4 C3 C25 122.8(4) . . ? C3 C4 C5 123.0(4) . . ? C3 C4 H4A 118.5 . . ? C5 C4 H4A 118.5 . . ? C4 C5 C21 121.1(3) . . ? C4 C5 S2 114.2(3) . . ? C21 C5 S2 124.6(2) . . ? C22 C6 C7 121.0(3) . . ? C22 C6 S2 125.3(2) . . ? C7 C6 S2 113.7(3) . . ? C8 C7 C6 121.8(3) . . ? C8 C7 H7A 119.1 . . ? C6 C7 H7A 119.1 . . ? C9 C8 C7 117.1(3) . . ? C9 C8 C26 120.0(4) . . ? C7 C8 C26 122.8(4) . . ? C8 C9 C10 121.4(3) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C9 C10 C22 122.4(3) . . ? C9 C10 S3 119.6(3) . . ? C22 C10 S3 118.0(2) . . ? C12 C11 C23 122.9(3) . . ? C12 C11 S3 119.3(2) . . ? C23 C11 S3 117.8(2) . . ? C11 C12 C13 121.5(3) . . ? C11 C12 H12A 119.3 . . ? C13 C12 H12A 119.3 . . ? C14 C13 C12 116.5(3) . . ? C14 C13 C27 123.5(3) . . ? C12 C13 C27 120.0(3) . . ? C13 C14 C15 122.4(3) . . ? C13 C14 H14A 118.8 . . ? C15 C14 H14A 118.8 . . ? C14 C15 C23 121.3(3) . . ? C14 C15 S4 115.1(2) . . ? C23 C15 S4 123.6(2) . . ? C17 C16 C24 122.5(3) . . ? C17 C16 S4 111.7(3) . . ? C24 C16 S4 125.7(2) . . ? C18 C17 C16 122.5(3) . . ? C18 C17 H17A 118.8 . . ? C16 C17 H17A 118.8 . . ? C19 C18 C17 115.8(3) . . ? C19 C18 C28 120.0(3) . . ? C17 C18 C28 124.1(4) . . ? C18 C19 C20 123.0(3) . . ? C18 C19 H19A 118.5 . . ? C20 C19 H19A 118.5 . . ? C19 C20 C24 122.1(3) . . ? C19 C20 S1 115.8(3) . . ? C24 C20 S1 122.2(2) . . ? O1 C21 C1 123.2(3) . . ? O1 C21 C5 123.3(3) . . ? C1 C21 C5 113.4(3) . . ? O2 C22 C10 119.7(3) . . ? O2 C22 C6 124.0(3) . . ? C10 C22 C6 116.3(3) . . ? O3 C23 C11 121.2(3) . . ? O3 C23 C15 123.4(3) . . ? C11 C23 C15 115.4(3) . . ? O4 C24 C16 124.4(3) . . ? O4 C24 C20 121.6(3) . . ? C16 C24 C20 114.1(3) . . ? C31 C25 C30 101.5(8) . . ? C31 C25 C29 119.8(8) . . ? C30 C25 C29 104.4(6) . . ? C31 C25 C3 108.9(6) . . ? C30 C25 C3 111.0(5) . . ? C29 C25 C3 110.7(5) . . ? C33 C26 C34 110.8(5) . . ? C33 C26 C32 110.8(5) . . ? C34 C26 C32 106.4(4) . . ? C33 C26 C8 109.3(4) . . ? C34 C26 C8 109.1(3) . . ? C32 C26 C8 110.4(4) . . ? C36 C27 C35 109.8(3) . . ? C36 C27 C37 108.1(4) . . ? C35 C27 C37 108.8(4) . . ? C36 C27 C13 111.5(3) . . ? C35 C27 C13 109.0(3) . . ? C37 C27 C13 109.7(3) . . ? C38 C28 C40 109.9(5) . . ? C38 C28 C18 112.4(4) . . ? C40 C28 C18 108.3(3) . . ? C38 C28 C39 106.2(4) . . ? C40 C28 C39 109.7(5) . . ? C18 C28 C39 110.3(3) . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 C31 H31A 109.5 . . ? C25 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C25 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C26 C33 H33A 109.5 . . ? C26 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C26 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 H34A 109.5 . . ? C26 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C26 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C27 C35 H35A 109.5 . . ? C27 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C27 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C27 C36 H36A 109.5 . . ? C27 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C27 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C27 C37 H37A 109.5 . . ? C27 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C27 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C28 C38 H38A 109.5 . . ? C28 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C28 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C28 C39 H39A 109.5 . . ? C28 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C28 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C28 C40 H40A 109.5 . . ? C28 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C28 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.732 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.085 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.066 0.000 -0.001 11479 3419 ' ' _platon_squeeze_details ; ; ###end