# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr. Polly L. Arnold' _publ_contact_author_address ; School of Chemistry University of Edinburgh West Mains Road Edinburgh EH9 3JJ ; _publ_section_title ; Tetravalent Sigma-Organometallic Cerium Complexes ; _publ_contact_author_email Polly.Arnold@ed.ac.uk loop_ _publ_author_name I.J.Casely S.T.Liddle A.J.Blake C.Wilson P.L.Arnold data_cenobq_compound_2 _database_code_depnum_ccdc_archive 'CCDC 650969' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H92 Ce N8 O7' _chemical_formula_weight 1081.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 23.188(3) _cell_length_b 11.1458(14) _cell_length_c 24.392(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.709(2) _cell_angle_gamma 90.00 _cell_volume 6213.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3066 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.15 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.333 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.05' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 38792 _diffrn_reflns_av_R_equivalents 0.11 _diffrn_reflns_av_sigmaI/netI 0.1161 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10920 _reflns_number_gt 6660 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _refine_special_details ; Poorly defined THF molecules accounted for using SQUEEZE, within PLATON. 80 electrons per unit cell in void of 646.9 cubic angstroms. Included in unit cell contents as 2 molecules of THF. Further molecules of thf included explicitly in model. One 0.5 occupied and 2 further sites show disorder. O804 modelled over 2 sites with occupancies 0.70 and 0.30. A second molecule has both the oxygen and some carbon atoms over 2 partially occupied sites 0.6/0.4. Distance and adp restraints applied. ; _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^)+(0.1019P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10920 _refine_ls_number_parameters 640 _refine_ls_number_restraints 222 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1616 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.499896(16) 0.17555(3) 0.763322(16) 0.02802(14) Uani 1 1 d . . . C1 C 0.5949(3) 0.3190(6) 0.7749(3) 0.0342(16) Uani 1 1 d . . . N1 N 0.5953(2) 0.4197(5) 0.7442(2) 0.0352(14) Uani 1 1 d . . . O1 O 0.48417(19) 0.3036(4) 0.69733(19) 0.0365(12) Uani 1 1 d . . . C2 C 0.6741(3) 0.2003(6) 0.8323(3) 0.0424(19) Uani 1 1 d . . . H20I H 0.6403 0.1474 0.8366 0.051 Uiso 1 1 calc R . . N2 N 0.6521(2) 0.2951(5) 0.7920(2) 0.0359(14) Uani 1 1 d . . . O2 O 0.52244(19) 0.1156(4) 0.84785(18) 0.0339(11) Uani 1 1 d . . . C3 C 0.6969(4) 0.2546(8) 0.8881(3) 0.053(2) Uani 1 1 d . . . H20F H 0.6661 0.3027 0.9003 0.080 Uiso 1 1 calc R . . H20G H 0.7306 0.3060 0.8852 0.080 Uiso 1 1 calc R . . H20H H 0.7090 0.1906 0.9151 0.080 Uiso 1 1 calc R . . N3 N 0.4646(3) 0.3281(5) 0.8831(2) 0.0386(14) Uani 1 1 d . . . O3 O 0.41672(19) 0.0905(4) 0.74375(19) 0.0369(12) Uani 1 1 d . . . C4 C 0.7193(4) 0.1239(7) 0.8121(4) 0.054(2) Uani 1 1 d . . . H20C H 0.7028 0.0884 0.7762 0.080 Uiso 1 1 calc R . . H20D H 0.7316 0.0599 0.8391 0.080 Uiso 1 1 calc R . . H20E H 0.7532 0.1735 0.8079 0.080 Uiso 1 1 calc R . . N4 N 0.3988(2) 0.3868(5) 0.8167(2) 0.0353(14) Uani 1 1 d . . . O4 O 0.5508(2) 0.0480(4) 0.7274(2) 0.0404(12) Uani 1 1 d . . . C5 C 0.6868(4) 0.3781(7) 0.7727(3) 0.048(2) Uani 1 1 d . . . H20A H 0.7284 0.3788 0.7795 0.058 Uiso 1 1 calc R . . N5 N 0.3210(3) 0.0701(5) 0.6511(2) 0.0391(15) Uani 1 1 d . . . C6 C 0.6525(3) 0.4578(7) 0.7428(3) 0.0422(19) Uani 1 1 d . . . H20B H 0.6643 0.5263 0.7244 0.051 Uiso 1 1 calc R . . N6 N 0.2566(3) 0.1760(6) 0.6013(3) 0.0450(15) Uani 1 1 d . . . C7 C 0.5433(3) 0.4808(6) 0.7152(3) 0.0413(18) Uani 1 1 d . . . H20J H 0.5553 0.5543 0.6973 0.050 Uiso 1 1 calc R . . H20K H 0.5185 0.5054 0.7425 0.050 Uiso 1 1 calc R . . N7 N 0.6159(3) -0.1670(5) 0.7657(3) 0.0387(14) Uani 1 1 d . . . C8 C 0.5070(3) 0.4002(6) 0.6702(3) 0.0379(17) Uani 1 1 d . . . N8 N 0.6918(3) -0.2199(5) 0.8225(3) 0.0422(15) Uani 1 1 d . . . C9 C 0.5430(4) 0.3532(7) 0.6280(3) 0.048(2) Uani 1 1 d . . . H21D H 0.5752 0.3038 0.6471 0.073 Uiso 1 1 calc R . . H21E H 0.5590 0.4210 0.6098 0.073 Uiso 1 1 calc R . . H21F H 0.5181 0.3047 0.6000 0.073 Uiso 1 1 calc R . . C10 C 0.4561(3) 0.4785(7) 0.6394(3) 0.056(2) Uani 1 1 d . . . H21A H 0.4326 0.5091 0.6662 0.084 Uiso 1 1 calc R . . H21B H 0.4313 0.4297 0.6114 0.084 Uiso 1 1 calc R . . H21C H 0.4722 0.5460 0.6211 0.084 Uiso 1 1 calc R . . C11 C 0.4517(3) 0.3289(6) 0.8257(3) 0.0330(15) Uani 1 1 d . . . C12 C 0.3674(3) 0.4150(7) 0.7617(3) 0.0397(18) Uani 1 1 d . . . H30I H 0.3900 0.3819 0.7337 0.048 Uiso 1 1 calc R . . C13 C 0.3081(4) 0.3565(8) 0.7527(4) 0.066(3) Uani 1 1 d . . . H30F H 0.3127 0.2696 0.7577 0.100 Uiso 1 1 calc R . . H30G H 0.2879 0.3737 0.7149 0.100 Uiso 1 1 calc R . . H30H H 0.2851 0.3882 0.7797 0.100 Uiso 1 1 calc R . . C14 C 0.3620(4) 0.5505(8) 0.7533(4) 0.069(3) Uani 1 1 d . . . H30C H 0.4011 0.5864 0.7587 0.103 Uiso 1 1 calc R . . H30D H 0.3397 0.5846 0.7803 0.103 Uiso 1 1 calc R . . H30E H 0.3417 0.5676 0.7155 0.103 Uiso 1 1 calc R . . C15 C 0.3803(3) 0.4191(7) 0.8649(3) 0.046(2) Uani 1 1 d . . . H30A H 0.3452 0.4607 0.8679 0.055 Uiso 1 1 calc R . . C16 C 0.4217(4) 0.3806(7) 0.9080(3) 0.047(2) Uani 1 1 d . . . H30B H 0.4210 0.3884 0.9467 0.057 Uiso 1 1 calc R . . C17 C 0.5167(3) 0.2696(7) 0.9145(3) 0.0432(19) Uani 1 1 d . . . H30J H 0.5180 0.2845 0.9547 0.052 Uiso 1 1 calc R . . H30K H 0.5521 0.3061 0.9037 0.052 Uiso 1 1 calc R . . C18 C 0.5180(3) 0.1337(7) 0.9045(3) 0.0380(18) Uani 1 1 d . . . C19 C 0.5721(3) 0.0821(7) 0.9423(3) 0.049(2) Uani 1 1 d . . . H31A H 0.6074 0.1218 0.9341 0.074 Uiso 1 1 calc R . . H31B H 0.5747 -0.0043 0.9357 0.074 Uiso 1 1 calc R . . H31C H 0.5688 0.0960 0.9814 0.074 Uiso 1 1 calc R . . C20 C 0.4617(3) 0.0730(7) 0.9168(3) 0.045(2) Uani 1 1 d . . . H31D H 0.4277 0.1073 0.8926 0.068 Uiso 1 1 calc R . . H31E H 0.4582 0.0867 0.9558 0.068 Uiso 1 1 calc R . . H31F H 0.4636 -0.0134 0.9099 0.068 Uiso 1 1 calc R . . C21 C 0.2614(3) 0.0717(8) 0.6298(3) 0.047(2) Uani 1 1 d . . . C22 C 0.2006(4) 0.2206(9) 0.5691(4) 0.064(3) Uani 1 1 d . . . H40J H 0.2109 0.2914 0.5475 0.077 Uiso 1 1 calc R . . C23 C 0.1614(4) 0.2656(10) 0.6051(4) 0.074(3) Uani 1 1 d . . . H40G H 0.1818 0.3257 0.6306 0.111 Uiso 1 1 calc R . . H40H H 0.1489 0.1990 0.6266 0.111 Uiso 1 1 calc R . . H40I H 0.1270 0.3023 0.5824 0.111 Uiso 1 1 calc R . . C24 C 0.1747(4) 0.1305(9) 0.5273(4) 0.074(3) Uani 1 1 d . . . H40D H 0.1384 0.1625 0.5059 0.110 Uiso 1 1 calc R . . H40E H 0.1661 0.0569 0.5464 0.110 Uiso 1 1 calc R . . H40F H 0.2024 0.1128 0.5022 0.110 Uiso 1 1 calc R . . C25 C 0.3089(4) 0.2387(8) 0.6045(3) 0.052(2) Uani 1 1 d . . . H40B H 0.3151 0.3135 0.5878 0.062 Uiso 1 1 calc R . . C26 C 0.3488(3) 0.1697(7) 0.6367(3) 0.0451(19) Uani 1 1 d . . . H40C H 0.3892 0.1876 0.6473 0.054 Uiso 1 1 calc R . . C27 C 0.3500(3) -0.0311(6) 0.6827(3) 0.0385(17) Uani 1 1 d . . . H40K H 0.3811 -0.0614 0.6631 0.046 Uiso 1 1 calc R . . H40L H 0.3210 -0.0963 0.6828 0.046 Uiso 1 1 calc R . . C28 C 0.3772(3) -0.0043(6) 0.7426(3) 0.0344(17) Uani 1 1 d . . . C29 C 0.3294(3) 0.0252(7) 0.7761(3) 0.051(2) Uani 1 1 d . . . H41D H 0.3088 0.0981 0.7613 0.076 Uiso 1 1 calc R . . H41E H 0.3469 0.0382 0.8151 0.076 Uiso 1 1 calc R . . H41F H 0.3016 -0.0416 0.7737 0.076 Uiso 1 1 calc R . . C30 C 0.4100(4) -0.1176(7) 0.7669(4) 0.056(2) Uani 1 1 d . . . H41A H 0.4279 -0.1025 0.8056 0.084 Uiso 1 1 calc R . . H41B H 0.4405 -0.1377 0.7451 0.084 Uiso 1 1 calc R . . H41C H 0.3824 -0.1845 0.7655 0.084 Uiso 1 1 calc R . . C31 C 0.6673(3) -0.2308(7) 0.7670(3) 0.0448(19) Uani 1 1 d . . . C32 C 0.7471(4) -0.2808(8) 0.8462(3) 0.052(2) Uani 1 1 d . . . H50J H 0.7651 -0.3124 0.8146 0.063 Uiso 1 1 calc R . . C33 C 0.7896(4) -0.1909(8) 0.8781(4) 0.063(3) Uani 1 1 d . . . H50G H 0.7967 -0.1256 0.8532 0.094 Uiso 1 1 calc R . . H50H H 0.8266 -0.2312 0.8924 0.094 Uiso 1 1 calc R . . H50I H 0.7728 -0.1581 0.9092 0.094 Uiso 1 1 calc R . . C34 C 0.7346(4) -0.3851(7) 0.8808(4) 0.061(2) Uani 1 1 d . . . H50D H 0.7073 -0.4399 0.8580 0.092 Uiso 1 1 calc R . . H50E H 0.7170 -0.3564 0.9122 0.092 Uiso 1 1 calc R . . H50F H 0.7711 -0.4275 0.8948 0.092 Uiso 1 1 calc R . . C35 C 0.6575(3) -0.1539(6) 0.8527(3) 0.0428(19) Uani 1 1 d . . . H50B H 0.6663 -0.1352 0.8912 0.051 Uiso 1 1 calc R . . C36 C 0.6096(3) -0.1214(6) 0.8172(3) 0.0392(18) Uani 1 1 d . . . H50C H 0.5775 -0.0761 0.8256 0.047 Uiso 1 1 calc R . . C37 C 0.5726(3) -0.1575(6) 0.7155(3) 0.0394(18) Uani 1 1 d . . . H50K H 0.5340 -0.1803 0.7245 0.047 Uiso 1 1 calc R . . H50L H 0.5825 -0.2161 0.6880 0.047 Uiso 1 1 calc R . . C38 C 0.5674(3) -0.0334(6) 0.6887(3) 0.0350(16) Uani 1 1 d . . . C39 C 0.6255(3) 0.0052(7) 0.6726(3) 0.0454(19) Uani 1 1 d . . . H51D H 0.6557 0.0082 0.7059 0.068 Uiso 1 1 calc R . . H51E H 0.6211 0.0849 0.6553 0.068 Uiso 1 1 calc R . . H51F H 0.6370 -0.0526 0.6461 0.068 Uiso 1 1 calc R . . C40 C 0.5174(3) -0.0383(8) 0.6376(3) 0.054(2) Uani 1 1 d . . . H51A H 0.4810 -0.0636 0.6496 0.081 Uiso 1 1 calc R . . H51B H 0.5276 -0.0959 0.6104 0.081 Uiso 1 1 calc R . . H51C H 0.5120 0.0413 0.6205 0.081 Uiso 1 1 calc R . . C101 C 0.6575(9) 0.0941(18) 0.4747(8) 0.084(4) Uani 0.50 1 d PDU . . H10A H 0.6947 0.1123 0.4998 0.101 Uiso 0.50 1 calc PR . . H10B H 0.6663 0.0407 0.4448 0.101 Uiso 0.50 1 calc PR . . C102 C 0.6182(8) 0.0348(18) 0.5054(9) 0.096(4) Uani 0.50 1 d PDU . . H10C H 0.6026 -0.0394 0.4860 0.116 Uiso 0.50 1 calc PR . . H10D H 0.6387 0.0131 0.5430 0.116 Uiso 0.50 1 calc PR . . O103 O 0.5726(6) 0.1158(13) 0.5089(6) 0.089(3) Uani 0.50 1 d PDU . . C104 C 0.5853(8) 0.2215(15) 0.4819(8) 0.083(4) Uani 0.50 1 d PDU . . H10E H 0.5966 0.2854 0.5099 0.099 Uiso 0.50 1 calc PR . . H10F H 0.5499 0.2486 0.4564 0.099 Uiso 0.50 1 calc PR . . C105 C 0.6318(8) 0.2032(18) 0.4510(8) 0.088(4) Uani 0.50 1 d PDU . . H10G H 0.6602 0.2702 0.4564 0.106 Uiso 0.50 1 calc PR . . H10H H 0.6166 0.1937 0.4108 0.106 Uiso 0.50 1 calc PR . . C701 C 0.5748(4) 0.6642(11) 0.5846(5) 0.106(3) Uani 0.60 1 d PDU A 1 H70A H 0.5612 0.6002 0.6076 0.128 Uiso 0.60 1 calc PR A 1 H70B H 0.5584 0.7425 0.5936 0.128 Uiso 0.60 1 calc PR A 1 C702 C 0.6376(4) 0.6670(13) 0.5896(6) 0.118(3) Uani 0.60 1 d PDU A 1 H70C H 0.6508 0.7498 0.5995 0.142 Uiso 0.60 1 calc PR A 1 H70D H 0.6542 0.6146 0.6210 0.142 Uiso 0.60 1 calc PR A 1 O703 O 0.6620(6) 0.6316(15) 0.5424(6) 0.129(4) Uani 0.60 1 d PDU A 1 C704 C 0.6125(7) 0.5688(19) 0.5156(10) 0.128(4) Uani 0.60 1 d PDU A 1 H70E H 0.6116 0.4867 0.5308 0.154 Uiso 0.60 1 calc PR A 1 H70F H 0.6127 0.5633 0.4751 0.154 Uiso 0.60 1 calc PR A 1 C705 C 0.5622(6) 0.6374(13) 0.5263(5) 0.120(3) Uani 0.60 1 d PDU A 1 H70G H 0.5577 0.7121 0.5040 0.145 Uiso 0.60 1 calc PR A 1 H70H H 0.5258 0.5897 0.5172 0.145 Uiso 0.60 1 calc PR A 1 C711 C 0.5748(4) 0.6642(11) 0.5846(5) 0.106(3) Uani 0.40 1 d PDU B 2 H71A H 0.5612 0.6002 0.6076 0.128 Uiso 0.40 1 calc PR B 2 H71B H 0.5584 0.7425 0.5936 0.128 Uiso 0.40 1 calc PR B 2 C712 C 0.6376(4) 0.6670(13) 0.5896(6) 0.118(3) Uani 0.40 1 d PDU B 2 H71G H 0.6535 0.5853 0.5865 0.142 Uiso 0.40 1 calc PR B 2 H71H H 0.6558 0.7024 0.6256 0.142 Uiso 0.40 1 calc PR B 2 O713 O 0.6495(9) 0.754(2) 0.5360(9) 0.118(4) Uani 0.40 1 d PDU B 2 C714 C 0.5905(10) 0.743(2) 0.5099(13) 0.116(4) Uani 0.40 1 d PDU B 2 H71C H 0.5889 0.7422 0.4691 0.140 Uiso 0.40 1 calc PR B 2 H71D H 0.5687 0.8151 0.5191 0.140 Uiso 0.40 1 calc PR B 2 C715 C 0.5622(6) 0.6374(13) 0.5263(5) 0.120(3) Uani 0.40 1 d PDU B 2 H71E H 0.5197 0.6357 0.5115 0.145 Uiso 0.40 1 calc PR B 2 H71F H 0.5809 0.5623 0.5166 0.145 Uiso 0.40 1 calc PR B 2 C801 C 0.5070(4) 0.6541(8) 0.8651(4) 0.070(3) Uani 1 1 d D D . H80A H 0.5070 0.7261 0.8414 0.084 Uiso 1 1 calc R . . H80B H 0.4727 0.6040 0.8502 0.084 Uiso 1 1 calc R . . C802 C 0.5610(4) 0.5864(7) 0.8672(3) 0.056(2) Uani 1 1 d D D . H80C H 0.5870 0.6253 0.8442 0.067 Uiso 1 1 calc R . . H80D H 0.5527 0.5034 0.8537 0.067 Uiso 1 1 calc R . . C803 C 0.5880(5) 0.5866(9) 0.9259(4) 0.080(3) Uani 1 1 d D . . H80E H 0.6072 0.5086 0.9364 0.095 Uiso 0.70 1 calc PR C 1 H80F H 0.6177 0.6509 0.9334 0.095 Uiso 0.70 1 calc PR C 1 H81E H 0.6309 0.5972 0.9295 0.095 Uiso 0.30 1 d PR C 2 H81F H 0.5804 0.5093 0.9434 0.095 Uiso 0.30 1 d PR C 2 O804 O 0.5431(5) 0.6064(12) 0.9554(4) 0.106(4) Uani 0.70 1 d PD D 1 O814 O 0.5619(6) 0.6877(16) 0.9543(7) 0.051(5) Uani 0.30 1 d PD D 2 C805 C 0.5056(5) 0.6882(13) 0.9223(5) 0.143(7) Uani 1 1 d D . . H80G H 0.5196 0.7715 0.9293 0.171 Uiso 0.70 1 calc PR D 1 H80H H 0.4653 0.6823 0.9305 0.171 Uiso 0.70 1 calc PR D 1 H81G H 0.4886 0.7696 0.9228 0.171 Uiso 0.30 1 d PR D 2 H81H H 0.4802 0.6321 0.9388 0.171 Uiso 0.30 1 d PR D 2 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 0.0203(2) 0.0293(2) 0.0334(2) 0.00278(19) 0.00166(13) -0.00064(19) C1 0.031(4) 0.031(4) 0.043(4) -0.007(3) 0.011(3) -0.006(3) N1 0.029(3) 0.027(3) 0.048(4) 0.003(3) 0.004(3) 0.000(3) O1 0.024(3) 0.041(3) 0.044(3) 0.009(2) 0.005(2) 0.001(2) C2 0.025(4) 0.040(5) 0.058(5) 0.005(4) -0.004(3) -0.004(3) N2 0.022(3) 0.037(4) 0.049(4) 0.003(3) 0.005(3) -0.008(2) O2 0.029(3) 0.039(3) 0.032(3) 0.004(2) 0.003(2) 0.003(2) C3 0.049(5) 0.064(6) 0.044(5) 0.003(4) -0.002(4) 0.003(4) N3 0.033(3) 0.038(3) 0.043(4) -0.002(3) -0.001(3) 0.004(3) O3 0.028(3) 0.041(3) 0.040(3) 0.004(2) 0.000(2) -0.004(2) C4 0.043(5) 0.044(5) 0.075(6) -0.002(4) 0.015(4) 0.005(4) N4 0.029(3) 0.037(3) 0.039(4) -0.001(3) 0.001(3) 0.008(3) O4 0.037(3) 0.039(3) 0.044(3) -0.006(2) 0.004(2) 0.001(2) C5 0.038(5) 0.045(5) 0.062(6) 0.004(4) 0.010(4) -0.015(4) N5 0.029(3) 0.043(4) 0.043(4) 0.000(3) 0.000(3) -0.005(3) C6 0.043(5) 0.044(4) 0.042(4) -0.003(4) 0.011(4) -0.017(4) N6 0.034(4) 0.051(4) 0.047(4) 0.004(3) -0.002(3) 0.005(3) C7 0.039(5) 0.027(4) 0.058(5) 0.006(3) 0.009(4) 0.006(3) N7 0.033(3) 0.033(3) 0.052(4) -0.002(3) 0.010(3) 0.004(3) C8 0.034(4) 0.040(4) 0.040(4) 0.012(3) 0.008(3) 0.006(3) N8 0.042(4) 0.036(3) 0.051(4) 0.004(3) 0.015(3) 0.009(3) C9 0.050(5) 0.050(5) 0.047(5) 0.012(4) 0.016(4) 0.002(4) C10 0.046(5) 0.062(6) 0.060(6) 0.029(4) 0.009(4) 0.012(4) C11 0.030(4) 0.037(4) 0.032(4) -0.002(3) 0.004(3) -0.006(3) C12 0.024(4) 0.049(5) 0.044(5) -0.004(4) 0.000(3) 0.012(3) C13 0.047(6) 0.085(7) 0.059(6) -0.003(5) -0.015(4) -0.002(5) C14 0.082(7) 0.055(6) 0.063(6) 0.007(5) -0.004(5) 0.010(5) C15 0.037(5) 0.050(5) 0.054(5) -0.003(4) 0.014(4) 0.009(4) C16 0.050(5) 0.052(5) 0.041(5) -0.009(4) 0.013(4) 0.009(4) C17 0.042(5) 0.048(4) 0.035(4) 0.001(4) -0.005(3) -0.001(4) C18 0.027(4) 0.048(4) 0.038(4) 0.011(3) 0.003(3) 0.000(3) C19 0.042(5) 0.058(5) 0.043(5) 0.010(4) -0.007(4) 0.008(4) C20 0.039(5) 0.061(5) 0.038(4) 0.012(4) 0.013(4) -0.009(4) C21 0.026(4) 0.064(5) 0.046(5) -0.007(4) -0.004(3) 0.008(4) C22 0.053(6) 0.072(6) 0.059(6) -0.001(5) -0.015(5) 0.015(5) C23 0.051(6) 0.102(8) 0.067(7) -0.003(6) 0.005(5) 0.022(6) C24 0.052(6) 0.114(8) 0.048(5) 0.000(5) -0.014(5) -0.005(6) C25 0.048(5) 0.063(6) 0.040(5) 0.009(4) -0.002(4) -0.014(4) C26 0.031(4) 0.053(5) 0.048(5) 0.009(4) 0.000(3) -0.002(4) C27 0.034(4) 0.035(4) 0.045(4) -0.002(3) 0.000(3) 0.005(3) C28 0.023(4) 0.036(4) 0.043(4) 0.000(3) 0.000(3) -0.008(3) C29 0.035(5) 0.065(5) 0.050(5) 0.003(4) 0.002(4) -0.003(4) C30 0.042(5) 0.049(5) 0.072(6) 0.020(4) -0.006(4) -0.003(4) C31 0.038(5) 0.035(4) 0.058(5) 0.004(4) -0.001(4) 0.003(4) C32 0.044(5) 0.061(5) 0.051(5) 0.009(4) 0.008(4) 0.026(4) C33 0.040(5) 0.076(7) 0.071(6) 0.021(5) 0.005(4) 0.009(5) C34 0.047(5) 0.051(5) 0.081(7) 0.012(5) -0.003(5) 0.016(4) C35 0.042(5) 0.040(5) 0.049(5) 0.002(3) 0.015(4) 0.005(3) C36 0.040(5) 0.032(4) 0.050(5) 0.005(3) 0.020(4) 0.005(3) C37 0.033(4) 0.036(4) 0.050(5) -0.004(3) 0.011(3) 0.001(3) C38 0.031(4) 0.036(4) 0.041(4) -0.004(3) 0.013(3) 0.001(3) C39 0.036(5) 0.048(5) 0.053(5) 0.002(4) 0.011(4) -0.002(4) C40 0.043(5) 0.073(6) 0.040(5) -0.006(4) -0.006(4) -0.006(4) C101 0.074(9) 0.123(10) 0.055(8) -0.033(7) 0.009(7) -0.015(7) C102 0.090(9) 0.116(10) 0.082(9) -0.009(7) 0.010(7) -0.008(7) O103 0.079(8) 0.115(9) 0.075(7) -0.010(7) 0.016(6) -0.017(6) C104 0.074(9) 0.099(9) 0.073(9) -0.026(7) 0.007(7) -0.031(7) C105 0.079(9) 0.112(10) 0.074(9) -0.027(7) 0.013(7) -0.044(7) C701 0.068(5) 0.126(7) 0.116(6) -0.024(5) -0.010(5) 0.006(5) C702 0.081(5) 0.145(7) 0.120(6) -0.026(5) -0.010(5) 0.016(6) O703 0.093(6) 0.153(8) 0.131(8) -0.045(7) -0.012(6) 0.030(7) C704 0.099(8) 0.145(9) 0.132(8) -0.037(7) -0.005(7) 0.008(7) C705 0.083(5) 0.137(7) 0.128(6) -0.013(6) -0.019(5) -0.002(5) C711 0.068(5) 0.126(7) 0.116(6) -0.024(5) -0.010(5) 0.006(5) C712 0.081(5) 0.145(7) 0.120(6) -0.026(5) -0.010(5) 0.016(6) O713 0.078(7) 0.143(9) 0.125(8) -0.018(8) -0.010(7) 0.004(7) C714 0.076(8) 0.136(9) 0.125(8) -0.011(8) -0.018(7) -0.003(8) C715 0.083(5) 0.137(7) 0.128(6) -0.013(6) -0.019(5) -0.002(5) C801 0.050(6) 0.081(7) 0.070(7) 0.022(5) -0.018(5) -0.012(5) C802 0.065(6) 0.047(5) 0.055(6) -0.005(4) 0.006(5) -0.004(4) C803 0.085(8) 0.066(7) 0.077(8) -0.008(6) -0.017(6) 0.019(6) O804 0.068(8) 0.205(15) 0.040(6) 0.003(8) -0.002(5) -0.034(9) O814 0.052(13) 0.052(12) 0.045(11) -0.016(9) 0.001(9) -0.042(10) C805 0.075(9) 0.211(16) 0.124(12) -0.083(11) -0.033(8) 0.064(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O4 2.128(5) . ? Ce1 O3 2.130(4) . ? Ce1 O1 2.136(4) . ? Ce1 O2 2.146(4) . ? Ce1 C11 2.656(7) . ? Ce1 C1 2.697(7) . ? C1 N2 1.350(8) . ? C1 N1 1.350(8) . ? N1 C6 1.399(9) . ? N1 C7 1.462(8) . ? O1 C8 1.412(8) . ? C2 N2 1.474(9) . ? C2 C4 1.497(10) . ? C2 C3 1.501(10) . ? N2 C5 1.361(9) . ? O2 C18 1.417(8) . ? N3 C16 1.381(9) . ? N3 C11 1.384(8) . ? N3 C17 1.469(9) . ? O3 C28 1.396(8) . ? N4 C15 1.366(9) . ? N4 C11 1.371(8) . ? N4 C12 1.448(9) . ? O4 C38 1.410(8) . ? C5 C6 1.325(10) . ? N5 C26 1.359(9) . ? N5 C21 1.392(8) . ? N5 C27 1.465(8) . ? N6 C21 1.349(10) . ? N6 C25 1.389(10) . ? N6 C22 1.486(10) . ? C7 C8 1.551(10) . ? N7 C31 1.383(9) . ? N7 C36 1.385(9) . ? N7 C37 1.449(9) . ? C8 C9 1.525(10) . ? C8 C10 1.556(9) . ? N8 C35 1.382(9) . ? N8 C31 1.383(9) . ? N8 C32 1.478(9) . ? C12 C13 1.503(11) . ? C12 C14 1.527(10) . ? C15 C16 1.367(10) . ? C17 C18 1.535(10) . ? C18 C19 1.539(9) . ? C18 C20 1.544(9) . ? C22 C23 1.456(12) . ? C22 C24 1.483(12) . ? C25 C26 1.348(10) . ? C27 C28 1.518(9) . ? C28 C29 1.521(10) . ? C28 C30 1.540(9) . ? C32 C34 1.494(11) . ? C32 C33 1.524(11) . ? C35 C36 1.339(10) . ? C37 C38 1.526(9) . ? C38 C39 1.528(10) . ? C38 C40 1.556(9) . ? C101 C105 1.432(9) . ? C101 C102 1.434(9) . ? C102 O103 1.406(10) . ? O103 C104 1.406(10) . ? C104 C105 1.430(9) . ? C701 C705 1.435(7) . ? C701 C702 1.441(7) . ? C702 O703 1.422(8) . ? O703 C704 1.409(10) . ? C704 C705 1.455(9) . ? O713 C714 1.412(10) . ? C801 C805 1.450(8) . ? C801 C802 1.457(7) . ? C802 C803 1.463(7) . ? C803 O804 1.380(9) . ? C803 O814 1.50(2) . ? O804 C805 1.416(9) . ? O814 C805 1.404(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 O4 Ce1 O3 98.89(18) . . ? O4 Ce1 O1 99.93(18) . . ? O3 Ce1 O1 95.49(17) . . ? O4 Ce1 O2 97.19(18) . . ? O3 Ce1 O2 98.13(17) . . ? O1 Ce1 O2 156.16(18) . . ? O4 Ce1 C11 168.93(19) . . ? O3 Ce1 C11 87.83(19) . . ? O1 Ce1 C11 88.09(19) . . ? O2 Ce1 C11 73.03(19) . . ? O4 Ce1 C1 86.5(2) . . ? O3 Ce1 C1 168.47(19) . . ? O1 Ce1 C1 73.47(19) . . ? O2 Ce1 C1 91.2(2) . . ? C11 Ce1 C1 88.5(2) . . ? N2 C1 N1 103.6(6) . . ? N2 C1 Ce1 131.2(5) . . ? N1 C1 Ce1 121.2(5) . . ? C1 N1 C6 111.2(6) . . ? C1 N1 C7 125.0(6) . . ? C6 N1 C7 123.7(6) . . ? C8 O1 Ce1 146.3(4) . . ? N2 C2 C4 111.7(7) . . ? N2 C2 C3 110.2(6) . . ? C4 C2 C3 111.5(6) . . ? C1 N2 C5 111.6(6) . . ? C1 N2 C2 123.9(6) . . ? C5 N2 C2 124.0(6) . . ? C18 O2 Ce1 147.8(4) . . ? C16 N3 C11 113.2(6) . . ? C16 N3 C17 123.4(6) . . ? C11 N3 C17 123.3(6) . . ? C28 O3 Ce1 155.3(4) . . ? C15 N4 C11 112.9(6) . . ? C15 N4 C12 123.9(6) . . ? C11 N4 C12 123.2(6) . . ? C38 O4 Ce1 159.9(4) . . ? C6 C5 N2 108.1(7) . . ? C26 N5 C21 112.1(6) . . ? C26 N5 C27 124.8(6) . . ? C21 N5 C27 123.0(6) . . ? C5 C6 N1 105.5(7) . . ? C21 N6 C25 114.2(6) . . ? C21 N6 C22 123.3(7) . . ? C25 N6 C22 122.5(7) . . ? N1 C7 C8 112.2(6) . . ? C31 N7 C36 112.9(6) . . ? C31 N7 C37 121.9(6) . . ? C36 N7 C37 125.0(6) . . ? O1 C8 C9 110.2(6) . . ? O1 C8 C7 108.2(6) . . ? C9 C8 C7 112.5(6) . . ? O1 C8 C10 109.9(6) . . ? C9 C8 C10 108.9(6) . . ? C7 C8 C10 107.1(6) . . ? C35 N8 C31 112.9(6) . . ? C35 N8 C32 125.1(7) . . ? C31 N8 C32 121.9(6) . . ? N4 C11 N3 101.6(6) . . ? N4 C11 Ce1 131.5(5) . . ? N3 C11 Ce1 122.4(5) . . ? N4 C12 C13 110.3(7) . . ? N4 C12 C14 110.9(6) . . ? C13 C12 C14 110.9(7) . . ? N4 C15 C16 107.4(7) . . ? C15 C16 N3 105.0(7) . . ? N3 C17 C18 113.1(6) . . ? O2 C18 C17 107.6(5) . . ? O2 C18 C19 110.2(6) . . ? C17 C18 C19 108.0(6) . . ? O2 C18 C20 109.3(6) . . ? C17 C18 C20 111.2(6) . . ? C19 C18 C20 110.5(6) . . ? N6 C21 N5 101.1(6) . . ? C23 C22 C24 115.1(9) . . ? C23 C22 N6 112.0(7) . . ? C24 C22 N6 110.7(7) . . ? C26 C25 N6 104.6(7) . . ? C25 C26 N5 107.9(7) . . ? N5 C27 C28 115.8(6) . . ? O3 C28 C27 109.4(6) . . ? O3 C28 C29 111.1(6) . . ? C27 C28 C29 109.7(6) . . ? O3 C28 C30 109.4(6) . . ? C27 C28 C30 107.9(6) . . ? C29 C28 C30 109.1(6) . . ? N8 C31 N7 100.9(7) . . ? N8 C32 C34 109.8(7) . . ? N8 C32 C33 110.0(7) . . ? C34 C32 C33 113.2(7) . . ? C36 C35 N8 106.8(7) . . ? C35 C36 N7 106.5(6) . . ? N7 C37 C38 114.9(6) . . ? O4 C38 C37 107.9(6) . . ? O4 C38 C39 110.1(6) . . ? C37 C38 C39 110.9(6) . . ? O4 C38 C40 108.0(6) . . ? C37 C38 C40 107.8(6) . . ? C39 C38 C40 112.0(6) . . ? C105 C101 C102 110.1(17) . . ? O103 C102 C101 106.7(16) . . ? C102 O103 C104 106.8(15) . . ? O103 C104 C105 111.4(16) . . ? C104 C105 C101 102.0(17) . . ? C705 C701 C702 97.0(10) . . ? O703 C702 C701 117.5(11) . . ? C704 O703 C702 96.2(14) . . ? O703 C704 C705 105.8(13) . . ? C701 C705 C704 104.6(13) . . ? C805 C801 C802 105.1(7) . . ? C801 C802 C803 104.9(7) . . ? O804 C803 C802 106.0(8) . . ? C802 C803 O814 108.2(8) . . ? C803 O804 C805 104.5(9) . . ? C805 O814 C803 99.0(10) . . ? O814 C805 C801 111.3(11) . . ? O804 C805 C801 105.6(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.175 _refine_diff_density_min -1.644 _refine_diff_density_rms 0.131 #===END of CIF data_cenbbn_compound_3 _database_code_depnum_ccdc_archive 'CCDC 650970' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H116 B2 Ce N8 O4' _chemical_formula_sum 'C74 H116 B2 Ce N8 O4' _chemical_formula_weight 1343.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6344(5) _cell_length_b 15.6439(6) _cell_length_c 19.9007(7) _cell_angle_alpha 78.468(2) _cell_angle_beta 74.110(2) _cell_angle_gamma 66.660(2) _cell_volume 3728.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18536 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.661 #scaled 0.833 _exptl_absorpt_correction_T_max 0.793 # scaled 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, v2.05)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 34250 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.52 _reflns_number_total 16851 _reflns_number_gt 15594 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.2004);PLATON(Spek2003)' _refine_special_details ; Restraints to bond lengths and displacement parameters applied to benzene molecules 100 and 200. ; _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^)+(0.0503P)^2^+0.7231P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me & HB from difmap' _refine_ls_hydrogen_treatment 'constr, HB refall' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16848 _refine_ls_number_parameters 826 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.449214(7) 1.010882(6) 1.255204(5) 0.02047(4) Uani 1 1 d . . . C1 C 0.31227(17) 0.97611(14) 1.19771(11) 0.0316(4) Uani 1 1 d . . . C2 C 0.4094(2) 0.81156(16) 1.16664(14) 0.0461(6) Uani 1 1 d . . . H2 H 0.4630 0.8139 1.1913 0.055 Uiso 1 1 calc R . . C3 C 0.3614(3) 0.7388(2) 1.20832(18) 0.0726(10) Uani 1 1 d . . . H3A H 0.3234 0.7572 1.2556 0.109 Uiso 1 1 calc R . . H3B H 0.4204 0.6777 1.2116 0.109 Uiso 1 1 calc R . . H3C H 0.3095 0.7348 1.1845 0.109 Uiso 1 1 calc R . . C4 C 0.4693(2) 0.7859(2) 1.09294(16) 0.0586(7) Uani 1 1 d . . . H4A H 0.4199 0.7771 1.0695 0.088 Uiso 1 1 calc R . . H4B H 0.5328 0.7278 1.0954 0.088 Uiso 1 1 calc R . . H4C H 0.4939 0.8363 1.0663 0.088 Uiso 1 1 calc R . . C5 C 0.2383(2) 0.92663(19) 1.13043(12) 0.0443(5) Uani 1 1 d . . . H5 H 0.2282 0.8873 1.1043 0.053 Uiso 1 1 calc R . . C6 C 0.17455(19) 1.0147(2) 1.14123(12) 0.0478(6) Uani 1 1 d . . . H6 H 0.1100 1.0505 1.1241 0.057 Uiso 1 1 calc R . . C7 C 0.17369(18) 1.13884(17) 1.20405(14) 0.0468(6) Uani 1 1 d . . . H7A H 0.1477 1.1347 1.2558 0.056 Uiso 1 1 calc R . . H7B H 0.1094 1.1761 1.1831 0.056 Uiso 1 1 calc R . . C8 C 0.25426(18) 1.19022(15) 1.18322(11) 0.0376(5) Uani 1 1 d . . . C9 C 0.1925(2) 1.29075(17) 1.20275(17) 0.0590(7) Uani 1 1 d . . . H9A H 0.1583 1.2896 1.2529 0.089 Uiso 1 1 calc R . . H9B H 0.1360 1.3234 1.1753 0.089 Uiso 1 1 calc R . . H9C H 0.2439 1.3236 1.1925 0.089 Uiso 1 1 calc R . . C10 C 0.3063(2) 1.19014(18) 1.10483(13) 0.0506(6) Uani 1 1 d . . . H10A H 0.3528 1.2278 1.0924 0.076 Uiso 1 1 calc R . . H10B H 0.2488 1.2169 1.0778 0.076 Uiso 1 1 calc R . . H10C H 0.3509 1.1258 1.0940 0.076 Uiso 1 1 calc R . . O1 O 0.33674(11) 1.14448(9) 1.22172(7) 0.0306(3) Uani 1 1 d . . . N1 N 0.21970(14) 1.04444(14) 1.18205(10) 0.0374(4) Uani 1 1 d . . . N2 N 0.32242(15) 0.90357(13) 1.16486(9) 0.0354(4) Uani 1 1 d . . . C11 C 0.31004(15) 1.00354(13) 1.38062(10) 0.0272(4) Uani 1 1 d . . . C12 C 0.22012(19) 1.16798(15) 1.41163(12) 0.0425(5) Uani 1 1 d . . . H12 H 0.2683 1.1800 1.3658 0.051 Uiso 1 1 calc R . . C13 C 0.1012(2) 1.2161(2) 1.40475(17) 0.0647(8) Uani 1 1 d . . . H13A H 0.0901 1.1916 1.3669 0.097 Uiso 1 1 calc R . . H13B H 0.0840 1.2837 1.3939 0.097 Uiso 1 1 calc R . . H13C H 0.0530 1.2038 1.4490 0.097 Uiso 1 1 calc R . . C14 C 0.2419(3) 1.2059(2) 1.46815(17) 0.0686(9) Uani 1 1 d . . . H14A H 0.1866 1.2049 1.5115 0.103 Uiso 1 1 calc R . . H14B H 0.2385 1.2703 1.4526 0.103 Uiso 1 1 calc R . . H14C H 0.3147 1.1669 1.4769 0.103 Uiso 1 1 calc R . . C15 C 0.20607(18) 1.02507(16) 1.49107(11) 0.0381(5) Uani 1 1 d . . . H15 H 0.1593 1.0555 1.5311 0.046 Uiso 1 1 calc R . . C16 C 0.24624(18) 0.93333(16) 1.48518(11) 0.0382(5) Uani 1 1 d . . . H16 H 0.2339 0.8857 1.5205 0.046 Uiso 1 1 calc R . . C17 C 0.36686(18) 0.82902(14) 1.39128(12) 0.0366(4) Uani 1 1 d . . . H17A H 0.3346 0.8268 1.3530 0.044 Uiso 1 1 calc R . . H17B H 0.3556 0.7803 1.4295 0.044 Uiso 1 1 calc R . . C18 C 0.49019(17) 0.80654(13) 1.36340(10) 0.0308(4) Uani 1 1 d . . . C19 C 0.5411(2) 0.70560(14) 1.34392(13) 0.0438(5) Uani 1 1 d . . . H19A H 0.5073 0.7001 1.3082 0.066 Uiso 1 1 calc R . . H19B H 0.5286 0.6629 1.3858 0.066 Uiso 1 1 calc R . . H19C H 0.6199 0.6893 1.3253 0.066 Uiso 1 1 calc R . . C20 C 0.5431(2) 0.81638(17) 1.41833(12) 0.0428(5) Uani 1 1 d . . . H20A H 0.6221 0.7989 1.3998 0.064 Uiso 1 1 calc R . . H20B H 0.5296 0.7751 1.4610 0.064 Uiso 1 1 calc R . . H20C H 0.5116 0.8814 1.4295 0.064 Uiso 1 1 calc R . . O2 O 0.50542(11) 0.86837(9) 1.30307(7) 0.0271(3) Uani 1 1 d . . . N3 N 0.30927(13) 0.92090(12) 1.41793(9) 0.0309(3) Uani 1 1 d . . . N4 N 0.24622(13) 1.06689(12) 1.42721(9) 0.0309(3) Uani 1 1 d . . . C21 C 0.52755(18) 1.32663(14) 1.34104(11) 0.0341(4) Uani 1 1 d . . . C22 C 0.3730(2) 1.46161(16) 1.39959(14) 0.0447(5) Uani 1 1 d . . . H22 H 0.4319 1.4617 1.4204 0.054 Uiso 1 1 calc R . . C23 C 0.2865(2) 1.4401(2) 1.45891(15) 0.0563(7) Uani 1 1 d . . . H23A H 0.2263 1.4422 1.4399 0.084 Uiso 1 1 calc R . . H23B H 0.2586 1.4866 1.4926 0.084 Uiso 1 1 calc R . . H23C H 0.3187 1.3775 1.4826 0.084 Uiso 1 1 calc R . . C24 C 0.3293(3) 1.55616(18) 1.35873(18) 0.0649(8) Uani 1 1 d . . . H24A H 0.3877 1.5652 1.3199 0.097 Uiso 1 1 calc R . . H24B H 0.3033 1.6055 1.3899 0.097 Uiso 1 1 calc R . . H24C H 0.2686 1.5590 1.3399 0.097 Uiso 1 1 calc R . . C25 C 0.3611(2) 1.36201(16) 1.31924(13) 0.0424(5) Uani 1 1 d . . . H25 H 0.2856 1.3937 1.3190 0.051 Uiso 1 1 calc R . . C26 C 0.42882(19) 1.28480(15) 1.28778(12) 0.0390(5) Uani 1 1 d . . . H26 H 0.4104 1.2513 1.2613 0.047 Uiso 1 1 calc R . . C27 C 0.62077(18) 1.17721(15) 1.28338(11) 0.0354(4) Uani 1 1 d . . . H27A H 0.6881 1.1799 1.2912 0.042 Uiso 1 1 calc R . . H27B H 0.6324 1.1719 1.2328 0.042 Uiso 1 1 calc R . . C28 C 0.60211(17) 1.08894(15) 1.32643(11) 0.0332(4) Uani 1 1 d . . . C29 C 0.7114(2) 1.00757(18) 1.31532(15) 0.0514(6) Uani 1 1 d . . . H29A H 0.7007 0.9493 1.3378 0.077 Uiso 1 1 calc R . . H29B H 0.7626 1.0181 1.3361 0.077 Uiso 1 1 calc R . . H29C H 0.7414 1.0030 1.2649 0.077 Uiso 1 1 calc R . . C30 C 0.5585(2) 1.10235(17) 1.40381(12) 0.0413(5) Uani 1 1 d . . . H30A H 0.4876 1.1541 1.4102 0.062 Uiso 1 1 calc R . . H30B H 0.6102 1.1167 1.4213 0.062 Uiso 1 1 calc R . . H30C H 0.5496 1.0448 1.4300 0.062 Uiso 1 1 calc R . . O3 O 0.52645(12) 1.07105(10) 1.30114(8) 0.0344(3) Uani 1 1 d . . . N5 N 0.53040(15) 1.26371(12) 1.30136(9) 0.0340(4) Uani 1 1 d . . . N6 N 0.42221(16) 1.38676(12) 1.35205(10) 0.0385(4) Uani 1 1 d . . . B1 B 0.6210(2) 1.33547(16) 1.37349(12) 0.0332(5) Uani 1 1 d . . . C50 C 0.8082(2) 1.37313(17) 1.39890(13) 0.0444(5) Uani 1 1 d . . . H50A H 0.8379 1.3811 1.4364 0.053 Uiso 1 1 calc R . . H50B H 0.8592 1.3787 1.3535 0.053 Uiso 1 1 calc R . . C51 C 0.8023(2) 1.27572(16) 1.41160(13) 0.0421(5) Uani 1 1 d . . . H51A H 0.7614 1.2665 1.4602 0.051 Uiso 1 1 calc R . . H51B H 0.8774 1.2285 1.4073 0.051 Uiso 1 1 calc R . . C52 C 0.74659(18) 1.25936(15) 1.35996(11) 0.0351(4) Uani 1 1 d . . . H52 H 0.7445 1.1948 1.3717 0.042 Uiso 1 1 calc R . . C53 C 0.8131(2) 1.26835(18) 1.28323(13) 0.0463(6) Uani 1 1 d . . . H53A H 0.8821 1.2746 1.2843 0.056 Uiso 1 1 calc R . . H53B H 0.8324 1.2105 1.2616 0.056 Uiso 1 1 calc R . . C54 C 0.7498(3) 1.3523(2) 1.23793(13) 0.0599(8) Uani 1 1 d . . . H54A H 0.8000 1.3600 1.1926 0.072 Uiso 1 1 calc R . . H54B H 0.6907 1.3386 1.2278 0.072 Uiso 1 1 calc R . . C55 C 0.6999(2) 1.44354(19) 1.27040(14) 0.0536(7) Uani 1 1 d . . . H55A H 0.6492 1.4902 1.2420 0.064 Uiso 1 1 calc R . . H55B H 0.7589 1.4665 1.2680 0.064 Uiso 1 1 calc R . . C56 C 0.6370(2) 1.43766(15) 1.34764(13) 0.0401(5) Uani 1 1 d . . . H56 H 0.5631 1.4885 1.3522 0.048 Uiso 1 1 calc R . . C57 C 0.6976(2) 1.45042(16) 1.39765(14) 0.0451(5) Uani 1 1 d . . . H57A H 0.7080 1.5111 1.3832 0.054 Uiso 1 1 calc R . . H57B H 0.6515 1.4527 1.4458 0.054 Uiso 1 1 calc R . . C31 C 0.86042(15) 0.75117(12) 1.08474(10) 0.0251(3) Uani 1 1 d . . . C32 C 0.88714(16) 0.58672(13) 1.06752(10) 0.0299(4) Uani 1 1 d . . . H32 H 0.9470 0.5950 1.0277 0.036 Uiso 1 1 calc R . . C33 C 0.80249(19) 0.57616(16) 1.03688(13) 0.0411(5) Uani 1 1 d . . . H33A H 0.7449 0.5644 1.0751 0.062 Uiso 1 1 calc R . . H33B H 0.8377 0.5235 1.0081 0.062 Uiso 1 1 calc R . . H33C H 0.7703 0.6338 1.0076 0.062 Uiso 1 1 calc R . . C34 C 0.93779(19) 0.50129(14) 1.11624(12) 0.0380(5) Uani 1 1 d . . . H34A H 0.9934 0.5107 1.1333 0.057 Uiso 1 1 calc R . . H34B H 0.9719 0.4457 1.0905 0.057 Uiso 1 1 calc R . . H34C H 0.8807 0.4924 1.1562 0.057 Uiso 1 1 calc R . . C35 C 0.74731(17) 0.68500(14) 1.16128(11) 0.0332(4) Uani 1 1 d . . . H35 H 0.7157 0.6399 1.1848 0.040 Uiso 1 1 calc R . . C36 C 0.71448(16) 0.77336(14) 1.17631(10) 0.0321(4) Uani 1 1 d . . . H36 H 0.6553 0.8028 1.2125 0.038 Uiso 1 1 calc R . . C37 C 0.76628(15) 0.91216(12) 1.12461(10) 0.0277(4) Uani 1 1 d . . . H37A H 0.8273 0.9247 1.0893 0.033 Uiso 1 1 calc R . . H37B H 0.7680 0.9260 1.1706 0.033 Uiso 1 1 calc R . . C38 C 0.65719(15) 0.97872(13) 1.10468(9) 0.0256(4) Uani 1 1 d . . . C39 C 0.66096(18) 1.07737(14) 1.08936(11) 0.0358(4) Uani 1 1 d . . . H39A H 0.5901 1.1226 1.0811 0.054 Uiso 1 1 calc R . . H39B H 0.7183 1.0800 1.0476 0.054 Uiso 1 1 calc R . . H39C H 0.6769 1.0927 1.1296 0.054 Uiso 1 1 calc R . . C40 C 0.64270(19) 0.94993(16) 1.04018(11) 0.0366(4) Uani 1 1 d . . . H40A H 0.6415 0.8864 1.0505 0.055 Uiso 1 1 calc R . . H40B H 0.7037 0.9515 1.0007 0.055 Uiso 1 1 calc R . . H40C H 0.5737 0.9934 1.0279 0.055 Uiso 1 1 calc R . . O4 O 0.57031(11) 0.97707(9) 1.16147(7) 0.0292(3) Uani 1 1 d . . . N7 N 0.78351(13) 0.81316(11) 1.12888(8) 0.0268(3) Uani 1 1 d . . . N8 N 0.83634(13) 0.67224(11) 1.10481(9) 0.0284(3) Uani 1 1 d . . . B2 B 0.96462(17) 0.75674(14) 1.02142(11) 0.0252(4) Uani 1 1 d . . . C60 C 1.18290(17) 0.75969(14) 0.93501(12) 0.0349(4) Uani 1 1 d . . . H60A H 1.2184 0.7786 0.9637 0.042 Uiso 1 1 calc R . . H60B H 1.2322 0.7492 0.8881 0.042 Uiso 1 1 calc R . . C61 C 1.07515(17) 0.83886(14) 0.92675(11) 0.0329(4) Uani 1 1 d . . . H61A H 1.0456 0.8243 0.8920 0.040 Uiso 1 1 calc R . . H61B H 1.0894 0.8974 0.9081 0.040 Uiso 1 1 calc R . . C62 C 0.98818(15) 0.85489(13) 0.99633(10) 0.0273(4) Uani 1 1 d . . . H62 H 0.9194 0.9067 0.9873 0.033 Uiso 1 1 calc R . . C63 C 1.03135(16) 0.88245(14) 1.05062(11) 0.0318(4) Uani 1 1 d . . . H63A H 1.1013 0.8910 1.0270 0.038 Uiso 1 1 calc R . . H63B H 0.9782 0.9432 1.0668 0.038 Uiso 1 1 calc R . . C64 C 1.04932(17) 0.81025(15) 1.11416(11) 0.0341(4) Uani 1 1 d . . . H64A H 0.9773 0.8110 1.1432 0.041 Uiso 1 1 calc R . . H64B H 1.0855 0.8281 1.1430 0.041 Uiso 1 1 calc R . . C65 C 1.11888(17) 0.71106(15) 1.09460(12) 0.0352(4) Uani 1 1 d . . . H65A H 1.1170 0.6668 1.1377 0.042 Uiso 1 1 calc R . . H65B H 1.1957 0.7067 1.0760 0.042 Uiso 1 1 calc R . . C66 C 1.08133(15) 0.68038(13) 1.03931(10) 0.0287(4) Uani 1 1 d . . . H66 H 1.0723 0.6190 1.0578 0.034 Uiso 1 1 calc R . . C67 C 1.16757(16) 0.66818(13) 0.96974(11) 0.0330(4) Uani 1 1 d . . . H67A H 1.2384 0.6219 0.9789 0.040 Uiso 1 1 calc R . . H67B H 1.1451 0.6431 0.9370 0.040 Uiso 1 1 calc R . . C100 C 0.0676(4) 0.8055(4) 1.3749(3) 0.1214(16) Uani 1 1 d DU . . H100 H 0.0834 0.7414 1.3923 0.146 Uiso 1 1 calc R . . C101 C 0.0300(4) 0.8406(5) 1.3126(3) 0.1242(17) Uani 1 1 d DU . . H101 H 0.0210 0.7997 1.2873 0.149 Uiso 1 1 calc R . . C102 C 0.0072(4) 0.9287(5) 1.2886(2) 0.1107(15) Uani 1 1 d DU . . H102 H -0.0160 0.9509 1.2454 0.133 Uiso 1 1 calc R . . C103 C 0.0167(3) 0.9892(4) 1.3254(3) 0.1061(14) Uani 1 1 d DU . . H103 H -0.0030 1.0536 1.3082 0.127 Uiso 1 1 calc R . . C104 C 0.0540(3) 0.9588(4) 1.3865(2) 0.0946(12) Uani 1 1 d DU . . H104 H 0.0606 1.0014 1.4114 0.114 Uiso 1 1 calc R . . C105 C 0.0814(3) 0.8659(4) 1.4110(2) 0.0917(12) Uani 1 1 d DU . . H105 H 0.1097 0.8429 1.4524 0.110 Uiso 1 1 calc R . . C200 C 0.8855(5) 0.6337(4) 1.3825(3) 0.1360(19) Uani 1 1 d DU . . H200 H 0.8347 0.6668 1.4204 0.163 Uiso 1 1 calc R . . C201 C 0.9635(4) 0.5475(4) 1.3962(3) 0.1289(19) Uani 1 1 d DU . . H201 H 0.9680 0.5215 1.4431 0.155 Uiso 1 1 calc R . . C202 C 1.0326(4) 0.5013(3) 1.3420(3) 0.1048(14) Uani 1 1 d DU . . H202 H 1.0833 0.4397 1.3500 0.126 Uiso 1 1 calc R . . C203 C 1.0299(4) 0.5429(3) 1.2758(2) 0.1010(13) Uani 1 1 d DU . . H203 H 1.0843 0.5131 1.2376 0.121 Uiso 1 1 calc R . . C204 C 0.9539(3) 0.6232(3) 1.2634(2) 0.0902(11) Uani 1 1 d DU . . H204 H 0.9508 0.6478 1.2160 0.108 Uiso 1 1 calc R . . C205 C 0.8805(4) 0.6722(3) 1.3146(2) 0.0967(12) Uani 1 1 d DU . . H205 H 0.8268 0.7314 1.3046 0.116 Uiso 1 1 calc R . . C300 C 1.4573(2) 0.4807(2) 1.16057(16) 0.0621(7) Uani 1 1 d . . . H300 H 1.4726 0.5034 1.1959 0.075 Uiso 1 1 calc R . . C301 C 1.3523(3) 0.5111(2) 1.15154(18) 0.0685(8) Uani 1 1 d . . . H301 H 1.2951 0.5552 1.1804 0.082 Uiso 1 1 calc R . . C302 C 1.3289(2) 0.4784(2) 1.10133(18) 0.0622(7) Uani 1 1 d . . . H302 H 1.2558 0.4993 1.0955 0.075 Uiso 1 1 calc R . . C303 C 1.4116(3) 0.4153(2) 1.0596(2) 0.0732(9) Uani 1 1 d . . . H303 H 1.3960 0.3925 1.0244 0.088 Uiso 1 1 calc R . . C304 C 1.5178(3) 0.3845(3) 1.0683(2) 0.0786(10) Uani 1 1 d . . . H304 H 1.5751 0.3403 1.0395 0.094 Uiso 1 1 calc R . . C305 C 1.5399(2) 0.4180(2) 1.11881(16) 0.0622(7) Uani 1 1 d . . . H305 H 1.6128 0.3974 1.1247 0.075 Uiso 1 1 calc R . . HB2 H 0.9477(19) 0.7369(16) 0.9751(12) 0.035(6) Uiso 1 1 d . . . HB1 H 0.578(2) 1.3343(17) 1.4302(14) 0.042(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.02221(6) 0.01866(6) 0.02002(6) -0.00465(4) -0.00389(4) -0.00604(4) C1 0.0328(10) 0.0346(10) 0.0328(10) 0.0002(8) -0.0118(8) -0.0165(8) C2 0.0657(16) 0.0337(11) 0.0530(14) -0.0042(10) -0.0283(12) -0.0225(11) C3 0.126(3) 0.0514(17) 0.0601(18) 0.0068(14) -0.0304(19) -0.052(2) C4 0.0631(17) 0.0529(16) 0.0656(18) -0.0180(13) -0.0158(14) -0.0202(14) C5 0.0469(13) 0.0682(16) 0.0343(11) -0.0035(10) -0.0147(9) -0.0348(13) C6 0.0354(11) 0.0791(18) 0.0361(12) -0.0004(11) -0.0149(9) -0.0260(12) C7 0.0288(11) 0.0488(14) 0.0539(14) -0.0087(11) -0.0128(10) -0.0006(10) C8 0.0386(11) 0.0305(10) 0.0352(11) 0.0000(8) -0.0156(9) -0.0002(9) C9 0.0571(16) 0.0313(12) 0.0692(18) -0.0025(11) -0.0239(14) 0.0097(11) C10 0.0690(17) 0.0430(13) 0.0362(12) 0.0062(10) -0.0196(11) -0.0158(12) O1 0.0338(7) 0.0229(6) 0.0301(7) -0.0022(5) -0.0104(5) -0.0029(5) N1 0.0302(9) 0.0468(11) 0.0371(9) -0.0011(8) -0.0118(7) -0.0145(8) N2 0.0433(10) 0.0411(10) 0.0330(9) 0.0000(7) -0.0146(7) -0.0243(8) C11 0.0250(9) 0.0275(9) 0.0277(9) -0.0051(7) -0.0017(7) -0.0098(7) C12 0.0447(12) 0.0308(11) 0.0428(12) -0.0128(9) 0.0107(9) -0.0131(9) C13 0.0527(16) 0.0443(15) 0.0672(19) -0.0009(13) -0.0008(13) 0.0030(12) C14 0.077(2) 0.0696(19) 0.071(2) -0.0383(16) 0.0151(16) -0.0448(17) C15 0.0376(11) 0.0468(12) 0.0256(10) -0.0080(8) 0.0022(8) -0.0146(10) C16 0.0391(11) 0.0438(12) 0.0263(10) -0.0003(8) 0.0000(8) -0.0157(10) C17 0.0390(11) 0.0263(10) 0.0398(11) -0.0036(8) 0.0008(9) -0.0130(9) C18 0.0375(10) 0.0219(9) 0.0261(9) 0.0010(7) -0.0043(7) -0.0071(8) C19 0.0521(13) 0.0218(10) 0.0451(12) -0.0011(8) -0.0017(10) -0.0073(9) C20 0.0454(12) 0.0431(12) 0.0321(11) -0.0012(9) -0.0145(9) -0.0051(10) O2 0.0298(7) 0.0224(6) 0.0237(6) -0.0024(5) -0.0032(5) -0.0058(5) N3 0.0295(8) 0.0309(8) 0.0279(8) -0.0034(6) -0.0007(6) -0.0099(7) N4 0.0300(8) 0.0325(9) 0.0267(8) -0.0070(6) -0.0001(6) -0.0098(7) C21 0.0454(12) 0.0285(10) 0.0330(10) -0.0049(8) -0.0081(8) -0.0177(9) C22 0.0480(13) 0.0330(11) 0.0577(15) -0.0189(10) -0.0132(11) -0.0114(10) C23 0.0629(17) 0.0554(16) 0.0573(16) -0.0253(13) -0.0068(13) -0.0232(14) C24 0.078(2) 0.0316(13) 0.083(2) -0.0138(13) -0.0217(16) -0.0104(13) C25 0.0471(13) 0.0344(11) 0.0522(14) -0.0076(10) -0.0213(10) -0.0130(10) C26 0.0494(13) 0.0357(11) 0.0418(12) -0.0052(9) -0.0179(10) -0.0197(10) C27 0.0378(11) 0.0394(11) 0.0349(10) -0.0155(9) -0.0021(8) -0.0184(9) C28 0.0363(10) 0.0332(10) 0.0374(11) -0.0119(8) -0.0128(8) -0.0131(9) C29 0.0456(13) 0.0484(14) 0.0615(16) -0.0226(12) -0.0198(12) -0.0049(11) C30 0.0497(13) 0.0471(13) 0.0336(11) -0.0065(9) -0.0109(9) -0.0219(11) O3 0.0411(8) 0.0305(7) 0.0394(8) -0.0081(6) -0.0151(6) -0.0149(6) N5 0.0433(10) 0.0308(9) 0.0341(9) -0.0073(7) -0.0080(7) -0.0181(8) N6 0.0459(10) 0.0297(9) 0.0452(10) -0.0100(7) -0.0142(8) -0.0133(8) B1 0.0439(13) 0.0324(11) 0.0309(11) -0.0054(9) -0.0087(9) -0.0202(10) C50 0.0557(14) 0.0435(13) 0.0472(13) -0.0068(10) -0.0187(11) -0.0258(11) C51 0.0487(13) 0.0391(12) 0.0462(13) -0.0021(10) -0.0185(10) -0.0195(10) C52 0.0448(12) 0.0325(10) 0.0346(10) -0.0029(8) -0.0083(9) -0.0211(9) C53 0.0501(14) 0.0560(15) 0.0420(12) -0.0154(11) 0.0017(10) -0.0315(12) C54 0.088(2) 0.078(2) 0.0319(12) -0.0024(12) -0.0043(12) -0.0562(18) C55 0.0753(18) 0.0537(15) 0.0479(14) 0.0169(11) -0.0254(13) -0.0425(14) C56 0.0495(13) 0.0313(11) 0.0487(13) -0.0016(9) -0.0181(10) -0.0204(10) C57 0.0561(14) 0.0363(12) 0.0553(14) -0.0088(10) -0.0188(11) -0.0230(11) C31 0.0259(9) 0.0216(8) 0.0277(9) -0.0071(7) -0.0049(7) -0.0070(7) C32 0.0333(10) 0.0221(9) 0.0324(10) -0.0090(7) 0.0005(8) -0.0102(8) C33 0.0444(12) 0.0315(11) 0.0511(13) -0.0105(9) -0.0121(10) -0.0135(9) C34 0.0391(11) 0.0265(10) 0.0411(12) -0.0067(8) -0.0035(9) -0.0060(9) C35 0.0315(10) 0.0287(10) 0.0338(10) -0.0048(8) 0.0038(8) -0.0116(8) C36 0.0298(9) 0.0284(10) 0.0303(10) -0.0055(7) 0.0026(7) -0.0074(8) C37 0.0273(9) 0.0221(8) 0.0339(10) -0.0119(7) -0.0036(7) -0.0069(7) C38 0.0261(9) 0.0248(9) 0.0234(8) -0.0059(7) -0.0003(7) -0.0085(7) C39 0.0396(11) 0.0265(10) 0.0374(11) -0.0042(8) -0.0027(8) -0.0112(8) C40 0.0437(12) 0.0443(12) 0.0263(10) -0.0054(8) -0.0075(8) -0.0198(10) O4 0.0273(6) 0.0280(7) 0.0257(6) -0.0043(5) 0.0010(5) -0.0069(5) N7 0.0258(8) 0.0226(7) 0.0295(8) -0.0084(6) -0.0012(6) -0.0065(6) N8 0.0282(8) 0.0223(7) 0.0310(8) -0.0085(6) 0.0019(6) -0.0083(6) B2 0.0256(10) 0.0232(9) 0.0267(10) -0.0074(7) -0.0024(7) -0.0086(8) C60 0.0304(10) 0.0278(10) 0.0400(11) -0.0069(8) 0.0036(8) -0.0098(8) C61 0.0346(10) 0.0252(9) 0.0343(10) -0.0036(7) 0.0000(8) -0.0107(8) C62 0.0262(9) 0.0232(9) 0.0308(9) -0.0052(7) -0.0043(7) -0.0074(7) C63 0.0302(10) 0.0267(9) 0.0412(11) -0.0108(8) -0.0050(8) -0.0113(8) C64 0.0320(10) 0.0382(11) 0.0371(11) -0.0108(8) -0.0102(8) -0.0128(9) C65 0.0297(10) 0.0362(11) 0.0372(11) -0.0029(8) -0.0104(8) -0.0075(8) C66 0.0261(9) 0.0211(8) 0.0349(10) -0.0048(7) -0.0016(7) -0.0067(7) C67 0.0278(9) 0.0245(9) 0.0404(11) -0.0083(8) 0.0024(8) -0.0071(8) C100 0.073(3) 0.128(4) 0.122(4) -0.025(3) 0.008(2) -0.007(3) C101 0.099(3) 0.173(4) 0.089(3) -0.055(3) 0.002(2) -0.032(3) C102 0.078(3) 0.189(5) 0.067(2) -0.014(3) -0.0056(19) -0.057(3) C103 0.067(2) 0.156(4) 0.096(3) 0.027(3) -0.015(2) -0.061(2) C104 0.068(2) 0.149(3) 0.083(2) 0.011(2) -0.0176(18) -0.066(2) C105 0.0471(17) 0.147(4) 0.070(2) 0.002(2) -0.0096(15) -0.032(2) C200 0.139(4) 0.158(4) 0.072(3) -0.043(3) 0.007(3) -0.018(3) C201 0.109(3) 0.188(5) 0.068(2) 0.044(3) -0.020(2) -0.058(3) C202 0.088(3) 0.081(3) 0.137(4) 0.022(2) -0.028(3) -0.035(2) C203 0.099(3) 0.097(3) 0.097(3) -0.040(2) -0.024(2) -0.009(2) C204 0.077(2) 0.110(3) 0.067(2) -0.013(2) -0.0136(17) -0.015(2) C205 0.096(3) 0.086(3) 0.082(3) -0.013(2) -0.010(2) -0.011(2) C300 0.0559(16) 0.0668(19) 0.0537(16) -0.0134(14) -0.0183(13) -0.0044(14) C301 0.0515(16) 0.0649(19) 0.0674(19) -0.0174(15) -0.0172(14) 0.0092(14) C302 0.0467(15) 0.0567(17) 0.077(2) 0.0001(14) -0.0240(14) -0.0083(13) C303 0.0623(19) 0.076(2) 0.092(3) -0.0250(18) -0.0278(17) -0.0205(17) C304 0.0478(16) 0.092(3) 0.090(2) -0.046(2) -0.0089(16) -0.0059(16) C305 0.0409(14) 0.084(2) 0.0531(16) -0.0119(14) -0.0084(11) -0.0125(14) _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 O3 2.1183(13) . ? Ce1 O4 2.1217(13) . ? Ce1 O1 2.1510(13) . ? Ce1 O2 2.1592(13) . ? Ce1 C11 2.7033(18) . ? Ce1 C1 2.7046(19) . ? C1 N1 1.359(3) . ? C1 N2 1.363(3) . ? C2 N2 1.460(3) . ? C2 C4 1.516(4) . ? C2 C3 1.526(4) . ? C5 C6 1.330(4) . ? C5 N2 1.385(3) . ? C6 N1 1.381(3) . ? C7 N1 1.463(3) . ? C7 C8 1.530(3) . ? C8 O1 1.407(2) . ? C8 C10 1.527(3) . ? C8 C9 1.533(3) . ? C11 N4 1.357(2) . ? C11 N3 1.358(2) . ? C12 N4 1.464(3) . ? C12 C14 1.515(4) . ? C12 C13 1.526(4) . ? C15 C16 1.335(3) . ? C15 N4 1.383(3) . ? C16 N3 1.382(3) . ? C17 N3 1.465(3) . ? C17 C18 1.535(3) . ? C18 O2 1.407(2) . ? C18 C20 1.525(3) . ? C18 C19 1.534(3) . ? C21 N6 1.355(3) . ? C21 N5 1.363(2) . ? C21 B1 1.639(3) . ? C22 N6 1.480(3) . ? C22 C23 1.513(4) . ? C22 C24 1.513(4) . ? C25 C26 1.344(3) . ? C25 N6 1.387(3) . ? C26 N5 1.381(3) . ? C27 N5 1.452(3) . ? C27 C28 1.546(3) . ? C28 O3 1.402(2) . ? C28 C30 1.516(3) . ? C28 C29 1.523(3) . ? B1 C52 1.637(3) . ? B1 C56 1.659(3) . ? C50 C57 1.517(4) . ? C50 C51 1.525(3) . ? C51 C52 1.545(3) . ? C52 C53 1.559(3) . ? C53 C54 1.529(4) . ? C54 C55 1.508(4) . ? C55 C56 1.546(4) . ? C56 C57 1.541(3) . ? C31 N7 1.357(2) . ? C31 N8 1.358(2) . ? C31 B2 1.639(3) . ? C32 N8 1.484(2) . ? C32 C33 1.519(3) . ? C32 C34 1.523(3) . ? C35 C36 1.343(3) . ? C35 N8 1.388(2) . ? C36 N7 1.381(2) . ? C37 N7 1.460(2) . ? C37 C38 1.544(3) . ? C38 O4 1.400(2) . ? C38 C40 1.526(3) . ? C38 C39 1.531(3) . ? B2 C62 1.645(3) . ? B2 C66 1.649(3) . ? C60 C61 1.526(3) . ? C60 C67 1.527(3) . ? C61 C62 1.546(3) . ? C62 C63 1.560(3) . ? C63 C64 1.521(3) . ? C64 C65 1.527(3) . ? C65 C66 1.555(3) . ? C66 C67 1.540(3) . ? C100 C105 1.390(7) . ? C100 C101 1.398(6) . ? C101 C102 1.305(8) . ? C102 C103 1.370(6) . ? C103 C104 1.371(6) . ? C104 C105 1.369(5) . ? C200 C205 1.373(7) . ? C200 C201 1.377(6) . ? C201 C202 1.338(7) . ? C202 C203 1.352(5) . ? C203 C204 1.302(6) . ? C204 C205 1.332(5) . ? C300 C305 1.364(4) . ? C300 C301 1.369(4) . ? C301 C302 1.367(4) . ? C302 C303 1.367(5) . ? C303 C304 1.383(4) . ? C304 C305 1.370(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ce1 O4 98.21(6) . . ? O3 Ce1 O1 93.48(5) . . ? O4 Ce1 O1 101.80(5) . . ? O3 Ce1 O2 100.41(5) . . ? O4 Ce1 O2 92.27(5) . . ? O1 Ce1 O2 158.63(5) . . ? O3 Ce1 C11 88.87(6) . . ? O4 Ce1 C11 164.58(5) . . ? O1 Ce1 C11 91.36(6) . . ? O2 Ce1 C11 72.91(5) . . ? O3 Ce1 C1 166.02(6) . . ? O4 Ce1 C1 88.65(6) . . ? O1 Ce1 C1 73.12(6) . . ? O2 Ce1 C1 91.42(6) . . ? C11 Ce1 C1 87.51(6) . . ? N1 C1 N2 102.89(17) . . ? N1 C1 Ce1 122.18(14) . . ? N2 C1 Ce1 133.52(14) . . ? N2 C2 C4 110.9(2) . . ? N2 C2 C3 109.5(2) . . ? C4 C2 C3 111.4(2) . . ? C6 C5 N2 106.4(2) . . ? C5 C6 N1 107.2(2) . . ? N1 C7 C8 113.99(18) . . ? O1 C8 C10 109.20(19) . . ? O1 C8 C7 108.26(17) . . ? C10 C8 C7 111.4(2) . . ? O1 C8 C9 109.11(19) . . ? C10 C8 C9 110.5(2) . . ? C7 C8 C9 108.4(2) . . ? C8 O1 Ce1 144.92(13) . . ? C1 N1 C6 111.7(2) . . ? C1 N1 C7 124.77(18) . . ? C6 N1 C7 123.5(2) . . ? C1 N2 C5 111.86(19) . . ? C1 N2 C2 124.66(17) . . ? C5 N2 C2 123.46(19) . . ? N4 C11 N3 102.98(16) . . ? N4 C11 Ce1 133.89(13) . . ? N3 C11 Ce1 121.87(13) . . ? N4 C12 C14 110.3(2) . . ? N4 C12 C13 109.6(2) . . ? C14 C12 C13 111.3(2) . . ? C16 C15 N4 106.30(18) . . ? C15 C16 N3 106.89(18) . . ? N3 C17 C18 113.21(17) . . ? O2 C18 C20 109.76(17) . . ? O2 C18 C19 109.71(16) . . ? C20 C18 C19 110.01(18) . . ? O2 C18 C17 108.45(16) . . ? C20 C18 C17 111.39(18) . . ? C19 C18 C17 107.48(17) . . ? C18 O2 Ce1 145.71(11) . . ? C11 N3 C16 111.74(17) . . ? C11 N3 C17 125.11(16) . . ? C16 N3 C17 123.15(17) . . ? C11 N4 C15 112.09(17) . . ? C11 N4 C12 124.32(17) . . ? C15 N4 C12 123.57(17) . . ? N6 C21 N5 104.38(18) . . ? N6 C21 B1 123.11(17) . . ? N5 C21 B1 132.5(2) . . ? N6 C22 C23 109.50(19) . . ? N6 C22 C24 110.3(2) . . ? C23 C22 C24 113.0(2) . . ? C26 C25 N6 107.1(2) . . ? C25 C26 N5 106.63(19) . . ? N5 C27 C28 113.40(17) . . ? O3 C28 C30 109.25(18) . . ? O3 C28 C29 109.64(17) . . ? C30 C28 C29 110.4(2) . . ? O3 C28 C27 108.68(17) . . ? C30 C28 C27 111.23(17) . . ? C29 C28 C27 107.6(2) . . ? C28 O3 Ce1 164.42(13) . . ? C21 N5 C26 111.10(18) . . ? C21 N5 C27 126.42(18) . . ? C26 N5 C27 121.87(17) . . ? C21 N6 C25 110.76(18) . . ? C21 N6 C22 125.82(18) . . ? C25 N6 C22 122.98(19) . . ? C52 B1 C21 121.02(17) . . ? C52 B1 C56 103.45(17) . . ? C21 B1 C56 112.39(18) . . ? C57 C50 C51 112.7(2) . . ? C50 C51 C52 113.21(19) . . ? C51 C52 C53 109.94(18) . . ? C51 C52 B1 106.10(17) . . ? C53 C52 B1 113.97(19) . . ? C54 C53 C52 112.5(2) . . ? C55 C54 C53 114.7(2) . . ? C54 C55 C56 114.68(19) . . ? C57 C56 C55 111.2(2) . . ? C57 C56 B1 107.48(18) . . ? C55 C56 B1 112.04(19) . . ? C50 C57 C56 113.46(19) . . ? N7 C31 N8 104.08(15) . . ? N7 C31 B2 133.37(16) . . ? N8 C31 B2 122.53(15) . . ? N8 C32 C33 109.36(16) . . ? N8 C32 C34 110.64(16) . . ? C33 C32 C34 112.68(17) . . ? C36 C35 N8 106.86(17) . . ? C35 C36 N7 106.65(17) . . ? N7 C37 C38 113.70(15) . . ? O4 C38 C40 110.01(16) . . ? O4 C38 C39 109.20(15) . . ? C40 C38 C39 110.39(17) . . ? O4 C38 C37 109.42(15) . . ? C40 C38 C37 110.64(15) . . ? C39 C38 C37 107.12(16) . . ? C38 O4 Ce1 161.24(12) . . ? C31 N7 C36 111.46(15) . . ? C31 N7 C37 125.96(16) . . ? C36 N7 C37 122.35(15) . . ? C31 N8 C35 110.94(15) . . ? C31 N8 C32 125.92(16) . . ? C35 N8 C32 122.74(16) . . ? C31 B2 C62 121.13(15) . . ? C31 B2 C66 111.42(15) . . ? C62 B2 C66 103.70(15) . . ? C61 C60 C67 112.70(17) . . ? C60 C61 C62 113.17(17) . . ? C61 C62 C63 109.57(16) . . ? C61 C62 B2 105.81(14) . . ? C63 C62 B2 113.60(16) . . ? C64 C63 C62 113.41(16) . . ? C63 C64 C65 113.21(17) . . ? C64 C65 C66 114.10(16) . . ? C67 C66 C65 110.60(16) . . ? C67 C66 B2 107.36(16) . . ? C65 C66 B2 112.80(15) . . ? C60 C67 C66 112.73(16) . . ? C105 C100 C101 118.9(6) . . ? C102 C101 C100 121.0(6) . . ? C101 C102 C103 120.2(5) . . ? C102 C103 C104 121.4(5) . . ? C105 C104 C103 118.8(5) . . ? C104 C105 C100 119.6(4) . . ? C205 C200 C201 120.6(4) . . ? C202 C201 C200 118.6(4) . . ? C201 C202 C203 119.5(5) . . ? C204 C203 C202 121.0(4) . . ? C203 C204 C205 122.5(4) . . ? C204 C205 C200 117.3(4) . . ? C305 C300 C301 120.0(3) . . ? C302 C301 C300 120.6(3) . . ? C303 C302 C301 119.4(3) . . ? C302 C303 C304 120.2(3) . . ? C305 C304 C303 119.7(3) . . ? C300 C305 C304 120.1(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.461 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.076 #===END of CIF data_ceimc4_compound_5 _database_code_depnum_ccdc_archive 'CCDC 650971' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H91 Ce I N8 O4' _chemical_formula_sum 'C61 H91 Ce I N8 O4' _chemical_formula_weight 1267.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.371(2) _cell_length_b 16.609(3) _cell_length_c 19.615(3) _cell_angle_alpha 70.250(3) _cell_angle_beta 74.282(3) _cell_angle_gamma 74.021(3) _cell_volume 3286.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13588 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour pale_yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.701 #scaled 0.841 _exptl_absorpt_correction_T_max 0.834 #scaled 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ' sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29604 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.51 _reflns_number_total 14551 _reflns_number_gt 11968 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.2004);PLATON(Spek,2003)' _refine_special_details ; Restraints applied to benzene geometry and displacement parameters. ; _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^)+(0.0308P)^2^+3.3194P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14551 _refine_ls_number_parameters 676 _refine_ls_number_restraints 174 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.532225(13) 0.146628(9) 0.211291(8) 0.02355(4) Uani 1 1 d . . . C1 C 0.5818(2) -0.02566(17) 0.20510(17) 0.0338(6) Uani 1 1 d . . . C2 C 0.7612(3) -0.0436(2) 0.10168(19) 0.0439(7) Uani 1 1 d . . . H2A H 0.7580 0.0182 0.0987 0.053 Uiso 1 1 calc R . . C3 C 0.7445(3) -0.0452(3) 0.0275(2) 0.0589(10) Uani 1 1 d . . . H3A H 0.6636 -0.0091 0.0175 0.088 Uiso 1 1 calc R . . H3B H 0.7480 -0.1054 0.0291 0.088 Uiso 1 1 calc R . . H3C H 0.8113 -0.0221 -0.0117 0.088 Uiso 1 1 calc R . . C4 C 0.8873(3) -0.0978(2) 0.1188(2) 0.0549(9) Uani 1 1 d . . . H4A H 0.8959 -0.0951 0.1663 0.082 Uiso 1 1 calc R . . H4B H 0.9542 -0.0745 0.0797 0.082 Uiso 1 1 calc R . . H4C H 0.8929 -0.1587 0.1213 0.082 Uiso 1 1 calc R . . C5 C 0.6332(3) -0.1574(2) 0.1808(2) 0.0529(9) Uani 1 1 d . . . H5A H 0.6757 -0.2028 0.1584 0.063 Uiso 1 1 calc R . . C6 C 0.5363(3) -0.16039(19) 0.2371(2) 0.0499(9) Uani 1 1 d . . . H6A H 0.4960 -0.2084 0.2624 0.060 Uiso 1 1 calc R . . C7 C 0.4028(3) -0.05718(18) 0.30977(18) 0.0384(7) Uani 1 1 d . . . H7A H 0.4368 -0.0419 0.3442 0.046 Uiso 1 1 calc R . . H7B H 0.3652 -0.1088 0.3381 0.046 Uiso 1 1 calc R . . C8 C 0.2994(2) 0.02024(17) 0.28029(17) 0.0327(6) Uani 1 1 d . . . C9 C 0.1930(3) 0.0286(2) 0.34688(18) 0.0446(7) Uani 1 1 d . . . H9A H 0.1251 0.0769 0.3306 0.067 Uiso 1 1 calc R . . H9B H 0.2242 0.0401 0.3839 0.067 Uiso 1 1 calc R . . H9C H 0.1619 -0.0259 0.3686 0.067 Uiso 1 1 calc R . . C10 C 0.2517(3) 0.0015(2) 0.22265(18) 0.0404(7) Uani 1 1 d . . . H10A H 0.1869 0.0510 0.2041 0.061 Uiso 1 1 calc R . . H10B H 0.2167 -0.0514 0.2453 0.061 Uiso 1 1 calc R . . H10C H 0.3209 -0.0071 0.1816 0.061 Uiso 1 1 calc R . . O1 O 0.34553(16) 0.09675(11) 0.25090(11) 0.0328(4) Uani 1 1 d . . . N1 N 0.5051(2) -0.08032(14) 0.25192(15) 0.0375(6) Uani 1 1 d . . . N2 N 0.6601(2) -0.07473(16) 0.16124(15) 0.0398(6) Uani 1 1 d . . . C11 C 0.6129(3) 0.05813(18) 0.34541(16) 0.0338(6) Uani 1 1 d . . . C12 C 0.7982(3) -0.0562(2) 0.31907(19) 0.0420(7) Uani 1 1 d . . . H12A H 0.7801 -0.0294 0.2681 0.050 Uiso 1 1 calc R . . C13 C 0.7720(3) -0.1482(2) 0.3472(2) 0.0587(10) Uani 1 1 d . . . H13A H 0.6840 -0.1452 0.3488 0.088 Uiso 1 1 calc R . . H13B H 0.7902 -0.1761 0.3969 0.088 Uiso 1 1 calc R . . H13C H 0.8249 -0.1824 0.3139 0.088 Uiso 1 1 calc R . . C14 C 0.9349(3) -0.0577(2) 0.3144(2) 0.0576(10) Uani 1 1 d . . . H14A H 0.9493 0.0021 0.2954 0.086 Uiso 1 1 calc R . . H14B H 0.9879 -0.0919 0.2812 0.086 Uiso 1 1 calc R . . H14C H 0.9552 -0.0844 0.3637 0.086 Uiso 1 1 calc R . . C15 C 0.7265(3) -0.0073(2) 0.43576(19) 0.0499(8) Uani 1 1 d . . . H15A H 0.7902 -0.0447 0.4615 0.060 Uiso 1 1 calc R . . C16 C 0.6308(3) 0.0498(2) 0.46016(19) 0.0495(8) Uani 1 1 d . . . H16A H 0.6132 0.0613 0.5066 0.059 Uiso 1 1 calc R . . C17 C 0.4527(3) 0.1610(2) 0.40739(17) 0.0398(7) Uani 1 1 d . . . H17A H 0.4295 0.1695 0.4573 0.048 Uiso 1 1 calc R . . H17B H 0.3818 0.1442 0.3991 0.048 Uiso 1 1 calc R . . C18 C 0.4744(3) 0.24859(18) 0.34930(15) 0.0331(6) Uani 1 1 d . . . C19 C 0.3605(3) 0.3181(2) 0.36920(18) 0.0454(7) Uani 1 1 d . . . H19A H 0.3691 0.3753 0.3341 0.068 Uiso 1 1 calc R . . H19B H 0.3554 0.3201 0.4193 0.068 Uiso 1 1 calc R . . H19C H 0.2844 0.3031 0.3669 0.068 Uiso 1 1 calc R . . C20 C 0.5937(3) 0.2717(2) 0.3532(2) 0.0477(8) Uani 1 1 d . . . H20A H 0.6058 0.3270 0.3158 0.072 Uiso 1 1 calc R . . H20B H 0.6654 0.2253 0.3441 0.072 Uiso 1 1 calc R . . H20C H 0.5860 0.2777 0.4024 0.072 Uiso 1 1 calc R . . O2 O 0.48120(18) 0.24382(12) 0.27904(10) 0.0321(4) Uani 1 1 d . . . N3 N 0.5621(2) 0.08947(16) 0.40496(13) 0.0369(5) Uani 1 1 d . . . N4 N 0.7155(2) -0.00195(16) 0.36585(14) 0.0379(6) Uani 1 1 d . . . C21 C 0.6107(3) 0.35892(18) 0.10138(15) 0.0330(6) Uani 1 1 d . . . H21A H 0.5609 0.3223 0.1000 0.040 Uiso 1 1 calc R . . C22 C 0.4363(3) 0.45705(19) 0.15937(18) 0.0398(7) Uani 1 1 d . . . H22A H 0.4040 0.4047 0.1945 0.048 Uiso 1 1 calc R . . C23 C 0.3619(3) 0.4956(2) 0.0981(2) 0.0481(8) Uani 1 1 d . . . H23A H 0.3731 0.4523 0.0719 0.072 Uiso 1 1 calc R . . H23B H 0.3912 0.5476 0.0633 0.072 Uiso 1 1 calc R . . H23C H 0.2733 0.5117 0.1193 0.072 Uiso 1 1 calc R . . C24 C 0.4235(4) 0.5206(2) 0.2021(2) 0.0515(8) Uani 1 1 d . . . H24A H 0.4725 0.4929 0.2411 0.077 Uiso 1 1 calc R . . H24B H 0.3356 0.5375 0.2242 0.077 Uiso 1 1 calc R . . H24C H 0.4543 0.5727 0.1685 0.077 Uiso 1 1 calc R . . C25 C 0.6698(3) 0.4642(2) 0.1199(2) 0.0473(8) Uani 1 1 d . . . H25A H 0.6672 0.5142 0.1340 0.057 Uiso 1 1 calc R . . C26 C 0.7717(3) 0.4154(2) 0.0889(2) 0.0483(8) Uani 1 1 d . . . H26A H 0.8546 0.4245 0.0770 0.058 Uiso 1 1 calc R . . C27 C 0.8163(3) 0.2757(2) 0.05259(17) 0.0422(7) Uani 1 1 d . . . H27A H 0.8973 0.2918 0.0251 0.051 Uiso 1 1 calc R . . H27B H 0.7786 0.2630 0.0183 0.051 Uiso 1 1 calc R . . C28 C 0.8392(2) 0.19218(19) 0.11772(17) 0.0343(6) Uani 1 1 d . . . C29 C 0.9387(3) 0.1253(2) 0.0845(2) 0.0590(10) Uani 1 1 d . . . H29A H 0.9569 0.0711 0.1237 0.088 Uiso 1 1 calc R . . H29B H 1.0150 0.1486 0.0612 0.088 Uiso 1 1 calc R . . H29C H 0.9082 0.1134 0.0475 0.088 Uiso 1 1 calc R . . C30 C 0.8872(3) 0.2116(2) 0.17485(18) 0.0425(7) Uani 1 1 d . . . H30A H 0.9008 0.1585 0.2158 0.064 Uiso 1 1 calc R . . H30B H 0.8257 0.2574 0.1937 0.064 Uiso 1 1 calc R . . H30C H 0.9661 0.2315 0.1517 0.064 Uiso 1 1 calc R . . O3 O 0.72919(16) 0.16276(12) 0.14972(11) 0.0337(4) Uani 1 1 d . . . N5 N 0.7339(2) 0.34966(16) 0.07738(14) 0.0372(6) Uani 1 1 d . . . N6 N 0.5692(2) 0.42797(15) 0.12758(14) 0.0352(5) Uani 1 1 d . . . C31 C 0.1860(2) 0.26733(17) 0.17787(15) 0.0282(5) Uani 1 1 d . . . H31A H 0.2218 0.2159 0.2115 0.034 Uiso 1 1 calc R . . C32 C 0.0603(3) 0.3452(2) 0.27143(16) 0.0365(6) Uani 1 1 d . . . H32A H 0.1065 0.2947 0.3058 0.044 Uiso 1 1 calc R . . C33 C 0.0823(3) 0.4288(2) 0.27642(19) 0.0502(8) Uani 1 1 d . . . H33A H 0.1718 0.4289 0.2622 0.075 Uiso 1 1 calc R . . H33B H 0.0516 0.4325 0.3272 0.075 Uiso 1 1 calc R . . H33C H 0.0376 0.4791 0.2431 0.075 Uiso 1 1 calc R . . C34 C -0.0764(3) 0.3403(3) 0.29331(19) 0.0596(10) Uani 1 1 d . . . H34A H -0.0860 0.2851 0.2898 0.089 Uiso 1 1 calc R . . H34B H -0.1233 0.3892 0.2601 0.089 Uiso 1 1 calc R . . H34C H -0.1085 0.3434 0.3442 0.089 Uiso 1 1 calc R . . C35 C 0.0794(2) 0.39935(18) 0.13141(15) 0.0321(6) Uani 1 1 d . . . H35A H 0.0270 0.4555 0.1278 0.039 Uiso 1 1 calc R . . C36 C 0.1384(2) 0.36414(17) 0.07523(15) 0.0303(6) Uani 1 1 d . . . H36A H 0.1359 0.3913 0.0244 0.036 Uiso 1 1 calc R . . C37 C 0.2854(2) 0.22031(17) 0.06531(15) 0.0282(5) Uani 1 1 d . . . H37A H 0.2563 0.2295 0.0195 0.034 Uiso 1 1 calc R . . H37B H 0.2814 0.1598 0.0963 0.034 Uiso 1 1 calc R . . C38 C 0.4225(2) 0.23195(17) 0.04508(14) 0.0268(5) Uani 1 1 d . . . C39 C 0.4389(3) 0.31345(18) -0.01996(15) 0.0339(6) Uani 1 1 d . . . H39A H 0.5257 0.3202 -0.0318 0.051 Uiso 1 1 calc R . . H39B H 0.3836 0.3650 -0.0067 0.051 Uiso 1 1 calc R . . H39C H 0.4179 0.3074 -0.0630 0.051 Uiso 1 1 calc R . . C40 C 0.5012(3) 0.15005(19) 0.02280(18) 0.0386(7) Uani 1 1 d . . . H40A H 0.5896 0.1534 0.0096 0.058 Uiso 1 1 calc R . . H40B H 0.4755 0.1465 -0.0198 0.058 Uiso 1 1 calc R . . H40C H 0.4887 0.0980 0.0643 0.058 Uiso 1 1 calc R . . O4 O 0.45512(16) 0.23821(12) 0.10617(10) 0.0311(4) Uani 1 1 d . . . N7 N 0.20265(19) 0.28168(14) 0.10528(12) 0.0267(4) Uani 1 1 d . . . N8 N 0.1105(2) 0.33761(15) 0.19527(12) 0.0297(5) Uani 1 1 d . . . I1 I 0.130310(18) 0.370367(12) -0.120653(11) 0.03842(6) Uani 1 1 d . . . C100 C 1.2748(4) -0.2222(3) 0.1856(2) 0.0699(11) Uani 1 1 d DU . . H10D H 1.3425 -0.1926 0.1686 0.084 Uiso 1 1 calc R . . C101 C 1.2246(4) -0.2483(3) 0.2595(2) 0.0771(12) Uani 1 1 d DU . . H10E H 1.2574 -0.2365 0.2940 0.093 Uiso 1 1 calc R . . C102 C 1.1263(4) -0.2920(3) 0.2844(2) 0.0732(11) Uani 1 1 d DU . . H10F H 1.0903 -0.3087 0.3355 0.088 Uiso 1 1 calc R . . C103 C 1.0815(4) -0.3108(2) 0.2344(2) 0.0587(9) Uani 1 1 d DU . . H10G H 1.0161 -0.3424 0.2512 0.070 Uiso 1 1 calc R . . C104 C 1.1304(3) -0.2843(2) 0.1607(2) 0.0539(8) Uani 1 1 d DU . . H10H H 1.0987 -0.2969 0.1261 0.065 Uiso 1 1 calc R . . C105 C 1.2257(3) -0.2393(3) 0.1366(2) 0.0625(10) Uani 1 1 d DU . . H10I H 1.2582 -0.2198 0.0852 0.075 Uiso 1 1 calc R . . C200 C 0.4993(7) -0.4438(5) 0.3694(4) 0.1343(11) Uani 1 1 d DU . . H20D H 0.4513 -0.4763 0.3601 0.161 Uiso 1 1 calc R . . C201 C 0.4605(7) -0.4132(5) 0.4297(4) 0.1342(11) Uani 1 1 d DU . . H20E H 0.3874 -0.4271 0.4645 0.161 Uiso 1 1 calc R . . C202 C 0.5278(7) -0.3617(5) 0.4406(4) 0.1337(11) Uani 1 1 d DU . . H20F H 0.4992 -0.3386 0.4817 0.160 Uiso 1 1 calc R . . C203 C 0.6360(7) -0.3444(5) 0.3913(4) 0.1337(11) Uani 1 1 d DU . . H20G H 0.6823 -0.3093 0.3986 0.160 Uiso 1 1 calc R . . C204 C 0.6768(7) -0.3770(5) 0.3325(4) 0.1341(11) Uani 1 1 d DU . . H20H H 0.7520 -0.3648 0.2993 0.161 Uiso 1 1 calc R . . C205 C 0.6133(7) -0.4263(5) 0.3203(4) 0.1343(11) Uani 1 1 d DU . . H20I H 0.6441 -0.4493 0.2791 0.161 Uiso 1 1 calc R . . C300 C -0.1053(7) 0.2921(4) 0.5174(3) 0.1070(17) Uani 1 1 d DU . . H30D H -0.1296 0.3417 0.5357 0.128 Uiso 1 1 calc R . . C301 C 0.0169(5) 0.2664(3) 0.4857(3) 0.0932(15) Uani 1 1 d DU . . H30E H 0.0776 0.2979 0.4821 0.112 Uiso 1 1 calc R . . C302 C 0.0507(4) 0.1957(3) 0.4595(3) 0.0811(13) Uani 1 1 d DU . . H30F H 0.1349 0.1779 0.4370 0.097 Uiso 1 1 calc R . . C303 C -0.0353(4) 0.1510(3) 0.4655(2) 0.0695(11) Uani 1 1 d DU . . H30G H -0.0107 0.1010 0.4478 0.083 Uiso 1 1 calc R . . C304 C -0.1556(4) 0.1755(3) 0.4959(2) 0.0702(11) Uani 1 1 d DU . . H30H H -0.2148 0.1433 0.4985 0.084 Uiso 1 1 calc R . . C305 C -0.1931(5) 0.2453(3) 0.5227(3) 0.0990(16) Uani 1 1 d DU . . H30I H -0.2779 0.2621 0.5448 0.119 Uiso 1 1 calc R . . C400 C -0.0392(5) 0.5344(3) 0.4337(2) 0.0745(12) Uani 1 1 d D . . H40D H -0.0667 0.5586 0.3880 0.112 Uiso 1 1 calc R . . C401 C 0.0853(5) 0.5045(3) 0.4344(3) 0.0761(13) Uani 1 1 d D . . H40G H 0.1441 0.5071 0.3893 0.091 Uiso 1 1 calc R . . C402 C 0.1253(5) 0.4704(3) 0.5006(3) 0.0743(12) Uani 1 1 d D . . H40H H 0.2119 0.4503 0.5012 0.112 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 0.01926(7) 0.02244(7) 0.03072(8) -0.00837(6) -0.00632(5) -0.00465(5) C1 0.0264(13) 0.0268(13) 0.0510(17) -0.0138(13) -0.0118(12) -0.0020(10) C2 0.0349(16) 0.0391(16) 0.062(2) -0.0296(16) -0.0041(14) -0.0008(13) C3 0.046(2) 0.063(2) 0.074(3) -0.043(2) -0.0099(18) 0.0050(17) C4 0.0326(17) 0.057(2) 0.082(3) -0.037(2) -0.0102(17) 0.0008(15) C5 0.0435(19) 0.0310(16) 0.094(3) -0.0327(18) -0.0163(18) -0.0014(13) C6 0.0398(17) 0.0252(14) 0.089(3) -0.0180(16) -0.0177(17) -0.0053(12) C7 0.0343(15) 0.0284(14) 0.0490(18) -0.0034(13) -0.0097(13) -0.0086(12) C8 0.0243(13) 0.0251(13) 0.0466(17) -0.0056(12) -0.0063(11) -0.0082(10) C9 0.0364(16) 0.0411(17) 0.0504(19) -0.0069(15) -0.0010(14) -0.0136(13) C10 0.0329(15) 0.0373(16) 0.0556(19) -0.0129(14) -0.0108(13) -0.0125(12) O1 0.0239(9) 0.0244(9) 0.0479(12) -0.0047(8) -0.0073(8) -0.0083(7) N1 0.0309(12) 0.0224(11) 0.0601(16) -0.0094(11) -0.0143(11) -0.0044(9) N2 0.0308(12) 0.0320(13) 0.0622(17) -0.0237(12) -0.0106(12) -0.0009(10) C11 0.0303(14) 0.0296(14) 0.0411(16) -0.0027(12) -0.0123(12) -0.0097(11) C12 0.0332(15) 0.0361(16) 0.0553(19) -0.0087(14) -0.0175(14) -0.0017(12) C13 0.046(2) 0.0389(18) 0.095(3) -0.0168(19) -0.026(2) -0.0054(15) C14 0.0328(17) 0.053(2) 0.082(3) -0.0102(19) -0.0170(17) -0.0060(15) C15 0.053(2) 0.0495(19) 0.0486(19) -0.0025(16) -0.0300(16) -0.0063(16) C16 0.059(2) 0.050(2) 0.0379(17) -0.0034(15) -0.0207(16) -0.0103(16) C17 0.0387(16) 0.0416(17) 0.0341(16) -0.0082(13) -0.0033(12) -0.0074(13) C18 0.0347(15) 0.0342(14) 0.0334(15) -0.0130(12) -0.0068(11) -0.0072(11) C19 0.0497(19) 0.0453(18) 0.0390(17) -0.0164(14) -0.0073(14) -0.0023(14) C20 0.0516(19) 0.0471(19) 0.057(2) -0.0200(16) -0.0187(16) -0.0152(15) O2 0.0398(11) 0.0300(10) 0.0294(10) -0.0107(8) -0.0073(8) -0.0082(8) N3 0.0386(13) 0.0346(13) 0.0347(13) -0.0010(11) -0.0128(11) -0.0087(10) N4 0.0333(13) 0.0330(13) 0.0471(15) -0.0023(11) -0.0180(11) -0.0075(10) C21 0.0360(15) 0.0317(14) 0.0335(15) -0.0001(12) -0.0126(12) -0.0162(12) C22 0.0443(17) 0.0308(15) 0.0457(17) -0.0082(13) -0.0105(14) -0.0117(12) C23 0.0377(17) 0.054(2) 0.058(2) -0.0192(17) -0.0166(15) -0.0068(14) C24 0.069(2) 0.0385(17) 0.049(2) -0.0111(15) -0.0146(17) -0.0124(16) C25 0.0497(19) 0.0301(15) 0.070(2) -0.0033(15) -0.0290(17) -0.0179(14) C26 0.0396(17) 0.0356(16) 0.071(2) 0.0042(16) -0.0250(16) -0.0197(14) C27 0.0348(16) 0.0517(19) 0.0393(17) -0.0112(14) -0.0003(13) -0.0169(14) C28 0.0203(12) 0.0380(15) 0.0450(17) -0.0139(13) -0.0011(11) -0.0087(11) C29 0.0326(17) 0.057(2) 0.086(3) -0.036(2) 0.0122(17) -0.0110(15) C30 0.0351(16) 0.0399(17) 0.0552(19) -0.0066(15) -0.0187(14) -0.0109(13) O3 0.0210(9) 0.0340(10) 0.0466(12) -0.0119(9) -0.0032(8) -0.0094(7) N5 0.0330(13) 0.0360(13) 0.0405(14) 0.0027(11) -0.0129(10) -0.0154(10) N6 0.0406(13) 0.0273(12) 0.0417(14) -0.0015(10) -0.0175(11) -0.0144(10) C31 0.0215(12) 0.0304(13) 0.0343(14) -0.0085(11) -0.0069(10) -0.0073(10) C32 0.0372(15) 0.0440(16) 0.0300(14) -0.0146(13) -0.0093(12) -0.0034(12) C33 0.064(2) 0.0496(19) 0.0453(19) -0.0237(16) -0.0163(16) -0.0064(16) C34 0.0422(19) 0.100(3) 0.0405(19) -0.028(2) 0.0018(15) -0.0204(19) C35 0.0282(13) 0.0311(14) 0.0369(15) -0.0094(12) -0.0111(11) -0.0014(11) C36 0.0270(13) 0.0308(14) 0.0328(14) -0.0063(11) -0.0101(11) -0.0045(10) C37 0.0234(12) 0.0277(13) 0.0372(15) -0.0129(11) -0.0066(11) -0.0058(10) C38 0.0217(12) 0.0292(13) 0.0304(13) -0.0092(11) -0.0044(10) -0.0065(10) C39 0.0336(15) 0.0364(15) 0.0315(14) -0.0060(12) -0.0059(11) -0.0115(12) C40 0.0287(14) 0.0372(16) 0.0477(18) -0.0171(14) -0.0017(12) -0.0025(12) O4 0.0266(9) 0.0358(10) 0.0341(10) -0.0065(8) -0.0107(8) -0.0112(8) N7 0.0200(10) 0.0287(11) 0.0324(12) -0.0093(9) -0.0061(9) -0.0050(8) N8 0.0261(11) 0.0334(12) 0.0303(12) -0.0100(10) -0.0073(9) -0.0042(9) I1 0.04464(11) 0.03167(10) 0.04494(12) -0.01487(8) -0.02014(9) -0.00109(8) C100 0.071(3) 0.072(3) 0.082(3) -0.029(2) -0.011(2) -0.035(2) C101 0.106(3) 0.073(3) 0.075(3) -0.021(2) -0.032(2) -0.039(2) C102 0.102(3) 0.065(2) 0.055(2) -0.0089(19) -0.017(2) -0.031(2) C103 0.057(2) 0.054(2) 0.069(2) -0.0174(18) -0.0127(18) -0.0181(17) C104 0.0421(18) 0.062(2) 0.064(2) -0.0267(18) -0.0133(16) -0.0071(15) C105 0.054(2) 0.076(3) 0.063(2) -0.028(2) -0.0019(17) -0.0200(18) C200 0.138(3) 0.164(3) 0.125(3) -0.067(2) -0.018(2) -0.043(2) C201 0.137(3) 0.163(3) 0.125(3) -0.067(2) -0.0178(19) -0.043(2) C202 0.138(3) 0.162(3) 0.125(3) -0.066(2) -0.0195(19) -0.042(2) C203 0.137(3) 0.161(3) 0.125(3) -0.063(2) -0.021(2) -0.043(2) C204 0.136(3) 0.163(3) 0.124(3) -0.063(2) -0.0193(19) -0.042(2) C205 0.138(3) 0.164(3) 0.124(3) -0.066(2) -0.0178(19) -0.043(2) C300 0.185(5) 0.077(3) 0.069(3) -0.036(3) -0.011(3) -0.037(3) C301 0.128(4) 0.094(3) 0.076(3) 0.018(2) -0.053(3) -0.072(3) C302 0.061(2) 0.078(3) 0.072(3) 0.024(2) -0.019(2) -0.016(2) C303 0.087(3) 0.054(2) 0.055(2) -0.0075(18) -0.003(2) -0.015(2) C304 0.072(2) 0.071(3) 0.068(3) -0.001(2) -0.017(2) -0.033(2) C305 0.094(3) 0.086(3) 0.079(3) -0.013(3) 0.021(3) -0.009(3) C400 0.101(4) 0.064(3) 0.066(3) -0.030(2) -0.013(3) -0.018(3) C401 0.097(4) 0.073(3) 0.068(3) -0.037(2) 0.000(3) -0.029(3) C402 0.087(3) 0.064(3) 0.083(3) -0.038(2) -0.011(3) -0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O3 2.2787(18) . ? Ce1 O2 2.2858(18) . ? Ce1 O1 2.3316(18) . ? Ce1 O4 2.3365(18) . ? Ce1 C1 2.798(3) . ? Ce1 C11 2.806(3) . ? C1 N2 1.363(4) . ? C1 N1 1.366(4) . ? C2 N2 1.464(4) . ? C2 C4 1.525(4) . ? C2 C3 1.526(5) . ? C5 C6 1.329(5) . ? C5 N2 1.392(4) . ? C6 N1 1.388(4) . ? C7 N1 1.456(4) . ? C7 C8 1.551(4) . ? C8 O1 1.390(3) . ? C8 C10 1.527(4) . ? C8 C9 1.537(4) . ? C11 N3 1.360(4) . ? C11 N4 1.364(3) . ? C12 N4 1.471(4) . ? C12 C13 1.524(4) . ? C12 C14 1.525(4) . ? C15 C16 1.331(5) . ? C15 N4 1.381(4) . ? C16 N3 1.383(4) . ? C17 N3 1.467(4) . ? C17 C18 1.549(4) . ? C18 O2 1.387(3) . ? C18 C20 1.535(4) . ? C18 C19 1.540(4) . ? C21 N6 1.331(4) . ? C21 N5 1.335(4) . ? C22 N6 1.483(4) . ? C22 C24 1.512(4) . ? C22 C23 1.518(4) . ? C25 C26 1.343(5) . ? C25 N6 1.385(4) . ? C26 N5 1.381(4) . ? C27 N5 1.465(4) . ? C27 C28 1.552(4) . ? C28 O3 1.379(3) . ? C28 C30 1.527(4) . ? C28 C29 1.528(4) . ? C31 N7 1.330(3) . ? C31 N8 1.332(3) . ? C32 N8 1.483(3) . ? C32 C34 1.514(4) . ? C32 C33 1.516(4) . ? C35 C36 1.351(4) . ? C35 N8 1.385(3) . ? C36 N7 1.376(3) . ? C37 N7 1.467(3) . ? C37 C38 1.550(3) . ? C38 O4 1.390(3) . ? C38 C39 1.529(4) . ? C38 C40 1.537(4) . ? C100 C105 1.370(5) . ? C100 C101 1.372(5) . ? C101 C102 1.388(5) . ? C102 C103 1.373(5) . ? C103 C104 1.366(5) . ? C104 C105 1.373(5) . ? C200 C201 1.362(7) . ? C200 C205 1.426(7) . ? C201 C202 1.391(7) . ? C202 C203 1.376(7) . ? C203 C204 1.354(7) . ? C204 C205 1.342(7) . ? C300 C301 1.373(6) . ? C300 C305 1.389(6) . ? C301 C302 1.358(6) . ? C302 C303 1.341(5) . ? C303 C304 1.344(5) . ? C304 C305 1.349(6) . ? C400 C401 1.368(5) . ? C400 C402 1.384(5) 2_566 ? C401 C402 1.376(5) . ? C402 C400 1.384(5) 2_566 ? 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 O3 Ce1 O2 101.76(7) . . ? O3 Ce1 O1 160.48(7) . . ? O2 Ce1 O1 97.75(7) . . ? O3 Ce1 O4 89.62(7) . . ? O2 Ce1 O4 99.07(7) . . ? O1 Ce1 O4 86.97(6) . . ? O3 Ce1 C1 91.64(7) . . ? O2 Ce1 C1 149.82(8) . . ? O1 Ce1 C1 71.27(7) . . ? O4 Ce1 C1 108.03(8) . . ? O3 Ce1 C11 91.99(8) . . ? O2 Ce1 C11 72.53(8) . . ? O1 Ce1 C11 94.18(7) . . ? O4 Ce1 C11 171.60(8) . . ? C1 Ce1 C11 80.17(8) . . ? N2 C1 N1 103.0(2) . . ? N2 C1 Ce1 137.6(2) . . ? N1 C1 Ce1 119.10(18) . . ? N2 C2 C4 110.3(3) . . ? N2 C2 C3 110.9(3) . . ? C4 C2 C3 111.2(3) . . ? C6 C5 N2 106.5(3) . . ? C5 C6 N1 107.2(3) . . ? N1 C7 C8 113.7(2) . . ? O1 C8 C10 111.1(2) . . ? O1 C8 C9 109.3(2) . . ? C10 C8 C9 109.7(2) . . ? O1 C8 C7 109.7(2) . . ? C10 C8 C7 110.1(2) . . ? C9 C8 C7 106.7(2) . . ? C8 O1 Ce1 141.63(16) . . ? C1 N1 C6 111.5(3) . . ? C1 N1 C7 124.2(2) . . ? C6 N1 C7 124.3(3) . . ? C1 N2 C5 111.8(3) . . ? C1 N2 C2 123.4(2) . . ? C5 N2 C2 124.8(3) . . ? N3 C11 N4 103.0(2) . . ? N3 C11 Ce1 119.94(18) . . ? N4 C11 Ce1 135.1(2) . . ? N4 C12 C13 110.6(3) . . ? N4 C12 C14 111.0(3) . . ? C13 C12 C14 111.3(3) . . ? C16 C15 N4 106.9(3) . . ? C15 C16 N3 106.8(3) . . ? N3 C17 C18 113.4(2) . . ? O2 C18 C20 110.3(2) . . ? O2 C18 C19 110.1(2) . . ? C20 C18 C19 109.6(3) . . ? O2 C18 C17 110.0(2) . . ? C20 C18 C17 111.0(2) . . ? C19 C18 C17 105.8(2) . . ? C18 O2 Ce1 142.04(16) . . ? C11 N3 C16 111.7(3) . . ? C11 N3 C17 123.5(2) . . ? C16 N3 C17 124.6(3) . . ? C11 N4 C15 111.6(3) . . ? C11 N4 C12 122.6(3) . . ? C15 N4 C12 125.7(3) . . ? N6 C21 N5 108.8(2) . . ? N6 C22 C24 110.5(3) . . ? N6 C22 C23 109.4(3) . . ? C24 C22 C23 112.4(3) . . ? C26 C25 N6 107.1(3) . . ? C25 C26 N5 107.6(3) . . ? N5 C27 C28 112.5(2) . . ? O3 C28 C30 110.2(2) . . ? O3 C28 C29 111.3(2) . . ? C30 C28 C29 109.6(3) . . ? O3 C28 C27 109.1(2) . . ? C30 C28 C27 110.3(2) . . ? C29 C28 C27 106.3(3) . . ? C28 O3 Ce1 165.19(17) . . ? C21 N5 C26 108.2(3) . . ? C21 N5 C27 125.4(2) . . ? C26 N5 C27 125.9(3) . . ? C21 N6 C25 108.4(3) . . ? C21 N6 C22 123.3(2) . . ? C25 N6 C22 128.3(3) . . ? N7 C31 N8 108.1(2) . . ? N8 C32 C34 109.8(2) . . ? N8 C32 C33 109.8(3) . . ? C34 C32 C33 112.4(3) . . ? C36 C35 N8 106.6(2) . . ? C35 C36 N7 107.3(2) . . ? N7 C37 C38 111.9(2) . . ? O4 C38 C39 110.4(2) . . ? O4 C38 C40 111.0(2) . . ? C39 C38 C40 109.8(2) . . ? O4 C38 C37 109.5(2) . . ? C39 C38 C37 110.4(2) . . ? C40 C38 C37 105.6(2) . . ? C38 O4 Ce1 139.16(16) . . ? C31 N7 C36 109.0(2) . . ? C31 N7 C37 123.8(2) . . ? C36 N7 C37 127.1(2) . . ? C31 N8 C35 109.0(2) . . ? C31 N8 C32 125.1(2) . . ? C35 N8 C32 125.7(2) . . ? C105 C100 C101 118.9(4) . . ? C100 C101 C102 120.5(4) . . ? C103 C102 C101 119.4(4) . . ? C104 C103 C102 120.3(4) . . ? C103 C104 C105 119.7(4) . . ? C100 C105 C104 121.1(4) . . ? C201 C200 C205 118.8(7) . . ? C200 C201 C202 120.2(7) . . ? C203 C202 C201 119.5(7) . . ? C204 C203 C202 120.4(7) . . ? C205 C204 C203 121.4(8) . . ? C204 C205 C200 119.6(7) . . ? C301 C300 C305 119.7(5) . . ? C302 C301 C300 119.7(4) . . ? C303 C302 C301 119.8(5) . . ? C302 C303 C304 121.5(4) . . ? C303 C304 C305 120.7(4) . . ? C304 C305 C300 118.7(5) . . ? C401 C400 C402 120.2(4) . 2_566 ? C400 C401 C402 120.0(4) . . ? C401 C402 C400 119.8(4) . 2_566 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.827 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.070 #===END of CIF