data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'He, Cheng' _publ_contact_author_email hecheng@dlut.edu.cn _publ_section_title ; Symmetry-Controlled and Face-Driven Approach for the Assembly of Cerium-based Molecular Polyhedra ; loop_ _publ_author_name 'Chun-ying Duan' 'Cheng He' # Attachment '- Ce-NATB.cif' data_Ce-NATB _database_code_depnum_ccdc_archive 'CCDC 675065' #TrackingRef '- Ce-NATB.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C194 H208 Ce4 N24 O50' _chemical_formula_weight 4236.32 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 Cubic _symmetry_space_group_name_H-M Fd-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' '-x+1/4, y, -z+1/4' 'x, -y+1/4, -z+1/4' 'z, x, y' 'z, -x+1/4, -y+1/4' '-z+1/4, -x+1/4, y' '-z+1/4, x, -y+1/4' 'y, z, x' '-y+1/4, z, -x+1/4' 'y, -z+1/4, -x+1/4' '-y+1/4, -z+1/4, x' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' '-x+1/4, y+1/2, -z+3/4' 'x, -y+3/4, -z+3/4' 'z, x+1/2, y+1/2' 'z, -x+3/4, -y+3/4' '-z+1/4, -x+3/4, y+1/2' '-z+1/4, x+1/2, -y+3/4' 'y, z+1/2, x+1/2' '-y+1/4, z+1/2, -x+3/4' 'y, -z+3/4, -x+3/4' '-y+1/4, -z+3/4, x+1/2' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' '-x+3/4, y, -z+3/4' 'x+1/2, -y+1/4, -z+3/4' 'z+1/2, x, y+1/2' 'z+1/2, -x+1/4, -y+3/4' '-z+3/4, -x+1/4, y+1/2' '-z+3/4, x, -y+3/4' 'y+1/2, z, x+1/2' '-y+3/4, z, -x+3/4' 'y+1/2, -z+1/4, -x+3/4' '-y+3/4, -z+1/4, x+1/2' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' '-x+3/4, y+1/2, -z+1/4' 'x+1/2, -y+3/4, -z+1/4' 'z+1/2, x+1/2, y' 'z+1/2, -x+3/4, -y+1/4' '-z+3/4, -x+3/4, y' '-z+3/4, x+1/2, -y+1/4' 'y+1/2, z+1/2, x' '-y+3/4, z+1/2, -x+1/4' 'y+1/2, -z+3/4, -x+1/4' '-y+3/4, -z+3/4, x' '-x, -y, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y, z-1/4' '-x, y-1/4, z-1/4' '-z, -x, -y' '-z, x-1/4, y-1/4' 'z-1/4, x-1/4, -y' 'z-1/4, -x, y-1/4' '-y, -z, -x' 'y-1/4, -z, x-1/4' '-y, z-1/4, x-1/4' 'y-1/4, z-1/4, -x' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' 'x-1/4, -y+1/2, z+1/4' '-x, y+1/4, z+1/4' '-z, -x+1/2, -y+1/2' '-z, x+1/4, y+1/4' 'z-1/4, x+1/4, -y+1/2' 'z-1/4, -x+1/2, y+1/4' '-y, -z+1/2, -x+1/2' 'y-1/4, -z+1/2, x+1/4' '-y, z+1/4, x+1/4' 'y-1/4, z+1/4, -x+1/2' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' 'x+1/4, -y, z+1/4' '-x+1/2, y-1/4, z+1/4' '-z+1/2, -x, -y+1/2' '-z+1/2, x-1/4, y+1/4' 'z+1/4, x-1/4, -y+1/2' 'z+1/4, -x, y+1/4' '-y+1/2, -z, -x+1/2' 'y+1/4, -z, x+1/4' '-y+1/2, z-1/4, x+1/4' 'y+1/4, z-1/4, -x+1/2' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' 'x+1/4, -y+1/2, z-1/4' '-x+1/2, y+1/4, z-1/4' '-z+1/2, -x+1/2, -y' '-z+1/2, x+1/4, y-1/4' 'z+1/4, x+1/4, -y' 'z+1/4, -x+1/2, y-1/4' '-y+1/2, -z+1/2, -x' 'y+1/4, -z+1/2, x-1/4' '-y+1/2, z+1/4, x-1/4' 'y+1/4, z+1/4, -x' _cell_length_a 35.1092(2) _cell_length_b 35.1092(2) _cell_length_c 35.1092(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 43277.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description bolck _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 17376 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 47136 _diffrn_reflns_av_R_equivalents 0.1002 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3561 _reflns_number_gt 2442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1050P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3561 _refine_ls_number_parameters 216 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1525 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.275096(7) 0.775096(7) 0.275096(7) 0.0298(2) Uani 1 3 d S . . O1 O 0.21590(9) 0.78433(10) 0.25341(10) 0.0368(8) Uani 1 1 d . . . O2 O 0.29793(9) 0.77452(9) 0.34094(9) 0.0326(8) Uani 1 1 d . . . N1 N 0.22584(11) 0.78035(11) 0.32901(11) 0.0302(9) Uani 1 1 d . . . N2 N 0.24054(11) 0.79299(12) 0.36381(11) 0.0340(9) Uani 1 1 d . . . H2A H 0.2266 0.8023 0.3817 0.041 Uiso 0.67 1 calc PR . . C11 C 0.19010(14) 0.77263(13) 0.32890(14) 0.0331(11) Uani 1 1 d . . . H11A H 0.1767 0.7756 0.3516 0.040 Uiso 1 1 calc R . . C1 C 0.16931(14) 0.75958(15) 0.29588(14) 0.0340(11) Uani 1 1 d . . . C2 C 0.18359(14) 0.76692(14) 0.25993(15) 0.0335(11) Uani 1 1 d . . . C3 C 0.16221(15) 0.75478(17) 0.22712(15) 0.0444(14) Uani 1 1 d . . . H3A H 0.1717 0.7590 0.2027 0.053 Uiso 1 1 calc R . . C4 C 0.12814(18) 0.73715(18) 0.23202(18) 0.0562(16) Uani 1 1 d . . . H4A H 0.1145 0.7296 0.2106 0.067 Uiso 1 1 calc R . . C5 C 0.07725(17) 0.71096(19) 0.2721(2) 0.0580(17) Uani 1 1 d . . . H5A H 0.0639 0.7038 0.2503 0.070 Uiso 1 1 calc R . . C6 C 0.06217(19) 0.70297(19) 0.3070(2) 0.0624(18) Uani 1 1 d . . . H6A H 0.0388 0.6908 0.3092 0.075 Uiso 1 1 calc R . . C7 C 0.08269(17) 0.71353(19) 0.3392(2) 0.0591(17) Uani 1 1 d . . . H7A H 0.0727 0.7085 0.3632 0.071 Uiso 1 1 calc R . . C8 C 0.11748(16) 0.73129(16) 0.33607(18) 0.0505(15) Uani 1 1 d . . . H8A H 0.1309 0.7372 0.3581 0.061 Uiso 1 1 calc R . . C9 C 0.11272(16) 0.72988(16) 0.26813(16) 0.0447(14) Uani 1 1 d . . . C10 C 0.13341(14) 0.74083(14) 0.30046(15) 0.0366(12) Uani 1 1 d . . . C12 C 0.27798(14) 0.78925(13) 0.36660(13) 0.0303(11) Uani 1 1 d . . . C13 C 0.29655(13) 0.80266(14) 0.40228(13) 0.0308(11) Uani 1 1 d . . . C14 C 0.28355(13) 0.83499(13) 0.42140(13) 0.0307(11) Uani 1 1 d . . . H14A H 0.2621 0.8479 0.4127 0.037 Uiso 1 1 calc R . . O3 O 0.1853(13) 0.8723(14) 0.4139(4) 0.126(12) Uiso 0.17 1 d PDU . 2 C15 C 0.1819(13) 0.8750 0.3750 0.115(13) Uiso 0.33 2 d SPDU . 2 C15' C 0.1899(6) 0.8014(5) 0.4252(6) 0.114(6) Uiso 0.50 1 d PDU A 1 O3' O 0.1895(3) 0.8360(3) 0.4070(3) 0.075(3) Uiso 0.50 1 d PDU A 1 O4 O -0.0467(5) 0.8666(6) 0.3834(6) 0.103(6) Uiso 0.33 1 d PDU . 1 C16 C -0.0096(6) 0.8750 0.3750 0.135(8) Uiso 0.67 2 d SPDU . 1 O7 O -0.0839(4) 0.9161(4) 0.4161(4) 0.116(7) Uiso 0.50 3 d SPDU B 2 C19 C -0.0573(12) 0.8955(15) 0.3961(15) 0.096(13) Uiso 0.17 1 d PDU B 2 C17 C 0.1023(5) 0.8032(5) 0.4134(5) 0.131(6) Uiso 0.67 1 d PDU . . O5 O 0.1073(4) 0.7732(4) 0.4384(4) 0.119(4) Uiso 0.50 1 d PDU C 1 O5' O 0.0992(11) 0.8322(9) 0.3873(10) 0.116(12) Uiso 0.17 1 d PDU C 2 O6 O 0.1196(7) 0.7266(7) 0.4427(8) 0.113(8) Uiso 0.25 1 d PDU D 3 C18 C 0.1580(8) 0.7313(10) 0.4359(10) 0.088(9) Uiso 0.25 1 d PDU D 3 C20 C 0.3750 0.8750 0.3750 0.098(9) Uiso 1 12 d SDU . . O8 O 0.3524(2) 0.8976(2) 0.3976(2) 0.096(11) Uiso 0.25 3 d SPDU . . 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 0.0298(2) 0.0298(2) 0.0298(2) -0.00343(11) -0.00343(11) -0.00343(11) O1 0.0323(19) 0.044(2) 0.035(2) 0.0008(16) -0.0037(15) -0.0051(15) O2 0.0324(19) 0.0356(19) 0.0298(18) -0.0062(14) -0.0018(14) 0.0052(15) N1 0.029(2) 0.031(2) 0.031(2) -0.0029(17) -0.0068(17) 0.0001(17) N2 0.031(2) 0.042(2) 0.029(2) -0.0060(18) -0.0047(17) -0.0005(18) C11 0.032(3) 0.035(3) 0.032(3) -0.001(2) -0.004(2) -0.002(2) C1 0.033(3) 0.035(3) 0.035(3) -0.002(2) -0.005(2) -0.002(2) C2 0.026(3) 0.034(3) 0.040(3) -0.002(2) -0.008(2) 0.002(2) C3 0.036(3) 0.061(4) 0.036(3) 0.003(3) -0.009(2) -0.003(3) C4 0.048(4) 0.064(4) 0.056(4) -0.008(3) -0.023(3) -0.015(3) C5 0.042(3) 0.065(4) 0.067(4) 0.001(3) -0.012(3) -0.020(3) C6 0.050(4) 0.060(4) 0.077(5) 0.001(4) 0.001(3) -0.019(3) C7 0.041(4) 0.072(4) 0.064(4) 0.011(3) 0.000(3) -0.014(3) C8 0.037(3) 0.055(4) 0.060(4) 0.007(3) -0.004(3) -0.009(3) C9 0.038(3) 0.048(3) 0.049(3) 0.001(3) -0.009(2) -0.011(2) C10 0.031(3) 0.038(3) 0.041(3) -0.001(2) -0.004(2) 0.000(2) C12 0.038(3) 0.025(2) 0.028(3) 0.0009(19) -0.005(2) -0.001(2) C13 0.027(2) 0.033(3) 0.032(3) -0.005(2) -0.002(2) -0.001(2) C14 0.029(3) 0.032(3) 0.031(3) 0.000(2) -0.005(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O1 2.237(3) . ? Ce1 O1 2.237(3) 17_554 ? Ce1 O1 2.237(3) 45_455 ? Ce1 O2 2.447(3) 17_554 ? Ce1 O2 2.447(3) 45_455 ? Ce1 O2 2.447(3) . ? Ce1 N1 2.570(4) 17_554 ? Ce1 N1 2.570(4) . ? Ce1 N1 2.570(4) 45_455 ? O1 C2 1.309(6) . ? O2 C12 1.253(6) . ? N1 C11 1.284(6) . ? N1 N2 1.399(5) . ? N2 C12 1.325(6) . ? C11 C1 1.444(7) . ? C1 C2 1.383(7) . ? C1 C10 1.431(7) . ? C2 C3 1.439(7) . ? C3 C4 1.358(8) . ? C4 C9 1.402(8) . ? C5 C6 1.364(9) . ? C5 C9 1.418(8) . ? C6 C7 1.392(9) . ? C7 C8 1.376(8) . ? C8 C10 1.410(8) . ? C9 C10 1.401(7) . ? C12 C13 1.489(6) . ? C13 C14 1.384(6) 44_556 ? C13 C14 1.395(6) . ? C14 C13 1.384(6) 35_465 ? O3 C15 1.376(13) . ? C15 O3 1.376(13) 16_565 ? C15' O3' 1.373(12) . ? O4 O4 0.84(3) 16_565 ? O4 C16 1.369(12) . ? C16 O4 1.369(12) 16_565 ? O7 C19 1.375(13) 21_455 ? O7 C19 1.375(13) . ? O7 C19 1.375(13) 29_464 ? C17 O5' 1.375(13) . ? C17 O5 1.382(12) . ? O6 C18 1.379(13) . ? C20 O8 1.373(13) 38_565 ? C20 O8 1.373(13) 27 ? C20 O8 1.373(13) . ? C20 O8 1.373(13) 16_565 ? 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 O1 Ce1 O1 82.41(14) . 17_554 ? O1 Ce1 O1 82.41(13) . 45_455 ? O1 Ce1 O1 82.41(14) 17_554 45_455 ? O1 Ce1 O2 145.84(12) . 17_554 ? O1 Ce1 O2 128.83(12) 17_554 17_554 ? O1 Ce1 O2 88.10(12) 45_455 17_554 ? O1 Ce1 O2 88.10(12) . 45_455 ? O1 Ce1 O2 145.84(12) 17_554 45_455 ? O1 Ce1 O2 128.83(12) 45_455 45_455 ? O2 Ce1 O2 72.60(12) 17_554 45_455 ? O1 Ce1 O2 128.83(12) . . ? O1 Ce1 O2 88.10(12) 17_554 . ? O1 Ce1 O2 145.84(12) 45_455 . ? O2 Ce1 O2 72.60(12) 17_554 . ? O2 Ce1 O2 72.60(12) 45_455 . ? O1 Ce1 N1 143.71(13) . 17_554 ? O1 Ce1 N1 67.37(12) 17_554 17_554 ? O1 Ce1 N1 74.39(13) 45_455 17_554 ? O2 Ce1 N1 61.66(11) 17_554 17_554 ? O2 Ce1 N1 128.19(12) 45_455 17_554 ? O2 Ce1 N1 71.67(11) . 17_554 ? O1 Ce1 N1 67.37(12) . . ? O1 Ce1 N1 74.39(13) 17_554 . ? O1 Ce1 N1 143.71(13) 45_455 . ? O2 Ce1 N1 128.19(12) 17_554 . ? O2 Ce1 N1 71.67(11) 45_455 . ? O2 Ce1 N1 61.66(11) . . ? N1 Ce1 N1 119.40(2) 17_554 . ? O1 Ce1 N1 74.39(13) . 45_455 ? O1 Ce1 N1 143.71(13) 17_554 45_455 ? O1 Ce1 N1 67.37(12) 45_455 45_455 ? O2 Ce1 N1 71.67(11) 17_554 45_455 ? O2 Ce1 N1 61.66(11) 45_455 45_455 ? O2 Ce1 N1 128.19(12) . 45_455 ? N1 Ce1 N1 119.40(2) 17_554 45_455 ? N1 Ce1 N1 119.40(2) . 45_455 ? C2 O1 Ce1 132.7(3) . . ? C12 O2 Ce1 119.5(3) . . ? C11 N1 N2 115.5(4) . . ? C11 N1 Ce1 129.8(3) . . ? N2 N1 Ce1 114.7(3) . . ? C12 N2 N1 113.5(4) . . ? N1 C11 C1 124.3(5) . . ? C2 C1 C10 120.5(4) . . ? C2 C1 C11 119.4(4) . . ? C10 C1 C11 120.1(5) . . ? O1 C2 C1 124.1(5) . . ? O1 C2 C3 116.8(5) . . ? C1 C2 C3 119.1(5) . . ? C4 C3 C2 119.5(5) . . ? C3 C4 C9 122.5(5) . . ? C6 C5 C9 121.7(6) . . ? C5 C6 C7 118.3(6) . . ? C8 C7 C6 121.0(6) . . ? C7 C8 C10 122.1(6) . . ? C10 C9 C4 118.8(5) . . ? C10 C9 C5 120.3(5) . . ? C4 C9 C5 120.9(5) . . ? C9 C10 C8 116.6(5) . . ? C9 C10 C1 119.5(5) . . ? C8 C10 C1 123.9(5) . . ? O2 C12 N2 122.8(4) . . ? O2 C12 C13 119.4(4) . . ? N2 C12 C13 117.7(4) . . ? C14 C13 C14 120.3(5) 44_556 . ? C14 C13 C12 118.3(4) 44_556 . ? C14 C13 C12 121.3(4) . . ? C13 C14 C13 119.7(5) 35_465 . ? O3 C15 O3 170(6) . 16_565 ? O4 O4 C16 72.2(7) 16_565 . ? O4 C16 O4 35.5(15) . 16_565 ? C19 O7 C19 115.9(18) 21_455 . ? C19 O7 C19 115.9(18) 21_455 29_464 ? C19 O7 C19 115.9(18) . 29_464 ? O5' C17 O5 176(3) . . ? O8 C20 O8 109.472(8) 38_565 27 ? O8 C20 O8 109.5 38_565 . ? O8 C20 O8 109.471(2) 27 . ? O8 C20 O8 109.471(3) 38_565 16_565 ? O8 C20 O8 109.471(1) 27 16_565 ? O8 C20 O8 109.471(1) . 16_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.878 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.123 # Attachment '- Ce-NATB-Cl.cif' data_cl1 _database_code_depnum_ccdc_archive 'CCDC 675068' #TrackingRef '- Ce-NATB-Cl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C181 H160 Ce4 Cl4 N24 O39' _chemical_formula_weight 3997.61 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.496(13) _cell_length_b 18.588(13) _cell_length_c 30.52(2) _cell_angle_alpha 104.616(13) _cell_angle_beta 102.949(13) _cell_angle_gamma 91.295(14) _cell_volume 9861(12) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4052 _exptl_absorpt_coefficient_mu 1.035 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7134 _exptl_absorpt_correction_T_max 0.8197 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 38254 _diffrn_reflns_av_R_equivalents 0.2134 _diffrn_reflns_av_sigmaI/netI 0.6412 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 24.00 _reflns_number_total 28428 _reflns_number_gt 5382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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 [0.00000+1.00000exp(2.50(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0000P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28428 _refine_ls_number_parameters 1927 _refine_ls_number_restraints 3918 _refine_ls_R_factor_all 0.4078 _refine_ls_R_factor_gt 0.1486 _refine_ls_wR_factor_ref 0.3337 _refine_ls_wR_factor_gt 0.2761 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 0.962 _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 Ce1 Ce -0.08744(7) -1.18886(7) -0.41321(5) 0.0728(5) Uani 1 1 d . . . Ce2 Ce 0.46087(7) -1.16265(8) -0.31633(6) 0.0783(6) Uani 1 1 d . . . Ce3 Ce 0.18955(7) -0.91273(7) -0.08786(5) 0.0765(5) Uani 1 1 d . . . Ce4 Ce 0.15802(8) -1.45945(8) -0.18731(6) 0.0850(6) Uani 1 1 d . . . O1 O 0.1048(7) -1.3439(6) -0.1796(5) 0.072(4) Uani 1 1 d DU . . O2 O 0.1050(6) -1.5695(7) -0.2272(5) 0.086(4) Uani 1 1 d DU . . O3 O 0.1008(7) -1.0078(6) -0.1477(4) 0.067(3) Uani 1 1 d DU . . O4 O 0.2333(7) -0.9099(7) -0.0153(4) 0.063(3) Uani 1 1 d DU . . O5 O -0.0778(7) -1.2181(6) -0.3412(4) 0.057(3) Uani 1 1 d DU . . O6 O -0.1384(6) -1.0964(7) -0.4367(5) 0.072(3) Uani 1 1 d DU . . O11 O 0.4359(7) -1.1486(7) -0.2485(5) 0.071(3) Uani 1 1 d DU . . O12 O 0.5153(7) -1.2517(6) -0.3507(6) 0.094(4) Uani 1 1 d DU . . O13 O 0.2442(6) -1.0293(7) -0.1034(5) 0.064(4) Uani 1 1 d DU . . O14 O 0.2422(6) -0.8022(7) -0.0694(5) 0.082(4) Uani 1 1 d DU . . O15 O 0.2530(8) -1.3607(7) -0.1813(5) 0.079(4) Uani 1 1 d DU . . O16 O 0.1133(10) -1.4758(7) -0.1327(4) 0.097(4) Uani 1 1 d DU . . O21 O 0.3604(6) -1.2561(7) -0.3240(4) 0.070(3) Uani 1 1 d DU . . O22 O 0.4747(6) -1.1141(8) -0.3709(3) 0.072(4) Uani 1 1 d DU . . O23 O 0.1386(7) -1.4340(7) -0.2590(5) 0.073(3) Uani 1 1 d DU . . O24 O 0.2423(6) -1.5132(8) -0.1560(6) 0.113(4) Uani 1 1 d DU . . O25 O 0.0260(7) -1.2427(6) -0.3983(5) 0.067(4) Uani 1 1 d DU . . O26 O -0.2011(7) -1.2389(6) -0.4296(5) 0.080(4) Uani 1 1 d DU . . O31 O 0.0072(6) -1.0963(7) -0.3534(4) 0.061(3) Uani 1 1 d DU . . O32 O -0.0912(7) -1.2291(7) -0.4851(4) 0.062(3) Uani 1 1 d DU . . O33 O 0.2190(7) -0.9249(7) -0.1606(4) 0.066(3) Uani 1 1 d DU . . O34 O 0.0985(7) -0.8610(7) -0.0628(5) 0.080(3) Uani 1 1 d DU . . O35 O 0.3453(7) -1.1076(6) -0.3267(5) 0.070(4) Uani 1 1 d DU . . O36 O 0.5735(7) -1.1113(6) -0.2788(5) 0.087(4) Uani 1 1 d DU . . N1 N -0.0057(10) -1.3957(9) -0.2326(6) 0.075(4) Uani 1 1 d U . . H1A H -0.0476 -1.3937 -0.2512 0.090 Uiso 1 1 calc R . . N2 N 0.0199(10) -1.4588(10) -0.2253(7) 0.079(4) Uani 1 1 d U . . N3 N 0.0837(9) -1.0773(9) -0.1001(6) 0.064(4) Uani 1 1 d U . . N4 N 0.1230(9) -1.0149(8) -0.0620(6) 0.055(3) Uani 1 1 d U . . N5 N -0.1055(8) -1.1056(9) -0.3057(6) 0.051(3) Uani 1 1 d U . . H5A H -0.1137 -1.0744 -0.2816 0.061 Uiso 1 1 calc R . . N6 N -0.1292(9) -1.0949(9) -0.3479(6) 0.060(4) Uani 1 1 d U . . N11 N 0.4639(9) -1.2486(9) -0.2316(6) 0.072(4) Uani 1 1 d U . . H11G H 0.4691 -1.2802 -0.2150 0.087 Uiso 1 1 calc R . . N12 N 0.4945(10) -1.2588(11) -0.2711(7) 0.085(4) Uani 1 1 d U . . N13 N 0.3560(9) -0.9719(9) -0.1010(6) 0.075(4) Uani 1 1 d U . . H13F H 0.3993 -0.9737 -0.1069 0.090 Uiso 1 1 calc R . . N14 N 0.3336(10) -0.9080(10) -0.0790(6) 0.074(4) Uani 1 1 d U . . N15 N 0.2564(9) -1.3059(9) -0.1044(6) 0.065(3) Uani 1 1 d U . . N16 N 0.2140(10) -1.3711(9) -0.1117(7) 0.079(4) Uani 1 1 d U . . N21 N 0.3038(9) -1.2591(9) -0.3988(6) 0.058(3) Uani 1 1 d U . . N22 N 0.3736(8) -1.2201(9) -0.3956(6) 0.066(4) Uani 1 1 d U . . N23 N 0.2487(10) -1.4662(9) -0.2732(7) 0.083(4) Uani 1 1 d U . . H23B H 0.2779 -1.4736 -0.2919 0.100 Uiso 1 1 calc R . . N24 N 0.2658(12) -1.4961(11) -0.2320(8) 0.103(4) Uani 1 1 d U . . N25 N -0.0271(8) -1.3530(9) -0.4018(6) 0.070(4) Uani 1 1 d U . . H25A H -0.0246 -1.3969 -0.3974 0.084 Uiso 1 1 calc R . . N26 N -0.0933(9) -1.3324(9) -0.4209(6) 0.073(4) Uani 1 1 d U . . N31 N 0.0758(9) -1.0878(8) -0.4033(6) 0.060(3) Uani 1 1 d U . . H31A H 0.1158 -1.0713 -0.4088 0.072 Uiso 1 1 calc R . . N32 N 0.0151(9) -1.1249(9) -0.4412(6) 0.067(4) Uani 1 1 d U . . N33 N 0.1078(9) -0.8958(8) -0.1968(6) 0.051(3) Uani 1 1 d U . . N34 N 0.0981(9) -0.8686(9) -0.1507(6) 0.065(4) Uani 1 1 d U . . N35 N 0.3959(9) -1.0011(9) -0.2696(6) 0.074(4) Uani 1 1 d U . . H35B H 0.3917 -0.9585 -0.2515 0.089 Uiso 1 1 calc R . . N36 N 0.4612(10) -1.0238(10) -0.2744(6) 0.082(4) Uani 1 1 d U . . C1 C -0.0256(6) -1.5921(5) -0.2463(4) 0.104(4) Uani 1 1 d GU . . C2 C 0.0453(6) -1.6171(6) -0.2405(5) 0.096(4) Uani 1 1 d GDU . . C3 C 0.0540(5) -1.6930(7) -0.2478(5) 0.102(5) Uani 1 1 d GU . . H3A H 0.1014 -1.7097 -0.2439 0.122 Uiso 1 1 calc R . . C4 C -0.0082(6) -1.7438(5) -0.2607(5) 0.115(5) Uani 1 1 d GU . . H4A H -0.0024 -1.7946 -0.2656 0.138 Uiso 1 1 calc R . . C5 C -0.0791(6) -1.7189(5) -0.2665(4) 0.127(5) Uani 1 1 d GU . . C6 C -0.0878(5) -1.6430(5) -0.2593(3) 0.121(4) Uani 1 1 d GU . . C7 C -0.1587(6) -1.6180(7) -0.2650(5) 0.140(5) Uani 1 1 d GU . . H7A H -0.1646 -1.5673 -0.2602 0.168 Uiso 1 1 calc R . . C8 C -0.2209(5) -1.6689(8) -0.2780(6) 0.151(6) Uani 1 1 d GU . . H8A H -0.2684 -1.6522 -0.2818 0.182 Uiso 1 1 calc R . . C9 C -0.2122(6) -1.7447(8) -0.2852(6) 0.144(6) Uani 1 1 d GU . . H9A H -0.2538 -1.7788 -0.2939 0.173 Uiso 1 1 calc R . . C10 C -0.1413(7) -1.7697(6) -0.2795(5) 0.140(5) Uani 1 1 d GU . . H10A H -0.1355 -1.8205 -0.2843 0.168 Uiso 1 1 calc R . . C11 C -0.0348(14) -1.5136(12) -0.2435(9) 0.098(5) Uani 1 1 d U . . H11A H -0.0821 -1.5007 -0.2552 0.118 Uiso 1 1 calc R . . C12 C 0.0429(9) -1.3322(11) -0.2067(7) 0.066(4) Uani 1 1 d DU . . C13 C 0.0231(6) -1.2604(5) -0.2119(5) 0.065(4) Uani 1 1 d GU . . C14 C 0.0549(7) -1.2000(6) -0.1745(4) 0.067(4) Uani 1 1 d GU . . H14A H 0.0827 -1.2080 -0.1470 0.080 Uiso 1 1 calc R . . C15 C 0.0453(7) -1.1277(5) -0.1783(4) 0.061(4) Uani 1 1 d GU . . C16 C 0.0038(7) -1.1158(5) -0.2194(5) 0.058(4) Uani 1 1 d GU . . H16A H -0.0027 -1.0674 -0.2220 0.070 Uiso 1 1 calc R . . C17 C -0.0280(7) -1.1762(7) -0.2568(4) 0.058(4) Uani 1 1 d GU . . C18 C -0.0184(7) -1.2485(6) -0.2531(4) 0.063(4) Uani 1 1 d GU . . H18A H -0.0397 -1.2889 -0.2781 0.075 Uiso 1 1 calc R . . C19 C 0.0797(11) -1.0688(8) -0.1392(7) 0.059(4) Uani 1 1 d DU . . C20 C 0.1168(11) -1.0232(11) -0.0217(7) 0.062(4) Uani 1 1 d U . . H20A H 0.0890 -1.0642 -0.0198 0.075 Uiso 1 1 calc R . . C21 C 0.1553(5) -0.9657(5) 0.0208(3) 0.067(4) Uani 1 1 d GU . . C22 C 0.2116(6) -0.9137(6) 0.0223(3) 0.068(4) Uani 1 1 d GDU . . C23 C 0.2502(6) -0.8671(6) 0.0648(4) 0.080(5) Uani 1 1 d GU . . H23A H 0.2878 -0.8323 0.0658 0.096 Uiso 1 1 calc R . . C24 C 0.2325(5) -0.8726(5) 0.1058(3) 0.085(5) Uani 1 1 d GU . . H24A H 0.2583 -0.8414 0.1342 0.102 Uiso 1 1 calc R . . C25 C 0.1762(4) -0.9246(4) 0.1043(3) 0.079(4) Uani 1 1 d GU . . C26 C 0.1376(4) -0.9712(4) 0.0618(3) 0.073(4) Uani 1 1 d GU . . C27 C 0.0813(5) -1.0232(5) 0.0603(3) 0.076(5) Uani 1 1 d GU . . H27A H 0.0555 -1.0543 0.0319 0.091 Uiso 1 1 calc R . . C28 C 0.0637(6) -1.0287(6) 0.1014(4) 0.078(5) Uani 1 1 d GU . . H28A H 0.0260 -1.0635 0.1004 0.094 Uiso 1 1 calc R . . C29 C 0.1022(7) -0.9821(6) 0.1439(4) 0.086(5) Uani 1 1 d GU . . H29A H 0.0904 -0.9858 0.1713 0.103 Uiso 1 1 calc R . . C30 C 0.1585(6) -0.9301(6) 0.1454(3) 0.085(5) Uani 1 1 d GU . . H30A H 0.1843 -0.8989 0.1738 0.102 Uiso 1 1 calc R . . C31 C -0.0681(10) -1.1667(9) -0.3011(5) 0.046(4) Uani 1 1 d DU . . C32 C -0.1745(12) -1.0477(12) -0.3500(8) 0.064(4) Uani 1 1 d U . . H32A H -0.1854 -1.0231 -0.3219 0.076 Uiso 1 1 calc R . . C33 C -0.2143(6) -1.0248(6) -0.3925(4) 0.075(3) Uani 1 1 d GU . . C34 C -0.1892(6) -1.0484(6) -0.4330(5) 0.074(4) Uani 1 1 d GDU . . C35 C -0.2204(8) -1.0239(8) -0.4720(4) 0.084(4) Uani 1 1 d GU . . H35A H -0.2036 -1.0396 -0.4991 0.101 Uiso 1 1 calc R . . C36 C -0.2768(7) -0.9758(7) -0.4704(4) 0.087(5) Uani 1 1 d GU . . H36A H -0.2978 -0.9594 -0.4964 0.105 Uiso 1 1 calc R . . C37 C -0.3020(5) -0.9522(5) -0.4298(4) 0.087(4) Uani 1 1 d GU . . C38 C -0.2707(5) -0.9767(5) -0.3909(4) 0.081(3) Uani 1 1 d GU . . C39 C -0.2958(7) -0.9531(7) -0.3504(4) 0.088(5) Uani 1 1 d GU . . H39A H -0.2749 -0.9695 -0.3243 0.106 Uiso 1 1 calc R . . C40 C -0.3522(8) -0.9051(7) -0.3488(5) 0.106(6) Uani 1 1 d GU . . H40A H -0.3691 -0.8893 -0.3217 0.127 Uiso 1 1 calc R . . C41 C -0.3835(7) -0.8806(7) -0.3877(6) 0.096(5) Uani 1 1 d GU . . H41A H -0.4213 -0.8484 -0.3867 0.115 Uiso 1 1 calc R . . C42 C -0.3584(6) -0.9041(6) -0.4283(5) 0.094(5) Uani 1 1 d GU . . H42A H -0.3793 -0.8878 -0.4543 0.113 Uiso 1 1 calc R . . C51 C 0.5584(6) -1.3512(6) -0.3219(5) 0.106(4) Uani 1 1 d GU . . C52 C 0.5412(6) -1.3181(6) -0.3587(6) 0.102(5) Uani 1 1 d GDU . . C53 C 0.5614(7) -1.3495(7) -0.4001(5) 0.104(5) Uani 1 1 d GU . . H53A H 0.5499 -1.3274 -0.4247 0.125 Uiso 1 1 calc R . . C54 C 0.5988(7) -1.4140(7) -0.4049(4) 0.108(5) Uani 1 1 d GU . . H54A H 0.6123 -1.4350 -0.4326 0.130 Uiso 1 1 calc R . . C55 C 0.6160(5) -1.4471(6) -0.3682(4) 0.116(5) Uani 1 1 d GU . . C56 C 0.5958(5) -1.4157(6) -0.3267(4) 0.110(4) Uani 1 1 d GU . . C57 C 0.6130(7) -1.4488(8) -0.2900(5) 0.128(5) Uani 1 1 d GU . . H57A H 0.5995 -1.4277 -0.2622 0.153 Uiso 1 1 calc R . . C58 C 0.6504(8) -1.5132(8) -0.2948(6) 0.129(6) Uani 1 1 d GU . . H58A H 0.6620 -1.5354 -0.2702 0.155 Uiso 1 1 calc R . . C59 C 0.6707(8) -1.5447(7) -0.3362(7) 0.131(6) Uani 1 1 d GU . . H59A H 0.6957 -1.5878 -0.3394 0.157 Uiso 1 1 calc R . . C60 C 0.6534(7) -1.5116(6) -0.3729(6) 0.123(5) Uani 1 1 d GU . . H60A H 0.6670 -1.5326 -0.4007 0.147 Uiso 1 1 calc R . . C61 C 0.5248(11) -1.3212(13) -0.2791(9) 0.089(5) Uani 1 1 d U . . H61A H 0.5267 -1.3499 -0.2580 0.107 Uiso 1 1 calc R . . C62 C 0.4287(12) -1.1912(11) -0.2215(6) 0.058(3) Uani 1 1 d DU . . C63 C 0.3884(6) -1.1847(7) -0.1880(4) 0.069(4) Uani 1 1 d GU . . C64 C 0.3765(7) -1.1135(6) -0.1640(5) 0.068(4) Uani 1 1 d GU . . H64A H 0.3995 -1.0719 -0.1685 0.081 Uiso 1 1 calc R . . C65 C 0.3301(7) -1.1046(6) -0.1333(5) 0.061(4) Uani 1 1 d GU . . C66 C 0.2957(6) -1.1668(8) -0.1265(4) 0.066(4) Uani 1 1 d GU . . H66A H 0.2646 -1.1608 -0.1059 0.079 Uiso 1 1 calc R . . C67 C 0.3076(7) -1.2380(6) -0.1505(5) 0.066(4) Uani 1 1 d GU . . C68 C 0.3539(7) -1.2469(6) -0.1813(4) 0.061(4) Uani 1 1 d GU . . H68A H 0.3619 -1.2946 -0.1973 0.074 Uiso 1 1 calc R . . C69 C 0.3098(8) -1.0316(12) -0.1131(7) 0.071(4) Uani 1 1 d DU . . C70 C 0.3804(13) -0.8534(12) -0.0640(7) 0.073(4) Uani 1 1 d U . . H70A H 0.4282 -0.8645 -0.0668 0.087 Uiso 1 1 calc R . . C71 C 0.3744(6) -0.7783(5) -0.0438(4) 0.078(3) Uani 1 1 d GU . . C72 C 0.3021(5) -0.7569(7) -0.0485(4) 0.070(3) Uani 1 1 d GDU . . C73 C 0.2897(5) -0.6840(7) -0.0281(5) 0.074(4) Uani 1 1 d GU . . H73A H 0.2414 -0.6697 -0.0313 0.089 Uiso 1 1 calc R . . C74 C 0.3496(6) -0.6324(6) -0.0031(4) 0.097(5) Uani 1 1 d GU . . H74A H 0.3412 -0.5836 0.0106 0.117 Uiso 1 1 calc R . . C75 C 0.4218(5) -0.6538(5) 0.0016(3) 0.103(4) Uani 1 1 d GU . . C76 C 0.4343(5) -0.7268(5) -0.0187(3) 0.094(4) Uani 1 1 d GU . . C77 C 0.5065(5) -0.7482(7) -0.0140(4) 0.107(5) Uani 1 1 d GU . . H77A H 0.5148 -0.7970 -0.0277 0.129 Uiso 1 1 calc R . . C78 C 0.5664(5) -0.6966(8) 0.0110(5) 0.121(6) Uani 1 1 d GU . . H78A H 0.6147 -0.7109 0.0142 0.145 Uiso 1 1 calc R . . C79 C 0.5539(6) -0.6236(8) 0.0314(5) 0.121(6) Uani 1 1 d GU . . H79A H 0.5940 -0.5891 0.0482 0.145 Uiso 1 1 calc R . . C80 C 0.4817(7) -0.6022(6) 0.0267(4) 0.114(5) Uani 1 1 d GU . . H80A H 0.4733 -0.5534 0.0404 0.137 Uiso 1 1 calc R . . C81 C 0.2696(12) -1.3057(10) -0.1433(6) 0.061(3) Uani 1 1 d DU . . C82 C 0.2226(12) -1.3803(12) -0.0666(9) 0.085(5) Uani 1 1 d U . . H82A H 0.2527 -1.3446 -0.0418 0.102 Uiso 1 1 calc R . . C83 C 0.1859(6) -1.4444(5) -0.0567(3) 0.086(4) Uani 1 1 d GU . . C84 C 0.1259(6) -1.4852(6) -0.0906(3) 0.082(4) Uani 1 1 d GDU . . C85 C 0.0897(6) -1.5456(6) -0.0829(4) 0.087(5) Uani 1 1 d GU . . H85A H 0.0495 -1.5729 -0.1056 0.104 Uiso 1 1 calc R . . C86 C 0.1135(6) -1.5651(5) -0.0412(4) 0.089(5) Uani 1 1 d GU . . H86A H 0.0893 -1.6055 -0.0360 0.107 Uiso 1 1 calc R . . C87 C 0.1736(5) -1.5243(4) -0.0073(3) 0.095(4) Uani 1 1 d GU . . C88 C 0.2098(5) -1.4639(4) -0.0150(3) 0.094(4) Uani 1 1 d GU . . C89 C 0.2699(6) -1.4231(5) 0.0189(4) 0.099(5) Uani 1 1 d GU . . H89A H 0.2941 -1.3827 0.0138 0.119 Uiso 1 1 calc R . . C90 C 0.2937(6) -1.4426(7) 0.0606(4) 0.104(5) Uani 1 1 d GU . . H90A H 0.3339 -1.4153 0.0833 0.125 Uiso 1 1 calc R . . C91 C 0.2575(7) -1.5030(7) 0.0683(3) 0.110(5) Uani 1 1 d GU . . H91A H 0.2735 -1.5160 0.0962 0.132 Uiso 1 1 calc R . . C92 C 0.1975(7) -1.5438(6) 0.0344(4) 0.094(5) Uani 1 1 d GU . . H92A H 0.1732 -1.5841 0.0396 0.113 Uiso 1 1 calc R . . C101 C 0.4478(4) -1.1916(5) -0.4473(3) 0.066(4) Uani 1 1 d GU . . C102 C 0.4876(5) -1.1309(6) -0.4129(3) 0.059(4) Uani 1 1 d GDU . . C103 C 0.5463(5) -1.0927(5) -0.4212(3) 0.069(4) Uani 1 1 d GU . . H10B H 0.5730 -1.0521 -0.3983 0.083 Uiso 1 1 calc R . . C104 C 0.5654(5) -1.1151(5) -0.4639(3) 0.075(5) Uani 1 1 d GU . . H10C H 0.6047 -1.0895 -0.4695 0.090 Uiso 1 1 calc R . . C105 C 0.5256(4) -1.1757(4) -0.4983(3) 0.078(4) Uani 1 1 d GU . . C106 C 0.4668(4) -1.2140(4) -0.4900(3) 0.072(4) Uani 1 1 d GU . . C107 C 0.4270(5) -1.2746(5) -0.5243(3) 0.076(5) Uani 1 1 d GU . . H10D H 0.3877 -1.3002 -0.5188 0.091 Uiso 1 1 calc R . . C108 C 0.4461(6) -1.2971(6) -0.5670(3) 0.090(5) Uani 1 1 d GU . . H10E H 0.4194 -1.3376 -0.5900 0.109 Uiso 1 1 calc R . . C109 C 0.5048(6) -1.2588(7) -0.5753(3) 0.089(5) Uani 1 1 d GU . . H10F H 0.5176 -1.2738 -0.6039 0.107 Uiso 1 1 calc R . . C110 C 0.5446(5) -1.1982(6) -0.5410(3) 0.084(5) Uani 1 1 d GU . . H11B H 0.5839 -1.1726 -0.5465 0.101 Uiso 1 1 calc R . . C111 C 0.3842(11) -1.2256(11) -0.4387(8) 0.065(4) Uani 1 1 d U . . H11C H 0.3480 -1.2531 -0.4641 0.078 Uiso 1 1 calc R . . C112 C 0.3018(9) -1.2700(11) -0.3590(6) 0.054(3) Uani 1 1 d DU . . C113 C 0.2365(5) -1.3059(6) -0.3532(4) 0.064(4) Uani 1 1 d GU . . C114 C 0.2456(6) -1.3512(7) -0.3227(4) 0.063(4) Uani 1 1 d GU . . H11D H 0.2931 -1.3587 -0.3075 0.076 Uiso 1 1 calc R . . C115 C 0.1835(8) -1.3851(7) -0.3151(4) 0.066(4) Uani 1 1 d GU . . C116 C 0.1125(6) -1.3738(7) -0.3379(5) 0.065(4) Uani 1 1 d GU . . H11E H 0.0710 -1.3966 -0.3327 0.078 Uiso 1 1 calc R . . C117 C 0.1034(5) -1.3286(7) -0.3683(5) 0.067(4) Uani 1 1 d GU . . C118 C 0.1655(6) -1.2946(6) -0.3760(4) 0.065(4) Uani 1 1 d GU . . H11F H 0.1594 -1.2643 -0.3964 0.078 Uiso 1 1 calc R . . C119 C 0.1882(11) -1.4272(13) -0.2826(7) 0.075(4) Uani 1 1 d DU . . C120 C 0.3276(16) -1.5321(14) -0.2232(10) 0.117(5) Uani 1 1 d U . . H12A H 0.3584 -1.5412 -0.2439 0.140 Uiso 1 1 calc R . . C121 C 0.3443(7) -1.5550(7) -0.1827(6) 0.127(4) Uani 1 1 d GU . . C122 C 0.3109(6) -1.5344(7) -0.1454(7) 0.127(5) Uani 1 1 d GDU . . C123 C 0.3394(8) -1.5549(8) -0.1045(6) 0.135(5) Uani 1 1 d GU . . H12B H 0.3170 -1.5411 -0.0796 0.162 Uiso 1 1 calc R . . C124 C 0.4013(8) -1.5960(8) -0.1010(5) 0.142(5) Uani 1 1 d GU . . H12C H 0.4204 -1.6097 -0.0737 0.171 Uiso 1 1 calc R . . C125 C 0.4347(6) -1.6166(6) -0.1383(5) 0.144(5) Uani 1 1 d GU . . C126 C 0.4062(6) -1.5961(6) -0.1792(5) 0.139(4) Uani 1 1 d GU . . C127 C 0.4396(9) -1.6167(8) -0.2165(5) 0.146(5) Uani 1 1 d GU . . H12D H 0.4205 -1.6030 -0.2438 0.175 Uiso 1 1 calc R . . C128 C 0.5015(9) -1.6578(9) -0.2130(7) 0.152(6) Uani 1 1 d GU . . H12E H 0.5238 -1.6716 -0.2379 0.182 Uiso 1 1 calc R . . C129 C 0.5300(8) -1.6783(8) -0.1721(8) 0.153(6) Uani 1 1 d GU . . H12F H 0.5714 -1.7058 -0.1698 0.184 Uiso 1 1 calc R . . C130 C 0.4966(7) -1.6577(8) -0.1348(7) 0.154(6) Uani 1 1 d GU . . H13A H 0.5157 -1.6715 -0.1075 0.184 Uiso 1 1 calc R . . C131 C 0.0347(11) -1.3075(8) -0.3893(7) 0.070(4) Uani 1 1 d DU . . C132 C -0.1452(11) -1.3819(12) -0.4363(8) 0.074(4) Uani 1 1 d U . . H13B H -0.1340 -1.4300 -0.4350 0.089 Uiso 1 1 calc R . . C133 C -0.2233(5) -1.3717(6) -0.4566(4) 0.088(4) Uani 1 1 d GU . . C134 C -0.2435(6) -1.2994(5) -0.4542(4) 0.078(4) Uani 1 1 d GDU . . C135 C -0.3149(7) -1.2878(5) -0.4762(5) 0.090(5) Uani 1 1 d GU . . H13C H -0.3284 -1.2394 -0.4746 0.108 Uiso 1 1 calc R . . C136 C -0.3661(5) -1.3483(6) -0.5008(4) 0.090(5) Uani 1 1 d GU . . H13D H -0.4138 -1.3405 -0.5155 0.108 Uiso 1 1 calc R . . C137 C -0.3459(5) -1.4205(5) -0.5032(3) 0.099(4) Uani 1 1 d GU . . C138 C -0.2745(5) -1.4322(5) -0.4812(3) 0.088(4) Uani 1 1 d GU . . C139 C -0.2543(6) -1.5044(5) -0.4836(4) 0.103(5) Uani 1 1 d GU . . H13E H -0.2065 -1.5122 -0.4689 0.123 Uiso 1 1 calc R . . C140 C -0.3054(8) -1.5650(5) -0.5082(5) 0.094(4) Uani 1 1 d GU . . H14B H -0.2919 -1.6133 -0.5098 0.113 Uiso 1 1 calc R . . C141 C -0.3768(7) -1.5533(6) -0.5302(5) 0.106(5) Uani 1 1 d GU . . H14C H -0.4111 -1.5938 -0.5467 0.127 Uiso 1 1 calc R . . C142 C -0.3970(5) -1.4811(6) -0.5278(4) 0.102(5) Uani 1 1 d GU . . H14D H -0.4448 -1.4733 -0.5425 0.123 Uiso 1 1 calc R . . C151 C -0.0334(5) -1.1542(5) -0.5221(3) 0.074(4) Uani 1 1 d GU . . C152 C -0.0854(6) -1.2100(6) -0.5229(3) 0.070(4) Uani 1 1 d GDU . . C153 C -0.1321(6) -1.2496(6) -0.5649(4) 0.080(5) Uani 1 1 d GU . . H15A H -0.1669 -1.2869 -0.5654 0.095 Uiso 1 1 calc R . . C154 C -0.1269(5) -1.2333(6) -0.6062(3) 0.080(5) Uani 1 1 d GU . . H15B H -0.1581 -1.2598 -0.6343 0.096 Uiso 1 1 calc R . . C155 C -0.0749(4) -1.1775(5) -0.6054(3) 0.077(4) Uani 1 1 d GU . . C156 C -0.0282(4) -1.1380(4) -0.5634(3) 0.075(4) Uani 1 1 d GU . . C157 C 0.0238(5) -1.0822(5) -0.5626(4) 0.080(5) Uani 1 1 d GU . . H15C H 0.0551 -1.0558 -0.5345 0.096 Uiso 1 1 calc R . . C158 C 0.0291(7) -1.0660(6) -0.6038(4) 0.085(5) Uani 1 1 d GU . . H15D H 0.0638 -1.0287 -0.6033 0.102 Uiso 1 1 calc R . . C159 C -0.0177(7) -1.1055(7) -0.6459(4) 0.089(5) Uani 1 1 d GU . . H15E H -0.0142 -1.0947 -0.6735 0.107 Uiso 1 1 calc R . . C160 C -0.0697(6) -1.1613(6) -0.6467(3) 0.083(5) Uani 1 1 d GU . . H16B H -0.1009 -1.1878 -0.6748 0.099 Uiso 1 1 calc R . . C161 C 0.0216(11) -1.1178(12) -0.4812(8) 0.067(4) Uani 1 1 d U . . H16C H 0.0620 -1.0891 -0.4832 0.081 Uiso 1 1 calc R . . C162 C 0.0703(8) -1.0795(11) -0.3623(7) 0.050(3) Uani 1 1 d DU . . C163 C 0.1290(6) -1.0476(6) -0.3238(4) 0.058(4) Uani 1 1 d GU . . C164 C 0.1180(5) -1.0040(7) -0.2819(4) 0.055(4) Uani 1 1 d GU . . H16D H 0.0700 -0.9949 -0.2786 0.066 Uiso 1 1 calc R . . C165 C 0.1787(7) -0.9738(7) -0.2450(4) 0.059(4) Uani 1 1 d GU . . C166 C 0.2505(6) -0.9874(7) -0.2499(4) 0.066(4) Uani 1 1 d GU . . H16E H 0.2911 -0.9672 -0.2251 0.080 Uiso 1 1 calc R . . C167 C 0.2615(5) -1.0310(8) -0.2917(5) 0.065(4) Uani 1 1 d GU . . C168 C 0.2008(7) -1.0611(7) -0.3286(4) 0.065(4) Uani 1 1 d GU . . H16F H 0.2082 -1.0903 -0.3566 0.078 Uiso 1 1 calc R . . C169 C 0.1665(10) -0.9290(11) -0.1983(6) 0.053(4) Uani 1 1 d DU . . C170 C 0.0457(12) -0.8225(11) -0.1516(8) 0.068(4) Uani 1 1 d U . . H17A H 0.0211 -0.8131 -0.1794 0.082 Uiso 1 1 calc R . . C171 C 0.0264(6) -0.7854(6) -0.1065(4) 0.078(4) Uani 1 1 d GU . . C172 C 0.0522(6) -0.8082(6) -0.0662(5) 0.073(4) Uani 1 1 d GDU . . C173 C 0.0290(7) -0.7754(8) -0.0259(5) 0.089(5) Uani 1 1 d GU . . H17B H 0.0463 -0.7907 0.0010 0.107 Uiso 1 1 calc R . . C174 C -0.0199(7) -0.7198(7) -0.0260(4) 0.092(5) Uani 1 1 d GU . . H17C H -0.0354 -0.6979 0.0009 0.110 Uiso 1 1 calc R . . C175 C -0.0457(5) -0.6969(5) -0.0663(4) 0.094(4) Uani 1 1 d GU . . C176 C -0.0225(5) -0.7297(5) -0.1066(4) 0.088(4) Uani 1 1 d GU . . C177 C -0.0483(7) -0.7068(7) -0.1469(4) 0.096(5) Uani 1 1 d GU . . H17D H -0.0328 -0.7288 -0.1738 0.116 Uiso 1 1 calc R . . C178 C -0.0972(7) -0.6512(8) -0.1470(5) 0.102(5) Uani 1 1 d GU . . H17E H -0.1145 -0.6359 -0.1739 0.122 Uiso 1 1 calc R . . C179 C -0.1204(7) -0.6184(7) -0.1068(6) 0.105(6) Uani 1 1 d GU . . H17F H -0.1532 -0.5812 -0.1068 0.126 Uiso 1 1 calc R . . C180 C -0.0946(7) -0.6413(6) -0.0664(5) 0.096(5) Uani 1 1 d GU . . H18B H -0.1102 -0.6194 -0.0395 0.115 Uiso 1 1 calc R . . C181 C 0.3343(11) -1.0494(9) -0.2951(7) 0.068(4) Uani 1 1 d DU . . C182 C 0.5142(12) -0.9713(13) -0.2575(8) 0.092(5) Uani 1 1 d U . . H18C H 0.5005 -0.9240 -0.2454 0.111 Uiso 1 1 calc R . . C183 C 0.5936(5) -0.9774(6) -0.2550(4) 0.102(4) Uani 1 1 d GU . . C184 C 0.6177(7) -1.0487(6) -0.2645(4) 0.092(4) Uani 1 1 d GDU . . C185 C 0.6935(7) -1.0583(6) -0.2552(5) 0.082(4) Uani 1 1 d GU . . H18D H 0.7096 -1.1060 -0.2615 0.099 Uiso 1 1 calc R . . C186 C 0.7451(6) -0.9965(7) -0.2364(5) 0.110(5) Uani 1 1 d GU . . H18E H 0.7957 -1.0029 -0.2302 0.133 Uiso 1 1 calc R . . C187 C 0.7210(5) -0.9251(6) -0.2270(4) 0.123(4) Uani 1 1 d GU . . C188 C 0.6452(5) -0.9156(6) -0.2363(3) 0.122(4) Uani 1 1 d GU . . C189 C 0.6211(7) -0.8443(6) -0.2268(5) 0.140(5) Uani 1 1 d GU . . H18F H 0.5704 -0.8379 -0.2330 0.168 Uiso 1 1 calc R . . C190 C 0.6727(9) -0.7825(5) -0.2080(6) 0.157(6) Uani 1 1 d GU . . H19A H 0.6566 -0.7347 -0.2017 0.189 Uiso 1 1 calc R . . C191 C 0.7484(8) -0.7920(6) -0.1987(6) 0.157(6) Uani 1 1 d GU . . H19B H 0.7830 -0.7507 -0.1862 0.189 Uiso 1 1 calc R . . C192 C 0.7726(6) -0.8633(7) -0.2082(5) 0.141(5) Uani 1 1 d GU . . H19C H 0.8232 -0.8697 -0.2020 0.169 Uiso 1 1 calc R . . C201 C -0.196(2) -1.049(2) -0.5978(12) 0.087(12) Uiso 0.67 1 d P . . O201 O -0.1938(10) -0.9701(10) -0.5716(6) 0.046(5) Uiso 0.67 1 d P . . O202 O 0.3483(16) -1.0297(16) -0.4020(10) 0.074(9) Uiso 0.50 1 d P . . C202 C 0.418(3) -0.958(3) -0.3799(19) 0.12(2) Uiso 0.50 1 d P . . O203 O 0.1987(12) -1.2913(12) -0.4785(7) 0.069(7) Uiso 0.67 1 d P . . C203 C 0.183(3) -1.220(3) -0.4861(16) 0.138(18) Uiso 0.67 1 d P . . O204 O 0.183(2) -1.184(2) -0.2539(12) 0.108(12) Uiso 0.50 1 d P . . C204 C 0.158(4) -1.239(4) -0.239(2) 0.14(2) Uiso 0.50 1 d P . . C205 C 0.480(2) -1.374(3) -0.1880(16) 0.068(14) Uiso 0.50 1 d P . . O205 O 0.457(4) -1.420(4) -0.221(2) 0.17(3) Uiso 0.33 1 d P A 1 O206 O 0.461(3) -1.384(3) -0.148(2) 0.009(15) Uiso 0.17 1 d P A 2 C207 C 0.374(3) -1.459(3) -0.3614(19) 0.11(2) Uiso 0.50 1 d P . . O207 O 0.368(2) -1.491(2) -0.3165(15) 0.151(16) Uiso 0.50 1 d P . . O208 O -0.1498(11) -1.3868(11) -0.2833(7) 0.096(7) Uiso 0.83 1 d P . . C208 C -0.160(2) -1.4131(19) -0.3341(12) 0.118(13) Uiso 0.83 1 d P . . O210 O 0.037(3) -1.549(3) -0.3382(15) 0.231(19) Uiso 0.67 1 d P . . C210 C 0.090(3) -1.602(3) -0.3422(14) 0.115(16) Uiso 0.67 1 d P . . C209 C 0.732(3) -1.257(3) -0.2504(18) 0.094(17) Uiso 0.50 1 d P . . O209 O 0.7829(18) -1.2650(17) -0.2744(10) 0.084(10) Uiso 0.50 1 d P . . O211 O 0.7396(12) -1.2191(11) -0.3468(7) 0.138(7) Uiso 1 1 d . . . C211 C 0.6759(17) -1.1799(16) -0.3662(10) 0.114(10) Uiso 1 1 d . . . C213 C 0.051(3) -0.815(3) 0.0895(16) 0.085(16) Uiso 0.50 1 d P . 2 O213 O -0.0273(10) -0.8060(9) 0.0737(6) 0.098(6) Uiso 1 1 d . . . C214 C -0.097(3) -0.777(3) 0.0569(16) 0.080(16) Uiso 0.50 1 d P . 1 O215 O 0.676(4) -1.366(4) -0.653(2) 0.15(2) Uiso 0.33 1 d P B 2 C215 C 0.610(4) -1.338(3) -0.666(2) 0.06(2) Uiso 0.33 1 d P B 2 O217 O 0.7114(13) -0.7995(12) 0.0226(7) 0.072(7) Uiso 0.67 1 d P C 1 C217 C 0.774(3) -0.827(3) 0.0244(16) 0.140(19) Uiso 0.67 1 d P C 1 C218 C 0.246(4) -1.539(4) -0.402(2) 0.08(2) Uiso 0.33 1 d P D 1 O218 O 0.262(4) -1.562(4) -0.357(2) 0.17(3) Uiso 0.33 1 d P D 1 O219 O 0.171(3) -1.513(3) -0.4361(17) 0.102(18) Uiso 0.33 1 d P E 2 C219 C 0.084(4) -1.511(4) -0.460(3) 0.09(3) Uiso 0.33 1 d P E 2 C220 C 0.4846(16) -1.0236(16) 0.0852(11) 0.054(9) Uiso 0.67 1 d P F 2 O220 O 0.4896(14) -1.0468(15) 0.1211(9) 0.105(9) Uiso 0.67 1 d P F 2 O221 O 0.6031(19) -1.1439(18) 0.2136(12) 0.097(11) Uiso 0.50 1 d P . . C221 C 0.581(3) -1.159(3) 0.1683(18) 0.088(17) Uiso 0.50 1 d P . . C222 C 0.040(3) -1.349(3) -0.5035(19) 0.12(2) Uiso 0.50 1 d P . . O222 O 0.0911(19) -1.3914(18) -0.5041(11) 0.092(11) Uiso 0.50 1 d P . . C223 C -0.0233(19) -0.6527(19) 0.0955(12) 0.072(11) Uiso 0.67 1 d P . . O223 O 0.040(3) -0.582(3) 0.1283(18) 0.084(17) Uiso 0.33 1 d P G 1 O224 O 0.044(4) -0.585(4) 0.098(3) 0.17(3) Uiso 0.33 1 d P G 2 O225 O 0.605(3) -1.098(3) -0.1666(16) 0.091(16) Uiso 0.33 1 d P H 1 C225 C 0.553(4) -1.041(4) -0.164(2) 0.07(2) Uiso 0.33 1 d P H 1 O226 O 0.263(3) -1.718(3) -0.2551(19) 0.12(2) Uiso 0.33 1 d P I 1 C226 C 0.262(3) -1.781(3) -0.2286(17) 0.024(13) Uiso 0.33 1 d P I 1 Cl11 Cl 0.2629(6) -1.2728(8) -0.5884(5) 0.121(7) Uiso 0.443(8) 1 d PDU J 1 Cl12 Cl 0.1191(8) -1.2179(8) -0.6042(7) 0.187(9) Uiso 0.443(8) 1 d PDU J 1 Cl13 Cl 0.1330(8) -1.3741(7) -0.6131(6) 0.138(7) Uiso 0.443(8) 1 d PDU J 1 Cl14 Cl 0.1972(13) -1.3712(8) -0.6007(9) 0.163(14) Uiso 0.224(8) 1 d PDU J 2 Cl15 Cl 0.0841(8) -1.2711(14) -0.6091(10) 0.170(14) Uiso 0.224(8) 1 d PDU J 2 Cl16 Cl 0.2360(10) -1.2173(10) -0.5889(11) 0.172(14) Uiso 0.224(8) 1 d PDU J 2 C301 C 0.1706(6) -1.2941(7) -0.6257(7) 0.150(12) Uiso 0.67 1 d PDU . . Cl21 Cl 0.2504(11) -1.2556(8) 0.0971(12) 0.142(15) Uiso 0.17 1 d PDU K 1 Cl22 Cl 0.3805(8) -1.1704(15) 0.1052(10) 0.129(14) Uiso 0.17 1 d PDU K 1 Cl23 Cl 0.2452(12) -1.1068(11) 0.0955(11) 0.125(14) Uiso 0.17 1 d PDU K 1 Cl24 Cl 0.2816(14) -1.2527(9) 0.0833(10) 0.156(16) Uiso 0.17 1 d PDU K 2 Cl25 Cl 0.2136(9) -1.1223(12) 0.1097(12) 0.109(13) Uiso 0.17 1 d PDU K 2 Cl26 Cl 0.3633(10) -1.1152(13) 0.1078(11) 0.124(14) Uiso 0.17 1 d PDU K 2 C302 C 0.2978(8) -1.1652(8) 0.1275(8) 0.138(15) Uiso 0.33 1 d PDU . . O1W O -0.0326(16) -1.5043(16) -0.4005(10) 0.078(10) Uiso 0.50 1 d P . . O2W O 0.320(3) -0.606(3) 0.170(2) 0.021(17) Uiso 0.17 1 d P . . O6W O 0.416(6) -1.814(6) -0.318(4) 0.12(4) Uiso 0.17 1 d P . . O7W O 0.928(4) -1.281(4) -0.133(2) 0.17(3) Uiso 0.33 1 d P . . O4W O 0.2140(18) -1.7232(18) -0.1510(10) 0.245(13) Uiso 1 1 d . . . O3W O 0.264(5) -0.497(5) 0.189(3) 0.23(4) Uiso 0.33 1 d P . . O8W O 0.485(5) -1.081(5) -0.030(3) 0.08(3) Uiso 0.17 1 d P . . O9W O 0.386(5) -1.079(5) 0.000(3) 0.22(4) Uiso 0.33 1 d P . . Cl1 Cl -0.0585(2) -0.9403(2) -0.24964(15) 0.0234(9) Uani 1 1 d U L 2 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 0.0453(8) 0.0659(9) 0.0864(12) 0.0012(8) 0.0000(8) -0.0484(7) Ce2 0.0409(8) 0.0669(9) 0.1123(13) 0.0087(9) 0.0093(8) -0.0420(7) Ce3 0.0621(9) 0.0552(8) 0.0892(12) -0.0163(8) 0.0166(8) -0.0514(7) Ce4 0.0699(10) 0.0506(8) 0.1206(14) -0.0014(9) 0.0265(10) -0.0437(8) O1 0.055(7) 0.029(6) 0.115(8) 0.003(6) 0.004(6) -0.018(6) O2 0.058(7) 0.052(6) 0.133(8) 0.014(7) 0.006(7) -0.030(6) O3 0.068(6) 0.043(6) 0.070(6) -0.013(6) 0.013(6) -0.043(5) O4 0.067(4) 0.061(4) 0.063(4) 0.017(3) 0.020(3) -0.014(4) O5 0.051(4) 0.051(4) 0.068(4) 0.011(3) 0.015(3) -0.007(3) O6 0.064(4) 0.072(4) 0.075(4) 0.015(3) 0.012(4) 0.000(4) O11 0.058(4) 0.064(4) 0.083(4) 0.018(3) 0.007(3) -0.009(4) O12 0.034(6) 0.091(7) 0.133(8) -0.004(7) 0.016(6) -0.039(6) O13 0.047(6) 0.050(6) 0.084(7) 0.000(6) 0.017(6) -0.022(6) O14 0.046(6) 0.083(7) 0.093(7) -0.007(7) 0.003(6) -0.028(6) O15 0.067(6) 0.058(6) 0.098(7) -0.004(6) 0.021(6) -0.046(6) O16 0.130(8) 0.052(7) 0.084(8) -0.016(7) 0.017(7) -0.035(7) O21 0.044(6) 0.068(6) 0.088(7) 0.018(6) 0.001(6) -0.037(5) O22 0.035(6) 0.093(7) 0.057(7) -0.004(7) -0.021(6) -0.029(6) O23 0.070(4) 0.064(4) 0.085(4) 0.018(3) 0.024(3) -0.015(4) O24 0.104(8) 0.059(7) 0.155(8) -0.003(7) 0.032(7) -0.046(7) O25 0.058(6) 0.057(6) 0.075(7) 0.010(6) 0.003(6) -0.049(6) O26 0.043(6) 0.071(7) 0.101(8) 0.004(7) -0.009(6) -0.040(6) O31 0.045(6) 0.063(6) 0.065(6) 0.006(6) 0.012(5) -0.042(5) O32 0.055(4) 0.070(4) 0.064(4) 0.018(3) 0.020(3) -0.015(4) O33 0.059(4) 0.060(4) 0.074(4) 0.016(3) 0.009(3) -0.007(4) O34 0.078(5) 0.072(4) 0.085(5) 0.019(4) 0.014(4) -0.010(4) O35 0.041(6) 0.053(6) 0.090(7) -0.016(6) 0.008(6) -0.040(6) O36 0.056(7) 0.098(7) 0.101(7) 0.022(7) 0.014(6) -0.037(6) N1 0.062(7) 0.042(7) 0.109(8) 0.012(7) 0.008(7) -0.022(6) N2 0.064(6) 0.044(6) 0.117(7) 0.009(6) 0.012(6) -0.028(6) N3 0.066(7) 0.048(6) 0.056(7) -0.013(6) 0.005(6) -0.043(6) N4 0.055(4) 0.049(4) 0.057(4) 0.008(3) 0.014(3) -0.016(3) N5 0.047(4) 0.052(4) 0.054(4) 0.012(3) 0.016(3) -0.010(4) N6 0.055(6) 0.051(6) 0.069(6) 0.019(6) 0.006(6) -0.020(5) N11 0.053(7) 0.066(7) 0.086(7) 0.011(7) 0.008(6) -0.051(6) N12 0.047(6) 0.079(6) 0.103(7) -0.002(6) 0.004(6) -0.044(6) N13 0.053(7) 0.061(7) 0.095(7) -0.001(7) 0.014(7) -0.029(6) N14 0.059(6) 0.061(6) 0.089(7) -0.001(6) 0.020(6) -0.026(6) N15 0.062(4) 0.059(4) 0.070(5) 0.015(4) 0.015(4) -0.008(4) N16 0.081(7) 0.044(6) 0.103(7) 0.012(6) 0.020(6) -0.044(6) N21 0.052(4) 0.058(4) 0.064(4) 0.016(3) 0.015(4) -0.012(4) N22 0.035(6) 0.068(6) 0.080(7) 0.004(6) 0.007(6) -0.044(5) N23 0.075(7) 0.060(7) 0.109(7) 0.011(7) 0.026(7) -0.051(6) N24 0.091(6) 0.071(6) 0.126(7) -0.003(6) 0.023(6) -0.043(6) N25 0.038(6) 0.055(7) 0.099(7) 0.002(6) 0.004(6) -0.042(6) N26 0.045(6) 0.058(6) 0.095(7) 0.005(6) -0.006(6) -0.048(6) N31 0.054(4) 0.060(4) 0.061(5) 0.011(4) 0.013(4) -0.013(4) N32 0.045(6) 0.072(6) 0.069(7) 0.003(6) 0.004(6) -0.038(6) N33 0.047(4) 0.045(4) 0.059(4) 0.010(3) 0.015(4) -0.010(4) N34 0.048(6) 0.054(6) 0.085(6) 0.010(6) 0.011(6) -0.031(5) N35 0.042(7) 0.058(7) 0.102(7) -0.005(7) 0.008(7) -0.029(6) N36 0.050(6) 0.082(6) 0.095(6) -0.003(6) 0.015(6) -0.044(6) C1 0.076(6) 0.057(6) 0.156(7) 0.016(6) -0.001(6) -0.040(6) C2 0.068(7) 0.048(7) 0.153(8) 0.016(7) 0.002(7) -0.049(6) C3 0.071(7) 0.052(7) 0.157(8) 0.015(8) -0.006(8) -0.055(7) C4 0.075(8) 0.062(7) 0.173(8) 0.009(8) -0.010(8) -0.047(7) C5 0.084(7) 0.067(7) 0.191(7) 0.014(7) -0.018(7) -0.053(7) C6 0.073(7) 0.069(6) 0.185(7) 0.011(7) -0.013(7) -0.049(6) C7 0.088(8) 0.081(8) 0.206(9) 0.011(8) -0.021(8) -0.049(8) C8 0.089(9) 0.087(9) 0.225(10) 0.001(9) -0.020(9) -0.056(8) C9 0.086(9) 0.075(8) 0.224(10) 0.012(9) -0.024(9) -0.061(8) C10 0.082(8) 0.076(8) 0.212(9) 0.010(8) -0.028(8) -0.059(8) C11 0.075(8) 0.051(7) 0.143(8) 0.005(8) 0.001(8) -0.036(7) C12 0.059(7) 0.042(6) 0.088(7) 0.006(7) 0.016(7) -0.023(6) C13 0.062(6) 0.043(6) 0.080(7) 0.004(6) 0.012(6) -0.025(6) C14 0.059(7) 0.045(6) 0.082(7) -0.007(7) 0.019(6) -0.044(6) C15 0.060(6) 0.043(6) 0.069(7) -0.004(6) 0.017(6) -0.024(6) C16 0.058(7) 0.045(6) 0.067(7) 0.003(6) 0.021(6) -0.032(6) C17 0.054(6) 0.044(6) 0.069(7) 0.007(6) 0.016(6) -0.022(6) C18 0.057(7) 0.050(7) 0.073(7) 0.005(7) 0.014(6) -0.031(6) C19 0.056(7) 0.041(6) 0.066(7) -0.006(7) 0.012(7) -0.037(6) C20 0.065(7) 0.053(7) 0.052(7) -0.010(7) 0.011(7) -0.047(6) C21 0.063(6) 0.061(6) 0.060(6) -0.008(6) 0.012(6) -0.050(6) C22 0.072(7) 0.064(7) 0.050(7) -0.012(7) 0.016(6) -0.052(6) C23 0.082(7) 0.077(7) 0.065(8) 0.001(7) 0.013(7) -0.058(7) C24 0.086(8) 0.078(7) 0.066(8) -0.016(7) 0.013(7) -0.068(7) C25 0.080(7) 0.070(6) 0.066(7) -0.010(6) 0.014(6) -0.063(6) C26 0.076(6) 0.064(6) 0.062(6) -0.006(6) 0.015(6) -0.056(6) C27 0.076(7) 0.063(7) 0.069(8) -0.006(7) 0.011(7) -0.057(7) C28 0.086(8) 0.058(8) 0.071(9) -0.012(8) 0.016(8) -0.055(7) C29 0.091(8) 0.073(8) 0.076(9) -0.005(8) 0.020(8) -0.058(8) C30 0.087(8) 0.069(7) 0.077(8) -0.013(7) 0.017(7) -0.062(7) C31 0.035(6) 0.045(6) 0.057(7) 0.014(6) 0.012(6) -0.021(6) C32 0.061(5) 0.062(5) 0.067(5) 0.016(4) 0.016(4) -0.004(4) C33 0.073(4) 0.071(4) 0.079(4) 0.019(3) 0.017(3) 0.000(4) C34 0.072(5) 0.071(5) 0.077(5) 0.021(4) 0.016(4) 0.000(4) C35 0.083(5) 0.081(5) 0.087(5) 0.022(4) 0.018(4) 0.000(4) C36 0.079(8) 0.077(7) 0.100(8) 0.022(7) 0.013(7) -0.008(7) C37 0.077(7) 0.070(7) 0.105(7) 0.020(6) 0.010(7) -0.017(6) C38 0.077(4) 0.076(4) 0.087(4) 0.020(3) 0.016(3) -0.003(4) C39 0.077(8) 0.066(8) 0.108(8) 0.010(7) 0.011(8) -0.014(7) C40 0.095(9) 0.079(9) 0.118(9) 0.007(8) -0.002(9) -0.020(8) C41 0.088(9) 0.066(8) 0.118(9) 0.018(8) 0.001(9) -0.017(8) C42 0.089(8) 0.071(8) 0.110(8) 0.019(8) 0.005(8) -0.010(8) C51 0.060(6) 0.092(7) 0.129(7) -0.008(7) -0.005(6) -0.044(6) C52 0.056(7) 0.090(7) 0.128(8) -0.008(7) 0.004(7) -0.059(7) C53 0.052(7) 0.091(8) 0.130(8) -0.019(8) 0.003(8) -0.056(7) C54 0.059(8) 0.093(8) 0.130(8) -0.009(8) -0.013(8) -0.053(7) C55 0.070(7) 0.100(7) 0.137(7) -0.016(7) -0.004(7) -0.041(7) C56 0.073(7) 0.095(7) 0.127(7) -0.004(7) -0.002(7) -0.041(6) C57 0.090(8) 0.109(8) 0.138(8) -0.018(8) -0.005(8) -0.033(8) C58 0.097(9) 0.112(9) 0.135(9) -0.015(9) -0.005(9) -0.026(9) C59 0.093(9) 0.115(9) 0.140(10) -0.014(9) -0.004(9) -0.037(9) C60 0.086(8) 0.101(8) 0.137(9) -0.007(8) -0.014(8) -0.041(8) C61 0.048(7) 0.078(8) 0.117(8) 0.008(8) -0.002(7) -0.057(7) C62 0.053(4) 0.061(5) 0.060(5) 0.011(4) 0.018(4) -0.004(4) C63 0.059(6) 0.061(6) 0.077(7) 0.001(6) 0.019(6) -0.021(6) C64 0.056(7) 0.061(7) 0.078(7) -0.001(7) 0.022(6) -0.020(6) C65 0.056(6) 0.051(6) 0.073(7) 0.006(6) 0.026(6) -0.024(6) C66 0.054(7) 0.054(7) 0.079(7) 0.003(7) 0.015(6) -0.029(6) C67 0.063(6) 0.058(6) 0.074(7) 0.006(6) 0.025(6) -0.014(6) C68 0.055(7) 0.053(7) 0.072(7) 0.002(7) 0.026(6) -0.012(6) C69 0.056(7) 0.055(7) 0.086(7) -0.007(7) 0.021(7) -0.027(7) C70 0.067(5) 0.070(5) 0.076(5) 0.013(4) 0.015(4) -0.002(4) C71 0.072(4) 0.073(4) 0.084(4) 0.015(3) 0.016(3) 0.001(4) C72 0.065(5) 0.067(5) 0.076(5) 0.015(4) 0.018(4) -0.001(4) C73 0.069(5) 0.072(5) 0.080(5) 0.015(4) 0.018(4) -0.002(4) C74 0.071(8) 0.074(8) 0.122(8) -0.003(7) 0.006(7) -0.014(7) C75 0.079(7) 0.074(7) 0.128(7) -0.006(7) 0.008(7) -0.017(7) C76 0.069(6) 0.070(6) 0.120(7) -0.003(6) 0.009(6) -0.020(6) C77 0.079(8) 0.073(8) 0.138(8) -0.009(8) 0.007(8) -0.011(8) C78 0.083(9) 0.077(9) 0.159(9) -0.023(9) 0.003(9) -0.026(8) C79 0.086(9) 0.080(9) 0.158(9) -0.013(9) 0.002(9) -0.026(9) C80 0.076(8) 0.079(8) 0.153(9) -0.013(8) 0.009(8) -0.030(8) C81 0.059(5) 0.058(5) 0.067(5) 0.013(4) 0.018(4) -0.004(4) C82 0.083(7) 0.055(7) 0.097(8) -0.013(7) 0.023(7) -0.053(7) C83 0.098(6) 0.051(6) 0.097(7) -0.002(6) 0.029(6) -0.040(6) C84 0.092(7) 0.059(7) 0.090(7) -0.002(7) 0.039(7) -0.045(6) C85 0.108(8) 0.058(7) 0.090(8) 0.009(7) 0.031(8) -0.031(7) C86 0.106(8) 0.050(7) 0.101(8) 0.005(7) 0.028(8) -0.044(7) C87 0.107(7) 0.056(7) 0.107(7) -0.010(7) 0.032(7) -0.039(6) C88 0.104(7) 0.058(6) 0.105(7) -0.008(6) 0.031(6) -0.043(6) C89 0.110(8) 0.061(7) 0.109(8) -0.011(8) 0.034(8) -0.044(7) C90 0.115(9) 0.055(8) 0.120(9) -0.009(8) 0.020(9) -0.039(8) C91 0.119(9) 0.076(9) 0.120(9) -0.004(9) 0.032(9) -0.036(8) C92 0.110(8) 0.053(7) 0.104(8) -0.007(8) 0.032(8) -0.038(7) C101 0.039(6) 0.074(6) 0.073(6) 0.012(6) 0.002(6) -0.036(6) C102 0.034(6) 0.070(7) 0.064(7) 0.022(7) -0.002(7) -0.039(6) C103 0.045(7) 0.082(7) 0.067(8) 0.009(7) 0.002(7) -0.036(7) C104 0.048(7) 0.079(7) 0.080(8) 0.006(7) -0.003(7) -0.033(7) C105 0.044(6) 0.089(7) 0.079(7) 0.008(7) -0.011(6) -0.031(6) C106 0.044(6) 0.079(6) 0.079(7) 0.013(6) -0.002(6) -0.035(6) C107 0.046(7) 0.084(8) 0.083(8) 0.012(7) 0.001(7) -0.033(7) C108 0.061(8) 0.096(9) 0.090(9) 0.006(8) -0.007(8) -0.033(8) C109 0.066(8) 0.097(9) 0.087(9) 0.020(8) -0.008(8) -0.022(8) C110 0.050(7) 0.095(8) 0.089(8) 0.013(8) -0.007(7) -0.030(7) C111 0.041(7) 0.070(7) 0.073(8) 0.008(7) 0.006(7) -0.039(6) C112 0.049(4) 0.053(4) 0.058(5) 0.015(4) 0.012(4) -0.009(4) C113 0.050(6) 0.065(6) 0.074(7) 0.015(6) 0.015(6) -0.030(6) C114 0.043(6) 0.063(7) 0.078(7) 0.009(6) 0.015(6) -0.028(6) C115 0.052(6) 0.061(6) 0.081(7) 0.014(6) 0.017(6) -0.032(6) C116 0.046(7) 0.062(7) 0.079(7) 0.002(7) 0.018(7) -0.033(6) C117 0.045(6) 0.059(6) 0.086(7) 0.003(6) 0.017(6) -0.040(6) C118 0.044(6) 0.060(7) 0.080(7) 0.005(6) 0.015(6) -0.042(6) C119 0.059(7) 0.063(7) 0.091(7) 0.008(7) 0.015(7) -0.033(7) C120 0.093(7) 0.079(7) 0.151(8) -0.007(7) 0.022(7) -0.060(7) C121 0.102(7) 0.079(6) 0.162(7) -0.019(7) 0.021(7) -0.064(6) C122 0.108(8) 0.078(7) 0.163(8) -0.010(7) 0.018(8) -0.080(7) C123 0.109(8) 0.084(8) 0.174(9) -0.014(8) 0.019(8) -0.063(8) C124 0.123(8) 0.088(8) 0.175(9) -0.022(8) 0.023(8) -0.064(8) C125 0.120(7) 0.093(7) 0.177(8) -0.020(7) 0.021(7) -0.054(7) C126 0.118(7) 0.095(7) 0.166(7) -0.016(7) 0.021(7) -0.057(7) C127 0.121(8) 0.104(8) 0.172(8) -0.019(8) 0.018(8) -0.049(7) C128 0.129(9) 0.118(9) 0.170(10) -0.015(9) 0.023(9) -0.037(9) C129 0.134(9) 0.110(9) 0.178(10) -0.018(9) 0.032(9) -0.043(9) C130 0.132(9) 0.108(8) 0.178(9) -0.023(9) 0.026(9) -0.056(8) C131 0.043(7) 0.059(7) 0.088(7) -0.003(7) 0.003(7) -0.039(6) C132 0.043(7) 0.063(7) 0.100(8) 0.005(7) 0.006(7) -0.037(7) C133 0.052(6) 0.069(6) 0.116(7) 0.002(6) -0.006(6) -0.038(6) C134 0.044(7) 0.059(7) 0.111(7) 0.012(7) -0.004(7) -0.040(6) C135 0.054(7) 0.067(7) 0.120(8) -0.002(7) -0.001(7) -0.042(7) C136 0.058(7) 0.069(7) 0.123(8) 0.012(8) -0.001(7) -0.033(7) C137 0.062(7) 0.077(7) 0.130(7) 0.001(7) 0.004(7) -0.038(6) C138 0.056(6) 0.065(6) 0.119(7) 0.007(6) -0.002(6) -0.039(6) C139 0.070(8) 0.079(8) 0.131(8) 0.001(8) -0.001(8) -0.029(7) C140 0.086(5) 0.088(5) 0.100(5) 0.018(4) 0.015(4) -0.002(4) C141 0.069(8) 0.084(8) 0.134(9) -0.010(8) 0.014(8) -0.028(8) C142 0.070(8) 0.084(8) 0.128(8) 0.005(8) 0.001(8) -0.030(7) C151 0.062(6) 0.080(6) 0.066(6) 0.007(6) 0.003(6) -0.051(6) C152 0.060(7) 0.073(7) 0.063(7) 0.011(7) -0.003(7) -0.047(6) C153 0.069(7) 0.089(7) 0.065(8) 0.012(7) 0.000(7) -0.054(7) C154 0.073(7) 0.089(8) 0.063(8) 0.009(7) 0.002(7) -0.064(7) C155 0.066(6) 0.086(7) 0.062(7) 0.005(6) 0.004(6) -0.058(6) C156 0.065(6) 0.082(6) 0.065(6) 0.008(6) 0.008(6) -0.057(6) C157 0.069(7) 0.086(8) 0.071(8) 0.009(7) 0.007(7) -0.060(7) C158 0.074(8) 0.093(8) 0.069(9) 0.004(8) 0.007(8) -0.052(8) C159 0.079(8) 0.096(9) 0.075(9) 0.010(8) 0.002(8) -0.054(8) C160 0.072(8) 0.092(8) 0.068(8) 0.008(8) 0.004(7) -0.062(7) C161 0.052(7) 0.076(7) 0.063(8) 0.008(7) 0.008(7) -0.040(7) C162 0.046(4) 0.052(4) 0.052(5) 0.013(4) 0.013(4) -0.008(4) C163 0.040(6) 0.058(6) 0.065(6) 0.002(6) 0.009(6) -0.023(6) C164 0.037(6) 0.061(7) 0.065(7) 0.011(6) 0.017(6) -0.016(6) C165 0.038(6) 0.060(6) 0.068(7) -0.004(6) 0.013(6) -0.026(6) C166 0.040(6) 0.067(7) 0.076(7) -0.004(7) 0.009(7) -0.029(6) C167 0.037(6) 0.066(6) 0.079(7) -0.005(6) 0.013(6) -0.028(6) C168 0.043(7) 0.067(7) 0.072(7) 0.003(7) 0.009(6) -0.024(6) C169 0.043(6) 0.049(7) 0.066(7) 0.013(6) 0.015(6) -0.020(6) C170 0.054(7) 0.054(7) 0.088(7) 0.009(7) 0.014(7) -0.026(7) C171 0.057(6) 0.071(6) 0.098(6) 0.012(6) 0.019(6) -0.027(6) C172 0.067(5) 0.072(5) 0.079(5) 0.015(4) 0.023(4) -0.006(4) C173 0.070(7) 0.079(8) 0.105(8) 0.003(7) 0.020(7) -0.026(7) C174 0.072(8) 0.085(8) 0.107(8) 0.003(8) 0.026(7) -0.022(7) C175 0.063(7) 0.082(7) 0.120(7) -0.005(7) 0.026(7) -0.031(6) C176 0.063(6) 0.073(6) 0.108(7) -0.009(6) 0.023(6) -0.029(6) C177 0.062(8) 0.081(8) 0.124(8) -0.008(8) 0.023(8) -0.024(7) C178 0.068(9) 0.082(9) 0.128(9) -0.021(9) 0.023(9) -0.026(8) C179 0.077(9) 0.079(9) 0.132(9) -0.011(9) 0.019(9) -0.022(8) C180 0.070(8) 0.080(8) 0.121(8) -0.004(8) 0.026(8) -0.029(7) C181 0.036(6) 0.072(7) 0.085(7) 0.003(7) 0.013(7) -0.027(7) C182 0.056(7) 0.082(7) 0.115(8) -0.003(7) 0.011(7) -0.052(7) C183 0.056(6) 0.095(6) 0.129(7) -0.012(6) 0.020(6) -0.045(6) C184 0.052(7) 0.087(7) 0.119(7) 0.004(7) 0.014(7) -0.046(7) C185 0.072(5) 0.081(5) 0.091(5) 0.015(4) 0.022(4) -0.009(4) C186 0.069(8) 0.096(8) 0.141(8) -0.010(8) 0.024(8) -0.036(7) C187 0.075(7) 0.088(7) 0.164(7) -0.023(7) 0.012(7) -0.056(7) C188 0.069(6) 0.095(7) 0.162(7) -0.026(7) 0.019(7) -0.048(6) C189 0.079(8) 0.101(8) 0.187(9) -0.035(8) 0.012(8) -0.059(8) C190 0.084(9) 0.111(9) 0.211(10) -0.044(9) 0.004(9) -0.062(8) C191 0.084(9) 0.109(9) 0.211(10) -0.047(9) 0.006(9) -0.063(9) C192 0.080(8) 0.100(8) 0.189(9) -0.038(9) 0.016(8) -0.058(8) Cl1 0.0220(11) 0.0228(11) 0.0255(12) 0.0059(8) 0.0066(8) -0.0019(8) _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 O32 2.116(11) . ? Ce1 O26 2.177(11) . ? Ce1 O6 2.179(12) . ? Ce1 O25 2.347(13) . ? Ce1 O5 2.363(12) . ? Ce1 O31 2.491(11) . ? Ce1 N6 2.573(18) . ? Ce1 N26 2.617(17) . ? Ce1 N32 2.622(18) . ? Ce2 O12 2.127(12) . ? Ce2 O22 2.144(13) . ? Ce2 O11 2.174(14) . ? Ce2 O36 2.204(11) . ? Ce2 O35 2.383(13) . ? Ce2 O21 2.445(12) . ? Ce2 N12 2.53(2) . ? Ce2 N22 2.543(16) . ? Ce2 N36 2.575(18) . ? Ce3 O14 2.136(12) . ? Ce3 O34 2.150(13) . ? Ce3 O4 2.168(11) . ? Ce3 O33 2.359(13) . ? Ce3 O13 2.395(13) . ? Ce3 O3 2.459(11) . ? Ce3 N34 2.573(18) . ? Ce3 N14 2.614(18) . ? Ce3 N4 2.614(17) . ? Ce4 O24 2.055(14) . ? Ce4 O16 2.102(14) . ? Ce4 O2 2.178(11) . ? Ce4 O23 2.305(14) . ? Ce4 O1 2.362(12) . ? Ce4 O15 2.455(13) . ? Ce4 N16 2.457(18) . ? Ce4 N2 2.560(18) . ? Ce4 N24 2.67(2) . ? O1 C12 1.312(9) . ? O2 C2 1.320(8) . ? O3 C19 1.297(9) . ? O4 C22 1.314(8) . ? O5 C31 1.322(9) . ? O6 C34 1.314(9) . ? O11 C62 1.305(9) . ? O12 C52 1.319(9) . ? O13 C69 1.312(9) . ? O14 C72 1.310(8) . ? O15 C81 1.307(9) . ? O16 C84 1.310(9) . ? O21 C112 1.308(9) . ? O22 C102 1.318(8) . ? O23 C119 1.310(10) . ? O24 C122 1.331(9) . ? O25 C131 1.307(9) . ? O26 C134 1.310(8) . ? O31 C162 1.307(9) . ? O32 C152 1.315(8) . ? O33 C169 1.315(9) . ? O34 C172 1.326(9) . ? O35 C181 1.310(9) . ? O36 C184 1.323(9) . ? N1 N2 1.33(2) . ? N1 C12 1.41(2) . ? N1 H1A 0.8600 . ? N2 C11 1.34(2) . ? N3 C19 1.23(2) . ? N3 N4 1.460(19) . ? N4 C20 1.31(2) . ? N5 N6 1.329(19) . ? N5 C31 1.36(2) . ? N5 H5A 0.8600 . ? N6 C32 1.23(2) . ? N11 C62 1.27(2) . ? N11 N12 1.41(2) . ? N11 H11G 0.8600 . ? N12 C61 1.29(3) . ? N13 C69 1.31(2) . ? N13 N14 1.33(2) . ? N13 H13F 0.8600 . ? N14 C70 1.24(3) . ? N15 C81 1.27(2) . ? N15 N16 1.37(2) . ? N16 C82 1.40(3) . ? N21 C112 1.29(2) . ? N21 N22 1.44(2) . ? N22 C111 1.35(2) . ? N23 C119 1.36(3) . ? N23 N24 1.47(3) . ? N23 H23B 0.8600 . ? N24 C120 1.35(3) . ? N25 C131 1.33(2) . ? N25 N26 1.34(2) . ? N25 H25A 0.8600 . ? N26 C132 1.24(2) . ? N31 C162 1.25(2) . ? N31 N32 1.43(2) . ? N31 H31A 0.8600 . ? N32 C161 1.29(2) . ? N33 C169 1.26(2) . ? N33 N34 1.42(2) . ? N34 C170 1.31(2) . ? N35 N36 1.32(2) . ? N35 C181 1.38(2) . ? N35 H35B 0.8600 . ? N36 C182 1.29(2) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 C11 1.46(2) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C6 1.3900 . ? C5 C10 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C7 H7A 0.9300 . ? C8 C9 1.3900 . ? C8 H8A 0.9300 . ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C13 1.43(2) . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 C16 1.3900 . ? C15 C19 1.41(2) . ? C16 C17 1.3900 . ? C16 H16A 0.9300 . ? C17 C18 1.3900 . ? C17 C31 1.44(2) . ? C18 H18A 0.9300 . ? C20 C21 1.478(19) . ? C20 H20A 0.9300 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C23 H23A 0.9300 . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C27 H27A 0.9300 . ? C28 C29 1.3900 . ? C28 H28A 0.9300 . ? C29 C30 1.3900 . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C32 C33 1.51(2) . ? C32 H32A 0.9300 . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C35 H35A 0.9300 . ? C36 C37 1.3900 . ? C36 H36A 0.9300 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C39 H39A 0.9300 . ? C40 C41 1.3900 . ? C40 H40A 0.9300 . ? C41 C42 1.3900 . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C51 C61 1.56(3) . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C53 H53A 0.9300 . ? C54 C55 1.3900 . ? C54 H54A 0.9300 . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C57 H57A 0.9300 . ? C58 C59 1.3900 . ? C58 H58A 0.9300 . ? C59 C60 1.3900 . ? C59 H59A 0.9300 . ? C60 H60A 0.9300 . ? C61 H61A 0.9300 . ? C62 C63 1.38(2) . ? C63 C64 1.3900 . ? C63 C68 1.3900 . ? C64 C65 1.3900 . ? C64 H64A 0.9300 . ? C65 C66 1.3900 . ? C65 C69 1.44(2) . ? C66 C67 1.3900 . ? C66 H66A 0.9300 . ? C67 C68 1.3900 . ? C67 C81 1.51(2) . ? C68 H68A 0.9300 . ? C70 C71 1.39(2) . ? C70 H70A 0.9300 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C73 H73A 0.9300 . ? C74 C75 1.3900 . ? C74 H74A 0.9300 . ? C75 C76 1.3900 . ? C75 C80 1.3900 . ? C76 C77 1.3900 . ? C77 C78 1.3900 . ? C77 H77A 0.9300 . ? C78 C79 1.3900 . ? C78 H78A 0.9300 . ? C79 C80 1.3900 . ? C79 H79A 0.9300 . ? C80 H80A 0.9300 . ? C82 C83 1.49(2) . ? C82 H82A 0.9300 . ? C83 C84 1.3900 . ? C83 C88 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? C85 H85A 0.9300 . ? C86 C87 1.3900 . ? C86 H86A 0.9300 . ? C87 C88 1.3900 . ? C87 C92 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.3900 . ? C89 H89A 0.9300 . ? C90 C91 1.3900 . ? C90 H90A 0.9300 . ? C91 C92 1.3900 . ? C91 H91A 0.9300 . ? C92 H92A 0.9300 . ? C101 C102 1.3900 . ? C101 C106 1.3900 . ? C101 C111 1.43(2) . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C103 H10B 0.9300 . ? C104 C105 1.3900 . ? C104 H10C 0.9300 . ? C105 C106 1.3900 . ? C105 C110 1.3900 . ? C106 C107 1.3900 . ? C107 C108 1.3900 . ? C107 H10D 0.9300 . ? C108 C109 1.3900 . ? C108 H10E 0.9300 . ? C109 C110 1.3900 . ? C109 H10F 0.9300 . ? C110 H11B 0.9300 . ? C111 H11C 0.9300 . ? C112 C113 1.43(2) . ? C113 C114 1.3900 . ? C113 C118 1.3900 . ? C114 C115 1.3900 . ? C114 H11D 0.9300 . ? C115 C116 1.3900 . ? C115 C119 1.40(2) . ? C116 C117 1.3900 . ? C116 H11E 0.9300 . ? C117 C118 1.3900 . ? C117 C131 1.40(2) . ? C118 H11F 0.9300 . ? C120 C121 1.38(3) . ? C120 H12A 0.9300 . ? C121 C122 1.3900 . ? C121 C126 1.3900 . ? C122 C123 1.3900 . ? C123 C124 1.3900 . ? C123 H12B 0.9300 . ? C124 C125 1.3900 . ? C124 H12C 0.9300 . ? C125 C126 1.3900 . ? C125 C130 1.3900 . ? C126 C127 1.3900 . ? C127 C128 1.3900 . ? C127 H12D 0.9300 . ? C128 C129 1.3900 . ? C128 H12E 0.9300 . ? C129 C130 1.3900 . ? C129 H12F 0.9300 . ? C130 H13A 0.9300 . ? C132 C133 1.48(2) . ? C132 H13B 0.9300 . ? C133 C134 1.3900 . ? C133 C138 1.3900 . ? C134 C135 1.3900 . ? C135 C136 1.3900 . ? C135 H13C 0.9300 . ? C136 C137 1.3900 . ? C136 H13D 0.9300 . ? C137 C138 1.3900 . ? C137 C142 1.3900 . ? C138 C139 1.3900 . ? C139 C140 1.3900 . ? C139 H13E 0.9300 . ? C140 C141 1.3900 . ? C140 H14B 0.9300 . ? C141 C142 1.3900 . ? C141 H14C 0.9300 . ? C142 H14D 0.9300 . ? C151 C152 1.3900 . ? C151 C156 1.3900 . ? C151 C161 1.42(2) . ? C152 C153 1.3900 . ? C153 C154 1.3900 . ? C153 H15A 0.9300 . ? C154 C155 1.3900 . ? C154 H15B 0.9300 . ? C155 C156 1.3900 . ? C155 C160 1.3900 . ? C156 C157 1.3900 . ? C157 C158 1.3900 . ? C157 H15C 0.9300 . ? C158 C159 1.3900 . ? C158 H15D 0.9300 . ? C159 C160 1.3900 . ? C159 H15E 0.9300 . ? C160 H16B 0.9300 . ? C161 H16C 0.9300 . ? C162 C163 1.401(19) . ? C163 C164 1.3900 . ? C163 C168 1.3900 . ? C164 C165 1.3900 . ? C164 H16D 0.9300 . ? C165 C166 1.3900 . ? C165 C169 1.53(2) . ? C166 C167 1.3900 . ? C166 H16E 0.9300 . ? C167 C168 1.3900 . ? C167 C181 1.42(2) . ? C168 H16F 0.9300 . ? C170 C171 1.50(2) . ? C170 H17A 0.9300 . ? C171 C172 1.3900 . ? C171 C176 1.3900 . ? C172 C173 1.3900 . ? C173 C174 1.3900 . ? C173 H17B 0.9300 . ? C174 C175 1.3900 . ? C174 H17C 0.9300 . ? C175 C176 1.3900 . ? C175 C180 1.3900 . ? C176 C177 1.3900 . ? C177 C178 1.3900 . ? C177 H17D 0.9300 . ? C178 C179 1.3900 . ? C178 H17E 0.9300 . ? C179 C180 1.3900 . ? C179 H17F 0.9300 . ? C180 H18B 0.9300 . ? C182 C183 1.46(2) . ? C182 H18C 0.9300 . ? C183 C184 1.3900 . ? C183 C188 1.3900 . ? C184 C185 1.3900 . ? C185 C186 1.3900 . ? C185 H18D 0.9300 . ? C186 C187 1.3900 . ? C186 H18E 0.9300 . ? C187 C188 1.3900 . ? C187 C192 1.3900 . ? C188 C189 1.3900 . ? C189 C190 1.3900 . ? C189 H18F 0.9300 . ? C190 C191 1.3900 . ? C190 H19A 0.9300 . ? C191 C192 1.3900 . ? C191 H19B 0.9300 . ? C192 H19C 0.9300 . ? C201 O201 1.47(4) . ? O202 C202 1.73(6) . ? O203 C203 1.43(5) . ? O204 C204 1.33(7) . ? C205 O205 1.14(7) . ? C205 O206 1.40(6) . ? C207 O207 1.64(6) . ? O208 C208 1.47(3) . ? O210 C210 1.42(5) . ? C209 O209 1.30(5) . ? O211 C211 1.49(3) . ? C213 O213 1.45(5) . ? C213 O7W 1.90(8) 2_635 ? O213 C214 1.44(5) . ? O215 C215 1.34(7) . ? O217 C217 1.26(5) . ? C218 O218 1.54(8) . ? O219 C219 1.62(8) . ? C220 O220 1.26(3) . ? O221 C221 1.31(5) . ? C222 O222 1.24(6) . ? C223 O223 1.69(6) . ? C223 O224 1.73(8) . ? O225 C225 1.46(7) . ? O226 C226 1.59(7) . ? Cl11 C301 1.798(10) . ? Cl12 C301 1.795(10) . ? Cl13 C301 1.790(10) . ? Cl14 C301 1.815(11) . ? Cl15 C301 1.812(11) . ? Cl16 C301 1.808(11) . ? Cl21 C302 1.799(11) . ? Cl22 C302 1.803(11) . ? Cl23 C302 1.799(11) . ? Cl24 C302 1.802(11) . ? Cl25 C302 1.803(11) . ? Cl26 C302 1.802(11) . ? O7W C213 1.90(8) 2_635 ? 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 O32 Ce1 O26 86.9(5) . . ? O32 Ce1 O6 81.5(5) . . ? O26 Ce1 O6 85.1(5) . . ? O32 Ce1 O25 87.6(5) . . ? O26 Ce1 O25 129.9(4) . . ? O6 Ce1 O25 142.8(5) . . ? O32 Ce1 O5 146.8(4) . . ? O26 Ce1 O5 84.3(5) . . ? O6 Ce1 O5 129.2(5) . . ? O25 Ce1 O5 74.2(5) . . ? O32 Ce1 O31 127.4(4) . . ? O26 Ce1 O31 143.7(5) . . ? O6 Ce1 O31 88.4(5) . . ? O25 Ce1 O31 70.4(4) . . ? O5 Ce1 O31 72.5(4) . . ? O32 Ce1 N6 148.5(5) . . ? O26 Ce1 N6 83.7(5) . . ? O6 Ce1 N6 67.8(5) . . ? O25 Ce1 N6 121.1(5) . . ? O5 Ce1 N6 61.7(5) . . ? O31 Ce1 N6 60.9(4) . . ? O32 Ce1 N26 80.3(5) . . ? O26 Ce1 N26 67.4(5) . . ? O6 Ce1 N26 147.6(5) . . ? O25 Ce1 N26 62.6(4) . . ? O5 Ce1 N26 66.8(5) . . ? O31 Ce1 N26 123.9(5) . . ? N6 Ce1 N26 122.7(6) . . ? O32 Ce1 N32 65.5(5) . . ? O26 Ce1 N32 147.4(6) . . ? O6 Ce1 N32 74.5(5) . . ? O25 Ce1 N32 68.6(5) . . ? O5 Ce1 N32 128.3(5) . . ? O31 Ce1 N32 62.0(5) . . ? N6 Ce1 N32 110.5(5) . . ? N26 Ce1 N32 120.5(6) . . ? O12 Ce2 O22 84.0(6) . . ? O12 Ce2 O11 126.2(6) . . ? O22 Ce2 O11 148.5(5) . . ? O12 Ce2 O36 85.9(5) . . ? O22 Ce2 O36 86.5(5) . . ? O11 Ce2 O36 87.2(5) . . ? O12 Ce2 O35 140.5(5) . . ? O22 Ce2 O35 82.5(5) . . ? O11 Ce2 O35 78.1(5) . . ? O36 Ce2 O35 129.9(4) . . ? O12 Ce2 O21 86.9(5) . . ? O22 Ce2 O21 124.4(4) . . ? O11 Ce2 O21 71.7(5) . . ? O36 Ce2 O21 147.3(5) . . ? O35 Ce2 O21 70.9(4) . . ? O12 Ce2 N12 66.6(7) . . ? O22 Ce2 N12 149.5(6) . . ? O11 Ce2 N12 59.6(6) . . ? O36 Ce2 N12 83.6(5) . . ? O35 Ce2 N12 125.4(6) . . ? O21 Ce2 N12 64.3(5) . . ? O12 Ce2 N22 73.7(5) . . ? O22 Ce2 N22 64.7(5) . . ? O11 Ce2 N22 127.0(5) . . ? O36 Ce2 N22 145.8(6) . . ? O35 Ce2 N22 66.9(5) . . ? O21 Ce2 N22 60.1(5) . . ? N12 Ce2 N22 111.6(6) . . ? O12 Ce2 N36 149.8(5) . . ? O22 Ce2 N36 80.5(6) . . ? O11 Ce2 N36 68.6(5) . . ? O36 Ce2 N36 67.5(5) . . ? O35 Ce2 N36 62.5(5) . . ? O21 Ce2 N36 123.2(5) . . ? N12 Ce2 N36 121.3(6) . . ? N22 Ce2 N36 121.1(6) . . ? O14 Ce3 O34 85.8(5) . . ? O14 Ce3 O4 85.5(5) . . ? O34 Ce3 O4 83.6(5) . . ? O14 Ce3 O33 85.5(5) . . ? O34 Ce3 O33 129.1(5) . . ? O4 Ce3 O33 145.1(4) . . ? O14 Ce3 O13 128.8(4) . . ? O34 Ce3 O13 142.2(5) . . ? O4 Ce3 O13 84.5(5) . . ? O33 Ce3 O13 75.2(5) . . ? O14 Ce3 O3 145.6(5) . . ? O34 Ce3 O3 89.8(5) . . ? O4 Ce3 O3 127.9(4) . . ? O33 Ce3 O3 71.1(4) . . ? O13 Ce3 O3 69.9(4) . . ? O14 Ce3 N34 84.4(5) . . ? O34 Ce3 N34 67.6(6) . . ? O4 Ce3 N34 150.1(5) . . ? O33 Ce3 N34 61.7(5) . . ? O13 Ce3 N34 123.2(5) . . ? O3 Ce3 N34 62.5(4) . . ? O14 Ce3 N14 66.2(5) . . ? O34 Ce3 N14 146.5(5) . . ? O4 Ce3 N14 76.4(5) . . ? O33 Ce3 N14 69.1(5) . . ? O13 Ce3 N14 62.6(5) . . ? O3 Ce3 N14 123.7(5) . . ? N34 Ce3 N14 124.0(6) . . ? O14 Ce3 N4 147.5(5) . . ? O34 Ce3 N4 74.6(5) . . ? O4 Ce3 N4 67.0(5) . . ? O33 Ce3 N4 126.9(5) . . ? O13 Ce3 N4 67.7(5) . . ? O3 Ce3 N4 61.4(5) . . ? N34 Ce3 N4 110.5(5) . . ? N14 Ce3 N4 119.9(5) . . ? O24 Ce4 O16 80.8(7) . . ? O24 Ce4 O2 87.2(5) . . ? O16 Ce4 O2 86.7(5) . . ? O24 Ce4 O23 128.8(6) . . ? O16 Ce4 O23 148.4(5) . . ? O2 Ce4 O23 84.5(5) . . ? O24 Ce4 O1 143.1(5) . . ? O16 Ce4 O1 88.7(5) . . ? O2 Ce4 O1 127.7(4) . . ? O23 Ce4 O1 73.2(5) . . ? O24 Ce4 O15 87.5(5) . . ? O16 Ce4 O15 126.1(5) . . ? O2 Ce4 O15 145.4(5) . . ? O23 Ce4 O15 72.6(5) . . ? O1 Ce4 O15 70.4(4) . . ? O24 Ce4 N16 75.1(6) . . ? O16 Ce4 N16 66.5(6) . . ? O2 Ce4 N16 149.6(6) . . ? O23 Ce4 N16 125.8(5) . . ? O1 Ce4 N16 68.3(5) . . ? O15 Ce4 N16 59.6(5) . . ? O24 Ce4 N2 148.9(6) . . ? O16 Ce4 N2 81.4(6) . . ? O2 Ce4 N2 66.4(5) . . ? O23 Ce4 N2 67.2(5) . . ? O1 Ce4 N2 61.4(5) . . ? O15 Ce4 N2 123.6(5) . . ? N16 Ce4 N2 120.0(6) . . ? O24 Ce4 N24 63.7(7) . . ? O16 Ce4 N24 143.9(7) . . ? O2 Ce4 N24 85.0(5) . . ? O23 Ce4 N24 65.2(6) . . ? O1 Ce4 N24 123.6(6) . . ? O15 Ce4 N24 62.1(5) . . ? N16 Ce4 N24 107.9(6) . . ? N2 Ce4 N24 126.0(7) . . ? C12 O1 Ce4 124.9(12) . . ? C2 O2 Ce4 148.3(11) . . ? C19 O3 Ce3 121.0(12) . . ? C22 O4 Ce3 141.5(9) . . ? C31 O5 Ce1 123.0(12) . . ? C34 O6 Ce1 146.3(12) . . ? C62 O11 Ce2 136.7(13) . . ? C52 O12 Ce2 156.1(14) . . ? C69 O13 Ce3 119.6(13) . . ? C72 O14 Ce3 147.8(11) . . ? C81 O15 Ce4 118.4(13) . . ? C84 O16 Ce4 147.6(13) . . ? C112 O21 Ce2 121.6(13) . . ? C102 O22 Ce2 142.2(11) . . ? C119 O23 Ce4 127.7(14) . . ? C122 O24 Ce4 156.9(15) . . ? C131 O25 Ce1 125.7(12) . . ? C134 O26 Ce1 141.9(11) . . ? C162 O31 Ce1 120.0(11) . . ? C152 O32 Ce1 144.8(10) . . ? C169 O33 Ce3 120.8(12) . . ? C172 O34 Ce3 144.0(12) . . ? C181 O35 Ce2 120.4(12) . . ? C184 O36 Ce2 144.9(11) . . ? N2 N1 C12 113.0(16) . . ? N2 N1 H1A 123.5 . . ? C12 N1 H1A 123.5 . . ? N1 N2 C11 109.1(19) . . ? N1 N2 Ce4 119.0(12) . . ? C11 N2 Ce4 131.8(16) . . ? C19 N3 N4 114.5(16) . . ? C20 N4 N3 111.2(15) . . ? C20 N4 Ce3 134.1(12) . . ? N3 N4 Ce3 114.7(12) . . ? N6 N5 C31 119.3(16) . . ? N6 N5 H5A 120.3 . . ? C31 N5 H5A 120.3 . . ? C32 N6 N5 114.5(19) . . ? C32 N6 Ce1 130.4(16) . . ? N5 N6 Ce1 114.5(13) . . ? C62 N11 N12 117.7(19) . . ? C62 N11 H11G 121.2 . . ? N12 N11 H11G 121.2 . . ? C61 N12 N11 111(2) . . ? C61 N12 Ce2 134.2(19) . . ? N11 N12 Ce2 113.6(14) . . ? C69 N13 N14 117.6(18) . . ? C69 N13 H13F 121.2 . . ? N14 N13 H13F 121.2 . . ? C70 N14 N13 117(2) . . ? C70 N14 Ce3 129.3(17) . . ? N13 N14 Ce3 113.0(12) . . ? C81 N15 N16 106.2(18) . . ? N15 N16 C82 103.2(17) . . ? N15 N16 Ce4 126.6(15) . . ? C82 N16 Ce4 129.4(13) . . ? C112 N21 N22 110.1(16) . . ? C111 N22 N21 110.1(15) . . ? C111 N22 Ce2 129.6(12) . . ? N21 N22 Ce2 120.1(13) . . ? C119 N23 N24 122.2(19) . . ? C119 N23 H23B 118.9 . . ? N24 N23 H23B 118.9 . . ? C120 N24 N23 120(2) . . ? C120 N24 Ce4 133(2) . . ? N23 N24 Ce4 106.5(14) . . ? C131 N25 N26 121.9(16) . . ? C131 N25 H25A 119.0 . . ? N26 N25 H25A 119.0 . . ? C132 N26 N25 116.3(19) . . ? C132 N26 Ce1 132.3(16) . . ? N25 N26 Ce1 111.2(10) . . ? C162 N31 N32 119.6(17) . . ? C162 N31 H31A 120.2 . . ? N32 N31 H31A 120.2 . . ? C161 N32 N31 113.6(16) . . ? C161 N32 Ce1 134.1(13) . . ? N31 N32 Ce1 112.4(13) . . ? C169 N33 N34 113.1(16) . . ? C170 N34 N33 108.5(18) . . ? C170 N34 Ce3 136.3(16) . . ? N33 N34 Ce3 115.0(12) . . ? N36 N35 C181 116.6(16) . . ? N36 N35 H35B 121.7 . . ? C181 N35 H35B 121.7 . . ? C182 N36 N35 113(2) . . ? C182 N36 Ce2 131.5(17) . . ? N35 N36 Ce2 115.4(12) . . ? C2 C1 C6 120.0 . . ? C2 C1 C11 119.7(11) . . ? C6 C1 C11 120.0(11) . . ? O2 C2 C1 120.8(9) . . ? O2 C2 C3 119.2(9) . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 C10 120.0 . . ? C6 C5 C10 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 C1 120.0 . . ? C5 C6 C1 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 C5 120.0 . . ? C9 C10 H10A 120.0 . . ? C5 C10 H10A 120.0 . . ? N2 C11 C1 125(2) . . ? N2 C11 H11A 117.6 . . ? C1 C11 H11A 117.6 . . ? O1 C12 N1 116.6(17) . . ? O1 C12 C13 124.4(16) . . ? N1 C12 C13 119.0(13) . . ? C14 C13 C18 120.0 . . ? C14 C13 C12 115.8(10) . . ? C18 C13 C12 123.8(11) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 C19 122.8(11) . . ? C14 C15 C19 117.2(11) . . ? C17 C16 C15 120.0 . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 C31 117.9(10) . . ? C16 C17 C31 122.0(10) . . ? C17 C18 C13 120.0 . . ? C17 C18 H18A 120.0 . . ? C13 C18 H18A 120.0 . . ? N3 C19 O3 124.9(18) . . ? N3 C19 C15 118.5(13) . . ? O3 C19 C15 116.5(17) . . ? N4 C20 C21 118.1(16) . . ? N4 C20 H20A 121.0 . . ? C21 C20 H20A 121.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 C20 124.2(10) . . ? C26 C21 C20 115.4(10) . . ? O4 C22 C23 117.9(8) . . ? O4 C22 C21 121.9(8) . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 C30 120.0 . . ? C26 C25 C30 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 C21 120.0 . . ? C25 C26 C21 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30A 120.0 . . ? C25 C30 H30A 120.0 . . ? O5 C31 N5 112.1(16) . . ? O5 C31 C17 124.3(16) . . ? N5 C31 C17 123.5(13) . . ? N6 C32 C33 128(2) . . ? N6 C32 H32A 116.1 . . ? C33 C32 H32A 116.1 . . ? C34 C33 C38 120.0 . . ? C34 C33 C32 118.0(11) . . ? C38 C33 C32 121.8(11) . . ? O6 C34 C33 122.0(11) . . ? O6 C34 C35 118.0(11) . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 C42 120.0 . . ? C38 C37 C42 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 C33 120.0 . . ? C37 C38 C33 120.0 . . ? C38 C39 C40 120.0 . . ? C38 C39 H39A 120.0 . . ? C40 C39 H39A 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C41 C42 C37 120.0 . . ? C41 C42 H42A 120.0 . . ? C37 C42 H42A 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 C61 118.2(13) . . ? C56 C51 C61 121.2(13) . . ? O12 C52 C51 118.1(13) . . ? O12 C52 C53 121.2(13) . . ? C51 C52 C53 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54A 120.0 . . ? C53 C54 H54A 120.0 . . ? C54 C55 C56 120.0 . . ? C54 C55 C60 120.0 . . ? C56 C55 C60 120.0 . . ? C57 C56 C55 120.0 . . ? C57 C56 C51 120.0 . . ? C55 C56 C51 120.0 . . ? C56 C57 C58 120.0 . . ? C56 C57 H57A 120.0 . . ? C58 C57 H57A 120.0 . . ? C59 C58 C57 120.0 . . ? C59 C58 H58A 120.0 . . ? C57 C58 H58A 120.0 . . ? C60 C59 C58 120.0 . . ? C60 C59 H59A 120.0 . . ? C58 C59 H59A 120.0 . . ? C59 C60 C55 120.0 . . ? C59 C60 H60A 120.0 . . ? C55 C60 H60A 120.0 . . ? N12 C61 C51 124(2) . . ? N12 C61 H61A 118.1 . . ? C51 C61 H61A 118.1 . . ? N11 C62 O11 109.0(18) . . ? N11 C62 C63 119.7(16) . . ? O11 C62 C63 131.2(19) . . ? C62 C63 C64 118.2(12) . . ? C62 C63 C68 121.5(12) . . ? C64 C63 C68 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64A 120.0 . . ? C63 C64 H64A 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 C69 119.3(11) . . ? C64 C65 C69 120.2(12) . . ? C67 C66 C65 120.0 . . ? C67 C66 H66A 120.0 . . ? C65 C66 H66A 120.0 . . ? C66 C67 C68 120.0 . . ? C66 C67 C81 120.0(11) . . ? C68 C67 C81 120.0(11) . . ? C67 C68 C63 120.0 . . ? C67 C68 H68A 120.0 . . ? C63 C68 H68A 120.0 . . ? N13 C69 O13 121.3(19) . . ? N13 C69 C65 122.6(14) . . ? O13 C69 C65 115.8(16) . . ? N14 C70 C71 132(2) . . ? N14 C70 H70A 114.1 . . ? C71 C70 H70A 114.1 . . ? C72 C71 C76 120.0 . . ? C72 C71 C70 115.3(11) . . ? C76 C71 C70 124.7(11) . . ? O14 C72 C71 124.5(10) . . ? O14 C72 C73 115.4(10) . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74A 120.0 . . ? C75 C74 H74A 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 C80 120.0 . . ? C76 C75 C80 120.0 . . ? C77 C76 C75 120.0 . . ? C77 C76 C71 120.0 . . ? C75 C76 C71 120.0 . . ? C78 C77 C76 120.0 . . ? C78 C77 H77A 120.0 . . ? C76 C77 H77A 120.0 . . ? C77 C78 C79 120.0 . . ? C77 C78 H78A 120.0 . . ? C79 C78 H78A 120.0 . . ? C80 C79 C78 120.0 . . ? C80 C79 H79A 120.0 . . ? C78 C79 H79A 120.0 . . ? C79 C80 C75 120.0 . . ? C79 C80 H80A 120.0 . . ? C75 C80 H80A 120.0 . . ? N15 C81 O15 126(2) . . ? N15 C81 C67 121.6(14) . . ? O15 C81 C67 112.2(17) . . ? N16 C82 C83 123.1(17) . . ? N16 C82 H82A 118.5 . . ? C83 C82 H82A 118.5 . . ? C84 C83 C88 120.0 . . ? C84 C83 C82 117.9(11) . . ? C88 C83 C82 122.1(11) . . ? O16 C84 C85 119.7(9) . . ? O16 C84 C83 119.0(10) . . ? C85 C84 C83 120.0 . . ? C84 C85 C86 120.0 . . ? C84 C85 H85A 120.0 . . ? C86 C85 H85A 120.0 . . ? C87 C86 C85 120.0 . . ? C87 C86 H86A 120.0 . . ? C85 C86 H86A 120.0 . . ? C86 C87 C88 120.0 . . ? C86 C87 C92 120.0 . . ? C88 C87 C92 120.0 . . ? C89 C88 C87 120.0 . . ? C89 C88 C83 120.0 . . ? C87 C88 C83 120.0 . . ? C88 C89 C90 120.0 . . ? C88 C89 H89A 120.0 . . ? C90 C89 H89A 120.0 . . ? C91 C90 C89 120.0 . . ? C91 C90 H90A 120.0 . . ? C89 C90 H90A 120.0 . . ? C90 C91 C92 120.0 . . ? C90 C91 H91A 120.0 . . ? C92 C91 H91A 120.0 . . ? C91 C92 C87 120.0 . . ? C91 C92 H92A 120.0 . . ? C87 C92 H92A 120.0 . . ? C102 C101 C106 120.0 . . ? C102 C101 C111 118.1(10) . . ? C106 C101 C111 121.7(10) . . ? O22 C102 C101 120.2(8) . . ? O22 C102 C103 119.5(8) . . ? C101 C102 C103 120.0 . . ? C102 C103 C104 120.0 . . ? C102 C103 H10B 120.0 . . ? C104 C103 H10B 120.0 . . ? C105 C104 C103 120.0 . . ? C105 C104 H10C 120.0 . . ? C103 C104 H10C 120.0 . . ? C104 C105 C106 120.0 . . ? C104 C105 C110 120.0 . . ? C106 C105 C110 120.0 . . ? C107 C106 C105 120.0 . . ? C107 C106 C101 120.0 . . ? C105 C106 C101 120.0 . . ? C106 C107 C108 120.0 . . ? C106 C107 H10D 120.0 . . ? C108 C107 H10D 120.0 . . ? C107 C108 C109 120.0 . . ? C107 C108 H10E 120.0 . . ? C109 C108 H10E 120.0 . . ? C110 C109 C108 120.0 . . ? C110 C109 H10F 120.0 . . ? C108 C109 H10F 120.0 . . ? C109 C110 C105 120.0 . . ? C109 C110 H11B 120.0 . . ? C105 C110 H11B 120.0 . . ? N22 C111 C101 123.8(16) . . ? N22 C111 H11C 118.1 . . ? C101 C111 H11C 118.1 . . ? N21 C112 O21 122.1(18) . . ? N21 C112 C113 120.4(13) . . ? O21 C112 C113 117.2(17) . . ? C114 C113 C118 120.0 . . ? C114 C113 C112 118.3(11) . . ? C118 C113 C112 121.7(11) . . ? C113 C114 C115 120.0 . . ? C113 C114 H11D 120.0 . . ? C115 C114 H11D 120.0 . . ? C116 C115 C114 120.0 . . ? C116 C115 C119 116.8(12) . . ? C114 C115 C119 123.1(12) . . ? C115 C116 C117 120.0 . . ? C115 C116 H11E 120.0 . . ? C117 C116 H11E 120.0 . . ? C118 C117 C116 120.0 . . ? C118 C117 C131 115.3(12) . . ? C116 C117 C131 124.4(12) . . ? C117 C118 C113 120.0 . . ? C117 C118 H11F 120.0 . . ? C113 C118 H11F 120.0 . . ? O23 C119 N23 114(2) . . ? O23 C119 C115 126(2) . . ? N23 C119 C115 120.0(16) . . ? N24 C120 C121 119(3) . . ? N24 C120 H12A 120.7 . . ? C121 C120 H12A 120.7 . . ? C120 C121 C122 126.5(16) . . ? C120 C121 C126 113.2(16) . . ? C122 C121 C126 120.0 . . ? O24 C122 C121 114.8(14) . . ? O24 C122 C123 122.8(14) . . ? C121 C122 C123 120.0 . . ? C124 C123 C122 120.0 . . ? C124 C123 H12B 120.0 . . ? C122 C123 H12B 120.0 . . ? C123 C124 C125 120.0 . . ? C123 C124 H12C 120.0 . . ? C125 C124 H12C 120.0 . . ? C124 C125 C126 120.0 . . ? C124 C125 C130 120.0 . . ? C126 C125 C130 120.0 . . ? C127 C126 C125 120.0 . . ? C127 C126 C121 120.0 . . ? C125 C126 C121 120.0 . . ? C126 C127 C128 120.0 . . ? C126 C127 H12D 120.0 . . ? C128 C127 H12D 120.0 . . ? C129 C128 C127 120.0 . . ? C129 C128 H12E 120.0 . . ? C127 C128 H12E 120.0 . . ? C130 C129 C128 120.0 . . ? C130 C129 H12F 120.0 . . ? C128 C129 H12F 120.0 . . ? C129 C130 C125 120.0 . . ? C129 C130 H13A 120.0 . . ? C125 C130 H13A 120.0 . . ? O25 C131 N25 114.8(17) . . ? O25 C131 C117 123.4(16) . . ? N25 C131 C117 121.8(14) . . ? N26 C132 C133 126(2) . . ? N26 C132 H13B 117.1 . . ? C133 C132 H13B 117.1 . . ? C134 C133 C138 120.0 . . ? C134 C133 C132 118.3(10) . . ? C138 C133 C132 121.4(10) . . ? O26 C134 C135 115.3(10) . . ? O26 C134 C133 124.6(10) . . ? C135 C134 C133 120.0 . . ? C134 C135 C136 120.0 . . ? C134 C135 H13C 120.0 . . ? C136 C135 H13C 120.0 . . ? C135 C136 C137 120.0 . . ? C135 C136 H13D 120.0 . . ? C137 C136 H13D 120.0 . . ? C138 C137 C136 120.0 . . ? C138 C137 C142 120.0 . . ? C136 C137 C142 120.0 . . ? C139 C138 C137 120.0 . . ? C139 C138 C133 120.0 . . ? C137 C138 C133 120.0 . . ? C140 C139 C138 120.0 . . ? C140 C139 H13E 120.0 . . ? C138 C139 H13E 120.0 . . ? C139 C140 C141 120.0 . . ? C139 C140 H14B 120.0 . . ? C141 C140 H14B 120.0 . . ? C142 C141 C140 120.0 . . ? C142 C141 H14C 120.0 . . ? C140 C141 H14C 120.0 . . ? C141 C142 C137 120.0 . . ? C141 C142 H14D 120.0 . . ? C137 C142 H14D 120.0 . . ? C152 C151 C156 120.0 . . ? C152 C151 C161 122.6(11) . . ? C156 C151 C161 117.0(11) . . ? O32 C152 C151 122.5(8) . . ? O32 C152 C153 117.5(8) . . ? C151 C152 C153 120.0 . . ? C154 C153 C152 120.0 . . ? C154 C153 H15A 120.0 . . ? C152 C153 H15A 120.0 . . ? C155 C154 C153 120.0 . . ? C155 C154 H15B 120.0 . . ? C153 C154 H15B 120.0 . . ? C156 C155 C154 120.0 . . ? C156 C155 C160 120.0 . . ? C154 C155 C160 120.0 . . ? C157 C156 C155 120.0 . . ? C157 C156 C151 120.0 . . ? C155 C156 C151 120.0 . . ? C158 C157 C156 120.0 . . ? C158 C157 H15C 120.0 . . ? C156 C157 H15C 120.0 . . ? C157 C158 C159 120.0 . . ? C157 C158 H15D 120.0 . . ? C159 C158 H15D 120.0 . . ? C160 C159 C158 120.0 . . ? C160 C159 H15E 120.0 . . ? C158 C159 H15E 120.0 . . ? C159 C160 C155 120.0 . . ? C159 C160 H16B 120.0 . . ? C155 C160 H16B 120.0 . . ? N32 C161 C151 119.5(18) . . ? N32 C161 H16C 120.3 . . ? C151 C161 H16C 120.3 . . ? N31 C162 O31 120.9(17) . . ? N31 C162 C163 122.5(13) . . ? O31 C162 C163 116.4(16) . . ? C164 C163 C168 120.0 . . ? C164 C163 C162 122.9(10) . . ? C168 C163 C162 117.1(10) . . ? C163 C164 C165 120.0 . . ? C163 C164 H16D 120.0 . . ? C165 C164 H16D 120.0 . . ? C166 C165 C164 120.0 . . ? C166 C165 C169 119.9(10) . . ? C164 C165 C169 120.0(10) . . ? C165 C166 C167 120.0 . . ? C165 C166 H16E 120.0 . . ? C167 C166 H16E 120.0 . . ? C168 C167 C166 120.0 . . ? C168 C167 C181 120.4(11) . . ? C166 C167 C181 119.5(11) . . ? C167 C168 C163 120.0 . . ? C167 C168 H16F 120.0 . . ? C163 C168 H16F 120.0 . . ? N33 C169 O33 121.8(18) . . ? N33 C169 C165 120.1(14) . . ? O33 C169 C165 118.1(16) . . ? N34 C170 C171 118(2) . . ? N34 C170 H17A 120.9 . . ? C171 C170 H17A 120.9 . . ? C172 C171 C176 120.0 . . ? C172 C171 C170 122.0(11) . . ? C176 C171 C170 117.9(11) . . ? O34 C172 C171 124.3(11) . . ? O34 C172 C173 115.6(11) . . ? C171 C172 C173 120.0 . . ? C174 C173 C172 120.0 . . ? C174 C173 H17B 120.0 . . ? C172 C173 H17B 120.0 . . ? C173 C174 C175 120.0 . . ? C173 C174 H17C 120.0 . . ? C175 C174 H17C 120.0 . . ? C176 C175 C174 120.0 . . ? C176 C175 C180 120.0 . . ? C174 C175 C180 120.0 . . ? C177 C176 C175 120.0 . . ? C177 C176 C171 120.0 . . ? C175 C176 C171 120.0 . . ? C176 C177 C178 120.0 . . ? C176 C177 H17D 120.0 . . ? C178 C177 H17D 120.0 . . ? C179 C178 C177 120.0 . . ? C179 C178 H17E 120.0 . . ? C177 C178 H17E 120.0 . . ? C178 C179 C180 120.0 . . ? C178 C179 H17F 120.0 . . ? C180 C179 H17F 120.0 . . ? C179 C180 C175 120.0 . . ? C179 C180 H18B 120.0 . . ? C175 C180 H18B 120.0 . . ? O35 C181 N35 117.1(16) . . ? O35 C181 C167 121.2(16) . . ? N35 C181 C167 121.1(14) . . ? N36 C182 C183 128(2) . . ? N36 C182 H18C 116.2 . . ? C183 C182 H18C 116.2 . . ? C184 C183 C188 120.0 . . ? C184 C183 C182 117.3(11) . . ? C188 C183 C182 121.7(11) . . ? O36 C184 C183 124.8(10) . . ? O36 C184 C185 115.0(10) . . ? C183 C184 C185 120.0 . . ? C186 C185 C184 120.0 . . ? C186 C185 H18D 120.0 . . ? C184 C185 H18D 120.0 . . ? C185 C186 C187 120.0 . . ? C185 C186 H18E 120.0 . . ? C187 C186 H18E 120.0 . . ? C188 C187 C186 120.0 . . ? C188 C187 C192 120.0 . . ? C186 C187 C192 120.0 . . ? C189 C188 C187 120.0 . . ? C189 C188 C183 120.0 . . ? C187 C188 C183 120.0 . . ? C190 C189 C188 120.0 . . ? C190 C189 H18F 120.0 . . ? C188 C189 H18F 120.0 . . ? C189 C190 C191 120.0 . . ? C189 C190 H19A 120.0 . . ? C191 C190 H19A 120.0 . . ? C192 C191 C190 120.0 . . ? C192 C191 H19B 120.0 . . ? C190 C191 H19B 120.0 . . ? C191 C192 C187 120.0 . . ? C191 C192 H19C 120.0 . . ? C187 C192 H19C 120.0 . . ? O205 C205 O206 115(6) . . ? O213 C213 O7W 95(3) . 2_635 ? C214 O213 C213 164(3) . . ? O223 C223 O224 32(3) . . ? Cl13 C301 Cl12 106.4(10) . . ? Cl13 C301 Cl11 105.5(10) . . ? Cl12 C301 Cl11 105.2(9) . . ? Cl13 C301 Cl16 130.9(16) . . ? Cl12 C301 Cl16 71.6(9) . . ? Cl11 C301 Cl16 37.5(8) . . ? Cl13 C301 Cl15 72.3(10) . . ? Cl12 C301 Cl15 36.4(9) . . ? Cl11 C301 Cl15 126.7(14) . . ? Cl16 C301 Cl15 103.3(10) . . ? Cl13 C301 Cl14 37.5(9) . . ? Cl12 C301 Cl14 127.7(16) . . ? Cl11 C301 Cl14 70.2(9) . . ? Cl16 C301 Cl14 103.7(10) . . ? Cl15 C301 Cl14 103.2(10) . . ? Cl21 C302 Cl23 101.4(11) . . ? Cl21 C302 Cl24 25.6(13) . . ? Cl23 C302 Cl24 100.2(16) . . ? Cl21 C302 Cl26 126.0(19) . . ? Cl23 C302 Cl26 73.2(12) . . ? Cl24 C302 Cl26 100.9(12) . . ? Cl21 C302 Cl25 89.8(11) . . ? Cl23 C302 Cl25 28.4(12) . . ? Cl24 C302 Cl25 100.8(11) . . ? Cl26 C302 Cl25 101.0(11) . . ? Cl21 C302 Cl22 101.0(11) . . ? Cl23 C302 Cl22 101.0(12) . . ? Cl24 C302 Cl22 76.1(12) . . ? Cl26 C302 Cl22 34.5(11) . . ? Cl25 C302 Cl22 129.0(17) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.681 _refine_diff_density_min -1.266 _refine_diff_density_rms 0.169 # Attachment '- Ce-TBMS.cif' data_ce _database_code_depnum_ccdc_archive 'CCDC 794083' #TrackingRef '- Ce-TBMS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C418 H408 Ce8 N64 O77' _chemical_formula_weight 8681.04 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 cubic _symmetry_space_group_name_H-M P-43n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 44.9318(3) _cell_length_b 44.9318(3) _cell_length_c 44.9318(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 90711.3(10) _cell_formula_units_Z 6 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.953 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 26664 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 130565 _diffrn_reflns_av_R_equivalents 0.1266 _diffrn_reflns_av_sigmaI/netI 0.1641 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -52 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 24.99 _reflns_number_total 26583 _reflns_number_gt 8880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0600P)^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 'riding mode' _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 -0.012(16) _refine_ls_number_reflns 26583 _refine_ls_number_parameters 1199 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.2232 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.1927 _refine_ls_wR_factor_gt 0.1669 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.123620(11) 1.149453(12) 0.533905(13) 0.09446(17) Uani 1 1 d . . . Ce2 Ce 0.130343(13) 0.954401(14) 0.655639(13) 0.1067(2) Uani 1 1 d . . . O11 O 0.07808(12) 1.15918(12) 0.54868(14) 0.108(2) Uani 1 1 d . . . N11 N 0.10683(15) 1.11713(16) 0.57850(17) 0.103(3) Uani 1 1 d . . . O12 O 0.15350(15) 0.93024(14) 0.69194(13) 0.120(2) Uani 1 1 d . . . N12 N 0.12633(16) 1.09442(15) 0.58526(16) 0.102(2) Uani 1 1 d . . . H12A H 0.1228 1.0825 0.5998 0.123 Uiso 1 1 calc R . . O13 O 0.36035(12) 0.92717(15) 0.67188(13) 0.112(2) Uani 1 1 d . . . N13 N 0.17814(15) 0.97910(16) 0.67090(16) 0.098(2) Uani 1 1 d . . . N14 N 0.19063(16) 0.99607(16) 0.64890(17) 0.106(3) Uani 1 1 d . . . H14A H 0.2091 1.0011 0.6491 0.127 Uiso 1 1 calc R . . O15 O 0.15541(12) 1.10873(12) 0.54927(13) 0.0964(19) Uani 1 1 d . . . N15 N 0.31945(15) 0.96834(19) 0.66057(15) 0.110(3) Uani 1 1 d . . . O16 O 0.14716(13) 0.99562(12) 0.62819(13) 0.105(2) Uani 1 1 d . . . N16 N 0.30584(15) 0.99144(17) 0.64515(16) 0.105(3) Uani 1 1 d . . . H16A H 0.2868 0.9936 0.6459 0.125 Uiso 1 1 calc R . . O17 O 0.34946(12) 1.00816(12) 0.63206(11) 0.0969(19) Uani 1 1 d . . . O18 O 0.33008(11) 1.12082(12) 0.56111(12) 0.0881(18) Uani 1 1 d . . . N18 N 0.35086(17) 1.11443(16) 0.60562(17) 0.110(3) Uani 1 1 d . . . H18A H 0.3513 1.1044 0.6219 0.132 Uiso 1 1 calc R . . C100 C 0.24796(16) 1.04369(17) 0.55524(18) 0.085(3) Uani 1 1 d . . . H10A H 0.2497 1.0242 0.5461 0.102 Uiso 1 1 calc R . . H10B H 0.2484 1.0584 0.5394 0.102 Uiso 1 1 calc R . . C101 C 0.08504(17) 1.1186(2) 0.5956(2) 0.100(3) Uani 1 1 d . . . H10C H 0.0848 1.1062 0.6121 0.120 Uiso 1 1 calc R . . C102 C 0.1908(2) 0.9786(2) 0.6953(2) 0.109(4) Uani 1 1 d . . . H10D H 0.2077 0.9904 0.6969 0.130 Uiso 1 1 calc R . . C103 C 0.3017(2) 0.9527(2) 0.6777(2) 0.110(4) Uani 1 1 d . . . H10E H 0.2823 0.9594 0.6799 0.132 Uiso 1 1 calc R . . C111 C 0.06038(17) 1.13834(17) 0.59138(18) 0.099(3) Uani 1 1 d D . . C112 C 0.05766(15) 1.15711(18) 0.56788(18) 0.100(3) Uani 1 1 d D . . C113 C 0.03327(16) 1.1755(2) 0.5623(2) 0.149(5) Uani 1 1 d D . . H11A H 0.0324 1.1881 0.5460 0.179 Uiso 1 1 calc R . . C114 C 0.01072(19) 1.1736(2) 0.58258(18) 0.128(4) Uani 1 1 d D . . H11B H -0.0065 1.1847 0.5792 0.153 Uiso 1 1 calc R . . C115 C 0.01216(16) 1.15598(19) 0.60821(19) 0.117(4) Uani 1 1 d D . . C116 C 0.03698(18) 1.13774(18) 0.61121(17) 0.113(4) Uani 1 1 d D . . C117 C 0.03894(19) 1.1221(2) 0.63777(19) 0.166(5) Uani 1 1 d D . . H11C H 0.0565 1.1119 0.6419 0.200 Uiso 1 1 calc R . . C118 C 0.01629(18) 1.1208(2) 0.6582(2) 0.157(5) Uani 1 1 d D . . H11D H 0.0170 1.1081 0.6745 0.188 Uiso 1 1 calc R . . C119 C -0.0081(2) 1.1396(2) 0.65312(19) 0.150(5) Uani 1 1 d D . . H11E H -0.0227 1.1404 0.6678 0.180 Uiso 1 1 calc R . . C120 C -0.0122(2) 1.1571(2) 0.6281(2) 0.136(4) Uani 1 1 d D . . H12B H -0.0291 1.1685 0.6248 0.164 Uiso 1 1 calc R . . C121 C 0.18325(19) 0.96259(19) 0.7204(2) 0.115(4) Uani 1 1 d D . . C122 C 0.1640(2) 0.93896(19) 0.71716(17) 0.119(4) Uani 1 1 d D . . C123 C 0.1546(2) 0.9205(2) 0.74038(16) 0.163(5) Uani 1 1 d D . . H12C H 0.1421 0.9043 0.7375 0.196 Uiso 1 1 calc R . . C124 C 0.1658(2) 0.9285(2) 0.76807(19) 0.176(6) Uani 1 1 d D . . H12D H 0.1610 0.9163 0.7841 0.211 Uiso 1 1 calc R . . C125 C 0.1833(2) 0.9531(2) 0.77392(17) 0.140(5) Uani 1 1 d D . . C126 C 0.19098(19) 0.96931(19) 0.74904(17) 0.137(4) Uani 1 1 d D . . C127 C 0.2080(2) 0.9941(2) 0.75548(18) 0.196(7) Uani 1 1 d D . . H12E H 0.2133 1.0065 0.7397 0.235 Uiso 1 1 calc R . . C128 C 0.2180(3) 1.0021(3) 0.7839(2) 0.243(8) Uani 1 1 d D . . H12F H 0.2313 1.0175 0.7875 0.291 Uiso 1 1 calc R . . C129 C 0.2057(3) 0.9842(2) 0.8060(2) 0.225(8) Uani 1 1 d D . . H12G H 0.2073 0.9911 0.8255 0.270 Uiso 1 1 calc R . . C130 C 0.1913(3) 0.9572(3) 0.8021(3) 0.226(8) Uani 1 1 d D . . H13A H 0.1878 0.9436 0.8173 0.271 Uiso 1 1 calc R . . C131 C 0.30998(16) 0.9265(2) 0.6929(2) 0.105(3) Uani 1 1 d D . . C132 C 0.33856(18) 0.91492(17) 0.68778(19) 0.110(4) Uani 1 1 d D . . C133 C 0.34492(18) 0.88721(17) 0.7005(2) 0.122(4) Uani 1 1 d D . . H13B H 0.3639 0.8794 0.6981 0.146 Uiso 1 1 calc R . . C134 C 0.32438(17) 0.8710(2) 0.7163(2) 0.148(5) Uani 1 1 d D . . H13C H 0.3283 0.8518 0.7230 0.177 Uiso 1 1 calc R . . C135 C 0.29731(18) 0.88523(18) 0.7217(2) 0.131(4) Uani 1 1 d D . . C136 C 0.28973(16) 0.91222(19) 0.7086(2) 0.114(4) Uani 1 1 d D . . C137 C 0.26162(17) 0.9230(2) 0.71457(19) 0.124(4) Uani 1 1 d D . . H13D H 0.2558 0.9409 0.7060 0.148 Uiso 1 1 calc R . . C138 C 0.24189(19) 0.90809(19) 0.7327(2) 0.153(5) Uani 1 1 d D . . H13E H 0.2236 0.9163 0.7378 0.183 Uiso 1 1 calc R . . C139 C 0.2507(2) 0.87996(18) 0.7432(2) 0.166(5) Uani 1 1 d D . . H13F H 0.2379 0.8695 0.7557 0.199 Uiso 1 1 calc R . . C140 C 0.2779(2) 0.8673(3) 0.7356(3) 0.204(7) Uani 1 1 d D . . H14B H 0.2823 0.8475 0.7400 0.245 Uiso 1 1 calc R . . C151 C 0.1702(2) 1.06771(19) 0.5768(2) 0.096(3) Uani 1 1 d . . . C152 C 0.1633(2) 1.04634(18) 0.5972(2) 0.096(3) Uani 1 1 d . . . H15B H 0.1446 1.0460 0.6059 0.116 Uiso 1 1 calc R . . C153 C 0.1839(2) 1.0255(2) 0.6049(2) 0.097(3) Uani 1 1 d . . . C154 C 0.21142(19) 1.0253(2) 0.59169(19) 0.094(3) Uani 1 1 d . . . H15C H 0.2254 1.0110 0.5971 0.113 Uiso 1 1 calc R . . C155 C 0.21839(19) 1.04564(18) 0.5709(2) 0.081(3) Uani 1 1 d . . . C156 C 0.19941(18) 1.0679(2) 0.5641(2) 0.090(3) Uani 1 1 d . . . H15D H 0.2052 1.0832 0.5514 0.108 Uiso 1 1 calc R . . C157 C 0.1501(2) 1.0914(2) 0.5692(2) 0.097(3) Uani 1 1 d . . . C158 C 0.1728(2) 1.0039(2) 0.6281(2) 0.097(3) Uani 1 1 d . . . C161 C 0.30957(18) 1.0323(2) 0.6104(2) 0.091(3) Uani 1 1 d . . . C162 C 0.32503(19) 1.0580(2) 0.60809(18) 0.088(3) Uani 1 1 d . . . H16B H 0.3419 1.0609 0.6197 0.105 Uiso 1 1 calc R . . C163 C 0.31598(19) 1.0798(2) 0.58874(19) 0.084(3) Uani 1 1 d . . . C164 C 0.29011(18) 1.0739(2) 0.57245(18) 0.085(3) Uani 1 1 d . . . H16C H 0.2835 1.0883 0.5591 0.102 Uiso 1 1 calc R . . C165 C 0.27412(18) 1.04847(19) 0.57484(18) 0.081(3) Uani 1 1 d . . . C166 C 0.28340(19) 1.0268(2) 0.59425(19) 0.095(3) Uani 1 1 d . . . H16D H 0.2728 1.0092 0.5966 0.114 Uiso 1 1 calc R . . C167 C 0.32178(19) 1.0095(2) 0.6298(2) 0.085(3) Uani 1 1 d . . . C168 C 0.3320(2) 1.1060(2) 0.5837(2) 0.087(3) Uani 1 1 d . . . O14 O 0.40841(15) 1.17214(14) 0.57146(16) 0.129(3) Uani 1 1 d . . . N17 N 0.36927(16) 1.13863(16) 0.60248(17) 0.103(3) Uani 1 1 d . . . C104 C 0.38411(19) 1.1473(2) 0.6245(2) 0.118(4) Uani 1 1 d . . . H10F H 0.3688 1.1538 0.6380 0.142 Uiso 1 1 d R A . C141 C 0.4021(3) 1.1664(3) 0.62808(18) 0.094(5) Uiso 0.580(6) 1 d PD A 1 C142 C 0.4138(3) 1.1808(2) 0.6032(2) 0.097(5) Uiso 0.580(6) 1 d PD A 1 C143 C 0.4324(3) 1.2059(2) 0.6015(2) 0.090(5) Uiso 0.580(6) 1 d PD A 1 H14C H 0.4411 1.2132 0.5841 0.108 Uiso 0.580(6) 1 calc PR A 1 C144 C 0.4358(3) 1.2180(3) 0.62930(19) 0.124(6) Uiso 0.580(6) 1 d PD A 1 H14D H 0.4423 1.2377 0.6299 0.148 Uiso 0.580(6) 1 calc PR A 1 C145 C 0.4306(3) 1.2045(2) 0.65668(18) 0.138(7) Uiso 0.580(6) 1 d PD A 1 C146 C 0.4125(3) 1.1796(3) 0.65425(17) 0.118(6) Uiso 0.580(6) 1 d PD A 1 C147 C 0.4043(3) 1.1679(3) 0.68173(19) 0.113(6) Uiso 0.580(6) 1 d PD A 1 H14E H 0.3907 1.1523 0.6818 0.136 Uiso 0.580(6) 1 calc PR A 1 C148 C 0.4148(3) 1.1779(3) 0.7089(2) 0.153(8) Uiso 0.580(6) 1 d PD A 1 H14F H 0.4106 1.1681 0.7267 0.184 Uiso 0.580(6) 1 calc PR A 1 C149 C 0.4322(3) 1.2033(3) 0.7079(2) 0.131(7) Uiso 0.580(6) 1 d PD A 1 H14G H 0.4386 1.2110 0.7260 0.158 Uiso 0.580(6) 1 calc PR A 1 C150 C 0.4407(3) 1.2182(3) 0.6828(2) 0.129(7) Uiso 0.580(6) 1 d PD A 1 H15E H 0.4519 1.2356 0.6830 0.155 Uiso 0.580(6) 1 calc PR A 1 C41' C 0.4017(3) 1.1773(3) 0.61890(19) 0.056(5) Uiso 0.420(6) 1 d PD A 2 C42' C 0.4117(3) 1.1895(3) 0.5921(2) 0.076(6) Uiso 0.420(6) 1 d PD A 2 C43' C 0.4320(4) 1.2127(4) 0.5893(2) 0.122(9) Uiso 0.420(6) 1 d PD A 2 H43A H 0.4383 1.2199 0.5709 0.146 Uiso 0.420(6) 1 calc PR A 2 C44' C 0.4421(3) 1.2242(3) 0.6159(2) 0.094(7) Uiso 0.420(6) 1 d PD A 2 H44A H 0.4568 1.2388 0.6151 0.112 Uiso 0.420(6) 1 calc PR A 2 C45' C 0.4319(3) 1.2155(3) 0.6439(2) 0.100(7) Uiso 0.420(6) 1 d PD A 2 C46' C 0.4113(3) 1.1924(3) 0.64418(18) 0.111(8) Uiso 0.420(6) 1 d PD A 2 C47' C 0.4025(5) 1.1822(4) 0.6720(2) 0.164(12) Uiso 0.420(6) 1 d PD A 2 H47A H 0.3916 1.1647 0.6731 0.196 Uiso 0.420(6) 1 calc PR A 2 C48' C 0.4094(3) 1.1967(3) 0.6984(3) 0.119(8) Uiso 0.420(6) 1 d PD A 2 H48A H 0.4017 1.1904 0.7166 0.143 Uiso 0.420(6) 1 calc PR A 2 C49' C 0.4281(4) 1.2210(3) 0.6964(2) 0.111(8) Uiso 0.420(6) 1 d PD A 2 H49A H 0.4346 1.2300 0.7139 0.133 Uiso 0.420(6) 1 calc PR A 2 C50' C 0.4377(6) 1.2328(4) 0.6693(2) 0.219(17) Uiso 0.420(6) 1 d PD A 2 H50A H 0.4474 1.2510 0.6681 0.263 Uiso 0.420(6) 1 calc PR A 2 O21 O 0.12395(13) 1.19284(13) 0.51138(13) 0.107(2) Uani 1 1 d . . . O22 O 0.11647(14) 1.01596(14) 0.30921(13) 0.117(2) Uani 1 1 d . . . O23 O 0.10110(12) 1.10237(11) 0.51689(12) 0.0829(18) Uani 1 1 d . . . O24 O 0.10990(13) 1.05132(14) 0.39347(12) 0.103(2) Uani 1 1 d . . . N21 N 0.09584(15) 1.14947(16) 0.48367(17) 0.100(3) Uani 1 1 d . . . N22 N 0.08920(14) 1.12161(18) 0.47347(17) 0.102(2) Uani 1 1 d . C . H22A H 0.0823 1.1192 0.4558 0.123 Uiso 1 1 calc R . . N23 N 0.08597(16) 1.01169(17) 0.36066(18) 0.109(3) Uani 1 1 d . . . N24 N 0.08156(16) 1.01291(17) 0.39112(16) 0.107(3) Uani 1 1 d . . . H24A H 0.0705 1.0001 0.4000 0.128 Uiso 1 1 calc R . . C200 C 0.0471(3) 1.0000 0.5000 0.100(4) Uani 1 2 d S . . H20A H 0.0343 0.9891 0.4865 0.120 Uiso 0.50 1 calc PR . . H20B H 0.0343 1.0109 0.5135 0.120 Uiso 0.50 1 calc PR . . C201 C 0.09287(19) 1.16866(19) 0.4637(3) 0.108(4) Uani 1 1 d . C . H20C H 0.0863 1.1630 0.4449 0.130 Uiso 1 1 calc R B 1 C202 C 0.0688(2) 0.9958(2) 0.3442(2) 0.131(4) Uani 1 1 d . . . H20E H 0.0570 0.9810 0.3542 0.157 Uiso 1 1 d R D . C211 C 0.0998(3) 1.2002(2) 0.4699(2) 0.078(5) Uiso 0.50 1 d PD C 1 C212 C 0.1167(3) 1.2115(2) 0.4933(3) 0.090(6) Uiso 0.50 1 d PD C 1 C213 C 0.1284(4) 1.2403(2) 0.4949(3) 0.115(7) Uiso 0.50 1 d PD C 1 H21A H 0.1388 1.2473 0.5114 0.138 Uiso 0.50 1 calc PR C 1 C214 C 0.1229(3) 1.2576(3) 0.4696(2) 0.100(6) Uiso 0.50 1 d PD C 1 H21B H 0.1330 1.2756 0.4680 0.120 Uiso 0.50 1 calc PR C 1 C215 C 0.1035(3) 1.25033(19) 0.4464(2) 0.086(5) Uiso 0.50 1 d PD C 1 C216 C 0.0922(3) 1.2213(2) 0.4479(2) 0.142(9) Uiso 0.50 1 d PD C 1 C217 C 0.0751(3) 1.2128(3) 0.4232(3) 0.119(7) Uiso 0.50 1 d PD C 1 H21C H 0.0704 1.1928 0.4211 0.143 Uiso 0.50 1 calc PR C 1 C218 C 0.0647(3) 1.2326(2) 0.4016(3) 0.138(9) Uiso 0.50 1 d PD C 1 H21D H 0.0488 1.2282 0.3892 0.165 Uiso 0.50 1 calc PR C 1 C219 C 0.0799(3) 1.2596(3) 0.4002(3) 0.111(7) Uiso 0.50 1 d PD C 1 H21E H 0.0776 1.2714 0.3833 0.133 Uiso 0.50 1 calc PR C 1 C220 C 0.0985(4) 1.2698(3) 0.4229(3) 0.140(9) Uiso 0.50 1 d PD C 1 H22B H 0.1071 1.2886 0.4223 0.168 Uiso 0.50 1 calc PR C 1 C11' C 0.0977(3) 1.1961(2) 0.4602(3) 0.108(7) Uiso 0.50 1 d PD C 2 C12' C 0.1137(4) 1.2074(2) 0.4842(3) 0.097(7) Uiso 0.50 1 d PD C 2 C13' C 0.1201(4) 1.2376(2) 0.4888(3) 0.131(9) Uiso 0.50 1 d PD C 2 H13G H 0.1316 1.2442 0.5047 0.158 Uiso 0.50 1 calc PR C 2 C14' C 0.1081(3) 1.2572(3) 0.4677(3) 0.118(7) Uiso 0.50 1 d PD C 2 H14H H 0.1126 1.2773 0.4692 0.142 Uiso 0.50 1 calc PR C 2 C15' C 0.0896(4) 1.24788(19) 0.4444(3) 0.168(11) Uiso 0.50 1 d PD C 2 C16' C 0.0887(3) 1.21723(19) 0.4391(2) 0.094(6) Uiso 0.50 1 d PD C 2 C17' C 0.0762(4) 1.2079(3) 0.4121(3) 0.164(11) Uiso 0.50 1 d PD C 2 H17B H 0.0745 1.1877 0.4083 0.197 Uiso 0.50 1 calc PR C 2 C18' C 0.0662(5) 1.2282(2) 0.3908(3) 0.169(11) Uiso 0.50 1 d PD C 2 H18B H 0.0608 1.2220 0.3718 0.203 Uiso 0.50 1 calc PR C 2 C19' C 0.0645(4) 1.2582(3) 0.3990(3) 0.172(11) Uiso 0.50 1 d PD C 2 H19A H 0.0520 1.2711 0.3888 0.207 Uiso 0.50 1 calc PR C 2 C20' C 0.0816(4) 1.2684(3) 0.4226(3) 0.115(7) Uiso 0.50 1 d PD C 2 H20F H 0.0876 1.2882 0.4238 0.138 Uiso 0.50 1 calc PR C 2 C221 C 0.0665(2) 0.9986(4) 0.3128(3) 0.132(9) Uiso 0.50 1 d PD D 1 C222 C 0.0934(2) 1.0015(3) 0.29768(19) 0.055(4) Uiso 0.50 1 d PD D 1 C223 C 0.0963(2) 0.9966(4) 0.2672(2) 0.113(7) Uiso 0.50 1 d PD D 1 H22C H 0.1132 1.0021 0.2566 0.136 Uiso 0.50 1 calc PR D 1 C224 C 0.0722(2) 0.9829(4) 0.2539(3) 0.121(7) Uiso 0.50 1 d PD D 1 H22D H 0.0749 0.9728 0.2360 0.146 Uiso 0.50 1 calc PR D 1 C225 C 0.04370(19) 0.9838(4) 0.26674(18) 0.141(8) Uiso 0.50 1 d PD D 1 C226 C 0.0451(2) 0.9813(3) 0.29781(19) 0.077(5) Uiso 0.50 1 d PD D 1 C227 C 0.0205(2) 0.9699(3) 0.3133(2) 0.084(5) Uiso 0.50 1 d PD D 1 H22F H 0.0208 0.9688 0.3339 0.101 Uiso 0.50 1 calc PR D 1 C228 C -0.0044(2) 0.9603(3) 0.2975(2) 0.096(6) Uiso 0.50 1 d PD D 1 H22G H -0.0185 0.9479 0.3062 0.115 Uiso 0.50 1 calc PR D 1 C229 C -0.0072(2) 0.9701(6) 0.2684(3) 0.244(15) Uiso 0.50 1 d PD D 1 H22H H -0.0257 0.9749 0.2602 0.292 Uiso 0.50 1 calc PR D 1 C230 C 0.0189(2) 0.9724(4) 0.2519(3) 0.117(7) Uiso 0.50 1 d PD D 1 H23B H 0.0198 0.9666 0.2321 0.140 Uiso 0.50 1 calc PR D 1 C21' C 0.0713(2) 0.9905(3) 0.3138(2) 0.056(5) Uiso 0.50 1 d PD D 2 C22' C 0.0875(4) 1.0106(4) 0.2967(2) 0.150(11) Uiso 0.50 1 d PD D 2 C23' C 0.0884(3) 1.0069(4) 0.2660(2) 0.110(7) Uiso 0.50 1 d PD D 2 H23C H 0.1048 1.0127 0.2548 0.132 Uiso 0.50 1 calc PR D 2 C24' C 0.0636(3) 0.9941(3) 0.2533(3) 0.159(11) Uiso 0.50 1 d PD D 2 H24B H 0.0560 1.0010 0.2353 0.191 Uiso 0.50 1 calc PR D 2 C25' C 0.0500(3) 0.9705(3) 0.26831(19) 0.125(8) Uiso 0.50 1 d PD D 2 C26' C 0.0494(2) 0.9731(4) 0.2994(2) 0.160(12) Uiso 0.50 1 d PD D 2 C27' C 0.0258(3) 0.9588(4) 0.3136(3) 0.166(12) Uiso 0.50 1 d PD D 2 H27A H 0.0249 0.9594 0.3343 0.200 Uiso 0.50 1 calc PR D 2 C28' C 0.0034(3) 0.9437(4) 0.2983(2) 0.155(10) Uiso 0.50 1 d PD D 2 H28A H -0.0096 0.9307 0.3078 0.186 Uiso 0.50 1 calc PR D 2 C29' C 0.0016(2) 0.9491(4) 0.2681(2) 0.116(7) Uiso 0.50 1 d PD D 2 H29A H -0.0166 0.9485 0.2583 0.139 Uiso 0.50 1 calc PR D 2 C30' C 0.0279(3) 0.9555(4) 0.2526(3) 0.136(8) Uiso 0.50 1 d PD D 2 H30A H 0.0304 0.9499 0.2328 0.164 Uiso 0.50 1 calc PR D 2 C231 C 0.08788(19) 1.0692(2) 0.4789(2) 0.089(3) Uani 1 1 d . . . C232 C 0.07235(17) 1.0474(2) 0.4950(2) 0.087(3) Uani 1 1 d . C . H23D H 0.0678 1.0507 0.5150 0.104 Uiso 1 1 calc R . . C233 C 0.06407(19) 1.02204(18) 0.4823(2) 0.084(3) Uani 1 1 d . . . C234 C 0.07077(16) 1.0165(2) 0.45328(19) 0.088(3) Uani 1 1 d . C . H23E H 0.0646 0.9989 0.4443 0.106 Uiso 1 1 calc R . . C235 C 0.08747(17) 1.0381(2) 0.43665(18) 0.082(3) Uani 1 1 d . . . C236 C 0.09457(18) 1.06433(18) 0.4502(2) 0.087(3) Uani 1 1 d . C . H23F H 0.1042 1.0791 0.4393 0.105 Uiso 1 1 calc R . . C237 C 0.09371(17) 1.0972(2) 0.4919(2) 0.080(3) Uani 1 1 d . C . C238 C 0.0949(2) 1.0343(2) 0.4060(2) 0.092(3) Uani 1 1 d . C . O31 O 0.07046(15) 0.87879(16) 0.58543(15) 0.135(2) Uiso 1 1 d U . . N31 N 0.0375(2) 0.91392(19) 0.60060(19) 0.131(3) Uiso 1 1 d U . . C301 C 0.0621(3) 0.8970(3) 0.6064(3) 0.139(4) Uiso 1 1 d U . . C302 C 0.0213(3) 0.9113(3) 0.5715(3) 0.166(5) Uiso 1 1 d U . . C303 C 0.0298(2) 0.9333(2) 0.6218(2) 0.123(3) Uiso 1 1 d U . . O32 O 0.2503(2) 1.1279(2) 0.5336(2) 0.077(3) Uiso 0.50 1 d PU . . N32 N 0.2584(3) 1.1432(2) 0.5878(3) 0.068(3) Uiso 0.50 1 d PU . . C304 C 0.2591(4) 1.1394(4) 0.5567(5) 0.110(6) Uiso 0.50 1 d PU . . C305 C 0.2809(4) 1.1576(4) 0.6037(4) 0.104(6) Uiso 0.50 1 d PU . . C306 C 0.2317(5) 1.1290(5) 0.6016(5) 0.136(7) Uiso 0.50 1 d PU . . O33 O 0.3897(3) 0.8585(3) 0.5735(3) 0.114(4) Uiso 0.50 1 d PU . . N33 N 0.3679(5) 0.8212(5) 0.5637(4) 0.164(6) Uiso 0.50 1 d PU . . C307 C 0.3783(5) 0.8457(6) 0.5687(5) 0.125(7) Uiso 0.50 1 d PU . . C308 C 0.3463(5) 0.7910(5) 0.5492(5) 0.144(7) Uiso 0.50 1 d PU . . C309 C 0.3984(6) 0.7973(6) 0.5787(6) 0.174(9) Uiso 0.50 1 d PU . . O35 O 0.3550(2) 0.9034(2) 0.3364(2) 0.106(4) Uiso 0.50 1 d PDU . . N35 N 0.3366(3) 0.9090(3) 0.2910(2) 0.138(6) Uiso 0.50 1 d PDU . . C313 C 0.3414(4) 0.9171(3) 0.3199(3) 0.142(7) Uiso 0.50 1 d PDU . . C314 C 0.3470(4) 0.8816(3) 0.2779(4) 0.147(8) Uiso 0.50 1 d PDU . . C315 C 0.3192(5) 0.9286(4) 0.2709(4) 0.199(10) Uiso 0.50 1 d PDU . . N34 N 0.4550(3) 0.9115(3) 0.5416(3) 0.176(6) Uiso 0.50 1 d PDU . . O34 O 0.4904(4) 0.9269(4) 0.5131(5) 0.259(8) Uiso 0.50 1 d PDU . . C310 C 0.4711(3) 0.9052(3) 0.5181(3) 0.131(6) Uiso 0.50 1 d PDU . . C311 C 0.4616(4) 0.9390(4) 0.5608(4) 0.174(9) Uiso 0.50 1 d PDU . . C312 C 0.4223(3) 0.9027(5) 0.5465(5) 0.173(9) Uiso 0.50 1 d PDU . . O402 O 0.2501(3) 0.8369(3) 0.5149(3) 0.123(4) Uiso 0.50 1 d PU . . C317 C 0.3171(4) 1.2610(4) 0.6953(6) 0.315(15) Uiso 0.50 1 d PDU . . N36 N 0.3422(4) 1.2457(3) 0.6781(5) 0.274(10) Uiso 0.50 1 d PDU . . C316 C 0.3323(5) 1.2136(4) 0.6708(7) 0.292(14) Uiso 0.50 1 d PDU . . C318 C 0.3635(4) 1.2595(4) 0.6642(6) 0.288(11) Uiso 0.50 1 d PDU . . O36 O 0.3762(5) 1.2821(5) 0.6669(6) 0.337(12) Uiso 0.50 1 d PDU . . C402 C 0.2383(6) 0.8222(6) 0.5448(6) 0.186(10) Uiso 0.50 1 d PU . . N37 N 0.5000 1.0000 0.6227(3) 0.333(7) Uiso 1 2 d SDU . . O37 O 0.5000 1.0000 0.5748(3) 0.362(8) Uiso 1 2 d SDU . . C320 C 0.5240(4) 1.0219(5) 0.6152(5) 0.260(8) Uiso 0.50 1 d PDU . . C321 C 0.4851(5) 0.9868(5) 0.5969(3) 0.292(9) Uiso 0.50 1 d PDU . . C319 C 0.4790(4) 1.0102(6) 0.6464(4) 0.287(10) Uiso 0.50 1 d PDU . . O3W O 0.2978(6) 0.9810(7) 0.2239(7) 0.319(14) Uiso 0.50 1 d P . . O5W O 0.3096(14) 0.9418(14) 0.1905(13) 0.32(3) Uiso 0.25 1 d P . . O1W O 0.3315(5) 0.9067(5) 0.1783(5) 0.252(9) Uiso 0.50 1 d P . . O4W O 0.4545(5) 0.9874(5) 0.7488(5) 0.222(8) Uiso 0.50 1 d P . . O401 O 0.1735(10) 1.0000 0.5000 0.57(2) Uiso 1 2 d S . 1 C401 C 0.1552(10) 0.9724(11) 0.5131(10) 0.31(2) Uiso 0.50 1 d P . 1 O2W O 0.2132(6) 1.0000 0.5000 0.194(10) Uiso 0.50 2 d SP E 2 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 0.0778(3) 0.0776(3) 0.1280(4) 0.0032(3) 0.0131(3) 0.0103(3) Ce2 0.0951(4) 0.1299(5) 0.0952(4) 0.0244(4) 0.0064(3) 0.0030(4) O11 0.086(4) 0.084(4) 0.155(5) 0.021(4) 0.017(4) 0.016(3) N11 0.062(4) 0.113(6) 0.135(6) 0.001(5) 0.018(4) 0.011(4) O12 0.130(5) 0.136(5) 0.095(4) 0.037(4) 0.005(4) -0.012(4) N12 0.086(5) 0.103(5) 0.117(6) 0.031(4) 0.014(5) 0.033(5) O13 0.084(4) 0.161(6) 0.091(4) 0.002(4) -0.014(3) 0.012(4) N13 0.090(5) 0.118(6) 0.088(5) 0.022(5) 0.023(4) 0.019(5) N14 0.086(5) 0.113(6) 0.119(6) 0.018(5) 0.011(5) 0.006(5) O15 0.082(4) 0.089(4) 0.118(5) 0.017(3) 0.017(4) 0.026(3) N15 0.090(5) 0.155(7) 0.085(5) 0.002(5) -0.028(4) 0.050(5) O16 0.082(4) 0.111(4) 0.124(5) 0.023(4) 0.002(4) 0.011(4) N16 0.055(4) 0.141(7) 0.117(6) 0.015(5) 0.009(4) 0.029(4) O17 0.073(4) 0.128(5) 0.089(4) -0.013(3) -0.015(3) 0.009(4) O18 0.083(4) 0.090(4) 0.091(4) -0.010(3) -0.003(3) 0.004(3) N18 0.110(6) 0.118(6) 0.103(6) -0.020(5) 0.006(5) 0.006(5) C100 0.066(5) 0.071(6) 0.118(7) 0.001(5) -0.030(5) -0.003(5) C101 0.052(5) 0.116(8) 0.132(8) 0.011(6) 0.031(5) 0.017(5) C102 0.101(7) 0.137(9) 0.089(7) 0.022(7) -0.015(6) 0.001(6) C103 0.089(7) 0.150(9) 0.091(7) 0.032(7) 0.007(6) 0.002(7) C111 0.068(6) 0.100(7) 0.130(8) -0.014(6) 0.054(6) -0.005(5) C112 0.069(6) 0.102(7) 0.128(8) -0.007(6) 0.061(6) -0.013(5) C113 0.072(6) 0.155(10) 0.221(12) -0.058(8) 0.052(7) 0.024(7) C114 0.095(7) 0.117(8) 0.172(11) -0.007(8) -0.010(7) 0.028(7) C115 0.070(6) 0.111(8) 0.171(10) -0.014(7) 0.014(7) 0.005(6) C116 0.086(7) 0.119(8) 0.134(9) 0.005(6) -0.007(7) 0.007(6) C117 0.107(8) 0.190(12) 0.202(12) -0.037(10) 0.061(9) 0.031(8) C118 0.118(9) 0.168(11) 0.184(12) -0.018(9) 0.025(9) 0.005(8) C119 0.129(9) 0.199(12) 0.121(9) -0.025(8) 0.071(7) -0.009(8) C120 0.114(8) 0.147(10) 0.148(10) -0.042(8) 0.059(8) -0.022(7) C121 0.101(7) 0.140(9) 0.106(8) 0.029(7) -0.008(6) -0.001(7) C122 0.140(9) 0.155(9) 0.062(6) 0.050(6) 0.020(6) 0.043(7) C123 0.167(10) 0.242(13) 0.081(7) 0.041(8) -0.024(7) 0.073(10) C124 0.095(8) 0.304(16) 0.128(10) 0.098(10) 0.030(7) 0.022(9) C125 0.141(10) 0.200(12) 0.077(7) -0.012(8) -0.030(7) 0.031(9) C126 0.125(8) 0.231(12) 0.056(6) -0.030(8) -0.045(6) 0.061(8) C127 0.191(13) 0.319(18) 0.079(8) -0.074(10) -0.057(8) 0.052(12) C128 0.218(16) 0.304(19) 0.206(16) -0.090(15) 0.023(14) 0.034(15) C129 0.244(16) 0.35(2) 0.080(9) 0.011(11) 0.002(10) 0.149(15) C130 0.167(13) 0.36(2) 0.156(13) -0.076(15) -0.008(11) 0.026(15) C131 0.068(6) 0.147(9) 0.101(7) 0.055(6) -0.011(5) 0.021(6) C132 0.116(8) 0.119(8) 0.096(8) 0.007(6) -0.028(6) 0.015(7) C133 0.111(8) 0.133(9) 0.122(8) 0.015(7) 0.015(7) 0.039(7) C134 0.136(9) 0.149(10) 0.158(11) 0.029(9) 0.004(8) 0.020(8) C135 0.106(8) 0.132(9) 0.154(10) 0.023(8) 0.023(8) 0.001(7) C136 0.095(7) 0.134(9) 0.114(8) 0.032(7) 0.004(6) 0.020(7) C137 0.123(9) 0.160(10) 0.088(7) 0.052(7) 0.024(6) 0.010(7) C138 0.110(9) 0.201(12) 0.147(10) 0.058(9) 0.004(8) 0.017(8) C139 0.220(13) 0.106(8) 0.172(11) 0.070(8) -0.040(10) -0.030(9) C140 0.119(10) 0.170(12) 0.32(2) 0.078(12) 0.016(12) 0.055(9) C151 0.121(8) 0.069(6) 0.097(7) 0.012(5) 0.001(6) 0.016(6) C152 0.096(7) 0.072(6) 0.121(8) 0.012(6) 0.000(6) 0.022(5) C153 0.104(7) 0.079(6) 0.107(7) 0.024(5) -0.011(6) -0.015(6) C154 0.070(6) 0.108(7) 0.103(7) -0.002(6) 0.022(5) 0.003(5) C155 0.072(6) 0.067(6) 0.105(7) 0.020(5) -0.016(5) 0.002(5) C156 0.060(6) 0.096(7) 0.114(7) 0.005(6) 0.013(5) 0.004(5) C157 0.071(6) 0.129(8) 0.090(7) 0.022(6) 0.014(6) 0.016(6) C158 0.055(6) 0.107(7) 0.130(9) 0.013(7) 0.003(6) 0.020(6) C161 0.064(6) 0.105(7) 0.105(7) 0.005(6) 0.005(5) 0.015(5) C162 0.082(6) 0.103(7) 0.079(6) -0.024(5) -0.001(5) -0.004(5) C163 0.071(6) 0.110(7) 0.073(6) -0.016(5) 0.006(5) 0.013(5) C164 0.080(6) 0.104(7) 0.070(6) 0.015(5) 0.005(5) 0.021(5) C165 0.075(6) 0.081(6) 0.085(6) 0.019(5) -0.003(5) -0.005(5) C166 0.074(6) 0.125(8) 0.087(7) 0.004(6) 0.005(5) 0.000(6) C167 0.052(5) 0.119(8) 0.084(7) -0.026(6) 0.005(5) -0.003(5) C168 0.102(7) 0.074(6) 0.085(7) -0.021(6) -0.003(6) -0.011(6) O14 0.132(5) 0.093(5) 0.164(6) -0.009(4) 0.006(5) 0.008(4) N17 0.081(5) 0.095(5) 0.132(6) -0.040(5) 0.023(5) -0.010(4) C104 0.088(7) 0.114(7) 0.153(9) -0.069(7) -0.031(6) -0.016(6) O21 0.101(4) 0.095(4) 0.125(5) 0.002(4) 0.017(4) 0.010(4) O22 0.109(5) 0.139(5) 0.103(5) 0.013(4) -0.002(4) -0.004(4) O23 0.083(4) 0.066(4) 0.100(4) -0.005(3) -0.006(3) 0.009(3) O24 0.095(4) 0.121(5) 0.092(4) 0.032(4) -0.009(3) -0.006(4) N21 0.097(5) 0.064(5) 0.138(6) 0.013(5) 0.027(5) 0.010(4) N22 0.080(5) 0.108(6) 0.118(6) 0.020(5) -0.014(4) 0.001(5) N23 0.084(5) 0.126(6) 0.117(7) 0.031(5) 0.005(5) -0.008(5) N24 0.092(5) 0.138(7) 0.091(6) 0.056(5) 0.022(5) -0.002(5) C200 0.079(9) 0.126(11) 0.095(10) -0.022(9) 0.000 0.000 C201 0.093(7) 0.064(6) 0.168(10) 0.018(6) 0.003(7) -0.003(5) C202 0.125(8) 0.137(9) 0.131(9) -0.021(7) -0.045(7) -0.034(7) C231 0.087(6) 0.086(7) 0.095(7) 0.008(6) -0.006(5) -0.009(5) C232 0.069(6) 0.090(7) 0.100(7) 0.009(6) 0.000(5) 0.013(5) C233 0.089(6) 0.050(5) 0.113(8) 0.020(5) 0.009(6) 0.005(5) C234 0.059(5) 0.126(8) 0.079(6) -0.007(6) -0.004(5) 0.022(5) C235 0.056(5) 0.120(7) 0.070(6) 0.029(6) 0.017(4) 0.001(5) C236 0.078(6) 0.061(6) 0.123(8) -0.001(6) -0.001(6) -0.009(5) C237 0.050(5) 0.088(7) 0.103(7) -0.009(6) -0.001(5) 0.011(5) C238 0.090(7) 0.068(6) 0.117(8) 0.013(6) -0.032(6) -0.023(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O13 2.143(7) 18_556 ? Ce1 O11 2.195(6) . ? Ce1 O21 2.196(6) . ? Ce1 O17 2.376(5) 18_556 ? Ce1 O15 2.422(5) . ? Ce1 O23 2.467(5) . ? Ce1 N21 2.579(8) . ? Ce1 N11 2.587(7) . ? Ce1 N15 2.608(7) 18_556 ? Ce2 O22 2.158(6) 4_576 ? Ce2 O12 2.218(6) . ? Ce2 O14 2.221(7) 19_564 ? Ce2 O16 2.350(6) . ? Ce2 O24 2.404(6) 4_576 ? Ce2 O18 2.469(5) 19_564 ? Ce2 N13 2.513(7) . ? Ce2 N23 2.614(7) 4_576 ? Ce2 N17 2.668(8) 19_564 ? O11 C112 1.263(8) . ? N11 C101 1.246(9) . ? N11 N12 1.379(9) . ? O12 C122 1.288(9) . ? N12 C157 1.296(10) . ? N12 H12A 0.8600 . ? O13 C132 1.331(9) . ? O13 Ce1 2.143(6) 19_564 ? N13 C102 1.236(10) . ? N13 N14 1.369(9) . ? N14 C158 1.280(11) . ? N14 H14A 0.8600 . ? O15 C157 1.210(10) . ? N15 C103 1.310(10) . ? N15 N16 1.390(9) . ? N15 Ce1 2.608(7) 19_564 ? O16 C158 1.212(9) . ? N16 C167 1.284(10) . ? N16 H16A 0.8600 . ? O17 C167 1.249(9) . ? O17 Ce1 2.376(5) 19_564 ? O18 C168 1.219(10) . ? O18 Ce2 2.469(5) 18_556 ? N18 C168 1.352(11) . ? N18 N17 1.373(9) . ? N18 H18A 0.8600 . ? C100 C165 1.484(11) . ? C100 C155 1.507(11) . ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? C101 C111 1.430(10) . ? C101 H10C 0.9300 . ? C102 C121 1.381(12) . ? C102 H10D 0.9300 . ? C103 C131 1.411(11) . ? C103 H10E 0.9300 . ? C111 C112 1.357(7) . ? C111 C116 1.378(10) . ? C112 C113 1.394(7) . ? C113 C114 1.364(8) . ? C113 H11A 0.9300 . ? C114 C115 1.400(8) . ? C114 H11B 0.9300 . ? C115 C116 1.391(7) . ? C115 C120 1.413(11) . ? C116 C117 1.389(8) . ? C117 C118 1.371(8) . ? C117 H11C 0.9300 . ? C118 C119 1.404(8) . ? C118 H11D 0.9300 . ? C119 C120 1.382(8) . ? C119 H11E 0.9300 . ? C120 H12B 0.9300 . ? C121 C126 1.365(11) . ? C121 C122 1.378(8) . ? C122 C123 1.397(8) . ? C123 C124 1.389(8) . ? C123 H12C 0.9300 . ? C124 C125 1.381(8) . ? C124 H12D 0.9300 . ? C125 C130 1.331(14) . ? C125 C126 1.378(8) . ? C126 C127 1.384(8) . ? C127 C128 1.398(8) . ? C127 H12E 0.9300 . ? C128 C129 1.394(9) . ? C128 H12F 0.9300 . ? C129 C130 1.386(9) . ? C129 H12G 0.9300 . ? C130 H13A 0.9300 . ? C131 C136 1.320(10) . ? C131 C132 1.405(7) . ? C132 C133 1.399(7) . ? C133 C134 1.373(8) . ? C133 H13B 0.9300 . ? C134 C135 1.394(8) . ? C134 H13C 0.9300 . ? C135 C140 1.346(13) . ? C135 C136 1.389(8) . ? C136 C137 1.378(7) . ? C137 C138 1.377(8) . ? C137 H13D 0.9300 . ? C138 C139 1.406(8) . ? C138 H13E 0.9300 . ? C139 C140 1.390(8) . ? C139 H13F 0.9300 . ? C140 H14B 0.9300 . ? C151 C152 1.365(11) . ? C151 C156 1.429(11) . ? C151 C157 1.438(12) . ? C152 C153 1.361(11) . ? C152 H15B 0.9300 . ? C153 C154 1.373(11) . ? C153 C158 1.506(13) . ? C154 C155 1.342(11) . ? C154 H15C 0.9300 . ? C155 C156 1.351(10) . ? C156 H15D 0.9300 . ? C161 C162 1.353(11) . ? C161 C166 1.404(11) . ? C161 C167 1.451(12) . ? C162 C163 1.371(11) . ? C162 H16B 0.9300 . ? C163 C168 1.397(12) . ? C163 C164 1.399(11) . ? C164 C165 1.353(11) . ? C164 H16C 0.9300 . ? C165 C166 1.372(11) . ? C166 H16D 0.9300 . ? O14 C42' 1.218(13) . ? O14 C142 1.497(12) . ? O14 Ce2 2.221(7) 18_556 ? N17 C104 1.257(10) . ? N17 Ce2 2.668(8) 18_556 ? C104 C141 1.190(12) . ? C104 C41' 1.584(14) . ? C104 H10F 0.9601 . ? C141 C142 1.395(9) . ? C141 C146 1.399(8) . ? C142 C143 1.406(9) . ? C143 C144 1.373(8) . ? C143 H14C 0.9300 . ? C144 C145 1.393(8) . ? C144 H14D 0.9300 . ? C145 C146 1.384(9) . ? C145 C150 1.401(9) . ? C146 C147 1.393(8) . ? C147 C148 1.385(9) . ? C147 H14E 0.9300 . ? C148 C149 1.385(9) . ? C148 H14F 0.9300 . ? C149 C150 1.369(9) . ? C149 H14G 0.9300 . ? C150 H15E 0.9300 . ? C41' C46' 1.391(8) . ? C41' C42' 1.397(9) . ? C42' C43' 1.396(9) . ? C43' C44' 1.378(9) . ? C43' H43A 0.9300 . ? C44' C45' 1.395(9) . ? C44' H44A 0.9300 . ? C45' C46' 1.392(9) . ? C45' C50' 1.401(9) . ? C46' C47' 1.390(9) . ? C47' C48' 1.388(9) . ? C47' H47A 0.9300 . ? C48' C49' 1.380(9) . ? C48' H48A 0.9300 . ? C49' C50' 1.396(9) . ? C49' H49A 0.9300 . ? C50' H50A 0.9300 . ? O21 C212 1.214(12) . ? O21 C12' 1.459(13) . ? O22 C222 1.329(11) . ? O22 C22' 1.439(16) . ? O22 Ce2 2.158(6) 4_576 ? O23 C237 1.195(9) . ? O24 C238 1.165(10) . ? O24 Ce2 2.404(6) 4_576 ? N21 C201 1.251(11) . ? N21 N22 1.366(9) . ? N22 C237 1.390(11) . ? N22 H22A 0.8600 . ? N23 C202 1.284(11) . ? N23 N24 1.384(9) . ? N23 Ce2 2.614(7) 4_576 ? N24 C238 1.317(11) . ? N24 H24A 0.8600 . ? C200 C233 1.481(10) . ? C200 C233 1.481(10) 4_576 ? C200 H20A 0.9700 . ? C200 H20B 0.9700 . ? C201 C11' 1.263(12) . ? C201 C211 1.479(13) . ? C201 H20C 0.9300 . ? C202 C21' 1.393(14) . ? C202 C221 1.423(15) . ? C202 H20E 0.9596 . ? C211 C212 1.393(9) . ? C211 C216 1.408(8) . ? C212 C213 1.398(9) . ? C213 C214 1.402(9) . ? C213 H21A 0.9300 . ? C214 C215 1.395(9) . ? C214 H21B 0.9300 . ? C215 C220 1.391(9) . ? C215 C216 1.404(8) . ? C216 C217 1.400(9) . ? C217 C218 1.399(9) . ? C217 H21C 0.9300 . ? C218 C219 1.395(9) . ? C218 H21D 0.9300 . ? C219 C220 1.393(9) . ? C219 H21E 0.9300 . ? C220 H22B 0.9300 . ? C11' C12' 1.393(9) . ? C11' C16' 1.403(9) . ? C12' C13' 1.400(9) . ? C13' C14' 1.402(9) . ? C13' H13G 0.9300 . ? C14' C15' 1.397(9) . ? C14' H14H 0.9300 . ? C15' C20' 1.392(9) . ? C15' C16' 1.399(8) . ? C16' C17' 1.399(9) . ? C17' C18' 1.397(9) . ? C17' H17B 0.9300 . ? C18' C19' 1.398(9) . ? C18' H18B 0.9300 . ? C19' C20' 1.390(9) . ? C19' H19A 0.9300 . ? C20' H20F 0.9300 . ? C221 C222 1.392(9) . ? C221 C226 1.409(9) . ? C222 C223 1.391(8) . ? C223 C224 1.381(9) . ? C223 H22C 0.9300 . ? C224 C225 1.404(8) . ? C224 H22D 0.9300 . ? C225 C230 1.397(9) . ? C225 C226 1.402(8) . ? C226 C227 1.400(8) . ? C227 C228 1.392(9) . ? C227 H22F 0.9300 . ? C228 C229 1.388(9) . ? C228 H22G 0.9300 . ? C229 C230 1.390(9) . ? C229 H22H 0.9300 . ? C230 H23B 0.9300 . ? C21' C22' 1.391(9) . ? C21' C26' 1.412(9) . ? C22' C23' 1.391(9) . ? C23' C24' 1.381(9) . ? C23' H23C 0.9300 . ? C24' C25' 1.397(9) . ? C24' H24B 0.9300 . ? C25' C30' 1.394(9) . ? C25' C26' 1.400(8) . ? C26' C27' 1.397(9) . ? C27' C28' 1.395(9) . ? C27' H27A 0.9300 . ? C28' C29' 1.381(9) . ? C28' H28A 0.9300 . ? C29' C30' 1.397(9) . ? C29' H29A 0.9300 . ? C30' H30A 0.9300 . ? C231 C236 1.346(11) . ? C231 C232 1.406(11) . ? C231 C237 1.408(12) . ? C232 C233 1.329(11) . ? C232 H23D 0.9300 . ? C233 C234 1.361(11) . ? C234 C235 1.436(11) . ? C234 H23E 0.9300 . ? C235 C236 1.363(11) . ? C235 C238 1.425(12) . ? C236 H23F 0.9300 . ? O31 C301 1.303(12) . ? N31 C303 1.337(12) . ? N31 C301 1.367(13) . ? N31 C302 1.503(14) . ? O32 C304 1.23(2) . ? N32 C305 1.398(19) . ? N32 C304 1.41(2) . ? N32 C306 1.49(2) . ? O33 C307 0.80(3) . ? N33 C307 1.22(3) . ? N33 C308 1.79(3) . ? N33 C309 1.87(3) . ? O35 C313 1.142(13) . ? N35 C313 1.365(13) . ? N35 C314 1.442(14) . ? N35 C315 1.483(14) . ? N34 C310 1.313(14) . ? N34 C311 1.535(15) . ? N34 C312 1.539(14) . ? O34 C310 1.320(15) . ? O34 O34 1.46(3) 3_656 ? O402 C402 1.59(3) . ? C317 N36 1.530(16) . ? N36 C318 1.301(15) . ? N36 C316 1.543(15) . ? C318 O36 1.171(16) . ? N37 C321 1.464(14) . ? N37 C321 1.464(14) 2_675 ? N37 C319 1.494(14) . ? N37 C319 1.494(15) 2_675 ? N37 C320 1.496(14) 2_675 ? N37 C320 1.496(14) . ? O37 C321 1.335(15) . ? O37 C321 1.335(15) 2_675 ? C320 C321 1.00(3) 2_675 ? C320 C319 2.01(3) 2_675 ? C321 C320 1.00(3) 2_675 ? C321 C321 1.78(3) 2_675 ? C319 C320 2.01(3) 2_675 ? O401 C401 1.60(5) 4_576 ? O401 C401 1.60(5) . ? 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 O13 Ce1 O11 88.4(2) 18_556 . ? O13 Ce1 O21 87.5(2) 18_556 . ? O11 Ce1 O21 88.2(2) . . ? O13 Ce1 O17 129.3(2) 18_556 18_556 ? O11 Ce1 O17 141.3(2) . 18_556 ? O21 Ce1 O17 85.5(2) . 18_556 ? O13 Ce1 O15 85.7(2) 18_556 . ? O11 Ce1 O15 127.9(2) . . ? O21 Ce1 O15 142.9(2) . . ? O17 Ce1 O15 71.21(19) 18_556 . ? O13 Ce1 O23 142.6(2) 18_556 . ? O11 Ce1 O23 83.23(19) . . ? O21 Ce1 O23 128.4(2) . . ? O17 Ce1 O23 71.35(18) 18_556 . ? O15 Ce1 O23 71.48(18) . . ? O13 Ce1 N21 151.2(2) 18_556 . ? O11 Ce1 N21 79.3(2) . . ? O21 Ce1 N21 66.4(2) . . ? O17 Ce1 N21 63.3(2) 18_556 . ? O15 Ce1 N21 122.4(2) . . ? O23 Ce1 N21 62.0(2) . . ? O13 Ce1 N11 74.3(2) 18_556 . ? O11 Ce1 N11 66.8(2) . . ? O21 Ce1 N11 149.0(2) . . ? O17 Ce1 N11 125.4(2) 18_556 . ? O15 Ce1 N11 61.8(2) . . ? O23 Ce1 N11 68.8(2) . . ? N21 Ce1 N11 122.5(2) . . ? O13 Ce1 N15 67.2(2) 18_556 18_556 ? O11 Ce1 N15 152.6(2) . 18_556 ? O21 Ce1 N15 78.8(2) . 18_556 ? O17 Ce1 N15 62.2(2) 18_556 18_556 ? O15 Ce1 N15 65.0(2) . 18_556 ? O23 Ce1 N15 123.7(2) . 18_556 ? N21 Ce1 N15 116.1(2) . 18_556 ? N11 Ce1 N15 115.1(2) . 18_556 ? O22 Ce2 O12 84.2(2) 4_576 . ? O22 Ce2 O14 81.5(2) 4_576 19_564 ? O12 Ce2 O14 82.3(2) . 19_564 ? O22 Ce2 O16 89.5(2) 4_576 . ? O12 Ce2 O16 128.4(2) . . ? O14 Ce2 O16 147.1(2) 19_564 . ? O22 Ce2 O24 128.9(2) 4_576 4_576 ? O12 Ce2 O24 143.3(2) . 4_576 ? O14 Ce2 O24 87.2(2) 19_564 4_576 ? O16 Ce2 O24 74.1(2) . 4_576 ? O22 Ce2 O18 147.8(2) 4_576 19_564 ? O12 Ce2 O18 89.4(2) . 19_564 ? O14 Ce2 O18 128.9(2) 19_564 19_564 ? O16 Ce2 O18 70.01(19) . 19_564 ? O24 Ce2 O18 70.33(18) 4_576 19_564 ? O22 Ce2 N13 77.0(2) 4_576 . ? O12 Ce2 N13 67.3(2) . . ? O14 Ce2 N13 144.1(2) 19_564 . ? O16 Ce2 N13 61.3(2) . . ? O24 Ce2 N13 128.6(2) 4_576 . ? O18 Ce2 N13 71.5(2) 19_564 . ? O22 Ce2 N23 68.0(2) 4_576 4_576 ? O12 Ce2 N23 148.1(2) . 4_576 ? O14 Ce2 N23 78.5(2) 19_564 4_576 ? O16 Ce2 N23 68.8(2) . 4_576 ? O24 Ce2 N23 60.9(2) 4_576 4_576 ? O18 Ce2 N23 122.4(2) 19_564 4_576 ? N13 Ce2 N23 118.1(2) . 4_576 ? O22 Ce2 N17 143.4(2) 4_576 19_564 ? O12 Ce2 N17 74.9(2) . 19_564 ? O14 Ce2 N17 66.4(2) 19_564 19_564 ? O16 Ce2 N17 127.0(2) . 19_564 ? O24 Ce2 N17 68.7(2) 4_576 19_564 ? O18 Ce2 N17 62.8(2) 19_564 19_564 ? N13 Ce2 N17 119.7(2) . 19_564 ? N23 Ce2 N17 118.9(2) 4_576 19_564 ? C112 O11 Ce1 150.4(5) . . ? C101 N11 N12 113.8(8) . . ? C101 N11 Ce1 132.5(6) . . ? N12 N11 Ce1 113.6(5) . . ? C122 O12 Ce2 132.0(6) . . ? C157 N12 N11 118.6(8) . . ? C157 N12 H12A 120.7 . . ? N11 N12 H12A 120.7 . . ? C132 O13 Ce1 146.8(5) . 19_564 ? C102 N13 N14 117.5(8) . . ? C102 N13 Ce2 128.9(7) . . ? N14 N13 Ce2 113.5(5) . . ? C158 N14 N13 115.1(8) . . ? C158 N14 H14A 122.4 . . ? N13 N14 H14A 122.4 . . ? C157 O15 Ce1 125.5(6) . . ? C103 N15 N16 115.1(7) . . ? C103 N15 Ce1 133.4(6) . 19_564 ? N16 N15 Ce1 111.4(5) . 19_564 ? C158 O16 Ce2 123.4(6) . . ? C167 N16 N15 119.6(7) . . ? C167 N16 H16A 120.2 . . ? N15 N16 H16A 120.2 . . ? C167 O17 Ce1 124.9(6) . 19_564 ? C168 O18 Ce2 122.1(6) . 18_556 ? C168 N18 N17 121.7(8) . . ? C168 N18 H18A 119.2 . . ? N17 N18 H18A 119.2 . . ? C165 C100 C155 114.4(7) . . ? C165 C100 H10A 108.7 . . ? C155 C100 H10A 108.7 . . ? C165 C100 H10B 108.7 . . ? C155 C100 H10B 108.7 . . ? H10A C100 H10B 107.6 . . ? N11 C101 C111 124.1(9) . . ? N11 C101 H10C 117.9 . . ? C111 C101 H10C 117.9 . . ? N13 C102 C121 128.4(10) . . ? N13 C102 H10D 115.8 . . ? C121 C102 H10D 115.8 . . ? N15 C103 C131 124.9(9) . . ? N15 C103 H10E 117.6 . . ? C131 C103 H10E 117.6 . . ? C112 C111 C116 116.5(7) . . ? C112 C111 C101 123.9(7) . . ? C116 C111 C101 119.5(7) . . ? O11 C112 C111 120.8(7) . . ? O11 C112 C113 113.9(7) . . ? C111 C112 C113 125.3(7) . . ? C114 C113 C112 115.4(8) . . ? C114 C113 H11A 122.3 . . ? C112 C113 H11A 122.3 . . ? C113 C114 C115 123.3(8) . . ? C113 C114 H11B 118.4 . . ? C115 C114 H11B 118.4 . . ? C116 C115 C114 116.8(7) . . ? C116 C115 C120 125.4(8) . . ? C114 C115 C120 117.7(7) . . ? C111 C116 C117 121.1(7) . . ? C111 C116 C115 122.5(7) . . ? C117 C116 C115 115.7(8) . . ? C118 C117 C116 123.3(8) . . ? C118 C117 H11C 118.4 . . ? C116 C117 H11C 118.4 . . ? C117 C118 C119 116.5(9) . . ? C117 C118 H11D 121.7 . . ? C119 C118 H11D 121.7 . . ? C120 C119 C118 125.2(8) . . ? C120 C119 H11E 117.4 . . ? C118 C119 H11E 117.4 . . ? C119 C120 C115 113.1(8) . . ? C119 C120 H12B 123.5 . . ? C115 C120 H12B 123.5 . . ? C126 C121 C122 115.5(8) . . ? C126 C121 C102 126.3(8) . . ? C122 C121 C102 117.9(9) . . ? O12 C122 C121 123.9(8) . . ? O12 C122 C123 111.6(7) . . ? C121 C122 C123 124.5(8) . . ? C124 C123 C122 114.0(8) . . ? C124 C123 H12C 123.0 . . ? C122 C123 H12C 123.0 . . ? C125 C124 C123 125.7(8) . . ? C125 C124 H12D 117.2 . . ? C123 C124 H12D 117.2 . . ? C130 C125 C126 129.2(9) . . ? C130 C125 C124 116.4(8) . . ? C126 C125 C124 114.3(8) . . ? C121 C126 C125 125.7(8) . . ? C121 C126 C127 121.1(8) . . ? C125 C126 C127 113.3(7) . . ? C126 C127 C128 125.0(9) . . ? C126 C127 H12E 117.5 . . ? C128 C127 H12E 117.5 . . ? C129 C128 C127 112.2(9) . . ? C129 C128 H12F 123.9 . . ? C127 C128 H12F 123.9 . . ? C130 C129 C128 126.9(11) . . ? C130 C129 H12G 116.5 . . ? C128 C129 H12G 116.5 . . ? C125 C130 C129 111.4(11) . . ? C125 C130 H13A 124.3 . . ? C129 C130 H13A 124.3 . . ? C136 C131 C132 122.5(8) . . ? C136 C131 C103 119.0(7) . . ? C132 C131 C103 118.1(8) . . ? O13 C132 C133 115.9(7) . . ? O13 C132 C131 127.3(7) . . ? C133 C132 C131 116.8(8) . . ? C134 C133 C132 123.1(8) . . ? C134 C133 H13B 118.5 . . ? C132 C133 H13B 118.5 . . ? C133 C134 C135 115.6(8) . . ? C133 C134 H13C 122.2 . . ? C135 C134 H13C 122.2 . . ? C140 C135 C136 124.1(8) . . ? C140 C135 C134 111.9(8) . . ? C136 C135 C134 122.8(8) . . ? C131 C136 C137 124.4(8) . . ? C131 C136 C135 118.8(7) . . ? C137 C136 C135 116.7(7) . . ? C138 C137 C136 122.3(8) . . ? C138 C137 H13D 118.8 . . ? C136 C137 H13D 118.8 . . ? C137 C138 C139 117.0(8) . . ? C137 C138 H13E 121.5 . . ? C139 C138 H13E 121.5 . . ? C140 C139 C138 122.2(9) . . ? C140 C139 H13F 118.9 . . ? C138 C139 H13F 118.9 . . ? C135 C140 C139 116.0(9) . . ? C135 C140 H14B 122.0 . . ? C139 C140 H14B 122.0 . . ? C152 C151 C156 118.7(8) . . ? C152 C151 C157 122.6(9) . . ? C156 C151 C157 118.5(8) . . ? C153 C152 C151 120.1(9) . . ? C153 C152 H15B 119.9 . . ? C151 C152 H15B 119.9 . . ? C152 C153 C154 120.3(9) . . ? C152 C153 C158 113.3(8) . . ? C154 C153 C158 126.4(9) . . ? C155 C154 C153 120.6(9) . . ? C155 C154 H15C 119.7 . . ? C153 C154 H15C 119.7 . . ? C154 C155 C156 120.9(9) . . ? C154 C155 C100 119.4(8) . . ? C156 C155 C100 119.6(8) . . ? C155 C156 C151 118.9(8) . . ? C155 C156 H15D 120.5 . . ? C151 C156 H15D 120.5 . . ? O15 C157 N12 120.5(9) . . ? O15 C157 C151 121.9(9) . . ? N12 C157 C151 117.6(9) . . ? O16 C158 N14 120.5(10) . . ? O16 C158 C153 121.0(9) . . ? N14 C158 C153 118.4(8) . . ? C162 C161 C166 122.6(9) . . ? C162 C161 C167 117.1(8) . . ? C166 C161 C167 120.2(9) . . ? C161 C162 C163 120.5(9) . . ? C161 C162 H16B 119.7 . . ? C163 C162 H16B 119.7 . . ? C162 C163 C168 123.4(9) . . ? C162 C163 C164 116.2(9) . . ? C168 C163 C164 120.3(9) . . ? C165 C164 C163 124.1(8) . . ? C165 C164 H16C 118.0 . . ? C163 C164 H16C 118.0 . . ? C164 C165 C166 119.2(8) . . ? C164 C165 C100 119.7(8) . . ? C166 C165 C100 121.0(8) . . ? C165 C166 C161 117.4(9) . . ? C165 C166 H16D 121.3 . . ? C161 C166 H16D 121.3 . . ? O17 C167 N16 118.8(9) . . ? O17 C167 C161 117.3(8) . . ? N16 C167 C161 123.8(8) . . ? O18 C168 N18 119.8(9) . . ? O18 C168 C163 123.9(9) . . ? N18 C168 C163 116.2(9) . . ? C42' O14 C142 24.7(8) . . ? C42' O14 Ce2 134.8(8) . 18_556 ? C142 O14 Ce2 135.4(6) . 18_556 ? C104 N17 N18 118.9(8) . . ? C104 N17 Ce2 131.6(7) . 18_556 ? N18 N17 Ce2 109.2(5) . 18_556 ? C141 C104 N17 133.6(11) . . ? C141 C104 C41' 21.2(7) . . ? N17 C104 C41' 113.7(9) . . ? C141 C104 H10F 100.5 . . ? N17 C104 H10F 102.3 . . ? C41' C104 H10F 101.4 . . ? C104 C141 C142 118.9(9) . . ? C104 C141 C146 130.3(10) . . ? C142 C141 C146 110.5(9) . . ? C141 C142 C143 129.8(10) . . ? C141 C142 O14 125.6(8) . . ? C143 C142 O14 104.6(8) . . ? C144 C143 C142 109.5(10) . . ? C144 C143 H14C 125.2 . . ? C142 C143 H14C 125.2 . . ? C143 C144 C145 127.7(10) . . ? C143 C144 H14D 116.1 . . ? C145 C144 H14D 116.1 . . ? C146 C145 C144 112.4(9) . . ? C146 C145 C150 127.7(9) . . ? C144 C145 C150 119.5(9) . . ? C145 C146 C147 113.1(8) . . ? C145 C146 C141 127.3(8) . . ? C147 C146 C141 119.6(9) . . ? C148 C147 C146 124.7(10) . . ? C148 C147 H14E 117.7 . . ? C146 C147 H14E 117.7 . . ? C149 C148 C147 115.5(11) . . ? C149 C148 H14F 122.2 . . ? C147 C148 H14F 122.2 . . ? C150 C149 C148 126.0(11) . . ? C150 C149 H14G 117.0 . . ? C148 C149 H14G 117.0 . . ? C149 C150 C145 112.6(10) . . ? C149 C150 H15E 123.7 . . ? C145 C150 H15E 123.7 . . ? C46' C41' C42' 114.6(10) . . ? C46' C41' C104 116.0(8) . . ? C42' C41' C104 129.1(9) . . ? O14 C42' C43' 119.3(10) . . ? O14 C42' C41' 111.6(10) . . ? C43' C42' C41' 125.4(11) . . ? C44' C43' C42' 114.7(11) . . ? C44' C43' H43A 122.7 . . ? C42' C43' H43A 122.7 . . ? C43' C44' C45' 124.8(11) . . ? C43' C44' H44A 117.6 . . ? C45' C44' H44A 117.6 . . ? C46' C45' C44' 115.8(10) . . ? C46' C45' C50' 121.9(11) . . ? C44' C45' C50' 121.2(10) . . ? C47' C46' C41' 119.2(10) . . ? C47' C46' C45' 116.2(10) . . ? C41' C46' C45' 124.2(9) . . ? C48' C47' C46' 123.4(12) . . ? C48' C47' H47A 118.3 . . ? C46' C47' H47A 118.3 . . ? C49' C48' C47' 116.7(12) . . ? C49' C48' H48A 121.6 . . ? C47' C48' H48A 121.6 . . ? C48' C49' C50' 123.1(12) . . ? C48' C49' H49A 118.4 . . ? C50' C49' H49A 118.4 . . ? C49' C50' C45' 116.2(12) . . ? C49' C50' H50A 121.9 . . ? C45' C50' H50A 121.9 . . ? C212 O21 C12' 17.1(7) . . ? C212 O21 Ce1 157.1(7) . . ? C12' O21 Ce1 141.5(5) . . ? C222 O22 C22' 20.0(10) . . ? C222 O22 Ce2 144.4(6) . 4_576 ? C22' O22 Ce2 130.5(8) . 4_576 ? C237 O23 Ce1 125.0(6) . . ? C238 O24 Ce2 126.6(7) . 4_576 ? C201 N21 N22 111.6(8) . . ? C201 N21 Ce1 132.8(7) . . ? N22 N21 Ce1 113.5(5) . . ? N21 N22 C237 119.5(8) . . ? N21 N22 H22A 120.3 . . ? C237 N22 H22A 120.3 . . ? C202 N23 N24 120.3(8) . . ? C202 N23 Ce2 128.4(7) . 4_576 ? N24 N23 Ce2 111.3(5) . 4_576 ? C238 N24 N23 117.8(8) . . ? C238 N24 H24A 121.1 . . ? N23 N24 H24A 121.1 . . ? C233 C200 C233 118.1(10) . 4_576 ? C233 C200 H20A 107.8 . . ? C233 C200 H20A 107.8 4_576 . ? C233 C200 H20B 107.8 . . ? C233 C200 H20B 107.8 4_576 . ? H20A C200 H20B 107.1 . . ? N21 C201 C11' 138.1(11) . . ? N21 C201 C211 120.3(10) . . ? C11' C201 C211 18.1(7) . . ? N21 C201 H20C 119.8 . . ? C11' C201 H20C 102.0 . . ? C211 C201 H20C 119.8 . . ? N23 C202 C21' 127.7(10) . . ? N23 C202 C221 124.5(10) . . ? C21' C202 C221 17.3(9) . . ? N23 C202 H20E 116.7 . . ? C21' C202 H20E 112.4 . . ? C221 C202 H20E 118.9 . . ? C212 C211 C216 114.7(9) . . ? C212 C211 C201 127.2(9) . . ? C216 C211 C201 117.5(9) . . ? O21 C212 C211 113.6(9) . . ? O21 C212 C213 120.2(10) . . ? C211 C212 C213 125.6(11) . . ? C212 C213 C214 113.7(11) . . ? C212 C213 H21A 123.1 . . ? C214 C213 H21A 123.1 . . ? C215 C214 C213 125.9(11) . . ? C215 C214 H21B 117.0 . . ? C213 C214 H21B 117.0 . . ? C220 C215 C214 121.4(9) . . ? C220 C215 C216 124.2(9) . . ? C214 C215 C216 114.2(9) . . ? C217 C216 C215 114.5(9) . . ? C217 C216 C211 120.4(9) . . ? C215 C216 C211 124.7(9) . . ? C218 C217 C216 124.0(11) . . ? C218 C217 H21C 118.0 . . ? C216 C217 H21C 118.0 . . ? C219 C218 C217 115.0(11) . . ? C219 C218 H21D 122.5 . . ? C217 C218 H21D 122.5 . . ? C220 C219 C218 123.0(12) . . ? C220 C219 H21E 118.5 . . ? C218 C219 H21E 118.5 . . ? C215 C220 C219 116.5(11) . . ? C215 C220 H22B 121.7 . . ? C219 C220 H22B 121.7 . . ? C201 C11' C12' 110.5(10) . . ? C201 C11' C16' 134.0(11) . . ? C12' C11' C16' 115.3(10) . . ? C11' C12' C13' 124.8(11) . . ? C11' C12' O21 130.2(9) . . ? C13' C12' O21 104.5(9) . . ? C12' C13' C14' 115.5(12) . . ? C12' C13' H13G 122.2 . . ? C14' C13' H13G 122.2 . . ? C15' C14' C13' 123.1(11) . . ? C15' C14' H14H 118.5 . . ? C13' C14' H14H 118.5 . . ? C20' C15' C14' 118.7(10) . . ? C20' C15' C16' 121.5(10) . . ? C14' C15' C16' 116.2(10) . . ? C15' C16' C17' 117.1(9) . . ? C15' C16' C11' 122.7(9) . . ? C17' C16' C11' 120.1(9) . . ? C18' C17' C16' 121.9(11) . . ? C18' C17' H17B 119.1 . . ? C16' C17' H17B 119.1 . . ? C17' C18' C19' 117.7(12) . . ? C17' C18' H18B 121.2 . . ? C19' C18' H18B 121.2 . . ? C20' C19' C18' 119.3(13) . . ? C20' C19' H19A 120.3 . . ? C18' C19' H19A 120.3 . . ? C19' C20' C15' 117.5(12) . . ? C19' C20' H20F 121.2 . . ? C15' C20' H20F 121.2 . . ? C222 C221 C226 114.4(10) . . ? C222 C221 C202 115.5(9) . . ? C226 C221 C202 118.4(11) . . ? O22 C222 C223 112.9(8) . . ? O22 C222 C221 122.1(9) . . ? C223 C222 C221 123.0(10) . . ? C224 C223 C222 115.1(10) . . ? C224 C223 H22C 122.5 . . ? C222 C223 H22C 122.5 . . ? C223 C224 C225 121.6(11) . . ? C223 C224 H22D 119.2 . . ? C225 C224 H22D 119.2 . . ? C230 C225 C226 118.7(10) . . ? C230 C225 C224 121.4(10) . . ? C226 C225 C224 111.5(9) . . ? C227 C226 C225 119.3(9) . . ? C227 C226 C221 120.2(9) . . ? C225 C226 C221 117.4(10) . . ? C228 C227 C226 119.7(9) . . ? C228 C227 H22F 120.2 . . ? C226 C227 H22F 120.2 . . ? C229 C228 C227 117.0(11) . . ? C229 C228 H22G 121.5 . . ? C227 C228 H22G 121.5 . . ? C228 C229 C230 116.6(12) . . ? C228 C229 H22H 121.7 . . ? C230 C229 H22H 121.7 . . ? C229 C230 C225 116.6(11) . . ? C229 C230 H23B 121.7 . . ? C225 C230 H23B 121.7 . . ? C22' C21' C202 118.1(9) . . ? C22' C21' C26' 118.0(10) . . ? C202 C21' C26' 119.5(9) . . ? C23' C22' C21' 119.0(12) . . ? C23' C22' O22 112.2(12) . . ? C21' C22' O22 111.6(11) . . ? C24' C23' C22' 115.7(12) . . ? C24' C23' H23C 122.1 . . ? C22' C23' H23C 122.1 . . ? C23' C24' C25' 118.1(12) . . ? C23' C24' H24B 121.0 . . ? C25' C24' H24B 121.0 . . ? C30' C25' C24' 115.9(11) . . ? C30' C25' C26' 122.1(10) . . ? C24' C25' C26' 115.1(11) . . ? C27' C26' C25' 115.6(10) . . ? C27' C26' C21' 124.8(9) . . ? C25' C26' C21' 119.5(9) . . ? C28' C27' C26' 123.0(11) . . ? C28' C27' H27A 118.5 . . ? C26' C27' H27A 118.5 . . ? C29' C28' C27' 116.3(12) . . ? C29' C28' H28A 121.9 . . ? C27' C28' H28A 121.9 . . ? C28' C29' C30' 118.4(11) . . ? C28' C29' H29A 120.8 . . ? C30' C29' H29A 120.8 . . ? C25' C30' C29' 116.7(11) . . ? C25' C30' H30A 121.6 . . ? C29' C30' H30A 121.6 . . ? C236 C231 C232 119.4(9) . . ? C236 C231 C237 120.2(9) . . ? C232 C231 C237 120.1(9) . . ? C233 C232 C231 121.0(9) . . ? C233 C232 H23D 119.5 . . ? C231 C232 H23D 119.5 . . ? C232 C233 C234 120.5(9) . . ? C232 C233 C200 119.0(8) . . ? C234 C233 C200 120.4(8) . . ? C233 C234 C235 119.4(8) . . ? C233 C234 H23E 120.3 . . ? C235 C234 H23E 120.3 . . ? C236 C235 C238 118.5(8) . . ? C236 C235 C234 118.3(8) . . ? C238 C235 C234 122.9(9) . . ? C231 C236 C235 121.2(9) . . ? C231 C236 H23F 119.4 . . ? C235 C236 H23F 119.4 . . ? O23 C237 N22 116.5(9) . . ? O23 C237 C231 128.0(9) . . ? N22 C237 C231 115.5(9) . . ? O24 C238 N24 119.7(10) . . ? O24 C238 C235 121.7(9) . . ? N24 C238 C235 118.2(9) . . ? C303 N31 C301 115.9(10) . . ? C303 N31 C302 123.1(10) . . ? C301 N31 C302 120.9(10) . . ? O31 C301 N31 116.4(10) . . ? C305 N32 C304 123.3(14) . . ? C305 N32 C306 124.3(14) . . ? C304 N32 C306 112.3(14) . . ? O32 C304 N32 152.1(18) . . ? C307 N33 C308 164(2) . . ? C307 N33 C309 100.0(19) . . ? C308 N33 C309 95.3(15) . . ? O33 C307 N33 161(3) . . ? C313 N35 C314 124.4(11) . . ? C313 N35 C315 120.2(11) . . ? C314 N35 C315 115.4(10) . . ? O35 C313 N35 123.9(13) . . ? C310 N34 C311 121.2(11) . . ? C310 N34 C312 125.9(12) . . ? C311 N34 C312 108.1(10) . . ? C310 O34 O34 121.7(15) . 3_656 ? N34 C310 O34 109.9(13) . . ? C318 N36 C317 124.8(13) . . ? C318 N36 C316 123.7(15) . . ? C317 N36 C316 108.3(10) . . ? O36 C318 N36 136(2) . . ? C321 N37 C321 75.1(13) . 2_675 ? C321 N37 C319 113.6(10) . . ? C321 N37 C319 136.7(16) 2_675 . ? C321 N37 C319 136.7(16) . 2_675 ? C321 N37 C319 113.6(10) 2_675 2_675 ? C319 N37 C319 89(2) . 2_675 ? C321 N37 C320 39.5(11) . 2_675 ? C321 N37 C320 114.5(11) 2_675 2_675 ? C319 N37 C320 84.7(13) . 2_675 ? C319 N37 C320 114.4(11) 2_675 2_675 ? C321 N37 C320 114.5(11) . . ? C321 N37 C320 39.5(11) 2_675 . ? C319 N37 C320 114.4(11) . . ? C319 N37 C320 84.7(13) 2_675 . ? C320 N37 C320 154.0(17) 2_675 . ? C321 O37 C321 83.8(15) . 2_675 ? C321 C320 N37 68.5(13) 2_675 . ? C321 C320 C319 105(2) 2_675 2_675 ? N37 C320 C319 47.6(9) . 2_675 ? C320 C321 O37 172.5(18) 2_675 . ? C320 C321 N37 72.0(12) 2_675 . ? O37 C321 N37 100.5(12) . . ? C320 C321 C321 124.5(12) 2_675 2_675 ? O37 C321 C321 48.1(7) . 2_675 ? N37 C321 C321 52.5(7) . 2_675 ? N37 C319 C320 47.7(6) . 2_675 ? C401 O401 C401 118(5) 4_576 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.537 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.086