# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global #TrackingRef '- mfl_28jul2009.CIF' _journal_coden_Cambridge 222 loop_ _publ_author_name 'M. F. Lappert' 'P. B. Hitchcock' 'A. V. Khvostov' 'Z. Li' 'A. V. Protchenko' _publ_contact_author_name 'M. F. Lappert' _publ_contact_author_address ; Department of Chemistry University of Sussex BRIGHTON BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email m.f.lappert@sussex.ac.uk _publ_requested_category FM data_(3)-oct1004 _database_code_depnum_ccdc_archive 'CCDC 774593' #TrackingRef '- mfl_28jul2009.CIF' _audit_creation_date 2004-10-15T08:20:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H72 Ce2 N4 O2 Si8' _chemical_formula_sum 'C24 H72 Ce2 N4 O2 Si8' _chemical_formula_weight 953.82 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7748(2) _cell_length_b 70.064(2) _cell_length_c 12.0284(4) _cell_angle_alpha 90.014(1) _cell_angle_beta 108.399(1) _cell_angle_gamma 89.983(1) _cell_volume 7017.0(3) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 60560 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 22.986 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.15 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6622 _exptl_absorpt_correction_T_max 0.728 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.566015E-1 _diffrn_orient_matrix_ub_12 -0.118055E-1 _diffrn_orient_matrix_ub_13 -0.124059E-1 _diffrn_orient_matrix_ub_21 0.770236E-1 _diffrn_orient_matrix_ub_22 0.79903E-2 _diffrn_orient_matrix_ub_23 -0.259243E-1 _diffrn_orient_matrix_ub_31 0.727385E-1 _diffrn_orient_matrix_ub_32 0.731E-3 _diffrn_orient_matrix_ub_33 0.827763E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_unetI/netI 0.0658 _diffrn_reflns_number 43092 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -76 _diffrn_reflns_limit_k_max 75 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 23.01 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.924 _diffrn_measured_fraction_theta_max 0.924 _reflns_number_total 18117 _reflns_number_gt 8816 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Although the cell dimensions look like monoclinic the diffraction symmetry is triclinic. The structure was solved in space group P-1 but refined to a high R factor and with large residual peaks. Assuming the crystals to be twinned the structure refined to an acceptable value and the residual peaks disappeared. However the refinement did not want to converge properly and some of the C atoms went non-positive-definite. Finally the C atoms were left isotropic and the three independent molecules were restrained to have equivalent bond lengths using the SAME parameter in SHELXL . Twin relationship (1 0 0 \ 0 -1 0 \ 0 0 1) Twin ratio 0.63 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^)+(0.0526P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 18117 _refine_ls_number_parameters 632 _refine_ls_number_restraints 336 _refine_ls_R_factor_all 0.0984 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.98 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.656 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.122 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 -0.32910(16) 0.26983(2) -0.80058(11) 0.0318(4) Uani 1 1 d D . . Ce2 Ce -0.15920(15) 0.22718(2) -0.78872(11) 0.0315(4) Uani 1 1 d D . . Si1 Si -0.6062(7) 0.27351(9) -1.0866(5) 0.0311(19) Uani 1 1 d D . . Si2 Si -0.3267(7) 0.30220(9) -0.9988(5) 0.0319(18) Uani 1 1 d D . . Si3 Si -0.1562(7) 0.28576(10) -0.5087(5) 0.0362(19) Uani 1 1 d D . . Si4 Si -0.4906(7) 0.29938(10) -0.6475(5) 0.034(2) Uani 1 1 d D . . Si5 Si -0.3426(8) 0.19078(10) -0.9485(6) 0.040(2) Uani 1 1 d D . . Si6 Si -0.2043(7) 0.21775(10) -1.0902(5) 0.038(2) Uani 1 1 d D . . Si7 Si 0.2218(7) 0.21747(11) -0.6495(5) 0.042(2) Uani 1 1 d D . . Si8 Si 0.0111(7) 0.21151(10) -0.4936(5) 0.036(2) Uani 1 1 d D . . O1 O -0.1238(12) 0.25638(16) -0.8103(10) 0.036(4) Uiso 1 1 d D . . O2 O -0.3677(11) 0.24128(14) -0.7712(9) 0.023(3) Uiso 1 1 d D . . N1 N -0.4392(13) 0.28309(17) -0.9809(9) 0.026(5) Uiso 1 1 d D . . N2 N -0.3204(13) 0.28615(19) -0.6362(9) 0.032(5) Uiso 1 1 d D . . N3 N -0.2392(16) 0.21114(17) -0.9609(9) 0.036(5) Uiso 1 1 d D . . N4 N 0.0376(12) 0.2166(2) -0.6266(9) 0.029(5) Uiso 1 1 d D . . C1 C -0.570(2) 0.2700(3) -1.2303(12) 0.040(6) Uiso 1 1 d D . . H1A H -0.5518 0.2824 -1.2614 0.061 Uiso 1 1 calc R . . H1B H -0.6642 0.2639 -1.2856 0.061 Uiso 1 1 calc R . . H1C H -0.4756 0.2619 -1.2192 0.061 Uiso 1 1 calc R . . C2 C -0.7880(16) 0.2895(2) -1.1114(14) 0.034(5) Uiso 1 1 d D . . H2A H -0.8136 0.2908 -1.0381 0.051 Uiso 1 1 calc R . . H2B H -0.8798 0.2839 -1.1716 0.051 Uiso 1 1 calc R . . H2C H -0.7647 0.3021 -1.1372 0.051 Uiso 1 1 calc R . . C3 C -0.645(2) 0.2500(2) -1.0350(17) 0.060(8) Uiso 1 1 d D . . H3A H -0.6608 0.2513 -0.9582 0.09 Uiso 1 1 calc R . . H3B H -0.5535 0.2416 -1.0283 0.09 Uiso 1 1 calc R . . H3C H -0.7421 0.2446 -1.0908 0.09 Uiso 1 1 calc R . . C4 C -0.234(2) 0.2993(3) -1.1177(13) 0.036(6) Uiso 1 1 d D . . H4A H -0.3183 0.2975 -1.1928 0.054 Uiso 1 1 calc R . . H4B H -0.1621 0.2882 -1.1008 0.054 Uiso 1 1 calc R . . H4C H -0.172 0.3108 -1.1218 0.054 Uiso 1 1 calc R . . C5 C -0.1583(19) 0.3059(3) -0.8596(13) 0.045(7) Uiso 1 1 d D . . H5A H -0.0938 0.2942 -0.84 0.067 Uiso 1 1 calc R . . H5B H -0.2021 0.3089 -0.7961 0.067 Uiso 1 1 calc R . . H5C H -0.0906 0.3164 -0.8695 0.067 Uiso 1 1 calc R . . C6 C -0.446(2) 0.3245(2) -1.0285(16) 0.049(7) Uiso 1 1 d D . . H6A H -0.5359 0.3231 -1.1013 0.073 Uiso 1 1 calc R . . H6B H -0.3776 0.3352 -1.0365 0.073 Uiso 1 1 calc R . . H6C H -0.488 0.3271 -0.9635 0.073 Uiso 1 1 calc R . . C7 C -0.095(2) 0.3087(2) -0.4373(14) 0.042(6) Uiso 1 1 d D . . H7A H -0.0718 0.3176 -0.4928 0.064 Uiso 1 1 calc R . . H7B H 0.0013 0.307 -0.3695 0.064 Uiso 1 1 calc R . . H7C H -0.182 0.3139 -0.4113 0.064 Uiso 1 1 calc R . . C8 C 0.0195(19) 0.2756(3) -0.5471(17) 0.061(8) Uiso 1 1 d D . . H8A H 0.047 0.2841 -0.6025 0.091 Uiso 1 1 calc R . . H8B H -0.0091 0.263 -0.5829 0.091 Uiso 1 1 calc R . . H8C H 0.1119 0.2744 -0.4758 0.091 Uiso 1 1 calc R . . C9 C -0.197(2) 0.2687(3) -0.4013(15) 0.052(8) Uiso 1 1 d D . . H9A H -0.2926 0.2729 -0.3824 0.078 Uiso 1 1 calc R . . H9B H -0.1047 0.2685 -0.3297 0.078 Uiso 1 1 calc R . . H9C H -0.2157 0.2559 -0.4358 0.078 Uiso 1 1 calc R . . C10 C -0.6569(18) 0.2869(3) -0.7661(14) 0.049(7) Uiso 1 1 d D . . H10A H -0.6311 0.2869 -0.8396 0.074 Uiso 1 1 calc R . . H10B H -0.7587 0.2935 -0.7774 0.074 Uiso 1 1 calc R . . H10C H -0.6665 0.2736 -0.7424 0.074 Uiso 1 1 calc R . . C11 C -0.550(2) 0.2990(3) -0.5119(13) 0.044(7) Uiso 1 1 d D . . H11A H -0.4656 0.305 -0.4475 0.066 Uiso 1 1 calc R . . H11B H -0.5658 0.2858 -0.4913 0.066 Uiso 1 1 calc R . . H11C H -0.6507 0.3062 -0.5255 0.066 Uiso 1 1 calc R . . C12 C -0.475(3) 0.3242(2) -0.6923(17) 0.067(8) Uiso 1 1 d D . . H12A H -0.4468 0.3244 -0.7648 0.101 Uiso 1 1 calc R . . H12B H -0.3921 0.3309 -0.6304 0.101 Uiso 1 1 calc R . . H12C H -0.5786 0.3307 -0.7055 0.101 Uiso 1 1 calc R . . C13 C -0.244(2) 0.1691(3) -0.9821(16) 0.059(7) Uiso 1 1 d D . . H13A H -0.1323 0.1686 -0.9302 0.089 Uiso 1 1 calc R . . H13B H -0.2446 0.1696 -1.0638 0.089 Uiso 1 1 calc R . . H13C H -0.3014 0.1577 -0.9702 0.089 Uiso 1 1 calc R . . C14 C -0.5592(16) 0.1919(3) -1.0363(15) 0.054(7) Uiso 1 1 d D . . H14A H -0.6068 0.2035 -1.0163 0.081 Uiso 1 1 calc R . . H14B H -0.6148 0.1807 -1.0189 0.081 Uiso 1 1 calc R . . H14C H -0.57 0.192 -1.1199 0.081 Uiso 1 1 calc R . . C15 C -0.315(2) 0.1877(3) -0.7886(12) 0.053(6) Uiso 1 1 d D . . H15A H -0.2003 0.1875 -0.7446 0.08 Uiso 1 1 calc R . . H15B H -0.3651 0.1757 -0.7764 0.08 Uiso 1 1 calc R . . H15C H -0.366 0.1984 -0.7612 0.08 Uiso 1 1 calc R . . C16 C -0.394(2) 0.2169(3) -1.2175(15) 0.056(8) Uiso 1 1 d D . . H16A H -0.4753 0.2249 -1.2011 0.084 Uiso 1 1 calc R . . H16B H -0.4323 0.2037 -1.2303 0.084 Uiso 1 1 calc R . . H16C H -0.3721 0.2216 -1.2879 0.084 Uiso 1 1 calc R . . C17 C -0.133(2) 0.2433(2) -1.0798(17) 0.047(7) Uiso 1 1 d D . . H17A H -0.2101 0.2515 -1.0589 0.07 Uiso 1 1 calc R . . H17B H -0.1242 0.2473 -1.1556 0.07 Uiso 1 1 calc R . . H17C H -0.0277 0.2443 -1.0197 0.07 Uiso 1 1 calc R . . C18 C -0.060(2) 0.2009(3) -1.1271(15) 0.051(7) Uiso 1 1 d D . . H18A H -0.1013 0.1879 -1.1314 0.077 Uiso 1 1 calc R . . H18B H 0.0448 0.2017 -1.0663 0.077 Uiso 1 1 calc R . . H18C H -0.0488 0.2045 -1.2029 0.077 Uiso 1 1 calc R . . C19 C 0.3105(19) 0.19292(19) -0.6420(15) 0.050(5) Uiso 1 1 d D . . H19A H 0.34 0.1882 -0.5613 0.076 Uiso 1 1 calc R . . H19B H 0.4064 0.1935 -0.6671 0.076 Uiso 1 1 calc R . . H19C H 0.2314 0.1843 -0.6937 0.076 Uiso 1 1 calc R . . C20 C 0.186(2) 0.2258(3) -0.8055(12) 0.055(6) Uiso 1 1 d D . . H20A H 0.1282 0.2379 -0.8179 0.082 Uiso 1 1 calc R . . H20B H 0.1222 0.2162 -0.8599 0.082 Uiso 1 1 calc R . . H20C H 0.2895 0.2274 -0.8193 0.082 Uiso 1 1 calc R . . C21 C 0.363(2) 0.2352(3) -0.5594(16) 0.064(8) Uiso 1 1 d D . . H21A H 0.3803 0.2326 -0.4762 0.096 Uiso 1 1 calc R . . H21B H 0.3182 0.2481 -0.5787 0.096 Uiso 1 1 calc R . . H21C H 0.4657 0.2344 -0.5753 0.096 Uiso 1 1 calc R . . C22 C 0.069(3) 0.1863(2) -0.4471(18) 0.076(9) Uiso 1 1 d D . . H22A H 0.0109 0.1776 -0.51 0.114 Uiso 1 1 calc R . . H22B H 0.0406 0.1834 -0.3762 0.114 Uiso 1 1 calc R . . H22C H 0.1846 0.1847 -0.4309 0.114 Uiso 1 1 calc R . . C23 C -0.2057(16) 0.2152(3) -0.5083(16) 0.048(7) Uiso 1 1 d D . . H23A H -0.2724 0.2072 -0.5723 0.073 Uiso 1 1 calc R . . H23B H -0.2339 0.2286 -0.5254 0.073 Uiso 1 1 calc R . . H23C H -0.2244 0.2116 -0.435 0.073 Uiso 1 1 calc R . . C24 C 0.133(2) 0.2275(3) -0.3738(15) 0.065(9) Uiso 1 1 d D . . H24A H 0.2467 0.2265 -0.3681 0.098 Uiso 1 1 calc R . . H24B H 0.1194 0.2236 -0.2992 0.098 Uiso 1 1 calc R . . H24C H 0.0972 0.2407 -0.3912 0.098 Uiso 1 1 calc R . . Ce1B Ce 0.82564(15) 0.43939(2) 0.12303(11) 0.0286(4) Uani 1 1 d D . . Ce2B Ce 0.99523(16) 0.39681(2) 0.13452(10) 0.0301(4) Uani 1 1 d D . . Si1B Si 0.6598(7) 0.45536(10) -0.1718(5) 0.0332(19) Uani 1 1 d D . . Si2B Si 0.4444(7) 0.44924(9) -0.0169(5) 0.0316(18) Uani 1 1 d D . . Si3B Si 0.8708(7) 0.44879(10) 0.4253(5) 0.034(2) Uani 1 1 d D . . Si4B Si 1.0133(7) 0.47547(9) 0.2845(5) 0.0352(19) Uani 1 1 d D . . Si5B Si 1.2687(7) 0.39281(10) 0.4197(5) 0.033(2) Uani 1 1 d D . . Si6B Si 0.9925(7) 0.36440(10) 0.3353(5) 0.033(2) Uani 1 1 d D . . Si7B Si 1.1549(8) 0.36751(9) -0.0203(5) 0.0372(19) Uani 1 1 d D . . Si8B Si 0.8224(7) 0.38126(9) -0.1559(5) 0.0352(19) Uani 1 1 d D . . O1B O 1.0256(13) 0.42570(15) 0.1021(10) 0.041(4) Uiso 1 1 d D . . O2B O 0.7869(12) 0.41086(13) 0.1473(9) 0.026(4) Uiso 1 1 d D . . N1B N 0.6294(11) 0.44952(19) -0.0408(8) 0.026(5) Uiso 1 1 d D . . N2B N 0.9032(14) 0.45572(15) 0.2966(8) 0.027(5) Uiso 1 1 d D . . N3B N 1.1014(12) 0.38381(15) 0.3161(8) 0.021(4) Uiso 1 1 d D . . N4B N 0.9833(12) 0.37984(18) -0.0282(8) 0.033(5) Uiso 1 1 d D . . C1B C 0.8745(15) 0.4542(3) -0.1622(14) 0.041(6) Uiso 1 1 d D . . H1B1 H 0.9153 0.4413 -0.1399 0.062 Uiso 1 1 calc R . . H1B2 H 0.936 0.4633 -0.1032 0.062 Uiso 1 1 calc R . . H1B3 H 0.8859 0.4574 -0.2385 0.062 Uiso 1 1 calc R . . C2B C 0.5454(18) 0.4383(2) -0.2944(12) 0.037(5) Uiso 1 1 d D . . H2B1 H 0.5777 0.4251 -0.2711 0.056 Uiso 1 1 calc R . . H2B2 H 0.5704 0.4414 -0.3662 0.056 Uiso 1 1 calc R . . H2B3 H 0.4297 0.4397 -0.3085 0.056 Uiso 1 1 calc R . . C3B C 0.597(2) 0.4799(2) -0.2216(17) 0.064(8) Uiso 1 1 d D . . H3B1 H 0.6569 0.489 -0.162 0.096 Uiso 1 1 calc R . . H3B2 H 0.4817 0.4813 -0.2338 0.096 Uiso 1 1 calc R . . H3B3 H 0.6188 0.4823 -0.2953 0.096 Uiso 1 1 calc R . . C4B C 0.3102(17) 0.4293(2) -0.0972(13) 0.043(6) Uiso 1 1 d D . . H4B1 H 0.3697 0.4173 -0.0822 0.064 Uiso 1 1 calc R . . H4B2 H 0.2743 0.432 -0.1814 0.064 Uiso 1 1 calc R . . H4B3 H 0.2166 0.4284 -0.0696 0.064 Uiso 1 1 calc R . . C5B C 0.479(2) 0.4446(3) 0.1413(10) 0.045(6) Uiso 1 1 d D . . H5B1 H 0.5581 0.4537 0.1883 0.067 Uiso 1 1 calc R . . H5B2 H 0.5197 0.4316 0.1604 0.067 Uiso 1 1 calc R . . H5B3 H 0.3779 0.4461 0.1587 0.067 Uiso 1 1 calc R . . C6B C 0.3275(16) 0.47139(18) -0.0581(13) 0.036(5) Uiso 1 1 d D . . H6B1 H 0.389 0.4821 -0.0132 0.054 Uiso 1 1 calc R . . H6B2 H 0.2259 0.4701 -0.0412 0.054 Uiso 1 1 calc R . . H6B3 H 0.3055 0.4738 -0.142 0.054 Uiso 1 1 calc R . . C7B C 0.798(2) 0.42361(18) 0.4149(15) 0.040(6) Uiso 1 1 d D . . H7B1 H 0.6992 0.4224 0.3483 0.06 Uiso 1 1 calc R . . H7B2 H 0.7759 0.4202 0.4873 0.06 Uiso 1 1 calc R . . H7B3 H 0.8802 0.4151 0.4036 0.06 Uiso 1 1 calc R . . C8B C 1.0575(17) 0.4490(3) 0.5557(13) 0.045(7) Uiso 1 1 d D . . H8B1 H 1.1386 0.4407 0.5405 0.068 Uiso 1 1 calc R . . H8B2 H 1.032 0.4443 0.6247 0.068 Uiso 1 1 calc R . . H8B3 H 1.0992 0.462 0.5701 0.068 Uiso 1 1 calc R . . C9B C 0.7120(18) 0.4633(3) 0.4579(16) 0.054(7) Uiso 1 1 d D . . H9B1 H 0.6132 0.4628 0.391 0.081 Uiso 1 1 calc R . . H9B2 H 0.7481 0.4766 0.4722 0.081 Uiso 1 1 calc R . . H9B3 H 0.6913 0.4582 0.5276 0.081 Uiso 1 1 calc R . . C10B C 0.999(2) 0.4771(3) 0.1223(10) 0.039(6) Uiso 1 1 d D . . H10D H 1.051 0.466 0.1008 0.059 Uiso 1 1 calc R . . H10E H 1.0526 0.4888 0.1093 0.059 Uiso 1 1 calc R . . H10F H 0.8857 0.4775 0.074 0.059 Uiso 1 1 calc R . . C11B C 1.2338(14) 0.4739(3) 0.3590(14) 0.049(6) Uiso 1 1 d D . . H11D H 1.2555 0.4736 0.4441 0.074 Uiso 1 1 calc R . . H11E H 1.2866 0.485 0.3382 0.074 Uiso 1 1 calc R . . H11F H 1.2756 0.4622 0.3341 0.074 Uiso 1 1 calc R . . C12B C 0.935(2) 0.4985(2) 0.3181(14) 0.048(6) Uiso 1 1 d D . . H12D H 0.9332 0.4983 0.3993 0.072 Uiso 1 1 calc R . . H12E H 0.8252 0.5004 0.265 0.072 Uiso 1 1 calc R . . H12F H 1.0036 0.5089 0.308 0.072 Uiso 1 1 calc R . . C13B C 1.4553(18) 0.3790(3) 0.4421(15) 0.049(7) Uiso 1 1 d D . . H13D H 1.4736 0.3771 0.3666 0.074 Uiso 1 1 calc R . . H13E H 1.4453 0.3666 0.4765 0.074 Uiso 1 1 calc R . . H13F H 1.546 0.386 0.4951 0.074 Uiso 1 1 calc R . . C14B C 1.308(2) 0.41728(19) 0.3667(15) 0.045(7) Uiso 1 1 d D . . H14D H 1.3235 0.4161 0.29 0.068 Uiso 1 1 calc R . . H14E H 1.4042 0.4228 0.4228 0.068 Uiso 1 1 calc R . . H14F H 1.2155 0.4256 0.3601 0.068 Uiso 1 1 calc R . . C15B C 1.2428(19) 0.3955(3) 0.5641(12) 0.032(6) Uiso 1 1 d D . . H15D H 1.1447 0.4028 0.5565 0.048 Uiso 1 1 calc R . . H15E H 1.3355 0.4023 0.6164 0.048 Uiso 1 1 calc R . . H15F H 1.2344 0.3829 0.5966 0.048 Uiso 1 1 calc R . . C16B C 1.106(2) 0.3417(2) 0.3698(16) 0.053(7) Uiso 1 1 d D . . H16D H 1.16 0.3393 0.311 0.079 Uiso 1 1 calc R . . H16E H 1.0324 0.3312 0.3692 0.079 Uiso 1 1 calc R . . H16F H 1.187 0.3426 0.4475 0.079 Uiso 1 1 calc R . . C17B C 0.8201(17) 0.3612(3) 0.1920(11) 0.035(6) Uiso 1 1 d D . . H17D H 0.7561 0.3729 0.1744 0.053 Uiso 1 1 calc R . . H17E H 0.752 0.3506 0.2001 0.053 Uiso 1 1 calc R . . H17F H 0.864 0.3585 0.1282 0.053 Uiso 1 1 calc R . . C18B C 0.887(2) 0.3688(3) 0.4481(14) 0.057(7) Uiso 1 1 d D . . H18D H 0.8264 0.3808 0.43 0.086 Uiso 1 1 calc R . . H18E H 0.9668 0.3697 0.5262 0.086 Uiso 1 1 calc R . . H18F H 0.8131 0.3583 0.4467 0.086 Uiso 1 1 calc R . . C19B C 1.141(2) 0.34180(18) 0.0186(16) 0.049(7) Uiso 1 1 d D . . H19D H 1.1069 0.341 0.0886 0.073 Uiso 1 1 calc R . . H19E H 1.246 0.3357 0.0341 0.073 Uiso 1 1 calc R . . H19F H 1.0621 0.3353 -0.0467 0.073 Uiso 1 1 calc R . . C20B C 1.3249(18) 0.3772(3) 0.1054(13) 0.043(6) Uiso 1 1 d D . . H20D H 1.341 0.3908 0.0916 0.064 Uiso 1 1 calc R . . H20E H 1.4234 0.3701 0.1117 0.064 Uiso 1 1 calc R . . H20F H 1.2985 0.3759 0.1784 0.064 Uiso 1 1 calc R . . C21B C 1.215(2) 0.3693(3) -0.1550(13) 0.046(7) Uiso 1 1 d D . . H21D H 1.2197 0.3827 -0.1759 0.069 Uiso 1 1 calc R . . H21E H 1.1365 0.3626 -0.2194 0.069 Uiso 1 1 calc R . . H21F H 1.3212 0.3634 -0.1405 0.069 Uiso 1 1 calc R . . C22B C 0.773(2) 0.3570(2) -0.2282(16) 0.052(7) Uiso 1 1 d D . . H22D H 0.8666 0.352 -0.2466 0.078 Uiso 1 1 calc R . . H22E H 0.6822 0.3582 -0.3006 0.078 Uiso 1 1 calc R . . H22F H 0.7441 0.3482 -0.1747 0.078 Uiso 1 1 calc R . . C23B C 0.865(2) 0.3977(2) -0.2648(12) 0.030(6) Uiso 1 1 d D . . H23D H 0.955 0.3928 -0.2876 0.045 Uiso 1 1 calc R . . H23E H 0.8922 0.4104 -0.2296 0.045 Uiso 1 1 calc R . . H23F H 0.7694 0.3987 -0.3342 0.045 Uiso 1 1 calc R . . C24B C 0.6431(18) 0.3901(3) -0.1210(16) 0.052(7) Uiso 1 1 d D . . H24D H 0.6206 0.3817 -0.0631 0.078 Uiso 1 1 calc R . . H24E H 0.5504 0.3903 -0.1925 0.078 Uiso 1 1 calc R . . H24F H 0.6639 0.4031 -0.0889 0.078 Uiso 1 1 calc R . . Ce1C Ce 0.49267(15) 0.10607(2) 0.45644(12) 0.0334(4) Uani 1 1 d D . . Ce2C Ce 0.66244(16) 0.06345(2) 0.46780(11) 0.0345(4) Uani 1 1 d D . . Si1C Si 0.3226(6) 0.12235(10) 0.1615(5) 0.037(2) Uani 1 1 d D . . Si2C Si 0.1116(7) 0.11607(11) 0.3167(5) 0.039(2) Uani 1 1 d D . . Si3C Si 0.5396(8) 0.11529(11) 0.7606(5) 0.043(2) Uani 1 1 d D . . Si4C Si 0.6718(8) 0.14215(10) 0.6139(5) 0.041(2) Uani 1 1 d D . . Si5C Si 0.9349(7) 0.05971(9) 0.7522(5) 0.039(2) Uani 1 1 d D . . Si6C Si 0.6591(7) 0.03087(9) 0.6679(5) 0.0292(18) Uani 1 1 d D . . Si7C Si 0.8250(7) 0.03406(10) 0.3150(5) 0.038(2) Uani 1 1 d D . . Si8C Si 0.4890(7) 0.04735(11) 0.1755(5) 0.040(2) Uani 1 1 d D . . O1C O 0.4541(13) 0.07721(16) 0.4750(10) 0.041(4) Uiso 1 1 d D . . O2C O 0.6978(13) 0.09256(16) 0.4411(10) 0.042(4) Uiso 1 1 d D . . N1C N 0.2958(11) 0.1163(2) 0.2944(8) 0.033(5) Uiso 1 1 d D . . N2C N 0.5696(14) 0.12215(15) 0.6296(8) 0.028(5) Uiso 1 1 d D . . N3C N 0.7735(13) 0.04969(16) 0.6463(8) 0.032(5) Uiso 1 1 d D . . N4C N 0.6495(12) 0.04624(18) 0.3034(8) 0.032(5) Uiso 1 1 d D . . C1C C 0.284(2) 0.1480(2) 0.1236(16) 0.065(7) Uiso 1 1 d D . . H1C1 H 0.349 0.1558 0.1888 0.097 Uiso 1 1 calc R . . H1C2 H 0.1702 0.1508 0.1087 0.097 Uiso 1 1 calc R . . H1C3 H 0.3137 0.1508 0.0532 0.097 Uiso 1 1 calc R . . C2C C 0.5437(16) 0.1175(3) 0.1751(16) 0.052(7) Uiso 1 1 d D . . H2C1 H 0.5714 0.1044 0.2013 0.079 Uiso 1 1 calc R . . H2C2 H 0.6129 0.1264 0.2321 0.079 Uiso 1 1 calc R . . H2C3 H 0.5594 0.1194 0.0987 0.079 Uiso 1 1 calc R . . C3C C 0.1952(19) 0.1088(2) 0.0379(13) 0.047(6) Uiso 1 1 d D . . H3C1 H 0.2137 0.0951 0.0532 0.071 Uiso 1 1 calc R . . H3C2 H 0.2209 0.1122 -0.0332 0.071 Uiso 1 1 calc R . . H3C3 H 0.0822 0.1118 0.027 0.071 Uiso 1 1 calc R . . C4C C -0.028(2) 0.0974(3) 0.2289(18) 0.082(9) Uiso 1 1 d D . . H4C1 H 0.0241 0.0849 0.2438 0.123 Uiso 1 1 calc R . . H4C2 H -0.0564 0.1005 0.1453 0.123 Uiso 1 1 calc R . . H4C3 H -0.1263 0.0971 0.2516 0.123 Uiso 1 1 calc R . . C5C C 0.145(2) 0.1104(3) 0.4736(11) 0.056(8) Uiso 1 1 d D . . H5C1 H 0.1937 0.0977 0.4913 0.084 Uiso 1 1 calc R . . H5C2 H 0.0421 0.1105 0.4893 0.084 Uiso 1 1 calc R . . H5C3 H 0.2171 0.1199 0.523 0.084 Uiso 1 1 calc R . . C6C C 0.007(3) 0.1394(2) 0.2851(19) 0.086(10) Uiso 1 1 d D . . H6C1 H -0.0076 0.1431 0.2039 0.128 Uiso 1 1 calc R . . H6C2 H 0.0707 0.1491 0.3382 0.128 Uiso 1 1 calc R . . H6C3 H -0.0988 0.1384 0.2967 0.128 Uiso 1 1 calc R . . C7C C 0.464(2) 0.0906(2) 0.7506(18) 0.063(8) Uiso 1 1 d D . . H7C1 H 0.366 0.0895 0.6836 0.094 Uiso 1 1 calc R . . H7C2 H 0.441 0.0873 0.8227 0.094 Uiso 1 1 calc R . . H7C3 H 0.546 0.0819 0.7401 0.094 Uiso 1 1 calc R . . C8C C 0.7292(17) 0.1165(3) 0.8875(13) 0.047(7) Uiso 1 1 d D . . H8C1 H 0.7714 0.1296 0.8953 0.071 Uiso 1 1 calc R . . H8C2 H 0.8086 0.1077 0.8742 0.071 Uiso 1 1 calc R . . H8C3 H 0.7067 0.1129 0.9594 0.071 Uiso 1 1 calc R . . C9C C 0.386(2) 0.1309(3) 0.7930(18) 0.081(10) Uiso 1 1 d D . . H9C1 H 0.2876 0.1309 0.7255 0.122 Uiso 1 1 calc R . . H9C2 H 0.4276 0.1439 0.8084 0.122 Uiso 1 1 calc R . . H9C3 H 0.3618 0.126 0.8619 0.122 Uiso 1 1 calc R . . C10C C 0.672(2) 0.1436(3) 0.4585(11) 0.052(7) Uiso 1 1 d D . . H10G H 0.7045 0.1313 0.4351 0.078 Uiso 1 1 calc R . . H10H H 0.7468 0.1535 0.4517 0.078 Uiso 1 1 calc R . . H10I H 0.5633 0.1467 0.4075 0.078 Uiso 1 1 calc R . . C11C C 0.8895(17) 0.1419(3) 0.7075(16) 0.080(9) Uiso 1 1 d D . . H11G H 0.9388 0.1298 0.6965 0.12 Uiso 1 1 calc R . . H11H H 0.8967 0.1433 0.7901 0.12 Uiso 1 1 calc R . . H11I H 0.9461 0.1525 0.6845 0.12 Uiso 1 1 calc R . . C12C C 0.589(3) 0.1647(3) 0.6539(18) 0.084(10) Uiso 1 1 d D . . H12G H 0.595 0.1642 0.7366 0.126 Uiso 1 1 calc R . . H12H H 0.4768 0.1662 0.6051 0.126 Uiso 1 1 calc R . . H12I H 0.6518 0.1756 0.6411 0.126 Uiso 1 1 calc R . . C13C C 0.903(3) 0.0630(3) 0.8967(14) 0.078(9) Uiso 1 1 d D . . H13G H 0.8111 0.0715 0.8876 0.117 Uiso 1 1 calc R . . H13H H 0.9993 0.0687 0.9521 0.117 Uiso 1 1 calc R . . H13I H 0.8815 0.0506 0.9264 0.117 Uiso 1 1 calc R . . C14C C 0.980(2) 0.08348(18) 0.6983(14) 0.033(6) Uiso 1 1 d D . . H14G H 0.8843 0.0916 0.6805 0.05 Uiso 1 1 calc R . . H14H H 1.0102 0.0817 0.6272 0.05 Uiso 1 1 calc R . . H14I H 1.0686 0.0896 0.7589 0.05 Uiso 1 1 calc R . . C15C C 1.114(2) 0.0444(3) 0.7845(19) 0.100(10) Uiso 1 1 d D . . H15G H 1.139 0.0418 0.7119 0.15 Uiso 1 1 calc R . . H15H H 1.094 0.0323 0.8186 0.15 Uiso 1 1 calc R . . H15I H 1.2057 0.0509 0.8402 0.15 Uiso 1 1 calc R . . C16C C 0.573(2) 0.0336(3) 0.7903(13) 0.038(6) Uiso 1 1 d D . . H16G H 0.5101 0.0454 0.7796 0.058 Uiso 1 1 calc R . . H16H H 0.6603 0.0341 0.8649 0.058 Uiso 1 1 calc R . . H16I H 0.5034 0.0226 0.7906 0.058 Uiso 1 1 calc R . . C17C C 0.4838(17) 0.0287(3) 0.5275(12) 0.037(6) Uiso 1 1 d D . . H17G H 0.4233 0.0407 0.5129 0.055 Uiso 1 1 calc R . . H17H H 0.4132 0.0183 0.5352 0.055 Uiso 1 1 calc R . . H17I H 0.5243 0.0261 0.462 0.055 Uiso 1 1 calc R . . C18C C 0.7769(19) 0.0079(2) 0.6927(15) 0.037(6) Uiso 1 1 d D . . H18G H 0.867 0.0088 0.7656 0.055 Uiso 1 1 calc R . . H18H H 0.818 0.0057 0.627 0.055 Uiso 1 1 calc R . . H18I H 0.7069 -0.0027 0.6985 0.055 Uiso 1 1 calc R . . C19C C 0.800(2) 0.00838(18) 0.3461(17) 0.053(7) Uiso 1 1 d D . . H19G H 0.7106 0.003 0.2827 0.08 Uiso 1 1 calc R . . H19H H 0.7768 0.0072 0.4204 0.08 Uiso 1 1 calc R . . H19I H 0.8989 0.0014 0.3514 0.08 Uiso 1 1 calc R . . C20C C 0.894(2) 0.0350(3) 0.1828(13) 0.058(8) Uiso 1 1 d D . . H20G H 0.8093 0.03 0.1148 0.088 Uiso 1 1 calc R . . H20H H 0.9911 0.0272 0.1966 0.088 Uiso 1 1 calc R . . H20I H 0.9181 0.0482 0.168 0.088 Uiso 1 1 calc R . . C21C C 0.990(2) 0.0450(3) 0.4385(14) 0.057(8) Uiso 1 1 d D . . H21G H 0.9595 0.0448 0.5101 0.085 Uiso 1 1 calc R . . H21H H 1.0072 0.0582 0.4187 0.085 Uiso 1 1 calc R . . H21I H 1.0892 0.0377 0.451 0.085 Uiso 1 1 calc R . . C22C C 0.443(2) 0.0229(2) 0.1040(17) 0.066(8) Uiso 1 1 d D . . H22G H 0.536 0.0184 0.0824 0.099 Uiso 1 1 calc R . . H22H H 0.3494 0.0238 0.0335 0.099 Uiso 1 1 calc R . . H22I H 0.421 0.0139 0.1592 0.099 Uiso 1 1 calc R . . C23C C 0.521(2) 0.0641(3) 0.0668(15) 0.060(8) Uiso 1 1 d D . . H23G H 0.6146 0.06 0.0448 0.09 Uiso 1 1 calc R . . H23H H 0.5403 0.077 0.1008 0.09 Uiso 1 1 calc R . . H23I H 0.4258 0.0643 -0.0029 0.09 Uiso 1 1 calc R . . C24C C 0.3055(16) 0.0551(3) 0.2120(14) 0.042(6) Uiso 1 1 d D . . H24G H 0.2874 0.0465 0.2706 0.063 Uiso 1 1 calc R . . H24H H 0.2121 0.0549 0.1409 0.063 Uiso 1 1 calc R . . H24I H 0.3213 0.0682 0.2434 0.063 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 0.0377(9) 0.0353(11) 0.0235(8) 0.0024(7) 0.0114(7) 0.0082(8) Ce2 0.0272(9) 0.0345(11) 0.0285(8) 0.0002(7) 0.0026(7) 0.0055(8) Si1 0.022(4) 0.037(5) 0.021(3) -0.002(3) -0.012(3) -0.012(3) Si2 0.041(4) 0.026(5) 0.032(4) -0.004(3) 0.016(3) -0.005(4) Si3 0.037(4) 0.035(5) 0.037(4) 0.000(4) 0.013(3) -0.004(4) Si4 0.029(4) 0.046(6) 0.033(4) 0.002(4) 0.020(3) 0.002(4) Si5 0.033(4) 0.039(6) 0.044(4) 0.004(4) 0.005(4) -0.006(4) Si6 0.034(4) 0.053(6) 0.018(3) -0.003(3) -0.004(3) 0.005(4) Si7 0.024(4) 0.065(6) 0.035(4) 0.013(4) 0.007(3) 0.005(4) Si8 0.032(4) 0.045(6) 0.036(4) 0.013(4) 0.018(3) 0.005(4) Ce1B 0.0286(8) 0.0330(11) 0.0222(8) 0.0010(7) 0.0050(6) 0.0027(8) Ce2B 0.0382(9) 0.0328(11) 0.0193(8) 0.0020(7) 0.0093(7) 0.0044(8) Si1B 0.045(5) 0.032(5) 0.024(4) 0.007(3) 0.015(3) -0.003(4) Si2B 0.027(4) 0.036(5) 0.039(4) 0.014(3) 0.019(3) 0.005(4) Si3B 0.026(4) 0.043(6) 0.032(4) 0.005(4) 0.007(3) 0.004(4) Si4B 0.041(4) 0.030(5) 0.033(4) -0.010(3) 0.010(3) -0.008(4) Si5B 0.021(4) 0.057(6) 0.018(3) 0.002(3) 0.005(3) -0.001(4) Si6B 0.028(4) 0.045(6) 0.024(4) 0.001(4) 0.004(3) -0.004(4) Si7B 0.056(5) 0.025(5) 0.033(4) 0.003(3) 0.017(3) -0.006(4) Si8B 0.050(5) 0.032(5) 0.020(4) -0.004(3) 0.006(3) 0.001(4) Ce1C 0.0244(9) 0.0345(11) 0.0368(9) -0.0012(8) 0.0033(7) 0.0030(8) Ce2C 0.0356(9) 0.0351(11) 0.0316(9) 0.0040(8) 0.0086(7) 0.0073(8) Si1C 0.011(3) 0.060(6) 0.035(4) 0.000(4) -0.002(3) -0.009(3) Si2C 0.018(4) 0.054(6) 0.041(4) 0.012(4) 0.004(3) 0.003(4) Si3C 0.046(4) 0.058(6) 0.036(4) 0.011(4) 0.031(3) 0.015(4) Si4C 0.052(5) 0.032(5) 0.031(4) 0.004(3) 0.001(3) 0.005(4) Si5C 0.037(4) 0.027(5) 0.053(4) 0.009(4) 0.016(4) 0.003(4) Si6C 0.022(4) 0.035(5) 0.032(4) 0.010(3) 0.012(3) 0.003(3) Si7C 0.020(4) 0.061(6) 0.034(4) -0.004(4) 0.008(3) 0.013(4) Si8C 0.026(4) 0.061(6) 0.027(4) 0.002(4) -0.001(3) 0.002(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O1 2.069(10) . ? Ce1 O2 2.078(10) . ? Ce1 N2 2.264(10) . ? Ce1 N1 2.276(10) . ? Ce2 O1 2.098(11) . ? Ce2 O2 2.147(9) . ? Ce2 N3 2.264(10) . ? Ce2 N4 2.283(10) . ? Si1 N1 1.743(10) . ? Si1 C3 1.830(15) . ? Si1 C1 1.868(12) . ? Si1 C2 1.895(12) . ? Si2 N1 1.716(11) . ? Si2 C6 1.855(12) . ? Si2 C4 1.868(12) . ? Si2 C5 1.869(13) . ? Si3 N2 1.742(10) . ? Si3 C7 1.821(13) . ? Si3 C9 1.874(14) . ? Si3 C8 1.884(13) . ? Si4 N2 1.726(10) . ? Si4 C12 1.840(14) . ? Si4 C11 1.864(12) . ? Si4 C10 1.903(12) . ? Si5 N3 1.722(11) . ? Si5 C13 1.855(14) . ? Si5 C14 1.862(13) . ? Si5 C15 1.873(13) . ? Si6 N3 1.740(11) . ? Si6 C16 1.872(14) . ? Si6 C17 1.885(13) . ? Si6 C18 1.882(13) . ? Si7 N4 1.724(11) . ? Si7 C21 1.847(14) . ? Si7 C19 1.878(12) . ? Si7 C20 1.893(13) . ? Si8 N4 1.725(10) . ? Si8 C23 1.872(13) . ? Si8 C22 1.874(14) . ? Si8 C24 1.872(13) . ? Ce1B O2B 2.064(10) . ? Ce1B O1B 2.083(10) . ? Ce1B N2B 2.287(9) . ? Ce1B N1B 2.283(9) . ? Ce2B O1B 2.094(11) . ? Ce2B O2B 2.124(9) . ? Ce2B N4B 2.264(9) . ? Ce2B N3B 2.277(8) . ? Si1B N1B 1.728(9) . ? Si1B C3B 1.844(14) . ? Si1B C1B 1.853(12) . ? Si1B C2B 1.917(12) . ? Si2B N1B 1.735(9) . ? Si2B C6B 1.839(10) . ? Si2B C5B 1.859(11) . ? Si2B C4B 1.883(11) . ? Si3B N2B 1.729(9) . ? Si3B C9B 1.864(12) . ? Si3B C7B 1.868(11) . ? Si3B C8B 1.877(11) . ? Si4B N2B 1.720(10) . ? Si4B C12B 1.847(12) . ? Si4B C11B 1.862(11) . ? Si4B C10B 1.919(11) . ? Si5B N3B 1.718(9) . ? Si5B C15B 1.830(12) . ? Si5B C13B 1.846(13) . ? Si5B C14B 1.898(12) . ? Si6B N3B 1.719(9) . ? Si6B C16B 1.853(14) . ? Si6B C18B 1.895(13) . ? Si6B C17B 1.913(11) . ? Si7B N4B 1.712(9) . ? Si7B C21B 1.860(13) . ? Si7B C20B 1.885(13) . ? Si7B C19B 1.875(11) . ? Si8B N4B 1.730(9) . ? Si8B C23B 1.870(11) . ? Si8B C24B 1.859(11) . ? Si8B C22B 1.898(12) . ? Ce1C O1C 2.075(11) . ? Ce1C O2C 2.093(10) . ? Ce1C N1C 2.273(9) . ? Ce1C N2C 2.275(9) . ? Ce2C O1C 2.092(11) . ? Ce2C O2C 2.103(11) . ? Ce2C N3C 2.274(9) . ? Ce2C N4C 2.288(9) . ? Si1C N1C 1.741(9) . ? Si1C C3C 1.819(13) . ? Si1C C1C 1.857(13) . ? Si1C C2C 1.925(12) . ? Si2C N1C 1.721(10) . ? Si2C C4C 1.875(13) . ? Si2C C5C 1.859(12) . ? Si2C C6C 1.857(13) . ? Si3C N2C 1.745(9) . ? Si3C C7C 1.841(12) . ? Si3C C8C 1.871(11) . ? Si3C C9C 1.870(13) . ? Si4C N2C 1.706(10) . ? Si4C C10C 1.870(11) . ? Si4C C12C 1.865(13) . ? Si4C C11C 1.887(12) . ? Si5C N3C 1.726(10) . ? Si5C C15C 1.842(15) . ? Si5C C13C 1.861(15) . ? Si5C C14C 1.874(11) . ? Si6C N3C 1.727(10) . ? Si6C C16C 1.863(12) . ? Si6C C18C 1.884(12) . ? Si6C C17C 1.898(11) . ? Si7C N4C 1.727(9) . ? Si7C C19C 1.865(12) . ? Si7C C20C 1.873(13) . ? Si7C C21C 1.880(13) . ? Si8C N4C 1.728(9) . ? Si8C C23C 1.846(12) . ? Si8C C24C 1.878(11) . ? Si8C C22C 1.904(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ce1 O2 76.3(4) . . ? O1 Ce1 N2 119.3(4) . . ? O2 Ce1 N2 107.5(4) . . ? O1 Ce1 N1 104.3(4) . . ? O2 Ce1 N1 120.8(4) . . ? N2 Ce1 N1 120.9(5) . . ? O1 Ce2 O2 74.2(4) . . ? O1 Ce2 N3 112.7(4) . . ? O2 Ce2 N3 106.9(4) . . ? O1 Ce2 N4 108.8(5) . . ? O2 Ce2 N4 120.3(4) . . ? N3 Ce2 N4 123.5(5) . . ? N1 Si1 C3 107.6(8) . . ? N1 Si1 C1 112.1(8) . . ? C3 Si1 C1 107.5(9) . . ? N1 Si1 C2 111.1(7) . . ? C3 Si1 C2 110.3(9) . . ? C1 Si1 C2 108.2(8) . . ? N1 Si2 C6 111.8(8) . . ? N1 Si2 C4 114.8(8) . . ? C6 Si2 C4 107.4(8) . . ? N1 Si2 C5 108.6(8) . . ? C6 Si2 C5 107.2(8) . . ? C4 Si2 C5 106.7(8) . . ? N2 Si3 C7 116.1(7) . . ? N2 Si3 C9 109.4(8) . . ? C7 Si3 C9 109.2(8) . . ? N2 Si3 C8 107.7(7) . . ? C7 Si3 C8 107.9(9) . . ? C9 Si3 C8 106.1(9) . . ? N2 Si4 C12 112.9(9) . . ? N2 Si4 C11 113.5(7) . . ? C12 Si4 C11 109.6(9) . . ? N2 Si4 C10 104.5(7) . . ? C12 Si4 C10 109.1(9) . . ? C11 Si4 C10 106.8(9) . . ? N3 Si5 C13 111.2(8) . . ? N3 Si5 C14 112.8(8) . . ? C13 Si5 C14 112.0(9) . . ? N3 Si5 C15 106.4(8) . . ? C13 Si5 C15 102.4(8) . . ? C14 Si5 C15 111.4(8) . . ? N3 Si6 C16 111.2(8) . . ? N3 Si6 C17 110.0(7) . . ? C16 Si6 C17 105.9(9) . . ? N3 Si6 C18 111.4(8) . . ? C16 Si6 C18 106.0(8) . . ? C17 Si6 C18 112.1(9) . . ? N4 Si7 C21 114.9(8) . . ? N4 Si7 C19 110.7(8) . . ? C21 Si7 C19 113.4(9) . . ? N4 Si7 C20 107.4(7) . . ? C21 Si7 C20 104.2(9) . . ? C19 Si7 C20 105.4(8) . . ? N4 Si8 C23 108.3(7) . . ? N4 Si8 C22 111.6(8) . . ? C23 Si8 C22 109.1(9) . . ? N4 Si8 C24 112.3(9) . . ? C23 Si8 C24 107.9(9) . . ? C22 Si8 C24 107.4(9) . . ? Ce1 O1 Ce2 105.7(4) . . ? Ce1 O2 Ce2 103.7(4) . . ? Si2 N1 Si1 126.4(7) . . ? Si2 N1 Ce1 110.5(5) . . ? Si1 N1 Ce1 122.9(6) . . ? Si4 N2 Si3 122.1(6) . . ? Si4 N2 Ce1 114.4(5) . . ? Si3 N2 Ce1 123.5(6) . . ? Si5 N3 Si6 123.0(7) . . ? Si5 N3 Ce2 110.6(5) . . ? Si6 N3 Ce2 126.4(6) . . ? Si8 N4 Si7 124.3(6) . . ? Si8 N4 Ce2 124.9(6) . . ? Si7 N4 Ce2 110.2(5) . . ? O2B Ce1B O1B 75.8(4) . . ? O2B Ce1B N2B 111.7(4) . . ? O1B Ce1B N2B 108.7(4) . . ? O2B Ce1B N1B 108.1(4) . . ? O1B Ce1B N1B 118.3(4) . . ? N2B Ce1B N1B 123.9(4) . . ? O1B Ce2B O2B 74.3(3) . . ? O1B Ce2B N4B 108.7(5) . . ? O2B Ce2B N4B 120.0(4) . . ? O1B Ce2B N3B 121.8(4) . . ? O2B Ce2B N3B 102.5(4) . . ? N4B Ce2B N3B 120.8(4) . . ? N1B Si1B C3B 113.6(8) . . ? N1B Si1B C1B 112.3(7) . . ? C3B Si1B C1B 104.8(9) . . ? N1B Si1B C2B 111.1(7) . . ? C3B Si1B C2B 107.5(8) . . ? C1B Si1B C2B 107.2(8) . . ? N1B Si2B C6B 114.6(7) . . ? N1B Si2B C5B 108.2(7) . . ? C6B Si2B C5B 108.7(7) . . ? N1B Si2B C4B 113.0(7) . . ? C6B Si2B C4B 106.3(7) . . ? C5B Si2B C4B 105.6(8) . . ? N2B Si3B C9B 112.3(7) . . ? N2B Si3B C7B 110.8(7) . . ? C9B Si3B C7B 105.4(8) . . ? N2B Si3B C8B 113.6(7) . . ? C9B Si3B C8B 109.5(8) . . ? C7B Si3B C8B 104.7(8) . . ? N2B Si4B C12B 115.1(7) . . ? N2B Si4B C11B 116.0(7) . . ? C12B Si4B C11B 110.4(8) . . ? N2B Si4B C10B 106.1(7) . . ? C12B Si4B C10B 105.1(8) . . ? C11B Si4B C10B 102.6(7) . . ? N3B Si5B C15B 113.1(7) . . ? N3B Si5B C13B 115.4(8) . . ? C15B Si5B C13B 106.6(8) . . ? N3B Si5B C14B 106.9(7) . . ? C15B Si5B C14B 108.4(8) . . ? C13B Si5B C14B 106.0(9) . . ? N3B Si6B C16B 115.2(8) . . ? N3B Si6B C18B 112.6(8) . . ? C16B Si6B C18B 109.3(8) . . ? N3B Si6B C17B 106.6(7) . . ? C16B Si6B C17B 108.6(8) . . ? C18B Si6B C17B 103.8(8) . . ? N4B Si7B C21B 113.9(7) . . ? N4B Si7B C20B 108.8(7) . . ? C21B Si7B C20B 107.7(8) . . ? N4B Si7B C19B 111.8(8) . . ? C21B Si7B C19B 109.9(8) . . ? C20B Si7B C19B 104.2(8) . . ? N4B Si8B C23B 111.8(7) . . ? N4B Si8B C24B 109.3(7) . . ? C23B Si8B C24B 108.7(8) . . ? N4B Si8B C22B 111.1(7) . . ? C23B Si8B C22B 107.5(7) . . ? C24B Si8B C22B 108.4(9) . . ? Ce1B O1B Ce2B 105.1(5) . . ? Ce1B O2B Ce2B 104.7(4) . . ? Si2B N1B Si1B 125.1(6) . . ? Si2B N1B Ce1B 110.1(4) . . ? Si1B N1B Ce1B 124.7(5) . . ? Si4B N2B Si3B 123.9(6) . . ? Si4B N2B Ce1B 109.8(5) . . ? Si3B N2B Ce1B 126.2(5) . . ? Si5B N3B Si6B 125.2(6) . . ? Si5B N3B Ce2B 123.1(5) . . ? Si6B N3B Ce2B 111.7(5) . . ? Si7B N4B Si8B 122.3(6) . . ? Si7B N4B Ce2B 114.6(5) . . ? Si8B N4B Ce2B 122.7(5) . . ? O1C Ce1C O2C 75.1(4) . . ? O1C Ce1C N1C 107.1(5) . . ? O2C Ce1C N1C 120.6(4) . . ? O1C Ce1C N2C 113.3(4) . . ? O2C Ce1C N2C 106.8(5) . . ? N1C Ce1C N2C 123.7(5) . . ? O1C Ce2C O2C 74.5(4) . . ? O1C Ce2C N3C 106.0(5) . . ? O2C Ce2C N3C 121.0(4) . . ? O1C Ce2C N4C 118.2(4) . . ? O2C Ce2C N4C 110.4(5) . . ? N3C Ce2C N4C 118.8(4) . . ? N1C Si1C C3C 113.4(8) . . ? N1C Si1C C1C 113.3(8) . . ? C3C Si1C C1C 106.7(8) . . ? N1C Si1C C2C 107.7(7) . . ? C3C Si1C C2C 108.7(8) . . ? C1C Si1C C2C 106.9(9) . . ? N1C Si2C C4C 113.5(8) . . ? N1C Si2C C5C 107.8(7) . . ? C4C Si2C C5C 106.7(10) . . ? N1C Si2C C6C 113.0(9) . . ? C4C Si2C C6C 107.7(9) . . ? C5C Si2C C6C 107.8(9) . . ? N2C Si3C C7C 110.7(8) . . ? N2C Si3C C8C 112.0(8) . . ? C7C Si3C C8C 107.7(9) . . ? N2C Si3C C9C 110.6(8) . . ? C7C Si3C C9C 107.2(10) . . ? C8C Si3C C9C 108.5(8) . . ? N2C Si4C C10C 108.7(7) . . ? N2C Si4C C12C 114.0(9) . . ? C10C Si4C C12C 109.6(9) . . ? N2C Si4C C11C 113.3(8) . . ? C10C Si4C C11C 106.2(9) . . ? C12C Si4C C11C 104.8(9) . . ? N3C Si5C C15C 111.5(9) . . ? N3C Si5C C13C 114.1(9) . . ? C15C Si5C C13C 104.2(9) . . ? N3C Si5C C14C 108.6(6) . . ? C15C Si5C C14C 109.3(9) . . ? C13C Si5C C14C 108.8(9) . . ? N3C Si6C C16C 116.2(8) . . ? N3C Si6C C18C 111.1(7) . . ? C16C Si6C C18C 107.4(8) . . ? N3C Si6C C17C 105.8(7) . . ? C16C Si6C C17C 107.1(8) . . ? C18C Si6C C17C 108.9(8) . . ? N4C Si7C C19C 109.5(8) . . ? N4C Si7C C20C 115.7(7) . . ? C19C Si7C C20C 107.1(9) . . ? N4C Si7C C21C 107.9(7) . . ? C19C Si7C C21C 110.2(9) . . ? C20C Si7C C21C 106.4(9) . . ? N4C Si8C C23C 113.3(8) . . ? N4C Si8C C24C 108.9(7) . . ? C23C Si8C C24C 108.3(8) . . ? N4C Si8C C22C 111.0(8) . . ? C23C Si8C C22C 108.1(9) . . ? C24C Si8C C22C 107.1(8) . . ? Ce1C O1C Ce2C 105.7(5) . . ? Ce1C O2C Ce2C 104.6(5) . . ? Si2C N1C Si1C 123.5(6) . . ? Si2C N1C Ce1C 111.1(5) . . ? Si1C N1C Ce1C 125.3(5) . . ? Si4C N2C Si3C 124.2(6) . . ? Si4C N2C Ce1C 108.6(5) . . ? Si3C N2C Ce1C 127.2(6) . . ? Si5C N3C Si6C 125.5(6) . . ? Si5C N3C Ce2C 122.1(5) . . ? Si6C N3C Ce2C 111.7(5) . . ? Si7C N4C Si8C 123.3(6) . . ? Si7C N4C Ce2C 113.0(5) . . ? Si8C N4C Ce2C 123.3(5) . . ? #===END data_(4)-dec1501 _database_code_depnum_ccdc_archive 'CCDC 774594' #TrackingRef '- mfl_28jul2009.CIF' _audit_creation_date 2001-12-19T09:46:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{Ce(O)(N(SiMe3)2)2}3]' _chemical_formula_moiety 'C36 H108 Ce3 N6 O3 Si12' _chemical_formula_sum 'C36 H108 Ce3 N6 O3 Si12' _chemical_formula_weight 1430.72 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4998(2) _cell_length_b 21.6470(6) _cell_length_c 26.9181(7) _cell_angle_alpha 83.767(1) _cell_angle_beta 78.217(2) _cell_angle_gamma 79.110(2) _cell_volume 6983.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 43630 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.16 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.868 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 42101 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_unetI/netI 0.0712 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.968 _diffrn_measured_fraction_theta_max 0.968 _reflns_number_total 23952 _reflns_number_gt 17840 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+18.2225P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 23952 _refine_ls_number_parameters 1081 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.082 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.654 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.118 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.21022(2) 0.837597(15) 0.142364(12) 0.02164(8) Uani 1 1 d . . . Ce2 Ce 0.27200(2) 0.745212(15) 0.273147(12) 0.02359(8) Uani 1 1 d . . . Ce3 Ce 0.36356(2) 0.659579(15) 0.144348(12) 0.02174(8) Uani 1 1 d . . . Si1 Si -0.03798(13) 0.92770(8) 0.14858(7) 0.0311(4) Uani 1 1 d . . . Si2 Si -0.03453(12) 0.80215(8) 0.10909(6) 0.0273(4) Uani 1 1 d . . . Si3 Si 0.32276(14) 0.92084(8) 0.04061(7) 0.0340(4) Uani 1 1 d . . . Si4 Si 0.37252(14) 0.95860(8) 0.13795(7) 0.0340(4) Uani 1 1 d . . . Si5 Si 0.53390(13) 0.76969(9) 0.29375(7) 0.0365(4) Uani 1 1 d . . . Si6 Si 0.32406(13) 0.83927(9) 0.35306(7) 0.0333(4) Uani 1 1 d . . . Si7 Si 0.00750(13) 0.73284(8) 0.35244(7) 0.0331(4) Uani 1 1 d . . . Si8 Si 0.20668(13) 0.63440(8) 0.36593(7) 0.0324(4) Uani 1 1 d . . . Si9 Si 0.61833(13) 0.69821(8) 0.07477(7) 0.0303(4) Uani 1 1 d . . . Si10 Si 0.60901(13) 0.56963(8) 0.13386(7) 0.0300(4) Uani 1 1 d . . . Si11 Si 0.14762(13) 0.57485(8) 0.17589(7) 0.0311(4) Uani 1 1 d . . . Si12 Si 0.28601(13) 0.56112(8) 0.07003(6) 0.0294(4) Uani 1 1 d . . . O1 O 0.2091(3) 0.81297(18) 0.21987(14) 0.0287(9) Uani 1 1 d . . . O2 O 0.3459(3) 0.67812(18) 0.22122(14) 0.0274(9) Uani 1 1 d . . . O3 O 0.2985(3) 0.74965(17) 0.11837(14) 0.0272(9) Uani 1 1 d . . . N1 N 0.0326(3) 0.8542(2) 0.13117(17) 0.0229(10) Uani 1 1 d . . . N2 N 0.3133(4) 0.9123(2) 0.10579(18) 0.0284(11) Uani 1 1 d . . . N3 N 0.3901(3) 0.7876(2) 0.30717(18) 0.0281(11) Uani 1 1 d . . . N4 N 0.1483(3) 0.7033(2) 0.33552(17) 0.0245(11) Uani 1 1 d . . . N5 N 0.5466(3) 0.6432(2) 0.11297(18) 0.0261(11) Uani 1 1 d . . . N6 N 0.2554(3) 0.5934(2) 0.12823(17) 0.0236(10) Uani 1 1 d . . . C1 C 0.0509(5) 0.9602(3) 0.1836(2) 0.0374(16) Uani 1 1 d . . . H1A H 0.0639 0.9317 0.2135 0.056 Uiso 1 1 calc R . . H1B H 0.0133 1.0018 0.1946 0.056 Uiso 1 1 calc R . . H1C H 0.122 0.9642 0.1612 0.056 Uiso 1 1 calc R . . C2 C -0.1744(5) 0.9263(3) 0.1916(3) 0.057(2) Uani 1 1 d . . . H2A H -0.1645 0.8971 0.2214 0.085 Uiso 1 1 calc R . . H2B H -0.225 0.9122 0.1734 0.085 Uiso 1 1 calc R . . H2C H -0.2058 0.9687 0.2025 0.085 Uiso 1 1 calc R . . C3 C -0.0598(6) 0.9832(3) 0.0921(3) 0.0516(19) Uani 1 1 d . . . H3A H 0.0115 0.9846 0.069 0.077 Uiso 1 1 calc R . . H3B H -0.0918 1.0255 0.1033 0.077 Uiso 1 1 calc R . . H3C H -0.1105 0.9688 0.0743 0.077 Uiso 1 1 calc R . . C4 C -0.1293(5) 0.7646(3) 0.1626(3) 0.0422(17) Uani 1 1 d . . . H4A H -0.1841 0.7976 0.1802 0.063 Uiso 1 1 calc R . . H4B H -0.0856 0.74 0.1866 0.063 Uiso 1 1 calc R . . H4C H -0.1676 0.7368 0.1487 0.063 Uiso 1 1 calc R . . C5 C 0.0673(5) 0.7373(3) 0.0773(2) 0.0325(14) Uani 1 1 d . . . H5A H 0.1134 0.7148 0.1012 0.049 Uiso 1 1 calc R . . H5B H 0.1145 0.755 0.0476 0.049 Uiso 1 1 calc R . . H5C H 0.0276 0.7078 0.0663 0.049 Uiso 1 1 calc R . . C6 C -0.1189(5) 0.8422(3) 0.0613(3) 0.0420(17) Uani 1 1 d . . . H6A H -0.1736 0.877 0.0765 0.063 Uiso 1 1 calc R . . H6B H -0.1572 0.8119 0.0506 0.063 Uiso 1 1 calc R . . H6C H -0.0701 0.8589 0.0316 0.063 Uiso 1 1 calc R . . C7 C 0.2575(6) 1.0005(3) 0.0161(3) 0.054(2) Uani 1 1 d . . . H7A H 0.181 1.0108 0.0345 0.081 Uiso 1 1 calc R . . H7B H 0.2577 1.0001 -0.0203 0.081 Uiso 1 1 calc R . . H7C H 0.2999 1.0323 0.0212 0.081 Uiso 1 1 calc R . . C8 C 0.4675(5) 0.9037(4) 0.0047(3) 0.0492(18) Uani 1 1 d . . . H8A H 0.5036 0.8622 0.0169 0.074 Uiso 1 1 calc R . . H8B H 0.5085 0.9361 0.0098 0.074 Uiso 1 1 calc R . . H8C H 0.4666 0.9037 -0.0316 0.074 Uiso 1 1 calc R . . C9 C 0.2461(5) 0.8623(3) 0.0228(2) 0.0439(17) Uani 1 1 d . . . H9A H 0.169 0.8697 0.0409 0.066 Uiso 1 1 calc R . . H9B H 0.2816 0.8195 0.0321 0.066 Uiso 1 1 calc R . . H9C H 0.2478 0.8674 -0.014 0.066 Uiso 1 1 calc R . . C10 C 0.3165(6) 1.0450(3) 0.1286(3) 0.0496(18) Uani 1 1 d . . . H10A H 0.3307 1.0584 0.0922 0.074 Uiso 1 1 calc R . . H10B H 0.3533 1.069 0.1468 0.074 Uiso 1 1 calc R . . H10C H 0.2365 1.0527 0.1418 0.074 Uiso 1 1 calc R . . C11 C 0.5270(5) 0.9498(3) 0.1190(3) 0.052(2) Uani 1 1 d . . . H11A H 0.5471 0.9603 0.0824 0.078 Uiso 1 1 calc R . . H11B H 0.5606 0.9061 0.1272 0.078 Uiso 1 1 calc R . . H11C H 0.5541 0.9782 0.1376 0.078 Uiso 1 1 calc R . . C12 C 0.3418(6) 0.9371(4) 0.2080(3) 0.0514(19) Uani 1 1 d . . . H12A H 0.2614 0.9411 0.2197 0.077 Uiso 1 1 calc R . . H12B H 0.3709 0.9654 0.2259 0.077 Uiso 1 1 calc R . . H12C H 0.377 0.8934 0.215 0.077 Uiso 1 1 calc R . . C13 C 0.5935(6) 0.7506(4) 0.3526(3) 0.067(2) Uani 1 1 d . . . H13A H 0.5703 0.7864 0.374 0.1 Uiso 1 1 calc R . . H13B H 0.6747 0.742 0.3435 0.1 Uiso 1 1 calc R . . H13C H 0.5671 0.7133 0.3714 0.1 Uiso 1 1 calc R . . C14 C 0.5825(5) 0.6992(3) 0.2552(3) 0.0498(19) Uani 1 1 d . . . H14A H 0.5531 0.7072 0.2236 0.075 Uiso 1 1 calc R . . H14B H 0.5561 0.6623 0.2748 0.075 Uiso 1 1 calc R . . H14C H 0.6638 0.6911 0.2471 0.075 Uiso 1 1 calc R . . C15 C 0.5980(5) 0.8358(4) 0.2562(3) 0.058(2) Uani 1 1 d . . . H15A H 0.5681 0.8468 0.2249 0.087 Uiso 1 1 calc R . . H15B H 0.6786 0.8226 0.2476 0.087 Uiso 1 1 calc R . . H15C H 0.581 0.8726 0.2765 0.087 Uiso 1 1 calc R . . C16 C 0.3047(6) 0.7977(4) 0.4177(3) 0.055(2) Uani 1 1 d . . . H16A H 0.3773 0.7791 0.426 0.082 Uiso 1 1 calc R . . H16B H 0.2613 0.7642 0.4183 0.082 Uiso 1 1 calc R . . H16C H 0.2653 0.8278 0.4427 0.082 Uiso 1 1 calc R . . C17 C 0.1830(5) 0.8738(3) 0.3392(3) 0.0401(16) Uani 1 1 d . . . H17A H 0.1907 0.8962 0.3053 0.06 Uiso 1 1 calc R . . H17B H 0.1443 0.9034 0.3647 0.06 Uiso 1 1 calc R . . H17C H 0.1404 0.8399 0.3402 0.06 Uiso 1 1 calc R . . C18 C 0.3953(5) 0.9077(3) 0.3544(3) 0.052(2) Uani 1 1 d . . . H18A H 0.4057 0.9301 0.3206 0.078 Uiso 1 1 calc R . . H18B H 0.4677 0.8923 0.364 0.078 Uiso 1 1 calc R . . H18C H 0.3498 0.9365 0.3792 0.078 Uiso 1 1 calc R . . C19 C -0.0266(6) 0.7708(3) 0.4145(3) 0.0512(19) Uani 1 1 d . . . H19A H -0.0026 0.7401 0.4413 0.077 Uiso 1 1 calc R . . H19B H -0.1069 0.7852 0.4233 0.077 Uiso 1 1 calc R . . H19C H 0.0118 0.8069 0.4114 0.077 Uiso 1 1 calc R . . C20 C -0.0813(5) 0.6702(3) 0.3614(3) 0.053(2) Uani 1 1 d . . . H20A H -0.0593 0.6381 0.3878 0.08 Uiso 1 1 calc R . . H20B H -0.0717 0.6505 0.3294 0.08 Uiso 1 1 calc R . . H20C H -0.1593 0.6892 0.3719 0.08 Uiso 1 1 calc R . . C21 C -0.0386(5) 0.7921(3) 0.3019(3) 0.0450(18) Uani 1 1 d . . . H21A H 0.0062 0.8257 0.2961 0.067 Uiso 1 1 calc R . . H21B H -0.1169 0.8103 0.3127 0.067 Uiso 1 1 calc R . . H21C H -0.0293 0.7715 0.2702 0.067 Uiso 1 1 calc R . . C22 C 0.1698(6) 0.6323(3) 0.4368(2) 0.0494(18) Uani 1 1 d . . . H22A H 0.1872 0.67 0.4484 0.074 Uiso 1 1 calc R . . H22B H 0.2125 0.5945 0.4514 0.074 Uiso 1 1 calc R . . H22C H 0.0904 0.6314 0.4477 0.074 Uiso 1 1 calc R . . C23 C 0.1717(6) 0.5617(3) 0.3469(3) 0.0530(19) Uani 1 1 d . . . H23A H 0.19 0.5609 0.3098 0.079 Uiso 1 1 calc R . . H23B H 0.0923 0.5612 0.3586 0.079 Uiso 1 1 calc R . . H23C H 0.2145 0.5245 0.3624 0.079 Uiso 1 1 calc R . . C24 C 0.3616(5) 0.6270(3) 0.3477(3) 0.0481(18) Uani 1 1 d . . . H24A H 0.3845 0.6644 0.357 0.072 Uiso 1 1 calc R . . H24B H 0.3843 0.6235 0.3109 0.072 Uiso 1 1 calc R . . H24C H 0.3967 0.5893 0.3657 0.072 Uiso 1 1 calc R . . C25 C 0.5942(5) 0.7719(3) 0.1079(3) 0.0469(18) Uani 1 1 d . . . H25A H 0.6192 0.7625 0.1405 0.07 Uiso 1 1 calc R . . H25B H 0.5148 0.7896 0.1139 0.07 Uiso 1 1 calc R . . H25C H 0.6357 0.8025 0.0867 0.07 Uiso 1 1 calc R . . C26 C 0.7717(5) 0.6706(3) 0.0585(3) 0.056(2) Uani 1 1 d . . . H26A H 0.7866 0.6316 0.041 0.084 Uiso 1 1 calc R . . H26B H 0.8024 0.6627 0.0898 0.084 Uiso 1 1 calc R . . H26C H 0.8064 0.7031 0.0362 0.084 Uiso 1 1 calc R . . C27 C 0.5691(6) 0.7185(4) 0.0133(3) 0.058(2) Uani 1 1 d . . . H27A H 0.5805 0.6802 -0.005 0.086 Uiso 1 1 calc R . . H27B H 0.6109 0.7492 -0.0075 0.086 Uiso 1 1 calc R . . H27C H 0.4899 0.7365 0.0199 0.086 Uiso 1 1 calc R . . C28 C 0.4986(5) 0.5337(3) 0.1790(2) 0.0362(15) Uani 1 1 d . . . H28A H 0.4672 0.5609 0.2071 0.054 Uiso 1 1 calc R . . H28B H 0.5309 0.492 0.1925 0.054 Uiso 1 1 calc R . . H28C H 0.44 0.5294 0.161 0.054 Uiso 1 1 calc R . . C29 C 0.7207(5) 0.5700(4) 0.1703(3) 0.053(2) Uani 1 1 d . . . H29A H 0.6921 0.5976 0.1983 0.08 Uiso 1 1 calc R . . H29B H 0.7835 0.5855 0.1476 0.08 Uiso 1 1 calc R . . H29C H 0.7453 0.5271 0.184 0.08 Uiso 1 1 calc R . . C30 C 0.6666(6) 0.5169(3) 0.0810(3) 0.0502(19) Uani 1 1 d . . . H30A H 0.609 0.5161 0.0613 0.075 Uiso 1 1 calc R . . H30B H 0.6917 0.4742 0.095 0.075 Uiso 1 1 calc R . . H30C H 0.7295 0.5329 0.0587 0.075 Uiso 1 1 calc R . . C31 C 0.1922(6) 0.5009(3) 0.2138(3) 0.0528(19) Uani 1 1 d . . . H31A H 0.2587 0.5044 0.2266 0.079 Uiso 1 1 calc R . . H31B H 0.2089 0.4652 0.1923 0.079 Uiso 1 1 calc R . . H31C H 0.1326 0.4939 0.2426 0.079 Uiso 1 1 calc R . . C32 C 0.1039(5) 0.6413(3) 0.2193(3) 0.0441(17) Uani 1 1 d . . . H32A H 0.0803 0.6806 0.1996 0.066 Uiso 1 1 calc R . . H32B H 0.1664 0.6458 0.2346 0.066 Uiso 1 1 calc R . . H32C H 0.042 0.632 0.2462 0.066 Uiso 1 1 calc R . . C33 C 0.0214(5) 0.5658(4) 0.1527(3) 0.053(2) Uani 1 1 d . . . H33A H -0.0037 0.6042 0.1324 0.079 Uiso 1 1 calc R . . H33B H -0.0374 0.5587 0.1819 0.079 Uiso 1 1 calc R . . H33C H 0.0388 0.5297 0.1316 0.079 Uiso 1 1 calc R . . C34 C 0.3378(6) 0.4749(3) 0.0756(3) 0.0517(19) Uani 1 1 d . . . H34A H 0.3995 0.4665 0.0941 0.078 Uiso 1 1 calc R . . H34B H 0.3633 0.4595 0.0416 0.078 Uiso 1 1 calc R . . H34C H 0.2778 0.4533 0.0942 0.078 Uiso 1 1 calc R . . C35 C 0.1705(5) 0.5731(4) 0.0341(3) 0.055(2) Uani 1 1 d . . . H35A H 0.1405 0.6182 0.0303 0.082 Uiso 1 1 calc R . . H35B H 0.1119 0.5505 0.0527 0.082 Uiso 1 1 calc R . . H35C H 0.1983 0.557 0.0004 0.082 Uiso 1 1 calc R . . C36 C 0.3953(5) 0.6014(4) 0.0286(3) 0.0481(18) Uani 1 1 d . . . H36A H 0.3682 0.647 0.0257 0.072 Uiso 1 1 calc R . . H36B H 0.4129 0.5853 -0.0053 0.072 Uiso 1 1 calc R . . H36C H 0.4623 0.5931 0.0436 0.072 Uiso 1 1 calc R . . Ce1B Ce 0.15418(2) 0.844076(15) 0.645020(12) 0.02197(8) Uani 1 1 d . . . Ce2B Ce 0.21851(3) 0.747720(15) 0.773685(12) 0.02372(8) Uani 1 1 d . . . Ce3B Ce 0.29794(2) 0.663478(15) 0.643455(12) 0.02278(8) Uani 1 1 d . . . Si1B Si -0.13851(13) 0.85614(9) 0.68574(7) 0.0325(4) Uani 1 1 d . . . Si2B Si -0.04588(12) 0.88479(8) 0.57514(6) 0.0281(4) Uani 1 1 d . . . Si3B Si 0.20448(14) 0.99216(8) 0.63065(7) 0.0349(4) Uani 1 1 d . . . Si4B Si 0.38230(13) 0.90441(8) 0.56562(7) 0.0329(4) Uani 1 1 d . . . Si5B Si 0.39874(15) 0.84190(9) 0.80759(7) 0.0370(4) Uani 1 1 d . . . Si6B Si 0.41955(14) 0.70397(9) 0.84076(7) 0.0386(4) Uani 1 1 d . . . Si7B Si 0.02336(15) 0.78314(9) 0.87738(7) 0.0377(4) Uani 1 1 d . . . Si8B Si 0.00834(14) 0.66106(9) 0.83802(7) 0.0382(4) Uani 1 1 d . . . Si9B Si 0.57761(13) 0.66994(9) 0.63715(7) 0.0341(4) Uani 1 1 d . . . Si1A Si 0.51403(13) 0.62339(8) 0.54626(6) 0.0306(4) Uani 1 1 d . . . Si2A Si 0.08208(13) 0.59684(8) 0.61380(7) 0.0331(4) Uani 1 1 d . . . Si3A Si 0.26340(13) 0.51134(8) 0.65977(6) 0.0290(4) Uani 1 1 d . . . O1B O 0.1667(3) 0.82008(18) 0.72140(15) 0.0308(9) Uani 1 1 d . . . O2B O 0.2797(3) 0.67977(17) 0.72056(14) 0.0274(9) Uani 1 1 d . . . O3B O 0.2210(3) 0.75367(17) 0.62178(14) 0.0263(9) Uani 1 1 d . . . N1B N -0.0256(3) 0.8645(2) 0.63705(17) 0.0247(11) Uani 1 1 d . . . N2B N 0.2611(3) 0.9176(2) 0.61050(17) 0.0245(11) Uani 1 1 d . . . N3B N 0.3548(4) 0.7702(2) 0.80933(18) 0.0274(11) Uani 1 1 d . . . N4B N 0.0697(4) 0.7274(2) 0.83269(17) 0.0273(11) Uani 1 1 d . . . N5B N 0.4795(3) 0.6528(2) 0.60610(17) 0.0264(11) Uani 1 1 d . . . N6B N 0.2038(4) 0.5856(2) 0.63836(17) 0.0267(11) Uani 1 1 d . . . C1B C -0.1118(6) 0.8677(4) 0.7490(3) 0.066(2) Uani 1 1 d . . . H1B1 H -0.0935 0.9098 0.7487 0.099 Uiso 1 1 calc R . . H1B2 H -0.0496 0.8358 0.7569 0.099 Uiso 1 1 calc R . . H1B3 H -0.1782 0.8636 0.7749 0.099 Uiso 1 1 calc R . . C2B C -0.1709(8) 0.7753(4) 0.6888(4) 0.089(3) Uani 1 1 d . . . H2B1 H -0.1862 0.7676 0.6559 0.133 Uiso 1 1 calc R . . H2B2 H -0.2361 0.7712 0.7154 0.133 Uiso 1 1 calc R . . H2B3 H -0.1074 0.7443 0.6966 0.133 Uiso 1 1 calc R . . C3B C -0.2649(6) 0.9132(5) 0.6770(3) 0.095(4) Uani 1 1 d . . . H3B1 H -0.2829 0.9089 0.6439 0.142 Uiso 1 1 calc R . . H3B2 H -0.2519 0.9562 0.6784 0.142 Uiso 1 1 calc R . . H3B3 H -0.3269 0.9047 0.7041 0.142 Uiso 1 1 calc R . . C4B C 0.0930(4) 0.8698(3) 0.5329(2) 0.0353(15) Uani 1 1 d . . . H4B1 H 0.1263 0.8254 0.5379 0.053 Uiso 1 1 calc R . . H4B2 H 0.1409 0.8966 0.5414 0.053 Uiso 1 1 calc R . . H4B3 H 0.0847 0.8796 0.4974 0.053 Uiso 1 1 calc R . . C5B C -0.1344(5) 0.8370(3) 0.5533(3) 0.0431(17) Uani 1 1 d . . . H5B1 H -0.2087 0.8435 0.5745 0.065 Uiso 1 1 calc R . . H5B2 H -0.1014 0.7923 0.5562 0.065 Uiso 1 1 calc R . . H5B3 H -0.1396 0.8501 0.5177 0.065 Uiso 1 1 calc R . . C6B C -0.1062(5) 0.9697(3) 0.5647(3) 0.0446(17) Uani 1 1 d . . . H6B1 H -0.1795 0.9787 0.5865 0.067 Uiso 1 1 calc R . . H6B2 H -0.1133 0.9792 0.529 0.067 Uiso 1 1 calc R . . H6B3 H -0.0573 0.9959 0.5731 0.067 Uiso 1 1 calc R . . C7B C 0.1441(6) 1.0470(3) 0.5811(3) 0.056(2) Uani 1 1 d . . . H7B1 H 0.2028 1.0532 0.5516 0.084 Uiso 1 1 calc R . . H7B2 H 0.1108 1.0876 0.5951 0.084 Uiso 1 1 calc R . . H7B3 H 0.087 1.0288 0.5704 0.084 Uiso 1 1 calc R . . C8B C 0.0861(5) 0.9834(3) 0.6851(3) 0.0457(17) Uani 1 1 d . . . H8B1 H 0.1134 0.9547 0.7123 0.069 Uiso 1 1 calc R . . H8B2 H 0.0295 0.966 0.6733 0.069 Uiso 1 1 calc R . . H8B3 H 0.0536 1.0247 0.6981 0.069 Uiso 1 1 calc R . . C9B C 0.3038(6) 1.0326(3) 0.6531(3) 0.058(2) Uani 1 1 d . . . H9B1 H 0.3663 1.0377 0.6253 0.088 Uiso 1 1 calc R . . H9B2 H 0.3313 1.0071 0.6817 0.088 Uiso 1 1 calc R . . H9B3 H 0.2657 1.0741 0.6641 0.088 Uiso 1 1 calc R . . C10B C 0.4095(5) 0.8234(3) 0.5437(3) 0.0429(17) Uani 1 1 d . . . H10D H 0.4136 0.7925 0.573 0.064 Uiso 1 1 calc R . . H10E H 0.48 0.817 0.5194 0.064 Uiso 1 1 calc R . . H10F H 0.3494 0.8179 0.5271 0.064 Uiso 1 1 calc R . . C11B C 0.5062(5) 0.9124(4) 0.5918(3) 0.053(2) Uani 1 1 d . . . H11D H 0.496 0.9547 0.6037 0.079 Uiso 1 1 calc R . . H11E H 0.5726 0.906 0.5651 0.079 Uiso 1 1 calc R . . H11F H 0.5148 0.8807 0.6202 0.079 Uiso 1 1 calc R . . C12B C 0.3761(5) 0.9587(3) 0.5070(3) 0.0486(18) Uani 1 1 d . . . H12D H 0.3619 1.0025 0.5161 0.073 Uiso 1 1 calc R . . H12E H 0.3162 0.9515 0.4909 0.073 Uiso 1 1 calc R . . H12F H 0.4469 0.9506 0.4831 0.073 Uiso 1 1 calc R . . C13B C 0.3497(7) 0.8966(3) 0.7552(3) 0.060(2) Uani 1 1 d . . . H13D H 0.2688 0.9016 0.7598 0.09 Uiso 1 1 calc R . . H13E H 0.3837 0.8793 0.7224 0.09 Uiso 1 1 calc R . . H13F H 0.3708 0.9378 0.7559 0.09 Uiso 1 1 calc R . . C14B C 0.5531(5) 0.8349(4) 0.7961(3) 0.064(2) Uani 1 1 d . . . H14D H 0.5823 0.8065 0.823 0.095 Uiso 1 1 calc R . . H14E H 0.5726 0.8767 0.7964 0.095 Uiso 1 1 calc R . . H14F H 0.5853 0.8179 0.763 0.095 Uiso 1 1 calc R . . C15B C 0.3464(6) 0.8815(4) 0.8685(3) 0.054(2) Uani 1 1 d . . . H15D H 0.3712 0.8536 0.8967 0.081 Uiso 1 1 calc R . . H15E H 0.2652 0.8907 0.8748 0.081 Uiso 1 1 calc R . . H15F H 0.3755 0.921 0.866 0.081 Uiso 1 1 calc R . . C16B C 0.5638(5) 0.6724(4) 0.8087(3) 0.062(2) Uani 1 1 d . . . H16D H 0.5641 0.6659 0.7732 0.093 Uiso 1 1 calc R . . H16E H 0.5904 0.6322 0.8263 0.093 Uiso 1 1 calc R . . H16F H 0.6125 0.7026 0.8098 0.093 Uiso 1 1 calc R . . C17B C 0.4259(7) 0.7153(4) 0.9076(3) 0.070(2) Uani 1 1 d . . . H17D H 0.3515 0.7319 0.9259 0.105 Uiso 1 1 calc R . . H17E H 0.4756 0.7453 0.9077 0.105 Uiso 1 1 calc R . . H17F H 0.4539 0.6748 0.9245 0.105 Uiso 1 1 calc R . . C18B C 0.3380(6) 0.6397(3) 0.8418(3) 0.0522(19) Uani 1 1 d . . . H18D H 0.2608 0.6536 0.8582 0.078 Uiso 1 1 calc R . . H18E H 0.3699 0.602 0.8609 0.078 Uiso 1 1 calc R . . H18F H 0.3404 0.6298 0.8069 0.078 Uiso 1 1 calc R . . C19B C 0.0637(6) 0.8593(3) 0.8467(3) 0.0508(19) Uani 1 1 d . . . H19D H 0.1441 0.8531 0.8342 0.076 Uiso 1 1 calc R . . H19E H 0.043 0.8913 0.8717 0.076 Uiso 1 1 calc R . . H19F H 0.0252 0.8734 0.8182 0.076 Uiso 1 1 calc R . . C20B C 0.0920(7) 0.7629(4) 0.9341(3) 0.066(2) Uani 1 1 d . . . H20D H 0.0732 0.723 0.9514 0.099 Uiso 1 1 calc R . . H20E H 0.066 0.7965 0.9575 0.099 Uiso 1 1 calc R . . H20F H 0.1726 0.7585 0.923 0.099 Uiso 1 1 calc R . . C21B C -0.1308(6) 0.7985(4) 0.9007(3) 0.063(2) Uani 1 1 d . . . H21D H -0.155 0.7595 0.9171 0.095 Uiso 1 1 calc R . . H21E H -0.1682 0.8132 0.8719 0.095 Uiso 1 1 calc R . . H21F H -0.1496 0.8308 0.9254 0.095 Uiso 1 1 calc R . . C22B C 0.0903(6) 0.6029(4) 0.7917(3) 0.064(2) Uani 1 1 d . . . H22D H 0.0958 0.6228 0.7571 0.096 Uiso 1 1 calc R . . H22E H 0.0531 0.5663 0.7946 0.096 Uiso 1 1 calc R . . H22F H 0.1649 0.5891 0.7994 0.096 Uiso 1 1 calc R . . C23B C -0.1351(6) 0.6796(4) 0.8241(4) 0.081(3) Uani 1 1 d . . . H23D H -0.1336 0.7018 0.7903 0.121 Uiso 1 1 calc R . . H23E H -0.1832 0.7064 0.8498 0.121 Uiso 1 1 calc R . . H23F H -0.1638 0.6403 0.825 0.121 Uiso 1 1 calc R . . C24B C 0.0022(7) 0.6188(4) 0.9027(3) 0.065(2) Uani 1 1 d . . . H24D H 0.0769 0.6085 0.9106 0.097 Uiso 1 1 calc R . . H24E H -0.0273 0.5798 0.9033 0.097 Uiso 1 1 calc R . . H24F H -0.0462 0.6459 0.928 0.097 Uiso 1 1 calc R . . C25B C 0.6190(6) 0.6032(3) 0.6833(3) 0.058(2) Uani 1 1 d . . . H25D H 0.5528 0.5929 0.7068 0.087 Uiso 1 1 calc R . . H25E H 0.6693 0.6154 0.7026 0.087 Uiso 1 1 calc R . . H25F H 0.6568 0.5662 0.6648 0.087 Uiso 1 1 calc R . . C26B C 0.5175(5) 0.7420(3) 0.6729(3) 0.0448(17) Uani 1 1 d . . . H26D H 0.4485 0.7353 0.696 0.067 Uiso 1 1 calc R . . H26E H 0.5019 0.7783 0.6487 0.067 Uiso 1 1 calc R . . H26F H 0.5706 0.7501 0.6926 0.067 Uiso 1 1 calc R . . C27B C 0.7075(6) 0.6867(4) 0.5939(3) 0.070(3) Uani 1 1 d . . . H27D H 0.6892 0.7215 0.569 0.105 Uiso 1 1 calc R . . H27E H 0.7445 0.649 0.5761 0.105 Uiso 1 1 calc R . . H27F H 0.757 0.6983 0.6139 0.105 Uiso 1 1 calc R . . C28B C 0.5964(5) 0.5418(3) 0.5482(3) 0.0470(18) Uani 1 1 d . . . H28D H 0.5575 0.5151 0.575 0.07 Uiso 1 1 calc R . . H28E H 0.6696 0.5432 0.5554 0.07 Uiso 1 1 calc R . . H28F H 0.6052 0.5242 0.5153 0.07 Uiso 1 1 calc R . . C29B C 0.3810(5) 0.6228(3) 0.5245(3) 0.0443(17) Uani 1 1 d . . . H29D H 0.3383 0.6657 0.5236 0.066 Uiso 1 1 calc R . . H29E H 0.3376 0.595 0.5482 0.066 Uiso 1 1 calc R . . H29F H 0.3975 0.6074 0.4904 0.066 Uiso 1 1 calc R . . C30B C 0.5922(5) 0.6715(3) 0.4945(3) 0.0463(18) Uani 1 1 d . . . H30D H 0.5513 0.7148 0.4925 0.07 Uiso 1 1 calc R . . H30E H 0.6005 0.6531 0.4619 0.07 Uiso 1 1 calc R . . H30F H 0.6656 0.6719 0.5019 0.07 Uiso 1 1 calc R . . C31B C 0.0612(5) 0.6753(3) 0.5774(3) 0.0423(17) Uani 1 1 d . . . H31D H 0.1252 0.678 0.5499 0.063 Uiso 1 1 calc R . . H31E H 0.0536 0.7088 0.6003 0.063 Uiso 1 1 calc R . . H31F H -0.0062 0.6802 0.563 0.063 Uiso 1 1 calc R . . C32B C -0.0419(5) 0.5943(4) 0.6658(3) 0.052(2) Uani 1 1 d . . . H32D H -0.0334 0.5536 0.6856 0.079 Uiso 1 1 calc R . . H32E H -0.1088 0.5998 0.6509 0.079 Uiso 1 1 calc R . . H32F H -0.0487 0.6284 0.6881 0.079 Uiso 1 1 calc R . . C33B C 0.0833(6) 0.5355(3) 0.5695(3) 0.054(2) Uani 1 1 d . . . H33D H 0.0936 0.4936 0.5875 0.081 Uiso 1 1 calc R . . H33E H 0.1443 0.5377 0.5404 0.081 Uiso 1 1 calc R . . H33F H 0.0127 0.5432 0.5575 0.081 Uiso 1 1 calc R . . C34B C 0.3326(5) 0.4583(3) 0.6080(3) 0.0449(17) Uani 1 1 d . . . H34D H 0.3855 0.4796 0.5833 0.067 Uiso 1 1 calc R . . H34E H 0.2766 0.4483 0.5909 0.067 Uiso 1 1 calc R . . H34F H 0.372 0.4193 0.6226 0.067 Uiso 1 1 calc R . . C35B C 0.1647(5) 0.4680(3) 0.7048(2) 0.0408(16) Uani 1 1 d . . . H35D H 0.1265 0.4943 0.7327 0.061 Uiso 1 1 calc R . . H35E H 0.2054 0.4288 0.7186 0.061 Uiso 1 1 calc R . . H35F H 0.1101 0.4579 0.6868 0.061 Uiso 1 1 calc R . . C36B C 0.3750(5) 0.5232(3) 0.6936(2) 0.0369(15) Uani 1 1 d . . . H36D H 0.3423 0.551 0.7212 0.055 Uiso 1 1 calc R . . H36E H 0.4316 0.5425 0.6695 0.055 Uiso 1 1 calc R . . H36F H 0.4093 0.4824 0.7078 0.055 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 0.02202(16) 0.02032(18) 0.02260(18) 0.00266(14) -0.00537(13) -0.00483(12) Ce2 0.02649(17) 0.02538(19) 0.01833(18) -0.00045(14) -0.00416(13) -0.00375(13) Ce3 0.02197(16) 0.02089(18) 0.02245(18) -0.00236(14) -0.00472(13) -0.00286(13) Si1 0.0274(9) 0.0272(10) 0.0389(11) -0.0072(8) -0.0078(7) -0.0010(7) Si2 0.0252(8) 0.0277(9) 0.0308(10) -0.0014(7) -0.0086(7) -0.0055(7) Si3 0.0369(10) 0.0361(11) 0.0300(10) 0.0093(8) -0.0060(8) -0.0154(8) Si4 0.0386(10) 0.0290(10) 0.0378(11) 0.0015(8) -0.0091(8) -0.0147(7) Si5 0.0251(9) 0.0475(12) 0.0357(11) -0.0061(9) -0.0046(7) -0.0029(8) Si6 0.0304(9) 0.0407(11) 0.0294(10) -0.0115(8) -0.0048(7) -0.0039(7) Si7 0.0287(9) 0.0322(10) 0.0354(11) -0.0045(8) 0.0005(7) -0.0035(7) Si8 0.0353(9) 0.0321(10) 0.0266(10) 0.0053(8) -0.0052(7) -0.0024(7) Si9 0.0289(9) 0.0323(10) 0.0304(10) -0.0017(8) -0.0040(7) -0.0089(7) Si10 0.0280(9) 0.0293(10) 0.0286(10) -0.0008(8) -0.0040(7) 0.0030(7) Si11 0.0298(9) 0.0339(10) 0.0299(10) 0.0000(8) -0.0025(7) -0.0110(7) Si12 0.0305(9) 0.0310(10) 0.0278(10) -0.0066(8) -0.0043(7) -0.0066(7) O1 0.032(2) 0.029(2) 0.025(2) -0.0036(18) -0.0073(17) -0.0021(17) O2 0.031(2) 0.028(2) 0.023(2) -0.0021(18) -0.0060(17) -0.0029(17) O3 0.027(2) 0.026(2) 0.026(2) -0.0007(18) -0.0048(17) -0.0009(16) N1 0.022(2) 0.024(3) 0.023(3) -0.002(2) -0.0054(19) -0.0047(19) N2 0.031(3) 0.028(3) 0.028(3) 0.002(2) -0.005(2) -0.013(2) N3 0.028(3) 0.033(3) 0.021(3) 0.003(2) -0.004(2) -0.003(2) N4 0.026(2) 0.026(3) 0.019(3) 0.000(2) -0.0021(19) -0.003(2) N5 0.029(3) 0.025(3) 0.025(3) -0.006(2) -0.006(2) -0.006(2) N6 0.028(2) 0.017(3) 0.027(3) 0.001(2) -0.006(2) -0.0077(19) C1 0.039(4) 0.036(4) 0.038(4) -0.013(3) -0.012(3) 0.001(3) C2 0.041(4) 0.041(4) 0.085(6) -0.026(4) 0.006(4) -0.004(3) C3 0.063(5) 0.036(4) 0.059(5) -0.004(4) -0.030(4) 0.004(3) C4 0.032(3) 0.049(4) 0.047(4) -0.006(3) -0.003(3) -0.014(3) C5 0.038(3) 0.029(4) 0.034(4) -0.004(3) -0.012(3) -0.008(3) C6 0.038(4) 0.044(4) 0.050(5) -0.006(3) -0.025(3) -0.003(3) C7 0.063(5) 0.048(5) 0.053(5) 0.026(4) -0.023(4) -0.020(4) C8 0.052(4) 0.064(5) 0.030(4) 0.017(4) -0.001(3) -0.025(4) C9 0.052(4) 0.055(5) 0.026(4) 0.003(3) -0.001(3) -0.026(3) C10 0.064(5) 0.037(4) 0.052(5) -0.004(4) -0.010(4) -0.018(3) C11 0.041(4) 0.047(5) 0.075(6) -0.009(4) -0.012(4) -0.024(3) C12 0.066(5) 0.060(5) 0.041(5) 0.004(4) -0.022(4) -0.034(4) C13 0.044(4) 0.093(7) 0.065(6) -0.009(5) -0.027(4) 0.006(4) C14 0.031(4) 0.054(5) 0.057(5) -0.010(4) 0.004(3) 0.003(3) C15 0.042(4) 0.061(5) 0.066(6) -0.008(4) 0.010(4) -0.020(4) C16 0.057(5) 0.071(6) 0.029(4) -0.008(4) 0.002(3) -0.004(4) C17 0.035(4) 0.042(4) 0.041(4) -0.012(3) 0.001(3) -0.008(3) C18 0.040(4) 0.053(5) 0.069(6) -0.027(4) -0.008(4) -0.010(3) C19 0.056(4) 0.048(5) 0.041(5) -0.008(4) 0.009(3) -0.004(3) C20 0.030(4) 0.056(5) 0.073(6) -0.008(4) -0.004(3) -0.012(3) C21 0.034(4) 0.053(5) 0.046(5) -0.006(4) -0.009(3) -0.002(3) C22 0.061(5) 0.059(5) 0.025(4) 0.014(3) -0.008(3) -0.012(4) C23 0.071(5) 0.027(4) 0.059(5) 0.008(4) -0.019(4) -0.003(3) C24 0.040(4) 0.046(4) 0.050(5) 0.018(4) -0.006(3) 0.002(3) C25 0.042(4) 0.044(4) 0.056(5) -0.006(4) -0.004(3) -0.014(3) C26 0.037(4) 0.040(4) 0.085(6) -0.006(4) 0.009(4) -0.012(3) C27 0.075(5) 0.069(6) 0.039(5) 0.018(4) -0.019(4) -0.041(4) C28 0.038(4) 0.032(4) 0.035(4) 0.002(3) -0.010(3) 0.003(3) C29 0.034(4) 0.069(5) 0.053(5) 0.009(4) -0.019(3) 0.006(3) C30 0.062(5) 0.037(4) 0.042(5) -0.003(3) 0.005(3) -0.001(3) C31 0.066(5) 0.049(5) 0.037(4) 0.015(4) 0.003(3) -0.017(4) C32 0.042(4) 0.050(5) 0.039(4) -0.009(3) 0.003(3) -0.013(3) C33 0.046(4) 0.071(6) 0.049(5) -0.003(4) -0.007(3) -0.030(4) C34 0.071(5) 0.037(4) 0.044(5) -0.012(4) -0.002(4) -0.007(3) C35 0.049(4) 0.070(6) 0.048(5) -0.030(4) -0.014(3) 0.000(4) C36 0.052(4) 0.065(5) 0.031(4) -0.004(4) 0.003(3) -0.031(4) Ce1B 0.02286(17) 0.02093(18) 0.02201(18) 0.00263(14) -0.00605(13) -0.00382(13) Ce2B 0.03052(18) 0.02255(18) 0.01848(18) 0.00030(14) -0.00654(13) -0.00444(13) Ce3B 0.02484(17) 0.02081(18) 0.02215(18) -0.00220(14) -0.00323(13) -0.00348(13) Si1B 0.0250(9) 0.0440(11) 0.0264(10) 0.0009(8) -0.0039(7) -0.0037(7) Si2B 0.0269(8) 0.0324(10) 0.0238(9) 0.0003(7) -0.0072(7) -0.0008(7) Si3B 0.0492(11) 0.0237(10) 0.0327(11) 0.0022(8) -0.0093(8) -0.0093(8) Si4B 0.0278(9) 0.0366(10) 0.0326(10) 0.0095(8) -0.0052(7) -0.0086(7) Si5B 0.0488(11) 0.0377(11) 0.0293(10) -0.0034(8) -0.0064(8) -0.0200(8) Si6B 0.0402(10) 0.0446(12) 0.0323(11) 0.0054(9) -0.0157(8) -0.0052(8) Si7B 0.0461(11) 0.0350(11) 0.0282(10) -0.0050(8) -0.0027(8) -0.0002(8) Si8B 0.0422(10) 0.0353(11) 0.0367(11) 0.0038(9) -0.0018(8) -0.0158(8) Si9B 0.0280(9) 0.0410(11) 0.0352(11) -0.0064(8) -0.0062(7) -0.0082(7) Si1A 0.0342(9) 0.0302(10) 0.0250(10) -0.0039(8) -0.0019(7) -0.0024(7) Si2A 0.0340(9) 0.0354(10) 0.0336(11) 0.0028(8) -0.0127(8) -0.0116(7) Si3A 0.0392(9) 0.0233(9) 0.0250(9) -0.0017(7) -0.0062(7) -0.0066(7) O1B 0.039(2) 0.025(2) 0.027(2) -0.0012(18) -0.0078(18) -0.0015(17) O2B 0.032(2) 0.028(2) 0.020(2) 0.0000(18) -0.0054(17) -0.0023(17) O3B 0.027(2) 0.025(2) 0.027(2) -0.0014(18) -0.0053(16) -0.0037(16) N1B 0.021(2) 0.035(3) 0.018(3) 0.001(2) -0.0044(19) -0.005(2) N2B 0.030(3) 0.023(3) 0.021(3) 0.006(2) -0.006(2) -0.010(2) N3B 0.033(3) 0.027(3) 0.024(3) -0.001(2) -0.009(2) -0.006(2) N4B 0.037(3) 0.025(3) 0.020(3) 0.006(2) -0.006(2) -0.010(2) N5B 0.029(3) 0.025(3) 0.022(3) 0.000(2) -0.002(2) -0.004(2) N6B 0.034(3) 0.025(3) 0.021(3) -0.001(2) -0.004(2) -0.006(2) C1B 0.046(4) 0.117(8) 0.037(5) -0.005(5) 0.002(3) -0.029(4) C2B 0.116(7) 0.070(7) 0.077(7) -0.007(5) 0.027(6) -0.055(6) C3B 0.041(5) 0.154(10) 0.054(6) 0.036(6) 0.009(4) 0.026(5) C4B 0.036(3) 0.048(4) 0.019(3) 0.001(3) -0.006(3) -0.001(3) C5B 0.039(4) 0.056(5) 0.038(4) -0.003(3) -0.017(3) -0.006(3) C6B 0.050(4) 0.044(4) 0.039(4) 0.002(3) -0.015(3) 0.000(3) C7B 0.070(5) 0.037(4) 0.057(5) 0.008(4) -0.012(4) -0.001(4) C8B 0.057(4) 0.037(4) 0.041(4) -0.005(3) -0.005(3) -0.004(3) C9B 0.077(5) 0.040(5) 0.066(6) -0.007(4) -0.014(4) -0.028(4) C10B 0.037(4) 0.043(4) 0.046(4) -0.004(3) 0.000(3) -0.007(3) C11B 0.036(4) 0.063(5) 0.059(5) 0.012(4) -0.010(3) -0.016(3) C12B 0.044(4) 0.053(5) 0.043(5) 0.018(4) -0.004(3) -0.012(3) C13B 0.102(6) 0.040(5) 0.050(5) 0.009(4) -0.030(4) -0.032(4) C14B 0.051(4) 0.078(6) 0.067(6) -0.015(5) 0.004(4) -0.036(4) C15B 0.068(5) 0.054(5) 0.046(5) -0.013(4) -0.010(4) -0.022(4) C16B 0.050(5) 0.072(6) 0.059(6) 0.000(4) -0.020(4) 0.008(4) C17B 0.091(6) 0.088(7) 0.034(5) 0.014(4) -0.026(4) -0.018(5) C18B 0.055(4) 0.037(4) 0.063(5) 0.014(4) -0.022(4) -0.004(3) C19B 0.063(5) 0.038(4) 0.054(5) -0.006(4) -0.013(4) -0.011(3) C20B 0.086(6) 0.067(6) 0.042(5) -0.010(4) -0.021(4) 0.005(4) C21B 0.059(5) 0.048(5) 0.067(6) -0.007(4) 0.013(4) 0.008(4) C22B 0.072(5) 0.049(5) 0.073(6) -0.017(4) 0.005(4) -0.030(4) C23B 0.060(5) 0.091(7) 0.105(8) -0.011(6) -0.026(5) -0.032(5) C24B 0.098(6) 0.045(5) 0.047(5) 0.018(4) -0.005(4) -0.025(4) C25B 0.056(5) 0.050(5) 0.074(6) -0.006(4) -0.040(4) 0.009(4) C26B 0.057(4) 0.043(4) 0.042(4) -0.001(3) -0.017(3) -0.019(3) C27B 0.047(4) 0.119(8) 0.053(5) -0.016(5) 0.002(4) -0.041(5) C28B 0.058(4) 0.041(4) 0.037(4) -0.010(3) -0.003(3) 0.002(3) C29B 0.055(4) 0.051(5) 0.029(4) -0.010(3) -0.011(3) -0.009(3) C30B 0.055(4) 0.045(4) 0.034(4) -0.002(3) 0.006(3) -0.011(3) C31B 0.037(4) 0.039(4) 0.054(5) 0.008(3) -0.019(3) -0.008(3) C32B 0.032(4) 0.063(5) 0.056(5) 0.015(4) -0.005(3) -0.008(3) C33B 0.067(5) 0.057(5) 0.052(5) -0.006(4) -0.028(4) -0.025(4) C34B 0.057(4) 0.029(4) 0.045(4) -0.008(3) -0.008(3) 0.002(3) C35B 0.051(4) 0.037(4) 0.037(4) 0.005(3) -0.012(3) -0.017(3) C36B 0.039(4) 0.029(4) 0.043(4) 0.002(3) -0.018(3) 0.001(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O1 2.094(4) . ? Ce1 O3 2.108(4) . ? Ce1 N1 2.258(4) . ? Ce1 N2 2.273(4) . ? Ce2 O2 2.079(4) . ? Ce2 O1 2.096(4) . ? Ce2 N3 2.259(5) . ? Ce2 N4 2.274(4) . ? Ce3 O3 2.071(4) . ? Ce3 O2 2.110(4) . ? Ce3 N5 2.246(4) . ? Ce3 N6 2.275(4) . ? Si1 N1 1.729(5) . ? Si1 C2 1.859(7) . ? Si1 C3 1.865(7) . ? Si1 C1 1.867(6) . ? Si2 N1 1.742(4) . ? Si2 C5 1.862(6) . ? Si2 C6 1.867(6) . ? Si2 C4 1.884(6) . ? Si3 N2 1.726(5) . ? Si3 C8 1.859(6) . ? Si3 C7 1.875(7) . ? Si3 C9 1.879(6) . ? Si4 N2 1.742(5) . ? Si4 C12 1.871(7) . ? Si4 C11 1.872(6) . ? Si4 C10 1.878(7) . ? Si5 N3 1.736(5) . ? Si5 C13 1.861(7) . ? Si5 C15 1.871(7) . ? Si5 C14 1.874(7) . ? Si6 N3 1.731(5) . ? Si6 C16 1.861(7) . ? Si6 C18 1.874(7) . ? Si6 C17 1.875(6) . ? Si7 N4 1.740(4) . ? Si7 C21 1.869(7) . ? Si7 C20 1.876(7) . ? Si7 C19 1.877(7) . ? Si8 N4 1.730(5) . ? Si8 C23 1.860(7) . ? Si8 C22 1.866(7) . ? Si8 C24 1.878(6) . ? Si9 N5 1.744(5) . ? Si9 C25 1.857(7) . ? Si9 C27 1.863(7) . ? Si9 C26 1.872(6) . ? Si10 N5 1.725(5) . ? Si10 C30 1.863(6) . ? Si10 C29 1.864(6) . ? Si10 C28 1.871(6) . ? Si11 N6 1.734(5) . ? Si11 C31 1.860(7) . ? Si11 C33 1.861(6) . ? Si11 C32 1.881(6) . ? Si12 N6 1.726(5) . ? Si12 C34 1.856(7) . ? Si12 C35 1.860(6) . ? Si12 C36 1.868(6) . ? Ce1B O3B 2.087(4) . ? Ce1B O1B 2.095(4) . ? Ce1B N1B 2.257(4) . ? Ce1B N2B 2.271(4) . ? Ce2B O1B 2.089(4) . ? Ce2B O2B 2.092(4) . ? Ce2B N4B 2.265(5) . ? Ce2B N3B 2.267(4) . ? Ce3B O3B 2.085(4) . ? Ce3B O2B 2.102(4) . ? Ce3B N6B 2.261(5) . ? Ce3B N5B 2.266(4) . ? Si1B N1B 1.741(5) . ? Si1B C3B 1.852(7) . ? Si1B C1B 1.852(7) . ? Si1B C2B 1.860(8) . ? Si2B N1B 1.734(5) . ? Si2B C5B 1.862(6) . ? Si2B C4B 1.863(6) . ? Si2B C6B 1.865(6) . ? Si3B N2B 1.732(5) . ? Si3B C7B 1.868(7) . ? Si3B C9B 1.872(7) . ? Si3B C8B 1.880(7) . ? Si4B N2B 1.732(5) . ? Si4B C10B 1.860(6) . ? Si4B C12B 1.869(7) . ? Si4B C11B 1.869(6) . ? Si5B N3B 1.736(5) . ? Si5B C13B 1.867(7) . ? Si5B C14B 1.870(7) . ? Si5B C15B 1.874(7) . ? Si6B N3B 1.733(5) . ? Si6B C17B 1.862(7) . ? Si6B C16B 1.867(7) . ? Si6B C18B 1.868(7) . ? Si7B N4B 1.734(5) . ? Si7B C20B 1.872(7) . ? Si7B C19B 1.872(7) . ? Si7B C21B 1.878(7) . ? Si8B N4B 1.731(5) . ? Si8B C23B 1.867(8) . ? Si8B C24B 1.871(7) . ? Si8B C22B 1.876(7) . ? Si9B N5B 1.732(5) . ? Si9B C27B 1.865(7) . ? Si9B C25B 1.868(7) . ? Si9B C26B 1.874(7) . ? Si1A N5B 1.738(5) . ? Si1A C30B 1.870(7) . ? Si1A C28B 1.871(6) . ? Si1A C29B 1.874(6) . ? Si2A N6B 1.746(5) . ? Si2A C31B 1.867(6) . ? Si2A C32B 1.869(7) . ? Si2A C33B 1.873(7) . ? Si3A N6B 1.730(5) . ? Si3A C35B 1.858(6) . ? Si3A C34B 1.868(6) . ? Si3A C36B 1.884(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ce1 O3 94.88(14) . . ? O1 Ce1 N1 107.39(15) . . ? O3 Ce1 N1 112.32(14) . . ? O1 Ce1 N2 116.08(16) . . ? O3 Ce1 N2 107.58(15) . . ? N1 Ce1 N2 116.58(16) . . ? O2 Ce2 O1 95.57(14) . . ? O2 Ce2 N3 115.53(15) . . ? O1 Ce2 N3 107.60(16) . . ? O2 Ce2 N4 109.28(15) . . ? O1 Ce2 N4 117.83(15) . . ? N3 Ce2 N4 110.54(16) . . ? O3 Ce3 O2 97.00(14) . . ? O3 Ce3 N5 107.55(16) . . ? O2 Ce3 N5 106.14(15) . . ? O3 Ce3 N6 107.12(15) . . ? O2 Ce3 N6 116.09(15) . . ? N5 Ce3 N6 120.18(15) . . ? N1 Si1 C2 114.2(3) . . ? N1 Si1 C3 111.9(3) . . ? C2 Si1 C3 108.4(4) . . ? N1 Si1 C1 106.8(2) . . ? C2 Si1 C1 107.4(3) . . ? C3 Si1 C1 107.8(3) . . ? C2 Si1 Ce1 133.7(3) . . ? C3 Si1 Ce1 116.7(2) . . ? C1 Si1 Ce1 68.57(18) . . ? N1 Si2 C5 111.0(2) . . ? N1 Si2 C6 111.8(3) . . ? C5 Si2 C6 106.8(3) . . ? N1 Si2 C4 111.6(3) . . ? C5 Si2 C4 107.3(3) . . ? C6 Si2 C4 108.0(3) . . ? N2 Si3 C8 113.4(3) . . ? N2 Si3 C7 114.2(3) . . ? C8 Si3 C7 107.8(3) . . ? N2 Si3 C9 107.9(3) . . ? C8 Si3 C9 106.6(3) . . ? C7 Si3 C9 106.4(3) . . ? C8 Si3 Ce1 126.5(2) . . ? C7 Si3 Ce1 125.0(2) . . ? C9 Si3 Ce1 68.4(2) . . ? N2 Si4 C12 110.1(3) . . ? N2 Si4 C11 114.0(3) . . ? C12 Si4 C11 106.6(3) . . ? N2 Si4 C10 112.6(3) . . ? C12 Si4 C10 106.7(3) . . ? C11 Si4 C10 106.5(3) . . ? N3 Si5 C13 112.0(3) . . ? N3 Si5 C15 112.4(3) . . ? C13 Si5 C15 107.7(4) . . ? N3 Si5 C14 111.1(3) . . ? C13 Si5 C14 106.7(4) . . ? C15 Si5 C14 106.6(3) . . ? N3 Si6 C16 111.2(3) . . ? N3 Si6 C18 114.5(3) . . ? C16 Si6 C18 108.7(4) . . ? N3 Si6 C17 108.2(3) . . ? C16 Si6 C17 107.7(3) . . ? C18 Si6 C17 106.2(3) . . ? C16 Si6 Ce2 107.2(2) . . ? C18 Si6 Ce2 142.0(3) . . ? C17 Si6 Ce2 73.84(19) . . ? N4 Si7 C21 110.2(3) . . ? N4 Si7 C20 113.0(3) . . ? C21 Si7 C20 107.2(3) . . ? N4 Si7 C19 112.1(3) . . ? C21 Si7 C19 108.9(3) . . ? C20 Si7 C19 105.2(3) . . ? N4 Si8 C23 114.0(3) . . ? N4 Si8 C22 113.9(3) . . ? C23 Si8 C22 106.9(3) . . ? N4 Si8 C24 107.9(3) . . ? C23 Si8 C24 106.2(3) . . ? C22 Si8 C24 107.5(3) . . ? C23 Si8 Ce2 117.3(2) . . ? C22 Si8 Ce2 134.6(2) . . ? C24 Si8 Ce2 70.3(2) . . ? N5 Si9 C25 109.5(3) . . ? N5 Si9 C27 111.1(3) . . ? C25 Si9 C27 107.8(4) . . ? N5 Si9 C26 113.7(3) . . ? C25 Si9 C26 107.9(3) . . ? C27 Si9 C26 106.6(4) . . ? N5 Si10 C30 112.4(3) . . ? N5 Si10 C29 114.9(3) . . ? C30 Si10 C29 108.2(3) . . ? N5 Si10 C28 106.6(2) . . ? C30 Si10 C28 108.3(3) . . ? C29 Si10 C28 106.0(3) . . ? C30 Si10 Ce3 122.7(2) . . ? C29 Si10 Ce3 128.5(2) . . ? C28 Si10 Ce3 67.05(18) . . ? N6 Si11 C31 111.2(3) . . ? N6 Si11 C33 114.4(3) . . ? C31 Si11 C33 107.8(3) . . ? N6 Si11 C32 108.2(3) . . ? C31 Si11 C32 108.7(3) . . ? C33 Si11 C32 106.3(3) . . ? C31 Si11 Ce3 109.1(2) . . ? C33 Si11 Ce3 139.7(2) . . ? C32 Si11 Ce3 76.2(2) . . ? N6 Si12 C34 112.1(3) . . ? N6 Si12 C35 116.0(3) . . ? C34 Si12 C35 106.8(3) . . ? N6 Si12 C36 107.2(3) . . ? C34 Si12 C36 109.4(3) . . ? C35 Si12 C36 105.0(3) . . ? C34 Si12 Ce3 119.9(2) . . ? C35 Si12 Ce3 131.5(2) . . ? C36 Si12 Ce3 72.6(2) . . ? Ce1 O1 Ce2 145.16(18) . . ? Ce2 O2 Ce3 142.53(19) . . ? Ce3 O3 Ce1 143.3(2) . . ? Si1 N1 Si2 120.5(2) . . ? Si1 N1 Ce1 112.2(2) . . ? Si2 N1 Ce1 127.3(2) . . ? Si3 N2 Si4 122.5(3) . . ? Si3 N2 Ce1 111.7(2) . . ? Si4 N2 Ce1 125.8(3) . . ? Si6 N3 Si5 120.0(3) . . ? Si6 N3 Ce2 113.5(2) . . ? Si5 N3 Ce2 126.4(2) . . ? Si8 N4 Si7 120.4(3) . . ? Si8 N4 Ce2 113.2(2) . . ? Si7 N4 Ce2 126.4(2) . . ? Si10 N5 Si9 124.0(3) . . ? Si10 N5 Ce3 111.0(2) . . ? Si9 N5 Ce3 125.0(2) . . ? Si12 N6 Si11 122.2(3) . . ? Si12 N6 Ce3 119.2(2) . . ? Si11 N6 Ce3 118.6(2) . . ? O3B Ce1B O1B 94.58(15) . . ? O3B Ce1B N1B 107.81(15) . . ? O1B Ce1B N1B 110.14(15) . . ? O3B Ce1B N2B 113.63(15) . . ? O1B Ce1B N2B 110.58(15) . . ? N1B Ce1B N2B 117.67(16) . . ? O1B Ce2B O2B 95.64(14) . . ? O1B Ce2B N4B 109.19(15) . . ? O2B Ce2B N4B 114.78(16) . . ? O1B Ce2B N3B 112.01(16) . . ? O2B Ce2B N3B 111.83(15) . . ? N4B Ce2B N3B 112.27(16) . . ? O3B Ce3B O2B 95.41(14) . . ? O3B Ce3B N6B 114.61(15) . . ? O2B Ce3B N6B 108.32(16) . . ? O3B Ce3B N5B 107.75(15) . . ? O2B Ce3B N5B 109.72(15) . . ? N6B Ce3B N5B 118.53(16) . . ? N1B Si1B C3B 112.8(3) . . ? N1B Si1B C1B 112.6(3) . . ? C3B Si1B C1B 106.2(4) . . ? N1B Si1B C2B 109.7(3) . . ? C3B Si1B C2B 108.0(5) . . ? C1B Si1B C2B 107.3(4) . . ? N1B Si2B C5B 114.3(3) . . ? N1B Si2B C4B 107.0(2) . . ? C5B Si2B C4B 106.6(3) . . ? N1B Si2B C6B 112.6(3) . . ? C5B Si2B C6B 108.0(3) . . ? C4B Si2B C6B 108.1(3) . . ? C5B Si2B Ce1B 131.5(2) . . ? C4B Si2B Ce1B 69.66(18) . . ? C6B Si2B Ce1B 119.3(2) . . ? N2B Si3B C7B 113.3(3) . . ? N2B Si3B C9B 114.2(3) . . ? C7B Si3B C9B 107.2(4) . . ? N2B Si3B C8B 107.5(3) . . ? C7B Si3B C8B 106.1(3) . . ? C9B Si3B C8B 108.1(3) . . ? C7B Si3B Ce1B 117.7(2) . . ? C9B Si3B Ce1B 134.1(3) . . ? C8B Si3B Ce1B 69.5(2) . . ? N2B Si4B C10B 111.7(3) . . ? N2B Si4B C12B 112.1(3) . . ? C10B Si4B C12B 105.5(3) . . ? N2B Si4B C11B 111.8(3) . . ? C10B Si4B C11B 106.3(3) . . ? C12B Si4B C11B 109.0(3) . . ? N3B Si5B C13B 110.2(3) . . ? N3B Si5B C14B 113.4(3) . . ? C13B Si5B C14B 106.8(4) . . ? N3B Si5B C15B 112.7(3) . . ? C13B Si5B C15B 108.0(4) . . ? C14B Si5B C15B 105.5(3) . . ? N3B Si6B C17B 113.9(3) . . ? N3B Si6B C16B 114.8(3) . . ? C17B Si6B C16B 106.9(4) . . ? N3B Si6B C18B 107.1(3) . . ? C17B Si6B C18B 108.2(4) . . ? C16B Si6B C18B 105.6(4) . . ? C17B Si6B Ce2B 131.9(3) . . ? C16B Si6B Ce2B 120.5(2) . . ? C18B Si6B Ce2B 68.2(2) . . ? N4B Si7B C20B 112.2(3) . . ? N4B Si7B C19B 107.4(3) . . ? C20B Si7B C19B 106.6(4) . . ? N4B Si7B C21B 115.0(3) . . ? C20B Si7B C21B 108.1(4) . . ? C19B Si7B C21B 107.2(3) . . ? C20B Si7B Ce2B 107.4(3) . . ? C19B Si7B Ce2B 73.1(2) . . ? C21B Si7B Ce2B 142.6(3) . . ? N4B Si8B C23B 112.6(3) . . ? N4B Si8B C24B 112.1(3) . . ? C23B Si8B C24B 108.3(4) . . ? N4B Si8B C22B 110.7(3) . . ? C23B Si8B C22B 106.5(4) . . ? C24B Si8B C22B 106.3(4) . . ? N5B Si9B C27B 114.1(3) . . ? N5B Si9B C25B 110.9(3) . . ? C27B Si9B C25B 107.0(4) . . ? N5B Si9B C26B 109.1(3) . . ? C27B Si9B C26B 106.8(4) . . ? C25B Si9B C26B 108.7(3) . . ? N5B Si1A C30B 116.3(3) . . ? N5B Si1A C28B 111.4(3) . . ? C30B Si1A C28B 107.4(3) . . ? N5B Si1A C29B 107.3(3) . . ? C30B Si1A C29B 104.2(3) . . ? C28B Si1A C29B 110.0(3) . . ? C30B Si1A Ce3B 132.4(2) . . ? C28B Si1A Ce3B 118.9(2) . . ? C29B Si1A Ce3B 71.2(2) . . ? N6B Si2A C31B 110.6(3) . . ? N6B Si2A C32B 111.2(3) . . ? C31B Si2A C32B 107.6(3) . . ? N6B Si2A C33B 112.6(3) . . ? C31B Si2A C33B 107.3(3) . . ? C32B Si2A C33B 107.4(3) . . ? N6B Si3A C35B 113.9(3) . . ? N6B Si3A C34B 114.2(3) . . ? C35B Si3A C34B 106.9(3) . . ? N6B Si3A C36B 106.5(3) . . ? C35B Si3A C36B 108.5(3) . . ? C34B Si3A C36B 106.6(3) . . ? C35B Si3A Ce3B 133.4(2) . . ? C34B Si3A Ce3B 118.4(2) . . ? C36B Si3A Ce3B 69.67(19) . . ? Ce2B O1B Ce1B 145.02(19) . . ? Ce2B O2B Ce3B 143.64(19) . . ? Ce3B O3B Ce1B 145.38(19) . . ? Si2B N1B Si1B 119.9(2) . . ? Si2B N1B Ce1B 114.1(2) . . ? Si1B N1B Ce1B 125.8(2) . . ? Si4B N2B Si3B 121.7(3) . . ? Si4B N2B Ce1B 125.4(2) . . ? Si3B N2B Ce1B 112.8(2) . . ? Si6B N3B Si5B 119.8(3) . . ? Si6B N3B Ce2B 111.8(2) . . ? Si5B N3B Ce2B 128.4(2) . . ? Si8B N4B Si7B 120.2(3) . . ? Si8B N4B Ce2B 125.9(2) . . ? Si7B N4B Ce2B 113.8(2) . . ? Si9B N5B Si1A 122.6(3) . . ? Si9B N5B Ce3B 121.3(2) . . ? Si1A N5B Ce3B 116.0(2) . . ? Si3A N6B Si2A 121.1(3) . . ? Si3A N6B Ce3B 114.7(2) . . ? Si2A N6B Ce3B 124.2(2) . . ? #===END data_(5)-oct1305 _database_code_depnum_ccdc_archive 'CCDC 774595' #TrackingRef '- mfl_28jul2009.CIF' _audit_creation_date 2005-10-28T11:25:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C72 H144 Ce4 N8 O4' _chemical_formula_sum 'C72 H144 Ce4 N8 O4' _chemical_formula_weight 1746.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9386(6) _cell_length_b 16.2491(8) _cell_length_c 21.5659(11) _cell_angle_alpha 88.222(3) _cell_angle_beta 82.782(2) _cell_angle_gamma 77.134(3) _cell_volume 4046.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 70639 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8895 _exptl_absorpt_correction_T_max 0.9633 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.665496E-1 _diffrn_orient_matrix_ub_12 0.268991E-1 _diffrn_orient_matrix_ub_13 -0.14045E-1 _diffrn_orient_matrix_ub_21 0.457494E-1 _diffrn_orient_matrix_ub_22 -0.344502E-1 _diffrn_orient_matrix_ub_23 0.312888E-1 _diffrn_orient_matrix_ub_31 0.311691E-1 _diffrn_orient_matrix_ub_32 -0.455484E-1 _diffrn_orient_matrix_ub_33 -0.317552E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1239 _diffrn_reflns_av_unetI/netI 0.1208 _diffrn_reflns_number 43907 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 23.03 _diffrn_reflns_theta_full 23.03 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 11209 _reflns_number_gt 6961 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There is a residual peak of about 2 electrons at the centre of the Ce4O4 square. 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^)+(0.0000P)^2^+34.4080P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11209 _refine_ls_number_parameters 793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_gt 0.067 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.07 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.023 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.149 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.23689(6) 0.76372(4) 0.38617(3) 0.0311(2) Uani 1 1 d . . . Ce2 Ce 0.16822(6) 0.93513(4) 0.23281(3) 0.0308(2) Uani 1 1 d . . . Ce3 Ce 0.30868(6) 0.72664(4) 0.10825(3) 0.0323(2) Uani 1 1 d . . . Ce4 Ce 0.27157(6) 0.55574(4) 0.26109(3) 0.0319(2) Uani 1 1 d . . . O1 O 0.2024(7) 0.8509(5) 0.3098(4) 0.041(2) Uani 1 1 d . . . O2 O 0.2384(7) 0.8294(5) 0.1719(4) 0.043(2) Uani 1 1 d . . . O3 O 0.2915(7) 0.6430(5) 0.1847(4) 0.045(2) Uani 1 1 d . . . O4 O 0.2545(7) 0.6620(5) 0.3234(4) 0.041(2) Uani 1 1 d . . . N1 N 0.0984(8) 0.7430(6) 0.4644(4) 0.038(3) Uani 1 1 d . . . N2 N 0.3954(8) 0.7924(5) 0.4220(4) 0.030(2) Uani 1 1 d . . . N3 N -0.0275(8) 0.9932(6) 0.2462(4) 0.033(2) Uani 1 1 d . . . N4 N 0.2779(8) 1.0311(6) 0.1980(4) 0.039(3) Uani 1 1 d . . . N5 N 0.1819(8) 0.7413(6) 0.0361(4) 0.041(3) Uani 1 1 d . . . N6 N 0.5014(8) 0.7058(6) 0.0731(4) 0.042(3) Uani 1 1 d . . . N7 N 0.1098(8) 0.5049(6) 0.2514(4) 0.041(3) Uani 1 1 d . . . N8 N 0.4311(8) 0.4591(6) 0.2863(4) 0.039(3) Uani 1 1 d . . . C1 C -0.0249(11) 0.7820(8) 0.4658(5) 0.042(3) Uani 1 1 d . . . C2 C -0.0974(11) 0.7156(9) 0.4637(6) 0.054(4) Uani 1 1 d . . . H2B H -0.082 0.6903 0.4215 0.064 Uiso 1 1 calc R . . H2A H -0.1805 0.7438 0.4708 0.064 Uiso 1 1 calc R . . C3 C -0.0722(13) 0.6448(10) 0.5126(7) 0.072(5) Uani 1 1 d . . . H3B H -0.097 0.6682 0.5552 0.087 Uiso 1 1 calc R . . H3A H -0.1159 0.6011 0.5066 0.087 Uiso 1 1 calc R . . C4 C 0.0564(11) 0.6060(8) 0.5049(7) 0.054(4) Uani 1 1 d . . . H4B H 0.0739 0.5633 0.5382 0.065 Uiso 1 1 calc R . . H4A H 0.0788 0.577 0.4641 0.065 Uiso 1 1 calc R . . C5 C 0.1268(12) 0.6722(7) 0.5085(6) 0.046(4) Uani 1 1 d . . . C6 C -0.0368(11) 0.8405(9) 0.4078(6) 0.064(4) Uani 1 1 d . . . H6C H -0.1184 0.868 0.4068 0.096 Uiso 1 1 calc R . . H6B H -0.008 0.8069 0.3698 0.096 Uiso 1 1 calc R . . H6A H 0.0085 0.8835 0.4101 0.096 Uiso 1 1 calc R . . C7 C -0.0725(11) 0.8413(8) 0.5229(6) 0.060(4) Uani 1 1 d . . . H7C H -0.0265 0.8842 0.5233 0.09 Uiso 1 1 calc R . . H7B H -0.0676 0.808 0.5616 0.09 Uiso 1 1 calc R . . H7A H -0.1535 0.8689 0.5199 0.09 Uiso 1 1 calc R . . C8 C 0.2556(11) 0.6294(8) 0.4898(6) 0.052(4) Uani 1 1 d . . . H8C H 0.2792 0.5831 0.5189 0.078 Uiso 1 1 calc R . . H8B H 0.3034 0.6709 0.4913 0.078 Uiso 1 1 calc R . . H8A H 0.2656 0.607 0.4473 0.078 Uiso 1 1 calc R . . C9 C 0.1192(13) 0.7010(9) 0.5777(6) 0.068(4) Uani 1 1 d . . . H9C H 0.0382 0.7246 0.5937 0.101 Uiso 1 1 calc R . . H9B H 0.1645 0.7442 0.5794 0.101 Uiso 1 1 calc R . . H9A H 0.1502 0.6524 0.6034 0.101 Uiso 1 1 calc R . . C10 C 0.3798(11) 0.8581(7) 0.4690(6) 0.039(3) Uani 1 1 d . . . C11 C 0.4569(12) 0.9206(8) 0.4487(7) 0.056(4) Uani 1 1 d . . . H11B H 0.4277 0.9535 0.4124 0.067 Uiso 1 1 calc R . . H11A H 0.451 0.9607 0.4832 0.067 Uiso 1 1 calc R . . C12 C 0.5814(12) 0.8788(9) 0.4314(6) 0.056(4) Uani 1 1 d . . . H12B H 0.6257 0.922 0.4167 0.068 Uiso 1 1 calc R . . H12A H 0.6137 0.8506 0.4686 0.068 Uiso 1 1 calc R . . C13 C 0.5936(11) 0.8153(8) 0.3810(6) 0.049(4) Uani 1 1 d . . . H13B H 0.6755 0.7847 0.3731 0.059 Uiso 1 1 calc R . . H13A H 0.5721 0.8449 0.342 0.059 Uiso 1 1 calc R . . C14 C 0.5160(10) 0.7505(8) 0.3986(5) 0.038(3) Uani 1 1 d . . . C15 C 0.2520(11) 0.9072(8) 0.4737(6) 0.055(4) Uani 1 1 d . . . H15C H 0.2011 0.8693 0.489 0.083 Uiso 1 1 calc R . . H15B H 0.2341 0.9289 0.4323 0.083 Uiso 1 1 calc R . . H15A H 0.2399 0.9544 0.5028 0.083 Uiso 1 1 calc R . . C16 C 0.3996(12) 0.8270(9) 0.5341(6) 0.060(4) Uani 1 1 d . . . H16C H 0.3852 0.8753 0.5623 0.09 Uiso 1 1 calc R . . H16B H 0.4798 0.7954 0.5339 0.09 Uiso 1 1 calc R . . H16A H 0.3468 0.7901 0.5484 0.09 Uiso 1 1 calc R . . C17 C 0.5132(11) 0.7035(8) 0.3380(6) 0.052(4) Uani 1 1 d . . . H17C H 0.5925 0.6777 0.3203 0.078 Uiso 1 1 calc R . . H17B H 0.4762 0.7435 0.3078 0.078 Uiso 1 1 calc R . . H17A H 0.4693 0.6595 0.3474 0.078 Uiso 1 1 calc R . . C18 C 0.5752(11) 0.6827(8) 0.4430(6) 0.058(4) Uani 1 1 d . . . H18C H 0.5301 0.6391 0.4507 0.088 Uiso 1 1 calc R . . H18B H 0.5794 0.709 0.4826 0.088 Uiso 1 1 calc R . . H18A H 0.6535 0.6571 0.4237 0.088 Uiso 1 1 calc R . . C19 C -0.0702(10) 1.0719(8) 0.2822(5) 0.039(3) Uani 1 1 d . . . C20 C -0.1725(11) 1.0656(8) 0.3313(6) 0.050(4) Uani 1 1 d . . . H20B H -0.1442 1.0272 0.3652 0.06 Uiso 1 1 calc R . . H20A H -0.2067 1.122 0.3497 0.06 Uiso 1 1 calc R . . C21 C -0.2641(11) 1.0335(9) 0.3041(6) 0.051(4) Uani 1 1 d . . . H21B H -0.2975 1.0742 0.2726 0.061 Uiso 1 1 calc R . . H21A H -0.3271 1.0283 0.3375 0.061 Uiso 1 1 calc R . . C22 C -0.2135(11) 0.9480(8) 0.2735(6) 0.050(4) Uani 1 1 d . . . H22B H -0.185 0.9065 0.3057 0.06 Uiso 1 1 calc R . . H22A H -0.275 0.9283 0.2553 0.06 Uiso 1 1 calc R . . C23 C -0.1147(10) 0.9521(7) 0.2226(5) 0.030(3) Uani 1 1 d . . . C24 C 0.0296(11) 1.0860(8) 0.3154(6) 0.053(4) Uani 1 1 d . . . H24C H 0.0051 1.1388 0.3392 0.08 Uiso 1 1 calc R . . H24B H 0.0959 1.0894 0.2844 0.08 Uiso 1 1 calc R . . H24A H 0.0519 1.0388 0.3441 0.08 Uiso 1 1 calc R . . C25 C -0.1026(11) 1.1505(8) 0.2416(6) 0.056(4) Uani 1 1 d . . . H25C H -0.1704 1.1473 0.2213 0.083 Uiso 1 1 calc R . . H25B H -0.0375 1.1536 0.2097 0.083 Uiso 1 1 calc R . . H25A H -0.1207 1.201 0.2679 0.083 Uiso 1 1 calc R . . C26 C -0.0508(11) 0.8609(8) 0.2044(6) 0.055(4) Uani 1 1 d . . . H26C H -0.0203 0.8313 0.2411 0.083 Uiso 1 1 calc R . . H26B H 0.0132 0.8624 0.1714 0.083 Uiso 1 1 calc R . . H26A H -0.1049 0.8312 0.1891 0.083 Uiso 1 1 calc R . . C27 C -0.1584(10) 0.9932(8) 0.1627(5) 0.046(4) Uani 1 1 d . . . H27C H -0.2079 0.9601 0.1468 0.07 Uiso 1 1 calc R . . H27B H -0.0923 0.995 0.1312 0.07 Uiso 1 1 calc R . . H27A H -0.203 1.0507 0.1718 0.07 Uiso 1 1 calc R . . C28 C 0.3788(10) 1.0425(8) 0.2259(6) 0.042(3) Uani 1 1 d . . . C29 C 0.4894(11) 1.0199(8) 0.1816(7) 0.057(4) Uani 1 1 d . . . H29B H 0.5109 0.9579 0.1758 0.068 Uiso 1 1 calc R . . H29A H 0.5524 1.0369 0.2003 0.068 Uiso 1 1 calc R . . C30 C 0.4781(11) 1.0626(9) 0.1181(7) 0.066(5) Uani 1 1 d . . . H30B H 0.5495 1.0418 0.0892 0.079 Uiso 1 1 calc R . . H30A H 0.4677 1.1244 0.1226 0.079 Uiso 1 1 calc R . . C31 C 0.3732(10) 1.0433(9) 0.0908(6) 0.054(4) Uani 1 1 d . . . H31B H 0.3639 1.074 0.0507 0.064 Uiso 1 1 calc R . . H31A H 0.388 0.9821 0.0821 0.064 Uiso 1 1 calc R . . C32 C 0.2615(10) 1.0689(8) 0.1353(6) 0.042(3) Uani 1 1 d . . . C33 C 0.3651(13) 1.1303(9) 0.2546(7) 0.072(5) Uani 1 1 d . . . H33C H 0.43 1.1301 0.2782 0.108 Uiso 1 1 calc R . . H33B H 0.2923 1.144 0.2826 0.108 Uiso 1 1 calc R . . H33A H 0.3641 1.1726 0.2211 0.108 Uiso 1 1 calc R . . C34 C 0.3894(12) 0.9814(9) 0.2825(6) 0.065(4) Uani 1 1 d . . . H34C H 0.401 0.9232 0.268 0.097 Uiso 1 1 calc R . . H34B H 0.3183 0.9952 0.3119 0.097 Uiso 1 1 calc R . . H34A H 0.4554 0.987 0.3035 0.097 Uiso 1 1 calc R . . C35 C 0.2211(12) 1.1673(8) 0.1370(6) 0.061(4) Uani 1 1 d . . . H35C H 0.282 1.1918 0.1505 0.091 Uiso 1 1 calc R . . H35B H 0.1504 1.1835 0.1665 0.091 Uiso 1 1 calc R . . H35A H 0.2053 1.1884 0.0952 0.091 Uiso 1 1 calc R . . C36 C 0.1674(10) 1.0346(8) 0.1102(6) 0.045(3) Uani 1 1 d . . . H36C H 0.155 1.0587 0.0688 0.068 Uiso 1 1 calc R . . H36B H 0.0953 1.0501 0.1386 0.068 Uiso 1 1 calc R . . H36A H 0.1912 0.973 0.1071 0.068 Uiso 1 1 calc R . . C37 C 0.1784(11) 0.8124(9) -0.0076(6) 0.050(4) Uani 1 1 d . . . C38 C 0.1958(14) 0.7799(9) -0.0760(6) 0.065(4) Uani 1 1 d . . . H38B H 0.1847 0.8289 -0.1048 0.078 Uiso 1 1 calc R . . H38A H 0.2761 0.747 -0.0859 0.078 Uiso 1 1 calc R . . C39 C 0.1127(15) 0.7253(10) -0.0866(7) 0.082(5) Uani 1 1 d . . . H39B H 0.1317 0.7015 -0.1293 0.098 Uiso 1 1 calc R . . H39A H 0.0326 0.7598 -0.0826 0.098 Uiso 1 1 calc R . . C40 C 0.1221(12) 0.6531(9) -0.0378(6) 0.059(4) Uani 1 1 d . . . H40B H 0.0621 0.621 -0.0422 0.071 Uiso 1 1 calc R . . H40A H 0.1986 0.614 -0.0466 0.071 Uiso 1 1 calc R . . C41 C 0.1076(11) 0.6839(9) 0.0287(6) 0.049(4) Uani 1 1 d . . . C42 C 0.0684(12) 0.8835(8) 0.0034(7) 0.067(4) Uani 1 1 d . . . H42C H 0.0615 0.9063 0.0457 0.1 Uiso 1 1 calc R . . H42B H 0.0003 0.8609 -0.001 0.1 Uiso 1 1 calc R . . H42A H 0.0734 0.9286 -0.0273 0.1 Uiso 1 1 calc R . . C43 C 0.2797(11) 0.8538(8) 0.0000(6) 0.055(4) Uani 1 1 d . . . H43C H 0.2812 0.8992 -0.0308 0.082 Uiso 1 1 calc R . . H43B H 0.3526 0.8114 -0.0065 0.082 Uiso 1 1 calc R . . H43A H 0.2697 0.8771 0.0422 0.082 Uiso 1 1 calc R . . C44 C -0.0221(11) 0.7206(10) 0.0504(7) 0.082(5) Uani 1 1 d . . . H44C H -0.0665 0.6776 0.0458 0.123 Uiso 1 1 calc R . . H44B H -0.0501 0.7699 0.0247 0.123 Uiso 1 1 calc R . . H44A H -0.0319 0.7375 0.0943 0.123 Uiso 1 1 calc R . . C45 C 0.1444(12) 0.6080(9) 0.0699(6) 0.063(4) Uani 1 1 d . . . H45C H 0.0955 0.5677 0.0663 0.095 Uiso 1 1 calc R . . H45B H 0.136 0.6262 0.1135 0.095 Uiso 1 1 calc R . . H45A H 0.2254 0.581 0.0566 0.095 Uiso 1 1 calc R . . C46 C 0.5484(11) 0.6537(9) 0.0154(6) 0.048(4) Uani 1 1 d . . . C47 C 0.6513(11) 0.5832(8) 0.0285(7) 0.056(4) Uani 1 1 d . . . H47B H 0.6234 0.5429 0.0588 0.067 Uiso 1 1 calc R . . H47A H 0.6841 0.5522 -0.0108 0.067 Uiso 1 1 calc R . . C48 C 0.7444(12) 0.6146(9) 0.0539(7) 0.064(4) Uani 1 1 d . . . H48B H 0.777 0.652 0.0231 0.076 Uiso 1 1 calc R . . H48A H 0.8076 0.5665 0.0629 0.076 Uiso 1 1 calc R . . C49 C 0.6920(11) 0.6626(9) 0.1133(7) 0.061(4) Uani 1 1 d . . . H49B H 0.7519 0.6868 0.1293 0.074 Uiso 1 1 calc R . . H49A H 0.6682 0.6227 0.1452 0.074 Uiso 1 1 calc R . . C50 C 0.5864(11) 0.7345(8) 0.1046(6) 0.048(4) Uani 1 1 d . . . C51 C 0.5813(12) 0.7049(9) -0.0424(6) 0.062(4) Uani 1 1 d . . . H51C H 0.6083 0.667 -0.0783 0.093 Uiso 1 1 calc R . . H51B H 0.6432 0.7324 -0.0343 0.093 Uiso 1 1 calc R . . H51A H 0.5135 0.7478 -0.0515 0.093 Uiso 1 1 calc R . . C52 C 0.4534(12) 0.6128(9) -0.0003(7) 0.067(4) Uani 1 1 d . . . H52C H 0.387 0.6566 -0.01 0.101 Uiso 1 1 calc R . . H52B H 0.4295 0.5794 0.0355 0.101 Uiso 1 1 calc R . . H52A H 0.4822 0.5759 -0.0366 0.101 Uiso 1 1 calc R . . C53 C 0.5265(11) 0.7646(9) 0.1693(6) 0.061(4) Uani 1 1 d . . . H53C H 0.5014 0.7176 0.1923 0.091 Uiso 1 1 calc R . . H53B H 0.459 0.8104 0.1649 0.091 Uiso 1 1 calc R . . H53A H 0.5806 0.7851 0.1923 0.091 Uiso 1 1 calc R . . C54 C 0.6266(11) 0.8106(8) 0.0720(6) 0.059(4) Uani 1 1 d . . . H54C H 0.5592 0.8566 0.0681 0.088 Uiso 1 1 calc R . . H54B H 0.667 0.7938 0.0304 0.088 Uiso 1 1 calc R . . H54A H 0.6792 0.8296 0.0969 0.088 Uiso 1 1 calc R . . C55 C -0.0108(11) 0.5534(8) 0.2694(6) 0.040(3) Uani 1 1 d . . . C56 C -0.0868(12) 0.5548(9) 0.2170(7) 0.063(4) Uani 1 1 d . . . H56B H -0.0618 0.5903 0.1821 0.076 Uiso 1 1 calc R . . H56A H -0.1682 0.5805 0.2328 0.076 Uiso 1 1 calc R . . C57 C -0.0792(13) 0.4655(10) 0.1927(6) 0.065(5) Uani 1 1 d . . . H57B H -0.1103 0.4312 0.2266 0.079 Uiso 1 1 calc R . . H57A H -0.1266 0.4688 0.1579 0.079 Uiso 1 1 calc R . . C58 C 0.0433(12) 0.4243(9) 0.1707(6) 0.058(4) Uani 1 1 d . . . H58B H 0.0725 0.4569 0.1351 0.069 Uiso 1 1 calc R . . H58A H 0.0467 0.3668 0.1556 0.069 Uiso 1 1 calc R . . C59 C 0.1206(11) 0.4188(8) 0.2223(6) 0.047(3) Uani 1 1 d . . . C60 C -0.0679(12) 0.5266(8) 0.3315(6) 0.056(4) Uani 1 1 d . . . H60C H -0.1414 0.5668 0.3434 0.085 Uiso 1 1 calc R . . H60B H -0.0166 0.5256 0.3637 0.085 Uiso 1 1 calc R . . H60A H -0.0825 0.4701 0.3274 0.085 Uiso 1 1 calc R . . C61 C -0.0023(11) 0.6453(8) 0.2793(6) 0.051(4) Uani 1 1 d . . . H61C H 0.0325 0.6672 0.2405 0.076 Uiso 1 1 calc R . . H61B H 0.046 0.6471 0.3126 0.076 Uiso 1 1 calc R . . H61A H -0.0799 0.6801 0.2912 0.076 Uiso 1 1 calc R . . C62 C 0.0970(11) 0.3520(8) 0.2719(6) 0.058(4) Uani 1 1 d . . . H62C H 0.11 0.2969 0.2518 0.087 Uiso 1 1 calc R . . H62B H 0.0167 0.368 0.2915 0.087 Uiso 1 1 calc R . . H62A H 0.1494 0.3487 0.3038 0.087 Uiso 1 1 calc R . . C63 C 0.2445(11) 0.3926(8) 0.1919(6) 0.059(4) Uani 1 1 d . . . H63C H 0.2561 0.3377 0.1717 0.089 Uiso 1 1 calc R . . H63B H 0.2972 0.3884 0.2239 0.089 Uiso 1 1 calc R . . H63A H 0.2605 0.4348 0.1606 0.089 Uiso 1 1 calc R . . C64 C 0.4196(11) 0.4166(8) 0.3485(6) 0.048(4) Uani 1 1 d . . . C65 C 0.4496(16) 0.3218(9) 0.3413(8) 0.088(6) Uani 1 1 d . . . H65B H 0.3919 0.3038 0.3187 0.106 Uiso 1 1 calc R . . H65A H 0.4486 0.2944 0.3829 0.106 Uiso 1 1 calc R . . C66 C 0.5753(18) 0.2945(12) 0.3031(10) 0.127(8) Uani 1 1 d . . . H66B H 0.6332 0.3115 0.3261 0.153 Uiso 1 1 calc R . . H66A H 0.5966 0.2324 0.298 0.153 Uiso 1 1 calc R . . C67 C 0.5740(13) 0.3390(9) 0.2369(8) 0.078(5) Uani 1 1 d . . . H67B H 0.6515 0.3234 0.2125 0.093 Uiso 1 1 calc R . . H67A H 0.5175 0.321 0.2134 0.093 Uiso 1 1 calc R . . C68 C 0.5404(11) 0.4329(9) 0.2474(7) 0.060(4) Uani 1 1 d . . . C69 C 0.2939(12) 0.4442(8) 0.3773(6) 0.056(4) Uani 1 1 d . . . H69C H 0.2433 0.4277 0.3498 0.084 Uiso 1 1 calc R . . H69B H 0.2739 0.5057 0.3825 0.084 Uiso 1 1 calc R . . H69A H 0.2836 0.417 0.4182 0.084 Uiso 1 1 calc R . . C70 C 0.4949(14) 0.4450(11) 0.3944(7) 0.094(6) Uani 1 1 d . . . H70C H 0.4731 0.5065 0.3991 0.142 Uiso 1 1 calc R . . H70B H 0.5769 0.4281 0.3777 0.142 Uiso 1 1 calc R . . H70A H 0.4821 0.4182 0.4352 0.142 Uiso 1 1 calc R . . C71 C 0.5235(12) 0.4736(10) 0.1824(7) 0.080(5) Uani 1 1 d . . . H71C H 0.5961 0.4581 0.1544 0.12 Uiso 1 1 calc R . . H71B H 0.5011 0.5352 0.1866 0.12 Uiso 1 1 calc R . . H71A H 0.4626 0.4534 0.165 0.12 Uiso 1 1 calc R . . C72 C 0.6378(13) 0.4662(12) 0.2691(9) 0.109(7) Uani 1 1 d . . . H72C H 0.659 0.4379 0.3081 0.163 Uiso 1 1 calc R . . H72B H 0.6123 0.5271 0.2762 0.163 Uiso 1 1 calc R . . H72A H 0.705 0.4551 0.237 0.163 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 0.0325(5) 0.0349(4) 0.0280(4) 0.0020(3) -0.0046(3) -0.0118(4) Ce2 0.0299(4) 0.0305(4) 0.0318(4) 0.0031(3) -0.0037(3) -0.0067(3) Ce3 0.0310(5) 0.0369(5) 0.0288(4) 0.0026(3) -0.0026(3) -0.0078(4) Ce4 0.0321(5) 0.0315(4) 0.0323(5) 0.0029(3) -0.0042(3) -0.0081(3) O1 0.032(5) 0.046(5) 0.046(5) 0.012(4) -0.007(4) -0.011(4) O2 0.041(5) 0.038(5) 0.049(5) 0.001(4) -0.009(4) -0.006(4) O3 0.034(5) 0.062(6) 0.041(5) 0.018(4) -0.010(4) -0.014(4) O4 0.038(5) 0.046(5) 0.037(5) -0.004(4) -0.006(4) -0.006(4) N1 0.051(7) 0.038(6) 0.028(6) 0.007(5) -0.004(5) -0.017(5) N2 0.036(6) 0.023(5) 0.027(6) 0.004(4) 0.004(5) -0.004(5) N3 0.034(6) 0.046(7) 0.020(6) 0.004(5) -0.007(5) -0.007(5) N4 0.040(6) 0.037(6) 0.043(7) 0.008(5) -0.006(5) -0.013(5) N5 0.048(7) 0.045(7) 0.035(6) 0.011(5) -0.006(5) -0.016(6) N6 0.040(7) 0.054(7) 0.034(7) 0.004(5) -0.004(5) -0.017(6) N7 0.041(7) 0.050(7) 0.037(7) 0.006(5) -0.009(5) -0.017(6) N8 0.028(6) 0.045(7) 0.034(6) 0.011(5) 0.001(5) 0.010(5) C1 0.045(9) 0.053(9) 0.026(8) 0.003(7) 0.002(6) -0.011(7) C2 0.035(8) 0.074(11) 0.054(10) -0.029(8) 0.015(7) -0.025(8) C3 0.087(13) 0.075(12) 0.060(11) -0.001(9) 0.013(9) -0.041(10) C4 0.046(10) 0.047(9) 0.066(10) -0.001(7) 0.012(7) -0.012(8) C5 0.064(10) 0.029(8) 0.036(8) 0.007(6) 0.012(7) -0.004(7) C6 0.040(9) 0.078(11) 0.066(11) 0.006(9) -0.006(8) 0.004(8) C7 0.059(10) 0.062(10) 0.053(10) -0.009(8) 0.016(8) -0.011(8) C8 0.069(11) 0.047(9) 0.044(9) 0.019(7) -0.012(8) -0.024(8) C9 0.086(12) 0.075(11) 0.039(9) -0.003(8) 0.008(8) -0.019(9) C10 0.053(9) 0.034(8) 0.035(8) 0.001(6) -0.010(7) -0.016(7) C11 0.056(10) 0.051(9) 0.068(11) -0.012(8) -0.022(8) -0.017(8) C12 0.054(10) 0.065(10) 0.058(10) -0.003(8) -0.009(8) -0.029(8) C13 0.043(9) 0.064(10) 0.045(9) 0.008(7) -0.013(7) -0.019(7) C14 0.034(8) 0.050(9) 0.032(8) 0.000(7) -0.004(6) -0.014(7) C15 0.044(9) 0.066(10) 0.055(10) -0.014(8) 0.003(7) -0.012(8) C16 0.064(10) 0.067(10) 0.050(10) -0.012(8) -0.021(8) -0.008(8) C17 0.042(9) 0.060(10) 0.053(9) -0.022(7) -0.005(7) -0.005(7) C18 0.049(9) 0.062(10) 0.067(10) 0.019(8) -0.010(8) -0.017(8) C19 0.044(8) 0.043(8) 0.028(8) -0.003(6) -0.005(6) -0.001(7) C20 0.051(9) 0.046(9) 0.040(9) -0.002(7) 0.015(7) 0.004(7) C21 0.035(8) 0.064(10) 0.048(9) 0.003(8) 0.008(7) -0.010(8) C22 0.044(9) 0.052(9) 0.055(9) 0.013(7) -0.009(7) -0.012(7) C23 0.038(8) 0.033(7) 0.019(7) 0.003(6) 0.001(6) -0.012(6) C24 0.052(9) 0.055(9) 0.057(10) -0.016(7) -0.011(7) -0.017(7) C25 0.054(9) 0.047(9) 0.058(10) 0.001(7) 0.000(7) 0.001(7) C26 0.046(9) 0.053(10) 0.072(11) -0.006(8) -0.018(8) -0.016(7) C27 0.041(8) 0.067(10) 0.037(8) 0.013(7) -0.016(6) -0.021(7) C28 0.028(8) 0.048(9) 0.054(9) 0.004(7) -0.010(7) -0.016(7) C29 0.039(9) 0.054(9) 0.082(11) 0.031(8) -0.019(8) -0.021(7) C30 0.024(8) 0.075(11) 0.096(13) 0.025(10) 0.003(8) -0.010(8) C31 0.035(9) 0.063(10) 0.058(10) 0.014(8) 0.001(7) -0.007(7) C32 0.035(8) 0.045(9) 0.046(9) 0.010(7) -0.005(7) -0.007(7) C33 0.073(11) 0.061(11) 0.090(13) -0.008(9) -0.013(9) -0.030(9) C34 0.061(10) 0.076(11) 0.071(11) 0.017(9) -0.032(8) -0.035(9) C35 0.073(11) 0.046(9) 0.064(10) 0.014(8) -0.022(8) -0.008(8) C36 0.048(9) 0.053(9) 0.037(8) 0.014(7) -0.015(7) -0.010(7) C37 0.048(9) 0.057(10) 0.047(9) 0.000(7) -0.027(7) -0.003(8) C38 0.103(13) 0.057(10) 0.035(9) 0.014(7) -0.018(8) -0.012(9) C39 0.096(14) 0.091(13) 0.064(12) 0.005(10) -0.026(10) -0.026(11) C40 0.071(11) 0.065(10) 0.047(10) 0.005(8) -0.018(8) -0.019(8) C41 0.044(9) 0.066(10) 0.042(9) -0.005(7) -0.016(7) -0.018(8) C42 0.068(11) 0.056(10) 0.075(11) 0.000(8) -0.044(9) 0.010(8) C43 0.069(11) 0.045(9) 0.039(9) 0.012(7) 0.007(7) 0.004(8) C44 0.042(10) 0.117(15) 0.093(13) -0.006(11) -0.027(9) -0.019(10) C45 0.070(11) 0.074(11) 0.058(10) 0.015(9) -0.018(8) -0.038(9) C46 0.045(9) 0.059(9) 0.040(9) 0.008(7) -0.005(7) -0.010(8) C47 0.045(9) 0.048(9) 0.071(11) -0.012(8) 0.007(8) -0.008(8) C48 0.047(10) 0.048(9) 0.084(12) -0.008(8) 0.010(9) 0.007(8) C49 0.042(9) 0.070(11) 0.076(12) 0.025(9) -0.019(8) -0.018(8) C50 0.042(9) 0.055(9) 0.045(9) 0.002(7) -0.008(7) -0.006(8) C51 0.060(10) 0.083(11) 0.034(9) -0.017(8) 0.021(7) -0.008(8) C52 0.063(11) 0.071(11) 0.062(11) -0.022(8) -0.003(8) -0.002(9) C53 0.053(10) 0.083(11) 0.053(10) -0.004(8) -0.015(8) -0.027(8) C54 0.048(9) 0.059(10) 0.074(11) 0.010(8) -0.001(8) -0.025(8) C55 0.040(9) 0.042(8) 0.041(8) 0.009(6) -0.004(7) -0.020(7) C56 0.056(10) 0.076(11) 0.071(11) 0.013(9) -0.032(8) -0.031(9) C57 0.072(12) 0.096(13) 0.048(10) 0.019(9) -0.039(9) -0.045(10) C58 0.071(11) 0.062(10) 0.051(10) 0.000(8) -0.009(8) -0.036(9) C59 0.047(9) 0.049(9) 0.045(9) -0.008(7) 0.005(7) -0.014(7) C60 0.073(11) 0.043(9) 0.051(10) 0.018(7) -0.005(8) -0.013(8) C61 0.043(9) 0.060(10) 0.049(9) 0.004(7) -0.010(7) -0.006(7) C62 0.060(10) 0.052(9) 0.071(11) 0.007(8) -0.009(8) -0.030(8) C63 0.063(10) 0.044(9) 0.068(11) -0.010(8) 0.000(8) -0.009(8) C64 0.044(9) 0.056(10) 0.039(9) 0.003(7) -0.001(7) 0.001(7) C65 0.118(16) 0.048(11) 0.081(13) 0.014(9) -0.021(11) 0.022(10) C66 0.13(2) 0.072(14) 0.15(2) 0.013(14) -0.015(16) 0.037(13) C67 0.052(10) 0.062(11) 0.101(14) 0.017(10) 0.000(9) 0.020(8) C68 0.022(8) 0.065(11) 0.085(12) 0.009(9) -0.013(8) 0.007(7) C69 0.103(13) 0.043(9) 0.032(8) 0.026(7) -0.019(8) -0.034(9) C70 0.104(14) 0.114(15) 0.080(13) 0.045(11) -0.052(11) -0.040(12) C71 0.051(10) 0.089(12) 0.075(12) 0.031(10) 0.034(8) 0.010(9) C72 0.044(11) 0.135(17) 0.137(18) -0.030(14) -0.024(11) 0.013(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O4 2.126(8) . ? Ce1 O1 2.157(8) . ? Ce1 N2 2.276(9) . ? Ce1 N1 2.281(9) . ? Ce2 O1 2.140(8) . ? Ce2 O2 2.146(8) . ? Ce2 N3 2.302(9) . ? Ce2 N4 2.303(9) . ? Ce3 O3 2.123(8) . ? Ce3 O2 2.145(8) . ? Ce3 N5 2.275(9) . ? Ce3 N6 2.283(9) . ? Ce4 O3 2.166(8) . ? Ce4 O4 2.179(8) . ? Ce4 N8 2.294(9) . ? Ce4 N7 2.297(9) . ? N1 C1 1.464(14) . ? N1 C5 1.478(14) . ? N2 C10 1.460(14) . ? N2 C14 1.482(14) . ? N3 C19 1.474(14) . ? N3 C23 1.500(13) . ? N4 C28 1.461(14) . ? N4 C32 1.484(14) . ? N5 C41 1.447(14) . ? N5 C37 1.464(15) . ? N6 C50 1.453(14) . ? N6 C46 1.503(15) . ? N7 C55 1.489(15) . ? N7 C59 1.523(15) . ? N8 C68 1.445(15) . ? N8 C64 1.495(14) . ? C1 C2 1.531(16) . ? C1 C6 1.549(16) . ? C1 C7 1.555(17) . ? C2 C3 1.540(18) . ? C2 H2B 0.99 . ? C2 H2A 0.99 . ? C3 C4 1.515(18) . ? C3 H3B 0.99 . ? C3 H3A 0.99 . ? C4 C5 1.514(16) . ? C4 H4B 0.99 . ? C4 H4A 0.99 . ? C5 C8 1.549(17) . ? C5 C9 1.564(17) . ? C6 H6C 0.98 . ? C6 H6B 0.98 . ? C6 H6A 0.98 . ? C7 H7C 0.98 . ? C7 H7B 0.98 . ? C7 H7A 0.98 . ? C8 H8C 0.98 . ? C8 H8B 0.98 . ? C8 H8A 0.98 . ? C9 H9C 0.98 . ? C9 H9B 0.98 . ? C9 H9A 0.98 . ? C10 C16 1.506(16) . ? C10 C11 1.536(16) . ? C10 C15 1.548(16) . ? C11 C12 1.496(17) . ? C11 H11B 0.99 . ? C11 H11A 0.99 . ? C12 C13 1.493(17) . ? C12 H12B 0.99 . ? C12 H12A 0.99 . ? C13 C14 1.559(15) . ? C13 H13B 0.99 . ? C13 H13A 0.99 . ? C14 C17 1.540(16) . ? C14 C18 1.545(16) . ? C15 H15C 0.98 . ? C15 H15B 0.98 . ? C15 H15A 0.98 . ? C16 H16C 0.98 . ? C16 H16B 0.98 . ? C16 H16A 0.98 . ? C17 H17C 0.98 . ? C17 H17B 0.98 . ? C17 H17A 0.98 . ? C18 H18C 0.98 . ? C18 H18B 0.98 . ? C18 H18A 0.98 . ? C19 C24 1.527(15) . ? C19 C25 1.530(16) . ? C19 C20 1.532(16) . ? C20 C21 1.499(16) . ? C20 H20B 0.99 . ? C20 H20A 0.99 . ? C21 C22 1.521(17) . ? C21 H21B 0.99 . ? C21 H21A 0.99 . ? C22 C23 1.519(15) . ? C22 H22B 0.99 . ? C22 H22A 0.99 . ? C23 C27 1.533(14) . ? C23 C26 1.546(16) . ? C24 H24C 0.98 . ? C24 H24B 0.98 . ? C24 H24A 0.98 . ? C25 H25C 0.98 . ? C25 H25B 0.98 . ? C25 H25A 0.98 . ? C26 H26C 0.98 . ? C26 H26B 0.98 . ? C26 H26A 0.98 . ? C27 H27C 0.98 . ? C27 H27B 0.98 . ? C27 H27A 0.98 . ? C28 C29 1.510(17) . ? C28 C33 1.538(17) . ? C28 C34 1.550(16) . ? C29 C30 1.525(17) . ? C29 H29B 0.99 . ? C29 H29A 0.99 . ? C30 C31 1.543(17) . ? C30 H30B 0.99 . ? C30 H30A 0.99 . ? C31 C32 1.526(16) . ? C31 H31B 0.99 . ? C31 H31A 0.99 . ? C32 C36 1.522(15) . ? C32 C35 1.564(16) . ? C33 H33C 0.98 . ? C33 H33B 0.98 . ? C33 H33A 0.98 . ? C34 H34C 0.98 . ? C34 H34B 0.98 . ? C34 H34A 0.98 . ? C35 H35C 0.98 . ? C35 H35B 0.98 . ? C35 H35A 0.98 . ? C36 H36C 0.98 . ? C36 H36B 0.98 . ? C36 H36A 0.98 . ? C37 C43 1.536(16) . ? C37 C42 1.543(17) . ? C37 C38 1.555(18) . ? C38 C39 1.512(18) . ? C38 H38B 0.99 . ? C38 H38A 0.99 . ? C39 C40 1.548(18) . ? C39 H39B 0.99 . ? C39 H39A 0.99 . ? C40 C41 1.511(17) . ? C40 H40B 0.99 . ? C40 H40A 0.99 . ? C41 C45 1.514(17) . ? C41 C44 1.548(18) . ? C42 H42C 0.98 . ? C42 H42B 0.98 . ? C42 H42A 0.98 . ? C43 H43C 0.98 . ? C43 H43B 0.98 . ? C43 H43A 0.98 . ? C44 H44C 0.98 . ? C44 H44B 0.98 . ? C44 H44A 0.98 . ? C45 H45C 0.98 . ? C45 H45B 0.98 . ? C45 H45A 0.98 . ? C46 C52 1.513(16) . ? C46 C47 1.530(17) . ? C46 C51 1.536(16) . ? C47 C48 1.490(17) . ? C47 H47B 0.99 . ? C47 H47A 0.99 . ? C48 C49 1.511(18) . ? C48 H48B 0.99 . ? C48 H48A 0.99 . ? C49 C50 1.543(17) . ? C49 H49B 0.99 . ? C49 H49A 0.99 . ? C50 C53 1.528(17) . ? C50 C54 1.542(16) . ? C51 H51C 0.98 . ? C51 H51B 0.98 . ? C51 H51A 0.98 . ? C52 H52C 0.98 . ? C52 H52B 0.98 . ? C52 H52A 0.98 . ? C53 H53C 0.98 . ? C53 H53B 0.98 . ? C53 H53A 0.98 . ? C54 H54C 0.98 . ? C54 H54B 0.98 . ? C54 H54A 0.98 . ? C55 C60 1.521(16) . ? C55 C56 1.532(16) . ? C55 C61 1.543(16) . ? C56 C57 1.538(18) . ? C56 H56B 0.99 . ? C56 H56A 0.99 . ? C57 C58 1.490(18) . ? C57 H57B 0.99 . ? C57 H57A 0.99 . ? C58 C59 1.522(17) . ? C58 H58B 0.99 . ? C58 H58A 0.99 . ? C59 C63 1.515(16) . ? C59 C62 1.545(16) . ? C60 H60C 0.98 . ? C60 H60B 0.98 . ? C60 H60A 0.98 . ? C61 H61C 0.98 . ? C61 H61B 0.98 . ? C61 H61A 0.98 . ? C62 H62C 0.98 . ? C62 H62B 0.98 . ? C62 H62A 0.98 . ? C63 H63C 0.98 . ? C63 H63B 0.98 . ? C63 H63A 0.98 . ? C64 C65 1.511(18) . ? C64 C69 1.524(17) . ? C64 C70 1.560(18) . ? C65 C66 1.59(2) . ? C65 H65B 0.99 . ? C65 H65A 0.99 . ? C66 C67 1.58(2) . ? C66 H66B 0.99 . ? C66 H66A 0.99 . ? C67 C68 1.505(19) . ? C67 H67B 0.99 . ? C67 H67A 0.99 . ? C68 C72 1.514(19) . ? C68 C71 1.550(18) . ? C69 H69C 0.98 . ? C69 H69B 0.98 . ? C69 H69A 0.98 . ? C70 H70C 0.98 . ? C70 H70B 0.98 . ? C70 H70A 0.98 . ? C71 H71C 0.98 . ? C71 H71B 0.98 . ? C71 H71A 0.98 . ? C72 H72C 0.98 . ? C72 H72B 0.98 . ? C72 H72A 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ce1 O1 89.1(3) . . ? O4 Ce1 N2 120.5(3) . . ? O1 Ce1 N2 104.9(3) . . ? O4 Ce1 N1 104.7(3) . . ? O1 Ce1 N1 123.5(3) . . ? N2 Ce1 N1 113.1(3) . . ? O1 Ce2 O2 87.8(3) . . ? O1 Ce2 N3 106.5(3) . . ? O2 Ce2 N3 120.8(3) . . ? O1 Ce2 N4 124.1(3) . . ? O2 Ce2 N4 103.2(3) . . ? N3 Ce2 N4 113.2(3) . . ? O3 Ce3 O2 88.0(3) . . ? O3 Ce3 N5 118.8(3) . . ? O2 Ce3 N5 104.8(3) . . ? O3 Ce3 N6 107.2(3) . . ? O2 Ce3 N6 116.6(3) . . ? N5 Ce3 N6 118.1(3) . . ? O3 Ce4 O4 86.8(3) . . ? O3 Ce4 N8 119.2(3) . . ? O4 Ce4 N8 105.0(3) . . ? O3 Ce4 N7 107.7(3) . . ? O4 Ce4 N7 118.5(3) . . ? N8 Ce4 N7 116.5(3) . . ? Ce2 O1 Ce1 178.8(4) . . ? Ce3 O2 Ce2 178.0(4) . . ? Ce3 O3 Ce4 178.4(4) . . ? Ce1 O4 Ce4 178.6(4) . . ? C1 N1 C5 115.4(9) . . ? C1 N1 Ce1 124.0(7) . . ? C5 N1 Ce1 119.0(8) . . ? C10 N2 C14 117.0(9) . . ? C10 N2 Ce1 119.2(7) . . ? C14 N2 Ce1 123.8(7) . . ? C19 N3 C23 118.2(9) . . ? C19 N3 Ce2 118.8(7) . . ? C23 N3 Ce2 122.9(7) . . ? C28 N4 C32 117.3(9) . . ? C28 N4 Ce2 124.3(7) . . ? C32 N4 Ce2 116.9(7) . . ? C41 N5 C37 117.6(10) . . ? C41 N5 Ce3 124.8(7) . . ? C37 N5 Ce3 117.5(7) . . ? C50 N6 C46 115.8(10) . . ? C50 N6 Ce3 125.1(8) . . ? C46 N6 Ce3 119.0(7) . . ? C55 N7 C59 115.4(9) . . ? C55 N7 Ce4 123.8(7) . . ? C59 N7 Ce4 120.8(7) . . ? C68 N8 C64 116.4(10) . . ? C68 N8 Ce4 126.8(8) . . ? C64 N8 Ce4 116.7(7) . . ? N1 C1 C2 111.6(10) . . ? N1 C1 C6 106.6(9) . . ? C2 C1 C6 110.1(11) . . ? N1 C1 C7 112.9(10) . . ? C2 C1 C7 110.3(10) . . ? C6 C1 C7 105.2(11) . . ? C1 C2 C3 113.3(11) . . ? C1 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? H2B C2 H2A 107.7 . . ? C4 C3 C2 109.0(11) . . ? C4 C3 H3B 109.9 . . ? C2 C3 H3B 109.9 . . ? C4 C3 H3A 109.9 . . ? C2 C3 H3A 109.9 . . ? H3B C3 H3A 108.3 . . ? C5 C4 C3 111.5(11) . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? H4B C4 H4A 108 . . ? N1 C5 C4 113.2(11) . . ? N1 C5 C8 106.5(9) . . ? C4 C5 C8 107.5(10) . . ? N1 C5 C9 113.5(10) . . ? C4 C5 C9 110.2(10) . . ? C8 C5 C9 105.3(11) . . ? C1 C6 H6C 109.5 . . ? C1 C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? C1 C6 H6A 109.5 . . ? H6C C6 H6A 109.5 . . ? H6B C6 H6A 109.5 . . ? C1 C7 H7C 109.5 . . ? C1 C7 H7B 109.5 . . ? H7C C7 H7B 109.5 . . ? C1 C7 H7A 109.5 . . ? H7C C7 H7A 109.5 . . ? H7B C7 H7A 109.5 . . ? C5 C8 H8C 109.5 . . ? C5 C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? C5 C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? H8B C8 H8A 109.5 . . ? C5 C9 H9C 109.5 . . ? C5 C9 H9B 109.5 . . ? H9C C9 H9B 109.5 . . ? C5 C9 H9A 109.5 . . ? H9C C9 H9A 109.5 . . ? H9B C9 H9A 109.5 . . ? N2 C10 C16 115.4(10) . . ? N2 C10 C11 110.6(10) . . ? C16 C10 C11 109.1(10) . . ? N2 C10 C15 107.4(9) . . ? C16 C10 C15 106.0(10) . . ? C11 C10 C15 107.9(10) . . ? C12 C11 C10 113.4(11) . . ? C12 C11 H11B 108.9 . . ? C10 C11 H11B 108.9 . . ? C12 C11 H11A 108.9 . . ? C10 C11 H11A 108.9 . . ? H11B C11 H11A 107.7 . . ? C13 C12 C11 110.5(11) . . ? C13 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? H12B C12 H12A 108.1 . . ? C12 C13 C14 112.1(10) . . ? C12 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? H13B C13 H13A 107.9 . . ? N2 C14 C17 107.8(9) . . ? N2 C14 C18 114.5(9) . . ? C17 C14 C18 105.6(11) . . ? N2 C14 C13 112.1(10) . . ? C17 C14 C13 106.7(10) . . ? C18 C14 C13 109.6(10) . . ? C10 C15 H15C 109.5 . . ? C10 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C10 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? C10 C16 H16C 109.5 . . ? C10 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? C10 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? C14 C17 H17C 109.5 . . ? C14 C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? C14 C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? C14 C18 H18C 109.5 . . ? C14 C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? C14 C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? N3 C19 C24 107.0(10) . . ? N3 C19 C25 113.8(10) . . ? C24 C19 C25 105.4(10) . . ? N3 C19 C20 111.5(10) . . ? C24 C19 C20 108.9(10) . . ? C25 C19 C20 109.8(10) . . ? C21 C20 C19 112.2(11) . . ? C21 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? H20B C20 H20A 107.9 . . ? C20 C21 C22 110.6(11) . . ? C20 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? H21B C21 H21A 108.1 . . ? C23 C22 C21 111.6(10) . . ? C23 C22 H22B 109.3 . . ? C21 C22 H22B 109.3 . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22A 109.3 . . ? H22B C22 H22A 108 . . ? N3 C23 C22 110.9(9) . . ? N3 C23 C27 113.0(8) . . ? C22 C23 C27 112.0(10) . . ? N3 C23 C26 106.5(9) . . ? C22 C23 C26 108.4(10) . . ? C27 C23 C26 105.7(10) . . ? C19 C24 H24C 109.5 . . ? C19 C24 H24B 109.5 . . ? H24C C24 H24B 109.5 . . ? C19 C24 H24A 109.5 . . ? H24C C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? C19 C25 H25C 109.5 . . ? C19 C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? C19 C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? C23 C26 H26C 109.5 . . ? C23 C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? C23 C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? C23 C27 H27C 109.5 . . ? C23 C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? C23 C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? N4 C28 C29 112.6(11) . . ? N4 C28 C33 114.3(10) . . ? C29 C28 C33 110.8(10) . . ? N4 C28 C34 106.0(9) . . ? C29 C28 C34 108.3(11) . . ? C33 C28 C34 104.2(11) . . ? C28 C29 C30 112.3(11) . . ? C28 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? H29B C29 H29A 107.9 . . ? C29 C30 C31 109.9(10) . . ? C29 C30 H30B 109.7 . . ? C31 C30 H30B 109.7 . . ? C29 C30 H30A 109.7 . . ? C31 C30 H30A 109.7 . . ? H30B C30 H30A 108.2 . . ? C32 C31 C30 112.0(11) . . ? C32 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? H31B C31 H31A 107.9 . . ? N4 C32 C36 108.0(9) . . ? N4 C32 C31 110.1(10) . . ? C36 C32 C31 108.6(11) . . ? N4 C32 C35 113.0(10) . . ? C36 C32 C35 107.3(10) . . ? C31 C32 C35 109.8(10) . . ? C28 C33 H33C 109.5 . . ? C28 C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? C28 C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? C28 C34 H34C 109.5 . . ? C28 C34 H34B 109.5 . . ? H34C C34 H34B 109.5 . . ? C28 C34 H34A 109.5 . . ? H34C C34 H34A 109.5 . . ? H34B C34 H34A 109.5 . . ? C32 C35 H35C 109.5 . . ? C32 C35 H35B 109.5 . . ? H35C C35 H35B 109.5 . . ? C32 C35 H35A 109.5 . . ? H35C C35 H35A 109.5 . . ? H35B C35 H35A 109.5 . . ? C32 C36 H36C 109.5 . . ? C32 C36 H36B 109.5 . . ? H36C C36 H36B 109.5 . . ? C32 C36 H36A 109.5 . . ? H36C C36 H36A 109.5 . . ? H36B C36 H36A 109.5 . . ? N5 C37 C43 108.7(9) . . ? N5 C37 C42 114.8(11) . . ? C43 C37 C42 105.6(11) . . ? N5 C37 C38 109.9(10) . . ? C43 C37 C38 107.3(11) . . ? C42 C37 C38 110.3(11) . . ? C39 C38 C37 112.5(12) . . ? C39 C38 H38B 109.1 . . ? C37 C38 H38B 109.1 . . ? C39 C38 H38A 109.1 . . ? C37 C38 H38A 109.1 . . ? H38B C38 H38A 107.8 . . ? C38 C39 C40 109.2(12) . . ? C38 C39 H39B 109.8 . . ? C40 C39 H39B 109.8 . . ? C38 C39 H39A 109.8 . . ? C40 C39 H39A 109.8 . . ? H39B C39 H39A 108.3 . . ? C41 C40 C39 113.2(12) . . ? C41 C40 H40B 108.9 . . ? C39 C40 H40B 108.9 . . ? C41 C40 H40A 108.9 . . ? C39 C40 H40A 108.9 . . ? H40B C40 H40A 107.7 . . ? N5 C41 C40 111.6(11) . . ? N5 C41 C45 107.1(10) . . ? C40 C41 C45 107.7(12) . . ? N5 C41 C44 114.0(12) . . ? C40 C41 C44 109.6(11) . . ? C45 C41 C44 106.5(11) . . ? C37 C42 H42C 109.5 . . ? C37 C42 H42B 109.5 . . ? H42C C42 H42B 109.5 . . ? C37 C42 H42A 109.5 . . ? H42C C42 H42A 109.5 . . ? H42B C42 H42A 109.5 . . ? C37 C43 H43C 109.5 . . ? C37 C43 H43B 109.5 . . ? H43C C43 H43B 109.5 . . ? C37 C43 H43A 109.5 . . ? H43C C43 H43A 109.5 . . ? H43B C43 H43A 109.5 . . ? C41 C44 H44C 109.5 . . ? C41 C44 H44B 109.5 . . ? H44C C44 H44B 109.5 . . ? C41 C44 H44A 109.5 . . ? H44C C44 H44A 109.5 . . ? H44B C44 H44A 109.5 . . ? C41 C45 H45C 109.5 . . ? C41 C45 H45B 109.5 . . ? H45C C45 H45B 109.5 . . ? C41 C45 H45A 109.5 . . ? H45C C45 H45A 109.5 . . ? H45B C45 H45A 109.5 . . ? N6 C46 C52 107.1(10) . . ? N6 C46 C47 110.3(10) . . ? C52 C46 C47 107.7(11) . . ? N6 C46 C51 114.3(11) . . ? C52 C46 C51 106.6(11) . . ? C47 C46 C51 110.4(11) . . ? C48 C47 C46 113.3(11) . . ? C48 C47 H47B 108.9 . . ? C46 C47 H47B 108.9 . . ? C48 C47 H47A 108.9 . . ? C46 C47 H47A 108.9 . . ? H47B C47 H47A 107.7 . . ? C47 C48 C49 108.0(11) . . ? C47 C48 H48B 110.1 . . ? C49 C48 H48B 110.1 . . ? C47 C48 H48A 110.1 . . ? C49 C48 H48A 110.1 . . ? H48B C48 H48A 108.4 . . ? C48 C49 C50 113.6(12) . . ? C48 C49 H49B 108.8 . . ? C50 C49 H49B 108.8 . . ? C48 C49 H49A 108.8 . . ? C50 C49 H49A 108.8 . . ? H49B C49 H49A 107.7 . . ? N6 C50 C53 106.6(10) . . ? N6 C50 C54 113.2(10) . . ? C53 C50 C54 106.6(11) . . ? N6 C50 C49 112.0(11) . . ? C53 C50 C49 108.1(11) . . ? C54 C50 C49 110.0(11) . . ? C46 C51 H51C 109.5 . . ? C46 C51 H51B 109.5 . . ? H51C C51 H51B 109.5 . . ? C46 C51 H51A 109.5 . . ? H51C C51 H51A 109.5 . . ? H51B C51 H51A 109.5 . . ? C46 C52 H52C 109.5 . . ? C46 C52 H52B 109.5 . . ? H52C C52 H52B 109.5 . . ? C46 C52 H52A 109.5 . . ? H52C C52 H52A 109.5 . . ? H52B C52 H52A 109.5 . . ? C50 C53 H53C 109.5 . . ? C50 C53 H53B 109.5 . . ? H53C C53 H53B 109.5 . . ? C50 C53 H53A 109.5 . . ? H53C C53 H53A 109.5 . . ? H53B C53 H53A 109.5 . . ? C50 C54 H54C 109.5 . . ? C50 C54 H54B 109.5 . . ? H54C C54 H54B 109.5 . . ? C50 C54 H54A 109.5 . . ? H54C C54 H54A 109.5 . . ? H54B C54 H54A 109.5 . . ? N7 C55 C60 114.2(10) . . ? N7 C55 C56 111.9(11) . . ? C60 C55 C56 111.6(10) . . ? N7 C55 C61 106.3(9) . . ? C60 C55 C61 105.1(10) . . ? C56 C55 C61 107.0(10) . . ? C55 C56 C57 111.6(11) . . ? C55 C56 H56B 109.3 . . ? C57 C56 H56B 109.3 . . ? C55 C56 H56A 109.3 . . ? C57 C56 H56A 109.3 . . ? H56B C56 H56A 108 . . ? C58 C57 C56 110.4(11) . . ? C58 C57 H57B 109.6 . . ? C56 C57 H57B 109.6 . . ? C58 C57 H57A 109.6 . . ? C56 C57 H57A 109.6 . . ? H57B C57 H57A 108.1 . . ? C57 C58 C59 111.8(11) . . ? C57 C58 H58B 109.3 . . ? C59 C58 H58B 109.3 . . ? C57 C58 H58A 109.3 . . ? C59 C58 H58A 109.3 . . ? H58B C58 H58A 107.9 . . ? C63 C59 C58 107.0(11) . . ? C63 C59 N7 105.9(9) . . ? C58 C59 N7 111.4(11) . . ? C63 C59 C62 108.8(11) . . ? C58 C59 C62 111.3(10) . . ? N7 C59 C62 112.0(10) . . ? C55 C60 H60C 109.5 . . ? C55 C60 H60B 109.5 . . ? H60C C60 H60B 109.5 . . ? C55 C60 H60A 109.5 . . ? H60C C60 H60A 109.5 . . ? H60B C60 H60A 109.5 . . ? C55 C61 H61C 109.5 . . ? C55 C61 H61B 109.5 . . ? H61C C61 H61B 109.5 . . ? C55 C61 H61A 109.5 . . ? H61C C61 H61A 109.5 . . ? H61B C61 H61A 109.5 . . ? C59 C62 H62C 109.5 . . ? C59 C62 H62B 109.5 . . ? H62C C62 H62B 109.5 . . ? C59 C62 H62A 109.5 . . ? H62C C62 H62A 109.5 . . ? H62B C62 H62A 109.5 . . ? C59 C63 H63C 109.5 . . ? C59 C63 H63B 109.5 . . ? H63C C63 H63B 109.5 . . ? C59 C63 H63A 109.5 . . ? H63C C63 H63A 109.5 . . ? H63B C63 H63A 109.5 . . ? N8 C64 C65 110.7(11) . . ? N8 C64 C69 107.6(10) . . ? C65 C64 C69 109.0(12) . . ? N8 C64 C70 111.8(11) . . ? C65 C64 C70 110.8(12) . . ? C69 C64 C70 106.8(12) . . ? C64 C65 C66 108.8(14) . . ? C64 C65 H65B 109.9 . . ? C66 C65 H65B 109.9 . . ? C64 C65 H65A 109.9 . . ? C66 C65 H65A 109.9 . . ? H65B C65 H65A 108.3 . . ? C67 C66 C65 108.7(14) . . ? C67 C66 H66B 110 . . ? C65 C66 H66B 110 . . ? C67 C66 H66A 110 . . ? C65 C66 H66A 110 . . ? H66B C66 H66A 108.3 . . ? C68 C67 C66 107.8(14) . . ? C68 C67 H67B 110.2 . . ? C66 C67 H67B 110.2 . . ? C68 C67 H67A 110.2 . . ? C66 C67 H67A 110.2 . . ? H67B C67 H67A 108.5 . . ? N8 C68 C67 112.9(12) . . ? N8 C68 C72 113.6(13) . . ? C67 C68 C72 111.8(12) . . ? N8 C68 C71 106.5(10) . . ? C67 C68 C71 106.1(13) . . ? C72 C68 C71 105.2(13) . . ? C64 C69 H69C 109.5 . . ? C64 C69 H69B 109.5 . . ? H69C C69 H69B 109.5 . . ? C64 C69 H69A 109.5 . . ? H69C C69 H69A 109.5 . . ? H69B C69 H69A 109.5 . . ? C64 C70 H70C 109.5 . . ? C64 C70 H70B 109.5 . . ? H70C C70 H70B 109.5 . . ? C64 C70 H70A 109.5 . . ? H70C C70 H70A 109.5 . . ? H70B C70 H70A 109.5 . . ? C68 C71 H71C 109.5 . . ? C68 C71 H71B 109.5 . . ? H71C C71 H71B 109.5 . . ? C68 C71 H71A 109.5 . . ? H71C C71 H71A 109.5 . . ? H71B C71 H71A 109.5 . . ? C68 C72 H72C 109.5 . . ? C68 C72 H72B 109.5 . . ? H72C C72 H72B 109.5 . . ? C68 C72 H72A 109.5 . . ? H72C C72 H72A 109.5 . . ? H72B C72 H72A 109.5 . . ? #===END data_(6)-dec303 _database_code_depnum_ccdc_archive 'CCDC 774596' #TrackingRef '- mfl_28jul2009.CIF' _audit_creation_date 2004-03-22T10:01:19-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H108 Ce2 N6 Na2 O2 Si12' _chemical_formula_sum 'C36 H108 Ce2 N6 Na2 O2 Si12' _chemical_formula_weight 1320.58 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 15.7068(4) _cell_length_b 18.5131(4) _cell_length_c 12.4916(3) _cell_angle_alpha 90 _cell_angle_beta 109.085(1) _cell_angle_gamma 90 _cell_volume 3432.67(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 35515 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5767 _exptl_absorpt_correction_T_max 0.7597 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.227229E-1 _diffrn_orient_matrix_ub_12 0.481717E-1 _diffrn_orient_matrix_ub_13 0.172858E-1 _diffrn_orient_matrix_ub_21 -0.710145E-1 _diffrn_orient_matrix_ub_22 -0.16088E-2 _diffrn_orient_matrix_ub_23 -0.531236E-1 _diffrn_orient_matrix_ub_31 -0.402041E-1 _diffrn_orient_matrix_ub_32 -0.243845E-1 _diffrn_orient_matrix_ub_33 0.37653E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_reflns_number 51628 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 6038 _reflns_number_gt 4821 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0299P)^2^+10.6013P] 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_number_reflns 6038 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.091 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.42 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.089 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Na Na 0.0362 0.0249 '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 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce Ce 0.726860(16) 0.495988(13) 0.70090(2) 0.02365(9) Uani 1 1 d . . . Na Na 0.49464(17) 0.41713(13) 0.5008(3) 0.0746(8) Uani 1 1 d . . . Si1 Si 0.67719(9) 0.31186(7) 0.67755(11) 0.0303(3) Uani 1 1 d . . . Si2 Si 0.87262(8) 0.34938(7) 0.72901(11) 0.0280(3) Uani 1 1 d . . . Si3 Si 0.72399(9) 0.50134(8) 0.98257(10) 0.0339(3) Uani 1 1 d . . . Si4 Si 0.59870(9) 0.60259(7) 0.81590(12) 0.0346(3) Uani 1 1 d . . . Si5 Si 0.87790(9) 0.63672(7) 0.71002(12) 0.0343(3) Uani 1 1 d . . . Si6 Si 0.78351(9) 0.57299(8) 0.47957(11) 0.0348(3) Uani 1 1 d . . . O O 0.6089(3) 0.4963(2) 0.5841(5) 0.0874(18) Uani 1 1 d . . . N1 N 0.7624(2) 0.37438(18) 0.7072(3) 0.0248(8) Uani 1 1 d . . . N2 N 0.6827(2) 0.5387(2) 0.8493(3) 0.0284(8) Uani 1 1 d . . . N3 N 0.8038(2) 0.57545(19) 0.6239(3) 0.0286(8) Uani 1 1 d . . . C1 C 0.6265(4) 0.2963(3) 0.5211(4) 0.0479(14) Uani 1 1 d . . . H1C H 0.5806 0.2584 0.5071 0.072 Uiso 1 1 calc R . . H1B H 0.6738 0.2813 0.4905 0.072 Uiso 1 1 calc R . . H1A H 0.5987 0.3411 0.4841 0.072 Uiso 1 1 calc R . . C2 C 0.7111(4) 0.2199(3) 0.7396(5) 0.0484(14) Uani 1 1 d . . . H2C H 0.6578 0.1888 0.7215 0.073 Uiso 1 1 calc R . . H2B H 0.7383 0.2239 0.822 0.073 Uiso 1 1 calc R . . H2A H 0.7548 0.199 0.7077 0.073 Uiso 1 1 calc R . . C3 C 0.5871(3) 0.3421(3) 0.7362(5) 0.0450(13) Uani 1 1 d . . . H3C H 0.5603 0.3872 0.6992 0.067 Uiso 1 1 calc R . . H3B H 0.6137 0.3501 0.8179 0.067 Uiso 1 1 calc R . . H3A H 0.5404 0.3049 0.7219 0.067 Uiso 1 1 calc R . . C4 C 0.8851(4) 0.2980(3) 0.6065(4) 0.0415(12) Uani 1 1 d . . . H4C H 0.8657 0.3283 0.5384 0.062 Uiso 1 1 calc R . . H4B H 0.8477 0.2543 0.5939 0.062 Uiso 1 1 calc R . . H4A H 0.9483 0.2843 0.6227 0.062 Uiso 1 1 calc R . . C5 C 0.9235(3) 0.2959(3) 0.8614(4) 0.0377(12) Uani 1 1 d . . . H5C H 0.9865 0.285 0.8703 0.057 Uiso 1 1 calc R . . H5B H 0.89 0.2507 0.8567 0.057 Uiso 1 1 calc R . . H5A H 0.9207 0.324 0.9267 0.057 Uiso 1 1 calc R . . C6 C 0.9440(3) 0.4323(3) 0.7472(5) 0.0450(13) Uani 1 1 d . . . H6C H 0.9414 0.4593 0.8136 0.067 Uiso 1 1 calc R . . H6B H 0.9214 0.4627 0.6796 0.067 Uiso 1 1 calc R . . H6A H 1.0064 0.4183 0.7581 0.067 Uiso 1 1 calc R . . C7 C 0.6331(4) 0.4567(3) 1.0253(5) 0.0569(16) Uani 1 1 d . . . H7C H 0.6076 0.4165 0.9736 0.085 Uiso 1 1 calc R . . H7B H 0.5857 0.4918 1.0218 0.085 Uiso 1 1 calc R . . H7A H 0.6585 0.4382 1.1028 0.085 Uiso 1 1 calc R . . C8 C 0.8093(4) 0.4312(3) 0.9849(4) 0.0511(15) Uani 1 1 d . . . H8C H 0.834 0.4111 1.0614 0.077 Uiso 1 1 calc R . . H8B H 0.858 0.453 0.9629 0.077 Uiso 1 1 calc R . . H8A H 0.7809 0.3926 0.9315 0.077 Uiso 1 1 calc R . . C9 C 0.7828(4) 0.5658(3) 1.0974(5) 0.0564(16) Uani 1 1 d . . . H9C H 0.7398 0.602 1.1056 0.085 Uiso 1 1 calc R . . H9B H 0.8314 0.5899 1.0782 0.085 Uiso 1 1 calc R . . H9A H 0.8081 0.5394 1.1688 0.085 Uiso 1 1 calc R . . C10 C 0.5925(5) 0.6594(3) 0.9379(5) 0.0618(17) Uani 1 1 d . . . H10C H 0.6496 0.6851 0.9713 0.093 Uiso 1 1 calc R . . H10B H 0.5812 0.6282 0.9953 0.093 Uiso 1 1 calc R . . H10A H 0.5434 0.6944 0.9108 0.093 Uiso 1 1 calc R . . C11 C 0.6167(4) 0.6698(3) 0.7118(5) 0.0474(14) Uani 1 1 d . . . H11C H 0.5651 0.7027 0.6869 0.071 Uiso 1 1 calc R . . H11B H 0.6228 0.644 0.6461 0.071 Uiso 1 1 calc R . . H11A H 0.6717 0.6976 0.7483 0.071 Uiso 1 1 calc R . . C12 C 0.4845(3) 0.5609(3) 0.7548(5) 0.0469(14) Uani 1 1 d . . . H12C H 0.4711 0.5319 0.813 0.07 Uiso 1 1 calc R . . H12B H 0.4834 0.5299 0.6908 0.07 Uiso 1 1 calc R . . H12A H 0.4392 0.5991 0.7287 0.07 Uiso 1 1 calc R . . C13 C 0.9978(3) 0.6229(3) 0.7168(5) 0.0457(13) Uani 1 1 d . . . H13C H 1.0032 0.6319 0.642 0.069 Uiso 1 1 calc R . . H13B H 1.016 0.5731 0.7399 0.069 Uiso 1 1 calc R . . H13A H 1.0368 0.6564 0.772 0.069 Uiso 1 1 calc R . . C14 C 0.8445(4) 0.7327(3) 0.6668(5) 0.0501(14) Uani 1 1 d . . . H14C H 0.8828 0.7657 0.7236 0.075 Uiso 1 1 calc R . . H14B H 0.7814 0.7401 0.6611 0.075 Uiso 1 1 calc R . . H14A H 0.8518 0.7423 0.5931 0.075 Uiso 1 1 calc R . . C15 C 0.8794(4) 0.6264(3) 0.8599(4) 0.0536(15) Uani 1 1 d . . . H15C H 0.9009 0.578 0.8874 0.08 Uiso 1 1 calc R . . H15B H 0.8184 0.6333 0.863 0.08 Uiso 1 1 calc R . . H15A H 0.9197 0.6627 0.9077 0.08 Uiso 1 1 calc R . . C16 C 0.8755(5) 0.6127(4) 0.4330(5) 0.072(2) Uani 1 1 d . . . H16C H 0.9308 0.5845 0.4651 0.107 Uiso 1 1 calc R . . H16B H 0.8863 0.6628 0.4594 0.107 Uiso 1 1 calc R . . H16A H 0.8574 0.6116 0.3501 0.107 Uiso 1 1 calc R . . C17 C 0.6778(4) 0.6229(4) 0.4000(5) 0.0637(17) Uani 1 1 d . . . H17C H 0.6692 0.6214 0.3187 0.096 Uiso 1 1 calc R . . H17B H 0.6828 0.6733 0.4254 0.096 Uiso 1 1 calc R . . H17A H 0.6262 0.6002 0.4142 0.096 Uiso 1 1 calc R . . C18 C 0.7702(4) 0.4779(3) 0.4276(5) 0.0518(15) Uani 1 1 d . . . H18C H 0.7567 0.4776 0.3452 0.078 Uiso 1 1 calc R . . H18B H 0.7207 0.4549 0.4465 0.078 Uiso 1 1 calc R . . H18A H 0.8262 0.4513 0.4636 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.02327(13) 0.02197(14) 0.02645(14) 0.00091(11) 0.00913(10) 0.00034(11) Na 0.0571(15) 0.0375(12) 0.107(2) 0.0075(13) -0.0034(14) -0.0015(12) Si1 0.0305(7) 0.0260(7) 0.0326(7) -0.0008(5) 0.0079(6) -0.0032(5) Si2 0.0262(7) 0.0271(7) 0.0305(7) -0.0004(5) 0.0088(6) 0.0047(5) Si3 0.0378(7) 0.0407(7) 0.0234(6) 0.0015(6) 0.0104(5) 0.0083(6) Si4 0.0344(7) 0.0337(7) 0.0345(7) -0.0013(6) 0.0099(6) 0.0082(6) Si5 0.0306(7) 0.0314(7) 0.0366(8) 0.0006(6) 0.0052(6) -0.0103(6) Si6 0.0358(7) 0.0387(8) 0.0291(7) 0.0041(6) 0.0095(6) -0.0070(6) O 0.054(3) 0.041(2) 0.114(4) 0.023(2) -0.046(3) -0.011(2) N1 0.0251(19) 0.0223(19) 0.0262(19) 0.0003(15) 0.0073(16) -0.0004(15) N2 0.029(2) 0.030(2) 0.024(2) -0.0005(16) 0.0053(17) 0.0022(16) N3 0.026(2) 0.027(2) 0.031(2) 0.0023(17) 0.0076(17) -0.0047(16) C1 0.049(3) 0.049(3) 0.038(3) -0.010(3) 0.004(3) -0.015(3) C2 0.051(3) 0.030(3) 0.065(4) 0.006(3) 0.019(3) -0.005(2) C3 0.032(3) 0.044(3) 0.058(4) 0.000(3) 0.013(3) -0.007(2) C4 0.045(3) 0.045(3) 0.038(3) 0.001(2) 0.018(3) 0.010(2) C5 0.035(3) 0.039(3) 0.037(3) 0.003(2) 0.010(2) 0.014(2) C6 0.028(3) 0.041(3) 0.063(4) 0.005(3) 0.010(3) 0.001(2) C7 0.068(4) 0.065(4) 0.047(4) 0.015(3) 0.032(3) 0.006(3) C8 0.060(4) 0.061(4) 0.030(3) 0.007(3) 0.011(3) 0.025(3) C9 0.064(4) 0.063(4) 0.035(3) -0.007(3) 0.007(3) 0.008(3) C10 0.077(4) 0.052(4) 0.055(4) -0.012(3) 0.020(3) 0.022(3) C11 0.049(3) 0.036(3) 0.052(3) 0.009(3) 0.008(3) 0.007(2) C12 0.036(3) 0.058(4) 0.049(3) 0.008(3) 0.017(3) 0.011(3) C13 0.035(3) 0.038(3) 0.054(3) 0.005(3) 0.001(3) -0.009(2) C14 0.050(3) 0.031(3) 0.069(4) -0.004(3) 0.020(3) -0.009(2) C15 0.052(4) 0.064(4) 0.036(3) -0.008(3) 0.002(3) -0.022(3) C16 0.078(5) 0.102(5) 0.043(4) -0.009(4) 0.032(3) -0.041(4) C17 0.073(4) 0.065(4) 0.040(3) 0.014(3) 0.000(3) 0.013(3) C18 0.067(4) 0.049(3) 0.038(3) -0.009(3) 0.015(3) -0.006(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce O 1.948(4) . ? Ce N3 2.304(3) . ? Ce N1 2.315(3) . ? Ce N2 2.320(4) . ? Na O 2.282(5) 3_666 ? Na O 2.287(5) . ? Si1 N1 1.716(4) . ? Si1 C2 1.873(5) . ? Si1 C1 1.876(5) . ? Si1 C3 1.879(5) . ? Si2 N1 1.725(4) . ? Si2 C4 1.867(5) . ? Si2 C5 1.868(5) . ? Si2 C6 1.870(5) . ? Si3 N2 1.722(4) . ? Si3 C8 1.860(5) . ? Si3 C9 1.862(6) . ? Si3 C7 1.872(6) . ? Si4 N2 1.719(4) . ? Si4 C12 1.871(6) . ? Si4 C10 1.880(5) . ? Si4 C11 1.887(5) . ? Si5 N3 1.726(4) . ? Si5 C15 1.874(5) . ? Si5 C13 1.875(5) . ? Si5 C14 1.881(5) . ? Si6 N3 1.726(4) . ? Si6 C18 1.864(5) . ? Si6 C16 1.875(6) . ? Si6 C17 1.876(6) . ? O Na 2.282(5) 3_666 ? 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 O Ce N3 100.69(18) . . ? O Ce N1 100.85(15) . . ? N3 Ce N1 118.79(13) . . ? O Ce N2 97.9(2) . . ? N3 Ce N2 116.75(13) . . ? N1 Ce N2 115.88(12) . . ? O Na O 95.46(15) 3_666 . ? N1 Si1 C2 115.3(2) . . ? N1 Si1 C1 111.3(2) . . ? C2 Si1 C1 104.9(3) . . ? N1 Si1 C3 110.4(2) . . ? C2 Si1 C3 105.0(3) . . ? C1 Si1 C3 109.6(3) . . ? N1 Si2 C4 112.1(2) . . ? N1 Si2 C5 113.5(2) . . ? C4 Si2 C5 109.1(2) . . ? N1 Si2 C6 109.2(2) . . ? C4 Si2 C6 107.4(3) . . ? C5 Si2 C6 105.1(2) . . ? N2 Si3 C8 109.7(2) . . ? N2 Si3 C9 115.0(2) . . ? C8 Si3 C9 105.2(3) . . ? N2 Si3 C7 111.9(2) . . ? C8 Si3 C7 107.5(3) . . ? C9 Si3 C7 107.2(3) . . ? N2 Si4 C12 111.9(2) . . ? N2 Si4 C10 115.3(2) . . ? C12 Si4 C10 105.3(3) . . ? N2 Si4 C11 110.1(2) . . ? C12 Si4 C11 109.3(3) . . ? C10 Si4 C11 104.4(3) . . ? N3 Si5 C15 110.0(2) . . ? N3 Si5 C13 113.6(2) . . ? C15 Si5 C13 104.9(3) . . ? N3 Si5 C14 111.9(2) . . ? C15 Si5 C14 107.1(3) . . ? C13 Si5 C14 108.9(2) . . ? N3 Si6 C18 110.5(2) . . ? N3 Si6 C16 114.6(2) . . ? C18 Si6 C16 105.8(3) . . ? N3 Si6 C17 111.7(2) . . ? C18 Si6 C17 107.5(3) . . ? C16 Si6 C17 106.3(3) . . ? Ce O Na 135.2(2) . 3_666 ? Ce O Na 138.7(2) . . ? Na O Na 84.54(15) 3_666 . ? Si1 N1 Si2 121.7(2) . . ? Si1 N1 Ce 119.10(18) . . ? Si2 N1 Ce 118.99(18) . . ? Si4 N2 Si3 121.8(2) . . ? Si4 N2 Ce 116.55(18) . . ? Si3 N2 Ce 121.27(19) . . ? Si6 N3 Si5 121.6(2) . . ? Si6 N3 Ce 118.45(18) . . ? Si5 N3 Ce 119.88(19) . . ? #===END data_(7)-mar1904 _database_code_depnum_ccdc_archive 'CCDC 774597' #TrackingRef '- mfl_28jul2009.CIF' _audit_creation_date 2004-03-22T09:23:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H108 Ce2 K2 N6 O2 Si12' _chemical_formula_sum 'C36 H108 Ce2 K2 N6 O2 Si12' _chemical_formula_weight 1352.8 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 15.8871(5) _cell_length_b 18.4094(4) _cell_length_c 12.4629(4) _cell_angle_alpha 90 _cell_angle_beta 107.904(1) _cell_angle_gamma 90 _cell_volume 3468.53(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16925 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5783 _exptl_absorpt_correction_T_max 0.6255 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.231038E-1 _diffrn_orient_matrix_ub_12 0.18015E-2 _diffrn_orient_matrix_ub_13 0.660711E-1 _diffrn_orient_matrix_ub_21 -0.809024E-1 _diffrn_orient_matrix_ub_22 -0.32249E-2 _diffrn_orient_matrix_ub_23 -0.21661E-2 _diffrn_orient_matrix_ub_31 0.55823E-2 _diffrn_orient_matrix_ub_32 -0.541943E-1 _diffrn_orient_matrix_ub_33 0.23252E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_unetI/netI 0.0448 _diffrn_reflns_number 27223 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 24.92 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 5911 _reflns_number_gt 4741 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0241P)^2^+6.7323P] 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_number_reflns 5911 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.071 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.368 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.091 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' K K 0.2009 0.2494 '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 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce Ce 0.731713(14) 0.494256(11) 0.707314(18) 0.01911(8) Uani 1 1 d . . . K K 0.48371(7) 0.40323(6) 0.51776(10) 0.0509(3) Uani 1 1 d . . . Si1 Si 0.68616(8) 0.30748(6) 0.68913(10) 0.0262(3) Uani 1 1 d . . . Si2 Si 0.87756(7) 0.34822(6) 0.74139(10) 0.0251(3) Uani 1 1 d . . . Si3 Si 0.72082(8) 0.50423(6) 0.98605(9) 0.0297(3) Uani 1 1 d . . . Si4 Si 0.59938(8) 0.60368(7) 0.81580(10) 0.0325(3) Uani 1 1 d . . . Si5 Si 0.87847(8) 0.63632(6) 0.70951(11) 0.0320(3) Uani 1 1 d . . . Si6 Si 0.79286(8) 0.56794(7) 0.48273(10) 0.0319(3) Uani 1 1 d . . . O O 0.6193(2) 0.49261(16) 0.5937(3) 0.0525(10) Uani 1 1 d . . . N1 N 0.7681(2) 0.37125(16) 0.7176(3) 0.0213(7) Uani 1 1 d . . . N2 N 0.6818(2) 0.54002(18) 0.8525(3) 0.0257(8) Uani 1 1 d . . . N3 N 0.8072(2) 0.57357(17) 0.6250(3) 0.0263(8) Uani 1 1 d . . . C1 C 0.6381(3) 0.2916(3) 0.5325(4) 0.0401(12) Uani 1 1 d . . . H1C H 0.5925 0.2539 0.5186 0.06 Uiso 1 1 calc R . . H1B H 0.6851 0.2759 0.5019 0.06 Uiso 1 1 calc R . . H1A H 0.6118 0.3368 0.4955 0.06 Uiso 1 1 calc R . . C2 C 0.7196(3) 0.2149(2) 0.7503(4) 0.0423(12) Uani 1 1 d . . . H2C H 0.6674 0.1835 0.733 0.064 Uiso 1 1 calc R . . H2B H 0.7458 0.2189 0.8322 0.064 Uiso 1 1 calc R . . H2A H 0.763 0.1942 0.7176 0.064 Uiso 1 1 calc R . . C3 C 0.5977(3) 0.3370(2) 0.7509(4) 0.0336(10) Uani 1 1 d . . . H3C H 0.5705 0.382 0.7145 0.05 Uiso 1 1 calc R . . H3B H 0.6239 0.3453 0.8321 0.05 Uiso 1 1 calc R . . H3A H 0.5525 0.299 0.7385 0.05 Uiso 1 1 calc R . . C4 C 0.8939(3) 0.2975(2) 0.6194(4) 0.0402(12) Uani 1 1 d . . . H4C H 0.8746 0.3278 0.5515 0.06 Uiso 1 1 calc R . . H4B H 0.859 0.2527 0.6072 0.06 Uiso 1 1 calc R . . H4A H 0.9567 0.2856 0.6354 0.06 Uiso 1 1 calc R . . C5 C 0.9261(3) 0.2947(2) 0.8733(4) 0.0365(11) Uani 1 1 d . . . H5C H 0.9883 0.2839 0.882 0.055 Uiso 1 1 calc R . . H5B H 0.8933 0.2491 0.8688 0.055 Uiso 1 1 calc R . . H5A H 0.9222 0.3229 0.9383 0.055 Uiso 1 1 calc R . . C6 C 0.9457(3) 0.4326(2) 0.7592(4) 0.0417(12) Uani 1 1 d . . . H6C H 0.9424 0.459 0.826 0.063 Uiso 1 1 calc R . . H6B H 0.923 0.4635 0.6924 0.063 Uiso 1 1 calc R . . H6A H 1.0073 0.4197 0.7684 0.063 Uiso 1 1 calc R . . C7 C 0.6311(3) 0.4591(3) 1.0301(4) 0.0514(14) Uani 1 1 d . . . H7C H 0.6059 0.4192 0.9782 0.077 Uiso 1 1 calc R . . H7B H 0.5847 0.4946 1.0284 0.077 Uiso 1 1 calc R . . H7A H 0.6558 0.44 1.1068 0.077 Uiso 1 1 calc R . . C8 C 0.8067(3) 0.4338(3) 0.9918(4) 0.0446(12) Uani 1 1 d . . . H8C H 0.8298 0.4149 1.0688 0.067 Uiso 1 1 calc R . . H8B H 0.855 0.4555 0.9692 0.067 Uiso 1 1 calc R . . H8A H 0.7802 0.394 0.9402 0.067 Uiso 1 1 calc R . . C9 C 0.7758(4) 0.5714(3) 1.0982(4) 0.0520(14) Uani 1 1 d . . . H9C H 0.7322 0.6071 1.1055 0.078 Uiso 1 1 calc R . . H9B H 0.8232 0.5962 1.0777 0.078 Uiso 1 1 calc R . . H9A H 0.8007 0.546 1.1701 0.078 Uiso 1 1 calc R . . C10 C 0.5851(4) 0.6605(3) 0.9341(5) 0.0610(16) Uani 1 1 d . . . H10C H 0.6399 0.6871 0.9702 0.092 Uiso 1 1 calc R . . H10B H 0.5712 0.629 0.9898 0.092 Uiso 1 1 calc R . . H10A H 0.5366 0.6951 0.9042 0.092 Uiso 1 1 calc R . . C11 C 0.6235(3) 0.6726(2) 0.7169(4) 0.0411(12) Uani 1 1 d . . . H11C H 0.5734 0.7061 0.6906 0.062 Uiso 1 1 calc R . . H11B H 0.6328 0.6475 0.6521 0.062 Uiso 1 1 calc R . . H11A H 0.6769 0.7 0.7566 0.062 Uiso 1 1 calc R . . C12 C 0.4883(3) 0.5610(3) 0.7466(4) 0.0475(13) Uani 1 1 d . . . H12C H 0.4714 0.5311 0.8017 0.071 Uiso 1 1 calc R . . H12B H 0.4916 0.5305 0.6835 0.071 Uiso 1 1 calc R . . H12A H 0.444 0.5992 0.7184 0.071 Uiso 1 1 calc R . . C13 C 0.9976(3) 0.6223(2) 0.7202(4) 0.0423(12) Uani 1 1 d . . . H13C H 1.0058 0.6309 0.6464 0.063 Uiso 1 1 calc R . . H13B H 1.015 0.5724 0.7443 0.063 Uiso 1 1 calc R . . H13A H 1.0344 0.6564 0.7754 0.063 Uiso 1 1 calc R . . C14 C 0.8460(3) 0.7316(2) 0.6621(5) 0.0476(13) Uani 1 1 d . . . H14C H 0.8829 0.7657 0.7168 0.071 Uiso 1 1 calc R . . H14B H 0.7837 0.7393 0.6563 0.071 Uiso 1 1 calc R . . H14A H 0.8542 0.7395 0.5882 0.071 Uiso 1 1 calc R . . C15 C 0.8751(3) 0.6290(3) 0.8579(4) 0.0493(13) Uani 1 1 d . . . H15C H 0.8963 0.5809 0.8881 0.074 Uiso 1 1 calc R . . H15B H 0.8142 0.6357 0.8591 0.074 Uiso 1 1 calc R . . H15A H 0.913 0.6665 0.9043 0.074 Uiso 1 1 calc R . . C16 C 0.8891(4) 0.5999(4) 0.4392(5) 0.0685(18) Uani 1 1 d . . . H16C H 0.9405 0.5692 0.4743 0.103 Uiso 1 1 calc R . . H16B H 0.9028 0.6503 0.4633 0.103 Uiso 1 1 calc R . . H16A H 0.8744 0.5969 0.3569 0.103 Uiso 1 1 calc R . . C17 C 0.6953(4) 0.6226(3) 0.3967(5) 0.0669(17) Uani 1 1 d . . . H17C H 0.6907 0.6188 0.3167 0.1 Uiso 1 1 calc R . . H17B H 0.7034 0.6736 0.4202 0.1 Uiso 1 1 calc R . . H17A H 0.6411 0.6038 0.4085 0.1 Uiso 1 1 calc R . . C18 C 0.7719(4) 0.4723(3) 0.4333(4) 0.0609(16) Uani 1 1 d . . . H18C H 0.7583 0.4708 0.3511 0.091 Uiso 1 1 calc R . . H18B H 0.7217 0.453 0.4544 0.091 Uiso 1 1 calc R . . H18A H 0.8246 0.4429 0.4684 0.091 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.01734(12) 0.01956(13) 0.01948(12) 0.00083(9) 0.00423(9) 0.00014(10) K 0.0359(6) 0.0391(6) 0.0607(8) 0.0116(5) -0.0104(5) -0.0045(5) Si1 0.0283(6) 0.0233(6) 0.0264(6) -0.0013(5) 0.0076(5) -0.0032(5) Si2 0.0237(6) 0.0255(6) 0.0259(6) 0.0015(5) 0.0075(5) 0.0053(5) Si3 0.0326(6) 0.0365(7) 0.0193(6) -0.0005(5) 0.0067(5) 0.0068(6) Si4 0.0338(7) 0.0353(7) 0.0280(7) -0.0015(5) 0.0091(6) 0.0100(5) Si5 0.0289(7) 0.0291(7) 0.0339(7) 0.0004(5) 0.0039(6) -0.0104(5) Si6 0.0322(7) 0.0369(7) 0.0265(7) 0.0044(5) 0.0088(6) -0.0056(5) O 0.0388(19) 0.0281(18) 0.065(2) 0.0155(16) -0.0219(17) -0.0087(15) N1 0.0212(17) 0.0202(17) 0.0211(18) 0.0029(13) 0.0046(14) 0.0025(14) N2 0.0254(18) 0.0290(19) 0.0211(19) -0.0017(14) 0.0049(15) 0.0042(15) N3 0.0241(18) 0.0260(19) 0.0263(19) 0.0013(15) 0.0042(15) -0.0063(15) C1 0.040(3) 0.048(3) 0.029(3) -0.008(2) 0.007(2) -0.013(2) C2 0.047(3) 0.029(3) 0.051(3) 0.001(2) 0.016(3) -0.003(2) C3 0.031(2) 0.040(3) 0.030(3) 0.004(2) 0.011(2) -0.004(2) C4 0.047(3) 0.041(3) 0.036(3) 0.004(2) 0.018(2) 0.017(2) C5 0.034(3) 0.041(3) 0.032(3) 0.003(2) 0.006(2) 0.014(2) C6 0.023(2) 0.041(3) 0.056(3) 0.004(2) 0.005(2) 0.000(2) C7 0.057(3) 0.063(3) 0.042(3) 0.012(3) 0.027(3) 0.007(3) C8 0.047(3) 0.057(3) 0.026(3) 0.005(2) 0.006(2) 0.022(2) C9 0.062(4) 0.060(3) 0.026(3) -0.008(2) 0.002(3) 0.004(3) C10 0.081(4) 0.055(3) 0.049(3) -0.006(3) 0.023(3) 0.032(3) C11 0.043(3) 0.032(3) 0.043(3) 0.004(2) 0.006(2) 0.007(2) C12 0.032(3) 0.066(3) 0.049(3) 0.008(3) 0.018(2) 0.011(2) C13 0.030(3) 0.037(3) 0.052(3) 0.002(2) 0.001(2) -0.011(2) C14 0.043(3) 0.032(3) 0.067(4) -0.002(2) 0.016(3) -0.009(2) C15 0.044(3) 0.059(3) 0.036(3) -0.009(2) -0.002(2) -0.023(3) C16 0.065(4) 0.110(5) 0.039(3) -0.011(3) 0.028(3) -0.035(4) C17 0.069(4) 0.087(4) 0.038(3) 0.023(3) 0.007(3) 0.018(3) C18 0.096(5) 0.050(3) 0.035(3) -0.009(2) 0.016(3) -0.010(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce O 1.908(3) . ? Ce N3 2.319(3) . ? Ce N1 2.331(3) . ? Ce N2 2.344(3) . ? K O 2.624(3) 3_666 ? K O 2.644(3) . ? Si1 N1 1.708(3) . ? Si1 C2 1.875(4) . ? Si1 C3 1.879(4) . ? Si1 C1 1.888(4) . ? Si2 N1 1.724(3) . ? Si2 C6 1.867(4) . ? Si2 C5 1.868(4) . ? Si2 C4 1.869(4) . ? Si3 N2 1.718(3) . ? Si3 C8 1.868(4) . ? Si3 C9 1.869(5) . ? Si3 C7 1.871(5) . ? Si4 N2 1.712(3) . ? Si4 C10 1.878(5) . ? Si4 C12 1.881(5) . ? Si4 C11 1.889(5) . ? Si5 N3 1.730(3) . ? Si5 C14 1.872(5) . ? Si5 C15 1.872(5) . ? Si5 C13 1.874(5) . ? Si6 N3 1.720(4) . ? Si6 C18 1.861(5) . ? Si6 C16 1.867(5) . ? Si6 C17 1.881(5) . ? O K 2.624(3) 3_666 ? 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 O Ce N3 100.07(13) . . ? O Ce N1 100.68(12) . . ? N3 Ce N1 118.86(11) . . ? O Ce N2 96.73(15) . . ? N3 Ce N2 117.30(11) . . ? N1 Ce N2 116.34(11) . . ? O K O 92.39(10) 3_666 . ? N1 Si1 C2 115.95(19) . . ? N1 Si1 C3 109.56(18) . . ? C2 Si1 C3 104.5(2) . . ? N1 Si1 C1 111.19(18) . . ? C2 Si1 C1 104.7(2) . . ? C3 Si1 C1 110.7(2) . . ? N1 Si2 C6 109.43(18) . . ? N1 Si2 C5 113.74(18) . . ? C6 Si2 C5 105.5(2) . . ? N1 Si2 C4 111.59(19) . . ? C6 Si2 C4 107.0(2) . . ? C5 Si2 C4 109.2(2) . . ? N2 Si3 C8 110.17(19) . . ? N2 Si3 C9 114.6(2) . . ? C8 Si3 C9 105.2(2) . . ? N2 Si3 C7 112.0(2) . . ? C8 Si3 C7 107.1(2) . . ? C9 Si3 C7 107.3(2) . . ? N2 Si4 C10 116.0(2) . . ? N2 Si4 C12 111.7(2) . . ? C10 Si4 C12 105.7(3) . . ? N2 Si4 C11 110.02(19) . . ? C10 Si4 C11 103.6(2) . . ? C12 Si4 C11 109.3(2) . . ? N3 Si5 C14 111.6(2) . . ? N3 Si5 C15 109.95(19) . . ? C14 Si5 C15 106.9(2) . . ? N3 Si5 C13 114.2(2) . . ? C14 Si5 C13 109.0(2) . . ? C15 Si5 C13 104.8(2) . . ? N3 Si6 C18 110.6(2) . . ? N3 Si6 C16 114.9(2) . . ? C18 Si6 C16 106.3(3) . . ? N3 Si6 C17 112.3(2) . . ? C18 Si6 C17 106.5(3) . . ? C16 Si6 C17 105.7(3) . . ? Ce O K 132.10(14) . 3_666 ? Ce O K 138.53(14) . . ? K O K 87.61(10) 3_666 . ? Si1 N1 Si2 122.06(18) . . ? Si1 N1 Ce 119.73(16) . . ? Si2 N1 Ce 117.94(16) . . ? Si4 N2 Si3 122.68(19) . . ? Si4 N2 Ce 116.87(17) . . ? Si3 N2 Ce 120.21(16) . . ? Si6 N3 Si5 121.46(19) . . ? Si6 N3 Ce 119.72(17) . . ? Si5 N3 Ce 118.81(17) . . ? #===END data_(8)-mar1104 _database_code_depnum_ccdc_archive 'CCDC 774598' #TrackingRef '- mfl_28jul2009.CIF' _audit_creation_date 2004-03-16T11:01:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C60 H180 Ce4 K2 N10 O4 Si20, C12 H28' _chemical_formula_sum 'C72 H208 Ce4 K2 N10 O4 Si20' _chemical_formula_weight 2478.96 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.0329(3) _cell_length_b 15.0799(2) _cell_length_c 16.5110(2) _cell_angle_alpha 65.813(1) _cell_angle_beta 71.175(1) _cell_angle_gamma 81.622(1) _cell_volume 3231.34(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34171 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5465 _exptl_absorpt_correction_T_max 0.6509 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.73885E-2 _diffrn_orient_matrix_ub_12 -0.690374E-1 _diffrn_orient_matrix_ub_13 0.104583E-1 _diffrn_orient_matrix_ub_21 -0.186376E-1 _diffrn_orient_matrix_ub_22 0.226619E-1 _diffrn_orient_matrix_ub_23 -0.583513E-1 _diffrn_orient_matrix_ub_31 0.673687E-1 _diffrn_orient_matrix_ub_32 -0.24872E-2 _diffrn_orient_matrix_ub_33 -0.360974E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_unetI/netI 0.034 _diffrn_reflns_number 48884 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.69 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.949 _diffrn_measured_fraction_theta_max 0.949 _reflns_number_total 11665 _reflns_number_gt 10199 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The molecule of hexane solvate is poorly defined and was included with isotropic C atoms and SADI constraints. 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^)+(0.0305P)^2^+5.9499P] 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_number_reflns 11665 _refine_ls_number_parameters 475 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.849 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.084 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.436552(12) 0.970573(13) 0.233929(11) 0.01874(6) Uani 1 1 d . . . Ce2 Ce 0.232079(12) 0.747364(13) 0.364636(12) 0.02049(6) Uani 1 1 d . . . K K 0.62810(5) 0.97646(6) 0.01670(5) 0.03207(18) Uani 1 1 d . . . Si1 Si 0.63811(7) 0.82282(7) 0.24738(7) 0.0289(2) Uani 1 1 d . . . Si2 Si 0.67424(7) 1.03337(8) 0.19611(7) 0.0298(2) Uani 1 1 d . . . Si3 Si 0.34640(7) 1.22009(7) 0.17645(7) 0.0278(2) Uani 1 1 d . . . Si4 Si 0.36776(7) 1.09519(7) 0.36843(6) 0.0283(2) Uani 1 1 d . . . Si5 Si 0.09823(7) 0.94499(7) 0.27718(7) 0.0283(2) Uani 1 1 d . . . Si6 Si 0.03166(7) 0.76327(8) 0.28536(8) 0.0346(2) Uani 1 1 d . . . Si7 Si 0.08950(8) 0.70079(8) 0.59854(7) 0.0378(3) Uani 1 1 d . . . Si8 Si 0.29577(8) 0.65964(8) 0.56644(7) 0.0358(2) Uani 1 1 d . . . Si9 Si 0.28735(8) 0.50567(7) 0.38017(7) 0.0330(2) Uani 1 1 d . . . Si10 Si 0.33220(8) 0.65808(7) 0.18891(7) 0.0307(2) Uani 1 1 d . . . O1 O 0.32681(15) 0.85250(16) 0.30692(15) 0.0249(5) Uani 1 1 d . . . O2 O 0.45067(16) 0.99571(17) 0.11030(15) 0.0260(5) Uani 1 1 d . . . N1 N 0.60277(19) 0.9425(2) 0.21618(18) 0.0242(6) Uani 1 1 d . . . N2 N 0.37518(19) 1.11226(19) 0.25657(18) 0.0232(6) Uani 1 1 d . . . N3 N 0.10839(19) 0.8205(2) 0.30680(19) 0.0261(6) Uani 1 1 d . . . N4 N 0.2004(2) 0.6982(2) 0.52250(19) 0.0279(6) Uani 1 1 d . . . N5 N 0.2894(2) 0.62785(19) 0.30730(19) 0.0249(6) Uani 1 1 d . . . C1 C 0.5525(3) 0.7553(3) 0.2326(3) 0.0382(9) Uani 1 1 d . . . H1A H 0.4903 0.7573 0.2755 0.057 Uiso 1 1 calc R . . H1B H 0.5737 0.6875 0.2459 0.057 Uiso 1 1 calc R . . H1C H 0.549 0.7859 0.1686 0.057 Uiso 1 1 calc R . . C2 C 0.6452(3) 0.7659(3) 0.3689(3) 0.0455(11) Uani 1 1 d . . . H2A H 0.6662 0.698 0.3829 0.068 Uiso 1 1 calc R . . H2B H 0.5831 0.7684 0.4118 0.068 Uiso 1 1 calc R . . H2C H 0.6901 0.8013 0.3759 0.068 Uiso 1 1 calc R . . C3 C 0.7545(3) 0.7982(3) 0.1716(3) 0.0538(12) Uani 1 1 d . . . H3A H 0.7651 0.7278 0.1902 0.081 Uiso 1 1 calc R . . H3B H 0.805 0.8266 0.1784 0.081 Uiso 1 1 calc R . . H3C H 0.7541 0.8273 0.1066 0.081 Uiso 1 1 calc R . . C4 C 0.7917(3) 1.0389(4) 0.1075(3) 0.0575(13) Uani 1 1 d . . . H4A H 0.8281 1.0922 0.0998 0.086 Uiso 1 1 calc R . . H4B H 0.7823 1.0501 0.048 0.086 Uiso 1 1 calc R . . H4C H 0.8259 0.9773 0.1285 0.086 Uiso 1 1 calc R . . C5 C 0.6998(3) 1.0252(3) 0.3026(3) 0.0511(11) Uani 1 1 d . . . H5A H 0.6409 1.0311 0.3482 0.077 Uiso 1 1 calc R . . H5B H 0.7417 1.0779 0.2862 0.077 Uiso 1 1 calc R . . H5C H 0.7301 0.9624 0.3292 0.077 Uiso 1 1 calc R . . C6 C 0.6173(3) 1.1544(3) 0.1479(3) 0.0442(10) Uani 1 1 d . . . H6A H 0.6599 1.206 0.1325 0.066 Uiso 1 1 calc R . . H6B H 0.5588 1.1598 0.1941 0.066 Uiso 1 1 calc R . . H6C H 0.6033 1.1607 0.0917 0.066 Uiso 1 1 calc R . . C7 C 0.3630(3) 1.2114(3) 0.0622(2) 0.0372(9) Uani 1 1 d . . . H7A H 0.3491 1.2748 0.0178 0.056 Uiso 1 1 calc R . . H7B H 0.3204 1.1628 0.0708 0.056 Uiso 1 1 calc R . . H7C H 0.4281 1.1922 0.0383 0.056 Uiso 1 1 calc R . . C8 C 0.4205(3) 1.3254(3) 0.1468(3) 0.0431(10) Uani 1 1 d . . . H8A H 0.4088 1.3404 0.2018 0.065 Uiso 1 1 calc R . . H8B H 0.4042 1.3824 0.0971 0.065 Uiso 1 1 calc R . . H8C H 0.487 1.3085 0.1259 0.065 Uiso 1 1 calc R . . C9 C 0.2208(3) 1.2572(3) 0.2157(3) 0.0447(10) Uani 1 1 d . . . H9A H 0.2059 1.3146 0.1656 0.067 Uiso 1 1 calc R . . H9B H 0.2107 1.2727 0.2702 0.067 Uiso 1 1 calc R . . H9C H 0.1799 1.2038 0.232 0.067 Uiso 1 1 calc R . . C10 C 0.4093(3) 0.9662(3) 0.4257(2) 0.0402(10) Uani 1 1 d . . . H10A H 0.4033 0.9525 0.4906 0.06 Uiso 1 1 calc R . . H10B H 0.4752 0.9586 0.393 0.06 Uiso 1 1 calc R . . H10C H 0.3708 0.9207 0.4232 0.06 Uiso 1 1 calc R . . C11 C 0.2477(3) 1.1064(3) 0.4444(3) 0.0452(10) Uani 1 1 d . . . H11A H 0.2262 1.1744 0.4228 0.068 Uiso 1 1 calc R . . H11B H 0.2496 1.0851 0.5085 0.068 Uiso 1 1 calc R . . H11C H 0.2043 1.0657 0.442 0.068 Uiso 1 1 calc R . . C12 C 0.4449(3) 1.1751(3) 0.3777(3) 0.0470(11) Uani 1 1 d . . . H12A H 0.4449 1.1529 0.4424 0.07 Uiso 1 1 calc R . . H12B H 0.4211 1.2423 0.357 0.07 Uiso 1 1 calc R . . H12C H 0.5091 1.172 0.3386 0.07 Uiso 1 1 calc R . . C13 C 0.1816(3) 1.0104(3) 0.1602(3) 0.0400(9) Uani 1 1 d . . . H13A H 0.1801 1.0799 0.1476 0.06 Uiso 1 1 calc R . . H13B H 0.1628 1.0011 0.1126 0.06 Uiso 1 1 calc R . . H13C H 0.2454 0.9843 0.1592 0.06 Uiso 1 1 calc R . . C14 C 0.1268(3) 0.9751(3) 0.3653(3) 0.0430(10) Uani 1 1 d . . . H14A H 0.0788 0.9481 0.4252 0.065 Uiso 1 1 calc R . . H14B H 0.1281 1.0459 0.345 0.065 Uiso 1 1 calc R . . H14C H 0.1884 0.9471 0.3717 0.065 Uiso 1 1 calc R . . C15 C -0.0200(3) 1.0014(3) 0.2702(3) 0.0461(10) Uani 1 1 d . . . H15A H -0.0361 0.9925 0.2211 0.069 Uiso 1 1 calc R . . H15B H -0.0184 1.0711 0.256 0.069 Uiso 1 1 calc R . . H15C H -0.0673 0.9703 0.3297 0.069 Uiso 1 1 calc R . . C16 C -0.0957(3) 0.7794(3) 0.3418(3) 0.0509(11) Uani 1 1 d . . . H16A H -0.1082 0.7511 0.4093 0.076 Uiso 1 1 calc R . . H16B H -0.1337 0.7468 0.3241 0.076 Uiso 1 1 calc R . . H16C H -0.112 0.8489 0.3214 0.076 Uiso 1 1 calc R . . C17 C 0.0457(3) 0.8096(4) 0.1579(3) 0.0543(12) Uani 1 1 d . . . H17A H -0.0006 0.7789 0.1477 0.081 Uiso 1 1 calc R . . H17B H 0.1092 0.7939 0.1257 0.081 Uiso 1 1 calc R . . H17C H 0.0357 0.8803 0.1337 0.081 Uiso 1 1 calc R . . C18 C 0.0511(3) 0.6287(3) 0.3313(3) 0.0489(11) Uani 1 1 d . . . H18A H 0.1148 0.6133 0.2994 0.073 Uiso 1 1 calc R . . H18B H 0.0053 0.5979 0.3206 0.073 Uiso 1 1 calc R . . H18C H 0.0433 0.6044 0.398 0.073 Uiso 1 1 calc R . . C19 C -0.0023(3) 0.7059(4) 0.5451(3) 0.0625(14) Uani 1 1 d . . . H19A H -0.0642 0.7112 0.5872 0.094 Uiso 1 1 calc R . . H19B H 0.001 0.6467 0.5335 0.094 Uiso 1 1 calc R . . H19C H 0.0074 0.7627 0.4863 0.094 Uiso 1 1 calc R . . C20 C 0.0643(4) 0.5899(4) 0.7091(3) 0.0638(14) Uani 1 1 d . . . H20C H 0.0016 0.5964 0.7493 0.096 Uiso 1 1 calc R . . H20B H 0.1114 0.5831 0.7409 0.096 Uiso 1 1 calc R . . H20A H 0.0667 0.5323 0.6951 0.096 Uiso 1 1 calc R . . C21 C 0.0727(4) 0.8081(4) 0.6319(4) 0.0721(16) Uani 1 1 d . . . H21A H 0.0106 0.8052 0.6767 0.108 Uiso 1 1 calc R . . H21B H 0.0772 0.8681 0.5765 0.108 Uiso 1 1 calc R . . H21C H 0.1214 0.807 0.6599 0.108 Uiso 1 1 calc R . . C22 C 0.2993(3) 0.5268(3) 0.6425(3) 0.0568(13) Uani 1 1 d . . . H22A H 0.3565 0.5123 0.6623 0.085 Uiso 1 1 calc R . . H22B H 0.2993 0.4876 0.6076 0.085 Uiso 1 1 calc R . . H22C H 0.244 0.5114 0.6972 0.085 Uiso 1 1 calc R . . C23 C 0.3089(4) 0.7279(4) 0.6341(3) 0.0629(14) Uani 1 1 d . . . H23A H 0.3165 0.7972 0.5943 0.094 Uiso 1 1 calc R . . H23B H 0.3643 0.7033 0.6562 0.094 Uiso 1 1 calc R . . H23C H 0.2528 0.7191 0.6874 0.094 Uiso 1 1 calc R . . C24 C 0.4046(3) 0.6791(3) 0.4658(3) 0.0462(11) Uani 1 1 d . . . H24A H 0.4595 0.6548 0.4888 0.069 Uiso 1 1 calc R . . H24B H 0.4116 0.7487 0.427 0.069 Uiso 1 1 calc R . . H24C H 0.3997 0.644 0.4289 0.069 Uiso 1 1 calc R . . C25 C 0.4035(3) 0.4621(3) 0.4019(3) 0.0538(12) Uani 1 1 d . . . H25A H 0.4008 0.3923 0.4402 0.081 Uiso 1 1 calc R . . H25B H 0.4184 0.4972 0.4343 0.081 Uiso 1 1 calc R . . H25C H 0.4523 0.474 0.3426 0.081 Uiso 1 1 calc R . . C26 C 0.1937(3) 0.4832(3) 0.4928(3) 0.0452(10) Uani 1 1 d . . . H26A H 0.2079 0.5186 0.5252 0.068 Uiso 1 1 calc R . . H26B H 0.191 0.4134 0.5313 0.068 Uiso 1 1 calc R . . H26C H 0.1329 0.5057 0.4809 0.068 Uiso 1 1 calc R . . C27 C 0.2572(3) 0.4224(3) 0.3344(3) 0.0515(12) Uani 1 1 d . . . H27A H 0.1945 0.4394 0.3257 0.077 Uiso 1 1 calc R . . H27B H 0.2578 0.355 0.3787 0.077 Uiso 1 1 calc R . . H27C H 0.3036 0.4293 0.2747 0.077 Uiso 1 1 calc R . . C28 C 0.2568(4) 0.6221(3) 0.1363(3) 0.0523(12) Uani 1 1 d . . . H28A H 0.2546 0.551 0.1602 0.078 Uiso 1 1 calc R . . H28B H 0.2834 0.6479 0.0686 0.078 Uiso 1 1 calc R . . H28C H 0.193 0.6485 0.1526 0.078 Uiso 1 1 calc R . . C29 C 0.3394(3) 0.7940(3) 0.1273(2) 0.0382(9) Uani 1 1 d . . . H29A H 0.3592 0.8114 0.0601 0.057 Uiso 1 1 calc R . . H29B H 0.3852 0.8181 0.144 0.057 Uiso 1 1 calc R . . H29C H 0.2776 0.8234 0.1457 0.057 Uiso 1 1 calc R . . C30 C 0.4508(3) 0.6043(3) 0.1526(3) 0.0458(11) Uani 1 1 d . . . H30A H 0.4746 0.6306 0.0847 0.069 Uiso 1 1 calc R . . H30B H 0.4462 0.5335 0.1762 0.069 Uiso 1 1 calc R . . H30C H 0.494 0.6206 0.1779 0.069 Uiso 1 1 calc R . . C1A C 0.3051(10) 1.5413(10) -0.0939(10) 0.211(6) Uiso 1 1 d D . . H1A1 H 0.2996 1.5918 -0.0694 0.316 Uiso 1 1 calc R . . H1A2 H 0.3211 1.5713 -0.1618 0.316 Uiso 1 1 calc R . . H1A3 H 0.3546 1.4945 -0.0756 0.316 Uiso 1 1 calc R . . C2A C 0.2107(13) 1.4883(14) -0.0543(15) 0.340(11) Uiso 1 1 d D . . H2A1 H 0.1679 1.5457 -0.0601 0.408 Uiso 1 1 calc R . . H2A2 H 0.2079 1.4599 0.0121 0.408 Uiso 1 1 calc R . . C3A C 0.142(3) 1.416(4) -0.052(3) 1.51(12) Uiso 1 1 d D . . H3A1 H 0.1825 1.3964 -0.1024 1.811 Uiso 1 1 calc R . . H3A2 H 0.097 1.4634 -0.0798 1.811 Uiso 1 1 calc R . . C4A C 0.0761(12) 1.3229(15) 0.0065(16) 0.377(13) Uiso 1 1 d D . . H4A1 H 0.0989 1.2913 0.062 0.452 Uiso 1 1 calc R . . H4A2 H 0.1028 1.2825 -0.0303 0.452 Uiso 1 1 calc R . . C5A C -0.0314(13) 1.2902(11) 0.0493(12) 0.251(7) Uiso 1 1 d D . . H5A1 H -0.0373 1.2428 0.1136 0.302 Uiso 1 1 calc R . . H5A2 H -0.039 1.2527 0.0149 0.302 Uiso 1 1 calc R . . C6A C -0.1280(15) 1.3636(18) 0.0566(16) 0.405(14) Uiso 1 1 d D . . H6A1 H -0.1812 1.3321 0.0577 0.608 Uiso 1 1 calc R . . H6A2 H -0.1156 1.4255 0.0028 0.608 Uiso 1 1 calc R . . H6A3 H -0.143 1.3756 0.1136 0.608 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 0.01838(10) 0.02249(10) 0.01658(9) -0.00874(8) -0.00485(7) -0.00095(7) Ce2 0.01869(10) 0.02081(10) 0.02180(10) -0.00901(8) -0.00440(7) -0.00091(7) K 0.0273(4) 0.0493(5) 0.0213(4) -0.0153(4) -0.0081(3) 0.0017(3) Si1 0.0210(5) 0.0316(5) 0.0295(5) -0.0082(4) -0.0079(4) 0.0032(4) Si2 0.0239(5) 0.0398(6) 0.0305(5) -0.0171(5) -0.0074(4) -0.0053(4) Si3 0.0328(6) 0.0227(5) 0.0270(5) -0.0097(4) -0.0073(4) -0.0005(4) Si4 0.0349(6) 0.0316(5) 0.0241(5) -0.0163(4) -0.0085(4) -0.0006(4) Si5 0.0228(5) 0.0266(5) 0.0364(5) -0.0135(4) -0.0089(4) 0.0017(4) Si6 0.0249(5) 0.0351(6) 0.0483(6) -0.0168(5) -0.0139(5) -0.0041(4) Si7 0.0342(6) 0.0472(7) 0.0275(5) -0.0174(5) 0.0020(4) -0.0038(5) Si8 0.0361(6) 0.0371(6) 0.0281(5) -0.0021(5) -0.0120(4) -0.0087(5) Si9 0.0361(6) 0.0190(5) 0.0359(5) -0.0083(4) -0.0027(5) -0.0015(4) Si10 0.0379(6) 0.0273(5) 0.0276(5) -0.0146(4) -0.0034(4) -0.0046(4) O1 0.0241(13) 0.0262(12) 0.0248(12) -0.0105(10) -0.0060(10) -0.0024(10) O2 0.0246(13) 0.0345(13) 0.0192(11) -0.0106(10) -0.0074(9) 0.0013(10) N1 0.0195(15) 0.0310(16) 0.0220(14) -0.0092(12) -0.0077(11) 0.0006(12) N2 0.0269(15) 0.0232(14) 0.0224(14) -0.0113(12) -0.0078(12) 0.0001(12) N3 0.0207(15) 0.0259(15) 0.0316(15) -0.0103(13) -0.0083(12) -0.0009(12) N4 0.0279(16) 0.0281(16) 0.0252(15) -0.0097(13) -0.0037(12) -0.0046(12) N5 0.0254(15) 0.0225(14) 0.0266(15) -0.0112(12) -0.0045(12) -0.0012(12) C1 0.045(2) 0.028(2) 0.039(2) -0.0104(17) -0.0126(18) 0.0000(17) C2 0.034(2) 0.049(3) 0.043(2) 0.000(2) -0.0194(19) -0.0041(19) C3 0.036(2) 0.048(3) 0.063(3) -0.020(2) -0.003(2) 0.010(2) C4 0.035(3) 0.071(3) 0.069(3) -0.038(3) 0.006(2) -0.022(2) C5 0.059(3) 0.063(3) 0.054(3) -0.033(2) -0.032(2) 0.001(2) C6 0.051(3) 0.036(2) 0.042(2) -0.0109(19) -0.010(2) -0.0107(19) C7 0.049(3) 0.029(2) 0.0299(19) -0.0079(16) -0.0127(18) 0.0001(17) C8 0.052(3) 0.026(2) 0.049(2) -0.0130(18) -0.014(2) -0.0019(18) C9 0.043(3) 0.038(2) 0.045(2) -0.0125(19) -0.0114(19) 0.0075(19) C10 0.063(3) 0.039(2) 0.0231(18) -0.0147(17) -0.0167(18) 0.005(2) C11 0.047(3) 0.063(3) 0.035(2) -0.031(2) -0.0073(19) -0.001(2) C12 0.060(3) 0.051(3) 0.047(2) -0.029(2) -0.023(2) -0.002(2) C13 0.036(2) 0.034(2) 0.045(2) -0.0104(18) -0.0114(18) -0.0001(17) C14 0.048(3) 0.040(2) 0.050(2) -0.025(2) -0.018(2) 0.0020(19) C15 0.034(2) 0.039(2) 0.070(3) -0.026(2) -0.018(2) 0.0078(18) C16 0.028(2) 0.046(3) 0.075(3) -0.016(2) -0.017(2) -0.0063(18) C17 0.055(3) 0.063(3) 0.058(3) -0.026(2) -0.028(2) -0.005(2) C18 0.032(2) 0.039(2) 0.078(3) -0.025(2) -0.014(2) -0.0069(18) C19 0.034(3) 0.096(4) 0.052(3) -0.031(3) 0.000(2) -0.005(2) C20 0.057(3) 0.072(3) 0.037(2) -0.007(2) 0.006(2) -0.016(3) C21 0.081(4) 0.071(4) 0.068(3) -0.048(3) -0.003(3) 0.009(3) C22 0.058(3) 0.048(3) 0.048(3) 0.004(2) -0.021(2) -0.007(2) C23 0.077(4) 0.077(4) 0.043(3) -0.018(2) -0.025(2) -0.025(3) C24 0.030(2) 0.049(3) 0.045(2) -0.001(2) -0.0144(18) 0.0011(18) C25 0.053(3) 0.035(2) 0.057(3) -0.006(2) -0.015(2) 0.011(2) C26 0.053(3) 0.029(2) 0.040(2) -0.0066(18) -0.0015(19) -0.0081(18) C27 0.062(3) 0.027(2) 0.060(3) -0.023(2) 0.001(2) -0.009(2) C28 0.069(3) 0.053(3) 0.045(2) -0.028(2) -0.014(2) -0.009(2) C29 0.058(3) 0.034(2) 0.0229(18) -0.0114(16) -0.0102(18) -0.0044(18) C30 0.045(3) 0.041(2) 0.045(2) -0.025(2) 0.0074(19) -0.0065(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O2 1.862(2) . ? Ce1 O1 2.271(2) . ? Ce1 N2 2.327(3) . ? Ce1 N1 2.414(3) . ? Ce2 O1 1.999(2) . ? Ce2 N3 2.296(3) . ? Ce2 N4 2.300(3) . ? Ce2 N5 2.303(3) . ? K O2 2.591(2) 2_675 ? K O2 2.659(2) . ? Si1 N1 1.714(3) . ? Si1 C2 1.864(4) . ? Si1 C1 1.881(4) . ? Si1 C3 1.883(4) . ? Si2 N1 1.723(3) . ? Si2 C6 1.868(4) . ? Si2 C5 1.870(4) . ? Si2 C4 1.882(4) . ? Si3 N2 1.727(3) . ? Si3 C9 1.871(4) . ? Si3 C8 1.879(4) . ? Si3 C7 1.879(4) . ? Si4 N2 1.725(3) . ? Si4 C11 1.867(4) . ? Si4 C12 1.869(4) . ? Si4 C10 1.894(4) . ? Si5 N3 1.732(3) . ? Si5 C14 1.872(4) . ? Si5 C15 1.873(4) . ? Si5 C13 1.874(4) . ? Si6 N3 1.733(3) . ? Si6 C18 1.867(4) . ? Si6 C16 1.869(4) . ? Si6 C17 1.875(5) . ? Si7 N4 1.740(3) . ? Si7 C19 1.840(5) . ? Si7 C21 1.872(5) . ? Si7 C20 1.873(5) . ? Si8 N4 1.733(3) . ? Si8 C23 1.869(5) . ? Si8 C24 1.874(4) . ? Si8 C22 1.882(4) . ? Si9 N5 1.738(3) . ? Si9 C26 1.867(4) . ? Si9 C25 1.868(5) . ? Si9 C27 1.876(4) . ? Si10 N5 1.728(3) . ? Si10 C30 1.867(4) . ? Si10 C29 1.880(4) . ? Si10 C28 1.881(4) . ? O2 K 2.591(2) 2_675 ? C1A C2A 1.54(3) . ? C2A C3A 1.59(6) . ? C3A C4A 1.60(6) . ? C4A C5A 1.60(3) . ? C5A C6A 1.70(3) . ? 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 O2 Ce1 O1 100.71(9) . . ? O2 Ce1 N2 106.49(10) . . ? O1 Ce1 N2 110.86(9) . . ? O2 Ce1 N1 93.37(9) . . ? O1 Ce1 N1 124.87(9) . . ? N2 Ce1 N1 115.49(10) . . ? O1 Ce2 N3 103.98(9) . . ? O1 Ce2 N4 106.10(9) . . ? N3 Ce2 N4 115.17(10) . . ? O1 Ce2 N5 109.20(9) . . ? N3 Ce2 N5 106.25(10) . . ? N4 Ce2 N5 115.46(10) . . ? O2 K O2 81.17(7) 2_675 . ? N1 Si1 C2 112.88(18) . . ? N1 Si1 C1 108.01(16) . . ? C2 Si1 C1 110.02(18) . . ? N1 Si1 C3 115.51(18) . . ? C2 Si1 C3 106.6(2) . . ? C1 Si1 C3 103.3(2) . . ? N1 Si2 C6 109.60(17) . . ? N1 Si2 C5 113.61(18) . . ? C6 Si2 C5 107.8(2) . . ? N1 Si2 C4 114.26(18) . . ? C6 Si2 C4 104.9(2) . . ? C5 Si2 C4 106.1(2) . . ? N2 Si3 C9 112.40(16) . . ? N2 Si3 C8 113.99(17) . . ? C9 Si3 C8 107.1(2) . . ? N2 Si3 C7 111.96(15) . . ? C9 Si3 C7 106.1(2) . . ? C8 Si3 C7 104.58(19) . . ? N2 Si4 C11 116.08(17) . . ? N2 Si4 C12 114.98(17) . . ? C11 Si4 C12 106.2(2) . . ? N2 Si4 C10 106.95(15) . . ? C11 Si4 C10 106.0(2) . . ? C12 Si4 C10 105.8(2) . . ? N3 Si5 C14 109.29(17) . . ? N3 Si5 C15 116.51(17) . . ? C14 Si5 C15 106.1(2) . . ? N3 Si5 C13 110.54(16) . . ? C14 Si5 C13 108.8(2) . . ? C15 Si5 C13 105.25(19) . . ? N3 Si6 C18 111.01(17) . . ? N3 Si6 C16 115.13(18) . . ? C18 Si6 C16 104.1(2) . . ? N3 Si6 C17 110.87(18) . . ? C18 Si6 C17 109.4(2) . . ? C16 Si6 C17 105.9(2) . . ? N4 Si7 C19 110.30(18) . . ? N4 Si7 C21 112.1(2) . . ? C19 Si7 C21 108.3(3) . . ? N4 Si7 C20 113.4(2) . . ? C19 Si7 C20 105.6(2) . . ? C21 Si7 C20 106.8(3) . . ? N4 Si8 C23 113.6(2) . . ? N4 Si8 C24 107.75(16) . . ? C23 Si8 C24 107.6(2) . . ? N4 Si8 C22 115.97(19) . . ? C23 Si8 C22 106.3(2) . . ? C24 Si8 C22 105.0(2) . . ? N5 Si9 C26 110.73(16) . . ? N5 Si9 C25 111.73(18) . . ? C26 Si9 C25 109.9(2) . . ? N5 Si9 C27 114.06(18) . . ? C26 Si9 C27 103.9(2) . . ? C25 Si9 C27 106.1(2) . . ? N5 Si10 C30 113.36(18) . . ? N5 Si10 C29 109.42(15) . . ? C30 Si10 C29 108.47(19) . . ? N5 Si10 C28 115.57(18) . . ? C30 Si10 C28 105.3(2) . . ? C29 Si10 C28 104.1(2) . . ? Ce2 O1 Ce1 176.83(12) . . ? Ce1 O2 K 148.12(12) . 2_675 ? Ce1 O2 K 112.44(10) . . ? K O2 K 98.83(7) 2_675 . ? Si1 N1 Si2 122.64(16) . . ? Si1 N1 Ce1 114.91(14) . . ? Si2 N1 Ce1 121.24(14) . . ? Si4 N2 Si3 123.95(16) . . ? Si4 N2 Ce1 108.26(13) . . ? Si3 N2 Ce1 127.72(14) . . ? Si5 N3 Si6 119.25(16) . . ? Si5 N3 Ce2 114.88(14) . . ? Si6 N3 Ce2 125.76(15) . . ? Si8 N4 Si7 118.74(17) . . ? Si8 N4 Ce2 116.48(14) . . ? Si7 N4 Ce2 124.75(16) . . ? Si10 N5 Si9 118.15(16) . . ? Si10 N5 Ce2 120.13(14) . . ? Si9 N5 Ce2 121.68(14) . . ? C1A C2A C3A 152(2) . . ? C2A C3A C4A 149(4) . . ? C3A C4A C5A 143(2) . . ? C4A C5A C6A 126.9(12) . . ? #===END data_(9)-dec1803 _database_code_depnum_ccdc_archive 'CCDC 774599' #TrackingRef '- mfl_28jul2009.CIF' _audit_creation_date 2003-12-19T09:21:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H108 Ce2 N6 O2 Si12, 2(C6 H14)' _chemical_formula_sum 'C48 H136 Ce2 N6 O2 Si12' _chemical_formula_weight 1446.95 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 16.6202(4) _cell_length_b 16.3746(4) _cell_length_c 29.3114(6) _cell_angle_alpha 90 _cell_angle_beta 104.453(1) _cell_angle_gamma 90 _cell_volume 7724.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 247558 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7413 _exptl_absorpt_correction_T_max 0.7976 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.379005E-1 _diffrn_orient_matrix_ub_12 0.256568E-1 _diffrn_orient_matrix_ub_13 0.282858E-1 _diffrn_orient_matrix_ub_21 0.490786E-1 _diffrn_orient_matrix_ub_22 -0.23825E-1 _diffrn_orient_matrix_ub_23 -0.91973E-2 _diffrn_orient_matrix_ub_31 0.3935E-2 _diffrn_orient_matrix_ub_32 0.500366E-1 _diffrn_orient_matrix_ub_33 -0.188831E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0806 _diffrn_reflns_av_unetI/netI 0.0469 _diffrn_reflns_number 74536 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 23 _diffrn_reflns_theta_full 23 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 10685 _reflns_number_gt 8005 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There are two hexane solvate molecules; one of which was very poorly defined and included with isotropic C atoms and SADI constraints. 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^)+(0.0328P)^2^+24.9069P] 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_number_reflns 10685 _refine_ls_number_parameters 601 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.141 _refine_ls_shift/su_mean 0.006 _refine_diff_density_max 0.957 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.089 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.220491(19) 0.22987(2) 0.288032(11) 0.02886(11) Uani 1 1 d . . . Ce2 Ce 0.18918(2) 0.23565(2) 0.133276(11) 0.02970(11) Uani 1 1 d . . . Si1 Si 0.28445(12) 0.02530(11) 0.29942(7) 0.0447(5) Uani 1 1 d . . . Si2 Si 0.38797(11) 0.13390(12) 0.37151(7) 0.0451(5) Uani 1 1 d . . . Si3 Si 0.37081(12) 0.38226(12) 0.30947(7) 0.0468(5) Uani 1 1 d . . . Si4 Si 0.23738(12) 0.41198(12) 0.35772(7) 0.0498(5) Uani 1 1 d . . . Si5 Si 0.07450(11) 0.14096(12) 0.34606(6) 0.0454(5) Uani 1 1 d . . . Si6 Si 0.01510(11) 0.27473(13) 0.27810(7) 0.0467(5) Uani 1 1 d . . . Si7 Si -0.01848(11) 0.18576(12) 0.10828(6) 0.0442(5) Uani 1 1 d . . . Si8 Si 0.01616(11) 0.31985(12) 0.04725(6) 0.0449(5) Uani 1 1 d . . . Si9 Si 0.24713(12) 0.44011(11) 0.13080(7) 0.0453(5) Uani 1 1 d . . . Si10 Si 0.33306(12) 0.33095(12) 0.07723(7) 0.0459(5) Uani 1 1 d . . . Si11 Si 0.18352(12) 0.05521(12) 0.06238(7) 0.0482(5) Uani 1 1 d . . . Si12 Si 0.33525(11) 0.08253(11) 0.13932(7) 0.0426(5) Uani 1 1 d . . . O1 O 0.2190(4) 0.2732(3) 0.21223(16) 0.088(2) Uani 1 1 d . . . O2 O 0.1960(4) 0.1953(3) 0.20993(17) 0.089(2) Uani 1 1 d . . . N1 N 0.3016(3) 0.1247(3) 0.32244(16) 0.0360(12) Uani 1 1 d . . . N2 N 0.2787(3) 0.3472(3) 0.32126(16) 0.0359(12) Uani 1 1 d . . . N3 N 0.0983(3) 0.2141(3) 0.30715(17) 0.0377(13) Uani 1 1 d . . . N4 N 0.0554(3) 0.2492(3) 0.09258(16) 0.0351(12) Uani 1 1 d . . . N5 N 0.2596(3) 0.3407(3) 0.11133(17) 0.0383(13) Uani 1 1 d . . . N6 N 0.2370(3) 0.1189(3) 0.10880(17) 0.0392(13) Uani 1 1 d . . . C1 C 0.3793(4) -0.0200(4) 0.2866(3) 0.057(2) Uani 1 1 d . . . H1A H 0.4242 -0.0214 0.3156 0.086 Uiso 1 1 calc R . . H1B H 0.3965 0.0132 0.2629 0.086 Uiso 1 1 calc R . . H1C H 0.3672 -0.0757 0.2747 0.086 Uiso 1 1 calc R . . C2 C 0.2011(4) 0.0261(4) 0.2437(2) 0.0506(18) Uani 1 1 d . . . H2A H 0.1504 0.0496 0.2495 0.076 Uiso 1 1 calc R . . H2B H 0.1901 -0.0299 0.232 0.076 Uiso 1 1 calc R . . H2C H 0.219 0.059 0.2201 0.076 Uiso 1 1 calc R . . C3 C 0.2473(5) -0.0503(4) 0.3381(3) 0.066(2) Uani 1 1 d . . . H3A H 0.1971 -0.0292 0.3458 0.099 Uiso 1 1 calc R . . H3B H 0.2908 -0.0587 0.3671 0.099 Uiso 1 1 calc R . . H3C H 0.2345 -0.1024 0.3214 0.099 Uiso 1 1 calc R . . C4 C 0.4102(5) 0.0415(5) 0.4103(3) 0.064(2) Uani 1 1 d . . . H4A H 0.3608 0.0276 0.4214 0.096 Uiso 1 1 calc R . . H4B H 0.4567 0.053 0.4375 0.096 Uiso 1 1 calc R . . H4C H 0.4245 -0.0045 0.3925 0.096 Uiso 1 1 calc R . . C5 C 0.3704(4) 0.2159(4) 0.4127(2) 0.056(2) Uani 1 1 d . . . H5A H 0.3191 0.2044 0.4223 0.084 Uiso 1 1 calc R . . H5B H 0.3655 0.2689 0.3967 0.084 Uiso 1 1 calc R . . H5C H 0.4174 0.2173 0.4406 0.084 Uiso 1 1 calc R . . C6 C 0.4851(4) 0.1541(5) 0.3525(3) 0.061(2) Uani 1 1 d . . . H6A H 0.4772 0.2021 0.332 0.091 Uiso 1 1 calc R . . H6B H 0.4982 0.1066 0.3354 0.091 Uiso 1 1 calc R . . H6C H 0.5309 0.1641 0.3803 0.091 Uiso 1 1 calc R . . C7 C 0.3981(4) 0.3187(5) 0.2625(2) 0.059(2) Uani 1 1 d . . . H7A H 0.4022 0.2612 0.2722 0.089 Uiso 1 1 calc R . . H7B H 0.4515 0.3368 0.2577 0.089 Uiso 1 1 calc R . . H7C H 0.3549 0.3247 0.2331 0.089 Uiso 1 1 calc R . . C8 C 0.3643(5) 0.4904(4) 0.2880(3) 0.062(2) Uani 1 1 d . . . H8A H 0.3502 0.5263 0.3116 0.092 Uiso 1 1 calc R . . H8B H 0.3214 0.4947 0.2583 0.092 Uiso 1 1 calc R . . H8C H 0.418 0.5069 0.2828 0.092 Uiso 1 1 calc R . . C9 C 0.4636(4) 0.3769(5) 0.3612(3) 0.063(2) Uani 1 1 d . . . H9A H 0.4529 0.4091 0.3873 0.094 Uiso 1 1 calc R . . H9B H 0.5123 0.3989 0.3522 0.094 Uiso 1 1 calc R . . H9C H 0.474 0.3199 0.3711 0.094 Uiso 1 1 calc R . . C10 C 0.1669(5) 0.4904(5) 0.3219(3) 0.069(2) Uani 1 1 d . . . H10A H 0.1239 0.463 0.2977 0.104 Uiso 1 1 calc R . . H10B H 0.1993 0.5267 0.3067 0.104 Uiso 1 1 calc R . . H10C H 0.1408 0.5225 0.3425 0.104 Uiso 1 1 calc R . . C11 C 0.3168(5) 0.4702(5) 0.4027(3) 0.075(2) Uani 1 1 d . . . H11A H 0.3554 0.4318 0.4225 0.113 Uiso 1 1 calc R . . H11B H 0.2888 0.5025 0.4223 0.113 Uiso 1 1 calc R . . H11C H 0.3476 0.5067 0.3866 0.113 Uiso 1 1 calc R . . C12 C 0.1814(4) 0.3539(5) 0.3953(2) 0.060(2) Uani 1 1 d . . . H12A H 0.1375 0.3207 0.3752 0.089 Uiso 1 1 calc R . . H12B H 0.1567 0.3923 0.4136 0.089 Uiso 1 1 calc R . . H12C H 0.2207 0.3182 0.4168 0.089 Uiso 1 1 calc R . . C13 C 0.1652(4) 0.1181(4) 0.3962(2) 0.0532(19) Uani 1 1 d . . . H13A H 0.2121 0.1003 0.3841 0.08 Uiso 1 1 calc R . . H13B H 0.1504 0.0746 0.4156 0.08 Uiso 1 1 calc R . . H13C H 0.1807 0.1673 0.4154 0.08 Uiso 1 1 calc R . . C14 C 0.0353(5) 0.0448(5) 0.3135(3) 0.064(2) Uani 1 1 d . . . H14A H -0.0121 0.0576 0.2871 0.096 Uiso 1 1 calc R . . H14B H 0.0179 0.0065 0.3348 0.096 Uiso 1 1 calc R . . H14C H 0.0797 0.0201 0.3015 0.096 Uiso 1 1 calc R . . C15 C -0.0069(4) 0.1739(5) 0.3758(3) 0.068(2) Uani 1 1 d . . . H15A H -0.058 0.1875 0.352 0.101 Uiso 1 1 calc R . . H15B H 0.0125 0.2221 0.3953 0.101 Uiso 1 1 calc R . . H15C H -0.0182 0.1295 0.3958 0.101 Uiso 1 1 calc R . . C16 C -0.0779(4) 0.2131(5) 0.2484(2) 0.063(2) Uani 1 1 d . . . H16A H -0.0963 0.1805 0.2719 0.094 Uiso 1 1 calc R . . H16B H -0.0633 0.1767 0.2252 0.094 Uiso 1 1 calc R . . H16C H -0.1228 0.2497 0.2325 0.094 Uiso 1 1 calc R . . C17 C -0.0226(5) 0.3516(5) 0.3159(3) 0.069(2) Uani 1 1 d . . . H17A H -0.0406 0.3231 0.3411 0.104 Uiso 1 1 calc R . . H17B H -0.0693 0.3823 0.2966 0.104 Uiso 1 1 calc R . . H17C H 0.0227 0.3893 0.3299 0.104 Uiso 1 1 calc R . . C18 C 0.0480(4) 0.3362(5) 0.2320(3) 0.062(2) Uani 1 1 d . . . H18A H 0.0965 0.3694 0.2468 0.093 Uiso 1 1 calc R . . H18B H 0.0024 0.3719 0.216 0.093 Uiso 1 1 calc R . . H18C H 0.0625 0.2993 0.2089 0.093 Uiso 1 1 calc R . . C19 C 0.0336(4) 0.1216(4) 0.1603(2) 0.0551(19) Uani 1 1 d . . . H19A H 0.0792 0.0907 0.1529 0.083 Uiso 1 1 calc R . . H19B H -0.0068 0.0835 0.1678 0.083 Uiso 1 1 calc R . . H19C H 0.0557 0.157 0.1876 0.083 Uiso 1 1 calc R . . C20 C -0.0703(4) 0.1090(5) 0.0627(2) 0.062(2) Uani 1 1 d . . . H20A H -0.0279 0.0761 0.0533 0.093 Uiso 1 1 calc R . . H20B H -0.104 0.1376 0.0352 0.093 Uiso 1 1 calc R . . H20C H -0.106 0.0733 0.076 0.093 Uiso 1 1 calc R . . C21 C -0.1048(4) 0.2441(5) 0.1229(2) 0.059(2) Uani 1 1 d . . . H21A H -0.1324 0.2777 0.0958 0.089 Uiso 1 1 calc R . . H21B H -0.0825 0.2794 0.1501 0.089 Uiso 1 1 calc R . . H21C H -0.1451 0.2059 0.1304 0.089 Uiso 1 1 calc R . . C22 C -0.0755(4) 0.2819(5) 0.0010(2) 0.060(2) Uani 1 1 d . . . H22A H -0.1203 0.2671 0.0158 0.09 Uiso 1 1 calc R . . H22B H -0.0593 0.2337 -0.0144 0.09 Uiso 1 1 calc R . . H22C H -0.0948 0.3249 -0.0224 0.09 Uiso 1 1 calc R . . C23 C 0.0936(4) 0.3445(4) 0.0128(2) 0.0540(19) Uani 1 1 d . . . H23A H 0.1446 0.3654 0.0341 0.081 Uiso 1 1 calc R . . H23B H 0.0705 0.386 -0.0109 0.081 Uiso 1 1 calc R . . H23C H 0.1064 0.295 -0.0029 0.081 Uiso 1 1 calc R . . C24 C -0.0192(5) 0.4165(4) 0.0710(3) 0.064(2) Uani 1 1 d . . . H24A H -0.0599 0.4032 0.0889 0.096 Uiso 1 1 calc R . . H24B H -0.0448 0.4527 0.0447 0.096 Uiso 1 1 calc R . . H24C H 0.0287 0.4439 0.0916 0.096 Uiso 1 1 calc R . . C25 C 0.1939(5) 0.5127(4) 0.0833(3) 0.063(2) Uani 1 1 d . . . H25A H 0.2254 0.5161 0.0592 0.095 Uiso 1 1 calc R . . H25B H 0.1908 0.5669 0.097 0.095 Uiso 1 1 calc R . . H25C H 0.1376 0.4929 0.0689 0.095 Uiso 1 1 calc R . . C26 C 0.3487(4) 0.4876(4) 0.1606(3) 0.060(2) Uani 1 1 d . . . H26A H 0.3848 0.4888 0.1388 0.09 Uiso 1 1 calc R . . H26B H 0.3752 0.4555 0.1885 0.09 Uiso 1 1 calc R . . H26C H 0.3393 0.5435 0.1701 0.09 Uiso 1 1 calc R . . C27 C 0.1811(4) 0.4395(4) 0.1740(3) 0.0537(19) Uani 1 1 d . . . H27A H 0.127 0.4153 0.1592 0.08 Uiso 1 1 calc R . . H27B H 0.1733 0.4956 0.1837 0.08 Uiso 1 1 calc R . . H27C H 0.2086 0.4072 0.2017 0.08 Uiso 1 1 calc R . . C28 C 0.4393(4) 0.3151(5) 0.1162(3) 0.061(2) Uani 1 1 d . . . H28A H 0.4388 0.2678 0.1367 0.092 Uiso 1 1 calc R . . H28B H 0.4563 0.3638 0.1356 0.092 Uiso 1 1 calc R . . H28C H 0.4786 0.3052 0.0968 0.092 Uiso 1 1 calc R . . C29 C 0.3403(5) 0.4217(5) 0.0395(3) 0.068(2) Uani 1 1 d . . . H29A H 0.3555 0.4701 0.0595 0.102 Uiso 1 1 calc R . . H29B H 0.2865 0.4308 0.0171 0.102 Uiso 1 1 calc R . . H29C H 0.3827 0.4117 0.0222 0.102 Uiso 1 1 calc R . . C30 C 0.3053(4) 0.2472(4) 0.0331(2) 0.054(2) Uani 1 1 d . . . H30A H 0.3003 0.1957 0.0492 0.081 Uiso 1 1 calc R . . H30B H 0.3488 0.2419 0.016 0.081 Uiso 1 1 calc R . . H30C H 0.2523 0.2598 0.0107 0.081 Uiso 1 1 calc R . . C31 C 0.2540(5) 0.0022(5) 0.0306(2) 0.064(2) Uani 1 1 d . . . H31A H 0.2946 -0.0308 0.0531 0.096 Uiso 1 1 calc R . . H31B H 0.2831 0.0431 0.0163 0.096 Uiso 1 1 calc R . . H31C H 0.2209 -0.0331 0.006 0.096 Uiso 1 1 calc R . . C32 C 0.1117(4) 0.1143(5) 0.0153(2) 0.059(2) Uani 1 1 d . . . H32A H 0.1428 0.157 0.0037 0.088 Uiso 1 1 calc R . . H32B H 0.0685 0.1395 0.0281 0.088 Uiso 1 1 calc R . . H32C H 0.0859 0.0776 -0.0106 0.088 Uiso 1 1 calc R . . C33 C 0.1249(5) -0.0268(4) 0.0842(3) 0.066(2) Uani 1 1 d . . . H33A H 0.1631 -0.058 0.109 0.098 Uiso 1 1 calc R . . H33B H 0.0995 -0.0634 0.0582 0.098 Uiso 1 1 calc R . . H33C H 0.0814 -0.0022 0.097 0.098 Uiso 1 1 calc R . . C34 C 0.4180(4) 0.0866(5) 0.1061(3) 0.060(2) Uani 1 1 d . . . H34A H 0.401 0.0535 0.0774 0.09 Uiso 1 1 calc R . . H34B H 0.4702 0.0652 0.1259 0.09 Uiso 1 1 calc R . . H34C H 0.4262 0.1433 0.0975 0.09 Uiso 1 1 calc R . . C35 C 0.3321(4) -0.0255(4) 0.1588(2) 0.0510(18) Uani 1 1 d . . . H35A H 0.311 -0.0604 0.1312 0.076 Uiso 1 1 calc R . . H35B H 0.2954 -0.0297 0.1802 0.076 Uiso 1 1 calc R . . H35C H 0.3882 -0.0431 0.1752 0.076 Uiso 1 1 calc R . . C36 C 0.3758(4) 0.1474(4) 0.1927(2) 0.0553(19) Uani 1 1 d . . . H36A H 0.3353 0.1483 0.2119 0.083 Uiso 1 1 calc R . . H36B H 0.385 0.2031 0.1829 0.083 Uiso 1 1 calc R . . H36C H 0.4284 0.1246 0.2113 0.083 Uiso 1 1 calc R . . C37 C 0.3444(6) 0.7178(6) 0.3297(4) 0.107(3) Uani 1 1 d . . . H37A H 0.3924 0.7137 0.3569 0.161 Uiso 1 1 calc R . . H37B H 0.3101 0.6687 0.3278 0.161 Uiso 1 1 calc R . . H37C H 0.3114 0.7659 0.3332 0.161 Uiso 1 1 calc R . . C38 C 0.3746(6) 0.7259(6) 0.2848(4) 0.097(3) Uani 1 1 d . . . H38A H 0.4105 0.7747 0.2872 0.116 Uiso 1 1 calc R . . H38B H 0.4083 0.6774 0.2815 0.116 Uiso 1 1 calc R . . C39 C 0.3050(5) 0.7331(6) 0.2430(4) 0.094(3) Uani 1 1 d . . . H39A H 0.2721 0.7818 0.2468 0.113 Uiso 1 1 calc R . . H39B H 0.2687 0.6848 0.2418 0.113 Uiso 1 1 calc R . . C40 C 0.3285(6) 0.7400(5) 0.1958(4) 0.090(3) Uani 1 1 d . . . H40A H 0.3638 0.789 0.1968 0.108 Uiso 1 1 calc R . . H40B H 0.3625 0.6918 0.1923 0.108 Uiso 1 1 calc R . . C41 C 0.2560(6) 0.7457(6) 0.1523(5) 0.107(4) Uani 1 1 d . . . H41A H 0.2195 0.6977 0.1518 0.129 Uiso 1 1 calc R . . H41B H 0.2232 0.7951 0.155 0.129 Uiso 1 1 calc R . . C42 C 0.2799(7) 0.7492(7) 0.1065(5) 0.124(4) Uani 1 1 d . . . H42A H 0.2297 0.7528 0.0806 0.185 Uiso 1 1 calc R . . H42B H 0.3109 0.6998 0.1028 0.185 Uiso 1 1 calc R . . H42C H 0.3147 0.7973 0.1061 0.185 Uiso 1 1 calc R . . C43 C 0.3017(10) 0.6337(9) -0.0195(6) 0.199(7) Uiso 1 1 d D . . H43A H 0.3039 0.5763 -0.0286 0.299 Uiso 1 1 calc R . . H43B H 0.2552 0.6608 -0.0415 0.299 Uiso 1 1 calc R . . H43C H 0.294 0.6369 0.0125 0.299 Uiso 1 1 calc R . . C44 C 0.3795(10) 0.6742(8) -0.0211(9) 0.334(14) Uiso 1 1 d D . . H44A H 0.4265 0.6462 0.0007 0.401 Uiso 1 1 calc R . . H44B H 0.3877 0.6699 -0.0533 0.401 Uiso 1 1 calc R . . C45 C 0.3793(9) 0.7604(8) -0.0079(7) 0.289(12) Uiso 1 1 d D . . H45 H 0.3926 0.7628 0.0273 0.347 Uiso 1 1 calc R . . C46 C 0.4440(11) 0.8065(10) -0.0226(8) 0.294(12) Uiso 1 1 d D . . H46A H 0.4975 0.7771 -0.0124 0.352 Uiso 1 1 calc R . . H46B H 0.4297 0.8101 -0.0574 0.352 Uiso 1 1 calc R . . C47 C 0.4533(11) 0.8889(11) -0.0027(6) 0.238(9) Uiso 1 1 d D . . H47A H 0.4975 0.9176 -0.0129 0.357 Uiso 1 1 calc R . . H47B H 0.4677 0.8854 0.0318 0.357 Uiso 1 1 calc R . . H47C H 0.4009 0.9187 -0.0136 0.357 Uiso 1 1 calc R . . C48 C 0.2974(10) 0.7974(12) -0.0256(13) 0.51(3) Uiso 1 1 d D . . H48A H 0.2559 0.7661 -0.0144 0.763 Uiso 1 1 calc R . . H48B H 0.2828 0.7972 -0.0602 0.763 Uiso 1 1 calc R . . H48C H 0.2984 0.8538 -0.0143 0.763 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 0.02784(19) 0.0314(2) 0.02879(19) -0.00225(15) 0.00976(15) -0.00065(16) Ce2 0.0311(2) 0.0311(2) 0.02884(19) -0.00355(15) 0.01117(15) -0.00362(16) Si1 0.0499(12) 0.0348(11) 0.0496(12) 0.0045(9) 0.0126(9) 0.0059(9) Si2 0.0382(11) 0.0497(12) 0.0451(11) 0.0048(9) 0.0060(9) 0.0087(9) Si3 0.0478(12) 0.0433(12) 0.0516(12) -0.0132(9) 0.0167(10) -0.0113(9) Si4 0.0546(12) 0.0479(13) 0.0482(12) -0.0176(9) 0.0152(10) 0.0010(10) Si5 0.0394(11) 0.0587(13) 0.0423(11) 0.0062(9) 0.0185(9) -0.0039(9) Si6 0.0338(10) 0.0618(13) 0.0465(11) 0.0076(10) 0.0139(9) 0.0082(9) Si7 0.0342(10) 0.0580(13) 0.0392(10) -0.0002(9) 0.0071(8) -0.0075(9) Si8 0.0436(11) 0.0532(13) 0.0362(10) 0.0007(9) 0.0067(9) 0.0021(9) Si9 0.0533(12) 0.0370(11) 0.0499(12) 0.0004(9) 0.0212(10) -0.0082(9) Si10 0.0462(11) 0.0498(12) 0.0483(11) 0.0034(9) 0.0242(9) -0.0065(9) Si11 0.0501(12) 0.0464(12) 0.0509(12) -0.0192(9) 0.0180(10) -0.0049(9) Si12 0.0423(11) 0.0391(11) 0.0489(11) -0.0086(9) 0.0164(9) 0.0015(9) O1 0.185(7) 0.044(4) 0.035(3) -0.006(2) 0.030(3) -0.018(4) O2 0.187(6) 0.041(3) 0.044(3) -0.010(3) 0.039(4) -0.044(4) N1 0.036(3) 0.036(3) 0.039(3) 0.002(2) 0.015(2) 0.004(2) N2 0.035(3) 0.037(3) 0.034(3) -0.006(2) 0.005(2) -0.001(2) N3 0.028(3) 0.045(3) 0.043(3) 0.002(2) 0.015(2) -0.001(2) N4 0.035(3) 0.041(3) 0.030(3) -0.006(2) 0.009(2) -0.002(2) N5 0.042(3) 0.039(3) 0.037(3) -0.002(2) 0.013(2) -0.006(2) N6 0.038(3) 0.039(3) 0.043(3) -0.010(2) 0.015(2) -0.003(2) C1 0.063(5) 0.051(5) 0.057(5) -0.001(4) 0.014(4) 0.018(4) C2 0.053(4) 0.038(4) 0.060(5) -0.005(3) 0.013(4) -0.006(3) C3 0.083(6) 0.047(5) 0.069(5) 0.012(4) 0.023(4) 0.004(4) C4 0.065(5) 0.069(6) 0.054(5) 0.006(4) 0.007(4) 0.013(4) C5 0.050(4) 0.073(6) 0.041(4) -0.004(4) 0.004(3) -0.001(4) C6 0.040(4) 0.073(6) 0.064(5) -0.004(4) 0.004(4) 0.008(4) C7 0.059(5) 0.064(5) 0.062(5) -0.022(4) 0.031(4) -0.010(4) C8 0.077(5) 0.048(5) 0.063(5) -0.016(4) 0.024(4) -0.014(4) C9 0.052(5) 0.061(5) 0.074(5) -0.013(4) 0.014(4) -0.017(4) C10 0.080(6) 0.051(5) 0.084(6) -0.008(4) 0.034(5) 0.012(4) C11 0.085(6) 0.076(6) 0.065(5) -0.033(5) 0.019(5) -0.012(5) C12 0.065(5) 0.074(6) 0.044(4) -0.008(4) 0.022(4) 0.011(4) C13 0.049(4) 0.063(5) 0.053(4) 0.015(4) 0.024(4) 0.000(4) C14 0.069(5) 0.066(5) 0.060(5) 0.008(4) 0.022(4) -0.022(4) C15 0.050(5) 0.107(7) 0.055(5) 0.020(4) 0.029(4) 0.008(4) C16 0.036(4) 0.106(7) 0.048(4) 0.013(4) 0.013(3) -0.003(4) C17 0.052(5) 0.080(6) 0.078(6) 0.005(5) 0.022(4) 0.028(4) C18 0.050(5) 0.064(5) 0.068(5) 0.022(4) 0.009(4) 0.002(4) C19 0.043(4) 0.059(5) 0.063(5) 0.013(4) 0.014(4) -0.010(4) C20 0.054(5) 0.074(6) 0.058(5) -0.007(4) 0.011(4) -0.022(4) C21 0.041(4) 0.091(6) 0.045(4) 0.009(4) 0.010(3) 0.005(4) C22 0.048(4) 0.084(6) 0.044(4) 0.005(4) 0.003(3) 0.000(4) C23 0.057(5) 0.060(5) 0.043(4) 0.008(4) 0.008(4) -0.001(4) C24 0.071(5) 0.051(5) 0.066(5) 0.002(4) 0.010(4) 0.016(4) C25 0.078(6) 0.042(5) 0.071(5) 0.009(4) 0.020(4) -0.006(4) C26 0.066(5) 0.052(5) 0.066(5) -0.001(4) 0.025(4) -0.023(4) C27 0.062(5) 0.035(4) 0.071(5) 0.000(4) 0.029(4) 0.002(3) C28 0.046(4) 0.069(6) 0.076(5) -0.003(4) 0.030(4) -0.012(4) C29 0.092(6) 0.062(5) 0.064(5) 0.003(4) 0.043(5) -0.012(5) C30 0.070(5) 0.054(5) 0.049(4) -0.003(3) 0.035(4) -0.003(4) C31 0.065(5) 0.077(6) 0.050(4) -0.035(4) 0.013(4) 0.003(4) C32 0.061(5) 0.068(5) 0.047(4) -0.016(4) 0.013(4) -0.010(4) C33 0.060(5) 0.041(5) 0.094(6) -0.017(4) 0.015(4) -0.013(4) C34 0.048(4) 0.067(5) 0.071(5) -0.005(4) 0.025(4) 0.006(4) C35 0.064(5) 0.043(4) 0.050(4) -0.005(3) 0.022(4) 0.005(4) C36 0.059(5) 0.056(5) 0.052(4) -0.010(4) 0.015(4) -0.005(4) C37 0.094(8) 0.081(8) 0.150(10) -0.003(7) 0.036(7) 0.015(6) C38 0.057(6) 0.082(7) 0.146(10) 0.010(7) 0.016(7) 0.003(5) C39 0.059(6) 0.065(6) 0.162(11) -0.019(6) 0.035(7) -0.008(5) C40 0.065(6) 0.053(6) 0.148(10) -0.004(6) 0.020(7) 0.000(4) C41 0.070(7) 0.096(8) 0.153(11) -0.044(7) 0.024(7) -0.014(6) C42 0.101(9) 0.111(10) 0.144(11) -0.042(8) 0.005(8) -0.001(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 N3 2.253(4) . ? Ce1 N2 2.260(5) . ? Ce1 N1 2.264(5) . ? Ce1 O2 2.294(5) . ? Ce1 O1 2.327(5) . ? Ce2 N6 2.256(5) . ? Ce2 N4 2.256(5) . ? Ce2 N5 2.262(5) . ? Ce2 O2 2.317(5) . ? Ce2 O1 2.325(5) . ? Si1 N1 1.758(5) . ? Si1 C2 1.859(7) . ? Si1 C1 1.864(7) . ? Si1 C3 1.884(7) . ? Si2 N1 1.767(5) . ? Si2 C6 1.863(7) . ? Si2 C4 1.874(7) . ? Si2 C5 1.877(7) . ? Si3 N2 1.749(5) . ? Si3 C7 1.870(6) . ? Si3 C8 1.874(7) . ? Si3 C9 1.875(7) . ? Si4 N2 1.761(5) . ? Si4 C12 1.869(7) . ? Si4 C10 1.873(8) . ? Si4 C11 1.875(7) . ? Si5 N3 1.765(5) . ? Si5 C13 1.862(7) . ? Si5 C15 1.864(7) . ? Si5 C14 1.872(7) . ? Si6 N3 1.741(5) . ? Si6 C16 1.869(7) . ? Si6 C18 1.874(7) . ? Si6 C17 1.885(7) . ? Si7 N4 1.756(5) . ? Si7 C21 1.861(7) . ? Si7 C19 1.877(7) . ? Si7 C20 1.879(7) . ? Si8 N4 1.759(5) . ? Si8 C23 1.868(7) . ? Si8 C22 1.874(7) . ? Si8 C24 1.881(7) . ? Si9 N5 1.755(5) . ? Si9 C26 1.865(7) . ? Si9 C27 1.870(7) . ? Si9 C25 1.876(7) . ? Si10 N5 1.767(5) . ? Si10 C30 1.863(7) . ? Si10 C28 1.867(7) . ? Si10 C29 1.874(7) . ? Si11 N6 1.768(5) . ? Si11 C32 1.855(7) . ? Si11 C33 1.864(7) . ? Si11 C31 1.880(7) . ? Si12 N6 1.758(5) . ? Si12 C35 1.863(7) . ? Si12 C34 1.875(7) . ? Si12 C36 1.872(7) . ? O1 O2 1.328(6) . ? C37 C38 1.527(13) . ? C38 C39 1.463(13) . ? C39 C40 1.534(13) . ? C40 C41 1.524(13) . ? C41 C42 1.491(14) . ? C43 C44 1.46(2) . ? C44 C45 1.46(2) . ? C45 C46 1.46(2) . ? C45 C48 1.46(3) . ? C46 C47 1.46(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ce1 N2 107.79(17) . . ? N3 Ce1 N1 106.02(17) . . ? N2 Ce1 N1 108.17(17) . . ? N3 Ce1 O2 105.9(2) . . ? N2 Ce1 O2 126.16(17) . . ? N1 Ce1 O2 101.2(2) . . ? N3 Ce1 O1 118.5(2) . . ? N2 Ce1 O1 93.08(18) . . ? N1 Ce1 O1 121.39(19) . . ? O2 Ce1 O1 33.39(16) . . ? N6 Ce2 N4 107.13(17) . . ? N6 Ce2 N5 107.77(17) . . ? N4 Ce2 N5 106.64(17) . . ? N6 Ce2 O2 97.53(19) . . ? N4 Ce2 O2 110.1(2) . . ? N5 Ce2 O2 126.06(18) . . ? N6 Ce2 O1 122.43(19) . . ? N4 Ce2 O1 115.9(2) . . ? N5 Ce2 O1 94.89(18) . . ? O2 Ce2 O1 33.24(16) . . ? N1 Si1 C2 110.2(3) . . ? N1 Si1 C1 112.4(3) . . ? C2 Si1 C1 107.9(3) . . ? N1 Si1 C3 115.1(3) . . ? C2 Si1 C3 104.4(3) . . ? C1 Si1 C3 106.3(3) . . ? N1 Si2 C6 111.1(3) . . ? N1 Si2 C4 115.0(3) . . ? C6 Si2 C4 105.7(3) . . ? N1 Si2 C5 111.1(3) . . ? C6 Si2 C5 110.5(3) . . ? C4 Si2 C5 103.1(3) . . ? N2 Si3 C7 110.4(3) . . ? N2 Si3 C8 113.4(3) . . ? C7 Si3 C8 106.4(3) . . ? N2 Si3 C9 114.1(3) . . ? C7 Si3 C9 105.5(3) . . ? C8 Si3 C9 106.4(3) . . ? N2 Si4 C12 112.2(3) . . ? N2 Si4 C10 110.8(3) . . ? C12 Si4 C10 110.3(3) . . ? N2 Si4 C11 114.8(3) . . ? C12 Si4 C11 102.2(4) . . ? C10 Si4 C11 106.1(4) . . ? N3 Si5 C13 112.3(3) . . ? N3 Si5 C15 114.3(3) . . ? C13 Si5 C15 103.2(3) . . ? N3 Si5 C14 110.3(3) . . ? C13 Si5 C14 110.1(4) . . ? C15 Si5 C14 106.4(4) . . ? N3 Si6 C16 112.5(3) . . ? N3 Si6 C18 108.6(3) . . ? C16 Si6 C18 108.1(3) . . ? N3 Si6 C17 115.6(3) . . ? C16 Si6 C17 106.1(3) . . ? C18 Si6 C17 105.4(4) . . ? N4 Si7 C21 112.7(3) . . ? N4 Si7 C19 109.5(3) . . ? C21 Si7 C19 109.0(3) . . ? N4 Si7 C20 115.9(3) . . ? C21 Si7 C20 105.3(3) . . ? C19 Si7 C20 103.9(3) . . ? N4 Si8 C23 112.0(3) . . ? N4 Si8 C22 114.1(3) . . ? C23 Si8 C22 103.1(3) . . ? N4 Si8 C24 111.4(3) . . ? C23 Si8 C24 109.8(3) . . ? C22 Si8 C24 105.9(3) . . ? N5 Si9 C26 111.9(3) . . ? N5 Si9 C27 110.6(3) . . ? C26 Si9 C27 107.5(3) . . ? N5 Si9 C25 114.7(3) . . ? C26 Si9 C25 106.7(3) . . ? C27 Si9 C25 105.0(3) . . ? N5 Si10 C30 111.9(3) . . ? N5 Si10 C28 110.4(3) . . ? C30 Si10 C28 110.8(3) . . ? N5 Si10 C29 114.7(3) . . ? C30 Si10 C29 102.4(3) . . ? C28 Si10 C29 106.3(4) . . ? N6 Si11 C32 111.8(3) . . ? N6 Si11 C33 111.5(3) . . ? C32 Si11 C33 109.7(3) . . ? N6 Si11 C31 113.4(3) . . ? C32 Si11 C31 103.7(3) . . ? C33 Si11 C31 106.3(4) . . ? N6 Si12 C35 112.5(3) . . ? N6 Si12 C34 115.6(3) . . ? C35 Si12 C34 105.9(3) . . ? N6 Si12 C36 109.2(3) . . ? C35 Si12 C36 108.3(3) . . ? C34 Si12 C36 104.9(3) . . ? O2 O1 Ce2 73.0(3) . . ? O2 O1 Ce1 71.9(3) . . ? Ce2 O1 Ce1 144.9(2) . . ? O1 O2 Ce1 74.7(3) . . ? O1 O2 Ce2 73.7(3) . . ? Ce1 O2 Ce2 148.3(2) . . ? Si1 N1 Si2 114.4(3) . . ? Si1 N1 Ce1 120.8(2) . . ? Si2 N1 Ce1 124.8(3) . . ? Si3 N2 Si4 114.5(3) . . ? Si3 N2 Ce1 119.7(2) . . ? Si4 N2 Ce1 125.7(2) . . ? Si6 N3 Si5 115.1(3) . . ? Si6 N3 Ce1 117.9(2) . . ? Si5 N3 Ce1 126.8(3) . . ? Si7 N4 Si8 115.8(3) . . ? Si7 N4 Ce2 117.7(2) . . ? Si8 N4 Ce2 126.5(2) . . ? Si9 N5 Si10 115.0(3) . . ? Si9 N5 Ce2 120.1(2) . . ? Si10 N5 Ce2 124.9(3) . . ? Si12 N6 Si11 114.7(3) . . ? Si12 N6 Ce2 118.8(2) . . ? Si11 N6 Ce2 126.5(3) . . ? C39 C38 C37 111.5(8) . . ? C38 C39 C40 115.8(8) . . ? C41 C40 C39 115.7(8) . . ? C42 C41 C40 115.0(9) . . ? C45 C44 C43 111.6(10) . . ? C46 C45 C44 111.7(10) . . ? C46 C45 C48 111.6(10) . . ? C44 C45 C48 111.7(10) . . ? C47 C46 C45 111.7(10) . . ? #===END data_(9')-dec401 _database_code_depnum_ccdc_archive 'CCDC 774600' #TrackingRef '- mfl_28jul2009.CIF' _audit_creation_date 2001-12-06T15:56:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[{N(SiMe3)2}3Ce(O2)Ce{N(SiMe3)2}3].2(pentane)' ; _chemical_formula_moiety 'C36 H108 Ce2 N6 O2 Si12, 2(C5 H12)' _chemical_formula_sum 'C46 H132 Ce2 N6 O2 Si12' _chemical_formula_weight 1418.9 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 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 16.4576(4) _cell_length_b 16.4923(5) _cell_length_c 29.0764(6) _cell_angle_alpha 90 _cell_angle_beta 106.119(2) _cell_angle_gamma 90 _cell_volume 7581.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 52169 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3000 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.409 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_T_max 0.613 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 41095 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_unetI/netI 0.079 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 13310 _reflns_number_gt 9072 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The bridging O2 is disordered unequally over 3 orientations. The lower occupancy O positions were left isotropic. 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^)+(0.0319P)^2^+13.9762P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 13310 _refine_ls_number_parameters 579 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.717 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.101 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.945922(19) 0.733626(19) 0.137328(10) 0.02851(9) Uani 1 1 d . . . Ce2 Ce 1.071612(18) 0.725038(19) 0.293683(10) 0.02832(9) Uani 1 1 d . . . Si1 Si 0.88515(11) 0.93516(10) 0.13682(6) 0.0417(4) Uani 1 1 d . . . Si2 Si 0.74569(10) 0.82829(11) 0.08315(6) 0.0424(4) Uani 1 1 d . . . Si3 Si 1.03276(11) 0.81883(11) 0.04702(6) 0.0449(4) Uani 1 1 d . . . Si4 Si 1.13027(11) 0.68768(12) 0.10827(6) 0.0449(4) Uani 1 1 d . . . Si5 Si 0.88283(11) 0.55396(11) 0.06658(6) 0.0453(4) Uani 1 1 d . . . Si6 Si 0.80358(11) 0.58147(10) 0.14479(6) 0.0400(4) Uani 1 1 d . . . Si7 Si 1.01945(11) 0.52154(10) 0.30484(6) 0.0410(4) Uani 1 1 d . . . Si8 Si 0.98923(11) 0.62652(10) 0.38122(6) 0.0411(4) Uani 1 1 d . . . Si9 Si 1.27545(10) 0.63578(11) 0.34707(6) 0.0434(4) Uani 1 1 d . . . Si10 Si 1.26772(11) 0.77286(12) 0.28007(6) 0.0503(5) Uani 1 1 d . . . Si11 Si 0.94290(11) 0.87552(10) 0.31892(6) 0.0414(4) Uani 1 1 d . . . Si12 Si 1.12467(12) 0.90312(11) 0.36656(6) 0.0505(5) Uani 1 1 d . . . O1 O 0.9904(16) 0.6878(8) 0.2173(3) 0.043(4) Uani 0.56(3) 1 d P . . O2 O 1.0227(17) 0.7701(9) 0.2146(3) 0.053(5) Uani 0.56(3) 1 d P . . N1 N 0.8530(3) 0.8371(3) 0.11668(14) 0.0354(11) Uani 1 1 d . . . N2 N 1.0396(3) 0.7486(3) 0.09397(14) 0.0336(11) Uani 1 1 d . . . N3 N 0.8736(3) 0.6174(3) 0.11393(15) 0.0353(11) Uani 1 1 d . . . N4 N 1.0261(3) 0.6192(3) 0.32980(14) 0.0340(11) Uani 1 1 d . . . N5 N 1.2125(3) 0.7098(3) 0.30984(15) 0.0346(11) Uani 1 1 d . . . N6 N 1.0471(3) 0.8404(3) 0.32955(14) 0.0342(11) Uani 1 1 d . . . C1 C 0.9952(4) 0.9345(4) 0.1791(2) 0.0501(17) Uani 1 1 d . . . H1A H 1.0346 0.9111 0.1629 0.075 Uiso 1 1 calc R . . H1B H 0.9957 0.902 0.2073 0.075 Uiso 1 1 calc R . . H1C H 1.0124 0.9902 0.1889 0.075 Uiso 1 1 calc R . . C2 C 0.8143(4) 0.9812(4) 0.1704(2) 0.0575(19) Uani 1 1 d . . . H2A H 0.7561 0.9828 0.1497 0.086 Uiso 1 1 calc R . . H2B H 0.8333 1.0364 0.1802 0.086 Uiso 1 1 calc R . . H2C H 0.8165 0.9484 0.1988 0.086 Uiso 1 1 calc R . . C3 C 0.8893(5) 1.0100(4) 0.0883(2) 0.063(2) Uani 1 1 d . . . H3A H 0.8336 1.0133 0.065 0.095 Uiso 1 1 calc R . . H3B H 0.9312 0.9919 0.0723 0.095 Uiso 1 1 calc R . . H3C H 0.9053 1.0635 0.1026 0.095 Uiso 1 1 calc R . . C4 C 0.7307(4) 0.7461(4) 0.0376(2) 0.0489(17) Uani 1 1 d . . . H4A H 0.752 0.6948 0.0535 0.073 Uiso 1 1 calc R . . H4B H 0.7618 0.7596 0.0144 0.073 Uiso 1 1 calc R . . H4C H 0.6704 0.7406 0.021 0.073 Uiso 1 1 calc R . . C5 C 0.6764(4) 0.8121(4) 0.1237(2) 0.0553(18) Uani 1 1 d . . . H5A H 0.6853 0.8562 0.1471 0.083 Uiso 1 1 calc R . . H5B H 0.6906 0.7603 0.1404 0.083 Uiso 1 1 calc R . . H5C H 0.617 0.8115 0.1047 0.083 Uiso 1 1 calc R . . C6 C 0.7013(4) 0.9199(4) 0.0465(2) 0.062(2) Uani 1 1 d . . . H6A H 0.706 0.9671 0.0676 0.093 Uiso 1 1 calc R . . H6B H 0.6416 0.9104 0.0297 0.093 Uiso 1 1 calc R . . H6C H 0.733 0.93 0.0231 0.093 Uiso 1 1 calc R . . C7 C 1.0901(4) 0.9155(4) 0.0700(2) 0.067(2) Uani 1 1 d . . . H7A H 1.1489 0.9031 0.0872 0.101 Uiso 1 1 calc R . . H7B H 1.0624 0.9422 0.0917 0.101 Uiso 1 1 calc R . . H7C H 1.0889 0.9515 0.043 0.101 Uiso 1 1 calc R . . C8 C 0.9209(4) 0.8426(4) 0.01380(19) 0.0504(17) Uani 1 1 d . . . H8A H 0.8909 0.8628 0.0363 0.076 Uiso 1 1 calc R . . H8B H 0.893 0.7934 -0.0019 0.076 Uiso 1 1 calc R . . H8C H 0.9201 0.8841 -0.0104 0.076 Uiso 1 1 calc R . . C9 C 1.0794(4) 0.7824(4) -0.0011(2) 0.0601(19) Uani 1 1 d . . . H9A H 1.139 0.7685 0.013 0.09 Uiso 1 1 calc R . . H9B H 1.0751 0.8253 -0.025 0.09 Uiso 1 1 calc R . . H9C H 1.0485 0.7344 -0.0165 0.09 Uiso 1 1 calc R . . C10 C 1.2302(4) 0.7484(4) 0.1211(2) 0.060(2) Uani 1 1 d . . . H10A H 1.2302 0.7814 0.0931 0.09 Uiso 1 1 calc R . . H10B H 1.279 0.7117 0.1284 0.09 Uiso 1 1 calc R . . H10C H 1.2338 0.784 0.1486 0.09 Uiso 1 1 calc R . . C11 C 1.1309(4) 0.6252(4) 0.1621(2) 0.0563(18) Uani 1 1 d . . . H11A H 1.0786 0.5934 0.1556 0.085 Uiso 1 1 calc R . . H11B H 1.1348 0.661 0.1895 0.085 Uiso 1 1 calc R . . H11C H 1.1797 0.5885 0.1693 0.085 Uiso 1 1 calc R . . C12 C 1.1379(4) 0.6111(4) 0.0621(2) 0.065(2) Uani 1 1 d . . . H12A H 1.1377 0.639 0.0323 0.097 Uiso 1 1 calc R . . H12B H 1.0894 0.5741 0.0561 0.097 Uiso 1 1 calc R . . H12C H 1.1904 0.5801 0.0736 0.097 Uiso 1 1 calc R . . C13 C 0.9075(4) 0.6130(4) 0.0176(2) 0.0569(19) Uani 1 1 d . . . H13A H 0.9599 0.6438 0.0305 0.085 Uiso 1 1 calc R . . H13B H 0.861 0.6505 0.0037 0.085 Uiso 1 1 calc R . . H13C H 0.9147 0.5758 -0.0073 0.085 Uiso 1 1 calc R . . C14 C 0.7828(4) 0.4997(4) 0.0355(2) 0.065(2) Uani 1 1 d . . . H14A H 0.7376 0.5393 0.0233 0.098 Uiso 1 1 calc R . . H14B H 0.7668 0.4633 0.0582 0.098 Uiso 1 1 calc R . . H14C H 0.7916 0.468 0.0088 0.098 Uiso 1 1 calc R . . C15 C 0.9649(4) 0.4742(4) 0.0882(2) 0.063(2) Uani 1 1 d . . . H15A H 1.0189 0.4998 0.1046 0.094 Uiso 1 1 calc R . . H15B H 0.9716 0.4428 0.0608 0.094 Uiso 1 1 calc R . . H15C H 0.9474 0.438 0.1104 0.094 Uiso 1 1 calc R . . C16 C 0.6886(4) 0.5862(4) 0.1111(2) 0.0512(17) Uani 1 1 d . . . H16A H 0.6786 0.5539 0.0818 0.077 Uiso 1 1 calc R . . H16B H 0.6724 0.6426 0.1028 0.077 Uiso 1 1 calc R . . H16C H 0.6547 0.5644 0.1312 0.077 Uiso 1 1 calc R . . C17 C 0.8253(4) 0.4742(4) 0.1648(2) 0.0509(17) Uani 1 1 d . . . H17A H 0.821 0.4394 0.1369 0.076 Uiso 1 1 calc R . . H17B H 0.7839 0.4567 0.1814 0.076 Uiso 1 1 calc R . . H17C H 0.8824 0.4701 0.1867 0.076 Uiso 1 1 calc R . . C18 C 0.8132(4) 0.6450(4) 0.1996(2) 0.0559(18) Uani 1 1 d . . . H18A H 0.8024 0.7019 0.1903 0.084 Uiso 1 1 calc R . . H18B H 0.8704 0.6396 0.2212 0.084 Uiso 1 1 calc R . . H18C H 0.7719 0.6266 0.216 0.084 Uiso 1 1 calc R . . C19 C 1.0446(4) 0.5244(4) 0.2459(2) 0.0499(17) Uani 1 1 d . . . H19A H 1.1009 0.5479 0.2502 0.075 Uiso 1 1 calc R . . H19B H 1.0025 0.5577 0.2233 0.075 Uiso 1 1 calc R . . H19C H 1.0435 0.4692 0.2333 0.075 Uiso 1 1 calc R . . C20 C 0.9120(4) 0.4765(4) 0.2937(2) 0.0541(18) Uani 1 1 d . . . H20A H 0.8964 0.4738 0.3238 0.081 Uiso 1 1 calc R . . H20B H 0.912 0.4218 0.2806 0.081 Uiso 1 1 calc R . . H20C H 0.871 0.5103 0.2707 0.081 Uiso 1 1 calc R . . C21 C 1.0953(4) 0.4449(4) 0.3416(2) 0.0579(19) Uani 1 1 d . . . H21A H 1.0856 0.4399 0.3732 0.087 Uiso 1 1 calc R . . H21B H 1.1536 0.4628 0.3452 0.087 Uiso 1 1 calc R . . H21C H 1.0862 0.3922 0.3254 0.087 Uiso 1 1 calc R . . C22 C 0.8725(4) 0.6462(4) 0.3643(2) 0.0545(18) Uani 1 1 d . . . H22A H 0.8596 0.6944 0.3439 0.082 Uiso 1 1 calc R . . H22B H 0.8546 0.6553 0.3934 0.082 Uiso 1 1 calc R . . H22C H 0.8424 0.5993 0.347 0.082 Uiso 1 1 calc R . . C23 C 1.0463(4) 0.7079(4) 0.4227(2) 0.0479(17) Uani 1 1 d . . . H23A H 1.0411 0.7594 0.4053 0.072 Uiso 1 1 calc R . . H23B H 1.1062 0.6934 0.435 0.072 Uiso 1 1 calc R . . H23C H 1.0214 0.7135 0.4495 0.072 Uiso 1 1 calc R . . C24 C 1.0066(4) 0.5339(4) 0.4199(2) 0.0599(19) Uani 1 1 d . . . H24A H 0.9785 0.4874 0.4011 0.09 Uiso 1 1 calc R . . H24B H 0.9829 0.5426 0.4469 0.09 Uiso 1 1 calc R . . H24C H 1.0673 0.5231 0.432 0.09 Uiso 1 1 calc R . . C25 C 1.2817(4) 0.5420(4) 0.3121(2) 0.062(2) Uani 1 1 d . . . H25A H 1.3027 0.556 0.2847 0.092 Uiso 1 1 calc R . . H25B H 1.2253 0.5178 0.3006 0.092 Uiso 1 1 calc R . . H25C H 1.3203 0.5032 0.3326 0.092 Uiso 1 1 calc R . . C26 C 1.2360(4) 0.6108(4) 0.39947(19) 0.0465(16) Uani 1 1 d . . . H26A H 1.2331 0.6604 0.4175 0.07 Uiso 1 1 calc R . . H26B H 1.2746 0.5721 0.4202 0.07 Uiso 1 1 calc R . . H26C H 1.1795 0.5867 0.3883 0.07 Uiso 1 1 calc R . . C27 C 1.3881(4) 0.6670(5) 0.3751(2) 0.062(2) Uani 1 1 d . . . H27A H 1.4146 0.6816 0.3499 0.093 Uiso 1 1 calc R . . H27B H 1.4192 0.6218 0.394 0.093 Uiso 1 1 calc R . . H27C H 1.3894 0.7138 0.3961 0.093 Uiso 1 1 calc R . . C28 C 1.3302(4) 0.7138(5) 0.2467(2) 0.066(2) Uani 1 1 d . . . H28A H 1.3717 0.6798 0.2692 0.098 Uiso 1 1 calc R . . H28B H 1.3596 0.7513 0.2306 0.098 Uiso 1 1 calc R . . H28C H 1.2919 0.6793 0.2228 0.098 Uiso 1 1 calc R . . C29 C 1.1893(4) 0.8366(4) 0.2359(2) 0.063(2) Uani 1 1 d . . . H29A H 1.1479 0.8014 0.2142 0.095 Uiso 1 1 calc R . . H29B H 1.2188 0.8692 0.2174 0.095 Uiso 1 1 calc R . . H29C H 1.1602 0.8726 0.253 0.095 Uiso 1 1 calc R . . C30 C 1.3428(4) 0.8464(5) 0.3187(3) 0.076(2) Uani 1 1 d . . . H30A H 1.3857 0.8168 0.3429 0.113 Uiso 1 1 calc R . . H30B H 1.3116 0.8827 0.3344 0.113 Uiso 1 1 calc R . . H30C H 1.3703 0.8784 0.2988 0.113 Uiso 1 1 calc R . . C31 C 0.9302(4) 0.9831(4) 0.2972(2) 0.0543(18) Uani 1 1 d . . . H31A H 0.9675 1.0184 0.3211 0.081 Uiso 1 1 calc R . . H31B H 0.8713 1.0001 0.2923 0.081 Uiso 1 1 calc R . . H31C H 0.9452 0.9871 0.2669 0.081 Uiso 1 1 calc R . . C32 C 0.8700(4) 0.8127(4) 0.2715(2) 0.0561(18) Uani 1 1 d . . . H32A H 0.8744 0.7557 0.2814 0.084 Uiso 1 1 calc R . . H32B H 0.8857 0.8181 0.2415 0.084 Uiso 1 1 calc R . . H32C H 0.8117 0.8314 0.2666 0.084 Uiso 1 1 calc R . . C33 C 0.8999(4) 0.8700(4) 0.3718(2) 0.0544(18) Uani 1 1 d . . . H33A H 0.9051 0.8144 0.3842 0.082 Uiso 1 1 calc R . . H33B H 0.8402 0.886 0.3623 0.082 Uiso 1 1 calc R . . H33C H 0.9318 0.9068 0.3968 0.082 Uiso 1 1 calc R . . C34 C 1.2179(4) 0.8448(4) 0.4021(2) 0.0583(19) Uani 1 1 d . . . H34A H 1.2425 0.8142 0.3803 0.087 Uiso 1 1 calc R . . H34B H 1.2001 0.8071 0.4235 0.087 Uiso 1 1 calc R . . H34C H 1.2602 0.8823 0.4211 0.087 Uiso 1 1 calc R . . C35 C 1.0881(5) 0.9575(5) 0.4144(2) 0.075(2) Uani 1 1 d . . . H35A H 1.0384 0.9906 0.3994 0.112 Uiso 1 1 calc R . . H35B H 1.1337 0.9925 0.433 0.112 Uiso 1 1 calc R . . H35C H 1.0733 0.9176 0.4357 0.112 Uiso 1 1 calc R . . C36 C 1.1593(5) 0.9843(4) 0.3307(3) 0.072(2) Uani 1 1 d . . . H36A H 1.1098 1.0146 0.3122 0.108 Uiso 1 1 calc R . . H36B H 1.1878 0.9593 0.3088 0.108 Uiso 1 1 calc R . . H36C H 1.1985 1.0213 0.3524 0.108 Uiso 1 1 calc R . . O1A O 1.0286(18) 0.6953(18) 0.2127(6) 0.033(6) Uiso 0.34(3) 1 d P . . O2A O 0.9836(17) 0.7673(18) 0.2194(6) 0.027(5) Uiso 0.34(3) 1 d P . . O1B O 1.050(3) 0.728(4) 0.2076(13) 0.015(14) Uiso 0.11(3) 1 d P . . O2B O 0.965(3) 0.733(6) 0.2194(15) 0.030(16) Uiso 0.11(3) 1 d P . . C37 C 1.0342(9) 1.1296(9) 0.4856(5) 0.180(6) Uiso 1 1 d . . . H37A H 1.021 1.0776 0.4689 0.27 Uiso 1 1 calc R . . H37B H 0.9846 1.149 0.4947 0.27 Uiso 1 1 calc R . . H37C H 1.0817 1.1226 0.5143 0.27 Uiso 1 1 calc R . . C38 C 1.0564(13) 1.1870(14) 0.4549(7) 0.251(9) Uiso 1 1 d . . . H38A H 1.0081 1.1855 0.4256 0.301 Uiso 1 1 calc R . . H38B H 1.1039 1.1609 0.4458 0.301 Uiso 1 1 calc R . . C39 C 1.0827(13) 1.2816(13) 0.4604(7) 0.260(9) Uiso 1 1 d . . . H39A H 1.0981 1.3046 0.4325 0.312 Uiso 1 1 calc R . . H39B H 1.0418 1.3168 0.4703 0.312 Uiso 1 1 calc R . . C40 C 1.1521(12) 1.2579(11) 0.4981(6) 0.213(7) Uiso 1 1 d . . . H40A H 1.1907 1.2186 0.4893 0.256 Uiso 1 1 calc R . . H40B H 1.1383 1.2421 0.5279 0.256 Uiso 1 1 calc R . . C41 C 1.1795(8) 1.3595(8) 0.4950(5) 0.171(5) Uiso 1 1 d . . . H41A H 1.2325 1.3706 0.5197 0.257 Uiso 1 1 calc R . . H41B H 1.1346 1.394 0.5004 0.257 Uiso 1 1 calc R . . H41C H 1.1869 1.3709 0.4634 0.257 Uiso 1 1 calc R . . C42 C 0.8667(8) 0.2507(7) 0.1258(4) 0.142(4) Uiso 1 1 d . . . H42A H 0.8116 0.2527 0.1016 0.214 Uiso 1 1 calc R . . H42B H 0.9002 0.206 0.1184 0.214 Uiso 1 1 calc R . . H42C H 0.8966 0.302 0.1255 0.214 Uiso 1 1 calc R . . C43 C 0.8541(8) 0.2382(8) 0.1726(5) 0.150(5) Uiso 1 1 d . . . H43A H 0.8157 0.2821 0.1766 0.18 Uiso 1 1 calc R . . H43B H 0.8213 0.1872 0.17 0.18 Uiso 1 1 calc R . . C44 C 0.9157(7) 0.2334(7) 0.2155(4) 0.132(4) Uiso 1 1 d . . . H44A H 0.9472 0.2851 0.2185 0.158 Uiso 1 1 calc R . . H44B H 0.9551 0.1907 0.2111 0.158 Uiso 1 1 calc R . . C45 C 0.9040(8) 0.2186(8) 0.2622(5) 0.153(5) Uiso 1 1 d . . . H45A H 0.8624 0.2593 0.2664 0.184 Uiso 1 1 calc R . . H45B H 0.8758 0.1652 0.2603 0.184 Uiso 1 1 calc R . . C46 C 0.9686(8) 0.2183(7) 0.3046(4) 0.148(5) Uiso 1 1 d . . . H46A H 0.9451 0.2072 0.3314 0.222 Uiso 1 1 calc R . . H46B H 0.9966 0.2713 0.3091 0.222 Uiso 1 1 calc R . . H46C H 1.0098 0.1762 0.3031 0.222 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 0.02726(18) 0.03010(18) 0.02659(16) -0.00222(14) 0.00483(13) 0.00183(15) Ce2 0.02755(18) 0.02876(19) 0.02725(17) -0.00081(14) 0.00530(13) -0.00070(15) Si1 0.0436(10) 0.0306(10) 0.0474(10) 0.0018(8) 0.0066(8) 0.0056(8) Si2 0.0366(10) 0.0423(11) 0.0434(9) 0.0005(8) 0.0031(7) 0.0087(8) Si3 0.0483(11) 0.0523(12) 0.0343(9) 0.0037(8) 0.0121(8) -0.0031(9) Si4 0.0374(10) 0.0606(12) 0.0394(9) 0.0012(9) 0.0151(8) 0.0086(9) Si5 0.0468(11) 0.0414(11) 0.0465(10) -0.0159(8) 0.0108(8) -0.0024(8) Si6 0.0413(10) 0.0346(10) 0.0423(9) -0.0067(7) 0.0084(8) -0.0056(8) Si7 0.0469(11) 0.0318(10) 0.0438(9) 0.0029(8) 0.0116(8) -0.0019(8) Si8 0.0420(10) 0.0414(10) 0.0417(9) 0.0032(8) 0.0145(8) -0.0045(8) Si9 0.0318(9) 0.0522(12) 0.0422(10) 0.0060(8) 0.0037(7) 0.0059(8) Si10 0.0343(10) 0.0647(13) 0.0497(10) 0.0117(9) 0.0081(8) -0.0040(9) Si11 0.0450(10) 0.0356(10) 0.0418(9) -0.0082(8) 0.0089(8) 0.0029(8) Si12 0.0545(12) 0.0423(11) 0.0487(10) -0.0128(8) 0.0045(9) -0.0099(9) O1 0.059(9) 0.029(7) 0.038(5) 0.001(4) 0.007(5) -0.023(6) O2 0.075(11) 0.041(8) 0.044(5) -0.001(4) 0.019(6) -0.037(8) N1 0.038(3) 0.034(3) 0.031(2) 0.001(2) 0.004(2) 0.006(2) N2 0.033(3) 0.040(3) 0.029(2) -0.002(2) 0.010(2) -0.003(2) N3 0.029(3) 0.036(3) 0.038(3) -0.007(2) 0.005(2) -0.002(2) N4 0.036(3) 0.031(3) 0.035(3) 0.001(2) 0.009(2) -0.001(2) N5 0.029(3) 0.039(3) 0.034(2) 0.003(2) 0.008(2) -0.002(2) N6 0.039(3) 0.029(3) 0.033(2) -0.007(2) 0.007(2) 0.001(2) C1 0.045(4) 0.042(4) 0.057(4) 0.000(3) 0.005(3) -0.005(3) C2 0.063(5) 0.044(4) 0.061(4) -0.011(3) 0.011(4) 0.015(4) C3 0.076(5) 0.040(4) 0.071(5) 0.008(3) 0.018(4) 0.004(4) C4 0.041(4) 0.054(5) 0.043(4) -0.004(3) -0.003(3) 0.000(3) C5 0.042(4) 0.059(5) 0.068(4) -0.012(4) 0.019(3) 0.010(3) C6 0.053(4) 0.059(5) 0.062(4) 0.008(4) -0.005(3) 0.010(4) C7 0.065(5) 0.069(5) 0.068(5) 0.004(4) 0.020(4) -0.020(4) C8 0.052(4) 0.065(5) 0.033(3) 0.014(3) 0.009(3) 0.006(3) C9 0.063(5) 0.083(6) 0.040(4) 0.004(3) 0.024(3) 0.006(4) C10 0.041(4) 0.092(6) 0.048(4) 0.012(4) 0.013(3) -0.003(4) C11 0.050(4) 0.071(5) 0.050(4) 0.010(3) 0.018(3) 0.010(4) C12 0.065(5) 0.073(5) 0.061(4) -0.009(4) 0.025(4) 0.022(4) C13 0.057(4) 0.068(5) 0.044(4) -0.017(3) 0.013(3) 0.003(4) C14 0.068(5) 0.068(5) 0.060(4) -0.030(4) 0.017(4) -0.017(4) C15 0.067(5) 0.050(5) 0.075(5) -0.013(4) 0.025(4) 0.005(4) C16 0.048(4) 0.048(4) 0.059(4) -0.008(3) 0.018(3) -0.009(3) C17 0.052(4) 0.042(4) 0.053(4) -0.005(3) 0.006(3) -0.009(3) C18 0.058(4) 0.055(4) 0.056(4) -0.014(3) 0.017(3) 0.000(4) C19 0.058(4) 0.047(4) 0.047(4) -0.005(3) 0.018(3) 0.006(3) C20 0.063(5) 0.044(4) 0.053(4) 0.000(3) 0.012(3) -0.018(3) C21 0.073(5) 0.031(4) 0.067(4) 0.008(3) 0.014(4) 0.010(3) C22 0.045(4) 0.060(5) 0.066(4) -0.008(3) 0.029(3) -0.015(3) C23 0.047(4) 0.059(5) 0.036(3) -0.002(3) 0.009(3) -0.001(3) C24 0.076(5) 0.052(5) 0.051(4) 0.013(3) 0.018(4) -0.007(4) C25 0.049(4) 0.065(5) 0.066(4) 0.005(4) 0.009(3) 0.020(4) C26 0.044(4) 0.052(4) 0.039(3) 0.015(3) 0.004(3) 0.003(3) C27 0.033(4) 0.096(6) 0.050(4) 0.015(4) 0.001(3) 0.003(4) C28 0.037(4) 0.108(7) 0.050(4) 0.017(4) 0.010(3) 0.006(4) C29 0.060(5) 0.063(5) 0.069(5) 0.026(4) 0.022(4) 0.008(4) C30 0.052(5) 0.084(6) 0.091(6) 0.008(5) 0.022(4) -0.026(4) C31 0.070(5) 0.040(4) 0.049(4) -0.009(3) 0.011(3) 0.012(3) C32 0.045(4) 0.061(5) 0.059(4) -0.006(4) 0.008(3) 0.001(4) C33 0.059(4) 0.046(4) 0.061(4) -0.007(3) 0.020(3) 0.008(3) C34 0.052(4) 0.069(5) 0.047(4) -0.017(3) 0.002(3) -0.015(4) C35 0.084(6) 0.072(5) 0.063(5) -0.043(4) 0.012(4) -0.001(4) C36 0.079(5) 0.051(5) 0.081(5) -0.010(4) 0.014(4) -0.020(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 N1 2.258(4) . ? Ce1 N3 2.259(4) . ? Ce1 N2 2.259(4) . ? Ce1 O1B 2.27(3) . ? Ce1 O2B 2.32(4) . ? Ce1 O1A 2.323(16) . ? Ce1 O2 2.329(8) . ? Ce1 O2A 2.358(17) . ? Ce1 O1 2.361(8) . ? Ce2 N5 2.248(4) . ? Ce2 N6 2.259(4) . ? Ce2 N4 2.270(4) . ? Ce2 O1A 2.316(16) . ? Ce2 O1 2.333(8) . ? Ce2 O2 2.338(8) . ? Ce2 O2A 2.349(15) . ? Ce2 O2B 2.38(4) . ? Ce2 O1B 2.43(4) . ? Si1 N1 1.752(5) . ? Si1 C2 1.877(6) . ? Si1 C1 1.8848(16) . ? Si1 C3 1.889(6) . ? Si2 N1 1.771(4) . ? Si2 C4 1.863(6) . ? Si2 C5 1.872(6) . ? Si2 C6 1.876(6) . ? Si3 N2 1.770(4) . ? Si3 C8 1.868(6) . ? Si3 C9 1.872(6) . ? Si3 C7 1.878(7) . ? Si4 N2 1.752(5) . ? Si4 C11 1.871(6) . ? Si4 C10 1.873(6) . ? Si4 C12 1.874(6) . ? Si5 N3 1.770(5) . ? Si5 C13 1.861(7) . ? Si5 C15 1.865(7) . ? Si5 C14 1.872(6) . ? Si6 N3 1.748(5) . ? Si6 C17 1.867(6) . ? Si6 C16 1.876(6) . ? Si6 C18 1.877(6) . ? Si7 N4 1.757(5) . ? Si7 C20 1.861(6) . ? Si7 C19 1.873(6) . ? Si7 C21 1.886(6) . ? Si8 N4 1.767(5) . ? Si8 C24 1.872(6) . ? Si8 C23 1.873(6) . ? Si8 C22 1.874(6) . ? Si9 N5 1.764(4) . ? Si9 C26 1.861(6) . ? Si9 C25 1.869(7) . ? Si9 C27 1.879(6) . ? Si10 N5 1.759(5) . ? Si10 C30 1.867(7) . ? Si10 C29 1.870(6) . ? Si10 C28 1.871(7) . ? Si11 N6 1.755(5) . ? Si11 C33 1.866(6) . ? Si11 C32 1.870(6) . ? Si11 C31 1.876(6) . ? Si12 N6 1.759(4) . ? Si12 C34 1.862(7) . ? Si12 C36 1.880(7) . ? Si12 C35 1.889(7) . ? O1 O2 1.469(18) . ? O1A O2A 1.44(3) . ? O1B O2B 1.52(9) . ? C37 C38 1.42(2) . ? C38 C39 1.62(2) . ? C39 C40 1.40(2) . ? C40 C41 1.744(18) . ? C42 C43 1.447(14) . ? C43 C44 1.374(13) . ? C44 C45 1.444(14) . ? C45 C46 1.385(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ce1 N3 107.41(16) . . ? N1 Ce1 N2 106.58(16) . . ? N3 Ce1 N2 108.01(16) . . ? N1 Ce1 O1B 123.7(16) . . ? N3 Ce1 O1B 115.9(17) . . ? N2 Ce1 O1B 92.7(14) . . ? N1 Ce1 O2B 99.6(19) . . ? N3 Ce1 O2B 103(2) . . ? N2 Ce1 O2B 130.9(15) . . ? O1B Ce1 O2B 39(2) . . ? N1 Ce1 O1A 129.2(5) . . ? N3 Ce1 O1A 100.1(9) . . ? N2 Ce1 O1A 104.1(8) . . ? N1 Ce1 O2 101.9(7) . . ? N3 Ce1 O2 127.5(3) . . ? N2 Ce1 O2 103.8(7) . . ? N1 Ce1 O2A 93.4(5) . . ? N3 Ce1 O2A 118.2(9) . . ? N2 Ce1 O2A 120.7(8) . . ? O1A Ce1 O2A 35.9(8) . . ? N1 Ce1 O1 120.4(6) . . ? N3 Ce1 O1 91.1(3) . . ? N2 Ce1 O1 120.8(7) . . ? O2 Ce1 O1 36.5(4) . . ? N5 Ce2 N6 107.68(16) . . ? N5 Ce2 N4 105.74(15) . . ? N6 Ce2 N4 108.07(16) . . ? N5 Ce2 O1A 101.2(7) . . ? N6 Ce2 O1A 127.2(6) . . ? N4 Ce2 O1A 105.1(9) . . ? N5 Ce2 O1 117.0(7) . . ? N6 Ce2 O1 122.2(6) . . ? N4 Ce2 O1 93.6(3) . . ? N5 Ce2 O2 107.1(7) . . ? N6 Ce2 O2 97.4(6) . . ? N4 Ce2 O2 129.2(4) . . ? O1 Ce2 O2 36.6(4) . . ? N5 Ce2 O2A 124.2(8) . . ? N6 Ce2 O2A 91.8(6) . . ? N4 Ce2 O2A 117.1(9) . . ? O1A Ce2 O2A 36.0(8) . . ? N5 Ce2 O2B 130.8(13) . . ? N6 Ce2 O2B 101(2) . . ? N4 Ce2 O2B 102(2) . . ? N5 Ce2 O1B 93.9(11) . . ? N6 Ce2 O1B 117.7(15) . . ? N4 Ce2 O1B 121.2(16) . . ? N1 Si1 C2 112.0(3) . . ? N1 Si1 C1 111.03(16) . . ? C2 Si1 C1 106.7(2) . . ? N1 Si1 C3 115.1(3) . . ? C2 Si1 C3 106.3(3) . . ? C1 Si1 C3 105.2(2) . . ? N1 Si2 C4 111.5(2) . . ? N1 Si2 C5 110.7(3) . . ? C4 Si2 C5 111.1(3) . . ? N1 Si2 C6 114.8(3) . . ? C4 Si2 C6 103.2(3) . . ? C5 Si2 C6 105.2(3) . . ? N2 Si3 C8 112.2(3) . . ? N2 Si3 C9 114.6(3) . . ? C8 Si3 C9 103.3(3) . . ? N2 Si3 C7 111.3(3) . . ? C8 Si3 C7 109.4(3) . . ? C9 Si3 C7 105.6(3) . . ? N2 Si4 C11 108.7(3) . . ? N2 Si4 C10 112.6(3) . . ? C11 Si4 C10 109.1(3) . . ? N2 Si4 C12 116.0(3) . . ? C11 Si4 C12 104.0(3) . . ? C10 Si4 C12 105.9(3) . . ? N3 Si5 C13 111.7(3) . . ? N3 Si5 C15 111.5(3) . . ? C13 Si5 C15 109.6(3) . . ? N3 Si5 C14 113.8(3) . . ? C13 Si5 C14 103.4(3) . . ? C15 Si5 C14 106.4(3) . . ? N3 Si6 C17 112.7(3) . . ? N3 Si6 C16 115.5(3) . . ? C17 Si6 C16 106.3(3) . . ? N3 Si6 C18 109.5(3) . . ? C17 Si6 C18 107.5(3) . . ? C16 Si6 C18 104.8(3) . . ? N4 Si7 C20 112.6(3) . . ? N4 Si7 C19 110.5(3) . . ? C20 Si7 C19 106.9(3) . . ? N4 Si7 C21 115.1(3) . . ? C20 Si7 C21 106.2(3) . . ? C19 Si7 C21 104.8(3) . . ? N4 Si8 C24 114.9(3) . . ? N4 Si8 C23 111.4(3) . . ? C24 Si8 C23 103.5(3) . . ? N4 Si8 C22 111.0(3) . . ? C24 Si8 C22 105.8(3) . . ? C23 Si8 C22 109.8(3) . . ? N5 Si9 C26 112.1(3) . . ? N5 Si9 C25 110.5(3) . . ? C26 Si9 C25 110.3(3) . . ? N5 Si9 C27 114.7(3) . . ? C26 Si9 C27 103.4(3) . . ? C25 Si9 C27 105.4(3) . . ? N5 Si10 C30 115.8(3) . . ? N5 Si10 C29 108.6(3) . . ? C30 Si10 C29 105.2(3) . . ? N5 Si10 C28 112.3(3) . . ? C30 Si10 C28 106.5(3) . . ? C29 Si10 C28 108.0(3) . . ? N6 Si11 C33 114.5(3) . . ? N6 Si11 C32 110.0(3) . . ? C33 Si11 C32 105.6(3) . . ? N6 Si11 C31 112.6(3) . . ? C33 Si11 C31 106.9(3) . . ? C32 Si11 C31 106.7(3) . . ? N6 Si12 C34 112.4(3) . . ? N6 Si12 C36 111.1(3) . . ? C34 Si12 C36 110.2(3) . . ? N6 Si12 C35 113.9(3) . . ? C34 Si12 C35 102.7(3) . . ? C36 Si12 C35 106.1(4) . . ? Ce2 O1 Ce1 142.4(5) . . ? Ce1 O2 Ce2 144.4(5) . . ? Si1 N1 Si2 115.0(2) . . ? Si1 N1 Ce1 119.3(2) . . ? Si2 N1 Ce1 125.7(2) . . ? Si4 N2 Si3 115.2(3) . . ? Si4 N2 Ce1 118.2(2) . . ? Si3 N2 Ce1 126.5(2) . . ? Si6 N3 Si5 114.2(2) . . ? Si6 N3 Ce1 120.0(2) . . ? Si5 N3 Ce1 125.7(2) . . ? Si7 N4 Si8 114.6(2) . . ? Si7 N4 Ce2 120.3(2) . . ? Si8 N4 Ce2 125.0(2) . . ? Si10 N5 Si9 114.6(2) . . ? Si10 N5 Ce2 118.3(2) . . ? Si9 N5 Ce2 127.0(2) . . ? Si11 N6 Si12 114.9(2) . . ? Si11 N6 Ce2 119.2(2) . . ? Si12 N6 Ce2 125.8(2) . . ? Ce2 O1A Ce1 146.6(10) . . ? Ce2 O2A Ce1 141.5(10) . . ? Ce1 O1B Ce2 142(2) . . ? Ce1 O2B Ce2 142(3) . . ? C37 C38 C39 133.7(17) . . ? C40 C39 C38 86.9(15) . . ? C39 C40 C41 81.8(13) . . ? C44 C43 C42 127.0(13) . . ? C43 C44 C45 127.4(12) . . ? C46 C45 C44 124.5(12) . . ? #===END data_(10)-oct1404 _database_code_depnum_ccdc_archive 'CCDC 774601' #TrackingRef '- mfl_28jul2009.CIF' _audit_creation_date 2004-10-15T14:10:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C72 H60 Ce2 N6, 2.5(C6 H6)' _chemical_formula_sum 'C87 H75 Ce2 N6' _chemical_formula_weight 1484.83 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.8388(3) _cell_length_b 21.3584(4) _cell_length_c 44.6247(9) _cell_angle_alpha 90 _cell_angle_beta 98.467(1) _cell_angle_gamma 90 _cell_volume 13988.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 124379 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 23.257 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.42 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6040 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7551 _exptl_absorpt_correction_T_max 0.8154 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.18462E-2 _diffrn_orient_matrix_ub_12 -0.384045E-1 _diffrn_orient_matrix_ub_13 -0.127131E-1 _diffrn_orient_matrix_ub_21 -0.350862E-1 _diffrn_orient_matrix_ub_22 -0.234727E-1 _diffrn_orient_matrix_ub_23 0.138636E-1 _diffrn_orient_matrix_ub_31 -0.583758E-1 _diffrn_orient_matrix_ub_32 0.128935E-1 _diffrn_orient_matrix_ub_33 -0.126284E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.0269 _diffrn_reflns_number 71708 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 23.28 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 9989 _reflns_number_gt 8860 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The diffraction was not visible at higher angle. 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^)+(0.0162P)^2^+26.1771P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9989 _refine_ls_number_parameters 857 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0513 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.324 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.188077(10) 0.398023(7) 0.157571(4) 0.02444(5) Uani 1 1 d . . . Ce2 Ce -0.052339(10) 0.442554(7) 0.107435(4) 0.02574(5) Uani 1 1 d . . . N1 N 0.34161(15) 0.39734(10) 0.14942(5) 0.0302(6) Uani 1 1 d . . . N2 N 0.18653(15) 0.35288(10) 0.20561(5) 0.0306(6) Uani 1 1 d . . . N3 N -0.09448(15) 0.53873(10) 0.08504(5) 0.0296(6) Uani 1 1 d . . . N4 N -0.18499(15) 0.38084(10) 0.10748(5) 0.0275(5) Uani 1 1 d . . . N5 N 0.08893(14) 0.37371(10) 0.10821(5) 0.0261(5) Uani 1 1 d . . . N6 N 0.05422(14) 0.47611(10) 0.15505(5) 0.0250(5) Uani 1 1 d . . . C1 C 0.41838(18) 0.43692(13) 0.15475(6) 0.0296(7) Uani 1 1 d . . . C2 C 0.50191(19) 0.42213(14) 0.14545(7) 0.0379(8) Uani 1 1 d . . . H2 H 0.5093 0.3829 0.1361 0.046 Uiso 1 1 calc R . . C3 C 0.5736(2) 0.46377(16) 0.14966(8) 0.0490(9) Uani 1 1 d . . . H3 H 0.6298 0.4529 0.1432 0.059 Uiso 1 1 calc R . . C4 C 0.5649(2) 0.52106(16) 0.16315(8) 0.0503(9) Uani 1 1 d . . . H4 H 0.6143 0.5498 0.1659 0.06 Uiso 1 1 calc R . . C5 C 0.4831(2) 0.53607(14) 0.17264(7) 0.0412(8) Uani 1 1 d . . . H5 H 0.4764 0.5753 0.1821 0.049 Uiso 1 1 calc R . . C6 C 0.41081(19) 0.49469(13) 0.16852(6) 0.0325(7) Uani 1 1 d . . . H6 H 0.3551 0.5059 0.1752 0.039 Uiso 1 1 calc R . . C7 C 0.35436(18) 0.33232(13) 0.14849(7) 0.0305(7) Uani 1 1 d . . . C8 C 0.4181(2) 0.29960(14) 0.16928(8) 0.0439(8) Uani 1 1 d . . . H8 H 0.4588 0.3222 0.1838 0.053 Uiso 1 1 calc R . . C9 C 0.4220(2) 0.23533(16) 0.16883(9) 0.0526(9) Uani 1 1 d . . . H9 H 0.4661 0.2141 0.1828 0.063 Uiso 1 1 calc R . . C10 C 0.3623(2) 0.20110(15) 0.14820(9) 0.0533(10) Uani 1 1 d . . . H10 H 0.3654 0.1567 0.1481 0.064 Uiso 1 1 calc R . . C11 C 0.2992(2) 0.23135(15) 0.12805(8) 0.0491(9) Uani 1 1 d . . . H11 H 0.2576 0.208 0.1141 0.059 Uiso 1 1 calc R . . C12 C 0.2956(2) 0.29662(14) 0.12786(7) 0.0375(7) Uani 1 1 d . . . H12 H 0.2523 0.3172 0.1134 0.045 Uiso 1 1 calc R . . C13 C 0.24468(18) 0.39364(13) 0.22365(6) 0.0281(6) Uani 1 1 d . . . C14 C 0.3214(2) 0.37518(14) 0.24424(7) 0.0369(7) Uani 1 1 d . . . H14 H 0.3317 0.332 0.2484 0.044 Uiso 1 1 calc R . . C15 C 0.3813(2) 0.41865(16) 0.25833(7) 0.0424(8) Uani 1 1 d . . . H15 H 0.4314 0.405 0.2726 0.051 Uiso 1 1 calc R . . C16 C 0.3704(2) 0.48204(15) 0.25216(7) 0.0395(8) Uani 1 1 d . . . H16 H 0.4138 0.5115 0.2614 0.047 Uiso 1 1 calc R . . C17 C 0.29616(19) 0.50151(14) 0.23251(6) 0.0336(7) Uani 1 1 d . . . H17 H 0.288 0.5448 0.228 0.04 Uiso 1 1 calc R . . C18 C 0.23253(18) 0.45825(12) 0.21907(6) 0.0273(6) Uani 1 1 d . . . H18 H 0.1795 0.4729 0.2065 0.033 Uiso 1 1 calc R . . C19 C 0.17401(19) 0.29153(13) 0.21622(7) 0.0330(7) Uani 1 1 d . . . C20 C 0.1863(2) 0.24035(15) 0.19836(8) 0.0498(9) Uani 1 1 d . . . H20 H 0.2077 0.2463 0.1795 0.06 Uiso 1 1 calc R . . C21 C 0.1678(3) 0.18052(17) 0.20756(11) 0.0715(13) Uani 1 1 d . . . H21 H 0.1753 0.146 0.1947 0.086 Uiso 1 1 calc R . . C22 C 0.1391(3) 0.17028(18) 0.23471(12) 0.0794(14) Uani 1 1 d . . . H22 H 0.1276 0.129 0.2411 0.095 Uiso 1 1 calc R . . C23 C 0.1273(4) 0.2203(2) 0.25265(11) 0.0907(15) Uani 1 1 d . . . H23 H 0.1068 0.2139 0.2716 0.109 Uiso 1 1 calc R . . C24 C 0.1448(3) 0.28037(16) 0.24355(8) 0.0635(11) Uani 1 1 d . . . H24 H 0.1365 0.3146 0.2564 0.076 Uiso 1 1 calc R . . C25 C -0.02061(18) 0.57332(13) 0.07659(6) 0.0282(7) Uani 1 1 d . . . C26 C -0.0003(2) 0.63414(14) 0.08695(7) 0.0373(7) Uani 1 1 d . . . H26 H -0.0383 0.6541 0.0994 0.045 Uiso 1 1 calc R . . C27 C 0.0741(2) 0.66549(15) 0.07926(8) 0.0474(9) Uani 1 1 d . . . H27 H 0.0859 0.7073 0.086 0.057 Uiso 1 1 calc R . . C28 C 0.1315(2) 0.63687(17) 0.06189(8) 0.0505(9) Uani 1 1 d . . . H28 H 0.1829 0.6588 0.0568 0.061 Uiso 1 1 calc R . . C29 C 0.1145(2) 0.57717(17) 0.05202(8) 0.0466(9) Uani 1 1 d . . . H29 H 0.1551 0.557 0.0405 0.056 Uiso 1 1 calc R . . C30 C 0.0376(2) 0.54546(14) 0.05870(7) 0.0348(7) Uani 1 1 d . . . H30 H 0.0249 0.5045 0.051 0.042 Uiso 1 1 calc R . . C31 C -0.18166(19) 0.56491(13) 0.07804(6) 0.0304(7) Uani 1 1 d . . . C32 C -0.2039(2) 0.61087(14) 0.05601(7) 0.0357(7) Uani 1 1 d . . . H32 H -0.157 0.6297 0.0467 0.043 Uiso 1 1 calc R . . C33 C -0.2932(2) 0.62956(17) 0.04745(8) 0.0499(9) Uani 1 1 d . . . H33 H -0.3067 0.6605 0.0321 0.06 Uiso 1 1 calc R . . C34 C -0.3629(2) 0.60405(18) 0.06078(8) 0.0545(10) Uani 1 1 d . . . H34 H -0.4242 0.6162 0.0544 0.065 Uiso 1 1 calc R . . C35 C -0.3419(2) 0.56061(17) 0.08351(8) 0.0512(9) Uani 1 1 d . . . H35 H -0.3891 0.5437 0.0933 0.061 Uiso 1 1 calc R . . C36 C -0.2532(2) 0.54138(14) 0.09215(8) 0.0419(8) Uani 1 1 d . . . H36 H -0.2401 0.5116 0.108 0.05 Uiso 1 1 calc R . . C37 C -0.23087(17) 0.35026(12) 0.12864(6) 0.0269(6) Uani 1 1 d . . . C38 C -0.30151(19) 0.30740(14) 0.12132(7) 0.0367(7) Uani 1 1 d . . . H38 H -0.3186 0.2952 0.1008 0.044 Uiso 1 1 calc R . . C39 C -0.3471(2) 0.28239(15) 0.14333(8) 0.0438(8) Uani 1 1 d . . . H39 H -0.3944 0.2528 0.1377 0.053 Uiso 1 1 calc R . . C40 C -0.3255(2) 0.29955(14) 0.17318(8) 0.0422(8) Uani 1 1 d . . . H40 H -0.3575 0.2825 0.1882 0.051 Uiso 1 1 calc R . . C41 C -0.2561(2) 0.34210(15) 0.18072(7) 0.0433(8) Uani 1 1 d . . . H41 H -0.24 0.3546 0.2012 0.052 Uiso 1 1 calc R . . C42 C -0.20983(19) 0.36667(14) 0.15888(7) 0.0364(7) Uani 1 1 d . . . H42 H -0.162 0.3958 0.1647 0.044 Uiso 1 1 calc R . . C43 C -0.18933(17) 0.35612(13) 0.07814(6) 0.0294(7) Uani 1 1 d . . . C44 C -0.17549(19) 0.29241(14) 0.07206(7) 0.0355(7) Uani 1 1 d . . . H44 H -0.1698 0.2628 0.0881 0.043 Uiso 1 1 calc R . . C45 C -0.1702(2) 0.27298(15) 0.04299(8) 0.0447(8) Uani 1 1 d . . . H45 H -0.1619 0.2297 0.0392 0.054 Uiso 1 1 calc R . . C46 C -0.1767(2) 0.31493(17) 0.01912(8) 0.0475(9) Uani 1 1 d . . . H46 H -0.1725 0.3008 -0.0008 0.057 Uiso 1 1 calc R . . C47 C -0.1893(2) 0.37749(16) 0.02474(7) 0.0431(8) Uani 1 1 d . . . H47 H -0.193 0.4068 0.0086 0.052 Uiso 1 1 calc R . . C48 C -0.19675(19) 0.39806(14) 0.05385(7) 0.0343(7) Uani 1 1 d . . . H48 H -0.207 0.4412 0.0573 0.041 Uiso 1 1 calc R . . C49 C 0.10566(19) 0.38199(13) 0.07788(6) 0.0290(7) Uani 1 1 d . . . C50 C 0.1865(2) 0.41083(13) 0.07233(7) 0.0354(7) Uani 1 1 d . . . H50 H 0.2331 0.4199 0.0887 0.042 Uiso 1 1 calc R . . C51 C 0.1985(2) 0.42611(16) 0.04303(7) 0.0461(8) Uani 1 1 d . . . H51 H 0.2538 0.4452 0.0395 0.055 Uiso 1 1 calc R . . C52 C 0.1313(3) 0.41392(17) 0.01897(8) 0.0537(9) Uani 1 1 d . . . H52 H 0.1396 0.4255 -0.001 0.064 Uiso 1 1 calc R . . C53 C 0.0521(2) 0.38495(16) 0.02399(7) 0.0472(9) Uani 1 1 d . . . H53 H 0.0059 0.3761 0.0074 0.057 Uiso 1 1 calc R . . C54 C 0.0395(2) 0.36850(14) 0.05326(7) 0.0355(7) Uani 1 1 d . . . H54 H -0.015 0.3478 0.0565 0.043 Uiso 1 1 calc R . . C55 C 0.05394(17) 0.31572(12) 0.11696(6) 0.0275(7) Uani 1 1 d . . . C56 C 0.0623(2) 0.25861(13) 0.10206(7) 0.0374(7) Uani 1 1 d . . . H56 H 0.0905 0.2573 0.0843 0.045 Uiso 1 1 calc R . . C57 C 0.0295(2) 0.20436(14) 0.11324(8) 0.0475(9) Uani 1 1 d . . . H57 H 0.0364 0.1658 0.1032 0.057 Uiso 1 1 calc R . . C58 C -0.0131(2) 0.20469(15) 0.13873(9) 0.0506(9) Uani 1 1 d . . . H58 H -0.0368 0.1669 0.1457 0.061 Uiso 1 1 calc R . . C59 C -0.0212(2) 0.25968(14) 0.15390(8) 0.0423(8) Uani 1 1 d . . . H59 H -0.0495 0.2602 0.1717 0.051 Uiso 1 1 calc R . . C60 C 0.01254(18) 0.31500(13) 0.14307(7) 0.0317(7) Uani 1 1 d . . . H60 H 0.0072 0.353 0.1537 0.038 Uiso 1 1 calc R . . C61 C 0.11071(17) 0.52925(12) 0.15373(6) 0.0242(6) Uani 1 1 d . . . C62 C 0.11758(19) 0.57840(12) 0.17480(7) 0.0305(7) Uani 1 1 d . . . H62 H 0.079 0.5789 0.19 0.037 Uiso 1 1 calc R . . C63 C 0.1797(2) 0.62594(14) 0.17367(7) 0.0399(8) Uani 1 1 d . . . H63 H 0.1832 0.659 0.188 0.048 Uiso 1 1 calc R . . C64 C 0.2373(2) 0.62630(15) 0.15185(8) 0.0450(8) Uani 1 1 d . . . H64 H 0.2802 0.6591 0.1513 0.054 Uiso 1 1 calc R . . C65 C 0.2315(2) 0.57851(15) 0.13107(8) 0.0404(8) Uani 1 1 d . . . H65 H 0.2709 0.5783 0.1161 0.048 Uiso 1 1 calc R . . C66 C 0.16850(18) 0.53032(13) 0.13172(6) 0.0300(7) Uani 1 1 d . . . H66 H 0.1648 0.4979 0.117 0.036 Uiso 1 1 calc R . . C67 C -0.01660(17) 0.48269(12) 0.17336(6) 0.0260(6) Uani 1 1 d . . . C68 C -0.01917(19) 0.44714(13) 0.19938(6) 0.0312(7) Uani 1 1 d . . . H68 H 0.0289 0.4187 0.206 0.037 Uiso 1 1 calc R . . C69 C -0.0914(2) 0.45304(14) 0.21556(7) 0.0377(8) Uani 1 1 d . . . H69 H -0.092 0.4291 0.2335 0.045 Uiso 1 1 calc R . . C70 C -0.1623(2) 0.49334(16) 0.20597(8) 0.0454(8) Uani 1 1 d . . . H70 H -0.2118 0.4968 0.2172 0.054 Uiso 1 1 calc R . . C71 C -0.1616(2) 0.52856(15) 0.18024(8) 0.0441(8) Uani 1 1 d . . . H71 H -0.2107 0.5562 0.1736 0.053 Uiso 1 1 calc R . . C72 C -0.08916(19) 0.52383(13) 0.16393(7) 0.0355(7) Uani 1 1 d . . . H72 H -0.0886 0.5486 0.1463 0.043 Uiso 1 1 calc R . . C1S C -0.0632(4) 0.8121(2) 0.06396(11) 0.0774(13) Uani 1 1 d . . . H1S H -0.0777 0.8256 0.083 0.093 Uiso 1 1 calc R . . C2S C -0.1228(3) 0.77692(19) 0.04567(12) 0.0763(13) Uani 1 1 d . . . H2S H -0.1788 0.7652 0.052 0.092 Uiso 1 1 calc R . . C3S C -0.1039(3) 0.75776(19) 0.01807(11) 0.0747(12) Uani 1 1 d . . . H3S H -0.1466 0.7332 0.0051 0.09 Uiso 1 1 calc R . . C4S C -0.0227(4) 0.7744(2) 0.00922(11) 0.0837(14) Uani 1 1 d . . . H4S H -0.0087 0.7614 -0.0099 0.1 Uiso 1 1 calc R . . C5S C 0.0386(3) 0.8099(2) 0.02809(14) 0.0821(15) Uani 1 1 d . . . H5S H 0.0952 0.8214 0.0221 0.099 Uiso 1 1 calc R . . C6S C 0.0176(3) 0.82860(19) 0.05543(12) 0.0762(13) Uani 1 1 d . . . H6S H 0.0597 0.8532 0.0686 0.091 Uiso 1 1 calc R . . C7S C -0.4279(2) 0.51750(18) -0.03501(9) 0.0550(9) Uani 1 1 d . . . H7S H -0.4446 0.5539 -0.0249 0.066 Uiso 1 1 calc R . . C8S C -0.3946(2) 0.46593(18) -0.01867(8) 0.0522(9) Uani 1 1 d . . . H8S H -0.3878 0.4665 0.0028 0.063 Uiso 1 1 calc R . . C9S C -0.3711(2) 0.41334(17) -0.03363(8) 0.0500(9) Uani 1 1 d . . . H9S H -0.3484 0.3774 -0.0224 0.06 Uiso 1 1 calc R . . C10S C -0.3802(2) 0.41265(16) -0.06472(8) 0.0476(9) Uani 1 1 d . . . H10S H -0.3636 0.3763 -0.0749 0.057 Uiso 1 1 calc R . . C11S C -0.4132(2) 0.46413(17) -0.08113(8) 0.0479(9) Uani 1 1 d . . . H11S H -0.4195 0.4637 -0.1026 0.057 Uiso 1 1 calc R . . C12S C -0.4370(2) 0.51616(17) -0.06616(9) 0.0535(9) Uani 1 1 d . . . H12S H -0.4602 0.5519 -0.0774 0.064 Uiso 1 1 calc R . . C13S C 0.5 0.2331(2) 0.25 0.083(2) Uani 1 2 d S . . H13S H 0.5 0.2776 0.25 0.1 Uiso 1 2 calc SR . . C14S C 0.5813(3) 0.20096(17) 0.25223(9) 0.0654(11) Uani 1 1 d . . . H14S H 0.6372 0.2232 0.2536 0.078 Uiso 1 1 calc R . . C15S C 0.5811(2) 0.13754(16) 0.25248(8) 0.0521(9) Uani 1 1 d . . . H15S H 0.637 0.1151 0.2544 0.063 Uiso 1 1 calc R . . C16S C 0.5 0.1057(2) 0.25 0.0580(14) Uani 1 2 d S . . H16S H 0.5 0.0612 0.25 0.07 Uiso 1 2 calc SR . . 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 0.02103(9) 0.02523(9) 0.02672(9) -0.00175(7) 0.00238(7) 0.00110(7) Ce2 0.02048(9) 0.02603(9) 0.03033(10) 0.00322(7) 0.00242(7) -0.00214(7) N1 0.0261(13) 0.0268(13) 0.0377(15) -0.0002(11) 0.0050(11) 0.0026(10) N2 0.0338(14) 0.0256(13) 0.0310(14) -0.0011(10) 0.0002(11) -0.0030(11) N3 0.0237(13) 0.0298(13) 0.0365(14) 0.0069(11) 0.0080(11) 0.0010(10) N4 0.0259(13) 0.0303(13) 0.0257(13) 0.0008(10) 0.0024(10) -0.0042(10) N5 0.0264(13) 0.0265(13) 0.0260(13) -0.0046(10) 0.0059(10) -0.0018(10) N6 0.0225(12) 0.0239(12) 0.0296(13) -0.0035(10) 0.0071(10) -0.0010(10) C1 0.0257(16) 0.0320(17) 0.0307(17) 0.0073(13) 0.0026(13) 0.0035(13) C2 0.0313(17) 0.0355(17) 0.048(2) 0.0080(15) 0.0107(15) 0.0062(14) C3 0.0241(17) 0.054(2) 0.069(2) 0.0152(19) 0.0083(16) 0.0017(16) C4 0.0324(19) 0.050(2) 0.066(2) 0.0142(18) -0.0026(17) -0.0136(16) C5 0.047(2) 0.0313(17) 0.042(2) 0.0049(14) -0.0032(16) -0.0049(15) C6 0.0295(16) 0.0365(18) 0.0320(17) 0.0038(13) 0.0059(13) -0.0009(13) C7 0.0245(15) 0.0314(17) 0.0379(18) 0.0028(13) 0.0128(14) 0.0048(13) C8 0.0332(18) 0.039(2) 0.060(2) 0.0092(16) 0.0077(16) 0.0042(15) C9 0.043(2) 0.042(2) 0.076(3) 0.0181(19) 0.0167(19) 0.0138(17) C10 0.055(2) 0.0247(18) 0.087(3) 0.0014(18) 0.033(2) 0.0091(17) C11 0.046(2) 0.037(2) 0.069(3) -0.0175(17) 0.0209(19) -0.0006(16) C12 0.0332(17) 0.0337(18) 0.047(2) -0.0058(15) 0.0106(15) 0.0065(14) C13 0.0274(15) 0.0334(17) 0.0247(16) 0.0007(13) 0.0072(13) -0.0004(13) C14 0.0372(18) 0.0367(17) 0.0355(18) 0.0024(14) 0.0011(15) 0.0049(14) C15 0.0287(17) 0.057(2) 0.0381(19) -0.0025(16) -0.0049(14) 0.0045(15) C16 0.0307(17) 0.048(2) 0.0403(19) -0.0090(15) 0.0074(15) -0.0106(15) C17 0.0366(17) 0.0328(17) 0.0328(17) -0.0055(13) 0.0102(14) -0.0044(14) C18 0.0268(15) 0.0325(17) 0.0223(15) -0.0005(12) 0.0028(12) 0.0022(12) C19 0.0329(16) 0.0269(16) 0.0371(18) 0.0025(14) -0.0013(14) 0.0001(13) C20 0.053(2) 0.039(2) 0.056(2) -0.0042(17) 0.0029(18) 0.0107(16) C21 0.080(3) 0.030(2) 0.096(4) -0.009(2) -0.017(3) 0.0053(19) C22 0.087(3) 0.033(2) 0.109(4) 0.028(3) -0.018(3) -0.013(2) C23 0.139(4) 0.056(3) 0.082(3) 0.026(3) 0.032(3) -0.020(3) C24 0.103(3) 0.039(2) 0.052(2) 0.0052(17) 0.023(2) -0.009(2) C25 0.0270(15) 0.0316(16) 0.0255(16) 0.0075(12) 0.0021(13) 0.0016(13) C26 0.0350(18) 0.0401(19) 0.0369(18) -0.0002(14) 0.0063(14) -0.0014(14) C27 0.043(2) 0.0384(19) 0.057(2) 0.0077(16) -0.0036(18) -0.0126(16) C28 0.0315(18) 0.060(2) 0.060(2) 0.0242(19) 0.0053(17) -0.0082(17) C29 0.0399(19) 0.059(2) 0.045(2) 0.0146(17) 0.0197(16) 0.0067(17) C30 0.0404(18) 0.0343(17) 0.0308(17) 0.0056(13) 0.0087(14) 0.0009(14) C31 0.0301(16) 0.0273(16) 0.0344(17) -0.0017(13) 0.0071(13) 0.0010(13) C32 0.0339(17) 0.0398(18) 0.0337(18) 0.0041(14) 0.0057(14) 0.0010(14) C33 0.040(2) 0.061(2) 0.047(2) 0.0143(17) -0.0005(17) 0.0116(17) C34 0.0269(18) 0.077(3) 0.058(2) -0.001(2) 0.0019(17) 0.0075(18) C35 0.0291(18) 0.063(2) 0.064(2) 0.003(2) 0.0174(17) -0.0008(17) C36 0.0372(19) 0.0402(19) 0.051(2) 0.0071(15) 0.0152(16) 0.0020(15) C37 0.0212(14) 0.0261(15) 0.0336(17) 0.0027(13) 0.0044(13) 0.0015(12) C38 0.0344(17) 0.0391(18) 0.0374(19) -0.0026(14) 0.0080(15) -0.0094(14) C39 0.0391(18) 0.0384(19) 0.056(2) -0.0038(16) 0.0147(17) -0.0147(15) C40 0.0433(19) 0.0422(19) 0.046(2) 0.0089(16) 0.0217(16) -0.0032(16) C41 0.0410(19) 0.058(2) 0.0323(19) 0.0016(16) 0.0101(15) -0.0045(17) C42 0.0270(16) 0.0470(19) 0.0356(19) -0.0027(15) 0.0057(14) -0.0104(14) C43 0.0200(14) 0.0344(17) 0.0333(18) -0.0010(13) 0.0024(13) -0.0064(12) C44 0.0339(17) 0.0362(18) 0.0362(18) -0.0028(14) 0.0047(14) -0.0054(14) C45 0.044(2) 0.043(2) 0.047(2) -0.0117(17) 0.0078(16) -0.0092(16) C46 0.042(2) 0.065(2) 0.035(2) -0.0141(17) 0.0034(16) -0.0119(17) C47 0.0354(18) 0.061(2) 0.0306(19) 0.0069(16) -0.0038(14) -0.0095(16) C48 0.0306(16) 0.0365(17) 0.0342(18) 0.0025(14) -0.0002(14) -0.0058(13) C49 0.0288(16) 0.0292(16) 0.0290(17) -0.0059(12) 0.0047(13) 0.0013(12) C50 0.0319(17) 0.0392(18) 0.0359(19) -0.0074(14) 0.0080(14) -0.0007(14) C51 0.042(2) 0.058(2) 0.043(2) -0.0053(16) 0.0218(17) -0.0053(16) C52 0.065(3) 0.068(2) 0.031(2) -0.0070(17) 0.0196(18) -0.006(2) C53 0.052(2) 0.058(2) 0.032(2) -0.0089(16) 0.0064(16) -0.0046(18) C54 0.0317(17) 0.0404(18) 0.0350(19) -0.0075(14) 0.0078(14) -0.0040(14) C55 0.0206(14) 0.0256(16) 0.0349(17) -0.0032(12) -0.0001(13) 0.0004(12) C56 0.0317(17) 0.0364(18) 0.0436(19) -0.0060(15) 0.0042(14) 0.0009(14) C57 0.0416(19) 0.0268(18) 0.072(3) -0.0074(17) 0.0011(18) -0.0015(15) C58 0.044(2) 0.033(2) 0.073(3) 0.0134(18) 0.0021(19) -0.0059(15) C59 0.0400(19) 0.039(2) 0.048(2) 0.0144(16) 0.0081(16) -0.0036(15) C60 0.0277(16) 0.0314(17) 0.0351(18) 0.0012(13) 0.0015(14) 0.0007(13) C61 0.0220(14) 0.0249(15) 0.0256(15) 0.0059(12) 0.0030(12) 0.0030(12) C62 0.0320(16) 0.0270(16) 0.0332(17) 0.0000(13) 0.0068(13) -0.0005(13) C63 0.0423(19) 0.0278(17) 0.048(2) -0.0008(14) 0.0009(16) -0.0042(14) C64 0.0340(18) 0.0321(18) 0.069(2) 0.0106(17) 0.0065(17) -0.0061(14) C65 0.0290(17) 0.045(2) 0.050(2) 0.0192(16) 0.0141(15) 0.0058(15) C66 0.0250(15) 0.0340(16) 0.0320(17) 0.0035(13) 0.0071(13) 0.0064(13) C67 0.0228(15) 0.0253(15) 0.0310(17) -0.0064(12) 0.0078(13) -0.0051(12) C68 0.0259(16) 0.0355(17) 0.0318(17) -0.0021(13) 0.0028(13) -0.0071(13) C69 0.0389(19) 0.0469(19) 0.0279(17) -0.0041(14) 0.0069(15) -0.0162(15) C70 0.0356(19) 0.059(2) 0.046(2) -0.0112(17) 0.0222(16) -0.0078(17) C71 0.0313(18) 0.048(2) 0.057(2) -0.0021(17) 0.0180(16) 0.0083(15) C72 0.0342(17) 0.0338(17) 0.0405(19) 0.0014(14) 0.0123(15) 0.0023(14) C1S 0.104(4) 0.056(3) 0.079(3) 0.002(2) 0.036(3) 0.005(3) C2S 0.077(3) 0.053(3) 0.106(4) 0.006(3) 0.039(3) 0.004(2) C3S 0.079(3) 0.055(3) 0.085(3) 0.007(2) -0.007(3) 0.012(2) C4S 0.116(4) 0.075(3) 0.067(3) 0.017(3) 0.034(3) 0.030(3) C5S 0.068(3) 0.062(3) 0.125(5) 0.031(3) 0.045(3) 0.016(2) C6S 0.072(3) 0.054(3) 0.099(4) 0.010(2) 0.000(3) 0.010(2) C7S 0.049(2) 0.055(2) 0.063(3) -0.006(2) 0.0160(19) 0.0017(18) C8S 0.045(2) 0.070(3) 0.042(2) 0.0018(19) 0.0110(17) -0.0069(19) C9S 0.040(2) 0.052(2) 0.057(3) 0.0112(18) 0.0047(17) -0.0004(16) C10S 0.0332(18) 0.053(2) 0.056(2) -0.0033(18) 0.0064(17) 0.0029(16) C11S 0.0318(18) 0.065(2) 0.046(2) 0.0038(18) 0.0059(16) -0.0009(17) C12S 0.047(2) 0.052(2) 0.062(3) 0.0112(19) 0.0087(19) 0.0055(18) C13S 0.088(5) 0.029(3) 0.118(5) 0 -0.036(4) 0 C14S 0.069(3) 0.046(2) 0.073(3) 0.0049(19) -0.018(2) -0.013(2) C15S 0.056(2) 0.047(2) 0.053(2) -0.0032(17) 0.0083(18) 0.0023(18) C16S 0.069(4) 0.032(3) 0.076(4) 0 0.020(3) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 N2 2.354(2) . ? Ce1 N1 2.359(2) . ? Ce1 N5 2.516(2) . ? Ce1 N6 2.583(2) . ? Ce2 N3 2.329(2) . ? Ce2 N4 2.369(2) . ? Ce2 N5 2.557(2) . ? Ce2 N6 2.557(2) . ? N1 C7 1.403(3) . ? N1 C1 1.410(3) . ? N2 C13 1.395(3) . ? N2 C19 1.415(3) . ? N3 C31 1.402(3) . ? N3 C25 1.418(3) . ? N4 C37 1.404(3) . ? N4 C43 1.404(3) . ? N5 C55 1.420(3) . ? N5 C49 1.423(3) . ? N6 C61 1.417(3) . ? N6 C67 1.430(3) . ? C1 C6 1.391(4) . ? C1 C2 1.400(4) . ? C2 C3 1.378(4) . ? C3 C4 1.378(5) . ? C4 C5 1.381(5) . ? C5 C6 1.381(4) . ? C7 C12 1.397(4) . ? C7 C8 1.409(4) . ? C8 C9 1.374(4) . ? C9 C10 1.388(5) . ? C10 C11 1.362(5) . ? C11 C12 1.395(4) . ? C13 C18 1.403(4) . ? C13 C14 1.410(4) . ? C14 C15 1.373(4) . ? C15 C16 1.386(4) . ? C16 C17 1.368(4) . ? C17 C18 1.392(4) . ? C19 C24 1.374(4) . ? C19 C20 1.381(4) . ? C20 C21 1.382(5) . ? C21 C22 1.360(6) . ? C22 C23 1.363(6) . ? C23 C24 1.381(5) . ? C25 C30 1.393(4) . ? C25 C26 1.397(4) . ? C26 C27 1.377(4) . ? C27 C28 1.377(5) . ? C28 C29 1.360(5) . ? C29 C30 1.396(4) . ? C31 C32 1.394(4) . ? C31 C36 1.404(4) . ? C32 C33 1.382(4) . ? C33 C34 1.379(5) . ? C34 C35 1.376(5) . ? C35 C36 1.379(4) . ? C37 C42 1.384(4) . ? C37 C38 1.394(4) . ? C38 C39 1.380(4) . ? C39 C40 1.373(4) . ? C40 C41 1.377(4) . ? C41 C42 1.376(4) . ? C43 C48 1.398(4) . ? C43 C44 1.409(4) . ? C44 C45 1.375(4) . ? C45 C46 1.384(5) . ? C46 C47 1.377(5) . ? C47 C48 1.391(4) . ? C49 C54 1.392(4) . ? C49 C50 1.403(4) . ? C50 C51 1.385(4) . ? C51 C52 1.379(5) . ? C52 C53 1.375(5) . ? C53 C54 1.391(4) . ? C55 C60 1.395(4) . ? C55 C56 1.404(4) . ? C56 C57 1.378(4) . ? C57 C58 1.380(5) . ? C58 C59 1.370(5) . ? C59 C60 1.397(4) . ? C61 C66 1.396(4) . ? C61 C62 1.403(4) . ? C62 C63 1.378(4) . ? C63 C64 1.387(4) . ? C64 C65 1.373(5) . ? C65 C66 1.394(4) . ? C67 C68 1.393(4) . ? C67 C72 1.405(4) . ? C68 C69 1.383(4) . ? C69 C70 1.379(4) . ? C70 C71 1.374(4) . ? C71 C72 1.387(4) . ? C1S C2S 1.342(6) . ? C1S C6S 1.358(6) . ? C2S C3S 1.366(6) . ? C3S C4S 1.369(6) . ? C4S C5S 1.373(7) . ? C5S C6S 1.362(6) . ? C7S C8S 1.372(5) . ? C7S C12S 1.377(5) . ? C8S C9S 1.378(5) . ? C9S C10S 1.374(5) . ? C10S C11S 1.371(5) . ? C11S C12S 1.369(5) . ? C13S C14S 1.380(5) . ? C13S C14S 1.380(5) 2_655 ? C14S C15S 1.355(5) . ? C15S C16S 1.372(4) . ? C16S C15S 1.372(4) 2_655 ? 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 N2 Ce1 N1 106.08(8) . . ? N2 Ce1 N5 129.05(7) . . ? N1 Ce1 N5 108.49(7) . . ? N2 Ce1 N6 101.16(7) . . ? N1 Ce1 N6 138.67(7) . . ? N5 Ce1 N6 75.43(7) . . ? N3 Ce2 N4 108.69(8) . . ? N3 Ce2 N5 132.91(7) . . ? N4 Ce2 N5 111.08(7) . . ? N3 Ce2 N6 101.74(7) . . ? N4 Ce2 N6 124.57(7) . . ? N5 Ce2 N6 75.20(7) . . ? C7 N1 C1 119.3(2) . . ? C7 N1 Ce1 98.52(16) . . ? C1 N1 Ce1 138.12(18) . . ? C13 N2 C19 119.0(2) . . ? C13 N2 Ce1 100.48(16) . . ? C19 N2 Ce1 134.71(18) . . ? C31 N3 C25 117.2(2) . . ? C31 N3 Ce2 128.91(17) . . ? C25 N3 Ce2 113.85(16) . . ? C37 N4 C43 119.5(2) . . ? C37 N4 Ce2 138.12(17) . . ? C43 N4 Ce2 97.61(15) . . ? C55 N5 C49 119.5(2) . . ? C55 N5 Ce1 97.44(15) . . ? C49 N5 Ce1 130.23(16) . . ? C55 N5 Ce2 99.97(15) . . ? C49 N5 Ce2 99.98(15) . . ? Ce1 N5 Ce2 105.41(8) . . ? C61 N6 C67 115.7(2) . . ? C61 N6 Ce2 119.14(16) . . ? C67 N6 Ce2 94.92(15) . . ? C61 N6 Ce1 93.62(14) . . ? C67 N6 Ce1 131.57(17) . . ? Ce2 N6 Ce1 103.45(7) . . ? C6 C1 C2 117.6(3) . . ? C6 C1 N1 119.4(2) . . ? C2 C1 N1 122.9(3) . . ? C3 C2 C1 120.9(3) . . ? C4 C3 C2 120.8(3) . . ? C3 C4 C5 118.9(3) . . ? C6 C5 C4 120.7(3) . . ? C5 C6 C1 121.0(3) . . ? C12 C7 N1 119.1(3) . . ? C12 C7 C8 117.1(3) . . ? N1 C7 C8 123.5(3) . . ? C12 C7 Ce1 84.02(16) . . ? N1 C7 Ce1 53.09(13) . . ? C8 C7 Ce1 130.3(2) . . ? C9 C8 C7 120.8(3) . . ? C8 C9 C10 120.8(3) . . ? C11 C10 C9 119.8(3) . . ? C10 C11 C12 120.0(3) . . ? C11 C12 C7 121.5(3) . . ? N2 C13 C18 118.3(2) . . ? N2 C13 C14 125.0(3) . . ? C18 C13 C14 116.4(3) . . ? N2 C13 Ce1 51.78(13) . . ? C18 C13 Ce1 79.12(15) . . ? C14 C13 Ce1 138.17(19) . . ? C15 C14 C13 121.1(3) . . ? C14 C15 C16 121.4(3) . . ? C17 C16 C15 118.9(3) . . ? C16 C17 C18 120.4(3) . . ? C17 C18 C13 121.7(3) . . ? C24 C19 C20 117.4(3) . . ? C24 C19 N2 122.1(3) . . ? C20 C19 N2 120.3(3) . . ? C19 C20 C21 120.8(4) . . ? C22 C21 C20 121.0(4) . . ? C21 C22 C23 118.8(4) . . ? C22 C23 C24 120.6(4) . . ? C19 C24 C23 121.3(4) . . ? C30 C25 C26 117.7(3) . . ? C30 C25 N3 119.9(3) . . ? C26 C25 N3 122.3(3) . . ? C27 C26 C25 120.7(3) . . ? C28 C27 C26 120.7(3) . . ? C29 C28 C27 119.8(3) . . ? C28 C29 C30 120.3(3) . . ? C25 C30 C29 120.7(3) . . ? C32 C31 N3 123.6(3) . . ? C32 C31 C36 116.9(3) . . ? N3 C31 C36 119.4(3) . . ? C33 C32 C31 121.1(3) . . ? C34 C33 C32 121.0(3) . . ? C35 C34 C33 118.8(3) . . ? C34 C35 C36 120.6(3) . . ? C35 C36 C31 121.4(3) . . ? C42 C37 C38 116.7(3) . . ? C42 C37 N4 118.4(2) . . ? C38 C37 N4 124.8(3) . . ? C39 C38 C37 121.2(3) . . ? C40 C39 C38 121.2(3) . . ? C39 C40 C41 118.2(3) . . ? C42 C41 C40 120.8(3) . . ? C41 C42 C37 121.9(3) . . ? C48 C43 N4 118.0(3) . . ? C48 C43 C44 117.8(3) . . ? N4 C43 C44 123.7(3) . . ? C48 C43 Ce2 84.94(16) . . ? N4 C43 Ce2 53.81(12) . . ? C44 C43 Ce2 125.97(19) . . ? C45 C44 C43 120.2(3) . . ? C44 C45 C46 121.6(3) . . ? C47 C46 C45 118.9(3) . . ? C46 C47 C48 120.5(3) . . ? C47 C48 C43 120.9(3) . . ? C54 C49 C50 118.3(3) . . ? C54 C49 N5 121.6(2) . . ? C50 C49 N5 119.7(2) . . ? C51 C50 C49 120.2(3) . . ? C52 C51 C50 120.8(3) . . ? C53 C52 C51 119.7(3) . . ? C52 C53 C54 120.2(3) . . ? C53 C54 C49 120.8(3) . . ? C60 C55 C56 117.8(3) . . ? C60 C55 N5 117.6(2) . . ? C56 C55 N5 124.5(3) . . ? C57 C56 C55 119.9(3) . . ? C56 C57 C58 121.5(3) . . ? C59 C58 C57 119.7(3) . . ? C58 C59 C60 119.5(3) . . ? C55 C60 C59 121.5(3) . . ? C66 C61 C62 117.9(3) . . ? C66 C61 N6 118.1(2) . . ? C62 C61 N6 123.8(2) . . ? C63 C62 C61 120.6(3) . . ? C62 C63 C64 121.0(3) . . ? C65 C64 C63 119.1(3) . . ? C64 C65 C66 120.7(3) . . ? C65 C66 C61 120.7(3) . . ? C68 C67 C72 118.5(3) . . ? C68 C67 N6 122.4(2) . . ? C72 C67 N6 119.0(2) . . ? C69 C68 C67 120.3(3) . . ? C70 C69 C68 120.6(3) . . ? C71 C70 C69 120.1(3) . . ? C70 C71 C72 120.0(3) . . ? C71 C72 C67 120.5(3) . . ? C2S C1S C6S 120.3(5) . . ? C1S C2S C3S 120.8(4) . . ? C2S C3S C4S 119.3(5) . . ? C3S C4S C5S 119.9(5) . . ? C6S C5S C4S 119.6(4) . . ? C1S C6S C5S 120.2(5) . . ? C8S C7S C12S 119.6(4) . . ? C7S C8S C9S 119.6(3) . . ? C10S C9S C8S 120.2(3) . . ? C11S C10S C9S 120.3(3) . . ? C12S C11S C10S 119.2(3) . . ? C11S C12S C7S 121.0(3) . . ? C14S C13S C14S 120.3(5) . 2_655 ? C15S C14S C13S 119.7(4) . . ? C14S C15S C16S 119.8(4) . . ? C15S C16S C15S 120.6(5) . 2_655 ? #===END