# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' # Attachment '9067805880598084.cif' _journal_coden_Cambridge 0222 #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Polly L Arnold' _publ_contact_author_email Polly.Arnold@ed.ac.uk _publ_contact_author_fax '+44 131 650 6453' _publ_contact_author_phone '+44 131 650 5429' #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_address 'Polly L Arnold' ; School of Chemistry Joseph Black Building, University of Edinburgh, The King's Buildings, Edinburgh, EH9 3JJ, UK. ; 'Ronan Bellabarba' . 'Ian J. Casely' . 'Anne I. Germeroth' . 'R P Tooze' . ; Z.R.Turner ; . ##===========end of cif========================= data_po8058_CeLm2N _database_code_depnum_ccdc_archive 'CCDC 763328' #TrackingRef '9067805880598084.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H64 Ce N5 O2 Si2' _chemical_formula_sum 'C38 H64 Ce N5 O2 Si2' _chemical_formula_weight 819.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.1139(4) _cell_length_b 18.0530(6) _cell_length_c 11.5188(4) _cell_angle_alpha 89.924(2) _cell_angle_beta 112.910(2) _cell_angle_gamma 89.187(2) _cell_volume 2128.54(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15887 _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 28.4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 1.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6272 _exptl_absorpt_correction_T_max 0.8202 _exptl_absorpt_process_details SADABS _exptl_special_details ; Single crystals were grown from a toluene solution at room temperature. Crystal was a two component twin and was refined using hklf5. Twin law; Rotated from first domain by 178.8 degrees about reciprocal axis 1.000 0.060 0.960 and real axis 1.000 0.006 0.978 Twin law to convert hkl from first to 0.032 -0.005 1.009 this domain (SHELXL TWIN matrix): 0.082 -1.000 0.041 0.990 0.016 -0.032 Data is not fully merged due to structure being twinned ; _diffrn_ambient_temperature 150(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 'Brucker SMART APEX CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17055 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 28.40 _reflns_number_total 17055 _reflns_number_gt 15887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement 'SAINT (Siemans, 1995)' _computing_data_reduction 'SAINT (Siemans, 1995)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^)+(0.0352P)^2^+5.4025P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17055 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1269 _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 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1674(4) 0.3082(2) 0.4259(4) 0.0251(8) Uani 1 1 d . . . C5 C -0.0348(5) 0.3288(3) 0.2537(5) 0.0370(11) Uani 1 1 d . . . H5A H -0.1145 0.3063 0.2563 0.044 Uiso 1 1 calc R . . H5B H -0.0485 0.3392 0.1650 0.044 Uiso 1 1 calc R . . C6 C 0.0023(5) 0.3980(3) 0.3335(5) 0.0362(11) Uani 1 1 d . . . H6A H 0.0202 0.4394 0.2864 0.043 Uiso 1 1 calc R . . H6B H -0.0675 0.4133 0.3621 0.043 Uiso 1 1 calc R . . C7 C 0.1884(5) 0.4283(3) 0.5379(5) 0.0336(10) Uani 1 1 d . . . H7A H 0.1285 0.4709 0.5293 0.040 Uiso 1 1 calc R . . H7B H 0.2647 0.4468 0.5231 0.040 Uiso 1 1 calc R . . C8 C 0.2363(4) 0.3981(2) 0.6747(4) 0.0269(9) Uani 1 1 d . . . C9 C 0.1206(6) 0.3696(4) 0.7013(6) 0.0526(16) Uani 1 1 d . . . H9A H 0.0792 0.3293 0.6432 0.079 Uiso 1 1 calc R . . H9B H 0.0570 0.4100 0.6894 0.079 Uiso 1 1 calc R . . H9C H 0.1516 0.3512 0.7883 0.079 Uiso 1 1 calc R . . C10 C 0.3014(5) 0.4622(3) 0.7636(5) 0.0413(12) Uani 1 1 d . . . H10A H 0.3316 0.4449 0.8512 0.062 Uiso 1 1 calc R . . H10B H 0.2380 0.5029 0.7499 0.062 Uiso 1 1 calc R . . H10C H 0.3760 0.4795 0.7464 0.062 Uiso 1 1 calc R . . C11 C 0.5787(4) 0.1850(2) 0.8328(4) 0.0229(8) Uani 1 1 d . . . C15 C 0.7417(5) 0.1675(3) 1.0372(4) 0.0322(10) Uani 1 1 d . . . H15A H 0.7415 0.1910 1.1147 0.039 Uiso 1 1 calc R . . H15B H 0.8326 0.1544 1.0493 0.039 Uiso 1 1 calc R . . C16 C 0.6542(5) 0.1000(3) 1.0015(4) 0.0333(10) Uani 1 1 d . . . H16A H 0.7055 0.0541 1.0055 0.040 Uiso 1 1 calc R . . H16B H 0.6059 0.0945 1.0572 0.040 Uiso 1 1 calc R . . C17 C 0.4648(5) 0.0645(2) 0.8027(4) 0.0294(10) Uani 1 1 d . . . H17A H 0.4743 0.0206 0.8572 0.035 Uiso 1 1 calc R . . H17B H 0.4808 0.0479 0.7280 0.035 Uiso 1 1 calc R . . C18 C 0.3242(5) 0.0935(2) 0.7585(4) 0.0269(9) Uani 1 1 d . . . C19 C 0.2953(6) 0.1224(3) 0.8704(5) 0.0417(13) Uani 1 1 d . . . H19A H 0.3526 0.1639 0.9092 0.063 Uiso 1 1 calc R . . H19B H 0.3108 0.0826 0.9327 0.063 Uiso 1 1 calc R . . H19C H 0.2039 0.1392 0.8407 0.063 Uiso 1 1 calc R . . C20 C 0.2326(5) 0.0309(3) 0.6945(5) 0.0416(12) Uani 1 1 d . . . H20A H 0.1419 0.0482 0.6690 0.062 Uiso 1 1 calc R . . H20B H 0.2491 -0.0109 0.7532 0.062 Uiso 1 1 calc R . . H20C H 0.2478 0.0151 0.6199 0.062 Uiso 1 1 calc R . . C21 C 0.0894(4) 0.2073(2) 0.2720(4) 0.0254(9) Uani 1 1 d . . . C22 C 0.0491(4) 0.1478(3) 0.3248(4) 0.0289(9) Uani 1 1 d . . . C23 C 0.0601(5) 0.0766(3) 0.2811(5) 0.0348(10) Uani 1 1 d . . . H23 H 0.0339 0.0353 0.3163 0.042 Uiso 1 1 calc R . . C24 C 0.1082(5) 0.0646(3) 0.1878(5) 0.0366(11) Uani 1 1 d . . . C25 C 0.1421(5) 0.1256(3) 0.1358(4) 0.0343(11) Uani 1 1 d . . . H25 H 0.1718 0.1182 0.0697 0.041 Uiso 1 1 calc R . . C26 C 0.1349(4) 0.1975(3) 0.1757(4) 0.0293(9) Uani 1 1 d . . . C31 C 0.7178(4) 0.2909(2) 0.9245(4) 0.0274(9) Uani 1 1 d . . . C32 C 0.6549(5) 0.3473(3) 0.9656(4) 0.0323(10) Uani 1 1 d . . . C33 C 0.6939(5) 0.4186(3) 0.9632(5) 0.0403(12) Uani 1 1 d . . . H33 H 0.6509 0.4572 0.9889 0.048 Uiso 1 1 calc R . . C34 C 0.7932(5) 0.4369(3) 0.9249(5) 0.0402(12) Uani 1 1 d . . . C35 C 0.8565(5) 0.3807(3) 0.8893(5) 0.0379(11) Uani 1 1 d . . . H35 H 0.9271 0.3924 0.8658 0.045 Uiso 1 1 calc R . . C36 C 0.8195(4) 0.3070(3) 0.8867(4) 0.0279(9) Uani 1 1 d . . . C37 C 0.5749(5) 0.4025(3) 0.5932(5) 0.0361(11) Uani 1 1 d . . . H37A H 0.4838 0.4119 0.5814 0.054 Uiso 1 1 calc R . . H37B H 0.6151 0.4491 0.5849 0.054 Uiso 1 1 calc R . . H37C H 0.6229 0.3812 0.6773 0.054 Uiso 1 1 calc R . . C38 C 0.7520(6) 0.3356(3) 0.4787(7) 0.0584(18) Uani 1 1 d . . . H38A H 0.8111 0.3147 0.5597 0.088 Uiso 1 1 calc R . . H38B H 0.7774 0.3865 0.4703 0.088 Uiso 1 1 calc R . . H38C H 0.7571 0.3055 0.4100 0.088 Uiso 1 1 calc R . . C39 C 0.4743(6) 0.3791(3) 0.3162(5) 0.0466(14) Uani 1 1 d . . . H39A H 0.4778 0.3485 0.2473 0.070 Uiso 1 1 calc R . . H39B H 0.5056 0.4288 0.3100 0.070 Uiso 1 1 calc R . . H39C H 0.3840 0.3825 0.3103 0.070 Uiso 1 1 calc R . . C40 C 0.4292(5) 0.1011(3) 0.4372(5) 0.0355(11) Uani 1 1 d . . . H40A H 0.4317 0.0946 0.5226 0.053 Uiso 1 1 calc R . . H40B H 0.4464 0.0533 0.4059 0.053 Uiso 1 1 calc R . . H40C H 0.3428 0.1200 0.3815 0.053 Uiso 1 1 calc R . . C41 C 0.5545(6) 0.1709(3) 0.2755(5) 0.0465(14) Uani 1 1 d . . . H41A H 0.4675 0.1867 0.2161 0.070 Uiso 1 1 calc R . . H41B H 0.5749 0.1213 0.2531 0.070 Uiso 1 1 calc R . . H41C H 0.6196 0.2058 0.2718 0.070 Uiso 1 1 calc R . . C42 C 0.7177(5) 0.1265(3) 0.5449(5) 0.0416(12) Uani 1 1 d . . . H42A H 0.7887 0.1584 0.5460 0.062 Uiso 1 1 calc R . . H42B H 0.7279 0.0776 0.5129 0.062 Uiso 1 1 calc R . . H42C H 0.7204 0.1214 0.6306 0.062 Uiso 1 1 calc R . . C220 C -0.0040(5) 0.1576(3) 0.4251(5) 0.0396(12) Uani 1 1 d . . . H22A H 0.0675 0.1689 0.5053 0.059 Uiso 1 1 calc R . . H22B H -0.0462 0.1118 0.4341 0.059 Uiso 1 1 calc R . . H22C H -0.0682 0.1984 0.4015 0.059 Uiso 1 1 calc R . . C240 C 0.1287(7) -0.0127(3) 0.1499(6) 0.0532(15) Uani 1 1 d . . . H24A H 0.2182 -0.0296 0.2006 0.080 Uiso 1 1 calc R . . H24B H 0.1146 -0.0130 0.0605 0.080 Uiso 1 1 calc R . . H24C H 0.0668 -0.0460 0.1641 0.080 Uiso 1 1 calc R . . C260 C 0.1801(5) 0.2621(3) 0.1214(5) 0.0391(11) Uani 1 1 d . . . H26A H 0.2518 0.2866 0.1886 0.059 Uiso 1 1 calc R . . H26B H 0.1074 0.2975 0.0833 0.059 Uiso 1 1 calc R . . H26C H 0.2104 0.2445 0.0569 0.059 Uiso 1 1 calc R . . C320 C 0.5436(6) 0.3287(3) 1.0056(5) 0.0450(13) Uani 1 1 d . . . H32A H 0.4675 0.3136 0.9317 0.067 Uiso 1 1 calc R . . H32B H 0.5204 0.3725 1.0433 0.067 Uiso 1 1 calc R . . H32C H 0.5710 0.2882 1.0675 0.067 Uiso 1 1 calc R . . C340 C 0.8275(7) 0.5170(3) 0.9183(8) 0.072(2) Uani 1 1 d . . . H34A H 0.7517 0.5438 0.8576 0.108 Uiso 1 1 calc R . . H34B H 0.9008 0.5198 0.8914 0.108 Uiso 1 1 calc R . . H34C H 0.8522 0.5395 1.0017 0.108 Uiso 1 1 calc R . . C360 C 0.8835(5) 0.2464(3) 0.8394(5) 0.0373(11) Uani 1 1 d . . . H36A H 0.9156 0.2070 0.9031 0.056 Uiso 1 1 calc R . . H36B H 0.9568 0.2668 0.8233 0.056 Uiso 1 1 calc R . . H36C H 0.8195 0.2262 0.7612 0.056 Uiso 1 1 calc R . . N1 N 0.1211(4) 0.3743(2) 0.4402(4) 0.0307(8) Uani 1 1 d . . . N2 N 0.0818(4) 0.2807(2) 0.3166(3) 0.0273(8) Uani 1 1 d . . . N3 N 0.5651(4) 0.1172(2) 0.8715(3) 0.0246(7) Uani 1 1 d . . . N4 N 0.6783(3) 0.2161(2) 0.9253(3) 0.0258(7) Uani 1 1 d . . . N5 N 0.5276(4) 0.2520(2) 0.4931(4) 0.0263(7) Uani 1 1 d . . . O1 O 0.3275(3) 0.34163(17) 0.6916(3) 0.0262(6) Uani 1 1 d . . . O2 O 0.3052(3) 0.15100(17) 0.6709(3) 0.0276(7) Uani 1 1 d . . . Si1 Si 0.58041(12) 0.33592(7) 0.47105(12) 0.0273(3) Uani 1 1 d . . . Si2 Si 0.55728(13) 0.16884(7) 0.44024(11) 0.0266(3) Uani 1 1 d . . . Ce1 Ce 0.38900(2) 0.245969(13) 0.61323(2) 0.01718(6) 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 0.026(2) 0.024(2) 0.022(2) -0.0016(16) 0.0061(18) 0.0035(16) C5 0.029(2) 0.046(3) 0.027(2) -0.005(2) 0.002(2) 0.012(2) C6 0.031(2) 0.037(3) 0.031(2) 0.002(2) 0.002(2) 0.014(2) C7 0.034(2) 0.023(2) 0.033(2) -0.0049(19) 0.002(2) 0.0045(19) C8 0.023(2) 0.027(2) 0.027(2) -0.0080(17) 0.0047(19) 0.0026(17) C9 0.036(3) 0.078(5) 0.050(3) -0.020(3) 0.023(3) -0.010(3) C10 0.042(3) 0.033(3) 0.037(3) -0.013(2) 0.002(3) 0.009(2) C11 0.0222(19) 0.025(2) 0.0215(19) 0.0011(16) 0.0091(17) 0.0005(16) C15 0.030(2) 0.036(3) 0.023(2) 0.0107(19) 0.002(2) 0.0003(19) C16 0.039(3) 0.032(3) 0.024(2) 0.0081(19) 0.007(2) 0.000(2) C17 0.041(3) 0.019(2) 0.028(2) 0.0023(17) 0.012(2) -0.0041(19) C18 0.031(2) 0.023(2) 0.029(2) 0.0002(17) 0.013(2) -0.0053(17) C19 0.044(3) 0.049(3) 0.037(3) 0.002(2) 0.022(3) 0.000(3) C20 0.042(3) 0.031(3) 0.043(3) 0.005(2) 0.007(3) -0.013(2) C21 0.0204(19) 0.030(2) 0.0205(19) -0.0054(16) 0.0018(17) 0.0011(16) C22 0.0179(19) 0.039(3) 0.024(2) -0.0039(18) 0.0008(18) -0.0023(18) C23 0.029(2) 0.032(3) 0.034(3) 0.000(2) 0.003(2) -0.0037(19) C24 0.038(3) 0.032(3) 0.031(2) -0.008(2) 0.004(2) 0.002(2) C25 0.037(3) 0.040(3) 0.022(2) -0.0076(19) 0.008(2) 0.004(2) C26 0.025(2) 0.039(3) 0.020(2) -0.0039(18) 0.0052(19) 0.0017(19) C31 0.027(2) 0.026(2) 0.022(2) 0.0021(16) 0.0015(18) -0.0024(17) C32 0.035(2) 0.036(3) 0.019(2) -0.0015(19) 0.003(2) 0.004(2) C33 0.046(3) 0.032(3) 0.028(2) -0.011(2) -0.001(2) 0.003(2) C34 0.036(3) 0.026(3) 0.035(3) -0.004(2) -0.012(2) -0.011(2) C35 0.031(2) 0.042(3) 0.032(2) 0.005(2) 0.003(2) -0.010(2) C36 0.024(2) 0.033(2) 0.020(2) -0.0040(17) 0.0004(18) -0.0096(18) C37 0.044(3) 0.026(2) 0.034(2) -0.0025(19) 0.011(2) -0.005(2) C38 0.036(3) 0.050(4) 0.101(5) 0.003(3) 0.040(4) -0.006(3) C39 0.064(4) 0.038(3) 0.033(3) 0.011(2) 0.014(3) -0.008(3) C40 0.041(3) 0.030(3) 0.036(3) -0.002(2) 0.015(2) 0.001(2) C41 0.069(4) 0.046(3) 0.037(3) -0.002(2) 0.034(3) 0.005(3) C42 0.037(3) 0.047(3) 0.037(3) -0.003(2) 0.011(2) 0.016(2) C220 0.034(3) 0.053(3) 0.035(3) 0.006(2) 0.017(2) -0.002(2) C240 0.064(4) 0.038(3) 0.044(3) -0.011(3) 0.006(3) 0.009(3) C260 0.040(3) 0.044(3) 0.036(3) -0.001(2) 0.018(2) -0.003(2) C320 0.051(3) 0.055(4) 0.034(3) 0.005(2) 0.022(3) 0.012(3) C340 0.050(4) 0.032(3) 0.095(5) 0.006(3) -0.014(4) -0.011(3) C360 0.032(2) 0.043(3) 0.038(3) -0.005(2) 0.015(2) -0.006(2) N1 0.0263(19) 0.030(2) 0.0263(19) -0.0052(16) 0.0005(17) 0.0108(16) N2 0.0255(18) 0.0287(19) 0.0214(17) -0.0041(14) 0.0024(16) 0.0069(15) N3 0.0270(18) 0.0230(19) 0.0208(17) 0.0079(14) 0.0061(16) 0.0001(14) N4 0.0249(18) 0.0268(18) 0.0185(16) 0.0059(14) 0.0007(15) -0.0027(14) N5 0.0290(19) 0.0268(18) 0.0264(18) 0.0008(14) 0.0143(17) 0.0015(14) O1 0.0265(15) 0.0260(16) 0.0231(15) -0.0026(12) 0.0064(14) 0.0057(12) O2 0.0275(16) 0.0258(16) 0.0294(16) 0.0031(13) 0.0108(15) -0.0050(13) Si1 0.0256(6) 0.0306(7) 0.0291(6) 0.0030(5) 0.0144(5) -0.0014(5) Si2 0.0316(6) 0.0290(6) 0.0228(6) 0.0003(5) 0.0146(5) 0.0046(5) Ce1 0.01809(10) 0.01731(9) 0.01675(10) 0.00164(7) 0.00752(7) 0.00144(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 N1 1.328(5) . ? C1 N2 1.348(6) . ? C1 Ce1 2.786(4) . ? C5 N2 1.480(6) . ? C5 C6 1.516(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.469(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N1 1.465(6) . ? C7 C8 1.549(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O1 1.386(5) . ? C8 C9 1.528(7) . ? C8 C10 1.536(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.332(5) . ? C11 N4 1.334(5) . ? C11 Ce1 2.798(4) . ? C15 N4 1.483(5) . ? C15 C16 1.524(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N3 1.467(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N3 1.456(6) . ? C17 C18 1.527(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O2 1.402(5) . ? C18 C20 1.519(7) . ? C18 C19 1.535(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.396(6) . ? C21 C26 1.397(6) . ? C21 N2 1.436(5) . ? C22 C23 1.401(7) . ? C22 C220 1.498(6) . ? C23 C24 1.390(7) . ? C23 H23 0.9500 . ? C24 C25 1.379(7) . ? C24 C240 1.504(7) . ? C25 C26 1.389(7) . ? C25 H25 0.9500 . ? C26 C260 1.505(7) . ? C31 C36 1.394(6) . ? C31 C32 1.410(6) . ? C31 N4 1.427(5) . ? C32 C33 1.368(7) . ? C32 C320 1.520(7) . ? C33 C34 1.383(7) . ? C33 H33 0.9500 . ? C34 C35 1.378(8) . ? C34 C340 1.510(8) . ? C35 C36 1.395(7) . ? C35 H35 0.9500 . ? C36 C360 1.509(7) . ? C37 Si1 1.870(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 Si1 1.874(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 Si1 1.874(6) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 Si2 1.880(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 Si2 1.886(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 Si2 1.871(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C220 H22A 0.9800 . ? C220 H22B 0.9800 . ? C220 H22C 0.9800 . ? C240 H24A 0.9800 . ? C240 H24B 0.9800 . ? C240 H24C 0.9800 . ? C260 H26A 0.9800 . ? C260 H26B 0.9800 . ? C260 H26C 0.9800 . ? C320 H32A 0.9800 . ? C320 H32B 0.9800 . ? C320 H32C 0.9800 . ? C340 H34A 0.9800 . ? C340 H34B 0.9800 . ? C340 H34C 0.9800 . ? C360 H36A 0.9800 . ? C360 H36B 0.9800 . ? C360 H36C 0.9800 . ? N5 Si1 1.687(4) . ? N5 Si2 1.697(4) . ? N5 Ce1 2.442(3) . ? O1 Ce1 2.172(3) . ? O2 Ce1 2.184(3) . ? Si2 Ce1 3.4990(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 106.7(4) . . ? N1 C1 Ce1 121.3(3) . . ? N2 C1 Ce1 131.7(3) . . ? N2 C5 C6 101.4(4) . . ? N2 C5 H5A 111.5 . . ? C6 C5 H5A 111.5 . . ? N2 C5 H5B 111.5 . . ? C6 C5 H5B 111.5 . . ? H5A C5 H5B 109.3 . . ? N1 C6 C5 102.8(4) . . ? N1 C6 H6A 111.2 . . ? C5 C6 H6A 111.2 . . ? N1 C6 H6B 111.2 . . ? C5 C6 H6B 111.2 . . ? H6A C6 H6B 109.1 . . ? N1 C7 C8 114.8(4) . . ? N1 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? O1 C8 C9 110.2(4) . . ? O1 C8 C10 109.2(4) . . ? C9 C8 C10 110.3(4) . . ? O1 C8 C7 109.6(3) . . ? C9 C8 C7 110.0(4) . . ? C10 C8 C7 107.5(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 N4 107.4(4) . . ? N3 C11 Ce1 120.7(3) . . ? N4 C11 Ce1 131.0(3) . . ? N4 C15 C16 101.5(4) . . ? N4 C15 H15A 111.5 . . ? C16 C15 H15A 111.5 . . ? N4 C15 H15B 111.5 . . ? C16 C15 H15B 111.5 . . ? H15A C15 H15B 109.3 . . ? N3 C16 C15 102.7(3) . . ? N3 C16 H16A 111.2 . . ? C15 C16 H16A 111.2 . . ? N3 C16 H16B 111.2 . . ? C15 C16 H16B 111.2 . . ? H16A C16 H16B 109.1 . . ? N3 C17 C18 115.5(4) . . ? N3 C17 H17A 108.4 . . ? C18 C17 H17A 108.4 . . ? N3 C17 H17B 108.4 . . ? C18 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? O2 C18 C20 108.8(4) . . ? O2 C18 C17 109.2(3) . . ? C20 C18 C17 108.7(4) . . ? O2 C18 C19 109.5(4) . . ? C20 C18 C19 110.1(4) . . ? C17 C18 C19 110.7(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 121.9(4) . . ? C22 C21 N2 119.0(4) . . ? C26 C21 N2 119.1(4) . . ? C21 C22 C23 117.7(4) . . ? C21 C22 C220 122.5(4) . . ? C23 C22 C220 119.8(4) . . ? C24 C23 C22 122.0(4) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C25 C24 C23 117.8(4) . . ? C25 C24 C240 121.3(5) . . ? C23 C24 C240 120.8(5) . . ? C24 C25 C26 123.0(4) . . ? C24 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? C25 C26 C21 117.5(4) . . ? C25 C26 C260 121.3(4) . . ? C21 C26 C260 121.2(4) . . ? C36 C31 C32 121.1(4) . . ? C36 C31 N4 119.9(4) . . ? C32 C31 N4 118.9(4) . . ? C33 C32 C31 117.8(4) . . ? C33 C32 C320 121.8(5) . . ? C31 C32 C320 120.3(5) . . ? C32 C33 C34 122.8(5) . . ? C32 C33 H33 118.6 . . ? C34 C33 H33 118.6 . . ? C35 C34 C33 118.4(5) . . ? C35 C34 C340 121.2(5) . . ? C33 C34 C340 120.3(5) . . ? C34 C35 C36 121.7(5) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C31 C36 C35 118.1(4) . . ? C31 C36 C360 120.6(4) . . ? C35 C36 C360 121.3(4) . . ? Si1 C37 H37A 109.5 . . ? Si1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si1 C38 H38A 109.5 . . ? Si1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si1 C39 H39A 109.5 . . ? Si1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si2 C40 H40A 109.5 . . ? Si2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si2 C41 H41A 109.5 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si2 C42 H42A 109.5 . . ? Si2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C22 C220 H22A 109.5 . . ? C22 C220 H22B 109.5 . . ? H22A C220 H22B 109.5 . . ? C22 C220 H22C 109.5 . . ? H22A C220 H22C 109.5 . . ? H22B C220 H22C 109.5 . . ? C24 C240 H24A 109.5 . . ? C24 C240 H24B 109.5 . . ? H24A C240 H24B 109.5 . . ? C24 C240 H24C 109.5 . . ? H24A C240 H24C 109.5 . . ? H24B C240 H24C 109.5 . . ? C26 C260 H26A 109.5 . . ? C26 C260 H26B 109.5 . . ? H26A C260 H26B 109.5 . . ? C26 C260 H26C 109.5 . . ? H26A C260 H26C 109.5 . . ? H26B C260 H26C 109.5 . . ? C32 C320 H32A 109.5 . . ? C32 C320 H32B 109.5 . . ? H32A C320 H32B 109.5 . . ? C32 C320 H32C 109.5 . . ? H32A C320 H32C 109.5 . . ? H32B C320 H32C 109.5 . . ? C34 C340 H34A 109.5 . . ? C34 C340 H34B 109.5 . . ? H34A C340 H34B 109.5 . . ? C34 C340 H34C 109.5 . . ? H34A C340 H34C 109.5 . . ? H34B C340 H34C 109.5 . . ? C36 C360 H36A 109.5 . . ? C36 C360 H36B 109.5 . . ? H36A C360 H36B 109.5 . . ? C36 C360 H36C 109.5 . . ? H36A C360 H36C 109.5 . . ? H36B C360 H36C 109.5 . . ? C1 N1 C7 126.2(4) . . ? C1 N1 C6 114.1(4) . . ? C7 N1 C6 118.7(4) . . ? C1 N2 C21 124.4(4) . . ? C1 N2 C5 113.9(4) . . ? C21 N2 C5 121.1(4) . . ? C11 N3 C17 126.3(4) . . ? C11 N3 C16 114.0(4) . . ? C17 N3 C16 119.4(4) . . ? C11 N4 C31 124.7(4) . . ? C11 N4 C15 114.0(4) . . ? C31 N4 C15 121.1(4) . . ? Si1 N5 Si2 127.9(2) . . ? Si1 N5 Ce1 117.80(18) . . ? Si2 N5 Ce1 114.25(19) . . ? C8 O1 Ce1 147.8(3) . . ? C18 O2 Ce1 147.1(3) . . ? N5 Si1 C37 110.6(2) . . ? N5 Si1 C39 112.5(2) . . ? C37 Si1 C39 105.2(3) . . ? N5 Si1 C38 114.2(2) . . ? C37 Si1 C38 106.7(3) . . ? C39 Si1 C38 107.0(3) . . ? N5 Si2 C42 112.7(2) . . ? N5 Si2 C40 109.8(2) . . ? C42 Si2 C40 106.0(3) . . ? N5 Si2 C41 114.6(2) . . ? C42 Si2 C41 107.1(2) . . ? C40 Si2 C41 106.1(3) . . ? C42 Si2 Ce1 111.93(16) . . ? C40 Si2 Ce1 72.60(15) . . ? C41 Si2 Ce1 139.72(19) . . ? O1 Ce1 O2 105.00(10) . . ? O1 Ce1 N5 124.33(13) . . ? O2 Ce1 N5 130.65(12) . . ? O1 Ce1 C1 71.79(12) . . ? O2 Ce1 C1 100.99(12) . . ? N5 Ce1 C1 95.91(13) . . ? O1 Ce1 C11 100.04(11) . . ? O2 Ce1 C11 71.56(12) . . ? N5 Ce1 C11 96.48(12) . . ? C1 Ce1 C11 167.55(10) . . ? O1 Ce1 Si2 150.56(8) . . ? O2 Ce1 Si2 104.44(8) . . ? N5 Ce1 Si2 26.24(10) . . ? C1 Ce1 Si2 102.62(8) . . ? C11 Ce1 Si2 89.08(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 N2 C5 C6 N1 -9.5(5) . . . . ? N1 C7 C8 O1 62.5(5) . . . . ? N1 C7 C8 C9 -58.8(5) . . . . ? N1 C7 C8 C10 -178.9(4) . . . . ? N4 C15 C16 N3 5.8(4) . . . . ? N3 C17 C18 O2 64.2(5) . . . . ? N3 C17 C18 C20 -177.3(4) . . . . ? N3 C17 C18 C19 -56.3(5) . . . . ? C26 C21 C22 C23 2.3(6) . . . . ? N2 C21 C22 C23 -178.8(4) . . . . ? C26 C21 C22 C220 -177.9(4) . . . . ? N2 C21 C22 C220 1.0(6) . . . . ? C21 C22 C23 C24 -0.5(7) . . . . ? C220 C22 C23 C24 179.7(5) . . . . ? C22 C23 C24 C25 -1.8(7) . . . . ? C22 C23 C24 C240 175.2(5) . . . . ? C23 C24 C25 C26 2.5(8) . . . . ? C240 C24 C25 C26 -174.5(5) . . . . ? C24 C25 C26 C21 -0.7(8) . . . . ? C24 C25 C26 C260 176.5(5) . . . . ? C22 C21 C26 C25 -1.7(7) . . . . ? N2 C21 C26 C25 179.4(4) . . . . ? C22 C21 C26 C260 -179.0(4) . . . . ? N2 C21 C26 C260 2.2(6) . . . . ? C36 C31 C32 C33 2.2(7) . . . . ? N4 C31 C32 C33 -179.6(4) . . . . ? C36 C31 C32 C320 179.6(4) . . . . ? N4 C31 C32 C320 -2.2(7) . . . . ? C31 C32 C33 C34 -1.4(7) . . . . ? C320 C32 C33 C34 -178.7(5) . . . . ? C32 C33 C34 C35 -0.9(8) . . . . ? C32 C33 C34 C340 177.1(6) . . . . ? C33 C34 C35 C36 2.4(8) . . . . ? C340 C34 C35 C36 -175.5(5) . . . . ? C32 C31 C36 C35 -0.8(7) . . . . ? N4 C31 C36 C35 -179.0(4) . . . . ? C32 C31 C36 C360 -178.3(4) . . . . ? N4 C31 C36 C360 3.5(6) . . . . ? C34 C35 C36 C31 -1.5(7) . . . . ? C34 C35 C36 C360 175.9(5) . . . . ? N2 C1 N1 C7 -172.6(4) . . . . ? Ce1 C1 N1 C7 12.6(6) . . . . ? N2 C1 N1 C6 -4.1(5) . . . . ? Ce1 C1 N1 C6 -178.8(3) . . . . ? C8 C7 N1 C1 -54.4(6) . . . . ? C8 C7 N1 C6 137.5(4) . . . . ? C5 C6 N1 C1 9.1(5) . . . . ? C5 C6 N1 C7 178.5(4) . . . . ? N1 C1 N2 C21 -174.0(4) . . . . ? Ce1 C1 N2 C21 0.0(6) . . . . ? N1 C1 N2 C5 -3.1(5) . . . . ? Ce1 C1 N2 C5 170.9(3) . . . . ? C22 C21 N2 C1 77.4(5) . . . . ? C26 C21 N2 C1 -103.7(5) . . . . ? C22 C21 N2 C5 -92.9(5) . . . . ? C26 C21 N2 C5 86.0(5) . . . . ? C6 C5 N2 C1 8.3(5) . . . . ? C6 C5 N2 C21 179.6(4) . . . . ? N4 C11 N3 C17 177.3(4) . . . . ? Ce1 C11 N3 C17 7.6(5) . . . . ? N4 C11 N3 C16 3.6(5) . . . . ? Ce1 C11 N3 C16 -166.1(3) . . . . ? C18 C17 N3 C11 -53.6(5) . . . . ? C18 C17 N3 C16 119.8(4) . . . . ? C15 C16 N3 C11 -6.2(5) . . . . ? C15 C16 N3 C17 179.6(4) . . . . ? N3 C11 N4 C31 -174.9(4) . . . . ? Ce1 C11 N4 C31 -6.6(6) . . . . ? N3 C11 N4 C15 0.8(5) . . . . ? Ce1 C11 N4 C15 169.1(3) . . . . ? C36 C31 N4 C11 -96.7(5) . . . . ? C32 C31 N4 C11 85.1(5) . . . . ? C36 C31 N4 C15 87.9(5) . . . . ? C32 C31 N4 C15 -90.4(5) . . . . ? C16 C15 N4 C11 -4.4(5) . . . . ? C16 C15 N4 C31 171.5(4) . . . . ? C9 C8 O1 Ce1 83.2(6) . . . . ? C10 C8 O1 Ce1 -155.6(4) . . . . ? C7 C8 O1 Ce1 -38.0(7) . . . . ? C20 C18 O2 Ce1 -154.0(4) . . . . ? C17 C18 O2 Ce1 -35.6(6) . . . . ? C19 C18 O2 Ce1 85.7(6) . . . . ? Si2 N5 Si1 C37 -159.0(3) . . . . ? Ce1 N5 Si1 C37 21.7(3) . . . . ? Si2 N5 Si1 C39 83.6(4) . . . . ? Ce1 N5 Si1 C39 -95.6(3) . . . . ? Si2 N5 Si1 C38 -38.6(4) . . . . ? Ce1 N5 Si1 C38 142.2(3) . . . . ? Si1 N5 Si2 C42 83.3(4) . . . . ? Ce1 N5 Si2 C42 -97.4(3) . . . . ? Si1 N5 Si2 C40 -158.7(3) . . . . ? Ce1 N5 Si2 C40 20.5(3) . . . . ? Si1 N5 Si2 C41 -39.5(4) . . . . ? Ce1 N5 Si2 C41 139.8(3) . . . . ? Si1 N5 Si2 Ce1 -179.3(5) . . . . ? C8 O1 Ce1 O2 -92.4(5) . . . . ? C8 O1 Ce1 N5 89.1(5) . . . . ? C8 O1 Ce1 C1 4.4(5) . . . . ? C8 O1 Ce1 C11 -165.9(5) . . . . ? C8 O1 Ce1 Si2 87.8(5) . . . . ? C18 O2 Ce1 O1 -95.5(5) . . . . ? C18 O2 Ce1 N5 82.9(5) . . . . ? C18 O2 Ce1 C1 -169.4(5) . . . . ? C18 O2 Ce1 C11 0.3(5) . . . . ? C18 O2 Ce1 Si2 84.4(5) . . . . ? Si1 N5 Ce1 O1 0.7(3) . . . . ? Si2 N5 Ce1 O1 -178.63(17) . . . . ? Si1 N5 Ce1 O2 -177.36(18) . . . . ? Si2 N5 Ce1 O2 3.3(3) . . . . ? Si1 N5 Ce1 C1 72.7(2) . . . . ? Si2 N5 Ce1 C1 -106.7(2) . . . . ? Si1 N5 Ce1 C11 -106.1(2) . . . . ? Si2 N5 Ce1 C11 74.5(2) . . . . ? Si1 N5 Ce1 Si2 179.3(4) . . . . ? N1 C1 Ce1 O1 11.4(3) . . . . ? N2 C1 Ce1 O1 -161.9(4) . . . . ? N1 C1 Ce1 O2 113.7(3) . . . . ? N2 C1 Ce1 O2 -59.5(4) . . . . ? N1 C1 Ce1 N5 -112.8(3) . . . . ? N2 C1 Ce1 N5 73.9(4) . . . . ? N1 C1 Ce1 C11 61.7(8) . . . . ? N2 C1 Ce1 C11 -111.5(6) . . . . ? N1 C1 Ce1 Si2 -138.6(3) . . . . ? N2 C1 Ce1 Si2 48.2(4) . . . . ? N3 C11 Ce1 O1 118.5(3) . . . . ? N4 C11 Ce1 O1 -48.5(4) . . . . ? N3 C11 Ce1 O2 15.9(3) . . . . ? N4 C11 Ce1 O2 -151.1(4) . . . . ? N3 C11 Ce1 N5 -114.9(3) . . . . ? N4 C11 Ce1 N5 78.1(4) . . . . ? N3 C11 Ce1 C1 70.6(7) . . . . ? N4 C11 Ce1 C1 -96.5(7) . . . . ? N3 C11 Ce1 Si2 -89.7(3) . . . . ? N4 C11 Ce1 Si2 103.3(3) . . . . ? N5 Si2 Ce1 O1 2.3(3) . . . . ? C42 Si2 Ce1 O1 101.8(3) . . . . ? C40 Si2 Ce1 O1 -157.5(2) . . . . ? C41 Si2 Ce1 O1 -62.9(4) . . . . ? N5 Si2 Ce1 O2 -177.4(2) . . . . ? C42 Si2 Ce1 O2 -77.9(2) . . . . ? C40 Si2 Ce1 O2 22.8(2) . . . . ? C41 Si2 Ce1 O2 117.4(3) . . . . ? C42 Si2 Ce1 N5 99.5(3) . . . . ? C40 Si2 Ce1 N5 -159.8(3) . . . . ? C41 Si2 Ce1 N5 -65.2(4) . . . . ? N5 Si2 Ce1 C1 77.6(2) . . . . ? C42 Si2 Ce1 C1 177.1(2) . . . . ? C40 Si2 Ce1 C1 -82.2(2) . . . . ? C41 Si2 Ce1 C1 12.3(3) . . . . ? N5 Si2 Ce1 C11 -106.7(2) . . . . ? C42 Si2 Ce1 C11 -7.2(2) . . . . ? C40 Si2 Ce1 C11 93.5(2) . . . . ? C41 Si2 Ce1 C11 -171.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.511 _refine_diff_density_min -1.834 _refine_diff_density_rms 0.132 ##===========end of cif========================= data_po8059_CeLd2N _database_code_depnum_ccdc_archive 'CCDC 763329' #TrackingRef '9067805880598084.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H79 Ce N5 O2 Si2' _chemical_formula_sum 'C47 H79 Ce N5 O2 Si2' _chemical_formula_weight 942.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 19.9366(6) _cell_length_b 12.7554(4) _cell_length_c 20.3716(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.147(2) _cell_angle_gamma 90.00 _cell_volume 5176.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14500 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 30.0 _exptl_crystal_description Shard _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6085 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details sadabs _exptl_special_details ; Single crystals were grown from a toluene solution at -30 deg C. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 66609 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 30.03 _reflns_number_total 14500 _reflns_number_gt 11504 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^ > 2\s(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^)+(0.0348P)^2^+2.6616P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14500 _refine_ls_number_parameters 547 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.233992(7) 0.102443(11) 0.308551(7) 0.01826(5) Uani 1 1 d . . . Si2 Si 0.22128(4) 0.09880(6) 0.48386(3) 0.02358(16) Uani 1 1 d . . . Si1 Si 0.20500(4) -0.11039(6) 0.41549(3) 0.02291(16) Uani 1 1 d . . . O1 O 0.18632(10) 0.02597(15) 0.22300(9) 0.0289(5) Uani 1 1 d . . . O2 O 0.30119(11) 0.23935(16) 0.31022(10) 0.0348(5) Uani 1 1 d . . . N1 N 0.11225(12) 0.21998(17) 0.19356(10) 0.0229(5) Uani 1 1 d . . . N3 N 0.37351(12) 0.12260(18) 0.20772(11) 0.0257(5) Uani 1 1 d . . . N5 N 0.21617(11) 0.02186(17) 0.41549(10) 0.0211(5) Uani 1 1 d . . . N2 N 0.07736(11) 0.29032(17) 0.28182(10) 0.0212(5) Uani 1 1 d . . . C21 C 0.06795(13) 0.3187(2) 0.34901(12) 0.0215(5) Uani 1 1 d . . . N4 N 0.39381(12) -0.03634(18) 0.23712(11) 0.0242(5) Uani 1 1 d . . . C31 C 0.39494(13) -0.1320(2) 0.27367(13) 0.0224(6) Uani 1 1 d . . . C11 C 0.35204(13) 0.0449(2) 0.24627(12) 0.0219(5) Uani 1 1 d . . . C6 C 0.05042(14) 0.2725(2) 0.17019(13) 0.0270(6) Uani 1 1 d . . . H6A H 0.0169 0.2212 0.1531 0.032 Uiso 1 1 calc R . . H6B H 0.0596 0.3241 0.1354 0.032 Uiso 1 1 calc R . . C8 C 0.15449(15) 0.0415(2) 0.16184(13) 0.0278(6) Uani 1 1 d . . . C7 C 0.15064(15) 0.1600(2) 0.14725(12) 0.0249(6) Uani 1 1 d . . . H7A H 0.1968 0.1884 0.1472 0.030 Uiso 1 1 calc R . . H7B H 0.1303 0.1700 0.1026 0.030 Uiso 1 1 calc R . . C26 C 0.09805(14) 0.4106(2) 0.37427(14) 0.0255(6) Uani 1 1 d . . . C32 C 0.42453(14) -0.1331(2) 0.33748(14) 0.0260(6) Uani 1 1 d . . . C17 C 0.34451(16) 0.2266(2) 0.20226(15) 0.0317(7) Uani 1 1 d . . . H17A H 0.2975 0.2205 0.1852 0.038 Uiso 1 1 calc R . . H17B H 0.3697 0.2676 0.1700 0.038 Uiso 1 1 calc R . . C1 C 0.12595(13) 0.2293(2) 0.25805(12) 0.0204(5) Uani 1 1 d . . . C222 C -0.08606(16) 0.1698(3) 0.35876(16) 0.0381(8) Uani 1 1 d . . . H22A H -0.1002 0.1811 0.4038 0.057 Uiso 1 1 calc R . . H22B H -0.1064 0.1052 0.3413 0.057 Uiso 1 1 calc R . . H22C H -0.1006 0.2292 0.3312 0.057 Uiso 1 1 calc R . . C360 C 0.33971(16) -0.2262(3) 0.17487(14) 0.0348(7) Uani 1 1 d . . . H360 H 0.3379 -0.1526 0.1580 0.042 Uiso 1 1 calc R . . C37 C 0.22013(19) 0.2395(2) 0.45854(16) 0.0418(8) Uani 1 1 d . . . H37A H 0.2586 0.2538 0.4314 0.063 Uiso 1 1 calc R . . H37B H 0.2228 0.2841 0.4977 0.063 Uiso 1 1 calc R . . H37C H 0.1784 0.2544 0.4333 0.063 Uiso 1 1 calc R . . C33 C 0.42378(16) -0.2262(2) 0.37262(15) 0.0338(7) Uani 1 1 d . . . H33 H 0.4423 -0.2281 0.4163 0.041 Uiso 1 1 calc R . . C22 C 0.02457(14) 0.2584(2) 0.38558(13) 0.0235(6) Uani 1 1 d . . . C110 C 0.4165(2) 0.2866(4) 0.2990(2) 0.0676(13) Uani 1 1 d . . . H11A H 0.4179 0.3320 0.3378 0.101 Uiso 1 1 calc R . . H11B H 0.4481 0.3128 0.2671 0.101 Uiso 1 1 calc R . . H11C H 0.4290 0.2151 0.3120 0.101 Uiso 1 1 calc R . . C23 C 0.01268(15) 0.2900(2) 0.44992(13) 0.0285(6) Uani 1 1 d . . . H23 H -0.0157 0.2490 0.4762 0.034 Uiso 1 1 calc R . . C19 C 0.3217(3) 0.3977(3) 0.2521(3) 0.0835(19) Uani 1 1 d . . . H19A H 0.2768 0.3953 0.2309 0.125 Uiso 1 1 calc R . . H19B H 0.3529 0.4310 0.2225 0.125 Uiso 1 1 calc R . . H19C H 0.3201 0.4383 0.2929 0.125 Uiso 1 1 calc R . . C36 C 0.36879(14) -0.2235(2) 0.24469(14) 0.0268(6) Uani 1 1 d . . . C18 C 0.34532(18) 0.2865(2) 0.26775(17) 0.0408(8) Uani 1 1 d . . . C261 C 0.20804(17) 0.5086(3) 0.37239(19) 0.0467(9) Uani 1 1 d . . . H26A H 0.1971 0.5497 0.4112 0.070 Uiso 1 1 calc R . . H26B H 0.2366 0.5503 0.3442 0.070 Uiso 1 1 calc R . . H26C H 0.2319 0.4447 0.3862 0.070 Uiso 1 1 calc R . . C24 C 0.04173(15) 0.3799(2) 0.47541(14) 0.0296(7) Uani 1 1 d . . . H24 H 0.0329 0.4008 0.5190 0.036 Uiso 1 1 calc R . . C5 C 0.02680(15) 0.3260(3) 0.23132(13) 0.0319(7) Uani 1 1 d . . . H5A H 0.0273 0.4033 0.2266 0.038 Uiso 1 1 calc R . . H5B H -0.0190 0.3030 0.2420 0.038 Uiso 1 1 calc R . . C34 C 0.39652(16) -0.3162(3) 0.34515(16) 0.0371(7) Uani 1 1 d . . . H34 H 0.3958 -0.3791 0.3701 0.045 Uiso 1 1 calc R . . C25 C 0.08314(15) 0.4390(2) 0.43851(14) 0.0307(7) Uani 1 1 d . . . H25 H 0.1023 0.5011 0.4569 0.037 Uiso 1 1 calc R . . C35 C 0.37030(16) -0.3153(2) 0.28166(16) 0.0353(7) Uani 1 1 d . . . H35 H 0.3530 -0.3783 0.2628 0.042 Uiso 1 1 calc R . . C361 C 0.26853(17) -0.2706(3) 0.17126(17) 0.0472(9) Uani 1 1 d . . . H36A H 0.2696 -0.3445 0.1843 0.071 Uiso 1 1 calc R . . H36B H 0.2500 -0.2645 0.1262 0.071 Uiso 1 1 calc R . . H36C H 0.2404 -0.2312 0.2010 0.071 Uiso 1 1 calc R . . C321 C 0.41472(18) 0.0111(3) 0.41982(19) 0.0562(11) Uani 1 1 d . . . H32A H 0.4113 -0.0386 0.4562 0.084 Uiso 1 1 calc R . . H32B H 0.3698 0.0260 0.4010 0.084 Uiso 1 1 calc R . . H32C H 0.4354 0.0763 0.4360 0.084 Uiso 1 1 calc R . . C41 C 0.22023(17) -0.1634(2) 0.33210(14) 0.0325(7) Uani 1 1 d . . . H41A H 0.1864 -0.1355 0.3006 0.049 Uiso 1 1 calc R . . H41B H 0.2172 -0.2401 0.3330 0.049 Uiso 1 1 calc R . . H41C H 0.2651 -0.1425 0.3189 0.049 Uiso 1 1 calc R . . C320 C 0.45763(15) -0.0361(2) 0.36740(14) 0.0307(7) Uani 1 1 d . . . H320 H 0.4617 0.0171 0.3317 0.037 Uiso 1 1 calc R . . C9 C 0.1954(2) -0.0084(3) 0.10812(15) 0.0508(10) Uani 1 1 d . . . H9A H 0.2405 0.0222 0.1091 0.076 Uiso 1 1 calc R . . H9B H 0.1733 0.0047 0.0652 0.076 Uiso 1 1 calc R . . H9C H 0.1987 -0.0842 0.1156 0.076 Uiso 1 1 calc R . . C221 C 0.01468(18) 0.0632(3) 0.39689(17) 0.0418(8) Uani 1 1 d . . . H22D H 0.0636 0.0576 0.3948 0.063 Uiso 1 1 calc R . . H22E H -0.0063 0.0005 0.3774 0.063 Uiso 1 1 calc R . . H22F H 0.0024 0.0694 0.4429 0.063 Uiso 1 1 calc R . . C16 C 0.43001(18) 0.0943(3) 0.16756(18) 0.0440(9) Uani 1 1 d . . . H16A H 0.4674 0.1449 0.1736 0.053 Uiso 1 1 calc R . . H16B H 0.4162 0.0910 0.1204 0.053 Uiso 1 1 calc R . . C323 C 0.52767(17) -0.0590(3) 0.39552(19) 0.0484(9) Uani 1 1 d . . . H32D H 0.5250 -0.1108 0.4309 0.073 Uiso 1 1 calc R . . H32E H 0.5478 0.0058 0.4130 0.073 Uiso 1 1 calc R . . H32F H 0.5554 -0.0867 0.3608 0.073 Uiso 1 1 calc R . . C10 C 0.08442(18) -0.0058(3) 0.16233(17) 0.0451(9) Uani 1 1 d . . . H10A H 0.0878 -0.0814 0.1706 0.068 Uiso 1 1 calc R . . H10B H 0.0613 0.0061 0.1197 0.068 Uiso 1 1 calc R . . H10C H 0.0590 0.0272 0.1970 0.068 Uiso 1 1 calc R . . C15 C 0.44957(16) -0.0125(2) 0.19368(15) 0.0346(7) Uani 1 1 d . . . H15A H 0.4521 -0.0646 0.1578 0.041 Uiso 1 1 calc R . . H15B H 0.4932 -0.0103 0.2186 0.041 Uiso 1 1 calc R . . C362 C 0.38544(19) -0.2900(3) 0.13076(17) 0.0544(10) Uani 1 1 d . . . H36D H 0.4308 -0.2602 0.1330 0.082 Uiso 1 1 calc R . . H36E H 0.3676 -0.2875 0.0853 0.082 Uiso 1 1 calc R . . H36F H 0.3871 -0.3629 0.1458 0.082 Uiso 1 1 calc R . . C220 C -0.00964(15) 0.1605(2) 0.35877(14) 0.0285(6) Uani 1 1 d . . . H220 H 0.0034 0.1518 0.3122 0.034 Uiso 1 1 calc R . . C39 C 0.29859(19) 0.0825(3) 0.53776(16) 0.0510(10) Uani 1 1 d . . . H39A H 0.3018 0.0098 0.5530 0.077 Uiso 1 1 calc R . . H39B H 0.2963 0.1294 0.5757 0.077 Uiso 1 1 calc R . . H39C H 0.3382 0.0999 0.5128 0.077 Uiso 1 1 calc R . . C42 C 0.26290(19) -0.1822(3) 0.47424(17) 0.0477(9) Uani 1 1 d . . . H42A H 0.3095 -0.1658 0.4645 0.072 Uiso 1 1 calc R . . H42B H 0.2554 -0.2578 0.4697 0.072 Uiso 1 1 calc R . . H42C H 0.2541 -0.1606 0.5193 0.072 Uiso 1 1 calc R . . C38 C 0.1507(2) 0.0811(3) 0.54067(17) 0.0487(10) Uani 1 1 d . . . H38A H 0.1085 0.1024 0.5184 0.073 Uiso 1 1 calc R . . H38B H 0.1588 0.1244 0.5799 0.073 Uiso 1 1 calc R . . H38C H 0.1479 0.0072 0.5535 0.073 Uiso 1 1 calc R . . C262 C 0.1063(2) 0.5801(3) 0.3126(2) 0.0547(11) Uani 1 1 d . . . H26D H 0.0949 0.6207 0.3515 0.082 Uiso 1 1 calc R . . H26E H 0.0650 0.5614 0.2876 0.082 Uiso 1 1 calc R . . H26F H 0.1351 0.6221 0.2850 0.082 Uiso 1 1 calc R . . C40 C 0.11841(17) -0.1553(3) 0.43553(17) 0.0406(8) Uani 1 1 d . . . H40A H 0.1042 -0.1194 0.4752 0.061 Uiso 1 1 calc R . . H40B H 0.1188 -0.2312 0.4431 0.061 Uiso 1 1 calc R . . H40C H 0.0871 -0.1388 0.3988 0.061 Uiso 1 1 calc R . . C260 C 0.14358(17) 0.4793(2) 0.33433(16) 0.0369(7) Uani 1 1 d . . . H260 H 0.1557 0.4397 0.2941 0.044 Uiso 1 1 calc R . . C2S C 0.4886(4) 0.9721(10) 0.0015(6) 0.126(4) Uani 0.50 1 d PGU A -1 H2SA H 0.4409 0.9701 -0.0011 0.151 Uiso 0.50 1 calc PR A -1 C3S C 0.5223(6) 1.0636(8) -0.0142(6) 0.122(4) Uani 0.50 1 d PGU A -1 H3S H 0.4976 1.1242 -0.0276 0.147 Uiso 0.50 1 calc PR A -1 C4S C 0.5920(6) 1.0665(7) -0.0103(4) 0.129(3) Uani 0.50 1 d PGU A -1 H4S H 0.6150 1.1291 -0.0211 0.154 Uiso 0.50 1 calc PR A -1 C5S C 0.6280(4) 0.9779(9) 0.0092(4) 0.130(3) Uani 0.50 1 d PGU A -1 H5S H 0.6757 0.9799 0.0119 0.157 Uiso 0.50 1 calc PR A -1 C6S C 0.5944(6) 0.8864(7) 0.0250(3) 0.125(3) Uani 0.50 1 d PGU A -1 H6S H 0.6190 0.8258 0.0383 0.150 Uiso 0.50 1 calc PR A -1 C1S C 0.5246(6) 0.8835(7) 0.0211(4) 0.120(3) Uani 0.50 1 d PGU A -1 H7S H 0.5016 0.8209 0.0318 0.144 Uiso 0.50 1 calc PR A -1 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 0.01718(8) 0.01875(8) 0.01895(7) 0.00155(6) 0.00181(5) -0.00008(6) Si2 0.0238(4) 0.0255(4) 0.0215(3) -0.0020(3) 0.0014(3) 0.0011(3) Si1 0.0261(4) 0.0210(4) 0.0219(3) 0.0028(3) 0.0041(3) 0.0005(3) O1 0.0351(12) 0.0273(11) 0.0239(9) -0.0012(8) -0.0058(8) 0.0078(9) O2 0.0381(13) 0.0241(11) 0.0435(12) -0.0048(9) 0.0183(10) -0.0073(9) N1 0.0273(13) 0.0211(12) 0.0203(10) -0.0005(9) -0.0008(9) 0.0056(10) N3 0.0221(12) 0.0249(13) 0.0306(12) 0.0038(9) 0.0068(10) 0.0017(10) N5 0.0216(12) 0.0216(12) 0.0203(10) 0.0016(9) 0.0018(9) -0.0010(9) N2 0.0205(12) 0.0228(12) 0.0203(10) -0.0004(9) 0.0000(9) 0.0036(9) C21 0.0181(13) 0.0242(14) 0.0221(12) -0.0024(10) -0.0005(10) 0.0061(11) N4 0.0232(12) 0.0240(12) 0.0259(11) 0.0014(9) 0.0058(9) 0.0036(10) C31 0.0173(13) 0.0226(14) 0.0277(13) 0.0016(10) 0.0063(11) 0.0060(11) C11 0.0211(14) 0.0216(14) 0.0230(12) 0.0002(10) 0.0002(10) 0.0003(11) C6 0.0245(15) 0.0343(16) 0.0222(12) 0.0049(11) 0.0008(11) 0.0062(12) C8 0.0381(18) 0.0242(15) 0.0206(12) -0.0035(11) -0.0050(11) 0.0037(13) C7 0.0294(16) 0.0270(15) 0.0182(12) -0.0010(10) 0.0013(11) -0.0004(12) C26 0.0225(14) 0.0212(14) 0.0328(14) -0.0037(11) 0.0008(11) 0.0001(11) C32 0.0205(14) 0.0277(15) 0.0297(14) -0.0011(11) 0.0005(11) 0.0022(12) C17 0.0300(17) 0.0218(15) 0.0441(17) 0.0074(12) 0.0111(13) 0.0007(12) C1 0.0211(14) 0.0176(13) 0.0228(12) -0.0011(10) 0.0023(10) -0.0015(10) C222 0.0308(18) 0.041(2) 0.0418(17) 0.0025(15) -0.0040(14) -0.0073(15) C360 0.0371(19) 0.0361(18) 0.0310(15) -0.0080(13) -0.0022(13) 0.0013(14) C37 0.063(3) 0.0270(17) 0.0352(16) -0.0023(13) 0.0020(16) -0.0030(16) C33 0.0317(17) 0.0377(18) 0.0315(15) 0.0047(13) -0.0045(13) 0.0049(14) C22 0.0211(14) 0.0247(14) 0.0246(13) -0.0018(11) -0.0007(11) 0.0008(11) C110 0.055(3) 0.078(3) 0.070(3) -0.029(2) 0.017(2) -0.044(2) C23 0.0266(16) 0.0345(17) 0.0246(13) 0.0001(12) 0.0050(11) 0.0019(13) C19 0.127(5) 0.0208(19) 0.108(4) 0.003(2) 0.079(4) 0.001(2) C36 0.0209(14) 0.0271(15) 0.0326(14) -0.0045(12) 0.0028(11) 0.0035(12) C18 0.046(2) 0.0241(16) 0.054(2) -0.0046(14) 0.0251(17) -0.0125(15) C261 0.0331(19) 0.0324(19) 0.075(3) 0.0059(17) 0.0017(17) -0.0051(15) C24 0.0320(17) 0.0331(17) 0.0237(13) -0.0074(11) 0.0004(12) 0.0068(13) C5 0.0295(16) 0.0379(18) 0.0279(14) -0.0004(12) -0.0040(12) 0.0117(14) C34 0.0353(18) 0.0267(16) 0.0492(18) 0.0102(14) 0.0009(14) 0.0040(14) C25 0.0302(17) 0.0267(15) 0.0349(15) -0.0116(12) -0.0048(13) 0.0036(13) C35 0.0310(17) 0.0259(16) 0.0491(18) -0.0032(14) 0.0028(14) 0.0004(13) C361 0.036(2) 0.065(3) 0.0399(17) -0.0145(17) -0.0048(15) 0.0004(18) C321 0.037(2) 0.064(3) 0.068(2) -0.035(2) 0.0001(18) -0.0023(19) C41 0.0422(19) 0.0250(16) 0.0311(14) -0.0035(12) 0.0110(13) -0.0041(14) C320 0.0289(16) 0.0324(17) 0.0304(14) -0.0024(12) -0.0032(12) -0.0001(13) C9 0.075(3) 0.045(2) 0.0317(16) -0.0100(15) -0.0018(17) 0.027(2) C221 0.043(2) 0.0280(17) 0.054(2) -0.0002(15) -0.0037(16) -0.0063(15) C16 0.043(2) 0.041(2) 0.050(2) 0.0146(16) 0.0265(16) 0.0148(16) C323 0.0271(18) 0.053(2) 0.065(2) -0.0049(19) -0.0076(17) -0.0040(16) C10 0.052(2) 0.0323(18) 0.0491(19) 0.0056(15) -0.0210(17) -0.0123(16) C15 0.0303(17) 0.0354(18) 0.0391(16) 0.0041(13) 0.0157(13) 0.0080(14) C362 0.042(2) 0.077(3) 0.0440(19) -0.026(2) 0.0038(16) 0.002(2) C220 0.0274(16) 0.0305(16) 0.0278(14) -0.0032(12) 0.0018(12) -0.0058(13) C39 0.050(2) 0.067(3) 0.0352(17) -0.0207(17) -0.0149(16) 0.0211(19) C42 0.059(2) 0.0347(19) 0.048(2) 0.0102(16) -0.0124(17) 0.0050(17) C38 0.056(2) 0.050(2) 0.0412(18) -0.0186(16) 0.0233(17) -0.0106(18) C262 0.051(2) 0.046(2) 0.066(2) 0.0177(19) -0.0131(19) -0.0145(18) C40 0.040(2) 0.0288(17) 0.054(2) -0.0042(15) 0.0185(16) -0.0097(15) C260 0.0407(19) 0.0282(17) 0.0424(17) -0.0079(13) 0.0091(14) -0.0119(14) C2S 0.186(8) 0.150(9) 0.043(5) -0.012(7) 0.022(5) 0.027(7) C3S 0.203(8) 0.131(8) 0.032(5) -0.006(6) -0.006(6) 0.035(7) C4S 0.208(9) 0.132(7) 0.045(5) -0.017(5) -0.009(6) -0.009(7) C5S 0.183(8) 0.152(8) 0.055(5) -0.016(6) -0.014(6) -0.001(6) C6S 0.185(8) 0.147(8) 0.043(4) -0.004(5) 0.007(6) 0.017(7) C1S 0.181(8) 0.143(8) 0.037(4) -0.007(5) 0.022(6) 0.017(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.1836(18) . ? Ce1 O2 2.201(2) . ? Ce1 N5 2.447(2) . ? Ce1 C11 2.813(3) . ? Ce1 C1 2.855(3) . ? Si2 N5 1.704(2) . ? Si2 C37 1.867(3) . ? Si2 C38 1.869(3) . ? Si2 C39 1.870(3) . ? Si1 N5 1.701(2) . ? Si1 C41 1.864(3) . ? Si1 C42 1.871(3) . ? Si1 C40 1.878(3) . ? O1 C8 1.391(3) . ? O2 C18 1.393(4) . ? N1 C1 1.337(3) . ? N1 C7 1.454(3) . ? N1 C6 1.466(3) . ? N3 C11 1.345(3) . ? N3 C17 1.450(4) . ? N3 C16 1.462(4) . ? N2 C1 1.347(3) . ? N2 C21 1.435(3) . ? N2 C5 1.485(3) . ? C21 C22 1.394(4) . ? C21 C26 1.405(4) . ? N4 C11 1.346(3) . ? N4 C31 1.429(3) . ? N4 C15 1.478(4) . ? C31 C36 1.400(4) . ? C31 C32 1.407(4) . ? C6 C5 1.511(4) . ? C8 C10 1.522(4) . ? C8 C9 1.528(4) . ? C8 C7 1.542(4) . ? C26 C25 1.401(4) . ? C26 C260 1.520(4) . ? C32 C33 1.387(4) . ? C32 C320 1.520(4) . ? C17 C18 1.537(4) . ? C222 C220 1.528(4) . ? C360 C36 1.516(4) . ? C360 C361 1.527(4) . ? C360 C362 1.537(5) . ? C33 C34 1.380(4) . ? C22 C23 1.400(4) . ? C22 C220 1.515(4) . ? C110 C18 1.533(5) . ? C23 C24 1.377(4) . ? C19 C18 1.525(5) . ? C36 C35 1.391(4) . ? C261 C260 1.522(5) . ? C24 C25 1.365(4) . ? C34 C35 1.377(4) . ? C321 C320 1.517(4) . ? C320 C323 1.518(4) . ? C221 C220 1.533(4) . ? C16 C15 1.509(4) . ? C262 C260 1.541(5) . ? C2S C3S 1.3900 . ? C2S C1S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C6S C1S 1.3900 . ? 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 O2 127.84(8) . . ? O1 Ce1 N5 116.72(7) . . ? O2 Ce1 N5 115.36(8) . . ? O1 Ce1 C11 82.52(7) . . ? O2 Ce1 C11 72.24(8) . . ? N5 Ce1 C11 116.35(7) . . ? O1 Ce1 C1 70.47(7) . . ? O2 Ce1 C1 90.37(8) . . ? N5 Ce1 C1 115.23(7) . . ? C11 Ce1 C1 128.18(7) . . ? N5 Si2 C37 109.16(12) . . ? N5 Si2 C38 114.41(14) . . ? C37 Si2 C38 106.60(17) . . ? N5 Si2 C39 116.02(14) . . ? C37 Si2 C39 105.67(18) . . ? C38 Si2 C39 104.23(18) . . ? N5 Si1 C41 109.51(12) . . ? N5 Si1 C42 114.06(14) . . ? C41 Si1 C42 106.72(16) . . ? N5 Si1 C40 115.08(13) . . ? C41 Si1 C40 105.66(15) . . ? C42 Si1 C40 105.16(17) . . ? C8 O1 Ce1 145.24(17) . . ? C18 O2 Ce1 136.98(19) . . ? C1 N1 C7 126.3(2) . . ? C1 N1 C6 114.6(2) . . ? C7 N1 C6 119.1(2) . . ? C11 N3 C17 125.8(2) . . ? C11 N3 C16 114.4(2) . . ? C17 N3 C16 119.7(2) . . ? Si1 N5 Si2 125.10(13) . . ? Si1 N5 Ce1 116.09(10) . . ? Si2 N5 Ce1 118.66(11) . . ? C1 N2 C21 127.6(2) . . ? C1 N2 C5 114.0(2) . . ? C21 N2 C5 118.3(2) . . ? C22 C21 C26 122.0(2) . . ? C22 C21 N2 118.4(2) . . ? C26 C21 N2 119.4(2) . . ? C11 N4 C31 125.6(2) . . ? C11 N4 C15 114.1(2) . . ? C31 N4 C15 119.3(2) . . ? C36 C31 C32 121.1(3) . . ? C36 C31 N4 119.6(2) . . ? C32 C31 N4 119.2(2) . . ? N3 C11 N4 105.9(2) . . ? N3 C11 Ce1 111.16(17) . . ? N4 C11 Ce1 142.71(19) . . ? N1 C6 C5 102.9(2) . . ? O1 C8 C10 109.0(2) . . ? O1 C8 C9 110.1(2) . . ? C10 C8 C9 110.7(3) . . ? O1 C8 C7 109.3(2) . . ? C10 C8 C7 110.6(2) . . ? C9 C8 C7 107.1(2) . . ? N1 C7 C8 114.5(2) . . ? C25 C26 C21 117.1(3) . . ? C25 C26 C260 120.2(3) . . ? C21 C26 C260 122.7(3) . . ? C33 C32 C31 118.3(3) . . ? C33 C32 C320 120.2(2) . . ? C31 C32 C320 121.5(3) . . ? N3 C17 C18 113.4(3) . . ? N1 C1 N2 106.4(2) . . ? N1 C1 Ce1 115.28(17) . . ? N2 C1 Ce1 137.82(17) . . ? C36 C360 C361 112.0(3) . . ? C36 C360 C362 110.2(3) . . ? C361 C360 C362 110.2(3) . . ? C34 C33 C32 121.0(3) . . ? C21 C22 C23 118.1(3) . . ? C21 C22 C220 122.8(2) . . ? C23 C22 C220 119.0(3) . . ? C24 C23 C22 120.6(3) . . ? C35 C36 C31 118.2(3) . . ? C35 C36 C360 119.3(3) . . ? C31 C36 C360 122.5(3) . . ? O2 C18 C19 109.5(3) . . ? O2 C18 C110 109.8(3) . . ? C19 C18 C110 111.1(4) . . ? O2 C18 C17 109.8(2) . . ? C19 C18 C17 106.7(3) . . ? C110 C18 C17 109.9(3) . . ? C25 C24 C23 120.5(3) . . ? N2 C5 C6 102.0(2) . . ? C35 C34 C33 120.2(3) . . ? C24 C25 C26 121.7(3) . . ? C34 C35 C36 121.0(3) . . ? C321 C320 C323 110.2(3) . . ? C321 C320 C32 110.9(3) . . ? C323 C320 C32 112.0(3) . . ? N3 C16 C15 102.7(2) . . ? N4 C15 C16 101.9(2) . . ? C22 C220 C222 111.8(2) . . ? C22 C220 C221 110.8(2) . . ? C222 C220 C221 111.1(3) . . ? C26 C260 C261 112.3(3) . . ? C26 C260 C262 110.1(3) . . ? C261 C260 C262 109.3(3) . . ? C3S C2S C1S 120.0 . . ? C2S C3S C4S 120.0 . . ? C5S C4S C3S 120.0 . . ? C6S C5S C4S 120.0 . . ? C5S C6S C1S 120.0 . . ? C6S C1S C2S 120.0 . . ? 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 O2 Ce1 O1 C8 -39.8(4) . . . . ? N5 Ce1 O1 C8 143.9(3) . . . . ? C11 Ce1 O1 C8 -100.3(3) . . . . ? C1 Ce1 O1 C8 34.8(3) . . . . ? O1 Ce1 O2 C18 -25.8(3) . . . . ? N5 Ce1 O2 C18 150.6(3) . . . . ? C11 Ce1 O2 C18 39.3(3) . . . . ? C1 Ce1 O2 C18 -91.0(3) . . . . ? C41 Si1 N5 Si2 -168.33(16) . . . . ? C42 Si1 N5 Si2 -48.8(2) . . . . ? C40 Si1 N5 Si2 72.9(2) . . . . ? C41 Si1 N5 Ce1 7.13(17) . . . . ? C42 Si1 N5 Ce1 126.63(16) . . . . ? C40 Si1 N5 Ce1 -111.69(15) . . . . ? C37 Si2 N5 Si1 -171.28(18) . . . . ? C38 Si2 N5 Si1 -51.9(2) . . . . ? C39 Si2 N5 Si1 69.5(2) . . . . ? C37 Si2 N5 Ce1 13.37(18) . . . . ? C38 Si2 N5 Ce1 132.70(17) . . . . ? C39 Si2 N5 Ce1 -105.82(18) . . . . ? O1 Ce1 N5 Si1 30.14(15) . . . . ? O2 Ce1 N5 Si1 -146.67(11) . . . . ? C11 Ce1 N5 Si1 -64.83(14) . . . . ? C1 Ce1 N5 Si1 109.97(12) . . . . ? O1 Ce1 N5 Si2 -154.09(11) . . . . ? O2 Ce1 N5 Si2 29.10(15) . . . . ? C11 Ce1 N5 Si2 110.93(13) . . . . ? C1 Ce1 N5 Si2 -74.27(14) . . . . ? C1 N2 C21 C22 -94.3(3) . . . . ? C5 N2 C21 C22 82.2(3) . . . . ? C1 N2 C21 C26 90.9(3) . . . . ? C5 N2 C21 C26 -92.6(3) . . . . ? C11 N4 C31 C36 105.6(3) . . . . ? C15 N4 C31 C36 -86.5(3) . . . . ? C11 N4 C31 C32 -76.6(4) . . . . ? C15 N4 C31 C32 91.3(3) . . . . ? C17 N3 C11 N4 -178.8(3) . . . . ? C16 N3 C11 N4 3.0(3) . . . . ? C17 N3 C11 Ce1 5.2(3) . . . . ? C16 N3 C11 Ce1 -173.0(2) . . . . ? C31 N4 C11 N3 172.4(2) . . . . ? C15 N4 C11 N3 3.9(3) . . . . ? C31 N4 C11 Ce1 -13.7(5) . . . . ? C15 N4 C11 Ce1 177.8(2) . . . . ? O1 Ce1 C11 N3 93.03(18) . . . . ? O2 Ce1 C11 N3 -40.73(18) . . . . ? N5 Ce1 C11 N3 -150.80(17) . . . . ? C1 Ce1 C11 N3 35.2(2) . . . . ? O1 Ce1 C11 N4 -80.6(3) . . . . ? O2 Ce1 C11 N4 145.6(3) . . . . ? N5 Ce1 C11 N4 35.5(3) . . . . ? C1 Ce1 C11 N4 -138.5(3) . . . . ? C1 N1 C6 C5 3.6(3) . . . . ? C7 N1 C6 C5 -179.2(2) . . . . ? Ce1 O1 C8 C10 -120.9(3) . . . . ? Ce1 O1 C8 C9 117.5(3) . . . . ? Ce1 O1 C8 C7 0.0(4) . . . . ? C1 N1 C7 C8 61.2(4) . . . . ? C6 N1 C7 C8 -115.6(3) . . . . ? O1 C8 C7 N1 -61.5(3) . . . . ? C10 C8 C7 N1 58.4(3) . . . . ? C9 C8 C7 N1 179.2(2) . . . . ? C22 C21 C26 C25 0.6(4) . . . . ? N2 C21 C26 C25 175.2(2) . . . . ? C22 C21 C26 C260 -177.9(3) . . . . ? N2 C21 C26 C260 -3.2(4) . . . . ? C36 C31 C32 C33 -3.6(4) . . . . ? N4 C31 C32 C33 178.6(3) . . . . ? C36 C31 C32 C320 175.4(3) . . . . ? N4 C31 C32 C320 -2.4(4) . . . . ? C11 N3 C17 C18 59.4(4) . . . . ? C16 N3 C17 C18 -122.5(3) . . . . ? C7 N1 C1 N2 -179.2(2) . . . . ? C6 N1 C1 N2 -2.3(3) . . . . ? C7 N1 C1 Ce1 -6.1(3) . . . . ? C6 N1 C1 Ce1 170.85(18) . . . . ? C21 N2 C1 N1 176.5(2) . . . . ? C5 N2 C1 N1 -0.1(3) . . . . ? C21 N2 C1 Ce1 5.7(4) . . . . ? C5 N2 C1 Ce1 -170.9(2) . . . . ? O1 Ce1 C1 N1 -28.63(18) . . . . ? O2 Ce1 C1 N1 101.81(19) . . . . ? N5 Ce1 C1 N1 -139.74(18) . . . . ? C11 Ce1 C1 N1 34.3(2) . . . . ? O1 Ce1 C1 N2 141.5(3) . . . . ? O2 Ce1 C1 N2 -88.0(3) . . . . ? N5 Ce1 C1 N2 30.4(3) . . . . ? C11 Ce1 C1 N2 -155.5(2) . . . . ? C31 C32 C33 C34 1.9(5) . . . . ? C320 C32 C33 C34 -177.2(3) . . . . ? C26 C21 C22 C23 -1.8(4) . . . . ? N2 C21 C22 C23 -176.5(2) . . . . ? C26 C21 C22 C220 178.6(3) . . . . ? N2 C21 C22 C220 3.9(4) . . . . ? C21 C22 C23 C24 1.8(4) . . . . ? C220 C22 C23 C24 -178.5(3) . . . . ? C32 C31 C36 C35 2.6(4) . . . . ? N4 C31 C36 C35 -179.7(3) . . . . ? C32 C31 C36 C360 -176.9(3) . . . . ? N4 C31 C36 C360 0.9(4) . . . . ? C361 C360 C36 C35 54.6(4) . . . . ? C362 C360 C36 C35 -68.5(4) . . . . ? C361 C360 C36 C31 -125.9(3) . . . . ? C362 C360 C36 C31 110.9(3) . . . . ? Ce1 O2 C18 C19 118.6(3) . . . . ? Ce1 O2 C18 C110 -119.2(3) . . . . ? Ce1 O2 C18 C17 1.7(5) . . . . ? N3 C17 C18 O2 -68.4(4) . . . . ? N3 C17 C18 C19 173.0(3) . . . . ? N3 C17 C18 C110 52.5(4) . . . . ? C22 C23 C24 C25 -0.7(4) . . . . ? C1 N2 C5 C6 2.3(3) . . . . ? C21 N2 C5 C6 -174.7(2) . . . . ? N1 C6 C5 N2 -3.2(3) . . . . ? C32 C33 C34 C35 0.9(5) . . . . ? C23 C24 C25 C26 -0.6(5) . . . . ? C21 C26 C25 C24 0.6(4) . . . . ? C260 C26 C25 C24 179.1(3) . . . . ? C33 C34 C35 C36 -2.0(5) . . . . ? C31 C36 C35 C34 0.3(5) . . . . ? C360 C36 C35 C34 179.8(3) . . . . ? C33 C32 C320 C321 -74.1(4) . . . . ? C31 C32 C320 C321 106.9(3) . . . . ? C33 C32 C320 C323 49.5(4) . . . . ? C31 C32 C320 C323 -129.5(3) . . . . ? C11 N3 C16 C15 -8.2(4) . . . . ? C17 N3 C16 C15 173.5(3) . . . . ? C11 N4 C15 C16 -8.7(3) . . . . ? C31 N4 C15 C16 -178.0(3) . . . . ? N3 C16 C15 N4 9.2(3) . . . . ? C21 C22 C220 C222 -120.3(3) . . . . ? C23 C22 C220 C222 60.0(3) . . . . ? C21 C22 C220 C221 115.2(3) . . . . ? C23 C22 C220 C221 -64.5(3) . . . . ? C25 C26 C260 C261 49.0(4) . . . . ? C21 C26 C260 C261 -132.6(3) . . . . ? C25 C26 C260 C262 -73.0(4) . . . . ? C21 C26 C260 C262 105.4(3) . . . . ? C1S C2S C3S C4S 0.0 . . . . ? C2S C3S C4S C5S 0.0 . . . . ? C3S C4S C5S C6S 0.0 . . . . ? C4S C5S C6S C1S 0.0 . . . . ? C5S C6S C1S C2S 0.0 . . . . ? C3S C2S C1S C6S 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 29.84 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.379 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.097 ##===========end of cif========================= data_po8084_ULm2I2 _database_code_depnum_ccdc_archive 'CCDC 763330' #TrackingRef '9067805880598084.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H46 I2 N4 O2 U' _chemical_formula_sum 'C32 H46 I2 N4 O2 U' _chemical_formula_weight 1010.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 Monoclinic _symmetry_space_group_name_H-M P21/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 12.1805(4) _cell_length_b 12.0395(4) _cell_length_c 12.3962(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.881(2) _cell_angle_gamma 90.00 _cell_volume 1778.92(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9917 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 29.55 _exptl_crystal_description prism _exptl_crystal_colour 'dark pink' _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 6.330 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.040944 _exptl_absorpt_correction_T_max 0.069152 _exptl_absorpt_process_details SADABS _exptl_special_details ; Single crystals were grown by allowing a C6D6 solution of the reaction mixture to stand at room temperature for four weeks. ; _diffrn_ambient_temperature 150(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 'Brucker SMART APEX CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18933 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 29.57 _reflns_number_total 4693 _reflns_number_gt 4138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement 'SAINT (Siemans, 1995)' _computing_data_reduction 'SAINT (Siemans, 1995)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; CheckCif alert B possible missed higher symmetry. Platon checked and definitely no symmetry missed. The U is on a special position, and that gives rise to the pseudotranslation that Platon finds (platon addsym suggests the possibility of a pseudotranslation of 0.5 0.5 0.5, but not in addsym-exact),but although the orientation of the ligands are similar, they are distinct; changing the space group to higher symmetry would mean you'd need to model the ligands as disordered, but they aren't. 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^)+(0.0299P)^2^+3.0930P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4693 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2143(3) 0.0062(3) 1.0990(3) 0.0206(7) Uani 1 1 d . . . C5 C 0.4090(3) -0.0285(4) 1.1520(4) 0.0334(10) Uani 1 1 d . . . H5A H 0.4668 0.0241 1.1375 0.040 Uiso 1 1 calc R . . H5B H 0.4411 -0.1043 1.1607 0.040 Uiso 1 1 calc R . . C6 C 0.3641(4) 0.0061(4) 1.2528(4) 0.0368(11) Uani 1 1 d . . . H6A H 0.3777 -0.0522 1.3104 0.044 Uiso 1 1 calc R . . H6B H 0.3986 0.0765 1.2843 0.044 Uiso 1 1 calc R . . C7 C 0.1676(3) 0.0572(4) 1.2778(3) 0.0267(9) Uani 1 1 d . . . H7A H 0.1394 0.1322 1.2537 0.032 Uiso 1 1 calc R . . H7B H 0.2105 0.0634 1.3546 0.032 Uiso 1 1 calc R . . C8 C 0.0672(4) -0.0200(4) 1.2758(3) 0.0295(9) Uani 1 1 d . . . C9 C 0.1046(5) -0.1360(4) 1.3140(4) 0.0499(15) Uani 1 1 d . . . H9A H 0.0386 -0.1838 1.3095 0.075 Uiso 1 1 calc R . . H9B H 0.1464 -0.1331 1.3905 0.075 Uiso 1 1 calc R . . H9C H 0.1528 -0.1661 1.2669 0.075 Uiso 1 1 calc R . . C10 C -0.0082(5) 0.0325(6) 1.3456(4) 0.0490(14) Uani 1 1 d . . . H10A H -0.0329 0.1058 1.3158 0.074 Uiso 1 1 calc R . . H10B H 0.0336 0.0406 1.4217 0.074 Uiso 1 1 calc R . . H10C H -0.0738 -0.0150 1.3444 0.074 Uiso 1 1 calc R . . C21 C 0.3132(3) -0.0291(3) 0.9492(3) 0.0214(8) Uani 1 1 d . . . C22 C 0.3071(3) 0.0694(3) 0.8889(3) 0.0230(8) Uani 1 1 d . . . C23 C 0.3113(3) 0.0638(3) 0.7787(3) 0.0241(8) Uani 1 1 d . . . H23 H 0.3062 0.1305 0.7371 0.029 Uiso 1 1 calc R . . C24 C 0.3230(3) -0.0366(4) 0.7268(3) 0.0247(8) Uani 1 1 d . . . C25 C 0.3335(3) -0.1330(3) 0.7903(4) 0.0253(8) Uani 1 1 d . . . H25 H 0.3438 -0.2020 0.7566 0.030 Uiso 1 1 calc R . . C26 C 0.3295(3) -0.1311(3) 0.9014(4) 0.0241(8) Uani 1 1 d . . . C220 C 0.3008(4) 0.1802(4) 0.9441(4) 0.0323(10) Uani 1 1 d . . . H22A H 0.3223 0.2393 0.8982 0.048 Uiso 1 1 calc R . . H22B H 0.3520 0.1804 1.0163 0.048 Uiso 1 1 calc R . . H22C H 0.2239 0.1930 0.9538 0.048 Uiso 1 1 calc R . . C240 C 0.3248(4) -0.0392(4) 0.6053(4) 0.0331(10) Uani 1 1 d . . . H24A H 0.2480 -0.0465 0.5625 0.050 Uiso 1 1 calc R . . H24B H 0.3697 -0.1025 0.5899 0.050 Uiso 1 1 calc R . . H24C H 0.3579 0.0298 0.5847 0.050 Uiso 1 1 calc R . . C260 C 0.3444(4) -0.2369(4) 0.9679(4) 0.0332(10) Uani 1 1 d . . . H26A H 0.2879 -0.2405 1.0137 0.050 Uiso 1 1 calc R . . H26B H 0.4196 -0.2382 1.0152 0.050 Uiso 1 1 calc R . . H26C H 0.3356 -0.3009 0.9179 0.050 Uiso 1 1 calc R . . N1 N 0.2436(3) 0.0201(3) 1.2076(3) 0.0253(7) Uani 1 1 d . . . N2 N 0.3064(3) -0.0244(3) 1.0631(3) 0.0236(7) Uani 1 1 d . . . O1 O 0.0057(2) -0.0268(2) 1.1652(2) 0.0235(6) Uani 1 1 d . . . I1 I 0.01718(3) -0.25130(3) 0.96070(3) 0.03691(9) Uani 1 1 d . . . U1 U 0.0000 0.0000 1.0000 0.01766(6) Uani 1 2 d S . . 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 0.0178(16) 0.0183(18) 0.0246(17) 0.0020(14) 0.0018(14) -0.0022(14) C5 0.0168(18) 0.047(3) 0.033(2) -0.0002(19) -0.0032(16) 0.0020(18) C6 0.023(2) 0.053(3) 0.030(2) 0.000(2) -0.0048(17) 0.002(2) C7 0.0255(19) 0.034(2) 0.0203(18) -0.0039(16) 0.0048(15) -0.0049(17) C8 0.030(2) 0.039(3) 0.0183(18) 0.0041(16) 0.0034(16) -0.0086(18) C9 0.056(3) 0.044(3) 0.040(3) 0.020(2) -0.012(2) -0.016(3) C10 0.041(3) 0.081(4) 0.029(2) -0.011(3) 0.016(2) -0.024(3) C21 0.0118(15) 0.0230(19) 0.0290(19) -0.0018(15) 0.0030(14) -0.0008(13) C22 0.0166(17) 0.021(2) 0.030(2) -0.0023(15) 0.0014(15) 0.0020(14) C23 0.0207(17) 0.020(2) 0.031(2) -0.0008(16) 0.0049(15) 0.0015(15) C24 0.0193(18) 0.026(2) 0.029(2) -0.0043(16) 0.0067(15) -0.0022(15) C25 0.0210(18) 0.019(2) 0.036(2) -0.0079(16) 0.0073(16) -0.0024(15) C26 0.0172(17) 0.021(2) 0.033(2) -0.0018(16) 0.0039(15) 0.0011(14) C220 0.041(2) 0.021(2) 0.035(2) -0.0029(17) 0.0078(19) 0.0045(18) C240 0.037(2) 0.029(2) 0.034(2) -0.0053(18) 0.0114(19) -0.0058(19) C260 0.035(2) 0.021(2) 0.044(3) 0.0036(18) 0.0072(19) 0.0002(18) N1 0.0189(15) 0.0315(19) 0.0240(16) -0.0001(13) 0.0007(13) -0.0003(14) N2 0.0158(14) 0.0274(18) 0.0258(16) -0.0008(13) 0.0000(13) 0.0015(13) O1 0.0205(13) 0.0290(15) 0.0205(13) 0.0006(11) 0.0029(10) -0.0040(11) I1 0.03835(16) 0.02136(15) 0.05255(19) -0.00389(13) 0.01293(13) 0.00071(12) U1 0.01494(9) 0.02063(11) 0.01687(9) -0.00005(7) 0.00200(6) -0.00060(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 N1 1.331(5) . ? C1 N2 1.341(5) . ? C1 U1 2.647(4) . ? C5 N2 1.488(5) . ? C5 C6 1.522(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.468(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N1 1.465(5) . ? C7 C8 1.533(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O1 1.422(5) . ? C8 C9 1.514(7) . ? C8 C10 1.523(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C21 C26 1.395(5) . ? C21 C22 1.396(6) . ? C21 N2 1.433(5) . ? C22 C23 1.379(6) . ? C22 C220 1.508(6) . ? C23 C24 1.390(6) . ? C23 H23 0.9500 . ? C24 C25 1.393(6) . ? C24 C240 1.511(6) . ? C25 C26 1.388(6) . ? C25 H25 0.9500 . ? C26 C260 1.509(6) . ? C220 H22A 0.9800 . ? C220 H22B 0.9800 . ? C220 H22C 0.9800 . ? C240 H24A 0.9800 . ? C240 H24B 0.9800 . ? C240 H24C 0.9800 . ? C260 H26A 0.9800 . ? C260 H26B 0.9800 . ? C260 H26C 0.9800 . ? O1 U1 2.061(3) . ? I1 U1 3.0784(3) . ? U1 O1 2.061(3) 3_557 ? U1 C1 2.647(4) 3_557 ? U1 I1 3.0784(3) 3_557 ? 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 C1 N2 107.6(3) . . ? N1 C1 U1 120.4(3) . . ? N2 C1 U1 130.6(3) . . ? N2 C5 C6 102.1(3) . . ? N2 C5 H5A 111.3 . . ? C6 C5 H5A 111.3 . . ? N2 C5 H5B 111.3 . . ? C6 C5 H5B 111.3 . . ? H5A C5 H5B 109.2 . . ? N1 C6 C5 102.6(3) . . ? N1 C6 H6A 111.2 . . ? C5 C6 H6A 111.2 . . ? N1 C6 H6B 111.2 . . ? C5 C6 H6B 111.2 . . ? H6A C6 H6B 109.2 . . ? N1 C7 C8 113.9(4) . . ? N1 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O1 C8 C9 108.3(4) . . ? O1 C8 C10 108.2(4) . . ? C9 C8 C10 112.5(4) . . ? O1 C8 C7 108.1(3) . . ? C9 C8 C7 111.5(4) . . ? C10 C8 C7 108.2(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C26 C21 C22 121.2(4) . . ? C26 C21 N2 119.7(4) . . ? C22 C21 N2 119.1(4) . . ? C23 C22 C21 118.6(4) . . ? C23 C22 C220 120.6(4) . . ? C21 C22 C220 120.7(4) . . ? C22 C23 C24 122.0(4) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C23 C24 C25 118.0(4) . . ? C23 C24 C240 120.2(4) . . ? C25 C24 C240 121.8(4) . . ? C26 C25 C24 121.9(4) . . ? C26 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C25 C26 C21 118.2(4) . . ? C25 C26 C260 120.2(4) . . ? C21 C26 C260 121.5(4) . . ? C22 C220 H22A 109.5 . . ? C22 C220 H22B 109.5 . . ? H22A C220 H22B 109.5 . . ? C22 C220 H22C 109.5 . . ? H22A C220 H22C 109.5 . . ? H22B C220 H22C 109.5 . . ? C24 C240 H24A 109.5 . . ? C24 C240 H24B 109.5 . . ? H24A C240 H24B 109.5 . . ? C24 C240 H24C 109.5 . . ? H24A C240 H24C 109.5 . . ? H24B C240 H24C 109.5 . . ? C26 C260 H26A 109.5 . . ? C26 C260 H26B 109.5 . . ? H26A C260 H26B 109.5 . . ? C26 C260 H26C 109.5 . . ? H26A C260 H26C 109.5 . . ? H26B C260 H26C 109.5 . . ? C1 N1 C7 124.7(3) . . ? C1 N1 C6 114.3(4) . . ? C7 N1 C6 120.8(3) . . ? C1 N2 C21 124.1(3) . . ? C1 N2 C5 113.3(3) . . ? C21 N2 C5 121.2(3) . . ? C8 O1 U1 148.4(3) . . ? O1 U1 O1 180.000(1) 3_557 . ? O1 U1 C1 73.47(11) 3_557 3_557 ? O1 U1 C1 106.53(11) . 3_557 ? O1 U1 C1 106.53(11) 3_557 . ? O1 U1 C1 73.47(11) . . ? C1 U1 C1 180.0 3_557 . ? O1 U1 I1 89.20(8) 3_557 . ? O1 U1 I1 90.80(8) . . ? C1 U1 I1 89.53(8) 3_557 . ? C1 U1 I1 90.47(8) . . ? O1 U1 I1 90.80(8) 3_557 3_557 ? O1 U1 I1 89.20(8) . 3_557 ? C1 U1 I1 90.47(8) 3_557 3_557 ? C1 U1 I1 89.53(8) . 3_557 ? I1 U1 I1 180.0 . 3_557 ? 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 N2 C5 C6 N1 2.2(5) . . . . ? N1 C7 C8 O1 -59.3(5) . . . . ? N1 C7 C8 C9 59.6(5) . . . . ? N1 C7 C8 C10 -176.2(4) . . . . ? C26 C21 C22 C23 3.4(6) . . . . ? N2 C21 C22 C23 -178.6(3) . . . . ? C26 C21 C22 C220 -174.0(4) . . . . ? N2 C21 C22 C220 3.9(5) . . . . ? C21 C22 C23 C24 -0.9(6) . . . . ? C220 C22 C23 C24 176.6(4) . . . . ? C22 C23 C24 C25 -1.7(6) . . . . ? C22 C23 C24 C240 178.7(4) . . . . ? C23 C24 C25 C26 1.8(6) . . . . ? C240 C24 C25 C26 -178.6(4) . . . . ? C24 C25 C26 C21 0.6(6) . . . . ? C24 C25 C26 C260 -178.3(4) . . . . ? C22 C21 C26 C25 -3.3(6) . . . . ? N2 C21 C26 C25 178.8(3) . . . . ? C22 C21 C26 C260 175.6(4) . . . . ? N2 C21 C26 C260 -2.3(6) . . . . ? N2 C1 N1 C7 177.8(4) . . . . ? U1 C1 N1 C7 -14.3(5) . . . . ? N2 C1 N1 C6 3.9(5) . . . . ? U1 C1 N1 C6 171.8(3) . . . . ? C8 C7 N1 C1 60.5(5) . . . . ? C8 C7 N1 C6 -125.9(4) . . . . ? C5 C6 N1 C1 -3.8(5) . . . . ? C5 C6 N1 C7 -178.0(4) . . . . ? N1 C1 N2 C21 -169.1(4) . . . . ? U1 C1 N2 C21 24.7(6) . . . . ? N1 C1 N2 C5 -2.2(5) . . . . ? U1 C1 N2 C5 -168.4(3) . . . . ? C26 C21 N2 C1 -115.2(4) . . . . ? C22 C21 N2 C1 66.8(5) . . . . ? C26 C21 N2 C5 78.9(5) . . . . ? C22 C21 N2 C5 -99.0(5) . . . . ? C6 C5 N2 C1 -0.1(5) . . . . ? C6 C5 N2 C21 167.1(4) . . . . ? C9 C8 O1 U1 -105.8(5) . . . . ? C10 C8 O1 U1 132.1(5) . . . . ? C7 C8 O1 U1 15.2(7) . . . . ? C8 O1 U1 C1 -162.7(5) . . . 3_557 ? C8 O1 U1 C1 17.3(5) . . . . ? C8 O1 U1 I1 107.5(5) . . . . ? C8 O1 U1 I1 -72.5(5) . . . 3_557 ? N1 C1 U1 O1 162.7(3) . . . 3_557 ? N2 C1 U1 O1 -32.6(4) . . . 3_557 ? N1 C1 U1 O1 -17.3(3) . . . . ? N2 C1 U1 O1 147.4(4) . . . . ? N1 C1 U1 I1 -108.0(3) . . . . ? N2 C1 U1 I1 56.7(3) . . . . ? N1 C1 U1 I1 72.0(3) . . . 3_557 ? N2 C1 U1 I1 -123.3(3) . . . 3_557 ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.225 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.138 ##===========end of cif========================= #============================================================================== data_po9067_CeLmN2 _database_code_depnum_ccdc_archive 'CCDC 763331' #TrackingRef '9067805880598084.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H64 Ce N5 O Si4 C5 H5 N' _chemical_formula_sum 'C38 H69 Ce N6 O Si4' _chemical_formula_weight 878.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 16.1984(6) _cell_length_b 13.4476(5) _cell_length_c 22.0515(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.384(2) _cell_angle_gamma 90.00 _cell_volume 4752.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9754 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 26.4 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 1.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5346 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details SADABS _exptl_special_details ; Single crystals were grown from a pyridine solution at -30 \%C. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 30810 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.44 _reflns_number_total 9754 _reflns_number_gt 7308 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement 'SAINT (Siemans, 1995)' _computing_data_reduction 'SAINT (Siemans, 1995)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^ > 2\s(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^)+(0.0535P)^2^+7.3231P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9754 _refine_ls_number_parameters 427 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.769843(16) 0.291881(19) 0.342137(14) 0.02603(10) Uani 1 1 d . . . Si3 Si 0.97478(8) 0.27070(10) 0.41352(8) 0.0328(3) Uani 1 1 d . . . Si1 Si 0.80983(9) 0.55208(10) 0.33182(8) 0.0351(4) Uani 1 1 d . . . Si4 Si 0.85156(9) 0.23751(10) 0.50069(7) 0.0319(3) Uani 1 1 d . . . Si2 Si 0.76631(9) 0.44141(11) 0.21290(8) 0.0378(4) Uani 1 1 d . . . O1 O 0.6689(2) 0.3256(3) 0.39252(17) 0.0344(8) Uani 1 1 d . . . N1 N 0.5508(2) 0.2916(3) 0.2806(2) 0.0347(10) Uani 1 1 d . . . N4 N 0.8752(2) 0.2589(3) 0.4286(2) 0.0291(9) Uani 1 1 d . . . N3 N 0.7844(2) 0.4465(3) 0.2906(2) 0.0330(10) Uani 1 1 d . . . C26 C 0.6464(3) 0.0758(4) 0.1531(3) 0.0366(13) Uani 1 1 d . . . N2 N 0.5860(2) 0.1637(3) 0.2317(2) 0.0335(10) Uani 1 1 d . . . C22 C 0.6529(3) 0.0033(4) 0.2540(3) 0.0333(12) Uani 1 1 d . . . C23 C 0.6930(3) -0.0786(4) 0.2346(3) 0.0374(13) Uani 1 1 d . . . H3 H 0.7088 -0.1314 0.2625 0.045 Uiso 1 1 calc R . . C7 C 0.5541(3) 0.3778(4) 0.3209(3) 0.0332(12) Uani 1 1 d . . . H10A H 0.4973 0.4065 0.3179 0.040 Uiso 1 1 calc R . . H10B H 0.5906 0.4287 0.3061 0.040 Uiso 1 1 calc R . . C21 C 0.6309(3) 0.0806(3) 0.2128(3) 0.0300(12) Uani 1 1 d . . . N5 N 0.8282(3) 0.1055(3) 0.3094(2) 0.0374(11) Uani 1 1 d . . . C25 C 0.6881(3) -0.0074(4) 0.1352(3) 0.0421(14) Uani 1 1 d . . . H4 H 0.7013 -0.0108 0.0946 0.051 Uiso 1 1 calc R . . C27 C 0.8103(3) 0.5258(4) 0.4149(3) 0.0425(14) Uani 1 1 d . . . H01A H 0.7549 0.5031 0.4215 0.064 Uiso 1 1 calc R . . H01B H 0.8248 0.5866 0.4386 0.064 Uiso 1 1 calc R . . H01C H 0.8515 0.4740 0.4281 0.064 Uiso 1 1 calc R . . C8 C 0.5859(3) 0.3558(4) 0.3879(3) 0.0367(13) Uani 1 1 d . . . C24 C 0.7107(3) -0.0854(4) 0.1755(3) 0.0421(15) Uani 1 1 d . . . C36 C 0.9346(4) 0.1706(5) 0.5534(3) 0.0537(17) Uani 1 1 d . . . H02A H 0.9444 0.1051 0.5362 0.081 Uiso 1 1 calc R . . H02B H 0.9164 0.1622 0.5936 0.081 Uiso 1 1 calc R . . H02C H 0.9863 0.2094 0.5580 0.081 Uiso 1 1 calc R . . C39 C 0.8565(3) 0.0788(4) 0.2579(3) 0.0452(15) Uani 1 1 d . . . H022 H 0.8471 0.1225 0.2237 0.054 Uiso 1 1 calc R . . C43 C 0.8415(4) 0.0424(4) 0.3561(3) 0.0481(16) Uani 1 1 d . . . H023 H 0.8222 0.0596 0.3934 0.058 Uiso 1 1 calc R . . C261 C 0.6199(4) 0.1575(4) 0.1074(3) 0.0468(15) Uani 1 1 d . . . H02D H 0.6551 0.1559 0.0748 0.070 Uiso 1 1 calc R . . H02E H 0.6258 0.2221 0.1282 0.070 Uiso 1 1 calc R . . H02F H 0.5614 0.1475 0.0895 0.070 Uiso 1 1 calc R . . C6 C 0.4705(3) 0.2580(4) 0.2467(3) 0.0458(15) Uani 1 1 d . . . H02G H 0.4475 0.3075 0.2155 0.055 Uiso 1 1 calc R . . H02H H 0.4291 0.2458 0.2748 0.055 Uiso 1 1 calc R . . C31 C 0.6562(4) 0.4706(5) 0.1799(3) 0.0562(17) Uani 1 1 d . . . H02X H 0.6183 0.4265 0.1980 0.084 Uiso 1 1 calc R . . H02Y H 0.6487 0.4607 0.1354 0.084 Uiso 1 1 calc R . . H02Z H 0.6438 0.5399 0.1889 0.084 Uiso 1 1 calc R . . C221 C 0.6305(3) 0.0070(4) 0.3180(3) 0.0431(14) Uani 1 1 d . . . H02J H 0.5697 0.0092 0.3158 0.065 Uiso 1 1 calc R . . H02K H 0.6550 0.0665 0.3390 0.065 Uiso 1 1 calc R . . H02L H 0.6522 -0.0524 0.3406 0.065 Uiso 1 1 calc R . . C40 C 0.8986(4) -0.0086(4) 0.2515(4) 0.0543(19) Uani 1 1 d . . . H028 H 0.9179 -0.0243 0.2139 0.065 Uiso 1 1 calc R . . C1 C 0.6162(3) 0.2365(3) 0.2706(2) 0.0266(11) Uani 1 1 d . . . C32 C 0.8344(4) 0.5234(4) 0.1733(3) 0.0544(17) Uani 1 1 d . . . H03A H 0.8211 0.5932 0.1803 0.082 Uiso 1 1 calc R . . H03B H 0.8250 0.5095 0.1292 0.082 Uiso 1 1 calc R . . H03C H 0.8931 0.5107 0.1896 0.082 Uiso 1 1 calc R . . C30 C 0.7874(4) 0.3113(4) 0.1896(3) 0.0430(14) Uani 1 1 d . . . H03D H 0.8461 0.2949 0.2033 0.065 Uiso 1 1 calc R . . H03E H 0.7755 0.3056 0.1448 0.065 Uiso 1 1 calc R . . H03F H 0.7516 0.2652 0.2083 0.065 Uiso 1 1 calc R . . C5 C 0.4934(3) 0.1626(4) 0.2171(3) 0.0422(15) Uani 1 1 d . . . H03G H 0.4693 0.1039 0.2353 0.051 Uiso 1 1 calc R . . H03H H 0.4748 0.1632 0.1723 0.051 Uiso 1 1 calc R . . C35 C 0.9744(3) 0.2997(4) 0.3298(3) 0.0391(13) Uani 1 1 d . . . H03X H 0.9508 0.2434 0.3049 0.059 Uiso 1 1 calc R . . H03Y H 1.0317 0.3117 0.3222 0.059 Uiso 1 1 calc R . . H03Z H 0.9405 0.3592 0.3188 0.059 Uiso 1 1 calc R . . C38 C 0.7554(4) 0.1598(4) 0.4974(3) 0.0475(15) Uani 1 1 d . . . H03J H 0.7106 0.1890 0.4681 0.071 Uiso 1 1 calc R . . H03K H 0.7379 0.1573 0.5381 0.071 Uiso 1 1 calc R . . H03L H 0.7671 0.0923 0.4842 0.071 Uiso 1 1 calc R . . C241 C 0.7559(4) -0.1764(4) 0.1546(4) 0.060(2) Uani 1 1 d . . . H03M H 0.7978 -0.1994 0.1882 0.091 Uiso 1 1 calc R . . H03N H 0.7834 -0.1584 0.1193 0.091 Uiso 1 1 calc R . . H03O H 0.7154 -0.2296 0.1427 0.091 Uiso 1 1 calc R . . C29 C 0.7339(4) 0.6550(4) 0.3096(3) 0.0527(17) Uani 1 1 d . . . H03P H 0.7319 0.6698 0.2659 0.079 Uiso 1 1 calc R . . H03Q H 0.7515 0.7146 0.3337 0.079 Uiso 1 1 calc R . . H03R H 0.6783 0.6348 0.3176 0.079 Uiso 1 1 calc R . . C9 C 0.5782(4) 0.4502(5) 0.4247(3) 0.0524(17) Uani 1 1 d . . . H03S H 0.6041 0.4397 0.4672 0.079 Uiso 1 1 calc R . . H03T H 0.5191 0.4668 0.4237 0.079 Uiso 1 1 calc R . . H03U H 0.6065 0.5050 0.4068 0.079 Uiso 1 1 calc R . . C37 C 0.8318(4) 0.3546(4) 0.5416(3) 0.0476(15) Uani 1 1 d . . . H03V H 0.8809 0.3978 0.5442 0.071 Uiso 1 1 calc R . . H03 H 0.8207 0.3386 0.5830 0.071 Uiso 1 1 calc R . . H03W H 0.7834 0.3889 0.5191 0.071 Uiso 1 1 calc R . . C41 C 0.9122(4) -0.0723(5) 0.3002(4) 0.066(2) Uani 1 1 d . . . H040 H 0.9418 -0.1327 0.2973 0.079 Uiso 1 1 calc R . . C10 C 0.5332(4) 0.2719(5) 0.4112(3) 0.0523(17) Uani 1 1 d . . . H04A H 0.5387 0.2112 0.3876 0.078 Uiso 1 1 calc R . . H04B H 0.4745 0.2922 0.4062 0.078 Uiso 1 1 calc R . . H04C H 0.5530 0.2593 0.4547 0.078 Uiso 1 1 calc R . . C34 C 1.0337(3) 0.3754(5) 0.4567(3) 0.0537(17) Uani 1 1 d . . . H04D H 1.0054 0.4385 0.4452 0.081 Uiso 1 1 calc R . . H04E H 1.0906 0.3777 0.4466 0.081 Uiso 1 1 calc R . . H04F H 1.0359 0.3645 0.5009 0.081 Uiso 1 1 calc R . . C42 C 0.8826(4) -0.0481(5) 0.3527(4) 0.0583(19) Uani 1 1 d . . . H043 H 0.8898 -0.0922 0.3867 0.070 Uiso 1 1 calc R . . C33 C 1.0415(3) 0.1566(4) 0.4271(3) 0.0498(16) Uani 1 1 d . . . H04G H 1.0456 0.1368 0.4702 0.075 Uiso 1 1 calc R . . H04H H 1.0974 0.1709 0.4174 0.075 Uiso 1 1 calc R . . H04I H 1.0165 0.1025 0.4009 0.075 Uiso 1 1 calc R . . C28 C 0.9155(4) 0.6042(5) 0.3250(4) 0.0597(19) Uani 1 1 d . . . H12A H 0.9586 0.5562 0.3414 0.090 Uiso 1 1 calc R . . H12B H 0.9238 0.6663 0.3483 0.090 Uiso 1 1 calc R . . H12C H 0.9194 0.6173 0.2818 0.090 Uiso 1 1 calc R . . N1S N 0.5622(6) 0.8507(14) 0.4543(6) 0.247(7) Uiso 1 1 d GD . . C2S C 0.5897(10) 0.7577(12) 0.4382(5) 0.233(8) Uiso 1 1 d GD . . H2S H 0.5526 0.7142 0.4137 0.280 Uiso 1 1 calc R . . C3S C 0.6715(12) 0.7286(9) 0.4580(7) 0.307(12) Uiso 1 1 d GD . . H3S H 0.6904 0.6651 0.4470 0.368 Uiso 1 1 calc R . . C4S C 0.7258(6) 0.7923(15) 0.4939(7) 0.248(9) Uiso 1 1 d GD . . H4S H 0.7818 0.7724 0.5074 0.297 Uiso 1 1 calc R . . C5S C 0.6983(10) 0.8853(13) 0.5100(6) 0.312(12) Uiso 1 1 d GD . . H5S H 0.7354 0.9288 0.5345 0.374 Uiso 1 1 calc R . . C6S C 0.6165(12) 0.9144(8) 0.4902(7) 0.277(10) Uiso 1 1 d GD . . H6S H 0.5977 0.9779 0.5012 0.332 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 0.02702(14) 0.02212(14) 0.02723(17) 0.00027(14) -0.00182(11) 0.00047(11) Si3 0.0286(7) 0.0310(7) 0.0372(9) -0.0058(7) -0.0008(6) 0.0014(5) Si1 0.0352(7) 0.0251(7) 0.0426(10) 0.0025(7) -0.0029(7) -0.0003(6) Si4 0.0355(7) 0.0300(7) 0.0282(9) 0.0017(7) -0.0021(7) 0.0036(6) Si2 0.0420(8) 0.0383(8) 0.0327(9) 0.0081(8) 0.0048(7) -0.0004(6) O1 0.0311(17) 0.0389(19) 0.032(2) -0.0008(18) 0.0014(16) 0.0058(14) N1 0.031(2) 0.030(2) 0.041(3) -0.005(2) -0.005(2) 0.0021(17) N4 0.031(2) 0.026(2) 0.029(3) -0.0003(19) -0.0013(19) 0.0005(16) N3 0.036(2) 0.028(2) 0.035(3) 0.007(2) 0.003(2) -0.0031(17) C26 0.033(3) 0.034(3) 0.042(4) -0.005(3) 0.002(3) -0.008(2) N2 0.028(2) 0.031(2) 0.038(3) -0.010(2) -0.004(2) -0.0007(17) C22 0.027(2) 0.030(3) 0.042(4) -0.003(3) 0.001(2) -0.0064(19) C23 0.033(3) 0.028(3) 0.049(4) 0.002(3) -0.003(3) -0.001(2) C7 0.030(2) 0.030(3) 0.038(3) -0.006(3) -0.003(2) 0.003(2) C21 0.025(2) 0.028(2) 0.035(3) -0.006(2) -0.002(2) -0.0031(18) N5 0.034(2) 0.029(2) 0.046(3) -0.006(2) -0.002(2) 0.0023(18) C25 0.044(3) 0.037(3) 0.047(4) -0.005(3) 0.014(3) -0.009(2) C27 0.046(3) 0.038(3) 0.039(4) -0.009(3) -0.005(3) 0.000(2) C8 0.034(3) 0.034(3) 0.043(4) 0.000(3) 0.008(3) 0.005(2) C24 0.037(3) 0.028(3) 0.061(5) -0.008(3) 0.008(3) -0.002(2) C36 0.055(4) 0.062(4) 0.043(4) 0.017(3) 0.002(3) 0.013(3) C39 0.042(3) 0.034(3) 0.061(5) -0.009(3) 0.010(3) -0.005(2) C43 0.053(3) 0.036(3) 0.050(4) -0.005(3) -0.013(3) -0.001(3) C261 0.051(3) 0.040(3) 0.045(4) 0.003(3) -0.004(3) -0.003(3) C6 0.034(3) 0.041(3) 0.057(4) -0.016(3) -0.010(3) 0.007(2) C31 0.056(4) 0.073(4) 0.037(4) 0.010(4) -0.003(3) 0.007(3) C221 0.036(3) 0.044(3) 0.048(4) 0.004(3) 0.001(3) -0.005(2) C40 0.043(3) 0.038(3) 0.084(6) -0.024(4) 0.018(4) -0.006(3) C1 0.032(2) 0.019(2) 0.028(3) 0.005(2) 0.002(2) 0.0026(18) C32 0.066(4) 0.048(3) 0.053(5) 0.014(3) 0.020(4) 0.000(3) C30 0.052(3) 0.042(3) 0.035(4) -0.004(3) 0.005(3) -0.009(2) C5 0.026(2) 0.040(3) 0.058(4) -0.011(3) -0.005(3) 0.001(2) C35 0.033(3) 0.045(3) 0.038(3) -0.007(3) 0.002(2) -0.007(2) C38 0.052(3) 0.051(3) 0.038(4) 0.009(3) 0.001(3) -0.007(3) C241 0.064(4) 0.035(3) 0.085(6) -0.013(4) 0.021(4) 0.010(3) C29 0.060(4) 0.037(3) 0.057(5) 0.002(3) -0.008(3) 0.010(3) C9 0.044(3) 0.062(4) 0.049(4) -0.014(4) 0.000(3) 0.014(3) C37 0.066(4) 0.044(3) 0.037(4) -0.004(3) 0.018(3) -0.005(3) C41 0.047(4) 0.041(4) 0.106(7) -0.023(4) -0.005(4) 0.010(3) C10 0.044(3) 0.057(4) 0.058(5) 0.013(3) 0.014(3) -0.003(3) C34 0.037(3) 0.059(4) 0.062(5) -0.020(4) -0.001(3) -0.011(3) C42 0.063(4) 0.038(3) 0.064(5) -0.003(4) -0.025(4) 0.004(3) C33 0.046(3) 0.051(3) 0.053(4) -0.003(3) 0.009(3) 0.017(3) C28 0.052(4) 0.046(3) 0.081(6) -0.004(4) 0.007(4) -0.013(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.155(3) . ? Ce1 N3 2.398(4) . ? Ce1 N4 2.408(4) . ? Ce1 N5 2.810(4) . ? Ce1 C1 2.844(5) . ? Ce1 Si3 3.4720(14) . ? Ce1 Si2 3.4816(16) . ? Si3 N4 1.701(4) . ? Si3 C33 1.876(5) . ? Si3 C34 1.880(6) . ? Si3 C35 1.886(6) . ? Si1 N3 1.703(4) . ? Si1 C27 1.864(6) . ? Si1 C29 1.870(6) . ? Si1 C28 1.876(6) . ? Si4 N4 1.713(5) . ? Si4 C37 1.865(6) . ? Si4 C38 1.869(6) . ? Si4 C36 1.875(6) . ? Si2 N3 1.697(5) . ? Si2 C32 1.865(6) . ? Si2 C31 1.867(6) . ? Si2 C30 1.869(5) . ? O1 C8 1.394(6) . ? N1 C1 1.337(6) . ? N1 C7 1.456(6) . ? N1 C6 1.474(6) . ? C26 C21 1.378(8) . ? C26 C25 1.393(7) . ? C26 C261 1.511(8) . ? N2 C1 1.347(6) . ? N2 C21 1.428(6) . ? N2 C5 1.488(6) . ? C22 C23 1.379(7) . ? C22 C21 1.391(7) . ? C22 C221 1.508(8) . ? C23 C24 1.378(8) . ? C23 H3 0.9500 . ? C7 C8 1.521(8) . ? C7 H10A 0.9900 . ? C7 H10B 0.9900 . ? N5 C43 1.328(8) . ? N5 C39 1.335(7) . ? C25 C24 1.389(8) . ? C25 H4 0.9500 . ? C27 H01A 0.9800 . ? C27 H01B 0.9800 . ? C27 H01C 0.9800 . ? C8 C9 1.522(8) . ? C8 C10 1.549(7) . ? C24 C241 1.531(7) . ? C36 H02A 0.9800 . ? C36 H02B 0.9800 . ? C36 H02C 0.9800 . ? C39 C40 1.376(8) . ? C39 H022 0.9500 . ? C43 C42 1.395(8) . ? C43 H023 0.9500 . ? C261 H02D 0.9800 . ? C261 H02E 0.9800 . ? C261 H02F 0.9800 . ? C6 C5 1.511(7) . ? C6 H02G 0.9900 . ? C6 H02H 0.9900 . ? C31 H02X 0.9800 . ? C31 H02Y 0.9800 . ? C31 H02Z 0.9800 . ? C221 H02J 0.9800 . ? C221 H02K 0.9800 . ? C221 H02L 0.9800 . ? C40 C41 1.367(10) . ? C40 H028 0.9500 . ? C32 H03A 0.9800 . ? C32 H03B 0.9800 . ? C32 H03C 0.9800 . ? C30 H03D 0.9800 . ? C30 H03E 0.9800 . ? C30 H03F 0.9800 . ? C5 H03G 0.9900 . ? C5 H03H 0.9900 . ? C35 H03X 0.9800 . ? C35 H03Y 0.9800 . ? C35 H03Z 0.9800 . ? C38 H03J 0.9800 . ? C38 H03K 0.9800 . ? C38 H03L 0.9800 . ? C241 H03M 0.9800 . ? C241 H03N 0.9800 . ? C241 H03O 0.9800 . ? C29 H03P 0.9800 . ? C29 H03Q 0.9800 . ? C29 H03R 0.9800 . ? C9 H03S 0.9800 . ? C9 H03T 0.9800 . ? C9 H03U 0.9800 . ? C37 H03V 0.9800 . ? C37 H03 0.9800 . ? C37 H03W 0.9800 . ? C41 C42 1.355(10) . ? C41 H040 0.9500 . ? C10 H04A 0.9800 . ? C10 H04B 0.9800 . ? C10 H04C 0.9800 . ? C34 H04D 0.9800 . ? C34 H04E 0.9800 . ? C34 H04F 0.9800 . ? C42 H043 0.9500 . ? C33 H04G 0.9800 . ? C33 H04H 0.9800 . ? C33 H04I 0.9800 . ? C28 H12A 0.9800 . ? C28 H12B 0.9800 . ? C28 H12C 0.9800 . ? N1S C2S 1.3900 . ? N1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C2S H2S 0.9500 . ? C3S C4S 1.3900 . ? C3S H3S 0.9500 . ? C4S C5S 1.3900 . ? C4S H4S 0.9500 . ? C5S C6S 1.3900 . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? 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 N3 101.31(14) . . ? O1 Ce1 N4 97.69(14) . . ? N3 Ce1 N4 115.34(14) . . ? O1 Ce1 N5 129.00(13) . . ? N3 Ce1 N5 126.28(15) . . ? N4 Ce1 N5 79.23(13) . . ? O1 Ce1 C1 70.89(14) . . ? N3 Ce1 C1 95.89(14) . . ? N4 Ce1 C1 148.51(13) . . ? N5 Ce1 C1 85.64(13) . . ? O1 Ce1 Si3 122.05(10) . . ? N3 Ce1 Si3 97.62(10) . . ? N4 Ce1 Si3 26.53(10) . . ? N5 Ce1 Si3 73.04(9) . . ? C1 Ce1 Si3 158.65(9) . . ? O1 Ce1 Si2 112.17(10) . . ? N3 Ce1 Si2 26.12(11) . . ? N4 Ce1 Si2 132.84(10) . . ? N5 Ce1 Si2 105.71(11) . . ? C1 Ce1 Si2 77.81(10) . . ? Si3 Ce1 Si2 108.60(4) . . ? N4 Si3 C33 115.7(2) . . ? N4 Si3 C34 113.4(2) . . ? C33 Si3 C34 107.0(3) . . ? N4 Si3 C35 110.1(2) . . ? C33 Si3 C35 104.2(3) . . ? C34 Si3 C35 105.6(3) . . ? N4 Si3 Ce1 39.22(15) . . ? C33 Si3 Ce1 129.1(2) . . ? C34 Si3 Ce1 123.3(2) . . ? C35 Si3 Ce1 70.91(16) . . ? N3 Si1 C27 109.4(2) . . ? N3 Si1 C29 112.2(3) . . ? C27 Si1 C29 107.8(3) . . ? N3 Si1 C28 114.9(3) . . ? C27 Si1 C28 106.0(3) . . ? C29 Si1 C28 106.0(3) . . ? N4 Si4 C37 112.6(2) . . ? N4 Si4 C38 110.8(3) . . ? C37 Si4 C38 106.9(3) . . ? N4 Si4 C36 114.8(2) . . ? C37 Si4 C36 105.3(3) . . ? C38 Si4 C36 105.9(3) . . ? N3 Si2 C32 114.9(3) . . ? N3 Si2 C31 113.6(3) . . ? C32 Si2 C31 106.9(3) . . ? N3 Si2 C30 107.7(2) . . ? C32 Si2 C30 106.3(3) . . ? C31 Si2 C30 107.0(3) . . ? N3 Si2 Ce1 38.48(14) . . ? C32 Si2 Ce1 141.7(2) . . ? C31 Si2 Ce1 110.0(2) . . ? C30 Si2 Ce1 72.71(19) . . ? C8 O1 Ce1 145.0(4) . . ? C1 N1 C7 125.6(4) . . ? C1 N1 C6 114.1(4) . . ? C7 N1 C6 120.3(4) . . ? Si3 N4 Si4 123.0(3) . . ? Si3 N4 Ce1 114.2(2) . . ? Si4 N4 Ce1 122.5(2) . . ? Si2 N3 Si1 124.4(2) . . ? Si2 N3 Ce1 115.4(2) . . ? Si1 N3 Ce1 120.2(2) . . ? C21 C26 C25 118.2(5) . . ? C21 C26 C261 122.0(5) . . ? C25 C26 C261 119.8(5) . . ? C1 N2 C21 127.0(4) . . ? C1 N2 C5 113.9(4) . . ? C21 N2 C5 118.0(4) . . ? C23 C22 C21 118.9(5) . . ? C23 C22 C221 120.3(5) . . ? C21 C22 C221 120.8(5) . . ? C24 C23 C22 121.2(5) . . ? C24 C23 H3 119.4 . . ? C22 C23 H3 119.4 . . ? N1 C7 C8 114.5(4) . . ? N1 C7 H10A 108.6 . . ? C8 C7 H10A 108.6 . . ? N1 C7 H10B 108.6 . . ? C8 C7 H10B 108.6 . . ? H10A C7 H10B 107.6 . . ? C26 C21 C22 121.6(5) . . ? C26 C21 N2 119.1(5) . . ? C22 C21 N2 119.2(5) . . ? C43 N5 C39 116.8(5) . . ? C43 N5 Ce1 113.1(4) . . ? C39 N5 Ce1 129.0(4) . . ? C24 C25 C26 121.2(6) . . ? C24 C25 H4 119.4 . . ? C26 C25 H4 119.4 . . ? Si1 C27 H01A 109.5 . . ? Si1 C27 H01B 109.5 . . ? H01A C27 H01B 109.5 . . ? Si1 C27 H01C 109.5 . . ? H01A C27 H01C 109.5 . . ? H01B C27 H01C 109.5 . . ? O1 C8 C7 108.4(4) . . ? O1 C8 C9 110.9(4) . . ? C7 C8 C9 108.3(4) . . ? O1 C8 C10 109.6(4) . . ? C7 C8 C10 109.8(5) . . ? C9 C8 C10 109.8(5) . . ? C23 C24 C25 118.9(5) . . ? C23 C24 C241 120.8(6) . . ? C25 C24 C241 120.2(6) . . ? Si4 C36 H02A 109.5 . . ? Si4 C36 H02B 109.5 . . ? H02A C36 H02B 109.5 . . ? Si4 C36 H02C 109.5 . . ? H02A C36 H02C 109.5 . . ? H02B C36 H02C 109.5 . . ? N5 C39 C40 123.7(7) . . ? N5 C39 H022 118.2 . . ? C40 C39 H022 118.2 . . ? N5 C43 C42 122.7(7) . . ? N5 C43 H023 118.6 . . ? C42 C43 H023 118.6 . . ? C26 C261 H02D 109.5 . . ? C26 C261 H02E 109.5 . . ? H02D C261 H02E 109.5 . . ? C26 C261 H02F 109.5 . . ? H02D C261 H02F 109.5 . . ? H02E C261 H02F 109.5 . . ? N1 C6 C5 103.0(4) . . ? N1 C6 H02G 111.2 . . ? C5 C6 H02G 111.2 . . ? N1 C6 H02H 111.2 . . ? C5 C6 H02H 111.2 . . ? H02G C6 H02H 109.1 . . ? Si2 C31 H02X 109.5 . . ? Si2 C31 H02Y 109.5 . . ? H02X C31 H02Y 109.5 . . ? Si2 C31 H02Z 109.5 . . ? H02X C31 H02Z 109.5 . . ? H02Y C31 H02Z 109.5 . . ? C22 C221 H02J 109.5 . . ? C22 C221 H02K 109.5 . . ? H02J C221 H02K 109.5 . . ? C22 C221 H02L 109.5 . . ? H02J C221 H02L 109.5 . . ? H02K C221 H02L 109.5 . . ? C41 C40 C39 118.6(7) . . ? C41 C40 H028 120.7 . . ? C39 C40 H028 120.7 . . ? N1 C1 N2 106.6(4) . . ? N1 C1 Ce1 114.5(3) . . ? N2 C1 Ce1 138.6(3) . . ? Si2 C32 H03A 109.5 . . ? Si2 C32 H03B 109.5 . . ? H03A C32 H03B 109.5 . . ? Si2 C32 H03C 109.5 . . ? H03A C32 H03C 109.5 . . ? H03B C32 H03C 109.5 . . ? Si2 C30 H03D 109.5 . . ? Si2 C30 H03E 109.5 . . ? H03D C30 H03E 109.5 . . ? Si2 C30 H03F 109.5 . . ? H03D C30 H03F 109.5 . . ? H03E C30 H03F 109.5 . . ? N2 C5 C6 101.6(4) . . ? N2 C5 H03G 111.4 . . ? C6 C5 H03G 111.4 . . ? N2 C5 H03H 111.4 . . ? C6 C5 H03H 111.4 . . ? H03G C5 H03H 109.3 . . ? Si3 C35 H03X 109.5 . . ? Si3 C35 H03Y 109.5 . . ? H03X C35 H03Y 109.5 . . ? Si3 C35 H03Z 109.5 . . ? H03X C35 H03Z 109.5 . . ? H03Y C35 H03Z 109.5 . . ? Si4 C38 H03J 109.5 . . ? Si4 C38 H03K 109.5 . . ? H03J C38 H03K 109.5 . . ? Si4 C38 H03L 109.5 . . ? H03J C38 H03L 109.5 . . ? H03K C38 H03L 109.5 . . ? C24 C241 H03M 109.5 . . ? C24 C241 H03N 109.5 . . ? H03M C241 H03N 109.5 . . ? C24 C241 H03O 109.5 . . ? H03M C241 H03O 109.5 . . ? H03N C241 H03O 109.5 . . ? Si1 C29 H03P 109.5 . . ? Si1 C29 H03Q 109.5 . . ? H03P C29 H03Q 109.5 . . ? Si1 C29 H03R 109.5 . . ? H03P C29 H03R 109.5 . . ? H03Q C29 H03R 109.5 . . ? C8 C9 H03S 109.5 . . ? C8 C9 H03T 109.5 . . ? H03S C9 H03T 109.5 . . ? C8 C9 H03U 109.5 . . ? H03S C9 H03U 109.5 . . ? H03T C9 H03U 109.5 . . ? Si4 C37 H03V 109.5 . . ? Si4 C37 H03 109.5 . . ? H03V C37 H03 109.5 . . ? Si4 C37 H03W 109.5 . . ? H03V C37 H03W 109.5 . . ? H03 C37 H03W 109.5 . . ? C42 C41 C40 119.0(6) . . ? C42 C41 H040 120.5 . . ? C40 C41 H040 120.5 . . ? C8 C10 H04A 109.5 . . ? C8 C10 H04B 109.5 . . ? H04A C10 H04B 109.5 . . ? C8 C10 H04C 109.5 . . ? H04A C10 H04C 109.5 . . ? H04B C10 H04C 109.5 . . ? Si3 C34 H04D 109.5 . . ? Si3 C34 H04E 109.5 . . ? H04D C34 H04E 109.5 . . ? Si3 C34 H04F 109.5 . . ? H04D C34 H04F 109.5 . . ? H04E C34 H04F 109.5 . . ? C41 C42 C43 119.1(7) . . ? C41 C42 H043 120.4 . . ? C43 C42 H043 120.4 . . ? Si3 C33 H04G 109.5 . . ? Si3 C33 H04H 109.5 . . ? H04G C33 H04H 109.5 . . ? Si3 C33 H04I 109.5 . . ? H04G C33 H04I 109.5 . . ? H04H C33 H04I 109.5 . . ? Si1 C28 H12A 109.5 . . ? Si1 C28 H12B 109.5 . . ? H12A C28 H12B 109.5 . . ? Si1 C28 H12C 109.5 . . ? H12A C28 H12C 109.5 . . ? H12B C28 H12C 109.5 . . ? C2S N1S C6S 120.0 . . ? N1S C2S C3S 120.0 . . ? N1S C2S H2S 120.0 . . ? C3S C2S H2S 120.0 . . ? C4S C3S C2S 120.0 . . ? C4S C3S H3S 120.0 . . ? C2S C3S H3S 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S H4S 120.0 . . ? C3S C4S H4S 120.0 . . ? C6S C5S C4S 120.0 . . ? C6S C5S H5S 120.0 . . ? C4S C5S H5S 120.0 . . ? C5S C6S N1S 120.0 . . ? C5S C6S H6S 120.0 . . ? N1S C6S H6S 120.0 . . ? 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 Si3 N4 25.8(2) . . . . ? N3 Ce1 Si3 N4 134.3(2) . . . . ? N5 Ce1 Si3 N4 -100.0(2) . . . . ? C1 Ce1 Si3 N4 -96.9(4) . . . . ? Si2 Ce1 Si3 N4 158.7(2) . . . . ? O1 Ce1 Si3 C33 109.4(3) . . . . ? N3 Ce1 Si3 C33 -142.1(3) . . . . ? N4 Ce1 Si3 C33 83.5(3) . . . . ? N5 Ce1 Si3 C33 -16.5(3) . . . . ? C1 Ce1 Si3 C33 -13.3(4) . . . . ? Si2 Ce1 Si3 C33 -117.8(3) . . . . ? O1 Ce1 Si3 C34 -61.0(3) . . . . ? N3 Ce1 Si3 C34 47.5(3) . . . . ? N4 Ce1 Si3 C34 -86.9(3) . . . . ? N5 Ce1 Si3 C34 173.1(3) . . . . ? C1 Ce1 Si3 C34 176.3(4) . . . . ? Si2 Ce1 Si3 C34 71.9(3) . . . . ? O1 Ce1 Si3 C35 -157.6(2) . . . . ? N3 Ce1 Si3 C35 -49.1(2) . . . . ? N4 Ce1 Si3 C35 176.6(3) . . . . ? N5 Ce1 Si3 C35 76.6(2) . . . . ? C1 Ce1 Si3 C35 79.7(3) . . . . ? Si2 Ce1 Si3 C35 -24.69(18) . . . . ? O1 Ce1 Si2 N3 69.5(2) . . . . ? N4 Ce1 Si2 N3 -55.6(3) . . . . ? N5 Ce1 Si2 N3 -145.3(2) . . . . ? C1 Ce1 Si2 N3 132.8(2) . . . . ? Si3 Ce1 Si2 N3 -68.4(2) . . . . ? O1 Ce1 Si2 C32 129.6(4) . . . . ? N3 Ce1 Si2 C32 60.1(4) . . . . ? N4 Ce1 Si2 C32 4.5(4) . . . . ? N5 Ce1 Si2 C32 -85.2(4) . . . . ? C1 Ce1 Si2 C32 -167.1(4) . . . . ? Si3 Ce1 Si2 C32 -8.3(3) . . . . ? O1 Ce1 Si2 C31 -33.6(3) . . . . ? N3 Ce1 Si2 C31 -103.1(3) . . . . ? N4 Ce1 Si2 C31 -158.7(3) . . . . ? N5 Ce1 Si2 C31 111.6(3) . . . . ? C1 Ce1 Si2 C31 29.7(3) . . . . ? Si3 Ce1 Si2 C31 -171.4(2) . . . . ? O1 Ce1 Si2 C30 -135.8(2) . . . . ? N3 Ce1 Si2 C30 154.7(3) . . . . ? N4 Ce1 Si2 C30 99.1(2) . . . . ? N5 Ce1 Si2 C30 9.3(2) . . . . ? C1 Ce1 Si2 C30 -72.5(2) . . . . ? Si3 Ce1 Si2 C30 86.32(19) . . . . ? N3 Ce1 O1 C8 59.1(6) . . . . ? N4 Ce1 O1 C8 177.0(5) . . . . ? N5 Ce1 O1 C8 -100.7(5) . . . . ? C1 Ce1 O1 C8 -33.2(5) . . . . ? Si3 Ce1 O1 C8 165.7(5) . . . . ? Si2 Ce1 O1 C8 34.3(6) . . . . ? C33 Si3 N4 Si4 65.0(4) . . . . ? C34 Si3 N4 Si4 -59.2(4) . . . . ? C35 Si3 N4 Si4 -177.3(3) . . . . ? Ce1 Si3 N4 Si4 -173.9(4) . . . . ? C33 Si3 N4 Ce1 -121.2(3) . . . . ? C34 Si3 N4 Ce1 114.7(3) . . . . ? C35 Si3 N4 Ce1 -3.4(3) . . . . ? C37 Si4 N4 Si3 93.0(3) . . . . ? C38 Si4 N4 Si3 -147.3(3) . . . . ? C36 Si4 N4 Si3 -27.4(4) . . . . ? C37 Si4 N4 Ce1 -80.3(3) . . . . ? C38 Si4 N4 Ce1 39.3(3) . . . . ? C36 Si4 N4 Ce1 159.3(3) . . . . ? O1 Ce1 N4 Si3 -158.1(2) . . . . ? N3 Ce1 N4 Si3 -51.7(2) . . . . ? N5 Ce1 N4 Si3 73.5(2) . . . . ? C1 Ce1 N4 Si3 136.2(2) . . . . ? Si2 Ce1 N4 Si3 -28.0(3) . . . . ? O1 Ce1 N4 Si4 15.8(2) . . . . ? N3 Ce1 N4 Si4 122.2(2) . . . . ? N5 Ce1 N4 Si4 -112.6(2) . . . . ? C1 Ce1 N4 Si4 -49.9(4) . . . . ? Si3 Ce1 N4 Si4 173.9(4) . . . . ? Si2 Ce1 N4 Si4 145.89(16) . . . . ? C32 Si2 N3 Si1 37.3(4) . . . . ? C31 Si2 N3 Si1 -86.2(4) . . . . ? C30 Si2 N3 Si1 155.5(3) . . . . ? Ce1 Si2 N3 Si1 -179.1(4) . . . . ? C32 Si2 N3 Ce1 -143.6(3) . . . . ? C31 Si2 N3 Ce1 92.9(3) . . . . ? C30 Si2 N3 Ce1 -25.4(3) . . . . ? C27 Si1 N3 Si2 172.7(3) . . . . ? C29 Si1 N3 Si2 53.1(4) . . . . ? C28 Si1 N3 Si2 -68.1(4) . . . . ? C27 Si1 N3 Ce1 -6.3(3) . . . . ? C29 Si1 N3 Ce1 -126.0(3) . . . . ? C28 Si1 N3 Ce1 112.8(3) . . . . ? O1 Ce1 N3 Si2 -117.8(2) . . . . ? N4 Ce1 N3 Si2 138.0(2) . . . . ? N5 Ce1 N3 Si2 42.8(3) . . . . ? C1 Ce1 N3 Si2 -46.1(2) . . . . ? Si3 Ce1 N3 Si2 117.3(2) . . . . ? O1 Ce1 N3 Si1 61.3(2) . . . . ? N4 Ce1 N3 Si1 -42.9(3) . . . . ? N5 Ce1 N3 Si1 -138.1(2) . . . . ? C1 Ce1 N3 Si1 133.0(2) . . . . ? Si3 Ce1 N3 Si1 -63.6(2) . . . . ? Si2 Ce1 N3 Si1 179.1(4) . . . . ? C21 C22 C23 C24 -0.6(7) . . . . ? C221 C22 C23 C24 177.0(5) . . . . ? C1 N1 C7 C8 -61.5(7) . . . . ? C6 N1 C7 C8 118.4(5) . . . . ? C25 C26 C21 C22 -2.5(7) . . . . ? C261 C26 C21 C22 177.6(5) . . . . ? C25 C26 C21 N2 -178.1(4) . . . . ? C261 C26 C21 N2 2.1(7) . . . . ? C23 C22 C21 C26 1.6(7) . . . . ? C221 C22 C21 C26 -176.0(5) . . . . ? C23 C22 C21 N2 177.2(4) . . . . ? C221 C22 C21 N2 -0.4(7) . . . . ? C1 N2 C21 C26 -111.1(6) . . . . ? C5 N2 C21 C26 81.3(6) . . . . ? C1 N2 C21 C22 73.2(7) . . . . ? C5 N2 C21 C22 -94.4(6) . . . . ? O1 Ce1 N5 C43 -49.6(4) . . . . ? N3 Ce1 N5 C43 155.3(3) . . . . ? N4 Ce1 N5 C43 41.7(4) . . . . ? C1 Ce1 N5 C43 -110.6(4) . . . . ? Si3 Ce1 N5 C43 68.3(4) . . . . ? Si2 Ce1 N5 C43 173.4(3) . . . . ? O1 Ce1 N5 C39 142.7(4) . . . . ? N3 Ce1 N5 C39 -12.5(5) . . . . ? N4 Ce1 N5 C39 -126.1(5) . . . . ? C1 Ce1 N5 C39 81.7(4) . . . . ? Si3 Ce1 N5 C39 -99.5(4) . . . . ? Si2 Ce1 N5 C39 5.6(5) . . . . ? C21 C26 C25 C24 2.4(8) . . . . ? C261 C26 C25 C24 -177.7(5) . . . . ? Ce1 O1 C8 C7 -3.5(7) . . . . ? Ce1 O1 C8 C9 -122.2(6) . . . . ? Ce1 O1 C8 C10 116.4(6) . . . . ? N1 C7 C8 O1 64.7(5) . . . . ? N1 C7 C8 C9 -174.9(4) . . . . ? N1 C7 C8 C10 -55.0(6) . . . . ? C22 C23 C24 C25 0.6(8) . . . . ? C22 C23 C24 C241 179.5(5) . . . . ? C26 C25 C24 C23 -1.5(8) . . . . ? C26 C25 C24 C241 179.6(5) . . . . ? C43 N5 C39 C40 -0.7(8) . . . . ? Ce1 N5 C39 C40 166.7(4) . . . . ? C39 N5 C43 C42 -0.2(8) . . . . ? Ce1 N5 C43 C42 -169.6(5) . . . . ? C1 N1 C6 C5 5.9(7) . . . . ? C7 N1 C6 C5 -174.0(5) . . . . ? N5 C39 C40 C41 0.3(9) . . . . ? C7 N1 C1 N2 178.9(5) . . . . ? C6 N1 C1 N2 -1.0(6) . . . . ? C7 N1 C1 Ce1 4.0(6) . . . . ? C6 N1 C1 Ce1 -175.8(4) . . . . ? C21 N2 C1 N1 -172.8(5) . . . . ? C5 N2 C1 N1 -4.7(6) . . . . ? C21 N2 C1 Ce1 0.2(9) . . . . ? C5 N2 C1 Ce1 168.2(4) . . . . ? O1 Ce1 C1 N1 30.0(3) . . . . ? N3 Ce1 C1 N1 -70.0(4) . . . . ? N4 Ce1 C1 N1 102.8(4) . . . . ? N5 Ce1 C1 N1 164.0(4) . . . . ? Si3 Ce1 C1 N1 161.0(2) . . . . ? Si2 Ce1 C1 N1 -88.9(3) . . . . ? O1 Ce1 C1 N2 -142.6(5) . . . . ? N3 Ce1 C1 N2 117.4(5) . . . . ? N4 Ce1 C1 N2 -69.7(6) . . . . ? N5 Ce1 C1 N2 -8.6(5) . . . . ? Si3 Ce1 C1 N2 -11.6(7) . . . . ? Si2 Ce1 C1 N2 98.5(5) . . . . ? C1 N2 C5 C6 8.1(7) . . . . ? C21 N2 C5 C6 177.3(5) . . . . ? N1 C6 C5 N2 -7.6(6) . . . . ? C39 C40 C41 C42 1.0(9) . . . . ? C40 C41 C42 C43 -1.9(10) . . . . ? N5 C43 C42 C41 1.5(9) . . . . ? C6S N1S C2S C3S 0.0 . . . . ? N1S C2S C3S C4S 0.0 . . . . ? C2S C3S C4S C5S 0.0 . . . . ? C3S C4S C5S C6S 0.0 . . . . ? C4S C5S C6S N1S 0.0 . . . . ? C2S N1S C6S C5S 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.992 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.110