# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Odile Eisenstein' _publ_contact_author_email eisenst@univ-montp2.fr loop_ _publ_author_name 'Evan Werkema' 'Ludovic Castro' 'Laurent Maron' 'Odile Eisenstein' R.Andersen data_shelxl _database_code_depnum_ccdc_archive 'CCDC 889316' #TrackingRef 'Cp2Ce-SO3-CeCp2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ceotfb _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H116 Ce2 O3 S' _chemical_formula_weight 1293.91 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.6275(8) _cell_length_b 10.5366(4) _cell_length_c 30.6641(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.5900(10) _cell_angle_gamma 90.00 _cell_volume 6571.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9193 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 25.33 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 1.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8693 _exptl_absorpt_correction_T_max 0.9580 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 123246 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.37 _reflns_number_total 12055 _reflns_number_gt 9588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0328P)^2^+14.9676P] 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 12055 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 C1 C 0.7544(2) 0.2989(4) 0.74989(14) 0.0214(9) Uani 1 1 d . . . C2 C 0.72660(19) 0.2525(4) 0.78545(14) 0.0214(9) Uani 1 1 d . . . H2 H 0.7487 0.2453 0.8144 0.026 Uiso 1 1 calc R . . C3 C 0.65943(19) 0.2180(4) 0.77090(14) 0.0206(9) Uani 1 1 d . . . C4 C 0.64559(19) 0.2413(4) 0.72414(13) 0.0203(9) Uani 1 1 d . . . C5 C 0.7052(2) 0.2904(4) 0.71272(14) 0.0222(9) Uani 1 1 d . . . H5 H 0.7105 0.3135 0.6843 0.027 Uiso 1 1 calc R . . C6 C 0.8234(2) 0.3530(4) 0.75275(15) 0.0255(10) Uani 1 1 d . . . C7 C 0.8324(2) 0.4625(4) 0.78642(15) 0.0318(11) Uani 1 1 d . . . H7A H 0.8045 0.5320 0.7752 0.048 Uiso 1 1 calc R . . H7B H 0.8775 0.4898 0.7912 0.048 Uiso 1 1 calc R . . H7C H 0.8210 0.4339 0.8139 0.048 Uiso 1 1 calc R . . C8 C 0.8730(2) 0.2502(5) 0.76932(19) 0.0462(14) Uani 1 1 d . . . H8A H 0.8640 0.2173 0.7969 0.069 Uiso 1 1 calc R . . H8B H 0.9166 0.2853 0.7736 0.069 Uiso 1 1 calc R . . H8C H 0.8699 0.1829 0.7480 0.069 Uiso 1 1 calc R . . C9 C 0.8353(2) 0.4030(5) 0.70785(16) 0.0393(13) Uani 1 1 d . . . H9A H 0.8300 0.3350 0.6867 0.059 Uiso 1 1 calc R . . H9B H 0.8792 0.4362 0.7107 0.059 Uiso 1 1 calc R . . H9C H 0.8043 0.4691 0.6980 0.059 Uiso 1 1 calc R . . C10 C 0.61600(19) 0.1986(4) 0.80667(14) 0.0219(9) Uani 1 1 d . . . C11 C 0.5959(2) 0.3317(4) 0.82157(15) 0.0288(10) Uani 1 1 d . . . H11A H 0.5714 0.3756 0.7967 0.043 Uiso 1 1 calc R . . H11B H 0.6347 0.3794 0.8329 0.043 Uiso 1 1 calc R . . H11C H 0.5693 0.3224 0.8442 0.043 Uiso 1 1 calc R . . C12 C 0.6554(2) 0.1331(5) 0.84773(15) 0.0340(11) Uani 1 1 d . . . H12A H 0.6272 0.1189 0.8692 0.051 Uiso 1 1 calc R . . H12B H 0.6915 0.1863 0.8603 0.051 Uiso 1 1 calc R . . H12C H 0.6720 0.0532 0.8392 0.051 Uiso 1 1 calc R . . C13 C 0.5536(2) 0.1192(4) 0.79392(15) 0.0279(10) Uani 1 1 d . . . H13A H 0.5266 0.1565 0.7686 0.042 Uiso 1 1 calc R . . H13B H 0.5297 0.1170 0.8182 0.042 Uiso 1 1 calc R . . H13C H 0.5653 0.0344 0.7869 0.042 Uiso 1 1 calc R . . C14 C 0.58134(19) 0.2413(4) 0.68955(14) 0.0223(9) Uani 1 1 d . . . C15 C 0.5316(2) 0.3353(4) 0.70313(15) 0.0289(10) Uani 1 1 d . . . H15A H 0.5519 0.4170 0.7086 0.043 Uiso 1 1 calc R . . H15B H 0.5172 0.3057 0.7295 0.043 Uiso 1 1 calc R . . H15C H 0.4944 0.3422 0.6798 0.043 Uiso 1 1 calc R . . C16 C 0.5953(2) 0.2886(5) 0.64491(14) 0.0303(11) Uani 1 1 d . . . H16A H 0.6278 0.2351 0.6351 0.045 Uiso 1 1 calc R . . H16B H 0.6114 0.3741 0.6479 0.045 Uiso 1 1 calc R . . H16C H 0.5556 0.2862 0.6236 0.045 Uiso 1 1 calc R . . C17 C 0.5495(2) 0.1101(4) 0.68093(14) 0.0247(9) Uani 1 1 d . . . H17A H 0.5082 0.1185 0.6614 0.037 Uiso 1 1 calc R . . H17B H 0.5423 0.0737 0.7084 0.037 Uiso 1 1 calc R . . H17C H 0.5781 0.0559 0.6676 0.037 Uiso 1 1 calc R . . C18 C 0.73492(19) -0.2097(4) 0.76117(13) 0.0197(9) Uani 1 1 d . . . C19 C 0.76789(19) -0.1481(4) 0.79924(13) 0.0200(9) Uani 1 1 d . . . H19 H 0.7493 -0.1295 0.8241 0.024 Uiso 1 1 calc R . . C20 C 0.83387(19) -0.1182(4) 0.79430(13) 0.0202(9) Uani 1 1 d . . . C21 C 0.84116(19) -0.1592(4) 0.75091(13) 0.0190(9) Uani 1 1 d . . . C22 C 0.77965(19) -0.2130(4) 0.73118(14) 0.0206(9) Uani 1 1 d . . . H22 H 0.7705 -0.2455 0.7026 0.025 Uiso 1 1 calc R . . C23 C 0.66496(19) -0.2617(4) 0.75392(14) 0.0215(9) Uani 1 1 d . . . C24 C 0.6200(2) -0.1617(4) 0.72823(15) 0.0263(10) Uani 1 1 d . . . H24A H 0.6228 -0.0842 0.7449 0.040 Uiso 1 1 calc R . . H24B H 0.5755 -0.1918 0.7234 0.040 Uiso 1 1 calc R . . H24C H 0.6336 -0.1465 0.7002 0.040 Uiso 1 1 calc R . . C25 C 0.6608(2) -0.3832(4) 0.72663(17) 0.0339(11) Uani 1 1 d . . . H25A H 0.6762 -0.3669 0.6993 0.051 Uiso 1 1 calc R . . H25B H 0.6160 -0.4118 0.7206 0.051 Uiso 1 1 calc R . . H25C H 0.6877 -0.4475 0.7429 0.051 Uiso 1 1 calc R . . C26 C 0.6423(2) -0.2881(5) 0.79785(15) 0.0352(12) Uani 1 1 d . . . H26A H 0.6729 -0.3445 0.8152 0.053 Uiso 1 1 calc R . . H26B H 0.5996 -0.3266 0.7925 0.053 Uiso 1 1 calc R . . H26C H 0.6403 -0.2098 0.8136 0.053 Uiso 1 1 calc R . . C27 C 0.8815(2) -0.0865(4) 0.83725(14) 0.0255(10) Uani 1 1 d . . . C28 C 0.8491(2) 0.0041(5) 0.86654(15) 0.0327(11) Uani 1 1 d . . . H28A H 0.8802 0.0257 0.8924 0.049 Uiso 1 1 calc R . . H28B H 0.8117 -0.0366 0.8753 0.049 Uiso 1 1 calc R . . H28C H 0.8353 0.0799 0.8503 0.049 Uiso 1 1 calc R . . C29 C 0.8950(2) -0.2137(5) 0.86273(15) 0.0344(11) Uani 1 1 d . . . H29A H 0.9150 -0.2727 0.8451 0.052 Uiso 1 1 calc R . . H29B H 0.8542 -0.2483 0.8686 0.052 Uiso 1 1 calc R . . H29C H 0.9239 -0.1990 0.8902 0.052 Uiso 1 1 calc R . . C30 C 0.9480(2) -0.0280(5) 0.83282(16) 0.0330(11) Uani 1 1 d . . . H30A H 0.9412 0.0530 0.8185 0.050 Uiso 1 1 calc R . . H30B H 0.9708 -0.0831 0.8155 0.050 Uiso 1 1 calc R . . H30C H 0.9738 -0.0173 0.8617 0.050 Uiso 1 1 calc R . . C31 C 0.9022(2) -0.1738(4) 0.72755(14) 0.0240(9) Uani 1 1 d . . . C32 C 0.8808(2) -0.2231(4) 0.67997(15) 0.0306(11) Uani 1 1 d . . . H32A H 0.9188 -0.2325 0.6659 0.046 Uiso 1 1 calc R . . H32B H 0.8509 -0.1638 0.6636 0.046 Uiso 1 1 calc R . . H32C H 0.8595 -0.3038 0.6808 0.046 Uiso 1 1 calc R . . C33 C 0.9394(2) -0.0500(4) 0.72281(15) 0.0278(10) Uani 1 1 d . . . H33A H 0.9529 -0.0129 0.7515 0.042 Uiso 1 1 calc R . . H33B H 0.9112 0.0080 0.7044 0.042 Uiso 1 1 calc R . . H33C H 0.9775 -0.0677 0.7096 0.042 Uiso 1 1 calc R . . C34 C 0.9478(2) -0.2750(4) 0.75172(16) 0.0320(11) Uani 1 1 d . . . H34A H 0.9819 -0.2940 0.7350 0.048 Uiso 1 1 calc R . . H34B H 0.9230 -0.3505 0.7549 0.048 Uiso 1 1 calc R . . H34C H 0.9670 -0.2440 0.7804 0.048 Uiso 1 1 calc R . . C35 C 0.87811(18) -0.1870(4) 0.52050(13) 0.0177(8) Uani 1 1 d . . . C36 C 0.85188(18) -0.1308(4) 0.48004(13) 0.0200(9) Uani 1 1 d . . . H36 H 0.8369 -0.1752 0.4541 0.024 Uiso 1 1 calc R . . C37 C 0.85133(19) 0.0045(4) 0.48422(13) 0.0202(9) Uani 1 1 d . . . C38 C 0.87860(18) 0.0320(4) 0.52973(13) 0.0189(9) Uani 1 1 d . . . C39 C 0.89254(18) -0.0866(4) 0.55100(13) 0.0180(8) Uani 1 1 d . . . H39 H 0.9089 -0.0968 0.5809 0.022 Uiso 1 1 calc R . . C40 C 0.88588(19) -0.3267(4) 0.53207(13) 0.0206(9) Uani 1 1 d . . . C41 C 0.8812(2) -0.4086(4) 0.49032(14) 0.0264(10) Uani 1 1 d . . . H41A H 0.8388 -0.3970 0.4723 0.040 Uiso 1 1 calc R . . H41B H 0.8868 -0.4963 0.4986 0.040 Uiso 1 1 calc R . . H41C H 0.9149 -0.3838 0.4739 0.040 Uiso 1 1 calc R . . C42 C 0.9522(2) -0.3528(4) 0.56122(14) 0.0262(10) Uani 1 1 d . . . H42A H 0.9871 -0.3284 0.5457 0.039 Uiso 1 1 calc R . . H42B H 0.9558 -0.4417 0.5681 0.039 Uiso 1 1 calc R . . H42C H 0.9554 -0.3048 0.5881 0.039 Uiso 1 1 calc R . . C43 C 0.8309(2) -0.3636(4) 0.55786(14) 0.0249(10) Uani 1 1 d . . . H43A H 0.8348 -0.3139 0.5844 0.037 Uiso 1 1 calc R . . H43B H 0.8345 -0.4520 0.5654 0.037 Uiso 1 1 calc R . . H43C H 0.7889 -0.3478 0.5399 0.037 Uiso 1 1 calc R . . C44 C 0.8383(2) 0.0838(4) 0.44119(13) 0.0220(9) Uani 1 1 d . . . C45 C 0.9012(2) 0.0762(4) 0.41970(15) 0.0302(11) Uani 1 1 d . . . H45A H 0.8949 0.1250 0.3929 0.045 Uiso 1 1 calc R . . H45B H 0.9097 -0.0107 0.4131 0.045 Uiso 1 1 calc R . . H45C H 0.9379 0.1095 0.4398 0.045 Uiso 1 1 calc R . . C46 C 0.7816(2) 0.0241(4) 0.40849(13) 0.0266(10) Uani 1 1 d . . . H46A H 0.7425 0.0222 0.4217 0.040 Uiso 1 1 calc R . . H46B H 0.7932 -0.0609 0.4015 0.040 Uiso 1 1 calc R . . H46C H 0.7736 0.0738 0.3819 0.040 Uiso 1 1 calc R . . C47 C 0.8201(2) 0.2234(4) 0.44509(15) 0.0294(10) Uani 1 1 d . . . H47A H 0.7802 0.2296 0.4573 0.044 Uiso 1 1 calc R . . H47B H 0.8138 0.2620 0.4163 0.044 Uiso 1 1 calc R . . H47C H 0.8549 0.2664 0.4641 0.044 Uiso 1 1 calc R . . C48 C 0.90141(19) 0.1555(4) 0.55476(14) 0.0222(9) Uani 1 1 d . . . C49 C 0.9564(2) 0.2164(4) 0.53392(15) 0.0281(10) Uani 1 1 d . . . H49A H 0.9396 0.2403 0.5040 0.042 Uiso 1 1 calc R . . H49B H 0.9916 0.1566 0.5342 0.042 Uiso 1 1 calc R . . H49C H 0.9726 0.2903 0.5506 0.042 Uiso 1 1 calc R . . C50 C 0.8462(2) 0.2524(4) 0.55710(14) 0.0261(10) Uani 1 1 d . . . H50A H 0.8645 0.3272 0.5723 0.039 Uiso 1 1 calc R . . H50B H 0.8142 0.2158 0.5728 0.039 Uiso 1 1 calc R . . H50C H 0.8256 0.2746 0.5277 0.039 Uiso 1 1 calc R . . C51 C 0.9309(2) 0.1268(4) 0.60318(14) 0.0264(10) Uani 1 1 d . . . H51A H 0.9684 0.0723 0.6041 0.040 Uiso 1 1 calc R . . H51B H 0.8985 0.0856 0.6174 0.040 Uiso 1 1 calc R . . H51C H 0.9442 0.2048 0.6183 0.040 Uiso 1 1 calc R . . C52 C 0.62709(18) -0.0279(4) 0.50249(13) 0.0195(9) Uani 1 1 d . . . C53 C 0.62360(18) -0.1002(4) 0.54057(13) 0.0193(9) Uani 1 1 d . . . H53 H 0.6156 -0.0672 0.5673 0.023 Uiso 1 1 calc R . . C54 C 0.63392(18) -0.2307(4) 0.53247(13) 0.0192(9) Uani 1 1 d . . . C55 C 0.64770(19) -0.2390(4) 0.48790(13) 0.0191(9) Uani 1 1 d . . . C56 C 0.64331(18) -0.1134(4) 0.47078(13) 0.0190(9) Uani 1 1 d . . . H56 H 0.6502 -0.0909 0.4426 0.023 Uiso 1 1 calc R . . C57 C 0.61801(19) 0.1156(4) 0.49797(14) 0.0222(9) Uani 1 1 d . . . C58 C 0.6000(2) 0.1538(4) 0.44953(14) 0.0296(10) Uani 1 1 d . . . H58A H 0.5925 0.2437 0.4475 0.044 Uiso 1 1 calc R . . H58B H 0.5608 0.1099 0.4364 0.044 Uiso 1 1 calc R . . H58C H 0.6353 0.1318 0.4342 0.044 Uiso 1 1 calc R . . C59 C 0.6822(2) 0.1795(4) 0.51836(16) 0.0324(11) Uani 1 1 d . . . H59A H 0.6922 0.1588 0.5492 0.049 Uiso 1 1 calc R . . H59B H 0.6778 0.2698 0.5150 0.049 Uiso 1 1 calc R . . H59C H 0.7170 0.1502 0.5037 0.049 Uiso 1 1 calc R . . C60 C 0.5626(2) 0.1588(4) 0.52277(16) 0.0336(11) Uani 1 1 d . . . H60A H 0.5725 0.1320 0.5531 0.050 Uiso 1 1 calc R . . H60B H 0.5217 0.1217 0.5091 0.050 Uiso 1 1 calc R . . H60C H 0.5590 0.2496 0.5216 0.050 Uiso 1 1 calc R . . C61 C 0.6210(2) -0.3317(4) 0.56661(14) 0.0232(9) Uani 1 1 d . . . C62 C 0.6818(2) -0.4120(4) 0.58503(15) 0.0298(11) Uani 1 1 d . . . H62A H 0.6700 -0.4739 0.6053 0.045 Uiso 1 1 calc R . . H62B H 0.7156 -0.3578 0.6001 0.045 Uiso 1 1 calc R . . H62C H 0.6975 -0.4543 0.5611 0.045 Uiso 1 1 calc R . . C63 C 0.5632(2) -0.4174(4) 0.54733(15) 0.0288(10) Uani 1 1 d . . . H63A H 0.5742 -0.4638 0.5226 0.043 Uiso 1 1 calc R . . H63B H 0.5250 -0.3662 0.5377 0.043 Uiso 1 1 calc R . . H63C H 0.5542 -0.4758 0.5696 0.043 Uiso 1 1 calc R . . C64 C 0.6001(2) -0.2653(4) 0.60705(14) 0.0299(10) Uani 1 1 d . . . H64A H 0.5602 -0.2187 0.5977 0.045 Uiso 1 1 calc R . . H64B H 0.6341 -0.2080 0.6200 0.045 Uiso 1 1 calc R . . H64C H 0.5930 -0.3278 0.6285 0.045 Uiso 1 1 calc R . . C65 C 0.6497(2) -0.3488(4) 0.45473(14) 0.0224(9) Uani 1 1 d . . . C66 C 0.6765(2) -0.4760(4) 0.47403(15) 0.0283(10) Uani 1 1 d . . . H66A H 0.6770 -0.5359 0.4505 0.042 Uiso 1 1 calc R . . H66B H 0.6490 -0.5073 0.4940 0.042 Uiso 1 1 calc R . . H66C H 0.7205 -0.4645 0.4897 0.042 Uiso 1 1 calc R . . C67 C 0.5788(2) -0.3681(4) 0.42997(15) 0.0303(11) Uani 1 1 d . . . H67A H 0.5784 -0.4348 0.4086 0.045 Uiso 1 1 calc R . . H67B H 0.5634 -0.2909 0.4152 0.045 Uiso 1 1 calc R . . H67C H 0.5507 -0.3907 0.4507 0.045 Uiso 1 1 calc R . . C68 C 0.6924(2) -0.3121(4) 0.41994(14) 0.0260(10) Uani 1 1 d . . . H68A H 0.7361 -0.2920 0.4345 0.039 Uiso 1 1 calc R . . H68B H 0.6736 -0.2396 0.4036 0.039 Uiso 1 1 calc R . . H68C H 0.6942 -0.3820 0.4001 0.039 Uiso 1 1 calc R . . O1 O 0.80145(14) 0.0841(3) 0.67322(9) 0.0269(7) Uani 1 1 d . . . O2 O 0.69272(14) 0.0029(3) 0.65722(9) 0.0256(7) Uani 1 1 d . . . O3 O 0.76666(14) -0.0306(3) 0.60446(10) 0.0306(7) Uani 1 1 d . . . S1 S 0.74408(5) 0.06981(11) 0.63504(4) 0.0247(2) Uani 1 1 d . . . Ce1 Ce 0.743384(11) 0.03919(2) 0.733652(7) 0.01708(7) Uani 1 1 d . . . Ce2 Ce 0.756555(11) -0.09700(2) 0.533437(7) 0.01747(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 C1 0.022(2) 0.013(2) 0.029(2) 0.0015(17) 0.0035(17) 0.0012(17) C2 0.023(2) 0.018(2) 0.023(2) -0.0018(17) 0.0010(17) 0.0011(17) C3 0.019(2) 0.015(2) 0.028(2) -0.0006(17) 0.0026(17) 0.0017(17) C4 0.020(2) 0.014(2) 0.026(2) 0.0043(17) 0.0017(17) 0.0023(17) C5 0.025(2) 0.014(2) 0.029(3) 0.0027(17) 0.0110(18) 0.0003(17) C6 0.020(2) 0.021(2) 0.037(3) 0.0054(19) 0.0089(18) -0.0028(18) C7 0.029(3) 0.032(3) 0.034(3) -0.001(2) 0.0028(19) -0.010(2) C8 0.030(3) 0.032(3) 0.079(4) 0.006(3) 0.012(3) 0.003(2) C9 0.039(3) 0.041(3) 0.042(3) -0.014(2) 0.020(2) -0.021(2) C10 0.021(2) 0.019(2) 0.027(2) 0.0004(17) 0.0078(17) 0.0022(17) C11 0.026(2) 0.029(3) 0.032(3) -0.004(2) 0.0084(19) 0.001(2) C12 0.039(3) 0.035(3) 0.031(3) 0.001(2) 0.012(2) 0.004(2) C13 0.028(2) 0.024(2) 0.035(3) -0.0008(19) 0.0148(19) -0.0019(19) C14 0.017(2) 0.024(2) 0.025(2) 0.0040(18) 0.0030(16) 0.0045(18) C15 0.021(2) 0.023(2) 0.042(3) 0.003(2) 0.0014(19) 0.0019(19) C16 0.025(2) 0.037(3) 0.026(3) 0.007(2) -0.0010(18) -0.001(2) C17 0.022(2) 0.024(2) 0.027(3) 0.0026(18) -0.0005(17) 0.0017(18) C18 0.020(2) 0.014(2) 0.025(2) 0.0064(16) 0.0032(16) 0.0041(16) C19 0.024(2) 0.015(2) 0.022(2) 0.0000(17) 0.0044(17) 0.0019(17) C20 0.019(2) 0.018(2) 0.021(2) 0.0026(17) -0.0035(16) 0.0010(17) C21 0.019(2) 0.014(2) 0.024(2) 0.0031(16) 0.0013(16) 0.0000(16) C22 0.026(2) 0.011(2) 0.024(2) -0.0006(16) 0.0042(17) 0.0000(17) C23 0.017(2) 0.017(2) 0.030(3) 0.0018(18) 0.0022(17) -0.0031(17) C24 0.019(2) 0.026(2) 0.035(3) 0.003(2) 0.0051(18) -0.0030(18) C25 0.024(2) 0.023(3) 0.053(3) -0.009(2) 0.001(2) -0.006(2) C26 0.023(2) 0.046(3) 0.037(3) 0.013(2) 0.007(2) -0.005(2) C27 0.022(2) 0.028(2) 0.024(2) -0.0001(19) -0.0030(17) -0.0008(19) C28 0.039(3) 0.033(3) 0.023(3) -0.005(2) -0.0040(19) -0.001(2) C29 0.031(3) 0.040(3) 0.030(3) 0.003(2) -0.004(2) 0.004(2) C30 0.024(2) 0.035(3) 0.037(3) -0.004(2) -0.0046(19) -0.004(2) C31 0.021(2) 0.021(2) 0.032(3) 0.0004(18) 0.0077(18) 0.0000(18) C32 0.030(3) 0.031(3) 0.035(3) -0.003(2) 0.016(2) 0.000(2) C33 0.021(2) 0.021(2) 0.042(3) 0.005(2) 0.0059(19) 0.0029(18) C34 0.023(2) 0.028(3) 0.047(3) 0.008(2) 0.012(2) 0.003(2) C35 0.0122(19) 0.020(2) 0.020(2) 0.0004(17) 0.0009(15) -0.0001(16) C36 0.016(2) 0.026(2) 0.019(2) -0.0028(17) 0.0032(16) -0.0046(17) C37 0.018(2) 0.022(2) 0.021(2) 0.0021(17) 0.0011(16) 0.0012(17) C38 0.017(2) 0.019(2) 0.022(2) 0.0021(17) 0.0060(16) -0.0024(17) C39 0.016(2) 0.021(2) 0.016(2) 0.0022(16) -0.0003(15) -0.0016(17) C40 0.023(2) 0.019(2) 0.020(2) 0.0007(17) 0.0022(16) -0.0023(17) C41 0.031(2) 0.020(2) 0.027(3) -0.0022(18) 0.0024(18) 0.0004(19) C42 0.030(2) 0.020(2) 0.028(3) 0.0018(18) 0.0030(18) 0.0030(19) C43 0.026(2) 0.020(2) 0.030(3) 0.0025(18) 0.0062(18) 0.0014(18) C44 0.021(2) 0.024(2) 0.021(2) 0.0052(17) 0.0037(17) -0.0032(18) C45 0.028(2) 0.036(3) 0.027(3) 0.007(2) 0.0065(19) -0.005(2) C46 0.026(2) 0.032(3) 0.021(2) 0.0078(19) 0.0008(17) -0.001(2) C47 0.037(3) 0.027(3) 0.025(3) 0.0067(19) 0.0042(19) 0.001(2) C48 0.021(2) 0.020(2) 0.026(2) 0.0008(18) 0.0035(17) -0.0061(18) C49 0.023(2) 0.026(3) 0.035(3) -0.0002(19) 0.0036(19) -0.0107(19) C50 0.025(2) 0.023(2) 0.030(3) -0.0008(19) 0.0036(18) -0.0044(19) C51 0.025(2) 0.028(3) 0.026(3) -0.0038(19) 0.0026(18) -0.0043(19) C52 0.013(2) 0.022(2) 0.022(2) 0.0017(17) -0.0010(15) -0.0020(17) C53 0.019(2) 0.021(2) 0.018(2) -0.0012(17) 0.0028(16) -0.0018(17) C54 0.016(2) 0.020(2) 0.021(2) 0.0024(17) 0.0012(16) -0.0019(17) C55 0.018(2) 0.016(2) 0.023(2) 0.0008(17) 0.0029(16) -0.0008(17) C56 0.017(2) 0.025(2) 0.015(2) 0.0027(17) 0.0010(15) -0.0019(17) C57 0.019(2) 0.022(2) 0.025(2) 0.0020(18) 0.0001(16) 0.0034(17) C58 0.036(3) 0.025(3) 0.027(3) 0.0052(19) 0.0018(19) 0.006(2) C59 0.030(3) 0.021(2) 0.043(3) 0.009(2) -0.004(2) -0.005(2) C60 0.038(3) 0.025(3) 0.039(3) 0.000(2) 0.010(2) 0.008(2) C61 0.025(2) 0.020(2) 0.024(2) 0.0041(18) 0.0041(17) -0.0056(18) C62 0.028(2) 0.032(3) 0.029(3) 0.017(2) 0.0036(19) -0.002(2) C63 0.026(2) 0.028(3) 0.032(3) 0.001(2) 0.0040(19) -0.008(2) C64 0.035(3) 0.033(3) 0.023(3) 0.005(2) 0.0073(19) -0.009(2) C65 0.022(2) 0.020(2) 0.024(2) -0.0042(17) 0.0019(17) -0.0051(18) C66 0.031(3) 0.025(3) 0.029(3) -0.0034(19) 0.0046(19) 0.000(2) C67 0.029(3) 0.031(3) 0.029(3) -0.008(2) -0.0025(19) -0.003(2) C68 0.029(2) 0.024(2) 0.025(2) -0.0069(18) 0.0043(18) -0.0034(19) O1 0.0231(16) 0.0309(18) 0.0267(17) -0.0032(13) 0.0043(12) -0.0044(13) O2 0.0270(16) 0.0267(17) 0.0235(17) -0.0012(13) 0.0055(12) -0.0041(13) O3 0.0254(17) 0.0335(19) 0.0346(19) -0.0051(14) 0.0095(13) 0.0005(14) S1 0.0236(6) 0.0278(6) 0.0234(6) 0.0003(4) 0.0059(4) 0.0009(5) Ce1 0.01593(12) 0.01570(13) 0.01951(13) 0.00006(9) 0.00266(8) 0.00069(9) Ce2 0.01647(12) 0.01705(13) 0.01852(13) 0.00053(9) 0.00184(8) -0.00164(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.397(6) . ? C1 C2 1.401(6) . ? C1 C6 1.522(6) . ? C1 Ce1 2.784(4) . ? C2 C3 1.430(6) . ? C2 Ce1 2.807(4) . ? C3 C4 1.436(6) . ? C3 C10 1.541(5) . ? C3 Ce1 2.918(4) . ? C4 C5 1.430(5) . ? C4 C14 1.553(5) . ? C4 Ce1 2.915(4) . ? C5 Ce1 2.805(4) . ? C6 C8 1.520(6) . ? C6 C9 1.532(6) . ? C6 C7 1.538(6) . ? C10 C13 1.530(6) . ? C10 C12 1.543(6) . ? C10 C11 1.553(6) . ? C14 C16 1.529(6) . ? C14 C15 1.534(6) . ? C14 C17 1.534(6) . ? C18 C19 1.408(6) . ? C18 C22 1.407(5) . ? C18 C23 1.525(5) . ? C18 Ce1 2.769(4) . ? C19 C20 1.429(5) . ? C19 Ce1 2.803(4) . ? C20 C21 1.431(6) . ? C20 C27 1.543(6) . ? C20 Ce1 2.921(4) . ? C21 C22 1.429(6) . ? C21 C31 1.556(5) . ? C21 Ce1 2.892(4) . ? C22 Ce1 2.765(4) . ? C23 C26 1.523(6) . ? C23 C25 1.524(6) . ? C23 C24 1.532(6) . ? C27 C30 1.530(6) . ? C27 C28 1.537(6) . ? C27 C29 1.554(6) . ? C31 C34 1.529(6) . ? C31 C33 1.533(6) . ? C31 C32 1.542(6) . ? C35 C36 1.399(5) . ? C35 C39 1.411(5) . ? C35 C40 1.517(6) . ? C35 Ce2 2.770(4) . ? C36 C37 1.432(6) . ? C36 Ce2 2.783(4) . ? C37 C38 1.444(6) . ? C37 C44 1.547(5) . ? C37 Ce2 2.868(4) . ? C38 C39 1.416(5) . ? C38 C48 1.544(6) . ? C38 Ce2 2.880(4) . ? C39 Ce2 2.769(4) . ? C40 C42 1.530(6) . ? C40 C41 1.534(6) . ? C40 C43 1.537(5) . ? C44 C47 1.528(6) . ? C44 C46 1.543(6) . ? C44 C45 1.552(5) . ? C48 C49 1.533(5) . ? C48 C51 1.538(6) . ? C48 C50 1.540(6) . ? C52 C56 1.406(6) . ? C52 C53 1.406(5) . ? C52 C57 1.526(6) . ? C52 Ce2 2.778(4) . ? C53 C54 1.420(6) . ? C53 Ce2 2.788(4) . ? C54 C55 1.444(6) . ? C54 C61 1.547(5) . ? C54 Ce2 2.891(4) . ? C55 C56 1.421(6) . ? C55 C65 1.546(6) . ? C55 Ce2 2.861(4) . ? C56 Ce2 2.772(4) . ? C57 C59 1.523(6) . ? C57 C58 1.524(6) . ? C57 C60 1.543(6) . ? C61 C63 1.532(6) . ? C61 C62 1.539(6) . ? C61 C64 1.547(6) . ? C65 C66 1.531(6) . ? C65 C68 1.542(5) . ? C65 C67 1.544(6) . ? O1 S1 1.527(3) . ? O1 Ce1 2.415(3) . ? O2 S1 1.524(3) . ? O2 Ce1 2.432(3) . ? O3 S1 1.537(3) . ? O3 Ce2 2.264(3) . ? S1 Ce1 3.0433(11) . ? 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 C5 C1 C2 106.1(4) . . ? C5 C1 C6 128.0(4) . . ? C2 C1 C6 125.8(4) . . ? C5 C1 Ce1 76.4(2) . . ? C2 C1 Ce1 76.4(2) . . ? C6 C1 Ce1 115.2(3) . . ? C1 C2 C3 110.3(4) . . ? C1 C2 Ce1 74.6(2) . . ? C3 C2 Ce1 79.9(2) . . ? C2 C3 C4 106.8(3) . . ? C2 C3 C10 117.4(4) . . ? C4 C3 C10 133.7(4) . . ? C2 C3 Ce1 71.3(2) . . ? C4 C3 Ce1 75.6(2) . . ? C10 C3 Ce1 130.2(3) . . ? C5 C4 C3 105.7(4) . . ? C5 C4 C14 120.2(4) . . ? C3 C4 C14 133.4(3) . . ? C5 C4 Ce1 71.3(2) . . ? C3 C4 Ce1 75.9(2) . . ? C14 C4 Ce1 124.4(3) . . ? C1 C5 C4 111.1(4) . . ? C1 C5 Ce1 74.7(2) . . ? C4 C5 Ce1 79.8(2) . . ? C8 C6 C1 108.9(4) . . ? C8 C6 C9 110.2(4) . . ? C1 C6 C9 111.5(4) . . ? C8 C6 C7 108.1(4) . . ? C1 C6 C7 109.1(3) . . ? C9 C6 C7 109.0(4) . . ? C13 C10 C3 117.0(3) . . ? C13 C10 C12 105.7(3) . . ? C3 C10 C12 110.5(3) . . ? C13 C10 C11 108.4(3) . . ? C3 C10 C11 107.7(3) . . ? C12 C10 C11 107.1(4) . . ? C16 C14 C15 105.5(3) . . ? C16 C14 C17 106.2(3) . . ? C15 C14 C17 110.0(3) . . ? C16 C14 C4 110.1(3) . . ? C15 C14 C4 110.4(3) . . ? C17 C14 C4 114.2(3) . . ? C19 C18 C22 105.9(3) . . ? C19 C18 C23 127.0(4) . . ? C22 C18 C23 127.1(4) . . ? C19 C18 Ce1 76.7(2) . . ? C22 C18 Ce1 75.1(2) . . ? C23 C18 Ce1 113.7(2) . . ? C18 C19 C20 110.5(3) . . ? C18 C19 Ce1 74.1(2) . . ? C20 C19 Ce1 80.2(2) . . ? C19 C20 C21 106.3(3) . . ? C19 C20 C27 116.1(4) . . ? C21 C20 C27 135.1(4) . . ? C19 C20 Ce1 71.0(2) . . ? C21 C20 Ce1 74.6(2) . . ? C27 C20 Ce1 132.0(3) . . ? C22 C21 C20 106.9(3) . . ? C22 C21 C31 119.7(4) . . ? C20 C21 C31 132.6(4) . . ? C22 C21 Ce1 70.5(2) . . ? C20 C21 Ce1 76.9(2) . . ? C31 C21 Ce1 125.4(3) . . ? C18 C22 C21 110.3(4) . . ? C18 C22 Ce1 75.5(2) . . ? C21 C22 Ce1 80.4(2) . . ? C26 C23 C25 109.6(4) . . ? C26 C23 C18 111.0(3) . . ? C25 C23 C18 110.3(3) . . ? C26 C23 C24 109.4(3) . . ? C25 C23 C24 108.8(4) . . ? C18 C23 C24 107.7(3) . . ? C30 C27 C28 106.6(4) . . ? C30 C27 C20 117.7(4) . . ? C28 C27 C20 110.9(3) . . ? C30 C27 C29 107.7(4) . . ? C28 C27 C29 107.5(4) . . ? C20 C27 C29 106.1(3) . . ? C34 C31 C33 111.2(3) . . ? C34 C31 C32 106.2(4) . . ? C33 C31 C32 105.4(3) . . ? C34 C31 C21 109.0(3) . . ? C33 C31 C21 114.6(3) . . ? C32 C31 C21 110.1(3) . . ? C36 C35 C39 106.2(4) . . ? C36 C35 C40 128.9(4) . . ? C39 C35 C40 124.8(4) . . ? C36 C35 Ce2 75.9(2) . . ? C39 C35 Ce2 75.2(2) . . ? C40 C35 Ce2 111.2(2) . . ? C35 C36 C37 110.4(4) . . ? C35 C36 Ce2 74.9(2) . . ? C37 C36 Ce2 78.6(2) . . ? C36 C37 C38 106.2(3) . . ? C36 C37 C44 117.7(4) . . ? C38 C37 C44 134.4(4) . . ? C36 C37 Ce2 72.1(2) . . ? C38 C37 Ce2 75.9(2) . . ? C44 C37 Ce2 127.8(2) . . ? C39 C38 C37 106.5(3) . . ? C39 C38 C48 119.5(3) . . ? C37 C38 C48 133.4(4) . . ? C39 C38 Ce2 71.2(2) . . ? C37 C38 Ce2 75.0(2) . . ? C48 C38 Ce2 125.0(2) . . ? C35 C39 C38 110.6(3) . . ? C35 C39 Ce2 75.3(2) . . ? C38 C39 Ce2 79.9(2) . . ? C35 C40 C42 111.1(3) . . ? C35 C40 C41 111.2(3) . . ? C42 C40 C41 108.2(3) . . ? C35 C40 C43 107.9(3) . . ? C42 C40 C43 108.6(3) . . ? C41 C40 C43 109.7(3) . . ? C47 C44 C46 105.9(3) . . ? C47 C44 C37 117.6(3) . . ? C46 C44 C37 109.8(3) . . ? C47 C44 C45 108.5(3) . . ? C46 C44 C45 107.5(3) . . ? C37 C44 C45 107.2(3) . . ? C49 C48 C51 106.5(3) . . ? C49 C48 C50 110.3(3) . . ? C51 C48 C50 105.2(3) . . ? C49 C48 C38 109.3(3) . . ? C51 C48 C38 110.7(3) . . ? C50 C48 C38 114.6(3) . . ? C56 C52 C53 106.1(4) . . ? C56 C52 C57 127.7(4) . . ? C53 C52 C57 126.1(4) . . ? C56 C52 Ce2 75.1(2) . . ? C53 C52 Ce2 75.7(2) . . ? C57 C52 Ce2 112.8(2) . . ? C52 C53 C54 110.5(4) . . ? C52 C53 Ce2 75.0(2) . . ? C54 C53 Ce2 79.6(2) . . ? C53 C54 C55 106.4(3) . . ? C53 C54 C61 120.0(3) . . ? C55 C54 C61 133.0(4) . . ? C53 C54 Ce2 71.5(2) . . ? C55 C54 Ce2 74.3(2) . . ? C61 C54 Ce2 125.3(3) . . ? C56 C55 C54 106.4(3) . . ? C56 C55 C65 117.5(3) . . ? C54 C55 C65 134.3(4) . . ? C56 C55 Ce2 71.9(2) . . ? C54 C55 Ce2 76.6(2) . . ? C65 C55 Ce2 127.4(2) . . ? C52 C56 C55 110.4(3) . . ? C52 C56 Ce2 75.6(2) . . ? C55 C56 Ce2 78.9(2) . . ? C59 C57 C58 109.7(4) . . ? C59 C57 C52 108.4(3) . . ? C58 C57 C52 110.9(3) . . ? C59 C57 C60 109.4(4) . . ? C58 C57 C60 108.8(3) . . ? C52 C57 C60 109.7(3) . . ? C63 C61 C62 110.6(4) . . ? C63 C61 C54 110.8(3) . . ? C62 C61 C54 113.9(3) . . ? C63 C61 C64 105.9(3) . . ? C62 C61 C64 105.9(3) . . ? C54 C61 C64 109.5(3) . . ? C66 C65 C68 106.0(3) . . ? C66 C65 C67 109.1(3) . . ? C68 C65 C67 107.2(3) . . ? C66 C65 C55 116.7(3) . . ? C68 C65 C55 110.4(3) . . ? C67 C65 C55 107.2(3) . . ? S1 O1 Ce1 98.56(14) . . ? S1 O2 Ce1 97.94(14) . . ? S1 O3 Ce2 144.20(19) . . ? O2 S1 O1 102.19(16) . . ? O2 S1 O3 104.93(17) . . ? O1 S1 O3 105.10(17) . . ? O2 S1 Ce1 52.33(11) . . ? O1 S1 Ce1 51.69(11) . . ? O3 S1 Ce1 125.83(13) . . ? O1 Ce1 O2 58.65(9) . . ? O1 Ce1 C22 89.77(11) . . ? O2 Ce1 C22 84.11(11) . . ? O1 Ce1 C18 118.92(11) . . ? O2 Ce1 C18 96.08(11) . . ? C22 Ce1 C18 29.46(11) . . ? O1 Ce1 C1 84.77(11) . . ? O2 Ce1 C1 109.63(11) . . ? C22 Ce1 C1 159.26(12) . . ? C18 Ce1 C1 152.10(12) . . ? O1 Ce1 C19 129.44(11) . . ? O2 Ce1 C19 125.31(11) . . ? C22 Ce1 C19 47.60(12) . . ? C18 Ce1 C19 29.26(11) . . ? C1 Ce1 C19 124.35(12) . . ? O1 Ce1 C5 78.23(11) . . ? O2 Ce1 C5 82.45(11) . . ? C22 Ce1 C5 165.33(12) . . ? C18 Ce1 C5 159.01(11) . . ? C1 Ce1 C5 28.94(12) . . ? C19 Ce1 C5 147.00(12) . . ? O1 Ce1 C2 113.65(11) . . ? O2 Ce1 C2 126.69(11) . . ? C22 Ce1 C2 147.63(12) . . ? C18 Ce1 C2 124.48(12) . . ? C1 Ce1 C2 29.03(11) . . ? C19 Ce1 C2 100.51(12) . . ? C5 Ce1 C2 46.96(12) . . ? O1 Ce1 C21 82.07(10) . . ? O2 Ce1 C21 103.73(11) . . ? C22 Ce1 C21 29.14(11) . . ? C18 Ce1 C21 48.47(11) . . ? C1 Ce1 C21 130.12(12) . . ? C19 Ce1 C21 47.37(11) . . ? C5 Ce1 C21 152.22(11) . . ? C2 Ce1 C21 128.57(12) . . ? O1 Ce1 C4 101.75(11) . . ? O2 Ce1 C4 80.76(11) . . ? C22 Ce1 C4 152.31(12) . . ? C18 Ce1 C4 130.15(11) . . ? C1 Ce1 C4 48.23(11) . . ? C19 Ce1 C4 128.71(11) . . ? C5 Ce1 C4 28.87(11) . . ? C2 Ce1 C4 47.37(12) . . ? C21 Ce1 C4 175.27(11) . . ? O1 Ce1 C3 125.21(11) . . ? O2 Ce1 C3 106.91(11) . . ? C22 Ce1 C3 144.32(11) . . ? C18 Ce1 C3 114.88(11) . . ? C1 Ce1 C3 48.02(11) . . ? C19 Ce1 C3 102.81(11) . . ? C5 Ce1 C3 46.99(11) . . ? C2 Ce1 C3 28.85(11) . . ? C21 Ce1 C3 146.78(11) . . ? C4 Ce1 C3 28.50(11) . . ? O1 Ce1 C20 104.69(11) . . ? O2 Ce1 C20 130.59(11) . . ? C22 Ce1 C20 47.54(12) . . ? C18 Ce1 C20 48.29(11) . . ? C1 Ce1 C20 114.81(12) . . ? C19 Ce1 C20 28.83(11) . . ? C5 Ce1 C20 143.75(12) . . ? C2 Ce1 C20 102.72(12) . . ? C21 Ce1 C20 28.49(11) . . ? C4 Ce1 C20 146.78(11) . . ? C3 Ce1 C20 118.38(11) . . ? O3 Ce2 C39 82.69(11) . . ? O3 Ce2 C35 107.64(11) . . ? C39 Ce2 C35 29.50(11) . . ? O3 Ce2 C56 128.17(11) . . ? C39 Ce2 C56 147.86(11) . . ? C35 Ce2 C56 123.91(11) . . ? O3 Ce2 C52 100.18(11) . . ? C39 Ce2 C52 160.22(12) . . ? C35 Ce2 C52 151.92(11) . . ? C56 Ce2 C52 29.36(11) . . ? O3 Ce2 C36 130.14(11) . . ? C39 Ce2 C36 47.74(12) . . ? C35 Ce2 C36 29.19(11) . . ? C56 Ce2 C36 100.41(12) . . ? C52 Ce2 C36 124.45(12) . . ? O3 Ce2 C53 82.08(11) . . ? C39 Ce2 C53 164.42(12) . . ? C35 Ce2 C53 158.90(12) . . ? C56 Ce2 C53 47.71(11) . . ? C52 Ce2 C53 29.27(11) . . ? C36 Ce2 C53 147.71(12) . . ? O3 Ce2 C55 124.76(11) . . ? C39 Ce2 C55 143.42(11) . . ? C35 Ce2 C55 114.00(11) . . ? C56 Ce2 C55 29.16(11) . . ? C52 Ce2 C55 48.61(12) . . ? C36 Ce2 C55 102.70(11) . . ? C53 Ce2 C55 47.90(11) . . ? O3 Ce2 C37 115.44(11) . . ? C39 Ce2 C37 47.96(11) . . ? C35 Ce2 C37 48.67(11) . . ? C56 Ce2 C37 103.19(11) . . ? C52 Ce2 C37 115.04(11) . . ? C36 Ce2 C37 29.30(12) . . ? C53 Ce2 C37 144.25(11) . . ? C55 Ce2 C37 119.11(11) . . ? O3 Ce2 C38 87.21(11) . . ? C39 Ce2 C38 28.96(11) . . ? C35 Ce2 C38 48.53(11) . . ? C56 Ce2 C38 130.04(11) . . ? C52 Ce2 C38 131.27(12) . . ? C36 Ce2 C38 47.88(11) . . ? C53 Ce2 C38 152.47(12) . . ? C55 Ce2 C38 147.96(11) . . ? C37 Ce2 C38 29.10(11) . . ? O3 Ce2 C54 95.77(11) . . ? C39 Ce2 C54 151.35(11) . . ? C35 Ce2 C54 130.01(12) . . ? C56 Ce2 C54 47.75(11) . . ? C52 Ce2 C54 48.30(11) . . ? C36 Ce2 C54 129.35(12) . . ? C53 Ce2 C54 28.89(11) . . ? C55 Ce2 C54 29.07(11) . . ? C37 Ce2 C54 148.01(11) . . ? C38 Ce2 C54 177.02(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.618 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.109 # Attachment 'ceotf-rev.cif' data_shelxla _database_code_depnum_ccdc_archive 'CCDC 901437' #TrackingRef 'ceotf-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ceotf _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H58 Ce F3 O3 S' _chemical_formula_weight 755.99 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' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5673(12) _cell_length_b 21.532(2) _cell_length_c 16.3041(18) _cell_angle_alpha 90.00 _cell_angle_beta 98.267(2) _cell_angle_gamma 90.00 _cell_volume 3671.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9738 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 1.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8139 _exptl_absorpt_correction_T_max 0.9238 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 46441 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.36 _reflns_number_total 6719 _reflns_number_gt 6134 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0192P)^2^+3.7609P] 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 6719 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0522 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.04988(19) 0.06145(9) 0.63894(12) 0.0166(4) Uani 1 1 d . . . C2 C -0.0688(2) 0.09218(9) 0.63035(13) 0.0191(4) Uani 1 1 d . . . H2 H -0.0915 0.1261 0.5940 0.023 Uiso 1 1 calc R . . C3 C -0.15008(19) 0.06582(10) 0.68313(13) 0.0204(4) Uani 1 1 d . . . C4 C -0.07539(19) 0.01818(9) 0.73057(12) 0.0185(4) Uani 1 1 d . . . C5 C 0.04588(19) 0.01729(9) 0.70209(12) 0.0161(4) Uani 1 1 d . . . H5 H 0.1146 -0.0094 0.7229 0.019 Uiso 1 1 calc R . . C6 C 0.1580(2) 0.07323(9) 0.58858(12) 0.0184(4) Uani 1 1 d . . . C7 C 0.1048(2) 0.08881(14) 0.49899(14) 0.0373(6) Uani 1 1 d . . . H7A H 0.0508 0.0546 0.4748 0.056 Uiso 1 1 calc R . . H7B H 0.1756 0.0950 0.4671 0.056 Uiso 1 1 calc R . . H7C H 0.0537 0.1269 0.4975 0.056 Uiso 1 1 calc R . . C8 C 0.2428(2) 0.01548(12) 0.58854(17) 0.0358(6) Uani 1 1 d . . . H8A H 0.2811 0.0058 0.6455 0.054 Uiso 1 1 calc R . . H8B H 0.3107 0.0235 0.5548 0.054 Uiso 1 1 calc R . . H8C H 0.1909 -0.0198 0.5653 0.054 Uiso 1 1 calc R . . C9 C 0.2410(3) 0.12707(11) 0.62625(16) 0.0338(6) Uani 1 1 d . . . H9A H 0.1874 0.1638 0.6300 0.051 Uiso 1 1 calc R . . H9B H 0.3065 0.1364 0.5911 0.051 Uiso 1 1 calc R . . H9C H 0.2825 0.1155 0.6818 0.051 Uiso 1 1 calc R . . C10 C -0.2950(2) 0.08115(10) 0.67080(14) 0.0252(5) Uani 1 1 d . . . C11 C -0.3739(2) 0.02204(11) 0.64588(16) 0.0306(5) Uani 1 1 d . . . H11A H -0.3667 -0.0065 0.6931 0.046 Uiso 1 1 calc R . . H11B H -0.3412 0.0018 0.5993 0.046 Uiso 1 1 calc R . . H11C H -0.4638 0.0333 0.6294 0.046 Uiso 1 1 calc R . . C12 C -0.3271(2) 0.12662(12) 0.59763(17) 0.0355(6) Uani 1 1 d . . . H12A H -0.4193 0.1348 0.5886 0.053 Uiso 1 1 calc R . . H12B H -0.3017 0.1083 0.5475 0.053 Uiso 1 1 calc R . . H12C H -0.2808 0.1657 0.6103 0.053 Uiso 1 1 calc R . . C13 C -0.3420(2) 0.11147(12) 0.74580(16) 0.0335(6) Uani 1 1 d . . . H13A H -0.4342 0.1192 0.7333 0.050 Uiso 1 1 calc R . . H13B H -0.2972 0.1509 0.7583 0.050 Uiso 1 1 calc R . . H13C H -0.3249 0.0837 0.7938 0.050 Uiso 1 1 calc R . . C14 C -0.1086(2) -0.03572(10) 0.78681(13) 0.0221(5) Uani 1 1 d . . . C15 C -0.1522(2) -0.09163(10) 0.73040(14) 0.0246(5) Uani 1 1 d . . . H15A H -0.1675 -0.1275 0.7647 0.037 Uiso 1 1 calc R . . H15B H -0.0855 -0.1019 0.6967 0.037 Uiso 1 1 calc R . . H15C H -0.2313 -0.0810 0.6940 0.037 Uiso 1 1 calc R . . C16 C 0.0108(2) -0.05756(11) 0.84509(15) 0.0302(5) Uani 1 1 d . . . H16A H 0.0446 -0.0231 0.8809 0.045 Uiso 1 1 calc R . . H16B H 0.0760 -0.0715 0.8121 0.045 Uiso 1 1 calc R . . H16C H -0.0124 -0.0920 0.8793 0.045 Uiso 1 1 calc R . . C17 C -0.2094(2) -0.02162(11) 0.84291(14) 0.0289(5) Uani 1 1 d . . . H17A H -0.2902 -0.0105 0.8087 0.043 Uiso 1 1 calc R . . H17B H -0.1803 0.0130 0.8798 0.043 Uiso 1 1 calc R . . H17C H -0.2223 -0.0584 0.8761 0.043 Uiso 1 1 calc R . . C18 C -0.0159(2) 0.22232(9) 0.88235(13) 0.0194(4) Uani 1 1 d . . . C19 C -0.0609(2) 0.24063(9) 0.80089(13) 0.0191(4) Uani 1 1 d . . . H19 H -0.1478 0.2389 0.7760 0.023 Uiso 1 1 calc R . . C20 C 0.0422(2) 0.26228(9) 0.76040(13) 0.0178(4) Uani 1 1 d . . . C21 C 0.1569(2) 0.25510(9) 0.81955(12) 0.0174(4) Uani 1 1 d . . . C22 C 0.1177(2) 0.22900(9) 0.89208(13) 0.0192(4) Uani 1 1 d . . . H22 H 0.1742 0.2176 0.9404 0.023 Uiso 1 1 calc R . . C23 C -0.0966(2) 0.20119(10) 0.94774(13) 0.0244(5) Uani 1 1 d . . . C24 C -0.1165(2) 0.13089(10) 0.94252(14) 0.0255(5) Uani 1 1 d . . . H24A H -0.1530 0.1195 0.8858 0.038 Uiso 1 1 calc R . . H24B H -0.1751 0.1183 0.9809 0.038 Uiso 1 1 calc R . . H24C H -0.0342 0.1099 0.9575 0.038 Uiso 1 1 calc R . . C25 C -0.2280(3) 0.23310(13) 0.93212(17) 0.0414(7) Uani 1 1 d . . . H25A H -0.2164 0.2783 0.9336 0.062 Uiso 1 1 calc R . . H25B H -0.2788 0.2206 0.9751 0.062 Uiso 1 1 calc R . . H25C H -0.2725 0.2208 0.8776 0.062 Uiso 1 1 calc R . . C26 C -0.0293(3) 0.21758(12) 1.03413(15) 0.0408(7) Uani 1 1 d . . . H26A H 0.0539 0.1967 1.0440 0.061 Uiso 1 1 calc R . . H26B H -0.0818 0.2040 1.0756 0.061 Uiso 1 1 calc R . . H26C H -0.0166 0.2626 1.0383 0.061 Uiso 1 1 calc R . . C27 C 0.0079(2) 0.30094(9) 0.68070(13) 0.0202(4) Uani 1 1 d . . . C28 C -0.1124(2) 0.27473(11) 0.62753(14) 0.0279(5) Uani 1 1 d . . . H28A H -0.1840 0.2753 0.6596 0.042 Uiso 1 1 calc R . . H28B H -0.0961 0.2319 0.6114 0.042 Uiso 1 1 calc R . . H28C H -0.1336 0.3002 0.5777 0.042 Uiso 1 1 calc R . . C29 C 0.1095(2) 0.30536(11) 0.62262(14) 0.0281(5) Uani 1 1 d . . . H29A H 0.0758 0.3297 0.5735 0.042 Uiso 1 1 calc R . . H29B H 0.1316 0.2635 0.6057 0.042 Uiso 1 1 calc R . . H29C H 0.1861 0.3257 0.6516 0.042 Uiso 1 1 calc R . . C30 C -0.0255(2) 0.36692(10) 0.70684(14) 0.0247(5) Uani 1 1 d . . . H30A H 0.0497 0.3857 0.7397 0.037 Uiso 1 1 calc R . . H30B H -0.0956 0.3649 0.7401 0.037 Uiso 1 1 calc R . . H30C H -0.0518 0.3922 0.6573 0.037 Uiso 1 1 calc R . . C31 C 0.2946(2) 0.27981(9) 0.82131(13) 0.0206(4) Uani 1 1 d . . . C32 C 0.3668(2) 0.25303(10) 0.75418(14) 0.0241(5) Uani 1 1 d . . . H32A H 0.3143 0.2575 0.6998 0.036 Uiso 1 1 calc R . . H32B H 0.3848 0.2090 0.7655 0.036 Uiso 1 1 calc R . . H32C H 0.4474 0.2755 0.7543 0.036 Uiso 1 1 calc R . . C33 C 0.3768(2) 0.26470(10) 0.90477(14) 0.0271(5) Uani 1 1 d . . . H33A H 0.3778 0.2197 0.9138 0.041 Uiso 1 1 calc R . . H33B H 0.3407 0.2853 0.9497 0.041 Uiso 1 1 calc R . . H33C H 0.4644 0.2795 0.9040 0.041 Uiso 1 1 calc R . . C34 C 0.2902(2) 0.35119(10) 0.81679(16) 0.0282(5) Uani 1 1 d . . . H34A H 0.3772 0.3678 0.8285 0.042 Uiso 1 1 calc R . . H34B H 0.2390 0.3671 0.8578 0.042 Uiso 1 1 calc R . . H34C H 0.2514 0.3641 0.7612 0.042 Uiso 1 1 calc R . . C35 C 0.3643(2) 0.00400(10) 0.89418(14) 0.0237(5) Uani 1 1 d . . . O1 O 0.30552(14) 0.11242(7) 0.82937(9) 0.0224(3) Uani 1 1 d . . . O2 O 0.16243(14) 0.07071(7) 0.91418(9) 0.0232(3) Uani 1 1 d . . . O3 O 0.37408(16) 0.10518(7) 0.97988(10) 0.0309(4) Uani 1 1 d . . . F1 F 0.31216(13) -0.02058(6) 0.82231(8) 0.0307(3) Uani 1 1 d . . . F2 F 0.48905(12) 0.00850(6) 0.89420(9) 0.0350(3) Uani 1 1 d . . . F3 F 0.34193(14) -0.03364(6) 0.95432(9) 0.0368(3) Uani 1 1 d . . . S1 S 0.29760(5) 0.08117(2) 0.90809(3) 0.02003(11) Uani 1 1 d . . . Ce1 Ce 0.062624(11) 0.130577(5) 0.782890(7) 0.01569(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0177(10) 0.0167(10) 0.0149(10) -0.0019(8) 0.0007(8) -0.0019(8) C2 0.0187(11) 0.0195(10) 0.0179(10) 0.0016(8) -0.0011(8) -0.0013(8) C3 0.0128(10) 0.0244(11) 0.0239(11) -0.0045(9) 0.0018(8) -0.0032(8) C4 0.0182(11) 0.0181(10) 0.0183(10) 0.0007(8) 0.0000(8) -0.0043(8) C5 0.0152(10) 0.0151(9) 0.0176(10) -0.0012(8) 0.0009(8) -0.0009(8) C6 0.0176(11) 0.0198(10) 0.0182(10) 0.0002(8) 0.0040(8) -0.0017(8) C7 0.0261(13) 0.0662(18) 0.0199(12) 0.0092(12) 0.0048(10) -0.0039(12) C8 0.0296(14) 0.0351(14) 0.0475(16) 0.0055(12) 0.0219(12) 0.0059(11) C9 0.0348(14) 0.0367(14) 0.0334(14) -0.0110(11) 0.0163(11) -0.0170(11) C10 0.0143(11) 0.0291(12) 0.0312(13) -0.0002(10) -0.0002(9) 0.0009(9) C11 0.0158(11) 0.0374(13) 0.0374(14) -0.0058(11) 0.0000(10) -0.0030(10) C12 0.0192(12) 0.0400(14) 0.0455(16) 0.0087(12) -0.0017(11) 0.0046(10) C13 0.0201(12) 0.0351(13) 0.0450(15) -0.0074(11) 0.0039(11) 0.0027(10) C14 0.0220(11) 0.0219(11) 0.0227(11) 0.0032(9) 0.0043(9) -0.0053(9) C15 0.0229(12) 0.0237(11) 0.0282(12) 0.0014(9) 0.0069(9) -0.0041(9) C16 0.0327(13) 0.0287(12) 0.0277(12) 0.0105(10) -0.0009(10) -0.0092(10) C17 0.0354(14) 0.0271(12) 0.0263(12) -0.0009(9) 0.0118(10) -0.0094(10) C18 0.0267(12) 0.0138(9) 0.0198(11) -0.0018(8) 0.0099(9) 0.0010(8) C19 0.0208(11) 0.0170(10) 0.0206(11) 0.0013(8) 0.0068(8) 0.0032(8) C20 0.0213(11) 0.0142(9) 0.0189(10) 0.0014(8) 0.0065(8) 0.0031(8) C21 0.0210(11) 0.0135(9) 0.0188(10) -0.0011(8) 0.0064(8) 0.0006(8) C22 0.0276(12) 0.0154(10) 0.0149(10) -0.0010(8) 0.0040(9) 0.0013(9) C23 0.0335(13) 0.0209(11) 0.0222(11) 0.0012(9) 0.0156(10) 0.0019(9) C24 0.0295(13) 0.0242(11) 0.0238(12) 0.0020(9) 0.0080(10) -0.0054(9) C25 0.0453(16) 0.0424(15) 0.0440(16) 0.0116(12) 0.0318(13) 0.0130(13) C26 0.067(2) 0.0371(14) 0.0219(13) -0.0070(10) 0.0200(13) -0.0178(14) C27 0.0214(11) 0.0193(10) 0.0209(11) 0.0066(8) 0.0057(9) 0.0050(9) C28 0.0329(13) 0.0264(12) 0.0228(12) 0.0084(9) -0.0011(10) -0.0006(10) C29 0.0311(13) 0.0335(13) 0.0222(12) 0.0107(10) 0.0118(10) 0.0092(10) C30 0.0240(12) 0.0193(11) 0.0324(13) 0.0072(9) 0.0095(10) 0.0041(9) C31 0.0212(11) 0.0164(10) 0.0244(11) 0.0002(8) 0.0039(9) -0.0009(8) C32 0.0186(11) 0.0246(11) 0.0293(12) 0.0022(9) 0.0049(9) -0.0013(9) C33 0.0257(12) 0.0230(11) 0.0308(13) -0.0021(9) -0.0016(10) -0.0036(9) C34 0.0251(12) 0.0201(11) 0.0394(14) -0.0002(10) 0.0048(10) -0.0030(9) C35 0.0231(12) 0.0198(11) 0.0252(12) -0.0024(9) -0.0063(9) 0.0041(9) O1 0.0201(8) 0.0210(7) 0.0255(8) 0.0029(6) 0.0012(6) 0.0013(6) O2 0.0245(8) 0.0241(8) 0.0216(8) 0.0032(6) 0.0052(6) 0.0032(6) O3 0.0371(10) 0.0236(8) 0.0277(9) -0.0067(7) -0.0099(7) 0.0037(7) F1 0.0301(7) 0.0274(7) 0.0305(7) -0.0120(6) -0.0093(6) 0.0075(6) F2 0.0206(7) 0.0317(7) 0.0497(9) -0.0091(6) -0.0050(6) 0.0056(6) F3 0.0484(9) 0.0229(7) 0.0365(8) 0.0084(6) -0.0028(7) 0.0058(6) S1 0.0230(3) 0.0164(2) 0.0192(3) -0.00124(19) -0.0021(2) 0.0027(2) Ce1 0.01630(7) 0.01457(6) 0.01599(7) 0.00045(4) 0.00162(5) 0.00091(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.407(3) . ? C1 C2 1.407(3) . ? C1 C6 1.521(3) . ? C1 Ce1 2.7661(19) . ? C2 C3 1.419(3) . ? C2 Ce1 2.794(2) . ? C2 H2 0.9500 . ? C3 C4 1.448(3) . ? C3 C10 1.551(3) . ? C3 Ce1 2.931(2) . ? C4 C5 1.425(3) . ? C4 C14 1.550(3) . ? C4 Ce1 2.890(2) . ? C5 Ce1 2.7658(19) . ? C5 H5 0.9500 . ? C6 C7 1.525(3) . ? C6 C9 1.528(3) . ? C6 C8 1.533(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C13 1.531(3) . ? C10 C12 1.543(3) . ? C10 C11 1.544(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C17 1.531(3) . ? C14 C16 1.540(3) . ? C14 C15 1.545(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.401(3) . ? C18 C22 1.406(3) . ? C18 C23 1.527(3) . ? C18 Ce1 2.758(2) . ? C19 C20 1.431(3) . ? C19 Ce1 2.741(2) . ? C19 H19 0.9500 . ? C20 C21 1.444(3) . ? C20 C27 1.542(3) . ? C20 Ce1 2.864(2) . ? C21 C22 1.423(3) . ? C21 C31 1.546(3) . ? C21 Ce1 2.893(2) . ? C22 Ce1 2.775(2) . ? C22 H22 0.9500 . ? C23 C26 1.525(3) . ? C23 C24 1.529(3) . ? C23 C25 1.537(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.533(3) . ? C27 C30 1.539(3) . ? C27 C28 1.539(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.534(3) . ? C31 C34 1.539(3) . ? C31 C33 1.540(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 F3 1.320(3) . ? C35 F2 1.321(3) . ? C35 F1 1.331(2) . ? C35 S1 1.832(2) . ? O1 S1 1.4622(16) . ? O1 Ce1 2.5992(15) . ? O2 S1 1.4635(16) . ? O2 Ce1 2.5899(14) . ? O3 S1 1.4207(16) . ? S1 Ce1 3.1633(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 105.70(18) . . ? C5 C1 C6 127.72(18) . . ? C2 C1 C6 126.57(18) . . ? C5 C1 Ce1 75.26(11) . . ? C2 C1 Ce1 76.43(12) . . ? C6 C1 Ce1 114.80(12) . . ? C1 C2 C3 111.11(18) . . ? C1 C2 Ce1 74.26(11) . . ? C3 C2 Ce1 81.09(12) . . ? C1 C2 H2 124.4 . . ? C3 C2 H2 124.4 . . ? Ce1 C2 H2 112.1 . . ? C2 C3 C4 106.04(18) . . ? C2 C3 C10 120.58(19) . . ? C4 C3 C10 132.22(19) . . ? C2 C3 Ce1 70.33(11) . . ? C4 C3 Ce1 74.04(11) . . ? C10 C3 Ce1 129.40(14) . . ? C5 C4 C3 106.39(18) . . ? C5 C4 C14 118.26(18) . . ? C3 C4 C14 133.93(19) . . ? C5 C4 Ce1 70.61(11) . . ? C3 C4 Ce1 77.16(11) . . ? C14 C4 Ce1 126.86(13) . . ? C1 C5 C4 110.65(18) . . ? C1 C5 Ce1 75.28(11) . . ? C4 C5 Ce1 80.32(12) . . ? C1 C5 H5 124.7 . . ? C4 C5 H5 124.7 . . ? Ce1 C5 H5 111.8 . . ? C1 C6 C7 110.57(17) . . ? C1 C6 C9 110.00(17) . . ? C7 C6 C9 109.23(19) . . ? C1 C6 C8 110.47(17) . . ? C7 C6 C8 108.3(2) . . ? C9 C6 C8 108.27(19) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C13 C10 C12 106.6(2) . . ? C13 C10 C11 109.68(19) . . ? C12 C10 C11 105.61(19) . . ? C13 C10 C3 114.54(18) . . ? C12 C10 C3 109.81(19) . . ? C11 C10 C3 110.15(18) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C17 C14 C16 105.70(19) . . ? C17 C14 C15 109.66(18) . . ? C16 C14 C15 106.10(18) . . ? C17 C14 C4 116.17(18) . . ? C16 C14 C4 111.02(17) . . ? C15 C14 C4 107.75(17) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C22 106.06(18) . . ? C19 C18 C23 126.7(2) . . ? C22 C18 C23 127.18(19) . . ? C19 C18 Ce1 74.57(11) . . ? C22 C18 Ce1 75.95(12) . . ? C23 C18 Ce1 116.26(13) . . ? C18 C19 C20 110.60(19) . . ? C18 C19 Ce1 75.90(12) . . ? C20 C19 Ce1 80.00(12) . . ? C18 C19 H19 124.7 . . ? C20 C19 H19 124.7 . . ? Ce1 C19 H19 111.5 . . ? C19 C20 C21 106.17(18) . . ? C19 C20 C27 117.54(18) . . ? C21 C20 C27 133.91(19) . . ? C19 C20 Ce1 70.52(11) . . ? C21 C20 Ce1 76.58(11) . . ? C27 C20 Ce1 130.30(13) . . ? C22 C21 C20 106.31(18) . . ? C22 C21 C31 120.38(18) . . ? C20 C21 C31 132.28(18) . . ? C22 C21 Ce1 70.92(11) . . ? C20 C21 Ce1 74.36(11) . . ? C31 C21 Ce1 128.17(13) . . ? C18 C22 C21 110.73(18) . . ? C18 C22 Ce1 74.62(11) . . ? C21 C22 Ce1 80.08(11) . . ? C18 C22 H22 124.6 . . ? C21 C22 H22 124.6 . . ? Ce1 C22 H22 112.6 . . ? C26 C23 C18 110.05(19) . . ? C26 C23 C24 108.83(19) . . ? C18 C23 C24 110.02(17) . . ? C26 C23 C25 109.9(2) . . ? C18 C23 C25 109.43(18) . . ? C24 C23 C25 108.6(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C30 108.81(18) . . ? C29 C27 C28 105.66(18) . . ? C30 C27 C28 106.92(18) . . ? C29 C27 C20 116.96(17) . . ? C30 C27 C20 107.48(17) . . ? C28 C27 C20 110.60(17) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C34 110.88(18) . . ? C32 C31 C33 106.01(18) . . ? C34 C31 C33 105.24(18) . . ? C32 C31 C21 114.89(17) . . ? C34 C31 C21 108.68(17) . . ? C33 C31 C21 110.70(18) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? F3 C35 F2 109.29(17) . . ? F3 C35 F1 108.29(18) . . ? F2 C35 F1 108.43(19) . . ? F3 C35 S1 110.60(16) . . ? F2 C35 S1 109.59(15) . . ? F1 C35 S1 110.59(14) . . ? S1 O1 Ce1 98.42(7) . . ? S1 O2 Ce1 98.78(7) . . ? O3 S1 O1 117.27(10) . . ? O3 S1 O2 116.44(10) . . ? O1 S1 O2 108.06(9) . . ? O3 S1 C35 104.39(9) . . ? O1 S1 C35 103.71(10) . . ? O2 S1 C35 105.40(10) . . ? O3 S1 Ce1 135.24(7) . . ? O1 S1 Ce1 54.37(6) . . ? O2 S1 Ce1 54.01(6) . . ? C35 S1 Ce1 120.37(7) . . ? O2 Ce1 O1 54.30(5) . . ? O2 Ce1 C19 119.04(5) . . ? O1 Ce1 C19 124.35(6) . . ? O2 Ce1 C18 89.53(5) . . ? O1 Ce1 C18 107.72(6) . . ? C19 Ce1 C18 29.52(6) . . ? O2 Ce1 C5 86.86(5) . . ? O1 Ce1 C5 89.95(5) . . ? C19 Ce1 C5 144.54(6) . . ? C18 Ce1 C5 155.18(6) . . ? O2 Ce1 C1 113.44(5) . . ? O1 Ce1 C1 95.28(5) . . ? C19 Ce1 C1 126.16(6) . . ? C18 Ce1 C1 154.45(6) . . ? C5 Ce1 C1 29.46(6) . . ? O2 Ce1 C22 80.03(5) . . ? O1 Ce1 C22 79.66(6) . . ? C19 Ce1 C22 47.97(6) . . ? C18 Ce1 C22 29.43(6) . . ? C5 Ce1 C22 166.45(6) . . ? C1 Ce1 C22 159.29(6) . . ? O2 Ce1 C2 132.83(5) . . ? O1 Ce1 C2 123.96(5) . . ? C19 Ce1 C2 99.65(6) . . ? C18 Ce1 C2 125.61(6) . . ? C5 Ce1 C2 47.58(6) . . ? C1 Ce1 C2 29.31(6) . . ? C22 Ce1 C2 145.97(6) . . ? O2 Ce1 C20 127.81(5) . . ? O1 Ce1 C20 103.85(5) . . ? C19 Ce1 C20 29.47(6) . . ? C18 Ce1 C20 48.89(6) . . ? C5 Ce1 C20 144.48(6) . . ? C1 Ce1 C20 115.51(6) . . ? C22 Ce1 C20 48.00(6) . . ? C2 Ce1 C20 99.23(6) . . ? O2 Ce1 C4 87.44(5) . . ? O1 Ce1 C4 113.28(5) . . ? C19 Ce1 C4 121.84(6) . . ? C18 Ce1 C4 126.26(6) . . ? C5 Ce1 C4 29.07(6) . . ? C1 Ce1 C4 48.55(6) . . ? C22 Ce1 C4 151.54(6) . . ? C2 Ce1 C4 47.49(6) . . ? C20 Ce1 C4 139.99(6) . . ? O2 Ce1 C21 101.74(5) . . ? O1 Ce1 C21 77.46(5) . . ? C19 Ce1 C21 48.07(6) . . ? C18 Ce1 C21 48.58(6) . . ? C5 Ce1 C21 155.85(6) . . ? C1 Ce1 C21 130.35(6) . . ? C22 Ce1 C21 28.99(6) . . ? C2 Ce1 C21 124.79(6) . . ? C20 Ce1 C21 29.06(6) . . ? C4 Ce1 C21 168.89(6) . . ? O2 Ce1 C3 114.24(6) . . ? O1 Ce1 C3 137.44(5) . . ? C19 Ce1 C3 97.57(6) . . ? C18 Ce1 C3 113.29(6) . . ? C5 Ce1 C3 47.52(6) . . ? C1 Ce1 C3 48.18(6) . . ? C22 Ce1 C3 142.44(6) . . ? C2 Ce1 C3 28.57(6) . . ? C20 Ce1 C3 111.25(6) . . ? C4 Ce1 C3 28.80(6) . . ? C21 Ce1 C3 140.31(6) . . ? 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 C5 C1 C2 C3 -3.5(2) . . . . ? C6 C1 C2 C3 175.34(18) . . . . ? Ce1 C1 C2 C3 -73.67(15) . . . . ? C5 C1 C2 Ce1 70.13(13) . . . . ? C6 C1 C2 Ce1 -111.00(19) . . . . ? C1 C2 C3 C4 3.2(2) . . . . ? Ce1 C2 C3 C4 -66.01(14) . . . . ? C1 C2 C3 C10 -165.91(18) . . . . ? Ce1 C2 C3 C10 124.87(18) . . . . ? C1 C2 C3 Ce1 69.22(15) . . . . ? C2 C3 C4 C5 -1.6(2) . . . . ? C10 C3 C4 C5 165.8(2) . . . . ? Ce1 C3 C4 C5 -65.04(13) . . . . ? C2 C3 C4 C14 -167.1(2) . . . . ? C10 C3 C4 C14 0.2(4) . . . . ? Ce1 C3 C4 C14 129.4(2) . . . . ? C2 C3 C4 Ce1 63.48(14) . . . . ? C10 C3 C4 Ce1 -129.2(2) . . . . ? C2 C1 C5 C4 2.5(2) . . . . ? C6 C1 C5 C4 -176.37(18) . . . . ? Ce1 C1 C5 C4 73.46(14) . . . . ? C2 C1 C5 Ce1 -70.97(14) . . . . ? C6 C1 C5 Ce1 110.2(2) . . . . ? C3 C4 C5 C1 -0.6(2) . . . . ? C14 C4 C5 C1 167.67(17) . . . . ? Ce1 C4 C5 C1 -70.14(14) . . . . ? C3 C4 C5 Ce1 69.56(14) . . . . ? C14 C4 C5 Ce1 -122.19(16) . . . . ? C5 C1 C6 C7 142.7(2) . . . . ? C2 C1 C6 C7 -35.9(3) . . . . ? Ce1 C1 C6 C7 -127.13(17) . . . . ? C5 C1 C6 C9 -96.6(2) . . . . ? C2 C1 C6 C9 84.8(3) . . . . ? Ce1 C1 C6 C9 -6.4(2) . . . . ? C5 C1 C6 C8 22.9(3) . . . . ? C2 C1 C6 C8 -155.7(2) . . . . ? Ce1 C1 C6 C8 113.06(17) . . . . ? C2 C3 C10 C13 -120.5(2) . . . . ? C4 C3 C10 C13 73.7(3) . . . . ? Ce1 C3 C10 C13 -31.6(3) . . . . ? C2 C3 C10 C12 -0.5(3) . . . . ? C4 C3 C10 C12 -166.4(2) . . . . ? Ce1 C3 C10 C12 88.3(2) . . . . ? C2 C3 C10 C11 115.4(2) . . . . ? C4 C3 C10 C11 -50.5(3) . . . . ? Ce1 C3 C10 C11 -155.82(15) . . . . ? C5 C4 C14 C17 156.41(19) . . . . ? C3 C4 C14 C17 -39.3(3) . . . . ? Ce1 C4 C14 C17 70.3(2) . . . . ? C5 C4 C14 C16 35.6(3) . . . . ? C3 C4 C14 C16 -160.1(2) . . . . ? Ce1 C4 C14 C16 -50.5(2) . . . . ? C5 C4 C14 C15 -80.2(2) . . . . ? C3 C4 C14 C15 84.1(3) . . . . ? Ce1 C4 C14 C15 -166.25(14) . . . . ? C22 C18 C19 C20 -3.4(2) . . . . ? C23 C18 C19 C20 175.08(19) . . . . ? Ce1 C18 C19 C20 -73.41(15) . . . . ? C22 C18 C19 Ce1 70.03(14) . . . . ? C23 C18 C19 Ce1 -111.5(2) . . . . ? C18 C19 C20 C21 1.7(2) . . . . ? Ce1 C19 C20 C21 -68.97(13) . . . . ? C18 C19 C20 C27 -163.19(18) . . . . ? Ce1 C19 C20 C27 126.10(17) . . . . ? C18 C19 C20 Ce1 70.70(14) . . . . ? C19 C20 C21 C22 0.6(2) . . . . ? C27 C20 C21 C22 161.9(2) . . . . ? Ce1 C20 C21 C22 -64.18(13) . . . . ? C19 C20 C21 C31 -167.4(2) . . . . ? C27 C20 C21 C31 -6.1(4) . . . . ? Ce1 C20 C21 C31 127.8(2) . . . . ? C19 C20 C21 Ce1 64.78(13) . . . . ? C27 C20 C21 Ce1 -133.9(2) . . . . ? C19 C18 C22 C21 3.8(2) . . . . ? C23 C18 C22 C21 -174.67(19) . . . . ? Ce1 C18 C22 C21 72.84(15) . . . . ? C19 C18 C22 Ce1 -69.06(14) . . . . ? C23 C18 C22 Ce1 112.5(2) . . . . ? C20 C21 C22 C18 -2.7(2) . . . . ? C31 C21 C22 C18 167.00(17) . . . . ? Ce1 C21 C22 C18 -69.26(14) . . . . ? C20 C21 C22 Ce1 66.52(13) . . . . ? C31 C21 C22 Ce1 -123.73(17) . . . . ? C19 C18 C23 C26 -150.4(2) . . . . ? C22 C18 C23 C26 27.7(3) . . . . ? Ce1 C18 C23 C26 119.69(18) . . . . ? C19 C18 C23 C24 89.7(3) . . . . ? C22 C18 C23 C24 -92.2(3) . . . . ? Ce1 C18 C23 C24 -0.2(2) . . . . ? C19 C18 C23 C25 -29.6(3) . . . . ? C22 C18 C23 C25 148.5(2) . . . . ? Ce1 C18 C23 C25 -119.50(18) . . . . ? C19 C20 C27 C29 -160.05(19) . . . . ? C21 C20 C27 C29 40.2(3) . . . . ? Ce1 C20 C27 C29 -73.0(2) . . . . ? C19 C20 C27 C30 77.3(2) . . . . ? C21 C20 C27 C30 -82.4(3) . . . . ? Ce1 C20 C27 C30 164.39(14) . . . . ? C19 C20 C27 C28 -39.1(3) . . . . ? C21 C20 C27 C28 161.2(2) . . . . ? Ce1 C20 C27 C28 48.0(2) . . . . ? C22 C21 C31 C32 126.5(2) . . . . ? C20 C21 C31 C32 -66.9(3) . . . . ? Ce1 C21 C31 C32 37.7(2) . . . . ? C22 C21 C31 C34 -108.7(2) . . . . ? C20 C21 C31 C34 58.0(3) . . . . ? Ce1 C21 C31 C34 162.55(14) . . . . ? C22 C21 C31 C33 6.5(3) . . . . ? C20 C21 C31 C33 173.1(2) . . . . ? Ce1 C21 C31 C33 -82.3(2) . . . . ? Ce1 O1 S1 O3 -127.83(9) . . . . ? Ce1 O1 S1 O2 6.20(9) . . . . ? Ce1 O1 S1 C35 117.74(8) . . . . ? Ce1 O2 S1 O3 128.24(8) . . . . ? Ce1 O2 S1 O1 -6.23(9) . . . . ? Ce1 O2 S1 C35 -116.62(8) . . . . ? F3 C35 S1 O3 68.36(17) . . . . ? F2 C35 S1 O3 -52.20(18) . . . . ? F1 C35 S1 O3 -171.69(16) . . . . ? F3 C35 S1 O1 -168.31(14) . . . . ? F2 C35 S1 O1 71.14(16) . . . . ? F1 C35 S1 O1 -48.35(18) . . . . ? F3 C35 S1 O2 -54.84(16) . . . . ? F2 C35 S1 O2 -175.40(14) . . . . ? F1 C35 S1 O2 65.12(18) . . . . ? F3 C35 S1 Ce1 -111.81(13) . . . . ? F2 C35 S1 Ce1 127.63(12) . . . . ? F1 C35 S1 Ce1 8.1(2) . . . . ? S1 O2 Ce1 O1 4.10(6) . . . . ? S1 O2 Ce1 C19 -109.22(8) . . . . ? S1 O2 Ce1 C18 -108.28(8) . . . . ? S1 O2 Ce1 C5 96.29(8) . . . . ? S1 O2 Ce1 C1 83.25(8) . . . . ? S1 O2 Ce1 C22 -80.27(8) . . . . ? S1 O2 Ce1 C2 109.88(9) . . . . ? S1 O2 Ce1 C20 -75.27(9) . . . . ? S1 O2 Ce1 C4 125.39(8) . . . . ? S1 O2 Ce1 C21 -60.92(8) . . . . ? S1 O2 Ce1 C3 136.26(7) . . . . ? S1 O1 Ce1 O2 -4.10(6) . . . . ? S1 O1 Ce1 C19 99.37(8) . . . . ? S1 O1 Ce1 C18 72.00(8) . . . . ? S1 O1 Ce1 C5 -90.27(8) . . . . ? S1 O1 Ce1 C1 -119.28(8) . . . . ? S1 O1 Ce1 C22 81.00(8) . . . . ? S1 O1 Ce1 C2 -125.78(8) . . . . ? S1 O1 Ce1 C20 122.79(8) . . . . ? S1 O1 Ce1 C4 -72.44(9) . . . . ? S1 O1 Ce1 C21 110.51(8) . . . . ? S1 O1 Ce1 C3 -92.08(10) . . . . ? C18 C19 Ce1 O2 1.91(14) . . . . ? C20 C19 Ce1 O2 116.28(12) . . . . ? C18 C19 Ce1 O1 -62.69(14) . . . . ? C20 C19 Ce1 O1 51.68(14) . . . . ? C20 C19 Ce1 C18 114.37(18) . . . . ? C18 C19 Ce1 C5 134.08(13) . . . . ? C20 C19 Ce1 C5 -111.55(14) . . . . ? C18 C19 Ce1 C1 167.70(11) . . . . ? C20 C19 Ce1 C1 -77.93(14) . . . . ? C18 C19 Ce1 C22 -38.02(12) . . . . ? C20 C19 Ce1 C22 76.35(13) . . . . ? C18 C19 Ce1 C2 153.93(12) . . . . ? C20 C19 Ce1 C2 -91.71(13) . . . . ? C18 C19 Ce1 C20 -114.37(18) . . . . ? C18 C19 Ce1 C4 108.45(13) . . . . ? C20 C19 Ce1 C4 -137.19(12) . . . . ? C18 C19 Ce1 C21 -77.38(13) . . . . ? C20 C19 Ce1 C21 36.99(11) . . . . ? C18 C19 Ce1 C3 125.10(13) . . . . ? C20 C19 Ce1 C3 -120.54(12) . . . . ? C19 C18 Ce1 O2 -178.33(13) . . . . ? C22 C18 Ce1 O2 70.27(12) . . . . ? C23 C18 Ce1 O2 -54.56(15) . . . . ? C19 C18 Ce1 O1 129.64(12) . . . . ? C22 C18 Ce1 O1 18.24(13) . . . . ? C23 C18 Ce1 O1 -106.59(15) . . . . ? C22 C18 Ce1 C19 -111.40(18) . . . . ? C23 C18 Ce1 C19 123.8(2) . . . . ? C19 C18 Ce1 C5 -96.86(17) . . . . ? C22 C18 Ce1 C5 151.74(14) . . . . ? C23 C18 Ce1 C5 26.9(2) . . . . ? C19 C18 Ce1 C1 -23.5(2) . . . . ? C22 C18 Ce1 C1 -134.90(15) . . . . ? C23 C18 Ce1 C1 100.27(19) . . . . ? C19 C18 Ce1 C22 111.40(18) . . . . ? C23 C18 Ce1 C22 -124.8(2) . . . . ? C19 C18 Ce1 C2 -32.21(15) . . . . ? C22 C18 Ce1 C2 -143.60(11) . . . . ? C23 C18 Ce1 C2 91.56(16) . . . . ? C19 C18 Ce1 C20 36.50(12) . . . . ? C22 C18 Ce1 C20 -74.90(13) . . . . ? C23 C18 Ce1 C20 160.27(19) . . . . ? C19 C18 Ce1 C4 -91.85(13) . . . . ? C22 C18 Ce1 C4 156.75(11) . . . . ? C23 C18 Ce1 C4 31.91(18) . . . . ? C19 C18 Ce1 C21 75.49(13) . . . . ? C22 C18 Ce1 C21 -35.90(11) . . . . ? C23 C18 Ce1 C21 -160.74(19) . . . . ? C19 C18 Ce1 C3 -62.01(14) . . . . ? C22 C18 Ce1 C3 -173.41(11) . . . . ? C23 C18 Ce1 C3 61.76(17) . . . . ? C1 C5 Ce1 O2 -155.12(12) . . . . ? C4 C5 Ce1 O2 90.38(12) . . . . ? C1 C5 Ce1 O1 -100.88(12) . . . . ? C4 C5 Ce1 O1 144.62(12) . . . . ? C1 C5 Ce1 C19 65.34(16) . . . . ? C4 C5 Ce1 C19 -49.16(16) . . . . ? C1 C5 Ce1 C18 122.83(16) . . . . ? C4 C5 Ce1 C18 8.3(2) . . . . ? C4 C5 Ce1 C1 -114.50(17) . . . . ? C1 C5 Ce1 C22 -140.5(2) . . . . ? C4 C5 Ce1 C22 105.0(3) . . . . ? C1 C5 Ce1 C2 38.38(11) . . . . ? C4 C5 Ce1 C2 -76.12(13) . . . . ? C1 C5 Ce1 C20 13.37(17) . . . . ? C4 C5 Ce1 C20 -101.13(14) . . . . ? C1 C5 Ce1 C4 114.50(17) . . . . ? C1 C5 Ce1 C21 -43.1(2) . . . . ? C4 C5 Ce1 C21 -157.56(13) . . . . ? C1 C5 Ce1 C3 77.46(13) . . . . ? C4 C5 Ce1 C3 -37.04(11) . . . . ? C5 C1 Ce1 O2 27.25(13) . . . . ? C2 C1 Ce1 O2 137.83(11) . . . . ? C6 C1 Ce1 O2 -97.86(14) . . . . ? C5 C1 Ce1 O1 80.47(12) . . . . ? C2 C1 Ce1 O1 -168.95(12) . . . . ? C6 C1 Ce1 O1 -44.64(14) . . . . ? C5 C1 Ce1 C19 -139.22(12) . . . . ? C2 C1 Ce1 C19 -28.65(15) . . . . ? C6 C1 Ce1 C19 95.66(15) . . . . ? C5 C1 Ce1 C18 -125.14(15) . . . . ? C2 C1 Ce1 C18 -14.6(2) . . . . ? C6 C1 Ce1 C18 109.75(17) . . . . ? C2 C1 Ce1 C5 110.57(17) . . . . ? C6 C1 Ce1 C5 -125.1(2) . . . . ? C5 C1 Ce1 C22 155.09(16) . . . . ? C2 C1 Ce1 C22 -94.3(2) . . . . ? C6 C1 Ce1 C22 30.0(3) . . . . ? C5 C1 Ce1 C2 -110.57(17) . . . . ? C6 C1 Ce1 C2 124.3(2) . . . . ? C5 C1 Ce1 C20 -171.44(11) . . . . ? C2 C1 Ce1 C20 -60.86(13) . . . . ? C6 C1 Ce1 C20 63.45(15) . . . . ? C5 C1 Ce1 C4 -36.14(11) . . . . ? C2 C1 Ce1 C4 74.43(13) . . . . ? C6 C1 Ce1 C4 -161.26(17) . . . . ? C5 C1 Ce1 C21 158.50(11) . . . . ? C2 C1 Ce1 C21 -90.93(13) . . . . ? C6 C1 Ce1 C21 33.38(17) . . . . ? C5 C1 Ce1 C3 -75.01(13) . . . . ? C2 C1 Ce1 C3 35.56(12) . . . . ? C6 C1 Ce1 C3 159.87(17) . . . . ? C18 C22 Ce1 O2 -107.12(12) . . . . ? C21 C22 Ce1 O2 138.00(13) . . . . ? C18 C22 Ce1 O1 -162.35(12) . . . . ? C21 C22 Ce1 O1 82.76(12) . . . . ? C18 C22 Ce1 C19 38.15(12) . . . . ? C21 C22 Ce1 C19 -76.73(13) . . . . ? C21 C22 Ce1 C18 -114.88(18) . . . . ? C18 C22 Ce1 C5 -121.9(3) . . . . ? C21 C22 Ce1 C5 123.2(2) . . . . ? C18 C22 Ce1 C1 120.24(18) . . . . ? C21 C22 Ce1 C1 5.4(2) . . . . ? C18 C22 Ce1 C2 59.53(17) . . . . ? C21 C22 Ce1 C2 -55.35(18) . . . . ? C18 C22 Ce1 C20 78.19(13) . . . . ? C21 C22 Ce1 C20 -36.69(11) . . . . ? C18 C22 Ce1 C4 -41.91(19) . . . . ? C21 C22 Ce1 C4 -156.79(12) . . . . ? C18 C22 Ce1 C21 114.88(18) . . . . ? C18 C22 Ce1 C3 9.96(17) . . . . ? C21 C22 Ce1 C3 -104.92(14) . . . . ? C1 C2 Ce1 O2 -57.12(14) . . . . ? C3 C2 Ce1 O2 57.89(14) . . . . ? C1 C2 Ce1 O1 13.30(14) . . . . ? C3 C2 Ce1 O1 128.32(12) . . . . ? C1 C2 Ce1 C19 156.88(12) . . . . ? C3 C2 Ce1 C19 -88.10(13) . . . . ? C1 C2 Ce1 C18 172.33(11) . . . . ? C3 C2 Ce1 C18 -72.65(14) . . . . ? C1 C2 Ce1 C5 -38.59(11) . . . . ? C3 C2 Ce1 C5 76.42(13) . . . . ? C3 C2 Ce1 C1 115.01(18) . . . . ? C1 C2 Ce1 C22 140.94(13) . . . . ? C3 C2 Ce1 C22 -104.05(15) . . . . ? C1 C2 Ce1 C20 127.00(12) . . . . ? C3 C2 Ce1 C20 -117.99(12) . . . . ? C1 C2 Ce1 C4 -78.37(13) . . . . ? C3 C2 Ce1 C4 36.65(12) . . . . ? C1 C2 Ce1 C21 111.89(12) . . . . ? C3 C2 Ce1 C21 -133.10(12) . . . . ? C1 C2 Ce1 C3 -115.01(18) . . . . ? C19 C20 Ce1 O2 -82.87(13) . . . . ? C21 C20 Ce1 O2 29.97(14) . . . . ? C27 C20 Ce1 O2 167.07(16) . . . . ? C19 C20 Ce1 O1 -138.15(12) . . . . ? C21 C20 Ce1 O1 -25.32(12) . . . . ? C27 C20 Ce1 O1 111.78(17) . . . . ? C21 C20 Ce1 C19 112.84(18) . . . . ? C27 C20 Ce1 C19 -110.1(2) . . . . ? C19 C20 Ce1 C18 -36.57(12) . . . . ? C21 C20 Ce1 C18 76.27(13) . . . . ? C27 C20 Ce1 C18 -146.6(2) . . . . ? C19 C20 Ce1 C5 111.74(14) . . . . ? C21 C20 Ce1 C5 -135.42(12) . . . . ? C27 C20 Ce1 C5 1.7(2) . . . . ? C19 C20 Ce1 C1 118.98(12) . . . . ? C21 C20 Ce1 C1 -128.18(12) . . . . ? C27 C20 Ce1 C1 8.91(19) . . . . ? C19 C20 Ce1 C22 -76.24(13) . . . . ? C21 C20 Ce1 C22 36.60(11) . . . . ? C27 C20 Ce1 C22 173.7(2) . . . . ? C19 C20 Ce1 C2 93.31(13) . . . . ? C21 C20 Ce1 C2 -153.85(12) . . . . ? C27 C20 Ce1 C2 -16.76(18) . . . . ? C19 C20 Ce1 C4 63.89(15) . . . . ? C21 C20 Ce1 C4 176.73(11) . . . . ? C27 C20 Ce1 C4 -46.2(2) . . . . ? C19 C20 Ce1 C21 -112.84(18) . . . . ? C27 C20 Ce1 C21 137.1(2) . . . . ? C19 C20 Ce1 C3 66.36(13) . . . . ? C21 C20 Ce1 C3 179.20(11) . . . . ? C27 C20 Ce1 C3 -43.71(19) . . . . ? C5 C4 Ce1 O2 -88.14(12) . . . . ? C3 C4 Ce1 O2 159.09(12) . . . . ? C14 C4 Ce1 O2 23.18(17) . . . . ? C5 C4 Ce1 O1 -39.07(13) . . . . ? C3 C4 Ce1 O1 -151.84(11) . . . . ? C14 C4 Ce1 O1 72.24(17) . . . . ? C5 C4 Ce1 C19 148.89(11) . . . . ? C3 C4 Ce1 C19 36.12(14) . . . . ? C14 C4 Ce1 C19 -99.79(17) . . . . ? C5 C4 Ce1 C18 -175.67(11) . . . . ? C3 C4 Ce1 C18 71.56(14) . . . . ? C14 C4 Ce1 C18 -64.36(18) . . . . ? C3 C4 Ce1 C5 -112.77(17) . . . . ? C14 C4 Ce1 C5 111.3(2) . . . . ? C5 C4 Ce1 C1 36.66(11) . . . . ? C3 C4 Ce1 C1 -76.11(13) . . . . ? C14 C4 Ce1 C1 148.0(2) . . . . ? C5 C4 Ce1 C22 -151.65(13) . . . . ? C3 C4 Ce1 C22 95.58(16) . . . . ? C14 C4 Ce1 C22 -40.3(2) . . . . ? C5 C4 Ce1 C2 76.43(13) . . . . ? C3 C4 Ce1 C2 -36.34(12) . . . . ? C14 C4 Ce1 C2 -172.3(2) . . . . ? C5 C4 Ce1 C20 117.55(12) . . . . ? C3 C4 Ce1 C20 4.79(17) . . . . ? C14 C4 Ce1 C20 -131.13(16) . . . . ? C5 C4 Ce1 C21 125.8(3) . . . . ? C3 C4 Ce1 C21 13.1(4) . . . . ? C14 C4 Ce1 C21 -122.9(3) . . . . ? C5 C4 Ce1 C3 112.77(17) . . . . ? C14 C4 Ce1 C3 -135.9(2) . . . . ? C22 C21 Ce1 O2 -42.31(13) . . . . ? C20 C21 Ce1 O2 -156.23(11) . . . . ? C31 C21 Ce1 O2 71.82(17) . . . . ? C22 C21 Ce1 O1 -91.26(12) . . . . ? C20 C21 Ce1 O1 154.83(12) . . . . ? C31 C21 Ce1 O1 22.88(16) . . . . ? C22 C21 Ce1 C19 76.36(13) . . . . ? C20 C21 Ce1 C19 -37.55(11) . . . . ? C31 C21 Ce1 C19 -169.5(2) . . . . ? C22 C21 Ce1 C18 36.47(12) . . . . ? C20 C21 Ce1 C18 -77.44(13) . . . . ? C31 C21 Ce1 C18 150.6(2) . . . . ? C22 C21 Ce1 C5 -151.37(14) . . . . ? C20 C21 Ce1 C5 94.71(17) . . . . ? C31 C21 Ce1 C5 -37.2(3) . . . . ? C22 C21 Ce1 C1 -177.52(11) . . . . ? C20 C21 Ce1 C1 68.57(14) . . . . ? C31 C21 Ce1 C1 -63.38(19) . . . . ? C20 C21 Ce1 C22 -113.92(18) . . . . ? C31 C21 Ce1 C22 114.1(2) . . . . ? C22 C21 Ce1 C2 145.90(12) . . . . ? C20 C21 Ce1 C2 31.98(14) . . . . ? C31 C21 Ce1 C2 -99.97(17) . . . . ? C22 C21 Ce1 C20 113.92(18) . . . . ? C31 C21 Ce1 C20 -132.0(2) . . . . ? C22 C21 Ce1 C4 102.9(3) . . . . ? C20 C21 Ce1 C4 -11.0(4) . . . . ? C31 C21 Ce1 C4 -142.9(3) . . . . ? C22 C21 Ce1 C3 112.75(13) . . . . ? C20 C21 Ce1 C3 -1.17(16) . . . . ? C31 C21 Ce1 C3 -133.12(16) . . . . ? C2 C3 Ce1 O2 -137.05(12) . . . . ? C4 C3 Ce1 O2 -23.01(13) . . . . ? C10 C3 Ce1 O2 109.02(18) . . . . ? C2 C3 Ce1 O1 -74.18(14) . . . . ? C4 C3 Ce1 O1 39.86(15) . . . . ? C10 C3 Ce1 O1 171.90(15) . . . . ? C2 C3 Ce1 C19 96.31(13) . . . . ? C4 C3 Ce1 C19 -149.65(12) . . . . ? C10 C3 Ce1 C19 -17.62(19) . . . . ? C2 C3 Ce1 C18 122.34(12) . . . . ? C4 C3 Ce1 C18 -123.62(12) . . . . ? C10 C3 Ce1 C18 8.4(2) . . . . ? C2 C3 Ce1 C5 -76.64(13) . . . . ? C4 C3 Ce1 C5 37.40(12) . . . . ? C10 C3 Ce1 C5 169.4(2) . . . . ? C2 C3 Ce1 C1 -36.53(12) . . . . ? C4 C3 Ce1 C1 77.51(13) . . . . ? C10 C3 Ce1 C1 -150.5(2) . . . . ? C2 C3 Ce1 C22 117.03(13) . . . . ? C4 C3 Ce1 C22 -128.92(13) . . . . ? C10 C3 Ce1 C22 3.1(2) . . . . ? C4 C3 Ce1 C2 114.04(18) . . . . ? C10 C3 Ce1 C2 -113.9(2) . . . . ? C2 C3 Ce1 C20 69.26(13) . . . . ? C4 C3 Ce1 C20 -176.70(12) . . . . ? C10 C3 Ce1 C20 -44.66(19) . . . . ? C2 C3 Ce1 C4 -114.04(18) . . . . ? C10 C3 Ce1 C4 132.0(2) . . . . ? C2 C3 Ce1 C21 69.87(15) . . . . ? C4 C3 Ce1 C21 -176.09(11) . . . . ? C10 C3 Ce1 C21 -44.1(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.045 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.061