# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 915627' #TrackingRef 'Compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ac334 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H78 Ce2 N2 O6 Si4' _chemical_formula_sum 'C30 H78 Ce2 N2 O6 Si4' _chemical_formula_weight 955.54 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall -P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.2304(16) _cell_length_b 18.3123(18) _cell_length_c 16.960(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4730.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26311 _cell_measurement_theta_min 5.79 _cell_measurement_theta_max 55.03 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 2.035 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.40053 _exptl_absorpt_correction_T_max 1.44821 _exptl_absorpt_process_details MulAbs _exptl_special_details ; weakly diffracting crystal ; _diffrn_ambient_temperature 173(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 StoeIPDS2T _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55312 _diffrn_reflns_av_R_equivalents 0.1909 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.35 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 4321 _reflns_number_gt 3137 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep2 _computing_publication_material POV-Ray _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+15.4987P] 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 4321 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.485 _refine_diff_density_min -1.737 _refine_diff_density_rms 0.108 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 0.40856(3) 0.07418(2) 0.50315(2) 0.03935(17) Uani 1 1 d . . . Si1 Si 0.21916(14) -0.01836(12) 0.49333(12) 0.0486(5) Uani 1 1 d . . . Si2 Si 0.21331(15) 0.10922(13) 0.60842(13) 0.0494(5) Uani 1 1 d . . . O1 O 0.4556(4) 0.1514(3) 0.5805(3) 0.0575(15) Uani 1 1 d . . . O2 O 0.5233(3) 0.0245(3) 0.4304(3) 0.0396(11) Uani 1 1 d . . . O3 O 0.3756(4) 0.1378(3) 0.4074(3) 0.0562(14) Uani 1 1 d . . . N1 N 0.2672(4) 0.0528(3) 0.5427(3) 0.0432(15) Uani 1 1 d . . . C1 C 0.3084(5) -0.0634(5) 0.4333(5) 0.059(2) Uani 1 1 d . . . H1A H 0.3331 -0.0280 0.3961 0.089 Uiso 1 1 calc R . . H1B H 0.2837 -0.1048 0.4041 0.089 Uiso 1 1 calc R . . H1C H 0.3549 -0.0809 0.4686 0.089 Uiso 1 1 calc R . . C2 C 0.1325(6) 0.0096(6) 0.4210(5) 0.072(3) Uani 1 1 d . . . H2A H 0.0826 0.0308 0.4494 0.108 Uiso 1 1 calc R . . H2B H 0.1128 -0.0333 0.3913 0.108 Uiso 1 1 calc R . . H2C H 0.1567 0.0459 0.3845 0.108 Uiso 1 1 calc R . . C3 C 0.1705(7) -0.0888(5) 0.5612(6) 0.072(3) Uani 1 1 d . . . H3A H 0.2166 -0.1085 0.5955 0.107 Uiso 1 1 calc R . . H3B H 0.1450 -0.1285 0.5299 0.107 Uiso 1 1 calc R . . H3C H 0.1247 -0.0662 0.5935 0.107 Uiso 1 1 calc R . . C4 C 0.2364(6) 0.2073(5) 0.5848(6) 0.076(3) Uani 1 1 d . . . H4A H 0.3000 0.2155 0.5848 0.113 Uiso 1 1 calc R . . H4B H 0.2088 0.2386 0.6245 0.113 Uiso 1 1 calc R . . H4C H 0.2125 0.2190 0.5326 0.113 Uiso 1 1 calc R . . C5 C 0.0909(5) 0.0991(6) 0.6071(6) 0.066(2) Uani 1 1 d . . . H5A H 0.0688 0.1092 0.5539 0.098 Uiso 1 1 calc R . . H5B H 0.0647 0.1336 0.6444 0.098 Uiso 1 1 calc R . . H5C H 0.0751 0.0492 0.6222 0.098 Uiso 1 1 calc R . . C6 C 0.2508(6) 0.0920(6) 0.7111(4) 0.073(3) Uani 1 1 d . . . H6A H 0.2400 0.0408 0.7248 0.109 Uiso 1 1 calc R . . H6B H 0.2183 0.1237 0.7475 0.109 Uiso 1 1 calc R . . H6C H 0.3137 0.1024 0.7152 0.109 Uiso 1 1 calc R . . C7 C 0.4879(8) 0.2145(6) 0.6179(6) 0.093(4) Uani 1 1 d . . . H7 H 0.4334 0.2434 0.6281 0.112 Uiso 1 1 calc R . . C8 C 0.5206(9) 0.2017(6) 0.6940(6) 0.104(4) Uani 1 1 d . . . H8A H 0.4759 0.1768 0.7256 0.155 Uiso 1 1 calc R . . H8B H 0.5357 0.2483 0.7189 0.155 Uiso 1 1 calc R . . H8C H 0.5732 0.1710 0.6907 0.155 Uiso 1 1 calc R . . C9 C 0.5363(9) 0.2606(7) 0.5646(7) 0.106(4) Uani 1 1 d . . . H9A H 0.5519 0.3063 0.5913 0.158 Uiso 1 1 calc R . . H9B H 0.5001 0.2715 0.5183 0.158 Uiso 1 1 calc R . . H9C H 0.5900 0.2355 0.5479 0.158 Uiso 1 1 calc R . . C10 C 0.5584(6) 0.0396(5) 0.3535(4) 0.054(2) Uani 1 1 d . . . H10 H 0.6116 0.0081 0.3466 0.065 Uiso 1 1 calc R . . C11 C 0.5882(6) 0.1175(6) 0.3480(5) 0.070(3) Uani 1 1 d . . . H11A H 0.5378 0.1500 0.3557 0.105 Uiso 1 1 calc R . . H11B H 0.6139 0.1263 0.2958 0.105 Uiso 1 1 calc R . . H11C H 0.6323 0.1271 0.3887 0.105 Uiso 1 1 calc R . . C12 C 0.4932(6) 0.0181(5) 0.2898(4) 0.064(3) Uani 1 1 d . . . H12A H 0.4749 -0.0327 0.2979 0.096 Uiso 1 1 calc R . . H12B H 0.5209 0.0229 0.2379 0.096 Uiso 1 1 calc R . . H12C H 0.4418 0.0501 0.2927 0.096 Uiso 1 1 calc R . . C13 C 0.3490(8) 0.1879(6) 0.3490(6) 0.083(3) Uani 1 1 d . . . H13 H 0.3968 0.1840 0.3087 0.100 Uiso 1 1 calc R . . C14 C 0.3567(8) 0.2640(5) 0.3763(6) 0.085(3) Uani 1 1 d . . . H14A H 0.3374 0.2971 0.3343 0.128 Uiso 1 1 calc R . . H14B H 0.4180 0.2745 0.3897 0.128 Uiso 1 1 calc R . . H14C H 0.3197 0.2710 0.4230 0.128 Uiso 1 1 calc R . . C15 C 0.2740(9) 0.1667(7) 0.3067(8) 0.139(6) Uani 1 1 d . . . H15A H 0.2811 0.1162 0.2884 0.209 Uiso 1 1 calc R . . H15B H 0.2662 0.1990 0.2612 0.209 Uiso 1 1 calc R . . H15C H 0.2224 0.1699 0.3410 0.209 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 0.0392(3) 0.0405(3) 0.0383(3) 0.00111(19) -0.00120(18) 0.00018(18) Si1 0.0428(12) 0.0540(13) 0.0489(11) -0.0051(10) -0.0002(10) -0.0066(11) Si2 0.0450(12) 0.0540(14) 0.0491(11) -0.0041(10) 0.0031(10) 0.0024(12) O1 0.067(4) 0.050(3) 0.055(3) -0.010(3) -0.010(3) -0.012(3) O2 0.041(3) 0.040(3) 0.038(2) 0.004(2) 0.007(2) 0.001(2) O3 0.062(4) 0.057(4) 0.049(3) 0.009(3) -0.004(3) 0.007(3) N1 0.042(4) 0.045(4) 0.042(3) -0.001(3) 0.001(3) -0.004(3) C1 0.051(5) 0.067(6) 0.060(5) -0.024(4) 0.000(4) -0.002(5) C2 0.061(6) 0.090(8) 0.067(6) -0.006(5) -0.015(5) -0.006(6) C3 0.074(7) 0.058(6) 0.083(6) 0.002(5) 0.010(5) -0.007(5) C4 0.064(6) 0.063(6) 0.100(7) -0.016(5) 0.010(6) 0.005(5) C5 0.053(6) 0.069(6) 0.075(6) -0.002(5) 0.007(5) 0.001(5) C6 0.073(7) 0.097(8) 0.047(5) -0.016(5) 0.000(4) 0.021(6) C7 0.120(10) 0.080(8) 0.079(7) -0.013(6) -0.021(7) -0.037(7) C8 0.157(12) 0.093(9) 0.061(6) -0.018(6) -0.026(7) -0.031(8) C9 0.126(10) 0.093(9) 0.097(8) 0.021(7) -0.023(8) -0.061(8) C10 0.052(5) 0.064(6) 0.045(4) 0.013(4) 0.010(4) 0.009(4) C11 0.055(6) 0.082(7) 0.073(6) 0.032(5) 0.008(5) -0.007(5) C12 0.082(7) 0.069(7) 0.040(4) 0.000(4) 0.008(4) 0.010(5) C13 0.125(10) 0.057(6) 0.068(6) 0.013(5) -0.034(6) 0.016(6) C14 0.128(10) 0.058(7) 0.070(6) 0.015(5) -0.006(6) 0.016(7) C15 0.143(12) 0.111(11) 0.163(13) 0.052(9) -0.100(11) -0.022(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O1 2.058(5) . ? Ce1 O3 2.061(5) . ? Ce1 N1 2.289(6) . ? Ce1 O2 2.324(5) . ? Ce1 O2 2.368(5) 5_656 ? Ce1 Si1 3.350(2) . ? Ce1 Ce1 3.8924(8) 5_656 ? Si1 N1 1.712(6) . ? Si1 C2 1.873(9) . ? Si1 C3 1.881(9) . ? Si1 C1 1.888(8) . ? Si2 N1 1.728(6) . ? Si2 C6 1.860(8) . ? Si2 C4 1.873(10) . ? Si2 C5 1.874(8) . ? O1 C7 1.405(11) . ? O2 C10 1.438(8) . ? O2 Ce1 2.368(5) 5_656 ? O3 C13 1.410(10) . ? C7 C8 1.404(13) . ? C7 C9 1.441(14) . ? C10 C11 1.501(13) . ? C10 C12 1.519(11) . ? C13 C15 1.403(14) . ? C13 C14 1.473(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 O1 Ce1 O3 101.4(2) . . ? O1 Ce1 N1 105.0(2) . . ? O3 Ce1 N1 95.6(2) . . ? O1 Ce1 O2 110.2(2) . . ? O3 Ce1 O2 89.24(19) . . ? N1 Ce1 O2 142.7(2) . . ? O1 Ce1 O2 93.9(2) . 5_656 ? O3 Ce1 O2 155.91(19) . 5_656 ? N1 Ce1 O2 98.20(19) . 5_656 ? O2 Ce1 O2 67.92(17) . 5_656 ? O1 Ce1 Si1 132.79(17) . . ? O3 Ce1 Si1 92.13(17) . . ? N1 Ce1 Si1 28.09(15) . . ? O2 Ce1 Si1 115.00(13) . . ? O2 Ce1 Si1 90.88(13) 5_656 . ? O1 Ce1 Ce1 104.36(17) . 5_656 ? O3 Ce1 Ce1 123.20(16) . 5_656 ? N1 Ce1 Ce1 124.17(16) . 5_656 ? O2 Ce1 Ce1 34.32(11) . 5_656 ? O2 Ce1 Ce1 33.60(11) 5_656 5_656 ? Si1 Ce1 Ce1 105.18(4) . 5_656 ? N1 Si1 C2 114.4(4) . . ? N1 Si1 C3 113.0(4) . . ? C2 Si1 C3 108.1(5) . . ? N1 Si1 C1 106.8(3) . . ? C2 Si1 C1 105.9(4) . . ? C3 Si1 C1 108.3(4) . . ? N1 Si1 Ce1 39.0(2) . . ? C2 Si1 Ce1 120.1(3) . . ? C3 Si1 Ce1 131.0(3) . . ? C1 Si1 Ce1 68.2(3) . . ? N1 Si2 C6 110.9(4) . . ? N1 Si2 C4 110.2(4) . . ? C6 Si2 C4 107.8(5) . . ? N1 Si2 C5 113.9(4) . . ? C6 Si2 C5 107.5(4) . . ? C4 Si2 C5 106.2(5) . . ? C7 O1 Ce1 166.8(6) . . ? C10 O2 Ce1 133.4(4) . . ? C10 O2 Ce1 114.5(4) . 5_656 ? Ce1 O2 Ce1 112.08(17) . 5_656 ? C13 O3 Ce1 172.7(6) . . ? Si1 N1 Si2 124.6(4) . . ? Si1 N1 Ce1 112.9(3) . . ? Si2 N1 Ce1 122.2(3) . . ? C8 C7 O1 113.7(10) . . ? C8 C7 C9 119.5(10) . . ? O1 C7 C9 112.2(9) . . ? O2 C10 C11 110.6(7) . . ? O2 C10 C12 110.6(7) . . ? C11 C10 C12 113.6(7) . . ? C15 C13 O3 114.3(10) . . ? C15 C13 C14 119.1(11) . . ? O3 C13 C14 111.8(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ce1 Si1 N1 9.7(4) . . . . ? O3 Ce1 Si1 N1 -98.0(4) . . . . ? O2 Ce1 Si1 N1 171.9(3) . . . . ? O2 Ce1 Si1 N1 105.9(3) 5_656 . . . ? Ce1 Ce1 Si1 N1 136.7(3) 5_656 . . . ? O1 Ce1 Si1 C2 102.2(4) . . . . ? O3 Ce1 Si1 C2 -5.5(4) . . . . ? N1 Ce1 Si1 C2 92.5(5) . . . . ? O2 Ce1 Si1 C2 -95.7(4) . . . . ? O2 Ce1 Si1 C2 -161.6(4) 5_656 . . . ? Ce1 Ce1 Si1 C2 -130.8(4) 5_656 . . . ? O1 Ce1 Si1 C3 -65.8(5) . . . . ? O3 Ce1 Si1 C3 -173.6(4) . . . . ? N1 Ce1 Si1 C3 -75.6(5) . . . . ? O2 Ce1 Si1 C3 96.3(4) . . . . ? O2 Ce1 Si1 C3 30.3(4) 5_656 . . . ? Ce1 Ce1 Si1 C3 61.1(4) 5_656 . . . ? O1 Ce1 Si1 C1 -161.5(4) . . . . ? O3 Ce1 Si1 C1 90.7(3) . . . . ? N1 Ce1 Si1 C1 -171.3(5) . . . . ? O2 Ce1 Si1 C1 0.6(3) . . . . ? O2 Ce1 Si1 C1 -65.4(3) 5_656 . . . ? Ce1 Ce1 Si1 C1 -34.6(3) 5_656 . . . ? O3 Ce1 O1 C7 -14(3) . . . . ? N1 Ce1 O1 C7 -113(3) . . . . ? O2 Ce1 O1 C7 80(3) . . . . ? O2 Ce1 O1 C7 148(3) 5_656 . . . ? Si1 Ce1 O1 C7 -118(3) . . . . ? Ce1 Ce1 O1 C7 115(3) 5_656 . . . ? O1 Ce1 O2 C10 -96.7(7) . . . . ? O3 Ce1 O2 C10 5.3(7) . . . . ? N1 Ce1 O2 C10 103.6(7) . . . . ? O2 Ce1 O2 C10 177.4(8) 5_656 . . . ? Si1 Ce1 O2 C10 97.2(6) . . . . ? Ce1 Ce1 O2 C10 177.4(8) 5_656 . . . ? O1 Ce1 O2 Ce1 85.9(2) . . . 5_656 ? O3 Ce1 O2 Ce1 -172.2(2) . . . 5_656 ? N1 Ce1 O2 Ce1 -73.8(4) . . . 5_656 ? O2 Ce1 O2 Ce1 0.0 5_656 . . 5_656 ? Si1 Ce1 O2 Ce1 -80.2(2) . . . 5_656 ? O1 Ce1 O3 C13 -40(5) . . . . ? N1 Ce1 O3 C13 67(5) . . . . ? O2 Ce1 O3 C13 -150(5) . . . . ? O2 Ce1 O3 C13 -168(5) 5_656 . . . ? Si1 Ce1 O3 C13 95(5) . . . . ? Ce1 Ce1 O3 C13 -156(5) 5_656 . . . ? C2 Si1 N1 Si2 65.6(6) . . . . ? C3 Si1 N1 Si2 -58.7(6) . . . . ? C1 Si1 N1 Si2 -177.6(4) . . . . ? Ce1 Si1 N1 Si2 173.9(6) . . . . ? C2 Si1 N1 Ce1 -108.3(4) . . . . ? C3 Si1 N1 Ce1 127.4(4) . . . . ? C1 Si1 N1 Ce1 8.5(4) . . . . ? C6 Si2 N1 Si1 109.5(5) . . . . ? C4 Si2 N1 Si1 -131.2(5) . . . . ? C5 Si2 N1 Si1 -11.9(6) . . . . ? C6 Si2 N1 Ce1 -77.1(5) . . . . ? C4 Si2 N1 Ce1 42.2(5) . . . . ? C5 Si2 N1 Ce1 161.5(4) . . . . ? O1 Ce1 N1 Si1 -172.6(3) . . . . ? O3 Ce1 N1 Si1 83.9(3) . . . . ? O2 Ce1 N1 Si1 -12.2(5) . . . . ? O2 Ce1 N1 Si1 -76.3(3) 5_656 . . . ? Ce1 Ce1 N1 Si1 -53.1(4) 5_656 . . . ? O1 Ce1 N1 Si2 13.3(4) . . . . ? O3 Ce1 N1 Si2 -90.1(4) . . . . ? O2 Ce1 N1 Si2 173.7(2) . . . . ? O2 Ce1 N1 Si2 109.6(4) 5_656 . . . ? Si1 Ce1 N1 Si2 -174.1(6) . . . . ? Ce1 Ce1 N1 Si2 132.8(3) 5_656 . . . ? Ce1 O1 C7 C8 -168(2) . . . . ? Ce1 O1 C7 C9 -28(4) . . . . ? Ce1 O2 C10 C11 58.6(9) . . . . ? Ce1 O2 C10 C11 -124.0(6) 5_656 . . . ? Ce1 O2 C10 C12 -68.1(9) . . . . ? Ce1 O2 C10 C12 109.3(6) 5_656 . . . ? Ce1 O3 C13 C15 -108(5) . . . . ? Ce1 O3 C13 C14 32(6) . . . . ? data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 915628' #TrackingRef 'Compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H66 Ce Li N2 O4 Si4' _chemical_formula_sum 'C26 H66 Ce Li N2 O4 Si4' _chemical_formula_weight 730.23 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.5799(3) _cell_length_b 16.2153(3) _cell_length_c 19.6833(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4015.13(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 36728 _cell_measurement_theta_min 5.82 _cell_measurement_theta_max 59.02 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 1.280 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.76388 _exptl_absorpt_correction_T_max 0.92459 _exptl_absorpt_process_details MulAbs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 StoeIPDS2T _diffrn_measurement_method 'omega scans ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76271 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 29.22 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.22 _diffrn_measured_fraction_theta_full 0.992 _reflns_number_total 10794 _reflns_number_gt 10361 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3, POV-Ray' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+2.6987P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(11) _refine_ls_number_reflns 10794 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.203 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.642 _refine_diff_density_min -1.227 _refine_diff_density_rms 0.068 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0324(4) 0.7820(3) 0.8646(2) 0.0587(11) Uani 1 1 d . . . H1A H 1.0722 0.7819 0.9074 0.088 Uiso 1 1 calc R . . H1B H 1.0383 0.7278 0.8430 0.088 Uiso 1 1 calc R . . H1C H 0.9575 0.7942 0.8738 0.088 Uiso 1 1 calc R . . C2 C 1.0126(5) 0.8548(4) 0.7252(3) 0.0871(18) Uani 1 1 d . . . H2A H 0.9372 0.8661 0.7337 0.131 Uiso 1 1 calc R . . H2B H 1.0204 0.7992 0.7063 0.131 Uiso 1 1 calc R . . H2C H 1.0405 0.8953 0.6928 0.131 Uiso 1 1 calc R . . C3 C 1.2288(4) 0.8302(3) 0.7882(3) 0.0771(16) Uani 1 1 d . . . H3A H 1.2588 0.8665 0.7532 0.116 Uiso 1 1 calc R . . H3B H 1.2294 0.7731 0.7719 0.116 Uiso 1 1 calc R . . H3C H 1.2714 0.8344 0.8297 0.116 Uiso 1 1 calc R . . C4 C 1.1578(4) 1.0589(3) 0.7276(2) 0.0666(13) Uani 1 1 d . . . H4A H 1.1824 1.0091 0.7042 0.100 Uiso 1 1 calc R . . H4B H 1.2065 1.1045 0.7180 0.100 Uiso 1 1 calc R . . H4C H 1.0863 1.0731 0.7117 0.100 Uiso 1 1 calc R . . C5 C 1.2952(4) 1.0328(4) 0.8530(3) 0.0743(16) Uani 1 1 d . . . H5A H 1.2953 1.0252 0.9024 0.111 Uiso 1 1 calc R . . H5B H 1.3329 1.0838 0.8416 0.111 Uiso 1 1 calc R . . H5C H 1.3308 0.9859 0.8313 0.111 Uiso 1 1 calc R . . C6 C 1.0962(4) 1.1352(3) 0.8608(2) 0.0658(13) Uani 1 1 d . . . H6A H 1.0251 1.1448 0.8421 0.099 Uiso 1 1 calc R . . H6B H 1.1419 1.1824 0.8505 0.099 Uiso 1 1 calc R . . H6C H 1.0913 1.1281 0.9101 0.099 Uiso 1 1 calc R . . C7 C 0.8312(5) 1.1874(3) 0.9602(3) 0.0811(17) Uani 1 1 d . . . H7A H 0.8819 1.2119 0.9282 0.122 Uiso 1 1 calc R . . H7B H 0.7770 1.2283 0.9721 0.122 Uiso 1 1 calc R . . H7C H 0.7971 1.1395 0.9391 0.122 Uiso 1 1 calc R . . C8 C 0.8011(5) 1.1330(4) 1.1062(3) 0.0868(18) Uani 1 1 d . . . H8A H 0.7569 1.0862 1.0922 0.130 Uiso 1 1 calc R . . H8B H 0.7563 1.1819 1.1121 0.130 Uiso 1 1 calc R . . H8C H 0.8366 1.1200 1.1491 0.130 Uiso 1 1 calc R . . C9 C 0.9829(5) 1.2450(3) 1.0684(4) 0.0922(19) Uani 1 1 d . . . H9A H 1.0208 1.2308 1.1103 0.138 Uiso 1 1 calc R . . H9B H 0.9351 1.2916 1.0771 0.138 Uiso 1 1 calc R . . H9C H 1.0343 1.2602 1.0332 0.138 Uiso 1 1 calc R . . C10 C 1.1198(4) 0.9290(3) 1.0335(2) 0.0557(11) Uani 1 1 d . . . H10A H 1.0590 0.8912 1.0349 0.084 Uiso 1 1 calc R . . H10B H 1.1780 0.9063 1.0608 0.084 Uiso 1 1 calc R . . H10C H 1.1434 0.9358 0.9864 0.084 Uiso 1 1 calc R . . C11 C 1.2010(4) 1.0968(3) 1.0685(3) 0.0662(12) Uani 1 1 d . . . H11A H 1.2225 1.1076 1.0215 0.099 Uiso 1 1 calc R . . H11B H 1.2584 1.0678 1.0923 0.099 Uiso 1 1 calc R . . H11C H 1.1865 1.1492 1.0915 0.099 Uiso 1 1 calc R . . C12 C 1.0442(4) 1.0152(3) 1.16058(19) 0.0659(11) Uani 1 1 d . . . H12A H 1.0294 1.0684 1.1822 0.099 Uiso 1 1 calc R . . H12B H 1.1038 0.9883 1.1838 0.099 Uiso 1 1 calc R . . H12C H 0.9810 0.9800 1.1636 0.099 Uiso 1 1 calc R . . C13 C 0.8372(5) 0.8262(3) 1.0153(2) 0.0620(12) Uani 1 1 d . . . H13 H 0.9135 0.8112 1.0225 0.074 Uiso 1 1 calc R . . C14 C 0.8000(4) 0.8652(3) 1.0811(2) 0.0648(12) Uani 1 1 d . . . H14A H 0.8471 0.9112 1.0929 0.097 Uiso 1 1 calc R . . H14B H 0.8017 0.8240 1.1175 0.097 Uiso 1 1 calc R . . H14C H 0.7272 0.8857 1.0755 0.097 Uiso 1 1 calc R . . C15 C 0.7832(5) 0.7501(3) 0.9979(3) 0.0769(16) Uani 1 1 d . . . H15A H 0.7077 0.7614 0.9898 0.115 Uiso 1 1 calc R . . H15B H 0.7903 0.7107 1.0354 0.115 Uiso 1 1 calc R . . H15C H 0.8150 0.7267 0.9567 0.115 Uiso 1 1 calc R . . C16 C 0.7499(4) 1.0327(4) 0.7978(2) 0.0726(16) Uani 1 1 d . . . H16 H 0.7275 0.9814 0.7736 0.087 Uiso 1 1 calc R . . C17 C 0.8304(6) 1.0667(6) 0.7561(3) 0.134(4) Uani 1 1 d . . . H17A H 0.8537 1.1196 0.7751 0.201 Uiso 1 1 calc R . . H17B H 0.8022 1.0755 0.7102 0.201 Uiso 1 1 calc R . . H17C H 0.8908 1.0287 0.7540 0.201 Uiso 1 1 calc R . . C18 C 0.6506(5) 1.0816(4) 0.8046(3) 0.0911(19) Uani 1 1 d . . . H18A H 0.5983 1.0501 0.8308 0.137 Uiso 1 1 calc R . . H18B H 0.6219 1.0935 0.7593 0.137 Uiso 1 1 calc R . . H18C H 0.6661 1.1336 0.8280 0.137 Uiso 1 1 calc R . . C19 C 0.5745(6) 1.0378(4) 0.9817(4) 0.110(3) Uani 1 1 d . . . H19A H 0.5411 1.0690 0.9442 0.133 Uiso 1 1 calc R . . H19B H 0.6442 1.0631 0.9921 0.133 Uiso 1 1 calc R . . C20 C 0.5054(7) 1.0395(6) 1.0427(4) 0.139(2) Uani 1 1 d . . . H20A H 0.5460 1.0580 1.0830 0.167 Uiso 1 1 calc R . . H20B H 0.4448 1.0775 1.0357 0.167 Uiso 1 1 calc R . . C21 C 0.4680(7) 0.9558(6) 1.0519(4) 0.139(2) Uani 1 1 d . . . H21A H 0.4949 0.9330 1.0953 0.167 Uiso 1 1 calc R . . H21B H 0.3893 0.9545 1.0529 0.167 Uiso 1 1 calc R . . C22 C 0.5065(5) 0.9088(4) 0.9966(3) 0.094(2) Uani 1 1 d . . . H22A H 0.4478 0.8969 0.9646 0.112 Uiso 1 1 calc R . . H22B H 0.5354 0.8557 1.0132 0.112 Uiso 1 1 calc R . . C23 C 0.6992(4) 0.7749(4) 0.8119(3) 0.0871(19) Uani 1 1 d . . . H23A H 0.7415 0.7388 0.8421 0.105 Uiso 1 1 calc R . . H23B H 0.7480 0.8021 0.7794 0.105 Uiso 1 1 calc R . . C24 C 0.6191(5) 0.7262(4) 0.7752(4) 0.102(2) Uani 1 1 d . . . H24A H 0.6370 0.7234 0.7262 0.123 Uiso 1 1 calc R . . H24B H 0.6161 0.6694 0.7934 0.123 Uiso 1 1 calc R . . C25 C 0.5186(5) 0.7672(4) 0.7847(4) 0.105(2) Uani 1 1 d . . . H25A H 0.4903 0.7864 0.7406 0.126 Uiso 1 1 calc R . . H25B H 0.4664 0.7288 0.8052 0.126 Uiso 1 1 calc R . . C26 C 0.5363(4) 0.8354(5) 0.8286(4) 0.114(3) Uani 1 1 d . . . H26A H 0.5209 0.8875 0.8043 0.137 Uiso 1 1 calc R . . H26B H 0.4883 0.8318 0.8684 0.137 Uiso 1 1 calc R . . N1 N 1.0787(2) 0.95696(18) 0.84356(14) 0.0395(6) Uani 1 1 d . . . N2 N 0.9774(2) 1.06960(18) 1.02156(16) 0.0415(7) Uani 1 1 d . . . O1 O 0.8361(2) 0.88438(15) 0.96237(13) 0.0411(6) Uani 1 1 d . . . O2 O 0.78799(19) 1.00454(19) 0.86191(12) 0.0492(6) Uani 1 1 d . . . O3 O 0.5880(2) 0.9545(2) 0.96288(17) 0.0635(8) Uani 1 1 d . . . O4 O 0.6433(2) 0.8347(2) 0.85045(17) 0.0624(8) Uani 1 1 d . . . Si1 Si 1.08826(9) 0.86229(7) 0.80679(6) 0.0466(3) Uani 1 1 d . . . Si2 Si 1.15424(9) 1.03942(8) 0.82175(6) 0.0481(3) Uani 1 1 d . . . Si3 Si 0.90345(10) 1.15395(7) 1.03920(7) 0.0553(3) Uani 1 1 d . . . Si4 Si 1.07919(8) 1.03202(6) 1.06907(5) 0.0420(2) Uani 1 1 d . . . Li Li 0.7109(5) 0.9175(4) 0.9096(4) 0.0487(16) Uani 1 1 d . . . Ce1 Ce 0.938069(14) 0.987892(11) 0.922540(9) 0.03538(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.059(3) 0.050(2) 0.067(3) 0.003(2) 0.016(2) -0.0012(19) C2 0.128(5) 0.073(4) 0.059(3) -0.013(3) -0.018(3) -0.008(3) C3 0.072(3) 0.064(3) 0.095(4) 0.008(3) 0.037(3) 0.017(3) C4 0.074(3) 0.078(3) 0.048(2) 0.014(2) 0.005(2) -0.018(3) C5 0.053(3) 0.105(5) 0.065(3) 0.012(3) -0.008(2) -0.021(3) C6 0.090(4) 0.048(2) 0.059(3) 0.006(2) 0.001(2) -0.014(2) C7 0.089(4) 0.057(3) 0.098(4) 0.003(3) -0.017(3) 0.035(3) C8 0.069(4) 0.101(4) 0.090(4) -0.017(3) 0.015(3) 0.024(3) C9 0.100(4) 0.048(3) 0.128(5) -0.028(3) -0.006(4) 0.001(2) C10 0.053(2) 0.055(3) 0.059(3) 0.003(2) -0.003(2) 0.017(2) C11 0.056(3) 0.066(3) 0.077(3) 0.006(3) -0.012(3) -0.010(2) C12 0.069(3) 0.085(3) 0.0440(19) 0.003(2) -0.0022(19) 0.004(3) C13 0.092(4) 0.044(2) 0.050(2) 0.0080(18) 0.007(2) -0.006(2) C14 0.094(3) 0.059(2) 0.041(2) 0.003(2) 0.009(3) -0.010(2) C15 0.114(5) 0.045(3) 0.071(3) 0.009(2) 0.013(3) -0.013(3) C16 0.064(3) 0.102(5) 0.052(3) 0.022(3) -0.010(2) 0.013(3) C17 0.105(5) 0.218(9) 0.079(4) 0.082(5) 0.014(4) 0.051(6) C18 0.082(4) 0.109(5) 0.082(4) 0.014(3) -0.024(3) 0.028(4) C19 0.120(5) 0.086(4) 0.126(5) -0.040(4) 0.066(5) -0.020(4) C20 0.138(5) 0.157(6) 0.123(4) -0.028(4) 0.076(4) 0.000(4) C21 0.138(5) 0.157(6) 0.123(4) -0.028(4) 0.076(4) 0.000(4) C22 0.075(4) 0.100(5) 0.107(5) 0.020(4) 0.044(4) 0.005(3) C23 0.060(3) 0.106(5) 0.096(4) -0.038(4) -0.014(3) 0.026(3) C24 0.095(5) 0.089(5) 0.123(5) -0.038(4) -0.037(4) 0.025(4) C25 0.067(4) 0.099(5) 0.149(7) -0.044(5) -0.022(4) -0.008(3) C26 0.057(3) 0.137(6) 0.147(6) -0.069(5) -0.040(4) 0.020(3) N1 0.0368(16) 0.0460(16) 0.0356(14) 0.0032(12) 0.0010(12) -0.0018(12) N2 0.0459(16) 0.0354(16) 0.0431(17) -0.0047(13) -0.0041(13) 0.0007(12) O1 0.0470(14) 0.0350(13) 0.0414(14) 0.0045(10) 0.0022(11) 0.0002(11) O2 0.0475(13) 0.0576(18) 0.0425(12) 0.0130(13) -0.0038(10) 0.0073(14) O3 0.0538(19) 0.070(2) 0.0668(19) -0.0018(15) 0.0175(15) 0.0050(14) O4 0.0495(17) 0.068(2) 0.070(2) -0.0145(16) -0.0112(15) 0.0036(15) Si1 0.0506(7) 0.0456(6) 0.0437(6) 0.0009(4) 0.0082(5) 0.0034(4) Si2 0.0485(6) 0.0565(7) 0.0392(5) 0.0079(5) 0.0004(5) -0.0111(5) Si3 0.0580(7) 0.0403(6) 0.0675(8) -0.0130(5) -0.0051(6) 0.0091(5) Si4 0.0434(5) 0.0425(5) 0.0400(5) -0.0004(4) -0.0041(4) -0.0004(4) Li 0.045(3) 0.051(4) 0.051(4) -0.003(3) 0.002(3) 0.001(3) Ce1 0.03676(8) 0.03609(8) 0.03328(7) 0.00185(7) 0.00064(8) -0.00057(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 C1 Si1 1.867(4) . ? C2 Si1 1.871(5) . ? C3 Si1 1.878(5) . ? C4 Si2 1.880(4) . ? C5 Si2 1.880(5) . ? C6 Si2 1.880(5) . ? C7 Si3 1.881(5) . ? C8 Si3 1.873(6) . ? C9 Si3 1.873(5) . ? C10 Si4 1.881(4) . ? C11 Si4 1.859(4) . ? C12 Si4 1.875(4) . ? C13 O1 1.406(5) . ? C13 C15 1.450(7) . ? C13 C14 1.515(6) . ? C16 C17 1.416(8) . ? C16 O2 1.424(5) . ? C16 C18 1.486(7) . ? C19 O3 1.410(6) . ? C19 C20 1.482(8) . ? C20 C21 1.449(11) . ? C21 C22 1.414(9) . ? C22 O3 1.429(6) . ? C23 O4 1.418(6) . ? C23 C24 1.469(8) . ? C24 C25 1.441(8) . ? C25 C26 1.421(8) . ? C26 O4 1.413(6) . ? N1 Si2 1.696(3) . ? N1 Si1 1.701(3) . ? N1 Ce1 2.408(3) . ? N2 Si3 1.690(3) . ? N2 Si4 1.699(3) . ? N2 Ce1 2.408(3) . ? O1 Li 1.962(7) . ? O1 Ce1 2.253(2) . ? O2 Li 1.953(8) . ? O2 Ce1 2.250(2) . ? O3 Li 1.962(7) . ? O4 Li 1.970(8) . ? Si2 Ce1 3.4684(11) . ? Si4 Ce1 3.4615(10) . ? Li Ce1 3.088(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 O1 C13 C15 113.0(4) . . ? O1 C13 C14 110.5(4) . . ? C15 C13 C14 114.4(4) . . ? C17 C16 O2 113.5(4) . . ? C17 C16 C18 116.4(5) . . ? O2 C16 C18 112.0(4) . . ? O3 C19 C20 107.6(6) . . ? C21 C20 C19 105.9(6) . . ? C22 C21 C20 107.3(6) . . ? C21 C22 O3 108.9(6) . . ? O4 C23 C24 106.9(4) . . ? C25 C24 C23 106.8(5) . . ? C26 C25 C24 107.5(5) . . ? O4 C26 C25 109.1(5) . . ? Si2 N1 Si1 124.32(18) . . ? Si2 N1 Ce1 114.27(15) . . ? Si1 N1 Ce1 120.98(15) . . ? Si3 N2 Si4 126.31(19) . . ? Si3 N2 Ce1 119.90(16) . . ? Si4 N2 Ce1 113.77(15) . . ? C13 O1 Li 125.7(4) . . ? C13 O1 Ce1 138.8(3) . . ? Li O1 Ce1 93.9(2) . . ? C16 O2 Li 119.4(4) . . ? C16 O2 Ce1 142.2(3) . . ? Li O2 Ce1 94.3(2) . . ? C19 O3 C22 106.7(4) . . ? C19 O3 Li 121.9(4) . . ? C22 O3 Li 130.9(4) . . ? C26 O4 C23 108.4(4) . . ? C26 O4 Li 125.8(4) . . ? C23 O4 Li 124.6(4) . . ? N1 Si1 C1 110.05(18) . . ? N1 Si1 C2 112.8(2) . . ? C1 Si1 C2 106.7(3) . . ? N1 Si1 C3 113.5(2) . . ? C1 Si1 C3 106.3(2) . . ? C2 Si1 C3 107.1(3) . . ? N1 Si2 C4 113.27(19) . . ? N1 Si2 C6 109.26(19) . . ? C4 Si2 C6 105.9(2) . . ? N1 Si2 C5 113.6(2) . . ? C4 Si2 C5 108.0(2) . . ? C6 Si2 C5 106.3(3) . . ? N1 Si2 Ce1 39.26(10) . . ? C4 Si2 Ce1 128.52(17) . . ? C6 Si2 Ce1 70.16(15) . . ? C5 Si2 Ce1 122.59(16) . . ? N2 Si3 C9 114.0(2) . . ? N2 Si3 C8 112.1(2) . . ? C9 Si3 C8 107.1(3) . . ? N2 Si3 C7 109.2(2) . . ? C9 Si3 C7 106.5(3) . . ? C8 Si3 C7 107.6(3) . . ? N2 Si4 C11 114.57(19) . . ? N2 Si4 C12 113.83(19) . . ? C11 Si4 C12 106.4(2) . . ? N2 Si4 C10 108.57(18) . . ? C11 Si4 C10 106.0(2) . . ? C12 Si4 C10 106.9(2) . . ? N2 Si4 Ce1 39.55(10) . . ? C11 Si4 Ce1 122.35(18) . . ? C12 Si4 Ce1 130.55(15) . . ? C10 Si4 Ce1 69.27(14) . . ? O2 Li O3 115.3(4) . . ? O2 Li O1 93.1(3) . . ? O3 Li O1 115.7(4) . . ? O2 Li O4 115.0(4) . . ? O3 Li O4 100.6(3) . . ? O1 Li O4 118.2(4) . . ? O2 Li Ce1 46.60(16) . . ? O3 Li Ce1 124.9(3) . . ? O1 Li Ce1 46.71(16) . . ? O4 Li Ce1 134.5(3) . . ? O2 Ce1 O1 78.25(10) . . ? O2 Ce1 N1 107.39(9) . . ? O1 Ce1 N1 119.18(10) . . ? O2 Ce1 N2 122.39(11) . . ? O1 Ce1 N2 104.19(10) . . ? N1 Ce1 N2 119.10(10) . . ? O2 Ce1 Li 39.10(15) . . ? O1 Ce1 Li 39.34(15) . . ? N1 Ce1 Li 123.33(15) . . ? N2 Ce1 Li 117.41(15) . . ? O2 Ce1 Si4 147.95(7) . . ? O1 Ce1 Si4 98.97(7) . . ? N1 Ce1 Si4 101.79(7) . . ? N2 Ce1 Si4 26.69(7) . . ? Li Ce1 Si4 128.31(13) . . ? O2 Ce1 Si2 109.00(7) . . ? O1 Ce1 Si2 145.57(7) . . ? N1 Ce1 Si2 26.47(7) . . ? N2 Ce1 Si2 99.75(8) . . ? Li Ce1 Si2 140.13(13) . . ? Si4 Ce1 Si2 91.41(3) . . ? data_Compound4 _database_code_depnum_ccdc_archive 'CCDC 915629' #TrackingRef 'Compound4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H70 Ce2 Li2 O10, (C4 H8 O2)' _chemical_formula_sum 'C34 H78 Ce2 Li2 O12' _chemical_formula_weight 973.08 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_HALL -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.9892(5) _cell_length_b 16.7465(5) _cell_length_c 15.0041(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.0900(10) _cell_angle_gamma 90.00 _cell_volume 4682.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9461 _cell_measurement_theta_min 3.024 _cell_measurement_theta_max 36.482 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 1.968 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5720 _exptl_absorpt_correction_T_max 0.7472 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'curved graphite' _diffrn_measurement_device_type 'APEX II SMART' _diffrn_measurement_method omega/phi _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51695 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.10 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 5164 _reflns_number_gt 4948 _reflns_threshold_expression >2sigma(I) _computing_data_collection COSMO _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The isopropylgroups and the dioxen ring of the molecule were highly disorded. This causes in the B Alerts 'Short Intra H...H Contact H10C ..H11 .. 1.80 for the dioxen ring. The C Alerts also belong to this disorder problem. ; _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^)+(0.0000P)^2^+70.8507P] 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 5164 _refine_ls_number_parameters 282 _refine_ls_number_restraints 309 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 1.340 _refine_ls_restrained_S_all 1.312 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.973 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.132 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 0.293577(15) 0.187230(19) 0.41299(2) 0.02269(10) Uani 1 1 d U . . O1 O 0.19697(19) 0.2777(2) 0.4274(2) 0.0237(8) Uani 1 1 d U . . O2 O 0.3832(2) 0.2776(3) 0.4439(3) 0.0300(9) Uani 1 1 d U . . O3 O 0.2732(3) 0.2028(3) 0.2718(3) 0.0430(11) Uani 1 1 d U . . O4 O 0.3612(2) 0.0887(3) 0.4201(3) 0.0385(10) Uani 1 1 d U . . O5 O 0.2010(2) 0.1075(3) 0.4228(3) 0.0409(11) Uani 1 1 d U . . O6 O 0.0483(3) 0.1593(4) 0.3319(3) 0.0614(17) Uani 1 1 d U . . C11 C 0.1688(3) 0.3296(4) 0.3518(4) 0.0352(13) Uani 1 1 d U . . H11 H 0.1639 0.2974 0.2948 0.042 Uiso 1 1 calc R . . C12 C 0.0946(3) 0.3600(4) 0.3590(4) 0.0402(15) Uani 1 1 d U . . H11A H 0.0642 0.3148 0.3689 0.060 Uiso 1 1 calc R . . H11B H 0.0731 0.3875 0.3026 0.060 Uiso 1 1 calc R . . H11C H 0.0987 0.3972 0.4101 0.060 Uiso 1 1 calc R . . C13 C 0.2202(4) 0.3970(5) 0.3455(6) 0.058(2) Uani 1 1 d U . . H11D H 0.2225 0.4326 0.3978 0.086 Uiso 1 1 calc R . . H11E H 0.2036 0.4271 0.2894 0.086 Uiso 1 1 calc R . . H11F H 0.2681 0.3752 0.3451 0.086 Uiso 1 1 calc R . . C21 C 0.4388(5) 0.2877(5) 0.3965(8) 0.0794(18) Uani 1 1 d DU . . H21 H 0.4212 0.2577 0.3389 0.095 Uiso 1 1 calc R . . C22 C 0.5050(5) 0.2451(6) 0.4359(8) 0.0794(18) Uani 1 1 d U . . H22A H 0.5235 0.2654 0.4972 0.119 Uiso 1 1 calc R . . H22B H 0.5409 0.2536 0.3978 0.119 Uiso 1 1 calc R . . H22C H 0.4949 0.1879 0.4389 0.119 Uiso 1 1 calc R . . C23 C 0.4454(5) 0.3714(5) 0.3635(8) 0.0794(18) Uani 1 1 d DU . . H23A H 0.3982 0.3904 0.3325 0.119 Uiso 1 1 calc R . . H23B H 0.4788 0.3722 0.3212 0.119 Uiso 1 1 calc R . . H23C H 0.4636 0.4062 0.4153 0.119 Uiso 1 1 calc R . . C31 C 0.2849(9) 0.2176(9) 0.1784(11) 0.050(4) Uani 0.572(13) 1 d PDU A 1 H31 H 0.3168 0.2648 0.1767 0.060 Uiso 0.572(13) 1 calc PR A 1 C32 C 0.2111(9) 0.2329(14) 0.1234(9) 0.085(7) Uani 0.572(13) 1 d PU A 1 H32A H 0.2147 0.2443 0.0603 0.128 Uiso 0.572(13) 1 calc PR A 1 H32B H 0.1896 0.2787 0.1487 0.128 Uiso 0.572(13) 1 calc PR A 1 H32C H 0.1810 0.1856 0.1252 0.128 Uiso 0.572(13) 1 calc PR A 1 C33 C 0.3168(10) 0.1439(10) 0.1455(10) 0.072(5) Uani 0.572(13) 1 d PDU A 1 H33A H 0.2855 0.0981 0.1499 0.108 Uiso 0.572(13) 1 calc PR A 1 H33B H 0.3643 0.1342 0.1829 0.108 Uiso 0.572(13) 1 calc PR A 1 H33C H 0.3214 0.1513 0.0821 0.108 Uiso 0.572(13) 1 calc PR A 1 C31A C 0.2601(14) 0.2028(13) 0.1820(14) 0.066(7) Uani 0.428(13) 1 d PDU A 2 H31A H 0.2151 0.2354 0.1729 0.079 Uiso 0.428(13) 1 calc PR A 2 C32A C 0.2299(13) 0.1327(12) 0.1250(12) 0.062(6) Uani 0.428(13) 1 d PDU A 2 H32D H 0.2478 0.0831 0.1559 0.093 Uiso 0.428(13) 1 calc PR A 2 H32E H 0.2447 0.1354 0.0660 0.093 Uiso 0.428(13) 1 calc PR A 2 H32F H 0.1774 0.1337 0.1159 0.093 Uiso 0.428(13) 1 calc PR A 2 C33A C 0.3060(14) 0.2625(15) 0.1452(13) 0.083(8) Uani 0.428(13) 1 d PDU A 2 H33D H 0.3549 0.2415 0.1513 0.124 Uiso 0.428(13) 1 calc PR A 2 H33E H 0.3071 0.3125 0.1793 0.124 Uiso 0.428(13) 1 calc PR A 2 H33F H 0.2860 0.2724 0.0809 0.124 Uiso 0.428(13) 1 calc PR A 2 C41 C 0.4155(4) 0.0313(5) 0.4178(6) 0.068(2) Uani 1 1 d DU A . H41 H 0.4570 0.0474 0.4663 0.081 Uiso 1 1 calc R B 1 C42 C 0.4418(5) 0.0355(6) 0.3311(7) 0.079(2) Uani 1 1 d U . . H42A H 0.4029 0.0207 0.2808 0.119 Uiso 1 1 calc R A . H42B H 0.4821 -0.0014 0.3332 0.119 Uiso 1 1 calc R . . H42C H 0.4576 0.0901 0.3218 0.119 Uiso 1 1 calc R . . C43 C 0.3795(14) -0.0463(14) 0.458(2) 0.079(2) Uani 0.43(3) 1 d PU A 1 H43A H 0.3655 -0.0322 0.5152 0.119 Uiso 0.43(3) 1 calc PR A 1 H43B H 0.4144 -0.0901 0.4679 0.119 Uiso 0.43(3) 1 calc PR A 1 H43C H 0.3370 -0.0633 0.4139 0.119 Uiso 0.43(3) 1 calc PR A 1 C43A C 0.3917(9) -0.0541(6) 0.4185(18) 0.079(2) Uani 0.57(3) 1 d PDU A 2 H43D H 0.3733 -0.0645 0.4741 0.119 Uiso 0.57(3) 1 calc PR A 2 H43E H 0.4325 -0.0894 0.4164 0.119 Uiso 0.57(3) 1 calc PR A 2 H43F H 0.3537 -0.0641 0.3655 0.119 Uiso 0.57(3) 1 calc PR A 2 C51 C 0.1970(5) 0.0234(5) 0.4266(7) 0.067(2) Uani 1 1 d DU A . H51A H 0.2362 -0.0027 0.4710 0.080 Uiso 0.40(3) 1 calc PR C 1 H51B H 0.2454 0.0061 0.4598 0.080 Uiso 0.60(3) 1 calc PR C 2 C52 C 0.1970(16) 0.0034(18) 0.318(2) 0.067(2) Uani 0.40(3) 1 d PU A 1 H52A H 0.1652 0.0409 0.2792 0.100 Uiso 0.40(3) 1 calc PR C 1 H52B H 0.1800 -0.0513 0.3040 0.100 Uiso 0.40(3) 1 calc PR C 1 H52C H 0.2459 0.0088 0.3063 0.100 Uiso 0.40(3) 1 calc PR C 1 C53 C 0.1202(12) 0.0030(14) 0.439(2) 0.053(5) Uani 0.40(3) 1 d PU A 1 H53A H 0.1122 0.0246 0.4965 0.080 Uiso 0.40(3) 1 calc PR C 1 H53B H 0.1141 -0.0551 0.4382 0.080 Uiso 0.40(3) 1 calc PR C 1 H53C H 0.0855 0.0265 0.3887 0.080 Uiso 0.40(3) 1 calc PR C 1 C52A C 0.1861(10) -0.0201(12) 0.3376(10) 0.067(2) Uani 0.60(3) 1 d PDU A 2 H52D H 0.1353 -0.0181 0.3087 0.100 Uiso 0.60(3) 1 calc PR C 2 H52E H 0.2011 -0.0758 0.3481 0.100 Uiso 0.60(3) 1 calc PR C 2 H52F H 0.2149 0.0053 0.2979 0.100 Uiso 0.60(3) 1 calc PR C 2 C53A C 0.1434(12) -0.0057(10) 0.4869(18) 0.064(5) Uani 0.60(3) 1 d PU A 2 H53D H 0.1576 0.0163 0.5482 0.096 Uiso 0.60(3) 1 calc PR C 2 H53E H 0.1443 -0.0642 0.4900 0.096 Uiso 0.60(3) 1 calc PR C 2 H53F H 0.0949 0.0124 0.4603 0.096 Uiso 0.60(3) 1 calc PR C 2 C101 C -0.0317(6) 0.1906(10) 0.3190(8) 0.039(4) Uani 0.503(17) 1 d PU A 1 H10A H -0.0536 0.1683 0.3685 0.047 Uiso 0.503(17) 1 calc PR A 1 H10B H -0.0305 0.2494 0.3260 0.047 Uiso 0.503(17) 1 calc PR A 1 C102 C -0.0641(7) 0.1770(12) 0.2585(10) 0.034(3) Uani 0.503(17) 1 d PU . 1 H10C H -0.0987 0.2217 0.2476 0.041 Uiso 0.503(17) 1 calc PR A 1 H10D H -0.0919 0.1302 0.2724 0.041 Uiso 0.503(17) 1 calc PR A 1 C10A C -0.0211(7) 0.1241(10) 0.3240(9) 0.038(3) Uani 0.497(17) 1 d PU . 2 H10E H -0.0138 0.0657 0.3297 0.046 Uiso 0.497(17) 1 calc PR A 2 H10F H -0.0401 0.1413 0.3780 0.046 Uiso 0.497(17) 1 calc PR A 2 C10B C 0.0748(8) 0.1364(13) 0.2499(10) 0.038(3) Uani 0.497(17) 1 d PU . 2 H10G H 0.1070 0.1788 0.2354 0.046 Uiso 0.497(17) 1 calc PR A 2 H10H H 0.1034 0.0868 0.2625 0.046 Uiso 0.497(17) 1 calc PR A 2 Li1 Li 0.1295(5) 0.1813(7) 0.4422(7) 0.0351(19) Uani 1 1 d U . . 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 0.01903(15) 0.02867(17) 0.01977(15) -0.00303(12) 0.00224(10) 0.00374(12) O1 0.0204(17) 0.032(2) 0.0176(17) 0.0020(15) 0.0011(14) 0.0067(14) O2 0.0238(18) 0.037(2) 0.029(2) -0.0005(17) 0.0059(16) -0.0001(16) O3 0.050(3) 0.058(3) 0.0200(19) -0.0010(19) 0.0040(17) 0.014(2) O4 0.033(2) 0.040(2) 0.038(2) -0.009(2) -0.0046(18) 0.0139(19) O5 0.037(2) 0.035(2) 0.054(3) -0.019(2) 0.017(2) -0.0071(18) O6 0.030(2) 0.123(5) 0.029(2) -0.010(3) -0.0013(18) -0.026(3) C11 0.034(3) 0.048(4) 0.021(3) 0.005(3) 0.001(2) 0.017(3) C12 0.034(3) 0.049(4) 0.034(3) -0.001(3) -0.002(3) 0.021(3) C13 0.049(4) 0.066(5) 0.061(5) 0.039(4) 0.017(4) 0.013(4) C21 0.054(3) 0.078(4) 0.119(5) 0.025(4) 0.048(3) 0.005(3) C22 0.054(3) 0.078(4) 0.119(5) 0.025(4) 0.048(3) 0.005(3) C23 0.054(3) 0.078(4) 0.119(5) 0.025(4) 0.048(3) 0.005(3) C31 0.051(8) 0.080(10) 0.022(5) 0.006(7) 0.016(5) -0.003(7) C32 0.069(9) 0.165(19) 0.019(6) 0.012(8) 0.004(6) 0.048(11) C33 0.096(12) 0.090(12) 0.035(7) 0.006(7) 0.025(8) 0.035(9) C31A 0.101(17) 0.078(12) 0.021(5) 0.001(7) 0.017(10) -0.034(11) C32A 0.091(15) 0.065(12) 0.036(8) -0.012(8) 0.027(9) -0.023(10) C33A 0.107(18) 0.112(18) 0.033(9) -0.015(10) 0.021(11) -0.068(15) C41 0.047(4) 0.058(4) 0.083(6) -0.034(4) -0.026(4) 0.032(3) C42 0.059(4) 0.068(4) 0.104(6) -0.041(4) -0.001(4) 0.035(4) C43 0.059(4) 0.068(4) 0.104(6) -0.041(4) -0.001(4) 0.035(4) C43A 0.059(4) 0.068(4) 0.104(6) -0.041(4) -0.001(4) 0.035(4) C51 0.063(4) 0.037(3) 0.108(6) -0.035(4) 0.037(4) -0.020(3) C52 0.063(4) 0.037(3) 0.108(6) -0.035(4) 0.037(4) -0.020(3) C53 0.043(9) 0.038(10) 0.075(15) 0.021(12) 0.001(9) -0.002(7) C52A 0.063(4) 0.037(3) 0.108(6) -0.035(4) 0.037(4) -0.020(3) C53A 0.073(12) 0.033(7) 0.090(12) 0.007(8) 0.024(10) -0.014(8) C101 0.023(5) 0.064(10) 0.028(6) -0.005(6) 0.000(4) -0.005(5) C102 0.018(5) 0.046(9) 0.037(6) -0.011(7) 0.000(4) -0.012(6) C10A 0.026(5) 0.048(9) 0.036(7) 0.005(6) -0.002(4) -0.005(5) C10B 0.027(7) 0.055(10) 0.029(6) 0.000(7) -0.003(5) 0.008(7) Li1 0.022(3) 0.050(5) 0.032(5) -0.005(4) 0.001(3) -0.004(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 O4 2.080(4) . ? Ce1 O3 2.095(4) . ? Ce1 O5 2.234(4) . ? Ce1 O2 2.257(4) . ? Ce1 O1 2.420(4) . ? Ce1 O1 2.439(4) 7_556 ? Ce1 Li1 3.230(10) . ? Ce1 Li1 3.237(11) 7_556 ? Ce1 Ce1 3.9547(6) 7_556 ? O1 C11 1.448(7) . ? O1 Li1 2.098(12) . ? O1 Ce1 2.439(4) 7_556 ? O2 C21 1.392(9) . ? O2 Li1 1.901(11) 7_556 ? O3 C31A 1.32(2) . ? O3 C31 1.483(16) . ? O4 C41 1.416(8) . ? O5 C51 1.412(9) . ? O5 Li1 1.899(12) . ? O6 C10A 1.429(13) . ? O6 C10B 1.466(16) . ? O6 C102 1.475(16) 2 ? O6 C101 1.584(14) . ? O6 Li1 2.066(11) . ? C11 C13 1.507(11) . ? C11 C12 1.521(8) . ? C11 H11 1.0000 . ? C12 H11A 0.9800 . ? C12 H11B 0.9800 . ? C12 H11C 0.9800 . ? C13 H11D 0.9800 . ? C13 H11E 0.9800 . ? C13 H11F 0.9800 . ? C21 C22 1.468(13) . ? C21 C23 1.4996(10) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C31 C33 1.4998(10) . ? C31 C32 1.50(2) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C31A C32A 1.4998(10) . ? C31A C33A 1.4999(10) . ? C31A H31A 1.0000 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C41 C42 1.482(14) . ? C41 C43A 1.4997(10) . ? C41 C43 1.63(3) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C43A H43D 0.9800 . ? C43A H43E 0.9800 . ? C43A H43F 0.9800 . ? C51 C52A 1.4998(10) . ? C51 C53 1.54(2) . ? C51 C53A 1.564(18) . ? C51 C52 1.67(3) . ? C51 H51A 1.0000 . ? C51 H51B 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C52A H52D 0.9800 . ? C52A H52E 0.9800 . ? C52A H52F 0.9800 . ? C53A H53D 0.9800 . ? C53A H53E 0.9800 . ? C53A H53F 0.9800 . ? C101 C102 1.019(19) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 O6 1.475(16) 2 ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C10A C10B 1.370(19) 2 ? C10A H10E 0.9900 . ? C10A H10F 0.9900 . ? C10B C10A 1.370(19) 2 ? C10B H10G 0.9900 . ? C10B H10H 0.9900 . ? Li1 O2 1.901(11) 7_556 ? Li1 Ce1 3.237(11) 7_556 ? 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 O4 Ce1 O3 98.20(18) . . ? O4 Ce1 O5 90.49(18) . . ? O3 Ce1 O5 98.40(19) . . ? O4 Ce1 O2 95.03(17) . . ? O3 Ce1 O2 96.30(18) . . ? O5 Ce1 O2 163.40(15) . . ? O4 Ce1 O1 164.26(17) . . ? O3 Ce1 O1 90.93(15) . . ? O5 Ce1 O1 75.44(15) . . ? O2 Ce1 O1 96.69(14) . . ? O4 Ce1 O1 102.29(15) . 7_556 ? O3 Ce1 O1 158.01(16) . 7_556 ? O5 Ce1 O1 89.39(15) . 7_556 ? O2 Ce1 O1 74.14(14) . 7_556 ? O1 Ce1 O1 71.07(13) . 7_556 ? O4 Ce1 Li1 124.8(3) . . ? O3 Ce1 Li1 98.4(2) . . ? O5 Ce1 Li1 35.0(2) . . ? O2 Ce1 Li1 134.5(2) . . ? O1 Ce1 Li1 40.5(2) . . ? O1 Ce1 Li1 76.4(2) 7_556 . ? O4 Ce1 Li1 108.1(2) . 7_556 ? O3 Ce1 Li1 124.5(3) . 7_556 ? O5 Ce1 Li1 128.4(2) . 7_556 ? O2 Ce1 Li1 35.1(2) . 7_556 ? O1 Ce1 Li1 76.5(2) . 7_556 ? O1 Ce1 Li1 40.4(2) 7_556 7_556 ? Li1 Ce1 Li1 104.6(2) . 7_556 ? O4 Ce1 Ce1 136.08(13) . 7_556 ? O3 Ce1 Ce1 125.58(13) . 7_556 ? O5 Ce1 Ce1 80.77(11) . 7_556 ? O2 Ce1 Ce1 84.42(10) . 7_556 ? O1 Ce1 Ce1 35.70(8) . 7_556 ? O1 Ce1 Ce1 35.37(8) 7_556 7_556 ? Li1 Ce1 Ce1 52.38(19) . 7_556 ? Li1 Ce1 Ce1 52.21(18) 7_556 7_556 ? C11 O1 Li1 113.8(4) . . ? C11 O1 Ce1 118.6(3) . . ? Li1 O1 Ce1 91.0(3) . . ? C11 O1 Ce1 124.8(3) . 7_556 ? Li1 O1 Ce1 90.7(3) . 7_556 ? Ce1 O1 Ce1 108.93(13) . 7_556 ? C21 O2 Li1 130.9(7) . 7_556 ? C21 O2 Ce1 126.4(6) . . ? Li1 O2 Ce1 101.9(4) 7_556 . ? C31A O3 Ce1 172.8(10) . . ? C31 O3 Ce1 160.9(7) . . ? C41 O4 Ce1 169.4(5) . . ? C51 O5 Li1 126.7(6) . . ? C51 O5 Ce1 130.4(5) . . ? Li1 O5 Ce1 102.5(4) . . ? C10A O6 C10B 106.4(9) . . ? C10A O6 C102 110.7(8) . 2 ? C10A O6 C101 43.7(8) . . ? C10B O6 C101 117.4(8) . . ? C102 O6 C101 100.4(8) 2 . ? C10A O6 Li1 132.4(7) . . ? C10B O6 Li1 113.3(7) . . ? C102 O6 Li1 116.7(7) 2 . ? C101 O6 Li1 126.1(7) . . ? O1 C11 C13 110.7(5) . . ? O1 C11 C12 110.7(5) . . ? C13 C11 C12 112.0(6) . . ? O1 C11 H11 107.8 . . ? C13 C11 H11 107.8 . . ? C12 C11 H11 107.8 . . ? C11 C12 H11A 109.5 . . ? C11 C12 H11B 109.5 . . ? H11A C12 H11B 109.5 . . ? C11 C12 H11C 109.5 . . ? H11A C12 H11C 109.5 . . ? H11B C12 H11C 109.5 . . ? C11 C13 H11D 109.5 . . ? C11 C13 H11E 109.5 . . ? H11D C13 H11E 109.5 . . ? C11 C13 H11F 109.5 . . ? H11D C13 H11F 109.5 . . ? H11E C13 H11F 109.5 . . ? O2 C21 C22 114.2(8) . . ? O2 C21 C23 113.8(7) . . ? C22 C21 C23 117.9(8) . . ? O2 C21 H21 102.7 . . ? C22 C21 H21 102.7 . . ? C23 C21 H21 102.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C31 C33 108.5(11) . . ? O3 C31 C32 104.7(11) . . ? C33 C31 C32 110.6(15) . . ? O3 C31 H31 110.9 . . ? C33 C31 H31 110.9 . . ? C32 C31 H31 110.9 . . ? O3 C31A C32A 123.9(16) . . ? O3 C31A C33A 111.5(14) . . ? C32A C31A C33A 119.8(17) . . ? O3 C31A H31A 97.3 . . ? C32A C31A H31A 97.3 . . ? C33A C31A H31A 97.3 . . ? C31A C32A H32D 109.5 . . ? C31A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C31A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C31A C33A H33D 109.5 . . ? C31A C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C31A C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? O4 C41 C42 111.0(7) . . ? O4 C41 C43A 115.1(9) . . ? C42 C41 C43A 101.8(12) . . ? O4 C41 C43 100.0(11) . . ? C42 C41 C43 126.5(13) . . ? C43A C41 C43 24.7(9) . . ? O4 C41 H41 106.0 . . ? C42 C41 H41 106.0 . . ? C43A C41 H41 116.7 . . ? C43 C41 H41 106.0 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? C41 C43A H43D 109.5 . . ? C41 C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C41 C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? O5 C51 C52A 116.6(11) . . ? O5 C51 C53 106.6(11) . . ? C52A C51 C53 91.4(13) . . ? O5 C51 C53A 112.4(8) . . ? C52A C51 C53A 111.7(10) . . ? C53 C51 C53A 29.3(9) . . ? O5 C51 C52 98.7(13) . . ? C52A C51 C52 19.3(9) . . ? C53 C51 C52 104.4(15) . . ? C53A C51 C52 128.8(12) . . ? O5 C51 H51A 115.1 . . ? C52A C51 H51A 109.8 . . ? C53 C51 H51A 115.1 . . ? C53A C51 H51A 87.8 . . ? C52 C51 H51A 115.1 . . ? O5 C51 H51B 105.0 . . ? C52A C51 H51B 105.0 . . ? C53 C51 H51B 132.5 . . ? C53A C51 H51B 105.0 . . ? C52 C51 H51B 104.8 . . ? H51A C51 H51B 17.4 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? C51 C52A H52D 109.5 . . ? C51 C52A H52E 109.5 . . ? H52D C52A H52E 109.5 . . ? C51 C52A H52F 109.5 . . ? H52D C52A H52F 109.5 . . ? H52E C52A H52F 109.5 . . ? C51 C53A H53D 109.5 . . ? C51 C53A H53E 109.5 . . ? H53D C53A H53E 109.5 . . ? C51 C53A H53F 109.5 . . ? H53D C53A H53F 109.5 . . ? H53E C53A H53F 109.5 . . ? C102 C101 O6 115.7(14) . . ? C102 C101 H10A 108.3 . . ? O6 C101 H10A 108.3 . . ? C102 C101 H10B 108.3 . . ? O6 C101 H10B 108.3 . . ? H10A C101 H10B 107.4 . . ? C101 C102 O6 132.1(14) . 2 ? C101 C102 H10C 104.2 . . ? O6 C102 H10C 104.2 2 . ? C101 C102 H10D 104.2 . . ? O6 C102 H10D 104.2 2 . ? H10C C102 H10D 105.5 . . ? C10B C10A O6 122.4(12) 2 . ? C10B C10A H10E 106.7 2 . ? O6 C10A H10E 106.7 . . ? C10B C10A H10F 106.7 2 . ? O6 C10A H10F 106.7 . . ? H10E C10A H10F 106.6 . . ? C10A C10B O6 113.4(12) 2 . ? C10A C10B H10G 108.9 2 . ? O6 C10B H10G 108.9 . . ? C10A C10B H10H 108.9 2 . ? O6 C10B H10H 108.9 . . ? H10G C10B H10H 107.7 . . ? O5 Li1 O2 126.3(6) . 7_556 ? O5 Li1 O6 101.9(5) . . ? O2 Li1 O6 125.5(5) 7_556 . ? O5 Li1 O1 90.9(4) . . ? O2 Li1 O1 90.1(5) 7_556 . ? O6 Li1 O1 115.4(6) . . ? O5 Li1 Ce1 42.5(2) . . ? O2 Li1 Ce1 113.8(4) 7_556 . ? O6 Li1 Ce1 119.2(4) . . ? O1 Li1 Ce1 48.5(2) . . ? O5 Li1 Ce1 107.6(4) . 7_556 ? O2 Li1 Ce1 43.0(3) 7_556 7_556 ? O6 Li1 Ce1 146.1(6) . 7_556 ? O1 Li1 Ce1 48.9(2) . 7_556 ? Ce1 Li1 Ce1 75.4(2) . 7_556 ?