Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr M Ephritikhine' _publ_contact_author_address ; Laboratoire de Chimie de coordinati Service de Chimie Moleculaire CEA Saclay, Batiment 125 Gif sur Yvette F91191 FRANCE ; _publ_contact_author_phone '33 01 69 08 64 36' _publ_contact_author_fax '33 1 69 08 66 40' _publ_contact_author_email ephri@drecam.cea.fr _publ_section_title ; The distinct affinity of cyclopentadienyl ligands towards trivalent uranium and lanthanide ions. Evidence for cooperative ligation and back-bonding in the actinide complexes ; loop_ _publ_author_name 'M. Ephritikhine' 'Jean-Claude Berthet' 'Thouraya Mehdoui' 'Pierre Thuery' data_1 _database_code_depnum_ccdc_archive 'CCDC 258864' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 I2 N3 Nd' _chemical_formula_weight 756.53 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' Nd Nd -0.1943 3.0179 '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 8.3944(4) _cell_length_b 8.7929(5) _cell_length_c 19.0781(12) _cell_angle_alpha 102.409(3) _cell_angle_beta 93.915(3) _cell_angle_gamma 108.264(4) _cell_volume 1291.96(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25027 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light blue' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method ? _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 4.414 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.188 _exptl_absorpt_correction_T_max 0.702 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(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 area-detector diffractometer' _diffrn_measurement_method 'one \f and four \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 25027 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4908 _reflns_number_gt 4674 _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); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) 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^)+(0.0190P)^2^+0.8166P] 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 4908 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.695 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.138 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 Nd Nd 0.51970(2) 0.261047(19) 0.262065(9) 0.03519(6) Uani 1 1 d . . . I1 I 0.76716(3) 0.14209(2) 0.166500(11) 0.04093(7) Uani 1 1 d . . . I2 I 0.32953(3) 0.29983(3) 0.399719(12) 0.04548(7) Uani 1 1 d . . . N1 N 0.2845(3) -0.0294(3) 0.22230(15) 0.0392(6) Uani 1 1 d . . . N2 N 0.6285(4) 0.0821(3) 0.34128(15) 0.0423(6) Uani 1 1 d . . . N3 N 0.7970(3) 0.4725(3) 0.34305(14) 0.0403(6) Uani 1 1 d . . . C1 C 0.3950(4) 0.3418(4) 0.13780(17) 0.0395(7) Uani 1 1 d . . . C2 C 0.2844(4) 0.3530(4) 0.19038(18) 0.0420(7) Uani 1 1 d . . . H2 H 0.1731 0.2834 0.1862 0.050 Uiso 1 1 calc R . . C3 C 0.3711(4) 0.4870(4) 0.24991(18) 0.0432(7) Uani 1 1 d . . . H3 H 0.3258 0.5210 0.2912 0.052 Uiso 1 1 calc R . . C4 C 0.5405(4) 0.5628(4) 0.23668(16) 0.0372(6) Uani 1 1 d . . . H4 H 0.6249 0.6543 0.2666 0.045 Uiso 1 1 calc R . . C5 C 0.5516(4) 0.4674(4) 0.16768(18) 0.0406(7) Uani 1 1 d . . . H5 H 0.6488 0.4856 0.1455 0.049 Uiso 1 1 calc R . . C6 C 0.3431(4) 0.2338(4) 0.06013(17) 0.0411(7) Uani 1 1 d . . . C7 C 0.2749(5) 0.0486(4) 0.05848(19) 0.0494(8) Uani 1 1 d . . . H7A H 0.3638 0.0172 0.0789 0.074 Uiso 1 1 calc R . . H7B H 0.2354 -0.0151 0.0092 0.074 Uiso 1 1 calc R . . H7C H 0.1828 0.0285 0.0863 0.074 Uiso 1 1 calc R . . C8 C 0.2001(5) 0.2772(4) 0.02220(19) 0.0478(8) Uani 1 1 d . . . H8A H 0.1055 0.2588 0.0487 0.072 Uiso 1 1 calc R . . H8B H 0.1648 0.2085 -0.0264 0.072 Uiso 1 1 calc R . . H8C H 0.2414 0.3913 0.0208 0.072 Uiso 1 1 calc R . . C9 C 0.4932(5) 0.2645(4) 0.01718(19) 0.0473(8) Uani 1 1 d . . . H9A H 0.5355 0.3793 0.0171 0.071 Uiso 1 1 calc R . . H9B H 0.4564 0.1983 -0.0318 0.071 Uiso 1 1 calc R . . H9C H 0.5815 0.2350 0.0394 0.071 Uiso 1 1 calc R . . C10 C 0.1172(4) -0.0510(4) 0.21787(18) 0.0407(7) Uani 1 1 d . . . H10 H 0.0842 0.0363 0.2409 0.049 Uiso 1 1 calc R . . C11 C -0.0067(4) -0.1969(4) 0.18075(19) 0.0445(7) Uani 1 1 d . . . H11 H -0.1208 -0.2076 0.1788 0.053 Uiso 1 1 calc R . . C12 C 0.0424(5) -0.3276(4) 0.14625(19) 0.0457(8) Uani 1 1 d . . . H12 H -0.0385 -0.4267 0.1201 0.055 Uiso 1 1 calc R . . C13 C 0.2124(5) -0.3086(4) 0.15127(19) 0.0459(8) Uani 1 1 d . . . H13 H 0.2479 -0.3951 0.1294 0.055 Uiso 1 1 calc R . . C14 C 0.3289(4) -0.1585(4) 0.18932(18) 0.0434(7) Uani 1 1 d . . . H14 H 0.4436 -0.1460 0.1923 0.052 Uiso 1 1 calc R . . C15 C 0.5187(4) -0.0237(4) 0.37170(18) 0.0426(7) Uani 1 1 d . . . H15 H 0.4047 -0.0338 0.3646 0.051 Uiso 1 1 calc R . . C16 C 0.5669(5) -0.1182(4) 0.41302(19) 0.0459(8) Uani 1 1 d . . . H16 H 0.4872 -0.1907 0.4327 0.055 Uiso 1 1 calc R . . C17 C 0.7369(5) -0.1019(4) 0.42424(19) 0.0459(8) Uani 1 1 d . . . H17 H 0.7736 -0.1624 0.4523 0.055 Uiso 1 1 calc R . . C18 C 0.8513(4) 0.0053(4) 0.39322(18) 0.0432(7) Uani 1 1 d . . . H18 H 0.9658 0.0174 0.3995 0.052 Uiso 1 1 calc R . . C19 C 0.7918(4) 0.0945(4) 0.35252(18) 0.0418(7) Uani 1 1 d . . . H19 H 0.8694 0.1668 0.3319 0.050 Uiso 1 1 calc R . . C20 C 0.8177(4) 0.5149(4) 0.41574(18) 0.0415(7) Uani 1 1 d . . . H20 H 0.7312 0.4625 0.4393 0.050 Uiso 1 1 calc R . . C21 C 0.9633(4) 0.6338(4) 0.45721(19) 0.0448(7) Uani 1 1 d . . . H21 H 0.9745 0.6593 0.5076 0.054 Uiso 1 1 calc R . . C22 C 1.0921(4) 0.7143(4) 0.4224(2) 0.0468(8) Uani 1 1 d . . . H22 H 1.1904 0.7955 0.4490 0.056 Uiso 1 1 calc R . . C23 C 1.0713(4) 0.6712(4) 0.34758(19) 0.0441(7) Uani 1 1 d . . . H23 H 1.1555 0.7230 0.3229 0.053 Uiso 1 1 calc R . . C24 C 0.9244(4) 0.5508(4) 0.30996(19) 0.0439(7) Uani 1 1 d . . . H24 H 0.9120 0.5218 0.2596 0.053 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 Nd 0.03433(10) 0.03553(10) 0.03471(10) 0.00900(7) 0.00458(7) 0.01032(7) I1 0.03822(12) 0.04627(12) 0.03793(12) 0.00778(9) 0.00576(9) 0.01548(9) I2 0.04422(13) 0.05083(13) 0.04105(13) 0.01126(9) 0.01238(9) 0.01439(10) N1 0.0394(14) 0.0382(13) 0.0402(14) 0.0140(11) 0.0039(11) 0.0109(11) N2 0.0426(15) 0.0410(14) 0.0418(15) 0.0112(11) 0.0053(12) 0.0117(12) N3 0.0417(15) 0.0392(13) 0.0387(14) 0.0108(11) 0.0038(11) 0.0117(11) C1 0.0441(18) 0.0367(15) 0.0399(17) 0.0135(13) 0.0067(14) 0.0138(13) C2 0.0405(17) 0.0414(16) 0.0460(18) 0.0158(14) 0.0044(14) 0.0133(13) C3 0.0504(19) 0.0442(16) 0.0392(17) 0.0096(13) 0.0067(14) 0.0223(15) C4 0.0427(17) 0.0374(15) 0.0343(15) 0.0086(12) 0.0021(13) 0.0180(13) C5 0.0421(17) 0.0391(15) 0.0417(17) 0.0128(13) 0.0055(14) 0.0137(13) C6 0.0452(18) 0.0407(16) 0.0361(16) 0.0109(13) 0.0041(14) 0.0125(14) C7 0.059(2) 0.0431(17) 0.0394(18) 0.0091(14) 0.0040(16) 0.0095(16) C8 0.0466(19) 0.0527(19) 0.0423(18) 0.0116(15) -0.0003(15) 0.0160(15) C9 0.054(2) 0.0482(18) 0.0401(18) 0.0117(14) 0.0088(15) 0.0161(16) C10 0.0417(18) 0.0408(16) 0.0422(17) 0.0166(13) 0.0074(14) 0.0130(13) C11 0.0393(18) 0.0470(18) 0.0467(19) 0.0163(14) 0.0043(14) 0.0113(14) C12 0.0480(19) 0.0384(16) 0.0430(18) 0.0105(14) -0.0007(15) 0.0052(14) C13 0.057(2) 0.0380(16) 0.0429(18) 0.0104(13) 0.0063(15) 0.0156(15) C14 0.0458(19) 0.0424(16) 0.0445(18) 0.0144(14) 0.0062(14) 0.0159(14) C15 0.0398(17) 0.0454(17) 0.0424(18) 0.0147(14) 0.0065(14) 0.0114(14) C16 0.0478(19) 0.0443(17) 0.0465(19) 0.0164(14) 0.0089(15) 0.0129(15) C17 0.050(2) 0.0461(17) 0.0449(19) 0.0141(14) 0.0053(15) 0.0196(15) C18 0.0409(18) 0.0436(17) 0.0433(18) 0.0089(14) 0.0005(14) 0.0142(14) C19 0.0419(18) 0.0412(16) 0.0409(17) 0.0102(13) 0.0069(14) 0.0120(13) C20 0.0405(17) 0.0449(17) 0.0404(17) 0.0115(13) 0.0060(13) 0.0155(14) C21 0.0440(18) 0.0478(18) 0.0410(18) 0.0050(14) 0.0037(14) 0.0179(15) C22 0.0357(17) 0.0469(18) 0.050(2) 0.0022(14) 0.0000(14) 0.0110(14) C23 0.0374(17) 0.0413(16) 0.0493(19) 0.0091(14) 0.0074(14) 0.0084(14) C24 0.0466(19) 0.0424(16) 0.0401(17) 0.0103(13) 0.0038(14) 0.0119(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 Nd N1 2.607(3) . ? Nd N3 2.612(3) . ? Nd C3 2.696(3) . ? Nd N2 2.707(3) . ? Nd C2 2.745(3) . ? Nd C4 2.753(3) . ? Nd C5 2.788(3) . ? Nd C1 2.841(3) . ? Nd I1 3.1293(3) . ? Nd I2 3.1765(3) . ? N1 C14 1.347(4) . ? N1 C10 1.350(4) . ? N2 C19 1.339(4) . ? N2 C15 1.349(4) . ? N3 C20 1.340(4) . ? N3 C24 1.354(4) . ? C1 C5 1.411(5) . ? C1 C2 1.421(5) . ? C1 C6 1.528(4) . ? C2 C3 1.408(5) . ? C3 C4 1.434(5) . ? C4 C5 1.427(4) . ? C6 C9 1.534(5) . ? C6 C7 1.540(4) . ? C6 C8 1.548(5) . ? C10 C11 1.379(5) . ? C11 C12 1.391(5) . ? C12 C13 1.377(5) . ? C13 C14 1.381(5) . ? C15 C16 1.388(5) . ? C16 C17 1.385(5) . ? C17 C18 1.383(5) . ? C18 C19 1.386(5) . ? C20 C21 1.387(5) . ? C21 C22 1.391(5) . ? C22 C23 1.379(5) . ? C23 C24 1.375(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Nd N3 152.16(8) . . ? N1 Nd N2 76.49(8) . . ? N3 Nd N2 75.81(8) . . ? N1 Nd I1 92.40(6) . . ? N3 Nd I1 84.57(6) . . ? N2 Nd I1 78.19(6) . . ? N1 Nd I2 83.13(6) . . ? N3 Nd I2 88.30(6) . . ? N2 Nd I2 77.45(6) . . ? I1 Nd I2 155.612(8) . . ? C14 N1 C10 117.4(3) . . ? C14 N1 Nd 117.8(2) . . ? C10 N1 Nd 123.0(2) . . ? C19 N2 C15 117.0(3) . . ? C19 N2 Nd 122.2(2) . . ? C15 N2 Nd 120.8(2) . . ? C20 N3 C24 117.7(3) . . ? C20 N3 Nd 123.9(2) . . ? C24 N3 Nd 118.3(2) . . ? C5 C1 C2 106.3(3) . . ? C5 C1 C6 127.3(3) . . ? C2 C1 C6 125.7(3) . . ? C3 C2 C1 108.8(3) . . ? C2 C3 C4 109.1(3) . . ? C5 C4 C3 105.1(3) . . ? C1 C5 C4 110.7(3) . . ? C1 C6 C9 111.1(3) . . ? C1 C6 C7 111.6(3) . . ? C9 C6 C7 108.7(3) . . ? C1 C6 C8 108.7(3) . . ? C9 C6 C8 108.7(3) . . ? C7 C6 C8 108.0(3) . . ? N1 C10 C11 122.9(3) . . ? C10 C11 C12 118.6(3) . . ? C13 C12 C11 119.2(3) . . ? C12 C13 C14 118.7(3) . . ? N1 C14 C13 123.1(3) . . ? N2 C15 C16 123.4(3) . . ? C17 C16 C15 118.3(3) . . ? C18 C17 C16 119.1(3) . . ? C17 C18 C19 118.6(3) . . ? N2 C19 C18 123.5(3) . . ? N3 C20 C21 122.5(3) . . ? C20 C21 C22 119.1(3) . . ? C23 C22 C21 118.6(3) . . ? C24 C23 C22 119.2(3) . . ? N3 C24 C23 122.9(3) . . ? #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 258865' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 I N2 Nd' _chemical_formula_weight 671.73 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.3034(3) _cell_length_b 26.7966(6) _cell_length_c 16.9004(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.365(2) _cell_angle_gamma 90.00 _cell_volume 8440.9(3) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 121274 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent light blue' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method ? _exptl_crystal_F_000 3972 _exptl_absorpt_coefficient_mu 2.959 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.438 _exptl_absorpt_correction_T_max 0.722 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 40 mm' _diffrn_ambient_temperature 100(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 area-detector diffractometer' _diffrn_measurement_method 'one \f and three \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 121274 _diffrn_reflns_av_R_equivalents 0.0989 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.68 _reflns_number_total 15940 _reflns_number_gt 11481 _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); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. The highest residual electron density peaks are located near the neodymium and iodine atoms. 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^)+(0.0516P)^2^+62.6001P] 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 15940 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.145 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.188 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 Nd1 Nd 0.02253(3) 0.28494(2) 0.35214(3) 0.04242(14) Uani 1 1 d . . . Nd2 Nd 0.25161(3) 0.56204(2) 0.48241(3) 0.04243(14) Uani 1 1 d . . . Nd3 Nd 0.54115(3) 0.72308(2) 0.33592(3) 0.04211(14) Uani 1 1 d . . . I1 I -0.03925(4) 0.22456(3) 0.17835(4) 0.04798(17) Uani 1 1 d . . . I2 I 0.24428(3) 0.44458(2) 0.49126(4) 0.04609(17) Uani 1 1 d . . . I3 I 0.48571(4) 0.77941(3) 0.15613(4) 0.04894(17) Uani 1 1 d . . . N1A N -0.0990(4) 0.2463(3) 0.3619(5) 0.0447(19) Uani 1 1 d . . . N2A N 0.1306(4) 0.2996(3) 0.2967(5) 0.0449(19) Uani 1 1 d . . . N1B N 0.1055(4) 0.5499(3) 0.4282(5) 0.0435(18) Uani 1 1 d . . . N2B N 0.3951(4) 0.5428(3) 0.5428(5) 0.047(2) Uani 1 1 d . . . N1C N 0.6491(4) 0.6960(3) 0.2852(5) 0.0455(19) Uani 1 1 d . . . N2C N 0.4150(4) 0.7587(3) 0.3363(5) 0.0454(19) Uani 1 1 d . . . C1B C 0.2759(5) 0.5744(4) 0.6610(6) 0.046(2) Uani 1 1 d . . . C1A C -0.0368(5) 0.3773(3) 0.2654(6) 0.044(2) Uani 1 1 d . . . C1C C 0.6038(5) 0.8130(4) 0.4285(6) 0.044(2) Uani 1 1 d . . . C2C C 0.6603(5) 0.7817(4) 0.4311(6) 0.048(2) Uani 1 1 d . . . H2C H 0.6918 0.7883 0.4049 0.058 Uiso 1 1 calc R . . C2B C 0.2074(5) 0.5941(4) 0.6107(6) 0.048(2) Uani 1 1 d . . . H2B H 0.1640 0.5814 0.6082 0.058 Uiso 1 1 calc R . . C2A C 0.0343(6) 0.3869(4) 0.3259(7) 0.055(3) Uani 1 1 d . . . H2A H 0.0729 0.3956 0.3123 0.066 Uiso 1 1 calc R . . C3B C 0.2150(6) 0.6353(4) 0.5657(7) 0.052(3) Uani 1 1 d . . . H3B H 0.1777 0.6546 0.5279 0.063 Uiso 1 1 calc R . . C3A C 0.0368(5) 0.3811(4) 0.4093(7) 0.047(2) Uani 1 1 d . . . H3A H 0.0766 0.3868 0.4602 0.056 Uiso 1 1 calc R . . C3C C 0.6614(5) 0.7394(4) 0.4791(6) 0.052(3) Uani 1 1 d . . . H3C H 0.6937 0.7131 0.4909 0.062 Uiso 1 1 calc R . . C4C C 0.6056(5) 0.7434(4) 0.5064(6) 0.050(2) Uani 1 1 d . . . H4C H 0.5940 0.7201 0.5396 0.060 Uiso 1 1 calc R . . C4B C 0.2896(6) 0.6432(4) 0.5868(6) 0.052(3) Uani 1 1 d . . . H4B H 0.3101 0.6681 0.5658 0.062 Uiso 1 1 calc R . . C4A C -0.0314(6) 0.3652(4) 0.4032(7) 0.051(3) Uani 1 1 d . . . H4A H -0.0441 0.3575 0.4490 0.061 Uiso 1 1 calc R . . C5C C 0.5699(5) 0.7881(4) 0.4757(6) 0.046(2) Uani 1 1 d . . . H5C H 0.5302 0.7997 0.4847 0.056 Uiso 1 1 calc R . . C5B C 0.3252(5) 0.6058(4) 0.6452(6) 0.051(3) Uani 1 1 d . . . H5B H 0.3747 0.6020 0.6704 0.061 Uiso 1 1 calc R . . C5A C -0.0765(6) 0.3631(4) 0.3153(7) 0.048(2) Uani 1 1 d . . . H5A H -0.1246 0.3539 0.2929 0.058 Uiso 1 1 calc R . . C6B C 0.2933(5) 0.5353(4) 0.7323(6) 0.047(2) Uani 1 1 d . . . C6A C -0.0667(5) 0.3889(4) 0.1695(6) 0.047(2) Uani 1 1 d . . . C6C C 0.5913(5) 0.8677(4) 0.3988(7) 0.050(2) Uani 1 1 d . . . C7C C 0.6243(6) 0.8796(4) 0.3346(7) 0.062(3) Uani 1 1 d . . . H7C1 H 0.6754 0.8750 0.3615 0.093 Uiso 1 1 calc R . . H7C2 H 0.6139 0.9136 0.3158 0.093 Uiso 1 1 calc R . . H7C3 H 0.6046 0.8577 0.2858 0.093 Uiso 1 1 calc R . . C7B C 0.3143(6) 0.5624(4) 0.8187(7) 0.063(3) Uani 1 1 d . . . H7B1 H 0.3258 0.5383 0.8643 0.094 Uiso 1 1 calc R . . H7B2 H 0.2750 0.5827 0.8175 0.094 Uiso 1 1 calc R . . H7B3 H 0.3554 0.5831 0.8285 0.094 Uiso 1 1 calc R . . C7A C -0.0764(6) 0.4461(4) 0.1612(8) 0.062(3) Uani 1 1 d . . . H7A1 H -0.1089 0.4566 0.1865 0.093 Uiso 1 1 calc R . . H7A2 H -0.0954 0.4553 0.1014 0.093 Uiso 1 1 calc R . . H7A3 H -0.0308 0.4621 0.1905 0.093 Uiso 1 1 calc R . . C8C C 0.5097(5) 0.8791(4) 0.3571(7) 0.057(3) Uani 1 1 d . . . H8C1 H 0.4867 0.8565 0.3100 0.085 Uiso 1 1 calc R . . H8C2 H 0.5024 0.9128 0.3360 0.085 Uiso 1 1 calc R . . H8C3 H 0.4895 0.8750 0.3993 0.085 Uiso 1 1 calc R . . C8A C -0.1393(5) 0.3643(4) 0.1210(7) 0.055(3) Uani 1 1 d . . . H8A1 H -0.1334 0.3287 0.1222 0.083 Uiso 1 1 calc R . . H8A2 H -0.1588 0.3757 0.0624 0.083 Uiso 1 1 calc R . . H8A3 H -0.1713 0.3730 0.1481 0.083 Uiso 1 1 calc R . . C8B C 0.2280(6) 0.5012(4) 0.7153(7) 0.061(3) Uani 1 1 d . . . H8B1 H 0.2395 0.4770 0.7607 0.091 Uiso 1 1 calc R . . H8B2 H 0.2159 0.4843 0.6612 0.091 Uiso 1 1 calc R . . H8B3 H 0.1880 0.5210 0.7133 0.091 Uiso 1 1 calc R . . C9A C -0.0141(6) 0.3731(4) 0.1289(7) 0.055(3) Uani 1 1 d . . . H9A1 H 0.0324 0.3869 0.1619 0.082 Uiso 1 1 calc R . . H9A2 H -0.0310 0.3853 0.0708 0.082 Uiso 1 1 calc R . . H9A3 H -0.0110 0.3374 0.1288 0.082 Uiso 1 1 calc R . . C9B C 0.3580(5) 0.5026(4) 0.7362(6) 0.051(3) Uani 1 1 d . . . H9B1 H 0.3990 0.5235 0.7470 0.077 Uiso 1 1 calc R . . H9B2 H 0.3459 0.4856 0.6822 0.077 Uiso 1 1 calc R . . H9B3 H 0.3689 0.4785 0.7817 0.077 Uiso 1 1 calc R . . C9C C 0.6257(6) 0.9005(4) 0.4799(7) 0.060(3) Uani 1 1 d . . . H9C1 H 0.6006 0.8956 0.5170 0.089 Uiso 1 1 calc R . . H9C2 H 0.6228 0.9349 0.4633 0.089 Uiso 1 1 calc R . . H9C3 H 0.6751 0.8912 0.5100 0.089 Uiso 1 1 calc R . . C10C C 0.4791(5) 0.6280(4) 0.2644(6) 0.045(2) Uani 1 1 d . . . C10A C 0.0947(5) 0.2015(4) 0.4583(6) 0.048(2) Uani 1 1 d . . . C10B C 0.2234(5) 0.5637(4) 0.3010(6) 0.048(2) Uani 1 1 d . . . C11A C 0.0551(5) 0.2251(4) 0.5000(6) 0.045(2) Uani 1 1 d . . . H11A H 0.0168 0.2108 0.5090 0.053 Uiso 1 1 calc R . . C11B C 0.1813(5) 0.6008(4) 0.3150(6) 0.048(2) Uani 1 1 d . . . H11B H 0.1314 0.6008 0.2918 0.058 Uiso 1 1 calc R . . C11C C 0.4439(5) 0.6457(4) 0.3161(7) 0.048(2) Uani 1 1 d . . . H11C H 0.3958 0.6550 0.2956 0.058 Uiso 1 1 calc R . . C12A C 0.0819(6) 0.2730(4) 0.5258(6) 0.052(3) Uani 1 1 d . . . H12A H 0.0649 0.2959 0.5546 0.063 Uiso 1 1 calc R . . C12B C 0.2243(6) 0.6383(4) 0.3689(6) 0.051(3) Uani 1 1 d . . . H12B H 0.2091 0.6664 0.3893 0.061 Uiso 1 1 calc R . . C12C C 0.4921(6) 0.6472(4) 0.4034(7) 0.053(3) Uani 1 1 d . . . H12C H 0.4817 0.6575 0.4497 0.063 Uiso 1 1 calc R . . C13A C 0.1389(6) 0.2803(4) 0.5006(6) 0.052(3) Uani 1 1 d . . . H13A H 0.1663 0.3092 0.5091 0.062 Uiso 1 1 calc R . . C13B C 0.2957(5) 0.6244(4) 0.3855(7) 0.052(3) Uani 1 1 d . . . H13B H 0.3366 0.6426 0.4177 0.062 Uiso 1 1 calc R . . C13C C 0.5585(6) 0.6304(4) 0.4072(7) 0.052(3) Uani 1 1 d . . . H13C H 0.6001 0.6272 0.4569 0.062 Uiso 1 1 calc R . . C14C C 0.5516(5) 0.6189(4) 0.3218(6) 0.046(2) Uani 1 1 d . . . H14C H 0.5881 0.6075 0.3062 0.055 Uiso 1 1 calc R . . C14A C 0.1476(5) 0.2362(4) 0.4597(6) 0.048(2) Uani 1 1 d . . . H14A H 0.1823 0.2310 0.4375 0.058 Uiso 1 1 calc R . . C14B C 0.2948(5) 0.5795(4) 0.3463(6) 0.049(2) Uani 1 1 d . . . H14B H 0.3352 0.5620 0.3492 0.059 Uiso 1 1 calc R . . C15B C 0.1965(5) 0.5215(4) 0.2348(6) 0.048(2) Uani 1 1 d . . . C15C C 0.4452(5) 0.6125(4) 0.1711(6) 0.047(2) Uani 1 1 d . . . C15A C 0.0908(5) 0.1465(4) 0.4319(6) 0.047(2) Uani 1 1 d . . . C16C C 0.3732(6) 0.6389(4) 0.1237(7) 0.059(3) Uani 1 1 d . . . H16A H 0.3808 0.6743 0.1251 0.088 Uiso 1 1 calc R . . H16B H 0.3413 0.6312 0.1515 0.088 Uiso 1 1 calc R . . H16C H 0.3524 0.6278 0.0650 0.088 Uiso 1 1 calc R . . C16B C 0.2544(6) 0.4819(4) 0.2479(7) 0.061(3) Uani 1 1 d . . . H16D H 0.2667 0.4662 0.3030 0.092 Uiso 1 1 calc R . . H16E H 0.2962 0.4975 0.2457 0.092 Uiso 1 1 calc R . . H16F H 0.2365 0.4572 0.2032 0.092 Uiso 1 1 calc R . . C16A C 0.1298(6) 0.1162(4) 0.5154(7) 0.058(3) Uani 1 1 d . . . H16G H 0.1788 0.1270 0.5424 0.087 Uiso 1 1 calc R . . H16H H 0.1284 0.0814 0.5016 0.087 Uiso 1 1 calc R . . H16I H 0.1063 0.1215 0.5542 0.087 Uiso 1 1 calc R . . C17B C 0.1289(5) 0.4967(4) 0.2396(7) 0.054(3) Uani 1 1 d . . . H17A H 0.0931 0.5218 0.2321 0.080 Uiso 1 1 calc R . . H17B H 0.1416 0.4810 0.2948 0.080 Uiso 1 1 calc R . . H17C H 0.1102 0.4721 0.1949 0.080 Uiso 1 1 calc R . . C17C C 0.4942(6) 0.6241(4) 0.1238(7) 0.057(3) Uani 1 1 d . . . H17D H 0.4732 0.6111 0.0663 0.085 Uiso 1 1 calc R . . H17E H 0.5403 0.6090 0.1540 0.085 Uiso 1 1 calc R . . H17F H 0.4998 0.6596 0.1216 0.085 Uiso 1 1 calc R . . C17A C 0.1280(6) 0.1375(5) 0.3714(7) 0.062(3) Uani 1 1 d . . . H17G H 0.1072 0.1585 0.3217 0.093 Uiso 1 1 calc R . . H17H H 0.1223 0.1032 0.3537 0.093 Uiso 1 1 calc R . . H17I H 0.1781 0.1450 0.4004 0.093 Uiso 1 1 calc R . . C18A C 0.0125(5) 0.1289(4) 0.3897(7) 0.058(3) Uani 1 1 d . . . H18A H -0.0100 0.1328 0.4297 0.087 Uiso 1 1 calc R . . H18B H 0.0113 0.0944 0.3739 0.087 Uiso 1 1 calc R . . H18C H -0.0127 0.1484 0.3390 0.087 Uiso 1 1 calc R . . C18B C 0.1758(6) 0.5454(4) 0.1446(7) 0.060(3) Uani 1 1 d . . . H18D H 0.1631 0.5197 0.1016 0.090 Uiso 1 1 calc R . . H18E H 0.2159 0.5640 0.1435 0.090 Uiso 1 1 calc R . . H18F H 0.1358 0.5674 0.1329 0.090 Uiso 1 1 calc R . . C18C C 0.4324(6) 0.5554(4) 0.1683(7) 0.061(3) Uani 1 1 d . . . H18G H 0.4114 0.5445 0.1094 0.092 Uiso 1 1 calc R . . H18H H 0.4005 0.5478 0.1961 0.092 Uiso 1 1 calc R . . H18I H 0.4773 0.5386 0.1977 0.092 Uiso 1 1 calc R . . C19C C 0.6517(5) 0.7048(4) 0.2089(7) 0.050(2) Uani 1 1 d . . . H19C H 0.6187 0.7270 0.1716 0.060 Uiso 1 1 calc R . . C19A C -0.1443(5) 0.2126(4) 0.3097(7) 0.051(2) Uani 1 1 d . . . H19A H -0.1393 0.2044 0.2589 0.061 Uiso 1 1 calc R . . C19B C 0.0692(5) 0.5076(4) 0.4236(7) 0.050(2) Uani 1 1 d . . . H19B H 0.0952 0.4782 0.4416 0.060 Uiso 1 1 calc R . . C20C C 0.7014(6) 0.6825(4) 0.1822(7) 0.056(3) Uani 1 1 d . . . H20C H 0.7012 0.6892 0.1282 0.067 Uiso 1 1 calc R . . C20A C -0.1986(5) 0.1891(4) 0.3268(7) 0.057(3) Uani 1 1 d . . . H20A H -0.2274 0.1650 0.2894 0.068 Uiso 1 1 calc R . . C20B C -0.0049(6) 0.5050(4) 0.3937(7) 0.056(3) Uani 1 1 d . . . H20B H -0.0275 0.4747 0.3922 0.067 Uiso 1 1 calc R . . C21B C -0.0443(6) 0.5477(4) 0.3663(8) 0.063(3) Uani 1 1 d . . . H21B H -0.0941 0.5471 0.3454 0.076 Uiso 1 1 calc R . . C21A C -0.2087(6) 0.2021(4) 0.3990(7) 0.053(3) Uani 1 1 d . . . H21A H -0.2455 0.1878 0.4108 0.064 Uiso 1 1 calc R . . C21C C 0.7502(6) 0.6505(4) 0.2371(7) 0.057(3) Uani 1 1 d . . . H21C H 0.7836 0.6349 0.2204 0.069 Uiso 1 1 calc R . . C22A C -0.1638(5) 0.2366(4) 0.4541(7) 0.049(2) Uani 1 1 d . . . H22A H -0.1691 0.2458 0.5043 0.059 Uiso 1 1 calc R . . C22B C -0.0076(5) 0.5920(4) 0.3708(6) 0.048(2) Uani 1 1 d . . . H22B H -0.0324 0.6219 0.3529 0.057 Uiso 1 1 calc R . . C22C C 0.7506(5) 0.6413(4) 0.3160(6) 0.050(3) Uani 1 1 d . . . H22C H 0.7845 0.6202 0.3546 0.061 Uiso 1 1 calc R . . C23C C 0.6986(5) 0.6644(4) 0.3376(7) 0.049(2) Uani 1 1 d . . . H23C H 0.6982 0.6576 0.3913 0.058 Uiso 1 1 calc R . . C23A C -0.1102(5) 0.2574(4) 0.4330(6) 0.048(2) Uani 1 1 d . . . H23A H -0.0799 0.2807 0.4709 0.058 Uiso 1 1 calc R . . C23B C 0.0651(5) 0.5908(4) 0.4019(6) 0.049(2) Uani 1 1 d . . . H23B H 0.0888 0.6209 0.4052 0.059 Uiso 1 1 calc R . . C24C C 0.3620(5) 0.7810(4) 0.2699(6) 0.047(2) Uani 1 1 d . . . H24C H 0.3692 0.7866 0.2196 0.056 Uiso 1 1 calc R . . C24A C 0.1382(5) 0.2786(4) 0.2293(6) 0.052(3) Uani 1 1 d . . . H24A H 0.1022 0.2574 0.1946 0.062 Uiso 1 1 calc R . . C24B C 0.4403(5) 0.5821(4) 0.5623(6) 0.047(2) Uani 1 1 d . . . H24B H 0.4205 0.6139 0.5488 0.057 Uiso 1 1 calc R . . C25A C 0.1958(6) 0.2865(5) 0.2082(7) 0.062(3) Uani 1 1 d . . . H25A H 0.1988 0.2705 0.1610 0.075 Uiso 1 1 calc R . . C25B C 0.5120(6) 0.5781(4) 0.6000(7) 0.054(3) Uani 1 1 d . . . H25B H 0.5405 0.6066 0.6120 0.065 Uiso 1 1 calc R . . C25C C 0.2982(6) 0.7959(4) 0.2720(7) 0.058(3) Uani 1 1 d . . . H25C H 0.2633 0.8113 0.2246 0.070 Uiso 1 1 calc R . . C26B C 0.5435(5) 0.5314(4) 0.6210(7) 0.055(3) Uani 1 1 d . . . H26B H 0.5931 0.5278 0.6472 0.065 Uiso 1 1 calc R . . C26A C 0.2500(6) 0.3189(4) 0.2583(7) 0.058(3) Uani 1 1 d . . . H26A H 0.2897 0.3248 0.2453 0.070 Uiso 1 1 calc R . . C26C C 0.2869(6) 0.7874(4) 0.3464(8) 0.060(3) Uani 1 1 d . . . H26C H 0.2437 0.7964 0.3493 0.072 Uiso 1 1 calc R . . C27A C 0.2432(5) 0.3416(4) 0.3265(6) 0.050(2) Uani 1 1 d . . . H27A H 0.2783 0.3636 0.3612 0.060 Uiso 1 1 calc R . . C27B C 0.4994(5) 0.4911(4) 0.6019(7) 0.050(2) Uani 1 1 d . . . H27B H 0.5186 0.4591 0.6151 0.060 Uiso 1 1 calc R . . C27C C 0.3403(6) 0.7656(4) 0.4161(7) 0.053(3) Uani 1 1 d . . . H27C H 0.3345 0.7600 0.4672 0.064 Uiso 1 1 calc R . . C28B C 0.4264(5) 0.4975(4) 0.5633(6) 0.048(2) Uani 1 1 d . . . H28B H 0.3972 0.4693 0.5505 0.058 Uiso 1 1 calc R . . C28A C 0.1830(5) 0.3316(4) 0.3438(6) 0.048(2) Uani 1 1 d . . . H28A H 0.1785 0.3477 0.3901 0.058 Uiso 1 1 calc R . . C28C C 0.4029(5) 0.7522(4) 0.4077(7) 0.049(2) Uani 1 1 d . . . H28C H 0.4391 0.7376 0.4550 0.059 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 Nd1 0.0445(3) 0.0407(3) 0.0423(3) -0.0022(2) 0.0174(2) -0.0034(2) Nd2 0.0404(3) 0.0378(3) 0.0463(3) 0.0007(2) 0.0142(2) 0.0000(2) Nd3 0.0448(3) 0.0424(3) 0.0391(3) 0.0022(2) 0.0165(2) 0.0037(2) I1 0.0530(4) 0.0450(4) 0.0448(4) -0.0031(3) 0.0181(3) -0.0046(3) I2 0.0502(4) 0.0405(4) 0.0458(4) 0.0005(3) 0.0171(3) -0.0003(3) I3 0.0549(4) 0.0480(4) 0.0432(3) 0.0049(3) 0.0187(3) 0.0061(3) N1A 0.042(5) 0.038(5) 0.052(5) -0.001(4) 0.016(4) 0.005(4) N2A 0.049(5) 0.041(5) 0.047(5) -0.001(4) 0.023(4) 0.004(4) N1B 0.047(5) 0.040(5) 0.045(4) -0.001(4) 0.020(4) -0.004(4) N2B 0.042(5) 0.044(5) 0.054(5) 0.001(4) 0.017(4) 0.001(4) N1C 0.047(5) 0.044(5) 0.043(5) 0.003(4) 0.016(4) -0.003(4) N2C 0.041(5) 0.045(5) 0.049(5) -0.003(4) 0.016(4) -0.002(4) C1B 0.049(6) 0.053(6) 0.041(5) -0.011(4) 0.023(4) 0.000(5) C1A 0.050(6) 0.033(5) 0.053(6) 0.001(4) 0.024(5) 0.002(4) C1C 0.042(5) 0.053(6) 0.035(5) -0.007(4) 0.011(4) -0.008(4) C2C 0.045(6) 0.052(6) 0.045(5) -0.002(5) 0.015(4) 0.004(5) C2B 0.049(6) 0.048(6) 0.054(6) -0.009(5) 0.026(5) 0.001(5) C2A 0.065(7) 0.042(6) 0.057(7) -0.006(5) 0.022(5) -0.003(5) C3B 0.061(7) 0.043(6) 0.054(6) -0.004(5) 0.024(5) 0.005(5) C3A 0.055(6) 0.037(5) 0.055(6) -0.010(5) 0.029(5) -0.007(4) C3C 0.044(6) 0.063(7) 0.044(6) -0.005(5) 0.013(5) 0.010(5) C4C 0.056(6) 0.054(6) 0.038(5) -0.001(5) 0.016(5) -0.009(5) C4B 0.059(7) 0.041(6) 0.050(6) -0.009(5) 0.017(5) -0.010(5) C4A 0.066(7) 0.044(6) 0.057(6) 0.003(5) 0.039(5) -0.003(5) C5C 0.040(5) 0.050(6) 0.047(6) -0.012(5) 0.015(4) 0.008(4) C5B 0.045(6) 0.051(6) 0.048(6) -0.004(5) 0.010(5) -0.012(5) C5A 0.054(6) 0.040(6) 0.058(6) -0.003(5) 0.029(5) 0.000(4) C6B 0.049(6) 0.045(6) 0.052(6) -0.009(5) 0.024(5) 0.003(4) C6A 0.059(6) 0.042(6) 0.044(5) 0.001(4) 0.025(5) -0.001(5) C6C 0.047(6) 0.045(6) 0.052(6) -0.005(5) 0.013(5) 0.005(5) C7C 0.067(7) 0.058(7) 0.056(7) 0.000(5) 0.019(6) -0.004(6) C7B 0.062(7) 0.058(7) 0.063(7) -0.004(6) 0.020(6) 0.000(6) C7A 0.065(7) 0.052(7) 0.074(8) 0.007(6) 0.032(6) 0.005(5) C8C 0.058(7) 0.054(7) 0.060(7) 0.001(5) 0.025(5) 0.006(5) C8A 0.055(7) 0.060(7) 0.052(6) 0.005(5) 0.024(5) 0.004(5) C8B 0.058(7) 0.053(7) 0.066(7) -0.002(6) 0.020(6) -0.006(5) C9A 0.064(7) 0.062(7) 0.049(6) 0.000(5) 0.033(5) -0.004(5) C9B 0.055(6) 0.055(7) 0.046(6) 0.003(5) 0.023(5) 0.007(5) C9C 0.071(7) 0.046(6) 0.059(7) -0.015(5) 0.024(6) 0.000(5) C10C 0.052(6) 0.034(5) 0.053(6) -0.003(4) 0.025(5) -0.001(4) C10A 0.043(6) 0.051(6) 0.040(5) 0.007(5) 0.005(4) 0.002(5) C10B 0.045(6) 0.042(6) 0.054(6) 0.009(5) 0.018(5) 0.001(4) C11A 0.051(6) 0.051(6) 0.037(5) 0.012(4) 0.024(4) 0.003(5) C11B 0.046(6) 0.055(6) 0.043(5) 0.013(5) 0.016(4) -0.001(5) C11C 0.048(6) 0.043(6) 0.058(6) 0.006(5) 0.027(5) 0.002(4) C12A 0.064(7) 0.052(7) 0.039(5) 0.000(5) 0.017(5) 0.003(5) C12B 0.060(7) 0.044(6) 0.048(6) 0.011(5) 0.019(5) 0.007(5) C12C 0.061(7) 0.036(6) 0.068(7) 0.004(5) 0.034(6) -0.004(5) C13A 0.060(7) 0.048(6) 0.039(5) -0.005(5) 0.011(5) -0.004(5) C13B 0.048(6) 0.048(6) 0.058(6) 0.010(5) 0.020(5) -0.006(5) C13C 0.062(7) 0.035(6) 0.051(6) 0.010(5) 0.015(5) 0.006(5) C14C 0.039(5) 0.041(5) 0.062(6) 0.012(5) 0.026(5) -0.003(4) C14A 0.040(5) 0.062(7) 0.042(5) 0.007(5) 0.015(4) 0.002(5) C14B 0.041(6) 0.051(6) 0.055(6) 0.010(5) 0.018(5) -0.004(4) C15B 0.050(6) 0.054(6) 0.045(6) 0.005(5) 0.024(5) -0.003(5) C15C 0.052(6) 0.046(6) 0.048(6) 0.002(5) 0.023(5) -0.003(5) C15A 0.043(6) 0.047(6) 0.049(6) 0.011(5) 0.017(4) 0.004(4) C16C 0.055(7) 0.066(8) 0.057(7) -0.004(6) 0.023(5) -0.003(5) C16B 0.062(7) 0.054(7) 0.064(7) -0.005(6) 0.021(6) 0.002(5) C16A 0.064(7) 0.048(6) 0.060(7) 0.015(5) 0.023(5) 0.010(5) C17B 0.048(6) 0.053(7) 0.057(6) -0.005(5) 0.018(5) -0.008(5) C17C 0.056(7) 0.068(8) 0.047(6) -0.006(5) 0.022(5) -0.003(5) C17A 0.064(7) 0.064(8) 0.062(7) -0.001(6) 0.030(6) 0.009(6) C18A 0.054(7) 0.055(7) 0.063(7) -0.002(5) 0.021(5) -0.002(5) C18B 0.066(7) 0.060(7) 0.049(6) -0.003(5) 0.018(5) -0.004(6) C18C 0.059(7) 0.054(7) 0.067(7) -0.005(6) 0.020(6) -0.008(5) C19C 0.048(6) 0.053(6) 0.050(6) 0.006(5) 0.018(5) -0.003(5) C19A 0.048(6) 0.055(7) 0.050(6) -0.004(5) 0.019(5) -0.003(5) C19B 0.051(6) 0.043(6) 0.060(6) 0.000(5) 0.026(5) 0.000(5) C20C 0.056(7) 0.065(7) 0.052(6) -0.001(5) 0.027(5) 0.000(5) C20A 0.047(6) 0.052(7) 0.068(7) -0.007(6) 0.020(5) -0.011(5) C20B 0.053(7) 0.046(6) 0.079(8) -0.006(6) 0.037(6) -0.011(5) C21B 0.045(6) 0.059(7) 0.087(8) -0.003(6) 0.026(6) -0.002(5) C21A 0.055(6) 0.055(7) 0.053(6) -0.002(5) 0.026(5) -0.006(5) C21C 0.054(7) 0.061(7) 0.067(7) 0.007(6) 0.034(6) 0.010(5) C22A 0.046(6) 0.050(6) 0.057(6) -0.002(5) 0.025(5) 0.003(5) C22B 0.049(6) 0.047(6) 0.058(6) -0.003(5) 0.032(5) 0.007(5) C22C 0.052(6) 0.059(7) 0.046(6) 0.008(5) 0.026(5) 0.000(5) C23C 0.049(6) 0.049(6) 0.048(6) 0.002(5) 0.019(5) -0.005(5) C23A 0.052(6) 0.048(6) 0.043(5) 0.001(5) 0.016(5) -0.004(5) C23B 0.054(7) 0.040(6) 0.042(5) -0.001(4) 0.007(5) 0.001(5) C24C 0.041(6) 0.052(6) 0.047(6) 0.005(5) 0.019(4) 0.000(5) C24A 0.043(6) 0.064(7) 0.048(6) -0.003(5) 0.018(5) 0.000(5) C24B 0.051(6) 0.041(6) 0.055(6) 0.001(5) 0.027(5) 0.003(5) C25A 0.056(7) 0.080(9) 0.049(6) -0.013(6) 0.019(5) -0.003(6) C25B 0.052(7) 0.050(6) 0.052(6) 0.002(5) 0.011(5) -0.011(5) C25C 0.054(7) 0.059(7) 0.059(7) 0.015(5) 0.020(5) 0.005(5) C26B 0.037(6) 0.058(7) 0.063(7) 0.002(5) 0.014(5) 0.005(5) C26A 0.052(6) 0.070(8) 0.062(7) 0.000(6) 0.032(5) -0.007(6) C26C 0.047(6) 0.059(7) 0.082(8) 0.009(6) 0.035(6) 0.011(5) C27A 0.044(6) 0.058(7) 0.048(6) -0.003(5) 0.017(5) 0.000(5) C27B 0.049(6) 0.050(6) 0.058(6) 0.009(5) 0.028(5) 0.011(5) C27C 0.057(7) 0.052(6) 0.056(6) 0.000(5) 0.027(5) -0.001(5) C28B 0.054(6) 0.041(6) 0.052(6) 0.002(5) 0.025(5) -0.003(5) C28A 0.055(6) 0.045(6) 0.046(6) 0.001(5) 0.021(5) -0.002(5) C28C 0.044(6) 0.044(6) 0.059(6) -0.001(5) 0.022(5) 0.001(4) _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 Nd1 C13A 2.681(10) . ? Nd1 C4A 2.706(10) . ? Nd1 C12A 2.714(10) . ? Nd1 C3A 2.727(9) . ? Nd1 N2A 2.735(8) . ? Nd1 N1A 2.740(8) . ? Nd1 C14A 2.792(9) . ? Nd1 C2A 2.794(11) . ? Nd1 C5A 2.797(10) . ? Nd1 C11A 2.819(9) . ? Nd1 C10A 2.878(10) . ? Nd1 C1A 2.886(9) . ? Nd1 I1 3.1457(8) . ? Nd2 C3B 2.686(10) . ? Nd2 C12B 2.706(9) . ? Nd2 C4B 2.712(10) . ? Nd2 N2B 2.728(8) . ? Nd2 C13B 2.727(10) . ? Nd2 N1B 2.756(8) . ? Nd2 C2B 2.790(9) . ? Nd2 C14B 2.806(10) . ? Nd2 C5B 2.813(10) . ? Nd2 C11B 2.814(9) . ? Nd2 C1B 2.879(9) . ? Nd2 C10B 2.887(10) . ? Nd2 I2 3.1574(9) . ? Nd3 C12C 2.706(10) . ? Nd3 C3C 2.706(10) . ? Nd3 C4C 2.705(9) . ? Nd3 C13C 2.722(9) . ? Nd3 N2C 2.735(8) . ? Nd3 N1C 2.749(8) . ? Nd3 C11C 2.791(10) . ? Nd3 C2C 2.796(10) . ? Nd3 C5C 2.804(9) . ? Nd3 C14C 2.817(10) . ? Nd3 C1C 2.880(10) . ? Nd3 C10C 2.887(9) . ? Nd3 I3 3.1725(8) . ? N1A C19A 1.340(12) . ? N1A C23A 1.343(12) . ? N2A C24A 1.332(12) . ? N2A C28A 1.351(12) . ? N1B C23B 1.334(12) . ? N1B C19B 1.336(12) . ? N2B C24B 1.349(12) . ? N2B C28B 1.351(12) . ? N1C C19C 1.334(12) . ? N1C C23C 1.343(12) . ? N2C C28C 1.335(12) . ? N2C C24C 1.348(12) . ? C1B C2B 1.413(14) . ? C1B C5B 1.411(14) . ? C1B C6B 1.530(14) . ? C1A C2A 1.422(14) . ? C1A C5A 1.429(13) . ? C1A C6A 1.521(13) . ? C1C C2C 1.407(14) . ? C1C C5C 1.411(14) . ? C1C C6C 1.537(14) . ? C2C C3C 1.389(14) . ? C2B C3B 1.383(14) . ? C2A C3A 1.399(14) . ? C3B C4B 1.427(15) . ? C3A C4A 1.412(14) . ? C3C C4C 1.386(14) . ? C4C C5C 1.389(14) . ? C4B C5B 1.391(14) . ? C4A C5A 1.405(14) . ? C6B C7B 1.533(14) . ? C6B C8B 1.540(14) . ? C6B C9B 1.558(13) . ? C6A C8A 1.523(14) . ? C6A C9A 1.539(13) . ? C6A C7A 1.546(14) . ? C6C C7C 1.518(15) . ? C6C C9C 1.542(14) . ? C6C C8C 1.552(14) . ? C10C C11C 1.414(13) . ? C10C C14C 1.427(13) . ? C10C C15C 1.507(14) . ? C10A C14A 1.416(14) . ? C10A C11A 1.412(14) . ? C10A C15A 1.531(14) . ? C10B C11B 1.392(14) . ? C10B C14B 1.409(13) . ? C10B C15B 1.532(14) . ? C11A C12A 1.396(14) . ? C11B C12B 1.403(14) . ? C11C C12C 1.410(14) . ? C12A C13A 1.397(15) . ? C12B C13B 1.413(14) . ? C12C C13C 1.399(15) . ? C13A C14A 1.415(14) . ? C13B C14B 1.369(15) . ? C13C C14C 1.427(14) . ? C15B C16B 1.532(14) . ? C15B C18B 1.551(14) . ? C15B C17B 1.555(13) . ? C15C C16C 1.534(14) . ? C15C C17C 1.535(14) . ? C15C C18C 1.548(14) . ? C15A C17A 1.512(14) . ? C15A C18A 1.537(14) . ? C15A C16A 1.546(13) . ? C19C C20C 1.393(14) . ? C19A C20A 1.395(14) . ? C19B C20B 1.385(14) . ? C20C C21C 1.358(15) . ? C20A C21A 1.360(14) . ? C20B C21B 1.367(15) . ? C21B C22B 1.386(15) . ? C21A C22A 1.371(14) . ? C21C C22C 1.352(14) . ? C22A C23A 1.389(14) . ? C22B C23B 1.358(14) . ? C22C C23C 1.390(14) . ? C24C C25C 1.370(14) . ? C24A C25A 1.367(15) . ? C24B C25B 1.343(14) . ? C25A C26A 1.393(15) . ? C25B C26B 1.386(14) . ? C25C C26C 1.383(15) . ? C26B C27B 1.359(15) . ? C26A C27A 1.359(14) . ? C26C C27C 1.376(15) . ? C27A C28A 1.391(13) . ? C27B C28B 1.372(14) . ? C27C C28C 1.381(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2A Nd1 N1A 159.9(2) . . ? N2A Nd1 I1 80.28(17) . . ? N1A Nd1 I1 80.02(17) . . ? N2B Nd2 N1B 162.1(2) . . ? N2B Nd2 I2 81.79(17) . . ? N1B Nd2 I2 80.39(17) . . ? N2C Nd3 N1C 162.9(2) . . ? N2C Nd3 I3 81.92(17) . . ? N1C Nd3 I3 81.44(16) . . ? C19A N1A C23A 115.0(9) . . ? C19A N1A Nd1 127.9(7) . . ? C23A N1A Nd1 116.5(6) . . ? C24A N2A C28A 116.1(9) . . ? C24A N2A Nd1 127.8(7) . . ? C28A N2A Nd1 116.1(6) . . ? C23B N1B C19B 115.2(9) . . ? C23B N1B Nd2 116.8(6) . . ? C19B N1B Nd2 128.0(7) . . ? C24B N2B C28B 115.8(8) . . ? C24B N2B Nd2 117.7(6) . . ? C28B N2B Nd2 126.2(6) . . ? C19C N1C C23C 116.3(9) . . ? C19C N1C Nd3 126.7(6) . . ? C23C N1C Nd3 116.3(6) . . ? C28C N2C C24C 116.0(8) . . ? C28C N2C Nd3 117.7(6) . . ? C24C N2C Nd3 126.3(6) . . ? C2B C1B C5B 105.4(9) . . ? C2B C1B C6B 126.5(9) . . ? C5B C1B C6B 126.7(9) . . ? C2A C1A C5A 105.8(9) . . ? C2A C1A C6A 126.4(9) . . ? C5A C1A C6A 127.0(9) . . ? C2C C1C C5C 105.9(9) . . ? C2C C1C C6C 127.2(9) . . ? C5C C1C C6C 125.6(9) . . ? C3C C2C C1C 109.2(9) . . ? C3B C2B C1B 109.4(9) . . ? C3A C2A C1A 109.0(10) . . ? C2B C3B C4B 108.6(9) . . ? C2A C3A C4A 108.5(9) . . ? C4C C3C C2C 107.8(9) . . ? C3C C4C C5C 108.5(10) . . ? C5B C4B C3B 105.8(9) . . ? C5A C4A C3A 107.3(9) . . ? C4C C5C C1C 108.7(9) . . ? C4B C5B C1B 110.8(9) . . ? C4A C5A C1A 109.3(9) . . ? C1B C6B C7B 108.4(8) . . ? C1B C6B C8B 110.3(8) . . ? C7B C6B C8B 110.7(9) . . ? C1B C6B C9B 110.3(8) . . ? C7B C6B C9B 108.3(8) . . ? C8B C6B C9B 108.8(8) . . ? C1A C6A C8A 112.2(8) . . ? C1A C6A C9A 111.4(8) . . ? C8A C6A C9A 109.6(8) . . ? C1A C6A C7A 106.3(8) . . ? C8A C6A C7A 108.7(9) . . ? C9A C6A C7A 108.5(9) . . ? C7C C6C C1C 111.8(9) . . ? C7C C6C C9C 110.1(9) . . ? C1C C6C C9C 107.1(8) . . ? C7C C6C C8C 109.1(9) . . ? C1C C6C C8C 110.1(9) . . ? C9C C6C C8C 108.5(9) . . ? C11C C10C C14C 106.0(9) . . ? C11C C10C C15C 127.3(9) . . ? C14C C10C C15C 125.8(9) . . ? C14A C10A C11A 106.0(9) . . ? C14A C10A C15A 126.1(9) . . ? C11A C10A C15A 127.0(9) . . ? C11B C10B C14B 105.2(9) . . ? C11B C10B C15B 125.9(9) . . ? C14B C10B C15B 127.7(9) . . ? C12A C11A C10A 109.8(9) . . ? C10B C11B C12B 110.8(9) . . ? C12C C11C C10C 110.1(9) . . ? C13A C12A C11A 107.6(9) . . ? C11B C12B C13B 105.4(10) . . ? C13C C12C C11C 107.2(10) . . ? C12A C13A C14A 108.2(9) . . ? C14B C13B C12B 108.6(9) . . ? C12C C13C C14C 108.5(9) . . ? C13C C14C C10C 108.2(9) . . ? C10A C14A C13A 108.4(9) . . ? C13B C14B C10B 110.0(9) . . ? C16B C15B C10B 112.0(8) . . ? C16B C15B C18B 108.8(9) . . ? C10B C15B C18B 106.9(8) . . ? C16B C15B C17B 109.9(9) . . ? C10B C15B C17B 110.1(8) . . ? C18B C15B C17B 109.1(8) . . ? C10C C15C C16C 111.4(8) . . ? C10C C15C C17C 111.5(8) . . ? C16C C15C C17C 108.3(8) . . ? C10C C15C C18C 107.8(8) . . ? C16C C15C C18C 109.1(9) . . ? C17C C15C C18C 108.7(9) . . ? C17A C15A C10A 111.7(9) . . ? C17A C15A C18A 109.8(9) . . ? C10A C15A C18A 110.8(8) . . ? C17A C15A C16A 108.7(9) . . ? C10A C15A C16A 106.8(8) . . ? C18A C15A C16A 108.8(8) . . ? N1C C19C C20C 123.2(10) . . ? N1A C19A C20A 124.0(10) . . ? N1B C19B C20B 123.9(10) . . ? C21C C20C C19C 118.5(10) . . ? C21A C20A C19A 118.9(10) . . ? C21B C20B C19B 119.1(10) . . ? C20B C21B C22B 117.9(10) . . ? C20A C21A C22A 119.0(10) . . ? C22C C21C C20C 120.3(10) . . ? C21A C22A C23A 118.3(10) . . ? C23B C22B C21B 118.5(10) . . ? C21C C22C C23C 118.0(10) . . ? N1C C23C C22C 123.7(9) . . ? N1A C23A C22A 124.6(10) . . ? N1B C23B C22B 125.4(10) . . ? N2C C24C C25C 123.9(10) . . ? N2A C24A C25A 123.9(10) . . ? C25B C24B N2B 123.9(10) . . ? C24A C25A C26A 119.3(10) . . ? C24B C25B C26B 119.7(10) . . ? C24C C25C C26C 118.4(10) . . ? C27B C26B C25B 117.7(10) . . ? C27A C26A C25A 118.2(10) . . ? C27C C26C C25C 119.3(10) . . ? C26A C27A C28A 119.0(10) . . ? C26B C27B C28B 119.9(10) . . ? C26C C27C C28C 117.9(10) . . ? N2B C28B C27B 122.9(10) . . ? N2A C28A C27A 123.5(9) . . ? N2C C28C C27C 124.5(10) . . ? #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 258866' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 Ce I2 N3' _chemical_formula_weight 752.41 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4213(4) _cell_length_b 8.8376(7) _cell_length_c 19.0845(15) _cell_angle_alpha 102.444(4) _cell_angle_beta 93.809(5) _cell_angle_gamma 108.371(4) _cell_volume 1302.39(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9001 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent dark yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method ? _exptl_crystal_F_000 714 _exptl_absorpt_coefficient_mu 4.133 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.374 _exptl_absorpt_correction_T_max 0.661 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(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_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 9001 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4559 _reflns_number_gt 3820 _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 subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) 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^)+1.5087P] 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 4559 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.605 _refine_diff_density_min -0.756 _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 0.52270(4) 0.25973(4) 0.261703(18) 0.03434(10) Uani 1 1 d . . . I1 I 0.77288(5) 0.14127(5) 0.16520(2) 0.04062(12) Uani 1 1 d . . . I2 I 0.32973(5) 0.29904(5) 0.40025(2) 0.04566(12) Uani 1 1 d . . . N1 N 0.2839(6) -0.0330(6) 0.2221(3) 0.0386(11) Uani 1 1 d . . . N2 N 0.6316(6) 0.0798(6) 0.3416(3) 0.0409(11) Uani 1 1 d . . . N3 N 0.8029(6) 0.4729(6) 0.3432(3) 0.0395(11) Uani 1 1 d . . . C1 C 0.3953(7) 0.3449(7) 0.1370(3) 0.0364(12) Uani 1 1 d . . . C2 C 0.2890(8) 0.3575(8) 0.1910(3) 0.0415(13) Uani 1 1 d . . . H2 H 0.1781 0.2883 0.1875 0.050 Uiso 1 1 calc R . . C3 C 0.3749(8) 0.4881(8) 0.2499(3) 0.0422(14) Uani 1 1 d . . . H3 H 0.3303 0.5209 0.2914 0.051 Uiso 1 1 calc R . . C4 C 0.5442(7) 0.5649(7) 0.2364(3) 0.0360(12) Uani 1 1 d . . . H4 H 0.6285 0.6560 0.2662 0.043 Uiso 1 1 calc R . . C5 C 0.5536(7) 0.4696(7) 0.1668(3) 0.0390(13) Uani 1 1 d . . . H5 H 0.6501 0.4869 0.1442 0.047 Uiso 1 1 calc R . . C6 C 0.3454(8) 0.2348(8) 0.0603(3) 0.0427(14) Uani 1 1 d . . . C7 C 0.2774(9) 0.0507(7) 0.0590(4) 0.0469(15) Uani 1 1 d . . . H7A H 0.3651 0.0206 0.0809 0.070 Uiso 1 1 calc R . . H7B H 0.2413 -0.0134 0.0097 0.070 Uiso 1 1 calc R . . H7C H 0.1832 0.0302 0.0856 0.070 Uiso 1 1 calc R . . C8 C 0.2028(8) 0.2751(8) 0.0213(4) 0.0482(15) Uani 1 1 d . . . H8A H 0.1102 0.2622 0.0489 0.072 Uiso 1 1 calc R . . H8B H 0.1647 0.2015 -0.0261 0.072 Uiso 1 1 calc R . . H8C H 0.2449 0.3866 0.0170 0.072 Uiso 1 1 calc R . . C9 C 0.4941(8) 0.2642(8) 0.0161(3) 0.0463(15) Uani 1 1 d . . . H9A H 0.5384 0.3788 0.0167 0.069 Uiso 1 1 calc R . . H9B H 0.4552 0.2000 -0.0331 0.069 Uiso 1 1 calc R . . H9C H 0.5813 0.2320 0.0371 0.069 Uiso 1 1 calc R . . C10 C 0.1173(8) -0.0549(8) 0.2171(3) 0.0413(13) Uani 1 1 d . . . H10 H 0.0839 0.0321 0.2396 0.050 Uiso 1 1 calc R . . C11 C -0.0059(8) -0.2008(7) 0.1801(3) 0.0423(14) Uani 1 1 d . . . H11 H -0.1198 -0.2124 0.1786 0.051 Uiso 1 1 calc R . . C12 C 0.0429(8) -0.3284(8) 0.1456(4) 0.0449(14) Uani 1 1 d . . . H12 H -0.0382 -0.4268 0.1195 0.054 Uiso 1 1 calc R . . C13 C 0.2131(8) -0.3107(8) 0.1497(4) 0.0450(14) Uani 1 1 d . . . H13 H 0.2486 -0.3961 0.1272 0.054 Uiso 1 1 calc R . . C14 C 0.3285(8) -0.1602(7) 0.1889(3) 0.0406(13) Uani 1 1 d . . . H14 H 0.4430 -0.1470 0.1922 0.049 Uiso 1 1 calc R . . C15 C 0.5244(8) -0.0237(8) 0.3732(3) 0.0423(14) Uani 1 1 d . . . H15 H 0.4112 -0.0321 0.3671 0.051 Uiso 1 1 calc R . . C16 C 0.5695(8) -0.1178(8) 0.4138(3) 0.0436(14) Uani 1 1 d . . . H16 H 0.4894 -0.1888 0.4338 0.052 Uiso 1 1 calc R . . C17 C 0.7395(8) -0.1038(7) 0.4243(4) 0.0439(14) Uani 1 1 d . . . H17 H 0.7752 -0.1652 0.4517 0.053 Uiso 1 1 calc R . . C18 C 0.8545(8) 0.0029(8) 0.3931(4) 0.0436(14) Uani 1 1 d . . . H18 H 0.9685 0.0144 0.3988 0.052 Uiso 1 1 calc R . . C19 C 0.7941(8) 0.0921(7) 0.3530(3) 0.0415(13) Uani 1 1 d . . . H19 H 0.8715 0.1651 0.3328 0.050 Uiso 1 1 calc R . . C20 C 0.8219(8) 0.5172(8) 0.4163(3) 0.0415(13) Uani 1 1 d . . . H20 H 0.7347 0.4665 0.4398 0.050 Uiso 1 1 calc R . . C21 C 0.9684(8) 0.6370(8) 0.4577(3) 0.0438(14) Uani 1 1 d . . . H21 H 0.9796 0.6632 0.5081 0.053 Uiso 1 1 calc R . . C22 C 1.0949(8) 0.7150(8) 0.4234(4) 0.0476(15) Uani 1 1 d . . . H22 H 1.1926 0.7960 0.4500 0.057 Uiso 1 1 calc R . . C23 C 1.0757(8) 0.6716(7) 0.3478(4) 0.0452(15) Uani 1 1 d . . . H23 H 1.1599 0.7228 0.3230 0.054 Uiso 1 1 calc R . . C24 C 0.9284(8) 0.5507(8) 0.3107(4) 0.0443(14) Uani 1 1 d . . . H24 H 0.9157 0.5217 0.2603 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.03488(19) 0.03254(17) 0.03531(19) 0.00917(13) 0.00397(12) 0.01075(13) I1 0.0395(2) 0.0440(2) 0.0386(2) 0.00756(16) 0.00523(15) 0.01646(17) I2 0.0458(2) 0.0488(2) 0.0425(2) 0.01133(18) 0.01269(17) 0.01496(18) N1 0.043(3) 0.037(2) 0.039(3) 0.014(2) 0.005(2) 0.015(2) N2 0.042(3) 0.040(3) 0.040(3) 0.011(2) 0.005(2) 0.012(2) N3 0.042(3) 0.034(2) 0.043(3) 0.012(2) 0.005(2) 0.013(2) C1 0.041(3) 0.029(3) 0.041(3) 0.015(2) -0.001(2) 0.011(2) C2 0.047(4) 0.041(3) 0.045(4) 0.020(3) 0.009(3) 0.019(3) C3 0.051(4) 0.045(3) 0.035(3) 0.010(3) 0.008(3) 0.022(3) C4 0.034(3) 0.040(3) 0.037(3) 0.011(2) 0.001(2) 0.016(2) C5 0.038(3) 0.034(3) 0.043(3) 0.011(3) 0.003(2) 0.009(2) C6 0.048(4) 0.044(3) 0.034(3) 0.010(3) 0.004(2) 0.012(3) C7 0.056(4) 0.038(3) 0.039(3) 0.007(3) 0.006(3) 0.007(3) C8 0.055(4) 0.050(4) 0.042(4) 0.015(3) 0.000(3) 0.020(3) C9 0.057(4) 0.045(3) 0.036(3) 0.014(3) 0.009(3) 0.012(3) C10 0.041(4) 0.041(3) 0.043(3) 0.013(3) 0.008(2) 0.013(3) C11 0.040(3) 0.044(3) 0.043(4) 0.015(3) 0.004(3) 0.012(3) C12 0.049(4) 0.036(3) 0.044(4) 0.010(3) -0.003(3) 0.008(3) C13 0.050(4) 0.039(3) 0.049(4) 0.019(3) 0.006(3) 0.015(3) C14 0.044(3) 0.039(3) 0.042(3) 0.013(3) 0.004(2) 0.017(3) C15 0.041(4) 0.043(3) 0.044(4) 0.014(3) 0.008(3) 0.013(3) C16 0.049(4) 0.045(3) 0.042(4) 0.015(3) 0.010(3) 0.019(3) C17 0.054(4) 0.039(3) 0.043(4) 0.012(3) 0.002(3) 0.023(3) C18 0.038(3) 0.043(3) 0.049(4) 0.006(3) 0.004(3) 0.017(3) C19 0.040(3) 0.036(3) 0.046(4) 0.008(3) 0.003(2) 0.011(3) C20 0.041(3) 0.045(3) 0.040(3) 0.010(3) 0.005(2) 0.018(3) C21 0.046(4) 0.045(3) 0.034(3) 0.001(3) -0.003(3) 0.015(3) C22 0.038(4) 0.048(3) 0.051(4) 0.001(3) -0.001(3) 0.015(3) C23 0.041(4) 0.036(3) 0.056(4) 0.009(3) 0.011(3) 0.011(3) C24 0.045(4) 0.050(4) 0.040(3) 0.016(3) 0.008(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce N3 2.643(5) . ? Ce N1 2.643(5) . ? Ce C3 2.723(6) . ? Ce N2 2.733(5) . ? Ce C2 2.767(6) . ? Ce C4 2.794(6) . ? Ce C5 2.827(6) . ? Ce C1 2.884(6) . ? Ce I1 3.1625(5) . ? Ce I2 3.2069(5) . ? N1 C14 1.340(8) . ? N1 C10 1.348(8) . ? N2 C19 1.337(8) . ? N2 C15 1.345(8) . ? N3 C24 1.337(8) . ? N3 C20 1.349(8) . ? C1 C2 1.418(9) . ? C1 C5 1.421(8) . ? C1 C6 1.521(8) . ? C2 C3 1.387(9) . ? C3 C4 1.439(8) . ? C4 C5 1.433(8) . ? C6 C7 1.539(8) . ? C6 C9 1.542(9) . ? C6 C8 1.545(9) . ? C10 C11 1.380(8) . ? C11 C12 1.372(9) . ? C12 C13 1.387(9) . ? C13 C14 1.390(9) . ? C15 C16 1.368(9) . ? C16 C17 1.394(9) . ? C17 C18 1.388(9) . ? C18 C19 1.388(9) . ? C20 C21 1.398(8) . ? C21 C22 1.365(9) . ? C22 C23 1.395(9) . ? C23 C24 1.379(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ce N1 152.18(15) . . ? N3 Ce N2 75.91(15) . . ? N1 Ce N2 76.42(15) . . ? N3 Ce I1 84.29(11) . . ? N1 Ce I1 92.87(11) . . ? N2 Ce I1 78.25(11) . . ? N3 Ce I2 88.62(11) . . ? N1 Ce I2 82.77(11) . . ? N2 Ce I2 77.69(11) . . ? I1 Ce I2 155.911(16) . . ? C14 N1 C10 117.3(5) . . ? C14 N1 Ce 117.3(4) . . ? C10 N1 Ce 123.4(4) . . ? C19 N2 C15 116.1(5) . . ? C19 N2 Ce 122.3(4) . . ? C15 N2 Ce 121.6(4) . . ? C24 N3 C20 117.7(5) . . ? C24 N3 Ce 118.7(4) . . ? C20 N3 Ce 123.5(4) . . ? C2 C1 C5 105.5(5) . . ? C2 C1 C6 127.3(5) . . ? C5 C1 C6 126.9(5) . . ? C3 C2 C1 110.0(6) . . ? C2 C3 C4 109.3(5) . . ? C5 C4 C3 104.6(5) . . ? C1 C5 C4 110.6(5) . . ? C1 C6 C7 112.5(5) . . ? C1 C6 C9 112.0(5) . . ? C7 C6 C9 108.5(5) . . ? C1 C6 C8 108.5(5) . . ? C7 C6 C8 107.5(5) . . ? C9 C6 C8 107.7(5) . . ? N1 C10 C11 122.9(6) . . ? C12 C11 C10 118.7(6) . . ? C11 C12 C13 120.0(6) . . ? C12 C13 C14 117.4(6) . . ? N1 C14 C13 123.6(6) . . ? N2 C15 C16 124.8(6) . . ? C15 C16 C17 117.9(6) . . ? C18 C17 C16 119.1(6) . . ? C17 C18 C19 118.0(6) . . ? N2 C19 C18 124.2(6) . . ? N3 C20 C21 122.1(6) . . ? C22 C21 C20 119.2(6) . . ? C21 C22 C23 119.2(6) . . ? C24 C23 C22 118.2(6) . . ? N3 C24 C23 123.6(6) . . ? #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 258867' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H52 Ce2 I2' _chemical_formula_weight 1018.82 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' 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 tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 14.8670(3) _cell_length_b 14.8670(3) _cell_length_c 33.9336(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7500.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 45357 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method ? _exptl_crystal_F_000 3920 _exptl_absorpt_coefficient_mu 4.065 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.296 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(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_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 45357 _diffrn_reflns_av_R_equivalents 0.0958 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7072 _reflns_number_gt 5721 _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 subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. The value of the Flack parameter indicates racemic twinning. 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^)+(0.0072P)^2^+26.6972P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(4) _refine_ls_number_reflns 7072 _refine_ls_number_parameters 376 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.703 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.103 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 0.51709(3) 0.74059(3) 0.000122(14) 0.02769(10) Uani 1 1 d . . . Ce2 Ce 0.22573(3) 0.22573(3) 0.0000 0.02961(14) Uani 1 2 d S . . Ce3 Ce 0.00354(3) 0.00354(3) 0.0000 0.02744(12) Uani 1 2 d S . . I1 I 0.52541(3) 0.52541(3) 0.0000 0.03893(18) Uani 1 2 d S . . I2 I 0.73341(3) 0.73341(3) 0.0000 0.03243(16) Uani 1 2 d S . . I3 I 0.21950(3) 0.00961(3) 0.004064(17) 0.03641(13) Uani 1 1 d . . . C1 C 0.4058(6) 0.7419(6) 0.0672(2) 0.0284(19) Uani 1 1 d . . . C2 C 0.4189(7) 0.8324(7) 0.0556(3) 0.037(2) Uani 1 1 d . . . H2 H 0.3752 0.8700 0.0450 0.044 Uiso 1 1 calc R . . C3 C 0.5094(7) 0.8560(7) 0.0629(3) 0.039(2) Uani 1 1 d . . . H3 H 0.5350 0.9120 0.0581 0.047 Uiso 1 1 calc R . . C4 C 0.5534(6) 0.7822(7) 0.0783(3) 0.039(2) Uani 1 1 d . . . H4 H 0.6135 0.7801 0.0857 0.047 Uiso 1 1 calc R . . C5 C 0.4908(6) 0.7101(6) 0.0808(2) 0.034(2) Uani 1 1 d . . . H5 H 0.5032 0.6522 0.0897 0.041 Uiso 1 1 calc R . . C6 C 0.3173(7) 0.6904(7) 0.0684(3) 0.043(2) Uani 1 1 d . . . C7 C 0.3328(8) 0.5929(8) 0.0797(4) 0.071(4) Uani 1 1 d . . . H7A H 0.2769 0.5608 0.0785 0.107 Uiso 1 1 calc R . . H7B H 0.3564 0.5900 0.1060 0.107 Uiso 1 1 calc R . . H7C H 0.3750 0.5662 0.0617 0.107 Uiso 1 1 calc R . . C8 C 0.2726(8) 0.6961(9) 0.0278(3) 0.075(4) Uani 1 1 d . . . H8A H 0.2137 0.6697 0.0291 0.112 Uiso 1 1 calc R . . H8B H 0.3084 0.6642 0.0089 0.112 Uiso 1 1 calc R . . H8C H 0.2676 0.7580 0.0200 0.112 Uiso 1 1 calc R . . C9 C 0.2571(7) 0.7329(9) 0.0997(4) 0.073(4) Uani 1 1 d . . . H9A H 0.2437 0.7938 0.0925 0.110 Uiso 1 1 calc R . . H9B H 0.2875 0.7322 0.1247 0.110 Uiso 1 1 calc R . . H9C H 0.2021 0.6993 0.1017 0.110 Uiso 1 1 calc R . . C10 C 0.5058(6) 0.8586(6) -0.0647(2) 0.0301(19) Uani 1 1 d . . . C11 C 0.5444(7) 0.7778(7) -0.0795(2) 0.040(2) Uani 1 1 d . . . H11 H 0.6032 0.7706 -0.0883 0.049 Uiso 1 1 calc R . . C12 C 0.4782(7) 0.7110(7) -0.0783(3) 0.044(2) Uani 1 1 d . . . H12 H 0.4856 0.6521 -0.0870 0.053 Uiso 1 1 calc R . . C13 C 0.4001(7) 0.7459(8) -0.0623(3) 0.048(3) Uani 1 1 d . . . H13 H 0.3467 0.7148 -0.0582 0.057 Uiso 1 1 calc R . . C14 C 0.4165(6) 0.8375(7) -0.0535(3) 0.035(2) Uani 1 1 d . . . H14 H 0.3756 0.8772 -0.0422 0.042 Uiso 1 1 calc R . . C15 C 0.5502(6) 0.9505(6) -0.0646(2) 0.0314(19) Uani 1 1 d . . . C16 C 0.6481(6) 0.9474(7) -0.0762(3) 0.048(3) Uani 1 1 d . . . H16A H 0.6720 1.0074 -0.0766 0.072 Uiso 1 1 calc R . . H16B H 0.6538 0.9210 -0.1019 0.072 Uiso 1 1 calc R . . H16C H 0.6808 0.9119 -0.0574 0.072 Uiso 1 1 calc R . . C17 C 0.4995(6) 1.0122(7) -0.0946(3) 0.045(2) Uani 1 1 d . . . H17A H 0.5264 1.0709 -0.0946 0.067 Uiso 1 1 calc R . . H17B H 0.4375 1.0170 -0.0870 0.067 Uiso 1 1 calc R . . H17C H 0.5035 0.9866 -0.1205 0.067 Uiso 1 1 calc R . . C18 C 0.5412(8) 0.9932(7) -0.0247(3) 0.057(3) Uani 1 1 d . . . H18A H 0.5697 0.9558 -0.0053 0.085 Uiso 1 1 calc R . . H18B H 0.4786 0.9999 -0.0183 0.085 Uiso 1 1 calc R . . H18C H 0.5695 1.0513 -0.0249 0.085 Uiso 1 1 calc R . . C19 C 0.2526(6) 0.3385(6) -0.0648(3) 0.034(2) Uani 1 1 d . . . C20 C 0.3387(6) 0.3116(6) -0.0520(3) 0.037(2) Uani 1 1 d . . . H20 H 0.3813 0.3493 -0.0405 0.045 Uiso 1 1 calc R . . C21 C 0.3505(7) 0.2197(7) -0.0590(3) 0.044(2) Uani 1 1 d . . . H21 H 0.4012 0.1857 -0.0529 0.053 Uiso 1 1 calc R . . C22 C 0.2716(8) 0.1886(7) -0.0769(3) 0.047(3) Uani 1 1 d . . . H22 H 0.2612 0.1298 -0.0850 0.057 Uiso 1 1 calc R . . C23 C 0.2112(7) 0.2599(7) -0.0806(3) 0.041(2) Uani 1 1 d . . . H23 H 0.1538 0.2567 -0.0915 0.049 Uiso 1 1 calc R . . C24 C 0.2139(7) 0.4336(6) -0.0665(3) 0.037(2) Uani 1 1 d . . . C25 C 0.1131(7) 0.4331(8) -0.0573(4) 0.059(3) Uani 1 1 d . . . H25A H 0.1036 0.4091 -0.0314 0.089 Uiso 1 1 calc R . . H25B H 0.0823 0.3965 -0.0763 0.089 Uiso 1 1 calc R . . H25C H 0.0903 0.4934 -0.0584 0.089 Uiso 1 1 calc R . . C26 C 0.2274(8) 0.4697(7) -0.1089(3) 0.061(3) Uani 1 1 d U . . H26A H 0.2012 0.5285 -0.1111 0.091 Uiso 1 1 calc R . . H26B H 0.1988 0.4298 -0.1273 0.091 Uiso 1 1 calc R . . H26C H 0.2906 0.4731 -0.1147 0.091 Uiso 1 1 calc R . . C27 C 0.2608(8) 0.4963(7) -0.0376(3) 0.069(3) Uani 1 1 d U . . H27A H 0.2467 0.4783 -0.0111 0.104 Uiso 1 1 calc R . . H27B H 0.2405 0.5568 -0.0418 0.104 Uiso 1 1 calc R . . H27C H 0.3246 0.4932 -0.0415 0.104 Uiso 1 1 calc R . . C28 C 0.0070(6) -0.1159(6) -0.0639(3) 0.031(2) Uani 1 1 d . . . C29 C 0.0484(7) -0.0354(6) -0.0783(3) 0.038(2) Uani 1 1 d . . . H29 H 0.1088 -0.0286 -0.0848 0.045 Uiso 1 1 calc R . . C30 C -0.0192(7) 0.0330(7) -0.0810(2) 0.042(2) Uani 1 1 d . . . H30 H -0.0110 0.0916 -0.0898 0.050 Uiso 1 1 calc R . . C31 C -0.1011(7) -0.0056(7) -0.0676(3) 0.037(2) Uani 1 1 d . . . H31 H -0.1562 0.0238 -0.0663 0.045 Uiso 1 1 calc R . . C32 C -0.0854(6) -0.0955(6) -0.0565(2) 0.0328(18) Uani 1 1 d . . . H32 H -0.1279 -0.1349 -0.0461 0.039 Uiso 1 1 calc R . . C33 C 0.0509(6) -0.2073(6) -0.0586(2) 0.0326(19) Uani 1 1 d . . . C34 C 0.0569(7) -0.2308(7) -0.0153(3) 0.048(2) Uani 1 1 d . . . H34A H -0.0026 -0.2381 -0.0048 0.072 Uiso 1 1 calc R . . H34B H 0.0872 -0.1834 -0.0015 0.072 Uiso 1 1 calc R . . H34C H 0.0898 -0.2859 -0.0122 0.072 Uiso 1 1 calc R . . C35 C -0.0043(7) -0.2802(7) -0.0792(3) 0.060(3) Uani 1 1 d . . . H35A H 0.0234 -0.3377 -0.0750 0.091 Uiso 1 1 calc R . . H35B H -0.0069 -0.2678 -0.1069 0.091 Uiso 1 1 calc R . . H35C H -0.0641 -0.2808 -0.0685 0.091 Uiso 1 1 calc R . . C36 C 0.1468(7) -0.2075(7) -0.0763(3) 0.053(3) Uani 1 1 d . . . H36A H 0.1716 -0.2670 -0.0747 0.080 Uiso 1 1 calc R . . H36B H 0.1842 -0.1665 -0.0618 0.080 Uiso 1 1 calc R . . H36C H 0.1442 -0.1891 -0.1034 0.080 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 0.0280(2) 0.0306(2) 0.0245(2) -0.0030(2) -0.0007(2) 0.00119(16) Ce2 0.02865(19) 0.02865(19) 0.0315(3) -0.0042(2) 0.0042(2) -0.0015(2) Ce3 0.02883(17) 0.02883(17) 0.0247(3) 0.00059(19) -0.00059(19) -0.0017(2) I1 0.0318(2) 0.0318(2) 0.0531(5) -0.0050(3) 0.0050(3) -0.0016(3) I2 0.0290(2) 0.0290(2) 0.0393(4) -0.0005(3) 0.0005(3) -0.0009(3) I3 0.0286(2) 0.0297(2) 0.0509(3) -0.0028(3) -0.0017(3) 0.0004(2) C1 0.037(5) 0.036(5) 0.013(4) -0.003(4) -0.006(3) -0.001(4) C2 0.046(6) 0.038(6) 0.027(5) -0.008(4) 0.006(4) 0.006(4) C3 0.042(5) 0.042(6) 0.034(5) -0.011(4) 0.005(4) -0.008(5) C4 0.033(5) 0.049(6) 0.036(5) -0.013(4) 0.001(4) -0.010(5) C5 0.040(5) 0.042(5) 0.021(4) 0.001(4) -0.002(4) 0.004(4) C6 0.044(6) 0.046(6) 0.038(5) -0.006(4) -0.001(4) -0.006(4) C7 0.079(9) 0.068(8) 0.067(8) -0.010(6) 0.036(7) -0.030(6) C8 0.067(7) 0.114(10) 0.044(6) 0.006(6) -0.023(6) -0.047(7) C9 0.045(6) 0.084(9) 0.091(9) -0.044(7) 0.021(6) -0.023(6) C10 0.031(5) 0.038(5) 0.021(4) -0.001(4) -0.004(4) 0.000(4) C11 0.049(6) 0.057(7) 0.016(4) -0.007(4) -0.001(4) 0.016(5) C12 0.065(7) 0.040(5) 0.027(4) -0.015(4) -0.005(4) 0.000(5) C13 0.041(5) 0.068(8) 0.034(6) 0.003(5) -0.008(4) -0.008(6) C14 0.031(5) 0.042(6) 0.032(5) 0.002(4) -0.006(4) 0.002(4) C15 0.044(5) 0.022(4) 0.027(5) 0.006(4) -0.006(4) -0.003(4) C16 0.033(5) 0.057(6) 0.054(7) 0.017(5) -0.001(5) -0.001(5) C17 0.037(5) 0.045(5) 0.052(6) 0.009(5) -0.001(4) 0.004(5) C18 0.082(8) 0.061(7) 0.027(5) -0.010(5) 0.010(5) -0.028(6) C19 0.037(5) 0.034(5) 0.030(5) 0.001(4) 0.006(4) 0.006(4) C20 0.039(5) 0.033(5) 0.039(5) 0.000(4) 0.012(4) -0.007(4) C21 0.036(5) 0.043(6) 0.054(7) 0.003(5) 0.016(5) 0.005(5) C22 0.074(8) 0.034(5) 0.033(5) -0.006(4) 0.018(5) 0.001(5) C23 0.046(5) 0.050(6) 0.026(5) -0.002(4) 0.005(4) -0.008(5) C24 0.039(5) 0.042(5) 0.031(5) 0.001(4) -0.001(4) 0.006(4) C25 0.051(7) 0.058(7) 0.070(8) 0.027(6) 0.017(6) 0.008(6) C26 0.074(6) 0.051(5) 0.058(5) 0.021(5) 0.028(5) 0.015(5) C27 0.079(6) 0.045(5) 0.085(6) -0.002(5) -0.032(5) 0.009(5) C28 0.036(5) 0.033(5) 0.025(5) -0.002(3) -0.004(4) -0.003(4) C29 0.047(6) 0.031(5) 0.035(5) 0.003(4) 0.002(4) -0.005(4) C30 0.060(7) 0.038(5) 0.027(4) 0.004(4) -0.003(4) 0.000(4) C31 0.044(5) 0.041(6) 0.026(5) 0.007(4) -0.009(4) 0.003(5) C32 0.038(5) 0.035(5) 0.025(4) 0.002(4) -0.008(4) -0.012(3) C33 0.042(5) 0.035(5) 0.021(4) -0.002(4) 0.001(4) -0.005(4) C34 0.056(6) 0.051(6) 0.036(5) 0.013(4) 0.002(4) 0.013(5) C35 0.063(7) 0.046(6) 0.072(7) -0.014(6) -0.033(6) -0.003(5) C36 0.054(6) 0.043(6) 0.063(7) -0.005(5) 0.014(5) 0.008(5) _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 C3 2.738(9) . ? Ce1 C13 2.743(10) . ? Ce1 C2 2.746(8) . ? Ce1 C12 2.760(8) . ? Ce1 C14 2.761(9) . ? Ce1 C4 2.776(9) . ? Ce1 C11 2.787(8) . ? Ce1 C5 2.802(8) . ? Ce1 C1 2.816(9) . ? Ce1 C10 2.820(9) . ? Ce1 I1 3.2014(7) . ? Ce1 I2 3.2178(6) . ? Ce1 Ce1 4.6990(8) 7 ? Ce2 C21 2.730(9) 7 ? Ce2 C21 2.730(9) . ? Ce2 C20 2.749(8) 7 ? Ce2 C20 2.749(8) . ? Ce2 C22 2.752(10) . ? Ce2 C22 2.752(10) 7 ? Ce2 C23 2.790(9) . ? Ce2 C23 2.790(9) 7 ? Ce2 C19 2.794(9) . ? Ce2 C19 2.794(9) 7 ? Ce2 I3 3.2173(7) 7 ? Ce2 I3 3.2174(7) . ? Ce2 Ce3 4.6716(9) . ? Ce3 C32 2.755(7) . ? Ce3 C32 2.755(7) 7 ? Ce3 C31 2.774(9) . ? Ce3 C31 2.774(9) 7 ? Ce3 C29 2.800(9) 7 ? Ce3 C29 2.800(9) . ? Ce3 C30 2.802(8) 7 ? Ce3 C30 2.802(8) . ? Ce3 C28 2.803(8) . ? Ce3 C28 2.803(8) 7 ? Ce3 I3 3.2148(7) 7 ? Ce3 I3 3.2149(7) . ? I1 Ce1 3.2014(7) 7 ? I2 Ce1 3.2178(6) 7 ? C1 C2 1.415(13) . ? C1 C5 1.426(12) . ? C1 C6 1.522(14) . ? C2 C3 1.412(14) . ? C3 C4 1.380(14) . ? C4 C5 1.423(13) . ? C6 C7 1.517(15) . ? C6 C9 1.527(12) . ? C6 C8 1.532(13) . ? C10 C14 1.417(13) . ? C10 C11 1.423(13) . ? C10 C15 1.517(12) . ? C11 C12 1.399(14) . ? C12 C13 1.382(14) . ? C13 C14 1.417(15) . ? C15 C18 1.503(12) . ? C15 C16 1.508(13) . ? C15 C17 1.563(12) . ? C19 C20 1.410(13) . ? C19 C23 1.424(13) . ? C19 C24 1.529(13) . ? C20 C21 1.397(13) . ? C21 C22 1.399(15) . ? C22 C23 1.396(14) . ? C24 C27 1.522(13) . ? C24 C25 1.530(13) . ? C24 C26 1.551(12) . ? C28 C32 1.429(13) . ? C28 C29 1.432(13) . ? C28 C33 1.518(12) . ? C29 C30 1.431(11) . ? C30 C31 1.421(14) . ? C31 C32 1.407(13) . ? C33 C34 1.513(11) . ? C33 C35 1.527(12) . ? C33 C36 1.547(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 Ce1 I2 85.886(15) . . ? I1 Ce1 Ce1 42.785(12) . 7 ? I2 Ce1 Ce1 43.100(11) . 7 ? I3 Ce2 I3 86.81(2) 7 . ? I3 Ce2 Ce3 43.403(11) 7 . ? I3 Ce2 Ce3 43.404(11) . . ? I3 Ce3 I3 86.89(2) 7 . ? I3 Ce3 Ce2 43.445(12) 7 . ? I3 Ce3 Ce2 43.446(12) . . ? Ce1 I1 Ce1 94.43(2) 7 . ? Ce1 I2 Ce1 93.80(2) 7 . ? Ce3 I3 Ce2 93.150(16) . . ? C2 C1 C5 106.4(8) . . ? C2 C1 C6 127.2(8) . . ? C5 C1 C6 126.2(8) . . ? C3 C2 C1 108.7(8) . . ? C4 C3 C2 108.6(9) . . ? C3 C4 C5 108.2(8) . . ? C4 C5 C1 108.1(8) . . ? C7 C6 C1 110.8(8) . . ? C7 C6 C9 107.9(9) . . ? C1 C6 C9 108.4(8) . . ? C7 C6 C8 110.3(9) . . ? C1 C6 C8 108.9(8) . . ? C9 C6 C8 110.4(9) . . ? C14 C10 C11 106.6(9) . . ? C14 C10 C15 127.3(8) . . ? C11 C10 C15 125.9(8) . . ? C12 C11 C10 107.8(9) . . ? C13 C12 C11 109.6(9) . . ? C12 C13 C14 107.4(9) . . ? C13 C14 C10 108.5(8) . . ? C18 C15 C16 109.5(8) . . ? C18 C15 C10 110.2(7) . . ? C16 C15 C10 113.0(8) . . ? C18 C15 C17 107.2(8) . . ? C16 C15 C17 108.3(7) . . ? C10 C15 C17 108.5(7) . . ? C20 C19 C23 106.1(8) . . ? C20 C19 C24 128.0(8) . . ? C23 C19 C24 125.6(9) . . ? C21 C20 C19 109.8(8) . . ? C20 C21 C22 107.0(9) . . ? C23 C22 C21 109.2(10) . . ? C22 C23 C19 108.0(9) . . ? C27 C24 C19 111.7(8) . . ? C27 C24 C25 108.7(9) . . ? C19 C24 C25 110.9(8) . . ? C27 C24 C26 109.1(8) . . ? C19 C24 C26 107.8(8) . . ? C25 C24 C26 108.6(8) . . ? C32 C28 C29 107.2(8) . . ? C32 C28 C33 125.6(8) . . ? C29 C28 C33 127.2(8) . . ? C30 C29 C28 108.3(10) . . ? C31 C30 C29 107.1(10) . . ? C32 C31 C30 109.1(8) . . ? C31 C32 C28 108.3(7) . . ? C34 C33 C28 110.3(7) . . ? C34 C33 C35 108.2(8) . . ? C28 C33 C35 110.5(8) . . ? C34 C33 C36 108.8(8) . . ? C28 C33 C36 110.6(7) . . ? C35 C33 C36 108.5(8) . . ? #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 258868' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 I2 La N3' _chemical_formula_weight 751.20 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' La La -0.2871 2.4523 '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 8.4495(4) _cell_length_b 8.8444(5) _cell_length_c 19.1107(10) _cell_angle_alpha 102.588(3) _cell_angle_beta 93.636(3) _cell_angle_gamma 108.458(3) _cell_volume 1308.53(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 29806 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.68 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_method ? _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 4.006 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.376 _exptl_absorpt_correction_T_max 0.755 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(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 area-detector diffractometer' _diffrn_measurement_method 'one \f and five \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 29806 _diffrn_reflns_av_R_equivalents 0.0913 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4967 _reflns_number_gt 4647 _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 subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) 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^)+(0.0143P)^2^+0.8513P] 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 4967 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.591 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.113 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 La La 0.52261(2) 0.25945(2) 0.261183(9) 0.03521(7) Uani 1 1 d . . . I1 I 0.77493(3) 0.14129(3) 0.164336(11) 0.04153(7) Uani 1 1 d . . . I2 I 0.32947(3) 0.29918(3) 0.400828(12) 0.04623(8) Uani 1 1 d . . . N1 N 0.2813(3) -0.0363(3) 0.22197(15) 0.0404(6) Uani 1 1 d . . . N2 N 0.6326(4) 0.0784(4) 0.34190(15) 0.0438(6) Uani 1 1 d . . . N3 N 0.8044(3) 0.4749(3) 0.34382(15) 0.0412(6) Uani 1 1 d . . . C1 C 0.3966(4) 0.3467(4) 0.13662(17) 0.0372(7) Uani 1 1 d . . . C2 C 0.2882(4) 0.3580(4) 0.18948(18) 0.0413(7) Uani 1 1 d . . . H2 H 0.1774 0.2887 0.1856 0.050 Uiso 1 1 calc R . . C3 C 0.3750(4) 0.4907(4) 0.24871(19) 0.0433(7) Uani 1 1 d . . . H3 H 0.3312 0.5259 0.2902 0.052 Uiso 1 1 calc R . . C4 C 0.5395(4) 0.5611(4) 0.23441(19) 0.0431(7) Uani 1 1 d . . . H4 H 0.6244 0.6507 0.2647 0.052 Uiso 1 1 calc R . . C5 C 0.5529(4) 0.4709(4) 0.16548(18) 0.0400(7) Uani 1 1 d . . . H5 H 0.6491 0.4905 0.1429 0.048 Uiso 1 1 calc R . . C6 C 0.3457(4) 0.2346(4) 0.05958(18) 0.0407(7) Uani 1 1 d . . . C7 C 0.2790(5) 0.0519(4) 0.05981(19) 0.0499(9) Uani 1 1 d . . . H7A H 0.3670 0.0233 0.0820 0.075 Uiso 1 1 calc R . . H7B H 0.2428 -0.0143 0.0109 0.075 Uiso 1 1 calc R . . H7C H 0.1856 0.0324 0.0867 0.075 Uiso 1 1 calc R . . C8 C 0.2009(5) 0.2748(5) 0.02126(19) 0.0484(8) Uani 1 1 d . . . H8A H 0.1091 0.2611 0.0492 0.073 Uiso 1 1 calc R . . H8B H 0.1624 0.2016 -0.0262 0.073 Uiso 1 1 calc R . . H8C H 0.2421 0.3865 0.0173 0.073 Uiso 1 1 calc R . . C9 C 0.4931(5) 0.2642(5) 0.01607(18) 0.0472(8) Uani 1 1 d . . . H9A H 0.5313 0.3770 0.0135 0.071 Uiso 1 1 calc R . . H9B H 0.4572 0.1933 -0.0320 0.071 Uiso 1 1 calc R . . H9C H 0.5836 0.2410 0.0394 0.071 Uiso 1 1 calc R . . C10 C 0.1164(4) -0.0562(4) 0.21710(18) 0.0403(7) Uani 1 1 d . . . H10 H 0.0841 0.0306 0.2406 0.048 Uiso 1 1 calc R . . C11 C -0.0075(4) -0.2008(4) 0.17858(19) 0.0445(8) Uani 1 1 d . . . H11 H -0.1208 -0.2108 0.1760 0.053 Uiso 1 1 calc R . . C12 C 0.0413(5) -0.3302(4) 0.1439(2) 0.0471(8) Uani 1 1 d . . . H12 H -0.0393 -0.4284 0.1174 0.056 Uiso 1 1 calc R . . C13 C 0.2110(5) -0.3123(4) 0.14902(19) 0.0461(8) Uani 1 1 d . . . H13 H 0.2464 -0.3980 0.1267 0.055 Uiso 1 1 calc R . . C14 C 0.3262(4) -0.1632(4) 0.18828(19) 0.0435(8) Uani 1 1 d . . . H14 H 0.4402 -0.1502 0.1915 0.052 Uiso 1 1 calc R . . C15 C 0.5239(4) -0.0249(4) 0.37321(18) 0.0426(7) Uani 1 1 d . . . H15 H 0.4111 -0.0333 0.3672 0.051 Uiso 1 1 calc R . . C16 C 0.5714(4) -0.1198(5) 0.41408(19) 0.0454(8) Uani 1 1 d . . . H16 H 0.4919 -0.1916 0.4339 0.055 Uiso 1 1 calc R . . C17 C 0.7397(5) -0.1047(5) 0.42457(19) 0.0468(8) Uani 1 1 d . . . H17 H 0.7760 -0.1645 0.4525 0.056 Uiso 1 1 calc R . . C18 C 0.8528(4) 0.0007(4) 0.39285(19) 0.0439(8) Uani 1 1 d . . . H18 H 0.9664 0.0118 0.3986 0.053 Uiso 1 1 calc R . . C19 C 0.7949(4) 0.0897(4) 0.35230(18) 0.0426(7) Uani 1 1 d . . . H19 H 0.8723 0.1606 0.3313 0.051 Uiso 1 1 calc R . . C20 C 0.8245(4) 0.5184(4) 0.41698(18) 0.0424(7) Uani 1 1 d . . . H20 H 0.7388 0.4661 0.4407 0.051 Uiso 1 1 calc R . . C21 C 0.9681(4) 0.6380(5) 0.45765(19) 0.0458(8) Uani 1 1 d . . . H21 H 0.9786 0.6652 0.5080 0.055 Uiso 1 1 calc R . . C22 C 1.0965(4) 0.7171(5) 0.4230(2) 0.0475(8) Uani 1 1 d . . . H22 H 1.1940 0.7982 0.4496 0.057 Uiso 1 1 calc R . . C23 C 1.0769(4) 0.6730(4) 0.3485(2) 0.0449(8) Uani 1 1 d . . . H23 H 1.1609 0.7240 0.3237 0.054 Uiso 1 1 calc R . . C24 C 0.9303(4) 0.5517(4) 0.31118(19) 0.0434(7) Uani 1 1 d . . . H24 H 0.9184 0.5218 0.2609 0.052 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 La 0.03396(11) 0.03586(11) 0.03549(11) 0.00983(8) 0.00464(8) 0.01090(8) I1 0.03839(12) 0.04733(14) 0.03905(13) 0.00835(10) 0.00543(9) 0.01648(10) I2 0.04521(13) 0.05210(15) 0.04127(13) 0.01202(10) 0.01248(10) 0.01495(10) N1 0.0400(14) 0.0383(15) 0.0424(15) 0.0137(12) 0.0047(12) 0.0103(12) N2 0.0429(15) 0.0452(16) 0.0423(15) 0.0125(13) 0.0028(12) 0.0133(13) N3 0.0421(15) 0.0393(15) 0.0413(15) 0.0120(12) 0.0042(12) 0.0118(12) C1 0.0414(17) 0.0355(16) 0.0367(16) 0.0141(13) 0.0047(13) 0.0126(13) C2 0.0398(17) 0.0451(19) 0.0412(18) 0.0148(15) 0.0050(14) 0.0149(14) C3 0.0503(19) 0.0430(18) 0.0429(18) 0.0120(15) 0.0065(15) 0.0237(16) C4 0.0473(18) 0.0377(17) 0.0438(18) 0.0108(14) 0.0023(15) 0.0142(15) C5 0.0398(17) 0.0379(17) 0.0424(18) 0.0119(14) 0.0054(14) 0.0123(14) C6 0.0425(17) 0.0414(18) 0.0374(17) 0.0105(14) 0.0055(14) 0.0127(14) C7 0.059(2) 0.043(2) 0.0410(19) 0.0095(15) 0.0017(16) 0.0098(17) C8 0.052(2) 0.051(2) 0.0414(19) 0.0114(16) -0.0003(15) 0.0169(17) C9 0.056(2) 0.049(2) 0.0367(18) 0.0112(15) 0.0082(15) 0.0174(17) C10 0.0427(17) 0.0404(18) 0.0416(17) 0.0149(14) 0.0061(14) 0.0161(14) C11 0.0394(17) 0.047(2) 0.0448(19) 0.0163(15) 0.0031(14) 0.0090(15) C12 0.0494(19) 0.0398(18) 0.0456(19) 0.0106(15) 0.0012(15) 0.0076(15) C13 0.056(2) 0.0377(18) 0.0464(19) 0.0128(15) 0.0080(16) 0.0170(16) C14 0.0434(18) 0.0440(19) 0.0469(19) 0.0179(15) 0.0061(15) 0.0158(15) C15 0.0378(17) 0.0438(19) 0.0463(19) 0.0148(15) 0.0065(14) 0.0113(14) C16 0.0469(19) 0.0447(19) 0.0466(19) 0.0179(15) 0.0090(15) 0.0134(16) C17 0.053(2) 0.046(2) 0.0457(19) 0.0138(15) 0.0037(16) 0.0217(16) C18 0.0395(17) 0.0454(19) 0.0456(19) 0.0084(15) 0.0013(14) 0.0158(15) C19 0.0424(18) 0.0452(19) 0.0398(17) 0.0102(14) 0.0062(14) 0.0145(15) C20 0.0404(17) 0.0477(19) 0.0404(18) 0.0123(15) 0.0051(14) 0.0161(15) C21 0.0421(18) 0.051(2) 0.0425(19) 0.0073(15) 0.0017(15) 0.0170(16) C22 0.0399(18) 0.0431(19) 0.054(2) 0.0014(16) 0.0011(15) 0.0143(15) C23 0.0404(17) 0.0394(18) 0.052(2) 0.0091(15) 0.0095(15) 0.0105(14) C24 0.0476(19) 0.0418(18) 0.0403(18) 0.0113(14) 0.0056(14) 0.0141(15) _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 La N3 2.671(3) . ? La N1 2.671(3) . ? La C3 2.755(3) . ? La N2 2.765(3) . ? La C4 2.786(3) . ? La C2 2.798(3) . ? La C5 2.856(3) . ? La C1 2.898(3) . ? La I1 3.1830(3) . ? La I2 3.2273(3) . ? N1 C10 1.342(4) . ? N1 C14 1.343(4) . ? N2 C19 1.342(4) . ? N2 C15 1.346(4) . ? N3 C24 1.339(4) . ? N3 C20 1.351(4) . ? C1 C5 1.407(4) . ? C1 C2 1.414(5) . ? C1 C6 1.533(5) . ? C2 C3 1.403(5) . ? C3 C4 1.404(5) . ? C4 C5 1.415(5) . ? C6 C9 1.527(5) . ? C6 C7 1.535(5) . ? C6 C8 1.560(5) . ? C10 C11 1.385(5) . ? C11 C12 1.386(5) . ? C12 C13 1.387(5) . ? C13 C14 1.383(5) . ? C15 C16 1.391(5) . ? C16 C17 1.383(5) . ? C17 C18 1.381(5) . ? C18 C19 1.386(5) . ? C20 C21 1.380(5) . ? C21 C22 1.384(5) . ? C22 C23 1.377(5) . ? C23 C24 1.381(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 La N1 151.88(8) . . ? N3 La N2 75.67(8) . . ? N1 La N2 76.41(8) . . ? N3 La I1 84.21(6) . . ? N1 La I1 93.37(6) . . ? N2 La I1 78.24(6) . . ? N3 La I2 88.34(6) . . ? N1 La I2 82.47(6) . . ? N2 La I2 77.56(6) . . ? I1 La I2 155.748(9) . . ? C10 N1 C14 118.0(3) . . ? C10 N1 La 122.8(2) . . ? C14 N1 La 116.8(2) . . ? C19 N2 C15 117.0(3) . . ? C19 N2 La 122.2(2) . . ? C15 N2 La 120.8(2) . . ? C24 N3 C20 117.6(3) . . ? C24 N3 La 118.4(2) . . ? C20 N3 La 123.9(2) . . ? C5 C1 C2 106.7(3) . . ? C5 C1 C6 126.9(3) . . ? C2 C1 C6 126.0(3) . . ? C3 C2 C1 108.9(3) . . ? C2 C3 C4 108.0(3) . . ? C3 C4 C5 107.5(3) . . ? C1 C5 C4 108.8(3) . . ? C9 C6 C1 111.4(3) . . ? C9 C6 C7 109.1(3) . . ? C1 C6 C7 111.7(3) . . ? C9 C6 C8 108.6(3) . . ? C1 C6 C8 108.0(3) . . ? C7 C6 C8 107.9(3) . . ? N1 C10 C11 122.7(3) . . ? C10 C11 C12 118.4(3) . . ? C13 C12 C11 119.6(3) . . ? C14 C13 C12 118.0(3) . . ? N1 C14 C13 123.2(3) . . ? N2 C15 C16 123.5(3) . . ? C17 C16 C15 118.4(3) . . ? C18 C17 C16 118.9(3) . . ? C17 C18 C19 119.1(3) . . ? N2 C19 C18 123.1(3) . . ? N3 C20 C21 122.1(3) . . ? C20 C21 C22 119.5(3) . . ? C23 C22 C21 118.6(3) . . ? C22 C23 C24 118.8(3) . . ? N3 C24 C23 123.3(3) . . ? #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 258869' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 I2 N3 U' _chemical_formula_weight 850.32 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 8.4321(13) _cell_length_b 8.8209(14) _cell_length_c 19.053(3) _cell_angle_alpha 102.423(9) _cell_angle_beta 93.827(8) _cell_angle_gamma 108.547(9) _cell_volume 1298.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8656 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.68 _exptl_crystal_description needle _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.176 _exptl_crystal_density_method ? _exptl_crystal_F_000 782 _exptl_absorpt_coefficient_mu 8.646 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.362 _exptl_absorpt_correction_T_max 0.772 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(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_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 8656 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.1082 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4511 _reflns_number_gt 3264 _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 subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) 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^)+6.8378P] 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 4511 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1124 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.056 _refine_diff_density_min -1.696 _refine_diff_density_rms 0.205 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 0.52331(6) 0.26041(6) 0.26178(3) 0.03356(16) Uani 1 1 d . . . I1 I 0.77174(11) 0.14250(11) 0.16568(5) 0.0411(2) Uani 1 1 d . . . I2 I 0.33104(12) 0.29929(12) 0.39968(5) 0.0455(3) Uani 1 1 d . . . N1 N 0.2859(13) -0.0286(13) 0.2238(6) 0.037(3) Uani 1 1 d . . . N2 N 0.6313(13) 0.0827(13) 0.3426(6) 0.039(3) Uani 1 1 d . . . N3 N 0.8025(14) 0.4751(14) 0.3439(6) 0.037(3) Uani 1 1 d . . . C1 C 0.3975(15) 0.3418(16) 0.1361(8) 0.036(3) Uani 1 1 d . . . C2 C 0.2886(18) 0.3534(17) 0.1902(8) 0.042(3) Uani 1 1 d . . . H2 H 0.1781 0.2825 0.1866 0.050 Uiso 1 1 calc R . . C3 C 0.3747(19) 0.4894(18) 0.2502(9) 0.049(4) Uani 1 1 d . . . H3 H 0.3283 0.5225 0.2913 0.058 Uiso 1 1 calc R . . C4 C 0.5507(13) 0.5711(14) 0.2374(6) 0.021(2) Uani 1 1 d . . . H4 H 0.6360 0.6626 0.2668 0.026 Uiso 1 1 calc R . . C5 C 0.5532(17) 0.4688(17) 0.1662(8) 0.042(4) Uani 1 1 d . . . H5 H 0.6486 0.4860 0.1429 0.050 Uiso 1 1 calc R . . C6 C 0.3445(19) 0.2302(16) 0.0593(8) 0.044(4) Uani 1 1 d . . . C7 C 0.275(2) 0.0515(17) 0.0590(9) 0.056(4) Uani 1 1 d . . . H7A H 0.3628 0.0182 0.0782 0.083 Uiso 1 1 calc R . . H7B H 0.2303 -0.0134 0.0101 0.083 Uiso 1 1 calc R . . H7C H 0.1857 0.0349 0.0885 0.083 Uiso 1 1 calc R . . C8 C 0.203(2) 0.274(2) 0.0222(9) 0.054(4) Uani 1 1 d . . . H8A H 0.1102 0.2579 0.0497 0.080 Uiso 1 1 calc R . . H8B H 0.1647 0.2034 -0.0261 0.080 Uiso 1 1 calc R . . H8C H 0.2453 0.3869 0.0198 0.080 Uiso 1 1 calc R . . C9 C 0.490(2) 0.2608(18) 0.0172(8) 0.051(4) Uani 1 1 d . . . H9A H 0.5247 0.3728 0.0129 0.077 Uiso 1 1 calc R . . H9B H 0.4562 0.1867 -0.0304 0.077 Uiso 1 1 calc R . . H9C H 0.5826 0.2426 0.0420 0.077 Uiso 1 1 calc R . . C10 C 0.1194(17) -0.0518(17) 0.2183(8) 0.040(3) Uani 1 1 d . . . H10 H 0.0850 0.0342 0.2412 0.048 Uiso 1 1 calc R . . C11 C -0.0044(17) -0.2007(19) 0.1792(8) 0.043(4) Uani 1 1 d . . . H11 H -0.1182 -0.2113 0.1757 0.052 Uiso 1 1 calc R . . C12 C 0.0433(18) -0.3300(18) 0.1465(8) 0.044(4) Uani 1 1 d . . . H12 H -0.0376 -0.4304 0.1218 0.053 Uiso 1 1 calc R . . C13 C 0.2155(18) -0.3090(16) 0.1507(8) 0.041(3) Uani 1 1 d . . . H13 H 0.2526 -0.3935 0.1282 0.049 Uiso 1 1 calc R . . C14 C 0.3280(19) -0.1578(17) 0.1894(8) 0.043(3) Uani 1 1 d . . . H14 H 0.4426 -0.1436 0.1921 0.051 Uiso 1 1 calc R . . C15 C 0.5209(17) -0.0203(19) 0.3723(8) 0.045(4) Uani 1 1 d . . . H15 H 0.4080 -0.0281 0.3661 0.054 Uiso 1 1 calc R . . C16 C 0.570(2) -0.1192(17) 0.4132(9) 0.049(4) Uani 1 1 d . . . H16 H 0.4910 -0.1942 0.4319 0.059 Uiso 1 1 calc R . . C17 C 0.7394(19) -0.1007(17) 0.4244(8) 0.047(4) Uani 1 1 d . . . H17 H 0.7757 -0.1591 0.4534 0.056 Uiso 1 1 calc R . . C18 C 0.8562(16) 0.0045(15) 0.3928(7) 0.034(3) Uani 1 1 d . . . H18 H 0.9699 0.0147 0.3983 0.041 Uiso 1 1 calc R . . C19 C 0.7958(15) 0.0934(16) 0.3525(8) 0.035(3) Uani 1 1 d . . . H19 H 0.8724 0.1644 0.3311 0.042 Uiso 1 1 calc R . . C20 C 0.8212(16) 0.5146(17) 0.4156(8) 0.039(3) Uani 1 1 d . . . H20 H 0.7337 0.4597 0.4380 0.047 Uiso 1 1 calc R . . C21 C 0.9621(17) 0.632(2) 0.4589(9) 0.049(4) Uani 1 1 d . . . H21 H 0.9702 0.6552 0.5093 0.059 Uiso 1 1 calc R . . C22 C 1.0976(18) 0.718(2) 0.4239(9) 0.053(4) Uani 1 1 d . . . H22 H 1.1942 0.8018 0.4502 0.063 Uiso 1 1 calc R . . C23 C 1.0744(18) 0.6680(18) 0.3491(8) 0.043(3) Uani 1 1 d . . . H23 H 1.1597 0.7168 0.3242 0.052 Uiso 1 1 calc R . . C24 C 0.9311(17) 0.5499(16) 0.3110(9) 0.043(3) Uani 1 1 d . . . H24 H 0.9209 0.5195 0.2606 0.051 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 U 0.0310(3) 0.0333(3) 0.0365(3) 0.0110(2) 0.0043(2) 0.0097(2) I1 0.0364(5) 0.0462(5) 0.0416(6) 0.0097(4) 0.0068(4) 0.0161(4) I2 0.0423(5) 0.0509(6) 0.0444(6) 0.0138(5) 0.0144(4) 0.0143(5) N1 0.029(6) 0.027(5) 0.053(8) 0.006(5) 0.010(5) 0.009(5) N2 0.030(6) 0.038(6) 0.041(7) 0.008(5) 0.005(5) 0.006(5) N3 0.044(6) 0.043(6) 0.028(7) 0.009(5) 0.003(5) 0.019(6) C1 0.030(6) 0.032(7) 0.055(9) 0.019(7) 0.021(6) 0.015(6) C2 0.043(8) 0.040(8) 0.043(9) 0.016(7) 0.006(7) 0.013(7) C3 0.052(9) 0.042(8) 0.063(11) 0.021(8) 0.001(8) 0.025(7) C4 0.019(5) 0.026(6) 0.023(6) 0.005(5) 0.000(5) 0.014(5) C5 0.034(7) 0.047(8) 0.045(9) 0.028(7) -0.002(6) 0.004(7) C6 0.057(9) 0.031(7) 0.037(8) 0.002(6) 0.003(7) 0.008(7) C7 0.070(11) 0.040(8) 0.050(10) 0.006(8) 0.006(8) 0.012(8) C8 0.059(10) 0.057(10) 0.045(10) 0.016(8) -0.004(8) 0.020(8) C9 0.064(10) 0.040(8) 0.037(9) 0.005(7) -0.008(8) 0.005(8) C10 0.039(7) 0.040(8) 0.047(9) 0.022(7) 0.004(7) 0.014(7) C11 0.030(7) 0.058(10) 0.039(9) 0.020(8) -0.008(6) 0.009(7) C12 0.046(8) 0.038(8) 0.042(9) 0.017(7) 0.005(7) 0.000(7) C13 0.054(9) 0.027(7) 0.040(9) 0.012(6) 0.010(7) 0.010(7) C14 0.053(9) 0.047(8) 0.037(8) 0.021(7) 0.010(7) 0.022(7) C15 0.032(7) 0.062(10) 0.046(9) 0.017(8) 0.006(7) 0.020(7) C16 0.055(9) 0.029(7) 0.056(10) 0.009(7) 0.007(8) 0.005(7) C17 0.058(9) 0.039(8) 0.039(9) 0.009(7) -0.005(7) 0.013(7) C18 0.036(7) 0.030(7) 0.039(8) 0.008(6) -0.007(6) 0.017(6) C19 0.024(6) 0.029(7) 0.042(8) -0.007(6) 0.000(6) 0.007(6) C20 0.031(7) 0.042(8) 0.048(9) 0.022(7) 0.009(6) 0.007(6) C21 0.041(8) 0.067(10) 0.049(10) 0.016(8) 0.016(7) 0.029(8) C22 0.032(7) 0.059(10) 0.048(10) -0.013(8) -0.011(7) 0.010(7) C23 0.047(8) 0.046(8) 0.038(9) 0.006(7) 0.009(7) 0.021(7) C24 0.038(8) 0.030(7) 0.050(10) 0.003(7) -0.004(7) 0.005(6) _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 N1 2.607(10) . ? U N3 2.641(11) . ? U N2 2.724(11) . ? U C3 2.732(14) . ? U C2 2.757(14) . ? U C4 2.818(11) . ? U C5 2.822(12) . ? U C1 2.873(14) . ? U I1 3.1466(11) . ? U I2 3.1912(11) . ? N1 C10 1.347(16) . ? N1 C14 1.349(17) . ? N2 C15 1.328(17) . ? N2 C19 1.357(16) . ? N3 C20 1.319(17) . ? N3 C24 1.350(17) . ? C1 C5 1.412(18) . ? C1 C2 1.434(18) . ? C1 C6 1.53(2) . ? C2 C3 1.42(2) . ? C3 C4 1.492(18) . ? C4 C5 1.465(19) . ? C6 C9 1.50(2) . ? C6 C7 1.496(19) . ? C6 C8 1.54(2) . ? C10 C11 1.404(19) . ? C11 C12 1.37(2) . ? C12 C13 1.40(2) . ? C13 C14 1.380(19) . ? C15 C16 1.42(2) . ? C16 C17 1.38(2) . ? C17 C18 1.390(18) . ? C18 C19 1.387(17) . ? C20 C21 1.37(2) . ? C21 C22 1.45(2) . ? C22 C23 1.38(2) . ? C23 C24 1.352(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 U N3 152.1(3) . . ? N1 U N2 76.6(3) . . ? N3 U N2 75.7(3) . . ? N1 U I1 93.4(2) . . ? N3 U I1 84.6(2) . . ? N2 U I1 78.7(2) . . ? N1 U I2 82.1(2) . . ? N3 U I2 88.4(2) . . ? N2 U I2 77.3(2) . . ? I1 U I2 155.97(3) . . ? C10 N1 C14 116.0(12) . . ? C10 N1 U 124.1(8) . . ? C14 N1 U 117.5(8) . . ? C15 N2 C19 118.4(12) . . ? C15 N2 U 119.8(8) . . ? C19 N2 U 121.8(9) . . ? C20 N3 C24 118.5(12) . . ? C20 N3 U 123.2(9) . . ? C24 N3 U 118.3(9) . . ? C5 C1 C2 105.2(13) . . ? C5 C1 C6 128.4(12) . . ? C2 C1 C6 125.8(12) . . ? C3 C2 C1 109.8(13) . . ? C2 C3 C4 109.7(13) . . ? C5 C4 C3 101.4(11) . . ? C1 C5 C4 113.8(12) . . ? C9 C6 C7 110.5(13) . . ? C9 C6 C1 110.4(11) . . ? C7 C6 C1 112.1(12) . . ? C9 C6 C8 108.8(12) . . ? C7 C6 C8 107.5(13) . . ? C1 C6 C8 107.5(12) . . ? N1 C10 C11 122.6(13) . . ? C12 C11 C10 119.6(13) . . ? C11 C12 C13 119.1(13) . . ? C14 C13 C12 117.2(14) . . ? N1 C14 C13 125.5(14) . . ? N2 C15 C16 121.8(12) . . ? C17 C16 C15 118.1(13) . . ? C16 C17 C18 120.7(13) . . ? C19 C18 C17 117.0(12) . . ? N2 C19 C18 123.8(12) . . ? N3 C20 C21 123.9(13) . . ? C20 C21 C22 118.0(14) . . ? C23 C22 C21 115.8(13) . . ? C24 C23 C22 121.8(14) . . ? N3 C24 C23 121.9(14) . . ? #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 258870' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 I N2 U' _chemical_formula_weight 765.52 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.3285(10) _cell_length_b 26.8832(17) _cell_length_c 16.9576(11) _cell_angle_alpha 90.00 _cell_angle_beta 113.450(3) _cell_angle_gamma 90.00 _cell_volume 8501.8(9) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 55233 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method ? _exptl_crystal_F_000 4356 _exptl_absorpt_coefficient_mu 6.833 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.250 _exptl_absorpt_correction_T_max 0.761 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(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_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 55233 _diffrn_reflns_av_R_equivalents 0.1475 _diffrn_reflns_av_sigmaI/netI 0.1152 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.68 _reflns_number_total 15807 _reflns_number_gt 9639 _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 subsequent Fourier-difference synthesis. Due to very low crystal quality and rather large size of the asymmetric unit (three independent molecules), the refinement was very unsatisfactory and only a rough model of the structure has been obtained. All non-hydrogen atoms were refined with anisotropic displacement parameters, but restraints had to be applied for the more badly behaving atoms. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. The highest residual electron density peaks are located near the uranium and iodine atoms. 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^)+119.4835P] 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 15807 _refine_ls_number_parameters 883 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.1864 _refine_ls_R_factor_gt 0.1266 _refine_ls_wR_factor_ref 0.2591 _refine_ls_wR_factor_gt 0.2290 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 4.942 _refine_diff_density_min -4.886 _refine_diff_density_rms 0.263 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 U1 U 0.02399(6) 0.28304(4) 0.34564(6) 0.0452(3) Uani 1 1 d . . . U2 U 0.25124(5) 0.56064(4) 0.48845(7) 0.0444(3) Uani 1 1 d . . . U3 U 0.53724(6) 0.72256(4) 0.33697(6) 0.0456(3) Uani 1 1 d . . . I1 I -0.03692(11) 0.22253(7) 0.17084(11) 0.0539(5) Uani 1 1 d . . . I2 I 0.24552(12) 0.44284(7) 0.49407(12) 0.0563(5) Uani 1 1 d . . . I3 I 0.48071(11) 0.77943(7) 0.15777(12) 0.0572(5) Uani 1 1 d . . . N1A N -0.0974(10) 0.2462(8) 0.3545(13) 0.040(5) Uani 1 1 d . . . N2A N 0.1338(13) 0.3006(8) 0.2932(14) 0.050(6) Uani 1 1 d . . . N1B N 0.1051(12) 0.5473(8) 0.4351(13) 0.042(5) Uani 1 1 d . . . N2B N 0.3954(12) 0.5437(7) 0.5490(13) 0.044(5) Uani 1 1 d . . . N1C N 0.6449(11) 0.6975(9) 0.2868(14) 0.046(5) Uani 1 1 d . . . N2C N 0.4102(12) 0.7577(8) 0.3381(14) 0.047(6) Uani 1 1 d . . . C1B C 0.2768(14) 0.5732(12) 0.6678(18) 0.054(7) Uani 1 1 d . . . C1A C -0.0351(14) 0.3769(10) 0.262(2) 0.052(7) Uani 1 1 d . . . C1C C 0.6004(15) 0.8112(13) 0.4326(15) 0.057(8) Uani 1 1 d . . . C2C C 0.6589(14) 0.7816(11) 0.4354(17) 0.053(7) Uani 1 1 d . . . H2C H 0.6915 0.7891 0.4112 0.064 Uiso 1 1 calc R . . C2B C 0.2053(17) 0.5928(12) 0.6163(19) 0.060(8) Uani 1 1 d U . . H2B H 0.1618 0.5800 0.6132 0.071 Uiso 1 1 calc R . . C2A C 0.0355(19) 0.3841(13) 0.321(2) 0.071(9) Uani 1 1 d U . . H2A H 0.0752 0.3908 0.3085 0.085 Uiso 1 1 calc R . . C3B C 0.2151(15) 0.6344(10) 0.572(2) 0.058(8) Uani 1 1 d . . . H3B H 0.1785 0.6539 0.5340 0.070 Uiso 1 1 calc R . . C3A C 0.0348(14) 0.3791(11) 0.4047(18) 0.054(8) Uani 1 1 d . . . H3A H 0.0730 0.3856 0.4565 0.065 Uiso 1 1 calc R . . C3C C 0.6578(15) 0.7379(13) 0.4824(18) 0.061(9) Uani 1 1 d . . . H3C H 0.6900 0.7117 0.4931 0.074 Uiso 1 1 calc R . . C4C C 0.6028(18) 0.7399(12) 0.5097(17) 0.063(9) Uani 1 1 d . . . H4C H 0.5914 0.7159 0.5418 0.076 Uiso 1 1 calc R . . C4B C 0.2861(16) 0.6418(10) 0.595(2) 0.062(8) Uani 1 1 d . . . H4B H 0.3058 0.6679 0.5755 0.074 Uiso 1 1 calc R . . C4A C -0.0316(17) 0.3631(10) 0.395(3) 0.064(9) Uani 1 1 d . . . H4A H -0.0435 0.3541 0.4411 0.077 Uiso 1 1 calc R . . C5C C 0.5659(13) 0.7862(9) 0.4794(15) 0.040(6) Uani 1 1 d U . . H5C H 0.5265 0.7977 0.4888 0.049 Uiso 1 1 calc R . . C5B C 0.3249(15) 0.6050(9) 0.6504(17) 0.049(7) Uani 1 1 d . . . H5B H 0.3745 0.6015 0.6727 0.059 Uiso 1 1 calc R . . C5A C -0.0786(17) 0.3619(10) 0.311(2) 0.061(9) Uani 1 1 d . . . H5A H -0.1270 0.3537 0.2898 0.074 Uiso 1 1 calc R . . C6B C 0.2962(16) 0.5335(11) 0.7401(18) 0.052(7) Uani 1 1 d . . . C6A C -0.0647(16) 0.3897(12) 0.169(2) 0.063(8) Uani 1 1 d . . . C6C C 0.5901(16) 0.8666(11) 0.4058(18) 0.054(7) Uani 1 1 d . . . C7C C 0.6261(16) 0.8770(13) 0.341(2) 0.067(9) Uani 1 1 d . . . H7C1 H 0.6752 0.8663 0.3663 0.100 Uiso 1 1 calc R . . H7C2 H 0.6243 0.9120 0.3295 0.100 Uiso 1 1 calc R . . H7C3 H 0.6010 0.8592 0.2890 0.100 Uiso 1 1 calc R . . C7B C 0.3131(18) 0.5595(13) 0.824(2) 0.071(9) Uani 1 1 d U . . H7B1 H 0.3236 0.5353 0.8690 0.107 Uiso 1 1 calc R . . H7B2 H 0.2726 0.5791 0.8206 0.107 Uiso 1 1 calc R . . H7B3 H 0.3539 0.5808 0.8361 0.107 Uiso 1 1 calc R . . C7A C -0.0781(17) 0.4451(12) 0.159(2) 0.064(8) Uani 1 1 d U . . H7A1 H -0.1008 0.4559 0.1957 0.096 Uiso 1 1 calc R . . H7A2 H -0.1087 0.4523 0.1001 0.096 Uiso 1 1 calc R . . H7A3 H -0.0333 0.4622 0.1738 0.096 Uiso 1 1 calc R . . C8C C 0.5088(15) 0.8780(10) 0.3607(19) 0.056(8) Uani 1 1 d . . . H8C1 H 0.4886 0.8597 0.3079 0.084 Uiso 1 1 calc R . . H8C2 H 0.5020 0.9130 0.3488 0.084 Uiso 1 1 calc R . . H8C3 H 0.4854 0.8684 0.3976 0.084 Uiso 1 1 calc R . . C8A C -0.1414(14) 0.3636(9) 0.120(2) 0.055(8) Uani 1 1 d . . . H8A1 H -0.1382 0.3291 0.1355 0.082 Uiso 1 1 calc R . . H8A2 H -0.1550 0.3663 0.0587 0.082 Uiso 1 1 calc R . . H8A3 H -0.1766 0.3797 0.1352 0.082 Uiso 1 1 calc R . . C8B C 0.2300(16) 0.4985(12) 0.722(2) 0.062(8) Uani 1 1 d . . . H8B1 H 0.2440 0.4711 0.7621 0.093 Uiso 1 1 calc R . . H8B2 H 0.2132 0.4860 0.6647 0.093 Uiso 1 1 calc R . . H8B3 H 0.1924 0.5169 0.7298 0.093 Uiso 1 1 calc R . . C9A C -0.0147(16) 0.3722(12) 0.1293(19) 0.062(8) Uani 1 1 d . . . H9A1 H 0.0297 0.3902 0.1538 0.092 Uiso 1 1 calc R . . H9A2 H -0.0362 0.3779 0.0684 0.092 Uiso 1 1 calc R . . H9A3 H -0.0056 0.3373 0.1401 0.092 Uiso 1 1 calc R . . C9B C 0.3577(16) 0.5024(11) 0.7390(18) 0.055(8) Uani 1 1 d . . . H9B1 H 0.4010 0.5217 0.7606 0.083 Uiso 1 1 calc R . . H9B2 H 0.3478 0.4921 0.6811 0.083 Uiso 1 1 calc R . . H9B3 H 0.3634 0.4735 0.7745 0.083 Uiso 1 1 calc R . . C10C C 0.4787(17) 0.6266(10) 0.263(2) 0.054(8) Uani 1 1 d . . . C10A C 0.0972(13) 0.1982(11) 0.4520(19) 0.053(7) Uani 1 1 d . . . C10B C 0.2235(13) 0.5650(10) 0.3079(18) 0.046(7) Uani 1 1 d . . . C11A C 0.0568(17) 0.2229(11) 0.4917(17) 0.057(8) Uani 1 1 d . . . H11A H 0.0176 0.2091 0.4989 0.068 Uiso 1 1 calc R . . C11B C 0.1822(15) 0.6004(11) 0.3209(17) 0.055(8) Uani 1 1 d . . . H11B H 0.1323 0.5998 0.2960 0.066 Uiso 1 1 calc R . . C11C C 0.4425(17) 0.6447(11) 0.3187(19) 0.059(8) Uani 1 1 d U . . H11C H 0.3945 0.6538 0.2994 0.071 Uiso 1 1 calc R . . C12A C 0.0843(16) 0.2724(10) 0.5197(16) 0.051(7) Uani 1 1 d . . . H12A H 0.0675 0.2950 0.5488 0.061 Uiso 1 1 calc R . . C12B C 0.2224(18) 0.6385(11) 0.376(2) 0.066(9) Uani 1 1 d . . . H12B H 0.2055 0.6661 0.3953 0.079 Uiso 1 1 calc R . . C12C C 0.4917(18) 0.6459(12) 0.404(2) 0.066(9) Uani 1 1 d U . . H12C H 0.4821 0.6558 0.4511 0.080 Uiso 1 1 calc R . . C13A C 0.1395(15) 0.2792(11) 0.4952(18) 0.054(7) Uani 1 1 d U . . H13A H 0.1664 0.3082 0.5030 0.065 Uiso 1 1 calc R . . C13B C 0.2942(18) 0.6249(12) 0.395(2) 0.063(8) Uani 1 1 d U . . H13B H 0.3342 0.6427 0.4307 0.076 Uiso 1 1 calc R . . C13C C 0.5550(16) 0.6305(10) 0.4068(19) 0.057(8) Uani 1 1 d . . . H13C H 0.5972 0.6291 0.4560 0.069 Uiso 1 1 calc R . . C14C C 0.5481(11) 0.6161(10) 0.3196(14) 0.038(6) Uani 1 1 d . . . H14C H 0.5839 0.6024 0.3054 0.045 Uiso 1 1 calc R . . C14A C 0.1497(14) 0.2352(10) 0.4558(16) 0.045(6) Uani 1 1 d U . . H14A H 0.1854 0.2307 0.4351 0.054 Uiso 1 1 calc R . . C14B C 0.2959(13) 0.5810(10) 0.3528(18) 0.053(8) Uani 1 1 d . . . H14B H 0.3367 0.5650 0.3535 0.063 Uiso 1 1 calc R . . C15B C 0.1970(13) 0.5213(10) 0.2406(15) 0.042(6) Uani 1 1 d . . . C15C C 0.4419(15) 0.6129(10) 0.167(2) 0.055(8) Uani 1 1 d . . . C15A C 0.0890(15) 0.1446(11) 0.4277(18) 0.052(7) Uani 1 1 d . . . C16C C 0.3719(17) 0.6392(12) 0.126(2) 0.074(10) Uani 1 1 d . . . H16A H 0.3802 0.6742 0.1235 0.111 Uiso 1 1 calc R . . H16B H 0.3432 0.6335 0.1580 0.111 Uiso 1 1 calc R . . H16C H 0.3472 0.6268 0.0682 0.111 Uiso 1 1 calc R . . C16B C 0.2590(15) 0.4842(11) 0.257(2) 0.061(8) Uani 1 1 d . . . H16D H 0.2749 0.4715 0.3146 0.091 Uiso 1 1 calc R . . H16E H 0.2980 0.5008 0.2499 0.091 Uiso 1 1 calc R . . H16F H 0.2426 0.4572 0.2169 0.091 Uiso 1 1 calc R . . C16A C 0.1299(17) 0.1136(13) 0.5087(18) 0.069(9) Uani 1 1 d . . . H16G H 0.1803 0.1203 0.5284 0.103 Uiso 1 1 calc R . . H16H H 0.1212 0.0789 0.4955 0.103 Uiso 1 1 calc R . . H16I H 0.1137 0.1224 0.5529 0.103 Uiso 1 1 calc R . . C17B C 0.1314(14) 0.4970(12) 0.2466(17) 0.053(7) Uani 1 1 d . . . H17A H 0.0955 0.5219 0.2393 0.080 Uiso 1 1 calc R . . H17B H 0.1448 0.4816 0.3019 0.080 Uiso 1 1 calc R . . H17C H 0.1125 0.4723 0.2024 0.080 Uiso 1 1 calc R . . C17C C 0.4929(14) 0.6259(11) 0.1238(19) 0.057(8) Uani 1 1 d . . . H17D H 0.4695 0.6196 0.0632 0.086 Uiso 1 1 calc R . . H17E H 0.5354 0.6059 0.1478 0.086 Uiso 1 1 calc R . . H17F H 0.5058 0.6605 0.1331 0.086 Uiso 1 1 calc R . . C17A C 0.1283(16) 0.1340(13) 0.3663(16) 0.063(9) Uani 1 1 d . . . H17G H 0.1035 0.1506 0.3124 0.095 Uiso 1 1 calc R . . H17H H 0.1287 0.0988 0.3566 0.095 Uiso 1 1 calc R . . H17I H 0.1767 0.1460 0.3923 0.095 Uiso 1 1 calc R . . C18A C 0.0119(13) 0.1287(11) 0.3855(19) 0.055(7) Uani 1 1 d . . . H18A H -0.0088 0.1281 0.4274 0.082 Uiso 1 1 calc R . . H18B H 0.0093 0.0961 0.3613 0.082 Uiso 1 1 calc R . . H18C H -0.0139 0.1519 0.3407 0.082 Uiso 1 1 calc R . . C18B C 0.1784(17) 0.5469(12) 0.1518(19) 0.066(8) Uani 1 1 d U . . H18D H 0.1719 0.5220 0.1088 0.099 Uiso 1 1 calc R . . H18E H 0.2168 0.5687 0.1552 0.099 Uiso 1 1 calc R . . H18F H 0.1350 0.5658 0.1368 0.099 Uiso 1 1 calc R . . C19C C 0.6502(17) 0.7069(12) 0.2090(17) 0.063(9) Uani 1 1 d . . . H19C H 0.6156 0.7266 0.1684 0.075 Uiso 1 1 calc R . . C19A C -0.1433(14) 0.2133(11) 0.301(2) 0.061(8) Uani 1 1 d . . . H19A H -0.1378 0.2052 0.2510 0.073 Uiso 1 1 calc R . . C19B C 0.0661(14) 0.5049(10) 0.424(2) 0.055(8) Uani 1 1 d . . . H19B H 0.0908 0.4749 0.4381 0.066 Uiso 1 1 calc R . . C20C C 0.7032(18) 0.6885(14) 0.1908(19) 0.068(10) Uani 1 1 d . . . H20C H 0.7068 0.6980 0.1399 0.082 Uiso 1 1 calc R . . C20A C -0.1988(19) 0.1903(14) 0.317(2) 0.076(10) Uani 1 1 d U . . H20A H -0.2286 0.1677 0.2769 0.091 Uiso 1 1 calc R . . C20B C -0.0054(18) 0.5035(14) 0.394(2) 0.071(9) Uani 1 1 d U . . H20B H -0.0282 0.4732 0.3913 0.086 Uiso 1 1 calc R . . C21B C -0.046(2) 0.5455(14) 0.366(2) 0.080(10) Uani 1 1 d U . . H21B H -0.0956 0.5446 0.3420 0.096 Uiso 1 1 calc R . . C21A C -0.2099(17) 0.2007(12) 0.390(2) 0.063(8) Uani 1 1 d U . . H21A H -0.2458 0.1854 0.4023 0.075 Uiso 1 1 calc R . . C21C C 0.7490(17) 0.6583(13) 0.241(2) 0.066(9) Uani 1 1 d . . . H21C H 0.7836 0.6454 0.2234 0.079 Uiso 1 1 calc R . . C22A C -0.1634(14) 0.2358(9) 0.4448(19) 0.046(7) Uani 1 1 d . . . H22A H -0.1687 0.2453 0.4947 0.055 Uiso 1 1 calc R . . C22B C -0.0081(15) 0.5890(11) 0.3766(18) 0.056(8) Uani 1 1 d . . . H22B H -0.0326 0.6188 0.3575 0.068 Uiso 1 1 calc R . . C22C C 0.7499(14) 0.6442(10) 0.3172(16) 0.045(6) Uani 1 1 d . . . H22C H 0.7831 0.6215 0.3526 0.054 Uiso 1 1 calc R . . C23C C 0.6975(11) 0.6660(11) 0.3396(14) 0.045(7) Uani 1 1 d . . . H23C H 0.6980 0.6588 0.3935 0.054 Uiso 1 1 calc R . . C23A C -0.1092(16) 0.2565(10) 0.425(2) 0.055(8) Uani 1 1 d . . . H23A H -0.0787 0.2793 0.4640 0.066 Uiso 1 1 calc R . . C23B C 0.0660(16) 0.5890(9) 0.4154(18) 0.056(8) Uani 1 1 d . . . H23B H 0.0897 0.6194 0.4283 0.067 Uiso 1 1 calc R . . C24C C 0.3621(13) 0.7831(10) 0.274(2) 0.057(8) Uani 1 1 d . . . H24C H 0.3717 0.7908 0.2265 0.068 Uiso 1 1 calc R . . C24A C 0.1408(15) 0.2796(10) 0.2234(18) 0.052(7) Uani 1 1 d . . . H24A H 0.1056 0.2576 0.1894 0.063 Uiso 1 1 calc R . . C24B C 0.4412(15) 0.5829(11) 0.5701(18) 0.053(8) Uani 1 1 d . . . H24B H 0.4215 0.6147 0.5606 0.064 Uiso 1 1 calc R . . C25A C 0.1975(17) 0.2896(13) 0.202(2) 0.068(9) Uani 1 1 d U . . H25A H 0.2009 0.2743 0.1541 0.081 Uiso 1 1 calc R . . C25B C 0.5137(17) 0.5790(12) 0.604(2) 0.064(8) Uani 1 1 d U . . H25B H 0.5428 0.6071 0.6150 0.077 Uiso 1 1 calc R . . C25C C 0.2976(19) 0.7986(13) 0.277(2) 0.071(9) Uani 1 1 d U . . H25C H 0.2630 0.8143 0.2298 0.086 Uiso 1 1 calc R . . C26B C 0.5431(18) 0.5307(12) 0.621(2) 0.063(8) Uani 1 1 d U . . H26B H 0.5925 0.5259 0.6456 0.076 Uiso 1 1 calc R . . C26A C 0.2505(13) 0.3234(12) 0.252(2) 0.060(8) Uani 1 1 d . . . H26A H 0.2881 0.3322 0.2366 0.072 Uiso 1 1 calc R . . C26C C 0.2864(16) 0.7901(12) 0.3502(19) 0.060(8) Uani 1 1 d U . . H26C H 0.2447 0.8015 0.3544 0.072 Uiso 1 1 calc R . . C27A C 0.2455(14) 0.3431(11) 0.3234(17) 0.048(7) Uani 1 1 d . . . H27A H 0.2808 0.3641 0.3598 0.058 Uiso 1 1 calc R . . C27B C 0.4982(16) 0.4922(12) 0.6023(19) 0.057(7) Uani 1 1 d U . . H27B H 0.5173 0.4603 0.6143 0.069 Uiso 1 1 calc R . . C27C C 0.3392(17) 0.7636(11) 0.421(2) 0.065(9) Uani 1 1 d . . . H27C H 0.3325 0.7558 0.4704 0.078 Uiso 1 1 calc R . . C28B C 0.4246(15) 0.4975(10) 0.5654(17) 0.050(7) Uani 1 1 d . . . H28B H 0.3952 0.4696 0.5518 0.060 Uiso 1 1 calc R . . C28A C 0.1861(16) 0.3306(10) 0.3401(16) 0.050(7) Uani 1 1 d . . . H28A H 0.1829 0.3447 0.3885 0.060 Uiso 1 1 calc R . . C28C C 0.4005(15) 0.7504(10) 0.4094(18) 0.051(7) Uani 1 1 d . . . H28C H 0.4374 0.7353 0.4552 0.062 Uiso 1 1 calc R . . C18C C 0.4320(18) 0.5536(12) 0.168(2) 0.080(11) Uani 1 1 d . . . H18G H 0.3953 0.5433 0.1143 0.120 Uiso 1 1 calc R . . H18H H 0.4184 0.5446 0.2142 0.120 Uiso 1 1 calc R . . H18I H 0.4764 0.5376 0.1758 0.120 Uiso 1 1 calc R . . C9C C 0.6271(16) 0.8979(12) 0.4856(19) 0.065(9) Uani 1 1 d . . . H9C1 H 0.6026 0.8941 0.5234 0.097 Uiso 1 1 calc R . . H9C2 H 0.6261 0.9322 0.4695 0.097 Uiso 1 1 calc R . . H9C3 H 0.6759 0.8872 0.5144 0.097 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 U1 0.0550(6) 0.0437(6) 0.0442(5) -0.0085(5) 0.0274(5) -0.0158(5) U2 0.0396(5) 0.0328(5) 0.0507(6) 0.0022(5) 0.0071(4) -0.0001(5) U3 0.0548(6) 0.0464(6) 0.0401(5) 0.0084(5) 0.0237(5) 0.0172(5) I1 0.0709(13) 0.0420(10) 0.0445(10) -0.0035(8) 0.0183(9) -0.0025(9) I2 0.0769(13) 0.0402(10) 0.0468(10) 0.0001(8) 0.0194(10) -0.0005(10) I3 0.0703(13) 0.0479(11) 0.0472(10) 0.0071(9) 0.0167(9) 0.0031(10) N1A 0.030(11) 0.050(13) 0.040(12) 0.006(10) 0.015(9) 0.003(10) N2A 0.064(15) 0.033(12) 0.047(13) -0.004(10) 0.017(12) 0.010(11) N1B 0.058(14) 0.039(12) 0.040(11) -0.017(9) 0.030(11) -0.016(10) N2B 0.061(14) 0.031(11) 0.052(13) 0.019(9) 0.037(12) 0.001(10) N1C 0.034(11) 0.064(15) 0.050(13) 0.002(11) 0.028(10) 0.014(11) N2C 0.058(14) 0.044(13) 0.048(13) -0.005(10) 0.031(12) 0.022(11) C1B 0.040(15) 0.07(2) 0.049(16) -0.023(14) 0.012(13) -0.005(14) C1A 0.038(14) 0.035(14) 0.09(2) 0.017(14) 0.027(15) 0.008(12) C1C 0.055(17) 0.09(2) 0.018(12) -0.010(13) 0.005(12) 0.010(16) C2C 0.042(15) 0.064(19) 0.046(15) -0.009(14) 0.010(13) 0.007(14) C2B 0.057(9) 0.060(9) 0.060(9) -0.002(5) 0.022(5) 0.001(5) C2A 0.071(10) 0.069(10) 0.071(10) -0.004(5) 0.028(6) 0.001(5) C3B 0.048(17) 0.033(15) 0.08(2) -0.022(14) 0.006(15) 0.004(12) C3A 0.040(15) 0.07(2) 0.060(18) -0.042(15) 0.031(14) -0.009(14) C3C 0.049(17) 0.08(2) 0.049(16) -0.014(15) 0.016(14) 0.035(16) C4C 0.09(2) 0.06(2) 0.040(16) 0.020(14) 0.028(16) 0.017(18) C4B 0.058(19) 0.032(15) 0.08(2) 0.000(14) 0.005(16) -0.012(14) C4A 0.056(19) 0.032(15) 0.12(3) 0.005(17) 0.05(2) -0.006(14) C5C 0.037(7) 0.042(7) 0.042(7) -0.002(5) 0.016(5) 0.005(5) C5B 0.046(15) 0.023(12) 0.057(17) -0.009(11) -0.002(13) 0.002(11) C5A 0.046(17) 0.038(16) 0.11(3) 0.009(17) 0.043(19) 0.005(13) C6B 0.065(18) 0.057(18) 0.051(16) -0.012(13) 0.040(15) 0.013(15) C6A 0.047(17) 0.054(19) 0.09(2) -0.005(17) 0.029(17) -0.012(15) C6C 0.064(19) 0.048(17) 0.051(17) -0.015(13) 0.023(15) 0.011(14) C7C 0.053(18) 0.08(2) 0.07(2) -0.009(17) 0.025(16) 0.015(17) C7B 0.070(10) 0.071(10) 0.072(10) -0.003(5) 0.028(6) 0.002(5) C7A 0.062(9) 0.062(9) 0.066(9) -0.001(5) 0.025(5) -0.001(5) C8C 0.061(19) 0.036(15) 0.07(2) -0.015(14) 0.029(16) -0.008(14) C8A 0.047(16) 0.021(13) 0.08(2) -0.004(13) 0.012(15) 0.002(11) C8B 0.061(19) 0.07(2) 0.08(2) -0.018(17) 0.051(17) -0.007(16) C9A 0.061(19) 0.07(2) 0.058(19) -0.020(16) 0.024(16) -0.016(16) C9B 0.08(2) 0.059(18) 0.056(16) 0.017(15) 0.052(16) 0.023(16) C10C 0.07(2) 0.045(16) 0.07(2) 0.012(14) 0.056(18) 0.007(14) C10A 0.020(12) 0.055(18) 0.064(18) 0.004(14) -0.004(12) 0.001(12) C10B 0.040(14) 0.038(14) 0.070(18) 0.031(13) 0.033(14) 0.009(12) C11A 0.069(19) 0.060(19) 0.043(15) 0.006(14) 0.023(14) -0.026(16) C11B 0.049(16) 0.059(18) 0.049(16) 0.010(13) 0.010(13) -0.042(15) C11C 0.059(9) 0.058(9) 0.063(9) -0.001(5) 0.026(5) 0.001(5) C12A 0.071(19) 0.046(16) 0.037(14) -0.003(12) 0.023(14) -0.012(14) C12B 0.08(2) 0.036(16) 0.09(2) 0.017(16) 0.05(2) 0.009(16) C12C 0.068(10) 0.066(10) 0.067(9) 0.003(5) 0.030(6) -0.001(5) C13A 0.056(8) 0.053(8) 0.054(8) 0.004(5) 0.022(5) -0.006(5) C13B 0.062(9) 0.062(9) 0.064(9) 0.004(5) 0.022(5) -0.002(5) C13C 0.049(17) 0.047(17) 0.056(18) 0.008(14) 0.000(14) 0.015(14) C14C 0.017(11) 0.071(17) 0.031(12) 0.003(11) 0.015(10) 0.010(11) C14A 0.041(7) 0.045(7) 0.045(7) 0.003(5) 0.015(5) -0.004(5) C14B 0.027(13) 0.050(16) 0.065(18) 0.022(14) 0.001(13) -0.009(12) C15B 0.041(14) 0.057(16) 0.038(13) -0.010(12) 0.027(12) -0.018(12) C15C 0.045(16) 0.045(16) 0.09(2) 0.019(15) 0.040(16) 0.004(13) C15A 0.048(16) 0.064(19) 0.055(17) 0.012(14) 0.031(14) 0.012(14) C16C 0.07(2) 0.06(2) 0.10(3) 0.005(18) 0.03(2) -0.006(17) C16B 0.044(16) 0.057(19) 0.07(2) 0.016(15) 0.011(15) 0.000(14) C16A 0.07(2) 0.10(3) 0.039(16) 0.031(16) 0.015(15) 0.016(19) C17B 0.043(15) 0.08(2) 0.051(15) -0.006(15) 0.031(13) -0.011(15) C17C 0.035(14) 0.064(19) 0.07(2) 0.037(16) 0.022(14) 0.009(14) C17A 0.058(18) 0.10(3) 0.022(13) 0.017(14) 0.008(13) 0.016(18) C18A 0.027(13) 0.057(18) 0.07(2) -0.001(15) 0.009(13) 0.009(13) C18B 0.066(9) 0.068(10) 0.065(9) 0.000(5) 0.027(6) -0.002(5) C19C 0.06(2) 0.07(2) 0.036(15) 0.007(14) 0.002(14) -0.037(17) C19A 0.037(15) 0.054(18) 0.10(2) -0.025(17) 0.032(16) -0.017(14) C19B 0.028(14) 0.037(15) 0.11(2) -0.003(16) 0.038(15) 0.005(11) C20C 0.07(2) 0.11(3) 0.049(17) 0.020(18) 0.051(17) 0.00(2) C20A 0.073(11) 0.075(11) 0.077(11) -0.001(5) 0.028(6) -0.001(5) C20B 0.069(10) 0.071(10) 0.074(10) 0.000(5) 0.029(6) -0.002(5) C21B 0.079(11) 0.080(11) 0.082(11) 0.000(5) 0.033(6) 0.000(5) C21A 0.060(9) 0.063(9) 0.064(9) -0.002(5) 0.024(5) 0.000(5) C21C 0.053(18) 0.08(2) 0.08(2) 0.010(19) 0.045(18) 0.022(17) C22A 0.044(15) 0.035(14) 0.074(19) -0.018(13) 0.039(14) -0.009(12) C22B 0.053(17) 0.055(18) 0.053(17) -0.028(14) 0.012(14) -0.022(14) C22C 0.052(16) 0.058(17) 0.044(14) 0.009(12) 0.038(13) 0.013(13) C23C 0.013(10) 0.10(2) 0.024(12) -0.010(13) 0.009(9) 0.006(12) C23A 0.062(18) 0.041(15) 0.09(2) -0.009(15) 0.054(18) -0.019(14) C23B 0.065(19) 0.023(13) 0.062(18) -0.003(12) 0.006(15) -0.019(13) C24C 0.025(12) 0.041(16) 0.09(2) 0.022(16) 0.012(14) -0.015(12) C24A 0.047(16) 0.042(16) 0.054(16) -0.009(13) 0.005(13) -0.017(13) C24B 0.061(18) 0.064(19) 0.060(17) 0.020(15) 0.051(16) 0.019(15) C25A 0.067(10) 0.071(10) 0.067(10) 0.000(5) 0.029(6) 0.001(5) C25B 0.064(9) 0.063(9) 0.066(9) 0.003(5) 0.026(6) 0.000(5) C25C 0.070(10) 0.071(10) 0.073(10) 0.002(5) 0.028(6) 0.001(5) C26B 0.061(9) 0.063(9) 0.065(9) 0.002(5) 0.025(5) 0.003(5) C26A 0.025(13) 0.09(2) 0.08(2) 0.002(18) 0.041(15) -0.002(14) C26C 0.057(9) 0.061(9) 0.062(9) 0.002(5) 0.024(5) 0.002(5) C27A 0.037(14) 0.062(18) 0.047(15) 0.000(13) 0.017(13) 0.012(13) C27B 0.056(9) 0.057(9) 0.062(9) 0.002(5) 0.026(5) -0.001(5) C27C 0.06(2) 0.047(17) 0.11(3) -0.010(17) 0.06(2) -0.016(15) C28B 0.049(16) 0.044(16) 0.057(16) 0.006(13) 0.021(13) 0.025(13) C28A 0.08(2) 0.045(15) 0.039(14) 0.000(12) 0.044(15) 0.010(15) C28C 0.047(16) 0.050(17) 0.050(16) -0.006(13) 0.011(13) 0.014(13) C18C 0.07(2) 0.06(2) 0.11(3) -0.03(2) 0.03(2) -0.018(18) C9C 0.059(19) 0.07(2) 0.06(2) -0.032(16) 0.019(16) -0.005(16) _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 U1 C13A 2.69(3) . ? U1 C4A 2.72(3) . ? U1 N1A 2.72(2) . ? U1 C12A 2.72(2) . ? U1 C3A 2.75(3) . ? U1 N2A 2.75(2) . ? U1 C2A 2.77(3) . ? U1 C14A 2.81(3) . ? U1 C11A 2.81(3) . ? U1 C5A 2.87(3) . ? U1 C1A 2.91(3) . ? U1 C10A 2.92(3) . ? U1 I1 3.169(2) . ? U2 C3B 2.71(3) . ? U2 C13B 2.71(3) . ? U2 N2B 2.73(2) . ? U2 C12B 2.73(3) . ? U2 C4B 2.74(3) . ? U2 N1B 2.76(2) . ? U2 C2B 2.82(3) . ? U2 C5B 2.82(3) . ? U2 C11B 2.83(3) . ? U2 C14B 2.84(3) . ? U2 C10B 2.89(3) . ? U2 C1B 2.89(3) . ? U2 I2 3.1718(19) . ? U3 C12C 2.69(3) . ? U3 C13C 2.70(3) . ? U3 C3C 2.73(3) . ? U3 N1C 2.729(18) . ? U3 C4C 2.73(3) . ? U3 N2C 2.76(2) . ? U3 C11C 2.78(3) . ? U3 C5C 2.83(2) . ? U3 C2C 2.85(3) . ? U3 C1C 2.88(3) . ? U3 C14C 2.89(3) . ? U3 C10C 2.91(3) . ? U3 I3 3.180(2) . ? N1A C19A 1.34(3) . ? N1A C23A 1.34(3) . ? N2A C28A 1.32(4) . ? N2A C24A 1.37(3) . ? N1B C23B 1.34(3) . ? N1B C19B 1.36(3) . ? N2B C24B 1.36(4) . ? N2B C28B 1.36(3) . ? N1C C23C 1.38(3) . ? N1C C19C 1.39(3) . ? N2C C28C 1.31(3) . ? N2C C24C 1.32(3) . ? C1B C5B 1.42(4) . ? C1B C2B 1.46(4) . ? C1B C6B 1.55(4) . ? C1A C2A 1.40(4) . ? C1A C6A 1.48(4) . ? C1A C5A 1.50(4) . ? C1C C2C 1.42(4) . ? C1C C5C 1.42(4) . ? C1C C6C 1.55(4) . ? C2C C3C 1.42(4) . ? C2B C3B 1.40(4) . ? C2A C3A 1.43(4) . ? C3B C4B 1.35(4) . ? C3A C4A 1.36(4) . ? C3C C4C 1.37(4) . ? C4C C5C 1.44(4) . ? C4B C5B 1.38(4) . ? C4A C5A 1.36(5) . ? C6B C7B 1.50(4) . ? C6B C9B 1.51(3) . ? C6B C8B 1.57(4) . ? C6A C9A 1.50(4) . ? C6A C7A 1.51(4) . ? C6A C8A 1.61(4) . ? C6C C9C 1.52(4) . ? C6C C8C 1.55(4) . ? C6C C7C 1.56(4) . ? C10C C14C 1.38(4) . ? C10C C11C 1.49(4) . ? C10C C15C 1.53(4) . ? C10A C11A 1.42(4) . ? C10A C14A 1.44(4) . ? C10A C15A 1.49(4) . ? C10B C11B 1.34(4) . ? C10B C14B 1.43(3) . ? C10B C15B 1.58(4) . ? C11A C12A 1.45(4) . ? C11B C12B 1.41(4) . ? C11C C12C 1.40(4) . ? C12A C13A 1.36(4) . ? C12B C13B 1.41(4) . ? C12C C13C 1.34(4) . ? C13A C14A 1.41(4) . ? C13B C14B 1.39(4) . ? C13C C14C 1.48(4) . ? C15B C17B 1.52(3) . ? C15B C16B 1.54(4) . ? C15B C18B 1.56(4) . ? C15C C16C 1.49(4) . ? C15C C17C 1.54(3) . ? C15C C18C 1.61(4) . ? C15A C18A 1.50(4) . ? C15A C16A 1.54(4) . ? C15A C17A 1.57(4) . ? C19C C20C 1.33(4) . ? C19A C20A 1.40(4) . ? C19B C20B 1.34(4) . ? C20C C21C 1.27(4) . ? C20A C21A 1.38(4) . ? C20B C21B 1.36(5) . ? C21B C22B 1.37(4) . ? C21A C22A 1.39(4) . ? C21C C22C 1.35(4) . ? C22A C23A 1.39(3) . ? C22B C23B 1.38(4) . ? C22C C23C 1.40(3) . ? C24C C25C 1.39(4) . ? C24A C25A 1.37(4) . ? C24B C25B 1.36(4) . ? C25A C26A 1.41(4) . ? C25B C26B 1.41(4) . ? C25C C26C 1.37(4) . ? C26B C27B 1.33(4) . ? C26A C27A 1.36(4) . ? C26C C27C 1.44(4) . ? C27A C28A 1.39(4) . ? C27B C28B 1.38(4) . ? C27C C28C 1.38(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 N1A U1 N2A 162.0(6) . . ? N1A U1 I1 80.8(4) . . ? N2A U1 I1 81.4(5) . . ? N2B U2 N1B 162.7(6) . . ? N2B U2 I2 82.5(4) . . ? N1B U2 I2 80.4(4) . . ? N1C U3 N2C 163.0(6) . . ? N1C U3 I3 81.4(5) . . ? N2C U3 I3 81.9(5) . . ? C19A N1A C23A 115(2) . . ? C19A N1A U1 127.4(17) . . ? C23A N1A U1 117.5(17) . . ? C28A N2A C24A 116(2) . . ? C28A N2A U1 118.3(16) . . ? C24A N2A U1 125.9(18) . . ? C23B N1B C19B 114(2) . . ? C23B N1B U2 115.3(16) . . ? C19B N1B U2 130.3(17) . . ? C24B N2B C28B 117(2) . . ? C24B N2B U2 119.5(16) . . ? C28B N2B U2 123.1(18) . . ? C23C N1C C19C 113(2) . . ? C23C N1C U3 117.3(14) . . ? C19C N1C U3 128.8(19) . . ? C28C N2C C24C 120(2) . . ? C28C N2C U3 116.0(17) . . ? C24C N2C U3 124.1(18) . . ? C5B C1B C2B 105(3) . . ? C5B C1B C6B 127(2) . . ? C2B C1B C6B 127(3) . . ? C2A C1A C6A 127(3) . . ? C2A C1A C5A 107(3) . . ? C6A C1A C5A 125(3) . . ? C2C C1C C5C 108(3) . . ? C2C C1C C6C 124(3) . . ? C5C C1C C6C 125(3) . . ? C1C C2C C3C 106(3) . . ? C3B C2B C1B 107(3) . . ? C1A C2A C3A 107(3) . . ? C4B C3B C2B 109(3) . . ? C4A C3A C2A 108(3) . . ? C4C C3C C2C 111(3) . . ? C3C C4C C5C 107(3) . . ? C3B C4B C5B 110(3) . . ? C5A C4A C3A 112(3) . . ? C1C C5C C4C 108(2) . . ? C4B C5B C1B 109(3) . . ? C4A C5A C1A 105(3) . . ? C7B C6B C9B 113(3) . . ? C7B C6B C1B 109(2) . . ? C9B C6B C1B 109(2) . . ? C7B C6B C8B 108(2) . . ? C9B C6B C8B 108(2) . . ? C1B C6B C8B 109(2) . . ? C1A C6A C9A 110(3) . . ? C1A C6A C7A 109(3) . . ? C9A C6A C7A 112(3) . . ? C1A C6A C8A 111(2) . . ? C9A C6A C8A 108(3) . . ? C7A C6A C8A 106(2) . . ? C9C C6C C1C 108(2) . . ? C9C C6C C8C 112(2) . . ? C1C C6C C8C 109(2) . . ? C9C C6C C7C 109(3) . . ? C1C C6C C7C 109(2) . . ? C8C C6C C7C 109(2) . . ? C14C C10C C11C 105(2) . . ? C14C C10C C15C 128(2) . . ? C11C C10C C15C 126(3) . . ? C11A C10A C14A 102(2) . . ? C11A C10A C15A 124(3) . . ? C14A C10A C15A 133(3) . . ? C11B C10B C14B 106(3) . . ? C11B C10B C15B 126(2) . . ? C14B C10B C15B 126(2) . . ? C10A C11A C12A 111(3) . . ? C10B C11B C12B 113(3) . . ? C12C C11C C10C 110(3) . . ? C13A C12A C11A 106(3) . . ? C11B C12B C13B 104(3) . . ? C13C C12C C11C 108(3) . . ? C12A C13A C14A 109(3) . . ? C14B C13B C12B 110(3) . . ? C12C C13C C14C 110(3) . . ? C10C C14C C13C 108(2) . . ? C13A C14A C10A 111(2) . . ? C13B C14B C10B 107(3) . . ? C17B C15B C16B 113(2) . . ? C17B C15B C18B 112(2) . . ? C16B C15B C18B 109(2) . . ? C17B C15B C10B 109.1(19) . . ? C16B C15B C10B 109(2) . . ? C18B C15B C10B 105(2) . . ? C16C C15C C10C 111(3) . . ? C16C C15C C17C 111(2) . . ? C10C C15C C17C 108(2) . . ? C16C C15C C18C 112(3) . . ? C10C C15C C18C 104(2) . . ? C17C C15C C18C 110(3) . . ? C10A C15A C18A 113(2) . . ? C10A C15A C16A 108(3) . . ? C18A C15A C16A 111(2) . . ? C10A C15A C17A 109(3) . . ? C18A C15A C17A 110(2) . . ? C16A C15A C17A 105(2) . . ? C20C C19C N1C 122(3) . . ? N1A C19A C20A 124(3) . . ? C20B C19B N1B 124(3) . . ? C21C C20C C19C 122(3) . . ? C21A C20A C19A 121(3) . . ? C19B C20B C21B 121(3) . . ? C20B C21B C22B 116(3) . . ? C20A C21A C22A 115(3) . . ? C20C C21C C22C 123(3) . . ? C23A C22A C21A 120(3) . . ? C21B C22B C23B 121(3) . . ? C21C C22C C23C 115(3) . . ? N1C C23C C22C 124(2) . . ? N1A C23A C22A 125(3) . . ? N1B C23B C22B 123(2) . . ? N2C C24C C25C 122(3) . . ? N2A C24A C25A 123(3) . . ? C25B C24B N2B 125(3) . . ? C24A C25A C26A 119(3) . . ? C24B C25B C26B 117(3) . . ? C26C C25C C24C 119(3) . . ? C27B C26B C25B 118(3) . . ? C27A C26A C25A 119(3) . . ? C25C C26C C27C 120(3) . . ? C26A C27A C28A 118(3) . . ? C26B C27B C28B 123(3) . . ? C28C C27C C26C 115(3) . . ? N2B C28B C27B 120(3) . . ? N2A C28A C27A 126(2) . . ? N2C C28C C27C 124(3) . . ?