# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Pantelis Trikalitis' _publ_contact_author_email PTRIKAL@CHEMISTRY.UOC.GR _publ_section_title ; Remarkable structural diversity and single-crystal-to-single-crystal transformations in sulfone functionalized lanthanide MOF's ; loop_ _publ_author_name 'Pantelis Trikalitis' 'Christos D. Malliakas' 'Eleftheria Neofotistou' # Attachment 'Revised_Ce2.cif' data_Ce2 _database_code_depnum_ccdc_archive 'CCDC 736837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H60 Ce2 N6 O24 S3' _chemical_formula_weight 1625.56 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.711(4) _cell_length_b 18.928(4) _cell_length_c 23.826(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.74(3) _cell_angle_gamma 90.00 _cell_volume 7938(3) _cell_formula_units_Z 4 _cell_measurement_temperature 130(1) _cell_measurement_reflns_used 5998 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 23.48 _exptl_crystal_description rod-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9108 _exptl_absorpt_correction_T_max 0.9898 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(1) _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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55316 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 23.48 _reflns_number_total 11543 _reflns_number_gt 7532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The following least-square restraints were applied (total 66) to atoms corresponding to disordered guest DMF molecules: isor 0.005 O3, O8, C14, C41, N1, C42, O19, O22, O23, C56, C58 All the other non-hydrogen atoms were refined anisotropically. 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^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11543 _refine_ls_number_parameters 856 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 0.852 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 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 Ce1 Ce 0.40374(2) 0.986238(18) 0.024158(14) 0.02317(11) Uani 1 1 d . . . Ce2 Ce 0.097502(19) 1.003948(18) -0.016414(14) 0.02162(10) Uani 1 1 d . . . O1 O 0.2281(2) 0.9995(2) 0.07096(17) 0.0323(11) Uani 1 1 d . . . O2 O 0.3298(2) 1.0479(3) 0.06731(19) 0.0409(13) Uani 1 1 d . . . C1 C 0.2836(3) 1.0416(4) 0.0905(3) 0.0310(16) Uani 1 1 d . . . C2 C 0.2981(3) 1.0861(4) 0.1475(3) 0.0291(15) Uani 1 1 d . . . C3 C 0.2627(4) 1.0707(3) 0.1853(3) 0.0297(15) Uani 1 1 d . . . H3 H 0.2294 1.0326 0.1749 0.036 Uiso 1 1 calc R . . C4 C 0.3464(4) 1.1440(4) 0.1609(3) 0.0394(18) Uani 1 1 d . . . H4 H 0.3701 1.1552 0.1361 0.047 Uiso 1 1 calc R . . C59 C 0.2758(4) 1.1108(3) 0.2379(3) 0.0296(15) Uani 1 1 d . . . H59 H 0.2529 1.0991 0.2633 0.035 Uiso 1 1 calc R . . C5 C 0.3576(4) 1.1843(4) 0.2131(3) 0.0369(17) Uani 1 1 d . . . C6 C 0.3236(4) 1.1684(3) 0.2518(3) 0.0293(15) Uani 1 1 d . . . C7 C 0.3438(4) 1.2204(3) 0.3037(3) 0.0333(16) Uani 1 1 d . . . C8 C 0.3951(4) 1.2725(3) 0.3040(3) 0.0314(16) Uani 1 1 d . . . C9 C 0.3176(4) 1.2240(3) 0.3488(3) 0.0311(16) Uani 1 1 d . . . H9 H 0.2838 1.1905 0.3500 0.037 Uiso 1 1 calc R . . C10 C 0.4219(4) 1.3257(4) 0.3474(3) 0.0354(17) Uani 1 1 d . . . H10 H 0.4571 1.3583 0.3471 0.043 Uiso 1 1 calc R . . C11 C 0.3434(4) 1.2792(3) 0.3923(3) 0.0296(15) Uani 1 1 d . . . H11 H 0.3256 1.2823 0.4224 0.036 Uiso 1 1 calc R . . C12 C 0.3942(4) 1.3292(3) 0.3924(3) 0.0325(16) Uani 1 1 d . . . C13 C 0.4171(5) 1.3884(4) 0.4395(3) 0.048(2) Uani 1 1 d . . . O3 O 0.5269(4) 0.9254(4) 0.0551(3) 0.097(2) Uani 1 1 d U . . O4 O 0.3811(3) 1.1020(2) -0.0304(2) 0.0483(15) Uani 1 1 d . . . S1 S 0.41444(11) 1.26127(11) 0.23875(9) 0.0456(5) Uani 1 1 d . . . O5 O 0.3821(3) 1.3183(3) 0.1940(2) 0.0656(17) Uani 1 1 d . . . O6 O 0.4929(3) 1.2449(3) 0.2585(2) 0.0587(16) Uani 1 1 d . . . O7 O 0.4981(2) 1.0755(2) 0.09258(18) 0.0308(11) Uani 1 1 d . . . O8 O 0.4102(4) 0.9392(5) -0.0656(3) 0.103(2) Uani 1 1 d U . . C14 C 0.5624(4) 1.0892(4) 0.0976(3) 0.0399(18) Uani 1 1 d U . . C15 C -0.3867(4) 1.3614(4) -0.3514(3) 0.0300(16) Uani 1 1 d . . . C16 C -0.4163(4) 1.3173(4) -0.3210(3) 0.0342(17) Uani 1 1 d . . . H16 H -0.4674 1.3211 -0.3304 0.041 Uiso 1 1 calc R . . C17 C -0.3092(4) 1.3589(4) -0.3355(3) 0.0319(16) Uani 1 1 d . . . H17 H -0.2885 1.3879 -0.3553 0.038 Uiso 1 1 calc R . . C18 C -0.2647(3) 1.3121(3) -0.2896(3) 0.0274(15) Uani 1 1 d . . . C19 C -0.2929(4) 1.2656(3) -0.2599(3) 0.0291(15) Uani 1 1 d . . . C60 C -0.3708(4) 1.2675(4) -0.2767(3) 0.0360(17) Uani 1 1 d . . . H60 H -0.3919 1.2363 -0.2587 0.043 Uiso 1 1 calc R . . C20 C -0.2358(3) 1.2169(3) -0.2161(3) 0.0285(15) Uani 1 1 d . . . C21 C -0.1629(3) 1.2275(3) -0.2118(3) 0.0233(14) Uani 1 1 d . . . C22 C -0.2463(4) 1.1618(3) -0.1823(3) 0.0329(16) Uani 1 1 d . . . H22 H -0.2942 1.1532 -0.1850 0.040 Uiso 1 1 calc R . . C23 C -0.1023(3) 1.1863(3) -0.1750(3) 0.0233(14) Uani 1 1 d . . . H23 H -0.0548 1.1944 -0.1730 0.028 Uiso 1 1 calc R . . C24 C -0.1856(3) 1.1199(3) -0.1447(3) 0.0277(15) Uani 1 1 d . . . H24 H -0.1930 1.0833 -0.1220 0.033 Uiso 1 1 calc R . . C25 C -0.1132(3) 1.1314(3) -0.1401(3) 0.0244(14) Uani 1 1 d . . . C26 C -0.0469(4) 1.0859(3) -0.0983(3) 0.0244(15) Uani 1 1 d . . . O9 O 0.0118(2) 1.0860(2) -0.10627(18) 0.0289(10) Uani 1 1 d . . . S2 S -0.16448(9) 1.30209(9) -0.25846(7) 0.0294(4) Uani 1 1 d . . . O10 O -0.1261(3) 1.3615(2) -0.2179(2) 0.0370(11) Uani 1 1 d . . . O11 O -0.1433(3) 1.2842(3) -0.30674(19) 0.0397(12) Uani 1 1 d . . . O12 O 0.0868(2) 1.1006(2) 0.05044(17) 0.0243(10) Uani 1 1 d . . . O13 O -0.0016(2) 0.9178(2) -0.08727(18) 0.0316(11) Uani 1 1 d . . . C27 C 0.0547(4) 1.1163(3) 0.0835(3) 0.0265(15) Uani 1 1 d . . . C28 C 0.0822(3) 1.1818(3) 0.1244(3) 0.0233(14) Uani 1 1 d . . . C29 C 0.1462(3) 1.2184(3) 0.1286(3) 0.0258(14) Uani 1 1 d . . . H29 H 0.1692 1.2037 0.1040 0.031 Uiso 1 1 calc R . . C30 C 0.0461(3) 1.2052(3) 0.1592(3) 0.0271(15) Uani 1 1 d . . . H30 H 0.0030 1.1822 0.1565 0.032 Uiso 1 1 calc R . . C31 C 0.0749(4) 1.2635(3) 0.1979(3) 0.0279(15) Uani 1 1 d . . . C32 C 0.1762(3) 1.2757(3) 0.1683(3) 0.0266(14) Uani 1 1 d . . . H32 H 0.2189 1.2988 0.1705 0.032 Uiso 1 1 calc R . . C33 C 0.1421(3) 1.2984(3) 0.2049(3) 0.0221(14) Uani 1 1 d . . . C34 C 0.1662(3) 1.3547(3) 0.2530(3) 0.0242(14) Uani 1 1 d . . . C35 C 0.2310(4) 1.3968(3) 0.2764(3) 0.0277(15) Uani 1 1 d . . . H35 H 0.2654 1.3929 0.2597 0.033 Uiso 1 1 calc R . . C36 C 0.1161(4) 1.3627(3) 0.2802(3) 0.0255(14) Uani 1 1 d . . . C37 C 0.1270(4) 1.4102(3) 0.3273(3) 0.0284(15) Uani 1 1 d . . . H37 H 0.0917 1.4146 0.3431 0.034 Uiso 1 1 calc R . . C38 C 0.2446(3) 1.4453(3) 0.3253(3) 0.0250(14) Uani 1 1 d . . . H38 H 0.2880 1.4733 0.3408 0.030 Uiso 1 1 calc R . . C39 C 0.1928(4) 1.4514(3) 0.3506(3) 0.0278(15) Uani 1 1 d . . . C40 C 0.2065(4) 0.9979(3) -0.0962(3) 0.0277(15) Uani 1 1 d . . . O14 O 0.0353(3) 1.2554(2) 0.2906(2) 0.0378(12) Uani 1 1 d . . . S3 S 0.03828(10) 1.30402(9) 0.24555(8) 0.0308(4) Uani 1 1 d . . . O24 O -0.0301(3) 1.3437(3) 0.2072(2) 0.0424(12) Uani 1 1 d . . . O15 O 0.2734(3) 0.9767(2) -0.06378(19) 0.0338(11) Uani 1 1 d . . . O16 O 0.1500(2) 0.9793(2) -0.08878(17) 0.0296(10) Uani 1 1 d . . . O17 O 0.0535(2) 0.9519(2) 0.05644(17) 0.0246(10) Uani 1 1 d . . . O18 O 0.1424(3) 0.8762(3) 0.00459(19) 0.0369(12) Uani 1 1 d . . . C41 C 0.1552(5) 0.8334(4) -0.0255(3) 0.050(2) Uani 1 1 d U . . H41 H 0.1761 0.8493 -0.0512 0.060 Uiso 1 1 calc R . . N1 N 0.1427(5) 0.7674(4) -0.0257(3) 0.070(2) Uani 1 1 d U . . C42 C 0.1658(9) 0.7192(8) -0.0611(6) 0.145(5) Uani 1 1 d U . . H42A H 0.1528 0.6717 -0.0555 0.217 Uiso 1 1 calc R . . H42B H 0.2198 0.7225 -0.0465 0.217 Uiso 1 1 calc R . . H42C H 0.1403 0.7313 -0.1049 0.217 Uiso 1 1 calc R . . C43 C 0.1048(6) 0.7396(5) 0.0077(5) 0.091(4) Uani 1 1 d . . . H43A H 0.1001 0.6893 0.0021 0.137 Uiso 1 1 calc R . . H43B H 0.0551 0.7603 -0.0080 0.137 Uiso 1 1 calc R . . H43C H 0.1334 0.7503 0.0515 0.137 Uiso 1 1 calc R . . O19 O 0.3631(4) 0.8626(3) 0.0287(4) 0.0810(19) Uani 1 1 d U . . C44 C 0.3868(7) 0.8043(6) 0.0280(6) 0.102(4) Uani 1 1 d . . . H44 H 0.4093 0.7948 0.0019 0.123 Uiso 1 1 calc R . . N2 N 0.3812(6) 0.7527(4) 0.0643(4) 0.093(3) Uani 1 1 d . . . C45 C 0.3420(7) 0.7607(7) 0.0988(5) 0.110(5) Uani 1 1 d . . . H45A H 0.3453 0.7180 0.1216 0.165 Uiso 1 1 calc R . . H45B H 0.2896 0.7707 0.0711 0.165 Uiso 1 1 calc R . . H45C H 0.3633 0.7991 0.1278 0.165 Uiso 1 1 calc R . . C46 C 0.4244(8) 0.6879(6) 0.0727(6) 0.127(5) Uani 1 1 d . . . H46A H 0.4489 0.6889 0.0458 0.190 Uiso 1 1 calc R . . H46B H 0.3907 0.6481 0.0620 0.190 Uiso 1 1 calc R . . H46C H 0.4620 0.6841 0.1157 0.190 Uiso 1 1 calc R . . O20 O 0.1698(3) 1.1129(2) -0.02313(19) 0.0324(11) Uani 1 1 d . . . C47 C 0.2063(5) 1.1668(5) -0.0163(3) 0.056(2) Uani 1 1 d . . . H47 H 0.2577 1.1607 -0.0047 0.067 Uiso 1 1 calc R . . N3 N 0.1821(4) 1.2330(3) -0.0232(3) 0.0427(15) Uani 1 1 d . . . C48 C 0.2284(7) 1.2936(5) -0.0171(6) 0.108(4) Uani 1 1 d . . . H48A H 0.1979 1.3355 -0.0261 0.161 Uiso 1 1 calc R . . H48B H 0.2497 1.2899 -0.0462 0.161 Uiso 1 1 calc R . . H48C H 0.2687 1.2960 0.0250 0.161 Uiso 1 1 calc R . . C49 C 0.1018(4) 1.2460(5) -0.0443(4) 0.058(2) Uani 1 1 d . . . H49A H 0.0923 1.2959 -0.0484 0.087 Uiso 1 1 calc R . . H49B H 0.0868 1.2270 -0.0142 0.087 Uiso 1 1 calc R . . H49C H 0.0731 1.2235 -0.0842 0.087 Uiso 1 1 calc R . . O21 O 0.1942(3) 1.1003(3) 0.3369(2) 0.0494(14) Uani 1 1 d . . . C50 C 0.1244(4) 1.0996(4) 0.3125(3) 0.0406(18) Uani 1 1 d . . . H50 H 0.1008 1.1338 0.3257 0.049 Uiso 1 1 calc R . . N4 N 0.0799(3) 1.0542(3) 0.2690(2) 0.0312(13) Uani 1 1 d . . . C51 C -0.0019(4) 1.0588(4) 0.2414(4) 0.055(2) Uani 1 1 d . . . H51A H -0.0240 1.0222 0.2106 0.083 Uiso 1 1 calc R . . H51B H -0.0181 1.1041 0.2217 0.083 Uiso 1 1 calc R . . H51C H -0.0180 1.0532 0.2737 0.083 Uiso 1 1 calc R . . C52 C 0.1111(4) 1.0007(4) 0.2443(3) 0.0492(19) Uani 1 1 d . . . H52A H 0.0705 0.9736 0.2130 0.074 Uiso 1 1 calc R . . H52B H 0.1435 0.9701 0.2778 0.074 Uiso 1 1 calc R . . H52C H 0.1400 1.0228 0.2258 0.074 Uiso 1 1 calc R . . O22 O 0.4509(4) 0.9536(3) 0.1430(2) 0.0658(16) Uani 1 1 d U . . C53 C 0.4709(6) 0.9983(4) 0.1862(3) 0.073(3) Uani 1 1 d . . . H53 H 0.4841 1.0431 0.1784 0.087 Uiso 1 1 calc R . . N5 N 0.4747(4) 0.9867(3) 0.2421(2) 0.0482(16) Uani 1 1 d . . . C54 C 0.4521(5) 0.9196(5) 0.2574(4) 0.060(2) Uani 1 1 d . . . H54A H 0.4592 0.9206 0.2999 0.091 Uiso 1 1 calc R . . H54B H 0.4826 0.8826 0.2528 0.091 Uiso 1 1 calc R . . H54C H 0.3996 0.9110 0.2295 0.091 Uiso 1 1 calc R . . C55 C 0.4965(6) 1.0419(5) 0.2895(3) 0.067(3) Uani 1 1 d . . . H55A H 0.4963 1.0232 0.3269 0.101 Uiso 1 1 calc R . . H55B H 0.4610 1.0803 0.2739 0.101 Uiso 1 1 calc R . . H55C H 0.5465 1.0585 0.2991 0.101 Uiso 1 1 calc R . . O23 O 0.3698(9) 0.9563(9) 0.3509(7) 0.224(6) Uani 1 1 d U . . C56 C 0.3309(15) 0.9842(15) 0.3759(12) 0.242(12) Uani 1 1 d U . . H56 H 0.3303 1.0311 0.3873 0.291 Uiso 1 1 calc R . . N6 N 0.2894(8) 0.9272(8) 0.3819(6) 0.150(5) Uani 1 1 d . . . C57 C 0.2302(12) 0.9438(11) 0.4044(10) 0.229(12) Uani 1 1 d . . . H57A H 0.2086 0.9005 0.4102 0.343 Uiso 1 1 calc R . . H57B H 0.1908 0.9725 0.3737 0.343 Uiso 1 1 calc R . . H57C H 0.2537 0.9688 0.4436 0.343 Uiso 1 1 calc R . . C58 C 0.3090(11) 0.8550(10) 0.3854(9) 0.192(8) Uani 1 1 d U . . H58A H 0.2731 0.8273 0.3930 0.287 Uiso 1 1 calc R . . H58B H 0.3590 0.8480 0.4191 0.287 Uiso 1 1 calc R . . H58C H 0.3081 0.8405 0.3464 0.287 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 Ce1 0.0379(2) 0.01660(17) 0.01829(17) -0.00031(15) 0.01549(16) -0.00024(18) Ce2 0.01491(17) 0.0351(2) 0.01330(16) 0.00016(15) 0.00492(13) -0.00778(18) O1 0.015(2) 0.059(3) 0.018(2) -0.001(2) 0.0030(17) -0.005(2) O2 0.020(3) 0.080(4) 0.025(2) -0.017(2) 0.012(2) -0.013(2) C1 0.012(3) 0.059(5) 0.016(3) -0.007(3) 0.002(3) -0.004(3) C2 0.017(3) 0.053(4) 0.018(3) -0.006(3) 0.008(3) -0.004(3) C3 0.021(4) 0.040(4) 0.028(3) -0.004(3) 0.010(3) -0.001(3) C4 0.020(4) 0.076(5) 0.029(4) -0.007(4) 0.017(3) -0.009(4) C59 0.027(4) 0.035(4) 0.032(4) -0.003(3) 0.018(3) -0.005(3) C5 0.023(4) 0.057(5) 0.035(4) -0.007(3) 0.017(3) -0.012(3) C6 0.019(4) 0.038(4) 0.032(4) -0.005(3) 0.013(3) -0.004(3) C7 0.024(4) 0.034(4) 0.043(4) 0.001(3) 0.015(3) -0.001(3) C8 0.022(4) 0.037(4) 0.035(4) -0.005(3) 0.014(3) -0.014(3) C9 0.032(4) 0.031(4) 0.042(4) -0.010(3) 0.027(3) -0.013(3) C10 0.020(4) 0.039(4) 0.040(4) 0.001(3) 0.007(3) -0.012(3) C11 0.027(4) 0.028(4) 0.033(3) -0.010(3) 0.012(3) -0.009(3) C12 0.021(4) 0.033(4) 0.029(4) 0.000(3) -0.001(3) -0.007(3) C13 0.045(5) 0.040(5) 0.024(4) 0.003(3) -0.014(4) -0.017(4) O3 0.120(4) 0.098(4) 0.055(3) 0.004(3) 0.023(3) 0.082(4) O4 0.041(3) 0.030(3) 0.042(3) 0.019(2) -0.009(3) -0.008(2) S1 0.0323(11) 0.0661(14) 0.0446(11) -0.0078(10) 0.0228(9) -0.0232(10) O5 0.072(4) 0.073(4) 0.047(3) 0.012(3) 0.022(3) -0.027(3) O6 0.031(3) 0.092(5) 0.062(4) -0.026(3) 0.030(3) -0.025(3) O7 0.021(3) 0.046(3) 0.024(2) -0.007(2) 0.008(2) 0.003(2) O8 0.069(4) 0.170(5) 0.086(4) -0.081(3) 0.047(3) -0.024(3) C14 0.024(3) 0.061(4) 0.032(3) -0.017(3) 0.009(3) 0.006(3) C15 0.023(4) 0.052(4) 0.022(3) 0.012(3) 0.016(3) 0.000(3) C16 0.015(4) 0.052(5) 0.035(4) 0.009(3) 0.011(3) 0.000(3) C17 0.026(4) 0.051(4) 0.024(3) 0.007(3) 0.016(3) -0.006(3) C18 0.019(3) 0.037(4) 0.027(3) 0.002(3) 0.011(3) -0.005(3) C19 0.021(4) 0.033(4) 0.036(4) 0.002(3) 0.015(3) -0.005(3) C60 0.029(4) 0.043(4) 0.046(4) 0.023(3) 0.026(4) 0.007(3) C20 0.022(4) 0.035(4) 0.032(3) 0.002(3) 0.016(3) -0.004(3) C21 0.022(4) 0.030(4) 0.020(3) 0.001(3) 0.012(3) 0.002(3) C22 0.019(4) 0.045(4) 0.037(4) 0.007(3) 0.014(3) -0.005(3) C23 0.016(3) 0.035(4) 0.023(3) -0.004(3) 0.012(3) -0.005(3) C24 0.024(4) 0.037(4) 0.025(3) 0.000(3) 0.014(3) -0.004(3) C25 0.023(4) 0.029(4) 0.021(3) -0.003(3) 0.010(3) -0.002(3) C26 0.026(4) 0.029(4) 0.015(3) -0.002(3) 0.006(3) -0.009(3) O9 0.016(2) 0.048(3) 0.021(2) 0.0079(19) 0.0065(19) -0.002(2) S2 0.0201(9) 0.0402(10) 0.0294(9) 0.0085(7) 0.0125(7) -0.0019(8) O10 0.031(3) 0.034(3) 0.038(3) 0.007(2) 0.008(2) -0.007(2) O11 0.032(3) 0.066(3) 0.029(2) 0.011(2) 0.020(2) 0.006(2) O12 0.019(2) 0.033(2) 0.021(2) -0.0030(18) 0.0091(19) -0.0084(19) O13 0.025(3) 0.045(3) 0.023(2) -0.010(2) 0.009(2) -0.014(2) C27 0.017(3) 0.039(4) 0.019(3) 0.003(3) 0.004(3) -0.007(3) C28 0.022(3) 0.031(4) 0.019(3) 0.000(3) 0.010(3) 0.000(3) C29 0.022(3) 0.036(4) 0.020(3) -0.003(3) 0.010(3) 0.001(3) C30 0.014(3) 0.042(4) 0.023(3) 0.006(3) 0.006(3) -0.001(3) C31 0.025(4) 0.037(4) 0.027(3) 0.002(3) 0.017(3) 0.007(3) C32 0.016(3) 0.038(4) 0.026(3) 0.001(3) 0.010(3) -0.006(3) C33 0.022(3) 0.026(3) 0.025(3) 0.003(3) 0.017(3) 0.004(3) C34 0.020(3) 0.032(4) 0.025(3) 0.003(3) 0.013(3) 0.003(3) C35 0.024(4) 0.037(4) 0.024(3) -0.001(3) 0.012(3) 0.009(3) C36 0.030(4) 0.026(3) 0.026(3) 0.005(3) 0.018(3) 0.006(3) C37 0.035(4) 0.034(4) 0.024(3) 0.010(3) 0.020(3) 0.014(3) C38 0.020(3) 0.034(4) 0.019(3) -0.003(3) 0.006(3) 0.005(3) C39 0.032(4) 0.028(4) 0.022(3) 0.011(3) 0.011(3) 0.018(3) C40 0.043(4) 0.024(4) 0.020(3) -0.011(3) 0.018(3) -0.018(3) O14 0.043(3) 0.039(3) 0.048(3) 0.004(2) 0.035(3) 0.002(2) S3 0.0279(9) 0.0358(10) 0.0395(9) 0.0008(7) 0.0248(8) 0.0020(8) O24 0.028(3) 0.048(3) 0.057(3) 0.006(2) 0.023(2) 0.011(2) O15 0.044(3) 0.033(3) 0.025(2) -0.002(2) 0.016(2) -0.020(2) O16 0.032(3) 0.038(3) 0.025(2) -0.0045(19) 0.018(2) -0.018(2) O17 0.023(2) 0.034(2) 0.018(2) 0.0030(18) 0.0110(19) -0.009(2) O18 0.034(3) 0.048(3) 0.029(3) 0.000(2) 0.015(2) -0.002(2) C41 0.056(4) 0.061(4) 0.039(3) 0.013(3) 0.027(3) 0.026(3) N1 0.100(5) 0.060(4) 0.042(3) -0.005(3) 0.026(3) 0.022(4) C42 0.169(7) 0.135(7) 0.130(7) -0.001(5) 0.067(5) 0.025(5) C43 0.065(7) 0.041(5) 0.128(9) -0.002(6) 0.008(7) -0.003(5) O19 0.081(4) 0.045(3) 0.136(4) 0.016(3) 0.065(3) 0.014(3) C44 0.121(11) 0.068(8) 0.117(10) -0.022(7) 0.053(8) -0.036(8) N2 0.152(9) 0.035(5) 0.088(6) 0.006(4) 0.048(6) -0.017(5) C45 0.113(10) 0.149(12) 0.054(6) 0.008(7) 0.024(7) 0.054(9) C46 0.160(14) 0.090(10) 0.123(11) 0.014(8) 0.058(10) -0.017(9) O20 0.031(3) 0.036(3) 0.032(2) -0.001(2) 0.015(2) -0.016(2) C47 0.070(6) 0.069(6) 0.043(5) -0.016(4) 0.038(5) -0.011(5) N3 0.048(4) 0.029(4) 0.058(4) -0.013(3) 0.030(3) -0.007(3) C48 0.134(11) 0.060(6) 0.177(12) -0.057(7) 0.113(10) -0.051(7) C49 0.036(5) 0.085(7) 0.047(5) -0.007(4) 0.013(4) 0.004(4) O21 0.043(3) 0.057(3) 0.046(3) -0.009(2) 0.018(3) -0.025(3) C50 0.044(5) 0.043(4) 0.043(4) -0.007(3) 0.028(4) -0.017(4) N4 0.022(3) 0.040(3) 0.031(3) -0.004(3) 0.012(3) -0.005(3) C51 0.026(4) 0.064(6) 0.063(5) -0.004(4) 0.009(4) -0.003(4) C52 0.054(5) 0.047(5) 0.046(4) -0.013(4) 0.022(4) 0.000(4) O22 0.108(4) 0.054(3) 0.037(3) 0.005(2) 0.034(3) 0.024(3) C53 0.135(9) 0.052(6) 0.034(4) 0.005(4) 0.042(5) 0.036(6) N5 0.063(4) 0.055(4) 0.029(3) 0.005(3) 0.023(3) 0.020(4) C54 0.059(6) 0.079(7) 0.047(5) -0.012(4) 0.026(4) 0.006(5) C55 0.094(7) 0.065(6) 0.041(5) -0.016(4) 0.028(5) 0.010(5) O23 0.232(8) 0.242(8) 0.214(7) -0.004(5) 0.115(5) 0.015(5) C56 0.239(12) 0.243(13) 0.245(12) 0.008(5) 0.110(7) 0.003(5) N6 0.117(11) 0.158(12) 0.141(10) 0.057(9) 0.027(9) -0.015(10) C57 0.22(2) 0.24(2) 0.30(3) 0.16(2) 0.18(2) 0.087(19) C58 0.199(9) 0.184(9) 0.190(9) -0.022(5) 0.087(6) 0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O8 2.372(6) . ? Ce1 O2 2.428(5) . ? Ce1 O3 2.480(6) . ? Ce1 O4 2.483(4) . ? Ce1 O15 2.486(5) . ? Ce1 O19 2.491(6) . ? Ce1 O7 2.499(4) . ? Ce1 O22 2.625(5) . ? Ce2 O16 2.422(4) . ? Ce2 O17 2.469(4) . ? Ce2 O1 2.478(4) . ? Ce2 O12 2.497(4) . ? Ce2 O13 2.522(4) . ? Ce2 O18 2.546(5) . ? Ce2 O20 2.553(4) . ? Ce2 O9 2.568(4) . ? Ce2 O17 2.812(4) 3_575 ? Ce2 C26 3.052(6) . ? O1 C1 1.261(7) . ? O2 C1 1.265(7) . ? C1 C2 1.513(8) . ? C2 C4 1.392(9) . ? C2 C3 1.395(9) . ? C3 C59 1.386(8) . ? C4 C5 1.389(9) . ? C59 C6 1.380(9) . ? C5 C6 1.394(9) . ? C5 S1 1.770(7) . ? C6 C7 1.488(9) . ? C7 C9 1.388(9) . ? C7 C8 1.410(9) . ? C8 C10 1.366(9) . ? C8 S1 1.773(7) . ? C9 C11 1.398(8) . ? C10 C12 1.409(9) . ? C11 C12 1.376(9) . ? C12 C13 1.505(10) . ? C13 O4 1.227(10) 4_586 ? C13 O3 1.265(10) 2_655 ? O3 C13 1.265(10) 2_645 ? O4 C13 1.227(10) 4_585 ? S1 O6 1.433(5) . ? S1 O5 1.448(6) . ? O7 C14 1.246(8) . ? O8 C14 1.239(8) 3_675 ? C14 O8 1.239(8) 3_675 ? C14 C15 1.504(9) 4_686 ? C15 C16 1.392(9) . ? C15 C17 1.400(9) . ? C15 C14 1.504(9) 4_485 ? C16 C60 1.398(9) . ? C17 C18 1.373(9) . ? C18 C19 1.394(8) . ? C18 S2 1.780(6) . ? C19 C60 1.402(9) . ? C19 C20 1.466(9) . ? C20 C22 1.389(9) . ? C20 C21 1.408(8) . ? C21 C23 1.364(8) . ? C21 S2 1.788(6) . ? C22 C24 1.378(9) . ? C23 C25 1.405(8) . ? C24 C25 1.400(9) . ? C25 C26 1.507(8) . ? C26 O9 1.255(7) . ? C26 O17 1.280(7) 3_575 ? S2 O11 1.430(5) . ? S2 O10 1.453(5) . ? O12 C27 1.247(7) . ? O13 C27 1.266(7) 3_575 ? C27 O13 1.266(7) 3_575 ? C27 C28 1.520(9) . ? C28 C30 1.386(8) . ? C28 C29 1.403(8) . ? C29 C32 1.384(8) . ? C30 C31 1.385(9) . ? C31 C33 1.422(8) . ? C31 S3 1.771(6) . ? C32 C33 1.386(8) . ? C33 C34 1.479(8) . ? C34 C35 1.392(9) . ? C34 C36 1.411(8) . ? C35 C38 1.411(8) . ? C36 C37 1.376(8) . ? C36 S3 1.769(6) . ? C37 C39 1.398(9) . ? C38 C39 1.405(9) . ? C39 C40 1.514(8) 4_586 ? C40 O16 1.254(7) . ? C40 O15 1.257(8) . ? C40 C39 1.514(8) 4_585 ? O14 S3 1.434(5) . ? S3 O24 1.451(5) . ? O17 C26 1.280(7) 3_575 ? O17 Ce2 2.812(4) 3_575 ? O18 C41 1.182(8) . ? C41 N1 1.272(10) . ? N1 C43 1.416(12) . ? N1 C42 1.449(14) . ? O19 C44 1.200(12) . ? C44 N2 1.343(13) . ? N2 C45 1.367(13) . ? N2 C46 1.453(15) . ? O20 C47 1.216(9) . ? C47 N3 1.325(10) . ? N3 C48 1.432(10) . ? N3 C49 1.451(9) . ? O21 C50 1.229(8) . ? C50 N4 1.329(8) . ? N4 C52 1.440(8) . ? N4 C51 1.444(9) . ? O22 C53 1.253(9) . ? C53 N5 1.319(9) . ? N5 C54 1.444(10) . ? N5 C55 1.454(9) . ? O23 C56 1.28(3) . ? C56 N6 1.40(3) . ? N6 C58 1.413(19) . ? N6 C57 1.52(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Ce1 O2 148.0(2) . . ? O8 Ce1 O3 69.6(2) . . ? O2 Ce1 O3 142.29(17) . . ? O8 Ce1 O4 85.9(3) . . ? O2 Ce1 O4 78.3(2) . . ? O3 Ce1 O4 119.1(2) . . ? O8 Ce1 O15 70.6(2) . . ? O2 Ce1 O15 78.58(14) . . ? O3 Ce1 O15 135.98(18) . . ? O4 Ce1 O15 75.45(15) . . ? O8 Ce1 O19 80.5(3) . . ? O2 Ce1 O19 99.65(19) . . ? O3 Ce1 O19 80.9(2) . . ? O4 Ce1 O19 150.0(2) . . ? O15 Ce1 O19 74.80(19) . . ? O8 Ce1 O7 121.1(2) . . ? O2 Ce1 O7 79.10(14) . . ? O3 Ce1 O7 77.2(2) . . ? O4 Ce1 O7 69.54(15) . . ? O15 Ce1 O7 141.49(14) . . ? O19 Ce1 O7 140.0(2) . . ? O8 Ce1 O22 138.3(2) . . ? O2 Ce1 O22 69.23(17) . . ? O3 Ce1 O22 75.3(2) . . ? O4 Ce1 O22 131.71(18) . . ? O15 Ce1 O22 128.47(18) . . ? O19 Ce1 O22 72.4(2) . . ? O7 Ce1 O22 69.95(17) . . ? O16 Ce2 O17 145.24(15) . . ? O16 Ce2 O1 88.67(13) . . ? O17 Ce2 O1 87.51(13) . . ? O16 Ce2 O12 141.40(13) . . ? O17 Ce2 O12 71.73(13) . . ? O1 Ce2 O12 80.97(14) . . ? O16 Ce2 O13 81.31(14) . . ? O17 Ce2 O13 78.52(13) . . ? O1 Ce2 O13 137.66(15) . . ? O12 Ce2 O13 129.69(14) . . ? O16 Ce2 O18 74.61(14) . . ? O17 Ce2 O18 71.57(14) . . ? O1 Ce2 O18 70.41(15) . . ? O12 Ce2 O18 133.82(13) . . ? O13 Ce2 O18 67.27(14) . . ? O16 Ce2 O20 71.45(14) . . ? O17 Ce2 O20 138.56(13) . . ? O1 Ce2 O20 71.46(14) . . ? O12 Ce2 O20 69.99(14) . . ? O13 Ce2 O20 140.07(13) . . ? O18 Ce2 O20 128.68(15) . . ? O16 Ce2 O9 81.62(14) . . ? O17 Ce2 O9 121.36(13) . . ? O1 Ce2 O9 139.97(14) . . ? O12 Ce2 O9 82.88(13) . . ? O13 Ce2 O9 79.17(14) . . ? O18 Ce2 O9 141.11(13) . . ? O20 Ce2 O9 68.62(14) . . ? O16 Ce2 O17 122.79(13) . 3_575 ? O17 Ce2 O17 72.78(14) . 3_575 ? O1 Ce2 O17 146.64(12) . 3_575 ? O12 Ce2 O17 67.54(12) . 3_575 ? O13 Ce2 O17 65.33(13) . 3_575 ? O18 Ce2 O17 124.79(13) . 3_575 ? O20 Ce2 O17 105.89(13) . 3_575 ? O9 Ce2 O17 48.62(12) . 3_575 ? O16 Ce2 C26 102.54(15) . . ? O17 Ce2 C26 97.50(15) . . ? O1 Ce2 C26 150.61(15) . . ? O12 Ce2 C26 73.32(14) . . ? O13 Ce2 C26 71.47(16) . . ? O18 Ce2 C26 138.61(15) . . ? O20 Ce2 C26 86.31(15) . . ? O9 Ce2 C26 23.85(14) . . ? O17 Ce2 C26 24.78(14) 3_575 . ? C1 O1 Ce2 133.6(4) . . ? C1 O2 Ce1 145.8(5) . . ? O1 C1 O2 125.1(6) . . ? O1 C1 C2 117.7(6) . . ? O2 C1 C2 117.2(6) . . ? C4 C2 C3 120.3(6) . . ? C4 C2 C1 118.6(6) . . ? C3 C2 C1 121.1(6) . . ? C59 C3 C2 121.6(6) . . ? C5 C4 C2 117.1(6) . . ? C6 C59 C3 118.6(6) . . ? C4 C5 C6 122.8(6) . . ? C4 C5 S1 125.6(5) . . ? C6 C5 S1 111.6(5) . . ? C59 C6 C5 119.4(6) . . ? C59 C6 C7 128.4(6) . . ? C5 C6 C7 112.2(6) . . ? C9 C7 C8 118.5(6) . . ? C9 C7 C6 128.4(6) . . ? C8 C7 C6 113.0(6) . . ? C10 C8 C7 123.5(6) . . ? C10 C8 S1 126.1(5) . . ? C7 C8 S1 110.3(5) . . ? C7 C9 C11 118.2(6) . . ? C8 C10 C12 117.4(6) . . ? C12 C11 C9 122.5(6) . . ? C11 C12 C10 119.9(6) . . ? C11 C12 C13 119.1(7) . . ? C10 C12 C13 121.0(6) . . ? O4 C13 O3 124.5(8) 4_586 2_655 ? O4 C13 C12 119.2(7) 4_586 . ? O3 C13 C12 116.3(9) 2_655 . ? C13 O3 Ce1 168.6(5) 2_645 . ? C13 O4 Ce1 115.0(5) 4_585 . ? O6 S1 O5 117.0(4) . . ? O6 S1 C5 111.0(3) . . ? O5 S1 C5 111.1(3) . . ? O6 S1 C8 111.3(3) . . ? O5 S1 C8 111.1(4) . . ? C5 S1 C8 92.8(3) . . ? C14 O7 Ce1 129.0(4) . . ? C14 O8 Ce1 159.0(6) 3_675 . ? O8 C14 O7 123.9(7) 3_675 . ? O8 C14 C15 116.8(7) 3_675 4_686 ? O7 C14 C15 119.2(6) . 4_686 ? C16 C15 C17 120.0(6) . . ? C16 C15 C14 120.6(6) . 4_485 ? C17 C15 C14 119.3(5) . 4_485 ? C15 C16 C60 121.3(6) . . ? C18 C17 C15 117.8(6) . . ? C17 C18 C19 123.6(6) . . ? C17 C18 S2 126.3(5) . . ? C19 C18 S2 110.0(5) . . ? C18 C19 C60 118.3(6) . . ? C18 C19 C20 113.8(6) . . ? C60 C19 C20 127.8(6) . . ? C16 C60 C19 118.8(6) . . ? C22 C20 C21 118.7(6) . . ? C22 C20 C19 128.1(6) . . ? C21 C20 C19 113.2(5) . . ? C23 C21 C20 122.3(6) . . ? C23 C21 S2 128.0(5) . . ? C20 C21 S2 109.6(4) . . ? C24 C22 C20 119.7(6) . . ? C21 C23 C25 118.7(6) . . ? C22 C24 C25 121.2(6) . . ? C24 C25 C23 119.4(6) . . ? C24 C25 C26 120.9(5) . . ? C23 C25 C26 119.8(5) . . ? O9 C26 O17 122.8(6) . 3_575 ? O9 C26 C25 118.9(5) . . ? O17 C26 C25 118.2(6) 3_575 . ? O9 C26 Ce2 55.9(3) . . ? O17 C26 Ce2 67.1(3) 3_575 . ? C25 C26 Ce2 174.2(4) . . ? C26 O9 Ce2 100.3(3) . . ? O11 S2 O10 117.7(3) . . ? O11 S2 C18 111.2(3) . . ? O10 S2 C18 110.0(3) . . ? O11 S2 C21 112.6(3) . . ? O10 S2 C21 109.8(3) . . ? C18 S2 C21 92.8(3) . . ? C27 O12 Ce2 142.1(4) . . ? C27 O13 Ce2 134.2(4) 3_575 . ? O12 C27 O13 126.5(6) . 3_575 ? O12 C27 C28 117.6(5) . . ? O13 C27 C28 116.0(6) 3_575 . ? C30 C28 C29 119.2(6) . . ? C30 C28 C27 120.9(6) . . ? C29 C28 C27 119.9(5) . . ? C32 C29 C28 121.9(6) . . ? C31 C30 C28 119.0(6) . . ? C30 C31 C33 122.0(6) . . ? C30 C31 S3 127.5(5) . . ? C33 C31 S3 110.5(4) . . ? C29 C32 C33 119.6(6) . . ? C32 C33 C31 118.2(5) . . ? C32 C33 C34 129.4(6) . . ? C31 C33 C34 112.5(5) . . ? C35 C34 C36 117.5(6) . . ? C35 C34 C33 129.7(6) . . ? C36 C34 C33 112.8(5) . . ? C34 C35 C38 120.0(6) . . ? C37 C36 C34 124.0(6) . . ? C37 C36 S3 125.1(5) . . ? C34 C36 S3 110.9(4) . . ? C36 C37 C39 117.7(6) . . ? C39 C38 C35 120.3(6) . . ? C37 C39 C38 120.4(6) . . ? C37 C39 C40 118.0(6) . 4_586 ? C38 C39 C40 121.5(6) . 4_586 ? O16 C40 O15 125.2(6) . . ? O16 C40 C39 117.5(6) . 4_585 ? O15 C40 C39 117.3(6) . 4_585 ? O14 S3 O24 117.6(3) . . ? O14 S3 C36 111.8(3) . . ? O24 S3 C36 109.5(3) . . ? O14 S3 C31 111.5(3) . . ? O24 S3 C31 110.6(3) . . ? C36 S3 C31 93.1(3) . . ? C40 O15 Ce1 153.6(4) . . ? C40 O16 Ce2 137.5(4) . . ? C26 O17 Ce2 164.1(4) 3_575 . ? C26 O17 Ce2 88.2(4) 3_575 3_575 ? Ce2 O17 Ce2 107.22(14) . 3_575 ? C41 O18 Ce2 133.1(5) . . ? O18 C41 N1 125.7(8) . . ? C41 N1 C43 120.8(8) . . ? C41 N1 C42 120.7(10) . . ? C43 N1 C42 118.5(9) . . ? C44 O19 Ce1 136.8(8) . . ? O19 C44 N2 121.1(12) . . ? C44 N2 C45 122.6(11) . . ? C44 N2 C46 119.3(12) . . ? C45 N2 C46 117.9(9) . . ? C47 O20 Ce2 169.3(4) . . ? O20 C47 N3 128.2(9) . . ? C47 N3 C48 124.6(8) . . ? C47 N3 C49 118.6(7) . . ? C48 N3 C49 116.5(7) . . ? O21 C50 N4 125.5(7) . . ? C50 N4 C52 121.3(6) . . ? C50 N4 C51 121.7(6) . . ? C52 N4 C51 116.9(6) . . ? C53 O22 Ce1 123.8(5) . . ? O22 C53 N5 124.9(8) . . ? C53 N5 C54 121.1(7) . . ? C53 N5 C55 121.8(7) . . ? C54 N5 C55 116.9(6) . . ? O23 C56 N6 103(2) . . ? C56 N6 C58 126(2) . . ? C56 N6 C57 117(2) . . ? C58 N6 C57 114.4(15) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 23.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.599 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.094 # 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 0.022 0.000 0.500 887 285 ' ' 2 0.351 0.500 0.000 887 284 ' ' _platon_squeeze_details ; ; # Attachment 'Revised_Ce-3.cif' data_Ce3 _database_code_depnum_ccdc_archive 'CCDC 736838' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H12 Ce O12 S2' _chemical_formula_weight 744.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.5890 1.7358 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 25.0566(12) _cell_length_b 25.0566(12) _cell_length_c 29.944(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16281.3(19) _cell_formula_units_Z 9 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 4.75 _cell_measurement_theta_max 12.81 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3294 _exptl_absorpt_coefficient_mu 0.379 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6517 _exptl_absorpt_correction_T_max 0.7436 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.41382 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 52820 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 4.75 _diffrn_reflns_theta_max 12.81 _reflns_number_total 4088 _reflns_number_gt 3031 _reflns_threshold_expression >2sigma(I) _computing_data_collection APEX2 _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4088 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2168 _refine_ls_wR_factor_gt 0.2104 _refine_ls_goodness_of_fit_ref 1.339 _refine_ls_restrained_S_all 1.339 _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 Ce1 Ce 0.3333 0.6667 0.29962(3) 0.0295(4) Uani 1 3 d S . . Ce2 Ce 0.3333 0.6667 0.1667 0.0241(4) Uani 1 6 d S . . S1 S 0.12773(12) 0.30871(9) 0.22881(9) 0.0576(8) Uani 1 1 d . . . O1 O 0.2521(2) 0.5530(2) 0.18889(19) 0.0352(13) Uani 1 1 d . . . O2 O 0.3274(2) 0.5981(2) 0.23817(17) 0.0316(12) Uani 1 1 d . . . O3 O 0.0355(2) 0.0868(2) 0.31112(19) 0.0437(14) Uani 1 1 d . . . O4 O 0.1069(2) 0.0948(2) 0.35788(19) 0.0388(13) Uani 1 1 d . . . O5 O 0.1328(4) 0.2904(3) 0.1834(2) 0.085(2) Uani 1 1 d . . . O6 O 0.0723(3) 0.3098(3) 0.2414(3) 0.076(2) Uani 1 1 d . . . C1 C 0.2815(3) 0.5492(3) 0.2209(3) 0.0276(17) Uani 1 1 d . . . C2 C 0.2639(3) 0.4887(3) 0.2408(3) 0.0294(17) Uani 1 1 d . . . C3 C 0.2991(3) 0.4814(3) 0.2730(3) 0.036(2) Uani 1 1 d . . . H3 H 0.3350 0.5158 0.2830 0.044 Uiso 1 1 calc R . . C4 C 0.2820(4) 0.4239(4) 0.2910(3) 0.043(2) Uani 1 1 d . . . H4 H 0.3060 0.4196 0.3129 0.051 Uiso 1 1 calc R . . C5 C 0.2101(4) 0.4366(4) 0.2251(3) 0.043(2) Uani 1 1 d . . . H5 H 0.1856 0.4408 0.2037 0.052 Uiso 1 1 calc R . . C6 C 0.1941(4) 0.3792(3) 0.2418(3) 0.046(2) Uani 1 1 d . . . C7 C 0.2283(3) 0.3725(3) 0.2755(3) 0.037(2) Uani 1 1 d . . . C8 C 0.1997(4) 0.3072(3) 0.2909(3) 0.0368(19) Uani 1 1 d . . . C9 C 0.1452(4) 0.2687(3) 0.2691(3) 0.040(2) Uani 1 1 d . . . C10 C 0.2213(4) 0.2818(3) 0.3243(3) 0.040(2) Uani 1 1 d . . . H10 H 0.2588 0.3059 0.3386 0.049 Uiso 1 1 calc R . . C11 C 0.1086(4) 0.2061(4) 0.2799(3) 0.049(2) Uani 1 1 d . . . H11 H 0.0718 0.1813 0.2649 0.059 Uiso 1 1 calc R . . C12 C 0.1847(4) 0.2209(4) 0.3344(3) 0.040(2) Uani 1 1 d . . . H12 H 0.1977 0.2042 0.3567 0.047 Uiso 1 1 calc R . . C13 C 0.1284(4) 0.1822(3) 0.3131(2) 0.0349(19) Uani 1 1 d . . . C14 C 0.0885(4) 0.1169(4) 0.3284(3) 0.040(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0192(4) 0.0192(4) 0.0500(6) 0.000 0.000 0.0096(2) Ce2 0.0150(4) 0.0150(4) 0.0422(7) 0.000 0.000 0.0075(2) S1 0.0560(16) 0.0220(12) 0.0684(18) 0.0042(11) -0.0222(13) -0.0004(11) O1 0.026(3) 0.016(3) 0.058(4) -0.004(2) -0.006(3) 0.006(2) O2 0.021(3) 0.022(3) 0.055(3) -0.001(2) 0.006(2) 0.014(2) O3 0.026(3) 0.040(3) 0.061(4) 0.002(3) -0.007(3) 0.013(3) O4 0.032(3) 0.026(3) 0.057(4) 0.008(3) -0.003(3) 0.014(2) O5 0.123(6) 0.043(4) 0.058(5) -0.002(3) -0.022(4) 0.017(4) O6 0.054(4) 0.032(3) 0.117(6) 0.023(4) -0.037(4) 0.003(3) C1 0.019(4) 0.026(4) 0.035(5) 0.005(3) 0.007(4) 0.009(4) C2 0.021(4) 0.021(4) 0.043(5) 0.002(3) -0.007(3) 0.008(3) C3 0.014(4) 0.015(4) 0.071(6) -0.008(4) -0.003(4) 0.000(3) C4 0.036(5) 0.037(5) 0.057(5) -0.006(4) -0.010(4) 0.019(4) C5 0.031(5) 0.038(5) 0.051(5) 0.013(4) 0.002(4) 0.010(4) C6 0.023(4) 0.015(4) 0.083(6) 0.009(4) -0.001(4) -0.003(3) C7 0.026(4) 0.016(4) 0.069(6) -0.003(4) 0.005(4) 0.011(4) C8 0.035(5) 0.024(4) 0.050(5) 0.001(4) 0.004(4) 0.014(4) C9 0.032(5) 0.016(4) 0.061(6) 0.005(4) -0.001(4) 0.003(4) C10 0.030(4) 0.026(5) 0.065(6) 0.006(4) 0.002(4) 0.013(4) C11 0.041(5) 0.041(5) 0.056(6) -0.014(4) -0.009(4) 0.013(4) C12 0.037(5) 0.035(5) 0.058(5) 0.010(4) 0.005(4) 0.027(4) C13 0.050(5) 0.029(4) 0.030(4) 0.009(3) 0.002(4) 0.023(4) C14 0.023(5) 0.028(4) 0.073(6) -0.012(4) 0.002(4) 0.016(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 Ce1 O2 2.470(5) . ? Ce1 O2 2.471(5) 3_565 ? Ce1 O2 2.471(5) 2_665 ? Ce1 O3 2.527(5) 18 ? Ce1 O3 2.527(6) 17 ? Ce1 O3 2.527(5) 16 ? Ce1 O4 2.555(5) 18 ? Ce1 O4 2.555(5) 16 ? Ce1 O4 2.555(5) 17 ? Ce1 C14 2.888(8) 18 ? Ce1 C14 2.888(8) 16 ? Ce1 C14 2.888(8) 17 ? Ce2 O1 2.626(5) 15 ? Ce2 O1 2.626(5) 3_565 ? Ce2 O1 2.626(5) 2_665 ? Ce2 O1 2.626(5) 13_565 ? Ce2 O1 2.626(5) . ? Ce2 O1 2.626(5) 14_455 ? Ce2 O2 2.702(5) 15 ? Ce2 O2 2.702(5) 14_455 ? Ce2 O2 2.702(5) 3_565 ? Ce2 O2 2.702(5) 2_665 ? Ce2 O2 2.702(5) 13_565 ? Ce2 O2 2.702(5) . ? S1 O6 1.452(8) . ? S1 O5 1.460(8) . ? S1 C9 1.757(8) . ? S1 C6 1.761(8) . ? O1 C1 1.241(9) . ? O2 C1 1.296(9) . ? O3 C14 1.264(10) . ? O3 Ce1 2.527(5) 16 ? O4 C14 1.247(10) . ? O4 Ce1 2.555(5) 16 ? C1 C2 1.476(10) . ? C2 C3 1.380(11) . ? C2 C5 1.408(11) . ? C3 C4 1.392(11) . ? C4 C7 1.396(11) . ? C5 C6 1.378(11) . ? C6 C7 1.389(12) . ? C7 C8 1.494(11) . ? C8 C9 1.381(11) . ? C8 C10 1.427(12) . ? C9 C11 1.404(12) . ? C10 C12 1.364(11) . ? C11 C13 1.376(12) . ? C12 C13 1.403(12) . ? C13 C14 1.499(11) . ? C14 Ce1 2.888(8) 16 ? 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 Ce1 O2 70.59(18) . 3_565 ? O2 Ce1 O2 70.59(18) . 2_665 ? O2 Ce1 O2 70.59(18) 3_565 2_665 ? O2 Ce1 O3 150.89(17) . 18 ? O2 Ce1 O3 91.30(17) 3_565 18 ? O2 Ce1 O3 125.76(17) 2_665 18 ? O2 Ce1 O3 125.75(17) . 17 ? O2 Ce1 O3 150.90(17) 3_565 17 ? O2 Ce1 O3 91.29(17) 2_665 17 ? O3 Ce1 O3 80.88(19) 18 17 ? O2 Ce1 O3 91.29(17) . 16 ? O2 Ce1 O3 125.76(17) 3_565 16 ? O2 Ce1 O3 150.89(17) 2_665 16 ? O3 Ce1 O3 80.88(19) 18 16 ? O3 Ce1 O3 80.88(19) 17 16 ? O2 Ce1 O4 138.00(17) . 18 ? O2 Ce1 O4 76.28(16) 3_565 18 ? O2 Ce1 O4 74.58(17) 2_665 18 ? O3 Ce1 O4 51.29(17) 18 18 ? O3 Ce1 O4 77.02(17) 17 18 ? O3 Ce1 O4 129.55(18) 16 18 ? O2 Ce1 O4 76.28(16) . 16 ? O2 Ce1 O4 74.58(17) 3_565 16 ? O2 Ce1 O4 137.99(17) 2_665 16 ? O3 Ce1 O4 77.01(17) 18 16 ? O3 Ce1 O4 129.55(18) 17 16 ? O3 Ce1 O4 51.29(17) 16 16 ? O4 Ce1 O4 118.87(5) 18 16 ? O2 Ce1 O4 74.57(17) . 17 ? O2 Ce1 O4 137.99(17) 3_565 17 ? O2 Ce1 O4 76.28(16) 2_665 17 ? O3 Ce1 O4 129.54(18) 18 17 ? O3 Ce1 O4 51.29(17) 17 17 ? O3 Ce1 O4 77.01(17) 16 17 ? O4 Ce1 O4 118.86(5) 18 17 ? O4 Ce1 O4 118.86(5) 16 17 ? O2 Ce1 C14 151.62(19) . 18 ? O2 Ce1 C14 81.03(19) 3_565 18 ? O2 Ce1 C14 99.9(2) 2_665 18 ? O3 Ce1 C14 25.9(2) 18 18 ? O3 Ce1 C14 79.89(18) 17 18 ? O3 Ce1 C14 106.2(2) 16 18 ? O4 Ce1 C14 25.6(2) 18 18 ? O4 Ce1 C14 97.14(19) 16 18 ? O4 Ce1 C14 130.46(18) 17 18 ? O2 Ce1 C14 81.03(19) . 16 ? O2 Ce1 C14 99.9(2) 3_565 16 ? O2 Ce1 C14 151.62(19) 2_665 16 ? O3 Ce1 C14 79.89(19) 18 16 ? O3 Ce1 C14 106.2(2) 17 16 ? O3 Ce1 C14 25.9(2) 16 16 ? O4 Ce1 C14 130.46(18) 18 16 ? O4 Ce1 C14 25.6(2) 16 16 ? O4 Ce1 C14 97.13(19) 17 16 ? C14 Ce1 C14 105.0(2) 18 16 ? O2 Ce1 C14 99.8(2) . 17 ? O2 Ce1 C14 151.6(2) 3_565 17 ? O2 Ce1 C14 81.0(2) 2_665 17 ? O3 Ce1 C14 106.2(2) 18 17 ? O3 Ce1 C14 25.9(2) 17 17 ? O3 Ce1 C14 79.88(18) 16 17 ? O4 Ce1 C14 97.14(19) 18 17 ? O4 Ce1 C14 130.46(18) 16 17 ? O4 Ce1 C14 25.6(2) 17 17 ? C14 Ce1 C14 105.0(2) 18 17 ? C14 Ce1 C14 105.0(2) 16 17 ? O1 Ce2 O1 180.00(18) 15 3_565 ? O1 Ce2 O1 66.19(10) 15 2_665 ? O1 Ce2 O1 113.81(10) 3_565 2_665 ? O1 Ce2 O1 113.81(10) 15 13_565 ? O1 Ce2 O1 66.19(10) 3_565 13_565 ? O1 Ce2 O1 66.19(10) 2_665 13_565 ? O1 Ce2 O1 66.19(10) 15 . ? O1 Ce2 O1 113.81(10) 3_565 . ? O1 Ce2 O1 113.81(10) 2_665 . ? O1 Ce2 O1 180.0 13_565 . ? O1 Ce2 O1 113.81(10) 15 14_455 ? O1 Ce2 O1 66.19(10) 3_565 14_455 ? O1 Ce2 O1 179.997(1) 2_665 14_455 ? O1 Ce2 O1 113.81(10) 13_565 14_455 ? O1 Ce2 O1 66.19(10) . 14_455 ? O1 Ce2 O2 48.94(16) 15 15 ? O1 Ce2 O2 131.06(16) 3_565 15 ? O1 Ce2 O2 69.42(15) 2_665 15 ? O1 Ce2 O2 72.72(15) 13_565 15 ? O1 Ce2 O2 107.28(15) . 15 ? O1 Ce2 O2 110.58(15) 14_455 15 ? O1 Ce2 O2 72.72(15) 15 14_455 ? O1 Ce2 O2 107.28(15) 3_565 14_455 ? O1 Ce2 O2 131.06(16) 2_665 14_455 ? O1 Ce2 O2 110.58(15) 13_565 14_455 ? O1 Ce2 O2 69.42(15) . 14_455 ? O1 Ce2 O2 48.94(16) 14_455 14_455 ? O2 Ce2 O2 63.78(16) 15 14_455 ? O1 Ce2 O2 131.06(16) 15 3_565 ? O1 Ce2 O2 48.94(16) 3_565 3_565 ? O1 Ce2 O2 110.58(15) 2_665 3_565 ? O1 Ce2 O2 107.28(15) 13_565 3_565 ? O1 Ce2 O2 72.72(15) . 3_565 ? O1 Ce2 O2 69.42(15) 14_455 3_565 ? O2 Ce2 O2 180.00(17) 15 3_565 ? O2 Ce2 O2 116.22(16) 14_455 3_565 ? O1 Ce2 O2 107.28(15) 15 2_665 ? O1 Ce2 O2 72.72(15) 3_565 2_665 ? O1 Ce2 O2 48.94(16) 2_665 2_665 ? O1 Ce2 O2 69.42(15) 13_565 2_665 ? O1 Ce2 O2 110.58(15) . 2_665 ? O1 Ce2 O2 131.06(16) 14_455 2_665 ? O2 Ce2 O2 116.22(16) 15 2_665 ? O2 Ce2 O2 179.997(1) 14_455 2_665 ? O2 Ce2 O2 63.78(16) 3_565 2_665 ? O1 Ce2 O2 110.59(15) 15 13_565 ? O1 Ce2 O2 69.41(15) 3_565 13_565 ? O1 Ce2 O2 107.28(15) 2_665 13_565 ? O1 Ce2 O2 48.94(16) 13_565 13_565 ? O1 Ce2 O2 131.06(16) . 13_565 ? O1 Ce2 O2 72.72(15) 14_455 13_565 ? O2 Ce2 O2 63.78(16) 15 13_565 ? O2 Ce2 O2 63.78(16) 14_455 13_565 ? O2 Ce2 O2 116.22(16) 3_565 13_565 ? O2 Ce2 O2 116.22(16) 2_665 13_565 ? O1 Ce2 O2 69.42(15) 15 . ? O1 Ce2 O2 110.58(15) 3_565 . ? O1 Ce2 O2 72.72(15) 2_665 . ? O1 Ce2 O2 131.06(16) 13_565 . ? O1 Ce2 O2 48.94(16) . . ? O1 Ce2 O2 107.28(15) 14_455 . ? O2 Ce2 O2 116.22(16) 15 . ? O2 Ce2 O2 116.22(16) 14_455 . ? O2 Ce2 O2 63.78(16) 3_565 . ? O2 Ce2 O2 63.78(16) 2_665 . ? O2 Ce2 O2 179.996(1) 13_565 . ? O6 S1 O5 118.8(5) . . ? O6 S1 C9 110.3(4) . . ? O5 S1 C9 111.9(4) . . ? O6 S1 C6 110.9(4) . . ? O5 S1 C6 109.5(5) . . ? C9 S1 C6 92.4(4) . . ? C1 O1 Ce2 96.4(4) . . ? C1 O2 Ce1 132.1(4) . . ? C1 O2 Ce2 91.5(4) . . ? Ce1 O2 Ce2 100.56(15) . . ? C14 O3 Ce1 93.2(5) . 16 ? C14 O4 Ce1 92.3(4) . 16 ? O1 C1 O2 121.0(6) . . ? O1 C1 C2 120.4(7) . . ? O2 C1 C2 118.6(7) . . ? O1 C1 Ce2 59.6(4) . . ? O2 C1 Ce2 63.2(4) . . ? C2 C1 Ce2 167.8(5) . . ? C3 C2 C5 119.3(7) . . ? C3 C2 C1 122.3(6) . . ? C5 C2 C1 118.4(7) . . ? C2 C3 C4 121.5(7) . . ? C3 C4 C7 118.8(7) . . ? C6 C5 C2 119.4(7) . . ? C5 C6 C7 121.0(7) . . ? C5 C6 S1 127.1(7) . . ? C7 C6 S1 111.7(6) . . ? C6 C7 C4 119.9(7) . . ? C6 C7 C8 111.8(7) . . ? C4 C7 C8 128.3(8) . . ? C9 C8 C10 118.9(7) . . ? C9 C8 C7 112.5(7) . . ? C10 C8 C7 128.6(7) . . ? C8 C9 C11 122.4(8) . . ? C8 C9 S1 111.6(5) . . ? C11 C9 S1 125.9(6) . . ? C12 C10 C8 117.5(7) . . ? C13 C11 C9 118.5(8) . . ? C10 C12 C13 123.7(7) . . ? C11 C13 C12 118.9(7) . . ? C11 C13 C14 120.5(8) . . ? C12 C13 C14 120.5(7) . . ? O4 C14 O3 122.4(7) . . ? O4 C14 C13 120.5(7) . . ? O3 C14 C13 117.1(8) . . ? O4 C14 Ce1 62.1(4) . 16 ? O3 C14 Ce1 60.9(4) . 16 ? C13 C14 Ce1 169.6(5) . 16 ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 12.81 _diffrn_measured_fraction_theta_full 0.875 _refine_diff_density_max 1.127 _refine_diff_density_min -1.417 _refine_diff_density_rms 0.155 # 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 -0.012 -0.007 -0.003 11439 5049 ' ' _platon_squeeze_details ; ; # Attachment 'Revised_Dy.cif' data_Dy _database_code_depnum_ccdc_archive 'CCDC 736839' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H59 Dy2 N6 O25 S3' _chemical_formula_weight 1685.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4996(12) _cell_length_b 17.7008(16) _cell_length_c 22.3869(18) _cell_angle_alpha 79.657(7) _cell_angle_beta 80.452(7) _cell_angle_gamma 81.326(8) _cell_volume 4767.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 4432 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 25.08 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1682 _exptl_absorpt_coefficient_mu 1.680 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6400 _exptl_absorpt_correction_T_max 0.9255 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46387 _diffrn_reflns_av_R_equivalents 0.1589 _diffrn_reflns_av_sigmaI/netI 0.2736 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.09 _reflns_number_total 16433 _reflns_number_gt 7474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0869P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16433 _refine_ls_number_parameters 865 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.1711 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.2047 _refine_ls_wR_factor_gt 0.1719 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.865 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.34663(6) 0.97079(4) 0.00208(3) 0.0182(2) Uani 1 1 d . . . Dy2 Dy 1.12882(6) 0.57010(4) 0.48195(3) 0.0178(2) Uani 1 1 d . . . O1 O 0.2871(8) 0.9853(6) -0.0960(4) 0.028(2) Uani 1 1 d U . . O2 O 0.2769(8) 0.8667(6) -0.0410(5) 0.029(3) Uani 1 1 d . . . C1 C 0.2759(12) 0.9153(9) -0.0922(7) 0.027(4) Uani 1 1 d . . . C2 C 0.2656(12) 0.8853(8) -0.1508(7) 0.026(3) Uani 1 1 d . . . C3 C 0.2490(13) 0.9404(8) -0.2034(7) 0.033(4) Uani 1 1 d . . . H3 H 0.2464 0.9927 -0.2017 0.040 Uiso 1 1 calc R . . C4 C 0.2752(12) 0.8067(9) -0.1535(7) 0.027(4) Uani 1 1 d . . . H4 H 0.2884 0.7698 -0.1195 0.032 Uiso 1 1 calc R . . C5 C 0.2644(13) 0.7855(9) -0.2078(7) 0.029(4) Uani 1 1 d . . . C6 C 0.2365(14) 0.9175(9) -0.2574(7) 0.038(4) Uani 1 1 d . . . H6 H 0.2226 0.9542 -0.2915 0.045 Uiso 1 1 calc R . . C7 C 0.2451(14) 0.8387(9) -0.2601(7) 0.035(4) Uani 1 1 d . . . C8 C 0.2322(12) 0.8023(8) -0.3132(7) 0.027(4) Uani 1 1 d . . . C9 C 0.2455(13) 0.7217(9) -0.3001(7) 0.029(4) Uani 1 1 d . . . C10 C 0.2083(13) 0.8377(9) -0.3707(7) 0.033(4) Uani 1 1 d U . . H10 H 0.2007 0.8914 -0.3810 0.040 Uiso 1 1 calc R . . C11 C 0.2331(12) 0.6752(8) -0.3420(7) 0.025(4) Uani 1 1 d . . . H11 H 0.2420 0.6215 -0.3321 0.030 Uiso 1 1 calc R . . C12 C 0.1957(14) 0.7918(8) -0.4129(7) 0.035(4) Uani 1 1 d . . . H12 H 0.1794 0.8152 -0.4515 0.042 Uiso 1 1 calc R . . C13 C 0.2072(11) 0.7112(8) -0.3983(7) 0.026(3) Uani 1 1 d . . . C14 C 0.1915(12) 0.6613(9) -0.4449(7) 0.023(4) Uani 1 1 d U . . O3 O 0.1588(9) 0.6961(6) -0.4949(5) 0.036(3) Uani 1 1 d . . . O4 O 0.2069(9) 0.5900(6) -0.4301(5) 0.030(3) Uani 1 1 d U . . S1 S 0.2800(4) 0.6894(2) -0.22441(19) 0.0330(10) Uani 1 1 d . . . O5 O 0.2004(10) 0.6443(6) -0.1850(5) 0.043(3) Uani 1 1 d . . . O6 O 0.3942(9) 0.6554(6) -0.2276(5) 0.045(3) Uani 1 1 d . . . O7 O 0.5504(8) 0.9326(5) 0.0506(4) 0.023(2) Uani 1 1 d U . . O8 O 0.4119(8) 0.8639(5) 0.0732(5) 0.027(2) Uani 1 1 d . . . C15 C 0.5033(13) 0.8759(8) 0.0813(7) 0.027(4) Uani 1 1 d . . . C16 C 0.5633(12) 0.8240(8) 0.1293(7) 0.027(4) Uani 1 1 d . . . C17 C 0.6587(14) 0.8425(9) 0.1455(7) 0.034(4) Uani 1 1 d . . . H17 H 0.6907 0.8859 0.1253 0.041 Uiso 1 1 calc R . . C18 C 0.5174(15) 0.7585(10) 0.1622(8) 0.048(5) Uani 1 1 d U . . H18 H 0.4542 0.7466 0.1511 0.058 Uiso 1 1 calc R . . C19 C 0.5623(16) 0.7097(11) 0.2113(9) 0.055(5) Uani 1 1 d U . . H19 H 0.5303 0.6667 0.2326 0.066 Uiso 1 1 calc R . . C20 C 0.7034(13) 0.7926(9) 0.1936(7) 0.031(4) Uani 1 1 d . . . C21 C 0.6573(15) 0.7295(9) 0.2261(8) 0.043(5) Uani 1 1 d . . . C22 C 0.7186(15) 0.6876(8) 0.2785(8) 0.037(4) Uani 1 1 d . . . C23 C 0.8099(14) 0.7246(8) 0.2819(7) 0.031(4) Uani 1 1 d . . . C24 C 0.6941(16) 0.6220(10) 0.3202(9) 0.055(6) Uani 1 1 d . . . H24 H 0.6355 0.5966 0.3176 0.066 Uiso 1 1 calc R . . C25 C 0.7619(14) 0.5949(9) 0.3671(8) 0.039(4) Uani 1 1 d . . . H25 H 0.7474 0.5514 0.3959 0.047 Uiso 1 1 calc R . . C26 C 0.8732(14) 0.6997(9) 0.3266(7) 0.033(4) Uani 1 1 d . . . H26 H 0.9311 0.7261 0.3285 0.040 Uiso 1 1 calc R . . C27 C 0.8526(13) 0.6349(8) 0.3697(7) 0.025(4) Uani 1 1 d . . . C28 C 0.9223(13) 0.6054(9) 0.4180(7) 0.027(4) Uani 1 1 d U . . O9 O 0.9033(8) 0.5450(5) 0.4566(4) 0.024(2) Uani 1 1 d . . . O10 O 1.0016(8) 0.6423(6) 0.4189(5) 0.030(3) Uani 1 1 d . . . S2 S 0.8207(4) 0.8064(3) 0.2240(2) 0.0417(12) Uani 1 1 d . . . O11 O 0.7999(11) 0.8747(7) 0.2505(6) 0.061(4) Uani 1 1 d . . . O12 O 0.9209(11) 0.7961(8) 0.1811(6) 0.068(4) Uani 1 1 d . . . O13 O 0.0194(8) 1.3950(5) 0.4420(4) 0.021(2) Uani 1 1 d . . . O14 O 0.1321(8) 1.4863(5) 0.4103(4) 0.023(2) Uani 1 1 d . . . C29 C 0.0959(12) 1.4238(8) 0.4081(6) 0.019(3) Uani 1 1 d . . . C30 C 0.1561(12) 1.3802(8) 0.3567(6) 0.024(3) Uani 1 1 d U . . C31 C 0.1106(12) 1.3195(8) 0.3421(7) 0.025(3) Uani 1 1 d . . . H31 H 0.0448 1.3046 0.3634 0.030 Uiso 1 1 calc R . . C32 C 0.2558(13) 1.3997(9) 0.3261(7) 0.035(4) Uani 1 1 d . . . H32 H 0.2853 1.4396 0.3370 0.042 Uiso 1 1 calc R . . C33 C 0.1678(13) 1.2822(8) 0.2943(7) 0.029(4) Uani 1 1 d . . . C34 C 0.3146(14) 1.3605(9) 0.2784(7) 0.036(4) Uani 1 1 d U . . H34 H 0.3813 1.3746 0.2577 0.044 Uiso 1 1 calc R . . C35 C 0.2689(13) 1.2999(8) 0.2635(7) 0.030(4) Uani 1 1 d . . . C36 C 0.3154(12) 1.2509(8) 0.2156(7) 0.028(4) Uani 1 1 d . . . C37 C 0.2494(12) 1.1954(9) 0.2122(7) 0.032(4) Uani 1 1 d . . . C38 C 0.4123(13) 1.2524(9) 0.1773(7) 0.037(4) Uani 1 1 d . . . H38 H 0.4580 1.2890 0.1780 0.044 Uiso 1 1 calc R . . C39 C 0.2784(13) 1.1410(8) 0.1714(7) 0.029(4) Uani 1 1 d . . . H39 H 0.2320 1.1053 0.1698 0.034 Uiso 1 1 calc R . . C40 C 0.4424(13) 1.1989(8) 0.1371(7) 0.031(4) Uani 1 1 d U . . H40 H 0.5084 1.2007 0.1110 0.037 Uiso 1 1 calc R . . C41 C 0.3771(11) 1.1427(8) 0.1345(6) 0.020(3) Uani 1 1 d U . . C42 C 0.4152(13) 1.0855(8) 0.0893(6) 0.019(3) Uani 1 1 d . . . O15 O 0.3512(8) 1.0389(6) 0.0847(4) 0.025(2) Uani 1 1 d . . . S3 S 0.1263(4) 1.2048(3) 0.2652(2) 0.0342(11) Uani 1 1 d . . . O16 O 0.1208(10) 1.1369(6) 0.3110(5) 0.049(3) Uani 1 1 d . . . O17 O 0.0337(9) 1.2325(7) 0.2322(5) 0.046(3) Uani 1 1 d . . . O18 O 0.4906(8) 0.9078(6) -0.0590(4) 0.027(2) Uani 1 1 d . . . O19 O 0.1936(8) 0.9359(6) 0.0723(5) 0.031(3) Uani 1 1 d . . . O20 O 0.2052(9) 1.0812(6) -0.0071(5) 0.039(3) Uani 1 1 d U . . O21 O 1.3092(9) 0.5014(6) 0.4762(6) 0.042(3) Uani 1 1 d . . . O22 O 1.2348(9) 0.6337(6) 0.3912(6) 0.056(4) Uani 1 1 d . . . C43 C 1.3432(14) 0.4388(10) 0.4646(9) 0.043(5) Uani 1 1 d . . . H43 H 1.2965 0.4008 0.4749 0.052 Uiso 1 1 calc R . . C44 C 0.1678(15) 0.9423(10) 0.1271(9) 0.041(4) Uani 1 1 d . . . C45 C 0.1553(19) 1.1199(13) 0.0311(11) 0.068(6) Uani 1 1 d . . . H45 H 0.1832 1.1144 0.0678 0.082 Uiso 1 1 calc R . . N1 N 0.0666(13) 0.9670(9) 0.1508(7) 0.047(4) Uani 1 1 d . . . N2 N 1.4447(12) 0.4198(8) 0.4377(8) 0.052(4) Uani 1 1 d . . . N3 N 0.0641(16) 1.1695(10) 0.0250(10) 0.074(6) Uani 1 1 d . . . C46 C -0.0211(17) 0.9894(15) 0.1081(11) 0.078(8) Uani 1 1 d . . . H46A H -0.0899 1.0056 0.1313 0.118 Uiso 1 1 calc R . . H46B H -0.0279 0.9455 0.0898 0.118 Uiso 1 1 calc R . . H46C H -0.0005 1.0310 0.0764 0.118 Uiso 1 1 calc R . . C47 C 1.4820(17) 0.3406(12) 0.4197(13) 0.088(9) Uani 1 1 d . . . H47A H 1.5571 0.3379 0.4012 0.132 Uiso 1 1 calc R . . H47B H 1.4378 0.3318 0.3910 0.132 Uiso 1 1 calc R . . H47C H 1.4746 0.3018 0.4556 0.132 Uiso 1 1 calc R . . C48 C 1.5242(17) 0.4752(12) 0.4148(13) 0.083(8) Uani 1 1 d . . . H48A H 1.5917 0.4486 0.3974 0.125 Uiso 1 1 calc R . . H48B H 1.5368 0.4986 0.4480 0.125 Uiso 1 1 calc R . . H48C H 1.4960 0.5145 0.3839 0.125 Uiso 1 1 calc R . . C49 C 0.0349(18) 0.9799(13) 0.2144(9) 0.073(7) Uani 1 1 d . . . H49A H -0.0420 0.9972 0.2213 0.109 Uiso 1 1 calc R . . H49B H 0.0751 1.0184 0.2221 0.109 Uiso 1 1 calc R . . H49C H 0.0509 0.9323 0.2415 0.109 Uiso 1 1 calc R . . C50 C 0.013(3) 1.2107(19) 0.0741(14) 0.131(13) Uani 1 1 d . . . H50A H -0.0517 1.2427 0.0626 0.196 Uiso 1 1 calc R . . H50B H 0.0630 1.2427 0.0822 0.196 Uiso 1 1 calc R . . H50C H -0.0059 1.1744 0.1103 0.196 Uiso 1 1 calc R . . C51 C 0.005(3) 1.178(2) -0.0298(15) 0.140(13) Uani 1 1 d . . . H51A H -0.0587 1.2157 -0.0253 0.210 Uiso 1 1 calc R . . H51B H -0.0163 1.1294 -0.0327 0.210 Uiso 1 1 calc R . . H51C H 0.0528 1.1956 -0.0664 0.210 Uiso 1 1 calc R . . O23 O 0.2801(14) 0.9331(10) 0.2624(8) 0.096(5) Uani 1 1 d . . . C52 C 0.320(3) 0.9816(18) 0.2877(15) 0.120(10) Uani 1 1 d U . . H52 H 0.2749 1.0043 0.3189 0.144 Uiso 1 1 calc R . . N4 N 0.4203(16) 1.0000(11) 0.2712(8) 0.071(5) Uani 1 1 d . . . C53 C 0.459(3) 1.0622(18) 0.292(2) 0.160(16) Uani 1 1 d . . . H53A H 0.5339 1.0655 0.2741 0.241 Uiso 1 1 calc R . . H53B H 0.4536 1.0524 0.3357 0.241 Uiso 1 1 calc R . . H53C H 0.4153 1.1101 0.2793 0.241 Uiso 1 1 calc R . . C54 C 0.497(2) 0.9722(18) 0.2283(14) 0.133(13) Uani 1 1 d . . . H54A H 0.5628 0.9956 0.2257 0.200 Uiso 1 1 calc R . . H54B H 0.4714 0.9839 0.1892 0.200 Uiso 1 1 calc R . . H54C H 0.5131 0.9171 0.2393 0.200 Uiso 1 1 calc R . . O24 O 0.8064(18) 0.9659(11) 0.3932(8) 0.115(7) Uani 1 1 d . . . C55 C 0.884(3) 0.9066(19) 0.3876(14) 0.108(10) Uani 1 1 d U . . H55 H 0.8623 0.8596 0.3843 0.130 Uiso 1 1 calc R . . N5 N 0.997(2) 0.9095(11) 0.3863(10) 0.099(8) Uani 1 1 d . . . C56 C 1.066(3) 0.8436(16) 0.3776(11) 0.109(10) Uani 1 1 d . . . H56A H 1.0250 0.8047 0.3717 0.164 Uiso 1 1 calc R . . H56B H 1.1026 0.8254 0.4130 0.164 Uiso 1 1 calc R . . H56C H 1.1195 0.8545 0.3421 0.164 Uiso 1 1 calc R . . C57 C 1.030(3) 0.9780(15) 0.3945(14) 0.125(12) Uani 1 1 d . . . H57A H 0.9671 1.0160 0.3994 0.187 Uiso 1 1 calc R . . H57B H 1.0798 0.9964 0.3592 0.187 Uiso 1 1 calc R . . H57C H 1.0657 0.9689 0.4304 0.187 Uiso 1 1 calc R . . O25 O 0.2468(14) 1.2703(10) 0.5043(8) 0.093(5) Uani 1 1 d . . . C58 C 0.170(2) 1.2418(12) 0.4964(9) 0.062(6) Uani 1 1 d . . . H58 H 0.1013 1.2643 0.5116 0.074 Uiso 1 1 calc R . . N6 N 0.1730(15) 1.1825(9) 0.4686(8) 0.055(4) Uani 1 1 d . . . C59 C 0.074(2) 1.1550(12) 0.4618(10) 0.078(7) Uani 1 1 d . . . H59A H 0.0918 1.1122 0.4394 0.116 Uiso 1 1 calc R . . H59B H 0.0293 1.1959 0.4398 0.116 Uiso 1 1 calc R . . H59C H 0.0352 1.1384 0.5016 0.116 Uiso 1 1 calc R . . C60 C 0.275(2) 1.149(2) 0.4428(16) 0.148(14) Uani 1 1 d . . . H60A H 0.2656 1.1068 0.4231 0.221 Uiso 1 1 calc R . . H60B H 0.3201 1.1294 0.4746 0.221 Uiso 1 1 calc R . . H60C H 0.3105 1.1869 0.4131 0.221 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 Dy1 0.0202(5) 0.0212(4) 0.0156(4) -0.0110(3) -0.0068(3) 0.0048(3) Dy2 0.0178(5) 0.0186(4) 0.0204(4) -0.0109(3) -0.0081(3) 0.0024(3) O1 0.031(4) 0.029(4) 0.027(4) -0.008(3) -0.012(3) 0.000(3) O2 0.028(7) 0.033(6) 0.029(6) -0.014(5) -0.004(5) -0.005(5) C1 0.022(9) 0.025(8) 0.038(10) -0.007(7) -0.012(7) -0.005(7) C2 0.022(9) 0.031(8) 0.032(9) -0.018(7) -0.007(7) -0.004(7) C3 0.042(11) 0.023(8) 0.043(10) -0.021(7) -0.022(8) 0.007(7) C4 0.032(10) 0.031(9) 0.020(8) -0.001(7) -0.015(7) -0.002(7) C5 0.040(11) 0.027(9) 0.029(9) -0.012(7) -0.011(8) -0.013(8) C6 0.064(13) 0.029(9) 0.026(9) -0.002(7) -0.021(8) -0.010(8) C7 0.058(12) 0.031(9) 0.024(9) 0.000(7) -0.028(8) -0.009(8) C8 0.035(10) 0.029(8) 0.024(9) -0.016(7) -0.014(7) -0.002(7) C9 0.036(10) 0.028(9) 0.026(9) -0.012(7) -0.007(7) -0.006(7) C10 0.040(6) 0.028(5) 0.033(5) -0.008(4) -0.005(4) -0.005(4) C11 0.031(10) 0.018(7) 0.035(10) -0.011(7) -0.012(7) -0.010(7) C12 0.053(12) 0.028(8) 0.035(10) -0.013(7) -0.027(8) -0.004(8) C13 0.014(9) 0.031(8) 0.039(10) -0.016(7) -0.008(7) -0.001(6) C14 0.020(5) 0.027(5) 0.025(5) -0.006(4) -0.007(4) -0.003(4) O3 0.040(7) 0.033(6) 0.045(7) -0.023(5) -0.016(6) -0.002(5) O4 0.029(4) 0.034(4) 0.033(4) -0.010(4) -0.017(4) -0.002(4) S1 0.048(3) 0.024(2) 0.034(2) -0.0111(17) -0.018(2) -0.0048(19) O5 0.070(9) 0.028(6) 0.039(7) -0.011(5) -0.017(6) -0.011(6) O6 0.044(8) 0.045(7) 0.056(8) -0.028(6) -0.030(6) 0.011(6) O7 0.028(4) 0.025(4) 0.020(4) -0.007(3) -0.012(3) 0.003(3) O8 0.018(6) 0.030(6) 0.036(6) 0.001(5) -0.019(5) -0.002(5) C15 0.035(11) 0.018(8) 0.026(9) -0.004(6) -0.011(7) 0.006(7) C16 0.030(10) 0.024(8) 0.029(9) 0.005(7) -0.020(7) -0.002(7) C17 0.051(12) 0.030(9) 0.026(9) 0.009(7) -0.023(8) -0.014(8) C18 0.049(6) 0.049(6) 0.049(6) -0.002(4) -0.019(5) -0.009(4) C19 0.055(7) 0.055(6) 0.058(7) -0.003(5) -0.014(5) -0.015(5) C20 0.025(9) 0.030(9) 0.038(10) 0.003(7) -0.023(8) 0.005(7) C21 0.056(13) 0.034(10) 0.045(11) 0.009(8) -0.036(10) -0.013(9) C22 0.057(12) 0.020(8) 0.040(10) 0.007(7) -0.028(9) -0.014(8) C23 0.043(11) 0.019(8) 0.036(10) 0.002(7) -0.023(8) -0.010(7) C24 0.064(14) 0.041(11) 0.066(14) 0.020(10) -0.045(12) -0.019(10) C25 0.051(12) 0.024(8) 0.044(11) 0.008(7) -0.026(9) -0.005(8) C26 0.035(11) 0.030(9) 0.041(10) -0.010(8) -0.017(8) -0.005(8) C27 0.032(10) 0.025(8) 0.019(8) -0.001(6) -0.017(7) -0.001(7) C28 0.030(5) 0.027(5) 0.026(5) -0.010(4) -0.007(4) -0.001(4) O9 0.041(7) 0.016(5) 0.018(5) -0.002(4) -0.016(5) 0.003(4) O10 0.030(7) 0.037(6) 0.026(6) -0.007(5) -0.017(5) 0.005(5) S2 0.046(3) 0.040(3) 0.043(3) 0.017(2) -0.031(2) -0.019(2) O11 0.081(10) 0.038(7) 0.078(10) 0.009(7) -0.057(8) -0.023(7) O12 0.042(9) 0.097(11) 0.057(9) 0.024(8) -0.011(7) -0.017(8) O13 0.024(6) 0.028(5) 0.012(5) -0.013(4) 0.001(4) 0.000(5) O14 0.037(7) 0.021(5) 0.013(5) -0.009(4) -0.003(5) -0.006(5) C29 0.025(9) 0.019(8) 0.012(8) -0.005(6) -0.003(7) 0.004(7) C30 0.025(5) 0.027(5) 0.020(5) -0.009(4) -0.002(4) -0.004(4) C31 0.027(9) 0.025(8) 0.026(8) -0.015(6) 0.001(7) -0.001(7) C32 0.031(10) 0.049(10) 0.031(9) -0.027(8) 0.008(8) -0.010(8) C33 0.029(10) 0.030(8) 0.032(9) -0.016(7) 0.002(7) -0.013(7) C34 0.035(6) 0.038(5) 0.038(6) -0.013(4) 0.001(4) -0.010(4) C35 0.035(10) 0.031(9) 0.029(9) -0.024(7) 0.004(7) -0.003(7) C36 0.017(9) 0.034(9) 0.037(10) -0.026(7) 0.005(7) -0.004(7) C37 0.024(9) 0.049(10) 0.028(9) -0.025(8) 0.004(7) -0.008(8) C38 0.033(10) 0.047(10) 0.037(10) -0.033(8) 0.008(8) -0.015(8) C39 0.033(10) 0.024(8) 0.031(9) -0.013(7) -0.007(7) -0.001(7) C40 0.030(5) 0.033(5) 0.031(5) -0.013(4) -0.002(4) -0.001(4) C41 0.017(5) 0.024(5) 0.018(5) -0.007(4) -0.002(4) 0.000(4) C42 0.029(10) 0.015(7) 0.016(8) -0.005(6) -0.011(7) -0.004(7) O15 0.015(6) 0.031(6) 0.030(6) -0.019(5) 0.002(5) 0.001(5) S3 0.034(3) 0.040(2) 0.035(2) -0.0285(19) 0.012(2) -0.016(2) O16 0.069(9) 0.042(7) 0.043(7) -0.032(6) 0.019(6) -0.023(6) O17 0.026(7) 0.071(9) 0.050(8) -0.043(7) 0.002(6) 0.000(6) O18 0.021(6) 0.038(6) 0.024(6) -0.019(5) -0.010(5) 0.011(5) O19 0.022(6) 0.048(7) 0.027(6) -0.015(5) -0.002(5) -0.005(5) O20 0.040(5) 0.040(4) 0.037(4) -0.015(4) -0.003(4) 0.006(4) O21 0.026(7) 0.034(7) 0.073(9) -0.031(6) -0.011(6) 0.006(5) O22 0.035(7) 0.043(7) 0.093(10) -0.038(7) 0.029(7) -0.017(6) C43 0.028(11) 0.042(11) 0.059(13) -0.015(9) -0.010(9) 0.006(8) C44 0.035(12) 0.039(10) 0.050(12) -0.010(9) 0.001(9) -0.006(8) C45 0.065(16) 0.073(15) 0.073(16) -0.013(13) -0.031(13) -0.005(13) N1 0.042(10) 0.053(10) 0.046(10) -0.013(8) 0.002(8) -0.012(8) N2 0.029(9) 0.042(9) 0.083(12) -0.011(8) 0.000(8) -0.005(7) N3 0.069(14) 0.051(11) 0.090(16) -0.006(10) -0.009(12) 0.025(10) C46 0.046(15) 0.12(2) 0.070(16) -0.005(15) -0.024(13) 0.000(14) C47 0.041(14) 0.061(15) 0.16(3) -0.029(16) -0.002(15) 0.017(11) C48 0.048(15) 0.064(15) 0.14(2) -0.004(15) -0.034(15) -0.015(12) C49 0.070(16) 0.087(16) 0.065(15) -0.053(13) 0.031(12) -0.018(13) C50 0.12(3) 0.16(3) 0.11(3) -0.08(2) 0.03(2) 0.00(2) C51 0.13(3) 0.16(3) 0.14(3) -0.03(2) -0.07(3) 0.01(2) O23 0.088(13) 0.101(13) 0.110(14) -0.029(11) -0.015(11) -0.032(10) C52 0.119(11) 0.120(11) 0.118(11) -0.017(5) -0.016(5) -0.013(5) N4 0.064(13) 0.089(14) 0.058(12) -0.020(10) 0.002(10) -0.007(11) C53 0.11(3) 0.13(3) 0.28(5) -0.08(3) -0.04(3) -0.05(2) C54 0.11(3) 0.15(3) 0.11(3) -0.01(2) 0.03(2) 0.03(2) O24 0.159(19) 0.097(14) 0.086(13) -0.003(11) -0.042(13) 0.006(13) C55 0.109(11) 0.108(10) 0.107(11) -0.015(5) -0.016(5) -0.012(5) N5 0.15(2) 0.059(13) 0.089(16) -0.028(11) 0.021(15) -0.035(14) C56 0.17(3) 0.10(2) 0.049(15) -0.018(14) 0.039(17) -0.02(2) C57 0.16(3) 0.09(2) 0.14(3) -0.031(19) 0.03(2) -0.08(2) O25 0.095(13) 0.112(14) 0.091(13) -0.025(10) -0.018(10) -0.055(11) C58 0.088(18) 0.054(13) 0.053(13) -0.020(11) -0.001(12) -0.035(12) N6 0.065(12) 0.045(9) 0.058(11) -0.019(8) -0.007(9) -0.006(9) C59 0.13(2) 0.059(14) 0.048(13) -0.012(11) -0.008(14) -0.015(14) C60 0.10(3) 0.18(3) 0.16(3) -0.10(3) 0.01(2) 0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O7 2.325(10) 2_675 ? Dy1 O18 2.340(10) . ? Dy1 O19 2.350(10) . ? Dy1 O8 2.379(9) . ? Dy1 O1 2.392(10) . ? Dy1 O15 2.395(10) . ? Dy1 O20 2.433(11) . ? Dy1 O2 2.546(10) . ? Dy1 C1 2.798(15) . ? Dy1 O7 2.874(9) . ? Dy1 C15 2.982(15) . ? Dy2 O9 2.293(9) 2_766 ? Dy2 O14 2.365(9) 1_645 ? Dy2 O10 2.375(9) . ? Dy2 O13 2.387(9) 2_676 ? Dy2 O21 2.391(11) . ? Dy2 O22 2.427(12) . ? Dy2 O4 2.439(10) 1_656 ? Dy2 O3 2.473(10) 1_656 ? Dy2 C14 2.768(15) 1_656 ? O1 C1 1.254(17) . ? O2 C1 1.305(17) . ? C1 C2 1.53(2) . ? C2 C4 1.39(2) . ? C2 C3 1.41(2) . ? C3 C6 1.38(2) . ? C3 H3 0.9300 . ? C4 C5 1.37(2) . ? C4 H4 0.9300 . ? C5 C7 1.39(2) . ? C5 S1 1.782(15) . ? C6 C7 1.39(2) . ? C6 H6 0.9300 . ? C7 C8 1.49(2) . ? C8 C10 1.39(2) . ? C8 C9 1.394(19) . ? C9 C11 1.39(2) . ? C9 S1 1.791(16) . ? C10 C12 1.39(2) . ? C10 H10 0.9300 . ? C11 C13 1.37(2) . ? C11 H11 0.9300 . ? C12 C13 1.395(19) . ? C12 H12 0.9300 . ? C13 C14 1.53(2) . ? C14 O4 1.240(17) . ? C14 O3 1.276(17) . ? C14 Dy2 2.768(15) 1_454 ? O3 Dy2 2.473(10) 1_454 ? O4 Dy2 2.439(10) 1_454 ? S1 O5 1.449(12) . ? S1 O6 1.459(12) . ? O7 C15 1.274(17) . ? O7 Dy1 2.325(10) 2_675 ? O8 C15 1.241(17) . ? C15 C16 1.506(19) . ? C16 C17 1.40(2) . ? C16 C18 1.40(2) . ? C17 C20 1.401(19) . ? C17 H17 0.9300 . ? C18 C19 1.41(2) . ? C18 H18 0.9300 . ? C19 C21 1.39(2) . ? C19 H19 0.9300 . ? C20 C21 1.37(2) . ? C20 S2 1.781(15) . ? C21 C22 1.53(2) . ? C22 C24 1.39(2) . ? C22 C23 1.42(2) . ? C23 C26 1.35(2) . ? C23 S2 1.766(15) . ? C24 C25 1.43(2) . ? C24 H24 0.9300 . ? C25 C27 1.44(2) . ? C25 H25 0.9300 . ? C26 C27 1.39(2) . ? C26 H26 0.9300 . ? C27 C28 1.47(2) . ? C28 O10 1.271(17) . ? C28 O9 1.274(17) . ? O9 Dy2 2.293(9) 2_766 ? S2 O11 1.412(14) . ? S2 O12 1.456(14) . ? O13 C29 1.232(16) . ? O13 Dy2 2.387(9) 2_676 ? O14 C29 1.267(16) . ? O14 Dy2 2.365(9) 1_465 ? C29 C30 1.532(19) . ? C30 C32 1.38(2) . ? C30 C31 1.398(19) . ? C31 C33 1.40(2) . ? C31 H31 0.9300 . ? C32 C34 1.42(2) . ? C32 H32 0.9300 . ? C33 C35 1.39(2) . ? C33 S3 1.794(14) . ? C34 C35 1.40(2) . ? C34 H34 0.9300 . ? C35 C36 1.488(19) . ? C36 C38 1.36(2) . ? C36 C37 1.39(2) . ? C37 C39 1.41(2) . ? C37 S3 1.787(15) . ? C38 C40 1.39(2) . ? C38 H38 0.9300 . ? C39 C41 1.37(2) . ? C39 H39 0.9300 . ? C40 C41 1.392(19) . ? C40 H40 0.9300 . ? C41 C42 1.530(19) . ? C42 O15 1.259(16) . ? C42 O18 1.268(17) 2_675 ? S3 O16 1.435(12) . ? S3 O17 1.452(13) . ? O18 C42 1.268(17) 2_675 ? O19 C44 1.24(2) . ? O20 C45 1.22(2) . ? O21 C43 1.182(18) . ? C43 N2 1.33(2) . ? C43 H43 0.9300 . ? C44 N1 1.33(2) . ? C45 N3 1.34(3) . ? C45 H45 0.9300 . ? N1 C49 1.46(2) . ? N1 C46 1.53(2) . ? N2 C48 1.47(2) . ? N2 C47 1.51(2) . ? N3 C50 1.44(3) . ? N3 C51 1.51(3) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? O23 C52 1.30(3) . ? C52 N4 1.32(3) . ? C52 H52 0.9300 . ? N4 C54 1.35(3) . ? N4 C53 1.44(3) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? O24 C55 1.32(3) . ? C55 N5 1.42(3) . ? C55 H55 0.9300 . ? N5 C56 1.36(3) . ? N5 C57 1.39(3) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? O25 C58 1.20(2) . ? C58 N6 1.31(2) . ? C58 H58 0.9300 . ? N6 C60 1.41(3) . ? N6 C59 1.43(3) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Dy1 O18 74.6(4) 2_675 . ? O7 Dy1 O19 148.6(4) 2_675 . ? O18 Dy1 O19 136.8(4) . . ? O7 Dy1 O8 124.7(3) 2_675 . ? O18 Dy1 O8 77.7(3) . . ? O19 Dy1 O8 73.6(3) . . ? O7 Dy1 O1 80.9(3) 2_675 . ? O18 Dy1 O1 74.9(3) . . ? O19 Dy1 O1 104.1(3) . . ? O8 Dy1 O1 134.9(3) . . ? O7 Dy1 O15 80.7(3) 2_675 . ? O18 Dy1 O15 129.7(3) . . ? O19 Dy1 O15 77.0(3) . . ? O8 Dy1 O15 81.7(3) . . ? O1 Dy1 O15 142.8(3) . . ? O7 Dy1 O20 79.2(4) 2_675 . ? O18 Dy1 O20 139.8(4) . . ? O19 Dy1 O20 73.4(4) . . ? O8 Dy1 O20 142.4(4) . . ? O1 Dy1 O20 71.2(4) . . ? O15 Dy1 O20 73.7(4) . . ? O7 Dy1 O2 128.1(3) 2_675 . ? O18 Dy1 O2 70.3(3) . . ? O19 Dy1 O2 74.8(3) . . ? O8 Dy1 O2 83.4(3) . . ? O1 Dy1 O2 54.0(3) . . ? O15 Dy1 O2 150.9(3) . . ? O20 Dy1 O2 104.8(4) . . ? O7 Dy1 C1 103.0(4) 2_675 . ? O18 Dy1 C1 67.5(4) . . ? O19 Dy1 C1 92.3(4) . . ? O8 Dy1 C1 109.1(4) . . ? O1 Dy1 C1 26.5(4) . . ? O15 Dy1 C1 162.3(4) . . ? O20 Dy1 C1 89.8(4) . . ? O2 Dy1 C1 27.8(4) . . ? O7 Dy1 O7 76.3(3) 2_675 . ? O18 Dy1 O7 64.1(3) . . ? O19 Dy1 O7 114.3(3) . . ? O8 Dy1 O7 48.5(3) . . ? O1 Dy1 O7 137.0(3) . . ? O15 Dy1 O7 67.8(3) . . ? O20 Dy1 O7 137.0(3) . . ? O2 Dy1 O7 118.1(3) . . ? C1 Dy1 O7 129.9(4) . . ? O7 Dy1 C15 101.4(4) 2_675 . ? O18 Dy1 C15 70.5(4) . . ? O19 Dy1 C15 92.8(4) . . ? O8 Dy1 C15 23.5(3) . . ? O1 Dy1 C15 143.1(4) . . ? O15 Dy1 C15 72.5(4) . . ? O20 Dy1 C15 145.6(4) . . ? O2 Dy1 C15 101.5(4) . . ? C1 Dy1 C15 122.7(4) . . ? O7 Dy1 C15 25.0(3) . . ? O9 Dy2 O14 77.1(3) 2_766 1_645 ? O9 Dy2 O10 122.6(4) 2_766 . ? O14 Dy2 O10 78.8(3) 1_645 . ? O9 Dy2 O13 75.7(3) 2_766 2_676 ? O14 Dy2 O13 127.5(3) 1_645 2_676 ? O10 Dy2 O13 79.4(3) . 2_676 ? O9 Dy2 O21 79.0(4) 2_766 . ? O14 Dy2 O21 75.9(4) 1_645 . ? O10 Dy2 O21 141.6(4) . . ? O13 Dy2 O21 139.0(4) 2_676 . ? O9 Dy2 O22 146.4(4) 2_766 . ? O14 Dy2 O22 77.9(4) 1_645 . ? O10 Dy2 O22 73.3(4) . . ? O13 Dy2 O22 137.8(3) 2_676 . ? O21 Dy2 O22 73.5(4) . . ? O9 Dy2 O4 82.4(3) 2_766 1_656 ? O14 Dy2 O4 145.2(3) 1_645 1_656 ? O10 Dy2 O4 136.0(4) . 1_656 ? O13 Dy2 O4 72.5(3) 2_676 1_656 ? O21 Dy2 O4 72.7(4) . 1_656 ? O22 Dy2 O4 106.7(4) . 1_656 ? O9 Dy2 O3 132.3(3) 2_766 1_656 ? O14 Dy2 O3 150.1(3) 1_645 1_656 ? O10 Dy2 O3 86.2(4) . 1_656 ? O13 Dy2 O3 73.6(3) 2_676 1_656 ? O21 Dy2 O3 102.0(4) . 1_656 ? O22 Dy2 O3 73.1(4) . 1_656 ? O4 Dy2 O3 53.9(4) 1_656 1_656 ? O9 Dy2 C14 106.7(4) 2_766 1_656 ? O14 Dy2 C14 162.9(4) 1_645 1_656 ? O10 Dy2 C14 111.2(4) . 1_656 ? O13 Dy2 C14 69.2(4) 2_676 1_656 ? O21 Dy2 C14 88.3(4) . 1_656 ? O22 Dy2 C14 91.5(4) . 1_656 ? O4 Dy2 C14 26.6(4) 1_656 1_656 ? O3 Dy2 C14 27.5(4) 1_656 1_656 ? C1 O1 Dy1 95.1(9) . . ? C1 O2 Dy1 86.9(8) . . ? O1 C1 O2 122.7(14) . . ? O1 C1 C2 118.4(13) . . ? O2 C1 C2 118.9(13) . . ? O1 C1 Dy1 58.4(8) . . ? O2 C1 Dy1 65.3(7) . . ? C2 C1 Dy1 166.3(10) . . ? C4 C2 C3 120.2(14) . . ? C4 C2 C1 122.1(14) . . ? C3 C2 C1 117.7(13) . . ? C6 C3 C2 120.9(13) . . ? C6 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C2 117.8(14) . . ? C5 C4 H4 121.1 . . ? C2 C4 H4 121.1 . . ? C4 C5 C7 123.2(14) . . ? C4 C5 S1 126.6(12) . . ? C7 C5 S1 110.1(11) . . ? C3 C6 C7 118.9(14) . . ? C3 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C5 C7 C6 118.9(14) . . ? C5 C7 C8 113.8(13) . . ? C6 C7 C8 127.3(14) . . ? C10 C8 C9 118.7(14) . . ? C10 C8 C7 128.8(14) . . ? C9 C8 C7 112.4(13) . . ? C11 C9 C8 122.7(14) . . ? C11 C9 S1 126.6(12) . . ? C8 C9 S1 110.6(11) . . ? C8 C10 C12 119.0(14) . . ? C8 C10 H10 120.5 . . ? C12 C10 H10 120.5 . . ? C13 C11 C9 117.8(14) . . ? C13 C11 H11 121.1 . . ? C9 C11 H11 121.1 . . ? C10 C12 C13 121.2(15) . . ? C10 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C11 C13 C12 120.5(14) . . ? C11 C13 C14 118.9(13) . . ? C12 C13 C14 120.6(14) . . ? O4 C14 O3 124.6(14) . . ? O4 C14 C13 117.6(13) . . ? O3 C14 C13 117.7(13) . . ? O4 C14 Dy2 61.7(8) . 1_454 ? O3 C14 Dy2 63.3(8) . 1_454 ? C13 C14 Dy2 170.5(10) . 1_454 ? C14 O3 Dy2 89.2(9) . 1_454 ? C14 O4 Dy2 91.7(9) . 1_454 ? O5 S1 O6 116.7(7) . . ? O5 S1 C5 111.4(7) . . ? O6 S1 C5 110.6(7) . . ? O5 S1 C9 112.8(7) . . ? O6 S1 C9 110.1(7) . . ? C5 S1 C9 92.7(6) . . ? C15 O7 Dy1 173.9(10) . 2_675 ? C15 O7 Dy1 82.2(9) . . ? Dy1 O7 Dy1 103.7(3) 2_675 . ? C15 O8 Dy1 106.7(8) . . ? O8 C15 O7 122.4(13) . . ? O8 C15 C16 120.9(13) . . ? O7 C15 C16 116.7(14) . . ? O8 C15 Dy1 49.9(7) . . ? O7 C15 Dy1 72.7(8) . . ? C16 C15 Dy1 169.1(11) . . ? C17 C16 C18 119.0(14) . . ? C17 C16 C15 121.9(13) . . ? C18 C16 C15 118.9(14) . . ? C20 C17 C16 116.9(14) . . ? C20 C17 H17 121.5 . . ? C16 C17 H17 121.5 . . ? C16 C18 C19 123.3(17) . . ? C16 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? C21 C19 C18 116.2(16) . . ? C21 C19 H19 121.9 . . ? C18 C19 H19 121.9 . . ? C21 C20 C17 123.7(15) . . ? C21 C20 S2 111.3(11) . . ? C17 C20 S2 124.9(12) . . ? C20 C21 C19 120.8(16) . . ? C20 C21 C22 113.3(14) . . ? C19 C21 C22 125.9(15) . . ? C24 C22 C23 120.6(15) . . ? C24 C22 C21 128.2(15) . . ? C23 C22 C21 111.2(13) . . ? C26 C23 C22 121.6(14) . . ? C26 C23 S2 127.5(12) . . ? C22 C23 S2 110.9(11) . . ? C22 C24 C25 117.9(16) . . ? C22 C24 H24 121.0 . . ? C25 C24 H24 121.1 . . ? C24 C25 C27 119.9(14) . . ? C24 C25 H25 120.1 . . ? C27 C25 H25 120.1 . . ? C23 C26 C27 120.6(15) . . ? C23 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C25 119.5(14) . . ? C26 C27 C28 121.6(14) . . ? C25 C27 C28 119.0(13) . . ? O10 C28 O9 122.1(14) . . ? O10 C28 C27 117.2(13) . . ? O9 C28 C27 120.7(14) . . ? C28 O9 Dy2 174.4(9) . 2_766 ? C28 O10 Dy2 112.1(9) . . ? O11 S2 O12 117.3(9) . . ? O11 S2 C23 110.1(8) . . ? O12 S2 C23 111.0(8) . . ? O11 S2 C20 110.1(8) . . ? O12 S2 C20 112.4(8) . . ? C23 S2 C20 93.4(7) . . ? C29 O13 Dy2 139.2(9) . 2_676 ? C29 O14 Dy2 138.5(9) . 1_465 ? O13 C29 O14 127.9(13) . . ? O13 C29 C30 117.4(12) . . ? O14 C29 C30 114.7(12) . . ? C32 C30 C31 120.4(13) . . ? C32 C30 C29 119.9(13) . . ? C31 C30 C29 119.6(13) . . ? C33 C31 C30 117.5(13) . . ? C33 C31 H31 121.3 . . ? C30 C31 H31 121.3 . . ? C30 C32 C34 121.8(14) . . ? C30 C32 H32 119.1 . . ? C34 C32 H32 119.1 . . ? C35 C33 C31 123.1(13) . . ? C35 C33 S3 110.3(11) . . ? C31 C33 S3 126.5(11) . . ? C35 C34 C32 117.8(15) . . ? C35 C34 H34 121.1 . . ? C32 C34 H34 121.1 . . ? C33 C35 C34 119.2(13) . . ? C33 C35 C36 113.4(13) . . ? C34 C35 C36 127.3(14) . . ? C38 C36 C37 117.8(13) . . ? C38 C36 C35 128.9(13) . . ? C37 C36 C35 113.2(13) . . ? C36 C37 C39 123.2(14) . . ? C36 C37 S3 110.4(11) . . ? C39 C37 S3 126.4(12) . . ? C36 C38 C40 119.7(14) . . ? C36 C38 H38 120.1 . . ? C40 C38 H38 120.1 . . ? C41 C39 C37 117.7(13) . . ? C41 C39 H39 121.2 . . ? C37 C39 H39 121.2 . . ? C38 C40 C41 122.3(15) . . ? C38 C40 H40 118.8 . . ? C41 C40 H40 118.8 . . ? C39 C41 C40 119.2(13) . . ? C39 C41 C42 121.1(12) . . ? C40 C41 C42 119.7(13) . . ? O15 C42 O18 127.1(13) . 2_675 ? O15 C42 C41 118.4(13) . . ? O18 C42 C41 114.5(12) 2_675 . ? C42 O15 Dy1 129.6(9) . . ? O16 S3 O17 118.7(8) . . ? O16 S3 C37 110.5(8) . . ? O17 S3 C37 110.0(7) . . ? O16 S3 C33 111.2(7) . . ? O17 S3 C33 110.8(7) . . ? C37 S3 C33 92.6(7) . . ? C42 O18 Dy1 143.4(9) 2_675 . ? C44 O19 Dy1 130.7(11) . . ? C45 O20 Dy1 130.9(13) . . ? C43 O21 Dy2 131.1(11) . . ? O21 C43 N2 123.6(17) . . ? O21 C43 H43 118.2 . . ? N2 C43 H43 118.2 . . ? O19 C44 N1 122.6(17) . . ? O20 C45 N3 126(2) . . ? O20 C45 H45 116.9 . . ? N3 C45 H45 116.9 . . ? C44 N1 C49 124.0(17) . . ? C44 N1 C46 118.5(16) . . ? C49 N1 C46 117.4(17) . . ? C43 N2 C48 124.0(17) . . ? C43 N2 C47 121.7(15) . . ? C48 N2 C47 113.7(17) . . ? C45 N3 C50 120(2) . . ? C45 N3 C51 122(2) . . ? C50 N3 C51 117(2) . . ? N1 C46 H46A 109.5 . . ? N1 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N1 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N2 C47 H47A 109.5 . . ? N2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N2 C48 H48A 109.5 . . ? N2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N1 C49 H49A 109.5 . . ? N1 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N1 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N3 C50 H50A 109.5 . . ? N3 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N3 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N3 C51 H51A 109.5 . . ? N3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O23 C52 N4 123(3) . . ? O23 C52 H52 118.4 . . ? N4 C52 H52 118.4 . . ? C52 N4 C54 127(3) . . ? C52 N4 C53 123(3) . . ? C54 N4 C53 109(3) . . ? N4 C53 H53A 109.5 . . ? N4 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N4 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N4 C54 H54A 109.5 . . ? N4 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N4 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O24 C55 N5 125(3) . . ? O24 C55 H55 117.6 . . ? N5 C55 H55 117.6 . . ? C56 N5 C57 125(3) . . ? C56 N5 C55 117(2) . . ? C57 N5 C55 118(3) . . ? N5 C56 H56A 109.5 . . ? N5 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N5 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N5 C57 H57A 109.5 . . ? N5 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N5 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O25 C58 N6 127(2) . . ? O25 C58 H58 116.4 . . ? N6 C58 H58 116.4 . . ? C58 N6 C60 118(2) . . ? C58 N6 C59 121.0(19) . . ? C60 N6 C59 121(2) . . ? N6 C59 H59A 109.5 . . ? N6 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N6 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N6 C60 H60A 109.5 . . ? N6 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N6 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Dy1 O1 C1 146.1(9) 2_675 . . . ? O18 Dy1 O1 C1 69.7(9) . . . . ? O19 Dy1 O1 C1 -65.6(9) . . . . ? O8 Dy1 O1 C1 15.2(11) . . . . ? O15 Dy1 O1 C1 -152.7(9) . . . . ? O20 Dy1 O1 C1 -132.2(10) . . . . ? O2 Dy1 O1 C1 -6.7(9) . . . . ? O7 Dy1 O1 C1 87.6(10) . . . . ? C15 Dy1 O1 C1 49.2(12) . . . . ? O7 Dy1 O2 C1 -28.6(10) 2_675 . . . ? O18 Dy1 O2 C1 -78.9(9) . . . . ? O19 Dy1 O2 C1 127.1(9) . . . . ? O8 Dy1 O2 C1 -158.1(9) . . . . ? O1 Dy1 O2 C1 6.4(8) . . . . ? O15 Dy1 O2 C1 142.4(9) . . . . ? O20 Dy1 O2 C1 59.3(9) . . . . ? O7 Dy1 O2 C1 -123.1(8) . . . . ? C15 Dy1 O2 C1 -143.1(9) . . . . ? Dy1 O1 C1 O2 12.6(16) . . . . ? Dy1 O1 C1 C2 -164.7(12) . . . . ? Dy1 O2 C1 O1 -11.8(15) . . . . ? Dy1 O2 C1 C2 165.4(12) . . . . ? O7 Dy1 C1 O1 -34.4(9) 2_675 . . . ? O18 Dy1 C1 O1 -101.4(9) . . . . ? O19 Dy1 C1 O1 117.9(9) . . . . ? O8 Dy1 C1 O1 -168.7(8) . . . . ? O15 Dy1 C1 O1 65.9(17) . . . . ? O20 Dy1 C1 O1 44.5(9) . . . . ? O2 Dy1 C1 O1 168.3(15) . . . . ? O7 Dy1 C1 O1 -117.3(8) . . . . ? C15 Dy1 C1 O1 -147.3(8) . . . . ? O7 Dy1 C1 O2 157.3(8) 2_675 . . . ? O18 Dy1 C1 O2 90.3(9) . . . . ? O19 Dy1 C1 O2 -50.4(9) . . . . ? O8 Dy1 C1 O2 23.0(9) . . . . ? O1 Dy1 C1 O2 -168.3(15) . . . . ? O15 Dy1 C1 O2 -102.4(14) . . . . ? O20 Dy1 C1 O2 -123.8(9) . . . . ? O7 Dy1 C1 O2 74.4(9) . . . . ? C15 Dy1 C1 O2 44.4(10) . . . . ? O7 Dy1 C1 C2 46(4) 2_675 . . . ? O18 Dy1 C1 C2 -21(4) . . . . ? O19 Dy1 C1 C2 -162(4) . . . . ? O8 Dy1 C1 C2 -88(4) . . . . ? O1 Dy1 C1 C2 80(4) . . . . ? O15 Dy1 C1 C2 146(4) . . . . ? O20 Dy1 C1 C2 125(4) . . . . ? O2 Dy1 C1 C2 -111(5) . . . . ? O7 Dy1 C1 C2 -37(5) . . . . ? C15 Dy1 C1 C2 -67(4) . . . . ? O1 C1 C2 C4 166.8(14) . . . . ? O2 C1 C2 C4 -11(2) . . . . ? Dy1 C1 C2 C4 94(4) . . . . ? O1 C1 C2 C3 -11(2) . . . . ? O2 C1 C2 C3 171.1(14) . . . . ? Dy1 C1 C2 C3 -84(5) . . . . ? C4 C2 C3 C6 3(2) . . . . ? C1 C2 C3 C6 -178.5(15) . . . . ? C3 C2 C4 C5 -2(2) . . . . ? C1 C2 C4 C5 179.8(14) . . . . ? C2 C4 C5 C7 0(2) . . . . ? C2 C4 C5 S1 176.5(12) . . . . ? C2 C3 C6 C7 -3(3) . . . . ? C4 C5 C7 C6 0(3) . . . . ? S1 C5 C7 C6 -176.5(14) . . . . ? C4 C5 C7 C8 -177.9(15) . . . . ? S1 C5 C7 C8 5.4(18) . . . . ? C3 C6 C7 C5 1(3) . . . . ? C3 C6 C7 C8 178.7(16) . . . . ? C5 C7 C8 C10 177.2(16) . . . . ? C6 C7 C8 C10 -1(3) . . . . ? C5 C7 C8 C9 -2(2) . . . . ? C6 C7 C8 C9 -179.7(17) . . . . ? C10 C8 C9 C11 -2(2) . . . . ? C7 C8 C9 C11 177.5(15) . . . . ? C10 C8 C9 S1 178.2(12) . . . . ? C7 C8 C9 S1 -2.7(17) . . . . ? C9 C8 C10 C12 2(2) . . . . ? C7 C8 C10 C12 -177.5(16) . . . . ? C8 C9 C11 C13 0(2) . . . . ? S1 C9 C11 C13 -179.5(12) . . . . ? C8 C10 C12 C13 0(2) . . . . ? C9 C11 C13 C12 1(2) . . . . ? C9 C11 C13 C14 -179.2(14) . . . . ? C10 C12 C13 C11 -1(2) . . . . ? C10 C12 C13 C14 179.1(15) . . . . ? C11 C13 C14 O4 -3(2) . . . . ? C12 C13 C14 O4 177.3(14) . . . . ? C11 C13 C14 O3 174.4(14) . . . . ? C12 C13 C14 O3 -6(2) . . . . ? C11 C13 C14 Dy2 81(7) . . . 1_454 ? C12 C13 C14 Dy2 -99(6) . . . 1_454 ? O4 C14 O3 Dy2 7.3(16) . . . 1_454 ? C13 C14 O3 Dy2 -169.3(12) . . . 1_454 ? O3 C14 O4 Dy2 -7.5(16) . . . 1_454 ? C13 C14 O4 Dy2 169.2(11) . . . 1_454 ? C4 C5 S1 O5 61.7(16) . . . . ? C7 C5 S1 O5 -121.7(12) . . . . ? C4 C5 S1 O6 -69.8(16) . . . . ? C7 C5 S1 O6 106.8(12) . . . . ? C4 C5 S1 C9 177.6(15) . . . . ? C7 C5 S1 C9 -5.9(13) . . . . ? C11 C9 S1 O5 -60.7(16) . . . . ? C8 C9 S1 O5 119.5(12) . . . . ? C11 C9 S1 O6 71.5(16) . . . . ? C8 C9 S1 O6 -108.2(12) . . . . ? C11 C9 S1 C5 -175.3(15) . . . . ? C8 C9 S1 C5 4.9(13) . . . . ? O7 Dy1 O7 C15 -178.5(10) 2_675 . . . ? O18 Dy1 O7 C15 -99.2(9) . . . . ? O19 Dy1 O7 C15 32.8(9) . . . . ? O8 Dy1 O7 C15 -2.7(8) . . . . ? O1 Dy1 O7 C15 -118.4(8) . . . . ? O15 Dy1 O7 C15 96.1(8) . . . . ? O20 Dy1 O7 C15 124.3(9) . . . . ? O2 Dy1 O7 C15 -52.3(9) . . . . ? C1 Dy1 O7 C15 -82.9(9) . . . . ? O7 Dy1 O7 Dy1 0.0 2_675 . . 2_675 ? O18 Dy1 O7 Dy1 79.3(4) . . . 2_675 ? O19 Dy1 O7 Dy1 -148.6(4) . . . 2_675 ? O8 Dy1 O7 Dy1 175.8(6) . . . 2_675 ? O1 Dy1 O7 Dy1 60.1(5) . . . 2_675 ? O15 Dy1 O7 Dy1 -85.4(4) . . . 2_675 ? O20 Dy1 O7 Dy1 -57.2(6) . . . 2_675 ? O2 Dy1 O7 Dy1 126.2(4) . . . 2_675 ? C1 Dy1 O7 Dy1 95.6(5) . . . 2_675 ? C15 Dy1 O7 Dy1 178.5(10) . . . 2_675 ? O7 Dy1 O8 C15 7.9(11) 2_675 . . . ? O18 Dy1 O8 C15 69.1(10) . . . . ? O19 Dy1 O8 C15 -143.5(10) . . . . ? O1 Dy1 O8 C15 122.7(9) . . . . ? O15 Dy1 O8 C15 -64.7(10) . . . . ? O20 Dy1 O8 C15 -113.9(10) . . . . ? O2 Dy1 O8 C15 140.4(10) . . . . ? C1 Dy1 O8 C15 129.8(10) . . . . ? O7 Dy1 O8 C15 2.9(9) . . . . ? Dy1 O8 C15 O7 -5.8(17) . . . . ? Dy1 O8 C15 C16 173.0(11) . . . . ? Dy1 O7 C15 O8 -162(8) 2_675 . . . ? Dy1 O7 C15 O8 4.7(14) . . . . ? Dy1 O7 C15 C16 20(10) 2_675 . . . ? Dy1 O7 C15 C16 -174.2(13) . . . . ? Dy1 O7 C15 Dy1 -166(9) 2_675 . . . ? O7 Dy1 C15 O8 -173.4(9) 2_675 . . . ? O18 Dy1 C15 O8 -104.4(10) . . . . ? O19 Dy1 C15 O8 34.8(10) . . . . ? O1 Dy1 C15 O8 -83.4(11) . . . . ? O15 Dy1 C15 O8 110.3(10) . . . . ? O20 Dy1 C15 O8 99.1(11) . . . . ? O2 Dy1 C15 O8 -40.3(10) . . . . ? C1 Dy1 C15 O8 -59.7(11) . . . . ? O7 Dy1 C15 O8 -174.8(15) . . . . ? O7 Dy1 C15 O7 1.5(10) 2_675 . . . ? O18 Dy1 C15 O7 70.4(8) . . . . ? O19 Dy1 C15 O7 -150.4(8) . . . . ? O8 Dy1 C15 O7 174.8(15) . . . . ? O1 Dy1 C15 O7 91.4(9) . . . . ? O15 Dy1 C15 O7 -74.9(8) . . . . ? O20 Dy1 C15 O7 -86.1(10) . . . . ? O2 Dy1 C15 O7 134.6(8) . . . . ? C1 Dy1 C15 O7 115.2(8) . . . . ? O7 Dy1 C15 C16 153(5) 2_675 . . . ? O18 Dy1 C15 C16 -138(6) . . . . ? O19 Dy1 C15 C16 1(6) . . . . ? O8 Dy1 C15 C16 -34(5) . . . . ? O1 Dy1 C15 C16 -117(5) . . . . ? O15 Dy1 C15 C16 76(5) . . . . ? O20 Dy1 C15 C16 65(6) . . . . ? O2 Dy1 C15 C16 -74(6) . . . . ? C1 Dy1 C15 C16 -94(6) . . . . ? O7 Dy1 C15 C16 151(6) . . . . ? O8 C15 C16 C17 -170.5(15) . . . . ? O7 C15 C16 C17 8(2) . . . . ? Dy1 C15 C16 C17 -141(5) . . . . ? O8 C15 C16 C18 4(2) . . . . ? O7 C15 C16 C18 -176.9(15) . . . . ? Dy1 C15 C16 C18 34(6) . . . . ? C18 C16 C17 C20 1(2) . . . . ? C15 C16 C17 C20 175.9(15) . . . . ? C17 C16 C18 C19 0(3) . . . . ? C15 C16 C18 C19 -174.8(17) . . . . ? C16 C18 C19 C21 0(3) . . . . ? C16 C17 C20 C21 -2(3) . . . . ? C16 C17 C20 S2 -177.5(13) . . . . ? C17 C20 C21 C19 2(3) . . . . ? S2 C20 C21 C19 177.8(16) . . . . ? C17 C20 C21 C22 -176.6(16) . . . . ? S2 C20 C21 C22 -1(2) . . . . ? C18 C19 C21 C20 -1(3) . . . . ? C18 C19 C21 C22 177.8(18) . . . . ? C20 C21 C22 C24 180(2) . . . . ? C19 C21 C22 C24 1(3) . . . . ? C20 C21 C22 C23 1(2) . . . . ? C19 C21 C22 C23 -177.9(19) . . . . ? C24 C22 C23 C26 -3(3) . . . . ? C21 C22 C23 C26 176.8(16) . . . . ? C24 C22 C23 S2 -179.5(16) . . . . ? C21 C22 C23 S2 0(2) . . . . ? C23 C22 C24 C25 2(3) . . . . ? C21 C22 C24 C25 -177.6(18) . . . . ? C22 C24 C25 C27 0(3) . . . . ? C22 C23 C26 C27 2(3) . . . . ? S2 C23 C26 C27 178.6(13) . . . . ? C23 C26 C27 C25 -1(3) . . . . ? C23 C26 C27 C28 178.3(15) . . . . ? C24 C25 C27 C26 0(3) . . . . ? C24 C25 C27 C28 -179.2(17) . . . . ? C26 C27 C28 O10 1(2) . . . . ? C25 C27 C28 O10 -180.0(14) . . . . ? C26 C27 C28 O9 -178.7(15) . . . . ? C25 C27 C28 O9 0(2) . . . . ? O10 C28 O9 Dy2 -121(10) . . . 2_766 ? C27 C28 O9 Dy2 59(11) . . . 2_766 ? O9 C28 O10 Dy2 13.9(18) . . . . ? C27 C28 O10 Dy2 -165.6(10) . . . . ? O9 Dy2 O10 C28 -7.8(11) 2_766 . . . ? O14 Dy2 O10 C28 58.8(10) 1_645 . . . ? O13 Dy2 O10 C28 -73.1(10) 2_676 . . . ? O21 Dy2 O10 C28 108.3(10) . . . . ? O22 Dy2 O10 C28 139.4(11) . . . . ? O4 Dy2 O10 C28 -123.7(10) 1_656 . . . ? O3 Dy2 O10 C28 -147.2(10) 1_656 . . . ? C14 Dy2 O10 C28 -135.7(10) 1_656 . . . ? C26 C23 S2 O11 -64.2(18) . . . . ? C22 C23 S2 O11 112.6(13) . . . . ? C26 C23 S2 O12 67.4(18) . . . . ? C22 C23 S2 O12 -115.8(14) . . . . ? C26 C23 S2 C20 -177.0(17) . . . . ? C22 C23 S2 C20 -0.2(14) . . . . ? C21 C20 S2 O11 -112.2(14) . . . . ? C17 C20 S2 O11 63.6(17) . . . . ? C21 C20 S2 O12 115.0(14) . . . . ? C17 C20 S2 O12 -69.3(17) . . . . ? C21 C20 S2 C23 0.6(14) . . . . ? C17 C20 S2 C23 176.4(16) . . . . ? Dy2 O13 C29 O14 12(2) 2_676 . . . ? Dy2 O13 C29 C30 -167.4(9) 2_676 . . . ? Dy2 O14 C29 O13 21(2) 1_465 . . . ? Dy2 O14 C29 C30 -159.2(10) 1_465 . . . ? O13 C29 C30 C32 -165.8(14) . . . . ? O14 C29 C30 C32 14(2) . . . . ? O13 C29 C30 C31 13(2) . . . . ? O14 C29 C30 C31 -167.2(13) . . . . ? C32 C30 C31 C33 -2(2) . . . . ? C29 C30 C31 C33 179.2(13) . . . . ? C31 C30 C32 C34 1(2) . . . . ? C29 C30 C32 C34 179.6(14) . . . . ? C30 C31 C33 C35 3(2) . . . . ? C30 C31 C33 S3 -178.4(12) . . . . ? C30 C32 C34 C35 -1(2) . . . . ? C31 C33 C35 C34 -3(2) . . . . ? S3 C33 C35 C34 178.3(13) . . . . ? C31 C33 C35 C36 178.2(15) . . . . ? S3 C33 C35 C36 -0.2(17) . . . . ? C32 C34 C35 C33 2(2) . . . . ? C32 C34 C35 C36 -179.9(16) . . . . ? C33 C35 C36 C38 -179.8(17) . . . . ? C34 C35 C36 C38 2(3) . . . . ? C33 C35 C36 C37 -1(2) . . . . ? C34 C35 C36 C37 -179.9(16) . . . . ? C38 C36 C37 C39 0(2) . . . . ? C35 C36 C37 C39 -178.1(15) . . . . ? C38 C36 C37 S3 -179.1(13) . . . . ? C35 C36 C37 S3 2.5(18) . . . . ? C37 C36 C38 C40 -1(2) . . . . ? C35 C36 C38 C40 177.5(16) . . . . ? C36 C37 C39 C41 1(2) . . . . ? S3 C37 C39 C41 -179.6(12) . . . . ? C36 C38 C40 C41 0(3) . . . . ? C37 C39 C41 C40 -2(2) . . . . ? C37 C39 C41 C42 179.6(13) . . . . ? C38 C40 C41 C39 2(2) . . . . ? C38 C40 C41 C42 -179.8(14) . . . . ? C39 C41 C42 O15 3(2) . . . . ? C40 C41 C42 O15 -174.9(13) . . . . ? C39 C41 C42 O18 -178.3(13) . . . 2_675 ? C40 C41 C42 O18 3.4(19) . . . 2_675 ? O18 C42 O15 Dy1 -20(2) 2_675 . . . ? C41 C42 O15 Dy1 157.7(9) . . . . ? O7 Dy1 O15 C42 -18.9(11) 2_675 . . . ? O18 Dy1 O15 C42 42.0(12) . . . . ? O19 Dy1 O15 C42 -176.6(12) . . . . ? O8 Dy1 O15 C42 108.4(11) . . . . ? O1 Dy1 O15 C42 -80.2(12) . . . . ? O20 Dy1 O15 C42 -100.4(12) . . . . ? O2 Dy1 O15 C42 168.2(10) . . . . ? C1 Dy1 O15 C42 -122.6(15) . . . . ? O7 Dy1 O15 C42 60.0(11) . . . . ? C15 Dy1 O15 C42 86.2(11) . . . . ? C36 C37 S3 O16 -116.0(12) . . . . ? C39 C37 S3 O16 64.6(16) . . . . ? C36 C37 S3 O17 111.0(12) . . . . ? C39 C37 S3 O17 -68.4(16) . . . . ? C36 C37 S3 C33 -2.2(13) . . . . ? C39 C37 S3 C33 178.4(15) . . . . ? C35 C33 S3 O16 114.6(12) . . . . ? C31 C33 S3 O16 -63.8(16) . . . . ? C35 C33 S3 O17 -111.1(12) . . . . ? C31 C33 S3 O17 70.5(16) . . . . ? C35 C33 S3 C37 1.4(13) . . . . ? C31 C33 S3 C37 -177.0(15) . . . . ? O7 Dy1 O18 C42 18.2(14) 2_675 . . 2_675 ? O19 Dy1 O18 C42 -162.6(13) . . . 2_675 ? O8 Dy1 O18 C42 -113.4(15) . . . 2_675 ? O1 Dy1 O18 C42 102.7(15) . . . 2_675 ? O15 Dy1 O18 C42 -45.4(16) . . . 2_675 ? O20 Dy1 O18 C42 69.4(16) . . . 2_675 ? O2 Dy1 O18 C42 159.3(15) . . . 2_675 ? C1 Dy1 O18 C42 129.7(15) . . . 2_675 ? O7 Dy1 O18 C42 -63.8(14) . . . 2_675 ? C15 Dy1 O18 C42 -90.2(15) . . . 2_675 ? O7 Dy1 O19 C44 -61.1(16) 2_675 . . . ? O18 Dy1 O19 C44 120.3(14) . . . . ? O8 Dy1 O19 C44 69.9(14) . . . . ? O1 Dy1 O19 C44 -156.8(14) . . . . ? O15 Dy1 O19 C44 -15.1(14) . . . . ? O20 Dy1 O19 C44 -91.7(14) . . . . ? O2 Dy1 O19 C44 157.3(15) . . . . ? C1 Dy1 O19 C44 179.1(14) . . . . ? O7 Dy1 O19 C44 42.9(15) . . . . ? C15 Dy1 O19 C44 56.2(14) . . . . ? O7 Dy1 O20 C45 -106.4(17) 2_675 . . . ? O18 Dy1 O20 C45 -156.3(16) . . . . ? O19 Dy1 O20 C45 58.0(17) . . . . ? O8 Dy1 O20 C45 28.3(19) . . . . ? O1 Dy1 O20 C45 169.7(18) . . . . ? O15 Dy1 O20 C45 -23.0(17) . . . . ? O2 Dy1 O20 C45 126.8(17) . . . . ? C1 Dy1 O20 C45 150.4(17) . . . . ? O7 Dy1 O20 C45 -50.1(18) . . . . ? C15 Dy1 O20 C45 -12(2) . . . . ? O9 Dy2 O21 C43 51.0(17) 2_766 . . . ? O14 Dy2 O21 C43 -28.3(17) 1_645 . . . ? O10 Dy2 O21 C43 -78.6(18) . . . . ? O13 Dy2 O21 C43 103.6(17) 2_676 . . . ? O22 Dy2 O21 C43 -109.6(17) . . . . ? O4 Dy2 O21 C43 136.5(18) 1_656 . . . ? O3 Dy2 O21 C43 -177.7(17) 1_656 . . . ? C14 Dy2 O21 C43 158.4(17) 1_656 . . . ? Dy2 O21 C43 N2 149.8(14) . . . . ? Dy1 O19 C44 N1 136.4(14) . . . . ? Dy1 O20 C45 N3 -165.7(16) . . . . ? O19 C44 N1 C49 -176.0(16) . . . . ? O19 C44 N1 C46 -1(3) . . . . ? O21 C43 N2 C48 -5(3) . . . . ? O21 C43 N2 C47 -176(2) . . . . ? O20 C45 N3 C50 179(2) . . . . ? O20 C45 N3 C51 6(4) . . . . ? O23 C52 N4 C54 -2(5) . . . . ? O23 C52 N4 C53 170(3) . . . . ? O24 C55 N5 C56 -177(3) . . . . ? O24 C55 N5 C57 3(4) . . . . ? O25 C58 N6 C60 -2(4) . . . . ? O25 C58 N6 C59 -179(2) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.913 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.209 # 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 -0.149 0.028 0.636 3324 1693 ' ' _platon_squeeze_details ; ; # Attachment 'revised_La2.cif' data_La2 _database_code_depnum_ccdc_archive 'CCDC 736840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H67 La2 N7 O25 S3' _chemical_formula_weight 1696.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.6411 1.6148 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.5011(13) _cell_length_b 16.7853(12) _cell_length_c 24.2950(17) _cell_angle_alpha 90.00 _cell_angle_beta 112.891(2) _cell_angle_gamma 90.00 _cell_volume 7326.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 5.85 _cell_measurement_theta_max 16.93 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6334 _exptl_absorpt_correction_T_max 0.7443 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.40759 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 161465 _diffrn_reflns_av_R_equivalents 0.0946 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 5.85 _diffrn_reflns_theta_max 16.93 _reflns_number_total 21354 _reflns_number_gt 12719 _reflns_threshold_expression >2sigma(I) _computing_data_collection APEX2 _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The following least-square restraints (total 66) were applied to atoms corresponding to disordered guest DMF molecules: DFIX 1.45 0.02 N4 C5 DFIX 1.45 0.02 N4 C8 DFIX 1.22 0.02 C58 O22 DFIX 2.26 0.02 N3 O22 DFIX 1.37 0.02 C30 C12 C15 C47 isor 0.005 C5, O6, C6, C8, C15, C17, O12 isor 0.005 C55, C58, N4 All the other non-hydrogen atoms were refined anisotropically. 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^)+(0.0600P)^2^+30.4768P] 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 21354 _refine_ls_number_parameters 901 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1485 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.2192 _refine_ls_wR_factor_gt 0.1693 _refine_ls_goodness_of_fit_ref 1.388 _refine_ls_restrained_S_all 1.402 _refine_ls_shift/su_max 0.011 _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 0.113202(17) 0.48420(2) 0.031491(15) 0.02100(10) Uani 1 1 d . . . La2 La 0.382445(18) 0.47805(3) -0.019118(16) 0.02827(11) Uani 1 1 d . . . S1 S 0.60346(8) 0.73756(11) -0.19846(7) 0.0302(3) Uani 1 1 d . . . S2 S 0.17717(8) 0.69600(11) -0.26297(8) 0.0329(4) Uani 1 1 d . . . S3 S 0.33319(10) 0.70654(12) 0.27047(9) 0.0397(4) Uani 1 1 d . . . O1 O 0.1541(2) 0.4833(3) -0.05168(19) 0.0263(9) Uani 1 1 d . . . O2 O 0.3496(2) 0.4707(3) 0.06934(19) 0.0296(10) Uani 1 1 d . . . O3 O 0.1217(2) 0.5957(3) 0.1099(2) 0.0314(10) Uani 1 1 d . . . O4 O 0.2462(2) 0.5124(4) 0.0796(2) 0.0405(12) Uani 1 1 d . . . O5 O 0.4233(3) 0.6082(3) 0.0360(2) 0.0383(11) Uani 1 1 d . . . O6 O 0.2577(3) 0.5379(5) -0.0547(3) 0.0524(15) Uani 1 1 d U . . O7 O 0.3779(3) 0.5858(4) -0.0942(3) 0.0485(15) Uani 1 1 d . . . O8 O 0.3037(3) 0.7776(4) 0.2355(3) 0.0561(17) Uani 1 1 d . . . O9 O 0.2208(3) 0.7631(4) -0.2308(3) 0.0486(14) Uani 1 1 d . . . O10 O 0.5082(3) 0.4577(4) 0.0659(3) 0.0504(15) Uani 1 1 d . . . O11 O 0.1630(6) 0.3459(4) 0.0241(3) 0.094(3) Uani 1 1 d . . . O12 O 0.2866(4) 0.6665(5) 0.2951(4) 0.0630(18) Uani 1 1 d U . . O13 O 0.4607(4) 0.3739(5) -0.0412(4) 0.070(2) Uani 1 1 d . . . O14 O 0.6423(3) 0.6702(4) -0.2090(3) 0.0468(14) Uani 1 1 d . . . O15 O 0.3503(6) 0.3281(6) -0.0044(6) 0.095(3) Uani 1 1 d . . . O16 O 0.0956(5) 0.6230(4) -0.0182(3) 0.061(2) Uani 1 1 d . . . O17 O 0.2112(3) 0.6438(4) -0.2920(3) 0.0429(13) Uani 1 1 d . . . O18 O 0.6455(3) 0.7933(4) -0.1530(2) 0.0449(13) Uani 1 1 d . . . O19 O 0.0097(2) 0.5393(4) 0.0674(2) 0.0420(13) Uani 1 1 d . . . O20 O 0.1560(3) 0.4345(3) 0.1399(2) 0.0442(13) Uani 1 1 d . . . O21 O 0.0301(5) 0.3741(6) 0.0339(3) 0.089(3) Uani 1 1 d . . . O22 O 0.3150(8) 0.4270(8) -0.1265(3) 0.120(4) Uani 1 1 d D . . O23 O 0.6588(6) 0.4771(6) 0.3759(5) 0.094(3) Uani 1 1 d . . . O24 O 0.1238(5) 0.9448(6) 0.0373(4) 0.084(2) Uani 1 1 d . . . O25 O 0.4525(8) 0.8486(7) -0.0535(6) 0.114(4) Uani 1 1 d . . . N1 N 0.2242(3) 0.4591(4) 0.2382(3) 0.0325(12) Uani 1 1 d . . . N2 N 0.1641(4) 0.2129(4) 0.0299(3) 0.0387(14) Uani 1 1 d . . . N3 N 0.2604(5) 0.4437(6) -0.2263(3) 0.058(2) Uani 1 1 d D . . N4 N 0.3251(7) 0.2038(8) -0.0438(5) 0.092(3) Uani 1 1 d DU . . N5 N 0.5432(4) 0.4754(4) 0.3772(3) 0.0464(16) Uani 1 1 d . . . N6 N 0.1755(4) 0.8229(5) 0.0682(3) 0.0477(16) Uani 1 1 d . . . N7 N 0.3383(5) 0.8134(6) -0.0614(4) 0.066(2) Uani 1 1 d . . . C1 C 0.3127(18) 0.8949(16) -0.0768(8) 0.158(12) Uani 1 1 d . . . H1A H 0.2609 0.8983 -0.0837 0.238 Uiso 1 1 calc R . . H1B H 0.3196 0.9104 -0.1123 0.238 Uiso 1 1 calc R . . H1C H 0.3408 0.9297 -0.0446 0.238 Uiso 1 1 calc R . . C2 C 0.1843(7) 0.4328(9) -0.2629(7) 0.081(4) Uani 1 1 d . . . H2A H 0.1768 0.4409 -0.3040 0.122 Uiso 1 1 calc R . . H2B H 0.1549 0.4705 -0.2518 0.122 Uiso 1 1 calc R . . H2C H 0.1695 0.3797 -0.2578 0.122 Uiso 1 1 calc R . . C4 C 0.2908(9) 0.7448(15) -0.0583(9) 0.117(7) Uani 1 1 d . . . H4A H 0.2410 0.7632 -0.0670 0.175 Uiso 1 1 calc R . . H4B H 0.3109 0.7222 -0.0189 0.175 Uiso 1 1 calc R . . H4C H 0.2900 0.7051 -0.0870 0.175 Uiso 1 1 calc R . . C5 C 0.2571(6) 0.2412(8) -0.0980(6) 0.078(3) Uani 1 1 d DU . . H5A H 0.2529 0.2968 -0.0906 0.117 Uiso 1 1 calc R . . H5B H 0.2120 0.2144 -0.1018 0.117 Uiso 1 1 calc R . . H5C H 0.2653 0.2350 -0.1343 0.117 Uiso 1 1 calc R . . C6 C 0.0866(13) 0.1972(14) -0.0113(11) 0.124(6) Uani 1 1 d U . . H6A H 0.0789 0.1408 -0.0166 0.187 Uiso 1 1 calc R . . H6B H 0.0775 0.2217 -0.0492 0.187 Uiso 1 1 calc R . . H6C H 0.0531 0.2190 0.0051 0.187 Uiso 1 1 calc R . . C7 C 0.3159(3) 0.5080(4) 0.0959(3) 0.0220(11) Uani 1 1 d . . . C8 C 0.3472(10) 0.1266(9) -0.0470(8) 0.101(4) Uani 1 1 d DU . . H8A H 0.3075 0.0982 -0.0773 0.152 Uiso 1 1 calc R . . H8B H 0.3591 0.1009 -0.0091 0.152 Uiso 1 1 calc R . . H8C H 0.3903 0.1268 -0.0569 0.152 Uiso 1 1 calc R . . C9 C 0.3609(3) 0.5511(4) 0.1525(3) 0.0245(12) Uani 1 1 d . . . C10 C 0.4386(3) 0.5448(4) 0.1784(3) 0.0245(12) Uani 1 1 d . . . H10 H 0.4627 0.5133 0.1600 0.029 Uiso 1 1 calc R . . C11 C 0.0621(3) 0.6441(4) -0.2427(3) 0.0252(12) Uani 1 1 d . . . C12 C -0.0412(3) 0.7141(4) -0.3312(3) 0.0283(13) Uani 1 1 d D . . H12 H -0.0799 0.6923 -0.3228 0.034 Uiso 1 1 calc R . . C13 C 0.1445(3) 0.5644(4) -0.1353(3) 0.0281(13) Uani 1 1 d . . . C14 C 0.0256(3) 0.6040(4) -0.2126(3) 0.0274(13) Uani 1 1 d . . . H14 H -0.0262 0.6039 -0.2275 0.033 Uiso 1 1 calc R . . C15 C 0.3893(4) 0.7193(5) -0.2339(3) 0.0345(14) Uani 1 1 d DU . . H15 H 0.3461 0.7392 -0.2635 0.041 Uiso 1 1 calc R . . C16 C 0.1132(8) 0.7938(7) 0.0796(8) 0.082(4) Uani 1 1 d . . . H16A H 0.1224 0.7398 0.0935 0.123 Uiso 1 1 calc R . . H16B H 0.0692 0.7958 0.0435 0.123 Uiso 1 1 calc R . . H16C H 0.1061 0.8264 0.1095 0.123 Uiso 1 1 calc R . . C17 C 0.3702(8) 0.2603(9) -0.0084(6) 0.077(3) Uani 1 1 d U . . H17 H 0.4194 0.2467 0.0143 0.092 Uiso 1 1 calc R . . C18 C 0.3095(8) 0.4642(10) -0.2564(10) 0.102(6) Uani 1 1 d . . . H18A H 0.2812 0.4670 -0.2987 0.153 Uiso 1 1 calc R . . H18B H 0.3474 0.4243 -0.2482 0.153 Uiso 1 1 calc R . . H18C H 0.3323 0.5150 -0.2423 0.153 Uiso 1 1 calc R . . C20 C 0.4807(3) 0.5847(4) 0.2312(3) 0.0252(12) Uani 1 1 d . . . H20 H 0.5321 0.5785 0.2484 0.030 Uiso 1 1 calc R . . C21 C 0.4757(3) 0.7821(4) -0.2791(3) 0.0252(12) Uani 1 1 d . . . C22 C 0.5519(4) 0.6958(4) 0.3494(3) 0.0267(12) Uani 1 1 d . . . H22 H 0.5894 0.6684 0.3427 0.032 Uiso 1 1 calc R . . C23 C 0.4500(3) 0.6412(4) -0.1430(3) 0.0291(13) Uani 1 1 d . . . C24 C 0.5220(3) 0.7065(4) -0.1883(3) 0.0246(12) Uani 1 1 d . . . C25 C 0.0663(3) 0.5635(4) -0.1595(3) 0.0292(13) Uani 1 1 d . . . H25 H 0.0412 0.5355 -0.1400 0.035 Uiso 1 1 calc R . . C26 C 0.0320(3) 0.6942(4) -0.2970(3) 0.0256(12) Uani 1 1 d . . . C27 C 0.4585(3) 0.7360(4) -0.2346(3) 0.0251(12) Uani 1 1 d . . . C28 C 0.4450(3) 0.6338(4) 0.2578(3) 0.0248(12) Uani 1 1 d . . . C29 C 0.2391(8) 0.7715(8) 0.0799(6) 0.076(3) Uani 1 1 d . . . H29A H 0.2297 0.7206 0.0936 0.115 Uiso 1 1 calc R . . H29B H 0.2822 0.7952 0.1099 0.115 Uiso 1 1 calc R . . H29C H 0.2476 0.7646 0.0438 0.115 Uiso 1 1 calc R . . C30 C -0.0560(3) 0.7678(4) -0.3788(3) 0.0315(14) Uani 1 1 d D . . H30 H -0.1049 0.7828 -0.4012 0.038 Uiso 1 1 calc R . . C31 C 0.5798(3) 0.8270(4) -0.3035(3) 0.0310(14) Uani 1 1 d . . . H31 H 0.6307 0.8282 -0.2945 0.037 Uiso 1 1 calc R . . C32 C 0.5133(5) 0.7906(4) 0.4082(3) 0.0348(15) Uani 1 1 d . . . C33 C 0.4256(3) 0.8184(5) -0.3307(3) 0.0312(14) Uani 1 1 d . . . H33 H 0.3747 0.8154 -0.3400 0.037 Uiso 1 1 calc R . . C34 C 0.3243(3) 0.5997(4) 0.1792(3) 0.0272(12) Uani 1 1 d . . . H34 H 0.2728 0.6051 0.1626 0.033 Uiso 1 1 calc R . . C36 C 0.6123(6) 0.5001(6) 0.3953(5) 0.053(2) Uani 1 1 d . . . H36 H 0.6277 0.5382 0.4255 0.064 Uiso 1 1 calc R . . C37 C 0.4921(6) 0.5055(6) 0.4022(5) 0.056(2) Uani 1 1 d . . . H37A H 0.4444 0.4805 0.3827 0.084 Uiso 1 1 calc R . . H37B H 0.4869 0.5621 0.3964 0.084 Uiso 1 1 calc R . . H37C H 0.5110 0.4938 0.4442 0.084 Uiso 1 1 calc R . . C38 C 0.1745(6) 0.8976(7) 0.0484(4) 0.059(2) Uani 1 1 d . . . H38 H 0.2165 0.9148 0.0425 0.071 Uiso 1 1 calc R . . C39 C 0.5141(7) 0.4140(7) 0.3308(5) 0.064(3) Uani 1 1 d . . . H39A H 0.4626 0.4042 0.3231 0.096 Uiso 1 1 calc R . . H39B H 0.5420 0.3657 0.3443 0.096 Uiso 1 1 calc R . . H39C H 0.5186 0.4319 0.2949 0.096 Uiso 1 1 calc R . . C40 C 0.4078(7) 0.7989(7) -0.0509(6) 0.068(3) Uani 1 1 d . . . H40 H 0.4248 0.7471 -0.0406 0.081 Uiso 1 1 calc R . . C41 C 0.5203(3) 0.6591(4) -0.1428(3) 0.0258(12) Uani 1 1 d . . . H41 H 0.5637 0.6396 -0.1133 0.031 Uiso 1 1 calc R . . C42 C 0.1825(3) 0.6029(4) -0.1657(3) 0.0300(14) Uani 1 1 d . . . H42 H 0.2342 0.6026 -0.1510 0.036 Uiso 1 1 calc R . . C43 C 0.4778(3) 0.6841(4) 0.3121(3) 0.0256(12) Uani 1 1 d . . . C44 C 0.0012(4) 0.7993(5) -0.3933(3) 0.0345(15) Uani 1 1 d . . . C45 C 0.1413(3) 0.6416(4) -0.2184(3) 0.0280(13) Uani 1 1 d . . . C46 C 0.5298(4) 0.8643(5) -0.3543(3) 0.0325(14) Uani 1 1 d . . . C47 C 0.3860(4) 0.6721(5) -0.1881(3) 0.0393(17) Uani 1 1 d D . . H47 H 0.3398 0.6605 -0.1873 0.047 Uiso 1 1 calc R . . C48 C 0.1895(4) 0.2851(5) 0.0459(4) 0.0395(16) Uani 1 1 d . . . H48 H 0.2345 0.2886 0.0787 0.047 Uiso 1 1 calc R . . C49 C 0.4871(4) 0.6385(5) 0.0584(4) 0.0451(19) Uani 1 1 d . . . C50 C 0.5516(3) 0.7879(4) -0.2665(3) 0.0283(13) Uani 1 1 d . . . C51 C 0.4401(3) 0.5881(5) -0.0969(3) 0.0362(16) Uani 1 1 d . . . C52 C 0.3669(3) 0.6392(4) 0.2307(3) 0.0270(12) Uani 1 1 d . . . C53 C 0.4231(4) 0.7260(4) 0.3246(3) 0.0297(13) Uani 1 1 d . . . C54 C 0.0881(3) 0.7267(4) -0.3127(3) 0.0286(13) Uani 1 1 d . . . C55 C 0.1859(10) 0.1410(9) 0.0624(8) 0.094(4) Uani 1 1 d U . . H55A H 0.1551 0.0982 0.0398 0.141 Uiso 1 1 calc R . . H55B H 0.1805 0.1460 0.0998 0.141 Uiso 1 1 calc R . . H55C H 0.2370 0.1299 0.0696 0.141 Uiso 1 1 calc R . . C56 C 0.0298(7) 0.6467(5) -0.0447(3) 0.058(3) Uani 1 1 d . . . C57 C 0.2953(5) 0.4553(6) 0.2882(3) 0.048(2) Uani 1 1 d . . . H57A H 0.2897 0.4732 0.3237 0.072 Uiso 1 1 calc R . . H57B H 0.3304 0.4888 0.2804 0.072 Uiso 1 1 calc R . . H57C H 0.3131 0.4014 0.2936 0.072 Uiso 1 1 calc R . . C58 C 0.2647(10) 0.4279(11) -0.1696(7) 0.100(5) Uani 1 1 d DU . . H58 H 0.2197 0.4162 -0.1665 0.120 Uiso 1 1 calc R . . C59 C 0.1626(4) 0.4842(7) 0.2526(4) 0.052(2) Uani 1 1 d . . . H59A H 0.1802 0.4971 0.2943 0.078 Uiso 1 1 calc R . . H59B H 0.1267 0.4420 0.2436 0.078 Uiso 1 1 calc R . . H59C H 0.1399 0.5304 0.2293 0.078 Uiso 1 1 calc R . . C60 C 0.5696(4) 0.7490(4) 0.3967(3) 0.0331(14) Uani 1 1 d . . . H60 H 0.6192 0.7574 0.4213 0.040 Uiso 1 1 calc R . . C61 C 0.0749(4) 0.7780(5) -0.3600(3) 0.0348(15) Uani 1 1 d . . . H61 H 0.1136 0.7976 -0.3693 0.042 Uiso 1 1 calc R . . C62 C 0.2168(4) 0.4375(4) 0.1839(3) 0.0367(15) Uani 1 1 d . . . H62 H 0.2596 0.4237 0.1780 0.044 Uiso 1 1 calc R . . C63 C 0.4525(4) 0.8591(5) -0.3680(3) 0.0339(15) Uani 1 1 d . . . H63 H 0.4191 0.8832 -0.4024 0.041 Uiso 1 1 calc R . . C64 C 0.0560(4) 0.5884(5) 0.1049(3) 0.0327(14) Uani 1 1 d . . . C65 C 0.4388(5) 0.7777(4) 0.3715(3) 0.0373(16) Uani 1 1 d . . . H65 H 0.4009 0.8036 0.3786 0.045 Uiso 1 1 calc R . . C66 C 0.1871(4) 0.5261(5) -0.0761(3) 0.0346(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01226(15) 0.02519(17) 0.02148(16) 0.00114(13) 0.00214(11) -0.00224(12) La2 0.01405(16) 0.0467(2) 0.02273(18) -0.00053(15) 0.00571(13) -0.00088(14) S1 0.0117(6) 0.0435(9) 0.0337(8) 0.0054(7) 0.0070(6) 0.0017(6) S2 0.0120(6) 0.0451(10) 0.0404(9) 0.0093(7) 0.0089(6) 0.0035(6) S3 0.0249(8) 0.0440(10) 0.0548(11) -0.0170(8) 0.0206(8) 0.0038(7) O1 0.025(2) 0.030(2) 0.026(2) 0.0071(18) 0.0121(17) 0.0090(18) O2 0.0132(18) 0.055(3) 0.0212(19) 0.0018(19) 0.0074(15) 0.0050(18) O3 0.018(2) 0.044(3) 0.036(2) 0.000(2) 0.0152(18) 0.0022(18) O4 0.0117(19) 0.072(4) 0.034(2) -0.016(2) 0.0050(17) 0.003(2) O5 0.028(2) 0.046(3) 0.034(3) 0.003(2) 0.004(2) -0.013(2) O6 0.023(2) 0.090(4) 0.046(3) 0.016(3) 0.015(2) 0.006(2) O7 0.022(2) 0.084(4) 0.040(3) 0.026(3) 0.013(2) 0.003(3) O8 0.041(3) 0.054(4) 0.054(3) -0.018(3) -0.002(3) 0.026(3) O9 0.020(2) 0.057(4) 0.055(3) 0.015(3) -0.001(2) -0.005(2) O10 0.029(3) 0.084(4) 0.040(3) 0.029(3) 0.015(2) 0.021(3) O11 0.137(8) 0.031(3) 0.056(4) -0.006(3) -0.025(5) 0.020(4) O12 0.052(3) 0.076(4) 0.083(4) -0.023(3) 0.050(3) -0.011(3) O13 0.040(3) 0.075(5) 0.095(5) -0.049(4) 0.028(3) -0.020(3) O14 0.031(3) 0.052(3) 0.066(4) 0.016(3) 0.029(3) 0.018(2) O15 0.099(7) 0.061(5) 0.152(9) -0.012(5) 0.077(7) -0.011(5) O16 0.113(6) 0.040(3) 0.039(3) 0.016(3) 0.038(4) 0.039(4) O17 0.022(2) 0.064(4) 0.049(3) 0.023(3) 0.021(2) 0.018(2) O18 0.023(2) 0.061(4) 0.041(3) 0.002(3) 0.003(2) -0.016(2) O19 0.013(2) 0.084(4) 0.025(2) -0.011(2) 0.0038(17) 0.003(2) O20 0.047(3) 0.041(3) 0.024(2) 0.008(2) -0.010(2) -0.013(2) O21 0.097(6) 0.101(6) 0.041(3) 0.018(4) -0.003(4) -0.067(5) O22 0.168(11) 0.134(9) 0.028(4) -0.025(4) 0.006(5) -0.005(8) O23 0.081(6) 0.108(7) 0.123(8) -0.051(6) 0.071(6) -0.032(5) O24 0.075(5) 0.089(6) 0.091(6) 0.033(5) 0.035(5) 0.028(5) O25 0.126(9) 0.082(7) 0.147(10) -0.012(6) 0.067(8) -0.033(6) N1 0.028(3) 0.034(3) 0.027(3) 0.003(2) 0.001(2) -0.002(2) N2 0.042(3) 0.029(3) 0.032(3) 0.002(2) 0.001(3) 0.000(3) N3 0.059(5) 0.077(5) 0.025(3) -0.007(3) 0.001(3) 0.031(4) N4 0.083(5) 0.102(5) 0.093(5) -0.001(4) 0.036(4) 0.007(4) N5 0.048(4) 0.042(4) 0.046(4) -0.003(3) 0.015(3) -0.007(3) N6 0.037(4) 0.062(5) 0.046(4) 0.007(3) 0.018(3) 0.002(3) N7 0.052(5) 0.075(6) 0.060(5) -0.004(4) 0.010(4) 0.016(4) C1 0.22(3) 0.159(19) 0.075(10) 0.019(11) 0.031(12) 0.13(2) C2 0.056(7) 0.082(8) 0.117(10) 0.027(7) 0.048(7) 0.016(6) C4 0.058(8) 0.183(19) 0.115(12) -0.043(12) 0.041(8) -0.048(10) C5 0.054(4) 0.086(5) 0.083(5) -0.032(4) 0.013(4) 0.010(4) C6 0.120(7) 0.115(7) 0.128(7) -0.010(5) 0.036(5) 0.001(5) C7 0.014(2) 0.030(3) 0.022(3) -0.001(2) 0.007(2) -0.002(2) C8 0.107(6) 0.091(6) 0.098(6) 0.001(4) 0.030(4) -0.023(4) C9 0.014(2) 0.033(3) 0.027(3) -0.001(2) 0.007(2) 0.004(2) C10 0.013(2) 0.037(3) 0.023(3) -0.005(2) 0.007(2) 0.003(2) C11 0.014(2) 0.032(3) 0.028(3) -0.008(2) 0.005(2) 0.001(2) C12 0.014(3) 0.031(3) 0.039(3) -0.010(3) 0.009(2) 0.001(2) C13 0.015(3) 0.040(4) 0.029(3) -0.008(3) 0.009(2) 0.004(2) C14 0.011(2) 0.041(4) 0.028(3) -0.002(3) 0.005(2) 0.003(2) C15 0.014(2) 0.047(3) 0.038(3) 0.011(3) 0.006(2) 0.000(2) C16 0.092(9) 0.045(5) 0.143(12) -0.025(6) 0.083(9) -0.023(6) C17 0.067(5) 0.079(5) 0.085(5) -0.008(4) 0.031(4) -0.003(4) C18 0.068(8) 0.091(9) 0.167(15) -0.075(10) 0.069(9) -0.025(7) C20 0.017(3) 0.033(3) 0.025(3) -0.005(2) 0.008(2) 0.003(2) C21 0.011(2) 0.034(3) 0.029(3) 0.003(2) 0.006(2) 0.000(2) C22 0.023(3) 0.029(3) 0.025(3) -0.004(2) 0.005(2) 0.001(2) C23 0.020(3) 0.042(4) 0.026(3) 0.010(3) 0.010(2) 0.006(2) C24 0.009(2) 0.030(3) 0.034(3) -0.001(2) 0.008(2) 0.000(2) C25 0.016(3) 0.044(4) 0.028(3) -0.001(3) 0.008(2) 0.005(2) C26 0.014(2) 0.032(3) 0.030(3) -0.005(2) 0.007(2) 0.002(2) C27 0.012(2) 0.034(3) 0.028(3) 0.005(2) 0.008(2) 0.004(2) C28 0.018(3) 0.029(3) 0.027(3) -0.002(2) 0.010(2) -0.002(2) C29 0.073(7) 0.071(7) 0.073(7) 0.004(6) 0.014(6) 0.025(6) C30 0.015(3) 0.040(4) 0.035(3) 0.003(3) 0.005(2) 0.009(2) C31 0.013(3) 0.044(4) 0.035(3) 0.003(3) 0.008(2) -0.001(2) C32 0.055(4) 0.025(3) 0.025(3) 0.000(2) 0.016(3) 0.007(3) C33 0.014(3) 0.049(4) 0.031(3) 0.010(3) 0.009(2) 0.002(3) C34 0.017(3) 0.032(3) 0.035(3) -0.002(3) 0.013(2) 0.002(2) C36 0.053(5) 0.055(5) 0.054(5) -0.012(4) 0.024(4) -0.012(4) C37 0.052(5) 0.051(5) 0.067(6) -0.002(4) 0.026(5) -0.006(4) C38 0.049(5) 0.078(7) 0.053(5) 0.023(5) 0.024(4) 0.012(5) C39 0.068(7) 0.056(6) 0.064(6) -0.014(5) 0.022(5) -0.018(5) C40 0.070(7) 0.051(6) 0.076(7) -0.010(5) 0.022(6) -0.001(5) C41 0.014(2) 0.036(3) 0.026(3) 0.006(2) 0.007(2) 0.004(2) C42 0.011(2) 0.049(4) 0.029(3) 0.002(3) 0.006(2) 0.004(2) C43 0.025(3) 0.026(3) 0.028(3) -0.003(2) 0.013(2) -0.001(2) C44 0.020(3) 0.046(4) 0.034(3) 0.002(3) 0.008(3) 0.007(3) C45 0.011(2) 0.041(4) 0.031(3) 0.001(3) 0.007(2) 0.005(2) C46 0.022(3) 0.052(4) 0.028(3) 0.000(3) 0.014(2) -0.002(3) C47 0.015(3) 0.056(5) 0.048(4) 0.017(4) 0.014(3) 0.007(3) C48 0.033(4) 0.033(4) 0.043(4) 0.002(3) 0.005(3) 0.002(3) C49 0.023(3) 0.055(5) 0.054(5) -0.018(4) 0.011(3) -0.012(3) C50 0.015(3) 0.039(4) 0.030(3) 0.000(3) 0.007(2) 0.002(2) C51 0.016(3) 0.063(5) 0.028(3) 0.020(3) 0.007(2) 0.006(3) C52 0.020(3) 0.028(3) 0.037(3) -0.005(3) 0.015(2) 0.000(2) C53 0.030(3) 0.027(3) 0.035(3) -0.002(3) 0.016(3) 0.004(2) C54 0.015(3) 0.035(3) 0.034(3) 0.005(3) 0.008(2) 0.008(2) C55 0.094(6) 0.078(5) 0.093(6) 0.007(4) 0.018(4) -0.006(4) C56 0.107(8) 0.027(4) 0.024(3) -0.002(3) 0.009(4) -0.030(5) C57 0.033(4) 0.066(5) 0.029(4) -0.005(3) -0.004(3) 0.010(4) C58 0.101(6) 0.100(6) 0.100(6) -0.007(4) 0.040(5) 0.012(4) C59 0.026(4) 0.092(7) 0.039(4) 0.024(4) 0.014(3) 0.000(4) C60 0.041(4) 0.028(3) 0.027(3) -0.003(3) 0.010(3) -0.001(3) C61 0.018(3) 0.041(4) 0.044(4) 0.009(3) 0.011(3) 0.007(3) C62 0.037(4) 0.033(4) 0.028(3) 0.003(3) -0.001(3) 0.003(3) C63 0.018(3) 0.057(5) 0.026(3) 0.005(3) 0.008(2) -0.003(3) C64 0.024(3) 0.052(4) 0.027(3) 0.006(3) 0.015(3) 0.005(3) C65 0.049(4) 0.033(4) 0.035(4) 0.000(3) 0.022(3) 0.007(3) C66 0.039(4) 0.050(4) 0.015(3) 0.002(3) 0.010(2) 0.011(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 La1 O4 2.441(5) . ? La1 O1 2.444(4) . ? La1 O21 2.474(7) . ? La1 O11 2.550(7) . ? La1 O20 2.572(5) . ? La1 O16 2.585(6) . ? La1 O3 2.629(5) . ? La1 O19 2.657(5) . ? La1 O19 2.682(5) 3_565 ? La1 C64 3.005(7) . ? La1 La1 4.1061(7) 3_565 ? La2 O6 2.457(6) . ? La2 O2 2.473(4) . ? La2 O13 2.512(7) . ? La2 O5 2.524(5) . ? La2 O10 2.540(5) . ? La2 O7 2.546(5) . ? La2 O22 2.569(8) . ? La2 O15 2.652(9) . ? La2 O10 2.982(6) 3_665 ? S1 O18 1.436(6) . ? S1 O14 1.438(6) . ? S1 C24 1.779(6) . ? S1 C50 1.779(7) . ? S2 O17 1.439(6) . ? S2 O9 1.444(6) . ? S2 C45 1.755(7) . ? S2 C54 1.764(6) . ? S3 O12 1.434(7) . ? S3 O8 1.447(7) . ? S3 C53 1.765(7) . ? S3 C52 1.771(6) . ? O1 C66 1.257(9) . ? O2 C7 1.253(7) . ? O3 C64 1.245(8) . ? O4 C7 1.261(7) . ? O5 C49 1.256(9) . ? O6 C66 1.284(9) . ? O7 C51 1.240(8) . ? O10 C51 1.259(9) 3_665 ? O10 La2 2.982(6) 3_665 ? O11 C48 1.173(10) . ? O13 C49 1.257(10) 3_665 ? O15 C17 1.218(17) . ? O16 C56 1.255(14) . ? O19 C64 1.298(9) . ? O19 La1 2.682(5) 3_565 ? O20 C62 1.251(8) . ? O21 C56 1.339(15) 3_565 ? O22 C58 1.123(15) . ? O23 C36 1.235(13) . ? O24 C38 1.213(13) . ? O25 C40 1.226(16) . ? N1 C62 1.322(10) . ? N1 C59 1.437(11) . ? N1 C57 1.446(9) . ? N2 C48 1.308(10) . ? N2 C55 1.415(17) . ? N2 C6 1.48(2) . ? N3 C58 1.37(2) . ? N3 C2 1.414(17) . ? N3 C18 1.455(19) . ? N4 C17 1.351(19) . ? N4 C8 1.377(15) . ? N4 C5 1.590(14) . ? N5 C36 1.312(12) . ? N5 C37 1.446(13) . ? N5 C39 1.468(13) . ? N6 C38 1.342(14) . ? N6 C16 1.432(13) . ? N6 C29 1.446(14) . ? N7 C40 1.301(16) . ? N7 C1 1.45(2) . ? N7 C4 1.50(2) . ? C7 C9 1.500(9) . ? C9 C34 1.397(8) . ? C9 C10 1.400(8) . ? C10 C20 1.396(9) . ? C11 C14 1.380(9) . ? C11 C45 1.423(8) . ? C11 C26 1.480(9) . ? C12 C26 1.384(8) . ? C12 C30 1.407(9) . ? C13 C42 1.392(9) . ? C13 C25 1.406(8) . ? C13 C66 1.497(9) . ? C14 C25 1.398(9) . ? C15 C27 1.383(8) . ? C15 C47 1.388(9) . ? C20 C28 1.391(8) . ? C21 C33 1.392(9) . ? C21 C50 1.394(8) . ? C21 C27 1.472(9) . ? C22 C60 1.388(9) . ? C22 C43 1.389(9) . ? C23 C47 1.401(9) . ? C23 C41 1.401(8) . ? C23 C51 1.502(9) . ? C24 C41 1.372(9) . ? C24 C27 1.400(8) . ? C26 C54 1.400(9) . ? C28 C52 1.408(8) . ? C28 C43 1.484(9) . ? C30 C44 1.397(10) . ? C31 C50 1.388(9) . ? C31 C46 1.390(10) . ? C32 C65 1.395(12) . ? C32 C60 1.416(11) . ? C32 C56 1.495(11) 4_676 ? C33 C63 1.390(9) . ? C34 C52 1.374(9) . ? C42 C45 1.381(9) . ? C43 C53 1.406(9) . ? C44 C61 1.394(9) . ? C44 C49 1.515(11) 4_575 ? C46 C63 1.415(9) . ? C46 C64 1.506(10) 4_675 ? C49 O13 1.257(10) 3_665 ? C49 C44 1.515(11) 4_676 ? C51 O10 1.259(9) 3_665 ? C53 C65 1.369(10) . ? C54 C61 1.378(10) . ? C56 O21 1.339(15) 3_565 ? C56 C32 1.495(11) 4_575 ? C64 C46 1.506(10) 4_576 ? 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 O4 La1 O1 76.67(16) . . ? O4 La1 O21 135.9(3) . . ? O1 La1 O21 116.3(3) . . ? O4 La1 O11 81.2(3) . . ? O1 La1 O11 71.4(3) . . ? O21 La1 O11 66.0(4) . . ? O4 La1 O20 73.23(19) . . ? O1 La1 O20 139.82(18) . . ? O21 La1 O20 71.83(19) . . ? O11 La1 O20 78.2(2) . . ? O4 La1 O16 88.4(3) . . ? O1 La1 O16 69.28(17) . . ? O21 La1 O16 135.6(3) . . ? O11 La1 O16 140.6(3) . . ? O20 La1 O16 134.56(19) . . ? O4 La1 O3 76.06(15) . . ? O1 La1 O3 130.89(15) . . ? O21 La1 O3 111.8(3) . . ? O11 La1 O3 141.34(19) . . ? O20 La1 O3 65.49(17) . . ? O16 La1 O3 69.90(17) . . ? O4 La1 O19 125.20(16) . . ? O1 La1 O19 143.85(15) . . ? O21 La1 O19 70.3(3) . . ? O11 La1 O19 134.3(3) . . ? O20 La1 O19 76.25(19) . . ? O16 La1 O19 81.9(2) . . ? O3 La1 O19 49.92(15) . . ? O4 La1 O19 150.50(16) . 3_565 ? O1 La1 O19 73.97(15) . 3_565 ? O21 La1 O19 63.0(2) . 3_565 ? O11 La1 O19 92.0(2) . 3_565 ? O20 La1 O19 133.66(18) . 3_565 ? O16 La1 O19 78.7(2) . 3_565 ? O3 La1 O19 122.43(16) . 3_565 ? O19 La1 O19 79.46(16) . 3_565 ? O4 La1 C64 99.98(18) . . ? O1 La1 C64 144.10(18) . . ? O21 La1 C64 91.3(3) . . ? O11 La1 C64 144.2(3) . . ? O20 La1 C64 68.2(2) . . ? O16 La1 C64 74.93(19) . . ? O3 La1 C64 24.38(16) . . ? O19 La1 C64 25.56(18) . . ? O19 La1 C64 102.04(17) 3_565 . ? O4 La1 La1 160.30(14) . 3_565 ? O1 La1 La1 110.00(10) . 3_565 ? O21 La1 La1 59.0(3) . 3_565 ? O11 La1 La1 118.4(2) . 3_565 ? O20 La1 La1 107.29(14) . 3_565 ? O16 La1 La1 77.4(2) . 3_565 ? O3 La1 La1 86.20(10) . 3_565 ? O19 La1 La1 39.96(10) . 3_565 ? O19 La1 La1 39.50(10) 3_565 3_565 ? C64 La1 La1 63.42(13) . 3_565 ? O6 La2 O2 76.76(17) . . ? O6 La2 O13 144.1(2) . . ? O2 La2 O13 122.4(3) . . ? O6 La2 O5 84.1(2) . . ? O2 La2 O5 73.58(17) . . ? O13 La2 O5 128.52(19) . . ? O6 La2 O10 148.4(2) . . ? O2 La2 O10 77.35(16) . . ? O13 La2 O10 66.8(2) . . ? O5 La2 O10 71.3(2) . . ? O6 La2 O7 72.75(18) . . ? O2 La2 O7 135.22(19) . . ? O13 La2 O7 101.3(3) . . ? O5 La2 O7 71.4(2) . . ? O10 La2 O7 115.57(19) . . ? O6 La2 O22 74.5(4) . . ? O2 La2 O22 131.5(4) . . ? O13 La2 O22 70.4(4) . . ? O5 La2 O22 139.4(3) . . ? O10 La2 O22 137.0(4) . . ? O7 La2 O22 69.4(3) . . ? O6 La2 O15 100.5(3) . . ? O2 La2 O15 71.4(3) . . ? O13 La2 O15 64.1(3) . . ? O5 La2 O15 142.4(3) . . ? O10 La2 O15 88.1(3) . . ? O7 La2 O15 145.8(3) . . ? O22 La2 O15 76.4(4) . . ? O6 La2 O10 118.34(18) . 3_665 ? O2 La2 O10 144.58(17) . 3_665 ? O13 La2 O10 65.5(2) . 3_665 ? O5 La2 O10 76.36(19) . 3_665 ? O10 La2 O10 75.60(17) . 3_665 ? O7 La2 O10 45.61(16) . 3_665 ? O22 La2 O10 83.9(4) . 3_665 ? O15 La2 O10 129.5(2) . 3_665 ? O18 S1 O14 117.8(4) . . ? O18 S1 C24 110.9(3) . . ? O14 S1 C24 110.8(3) . . ? O18 S1 C50 110.7(3) . . ? O14 S1 C50 110.8(3) . . ? C24 S1 C50 93.0(3) . . ? O17 S2 O9 117.0(4) . . ? O17 S2 C45 110.8(3) . . ? O9 S2 C45 111.3(4) . . ? O17 S2 C54 111.3(3) . . ? O9 S2 C54 111.0(3) . . ? C45 S2 C54 92.9(3) . . ? O12 S3 O8 117.3(4) . . ? O12 S3 C53 112.6(4) . . ? O8 S3 C53 109.7(4) . . ? O12 S3 C52 111.0(4) . . ? O8 S3 C52 110.7(4) . . ? C53 S3 C52 93.0(3) . . ? C66 O1 La1 141.2(4) . . ? C7 O2 La2 142.0(4) . . ? C64 O3 La1 95.0(4) . . ? C7 O4 La1 162.4(5) . . ? C49 O5 La2 129.5(5) . . ? C66 O6 La2 146.9(6) . . ? C51 O7 La2 107.3(4) . . ? C51 O10 La2 149.8(6) 3_665 . ? C51 O10 La2 85.6(4) 3_665 3_665 ? La2 O10 La2 104.40(17) . 3_665 ? C48 O11 La1 150.9(8) . . ? C49 O13 La2 145.4(7) 3_665 . ? C17 O15 La2 140.9(9) . . ? C56 O16 La1 116.7(6) . . ? C64 O19 La1 92.4(4) . . ? C64 O19 La1 149.0(5) . 3_565 ? La1 O19 La1 100.54(16) . 3_565 ? C62 O20 La1 133.2(5) . . ? C56 O21 La1 146.1(9) 3_565 . ? C58 O22 La2 149.3(13) . . ? C62 N1 C59 123.0(6) . . ? C62 N1 C57 121.6(7) . . ? C59 N1 C57 115.3(6) . . ? C48 N2 C55 128.9(9) . . ? C48 N2 C6 122.4(11) . . ? C55 N2 C6 103.4(12) . . ? C58 N3 C2 104.1(11) . . ? C58 N3 C18 139.1(12) . . ? C2 N3 C18 116.8(11) . . ? C17 N4 C8 123.8(13) . . ? C17 N4 C5 112.1(11) . . ? C8 N4 C5 120.2(12) . . ? C36 N5 C37 122.4(8) . . ? C36 N5 C39 121.3(8) . . ? C37 N5 C39 116.4(8) . . ? C38 N6 C16 119.6(9) . . ? C38 N6 C29 121.3(9) . . ? C16 N6 C29 119.2(10) . . ? C40 N7 C1 116.9(18) . . ? C40 N7 C4 117.7(12) . . ? C1 N7 C4 125.4(18) . . ? O2 C7 O4 125.8(6) . . ? O2 C7 C9 118.5(5) . . ? O4 C7 C9 115.7(5) . . ? C34 C9 C10 119.6(6) . . ? C34 C9 C7 119.0(5) . . ? C10 C9 C7 121.4(5) . . ? C20 C10 C9 121.6(5) . . ? C14 C11 C45 117.8(6) . . ? C14 C11 C26 130.0(5) . . ? C45 C11 C26 112.1(5) . . ? C26 C12 C30 118.8(6) . . ? C42 C13 C25 119.8(6) . . ? C42 C13 C66 119.9(6) . . ? C25 C13 C66 120.3(6) . . ? C11 C14 C25 120.0(5) . . ? C27 C15 C47 118.3(6) . . ? O15 C17 N4 123.8(13) . . ? C28 C20 C10 119.4(5) . . ? C33 C21 C50 118.8(6) . . ? C33 C21 C27 127.6(5) . . ? C50 C21 C27 113.6(5) . . ? C60 C22 C43 119.4(6) . . ? C47 C23 C41 119.7(6) . . ? C47 C23 C51 118.0(5) . . ? C41 C23 C51 122.3(5) . . ? C41 C24 C27 124.2(5) . . ? C41 C24 S1 125.7(4) . . ? C27 C24 S1 110.1(5) . . ? C14 C25 C13 121.1(6) . . ? C12 C26 C54 118.4(6) . . ? C12 C26 C11 129.1(6) . . ? C54 C26 C11 112.4(5) . . ? C15 C27 C24 118.7(6) . . ? C15 C27 C21 128.1(5) . . ? C24 C27 C21 113.2(5) . . ? C20 C28 C52 117.8(6) . . ? C20 C28 C43 129.1(5) . . ? C52 C28 C43 113.1(5) . . ? C44 C30 C12 121.4(6) . . ? C50 C31 C46 118.1(6) . . ? C65 C32 C60 119.5(6) . . ? C65 C32 C56 117.3(7) . 4_676 ? C60 C32 C56 123.1(8) . 4_676 ? C63 C33 C21 119.3(6) . . ? C52 C34 C9 117.9(5) . . ? O23 C36 N5 125.7(9) . . ? O24 C38 N6 125.9(10) . . ? O25 C40 N7 124.8(12) . . ? C24 C41 C23 116.8(5) . . ? C45 C42 C13 118.3(5) . . ? C22 C43 C53 118.2(6) . . ? C22 C43 C28 129.7(6) . . ? C53 C43 C28 112.0(5) . . ? C61 C44 C30 120.0(7) . . ? C61 C44 C49 117.5(6) . 4_575 ? C30 C44 C49 122.3(6) . 4_575 ? C42 C45 C11 122.9(6) . . ? C42 C45 S2 126.1(5) . . ? C11 C45 S2 111.0(5) . . ? C31 C46 C63 119.7(6) . . ? C31 C46 C64 121.5(6) . 4_675 ? C63 C46 C64 118.9(6) . 4_675 ? C15 C47 C23 122.2(6) . . ? O11 C48 N2 128.5(8) . . ? O5 C49 O13 125.7(8) . 3_665 ? O5 C49 C44 117.7(7) . 4_676 ? O13 C49 C44 116.4(6) 3_665 4_676 ? C31 C50 C21 122.9(6) . . ? C31 C50 S1 127.0(5) . . ? C21 C50 S1 110.1(5) . . ? O7 C51 O10 121.5(6) . 3_665 ? O7 C51 C23 118.0(6) . . ? O10 C51 C23 120.2(6) 3_665 . ? C34 C52 C28 123.8(6) . . ? C34 C52 S3 125.7(5) . . ? C28 C52 S3 110.4(5) . . ? C65 C53 C43 123.7(7) . . ? C65 C53 S3 124.9(5) . . ? C43 C53 S3 111.4(5) . . ? C61 C54 C26 123.9(6) . . ? C61 C54 S2 124.6(5) . . ? C26 C54 S2 111.5(5) . . ? O16 C56 O21 127.7(8) . 3_565 ? O16 C56 C32 119.2(9) . 4_575 ? O21 C56 C32 112.9(10) 3_565 4_575 ? O22 C58 N3 129.0(17) . . ? C22 C60 C32 121.2(7) . . ? C54 C61 C44 117.4(6) . . ? O20 C62 N1 124.3(8) . . ? C33 C63 C46 121.0(6) . . ? O3 C64 O19 122.6(6) . . ? O3 C64 C46 119.0(6) . 4_576 ? O19 C64 C46 118.4(6) . 4_576 ? O3 C64 La1 60.6(4) . . ? O19 C64 La1 62.0(3) . . ? C46 C64 La1 175.4(5) 4_576 . ? C53 C65 C32 118.0(7) . . ? O1 C66 O6 124.3(6) . . ? O1 C66 C13 120.2(6) . . ? O6 C66 C13 115.4(6) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 16.93 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 4.110 _refine_diff_density_min -2.563 _refine_diff_density_rms 0.195 # Attachment 'Revised_Pr2.cif' data_Pr2 _database_code_depnum_ccdc_archive 'CCDC 736841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H60 N6 O24 Pr2 S3' _chemical_formula_weight 1627.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.5424 1.8624 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.0141(19) _cell_length_b 14.9351(8) _cell_length_c 30.3411(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.4220(10) _cell_angle_gamma 90.00 _cell_volume 15733.6(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 5.93 _cell_measurement_theta_max 20.13 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6560 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.734803 ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.41328 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 206217 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -58 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 5.93 _diffrn_reflns_theta_max 20.13 _reflns_number_total 35429 _reflns_number_gt 27245 _reflns_threshold_expression >2sigma(I) _computing_data_collection APEX2 _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The following least-square restraints were applied (total 26) to atoms corresponding to disordered guest DMF molecules: DFIX 1.26 0.02 C44 O23 DFIX 1.45 0.02 N5 C60 isor 0.005 C32, C59, C60, C62 All the other non-hydrogen atoms were refined anisotropically. 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^)+(0.0705P)^2^+75.7846P] 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 35429 _refine_ls_number_parameters 856 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1601 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.072 _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 Pr1 Pr 0.085195(4) 0.460951(10) 0.841651(5) 0.01949(4) Uani 1 1 d . . . Pr2 Pr 0.206790(4) 0.414733(10) 0.855501(5) 0.01819(4) Uani 1 1 d . . . S1 S -0.09839(2) 0.18526(7) 0.90009(3) 0.03186(17) Uani 1 1 d . . . S2 S 0.20262(3) -0.04810(6) 0.85589(4) 0.03536(19) Uani 1 1 d . . . S3 S 0.09261(3) 0.52383(8) 0.59127(3) 0.0379(2) Uani 1 1 d . . . O1 O 0.02156(7) 0.41516(16) 0.80337(8) 0.0265(4) Uani 1 1 d . . . O2 O 0.10938(8) 0.4385(2) 0.77003(8) 0.0329(5) Uani 1 1 d . . . O3 O 0.06085(8) 0.58497(18) 0.79007(11) 0.0369(6) Uani 1 1 d . . . O4 O 0.11742(7) 0.4363(2) 0.91628(8) 0.0310(5) Uani 1 1 d . . . O5 O 0.18131(7) 0.4613(2) 0.92283(8) 0.0332(5) Uani 1 1 d . . . O6 O 0.02905(7) 0.38722(19) 0.87576(8) 0.0310(5) Uani 1 1 d . . . O7 O 0.27362(7) 0.47231(18) 0.87686(9) 0.0316(5) Uani 1 1 d . . . O8 O 0.17244(9) 0.4062(2) 0.78237(9) 0.0437(7) Uani 1 1 d . . . O9 O 0.14381(7) 0.54534(15) 0.84540(9) 0.0321(5) Uani 1 1 d . . . O10 O 0.25387(8) 0.4742(2) 0.80457(10) 0.0384(6) Uani 1 1 d . . . O11 O -0.11378(9) 0.2491(3) 0.92848(10) 0.0467(7) Uani 1 1 d . . . O12 O 0.09389(9) 0.29944(18) 0.83696(10) 0.0385(6) Uani 1 1 d . . . O13 O 0.06027(9) 0.5779(2) 0.88771(11) 0.0412(6) Uani 1 1 d . . . O14 O 0.20479(7) 0.58427(16) 0.85415(10) 0.0330(5) Uani 1 1 d . . . O15 O 0.15718(10) 0.30600(19) 0.85948(11) 0.0453(7) Uani 1 1 d . . . O16 O -0.07503(9) 0.1153(3) 0.92146(12) 0.0490(8) Uani 1 1 d . . . O17 O 0.22634(11) -0.0363(2) 0.89773(16) 0.0611(11) Uani 1 1 d . . . O18 O 0.09341(13) 0.6182(3) 0.59860(12) 0.0598(11) Uani 1 1 d . . . O19 O 0.05531(9) 0.4829(4) 0.58193(11) 0.0608(11) Uani 1 1 d . . . O20 O 0.22163(12) -0.0450(2) 0.81688(16) 0.0580(10) Uani 1 1 d . . . O21 O 0.26708(18) 0.7437(4) 0.9226(3) 0.0971(19) Uani 1 1 d . . . O22 O 0.23683(9) 0.3218(2) 0.91873(11) 0.0439(7) Uani 1 1 d . . . O23 O 0.1314(4) 0.1241(18) 1.0490(5) 0.245(11) Uani 1 1 d D . . O24 O 0.23780(9) 0.2787(2) 0.82678(12) 0.0449(7) Uani 1 1 d . . . N1 N 0.04593(17) 0.6309(4) 0.95344(15) 0.0620(13) Uani 1 1 d . . . N2 N 0.2871(2) 0.6327(4) 0.9726(2) 0.0730(15) Uani 1 1 d . . . N3 N 0.04189(12) 0.6426(2) 0.72116(15) 0.0470(9) Uani 1 1 d . . . N4 N 0.28030(19) 0.2190(4) 0.9449(3) 0.0832(19) Uani 1 1 d . . . N5 N 0.1081(8) 0.2136(18) 0.9883(10) 0.219(9) Uani 1 1 d D . . N6 N 0.27142(13) 0.1929(4) 0.7832(2) 0.0657(15) Uani 1 1 d . . . C1 C -0.04436(8) 0.3099(2) 0.78779(10) 0.0242(5) Uani 1 1 d . . . H1 H -0.0341 0.3341 0.7636 0.029 Uiso 1 1 calc R . . C2 C 0.01053(8) 0.3795(2) 0.83763(10) 0.0230(5) Uani 1 1 d . . . C3 C 0.33548(10) 0.5861(3) 0.86734(13) 0.0326(7) Uani 1 1 d . . . H3 H 0.3321 0.5692 0.8961 0.039 Uiso 1 1 calc R . . C4 C 0.15376(9) 0.4289(2) 0.61895(11) 0.0281(6) Uani 1 1 d . . . C5 C 0.15460(9) 0.4442(2) 0.57086(11) 0.0282(6) Uani 1 1 d . . . C6 C -0.09303(8) 0.2228(2) 0.81684(10) 0.0249(5) Uani 1 1 d . . . C7 C 0.16348(10) 0.1187(2) 0.85118(13) 0.0308(6) Uani 1 1 d . . . H7 H 0.1868 0.1493 0.8543 0.037 Uiso 1 1 calc R . . C8 C -0.02572(8) 0.3255(2) 0.83095(10) 0.0224(5) Uani 1 1 d . . . C9 C 0.15851(10) 0.7009(2) 0.85205(14) 0.0320(7) Uani 1 1 d . . . C10 C -0.04100(9) 0.2900(2) 0.86787(11) 0.0264(5) Uani 1 1 d . . . H10 H -0.0292 0.3000 0.8967 0.032 Uiso 1 1 calc R . . C11 C 0.14904(9) 0.4984(2) 0.98280(10) 0.0266(5) Uani 1 1 d . . . C12 C 0.14432(10) 0.4242(2) 0.70861(10) 0.0273(6) Uani 1 1 d . . . C13 C 0.14152(10) 0.4226(2) 0.75760(10) 0.0269(6) Uani 1 1 d . . . C14 C 0.27699(9) 0.4967(2) 0.83727(12) 0.0292(6) Uani 1 1 d . . . C15 C 0.14908(9) 0.4628(2) 0.93685(10) 0.0254(5) Uani 1 1 d . . . C16 C 0.34689(10) 0.6370(3) 0.78028(12) 0.0344(7) Uani 1 1 d . . . H16 H 0.3507 0.6533 0.7516 0.041 Uiso 1 1 calc R . . C17 C -0.07431(9) 0.2397(2) 0.85960(11) 0.0269(6) Uani 1 1 d . . . C18 C 0.12616(10) 0.2645(2) 0.84736(11) 0.0264(5) Uani 1 1 d . . . C19 C 0.12894(10) 0.1643(2) 0.84646(12) 0.0285(6) Uani 1 1 d . . . C20 C -0.07774(8) 0.2591(2) 0.78047(11) 0.0254(5) Uani 1 1 d . . . H20 H -0.0898 0.2494 0.7517 0.030 Uiso 1 1 calc R . . C21 C 0.18052(11) 0.5496(3) 1.00225(12) 0.0339(7) Uani 1 1 d . . . H21 H 0.2001 0.5632 0.9854 0.041 Uiso 1 1 calc R . . C22 C 0.11643(10) 0.4657(2) 0.67903(11) 0.0296(6) Uani 1 1 d . . . H22 H 0.0947 0.4913 0.6886 0.035 Uiso 1 1 calc R . . C23 C 0.31020(9) 0.5567(2) 0.83050(12) 0.0297(6) Uani 1 1 d . . . C24 C 0.12319(9) 0.4943(3) 0.55152(11) 0.0295(6) Uani 1 1 d . . . C25 C 0.16247(10) 0.0250(2) 0.85118(14) 0.0333(7) Uani 1 1 d . . . C26 C 0.17322(10) -0.1441(2) 0.85525(13) 0.0318(6) Uani 1 1 d . . . C27 C 0.16987(9) 0.60454(19) 0.85091(11) 0.0255(5) Uani 1 1 d . . . C28 C 0.12204(9) 0.4678(2) 0.63468(11) 0.0280(6) Uani 1 1 d . . . C29 C 0.11908(10) 0.4782(3) 1.00727(11) 0.0305(6) Uani 1 1 d . . . H29 H 0.0972 0.4477 0.9946 0.037 Uiso 1 1 calc R . . C30 C 0.31592(10) 0.5828(3) 0.78734(13) 0.0355(7) Uani 1 1 d . . . H30 H 0.2988 0.5635 0.7632 0.043 Uiso 1 1 calc R . . C31 C 0.04613(10) 0.5771(2) 0.75052(13) 0.0312(6) Uani 1 1 d . . . H31 H 0.0375 0.5206 0.7410 0.037 Uiso 1 1 calc R . . C32 C 0.3207(7) 0.1961(18) 0.9550(9) 0.180(7) Uani 1 1 d U . . H32A H 0.3296 0.2116 0.9852 0.270 Uiso 1 1 calc R . . H32B H 0.3353 0.2285 0.9355 0.270 Uiso 1 1 calc R . . H32C H 0.3239 0.1330 0.9508 0.270 Uiso 1 1 calc R . . C33 C 0.18329(11) 0.4196(3) 0.54569(12) 0.0365(8) Uani 1 1 d . . . H33 H 0.2037 0.3836 0.5576 0.044 Uiso 1 1 calc R . . C34 C -0.12790(9) 0.1667(2) 0.81656(11) 0.0277(6) Uani 1 1 d . . . C35 C -0.13437(9) 0.1409(2) 0.85939(11) 0.0282(6) Uani 1 1 d . . . C36 C 0.18640(11) 0.7675(2) 0.85710(13) 0.0316(6) Uani 1 1 d . . . H36 H 0.2125 0.7540 0.8615 0.038 Uiso 1 1 calc R . . C38 C 0.17626(10) 0.3845(3) 0.69291(12) 0.0357(7) Uani 1 1 d . . . H38 H 0.1949 0.3572 0.7132 0.043 Uiso 1 1 calc R . . C39 C 0.13441(11) -0.1209(3) 0.84919(19) 0.0434(10) Uani 1 1 d . . . C40 C 0.18109(11) 0.3844(3) 0.64820(12) 0.0370(8) Uani 1 1 d . . . H40 H 0.2019 0.3556 0.6382 0.044 Uiso 1 1 calc R . . C41 C 0.12793(11) -0.0225(2) 0.84669(19) 0.0445(10) Uani 1 1 d . . . C42 C 0.11865(12) 0.7239(3) 0.8474(2) 0.0546(14) Uani 1 1 d . . . H42 H 0.1002 0.6787 0.8449 0.065 Uiso 1 1 calc R . . C43 C 0.03963(13) 0.5767(3) 0.91903(15) 0.0440(9) Uani 1 1 d . . . H43 H 0.0193 0.5362 0.9177 0.053 Uiso 1 1 calc R . . C44 C 0.1114(10) 0.1832(16) 1.0269(8) 0.27(2) Uani 1 1 d D . . H44 H 0.0947 0.2116 1.0439 0.324 Uiso 1 1 calc R . . C45 C 0.2537(3) 0.1592(4) 0.9585(2) 0.0725(18) Uani 1 1 d . . . H45A H 0.2392 0.1884 0.9791 0.109 Uiso 1 1 calc R . . H45B H 0.2670 0.1086 0.9727 0.109 Uiso 1 1 calc R . . H45C H 0.2365 0.1394 0.9332 0.109 Uiso 1 1 calc R . . C47 C 0.10694(13) 0.8125(3) 0.8464(3) 0.0602(16) Uani 1 1 d . . . H47 H 0.0809 0.8269 0.8439 0.072 Uiso 1 1 calc R . . C48 C 0.25131(14) 0.2634(5) 0.79284(19) 0.0594(15) Uani 1 1 d . . . H48 H 0.2470 0.3068 0.7708 0.071 Uiso 1 1 calc R . . C49 C 0.09356(14) 0.1153(3) 0.8412(2) 0.0500(12) Uani 1 1 d . . . H49 H 0.0703 0.1461 0.8375 0.060 Uiso 1 1 calc R . . C50 C 0.02412(12) 0.6310(3) 0.67581(15) 0.0426(9) Uani 1 1 d . . . H50A H 0.0240 0.6871 0.6604 0.064 Uiso 1 1 calc R . . H50B H -0.0019 0.6103 0.6757 0.064 Uiso 1 1 calc R . . H50C H 0.0385 0.5878 0.6612 0.064 Uiso 1 1 calc R . . C51 C 0.09343(13) 0.0230(3) 0.8415(3) 0.0671(19) Uani 1 1 d . . . H51 H 0.0703 -0.0083 0.8382 0.081 Uiso 1 1 calc R . . C52 C 0.26688(19) 0.6679(5) 0.9346(3) 0.0657(16) Uani 1 1 d . . . H52 H 0.2515 0.6284 0.9165 0.079 Uiso 1 1 calc R . . C53 C 0.2838(4) 0.5410(6) 0.9821(3) 0.099(3) Uani 1 1 d . . . H53A H 0.2996 0.5272 1.0095 0.149 Uiso 1 1 calc R . . H53B H 0.2920 0.5061 0.9585 0.149 Uiso 1 1 calc R . . H53C H 0.2574 0.5272 0.9849 0.149 Uiso 1 1 calc R . . C54 C 0.0774(4) 0.6951(6) 0.9586(3) 0.105(3) Uani 1 1 d . . . H54A H 0.0768 0.7281 0.9856 0.157 Uiso 1 1 calc R . . H54B H 0.0745 0.7357 0.9338 0.157 Uiso 1 1 calc R . . H54C H 0.1014 0.6639 0.9596 0.157 Uiso 1 1 calc R . . C55 C 0.26963(17) 0.2965(4) 0.9264(2) 0.0633(15) Uani 1 1 d . . . H55 H 0.2888 0.3343 0.9189 0.076 Uiso 1 1 calc R . . C56 C 0.2814(3) 0.1263(4) 0.8167(5) 0.114(4) Uani 1 1 d . . . H56A H 0.2958 0.0794 0.8048 0.171 Uiso 1 1 calc R . . H56B H 0.2584 0.1018 0.8259 0.171 Uiso 1 1 calc R . . H56C H 0.2968 0.1530 0.8417 0.171 Uiso 1 1 calc R . . C57 C 0.3112(4) 0.6901(8) 1.0033(4) 0.115(4) Uani 1 1 d . . . H57A H 0.3232 0.6550 1.0277 0.172 Uiso 1 1 calc R . . H57B H 0.2956 0.7359 1.0142 0.172 Uiso 1 1 calc R . . H57C H 0.3307 0.7173 0.9882 0.172 Uiso 1 1 calc R . . C58 C 0.0182(4) 0.6297(10) 0.9866(3) 0.119(4) Uani 1 1 d . . . H58A H 0.0262 0.6723 1.0097 0.179 Uiso 1 1 calc R . . H58B H 0.0176 0.5709 0.9993 0.179 Uiso 1 1 calc R . . H58C H -0.0070 0.6453 0.9723 0.179 Uiso 1 1 calc R . . C59 C 0.0572(4) 0.7311(8) 0.7339(4) 0.114(3) Uani 1 1 d U . . H59A H 0.0519 0.7715 0.7093 0.172 Uiso 1 1 calc R . . H59B H 0.0846 0.7270 0.7423 0.172 Uiso 1 1 calc R . . H59C H 0.0453 0.7530 0.7586 0.172 Uiso 1 1 calc R . . C60 C 0.1418(8) 0.194(2) 0.9660(10) 0.196(8) Uani 1 1 d DU . . H60A H 0.1382 0.2192 0.9366 0.294 Uiso 1 1 calc R . . H60B H 0.1450 0.1304 0.9641 0.294 Uiso 1 1 calc R . . H60C H 0.1643 0.2198 0.9827 0.294 Uiso 1 1 calc R . . C61 C 0.0768(8) 0.2563(11) 0.9651(11) 0.222(15) Uani 1 1 d . . . H61A H 0.0828 0.2732 0.9362 0.334 Uiso 1 1 calc R . . H61B H 0.0707 0.3088 0.9811 0.334 Uiso 1 1 calc R . . H61C H 0.0550 0.2165 0.9619 0.334 Uiso 1 1 calc R . . C62 C 0.2851(4) 0.1895(9) 0.7393(4) 0.111(3) Uani 1 1 d U . . H62A H 0.2991 0.1349 0.7367 0.166 Uiso 1 1 calc R . . H62B H 0.3017 0.2397 0.7362 0.166 Uiso 1 1 calc R . . H62C H 0.2634 0.1917 0.7165 0.166 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 Pr1 0.01836(6) 0.01625(7) 0.02395(7) -0.00213(5) 0.00310(5) -0.00229(4) Pr2 0.02051(6) 0.01353(6) 0.02119(7) 0.00031(4) 0.00519(5) -0.00286(4) S1 0.0275(3) 0.0399(4) 0.0288(4) 0.0042(3) 0.0060(3) -0.0129(3) S2 0.0265(3) 0.0180(3) 0.0608(6) -0.0022(3) 0.0027(4) -0.0045(3) S3 0.0310(4) 0.0557(6) 0.0290(4) 0.0162(4) 0.0117(3) 0.0171(4) O1 0.0229(9) 0.0266(11) 0.0293(10) 0.0035(8) 0.0006(8) -0.0062(8) O2 0.0316(11) 0.0444(14) 0.0234(10) -0.0032(9) 0.0068(8) -0.0102(10) O3 0.0326(12) 0.0240(11) 0.0516(16) 0.0084(10) -0.0042(11) -0.0034(9) O4 0.0276(10) 0.0444(14) 0.0208(9) -0.0036(9) 0.0024(8) -0.0055(10) O5 0.0264(10) 0.0485(15) 0.0257(10) -0.0070(10) 0.0072(8) -0.0017(10) O6 0.0247(10) 0.0402(13) 0.0289(11) -0.0042(9) 0.0069(8) -0.0102(9) O7 0.0220(10) 0.0301(12) 0.0428(13) 0.0063(10) 0.0040(9) -0.0057(8) O8 0.0393(14) 0.064(2) 0.0251(11) -0.0011(12) -0.0067(10) 0.0007(13) O9 0.0325(12) 0.0173(10) 0.0447(14) 0.0030(9) -0.0015(10) -0.0103(8) O10 0.0334(12) 0.0474(16) 0.0371(13) -0.0055(11) 0.0142(10) -0.0205(11) O11 0.0403(15) 0.068(2) 0.0345(13) -0.0109(13) 0.0145(11) -0.0196(14) O12 0.0512(16) 0.0244(12) 0.0389(13) -0.0011(10) 0.0018(11) 0.0152(11) O13 0.0377(14) 0.0335(14) 0.0524(17) -0.0167(12) 0.0053(12) 0.0037(11) O14 0.0244(10) 0.0177(10) 0.0572(16) 0.0019(9) 0.0062(10) -0.0015(8) O15 0.0574(18) 0.0283(13) 0.0555(17) -0.0142(12) 0.0271(14) -0.0259(12) O16 0.0365(14) 0.060(2) 0.0496(17) 0.0225(15) 0.0002(12) -0.0126(14) O17 0.0502(19) 0.0272(14) 0.096(3) -0.0066(16) -0.0293(19) -0.0025(12) O18 0.078(2) 0.060(2) 0.0468(17) 0.0216(16) 0.0323(17) 0.0368(19) O19 0.0238(12) 0.119(3) 0.0399(15) 0.0300(19) 0.0052(11) 0.0103(16) O20 0.055(2) 0.0324(16) 0.092(3) 0.0052(16) 0.032(2) 0.0001(14) O21 0.083(3) 0.056(3) 0.142(5) -0.012(3) -0.025(3) -0.019(2) O22 0.0400(14) 0.0454(16) 0.0456(16) 0.0195(13) 0.0023(12) 0.0036(12) O23 0.169(10) 0.43(3) 0.137(9) 0.157(15) 0.011(8) -0.015(14) O24 0.0440(15) 0.0321(14) 0.0627(19) -0.0096(13) 0.0227(14) 0.0039(11) N1 0.080(3) 0.059(3) 0.044(2) -0.0217(19) -0.003(2) 0.023(2) N2 0.087(4) 0.069(3) 0.066(3) -0.009(3) 0.023(3) -0.025(3) N3 0.051(2) 0.0300(16) 0.057(2) 0.0180(15) -0.0047(16) -0.0071(14) N4 0.077(4) 0.062(3) 0.109(5) 0.036(3) 0.005(3) 0.029(3) N5 0.23(2) 0.192(18) 0.24(2) 0.015(17) 0.040(19) 0.047(16) N6 0.045(2) 0.059(3) 0.098(4) -0.047(3) 0.033(2) -0.0070(19) C1 0.0212(11) 0.0237(13) 0.0284(13) 0.0030(10) 0.0061(9) -0.0043(9) C2 0.0181(10) 0.0206(12) 0.0314(13) -0.0025(10) 0.0072(9) -0.0044(9) C3 0.0244(13) 0.0370(17) 0.0376(16) 0.0040(13) 0.0086(12) -0.0137(12) C4 0.0224(12) 0.0348(16) 0.0277(13) 0.0072(11) 0.0049(10) 0.0023(11) C5 0.0246(12) 0.0339(16) 0.0262(13) 0.0039(11) 0.0036(10) 0.0026(11) C6 0.0213(11) 0.0248(13) 0.0291(13) -0.0005(10) 0.0049(10) -0.0078(10) C7 0.0278(14) 0.0199(13) 0.0447(18) -0.0008(12) 0.0054(12) -0.0033(10) C8 0.0170(10) 0.0234(12) 0.0275(12) -0.0013(9) 0.0052(9) -0.0068(9) C9 0.0295(14) 0.0148(12) 0.050(2) 0.0005(12) 0.0000(13) -0.0012(10) C10 0.0225(12) 0.0300(14) 0.0273(13) -0.0010(11) 0.0051(10) -0.0071(10) C11 0.0276(13) 0.0340(16) 0.0185(11) -0.0016(10) 0.0038(9) 0.0001(11) C12 0.0305(14) 0.0315(15) 0.0199(11) 0.0046(10) 0.0035(10) -0.0038(11) C13 0.0309(14) 0.0304(15) 0.0193(11) 0.0020(10) 0.0029(10) -0.0074(11) C14 0.0217(12) 0.0255(14) 0.0419(17) -0.0008(12) 0.0106(11) -0.0039(10) C15 0.0273(13) 0.0299(14) 0.0194(11) -0.0031(10) 0.0044(9) -0.0017(10) C16 0.0304(15) 0.0403(18) 0.0334(15) 0.0000(13) 0.0080(12) -0.0157(13) C17 0.0233(12) 0.0299(14) 0.0282(13) 0.0023(11) 0.0058(10) -0.0093(10) C18 0.0365(15) 0.0143(11) 0.0302(13) -0.0011(9) 0.0111(11) -0.0051(10) C19 0.0310(14) 0.0146(11) 0.0394(16) -0.0007(10) 0.0030(12) -0.0006(10) C20 0.0207(11) 0.0268(13) 0.0287(13) 0.0015(10) 0.0032(10) -0.0070(10) C21 0.0345(16) 0.0400(18) 0.0291(15) -0.0059(13) 0.0112(12) -0.0079(14) C22 0.0276(13) 0.0370(17) 0.0252(13) 0.0065(11) 0.0078(10) 0.0030(12) C23 0.0237(12) 0.0290(15) 0.0377(16) 0.0008(12) 0.0085(11) -0.0095(11) C24 0.0250(13) 0.0389(17) 0.0258(13) 0.0071(12) 0.0078(10) 0.0031(12) C25 0.0262(14) 0.0228(14) 0.050(2) -0.0016(13) 0.0021(13) -0.0008(11) C26 0.0264(13) 0.0221(14) 0.0463(18) -0.0023(12) 0.0022(12) -0.0082(11) C27 0.0268(13) 0.0120(11) 0.0371(15) 0.0004(10) 0.0018(11) -0.0053(9) C28 0.0235(12) 0.0360(16) 0.0251(13) 0.0078(11) 0.0061(10) 0.0033(11) C29 0.0260(13) 0.0429(18) 0.0231(12) -0.0090(12) 0.0056(10) -0.0041(12) C30 0.0275(14) 0.044(2) 0.0359(16) -0.0024(14) 0.0066(12) -0.0171(14) C31 0.0248(13) 0.0243(14) 0.0444(18) 0.0086(12) 0.0043(12) -0.0013(10) C32 0.177(8) 0.175(8) 0.187(8) 0.013(5) 0.024(5) 0.004(5) C33 0.0363(17) 0.047(2) 0.0279(14) 0.0127(14) 0.0108(12) 0.0172(15) C34 0.0211(11) 0.0297(14) 0.0332(14) 0.0020(11) 0.0064(10) -0.0094(10) C35 0.0248(12) 0.0291(14) 0.0320(14) 0.0006(11) 0.0078(11) -0.0097(11) C36 0.0341(15) 0.0146(12) 0.0458(18) -0.0025(11) 0.0036(13) -0.0046(10) C38 0.0276(14) 0.052(2) 0.0279(14) 0.0100(14) 0.0040(11) 0.0021(14) C39 0.0257(15) 0.0241(16) 0.079(3) -0.0001(17) 0.0006(16) -0.0007(12) C40 0.0307(15) 0.050(2) 0.0312(15) 0.0133(15) 0.0092(12) 0.0105(15) C41 0.0274(15) 0.0195(15) 0.085(3) -0.0026(16) 0.0009(17) -0.0076(12) C42 0.0281(16) 0.0181(15) 0.115(4) -0.0020(19) 0.000(2) -0.0054(12) C43 0.0399(19) 0.052(2) 0.0397(19) -0.0128(17) 0.0020(15) 0.0122(17) C44 0.51(7) 0.19(2) 0.099(11) 0.038(13) -0.01(2) -0.15(3) C45 0.110(6) 0.048(3) 0.057(3) -0.001(2) 0.002(3) -0.012(3) C47 0.0286(17) 0.0226(17) 0.126(5) -0.003(2) -0.001(2) -0.0056(13) C48 0.037(2) 0.090(4) 0.051(2) -0.034(3) 0.0043(18) 0.007(2) C49 0.041(2) 0.0184(15) 0.087(4) -0.0022(17) -0.006(2) -0.0069(14) C50 0.0341(17) 0.048(2) 0.046(2) 0.0157(17) 0.0051(15) 0.0003(16) C51 0.0278(17) 0.0215(17) 0.147(6) -0.007(2) -0.007(3) -0.0043(13) C52 0.060(3) 0.057(3) 0.081(4) -0.021(3) 0.013(3) -0.019(3) C53 0.146(9) 0.075(5) 0.079(5) -0.004(4) 0.022(5) -0.031(5) C54 0.162(9) 0.062(4) 0.079(5) -0.026(4) -0.028(5) -0.019(5) C55 0.051(3) 0.043(3) 0.095(4) 0.027(3) 0.003(3) 0.005(2) C56 0.081(5) 0.032(3) 0.246(13) 0.001(5) 0.089(7) 0.001(3) C57 0.137(9) 0.082(6) 0.112(7) 0.004(5) -0.029(6) -0.040(6) C58 0.156(10) 0.150(10) 0.059(4) -0.035(5) 0.043(5) 0.029(8) C59 0.143(5) 0.086(4) 0.108(5) 0.020(4) -0.007(4) -0.017(4) C60 0.196(9) 0.199(9) 0.193(9) -0.001(5) 0.028(5) -0.004(5) C61 0.22(2) 0.079(8) 0.33(3) 0.051(13) -0.12(2) -0.034(11) C62 0.116(5) 0.126(5) 0.097(4) -0.034(4) 0.041(4) 0.008(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 Pr1 O9 2.399(2) . ? Pr1 O4 2.424(2) . ? Pr1 O12 2.438(3) . ? Pr1 O2 2.455(2) . ? Pr1 O13 2.466(3) . ? Pr1 O1 2.472(2) . ? Pr1 O3 2.502(3) . ? Pr1 O6 2.583(2) . ? Pr1 C2 2.872(3) . ? Pr2 O8 2.387(3) . ? Pr2 O15 2.392(3) . ? Pr2 O5 2.434(2) . ? Pr2 O22 2.488(3) . ? Pr2 O7 2.499(2) . ? Pr2 O24 2.512(3) . ? Pr2 O14 2.533(2) . ? Pr2 O10 2.560(2) . ? Pr2 C14 2.863(3) . ? Pr2 O9 2.930(3) . ? S1 O16 1.430(4) . ? S1 O11 1.436(4) . ? S1 C35 1.774(3) . ? S1 C17 1.775(3) . ? S2 O20 1.432(4) . ? S2 O17 1.435(4) . ? S2 C26 1.764(3) . ? S2 C25 1.771(4) . ? S3 O18 1.426(5) . ? S3 O19 1.436(4) . ? S3 C24 1.769(3) . ? S3 C28 1.774(3) . ? O1 C2 1.271(4) . ? O2 C13 1.255(4) . ? O3 C31 1.249(5) . ? O4 C15 1.263(4) . ? O5 C15 1.256(4) . ? O6 C2 1.256(4) . ? O7 C14 1.275(5) . ? O8 C13 1.260(4) . ? O9 C27 1.266(4) . ? O10 C14 1.243(5) . ? O12 C18 1.247(5) . ? O13 C43 1.266(6) . ? O14 C27 1.251(4) . ? O15 C18 1.263(4) . ? O21 C52 1.189(9) . ? O22 C55 1.203(6) . ? O23 C44 1.266(19) . ? O24 C48 1.209(6) . ? N1 C43 1.316(6) . ? N1 C54 1.453(13) . ? N1 C58 1.485(12) . ? N2 C52 1.377(11) . ? N2 C53 1.407(12) . ? N2 C57 1.452(12) . ? N3 C31 1.318(5) . ? N3 C50 1.445(6) . ? N3 C59 1.460(13) . ? N4 C55 1.318(7) . ? N4 C45 1.393(11) . ? N4 C32 1.45(3) . ? N5 C44 1.25(3) . ? N5 C61 1.38(3) . ? N5 C60 1.464(18) . ? N6 C48 1.320(7) . ? N6 C56 1.434(14) . ? N6 C62 1.471(12) . ? C1 C20 1.387(4) . ? C1 C8 1.405(4) . ? C2 C8 1.496(4) . ? C3 C35 1.382(4) 3 ? C3 C23 1.404(5) . ? C4 C40 1.388(5) . ? C4 C28 1.391(5) . ? C4 C5 1.481(5) . ? C5 C33 1.388(5) . ? C5 C24 1.395(5) . ? C6 C20 1.397(4) . ? C6 C17 1.399(5) . ? C6 C34 1.480(4) . ? C7 C19 1.380(5) . ? C7 C25 1.400(5) . ? C8 C10 1.406(4) . ? C9 C36 1.389(5) . ? C9 C42 1.427(6) . ? C9 C27 1.494(4) . ? C10 C17 1.383(4) . ? C11 C29 1.394(5) . ? C11 C21 1.406(5) . ? C11 C15 1.493(4) . ? C12 C22 1.385(5) . ? C12 C38 1.402(5) . ? C12 C13 1.502(4) . ? C14 C23 1.503(4) . ? C16 C34 1.391(5) 3 ? C16 C30 1.392(5) . ? C18 C19 1.501(4) . ? C19 C49 1.430(5) . ? C21 C33 1.388(5) 6_566 ? C22 C28 1.385(4) . ? C23 C30 1.405(5) . ? C24 C29 1.393(4) 6_565 ? C25 C41 1.394(5) . ? C26 C39 1.391(5) . ? C26 C36 1.397(5) 1_545 ? C29 C24 1.393(4) 6_566 ? C33 C21 1.388(5) 6_565 ? C34 C16 1.391(5) 3_445 ? C34 C35 1.402(5) . ? C35 C3 1.382(4) 3_445 ? C36 C26 1.397(5) 1_565 ? C38 C40 1.388(5) . ? C39 C47 1.378(6) 1_545 ? C39 C41 1.488(6) . ? C41 C51 1.377(6) . ? C42 C47 1.384(6) . ? C47 C39 1.378(6) 1_565 ? C49 C51 1.379(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Pr1 O4 75.12(9) . . ? O9 Pr1 O12 114.21(10) . . ? O4 Pr1 O12 81.83(10) . . ? O9 Pr1 O2 73.91(9) . . ? O4 Pr1 O2 129.35(9) . . ? O12 Pr1 O2 75.72(10) . . ? O9 Pr1 O13 87.95(10) . . ? O4 Pr1 O13 74.58(10) . . ? O12 Pr1 O13 142.19(11) . . ? O2 Pr1 O13 141.82(11) . . ? O9 Pr1 O1 151.80(8) . . ? O4 Pr1 O1 132.80(8) . . ? O12 Pr1 O1 79.09(9) . . ? O2 Pr1 O1 86.52(8) . . ? O13 Pr1 O1 95.66(9) . . ? O9 Pr1 O3 82.01(9) . . ? O4 Pr1 O3 140.93(10) . . ? O12 Pr1 O3 136.96(10) . . ? O2 Pr1 O3 71.09(10) . . ? O13 Pr1 O3 73.33(11) . . ? O1 Pr1 O3 72.38(8) . . ? O9 Pr1 O6 153.60(9) . . ? O4 Pr1 O6 81.23(8) . . ? O12 Pr1 O6 73.07(10) . . ? O2 Pr1 O6 131.58(8) . . ? O13 Pr1 O6 74.43(10) . . ? O1 Pr1 O6 51.98(8) . . ? O3 Pr1 O6 110.53(9) . . ? O9 Pr1 C2 173.33(9) . . ? O4 Pr1 C2 106.67(9) . . ? O12 Pr1 C2 72.45(10) . . ? O2 Pr1 C2 108.71(9) . . ? O13 Pr1 C2 86.39(9) . . ? O1 Pr1 C2 26.18(8) . . ? O3 Pr1 C2 92.99(9) . . ? O6 Pr1 C2 25.95(8) . . ? O8 Pr2 O15 74.27(12) . . ? O8 Pr2 O5 126.89(10) . . ? O15 Pr2 O5 78.71(10) . . ? O8 Pr2 O22 143.04(12) . . ? O15 Pr2 O22 79.62(12) . . ? O5 Pr2 O22 71.12(11) . . ? O8 Pr2 O7 127.01(10) . . ? O15 Pr2 O7 151.92(12) . . ? O5 Pr2 O7 96.69(9) . . ? O22 Pr2 O7 72.75(10) . . ? O8 Pr2 O24 79.80(12) . . ? O15 Pr2 O24 79.49(11) . . ? O5 Pr2 O24 138.06(11) . . ? O22 Pr2 O24 69.98(12) . . ? O7 Pr2 O24 86.34(10) . . ? O8 Pr2 O14 91.64(11) . . ? O15 Pr2 O14 131.34(10) . . ? O5 Pr2 O14 73.48(10) . . ? O22 Pr2 O14 125.31(11) . . ? O7 Pr2 O14 71.53(8) . . ? O24 Pr2 O14 144.60(10) . . ? O8 Pr2 O10 75.14(10) . . ? O15 Pr2 O10 142.59(10) . . ? O5 Pr2 O10 137.92(9) . . ? O22 Pr2 O10 114.70(11) . . ? O7 Pr2 O10 51.88(9) . . ? O24 Pr2 O10 74.35(11) . . ? O14 Pr2 O10 70.26(10) . . ? O8 Pr2 C14 100.67(11) . . ? O15 Pr2 C14 161.26(10) . . ? O5 Pr2 C14 117.20(10) . . ? O22 Pr2 C14 95.71(11) . . ? O7 Pr2 C14 26.41(10) . . ? O24 Pr2 C14 81.86(10) . . ? O14 Pr2 C14 65.94(9) . . ? O10 Pr2 C14 25.73(10) . . ? O8 Pr2 O9 69.89(10) . . ? O15 Pr2 O9 85.16(10) . . ? O5 Pr2 O9 62.95(9) . . ? O22 Pr2 O9 133.58(10) . . ? O7 Pr2 O9 117.71(8) . . ? O24 Pr2 O9 148.78(10) . . ? O14 Pr2 O9 46.69(7) . . ? O10 Pr2 O9 103.92(9) . . ? C14 Pr2 O9 110.40(8) . . ? O16 S1 O11 116.8(2) . . ? O16 S1 C35 110.8(2) . . ? O11 S1 C35 112.20(18) . . ? O16 S1 C17 110.69(18) . . ? O11 S1 C17 111.10(19) . . ? C35 S1 C17 92.71(15) . . ? O20 S2 O17 116.7(3) . . ? O20 S2 C26 110.5(2) . . ? O17 S2 C26 112.4(2) . . ? O20 S2 C25 111.3(2) . . ? O17 S2 C25 111.0(2) . . ? C26 S2 C25 92.54(17) . . ? O18 S3 O19 116.7(3) . . ? O18 S3 C24 110.55(19) . . ? O19 S3 C24 112.0(2) . . ? O18 S3 C28 110.6(2) . . ? O19 S3 C28 111.84(19) . . ? C24 S3 C28 92.51(15) . . ? C2 O1 Pr1 94.71(18) . . ? C13 O2 Pr1 135.8(2) . . ? C31 O3 Pr1 126.6(2) . . ? C15 O4 Pr1 133.4(2) . . ? C15 O5 Pr2 137.0(2) . . ? C2 O6 Pr1 89.95(17) . . ? C14 O7 Pr2 92.9(2) . . ? C13 O8 Pr2 146.6(3) . . ? C27 O9 Pr1 166.2(2) . . ? C27 O9 Pr2 86.05(19) . . ? Pr1 O9 Pr2 106.43(8) . . ? C14 O10 Pr2 90.9(2) . . ? C18 O12 Pr1 121.0(2) . . ? C43 O13 Pr1 133.9(3) . . ? C27 O14 Pr2 105.53(18) . . ? C18 O15 Pr2 157.1(3) . . ? C55 O22 Pr2 128.6(4) . . ? C48 O24 Pr2 133.0(4) . . ? C43 N1 C54 122.5(6) . . ? C43 N1 C58 118.2(7) . . ? C54 N1 C58 119.1(7) . . ? C52 N2 C53 119.8(7) . . ? C52 N2 C57 120.3(7) . . ? C53 N2 C57 119.9(8) . . ? C31 N3 C50 123.4(4) . . ? C31 N3 C59 119.1(6) . . ? C50 N3 C59 117.4(5) . . ? C55 N4 C45 121.7(6) . . ? C55 N4 C32 120.9(12) . . ? C45 N4 C32 117.3(11) . . ? C44 N5 C61 128(3) . . ? C44 N5 C60 112(3) . . ? C61 N5 C60 120(3) . . ? C48 N6 C56 119.0(6) . . ? C48 N6 C62 118.3(8) . . ? C56 N6 C62 122.6(7) . . ? C20 C1 C8 121.4(3) . . ? O6 C2 O1 122.6(3) . . ? O6 C2 C8 120.1(3) . . ? O1 C2 C8 117.2(3) . . ? O6 C2 Pr1 64.10(15) . . ? O1 C2 Pr1 59.11(14) . . ? C8 C2 Pr1 170.5(2) . . ? C35 C3 C23 117.6(3) 3 . ? C40 C4 C28 119.7(3) . . ? C40 C4 C5 127.2(3) . . ? C28 C4 C5 113.1(3) . . ? C33 C5 C24 119.9(3) . . ? C33 C5 C4 127.5(3) . . ? C24 C5 C4 112.5(3) . . ? C20 C6 C17 118.8(3) . . ? C20 C6 C34 128.0(3) . . ? C17 C6 C34 113.3(3) . . ? C19 C7 C25 118.2(3) . . ? C1 C8 C10 120.1(3) . . ? C1 C8 C2 120.0(3) . . ? C10 C8 C2 119.9(3) . . ? C36 C9 C42 120.2(3) . . ? C36 C9 C27 120.5(3) . . ? C42 C9 C27 119.4(3) . . ? C17 C10 C8 117.3(3) . . ? C29 C11 C21 119.8(3) . . ? C29 C11 C15 120.8(3) . . ? C21 C11 C15 119.4(3) . . ? C22 C12 C38 119.7(3) . . ? C22 C12 C13 121.2(3) . . ? C38 C12 C13 119.1(3) . . ? O2 C13 O8 126.4(3) . . ? O2 C13 C12 118.0(3) . . ? O8 C13 C12 115.6(3) . . ? O10 C14 O7 123.0(3) . . ? O10 C14 C23 119.2(3) . . ? O7 C14 C23 117.8(3) . . ? O10 C14 Pr2 63.37(17) . . ? O7 C14 Pr2 60.65(16) . . ? C23 C14 Pr2 168.5(2) . . ? O5 C15 O4 126.6(3) . . ? O5 C15 C11 115.6(3) . . ? O4 C15 C11 117.8(3) . . ? C34 C16 C30 119.4(3) 3 . ? C10 C17 C6 123.3(3) . . ? C10 C17 S1 126.0(3) . . ? C6 C17 S1 110.6(2) . . ? O12 C18 O15 125.9(3) . . ? O12 C18 C19 118.1(3) . . ? O15 C18 C19 116.0(3) . . ? C7 C19 C49 119.6(3) . . ? C7 C19 C18 123.3(3) . . ? C49 C19 C18 117.1(3) . . ? C1 C20 C6 119.1(3) . . ? C33 C21 C11 122.2(3) 6_566 . ? C12 C22 C28 117.6(3) . . ? C3 C23 C30 120.3(3) . . ? C3 C23 C14 119.8(3) . . ? C30 C23 C14 119.9(3) . . ? C29 C24 C5 122.7(3) 6_565 . ? C29 C24 S3 126.0(3) 6_565 . ? C5 C24 S3 111.1(2) . . ? C41 C25 C7 122.0(3) . . ? C41 C25 S2 111.3(3) . . ? C7 C25 S2 126.6(3) . . ? C39 C26 C36 123.6(3) . 1_545 ? C39 C26 S2 111.0(3) . . ? C36 C26 S2 125.3(3) 1_545 . ? O14 C27 O9 121.5(3) . . ? O14 C27 C9 119.4(3) . . ? O9 C27 C9 119.1(3) . . ? C22 C28 C4 122.9(3) . . ? C22 C28 S3 126.2(3) . . ? C4 C28 S3 110.8(2) . . ? C24 C29 C11 117.3(3) 6_566 . ? C16 C30 C23 120.8(3) . . ? O3 C31 N3 125.2(4) . . ? C21 C33 C5 117.9(3) 6_565 . ? C16 C34 C35 119.0(3) 3_445 . ? C16 C34 C6 128.6(3) 3_445 . ? C35 C34 C6 112.5(3) . . ? C3 C35 C34 122.9(3) 3_445 . ? C3 C35 S1 126.1(3) 3_445 . ? C34 C35 S1 111.0(2) . . ? C9 C36 C26 116.7(3) . 1_565 ? C40 C38 C12 122.4(3) . . ? C47 C39 C26 119.4(4) 1_545 . ? C47 C39 C41 127.5(4) 1_545 . ? C26 C39 C41 113.1(3) . . ? C4 C40 C38 117.6(3) . . ? C51 C41 C25 119.8(4) . . ? C51 C41 C39 128.2(3) . . ? C25 C41 C39 111.9(3) . . ? C47 C42 C9 121.1(3) . . ? O13 C43 N1 122.2(5) . . ? N5 C44 O23 137(3) . . ? C39 C47 C42 119.1(4) 1_565 . ? O24 C48 N6 128.2(7) . . ? C51 C49 C19 121.0(4) . . ? C41 C51 C49 119.4(4) . . ? O21 C52 N2 126.8(6) . . ? O22 C55 N4 124.7(6) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 20.13 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 4.284 _refine_diff_density_min -2.259 _refine_diff_density_rms 0.149