# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Paula L Diaconescu,' _publ_contact_author_email pld@chem.ucla.edu _publ_section_title ; Broderick, Erin; Guo, Neng; Wu, Tianpin; Vogel, Carola; Xu, Cuiling; Sutter, Joerg; Miller, Jeffery T.; Meyer, Karsten; Cantat, Thibault; Diaconescu, Paula L ; loop_ _publ_author_name E.Broderick 'Neng Guo' 'Tianpin Wu' C.Vogel 'Cuiling Xu' J.Sutter J.T.Miller K.Meyer T.Cantat P.L.Diaconescu # Attachment '- cerium_switch_cif.txt' data_[2-Ce(OtBu)]2 _database_code_depnum_ccdc_archive 'CCDC 827399' #TrackingRef '- cerium_switch_cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H110 Ce2 N4 O6, C5 H12, C4 H10' _chemical_formula_sum 'C81 H132 Ce2 N4 O7' _chemical_formula_weight 1554.15 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.471(3) _cell_length_b 16.704(3) _cell_length_c 17.748(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.508(2) _cell_angle_gamma 90.00 _cell_volume 4188.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 3.85 _cell_measurement_theta_max 30.52 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1636 _exptl_absorpt_coefficient_mu 1.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7589 _exptl_absorpt_correction_T_max 0.9357 _exptl_absorpt_process_details 'Twinabs (Bruker)' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41545 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 30.84 _reflns_number_total 23106 _reflns_number_gt 21599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0191P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(5) _refine_ls_number_reflns 23106 _refine_ls_number_parameters 856 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.382405(9) 0.673120(7) 0.276893(7) 0.01330(3) Uani 1 1 d . . . Ce2 Ce 0.390318(8) 0.826910(7) 0.429208(7) 0.01285(3) Uani 1 1 d . . . N1 N 0.51291(13) 0.56105(11) 0.29479(11) 0.0157(4) Uani 1 1 d . . . N2 N 0.55425(14) 0.71866(11) 0.29739(11) 0.0155(4) Uani 1 1 d . . . N3 N 0.45686(13) 0.91122(11) 0.33102(11) 0.0146(4) Uani 1 1 d . . . N4 N 0.31048(14) 0.96741(11) 0.38998(11) 0.0140(4) Uani 1 1 d . . . O1 O 0.41281(11) 0.68369(10) 0.41690(9) 0.0175(3) Uani 1 1 d . . . O2 O 0.28897(11) 0.78492(9) 0.31100(9) 0.0167(3) Uani 1 1 d . . . O3 O 0.31416(11) 0.55637(10) 0.23011(10) 0.0178(3) Uani 1 1 d . . . O4 O 0.40385(12) 0.74429(10) 0.17282(10) 0.0189(3) Uani 1 1 d . . . O5 O 0.55007(11) 0.84408(9) 0.47021(9) 0.0164(3) Uani 1 1 d . . . O6 O 0.30415(11) 0.86316(9) 0.51801(9) 0.0159(3) Uani 1 1 d . . . C1 C 0.32854(16) 0.48259(14) 0.20844(13) 0.0160(4) Uani 1 1 d . . . C2 C 0.42032(16) 0.44835(14) 0.22612(14) 0.0155(5) Uani 1 1 d . . . C3 C 0.43408(18) 0.36865(14) 0.20516(14) 0.0184(5) Uani 1 1 d . . . H3A H 0.4963 0.3472 0.2171 0.022 Uiso 1 1 calc R . . C4 C 0.36091(16) 0.32046(15) 0.16796(13) 0.0183(4) Uani 1 1 d . . . C5 C 0.27130(17) 0.35601(14) 0.14948(14) 0.0195(5) Uani 1 1 d . . . H5A H 0.2200 0.3242 0.1231 0.023 Uiso 1 1 calc R . . C6 C 0.25185(17) 0.43469(15) 0.16694(14) 0.0188(5) Uani 1 1 d . . . C7 C 0.15052(17) 0.46914(16) 0.14558(15) 0.0232(5) Uani 1 1 d . . . C8 C 0.14779(19) 0.54630(16) 0.09758(15) 0.0269(6) Uani 1 1 d . . . H8A H 0.1910 0.5859 0.1270 0.040 Uiso 1 1 calc R . . H8B H 0.0833 0.5678 0.0859 0.040 Uiso 1 1 calc R . . H8C H 0.1674 0.5342 0.0493 0.040 Uiso 1 1 calc R . . C9 C 0.08051(19) 0.41035(19) 0.09645(19) 0.0371(7) Uani 1 1 d . . . H9A H 0.0181 0.4356 0.0817 0.056 Uiso 1 1 calc R . . H9B H 0.0759 0.3618 0.1265 0.056 Uiso 1 1 calc R . . H9C H 0.1030 0.3962 0.0499 0.056 Uiso 1 1 calc R . . C10 C 0.11584(18) 0.48630(18) 0.22044(16) 0.0261(6) Uani 1 1 d . . . H10A H 0.1618 0.5206 0.2544 0.039 Uiso 1 1 calc R . . H10B H 0.1094 0.4357 0.2468 0.039 Uiso 1 1 calc R . . H10C H 0.0544 0.5134 0.2076 0.039 Uiso 1 1 calc R . . C11 C 0.37940(19) 0.23321(15) 0.14910(15) 0.0227(5) Uani 1 1 d . . . C12 C 0.4379(3) 0.23061(18) 0.0869(2) 0.0438(8) Uani 1 1 d . . . H12A H 0.4027 0.2567 0.0400 0.066 Uiso 1 1 calc R . . H12B H 0.4506 0.1748 0.0755 0.066 Uiso 1 1 calc R . . H12C H 0.4980 0.2587 0.1055 0.066 Uiso 1 1 calc R . . C13 C 0.4350(2) 0.19049(17) 0.22226(18) 0.0405(8) Uani 1 1 d . . . H13A H 0.3987 0.1929 0.2628 0.061 Uiso 1 1 calc R . . H13B H 0.4962 0.2171 0.2402 0.061 Uiso 1 1 calc R . . H13C H 0.4455 0.1344 0.2101 0.061 Uiso 1 1 calc R . . C14 C 0.2881(2) 0.18588(18) 0.1211(2) 0.0423(8) Uani 1 1 d . . . H14A H 0.2503 0.2114 0.0749 0.063 Uiso 1 1 calc R . . H14B H 0.2518 0.1849 0.1618 0.063 Uiso 1 1 calc R . . H14C H 0.3036 0.1310 0.1088 0.063 Uiso 1 1 calc R . . C15 C 0.50462(17) 0.48992(14) 0.26705(14) 0.0163(5) Uani 1 1 d . . . H15A H 0.5618 0.4601 0.2742 0.020 Uiso 1 1 calc R . . C16 C 0.61092(16) 0.58458(14) 0.33247(15) 0.0180(5) Uani 1 1 d . . . H16A H 0.6528 0.5781 0.2956 0.022 Uiso 1 1 calc R . . H16B H 0.6346 0.5493 0.3773 0.022 Uiso 1 1 calc R . . C17 C 0.61329(15) 0.67165(16) 0.35932(12) 0.0161(4) Uani 1 1 d . . . H17A H 0.5886 0.6757 0.4070 0.019 Uiso 1 1 calc R . . H17B H 0.6791 0.6920 0.3704 0.019 Uiso 1 1 calc R . . C18 C 0.59642(17) 0.76509(14) 0.25778(14) 0.0168(5) Uani 1 1 d . . . H18A H 0.6627 0.7716 0.2760 0.020 Uiso 1 1 calc R . . C19 C 0.55340(17) 0.80868(13) 0.18800(13) 0.0182(5) Uani 1 1 d . . . C20 C 0.45965(17) 0.79458(14) 0.14622(14) 0.0180(5) Uani 1 1 d . . . C21 C 0.42932(17) 0.83456(15) 0.07368(13) 0.0198(5) Uani 1 1 d . . . C22 C 0.49114(19) 0.88928(15) 0.05138(14) 0.0223(5) Uani 1 1 d . . . H22A H 0.4695 0.9176 0.0044 0.027 Uiso 1 1 calc R . . C23 C 0.58257(19) 0.90541(15) 0.09318(15) 0.0226(5) Uani 1 1 d . . . C24 C 0.61260(19) 0.86297(15) 0.16071(15) 0.0214(5) Uani 1 1 d . . . H24A H 0.6753 0.8707 0.1897 0.026 Uiso 1 1 calc R . . C25 C 0.33234(18) 0.81659(16) 0.02218(14) 0.0239(5) Uani 1 1 d . . . C26 C 0.25329(19) 0.84036(18) 0.06392(16) 0.0318(6) Uani 1 1 d . . . H26A H 0.2623 0.8117 0.1132 0.048 Uiso 1 1 calc R . . H26B H 0.1916 0.8263 0.0316 0.048 Uiso 1 1 calc R . . H26C H 0.2558 0.8982 0.0735 0.048 Uiso 1 1 calc R . . C27 C 0.3248(2) 0.72662(17) 0.00247(16) 0.0293(6) Uani 1 1 d . . . H27A H 0.3344 0.6954 0.0503 0.044 Uiso 1 1 calc R . . H27B H 0.3732 0.7122 -0.0261 0.044 Uiso 1 1 calc R . . H27C H 0.2619 0.7151 -0.0293 0.044 Uiso 1 1 calc R . . C28 C 0.3140(2) 0.86276(19) -0.05489(17) 0.0343(7) Uani 1 1 d . . . H28A H 0.3636 0.8497 -0.0828 0.051 Uiso 1 1 calc R . . H28B H 0.3148 0.9204 -0.0446 0.051 Uiso 1 1 calc R . . H28C H 0.2522 0.8475 -0.0862 0.051 Uiso 1 1 calc R . . C29 C 0.6490(2) 0.96648(17) 0.06756(16) 0.0291(6) Uani 1 1 d . . . C30 C 0.6705(3) 1.03397(18) 0.12645(18) 0.0433(9) Uani 1 1 d . . . H30A H 0.7019 1.0121 0.1767 0.065 Uiso 1 1 calc R . . H30B H 0.6112 1.0600 0.1310 0.065 Uiso 1 1 calc R . . H30C H 0.7120 1.0733 0.1096 0.065 Uiso 1 1 calc R . . C31 C 0.7427(2) 0.9245(2) 0.06249(19) 0.0414(8) Uani 1 1 d . . . H31A H 0.7700 0.8990 0.1120 0.062 Uiso 1 1 calc R . . H31B H 0.7873 0.9642 0.0504 0.062 Uiso 1 1 calc R . . H31C H 0.7302 0.8838 0.0218 0.062 Uiso 1 1 calc R . . C32 C 0.6068(2) 1.00269(18) -0.01185(16) 0.0360(7) Uani 1 1 d . . . H32A H 0.5481 1.0310 -0.0099 0.054 Uiso 1 1 calc R . . H32B H 0.5933 0.9599 -0.0504 0.054 Uiso 1 1 calc R . . H32C H 0.6522 1.0403 -0.0260 0.054 Uiso 1 1 calc R . . C33 C 0.62995(16) 0.86656(13) 0.45213(14) 0.0153(4) Uani 1 1 d . . . C34 C 0.72017(16) 0.84901(13) 0.50070(13) 0.0160(5) Uani 1 1 d . . . C35 C 0.80093(17) 0.87351(14) 0.47564(14) 0.0178(5) Uani 1 1 d . . . H35A H 0.8608 0.8610 0.5076 0.021 Uiso 1 1 calc R . . C36 C 0.80025(17) 0.91492(14) 0.40734(14) 0.0180(5) Uani 1 1 d . . . C37 C 0.71244(16) 0.93354(14) 0.36260(14) 0.0166(5) Uani 1 1 d . . . H37A H 0.7091 0.9635 0.3166 0.020 Uiso 1 1 calc R . . C38 C 0.62777(16) 0.90975(13) 0.38266(13) 0.0152(4) Uani 1 1 d . . . C39 C 0.54116(16) 0.93321(13) 0.32985(13) 0.0146(4) Uani 1 1 d . . . H39A H 0.5477 0.9690 0.2898 0.018 Uiso 1 1 calc R . . C40 C 0.72703(17) 0.80816(14) 0.57879(14) 0.0201(5) Uani 1 1 d . . . C41 C 0.6783(2) 0.85981(16) 0.63033(15) 0.0245(6) Uani 1 1 d . . . H41A H 0.6120 0.8683 0.6046 0.037 Uiso 1 1 calc R . . H41B H 0.7105 0.9116 0.6396 0.037 Uiso 1 1 calc R . . H41C H 0.6813 0.8325 0.6797 0.037 Uiso 1 1 calc R . . C42 C 0.68056(19) 0.72508(15) 0.56723(15) 0.0240(5) Uani 1 1 d . . . H42A H 0.6148 0.7305 0.5388 0.036 Uiso 1 1 calc R . . H42B H 0.6818 0.7006 0.6176 0.036 Uiso 1 1 calc R . . H42C H 0.7154 0.6911 0.5379 0.036 Uiso 1 1 calc R . . C43 C 0.83058(19) 0.79548(18) 0.62232(16) 0.0299(6) Uani 1 1 d . . . H43A H 0.8315 0.7695 0.6720 0.045 Uiso 1 1 calc R . . H43B H 0.8626 0.8474 0.6312 0.045 Uiso 1 1 calc R . . H43C H 0.8633 0.7615 0.5914 0.045 Uiso 1 1 calc R . . C44 C 0.89087(17) 0.93919(15) 0.38100(15) 0.0204(5) Uani 1 1 d . . . C45 C 0.98038(17) 0.91365(16) 0.43885(16) 0.0233(5) Uani 1 1 d . . . H45A H 0.9806 0.8553 0.4450 0.035 Uiso 1 1 calc R . . H45B H 0.9817 0.9392 0.4888 0.035 Uiso 1 1 calc R . . H45C H 1.0363 0.9301 0.4199 0.035 Uiso 1 1 calc R . . C46 C 0.8931(2) 1.03036(16) 0.37066(18) 0.0293(6) Uani 1 1 d . . . H46A H 0.8386 1.0470 0.3307 0.044 Uiso 1 1 calc R . . H46B H 0.9517 1.0456 0.3551 0.044 Uiso 1 1 calc R . . H46C H 0.8906 1.0567 0.4195 0.044 Uiso 1 1 calc R . . C47 C 0.89120(19) 0.89806(18) 0.30300(16) 0.0282(6) Uani 1 1 d . . . H47A H 0.8870 0.8399 0.3088 0.042 Uiso 1 1 calc R . . H47B H 0.9499 0.9114 0.2868 0.042 Uiso 1 1 calc R . . H47C H 0.8369 0.9168 0.2640 0.042 Uiso 1 1 calc R . . C48 C 0.37997(16) 0.95029(14) 0.27578(14) 0.0152(4) Uani 1 1 d . . . H48A H 0.3342 0.9099 0.2493 0.018 Uiso 1 1 calc R . . H48B H 0.4056 0.9798 0.2364 0.018 Uiso 1 1 calc R . . C49 C 0.33203(17) 1.00760(14) 0.32136(14) 0.0166(5) Uani 1 1 d . . . H49A H 0.3739 1.0541 0.3380 0.020 Uiso 1 1 calc R . . H49B H 0.2726 1.0276 0.2881 0.020 Uiso 1 1 calc R . . C50 C 0.25796(16) 1.00875(14) 0.42563(14) 0.0156(5) Uani 1 1 d . . . H50A H 0.2369 1.0588 0.4027 0.019 Uiso 1 1 calc R . . C51 C 0.22635(15) 0.98950(13) 0.49617(13) 0.0131(4) Uani 1 1 d . . . C52 C 0.24695(16) 0.91697(13) 0.53850(13) 0.0144(4) Uani 1 1 d . . . C53 C 0.20318(16) 0.90431(14) 0.60239(14) 0.0146(5) Uani 1 1 d . . . C54 C 0.14982(16) 0.96588(14) 0.62344(13) 0.0164(5) Uani 1 1 d . . . H54A H 0.1236 0.9580 0.6676 0.020 Uiso 1 1 calc R . . C55 C 0.13166(16) 1.03917(14) 0.58425(14) 0.0163(5) Uani 1 1 d . . . C56 C 0.16966(16) 1.04879(13) 0.52008(13) 0.0147(4) Uani 1 1 d . . . H56A H 0.1573 1.0969 0.4911 0.018 Uiso 1 1 calc R . . C57 C 0.21090(15) 0.82303(15) 0.64410(13) 0.0176(4) Uani 1 1 d . . . C58 C 0.15458(19) 0.82062(18) 0.70791(14) 0.0265(5) Uani 1 1 d . . . H58A H 0.0875 0.8303 0.6854 0.040 Uiso 1 1 calc R . . H58B H 0.1783 0.8621 0.7463 0.040 Uiso 1 1 calc R . . H58C H 0.1619 0.7679 0.7328 0.040 Uiso 1 1 calc R . . C59 C 0.31408(17) 0.80406(15) 0.68279(15) 0.0223(5) Uani 1 1 d . . . H59A H 0.3535 0.8076 0.6444 0.034 Uiso 1 1 calc R . . H59B H 0.3180 0.7498 0.7043 0.034 Uiso 1 1 calc R . . H59C H 0.3366 0.8427 0.7243 0.034 Uiso 1 1 calc R . . C60 C 0.16823(19) 0.75751(15) 0.58564(15) 0.0234(5) Uani 1 1 d . . . H60A H 0.1009 0.7686 0.5655 0.035 Uiso 1 1 calc R . . H60B H 0.1753 0.7052 0.6113 0.035 Uiso 1 1 calc R . . H60C H 0.2014 0.7571 0.5430 0.035 Uiso 1 1 calc R . . C61 C 0.06978(17) 1.10251(14) 0.61186(15) 0.0189(5) Uani 1 1 d . . . C62 C 0.1175(2) 1.12904(17) 0.69411(16) 0.0292(6) Uani 1 1 d . . . H62A H 0.1798 1.1520 0.6939 0.044 Uiso 1 1 calc R . . H62B H 0.1251 1.0827 0.7287 0.044 Uiso 1 1 calc R . . H62C H 0.0781 1.1694 0.7121 0.044 Uiso 1 1 calc R . . C63 C -0.02815(18) 1.06805(16) 0.61277(16) 0.0253(6) Uani 1 1 d . . . H63A H -0.0603 1.0533 0.5602 0.038 Uiso 1 1 calc R . . H63B H -0.0658 1.1084 0.6328 0.038 Uiso 1 1 calc R . . H63C H -0.0210 1.0205 0.6459 0.038 Uiso 1 1 calc R . . C64 C 0.05650(19) 1.17645(17) 0.55951(15) 0.0280(5) Uani 1 1 d . . . H64A H 0.0270 1.1605 0.5066 0.042 Uiso 1 1 calc R . . H64B H 0.1182 1.2009 0.5603 0.042 Uiso 1 1 calc R . . H64C H 0.0157 1.2152 0.5781 0.042 Uiso 1 1 calc R . . C65 C 0.18775(16) 0.78440(14) 0.29016(14) 0.0162(5) Uani 1 1 d . . . C66 C 0.14805(18) 0.78307(16) 0.36304(15) 0.0217(5) Uani 1 1 d . . . H66A H 0.1714 0.7355 0.3936 0.033 Uiso 1 1 calc R . . H66B H 0.0788 0.7816 0.3488 0.033 Uiso 1 1 calc R . . H66C H 0.1685 0.8313 0.3936 0.033 Uiso 1 1 calc R . . C67 C 0.15059(18) 0.85890(15) 0.24341(15) 0.0212(5) Uani 1 1 d . . . H67A H 0.1697 0.9068 0.2748 0.032 Uiso 1 1 calc R . . H67B H 0.0814 0.8565 0.2284 0.032 Uiso 1 1 calc R . . H67C H 0.1768 0.8612 0.1970 0.032 Uiso 1 1 calc R . . C68 C 0.15576(18) 0.70964(15) 0.24171(16) 0.0233(5) Uani 1 1 d . . . H68A H 0.1777 0.6617 0.2722 0.035 Uiso 1 1 calc R . . H68B H 0.1826 0.7104 0.1955 0.035 Uiso 1 1 calc R . . H68C H 0.0865 0.7089 0.2263 0.035 Uiso 1 1 calc R . . C69 C 0.40252(17) 0.62363(14) 0.47208(14) 0.0177(5) Uani 1 1 d . . . C70 C 0.4043(2) 0.66461(17) 0.54961(15) 0.0274(6) Uani 1 1 d . . . H70A H 0.4662 0.6897 0.5685 0.041 Uiso 1 1 calc R . . H70B H 0.3930 0.6247 0.5871 0.041 Uiso 1 1 calc R . . H70C H 0.3548 0.7056 0.5429 0.041 Uiso 1 1 calc R . . C71 C 0.30786(19) 0.58072(16) 0.44463(18) 0.0305(6) Uani 1 1 d . . . H71A H 0.3071 0.5541 0.3953 0.046 Uiso 1 1 calc R . . H71B H 0.2562 0.6198 0.4380 0.046 Uiso 1 1 calc R . . H71C H 0.2996 0.5407 0.4830 0.046 Uiso 1 1 calc R . . C72 C 0.48268(19) 0.56273(14) 0.48223(15) 0.0210(5) Uani 1 1 d . . . H72A H 0.4829 0.5373 0.4325 0.031 Uiso 1 1 calc R . . H72B H 0.4734 0.5218 0.5195 0.031 Uiso 1 1 calc R . . H72C H 0.5433 0.5899 0.5013 0.031 Uiso 1 1 calc R . . C1S C 0.3640(3) 0.1049(3) 0.8837(2) 0.0646(12) Uani 1 1 d . . . H1SA H 0.3899 0.0511 0.8807 0.097 Uiso 1 1 calc R . . H1SB H 0.4057 0.1352 0.9247 0.097 Uiso 1 1 calc R . . H1SC H 0.3596 0.1324 0.8342 0.097 Uiso 1 1 calc R . . C2S C 0.2690(3) 0.0989(2) 0.9008(2) 0.0621(11) Uani 1 1 d . . . H2SA H 0.2753 0.0772 0.9536 0.075 Uiso 1 1 calc R . . H2SB H 0.2309 0.0605 0.8644 0.075 Uiso 1 1 calc R . . C3S C 0.2169(3) 0.1777(2) 0.89531(19) 0.0594(11) Uani 1 1 d . . . H3SA H 0.2549 0.2158 0.9322 0.071 Uiso 1 1 calc R . . H3SB H 0.2118 0.1997 0.8428 0.071 Uiso 1 1 calc R . . C4S C 0.1198(3) 0.1729(3) 0.9115(2) 0.0637(11) Uani 1 1 d . . . H4SA H 0.1244 0.1454 0.9616 0.076 Uiso 1 1 calc R . . H4SB H 0.0802 0.1390 0.8713 0.076 Uiso 1 1 calc R . . C5S C 0.0701(4) 0.2511(3) 0.9142(3) 0.096(2) Uani 1 1 d . . . H5SA H 0.0109 0.2421 0.9312 0.145 Uiso 1 1 calc R . . H5SB H 0.0561 0.2753 0.8626 0.145 Uiso 1 1 calc R . . H5SC H 0.1109 0.2872 0.9504 0.145 Uiso 1 1 calc R . . O1S O 0.0216(7) 1.0902(7) 0.1999(6) 0.275(4) Uiso 1 1 d . . . C6S C 0.0858(6) 1.0280(5) 0.1008(5) 0.142(3) Uiso 1 1 d D . . H6SA H 0.1402 1.0170 0.1430 0.213 Uiso 1 1 calc R . . H6SB H 0.0930 1.0809 0.0790 0.213 Uiso 1 1 calc R . . H6SC H 0.0825 0.9872 0.0605 0.213 Uiso 1 1 calc R . . C7S C 0.0050(6) 1.0262(6) 0.1281(5) 0.159(3) Uiso 1 1 d D . . H7SA H -0.0064 0.9718 0.1462 0.190 Uiso 1 1 calc R . . H7SB H -0.0501 1.0421 0.0873 0.190 Uiso 1 1 calc R . . C8S C 0.0121(8) 1.1804(8) 0.1848(6) 0.219(4) Uiso 1 1 d D . . H8SA H 0.0054 1.2069 0.2332 0.263 Uiso 1 1 calc R . . H8SB H 0.0718 1.1998 0.1726 0.263 Uiso 1 1 calc R . . C9S C -0.0647(6) 1.2065(5) 0.1242(5) 0.144(3) Uiso 1 1 d D . . H9SA H -0.1250 1.1947 0.1385 0.216 Uiso 1 1 calc R . . H9SB H -0.0620 1.1783 0.0763 0.216 Uiso 1 1 calc R . . H9SC H -0.0596 1.2642 0.1165 0.216 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.01265(6) 0.01172(5) 0.01616(6) 0.00036(5) 0.00449(4) 0.00117(5) Ce2 0.01254(6) 0.01089(5) 0.01651(6) 0.00083(5) 0.00622(4) 0.00130(5) N1 0.0124(9) 0.0156(9) 0.0184(10) -0.0007(8) 0.0019(7) 0.0008(7) N2 0.0143(10) 0.0155(9) 0.0161(10) -0.0005(8) 0.0023(8) 0.0016(7) N3 0.0140(9) 0.0153(9) 0.0152(9) -0.0001(8) 0.0045(7) 0.0029(8) N4 0.0159(10) 0.0118(9) 0.0149(10) -0.0016(7) 0.0048(8) -0.0006(7) O1 0.0213(8) 0.0137(8) 0.0185(8) 0.0039(6) 0.0064(6) 0.0020(7) O2 0.0122(8) 0.0160(8) 0.0226(9) 0.0013(7) 0.0055(6) 0.0022(6) O3 0.0159(8) 0.0153(8) 0.0219(9) -0.0035(7) 0.0034(7) 0.0002(6) O4 0.0171(8) 0.0206(8) 0.0198(9) 0.0055(7) 0.0057(7) -0.0015(7) O5 0.0152(8) 0.0179(9) 0.0168(8) 0.0011(6) 0.0049(6) 0.0010(6) O6 0.0179(8) 0.0140(7) 0.0180(8) 0.0010(6) 0.0085(7) 0.0024(6) C1 0.0173(11) 0.0159(10) 0.0156(11) -0.0012(9) 0.0054(9) 0.0005(9) C2 0.0153(11) 0.0148(10) 0.0167(11) 0.0002(9) 0.0041(9) -0.0002(9) C3 0.0201(12) 0.0153(11) 0.0204(12) 0.0012(9) 0.0056(9) 0.0042(9) C4 0.0227(11) 0.0148(10) 0.0184(11) -0.0020(10) 0.0065(8) 0.0005(10) C5 0.0185(12) 0.0201(11) 0.0189(12) -0.0061(9) 0.0022(9) -0.0048(9) C6 0.0159(12) 0.0226(12) 0.0180(12) -0.0051(10) 0.0038(9) -0.0023(10) C7 0.0142(12) 0.0297(14) 0.0240(13) -0.0088(11) 0.0005(10) 0.0033(10) C8 0.0232(13) 0.0342(15) 0.0215(13) -0.0044(11) 0.0007(10) 0.0111(11) C9 0.0169(13) 0.0394(17) 0.0514(19) -0.0180(15) -0.0007(13) 0.0012(12) C10 0.0173(13) 0.0273(14) 0.0345(16) -0.0057(12) 0.0073(11) -0.0021(11) C11 0.0277(14) 0.0162(11) 0.0240(13) -0.0049(10) 0.0055(11) -0.0017(10) C12 0.060(2) 0.0282(15) 0.055(2) -0.0101(14) 0.0364(18) 0.0030(15) C13 0.057(2) 0.0222(15) 0.0390(18) 0.0010(12) 0.0036(16) 0.0046(13) C14 0.0343(16) 0.0245(16) 0.067(2) -0.0166(15) 0.0090(15) -0.0043(12) C15 0.0155(11) 0.0138(10) 0.0194(12) 0.0017(9) 0.0037(9) 0.0039(9) C16 0.0126(11) 0.0157(11) 0.0241(13) -0.0012(9) 0.0008(9) 0.0012(9) C17 0.0145(10) 0.0163(10) 0.0167(10) 0.0002(11) 0.0017(8) -0.0017(10) C18 0.0160(11) 0.0162(11) 0.0191(12) -0.0037(9) 0.0059(9) -0.0017(9) C19 0.0223(12) 0.0164(12) 0.0174(11) -0.0021(9) 0.0077(9) -0.0007(9) C20 0.0207(12) 0.0177(11) 0.0173(11) -0.0021(9) 0.0079(9) 0.0013(9) C21 0.0251(12) 0.0169(11) 0.0188(11) -0.0012(10) 0.0081(9) 0.0018(10) C22 0.0298(14) 0.0210(12) 0.0172(12) 0.0020(10) 0.0075(10) 0.0015(11) C23 0.0296(14) 0.0198(12) 0.0212(13) 0.0004(10) 0.0116(11) -0.0029(10) C24 0.0233(13) 0.0208(12) 0.0217(13) -0.0017(10) 0.0079(10) -0.0021(10) C25 0.0251(12) 0.0260(13) 0.0201(12) 0.0032(11) 0.0042(9) 0.0008(11) C26 0.0257(13) 0.0406(18) 0.0291(14) 0.0072(13) 0.0058(11) 0.0074(12) C27 0.0297(15) 0.0316(14) 0.0249(14) -0.0044(11) 0.0020(11) -0.0063(12) C28 0.0348(16) 0.0397(17) 0.0257(15) 0.0084(13) 0.0006(12) 0.0001(13) C29 0.0371(17) 0.0270(14) 0.0239(14) 0.0037(11) 0.0082(12) -0.0104(12) C30 0.064(2) 0.0324(16) 0.0329(17) 0.0040(13) 0.0091(16) -0.0246(16) C31 0.0370(17) 0.054(2) 0.0371(17) 0.0126(15) 0.0174(14) -0.0150(15) C32 0.0467(18) 0.0341(16) 0.0279(15) 0.0100(12) 0.0095(13) -0.0110(14) C33 0.0158(11) 0.0123(10) 0.0184(11) -0.0028(9) 0.0051(9) 0.0003(9) C34 0.0170(11) 0.0140(10) 0.0174(11) -0.0018(8) 0.0047(9) 0.0033(8) C35 0.0132(11) 0.0198(11) 0.0197(12) -0.0052(9) 0.0022(9) 0.0030(9) C36 0.0155(11) 0.0165(11) 0.0232(13) -0.0035(9) 0.0066(9) -0.0003(9) C37 0.0169(11) 0.0161(11) 0.0178(11) 0.0006(9) 0.0062(9) -0.0002(9) C38 0.0121(10) 0.0146(10) 0.0192(11) -0.0009(9) 0.0040(9) 0.0028(8) C39 0.0181(11) 0.0131(10) 0.0143(11) 0.0000(8) 0.0071(9) 0.0006(9) C40 0.0196(12) 0.0229(13) 0.0174(11) -0.0006(9) 0.0034(9) 0.0022(9) C41 0.0289(14) 0.0269(13) 0.0181(13) 0.0014(10) 0.0062(10) 0.0063(11) C42 0.0291(14) 0.0190(11) 0.0243(13) 0.0041(10) 0.0063(11) 0.0055(10) C43 0.0239(14) 0.0404(16) 0.0230(14) 0.0057(12) -0.0002(11) 0.0049(12) C44 0.0137(11) 0.0233(12) 0.0254(13) -0.0028(10) 0.0064(10) -0.0016(9) C45 0.0123(11) 0.0238(13) 0.0334(15) -0.0046(11) 0.0043(10) -0.0019(10) C46 0.0217(14) 0.0250(14) 0.0424(17) 0.0037(12) 0.0095(12) -0.0032(11) C47 0.0186(13) 0.0392(16) 0.0293(14) -0.0046(12) 0.0109(11) -0.0011(11) C48 0.0112(10) 0.0224(11) 0.0126(11) 0.0031(9) 0.0035(8) 0.0009(9) C49 0.0187(12) 0.0145(11) 0.0181(12) 0.0043(9) 0.0073(9) 0.0035(9) C50 0.0116(11) 0.0153(11) 0.0197(12) 0.0011(9) 0.0034(9) -0.0001(9) C51 0.0110(10) 0.0144(10) 0.0146(11) -0.0017(8) 0.0039(8) -0.0002(8) C52 0.0119(10) 0.0153(10) 0.0163(11) -0.0021(9) 0.0036(8) -0.0021(8) C53 0.0117(11) 0.0172(11) 0.0150(11) 0.0003(9) 0.0030(8) -0.0024(9) C54 0.0152(11) 0.0189(11) 0.0160(11) -0.0014(9) 0.0054(9) -0.0025(9) C55 0.0143(11) 0.0165(11) 0.0191(12) -0.0029(9) 0.0056(9) 0.0005(9) C56 0.0133(11) 0.0134(10) 0.0175(11) -0.0014(9) 0.0036(9) -0.0010(8) C57 0.0191(11) 0.0153(10) 0.0196(11) 0.0026(10) 0.0070(8) -0.0014(10) C58 0.0326(13) 0.0258(13) 0.0247(12) 0.0094(12) 0.0138(10) 0.0035(12) C59 0.0221(12) 0.0212(12) 0.0222(12) 0.0045(9) 0.0015(10) 0.0026(10) C60 0.0248(14) 0.0202(12) 0.0257(14) 0.0030(10) 0.0064(11) -0.0052(10) C61 0.0173(12) 0.0195(12) 0.0216(12) -0.0019(10) 0.0080(10) 0.0043(9) C62 0.0308(15) 0.0323(15) 0.0266(14) -0.0109(12) 0.0110(11) 0.0051(12) C63 0.0180(12) 0.0285(14) 0.0325(15) -0.0025(11) 0.0124(11) 0.0051(10) C64 0.0313(13) 0.0224(12) 0.0352(14) 0.0026(13) 0.0177(11) 0.0119(13) C65 0.0106(10) 0.0171(11) 0.0202(12) -0.0003(9) 0.0017(9) -0.0002(9) C66 0.0168(12) 0.0245(13) 0.0259(14) 0.0017(11) 0.0092(10) 0.0007(10) C67 0.0156(12) 0.0214(12) 0.0272(13) 0.0042(10) 0.0060(10) 0.0037(10) C68 0.0143(12) 0.0231(12) 0.0320(14) -0.0054(11) 0.0038(10) -0.0021(10) C69 0.0188(12) 0.0157(11) 0.0195(12) 0.0054(9) 0.0058(9) 0.0009(9) C70 0.0365(14) 0.0212(13) 0.0272(13) 0.0029(12) 0.0129(11) 0.0053(12) C71 0.0255(14) 0.0213(13) 0.0424(17) 0.0107(12) 0.0020(12) -0.0031(11) C72 0.0260(14) 0.0146(12) 0.0236(14) 0.0055(10) 0.0084(11) 0.0038(10) C1S 0.092(3) 0.056(3) 0.048(2) 0.0020(19) 0.021(2) 0.015(2) C2S 0.089(3) 0.050(2) 0.041(2) 0.0039(17) -0.001(2) 0.003(2) C3S 0.088(3) 0.0393(18) 0.0345(17) -0.0062(17) -0.0219(18) 0.002(2) C4S 0.077(3) 0.063(2) 0.042(2) -0.010(2) -0.0072(19) -0.011(3) C5S 0.099(4) 0.068(3) 0.092(4) -0.036(3) -0.046(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O3 2.2611(17) . ? Ce1 O4 2.2737(16) . ? Ce1 O1 2.4343(16) . ? Ce1 O2 2.4570(16) . ? Ce1 N2 2.550(2) . ? Ce1 N1 2.6291(19) . ? Ce1 Ce2 3.7130(5) . ? Ce2 O5 2.2864(16) . ? Ce2 O6 2.2928(16) . ? Ce2 O2 2.3898(17) . ? Ce2 O1 2.4305(17) . ? Ce2 N3 2.5834(19) . ? Ce2 N4 2.6418(19) . ? N1 C15 1.282(3) . ? N1 C16 1.484(3) . ? N2 C18 1.286(3) . ? N2 C17 1.466(3) . ? N3 C39 1.278(3) . ? N3 C48 1.467(3) . ? N4 C50 1.290(3) . ? N4 C49 1.482(3) . ? O1 C69 1.432(3) . ? O2 C65 1.431(3) . ? O3 C1 1.321(3) . ? O4 C20 1.321(3) . ? O5 C33 1.319(3) . ? O6 C52 1.325(3) . ? C1 C2 1.417(3) . ? C1 C6 1.435(3) . ? C2 C3 1.408(3) . ? C2 C15 1.454(3) . ? C3 C4 1.379(3) . ? C3 H3A 0.9500 . ? C4 C5 1.399(3) . ? C4 C11 1.532(3) . ? C5 C6 1.393(3) . ? C5 H5A 0.9500 . ? C6 C7 1.544(3) . ? C7 C9 1.539(4) . ? C7 C8 1.541(4) . ? C7 C10 1.545(4) . ? 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 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.528(4) . ? C11 C12 1.530(4) . ? C11 C13 1.546(4) . ? 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 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9500 . ? C16 C17 1.529(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.455(3) . ? C18 H18A 0.9500 . ? C19 C24 1.404(3) . ? C19 C20 1.418(3) . ? C20 C21 1.432(3) . ? C21 C22 1.395(3) . ? C21 C25 1.529(3) . ? C22 C23 1.396(4) . ? C22 H22A 0.9500 . ? C23 C24 1.379(4) . ? C23 C29 1.537(4) . ? C24 H24A 0.9500 . ? C25 C27 1.541(4) . ? C25 C28 1.543(4) . ? C25 C26 1.543(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.523(4) . ? C29 C32 1.534(4) . ? C29 C31 1.546(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C38 1.423(3) . ? C33 C34 1.430(3) . ? C34 C35 1.399(3) . ? C34 C40 1.529(3) . ? C35 C36 1.394(3) . ? C35 H35A 0.9500 . ? C36 C37 1.380(3) . ? C36 C44 1.539(3) . ? C37 C38 1.405(3) . ? C37 H37A 0.9500 . ? C38 C39 1.447(3) . ? C39 H39A 0.9500 . ? C40 C41 1.536(3) . ? C40 C42 1.536(3) . ? C40 C43 1.545(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.529(3) . ? C44 C46 1.535(4) . ? C44 C47 1.546(4) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.515(3) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.459(3) . ? C50 H50A 0.9500 . ? C51 C56 1.409(3) . ? C51 C52 1.423(3) . ? C52 C53 1.429(3) . ? C53 C54 1.385(3) . ? C53 C57 1.539(3) . ? C54 C55 1.404(3) . ? C54 H54A 0.9500 . ? C55 C56 1.377(3) . ? C55 C61 1.533(3) . ? C56 H56A 0.9500 . ? C57 C58 1.532(3) . ? C57 C59 1.535(3) . ? C57 C60 1.542(3) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C64 1.532(4) . ? C61 C63 1.533(4) . ? C61 C62 1.539(4) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.525(3) . ? C65 C67 1.527(3) . ? C65 C68 1.530(3) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C72 1.524(3) . ? C69 C71 1.529(4) . ? C69 C70 1.532(3) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C1S C2S 1.474(6) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S C3S 1.509(5) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S C4S 1.496(6) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S C5S 1.498(6) . ? C4S H4SA 0.9900 . ? C4S H4SB 0.9900 . ? C5S H5SA 0.9800 . ? C5S H5SB 0.9800 . ? C5S H5SC 0.9800 . ? O1S C8S 1.531(12) . ? O1S C7S 1.641(11) . ? C6S C7S 1.360(8) . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 0.9800 . ? C7S H7SA 0.9900 . ? C7S H7SB 0.9900 . ? C8S C9S 1.436(10) . ? C8S H8SA 0.9900 . ? C8S H8SB 0.9900 . ? C9S H9SA 0.9800 . ? C9S H9SB 0.9800 . ? C9S H9SC 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ce1 O4 106.15(6) . . ? O3 Ce1 O1 113.92(6) . . ? O4 Ce1 O1 139.91(6) . . ? O3 Ce1 O2 121.74(6) . . ? O4 Ce1 O2 88.97(6) . . ? O1 Ce1 O2 71.39(5) . . ? O3 Ce1 N2 130.13(6) . . ? O4 Ce1 N2 70.09(6) . . ? O1 Ce1 N2 82.97(6) . . ? O2 Ce1 N2 108.05(6) . . ? O3 Ce1 N1 71.06(6) . . ? O4 Ce1 N1 104.45(6) . . ? O1 Ce1 N1 87.82(6) . . ? O2 Ce1 N1 158.54(6) . . ? N2 Ce1 N1 62.77(6) . . ? O3 Ce1 Ce2 143.73(4) . . ? O4 Ce1 Ce2 103.98(5) . . ? O1 Ce1 Ce2 40.21(4) . . ? O2 Ce1 Ce2 39.34(4) . . ? N2 Ce1 Ce2 79.30(4) . . ? N1 Ce1 Ce2 119.77(4) . . ? O5 Ce2 O6 114.27(6) . . ? O5 Ce2 O2 134.60(5) . . ? O6 Ce2 O2 111.05(6) . . ? O5 Ce2 O1 90.35(5) . . ? O6 Ce2 O1 115.16(5) . . ? O2 Ce2 O1 72.60(5) . . ? O5 Ce2 N3 69.35(6) . . ? O6 Ce2 N3 131.10(6) . . ? O2 Ce2 N3 79.36(6) . . ? O1 Ce2 N3 113.52(6) . . ? O5 Ce2 N4 109.08(6) . . ? O6 Ce2 N4 71.01(6) . . ? O2 Ce2 N4 83.06(6) . . ? O1 Ce2 N4 155.52(6) . . ? N3 Ce2 N4 62.85(6) . . ? O5 Ce2 Ce1 100.84(4) . . ? O6 Ce2 Ce1 138.38(4) . . ? O2 Ce2 Ce1 40.67(4) . . ? O1 Ce2 Ce1 40.29(4) . . ? N3 Ce2 Ce1 80.98(4) . . ? N4 Ce2 Ce1 118.68(4) . . ? C15 N1 C16 114.80(19) . . ? C15 N1 Ce1 127.48(15) . . ? C16 N1 Ce1 117.21(13) . . ? C18 N2 C17 117.7(2) . . ? C18 N2 Ce1 131.72(16) . . ? C17 N2 Ce1 109.83(14) . . ? C39 N3 C48 116.7(2) . . ? C39 N3 Ce2 131.61(16) . . ? C48 N3 Ce2 110.71(13) . . ? C50 N4 C49 114.33(19) . . ? C50 N4 Ce2 128.09(16) . . ? C49 N4 Ce2 117.47(13) . . ? C69 O1 Ce2 126.31(13) . . ? C69 O1 Ce1 128.66(14) . . ? Ce2 O1 Ce1 99.50(6) . . ? C65 O2 Ce2 128.90(13) . . ? C65 O2 Ce1 121.25(13) . . ? Ce2 O2 Ce1 99.99(6) . . ? C1 O3 Ce1 145.87(15) . . ? C20 O4 Ce1 145.50(15) . . ? C33 O5 Ce2 146.82(15) . . ? C52 O6 Ce2 146.41(14) . . ? O3 C1 C2 120.8(2) . . ? O3 C1 C6 121.1(2) . . ? C2 C1 C6 118.2(2) . . ? C3 C2 C1 120.2(2) . . ? C3 C2 C15 115.6(2) . . ? C1 C2 C15 124.2(2) . . ? C4 C3 C2 122.7(2) . . ? C4 C3 H3A 118.6 . . ? C2 C3 H3A 118.6 . . ? C3 C4 C5 116.2(2) . . ? C3 C4 C11 120.5(2) . . ? C5 C4 C11 123.3(2) . . ? C6 C5 C4 124.8(2) . . ? C6 C5 H5A 117.6 . . ? C4 C5 H5A 117.6 . . ? C5 C6 C1 118.0(2) . . ? C5 C6 C7 121.6(2) . . ? C1 C6 C7 120.4(2) . . ? C9 C7 C8 106.6(2) . . ? C9 C7 C6 112.0(2) . . ? C8 C7 C6 110.9(2) . . ? C9 C7 C10 108.0(2) . . ? C8 C7 C10 110.2(2) . . ? C6 C7 C10 109.0(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 109.0(2) . . ? C14 C11 C4 112.6(2) . . ? C12 C11 C4 109.6(2) . . ? C14 C11 C13 106.9(2) . . ? C12 C11 C13 108.9(3) . . ? C4 C11 C13 109.8(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C2 129.3(2) . . ? N1 C15 H15A 115.4 . . ? C2 C15 H15A 115.4 . . ? N1 C16 C17 110.32(18) . . ? N1 C16 H16A 109.6 . . ? C17 C16 H16A 109.6 . . ? N1 C16 H16B 109.6 . . ? C17 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? N2 C17 C16 107.81(18) . . ? N2 C17 H17A 110.1 . . ? C16 C17 H17A 110.1 . . ? N2 C17 H17B 110.1 . . ? C16 C17 H17B 110.1 . . ? H17A C17 H17B 108.5 . . ? N2 C18 C19 126.9(2) . . ? N2 C18 H18A 116.5 . . ? C19 C18 H18A 116.5 . . ? C24 C19 C20 120.9(2) . . ? C24 C19 C18 115.9(2) . . ? C20 C19 C18 123.1(2) . . ? O4 C20 C19 120.6(2) . . ? O4 C20 C21 121.7(2) . . ? C19 C20 C21 117.7(2) . . ? C22 C21 C20 118.0(2) . . ? C22 C21 C25 121.4(2) . . ? C20 C21 C25 120.6(2) . . ? C21 C22 C23 124.6(2) . . ? C21 C22 H22A 117.7 . . ? C23 C22 H22A 117.7 . . ? C24 C23 C22 116.5(2) . . ? C24 C23 C29 119.9(2) . . ? C22 C23 C29 123.6(2) . . ? C23 C24 C19 122.1(2) . . ? C23 C24 H24A 119.0 . . ? C19 C24 H24A 119.0 . . ? C21 C25 C27 109.8(2) . . ? C21 C25 C28 113.0(2) . . ? C27 C25 C28 107.2(2) . . ? C21 C25 C26 110.0(2) . . ? C27 C25 C26 109.6(2) . . ? C28 C25 C26 107.1(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C32 108.7(2) . . ? C30 C29 C23 109.6(2) . . ? C32 C29 C23 112.6(2) . . ? C30 C29 C31 109.0(3) . . ? C32 C29 C31 107.7(2) . . ? C23 C29 C31 109.2(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O5 C33 C38 119.9(2) . . ? O5 C33 C34 121.9(2) . . ? C38 C33 C34 118.2(2) . . ? C35 C34 C33 117.7(2) . . ? C35 C34 C40 121.6(2) . . ? C33 C34 C40 120.6(2) . . ? C36 C35 C34 124.9(2) . . ? C36 C35 H35A 117.5 . . ? C34 C35 H35A 117.5 . . ? C37 C36 C35 116.4(2) . . ? C37 C36 C44 120.3(2) . . ? C35 C36 C44 123.3(2) . . ? C36 C37 C38 122.4(2) . . ? C36 C37 H37A 118.8 . . ? C38 C37 H37A 118.8 . . ? C37 C38 C33 120.4(2) . . ? C37 C38 C39 116.1(2) . . ? C33 C38 C39 123.5(2) . . ? N3 C39 C38 127.4(2) . . ? N3 C39 H39A 116.3 . . ? C38 C39 H39A 116.3 . . ? C34 C40 C41 109.96(19) . . ? C34 C40 C42 110.0(2) . . ? C41 C40 C42 110.1(2) . . ? C34 C40 C43 112.3(2) . . ? C41 C40 C43 107.5(2) . . ? C42 C40 C43 107.0(2) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C46 108.7(2) . . ? C45 C44 C36 112.1(2) . . ? C46 C44 C36 109.8(2) . . ? C45 C44 C47 108.1(2) . . ? C46 C44 C47 109.2(2) . . ? C36 C44 C47 108.8(2) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N3 C48 C49 107.04(19) . . ? N3 C48 H48A 110.3 . . ? C49 C48 H48A 110.3 . . ? N3 C48 H48B 110.3 . . ? C49 C48 H48B 110.3 . . ? H48A C48 H48B 108.6 . . ? N4 C49 C48 110.78(18) . . ? N4 C49 H49A 109.5 . . ? C48 C49 H49A 109.5 . . ? N4 C49 H49B 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 108.1 . . ? N4 C50 C51 129.1(2) . . ? N4 C50 H50A 115.4 . . ? C51 C50 H50A 115.4 . . ? C56 C51 C52 120.6(2) . . ? C56 C51 C50 114.5(2) . . ? C52 C51 C50 124.9(2) . . ? O6 C52 C51 120.3(2) . . ? O6 C52 C53 121.9(2) . . ? C51 C52 C53 117.8(2) . . ? C54 C53 C52 118.2(2) . . ? C54 C53 C57 120.8(2) . . ? C52 C53 C57 120.9(2) . . ? C53 C54 C55 124.7(2) . . ? C53 C54 H54A 117.7 . . ? C55 C54 H54A 117.7 . . ? C56 C55 C54 116.5(2) . . ? C56 C55 C61 123.3(2) . . ? C54 C55 C61 120.2(2) . . ? C55 C56 C51 122.0(2) . . ? C55 C56 H56A 119.0 . . ? C51 C56 H56A 119.0 . . ? C58 C57 C59 106.59(19) . . ? C58 C57 C53 112.6(2) . . ? C59 C57 C53 111.06(19) . . ? C58 C57 C60 106.2(2) . . ? C59 C57 C60 111.3(2) . . ? C53 C57 C60 109.01(19) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C64 C61 C63 108.3(2) . . ? C64 C61 C55 111.6(2) . . ? C63 C61 C55 110.5(2) . . ? C64 C61 C62 108.3(2) . . ? C63 C61 C62 108.9(2) . . ? C55 C61 C62 109.2(2) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O2 C65 C66 109.48(19) . . ? O2 C65 C67 110.83(19) . . ? C66 C65 C67 108.6(2) . . ? O2 C65 C68 108.57(18) . . ? C66 C65 C68 109.9(2) . . ? C67 C65 C68 109.4(2) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O1 C69 C72 111.05(19) . . ? O1 C69 C71 109.22(19) . . ? C72 C69 C71 109.3(2) . . ? O1 C69 C70 108.50(19) . . ? C72 C69 C70 109.1(2) . . ? C71 C69 C70 109.6(2) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C1S C2S C3S 113.8(4) . . ? C1S C2S H2SA 108.8 . . ? C3S C2S H2SA 108.8 . . ? C1S C2S H2SB 108.8 . . ? C3S C2S H2SB 108.8 . . ? H2SA C2S H2SB 107.7 . . ? C4S C3S C2S 114.7(4) . . ? C4S C3S H3SA 108.6 . . ? C2S C3S H3SA 108.6 . . ? C4S C3S H3SB 108.6 . . ? C2S C3S H3SB 108.6 . . ? H3SA C3S H3SB 107.6 . . ? C3S C4S C5S 115.9(4) . . ? C3S C4S H4SA 108.3 . . ? C5S C4S H4SA 108.3 . . ? C3S C4S H4SB 108.3 . . ? C5S C4S H4SB 108.3 . . ? H4SA C4S H4SB 107.4 . . ? C4S C5S H5SA 109.5 . . ? C4S C5S H5SB 109.5 . . ? H5SA C5S H5SB 109.5 . . ? C4S C5S H5SC 109.5 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? C8S O1S C7S 120.9(9) . . ? C7S C6S H6SA 109.5 . . ? C7S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? C7S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? C6S C7S O1S 105.6(8) . . ? C6S C7S H7SA 110.6 . . ? O1S C7S H7SA 110.6 . . ? C6S C7S H7SB 110.6 . . ? O1S C7S H7SB 110.6 . . ? H7SA C7S H7SB 108.7 . . ? C9S C8S O1S 117.1(9) . . ? C9S C8S H8SA 108.0 . . ? O1S C8S H8SA 108.0 . . ? C9S C8S H8SB 108.0 . . ? O1S C8S H8SB 108.0 . . ? H8SA C8S H8SB 107.3 . . ? C8S C9S H9SA 109.5 . . ? C8S C9S H9SB 109.5 . . ? H9SA C9S H9SB 109.5 . . ? C8S C9S H9SC 109.5 . . ? H9SA C9S H9SC 109.5 . . ? H9SB C9S H9SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.770 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.071 #===END