# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a #TrackingRef 'a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 La2 O15 S3' _chemical_formula_weight 842.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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 9.1069(12) _cell_length_b 10.5452(13) _cell_length_c 13.5137(17) _cell_angle_alpha 100.4410(10) _cell_angle_beta 102.8500(10) _cell_angle_gamma 102.9220(10) _cell_volume 1196.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6954 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.23 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 3.862 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3004 _exptl_absorpt_correction_T_max 0.5597 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8818 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4373 _reflns_number_gt 4088 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+1.2543P] 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 4373 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0197 _refine_ls_R_factor_gt 0.0179 _refine_ls_wR_factor_ref 0.0459 _refine_ls_wR_factor_gt 0.0446 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 1.027403(16) 0.213916(14) 0.024120(11) 0.01330(5) Uani 1 1 d . . . La2 La 0.640364(16) 0.393989(14) -0.079143(11) 0.01297(5) Uani 1 1 d . . . S1 S 0.95619(11) 0.62733(11) 0.42281(6) 0.0419(2) Uani 1 1 d . . . S2 S 0.78564(16) -0.01445(11) -0.48603(7) 0.0565(3) Uani 1 1 d . . . S3 S 0.64551(16) 0.18057(13) 0.35454(8) 0.0627(4) Uani 1 1 d . . . O1 O 1.1333(2) 0.47268(19) 0.14150(15) 0.0205(4) Uani 1 1 d . . . O2 O 0.8802(2) 0.39815(19) 0.06796(15) 0.0205(4) Uani 1 1 d . . . O3 O 0.8006(2) 0.63418(18) 0.05262(14) 0.0171(4) Uani 1 1 d . . . O4 O 0.6526(2) 0.71580(19) 0.14592(15) 0.0202(4) Uani 1 1 d . . . O5 O 0.8831(3) -0.19974(19) -0.21574(15) 0.0278(5) Uani 1 1 d . . . O6 O 0.9453(2) -0.00123(19) -0.10786(14) 0.0201(4) Uani 1 1 d . . . O7 O 0.8309(2) 0.23058(19) -0.13011(14) 0.0206(4) Uani 1 1 d . . . O8 O 0.6194(2) 0.2275(2) -0.24787(15) 0.0273(5) Uani 1 1 d . . . O9 O 0.7764(2) 0.11269(19) 0.05515(16) 0.0229(4) Uani 1 1 d . . . O10 O 0.5748(2) 0.18410(19) -0.01633(15) 0.0196(4) Uani 1 1 d . . . O11 O 0.5387(2) 0.42755(18) 0.07802(14) 0.0181(4) Uani 1 1 d . . . O12 O 0.4481(3) 0.4752(2) 0.21333(16) 0.0306(5) Uani 1 1 d . . . O13 O 1.2762(2) 0.1518(2) 0.02448(17) 0.0272(5) Uani 1 1 d . . . H1W H 1.3539 0.1886 0.0046 0.041 Uiso 1 1 d R . . H2W H 1.2851 0.0729 0.0223 0.041 Uiso 1 1 d R . . O14 O 0.5305(4) 0.3404(4) 0.5629(2) 0.0742(10) Uani 1 1 d . . . H3W H 0.5241 0.3056 0.6144 0.111 Uiso 1 1 d R . . H4W H 0.5772 0.4216 0.5679 0.111 Uiso 1 1 d R . . O15 O 0.7032(4) 0.6026(3) 0.5845(2) 0.0668(9) Uani 1 1 d . . . H5W H 0.7461 0.6662 0.6390 0.100 Uiso 1 1 d R . . H6W H 0.6449 0.6284 0.5384 0.100 Uiso 1 1 d R . . C1 C 1.0324(4) 0.5485(3) 0.3322(2) 0.0294(7) Uani 1 1 d . . . H1 H 1.1099 0.5054 0.3484 0.035 Uiso 1 1 calc R . . C2 C 0.9655(3) 0.5569(3) 0.2337(2) 0.0182(6) Uani 1 1 d . . . C3 C 0.8515(3) 0.6318(3) 0.2321(2) 0.0179(6) Uani 1 1 d . . . C4 C 0.8365(4) 0.6760(3) 0.3299(2) 0.0302(7) Uani 1 1 d . . . H4 H 0.7688 0.7266 0.3441 0.036 Uiso 1 1 calc R . . C5 C 0.9951(3) 0.4758(3) 0.1413(2) 0.0152(5) Uani 1 1 d . . . C6 C 0.7609(3) 0.6635(3) 0.1384(2) 0.0159(5) Uani 1 1 d . . . C7 C 0.8583(5) -0.0825(4) -0.3869(2) 0.0412(9) Uani 1 1 d . . . H7 H 0.9026 -0.1537 -0.3960 0.049 Uiso 1 1 calc R . . C8 C 0.8444(4) -0.0211(3) -0.2928(2) 0.0233(6) Uani 1 1 d . . . C9 C 0.7705(3) 0.0858(3) -0.3024(2) 0.0218(6) Uani 1 1 d . . . C10 C 0.7300(4) 0.0958(3) -0.4033(2) 0.0352(8) Uani 1 1 d . . . H10 H 0.6774 0.1564 -0.4248 0.042 Uiso 1 1 calc R . . C11 C 0.8932(3) -0.0769(3) -0.2003(2) 0.0188(6) Uani 1 1 d . . . C12 C 0.7376(3) 0.1850(3) -0.2214(2) 0.0178(6) Uani 1 1 d . . . C13 C 0.6819(5) 0.1274(4) 0.2377(3) 0.0437(9) Uani 1 1 d . . . H13 H 0.7243 0.0560 0.2231 0.052 Uiso 1 1 calc R . . C14 C 0.6420(3) 0.2008(3) 0.1684(2) 0.0232(6) Uani 1 1 d . . . C15 C 0.5795(3) 0.3056(3) 0.2124(2) 0.0222(6) Uani 1 1 d . . . C16 C 0.5788(4) 0.3062(4) 0.3135(3) 0.0376(8) Uani 1 1 d . . . H16 H 0.5458 0.3681 0.3552 0.045 Uiso 1 1 calc R . . C17 C 0.6632(3) 0.1646(3) 0.0612(2) 0.0178(6) Uani 1 1 d . . . C18 C 0.5189(3) 0.4077(3) 0.1653(2) 0.0177(6) 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 0.01371(9) 0.01244(8) 0.01580(8) 0.00459(6) 0.00456(6) 0.00622(6) La2 0.01253(8) 0.01437(9) 0.01409(8) 0.00383(6) 0.00495(6) 0.00622(6) S1 0.0512(5) 0.0666(6) 0.0159(4) 0.0079(4) 0.0089(4) 0.0341(5) S2 0.1134(10) 0.0617(6) 0.0190(4) 0.0146(4) 0.0237(5) 0.0637(7) S3 0.1124(10) 0.0836(8) 0.0371(5) 0.0430(6) 0.0386(6) 0.0755(8) O1 0.0167(10) 0.0214(10) 0.0249(10) 0.0046(8) 0.0086(8) 0.0067(8) O2 0.0174(10) 0.0187(10) 0.0222(10) 0.0006(8) 0.0002(8) 0.0076(8) O3 0.0193(10) 0.0168(9) 0.0178(9) 0.0051(8) 0.0082(8) 0.0066(8) O4 0.0157(9) 0.0202(10) 0.0250(10) 0.0016(8) 0.0051(8) 0.0092(8) O5 0.0461(13) 0.0177(10) 0.0203(10) 0.0042(8) 0.0053(9) 0.0144(10) O6 0.0252(10) 0.0176(10) 0.0175(9) 0.0035(8) 0.0036(8) 0.0084(8) O7 0.0242(10) 0.0210(10) 0.0161(9) 0.0031(8) 0.0023(8) 0.0096(8) O8 0.0279(11) 0.0331(12) 0.0230(10) 0.0018(9) 0.0035(9) 0.0199(10) O9 0.0210(10) 0.0215(10) 0.0356(12) 0.0124(9) 0.0151(9) 0.0124(8) O10 0.0196(10) 0.0191(10) 0.0227(10) 0.0075(8) 0.0062(8) 0.0084(8) O11 0.0213(10) 0.0187(10) 0.0176(9) 0.0069(8) 0.0076(8) 0.0078(8) O12 0.0411(13) 0.0422(13) 0.0299(11) 0.0201(10) 0.0228(10) 0.0317(11) O13 0.0190(10) 0.0193(10) 0.0511(14) 0.0133(10) 0.0171(10) 0.0094(8) O14 0.095(3) 0.080(2) 0.0468(18) 0.0178(16) 0.0041(17) 0.034(2) O15 0.062(2) 0.073(2) 0.0567(18) -0.0021(16) 0.0018(15) 0.0308(17) C1 0.0323(17) 0.0396(19) 0.0207(15) 0.0065(13) 0.0065(13) 0.0197(15) C2 0.0177(14) 0.0208(14) 0.0177(13) 0.0046(11) 0.0048(11) 0.0085(11) C3 0.0164(13) 0.0207(14) 0.0174(13) 0.0020(11) 0.0068(11) 0.0064(11) C4 0.0315(17) 0.0421(19) 0.0201(15) 0.0037(14) 0.0078(13) 0.0185(15) C5 0.0178(13) 0.0150(13) 0.0171(13) 0.0083(11) 0.0065(11) 0.0081(11) C6 0.0141(13) 0.0115(12) 0.0198(13) 0.0008(10) 0.0041(11) 0.0019(10) C7 0.075(3) 0.042(2) 0.0229(16) 0.0106(15) 0.0168(17) 0.043(2) C8 0.0315(16) 0.0238(15) 0.0176(14) 0.0050(12) 0.0066(12) 0.0136(13) C9 0.0285(15) 0.0216(15) 0.0176(14) 0.0048(11) 0.0060(12) 0.0116(12) C10 0.057(2) 0.0345(18) 0.0227(16) 0.0088(14) 0.0104(15) 0.0293(17) C11 0.0215(14) 0.0199(14) 0.0171(13) 0.0041(11) 0.0062(11) 0.0094(12) C12 0.0211(14) 0.0177(13) 0.0163(13) 0.0056(11) 0.0058(11) 0.0070(11) C13 0.068(3) 0.052(2) 0.0356(19) 0.0252(18) 0.0243(18) 0.045(2) C14 0.0215(14) 0.0291(16) 0.0277(15) 0.0138(13) 0.0113(12) 0.0140(13) C15 0.0218(14) 0.0290(16) 0.0234(14) 0.0113(12) 0.0104(12) 0.0138(13) C16 0.055(2) 0.049(2) 0.0272(17) 0.0193(16) 0.0180(16) 0.0356(18) C17 0.0172(14) 0.0117(13) 0.0281(15) 0.0086(11) 0.0108(12) 0.0037(11) C18 0.0156(13) 0.0207(14) 0.0178(13) 0.0061(11) 0.0043(11) 0.0061(11) _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 O9 2.4570(19) . ? La1 O6 2.4635(19) . ? La1 O7 2.4885(18) . ? La1 O13 2.4943(19) . ? La1 O3 2.5095(18) 2_765 ? La1 O5 2.578(2) 2_755 ? La1 O2 2.6502(18) . ? La1 O6 2.7233(19) 2_755 ? La1 O1 2.7324(19) . ? La1 C5 3.034(3) . ? La1 C11 3.037(3) 2_755 ? La2 O11 2.4985(18) . ? La2 O10 2.5082(19) . ? La2 O4 2.5381(19) 2_665 ? La2 O8 2.554(2) . ? La2 O12 2.568(2) 2_665 ? La2 O2 2.5920(18) . ? La2 O1 2.6154(19) 2_765 ? La2 O3 2.6966(18) . ? La2 O11 2.7520(18) 2_665 ? La2 O7 2.8093(19) . ? La2 C18 3.053(3) 2_665 ? La2 C12 3.071(3) . ? S1 C4 1.704(3) . ? S1 C1 1.714(3) . ? S2 C10 1.704(3) . ? S2 C7 1.708(3) . ? S3 C13 1.706(4) . ? S3 C16 1.705(3) . ? O1 C5 1.266(3) . ? O1 La2 2.6154(19) 2_765 ? O2 C5 1.269(3) . ? O3 C6 1.295(3) . ? O3 La1 2.5095(18) 2_765 ? O4 C6 1.247(3) . ? O4 La2 2.5381(18) 2_665 ? O5 C11 1.253(3) . ? O5 La1 2.578(2) 2_755 ? O6 C11 1.276(3) . ? O6 La1 2.7233(19) 2_755 ? O7 C12 1.270(3) . ? O8 C12 1.261(3) . ? O9 C17 1.282(3) . ? O10 C17 1.251(3) . ? O11 C18 1.278(3) . ? O11 La2 2.7520(18) 2_665 ? O12 C18 1.252(3) . ? O12 La2 2.568(2) 2_665 ? O13 H1W 0.8500 . ? O13 H2W 0.8500 . ? O14 H3W 0.8500 . ? O14 H4W 0.8500 . ? O15 H5W 0.8500 . ? O15 H6W 0.8500 . ? C1 C2 1.362(4) . ? C1 H1 0.9300 . ? C2 C3 1.438(4) . ? C2 C5 1.493(4) . ? C3 C4 1.367(4) . ? C3 C6 1.486(4) . ? C4 H4 0.9300 . ? C7 C8 1.365(4) . ? C7 H7 0.9300 . ? C8 C9 1.447(4) . ? C8 C11 1.497(4) . ? C9 C10 1.360(4) . ? C9 C12 1.501(4) . ? C10 H10 0.9300 . ? C11 La1 3.037(3) 2_755 ? C13 C14 1.359(4) . ? C13 H13 0.9300 . ? C14 C15 1.446(4) . ? C14 C17 1.495(4) . ? C15 C16 1.366(4) . ? C15 C18 1.493(4) . ? C16 H16 0.9300 . ? C18 La2 3.053(3) 2_665 ? 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 La1 O6 80.16(7) . . ? O9 La1 O7 76.93(7) . . ? O6 La1 O7 71.74(6) . . ? O9 La1 O13 136.29(6) . . ? O6 La1 O13 75.74(7) . . ? O7 La1 O13 126.90(7) . . ? O9 La1 O3 153.71(6) . 2_765 ? O6 La1 O3 102.64(6) . 2_765 ? O7 La1 O3 79.20(6) . 2_765 ? O13 La1 O3 68.35(6) . 2_765 ? O9 La1 O5 78.59(7) . 2_755 ? O6 La1 O5 115.45(6) . 2_755 ? O7 La1 O5 152.76(7) . 2_755 ? O13 La1 O5 79.67(7) . 2_755 ? O3 La1 O5 121.51(6) 2_765 2_755 ? O9 La1 O2 69.27(6) . . ? O6 La1 O2 132.13(6) . . ? O7 La1 O2 66.16(6) . . ? O13 La1 O2 149.84(6) . . ? O3 La1 O2 91.08(6) 2_765 . ? O5 La1 O2 94.02(6) 2_755 . ? O9 La1 O6 71.21(6) . 2_755 ? O6 La1 O6 66.62(7) . 2_755 ? O7 La1 O6 130.73(6) . 2_755 ? O13 La1 O6 65.89(6) . 2_755 ? O3 La1 O6 134.23(6) 2_765 2_755 ? O5 La1 O6 48.86(6) 2_755 2_755 ? O2 La1 O6 130.14(6) . 2_755 ? O9 La1 O1 107.44(6) . . ? O6 La1 O1 169.33(6) . . ? O7 La1 O1 102.23(6) . . ? O13 La1 O1 102.27(6) . . ? O3 La1 O1 67.19(6) 2_765 . ? O5 La1 O1 74.01(6) 2_755 . ? O2 La1 O1 48.05(6) . . ? O6 La1 O1 122.50(6) 2_755 . ? O9 La1 C5 84.93(7) . . ? O6 La1 C5 156.74(7) . . ? O7 La1 C5 87.61(6) . . ? O13 La1 C5 126.69(7) . . ? O3 La1 C5 83.23(6) 2_765 . ? O5 La1 C5 78.46(6) 2_755 . ? O2 La1 C5 24.62(6) . . ? O6 La1 C5 124.76(6) 2_755 . ? O1 La1 C5 24.66(6) . . ? O9 La1 C11 74.18(7) . 2_755 ? O6 La1 C11 91.44(7) . 2_755 ? O7 La1 C11 148.65(7) . 2_755 ? O13 La1 C11 70.59(7) . 2_755 ? O3 La1 C11 131.27(7) 2_765 2_755 ? O5 La1 C11 24.06(7) 2_755 2_755 ? O2 La1 C11 113.29(7) . 2_755 ? O6 La1 C11 24.82(6) 2_755 2_755 ? O1 La1 C11 97.80(7) . 2_755 ? C5 La1 C11 101.59(7) . 2_755 ? O11 La2 O10 67.33(6) . . ? O11 La2 O4 74.51(6) . 2_665 ? O10 La2 O4 70.61(6) . 2_665 ? O11 La2 O8 144.46(7) . . ? O10 La2 O8 82.60(7) . . ? O4 La2 O8 78.01(6) 2_665 . ? O11 La2 O12 114.64(6) . 2_665 ? O10 La2 O12 146.23(7) . 2_665 ? O4 La2 O12 77.49(7) 2_665 2_665 ? O8 La2 O12 80.19(7) . 2_665 ? O11 La2 O2 78.56(6) . . ? O10 La2 O2 71.94(6) . . ? O4 La2 O2 139.98(6) 2_665 . ? O8 La2 O2 110.57(6) . . ? O12 La2 O2 141.60(7) 2_665 . ? O11 La2 O1 136.08(6) . 2_765 ? O10 La2 O1 138.39(6) . 2_765 ? O4 La2 O1 139.22(6) 2_665 2_765 ? O8 La2 O1 79.22(7) . 2_765 ? O12 La2 O1 65.58(7) 2_665 2_765 ? O2 La2 O1 79.98(6) . 2_765 ? O11 La2 O3 69.82(6) . . ? O10 La2 O3 122.36(6) . . ? O4 La2 O3 130.07(6) 2_665 . ? O8 La2 O3 145.50(6) . . ? O12 La2 O3 86.77(7) 2_665 . ? O2 La2 O3 63.22(6) . . ? O1 La2 O3 66.32(6) 2_765 . ? O11 La2 O11 66.20(6) . 2_665 ? O10 La2 O11 122.50(6) . 2_665 ? O4 La2 O11 65.91(6) 2_665 2_665 ? O8 La2 O11 121.10(6) . 2_665 ? O12 La2 O11 48.49(6) 2_665 2_665 ? O2 La2 O11 127.24(6) . 2_665 ? O1 La2 O11 98.88(6) 2_765 2_665 ? O3 La2 O11 68.24(5) . 2_665 ? O11 La2 O7 129.11(6) . . ? O10 La2 O7 70.15(6) . . ? O4 La2 O7 115.57(6) 2_665 . ? O8 La2 O7 48.11(6) . . ? O12 La2 O7 116.24(6) 2_665 . ? O2 La2 O7 62.50(6) . . ? O1 La2 O7 69.82(6) 2_765 . ? O3 La2 O7 113.92(5) . . ? O11 La2 O7 164.68(5) 2_665 . ? O11 La2 C18 90.94(6) . 2_665 ? O10 La2 C18 139.92(7) . 2_665 ? O4 La2 C18 71.28(7) 2_665 2_665 ? O8 La2 C18 101.18(7) . 2_665 ? O12 La2 C18 23.80(7) 2_665 2_665 ? O2 La2 C18 138.59(6) . 2_665 ? O1 La2 C18 80.61(7) 2_765 2_665 ? O3 La2 C18 75.51(6) . 2_665 ? O11 La2 C18 24.75(6) 2_665 2_665 ? O7 La2 C18 139.94(6) . 2_665 ? O11 La2 C12 142.08(6) . . ? O10 La2 C12 74.90(7) . . ? O4 La2 C12 96.55(6) 2_665 . ? O8 La2 C12 23.70(6) . . ? O12 La2 C12 98.51(7) 2_665 . ? O2 La2 C12 86.87(6) . . ? O1 La2 C12 73.47(7) 2_765 . ? O3 La2 C12 132.82(6) . . ? O11 La2 C12 143.97(6) 2_665 . ? O7 La2 C12 24.41(6) . . ? C18 La2 C12 121.59(7) 2_665 . ? C4 S1 C1 92.07(15) . . ? C10 S2 C7 91.48(15) . . ? C13 S3 C16 91.80(16) . . ? C5 O1 La2 136.31(17) . 2_765 ? C5 O1 La1 91.14(15) . . ? La2 O1 La1 109.57(7) 2_765 . ? C5 O2 La2 143.26(16) . . ? C5 O2 La1 94.90(15) . . ? La2 O2 La1 115.90(7) . . ? C6 O3 La1 128.38(16) . 2_765 ? C6 O3 La2 116.53(15) . . ? La1 O3 La2 114.09(7) 2_765 . ? C6 O4 La2 128.01(16) . 2_665 ? C11 O5 La1 98.96(16) . 2_755 ? C11 O6 La1 155.11(17) . . ? C11 O6 La1 91.51(15) . 2_755 ? La1 O6 La1 113.38(7) . 2_755 ? C12 O7 La1 153.28(17) . . ? C12 O7 La2 89.43(15) . . ? La1 O7 La2 113.87(7) . . ? C12 O8 La2 101.82(16) . . ? C17 O9 La1 128.30(16) . . ? C17 O10 La2 122.24(16) . . ? C18 O11 La2 155.27(17) . . ? C18 O11 La2 90.92(15) . 2_665 ? La2 O11 La2 113.80(6) . 2_665 ? C18 O12 La2 100.38(16) . 2_665 ? La1 O13 H1W 129.8 . . ? La1 O13 H2W 123.7 . . ? H1W O13 H2W 102.9 . . ? H3W O14 H4W 125.1 . . ? H5W O15 H6W 110.0 . . ? C2 C1 S1 111.8(2) . . ? C2 C1 H1 124.1 . . ? S1 C1 H1 124.1 . . ? C1 C2 C3 112.2(3) . . ? C1 C2 C5 120.3(2) . . ? C3 C2 C5 126.8(2) . . ? C4 C3 C2 111.8(3) . . ? C4 C3 C6 122.1(3) . . ? C2 C3 C6 126.1(2) . . ? C3 C4 S1 112.1(2) . . ? C3 C4 H4 123.9 . . ? S1 C4 H4 123.9 . . ? O1 C5 O2 119.8(2) . . ? O1 C5 C2 120.1(2) . . ? O2 C5 C2 119.6(2) . . ? O1 C5 La1 64.20(13) . . ? O2 C5 La1 60.49(13) . . ? C2 C5 La1 150.61(17) . . ? O4 C6 O3 123.8(2) . . ? O4 C6 C3 119.3(2) . . ? O3 C6 C3 116.9(2) . . ? C8 C7 S2 112.6(2) . . ? C8 C7 H7 123.7 . . ? S2 C7 H7 123.7 . . ? C7 C8 C9 111.4(3) . . ? C7 C8 C11 118.3(3) . . ? C9 C8 C11 130.1(2) . . ? C10 C9 C8 111.5(3) . . ? C10 C9 C12 117.4(3) . . ? C8 C9 C12 131.1(2) . . ? C9 C10 S2 112.9(2) . . ? C9 C10 H10 123.5 . . ? S2 C10 H10 123.5 . . ? O5 C11 O6 120.6(2) . . ? O5 C11 C8 118.5(2) . . ? O6 C11 C8 121.0(2) . . ? O5 C11 La1 56.98(14) . 2_755 ? O6 C11 La1 63.67(14) . 2_755 ? C8 C11 La1 174.9(2) . 2_755 ? O8 C12 O7 120.6(2) . . ? O8 C12 C9 118.4(2) . . ? O7 C12 C9 120.9(2) . . ? O8 C12 La2 54.48(13) . . ? O7 C12 La2 66.16(14) . . ? C9 C12 La2 172.66(18) . . ? C14 C13 S3 112.6(3) . . ? C14 C13 H13 123.7 . . ? S3 C13 H13 123.7 . . ? C13 C14 C15 111.7(3) . . ? C13 C14 C17 119.1(3) . . ? C15 C14 C17 129.2(3) . . ? C16 C15 C14 111.5(3) . . ? C16 C15 C18 118.0(3) . . ? C14 C15 C18 130.5(3) . . ? C15 C16 S3 112.4(2) . . ? C15 C16 H16 123.8 . . ? S3 C16 H16 123.8 . . ? O10 C17 O9 123.2(3) . . ? O10 C17 C14 121.3(2) . . ? O9 C17 C14 115.5(2) . . ? O12 C18 O11 119.9(2) . . ? O12 C18 C15 118.7(2) . . ? O11 C18 C15 121.4(2) . . ? O12 C18 La2 55.82(14) . 2_665 ? O11 C18 La2 64.33(13) . 2_665 ? C15 C18 La2 172.87(19) . 2_665 ? 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 O9 La1 O1 C5 -25.00(16) . . . . ? O6 La1 O1 C5 109.4(3) . . . . ? O7 La1 O1 C5 54.95(15) . . . . ? O13 La1 O1 C5 -172.53(15) . . . . ? O3 La1 O1 C5 127.55(16) 2_765 . . . ? O5 La1 O1 C5 -97.20(15) 2_755 . . . ? O2 La1 O1 C5 13.62(14) . . . . ? O6 La1 O1 C5 -103.45(15) 2_755 . . . ? C11 La1 O1 C5 -100.80(15) 2_755 . . . ? O9 La1 O1 La2 -165.78(7) . . . 2_765 ? O6 La1 O1 La2 -31.4(3) . . . 2_765 ? O7 La1 O1 La2 -85.83(8) . . . 2_765 ? O13 La1 O1 La2 46.69(8) . . . 2_765 ? O3 La1 O1 La2 -13.23(6) 2_765 . . 2_765 ? O5 La1 O1 La2 122.02(8) 2_755 . . 2_765 ? O2 La1 O1 La2 -127.15(10) . . . 2_765 ? O6 La1 O1 La2 115.78(7) 2_755 . . 2_765 ? C5 La1 O1 La2 -140.78(18) . . . 2_765 ? C11 La1 O1 La2 118.43(8) 2_755 . . 2_765 ? O11 La2 O2 C5 -79.4(3) . . . . ? O10 La2 O2 C5 -149.1(3) . . . . ? O4 La2 O2 C5 -127.8(3) 2_665 . . . ? O8 La2 O2 C5 136.4(3) . . . . ? O12 La2 O2 C5 36.0(3) 2_665 . . . ? O1 La2 O2 C5 62.0(3) 2_765 . . . ? O3 La2 O2 C5 -6.4(3) . . . . ? O11 La2 O2 C5 -31.6(3) 2_665 . . . ? O7 La2 O2 C5 134.4(3) . . . . ? C18 La2 O2 C5 -1.2(3) 2_665 . . . ? C12 La2 O2 C5 135.8(3) . . . . ? O11 La2 O2 La1 136.56(9) . . . . ? O10 La2 O2 La1 66.90(8) . . . . ? O4 La2 O2 La1 88.23(11) 2_665 . . . ? O8 La2 O2 La1 -7.61(10) . . . . ? O12 La2 O2 La1 -108.01(10) 2_665 . . . ? O1 La2 O2 La1 -82.00(8) 2_765 . . . ? O3 La2 O2 La1 -150.43(10) . . . . ? O11 La2 O2 La1 -175.59(6) 2_665 . . . ? O7 La2 O2 La1 -9.64(6) . . . . ? C18 La2 O2 La1 -145.21(8) 2_665 . . . ? C12 La2 O2 La1 -8.23(8) . . . . ? O9 La1 O2 C5 126.80(16) . . . . ? O6 La1 O2 C5 -179.27(14) . . . . ? O7 La1 O2 C5 -148.77(17) . . . . ? O13 La1 O2 C5 -25.7(2) . . . . ? O3 La1 O2 C5 -71.08(15) 2_765 . . . ? O5 La1 O2 C5 50.61(16) 2_755 . . . ? O6 La1 O2 C5 87.14(16) 2_755 . . . ? O1 La1 O2 C5 -13.65(14) . . . . ? C11 La1 O2 C5 65.51(16) 2_755 . . . ? O9 La1 O2 La2 -73.87(8) . . . . ? O6 La1 O2 La2 -19.94(12) . . . . ? O7 La1 O2 La2 10.56(7) . . . . ? O13 La1 O2 La2 133.65(11) . . . . ? O3 La1 O2 La2 88.25(8) 2_765 . . . ? O5 La1 O2 La2 -150.06(8) 2_755 . . . ? O6 La1 O2 La2 -113.53(8) 2_755 . . . ? O1 La1 O2 La2 145.68(12) . . . . ? C5 La1 O2 La2 159.3(2) . . . . ? C11 La1 O2 La2 -135.16(8) 2_755 . . . ? O11 La2 O3 C6 0.97(17) . . . . ? O10 La2 O3 C6 -43.06(19) . . . . ? O4 La2 O3 C6 48.04(19) 2_665 . . . ? O8 La2 O3 C6 -173.82(16) . . . . ? O12 La2 O3 C6 118.72(18) 2_665 . . . ? O2 La2 O3 C6 -86.10(18) . . . . ? O1 La2 O3 C6 -176.59(19) 2_765 . . . ? O11 La2 O3 C6 72.53(17) 2_665 . . . ? O7 La2 O3 C6 -123.93(17) . . . . ? C18 La2 O3 C6 97.46(18) 2_665 . . . ? C12 La2 O3 C6 -142.66(17) . . . . ? O11 La2 O3 La1 -168.50(9) . . . 2_765 ? O10 La2 O3 La1 147.47(7) . . . 2_765 ? O4 La2 O3 La1 -121.43(8) 2_665 . . 2_765 ? O8 La2 O3 La1 16.71(14) . . . 2_765 ? O12 La2 O3 La1 -50.75(8) 2_665 . . 2_765 ? O2 La2 O3 La1 104.43(9) . . . 2_765 ? O1 La2 O3 La1 13.94(7) 2_765 . . 2_765 ? O11 La2 O3 La1 -96.94(8) 2_665 . . 2_765 ? O7 La2 O3 La1 66.60(8) . . . 2_765 ? C18 La2 O3 La1 -72.01(8) 2_665 . . 2_765 ? C12 La2 O3 La1 47.87(11) . . . 2_765 ? O9 La1 O6 C11 106.3(4) . . . . ? O7 La1 O6 C11 26.9(4) . . . . ? O13 La1 O6 C11 -110.5(4) . . . . ? O3 La1 O6 C11 -47.0(4) 2_765 . . . ? O5 La1 O6 C11 178.5(4) 2_755 . . . ? O2 La1 O6 C11 56.2(5) . . . . ? O6 La1 O6 C11 180.0(5) 2_755 . . . ? O1 La1 O6 C11 -29.9(6) . . . . ? C5 La1 O6 C11 55.4(5) . . . . ? C11 La1 O6 C11 180.0(4) 2_755 . . . ? O9 La1 O6 La1 -73.67(8) . . . 2_755 ? O7 La1 O6 La1 -153.04(9) . . . 2_755 ? O13 La1 O6 La1 69.56(8) . . . 2_755 ? O3 La1 O6 La1 133.00(7) 2_765 . . 2_755 ? O5 La1 O6 La1 -1.42(10) 2_755 . . 2_755 ? O2 La1 O6 La1 -123.77(8) . . . 2_755 ? O6 La1 O6 La1 0.0 2_755 . . 2_755 ? O1 La1 O6 La1 150.1(3) . . . 2_755 ? C5 La1 O6 La1 -124.55(15) . . . 2_755 ? C11 La1 O6 La1 0.01(8) 2_755 . . 2_755 ? O9 La1 O7 C12 -85.5(4) . . . . ? O6 La1 O7 C12 -1.7(4) . . . . ? O13 La1 O7 C12 53.4(4) . . . . ? O3 La1 O7 C12 105.6(4) 2_765 . . . ? O5 La1 O7 C12 -112.0(4) 2_755 . . . ? O2 La1 O7 C12 -158.3(4) . . . . ? O6 La1 O7 C12 -35.0(4) 2_755 . . . ? O1 La1 O7 C12 169.2(4) . . . . ? C5 La1 O7 C12 -170.8(4) . . . . ? C11 La1 O7 C12 -62.3(4) 2_755 . . . ? O9 La1 O7 La2 63.28(8) . . . . ? O6 La1 O7 La2 147.08(9) . . . . ? O13 La1 O7 La2 -157.82(7) . . . . ? O3 La1 O7 La2 -105.62(8) 2_765 . . . ? O5 La1 O7 La2 36.73(17) 2_755 . . . ? O2 La1 O7 La2 -9.57(6) . . . . ? O6 La1 O7 La2 113.76(8) 2_755 . . . ? O1 La1 O7 La2 -42.05(8) . . . . ? C5 La1 O7 La2 -22.06(8) . . . . ? C11 La1 O7 La2 86.48(14) 2_755 . . . ? O11 La2 O7 C12 131.96(15) . . . . ? O10 La2 O7 C12 97.20(16) . . . . ? O4 La2 O7 C12 41.54(17) 2_665 . . . ? O8 La2 O7 C12 -0.85(15) . . . . ? O12 La2 O7 C12 -46.64(17) 2_665 . . . ? O2 La2 O7 C12 176.61(17) . . . . ? O1 La2 O7 C12 -94.39(16) 2_765 . . . ? O3 La2 O7 C12 -145.27(15) . . . . ? O11 La2 O7 C12 -50.4(3) 2_665 . . . ? C18 La2 O7 C12 -49.40(19) 2_665 . . . ? O11 La2 O7 La1 -34.55(11) . . . . ? O10 La2 O7 La1 -69.31(8) . . . . ? O4 La2 O7 La1 -124.97(8) 2_665 . . . ? O8 La2 O7 La1 -167.36(12) . . . . ? O12 La2 O7 La1 146.85(8) 2_665 . . . ? O2 La2 O7 La1 10.10(7) . . . . ? O1 La2 O7 La1 99.10(8) 2_765 . . . ? O3 La2 O7 La1 48.22(9) . . . . ? O11 La2 O7 La1 143.07(17) 2_665 . . . ? C18 La2 O7 La1 144.09(9) 2_665 . . . ? C12 La2 O7 La1 -166.5(2) . . . . ? O11 La2 O8 C12 -100.79(19) . . . . ? O10 La2 O8 C12 -69.04(18) . . . . ? O4 La2 O8 C12 -140.70(18) 2_665 . . . ? O12 La2 O8 C12 140.14(18) 2_665 . . . ? O2 La2 O8 C12 -1.54(19) . . . . ? O1 La2 O8 C12 73.36(17) 2_765 . . . ? O3 La2 O8 C12 70.8(2) . . . . ? O11 La2 O8 C12 167.29(16) 2_665 . . . ? O7 La2 O8 C12 0.87(15) . . . . ? C18 La2 O8 C12 151.42(17) 2_665 . . . ? O6 La1 O9 C17 -130.0(2) . . . . ? O7 La1 O9 C17 -56.6(2) . . . . ? O13 La1 O9 C17 172.9(2) . . . . ? O3 La1 O9 C17 -31.4(3) 2_765 . . . ? O5 La1 O9 C17 111.3(2) 2_755 . . . ? O2 La1 O9 C17 12.5(2) . . . . ? O6 La1 O9 C17 161.5(2) 2_755 . . . ? O1 La1 O9 C17 42.3(2) . . . . ? C5 La1 O9 C17 32.1(2) . . . . ? C11 La1 O9 C17 135.7(2) 2_755 . . . ? O11 La2 O10 C17 -78.0(2) . . . . ? O4 La2 O10 C17 -158.8(2) 2_665 . . . ? O8 La2 O10 C17 121.3(2) . . . . ? O12 La2 O10 C17 -178.87(18) 2_665 . . . ? O2 La2 O10 C17 6.82(19) . . . . ? O1 La2 O10 C17 56.8(2) 2_765 . . . ? O3 La2 O10 C17 -33.0(2) . . . . ? O11 La2 O10 C17 -116.3(2) 2_665 . . . ? O7 La2 O10 C17 73.3(2) . . . . ? C18 La2 O10 C17 -140.07(19) 2_665 . . . ? C12 La2 O10 C17 98.5(2) . . . . ? O10 La2 O11 C18 33.8(4) . . . . ? O4 La2 O11 C18 108.9(4) 2_665 . . . ? O8 La2 O11 C18 68.2(4) . . . . ? O12 La2 O11 C18 176.9(4) 2_665 . . . ? O2 La2 O11 C18 -41.2(4) . . . . ? O1 La2 O11 C18 -103.5(4) 2_765 . . . ? O3 La2 O11 C18 -106.7(4) . . . . ? O11 La2 O11 C18 178.9(5) 2_665 . . . ? O7 La2 O11 C18 -1.8(4) . . . . ? C18 La2 O11 C18 179.1(4) 2_665 . . . ? C12 La2 O11 C18 28.3(5) . . . . ? O10 La2 O11 La2 -145.15(9) . . . 2_665 ? O4 La2 O11 La2 -70.08(7) 2_665 . . 2_665 ? O8 La2 O11 La2 -110.71(10) . . . 2_665 ? O12 La2 O11 La2 -2.07(10) 2_665 . . 2_665 ? O2 La2 O11 La2 139.82(8) . . . 2_665 ? O1 La2 O11 La2 77.59(10) 2_765 . . 2_665 ? O3 La2 O11 La2 74.37(7) . . . 2_665 ? O11 La2 O11 La2 0.0 2_665 . . 2_665 ? O7 La2 O11 La2 179.31(6) . . . 2_665 ? C18 La2 O11 La2 0.19(8) 2_665 . . 2_665 ? C12 La2 O11 La2 -150.68(9) . . . 2_665 ? C4 S1 C1 C2 -1.3(3) . . . . ? S1 C1 C2 C3 1.3(3) . . . . ? S1 C1 C2 C5 -169.7(2) . . . . ? C1 C2 C3 C4 -0.5(4) . . . . ? C5 C2 C3 C4 169.7(3) . . . . ? C1 C2 C3 C6 177.9(3) . . . . ? C5 C2 C3 C6 -11.8(5) . . . . ? C2 C3 C4 S1 -0.5(3) . . . . ? C6 C3 C4 S1 -179.0(2) . . . . ? C1 S1 C4 C3 1.0(3) . . . . ? La2 O1 C5 O2 95.5(3) 2_765 . . . ? La1 O1 C5 O2 -24.9(2) . . . . ? La2 O1 C5 C2 -92.6(3) 2_765 . . . ? La1 O1 C5 C2 147.0(2) . . . . ? La2 O1 C5 La1 120.4(2) 2_765 . . . ? La2 O2 C5 O1 -122.1(3) . . . . ? La1 O2 C5 O1 25.9(2) . . . . ? La2 O2 C5 C2 66.0(4) . . . . ? La1 O2 C5 C2 -146.1(2) . . . . ? La2 O2 C5 La1 -147.9(3) . . . . ? C1 C2 C5 O1 -47.3(4) . . . . ? C3 C2 C5 O1 143.2(3) . . . . ? C1 C2 C5 O2 124.6(3) . . . . ? C3 C2 C5 O2 -44.9(4) . . . . ? C1 C2 C5 La1 43.0(5) . . . . ? C3 C2 C5 La1 -126.5(3) . . . . ? O9 La1 C5 O1 156.12(15) . . . . ? O6 La1 C5 O1 -153.75(16) . . . . ? O7 La1 C5 O1 -126.80(15) . . . . ? O13 La1 C5 O1 9.12(18) . . . . ? O3 La1 C5 O1 -47.39(14) 2_765 . . . ? O5 La1 C5 O1 76.76(15) 2_755 . . . ? O2 La1 C5 O1 -155.1(2) . . . . ? O6 La1 C5 O1 93.21(15) 2_755 . . . ? C11 La1 C5 O1 83.43(15) 2_755 . . . ? O9 La1 C5 O2 -48.75(15) . . . . ? O6 La1 C5 O2 1.4(3) . . . . ? O7 La1 C5 O2 28.34(15) . . . . ? O13 La1 C5 O2 164.25(14) . . . . ? O3 La1 C5 O2 107.74(15) 2_765 . . . ? O5 La1 C5 O2 -128.11(16) 2_755 . . . ? O6 La1 C5 O2 -111.66(15) 2_755 . . . ? O1 La1 C5 O2 155.1(2) . . . . ? C11 La1 C5 O2 -121.43(15) 2_755 . . . ? O9 La1 C5 C2 50.0(4) . . . . ? O6 La1 C5 C2 100.1(4) . . . . ? O7 La1 C5 C2 127.0(4) . . . . ? O13 La1 C5 C2 -97.0(4) . . . . ? O3 La1 C5 C2 -153.6(4) 2_765 . . . ? O5 La1 C5 C2 -29.4(4) 2_755 . . . ? O2 La1 C5 C2 98.7(4) . . . . ? O6 La1 C5 C2 -13.0(4) 2_755 . . . ? O1 La1 C5 C2 -106.2(4) . . . . ? C11 La1 C5 C2 -22.7(4) 2_755 . . . ? La2 O4 C6 O3 74.7(3) 2_665 . . . ? La2 O4 C6 C3 -105.2(2) 2_665 . . . ? La1 O3 C6 O4 82.0(3) 2_765 . . . ? La2 O3 C6 O4 -85.7(3) . . . . ? La1 O3 C6 C3 -98.1(2) 2_765 . . . ? La2 O3 C6 C3 94.2(2) . . . . ? C4 C3 C6 O4 -10.1(4) . . . . ? C2 C3 C6 O4 171.6(3) . . . . ? C4 C3 C6 O3 170.0(3) . . . . ? C2 C3 C6 O3 -8.3(4) . . . . ? C10 S2 C7 C8 -1.5(3) . . . . ? S2 C7 C8 C9 0.3(4) . . . . ? S2 C7 C8 C11 175.8(2) . . . . ? C7 C8 C9 C10 1.6(4) . . . . ? C11 C8 C9 C10 -173.3(3) . . . . ? C7 C8 C9 C12 -176.5(3) . . . . ? C11 C8 C9 C12 8.6(6) . . . . ? C8 C9 C10 S2 -2.7(4) . . . . ? C12 C9 C10 S2 175.7(2) . . . . ? C7 S2 C10 C9 2.5(3) . . . . ? La1 O5 C11 O6 3.3(3) 2_755 . . . ? La1 O5 C11 C8 -177.4(2) 2_755 . . . ? La1 O6 C11 O5 176.9(3) . . . . ? La1 O6 C11 O5 -3.1(3) 2_755 . . . ? La1 O6 C11 C8 -2.3(6) . . . . ? La1 O6 C11 C8 177.6(2) 2_755 . . . ? La1 O6 C11 La1 -180.0(4) . . . 2_755 ? C7 C8 C11 O5 -28.8(4) . . . . ? C9 C8 C11 O5 145.8(3) . . . . ? C7 C8 C11 O6 150.5(3) . . . . ? C9 C8 C11 O6 -34.9(5) . . . . ? C7 C8 C11 La1 -54(2) . . . 2_755 ? C9 C8 C11 La1 120(2) . . . 2_755 ? La2 O8 C12 O7 -1.7(3) . . . . ? La2 O8 C12 C9 -178.0(2) . . . . ? La1 O7 C12 O8 153.2(3) . . . . ? La2 O7 C12 O8 1.5(3) . . . . ? La1 O7 C12 C9 -30.6(6) . . . . ? La2 O7 C12 C9 177.7(2) . . . . ? La1 O7 C12 La2 151.7(4) . . . . ? C10 C9 C12 O8 32.4(4) . . . . ? C8 C9 C12 O8 -149.6(3) . . . . ? C10 C9 C12 O7 -143.9(3) . . . . ? C8 C9 C12 O7 34.1(5) . . . . ? C10 C9 C12 La2 19.3(17) . . . . ? C8 C9 C12 La2 -162.7(13) . . . . ? O11 La2 C12 O8 111.72(18) . . . . ? O10 La2 C12 O8 106.43(18) . . . . ? O4 La2 C12 O8 38.59(18) 2_665 . . . ? O12 La2 C12 O8 -39.69(18) 2_665 . . . ? O2 La2 C12 O8 178.56(18) . . . . ? O1 La2 C12 O8 -100.97(18) 2_765 . . . ? O3 La2 C12 O8 -133.19(16) . . . . ? O11 La2 C12 O8 -18.7(2) 2_665 . . . ? O7 La2 C12 O8 -178.4(3) . . . . ? C18 La2 C12 O8 -33.4(2) 2_665 . . . ? O11 La2 C12 O7 -69.85(19) . . . . ? O10 La2 C12 O7 -75.14(15) . . . . ? O4 La2 C12 O7 -142.98(15) 2_665 . . . ? O8 La2 C12 O7 178.4(3) . . . . ? O12 La2 C12 O7 138.74(15) 2_665 . . . ? O2 La2 C12 O7 -3.01(15) . . . . ? O1 La2 C12 O7 77.46(15) 2_765 . . . ? O3 La2 C12 O7 45.24(18) . . . . ? O11 La2 C12 O7 159.75(13) 2_665 . . . ? C18 La2 C12 O7 145.00(14) 2_665 . . . ? O11 La2 C12 C9 125.9(15) . . . . ? O10 La2 C12 C9 120.6(15) . . . . ? O4 La2 C12 C9 52.8(15) 2_665 . . . ? O8 La2 C12 C9 14.2(14) . . . . ? O12 La2 C12 C9 -25.5(15) 2_665 . . . ? O2 La2 C12 C9 -167.3(15) . . . . ? O1 La2 C12 C9 -86.8(15) 2_765 . . . ? O3 La2 C12 C9 -119.0(15) . . . . ? O11 La2 C12 C9 -4.5(16) 2_665 . . . ? O7 La2 C12 C9 -164.3(16) . . . . ? C18 La2 C12 C9 -19.3(15) 2_665 . . . ? C16 S3 C13 C14 -1.2(3) . . . . ? S3 C13 C14 C15 0.2(4) . . . . ? S3 C13 C14 C17 -178.6(2) . . . . ? C13 C14 C15 C16 1.1(4) . . . . ? C17 C14 C15 C16 179.8(3) . . . . ? C13 C14 C15 C18 -178.9(3) . . . . ? C17 C14 C15 C18 -0.2(5) . . . . ? C14 C15 C16 S3 -2.0(4) . . . . ? C18 C15 C16 S3 178.0(2) . . . . ? C13 S3 C16 C15 1.8(3) . . . . ? La2 O10 C17 O9 -86.8(3) . . . . ? La2 O10 C17 C14 93.5(3) . . . . ? La1 O9 C17 O10 72.0(3) . . . . ? La1 O9 C17 C14 -108.3(2) . . . . ? C13 C14 C17 O10 149.1(3) . . . . ? C15 C14 C17 O10 -29.5(5) . . . . ? C13 C14 C17 O9 -30.6(4) . . . . ? C15 C14 C17 O9 150.8(3) . . . . ? La2 O12 C18 O11 5.7(3) 2_665 . . . ? La2 O12 C18 C15 -174.7(2) 2_665 . . . ? La2 O11 C18 O12 175.7(3) . . . . ? La2 O11 C18 O12 -5.2(3) 2_665 . . . ? La2 O11 C18 C15 -3.8(6) . . . . ? La2 O11 C18 C15 175.2(2) 2_665 . . . ? La2 O11 C18 La2 -179.0(4) . . . 2_665 ? C16 C15 C18 O12 -11.0(4) . . . . ? C14 C15 C18 O12 169.0(3) . . . . ? C16 C15 C18 O11 168.6(3) . . . . ? C14 C15 C18 O11 -11.4(5) . . . . ? C16 C15 C18 La2 -48.9(17) . . . 2_665 ? C14 C15 C18 La2 131.2(14) . . . 2_665 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H1W O10 0.85 2.10 2.853(3) 146.8 1_655 O13 H1W O4 0.85 2.42 3.016(3) 127.4 2_765 O13 H1W O11 0.85 2.57 3.170(3) 128.2 1_655 O13 H2W O9 0.85 1.94 2.693(3) 147.8 2_755 O14 H3W O8 0.85 2.25 3.037(4) 154.4 1_556 O14 H4W O15 0.85 1.94 2.786(5) 174.2 . O15 H5W O5 0.85 2.13 2.964(4) 168.3 1_566 O15 H6W O14 0.85 1.99 2.825(4) 167.0 2_666 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.973 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 932136' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_b #TrackingRef 'b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 O15 Pr2 S3' _chemical_formula_weight 846.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 '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 9.0148(15) _cell_length_b 10.4259(18) _cell_length_c 13.458(2) _cell_angle_alpha 100.259(2) _cell_angle_beta 102.113(2) _cell_angle_gamma 103.114(2) _cell_volume 1170.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6367 _cell_measurement_theta_min 0.177 _cell_measurement_theta_max 0.468 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 4.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2621 _exptl_absorpt_correction_T_max 0.5176 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8261 _diffrn_reflns_av_R_equivalents 0.0144 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4238 _reflns_number_gt 3951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+2.9358P] 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 4238 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0554 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 1.02504(2) 0.212997(19) 0.022838(15) 0.01304(7) Uani 1 1 d . . . Pr2 Pr 0.64092(2) 0.394558(19) -0.077956(14) 0.01284(7) Uani 1 1 d . . . S1 S 0.95676(17) 0.62976(15) 0.42247(9) 0.0444(3) Uani 1 1 d . . . S2 S 0.7747(3) -0.02253(19) -0.48550(10) 0.0744(6) Uani 1 1 d . . . S3 S 0.6410(2) 0.17694(17) 0.35419(11) 0.0598(5) Uani 1 1 d . . . O1 O 1.1332(3) 0.4709(3) 0.1390(2) 0.0197(6) Uani 1 1 d . . . O2 O 0.8783(3) 0.3960(3) 0.0678(2) 0.0195(6) Uani 1 1 d . . . O3 O 0.8013(3) 0.6344(3) 0.05167(19) 0.0167(5) Uani 1 1 d . . . O4 O 0.6500(3) 0.7165(3) 0.1449(2) 0.0205(6) Uani 1 1 d . . . O5 O 0.8904(4) -0.2017(3) -0.2120(2) 0.0277(7) Uani 1 1 d . . . O6 O 0.9498(3) -0.0003(3) -0.1063(2) 0.0192(6) Uani 1 1 d . . . O7 O 0.8349(3) 0.2323(3) -0.1285(2) 0.0210(6) Uani 1 1 d . . . O8 O 0.6213(3) 0.2304(3) -0.2438(2) 0.0257(6) Uani 1 1 d . . . O9 O 0.7754(3) 0.1098(3) 0.0537(2) 0.0225(6) Uani 1 1 d . . . O10 O 0.5747(3) 0.1846(3) -0.0170(2) 0.0186(5) Uani 1 1 d . . . O11 O 0.5358(3) 0.4275(3) 0.07655(19) 0.0169(5) Uani 1 1 d . . . O12 O 0.4487(3) 0.4803(3) 0.2137(2) 0.0258(6) Uani 1 1 d . . . O13 O 1.2747(3) 0.1548(3) 0.0279(2) 0.0260(6) Uani 1 1 d . . . H1W H 1.3524 0.1916 0.0080 0.039 Uiso 1 1 d R . . H2W H 1.2836 0.0759 0.0257 0.039 Uiso 1 1 d R . . O14 O 0.5325(8) 0.3500(8) 0.5653(4) 0.120(2) Uani 1 1 d . . . H3W H 0.5260 0.3152 0.6168 0.180 Uiso 1 1 d R . . H4W H 0.5791 0.4312 0.5703 0.180 Uiso 1 1 d R . . O15 O 0.7033(8) 0.6005(8) 0.5865(6) 0.144(3) Uani 1 1 d . . . H5W H 0.7462 0.6642 0.6411 0.215 Uiso 1 1 d R . . H6W H 0.6450 0.6264 0.5405 0.215 Uiso 1 1 d R . . C1 C 1.0326(5) 0.5492(5) 0.3309(3) 0.0320(10) Uani 1 1 d . . . H1 H 1.1108 0.5056 0.3466 0.038 Uiso 1 1 calc R . . C2 C 0.9646(4) 0.5567(4) 0.2327(3) 0.0180(8) Uani 1 1 d . . . C3 C 0.8510(4) 0.6323(4) 0.2317(3) 0.0177(8) Uani 1 1 d . . . C4 C 0.8358(5) 0.6784(5) 0.3296(3) 0.0297(10) Uani 1 1 d . . . H4 H 0.7678 0.7300 0.3439 0.036 Uiso 1 1 calc R . . C5 C 0.9943(4) 0.4742(4) 0.1403(3) 0.0142(7) Uani 1 1 d . . . C6 C 0.7596(4) 0.6640(4) 0.1377(3) 0.0163(7) Uani 1 1 d . . . C7 C 0.8510(8) -0.0896(6) -0.3860(4) 0.0553(17) Uani 1 1 d . . . H7 H 0.8938 -0.1626 -0.3956 0.066 Uiso 1 1 calc R . . C8 C 0.8424(5) -0.0243(4) -0.2910(3) 0.0263(9) Uani 1 1 d . . . C9 C 0.7700(5) 0.0845(4) -0.3001(3) 0.0218(8) Uani 1 1 d . . . C10 C 0.7247(6) 0.0929(5) -0.4020(3) 0.0396(12) Uani 1 1 d . . . H10 H 0.6725 0.1548 -0.4231 0.048 Uiso 1 1 calc R . . C11 C 0.8969(4) -0.0784(4) -0.1984(3) 0.0197(8) Uani 1 1 d . . . C12 C 0.7397(4) 0.1865(4) -0.2185(3) 0.0167(8) Uani 1 1 d . . . C13 C 0.6786(6) 0.1234(5) 0.2367(4) 0.0398(12) Uani 1 1 d . . . H13 H 0.7205 0.0508 0.2215 0.048 Uiso 1 1 calc R . . C14 C 0.6398(5) 0.1993(4) 0.1680(3) 0.0221(8) Uani 1 1 d . . . C15 C 0.5771(5) 0.3053(4) 0.2128(3) 0.0214(8) Uani 1 1 d . . . C16 C 0.5749(6) 0.3039(5) 0.3133(3) 0.0369(11) Uani 1 1 d . . . H16 H 0.5407 0.3659 0.3553 0.044 Uiso 1 1 calc R . . C17 C 0.6626(4) 0.1636(4) 0.0606(3) 0.0167(7) Uani 1 1 d . . . C18 C 0.5177(4) 0.4092(4) 0.1652(3) 0.0161(7) 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 Pr1 0.01264(11) 0.01182(11) 0.01698(11) 0.00506(8) 0.00463(8) 0.00594(8) Pr2 0.01204(10) 0.01390(11) 0.01495(11) 0.00427(8) 0.00511(8) 0.00607(8) S1 0.0553(8) 0.0700(9) 0.0168(5) 0.0083(5) 0.0094(5) 0.0364(7) S2 0.1539(18) 0.0843(12) 0.0179(6) 0.0143(7) 0.0230(8) 0.0953(13) S3 0.1066(13) 0.0763(11) 0.0361(7) 0.0390(7) 0.0342(8) 0.0686(10) O1 0.0152(13) 0.0214(14) 0.0250(14) 0.0061(11) 0.0075(11) 0.0075(11) O2 0.0162(13) 0.0168(14) 0.0231(14) 0.0008(11) 0.0007(11) 0.0069(11) O3 0.0166(13) 0.0169(13) 0.0202(13) 0.0059(10) 0.0090(10) 0.0069(10) O4 0.0146(13) 0.0203(14) 0.0272(15) 0.0019(11) 0.0054(11) 0.0092(11) O5 0.0423(18) 0.0185(15) 0.0238(15) 0.0056(11) 0.0049(13) 0.0142(13) O6 0.0234(14) 0.0170(14) 0.0184(13) 0.0034(11) 0.0041(11) 0.0093(11) O7 0.0257(14) 0.0203(14) 0.0171(13) 0.0039(11) 0.0026(11) 0.0101(11) O8 0.0272(15) 0.0308(16) 0.0220(14) 0.0030(12) 0.0043(12) 0.0181(13) O9 0.0203(14) 0.0203(14) 0.0361(16) 0.0126(12) 0.0146(12) 0.0121(11) O10 0.0172(13) 0.0171(13) 0.0246(14) 0.0069(11) 0.0073(11) 0.0077(11) O11 0.0196(13) 0.0165(13) 0.0176(13) 0.0062(10) 0.0069(11) 0.0074(11) O12 0.0322(16) 0.0339(17) 0.0258(15) 0.0143(13) 0.0176(13) 0.0227(13) O13 0.0185(14) 0.0163(14) 0.0496(18) 0.0126(13) 0.0148(13) 0.0084(11) O14 0.139(6) 0.174(7) 0.065(4) 0.037(4) 0.020(4) 0.078(5) O15 0.122(6) 0.163(7) 0.131(6) -0.009(5) 0.001(5) 0.076(5) C1 0.035(2) 0.043(3) 0.022(2) 0.0069(19) 0.0049(18) 0.022(2) C2 0.0160(18) 0.0181(19) 0.0199(19) 0.0048(15) 0.0039(15) 0.0051(15) C3 0.0161(18) 0.0192(19) 0.0182(18) 0.0021(15) 0.0056(15) 0.0063(15) C4 0.031(2) 0.040(3) 0.024(2) 0.0034(18) 0.0098(18) 0.019(2) C5 0.0172(18) 0.0130(18) 0.0190(18) 0.0108(14) 0.0075(15) 0.0089(14) C6 0.0131(17) 0.0131(18) 0.0199(19) 0.0015(14) 0.0021(14) 0.0017(14) C7 0.109(5) 0.057(4) 0.022(2) 0.011(2) 0.015(3) 0.067(4) C8 0.037(2) 0.027(2) 0.020(2) 0.0054(17) 0.0078(18) 0.0194(19) C9 0.029(2) 0.023(2) 0.0183(19) 0.0068(16) 0.0074(16) 0.0143(17) C10 0.070(3) 0.041(3) 0.020(2) 0.0078(19) 0.010(2) 0.039(3) C11 0.0213(19) 0.021(2) 0.021(2) 0.0063(16) 0.0083(16) 0.0094(16) C12 0.0209(19) 0.0147(19) 0.0180(19) 0.0059(14) 0.0078(15) 0.0078(15) C13 0.062(3) 0.045(3) 0.035(3) 0.024(2) 0.022(2) 0.038(3) C14 0.022(2) 0.027(2) 0.024(2) 0.0121(17) 0.0072(16) 0.0133(17) C15 0.0211(19) 0.026(2) 0.023(2) 0.0110(17) 0.0089(16) 0.0126(16) C16 0.057(3) 0.044(3) 0.027(2) 0.018(2) 0.019(2) 0.033(2) C17 0.0143(17) 0.0112(18) 0.029(2) 0.0102(15) 0.0095(15) 0.0045(14) C18 0.0118(17) 0.0176(19) 0.0197(19) 0.0066(15) 0.0040(14) 0.0040(14) _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 2.418(3) . ? Pr1 O6 2.423(3) . ? Pr1 O7 2.442(3) . ? Pr1 O13 2.451(3) . ? Pr1 O3 2.466(3) 2_765 ? Pr1 O5 2.532(3) 2_755 ? Pr1 O2 2.613(2) . ? Pr1 O6 2.690(3) 2_755 ? Pr1 O1 2.701(3) . ? Pr1 C11 2.997(4) 2_755 ? Pr2 O11 2.462(2) . ? Pr2 O10 2.464(3) . ? Pr2 O8 2.505(3) . ? Pr2 O4 2.508(3) 2_665 ? Pr2 O12 2.530(3) 2_665 ? Pr2 O1 2.570(3) 2_765 ? Pr2 O2 2.577(2) . ? Pr2 O3 2.671(3) . ? Pr2 O11 2.706(2) 2_665 ? Pr2 O7 2.795(3) . ? Pr2 C18 3.014(4) 2_665 ? S1 C4 1.706(4) . ? S1 C1 1.713(4) . ? S2 C10 1.701(4) . ? S2 C7 1.709(5) . ? S3 C16 1.700(4) . ? S3 C13 1.709(5) . ? O1 C5 1.264(4) . ? O1 Pr2 2.570(3) 2_765 ? O2 C5 1.269(4) . ? O3 C6 1.299(4) . ? O3 Pr1 2.466(3) 2_765 ? O4 C6 1.246(4) . ? O4 Pr2 2.508(3) 2_665 ? O5 C11 1.252(5) . ? O5 Pr1 2.532(3) 2_755 ? O6 C11 1.282(5) . ? O6 Pr1 2.690(3) 2_755 ? O7 C12 1.266(4) . ? O8 C12 1.260(4) . ? O9 C17 1.280(4) . ? O10 C17 1.257(5) . ? O11 C18 1.278(4) . ? O11 Pr2 2.706(2) 2_665 ? O12 C18 1.253(4) . ? O12 Pr2 2.530(3) 2_665 ? O13 H1W 0.8380 . ? O13 H2W 0.8407 . ? O14 H3W 0.8433 . ? O14 H4W 0.8397 . ? O15 H5W 0.8488 . ? O15 H6W 0.8484 . ? C1 C2 1.359(6) . ? C1 H1 0.9300 . ? C2 C3 1.426(5) . ? C2 C5 1.491(5) . ? C3 C4 1.366(5) . ? C3 C6 1.491(5) . ? C4 H4 0.9300 . ? C7 C8 1.363(6) . ? C7 H7 0.9300 . ? C8 C9 1.442(5) . ? C8 C11 1.493(5) . ? C9 C10 1.372(6) . ? C9 C12 1.501(5) . ? C10 H10 0.9300 . ? C11 Pr1 2.997(4) 2_755 ? C13 C14 1.361(6) . ? C13 H13 0.9300 . ? C14 C15 1.447(5) . ? C14 C17 1.497(5) . ? C15 C16 1.361(6) . ? C15 C18 1.496(5) . ? C16 H16 0.9300 . ? C18 Pr2 3.014(4) 2_665 ? 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 O6 80.50(9) . . ? O9 Pr1 O7 77.65(9) . . ? O6 Pr1 O7 72.69(9) . . ? O9 Pr1 O13 135.82(9) . . ? O6 Pr1 O13 76.21(9) . . ? O7 Pr1 O13 128.12(9) . . ? O9 Pr1 O3 154.34(8) . 2_765 ? O6 Pr1 O3 102.55(9) . 2_765 ? O7 Pr1 O3 79.02(9) . 2_765 ? O13 Pr1 O3 68.49(9) . 2_765 ? O9 Pr1 O5 78.44(10) . 2_755 ? O6 Pr1 O5 116.13(9) . 2_755 ? O7 Pr1 O5 152.57(9) . 2_755 ? O13 Pr1 O5 78.96(10) . 2_755 ? O3 Pr1 O5 120.81(9) 2_765 2_755 ? O9 Pr1 O2 69.60(8) . . ? O6 Pr1 O2 133.26(8) . . ? O7 Pr1 O2 66.49(8) . . ? O13 Pr1 O2 148.74(9) . . ? O3 Pr1 O2 91.34(8) 2_765 . ? O5 Pr1 O2 92.59(9) 2_755 . ? O9 Pr1 O6 70.65(8) . 2_755 ? O6 Pr1 O6 66.50(10) . 2_755 ? O7 Pr1 O6 131.33(8) . 2_755 ? O13 Pr1 O6 65.74(9) . 2_755 ? O3 Pr1 O6 134.24(8) 2_765 2_755 ? O5 Pr1 O6 49.64(8) 2_755 2_755 ? O2 Pr1 O6 129.53(8) . 2_755 ? O9 Pr1 O1 108.52(8) . . ? O6 Pr1 O1 168.87(8) . . ? O7 Pr1 O1 102.37(8) . . ? O13 Pr1 O1 100.30(8) . . ? O3 Pr1 O1 66.47(8) 2_765 . ? O5 Pr1 O1 72.91(8) 2_755 . ? O2 Pr1 O1 48.68(8) . . ? O6 Pr1 O1 122.07(8) 2_755 . ? O9 Pr1 C11 74.20(10) . 2_755 ? O6 Pr1 C11 91.81(10) . 2_755 ? O7 Pr1 C11 149.76(10) . 2_755 ? O13 Pr1 C11 69.63(10) . 2_755 ? O3 Pr1 C11 130.54(9) 2_765 2_755 ? O5 Pr1 C11 24.37(10) 2_755 2_755 ? O2 Pr1 C11 112.45(9) . 2_755 ? O6 Pr1 C11 25.32(9) 2_755 2_755 ? O1 Pr1 C11 96.87(9) . 2_755 ? O11 Pr2 O10 67.92(8) . . ? O11 Pr2 O8 144.33(9) . . ? O10 Pr2 O8 82.25(9) . . ? O11 Pr2 O4 74.81(8) . 2_665 ? O10 Pr2 O4 70.53(8) . 2_665 ? O8 Pr2 O4 77.16(9) . 2_665 ? O11 Pr2 O12 114.93(8) . 2_665 ? O10 Pr2 O12 144.71(9) . 2_665 ? O8 Pr2 O12 78.69(9) . 2_665 ? O4 Pr2 O12 76.40(9) 2_665 2_665 ? O11 Pr2 O1 135.78(8) . 2_765 ? O10 Pr2 O1 138.42(8) . 2_765 ? O8 Pr2 O1 79.72(9) . 2_765 ? O4 Pr2 O1 139.03(9) 2_665 2_765 ? O12 Pr2 O1 66.15(9) 2_665 2_765 ? O11 Pr2 O2 78.87(8) . . ? O10 Pr2 O2 71.62(8) . . ? O8 Pr2 O2 110.61(8) . . ? O4 Pr2 O2 139.79(9) 2_665 . ? O12 Pr2 O2 143.21(9) 2_665 . ? O1 Pr2 O2 80.24(8) 2_765 . ? O11 Pr2 O3 70.24(8) . . ? O10 Pr2 O3 122.80(8) . . ? O8 Pr2 O3 145.26(9) . . ? O4 Pr2 O3 131.05(8) 2_665 . ? O12 Pr2 O3 88.34(9) 2_665 . ? O1 Pr2 O3 65.58(8) 2_765 . ? O2 Pr2 O3 63.43(8) . . ? O11 Pr2 O11 65.91(9) . 2_665 ? O10 Pr2 O11 122.89(8) . 2_665 ? O8 Pr2 O11 120.90(8) . 2_665 ? O4 Pr2 O11 66.49(8) 2_665 2_665 ? O12 Pr2 O11 49.17(8) 2_665 2_665 ? O1 Pr2 O11 98.46(8) 2_765 2_665 ? O2 Pr2 O11 127.44(8) . 2_665 ? O3 Pr2 O11 68.43(7) . 2_665 ? O11 Pr2 O7 129.56(8) . . ? O10 Pr2 O7 70.18(8) . . ? O8 Pr2 O7 48.63(8) . . ? O4 Pr2 O7 115.47(8) 2_665 . ? O12 Pr2 O7 115.47(8) 2_665 . ? O1 Pr2 O7 69.76(8) 2_765 . ? O2 Pr2 O7 62.06(8) . . ? O3 Pr2 O7 113.11(8) . . ? O11 Pr2 O7 164.49(8) 2_665 . ? O11 Pr2 C18 90.99(9) . 2_665 ? O10 Pr2 C18 139.84(9) . 2_665 ? O8 Pr2 C18 100.37(9) . 2_665 ? O4 Pr2 C18 71.09(9) 2_665 2_665 ? O12 Pr2 C18 24.16(9) 2_665 2_665 ? O1 Pr2 C18 80.49(9) 2_765 2_665 ? O2 Pr2 C18 139.60(9) . 2_665 ? O3 Pr2 C18 76.29(9) . 2_665 ? O11 Pr2 C18 25.09(9) 2_665 2_665 ? O7 Pr2 C18 139.45(9) . 2_665 ? C4 S1 C1 91.9(2) . . ? C10 S2 C7 91.8(2) . . ? C16 S3 C13 91.8(2) . . ? C5 O1 Pr2 136.5(2) . 2_765 ? C5 O1 Pr1 90.7(2) . . ? Pr2 O1 Pr1 110.45(9) 2_765 . ? C5 O2 Pr2 142.9(2) . . ? C5 O2 Pr1 94.7(2) . . ? Pr2 O2 Pr1 115.81(9) . . ? C6 O3 Pr1 127.8(2) . 2_765 ? C6 O3 Pr2 116.3(2) . . ? Pr1 O3 Pr2 114.83(9) 2_765 . ? C6 O4 Pr2 127.7(2) . 2_665 ? C11 O5 Pr1 99.1(2) . 2_755 ? C11 O6 Pr1 155.6(2) . . ? C11 O6 Pr1 90.8(2) . 2_755 ? Pr1 O6 Pr1 113.50(10) . 2_755 ? C12 O7 Pr1 153.3(2) . . ? C12 O7 Pr2 88.2(2) . . ? Pr1 O7 Pr2 114.01(9) . . ? C12 O8 Pr2 102.2(2) . . ? C17 O9 Pr1 127.2(2) . . ? C17 O10 Pr2 122.4(2) . . ? C18 O11 Pr2 154.8(2) . . ? C18 O11 Pr2 91.1(2) . 2_665 ? Pr2 O11 Pr2 114.09(9) . 2_665 ? C18 O12 Pr2 100.1(2) . 2_665 ? Pr1 O13 H1W 129.6 . . ? Pr1 O13 H2W 123.2 . . ? H1W O13 H2W 102.7 . . ? H3W O14 H4W 124.4 . . ? H5W O15 H6W 110.7 . . ? C2 C1 S1 111.8(3) . . ? C2 C1 H1 124.1 . . ? S1 C1 H1 124.1 . . ? C1 C2 C3 112.3(4) . . ? C1 C2 C5 120.1(3) . . ? C3 C2 C5 126.9(3) . . ? C4 C3 C2 112.2(3) . . ? C4 C3 C6 121.8(3) . . ? C2 C3 C6 126.0(3) . . ? C3 C4 S1 111.8(3) . . ? C3 C4 H4 124.1 . . ? S1 C4 H4 124.1 . . ? O1 C5 O2 119.8(3) . . ? O1 C5 C2 120.3(3) . . ? O2 C5 C2 119.5(3) . . ? O4 C6 O3 123.8(3) . . ? O4 C6 C3 119.7(3) . . ? O3 C6 C3 116.5(3) . . ? C8 C7 S2 112.7(3) . . ? C8 C7 H7 123.7 . . ? S2 C7 H7 123.7 . . ? C7 C8 C9 111.4(4) . . ? C7 C8 C11 117.8(4) . . ? C9 C8 C11 130.6(3) . . ? C10 C9 C8 111.7(4) . . ? C10 C9 C12 117.1(3) . . ? C8 C9 C12 131.2(3) . . ? C9 C10 S2 112.4(3) . . ? C9 C10 H10 123.8 . . ? S2 C10 H10 123.8 . . ? O5 C11 O6 120.2(3) . . ? O5 C11 C8 118.9(3) . . ? O6 C11 C8 120.9(3) . . ? O5 C11 Pr1 56.53(19) . 2_755 ? O6 C11 Pr1 63.85(19) . 2_755 ? C8 C11 Pr1 173.7(3) . 2_755 ? O8 C12 O7 120.9(3) . . ? O8 C12 C9 118.2(3) . . ? O7 C12 C9 120.8(3) . . ? C14 C13 S3 112.1(3) . . ? C14 C13 H13 123.9 . . ? S3 C13 H13 123.9 . . ? C13 C14 C15 112.0(4) . . ? C13 C14 C17 118.8(4) . . ? C15 C14 C17 129.2(3) . . ? C16 C15 C14 111.2(4) . . ? C16 C15 C18 118.9(4) . . ? C14 C15 C18 130.0(3) . . ? C15 C16 S3 112.9(3) . . ? C15 C16 H16 123.5 . . ? S3 C16 H16 123.5 . . ? O10 C17 O9 123.0(4) . . ? O10 C17 C14 121.4(3) . . ? O9 C17 C14 115.5(3) . . ? O12 C18 O11 119.3(3) . . ? O12 C18 C15 119.0(3) . . ? O11 C18 C15 121.7(3) . . ? O12 C18 Pr2 55.75(18) . 2_665 ? O11 C18 Pr2 63.85(18) . 2_665 ? C15 C18 Pr2 172.5(2) . 2_665 ? 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 O9 Pr1 O1 C5 -24.8(2) . . . . ? O6 Pr1 O1 C5 118.6(4) . . . . ? O7 Pr1 O1 C5 56.2(2) . . . . ? O13 Pr1 O1 C5 -170.8(2) . . . . ? O3 Pr1 O1 C5 128.2(2) 2_765 . . . ? O5 Pr1 O1 C5 -95.9(2) 2_755 . . . ? O2 Pr1 O1 C5 13.60(19) . . . . ? O6 Pr1 O1 C5 -103.1(2) 2_755 . . . ? C11 Pr1 O1 C5 -100.4(2) 2_755 . . . ? O9 Pr1 O1 Pr2 -165.96(9) . . . 2_765 ? O6 Pr1 O1 Pr2 -22.6(5) . . . 2_765 ? O7 Pr1 O1 Pr2 -85.02(11) . . . 2_765 ? O13 Pr1 O1 Pr2 47.99(11) . . . 2_765 ? O3 Pr1 O1 Pr2 -12.97(9) 2_765 . . 2_765 ? O5 Pr1 O1 Pr2 122.95(12) 2_755 . . 2_765 ? O2 Pr1 O1 Pr2 -127.59(14) . . . 2_765 ? O6 Pr1 O1 Pr2 115.72(10) 2_755 . . 2_765 ? C11 Pr1 O1 Pr2 118.45(11) 2_755 . . 2_765 ? O11 Pr2 O2 C5 -80.5(4) . . . . ? O10 Pr2 O2 C5 -150.7(4) . . . . ? O8 Pr2 O2 C5 135.3(4) . . . . ? O4 Pr2 O2 C5 -130.3(4) 2_665 . . . ? O12 Pr2 O2 C5 36.5(4) 2_665 . . . ? O1 Pr2 O2 C5 60.3(4) 2_765 . . . ? O3 Pr2 O2 C5 -7.2(4) . . . . ? O11 Pr2 O2 C5 -32.9(4) 2_665 . . . ? O7 Pr2 O2 C5 132.5(4) . . . . ? C18 Pr2 O2 C5 -2.3(4) 2_665 . . . ? O11 Pr2 O2 Pr1 137.29(12) . . . . ? O10 Pr2 O2 Pr1 67.06(11) . . . . ? O8 Pr2 O2 Pr1 -6.87(14) . . . . ? O4 Pr2 O2 Pr1 87.54(15) 2_665 . . . ? O12 Pr2 O2 Pr1 -105.69(14) 2_665 . . . ? O1 Pr2 O2 Pr1 -81.91(11) 2_765 . . . ? O3 Pr2 O2 Pr1 -149.39(14) . . . . ? O11 Pr2 O2 Pr1 -175.14(8) 2_665 . . . ? O7 Pr2 O2 Pr1 -9.74(9) . . . . ? C18 Pr2 O2 Pr1 -144.48(12) 2_665 . . . ? O9 Pr1 O2 C5 127.5(2) . . . . ? O6 Pr1 O2 C5 -178.75(19) . . . . ? O7 Pr1 O2 C5 -147.5(2) . . . . ? O13 Pr1 O2 C5 -22.0(3) . . . . ? O3 Pr1 O2 C5 -70.1(2) 2_765 . . . ? O5 Pr1 O2 C5 50.9(2) 2_755 . . . ? O6 Pr1 O2 C5 87.4(2) 2_755 . . . ? O1 Pr1 O2 C5 -13.58(19) . . . . ? C11 Pr1 O2 C5 65.4(2) 2_755 . . . ? O9 Pr1 O2 Pr2 -74.25(12) . . . . ? O6 Pr1 O2 Pr2 -20.52(17) . . . . ? O7 Pr1 O2 Pr2 10.75(10) . . . . ? O13 Pr1 O2 Pr2 136.24(15) . . . . ? O3 Pr1 O2 Pr2 88.17(11) 2_765 . . . ? O5 Pr1 O2 Pr2 -150.90(12) 2_755 . . . ? O6 Pr1 O2 Pr2 -114.33(11) 2_755 . . . ? O1 Pr1 O2 Pr2 144.65(16) . . . . ? C11 Pr1 O2 Pr2 -136.35(11) 2_755 . . . ? O11 Pr2 O3 C6 1.1(2) . . . . ? O10 Pr2 O3 C6 -43.9(3) . . . . ? O8 Pr2 O3 C6 -174.3(2) . . . . ? O4 Pr2 O3 C6 48.1(3) 2_665 . . . ? O12 Pr2 O3 C6 118.4(2) 2_665 . . . ? O1 Pr2 O3 C6 -177.2(3) 2_765 . . . ? O2 Pr2 O3 C6 -86.1(2) . . . . ? O11 Pr2 O3 C6 72.2(2) 2_665 . . . ? O7 Pr2 O3 C6 -124.5(2) . . . . ? C18 Pr2 O3 C6 97.2(2) 2_665 . . . ? O11 Pr2 O3 Pr1 -168.11(12) . . . 2_765 ? O10 Pr2 O3 Pr1 146.86(9) . . . 2_765 ? O8 Pr2 O3 Pr1 16.48(19) . . . 2_765 ? O4 Pr2 O3 Pr1 -121.11(11) 2_665 . . 2_765 ? O12 Pr2 O3 Pr1 -50.81(10) 2_665 . . 2_765 ? O1 Pr2 O3 Pr1 13.65(9) 2_765 . . 2_765 ? O2 Pr2 O3 Pr1 104.73(12) . . . 2_765 ? O11 Pr2 O3 Pr1 -97.04(11) 2_665 . . 2_765 ? O7 Pr2 O3 Pr1 66.27(11) . . . 2_765 ? C18 Pr2 O3 Pr1 -72.00(11) 2_665 . . 2_765 ? O9 Pr1 O6 C11 103.0(6) . . . . ? O7 Pr1 O6 C11 23.1(6) . . . . ? O13 Pr1 O6 C11 -114.9(6) . . . . ? O3 Pr1 O6 C11 -51.1(6) 2_765 . . . ? O5 Pr1 O6 C11 175.0(6) 2_755 . . . ? O2 Pr1 O6 C11 53.0(6) . . . . ? O6 Pr1 O6 C11 175.9(7) 2_755 . . . ? O1 Pr1 O6 C11 -42.0(8) . . . . ? C11 Pr1 O6 C11 176.6(5) 2_755 . . . ? O9 Pr1 O6 Pr1 -72.93(11) . . . 2_755 ? O7 Pr1 O6 Pr1 -152.85(13) . . . 2_755 ? O13 Pr1 O6 Pr1 69.23(11) . . . 2_755 ? O3 Pr1 O6 Pr1 133.04(10) 2_765 . . 2_755 ? O5 Pr1 O6 Pr1 -0.89(14) 2_755 . . 2_755 ? O2 Pr1 O6 Pr1 -122.94(11) . . . 2_755 ? O6 Pr1 O6 Pr1 0.0 2_755 . . 2_755 ? O1 Pr1 O6 Pr1 142.1(4) . . . 2_755 ? C11 Pr1 O6 Pr1 0.72(11) 2_755 . . 2_755 ? O9 Pr1 O7 C12 -81.0(5) . . . . ? O6 Pr1 O7 C12 2.7(5) . . . . ? O13 Pr1 O7 C12 58.5(6) . . . . ? O3 Pr1 O7 C12 109.7(5) 2_765 . . . ? O5 Pr1 O7 C12 -110.9(5) 2_755 . . . ? O2 Pr1 O7 C12 -153.9(6) . . . . ? O6 Pr1 O7 C12 -31.1(6) 2_755 . . . ? O1 Pr1 O7 C12 172.4(5) . . . . ? C11 Pr1 O7 C12 -59.3(6) 2_755 . . . ? O9 Pr1 O7 Pr2 63.15(11) . . . . ? O6 Pr1 O7 Pr2 146.91(13) . . . . ? O13 Pr1 O7 Pr2 -157.27(10) . . . . ? O3 Pr1 O7 Pr2 -106.09(11) 2_765 . . . ? O5 Pr1 O7 Pr2 33.3(2) 2_755 . . . ? O2 Pr1 O7 Pr2 -9.76(9) . . . . ? O6 Pr1 O7 Pr2 113.04(11) 2_755 . . . ? O1 Pr1 O7 Pr2 -43.41(12) . . . . ? C11 Pr1 O7 Pr2 84.9(2) 2_755 . . . ? O11 Pr2 O7 C12 131.2(2) . . . . ? O10 Pr2 O7 C12 95.9(2) . . . . ? O8 Pr2 O7 C12 -1.4(2) . . . . ? O4 Pr2 O7 C12 40.2(2) 2_665 . . . ? O12 Pr2 O7 C12 -46.2(2) 2_665 . . . ? O1 Pr2 O7 C12 -95.5(2) 2_765 . . . ? O2 Pr2 O7 C12 175.0(2) . . . . ? O3 Pr2 O7 C12 -145.9(2) . . . . ? O11 Pr2 O7 C12 -53.5(4) 2_665 . . . ? C18 Pr2 O7 C12 -50.1(3) 2_665 . . . ? O11 Pr2 O7 Pr1 -33.55(16) . . . . ? O10 Pr2 O7 Pr1 -68.87(11) . . . . ? O8 Pr2 O7 Pr1 -166.14(17) . . . . ? O4 Pr2 O7 Pr1 -124.53(11) 2_665 . . . ? O12 Pr2 O7 Pr1 149.00(11) 2_665 . . . ? O1 Pr2 O7 Pr1 99.77(12) 2_765 . . . ? O2 Pr2 O7 Pr1 10.28(9) . . . . ? O3 Pr2 O7 Pr1 49.31(13) . . . . ? O11 Pr2 O7 Pr1 141.8(2) 2_665 . . . ? C18 Pr2 O7 Pr1 145.20(12) 2_665 . . . ? O11 Pr2 O8 C12 -101.8(3) . . . . ? O10 Pr2 O8 C12 -68.9(2) . . . . ? O4 Pr2 O8 C12 -140.6(2) 2_665 . . . ? O12 Pr2 O8 C12 140.9(2) 2_665 . . . ? O1 Pr2 O8 C12 73.4(2) 2_765 . . . ? O2 Pr2 O8 C12 -2.0(3) . . . . ? O3 Pr2 O8 C12 70.8(3) . . . . ? O11 Pr2 O8 C12 167.2(2) 2_665 . . . ? O7 Pr2 O8 C12 1.4(2) . . . . ? C18 Pr2 O8 C12 151.7(2) 2_665 . . . ? O6 Pr1 O9 C17 -131.2(3) . . . . ? O7 Pr1 O9 C17 -56.9(3) . . . . ? O13 Pr1 O9 C17 170.1(3) . . . . ? O3 Pr1 O9 C17 -31.9(4) 2_765 . . . ? O5 Pr1 O9 C17 109.5(3) 2_755 . . . ? O2 Pr1 O9 C17 12.3(3) . . . . ? O6 Pr1 O9 C17 160.6(3) 2_755 . . . ? O1 Pr1 O9 C17 42.1(3) . . . . ? C11 Pr1 O9 C17 134.2(3) 2_755 . . . ? O11 Pr2 O10 C17 -78.3(3) . . . . ? O8 Pr2 O10 C17 121.7(3) . . . . ? O4 Pr2 O10 C17 -159.3(3) 2_665 . . . ? O12 Pr2 O10 C17 179.3(2) 2_665 . . . ? O1 Pr2 O10 C17 56.8(3) 2_765 . . . ? O2 Pr2 O10 C17 6.9(3) . . . . ? O3 Pr2 O10 C17 -32.4(3) . . . . ? O11 Pr2 O10 C17 -116.4(3) 2_665 . . . ? O7 Pr2 O10 C17 73.0(3) . . . . ? C18 Pr2 O10 C17 -141.4(3) 2_665 . . . ? O10 Pr2 O11 C18 37.6(5) . . . . ? O8 Pr2 O11 C18 73.1(6) . . . . ? O4 Pr2 O11 C18 112.4(5) 2_665 . . . ? O12 Pr2 O11 C18 179.2(5) 2_665 . . . ? O1 Pr2 O11 C18 -100.2(5) 2_765 . . . ? O2 Pr2 O11 C18 -36.9(5) . . . . ? O3 Pr2 O11 C18 -102.4(5) . . . . ? O11 Pr2 O11 C18 -176.9(6) 2_665 . . . ? O7 Pr2 O11 C18 1.7(6) . . . . ? C18 Pr2 O11 C18 -177.5(5) 2_665 . . . ? O10 Pr2 O11 Pr2 -145.43(12) . . . 2_665 ? O8 Pr2 O11 Pr2 -109.98(14) . . . 2_665 ? O4 Pr2 O11 Pr2 -70.65(10) 2_665 . . 2_665 ? O12 Pr2 O11 Pr2 -3.90(13) 2_665 . . 2_665 ? O1 Pr2 O11 Pr2 76.79(14) 2_765 . . 2_665 ? O2 Pr2 O11 Pr2 140.06(11) . . . 2_665 ? O3 Pr2 O11 Pr2 74.50(10) . . . 2_665 ? O11 Pr2 O11 Pr2 0.0 2_665 . . 2_665 ? O7 Pr2 O11 Pr2 178.64(8) . . . 2_665 ? C18 Pr2 O11 Pr2 -0.55(11) 2_665 . . 2_665 ? C4 S1 C1 C2 -1.5(4) . . . . ? S1 C1 C2 C3 1.4(5) . . . . ? S1 C1 C2 C5 -169.9(3) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? C5 C2 C3 C4 170.0(4) . . . . ? C1 C2 C3 C6 177.6(4) . . . . ? C5 C2 C3 C6 -11.8(6) . . . . ? C2 C3 C4 S1 -0.5(5) . . . . ? C6 C3 C4 S1 -178.8(3) . . . . ? C1 S1 C4 C3 1.1(4) . . . . ? Pr2 O1 C5 O2 96.6(4) 2_765 . . . ? Pr1 O1 C5 O2 -24.8(3) . . . . ? Pr2 O1 C5 C2 -90.8(4) 2_765 . . . ? Pr1 O1 C5 C2 147.8(3) . . . . ? Pr2 O2 C5 O1 -120.6(4) . . . . ? Pr1 O2 C5 O1 25.7(3) . . . . ? Pr2 O2 C5 C2 66.7(5) . . . . ? Pr1 O2 C5 C2 -146.9(3) . . . . ? C1 C2 C5 O1 -47.2(5) . . . . ? C3 C2 C5 O1 142.9(4) . . . . ? C1 C2 C5 O2 125.4(4) . . . . ? C3 C2 C5 O2 -44.6(6) . . . . ? Pr2 O4 C6 O3 74.3(4) 2_665 . . . ? Pr2 O4 C6 C3 -105.9(3) 2_665 . . . ? Pr1 O3 C6 O4 82.4(4) 2_765 . . . ? Pr2 O3 C6 O4 -85.2(4) . . . . ? Pr1 O3 C6 C3 -97.4(3) 2_765 . . . ? Pr2 O3 C6 C3 95.0(3) . . . . ? C4 C3 C6 O4 -10.7(6) . . . . ? C2 C3 C6 O4 171.2(4) . . . . ? C4 C3 C6 O3 169.1(4) . . . . ? C2 C3 C6 O3 -9.0(6) . . . . ? C10 S2 C7 C8 -1.4(5) . . . . ? S2 C7 C8 C9 0.2(7) . . . . ? S2 C7 C8 C11 176.6(4) . . . . ? C7 C8 C9 C10 1.5(6) . . . . ? C11 C8 C9 C10 -174.3(5) . . . . ? C7 C8 C9 C12 -177.7(5) . . . . ? C11 C8 C9 C12 6.5(8) . . . . ? C8 C9 C10 S2 -2.5(6) . . . . ? C12 C9 C10 S2 176.8(3) . . . . ? C7 S2 C10 C9 2.2(5) . . . . ? Pr1 O5 C11 O6 5.2(4) 2_755 . . . ? Pr1 O5 C11 C8 -174.9(3) 2_755 . . . ? Pr1 O6 C11 O5 178.9(4) . . . . ? Pr1 O6 C11 O5 -4.9(4) 2_755 . . . ? Pr1 O6 C11 C8 -1.0(8) . . . . ? Pr1 O6 C11 C8 175.3(3) 2_755 . . . ? Pr1 O6 C11 Pr1 -176.2(6) . . . 2_755 ? C7 C8 C11 O5 -27.1(7) . . . . ? C9 C8 C11 O5 148.5(5) . . . . ? C7 C8 C11 O6 152.8(5) . . . . ? C9 C8 C11 O6 -31.6(7) . . . . ? C7 C8 C11 Pr1 -70(3) . . . 2_755 ? C9 C8 C11 Pr1 106(2) . . . 2_755 ? Pr2 O8 C12 O7 -2.7(4) . . . . ? Pr2 O8 C12 C9 -179.2(3) . . . . ? Pr1 O7 C12 O8 150.1(4) . . . . ? Pr2 O7 C12 O8 2.4(4) . . . . ? Pr1 O7 C12 C9 -33.6(7) . . . . ? Pr2 O7 C12 C9 178.8(3) . . . . ? C10 C9 C12 O8 31.3(6) . . . . ? C8 C9 C12 O8 -149.5(4) . . . . ? C10 C9 C12 O7 -145.1(4) . . . . ? C8 C9 C12 O7 34.0(6) . . . . ? C16 S3 C13 C14 -0.7(4) . . . . ? S3 C13 C14 C15 0.0(5) . . . . ? S3 C13 C14 C17 -178.8(3) . . . . ? C13 C14 C15 C16 1.0(6) . . . . ? C17 C14 C15 C16 179.6(4) . . . . ? C13 C14 C15 C18 -178.8(4) . . . . ? C17 C14 C15 C18 -0.1(7) . . . . ? C14 C15 C16 S3 -1.5(5) . . . . ? C18 C15 C16 S3 178.3(3) . . . . ? C13 S3 C16 C15 1.3(4) . . . . ? Pr2 O10 C17 O9 -87.7(4) . . . . ? Pr2 O10 C17 C14 93.0(4) . . . . ? Pr1 O9 C17 O10 72.6(4) . . . . ? Pr1 O9 C17 C14 -108.1(3) . . . . ? C13 C14 C17 O10 149.1(4) . . . . ? C15 C14 C17 O10 -29.4(6) . . . . ? C13 C14 C17 O9 -30.2(6) . . . . ? C15 C14 C17 O9 151.3(4) . . . . ? Pr2 O12 C18 O11 6.4(4) 2_665 . . . ? Pr2 O12 C18 C15 -173.7(3) 2_665 . . . ? Pr2 O11 C18 O12 171.3(4) . . . . ? Pr2 O11 C18 O12 -5.9(3) 2_665 . . . ? Pr2 O11 C18 C15 -8.6(8) . . . . ? Pr2 O11 C18 C15 174.2(3) 2_665 . . . ? Pr2 O11 C18 Pr2 177.2(6) . . . 2_665 ? C16 C15 C18 O12 -9.3(6) . . . . ? C14 C15 C18 O12 170.5(4) . . . . ? C16 C15 C18 O11 170.6(4) . . . . ? C14 C15 C18 O11 -9.7(6) . . . . ? C16 C15 C18 Pr2 -53(2) . . . 2_665 ? C14 C15 C18 Pr2 126.5(18) . . . 2_665 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O15 H6W O14 0.85 2.00 2.830(9) 166.2 2_666 O15 H5W O5 0.85 2.16 2.993(8) 167.1 1_566 O14 H4W O15 0.84 1.81 2.646(12) 172.6 . O14 H3W O8 0.84 2.30 3.086(6) 154.9 1_556 O13 H2W O9 0.84 1.93 2.677(4) 147.3 2_755 O13 H1W O11 0.84 2.52 3.115(4) 129.1 1_655 O13 H1W O4 0.84 2.42 3.005(4) 127.7 2_765 O13 H1W O10 0.84 2.12 2.854(4) 146.9 1_655 _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.041 _refine_diff_density_min -0.910 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 932137' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c #TrackingRef 'c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 Ce2 O15 S3' _chemical_formula_weight 844.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 '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 9.0536(11) _cell_length_b 10.4806(12) _cell_length_c 13.4765(16) _cell_angle_alpha 100.3860(10) _cell_angle_beta 102.3950(10) _cell_angle_gamma 103.0420(10) _cell_volume 1181.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6706 _cell_measurement_theta_min 0.201 _cell_measurement_theta_max 0.494 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 4.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2811 _exptl_absorpt_correction_T_max 0.5390 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8802 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4361 _reflns_number_gt 4060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+2.9403P] 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 4361 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0514 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 1.02561(2) 0.213176(18) 0.023145(14) 0.01361(6) Uani 1 1 d . . . Ce2 Ce 0.64075(2) 0.394193(18) -0.078584(14) 0.01336(6) Uani 1 1 d . . . S1 S 0.95730(16) 0.62986(15) 0.42296(8) 0.0460(3) Uani 1 1 d . . . S2 S 0.7759(2) -0.02173(17) -0.48627(9) 0.0757(6) Uani 1 1 d . . . S3 S 0.6413(2) 0.17788(16) 0.35413(10) 0.0623(4) Uani 1 1 d . . . O1 O 1.1330(3) 0.4719(2) 0.14002(19) 0.0204(5) Uani 1 1 d . . . O2 O 0.8789(3) 0.3968(2) 0.06792(19) 0.0199(5) Uani 1 1 d . . . O3 O 0.8006(3) 0.6341(2) 0.05222(18) 0.0178(5) Uani 1 1 d . . . O4 O 0.6511(3) 0.7164(2) 0.14566(19) 0.0209(5) Uani 1 1 d . . . O5 O 0.8878(3) -0.2017(3) -0.2136(2) 0.0292(6) Uani 1 1 d . . . O6 O 0.9474(3) -0.0008(2) -0.10735(19) 0.0207(5) Uani 1 1 d . . . O7 O 0.8340(3) 0.2315(2) -0.12910(19) 0.0212(5) Uani 1 1 d . . . O8 O 0.6210(3) 0.2292(3) -0.2455(2) 0.0265(6) Uani 1 1 d . . . O9 O 0.7752(3) 0.1109(2) 0.0541(2) 0.0236(6) Uani 1 1 d . . . O10 O 0.5747(3) 0.1843(2) -0.01661(19) 0.0197(5) Uani 1 1 d . . . O11 O 0.5372(3) 0.4275(2) 0.07732(18) 0.0176(5) Uani 1 1 d . . . O12 O 0.4482(3) 0.4785(3) 0.2137(2) 0.0280(6) Uani 1 1 d . . . O13 O 1.2755(3) 0.1536(3) 0.0263(2) 0.0273(6) Uani 1 1 d . . . H1W H 1.3531 0.1903 0.0064 0.041 Uiso 1 1 d R . . H2W H 1.2844 0.0747 0.0241 0.041 Uiso 1 1 d R . . O14 O 0.5317(7) 0.3494(7) 0.5649(4) 0.119(2) Uani 1 1 d . . . H3W H 0.5252 0.3146 0.6164 0.179 Uiso 1 1 d R . . H4W H 0.5783 0.4306 0.5699 0.179 Uiso 1 1 d R . . O15 O 0.7022(7) 0.5999(7) 0.5860(5) 0.132(2) Uani 1 1 d . . . H5W H 0.7452 0.6636 0.6405 0.199 Uiso 1 1 d R . . H6W H 0.6440 0.6257 0.5399 0.199 Uiso 1 1 d R . . C1 C 1.0336(5) 0.5498(4) 0.3319(3) 0.0319(9) Uani 1 1 d . . . H1 H 1.1119 0.5069 0.3478 0.038 Uiso 1 1 calc R . . C2 C 0.9653(4) 0.5568(4) 0.2335(3) 0.0188(7) Uani 1 1 d . . . C3 C 0.8513(4) 0.6327(4) 0.2321(3) 0.0187(7) Uani 1 1 d . . . C4 C 0.8369(5) 0.6775(4) 0.3300(3) 0.0321(9) Uani 1 1 d . . . H4 H 0.7688 0.7284 0.3445 0.039 Uiso 1 1 calc R . . C5 C 0.9944(4) 0.4746(3) 0.1406(3) 0.0156(7) Uani 1 1 d . . . C6 C 0.7603(4) 0.6638(3) 0.1381(3) 0.0155(7) Uani 1 1 d . . . C7 C 0.8501(8) -0.0890(5) -0.3868(3) 0.0569(16) Uani 1 1 d . . . H7 H 0.8921 -0.1621 -0.3963 0.068 Uiso 1 1 calc R . . C8 C 0.8413(5) -0.0244(4) -0.2919(3) 0.0271(8) Uani 1 1 d . . . C9 C 0.7691(5) 0.0837(4) -0.3014(3) 0.0235(8) Uani 1 1 d . . . C10 C 0.7256(6) 0.0930(5) -0.4023(3) 0.0415(12) Uani 1 1 d . . . H10 H 0.6742 0.1550 -0.4232 0.050 Uiso 1 1 calc R . . C11 C 0.8941(4) -0.0788(4) -0.1995(3) 0.0191(7) Uani 1 1 d . . . C12 C 0.7388(4) 0.1858(3) -0.2198(3) 0.0178(7) Uani 1 1 d . . . C13 C 0.6796(6) 0.1256(5) 0.2373(4) 0.0439(12) Uani 1 1 d . . . H13 H 0.7228 0.0541 0.2225 0.053 Uiso 1 1 calc R . . C14 C 0.6399(4) 0.1998(4) 0.1682(3) 0.0228(8) Uani 1 1 d . . . C15 C 0.5776(4) 0.3054(4) 0.2125(3) 0.0216(8) Uani 1 1 d . . . C16 C 0.5752(6) 0.3046(5) 0.3133(3) 0.0393(11) Uani 1 1 d . . . H16 H 0.5411 0.3663 0.3551 0.047 Uiso 1 1 calc R . . C17 C 0.6626(4) 0.1640(3) 0.0609(3) 0.0189(7) Uani 1 1 d . . . C18 C 0.5179(4) 0.4088(3) 0.1653(3) 0.0176(7) 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 0.01347(10) 0.01269(10) 0.01659(10) 0.00466(7) 0.00455(8) 0.00593(7) Ce2 0.01282(10) 0.01490(10) 0.01441(10) 0.00399(7) 0.00508(7) 0.00612(7) S1 0.0573(8) 0.0731(9) 0.0166(5) 0.0079(5) 0.0097(5) 0.0378(7) S2 0.1578(17) 0.0849(11) 0.0179(6) 0.0152(6) 0.0253(8) 0.0953(12) S3 0.1125(13) 0.0799(10) 0.0362(7) 0.0411(7) 0.0363(8) 0.0716(10) O1 0.0171(12) 0.0209(13) 0.0254(13) 0.0054(10) 0.0078(10) 0.0074(10) O2 0.0180(12) 0.0164(12) 0.0227(13) 0.0011(10) 0.0008(10) 0.0068(10) O3 0.0193(12) 0.0185(12) 0.0191(12) 0.0057(10) 0.0081(10) 0.0081(10) O4 0.0163(12) 0.0214(13) 0.0244(13) 0.0011(10) 0.0045(10) 0.0083(10) O5 0.0472(17) 0.0180(13) 0.0218(14) 0.0037(11) 0.0031(12) 0.0145(12) O6 0.0255(13) 0.0183(12) 0.0192(13) 0.0047(10) 0.0044(10) 0.0096(10) O7 0.0251(13) 0.0199(13) 0.0178(13) 0.0033(10) 0.0029(11) 0.0085(10) O8 0.0276(14) 0.0304(15) 0.0228(14) 0.0014(11) 0.0032(11) 0.0178(12) O9 0.0218(13) 0.0201(13) 0.0385(15) 0.0136(11) 0.0155(12) 0.0124(11) O10 0.0182(12) 0.0195(12) 0.0237(13) 0.0067(10) 0.0064(10) 0.0076(10) O11 0.0219(13) 0.0175(12) 0.0165(12) 0.0061(10) 0.0078(10) 0.0075(10) O12 0.0351(15) 0.0373(16) 0.0273(14) 0.0160(12) 0.0180(12) 0.0252(13) O13 0.0182(13) 0.0178(13) 0.0533(18) 0.0139(12) 0.0163(12) 0.0089(10) O14 0.140(5) 0.168(6) 0.065(3) 0.037(4) 0.017(3) 0.076(5) O15 0.120(5) 0.155(6) 0.110(5) -0.001(4) -0.001(4) 0.069(5) C1 0.035(2) 0.044(2) 0.021(2) 0.0072(18) 0.0056(17) 0.023(2) C2 0.0175(17) 0.0218(18) 0.0179(17) 0.0052(14) 0.0042(14) 0.0072(14) C3 0.0161(17) 0.0212(18) 0.0192(17) 0.0030(14) 0.0066(14) 0.0056(14) C4 0.034(2) 0.044(2) 0.022(2) 0.0016(18) 0.0090(17) 0.0207(19) C5 0.0167(17) 0.0162(16) 0.0182(17) 0.0093(14) 0.0066(14) 0.0069(13) C6 0.0145(16) 0.0122(16) 0.0197(17) 0.0024(13) 0.0054(14) 0.0038(13) C7 0.110(5) 0.060(3) 0.024(2) 0.010(2) 0.020(3) 0.068(3) C8 0.038(2) 0.028(2) 0.0201(19) 0.0049(16) 0.0073(17) 0.0188(18) C9 0.031(2) 0.0254(19) 0.0190(18) 0.0075(15) 0.0061(15) 0.0148(16) C10 0.071(3) 0.045(3) 0.021(2) 0.0069(19) 0.011(2) 0.042(3) C11 0.0201(18) 0.0207(18) 0.0180(18) 0.0036(14) 0.0058(14) 0.0090(14) C12 0.0220(18) 0.0172(17) 0.0162(17) 0.0070(14) 0.0055(14) 0.0064(14) C13 0.064(3) 0.052(3) 0.040(3) 0.025(2) 0.023(2) 0.042(3) C14 0.0224(19) 0.0273(19) 0.0261(19) 0.0131(16) 0.0092(15) 0.0135(16) C15 0.0226(19) 0.0259(19) 0.0213(18) 0.0089(15) 0.0083(15) 0.0118(15) C16 0.059(3) 0.049(3) 0.028(2) 0.019(2) 0.018(2) 0.036(2) C17 0.0174(17) 0.0129(16) 0.030(2) 0.0096(14) 0.0105(15) 0.0050(13) C18 0.0140(17) 0.0214(18) 0.0195(17) 0.0071(14) 0.0062(14) 0.0060(14) _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 O9 2.435(2) . ? Ce1 O6 2.440(2) . ? Ce1 O7 2.454(2) . ? Ce1 O13 2.473(2) . ? Ce1 O3 2.491(2) 2_765 ? Ce1 O5 2.551(3) 2_755 ? Ce1 O2 2.629(2) . ? Ce1 O6 2.709(2) 2_755 ? Ce1 O1 2.719(2) . ? Ce1 C11 3.015(3) 2_755 ? Ce2 O11 2.479(2) . ? Ce2 O10 2.486(2) . ? Ce2 O4 2.521(2) 2_665 ? Ce2 O8 2.523(2) . ? Ce2 O12 2.545(3) 2_665 ? Ce2 O2 2.583(2) . ? Ce2 O1 2.588(2) 2_765 ? Ce2 O3 2.681(2) . ? Ce2 O11 2.729(2) 2_665 ? Ce2 O7 2.806(2) . ? Ce2 C18 3.030(3) 2_665 ? S1 C4 1.700(4) . ? S1 C1 1.715(4) . ? S2 C10 1.706(4) . ? S2 C7 1.708(5) . ? S3 C16 1.704(4) . ? S3 C13 1.706(5) . ? O1 C5 1.263(4) . ? O1 Ce2 2.588(2) 2_765 ? O2 C5 1.267(4) . ? O3 C6 1.293(4) . ? O3 Ce1 2.491(2) 2_765 ? O4 C6 1.249(4) . ? O4 Ce2 2.521(2) 2_665 ? O5 C11 1.254(4) . ? O5 Ce1 2.551(3) 2_755 ? O6 C11 1.281(4) . ? O6 Ce1 2.709(2) 2_755 ? O7 C12 1.272(4) . ? O8 C12 1.257(4) . ? O9 C17 1.279(4) . ? O10 C17 1.253(4) . ? O11 C18 1.278(4) . ? O11 Ce2 2.729(2) 2_665 ? O12 C18 1.254(4) . ? O12 Ce2 2.545(3) 2_665 ? O13 H1W 0.8430 . ? O13 H2W 0.8450 . ? O14 H3W 0.8462 . ? O14 H4W 0.8442 . ? O15 H5W 0.8489 . ? O15 H6W 0.8494 . ? C1 C2 1.360(5) . ? C1 H1 0.9300 . ? C2 C3 1.437(5) . ? C2 C5 1.495(5) . ? C3 C4 1.363(5) . ? C3 C6 1.487(5) . ? C4 H4 0.9300 . ? C7 C8 1.362(6) . ? C7 H7 0.9300 . ? C8 C9 1.442(5) . ? C8 C11 1.493(5) . ? C9 C10 1.361(5) . ? C9 C12 1.505(5) . ? C10 H10 0.9300 . ? C11 Ce1 3.015(3) 2_755 ? C13 C14 1.359(6) . ? C13 H13 0.9300 . ? C14 C15 1.445(5) . ? C14 C17 1.497(5) . ? C15 C16 1.364(5) . ? C15 C18 1.495(5) . ? C16 H16 0.9300 . ? C18 Ce2 3.030(3) 2_665 ? 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 Ce1 O6 80.36(8) . . ? O9 Ce1 O7 77.47(8) . . ? O6 Ce1 O7 72.26(8) . . ? O9 Ce1 O13 136.10(8) . . ? O6 Ce1 O13 76.10(9) . . ? O7 Ce1 O13 127.50(9) . . ? O9 Ce1 O3 154.12(8) . 2_765 ? O6 Ce1 O3 102.64(8) . 2_765 ? O7 Ce1 O3 79.05(8) . 2_765 ? O13 Ce1 O3 68.33(8) . 2_765 ? O9 Ce1 O5 78.56(9) . 2_755 ? O6 Ce1 O5 116.07(8) . 2_755 ? O7 Ce1 O5 152.73(9) . 2_755 ? O13 Ce1 O5 79.34(9) . 2_755 ? O3 Ce1 O5 120.91(8) 2_765 2_755 ? O9 Ce1 O2 69.45(8) . . ? O6 Ce1 O2 132.79(8) . . ? O7 Ce1 O2 66.45(8) . . ? O13 Ce1 O2 149.12(8) . . ? O3 Ce1 O2 91.25(8) 2_765 . ? O5 Ce1 O2 92.98(8) 2_755 . ? O9 Ce1 O6 71.05(8) . 2_755 ? O6 Ce1 O6 66.74(9) . 2_755 ? O7 Ce1 O6 131.38(8) . 2_755 ? O13 Ce1 O6 65.73(8) . 2_755 ? O3 Ce1 O6 134.06(7) 2_765 2_755 ? O5 Ce1 O6 49.34(8) 2_755 2_755 ? O2 Ce1 O6 129.77(7) . 2_755 ? O9 Ce1 O1 108.06(8) . . ? O6 Ce1 O1 169.06(8) . . ? O7 Ce1 O1 102.26(8) . . ? O13 Ce1 O1 101.07(8) . . ? O3 Ce1 O1 66.70(7) 2_765 . ? O5 Ce1 O1 73.21(8) 2_755 . ? O2 Ce1 O1 48.37(7) . . ? O6 Ce1 O1 122.09(7) 2_755 . ? O9 Ce1 C11 74.48(9) . 2_755 ? O6 Ce1 C11 91.88(9) . 2_755 ? O7 Ce1 C11 149.73(9) . 2_755 ? O13 Ce1 C11 69.89(9) . 2_755 ? O3 Ce1 C11 130.48(9) 2_765 2_755 ? O5 Ce1 C11 24.25(9) 2_755 2_755 ? O2 Ce1 C11 112.77(8) . 2_755 ? O6 Ce1 C11 25.14(8) 2_755 2_755 ? O1 Ce1 C11 97.07(8) . 2_755 ? O11 Ce2 O10 67.60(8) . . ? O11 Ce2 O4 74.77(8) . 2_665 ? O10 Ce2 O4 70.62(8) . 2_665 ? O11 Ce2 O8 144.46(8) . . ? O10 Ce2 O8 82.47(8) . . ? O4 Ce2 O8 77.57(8) 2_665 . ? O11 Ce2 O12 114.88(8) . 2_665 ? O10 Ce2 O12 145.41(9) . 2_665 ? O4 Ce2 O12 76.85(9) 2_665 2_665 ? O8 Ce2 O12 79.35(8) . 2_665 ? O11 Ce2 O2 78.62(8) . . ? O10 Ce2 O2 71.65(8) . . ? O4 Ce2 O2 139.83(8) 2_665 . ? O8 Ce2 O2 110.54(8) . . ? O12 Ce2 O2 142.58(8) 2_665 . ? O11 Ce2 O1 135.85(8) . 2_765 ? O10 Ce2 O1 138.39(7) . 2_765 ? O4 Ce2 O1 139.11(8) 2_665 2_765 ? O8 Ce2 O1 79.47(8) . 2_765 ? O12 Ce2 O1 65.92(8) 2_665 2_765 ? O2 Ce2 O1 80.16(8) . 2_765 ? O11 Ce2 O3 69.92(7) . . ? O10 Ce2 O3 122.49(8) . . ? O4 Ce2 O3 130.56(7) 2_665 . ? O8 Ce2 O3 145.42(8) . . ? O12 Ce2 O3 87.71(8) 2_665 . ? O2 Ce2 O3 63.38(7) . . ? O1 Ce2 O3 65.99(7) 2_765 . ? O11 Ce2 O11 66.09(8) . 2_665 ? O10 Ce2 O11 122.71(7) . 2_665 ? O4 Ce2 O11 66.23(7) 2_665 2_665 ? O8 Ce2 O11 121.03(7) . 2_665 ? O12 Ce2 O11 48.88(7) 2_665 2_665 ? O2 Ce2 O11 127.37(7) . 2_665 ? O1 Ce2 O11 98.66(7) 2_765 2_665 ? O3 Ce2 O11 68.31(7) . 2_665 ? O11 Ce2 O7 129.26(7) . . ? O10 Ce2 O7 70.20(7) . . ? O4 Ce2 O7 115.60(7) 2_665 . ? O8 Ce2 O7 48.44(7) . . ? O12 Ce2 O7 115.83(7) 2_665 . ? O2 Ce2 O7 62.16(7) . . ? O1 Ce2 O7 69.74(7) 2_765 . ? O3 Ce2 O7 113.44(7) . . ? O11 Ce2 O7 164.61(7) 2_665 . ? O11 Ce2 C18 91.02(8) . 2_665 ? O10 Ce2 C18 139.91(8) . 2_665 ? O4 Ce2 C18 71.18(8) 2_665 2_665 ? O8 Ce2 C18 100.77(9) . 2_665 ? O12 Ce2 C18 24.02(8) 2_665 2_665 ? O2 Ce2 C18 139.19(8) . 2_665 ? O1 Ce2 C18 80.56(8) 2_765 2_665 ? O3 Ce2 C18 75.94(8) . 2_665 ? O11 Ce2 C18 24.93(8) 2_665 2_665 ? O7 Ce2 C18 139.70(8) . 2_665 ? C4 S1 C1 91.94(19) . . ? C10 S2 C7 91.4(2) . . ? C16 S3 C13 91.7(2) . . ? C5 O1 Ce2 136.6(2) . 2_765 ? C5 O1 Ce1 90.7(2) . . ? Ce2 O1 Ce1 110.11(8) 2_765 . ? C5 O2 Ce2 143.0(2) . . ? C5 O2 Ce1 94.75(19) . . ? Ce2 O2 Ce1 115.77(9) . . ? C6 O3 Ce1 127.9(2) . 2_765 ? C6 O3 Ce2 116.7(2) . . ? Ce1 O3 Ce2 114.48(9) 2_765 . ? C6 O4 Ce2 127.8(2) . 2_665 ? C11 O5 Ce1 99.1(2) . 2_755 ? C11 O6 Ce1 155.8(2) . . ? C11 O6 Ce1 90.92(19) . 2_755 ? Ce1 O6 Ce1 113.26(9) . 2_755 ? C12 O7 Ce1 153.5(2) . . ? C12 O7 Ce2 88.33(19) . . ? Ce1 O7 Ce2 113.99(9) . . ? C12 O8 Ce2 102.2(2) . . ? C17 O9 Ce1 127.7(2) . . ? C17 O10 Ce2 122.4(2) . . ? C18 O11 Ce2 155.2(2) . . ? C18 O11 Ce2 90.85(19) . 2_665 ? Ce2 O11 Ce2 113.91(8) . 2_665 ? C18 O12 Ce2 100.2(2) . 2_665 ? Ce1 O13 H1W 129.7 . . ? Ce1 O13 H2W 123.4 . . ? H1W O13 H2W 102.8 . . ? H3W O14 H4W 124.7 . . ? H5W O15 H6W 110.4 . . ? C2 C1 S1 111.7(3) . . ? C2 C1 H1 124.2 . . ? S1 C1 H1 124.2 . . ? C1 C2 C3 112.3(3) . . ? C1 C2 C5 120.4(3) . . ? C3 C2 C5 126.6(3) . . ? C4 C3 C2 111.6(3) . . ? C4 C3 C6 122.4(3) . . ? C2 C3 C6 126.0(3) . . ? C3 C4 S1 112.5(3) . . ? C3 C4 H4 123.8 . . ? S1 C4 H4 123.8 . . ? O1 C5 O2 120.1(3) . . ? O1 C5 C2 119.9(3) . . ? O2 C5 C2 119.6(3) . . ? O4 C6 O3 123.8(3) . . ? O4 C6 C3 119.3(3) . . ? O3 C6 C3 116.9(3) . . ? C8 C7 S2 112.9(3) . . ? C8 C7 H7 123.6 . . ? S2 C7 H7 123.6 . . ? C7 C8 C9 111.2(3) . . ? C7 C8 C11 118.0(3) . . ? C9 C8 C11 130.7(3) . . ? C10 C9 C8 112.0(3) . . ? C10 C9 C12 116.9(3) . . ? C8 C9 C12 131.1(3) . . ? C9 C10 S2 112.5(3) . . ? C9 C10 H10 123.7 . . ? S2 C10 H10 123.7 . . ? O5 C11 O6 120.4(3) . . ? O5 C11 C8 118.9(3) . . ? O6 C11 C8 120.6(3) . . ? O5 C11 Ce1 56.66(18) . 2_755 ? O6 C11 Ce1 63.94(18) . 2_755 ? C8 C11 Ce1 174.3(3) . 2_755 ? O8 C12 O7 121.0(3) . . ? O8 C12 C9 118.2(3) . . ? O7 C12 C9 120.7(3) . . ? C14 C13 S3 112.5(3) . . ? C14 C13 H13 123.8 . . ? S3 C13 H13 123.8 . . ? C13 C14 C15 111.9(4) . . ? C13 C14 C17 118.9(3) . . ? C15 C14 C17 129.2(3) . . ? C16 C15 C14 111.3(3) . . ? C16 C15 C18 118.4(3) . . ? C14 C15 C18 130.3(3) . . ? C15 C16 S3 112.7(3) . . ? C15 C16 H16 123.7 . . ? S3 C16 H16 123.7 . . ? O10 C17 O9 122.9(3) . . ? O10 C17 C14 121.3(3) . . ? O9 C17 C14 115.8(3) . . ? O12 C18 O11 119.7(3) . . ? O12 C18 C15 118.9(3) . . ? O11 C18 C15 121.4(3) . . ? O12 C18 Ce2 55.76(17) . 2_665 ? O11 C18 Ce2 64.22(17) . 2_665 ? C15 C18 Ce2 172.6(2) . 2_665 ? 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 O9 Ce1 O1 C5 -24.8(2) . . . . ? O6 Ce1 O1 C5 114.6(4) . . . . ? O7 Ce1 O1 C5 55.8(2) . . . . ? O13 Ce1 O1 C5 -171.54(19) . . . . ? O3 Ce1 O1 C5 128.1(2) 2_765 . . . ? O5 Ce1 O1 C5 -96.4(2) 2_755 . . . ? O2 Ce1 O1 C5 13.57(18) . . . . ? O6 Ce1 O1 C5 -103.36(19) 2_755 . . . ? C11 Ce1 O1 C5 -100.74(19) 2_755 . . . ? O9 Ce1 O1 Ce2 -165.91(9) . . . 2_765 ? O6 Ce1 O1 Ce2 -26.5(4) . . . 2_765 ? O7 Ce1 O1 Ce2 -85.27(10) . . . 2_765 ? O13 Ce1 O1 Ce2 47.37(11) . . . 2_765 ? O3 Ce1 O1 Ce2 -13.04(8) 2_765 . . 2_765 ? O5 Ce1 O1 Ce2 122.54(11) 2_755 . . 2_765 ? O2 Ce1 O1 Ce2 -127.53(13) . . . 2_765 ? O6 Ce1 O1 Ce2 115.55(9) 2_755 . . 2_765 ? C11 Ce1 O1 Ce2 118.17(10) 2_755 . . 2_765 ? O11 Ce2 O2 C5 -80.3(4) . . . . ? O10 Ce2 O2 C5 -150.3(4) . . . . ? O4 Ce2 O2 C5 -129.5(3) 2_665 . . . ? O8 Ce2 O2 C5 135.5(4) . . . . ? O12 Ce2 O2 C5 36.0(4) 2_665 . . . ? O1 Ce2 O2 C5 60.7(4) 2_765 . . . ? O3 Ce2 O2 C5 -7.3(3) . . . . ? O11 Ce2 O2 C5 -32.7(4) 2_665 . . . ? O7 Ce2 O2 C5 132.9(4) . . . . ? C18 Ce2 O2 C5 -2.2(4) 2_665 . . . ? O11 Ce2 O2 Ce1 137.04(11) . . . . ? O10 Ce2 O2 Ce1 67.08(10) . . . . ? O4 Ce2 O2 Ce1 87.86(14) 2_665 . . . ? O8 Ce2 O2 Ce1 -7.16(13) . . . . ? O12 Ce2 O2 Ce1 -106.65(13) 2_665 . . . ? O1 Ce2 O2 Ce1 -81.91(10) 2_765 . . . ? O3 Ce2 O2 Ce1 -149.88(12) . . . . ? O11 Ce2 O2 Ce1 -175.33(7) 2_665 . . . ? O7 Ce2 O2 Ce1 -9.72(8) . . . . ? C18 Ce2 O2 Ce1 -144.81(11) 2_665 . . . ? O9 Ce1 O2 C5 127.3(2) . . . . ? O6 Ce1 O2 C5 -178.87(18) . . . . ? O7 Ce1 O2 C5 -147.8(2) . . . . ? O13 Ce1 O2 C5 -23.4(3) . . . . ? O3 Ce1 O2 C5 -70.3(2) 2_765 . . . ? O5 Ce1 O2 C5 50.7(2) 2_755 . . . ? O6 Ce1 O2 C5 87.1(2) 2_755 . . . ? O1 Ce1 O2 C5 -13.57(18) . . . . ? C11 Ce1 O2 C5 65.2(2) 2_755 . . . ? O9 Ce1 O2 Ce2 -74.14(11) . . . . ? O6 Ce1 O2 Ce2 -20.36(16) . . . . ? O7 Ce1 O2 Ce2 10.73(9) . . . . ? O13 Ce1 O2 Ce2 135.14(14) . . . . ? O3 Ce1 O2 Ce2 88.21(10) 2_765 . . . ? O5 Ce1 O2 Ce2 -150.75(11) 2_755 . . . ? O6 Ce1 O2 Ce2 -114.40(11) 2_755 . . . ? O1 Ce1 O2 Ce2 144.94(15) . . . . ? C11 Ce1 O2 Ce2 -136.28(10) 2_755 . . . ? O11 Ce2 O3 C6 1.1(2) . . . . ? O10 Ce2 O3 C6 -43.4(2) . . . . ? O4 Ce2 O3 C6 48.2(2) 2_665 . . . ? O8 Ce2 O3 C6 -173.9(2) . . . . ? O12 Ce2 O3 C6 118.7(2) 2_665 . . . ? O2 Ce2 O3 C6 -86.0(2) . . . . ? O1 Ce2 O3 C6 -176.8(2) 2_765 . . . ? O11 Ce2 O3 C6 72.5(2) 2_665 . . . ? O7 Ce2 O3 C6 -124.1(2) . . . . ? C18 Ce2 O3 C6 97.5(2) 2_665 . . . ? O11 Ce2 O3 Ce1 -168.43(11) . . . 2_765 ? O10 Ce2 O3 Ce1 147.11(9) . . . 2_765 ? O4 Ce2 O3 Ce1 -121.35(10) 2_665 . . 2_765 ? O8 Ce2 O3 Ce1 16.57(18) . . . 2_765 ? O12 Ce2 O3 Ce1 -50.85(10) 2_665 . . 2_765 ? O2 Ce2 O3 Ce1 104.54(11) . . . 2_765 ? O1 Ce2 O3 Ce1 13.73(8) 2_765 . . 2_765 ? O11 Ce2 O3 Ce1 -97.03(10) 2_665 . . 2_765 ? O7 Ce2 O3 Ce1 66.40(11) . . . 2_765 ? C18 Ce2 O3 Ce1 -72.05(10) 2_665 . . 2_765 ? O9 Ce1 O6 C11 103.7(6) . . . . ? O7 Ce1 O6 C11 23.9(5) . . . . ? O13 Ce1 O6 C11 -113.6(6) . . . . ? O3 Ce1 O6 C11 -50.0(6) 2_765 . . . ? O5 Ce1 O6 C11 175.9(5) 2_755 . . . ? O2 Ce1 O6 C11 53.7(6) . . . . ? O6 Ce1 O6 C11 177.2(6) 2_755 . . . ? O1 Ce1 O6 C11 -37.4(8) . . . . ? C11 Ce1 O6 C11 177.7(5) 2_755 . . . ? O9 Ce1 O6 Ce1 -73.41(10) . . . 2_755 ? O7 Ce1 O6 Ce1 -153.24(12) . . . 2_755 ? O13 Ce1 O6 Ce1 69.24(10) . . . 2_755 ? O3 Ce1 O6 Ce1 132.80(9) 2_765 . . 2_755 ? O5 Ce1 O6 Ce1 -1.30(13) 2_755 . . 2_755 ? O2 Ce1 O6 Ce1 -123.43(10) . . . 2_755 ? O6 Ce1 O6 Ce1 0.000(1) 2_755 . . 2_755 ? O1 Ce1 O6 Ce1 145.5(3) . . . 2_755 ? C11 Ce1 O6 Ce1 0.49(11) 2_755 . . 2_755 ? O9 Ce1 O7 C12 -82.1(5) . . . . ? O6 Ce1 O7 C12 1.6(5) . . . . ? O13 Ce1 O7 C12 57.3(5) . . . . ? O3 Ce1 O7 C12 108.8(5) 2_765 . . . ? O5 Ce1 O7 C12 -111.1(5) 2_755 . . . ? O2 Ce1 O7 C12 -154.9(5) . . . . ? O6 Ce1 O7 C12 -31.8(5) 2_755 . . . ? O1 Ce1 O7 C12 171.8(5) . . . . ? C11 Ce1 O7 C12 -59.7(6) 2_755 . . . ? O9 Ce1 O7 Ce2 63.09(10) . . . . ? O6 Ce1 O7 Ce2 146.83(12) . . . . ? O13 Ce1 O7 Ce2 -157.46(9) . . . . ? O3 Ce1 O7 Ce2 -105.96(10) 2_765 . . . ? O5 Ce1 O7 Ce2 34.1(2) 2_755 . . . ? O2 Ce1 O7 Ce2 -9.73(8) . . . . ? O6 Ce1 O7 Ce2 113.37(10) 2_755 . . . ? O1 Ce1 O7 Ce2 -42.98(10) . . . . ? C11 Ce1 O7 Ce2 85.49(18) 2_755 . . . ? O11 Ce2 O7 C12 131.54(19) . . . . ? O10 Ce2 O7 C12 96.4(2) . . . . ? O4 Ce2 O7 C12 40.7(2) 2_665 . . . ? O8 Ce2 O7 C12 -1.29(18) . . . . ? O12 Ce2 O7 C12 -46.6(2) 2_665 . . . ? O2 Ce2 O7 C12 175.5(2) . . . . ? O1 Ce2 O7 C12 -95.1(2) 2_765 . . . ? O3 Ce2 O7 C12 -145.86(19) . . . . ? O11 Ce2 O7 C12 -52.6(4) 2_665 . . . ? C18 Ce2 O7 C12 -50.0(2) 2_665 . . . ? O11 Ce2 O7 Ce1 -33.69(14) . . . . ? O10 Ce2 O7 Ce1 -68.88(10) . . . . ? O4 Ce2 O7 Ce1 -124.58(10) 2_665 . . . ? O8 Ce2 O7 Ce1 -166.52(16) . . . . ? O12 Ce2 O7 Ce1 148.19(10) 2_665 . . . ? O2 Ce2 O7 Ce1 10.27(8) . . . . ? O1 Ce2 O7 Ce1 99.64(11) 2_765 . . . ? O3 Ce2 O7 Ce1 48.90(11) . . . . ? O11 Ce2 O7 Ce1 142.2(2) 2_665 . . . ? C18 Ce2 O7 Ce1 144.75(11) 2_665 . . . ? O11 Ce2 O8 C12 -101.0(2) . . . . ? O10 Ce2 O8 C12 -68.8(2) . . . . ? O4 Ce2 O8 C12 -140.5(2) 2_665 . . . ? O12 Ce2 O8 C12 140.7(2) 2_665 . . . ? O2 Ce2 O8 C12 -1.7(2) . . . . ? O1 Ce2 O8 C12 73.5(2) 2_765 . . . ? O3 Ce2 O8 C12 70.9(3) . . . . ? O11 Ce2 O8 C12 167.4(2) 2_665 . . . ? O7 Ce2 O8 C12 1.33(19) . . . . ? C18 Ce2 O8 C12 151.7(2) 2_665 . . . ? O6 Ce1 O9 C17 -130.8(3) . . . . ? O7 Ce1 O9 C17 -57.0(3) . . . . ? O13 Ce1 O9 C17 171.0(3) . . . . ? O3 Ce1 O9 C17 -31.7(4) 2_765 . . . ? O5 Ce1 O9 C17 109.9(3) 2_755 . . . ? O2 Ce1 O9 C17 12.3(3) . . . . ? O6 Ce1 O9 C17 160.6(3) 2_755 . . . ? O1 Ce1 O9 C17 42.0(3) . . . . ? C11 Ce1 O9 C17 134.5(3) 2_755 . . . ? O11 Ce2 O10 C17 -78.1(3) . . . . ? O4 Ce2 O10 C17 -159.1(3) 2_665 . . . ? O8 Ce2 O10 C17 121.4(3) . . . . ? O12 Ce2 O10 C17 -179.9(2) 2_665 . . . ? O2 Ce2 O10 C17 6.8(2) . . . . ? O1 Ce2 O10 C17 56.7(3) 2_765 . . . ? O3 Ce2 O10 C17 -32.8(3) . . . . ? O11 Ce2 O10 C17 -116.3(2) 2_665 . . . ? O7 Ce2 O10 C17 73.0(3) . . . . ? C18 Ce2 O10 C17 -140.8(2) 2_665 . . . ? O10 Ce2 O11 C18 35.8(5) . . . . ? O4 Ce2 O11 C18 110.7(5) 2_665 . . . ? O8 Ce2 O11 C18 70.6(6) . . . . ? O12 Ce2 O11 C18 178.0(5) 2_665 . . . ? O2 Ce2 O11 C18 -38.9(5) . . . . ? O1 Ce2 O11 C18 -101.7(5) 2_765 . . . ? O3 Ce2 O11 C18 -104.5(5) . . . . ? O11 Ce2 O11 C18 -178.9(6) 2_665 . . . ? O7 Ce2 O11 C18 -0.1(6) . . . . ? C18 Ce2 O11 C18 -179.1(5) 2_665 . . . ? O10 Ce2 O11 Ce2 -145.29(11) . . . 2_665 ? O4 Ce2 O11 Ce2 -70.35(9) 2_665 . . 2_665 ? O8 Ce2 O11 Ce2 -110.45(13) . . . 2_665 ? O12 Ce2 O11 Ce2 -3.07(13) 2_665 . . 2_665 ? O2 Ce2 O11 Ce2 140.04(10) . . . 2_665 ? O1 Ce2 O11 Ce2 77.27(13) 2_765 . . 2_665 ? O3 Ce2 O11 Ce2 74.43(9) . . . 2_665 ? O11 Ce2 O11 Ce2 0.0 2_665 . . 2_665 ? O7 Ce2 O11 Ce2 178.81(7) . . . 2_665 ? C18 Ce2 O11 Ce2 -0.19(10) 2_665 . . 2_665 ? C4 S1 C1 C2 -1.6(4) . . . . ? S1 C1 C2 C3 1.9(4) . . . . ? S1 C1 C2 C5 -169.7(3) . . . . ? C1 C2 C3 C4 -1.2(5) . . . . ? C5 C2 C3 C4 169.8(4) . . . . ? C1 C2 C3 C6 177.5(4) . . . . ? C5 C2 C3 C6 -11.5(6) . . . . ? C2 C3 C4 S1 0.0(4) . . . . ? C6 C3 C4 S1 -178.8(3) . . . . ? C1 S1 C4 C3 0.9(4) . . . . ? Ce2 O1 C5 O2 96.0(4) 2_765 . . . ? Ce1 O1 C5 O2 -24.9(3) . . . . ? Ce2 O1 C5 C2 -91.7(4) 2_765 . . . ? Ce1 O1 C5 C2 147.5(3) . . . . ? Ce2 O2 C5 O1 -120.9(3) . . . . ? Ce1 O2 C5 O1 25.9(3) . . . . ? Ce2 O2 C5 C2 66.8(5) . . . . ? Ce1 O2 C5 C2 -146.5(3) . . . . ? C1 C2 C5 O1 -47.0(5) . . . . ? C3 C2 C5 O1 142.7(4) . . . . ? C1 C2 C5 O2 125.4(4) . . . . ? C3 C2 C5 O2 -44.9(5) . . . . ? Ce2 O4 C6 O3 74.1(4) 2_665 . . . ? Ce2 O4 C6 C3 -105.9(3) 2_665 . . . ? Ce1 O3 C6 O4 82.5(4) 2_765 . . . ? Ce2 O3 C6 O4 -85.4(3) . . . . ? Ce1 O3 C6 C3 -97.4(3) 2_765 . . . ? Ce2 O3 C6 C3 94.7(3) . . . . ? C4 C3 C6 O4 -10.2(5) . . . . ? C2 C3 C6 O4 171.2(3) . . . . ? C4 C3 C6 O3 169.7(4) . . . . ? C2 C3 C6 O3 -8.9(5) . . . . ? C10 S2 C7 C8 -1.6(5) . . . . ? S2 C7 C8 C9 0.7(6) . . . . ? S2 C7 C8 C11 176.6(3) . . . . ? C7 C8 C9 C10 1.0(6) . . . . ? C11 C8 C9 C10 -174.3(4) . . . . ? C7 C8 C9 C12 -177.5(5) . . . . ? C11 C8 C9 C12 7.2(7) . . . . ? C8 C9 C10 S2 -2.2(5) . . . . ? C12 C9 C10 S2 176.5(3) . . . . ? C7 S2 C10 C9 2.2(5) . . . . ? Ce1 O5 C11 O6 5.2(4) 2_755 . . . ? Ce1 O5 C11 C8 -175.8(3) 2_755 . . . ? Ce1 O6 C11 O5 177.8(4) . . . . ? Ce1 O6 C11 O5 -4.8(3) 2_755 . . . ? Ce1 O6 C11 C8 -1.2(8) . . . . ? Ce1 O6 C11 C8 176.2(3) 2_755 . . . ? Ce1 O6 C11 Ce1 -177.4(6) . . . 2_755 ? C7 C8 C11 O5 -26.6(6) . . . . ? C9 C8 C11 O5 148.4(4) . . . . ? C7 C8 C11 O6 152.4(4) . . . . ? C9 C8 C11 O6 -32.6(6) . . . . ? C7 C8 C11 Ce1 -65(3) . . . 2_755 ? C9 C8 C11 Ce1 110(2) . . . 2_755 ? Ce2 O8 C12 O7 -2.6(4) . . . . ? Ce2 O8 C12 C9 -179.2(3) . . . . ? Ce1 O7 C12 O8 150.8(4) . . . . ? Ce2 O7 C12 O8 2.3(3) . . . . ? Ce1 O7 C12 C9 -32.6(7) . . . . ? Ce2 O7 C12 C9 178.8(3) . . . . ? C10 C9 C12 O8 32.0(5) . . . . ? C8 C9 C12 O8 -149.5(4) . . . . ? C10 C9 C12 O7 -144.6(4) . . . . ? C8 C9 C12 O7 33.8(6) . . . . ? C16 S3 C13 C14 -1.5(4) . . . . ? S3 C13 C14 C15 0.9(5) . . . . ? S3 C13 C14 C17 -178.5(3) . . . . ? C13 C14 C15 C16 0.4(5) . . . . ? C17 C14 C15 C16 179.6(4) . . . . ? C13 C14 C15 C18 -179.2(4) . . . . ? C17 C14 C15 C18 0.1(7) . . . . ? C14 C15 C16 S3 -1.5(5) . . . . ? C18 C15 C16 S3 178.1(3) . . . . ? C13 S3 C16 C15 1.7(4) . . . . ? Ce2 O10 C17 O9 -87.3(4) . . . . ? Ce2 O10 C17 C14 93.3(3) . . . . ? Ce1 O9 C17 O10 72.5(4) . . . . ? Ce1 O9 C17 C14 -108.2(3) . . . . ? C13 C14 C17 O10 149.5(4) . . . . ? C15 C14 C17 O10 -29.7(6) . . . . ? C13 C14 C17 O9 -29.9(5) . . . . ? C15 C14 C17 O9 150.9(4) . . . . ? Ce2 O12 C18 O11 6.2(4) 2_665 . . . ? Ce2 O12 C18 C15 -174.0(3) 2_665 . . . ? Ce2 O11 C18 O12 173.3(3) . . . . ? Ce2 O11 C18 O12 -5.7(3) 2_665 . . . ? Ce2 O11 C18 C15 -6.4(7) . . . . ? Ce2 O11 C18 C15 174.5(3) 2_665 . . . ? Ce2 O11 C18 Ce2 179.0(5) . . . 2_665 ? C16 C15 C18 O12 -9.7(5) . . . . ? C14 C15 C18 O12 169.8(4) . . . . ? C16 C15 C18 O11 170.0(4) . . . . ? C14 C15 C18 O11 -10.5(6) . . . . ? C16 C15 C18 Ce2 -52(2) . . . 2_665 ? C14 C15 C18 Ce2 127.6(18) . . . 2_665 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H1W O10 0.84 2.11 2.850(3) 146.8 1_655 O13 H1W O4 0.84 2.42 3.010(4) 127.5 2_765 O13 H1W O11 0.84 2.54 3.138(3) 128.7 1_655 O13 H2W O9 0.84 1.93 2.682(3) 147.7 2_755 O14 H3W O8 0.85 2.30 3.083(6) 154.5 1_556 O14 H4W O15 0.84 1.82 2.659(10) 172.6 . O15 H5W O5 0.85 2.15 2.982(7) 167.5 1_566 O15 H6W O14 0.85 1.99 2.820(8) 166.5 2_666 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.073 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.099 _database_code_depnum_ccdc_archive 'CCDC 932138'