Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chem. Comm.' # 1. SUBMISSION DETAILS loop_ _publ_author_name 'Ephritikhine, M.' 'Guillaneux, Denis' 'Iveson, Peter B.' 'Madic, C.' 'Nierlich, Martine' 'Riviere, Christelle' 'Thuery, Pierre' _publ_contact_author 'Dr M Ephritikhine' _publ_contact_address ; Dr M Ephritikhine Laboratoire de Chimie de coordinati Service de Chimie Moleculaire CEA Saclay, Batiment 125 Gif sur Yvette F91191 FRANCE ; _publ_contact_author_email 'EPHRI@DRECAM.CEA.FR' _publ_section_title ; ; _publ_requested_journal 'Chem. Comm.' data_Ce(MeBTP)3I3.9C5H5N _database_code_CSD 161597 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H90 Ce I3 N30' _chemical_formula_weight 2112.74 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' 'I' 'I' -0.4742 1.8119 '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 P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 14.078(3) _cell_length_b 13.889(3) _cell_length_c 24.741(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.94(3) _cell_angle_gamma 90.00 _cell_volume 4732.9(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 28115 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 24.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method ? _exptl_crystal_F_000 2114 _exptl_absorpt_coefficient_mu 1.520 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 28115 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 24.68 _reflns_number_total 7635 _reflns_number_gt 5824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and expanded by subsequent Fourier-difference synthesis. One pyridine molecule has been found disordered on two positions, which have been fixed in the subsequent refinement cycles. All non-hydrogen atoms were refined with anisotropic displacement parameters, except those in the disordered pyridine molecule. All hydrogen atoms, except those in the disordered pyridine molecule, were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH3) times that of the parent atom. The highest residual electron density peak is located near the disordered solvent. 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^)+(0.0578P)^2^+14.4497P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7635 _refine_ls_number_parameters 508 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 24.68 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.240 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.098 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 0.2500 0.16122(3) 0.2500 0.02774(13) Uani 1 2 d S . . I1 I 0.7500 0.14520(6) 0.2500 0.0779(3) Uani 1 2 d S . . I2 I -0.09461(4) -0.20274(4) 0.449829(18) 0.05328(16) Uani 1 1 d . . . N1A N 0.2500 -0.0289(4) 0.2500 0.0277(14) Uani 1 2 d S . . N2A N 0.4671(3) 0.1265(4) 0.3430(2) 0.0387(12) Uani 1 1 d . . . N3A N 0.3952(3) 0.0725(3) 0.31338(19) 0.0329(11) Uani 1 1 d . . . N4A N 0.4962(3) -0.0670(4) 0.3233(2) 0.0379(12) Uani 1 1 d . . . C1A C 0.3280(4) -0.0780(4) 0.2768(2) 0.0356(13) Uani 1 1 d . . . C2A C 0.3302(5) -0.1789(5) 0.2773(3) 0.0451(16) Uani 1 1 d . . . H2AA H 0.3849 -0.2117 0.2957 0.054 Uiso 1 1 calc R . . C3A C 0.2500 -0.2283(7) 0.2500 0.050(2) Uani 1 2 d S . . H3AA H 0.2500 -0.2953 0.2500 0.061 Uiso 1 2 calc SR . . C4A C 0.4111(4) -0.0206(4) 0.3063(2) 0.0338(13) Uani 1 1 d . . . C5A C 0.5687(4) -0.0126(5) 0.3496(3) 0.0406(15) Uani 1 1 d . . . C6A C 0.5522(4) 0.0861(5) 0.3618(3) 0.0417(15) Uani 1 1 d . . . C7A C 0.6682(5) -0.0549(5) 0.3649(3) 0.0574(19) Uani 1 1 d . . . H7AA H 0.6661 -0.1212 0.3538 0.086 Uiso 1 1 calc R . . H7AB H 0.6910 -0.0508 0.4042 0.086 Uiso 1 1 calc R . . H7AC H 0.7113 -0.0200 0.3467 0.086 Uiso 1 1 calc R . . C8A C 0.6295(5) 0.1473(5) 0.3953(3) 0.058(2) Uani 1 1 d . . . H8AA H 0.6043 0.2107 0.3989 0.088 Uiso 1 1 calc R . . H8AB H 0.6836 0.1513 0.3774 0.088 Uiso 1 1 calc R . . H8AC H 0.6503 0.1194 0.4313 0.088 Uiso 1 1 calc R . . N1B N 0.2724(3) 0.2576(3) 0.34302(18) 0.0297(10) Uani 1 1 d . . . N2B N 0.0779(3) 0.0413(3) 0.3055(2) 0.0354(11) Uani 1 1 d . . . N3B N 0.1424(3) 0.1145(3) 0.3195(2) 0.0336(11) Uani 1 1 d . . . N4B N 0.0609(3) 0.1685(4) 0.3892(2) 0.0355(11) Uani 1 1 d . . . N5B N 0.4376(4) 0.3109(3) 0.2307(2) 0.0360(11) Uani 1 1 d . . . N6B N 0.3825(3) 0.2970(3) 0.26906(19) 0.0319(11) Uani 1 1 d . . . N7B N 0.5003(4) 0.3705(4) 0.3386(2) 0.0396(12) Uani 1 1 d . . . C1B C 0.3465(4) 0.3200(4) 0.3584(2) 0.0339(13) Uani 1 1 d . . . C2B C 0.3603(5) 0.3720(5) 0.4071(3) 0.0455(16) Uani 1 1 d . . . H2BA H 0.4137 0.4123 0.4172 0.055 Uiso 1 1 calc R . . C3B C 0.2936(5) 0.3629(5) 0.4404(3) 0.0518(18) Uani 1 1 d . . . H3BA H 0.2996 0.3998 0.4723 0.062 Uiso 1 1 calc R . . C4B C 0.2170(5) 0.2979(5) 0.4260(3) 0.0444(16) Uani 1 1 d . . . H4BA H 0.1722 0.2894 0.4484 0.053 Uiso 1 1 calc R . . C5B C 0.2095(4) 0.2462(4) 0.3770(2) 0.0342(13) Uani 1 1 d . . . C6B C 0.1325(4) 0.1722(4) 0.3604(2) 0.0323(13) Uani 1 1 d . . . C7B C -0.0024(4) 0.0979(4) 0.3755(2) 0.0347(13) Uani 1 1 d . . . C8B C 0.0078(4) 0.0306(4) 0.3332(2) 0.0374(14) Uani 1 1 d . . . C9B C 0.4126(4) 0.3301(4) 0.3192(2) 0.0330(13) Uani 1 1 d . . . C10B C 0.5570(4) 0.3795(5) 0.3022(3) 0.0403(15) Uani 1 1 d . . . C11B C 0.5225(4) 0.3534(4) 0.2461(2) 0.0377(14) Uani 1 1 d . . . C12B C -0.0834(5) 0.0894(5) 0.4057(3) 0.0466(16) Uani 1 1 d . . . H12B H -0.0786 0.1404 0.4324 0.070 Uiso 1 1 calc R . . H12C H -0.0793 0.0284 0.4243 0.070 Uiso 1 1 calc R . . H12D H -0.1444 0.0940 0.3800 0.070 Uiso 1 1 calc R . . C13B C -0.0599(5) -0.0515(5) 0.3170(3) 0.0438(15) Uani 1 1 d . . . H13B H -0.0403 -0.0875 0.2880 0.066 Uiso 1 1 calc R . . H13C H -0.1246 -0.0275 0.3041 0.066 Uiso 1 1 calc R . . H13D H -0.0586 -0.0926 0.3483 0.066 Uiso 1 1 calc R . . C14B C 0.6600(5) 0.4109(6) 0.3228(3) 0.060(2) Uani 1 1 d . . . H14B H 0.6700 0.4253 0.3616 0.089 Uiso 1 1 calc R . . H14C H 0.6727 0.4674 0.3031 0.089 Uiso 1 1 calc R . . H14D H 0.7031 0.3602 0.3171 0.089 Uiso 1 1 calc R . . C15B C 0.5787(5) 0.3712(5) 0.2021(3) 0.0528(18) Uani 1 1 d . . . H15B H 0.5423 0.3483 0.1673 0.079 Uiso 1 1 calc R . . H15C H 0.6396 0.3376 0.2110 0.079 Uiso 1 1 calc R . . H15D H 0.5905 0.4389 0.1996 0.079 Uiso 1 1 calc R . . C1 C 0.2393(8) 0.6247(7) 0.5218(4) 0.081(3) Uani 1 1 d . . . H1A H 0.2893 0.6560 0.5094 0.097 Uiso 1 1 calc R . . C2 C 0.1672(8) 0.6768(7) 0.5327(4) 0.080(3) Uani 1 1 d . . . H2A H 0.1680 0.7432 0.5281 0.096 Uiso 1 1 calc R . . C3 C 0.0927(7) 0.6356(8) 0.5502(4) 0.080(3) Uani 1 1 d . . . H3A H 0.0417 0.6731 0.5570 0.096 Uiso 1 1 calc R . . C4 C 0.0927(9) 0.5381(9) 0.5580(4) 0.096(3) Uani 1 1 d . . . H4A H 0.0432 0.5072 0.5709 0.116 Uiso 1 1 calc R . . C5 C 0.1733(10) 0.4862(7) 0.5451(4) 0.089(3) Uani 1 1 d . . . H5A H 0.1756 0.4196 0.5492 0.107 Uiso 1 1 calc R . . C6 C 0.3359(7) 0.5352(7) 0.1906(5) 0.086(3) Uani 1 1 d . . . H6A H 0.2885 0.4896 0.1931 0.104 Uiso 1 1 calc R . . C7 C 0.3344(16) 0.5706(10) 0.1408(8) 0.161(7) Uani 1 1 d . . . H7A H 0.2850 0.5510 0.1118 0.193 Uiso 1 1 calc R . . C8 C 0.3947(11) 0.6279(12) 0.1308(7) 0.140(5) Uani 1 1 d . . . H8 H 0.3909 0.6497 0.0949 0.167 Uiso 1 1 calc R . . C9 C 0.4610(8) 0.6571(8) 0.1687(5) 0.088(3) Uani 1 1 d . . . H9A H 0.5071 0.6990 0.1599 0.106 Uiso 1 1 calc R . . C10 C 0.4694(8) 0.6292(9) 0.2243(7) 0.116(5) Uani 1 1 d . . . H10 H 0.5175 0.6538 0.2525 0.140 Uiso 1 1 calc R . . C11 C 0.7436(9) -0.0396(8) 0.5296(4) 0.095(4) Uani 1 1 d . . . H11A H 0.7412 -0.0951 0.5083 0.114 Uiso 1 1 calc R . . C12 C 0.6704(9) -0.0169(9) 0.5561(5) 0.102(4) Uani 1 1 d . . . H12A H 0.6171 -0.0579 0.5515 0.122 Uiso 1 1 calc R . . C13 C 0.6709(9) 0.0596(8) 0.5879(5) 0.100(4) Uani 1 1 d . . . H13A H 0.6221 0.0708 0.6073 0.120 Uiso 1 1 calc R . . C14 C 0.7437(11) 0.1187(10) 0.5904(5) 0.119(5) Uani 1 1 d . . . H14A H 0.7418 0.1757 0.6099 0.143 Uiso 1 1 calc R . . C15 C 0.8228(9) 0.1047(9) 0.5671(5) 0.100(3) Uani 1 1 d . . . H15A H 0.8746 0.1477 0.5721 0.120 Uiso 1 1 calc R . . C16 C -0.2246(5) -0.3580(5) 0.2969(3) 0.0509(17) Uani 1 1 d . . . H16A H -0.2072 -0.3913 0.3300 0.061 Uiso 1 1 calc R . . C17 C -0.2231(5) -0.2602(5) 0.2984(3) 0.0538(18) Uani 1 1 d . . . H17A H -0.2042 -0.2273 0.3316 0.065 Uiso 1 1 calc R . . C18 C -0.2500 -0.2122(8) 0.2500 0.069(3) Uani 1 2 d S . . H18A H -0.2500 -0.1452 0.2500 0.082 Uiso 1 2 calc SR . . N1 N 0.2438(7) 0.5299(7) 0.5277(3) 0.094(3) Uani 1 1 d . . . N2 N 0.3944(9) 0.5561(8) 0.2355(4) 0.108(3) Uani 1 1 d . . . N3 N 0.8205(8) 0.0227(10) 0.5357(4) 0.118(3) Uani 1 1 d U . . N4 N -0.2500 -0.4089(6) 0.2500 0.057(2) Uani 1 2 d S . . N5 N 0.5794 -0.3299 0.3955 0.120 Uiso 0.50 1 d P A 1 C19A C 0.4913 -0.3765 0.3829 0.120 Uiso 0.50 1 d P A 1 C20A C 0.4222 -0.3591 0.4137 0.120 Uiso 0.50 1 d P A 1 C21A C 0.4411 -0.2951 0.4571 0.120 Uiso 0.50 1 d P A 1 C22A C 0.5292 -0.2485 0.4697 0.120 Uiso 0.50 1 d P A 1 C23A C 0.5983 -0.2659 0.4389 0.120 Uiso 0.50 1 d P A 1 N6 N 0.5741 -0.3485 0.4035 0.120 Uiso 0.50 1 d P B 2 C19B C 0.5416 -0.2551 0.4050 0.120 Uiso 0.50 1 d P B 2 C20B C 0.4727 -0.2329 0.4353 0.120 Uiso 0.50 1 d P B 2 C21B C 0.4362 -0.3041 0.4640 0.120 Uiso 0.50 1 d P B 2 C22B C 0.4687 -0.3974 0.4625 0.120 Uiso 0.50 1 d P B 2 C23B C 0.5376 -0.4196 0.4322 0.120 Uiso 0.50 1 d P B 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 Ce 0.0279(2) 0.0255(3) 0.0304(3) 0.000 0.00730(18) 0.000 I1 0.1109(7) 0.0554(5) 0.0559(5) 0.000 -0.0094(4) 0.000 I2 0.0610(3) 0.0605(3) 0.0387(3) 0.0076(2) 0.0112(2) 0.0032(2) N1A 0.028(3) 0.023(3) 0.033(4) 0.000 0.008(3) 0.000 N2A 0.036(3) 0.035(3) 0.043(3) -0.001(2) 0.002(2) -0.003(2) N3A 0.036(3) 0.030(3) 0.032(3) -0.002(2) 0.004(2) 0.002(2) N4A 0.035(3) 0.034(3) 0.046(3) 0.005(2) 0.011(2) 0.007(2) C1A 0.036(3) 0.033(3) 0.040(3) 0.004(3) 0.013(3) 0.003(3) C2A 0.041(4) 0.036(4) 0.058(4) 0.008(3) 0.008(3) 0.002(3) C3A 0.053(6) 0.028(5) 0.071(7) 0.000 0.013(5) 0.000 C4A 0.033(3) 0.041(4) 0.029(3) 0.005(3) 0.010(2) 0.005(3) C5A 0.037(3) 0.041(4) 0.043(4) 0.008(3) 0.005(3) 0.003(3) C6A 0.037(3) 0.044(4) 0.041(4) 0.007(3) 0.001(3) 0.002(3) C7A 0.036(4) 0.055(5) 0.073(5) 0.005(4) -0.006(3) 0.011(3) C8A 0.047(4) 0.048(5) 0.071(5) -0.004(4) -0.010(4) -0.002(3) N1B 0.034(3) 0.026(3) 0.029(2) 0.000(2) 0.005(2) 0.003(2) N2B 0.037(3) 0.033(3) 0.040(3) 0.004(2) 0.015(2) -0.002(2) N3B 0.033(3) 0.032(3) 0.038(3) 0.001(2) 0.011(2) -0.003(2) N4B 0.037(3) 0.035(3) 0.036(3) 0.003(2) 0.009(2) -0.001(2) N5B 0.037(3) 0.030(3) 0.043(3) 0.003(2) 0.011(2) -0.006(2) N6B 0.034(3) 0.028(3) 0.035(3) 0.000(2) 0.010(2) -0.002(2) N7B 0.038(3) 0.038(3) 0.043(3) -0.002(2) 0.008(2) -0.005(2) C1B 0.035(3) 0.028(3) 0.038(3) 0.000(3) 0.007(3) 0.001(2) C2B 0.059(4) 0.039(4) 0.041(4) -0.009(3) 0.015(3) -0.015(3) C3B 0.066(5) 0.051(4) 0.043(4) -0.015(3) 0.020(3) -0.010(3) C4B 0.055(4) 0.041(4) 0.042(4) -0.006(3) 0.021(3) -0.006(3) C5B 0.038(3) 0.031(3) 0.036(3) 0.000(3) 0.014(3) 0.003(2) C6B 0.035(3) 0.032(3) 0.032(3) 0.003(3) 0.010(2) 0.004(2) C7B 0.036(3) 0.040(4) 0.029(3) 0.007(3) 0.009(2) 0.004(3) C8B 0.041(3) 0.035(3) 0.036(3) 0.007(3) 0.009(3) 0.000(3) C9B 0.036(3) 0.026(3) 0.036(3) -0.002(3) 0.005(3) -0.003(2) C10B 0.037(3) 0.038(4) 0.047(4) 0.001(3) 0.012(3) -0.007(3) C11B 0.039(3) 0.034(4) 0.041(4) -0.002(3) 0.013(3) -0.003(3) C12B 0.046(4) 0.059(5) 0.038(4) -0.002(3) 0.015(3) -0.008(3) C13B 0.048(4) 0.045(4) 0.042(4) -0.006(3) 0.018(3) -0.010(3) C14B 0.052(4) 0.066(5) 0.060(5) -0.005(4) 0.013(4) -0.025(4) C15B 0.051(4) 0.055(5) 0.057(4) -0.004(3) 0.021(3) -0.019(3) C1 0.112(8) 0.072(7) 0.067(6) -0.007(5) 0.035(5) 0.009(6) C2 0.104(7) 0.072(6) 0.067(6) 0.011(5) 0.026(5) 0.024(5) C3 0.085(7) 0.089(8) 0.063(6) 0.022(5) 0.008(5) 0.022(5) C4 0.113(9) 0.115(10) 0.053(6) 0.005(6) -0.002(5) -0.039(7) C5 0.149(11) 0.046(5) 0.059(6) -0.013(4) -0.009(6) 0.004(6) C6 0.077(6) 0.062(6) 0.109(8) 0.024(6) -0.005(6) -0.013(5) C7 0.25(2) 0.070(9) 0.156(16) 0.015(9) 0.018(14) -0.018(11) C8 0.131(12) 0.117(13) 0.155(14) -0.025(11) -0.007(11) -0.004(10) C9 0.083(7) 0.087(8) 0.093(8) -0.001(6) 0.019(6) 0.004(6) C10 0.061(6) 0.106(9) 0.166(13) -0.048(9) -0.013(7) 0.043(6) C11 0.140(10) 0.085(7) 0.068(6) 0.034(5) 0.040(6) 0.050(7) C12 0.113(9) 0.103(9) 0.108(8) 0.035(7) 0.063(7) 0.018(7) C13 0.118(9) 0.085(8) 0.127(9) 0.022(7) 0.096(8) 0.039(7) C14 0.166(13) 0.103(10) 0.108(9) 0.014(7) 0.071(9) 0.047(9) C15 0.111(9) 0.111(9) 0.082(7) 0.043(7) 0.031(6) 0.030(7) C16 0.049(4) 0.058(5) 0.046(4) 0.001(3) 0.010(3) -0.001(3) C17 0.051(4) 0.054(5) 0.051(4) -0.009(4) -0.004(3) 0.000(3) C18 0.067(7) 0.045(7) 0.078(8) 0.000 -0.020(6) 0.000 N1 0.127(8) 0.080(6) 0.074(6) -0.017(5) 0.018(5) 0.007(6) N2 0.126(8) 0.107(8) 0.095(7) 0.016(6) 0.029(6) 0.071(7) N3 0.129(7) 0.132(7) 0.095(6) 0.047(6) 0.028(5) 0.039(6) N4 0.072(6) 0.044(5) 0.050(5) 0.000 0.002(4) 0.000 _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 N3B 2.598(5) . ? Ce N3B 2.598(5) 2 ? Ce N3A 2.613(5) 2 ? Ce N3A 2.613(5) . ? Ce N1B 2.624(4) 2 ? Ce N1B 2.624(4) . ? Ce N6B 2.625(5) 2 ? Ce N6B 2.625(5) . ? Ce N1A 2.641(6) . ? N1A C1A 1.345(7) 2 ? N1A C1A 1.345(7) . ? N2A C6A 1.317(8) . ? N2A N3A 1.349(7) . ? N3A C4A 1.330(7) . ? N4A C5A 1.328(8) . ? N4A C4A 1.348(7) . ? C1A C2A 1.400(8) . ? C1A C4A 1.478(8) . ? C2A C3A 1.373(8) . ? C3A C2A 1.373(8) 2 ? C5A C6A 1.434(9) . ? C5A C7A 1.493(8) . ? C6A C8A 1.490(9) . ? N1B C5B 1.350(7) . ? N1B C1B 1.349(7) . ? N2B C8B 1.322(7) . ? N2B N3B 1.358(7) . ? N3B C6B 1.321(7) . ? N4B C7B 1.321(8) . ? N4B C6B 1.350(7) . ? N5B C11B 1.317(7) . ? N5B N6B 1.358(6) . ? N6B C9B 1.308(7) . ? N7B C10B 1.328(8) . ? N7B C9B 1.350(7) . ? C1B C2B 1.384(8) . ? C1B C9B 1.483(8) . ? C2B C3B 1.377(9) . ? C3B C4B 1.394(9) . ? C4B C5B 1.394(8) . ? C5B C6B 1.488(8) . ? C7B C8B 1.433(8) . ? C7B C12B 1.492(8) . ? C8B C13B 1.488(8) . ? C10B C11B 1.419(9) . ? C10B C14B 1.499(9) . ? C11B C15B 1.495(8) . ? C1 C2 1.318(12) . ? C1 N1 1.325(12) . ? C2 C3 1.342(13) . ? C3 C4 1.369(14) . ? C4 C5 1.436(15) . ? C5 N1 1.309(13) . ? C6 N2 1.271(13) . ? C6 C7 1.324(18) . ? C7 C8 1.226(19) . ? C8 C9 1.245(16) . ? C9 C10 1.411(17) . ? C10 N2 1.531(16) . ? C11 C12 1.367(13) . ? C11 N3 1.370(15) . ? C12 C13 1.322(15) . ? C13 C14 1.304(17) . ? C14 C15 1.371(15) . ? C15 N3 1.375(15) . ? C16 N4 1.342(8) . ? C16 C17 1.358(10) . ? C17 C18 1.354(9) . ? C18 C17 1.354(9) 2_455 ? N4 C16 1.342(8) 2_455 ? N5 C23A 1.3760 . ? N5 C19A 1.3761 . ? C19A C20A 1.3759 . ? C20A C21A 1.3760 . ? C21A C22A 1.3760 . ? C22A C23A 1.3758 . ? N6 C19B 1.3780 . ? N6 C23B 1.3780 . ? C19B C20B 1.3778 . ? C20B C21B 1.3779 . ? C21B C22B 1.3778 . ? C22B C23B 1.3780 . ? 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 N3B Ce N3B 151.1(2) . 2 ? N3B Ce N3A 77.79(15) . 2 ? N3B Ce N3A 88.61(15) 2 2 ? N3B Ce N3A 88.61(15) . . ? N3B Ce N3A 77.79(15) 2 . ? N3A Ce N3A 123.7(2) 2 . ? N3B Ce N1B 136.64(14) . 2 ? N3B Ce N1B 61.82(14) 2 2 ? N3A Ce N1B 77.13(14) 2 2 ? N3A Ce N1B 134.75(14) . 2 ? N3B Ce N1B 61.83(14) . . ? N3B Ce N1B 136.64(14) 2 . ? N3A Ce N1B 134.74(14) 2 . ? N3A Ce N1B 77.13(14) . . ? N1B Ce N1B 118.67(19) 2 . ? N3B Ce N6B 78.95(15) . 2 ? N3B Ce N6B 123.40(15) 2 2 ? N3A Ce N6B 78.03(15) 2 2 ? N3A Ce N6B 152.24(14) . 2 ? N1B Ce N6B 61.59(14) 2 2 ? N1B Ce N6B 75.12(14) . 2 ? N3B Ce N6B 123.41(15) . . ? N3B Ce N6B 78.95(15) 2 . ? N3A Ce N6B 152.24(15) 2 . ? N3A Ce N6B 78.03(15) . . ? N1B Ce N6B 75.12(14) 2 . ? N1B Ce N6B 61.60(14) . . ? N6B Ce N6B 88.2(2) 2 . ? N3B Ce N1A 75.53(11) . . ? N3B Ce N1A 75.53(11) 2 . ? N3A Ce N1A 61.85(10) 2 . ? N3A Ce N1A 61.85(10) . . ? N1B Ce N1A 120.66(10) 2 . ? N1B Ce N1A 120.66(10) . . ? N6B Ce N1A 135.90(10) 2 . ? N6B Ce N1A 135.90(10) . . ? C1A N1A C1A 119.0(7) 2 . ? C1A N1A Ce 120.5(3) 2 . ? C1A N1A Ce 120.5(3) . . ? C6A N2A N3A 118.7(5) . . ? C4A N3A N2A 119.0(5) . . ? C4A N3A Ce 120.8(4) . . ? N2A N3A Ce 118.0(3) . . ? C5A N4A C4A 115.2(5) . . ? N1A C1A C2A 121.7(6) . . ? N1A C1A C4A 116.8(5) . . ? C2A C1A C4A 121.4(5) . . ? C3A C2A C1A 118.8(6) . . ? C2A C3A C2A 119.9(9) . 2 ? N3A C4A N4A 125.9(5) . . ? N3A C4A C1A 116.9(5) . . ? N4A C4A C1A 117.2(5) . . ? N4A C5A C6A 120.4(5) . . ? N4A C5A C7A 119.1(6) . . ? C6A C5A C7A 120.5(6) . . ? N2A C6A C5A 120.5(6) . . ? N2A C6A C8A 117.4(6) . . ? C5A C6A C8A 122.1(6) . . ? C5B N1B C1B 118.0(5) . . ? C5B N1B Ce 120.7(4) . . ? C1B N1B Ce 121.3(4) . . ? C8B N2B N3B 118.9(5) . . ? C6B N3B N2B 118.6(5) . . ? C6B N3B Ce 121.5(4) . . ? N2B N3B Ce 117.9(3) . . ? C7B N4B C6B 115.6(5) . . ? C11B N5B N6B 118.5(5) . . ? C9B N6B N5B 119.5(5) . . ? C9B N6B Ce 120.1(4) . . ? N5B N6B Ce 117.6(3) . . ? C10B N7B C9B 115.6(5) . . ? N1B C1B C2B 122.8(5) . . ? N1B C1B C9B 115.5(5) . . ? C2B C1B C9B 121.7(5) . . ? C3B C2B C1B 118.9(6) . . ? C2B C3B C4B 119.5(6) . . ? C3B C4B C5B 118.2(6) . . ? N1B C5B C4B 122.6(5) . . ? N1B C5B C6B 116.3(5) . . ? C4B C5B C6B 121.1(5) . . ? N3B C6B N4B 126.1(5) . . ? N3B C6B C5B 116.4(5) . . ? N4B C6B C5B 117.5(5) . . ? N4B C7B C8B 120.4(5) . . ? N4B C7B C12B 118.4(5) . . ? C8B C7B C12B 121.2(6) . . ? N2B C8B C7B 120.3(5) . . ? N2B C8B C13B 116.9(5) . . ? C7B C8B C13B 122.8(5) . . ? N6B C9B N7B 125.2(5) . . ? N6B C9B C1B 117.5(5) . . ? N7B C9B C1B 117.2(5) . . ? N7B C10B C11B 120.4(5) . . ? N7B C10B C14B 118.1(6) . . ? C11B C10B C14B 121.3(6) . . ? N5B C11B C10B 120.3(5) . . ? N5B C11B C15B 116.7(5) . . ? C10B C11B C15B 123.0(5) . . ? C2 C1 N1 122.9(10) . . ? C1 C2 C3 121.2(10) . . ? C2 C3 C4 119.4(10) . . ? C3 C4 C5 116.2(10) . . ? N1 C5 C4 121.9(9) . . ? N2 C6 C7 127.6(13) . . ? C8 C7 C6 123(2) . . ? C7 C8 C9 120(2) . . ? C8 C9 C10 122.9(14) . . ? C9 C10 N2 115.9(10) . . ? C12 C11 N3 117.3(12) . . ? C13 C12 C11 124.0(12) . . ? C14 C13 C12 116.2(10) . . ? C13 C14 C15 126.1(13) . . ? C14 C15 N3 115.4(13) . . ? N4 C16 C17 123.4(7) . . ? C18 C17 C16 117.9(8) . . ? C17 C18 C17 120.9(11) 2_455 . ? C5 N1 C1 118.4(9) . . ? C6 N2 C10 109.9(10) . . ? C15 N3 C11 120.7(11) . . ? C16 N4 C16 116.3(9) . 2_455 ? C23A N5 C19A 120.0 . . ? C20A C19A N5 120.0 . . ? C19A C20A C21A 120.0 . . ? C22A C21A C20A 120.0 . . ? C23A C22A C21A 120.0 . . ? C22A C23A N5 120.0 . . ? C19B N6 C23B 120.0 . . ? C20B C19B N6 120.0 . . ? C19B C20B C21B 120.0 . . ? C22B C21B C20B 120.0 . . ? C21B C22B C23B 120.0 . . ? C22B C23B N6 120.0 . . ? #===END data_Ce(PrBTP)3I3.3C5H5N _database_code_CSD 161598 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H108 Ce I3 N24' _chemical_formula_weight 1974.76 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' 'I' 'I' -0.4742 1.8119 '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 Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 13.5760(15) _cell_length_b 19.695(2) _cell_length_c 16.6430(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.095(4) _cell_angle_gamma 90.00 _cell_volume 4432.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 19511 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method ? _exptl_crystal_F_000 1994 _exptl_absorpt_coefficient_mu 1.615 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.824 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details ; \f scans with 2\% steps, crystal-to-detector distance 28 mm ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 19511 _diffrn_reflns_av_R_equivalents 0.1171 _diffrn_reflns_av_sigmaI/netI 0.1290 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.68 _reflns_number_total 12500 _reflns_number_gt 4669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and expanded by subsequent Fourier-difference synthesis. The pyridine solvent molecules, in which the nitrogen atoms have not been located, have been refined as idealized hexagons with restrained displacement parameters. All non-hydrogen atoms have been refined anisotropically. Hydrogen atoms were introduced (except in the pyridine molecules) at calculated positions as riding atoms, with a displacement parameter equal to 1.2 (CH, CH2) or 1.5 (CH3) times that of the parent atom. The structure has been refined as corresponding to a racemic twin. Refinement in the centrosymmetric space group P2/c failed since the pseudo-binary axis parallel to the b axis does not hold for the propyl groups and pyridine solvent molecules. 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^)+(0.0468P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.25(4) _refine_ls_number_reflns 12500 _refine_ls_number_parameters 974 _refine_ls_number_restraints 110 _refine_ls_R_factor_all 0.2421 _refine_ls_R_factor_gt 0.0927 _refine_ls_wR_factor_ref 0.2196 _refine_ls_wR_factor_gt 0.1576 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.659 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.110 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 0.52371(12) 0.76634(7) 0.70033(11) 0.0526(4) Uani 1 1 d . . . I1 I 0.01365(19) 0.76428(9) 0.68789(16) 0.0816(6) Uani 1 1 d . . . I2 I 0.51653(19) 0.96554(8) 1.19545(16) 0.0697(5) Uani 1 1 d . . . I3 I 0.44885(14) 0.60344(11) 0.44774(12) 0.0813(6) Uani 1 1 d . . . N1A N 0.4926(17) 0.8239(12) 0.5575(14) 0.059(6) Uani 1 1 d . . . N2A N 0.3168(16) 0.6807(11) 0.6360(14) 0.070(7) Uani 1 1 d . . . N3A N 0.3749(17) 0.7291(12) 0.6041(14) 0.064(7) Uani 1 1 d . . . N4A N 0.2671(14) 0.7433(10) 0.4865(12) 0.052(5) Uani 1 1 d . . . N5A N 0.7206(14) 0.8779(10) 0.7237(11) 0.046(5) Uani 1 1 d . . . N6A N 0.6518(15) 0.8615(11) 0.6685(15) 0.058(6) Uani 1 1 d . . . N7A N 0.7058(16) 0.9397(12) 0.5744(13) 0.057(6) Uani 1 1 d . . . C1A C 0.547(2) 0.8737(16) 0.5332(19) 0.074(9) Uani 1 1 d . . . C2A C 0.550(2) 0.9048(15) 0.4617(18) 0.079(9) Uani 1 1 d . . . H2A H 0.5988 0.9342 0.4476 0.094 Uiso 1 1 calc R . . C3A C 0.4660(16) 0.8859(12) 0.4119(14) 0.044(6) Uani 1 1 d . . . H3A H 0.4550 0.9043 0.3604 0.053 Uiso 1 1 calc R . . C4A C 0.4015(17) 0.8414(13) 0.4380(16) 0.051(7) Uani 1 1 d . . . H4A H 0.3429 0.8329 0.4063 0.061 Uiso 1 1 calc R . . C5A C 0.4180(18) 0.8101(14) 0.5053(17) 0.056(7) Uani 1 1 d . . . C6A C 0.3521(19) 0.7600(13) 0.5332(16) 0.047(7) Uani 1 1 d . . . C7A C 0.210(2) 0.6905(15) 0.5133(18) 0.066(8) Uani 1 1 d . . . C8A C 0.2353(18) 0.6645(13) 0.5877(16) 0.053(7) Uani 1 1 d . . . C9A C 0.6397(18) 0.8926(14) 0.5991(16) 0.046(7) Uani 1 1 d . . . C10A C 0.783(2) 0.9514(14) 0.6223(18) 0.064(8) Uani 1 1 d . . . C11A C 0.789(2) 0.9215(15) 0.7060(19) 0.065(9) Uani 1 1 d . . . C12A C 0.1174(17) 0.6770(13) 0.4570(15) 0.057(7) Uani 1 1 d . . . H12A H 0.1092 0.6281 0.4536 0.069 Uiso 1 1 calc R . . H12B H 0.0616 0.6945 0.4832 0.069 Uiso 1 1 calc R . . C13A C 0.109(2) 0.7026(18) 0.376(2) 0.098(11) Uani 1 1 d . . . H13A H 0.1671 0.6884 0.3509 0.118 Uiso 1 1 calc R . . H13B H 0.1107 0.7518 0.3792 0.118 Uiso 1 1 calc R . . C14A C 0.021(2) 0.6839(16) 0.320(2) 0.114(12) Uani 1 1 d . . . H14A H 0.0206 0.6358 0.3108 0.171 Uiso 1 1 calc R . . H14B H 0.0239 0.7072 0.2695 0.171 Uiso 1 1 calc R . . H14C H -0.0385 0.6968 0.3434 0.171 Uiso 1 1 calc R . . C15A C 0.1624(17) 0.6148(12) 0.6211(15) 0.056(7) Uani 1 1 d . . . H15A H 0.0957 0.6260 0.5991 0.067 Uiso 1 1 calc R . . H15B H 0.1653 0.6196 0.6792 0.067 Uiso 1 1 calc R . . C16A C 0.186(2) 0.5410(14) 0.5998(18) 0.086(9) Uani 1 1 d . . . H16A H 0.1375 0.5111 0.6213 0.104 Uiso 1 1 calc R . . H16B H 0.1800 0.5358 0.5416 0.104 Uiso 1 1 calc R . . C17A C 0.288(2) 0.5209(15) 0.6337(19) 0.103(10) Uani 1 1 d . . . H17A H 0.3340 0.5566 0.6239 0.154 Uiso 1 1 calc R . . H17B H 0.3077 0.4800 0.6079 0.154 Uiso 1 1 calc R . . H17C H 0.2887 0.5134 0.6907 0.154 Uiso 1 1 calc R . . C18A C 0.859(2) 1.0005(15) 0.6040(19) 0.079(9) Uani 1 1 d . . . H18A H 0.8628 1.0013 0.5461 0.095 Uiso 1 1 calc R . . H18B H 0.9222 0.9855 0.6290 0.095 Uiso 1 1 calc R . . C19A C 0.838(2) 1.0742(14) 0.6334(18) 0.070(9) Uani 1 1 d . . . H19A H 0.7692 1.0852 0.6197 0.084 Uiso 1 1 calc R . . H19B H 0.8508 1.0760 0.6916 0.084 Uiso 1 1 calc R . . C20A C 0.903(2) 1.1277(15) 0.5954(17) 0.080(9) Uani 1 1 d . . . H20A H 0.9712 1.1135 0.6017 0.120 Uiso 1 1 calc R . . H20B H 0.8968 1.1706 0.6219 0.120 Uiso 1 1 calc R . . H20C H 0.8823 1.1324 0.5390 0.120 Uiso 1 1 calc R . . C21A C 0.8695(19) 0.9351(15) 0.7687(16) 0.060(8) Uani 1 1 d . . . H21A H 0.9000 0.9780 0.7571 0.072 Uiso 1 1 calc R . . H21B H 0.9193 0.8999 0.7666 0.072 Uiso 1 1 calc R . . C22A C 0.8362(19) 0.9378(14) 0.8549(15) 0.066(7) Uani 1 1 d . . . H22A H 0.7991 0.8974 0.8664 0.079 Uiso 1 1 calc R . . H22B H 0.8928 0.9416 0.8946 0.079 Uiso 1 1 calc R . . C23A C 0.771(2) 1.0012(14) 0.8557(17) 0.076(8) Uani 1 1 d . . . H23A H 0.7826 1.0297 0.8109 0.114 Uiso 1 1 calc R . . H23B H 0.7863 1.0256 0.9051 0.114 Uiso 1 1 calc R . . H23C H 0.7025 0.9879 0.8518 0.114 Uiso 1 1 calc R . . N1B N 0.5377(13) 0.6321(8) 0.7035(14) 0.050(5) Uani 1 1 d . . . N2B N 0.3498(15) 0.7413(10) 0.8355(13) 0.051(6) Uani 1 1 d . . . N3B N 0.4154(15) 0.7025(12) 0.8028(14) 0.064(7) Uani 1 1 d . . . N4B N 0.3590(15) 0.5990(11) 0.8523(12) 0.062(6) Uani 1 1 d . . . N5B N 0.7051(17) 0.7400(11) 0.5629(14) 0.060(6) Uani 1 1 d . . . N6B N 0.6400(13) 0.7045(11) 0.6070(13) 0.051(6) Uani 1 1 d . . . N7B N 0.7131(14) 0.6014(11) 0.5674(12) 0.056(5) Uani 1 1 d . . . C1B C 0.5909(18) 0.5939(14) 0.6604(15) 0.055(7) Uani 1 1 d . . . C2B C 0.5994(18) 0.5278(14) 0.6693(16) 0.066(8) Uani 1 1 d . . . H2B H 0.6404 0.5037 0.6376 0.080 Uiso 1 1 calc R . . C3B C 0.5467(15) 0.4922(12) 0.7269(12) 0.045(6) Uani 1 1 d . . . H3B H 0.5541 0.4459 0.7365 0.053 Uiso 1 1 calc R . . C4B C 0.4879(19) 0.5297(14) 0.7646(17) 0.071(8) Uani 1 1 d . . . H4B H 0.4450 0.5090 0.7978 0.085 Uiso 1 1 calc R . . C5B C 0.4866(18) 0.5980(15) 0.7573(16) 0.063(7) Uani 1 1 d . . . C6B C 0.4156(18) 0.6382(14) 0.8078(16) 0.053(7) Uani 1 1 d . . . C7B C 0.2870(19) 0.6346(14) 0.8840(16) 0.059(7) Uani 1 1 d . . . C8B C 0.2784(19) 0.7039(15) 0.8708(16) 0.051(7) Uani 1 1 d . . . C9B C 0.6430(18) 0.6387(13) 0.6076(15) 0.047(7) Uani 1 1 d . . . C10B C 0.7760(18) 0.6392(14) 0.5304(17) 0.060(8) Uani 1 1 d . . . C11B C 0.767(2) 0.7141(19) 0.519(2) 0.081(11) Uani 1 1 d . . . C12B C 0.2216(18) 0.5956(15) 0.9346(16) 0.071(8) Uani 1 1 d . . . H12C H 0.2640 0.5675 0.9711 0.085 Uiso 1 1 calc R . . H12D H 0.1898 0.6280 0.9676 0.085 Uiso 1 1 calc R . . C13B C 0.152(3) 0.556(2) 0.900(2) 0.132(14) Uani 1 1 d . . . H13C H 0.1070 0.5850 0.8670 0.158 Uiso 1 1 calc R . . H13D H 0.1145 0.5387 0.9429 0.158 Uiso 1 1 calc R . . C14B C 0.1723(19) 0.4940(14) 0.8468(17) 0.084(9) Uani 1 1 d . . . H14D H 0.2065 0.5087 0.8019 0.126 Uiso 1 1 calc R . . H14E H 0.1109 0.4731 0.8274 0.126 Uiso 1 1 calc R . . H14F H 0.2125 0.4618 0.8782 0.126 Uiso 1 1 calc R . . C15B C 0.199(2) 0.7506(14) 0.9038(17) 0.062(8) Uani 1 1 d . . . H15C H 0.1353 0.7315 0.8858 0.074 Uiso 1 1 calc R . . H15D H 0.2068 0.7464 0.9621 0.074 Uiso 1 1 calc R . . C16B C 0.194(2) 0.8236(15) 0.8855(18) 0.071(8) Uani 1 1 d . . . H16C H 0.1866 0.8306 0.8276 0.085 Uiso 1 1 calc R . . H16D H 0.2547 0.8459 0.9070 0.085 Uiso 1 1 calc R . . C17B C 0.105(2) 0.8539(16) 0.924(2) 0.095(11) Uani 1 1 d . . . H17D H 0.0448 0.8347 0.8991 0.143 Uiso 1 1 calc R . . H17E H 0.1038 0.9023 0.9169 0.143 Uiso 1 1 calc R . . H17F H 0.1102 0.8436 0.9809 0.143 Uiso 1 1 calc R . . C18B C 0.853(2) 0.6000(15) 0.4816(17) 0.077(8) Uani 1 1 d . . . H18C H 0.9181 0.6035 0.5106 0.093 Uiso 1 1 calc R . . H18D H 0.8562 0.6218 0.4296 0.093 Uiso 1 1 calc R . . C19B C 0.8269(19) 0.5216(13) 0.4674(16) 0.067(8) Uani 1 1 d . . . H19C H 0.8862 0.4981 0.4544 0.081 Uiso 1 1 calc R . . H19D H 0.8077 0.5028 0.5176 0.081 Uiso 1 1 calc R . . C20B C 0.747(2) 0.5076(15) 0.4026(18) 0.092(10) Uani 1 1 d . . . H20D H 0.6837 0.5127 0.4238 0.138 Uiso 1 1 calc R . . H20E H 0.7534 0.4621 0.3832 0.138 Uiso 1 1 calc R . . H20F H 0.7517 0.5391 0.3591 0.138 Uiso 1 1 calc R . . C21B C 0.842(2) 0.7490(14) 0.4791(17) 0.062(8) Uani 1 1 d . . . H21C H 0.8327 0.7390 0.4219 0.074 Uiso 1 1 calc R . . H21D H 0.9060 0.7308 0.4993 0.074 Uiso 1 1 calc R . . C22B C 0.845(2) 0.8245(14) 0.4895(17) 0.068(8) Uani 1 1 d . . . H22D H 0.7826 0.8433 0.4666 0.081 Uiso 1 1 calc R . . H22E H 0.8512 0.8349 0.5467 0.081 Uiso 1 1 calc R . . C23B C 0.9245(19) 0.8569(14) 0.4523(19) 0.070(9) Uani 1 1 d . . . H23D H 0.9861 0.8360 0.4713 0.105 Uiso 1 1 calc R . . H23E H 0.9264 0.9042 0.4659 0.105 Uiso 1 1 calc R . . H23F H 0.9141 0.8519 0.3947 0.105 Uiso 1 1 calc R . . N1C N 0.5410(12) 0.8386(9) 0.8352(11) 0.039(5) Uani 1 1 d . . . N2C N 0.3170(16) 0.8681(11) 0.6586(14) 0.062(6) Uani 1 1 d . . . N3C N 0.3972(18) 0.8594(12) 0.7165(16) 0.076(8) Uani 1 1 d . . . N4C N 0.3258(16) 0.9426(12) 0.8050(14) 0.061(6) Uani 1 1 d . . . N5C N 0.7375(13) 0.6877(9) 0.7881(12) 0.046(5) Uani 1 1 d . . . N6C N 0.6693(14) 0.7380(11) 0.8058(13) 0.051(6) Uani 1 1 d . . . N7C N 0.7774(14) 0.7719(10) 0.9236(12) 0.057(6) Uani 1 1 d . . . C1C C 0.619(2) 0.8308(15) 0.8852(19) 0.071(9) Uani 1 1 d . . . C2C C 0.630(2) 0.8587(15) 0.962(2) 0.076(10) Uani 1 1 d . . . H2C H 0.6822 0.8467 0.9990 0.091 Uiso 1 1 calc R . . C3C C 0.5544(18) 0.9081(13) 0.9816(16) 0.064(7) Uani 1 1 d . . . H3C H 0.5587 0.9281 1.0324 0.077 Uiso 1 1 calc R . . C4C C 0.4800(19) 0.9245(14) 0.9276(17) 0.068(8) Uani 1 1 d . . . H4C H 0.4341 0.9577 0.9384 0.081 Uiso 1 1 calc R . . C5C C 0.4731(17) 0.8872(13) 0.8483(15) 0.049(6) Uani 1 1 d . . . C6C C 0.392(2) 0.8989(16) 0.7887(18) 0.060(8) Uani 1 1 d . . . C7C C 0.2502(17) 0.9543(13) 0.7460(15) 0.050(7) Uani 1 1 d . . . C8C C 0.249(2) 0.9142(14) 0.6763(18) 0.062(9) Uani 1 1 d . . . C9C C 0.697(2) 0.7759(14) 0.8715(17) 0.062(8) Uani 1 1 d . . . C10C C 0.8364(15) 0.7226(10) 0.9020(13) 0.035(5) Uani 1 1 d . . . C11C C 0.820(2) 0.6817(15) 0.835(2) 0.072(8) Uani 1 1 d . . . C12C C 0.172(2) 1.0070(16) 0.775(2) 0.090(11) Uani 1 1 d . . . H12E H 0.1076 0.9977 0.7475 0.108 Uiso 1 1 calc R . . H12F H 0.1680 1.0022 0.8324 0.108 Uiso 1 1 calc R . . C13C C 0.201(3) 1.074(2) 0.757(2) 0.109(13) Uani 1 1 d . . . H13E H 0.2092 1.0780 0.7001 0.130 Uiso 1 1 calc R . . H13F H 0.2647 1.0839 0.7867 0.130 Uiso 1 1 calc R . . C14C C 0.124(3) 1.1266(19) 0.781(2) 0.122(14) Uani 1 1 d . . . H14G H 0.0679 1.1260 0.7413 0.183 Uiso 1 1 calc R . . H14H H 0.1530 1.1711 0.7829 0.183 Uiso 1 1 calc R . . H14I H 0.1030 1.1152 0.8327 0.183 Uiso 1 1 calc R . . C15C C 0.167(2) 0.9224(16) 0.6102(19) 0.077(10) Uani 1 1 d . . . H15E H 0.1509 0.8774 0.5895 0.093 Uiso 1 1 calc R . . H15F H 0.1099 0.9390 0.6349 0.093 Uiso 1 1 calc R . . C16C C 0.180(3) 0.963(2) 0.545(3) 0.149(17) Uani 1 1 d . . . H16E H 0.1440 1.0046 0.5554 0.179 Uiso 1 1 calc R . . H16F H 0.1416 0.9413 0.5002 0.179 Uiso 1 1 calc R . . C17C C 0.2709(17) 0.9863(13) 0.5119(16) 0.063(7) Uani 1 1 d . . . H17G H 0.2730 1.0350 0.5118 0.095 Uiso 1 1 calc R . . H17H H 0.2721 0.9699 0.4576 0.095 Uiso 1 1 calc R . . H17I H 0.3273 0.9690 0.5445 0.095 Uiso 1 1 calc R . . C18C C 0.9277(18) 0.7105(13) 0.9638(16) 0.066(7) Uani 1 1 d . . . H18E H 0.9802 0.6893 0.9368 0.079 Uiso 1 1 calc R . . H18F H 0.9518 0.7536 0.9856 0.079 Uiso 1 1 calc R . . C19C C 0.899(2) 0.6634(15) 1.0341(18) 0.092(9) Uani 1 1 d . . . H19E H 0.8485 0.6856 1.0628 0.111 Uiso 1 1 calc R . . H19F H 0.8714 0.6212 1.0120 0.111 Uiso 1 1 calc R . . C20C C 0.989(2) 0.6483(15) 1.0925(18) 0.092(10) Uani 1 1 d . . . H20G H 1.0388 0.6268 1.0640 0.137 Uiso 1 1 calc R . . H20H H 0.9703 0.6187 1.1344 0.137 Uiso 1 1 calc R . . H20I H 1.0145 0.6900 1.1159 0.137 Uiso 1 1 calc R . . C21C C 0.8880(18) 0.6219(12) 0.8143(15) 0.057(7) Uani 1 1 d . . . H21E H 0.9555 0.6384 0.8155 0.068 Uiso 1 1 calc R . . H21F H 0.8863 0.5872 0.8555 0.068 Uiso 1 1 calc R . . C22C C 0.8589(18) 0.5896(13) 0.7314(16) 0.070(8) Uani 1 1 d . . . H22G H 0.7920 0.5720 0.7298 0.084 Uiso 1 1 calc R . . H22H H 0.8606 0.6238 0.6895 0.084 Uiso 1 1 calc R . . C23C C 0.930(2) 0.5323(13) 0.7160(17) 0.084(9) Uani 1 1 d . . . H23G H 0.9930 0.5511 0.7052 0.127 Uiso 1 1 calc R . . H23H H 0.9039 0.5061 0.6704 0.127 Uiso 1 1 calc R . . H23I H 0.9387 0.5036 0.7627 0.127 Uiso 1 1 calc R . . C1 C 0.7244(7) 0.2122(8) 0.7356(9) 0.18(2) Uani 1 1 d GU . . C4 C 0.7609(6) 0.2769(8) 0.7230(8) 0.171(18) Uani 1 1 d GU . . C3 C 0.7305(7) 0.3314(8) 0.7677(7) 0.105(11) Uani 1 1 d GU . . C2 C 0.6636(8) 0.3212(9) 0.8251(6) 0.108(11) Uani 1 1 d GU . . C6 C 0.6271(8) 0.2565(8) 0.8378(6) 0.106(11) Uani 1 1 d GU . . C5 C 0.6575(8) 0.2020(8) 0.7930(8) 0.122(12) Uani 1 1 d GU . . C11 C 0.6295(8) 0.3515(8) 0.4902(6) 0.067(7) Uani 1 1 d GU . . C10 C 0.5626(9) 0.4049(8) 0.4809(7) 0.130(14) Uani 1 1 d GU . . C9 C 0.4832(8) 0.4079(6) 0.5280(7) 0.097(9) Uani 1 1 d GU . . C8 C 0.4707(6) 0.3574(5) 0.5845(5) 0.152(16) Uani 1 1 d GU . . C7 C 0.5375(6) 0.3039(5) 0.5939(5) 0.153(16) Uani 1 1 d GU . . C12 C 0.6169(7) 0.3010(7) 0.5467(6) 0.131(13) Uani 1 1 d GU . . C15 C 0.2340(6) 0.3280(7) 0.6776(8) 0.090(9) Uani 1 1 d GU . . C18 C 0.2337(6) 0.2729(7) 0.6253(8) 0.065(7) Uani 1 1 d GU . . C16 C 0.3004(7) 0.2201(6) 0.6411(8) 0.099(11) Uani 1 1 d GU . . C17 C 0.3675(7) 0.2223(5) 0.7092(7) 0.084(9) Uani 1 1 d GU . . C13 C 0.3678(7) 0.2773(6) 0.7615(6) 0.088(9) Uani 1 1 d GU . . C14 C 0.3010(7) 0.3302(7) 0.7457(7) 0.104(10) Uani 1 1 d GU . . 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 0.0539(8) 0.0587(9) 0.0448(9) 0.0008(11) 0.0020(6) -0.0014(12) I1 0.0889(13) 0.0711(12) 0.0858(17) 0.0034(15) 0.0135(12) -0.0038(16) I2 0.0750(10) 0.0790(12) 0.0559(11) -0.0016(13) 0.0106(9) -0.0031(14) I3 0.0785(13) 0.0836(15) 0.0811(15) -0.0164(13) 0.0037(11) 0.0066(12) N1A 0.059(9) 0.053(9) 0.065(10) -0.011(8) 0.005(8) -0.014(7) N2A 0.072(10) 0.066(10) 0.072(10) -0.003(8) 0.004(8) -0.006(8) N3A 0.065(9) 0.055(10) 0.070(10) 0.002(8) 0.004(8) 0.007(8) N4A 0.050(8) 0.050(9) 0.055(9) -0.003(7) 0.003(7) -0.004(7) N5A 0.052(8) 0.050(9) 0.036(8) -0.005(7) 0.003(7) 0.004(7) N6A 0.055(9) 0.056(10) 0.061(10) -0.009(8) 0.001(8) -0.002(7) N7A 0.063(9) 0.059(10) 0.050(9) -0.016(7) 0.008(8) 0.000(8) C1A 0.073(11) 0.077(12) 0.072(12) 0.004(9) 0.007(9) 0.005(9) C2A 0.077(10) 0.080(10) 0.080(10) 0.006(7) 0.014(7) -0.014(7) C3A 0.047(8) 0.048(8) 0.037(8) -0.005(6) -0.001(6) -0.007(6) C4A 0.045(8) 0.053(9) 0.053(9) 0.004(6) -0.005(6) 0.000(6) C5A 0.048(9) 0.059(11) 0.060(10) 0.001(8) 0.003(8) -0.004(8) C6A 0.052(10) 0.044(10) 0.046(10) -0.007(8) 0.006(8) 0.017(8) C7A 0.060(10) 0.069(11) 0.068(11) 0.002(9) 0.005(9) 0.008(8) C8A 0.058(10) 0.047(10) 0.055(10) -0.019(8) 0.010(8) 0.014(8) C9A 0.045(9) 0.043(10) 0.051(10) -0.016(8) 0.007(8) -0.005(8) C10A 0.064(11) 0.061(11) 0.066(11) -0.006(8) 0.007(8) 0.006(8) C11A 0.069(11) 0.062(12) 0.065(12) -0.009(8) 0.006(9) -0.003(8) C12A 0.051(9) 0.065(10) 0.056(10) -0.013(8) 0.005(8) -0.010(8) C13A 0.091(13) 0.103(14) 0.100(14) 0.003(9) 0.011(9) -0.006(9) C14A 0.108(14) 0.123(14) 0.111(14) 0.005(9) 0.006(9) -0.011(9) C15A 0.053(9) 0.058(11) 0.057(10) -0.001(8) 0.006(8) -0.009(8) C16A 0.083(11) 0.084(12) 0.091(12) 0.010(9) 0.003(9) -0.004(9) C17A 0.102(13) 0.097(13) 0.107(13) 0.000(9) -0.002(9) -0.005(9) C18A 0.073(12) 0.080(12) 0.084(12) -0.006(9) 0.012(9) -0.005(9) C19A 0.074(11) 0.069(12) 0.067(12) 0.012(8) 0.005(8) -0.009(8) C20A 0.086(12) 0.083(12) 0.069(12) 0.006(8) -0.001(9) -0.009(9) C21A 0.057(9) 0.064(10) 0.061(10) -0.005(6) 0.015(6) 0.005(6) C22A 0.065(10) 0.078(11) 0.057(10) -0.014(8) 0.012(8) 0.014(8) C23A 0.078(11) 0.079(12) 0.071(11) -0.002(9) 0.006(9) -0.004(9) N1B 0.033(8) 0.058(8) 0.060(8) 0.009(8) 0.001(7) -0.004(7) N2B 0.044(8) 0.055(9) 0.055(9) -0.007(7) 0.009(7) -0.006(7) N3B 0.060(9) 0.066(10) 0.065(10) 0.002(8) 0.011(8) 0.007(8) N4B 0.071(9) 0.063(9) 0.053(9) 0.000(8) 0.013(8) -0.003(8) N5B 0.065(9) 0.052(10) 0.065(10) 0.014(8) 0.015(8) -0.001(8) N6B 0.044(8) 0.046(9) 0.065(10) 0.005(7) 0.007(7) -0.005(7) N7B 0.059(8) 0.048(9) 0.060(9) -0.004(8) 0.003(7) -0.008(8) C1B 0.062(10) 0.047(10) 0.053(10) 0.000(8) -0.004(8) 0.000(8) C2B 0.067(9) 0.069(10) 0.063(10) 0.000(6) 0.001(7) 0.001(6) C3B 0.043(9) 0.042(9) 0.048(9) 0.014(7) -0.002(7) -0.008(7) C4B 0.067(11) 0.075(11) 0.070(11) 0.003(9) 0.005(9) -0.001(9) C5B 0.064(10) 0.061(10) 0.065(10) 0.002(8) 0.001(8) -0.004(9) C6B 0.055(10) 0.055(11) 0.047(10) -0.005(8) 0.001(8) -0.002(8) C7B 0.062(10) 0.059(11) 0.057(11) 0.016(8) 0.015(8) -0.006(8) C8B 0.050(10) 0.056(11) 0.048(10) -0.004(8) 0.016(8) -0.004(8) C9B 0.054(10) 0.047(10) 0.040(10) -0.004(8) 0.004(8) 0.005(8) C10B 0.053(10) 0.064(11) 0.063(11) -0.001(8) 0.005(8) -0.001(8) C11B 0.082(13) 0.081(13) 0.082(13) -0.001(9) 0.011(9) -0.003(9) C12B 0.061(10) 0.078(11) 0.075(11) 0.001(9) 0.012(8) -0.009(9) C13B 0.133(16) 0.134(16) 0.129(16) -0.007(10) 0.012(10) 0.006(10) C14B 0.079(11) 0.092(12) 0.084(12) -0.005(9) 0.014(9) -0.003(9) C15B 0.066(11) 0.067(12) 0.055(11) -0.002(8) 0.019(8) 0.007(8) C16B 0.071(11) 0.070(12) 0.073(12) -0.002(8) 0.008(9) 0.010(8) C17B 0.092(13) 0.095(14) 0.097(14) -0.001(9) -0.003(9) 0.007(9) C18B 0.076(11) 0.078(11) 0.081(11) -0.004(9) 0.016(9) 0.001(9) C19B 0.069(10) 0.067(11) 0.067(11) -0.006(8) 0.013(8) 0.003(8) C20B 0.092(12) 0.095(13) 0.092(13) -0.004(9) 0.022(9) 0.004(9) C21B 0.067(11) 0.066(12) 0.058(11) 0.009(8) 0.030(8) -0.006(8) C22B 0.072(11) 0.064(11) 0.068(11) 0.003(8) 0.007(8) -0.010(8) C23B 0.072(12) 0.057(11) 0.080(12) -0.006(9) 0.000(9) -0.009(8) N1C 0.030(7) 0.037(8) 0.049(8) -0.004(7) -0.001(7) 0.004(6) N2C 0.060(9) 0.061(10) 0.065(10) 0.014(8) 0.010(8) -0.005(8) N3C 0.076(10) 0.076(11) 0.073(11) 0.005(8) -0.002(8) 0.003(8) N4C 0.059(9) 0.061(10) 0.060(10) -0.004(8) -0.005(8) 0.005(8) N5C 0.036(7) 0.049(9) 0.052(9) -0.009(7) 0.007(7) -0.001(7) N6C 0.043(8) 0.053(9) 0.058(9) 0.001(7) 0.003(7) 0.010(7) N7C 0.050(8) 0.057(9) 0.062(9) 0.001(8) 0.000(7) 0.003(7) C1C 0.077(11) 0.068(12) 0.069(12) 0.004(9) 0.009(9) 0.001(9) C2C 0.080(12) 0.073(12) 0.073(13) -0.002(9) -0.001(9) 0.004(9) C3C 0.073(10) 0.066(11) 0.055(10) -0.025(8) 0.012(8) 0.003(8) C4C 0.068(11) 0.065(11) 0.071(11) -0.011(8) 0.011(8) 0.025(8) C5C 0.044(9) 0.052(10) 0.053(10) 0.001(8) 0.010(8) 0.004(8) C6C 0.057(10) 0.061(11) 0.061(11) 0.006(8) 0.001(8) 0.006(9) C7C 0.045(9) 0.050(10) 0.056(10) 0.000(8) 0.008(8) 0.007(8) C8C 0.068(11) 0.058(12) 0.060(11) 0.007(8) 0.006(8) -0.010(8) C9C 0.066(10) 0.058(10) 0.061(10) -0.009(6) 0.004(6) 0.002(6) C10C 0.036(7) 0.030(8) 0.039(7) -0.004(6) 0.003(6) -0.014(6) C11C 0.073(11) 0.070(12) 0.074(12) -0.003(9) 0.013(9) 0.007(9) C12C 0.092(13) 0.090(13) 0.088(13) 0.017(9) 0.014(9) 0.001(9) C13C 0.105(15) 0.108(16) 0.113(16) -0.004(9) 0.015(9) 0.002(9) C14C 0.122(16) 0.122(16) 0.123(16) -0.010(9) 0.020(10) 0.010(9) C15C 0.079(12) 0.079(13) 0.074(13) -0.002(9) 0.008(9) 0.001(9) C16C 0.146(18) 0.153(18) 0.148(18) 0.007(7) 0.012(7) -0.006(7) C17C 0.060(9) 0.066(9) 0.065(9) 0.005(6) 0.014(6) -0.001(6) C18C 0.065(10) 0.069(11) 0.062(11) 0.012(8) 0.004(8) -0.005(8) C19C 0.093(12) 0.096(12) 0.089(12) 0.002(9) 0.009(9) 0.006(9) C20C 0.086(12) 0.096(13) 0.092(13) 0.010(9) 0.005(9) 0.000(9) C21C 0.060(10) 0.059(11) 0.053(10) -0.010(8) 0.006(8) 0.005(8) C22C 0.065(10) 0.070(11) 0.076(11) 0.001(8) 0.009(8) 0.012(8) C23C 0.089(12) 0.080(12) 0.083(12) -0.010(9) 0.003(9) 0.004(9) C1 0.19(2) 0.18(2) 0.18(2) -0.006(10) 0.019(10) 0.009(10) C4 0.167(19) 0.18(2) 0.17(2) 0.001(10) 0.022(10) 0.001(10) C3 0.109(13) 0.104(13) 0.102(14) -0.001(9) 0.003(9) -0.017(9) C2 0.108(14) 0.104(14) 0.113(14) -0.005(9) 0.013(9) -0.002(9) C6 0.105(13) 0.105(14) 0.107(14) 0.002(9) -0.002(9) -0.008(9) C5 0.123(14) 0.119(15) 0.122(15) 0.006(9) 0.005(9) -0.002(9) C11 0.074(10) 0.061(11) 0.065(11) 0.009(8) 0.007(8) 0.001(8) C10 0.124(16) 0.135(16) 0.131(16) -0.005(10) 0.012(10) 0.005(10) C9 0.094(12) 0.098(12) 0.097(12) 0.003(9) 0.004(9) -0.004(9) C8 0.152(18) 0.152(18) 0.152(18) 0.008(10) 0.014(10) 0.007(10) C7 0.149(18) 0.151(18) 0.160(18) -0.004(10) 0.013(10) 0.001(10) C12 0.132(15) 0.128(16) 0.134(16) -0.001(9) 0.013(10) -0.002(9) C15 0.089(12) 0.091(12) 0.090(12) 0.017(9) 0.012(9) -0.009(9) C18 0.059(10) 0.066(10) 0.070(10) 0.012(8) 0.011(8) -0.001(8) C16 0.102(13) 0.089(13) 0.105(14) 0.014(9) 0.010(9) -0.009(9) C17 0.088(11) 0.079(12) 0.084(12) 0.004(9) 0.005(9) -0.009(9) C13 0.085(11) 0.086(12) 0.091(12) 0.010(9) 0.004(9) -0.012(9) C14 0.103(13) 0.106(13) 0.104(13) 0.006(9) 0.022(9) -0.009(9) _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 N3C 2.54(2) . ? Ce N3A 2.57(2) . ? Ce N6C 2.59(2) . ? Ce N6B 2.61(2) . ? Ce N1C 2.650(19) . ? Ce N1A 2.63(2) . ? Ce N6A 2.64(2) . ? Ce N1B 2.651(16) . ? Ce N3B 2.66(2) . ? N1A C5A 1.30(3) . ? N1A C1A 1.31(3) . ? N2A C8A 1.35(3) . ? N2A N3A 1.37(3) . ? N3A C6A 1.34(3) . ? N4A C6A 1.37(3) . ? N4A C7A 1.40(3) . ? N5A N6A 1.29(3) . ? N5A C11A 1.32(3) . ? N6A C9A 1.30(3) . ? N7A C10A 1.28(3) . ? N7A C9A 1.38(3) . ? C1A C2A 1.34(4) . ? C1A C9A 1.63(4) . ? C2A C3A 1.39(3) . ? C3A C4A 1.34(3) . ? C4A C5A 1.28(3) . ? C5A C6A 1.44(3) . ? C7A C8A 1.36(3) . ? C7A C12A 1.52(3) . ? C8A C15A 1.53(3) . ? C10A C18A 1.46(4) . ? C10A C11A 1.51(4) . ? C11A C21A 1.47(4) . ? C12A C13A 1.44(4) . ? C13A C14A 1.49(4) . ? C15A C16A 1.54(3) . ? C16A C17A 1.51(4) . ? C18A C19A 1.56(4) . ? C19A C20A 1.55(4) . ? C21A C22A 1.54(3) . ? C22A C23A 1.53(3) . ? N1B C1B 1.30(3) . ? N1B C5B 1.36(3) . ? N2B N3B 1.33(3) . ? N2B C8B 1.39(3) . ? N3B C6B 1.27(3) . ? N4B C6B 1.36(3) . ? N4B C7B 1.35(3) . ? N5B C11B 1.27(4) . ? N5B N6B 1.39(3) . ? N6B C9B 1.30(3) . ? N7B C10B 1.33(3) . ? N7B C9B 1.42(3) . ? C1B C2B 1.32(3) . ? C1B C9B 1.47(3) . ? C2B C3B 1.43(3) . ? C3B C4B 1.29(3) . ? C4B C5B 1.35(3) . ? C5B C6B 1.55(3) . ? C7B C8B 1.39(3) . ? C7B C12B 1.49(3) . ? C8B C15B 1.55(4) . ? C10B C11B 1.49(4) . ? C10B C18B 1.58(3) . ? C11B C21B 1.44(4) . ? C12B C13B 1.33(4) . ? C13B C14B 1.54(4) . ? C15B C16B 1.47(3) . ? C16B C17B 1.54(4) . ? C18B C19B 1.60(3) . ? C19B C20B 1.49(3) . ? C21B C22B 1.50(3) . ? C22B C23B 1.44(3) . ? N1C C1C 1.30(3) . ? N1C C5C 1.36(3) . ? N2C C8C 1.35(3) . ? N2C N3C 1.40(3) . ? N3C C6C 1.44(4) . ? N4C C6C 1.29(3) . ? N4C C7C 1.38(3) . ? N5C C11C 1.31(3) . ? N5C N6C 1.40(2) . ? N6C C9C 1.35(3) . ? N7C C10C 1.33(3) . ? N7C C9C 1.33(3) . ? C1C C2C 1.39(4) . ? C1C C9C 1.54(4) . ? C2C C3C 1.47(3) . ? C3C C4C 1.33(3) . ? C4C C5C 1.51(3) . ? C5C C6C 1.44(3) . ? C7C C8C 1.40(4) . ? C7C C12C 1.59(4) . ? C8C C15C 1.50(4) . ? C10C C11C 1.38(3) . ? C10C C18C 1.56(3) . ? C11C C21C 1.56(3) . ? C12C C13C 1.42(4) . ? C13C C14C 1.55(4) . ? C15C C16C 1.37(4) . ? C16C C17C 1.47(4) . ? C18C C19C 1.57(3) . ? C19C C20C 1.52(3) . ? C21C C22C 1.54(3) . ? C22C C23C 1.52(3) . ? C1 C4 1.3900 . ? C1 C5 1.3900 . ? C4 C3 1.3900 . ? C3 C2 1.3900 . ? C2 C6 1.3900 . ? C6 C5 1.3900 . ? C11 C10 1.3894 . ? C11 C12 1.3904 . ? C10 C9 1.3898 . ? C9 C8 1.3898 . ? C8 C7 1.3901 . ? C7 C12 1.3897 . ? C15 C14 1.3900 . ? C15 C18 1.3903 . ? C18 C16 1.3899 . ? C16 C17 1.3901 . ? C17 C13 1.3900 . ? C13 C14 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3C Ce N3A 76.7(8) . . ? N3C Ce N6C 124.5(8) . . ? N3A Ce N6C 150.8(6) . . ? N3C Ce N6B 148.1(8) . . ? N3A Ce N6B 88.9(7) . . ? N6C Ce N6B 80.6(7) . . ? N3C Ce N1C 62.2(7) . . ? N3A Ce N1C 133.3(6) . . ? N6C Ce N1C 62.3(6) . . ? N6B Ce N1C 137.8(6) . . ? N3C Ce N1A 74.3(8) . . ? N3A Ce N1A 60.4(7) . . ? N6C Ce N1A 139.2(7) . . ? N6B Ce N1A 73.8(7) . . ? N1C Ce N1A 121.9(5) . . ? N3C Ce N6A 88.4(5) . . ? N3A Ce N6A 124.9(7) . . ? N6C Ce N6A 79.2(7) . . ? N6B Ce N6A 76.6(6) . . ? N1C Ce N6A 77.2(6) . . ? N1A Ce N6A 64.5(7) . . ? N3C Ce N1B 139.9(7) . . ? N3A Ce N1B 77.2(6) . . ? N6C Ce N1B 73.9(6) . . ? N6B Ce N1B 60.1(7) . . ? N1C Ce N1B 121.2(6) . . ? N1A Ce N1B 116.9(7) . . ? N6A Ce N1B 131.6(6) . . ? N3C Ce N3B 81.7(8) . . ? N3A Ce N3B 79.4(7) . . ? N6C Ce N3B 84.0(6) . . ? N6B Ce N3B 123.9(5) . . ? N1C Ce N3B 74.0(6) . . ? N1A Ce N3B 136.7(7) . . ? N6A Ce N3B 150.9(7) . . ? N1B Ce N3B 63.8(7) . . ? C5A N1A C1A 112(3) . . ? C5A N1A Ce 124.3(19) . . ? C1A N1A Ce 123.2(19) . . ? C8A N2A N3A 114(2) . . ? C6A N3A N2A 124(2) . . ? C6A N3A Ce 121.8(19) . . ? N2A N3A Ce 113.8(16) . . ? C6A N4A C7A 118(2) . . ? N6A N5A C11A 119(2) . . ? N5A N6A C9A 123(2) . . ? N5A N6A Ce 118.8(18) . . ? C9A N6A Ce 118.4(18) . . ? C10A N7A C9A 117(3) . . ? N1A C1A C2A 132(3) . . ? N1A C1A C9A 113(3) . . ? C2A C1A C9A 115(3) . . ? C1A C2A C3A 109(3) . . ? C4A C3A C2A 120(3) . . ? C3A C4A C5A 122(3) . . ? N1A C5A C4A 123(3) . . ? N1A C5A C6A 113(3) . . ? C4A C5A C6A 123(3) . . ? N3A C6A N4A 120(3) . . ? N3A C6A C5A 120(3) . . ? N4A C6A C5A 120(2) . . ? C8A C7A N4A 118(3) . . ? C8A C7A C12A 129(3) . . ? N4A C7A C12A 113(2) . . ? N2A C8A C7A 126(3) . . ? N2A C8A C15A 117(2) . . ? C7A C8A C15A 117(2) . . ? N6A C9A N7A 123(2) . . ? N6A C9A C1A 121(2) . . ? N7A C9A C1A 116(2) . . ? N7A C10A C18A 123(3) . . ? N7A C10A C11A 119(3) . . ? C18A C10A C11A 118(3) . . ? N5A C11A C21A 117(3) . . ? N5A C11A C10A 119(3) . . ? C21A C11A C10A 124(3) . . ? C13A C12A C7A 121(2) . . ? C12A C13A C14A 120(3) . . ? C8A C15A C16A 112(2) . . ? C17A C16A C15A 111(2) . . ? C10A C18A C19A 114(2) . . ? C20A C19A C18A 112(2) . . ? C11A C21A C22A 114(2) . . ? C23A C22A C21A 105(2) . . ? C1B N1B C5B 114.8(19) . . ? C1B N1B Ce 127.4(17) . . ? C5B N1B Ce 117.7(18) . . ? N3B N2B C8B 113(2) . . ? C6B N3B N2B 123(2) . . ? C6B N3B Ce 121.0(17) . . ? N2B N3B Ce 114.8(17) . . ? C6B N4B C7B 113(2) . . ? C11B N5B N6B 126(3) . . ? C9B N6B N5B 119(2) . . ? C9B N6B Ce 118.8(15) . . ? N5B N6B Ce 121.8(16) . . ? C10B N7B C9B 115(2) . . ? N1B C1B C2B 124(2) . . ? N1B C1B C9B 108(2) . . ? C2B C1B C9B 128(2) . . ? C1B C2B C3B 121(2) . . ? C4B C3B C2B 114(2) . . ? C3B C4B C5B 122(3) . . ? C4B C5B N1B 123(2) . . ? C4B C5B C6B 118(2) . . ? N1B C5B C6B 119(2) . . ? N3B C6B N4B 127(2) . . ? N3B C6B C5B 118(2) . . ? N4B C6B C5B 115(2) . . ? N4B C7B C8B 120(2) . . ? N4B C7B C12B 116(2) . . ? C8B C7B C12B 123(2) . . ? N2B C8B C7B 123(2) . . ? N2B C8B C15B 111(2) . . ? C7B C8B C15B 125(2) . . ? N6B C9B N7B 122(2) . . ? N6B C9B C1B 126(2) . . ? N7B C9B C1B 111(2) . . ? N7B C10B C11B 124(2) . . ? N7B C10B C18B 117(2) . . ? C11B C10B C18B 118(2) . . ? N5B C11B C21B 127(3) . . ? N5B C11B C10B 112(3) . . ? C21B C11B C10B 118(3) . . ? C13B C12B C7B 120(3) . . ? C12B C13B C14B 124(3) . . ? C16B C15B C8B 122(2) . . ? C15B C16B C17B 108(2) . . ? C10B C18B C19B 113(2) . . ? C20B C19B C18B 115(2) . . ? C11B C21B C22B 116(3) . . ? C23B C22B C21B 114(2) . . ? C1C N1C C5C 121(2) . . ? C1C N1C Ce 119.0(18) . . ? C5C N1C Ce 120.2(15) . . ? C8C N2C N3C 116(2) . . ? N2C N3C C6C 114(2) . . ? N2C N3C Ce 120.5(19) . . ? C6C N3C Ce 124.3(19) . . ? C6C N4C C7C 117(2) . . ? C11C N5C N6C 119(2) . . ? C9C N6C N5C 115(2) . . ? C9C N6C Ce 125.0(17) . . ? N5C N6C Ce 119.2(15) . . ? C10C N7C C9C 110(2) . . ? N1C C1C C2C 124(3) . . ? N1C C1C C9C 121(3) . . ? C2C C1C C9C 113(3) . . ? C1C C2C C3C 117(3) . . ? C4C C3C C2C 121(3) . . ? C3C C4C C5C 117(2) . . ? N1C C5C C6C 120(2) . . ? N1C C5C C4C 120(2) . . ? C6C C5C C4C 121(2) . . ? N4C C6C C5C 118(3) . . ? N4C C6C N3C 129(3) . . ? C5C C6C N3C 113(3) . . ? N4C C7C C8C 117(2) . . ? N4C C7C C12C 112(2) . . ? C8C C7C C12C 131(3) . . ? N2C C8C C7C 127(3) . . ? N2C C8C C15C 113(3) . . ? C7C C8C C15C 120(3) . . ? N7C C9C N6C 131(3) . . ? N7C C9C C1C 118(2) . . ? N6C C9C C1C 111(2) . . ? N7C C10C C11C 126(2) . . ? N7C C10C C18C 113.5(19) . . ? C11C C10C C18C 121(2) . . ? N5C C11C C10C 120(3) . . ? N5C C11C C21C 115(3) . . ? C10C C11C C21C 124(3) . . ? C13C C12C C7C 110(3) . . ? C12C C13C C14C 111(3) . . ? C16C C15C C8C 121(3) . . ? C15C C16C C17C 130(4) . . ? C19C C18C C10C 110(2) . . ? C20C C19C C18C 111(2) . . ? C22C C21C C11C 114(2) . . ? C23C C22C C21C 110(2) . . ? C4 C1 C5 120.0 . . ? C1 C4 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C3 C2 C6 120.0 . . ? C5 C6 C2 120.0 . . ? C6 C5 C1 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C9 C8 120.0 . . ? C9 C8 C7 120.0 . . ? C12 C7 C8 120.0 . . ? C7 C12 C11 120.0 . . ? C14 C15 C18 120.0 . . ? C16 C18 C15 120.0 . . ? C18 C16 C17 120.0 . . ? C13 C17 C16 120.0 . . ? C17 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? #===END data_U(PrBTP)3I3.4C5H5N _database_code_CSD 161599 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H113 I3 N25 U' _chemical_formula_weight 2151.77 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4305(10) _cell_length_b 16.5088(12) _cell_length_c 21.1404(15) _cell_angle_alpha 80.601(4) _cell_angle_beta 88.755(4) _cell_angle_gamma 83.588(5) _cell_volume 4595.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 28304 _cell_measurement_theta_min 5.10 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method ? _exptl_crystal_F_000 2146 _exptl_absorpt_coefficient_mu 2.832 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.417 _exptl_absorpt_correction_T_max 0.654 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 28304 _diffrn_reflns_av_R_equivalents 0.0928 _diffrn_reflns_av_sigmaI/netI 0.1027 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _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 5.10 _diffrn_reflns_theta_max 25.68 _reflns_number_total 15377 _reflns_number_gt 5985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and expanded by subsequent Fourier-difference synthesis. The pyridine solvent molecules, in which the nitrogen atom has not been located, have been refined as idealized hexagons with restrained displacement parameters. Several n-propyl groups have been found disordered, at least partially, and were refined with two positions with occupations constrained to sum to unity. One of them, being unstable on refinement, has been fixed. Two iodine atoms were also found disordered over two positions. Some restraints on bond lenghts and displacement parameters have been applied in the disordered parts. All non-hydrogen atoms have been refined anisotropically, unless the disordered ones. Hydrogen atoms were introduced (except in the pyridine molecules and the disordered parts) at calculated positions as riding atoms, with a displacement parameter equal to 1.2 (CH, CH2) or 1.5 (CH3) times that of the parent atom. 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^)+(0.0857P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0053(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 15377 _refine_ls_number_parameters 1011 _refine_ls_number_restraints 346 _refine_ls_R_factor_all 0.2153 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2315 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.629 _refine_diff_density_min -1.354 _refine_diff_density_rms 0.105 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 U U 0.51643(10) 0.70021(8) 0.72291(6) 0.0738(6) Uani 1 1 d . . . I1A I 0.5641(5) 0.3974(2) 0.8399(2) 0.1071(18) Uani 0.911(15) 1 d PU . . I1B I 0.618(5) 0.401(3) 0.865(3) 0.131(10) Uani 0.089(15) 1 d PU . . I2A I 0.5173(3) 0.74988(16) 0.47517(16) 0.0916(12) Uani 0.934(8) 1 d PU . . I2B I 0.571(4) 0.737(2) 0.440(2) 0.098(10) Uani 0.066(8) 1 d PU . . I3 I 0.0213(3) 0.6807(2) 0.71525(15) 0.1330(12) Uani 1 1 d . . . N1A N 0.5135(19) 0.6671(16) 0.8454(11) 0.077(7) Uani 1 1 d . . . N2A N 0.703(2) 0.8186(15) 0.7465(12) 0.079(7) Uani 1 1 d . . . N3A N 0.634(2) 0.7759(17) 0.7790(14) 0.084(7) Uani 1 1 d . . . N4A N 0.708(2) 0.7898(19) 0.8786(13) 0.101(9) Uani 1 1 d . . . N5A N 0.345(2) 0.5583(17) 0.7378(13) 0.090(8) Uani 1 1 d . . . N6A N 0.402(2) 0.5934(17) 0.7754(13) 0.083(7) Uani 1 1 d . . . N7A N 0.326(3) 0.525(2) 0.8670(16) 0.114(11) Uani 1 1 d . . . C1A C 0.459(3) 0.615(2) 0.8774(18) 0.089(10) Uani 1 1 d . . . C2A C 0.454(3) 0.597(2) 0.9446(16) 0.091(10) Uani 1 1 d . . . H2A H 0.4128 0.5587 0.9649 0.109 Uiso 1 1 calc R . . C3A C 0.510(3) 0.636(3) 0.9782(18) 0.106(12) Uani 1 1 d . . . H3A H 0.5058 0.6276 1.0227 0.127 Uiso 1 1 calc R . . C4A C 0.573(3) 0.689(2) 0.9479(17) 0.097(11) Uani 1 1 d . . . H4A H 0.6140 0.7146 0.9712 0.116 Uiso 1 1 calc R . . C5A C 0.575(3) 0.703(2) 0.8826(17) 0.085(9) Uani 1 1 d . . . C6A C 0.639(3) 0.758(2) 0.8442(16) 0.085(9) Uani 1 1 d . . . C7A C 0.772(3) 0.833(2) 0.8447(16) 0.094(11) Uani 1 1 d . . . C8A C 0.769(3) 0.848(2) 0.7759(18) 0.088(10) Uani 1 1 d . . . C9A C 0.393(3) 0.576(2) 0.8362(17) 0.085(10) Uani 1 1 d . . . C10A C 0.276(3) 0.489(3) 0.830(3) 0.118(14) Uani 1 1 d . . . C11A C 0.283(3) 0.507(2) 0.764(2) 0.122(15) Uani 1 1 d . . . C12A C 0.852(3) 0.870(3) 0.879(2) 0.126(15) Uani 1 1 d D . . C13A C 0.837(6) 0.876(9) 0.950(3) 0.24(4) Uiso 0.60 1 d PDU . . C13D C 0.874(10) 0.835(7) 0.949(3) 0.23(4) Uiso 0.40 1 d PDU . . C14A C 0.934(7) 0.892(7) 0.980(6) 0.34(6) Uani 1 1 d D . . C15A C 0.847(2) 0.893(2) 0.7372(17) 0.095(11) Uani 1 1 d . . . H15A H 0.8428 0.9484 0.7473 0.114 Uiso 1 1 calc R . . H15B H 0.9126 0.8654 0.7504 0.114 Uiso 1 1 calc R . . C16A C 0.839(3) 0.899(2) 0.6668(19) 0.105(12) Uani 1 1 d . . . H16A H 0.7742 0.9270 0.6521 0.126 Uiso 1 1 calc R . . H16B H 0.8453 0.8439 0.6551 0.126 Uiso 1 1 calc R . . C17A C 0.924(4) 0.948(3) 0.636(2) 0.139(16) Uani 1 1 d . . . H17A H 0.9270 0.9954 0.6565 0.208 Uiso 1 1 calc R . . H17B H 0.9121 0.9646 0.5914 0.208 Uiso 1 1 calc R . . H17C H 0.9869 0.9131 0.6425 0.208 Uiso 1 1 calc R . . C18A C 0.191(4) 0.436(3) 0.864(2) 0.147(18) Uani 1 1 d D . . C19A C 0.211(7) 0.398(7) 0.933(3) 0.09(4) Uiso 0.33(6) 1 d PD . . C19D C 0.244(6) 0.356(4) 0.899(4) 0.18(3) Uiso 0.67(6) 1 d PD . . C20A C 0.118(7) 0.359(7) 0.961(5) 0.09(3) Uiso 0.33(6) 1 d PD . . C20D C 0.155(7) 0.315(6) 0.931(5) 0.18(4) Uiso 0.67(6) 1 d PD . . C21A C 0.228(4) 0.471(3) 0.714(3) 0.19(3) Uani 1 1 d . . . H21A H 0.2189 0.5086 0.6742 0.222 Uiso 1 1 calc R . . H21B H 0.1629 0.4552 0.7300 0.222 Uiso 1 1 calc R . . C22A C 0.3015 0.3941 0.7070 0.150 Uiso 1 1 d . . . H22A H 0.2730 0.3437 0.7248 0.180 Uiso 1 1 d . . . H22B H 0.3162 0.3928 0.6621 0.180 Uiso 1 1 d . . . C23A C 0.3972 0.3998 0.7425 0.150 Uiso 1 1 d . . . H23A H 0.3806 0.4226 0.7809 0.225 Uiso 1 1 d . . . H23B H 0.4388 0.4348 0.7155 0.225 Uiso 1 1 d . . . H23C H 0.4326 0.3457 0.7536 0.225 Uiso 1 1 d . . . N1B N 0.5014(19) 0.8469(15) 0.6637(12) 0.075(7) Uani 1 1 d . . . N2B N 0.718(2) 0.6758(17) 0.6215(12) 0.084(8) Uani 1 1 d . . . N3B N 0.6455(19) 0.7343(17) 0.6343(12) 0.074(7) Uani 1 1 d . . . N4B N 0.716(2) 0.8352(19) 0.5587(13) 0.092(8) Uani 1 1 d . . . N5B N 0.309(2) 0.7651(17) 0.8009(14) 0.086(8) Uani 1 1 d . . . N6B N 0.375(2) 0.7982(15) 0.7575(12) 0.081(7) Uani 1 1 d . . . N7B N 0.276(2) 0.9255(17) 0.7354(14) 0.090(8) Uani 1 1 d . . . C1B C 0.428(3) 0.904(2) 0.6776(16) 0.084(9) Uani 1 1 d . . . C2B C 0.418(3) 0.986(2) 0.644(2) 0.105(12) Uani 1 1 d . . . H2B H 0.3682 1.0253 0.6551 0.126 Uiso 1 1 calc R . . C3B C 0.483(3) 1.007(3) 0.5962(18) 0.097(12) Uani 1 1 d . . . H3B H 0.4781 1.0607 0.5732 0.117 Uiso 1 1 calc R . . C4B C 0.559(3) 0.947(3) 0.5818(17) 0.097(11) Uani 1 1 d . . . H4B H 0.6041 0.9596 0.5489 0.117 Uiso 1 1 calc R . . C5B C 0.564(2) 0.873(2) 0.6155(13) 0.076(9) Uani 1 1 d . . . C6B C 0.646(2) 0.809(2) 0.6014(16) 0.080(9) Uani 1 1 d . . . C7B C 0.784(3) 0.777(3) 0.5490(19) 0.107(12) Uani 1 1 d . . . C8B C 0.788(2) 0.693(3) 0.5782(17) 0.090(10) Uani 1 1 d . . . C9B C 0.355(3) 0.8747(19) 0.7263(17) 0.081(9) Uani 1 1 d . . . C10B C 0.205(3) 0.899(3) 0.775(2) 0.111(12) Uani 1 1 d . . . C11B C 0.225(3) 0.810(2) 0.8087(16) 0.087(10) Uani 1 1 d . . . C12B C 0.868(3) 0.805(3) 0.498(2) 0.16(2) Uani 1 1 d D . . C13B C 0.840(6) 0.884(4) 0.452(3) 0.05(3) Uiso 0.45(7) 1 d PD . . C13E C 0.821(5) 0.842(5) 0.432(3) 0.16(3) Uiso 0.55(7) 1 d PD . . C14B C 0.950(7) 0.889(10) 0.435(9) 0.22(7) Uiso 0.45(7) 1 d PD . . C14E C 0.898(8) 0.885(6) 0.389(4) 0.17(4) Uiso 0.55(7) 1 d PD . . C15B C 0.869(3) 0.628(3) 0.5695(18) 0.109(12) Uani 1 1 d D . . C16B C 0.826(15) 0.548(5) 0.563(7) 0.12(9) Uiso 0.17(7) 1 d PD . . C16E C 0.856(4) 0.591(4) 0.509(3) 0.18(3) Uiso 0.83(7) 1 d PD . . C17B C 0.758(4) 0.554(4) 0.506(3) 0.17(2) Uani 1 1 d D . . C18B C 0.118(3) 0.953(3) 0.788(2) 0.129(15) Uani 1 1 d D . . C19B C 0.120(10) 1.013(8) 0.835(7) 0.14(6) Uiso 0.49(3) 1 d PD . . C19E C 0.106(7) 1.036(4) 0.744(4) 0.15(4) Uiso 0.51(6) 1 d PD . . C20B C 0.021(8) 1.070(6) 0.830(5) 0.15(4) Uiso 0.49(6) 1 d PD . . C20E C 0.019(8) 1.094(6) 0.763(6) 0.17(4) Uiso 0.51(6) 1 d PD . . C21B C 0.147(3) 0.774(3) 0.854(2) 0.126(15) Uani 1 1 d . . . H21C H 0.1384 0.8054 0.8884 0.152 Uiso 1 1 calc R . . H21D H 0.0843 0.7813 0.8307 0.152 Uiso 1 1 calc R . . C22B C 0.166(3) 0.689(3) 0.881(2) 0.132(16) Uani 1 1 d . . . H22C H 0.2296 0.6794 0.9031 0.158 Uiso 1 1 calc R . . H22D H 0.1709 0.6555 0.8468 0.158 Uiso 1 1 calc R . . C23B C 0.083(3) 0.660(3) 0.928(2) 0.131(15) Uani 1 1 d . . . H23D H 0.0968 0.6724 0.9698 0.197 Uiso 1 1 calc R . . H23E H 0.0824 0.6011 0.9312 0.197 Uiso 1 1 calc R . . H23F H 0.0195 0.6874 0.9134 0.197 Uiso 1 1 calc R . . N1C N 0.5360(18) 0.5805(15) 0.6592(11) 0.069(6) Uani 1 1 d . . . N2C N 0.726(2) 0.5996(18) 0.7988(12) 0.083(8) Uani 1 1 d . . . N3C N 0.663(2) 0.5927(17) 0.7523(12) 0.079(7) Uani 1 1 d . . . N4C N 0.771(2) 0.4779(16) 0.7240(13) 0.084(8) Uani 1 1 d . . . N5C N 0.312(3) 0.7657(16) 0.6277(14) 0.086(8) Uani 1 1 d . . . N6C N 0.389(2) 0.7035(17) 0.6362(12) 0.075(7) Uani 1 1 d . . . N7C N 0.311(2) 0.6317(19) 0.5652(14) 0.094(8) Uani 1 1 d . . . C1C C 0.471(3) 0.572(2) 0.6149(14) 0.074(8) Uani 1 1 d . . . C2C C 0.474(3) 0.507(2) 0.5836(15) 0.079(9) Uani 1 1 d . . . H2C H 0.4270 0.5044 0.5529 0.095 Uiso 1 1 calc R . . C3C C 0.548(3) 0.447(2) 0.5988(16) 0.082(9) Uani 1 1 d . . . H3C H 0.5521 0.4011 0.5785 0.099 Uiso 1 1 calc R . . C4C C 0.620(3) 0.4508(19) 0.6436(17) 0.081(9) Uani 1 1 d . . . H4C H 0.6720 0.4086 0.6532 0.097 Uiso 1 1 calc R . . C5C C 0.612(2) 0.5167(19) 0.6726(13) 0.066(7) Uani 1 1 d . . . C6C C 0.684(3) 0.530(3) 0.7214(15) 0.085(10) Uani 1 1 d . . . C7C C 0.833(2) 0.490(2) 0.7673(19) 0.091(10) Uani 1 1 d . . . C8C C 0.809(3) 0.549(2) 0.8081(15) 0.084(10) Uani 1 1 d . . . C9C C 0.387(3) 0.641(2) 0.6035(17) 0.085(10) Uani 1 1 d . . . C10C C 0.239(3) 0.695(2) 0.5591(17) 0.090(10) Uani 1 1 d . . . C11C C 0.242(3) 0.760(2) 0.5910(19) 0.087(10) Uani 1 1 d . . . C12C C 0.934(3) 0.432(3) 0.773(2) 0.123(14) Uani 1 1 d D . . C13C C 0.918(8) 0.342(3) 0.792(5) 0.13(4) Uiso 0.48(7) 1 d PD . . C13F C 0.951(9) 0.362(5) 0.735(5) 0.17(5) Uiso 0.52(7) 1 d PD . . C14C C 0.93(2) 0.269(17) 0.844(13) 0.32(12) Uiso 0.48(7) 1 d PD . . C14F C 1.026(7) 0.290(5) 0.781(4) 0.14(3) Uiso 0.52(7) 1 d PD . . C15C C 0.879(3) 0.560(3) 0.8614(16) 0.101(11) Uani 1 1 d . . . H15C H 0.9473 0.5494 0.8470 0.121 Uiso 1 1 calc R . . H15D H 0.8685 0.6171 0.8681 0.121 Uiso 1 1 calc R . . C16C C 0.867(3) 0.507(3) 0.9231(19) 0.132(16) Uani 1 1 d . . . H16C H 0.9006 0.5305 0.9548 0.159 Uiso 1 1 calc R . . H16D H 0.9038 0.4540 0.9202 0.159 Uiso 1 1 calc R . . C17C C 0.766(4) 0.490(3) 0.950(2) 0.142(16) Uani 1 1 d U . . H17D H 0.7277 0.5417 0.9551 0.214 Uiso 1 1 calc R . . H17E H 0.7738 0.4553 0.9909 0.214 Uiso 1 1 calc R . . H17F H 0.7318 0.4637 0.9212 0.214 Uiso 1 1 calc R . . C18C C 0.152(3) 0.685(3) 0.514(2) 0.121(14) Uani 1 1 d . . . H18A H 0.0964 0.7270 0.5169 0.146 Uiso 1 1 calc R . . H18B H 0.1278 0.6312 0.5267 0.146 Uiso 1 1 calc R . . C19C C 0.192(3) 0.693(4) 0.442(2) 0.17(2) Uani 1 1 d D . . C20C C 0.125(10) 0.713(11) 0.383(5) 0.13(3) Uiso 0.32(6) 1 d PDU . . C20F C 0.107(4) 0.669(5) 0.405(3) 0.14(2) Uiso 0.68(6) 1 d PDU . . C21C C 0.163(2) 0.831(2) 0.5821(18) 0.095(11) Uani 1 1 d . . . H21F H 0.0988 0.8082 0.5866 0.115 Uiso 1 1 calc R . . H21G H 0.1679 0.8605 0.6176 0.115 Uiso 1 1 calc R . . C22C C 0.159(3) 0.890(2) 0.525(2) 0.119(14) Uani 1 1 d . . . H22F H 0.1086 0.9352 0.5298 0.143 Uiso 1 1 calc R . . H22G H 0.1371 0.8641 0.4898 0.143 Uiso 1 1 calc R . . C23C C 0.257(3) 0.924(2) 0.5057(18) 0.108(12) Uani 1 1 d . . . H23G H 0.2764 0.9530 0.5383 0.162 Uiso 1 1 calc R . . H23H H 0.2485 0.9611 0.4658 0.162 Uiso 1 1 calc R . . H23I H 0.3072 0.8794 0.5010 0.162 Uiso 1 1 calc R . . C1 C 0.743(3) 0.109(2) 0.6739(17) 0.235(16) Uani 1 1 d GU . . C2 C 0.659(3) 0.167(2) 0.6627(16) 0.229(16) Uani 1 1 d GU . . C3 C 0.639(3) 0.226(2) 0.7028(16) 0.226(16) Uani 1 1 d GU . . C4 C 0.702(2) 0.2262(18) 0.7543(14) 0.226(15) Uani 1 1 d GU . . C5 C 0.785(3) 0.1676(18) 0.7655(16) 0.233(16) Uani 1 1 d GU . . C6 C 0.805(3) 0.1090(19) 0.7253(18) 0.234(16) Uani 1 1 d GU . . C7 C 1.183(3) 0.879(3) 1.035(2) 0.28(2) Uani 1 1 d GU . . C8 C 1.219(3) 0.921(2) 0.979(2) 0.28(2) Uani 1 1 d GU . . C9 C 1.294(2) 0.883(2) 0.9442(18) 0.28(2) Uani 1 1 d GU . . C10 C 1.334(2) 0.802(2) 0.9665(17) 0.28(2) Uani 1 1 d GU . . C11 C 1.298(3) 0.760(2) 1.0231(16) 0.28(2) Uani 1 1 d GU . . C12 C 1.222(3) 0.798(3) 1.0575(17) 0.28(2) Uani 1 1 d GU . . C13 C 0.324(3) 0.181(3) 0.805(3) 0.49(4) Uani 1 1 d GU . . C14 C 0.278(3) 0.120(3) 0.844(3) 0.49(4) Uani 1 1 d GU . . C15 C 0.301(4) 0.101(4) 0.909(3) 0.49(4) Uani 1 1 d GU . . C16 C 0.370(4) 0.144(3) 0.935(3) 0.49(4) Uani 1 1 d GU . . C17 C 0.416(3) 0.205(3) 0.895(2) 0.49(4) Uani 1 1 d GU . . C18 C 0.393(3) 0.223(3) 0.830(3) 0.49(4) Uani 1 1 d GU . . C19 C 1.632(3) 1.028(3) 0.880(2) 0.34(3) Uani 1 1 d GU . . C20 C 1.595(3) 0.978(2) 0.932(2) 0.34(3) Uani 1 1 d GU . . C21 C 1.525(2) 0.924(2) 0.923(2) 0.33(3) Uani 1 1 d GU . . C22 C 1.493(3) 0.922(2) 0.861(2) 0.32(3) Uani 1 1 d GU . . C23 C 1.530(3) 0.972(2) 0.809(2) 0.33(3) Uani 1 1 d GU . . C24 C 1.600(3) 1.025(3) 0.818(2) 0.33(3) Uani 1 1 d GU . . 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 U 0.0683(9) 0.0829(9) 0.0720(9) -0.0161(6) 0.0052(6) -0.0116(6) I1A 0.106(4) 0.123(2) 0.090(3) -0.0167(18) 0.013(2) -0.006(2) I1B 0.122(19) 0.155(17) 0.107(18) 0.004(16) 0.007(16) -0.011(17) I2A 0.095(2) 0.0818(17) 0.099(2) -0.0125(14) -0.0094(18) -0.0162(15) I2B 0.109(18) 0.087(16) 0.097(18) -0.011(15) -0.006(16) -0.010(15) I3 0.129(2) 0.145(3) 0.119(2) 0.0130(18) -0.0131(18) -0.037(2) N1A 0.067(17) 0.082(17) 0.076(17) 0.000(13) 0.019(14) -0.002(14) N2A 0.072(18) 0.081(17) 0.084(18) -0.006(14) 0.001(14) -0.016(15) N3A 0.068(18) 0.101(19) 0.09(2) -0.036(16) -0.008(15) -0.008(15) N4A 0.12(2) 0.12(2) 0.075(18) -0.046(17) 0.001(17) -0.05(2) N5A 0.08(2) 0.088(18) 0.09(2) -0.009(16) 0.006(16) -0.010(16) N6A 0.075(18) 0.11(2) 0.075(18) -0.026(15) 0.004(14) -0.020(15) N7A 0.12(3) 0.12(2) 0.11(2) -0.03(2) 0.04(2) -0.06(2) C1A 0.09(3) 0.09(2) 0.09(3) -0.04(2) 0.00(2) -0.01(2) C2A 0.09(3) 0.12(3) 0.06(2) -0.03(2) 0.009(19) 0.00(2) C3A 0.13(3) 0.13(3) 0.06(2) 0.00(2) 0.01(2) -0.02(3) C4A 0.11(3) 0.12(3) 0.07(2) -0.03(2) 0.01(2) -0.01(2) C5A 0.09(3) 0.08(2) 0.09(3) -0.017(18) -0.01(2) -0.02(2) C6A 0.10(3) 0.09(2) 0.06(2) -0.017(18) -0.006(19) 0.00(2) C7A 0.11(3) 0.12(3) 0.06(2) -0.010(19) -0.016(19) -0.04(2) C8A 0.08(2) 0.08(2) 0.11(3) -0.02(2) 0.00(2) -0.001(19) C9A 0.11(3) 0.08(2) 0.07(2) -0.014(17) 0.02(2) -0.02(2) C10A 0.11(3) 0.10(3) 0.14(4) -0.01(3) 0.02(3) -0.03(3) C11A 0.13(4) 0.09(3) 0.14(4) 0.01(2) 0.01(3) -0.06(3) C12A 0.12(3) 0.17(4) 0.11(3) -0.03(3) 0.00(2) -0.05(3) C14A 0.22(9) 0.42(14) 0.41(13) -0.12(11) -0.15(9) -0.12(9) C15A 0.06(2) 0.12(3) 0.10(3) -0.01(2) -0.008(18) -0.04(2) C16A 0.09(3) 0.10(3) 0.12(3) 0.00(2) 0.00(2) -0.02(2) C17A 0.14(4) 0.15(4) 0.12(3) 0.01(3) 0.02(3) -0.05(3) C18A 0.16(4) 0.15(4) 0.15(4) -0.03(3) 0.00(3) -0.07(4) C21A 0.16(5) 0.10(3) 0.30(7) -0.02(4) -0.05(5) -0.07(4) N1B 0.065(17) 0.072(16) 0.087(18) -0.008(14) -0.002(14) -0.010(14) N2B 0.073(19) 0.10(2) 0.087(18) -0.028(15) 0.012(15) -0.019(17) N3B 0.059(16) 0.082(18) 0.084(17) -0.022(15) 0.014(13) -0.009(14) N4B 0.08(2) 0.10(2) 0.09(2) -0.019(16) 0.023(17) -0.011(18) N5B 0.064(18) 0.085(18) 0.11(2) -0.023(16) 0.002(16) -0.003(16) N6B 0.09(2) 0.064(16) 0.087(18) -0.011(13) 0.005(15) -0.018(15) N7B 0.09(2) 0.074(18) 0.11(2) -0.034(16) 0.009(18) -0.002(17) C1B 0.08(2) 0.09(2) 0.09(2) -0.02(2) -0.002(19) -0.02(2) C2B 0.05(2) 0.09(3) 0.17(4) 0.00(3) -0.01(2) 0.010(19) C3B 0.09(3) 0.11(3) 0.10(3) 0.00(2) -0.02(2) -0.04(3) C4B 0.06(2) 0.13(3) 0.11(3) -0.02(2) 0.04(2) -0.03(2) C5B 0.08(2) 0.08(2) 0.065(18) 0.018(16) 0.001(16) -0.04(2) C6B 0.06(2) 0.09(3) 0.09(2) -0.018(19) 0.015(18) -0.01(2) C7B 0.07(3) 0.14(4) 0.11(3) -0.03(3) 0.01(2) -0.02(3) C8B 0.05(2) 0.12(3) 0.10(2) -0.02(2) -0.002(18) -0.01(2) C9B 0.08(3) 0.054(19) 0.11(3) -0.025(18) -0.01(2) 0.003(19) C10B 0.10(3) 0.13(4) 0.11(3) -0.02(3) 0.01(2) -0.02(3) C11B 0.10(3) 0.08(2) 0.08(2) -0.021(19) -0.01(2) -0.01(2) C12B 0.12(4) 0.22(5) 0.12(3) -0.02(3) 0.07(3) 0.02(4) C15B 0.07(2) 0.17(4) 0.10(3) -0.05(3) 0.01(2) 0.01(2) C17B 0.12(4) 0.24(6) 0.16(4) -0.11(4) 0.00(3) -0.03(4) C18B 0.09(3) 0.13(3) 0.16(4) -0.04(3) 0.03(3) 0.01(3) C21B 0.13(4) 0.13(4) 0.13(3) -0.02(3) 0.04(3) -0.05(3) C22B 0.11(3) 0.14(4) 0.15(4) -0.02(3) 0.05(3) -0.05(3) C23B 0.09(3) 0.18(4) 0.12(3) -0.03(3) 0.01(2) -0.01(3) N1C 0.057(15) 0.081(16) 0.068(15) -0.013(12) -0.005(12) -0.005(14) N2C 0.08(2) 0.11(2) 0.059(16) -0.008(14) -0.007(15) -0.019(18) N3C 0.08(2) 0.092(18) 0.062(16) -0.022(14) 0.007(15) 0.001(15) N4C 0.055(18) 0.095(19) 0.11(2) -0.030(16) -0.008(16) -0.007(15) N5C 0.09(2) 0.075(18) 0.09(2) 0.001(15) 0.011(17) -0.008(18) N6C 0.068(17) 0.074(16) 0.088(18) -0.030(14) -0.008(14) -0.009(15) N7C 0.065(19) 0.11(2) 0.10(2) -0.014(17) -0.024(16) 0.004(18) C1C 0.08(2) 0.08(2) 0.059(18) -0.011(17) 0.004(17) -0.014(19) C2C 0.07(2) 0.09(2) 0.07(2) -0.013(19) -0.011(16) -0.01(2) C3C 0.09(3) 0.07(2) 0.08(2) -0.020(17) 0.00(2) 0.01(2) C4C 0.08(2) 0.061(19) 0.10(2) -0.007(18) -0.01(2) 0.008(16) C5C 0.06(2) 0.066(18) 0.065(18) 0.000(15) 0.007(15) -0.010(16) C6C 0.06(2) 0.13(3) 0.06(2) 0.00(2) 0.000(17) -0.03(2) C7C 0.05(2) 0.11(3) 0.11(3) -0.03(2) -0.018(19) -0.001(19) C8C 0.07(2) 0.11(3) 0.07(2) 0.00(2) -0.021(18) -0.02(2) C9C 0.07(2) 0.10(3) 0.09(2) -0.01(2) 0.007(19) -0.02(2) C10C 0.06(2) 0.10(3) 0.10(3) 0.00(2) -0.035(19) -0.01(2) C11C 0.06(2) 0.09(3) 0.11(3) -0.03(2) 0.01(2) -0.01(2) C12C 0.08(3) 0.13(3) 0.16(4) -0.04(3) -0.04(3) 0.01(2) C15C 0.08(2) 0.15(3) 0.08(2) -0.04(2) -0.034(19) 0.01(2) C16C 0.10(3) 0.21(5) 0.09(3) -0.01(3) 0.01(2) -0.05(3) C17C 0.13(2) 0.16(2) 0.13(2) -0.011(17) -0.010(17) -0.020(17) C18C 0.08(3) 0.12(3) 0.17(4) -0.04(3) -0.04(3) 0.00(2) C19C 0.09(3) 0.33(7) 0.09(3) -0.07(4) -0.04(2) 0.03(4) C21C 0.06(2) 0.09(2) 0.13(3) 0.01(2) 0.00(2) -0.006(19) C22C 0.07(3) 0.10(3) 0.17(4) 0.02(3) 0.02(2) -0.01(2) C23C 0.10(3) 0.09(2) 0.11(3) 0.03(2) 0.00(2) -0.01(2) C1 0.236(19) 0.233(19) 0.234(19) -0.042(13) -0.007(13) -0.016(13) C2 0.230(19) 0.228(19) 0.230(19) -0.037(13) -0.007(13) -0.019(13) C3 0.225(19) 0.226(19) 0.227(19) -0.034(13) -0.003(13) -0.021(13) C4 0.228(19) 0.225(19) 0.226(19) -0.046(13) -0.006(13) -0.018(13) C5 0.237(19) 0.232(19) 0.231(19) -0.049(13) -0.010(13) -0.015(13) C6 0.238(19) 0.232(19) 0.234(19) -0.046(13) -0.009(13) -0.013(13) C7 0.28(2) 0.28(2) 0.28(2) -0.044(14) -0.001(13) -0.027(14) C8 0.28(2) 0.28(2) 0.28(2) -0.044(14) -0.001(13) -0.027(14) C9 0.28(2) 0.28(2) 0.28(2) -0.045(14) -0.004(13) -0.028(14) C10 0.28(2) 0.28(2) 0.28(2) -0.044(14) -0.004(13) -0.030(14) C11 0.28(2) 0.28(2) 0.28(2) -0.043(14) -0.001(13) -0.030(14) C12 0.28(2) 0.27(2) 0.28(2) -0.045(14) -0.002(13) -0.028(14) C13 0.49(4) 0.49(4) 0.49(4) -0.079(12) -0.002(11) -0.055(11) C14 0.49(4) 0.49(4) 0.49(4) -0.079(12) -0.003(11) -0.056(11) C15 0.49(4) 0.49(4) 0.49(4) -0.079(12) -0.003(11) -0.056(11) C16 0.49(4) 0.49(4) 0.49(4) -0.080(12) -0.003(11) -0.055(11) C17 0.49(4) 0.49(4) 0.49(4) -0.080(12) -0.003(11) -0.055(11) C18 0.49(4) 0.49(4) 0.49(4) -0.080(12) -0.003(11) -0.055(11) C19 0.34(3) 0.33(3) 0.34(3) -0.051(14) -0.001(14) -0.037(14) C20 0.33(3) 0.34(3) 0.34(3) -0.052(14) 0.001(14) -0.036(14) C21 0.33(3) 0.33(3) 0.33(3) -0.055(14) 0.000(14) -0.035(14) C22 0.33(3) 0.32(3) 0.32(3) -0.058(14) -0.003(14) -0.033(14) C23 0.33(3) 0.33(3) 0.32(3) -0.056(14) -0.004(14) -0.034(14) C24 0.33(3) 0.33(3) 0.33(3) -0.055(14) -0.004(14) -0.035(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 U N3C 2.52(3) . ? U N6C 2.53(3) . ? U N1B 2.53(2) . ? U N6B 2.53(3) . ? U N3A 2.54(2) . ? U N1C 2.56(2) . ? U N1A 2.56(2) . ? U N3B 2.56(2) . ? U N6A 2.57(3) . ? I1A I1B 0.91(8) . ? I2A I2B 1.06(6) . ? N1A C1A 1.29(4) . ? N1A C5A 1.39(4) . ? N2A C8A 1.28(4) . ? N2A N3A 1.34(3) . ? N3A C6A 1.36(4) . ? N4A C7A 1.31(4) . ? N4A C6A 1.38(4) . ? N5A C11A 1.31(4) . ? N5A N6A 1.35(3) . ? N6A C9A 1.28(4) . ? N7A C10A 1.30(5) . ? N7A C9A 1.38(4) . ? C1A C2A 1.41(4) . ? C1A C9A 1.52(5) . ? C2A C3A 1.33(5) . ? C3A C4A 1.36(5) . ? C4A C5A 1.36(4) . ? C5A C6A 1.47(4) . ? C7A C8A 1.44(4) . ? C7A C12A 1.54(5) . ? C8A C15A 1.50(4) . ? C10A C11A 1.38(5) . ? C10A C18A 1.60(6) . ? C11A C21A 1.54(7) . ? C12A C13D 1.52(2) . ? C12A C13A 1.52(2) . ? C13A C13D 0.8(2) . ? C13A C14A 1.53(2) . ? C13D C14A 1.52(2) . ? C15A C16A 1.48(4) . ? C16A C17A 1.55(5) . ? C18A C19A 1.51(2) . ? C18A C19D 1.52(2) . ? C19A C19D 1.13(11) . ? C19A C20A 1.52(2) . ? C19A C20D 1.64(13) . ? C19D C20D 1.53(2) . ? C20A C20D 1.11(11) . ? C21A C22A 1.54(6) . ? C22A C23A 1.5224 . ? N1B C5B 1.35(3) . ? N1B C1B 1.35(4) . ? N2B C8B 1.32(4) . ? N2B N3B 1.35(3) . ? N3B C6B 1.32(4) . ? N4B C7B 1.30(5) . ? N4B C6B 1.34(4) . ? N5B C11B 1.30(4) . ? N5B N6B 1.35(3) . ? N6B C9B 1.33(4) . ? N7B C9B 1.31(4) . ? N7B C10B 1.33(4) . ? C1B C2B 1.42(5) . ? C1B C9B 1.47(4) . ? C2B C3B 1.35(5) . ? C3B C4B 1.40(5) . ? C4B C5B 1.31(5) . ? C5B C6B 1.50(4) . ? C7B C8B 1.41(5) . ? C7B C12B 1.59(5) . ? C8B C15B 1.47(5) . ? C10B C18B 1.43(6) . ? C10B C11B 1.53(5) . ? C11B C21B 1.50(5) . ? C12B C13B 1.51(2) . ? C12B C13E 1.53(2) . ? C13B C13E 0.92(10) . ? C13B C14E 1.52(2) . ? C13B C14B 1.519(15) . ? C13E C14E 1.52(2) . ? C13E C14B 1.98(11) . ? C14B C14E 1.21(17) . ? C15B C16B 1.52(2) . ? C15B C16E 1.52(2) . ? C16B C16E 1.32(16) . ? C16B C17B 1.52(2) . ? C16E C17B 1.52(2) . ? C18B C19B 1.52(2) . ? C18B C19E 1.52(2) . ? C19B C20B 1.52(2) . ? C19B C19E 1.90(16) . ? C19E C20E 1.52(2) . ? C20B C20E 1.41(13) . ? C21B C22B 1.42(6) . ? C22B C23B 1.54(5) . ? N1C C1C 1.32(4) . ? N1C C5C 1.38(4) . ? N2C C8C 1.30(4) . ? N2C N3C 1.34(3) . ? N3C C6C 1.31(4) . ? N4C C7C 1.31(4) . ? N4C C6C 1.37(4) . ? N5C C11C 1.26(4) . ? N5C N6C 1.36(4) . ? N6C C9C 1.33(4) . ? N7C C10C 1.33(4) . ? N7C C9C 1.35(4) . ? C1C C2C 1.35(4) . ? C1C C9C 1.51(5) . ? C2C C3C 1.33(4) . ? C3C C4C 1.38(4) . ? C4C C5C 1.33(4) . ? C5C C6C 1.49(4) . ? C7C C8C 1.41(5) . ? C7C C12C 1.57(5) . ? C8C C15C 1.53(4) . ? C10C C11C 1.36(5) . ? C10C C18C 1.57(5) . ? C11C C21C 1.48(5) . ? C12C C13F 1.51(2) . ? C12C C13C 1.52(2) . ? C13C C13F 1.28(12) . ? C13C C14F 1.63(13) . ? C13C C14C 1.5(3) . ? C13F C14F 1.66(14) . ? C14C C14F 1.8(3) . ? C15C C16C 1.46(5) . ? C16C C17C 1.49(6) . ? C18C C19C 1.58(6) . ? C19C C20C 1.52(2) . ? C19C C20F 1.53(2) . ? C20C C20F 0.85(15) . ? C21C C22C 1.43(5) . ? C22C C23C 1.51(5) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C12 1.3900 . ? C7 C8 1.3901 . ? C8 C9 1.3900 . ? C9 C10 1.3902 . ? C10 C11 1.3897 . ? C11 C12 1.3900 . ? C13 C18 1.3897 . ? C13 C14 1.3901 . ? C14 C15 1.3901 . ? C15 C16 1.3903 . ? C16 C17 1.3899 . ? C17 C18 1.3903 . ? C19 C20 1.3898 . ? C19 C24 1.3901 . ? C20 C21 1.3901 . ? C21 C22 1.3901 . ? C22 C23 1.3900 . ? C23 C24 1.3901 . ? 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 N3C U N6C 127.0(9) . . ? N3C U N1B 133.1(8) . . ? N6C U N1B 75.2(8) . . ? N3C U N6B 149.3(8) . . ? N6C U N6B 78.6(9) . . ? N1B U N6B 63.7(8) . . ? N3C U N3A 76.9(9) . . ? N6C U N3A 149.1(9) . . ? N1B U N3A 73.8(9) . . ? N6B U N3A 87.0(8) . . ? N3C U N1C 63.8(9) . . ? N6C U N1C 63.2(9) . . ? N1B U N1C 119.4(8) . . ? N6B U N1C 137.2(8) . . ? N3A U N1C 135.9(8) . . ? N3C U N1A 74.8(8) . . ? N6C U N1A 134.3(8) . . ? N1B U N1A 122.1(8) . . ? N6B U N1A 74.7(8) . . ? N3A U N1A 65.1(9) . . ? N1C U N1A 118.6(8) . . ? N3C U N3B 75.8(9) . . ? N6C U N3B 88.1(8) . . ? N1B U N3B 63.2(9) . . ? N6B U N3B 126.8(9) . . ? N3A U N3B 78.8(8) . . ? N1C U N3B 73.0(7) . . ? N1A U N3B 137.5(8) . . ? N3C U N6A 87.9(9) . . ? N6C U N6A 77.7(8) . . ? N1B U N6A 138.9(9) . . ? N6B U N6A 81.2(8) . . ? N3A U N6A 127.3(9) . . ? N1C U N6A 72.6(8) . . ? N1A U N6A 62.2(9) . . ? N3B U N6A 145.6(8) . . ? C1A N1A C5A 115(3) . . ? C1A N1A U 124(2) . . ? C5A N1A U 121(2) . . ? C8A N2A N3A 121(3) . . ? N2A N3A C6A 119(3) . . ? N2A N3A U 121.5(19) . . ? C6A N3A U 118(2) . . ? C7A N4A C6A 116(3) . . ? C11A N5A N6A 120(3) . . ? C9A N6A N5A 119(3) . . ? C9A N6A U 122(2) . . ? N5A N6A U 119(2) . . ? C10A N7A C9A 116(3) . . ? N1A C1A C2A 125(3) . . ? N1A C1A C9A 114(3) . . ? C2A C1A C9A 120(3) . . ? C3A C2A C1A 118(4) . . ? C2A C3A C4A 120(3) . . ? C3A C4A C5A 119(4) . . ? C4A C5A N1A 123(3) . . ? C4A C5A C6A 124(3) . . ? N1A C5A C6A 113(3) . . ? N3A C6A N4A 122(3) . . ? N3A C6A C5A 123(3) . . ? N4A C6A C5A 115(3) . . ? N4A C7A C8A 121(3) . . ? N4A C7A C12A 120(3) . . ? C8A C7A C12A 119(3) . . ? N2A C8A C7A 120(3) . . ? N2A C8A C15A 119(3) . . ? C7A C8A C15A 121(3) . . ? N6A C9A N7A 125(3) . . ? N6A C9A C1A 118(3) . . ? N7A C9A C1A 118(3) . . ? N7A C10A C11A 121(4) . . ? N7A C10A C18A 117(4) . . ? C11A C10A C18A 121(4) . . ? N5A C11A C10A 120(4) . . ? N5A C11A C21A 112(4) . . ? C10A C11A C21A 127(4) . . ? C13D C12A C13A 31(8) . . ? C13D C12A C7A 118(4) . . ? C13A C12A C7A 118(4) . . ? C13D C13A C12A 75(4) . . ? C13D C13A C14A 75(4) . . ? C12A C13A C14A 111(6) . . ? C13A C13D C12A 75(4) . . ? C13A C13D C14A 75(4) . . ? C12A C13D C14A 111(6) . . ? C13D C14A C13A 31(8) . . ? C16A C15A C8A 115(3) . . ? C15A C16A C17A 107(3) . . ? C19A C18A C19D 44(5) . . ? C19A C18A C10A 115(5) . . ? C19D C18A C10A 107(5) . . ? C19D C19A C18A 68(3) . . ? C19D C19A C20A 104(9) . . ? C18A C19A C20A 109(6) . . ? C19D C19A C20D 64(6) . . ? C18A C19A C20D 96(6) . . ? C20A C19A C20D 41(5) . . ? C19A C19D C18A 68(3) . . ? C19A C19D C20D 74(7) . . ? C18A C19D C20D 100(6) . . ? C20D C20A C19A 76(8) . . ? C20A C20D C19D 105(8) . . ? C20A C20D C19A 64(6) . . ? C19D C20D C19A 42(5) . . ? C11A C21A C22A 101(4) . . ? C23A C22A C21A 107.9(18) . . ? C5B N1B C1B 116(3) . . ? C5B N1B U 123(2) . . ? C1B N1B U 121.3(19) . . ? C8B N2B N3B 121(3) . . ? C6B N3B N2B 117(2) . . ? C6B N3B U 122(2) . . ? N2B N3B U 120.5(19) . . ? C7B N4B C6B 113(3) . . ? C11B N5B N6B 117(3) . . ? C9B N6B N5B 121(3) . . ? C9B N6B U 121(2) . . ? N5B N6B U 117.0(19) . . ? C9B N7B C10B 120(3) . . ? N1B C1B C2B 122(3) . . ? N1B C1B C9B 116(3) . . ? C2B C1B C9B 122(4) . . ? C3B C2B C1B 119(4) . . ? C2B C3B C4B 119(3) . . ? C5B C4B C3B 119(3) . . ? C4B C5B N1B 126(3) . . ? C4B C5B C6B 119(3) . . ? N1B C5B C6B 115(3) . . ? N3B C6B N4B 127(3) . . ? N3B C6B C5B 116(3) . . ? N4B C6B C5B 117(3) . . ? N4B C7B C8B 126(3) . . ? N4B C7B C12B 115(4) . . ? C8B C7B C12B 120(4) . . ? N2B C8B C7B 116(4) . . ? N2B C8B C15B 119(4) . . ? C7B C8B C15B 125(3) . . ? N7B C9B N6B 125(3) . . ? N7B C9B C1B 118(3) . . ? N6B C9B C1B 117(3) . . ? N7B C10B C18B 122(4) . . ? N7B C10B C11B 115(4) . . ? C18B C10B C11B 123(4) . . ? N5B C11B C21B 119(3) . . ? N5B C11B C10B 122(3) . . ? C21B C11B C10B 119(4) . . ? C13B C12B C13E 35(4) . . ? C13B C12B C7B 116(4) . . ? C13E C12B C7B 111(4) . . ? C13E C13B C12B 74(3) . . ? C13E C13B C14E 73(3) . . ? C12B C13B C14E 112(6) . . ? C13E C13B C14B 106(8) . . ? C12B C13B C14B 90(8) . . ? C14E C13B C14B 47(7) . . ? C13B C13E C14E 72(3) . . ? C13B C13E C12B 71(2) . . ? C14E C13E C12B 110(6) . . ? C13B C13E C14B 48(6) . . ? C14E C13E C14B 38(5) . . ? C12B C13E C14B 74(6) . . ? C14E C14B C13B 66(4) . . ? C14E C14B C13E 50(4) . . ? C13B C14B C13E 27(4) . . ? C14B C14E C13B 66(4) . . ? C14B C14E C13E 92(6) . . ? C13B C14E C13E 35(4) . . ? C8B C15B C16B 111(9) . . ? C8B C15B C16E 113(4) . . ? C16B C15B C16E 52(7) . . ? C16E C16B C15B 64(4) . . ? C16E C16B C17B 64(4) . . ? C15B C16B C17B 115(4) . . ? C16B C16E C15B 64(3) . . ? C16B C16E C17B 64(3) . . ? C15B C16E C17B 115(4) . . ? C16B C17B C16E 52(7) . . ? C10B C18B C19B 122(6) . . ? C10B C18B C19E 115(5) . . ? C19B C18B C19E 78(8) . . ? C18B C19B C20B 109(8) . . ? C18B C19B C19E 51(4) . . ? C20B C19B C19E 81(8) . . ? C18B C19E C20E 113(7) . . ? C18B C19E C19B 51(4) . . ? C20E C19E C19B 80(7) . . ? C20E C20B C19B 98(10) . . ? C20B C20E C19E 100(9) . . ? C22B C21B C11B 118(4) . . ? C21B C22B C23B 113(4) . . ? C1C N1C C5C 116(3) . . ? C1C N1C U 123(2) . . ? C5C N1C U 121.0(19) . . ? C8C N2C N3C 120(3) . . ? C6C N3C N2C 117(3) . . ? C6C N3C U 122(2) . . ? N2C N3C U 121(2) . . ? C7C N4C C6C 113(3) . . ? C11C N5C N6C 118(3) . . ? C9C N6C N5C 118(3) . . ? C9C N6C U 122(2) . . ? N5C N6C U 119(2) . . ? C10C N7C C9C 113(3) . . ? N1C C1C C2C 125(3) . . ? N1C C1C C9C 114(3) . . ? C2C C1C C9C 120(3) . . ? C3C C2C C1C 117(3) . . ? C2C C3C C4C 122(3) . . ? C5C C4C C3C 118(3) . . ? C4C C5C N1C 122(3) . . ? C4C C5C C6C 124(3) . . ? N1C C5C C6C 113(3) . . ? N3C C6C N4C 128(3) . . ? N3C C6C C5C 119(4) . . ? N4C C6C C5C 113(3) . . ? N4C C7C C8C 122(3) . . ? N4C C7C C12C 116(3) . . ? C8C C7C C12C 122(3) . . ? N2C C8C C7C 120(3) . . ? N2C C8C C15C 118(4) . . ? C7C C8C C15C 122(4) . . ? N6C C9C N7C 125(4) . . ? N6C C9C C1C 117(3) . . ? N7C C9C C1C 118(3) . . ? N7C C10C C11C 122(3) . . ? N7C C10C C18C 113(3) . . ? C11C C10C C18C 125(4) . . ? N5C C11C C10C 123(4) . . ? N5C C11C C21C 115(3) . . ? C10C C11C C21C 121(4) . . ? C13F C12C C13C 50(5) . . ? C13F C12C C7C 120(6) . . ? C13C C12C C7C 112(5) . . ? C13F C13C C12C 65(3) . . ? C13F C13C C14F 68(8) . . ? C12C C13C C14F 105(6) . . ? C13F C13C C14C 137(10) . . ? C12C C13C C14C 145(10) . . ? C14F C13C C14C 72(10) . . ? C13C C13F C12C 65(3) . . ? C13C C13F C14F 66(8) . . ? C12C C13F C14F 104(7) . . ? C13C C14C C14F 57(10) . . ? C13C C14F C13F 46(5) . . ? C13C C14F C14C 51(10) . . ? C13F C14F C14C 95(10) . . ? C16C C15C C8C 116(3) . . ? C15C C16C C17C 122(4) . . ? C10C C18C C19C 109(3) . . ? C20C C19C C20F 32(6) . . ? C20C C19C C18C 124(7) . . ? C20F C19C C18C 104(4) . . ? C20F C20C C19C 74(4) . . ? C20C C20F C19C 73(3) . . ? C22C C21C C11C 120(3) . . ? C21C C22C C23C 115(3) . . ? C2 C1 C6 120.0 . . ? C1 C2 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C12 C7 C8 120.0 . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C7 C12 C11 120.0 . . ? C18 C13 C14 120.0 . . ? C13 C14 C15 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C13 C18 C17 120.0 . . ? C20 C19 C24 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C23 C24 C19 120.0 . . ?