# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name M.Lappert P.B.Hitchcock 'Andrey Protchenko' _publ_contact_author_name 'Michael 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_journal 'Chemical Communications' _publ_section_title ; Facile formation of a homoleptic Ce(IV) amide via aerobic oxidation ; _publ_requested_category FM data_(1)-sep2804 _database_code_depnum_ccdc_archive 'CCDC 609099' _audit_creation_date 2004-09-22T17:02:06-00:00 _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 'C40 H74 Ce N3 O, C7 H8' _chemical_formula_sum 'C47 H82 Ce N3 O' _chemical_formula_weight 845.28 _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 10.3004(2) _cell_length_b 23.4770(4) _cell_length_c 19.3077(3) _cell_angle_alpha 90 _cell_angle_beta 101.189(1) _cell_angle_gamma 90 _cell_volume 4580.29(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25568 _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 yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.029 _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 0.7678 _exptl_absorpt_correction_T_max 0.8216 #----------------------------------------------------------------------------# # 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 0.945024E-1 _diffrn_orient_matrix_ub_12 0.16173E-2 _diffrn_orient_matrix_ub_13 0.250334E-1 _diffrn_orient_matrix_ub_21 0.292703E-1 _diffrn_orient_matrix_ub_22 -0.15057E-2 _diffrn_orient_matrix_ub_23 -0.464117E-1 _diffrn_orient_matrix_ub_31 -0.25569E-2 _diffrn_orient_matrix_ub_32 0.425375E-1 _diffrn_orient_matrix_ub_33 -0.25946E-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 0.0596 _diffrn_reflns_av_unetI/netI 0.0427 _diffrn_reflns_number 39309 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 8044 _reflns_number_gt 6438 _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^+3.2837P] 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 8044 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0689 _refine_ls_wR_factor_gt 0.063 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.507 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # 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 Ce Ce 0.505584(15) 0.633675(7) 0.735058(8) 0.02703(6) Uani 1 1 d . . . O O 0.6734(2) 0.71190(9) 0.78599(11) 0.0434(5) Uani 1 1 d . . . N1 N 0.5532(2) 0.55533(9) 0.67134(11) 0.0262(5) Uani 1 1 d . . . N2 N 0.4624(2) 0.60401(10) 0.84385(11) 0.0292(5) Uani 1 1 d . . . N3 N 0.3698(2) 0.69410(9) 0.65988(12) 0.0304(5) Uani 1 1 d . . . C1 C 0.4727(3) 0.50370(11) 0.66132(14) 0.0271(6) Uani 1 1 d . . . H1 H 0.5239 0.4725 0.6896 0.033 Uiso 1 1 calc R . . C2 C 0.3480(3) 0.51425(12) 0.69087(15) 0.0304(7) Uani 1 1 d . . . H2A H 0.2994 0.5469 0.6657 0.037 Uiso 1 1 calc R . . H2B H 0.3737 0.5247 0.7414 0.037 Uiso 1 1 calc R . . C3 C 0.2556(3) 0.46263(12) 0.68402(16) 0.0348(7) Uani 1 1 d . . . H3A H 0.2998 0.4312 0.7138 0.042 Uiso 1 1 calc R . . H3B H 0.1742 0.4728 0.7012 0.042 Uiso 1 1 calc R . . C4 C 0.2190(3) 0.44268(13) 0.60763(16) 0.0401(8) Uani 1 1 d . . . H4A H 0.1644 0.4077 0.605 0.048 Uiso 1 1 calc R . . H4B H 0.1661 0.4725 0.5787 0.048 Uiso 1 1 calc R . . C5 C 0.3435(3) 0.43052(13) 0.57875(16) 0.0387(7) Uani 1 1 d . . . H5A H 0.3186 0.4191 0.5286 0.046 Uiso 1 1 calc R . . H5B H 0.3924 0.3985 0.6053 0.046 Uiso 1 1 calc R . . C6 C 0.4337(3) 0.48322(12) 0.58489(15) 0.0337(7) Uani 1 1 d . . . H6A H 0.5146 0.4738 0.5667 0.04 Uiso 1 1 calc R . . H6B H 0.3871 0.5143 0.5554 0.04 Uiso 1 1 calc R . . C7 C 0.6723(3) 0.55354(11) 0.64023(15) 0.0288(6) Uani 1 1 d . . . H7 H 0.6436 0.5513 0.5878 0.035 Uiso 1 1 calc R . . C8 C 0.7493(3) 0.60921(12) 0.65811(16) 0.0334(7) Uani 1 1 d . . . H8A H 0.774 0.6131 0.7101 0.04 Uiso 1 1 calc R . . H8B H 0.6913 0.6417 0.64 0.04 Uiso 1 1 calc R . . C9 C 0.8749(3) 0.61187(14) 0.62665(19) 0.0458(8) Uani 1 1 d . . . H9A H 0.8499 0.6135 0.5745 0.055 Uiso 1 1 calc R . . H9B H 0.9246 0.647 0.643 0.055 Uiso 1 1 calc R . . C10 C 0.9629(3) 0.56031(14) 0.6481(2) 0.0528(9) Uani 1 1 d . . . H10A H 0.9984 0.5617 0.6995 0.063 Uiso 1 1 calc R . . H10B H 1.0387 0.5614 0.6235 0.063 Uiso 1 1 calc R . . C11 C 0.8864(3) 0.50496(13) 0.6299(2) 0.0471(9) Uani 1 1 d . . . H11A H 0.9445 0.4722 0.6466 0.057 Uiso 1 1 calc R . . H11B H 0.8584 0.5018 0.578 0.057 Uiso 1 1 calc R . . C12 C 0.7649(3) 0.50335(12) 0.66413(17) 0.0361(7) Uani 1 1 d . . . H12A H 0.7936 0.5045 0.7161 0.043 Uiso 1 1 calc R . . H12B H 0.7165 0.4672 0.6515 0.043 Uiso 1 1 calc R . . C13 C 0.5640(3) 0.56976(12) 0.89005(15) 0.0339(7) Uani 1 1 d . . . H13 H 0.5675 0.5822 0.9399 0.041 Uiso 1 1 calc R . . C14 C 0.6995(3) 0.57901(14) 0.87239(19) 0.0466(8) Uani 1 1 d . . . H14A H 0.7214 0.6201 0.8765 0.056 Uiso 1 1 calc R . . H14B H 0.6971 0.5675 0.8228 0.056 Uiso 1 1 calc R . . C15 C 0.8086(3) 0.54524(15) 0.9208(2) 0.0538(9) Uani 1 1 d . . . H15A H 0.8943 0.5519 0.9062 0.065 Uiso 1 1 calc R . . H15B H 0.8167 0.5588 0.97 0.065 Uiso 1 1 calc R . . C16 C 0.7780(3) 0.48260(15) 0.9176(2) 0.0560(10) Uani 1 1 d . . . H16A H 0.846 0.4621 0.9518 0.067 Uiso 1 1 calc R . . H16B H 0.7809 0.468 0.8698 0.067 Uiso 1 1 calc R . . C17 C 0.6425(3) 0.47115(16) 0.9343(2) 0.0633(11) Uani 1 1 d . . . H17A H 0.6429 0.4814 0.9841 0.076 Uiso 1 1 calc R . . H17B H 0.6219 0.43 0.9283 0.076 Uiso 1 1 calc R . . C18 C 0.5361(3) 0.50568(13) 0.8857(2) 0.0522(9) Uani 1 1 d . . . H18A H 0.4493 0.4983 0.8987 0.063 Uiso 1 1 calc R . . H18B H 0.5309 0.4928 0.8364 0.063 Uiso 1 1 calc R . . C19 C 0.3393(3) 0.60833(12) 0.87041(14) 0.0301(7) Uani 1 1 d . . . H19 H 0.3192 0.57 0.8883 0.036 Uiso 1 1 calc R . . C20 C 0.3441(3) 0.65107(14) 0.93020(17) 0.0447(8) Uani 1 1 d . . . H20A H 0.368 0.689 0.9141 0.054 Uiso 1 1 calc R . . H20B H 0.414 0.6395 0.9705 0.054 Uiso 1 1 calc R . . C21 C 0.2120(3) 0.65558(16) 0.95508(17) 0.0528(9) Uani 1 1 d . . . H21A H 0.1921 0.6187 0.9756 0.063 Uiso 1 1 calc R . . H21B H 0.2192 0.6849 0.9924 0.063 Uiso 1 1 calc R . . C22 C 0.1000(3) 0.67105(14) 0.89482(18) 0.0481(9) Uani 1 1 d . . . H22A H 0.1139 0.7101 0.8782 0.058 Uiso 1 1 calc R . . H22B H 0.0152 0.6705 0.9117 0.058 Uiso 1 1 calc R . . C23 C 0.0931(3) 0.62946(16) 0.83413(18) 0.0517(9) Uani 1 1 d . . . H23A H 0.0247 0.6423 0.7938 0.062 Uiso 1 1 calc R . . H23B H 0.067 0.5915 0.849 0.062 Uiso 1 1 calc R . . C24 C 0.2261(3) 0.62480(15) 0.81068(17) 0.0477(9) Uani 1 1 d . . . H24A H 0.2188 0.596 0.7727 0.057 Uiso 1 1 calc R . . H24B H 0.2469 0.6618 0.7909 0.057 Uiso 1 1 calc R . . C25 C 0.3359(3) 0.74373(12) 0.69906(15) 0.0340(7) Uani 1 1 d . . . H25 H 0.3699 0.7347 0.75 0.041 Uiso 1 1 calc R . . C26 C 0.1875(3) 0.75561(13) 0.69306(16) 0.0405(8) Uani 1 1 d . . . H26A H 0.1481 0.7646 0.6433 0.049 Uiso 1 1 calc R . . H26B H 0.1438 0.7208 0.7063 0.049 Uiso 1 1 calc R . . C27 C 0.1609(4) 0.80466(15) 0.73989(19) 0.0607(10) Uani 1 1 d . . . H27A H 0.0645 0.812 0.7319 0.073 Uiso 1 1 calc R . . H27B H 0.1906 0.7938 0.79 0.073 Uiso 1 1 calc R . . C28 C 0.2316(4) 0.85858(14) 0.7251(2) 0.0654(12) Uani 1 1 d . . . H28A H 0.2171 0.8886 0.7588 0.079 Uiso 1 1 calc R . . H28B H 0.1943 0.8721 0.6768 0.079 Uiso 1 1 calc R . . C29 C 0.3788(4) 0.84817(14) 0.7320(2) 0.0621(11) Uani 1 1 d . . . H29A H 0.4181 0.8393 0.7818 0.074 Uiso 1 1 calc R . . H29B H 0.4216 0.8832 0.7186 0.074 Uiso 1 1 calc R . . C30 C 0.4056(3) 0.79890(12) 0.68497(17) 0.0435(8) Uani 1 1 d . . . H30A H 0.5022 0.792 0.6928 0.052 Uiso 1 1 calc R . . H30B H 0.3757 0.8099 0.6349 0.052 Uiso 1 1 calc R . . C31 C 0.3152(3) 0.69473(12) 0.58357(14) 0.0296(7) Uani 1 1 d . . . H31 H 0.2921 0.735 0.5693 0.036 Uiso 1 1 calc R . . C32 C 0.1899(3) 0.65859(14) 0.56340(16) 0.0418(8) Uani 1 1 d . . . H32A H 0.121 0.6737 0.5877 0.05 Uiso 1 1 calc R . . H32B H 0.2097 0.619 0.5799 0.05 Uiso 1 1 calc R . . C33 C 0.1363(4) 0.65798(16) 0.48367(17) 0.0551(10) Uani 1 1 d . . . H33A H 0.0576 0.6329 0.4731 0.066 Uiso 1 1 calc R . . H33B H 0.1087 0.6969 0.4675 0.066 Uiso 1 1 calc R . . C34 C 0.2401(4) 0.63688(15) 0.44434(17) 0.0578(10) Uani 1 1 d . . . H34A H 0.2051 0.6387 0.3929 0.069 Uiso 1 1 calc R . . H34B H 0.2616 0.5966 0.457 0.069 Uiso 1 1 calc R . . C35 C 0.3646(4) 0.67281(15) 0.46257(17) 0.0529(9) Uani 1 1 d . . . H35A H 0.3447 0.7122 0.4453 0.063 Uiso 1 1 calc R . . H35B H 0.4331 0.6571 0.4384 0.063 Uiso 1 1 calc R . . C36 C 0.4182(3) 0.67406(14) 0.54245(15) 0.0403(8) Uani 1 1 d . . . H36A H 0.4474 0.6353 0.5586 0.048 Uiso 1 1 calc R . . H36B H 0.4963 0.6995 0.5524 0.048 Uiso 1 1 calc R . . C37 C 0.7755(3) 0.74077(14) 0.7578(2) 0.0539(9) Uani 1 1 d . . . H37A H 0.7443 0.7501 0.7073 0.065 Uiso 1 1 calc R . . H37B H 0.8558 0.7168 0.7625 0.065 Uiso 1 1 calc R . . C38 C 0.8041(4) 0.79452(16) 0.8015(2) 0.0777(13) Uani 1 1 d . . . H38A H 0.8985 0.8053 0.8075 0.093 Uiso 1 1 calc R . . H38B H 0.7488 0.8266 0.7792 0.093 Uiso 1 1 calc R . . C39 C 0.7692(4) 0.77881(17) 0.8712(2) 0.0694(12) Uani 1 1 d . . . H39A H 0.8439 0.7593 0.9021 0.083 Uiso 1 1 calc R . . H39B H 0.7444 0.8129 0.8958 0.083 Uiso 1 1 calc R . . C40 C 0.6565(4) 0.74048(15) 0.85118(19) 0.0585(10) Uani 1 1 d . . . H40A H 0.5726 0.7622 0.8432 0.07 Uiso 1 1 calc R . . H40B H 0.6545 0.7122 0.889 0.07 Uiso 1 1 calc R . . C1S C 0.1696(4) 0.3826(2) 0.8945(2) 0.0710(12) Uani 1 1 d . . . C2S C 0.2957(4) 0.3646(2) 0.8984(2) 0.0781(13) Uani 1 1 d . . . H2S H 0.3579 0.3883 0.8817 0.094 Uiso 1 1 calc R . . C3S C 0.3345(5) 0.3109(2) 0.9270(3) 0.0846(14) Uani 1 1 d . . . H3S H 0.4231 0.2985 0.9294 0.101 Uiso 1 1 calc R . . C4S C 0.2471(5) 0.2762(2) 0.9514(2) 0.0799(13) Uani 1 1 d . . . H4S H 0.2739 0.2397 0.9701 0.096 Uiso 1 1 calc R . . C5S C 0.1216(5) 0.2947(2) 0.9484(2) 0.0840(14) Uani 1 1 d . . . H5S H 0.0597 0.2709 0.9652 0.101 Uiso 1 1 calc R . . C6S C 0.0825(4) 0.3479(2) 0.9212(2) 0.0771(13) Uani 1 1 d . . . H6S H -0.0051 0.3607 0.9209 0.093 Uiso 1 1 calc R . . C7S C 0.1255(5) 0.4404(2) 0.8636(3) 0.0923(15) Uani 1 1 d . . . H7S1 H 0.0319 0.4462 0.8652 0.139 Uiso 0.5 1 calc PR . . H7S2 H 0.1373 0.4421 0.8144 0.139 Uiso 0.5 1 calc PR . . H7S3 H 0.1787 0.4702 0.8911 0.139 Uiso 0.5 1 calc PR . . H7S4 H 0.2001 0.4595 0.8486 0.139 Uiso 0.5 1 calc PR . . H7S5 H 0.0947 0.4636 0.8994 0.139 Uiso 0.5 1 calc PR . . H7S6 H 0.0532 0.4355 0.8227 0.139 Uiso 0.5 1 calc PR . . 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 0.02904(9) 0.02574(9) 0.02584(9) -0.00038(7) 0.00418(6) 0.00118(8) O 0.0451(13) 0.0385(12) 0.0446(13) -0.0053(11) 0.0037(10) -0.0101(10) N1 0.0231(12) 0.0266(12) 0.0293(13) -0.0010(10) 0.0061(10) -0.0002(10) N2 0.0282(13) 0.0300(13) 0.0286(13) 0.0038(11) 0.0035(10) 0.0026(10) N3 0.0342(14) 0.0287(13) 0.0268(13) -0.0021(11) 0.0023(11) 0.0024(10) C1 0.0257(15) 0.0268(15) 0.0280(15) 0.0016(13) 0.0033(12) 0.0007(12) C2 0.0298(16) 0.0322(16) 0.0297(16) -0.0004(13) 0.0068(13) 0.0005(13) C3 0.0255(16) 0.0380(17) 0.0412(18) 0.0020(15) 0.0073(13) -0.0027(13) C4 0.0315(17) 0.0402(18) 0.0466(19) -0.0018(15) 0.0025(15) -0.0063(14) C5 0.0369(18) 0.0398(18) 0.0382(18) -0.0081(15) 0.0043(14) -0.0085(14) C6 0.0311(16) 0.0372(17) 0.0329(17) -0.0022(14) 0.0063(13) -0.0033(13) C7 0.0234(15) 0.0325(16) 0.0307(16) -0.0024(13) 0.0061(12) -0.0014(12) C8 0.0292(16) 0.0299(16) 0.0416(18) -0.0021(14) 0.0075(14) -0.0041(12) C9 0.0350(18) 0.046(2) 0.059(2) -0.0110(17) 0.0158(16) -0.0103(15) C10 0.0257(17) 0.053(2) 0.080(3) -0.018(2) 0.0139(17) -0.0072(15) C11 0.0299(17) 0.0418(19) 0.071(2) -0.0129(18) 0.0130(16) -0.0003(14) C12 0.0272(16) 0.0337(17) 0.0472(19) -0.0076(15) 0.0070(14) 0.0008(13) C13 0.0339(17) 0.0374(17) 0.0298(16) -0.0015(14) 0.0050(13) 0.0052(13) C14 0.0332(18) 0.046(2) 0.059(2) 0.0138(17) 0.0052(16) 0.0025(15) C15 0.0351(19) 0.063(2) 0.062(2) 0.0133(19) 0.0047(17) 0.0084(17) C16 0.045(2) 0.060(2) 0.062(2) 0.0158(19) 0.0082(18) 0.0213(18) C17 0.050(2) 0.051(2) 0.087(3) 0.025(2) 0.008(2) 0.0134(18) C18 0.040(2) 0.042(2) 0.073(3) 0.0166(18) 0.0064(18) 0.0065(15) C19 0.0330(17) 0.0258(15) 0.0308(16) 0.0002(13) 0.0043(13) 0.0035(12) C20 0.044(2) 0.048(2) 0.0403(19) -0.0111(16) 0.0044(16) 0.0095(15) C21 0.059(2) 0.064(2) 0.0368(19) -0.0079(17) 0.0142(17) 0.0176(19) C22 0.044(2) 0.046(2) 0.057(2) 0.0001(17) 0.0169(17) 0.0146(16) C23 0.0333(18) 0.069(2) 0.051(2) -0.0111(19) 0.0045(16) 0.0133(17) C24 0.0375(19) 0.069(2) 0.0353(18) -0.0104(17) 0.0052(15) 0.0099(17) C25 0.0423(18) 0.0306(16) 0.0267(16) -0.0018(13) 0.0005(14) 0.0030(14) C26 0.048(2) 0.0396(18) 0.0341(17) -0.0004(15) 0.0072(15) 0.0090(15) C27 0.081(3) 0.056(2) 0.047(2) -0.0029(19) 0.018(2) 0.026(2) C28 0.104(3) 0.036(2) 0.053(2) -0.0095(17) 0.007(2) 0.021(2) C29 0.093(3) 0.0343(19) 0.051(2) -0.0074(17) -0.007(2) -0.0023(19) C30 0.053(2) 0.0338(18) 0.0398(19) -0.0019(15) -0.0016(16) -0.0017(15) C31 0.0347(17) 0.0244(15) 0.0286(15) 0.0022(12) 0.0034(13) -0.0009(12) C32 0.0423(19) 0.0442(18) 0.0363(18) -0.0008(15) 0.0009(15) -0.0086(15) C33 0.059(2) 0.058(2) 0.039(2) -0.0039(18) -0.0129(18) -0.0107(19) C34 0.098(3) 0.040(2) 0.0293(18) -0.0024(16) -0.0033(19) 0.000(2) C35 0.075(3) 0.052(2) 0.0375(19) 0.0032(17) 0.0247(18) 0.0144(19) C36 0.0432(19) 0.0413(18) 0.0377(18) 0.0017(15) 0.0107(15) 0.0044(15) C37 0.045(2) 0.044(2) 0.074(3) -0.0048(19) 0.0162(19) -0.0019(16) C38 0.086(3) 0.045(2) 0.108(4) -0.025(2) 0.035(3) -0.026(2) C39 0.066(3) 0.059(3) 0.081(3) -0.025(2) 0.009(2) -0.010(2) C40 0.074(3) 0.053(2) 0.047(2) -0.0137(18) 0.0069(19) -0.012(2) C1S 0.060(3) 0.098(4) 0.055(2) -0.013(2) 0.012(2) -0.010(2) C2S 0.065(3) 0.100(4) 0.075(3) -0.025(3) 0.028(2) -0.017(3) C3S 0.064(3) 0.105(4) 0.089(3) -0.020(3) 0.025(3) 0.000(3) C4S 0.072(3) 0.111(4) 0.056(3) -0.014(3) 0.011(2) 0.009(3) C5S 0.065(3) 0.118(4) 0.067(3) 0.001(3) 0.009(2) -0.021(3) C6S 0.051(3) 0.097(4) 0.081(3) -0.002(3) 0.006(2) -0.010(2) C7S 0.086(3) 0.111(4) 0.081(3) 0.003(3) 0.019(3) -0.003(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 N3 2.299(2) . ? Ce N1 2.317(2) . ? Ce N2 2.336(2) . ? Ce O 2.582(2) . ? O C37 1.444(4) . ? O C40 1.466(4) . ? N1 C1 1.460(3) . ? N1 C7 1.468(3) . ? N2 C19 1.460(4) . ? N2 C13 1.474(3) . ? N3 C25 1.468(4) . ? N3 C31 1.472(3) . ? C1 C2 1.523(4) . ? C1 C6 1.530(4) . ? C2 C3 1.530(4) . ? C3 C4 1.523(4) . ? C4 C5 1.522(4) . ? C5 C6 1.538(4) . ? C7 C12 1.530(4) . ? C7 C8 1.533(4) . ? C8 C9 1.533(4) . ? C9 C10 1.521(4) . ? C10 C11 1.525(4) . ? C11 C12 1.525(4) . ? C13 C14 1.516(4) . ? C13 C18 1.531(4) . ? C14 C15 1.535(4) . ? C15 C16 1.503(5) . ? C16 C17 1.516(5) . ? C17 C18 1.530(4) . ? C19 C24 1.522(4) . ? C19 C20 1.523(4) . ? C20 C21 1.532(5) . ? C21 C22 1.515(4) . ? C22 C23 1.516(4) . ? C23 C24 1.528(4) . ? C25 C30 1.531(4) . ? C25 C26 1.536(4) . ? C26 C27 1.521(4) . ? C27 C28 1.515(5) . ? C28 C29 1.517(6) . ? C29 C30 1.528(5) . ? C31 C36 1.523(4) . ? C31 C32 1.530(4) . ? C32 C33 1.531(4) . ? C33 C34 1.510(5) . ? C34 C35 1.518(5) . ? C35 C36 1.534(4) . ? C37 C38 1.514(5) . ? C38 C39 1.505(6) . ? C39 C40 1.460(5) . ? C1S C2S 1.355(6) . ? C1S C6S 1.384(6) . ? C1S C7S 1.517(6) . ? C2S C3S 1.402(6) . ? C3S C4S 1.364(6) . ? C4S C5S 1.355(6) . ? C5S C6S 1.384(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 N3 Ce N1 108.66(8) . . ? N3 Ce N2 123.57(8) . . ? N1 Ce N2 109.72(8) . . ? N3 Ce O 94.69(7) . . ? N1 Ce O 124.87(7) . . ? N2 Ce O 95.73(7) . . ? C37 O C40 109.0(2) . . ? C37 O Ce 132.31(19) . . ? C40 O Ce 118.04(19) . . ? C1 N1 C7 114.9(2) . . ? C1 N1 Ce 123.78(16) . . ? C7 N1 Ce 121.31(16) . . ? C19 N2 C13 112.8(2) . . ? C19 N2 Ce 128.66(16) . . ? C13 N2 Ce 118.04(17) . . ? C25 N3 C31 115.1(2) . . ? C25 N3 Ce 109.93(16) . . ? C31 N3 Ce 134.89(17) . . ? N1 C1 C2 108.3(2) . . ? N1 C1 C6 115.1(2) . . ? C2 C1 C6 109.3(2) . . ? C1 C2 C3 113.2(2) . . ? C4 C3 C2 111.1(2) . . ? C5 C4 C3 110.1(2) . . ? C4 C5 C6 111.1(2) . . ? C1 C6 C5 111.6(2) . . ? N1 C7 C12 114.9(2) . . ? N1 C7 C8 108.7(2) . . ? C12 C7 C8 108.9(2) . . ? C7 C8 C9 112.6(2) . . ? C10 C9 C8 111.3(3) . . ? C9 C10 C11 111.2(3) . . ? C10 C11 C12 110.6(3) . . ? C11 C12 C7 111.5(3) . . ? N2 C13 C14 111.2(2) . . ? N2 C13 C18 113.5(2) . . ? C14 C13 C18 107.4(3) . . ? C13 C14 C15 112.7(3) . . ? C16 C15 C14 110.9(3) . . ? C15 C16 C17 111.0(3) . . ? C16 C17 C18 110.8(3) . . ? C17 C18 C13 112.5(3) . . ? N2 C19 C24 110.0(2) . . ? N2 C19 C20 114.2(2) . . ? C24 C19 C20 108.3(2) . . ? C19 C20 C21 112.5(3) . . ? C22 C21 C20 111.5(3) . . ? C21 C22 C23 110.7(3) . . ? C22 C23 C24 111.4(3) . . ? C19 C24 C23 113.1(3) . . ? N3 C25 C30 114.4(2) . . ? N3 C25 C26 116.0(2) . . ? C30 C25 C26 109.1(2) . . ? C27 C26 C25 112.6(3) . . ? C28 C27 C26 111.8(3) . . ? C27 C28 C29 111.0(3) . . ? C28 C29 C30 111.2(3) . . ? C29 C30 C25 112.9(3) . . ? N3 C31 C36 110.4(2) . . ? N3 C31 C32 112.9(2) . . ? C36 C31 C32 109.2(2) . . ? C31 C32 C33 112.5(3) . . ? C34 C33 C32 110.9(3) . . ? C33 C34 C35 110.5(3) . . ? C34 C35 C36 111.5(3) . . ? C31 C36 C35 112.3(3) . . ? O C37 C38 105.0(3) . . ? C39 C38 C37 103.9(3) . . ? C40 C39 C38 103.3(3) . . ? C39 C40 O 106.8(3) . . ? C2S C1S C6S 118.7(5) . . ? C2S C1S C7S 120.8(4) . . ? C6S C1S C7S 120.5(4) . . ? C1S C2S C3S 120.0(4) . . ? C4S C3S C2S 121.0(5) . . ? C5S C4S C3S 118.9(5) . . ? C4S C5S C6S 120.6(5) . . ? C5S C6S C1S 120.7(5) . . ? #===END data_(2)-dec604 _database_code_depnum_ccdc_archive 'CCDC 609100' _audit_creation_date 2004-12-03T16:59:13-00:00 _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 'C52 H96 Ce Li N4 O' _chemical_formula_sum 'C52 H96 Ce Li N4 O' _chemical_formula_weight 940.39 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _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 15.1681(3) _cell_length_b 19.1024(4) _cell_length_c 18.1727(3) _cell_angle_alpha 90 _cell_angle_beta 96.822(1) _cell_angle_gamma 90 _cell_volume 5228.21(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 27157 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2020 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.908 _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 0.7542 _exptl_absorpt_correction_T_max 0.8404 #----------------------------------------------------------------------------# # 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 0.47118E-1 _diffrn_orient_matrix_ub_12 -0.36738E-1 _diffrn_orient_matrix_ub_13 0.81177E-2 _diffrn_orient_matrix_ub_21 0.222733E-1 _diffrn_orient_matrix_ub_22 0.135247E-1 _diffrn_orient_matrix_ub_23 -0.476435E-1 _diffrn_orient_matrix_ub_31 0.411396E-1 _diffrn_orient_matrix_ub_32 0.347544E-1 _diffrn_orient_matrix_ub_33 0.271214E-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 0.0781 _diffrn_reflns_av_unetI/netI 0.0561 _diffrn_reflns_number 60421 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 10277 _reflns_number_gt 7866 _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^)+(0.0243P)^2^+4.6319P] 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 10277 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.073 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.392 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.079 #----------------------------------------------------------------------------# # 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' Li Li -0.0003 0.0001 '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 Ce Ce 0.416031(10) 0.206293(8) 0.210787(8) 0.01608(5) Uani 1 1 d . . . Li Li 0.5167(3) 0.3428(3) 0.1872(3) 0.0257(11) Uani 1 1 d . . . O O 0.58236(15) 0.42901(11) 0.19240(12) 0.0372(6) Uani 1 1 d . . . N1 N 0.39172(15) 0.33489(12) 0.22275(12) 0.0211(5) Uani 1 1 d . . . N2 N 0.55238(14) 0.24293(12) 0.15906(12) 0.0192(5) Uani 1 1 d . . . N3 N 0.29195(15) 0.16037(12) 0.14019(12) 0.0200(5) Uani 1 1 d . . . N4 N 0.44931(15) 0.12687(12) 0.30739(11) 0.0191(5) Uani 1 1 d . . . C1 C 0.38612(18) 0.36637(16) 0.29608(15) 0.0233(7) Uani 1 1 d . . . H1 H 0.4014 0.4171 0.2925 0.028 Uiso 1 1 calc R . . C2 C 0.2945(2) 0.36222(18) 0.32292(16) 0.0316(8) Uani 1 1 d . . . H2A H 0.2769 0.3125 0.326 0.038 Uiso 1 1 calc R . . H2B H 0.2505 0.3857 0.2865 0.038 Uiso 1 1 calc R . . C3 C 0.2934(2) 0.39671(19) 0.39913(17) 0.0394(9) Uani 1 1 d . . . H3A H 0.3065 0.4473 0.3954 0.047 Uiso 1 1 calc R . . H3B H 0.2336 0.3918 0.4152 0.047 Uiso 1 1 calc R . . C4 C 0.3618(2) 0.3630(2) 0.45602(18) 0.0448(9) Uani 1 1 d . . . H4A H 0.3448 0.3138 0.4637 0.054 Uiso 1 1 calc R . . H4B H 0.3627 0.3879 0.5039 0.054 Uiso 1 1 calc R . . C5 C 0.4541(2) 0.3652(2) 0.43103(17) 0.0410(9) Uani 1 1 d . . . H5A H 0.496 0.339 0.467 0.049 Uiso 1 1 calc R . . H5B H 0.4746 0.4144 0.4305 0.049 Uiso 1 1 calc R . . C6 C 0.4550(2) 0.33348(18) 0.35387(16) 0.0317(8) Uani 1 1 d . . . H6A H 0.5148 0.3398 0.3381 0.038 Uiso 1 1 calc R . . H6B H 0.4436 0.2826 0.3564 0.038 Uiso 1 1 calc R . . C7 C 0.32901(19) 0.36952(15) 0.16486(15) 0.0228(7) Uani 1 1 d . . . H7 H 0.2672 0.3603 0.1765 0.027 Uiso 1 1 calc R . . C8 C 0.3385(2) 0.33736(16) 0.08950(15) 0.0269(7) Uani 1 1 d . . . H8A H 0.3262 0.2865 0.0916 0.032 Uiso 1 1 calc R . . H8B H 0.4006 0.3431 0.0789 0.032 Uiso 1 1 calc R . . C9 C 0.2765(2) 0.36964(17) 0.02616(16) 0.0345(8) Uani 1 1 d . . . H9A H 0.2882 0.3482 -0.0213 0.041 Uiso 1 1 calc R . . H9B H 0.2142 0.3595 0.0335 0.041 Uiso 1 1 calc R . . C10 C 0.2899(2) 0.44825(18) 0.02259(17) 0.0394(9) Uani 1 1 d . . . H10A H 0.2458 0.4685 -0.0162 0.047 Uiso 1 1 calc R . . H10B H 0.3499 0.4583 0.0091 0.047 Uiso 1 1 calc R . . C11 C 0.2793(3) 0.48194(19) 0.09693(18) 0.0467(10) Uani 1 1 d . . . H11A H 0.2171 0.4766 0.1074 0.056 Uiso 1 1 calc R . . H11B H 0.2923 0.5326 0.0944 0.056 Uiso 1 1 calc R . . C12 C 0.3412(2) 0.44902(16) 0.15974(17) 0.0378(8) Uani 1 1 d . . . H12A H 0.3301 0.4707 0.2072 0.045 Uiso 1 1 calc R . . H12B H 0.4035 0.4592 0.152 0.045 Uiso 1 1 calc R . . C13 C 0.64220(18) 0.22453(14) 0.19462(14) 0.0190(6) Uani 1 1 d . . . H13 H 0.6521 0.1735 0.1864 0.023 Uiso 1 1 calc R . . C14 C 0.72003(18) 0.26537(17) 0.16847(15) 0.0250(7) Uani 1 1 d . . . H14A H 0.7222 0.2562 0.1151 0.03 Uiso 1 1 calc R . . H14B H 0.7101 0.3161 0.1746 0.03 Uiso 1 1 calc R . . C15 C 0.80930(19) 0.24484(18) 0.21195(17) 0.0316(8) Uani 1 1 d . . . H15A H 0.8219 0.195 0.2024 0.038 Uiso 1 1 calc R . . H15B H 0.8573 0.2734 0.1946 0.038 Uiso 1 1 calc R . . C16 C 0.80829(19) 0.25594(19) 0.29484(16) 0.0339(8) Uani 1 1 d . . . H16A H 0.8649 0.2392 0.3218 0.041 Uiso 1 1 calc R . . H16B H 0.8027 0.3065 0.3051 0.041 Uiso 1 1 calc R . . C17 C 0.73154(19) 0.21670(18) 0.32206(16) 0.0319(8) Uani 1 1 d . . . H17A H 0.7295 0.2273 0.3751 0.038 Uiso 1 1 calc R . . H17B H 0.7412 0.1657 0.3173 0.038 Uiso 1 1 calc R . . C18 C 0.64306(19) 0.23676(16) 0.27808(15) 0.0238(7) Uani 1 1 d . . . H18A H 0.6309 0.2868 0.2869 0.029 Uiso 1 1 calc R . . H18B H 0.595 0.2089 0.2962 0.029 Uiso 1 1 calc R . . C19 C 0.53729(19) 0.23124(15) 0.07802(14) 0.0207(6) Uani 1 1 d . . . H19 H 0.4716 0.2254 0.0666 0.025 Uiso 1 1 calc R . . C20 C 0.56024(19) 0.29403(17) 0.03029(15) 0.0260(7) Uani 1 1 d . . . H20A H 0.5322 0.3368 0.0476 0.031 Uiso 1 1 calc R . . H20B H 0.6253 0.3012 0.0367 0.031 Uiso 1 1 calc R . . C21 C 0.5286(2) 0.28282(17) -0.05153(15) 0.0345(8) Uani 1 1 d . . . H21A H 0.463 0.2796 -0.0588 0.041 Uiso 1 1 calc R . . H21B H 0.5463 0.3233 -0.0804 0.041 Uiso 1 1 calc R . . C22 C 0.5682(2) 0.21627(18) -0.07952(16) 0.0390(9) Uani 1 1 d . . . H22A H 0.6334 0.2216 -0.0772 0.047 Uiso 1 1 calc R . . H22B H 0.5441 0.2085 -0.1319 0.047 Uiso 1 1 calc R . . C23 C 0.5471(2) 0.15313(17) -0.03344(16) 0.0332(8) Uani 1 1 d . . . H23A H 0.5772 0.1113 -0.0508 0.04 Uiso 1 1 calc R . . H23B H 0.4823 0.1444 -0.0408 0.04 Uiso 1 1 calc R . . C24 C 0.57694(19) 0.16411(16) 0.04904(15) 0.0249(7) Uani 1 1 d . . . H24A H 0.6425 0.1669 0.0572 0.03 Uiso 1 1 calc R . . H24B H 0.5583 0.1234 0.0772 0.03 Uiso 1 1 calc R . . C25 C 0.26718(18) 0.11899(15) 0.07323(14) 0.0222(6) Uani 1 1 d . . . H25 H 0.2153 0.089 0.0816 0.027 Uiso 1 1 calc R . . C26 C 0.3428(2) 0.07166(18) 0.05865(16) 0.0355(8) Uani 1 1 d . . . H26A H 0.3568 0.0403 0.1018 0.043 Uiso 1 1 calc R . . H26B H 0.396 0.1008 0.0544 0.043 Uiso 1 1 calc R . . C27 C 0.3244(3) 0.02667(19) -0.01153(17) 0.0471(10) Uani 1 1 d . . . H27A H 0.3797 0.0022 -0.0205 0.056 Uiso 1 1 calc R . . H27B H 0.2795 -0.0093 -0.0036 0.056 Uiso 1 1 calc R . . C28 C 0.2914(2) 0.06946(18) -0.07903(16) 0.0353(8) Uani 1 1 d . . . H28A H 0.3407 0.0983 -0.0936 0.042 Uiso 1 1 calc R . . H28B H 0.2715 0.0376 -0.1207 0.042 Uiso 1 1 calc R . . C29 C 0.2155(2) 0.11669(19) -0.06479(17) 0.0396(9) Uani 1 1 d . . . H29A H 0.1634 0.0878 -0.0564 0.048 Uiso 1 1 calc R . . H29B H 0.1986 0.1463 -0.1089 0.048 Uiso 1 1 calc R . . C30 C 0.2412(2) 0.16351(18) 0.00286(16) 0.0347(8) Uani 1 1 d . . . H30A H 0.1905 0.1942 0.0107 0.042 Uiso 1 1 calc R . . H30B H 0.2918 0.1937 -0.0063 0.042 Uiso 1 1 calc R . . C31 C 0.21954(18) 0.17583(15) 0.18414(15) 0.0199(6) Uani 1 1 d . . . H31 H 0.2474 0.2045 0.2267 0.024 Uiso 1 1 calc R . . C32 C 0.17983(19) 0.11222(16) 0.21999(16) 0.0255(7) Uani 1 1 d . . . H32A H 0.1494 0.0819 0.1806 0.031 Uiso 1 1 calc R . . H32B H 0.2284 0.0847 0.2474 0.031 Uiso 1 1 calc R . . C33 C 0.11387(19) 0.13355(17) 0.27302(16) 0.0284(7) Uani 1 1 d . . . H33A H 0.1455 0.1594 0.3154 0.034 Uiso 1 1 calc R . . H33B H 0.0874 0.091 0.2926 0.034 Uiso 1 1 calc R . . C34 C 0.0402(2) 0.17959(17) 0.23446(17) 0.0315(8) Uani 1 1 d . . . H34A H 0.0045 0.1522 0.1954 0.038 Uiso 1 1 calc R . . H34B H 0.0004 0.1947 0.2709 0.038 Uiso 1 1 calc R . . C35 C 0.0781(2) 0.24323(18) 0.20023(17) 0.0332(8) Uani 1 1 d . . . H35A H 0.1087 0.2731 0.2398 0.04 Uiso 1 1 calc R . . H35B H 0.0292 0.2709 0.1734 0.04 Uiso 1 1 calc R . . C36 C 0.14376(19) 0.22172(16) 0.14636(16) 0.0256(7) Uani 1 1 d . . . H36A H 0.1693 0.2643 0.1261 0.031 Uiso 1 1 calc R . . H36B H 0.1116 0.1956 0.1044 0.031 Uiso 1 1 calc R . . C37 C 0.48297(18) 0.06569(15) 0.27076(15) 0.0221(6) Uani 1 1 d . . . H37 H 0.4916 0.082 0.2198 0.026 Uiso 1 1 calc R . . C38 C 0.57423(19) 0.03848(17) 0.30433(17) 0.0310(8) Uani 1 1 d . . . H38A H 0.6175 0.0775 0.3075 0.037 Uiso 1 1 calc R . . H38B H 0.5701 0.0215 0.3553 0.037 Uiso 1 1 calc R . . C39 C 0.6078(2) -0.02087(19) 0.2584(2) 0.0425(9) Uani 1 1 d . . . H39A H 0.6187 -0.0025 0.2094 0.051 Uiso 1 1 calc R . . H39B H 0.6649 -0.0386 0.2836 0.051 Uiso 1 1 calc R . . C40 C 0.5421(2) -0.08051(17) 0.24763(18) 0.0365(8) Uani 1 1 d . . . H40A H 0.5643 -0.1164 0.215 0.044 Uiso 1 1 calc R . . H40B H 0.5363 -0.1026 0.2961 0.044 Uiso 1 1 calc R . . C41 C 0.4523(2) -0.05469(16) 0.21348(17) 0.0310(7) Uani 1 1 d . . . H41A H 0.4096 -0.0941 0.2099 0.037 Uiso 1 1 calc R . . H41B H 0.457 -0.0376 0.1627 0.037 Uiso 1 1 calc R . . C42 C 0.41783(19) 0.00409(15) 0.25896(16) 0.0243(7) Uani 1 1 d . . . H42A H 0.4067 -0.0146 0.3078 0.029 Uiso 1 1 calc R . . H42B H 0.3606 0.0212 0.2334 0.029 Uiso 1 1 calc R . . C43 C 0.43774(18) 0.11530(16) 0.38542(14) 0.0220(6) Uani 1 1 d . . . H43 H 0.4339 0.0637 0.3934 0.026 Uiso 1 1 calc R . . C44 C 0.5146(2) 0.14352(18) 0.44029(15) 0.0303(8) Uani 1 1 d . . . H44A H 0.5706 0.1204 0.4308 0.036 Uiso 1 1 calc R . . H44B H 0.5213 0.1944 0.4322 0.036 Uiso 1 1 calc R . . C45 C 0.4987(2) 0.13057(19) 0.52080(16) 0.0385(9) Uani 1 1 d . . . H45A H 0.4964 0.0795 0.5299 0.046 Uiso 1 1 calc R . . H45B H 0.5488 0.1501 0.5544 0.046 Uiso 1 1 calc R . . C46 C 0.4129(2) 0.1639(2) 0.53762(16) 0.0400(9) Uani 1 1 d . . . H46A H 0.4174 0.2154 0.5332 0.048 Uiso 1 1 calc R . . H46B H 0.4029 0.1528 0.5892 0.048 Uiso 1 1 calc R . . C47 C 0.3347(2) 0.1376(2) 0.48440(16) 0.0393(9) Uani 1 1 d . . . H47A H 0.2803 0.1631 0.4936 0.047 Uiso 1 1 calc R . . H47B H 0.3252 0.0872 0.4936 0.047 Uiso 1 1 calc R . . C48 C 0.35107(19) 0.14793(17) 0.40355(15) 0.0264(7) Uani 1 1 d . . . H48A H 0.3011 0.1271 0.3709 0.032 Uiso 1 1 calc R . . H48B H 0.3521 0.1987 0.3928 0.032 Uiso 1 1 calc R . . C49 C 0.6131(3) 0.4678(2) 0.1334(2) 0.0555(11) Uani 1 1 d . . . H49A H 0.5697 0.4648 0.0882 0.067 Uiso 1 1 calc R . . H49B H 0.6707 0.4491 0.1217 0.067 Uiso 1 1 calc R . . C50 C 0.6232(3) 0.5420(2) 0.1591(2) 0.0627(12) Uani 1 1 d . . . H50A H 0.5689 0.5693 0.143 0.075 Uiso 1 1 calc R . . H50B H 0.6744 0.5646 0.1395 0.075 Uiso 1 1 calc R . . C51 C 0.6386(2) 0.53638(19) 0.2419(2) 0.0469(9) Uani 1 1 d . . . H51A H 0.7028 0.5339 0.2595 0.056 Uiso 1 1 calc R . . H51B H 0.6126 0.5769 0.2655 0.056 Uiso 1 1 calc R . . C52 C 0.5934(3) 0.4710(2) 0.2581(2) 0.0719(14) Uani 1 1 d . . . H52A H 0.6292 0.4453 0.2986 0.086 Uiso 1 1 calc R . . H52B H 0.5347 0.4816 0.2742 0.086 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 0.01556(8) 0.01677(8) 0.01604(8) -0.00044(7) 0.00246(6) -0.00055(8) Li 0.023(3) 0.018(3) 0.036(3) 0.001(2) 0.004(2) -0.004(2) O 0.0418(14) 0.0256(13) 0.0448(14) 0.0032(10) 0.0074(11) -0.0122(11) N1 0.0217(13) 0.0199(14) 0.0220(13) -0.0014(10) 0.0034(10) 0.0027(10) N2 0.0167(12) 0.0232(14) 0.0170(12) -0.0012(10) -0.0002(10) -0.0004(10) N3 0.0181(12) 0.0233(14) 0.0189(12) -0.0012(10) 0.0040(10) 0.0000(10) N4 0.0229(13) 0.0196(13) 0.0148(12) 0.0005(10) 0.0019(10) 0.0005(10) C1 0.0237(16) 0.0206(17) 0.0262(16) -0.0040(12) 0.0046(13) 0.0001(13) C2 0.0249(17) 0.038(2) 0.0323(18) -0.0070(14) 0.0062(14) 0.0033(15) C3 0.036(2) 0.047(2) 0.039(2) -0.0124(16) 0.0169(16) 0.0052(17) C4 0.053(2) 0.052(3) 0.0317(19) -0.0098(16) 0.0144(17) 0.0054(19) C5 0.040(2) 0.054(3) 0.0284(18) -0.0064(16) 0.0014(16) 0.0056(18) C6 0.0294(18) 0.037(2) 0.0288(17) -0.0029(14) 0.0046(14) 0.0040(15) C7 0.0209(15) 0.0248(17) 0.0225(15) -0.0023(12) 0.0019(12) 0.0050(13) C8 0.0297(17) 0.0221(18) 0.0289(17) -0.0031(13) 0.0034(14) 0.0016(14) C9 0.042(2) 0.033(2) 0.0269(17) -0.0020(14) -0.0024(15) 0.0030(16) C10 0.050(2) 0.034(2) 0.0325(19) 0.0053(15) 0.0004(16) 0.0098(17) C11 0.063(3) 0.029(2) 0.045(2) 0.0029(16) -0.0037(19) 0.0191(19) C12 0.053(2) 0.0231(19) 0.0351(19) -0.0054(14) -0.0043(16) 0.0102(16) C13 0.0177(15) 0.0188(16) 0.0204(15) 0.0002(11) 0.0021(12) 0.0012(11) C14 0.0193(16) 0.0334(18) 0.0223(16) 0.0024(13) 0.0028(12) -0.0002(13) C15 0.0161(16) 0.040(2) 0.0388(19) 0.0025(15) 0.0036(14) 0.0014(14) C16 0.0189(16) 0.050(2) 0.0311(18) 0.0017(15) -0.0054(14) -0.0038(15) C17 0.0287(18) 0.041(2) 0.0250(17) 0.0056(14) -0.0018(13) 0.0017(15) C18 0.0209(16) 0.0288(17) 0.0209(15) 0.0022(13) -0.0005(12) -0.0017(13) C19 0.0165(15) 0.0269(17) 0.0184(15) -0.0017(12) 0.0010(12) -0.0015(12) C20 0.0248(16) 0.0304(18) 0.0232(15) 0.0022(14) 0.0054(12) 0.0032(15) C21 0.040(2) 0.042(2) 0.0204(16) 0.0059(14) 0.0024(14) 0.0019(16) C22 0.049(2) 0.051(2) 0.0180(16) -0.0048(15) 0.0077(15) 0.0073(18) C23 0.039(2) 0.035(2) 0.0259(17) -0.0108(14) 0.0075(15) 0.0028(16) C24 0.0251(16) 0.0258(18) 0.0244(16) -0.0039(13) 0.0061(13) 0.0029(14) C25 0.0209(15) 0.0249(17) 0.0215(15) -0.0019(12) 0.0054(12) -0.0042(13) C26 0.043(2) 0.043(2) 0.0197(16) 0.0016(14) 0.0003(15) 0.0178(17) C27 0.077(3) 0.037(2) 0.0278(19) -0.0038(15) 0.0115(18) 0.016(2) C28 0.044(2) 0.043(2) 0.0200(16) -0.0081(14) 0.0064(15) -0.0019(17) C29 0.038(2) 0.054(2) 0.0253(18) -0.0053(16) -0.0021(15) 0.0013(18) C30 0.039(2) 0.040(2) 0.0242(17) -0.0022(14) -0.0009(15) 0.0104(16) C31 0.0170(15) 0.0229(16) 0.0196(15) -0.0008(12) 0.0012(12) -0.0008(12) C32 0.0248(16) 0.0251(18) 0.0279(16) 0.0030(13) 0.0083(13) 0.0019(13) C33 0.0253(17) 0.0324(19) 0.0292(17) 0.0064(14) 0.0106(13) 0.0024(14) C34 0.0208(17) 0.042(2) 0.0332(18) -0.0015(15) 0.0078(14) 0.0050(15) C35 0.0279(18) 0.035(2) 0.0376(19) 0.0048(15) 0.0079(15) 0.0117(15) C36 0.0206(16) 0.0269(19) 0.0296(17) 0.0052(13) 0.0046(13) 0.0013(13) C37 0.0254(16) 0.0241(17) 0.0171(15) 0.0031(12) 0.0044(12) 0.0030(13) C38 0.0223(17) 0.0290(19) 0.042(2) -0.0029(14) 0.0039(14) -0.0020(14) C39 0.0277(19) 0.040(2) 0.060(2) -0.0041(18) 0.0081(17) 0.0107(16) C40 0.040(2) 0.029(2) 0.041(2) -0.0051(15) 0.0044(16) 0.0094(16) C41 0.0354(18) 0.0239(18) 0.0332(18) -0.0049(14) 0.0015(15) 0.0039(14) C42 0.0216(16) 0.0254(18) 0.0254(16) -0.0021(13) 0.0007(13) 0.0016(13) C43 0.0250(16) 0.0237(17) 0.0167(14) 0.0009(12) 0.0000(12) -0.0025(13) C44 0.0262(17) 0.041(2) 0.0231(16) -0.0048(14) -0.0008(13) -0.0010(15) C45 0.043(2) 0.048(2) 0.0224(17) -0.0066(15) -0.0044(15) -0.0014(18) C46 0.052(2) 0.048(2) 0.0190(17) -0.0060(15) 0.0023(15) -0.0034(18) C47 0.039(2) 0.056(3) 0.0245(17) -0.0076(16) 0.0122(15) -0.0086(18) C48 0.0243(16) 0.0328(19) 0.0226(16) -0.0041(13) 0.0053(13) -0.0016(14) C49 0.077(3) 0.043(3) 0.050(2) -0.0010(18) 0.022(2) -0.025(2) C50 0.096(3) 0.034(2) 0.061(3) 0.0040(19) 0.019(2) -0.020(2) C51 0.047(2) 0.033(2) 0.063(3) -0.0067(18) 0.0132(19) -0.0064(18) C52 0.111(4) 0.058(3) 0.042(2) 0.002(2) -0.008(2) -0.046(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 N3 2.320(2) . ? Ce N4 2.330(2) . ? Ce N2 2.472(2) . ? Ce N1 2.497(2) . ? Ce C31 3.019(3) . ? Ce C37 3.028(3) . ? Li O 1.921(5) . ? Li N2 2.065(5) . ? Li N1 2.079(5) . ? O C49 1.427(4) . ? O C52 1.432(4) . ? N1 C1 1.474(3) . ? N1 C7 1.487(3) . ? N2 C13 1.479(3) . ? N2 C19 1.480(3) . ? N3 C25 1.462(3) . ? N3 C31 1.463(3) . ? N4 C43 1.466(3) . ? N4 C37 1.466(3) . ? C1 C6 1.526(4) . ? C1 C2 1.528(4) . ? C2 C3 1.536(4) . ? C3 C4 1.517(5) . ? C4 C5 1.523(5) . ? C5 C6 1.529(4) . ? C7 C8 1.523(4) . ? C7 C12 1.534(4) . ? C8 C9 1.527(4) . ? C9 C10 1.518(4) . ? C10 C11 1.522(4) . ? C11 C12 1.525(4) . ? C13 C18 1.533(4) . ? C13 C14 1.537(4) . ? C14 C15 1.535(4) . ? C15 C16 1.523(4) . ? C16 C17 1.516(4) . ? C17 C18 1.527(4) . ? C19 C24 1.536(4) . ? C19 C20 1.544(4) . ? C20 C21 1.522(4) . ? C21 C22 1.519(4) . ? C22 C23 1.524(4) . ? C23 C24 1.528(4) . ? C25 C26 1.509(4) . ? C25 C30 1.547(4) . ? C26 C27 1.536(4) . ? C27 C28 1.509(4) . ? C28 C29 1.509(4) . ? C29 C30 1.533(4) . ? C31 C32 1.535(4) . ? C31 C36 1.540(4) . ? C32 C33 1.525(4) . ? C33 C34 1.526(4) . ? C34 C35 1.510(4) . ? C35 C36 1.534(4) . ? C37 C42 1.535(4) . ? C37 C38 1.536(4) . ? C38 C39 1.530(4) . ? C39 C40 1.511(5) . ? C40 C41 1.511(4) . ? C41 C42 1.523(4) . ? C43 C48 1.526(4) . ? C43 C44 1.539(4) . ? C44 C45 1.531(4) . ? C45 C46 1.512(5) . ? C46 C47 1.524(4) . ? C47 C48 1.532(4) . ? C49 C50 1.493(5) . ? C50 C51 1.499(5) . ? C51 C52 1.472(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ce N4 105.03(8) . . ? N3 Ce N2 123.85(7) . . ? N4 Ce N2 110.77(7) . . ? N3 Ce N1 107.55(8) . . ? N4 Ce N1 126.58(7) . . ? N2 Ce N1 83.88(8) . . ? N3 Ce C31 28.11(7) . . ? N4 Ce C31 96.71(8) . . ? N2 Ce C31 148.01(7) . . ? N1 Ce C31 92.89(8) . . ? N3 Ce C37 94.53(8) . . ? N4 Ce C37 28.10(7) . . ? N2 Ce C37 97.36(8) . . ? N1 Ce C37 152.60(7) . . ? C31 Ce C37 99.74(8) . . ? O Li N2 130.9(3) . . ? O Li N1 122.3(3) . . ? N2 Li N1 106.6(2) . . ? C49 O C52 108.7(3) . . ? C49 O Li 128.5(3) . . ? C52 O Li 121.9(3) . . ? C1 N1 C7 110.9(2) . . ? C1 N1 Li 113.8(2) . . ? C7 N1 Li 106.2(2) . . ? C1 N1 Ce 120.33(17) . . ? C7 N1 Ce 117.69(16) . . ? Li N1 Ce 83.99(16) . . ? C13 N2 C19 115.1(2) . . ? C13 N2 Li 111.5(2) . . ? C19 N2 Li 111.8(2) . . ? C13 N2 Ce 122.36(16) . . ? C19 N2 Ce 107.34(15) . . ? Li N2 Ce 84.92(15) . . ? C25 N3 C31 115.3(2) . . ? C25 N3 Ce 140.88(17) . . ? C31 N3 Ce 103.54(15) . . ? C43 N4 C37 114.0(2) . . ? C43 N4 Ce 141.88(18) . . ? C37 N4 Ce 103.46(15) . . ? N1 C1 C6 110.2(2) . . ? N1 C1 C2 114.8(2) . . ? C6 C1 C2 109.5(2) . . ? C1 C2 C3 111.9(2) . . ? C4 C3 C2 110.7(3) . . ? C3 C4 C5 111.3(3) . . ? C4 C5 C6 111.8(3) . . ? C1 C6 C5 112.8(3) . . ? N1 C7 C8 109.6(2) . . ? N1 C7 C12 114.3(2) . . ? C8 C7 C12 108.6(2) . . ? C7 C8 C9 113.6(2) . . ? C10 C9 C8 111.0(3) . . ? C9 C10 C11 110.6(3) . . ? C10 C11 C12 111.7(3) . . ? C11 C12 C7 112.7(3) . . ? N2 C13 C18 107.2(2) . . ? N2 C13 C14 116.5(2) . . ? C18 C13 C14 108.2(2) . . ? C15 C14 C13 112.0(2) . . ? C16 C15 C14 111.2(2) . . ? C17 C16 C15 110.6(3) . . ? C16 C17 C18 111.5(2) . . ? C17 C18 C13 112.5(2) . . ? N2 C19 C24 116.5(2) . . ? N2 C19 C20 115.0(2) . . ? C24 C19 C20 109.4(2) . . ? C21 C20 C19 111.9(2) . . ? C22 C21 C20 110.7(3) . . ? C21 C22 C23 111.2(3) . . ? C22 C23 C24 111.9(3) . . ? C23 C24 C19 111.6(2) . . ? N3 C25 C26 110.2(2) . . ? N3 C25 C30 113.9(2) . . ? C26 C25 C30 108.0(2) . . ? C25 C26 C27 114.5(3) . . ? C28 C27 C26 112.5(3) . . ? C29 C28 C27 111.8(3) . . ? C28 C29 C30 111.1(3) . . ? C29 C30 C25 111.0(3) . . ? N3 C31 C32 115.4(2) . . ? N3 C31 C36 116.1(2) . . ? C32 C31 C36 109.3(2) . . ? N3 C31 Ce 48.35(12) . . ? C32 C31 Ce 120.94(17) . . ? C36 C31 Ce 129.19(18) . . ? C33 C32 C31 112.1(2) . . ? C32 C33 C34 111.3(2) . . ? C35 C34 C33 111.0(3) . . ? C34 C35 C36 110.8(3) . . ? C35 C36 C31 112.0(2) . . ? N4 C37 C42 114.9(2) . . ? N4 C37 C38 115.8(2) . . ? C42 C37 C38 109.3(2) . . ? N4 C37 Ce 48.44(12) . . ? C42 C37 Ce 116.55(17) . . ? C38 C37 Ce 133.72(19) . . ? C39 C38 C37 112.1(3) . . ? C40 C39 C38 111.9(3) . . ? C41 C40 C39 110.8(3) . . ? C40 C41 C42 111.6(2) . . ? C41 C42 C37 112.6(2) . . ? N4 C43 C48 110.6(2) . . ? N4 C43 C44 113.9(2) . . ? C48 C43 C44 108.9(2) . . ? C45 C44 C43 111.7(3) . . ? C46 C45 C44 111.2(3) . . ? C45 C46 C47 110.9(3) . . ? C46 C47 C48 111.3(3) . . ? C43 C48 C47 113.3(2) . . ? O C49 C50 106.8(3) . . ? C49 C50 C51 104.1(3) . . ? C52 C51 C50 104.0(3) . . ? O C52 C51 108.6(3) . . ? #===END data_(3)-dec1704 _database_code_depnum_ccdc_archive 'CCDC 609101' _audit_creation_date 2004-12-10T10:27:10-00:00 _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 'C48 H88 Ce N4' _chemical_formula_sum 'C48 H88 Ce N4' _chemical_formula_weight 861.34 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-4 _symmetry_space_group_name_Hall 'P -4' _symmetry_Int_Tables_number 81 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' _cell_length_a 21.1876(5) _cell_length_b 21.1876(5) _cell_length_c 10.3198(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4632.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19600 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.018 _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 0.8501 _exptl_absorpt_correction_T_max 0.9868 #----------------------------------------------------------------------------# # 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 0.265666E-1 _diffrn_orient_matrix_ub_12 0.86946E-2 _diffrn_orient_matrix_ub_13 -0.780777E-1 _diffrn_orient_matrix_ub_21 0.389214E-1 _diffrn_orient_matrix_ub_22 -0.90125E-2 _diffrn_orient_matrix_ub_23 0.515934E-1 _diffrn_orient_matrix_ub_31 -0.26325E-2 _diffrn_orient_matrix_ub_32 -0.455058E-1 _diffrn_orient_matrix_ub_33 -0.251361E-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 0.0543 _diffrn_reflns_av_unetI/netI 0.0782 _diffrn_reflns_number 20827 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 8991 _reflns_number_gt 7005 _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^)+(0.0372P)^2^+8.2990P] 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 8991 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.106 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.510(18) _refine_diff_density_max 1.632 _refine_diff_density_min -1.145 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # 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 0.5 0.5 0 0.0255(3) Uani 1 4 d S . . N1 N 0.5821(3) 0.4907(3) 0.1363(6) 0.0270(15) Uani 1 1 d . . . C1 C 0.6343(4) 0.5306(3) 0.1848(7) 0.0305(17) Uani 1 1 d . . . H1 H 0.6513 0.5107 0.2654 0.037 Uiso 1 1 calc R . . C2 C 0.6882(3) 0.5345(3) 0.0858(7) 0.0364(17) Uani 1 1 d . . . H2A H 0.7053 0.4917 0.0708 0.044 Uiso 1 1 calc R . . H2B H 0.6713 0.5503 0.0025 0.044 Uiso 1 1 calc R . . C3 C 0.7417(3) 0.5778(3) 0.1300(7) 0.0436(19) Uani 1 1 d . . . H3A H 0.7736 0.581 0.0602 0.052 Uiso 1 1 calc R . . H3B H 0.7625 0.5592 0.2069 0.052 Uiso 1 1 calc R . . C4 C 0.7179(3) 0.6440(3) 0.1639(7) 0.0423(18) Uani 1 1 d . . . H4A H 0.7529 0.6697 0.1991 0.051 Uiso 1 1 calc R . . H4B H 0.7017 0.6651 0.0849 0.051 Uiso 1 1 calc R . . C5 C 0.6658(3) 0.6388(4) 0.2632(8) 0.0459(19) Uani 1 1 d . . . H5A H 0.6492 0.6816 0.2818 0.055 Uiso 1 1 calc R . . H5B H 0.6835 0.6217 0.3447 0.055 Uiso 1 1 calc R . . C6 C 0.6114(3) 0.5966(3) 0.2191(7) 0.0398(18) Uani 1 1 d . . . H6A H 0.5796 0.5937 0.2892 0.048 Uiso 1 1 calc R . . H6B H 0.5908 0.6157 0.1424 0.048 Uiso 1 1 calc R . . C7 C 0.5773(3) 0.4281(3) 0.1943(7) 0.0326(17) Uani 1 1 d . . . H7 H 0.5424 0.4061 0.1473 0.039 Uiso 1 1 calc R . . C8 C 0.6362(3) 0.3868(3) 0.1765(8) 0.0349(16) Uani 1 1 d . . . H8A H 0.6465 0.3845 0.083 0.042 Uiso 1 1 calc R . . H8B H 0.6722 0.4072 0.2209 0.042 Uiso 1 1 calc R . . C9 C 0.6289(4) 0.3199(3) 0.2287(7) 0.048(2) Uani 1 1 d . . . H9A H 0.5981 0.2967 0.1745 0.057 Uiso 1 1 calc R . . H9B H 0.6699 0.2978 0.223 0.057 Uiso 1 1 calc R . . C10 C 0.6064(4) 0.3199(4) 0.3686(7) 0.045(2) Uani 1 1 d . . . H10A H 0.5973 0.276 0.3958 0.054 Uiso 1 1 calc R . . H10B H 0.6403 0.3365 0.425 0.054 Uiso 1 1 calc R . . C11 C 0.5476(3) 0.3598(3) 0.3855(7) 0.0419(18) Uani 1 1 d . . . H11A H 0.5354 0.3606 0.4781 0.05 Uiso 1 1 calc R . . H11B H 0.5124 0.3409 0.3358 0.05 Uiso 1 1 calc R . . C12 C 0.5592(3) 0.4271(3) 0.3383(7) 0.0366(17) Uani 1 1 d . . . H12A H 0.5935 0.4464 0.39 0.044 Uiso 1 1 calc R . . H12B H 0.5205 0.4526 0.3515 0.044 Uiso 1 1 calc R . . Ce1B Ce 0 0 0 0.0140(2) Uani 1 4 d S . . N1B N 0.0310(3) 0.0769(3) 0.1351(6) 0.0206(14) Uani 1 1 d . . . C1B C 0.0919(3) 0.1010(3) 0.1839(7) 0.0218(15) Uani 1 1 d . . . H1B H 0.0837 0.1231 0.2678 0.026 Uiso 1 1 calc R . . C2B C 0.1214(3) 0.1494(3) 0.0893(7) 0.0263(15) Uani 1 1 d . . . H2B1 H 0.1261 0.1295 0.003 0.032 Uiso 1 1 calc R . . H2B2 H 0.0925 0.1858 0.08 0.032 Uiso 1 1 calc R . . C3B C 0.1860(3) 0.1731(3) 0.1352(7) 0.0335(17) Uani 1 1 d . . . H3B1 H 0.1808 0.1972 0.2166 0.04 Uiso 1 1 calc R . . H3B2 H 0.2039 0.2019 0.0692 0.04 Uiso 1 1 calc R . . C4B C 0.2320(3) 0.1182(3) 0.1583(6) 0.0339(17) Uani 1 1 d . . . H4B1 H 0.2412 0.0968 0.0751 0.041 Uiso 1 1 calc R . . H4B2 H 0.2722 0.1346 0.1939 0.041 Uiso 1 1 calc R . . C5B C 0.2028(3) 0.0712(3) 0.2534(7) 0.0325(17) Uani 1 1 d . . . H5B1 H 0.2315 0.0347 0.2633 0.039 Uiso 1 1 calc R . . H5B2 H 0.1985 0.0916 0.3392 0.039 Uiso 1 1 calc R . . C6B C 0.1384(3) 0.0476(3) 0.2099(6) 0.0254(15) Uani 1 1 d . . . H6B1 H 0.1208 0.0196 0.2777 0.03 Uiso 1 1 calc R . . H6B2 H 0.1435 0.0223 0.13 0.03 Uiso 1 1 calc R . . C7B C -0.0253(3) 0.1041(3) 0.1956(7) 0.0204(15) Uani 1 1 d . . . H7B H -0.0623 0.0853 0.1492 0.025 Uiso 1 1 calc R . . C8B C -0.0311(3) 0.1762(3) 0.1782(7) 0.0244(14) Uani 1 1 d . . . H8B1 H 0.0051 0.197 0.2213 0.029 Uiso 1 1 calc R . . H8B2 H -0.029 0.1864 0.0847 0.029 Uiso 1 1 calc R . . C9B C -0.0925(3) 0.2028(3) 0.2342(6) 0.0277(16) Uani 1 1 d . . . H9B1 H -0.0921 0.2494 0.2272 0.033 Uiso 1 1 calc R . . H9B2 H -0.1287 0.1868 0.1832 0.033 Uiso 1 1 calc R . . C10B C -0.1007(3) 0.1840(3) 0.3755(6) 0.0282(15) Uani 1 1 d . . . H10C H -0.0675 0.2046 0.4282 0.034 Uiso 1 1 calc R . . H10D H -0.1422 0.1992 0.4069 0.034 Uiso 1 1 calc R . . C11B C -0.0968(3) 0.1134(3) 0.3936(6) 0.0289(15) Uani 1 1 d . . . H11C H -0.1326 0.0929 0.3485 0.035 Uiso 1 1 calc R . . H11D H -0.0999 0.1031 0.487 0.035 Uiso 1 1 calc R . . C12B C -0.0343(3) 0.0878(3) 0.3394(6) 0.0243(15) Uani 1 1 d . . . H12C H 0.0012 0.1057 0.3898 0.029 Uiso 1 1 calc R . . H12D H -0.0333 0.0413 0.3501 0.029 Uiso 1 1 calc R . . Ce1C Ce 0 0.5 -0.34063(3) 0.01686(10) Uani 1 2 d S . . N1C N 0.0766(2) 0.4670(2) -0.2071(5) 0.0222(12) Uani 1 1 d . . . N2C N 0.0347(2) 0.5752(2) -0.4751(5) 0.0220(11) Uani 1 1 d . . . C1C C 0.0976(3) 0.4053(3) -0.1576(6) 0.0252(14) Uani 1 1 d . . . H1C H 0.1199 0.4122 -0.0733 0.03 Uiso 1 1 calc R . . C2C C 0.1440(3) 0.3738(3) -0.2523(6) 0.0318(16) Uani 1 1 d . . . H2C1 H 0.1242 0.3713 -0.3391 0.038 Uiso 1 1 calc R . . H2C2 H 0.1823 0.4003 -0.2598 0.038 Uiso 1 1 calc R . . C3C C 0.1633(3) 0.3071(3) -0.2093(7) 0.0358(17) Uani 1 1 d . . . H3C1 H 0.1902 0.2877 -0.2768 0.043 Uiso 1 1 calc R . . H3C2 H 0.1883 0.3099 -0.1285 0.043 Uiso 1 1 calc R . . C4C C 0.1067(3) 0.2660(3) -0.1865(7) 0.0362(17) Uani 1 1 d . . . H4C1 H 0.1205 0.2243 -0.1537 0.043 Uiso 1 1 calc R . . H4C2 H 0.084 0.2593 -0.2692 0.043 Uiso 1 1 calc R . . C5C C 0.0629(4) 0.2969(3) -0.0887(8) 0.033(2) Uani 1 1 d . . . H5C1 H 0.085 0.3008 -0.0046 0.04 Uiso 1 1 calc R . . H5C2 H 0.0255 0.2697 -0.0755 0.04 Uiso 1 1 calc R . . C6C C 0.0415(3) 0.3620(3) -0.1336(7) 0.0322(17) Uani 1 1 d . . . H6C1 H 0.0138 0.3809 -0.0669 0.039 Uiso 1 1 calc R . . H6C2 H 0.0167 0.3578 -0.2145 0.039 Uiso 1 1 calc R . . C7C C 0.1064(3) 0.5229(3) -0.1459(6) 0.0243(15) Uani 1 1 d . . . H7C H 0.0896 0.5604 -0.1934 0.029 Uiso 1 1 calc R . . C8C C 0.0882(3) 0.5327(3) -0.0028(5) 0.0253(15) Uani 1 1 d . . . H8C1 H 0.0417 0.5333 0.0054 0.03 Uiso 1 1 calc R . . H8C2 H 0.1045 0.4971 0.0496 0.03 Uiso 1 1 calc R . . C9C C 0.1154(3) 0.5947(3) 0.0490(7) 0.0341(16) Uani 1 1 d . . . H9C1 H 0.0957 0.6305 0.0022 0.041 Uiso 1 1 calc R . . H9C2 H 0.1045 0.5989 0.142 0.041 Uiso 1 1 calc R . . C10C C 0.1869(3) 0.5984(3) 0.0335(7) 0.0350(17) Uani 1 1 d . . . H10E H 0.2071 0.5661 0.0893 0.042 Uiso 1 1 calc R . . H10F H 0.2019 0.6404 0.0619 0.042 Uiso 1 1 calc R . . C11C C 0.2063(4) 0.5873(4) -0.1088(8) 0.0329(19) Uani 1 1 d . . . H11E H 0.1917 0.6231 -0.1624 0.04 Uiso 1 1 calc R . . H11F H 0.2529 0.5854 -0.1148 0.04 Uiso 1 1 calc R . . C12C C 0.1781(3) 0.5256(3) -0.1617(6) 0.0294(15) Uani 1 1 d . . . H12E H 0.1887 0.5215 -0.2547 0.035 Uiso 1 1 calc R . . H12F H 0.1972 0.4894 -0.1155 0.035 Uiso 1 1 calc R . . C13C C 0.0973(3) 0.5945(3) -0.5259(6) 0.0241(14) Uani 1 1 d . . . H13C H 0.0912 0.6135 -0.6137 0.029 Uiso 1 1 calc R . . C14C C 0.1301(3) 0.6434(3) -0.4397(6) 0.0323(16) Uani 1 1 d . . . H14A H 0.1045 0.6825 -0.4379 0.039 Uiso 1 1 calc R . . H14B H 0.1327 0.6269 -0.3501 0.039 Uiso 1 1 calc R . . C15C C 0.1960(4) 0.6587(4) -0.4878(8) 0.049(2) Uani 1 1 d . . . H15A H 0.1932 0.6787 -0.5743 0.059 Uiso 1 1 calc R . . H15B H 0.2162 0.6891 -0.4279 0.059 Uiso 1 1 calc R . . C16C C 0.2359(3) 0.5996(4) -0.4966(7) 0.049(2) Uani 1 1 d . . . H16A H 0.2414 0.5813 -0.4091 0.059 Uiso 1 1 calc R . . H16B H 0.2782 0.6105 -0.5309 0.059 Uiso 1 1 calc R . . C17C C 0.2049(4) 0.5517(5) -0.5845(9) 0.055(3) Uani 1 1 d . . . H17A H 0.2033 0.5687 -0.6738 0.066 Uiso 1 1 calc R . . H17B H 0.2306 0.5127 -0.5859 0.066 Uiso 1 1 calc R . . C18C C 0.1389(4) 0.5360(3) -0.5402(8) 0.0343(18) Uani 1 1 d . . . H18A H 0.1411 0.5139 -0.4558 0.041 Uiso 1 1 calc R . . H18B H 0.1192 0.507 -0.6035 0.041 Uiso 1 1 calc R . . C19C C -0.0203(3) 0.6055(3) -0.5390(6) 0.0245(15) Uani 1 1 d . . . H19C H -0.0584 0.5893 -0.4924 0.029 Uiso 1 1 calc R . . C20C C -0.0297(3) 0.5876(3) -0.6813(6) 0.0276(15) Uani 1 1 d . . . H20A H -0.0315 0.541 -0.6891 0.033 Uiso 1 1 calc R . . H20B H 0.0068 0.6027 -0.7325 0.033 Uiso 1 1 calc R . . C21C C -0.0907(3) 0.6163(3) -0.7365(6) 0.0324(16) Uani 1 1 d . . . H21A H -0.0949 0.6047 -0.829 0.039 Uiso 1 1 calc R . . H21B H -0.1276 0.5988 -0.6896 0.039 Uiso 1 1 calc R . . C22C C -0.0902(4) 0.6880(3) -0.7232(7) 0.0371(17) Uani 1 1 d . . . H22A H -0.1304 0.7054 -0.7566 0.044 Uiso 1 1 calc R . . H22B H -0.0553 0.7057 -0.7755 0.044 Uiso 1 1 calc R . . C23C C -0.0817(4) 0.7072(3) -0.5791(8) 0.038(2) Uani 1 1 d . . . H23A H -0.0788 0.7537 -0.5723 0.045 Uiso 1 1 calc R . . H23B H -0.1188 0.6931 -0.5283 0.045 Uiso 1 1 calc R . . C24C C -0.0224(3) 0.6776(3) -0.5243(7) 0.0322(17) Uani 1 1 d . . . H24A H -0.0193 0.6884 -0.4312 0.039 Uiso 1 1 calc R . . H24B H 0.0147 0.696 -0.5687 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0261(3) 0.0261(3) 0.0245(6) 0 0 0 N1 0.024(3) 0.030(4) 0.027(3) 0.002(3) -0.005(2) 0.001(3) C1 0.041(5) 0.027(4) 0.023(4) 0.001(3) -0.001(4) 0.001(4) C2 0.029(4) 0.038(4) 0.042(4) -0.011(3) 0.002(3) 0.000(3) C3 0.036(4) 0.050(5) 0.046(4) -0.001(4) -0.002(3) -0.008(4) C4 0.041(4) 0.034(4) 0.052(5) -0.002(4) -0.006(4) -0.004(3) C5 0.044(5) 0.043(5) 0.050(5) -0.011(4) 0.005(4) -0.013(4) C6 0.044(4) 0.037(4) 0.039(4) 0.000(3) 0.007(3) -0.008(3) C7 0.037(4) 0.031(4) 0.029(4) -0.006(3) -0.004(3) 0.000(3) C8 0.039(4) 0.027(4) 0.039(4) 0.002(3) -0.001(4) -0.002(3) C9 0.054(5) 0.040(5) 0.049(5) 0.008(4) -0.013(4) 0.003(4) C10 0.061(5) 0.034(4) 0.041(4) 0.006(3) -0.008(4) -0.004(4) C11 0.050(5) 0.043(4) 0.033(4) 0.009(3) -0.004(3) -0.005(4) C12 0.039(4) 0.033(4) 0.038(4) 0.004(3) -0.005(3) 0.007(3) Ce1B 0.0149(3) 0.0149(3) 0.0122(5) 0 0 0 N1B 0.020(3) 0.019(3) 0.023(3) -0.003(2) 0.001(3) 0.000(2) C1B 0.024(4) 0.024(4) 0.017(3) -0.001(3) -0.002(3) -0.005(3) C2B 0.025(4) 0.024(4) 0.030(4) 0.002(3) 0.002(3) 0.001(3) C3B 0.034(4) 0.025(4) 0.041(4) 0.002(3) 0.004(3) -0.010(3) C4B 0.027(4) 0.042(4) 0.032(4) -0.008(3) -0.001(3) -0.008(3) C5B 0.020(4) 0.044(4) 0.033(4) -0.004(3) -0.008(3) 0.001(3) C6B 0.026(4) 0.025(3) 0.025(4) 0.004(3) -0.002(3) -0.001(3) C7B 0.020(3) 0.021(4) 0.020(4) -0.003(3) 0.001(3) 0.004(3) C8B 0.039(4) 0.017(3) 0.018(3) 0.002(3) 0.000(3) -0.001(3) C9B 0.031(4) 0.019(3) 0.033(4) 0.002(3) 0.002(3) 0.005(3) C10B 0.036(4) 0.025(4) 0.024(3) -0.004(3) 0.007(3) 0.000(3) C11B 0.034(4) 0.023(4) 0.029(4) -0.009(3) 0.007(3) 0.001(3) C12B 0.033(4) 0.018(3) 0.022(4) -0.001(3) 0.001(3) -0.002(3) Ce1C 0.0196(4) 0.0169(4) 0.0141(2) 0 0 -0.0002(3) N1C 0.023(3) 0.022(3) 0.022(3) 0.003(2) -0.003(2) 0.001(2) N2C 0.022(3) 0.024(3) 0.020(3) 0.002(2) 0.000(2) -0.001(2) C1C 0.027(3) 0.030(4) 0.019(3) 0.005(3) -0.006(3) -0.002(3) C2C 0.031(4) 0.033(4) 0.031(4) 0.002(3) -0.002(3) 0.008(3) C3C 0.035(4) 0.033(4) 0.040(4) -0.001(3) -0.006(3) 0.009(3) C4C 0.045(4) 0.023(4) 0.041(4) 0.004(3) -0.005(4) 0.008(3) C5C 0.039(5) 0.024(4) 0.038(4) -0.001(3) 0.004(4) -0.005(3) C6C 0.036(4) 0.029(4) 0.032(4) 0.004(3) -0.002(3) 0.007(4) C7C 0.032(4) 0.026(4) 0.014(3) 0.007(3) -0.003(3) 0.003(3) C8C 0.031(4) 0.026(4) 0.019(4) -0.002(3) 0.002(3) -0.006(3) C9C 0.042(4) 0.035(4) 0.026(4) -0.011(3) 0.003(3) -0.002(3) C10C 0.033(4) 0.043(4) 0.029(4) -0.006(3) -0.011(3) -0.003(3) C11C 0.032(4) 0.034(5) 0.032(4) 0.002(4) -0.007(3) -0.013(4) C12C 0.031(4) 0.031(4) 0.026(4) 0.005(3) -0.002(3) -0.002(3) C13C 0.026(3) 0.028(4) 0.018(3) 0.007(3) -0.002(3) -0.004(3) C14C 0.037(4) 0.033(4) 0.027(4) -0.004(3) -0.003(3) -0.011(3) C15C 0.046(5) 0.057(5) 0.043(5) 0.012(4) -0.007(4) -0.028(4) C16C 0.023(4) 0.080(7) 0.045(5) 0.000(4) 0.006(4) -0.017(4) C17C 0.028(5) 0.099(8) 0.039(5) -0.019(5) 0.003(4) 0.004(5) C18C 0.032(4) 0.035(4) 0.035(4) -0.013(3) 0.002(4) -0.006(4) C19C 0.025(4) 0.030(4) 0.019(3) 0.004(3) 0.001(3) -0.002(3) C20C 0.035(4) 0.027(4) 0.021(3) 0.001(3) 0.001(3) 0.003(3) C21C 0.037(4) 0.035(4) 0.025(4) 0.002(3) -0.010(3) -0.006(3) C22C 0.046(4) 0.027(4) 0.038(4) 0.012(3) -0.015(3) 0.003(3) C23C 0.052(5) 0.015(4) 0.046(5) 0.005(3) 0.001(4) 0.008(4) C24C 0.048(5) 0.019(4) 0.030(4) 0.001(3) 0.004(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 N1 2.247(6) 4_655 ? Ce1 N1 2.247(6) 3_565 ? Ce1 N1 2.247(6) . ? Ce1 N1 2.247(6) 2_665 ? N1 C7 1.459(9) . ? N1 C1 1.479(9) . ? C1 C6 1.522(9) . ? C1 C2 1.534(9) . ? C2 C3 1.528(9) . ? C3 C4 1.530(10) . ? C4 C5 1.510(10) . ? C5 C6 1.529(9) . ? C7 C12 1.536(10) . ? C7 C8 1.536(9) . ? C8 C9 1.524(9) . ? C9 C10 1.520(10) . ? C10 C11 1.516(10) . ? C11 C12 1.527(9) . ? Ce1B N1B 2.242(6) 4 ? Ce1B N1B 2.242(6) . ? Ce1B N1B 2.242(6) 2 ? Ce1B N1B 2.242(6) 3 ? N1B C7B 1.465(8) . ? N1B C1B 1.476(8) . ? C1B C6B 1.525(8) . ? C1B C2B 1.547(9) . ? C2B C3B 1.534(9) . ? C3B C4B 1.535(9) . ? C4B C5B 1.529(9) . ? C5B C6B 1.520(8) . ? C7B C12B 1.536(9) . ? C7B C8B 1.544(8) . ? C8B C9B 1.531(9) . ? C9B C10B 1.521(9) . ? C10B C11B 1.511(8) . ? C11B C12B 1.537(8) . ? Ce1C N2C 2.238(5) 2_565 ? Ce1C N2C 2.238(5) . ? Ce1C N1C 2.240(5) . ? Ce1C N1C 2.240(5) 2_565 ? N1C C1C 1.473(7) . ? N1C C7C 1.484(8) . ? N2C C13C 1.483(7) . ? N2C C19C 1.486(8) . ? C1C C6C 1.522(9) . ? C1C C2C 1.539(8) . ? C2C C3C 1.537(8) . ? C3C C4C 1.499(9) . ? C4C C5C 1.520(9) . ? C5C C6C 1.525(10) . ? C7C C12C 1.527(9) . ? C7C C8C 1.540(8) . ? C8C C9C 1.530(8) . ? C9C C10C 1.527(9) . ? C10C C11C 1.543(10) . ? C11C C12C 1.538(9) . ? C13C C18C 1.527(9) . ? C13C C14C 1.530(8) . ? C14C C15C 1.517(9) . ? C15C C16C 1.514(11) . ? C16C C17C 1.511(11) . ? C17C C18C 1.509(10) . ? C19C C20C 1.530(9) . ? C19C C24C 1.535(9) . ? C20C C21C 1.538(8) . ? C21C C22C 1.526(9) . ? C22C C23C 1.553(11) . ? C23C C24C 1.513(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ce1 N1 102.5(3) 4_655 3_565 ? N1 Ce1 N1 113.09(17) 4_655 . ? N1 Ce1 N1 113.09(17) 3_565 . ? N1 Ce1 N1 113.09(17) 4_655 2_665 ? N1 Ce1 N1 113.09(17) 3_565 2_665 ? N1 Ce1 N1 102.5(3) . 2_665 ? C7 N1 C1 115.7(6) . . ? C7 N1 Ce1 106.4(4) . . ? C1 N1 Ce1 137.8(5) . . ? N1 C1 C6 111.4(6) . . ? N1 C1 C2 111.2(6) . . ? C6 C1 C2 110.1(6) . . ? C3 C2 C1 112.7(6) . . ? C2 C3 C4 111.9(6) . . ? C5 C4 C3 109.3(6) . . ? C4 C5 C6 113.0(6) . . ? C1 C6 C5 111.5(6) . . ? N1 C7 C12 115.3(6) . . ? N1 C7 C8 114.3(6) . . ? C12 C7 C8 108.1(6) . . ? C9 C8 C7 113.9(6) . . ? C10 C9 C8 111.6(7) . . ? C11 C10 C9 111.5(6) . . ? C10 C11 C12 110.6(6) . . ? C11 C12 C7 111.2(6) . . ? N1B Ce1B N1B 112.75(17) 4 . ? N1B Ce1B N1B 112.75(17) 4 2 ? N1B Ce1B N1B 103.1(3) . 2 ? N1B Ce1B N1B 103.1(3) 4 3 ? N1B Ce1B N1B 112.75(17) . 3 ? N1B Ce1B N1B 112.75(17) 2 3 ? C7B N1B C1B 115.5(5) . . ? C7B N1B Ce1B 108.2(4) . . ? C1B N1B Ce1B 136.1(4) . . ? N1B C1B C6B 111.6(5) . . ? N1B C1B C2B 111.6(5) . . ? C6B C1B C2B 110.0(5) . . ? C3B C2B C1B 112.5(5) . . ? C2B C3B C4B 111.5(5) . . ? C5B C4B C3B 109.7(5) . . ? C6B C5B C4B 112.8(5) . . ? C5B C6B C1B 112.8(5) . . ? N1B C7B C12B 115.1(5) . . ? N1B C7B C8B 113.9(5) . . ? C12B C7B C8B 109.0(6) . . ? C9B C8B C7B 112.8(5) . . ? C10B C9B C8B 111.3(5) . . ? C11B C10B C9B 111.8(5) . . ? C10B C11B C12B 110.6(5) . . ? C7B C12B C11B 112.2(5) . . ? N2C Ce1C N2C 103.4(3) 2_565 . ? N2C Ce1C N1C 113.41(17) 2_565 . ? N2C Ce1C N1C 111.44(17) . . ? N2C Ce1C N1C 111.44(17) 2_565 2_565 ? N2C Ce1C N1C 113.41(17) . 2_565 ? N1C Ce1C N1C 104.1(3) . 2_565 ? C1C N1C C7C 115.5(5) . . ? C1C N1C Ce1C 135.2(4) . . ? C7C N1C Ce1C 108.8(3) . . ? C13C N2C C19C 115.3(5) . . ? C13C N2C Ce1C 135.2(4) . . ? C19C N2C Ce1C 108.9(4) . . ? N1C C1C C6C 110.8(5) . . ? N1C C1C C2C 111.0(5) . . ? C6C C1C C2C 109.9(5) . . ? C3C C2C C1C 112.7(5) . . ? C4C C3C C2C 111.5(6) . . ? C3C C4C C5C 110.0(6) . . ? C4C C5C C6C 111.7(6) . . ? C5C C6C C1C 111.3(6) . . ? N1C C7C C12C 114.1(5) . . ? N1C C7C C8C 114.2(5) . . ? C12C C7C C8C 110.2(5) . . ? C9C C8C C7C 110.9(5) . . ? C10C C9C C8C 112.3(5) . . ? C9C C10C C11C 110.9(6) . . ? C12C C11C C10C 111.3(6) . . ? C7C C12C C11C 112.4(6) . . ? N2C C13C C18C 109.0(5) . . ? N2C C13C C14C 112.7(5) . . ? C18C C13C C14C 110.1(5) . . ? C15C C14C C13C 111.8(6) . . ? C16C C15C C14C 110.9(6) . . ? C15C C16C C17C 110.3(7) . . ? C18C C17C C16C 111.7(7) . . ? C17C C18C C13C 112.6(6) . . ? N2C C19C C20C 114.9(5) . . ? N2C C19C C24C 114.1(5) . . ? C20C C19C C24C 109.7(6) . . ? C19C C20C C21C 111.5(5) . . ? C22C C21C C20C 110.8(5) . . ? C21C C22C C23C 110.4(5) . . ? C24C C23C C22C 110.2(6) . . ? C23C C24C C19C 113.6(6) . . ? #===END