Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Michel Ephritikhine' 'Jean-Claude Berthet' 'Thouraya Mehdoui' 'Pierre Thuery' _publ_contact_author_name 'M. Ephritikhine' _publ_contact_author_address ; CEA/Saclay, SCM (CNRS URA 331) Bat. 125 91191 Gif-sur-Yvette France ; _publ_contact_author_phone '33 01 69 08 64 36' _publ_contact_author_fax '33 1 69 08 66 40' _publ_contact_author_email ephri@drecam.cea.fr _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Lanthanide(III)/actinide(III) differentiation in coordination of azine molecules to tris(cyclopentadienyl) complexes of cerium and uranium ; data_(Ce,Bu^t^,pyridine) _database_code_depnum_ccdc_archive 'CCDC 223524' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H44 Ce N' _chemical_formula_weight 582.80 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' 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 10.7142(5) _cell_length_b 10.8502(4) _cell_length_c 13.7197(6) _cell_angle_alpha 98.320(3) _cell_angle_beta 110.262(2) _cell_angle_gamma 96.681(3) _cell_volume 1456.49(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9932 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 25.67 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method ? _exptl_crystal_F_000 602 _exptl_absorpt_coefficient_mu 1.581 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.506 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 9932 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.67 _reflns_number_total 5060 _reflns_number_gt 4643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. All H atoms were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH3) times that of the parent atom. 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^)+0.3733P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5060 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.489 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.066 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 Ce Ce 0.497934(14) 0.721898(13) 0.277176(10) 0.01962(6) Uani 1 1 d . . . N N 0.6229(2) 0.5199(2) 0.28897(17) 0.0244(5) Uani 1 1 d . . . C1 C 0.7799(3) 0.8542(3) 0.3606(2) 0.0281(6) Uani 1 1 d . . . C2 C 0.6988(3) 0.9419(3) 0.3173(2) 0.0273(6) Uani 1 1 d . . . H2 H 0.6973 0.9745 0.2579 0.033 Uiso 1 1 calc R . . C3 C 0.6210(3) 0.9716(3) 0.3788(2) 0.0288(6) Uani 1 1 d . . . H3 H 0.5591 1.0264 0.3670 0.035 Uiso 1 1 calc R . . C4 C 0.6537(3) 0.9038(3) 0.4609(2) 0.0296(6) Uani 1 1 d . . . H4 H 0.6183 0.9070 0.5141 0.035 Uiso 1 1 calc R . . C5 C 0.7488(3) 0.8301(3) 0.4494(2) 0.0286(6) Uani 1 1 d . . . H5 H 0.7854 0.7747 0.4927 0.034 Uiso 1 1 calc R . . C6 C 0.8952(3) 0.8157(3) 0.3295(2) 0.0320(6) Uani 1 1 d . . . C7 C 0.9685(3) 0.7280(4) 0.4000(3) 0.0501(9) Uani 1 1 d . . . H7A H 1.0034 0.7710 0.4729 0.075 Uiso 1 1 calc R . . H7B H 1.0416 0.7060 0.3799 0.075 Uiso 1 1 calc R . . H7C H 0.9060 0.6525 0.3912 0.075 Uiso 1 1 calc R . . C8 C 0.9985(3) 0.9351(3) 0.3470(3) 0.0489(9) Uani 1 1 d . . . H8A H 0.9574 0.9892 0.3004 0.073 Uiso 1 1 calc R . . H8B H 1.0749 0.9116 0.3324 0.073 Uiso 1 1 calc R . . H8C H 1.0280 0.9793 0.4192 0.073 Uiso 1 1 calc R . . C9 C 0.8478(3) 0.7495(3) 0.2130(2) 0.0352(7) Uani 1 1 d . . . H9A H 0.7884 0.6709 0.2016 0.053 Uiso 1 1 calc R . . H9B H 0.9248 0.7331 0.1960 0.053 Uiso 1 1 calc R . . H9C H 0.8005 0.8029 0.1686 0.053 Uiso 1 1 calc R . . C10 C 0.3611(3) 0.8181(2) 0.0877(2) 0.0248(6) Uani 1 1 d . . . C11 C 0.4866(3) 0.8000(3) 0.08233(19) 0.0252(6) Uani 1 1 d . . . H11 H 0.5560 0.8638 0.0878 0.030 Uiso 1 1 calc R . . C12 C 0.4901(3) 0.6689(3) 0.0672(2) 0.0258(6) Uani 1 1 d . . . H12 H 0.5616 0.6315 0.0612 0.031 Uiso 1 1 calc R . . C13 C 0.3651(3) 0.6053(3) 0.0628(2) 0.0255(6) Uani 1 1 d . . . H13 H 0.3395 0.5182 0.0532 0.031 Uiso 1 1 calc R . . C14 C 0.2861(3) 0.6966(2) 0.0754(2) 0.0251(6) Uani 1 1 d . . . H14 H 0.1990 0.6800 0.0755 0.030 Uiso 1 1 calc R . . C15 C 0.3042(3) 0.9410(3) 0.0882(2) 0.0312(6) Uani 1 1 d . . . C16 C 0.2253(4) 0.9508(3) 0.1625(3) 0.0434(8) Uani 1 1 d . . . H16A H 0.1539 0.8787 0.1405 0.065 Uiso 1 1 calc R . . H16B H 0.1874 1.0268 0.1598 0.065 Uiso 1 1 calc R . . H16C H 0.2852 0.9531 0.2337 0.065 Uiso 1 1 calc R . . C17 C 0.2085(3) 0.9403(3) -0.0251(3) 0.0444(8) Uani 1 1 d . . . H17A H 0.2573 0.9336 -0.0720 0.067 Uiso 1 1 calc R . . H17B H 0.1728 1.0175 -0.0265 0.067 Uiso 1 1 calc R . . H17C H 0.1355 0.8695 -0.0476 0.067 Uiso 1 1 calc R . . C18 C 0.4180(3) 1.0567(3) 0.1232(2) 0.0319(6) Uani 1 1 d . . . H18A H 0.4770 1.0601 0.1949 0.048 Uiso 1 1 calc R . . H18B H 0.3797 1.1323 0.1191 0.048 Uiso 1 1 calc R . . H18C H 0.4685 1.0499 0.0775 0.048 Uiso 1 1 calc R . . C19 C 0.2730(3) 0.5493(2) 0.2981(2) 0.0232(5) Uani 1 1 d . . . C20 C 0.2428(3) 0.6733(2) 0.3025(2) 0.0249(6) Uani 1 1 d . . . H20 H 0.1717 0.6982 0.2524 0.030 Uiso 1 1 calc R . . C21 C 0.3388(3) 0.7526(3) 0.3956(2) 0.0260(6) Uani 1 1 d . . . H21 H 0.3417 0.8384 0.4178 0.031 Uiso 1 1 calc R . . C22 C 0.4293(3) 0.6783(3) 0.4487(2) 0.0266(6) Uani 1 1 d . . . H22 H 0.5023 0.7062 0.5126 0.032 Uiso 1 1 calc R . . C23 C 0.3899(3) 0.5554(2) 0.3882(2) 0.0233(5) Uani 1 1 d . . . H23 H 0.4341 0.4879 0.4048 0.028 Uiso 1 1 calc R . . C24 C 0.1816(3) 0.4268(3) 0.2272(2) 0.0283(6) Uani 1 1 d . . . C25 C 0.1060(3) 0.3688(3) 0.2920(3) 0.0437(8) Uani 1 1 d . . . H25A H 0.0532 0.4270 0.3106 0.066 Uiso 1 1 calc R . . H25B H 0.1704 0.3523 0.3554 0.066 Uiso 1 1 calc R . . H25C H 0.0475 0.2910 0.2503 0.066 Uiso 1 1 calc R . . C26 C 0.2646(3) 0.3319(3) 0.1984(3) 0.0381(7) Uani 1 1 d . . . H26A H 0.2051 0.2546 0.1567 0.057 Uiso 1 1 calc R . . H26B H 0.3278 0.3149 0.2621 0.057 Uiso 1 1 calc R . . H26C H 0.3128 0.3666 0.1585 0.057 Uiso 1 1 calc R . . C27 C 0.0763(3) 0.4485(3) 0.1260(2) 0.0357(7) Uani 1 1 d . . . H27A H 0.0241 0.5078 0.1440 0.054 Uiso 1 1 calc R . . H27B H 0.0175 0.3697 0.0873 0.054 Uiso 1 1 calc R . . H27C H 0.1210 0.4815 0.0831 0.054 Uiso 1 1 calc R . . C28 C 0.6842(3) 0.4917(3) 0.3843(2) 0.0278(6) Uani 1 1 d . . . H28 H 0.6824 0.5440 0.4436 0.033 Uiso 1 1 calc R . . C29 C 0.7499(3) 0.3893(3) 0.3996(2) 0.0307(6) Uani 1 1 d . . . H29 H 0.7909 0.3738 0.4674 0.037 Uiso 1 1 calc R . . C30 C 0.7534(3) 0.3109(3) 0.3127(2) 0.0339(7) Uani 1 1 d . . . H30 H 0.7969 0.2416 0.3206 0.041 Uiso 1 1 calc R . . C31 C 0.6907(3) 0.3375(3) 0.2129(2) 0.0319(6) Uani 1 1 d . . . H31 H 0.6917 0.2864 0.1527 0.038 Uiso 1 1 calc R . . C32 C 0.6269(3) 0.4410(3) 0.2049(2) 0.0276(6) Uani 1 1 d . . . H32 H 0.5842 0.4574 0.1377 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.01960(9) 0.02086(9) 0.01829(8) 0.00321(6) 0.00722(6) 0.00343(5) N 0.0240(12) 0.0284(12) 0.0225(11) 0.0059(10) 0.0096(9) 0.0068(9) C1 0.0214(14) 0.0287(14) 0.0284(14) 0.0010(12) 0.0070(11) -0.0056(11) C2 0.0265(14) 0.0272(14) 0.0246(13) 0.0023(12) 0.0091(11) -0.0049(11) C3 0.0281(15) 0.0237(14) 0.0307(15) -0.0004(12) 0.0104(12) -0.0021(11) C4 0.0281(15) 0.0303(15) 0.0240(13) -0.0024(12) 0.0088(11) -0.0064(11) C5 0.0256(14) 0.0330(15) 0.0231(13) 0.0049(12) 0.0066(11) -0.0024(11) C6 0.0242(14) 0.0402(17) 0.0322(15) 0.0084(13) 0.0125(12) 0.0005(12) C7 0.0279(17) 0.082(3) 0.053(2) 0.031(2) 0.0191(15) 0.0220(17) C8 0.0352(18) 0.055(2) 0.052(2) -0.0076(17) 0.0243(16) -0.0116(15) C9 0.0261(15) 0.0422(17) 0.0374(16) 0.0044(14) 0.0130(13) 0.0068(12) C10 0.0277(14) 0.0242(14) 0.0226(13) 0.0068(11) 0.0086(11) 0.0043(11) C11 0.0264(14) 0.0300(14) 0.0188(12) 0.0070(11) 0.0079(11) 0.0026(11) C12 0.0322(15) 0.0296(14) 0.0178(12) 0.0047(11) 0.0101(11) 0.0113(11) C13 0.0292(14) 0.0262(14) 0.0178(12) 0.0047(11) 0.0048(10) 0.0038(11) C14 0.0226(13) 0.0295(14) 0.0213(13) 0.0078(12) 0.0052(10) 0.0034(11) C15 0.0347(16) 0.0295(15) 0.0364(16) 0.0135(13) 0.0172(13) 0.0116(12) C16 0.053(2) 0.0315(16) 0.068(2) 0.0212(17) 0.0420(18) 0.0210(14) C17 0.0455(19) 0.0337(17) 0.053(2) 0.0206(16) 0.0105(16) 0.0138(14) C18 0.0413(17) 0.0233(14) 0.0388(16) 0.0117(13) 0.0208(13) 0.0094(12) C19 0.0245(13) 0.0229(13) 0.0242(13) 0.0049(11) 0.0113(11) 0.0048(10) C20 0.0222(13) 0.0275(14) 0.0284(14) 0.0079(12) 0.0119(11) 0.0074(10) C21 0.0293(14) 0.0246(14) 0.0280(13) 0.0033(12) 0.0161(11) 0.0042(11) C22 0.0259(14) 0.0325(15) 0.0199(12) 0.0035(11) 0.0089(11) -0.0001(11) C23 0.0242(13) 0.0254(14) 0.0235(13) 0.0066(11) 0.0120(10) 0.0059(10) C24 0.0268(14) 0.0263(14) 0.0290(14) 0.0075(12) 0.0074(12) 0.0001(11) C25 0.0406(18) 0.0449(19) 0.0377(17) 0.0096(15) 0.0101(14) -0.0113(14) C26 0.0435(18) 0.0234(15) 0.0388(17) 0.0014(13) 0.0072(14) 0.0041(12) C27 0.0318(16) 0.0310(15) 0.0322(15) 0.0053(13) 0.0001(12) -0.0034(12) C28 0.0261(14) 0.0343(15) 0.0252(14) 0.0067(12) 0.0110(11) 0.0075(11) C29 0.0251(14) 0.0376(16) 0.0318(15) 0.0147(13) 0.0091(12) 0.0089(12) C30 0.0299(15) 0.0310(15) 0.0466(18) 0.0147(14) 0.0162(13) 0.0125(12) C31 0.0351(16) 0.0299(15) 0.0335(15) 0.0021(13) 0.0167(13) 0.0097(12) C32 0.0326(15) 0.0278(14) 0.0228(13) 0.0046(12) 0.0105(11) 0.0066(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce N 2.694(2) . ? Ce C21 2.748(3) . ? Ce C22 2.782(3) . ? Ce C3 2.798(3) . ? Ce C13 2.808(3) . ? Ce C4 2.813(3) . ? Ce C12 2.825(2) . ? Ce C14 2.859(2) . ? Ce C20 2.871(3) . ? Ce C2 2.870(3) . ? Ce C5 2.872(3) . ? Ce C11 2.887(2) . ? Ce C23 2.907(3) . ? Ce C10 2.915(3) . ? Ce C1 2.935(3) . ? Ce C19 2.997(3) . ? N C28 1.343(3) . ? N C32 1.350(3) . ? C1 C2 1.418(4) . ? C1 C5 1.420(4) . ? C1 C6 1.522(4) . ? C2 C3 1.408(4) . ? C3 C4 1.400(4) . ? C4 C5 1.402(4) . ? C6 C9 1.532(4) . ? C6 C8 1.535(4) . ? C6 C7 1.540(4) . ? C10 C11 1.407(4) . ? C10 C14 1.417(4) . ? C10 C15 1.529(4) . ? C11 C12 1.414(4) . ? C12 C13 1.411(4) . ? C13 C14 1.405(4) . ? C15 C18 1.535(4) . ? C15 C16 1.533(4) . ? C15 C17 1.535(4) . ? C19 C23 1.410(4) . ? C19 C20 1.417(4) . ? C19 C24 1.528(4) . ? C20 C21 1.413(4) . ? C21 C22 1.409(4) . ? C22 C23 1.398(4) . ? C24 C27 1.526(4) . ? C24 C26 1.531(4) . ? C24 C25 1.545(4) . ? C28 C29 1.387(4) . ? C29 C30 1.374(4) . ? C30 C31 1.390(4) . ? C31 C32 1.380(4) . ? 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 N Ce C21 117.24(7) . . ? N Ce C22 89.80(7) . . ? C21 Ce C22 29.50(8) . . ? N Ce C3 125.47(8) . . ? C21 Ce C3 84.15(8) . . ? C22 Ce C3 91.56(8) . . ? N Ce C13 84.18(7) . . ? C21 Ce C13 116.70(8) . . ? C22 Ce C13 128.13(8) . . ? C3 Ce C13 132.68(8) . . ? N Ce C4 105.88(8) . . ? C21 Ce C4 73.47(8) . . ? C22 Ce C4 68.91(8) . . ? C3 Ce C4 28.90(8) . . ? C13 Ce C4 161.06(8) . . ? N Ce C12 81.00(7) . . ? C21 Ce C12 143.25(8) . . ? C22 Ce C12 155.76(8) . . ? C3 Ce C12 112.07(8) . . ? C13 Ce C12 29.01(8) . . ? C4 Ce C12 135.17(8) . . ? N Ce C14 111.97(7) . . ? C21 Ce C14 96.18(8) . . ? C22 Ce C14 118.67(8) . . ? C3 Ce C14 114.67(8) . . ? C13 Ce C14 28.70(8) . . ? C4 Ce C14 141.13(8) . . ? C12 Ce C14 47.26(8) . . ? N Ce C20 112.40(7) . . ? C21 Ce C20 29.02(8) . . ? C22 Ce C20 47.48(8) . . ? C3 Ce C20 107.96(8) . . ? C13 Ce C20 88.06(8) . . ? C4 Ce C20 102.28(8) . . ? C12 Ce C20 116.06(8) . . ? C14 Ce C20 71.43(8) . . ? N Ce C2 107.62(7) . . ? C21 Ce C2 112.86(8) . . ? C22 Ce C2 115.86(8) . . ? C3 Ce C2 28.73(8) . . ? C13 Ce C2 115.03(8) . . ? C4 Ce C2 47.00(8) . . ? C12 Ce C2 88.35(8) . . ? C14 Ce C2 110.62(8) . . ? C20 Ce C2 135.49(8) . . ? N Ce C5 79.69(8) . . ? C21 Ce C5 95.31(8) . . ? C22 Ce C5 79.54(8) . . ? C3 Ce C5 47.25(8) . . ? C13 Ce C5 147.96(8) . . ? C4 Ce C5 28.53(8) . . ? C12 Ce C5 120.19(8) . . ? C14 Ce C5 157.18(8) . . ? C20 Ce C5 123.67(8) . . ? C2 Ce C5 46.59(8) . . ? N Ce C11 106.71(7) . . ? C21 Ce C11 131.54(8) . . ? C22 Ce C11 160.89(8) . . ? C3 Ce C11 86.65(8) . . ? C13 Ce C11 47.11(8) . . ? C4 Ce C11 113.99(8) . . ? C12 Ce C11 28.64(7) . . ? C14 Ce C11 46.51(7) . . ? C20 Ce C11 115.31(7) . . ? C2 Ce C11 68.89(7) . . ? C5 Ce C11 112.28(8) . . ? C28 N C32 116.1(2) . . ? C2 C1 C5 106.3(3) . . ? C2 C1 C6 125.3(2) . . ? C5 C1 C6 127.5(3) . . ? C3 C2 C1 108.9(2) . . ? C4 C3 C2 107.7(3) . . ? C5 C4 C3 108.4(2) . . ? C4 C5 C1 108.7(3) . . ? C1 C6 C9 112.7(2) . . ? C1 C6 C8 108.6(3) . . ? C9 C6 C8 108.1(2) . . ? C1 C6 C7 110.8(2) . . ? C9 C6 C7 109.0(3) . . ? C8 C6 C7 107.5(3) . . ? C11 C10 C14 106.9(2) . . ? C11 C10 C15 127.5(2) . . ? C14 C10 C15 124.8(2) . . ? C10 C11 C12 109.0(2) . . ? C13 C12 C11 107.4(2) . . ? C14 C13 C12 108.0(2) . . ? C13 C14 C10 108.7(2) . . ? C10 C15 C18 110.9(2) . . ? C10 C15 C16 110.5(2) . . ? C18 C15 C16 109.4(3) . . ? C10 C15 C17 108.4(2) . . ? C18 C15 C17 108.4(2) . . ? C16 C15 C17 109.2(3) . . ? C23 C19 C20 106.4(2) . . ? C23 C19 C24 124.7(2) . . ? C20 C19 C24 127.4(2) . . ? C21 C20 C19 108.7(2) . . ? C22 C21 C20 107.6(2) . . ? C23 C22 C21 107.8(2) . . ? C22 C23 C19 109.5(2) . . ? C27 C24 C19 113.0(2) . . ? C27 C24 C26 109.4(2) . . ? C19 C24 C26 111.2(2) . . ? C27 C24 C25 108.0(2) . . ? C19 C24 C25 106.7(2) . . ? C26 C24 C25 108.3(2) . . ? N C28 C29 123.9(3) . . ? C30 C29 C28 118.8(3) . . ? C29 C30 C31 118.7(3) . . ? C32 C31 C30 118.7(3) . . ? N C32 C31 123.7(3) . . ? #===END data_(U,Bu^t^,pyridine) _database_code_depnum_ccdc_archive 'CCDC 223525' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H44 N U' _chemical_formula_weight 680.71 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' U U -9.6767 9.6646 '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 10.6759(9) _cell_length_b 10.8331(9) _cell_length_c 13.6419(8) _cell_angle_alpha 98.333(4) _cell_angle_beta 110.235(4) _cell_angle_gamma 96.726(3) _cell_volume 1440.76(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9649 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method ? _exptl_crystal_F_000 670 _exptl_absorpt_coefficient_mu 5.652 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.441 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 9649 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_sigmaI/netI 0.1123 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4936 _reflns_number_gt 3811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. All H atoms were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH3) times that of the parent atom. 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^)]' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4936 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.685 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.139 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 U U 0.49864(3) 0.72188(3) 0.27703(2) 0.02721(10) Uani 1 1 d . . . N N 0.6229(6) 0.5220(6) 0.2889(5) 0.0317(15) Uani 1 1 d . . . C1 C 0.7779(8) 0.8533(7) 0.3592(6) 0.0344(18) Uani 1 1 d . . . C2 C 0.6997(8) 0.9396(7) 0.3157(6) 0.0343(19) Uani 1 1 d . . . H2 H 0.6998 0.9722 0.2563 0.041 Uiso 1 1 calc R . . C3 C 0.6187(8) 0.9704(7) 0.3771(6) 0.038(2) Uani 1 1 d . . . H3 H 0.5550 1.0237 0.3638 0.046 Uiso 1 1 calc R . . C4 C 0.6535(8) 0.9052(7) 0.4603(6) 0.0352(19) Uani 1 1 d . . . H4 H 0.6191 0.9103 0.5145 0.042 Uiso 1 1 calc R . . C5 C 0.7494(8) 0.8297(7) 0.4500(6) 0.0367(19) Uani 1 1 d . . . H5 H 0.7868 0.7750 0.4941 0.044 Uiso 1 1 calc R . . C6 C 0.8947(8) 0.8154(7) 0.3286(6) 0.0365(19) Uani 1 1 d . . . C7 C 0.9691(9) 0.7277(10) 0.3990(8) 0.062(3) Uani 1 1 d . . . H7A H 0.9905 0.7640 0.4726 0.093 Uiso 1 1 calc R . . H7B H 1.0514 0.7182 0.3872 0.093 Uiso 1 1 calc R . . H7C H 0.9118 0.6461 0.3810 0.093 Uiso 1 1 calc R . . C8 C 0.9966(9) 0.9360(9) 0.3463(8) 0.059(3) Uani 1 1 d . . . H8A H 0.9558 0.9878 0.2969 0.088 Uiso 1 1 calc R . . H8B H 1.0757 0.9135 0.3351 0.088 Uiso 1 1 calc R . . H8C H 1.0222 0.9824 0.4179 0.088 Uiso 1 1 calc R . . C9 C 0.8475(8) 0.7486(8) 0.2111(6) 0.042(2) Uani 1 1 d . . . H9A H 0.7876 0.6700 0.1994 0.063 Uiso 1 1 calc R . . H9B H 0.9249 0.7321 0.1943 0.063 Uiso 1 1 calc R . . H9C H 0.8004 0.8022 0.1662 0.063 Uiso 1 1 calc R . . C10 C 0.3618(8) 0.8171(7) 0.0888(6) 0.0327(18) Uani 1 1 d . . . C11 C 0.4889(8) 0.7996(7) 0.0814(6) 0.0362(19) Uani 1 1 d . . . H11 H 0.5580 0.8629 0.0849 0.043 Uiso 1 1 calc R . . C12 C 0.4900(8) 0.6667(7) 0.0677(5) 0.0315(18) Uani 1 1 d . . . H12 H 0.5615 0.6284 0.0625 0.038 Uiso 1 1 calc R . . C13 C 0.3647(8) 0.6031(7) 0.0635(6) 0.0304(18) Uani 1 1 d . . . H13 H 0.3378 0.5159 0.0532 0.036 Uiso 1 1 calc R . . C14 C 0.2880(9) 0.6968(7) 0.0780(6) 0.0361(19) Uani 1 1 d . . . H14 H 0.2015 0.6811 0.0800 0.043 Uiso 1 1 calc R . . C15 C 0.3076(9) 0.9427(7) 0.0898(6) 0.0379(19) Uani 1 1 d . . . C16 C 0.2223(9) 0.9502(8) 0.1619(7) 0.050(2) Uani 1 1 d . . . H16A H 0.2792 0.9496 0.2338 0.076 Uiso 1 1 calc R . . H16B H 0.1494 0.8786 0.1363 0.076 Uiso 1 1 calc R . . H16C H 0.1857 1.0270 0.1600 0.076 Uiso 1 1 calc R . . C17 C 0.2073(10) 0.9385(8) -0.0264(7) 0.052(2) Uani 1 1 d . . . H17A H 0.1575 1.0068 -0.0263 0.079 Uiso 1 1 calc R . . H17B H 0.1452 0.8591 -0.0523 0.079 Uiso 1 1 calc R . . H17C H 0.2578 0.9472 -0.0720 0.079 Uiso 1 1 calc R . . C18 C 0.4192(9) 1.0571(7) 0.1255(7) 0.039(2) Uani 1 1 d . . . H18A H 0.4821 1.0564 0.1955 0.059 Uiso 1 1 calc R . . H18B H 0.3809 1.1328 0.1273 0.059 Uiso 1 1 calc R . . H18C H 0.4659 1.0549 0.0766 0.059 Uiso 1 1 calc R . . C19 C 0.2738(8) 0.5502(7) 0.2962(5) 0.0295(17) Uani 1 1 d . . . C20 C 0.2454(8) 0.6747(7) 0.3024(6) 0.0301(17) Uani 1 1 d . . . H20 H 0.1741 0.7003 0.2526 0.036 Uiso 1 1 calc R . . C21 C 0.3407(7) 0.7532(7) 0.3947(6) 0.0297(17) Uani 1 1 d . . . H21 H 0.3436 0.8392 0.4169 0.036 Uiso 1 1 calc R . . C22 C 0.4322(8) 0.6792(7) 0.4485(6) 0.0355(19) Uani 1 1 d . . . H22 H 0.5062 0.7076 0.5123 0.043 Uiso 1 1 calc R . . C23 C 0.3911(7) 0.5543(7) 0.3879(6) 0.0287(17) Uani 1 1 d . . . H23 H 0.4337 0.4860 0.4051 0.034 Uiso 1 1 calc R . . C24 C 0.1818(8) 0.4273(7) 0.2265(6) 0.0341(18) Uani 1 1 d . . . C25 C 0.1049(10) 0.3711(8) 0.2922(7) 0.051(2) Uani 1 1 d . . . H25A H 0.1688 0.3517 0.3548 0.077 Uiso 1 1 calc R . . H25B H 0.0428 0.2951 0.2497 0.077 Uiso 1 1 calc R . . H25C H 0.0555 0.4319 0.3129 0.077 Uiso 1 1 calc R . . C26 C 0.2634(9) 0.3314(7) 0.1980(6) 0.040(2) Uani 1 1 d . . . H26A H 0.3203 0.3689 0.1650 0.060 Uiso 1 1 calc R . . H26B H 0.2026 0.2580 0.1496 0.060 Uiso 1 1 calc R . . H26C H 0.3188 0.3069 0.2616 0.060 Uiso 1 1 calc R . . C27 C 0.0784(8) 0.4487(7) 0.1258(6) 0.040(2) Uani 1 1 d . . . H27A H 0.0253 0.5075 0.1435 0.061 Uiso 1 1 calc R . . H27B H 0.0201 0.3696 0.0863 0.061 Uiso 1 1 calc R . . H27C H 0.1240 0.4826 0.0834 0.061 Uiso 1 1 calc R . . C28 C 0.6855(8) 0.4951(7) 0.3856(6) 0.0348(19) Uani 1 1 d . . . H28 H 0.6865 0.5494 0.4454 0.042 Uiso 1 1 calc R . . C29 C 0.7477(8) 0.3917(7) 0.4005(6) 0.0373(19) Uani 1 1 d . . . H29 H 0.7867 0.3752 0.4685 0.045 Uiso 1 1 calc R . . C30 C 0.7516(8) 0.3127(8) 0.3130(7) 0.042(2) Uani 1 1 d . . . H30 H 0.7954 0.2434 0.3209 0.050 Uiso 1 1 calc R . . C31 C 0.6876(8) 0.3401(7) 0.2118(7) 0.040(2) Uani 1 1 d . . . H31 H 0.6876 0.2888 0.1509 0.048 Uiso 1 1 calc R . . C32 C 0.6257(8) 0.4430(7) 0.2046(6) 0.0336(18) Uani 1 1 d . . . H32 H 0.5826 0.4595 0.1372 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02769(17) 0.02699(15) 0.02725(16) 0.00544(10) 0.01057(11) 0.00468(11) N 0.030(4) 0.032(4) 0.040(4) 0.013(3) 0.019(3) 0.005(3) C1 0.036(5) 0.031(4) 0.031(4) 0.002(3) 0.010(4) -0.006(4) C2 0.045(5) 0.034(4) 0.021(4) 0.004(3) 0.013(4) -0.002(4) C3 0.033(5) 0.032(5) 0.043(5) 0.004(4) 0.010(4) 0.002(4) C4 0.038(5) 0.035(4) 0.026(4) -0.004(3) 0.012(4) -0.005(4) C5 0.032(5) 0.031(4) 0.039(5) 0.005(3) 0.009(4) -0.007(4) C6 0.031(5) 0.044(5) 0.029(4) 0.003(3) 0.007(4) 0.005(4) C7 0.035(6) 0.095(8) 0.070(7) 0.033(6) 0.028(5) 0.023(5) C8 0.046(6) 0.066(6) 0.059(6) -0.004(5) 0.027(5) -0.018(5) C9 0.024(5) 0.050(5) 0.055(6) 0.007(4) 0.019(4) 0.006(4) C10 0.049(5) 0.028(4) 0.024(4) 0.009(3) 0.016(4) 0.008(4) C11 0.045(5) 0.040(5) 0.030(4) 0.012(3) 0.020(4) 0.005(4) C12 0.045(5) 0.028(4) 0.026(4) 0.003(3) 0.019(4) 0.006(4) C13 0.034(5) 0.025(4) 0.031(4) 0.006(3) 0.013(4) 0.001(4) C14 0.048(6) 0.033(4) 0.029(4) 0.010(3) 0.014(4) 0.011(4) C15 0.044(5) 0.034(5) 0.046(5) 0.018(4) 0.023(4) 0.016(4) C16 0.051(6) 0.048(5) 0.069(6) 0.022(5) 0.034(5) 0.020(5) C17 0.068(7) 0.034(5) 0.063(6) 0.021(4) 0.028(5) 0.010(5) C18 0.047(6) 0.027(4) 0.055(5) 0.007(4) 0.030(5) 0.011(4) C19 0.035(5) 0.032(4) 0.024(4) 0.008(3) 0.011(3) 0.009(4) C20 0.028(4) 0.032(4) 0.040(5) 0.015(3) 0.018(4) 0.011(3) C21 0.025(4) 0.028(4) 0.036(4) 0.008(3) 0.011(4) 0.005(3) C22 0.038(5) 0.036(5) 0.035(4) 0.017(4) 0.014(4) 0.005(4) C23 0.020(4) 0.031(4) 0.038(4) 0.017(3) 0.010(3) 0.004(3) C24 0.032(5) 0.029(4) 0.034(4) 0.004(3) 0.006(4) -0.003(4) C25 0.061(7) 0.041(5) 0.046(5) 0.008(4) 0.019(5) -0.009(5) C26 0.051(6) 0.027(4) 0.032(4) -0.001(3) 0.008(4) 0.000(4) C27 0.035(5) 0.037(5) 0.041(5) 0.011(4) 0.003(4) 0.007(4) C28 0.041(5) 0.037(5) 0.032(4) 0.004(3) 0.021(4) 0.009(4) C29 0.033(5) 0.044(5) 0.041(5) 0.022(4) 0.014(4) 0.010(4) C30 0.040(5) 0.040(5) 0.050(5) 0.018(4) 0.015(4) 0.018(4) C31 0.046(6) 0.029(4) 0.050(5) 0.005(4) 0.027(4) 0.003(4) C32 0.036(5) 0.029(4) 0.037(5) 0.002(3) 0.015(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U N 2.665(6) . ? U C21 2.717(7) . ? U C22 2.752(7) . ? U C3 2.769(7) . ? U C13 2.790(7) . ? U C12 2.798(7) . ? U C4 2.804(7) . ? U C14 2.815(8) . ? U C20 2.840(7) . ? U C2 2.849(7) . ? U C5 2.864(8) . ? U C11 2.884(7) . ? U C10 2.885(7) . ? U C1 2.899(7) . ? U C23 2.900(7) . ? U C19 2.970(7) . ? N C32 1.341(9) . ? N C28 1.349(9) . ? C1 C2 1.388(11) . ? C1 C5 1.424(10) . ? C1 C6 1.525(11) . ? C2 C3 1.430(10) . ? C3 C4 1.390(11) . ? C4 C5 1.414(11) . ? C6 C7 1.539(11) . ? C6 C9 1.538(10) . ? C6 C8 1.531(11) . ? C10 C14 1.402(10) . ? C10 C11 1.427(11) . ? C10 C15 1.539(10) . ? C11 C12 1.427(10) . ? C12 C13 1.409(10) . ? C13 C14 1.410(10) . ? C15 C18 1.507(11) . ? C15 C16 1.554(11) . ? C15 C17 1.567(12) . ? C19 C20 1.414(10) . ? C19 C23 1.422(10) . ? C19 C24 1.524(10) . ? C20 C21 1.394(10) . ? C21 C22 1.412(10) . ? C22 C23 1.411(10) . ? C24 C27 1.504(10) . ? C24 C26 1.522(11) . ? C24 C25 1.548(10) . ? C28 C29 1.372(10) . ? C29 C30 1.380(11) . ? C30 C31 1.406(11) . ? C31 C32 1.359(10) . ? 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 N U C21 117.47(19) . . ? N U C22 89.7(2) . . ? C21 U C22 29.9(2) . . ? N U C3 126.0(2) . . ? C21 U C3 83.8(2) . . ? C22 U C3 91.4(2) . . ? N U C13 83.9(2) . . ? C21 U C13 116.3(2) . . ? C22 U C13 127.8(2) . . ? C3 U C13 133.0(2) . . ? N U C12 80.6(2) . . ? C21 U C12 143.1(2) . . ? C22 U C12 155.5(2) . . ? C3 U C12 112.5(2) . . ? C13 U C12 29.2(2) . . ? N U C4 106.3(2) . . ? C21 U C4 73.4(2) . . ? C22 U C4 68.8(2) . . ? C3 U C4 28.9(2) . . ? C13 U C4 161.4(2) . . ? C12 U C4 135.5(2) . . ? N U C14 112.2(2) . . ? C21 U C14 95.7(2) . . ? C22 U C14 118.6(2) . . ? C3 U C14 114.2(2) . . ? C13 U C14 29.1(2) . . ? C12 U C14 47.6(2) . . ? C4 U C14 140.6(2) . . ? N U C20 112.68(18) . . ? C21 U C20 29.0(2) . . ? C22 U C20 47.9(2) . . ? C3 U C20 107.4(2) . . ? C13 U C20 87.7(2) . . ? C12 U C20 115.9(2) . . ? C4 U C20 102.1(2) . . ? C14 U C20 71.0(2) . . ? N U C2 107.2(2) . . ? C21 U C2 113.2(2) . . ? C22 U C2 116.0(2) . . ? C3 U C2 29.5(2) . . ? C13 U C2 115.4(2) . . ? C12 U C2 88.4(2) . . ? C4 U C2 47.2(2) . . ? C14 U C2 110.7(2) . . ? C20 U C2 135.7(2) . . ? N U C5 79.6(2) . . ? C21 U C5 95.2(2) . . ? C22 U C5 79.0(2) . . ? C3 U C5 47.9(2) . . ? C13 U C5 148.4(2) . . ? C12 U C5 120.6(2) . . ? C4 U C5 28.9(2) . . ? C14 U C5 157.6(2) . . ? C20 U C5 123.5(2) . . ? C2 U C5 46.9(2) . . ? N U C11 106.45(19) . . ? C21 U C11 131.7(2) . . ? C22 U C11 161.5(2) . . ? C3 U C11 86.4(2) . . ? C13 U C11 47.9(2) . . ? C12 U C11 29.0(2) . . ? C4 U C11 113.6(2) . . ? C14 U C11 47.1(2) . . ? C20 U C11 115.6(2) . . ? C2 U C11 68.4(2) . . ? C5 U C11 112.2(2) . . ? C32 N C28 116.6(6) . . ? C2 C1 C5 107.9(7) . . ? C2 C1 C6 124.5(6) . . ? C5 C1 C6 126.4(7) . . ? C1 C2 C3 109.0(6) . . ? C4 C3 C2 106.7(7) . . ? C3 C4 C5 109.5(7) . . ? C4 C5 C1 107.0(7) . . ? C1 C6 C7 111.4(6) . . ? C1 C6 C9 112.5(6) . . ? C7 C6 C9 108.5(7) . . ? C1 C6 C8 108.1(6) . . ? C7 C6 C8 107.9(7) . . ? C9 C6 C8 108.2(6) . . ? C14 C10 C11 107.4(6) . . ? C14 C10 C15 126.3(7) . . ? C11 C10 C15 125.7(7) . . ? C12 C11 C10 107.1(7) . . ? C13 C12 C11 108.7(7) . . ? C14 C13 C12 107.0(7) . . ? C10 C14 C13 109.7(7) . . ? C18 C15 C10 112.5(7) . . ? C18 C15 C16 110.5(7) . . ? C10 C15 C16 109.8(6) . . ? C18 C15 C17 110.3(6) . . ? C10 C15 C17 107.0(6) . . ? C16 C15 C17 106.6(7) . . ? C20 C19 C23 106.2(6) . . ? C20 C19 C24 128.4(7) . . ? C23 C19 C24 123.5(6) . . ? C21 C20 C19 109.6(7) . . ? C20 C21 C22 107.9(7) . . ? C23 C22 C21 107.6(7) . . ? C22 C23 C19 108.8(7) . . ? C27 C24 C19 112.4(6) . . ? C27 C24 C26 109.3(6) . . ? C19 C24 C26 111.5(6) . . ? C27 C24 C25 108.1(7) . . ? C19 C24 C25 107.0(6) . . ? C26 C24 C25 108.5(7) . . ? N C28 C29 123.5(7) . . ? C28 C29 C30 119.0(7) . . ? C29 C30 C31 118.1(7) . . ? C32 C31 C30 118.7(7) . . ? N C32 C31 124.1(8) . . ? #===END data_(Ce,SiMe~3~,pyridine) _database_code_depnum_ccdc_archive 'CCDC 223526' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H44 Ce N Si3' _chemical_formula_weight 631.04 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' Si Si 0.0817 0.0704 '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 11.1698(11) _cell_length_b 11.2011(11) _cell_length_c 13.7417(9) _cell_angle_alpha 98.786(6) _cell_angle_beta 109.589(5) _cell_angle_gamma 96.900(3) _cell_volume 1573.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10763 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method ? _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 1.578 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.676 _exptl_absorpt_correction_T_max 0.855 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_decay_% none _diffrn_reflns_number 10763 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5467 _reflns_number_gt 4505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. One of the Si(Me)3 groups was found disordered over two positions which were refined with occupancy factors constrained to sum to unity and some restraints on bond lengths, angles and displacement parameters (SIMU). All non-hydrogen atoms were refined with anisotropic displacement parameters, except the disordered ones. The H atoms were introduced (except in the disordered group) at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH3) times that of the parent atom. 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^)+(0.0446P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5467 _refine_ls_number_parameters 312 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.924 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.101 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 Ce Ce 0.49224(3) 0.71955(3) 0.27760(2) 0.02839(11) Uani 1 1 d . . . Si1 Si 0.89146(14) 0.81734(16) 0.32315(12) 0.0419(4) Uani 1 1 d . . . Si2 Si 0.29759(16) 0.93933(16) 0.07938(14) 0.0455(4) Uani 1 1 d . . . Si3 Si 0.16927(17) 0.41397(15) 0.21982(13) 0.0480(4) Uani 1 1 d D . . N N 0.6209(4) 0.5295(4) 0.2931(3) 0.0350(10) Uani 1 1 d . . . C1 C 0.7488(5) 0.8560(5) 0.3557(4) 0.0382(12) Uani 1 1 d . . . C2 C 0.6694(5) 0.9384(5) 0.3115(4) 0.0376(12) Uani 1 1 d . . . H2 H 0.6669 0.9673 0.2510 0.045 Uiso 1 1 calc R . . C3 C 0.5958(5) 0.9695(5) 0.3725(5) 0.0427(13) Uani 1 1 d . . . H3 H 0.5348 1.0203 0.3592 0.051 Uiso 1 1 calc R . . C4 C 0.6315(5) 0.9090(5) 0.4588(4) 0.0404(13) Uani 1 1 d . . . H4 H 0.5992 0.9146 0.5132 0.048 Uiso 1 1 calc R . . C5 C 0.7232(5) 0.8398(5) 0.4475(4) 0.0411(13) Uani 1 1 d . . . H5 H 0.7618 0.7905 0.4931 0.049 Uiso 1 1 calc R . . C6 C 0.9787(6) 0.7245(8) 0.4152(6) 0.072(2) Uani 1 1 d . . . H6A H 1.0620 0.7215 0.4101 0.108 Uiso 1 1 calc R . . H6B H 0.9297 0.6426 0.3970 0.108 Uiso 1 1 calc R . . H6C H 0.9896 0.7613 0.4862 0.108 Uiso 1 1 calc R . . C7 C 0.8460(5) 0.7353(6) 0.1831(5) 0.0502(15) Uani 1 1 d . . . H7A H 0.9228 0.7311 0.1669 0.075 Uiso 1 1 calc R . . H7B H 0.7916 0.7790 0.1368 0.075 Uiso 1 1 calc R . . H7C H 0.8004 0.6536 0.1737 0.075 Uiso 1 1 calc R . . C8 C 1.0005(6) 0.9644(6) 0.3420(5) 0.0602(19) Uani 1 1 d . . . H8A H 1.0258 1.0087 0.4134 0.090 Uiso 1 1 calc R . . H8B H 0.9562 1.0129 0.2945 0.090 Uiso 1 1 calc R . . H8C H 1.0760 0.9478 0.3277 0.090 Uiso 1 1 calc R . . C9 C 0.3654(5) 0.7959(5) 0.0867(4) 0.0366(12) Uani 1 1 d . . . C10 C 0.4857(5) 0.7778(5) 0.0804(4) 0.0333(11) Uani 1 1 d . . . H10 H 0.5509 0.8399 0.0833 0.040 Uiso 1 1 calc R . . C11 C 0.4924(5) 0.6533(5) 0.0689(4) 0.0345(11) Uani 1 1 d . . . H11 H 0.5621 0.6185 0.0636 0.041 Uiso 1 1 calc R . . C12 C 0.3748(5) 0.5894(5) 0.0670(4) 0.0377(12) Uani 1 1 d . . . H12 H 0.3534 0.5050 0.0607 0.045 Uiso 1 1 calc R . . C13 C 0.2955(5) 0.6752(5) 0.0762(4) 0.0369(12) Uani 1 1 d . . . H13 H 0.2117 0.6572 0.0755 0.044 Uiso 1 1 calc R . . C14 C 0.1936(7) 0.9339(7) -0.0617(6) 0.0675(19) Uani 1 1 d . . . H14A H 0.1519 1.0040 -0.0652 0.101 Uiso 1 1 calc R . . H14B H 0.1294 0.8601 -0.0878 0.101 Uiso 1 1 calc R . . H14C H 0.2466 0.9347 -0.1041 0.101 Uiso 1 1 calc R . . C15 C 0.1928(7) 0.9513(7) 0.1610(6) 0.071(2) Uani 1 1 d U . . H15A H 0.2460 0.9689 0.2345 0.107 Uiso 1 1 calc R . . H15B H 0.1337 0.8751 0.1443 0.107 Uiso 1 1 calc R . . H15C H 0.1450 1.0163 0.1459 0.107 Uiso 1 1 calc R . . C16 C 0.4308(6) 1.0740(5) 0.1222(5) 0.0528(15) Uani 1 1 d . . . H16A H 0.4767 1.0862 0.1968 0.079 Uiso 1 1 calc R . . H16B H 0.3957 1.1458 0.1062 0.079 Uiso 1 1 calc R . . H16C H 0.4891 1.0596 0.0856 0.079 Uiso 1 1 calc R . . C17 C 0.2812(4) 0.5574(4) 0.2992(4) 0.0335(11) Uani 1 1 d D . . C18 C 0.2533(5) 0.6793(5) 0.3113(4) 0.0389(12) Uani 1 1 d . . . H18 H 0.1852 0.7053 0.2640 0.047 Uiso 1 1 calc R . . C19 C 0.3432(5) 0.7530(5) 0.4041(4) 0.0416(13) Uani 1 1 d . . . H19 H 0.3455 0.8355 0.4292 0.050 Uiso 1 1 calc R . . C20 C 0.4300(6) 0.6803(6) 0.4532(4) 0.0474(15) Uani 1 1 d . . . H20 H 0.5002 0.7059 0.5164 0.057 Uiso 1 1 calc R . . C21 C 0.3917(5) 0.5636(5) 0.3902(4) 0.0407(13) Uani 1 1 d . . . H21 H 0.4330 0.4978 0.4055 0.049 Uiso 1 1 calc R . . C22A C 0.2721(12) 0.3007(9) 0.1903(11) 0.081(4) Uiso 0.552(9) 1 d PDU . . C22B C 0.1861(14) 0.3411(11) 0.1000(8) 0.061(4) Uiso 0.448(9) 1 d PDU . . C23A C 0.0588(10) 0.4341(11) 0.0908(7) 0.070(4) Uiso 0.552(9) 1 d PD . . C23B C -0.0010(8) 0.4535(14) 0.1738(13) 0.078(5) Uiso 0.448(9) 1 d PD . . C24A C 0.0797(11) 0.3513(10) 0.2992(9) 0.060(3) Uiso 0.552(9) 1 d PDU . . C24B C 0.1538(15) 0.3036(10) 0.3067(10) 0.066(4) Uiso 0.448(9) 1 d PDU . . C25 C 0.6836(5) 0.5102(5) 0.3915(4) 0.0377(12) Uani 1 1 d . . . H25 H 0.6821 0.5646 0.4492 0.045 Uiso 1 1 calc R . . C26 C 0.7484(5) 0.4155(6) 0.4099(5) 0.0441(13) Uani 1 1 d . . . H26 H 0.7900 0.4065 0.4786 0.053 Uiso 1 1 calc R . . C27 C 0.7516(6) 0.3333(5) 0.3257(5) 0.0487(14) Uani 1 1 d . . . H27 H 0.7951 0.2680 0.3365 0.058 Uiso 1 1 calc R . . C28 C 0.6889(6) 0.3502(5) 0.2249(5) 0.0458(14) Uani 1 1 d . . . H28 H 0.6898 0.2966 0.1665 0.055 Uiso 1 1 calc R . . C29 C 0.6248(5) 0.4479(5) 0.2123(4) 0.0384(12) Uani 1 1 d . . . H29 H 0.5820 0.4578 0.1441 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.02729(16) 0.02956(16) 0.02631(16) 0.00221(10) 0.00945(11) 0.00280(11) Si1 0.0298(8) 0.0541(10) 0.0408(9) 0.0084(7) 0.0137(6) 0.0027(7) Si2 0.0442(9) 0.0469(10) 0.0543(10) 0.0177(8) 0.0229(8) 0.0172(8) Si3 0.0551(10) 0.0371(9) 0.0466(9) 0.0013(7) 0.0178(8) -0.0006(8) N 0.036(2) 0.036(2) 0.032(2) 0.0079(18) 0.0101(18) 0.0063(19) C1 0.033(3) 0.042(3) 0.033(3) 0.004(2) 0.010(2) -0.006(2) C2 0.035(3) 0.034(3) 0.040(3) 0.002(2) 0.014(2) -0.002(2) C3 0.040(3) 0.036(3) 0.048(3) -0.002(2) 0.017(3) 0.002(2) C4 0.042(3) 0.036(3) 0.036(3) -0.009(2) 0.015(2) -0.004(2) C5 0.036(3) 0.041(3) 0.039(3) 0.006(2) 0.010(2) -0.006(2) C6 0.040(4) 0.115(7) 0.085(5) 0.050(5) 0.034(4) 0.028(4) C7 0.033(3) 0.053(4) 0.059(4) -0.002(3) 0.018(3) 0.004(3) C8 0.043(4) 0.080(5) 0.043(4) -0.008(3) 0.016(3) -0.021(3) C9 0.030(3) 0.044(3) 0.034(3) 0.008(2) 0.009(2) 0.006(2) C10 0.038(3) 0.036(3) 0.027(3) 0.005(2) 0.016(2) 0.004(2) C11 0.037(3) 0.039(3) 0.024(3) 0.000(2) 0.009(2) 0.008(2) C12 0.043(3) 0.032(3) 0.030(3) 0.001(2) 0.007(2) 0.000(2) C13 0.033(3) 0.042(3) 0.029(3) 0.006(2) 0.005(2) 0.000(2) C14 0.061(4) 0.065(5) 0.075(5) 0.032(4) 0.012(4) 0.024(4) C15 0.079(5) 0.063(4) 0.103(5) 0.034(4) 0.058(4) 0.031(4) C16 0.064(4) 0.045(4) 0.060(4) 0.020(3) 0.029(3) 0.018(3) C17 0.027(3) 0.032(3) 0.041(3) 0.007(2) 0.013(2) 0.003(2) C18 0.032(3) 0.042(3) 0.051(3) 0.013(3) 0.024(2) 0.010(2) C19 0.044(3) 0.034(3) 0.048(3) -0.005(2) 0.028(3) -0.005(2) C20 0.040(3) 0.060(4) 0.033(3) 0.005(3) 0.011(2) -0.010(3) C21 0.028(3) 0.053(4) 0.041(3) 0.016(3) 0.011(2) 0.001(2) C25 0.032(3) 0.052(3) 0.032(3) 0.010(2) 0.013(2) 0.010(2) C26 0.038(3) 0.056(4) 0.040(3) 0.020(3) 0.012(2) 0.010(3) C27 0.046(3) 0.042(3) 0.063(4) 0.021(3) 0.018(3) 0.019(3) C28 0.050(4) 0.031(3) 0.051(3) -0.002(2) 0.015(3) 0.008(3) C29 0.041(3) 0.036(3) 0.038(3) 0.005(2) 0.013(2) 0.011(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 Ce N 2.704(4) . ? Ce C19 2.797(5) . ? Ce C20 2.807(5) . ? Ce C12 2.816(5) . ? Ce C3 2.823(5) . ? Ce C13 2.825(5) . ? Ce C2 2.830(5) . ? Ce C5 2.843(5) . ? Ce C1 2.843(5) . ? Ce C9 2.847(5) . ? Ce C4 2.849(5) . ? Ce C11 2.851(5) . ? Ce C18 2.853(5) . ? Ce C10 2.863(5) . ? Ce C21 2.868(5) . ? Ce C17 2.924(5) . ? Si1 C8 1.855(6) . ? Si1 C6 1.858(7) . ? Si1 C7 1.871(6) . ? Si1 C1 1.873(6) . ? Si2 C16 1.854(6) . ? Si2 C9 1.859(6) . ? Si2 C15 1.876(6) . ? Si2 C14 1.884(7) . ? Si3 C22B 1.802(8) . ? Si3 C17 1.844(4) . ? Si3 C23A 1.855(8) . ? Si3 C24A 1.865(7) . ? Si3 C24B 1.877(8) . ? Si3 C22A 1.896(8) . ? Si3 C23B 1.922(8) . ? N C29 1.343(6) . ? N C25 1.362(6) . ? C1 C2 1.419(8) . ? C1 C5 1.416(7) . ? C2 C3 1.393(7) . ? C3 C4 1.420(8) . ? C4 C5 1.391(8) . ? C9 C10 1.413(7) . ? C9 C13 1.438(7) . ? C10 C11 1.394(7) . ? C11 C12 1.409(7) . ? C12 C13 1.403(8) . ? C17 C21 1.418(7) . ? C17 C18 1.435(7) . ? C18 C19 1.392(8) . ? C19 C20 1.406(8) . ? C20 C21 1.383(8) . ? C25 C26 1.362(8) . ? C26 C27 1.378(8) . ? C27 C28 1.380(8) . ? C28 C29 1.378(8) . ? 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 N Ce C19 117.34(15) . . ? N Ce C20 89.72(16) . . ? C19 Ce C20 29.07(17) . . ? N Ce C12 81.60(14) . . ? C19 Ce C12 119.89(16) . . ? C20 Ce C12 128.25(16) . . ? N Ce C3 126.90(15) . . ? C19 Ce C3 81.76(16) . . ? C20 Ce C3 91.25(17) . . ? C12 Ce C3 133.82(16) . . ? N Ce C13 109.60(14) . . ? C19 Ce C13 99.57(16) . . ? C20 Ce C13 119.98(16) . . ? C12 Ce C13 28.81(15) . . ? C3 Ce C13 115.37(17) . . ? N Ce C2 108.96(14) . . ? C19 Ce C2 110.23(15) . . ? C20 Ce C2 115.25(16) . . ? C12 Ce C2 115.82(16) . . ? C3 Ce C2 28.53(15) . . ? C13 Ce C2 110.79(16) . . ? N Ce C5 81.23(15) . . ? C19 Ce C5 91.95(16) . . ? C20 Ce C5 78.34(16) . . ? C12 Ce C5 148.06(16) . . ? C3 Ce C5 47.30(17) . . ? C13 Ce C5 157.69(16) . . ? C2 Ce C5 46.97(16) . . ? N Ce C1 81.47(15) . . ? C19 Ce C1 117.68(15) . . ? C20 Ce C1 107.18(16) . . ? C12 Ce C1 121.49(15) . . ? C3 Ce C1 47.87(16) . . ? C13 Ce C1 131.06(15) . . ? C2 Ce C1 28.97(16) . . ? C5 Ce C1 28.84(15) . . ? N Ce C9 125.26(14) . . ? C19 Ce C9 107.25(16) . . ? C20 Ce C9 135.32(17) . . ? C12 Ce C9 48.08(16) . . ? C3 Ce C9 88.00(17) . . ? C13 Ce C9 29.37(15) . . ? C2 Ce C9 81.67(16) . . ? C5 Ce C9 128.61(15) . . ? C1 Ce C9 105.04(15) . . ? N Ce C4 107.29(15) . . ? C19 Ce C4 70.46(15) . . ? C20 Ce C4 68.28(16) . . ? C12 Ce C4 162.16(16) . . ? C3 Ce C4 29.00(16) . . ? C13 Ce C4 142.06(17) . . ? C2 Ce C4 47.02(16) . . ? C5 Ce C4 28.30(16) . . ? C1 Ce C4 47.48(15) . . ? C9 Ce C4 116.69(16) . . ? N Ce C11 78.22(14) . . ? C19 Ce C11 146.58(16) . . ? C20 Ce C11 154.90(16) . . ? C12 Ce C11 28.78(14) . . ? C3 Ce C11 113.63(16) . . ? C13 Ce C11 47.28(15) . . ? C2 Ce C11 89.61(15) . . ? C5 Ce C11 120.58(15) . . ? C1 Ce C11 92.86(15) . . ? C9 Ce C11 47.60(15) . . ? C4 Ce C11 136.26(15) . . ? C8 Si1 C6 108.9(3) . . ? C8 Si1 C7 107.5(3) . . ? C6 Si1 C7 110.4(3) . . ? C8 Si1 C1 107.3(3) . . ? C6 Si1 C1 109.6(3) . . ? C7 Si1 C1 112.9(2) . . ? C16 Si2 C9 109.8(3) . . ? C16 Si2 C15 111.8(3) . . ? C9 Si2 C15 110.1(3) . . ? C16 Si2 C14 108.2(3) . . ? C9 Si2 C14 109.0(3) . . ? C15 Si2 C14 107.9(4) . . ? C22B Si3 C17 119.2(4) . . ? C17 Si3 C23A 112.7(4) . . ? C17 Si3 C24A 109.2(4) . . ? C23A Si3 C24A 112.2(6) . . ? C22B Si3 C24B 112.8(7) . . ? C17 Si3 C24B 110.4(4) . . ? C17 Si3 C22A 106.9(4) . . ? C23A Si3 C22A 106.8(6) . . ? C24A Si3 C22A 108.9(6) . . ? C22B Si3 C23B 104.2(7) . . ? C17 Si3 C23B 106.6(4) . . ? C24B Si3 C23B 101.6(8) . . ? C29 N C25 116.0(5) . . ? C29 N Ce 126.2(3) . . ? C25 N Ce 117.8(3) . . ? C2 C1 C5 105.8(5) . . ? C2 C1 Si1 125.6(4) . . ? C5 C1 Si1 126.2(4) . . ? C2 C1 Ce 75.0(3) . . ? C5 C1 Ce 75.6(3) . . ? Si1 C1 Ce 128.5(2) . . ? C3 C2 C1 109.6(5) . . ? C3 C2 Ce 75.4(3) . . ? C1 C2 Ce 76.0(3) . . ? C2 C3 C4 107.2(5) . . ? C2 C3 Ce 76.0(3) . . ? C4 C3 Ce 76.5(3) . . ? C5 C4 C3 107.9(5) . . ? C5 C4 Ce 75.6(3) . . ? C3 C4 Ce 74.5(3) . . ? C4 C5 C1 109.4(5) . . ? C4 C5 Ce 76.1(3) . . ? C1 C5 Ce 75.6(3) . . ? C10 C9 C13 105.5(5) . . ? C10 C9 Si2 126.7(4) . . ? C13 C9 Si2 126.4(4) . . ? C10 C9 Ce 76.3(3) . . ? C13 C9 Ce 74.5(3) . . ? Si2 C9 Ce 124.6(2) . . ? C11 C10 C9 110.0(5) . . ? C11 C10 Ce 75.4(3) . . ? C9 C10 Ce 75.0(3) . . ? C10 C11 C12 107.8(5) . . ? C10 C11 Ce 76.4(3) . . ? C12 C11 Ce 74.2(3) . . ? C13 C12 C11 108.1(5) . . ? C13 C12 Ce 75.9(3) . . ? C11 C12 Ce 77.0(3) . . ? C12 C13 C9 108.6(5) . . ? C12 C13 Ce 75.3(3) . . ? C9 C13 Ce 76.2(3) . . ? C21 C17 C18 103.7(4) . . ? C21 C17 Si3 124.4(4) . . ? C18 C17 Si3 127.7(4) . . ? C21 C17 Ce 73.7(3) . . ? C18 C17 Ce 72.9(3) . . ? Si3 C17 Ce 135.5(2) . . ? C19 C18 C17 110.0(5) . . ? C19 C18 Ce 73.5(3) . . ? C17 C18 Ce 78.4(3) . . ? C18 C19 C20 107.7(5) . . ? C18 C19 Ce 78.0(3) . . ? C20 C19 Ce 75.8(3) . . ? C21 C20 C19 107.4(5) . . ? C21 C20 Ce 78.4(3) . . ? C19 C20 Ce 75.1(3) . . ? C20 C21 C17 111.2(5) . . ? C20 C21 Ce 73.4(3) . . ? C17 C21 Ce 78.0(3) . . ? N C25 C26 123.5(5) . . ? C25 C26 C27 119.4(5) . . ? C28 C27 C26 118.5(5) . . ? C27 C28 C29 118.9(5) . . ? N C29 C28 123.6(5) . . ? #===END data_(U,SiMe~3~,pyridine) _database_code_depnum_ccdc_archive 'CCDC 223527' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H44 N Si3 U' _chemical_formula_weight 728.95 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 11.1739(14) _cell_length_b 11.1737(15) _cell_length_c 13.7093(16) _cell_angle_alpha 98.747(6) _cell_angle_beta 109.359(8) _cell_angle_gamma 97.321(6) _cell_volume 1566.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10766 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 25.68 _exptl_crystal_description needle _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method ? _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 5.312 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 0.758 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 10766 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5488 _reflns_number_gt 4350 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. One of the Si(Me)3 groups was found disordered over two positions which were refined with occupancy factors constrained to sum to unity and some restraints on bond lengths, angles and displacement parameters (SIMU). All non-hydrogen atoms were refined with anisotropic displacement parameters, except the disordered ones. The H atoms were introduced (except in the disordered group) at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH3) times that of the parent atom. 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^)+(0.0550P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5488 _refine_ls_number_parameters 312 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1285 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 1.822 _refine_diff_density_min -2.915 _refine_diff_density_rms 0.176 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 U U 0.49302(3) 0.71890(3) 0.27756(3) 0.02939(13) Uani 1 1 d . . . Si1 Si 0.8911(3) 0.8164(3) 0.3222(2) 0.0441(7) Uani 1 1 d . . . Si2 Si 0.2990(3) 0.9385(3) 0.0814(3) 0.0446(7) Uani 1 1 d . . . Si3 Si 0.1687(3) 0.4127(3) 0.2188(2) 0.0425(7) Uani 1 1 d D . . N N 0.6216(7) 0.5314(7) 0.2943(6) 0.0353(18) Uani 1 1 d . . . C1 C 0.7488(9) 0.8520(10) 0.3543(8) 0.043(3) Uani 1 1 d . . . C2 C 0.6696(9) 0.9359(9) 0.3111(7) 0.037(2) Uani 1 1 d . . . H2 H 0.6680 0.9664 0.2513 0.044 Uiso 1 1 calc R . . C3 C 0.5948(10) 0.9653(9) 0.3721(8) 0.042(2) Uani 1 1 d . . . H3 H 0.5324 1.0144 0.3580 0.050 Uiso 1 1 calc R . . C4 C 0.6308(9) 0.9076(9) 0.4582(7) 0.037(2) Uani 1 1 d . . . H4 H 0.5994 0.9142 0.5133 0.045 Uiso 1 1 calc R . . C5 C 0.7217(9) 0.8391(9) 0.4465(7) 0.038(2) Uani 1 1 d . . . H5 H 0.7600 0.7907 0.4931 0.046 Uiso 1 1 calc R . . C6 C 0.9765(11) 0.7251(15) 0.4143(11) 0.073(4) Uani 1 1 d . . . H6A H 1.0477 0.7026 0.3960 0.109 Uiso 1 1 calc R . . H6B H 0.9181 0.6518 0.4097 0.109 Uiso 1 1 calc R . . H6C H 1.0083 0.7732 0.4851 0.109 Uiso 1 1 calc R . . C7 C 0.8466(10) 0.7343(11) 0.1815(8) 0.050(3) Uani 1 1 d . . . H7A H 0.9234 0.7343 0.1646 0.075 Uiso 1 1 calc R . . H7B H 0.7893 0.7758 0.1355 0.075 Uiso 1 1 calc R . . H7C H 0.8045 0.6508 0.1726 0.075 Uiso 1 1 calc R . . C8 C 1.0007(11) 0.9656(13) 0.3424(9) 0.070(4) Uani 1 1 d . . . H8A H 1.0225 1.0109 0.4133 0.105 Uiso 1 1 calc R . . H8B H 0.9579 1.0130 0.2932 0.105 Uiso 1 1 calc R . . H8C H 1.0780 0.9499 0.3310 0.105 Uiso 1 1 calc R . . C9 C 0.3653(8) 0.7959(10) 0.0888(8) 0.038(2) Uani 1 1 d . . . C10 C 0.4887(9) 0.7789(9) 0.0823(7) 0.036(2) Uani 1 1 d . . . H10 H 0.5544 0.8410 0.0852 0.044 Uiso 1 1 calc R . . C11 C 0.4922(9) 0.6513(9) 0.0708(7) 0.034(2) Uani 1 1 d . . . H11 H 0.5609 0.6155 0.0649 0.040 Uiso 1 1 calc R . . C12 C 0.3744(9) 0.5876(9) 0.0699(7) 0.034(2) Uani 1 1 d . . . H12 H 0.3525 0.5030 0.0641 0.041 Uiso 1 1 calc R . . C13 C 0.2960(9) 0.6737(10) 0.0790(8) 0.041(2) Uani 1 1 d . . . H13 H 0.2124 0.6551 0.0788 0.049 Uiso 1 1 calc R . . C14 C 0.1957(11) 0.9324(11) -0.0580(10) 0.060(3) Uani 1 1 d . . . H14A H 0.1657 1.0088 -0.0632 0.090 Uiso 1 1 calc R . . H14B H 0.1230 0.8658 -0.0799 0.090 Uiso 1 1 calc R . . H14C H 0.2452 0.9196 -0.1027 0.090 Uiso 1 1 calc R . . C15 C 0.1962(13) 0.9528(12) 0.1648(12) 0.073(4) Uani 1 1 d . . . H15A H 0.2505 0.9735 0.2382 0.109 Uiso 1 1 calc R . . H15B H 0.1382 0.8758 0.1508 0.109 Uiso 1 1 calc R . . H15C H 0.1472 1.0164 0.1483 0.109 Uiso 1 1 calc R . . C16 C 0.4346(11) 1.0737(10) 0.1242(9) 0.048(3) Uani 1 1 d . . . H16A H 0.4843 1.0823 0.1978 0.072 Uiso 1 1 calc R . . H16B H 0.4003 1.1471 0.1132 0.072 Uiso 1 1 calc R . . H16C H 0.4890 1.0613 0.0836 0.072 Uiso 1 1 calc R . . C17 C 0.2813(7) 0.5562(7) 0.2966(6) 0.034(2) Uani 1 1 d D . . C18 C 0.2547(9) 0.6777(9) 0.3096(9) 0.040(2) Uani 1 1 d . . . H18 H 0.1871 0.7043 0.2628 0.048 Uiso 1 1 calc R . . C19 C 0.3459(10) 0.7513(10) 0.4036(8) 0.043(3) Uani 1 1 d . . . H19 H 0.3482 0.8339 0.4293 0.052 Uiso 1 1 calc R . . C20 C 0.4330(10) 0.6797(10) 0.4525(8) 0.044(3) Uani 1 1 d . . . H20 H 0.5041 0.7056 0.5151 0.053 Uiso 1 1 calc R . . C21 C 0.3915(9) 0.5615(10) 0.3885(7) 0.039(2) Uani 1 1 d . . . H21 H 0.4308 0.4946 0.4037 0.047 Uiso 1 1 calc R . . C22A C 0.0609(18) 0.4326(18) 0.0883(10) 0.067(7) Uiso 0.531(14) 1 d PD . . C22B C -0.0008(9) 0.447(2) 0.174(2) 0.084(10) Uiso 0.469(14) 1 d PD . . C23A C 0.2653(18) 0.2971(14) 0.183(2) 0.077(7) Uiso 0.531(14) 1 d PDU . . C23B C 0.189(2) 0.344(2) 0.0976(14) 0.071(7) Uiso 0.469(14) 1 d PDU . . C24A C 0.0774(18) 0.3501(16) 0.2980(14) 0.056(5) Uiso 0.531(14) 1 d PDU . . C24B C 0.156(2) 0.3021(15) 0.3068(15) 0.060(6) Uiso 0.469(14) 1 d PDU . . C25 C 0.6835(9) 0.5122(10) 0.3915(7) 0.039(2) Uani 1 1 d . . . H25 H 0.6830 0.5675 0.4493 0.047 Uiso 1 1 calc R . . C26 C 0.7464(9) 0.4172(11) 0.4103(8) 0.046(3) Uani 1 1 d . . . H26 H 0.7874 0.4085 0.4792 0.055 Uiso 1 1 calc R . . C27 C 0.7491(10) 0.3344(10) 0.3268(9) 0.049(3) Uani 1 1 d . . . H27 H 0.7911 0.2682 0.3379 0.058 Uiso 1 1 calc R . . C28 C 0.6883(10) 0.3511(10) 0.2261(8) 0.045(2) Uani 1 1 d . . . H28 H 0.6901 0.2975 0.1679 0.054 Uiso 1 1 calc R . . C29 C 0.6242(9) 0.4497(8) 0.2127(8) 0.036(2) Uani 1 1 d . . . H29 H 0.5813 0.4594 0.1444 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02758(18) 0.0298(2) 0.02823(19) 0.00229(13) 0.00971(14) 0.00157(12) Si1 0.0286(13) 0.058(2) 0.0404(15) 0.0049(14) 0.0119(13) -0.0037(13) Si2 0.0413(15) 0.0448(18) 0.0549(18) 0.0154(14) 0.0226(15) 0.0135(13) Si3 0.0477(16) 0.0301(15) 0.0422(15) 0.0025(12) 0.0108(14) 0.0018(12) N 0.032(4) 0.037(5) 0.035(4) 0.006(4) 0.012(4) 0.001(3) C1 0.026(5) 0.054(7) 0.034(5) 0.000(5) 0.000(4) -0.007(4) C2 0.036(5) 0.040(6) 0.027(5) -0.003(4) 0.010(4) -0.003(4) C3 0.042(5) 0.031(5) 0.045(6) -0.008(4) 0.017(5) -0.004(4) C4 0.041(5) 0.034(6) 0.031(5) -0.010(4) 0.017(5) -0.007(4) C5 0.047(6) 0.034(6) 0.033(5) 0.010(4) 0.018(5) -0.004(4) C6 0.040(6) 0.114(12) 0.076(9) 0.041(8) 0.024(7) 0.023(7) C7 0.035(5) 0.057(7) 0.048(6) -0.007(5) 0.016(5) -0.006(5) C8 0.048(7) 0.094(11) 0.048(7) -0.013(7) 0.021(6) -0.033(7) C9 0.025(4) 0.046(6) 0.043(5) 0.012(5) 0.009(4) 0.007(4) C10 0.031(5) 0.048(6) 0.033(5) 0.013(4) 0.012(4) 0.015(4) C11 0.033(5) 0.040(6) 0.028(5) 0.008(4) 0.011(4) 0.007(4) C12 0.037(5) 0.029(5) 0.023(4) -0.003(4) -0.001(4) -0.001(4) C13 0.030(5) 0.049(7) 0.036(5) 0.002(5) 0.008(4) 0.001(4) C14 0.047(6) 0.053(8) 0.079(9) 0.020(6) 0.016(6) 0.015(6) C15 0.086(9) 0.047(8) 0.112(12) 0.022(7) 0.060(9) 0.031(7) C16 0.059(7) 0.039(6) 0.052(6) 0.019(5) 0.024(6) 0.007(5) C17 0.030(5) 0.037(6) 0.034(5) 0.006(4) 0.014(4) 0.002(4) C18 0.033(5) 0.044(6) 0.056(6) 0.015(5) 0.030(5) 0.014(4) C19 0.052(6) 0.037(6) 0.044(6) -0.008(5) 0.035(5) -0.008(5) C20 0.037(5) 0.057(7) 0.031(5) 0.006(5) 0.013(5) -0.010(5) C21 0.029(5) 0.052(6) 0.032(5) 0.009(5) 0.009(4) -0.004(4) C25 0.039(5) 0.054(7) 0.027(5) 0.015(4) 0.011(5) 0.015(5) C26 0.036(5) 0.071(8) 0.041(6) 0.032(6) 0.013(5) 0.020(5) C27 0.042(6) 0.045(7) 0.058(7) 0.015(5) 0.012(6) 0.015(5) C28 0.051(6) 0.040(6) 0.043(6) 0.002(5) 0.018(5) 0.009(5) C29 0.041(5) 0.022(5) 0.037(5) 0.004(4) 0.007(5) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U N 2.683(8) . ? U C19 2.769(9) . ? U C3 2.774(9) . ? U C20 2.776(10) . ? U C12 2.784(8) . ? U C13 2.799(9) . ? U C2 2.797(9) . ? U C1 2.817(9) . ? U C11 2.816(9) . ? U C5 2.820(9) . ? U C9 2.830(10) . ? U C4 2.829(8) . ? U C18 2.832(9) . ? U C10 2.843(10) . ? U C21 2.853(8) . ? U C17 2.903(9) . ? Si1 C6 1.840(13) . ? Si1 C1 1.858(11) . ? Si1 C8 1.863(12) . ? Si1 C7 1.876(10) . ? Si2 C9 1.845(11) . ? Si2 C14 1.862(12) . ? Si2 C16 1.865(11) . ? Si2 C15 1.874(13) . ? Si3 C23B 1.818(9) . ? Si3 C17 1.835(7) . ? Si3 C22A 1.861(9) . ? Si3 C24A 1.869(9) . ? Si3 C24B 1.877(9) . ? Si3 C23A 1.895(9) . ? Si3 C22B 1.897(9) . ? N C29 1.343(12) . ? N C25 1.346(12) . ? C1 C5 1.418(14) . ? C1 C2 1.430(15) . ? C2 C3 1.398(14) . ? C3 C4 1.397(15) . ? C4 C5 1.382(14) . ? C9 C13 1.445(14) . ? C9 C10 1.444(13) . ? C10 C11 1.418(14) . ? C11 C12 1.409(13) . ? C12 C13 1.399(14) . ? C17 C18 1.424(13) . ? C17 C21 1.427(12) . ? C18 C19 1.403(14) . ? C19 C20 1.402(16) . ? C20 C21 1.397(15) . ? C25 C26 1.357(15) . ? C26 C27 1.369(15) . ? C27 C28 1.375(15) . ? C28 C29 1.391(14) . ? 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 N U C19 117.1(3) . . ? N U C3 126.5(3) . . ? C19 U C3 81.4(3) . . ? N U C20 89.3(3) . . ? C19 U C20 29.3(3) . . ? C3 U C20 90.7(3) . . ? N U C12 82.1(3) . . ? C19 U C12 119.3(3) . . ? C3 U C12 134.7(3) . . ? C20 U C12 127.7(3) . . ? N U C13 110.3(3) . . ? C19 U C13 99.0(3) . . ? C3 U C13 115.7(3) . . ? C20 U C13 119.7(3) . . ? C12 U C13 29.0(3) . . ? N U C2 108.4(3) . . ? C19 U C2 110.4(3) . . ? C3 U C2 29.1(3) . . ? C20 U C2 115.0(3) . . ? C12 U C2 116.6(3) . . ? C13 U C2 111.4(3) . . ? N U C1 80.2(3) . . ? C19 U C1 118.1(3) . . ? C3 U C1 48.9(3) . . ? C20 U C1 106.9(3) . . ? C12 U C1 121.9(3) . . ? C13 U C1 131.9(3) . . ? C2 U C1 29.5(3) . . ? N U C11 78.3(3) . . ? C19 U C11 146.5(3) . . ? C3 U C11 114.5(3) . . ? C20 U C11 154.6(3) . . ? C12 U C11 29.1(3) . . ? C13 U C11 47.8(3) . . ? C2 U C11 90.0(3) . . ? C1 U C11 92.9(3) . . ? N U C5 80.7(3) . . ? C19 U C5 91.7(3) . . ? C3 U C5 47.3(3) . . ? C20 U C5 77.8(3) . . ? C12 U C5 148.9(3) . . ? C13 U C5 158.4(3) . . ? C2 U C5 47.0(3) . . ? C1 U C5 29.1(3) . . ? C11 U C5 121.1(3) . . ? N U C9 126.3(3) . . ? C19 U C9 106.7(3) . . ? C3 U C9 88.0(3) . . ? C20 U C9 135.0(3) . . ? C12 U C9 48.8(3) . . ? C13 U C9 29.7(3) . . ? C2 U C9 81.9(3) . . ? C1 U C9 105.8(3) . . ? C11 U C9 48.5(3) . . ? C5 U C9 128.9(3) . . ? N U C4 106.8(3) . . ? C19 U C4 70.2(3) . . ? C3 U C4 28.9(3) . . ? C20 U C4 67.8(3) . . ? C12 U C4 163.1(3) . . ? C13 U C4 142.0(3) . . ? C2 U C4 47.3(3) . . ? C1 U C4 48.3(3) . . ? C11 U C4 137.0(3) . . ? C5 U C4 28.3(3) . . ? C9 U C4 116.5(3) . . ? C6 Si1 C1 108.9(5) . . ? C6 Si1 C8 108.8(6) . . ? C1 Si1 C8 107.6(6) . . ? C6 Si1 C7 110.9(6) . . ? C1 Si1 C7 112.8(5) . . ? C8 Si1 C7 107.8(5) . . ? C9 Si2 C14 109.1(5) . . ? C9 Si2 C16 109.3(5) . . ? C14 Si2 C16 108.6(5) . . ? C9 Si2 C15 110.4(5) . . ? C14 Si2 C15 108.2(6) . . ? C16 Si2 C15 111.2(6) . . ? C23B Si3 C17 116.6(7) . . ? C17 Si3 C22A 112.1(6) . . ? C17 Si3 C24A 110.0(5) . . ? C22A Si3 C24A 112.8(10) . . ? C23B Si3 C24B 114.4(11) . . ? C17 Si3 C24B 110.3(6) . . ? C17 Si3 C23A 108.4(6) . . ? C22A Si3 C23A 103.5(11) . . ? C24A Si3 C23A 109.8(11) . . ? C23B Si3 C22B 104.4(13) . . ? C17 Si3 C22B 108.2(6) . . ? C24B Si3 C22B 101.5(13) . . ? C29 N C25 116.3(9) . . ? C29 N U 125.2(6) . . ? C25 N U 118.4(6) . . ? C5 C1 C2 103.7(9) . . ? C5 C1 Si1 127.7(8) . . ? C2 C1 Si1 125.5(8) . . ? C5 C1 U 75.5(5) . . ? C2 C1 U 74.5(5) . . ? Si1 C1 U 129.9(5) . . ? C3 C2 C1 109.9(9) . . ? C3 C2 U 74.5(5) . . ? C1 C2 U 76.0(5) . . ? C4 C3 C2 107.6(10) . . ? C4 C3 U 77.8(5) . . ? C2 C3 U 76.4(5) . . ? C5 C4 C3 107.6(9) . . ? C5 C4 U 75.5(5) . . ? C3 C4 U 73.4(5) . . ? C4 C5 C1 111.1(9) . . ? C4 C5 U 76.2(5) . . ? C1 C5 U 75.3(5) . . ? C13 C9 C10 105.5(9) . . ? C13 C9 Si2 127.1(7) . . ? C10 C9 Si2 126.1(7) . . ? C13 C9 U 73.9(6) . . ? C10 C9 U 75.7(5) . . ? Si2 C9 U 125.3(5) . . ? C11 C10 C9 108.2(8) . . ? C11 C10 U 74.5(5) . . ? C9 C10 U 74.8(5) . . ? C12 C11 C10 108.7(8) . . ? C12 C11 U 74.1(5) . . ? C10 C11 U 76.5(5) . . ? C13 C12 C11 108.2(9) . . ? C13 C12 U 76.1(5) . . ? C11 C12 U 76.7(5) . . ? C12 C13 C9 109.4(9) . . ? C12 C13 U 74.9(5) . . ? C9 C13 U 76.3(5) . . ? C18 C17 C21 103.7(8) . . ? C18 C17 Si3 127.8(7) . . ? C21 C17 Si3 123.6(7) . . ? C18 C17 U 72.9(5) . . ? C21 C17 U 73.7(5) . . ? Si3 C17 U 136.7(4) . . ? C19 C18 C17 109.8(9) . . ? C19 C18 U 73.0(5) . . ? C17 C18 U 78.4(5) . . ? C20 C19 C18 108.7(9) . . ? C20 C19 U 75.7(5) . . ? C18 C19 U 78.0(5) . . ? C21 C20 C19 106.2(9) . . ? C21 C20 U 78.7(6) . . ? C19 C20 U 75.1(5) . . ? C20 C21 C17 111.5(10) . . ? C20 C21 U 72.6(6) . . ? C17 C21 U 77.6(5) . . ? N C25 C26 124.1(10) . . ? C25 C26 C27 119.4(10) . . ? C26 C27 C28 118.5(10) . . ? C27 C28 C29 119.0(10) . . ? N C29 C28 122.7(9) . . ? #===END data_(Ce,Bu^t^,picoline) _database_code_depnum_ccdc_archive 'CCDC 223528' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H46 Ce N' _chemical_formula_weight 596.83 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0203(9) _cell_length_b 8.5826(8) _cell_length_c 31.085(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.788(5) _cell_angle_gamma 90.00 _cell_volume 2936.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19445 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method ? _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 1.570 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.954 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 19445 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5517 _reflns_number_gt 3981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. The highest residual electron density peak is located near the Ce atom, as a result of imperfect absorption corrections. 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^)+(0.0172P)^2^+1.8250P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5517 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.097 _refine_diff_density_min -1.245 _refine_diff_density_rms 0.101 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 Ce Ce 0.08439(2) 0.01720(3) 0.128629(8) 0.03033(10) Uani 1 1 d . . . N N 0.2140(4) -0.1913(4) 0.08646(13) 0.0371(10) Uani 1 1 d . . . C1 C -0.1271(5) -0.1336(5) 0.08113(16) 0.0351(12) Uani 1 1 d . . . C2 C -0.1732(4) -0.0256(6) 0.11028(15) 0.0362(11) Uani 1 1 d . . . H2 H -0.2182 -0.0501 0.1339 0.043 Uiso 1 1 calc R . . C3 C -0.1398(5) 0.1259(6) 0.09776(17) 0.0395(13) Uani 1 1 d . . . H3 H -0.1572 0.2179 0.1120 0.047 Uiso 1 1 calc R . . C4 C -0.0756(5) 0.1134(5) 0.06003(16) 0.0370(12) Uani 1 1 d . . . H4 H -0.0454 0.1956 0.0442 0.044 Uiso 1 1 calc R . . C5 C -0.0651(4) -0.0465(5) 0.05037(15) 0.0347(11) Uani 1 1 d . . . H5 H -0.0241 -0.0879 0.0275 0.042 Uiso 1 1 calc R . . C6 C -0.1627(5) -0.3057(5) 0.07590(16) 0.0360(12) Uani 1 1 d . . . C7 C -0.0621(5) -0.4006(6) 0.05587(18) 0.0473(14) Uani 1 1 d . . . H7A H -0.0874 -0.5072 0.0529 0.071 Uiso 1 1 calc R . . H7B H 0.0106 -0.3951 0.0741 0.071 Uiso 1 1 calc R . . H7C H -0.0465 -0.3589 0.0280 0.071 Uiso 1 1 calc R . . C8 C -0.2764(5) -0.3114(6) 0.04559(19) 0.0527(15) Uani 1 1 d . . . H8A H -0.2593 -0.2634 0.0187 0.079 Uiso 1 1 calc R . . H8B H -0.3414 -0.2565 0.0584 0.079 Uiso 1 1 calc R . . H8C H -0.2997 -0.4179 0.0407 0.079 Uiso 1 1 calc R . . C9 C -0.1953(6) -0.3780(6) 0.11853(18) 0.0552(16) Uani 1 1 d . . . H9A H -0.2583 -0.3178 0.1308 0.083 Uiso 1 1 calc R . . H9B H -0.1249 -0.3791 0.1379 0.083 Uiso 1 1 calc R . . H9C H -0.2233 -0.4828 0.1137 0.083 Uiso 1 1 calc R . . C10 C 0.0122(4) 0.0036(6) 0.21714(14) 0.0348(10) Uani 1 1 d . . . C11 C -0.0259(5) -0.1388(5) 0.19862(15) 0.0361(12) Uani 1 1 d . . . H11 H -0.1063 -0.1698 0.1938 0.043 Uiso 1 1 calc R . . C12 C 0.0763(5) -0.2269(5) 0.18859(16) 0.0371(12) Uani 1 1 d . . . H12 H 0.0755 -0.3247 0.1757 0.045 Uiso 1 1 calc R . . C13 C 0.1801(5) -0.1403(6) 0.20160(16) 0.0389(12) Uani 1 1 d . . . H13 H 0.2603 -0.1710 0.1989 0.047 Uiso 1 1 calc R . . C14 C 0.1416(4) -0.0004(6) 0.21922(14) 0.0375(11) Uani 1 1 d . . . H14 H 0.1922 0.0778 0.2305 0.045 Uiso 1 1 calc R . . C15 C -0.0669(5) 0.1267(6) 0.23709(16) 0.0393(12) Uani 1 1 d . . . C16 C -0.0340(7) 0.2908(7) 0.2209(2) 0.071(2) Uani 1 1 d . . . H16A H -0.0527 0.2976 0.1905 0.107 Uiso 1 1 calc R . . H16B H 0.0511 0.3093 0.2267 0.107 Uiso 1 1 calc R . . H16C H -0.0801 0.3676 0.2356 0.107 Uiso 1 1 calc R . . C17 C -0.0411(6) 0.1260(8) 0.28583(18) 0.0671(19) Uani 1 1 d . . . H17A H -0.0852 0.2090 0.2986 0.101 Uiso 1 1 calc R . . H17B H 0.0444 0.1403 0.2921 0.101 Uiso 1 1 calc R . . H17C H -0.0661 0.0281 0.2974 0.101 Uiso 1 1 calc R . . C18 C -0.2008(5) 0.0995(8) 0.2273(2) 0.0661(19) Uani 1 1 d . . . H18A H -0.2165 0.0955 0.1966 0.099 Uiso 1 1 calc R . . H18B H -0.2466 0.1831 0.2391 0.099 Uiso 1 1 calc R . . H18C H -0.2244 0.0027 0.2398 0.099 Uiso 1 1 calc R . . C19 C 0.3203(5) 0.1926(5) 0.13496(16) 0.0340(11) Uani 1 1 d . . . C20 C 0.2321(5) 0.2803(5) 0.15547(16) 0.0363(12) Uani 1 1 d . . . H20 H 0.2321 0.3013 0.1848 0.044 Uiso 1 1 calc R . . C21 C 0.1438(5) 0.3312(5) 0.12425(17) 0.0394(12) Uani 1 1 d . . . H21 H 0.0754 0.3905 0.1294 0.047 Uiso 1 1 calc R . . C22 C 0.1773(5) 0.2769(6) 0.08428(17) 0.0400(13) Uani 1 1 d . . . H22 H 0.1360 0.2955 0.0580 0.048 Uiso 1 1 calc R . . C23 C 0.2846(5) 0.1888(5) 0.09073(16) 0.0382(12) Uani 1 1 d . . . H23 H 0.3251 0.1369 0.0694 0.046 Uiso 1 1 calc R . . C24 C 0.4440(5) 0.1372(6) 0.15331(16) 0.0393(12) Uani 1 1 d . . . C25 C 0.5418(5) 0.2527(7) 0.13705(18) 0.0482(14) Uani 1 1 d . . . H25A H 0.6210 0.2203 0.1478 0.072 Uiso 1 1 calc R . . H25B H 0.5256 0.3558 0.1473 0.072 Uiso 1 1 calc R . . H25C H 0.5389 0.2528 0.1061 0.072 Uiso 1 1 calc R . . C26 C 0.4773(5) -0.0229(6) 0.13754(18) 0.0486(13) Uani 1 1 d . . . H26A H 0.5582 -0.0484 0.1481 0.073 Uiso 1 1 calc R . . H26B H 0.4736 -0.0238 0.1066 0.073 Uiso 1 1 calc R . . H26C H 0.4213 -0.0982 0.1479 0.073 Uiso 1 1 calc R . . C27 C 0.4508(5) 0.1410(6) 0.20252(16) 0.0454(13) Uani 1 1 d . . . H27A H 0.3944 0.0669 0.2133 0.068 Uiso 1 1 calc R . . H27B H 0.4305 0.2435 0.2122 0.068 Uiso 1 1 calc R . . H27C H 0.5316 0.1149 0.2130 0.068 Uiso 1 1 calc R . . C28 C 0.2657(5) -0.3174(6) 0.10530(17) 0.0406(12) Uani 1 1 d . . . H28A H 0.2432 -0.3439 0.1328 0.049 Uiso 1 1 calc R . . C29 C 0.3494(5) -0.4092(6) 0.08632(18) 0.0433(13) Uani 1 1 d . . . H29A H 0.3808 -0.4974 0.1002 0.052 Uiso 1 1 calc R . . C30 C 0.3860(5) -0.3682(6) 0.04639(19) 0.0451(14) Uani 1 1 d . . . H30A H 0.4443 -0.4275 0.0332 0.054 Uiso 1 1 calc R . . C31 C 0.3360(5) -0.2372(6) 0.02536(17) 0.0431(13) Uani 1 1 d . . . C32 C 0.2492(5) -0.1552(6) 0.04668(16) 0.0380(12) Uani 1 1 d . . . H32A H 0.2128 -0.0701 0.0328 0.046 Uiso 1 1 calc R . . C33 C 0.3766(5) -0.1862(7) -0.01802(17) 0.0553(16) Uani 1 1 d . . . H33A H 0.4625 -0.1668 -0.0162 0.083 Uiso 1 1 calc R . . H33B H 0.3345 -0.0925 -0.0267 0.083 Uiso 1 1 calc R . . H33C H 0.3587 -0.2666 -0.0388 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.03035(15) 0.03115(15) 0.02951(15) 0.00084(13) 0.00160(10) 0.00011(13) N 0.038(3) 0.031(2) 0.042(3) -0.0037(18) 0.003(2) 0.0014(18) C1 0.035(3) 0.036(3) 0.033(3) 0.000(2) -0.005(2) 0.003(2) C2 0.031(3) 0.044(3) 0.034(3) -0.005(2) 0.004(2) 0.001(2) C3 0.032(3) 0.040(3) 0.045(3) -0.006(2) -0.006(3) 0.005(2) C4 0.037(3) 0.033(3) 0.039(3) 0.004(2) -0.008(2) -0.002(2) C5 0.037(3) 0.036(3) 0.032(3) 0.000(2) 0.003(2) 0.002(2) C6 0.037(3) 0.033(3) 0.039(3) -0.003(2) 0.001(2) -0.003(2) C7 0.056(4) 0.030(3) 0.055(4) -0.004(2) 0.001(3) 0.003(2) C8 0.052(4) 0.041(3) 0.065(4) -0.006(3) -0.008(3) -0.002(3) C9 0.074(5) 0.037(3) 0.055(4) 0.003(3) 0.008(3) -0.015(3) C10 0.032(2) 0.044(3) 0.028(2) 0.001(2) 0.0023(19) -0.002(2) C11 0.037(3) 0.036(3) 0.035(3) 0.002(2) 0.003(2) -0.004(2) C12 0.045(3) 0.030(3) 0.037(3) 0.005(2) 0.000(2) 0.004(2) C13 0.037(3) 0.043(3) 0.036(3) 0.008(2) 0.001(2) 0.003(2) C14 0.038(3) 0.046(3) 0.028(2) 0.002(2) 0.002(2) -0.005(2) C15 0.039(3) 0.045(3) 0.034(3) -0.005(2) 0.007(2) -0.001(2) C16 0.087(5) 0.042(3) 0.088(5) -0.008(3) 0.042(4) 0.006(3) C17 0.069(5) 0.090(5) 0.043(4) -0.015(3) 0.003(3) 0.017(4) C18 0.033(3) 0.076(4) 0.091(5) -0.035(4) 0.016(3) -0.001(3) C19 0.032(3) 0.031(2) 0.038(3) 0.001(2) 0.000(2) 0.000(2) C20 0.040(3) 0.032(3) 0.037(3) -0.003(2) 0.004(2) 0.000(2) C21 0.031(3) 0.030(3) 0.057(4) 0.005(2) -0.001(2) 0.000(2) C22 0.037(3) 0.042(3) 0.040(3) 0.008(2) -0.007(2) -0.008(2) C23 0.042(3) 0.038(3) 0.035(3) 0.000(2) 0.007(2) -0.006(2) C24 0.043(3) 0.039(3) 0.036(3) 0.004(2) 0.000(2) -0.001(2) C25 0.039(3) 0.057(3) 0.049(3) 0.004(3) 0.002(3) -0.007(3) C26 0.043(3) 0.050(3) 0.054(3) 0.002(3) 0.001(3) 0.001(3) C27 0.032(3) 0.058(3) 0.046(3) 0.007(3) -0.004(3) -0.004(2) C28 0.036(3) 0.042(3) 0.044(3) -0.002(2) 0.006(3) -0.005(2) C29 0.042(3) 0.032(3) 0.055(4) -0.004(2) 0.000(3) 0.002(2) C30 0.032(3) 0.043(3) 0.060(4) -0.018(3) 0.005(3) 0.001(2) C31 0.040(3) 0.047(3) 0.042(3) -0.014(2) -0.003(3) -0.006(2) C32 0.037(3) 0.042(3) 0.034(3) -0.006(2) -0.002(2) -0.002(2) C33 0.037(4) 0.086(4) 0.043(3) -0.007(3) 0.008(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce N 2.673(4) . ? Ce C3 2.768(5) . ? Ce C21 2.778(5) . ? Ce C13 2.803(5) . ? Ce C12 2.808(5) . ? Ce C4 2.823(5) . ? Ce C22 2.838(5) . ? Ce C14 2.860(4) . ? Ce C11 2.874(5) . ? Ce C20 2.883(5) . ? Ce C2 2.891(5) . ? Ce C10 2.904(4) . ? Ce C5 2.923(4) . ? Ce C23 2.946(4) . ? Ce C1 2.993(5) . ? Ce C19 3.002(4) . ? N C28 1.344(6) . ? N C32 1.350(6) . ? C1 C2 1.408(7) . ? C1 C5 1.416(7) . ? C1 C6 1.534(6) . ? C2 C3 1.411(7) . ? C3 C4 1.403(7) . ? C4 C5 1.411(7) . ? C6 C9 1.522(7) . ? C6 C8 1.531(7) . ? C6 C7 1.532(7) . ? C10 C11 1.407(6) . ? C10 C14 1.425(6) . ? C10 C15 1.521(7) . ? C11 C12 1.404(7) . ? C12 C13 1.407(7) . ? C13 C14 1.395(7) . ? C15 C18 1.510(7) . ? C15 C17 1.528(7) . ? C15 C16 1.544(8) . ? C19 C20 1.406(7) . ? C19 C23 1.412(7) . ? C19 C24 1.527(7) . ? C20 C21 1.410(7) . ? C21 C22 1.394(7) . ? C22 C23 1.410(7) . ? C24 C26 1.510(7) . ? C24 C27 1.528(7) . ? C24 C25 1.566(7) . ? C28 C29 1.369(7) . ? C29 C30 1.370(8) . ? C30 C31 1.399(8) . ? C31 C32 1.383(7) . ? C31 C33 1.506(8) . ? 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 N Ce C3 123.01(14) . . ? N Ce C21 119.52(15) . . ? C3 Ce C21 82.21(15) . . ? N Ce C13 83.39(14) . . ? C3 Ce C13 137.53(16) . . ? C21 Ce C13 115.30(15) . . ? N Ce C12 82.02(14) . . ? C3 Ce C12 115.13(16) . . ? C21 Ce C12 140.47(15) . . ? C13 Ce C12 29.05(14) . . ? N Ce C4 98.88(14) . . ? C3 Ce C4 29.04(15) . . ? C21 Ce C4 79.59(14) . . ? C13 Ce C4 161.64(15) . . ? C12 Ce C4 132.89(15) . . ? N Ce C22 94.23(14) . . ? C3 Ce C22 84.47(15) . . ? C21 Ce C22 28.71(15) . . ? C13 Ce C22 129.92(15) . . ? C12 Ce C22 158.78(15) . . ? C4 Ce C22 68.29(15) . . ? N Ce C14 110.51(13) . . ? C3 Ce C14 120.62(15) . . ? C21 Ce C14 93.34(15) . . ? C13 Ce C14 28.50(14) . . ? C12 Ce C14 47.13(14) . . ? C4 Ce C14 149.18(15) . . ? C22 Ce C14 116.90(14) . . ? N Ce C11 108.37(13) . . ? C3 Ce C11 90.93(15) . . ? C21 Ce C11 126.74(15) . . ? C13 Ce C11 47.08(15) . . ? C12 Ce C11 28.57(14) . . ? C4 Ce C11 115.88(15) . . ? C22 Ce C11 155.42(14) . . ? C14 Ce C11 46.45(14) . . ? N Ce C20 111.02(14) . . ? C3 Ce C20 108.56(14) . . ? C21 Ce C20 28.77(14) . . ? C13 Ce C20 87.62(14) . . ? C12 Ce C20 115.33(14) . . ? C4 Ce C20 108.21(14) . . ? C22 Ce C20 46.66(14) . . ? C14 Ce C20 70.25(14) . . ? C11 Ce C20 113.54(14) . . ? N Ce C2 111.16(13) . . ? C3 Ce C2 28.77(14) . . ? C21 Ce C2 110.18(14) . . ? C13 Ce C2 115.20(15) . . ? C12 Ce C2 88.48(14) . . ? C4 Ce C2 46.94(14) . . ? C22 Ce C2 112.19(14) . . ? C14 Ce C2 110.78(14) . . ? C11 Ce C2 69.08(14) . . ? C20 Ce C2 133.77(14) . . ? N Ce C10 127.99(13) . . ? C3 Ce C10 93.50(15) . . ? C21 Ce C10 99.29(15) . . ? C13 Ce C10 47.42(14) . . ? C12 Ce C10 47.32(14) . . ? C4 Ce C10 122.52(14) . . ? C22 Ce C10 127.87(14) . . ? C14 Ce C10 28.61(13) . . ? C11 Ce C10 28.17(13) . . ? C20 Ce C10 86.22(14) . . ? C2 Ce C10 82.54(13) . . ? C28 N C32 116.7(4) . . ? C28 N Ce 123.4(3) . . ? C32 N Ce 118.7(3) . . ? C2 C1 C5 106.7(4) . . ? C2 C1 C6 127.1(5) . . ? C5 C1 C6 124.5(4) . . ? C2 C1 Ce 72.2(3) . . ? C5 C1 Ce 73.4(3) . . ? C6 C1 Ce 131.1(3) . . ? C1 C2 C3 108.8(4) . . ? C1 C2 Ce 80.2(3) . . ? C3 C2 Ce 70.8(3) . . ? C4 C3 C2 108.0(4) . . ? C4 C3 Ce 77.7(3) . . ? C2 C3 Ce 80.5(3) . . ? C3 C4 C5 107.6(4) . . ? C3 C4 Ce 73.3(3) . . ? C5 C4 Ce 79.7(3) . . ? C4 C5 C1 108.8(4) . . ? C4 C5 Ce 71.9(3) . . ? C1 C5 Ce 78.9(3) . . ? C9 C6 C8 107.6(5) . . ? C9 C6 C7 110.1(4) . . ? C8 C6 C7 108.6(4) . . ? C9 C6 C1 111.7(4) . . ? C8 C6 C1 107.1(4) . . ? C7 C6 C1 111.6(4) . . ? C11 C10 C14 106.0(4) . . ? C11 C10 C15 127.2(4) . . ? C14 C10 C15 126.2(4) . . ? C11 C10 Ce 74.8(3) . . ? C14 C10 Ce 74.0(3) . . ? C15 C10 Ce 123.2(3) . . ? C12 C11 C10 109.4(5) . . ? C12 C11 Ce 73.1(3) . . ? C10 C11 Ce 77.1(3) . . ? C11 C12 C13 107.6(4) . . ? C11 C12 Ce 78.3(3) . . ? C13 C12 Ce 75.2(3) . . ? C14 C13 C12 108.0(5) . . ? C14 C13 Ce 78.0(3) . . ? C12 C13 Ce 75.7(3) . . ? C13 C14 C10 109.0(4) . . ? C13 C14 Ce 73.5(3) . . ? C10 C14 Ce 77.4(3) . . ? C18 C15 C10 112.6(4) . . ? C18 C15 C17 109.5(5) . . ? C10 C15 C17 108.6(4) . . ? C18 C15 C16 108.5(5) . . ? C10 C15 C16 110.6(4) . . ? C17 C15 C16 106.9(5) . . ? C20 C19 C23 106.7(4) . . ? C20 C19 C24 128.4(4) . . ? C23 C19 C24 123.9(5) . . ? C20 C19 Ce 71.5(3) . . ? C23 C19 Ce 74.1(3) . . ? C24 C19 Ce 128.5(3) . . ? C19 C20 C21 108.8(5) . . ? C19 C20 Ce 80.9(3) . . ? C21 C20 Ce 71.5(3) . . ? C22 C21 C20 107.8(5) . . ? C22 C21 Ce 78.0(3) . . ? C20 C21 Ce 79.8(3) . . ? C21 C22 C23 108.0(4) . . ? C21 C22 Ce 73.3(3) . . ? C23 C22 Ce 80.2(3) . . ? C22 C23 C19 108.5(5) . . ? C22 C23 Ce 71.7(3) . . ? C19 C23 Ce 78.5(3) . . ? C26 C24 C19 112.9(4) . . ? C26 C24 C27 110.1(4) . . ? C19 C24 C27 111.5(4) . . ? C26 C24 C25 106.8(4) . . ? C19 C24 C25 107.4(4) . . ? C27 C24 C25 108.0(4) . . ? N C28 C29 123.8(5) . . ? C28 C29 C30 118.5(5) . . ? C29 C30 C31 120.2(5) . . ? C32 C31 C30 116.8(5) . . ? C32 C31 C33 121.6(5) . . ? C30 C31 C33 121.6(5) . . ? N C32 C31 124.0(5) . . ? #===END data_(U,Bu^t^,picoline) _database_code_depnum_ccdc_archive 'CCDC 223529' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H46 N U' _chemical_formula_weight 694.74 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' U U -9.6767 9.6646 '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 10.8282(13) _cell_length_b 10.8431(12) _cell_length_c 14.0262(11) _cell_angle_alpha 109.090(7) _cell_angle_beta 98.889(8) _cell_angle_gamma 98.832(5) _cell_volume 1500.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10168 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method ? _exptl_crystal_F_000 686 _exptl_absorpt_coefficient_mu 5.429 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.455 _exptl_absorpt_correction_T_max 0.637 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 10168 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5247 _reflns_number_gt 4432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. Some restraints on displacement parameters (ISOR) have been applied for the C atoms of the first Cp moiety and two tert-butyl groups. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. The highest residual electron density peak is located near the U atom, as a result of imperfect absorption corrections. 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^)+(0.0532P)^2^+0.4427P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5247 _refine_ls_number_parameters 325 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 1.287 _refine_diff_density_min -1.323 _refine_diff_density_rms 0.128 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 U U 0.78382(3) 0.99487(3) 0.72034(2) 0.03114(12) Uani 1 1 d . . . N N 0.9876(8) 0.8848(7) 0.7191(6) 0.0510(19) Uani 1 1 d . . . C1 C 0.6426(9) 0.7177(8) 0.6543(7) 0.050(2) Uani 1 1 d . . . C2 C 0.5552(9) 0.7994(9) 0.6784(7) 0.050(2) Uani 1 1 d . . . H2 H 0.5143 0.8088 0.7331 0.060 Uiso 1 1 calc R . . C3 C 0.5382(10) 0.8658(10) 0.6070(9) 0.066(3) Uani 1 1 d U . . H3 H 0.4855 0.9259 0.6066 0.079 Uiso 1 1 calc R . . C4 C 0.6124(13) 0.8254(11) 0.5407(9) 0.075(3) Uani 1 1 d U . . H4 H 0.6176 0.8526 0.4848 0.091 Uiso 1 1 calc R . . C5 C 0.6824(11) 0.7356(10) 0.5660(9) 0.071(3) Uani 1 1 d U . . H5 H 0.7418 0.6965 0.5323 0.085 Uiso 1 1 calc R . . C6 C 0.6658(11) 0.6119(9) 0.6987(10) 0.068(3) Uani 1 1 d U . . C7 C 0.8071(19) 0.608(2) 0.7269(15) 0.139(6) Uani 1 1 d U . . H7A H 0.8187 0.5669 0.7778 0.208 Uiso 1 1 calc R . . H7B H 0.8582 0.6976 0.7545 0.208 Uiso 1 1 calc R . . H7C H 0.8330 0.5574 0.6662 0.208 Uiso 1 1 calc R . . C8 C 0.5876(13) 0.4812(12) 0.6347(10) 0.082(3) Uani 1 1 d U . . H8A H 0.4991 0.4817 0.6351 0.123 Uiso 1 1 calc R . . H8B H 0.6123 0.4155 0.6615 0.123 Uiso 1 1 calc R . . H8C H 0.5996 0.4597 0.5652 0.123 Uiso 1 1 calc R . . C9 C 0.6392(18) 0.6452(18) 0.8079(14) 0.125(6) Uani 1 1 d U . . H9A H 0.5519 0.6535 0.8056 0.187 Uiso 1 1 calc R . . H9B H 0.6955 0.7279 0.8534 0.187 Uiso 1 1 calc R . . H9C H 0.6535 0.5749 0.8328 0.187 Uiso 1 1 calc R . . C10 C 0.6840(8) 1.1271(8) 0.8981(6) 0.0395(18) Uani 1 1 d . . . C11 C 0.6962(8) 1.0029(8) 0.9044(6) 0.0400(19) Uani 1 1 d . . . H11 H 0.6292 0.9337 0.8980 0.048 Uiso 1 1 calc R . . C12 C 0.8295(8) 1.0011(8) 0.9224(6) 0.0391(18) Uani 1 1 d . . . H12 H 0.8646 0.9300 0.9281 0.047 Uiso 1 1 calc R . . C13 C 0.8966(8) 1.1238(8) 0.9298(6) 0.0375(18) Uani 1 1 d . . . H13 H 0.9852 1.1512 0.9435 0.045 Uiso 1 1 calc R . . C14 C 0.8078(7) 1.2004(8) 0.9131(6) 0.0372(18) Uani 1 1 d . . . H14 H 0.8283 1.2864 0.9122 0.045 Uiso 1 1 calc R . . C15 C 0.5622(9) 1.1798(8) 0.8931(9) 0.055(3) Uani 1 1 d . . . C16 C 0.5542(12) 1.2534(13) 0.8182(11) 0.080(3) Uani 1 1 d U . . H16A H 0.6296 1.3233 0.8376 0.121 Uiso 1 1 calc R . . H16B H 0.4799 1.2915 0.8200 0.121 Uiso 1 1 calc R . . H16C H 0.5481 1.1920 0.7496 0.121 Uiso 1 1 calc R . . C17 C 0.5682(12) 1.2780(12) 1.0049(10) 0.086(4) Uani 1 1 d U . . H17A H 0.6266 1.3610 1.0184 0.129 Uiso 1 1 calc R . . H17B H 0.5973 1.2390 1.0543 0.129 Uiso 1 1 calc R . . H17C H 0.4845 1.2942 1.0107 0.129 Uiso 1 1 calc R . . C18 C 0.4427(10) 1.0698(11) 0.8672(10) 0.067(3) Uani 1 1 d . . . H18A H 0.3689 1.1087 0.8720 0.100 Uiso 1 1 calc R . . H18B H 0.4514 1.0238 0.9150 0.100 Uiso 1 1 calc R . . H18C H 0.4324 1.0075 0.7981 0.100 Uiso 1 1 calc R . . C19 C 0.9585(7) 1.2207(7) 0.7036(6) 0.0330(16) Uani 1 1 d . . . C20 C 0.8337(8) 1.2475(7) 0.6972(6) 0.0370(18) Uani 1 1 d . . . H20 H 0.8100 1.3168 0.7451 0.044 Uiso 1 1 calc R . . C21 C 0.7516(8) 1.1519(8) 0.6060(6) 0.0369(17) Uani 1 1 d . . . H21 H 0.6645 1.1458 0.5844 0.044 Uiso 1 1 calc R . . C22 C 0.8261(9) 1.0671(8) 0.5538(6) 0.043(2) Uani 1 1 d . . . H22 H 0.7971 0.9971 0.4904 0.052 Uiso 1 1 calc R . . C23 C 0.9508(8) 1.1069(8) 0.6140(7) 0.0403(19) Uani 1 1 d . . . H23 H 1.0181 1.0656 0.5982 0.048 Uiso 1 1 calc R . . C24 C 1.0828(8) 1.3132(8) 0.7728(6) 0.0410(19) Uani 1 1 d . . . C25 C 1.1455(10) 1.3889(9) 0.7105(8) 0.057(2) Uani 1 1 d . . . H25A H 1.1559 1.3258 0.6475 0.086 Uiso 1 1 calc R . . H25B H 1.2277 1.4427 0.7507 0.086 Uiso 1 1 calc R . . H25C H 1.0918 1.4454 0.6946 0.086 Uiso 1 1 calc R . . C26 C 1.1762(9) 1.2331(9) 0.8045(8) 0.053(2) Uani 1 1 d . . . H26A H 1.1378 1.1821 0.8410 0.080 Uiso 1 1 calc R . . H26B H 1.2538 1.2935 0.8485 0.080 Uiso 1 1 calc R . . H26C H 1.1954 1.1737 0.7437 0.080 Uiso 1 1 calc R . . C27 C 1.0628(9) 1.4152(8) 0.8712(7) 0.050(2) Uani 1 1 d . . . H27A H 1.0238 1.3691 0.9105 0.076 Uiso 1 1 calc R . . H27B H 1.0081 1.4695 0.8528 0.076 Uiso 1 1 calc R . . H27C H 1.1441 1.4711 0.9118 0.076 Uiso 1 1 calc R . . C28 C 1.0627(9) 0.8894(10) 0.8073(9) 0.059(3) Uani 1 1 d . . . H28 H 1.0456 0.9420 0.8689 0.071 Uiso 1 1 calc R . . C29 C 1.1624(9) 0.8244(10) 0.8162(9) 0.059(3) Uani 1 1 d . . . H29 H 1.2107 0.8324 0.8796 0.070 Uiso 1 1 calc R . . C30 C 1.1824(10) 0.7520(10) 0.7290(8) 0.057(3) Uani 1 1 d . . . H30 H 1.2449 0.7025 0.7320 0.068 Uiso 1 1 calc R . . C31 C 1.1213(10) 0.7405(8) 0.6328(7) 0.051(2) Uani 1 1 d . . . C32 C 1.0159(10) 0.8144(9) 0.6306(8) 0.057(3) Uani 1 1 d . . . H32 H 0.9700 0.8114 0.5678 0.069 Uiso 1 1 calc R . . C33 C 1.1422(13) 0.6588(11) 0.5313(9) 0.075(3) Uani 1 1 d . . . H33A H 1.2310 0.6812 0.5298 0.113 Uiso 1 1 calc R . . H33B H 1.0908 0.6765 0.4772 0.113 Uiso 1 1 calc R . . H33C H 1.1184 0.5656 0.5212 0.113 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.03426(17) 0.02938(16) 0.02913(19) 0.01223(12) 0.00307(11) 0.00515(10) N 0.061(5) 0.047(4) 0.062(5) 0.028(4) 0.030(4) 0.027(4) C1 0.054(6) 0.035(4) 0.049(6) 0.008(4) 0.007(4) -0.001(4) C2 0.041(5) 0.048(5) 0.050(6) 0.019(4) -0.012(4) -0.007(4) C3 0.049(5) 0.055(5) 0.084(7) 0.033(5) -0.016(5) -0.003(4) C4 0.091(7) 0.059(5) 0.059(6) 0.025(5) -0.003(5) -0.020(5) C5 0.073(6) 0.055(5) 0.058(6) -0.007(4) 0.022(5) -0.011(5) C6 0.068(6) 0.036(4) 0.101(7) 0.029(5) 0.020(5) 0.006(4) C7 0.139(6) 0.139(6) 0.139(6) 0.050(3) 0.0298(17) 0.0304(17) C8 0.082(4) 0.081(4) 0.082(4) 0.0295(16) 0.0173(13) 0.0175(13) C9 0.125(6) 0.124(6) 0.124(6) 0.045(2) 0.0268(16) 0.0274(16) C10 0.037(4) 0.042(4) 0.032(5) 0.007(3) 0.006(3) 0.002(3) C11 0.034(4) 0.037(4) 0.044(5) 0.012(4) 0.007(4) 0.001(3) C12 0.042(5) 0.050(5) 0.034(5) 0.022(4) 0.010(3) 0.015(4) C13 0.036(4) 0.045(4) 0.031(5) 0.013(3) 0.009(3) 0.008(3) C14 0.032(4) 0.037(4) 0.036(5) 0.004(3) 0.011(3) 0.004(3) C15 0.043(5) 0.039(4) 0.091(8) 0.025(5) 0.032(5) 0.017(4) C16 0.069(6) 0.095(7) 0.111(8) 0.066(6) 0.039(6) 0.032(5) C17 0.071(6) 0.078(6) 0.098(8) 0.009(5) 0.034(6) 0.019(5) C18 0.048(6) 0.076(7) 0.095(9) 0.050(6) 0.022(6) 0.021(5) C19 0.036(4) 0.029(4) 0.035(4) 0.012(3) 0.009(3) 0.006(3) C20 0.051(5) 0.027(4) 0.039(5) 0.018(3) 0.008(4) 0.011(3) C21 0.032(4) 0.043(4) 0.039(5) 0.022(4) 0.006(3) 0.006(3) C22 0.060(6) 0.041(4) 0.022(4) 0.009(3) 0.010(4) 0.000(4) C23 0.044(5) 0.034(4) 0.049(5) 0.020(4) 0.017(4) 0.007(3) C24 0.038(5) 0.043(4) 0.040(5) 0.014(4) 0.010(4) 0.002(3) C25 0.056(6) 0.051(5) 0.063(7) 0.021(5) 0.019(5) -0.004(4) C26 0.038(5) 0.058(5) 0.070(7) 0.031(5) 0.011(4) 0.012(4) C27 0.043(5) 0.042(5) 0.051(6) 0.006(4) 0.001(4) -0.002(4) C28 0.045(5) 0.062(6) 0.091(8) 0.050(6) 0.020(5) 0.015(5) C29 0.039(5) 0.060(6) 0.079(8) 0.031(6) 0.014(5) 0.005(4) C30 0.061(6) 0.050(5) 0.054(7) 0.024(5) 0.003(5) -0.005(4) C31 0.078(7) 0.029(4) 0.044(6) 0.003(4) 0.038(5) 0.001(4) C32 0.068(7) 0.040(5) 0.064(7) 0.009(4) 0.037(5) 0.011(4) C33 0.114(10) 0.067(7) 0.061(8) 0.033(6) 0.038(7) 0.030(7) _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 U N 2.665(7) . ? U C21 2.718(7) . ? U C4 2.766(11) . ? U C3 2.766(10) . ? U C22 2.774(8) . ? U C12 2.778(8) . ? U C13 2.785(8) . ? U C14 2.830(8) . ? U C20 2.844(7) . ? U C2 2.844(8) . ? U C5 2.851(10) . ? U C11 2.866(8) . ? U C23 2.883(7) . ? U C10 2.900(8) . ? U C1 2.925(11) . ? U C19 2.953(10) . ? N C32 1.336(11) . ? N C28 1.353(13) . ? C1 C2 1.398(14) . ? C1 C5 1.433(14) . ? C1 C6 1.508(14) . ? C2 C3 1.418(13) . ? C3 C4 1.332(17) . ? C4 C5 1.422(17) . ? C6 C8 1.447(15) . ? C6 C7 1.53(2) . ? C6 C9 1.54(2) . ? C10 C14 1.396(11) . ? C10 C11 1.404(11) . ? C10 C15 1.516(12) . ? C11 C12 1.431(12) . ? C12 C13 1.378(11) . ? C13 C14 1.404(12) . ? C15 C16 1.513(15) . ? C15 C18 1.526(13) . ? C15 C17 1.566(15) . ? C19 C20 1.420(11) . ? C19 C23 1.425(11) . ? C19 C24 1.518(11) . ? C20 C21 1.414(11) . ? C21 C22 1.415(12) . ? C22 C23 1.398(12) . ? C24 C27 1.530(12) . ? C24 C26 1.535(12) . ? C24 C25 1.543(12) . ? C28 C29 1.388(13) . ? C29 C30 1.290(14) . ? C30 C31 1.366(14) . ? C31 C33 1.484(13) . ? C31 C32 1.493(14) . ? 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 N U C21 118.8(2) . . ? N U C4 103.5(4) . . ? C21 U C4 76.2(3) . . ? N U C3 125.5(3) . . ? C21 U C3 81.4(3) . . ? C4 U C3 27.9(4) . . ? N U C22 91.4(3) . . ? C21 U C22 29.8(3) . . ? C4 U C22 69.4(3) . . ? C3 U C22 87.7(3) . . ? N U C12 80.9(2) . . ? C21 U C12 142.6(2) . . ? C4 U C12 133.2(3) . . ? C3 U C12 114.3(3) . . ? C22 U C12 157.2(3) . . ? N U C13 83.2(2) . . ? C21 U C13 117.0(2) . . ? C4 U C13 160.5(3) . . ? C3 U C13 135.1(3) . . ? C22 U C13 129.4(2) . . ? C12 U C13 28.7(2) . . ? N U C14 110.9(2) . . ? C21 U C14 95.3(2) . . ? C4 U C14 144.1(4) . . ? C3 U C14 117.1(3) . . ? C22 U C14 118.3(2) . . ? C12 U C14 47.4(2) . . ? C13 U C14 28.9(2) . . ? N U C20 112.5(2) . . ? C21 U C20 29.3(2) . . ? C4 U C20 105.5(3) . . ? C3 U C20 106.6(3) . . ? C22 U C20 47.9(2) . . ? C12 U C20 115.7(2) . . ? C13 U C20 88.3(2) . . ? C14 U C20 70.6(2) . . ? N U C2 110.9(3) . . ? C21 U C2 110.4(2) . . ? C4 U C2 46.3(3) . . ? C3 U C2 29.2(3) . . ? C22 U C2 114.7(3) . . ? C12 U C2 88.1(3) . . ? C13 U C2 114.2(3) . . ? C14 U C2 109.3(3) . . ? C20 U C2 132.9(3) . . ? N U C5 77.9(3) . . ? C21 U C5 100.8(3) . . ? C4 U C5 29.3(4) . . ? C3 U C5 47.8(4) . . ? C22 U C5 83.9(3) . . ? C12 U C5 115.0(3) . . ? C13 U C5 142.1(3) . . ? C14 U C5 154.9(3) . . ? C20 U C5 129.3(3) . . ? C2 U C5 46.8(3) . . ? N U C11 107.7(2) . . ? C21 U C11 129.0(2) . . ? C4 U C11 113.4(3) . . ? C3 U C11 88.7(3) . . ? C22 U C11 158.8(3) . . ? C12 U C11 29.3(2) . . ? C13 U C11 47.3(2) . . ? C14 U C11 46.5(2) . . ? C20 U C11 113.8(2) . . ? C2 U C11 67.8(3) . . ? C5 U C11 108.8(3) . . ? C32 N C28 116.4(9) . . ? C32 N U 121.5(7) . . ? C28 N U 121.9(6) . . ? C2 C1 C5 105.9(9) . . ? C2 C1 C6 125.4(9) . . ? C5 C1 C6 127.5(10) . . ? C2 C1 U 72.8(5) . . ? C5 C1 U 72.8(5) . . ? C6 C1 U 129.1(7) . . ? C1 C2 C3 110.0(10) . . ? C1 C2 U 79.2(5) . . ? C3 C2 U 72.4(5) . . ? C4 C3 C2 106.6(10) . . ? C4 C3 U 76.1(7) . . ? C2 C3 U 78.4(5) . . ? C3 C4 C5 111.5(10) . . ? C3 C4 U 76.1(6) . . ? C5 C4 U 78.7(6) . . ? C4 C5 C1 105.9(10) . . ? C4 C5 U 72.0(6) . . ? C1 C5 U 78.5(5) . . ? C8 C6 C1 112.3(10) . . ? C8 C6 C7 112.0(11) . . ? C1 C6 C7 114.1(11) . . ? C8 C6 C9 107.8(11) . . ? C1 C6 C9 112.1(10) . . ? C7 C6 C9 97.5(12) . . ? C14 C10 C11 106.8(7) . . ? C14 C10 C15 126.2(7) . . ? C11 C10 C15 126.4(7) . . ? C14 C10 U 73.1(4) . . ? C11 C10 U 74.5(5) . . ? C15 C10 U 124.9(6) . . ? C10 C11 C12 108.1(7) . . ? C10 C11 U 77.3(5) . . ? C12 C11 U 71.9(4) . . ? C13 C12 C11 107.5(7) . . ? C13 C12 U 76.0(4) . . ? C11 C12 U 78.7(5) . . ? C12 C13 C14 108.2(7) . . ? C12 C13 U 75.4(5) . . ? C14 C13 U 77.3(5) . . ? C10 C14 C13 109.3(7) . . ? C10 C14 U 78.7(5) . . ? C13 C14 U 73.8(4) . . ? C16 C15 C10 110.7(8) . . ? C16 C15 C18 111.5(10) . . ? C10 C15 C18 112.3(7) . . ? C16 C15 C17 110.0(9) . . ? C10 C15 C17 106.5(9) . . ? C18 C15 C17 105.7(8) . . ? C20 C19 C23 106.2(7) . . ? C20 C19 C24 127.3(7) . . ? C23 C19 C24 124.5(7) . . ? C20 C19 U 71.6(4) . . ? C23 C19 U 73.1(4) . . ? C24 C19 U 132.7(5) . . ? C21 C20 C19 109.0(7) . . ? C21 C20 U 70.4(4) . . ? C19 C20 U 80.1(4) . . ? C20 C21 C22 107.5(7) . . ? C20 C21 U 80.3(4) . . ? C22 C21 U 77.3(4) . . ? C23 C22 C21 108.2(7) . . ? C23 C22 U 80.1(5) . . ? C21 C22 U 72.9(4) . . ? C22 C23 C19 109.1(8) . . ? C22 C23 U 71.4(4) . . ? C19 C23 U 78.6(4) . . ? C19 C24 C27 112.9(7) . . ? C19 C24 C26 110.9(7) . . ? C27 C24 C26 108.3(7) . . ? C19 C24 C25 107.9(7) . . ? C27 C24 C25 108.8(7) . . ? C26 C24 C25 107.9(7) . . ? N C28 C29 127.3(11) . . ? C30 C29 C28 114.4(11) . . ? C29 C30 C31 126.7(11) . . ? C30 C31 C33 128.0(10) . . ? C30 C31 C32 115.2(8) . . ? C33 C31 C32 116.7(10) . . ? N C32 C31 119.9(10) . . ? #===END data_(Ce,SiMe~3~,picoline) _database_code_depnum_ccdc_archive 'CCDC 223530' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H46 Ce N Si3' _chemical_formula_weight 645.07 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' Si Si 0.0817 0.0704 '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 14.0043(6) _cell_length_b 14.8904(8) _cell_length_c 17.0833(9) _cell_angle_alpha 91.825(2) _cell_angle_beta 95.510(3) _cell_angle_gamma 112.849(3) _cell_volume 3258.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22578 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent dark yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method ? _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.525 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 22578 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.68 _reflns_number_total 11427 _reflns_number_gt 8994 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters with restraints on displacement parameters for two terminal C atoms of a Me~3~Si group. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. The highest residual electron density peak is located near the Ce atom, as a result of imperfect absorption corrections. 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^)+(0.0282P)^2^+5.1073P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11427 _refine_ls_number_parameters 651 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 1.017 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.105 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 0.292565(17) 0.350283(17) 0.158898(13) 0.01527(7) Uani 1 1 d . . . Si1A Si 0.21872(10) 0.03843(9) 0.14023(8) 0.0246(3) Uani 1 1 d . . . Si2A Si 0.14461(10) 0.37709(10) -0.05706(7) 0.0241(3) Uani 1 1 d . . . Si3A Si 0.26180(11) 0.60027(11) 0.27105(9) 0.0373(4) Uani 1 1 d . . . N1A N 0.2860(3) 0.3098(3) 0.3113(2) 0.0222(8) Uani 1 1 d . . . C1A C 0.3111(3) 0.1651(3) 0.1280(2) 0.0175(9) Uani 1 1 d . . . C2A C 0.3313(3) 0.2146(3) 0.0579(3) 0.0238(10) Uani 1 1 d . . . H2A H 0.2887 0.1953 0.0101 0.029 Uiso 1 1 calc R . . C3A C 0.4253(3) 0.2971(3) 0.0719(3) 0.0257(10) Uani 1 1 d . . . H3A H 0.4551 0.3416 0.0354 0.031 Uiso 1 1 calc R . . C4A C 0.4666(3) 0.3006(3) 0.1507(3) 0.0243(10) Uani 1 1 d . . . H4A H 0.5290 0.3473 0.1754 0.029 Uiso 1 1 calc R . . C5A C 0.3969(3) 0.2209(3) 0.1853(3) 0.0210(9) Uani 1 1 d . . . H5A H 0.4053 0.2066 0.2375 0.025 Uiso 1 1 calc R . . C6A C 0.1615(6) 0.0307(5) 0.2362(4) 0.0631(19) Uani 1 1 d . . . H6A1 H 0.1220 0.0709 0.2365 0.095 Uiso 1 1 calc R . . H6A2 H 0.2167 0.0531 0.2791 0.095 Uiso 1 1 calc R . . H6A3 H 0.1165 -0.0359 0.2419 0.095 Uiso 1 1 calc R . . C7A C 0.1134(5) -0.0096(4) 0.0574(4) 0.062(2) Uani 1 1 d . . . H7A1 H 0.0661 0.0225 0.0604 0.093 Uiso 1 1 calc R . . H7A2 H 0.0763 -0.0787 0.0602 0.093 Uiso 1 1 calc R . . H7A3 H 0.1429 0.0022 0.0084 0.093 Uiso 1 1 calc R . . C8A C 0.2930(4) -0.0417(4) 0.1476(4) 0.0503(16) Uani 1 1 d . . . H8A1 H 0.2466 -0.1070 0.1558 0.076 Uiso 1 1 calc R . . H8A2 H 0.3471 -0.0173 0.1912 0.076 Uiso 1 1 calc R . . H8A3 H 0.3235 -0.0422 0.0997 0.076 Uiso 1 1 calc R . . C9A C 0.1248(3) 0.3298(3) 0.0424(2) 0.0179(9) Uani 1 1 d . . . C10A C 0.1029(3) 0.2334(3) 0.0645(3) 0.0200(9) Uani 1 1 d . . . H10A H 0.1055 0.1828 0.0326 0.024 Uiso 1 1 calc R . . C11A C 0.0768(3) 0.2264(3) 0.1420(3) 0.0229(10) Uani 1 1 d . . . H11A H 0.0599 0.1710 0.1702 0.028 Uiso 1 1 calc R . . C12A C 0.0807(3) 0.3186(3) 0.1696(3) 0.0209(9) Uani 1 1 d . . . H12A H 0.0670 0.3345 0.2192 0.025 Uiso 1 1 calc R . . C13A C 0.1087(3) 0.3812(3) 0.1091(2) 0.0173(9) Uani 1 1 d . . . H13A H 0.1157 0.4460 0.1116 0.021 Uiso 1 1 calc R . . C14A C 0.2832(4) 0.4214(4) -0.0786(3) 0.0310(11) Uani 1 1 d . . . H14A H 0.3093 0.3714 -0.0692 0.046 Uiso 1 1 calc R . . H14B H 0.3247 0.4789 -0.0449 0.046 Uiso 1 1 calc R . . H14C H 0.2867 0.4366 -0.1327 0.046 Uiso 1 1 calc R . . C15A C 0.1021(5) 0.4814(5) -0.0594(3) 0.0477(16) Uani 1 1 d . . . H15A H 0.1138 0.5102 -0.1090 0.071 Uiso 1 1 calc R . . H15B H 0.1416 0.5296 -0.0172 0.071 Uiso 1 1 calc R . . H15C H 0.0292 0.4582 -0.0533 0.071 Uiso 1 1 calc R . . C16A C 0.0628(4) 0.2770(4) -0.1330(3) 0.0454(14) Uani 1 1 d . . . H16A H 0.0831 0.2226 -0.1283 0.068 Uiso 1 1 calc R . . H16B H 0.0725 0.3002 -0.1846 0.068 Uiso 1 1 calc R . . H16C H -0.0094 0.2566 -0.1251 0.068 Uiso 1 1 calc R . . C17A C 0.3372(3) 0.5474(3) 0.2139(3) 0.0233(10) Uani 1 1 d . . . C18A C 0.3482(4) 0.5492(3) 0.1325(3) 0.0286(11) Uani 1 1 d . . . H18A H 0.3043 0.5617 0.0940 0.034 Uiso 1 1 calc R . . C19A C 0.4356(4) 0.5291(3) 0.1190(3) 0.0333(12) Uani 1 1 d . . . H19A H 0.4584 0.5246 0.0702 0.040 Uiso 1 1 calc R . . C20A C 0.4823(3) 0.5172(3) 0.1922(3) 0.0297(11) Uani 1 1 d . . . H20A H 0.5422 0.5043 0.2009 0.036 Uiso 1 1 calc R . . C21A C 0.4222(3) 0.5282(3) 0.2496(3) 0.0257(10) Uani 1 1 d . . . H21A H 0.4360 0.5237 0.3033 0.031 Uiso 1 1 calc R . . C22A C 0.3542(4) 0.7172(4) 0.3195(4) 0.0496(15) Uani 1 1 d . . . H22A H 0.3831 0.7616 0.2803 0.074 Uiso 1 1 calc R . . H22B H 0.4092 0.7072 0.3511 0.074 Uiso 1 1 calc R . . H22C H 0.3187 0.7442 0.3525 0.074 Uiso 1 1 calc R . . C23A C 0.2086(7) 0.5219(6) 0.3571(5) 0.103(3) Uani 1 1 d U . . H23A H 0.1813 0.5560 0.3913 0.154 Uiso 1 1 calc R . . H23B H 0.2640 0.5098 0.3863 0.154 Uiso 1 1 calc R . . H23C H 0.1542 0.4608 0.3366 0.154 Uiso 1 1 calc R . . C24A C 0.1529(7) 0.6134(8) 0.2137(6) 0.124(4) Uani 1 1 d U . . H24A H 0.1199 0.6429 0.2469 0.186 Uiso 1 1 calc R . . H24B H 0.1035 0.5502 0.1923 0.186 Uiso 1 1 calc R . . H24C H 0.1777 0.6540 0.1714 0.186 Uiso 1 1 calc R . . C25A C 0.1960(3) 0.2735(3) 0.3425(3) 0.0208(9) Uani 1 1 d . . . H25A H 0.1341 0.2553 0.3090 0.025 Uiso 1 1 calc R . . C26A C 0.1904(3) 0.2616(3) 0.4218(3) 0.0243(10) Uani 1 1 d . . . H26A H 0.1260 0.2361 0.4411 0.029 Uiso 1 1 calc R . . C27A C 0.2818(3) 0.2881(3) 0.4722(3) 0.0233(10) Uani 1 1 d . . . H27A H 0.2797 0.2812 0.5260 0.028 Uiso 1 1 calc R . . C28A C 0.3769(3) 0.3252(3) 0.4416(2) 0.0206(9) Uani 1 1 d . . . C29A C 0.3741(3) 0.3337(3) 0.3614(3) 0.0230(10) Uani 1 1 d . . . H29A H 0.4373 0.3575 0.3404 0.028 Uiso 1 1 calc R . . C30A C 0.4785(4) 0.3554(4) 0.4948(3) 0.0350(12) Uani 1 1 d . . . H30A H 0.5351 0.3703 0.4633 0.052 Uiso 1 1 calc R . . H30B H 0.4765 0.3030 0.5268 0.052 Uiso 1 1 calc R . . H30C H 0.4885 0.4122 0.5282 0.052 Uiso 1 1 calc R . . Ce2 Ce 0.717487(17) 0.134958(16) 0.359787(13) 0.01440(7) Uani 1 1 d . . . Si1B Si 0.66983(11) -0.12339(10) 0.21647(8) 0.0324(3) Uani 1 1 d . . . Si2B Si 0.91325(10) 0.12574(9) 0.55676(7) 0.0213(3) Uani 1 1 d . . . Si3B Si 0.78217(9) 0.44551(9) 0.35523(7) 0.0203(3) Uani 1 1 d . . . N1B N 0.6933(3) 0.1562(3) 0.2031(2) 0.0206(8) Uani 1 1 d . . . C1B C 0.6388(3) -0.0676(3) 0.3046(3) 0.0245(10) Uani 1 1 d . . . C2B C 0.6828(4) -0.0638(3) 0.3830(3) 0.0254(10) Uani 1 1 d . . . H2B H 0.7416 -0.0765 0.3981 0.031 Uiso 1 1 calc R . . C3B C 0.6240(3) -0.0380(3) 0.4349(3) 0.0239(10) Uani 1 1 d . . . H3B H 0.6386 -0.0286 0.4896 0.029 Uiso 1 1 calc R . . C4B C 0.5396(3) -0.0289(3) 0.3898(3) 0.0272(11) Uani 1 1 d . . . H4B H 0.4869 -0.0145 0.4091 0.033 Uiso 1 1 calc R . . C5B C 0.5492(3) -0.0455(3) 0.3104(3) 0.0249(10) Uani 1 1 d . . . H5B H 0.5040 -0.0426 0.2679 0.030 Uiso 1 1 calc R . . C6B C 0.5625(5) -0.1468(6) 0.1346(4) 0.066(2) Uani 1 1 d . . . H6B1 H 0.4966 -0.1834 0.1529 0.099 Uiso 1 1 calc R . . H6B2 H 0.5724 -0.1834 0.0912 0.099 Uiso 1 1 calc R . . H6B3 H 0.5632 -0.0856 0.1178 0.099 Uiso 1 1 calc R . . C7B C 0.7979(4) -0.0495(4) 0.1815(3) 0.0458(14) Uani 1 1 d . . . H7B1 H 0.7971 0.0112 0.1647 0.069 Uiso 1 1 calc R . . H7B2 H 0.8093 -0.0852 0.1380 0.069 Uiso 1 1 calc R . . H7B3 H 0.8530 -0.0365 0.2237 0.069 Uiso 1 1 calc R . . C8B C 0.6772(5) -0.2408(4) 0.2444(4) 0.0517(16) Uani 1 1 d . . . H8B1 H 0.7328 -0.2278 0.2863 0.077 Uiso 1 1 calc R . . H8B2 H 0.6902 -0.2730 0.1996 0.077 Uiso 1 1 calc R . . H8B3 H 0.6123 -0.2821 0.2619 0.077 Uiso 1 1 calc R . . C9B C 0.9080(3) 0.1623(3) 0.4540(2) 0.0193(9) Uani 1 1 d . . . C10B C 0.9111(3) 0.1104(3) 0.3835(2) 0.0188(9) Uani 1 1 d . . . H10B H 0.9068 0.0465 0.3798 0.023 Uiso 1 1 calc R . . C11B C 0.9214(3) 0.1702(3) 0.3205(2) 0.0201(9) Uani 1 1 d . . . H11B H 0.9243 0.1526 0.2683 0.024 Uiso 1 1 calc R . . C12B C 0.9266(3) 0.2616(3) 0.3501(3) 0.0200(9) Uani 1 1 d . . . H12B H 0.9332 0.3150 0.3210 0.024 Uiso 1 1 calc R . . C13B C 0.9199(3) 0.2576(3) 0.4310(3) 0.0196(9) Uani 1 1 d . . . H13B H 0.9228 0.3089 0.4650 0.024 Uiso 1 1 calc R . . C14B C 1.0485(4) 0.1866(4) 0.6071(3) 0.0318(11) Uani 1 1 d . . . H14D H 1.0934 0.1621 0.5828 0.048 Uiso 1 1 calc R . . H14E H 1.0493 0.1734 0.6618 0.048 Uiso 1 1 calc R . . H14F H 1.0727 0.2559 0.6029 0.048 Uiso 1 1 calc R . . C15B C 0.8271(4) 0.1664(4) 0.6131(3) 0.0355(12) Uani 1 1 d . . . H15D H 0.8480 0.2357 0.6114 0.053 Uiso 1 1 calc R . . H15E H 0.8331 0.1506 0.6669 0.053 Uiso 1 1 calc R . . H15F H 0.7560 0.1337 0.5898 0.053 Uiso 1 1 calc R . . C16B C 0.8751(4) -0.0097(3) 0.5559(3) 0.0287(11) Uani 1 1 d . . . H16D H 0.8007 -0.0424 0.5440 0.043 Uiso 1 1 calc R . . H16E H 0.8964 -0.0259 0.6068 0.043 Uiso 1 1 calc R . . H16F H 0.9085 -0.0301 0.5166 0.043 Uiso 1 1 calc R . . C17B C 0.7016(3) 0.3216(3) 0.3836(2) 0.0163(9) Uani 1 1 d . . . C18B C 0.6980(3) 0.2821(3) 0.4584(2) 0.0196(9) Uani 1 1 d . . . H18B H 0.7495 0.3072 0.5011 0.024 Uiso 1 1 calc R . . C19B C 0.6049(3) 0.1996(3) 0.4577(3) 0.0201(9) Uani 1 1 d . . . H19B H 0.5846 0.1602 0.4993 0.024 Uiso 1 1 calc R . . C20B C 0.5478(3) 0.1869(3) 0.3833(3) 0.0230(10) Uani 1 1 d . . . H20B H 0.4823 0.1384 0.3669 0.028 Uiso 1 1 calc R . . C21B C 0.6074(3) 0.2606(3) 0.3381(2) 0.0166(9) Uani 1 1 d . . . H21B H 0.5879 0.2682 0.2859 0.020 Uiso 1 1 calc R . . C22B C 0.8042(4) 0.4406(4) 0.2493(3) 0.0335(12) Uani 1 1 d . . . H22D H 0.8379 0.5059 0.2337 0.050 Uiso 1 1 calc R . . H22E H 0.7384 0.4083 0.2173 0.050 Uiso 1 1 calc R . . H22F H 0.8476 0.4052 0.2424 0.050 Uiso 1 1 calc R . . C23B C 0.9103(4) 0.5039(4) 0.4176(3) 0.0346(12) Uani 1 1 d . . . H23D H 0.8991 0.5057 0.4721 0.052 Uiso 1 1 calc R . . H23E H 0.9460 0.5693 0.4030 0.052 Uiso 1 1 calc R . . H23F H 0.9519 0.4668 0.4098 0.052 Uiso 1 1 calc R . . C24B C 0.7076(4) 0.5250(3) 0.3675(3) 0.0365(12) Uani 1 1 d . . . H24D H 0.6982 0.5313 0.4220 0.055 Uiso 1 1 calc R . . H24E H 0.6407 0.4960 0.3365 0.055 Uiso 1 1 calc R . . H24F H 0.7458 0.5885 0.3502 0.055 Uiso 1 1 calc R . . C25B C 0.5942(3) 0.1307(3) 0.1701(3) 0.0232(10) Uani 1 1 d . . . H25B H 0.5407 0.1045 0.2015 0.028 Uiso 1 1 calc R . . C26B C 0.5682(4) 0.1413(4) 0.0922(3) 0.0270(10) Uani 1 1 d . . . H26B H 0.4989 0.1241 0.0718 0.032 Uiso 1 1 calc R . . C27B C 0.6471(4) 0.1781(3) 0.0451(3) 0.0262(10) Uani 1 1 d . . . H27B H 0.6311 0.1846 -0.0080 0.031 Uiso 1 1 calc R . . C28B C 0.7501(3) 0.2055(3) 0.0763(2) 0.0202(9) Uani 1 1 d . . . C29B C 0.7679(3) 0.1932(3) 0.1563(3) 0.0210(9) Uani 1 1 d . . . H29B H 0.8367 0.2122 0.1785 0.025 Uiso 1 1 calc R . . C30B C 0.8394(4) 0.2445(4) 0.0279(3) 0.0304(11) Uani 1 1 d . . . H30D H 0.8171 0.2673 -0.0196 0.046 Uiso 1 1 calc R . . H30E H 0.8623 0.1936 0.0146 0.046 Uiso 1 1 calc R . . H30F H 0.8959 0.2976 0.0576 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.01167(12) 0.01689(13) 0.01628(13) 0.00118(10) 0.00266(9) 0.00434(10) Si1A 0.0210(6) 0.0187(6) 0.0325(7) 0.0021(5) 0.0018(5) 0.0064(5) Si2A 0.0244(6) 0.0367(8) 0.0174(6) 0.0076(6) 0.0071(5) 0.0172(6) Si3A 0.0251(7) 0.0328(8) 0.0518(9) -0.0190(7) -0.0005(6) 0.0119(6) N1A 0.0208(19) 0.025(2) 0.0203(19) 0.0024(16) 0.0053(15) 0.0083(16) C1A 0.017(2) 0.020(2) 0.019(2) -0.0029(18) 0.0015(17) 0.0107(18) C2A 0.024(2) 0.037(3) 0.017(2) 0.001(2) 0.0030(18) 0.018(2) C3A 0.018(2) 0.030(3) 0.034(3) 0.014(2) 0.012(2) 0.012(2) C4A 0.014(2) 0.022(2) 0.038(3) 0.004(2) 0.0047(19) 0.0083(19) C5A 0.020(2) 0.025(2) 0.021(2) -0.0014(19) -0.0025(18) 0.0120(19) C6A 0.083(5) 0.040(4) 0.075(5) 0.023(3) 0.041(4) 0.025(4) C7A 0.056(4) 0.029(3) 0.079(5) 0.004(3) -0.032(3) 0.003(3) C8A 0.033(3) 0.028(3) 0.091(5) 0.008(3) 0.001(3) 0.015(2) C9A 0.0087(19) 0.027(2) 0.018(2) 0.0035(18) 0.0040(16) 0.0067(18) C10A 0.016(2) 0.015(2) 0.026(2) -0.0023(18) -0.0012(18) 0.0042(17) C11A 0.010(2) 0.027(2) 0.029(2) 0.011(2) 0.0034(18) 0.0038(18) C12A 0.012(2) 0.031(3) 0.020(2) 0.0012(19) 0.0045(17) 0.0078(19) C13A 0.014(2) 0.019(2) 0.018(2) 0.0018(18) -0.0002(16) 0.0058(17) C14A 0.030(3) 0.045(3) 0.022(2) 0.008(2) 0.013(2) 0.017(2) C15A 0.070(4) 0.071(4) 0.035(3) 0.029(3) 0.029(3) 0.055(4) C16A 0.047(3) 0.058(4) 0.020(3) -0.002(3) 0.000(2) 0.011(3) C17A 0.019(2) 0.018(2) 0.029(2) -0.0044(19) 0.0045(19) 0.0030(18) C18A 0.029(3) 0.019(2) 0.032(3) 0.006(2) 0.003(2) 0.003(2) C19A 0.028(3) 0.022(3) 0.037(3) -0.003(2) 0.017(2) -0.007(2) C20A 0.015(2) 0.024(3) 0.043(3) -0.009(2) 0.004(2) 0.001(2) C21A 0.026(2) 0.021(2) 0.027(2) -0.002(2) 0.000(2) 0.007(2) C22A 0.046(3) 0.038(3) 0.057(4) -0.020(3) 0.013(3) 0.009(3) C23A 0.115(6) 0.065(5) 0.120(6) -0.016(4) 0.087(5) 0.012(4) C24A 0.124(6) 0.145(7) 0.131(7) -0.082(5) -0.053(5) 0.106(6) C25A 0.018(2) 0.021(2) 0.024(2) 0.0058(19) 0.0004(18) 0.0084(19) C26A 0.024(2) 0.024(2) 0.024(2) 0.005(2) 0.0091(19) 0.006(2) C27A 0.028(2) 0.025(2) 0.018(2) 0.0041(19) 0.0039(19) 0.012(2) C28A 0.023(2) 0.023(2) 0.020(2) -0.0041(18) -0.0001(18) 0.0138(19) C29A 0.019(2) 0.028(3) 0.023(2) -0.0013(19) 0.0027(18) 0.009(2) C30A 0.034(3) 0.046(3) 0.028(3) -0.009(2) -0.006(2) 0.021(3) Ce2 0.01306(12) 0.01409(13) 0.01533(13) 0.00233(9) 0.00352(9) 0.00404(9) Si1B 0.0318(7) 0.0302(8) 0.0339(8) -0.0101(6) 0.0016(6) 0.0122(6) Si2B 0.0270(7) 0.0228(7) 0.0187(6) 0.0043(5) 0.0032(5) 0.0143(5) Si3B 0.0208(6) 0.0176(6) 0.0211(6) 0.0040(5) 0.0012(5) 0.0061(5) N1B 0.0212(19) 0.021(2) 0.0188(19) 0.0016(16) 0.0034(15) 0.0076(16) C1B 0.022(2) 0.015(2) 0.034(3) -0.002(2) 0.001(2) 0.0054(19) C2B 0.024(2) 0.012(2) 0.038(3) 0.002(2) 0.007(2) 0.0034(19) C3B 0.030(3) 0.014(2) 0.023(2) 0.0069(19) 0.008(2) 0.0029(19) C4B 0.021(2) 0.017(2) 0.044(3) 0.010(2) 0.015(2) 0.0048(19) C5B 0.023(2) 0.017(2) 0.028(3) 0.0025(19) -0.0039(19) 0.0031(19) C6B 0.063(4) 0.105(6) 0.039(3) -0.024(4) -0.003(3) 0.048(4) C7B 0.052(3) 0.035(3) 0.053(4) -0.006(3) 0.022(3) 0.015(3) C8B 0.060(4) 0.025(3) 0.070(4) -0.014(3) 0.017(3) 0.016(3) C9B 0.017(2) 0.019(2) 0.021(2) 0.0011(18) 0.0010(17) 0.0070(18) C10B 0.019(2) 0.022(2) 0.019(2) 0.0045(18) 0.0041(17) 0.0105(18) C11B 0.014(2) 0.031(3) 0.016(2) 0.0010(19) 0.0019(17) 0.0096(19) C12B 0.012(2) 0.021(2) 0.027(2) 0.0117(19) 0.0052(18) 0.0059(18) C13B 0.017(2) 0.018(2) 0.023(2) 0.0007(18) 0.0031(18) 0.0059(18) C14B 0.042(3) 0.032(3) 0.022(2) 0.002(2) -0.003(2) 0.017(2) C15B 0.051(3) 0.047(3) 0.023(3) 0.008(2) 0.011(2) 0.032(3) C16B 0.035(3) 0.028(3) 0.027(3) 0.009(2) 0.007(2) 0.015(2) C17B 0.016(2) 0.018(2) 0.016(2) 0.0000(17) 0.0030(16) 0.0072(17) C18B 0.019(2) 0.024(2) 0.019(2) 0.0021(18) 0.0019(17) 0.0120(19) C19B 0.025(2) 0.018(2) 0.023(2) 0.0081(18) 0.0136(19) 0.0121(19) C20B 0.013(2) 0.022(2) 0.035(3) 0.004(2) 0.0036(19) 0.0079(18) C21B 0.014(2) 0.019(2) 0.019(2) -0.0001(18) -0.0010(16) 0.0089(17) C22B 0.037(3) 0.038(3) 0.027(3) 0.011(2) 0.008(2) 0.015(2) C23B 0.033(3) 0.024(3) 0.040(3) 0.004(2) -0.003(2) 0.004(2) C24B 0.036(3) 0.019(3) 0.054(3) 0.003(2) 0.005(3) 0.009(2) C25B 0.019(2) 0.030(3) 0.019(2) -0.0011(19) 0.0045(18) 0.008(2) C26B 0.021(2) 0.036(3) 0.024(2) -0.001(2) -0.0003(19) 0.013(2) C27B 0.030(3) 0.032(3) 0.016(2) -0.003(2) -0.0015(19) 0.014(2) C28B 0.022(2) 0.021(2) 0.021(2) 0.0030(18) 0.0030(18) 0.0120(19) C29B 0.019(2) 0.022(2) 0.025(2) 0.0016(19) 0.0023(18) 0.0103(19) C30B 0.033(3) 0.036(3) 0.022(2) 0.005(2) 0.003(2) 0.012(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 N1A 2.693(3) . ? Ce1 C19A 2.794(4) . ? Ce1 C3A 2.809(4) . ? Ce1 C18A 2.818(4) . ? Ce1 C4A 2.824(4) . ? Ce1 C20A 2.838(4) . ? Ce1 C13A 2.844(4) . ? Ce1 C9A 2.842(4) . ? Ce1 C12A 2.843(4) . ? Ce1 C11A 2.844(4) . ? Ce1 C10A 2.845(4) . ? Ce1 C2A 2.856(4) . ? Ce1 C5A 2.858(4) . ? Ce1 C17A 2.859(4) . ? Ce1 C21A 2.860(4) . ? Ce1 C1A 2.905(4) . ? Si1A C7A 1.846(6) . ? Si1A C1A 1.859(4) . ? Si1A C8A 1.863(5) . ? Si1A C6A 1.880(6) . ? Si2A C9A 1.864(4) . ? Si2A C15A 1.868(5) . ? Si2A C14A 1.869(5) . ? Si2A C16A 1.866(5) . ? Si3A C24A 1.811(8) . ? Si3A C22A 1.829(6) . ? Si3A C17A 1.867(5) . ? Si3A C23A 1.930(8) . ? N1A C25A 1.336(5) . ? N1A C29A 1.348(5) . ? C1A C2A 1.420(6) . ? C1A C5A 1.428(6) . ? C2A C3A 1.401(6) . ? C3A C4A 1.404(6) . ? C4A C5A 1.402(6) . ? C9A C10A 1.419(6) . ? C9A C13A 1.436(6) . ? C10A C11A 1.404(6) . ? C11A C12A 1.416(6) . ? C12A C13A 1.394(6) . ? C17A C18A 1.412(6) . ? C17A C21A 1.416(6) . ? C18A C19A 1.406(7) . ? C19A C20A 1.405(7) . ? C20A C21A 1.398(6) . ? C25A C26A 1.377(6) . ? C26A C27A 1.383(6) . ? C27A C28A 1.391(6) . ? C28A C29A 1.378(6) . ? C28A C30A 1.511(6) . ? Ce2 N1B 2.709(3) . ? Ce2 C19B 2.791(4) . ? Ce2 C3B 2.812(4) . ? Ce2 C12B 2.825(4) . ? Ce2 C20B 2.828(4) . ? Ce2 C4B 2.833(4) . ? Ce2 C13B 2.833(4) . ? Ce2 C5B 2.836(4) . ? Ce2 C18B 2.834(4) . ? Ce2 C11B 2.848(4) . ? Ce2 C2B 2.855(4) . ? Ce2 C9B 2.857(4) . ? Ce2 C21B 2.861(4) . ? Ce2 C10B 2.866(4) . ? Ce2 C1B 2.870(4) . ? Ce2 C17B 2.892(4) . ? Si1B C1B 1.864(5) . ? Si1B C8B 1.865(6) . ? Si1B C7B 1.871(5) . ? Si1B C6B 1.869(6) . ? Si2B C9B 1.858(4) . ? Si2B C14B 1.858(5) . ? Si2B C16B 1.874(5) . ? Si2B C15B 1.871(5) . ? Si3B C17B 1.860(4) . ? Si3B C23B 1.864(5) . ? Si3B C22B 1.868(5) . ? Si3B C24B 1.877(5) . ? N1B C29B 1.332(5) . ? N1B C25B 1.347(5) . ? C1B C2B 1.409(6) . ? C1B C5B 1.426(6) . ? C2B C3B 1.405(6) . ? C3B C4B 1.403(7) . ? C4B C5B 1.399(7) . ? C9B C10B 1.424(6) . ? C9B C13B 1.434(6) . ? C10B C11B 1.401(6) . ? C11B C12B 1.409(6) . ? C12B C13B 1.396(6) . ? C17B C21B 1.413(6) . ? C17B C18B 1.420(6) . ? C18B C19B 1.401(6) . ? C19B C20B 1.402(6) . ? C20B C21B 1.401(6) . ? C25B C26B 1.377(6) . ? C26B C27B 1.378(6) . ? C27B C28B 1.383(6) . ? C28B C29B 1.397(6) . ? C28B C30B 1.500(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Ce1 C19A 119.81(13) . . ? N1A Ce1 C3A 118.37(12) . . ? C19A Ce1 C3A 76.46(14) . . ? N1A Ce1 C18A 114.88(13) . . ? C19A Ce1 C18A 29.01(14) . . ? C3A Ce1 C18A 103.21(14) . . ? N1A Ce1 C4A 91.14(12) . . ? C19A Ce1 C4A 80.92(14) . . ? C3A Ce1 C4A 28.86(13) . . ? C18A Ce1 C4A 109.78(13) . . ? N1A Ce1 C20A 93.02(13) . . ? C19A Ce1 C20A 28.87(14) . . ? C3A Ce1 C20A 78.71(14) . . ? C18A Ce1 C20A 47.34(14) . . ? C4A Ce1 C20A 68.79(13) . . ? N1A Ce1 C13A 107.16(11) . . ? C19A Ce1 C13A 97.02(14) . . ? C3A Ce1 C13A 130.87(12) . . ? C18A Ce1 C13A 71.06(13) . . ? C4A Ce1 C13A 159.62(13) . . ? C20A Ce1 C13A 117.76(13) . . ? N1A Ce1 C9A 128.70(11) . . ? C19A Ce1 C9A 97.97(14) . . ? C3A Ce1 C9A 102.42(13) . . ? C18A Ce1 C9A 81.46(13) . . ? C4A Ce1 C9A 130.61(13) . . ? C20A Ce1 C9A 126.10(13) . . ? C13A Ce1 C9A 29.25(12) . . ? N1A Ce1 C12A 81.70(11) . . ? C19A Ce1 C12A 121.46(14) . . ? C3A Ce1 C12A 143.97(13) . . ? C18A Ce1 C12A 92.87(13) . . ? C4A Ce1 C12A 157.14(13) . . ? C20A Ce1 C12A 132.95(13) . . ? C13A Ce1 C12A 28.38(12) . . ? C9A Ce1 C12A 47.91(12) . . ? N1A Ce1 C11A 84.28(12) . . ? C19A Ce1 C11A 143.27(14) . . ? C3A Ce1 C11A 118.39(14) . . ? C18A Ce1 C11A 118.00(14) . . ? C4A Ce1 C11A 129.16(13) . . ? C20A Ce1 C11A 161.78(14) . . ? C13A Ce1 C11A 47.07(12) . . ? C9A Ce1 C11A 47.77(12) . . ? C12A Ce1 C11A 28.84(13) . . ? N1A Ce1 C10A 111.66(11) . . ? C19A Ce1 C10A 124.66(14) . . ? C3A Ce1 C10A 96.73(13) . . ? C18A Ce1 C10A 110.31(13) . . ? C4A Ce1 C10A 118.07(13) . . ? C20A Ce1 C10A 153.53(13) . . ? C13A Ce1 C10A 47.13(12) . . ? C9A Ce1 C10A 28.90(12) . . ? C12A Ce1 C10A 47.26(13) . . ? C11A Ce1 C10A 28.57(12) . . ? N1A Ce1 C2A 115.27(12) . . ? C19A Ce1 C2A 101.84(14) . . ? C3A Ce1 C2A 28.62(13) . . ? C18A Ce1 C2A 124.09(13) . . ? C4A Ce1 C2A 47.10(13) . . ? C20A Ce1 C2A 107.33(13) . . ? C13A Ce1 C2A 114.65(12) . . ? C9A Ce1 C2A 86.02(12) . . ? C12A Ce1 C2A 117.21(13) . . ? C11A Ce1 C2A 90.01(13) . . ? C10A Ce1 C2A 71.45(13) . . ? C7A Si1A C1A 112.2(2) . . ? C7A Si1A C8A 109.5(3) . . ? C1A Si1A C8A 108.6(2) . . ? C7A Si1A C6A 110.0(3) . . ? C1A Si1A C6A 111.3(2) . . ? C8A Si1A C6A 105.0(3) . . ? C9A Si2A C15A 106.4(2) . . ? C9A Si2A C14A 113.61(19) . . ? C15A Si2A C14A 108.8(3) . . ? C9A Si2A C16A 108.6(2) . . ? C15A Si2A C16A 111.0(3) . . ? C14A Si2A C16A 108.4(2) . . ? C24A Si3A C22A 111.6(4) . . ? C24A Si3A C17A 114.7(3) . . ? C22A Si3A C17A 107.4(2) . . ? C24A Si3A C23A 107.8(5) . . ? C22A Si3A C23A 104.2(3) . . ? C17A Si3A C23A 110.6(3) . . ? C25A N1A C29A 116.7(4) . . ? C25A N1A Ce1 121.7(3) . . ? C29A N1A Ce1 121.4(3) . . ? C2A C1A C5A 105.3(4) . . ? C2A C1A Si1A 128.9(3) . . ? C5A C1A Si1A 123.6(3) . . ? C2A C1A Ce1 73.8(2) . . ? C5A C1A Ce1 73.8(2) . . ? Si1A C1A Ce1 130.06(19) . . ? C3A C2A C1A 109.6(4) . . ? C3A C2A Ce1 73.8(3) . . ? C1A C2A Ce1 77.6(2) . . ? C4A C3A C2A 108.0(4) . . ? C4A C3A Ce1 76.1(3) . . ? C2A C3A Ce1 77.6(3) . . ? C5A C4A C3A 107.7(4) . . ? C5A C4A Ce1 77.1(2) . . ? C3A C4A Ce1 75.0(2) . . ? C4A C5A C1A 109.5(4) . . ? C4A C5A Ce1 74.3(2) . . ? C1A C5A Ce1 77.5(2) . . ? C10A C9A C13A 105.6(4) . . ? C10A C9A Si2A 128.4(3) . . ? C13A C9A Si2A 124.9(3) . . ? C10A C9A Ce1 75.7(2) . . ? C13A C9A Ce1 75.5(2) . . ? Si2A C9A Ce1 123.04(18) . . ? C11A C10A C9A 109.3(4) . . ? C11A C10A Ce1 75.7(2) . . ? C9A C10A Ce1 75.4(2) . . ? C10A C11A C12A 107.9(4) . . ? C10A C11A Ce1 75.8(2) . . ? C12A C11A Ce1 75.5(2) . . ? C13A C12A C11A 107.8(4) . . ? C13A C12A Ce1 75.9(2) . . ? C11A C12A Ce1 75.6(2) . . ? C12A C13A C9A 109.3(4) . . ? C12A C13A Ce1 75.7(2) . . ? C9A C13A Ce1 75.3(2) . . ? C18A C17A C21A 105.4(4) . . ? C18A C17A Si3A 128.9(4) . . ? C21A C17A Si3A 122.6(3) . . ? C18A C17A Ce1 74.0(3) . . ? C21A C17A Ce1 75.7(3) . . ? Si3A C17A Ce1 131.0(2) . . ? C19A C18A C17A 109.4(4) . . ? C19A C18A Ce1 74.5(3) . . ? C17A C18A Ce1 77.2(3) . . ? C20A C19A C18A 107.8(4) . . ? C20A C19A Ce1 77.3(3) . . ? C18A C19A Ce1 76.5(3) . . ? C21A C20A C19A 107.3(4) . . ? C21A C20A Ce1 76.7(3) . . ? C19A C20A Ce1 73.8(2) . . ? C20A C21A C17A 110.0(4) . . ? C20A C21A Ce1 74.9(3) . . ? C17A C21A Ce1 75.6(3) . . ? N1A C25A C26A 123.2(4) . . ? C25A C26A C27A 119.1(4) . . ? C26A C27A C28A 119.2(4) . . ? C29A C28A C27A 117.2(4) . . ? C29A C28A C30A 121.9(4) . . ? C27A C28A C30A 120.9(4) . . ? N1A C29A C28A 124.6(4) . . ? N1B Ce2 C19B 118.46(12) . . ? N1B Ce2 C3B 126.32(12) . . ? C19B Ce2 C3B 81.60(13) . . ? N1B Ce2 C12B 83.67(11) . . ? C19B Ce2 C12B 117.23(13) . . ? C3B Ce2 C12B 133.65(12) . . ? N1B Ce2 C20B 91.24(12) . . ? C19B Ce2 C20B 28.89(13) . . ? C3B Ce2 C20B 90.04(13) . . ? C12B Ce2 C20B 127.63(13) . . ? N1B Ce2 C4B 106.28(12) . . ? C19B Ce2 C4B 71.84(13) . . ? C3B Ce2 C4B 28.77(13) . . ? C12B Ce2 C4B 161.91(13) . . ? C20B Ce2 C4B 68.26(13) . . ? N1B Ce2 C13B 111.69(11) . . ? C19B Ce2 C13B 97.44(13) . . ? C3B Ce2 C13B 114.13(13) . . ? C12B Ce2 C13B 28.56(12) . . ? C20B Ce2 C13B 119.04(13) . . ? C4B Ce2 C13B 140.84(13) . . ? N1B Ce2 C5B 80.35(12) . . ? C19B Ce2 C5B 94.53(13) . . ? C3B Ce2 C5B 47.15(13) . . ? C12B Ce2 C5B 148.23(13) . . ? C20B Ce2 C5B 80.18(13) . . ? C4B Ce2 C5B 28.57(13) . . ? C13B Ce2 C5B 155.76(13) . . ? N1B Ce2 C18B 115.00(11) . . ? C19B Ce2 C18B 28.83(12) . . ? C3B Ce2 C18B 104.46(13) . . ? C12B Ce2 C18B 88.60(13) . . ? C20B Ce2 C18B 47.18(13) . . ? C4B Ce2 C18B 100.28(13) . . ? C13B Ce2 C18B 72.24(12) . . ? C5B Ce2 C18B 123.06(13) . . ? N1B Ce2 C11B 78.96(11) . . ? C19B Ce2 C11B 144.05(13) . . ? C3B Ce2 C11B 114.65(13) . . ? C12B Ce2 C11B 28.77(12) . . ? C20B Ce2 C11B 154.66(13) . . ? C4B Ce2 C11B 136.85(13) . . ? C13B Ce2 C11B 47.01(13) . . ? C5B Ce2 C11B 120.32(13) . . ? C18B Ce2 C11B 116.46(12) . . ? N1B Ce2 C9B 126.45(11) . . ? C19B Ce2 C9B 105.45(13) . . ? C3B Ce2 C9B 87.23(13) . . ? C12B Ce2 C9B 48.06(12) . . ? C20B Ce2 C9B 133.73(13) . . ? C4B Ce2 C9B 115.80(13) . . ? C13B Ce2 C9B 29.18(12) . . ? C5B Ce2 C9B 126.82(12) . . ? C18B Ce2 C9B 89.11(12) . . ? C11B Ce2 C9B 47.76(12) . . ? N1B Ce2 C2B 109.11(12) . . ? C19B Ce2 C2B 110.30(12) . . ? C3B Ce2 C2B 28.70(13) . . ? C12B Ce2 C2B 115.77(13) . . ? C20B Ce2 C2B 115.07(13) . . ? C4B Ce2 C2B 47.04(13) . . ? C13B Ce2 C2B 109.17(13) . . ? C5B Ce2 C2B 46.69(13) . . ? C18B Ce2 C2B 131.55(13) . . ? C11B Ce2 C2B 90.25(13) . . ? C9B Ce2 C2B 80.14(13) . . ? C1B Si1B C8B 107.2(2) . . ? C1B Si1B C7B 115.1(2) . . ? C8B Si1B C7B 106.3(3) . . ? C1B Si1B C6B 108.4(2) . . ? C8B Si1B C6B 110.3(3) . . ? C7B Si1B C6B 109.4(3) . . ? C9B Si2B C14B 109.8(2) . . ? C9B Si2B C16B 109.8(2) . . ? C14B Si2B C16B 108.1(2) . . ? C9B Si2B C15B 109.8(2) . . ? C14B Si2B C15B 107.6(2) . . ? C16B Si2B C15B 111.7(2) . . ? C17B Si3B C23B 113.2(2) . . ? C17B Si3B C22B 110.5(2) . . ? C23B Si3B C22B 109.4(2) . . ? C17B Si3B C24B 107.8(2) . . ? C23B Si3B C24B 107.8(2) . . ? C22B Si3B C24B 107.9(2) . . ? C29B N1B C25B 116.7(4) . . ? C29B N1B Ce2 127.6(3) . . ? C25B N1B Ce2 115.6(3) . . ? C2B C1B C5B 105.4(4) . . ? C2B C1B Si1B 125.7(3) . . ? C5B C1B Si1B 126.9(3) . . ? C2B C1B Ce2 75.2(3) . . ? C5B C1B Ce2 74.2(2) . . ? Si1B C1B Ce2 128.2(2) . . ? C1B C2B C3B 109.6(4) . . ? C1B C2B Ce2 76.3(2) . . ? C3B C2B Ce2 74.0(2) . . ? C4B C3B C2B 107.9(4) . . ? C4B C3B Ce2 76.4(2) . . ? C2B C3B Ce2 77.3(2) . . ? C5B C4B C3B 107.5(4) . . ? C5B C4B Ce2 75.8(2) . . ? C3B C4B Ce2 74.8(2) . . ? C4B C5B C1B 109.6(4) . . ? C4B C5B Ce2 75.6(3) . . ? C1B C5B Ce2 76.8(2) . . ? C10B C9B C13B 104.9(4) . . ? C10B C9B Si2B 128.1(3) . . ? C13B C9B Si2B 126.0(3) . . ? C10B C9B Ce2 76.0(2) . . ? C13B C9B Ce2 74.5(2) . . ? Si2B C9B Ce2 123.08(19) . . ? C11B C10B C9B 109.6(4) . . ? C11B C10B Ce2 75.1(2) . . ? C9B C10B Ce2 75.2(2) . . ? C10B C11B C12B 107.9(4) . . ? C10B C11B Ce2 76.5(2) . . ? C12B C11B Ce2 74.7(2) . . ? C13B C12B C11B 107.7(4) . . ? C13B C12B Ce2 76.1(2) . . ? C11B C12B Ce2 76.5(2) . . ? C12B C13B C9B 109.7(4) . . ? C12B C13B Ce2 75.4(2) . . ? C9B C13B Ce2 76.3(2) . . ? C21B C17B C18B 105.4(4) . . ? C21B C17B Si3B 121.9(3) . . ? C18B C17B Si3B 129.8(3) . . ? C21B C17B Ce2 74.5(2) . . ? C18B C17B Ce2 73.4(2) . . ? Si3B C17B Ce2 131.80(19) . . ? C19B C18B C17B 109.4(4) . . ? C19B C18B Ce2 73.9(2) . . ? C17B C18B Ce2 77.9(2) . . ? C20B C19B C18B 107.9(4) . . ? C20B C19B Ce2 77.0(2) . . ? C18B C19B Ce2 77.3(2) . . ? C21B C20B C19B 107.5(4) . . ? C21B C20B Ce2 77.1(2) . . ? C19B C20B Ce2 74.1(2) . . ? C20B C21B C17B 109.8(4) . . ? C20B C21B Ce2 74.4(2) . . ? C17B C21B Ce2 77.0(2) . . ? N1B C25B C26B 123.3(4) . . ? C27B C26B C25B 118.5(4) . . ? C26B C27B C28B 120.3(4) . . ? C27B C28B C29B 116.4(4) . . ? C27B C28B C30B 122.9(4) . . ? C29B C28B C30B 120.7(4) . . ? N1B C29B C28B 124.7(4) . . ? #===END data_(Ce,SiMe~3~,lutidine) _database_code_depnum_ccdc_archive 'CCDC 223531' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H48 Ce N Si3' _chemical_formula_weight 659.09 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4967(3) _cell_length_b 20.2010(8) _cell_length_c 15.8279(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.302(2) _cell_angle_gamma 90.00 _cell_volume 3321.04(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22644 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method ? _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.560 _exptl_absorpt_correction_T_max 0.805 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 22644 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6178 _reflns_number_gt 5271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. All H atoms were introduced at calculated positions and treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0140P)^2^+2.4431P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6178 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0556 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.549 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.077 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 Ce Ce 0.220074(12) 0.054146(7) 0.803204(8) 0.01003(5) Uani 1 1 d . . . Si1 Si -0.14137(7) 0.16152(4) 0.79520(4) 0.01467(15) Uani 1 1 d . . . Si2 Si 0.39254(7) 0.21064(4) 0.95510(5) 0.01943(17) Uani 1 1 d . . . Si3 Si 0.26155(7) -0.04694(3) 0.56978(4) 0.01491(15) Uani 1 1 d . . . N N 0.0547(2) -0.04762(10) 0.80864(14) 0.0170(5) Uani 1 1 d . . . C1 C 0.0077(2) 0.14329(12) 0.74762(15) 0.0129(5) Uani 1 1 d . . . C2 C 0.0160(2) 0.10223(12) 0.67494(15) 0.0135(5) Uani 1 1 d . . . H2 H -0.0456 0.0715 0.6523 0.016 Uiso 1 1 calc R . . C3 C 0.1307(2) 0.11532(12) 0.64316(16) 0.0145(5) Uani 1 1 d . . . H3 H 0.1581 0.0953 0.5960 0.017 Uiso 1 1 calc R . . C4 C 0.1975(2) 0.16438(13) 0.69551(15) 0.0146(5) Uani 1 1 d . . . H4 H 0.2776 0.1820 0.6895 0.018 Uiso 1 1 calc R . . C5 C 0.1217(2) 0.18183(12) 0.75834(15) 0.0126(5) Uani 1 1 d . . . H5 H 0.1431 0.2137 0.8004 0.015 Uiso 1 1 calc R . . C6 C -0.2814(3) 0.15274(16) 0.70826(18) 0.0254(7) Uani 1 1 d . . . H6A H -0.3589 0.1656 0.7294 0.038 Uiso 1 1 calc R . . H6B H -0.2884 0.1075 0.6897 0.038 Uiso 1 1 calc R . . H6C H -0.2686 0.1806 0.6611 0.038 Uiso 1 1 calc R . . C7 C -0.1742(3) 0.10733(14) 0.88569(17) 0.0195(6) Uani 1 1 d . . . H7A H -0.1045 0.1111 0.9319 0.029 Uiso 1 1 calc R . . H7B H -0.1819 0.0622 0.8668 0.029 Uiso 1 1 calc R . . H7C H -0.2529 0.1210 0.9047 0.029 Uiso 1 1 calc R . . C8 C -0.1303(3) 0.24897(14) 0.83418(19) 0.0262(7) Uani 1 1 d . . . H8A H -0.0572 0.2535 0.8779 0.039 Uiso 1 1 calc R . . H8B H -0.2072 0.2602 0.8572 0.039 Uiso 1 1 calc R . . H8C H -0.1207 0.2781 0.7876 0.039 Uiso 1 1 calc R . . C9 C 0.3074(2) 0.13000(13) 0.95264(15) 0.0149(5) Uani 1 1 d . . . C10 C 0.1740(2) 0.11862(13) 0.95569(15) 0.0160(5) Uani 1 1 d . . . H10 H 0.1101 0.1509 0.9491 0.019 Uiso 1 1 calc R . . C11 C 0.1542(3) 0.05129(13) 0.97021(16) 0.0189(6) Uani 1 1 d . . . H11 H 0.0757 0.0312 0.9748 0.023 Uiso 1 1 calc R . . C12 C 0.2749(3) 0.01922(13) 0.97665(15) 0.0187(6) Uani 1 1 d . . . H12 H 0.2900 -0.0257 0.9859 0.022 Uiso 1 1 calc R . . C13 C 0.3676(2) 0.06729(13) 0.96657(15) 0.0162(6) Uani 1 1 d . . . H13 H 0.4553 0.0593 0.9687 0.019 Uiso 1 1 calc R . . C14 C 0.5268(3) 0.20721(18) 1.0466(2) 0.0499(10) Uani 1 1 d . . . H14A H 0.4920 0.2005 1.0988 0.075 Uiso 1 1 calc R . . H14B H 0.5739 0.2481 1.0498 0.075 Uiso 1 1 calc R . . H14C H 0.5835 0.1713 1.0381 0.075 Uiso 1 1 calc R . . C15 C 0.4629(3) 0.22635(15) 0.8550(2) 0.0314(7) Uani 1 1 d . . . H15A H 0.5133 0.1888 0.8427 0.047 Uiso 1 1 calc R . . H15B H 0.5169 0.2649 0.8623 0.047 Uiso 1 1 calc R . . H15C H 0.3948 0.2334 0.8085 0.047 Uiso 1 1 calc R . . C16 C 0.2810(3) 0.27967(14) 0.9724(2) 0.0314(7) Uani 1 1 d . . . H16A H 0.2156 0.2836 0.9236 0.047 Uiso 1 1 calc R . . H16B H 0.3286 0.3203 0.9804 0.047 Uiso 1 1 calc R . . H16C H 0.2415 0.2706 1.0222 0.047 Uiso 1 1 calc R . . C17 C 0.3379(2) -0.01805(12) 0.67641(16) 0.0140(5) Uani 1 1 d . . . C18 C 0.3530(2) -0.05887(13) 0.75078(16) 0.0164(5) Uani 1 1 d . . . H18 H 0.3127 -0.0995 0.7553 0.020 Uiso 1 1 calc R . . C19 C 0.4374(2) -0.02868(14) 0.81585(17) 0.0201(6) Uani 1 1 d . . . H19 H 0.4632 -0.0456 0.8703 0.024 Uiso 1 1 calc R . . C20 C 0.4763(2) 0.03199(14) 0.78407(17) 0.0197(6) Uani 1 1 d . . . H20 H 0.5317 0.0625 0.8141 0.024 Uiso 1 1 calc R . . C21 C 0.4166(2) 0.03841(13) 0.69863(17) 0.0167(6) Uani 1 1 d . . . H21 H 0.4270 0.0738 0.6627 0.020 Uiso 1 1 calc R . . C22 C 0.2830(3) 0.01408(14) 0.48335(16) 0.0214(6) Uani 1 1 d . . . H22A H 0.2252 0.0507 0.4858 0.032 Uiso 1 1 calc R . . H22B H 0.2645 -0.0071 0.4287 0.032 Uiso 1 1 calc R . . H22C H 0.3701 0.0299 0.4914 0.032 Uiso 1 1 calc R . . C23 C 0.0884(3) -0.06794(14) 0.57093(17) 0.0218(6) Uani 1 1 d . . . H23A H 0.0811 -0.0969 0.6181 0.033 Uiso 1 1 calc R . . H23B H 0.0546 -0.0896 0.5185 0.033 Uiso 1 1 calc R . . H23C H 0.0406 -0.0281 0.5768 0.033 Uiso 1 1 calc R . . C24 C 0.3464(3) -0.12436(14) 0.54456(19) 0.0267(7) Uani 1 1 d . . . H24A H 0.4346 -0.1143 0.5401 0.040 Uiso 1 1 calc R . . H24B H 0.3051 -0.1423 0.4914 0.040 Uiso 1 1 calc R . . H24C H 0.3430 -0.1562 0.5892 0.040 Uiso 1 1 calc R . . C25 C 0.0968(3) -0.10249(13) 0.85238(16) 0.0184(6) Uani 1 1 d . . . H25 H 0.1829 -0.1041 0.8766 0.022 Uiso 1 1 calc R . . C26 C 0.0196(2) -0.15676(13) 0.86352(16) 0.0170(6) Uani 1 1 d . . . C27 C -0.1083(2) -0.15300(13) 0.82638(17) 0.0183(6) Uani 1 1 d . . . H27 H -0.1633 -0.1882 0.8325 0.022 Uiso 1 1 calc R . . C28 C -0.1554(2) -0.09801(13) 0.78059(17) 0.0188(6) Uani 1 1 d . . . C29 C -0.0696(3) -0.04663(13) 0.77386(17) 0.0184(6) Uani 1 1 d . . . H29 H -0.1002 -0.0092 0.7433 0.022 Uiso 1 1 calc R . . C30 C 0.0723(3) -0.21662(13) 0.91282(18) 0.0228(6) Uani 1 1 d . . . H30A H 0.1644 -0.2134 0.9248 0.034 Uiso 1 1 calc R . . H30B H 0.0489 -0.2557 0.8797 0.034 Uiso 1 1 calc R . . H30C H 0.0372 -0.2190 0.9655 0.034 Uiso 1 1 calc R . . C31 C -0.2938(3) -0.09346(15) 0.7382(2) 0.0309(7) Uani 1 1 d . . . H31A H -0.3040 -0.1177 0.6855 0.046 Uiso 1 1 calc R . . H31B H -0.3161 -0.0479 0.7269 0.046 Uiso 1 1 calc R . . H31C H -0.3493 -0.1119 0.7754 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.01019(7) 0.00989(8) 0.00990(8) 0.00074(6) 0.00103(5) -0.00108(6) Si1 0.0144(3) 0.0167(4) 0.0140(3) 0.0018(3) 0.0056(3) 0.0014(3) Si2 0.0207(4) 0.0176(4) 0.0193(4) -0.0035(3) 0.0005(3) -0.0062(3) Si3 0.0179(4) 0.0140(4) 0.0129(3) -0.0006(3) 0.0021(3) 0.0024(3) N 0.0186(11) 0.0140(12) 0.0188(11) -0.0014(9) 0.0037(9) -0.0036(9) C1 0.0156(12) 0.0126(13) 0.0101(12) 0.0035(10) 0.0007(10) 0.0025(10) C2 0.0154(13) 0.0121(13) 0.0118(12) 0.0002(10) -0.0023(10) 0.0013(10) C3 0.0182(13) 0.0152(14) 0.0110(12) 0.0050(10) 0.0042(11) 0.0067(11) C4 0.0124(12) 0.0155(13) 0.0161(13) 0.0051(11) 0.0029(10) -0.0002(10) C5 0.0175(13) 0.0077(12) 0.0121(12) 0.0016(10) -0.0001(10) 0.0005(10) C6 0.0151(13) 0.0407(19) 0.0214(15) 0.0062(13) 0.0067(12) 0.0027(13) C7 0.0172(13) 0.0235(15) 0.0188(14) 0.0015(11) 0.0056(11) -0.0033(11) C8 0.0323(16) 0.0222(16) 0.0278(16) -0.0007(12) 0.0176(14) 0.0044(13) C9 0.0170(13) 0.0163(14) 0.0109(12) -0.0030(10) 0.0007(11) -0.0026(11) C10 0.0177(13) 0.0198(14) 0.0107(12) -0.0005(11) 0.0027(11) -0.0004(11) C11 0.0247(14) 0.0217(14) 0.0118(13) 0.0005(11) 0.0076(11) -0.0094(12) C12 0.0297(15) 0.0148(14) 0.0100(13) 0.0033(11) -0.0026(11) -0.0022(12) C13 0.0167(13) 0.0218(15) 0.0090(12) -0.0026(10) -0.0020(10) -0.0022(11) C14 0.050(2) 0.041(2) 0.050(2) 0.0054(18) -0.0224(18) -0.0232(17) C15 0.0297(16) 0.0275(17) 0.0409(19) -0.0109(14) 0.0185(15) -0.0149(14) C16 0.0450(19) 0.0182(16) 0.0346(18) -0.0088(13) 0.0177(15) -0.0069(14) C17 0.0125(12) 0.0152(14) 0.0146(13) 0.0007(10) 0.0035(11) 0.0043(10) C18 0.0164(13) 0.0144(13) 0.0187(13) 0.0006(11) 0.0041(11) 0.0053(11) C19 0.0168(13) 0.0285(16) 0.0147(13) 0.0021(12) 0.0009(11) 0.0085(12) C20 0.0081(12) 0.0271(15) 0.0233(14) -0.0069(12) 0.0003(11) 0.0003(11) C21 0.0134(12) 0.0167(14) 0.0211(14) -0.0008(11) 0.0064(11) 0.0027(10) C22 0.0279(15) 0.0223(15) 0.0147(13) 0.0022(11) 0.0055(12) 0.0027(12) C23 0.0236(15) 0.0223(16) 0.0181(14) -0.0013(11) -0.0019(12) -0.0018(12) C24 0.0357(17) 0.0203(15) 0.0245(15) -0.0019(12) 0.0056(13) 0.0082(13) C25 0.0186(13) 0.0215(15) 0.0150(13) -0.0035(11) 0.0021(11) -0.0027(11) C26 0.0243(14) 0.0156(14) 0.0130(13) -0.0056(11) 0.0087(11) -0.0029(11) C27 0.0212(14) 0.0137(14) 0.0225(14) -0.0075(11) 0.0119(12) -0.0069(11) C28 0.0166(13) 0.0182(14) 0.0232(15) -0.0057(11) 0.0085(12) -0.0023(11) C29 0.0208(14) 0.0160(14) 0.0197(14) -0.0018(11) 0.0077(11) 0.0018(11) C30 0.0300(15) 0.0176(15) 0.0209(14) -0.0016(12) 0.0041(12) -0.0041(12) C31 0.0170(14) 0.0257(17) 0.051(2) 0.0022(15) 0.0081(14) -0.0002(12) _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 Ce N 2.700(2) . ? Ce C20 2.786(2) . ? Ce C4 2.794(2) . ? Ce C12 2.812(2) . ? Ce C19 2.813(3) . ? Ce C11 2.828(2) . ? Ce C13 2.828(2) . ? Ce C5 2.830(2) . ? Ce C21 2.843(2) . ? Ce C10 2.845(2) . ? Ce C3 2.853(2) . ? Ce C9 2.856(2) . ? Ce C18 2.860(2) . ? Ce C2 2.898(3) . ? Ce C17 2.899(3) . ? Ce C1 2.902(2) . ? Si1 C1 1.868(2) . ? Si1 C8 1.869(3) . ? Si1 C6 1.871(3) . ? Si1 C7 1.874(3) . ? Si2 C9 1.855(3) . ? Si2 C16 1.866(3) . ? Si2 C15 1.870(3) . ? Si2 C14 1.870(3) . ? Si3 C17 1.855(3) . ? Si3 C23 1.869(3) . ? Si3 C24 1.871(3) . ? Si3 C22 1.879(3) . ? N C29 1.341(3) . ? N C25 1.347(3) . ? C1 C5 1.418(3) . ? C1 C2 1.431(3) . ? C2 C3 1.395(3) . ? C3 C4 1.412(4) . ? C4 C5 1.405(3) . ? C9 C13 1.419(4) . ? C9 C10 1.428(3) . ? C10 C11 1.400(4) . ? C11 C12 1.414(4) . ? C12 C13 1.400(4) . ? C17 C21 1.422(4) . ? C17 C18 1.427(4) . ? C18 C19 1.398(4) . ? C19 C20 1.407(4) . ? C20 C21 1.412(4) . ? C25 C26 1.390(4) . ? C26 C27 1.388(4) . ? C26 C30 1.501(4) . ? C27 C28 1.378(4) . ? C28 C29 1.389(4) . ? C28 C31 1.513(4) . ? 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 N Ce C20 121.09(7) . . ? N Ce C4 128.92(7) . . ? C20 Ce C4 93.43(8) . . ? N Ce C12 79.62(7) . . ? C20 Ce C12 90.06(8) . . ? C4 Ce C12 141.54(8) . . ? N Ce C19 93.63(8) . . ? C20 Ce C19 29.11(8) . . ? C4 Ce C19 120.92(8) . . ? C12 Ce C19 74.44(8) . . ? N Ce C11 73.12(7) . . ? C20 Ce C11 117.94(8) . . ? C4 Ce C11 125.17(8) . . ? C12 Ce C11 29.03(8) . . ? C19 Ce C11 103.10(8) . . ? N Ce C13 108.18(7) . . ? C20 Ce C13 72.82(8) . . ? C4 Ce C13 118.03(7) . . ? C12 Ce C13 28.74(7) . . ? C19 Ce C13 70.08(8) . . ? C11 Ce C13 47.38(8) . . ? N Ce C5 119.28(7) . . ? C20 Ce C5 116.23(8) . . ? C4 Ce C5 28.93(7) . . ? C12 Ce C5 119.30(8) . . ? C19 Ce C5 145.34(8) . . ? C11 Ce C5 97.10(7) . . ? C13 Ce C5 105.99(7) . . ? N Ce C21 117.21(7) . . ? C20 Ce C21 29.04(8) . . ? C4 Ce C21 74.84(7) . . ? C12 Ce C21 118.49(8) . . ? C19 Ce C21 47.60(8) . . ? C11 Ce C21 146.92(8) . . ? C13 Ce C21 101.26(8) . . ? C5 Ce C21 102.99(7) . . ? N Ce C10 97.62(7) . . ? C20 Ce C10 116.81(8) . . ? C4 Ce C10 98.22(7) . . ? C12 Ce C10 47.36(8) . . ? C19 Ce C10 116.59(8) . . ? C11 Ce C10 28.57(7) . . ? C13 Ce C10 47.09(7) . . ? C5 Ce C10 72.24(7) . . ? C21 Ce C10 140.52(7) . . ? N Ce C3 103.15(7) . . ? C20 Ce C3 99.91(8) . . ? C4 Ce C3 28.94(7) . . ? C12 Ce C3 165.98(8) . . ? C19 Ce C3 118.70(7) . . ? C11 Ce C3 138.19(8) . . ? C13 Ce C3 146.90(7) . . ? C5 Ce C3 47.25(7) . . ? C21 Ce C3 72.82(7) . . ? C10 Ce C3 118.72(7) . . ? N Ce C9 120.88(7) . . ? C20 Ce C9 88.66(8) . . ? C4 Ce C9 93.81(7) . . ? C12 Ce C9 47.95(7) . . ? C19 Ce C9 95.74(8) . . ? C11 Ce C9 47.89(7) . . ? C13 Ce C9 28.90(7) . . ? C5 Ce C9 77.33(7) . . ? C21 Ce C9 111.65(7) . . ? C10 Ce C9 29.00(7) . . ? C3 Ce C9 121.88(7) . . ? C1 Si1 C8 107.66(12) . . ? C1 Si1 C6 107.42(12) . . ? C8 Si1 C6 109.71(14) . . ? C1 Si1 C7 116.75(12) . . ? C8 Si1 C7 108.02(13) . . ? C6 Si1 C7 107.17(13) . . ? C9 Si2 C16 110.42(13) . . ? C9 Si2 C15 112.28(12) . . ? C16 Si2 C15 109.31(14) . . ? C9 Si2 C14 106.89(14) . . ? C16 Si2 C14 109.42(17) . . ? C15 Si2 C14 108.45(16) . . ? C17 Si3 C23 110.83(12) . . ? C17 Si3 C24 107.50(12) . . ? C23 Si3 C24 107.80(13) . . ? C17 Si3 C22 112.00(12) . . ? C23 Si3 C22 112.01(13) . . ? C24 Si3 C22 106.40(13) . . ? C29 N C25 116.8(2) . . ? C29 N Ce 124.57(17) . . ? C25 N Ce 118.57(16) . . ? C5 C1 C2 105.4(2) . . ? C5 C1 Si1 125.83(19) . . ? C2 C1 Si1 126.20(19) . . ? C5 C1 Ce 72.89(13) . . ? C2 C1 Ce 75.54(14) . . ? Si1 C1 Ce 130.66(11) . . ? C3 C2 C1 109.7(2) . . ? C3 C2 Ce 74.18(14) . . ? C1 C2 Ce 75.89(14) . . ? C2 C3 C4 107.6(2) . . ? C2 C3 Ce 77.76(14) . . ? C4 C3 Ce 73.20(14) . . ? C5 C4 C3 107.9(2) . . ? C5 C4 Ce 76.99(14) . . ? C3 C4 Ce 77.86(14) . . ? C4 C5 C1 109.4(2) . . ? C4 C5 Ce 74.08(14) . . ? C1 C5 Ce 78.50(14) . . ? C13 C9 C10 105.6(2) . . ? C13 C9 Si2 125.35(19) . . ? C10 C9 Si2 127.8(2) . . ? C13 C9 Ce 74.46(14) . . ? C10 C9 Ce 75.06(14) . . ? Si2 C9 Ce 125.76(11) . . ? C11 C10 C9 109.4(2) . . ? C11 C10 Ce 75.04(14) . . ? C9 C10 Ce 75.94(14) . . ? C10 C11 C12 107.7(2) . . ? C10 C11 Ce 76.39(14) . . ? C12 C11 Ce 74.88(14) . . ? C13 C12 C11 107.7(2) . . ? C13 C12 Ce 76.25(14) . . ? C11 C12 Ce 76.09(14) . . ? C12 C13 C9 109.6(2) . . ? C12 C13 Ce 75.00(14) . . ? C9 C13 Ce 76.64(14) . . ? C21 C17 C18 105.6(2) . . ? C21 C17 Si3 129.54(19) . . ? C18 C17 Si3 123.4(2) . . ? C21 C17 Ce 73.48(14) . . ? C18 C17 Ce 74.17(14) . . ? Si3 C17 Ce 128.08(11) . . ? C19 C18 C17 109.8(2) . . ? C19 C18 Ce 73.86(15) . . ? C17 C18 Ce 77.14(14) . . ? C18 C19 C20 107.6(2) . . ? C18 C19 Ce 77.62(15) . . ? C20 C19 Ce 74.38(15) . . ? C19 C20 C21 108.1(2) . . ? C19 C20 Ce 76.51(15) . . ? C21 C20 Ce 77.71(14) . . ? C20 C21 C17 109.0(2) . . ? C20 C21 Ce 73.25(14) . . ? C17 C21 Ce 77.85(14) . . ? N C25 C26 124.1(2) . . ? C27 C26 C25 116.7(2) . . ? C27 C26 C30 121.7(2) . . ? C25 C26 C30 121.6(2) . . ? C28 C27 C26 121.2(2) . . ? C27 C28 C29 117.1(2) . . ? C27 C28 C31 122.0(2) . . ? C29 C28 C31 120.9(3) . . ? N C29 C28 124.1(3) . . ? #===END data_(U,SiMe~3~,lutidine) _database_code_depnum_ccdc_archive 'CCDC 223532' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H48 N Si3 U' _chemical_formula_weight 757.00 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 8.8808(5) _cell_length_b 11.2881(7) _cell_length_c 17.2643(12) _cell_angle_alpha 71.573(3) _cell_angle_beta 81.505(3) _cell_angle_gamma 89.047(4) _cell_volume 1623.11(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11263 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method ? _exptl_crystal_F_000 750 _exptl_absorpt_coefficient_mu 5.130 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_T_max 0.638 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 11263 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5689 _reflns_number_gt 4917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5689 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.014 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.134 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 U U 0.58221(2) 0.518064(16) 0.752721(12) 0.01118(7) Uani 1 1 d . . . Si1 Si 0.68345(15) 0.19016(12) 0.67669(9) 0.0156(3) Uani 1 1 d . . . Si2 Si 0.76272(15) 0.76900(13) 0.52801(9) 0.0177(3) Uani 1 1 d . . . Si3 Si 0.23779(15) 0.73028(13) 0.84198(9) 0.0162(3) Uani 1 1 d . . . N N 0.3709(4) 0.3524(4) 0.8486(3) 0.0143(9) Uani 1 1 d . . . C1 C 0.7397(5) 0.3058(5) 0.7256(3) 0.0182(11) Uani 1 1 d . . . C2 C 0.8411(5) 0.4113(4) 0.6899(3) 0.0154(11) Uani 1 1 d . . . H2 H 0.8737 0.4482 0.6337 0.018 Uiso 1 1 calc R . . C3 C 0.8843(5) 0.4513(5) 0.7528(3) 0.0190(12) Uani 1 1 d . . . H3 H 0.9497 0.5188 0.7455 0.023 Uiso 1 1 calc R . . C4 C 0.8113(6) 0.3715(5) 0.8288(4) 0.0209(12) Uani 1 1 d . . . H4 H 0.8202 0.3758 0.8809 0.025 Uiso 1 1 calc R . . C5 C 0.7225(6) 0.2839(5) 0.8114(3) 0.0183(11) Uani 1 1 d . . . H5 H 0.6613 0.2207 0.8508 0.022 Uiso 1 1 calc R . . C6 C 0.4875(6) 0.1215(5) 0.7240(4) 0.0276(13) Uani 1 1 d . . . H6A H 0.4702 0.0500 0.7073 0.041 Uiso 1 1 calc R . . H6B H 0.4132 0.1829 0.7057 0.041 Uiso 1 1 calc R . . H6C H 0.4788 0.0966 0.7830 0.041 Uiso 1 1 calc R . . C7 C 0.8164(6) 0.0560(5) 0.7002(4) 0.0229(12) Uani 1 1 d . . . H7A H 0.8040 0.0149 0.7587 0.034 Uiso 1 1 calc R . . H7B H 0.9196 0.0869 0.6807 0.034 Uiso 1 1 calc R . . H7C H 0.7932 -0.0023 0.6731 0.034 Uiso 1 1 calc R . . C8 C 0.6947(6) 0.2564(5) 0.5620(3) 0.0240(12) Uani 1 1 d . . . H8A H 0.6985 0.1895 0.5386 0.036 Uiso 1 1 calc R . . H8B H 0.7848 0.3089 0.5395 0.036 Uiso 1 1 calc R . . H8C H 0.6066 0.3047 0.5489 0.036 Uiso 1 1 calc R . . C9 C 0.5946(5) 0.6651(4) 0.5875(3) 0.0137(10) Uani 1 1 d . . . C10 C 0.5731(5) 0.5411(4) 0.5868(3) 0.0158(11) Uani 1 1 d . . . H10 H 0.6445 0.4969 0.5628 0.019 Uiso 1 1 calc R . . C11 C 0.4278(6) 0.4961(5) 0.6277(3) 0.0178(11) Uani 1 1 d . . . H11 H 0.3868 0.4168 0.6364 0.021 Uiso 1 1 calc R . . C12 C 0.3533(5) 0.5926(5) 0.6538(3) 0.0165(11) Uani 1 1 d . . . H12 H 0.2554 0.5881 0.6827 0.020 Uiso 1 1 calc R . . C13 C 0.4556(5) 0.6961(5) 0.6276(3) 0.0156(11) Uani 1 1 d . . . H13 H 0.4353 0.7730 0.6354 0.019 Uiso 1 1 calc R . . C14 C 0.6984(7) 0.9319(5) 0.4870(5) 0.0423(18) Uani 1 1 d . . . H14A H 0.6541 0.9599 0.5321 0.063 Uiso 1 1 calc R . . H14B H 0.6239 0.9341 0.4516 0.063 Uiso 1 1 calc R . . H14C H 0.7841 0.9857 0.4562 0.063 Uiso 1 1 calc R . . C15 C 0.9181(6) 0.7730(5) 0.5883(4) 0.0277(13) Uani 1 1 d . . . H15A H 0.9595 0.6914 0.6066 0.042 Uiso 1 1 calc R . . H15B H 0.8783 0.7980 0.6354 0.042 Uiso 1 1 calc R . . H15C H 0.9968 0.8317 0.5542 0.042 Uiso 1 1 calc R . . C16 C 0.8421(7) 0.7099(7) 0.4408(4) 0.0458(19) Uani 1 1 d . . . H16A H 0.9359 0.7545 0.4129 0.069 Uiso 1 1 calc R . . H16B H 0.7704 0.7224 0.4027 0.069 Uiso 1 1 calc R . . H16C H 0.8609 0.6224 0.4623 0.069 Uiso 1 1 calc R . . C17 C 0.4413(5) 0.6867(4) 0.8318(3) 0.0141(10) Uani 1 1 d . . . C18 C 0.5722(5) 0.7519(4) 0.7786(3) 0.0136(10) Uani 1 1 d . . . H18 H 0.5703 0.8204 0.7315 0.016 Uiso 1 1 calc R . . C19 C 0.7046(5) 0.6975(5) 0.8077(3) 0.0160(11) Uani 1 1 d . . . H19 H 0.8044 0.7215 0.7829 0.019 Uiso 1 1 calc R . . C20 C 0.6577(5) 0.5985(4) 0.8824(3) 0.0138(10) Uani 1 1 d . . . H20 H 0.7213 0.5474 0.9161 0.017 Uiso 1 1 calc R . . C21 C 0.4980(5) 0.5926(5) 0.8956(3) 0.0165(11) Uani 1 1 d . . . H21 H 0.4382 0.5351 0.9398 0.020 Uiso 1 1 calc R . . C22 C 0.1779(6) 0.8330(5) 0.7442(3) 0.0209(12) Uani 1 1 d . . . H22A H 0.1704 0.7850 0.7077 0.031 Uiso 1 1 calc R . . H22B H 0.2518 0.9001 0.7181 0.031 Uiso 1 1 calc R . . H22C H 0.0805 0.8666 0.7564 0.031 Uiso 1 1 calc R . . C23 C 0.1120(5) 0.5855(5) 0.8858(4) 0.0245(13) Uani 1 1 d . . . H23A H 0.1399 0.5360 0.9377 0.037 Uiso 1 1 calc R . . H23B H 0.1240 0.5380 0.8481 0.037 Uiso 1 1 calc R . . H23C H 0.0077 0.6085 0.8939 0.037 Uiso 1 1 calc R . . C24 C 0.2106(6) 0.8195(5) 0.9182(4) 0.0260(13) Uani 1 1 d . . . H24A H 0.1051 0.8385 0.9279 0.039 Uiso 1 1 calc R . . H24B H 0.2710 0.8957 0.8964 0.039 Uiso 1 1 calc R . . H24C H 0.2417 0.7697 0.9692 0.039 Uiso 1 1 calc R . . C25 C 0.3973(5) 0.2888(4) 0.9257(3) 0.0158(11) Uani 1 1 d . . . H25 H 0.4723 0.3201 0.9469 0.019 Uiso 1 1 calc R . . C26 C 0.3190(6) 0.1795(4) 0.9749(3) 0.0165(11) Uani 1 1 d . . . C27 C 0.2080(5) 0.1330(4) 0.9430(3) 0.0164(11) Uani 1 1 d . . . H27 H 0.1538 0.0596 0.9745 0.020 Uiso 1 1 calc R . . C28 C 0.1771(5) 0.1957(4) 0.8637(3) 0.0161(11) Uani 1 1 d . . . C29 C 0.2602(5) 0.3058(4) 0.8204(3) 0.0154(11) Uani 1 1 d . . . H29 H 0.2377 0.3502 0.7683 0.018 Uiso 1 1 calc R . . C30 C 0.3574(7) 0.1119(5) 1.0591(4) 0.0322(14) Uani 1 1 d . . . H30A H 0.4312 0.0501 1.0552 0.048 Uiso 1 1 calc R . . H30B H 0.2669 0.0719 1.0949 0.048 Uiso 1 1 calc R . . H30C H 0.3988 0.1705 1.0810 0.048 Uiso 1 1 calc R . . C31 C 0.0666(6) 0.1449(5) 0.8234(4) 0.0220(12) Uani 1 1 d . . . H31A H 0.0290 0.2124 0.7819 0.033 Uiso 1 1 calc R . . H31B H -0.0169 0.1023 0.8642 0.033 Uiso 1 1 calc R . . H31C H 0.1171 0.0875 0.7982 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.01162(10) 0.01081(10) 0.01115(11) -0.00342(7) -0.00199(6) 0.00018(7) Si1 0.0153(7) 0.0127(7) 0.0203(8) -0.0071(6) -0.0031(6) 0.0018(6) Si2 0.0181(7) 0.0182(7) 0.0157(8) -0.0046(6) 0.0000(6) -0.0033(6) Si3 0.0137(7) 0.0171(7) 0.0184(8) -0.0064(6) -0.0026(6) 0.0037(6) N 0.016(2) 0.016(2) 0.012(2) -0.0065(18) 0.0000(17) 0.0023(17) C1 0.011(2) 0.020(3) 0.024(3) -0.010(2) 0.002(2) 0.004(2) C2 0.016(2) 0.016(2) 0.018(3) -0.010(2) -0.004(2) 0.005(2) C3 0.015(3) 0.018(3) 0.028(3) -0.012(3) -0.007(2) 0.007(2) C4 0.025(3) 0.020(3) 0.025(3) -0.014(3) -0.013(2) 0.011(2) C5 0.019(3) 0.015(2) 0.015(3) 0.000(2) 0.002(2) 0.006(2) C6 0.025(3) 0.022(3) 0.038(4) -0.012(3) -0.004(3) -0.001(2) C7 0.021(3) 0.016(3) 0.032(4) -0.009(2) -0.004(2) 0.003(2) C8 0.031(3) 0.024(3) 0.023(3) -0.014(3) -0.009(2) 0.008(2) C9 0.016(2) 0.015(2) 0.008(3) 0.000(2) -0.003(2) -0.001(2) C10 0.017(3) 0.019(3) 0.013(3) -0.006(2) -0.007(2) -0.001(2) C11 0.022(3) 0.015(2) 0.019(3) -0.006(2) -0.013(2) -0.001(2) C12 0.012(2) 0.023(3) 0.013(3) -0.002(2) -0.006(2) -0.001(2) C13 0.018(3) 0.015(2) 0.014(3) -0.004(2) -0.005(2) 0.003(2) C14 0.032(3) 0.026(3) 0.053(5) 0.012(3) -0.011(3) -0.006(3) C15 0.019(3) 0.030(3) 0.032(4) -0.009(3) 0.002(2) -0.007(2) C16 0.039(4) 0.073(5) 0.031(4) -0.030(4) 0.012(3) -0.027(4) C17 0.018(2) 0.015(2) 0.010(3) -0.005(2) -0.003(2) 0.002(2) C18 0.016(2) 0.012(2) 0.016(3) -0.009(2) -0.003(2) 0.002(2) C19 0.018(3) 0.022(3) 0.013(3) -0.013(2) 0.003(2) -0.003(2) C20 0.015(2) 0.014(2) 0.016(3) -0.008(2) -0.006(2) 0.008(2) C21 0.018(3) 0.019(3) 0.011(3) -0.003(2) -0.002(2) -0.002(2) C22 0.016(3) 0.028(3) 0.017(3) -0.006(2) -0.002(2) 0.007(2) C23 0.012(3) 0.027(3) 0.032(4) -0.008(3) 0.000(2) 0.004(2) C24 0.017(3) 0.029(3) 0.034(4) -0.015(3) -0.001(2) 0.008(2) C25 0.014(2) 0.019(3) 0.020(3) -0.013(2) -0.003(2) 0.003(2) C26 0.024(3) 0.012(2) 0.013(3) -0.004(2) -0.001(2) 0.005(2) C27 0.019(3) 0.007(2) 0.020(3) -0.005(2) 0.008(2) -0.003(2) C28 0.008(2) 0.015(2) 0.024(3) -0.010(2) 0.007(2) 0.003(2) C29 0.012(2) 0.015(2) 0.019(3) -0.006(2) -0.001(2) 0.007(2) C30 0.052(4) 0.024(3) 0.021(3) -0.005(3) -0.012(3) -0.005(3) C31 0.018(3) 0.015(3) 0.033(4) -0.007(2) -0.004(2) -0.002(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 U N 2.646(4) . ? U C3 2.775(5) . ? U C19 2.789(5) . ? U C9 2.797(5) . ? U C12 2.796(5) . ? U C11 2.797(5) . ? U C13 2.805(5) . ? U C10 2.807(5) . ? U C18 2.810(4) . ? U C2 2.813(4) . ? U C4 2.812(5) . ? U C20 2.834(5) . ? U C21 2.845(5) . ? U C17 2.848(5) . ? U C5 2.852(5) . ? U C1 2.885(5) . ? Si1 C8 1.871(6) . ? Si1 C1 1.874(5) . ? Si1 C6 1.876(5) . ? Si1 C7 1.883(5) . ? Si2 C15 1.857(6) . ? Si2 C14 1.863(6) . ? Si2 C16 1.875(6) . ? Si2 C9 1.872(5) . ? Si3 C17 1.863(5) . ? Si3 C22 1.867(5) . ? Si3 C24 1.881(5) . ? Si3 C23 1.876(5) . ? N C29 1.343(6) . ? N C25 1.350(6) . ? C1 C5 1.407(7) . ? C1 C2 1.420(7) . ? C2 C3 1.403(7) . ? C3 C4 1.406(7) . ? C4 C5 1.405(7) . ? C9 C13 1.418(7) . ? C9 C10 1.421(7) . ? C10 C11 1.395(7) . ? C11 C12 1.424(7) . ? C12 C13 1.405(7) . ? C17 C21 1.415(7) . ? C17 C18 1.422(7) . ? C18 C19 1.403(7) . ? C19 C20 1.424(7) . ? C20 C21 1.402(7) . ? C25 C26 1.386(7) . ? C26 C27 1.383(7) . ? C26 C30 1.499(8) . ? C27 C28 1.393(7) . ? C28 C29 1.388(7) . ? C28 C31 1.500(7) . ? 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 N U C3 117.79(14) . . ? N U C19 121.45(13) . . ? C3 U C19 77.92(14) . . ? N U C9 129.59(13) . . ? C3 U C9 99.92(15) . . ? C19 U C9 97.09(14) . . ? N U C12 83.21(14) . . ? C3 U C12 144.26(15) . . ? C19 U C12 117.32(15) . . ? C9 U C12 48.67(14) . . ? N U C11 82.85(14) . . ? C3 U C11 119.57(15) . . ? C19 U C11 141.29(15) . . ? C9 U C11 48.45(14) . . ? C12 U C11 29.49(14) . . ? N U C13 110.51(13) . . ? C3 U C13 127.81(15) . . ? C19 U C13 93.58(15) . . ? C9 U C13 29.32(14) . . ? C12 U C13 29.05(14) . . ? C11 U C13 47.91(14) . . ? N U C10 109.51(13) . . ? C3 U C10 96.32(15) . . ? C19 U C10 125.15(14) . . ? C9 U C10 29.37(14) . . ? C12 U C10 48.06(14) . . ? C11 U C10 28.83(14) . . ? C13 U C10 47.70(14) . . ? N U C18 114.94(13) . . ? C3 U C18 105.14(14) . . ? C19 U C18 29.02(14) . . ? C9 U C18 82.69(14) . . ? C12 U C18 89.04(14) . . ? C11 U C18 116.07(14) . . ? C13 U C18 69.02(14) . . ? C10 U C18 111.66(14) . . ? N U C2 113.92(13) . . ? C3 U C2 29.09(14) . . ? C19 U C2 103.44(14) . . ? C9 U C2 83.15(14) . . ? C12 U C2 117.69(15) . . ? C11 U C2 90.73(14) . . ? C13 U C2 112.22(15) . . ? C10 U C2 70.30(15) . . ? C18 U C2 126.26(13) . . ? N U C4 90.53(14) . . ? C3 U C4 29.13(15) . . ? C19 U C4 82.76(15) . . ? C9 U C4 128.28(15) . . ? C12 U C4 159.28(15) . . ? C11 U C4 130.18(14) . . ? C13 U C4 156.91(16) . . ? C10 U C4 117.29(15) . . ? C18 U C4 111.44(14) . . ? C2 U C4 47.64(15) . . ? N U C20 94.62(13) . . ? C3 U C20 78.97(14) . . ? C19 U C20 29.33(14) . . ? C9 U C20 126.12(14) . . ? C12 U C20 130.81(14) . . ? C11 U C20 160.25(14) . . ? C13 U C20 116.46(14) . . ? C10 U C20 154.45(14) . . ? C18 U C20 47.56(14) . . ? C2 U C20 108.05(14) . . ? C4 U C20 69.24(14) . . ? C8 Si1 C1 113.4(2) . . ? C8 Si1 C6 109.9(3) . . ? C1 Si1 C6 111.1(2) . . ? C8 Si1 C7 108.2(2) . . ? C1 Si1 C7 108.0(2) . . ? C6 Si1 C7 106.0(2) . . ? C15 Si2 C14 107.4(3) . . ? C15 Si2 C16 108.1(3) . . ? C14 Si2 C16 110.3(4) . . ? C15 Si2 C9 114.9(2) . . ? C14 Si2 C9 109.0(2) . . ? C16 Si2 C9 107.1(3) . . ? C17 Si3 C22 114.4(2) . . ? C17 Si3 C24 107.2(2) . . ? C22 Si3 C24 107.2(3) . . ? C17 Si3 C23 109.8(2) . . ? C22 Si3 C23 110.3(3) . . ? C24 Si3 C23 107.8(3) . . ? C29 N C25 116.7(4) . . ? C29 N U 123.8(3) . . ? C25 N U 117.4(3) . . ? C5 C1 C2 105.5(4) . . ? C5 C1 Si1 124.2(4) . . ? C2 C1 Si1 128.1(4) . . ? C5 C1 U 74.5(3) . . ? C2 C1 U 72.8(3) . . ? Si1 C1 U 130.4(2) . . ? C3 C2 C1 109.3(5) . . ? C3 C2 U 74.0(3) . . ? C1 C2 U 78.4(3) . . ? C2 C3 C4 108.0(5) . . ? C2 C3 U 77.0(3) . . ? C4 C3 U 76.9(3) . . ? C5 C4 C3 107.1(5) . . ? C5 C4 U 77.2(3) . . ? C3 C4 U 73.9(3) . . ? C4 C5 C1 110.1(5) . . ? C4 C5 U 74.1(3) . . ? C1 C5 U 77.1(3) . . ? C13 C9 C10 106.1(4) . . ? C13 C9 Si2 129.2(4) . . ? C10 C9 Si2 123.7(4) . . ? C13 C9 U 75.6(3) . . ? C10 C9 U 75.7(3) . . ? Si2 C9 U 122.9(2) . . ? C11 C10 C9 109.2(4) . . ? C11 C10 U 75.2(3) . . ? C9 C10 U 74.9(3) . . ? C10 C11 C12 108.1(4) . . ? C10 C11 U 76.0(3) . . ? C12 C11 U 75.2(3) . . ? C13 C12 C11 107.1(4) . . ? C13 C12 U 75.8(3) . . ? C11 C12 U 75.3(3) . . ? C12 C13 C9 109.5(4) . . ? C12 C13 U 75.1(3) . . ? C9 C13 U 75.0(3) . . ? C21 C17 C18 105.5(4) . . ? C21 C17 Si3 121.4(4) . . ? C18 C17 Si3 131.0(4) . . ? C21 C17 U 75.5(3) . . ? C18 C17 U 74.0(3) . . ? Si3 C17 U 128.4(2) . . ? C19 C18 C17 109.9(4) . . ? C19 C18 U 74.6(3) . . ? C17 C18 U 76.9(3) . . ? C18 C19 C20 107.2(4) . . ? C18 C19 U 76.4(3) . . ? C20 C19 U 77.1(3) . . ? C21 C20 C19 107.3(4) . . ? C21 C20 U 76.1(3) . . ? C19 C20 U 73.6(3) . . ? C20 C21 C17 110.1(4) . . ? C20 C21 U 75.3(3) . . ? C17 C21 U 75.7(3) . . ? N C25 C26 123.7(5) . . ? C25 C26 C27 117.9(5) . . ? C25 C26 C30 120.8(5) . . ? C27 C26 C30 121.3(5) . . ? C26 C27 C28 120.2(4) . . ? C29 C28 C27 117.1(5) . . ? C29 C28 C31 120.2(5) . . ? C27 C28 C31 122.6(4) . . ? N C29 C28 124.4(5) . . ? #===END data_(Ce,Bu^t^,pyridazine) _database_code_depnum_ccdc_archive 'CCDC 223533' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H43 Ce N2' _chemical_formula_weight 583.79 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5985(3) _cell_length_b 26.9296(8) _cell_length_c 11.8362(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.803(2) _cell_angle_gamma 90.00 _cell_volume 2799.22(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19232 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method ? _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 1.647 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.648 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 19232 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5285 _reflns_number_gt 4175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)+1.4833P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5285 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.662 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.088 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 Ce Ce 0.28308(2) 0.868859(6) 0.027420(16) 0.01772(6) Uani 1 1 d . . . N1 N 0.5645(3) 0.89764(10) 0.1668(2) 0.0238(6) Uani 1 1 d . . . N2 N 0.5701(3) 0.84929(10) 0.1950(2) 0.0228(6) Uani 1 1 d . . . C1 C 0.2548(4) 0.88026(11) 0.2682(3) 0.0195(7) Uani 1 1 d . . . C2 C 0.1587(4) 0.91518(12) 0.1856(3) 0.0209(7) Uani 1 1 d . . . H2 H 0.1709 0.9495 0.1922 0.025 Uiso 1 1 calc R . . C3 C 0.0398(4) 0.88973(14) 0.0904(3) 0.0253(7) Uani 1 1 d . . . H3 H -0.0404 0.9043 0.0251 0.030 Uiso 1 1 calc R . . C4 C 0.0643(4) 0.83856(13) 0.1120(3) 0.0241(7) Uani 1 1 d . . . H4 H 0.0030 0.8133 0.0636 0.029 Uiso 1 1 calc R . . C5 C 0.1989(4) 0.83226(12) 0.2206(3) 0.0234(7) Uani 1 1 d . . . H5 H 0.2430 0.8021 0.2548 0.028 Uiso 1 1 calc R . . C6 C 0.3739(4) 0.89089(12) 0.3979(3) 0.0224(7) Uani 1 1 d . . . C7 C 0.4861(4) 0.84784(13) 0.4490(3) 0.0288(8) Uani 1 1 d . . . H7A H 0.5578 0.8558 0.5309 0.043 Uiso 1 1 calc R . . H7B H 0.5395 0.8425 0.3967 0.043 Uiso 1 1 calc R . . H7C H 0.4314 0.8183 0.4513 0.043 Uiso 1 1 calc R . . C8 C 0.2887(4) 0.89717(14) 0.4830(3) 0.0306(8) Uani 1 1 d . . . H8A H 0.2204 0.9249 0.4555 0.046 Uiso 1 1 calc R . . H8B H 0.3608 0.9029 0.5661 0.046 Uiso 1 1 calc R . . H8C H 0.2317 0.8676 0.4804 0.046 Uiso 1 1 calc R . . C9 C 0.4601(4) 0.93919(13) 0.4013(3) 0.0317(8) Uani 1 1 d . . . H9A H 0.3886 0.9659 0.3688 0.048 Uiso 1 1 calc R . . H9B H 0.5182 0.9354 0.3522 0.048 Uiso 1 1 calc R . . H9C H 0.5274 0.9465 0.4850 0.048 Uiso 1 1 calc R . . C10 C 0.1130(4) 0.93471(11) -0.1885(3) 0.0216(7) Uani 1 1 d . . . C11 C 0.1379(4) 0.96218(11) -0.0800(3) 0.0230(7) Uani 1 1 d . . . H11 H 0.0626 0.9729 -0.0552 0.028 Uiso 1 1 calc R . . C12 C 0.2948(4) 0.97060(12) -0.0160(3) 0.0226(7) Uani 1 1 d . . . H12 H 0.3412 0.9876 0.0583 0.027 Uiso 1 1 calc R . . C13 C 0.3692(4) 0.94864(12) -0.0843(3) 0.0230(7) Uani 1 1 d . . . H13 H 0.4736 0.9486 -0.0632 0.028 Uiso 1 1 calc R . . C14 C 0.2574(4) 0.92677(11) -0.1903(3) 0.0216(7) Uani 1 1 d . . . H14 H 0.2757 0.9099 -0.2515 0.026 Uiso 1 1 calc R . . C15 C -0.0411(4) 0.92653(12) -0.2961(3) 0.0225(7) Uani 1 1 d . . . C16 C -0.0408(4) 0.88210(13) -0.3765(3) 0.0333(9) Uani 1 1 d . . . H16A H 0.0354 0.8869 -0.4086 0.050 Uiso 1 1 calc R . . H16B H -0.1390 0.8791 -0.4436 0.050 Uiso 1 1 calc R . . H16C H -0.0187 0.8524 -0.3276 0.050 Uiso 1 1 calc R . . C17 C -0.0774(4) 0.97323(13) -0.3777(3) 0.0315(9) Uani 1 1 d . . . H17A H -0.0800 1.0017 -0.3296 0.047 Uiso 1 1 calc R . . H17B H -0.1746 0.9693 -0.4455 0.047 Uiso 1 1 calc R . . H17C H -0.0002 0.9779 -0.4089 0.047 Uiso 1 1 calc R . . C18 C -0.1669(4) 0.91879(14) -0.2493(3) 0.0317(9) Uani 1 1 d . . . H18A H -0.1463 0.8892 -0.2000 0.048 Uiso 1 1 calc R . . H18B H -0.2633 0.9155 -0.3184 0.048 Uiso 1 1 calc R . . H18C H -0.1700 0.9468 -0.2002 0.048 Uiso 1 1 calc R . . C19 C 0.3976(4) 0.79010(11) -0.0946(3) 0.0202(7) Uani 1 1 d . . . C20 C 0.2488(4) 0.80388(11) -0.1760(3) 0.0213(7) Uani 1 1 d . . . H20 H 0.2236 0.8202 -0.2509 0.026 Uiso 1 1 calc R . . C21 C 0.1437(4) 0.78899(12) -0.1260(3) 0.0247(7) Uani 1 1 d . . . H21 H 0.0390 0.7942 -0.1609 0.030 Uiso 1 1 calc R . . C22 C 0.2281(4) 0.76485(11) -0.0135(3) 0.0252(7) Uani 1 1 d . . . H22 H 0.1883 0.7505 0.0386 0.030 Uiso 1 1 calc R . . C23 C 0.3819(4) 0.76605(11) 0.0067(3) 0.0235(7) Uani 1 1 d . . . H23 H 0.4615 0.7532 0.0755 0.028 Uiso 1 1 calc R . . C24 C 0.5415(4) 0.79448(12) -0.1185(3) 0.0223(7) Uani 1 1 d . . . C25 C 0.6650(4) 0.75889(13) -0.0354(3) 0.0289(8) Uani 1 1 d . . . H25A H 0.6903 0.7670 0.0496 0.043 Uiso 1 1 calc R . . H25B H 0.7541 0.7620 -0.0527 0.043 Uiso 1 1 calc R . . H25C H 0.6279 0.7254 -0.0510 0.043 Uiso 1 1 calc R . . C26 C 0.6083(4) 0.84742(12) -0.0967(3) 0.0288(8) Uani 1 1 d . . . H26A H 0.5343 0.8702 -0.1507 0.043 Uiso 1 1 calc R . . H26B H 0.6982 0.8482 -0.1134 0.043 Uiso 1 1 calc R . . H26C H 0.6339 0.8568 -0.0124 0.043 Uiso 1 1 calc R . . C27 C 0.5041(4) 0.78125(13) -0.2549(3) 0.0280(8) Uani 1 1 d . . . H27A H 0.4643 0.7481 -0.2715 0.042 Uiso 1 1 calc R . . H27B H 0.5950 0.7833 -0.2699 0.042 Uiso 1 1 calc R . . H27C H 0.4297 0.8041 -0.3080 0.042 Uiso 1 1 calc R . . C28 C 0.7039(4) 0.82775(12) 0.2567(3) 0.0256(8) Uani 1 1 d . . . H28 H 0.7064 0.7942 0.2757 0.031 Uiso 1 1 calc R . . C29 C 0.8400(4) 0.85355(13) 0.2937(3) 0.0280(8) Uani 1 1 d . . . H29 H 0.9325 0.8377 0.3369 0.034 Uiso 1 1 calc R . . C30 C 0.8348(4) 0.90299(14) 0.2649(3) 0.0296(8) Uani 1 1 d . . . H30 H 0.9231 0.9218 0.2877 0.036 Uiso 1 1 calc R . . C31 C 0.6923(4) 0.92381(12) 0.2004(3) 0.0258(8) Uani 1 1 d . . . H31 H 0.6860 0.9573 0.1799 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.01817(10) 0.01702(9) 0.01818(9) -0.00024(8) 0.00753(7) -0.00167(8) N1 0.0237(15) 0.0237(15) 0.0223(14) 0.0008(13) 0.0075(12) 0.0010(12) N2 0.0265(16) 0.0229(14) 0.0214(14) -0.0002(12) 0.0124(12) -0.0012(12) C1 0.0188(16) 0.0223(16) 0.0185(15) 0.0003(13) 0.0086(13) -0.0016(13) C2 0.0221(18) 0.0223(17) 0.0205(16) -0.0015(14) 0.0108(14) 0.0011(14) C3 0.0192(17) 0.039(2) 0.0188(16) 0.0025(16) 0.0088(13) 0.0005(15) C4 0.0213(18) 0.0308(19) 0.0224(17) -0.0022(15) 0.0110(14) -0.0078(15) C5 0.0247(18) 0.0233(17) 0.0270(17) 0.0028(15) 0.0153(15) -0.0034(14) C6 0.0227(17) 0.0239(16) 0.0196(16) -0.0010(14) 0.0075(14) 0.0007(14) C7 0.0251(19) 0.039(2) 0.0207(17) 0.0023(16) 0.0080(15) 0.0042(16) C8 0.038(2) 0.034(2) 0.0190(16) 0.0008(16) 0.0112(15) 0.0068(17) C9 0.030(2) 0.037(2) 0.0264(18) -0.0070(17) 0.0096(16) -0.0067(16) C10 0.0253(18) 0.0190(16) 0.0215(16) 0.0041(14) 0.0103(14) 0.0001(14) C11 0.0259(19) 0.0225(16) 0.0217(16) 0.0030(15) 0.0109(14) 0.0009(14) C12 0.0284(19) 0.0173(16) 0.0197(16) -0.0011(14) 0.0072(14) -0.0021(14) C13 0.0215(18) 0.0216(17) 0.0245(17) 0.0080(14) 0.0079(14) -0.0018(14) C14 0.0285(19) 0.0182(16) 0.0203(16) 0.0024(14) 0.0122(14) -0.0013(14) C15 0.0217(18) 0.0264(17) 0.0159(15) -0.0010(14) 0.0040(14) -0.0029(14) C16 0.0259(19) 0.040(2) 0.0260(18) -0.0061(16) 0.0019(15) 0.0019(16) C17 0.030(2) 0.035(2) 0.0242(18) 0.0081(16) 0.0054(15) 0.0028(16) C18 0.0236(19) 0.048(2) 0.0242(18) -0.0031(17) 0.0101(15) -0.0092(17) C19 0.0229(18) 0.0155(15) 0.0214(16) -0.0034(14) 0.0082(14) -0.0003(13) C20 0.0252(18) 0.0166(15) 0.0205(16) -0.0034(14) 0.0075(14) -0.0002(13) C21 0.0242(18) 0.0220(17) 0.0282(18) -0.0089(15) 0.0109(15) -0.0058(14) C22 0.0327(19) 0.0175(15) 0.0298(18) -0.0043(15) 0.0171(16) -0.0070(15) C23 0.0280(19) 0.0155(15) 0.0256(17) -0.0022(14) 0.0093(15) -0.0006(14) C24 0.0219(18) 0.0206(16) 0.0270(17) -0.0034(14) 0.0124(14) 0.0001(14) C25 0.0257(19) 0.0320(19) 0.0285(18) -0.0049(16) 0.0104(16) -0.0002(15) C26 0.0268(19) 0.0269(17) 0.036(2) -0.0021(16) 0.0166(16) -0.0007(15) C27 0.0265(19) 0.0308(19) 0.0273(18) -0.0005(16) 0.0113(15) 0.0035(15) C28 0.035(2) 0.0197(16) 0.0230(17) 0.0017(14) 0.0128(16) 0.0036(15) C29 0.0236(19) 0.037(2) 0.0224(17) -0.0001(16) 0.0080(14) 0.0062(15) C30 0.0226(19) 0.040(2) 0.0270(18) -0.0056(17) 0.0105(15) -0.0055(16) C31 0.032(2) 0.0216(17) 0.0229(17) -0.0004(15) 0.0100(15) -0.0060(15) _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 Ce N1 2.650(3) . ? Ce N2 2.719(3) . ? Ce C3 2.781(3) . ? Ce C21 2.784(3) . ? Ce C4 2.789(3) . ? Ce C12 2.798(3) . ? Ce C13 2.816(3) . ? Ce C22 2.855(3) . ? Ce C2 2.880(3) . ? Ce C20 2.885(3) . ? Ce C5 2.889(3) . ? Ce C11 2.906(3) . ? Ce C14 2.936(3) . ? Ce C1 2.986(3) . ? Ce C10 2.996(3) . ? Ce C19 3.012(3) . ? N1 C31 1.328(4) . ? N1 N2 1.340(4) . ? N2 C28 1.328(4) . ? C1 C2 1.401(4) . ? C1 C5 1.426(4) . ? C1 C6 1.526(4) . ? C2 C3 1.415(4) . ? C3 C4 1.404(5) . ? C4 C5 1.418(4) . ? C6 C7 1.531(5) . ? C6 C9 1.533(5) . ? C6 C8 1.543(5) . ? C10 C14 1.411(5) . ? C10 C11 1.416(4) . ? C10 C15 1.529(4) . ? C11 C12 1.404(5) . ? C12 C13 1.407(5) . ? C13 C14 1.409(4) . ? C15 C16 1.529(5) . ? C15 C18 1.532(5) . ? C15 C17 1.538(5) . ? C19 C20 1.412(4) . ? C19 C23 1.423(5) . ? C19 C24 1.523(5) . ? C20 C21 1.418(5) . ? C21 C22 1.408(5) . ? C22 C23 1.397(5) . ? C24 C25 1.533(5) . ? C24 C26 1.541(4) . ? C24 C27 1.547(4) . ? C28 C29 1.385(5) . ? C29 C30 1.370(5) . ? C30 C31 1.388(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 N1 Ce N2 28.87(8) . . ? N1 Ce C3 121.97(9) . . ? N2 Ce C3 123.85(9) . . ? N1 Ce C21 137.11(9) . . ? N2 Ce C21 113.88(9) . . ? C3 Ce C21 95.54(10) . . ? N1 Ce C4 126.05(9) . . ? N2 Ce C4 111.71(9) . . ? C3 Ce C4 29.20(10) . . ? C21 Ce C4 76.98(10) . . ? N1 Ce C12 73.83(9) . . ? N2 Ce C12 102.69(9) . . ? C3 Ce C12 87.23(11) . . ? C21 Ce C12 132.92(10) . . ? C4 Ce C12 116.38(10) . . ? N1 Ce C13 69.54(9) . . ? N2 Ce C13 95.01(9) . . ? C3 Ce C13 114.15(10) . . ? C21 Ce C13 115.98(10) . . ? C4 Ce C13 142.95(10) . . ? C12 Ce C13 29.03(10) . . ? N1 Ce C22 117.69(9) . . ? N2 Ce C22 89.83(9) . . ? C3 Ce C22 97.24(11) . . ? C21 Ce C22 28.88(9) . . ? C4 Ce C22 70.08(10) . . ? C12 Ce C22 161.41(10) . . ? C13 Ce C22 137.57(10) . . ? N1 Ce C2 93.14(9) . . ? N2 Ce C2 100.01(8) . . ? C3 Ce C2 28.89(9) . . ? C21 Ce C2 122.84(10) . . ? C4 Ce C2 47.41(10) . . ? C12 Ce C2 75.71(10) . . ? C13 Ce C2 104.60(10) . . ? C22 Ce C2 116.00(10) . . ? N1 Ce C20 116.17(9) . . ? N2 Ce C20 103.40(9) . . ? C3 Ce C20 121.40(10) . . ? C21 Ce C20 28.90(9) . . ? C4 Ce C20 105.85(10) . . ? C12 Ce C20 116.11(9) . . ? C13 Ce C20 91.56(9) . . ? C22 Ce C20 46.58(10) . . ? C2 Ce C20 150.17(9) . . ? N1 Ce C5 98.49(9) . . ? N2 Ce C5 83.18(9) . . ? C3 Ce C5 47.40(10) . . ? C21 Ce C5 92.20(10) . . ? C4 Ce C5 28.86(9) . . ? C12 Ce C5 121.61(10) . . ? C13 Ce C5 149.42(9) . . ? C22 Ce C5 73.01(10) . . ? C2 Ce C5 46.47(9) . . ? C20 Ce C5 118.64(9) . . ? N1 Ce C11 101.99(9) . . ? N2 Ce C11 130.74(9) . . ? C3 Ce C11 68.68(10) . . ? C21 Ce C11 111.30(10) . . ? C4 Ce C11 96.47(10) . . ? C12 Ce C11 28.42(9) . . ? C13 Ce C11 46.71(10) . . ? C22 Ce C11 138.68(10) . . ? C2 Ce C11 70.04(9) . . ? C20 Ce C11 106.63(9) . . ? C5 Ce C11 113.81(10) . . ? C31 N1 N2 120.1(3) . . ? C31 N1 Ce 158.0(2) . . ? N2 N1 Ce 78.41(17) . . ? C28 N2 N1 119.6(3) . . ? C28 N2 Ce 163.1(2) . . ? N1 N2 Ce 72.72(16) . . ? C2 C1 C5 107.2(3) . . ? C2 C1 C6 126.2(3) . . ? C5 C1 C6 125.3(3) . . ? C2 C1 Ce 71.99(18) . . ? C5 C1 Ce 72.20(17) . . ? C6 C1 Ce 131.3(2) . . ? C1 C2 C3 108.8(3) . . ? C1 C2 Ce 80.44(19) . . ? C3 C2 Ce 71.67(19) . . ? C4 C3 C2 108.0(3) . . ? C4 C3 Ce 75.7(2) . . ? C2 C3 Ce 79.44(19) . . ? C3 C4 C5 107.8(3) . . ? C3 C4 Ce 75.1(2) . . ? C5 C4 Ce 79.49(19) . . ? C4 C5 C1 108.0(3) . . ? C4 C5 Ce 71.64(18) . . ? C1 C5 Ce 79.78(18) . . ? C1 C6 C7 112.2(3) . . ? C1 C6 C9 111.3(3) . . ? C7 C6 C9 110.2(3) . . ? C1 C6 C8 107.3(3) . . ? C7 C6 C8 107.4(3) . . ? C9 C6 C8 108.2(3) . . ? C14 C10 C11 106.6(3) . . ? C14 C10 C15 126.2(3) . . ? C11 C10 C15 125.7(3) . . ? C14 C10 Ce 73.91(18) . . ? C11 C10 Ce 72.62(17) . . ? C15 C10 Ce 129.5(2) . . ? C12 C11 C10 109.0(3) . . ? C12 C11 Ce 71.52(18) . . ? C10 C11 Ce 79.67(18) . . ? C11 C12 C13 107.7(3) . . ? C11 C12 Ce 80.06(18) . . ? C13 C12 Ce 76.19(18) . . ? C12 C13 C14 107.9(3) . . ? C12 C13 Ce 74.79(18) . . ? C14 C13 Ce 80.62(18) . . ? C13 C14 C10 108.8(3) . . ? C13 C14 Ce 71.12(17) . . ? C10 C14 Ce 78.58(18) . . ? C10 C15 C16 112.8(3) . . ? C10 C15 C18 110.9(3) . . ? C16 C15 C18 108.5(3) . . ? C10 C15 C17 107.6(3) . . ? C16 C15 C17 107.8(3) . . ? C18 C15 C17 109.1(3) . . ? C20 C19 C23 105.8(3) . . ? C20 C19 C24 126.6(3) . . ? C23 C19 C24 127.2(3) . . ? C20 C19 Ce 71.21(18) . . ? C23 C19 Ce 74.55(18) . . ? C24 C19 Ce 124.66(19) . . ? C19 C20 C21 109.6(3) . . ? C19 C20 Ce 81.19(18) . . ? C21 C20 Ce 71.60(17) . . ? C22 C21 C20 106.9(3) . . ? C22 C21 Ce 78.35(18) . . ? C20 C21 Ce 79.51(18) . . ? C23 C22 C21 108.4(3) . . ? C23 C22 Ce 80.69(18) . . ? C21 C22 Ce 72.78(17) . . ? C22 C23 C19 109.3(3) . . ? C22 C23 Ce 71.63(18) . . ? C19 C23 Ce 77.93(17) . . ? C19 C24 C25 110.9(3) . . ? C19 C24 C26 112.8(3) . . ? C25 C24 C26 108.0(3) . . ? C19 C24 C27 109.3(3) . . ? C25 C24 C27 108.7(3) . . ? C26 C24 C27 107.1(3) . . ? N2 C28 C29 122.3(3) . . ? C30 C29 C28 118.3(3) . . ? C29 C30 C31 117.3(3) . . ? N1 C31 C30 122.4(3) . . ? #===END data_(Ce,Bu^t^,pyrimidine) _database_code_depnum_ccdc_archive 'CCDC 223534' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H47 Ce N4' _chemical_formula_weight 663.89 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.0533(4) _cell_length_b 8.6607(4) _cell_length_c 33.8212(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.866(2) _cell_angle_gamma 90.00 _cell_volume 3220.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21312 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method ? _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 1.442 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_decay_% none _diffrn_reflns_number 21312 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5962 _reflns_number_gt 4923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0210P)^2^+7.7123P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5962 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.506 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.089 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 Ce Ce 0.818045(18) 0.83253(2) 0.140142(6) 0.02309(8) Uani 1 1 d . . . N1 N 0.9407(3) 0.6208(4) 0.10262(10) 0.0278(7) Uani 1 1 d . . . N2 N 1.0294(4) 0.5833(4) 0.04147(11) 0.0448(9) Uani 1 1 d . . . C1 C 0.6014(3) 0.6763(5) 0.09565(11) 0.0285(8) Uani 1 1 d . . . C2 C 0.5594(3) 0.7860(5) 0.12198(12) 0.0321(9) Uani 1 1 d . . . H2 H 0.5183 0.7635 0.1439 0.039 Uiso 1 1 calc R . . C3 C 0.5899(3) 0.9355(5) 0.10955(13) 0.0343(9) Uani 1 1 d . . . H3 H 0.5732 1.0278 0.1219 0.041 Uiso 1 1 calc R . . C4 C 0.6498(4) 0.9198(5) 0.07535(12) 0.0342(9) Uani 1 1 d . . . H4 H 0.6784 1.0001 0.0606 0.041 Uiso 1 1 calc R . . C5 C 0.6593(3) 0.7611(5) 0.06717(12) 0.0309(9) Uani 1 1 d . . . H5 H 0.6975 0.7188 0.0464 0.037 Uiso 1 1 calc R . . C6 C 0.5639(3) 0.5079(5) 0.09202(12) 0.0335(9) Uani 1 1 d . . . C7 C 0.6590(4) 0.4105(5) 0.07313(16) 0.0481(12) Uani 1 1 d . . . H7A H 0.6712 0.4523 0.0475 0.072 Uiso 1 1 calc R . . H7B H 0.6307 0.3060 0.0701 0.072 Uiso 1 1 calc R . . H7C H 0.7344 0.4125 0.0899 0.072 Uiso 1 1 calc R . . C8 C 0.4435(4) 0.5006(5) 0.06488(16) 0.0499(12) Uani 1 1 d . . . H8A H 0.3829 0.5607 0.0763 0.075 Uiso 1 1 calc R . . H8B H 0.4168 0.3952 0.0622 0.075 Uiso 1 1 calc R . . H8C H 0.4556 0.5411 0.0392 0.075 Uiso 1 1 calc R . . C9 C 0.5424(5) 0.4343(6) 0.13206(15) 0.0533(13) Uani 1 1 d . . . H9A H 0.6178 0.4302 0.1488 0.080 Uiso 1 1 calc R . . H9B H 0.5112 0.3317 0.1277 0.080 Uiso 1 1 calc R . . H9C H 0.4847 0.4952 0.1447 0.080 Uiso 1 1 calc R . . C10 C 0.7614(3) 0.8147(5) 0.22162(11) 0.0292(8) Uani 1 1 d . . . C11 C 0.7212(4) 0.6729(5) 0.20399(11) 0.0315(8) Uani 1 1 d . . . H11 H 0.6405 0.6417 0.1992 0.038 Uiso 1 1 calc R . . C12 C 0.8225(4) 0.5870(5) 0.19483(12) 0.0332(9) Uani 1 1 d . . . H12 H 0.8207 0.4900 0.1830 0.040 Uiso 1 1 calc R . . C13 C 0.9277(4) 0.6748(5) 0.20690(11) 0.0318(9) Uani 1 1 d . . . H13 H 1.0075 0.6458 0.2043 0.038 Uiso 1 1 calc R . . C14 C 0.8907(3) 0.8129(5) 0.22338(11) 0.0295(8) Uani 1 1 d . . . H14 H 0.9422 0.8909 0.2338 0.035 Uiso 1 1 calc R . . C15 C 0.6856(4) 0.9364(5) 0.24037(12) 0.0329(9) Uani 1 1 d . . . C16 C 0.7107(5) 1.0986(6) 0.22479(16) 0.0560(14) Uani 1 1 d . . . H16A H 0.6866 1.1029 0.1967 0.084 Uiso 1 1 calc R . . H16B H 0.7960 1.1210 0.2298 0.084 Uiso 1 1 calc R . . H16C H 0.6652 1.1733 0.2381 0.084 Uiso 1 1 calc R . . C17 C 0.7208(5) 0.9388(7) 0.28509(14) 0.0606(14) Uani 1 1 d . . . H17A H 0.6752 1.0175 0.2970 0.091 Uiso 1 1 calc R . . H17B H 0.8062 0.9603 0.2903 0.091 Uiso 1 1 calc R . . H17C H 0.7034 0.8402 0.2962 0.091 Uiso 1 1 calc R . . C18 C 0.5504(4) 0.9044(7) 0.23248(19) 0.0696(18) Uani 1 1 d . . . H18A H 0.5323 0.8066 0.2439 0.104 Uiso 1 1 calc R . . H18B H 0.5276 0.9017 0.2043 0.104 Uiso 1 1 calc R . . H18C H 0.5058 0.9845 0.2442 0.104 Uiso 1 1 calc R . . C19 C 1.0530(3) 1.0041(5) 0.14414(11) 0.0273(8) Uani 1 1 d . . . C20 C 0.9714(3) 1.0907(4) 0.16481(11) 0.0277(8) Uani 1 1 d . . . H20 H 0.9793 1.1094 0.1920 0.033 Uiso 1 1 calc R . . C21 C 0.8757(3) 1.1441(4) 0.13739(12) 0.0317(9) Uani 1 1 d . . . H21 H 0.8095 1.2026 0.1434 0.038 Uiso 1 1 calc R . . C22 C 0.8981(4) 1.0937(5) 0.09955(13) 0.0357(10) Uani 1 1 d . . . H22 H 0.8508 1.1153 0.0759 0.043 Uiso 1 1 calc R . . C23 C 1.0042(3) 1.0049(5) 0.10371(11) 0.0305(8) Uani 1 1 d . . . H23 H 1.0376 0.9543 0.0831 0.037 Uiso 1 1 calc R . . C24 C 1.1802(3) 0.9504(5) 0.15961(12) 0.0300(9) Uani 1 1 d . . . C25 C 1.2718(4) 1.0631(5) 0.14335(13) 0.0384(10) Uani 1 1 d . . . H25A H 1.2620 1.0608 0.1148 0.058 Uiso 1 1 calc R . . H25B H 1.3531 1.0326 0.1528 0.058 Uiso 1 1 calc R . . H25C H 1.2570 1.1659 0.1524 0.058 Uiso 1 1 calc R . . C26 C 1.2064(4) 0.7890(5) 0.14437(15) 0.0417(11) Uani 1 1 d . . . H26A H 1.1524 0.7160 0.1547 0.063 Uiso 1 1 calc R . . H26B H 1.2890 0.7613 0.1529 0.063 Uiso 1 1 calc R . . H26C H 1.1942 0.7883 0.1159 0.063 Uiso 1 1 calc R . . C27 C 1.2003(4) 0.9523(5) 0.20499(12) 0.0384(10) Uani 1 1 d . . . H27A H 1.1832 1.0536 0.2145 0.058 Uiso 1 1 calc R . . H27B H 1.2832 0.9256 0.2135 0.058 Uiso 1 1 calc R . . H27C H 1.1470 0.8787 0.2155 0.058 Uiso 1 1 calc R . . C28 C 0.9605(4) 0.6570(5) 0.06504(12) 0.0354(9) Uani 1 1 d . . . H28 H 0.9209 0.7446 0.0544 0.043 Uiso 1 1 calc R . . C29 C 1.0845(4) 0.4568(5) 0.05730(15) 0.0475(12) Uani 1 1 d . . . H29 H 1.1345 0.4010 0.0420 0.057 Uiso 1 1 calc R . . C30 C 1.0707(4) 0.4058(5) 0.09489(15) 0.0412(11) Uani 1 1 d . . . H30 H 1.1088 0.3164 0.1050 0.049 Uiso 1 1 calc R . . C31 C 0.9970(3) 0.4936(5) 0.11721(13) 0.0338(9) Uani 1 1 d . . . H31 H 0.9867 0.4628 0.1430 0.041 Uiso 1 1 calc R . . N3 N 0.1422(3) -0.0801(4) 0.01189(10) 0.0365(8) Uani 1 1 d . . . N4 N 0.2584(3) 0.1492(4) 0.02663(10) 0.0365(8) Uani 1 1 d . . . C32 C 0.1555(4) 0.0725(5) 0.01613(12) 0.0339(9) Uani 1 1 d . . . H32 H 0.0854 0.1316 0.0112 0.041 Uiso 1 1 calc R . . C33 C 0.3577(4) 0.0616(5) 0.03360(13) 0.0378(10) Uani 1 1 d . . . H33 H 0.4319 0.1098 0.0407 0.045 Uiso 1 1 calc R . . C34 C 0.3550(4) -0.0968(5) 0.03071(13) 0.0354(9) Uani 1 1 d . . . H34 H 0.4249 -0.1561 0.0362 0.042 Uiso 1 1 calc R . . C35 C 0.2441(3) -0.1631(5) 0.01931(12) 0.0329(9) Uani 1 1 d . . . H35 H 0.2396 -0.2699 0.0166 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.02184(11) 0.02159(11) 0.02587(11) 0.00066(9) 0.00252(8) 0.00075(9) N1 0.0248(16) 0.0239(16) 0.0345(18) -0.0012(13) 0.0013(14) 0.0021(13) N2 0.056(2) 0.034(2) 0.047(2) -0.0084(17) 0.0147(19) -0.0002(18) C1 0.0233(18) 0.026(2) 0.035(2) -0.0024(18) -0.0013(15) 0.0037(17) C2 0.0233(19) 0.035(2) 0.038(2) -0.0002(17) 0.0027(17) -0.0001(17) C3 0.027(2) 0.022(2) 0.052(3) -0.0025(18) -0.0014(18) 0.0004(17) C4 0.031(2) 0.031(2) 0.038(2) 0.0100(18) -0.0089(18) -0.0046(18) C5 0.0256(19) 0.037(2) 0.029(2) -0.0001(17) -0.0018(16) 0.0014(18) C6 0.030(2) 0.024(2) 0.046(2) -0.0028(18) -0.0001(17) 0.0013(17) C7 0.044(3) 0.029(2) 0.070(3) -0.008(2) -0.001(2) 0.007(2) C8 0.043(3) 0.029(2) 0.073(3) -0.005(2) -0.016(2) 0.000(2) C9 0.069(3) 0.033(2) 0.060(3) 0.001(2) 0.012(3) -0.014(2) C10 0.0278(19) 0.033(2) 0.0276(19) 0.0005(17) 0.0046(15) -0.0001(17) C11 0.0292(19) 0.034(2) 0.032(2) 0.0037(18) 0.0047(16) -0.0022(18) C12 0.037(2) 0.029(2) 0.035(2) 0.0059(17) 0.0084(18) 0.0006(18) C13 0.0278(19) 0.036(2) 0.032(2) 0.0110(18) 0.0067(16) 0.0061(18) C14 0.0262(19) 0.035(2) 0.0281(19) 0.0038(17) 0.0048(15) -0.0004(17) C15 0.028(2) 0.041(2) 0.030(2) -0.0067(18) 0.0059(17) -0.0010(18) C16 0.063(3) 0.045(3) 0.065(3) 0.000(3) 0.031(3) 0.013(3) C17 0.070(4) 0.071(4) 0.042(3) -0.012(3) 0.010(3) 0.008(3) C18 0.033(3) 0.083(4) 0.095(4) -0.048(4) 0.016(3) -0.004(3) C19 0.0254(18) 0.0266(19) 0.0298(19) 0.0018(16) 0.0017(15) -0.0050(17) C20 0.029(2) 0.025(2) 0.030(2) -0.0007(16) 0.0033(16) -0.0042(16) C21 0.0243(19) 0.023(2) 0.048(2) 0.0067(18) 0.0042(17) 0.0020(16) C22 0.033(2) 0.035(2) 0.037(2) 0.0091(19) -0.0038(18) -0.0086(19) C23 0.032(2) 0.035(2) 0.0242(19) 0.0016(17) 0.0046(16) -0.0065(18) C24 0.0220(18) 0.030(2) 0.039(2) 0.0003(17) 0.0051(16) 0.0007(16) C25 0.033(2) 0.038(2) 0.045(3) 0.005(2) 0.0068(19) -0.0034(19) C26 0.028(2) 0.038(2) 0.061(3) 0.001(2) 0.011(2) 0.0042(18) C27 0.026(2) 0.047(3) 0.040(2) 0.009(2) -0.0039(18) -0.0046(19) C28 0.040(2) 0.031(2) 0.036(2) -0.0066(19) 0.0043(18) 0.0012(19) C29 0.049(3) 0.034(3) 0.063(3) -0.018(2) 0.023(2) -0.005(2) C30 0.035(2) 0.023(2) 0.067(3) -0.004(2) 0.007(2) 0.0012(18) C31 0.029(2) 0.027(2) 0.047(2) 0.0062(19) 0.0078(18) -0.0052(18) N3 0.0299(18) 0.039(2) 0.041(2) 0.0017(16) 0.0038(15) -0.0029(16) N4 0.0326(18) 0.037(2) 0.0394(19) 0.0001(16) 0.0020(15) 0.0048(16) C32 0.033(2) 0.038(2) 0.031(2) 0.0060(18) 0.0034(17) 0.0052(19) C33 0.030(2) 0.038(2) 0.045(2) -0.004(2) -0.0033(18) -0.0033(19) C34 0.032(2) 0.033(2) 0.041(2) -0.0006(18) -0.0012(18) 0.0066(18) C35 0.032(2) 0.032(2) 0.035(2) -0.0011(19) 0.0047(17) 0.0049(19) _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 Ce N1 2.676(3) . ? Ce C3 2.773(4) . ? Ce C21 2.777(4) . ? Ce C13 2.806(4) . ? Ce C12 2.815(4) . ? Ce C4 2.828(4) . ? Ce C22 2.834(4) . ? Ce C14 2.852(4) . ? Ce C11 2.862(4) . ? Ce C20 2.877(4) . ? Ce C2 2.890(4) . ? Ce C10 2.892(4) . ? Ce C23 2.916(4) . ? Ce C5 2.944(4) . ? Ce C19 2.983(4) . ? Ce C1 3.016(4) . ? N1 C31 1.335(5) . ? N1 C28 1.349(5) . ? N2 C28 1.321(5) . ? N2 C29 1.338(6) . ? C1 C2 1.413(5) . ? C1 C5 1.415(6) . ? C1 C6 1.518(6) . ? C2 C3 1.412(6) . ? C3 C4 1.397(6) . ? C4 C5 1.408(6) . ? C6 C7 1.537(6) . ? C6 C9 1.537(6) . ? C6 C8 1.539(6) . ? C10 C11 1.417(6) . ? C10 C14 1.424(5) . ? C10 C15 1.525(5) . ? C11 C12 1.406(6) . ? C12 C13 1.414(6) . ? C13 C14 1.398(6) . ? C15 C18 1.516(6) . ? C15 C17 1.523(6) . ? C15 C16 1.536(6) . ? C19 C20 1.412(5) . ? C19 C23 1.418(5) . ? C19 C24 1.522(5) . ? C20 C21 1.411(5) . ? C21 C22 1.398(6) . ? C22 C23 1.398(6) . ? C24 C26 1.528(6) . ? C24 C27 1.528(6) . ? C24 C25 1.547(5) . ? C29 C30 1.369(7) . ? C30 C31 1.392(6) . ? N3 C32 1.335(5) . ? N3 C35 1.338(5) . ? N4 C32 1.334(5) . ? N4 C33 1.335(5) . ? C33 C34 1.376(6) . ? C34 C35 1.373(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ce C3 121.91(11) . . ? N1 Ce C21 121.39(11) . . ? C3 Ce C21 83.00(12) . . ? N1 Ce C13 81.37(11) . . ? C3 Ce C13 139.31(12) . . ? C21 Ce C13 114.73(12) . . ? N1 Ce C12 79.53(11) . . ? C3 Ce C12 116.24(12) . . ? C21 Ce C12 140.12(12) . . ? C13 Ce C12 29.14(12) . . ? N1 Ce C4 98.08(11) . . ? C3 Ce C4 28.86(12) . . ? C21 Ce C4 81.33(12) . . ? C13 Ce C4 161.68(12) . . ? C12 Ce C4 132.60(12) . . ? N1 Ce C22 96.83(11) . . ? C3 Ce C22 83.08(12) . . ? C21 Ce C22 28.83(12) . . ? C13 Ce C22 130.38(12) . . ? C12 Ce C22 159.34(12) . . ? C4 Ce C22 67.93(12) . . ? N1 Ce C14 108.78(10) . . ? C3 Ce C14 122.75(12) . . ? C21 Ce C14 92.79(12) . . ? C13 Ce C14 28.59(11) . . ? C12 Ce C14 47.34(12) . . ? C4 Ce C14 151.30(12) . . ? C22 Ce C14 117.09(12) . . ? N1 Ce C11 105.88(11) . . ? C3 Ce C11 92.33(12) . . ? C21 Ce C11 126.83(12) . . ? C13 Ce C11 47.31(11) . . ? C12 Ce C11 28.65(11) . . ? C4 Ce C11 116.52(12) . . ? C22 Ce C11 155.53(12) . . ? C14 Ce C11 46.84(11) . . ? N1 Ce C20 110.98(10) . . ? C3 Ce C20 110.16(11) . . ? C21 Ce C20 28.84(11) . . ? C13 Ce C20 87.23(12) . . ? C12 Ce C20 115.22(12) . . ? C4 Ce C20 109.76(11) . . ? C22 Ce C20 46.88(11) . . ? C14 Ce C20 70.25(11) . . ? C11 Ce C20 114.28(11) . . ? N1 Ce C2 109.98(11) . . ? C3 Ce C2 28.79(11) . . ? C21 Ce C2 110.72(11) . . ? C13 Ce C2 116.08(12) . . ? C12 Ce C2 89.13(12) . . ? C4 Ce C2 46.75(12) . . ? C22 Ce C2 111.05(12) . . ? C14 Ce C2 111.97(11) . . ? C11 Ce C2 69.81(11) . . ? C20 Ce C2 135.27(11) . . ? N1 Ce C10 125.78(10) . . ? C3 Ce C10 95.49(12) . . ? C21 Ce C10 99.01(12) . . ? C13 Ce C10 47.54(11) . . ? C12 Ce C10 47.51(12) . . ? C4 Ce C10 124.30(12) . . ? C22 Ce C10 127.80(12) . . ? C14 Ce C10 28.70(10) . . ? C11 Ce C10 28.50(11) . . ? C20 Ce C10 86.77(11) . . ? C2 Ce C10 83.65(11) . . ? C31 N1 C28 115.2(3) . . ? C31 N1 Ce 129.0(3) . . ? C28 N1 Ce 115.3(3) . . ? C28 N2 C29 114.9(4) . . ? C2 C1 C5 106.3(4) . . ? C2 C1 C6 126.4(4) . . ? C5 C1 C6 125.6(4) . . ? C2 C1 Ce 71.3(2) . . ? C5 C1 Ce 73.5(2) . . ? C6 C1 Ce 131.9(2) . . ? C3 C2 C1 109.0(4) . . ? C3 C2 Ce 71.0(2) . . ? C1 C2 Ce 81.2(2) . . ? C4 C3 C2 107.8(4) . . ? C4 C3 Ce 77.8(2) . . ? C2 C3 Ce 80.2(2) . . ? C3 C4 C5 108.0(4) . . ? C3 C4 Ce 73.4(2) . . ? C5 C4 Ce 80.5(2) . . ? C4 C5 C1 108.9(4) . . ? C4 C5 Ce 71.3(2) . . ? C1 C5 Ce 79.1(2) . . ? C1 C6 C7 111.6(3) . . ? C1 C6 C9 113.1(4) . . ? C7 C6 C9 108.2(4) . . ? C1 C6 C8 107.5(3) . . ? C7 C6 C8 108.4(4) . . ? C9 C6 C8 107.8(4) . . ? C11 C10 C14 106.2(3) . . ? C11 C10 C15 127.7(3) . . ? C14 C10 C15 125.6(4) . . ? C11 C10 Ce 74.6(2) . . ? C14 C10 Ce 74.1(2) . . ? C15 C10 Ce 122.8(3) . . ? C12 C11 C10 109.2(4) . . ? C12 C11 Ce 73.8(2) . . ? C10 C11 Ce 76.9(2) . . ? C11 C12 C13 107.6(4) . . ? C11 C12 Ce 77.5(2) . . ? C13 C12 Ce 75.1(2) . . ? C14 C13 C12 108.1(3) . . ? C14 C13 Ce 77.6(2) . . ? C12 C13 Ce 75.8(2) . . ? C13 C14 C10 109.0(4) . . ? C13 C14 Ce 73.8(2) . . ? C10 C14 Ce 77.2(2) . . ? C18 C15 C17 109.0(4) . . ? C18 C15 C10 112.0(4) . . ? C17 C15 C10 109.1(4) . . ? C18 C15 C16 108.5(4) . . ? C17 C15 C16 106.9(4) . . ? C10 C15 C16 111.3(3) . . ? C20 C19 C23 106.0(3) . . ? C20 C19 C24 127.3(3) . . ? C23 C19 C24 125.5(3) . . ? C20 C19 Ce 71.9(2) . . ? C23 C19 Ce 73.4(2) . . ? C24 C19 Ce 129.3(3) . . ? C21 C20 C19 108.8(3) . . ? C21 C20 Ce 71.6(2) . . ? C19 C20 Ce 80.3(2) . . ? C22 C21 C20 108.0(4) . . ? C22 C21 Ce 77.9(2) . . ? C20 C21 Ce 79.5(2) . . ? C21 C22 C23 107.7(4) . . ? C21 C22 Ce 73.3(2) . . ? C23 C22 Ce 79.2(2) . . ? C22 C23 C19 109.4(4) . . ? C22 C23 Ce 72.7(2) . . ? C19 C23 Ce 78.8(2) . . ? C19 C24 C26 111.3(3) . . ? C19 C24 C27 112.1(3) . . ? C26 C24 C27 109.6(4) . . ? C19 C24 C25 107.4(3) . . ? C26 C24 C25 107.7(3) . . ? C27 C24 C25 108.5(3) . . ? N2 C28 N1 128.0(4) . . ? N2 C29 C30 123.1(4) . . ? C29 C30 C31 117.0(4) . . ? N1 C31 C30 121.8(4) . . ? C32 N3 C35 115.5(4) . . ? C32 N4 C33 115.3(4) . . ? N4 C32 N3 127.1(4) . . ? N4 C33 C34 122.9(4) . . ? C35 C34 C33 116.7(4) . . ? N3 C35 C34 122.5(4) . . ? #===END data_(Ce,SiMe~3~,pyrimidine) _database_code_depnum_ccdc_archive 'CCDC 223535' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H43 Ce N2 Si3' _chemical_formula_weight 632.03 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' Si Si 0.0817 0.0704 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.6932(8) _cell_length_b 17.8896(6) _cell_length_c 22.5040(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6317.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 41733 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method ? _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 1.572 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 41733 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5975 _reflns_number_gt 4069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. One Me~3~SiCp group has been found disordered over two positions sharing two C atoms of the Cp moiety and one terminal C atom, which have been refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters, with some restraints on bond lengths and displacement parameters for the disordered atoms. The H atoms were introduced at calculated positions, except in the disordered parts, and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0362P)^2^+12.1182P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5975 _refine_ls_number_parameters 363 _refine_ls_number_restraints 83 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.813 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.107 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 Ce Ce 0.558595(17) 0.800661(14) 0.091322(13) 0.02395(10) Uani 1 1 d . A . Si1 Si 0.51760(10) 0.80785(8) -0.09957(7) 0.0317(4) Uani 1 1 d . A . Si2 Si 0.49648(10) 0.58275(8) 0.13334(7) 0.0309(4) Uani 1 1 d . . . N1 N 0.6759(3) 0.8978(2) 0.0516(2) 0.0323(11) Uani 1 1 d . A . N2 N 0.8105(3) 0.9282(3) 0.0092(2) 0.0347(11) Uani 1 1 d . A . C1 C 0.4786(3) 0.8242(3) -0.0231(3) 0.0281(12) Uani 1 1 d . . . C2 C 0.4211(3) 0.7800(3) 0.0115(3) 0.0333(14) Uani 1 1 d . A . H2 H 0.4074 0.7303 0.0041 0.040 Uiso 1 1 calc R . . C3 C 0.3885(4) 0.8229(3) 0.0582(3) 0.0403(15) Uani 1 1 d . A . H3 H 0.3501 0.8068 0.0869 0.048 Uiso 1 1 calc R . . C4 C 0.4242(4) 0.8951(3) 0.0540(3) 0.0523(19) Uani 1 1 d . A . H4 H 0.4132 0.9353 0.0791 0.063 Uiso 1 1 calc R . . C5 C 0.4791(4) 0.8951(3) 0.0053(3) 0.0405(16) Uani 1 1 d . A . H5 H 0.5115 0.9358 -0.0069 0.049 Uiso 1 1 calc R . . C6 C 0.6201(4) 0.8588(4) -0.1121(3) 0.0479(17) Uani 1 1 d . . . H6A H 0.6139 0.9099 -0.0999 0.072 Uiso 1 1 calc R A . H6B H 0.6345 0.8570 -0.1535 0.072 Uiso 1 1 calc R . . H6C H 0.6646 0.8355 -0.0893 0.072 Uiso 1 1 calc R . . C7 C 0.5293(4) 0.7070(3) -0.1173(3) 0.0415(15) Uani 1 1 d . . . H7A H 0.5768 0.6868 -0.0958 0.062 Uiso 1 1 calc R A . H7B H 0.5387 0.7011 -0.1592 0.062 Uiso 1 1 calc R . . H7C H 0.4782 0.6810 -0.1061 0.062 Uiso 1 1 calc R . . C8 C 0.4356(4) 0.8486(4) -0.1507(3) 0.0468(16) Uani 1 1 d . . . H8A H 0.3805 0.8289 -0.1408 0.070 Uiso 1 1 calc R A . H8B H 0.4493 0.8356 -0.1910 0.070 Uiso 1 1 calc R . . H8C H 0.4351 0.9020 -0.1466 0.070 Uiso 1 1 calc R . . C9 C 0.5769(3) 0.6439(3) 0.0959(3) 0.0278(12) Uani 1 1 d . A . C10 C 0.5800(3) 0.6626(3) 0.0340(2) 0.0268(12) Uani 1 1 d . A . H10 H 0.5384 0.6513 0.0060 0.032 Uiso 1 1 calc R . . C11 C 0.6564(3) 0.7008(3) 0.0227(2) 0.0268(11) Uani 1 1 d . A . H11 H 0.6736 0.7196 -0.0139 0.032 Uiso 1 1 calc R . . C12 C 0.7027(3) 0.7059(3) 0.0764(2) 0.0295(13) Uani 1 1 d . A . H12 H 0.7554 0.7287 0.0816 0.035 Uiso 1 1 calc R . . C13 C 0.6544(3) 0.6702(3) 0.1201(3) 0.0305(13) Uani 1 1 d . A . H13 H 0.6709 0.6646 0.1596 0.037 Uiso 1 1 calc R . . C14 C 0.4838(4) 0.4958(3) 0.0882(3) 0.0482(17) Uani 1 1 d . A . H14A H 0.5374 0.4700 0.0861 0.072 Uiso 1 1 calc R . . H14B H 0.4654 0.5087 0.0489 0.072 Uiso 1 1 calc R . . H14C H 0.4421 0.4640 0.1065 0.072 Uiso 1 1 calc R . . C15 C 0.5380(4) 0.5586(3) 0.2083(3) 0.0442(16) Uani 1 1 d . A . H15A H 0.5933 0.5362 0.2045 0.066 Uiso 1 1 calc R . . H15B H 0.4999 0.5240 0.2272 0.066 Uiso 1 1 calc R . . H15C H 0.5422 0.6032 0.2319 0.066 Uiso 1 1 calc R . . C16 C 0.3894(4) 0.6273(3) 0.1379(3) 0.0471(17) Uani 1 1 d . A . H16A H 0.3489 0.5918 0.1529 0.071 Uiso 1 1 calc R . . H16B H 0.3721 0.6434 0.0990 0.071 Uiso 1 1 calc R . . H16C H 0.3919 0.6697 0.1640 0.071 Uiso 1 1 calc R . . Si3A Si 0.72971(18) 0.84940(19) 0.23167(14) 0.0321(10) Uani 0.522(5) 1 d P A 1 C18A C 0.5736(6) 0.9135(5) 0.1829(5) 0.023(3) Uani 0.522(5) 1 d PDU A 1 C19A C 0.4874(6) 0.9047(5) 0.1764(5) 0.043(3) Uani 0.522(5) 1 d PDU A 1 C21A C 0.5539(6) 0.7959(5) 0.2115(5) 0.030(2) Uani 0.522(5) 1 d PDU A 1 C22A C 0.7601(8) 0.7551(7) 0.2640(6) 0.046(3) Uani 0.522(5) 1 d PU A 1 C23A C 0.7317(9) 0.9189(8) 0.2959(7) 0.052(4) Uani 0.522(5) 1 d PU A 1 Si3B Si 0.7256(2) 0.9053(2) 0.22906(15) 0.0286(11) Uiso 0.478(5) 1 d PD A 2 C18B C 0.5985(7) 0.7831(5) 0.2198(5) 0.027(3) Uani 0.478(5) 1 d PDU A 2 C19B C 0.5124(7) 0.7722(5) 0.2131(6) 0.038(3) Uani 0.478(5) 1 d PDU A 2 C21B C 0.5427(6) 0.8938(5) 0.1928(6) 0.030(3) Uani 0.478(5) 1 d PDU A 2 C22B C 0.7200(7) 1.0092(6) 0.2231(6) 0.037(3) Uani 0.478(5) 1 d PU A 2 C23B C 0.7370(10) 0.8812(9) 0.3096(7) 0.046(4) Uani 0.478(5) 1 d PU A 2 C17 C 0.6208(3) 0.8539(3) 0.2047(2) 0.0331(13) Uani 1 1 d DU . . C20 C 0.4765(4) 0.8368(4) 0.1973(3) 0.0505(17) Uani 1 1 d DU A . C24 C 0.8143(4) 0.8725(4) 0.1796(3) 0.0515(18) Uani 1 1 d . . . C25 C 0.7504(4) 0.8812(3) 0.0259(3) 0.0308(13) Uani 1 1 d . . . H25 H 0.7610 0.8307 0.0191 0.037 Uiso 1 1 calc R A . C26 C 0.7930(4) 1.0004(3) 0.0172(3) 0.0403(15) Uani 1 1 d . . . H26 H 0.8332 1.0356 0.0055 0.048 Uiso 1 1 calc R A . C27 C 0.7179(4) 1.0249(3) 0.0422(3) 0.0466(17) Uani 1 1 d . A . H27 H 0.7064 1.0755 0.0474 0.056 Uiso 1 1 calc R . . C28 C 0.6609(4) 0.9708(3) 0.0591(3) 0.0468(17) Uani 1 1 d . . . H28 H 0.6097 0.9854 0.0763 0.056 Uiso 1 1 calc R A . 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 Ce 0.02360(15) 0.02232(14) 0.02594(16) -0.00459(13) 0.00527(14) -0.00142(13) Si1 0.0289(8) 0.0372(8) 0.0290(9) 0.0096(7) 0.0002(7) -0.0017(7) Si2 0.0375(9) 0.0280(7) 0.0272(9) 0.0047(6) 0.0043(7) -0.0021(7) N1 0.029(2) 0.026(2) 0.042(3) -0.003(2) 0.008(2) -0.004(2) N2 0.033(3) 0.036(3) 0.035(3) -0.001(2) 0.004(2) -0.008(2) C1 0.020(3) 0.034(3) 0.031(3) 0.013(2) 0.001(2) 0.006(2) C2 0.030(3) 0.042(3) 0.028(3) 0.009(2) -0.003(2) 0.001(2) C3 0.025(3) 0.058(4) 0.038(4) 0.010(3) 0.009(3) 0.009(3) C4 0.056(4) 0.037(3) 0.064(5) 0.001(3) 0.019(4) 0.029(3) C5 0.038(3) 0.030(3) 0.053(4) 0.010(3) 0.013(3) 0.007(3) C6 0.039(4) 0.064(4) 0.041(4) 0.008(3) 0.009(3) -0.005(3) C7 0.055(4) 0.047(3) 0.023(3) 0.004(3) -0.002(3) -0.001(3) C8 0.045(4) 0.060(4) 0.035(4) 0.020(3) -0.001(3) 0.004(3) C9 0.031(3) 0.025(2) 0.027(3) 0.002(2) 0.001(3) 0.003(2) C10 0.032(3) 0.022(2) 0.026(3) -0.001(2) 0.000(2) 0.000(2) C11 0.031(3) 0.022(2) 0.028(3) 0.002(2) 0.008(2) 0.006(2) C12 0.025(3) 0.028(3) 0.036(3) 0.002(2) -0.001(2) -0.003(2) C13 0.035(3) 0.029(3) 0.028(3) 0.005(2) -0.010(3) 0.002(2) C14 0.050(4) 0.039(3) 0.055(5) -0.004(3) 0.013(4) -0.012(3) C15 0.056(4) 0.034(3) 0.043(4) 0.010(3) 0.007(3) 0.001(3) C16 0.044(4) 0.040(3) 0.058(5) 0.009(3) 0.009(3) -0.008(3) Si3A 0.0239(16) 0.046(2) 0.0261(18) -0.0035(14) -0.0044(13) -0.0006(13) C18A 0.031(4) 0.019(4) 0.019(4) -0.002(3) -0.009(4) -0.002(4) C19A 0.045(5) 0.048(5) 0.036(5) -0.010(4) 0.005(4) 0.010(4) C21A 0.045(5) 0.023(4) 0.021(4) 0.003(3) 0.006(4) 0.005(4) C22A 0.044(5) 0.048(5) 0.047(5) 0.006(4) -0.005(4) -0.003(4) C23A 0.050(5) 0.054(5) 0.052(6) -0.012(4) -0.004(4) 0.000(4) C18B 0.035(5) 0.027(4) 0.018(4) 0.000(3) 0.000(4) 0.012(4) C19B 0.048(5) 0.039(5) 0.027(5) -0.002(4) 0.005(4) -0.009(4) C21B 0.038(5) 0.025(5) 0.027(5) 0.001(4) 0.004(4) 0.004(4) C22B 0.037(5) 0.038(5) 0.036(5) -0.006(4) -0.003(4) -0.004(4) C23B 0.044(5) 0.052(5) 0.041(6) 0.000(4) -0.007(4) -0.002(4) C17 0.026(3) 0.049(3) 0.023(3) 0.001(3) -0.002(2) 0.005(3) C20 0.037(3) 0.086(4) 0.029(3) -0.009(3) 0.006(3) 0.000(3) C24 0.032(3) 0.066(4) 0.056(5) -0.014(4) 0.012(3) -0.006(3) C25 0.034(3) 0.026(3) 0.033(4) -0.006(2) 0.001(3) 0.000(2) C26 0.040(3) 0.032(3) 0.049(4) 0.000(3) 0.003(3) -0.012(3) C27 0.050(4) 0.026(3) 0.064(5) -0.010(3) 0.007(4) -0.013(3) C28 0.047(4) 0.027(3) 0.066(5) -0.010(3) 0.020(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce N1 2.684(4) . ? Ce C21A 2.706(11) . ? Ce C20 2.787(6) . ? Ce C3 2.800(6) . ? Ce C10 2.806(5) . ? Ce C11 2.816(5) . ? Ce C9 2.820(5) . ? Ce C4 2.830(6) . ? Ce C2 2.832(6) . ? Ce C21B 2.837(13) . ? Ce C12 2.846(5) . ? Ce C13 2.851(5) . ? Ce C5 2.856(6) . ? Ce C19B 2.881(12) . ? Ce C17 2.893(6) . ? Ce C1 2.895(5) . ? Ce C19A 2.895(11) . ? Ce C18A 2.896(11) . ? Ce C18B 2.975(13) . ? Si1 C1 1.851(6) . ? Si1 C7 1.857(6) . ? Si1 C6 1.870(6) . ? Si1 C8 1.874(6) . ? Si2 C15 1.860(6) . ? Si2 C16 1.863(6) . ? Si2 C14 1.868(6) . ? Si2 C9 1.871(5) . ? N1 C25 1.337(7) . ? N1 C28 1.338(7) . ? N2 C25 1.319(7) . ? N2 C26 1.333(7) . ? C1 C5 1.418(8) . ? C1 C2 1.431(7) . ? C2 C3 1.398(8) . ? C3 C4 1.411(9) . ? C4 C5 1.395(9) . ? C9 C13 1.413(7) . ? C9 C10 1.433(8) . ? C10 C11 1.403(7) . ? C11 C12 1.412(7) . ? C12 C13 1.397(8) . ? Si3A C17 1.815(5) . ? Si3A C24 1.818(7) . ? Si3A C22A 1.898(12) . ? Si3A C23A 1.907(14) . ? C18A C19A 1.371(9) . ? C18A C17 1.388(8) . ? C19A C20 1.314(8) . ? C21A C20 1.454(8) . ? C21A C17 1.484(8) . ? Si3B C22B 1.867(12) . ? Si3B C23B 1.873(16) . ? Si3B C24 1.876(7) . ? Si3B C17 1.962(5) . ? C18B C17 1.359(8) . ? C18B C19B 1.373(9) . ? C19B C20 1.335(9) . ? C21B C17 1.444(8) . ? C21B C20 1.459(9) . ? C26 C27 1.378(8) . ? C27 C28 1.372(8) . ? 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 N1 Ce C21A 111.8(2) . . ? N1 Ce C20 116.86(17) . . ? C21A Ce C20 30.65(19) . . ? N1 Ce C3 118.24(16) . . ? C21A Ce C3 104.2(2) . . ? C20 Ce C3 75.76(18) . . ? N1 Ce C10 109.53(14) . . ? C21A Ce C10 115.8(2) . . ? C20 Ce C10 130.76(18) . . ? C3 Ce C10 96.73(17) . . ? N1 Ce C11 81.62(14) . . ? C21A Ce C11 122.9(2) . . ? C20 Ce C11 150.27(17) . . ? C3 Ce C11 117.64(17) . . ? C10 Ce C11 28.89(14) . . ? N1 Ce C9 125.84(14) . . ? C21A Ce C9 86.3(2) . . ? C20 Ce C9 104.27(18) . . ? C3 Ce C9 104.38(17) . . ? C10 Ce C9 29.51(15) . . ? C11 Ce C9 48.23(15) . . ? N1 Ce C4 91.48(17) . . ? C21A Ce C4 107.2(2) . . ? C20 Ce C4 76.8(2) . . ? C3 Ce C4 29.03(18) . . ? C10 Ce C4 118.59(19) . . ? C11 Ce C4 128.48(18) . . ? C9 Ce C4 132.88(18) . . ? N1 Ce C2 113.34(15) . . ? C21A Ce C2 127.5(2) . . ? C20 Ce C2 102.74(17) . . ? C3 Ce C2 28.74(17) . . ? C10 Ce C2 71.64(16) . . ? C11 Ce C2 89.13(16) . . ? C9 Ce C2 88.34(16) . . ? C4 Ce C2 47.31(19) . . ? N1 Ce C21B 87.0(2) . . ? C21A Ce C21B 38.0(3) . . ? C20 Ce C21B 30.05(19) . . ? C3 Ce C21B 92.7(2) . . ? C10 Ce C21B 153.8(2) . . ? C11 Ce C21B 149.5(2) . . ? C9 Ce C21B 124.3(2) . . ? C4 Ce C21B 79.8(2) . . ? C2 Ce C21B 121.3(2) . . ? N1 Ce C12 78.54(14) . . ? C21A Ce C12 96.9(2) . . ? C20 Ce C12 127.35(17) . . ? C3 Ce C12 144.16(17) . . ? C10 Ce C12 47.63(15) . . ? C11 Ce C12 28.87(15) . . ? C9 Ce C12 48.01(15) . . ? C4 Ce C12 155.88(18) . . ? C2 Ce C12 116.91(16) . . ? C21B Ce C12 121.0(2) . . ? N1 Ce C13 104.11(15) . . ? C21A Ce C13 76.2(2) . . ? C20 Ce C13 103.83(18) . . ? C3 Ce C13 132.82(17) . . ? C10 Ce C13 47.22(16) . . ? C11 Ce C13 47.00(16) . . ? C9 Ce C13 28.85(15) . . ? C4 Ce C13 161.68(18) . . ? C2 Ce C13 116.05(16) . . ? C21B Ce C13 110.1(2) . . ? C12 Ce C13 28.39(15) . . ? C1 Si1 C7 112.7(3) . . ? C1 Si1 C6 110.3(3) . . ? C7 Si1 C6 110.9(3) . . ? C1 Si1 C8 106.4(3) . . ? C7 Si1 C8 108.3(3) . . ? C6 Si1 C8 108.0(3) . . ? C15 Si2 C16 111.5(3) . . ? C15 Si2 C14 109.7(3) . . ? C16 Si2 C14 106.9(3) . . ? C15 Si2 C9 107.9(3) . . ? C16 Si2 C9 112.5(2) . . ? C14 Si2 C9 108.3(3) . . ? C25 N1 C28 115.2(5) . . ? C25 N1 Ce 126.8(3) . . ? C28 N1 Ce 118.0(4) . . ? C25 N2 C26 115.6(5) . . ? C5 C1 C2 104.7(5) . . ? C5 C1 Si1 123.9(4) . . ? C2 C1 Si1 128.8(4) . . ? C5 C1 Ce 74.2(3) . . ? C2 C1 Ce 73.1(3) . . ? Si1 C1 Ce 131.4(2) . . ? C3 C2 C1 109.6(5) . . ? C3 C2 Ce 74.3(3) . . ? C1 C2 Ce 78.0(3) . . ? C2 C3 C4 107.9(5) . . ? C2 C3 Ce 76.9(3) . . ? C4 C3 Ce 76.7(4) . . ? C5 C4 C3 107.3(6) . . ? C5 C4 Ce 76.9(3) . . ? C3 C4 Ce 74.3(3) . . ? C4 C5 C1 110.5(5) . . ? C4 C5 Ce 74.8(4) . . ? C1 C5 Ce 77.2(3) . . ? C13 C9 C10 105.6(5) . . ? C13 C9 Si2 127.0(4) . . ? C10 C9 Si2 126.7(4) . . ? C13 C9 Ce 76.8(3) . . ? C10 C9 Ce 74.7(3) . . ? Si2 C9 Ce 121.9(2) . . ? C11 C10 C9 108.6(5) . . ? C11 C10 Ce 75.9(3) . . ? C9 C10 Ce 75.8(3) . . ? C10 C11 C12 108.4(5) . . ? C10 C11 Ce 75.2(3) . . ? C12 C11 Ce 76.7(3) . . ? C13 C12 C11 107.1(5) . . ? C13 C12 Ce 76.0(3) . . ? C11 C12 Ce 74.4(3) . . ? C12 C13 C9 110.3(5) . . ? C12 C13 Ce 75.6(3) . . ? C9 C13 Ce 74.4(3) . . ? C17 Si3A C24 117.5(3) . . ? C17 Si3A C22A 113.9(4) . . ? C24 Si3A C22A 105.4(5) . . ? C17 Si3A C23A 103.9(5) . . ? C24 Si3A C23A 109.2(5) . . ? C22A Si3A C23A 106.6(7) . . ? C19A C18A C17 118.5(8) . . ? C19A C18A Ce 76.3(6) . . ? C17 C18A Ce 76.0(5) . . ? C20 C19A C18A 101.3(8) . . ? C20 C19A Ce 72.1(5) . . ? C18A C19A Ce 76.3(6) . . ? C20 C21A C17 102.5(6) . . ? C20 C21A Ce 77.7(5) . . ? C17 C21A Ce 81.7(5) . . ? Si3A C22A Ce 53.7(3) . . ? C22B Si3B C23B 107.7(6) . . ? C22B Si3B C24 107.7(5) . . ? C23B Si3B C24 115.6(6) . . ? C22B Si3B C17 114.0(4) . . ? C23B Si3B C17 104.1(5) . . ? C24 Si3B C17 108.0(3) . . ? C17 C18B C19B 111.1(8) . . ? C17 C18B Ce 73.3(5) . . ? C19B C18B Ce 72.6(7) . . ? C20 C19B C18B 108.7(9) . . ? C20 C19B Ce 72.5(6) . . ? C18B C19B Ce 80.3(8) . . ? C17 C21B C20 104.3(7) . . ? C17 C21B Ce 77.6(6) . . ? C20 C21B Ce 73.1(6) . . ? Si3B C22B Ce 51.2(3) . . ? C18B C17 C21B 106.7(7) . . ? C18A C17 C21A 101.3(6) . . ? C18A C17 Si3A 130.9(5) . . ? C21A C17 Si3A 126.9(5) . . ? C18B C17 Si3B 125.7(6) . . ? C21B C17 Si3B 122.2(5) . . ? C18B C17 Ce 80.0(6) . . ? C18A C17 Ce 76.2(5) . . ? C21B C17 Ce 73.3(6) . . ? C21A C17 Ce 67.8(5) . . ? Si3A C17 Ce 126.7(3) . . ? Si3B C17 Ce 133.2(3) . . ? C19A C20 C21A 115.8(7) . . ? C19B C20 C21B 108.9(7) . . ? C19A C20 Ce 81.3(6) . . ? C19B C20 Ce 80.3(6) . . ? C21A C20 Ce 71.6(5) . . ? C21B C20 Ce 76.9(6) . . ? N2 C25 N1 127.3(5) . . ? N2 C26 C27 122.7(5) . . ? C28 C27 C26 116.5(5) . . ? N1 C28 C27 122.6(6) . . ? #===END data_(U,SiMe~3~,pyrimidine) _database_code_depnum_ccdc_archive 'CCDC 223536' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H43 N2 Si3 U' _chemical_formula_weight 729.94 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4253(10) _cell_length_b 17.4702(18) _cell_length_c 15.5095(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.699(6) _cell_angle_gamma 90.00 _cell_volume 3095.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20594 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method ? _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 5.378 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.251 _exptl_absorpt_correction_T_max 0.650 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 293(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 20594 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.1135 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5847 _reflns_number_gt 3630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0120P)^2^+0.2968P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5847 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.723 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.165 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 U U 0.16946(3) 0.085112(19) 0.72329(2) 0.03051(11) Uani 1 1 d . . . Si1 Si -0.1887(2) 0.03102(14) 0.78784(18) 0.0361(6) Uani 1 1 d . . . Si2 Si 0.3402(2) -0.12195(14) 0.75645(16) 0.0356(6) Uani 1 1 d . . . Si3 Si 0.3838(2) 0.20536(16) 0.54251(17) 0.0413(7) Uani 1 1 d . . . N1 N 0.0428(6) 0.1761(4) 0.6181(5) 0.0339(18) Uani 1 1 d . . . N2 N -0.0199(6) 0.3055(4) 0.5929(5) 0.043(2) Uani 1 1 d . . . C1 C -0.0428(7) 0.0726(5) 0.8173(6) 0.034(2) Uani 1 1 d . . . C2 C 0.0459(7) 0.0386(5) 0.8688(6) 0.035(2) Uani 1 1 d . . . H2 H 0.0514 -0.0132 0.8821 0.042 Uiso 1 1 calc R . . C3 C 0.1239(7) 0.0951(5) 0.8966(6) 0.037(2) Uani 1 1 d . . . H3 H 0.1900 0.0867 0.9308 0.044 Uiso 1 1 calc R . . C4 C 0.0875(7) 0.1664(6) 0.8650(6) 0.042(2) Uani 1 1 d . . . H4 H 0.1237 0.2134 0.8741 0.050 Uiso 1 1 calc R . . C5 C -0.0153(7) 0.1523(5) 0.8164(6) 0.037(2) Uani 1 1 d . . . H5 H -0.0590 0.1896 0.7879 0.045 Uiso 1 1 calc R . . C6 C -0.2894(7) 0.0569(6) 0.8770(6) 0.050(3) Uani 1 1 d . . . H6A H -0.2605 0.0355 0.9302 0.075 Uiso 1 1 calc R . . H6B H -0.3661 0.0369 0.8647 0.075 Uiso 1 1 calc R . . H6C H -0.2936 0.1116 0.8821 0.075 Uiso 1 1 calc R . . C7 C -0.2472(7) 0.0687(5) 0.6848(6) 0.041(2) Uani 1 1 d . . . H7A H -0.2392 0.1234 0.6840 0.061 Uiso 1 1 calc R . . H7B H -0.3284 0.0553 0.6790 0.061 Uiso 1 1 calc R . . H7C H -0.2045 0.0470 0.6378 0.061 Uiso 1 1 calc R . . C8 C -0.1782(7) -0.0758(5) 0.7838(6) 0.040(2) Uani 1 1 d . . . H8A H -0.1393 -0.0910 0.7320 0.061 Uiso 1 1 calc R . . H8B H -0.2554 -0.0975 0.7844 0.061 Uiso 1 1 calc R . . H8C H -0.1344 -0.0938 0.8330 0.061 Uiso 1 1 calc R . . C9 C 0.2329(6) -0.0678(4) 0.6886(5) 0.029(2) Uani 1 1 d . . . C10 C 0.1082(7) -0.0683(5) 0.7011(6) 0.035(2) Uani 1 1 d . . . H10 H 0.0701 -0.0907 0.7473 0.042 Uiso 1 1 calc R . . C11 C 0.0530(7) -0.0293(5) 0.6322(6) 0.032(2) Uani 1 1 d . . . H11 H -0.0268 -0.0204 0.6253 0.039 Uiso 1 1 calc R . . C12 C 0.1414(7) -0.0066(5) 0.5760(6) 0.033(2) Uani 1 1 d . . . H12 H 0.1300 0.0197 0.5245 0.040 Uiso 1 1 calc R . . C13 C 0.2490(7) -0.0296(5) 0.6095(6) 0.036(2) Uani 1 1 d . . . H13 H 0.3208 -0.0211 0.5836 0.043 Uiso 1 1 calc R . . C14 C 0.3198(7) -0.0990(6) 0.8730(6) 0.050(3) Uani 1 1 d . . . H14A H 0.2391 -0.1060 0.8876 0.074 Uiso 1 1 calc R . . H14B H 0.3420 -0.0469 0.8836 0.074 Uiso 1 1 calc R . . H14C H 0.3677 -0.1325 0.9076 0.074 Uiso 1 1 calc R . . C15 C 0.4919(7) -0.0991(5) 0.7224(6) 0.039(2) Uani 1 1 d . . . H15A H 0.5442 -0.1385 0.7423 0.059 Uiso 1 1 calc R . . H15B H 0.5153 -0.0509 0.7467 0.059 Uiso 1 1 calc R . . H15C H 0.4944 -0.0962 0.6606 0.059 Uiso 1 1 calc R . . C16 C 0.3160(7) -0.2262(5) 0.7409(7) 0.050(3) Uani 1 1 d . . . H16A H 0.2433 -0.2407 0.7667 0.074 Uiso 1 1 calc R . . H16B H 0.3790 -0.2542 0.7677 0.074 Uiso 1 1 calc R . . H16C H 0.3133 -0.2376 0.6804 0.074 Uiso 1 1 calc R . . C17 C 0.3607(7) 0.1680(5) 0.6532(6) 0.036(2) Uani 1 1 d . . . C18 C 0.4095(7) 0.1018(5) 0.6905(6) 0.038(2) Uani 1 1 d . . . H18 H 0.4439 0.0620 0.6601 0.046 Uiso 1 1 calc R . . C19 C 0.3987(7) 0.1044(5) 0.7792(6) 0.040(2) Uani 1 1 d . . . H19 H 0.4220 0.0665 0.8178 0.048 Uiso 1 1 calc R . . C20 C 0.3468(7) 0.1740(5) 0.8005(6) 0.040(2) Uani 1 1 d . . . H20 H 0.3317 0.1913 0.8560 0.048 Uiso 1 1 calc R . . C21 C 0.3217(7) 0.2127(5) 0.7255(6) 0.033(2) Uani 1 1 d . . . H21 H 0.2853 0.2602 0.7220 0.040 Uiso 1 1 calc R . . C22 C 0.2896(7) 0.1553(6) 0.4584(6) 0.045(3) Uani 1 1 d . . . H22A H 0.2090 0.1689 0.4665 0.068 Uiso 1 1 calc R . . H22B H 0.2985 0.1009 0.4642 0.068 Uiso 1 1 calc R . . H22C H 0.3135 0.1708 0.4019 0.068 Uiso 1 1 calc R . . C23 C 0.5408(8) 0.1915(6) 0.5150(7) 0.058(3) Uani 1 1 d . . . H23A H 0.5561 0.2150 0.4603 0.088 Uiso 1 1 calc R . . H23B H 0.5577 0.1378 0.5117 0.088 Uiso 1 1 calc R . . H23C H 0.5894 0.2147 0.5586 0.088 Uiso 1 1 calc R . . C24 C 0.3518(8) 0.3114(5) 0.5456(6) 0.048(3) Uani 1 1 d . . . H24A H 0.2689 0.3192 0.5503 0.072 Uiso 1 1 calc R . . H24B H 0.3790 0.3349 0.4936 0.072 Uiso 1 1 calc R . . H24C H 0.3910 0.3339 0.5944 0.072 Uiso 1 1 calc R . . C25 C 0.0384(7) 0.2525(5) 0.6341(6) 0.039(2) Uani 1 1 d . . . H25 H 0.0832 0.2694 0.6809 0.046 Uiso 1 1 calc R . . C26 C -0.0828(7) 0.2814(6) 0.5240(6) 0.041(2) Uani 1 1 d . . . H26 H -0.1244 0.3169 0.4912 0.049 Uiso 1 1 calc R . . C27 C -0.0866(7) 0.2056(5) 0.5012(6) 0.040(2) Uani 1 1 d . . . H27 H -0.1310 0.1894 0.4539 0.048 Uiso 1 1 calc R . . C28 C -0.0228(7) 0.1537(5) 0.5504(6) 0.037(2) Uani 1 1 d . . . H28 H -0.0256 0.1021 0.5360 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02968(16) 0.02942(17) 0.03242(17) -0.0017(2) -0.00083(12) -0.0006(2) Si1 0.0285(14) 0.0346(14) 0.0451(17) 0.0001(13) -0.0015(12) -0.0003(12) Si2 0.0333(13) 0.0317(13) 0.0417(18) 0.0011(12) -0.0019(12) 0.0012(12) Si3 0.0421(15) 0.0476(17) 0.0342(16) 0.0011(13) 0.0035(13) -0.0027(13) N1 0.032(4) 0.033(5) 0.036(5) -0.003(4) -0.001(4) 0.004(3) N2 0.042(5) 0.041(5) 0.044(5) -0.001(4) -0.004(4) 0.004(4) C1 0.037(5) 0.029(6) 0.036(5) 0.005(4) 0.005(4) 0.003(4) C2 0.031(5) 0.036(6) 0.039(6) 0.004(5) 0.013(4) -0.008(4) C3 0.028(4) 0.040(6) 0.043(5) -0.003(5) 0.001(4) -0.002(5) C4 0.039(5) 0.051(7) 0.035(6) -0.021(5) 0.002(5) -0.011(5) C5 0.035(5) 0.030(5) 0.046(6) -0.005(5) 0.005(5) -0.004(4) C6 0.031(5) 0.062(7) 0.057(7) -0.004(5) 0.009(5) -0.010(5) C7 0.036(5) 0.035(6) 0.051(6) 0.000(5) -0.003(4) 0.006(4) C8 0.031(4) 0.032(5) 0.059(6) 0.005(6) -0.002(4) -0.007(5) C9 0.025(4) 0.026(5) 0.036(5) -0.006(4) -0.003(4) 0.001(4) C10 0.040(5) 0.027(6) 0.039(5) 0.001(4) 0.004(4) 0.000(4) C11 0.031(5) 0.028(5) 0.038(6) -0.006(4) -0.002(4) 0.002(4) C12 0.035(5) 0.030(5) 0.034(5) 0.002(4) -0.001(4) -0.007(4) C13 0.033(5) 0.038(5) 0.037(6) -0.010(4) 0.006(4) -0.005(4) C14 0.038(5) 0.060(8) 0.050(6) 0.011(6) 0.001(5) 0.004(5) C15 0.033(5) 0.047(7) 0.038(5) 0.000(5) -0.005(4) 0.008(4) C16 0.035(5) 0.046(6) 0.068(7) 0.003(5) -0.012(5) -0.001(5) C17 0.030(5) 0.032(5) 0.044(6) 0.007(5) 0.008(4) 0.000(4) C18 0.030(5) 0.040(7) 0.045(6) -0.002(5) -0.001(4) -0.002(4) C19 0.031(5) 0.037(6) 0.051(6) 0.009(5) -0.008(4) -0.008(4) C20 0.043(6) 0.045(6) 0.033(6) -0.001(5) 0.001(5) -0.013(5) C21 0.031(5) 0.027(5) 0.041(6) -0.008(4) -0.001(4) 0.002(4) C22 0.048(6) 0.051(6) 0.037(6) 0.006(5) 0.006(5) 0.001(5) C23 0.049(6) 0.078(8) 0.048(7) -0.005(6) 0.000(5) -0.012(6) C24 0.069(7) 0.040(6) 0.035(6) 0.008(5) 0.003(5) -0.007(5) C25 0.037(5) 0.033(6) 0.046(6) -0.007(5) -0.005(4) 0.000(5) C26 0.037(5) 0.046(6) 0.039(6) -0.001(5) 0.001(5) 0.005(5) C27 0.038(5) 0.047(6) 0.034(6) -0.002(5) -0.005(4) 0.008(5) C28 0.042(5) 0.033(5) 0.037(6) -0.006(5) 0.003(5) -0.009(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 U N1 2.688(7) . ? U C3 2.749(8) . ? U C19 2.770(8) . ? U C11 2.778(8) . ? U C4 2.788(8) . ? U C10 2.790(8) . ? U C2 2.797(8) . ? U C12 2.806(9) . ? U C18 2.810(8) . ? U C20 2.809(8) . ? U C9 2.822(8) . ? U C21 2.827(8) . ? U C5 2.827(8) . ? U C13 2.828(8) . ? U C17 2.848(8) . ? U C1 2.853(8) . ? Si1 C7 1.847(9) . ? Si1 C6 1.866(9) . ? Si1 C1 1.869(9) . ? Si1 C8 1.871(8) . ? Si2 C16 1.858(9) . ? Si2 C15 1.861(8) . ? Si2 C9 1.863(8) . ? Si2 C14 1.868(9) . ? Si3 C17 1.858(9) . ? Si3 C23 1.865(9) . ? Si3 C24 1.889(9) . ? Si3 C22 1.895(9) . ? N1 C28 1.341(10) . ? N1 C25 1.360(11) . ? N2 C25 1.303(11) . ? N2 C26 1.348(11) . ? C1 C2 1.414(11) . ? C1 C5 1.428(12) . ? C2 C3 1.394(11) . ? C3 C4 1.401(12) . ? C4 C5 1.408(12) . ? C9 C13 1.411(11) . ? C9 C10 1.441(11) . ? C10 C11 1.410(12) . ? C11 C12 1.399(11) . ? C12 C13 1.387(11) . ? C17 C18 1.406(11) . ? C17 C21 1.441(12) . ? C18 C19 1.383(12) . ? C19 C20 1.395(12) . ? C20 C21 1.372(12) . ? C26 C27 1.371(12) . ? C27 C28 1.386(12) . ? 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 N1 U C3 116.7(2) . . ? N1 U C19 128.2(2) . . ? C3 U C19 82.9(3) . . ? N1 U C11 82.3(2) . . ? C3 U C11 116.6(3) . . ? C19 U C11 133.8(3) . . ? N1 U C4 89.6(3) . . ? C3 U C4 29.3(3) . . ? C19 U C4 91.0(3) . . ? C11 U C4 127.2(3) . . ? N1 U C10 111.1(2) . . ? C3 U C10 97.5(3) . . ? C19 U C10 113.0(3) . . ? C11 U C10 29.3(2) . . ? C4 U C10 120.0(3) . . ? N1 U C2 112.9(2) . . ? C3 U C2 29.1(2) . . ? C19 U C2 105.5(3) . . ? C11 U C2 87.6(3) . . ? C4 U C2 48.3(3) . . ? C10 U C2 72.1(3) . . ? N1 U C12 77.8(2) . . ? C3 U C12 144.2(3) . . ? C19 U C12 115.0(3) . . ? C11 U C12 29.0(2) . . ? C4 U C12 153.7(2) . . ? C10 U C12 47.5(3) . . ? C2 U C12 115.9(3) . . ? N1 U C18 110.4(2) . . ? C3 U C18 111.5(3) . . ? C19 U C18 28.7(2) . . ? C11 U C18 116.4(3) . . ? C4 U C18 115.3(3) . . ? C10 U C18 108.7(2) . . ? C2 U C18 132.8(3) . . ? C12 U C18 90.8(3) . . ? N1 U C20 108.2(2) . . ? C3 U C20 72.1(3) . . ? C19 U C20 28.9(2) . . ? C11 U C20 162.4(3) . . ? C4 U C20 68.3(3) . . ? C10 U C20 139.7(3) . . ? C2 U C20 100.7(3) . . ? C12 U C20 137.5(2) . . ? C18 U C20 47.1(3) . . ? N1 U C9 125.6(2) . . ? C3 U C9 107.4(3) . . ? C19 U C9 86.0(2) . . ? C11 U C9 49.0(2) . . ? C4 U C9 136.2(3) . . ? C10 U C9 29.7(2) . . ? C2 U C9 90.7(3) . . ? C12 U C9 48.0(2) . . ? C18 U C9 79.1(2) . . ? C20 U C9 114.8(3) . . ? N1 U C21 82.4(2) . . ? C3 U C21 93.5(3) . . ? C19 U C21 47.2(3) . . ? C11 U C21 149.8(3) . . ? C4 U C21 78.5(3) . . ? C10 U C21 155.8(2) . . ? C2 U C21 122.4(3) . . ? C12 U C21 121.6(2) . . ? C18 U C21 47.1(2) . . ? C20 U C21 28.2(2) . . ? C9 U C21 126.1(2) . . ? C7 Si1 C6 109.6(4) . . ? C7 Si1 C1 112.7(4) . . ? C6 Si1 C1 106.3(4) . . ? C7 Si1 C8 110.5(4) . . ? C6 Si1 C8 107.9(4) . . ? C1 Si1 C8 109.8(4) . . ? C16 Si2 C15 108.1(4) . . ? C16 Si2 C9 109.2(4) . . ? C15 Si2 C9 109.8(4) . . ? C16 Si2 C14 108.4(5) . . ? C15 Si2 C14 110.9(4) . . ? C9 Si2 C14 110.4(4) . . ? C17 Si3 C23 108.3(4) . . ? C17 Si3 C24 106.9(4) . . ? C23 Si3 C24 108.7(5) . . ? C17 Si3 C22 112.8(4) . . ? C23 Si3 C22 108.8(4) . . ? C24 Si3 C22 111.2(4) . . ? C28 N1 C25 114.1(8) . . ? C28 N1 U 126.5(6) . . ? C25 N1 U 119.4(6) . . ? C25 N2 C26 115.6(8) . . ? C2 C1 C5 104.9(8) . . ? C2 C1 Si1 127.3(7) . . ? C5 C1 Si1 124.9(7) . . ? C2 C1 U 73.3(4) . . ? C5 C1 U 74.4(5) . . ? Si1 C1 U 131.8(4) . . ? C3 C2 C1 109.2(8) . . ? C3 C2 U 73.5(5) . . ? C1 C2 U 77.7(5) . . ? C2 C3 C4 109.6(8) . . ? C2 C3 U 77.4(5) . . ? C4 C3 U 76.9(5) . . ? C3 C4 C5 105.9(8) . . ? C3 C4 U 73.8(5) . . ? C5 C4 U 77.0(5) . . ? C4 C5 C1 110.4(9) . . ? C4 C5 U 73.9(5) . . ? C1 C5 U 76.5(5) . . ? C13 C9 C10 105.0(7) . . ? C13 C9 Si2 129.8(6) . . ? C10 C9 Si2 124.5(6) . . ? C13 C9 U 75.8(5) . . ? C10 C9 U 73.9(4) . . ? Si2 C9 U 122.8(4) . . ? C11 C10 C9 109.2(8) . . ? C11 C10 U 74.9(5) . . ? C9 C10 U 76.4(5) . . ? C12 C11 C10 106.8(7) . . ? C12 C11 U 76.6(5) . . ? C10 C11 U 75.8(5) . . ? C13 C12 C11 109.2(8) . . ? C13 C12 U 76.6(5) . . ? C11 C12 U 74.4(5) . . ? C12 C13 C9 109.8(7) . . ? C12 C13 U 74.9(5) . . ? C9 C13 U 75.3(5) . . ? C18 C17 C21 104.4(8) . . ? C18 C17 Si3 127.5(7) . . ? C21 C17 Si3 125.3(7) . . ? C18 C17 U 74.1(5) . . ? C21 C17 U 74.5(5) . . ? Si3 C17 U 130.5(4) . . ? C19 C18 C17 110.0(8) . . ? C19 C18 U 74.0(5) . . ? C17 C18 U 77.1(5) . . ? C18 C19 C20 108.0(8) . . ? C18 C19 U 77.3(5) . . ? C20 C19 U 77.1(5) . . ? C21 C20 C19 108.2(8) . . ? C21 C20 U 76.6(5) . . ? C19 C20 U 74.0(5) . . ? C20 C21 C17 109.3(8) . . ? C20 C21 U 75.2(5) . . ? C17 C21 U 76.1(5) . . ? N2 C25 N1 128.8(9) . . ? N2 C26 C27 121.4(9) . . ? C26 C27 C28 118.3(9) . . ? N1 C28 C27 121.8(9) . . ? #===END data_(Ce,Bu^t^,pyrazine) _database_code_depnum_ccdc_archive 'CCDC 223537' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H43 Ce N2' _chemical_formula_weight 583.79 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9926(4) _cell_length_b 8.4351(2) _cell_length_c 30.1082(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.049(2) _cell_angle_gamma 90.00 _cell_volume 2776.20(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18094 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent dark red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method ? _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 1.660 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.427 _exptl_absorpt_correction_T_max 0.808 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 18094 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5240 _reflns_number_gt 4233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0046P)^2^+1.6701P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5240 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.779 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.084 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 Ce Ce 0.904240(15) 0.926985(19) 0.132792(5) 0.02016(6) Uani 1 1 d . . . N1 N 0.7761(2) 1.1332(3) 0.07778(9) 0.0260(6) Uani 1 1 d . . . N2 N 0.6372(3) 1.3181(3) 0.01302(10) 0.0359(7) Uani 1 1 d . . . C1 C 1.1158(3) 1.0819(4) 0.09449(10) 0.0225(6) Uani 1 1 d . . . C2 C 1.0703(3) 0.9619(4) 0.06449(10) 0.0236(7) Uani 1 1 d . . . H2 H 1.0316 0.9789 0.0359 0.028 Uiso 1 1 calc R . . C3 C 1.0926(3) 0.8135(4) 0.08446(11) 0.0245(7) Uani 1 1 d . . . H3 H 1.0741 0.7156 0.0712 0.029 Uiso 1 1 calc R . . C4 C 1.1479(3) 0.8392(4) 0.12809(11) 0.0253(7) Uani 1 1 d . . . H4 H 1.1705 0.7615 0.1493 0.030 Uiso 1 1 calc R . . C5 C 1.1630(3) 1.0035(4) 0.13391(10) 0.0229(7) Uani 1 1 d . . . H5 H 1.1986 1.0528 0.1597 0.027 Uiso 1 1 calc R . . C6 C 1.1388(3) 1.2559(3) 0.08314(10) 0.0244(7) Uani 1 1 d . . . C7 C 1.1502(3) 1.3586(4) 0.12542(11) 0.0307(8) Uani 1 1 d . . . H7A H 1.1606 1.4675 0.1174 0.046 Uiso 1 1 calc R . . H7B H 1.2196 1.3245 0.1451 0.046 Uiso 1 1 calc R . . H7C H 1.0773 1.3481 0.1402 0.046 Uiso 1 1 calc R . . C8 C 1.0361(3) 1.3233(4) 0.04967(11) 0.0298(8) Uani 1 1 d . . . H8A H 0.9617 1.3301 0.0637 0.045 Uiso 1 1 calc R . . H8B H 1.0237 1.2549 0.0241 0.045 Uiso 1 1 calc R . . H8C H 1.0587 1.4271 0.0403 0.045 Uiso 1 1 calc R . . C9 C 1.2595(3) 1.2658(4) 0.06168(12) 0.0321(8) Uani 1 1 d . . . H9A H 1.2768 1.3746 0.0554 0.048 Uiso 1 1 calc R . . H9B H 1.2522 1.2060 0.0344 0.048 Uiso 1 1 calc R . . H9C H 1.3247 1.2230 0.0819 0.048 Uiso 1 1 calc R . . C10 C 0.9611(3) 0.9467(4) 0.22780(10) 0.0233(6) Uani 1 1 d . . . C11 C 0.9943(3) 1.0970(4) 0.21193(10) 0.0250(7) Uani 1 1 d . . . H11 H 1.0735 1.1366 0.2131 0.030 Uiso 1 1 calc R . . C12 C 0.8879(3) 1.1762(4) 0.19423(10) 0.0245(7) Uani 1 1 d . . . H12 H 0.8844 1.2763 0.1812 0.029 Uiso 1 1 calc R . . C13 C 0.7869(3) 1.0767(4) 0.19964(10) 0.0253(7) Uani 1 1 d . . . H13 H 0.7050 1.0999 0.1911 0.030 Uiso 1 1 calc R . . C14 C 0.8327(3) 0.9369(4) 0.22022(10) 0.0237(6) Uani 1 1 d . . . H14 H 0.7857 0.8511 0.2277 0.028 Uiso 1 1 calc R . . C15 C 1.0444(3) 0.8261(4) 0.25402(10) 0.0271(7) Uani 1 1 d . . . C16 C 1.0206(3) 0.6580(4) 0.23537(11) 0.0321(8) Uani 1 1 d . . . H16A H 1.0387 0.6545 0.2049 0.048 Uiso 1 1 calc R . . H16B H 0.9364 0.6306 0.2368 0.048 Uiso 1 1 calc R . . H16C H 1.0720 0.5839 0.2528 0.048 Uiso 1 1 calc R . . C17 C 1.0170(3) 0.8279(4) 0.30302(11) 0.0314(8) Uani 1 1 d . . . H17A H 0.9307 0.8154 0.3043 0.047 Uiso 1 1 calc R . . H17B H 1.0434 0.9269 0.3165 0.047 Uiso 1 1 calc R . . H17C H 1.0599 0.7424 0.3188 0.047 Uiso 1 1 calc R . . C18 C 1.1801(3) 0.8682(4) 0.25312(11) 0.0314(8) Uani 1 1 d . . . H18A H 1.2297 0.7924 0.2705 0.047 Uiso 1 1 calc R . . H18B H 1.1952 0.9723 0.2654 0.047 Uiso 1 1 calc R . . H18C H 1.2002 0.8663 0.2229 0.047 Uiso 1 1 calc R . . C19 C 0.6695(3) 0.7453(3) 0.11946(10) 0.0225(7) Uani 1 1 d . . . C20 C 0.7111(3) 0.7577(4) 0.07659(10) 0.0249(7) Uani 1 1 d . . . H20 H 0.6718 0.8124 0.0524 0.030 Uiso 1 1 calc R . . C21 C 0.8217(3) 0.6734(4) 0.07666(11) 0.0272(7) Uani 1 1 d . . . H21 H 0.8670 0.6614 0.0525 0.033 Uiso 1 1 calc R . . C22 C 0.8516(3) 0.6106(4) 0.11962(11) 0.0278(7) Uani 1 1 d . . . H22 H 0.9209 0.5515 0.1291 0.033 Uiso 1 1 calc R . . C23 C 0.7571(3) 0.6537(4) 0.14582(11) 0.0251(7) Uani 1 1 d . . . H23 H 0.7534 0.6261 0.1756 0.030 Uiso 1 1 calc R . . C24 C 0.5404(3) 0.7909(4) 0.12960(10) 0.0245(7) Uani 1 1 d . . . C25 C 0.4521(3) 0.6651(4) 0.10646(11) 0.0286(7) Uani 1 1 d . . . H25A H 0.4572 0.6672 0.0748 0.043 Uiso 1 1 calc R . . H25B H 0.3698 0.6885 0.1123 0.043 Uiso 1 1 calc R . . H25C H 0.4746 0.5618 0.1179 0.043 Uiso 1 1 calc R . . C26 C 0.5273(3) 0.7905(4) 0.17974(11) 0.0299(7) Uani 1 1 d . . . H26A H 0.5547 0.6906 0.1923 0.045 Uiso 1 1 calc R . . H26B H 0.4431 0.8065 0.1843 0.045 Uiso 1 1 calc R . . H26C H 0.5760 0.8744 0.1940 0.045 Uiso 1 1 calc R . . C27 C 0.5021(3) 0.9535(4) 0.11012(12) 0.0310(8) Uani 1 1 d . . . H27A H 0.5536 1.0340 0.1247 0.047 Uiso 1 1 calc R . . H27B H 0.4185 0.9740 0.1148 0.047 Uiso 1 1 calc R . . H27C H 0.5102 0.9543 0.0787 0.047 Uiso 1 1 calc R . . C28 C 0.7132(3) 1.2611(4) 0.08858(11) 0.0271(7) Uani 1 1 d . . . H28 H 0.7151 1.2898 0.1185 0.033 Uiso 1 1 calc R . . C29 C 0.6456(3) 1.3519(4) 0.05669(12) 0.0335(8) Uani 1 1 d . . . H29 H 0.6042 1.4401 0.0659 0.040 Uiso 1 1 calc R . . C30 C 0.7010(3) 1.1908(4) 0.00248(11) 0.0315(8) Uani 1 1 d . . . H30 H 0.6992 1.1622 -0.0274 0.038 Uiso 1 1 calc R . . C31 C 0.7689(3) 1.1008(4) 0.03404(10) 0.0263(7) Uani 1 1 d . . . H31 H 0.8116 1.0140 0.0247 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.02033(10) 0.02052(10) 0.01968(9) -0.00086(8) 0.00227(6) 0.00122(8) N1 0.0263(15) 0.0230(13) 0.0284(14) 0.0002(12) 0.0018(12) -0.0010(11) N2 0.0401(18) 0.0342(16) 0.0326(16) 0.0030(13) 0.0004(14) 0.0084(13) C1 0.0208(15) 0.0235(16) 0.0234(15) -0.0016(14) 0.0039(12) 0.0004(13) C2 0.0244(17) 0.0286(17) 0.0182(15) -0.0002(13) 0.0046(13) 0.0011(13) C3 0.0207(17) 0.0221(16) 0.0321(18) -0.0020(14) 0.0093(14) 0.0018(12) C4 0.0217(17) 0.0258(17) 0.0293(17) 0.0064(14) 0.0065(14) 0.0036(13) C5 0.0198(17) 0.0256(16) 0.0233(16) 0.0001(13) 0.0026(13) 0.0007(13) C6 0.0264(18) 0.0209(16) 0.0260(16) -0.0024(13) 0.0031(13) 0.0032(12) C7 0.035(2) 0.0240(16) 0.0325(19) -0.0019(15) -0.0005(15) -0.0004(14) C8 0.036(2) 0.0219(16) 0.0311(18) 0.0035(14) 0.0010(15) -0.0007(14) C9 0.0287(19) 0.0254(17) 0.043(2) 0.0022(16) 0.0074(15) -0.0018(14) C10 0.0253(17) 0.0249(16) 0.0198(14) -0.0045(13) 0.0029(12) 0.0015(13) C11 0.0260(17) 0.0286(17) 0.0206(15) -0.0014(14) 0.0032(13) -0.0013(13) C12 0.0316(19) 0.0221(16) 0.0194(15) -0.0028(13) 0.0010(13) 0.0008(13) C13 0.0234(16) 0.0303(17) 0.0229(15) -0.0040(15) 0.0052(12) 0.0006(14) C14 0.0258(16) 0.0250(16) 0.0207(14) -0.0033(14) 0.0045(12) -0.0012(13) C15 0.0282(18) 0.0295(18) 0.0230(16) 0.0025(14) 0.0000(14) -0.0017(14) C16 0.036(2) 0.0316(18) 0.0287(18) 0.0044(15) 0.0004(15) 0.0063(15) C17 0.035(2) 0.0325(19) 0.0263(18) 0.0022(15) 0.0006(15) -0.0004(15) C18 0.0285(19) 0.0365(18) 0.0280(18) 0.0057(15) -0.0022(15) 0.0021(14) C19 0.0211(16) 0.0231(16) 0.0231(16) -0.0031(13) 0.0015(13) -0.0029(12) C20 0.0272(18) 0.0227(16) 0.0242(16) -0.0020(13) -0.0005(13) -0.0015(13) C21 0.0225(17) 0.0285(18) 0.0313(18) -0.0052(14) 0.0060(14) -0.0037(13) C22 0.0257(18) 0.0225(18) 0.0346(18) -0.0051(14) 0.0002(14) 0.0030(13) C23 0.0280(18) 0.0221(16) 0.0245(16) -0.0007(13) -0.0003(14) -0.0025(13) C24 0.0207(17) 0.0261(16) 0.0268(17) -0.0021(14) 0.0023(13) 0.0010(13) C25 0.0245(18) 0.0304(18) 0.0309(18) -0.0009(15) 0.0031(14) -0.0025(13) C26 0.0225(18) 0.0354(18) 0.0326(18) -0.0053(15) 0.0063(14) -0.0020(14) C27 0.0271(18) 0.0277(18) 0.0386(19) 0.0020(15) 0.0053(15) 0.0032(14) C28 0.0330(19) 0.0226(16) 0.0257(16) -0.0025(14) 0.0032(14) -0.0002(13) C29 0.035(2) 0.0273(18) 0.039(2) -0.0013(16) 0.0071(16) 0.0053(15) C30 0.0317(19) 0.038(2) 0.0245(17) -0.0021(15) 0.0004(14) -0.0009(15) C31 0.0271(17) 0.0253(17) 0.0268(17) -0.0015(14) 0.0040(13) -0.0003(13) _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 Ce N1 2.695(3) . ? Ce C22 2.750(3) . ? Ce C4 2.797(3) . ? Ce C13 2.803(3) . ? Ce C21 2.816(3) . ? Ce C12 2.818(3) . ? Ce C3 2.820(3) . ? Ce C14 2.827(3) . ? Ce C11 2.867(3) . ? Ce C10 2.868(3) . ? Ce C23 2.867(3) . ? Ce C2 2.905(3) . ? Ce C5 2.914(3) . ? Ce C20 2.942(3) . ? Ce C19 2.992(3) . ? Ce C1 3.002(3) . ? N1 C31 1.339(4) . ? N1 C28 1.340(4) . ? N2 C29 1.339(4) . ? N2 C30 1.338(4) . ? C1 C5 1.409(4) . ? C1 C2 1.413(4) . ? C1 C6 1.533(4) . ? C2 C3 1.399(4) . ? C3 C4 1.405(4) . ? C4 C5 1.405(4) . ? C6 C7 1.534(4) . ? C6 C9 1.538(4) . ? C6 C8 1.541(4) . ? C10 C14 1.409(4) . ? C10 C11 1.416(4) . ? C10 C15 1.531(4) . ? C11 C12 1.402(4) . ? C12 C13 1.415(4) . ? C13 C14 1.401(4) . ? C15 C18 1.536(5) . ? C15 C17 1.537(4) . ? C15 C16 1.538(4) . ? C19 C23 1.412(4) . ? C19 C20 1.418(4) . ? C19 C24 1.532(4) . ? C20 C21 1.408(4) . ? C21 C22 1.404(5) . ? C22 C23 1.417(4) . ? C24 C27 1.533(4) . ? C24 C26 1.531(4) . ? C24 C25 1.553(4) . ? C28 C29 1.382(5) . ? C30 C31 1.374(4) . ? 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 N1 Ce C22 116.70(9) . . ? N1 Ce C4 125.54(9) . . ? C22 Ce C4 85.63(9) . . ? N1 Ce C13 84.27(9) . . ? C22 Ce C13 115.78(9) . . ? C4 Ce C13 132.16(9) . . ? N1 Ce C21 90.39(9) . . ? C22 Ce C21 29.19(9) . . ? C4 Ce C21 91.05(9) . . ? C13 Ce C21 129.01(9) . . ? N1 Ce C12 81.76(8) . . ? C22 Ce C12 142.31(9) . . ? C4 Ce C12 110.99(9) . . ? C13 Ce C12 29.16(9) . . ? C21 Ce C12 157.15(9) . . ? N1 Ce C3 105.46(9) . . ? C22 Ce C3 75.57(9) . . ? C4 Ce C3 28.97(9) . . ? C13 Ce C3 160.35(9) . . ? C21 Ce C3 68.91(9) . . ? C12 Ce C3 133.85(9) . . ? N1 Ce C14 112.00(8) . . ? C22 Ce C14 95.05(9) . . ? C4 Ce C14 114.63(9) . . ? C13 Ce C14 28.81(9) . . ? C21 Ce C14 118.53(9) . . ? C12 Ce C14 47.43(9) . . ? C3 Ce C14 141.43(9) . . ? N1 Ce C11 107.48(8) . . ? C22 Ce C11 130.86(9) . . ? C4 Ce C11 85.74(9) . . ? C13 Ce C11 47.36(9) . . ? C21 Ce C11 160.05(9) . . ? C12 Ce C11 28.55(9) . . ? C3 Ce C11 112.99(9) . . ? C14 Ce C11 46.91(9) . . ? N1 Ce C10 128.36(8) . . ? C22 Ce C10 102.74(9) . . ? C4 Ce C10 87.50(9) . . ? C13 Ce C10 47.64(9) . . ? C21 Ce C10 131.70(9) . . ? C12 Ce C10 47.49(9) . . ? C3 Ce C10 116.07(9) . . ? C14 Ce C10 28.63(8) . . ? C11 Ce C10 28.59(8) . . ? N1 Ce C23 109.71(8) . . ? C22 Ce C23 29.12(9) . . ? C4 Ce C23 110.56(9) . . ? C13 Ce C23 87.42(9) . . ? C21 Ce C23 47.20(9) . . ? C12 Ce C23 115.73(9) . . ? C3 Ce C23 104.66(9) . . ? C14 Ce C23 71.34(9) . . ? C11 Ce C23 116.04(9) . . ? C10 Ce C23 88.68(9) . . ? N1 Ce C2 79.99(8) . . ? C22 Ce C2 97.73(9) . . ? C4 Ce C2 46.72(9) . . ? C13 Ce C2 146.48(9) . . ? C21 Ce C2 80.74(9) . . ? C12 Ce C2 118.51(9) . . ? C3 Ce C2 28.24(9) . . ? C14 Ce C2 155.98(9) . . ? C11 Ce C2 110.48(9) . . ? C10 Ce C2 127.80(9) . . ? C23 Ce C2 125.74(9) . . ? C31 N1 C28 115.1(3) . . ? C31 N1 Ce 116.5(2) . . ? C28 N1 Ce 128.3(2) . . ? C29 N2 C30 114.8(3) . . ? C5 C1 C2 106.0(3) . . ? C5 C1 C6 125.6(3) . . ? C2 C1 C6 126.8(3) . . ? C5 C1 Ce 72.76(17) . . ? C2 C1 Ce 72.37(17) . . ? C6 C1 Ce 130.89(19) . . ? C3 C2 C1 109.4(3) . . ? C3 C2 Ce 72.50(17) . . ? C1 C2 Ce 80.01(17) . . ? C2 C3 C4 107.6(3) . . ? C2 C3 Ce 79.25(17) . . ? C4 C3 Ce 74.60(17) . . ? C5 C4 C3 107.6(3) . . ? C5 C4 Ce 80.44(18) . . ? C3 C4 Ce 76.43(18) . . ? C4 C5 C1 109.3(3) . . ? C4 C5 Ce 71.18(18) . . ? C1 C5 Ce 79.73(18) . . ? C1 C6 C7 110.9(3) . . ? C1 C6 C9 108.4(2) . . ? C7 C6 C9 108.6(3) . . ? C1 C6 C8 111.9(3) . . ? C7 C6 C8 108.9(2) . . ? C9 C6 C8 108.1(3) . . ? C14 C10 C11 106.7(3) . . ? C14 C10 C15 125.4(3) . . ? C11 C10 C15 127.4(3) . . ? C14 C10 Ce 74.07(16) . . ? C11 C10 Ce 75.65(17) . . ? C15 C10 Ce 122.11(19) . . ? C12 C11 C10 108.7(3) . . ? C12 C11 Ce 73.81(17) . . ? C10 C11 Ce 75.75(17) . . ? C11 C12 C13 107.9(3) . . ? C11 C12 Ce 77.64(17) . . ? C13 C12 Ce 74.83(17) . . ? C14 C13 C12 107.5(3) . . ? C14 C13 Ce 76.54(17) . . ? C12 C13 Ce 76.01(17) . . ? C13 C14 C10 109.2(3) . . ? C13 C14 Ce 74.65(17) . . ? C10 C14 Ce 77.30(17) . . ? C10 C15 C18 111.5(3) . . ? C10 C15 C17 108.8(3) . . ? C18 C15 C17 107.7(3) . . ? C10 C15 C16 110.8(3) . . ? C18 C15 C16 109.6(3) . . ? C17 C15 C16 108.5(3) . . ? C23 C19 C20 106.6(3) . . ? C23 C19 C24 128.1(3) . . ? C20 C19 C24 123.9(3) . . ? C23 C19 Ce 71.17(17) . . ? C20 C19 Ce 74.22(17) . . ? C24 C19 Ce 130.45(19) . . ? C21 C20 C19 108.8(3) . . ? C21 C20 Ce 70.94(18) . . ? C19 C20 Ce 78.14(18) . . ? C22 C21 C20 108.1(3) . . ? C22 C21 Ce 72.80(17) . . ? C20 C21 Ce 80.86(18) . . ? C21 C22 C23 107.6(3) . . ? C21 C22 Ce 78.01(17) . . ? C23 C22 Ce 79.99(18) . . ? C19 C23 C22 108.9(3) . . ? C19 C23 Ce 81.04(17) . . ? C22 C23 Ce 70.88(17) . . ? C19 C24 C27 111.8(3) . . ? C19 C24 C26 112.4(3) . . ? C27 C24 C26 109.2(3) . . ? C19 C24 C25 106.7(2) . . ? C27 C24 C25 107.8(3) . . ? C26 C24 C25 108.8(3) . . ? N1 C28 C29 122.1(3) . . ? N2 C29 C28 122.8(3) . . ? N2 C30 C31 122.6(3) . . ? N1 C31 C30 122.6(3) . . ? #===END data_(Ce,Bu^t^,dimethylpyrazine) _database_code_depnum_ccdc_archive 'CCDC 223538' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H47 Ce N2' _chemical_formula_weight 611.85 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.9794(10) _cell_length_b 20.3310(11) _cell_length_c 15.4327(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.978(3) _cell_angle_gamma 90.00 _cell_volume 6108.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 41749 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method ? _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 1.512 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 41749 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.68 _reflns_number_total 11544 _reflns_number_gt 6401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0235P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11544 _refine_ls_number_parameters 671 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1248 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.612 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.136 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 0.131529(19) 0.32363(2) 0.78964(2) 0.01512(10) Uani 1 1 d . . . N1A N 0.0984(3) 0.1955(3) 0.8025(4) 0.0228(14) Uani 1 1 d . . . N2A N 0.0612(3) 0.0623(3) 0.7966(3) 0.0220(14) Uani 1 1 d . . . C1A C 0.0057(4) 0.3223(3) 0.6423(4) 0.0186(14) Uani 1 1 d . . . C2A C 0.0312(4) 0.3878(3) 0.6521(4) 0.0185(16) Uani 1 1 d . . . H2A H 0.0090 0.4239 0.6697 0.022 Uiso 1 1 calc R . . C3A C 0.0969(4) 0.3883(3) 0.6301(4) 0.0233(17) Uani 1 1 d . . . H3A H 0.1260 0.4244 0.6331 0.028 Uiso 1 1 calc R . . C4A C 0.1098(4) 0.3245(4) 0.6030(4) 0.0218(15) Uani 1 1 d . . . H4A H 0.1480 0.3114 0.5822 0.026 Uiso 1 1 calc R . . C5A C 0.0553(4) 0.2841(3) 0.6129(4) 0.0204(16) Uani 1 1 d . . . H5A H 0.0523 0.2391 0.6018 0.024 Uiso 1 1 calc R . . C6A C -0.0670(4) 0.2993(4) 0.6420(4) 0.0253(18) Uani 1 1 d . . . C7A C -0.0671(4) 0.2377(4) 0.7008(5) 0.040(2) Uani 1 1 d . . . H7A1 H -0.0399 0.2037 0.6823 0.060 Uiso 1 1 calc R . . H7A2 H -0.1133 0.2224 0.6947 0.060 Uiso 1 1 calc R . . H7A3 H -0.0480 0.2487 0.7618 0.060 Uiso 1 1 calc R . . C8A C -0.1036(4) 0.2824(4) 0.5467(4) 0.0291(19) Uani 1 1 d . . . H8A1 H -0.1019 0.3196 0.5090 0.044 Uiso 1 1 calc R . . H8A2 H -0.1506 0.2714 0.5449 0.044 Uiso 1 1 calc R . . H8A3 H -0.0812 0.2456 0.5263 0.044 Uiso 1 1 calc R . . C9A C -0.1071(4) 0.3533(4) 0.6750(5) 0.037(2) Uani 1 1 d . . . H9A1 H -0.0864 0.3629 0.7360 0.056 Uiso 1 1 calc R . . H9A2 H -0.1536 0.3392 0.6702 0.056 Uiso 1 1 calc R . . H9A3 H -0.1067 0.3921 0.6397 0.056 Uiso 1 1 calc R . . C10A C 0.1090(4) 0.4314(3) 0.9056(4) 0.0164(16) Uani 1 1 d . . . C11A C 0.0449(4) 0.4028(3) 0.8716(4) 0.0195(16) Uani 1 1 d . . . H11A H 0.0086 0.4228 0.8321 0.023 Uiso 1 1 calc R . . C12A C 0.0438(4) 0.3393(3) 0.9064(4) 0.0257(18) Uani 1 1 d . . . H12A H 0.0069 0.3103 0.8946 0.031 Uiso 1 1 calc R . . C13A C 0.1081(4) 0.3274(4) 0.9620(4) 0.0245(17) Uani 1 1 d . . . H13A H 0.1217 0.2888 0.9934 0.029 Uiso 1 1 calc R . . C14A C 0.1488(4) 0.3840(3) 0.9620(4) 0.0213(17) Uani 1 1 d . . . H14A H 0.1939 0.3894 0.9937 0.026 Uiso 1 1 calc R . . C15A C 0.1291(4) 0.5033(3) 0.8957(4) 0.0264(18) Uani 1 1 d . . . C16A C 0.2035(4) 0.5173(4) 0.9438(4) 0.0272(18) Uani 1 1 d . . . H16A H 0.2338 0.4886 0.9214 0.041 Uiso 1 1 calc R . . H16B H 0.2088 0.5100 1.0065 0.041 Uiso 1 1 calc R . . H16C H 0.2146 0.5622 0.9338 0.041 Uiso 1 1 calc R . . C17A C 0.0807(4) 0.5469(3) 0.9364(4) 0.0254(17) Uani 1 1 d . . . H17A H 0.0945 0.5921 0.9353 0.038 Uiso 1 1 calc R . . H17B H 0.0830 0.5337 0.9967 0.038 Uiso 1 1 calc R . . H17C H 0.0344 0.5422 0.9023 0.038 Uiso 1 1 calc R . . C18A C 0.1187(4) 0.5221(3) 0.7971(4) 0.0310(19) Uani 1 1 d . . . H18A H 0.1277 0.5682 0.7923 0.046 Uiso 1 1 calc R . . H18B H 0.0723 0.5127 0.7668 0.046 Uiso 1 1 calc R . . H18C H 0.1497 0.4971 0.7706 0.046 Uiso 1 1 calc R . . C19A C 0.2714(4) 0.2618(3) 0.8486(4) 0.0177(16) Uani 1 1 d . . . C20A C 0.2725(3) 0.3252(3) 0.8838(4) 0.0191(14) Uani 1 1 d . . . H20A H 0.2786 0.3352 0.9439 0.023 Uiso 1 1 calc R . . C21A C 0.2631(4) 0.3717(3) 0.8144(4) 0.0184(16) Uani 1 1 d . . . H21A H 0.2621 0.4171 0.8207 0.022 Uiso 1 1 calc R . . C22A C 0.2552(4) 0.3367(3) 0.7332(4) 0.0199(16) Uani 1 1 d . . . H22A H 0.2488 0.3549 0.6767 0.024 Uiso 1 1 calc R . . C23A C 0.2591(4) 0.2698(3) 0.7543(5) 0.0211(17) Uani 1 1 d . . . H23A H 0.2544 0.2357 0.7133 0.025 Uiso 1 1 calc R . . C24A C 0.2959(4) 0.2000(3) 0.9021(4) 0.0210(16) Uani 1 1 d . . . C25A C 0.3742(4) 0.2078(4) 0.9389(5) 0.034(2) Uani 1 1 d . . . H25A H 0.3972 0.2074 0.8905 0.050 Uiso 1 1 calc R . . H25B H 0.3909 0.1721 0.9786 0.050 Uiso 1 1 calc R . . H25C H 0.3832 0.2488 0.9704 0.050 Uiso 1 1 calc R . . C26A C 0.2620(4) 0.1938(3) 0.9821(4) 0.034(2) Uani 1 1 d . . . H26A H 0.2695 0.2336 1.0165 0.051 Uiso 1 1 calc R . . H26B H 0.2819 0.1574 1.0185 0.051 Uiso 1 1 calc R . . H26C H 0.2136 0.1867 0.9612 0.051 Uiso 1 1 calc R . . C27A C 0.2857(4) 0.1373(3) 0.8470(5) 0.0290(19) Uani 1 1 d . . . H27A H 0.2375 0.1295 0.8250 0.044 Uiso 1 1 calc R . . H27B H 0.3059 0.1010 0.8833 0.044 Uiso 1 1 calc R . . H27C H 0.3075 0.1420 0.7978 0.044 Uiso 1 1 calc R . . C28A C 0.1148(4) 0.1541(3) 0.7444(4) 0.0215(16) Uani 1 1 d . . . H28A H 0.1393 0.1703 0.7043 0.026 Uiso 1 1 calc R . . C29A C 0.0974(4) 0.0875(3) 0.7401(4) 0.0198(16) Uani 1 1 d . . . C30A C 0.0447(4) 0.1047(3) 0.8560(4) 0.0249(18) Uani 1 1 d . . . C31A C 0.0637(4) 0.1695(4) 0.8600(4) 0.0239(16) Uani 1 1 d . . . H31A H 0.0524 0.1963 0.9033 0.029 Uiso 1 1 calc R . . C32A C 0.1207(5) 0.0418(3) 0.6767(5) 0.038(2) Uani 1 1 d . . . H32A H 0.1668 0.0275 0.7019 0.056 Uiso 1 1 calc R . . H32B H 0.1196 0.0643 0.6216 0.056 Uiso 1 1 calc R . . H32C H 0.0908 0.0043 0.6658 0.056 Uiso 1 1 calc R . . C33A C 0.0008(5) 0.0779(4) 0.9140(5) 0.039(2) Uani 1 1 d . . . H33A H -0.0461 0.0759 0.8812 0.058 Uiso 1 1 calc R . . H33B H 0.0039 0.1060 0.9648 0.058 Uiso 1 1 calc R . . H33C H 0.0162 0.0345 0.9335 0.058 Uiso 1 1 calc R . . Ce2 Ce 0.37684(2) 0.82450(2) 0.25993(2) 0.01520(10) Uani 1 1 d . . . N1B N 0.4607(3) 0.7196(3) 0.2875(3) 0.0197(13) Uani 1 1 d . . . N2B N 0.5272(3) 0.5970(3) 0.2986(3) 0.0220(14) Uani 1 1 d . . . C1B C 0.4976(4) 0.8924(3) 0.3713(4) 0.0203(16) Uani 1 1 d . . . C2B C 0.4426(4) 0.9370(3) 0.3527(4) 0.0210(16) Uani 1 1 d . . . H2B H 0.4408 0.9747 0.3182 0.025 Uiso 1 1 calc R . . C3B C 0.3907(4) 0.9159(3) 0.3943(4) 0.0205(16) Uani 1 1 d . . . H3B H 0.3492 0.9371 0.3927 0.025 Uiso 1 1 calc R . . C4B C 0.4132(4) 0.8564(4) 0.4392(4) 0.0222(17) Uani 1 1 d . . . H4B H 0.3890 0.8314 0.4723 0.027 Uiso 1 1 calc R . . C5B C 0.4788(4) 0.8419(3) 0.4247(4) 0.0189(16) Uani 1 1 d . . . H5B H 0.5053 0.8054 0.4465 0.023 Uiso 1 1 calc R . . C6B C 0.5702(4) 0.9041(3) 0.3596(4) 0.0230(17) Uani 1 1 d . . . C7B C 0.6064(4) 0.8406(3) 0.3443(5) 0.031(2) Uani 1 1 d . . . H7B1 H 0.6050 0.8101 0.3914 0.047 Uiso 1 1 calc R . . H7B2 H 0.6533 0.8500 0.3434 0.047 Uiso 1 1 calc R . . H7B3 H 0.5836 0.8217 0.2885 0.047 Uiso 1 1 calc R . . C8B C 0.6114(4) 0.9354(4) 0.4470(4) 0.0310(19) Uani 1 1 d . . . H8B1 H 0.5896 0.9756 0.4582 0.046 Uiso 1 1 calc R . . H8B2 H 0.6574 0.9445 0.4414 0.046 Uiso 1 1 calc R . . H8B3 H 0.6127 0.9055 0.4955 0.046 Uiso 1 1 calc R . . C9B C 0.5727(4) 0.9528(3) 0.2839(4) 0.0275(18) Uani 1 1 d . . . H9B1 H 0.5501 0.9337 0.2281 0.041 Uiso 1 1 calc R . . H9B2 H 0.6197 0.9621 0.2833 0.041 Uiso 1 1 calc R . . H9B3 H 0.5499 0.9928 0.2933 0.041 Uiso 1 1 calc R . . C10B C 0.3415(4) 0.9019(3) 0.0982(4) 0.0174(16) Uani 1 1 d . . . C11B C 0.4117(4) 0.9125(3) 0.1349(4) 0.0191(16) Uani 1 1 d . . . H11B H 0.4311 0.9516 0.1599 0.023 Uiso 1 1 calc R . . C12B C 0.4481(4) 0.8534(3) 0.1272(4) 0.0243(18) Uani 1 1 d . . . H12B H 0.4952 0.8470 0.1460 0.029 Uiso 1 1 calc R . . C13B C 0.3997(4) 0.8063(3) 0.0861(4) 0.0206(17) Uani 1 1 d . . . H13B H 0.4090 0.7629 0.0738 0.025 Uiso 1 1 calc R . . C14B C 0.3344(4) 0.8365(3) 0.0668(4) 0.0244(18) Uani 1 1 d . . . H14B H 0.2935 0.8166 0.0381 0.029 Uiso 1 1 calc R . . C15B C 0.2865(4) 0.9554(3) 0.0822(4) 0.0249(17) Uani 1 1 d . . . C16B C 0.2135(4) 0.9256(4) 0.0499(5) 0.0303(19) Uani 1 1 d . . . H16D H 0.2102 0.9042 -0.0063 0.045 Uiso 1 1 calc R . . H16E H 0.1799 0.9601 0.0434 0.045 Uiso 1 1 calc R . . H16F H 0.2052 0.8942 0.0928 0.045 Uiso 1 1 calc R . . C17B C 0.3001(5) 1.0016(4) 0.0088(5) 0.040(2) Uani 1 1 d . . . H17D H 0.3453 1.0201 0.0270 0.060 Uiso 1 1 calc R . . H17E H 0.2667 1.0363 -0.0011 0.060 Uiso 1 1 calc R . . H17F H 0.2968 0.9771 -0.0452 0.060 Uiso 1 1 calc R . . C18B C 0.2893(4) 0.9961(3) 0.1658(5) 0.0309(19) Uani 1 1 d . . . H18D H 0.2840 0.9677 0.2135 0.046 Uiso 1 1 calc R . . H18E H 0.2528 1.0279 0.1547 0.046 Uiso 1 1 calc R . . H18F H 0.3326 1.0184 0.1819 0.046 Uiso 1 1 calc R . . C19B C 0.2698(4) 0.7184(3) 0.2364(4) 0.0221(17) Uani 1 1 d . . . C20B C 0.2398(4) 0.7761(3) 0.1950(4) 0.0224(17) Uani 1 1 d . . . H20B H 0.2236 0.7818 0.1341 0.027 Uiso 1 1 calc R . . C21B C 0.2382(3) 0.8234(3) 0.2601(4) 0.0196(14) Uani 1 1 d . . . H21B H 0.2206 0.8657 0.2496 0.024 Uiso 1 1 calc R . . C22B C 0.2676(4) 0.7967(3) 0.3435(5) 0.0269(18) Uani 1 1 d . . . H22B H 0.2720 0.8173 0.3983 0.032 Uiso 1 1 calc R . . C23B C 0.2888(4) 0.7333(3) 0.3282(4) 0.0204(16) Uani 1 1 d . . . H23B H 0.3120 0.7049 0.3720 0.024 Uiso 1 1 calc R . . C24B C 0.2707(4) 0.6529(3) 0.1898(5) 0.0251(17) Uani 1 1 d . . . C25B C 0.2902(4) 0.5970(3) 0.2589(5) 0.0310(19) Uani 1 1 d . . . H25D H 0.3363 0.6035 0.2926 0.047 Uiso 1 1 calc R . . H25E H 0.2871 0.5554 0.2288 0.047 Uiso 1 1 calc R . . H25F H 0.2592 0.5973 0.2983 0.047 Uiso 1 1 calc R . . C26B C 0.1977(5) 0.6379(4) 0.1343(5) 0.037(2) Uani 1 1 d . . . H26D H 0.1652 0.6422 0.1714 0.056 Uiso 1 1 calc R . . H26E H 0.1962 0.5939 0.1114 0.056 Uiso 1 1 calc R . . H26F H 0.1863 0.6685 0.0858 0.056 Uiso 1 1 calc R . . C27B C 0.3191(5) 0.6515(4) 0.1263(5) 0.043(2) Uani 1 1 d . . . H27D H 0.3060 0.6850 0.0820 0.064 Uiso 1 1 calc R . . H27E H 0.3166 0.6092 0.0980 0.064 Uiso 1 1 calc R . . H27F H 0.3653 0.6593 0.1590 0.064 Uiso 1 1 calc R . . C28B C 0.4594(4) 0.6770(3) 0.3531(4) 0.0206(15) Uani 1 1 d . . . H28B H 0.4365 0.6891 0.3968 0.025 Uiso 1 1 calc R . . C29B C 0.4902(4) 0.6159(3) 0.3592(4) 0.0229(17) Uani 1 1 d . . . C30B C 0.5313(4) 0.6401(3) 0.2346(4) 0.0197(16) Uani 1 1 d . . . C31B C 0.4989(4) 0.7008(3) 0.2310(4) 0.0210(17) Uani 1 1 d . . . H31B H 0.5040 0.7301 0.1866 0.025 Uiso 1 1 calc R . . C32B C 0.4856(4) 0.5678(3) 0.4300(4) 0.0227(17) Uani 1 1 d . . . H32D H 0.4643 0.5281 0.4035 0.034 Uiso 1 1 calc R . . H32E H 0.4587 0.5862 0.4684 0.034 Uiso 1 1 calc R . . H32F H 0.5309 0.5580 0.4641 0.034 Uiso 1 1 calc R . . C33B C 0.5675(4) 0.6208(3) 0.1638(4) 0.0229(17) Uani 1 1 d . . . H33D H 0.6019 0.5885 0.1869 0.034 Uiso 1 1 calc R . . H33E H 0.5888 0.6588 0.1448 0.034 Uiso 1 1 calc R . . H33F H 0.5349 0.6026 0.1142 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0150(2) 0.01548(19) 0.01516(18) -0.00061(18) 0.00400(17) -0.0013(2) N1A 0.025(4) 0.015(3) 0.027(3) -0.001(2) 0.003(3) 0.005(3) N2A 0.028(4) 0.018(3) 0.020(3) -0.003(2) 0.004(3) -0.008(3) C1A 0.025(4) 0.016(3) 0.012(3) 0.003(3) -0.001(3) -0.004(4) C2A 0.017(4) 0.019(4) 0.018(3) 0.001(3) 0.002(3) 0.006(3) C3A 0.024(5) 0.026(4) 0.019(4) -0.005(3) 0.002(3) -0.007(4) C4A 0.023(4) 0.025(3) 0.018(3) -0.009(3) 0.004(3) 0.001(4) C5A 0.022(5) 0.016(3) 0.022(4) -0.005(3) 0.002(3) 0.001(3) C6A 0.018(5) 0.041(4) 0.016(3) -0.001(3) 0.001(3) 0.002(4) C7A 0.017(5) 0.060(6) 0.043(5) 0.004(4) 0.008(4) -0.012(4) C8A 0.019(5) 0.034(4) 0.032(4) -0.008(4) 0.000(4) -0.002(4) C9A 0.023(5) 0.055(5) 0.032(4) -0.011(4) 0.003(4) -0.003(4) C10A 0.025(5) 0.015(3) 0.010(3) -0.002(3) 0.005(3) -0.004(3) C11A 0.016(4) 0.024(4) 0.016(3) 0.001(3) 0.001(3) 0.000(3) C12A 0.032(5) 0.016(4) 0.033(4) 0.002(3) 0.015(4) -0.003(3) C13A 0.032(5) 0.020(3) 0.025(4) 0.003(3) 0.014(3) 0.009(4) C14A 0.023(5) 0.026(4) 0.015(3) -0.004(3) 0.004(3) 0.000(3) C15A 0.031(5) 0.026(4) 0.023(4) 0.004(3) 0.006(4) 0.006(4) C16A 0.027(5) 0.030(4) 0.022(4) -0.003(3) 0.000(3) -0.004(4) C17A 0.018(5) 0.022(4) 0.033(4) -0.005(3) -0.001(3) 0.005(3) C18A 0.038(6) 0.023(4) 0.034(4) -0.002(3) 0.011(4) -0.007(4) C19A 0.010(4) 0.023(4) 0.022(4) 0.004(3) 0.009(3) 0.003(3) C20A 0.009(4) 0.023(3) 0.025(3) -0.007(3) 0.004(3) 0.001(4) C21A 0.014(4) 0.019(3) 0.024(4) -0.001(3) 0.007(3) 0.000(3) C22A 0.014(4) 0.021(4) 0.026(4) 0.001(3) 0.008(3) 0.001(3) C23A 0.025(5) 0.018(4) 0.024(4) -0.002(3) 0.013(4) 0.003(3) C24A 0.014(4) 0.029(4) 0.020(3) 0.004(3) 0.003(3) 0.000(3) C25A 0.024(5) 0.033(4) 0.042(5) 0.010(4) 0.001(4) 0.000(4) C26A 0.047(6) 0.033(5) 0.025(4) 0.009(3) 0.016(4) 0.009(4) C27A 0.028(5) 0.022(4) 0.033(4) 0.004(3) 0.000(4) 0.005(4) C28A 0.019(5) 0.020(3) 0.028(4) 0.011(3) 0.010(3) -0.003(3) C29A 0.011(4) 0.022(4) 0.027(4) -0.007(3) 0.007(3) -0.002(3) C30A 0.031(5) 0.026(4) 0.017(3) -0.001(3) 0.004(3) -0.004(4) C31A 0.027(4) 0.028(4) 0.018(3) 0.001(3) 0.007(3) 0.000(4) C32A 0.040(6) 0.028(4) 0.050(5) -0.012(4) 0.023(4) -0.006(4) C33A 0.055(7) 0.035(5) 0.027(4) 0.000(4) 0.011(4) -0.015(4) Ce2 0.0170(2) 0.01397(19) 0.01510(18) -0.00019(18) 0.00450(17) 0.0001(2) N1B 0.022(4) 0.017(3) 0.022(3) -0.003(2) 0.009(3) -0.004(3) N2B 0.026(4) 0.020(3) 0.020(3) 0.001(3) 0.005(3) 0.000(3) C1B 0.022(5) 0.023(4) 0.016(3) -0.007(3) 0.005(3) -0.001(3) C2B 0.027(5) 0.014(3) 0.023(4) -0.005(3) 0.007(3) -0.008(3) C3B 0.012(4) 0.030(4) 0.018(3) -0.012(3) 0.001(3) 0.003(3) C4B 0.017(5) 0.035(4) 0.015(3) -0.004(3) 0.006(3) -0.003(4) C5B 0.017(4) 0.021(4) 0.015(3) 0.001(3) -0.004(3) 0.002(3) C6B 0.025(5) 0.024(4) 0.018(3) 0.006(3) 0.002(3) 0.002(3) C7B 0.030(5) 0.033(5) 0.034(4) 0.007(3) 0.013(4) 0.009(4) C8B 0.024(5) 0.037(4) 0.030(4) -0.001(3) 0.002(4) -0.008(4) C9B 0.018(5) 0.034(4) 0.030(4) 0.009(3) 0.002(3) -0.003(4) C10B 0.010(4) 0.023(4) 0.020(3) 0.000(3) 0.006(3) -0.001(3) C11B 0.024(5) 0.015(3) 0.019(3) 0.007(3) 0.004(3) 0.007(3) C12B 0.031(5) 0.027(4) 0.019(3) 0.003(3) 0.016(4) 0.007(4) C13B 0.028(5) 0.019(4) 0.015(3) 0.007(3) 0.005(3) 0.001(3) C14B 0.036(5) 0.024(4) 0.014(3) 0.004(3) 0.008(3) -0.003(4) C15B 0.029(5) 0.019(4) 0.023(4) 0.001(3) -0.002(3) 0.002(3) C16B 0.023(5) 0.032(4) 0.029(4) 0.001(3) -0.010(4) 0.008(4) C17B 0.045(6) 0.028(4) 0.049(5) 0.020(4) 0.015(5) 0.000(4) C18B 0.022(5) 0.026(4) 0.042(4) -0.004(4) 0.001(4) 0.010(4) C19B 0.025(5) 0.020(4) 0.023(4) -0.001(3) 0.011(3) -0.010(3) C20B 0.018(5) 0.030(4) 0.019(4) 0.002(3) 0.003(3) -0.009(3) C21B 0.018(4) 0.013(3) 0.026(3) -0.005(3) 0.001(3) 0.003(3) C22B 0.026(5) 0.027(4) 0.033(4) -0.010(3) 0.015(4) -0.012(4) C23B 0.012(4) 0.026(4) 0.024(4) 0.007(3) 0.006(3) 0.002(3) C24B 0.025(5) 0.020(4) 0.031(4) -0.006(3) 0.010(4) -0.008(3) C25B 0.027(5) 0.018(4) 0.046(5) -0.004(3) 0.005(4) 0.001(4) C26B 0.045(6) 0.031(4) 0.034(4) -0.016(4) 0.004(4) -0.010(4) C27B 0.054(7) 0.032(4) 0.053(5) -0.019(4) 0.031(5) -0.012(4) C28B 0.024(4) 0.017(3) 0.020(3) -0.007(3) 0.004(3) -0.005(4) C29B 0.032(5) 0.017(4) 0.020(3) 0.002(3) 0.006(3) 0.000(3) C30B 0.016(4) 0.020(4) 0.023(4) 0.000(3) 0.005(3) -0.001(3) C31B 0.034(5) 0.018(3) 0.012(3) 0.002(3) 0.008(3) 0.002(3) C32B 0.030(5) 0.022(4) 0.017(3) 0.002(3) 0.008(3) 0.010(3) C33B 0.020(5) 0.024(4) 0.029(4) 0.002(3) 0.013(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 N1A 2.707(5) . ? Ce1 C3A 2.740(7) . ? Ce1 C21A 2.749(7) . ? Ce1 C12A 2.799(7) . ? Ce1 C13A 2.803(6) . ? Ce1 C22A 2.811(7) . ? Ce1 C4A 2.815(6) . ? Ce1 C11A 2.858(7) . ? Ce1 C20A 2.865(6) . ? Ce1 C14A 2.880(6) . ? Ce1 C2A 2.884(7) . ? Ce1 C5A 2.923(6) . ? Ce1 C10A 2.927(7) . ? Ce1 C23A 2.935(6) . ? Ce1 C1A 2.987(6) . ? Ce1 C19A 3.012(7) . ? N1A C28A 1.322(8) . ? N1A C31A 1.351(8) . ? N2A C30A 1.352(8) . ? N2A C29A 1.353(8) . ? C1A C5A 1.412(9) . ? C1A C2A 1.422(9) . ? C1A C6A 1.526(10) . ? C2A C3A 1.429(10) . ? C3A C4A 1.403(9) . ? C4A C5A 1.400(9) . ? C6A C9A 1.514(10) . ? C6A C8A 1.527(9) . ? C6A C7A 1.546(10) . ? C10A C11A 1.399(9) . ? C10A C14A 1.416(9) . ? C10A C15A 1.532(9) . ? C11A C12A 1.398(9) . ? C12A C13A 1.397(10) . ? C13A C14A 1.409(10) . ? C15A C18A 1.538(9) . ? C15A C16A 1.532(10) . ? C15A C17A 1.545(9) . ? C19A C20A 1.397(9) . ? C19A C23A 1.430(8) . ? C19A C24A 1.522(9) . ? C20A C21A 1.409(9) . ? C21A C22A 1.418(9) . ? C22A C23A 1.397(9) . ? C24A C27A 1.520(9) . ? C24A C26A 1.540(9) . ? C24A C25A 1.549(10) . ? C28A C29A 1.397(9) . ? C29A C32A 1.498(9) . ? C30A C31A 1.369(9) . ? C30A C33A 1.490(10) . ? Ce2 N1B 2.685(6) . ? Ce2 C3B 2.752(6) . ? Ce2 C21B 2.770(7) . ? Ce2 C4B 2.775(6) . ? Ce2 C12B 2.806(6) . ? Ce2 C22B 2.831(7) . ? Ce2 C11B 2.830(6) . ? Ce2 C13B 2.844(6) . ? Ce2 C2B 2.857(6) . ? Ce2 C20B 2.870(7) . ? Ce2 C10B 2.900(6) . ? Ce2 C5B 2.901(6) . ? Ce2 C23B 2.912(6) . ? Ce2 C14B 2.920(7) . ? Ce2 C1B 2.971(6) . ? Ce2 C19B 3.002(6) . ? N1B C31B 1.338(8) . ? N1B C28B 1.337(8) . ? N2B C30B 1.335(8) . ? N2B C29B 1.372(8) . ? C1B C2B 1.403(10) . ? C1B C5B 1.420(9) . ? C1B C6B 1.518(10) . ? C2B C3B 1.404(9) . ? C3B C4B 1.415(9) . ? C4B C5B 1.409(9) . ? C6B C7B 1.525(9) . ? C6B C9B 1.540(9) . ? C6B C8B 1.550(9) . ? C10B C11B 1.406(10) . ? C10B C14B 1.410(9) . ? C10B C15B 1.526(9) . ? C11B C12B 1.423(9) . ? C12B C13B 1.406(10) . ? C13B C14B 1.411(10) . ? C15B C18B 1.524(9) . ? C15B C17B 1.542(9) . ? C15B C16B 1.555(10) . ? C19B C20B 1.404(10) . ? C19B C23B 1.414(9) . ? C19B C24B 1.516(9) . ? C20B C21B 1.395(9) . ? C21B C22B 1.398(9) . ? C22B C23B 1.394(9) . ? C24B C27B 1.523(10) . ? C24B C25B 1.548(9) . ? C24B C26B 1.547(11) . ? C28B C29B 1.380(9) . ? C29B C32B 1.484(8) . ? C30B C31B 1.389(9) . ? C30B C33B 1.492(8) . ? 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 N1A Ce1 C3A 120.75(19) . . ? N1A Ce1 C21A 125.00(19) . . ? C3A Ce1 C21A 89.7(2) . . ? N1A Ce1 C12A 82.19(18) . . ? C3A Ce1 C12A 117.1(2) . . ? C21A Ce1 C12A 126.0(2) . . ? N1A Ce1 C13A 82.01(19) . . ? C3A Ce1 C13A 141.1(2) . . ? C21A Ce1 C13A 102.5(2) . . ? C12A Ce1 C13A 28.9(2) . . ? N1A Ce1 C22A 111.11(18) . . ? C3A Ce1 C22A 74.8(2) . . ? C21A Ce1 C22A 29.51(18) . . ? C12A Ce1 C22A 155.4(2) . . ? C13A Ce1 C22A 129.6(2) . . ? N1A Ce1 C4A 95.58(19) . . ? C3A Ce1 C4A 29.23(19) . . ? C21A Ce1 C4A 93.59(19) . . ? C12A Ce1 C4A 133.1(2) . . ? C13A Ce1 C4A 161.9(2) . . ? C22A Ce1 C4A 68.1(2) . . ? N1A Ce1 C11A 109.10(18) . . ? C3A Ce1 C11A 94.1(2) . . ? C21A Ce1 C11A 113.19(19) . . ? C12A Ce1 C11A 28.60(17) . . ? C13A Ce1 C11A 47.01(19) . . ? C22A Ce1 C11A 138.22(19) . . ? C4A Ce1 C11A 118.7(2) . . ? N1A Ce1 C20A 101.67(19) . . ? C3A Ce1 C20A 118.1(2) . . ? C21A Ce1 C20A 28.97(18) . . ? C12A Ce1 C20A 111.0(2) . . ? C13A Ce1 C20A 82.71(19) . . ? C22A Ce1 C20A 47.42(19) . . ? C4A Ce1 C20A 115.26(19) . . ? C11A Ce1 C20A 113.18(19) . . ? N1A Ce1 C14A 108.87(18) . . ? C3A Ce1 C14A 125.4(2) . . ? C21A Ce1 C14A 78.9(2) . . ? C12A Ce1 C14A 47.1(2) . . ? C13A Ce1 C14A 28.68(19) . . ? C22A Ce1 C14A 108.3(2) . . ? C4A Ce1 C14A 154.4(2) . . ? C11A Ce1 C14A 46.3(2) . . ? C20A Ce1 C14A 68.1(2) . . ? N1A Ce1 C2A 110.40(19) . . ? C3A Ce1 C2A 29.3(2) . . ? C21A Ce1 C2A 115.25(19) . . ? C12A Ce1 C2A 89.4(2) . . ? C13A Ce1 C2A 116.7(2) . . ? C22A Ce1 C2A 104.09(19) . . ? C4A Ce1 C2A 47.31(19) . . ? C11A Ce1 C2A 71.40(19) . . ? C20A Ce1 C2A 144.10(19) . . ? C14A Ce1 C2A 113.97(19) . . ? N1A Ce1 C5A 73.66(18) . . ? C3A Ce1 C5A 47.1(2) . . ? C21A Ce1 C5A 120.58(19) . . ? C12A Ce1 C5A 111.2(2) . . ? C13A Ce1 C5A 136.9(2) . . ? C22A Ce1 C5A 92.68(19) . . ? C4A Ce1 C5A 28.16(18) . . ? C11A Ce1 C5A 109.1(2) . . ? C20A Ce1 C5A 136.31(18) . . ? C14A Ce1 C5A 155.4(2) . . ? C2A Ce1 C5A 46.15(18) . . ? C28A N1A C31A 116.0(6) . . ? C28A N1A Ce1 117.4(4) . . ? C31A N1A Ce1 126.5(4) . . ? C30A N2A C29A 116.3(6) . . ? C5A C1A C2A 106.9(6) . . ? C5A C1A C6A 124.5(6) . . ? C2A C1A C6A 127.2(6) . . ? C5A C1A Ce1 73.7(4) . . ? C2A C1A Ce1 72.0(4) . . ? C6A C1A Ce1 130.0(4) . . ? C1A C2A C3A 107.9(6) . . ? C1A C2A Ce1 80.1(4) . . ? C3A C2A Ce1 69.7(4) . . ? C4A C3A C2A 107.7(6) . . ? C4A C3A Ce1 78.4(4) . . ? C2A C3A Ce1 81.0(4) . . ? C5A C4A C3A 108.2(6) . . ? C5A C4A Ce1 80.2(4) . . ? C3A C4A Ce1 72.4(3) . . ? C4A C5A C1A 109.3(6) . . ? C4A C5A Ce1 71.6(4) . . ? C1A C5A Ce1 78.7(4) . . ? C9A C6A C1A 110.6(6) . . ? C9A C6A C8A 108.2(6) . . ? C1A C6A C8A 108.7(5) . . ? C9A C6A C7A 108.7(6) . . ? C1A C6A C7A 111.9(6) . . ? C8A C6A C7A 108.7(6) . . ? C11A C10A C14A 106.7(6) . . ? C11A C10A C15A 126.7(6) . . ? C14A C10A C15A 126.0(7) . . ? C11A C10A Ce1 73.3(4) . . ? C14A C10A Ce1 74.0(3) . . ? C15A C10A Ce1 125.0(4) . . ? C12A C11A C10A 109.4(7) . . ? C12A C11A Ce1 73.4(4) . . ? C10A C11A Ce1 78.8(4) . . ? C11A C12A C13A 107.8(7) . . ? C11A C12A Ce1 78.0(4) . . ? C13A C12A Ce1 75.7(4) . . ? C12A C13A C14A 107.9(6) . . ? C12A C13A Ce1 75.4(4) . . ? C14A C13A Ce1 78.7(4) . . ? C13A C14A C10A 108.2(7) . . ? C13A C14A Ce1 72.6(4) . . ? C10A C14A Ce1 77.7(3) . . ? C10A C15A C18A 110.8(6) . . ? C10A C15A C16A 112.1(6) . . ? C18A C15A C16A 109.5(6) . . ? C10A C15A C17A 107.8(6) . . ? C18A C15A C17A 107.5(6) . . ? C16A C15A C17A 108.9(6) . . ? C20A C19A C23A 105.9(5) . . ? C20A C19A C24A 125.2(6) . . ? C23A C19A C24A 127.3(6) . . ? C20A C19A Ce1 70.4(4) . . ? C23A C19A Ce1 73.1(4) . . ? C24A C19A Ce1 132.2(4) . . ? C19A C20A C21A 109.6(6) . . ? C19A C20A Ce1 82.2(4) . . ? C21A C20A Ce1 70.9(4) . . ? C20A C21A C22A 107.8(6) . . ? C20A C21A Ce1 80.1(4) . . ? C22A C21A Ce1 77.7(4) . . ? C23A C22A C21A 107.0(6) . . ? C23A C22A Ce1 80.9(4) . . ? C21A C22A Ce1 72.8(4) . . ? C22A C23A C19A 109.6(6) . . ? C22A C23A Ce1 71.1(4) . . ? C19A C23A Ce1 79.1(4) . . ? C19A C24A C27A 113.7(6) . . ? C19A C24A C26A 110.9(6) . . ? C27A C24A C26A 110.7(6) . . ? C19A C24A C25A 106.8(6) . . ? C27A C24A C25A 106.7(6) . . ? C26A C24A C25A 107.6(6) . . ? N1A C28A C29A 123.5(6) . . ? N2A C29A C28A 120.0(6) . . ? N2A C29A C32A 118.5(6) . . ? C28A C29A C32A 121.5(6) . . ? N2A C30A C31A 122.5(6) . . ? N2A C30A C33A 116.1(6) . . ? C31A C30A C33A 121.3(6) . . ? N1A C31A C30A 121.7(6) . . ? N1B Ce2 C3B 117.57(19) . . ? N1B Ce2 C21B 125.55(19) . . ? C3B Ce2 C21B 86.4(2) . . ? N1B Ce2 C4B 90.77(19) . . ? C3B Ce2 C4B 29.66(19) . . ? C21B Ce2 C4B 92.2(2) . . ? N1B Ce2 C12B 83.17(18) . . ? C3B Ce2 C12B 115.3(2) . . ? C21B Ce2 C12B 132.3(2) . . ? C4B Ce2 C12B 128.1(2) . . ? N1B Ce2 C22B 106.68(19) . . ? C3B Ce2 C22B 75.4(2) . . ? C21B Ce2 C22B 28.88(19) . . ? C4B Ce2 C22B 69.4(2) . . ? C12B Ce2 C22B 160.7(2) . . ? N1B Ce2 C11B 111.69(18) . . ? C3B Ce2 C11B 95.1(2) . . ? C21B Ce2 C11B 113.9(2) . . ? C4B Ce2 C11B 118.8(2) . . ? C12B Ce2 C11B 29.25(18) . . ? C22B Ce2 C11B 140.3(2) . . ? N1B Ce2 C13B 79.62(18) . . ? C3B Ce2 C13B 142.0(2) . . ? C21B Ce2 C13B 111.8(2) . . ? C4B Ce2 C13B 155.4(2) . . ? C12B Ce2 C13B 28.80(19) . . ? C22B Ce2 C13B 135.0(2) . . ? C11B Ce2 C13B 47.39(18) . . ? N1B Ce2 C2B 110.83(19) . . ? C3B Ce2 C2B 28.91(19) . . ? C21B Ce2 C2B 110.7(2) . . ? C4B Ce2 C2B 47.5(2) . . ? C12B Ce2 C2B 87.0(2) . . ? C22B Ce2 C2B 104.3(2) . . ? C11B Ce2 C2B 71.35(19) . . ? C13B Ce2 C2B 115.07(19) . . ? N1B Ce2 C20B 107.16(19) . . ? C3B Ce2 C20B 114.9(2) . . ? C21B Ce2 C20B 28.58(18) . . ? C4B Ce2 C20B 116.4(2) . . ? C12B Ce2 C20B 114.7(2) . . ? C22B Ce2 C20B 47.0(2) . . ? C11B Ce2 C20B 109.9(2) . . ? C13B Ce2 C20B 88.2(2) . . ? C2B Ce2 C20B 138.2(2) . . ? N1B Ce2 C10B 126.13(17) . . ? C3B Ce2 C10B 104.3(2) . . ? C21B Ce2 C10B 87.41(19) . . ? C4B Ce2 C10B 133.6(2) . . ? C12B Ce2 C10B 47.5(2) . . ? C22B Ce2 C10B 115.9(2) . . ? C11B Ce2 C10B 28.38(19) . . ? C13B Ce2 C10B 47.03(18) . . ? C2B Ce2 C10B 89.61(19) . . ? C20B Ce2 C10B 81.77(19) . . ? N1B Ce2 C5B 70.59(17) . . ? C3B Ce2 C5B 47.5(2) . . ? C21B Ce2 C5B 120.37(18) . . ? C4B Ce2 C5B 28.63(19) . . ? C12B Ce2 C5B 104.1(2) . . ? C22B Ce2 C5B 95.0(2) . . ? C11B Ce2 C5B 106.8(2) . . ? C13B Ce2 C5B 127.8(2) . . ? C2B Ce2 C5B 46.33(19) . . ? C20B Ce2 C5B 140.78(19) . . ? C10B Ce2 C5B 132.52(19) . . ? C31B N1B C28B 114.7(6) . . ? C31B N1B Ce2 123.4(4) . . ? C28B N1B Ce2 121.2(4) . . ? C30B N2B C29B 116.9(6) . . ? C2B C1B C5B 106.7(6) . . ? C2B C1B C6B 126.8(6) . . ? C5B C1B C6B 124.5(6) . . ? C2B C1B Ce2 71.6(4) . . ? C5B C1B Ce2 73.3(4) . . ? C6B C1B Ce2 132.6(4) . . ? C3B C2B C1B 109.6(6) . . ? C3B C2B Ce2 71.4(4) . . ? C1B C2B Ce2 80.6(4) . . ? C2B C3B C4B 107.4(6) . . ? C2B C3B Ce2 79.7(4) . . ? C4B C3B Ce2 76.1(4) . . ? C5B C4B C3B 107.8(6) . . ? C5B C4B Ce2 80.6(4) . . ? C3B C4B Ce2 74.3(3) . . ? C4B C5B C1B 108.5(6) . . ? C4B C5B Ce2 70.7(4) . . ? C1B C5B Ce2 78.8(4) . . ? C1B C6B C7B 112.6(6) . . ? C1B C6B C9B 112.6(6) . . ? C7B C6B C9B 109.2(6) . . ? C1B C6B C8B 107.2(5) . . ? C7B C6B C8B 107.7(6) . . ? C9B C6B C8B 107.1(6) . . ? C11B C10B C14B 107.3(6) . . ? C11B C10B C15B 124.9(6) . . ? C14B C10B C15B 127.1(7) . . ? C11B C10B Ce2 73.1(4) . . ? C14B C10B Ce2 76.8(4) . . ? C15B C10B Ce2 123.6(4) . . ? C10B C11B C12B 108.6(6) . . ? C10B C11B Ce2 78.6(4) . . ? C12B C11B Ce2 74.4(3) . . ? C13B C12B C11B 107.4(7) . . ? C13B C12B Ce2 77.1(4) . . ? C11B C12B Ce2 76.3(4) . . ? C12B C13B C14B 108.0(6) . . ? C12B C13B Ce2 74.1(3) . . ? C14B C13B Ce2 78.8(4) . . ? C13B C14B C10B 108.7(7) . . ? C13B C14B Ce2 72.9(4) . . ? C10B C14B Ce2 75.2(4) . . ? C18B C15B C10B 111.3(6) . . ? C18B C15B C17B 108.2(6) . . ? C10B C15B C17B 108.3(6) . . ? C18B C15B C16B 109.6(6) . . ? C10B C15B C16B 111.3(6) . . ? C17B C15B C16B 108.0(6) . . ? C20B C19B C23B 105.5(6) . . ? C20B C19B C24B 124.5(6) . . ? C23B C19B C24B 129.4(6) . . ? C20B C19B Ce2 71.0(4) . . ? C23B C19B Ce2 72.6(4) . . ? C24B C19B Ce2 127.2(5) . . ? C21B C20B C19B 108.9(6) . . ? C21B C20B Ce2 71.7(4) . . ? C19B C20B Ce2 81.5(4) . . ? C20B C21B C22B 108.8(7) . . ? C20B C21B Ce2 79.7(4) . . ? C22B C21B Ce2 78.0(4) . . ? C21B C22B C23B 106.4(6) . . ? C21B C22B Ce2 73.2(4) . . ? C23B C22B Ce2 79.2(4) . . ? C22B C23B C19B 110.1(6) . . ? C22B C23B Ce2 72.7(4) . . ? C19B C23B Ce2 79.8(4) . . ? C19B C24B C27B 113.5(6) . . ? C19B C24B C25B 110.2(6) . . ? C27B C24B C25B 109.4(6) . . ? C19B C24B C26B 108.9(6) . . ? C27B C24B C26B 107.3(6) . . ? C25B C24B C26B 107.3(6) . . ? N1B C28B C29B 123.5(6) . . ? N2B C29B C28B 120.3(6) . . ? N2B C29B C32B 116.8(6) . . ? C28B C29B C32B 122.9(6) . . ? N2B C30B C31B 120.5(6) . . ? N2B C30B C33B 119.2(6) . . ? C31B C30B C33B 120.1(6) . . ? N1B C31B C30B 123.8(6) . . ? #===END data_(Ce,SiMe~3~,dimethylpyrazine) _database_code_depnum_ccdc_archive 'CCDC 223539' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H47 Ce N2 Si3' _chemical_formula_weight 660.09 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3785(13) _cell_length_b 8.9945(9) _cell_length_c 32.191(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.433(7) _cell_angle_gamma 90.00 _cell_volume 3288.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22961 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method ? _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 1.514 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 22961 _diffrn_reflns_av_R_equivalents 0.1131 _diffrn_reflns_av_sigmaI/netI 0.1323 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6089 _reflns_number_gt 2601 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0619P)^2^+10.8171P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6089 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2243 _refine_ls_R_factor_gt 0.0991 _refine_ls_wR_factor_ref 0.2643 _refine_ls_wR_factor_gt 0.2132 _refine_ls_goodness_of_fit_ref 1.385 _refine_ls_restrained_S_all 1.789 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.877 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.127 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 Ce Ce 0.61668(9) 0.50409(13) 0.12463(4) 0.0650(5) Uani 1 1 d . . . Si1 Si 0.9817(6) 0.4085(8) 0.1604(2) 0.0788(19) Uani 1 1 d . . . Si2 Si 0.4644(7) 0.4633(8) 0.2378(2) 0.097(2) Uani 1 1 d . . . Si3 Si 0.3603(6) 0.8238(7) 0.0753(2) 0.0802(19) Uani 1 1 d . . . N1 N 0.7371(14) 0.6717(16) 0.0726(5) 0.065(4) Uani 1 1 d . . . N2 N 0.9008(12) 0.7933(15) 0.0201(5) 0.051(4) Uani 1 1 d . . . C1 C 0.8346(17) 0.345(2) 0.1389(6) 0.064(5) Uani 1 1 d . . . C2 C 0.749(2) 0.266(3) 0.1615(8) 0.090(7) Uani 1 1 d . . . H2 H 0.7463 0.2589 0.1902 0.108 Uiso 1 1 calc R . . C3 C 0.673(2) 0.206(2) 0.1326(7) 0.080(6) Uani 1 1 d . . . H3 H 0.6079 0.1491 0.1391 0.096 Uiso 1 1 calc R . . C4 C 0.7019(18) 0.237(2) 0.0909(7) 0.065(6) Uani 1 1 d . . . H4 H 0.6619 0.2073 0.0663 0.078 Uiso 1 1 calc R . . C5 C 0.8062(16) 0.323(2) 0.0960(6) 0.059(5) Uani 1 1 d . . . H5 H 0.8490 0.3596 0.0745 0.071 Uiso 1 1 calc R . . C6 C 0.984(2) 0.433(3) 0.2184(7) 0.106(8) Uani 1 1 d . . . H6A H 0.9415 0.5218 0.2247 0.159 Uiso 1 1 calc R . . H6B H 1.0639 0.4415 0.2294 0.159 Uiso 1 1 calc R . . H6C H 0.9474 0.3489 0.2306 0.159 Uiso 1 1 calc R . . C7 C 1.0988(19) 0.266(2) 0.1490(7) 0.083(7) Uani 1 1 d . . . H7A H 1.0846 0.1758 0.1638 0.125 Uiso 1 1 calc R . . H7B H 1.1751 0.3043 0.1577 0.125 Uiso 1 1 calc R . . H7C H 1.0958 0.2459 0.1197 0.125 Uiso 1 1 calc R . . C8 C 1.0295(18) 0.583(2) 0.1358(6) 0.078(6) Uani 1 1 d . . . H8A H 1.0117 0.5779 0.1063 0.117 Uiso 1 1 calc R . . H8B H 1.1128 0.5955 0.1412 0.117 Uiso 1 1 calc R . . H8C H 0.9887 0.6657 0.1471 0.117 Uiso 1 1 calc R . . C9 C 0.558(2) 0.581(3) 0.2063(7) 0.089(7) Uani 1 1 d . . . C10 C 0.687(2) 0.569(3) 0.2078(8) 0.102(8) Uani 1 1 d . . . H10 H 0.7351 0.4967 0.2206 0.122 Uiso 1 1 calc R . . C11 C 0.721(3) 0.693(3) 0.1853(8) 0.105(8) Uani 1 1 d . . . H11 H 0.7997 0.7175 0.1822 0.126 Uiso 1 1 calc R . . C12 C 0.630(2) 0.776(3) 0.1682(7) 0.093(7) Uani 1 1 d . . . H12 H 0.6333 0.8595 0.1515 0.111 Uiso 1 1 calc R . . C13 C 0.525(2) 0.702(3) 0.1822(6) 0.077(6) Uani 1 1 d . . . H13 H 0.4483 0.7325 0.1758 0.093 Uiso 1 1 calc R . . C14 C 0.442(3) 0.278(3) 0.2152(9) 0.146(12) Uani 1 1 d . . . H14A H 0.3677 0.2395 0.2224 0.218 Uiso 1 1 calc R . . H14B H 0.5041 0.2131 0.2257 0.218 Uiso 1 1 calc R . . H14C H 0.4438 0.2845 0.1854 0.218 Uiso 1 1 calc R . . C15 C 0.538(3) 0.447(3) 0.2913(8) 0.131(10) Uani 1 1 d . . . H15A H 0.5354 0.5418 0.3051 0.197 Uiso 1 1 calc R . . H15B H 0.6181 0.4172 0.2893 0.197 Uiso 1 1 calc R . . H15C H 0.4972 0.3746 0.3069 0.197 Uiso 1 1 calc R . . C16 C 0.318(2) 0.552(3) 0.2397(7) 0.094(7) Uani 1 1 d . . . H16A H 0.2801 0.5546 0.2122 0.142 Uiso 1 1 calc R . . H16B H 0.3270 0.6515 0.2502 0.142 Uiso 1 1 calc R . . H16C H 0.2703 0.4958 0.2577 0.142 Uiso 1 1 calc R . . C17 C 0.4069(17) 0.6235(19) 0.0830(6) 0.057(5) Uani 1 1 d . . . C18 C 0.3674(16) 0.517(2) 0.1106(6) 0.066(5) Uani 1 1 d . . . H18 H 0.3254 0.5374 0.1338 0.079 Uiso 1 1 calc R . . C19 C 0.4007(17) 0.376(2) 0.0980(6) 0.062(5) Uani 1 1 d . . . H19 H 0.3876 0.2868 0.1116 0.075 Uiso 1 1 calc R . . C20 C 0.4582(16) 0.3937(19) 0.0607(6) 0.059(5) Uani 1 1 d . . . H20 H 0.4895 0.3176 0.0453 0.070 Uiso 1 1 calc R . . C21 C 0.4600(16) 0.5421(18) 0.0512(6) 0.060(5) Uani 1 1 d . . . H21 H 0.4910 0.5831 0.0276 0.072 Uiso 1 1 calc R . . C22 C 0.244(2) 0.831(2) 0.0333(7) 0.088(7) Uani 1 1 d . . . H22A H 0.2750 0.7974 0.0079 0.132 Uiso 1 1 calc R . . H22B H 0.2170 0.9320 0.0299 0.132 Uiso 1 1 calc R . . H22C H 0.1798 0.7690 0.0403 0.132 Uiso 1 1 calc R . . C23 C 0.488(2) 0.937(2) 0.0570(8) 0.094(7) Uani 1 1 d . . . H23A H 0.5496 0.9400 0.0786 0.141 Uiso 1 1 calc R . . H23B H 0.4614 1.0361 0.0506 0.141 Uiso 1 1 calc R . . H23C H 0.5163 0.8917 0.0326 0.141 Uiso 1 1 calc R . . C24 C 0.304(2) 0.911(3) 0.1226(7) 0.106(8) Uani 1 1 d . . . H24A H 0.2541 0.8416 0.1358 0.158 Uiso 1 1 calc R . . H24B H 0.2600 0.9984 0.1148 0.158 Uiso 1 1 calc R . . H24C H 0.3692 0.9371 0.1415 0.158 Uiso 1 1 calc R . . C25 C 0.7574(16) 0.611(2) 0.0350(6) 0.060(5) Uani 1 1 d . . . H25 H 0.7149 0.5274 0.0263 0.072 Uiso 1 1 calc R . . C26 C 0.8385(15) 0.6692(17) 0.0090(6) 0.049(4) Uani 1 1 d . . . C27 C 0.8820(16) 0.8549(19) 0.0572(6) 0.054(5) Uani 1 1 d . . . C28 C 0.7981(15) 0.7959(19) 0.0825(6) 0.052(5) Uani 1 1 d . . . H28 H 0.7838 0.8446 0.1071 0.063 Uiso 1 1 calc R . . C29 C 0.8629(18) 0.596(2) -0.0311(6) 0.064(5) Uani 1 1 d . . . H29A H 0.9320 0.6388 -0.0419 0.096 Uiso 1 1 calc R . . H29B H 0.7970 0.6100 -0.0507 0.096 Uiso 1 1 calc R . . H29C H 0.8753 0.4914 -0.0265 0.096 Uiso 1 1 calc R . . C30 C 0.9537(16) 0.992(2) 0.0694(6) 0.069(5) Uani 1 1 d . . . H30A H 1.0283 0.9627 0.0823 0.104 Uiso 1 1 calc R . . H30B H 0.9118 1.0508 0.0886 0.104 Uiso 1 1 calc R . . H30C H 0.9662 1.0501 0.0450 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.0464(6) 0.0504(6) 0.1031(8) -0.0057(6) 0.0463(5) -0.0038(6) Si1 0.077(2) 0.082(2) 0.078(2) -0.0013(12) 0.0083(13) 0.0003(12) Si2 0.093(3) 0.099(3) 0.098(3) 0.0031(13) 0.0095(13) 0.0022(13) Si3 0.078(2) 0.077(2) 0.087(2) -0.0006(12) 0.0091(13) 0.0007(12) N1 0.052(8) 0.049(8) 0.096(9) -0.005(7) 0.034(8) -0.007(7) N2 0.035(7) 0.044(7) 0.077(9) 0.007(7) 0.019(7) -0.007(6) C1 0.051(9) 0.071(10) 0.075(10) 0.003(8) 0.034(8) 0.000(8) C2 0.084(12) 0.094(12) 0.095(12) 0.008(10) 0.027(10) 0.009(10) C3 0.064(10) 0.076(10) 0.102(12) 0.003(10) 0.029(10) 0.001(9) C4 0.053(10) 0.057(9) 0.084(11) -0.023(8) -0.001(9) 0.002(8) C5 0.045(9) 0.055(9) 0.080(10) -0.009(8) 0.022(8) 0.006(8) C6 0.096(13) 0.125(13) 0.097(12) -0.007(10) 0.017(10) 0.003(10) C7 0.071(11) 0.098(11) 0.082(11) -0.003(9) 0.021(9) 0.004(9) C8 0.061(10) 0.090(11) 0.084(11) -0.015(9) 0.029(9) 0.003(9) C9 0.074(11) 0.103(12) 0.093(11) -0.013(10) 0.031(10) 0.007(10) C10 0.084(12) 0.112(12) 0.110(12) -0.017(10) 0.021(10) 0.009(10) C11 0.104(13) 0.109(13) 0.104(12) -0.026(10) 0.023(10) -0.002(11) C12 0.096(12) 0.089(11) 0.097(12) -0.023(10) 0.046(10) -0.008(10) C13 0.066(11) 0.088(11) 0.082(11) -0.009(9) 0.036(9) 0.000(9) C14 0.122(15) 0.163(16) 0.154(15) 0.022(12) 0.026(11) -0.002(12) C15 0.112(14) 0.148(15) 0.135(14) 0.025(11) 0.015(11) 0.018(11) C16 0.075(11) 0.119(12) 0.093(11) 0.016(10) 0.033(9) 0.009(10) C17 0.051(10) 0.037(8) 0.086(10) -0.004(8) 0.023(9) -0.002(7) C18 0.049(9) 0.056(10) 0.095(10) -0.008(9) 0.032(8) -0.001(8) C19 0.052(10) 0.052(9) 0.085(10) -0.005(8) 0.022(9) -0.005(8) C20 0.050(9) 0.044(8) 0.085(10) 0.001(8) 0.025(8) 0.009(7) C21 0.048(9) 0.048(9) 0.088(10) 0.008(8) 0.030(8) 0.009(7) C22 0.084(12) 0.068(10) 0.115(12) 0.007(9) 0.030(10) 0.007(9) C23 0.083(12) 0.071(10) 0.131(12) 0.014(10) 0.024(10) -0.013(9) C24 0.101(13) 0.094(12) 0.123(13) -0.021(10) 0.016(10) 0.003(10) C25 0.050(9) 0.053(9) 0.079(10) -0.003(8) 0.019(8) -0.015(8) C26 0.039(8) 0.035(7) 0.074(9) 0.007(7) 0.019(8) -0.001(7) C27 0.041(9) 0.049(8) 0.074(10) -0.003(8) 0.015(8) 0.003(7) C28 0.040(9) 0.046(8) 0.073(10) -0.013(8) 0.021(8) -0.004(7) C29 0.066(10) 0.051(9) 0.078(10) 0.006(8) 0.023(8) 0.005(8) C30 0.056(9) 0.057(9) 0.096(10) 0.001(9) 0.017(8) -0.011(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce N1 2.689(15) . ? Ce C3 2.77(2) . ? Ce C11 2.80(2) . ? Ce C19 2.802(19) . ? Ce C10 2.81(3) . ? Ce C13 2.81(2) . ? Ce C12 2.82(2) . ? Ce C2 2.83(2) . ? Ce C4 2.833(18) . ? Ce C20 2.833(19) . ? Ce C9 2.84(2) . ? Ce C18 2.847(18) . ? Ce C17 2.875(18) . ? Ce C1 2.88(2) . ? Ce C5 2.90(2) . ? Ce C21 2.90(2) . ? Si1 C8 1.85(2) . ? Si1 C1 1.86(2) . ? Si1 C6 1.88(2) . ? Si1 C7 1.90(2) . ? Si2 C14 1.83(3) . ? Si2 C9 1.85(3) . ? Si2 C16 1.85(2) . ? Si2 C15 1.87(3) . ? Si3 C22 1.83(2) . ? Si3 C24 1.86(2) . ? Si3 C17 1.891(18) . ? Si3 C23 1.89(2) . ? N1 C28 1.34(2) . ? N1 C25 1.36(2) . ? N2 C27 1.35(2) . ? N2 C26 1.36(2) . ? C1 C5 1.41(2) . ? C1 C2 1.44(3) . ? C2 C3 1.35(3) . ? C3 C4 1.43(3) . ? C4 C5 1.42(2) . ? C9 C13 1.37(3) . ? C9 C10 1.48(3) . ? C10 C11 1.39(3) . ? C11 C12 1.37(3) . ? C12 C13 1.45(3) . ? C17 C18 1.40(2) . ? C17 C21 1.42(2) . ? C18 C19 1.39(2) . ? C19 C20 1.41(2) . ? C20 C21 1.37(2) . ? C25 C26 1.38(2) . ? C26 C29 1.49(2) . ? C27 C28 1.39(2) . ? C27 C30 1.52(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ce C3 118.6(6) . . ? N1 Ce C11 83.3(7) . . ? C3 Ce C11 116.0(8) . . ? N1 Ce C19 120.7(6) . . ? C3 Ce C19 79.8(7) . . ? C11 Ce C19 142.3(7) . . ? N1 Ce C10 110.4(7) . . ? C3 Ce C10 93.6(8) . . ? C11 Ce C10 28.8(7) . . ? C19 Ce C10 125.0(7) . . ? N1 Ce C13 106.1(6) . . ? C3 Ce C13 130.2(7) . . ? C11 Ce C13 46.7(8) . . ? C19 Ce C13 96.3(6) . . ? C10 Ce C13 48.4(7) . . ? N1 Ce C12 79.1(6) . . ? C3 Ce C12 142.2(8) . . ? C11 Ce C12 28.2(7) . . ? C19 Ce C12 121.9(7) . . ? C10 Ce C12 48.8(8) . . ? C13 Ce C12 29.9(6) . . ? N1 Ce C2 114.0(6) . . ? C3 Ce C2 27.8(6) . . ? C11 Ce C2 88.5(8) . . ? C19 Ce C2 104.6(7) . . ? C10 Ce C2 69.2(8) . . ? C13 Ce C2 114.2(7) . . ? C12 Ce C2 115.8(8) . . ? N1 Ce C4 92.2(5) . . ? C3 Ce C4 29.5(5) . . ? C11 Ce C4 129.9(7) . . ? C19 Ce C4 81.2(6) . . ? C10 Ce C4 117.2(7) . . ? C13 Ce C4 159.7(7) . . ? C12 Ce C4 156.6(7) . . ? C2 Ce C4 48.3(7) . . ? N1 Ce C20 94.0(5) . . ? C3 Ce C20 82.0(6) . . ? C11 Ce C20 160.9(7) . . ? C19 Ce C20 29.0(5) . . ? C10 Ce C20 153.9(7) . . ? C13 Ce C20 117.1(6) . . ? C12 Ce C20 132.7(7) . . ? C2 Ce C20 109.8(6) . . ? C4 Ce C20 69.0(5) . . ? N1 Ce C9 126.7(6) . . ? C3 Ce C9 102.5(7) . . ? C11 Ce C9 47.1(8) . . ? C19 Ce C9 97.6(7) . . ? C10 Ce C9 30.3(6) . . ? C13 Ce C9 28.1(6) . . ? C12 Ce C9 48.3(7) . . ? C2 Ce C9 86.9(8) . . ? C4 Ce C9 131.9(7) . . ? C20 Ce C9 125.7(6) . . ? N1 Ce C18 114.7(5) . . ? C3 Ce C18 106.0(6) . . ? C11 Ce C18 117.6(7) . . ? C19 Ce C18 28.5(5) . . ? C10 Ce C18 111.6(7) . . ? C13 Ce C18 71.0(6) . . ? C12 Ce C18 93.8(7) . . ? C2 Ce C18 126.6(7) . . ? C4 Ce C18 109.5(6) . . ? C20 Ce C18 46.7(5) . . ? C9 Ce C18 81.3(7) . . ? C8 Si1 C1 112.4(9) . . ? C8 Si1 C6 109.7(11) . . ? C1 Si1 C6 111.3(11) . . ? C8 Si1 C7 105.1(10) . . ? C1 Si1 C7 110.3(10) . . ? C6 Si1 C7 107.7(11) . . ? C14 Si2 C9 111.9(13) . . ? C14 Si2 C16 107.6(14) . . ? C9 Si2 C16 108.6(11) . . ? C14 Si2 C15 109.9(14) . . ? C9 Si2 C15 108.0(13) . . ? C16 Si2 C15 110.8(12) . . ? C22 Si3 C24 108.6(11) . . ? C22 Si3 C17 108.4(9) . . ? C24 Si3 C17 113.8(11) . . ? C22 Si3 C23 106.3(11) . . ? C24 Si3 C23 109.7(12) . . ? C17 Si3 C23 109.8(10) . . ? C28 N1 C25 115.5(15) . . ? C28 N1 Ce 126.5(13) . . ? C25 N1 Ce 116.8(11) . . ? C27 N2 C26 117.6(15) . . ? C5 C1 C2 107.6(19) . . ? C5 C1 Si1 123.7(14) . . ? C2 C1 Si1 125.9(17) . . ? C5 C1 Ce 76.6(11) . . ? C2 C1 Ce 73.8(12) . . ? Si1 C1 Ce 130.9(9) . . ? C3 C2 C1 106(2) . . ? C3 C2 Ce 73.4(14) . . ? C1 C2 Ce 77.1(13) . . ? C2 C3 C4 113(2) . . ? C2 C3 Ce 78.8(14) . . ? C4 C3 Ce 77.7(12) . . ? C5 C4 C3 103.8(18) . . ? C5 C4 Ce 78.1(10) . . ? C3 C4 Ce 72.7(11) . . ? C1 C5 C4 109.3(18) . . ? C1 C5 Ce 75.0(10) . . ? C4 C5 Ce 73.2(10) . . ? C13 C9 C10 108(2) . . ? C13 C9 Si2 128.4(19) . . ? C10 C9 Si2 123(2) . . ? C13 C9 Ce 74.9(13) . . ? C10 C9 Ce 73.8(13) . . ? Si2 C9 Ce 122.9(12) . . ? C11 C10 C9 103(3) . . ? C11 C10 Ce 75.2(15) . . ? C9 C10 Ce 75.9(14) . . ? C12 C11 C10 114(3) . . ? C12 C11 Ce 76.5(15) . . ? C10 C11 Ce 76.0(15) . . ? C11 C12 C13 104(2) . . ? C11 C12 Ce 75.3(15) . . ? C13 C12 Ce 75.0(12) . . ? C9 C13 C12 110(2) . . ? C9 C13 Ce 77.0(13) . . ? C12 C13 Ce 75.1(12) . . ? C18 C17 C21 105.8(15) . . ? C18 C17 Si3 129.5(15) . . ? C21 C17 Si3 121.7(14) . . ? C18 C17 Ce 74.8(11) . . ? C21 C17 Ce 76.6(11) . . ? Si3 C17 Ce 129.4(9) . . ? C19 C18 C17 109.6(17) . . ? C19 C18 Ce 73.9(11) . . ? C17 C18 Ce 76.9(11) . . ? C18 C19 C20 107.1(17) . . ? C18 C19 Ce 77.6(11) . . ? C20 C19 Ce 76.8(11) . . ? C21 C20 C19 108.4(17) . . ? C21 C20 Ce 78.7(12) . . ? C19 C20 Ce 74.3(11) . . ? C20 C21 C17 109.0(17) . . ? C20 C21 Ce 73.6(12) . . ? C17 C21 Ce 74.9(11) . . ? N1 C25 C26 122.9(17) . . ? N2 C26 C25 120.5(16) . . ? N2 C26 C29 118.0(15) . . ? C25 C26 C29 121.5(16) . . ? N2 C27 C28 120.7(16) . . ? N2 C27 C30 116.9(16) . . ? C28 C27 C30 122.3(17) . . ? N1 C28 C27 122.7(17) . . ? #===END data_(U,SiMe~3~,dimethylpyrazine) _database_code_depnum_ccdc_archive 'CCDC 223540' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H47 N2 Si3 U' _chemical_formula_weight 758.00 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 8.8397(9) _cell_length_b 11.2849(8) _cell_length_c 17.2078(15) _cell_angle_alpha 71.846(6) _cell_angle_beta 80.696(5) _cell_angle_gamma 89.117(6) _cell_volume 1608.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11093 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method ? _exptl_crystal_F_000 750 _exptl_absorpt_coefficient_mu 5.178 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.152 _exptl_absorpt_correction_T_max 0.608 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 11093 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0936 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5626 _reflns_number_gt 4912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0396P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5626 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 1.154 _refine_diff_density_min -1.312 _refine_diff_density_rms 0.174 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 U U 0.91919(3) 0.97513(2) 0.747065(14) 0.01677(10) Uani 1 1 d . . . Si1 Si 1.2679(2) 0.76586(17) 0.65262(11) 0.0204(4) Uani 1 1 d . . . Si2 Si 0.7403(2) 0.72898(18) 0.97483(12) 0.0241(4) Uani 1 1 d . . . Si3 Si 0.8171(2) 1.30427(17) 0.82192(12) 0.0232(4) Uani 1 1 d . . . N1 N 1.1307(6) 1.1435(5) 0.6487(3) 0.0225(12) Uani 1 1 d . . . N2 N 1.2882(7) 1.3682(5) 0.5516(4) 0.0281(14) Uani 1 1 d . . . C1 C 1.0621(8) 0.8074(6) 0.6650(4) 0.0199(14) Uani 1 1 d . . . C2 C 0.9299(8) 0.7411(6) 0.7202(4) 0.0227(15) Uani 1 1 d . . . H2 H 0.9315 0.6724 0.7671 0.027 Uiso 1 1 calc R . . C3 C 0.7966(8) 0.7973(6) 0.6919(4) 0.0228(14) Uani 1 1 d . . . H3 H 0.6958 0.7739 0.7173 0.027 Uiso 1 1 calc R . . C4 C 0.8449(8) 0.8950(6) 0.6181(4) 0.0208(14) Uani 1 1 d . . . H4 H 0.7808 0.9459 0.5850 0.025 Uiso 1 1 calc R . . C5 C 1.0045(7) 0.9028(6) 0.6030(4) 0.0184(13) Uani 1 1 d . . . H5 H 1.0641 0.9619 0.5588 0.022 Uiso 1 1 calc R . . C6 C 1.3938(8) 0.9103(7) 0.6129(5) 0.0288(16) Uani 1 1 d . . . H6A H 1.3820 0.9537 0.6533 0.043 Uiso 1 1 calc R . . H6B H 1.3655 0.9633 0.5622 0.043 Uiso 1 1 calc R . . H6C H 1.4988 0.8883 0.6026 0.043 Uiso 1 1 calc R . . C7 C 1.2972(8) 0.6855(8) 0.5713(5) 0.0319(17) Uani 1 1 d . . . H7A H 1.4038 0.6683 0.5599 0.048 Uiso 1 1 calc R . . H7B H 1.2657 0.7385 0.5215 0.048 Uiso 1 1 calc R . . H7C H 1.2372 0.6087 0.5909 0.048 Uiso 1 1 calc R . . C8 C 1.3262(8) 0.6595(7) 0.7496(5) 0.0293(16) Uani 1 1 d . . . H8A H 1.3232 0.7030 0.7896 0.044 Uiso 1 1 calc R . . H8B H 1.4284 0.6329 0.7372 0.044 Uiso 1 1 calc R . . H8C H 1.2568 0.5879 0.7718 0.044 Uiso 1 1 calc R . . C9 C 0.9105(8) 0.8323(6) 0.9120(4) 0.0198(14) Uani 1 1 d . . . C10 C 1.0488(8) 0.8000(6) 0.8703(4) 0.0205(14) Uani 1 1 d . . . H10 H 1.0675 0.7228 0.8627 0.025 Uiso 1 1 calc R . . C11 C 1.1518(8) 0.9013(7) 0.8427(4) 0.0237(15) Uani 1 1 d . . . H11 H 1.2502 0.9039 0.8131 0.028 Uiso 1 1 calc R . . C12 C 1.0811(8) 1.0005(6) 0.8674(4) 0.0234(15) Uani 1 1 d . . . H12 H 1.1240 1.0799 0.8567 0.028 Uiso 1 1 calc R . . C13 C 0.9342(8) 0.9562(6) 0.9112(4) 0.0202(14) Uani 1 1 d . . . H13 H 0.8637 1.0013 0.9357 0.024 Uiso 1 1 calc R . . C14 C 0.5829(9) 0.7185(8) 0.9168(5) 0.0352(18) Uani 1 1 d . . . H14A H 0.6232 0.6916 0.8700 0.053 Uiso 1 1 calc R . . H14B H 0.5397 0.7989 0.8977 0.053 Uiso 1 1 calc R . . H14C H 0.5047 0.6595 0.9526 0.053 Uiso 1 1 calc R . . C15 C 0.6543(10) 0.7962(9) 1.0577(6) 0.052(3) Uani 1 1 d . . . H15A H 0.5640 0.7475 1.0893 0.078 Uiso 1 1 calc R . . H15B H 0.6272 0.8807 1.0327 0.078 Uiso 1 1 calc R . . H15C H 0.7273 0.7949 1.0935 0.078 Uiso 1 1 calc R . . C16 C 0.8038(11) 0.5671(8) 1.0184(7) 0.054(3) Uani 1 1 d . . . H16A H 0.8706 0.5657 1.0575 0.082 Uiso 1 1 calc R . . H16B H 0.8578 0.5398 0.9744 0.082 Uiso 1 1 calc R . . H16C H 0.7159 0.5125 1.0459 0.082 Uiso 1 1 calc R . . C17 C 0.7596(7) 1.1860(6) 0.7752(4) 0.0198(14) Uani 1 1 d . . . C18 C 0.6586(8) 1.0790(6) 0.8149(4) 0.0230(14) Uani 1 1 d . . . H18 H 0.6275 1.0434 0.8718 0.028 Uiso 1 1 calc R . . C19 C 0.6140(7) 1.0367(6) 0.7520(4) 0.0238(15) Uani 1 1 d . . . H19 H 0.5494 0.9679 0.7606 0.029 Uiso 1 1 calc R . . C20 C 0.6832(7) 1.1154(6) 0.6755(5) 0.0237(15) Uani 1 1 d . . . H20 H 0.6720 1.1092 0.6241 0.028 Uiso 1 1 calc R . . C21 C 0.7733(7) 1.2064(6) 0.6893(4) 0.0226(15) Uani 1 1 d . . . H21 H 0.8325 1.2699 0.6481 0.027 Uiso 1 1 calc R . . C22 C 0.8061(9) 1.2428(7) 0.9368(5) 0.0331(18) Uani 1 1 d . . . H22A H 0.8882 1.1872 0.9499 0.050 Uiso 1 1 calc R . . H22B H 0.7095 1.1985 0.9613 0.050 Uiso 1 1 calc R . . H22C H 0.8149 1.3110 0.9581 0.050 Uiso 1 1 calc R . . C23 C 1.0127(8) 1.3720(7) 0.7717(5) 0.0320(17) Uani 1 1 d . . . H23A H 1.0862 1.3080 0.7830 0.048 Uiso 1 1 calc R . . H23B H 1.0369 1.4369 0.7934 0.048 Uiso 1 1 calc R . . H23C H 1.0158 1.4062 0.7129 0.048 Uiso 1 1 calc R . . C24 C 0.6838(8) 1.4371(6) 0.7984(5) 0.0285(16) Uani 1 1 d . . . H24A H 0.7120 1.4996 0.8212 0.043 Uiso 1 1 calc R . . H24B H 0.5805 1.4069 0.8226 0.043 Uiso 1 1 calc R . . H24C H 0.6907 1.4728 0.7395 0.043 Uiso 1 1 calc R . . C25 C 1.2467(8) 1.1915(6) 0.6725(4) 0.0226(14) Uani 1 1 d . . . H25 H 1.2780 1.1475 0.7223 0.027 Uiso 1 1 calc R . . C26 C 1.3214(8) 1.3043(6) 0.6256(4) 0.0231(15) Uani 1 1 d . . . C27 C 1.1765(8) 1.3203(6) 0.5233(4) 0.0247(15) Uani 1 1 d . . . C28 C 1.0990(8) 1.2099(6) 0.5718(4) 0.0223(14) Uani 1 1 d . . . H28 H 1.0220 1.1792 0.5515 0.027 Uiso 1 1 calc R . . C29 C 1.4419(9) 1.3600(7) 0.6583(5) 0.0338(18) Uani 1 1 d . . . H29A H 1.5245 1.3972 0.6140 0.051 Uiso 1 1 calc R . . H29B H 1.4805 1.2956 0.7009 0.051 Uiso 1 1 calc R . . H29C H 1.3972 1.4227 0.6810 0.051 Uiso 1 1 calc R . . C30 C 1.1403(10) 1.3905(7) 0.4414(5) 0.0376(19) Uani 1 1 d . . . H30A H 1.0998 1.4693 0.4430 0.056 Uiso 1 1 calc R . . H30B H 1.0655 1.3437 0.4271 0.056 Uiso 1 1 calc R . . H30C H 1.2318 1.4044 0.4008 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.01798(14) 0.01607(15) 0.01693(14) -0.00591(11) -0.00331(9) 0.00086(9) Si1 0.0193(9) 0.0200(9) 0.0217(9) -0.0063(8) -0.0034(7) 0.0031(7) Si2 0.0278(11) 0.0245(10) 0.0188(9) -0.0069(8) 0.0001(8) -0.0046(8) Si3 0.0241(10) 0.0209(10) 0.0266(10) -0.0109(9) -0.0032(8) 0.0033(7) N1 0.022(3) 0.023(3) 0.021(3) -0.005(3) -0.003(2) 0.003(2) N2 0.034(4) 0.021(3) 0.030(3) -0.014(3) 0.004(3) -0.002(3) C1 0.023(3) 0.016(3) 0.024(3) -0.009(3) -0.008(3) -0.004(3) C2 0.025(4) 0.019(3) 0.028(4) -0.016(3) 0.003(3) -0.008(3) C3 0.027(4) 0.023(3) 0.024(3) -0.014(3) -0.005(3) 0.002(3) C4 0.022(3) 0.026(4) 0.018(3) -0.012(3) -0.002(3) 0.003(3) C5 0.018(3) 0.021(3) 0.016(3) -0.007(3) -0.001(3) -0.001(3) C6 0.026(4) 0.027(4) 0.030(4) -0.004(3) -0.006(3) 0.003(3) C7 0.022(4) 0.048(5) 0.034(4) -0.024(4) -0.008(3) 0.010(3) C8 0.025(4) 0.031(4) 0.033(4) -0.008(3) -0.011(3) 0.009(3) C9 0.020(3) 0.024(3) 0.017(3) -0.006(3) -0.006(3) 0.000(3) C10 0.021(4) 0.024(4) 0.018(3) -0.009(3) -0.002(3) 0.002(3) C11 0.016(3) 0.039(4) 0.016(3) -0.006(3) -0.006(3) -0.004(3) C12 0.029(4) 0.025(4) 0.017(3) -0.006(3) -0.006(3) -0.008(3) C13 0.029(4) 0.023(4) 0.012(3) -0.008(3) -0.008(3) 0.004(3) C14 0.029(4) 0.041(5) 0.035(4) -0.011(4) -0.006(3) -0.010(3) C15 0.039(5) 0.081(7) 0.044(5) -0.041(5) 0.016(4) -0.022(5) C16 0.037(5) 0.038(5) 0.068(7) 0.012(5) -0.006(5) -0.012(4) C17 0.016(3) 0.021(3) 0.025(3) -0.011(3) -0.003(3) 0.005(3) C18 0.022(4) 0.022(4) 0.026(4) -0.009(3) -0.003(3) 0.004(3) C19 0.016(3) 0.027(4) 0.034(4) -0.018(3) -0.002(3) 0.001(3) C20 0.016(3) 0.026(4) 0.036(4) -0.014(3) -0.015(3) 0.009(3) C21 0.016(3) 0.026(4) 0.030(4) -0.016(3) -0.003(3) 0.005(3) C22 0.040(5) 0.029(4) 0.036(4) -0.018(4) -0.008(4) 0.009(3) C23 0.026(4) 0.032(4) 0.043(4) -0.020(4) -0.001(3) 0.001(3) C24 0.029(4) 0.018(3) 0.033(4) -0.005(3) 0.001(3) -0.001(3) C25 0.021(3) 0.023(4) 0.026(4) -0.011(3) -0.003(3) 0.003(3) C26 0.023(4) 0.021(4) 0.031(4) -0.017(3) -0.005(3) 0.007(3) C27 0.028(4) 0.018(3) 0.028(4) -0.010(3) 0.001(3) -0.001(3) C28 0.019(3) 0.026(4) 0.027(4) -0.015(3) -0.003(3) 0.003(3) C29 0.030(4) 0.020(4) 0.053(5) -0.012(4) -0.009(4) 0.001(3) C30 0.054(5) 0.027(4) 0.033(4) -0.007(4) -0.013(4) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U N1 2.656(6) . ? U C19 2.770(6) . ? U C3 2.774(6) . ? U C9 2.782(7) . ? U C12 2.786(6) . ? U C13 2.790(6) . ? U C11 2.796(6) . ? U C10 2.796(7) . ? U C20 2.809(6) . ? U C4 2.813(6) . ? U C2 2.817(6) . ? U C18 2.819(6) . ? U C5 2.831(6) . ? U C21 2.856(6) . ? U C1 2.862(6) . ? U C17 2.878(6) . ? Si1 C6 1.865(7) . ? Si1 C1 1.867(7) . ? Si1 C8 1.871(7) . ? Si1 C7 1.874(7) . ? Si2 C16 1.861(9) . ? Si2 C14 1.865(8) . ? Si2 C15 1.868(8) . ? Si2 C9 1.880(7) . ? Si3 C23 1.861(8) . ? Si3 C22 1.866(8) . ? Si3 C17 1.872(6) . ? Si3 C24 1.877(7) . ? N1 C25 1.344(9) . ? N1 C28 1.373(9) . ? N2 C26 1.329(9) . ? N2 C27 1.357(9) . ? C1 C5 1.414(9) . ? C1 C2 1.433(9) . ? C2 C3 1.413(10) . ? C3 C4 1.405(10) . ? C4 C5 1.392(9) . ? C9 C13 1.413(9) . ? C9 C10 1.416(9) . ? C10 C11 1.384(10) . ? C11 C12 1.419(10) . ? C12 C13 1.404(10) . ? C17 C21 1.409(9) . ? C17 C18 1.430(9) . ? C18 C19 1.422(9) . ? C19 C20 1.387(10) . ? C20 C21 1.408(9) . ? C25 C26 1.386(10) . ? C26 C29 1.511(10) . ? C27 C28 1.383(10) . ? C27 C30 1.468(10) . ? 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 N1 U C19 118.22(18) . . ? N1 U C3 121.18(19) . . ? C19 U C3 77.52(19) . . ? N1 U C9 129.01(18) . . ? C19 U C9 99.5(2) . . ? C3 U C9 98.4(2) . . ? N1 U C12 81.67(19) . . ? C19 U C12 120.46(19) . . ? C3 U C12 142.2(2) . . ? C9 U C12 48.71(19) . . ? N1 U C13 108.40(18) . . ? C19 U C13 96.56(19) . . ? C3 U C13 126.6(2) . . ? C9 U C13 29.38(18) . . ? C12 U C13 29.2(2) . . ? N1 U C11 83.35(19) . . ? C19 U C11 144.2(2) . . ? C3 U C11 117.3(2) . . ? C9 U C11 48.4(2) . . ? C12 U C11 29.4(2) . . ? C13 U C11 47.97(19) . . ? N1 U C10 110.51(18) . . ? C19 U C10 127.3(2) . . ? C3 U C10 94.29(19) . . ? C9 U C10 29.41(18) . . ? C12 U C10 47.96(19) . . ? C13 U C10 47.76(18) . . ? C11 U C10 28.7(2) . . ? N1 U C20 91.45(19) . . ? C19 U C20 28.8(2) . . ? C3 U C20 81.68(19) . . ? C9 U C20 127.5(2) . . ? C12 U C20 131.0(2) . . ? C13 U C20 117.2(2) . . ? C11 U C20 160.2(2) . . ? C10 U C20 156.0(2) . . ? N1 U C4 94.32(18) . . ? C19 U C4 79.33(19) . . ? C3 U C4 29.1(2) . . ? C9 U C4 127.18(19) . . ? C12 U C4 159.3(2) . . ? C13 U C4 155.8(2) . . ? C11 U C4 130.1(2) . . ? C10 U C4 116.71(19) . . ? C20 U C4 69.12(19) . . ? N1 U C2 115.13(18) . . ? C19 U C2 104.74(19) . . ? C3 U C2 29.3(2) . . ? C9 U C2 83.5(2) . . ? C12 U C2 116.1(2) . . ? C13 U C2 112.4(2) . . ? C11 U C2 88.6(2) . . ? C10 U C2 69.3(2) . . ? C20 U C2 110.7(2) . . ? C4 U C2 47.6(2) . . ? N1 U C18 113.92(18) . . ? C19 U C18 29.47(19) . . ? C3 U C18 103.6(2) . . ? C9 U C18 82.4(2) . . ? C12 U C18 91.2(2) . . ? C13 U C18 70.1(2) . . ? C11 U C18 117.6(2) . . ? C10 U C18 111.6(2) . . ? C20 U C18 47.8(2) . . ? C4 U C18 108.79(19) . . ? C2 U C18 126.3(2) . . ? C6 Si1 C1 110.1(3) . . ? C6 Si1 C8 109.9(3) . . ? C1 Si1 C8 113.9(3) . . ? C6 Si1 C7 107.3(4) . . ? C1 Si1 C7 106.8(3) . . ? C8 Si1 C7 108.6(3) . . ? C16 Si2 C14 106.7(4) . . ? C16 Si2 C15 112.2(5) . . ? C14 Si2 C15 106.0(4) . . ? C16 Si2 C9 109.3(4) . . ? C14 Si2 C9 115.4(3) . . ? C15 Si2 C9 107.5(3) . . ? C23 Si3 C22 110.3(4) . . ? C23 Si3 C17 110.7(3) . . ? C22 Si3 C17 113.7(3) . . ? C23 Si3 C24 106.0(3) . . ? C22 Si3 C24 107.9(3) . . ? C17 Si3 C24 108.0(3) . . ? C25 N1 C28 115.0(6) . . ? C25 N1 U 126.0(4) . . ? C28 N1 U 116.9(4) . . ? C26 N2 C27 117.9(6) . . ? C5 C1 C2 105.6(6) . . ? C5 C1 Si1 121.6(5) . . ? C2 C1 Si1 131.1(5) . . ? C5 C1 U 74.4(3) . . ? C2 C1 U 73.7(3) . . ? Si1 C1 U 128.1(3) . . ? C3 C2 C1 108.8(6) . . ? C3 C2 U 73.7(3) . . ? C1 C2 U 77.1(3) . . ? C4 C3 C2 107.3(6) . . ? C4 C3 U 77.0(4) . . ? C2 C3 U 77.1(4) . . ? C5 C4 C3 108.6(6) . . ? C5 C4 U 76.5(4) . . ? C3 C4 U 73.9(4) . . ? C4 C5 C1 109.6(6) . . ? C4 C5 U 75.0(3) . . ? C1 C5 U 76.8(4) . . ? C13 C9 C10 106.1(6) . . ? C13 C9 Si2 123.9(5) . . ? C10 C9 Si2 129.1(5) . . ? C13 C9 U 75.6(4) . . ? C10 C9 U 75.8(4) . . ? Si2 C9 U 122.7(3) . . ? C11 C10 C9 109.5(6) . . ? C11 C10 U 75.7(4) . . ? C9 C10 U 74.8(4) . . ? C10 C11 C12 108.1(6) . . ? C10 C11 U 75.7(4) . . ? C12 C11 U 74.9(4) . . ? C13 C12 C11 107.1(6) . . ? C13 C12 U 75.6(4) . . ? C11 C12 U 75.7(4) . . ? C12 C13 C9 109.2(6) . . ? C12 C13 U 75.3(4) . . ? C9 C13 U 75.0(4) . . ? C21 C17 C18 106.4(6) . . ? C21 C17 Si3 124.1(5) . . ? C18 C17 Si3 127.3(5) . . ? C21 C17 U 74.9(4) . . ? C18 C17 U 73.2(3) . . ? Si3 C17 U 130.4(3) . . ? C19 C18 C17 107.8(6) . . ? C19 C18 U 73.4(4) . . ? C17 C18 U 77.8(4) . . ? C20 C19 C18 108.4(6) . . ? C20 C19 U 77.2(4) . . ? C18 C19 U 77.2(4) . . ? C19 C20 C21 108.1(6) . . ? C19 C20 U 74.1(4) . . ? C21 C20 U 77.5(4) . . ? C20 C21 C17 109.3(7) . . ? C20 C21 U 73.8(4) . . ? C17 C21 U 76.7(4) . . ? N1 C25 C26 122.4(6) . . ? N2 C26 C25 121.7(6) . . ? N2 C26 C29 117.8(6) . . ? C25 C26 C29 120.5(6) . . ? N2 C27 C28 119.9(6) . . ? N2 C27 C30 117.9(6) . . ? C28 C27 C30 122.2(7) . . ? N1 C28 C27 122.9(6) . . ?