Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Berthet, Jean-Claude' ; CEA/Saclay,DSM/DRECAM/SCM Bat. 125 91191 Gif-sur-Yvette Cedex France ; 'Miquel, Yannick' ; CEA/Saclay,DSM/DRECAM/SCM Bat. 125 91191 Gif-sur-Yvette Cedex France ; 'Nierlich, Martine' ; CEA/Saclay,DSM/DRECAM/SCM Bat. 125 91191 Gif-sur-Yvette Cedex France ; 'Thuery, Pierre' ; CEA/Saclay, DSM/DRECAM/SCM Bat. 125 91191 Gif-sur-Yvette Cedex France ; 'Madic, Charles' ; CEA/Saclay,DEN 91191 Gif-sur-Yvette Cedex France ; 'Ephritikhine, Michel' ; CEA/Saclay, DSM/DRECAM/SCM Bat. 125 91191 Gif-sur-Yvette Cedex France ; _publ_contact_author_name 'Dr Michel Ephritikhine' _publ_contact_author_address ; CEA/Saclay, SCM Bat. 125 91191 Gif-sur-Yvette Cedex France ; _publ_contact_author_email EPHRI@DRECAM.CEA.FR _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in Dalton Trans. ; _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The affinity and selectivity of the terdentate nitrogen ligands 2,2':6',2"- terpyridine and 2,6-bis(5,6-dialkyl-1,2,4-triazin-3-yl)pyridine towards trivalent lanthanide (La, Ce, Nd) and uranium ions viewed from the crystal structures of the 1:3 complexes. ; data_1.2MeCN _database_code_CSD 181672 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H39 I3 La N11' _chemical_formula_weight 1301.52 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' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 19.107(4) _cell_length_b 16.659(3) _cell_length_c 14.724(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4686.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 29196 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 2.935 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.761 _exptl_absorpt_process_details 'MULABS in PLATON;Spek,1998' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10s exposure by frame.The crystal to detector distance was 30mm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f rotation scans with 2\%steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29196 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 24.72 _reflns_number_total 3941 _reflns_number_gt 3320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms (except H atoms of solvent molecules) were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. ; _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^)+(0.0280P)^2^+4.5124P] 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 3941 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0624 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.803 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.100 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 0.5000 -0.250787(17) 0.7500 0.01431(9) Uani 1 2 d S . . I1 I 0.2500 0.5000 1.28154(2) 0.02761(11) Uani 1 2 d S . . I2 I 0.264882(14) 0.134843(15) 0.983790(18) 0.02742(9) Uani 1 1 d . . . N1 N 0.58547(16) -0.29735(18) 0.88056(19) 0.0180(7) Uani 1 1 d . . . N2 N 0.49357(15) -0.17508(17) 0.9106(2) 0.0168(7) Uani 1 1 d . . . N3 N 0.41195(16) -0.12845(18) 0.76693(19) 0.0192(7) Uani 1 1 d . . . N4 N 0.41077(16) -0.33082(17) 0.8618(2) 0.0188(7) Uani 1 1 d . . . N5 N 0.5000 -0.4122(3) 0.7500 0.0182(10) Uani 1 2 d S . . N6 N 0.0977(2) 0.2455(2) 1.2294(2) 0.0399(10) Uani 1 1 d . . . C1 C 0.6327(2) -0.3553(2) 0.8640(3) 0.0220(9) Uani 1 1 d . . . H1A H 0.6385 -0.3723 0.8042 0.026 Uiso 1 1 calc R . . C2 C 0.6729(2) -0.3910(2) 0.9298(3) 0.0244(9) Uani 1 1 d . . . H2A H 0.7055 -0.4303 0.9148 0.029 Uiso 1 1 calc R . . C3 C 0.6639(2) -0.3671(2) 1.0191(3) 0.0269(9) Uani 1 1 d . . . H3A H 0.6898 -0.3904 1.0656 0.032 Uiso 1 1 calc R . . C4 C 0.6151(2) -0.3073(2) 1.0373(3) 0.0243(9) Uani 1 1 d . . . H4A H 0.6081 -0.2904 1.0968 0.029 Uiso 1 1 calc R . . C5 C 0.57684(19) -0.2726(2) 0.9679(2) 0.0184(8) Uani 1 1 d . . . C6 C 0.52703(19) -0.2061(2) 0.9838(3) 0.0188(8) Uani 1 1 d . . . C7 C 0.5150(2) -0.1768(2) 1.0710(3) 0.0268(9) Uani 1 1 d . . . H7A H 0.5379 -0.1993 1.1205 0.032 Uiso 1 1 calc R . . C8 C 0.4690(2) -0.1143(3) 1.0833(3) 0.0302(10) Uani 1 1 d . . . H8A H 0.4605 -0.0943 1.1412 0.036 Uiso 1 1 calc R . . C9 C 0.4352(2) -0.0812(2) 1.0088(3) 0.0261(9) Uani 1 1 d . . . H9A H 0.4039 -0.0389 1.0159 0.031 Uiso 1 1 calc R . . C10 C 0.4493(2) -0.1128(2) 0.9228(3) 0.0214(8) Uani 1 1 d . . . C11 C 0.41221(19) -0.0814(2) 0.8419(3) 0.0193(8) Uani 1 1 d . . . C12 C 0.3782(2) -0.0076(2) 0.8438(3) 0.0258(9) Uani 1 1 d . . . H12A H 0.3796 0.0243 0.8956 0.031 Uiso 1 1 calc R . . C13 C 0.3425(2) 0.0175(2) 0.7678(3) 0.0287(10) Uani 1 1 d . . . H13A H 0.3199 0.0669 0.7678 0.034 Uiso 1 1 calc R . . C14 C 0.3403(2) -0.0304(2) 0.6916(3) 0.0235(9) Uani 1 1 d . . . H14A H 0.3157 -0.0147 0.6401 0.028 Uiso 1 1 calc R . . C15 C 0.37580(19) -0.1024(2) 0.6941(2) 0.0198(8) Uani 1 1 d . . . H15A H 0.3747 -0.1348 0.6427 0.024 Uiso 1 1 calc R . . C16 C 0.36968(19) -0.2903(2) 0.9195(3) 0.0211(8) Uani 1 1 d . . . H16A H 0.3540 -0.2398 0.9022 0.025 Uiso 1 1 calc R . . C17 C 0.3490(2) -0.3195(2) 1.0041(3) 0.0258(9) Uani 1 1 d . . . H17A H 0.3198 -0.2896 1.0417 0.031 Uiso 1 1 calc R . . C18 C 0.3730(2) -0.3940(3) 1.0302(3) 0.0295(10) Uani 1 1 d . . . H18A H 0.3624 -0.4142 1.0875 0.035 Uiso 1 1 calc R . . C19 C 0.4130(2) -0.4382(2) 0.9706(3) 0.0261(9) Uani 1 1 d . . . H19A H 0.4288 -0.4890 0.9869 0.031 Uiso 1 1 calc R . . C20 C 0.42967(19) -0.4067(2) 0.8862(2) 0.0183(8) Uani 1 1 d . . . C21 C 0.46715(19) -0.4537(2) 0.8167(3) 0.0204(8) Uani 1 1 d . . . C22 C 0.4660(2) -0.5375(2) 0.8172(3) 0.0301(10) Uani 1 1 d . . . H22A H 0.4422 -0.5649 0.8629 0.036 Uiso 1 1 calc R . . C23 C 0.5000 -0.5794(3) 0.7500 0.0356(16) Uani 1 2 d S . . H23A H 0.5000 -0.6352 0.7500 0.043 Uiso 1 2 calc SR . . C24 C 0.1571(2) 0.2464(2) 1.2323(2) 0.0270(10) Uani 1 1 d . . . C25 C 0.2333(2) 0.2467(3) 1.2389(3) 0.0378(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La 0.01588(16) 0.01460(15) 0.01243(15) 0.000 0.00044(12) 0.000 I1 0.0325(2) 0.0275(2) 0.0228(2) 0.000 0.000 0.00218(16) I2 0.02896(16) 0.02433(14) 0.02896(15) -0.00251(12) -0.00413(11) 0.00177(11) N1 0.0190(17) 0.0198(16) 0.0153(16) 0.0005(14) -0.0010(13) 0.0003(13) N2 0.0175(17) 0.0179(16) 0.0150(15) -0.0005(13) -0.0013(13) -0.0026(13) N3 0.0188(17) 0.0203(16) 0.0184(17) -0.0001(14) 0.0023(13) 0.0002(13) N4 0.0204(18) 0.0197(16) 0.0165(16) -0.0038(14) -0.0015(13) -0.0021(13) N5 0.017(2) 0.020(2) 0.018(2) 0.000 -0.0031(18) 0.000 N6 0.036(3) 0.056(3) 0.028(2) -0.0044(18) 0.0050(17) 0.002(2) C1 0.021(2) 0.025(2) 0.020(2) -0.0014(17) 0.0000(16) -0.0046(16) C2 0.023(2) 0.022(2) 0.028(2) 0.0051(18) -0.0023(17) 0.0033(16) C3 0.027(2) 0.029(2) 0.024(2) 0.0068(19) -0.0068(18) -0.0013(17) C4 0.030(2) 0.026(2) 0.017(2) 0.0031(17) -0.0002(17) -0.0015(17) C5 0.020(2) 0.0191(19) 0.016(2) -0.0029(16) 0.0003(15) -0.0061(15) C6 0.016(2) 0.0208(19) 0.020(2) -0.0005(17) 0.0023(15) -0.0053(15) C7 0.035(3) 0.035(2) 0.0107(19) 0.0022(17) -0.0019(17) 0.0002(19) C8 0.034(2) 0.038(2) 0.019(2) -0.0088(19) 0.0018(18) 0.0042(19) C9 0.026(2) 0.026(2) 0.026(2) -0.0082(18) 0.0037(18) 0.0006(17) C10 0.018(2) 0.025(2) 0.021(2) -0.0028(17) 0.0043(16) -0.0039(16) C11 0.014(2) 0.022(2) 0.021(2) -0.0038(17) 0.0019(16) -0.0024(15) C12 0.030(2) 0.0179(19) 0.029(2) -0.0079(18) 0.0011(18) 0.0027(17) C13 0.032(3) 0.016(2) 0.038(3) -0.0009(19) 0.0003(19) 0.0050(17) C14 0.021(2) 0.022(2) 0.028(2) 0.0060(18) -0.0007(17) 0.0047(16) C15 0.019(2) 0.0212(19) 0.019(2) 0.0005(17) 0.0000(15) 0.0012(16) C16 0.017(2) 0.021(2) 0.025(2) -0.0024(17) -0.0012(16) -0.0011(15) C17 0.023(2) 0.032(2) 0.022(2) -0.0029(18) 0.0049(17) -0.0028(17) C18 0.034(2) 0.033(2) 0.022(2) 0.0049(19) 0.0045(18) -0.0008(19) C19 0.027(2) 0.023(2) 0.029(2) 0.0040(18) 0.0037(18) 0.0031(17) C20 0.014(2) 0.0175(19) 0.023(2) 0.0014(17) 0.0005(15) -0.0033(15) C21 0.013(2) 0.024(2) 0.024(2) 0.0031(17) 0.0007(15) 0.0005(15) C22 0.032(3) 0.022(2) 0.036(3) 0.0057(19) 0.0087(19) -0.0038(18) C23 0.045(4) 0.014(3) 0.049(4) 0.000 0.013(3) 0.000 C24 0.036(3) 0.031(2) 0.014(2) -0.0004(17) 0.0050(17) -0.003(2) C25 0.031(3) 0.039(3) 0.043(3) -0.001(2) 0.003(2) -0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La N1 2.639(3) 3_656 ? La N1 2.639(3) . ? La N3 2.654(3) 3_656 ? La N3 2.654(3) . ? La N2 2.683(3) . ? La N2 2.683(3) 3_656 ? La N5 2.689(4) . ? La N4 2.719(3) . ? La N4 2.719(3) 3_656 ? N1 C1 1.345(5) . ? N1 C5 1.360(4) . ? N2 C10 1.351(5) . ? N2 C6 1.356(5) . ? N3 C15 1.347(5) . ? N3 C11 1.354(5) . ? N4 C16 1.339(5) . ? N4 C20 1.363(5) . ? N5 C21 1.356(4) 3_656 ? N5 C21 1.356(4) . ? N6 C24 1.136(6) . ? C1 C2 1.372(5) . ? C2 C3 1.384(6) . ? C3 C4 1.391(6) . ? C4 C5 1.382(5) . ? C5 C6 1.479(5) . ? C6 C7 1.392(5) . ? C7 C8 1.375(6) . ? C8 C9 1.386(6) . ? C9 C10 1.397(5) . ? C10 C11 1.481(5) . ? C11 C12 1.391(5) . ? C12 C13 1.376(6) . ? C13 C14 1.379(6) . ? C14 C15 1.377(5) . ? C16 C17 1.393(5) . ? C17 C18 1.379(6) . ? C18 C19 1.376(5) . ? C19 C20 1.386(5) . ? C20 C21 1.474(5) . ? C21 C22 1.396(5) . ? C22 C23 1.375(5) . ? C23 C22 1.375(5) 3_656 ? C24 C25 1.459(7) . ? 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 La N1 145.81(13) 3_656 . ? N1 La N3 123.33(9) 3_656 3_656 ? N1 La N3 84.37(9) . 3_656 ? N1 La N3 84.37(9) 3_656 . ? N1 La N3 123.33(9) . . ? N3 La N3 79.69(13) 3_656 . ? N1 La N2 138.76(9) 3_656 . ? N1 La N2 61.60(9) . . ? N3 La N2 75.58(9) 3_656 . ? N3 La N2 61.79(9) . . ? N1 La N2 61.60(9) 3_656 3_656 ? N1 La N2 138.76(9) . 3_656 ? N3 La N2 61.79(9) 3_656 3_656 ? N3 La N2 75.58(9) . 3_656 ? N2 La N2 123.93(12) . 3_656 ? N1 La N5 72.90(6) 3_656 . ? N1 La N5 72.91(6) . . ? N3 La N5 140.15(7) 3_656 . ? N3 La N5 140.16(7) . . ? N2 La N5 118.03(6) . . ? N2 La N5 118.03(6) 3_656 . ? N1 La N4 84.77(9) 3_656 . ? N1 La N4 78.63(9) . . ? N3 La N4 146.17(9) 3_656 . ? N3 La N4 85.54(9) . . ? N2 La N4 70.62(9) . . ? N2 La N4 142.44(9) 3_656 . ? N5 La N4 60.64(6) . . ? N1 La N4 78.63(9) 3_656 3_656 ? N1 La N4 84.77(9) . 3_656 ? N3 La N4 85.54(9) 3_656 3_656 ? N3 La N4 146.17(9) . 3_656 ? N2 La N4 142.44(9) . 3_656 ? N2 La N4 70.62(9) 3_656 3_656 ? N5 La N4 60.64(6) . 3_656 ? N4 La N4 121.28(13) . 3_656 ? C1 N1 C5 118.1(3) . . ? C10 N2 C6 118.9(3) . . ? C15 N3 C11 117.6(3) . . ? C16 N4 C20 117.0(3) . . ? C21 N5 C21 118.6(4) 3_656 . ? N1 C1 C2 123.9(4) . . ? C1 C2 C3 118.5(4) . . ? C2 C3 C4 118.2(4) . . ? C5 C4 C3 120.7(4) . . ? N1 C5 C4 120.5(3) . . ? N1 C5 C6 117.1(3) . . ? C4 C5 C6 122.4(3) . . ? N2 C6 C7 121.4(3) . . ? N2 C6 C5 117.6(3) . . ? C7 C6 C5 121.0(3) . . ? C8 C7 C6 119.5(4) . . ? C7 C8 C9 119.7(4) . . ? C8 C9 C10 118.5(4) . . ? N2 C10 C9 122.0(4) . . ? N2 C10 C11 117.6(3) . . ? C9 C10 C11 120.2(3) . . ? N3 C11 C12 121.8(3) . . ? N3 C11 C10 116.9(3) . . ? C12 C11 C10 121.3(3) . . ? C13 C12 C11 119.0(4) . . ? C12 C13 C14 120.1(4) . . ? C15 C14 C13 117.9(4) . . ? N3 C15 C14 123.7(4) . . ? N4 C16 C17 123.9(4) . . ? C18 C17 C16 117.9(4) . . ? C19 C18 C17 119.2(4) . . ? C18 C19 C20 119.9(4) . . ? N4 C20 C19 121.7(3) . . ? N4 C20 C21 116.0(3) . . ? C19 C20 C21 122.2(3) . . ? N5 C21 C22 121.5(4) . . ? N5 C21 C20 117.2(3) . . ? C22 C21 C20 121.3(3) . . ? C23 C22 C21 119.7(4) . . ? C22 C23 C22 119.0(5) . 3_656 ? N6 C24 C25 178.3(4) . . ? #===END data_2.2MeCN _database_code_CSD 181673 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H39 Ce I3 N11' _chemical_formula_weight 1302.73 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' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 19.149(4) _cell_length_b 16.626(3) _cell_length_c 14.709(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4682.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 29360 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2508 _exptl_absorpt_coefficient_mu 2.998 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.762 _exptl_absorpt_process_details 'MULABS in PLATON;Spek,1998' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f rotation scans with 2\%steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29360 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 24.72 _reflns_number_total 3946 _reflns_number_gt 3235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms (except H atoms of solvent molecules) were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH)times that of the parent atom. ; _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^)+(0.0377P)^2^+2.7386P] 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 3946 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.652 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.106 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 0.5000 -0.251193(18) 0.7500 0.01797(10) Uani 1 2 d S . . I1 I 0.2500 0.5000 1.28328(3) 0.03141(12) Uani 1 2 d S . . I2 I 0.265327(16) 0.134602(17) 0.98159(2) 0.03145(10) Uani 1 1 d . . . N1 N 0.58453(18) -0.2985(2) 0.8788(2) 0.0222(8) Uani 1 1 d . . . N2 N 0.49384(17) -0.17576(19) 0.9090(2) 0.0209(8) Uani 1 1 d . . . N3 N 0.41268(18) -0.1301(2) 0.7651(2) 0.0223(8) Uani 1 1 d . . . N4 N 0.41132(18) -0.32954(19) 0.8613(2) 0.0219(8) Uani 1 1 d . . . N5 N 0.5000 -0.4116(3) 0.7500 0.0213(11) Uani 1 2 d S . . N6 N 0.0972(3) 0.2462(3) 1.2304(3) 0.0441(11) Uani 1 1 d . . . C1 C 0.6325(2) -0.3565(2) 0.8617(3) 0.0233(9) Uani 1 1 d . . . H1A H 0.6384 -0.3737 0.8021 0.028 Uiso 1 1 calc R . . C2 C 0.6726(2) -0.3909(3) 0.9284(3) 0.0289(10) Uani 1 1 d . . . H2A H 0.7054 -0.4300 0.9136 0.035 Uiso 1 1 calc R . . C3 C 0.6639(2) -0.3672(3) 1.0171(3) 0.0288(10) Uani 1 1 d . . . H3A H 0.6899 -0.3908 1.0633 0.035 Uiso 1 1 calc R . . C4 C 0.6159(2) -0.3078(3) 1.0366(3) 0.0292(10) Uani 1 1 d . . . H4A H 0.6097 -0.2903 1.0961 0.035 Uiso 1 1 calc R . . C5 C 0.5767(2) -0.2739(2) 0.9661(3) 0.0234(9) Uani 1 1 d . . . C6 C 0.5269(2) -0.2070(2) 0.9832(3) 0.0231(9) Uani 1 1 d . . . C7 C 0.5151(2) -0.1771(3) 1.0707(3) 0.0304(10) Uani 1 1 d . . . H7A H 0.5383 -0.1991 1.1204 0.037 Uiso 1 1 calc R . . C8 C 0.4686(3) -0.1148(3) 1.0824(3) 0.0348(11) Uani 1 1 d . . . H8A H 0.4596 -0.0949 1.1404 0.042 Uiso 1 1 calc R . . C9 C 0.4352(2) -0.0818(3) 1.0074(3) 0.0297(11) Uani 1 1 d . . . H9A H 0.4041 -0.0393 1.0144 0.036 Uiso 1 1 calc R . . C10 C 0.4491(2) -0.1135(2) 0.9215(3) 0.0215(9) Uani 1 1 d . . . C11 C 0.4123(2) -0.0821(2) 0.8398(3) 0.0228(9) Uani 1 1 d . . . C12 C 0.3783(2) -0.0078(3) 0.8414(3) 0.0299(10) Uani 1 1 d . . . H12A H 0.3800 0.0245 0.8930 0.036 Uiso 1 1 calc R . . C13 C 0.3424(2) 0.0169(3) 0.7660(3) 0.0319(11) Uani 1 1 d . . . H13A H 0.3195 0.0662 0.7660 0.038 Uiso 1 1 calc R . . C14 C 0.3405(2) -0.0313(3) 0.6898(3) 0.0271(10) Uani 1 1 d . . . H14A H 0.3159 -0.0159 0.6382 0.033 Uiso 1 1 calc R . . C15 C 0.3763(2) -0.1035(3) 0.6928(3) 0.0263(10) Uani 1 1 d . . . H15A H 0.3751 -0.1360 0.6413 0.032 Uiso 1 1 calc R . . C16 C 0.3699(2) -0.2897(3) 0.9196(3) 0.0269(10) Uani 1 1 d . . . H16A H 0.3541 -0.2390 0.9025 0.032 Uiso 1 1 calc R . . C17 C 0.3490(2) -0.3190(3) 1.0033(3) 0.0296(11) Uani 1 1 d . . . H17A H 0.3195 -0.2890 1.0404 0.036 Uiso 1 1 calc R . . C18 C 0.3726(2) -0.3932(3) 1.0309(3) 0.0312(11) Uani 1 1 d . . . H18A H 0.3619 -0.4131 1.0883 0.037 Uiso 1 1 calc R . . C19 C 0.4129(2) -0.4376(3) 0.9706(3) 0.0290(10) Uani 1 1 d . . . H19A H 0.4283 -0.4888 0.9865 0.035 Uiso 1 1 calc R . . C20 C 0.4302(2) -0.4055(2) 0.8863(3) 0.0238(9) Uani 1 1 d . . . C21 C 0.4676(2) -0.4532(3) 0.8166(3) 0.0259(10) Uani 1 1 d . . . C22 C 0.4664(2) -0.5370(3) 0.8178(4) 0.0340(12) Uani 1 1 d . . . H22A H 0.4432 -0.5645 0.8639 0.041 Uiso 1 1 calc R . . C23 C 0.5000 -0.5785(4) 0.7500 0.0335(16) Uani 1 2 d S . . H23A H 0.5000 -0.6345 0.7500 0.040 Uiso 1 2 calc SR . . C24 C 0.1569(3) 0.2461(3) 1.2326(3) 0.0318(11) Uani 1 1 d . . . C25 C 0.2331(3) 0.2470(3) 1.2376(4) 0.0402(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.01867(17) 0.01763(17) 0.01761(18) 0.000 0.00035(14) 0.000 I1 0.0351(2) 0.0308(2) 0.0284(2) 0.000 0.000 0.00227(18) I2 0.03221(18) 0.02766(17) 0.03447(18) -0.00245(13) -0.00430(13) 0.00228(12) N1 0.0213(19) 0.0264(19) 0.019(2) 0.0022(15) -0.0006(15) -0.0014(15) N2 0.0196(18) 0.0214(18) 0.0216(19) -0.0013(14) 0.0013(15) -0.0040(14) N3 0.0196(18) 0.0242(19) 0.023(2) 0.0003(15) 0.0023(15) 0.0020(15) N4 0.0212(19) 0.0193(18) 0.025(2) -0.0007(15) 0.0013(15) -0.0004(14) N5 0.016(3) 0.021(3) 0.027(3) 0.000 -0.001(2) 0.000 N6 0.038(3) 0.062(3) 0.032(3) 0.000(2) 0.004(2) 0.003(2) C1 0.023(2) 0.023(2) 0.024(2) -0.0033(18) 0.0002(18) -0.0003(18) C2 0.022(2) 0.028(2) 0.037(3) 0.004(2) -0.005(2) 0.0000(18) C3 0.030(2) 0.030(2) 0.026(2) 0.009(2) -0.007(2) -0.002(2) C4 0.035(3) 0.029(2) 0.024(3) 0.0016(19) -0.004(2) -0.003(2) C5 0.025(2) 0.020(2) 0.026(3) 0.0019(18) -0.0008(18) -0.0070(18) C6 0.021(2) 0.025(2) 0.023(2) 0.0016(19) 0.0049(18) -0.0030(17) C7 0.031(3) 0.041(3) 0.019(2) -0.001(2) 0.000(2) -0.003(2) C8 0.038(3) 0.041(3) 0.026(3) -0.011(2) 0.005(2) 0.004(2) C9 0.031(3) 0.024(2) 0.034(3) -0.0065(19) 0.003(2) 0.0027(19) C10 0.023(2) 0.018(2) 0.024(2) -0.0043(17) 0.0033(18) -0.0030(17) C11 0.019(2) 0.023(2) 0.027(2) 0.0002(18) 0.0057(19) -0.0021(17) C12 0.028(2) 0.025(2) 0.037(3) -0.006(2) 0.001(2) 0.0020(19) C13 0.025(2) 0.026(3) 0.045(3) 0.003(2) -0.001(2) 0.0044(19) C14 0.027(2) 0.030(2) 0.024(3) 0.007(2) 0.0041(19) 0.0021(19) C15 0.022(2) 0.029(2) 0.029(3) -0.0042(19) 0.0022(19) 0.0042(19) C16 0.025(2) 0.021(2) 0.035(3) -0.0017(19) 0.000(2) -0.0012(18) C17 0.024(2) 0.033(3) 0.032(3) -0.008(2) 0.005(2) -0.0021(19) C18 0.034(3) 0.034(3) 0.026(3) 0.003(2) 0.005(2) 0.001(2) C19 0.028(2) 0.026(2) 0.033(3) 0.004(2) 0.001(2) -0.0015(19) C20 0.020(2) 0.022(2) 0.030(3) -0.0007(19) -0.0010(19) -0.0048(17) C21 0.020(2) 0.025(2) 0.033(3) 0.005(2) 0.0019(19) -0.0027(18) C22 0.033(3) 0.026(2) 0.043(3) 0.005(2) 0.008(2) -0.001(2) C23 0.042(4) 0.017(3) 0.041(4) 0.000 0.004(3) 0.000 C24 0.043(3) 0.033(3) 0.019(3) 0.0000(19) 0.008(2) 0.001(2) C25 0.031(3) 0.048(3) 0.041(3) 0.002(2) 0.000(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce N1 2.613(3) 3_656 ? Ce N1 2.613(3) . ? Ce N3 2.626(3) 3_656 ? Ce N3 2.626(3) . ? Ce N2 2.657(3) 3_656 ? Ce N2 2.657(3) . ? Ce N5 2.667(5) . ? Ce N4 2.695(3) 3_656 ? Ce N4 2.695(3) . ? N1 C1 1.354(5) . ? N1 C5 1.356(5) . ? N2 C10 1.356(5) . ? N2 C6 1.364(6) . ? N3 C15 1.346(6) . ? N3 C11 1.359(5) . ? N4 C16 1.343(6) . ? N4 C20 1.365(5) . ? N5 C21 1.350(5) . ? N5 C21 1.350(5) 3_656 ? N6 C24 1.144(7) . ? C1 C2 1.370(6) . ? C2 C3 1.373(7) . ? C3 C4 1.379(7) . ? C4 C5 1.398(6) . ? C5 C6 1.487(6) . ? C6 C7 1.398(6) . ? C7 C8 1.377(7) . ? C8 C9 1.388(7) . ? C9 C10 1.395(6) . ? C10 C11 1.487(6) . ? C11 C12 1.398(6) . ? C12 C13 1.368(7) . ? C13 C14 1.379(7) . ? C14 C15 1.383(6) . ? C16 C17 1.384(7) . ? C17 C18 1.376(6) . ? C18 C19 1.389(6) . ? C19 C20 1.390(6) . ? C20 C21 1.481(6) . ? C21 C22 1.393(6) . ? C22 C23 1.372(6) . ? C23 C22 1.372(6) 3_656 ? C24 C25 1.461(8) . ? 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 Ce N1 144.96(15) 3_656 . ? N1 Ce N3 124.34(11) 3_656 3_656 ? N1 Ce N3 84.11(11) . 3_656 ? N1 Ce N3 84.12(11) 3_656 . ? N1 Ce N3 124.34(11) . . ? N3 Ce N3 79.92(15) 3_656 . ? N1 Ce N2 62.06(10) 3_656 3_656 ? N1 Ce N2 138.84(10) . 3_656 ? N3 Ce N2 62.33(10) 3_656 3_656 ? N3 Ce N2 74.97(10) . 3_656 ? N1 Ce N2 138.84(10) 3_656 . ? N1 Ce N2 62.05(10) . . ? N3 Ce N2 74.97(10) 3_656 . ? N3 Ce N2 62.33(10) . . ? N2 Ce N2 123.67(14) 3_656 . ? N1 Ce N5 72.48(7) 3_656 . ? N1 Ce N5 72.48(7) . . ? N3 Ce N5 140.04(8) 3_656 . ? N3 Ce N5 140.04(8) . . ? N2 Ce N5 118.17(7) 3_656 . ? N2 Ce N5 118.17(7) . . ? N1 Ce N4 78.72(11) 3_656 3_656 ? N1 Ce N4 84.52(11) . 3_656 ? N3 Ce N4 85.30(10) 3_656 3_656 ? N3 Ce N4 145.39(10) . 3_656 ? N2 Ce N4 70.44(10) 3_656 3_656 ? N2 Ce N4 142.29(10) . 3_656 ? N5 Ce N4 61.09(7) . 3_656 ? N1 Ce N4 84.52(11) 3_656 . ? N1 Ce N4 78.73(11) . . ? N3 Ce N4 145.39(10) 3_656 . ? N3 Ce N4 85.30(10) . . ? N2 Ce N4 142.29(10) 3_656 . ? N2 Ce N4 70.44(10) . . ? N5 Ce N4 61.09(7) . . ? N4 Ce N4 122.19(14) 3_656 . ? C1 N1 C5 117.6(4) . . ? C10 N2 C6 118.4(4) . . ? C15 N3 C11 116.3(4) . . ? C16 N4 C20 116.2(4) . . ? C21 N5 C21 118.3(5) . 3_656 ? N1 C1 C2 123.0(4) . . ? C1 C2 C3 119.5(4) . . ? C2 C3 C4 118.9(4) . . ? C3 C4 C5 119.4(4) . . ? N1 C5 C4 121.5(4) . . ? N1 C5 C6 117.2(4) . . ? C4 C5 C6 121.3(4) . . ? N2 C6 C7 121.7(4) . . ? N2 C6 C5 116.5(4) . . ? C7 C6 C5 121.7(4) . . ? C8 C7 C6 119.2(4) . . ? C7 C8 C9 119.7(4) . . ? C8 C9 C10 118.9(4) . . ? N2 C10 C9 122.1(4) . . ? N2 C10 C11 117.3(4) . . ? C9 C10 C11 120.6(4) . . ? N3 C11 C12 122.4(4) . . ? N3 C11 C10 116.4(3) . . ? C12 C11 C10 121.2(4) . . ? C13 C12 C11 119.1(4) . . ? C12 C13 C14 119.9(4) . . ? C13 C14 C15 117.8(4) . . ? N3 C15 C14 124.5(4) . . ? N4 C16 C17 124.4(4) . . ? C18 C17 C16 118.9(4) . . ? C17 C18 C19 118.1(4) . . ? C18 C19 C20 119.9(4) . . ? N4 C20 C19 122.2(4) . . ? N4 C20 C21 116.0(4) . . ? C19 C20 C21 121.8(4) . . ? N5 C21 C22 121.9(4) . . ? N5 C21 C20 116.7(4) . . ? C22 C21 C20 121.3(4) . . ? C23 C22 C21 119.1(5) . . ? C22 C23 C22 119.6(6) 3_656 . ? N6 C24 C25 178.6(5) . . ? #===END data_2.3MeCN _database_code_CSD 181674 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H42 Ce I3 N12' _chemical_formula_weight 1343.79 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 trigonal _symmetry_space_group_name_H-M R32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 12.6180(18) _cell_length_b 12.6180(18) _cell_length_c 27.903(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3847.4(11) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7985 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1947 _exptl_absorpt_coefficient_mu 2.740 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details 'MULABS in PLATON;Spek,1998' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f rotation scans with 2\%steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7985 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 24.69 _reflns_number_total 1362 _reflns_number_gt 1316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms (except H atoms of solvent molecules, CH3CN) were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. The badly resolved solvent molecules were found disordered over two positions refined with 0.5 occupation factors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+26.9124P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 1362 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.807 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.108 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 0.6667 0.3333 0.8333 0.0180(2) Uani 1 6 d S . . I I 1.0000 0.30898(6) 1.0000 0.0415(2) Uani 1 2 d S . . N1 N 0.6879(6) 0.1818(5) 0.89289(18) 0.0323(13) Uani 1 1 d . . . N2 N 0.8786(6) 0.3333 0.8333 0.0202(15) Uani 1 2 d S . . C1 C 0.5959(7) 0.1060(7) 0.9204(2) 0.0348(15) Uani 1 1 d . . . H1A H 0.5355 0.1253 0.9276 0.042 Uiso 1 1 calc R . . C2 C 0.5848(8) -0.0006(7) 0.9391(3) 0.0393(17) Uani 1 1 d . . . H2A H 0.5177 -0.0508 0.9582 0.047 Uiso 1 1 calc R . . C3 C 0.6694(7) -0.0327(6) 0.9301(3) 0.0357(16) Uani 1 1 d . . . H3A H 0.6602 -0.1061 0.9416 0.043 Uiso 1 1 calc R . . C4 C 0.7735(8) 0.0486(8) 0.9026(3) 0.0424(18) Uani 1 1 d . . . H4A H 0.8361 0.0316 0.8967 0.051 Uiso 1 1 calc R . . C5 C 0.7792(7) 0.1554(7) 0.8845(2) 0.0338(15) Uani 1 1 d . . . C6 C 0.8880(6) 0.2465(6) 0.8576(2) 0.0309(15) Uani 1 1 d . . . C7 C 0.9978(7) 0.2456(9) 0.8585(3) 0.046(2) Uani 1 1 d . . . H7A H 1.0042 0.1863 0.8760 0.055 Uiso 1 1 calc R . . C8 C 1.0969(8) 0.3333 0.8333 0.048(3) Uani 1 2 d S . . H8A H 1.1706 0.3333 0.8333 0.058 Uiso 1 2 calc SR . . C9 C 1.0000 0.0000 0.9728(6) 0.051(3) Uani 1 3 d S . . N3 N 1.0000 0.0000 0.9278(9) 0.050(5) Uani 0.50 3 d SP . . N4B N 1.0000 0.0000 0.8212(17) 0.068(8) Uani 0.50 3 d SP . . C11 C 1.0000 0.0000 0.7859(13) 0.102(9) Uani 1 3 d S . . C10 C 1.0000 0.0000 0.739(2) 0.141(17) Uani 1 3 d S . . N4A N 1.0000 0.0000 0.6913(10) 0.058(7) Uani 0.50 3 d SP . . 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 0.0179(3) 0.0179(3) 0.0184(4) 0.000 0.000 0.00893(13) I 0.0497(5) 0.0423(3) 0.0351(4) -0.00210(16) -0.0042(3) 0.0248(2) N1 0.048(4) 0.036(3) 0.024(3) 0.000(2) -0.001(2) 0.030(3) N2 0.020(3) 0.018(3) 0.022(3) -0.002(3) -0.0008(14) 0.0088(17) C1 0.042(4) 0.033(4) 0.034(3) 0.005(3) 0.000(3) 0.023(3) C2 0.041(4) 0.035(4) 0.038(4) -0.001(3) -0.004(3) 0.016(4) C3 0.037(4) 0.031(4) 0.039(4) 0.006(3) -0.004(3) 0.018(4) C4 0.050(5) 0.035(4) 0.051(4) 0.008(3) 0.002(4) 0.028(4) C5 0.038(4) 0.039(4) 0.029(3) -0.001(3) -0.004(3) 0.023(3) C6 0.031(4) 0.040(4) 0.027(3) -0.001(3) 0.001(3) 0.021(3) C7 0.042(4) 0.069(6) 0.035(4) 0.013(4) -0.001(3) 0.034(4) C8 0.034(4) 0.082(9) 0.046(6) 0.021(6) 0.010(3) 0.041(5) C9 0.043(5) 0.043(5) 0.067(10) 0.000 0.000 0.021(2) N3 0.050(8) 0.050(8) 0.051(14) 0.000 0.000 0.025(4) N4B 0.057(11) 0.057(11) 0.09(2) 0.000 0.000 0.029(6) C11 0.105(14) 0.105(14) 0.097(18) 0.000 0.000 0.052(7) C10 0.057(9) 0.057(9) 0.31(6) 0.000 0.000 0.029(5) N4A 0.065(12) 0.065(12) 0.045(14) 0.000 0.000 0.032(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 Ce N1 2.646(5) 18_656 ? Ce N1 2.646(5) . ? Ce N1 2.646(5) 16_546 ? Ce N1 2.646(5) 17_556 ? Ce N1 2.646(5) 2_655 ? Ce N1 2.646(5) 3_665 ? Ce N2 2.674(7) . ? Ce N2 2.674(7) 3_665 ? Ce N2 2.674(7) 2_655 ? N1 C1 1.321(9) . ? N1 C5 1.370(9) . ? N2 C6 1.343(8) 17_556 ? N2 C6 1.343(8) . ? C1 C2 1.383(11) . ? C2 C3 1.342(11) . ? C3 C4 1.421(12) . ? C4 C5 1.407(11) . ? C5 C6 1.481(10) . ? C6 C7 1.391(11) . ? C7 C8 1.378(10) . ? C8 C7 1.378(10) 17_556 ? C9 N3 1.25(3) . ? C9 C9 1.52(3) 4_647 ? N4B C11 0.99(4) . ? C11 C10 1.30(6) . ? C10 N4A 1.34(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ce N1 78.7(2) 18_656 . ? N1 Ce N1 84.73(17) 18_656 16_546 ? N1 Ce N1 143.8(3) . 16_546 ? N1 Ce N1 84.72(17) 18_656 17_556 ? N1 Ce N1 124.9(3) . 17_556 ? N1 Ce N1 84.73(17) 16_546 17_556 ? N1 Ce N1 143.8(3) 18_656 2_655 ? N1 Ce N1 84.73(17) . 2_655 ? N1 Ce N1 124.9(3) 16_546 2_655 ? N1 Ce N1 78.7(2) 17_556 2_655 ? N1 Ce N1 124.9(3) 18_656 3_665 ? N1 Ce N1 84.73(17) . 3_665 ? N1 Ce N1 78.7(2) 16_546 3_665 ? N1 Ce N1 143.8(3) 17_556 3_665 ? N1 Ce N1 84.73(17) 2_655 3_665 ? N1 Ce N2 71.90(13) 18_656 . ? N1 Ce N2 62.45(13) . . ? N1 Ce N2 140.63(11) 16_546 . ? N1 Ce N2 62.45(13) 17_556 . ? N1 Ce N2 71.90(13) 2_655 . ? N1 Ce N2 140.63(11) 3_665 . ? N1 Ce N2 62.45(13) 18_656 3_665 ? N1 Ce N2 71.90(13) . 3_665 ? N1 Ce N2 71.90(13) 16_546 3_665 ? N1 Ce N2 140.63(12) 17_556 3_665 ? N1 Ce N2 140.64(12) 2_655 3_665 ? N1 Ce N2 62.45(13) 3_665 3_665 ? N2 Ce N2 119.999(2) . 3_665 ? N1 Ce N2 140.63(11) 18_656 2_655 ? N1 Ce N2 140.64(11) . 2_655 ? N1 Ce N2 62.45(13) 16_546 2_655 ? N1 Ce N2 71.90(13) 17_556 2_655 ? N1 Ce N2 62.45(13) 2_655 2_655 ? N1 Ce N2 71.90(13) 3_665 2_655 ? N2 Ce N2 119.999(5) . 2_655 ? N2 Ce N2 120.002(2) 3_665 2_655 ? C1 N1 C5 117.7(6) . . ? C6 N2 C6 120.4(8) 17_556 . ? N1 C1 C2 123.3(7) . . ? C3 C2 C1 121.0(8) . . ? C2 C3 C4 118.1(7) . . ? C5 C4 C3 118.2(7) . . ? N1 C5 C4 121.7(7) . . ? N1 C5 C6 117.6(6) . . ? C4 C5 C6 120.6(7) . . ? N2 C6 C7 120.8(7) . . ? N2 C6 C5 117.6(6) . . ? C7 C6 C5 121.6(7) . . ? C8 C7 C6 119.4(8) . . ? C7 C8 C7 119.2(10) 17_556 . ? N3 C9 C9 179.999(12) . 4_647 ? N4B C11 C10 180.00(3) . . ? C11 C10 N4A 180.000(16) . . ? #===END data_3.2MeCN _database_code_CSD 181675 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H39 I3 N11 Nd' _chemical_formula_weight 1306.85 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 orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 19.220(4) _cell_length_b 16.591(3) _cell_length_c 14.685(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4682.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 29212 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2516 _exptl_absorpt_coefficient_mu 3.134 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.460 _exptl_absorpt_correction_T_max 0.540 _exptl_absorpt_process_details 'MULABS in PLATON;Spek,1998' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f rotation scans with 2\%steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29212 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 24.72 _reflns_number_total 3953 _reflns_number_gt 3270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms (except H atoms of solvent molecules) were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. ; _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^)+(0.0303P)^2^+7.0862P] 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 3953 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.872 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.109 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 0.5000 -0.251746(18) 0.7500 0.01509(9) Uani 1 2 d S . . I1 I 0.2500 0.5000 1.28567(3) 0.02811(12) Uani 1 2 d S . . I2 I 0.266449(15) 0.134342(17) 0.97741(2) 0.02763(10) Uani 1 1 d . . . N1 N 0.58442(17) -0.2992(2) 0.8763(2) 0.0189(8) Uani 1 1 d . . . N2 N 0.49390(16) -0.17734(19) 0.9070(2) 0.0162(7) Uani 1 1 d . . . N3 N 0.41247(17) -0.1315(2) 0.7630(2) 0.0185(8) Uani 1 1 d . . . N4 N 0.41157(16) -0.3283(2) 0.8611(2) 0.0187(8) Uani 1 1 d . . . N5 N 0.5000 -0.4107(3) 0.7500 0.0184(11) Uani 1 2 d S . . N6 N 0.0969(2) 0.2456(3) 1.2312(3) 0.0413(11) Uani 1 1 d . . . C1 C 0.6320(2) -0.3570(2) 0.8592(3) 0.0210(9) Uani 1 1 d . . . H1A H 0.6379 -0.3739 0.7993 0.025 Uiso 1 1 calc R . . C2 C 0.6724(2) -0.3922(3) 0.9258(3) 0.0212(9) Uani 1 1 d . . . H2A H 0.7048 -0.4316 0.9108 0.025 Uiso 1 1 calc R . . C3 C 0.6639(2) -0.3681(3) 1.0149(3) 0.0271(10) Uani 1 1 d . . . H3A H 0.6900 -0.3914 1.0613 0.033 Uiso 1 1 calc R . . C4 C 0.6158(2) -0.3085(3) 1.0339(3) 0.0239(10) Uani 1 1 d . . . H4A H 0.6098 -0.2908 1.0935 0.029 Uiso 1 1 calc R . . C5 C 0.5764(2) -0.2751(3) 0.9644(3) 0.0200(9) Uani 1 1 d . . . C6 C 0.5266(2) -0.2078(2) 0.9812(3) 0.0194(9) Uani 1 1 d . . . C7 C 0.5153(2) -0.1783(3) 1.0685(3) 0.0293(11) Uani 1 1 d . . . H7A H 0.5384 -0.2004 1.1181 0.035 Uiso 1 1 calc R . . C8 C 0.4687(2) -0.1151(3) 1.0805(3) 0.0305(11) Uani 1 1 d . . . H8A H 0.4598 -0.0949 1.1384 0.037 Uiso 1 1 calc R . . C9 C 0.4360(2) -0.0826(3) 1.0056(3) 0.0256(10) Uani 1 1 d . . . H9A H 0.4050 -0.0400 1.0124 0.031 Uiso 1 1 calc R . . C10 C 0.4496(2) -0.1143(2) 0.9198(3) 0.0196(9) Uani 1 1 d . . . C11 C 0.4132(2) -0.0833(3) 0.8375(3) 0.0208(10) Uani 1 1 d . . . C12 C 0.3791(2) -0.0092(3) 0.8385(3) 0.0265(10) Uani 1 1 d . . . H12A H 0.3808 0.0231 0.8901 0.032 Uiso 1 1 calc R . . C13 C 0.3429(2) 0.0160(3) 0.7627(3) 0.0286(11) Uani 1 1 d . . . H13A H 0.3203 0.0656 0.7623 0.034 Uiso 1 1 calc R . . C14 C 0.3408(2) -0.0336(3) 0.6872(3) 0.0226(10) Uani 1 1 d . . . H14A H 0.3163 -0.0182 0.6354 0.027 Uiso 1 1 calc R . . C15 C 0.3757(2) -0.1068(2) 0.6898(3) 0.0201(9) Uani 1 1 d . . . H15A H 0.3737 -0.1402 0.6390 0.024 Uiso 1 1 calc R . . C16 C 0.3697(2) -0.2876(3) 0.9180(3) 0.0214(10) Uani 1 1 d . . . H16A H 0.3544 -0.2368 0.9003 0.026 Uiso 1 1 calc R . . C17 C 0.3479(2) -0.3171(3) 1.0019(3) 0.0249(10) Uani 1 1 d . . . H17A H 0.3177 -0.2873 1.0383 0.030 Uiso 1 1 calc R . . C18 C 0.3721(2) -0.3915(3) 1.0302(3) 0.0288(10) Uani 1 1 d . . . H18A H 0.3614 -0.4111 1.0878 0.035 Uiso 1 1 calc R . . C19 C 0.4128(2) -0.4362(3) 0.9708(3) 0.0245(10) Uani 1 1 d . . . H19A H 0.4282 -0.4872 0.9874 0.029 Uiso 1 1 calc R . . C20 C 0.43043(19) -0.4045(2) 0.8863(3) 0.0185(9) Uani 1 1 d . . . C21 C 0.4678(2) -0.4524(3) 0.8166(3) 0.0198(9) Uani 1 1 d . . . C22 C 0.4668(2) -0.5363(3) 0.8184(3) 0.0283(11) Uani 1 1 d . . . H22A H 0.4440 -0.5634 0.8651 0.034 Uiso 1 1 calc R . . C23 C 0.5000 -0.5787(4) 0.7500 0.0334(16) Uani 1 2 d S . . H23A H 0.5000 -0.6348 0.7500 0.040 Uiso 1 2 calc SR . . C24 C 0.1562(3) 0.2461(3) 1.2320(3) 0.0287(11) Uani 1 1 d . . . C25 C 0.2327(3) 0.2466(3) 1.2353(4) 0.0398(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd 0.01481(16) 0.01466(16) 0.01580(17) 0.000 0.00032(13) 0.000 I1 0.0310(2) 0.0275(2) 0.0258(2) 0.000 0.000 0.00206(18) I2 0.02813(17) 0.02370(16) 0.03106(17) -0.00232(13) -0.00441(13) 0.00248(12) N1 0.0182(17) 0.0184(18) 0.020(2) 0.0012(15) 0.0002(15) -0.0043(15) N2 0.0145(16) 0.0169(18) 0.0170(18) 0.0014(14) 0.0012(14) -0.0048(14) N3 0.0162(17) 0.0205(19) 0.0187(19) -0.0031(15) 0.0007(14) 0.0017(15) N4 0.0135(17) 0.0189(19) 0.024(2) 0.0002(16) -0.0006(15) -0.0022(14) N5 0.018(2) 0.020(3) 0.017(3) 0.000 0.001(2) 0.000 N6 0.034(3) 0.058(3) 0.031(3) -0.005(2) 0.0022(19) 0.002(2) C1 0.016(2) 0.025(2) 0.022(2) -0.0001(19) 0.0009(18) -0.0004(18) C2 0.016(2) 0.019(2) 0.028(2) 0.004(2) -0.0011(18) 0.0011(17) C3 0.027(2) 0.030(3) 0.025(2) 0.008(2) -0.005(2) -0.001(2) C4 0.027(2) 0.025(2) 0.019(2) 0.0001(19) -0.0053(19) -0.0023(19) C5 0.020(2) 0.018(2) 0.022(2) 0.0060(18) -0.0005(18) -0.0029(18) C6 0.017(2) 0.018(2) 0.023(2) -0.0019(19) 0.0018(18) -0.0044(17) C7 0.034(3) 0.032(3) 0.022(2) -0.003(2) -0.002(2) -0.002(2) C8 0.030(2) 0.038(3) 0.023(3) -0.010(2) 0.002(2) 0.003(2) C9 0.023(2) 0.024(2) 0.030(3) -0.006(2) 0.002(2) -0.0020(19) C10 0.016(2) 0.015(2) 0.028(2) -0.0012(19) 0.0029(18) -0.0044(17) C11 0.017(2) 0.021(2) 0.025(2) -0.0014(19) 0.0059(18) -0.0018(18) C12 0.029(2) 0.021(2) 0.029(3) -0.005(2) 0.002(2) 0.000(2) C13 0.024(2) 0.023(3) 0.039(3) -0.002(2) 0.000(2) 0.005(2) C14 0.018(2) 0.022(2) 0.027(3) 0.005(2) 0.0016(18) 0.0030(18) C15 0.017(2) 0.020(2) 0.023(2) 0.0000(19) 0.0003(18) 0.0011(18) C16 0.018(2) 0.019(2) 0.027(2) -0.0044(19) -0.0022(19) -0.0014(18) C17 0.024(2) 0.028(3) 0.023(3) -0.002(2) 0.0023(19) -0.003(2) C18 0.031(2) 0.031(3) 0.024(2) 0.007(2) -0.001(2) -0.004(2) C19 0.025(2) 0.023(2) 0.025(3) 0.002(2) 0.003(2) 0.0013(19) C20 0.0123(19) 0.018(2) 0.025(2) 0.0000(19) -0.0027(18) -0.0016(17) C21 0.017(2) 0.020(2) 0.023(2) 0.0026(19) 0.0035(18) -0.0025(18) C22 0.028(2) 0.018(2) 0.038(3) 0.001(2) 0.007(2) 0.0007(19) C23 0.044(4) 0.016(3) 0.041(4) 0.000 0.009(4) 0.000 C24 0.037(3) 0.029(3) 0.020(3) 0.003(2) 0.002(2) -0.002(2) C25 0.027(3) 0.046(3) 0.047(3) 0.003(3) 0.003(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd N1 2.587(3) . ? Nd N1 2.587(3) 3_656 ? Nd N3 2.616(3) 3_656 ? Nd N3 2.617(3) . ? Nd N2 2.618(3) 3_656 ? Nd N2 2.618(3) . ? Nd N5 2.637(5) . ? Nd N4 2.676(3) . ? Nd N4 2.676(3) 3_656 ? N1 C1 1.349(5) . ? N1 C5 1.362(5) . ? N2 C6 1.356(5) . ? N2 C10 1.361(5) . ? N3 C15 1.350(5) . ? N3 C11 1.356(5) . ? N4 C16 1.343(5) . ? N4 C20 1.366(5) . ? N5 C21 1.348(5) . ? N5 C21 1.348(5) 3_656 ? N6 C24 1.140(6) . ? C1 C2 1.378(6) . ? C2 C3 1.378(6) . ? C3 C4 1.382(6) . ? C4 C5 1.387(6) . ? C5 C6 1.491(6) . ? C6 C7 1.390(6) . ? C7 C8 1.390(7) . ? C8 C9 1.376(6) . ? C9 C10 1.391(6) . ? C10 C11 1.488(6) . ? C11 C12 1.392(6) . ? C12 C13 1.378(7) . ? C13 C14 1.381(7) . ? C14 C15 1.388(6) . ? C16 C17 1.390(6) . ? C17 C18 1.384(6) . ? C18 C19 1.386(6) . ? C19 C20 1.389(6) . ? C20 C21 1.483(6) . ? C21 C22 1.391(6) . ? C22 C23 1.384(6) . ? C23 C22 1.384(6) 3_656 ? C24 C25 1.470(7) . ? 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 N1 144.59(15) . 3_656 ? N1 Nd N3 83.16(10) . 3_656 ? N1 Nd N3 125.65(11) 3_656 3_656 ? N1 Nd N3 125.65(11) . . ? N1 Nd N3 83.16(10) 3_656 . ? N3 Nd N3 80.64(15) 3_656 . ? N1 Nd N2 138.32(10) . 3_656 ? N1 Nd N2 62.61(10) 3_656 3_656 ? N3 Nd N2 63.09(10) 3_656 3_656 ? N3 Nd N2 74.54(10) . 3_656 ? N1 Nd N2 62.61(10) . . ? N1 Nd N2 138.32(10) 3_656 . ? N3 Nd N2 74.54(10) 3_656 . ? N3 Nd N2 63.09(10) . . ? N2 Nd N2 123.73(14) 3_656 . ? N1 Nd N5 72.29(7) . . ? N1 Nd N5 72.29(7) 3_656 . ? N3 Nd N5 139.68(7) 3_656 . ? N3 Nd N5 139.68(7) . . ? N2 Nd N5 118.14(7) 3_656 . ? N2 Nd N5 118.14(7) . . ? N1 Nd N4 79.45(10) . . ? N1 Nd N4 83.94(11) 3_656 . ? N3 Nd N4 144.54(10) 3_656 . ? N3 Nd N4 84.79(10) . . ? N2 Nd N4 142.10(10) 3_656 . ? N2 Nd N4 70.04(10) . . ? N5 Nd N4 61.66(7) . . ? N1 Nd N4 83.94(11) . 3_656 ? N1 Nd N4 79.45(10) 3_656 3_656 ? N3 Nd N4 84.79(10) 3_656 3_656 ? N3 Nd N4 144.55(10) . 3_656 ? N2 Nd N4 70.04(10) 3_656 3_656 ? N2 Nd N4 142.09(10) . 3_656 ? N5 Nd N4 61.66(7) . 3_656 ? N4 Nd N4 123.33(15) . 3_656 ? C1 N1 C5 117.6(4) . . ? C6 N2 C10 117.7(4) . . ? C15 N3 C11 118.0(4) . . ? C16 N4 C20 117.1(4) . . ? C21 N5 C21 118.2(5) . 3_656 ? N1 C1 C2 123.4(4) . . ? C1 C2 C3 119.0(4) . . ? C2 C3 C4 118.6(4) . . ? C3 C4 C5 120.2(4) . . ? N1 C5 C4 121.3(4) . . ? N1 C5 C6 116.7(4) . . ? C4 C5 C6 121.9(4) . . ? N2 C6 C7 122.5(4) . . ? N2 C6 C5 116.3(4) . . ? C7 C6 C5 121.2(4) . . ? C8 C7 C6 118.9(4) . . ? C9 C8 C7 119.3(4) . . ? C8 C9 C10 119.3(4) . . ? N2 C10 C9 122.3(4) . . ? N2 C10 C11 116.6(4) . . ? C9 C10 C11 121.1(4) . . ? N3 C11 C12 121.6(4) . . ? N3 C11 C10 117.1(4) . . ? C12 C11 C10 121.2(4) . . ? C13 C12 C11 119.9(4) . . ? C12 C13 C14 118.8(4) . . ? C13 C14 C15 119.0(4) . . ? N3 C15 C14 122.7(4) . . ? N4 C16 C17 123.8(4) . . ? C18 C17 C16 118.6(4) . . ? C17 C18 C19 118.5(4) . . ? C18 C19 C20 119.8(4) . . ? N4 C20 C19 121.9(4) . . ? N4 C20 C21 115.9(4) . . ? C19 C20 C21 122.1(4) . . ? N5 C21 C22 122.3(4) . . ? N5 C21 C20 116.6(4) . . ? C22 C21 C20 121.1(4) . . ? C23 C22 C21 119.2(5) . . ? C22 C23 C22 118.8(6) 3_656 . ? N6 C24 C25 178.7(5) . . ? #===END data_4.2MeCN _database_code_CSD 181676 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H39 I3 N11 U' _chemical_formula_weight 1400.64 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 orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 19.198(4) _cell_length_b 16.591(3) _cell_length_c 14.677(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4674.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 30940 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.990 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2644 _exptl_absorpt_coefficient_mu 5.501 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.378 _exptl_absorpt_correction_T_max 0.458 _exptl_absorpt_process_details 'MULABS in PLATON;Spek,1998' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%. A 180\% range in \f was scanned during data collection with 2\%\f steps and 10 s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f rotation scans with 2\%steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30940 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.69 _reflns_number_total 4324 _reflns_number_gt 3334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms (except H atoms of solvent molecules) were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) times that of the parent atom. ; _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^)+(0.0604P)^2^+0.2801P] 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 4324 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.055 _refine_ls_shift/su_mean 0.002 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.874 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.178 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 0.5000 0.748006(18) 0.2500 0.01518(11) Uani 1 2 d S . . I1 I 0.26618(2) 0.86571(3) -0.02197(3) 0.02831(14) Uani 1 1 d . . . I2 I 0.7500 0.5000 0.21502(4) 0.02841(17) Uani 1 2 d S . . N1 N 0.4156(3) 0.7004(3) 0.1231(3) 0.0177(11) Uani 1 1 d . . . N2 N 0.5064(3) 0.8236(3) 0.0931(3) 0.0200(12) Uani 1 1 d . . . N3 N 0.5873(3) 0.8690(3) 0.2367(3) 0.0191(11) Uani 1 1 d . . . N4 N 0.5881(3) 0.6712(3) 0.1382(3) 0.0210(12) Uani 1 1 d . . . N5 N 0.5000 0.5900(4) 0.2500 0.0197(16) Uani 1 2 d S . . N6 N 0.5971(4) 0.7554(4) -0.2311(4) 0.0412(18) Uani 1 1 d . . . C1 C 0.3679(3) 0.6426(4) 0.1391(4) 0.0202(13) Uani 1 1 d . . . H1A H 0.3622 0.6250 0.1988 0.024 Uiso 1 1 calc R . . C2 C 0.3272(3) 0.6080(4) 0.0729(4) 0.0225(14) Uani 1 1 d . . . H2A H 0.2944 0.5689 0.0876 0.027 Uiso 1 1 calc R . . C3 C 0.3361(4) 0.6329(4) -0.0163(5) 0.0281(15) Uani 1 1 d . . . H3A H 0.3097 0.6103 -0.0629 0.034 Uiso 1 1 calc R . . C4 C 0.3845(4) 0.6911(4) -0.0347(4) 0.0231(14) Uani 1 1 d . . . H4A H 0.3914 0.7079 -0.0945 0.028 Uiso 1 1 calc R . . C5 C 0.4234(3) 0.7257(4) 0.0352(4) 0.0193(13) Uani 1 1 d . . . C6 C 0.4730(3) 0.7919(4) 0.0186(4) 0.0185(13) Uani 1 1 d . . . C7 C 0.4852(4) 0.8232(4) -0.0682(4) 0.0268(16) Uani 1 1 d . . . H7A H 0.4620 0.8020 -0.1184 0.032 Uiso 1 1 calc R . . C8 C 0.5312(4) 0.8847(4) -0.0792(5) 0.0318(17) Uani 1 1 d . . . H8A H 0.5405 0.9043 -0.1373 0.038 Uiso 1 1 calc R . . C9 C 0.5637(4) 0.9182(4) -0.0054(4) 0.0246(15) Uani 1 1 d . . . H9A H 0.5939 0.9616 -0.0122 0.029 Uiso 1 1 calc R . . C10 C 0.5502(3) 0.8849(4) 0.0815(4) 0.0186(13) Uani 1 1 d . . . C11 C 0.5865(3) 0.9169(4) 0.1622(4) 0.0215(14) Uani 1 1 d . . . C12 C 0.6204(4) 0.9906(4) 0.1615(4) 0.0270(15) Uani 1 1 d . . . H12A H 0.6179 1.0232 0.1100 0.032 Uiso 1 1 calc R . . C13 C 0.6580(4) 1.0166(4) 0.2366(4) 0.0245(15) Uani 1 1 d . . . H13A H 0.6812 1.0658 0.2363 0.029 Uiso 1 1 calc R . . C14 C 0.6598(3) 0.9659(4) 0.3130(5) 0.0253(15) Uani 1 1 d . . . H14A H 0.6846 0.9808 0.3647 0.030 Uiso 1 1 calc R . . C15 C 0.6246(3) 0.8944(4) 0.3104(4) 0.0233(14) Uani 1 1 d . . . H15A H 0.6262 0.8614 0.3615 0.028 Uiso 1 1 calc R . . C16 C 0.6302(3) 0.7117(4) 0.0814(4) 0.0214(14) Uani 1 1 d . . . H16A H 0.6456 0.7625 0.0993 0.026 Uiso 1 1 calc R . . C17 C 0.6520(3) 0.6828(4) -0.0017(4) 0.0255(15) Uani 1 1 d . . . H17A H 0.6820 0.7129 -0.0382 0.031 Uiso 1 1 calc R . . C18 C 0.6283(4) 0.6078(4) -0.0299(4) 0.0273(15) Uani 1 1 d . . . H18A H 0.6398 0.5879 -0.0872 0.033 Uiso 1 1 calc R . . C19 C 0.5874(3) 0.5633(4) 0.0290(4) 0.0228(14) Uani 1 1 d . . . H19A H 0.5719 0.5123 0.0122 0.027 Uiso 1 1 calc R . . C20 C 0.5695(3) 0.5954(4) 0.1136(4) 0.0190(13) Uani 1 1 d . . . C21 C 0.5313(3) 0.5481(4) 0.1834(4) 0.0195(13) Uani 1 1 d . . . C22 C 0.5329(4) 0.4639(4) 0.1817(5) 0.0278(16) Uani 1 1 d . . . H22A H 0.5558 0.4367 0.1351 0.033 Uiso 1 1 calc R . . C23 C 0.5000 0.4218(6) 0.2500 0.034(2) Uani 1 2 d S . . H23A H 0.5000 0.3657 0.2500 0.041 Uiso 1 2 calc SR . . C24 C 0.6571(5) 0.7550(4) -0.2313(4) 0.0269(17) Uani 1 1 d . . . C25 C 0.7325(5) 0.7526(5) -0.2351(5) 0.038(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.01853(18) 0.01232(18) 0.01470(18) 0.000 0.00035(13) 0.000 I1 0.0327(3) 0.0217(2) 0.0305(2) 0.00270(18) -0.00454(18) -0.00256(19) I2 0.0353(4) 0.0253(3) 0.0246(3) 0.000 0.000 0.0023(3) N1 0.019(3) 0.016(3) 0.017(3) -0.001(2) 0.003(2) 0.004(2) N2 0.021(3) 0.020(3) 0.019(3) 0.002(2) 0.001(2) 0.006(2) N3 0.023(3) 0.018(3) 0.017(3) 0.002(2) 0.001(2) 0.004(2) N4 0.023(3) 0.016(3) 0.024(3) 0.003(2) -0.001(2) 0.003(2) N5 0.020(4) 0.015(4) 0.024(4) 0.000 -0.002(3) 0.000 N6 0.045(5) 0.048(5) 0.031(4) 0.003(3) 0.000(3) 0.004(4) C1 0.018(3) 0.020(3) 0.022(3) 0.002(3) 0.000(2) 0.002(3) C2 0.020(3) 0.016(3) 0.032(4) -0.002(3) -0.006(3) 0.000(3) C3 0.034(4) 0.023(4) 0.028(3) -0.009(3) -0.008(3) 0.005(3) C4 0.040(4) 0.016(3) 0.013(3) 0.001(2) -0.005(3) 0.001(3) C5 0.023(3) 0.020(3) 0.016(3) -0.002(3) -0.002(2) 0.007(3) C6 0.014(3) 0.022(3) 0.019(3) -0.002(3) -0.002(2) 0.000(3) C7 0.029(4) 0.032(4) 0.019(3) 0.006(3) 0.000(3) 0.003(3) C8 0.042(4) 0.031(4) 0.022(4) 0.009(3) 0.000(3) -0.002(3) C9 0.033(4) 0.013(3) 0.027(4) 0.006(3) 0.002(3) -0.004(3) C10 0.018(3) 0.013(3) 0.025(3) 0.006(3) 0.002(2) 0.003(3) C11 0.024(4) 0.021(4) 0.020(3) -0.004(3) -0.001(3) 0.004(3) C12 0.037(4) 0.016(3) 0.028(3) 0.009(3) 0.003(3) -0.003(3) C13 0.026(4) 0.016(4) 0.032(4) -0.001(3) 0.002(3) -0.007(3) C14 0.023(4) 0.024(4) 0.029(4) -0.008(3) 0.005(3) -0.002(3) C15 0.025(4) 0.023(4) 0.021(3) 0.002(3) 0.005(3) -0.002(3) C16 0.028(4) 0.014(3) 0.023(3) 0.001(3) -0.004(3) 0.000(3) C17 0.023(4) 0.028(4) 0.026(3) 0.004(3) 0.005(3) 0.001(3) C18 0.029(4) 0.029(4) 0.024(3) -0.004(3) 0.001(3) 0.001(3) C19 0.027(4) 0.020(3) 0.022(3) -0.005(3) 0.003(3) -0.004(3) C20 0.022(3) 0.017(3) 0.019(3) 0.001(3) -0.001(2) -0.001(3) C21 0.020(3) 0.017(3) 0.022(3) 0.000(3) 0.000(2) 0.000(3) C22 0.032(4) 0.017(4) 0.034(4) -0.004(3) 0.006(3) 0.005(3) C23 0.050(7) 0.019(5) 0.034(6) 0.000 0.010(5) 0.000 C24 0.045(5) 0.024(4) 0.011(3) 0.002(2) 0.000(3) -0.005(3) C25 0.037(5) 0.037(5) 0.040(5) 0.006(3) -0.003(3) 0.009(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 U N1 2.592(5) 3_655 ? U N1 2.592(5) . ? U N3 2.622(5) 3_655 ? U N3 2.622(5) . ? U N5 2.622(7) . ? U N2 2.625(5) . ? U N2 2.625(5) 3_655 ? U N4 2.679(5) . ? U N4 2.679(5) 3_655 ? N1 C1 1.345(8) . ? N1 C5 1.365(7) . ? N2 C10 1.331(8) . ? N2 C6 1.371(8) . ? N3 C11 1.352(8) . ? N3 C15 1.364(8) . ? N4 C16 1.343(8) . ? N4 C20 1.356(8) . ? N5 C21 1.341(7) . ? N5 C21 1.341(7) 3_655 ? N6 C24 1.152(11) . ? C1 C2 1.374(8) . ? C2 C3 1.383(9) . ? C3 C4 1.367(10) . ? C4 C5 1.392(8) . ? C5 C6 1.475(9) . ? C6 C7 1.396(9) . ? C7 C8 1.358(10) . ? C8 C9 1.368(9) . ? C9 C10 1.415(8) . ? C10 C11 1.472(8) . ? C11 C12 1.387(9) . ? C12 C13 1.386(9) . ? C13 C14 1.401(10) . ? C14 C15 1.365(9) . ? C16 C17 1.376(9) . ? C17 C18 1.389(9) . ? C18 C19 1.382(9) . ? C19 C20 1.395(8) . ? C20 C21 1.485(8) . ? C21 C22 1.398(9) . ? C22 C23 1.375(9) . ? C23 C22 1.375(9) 3_655 ? C24 C25 1.450(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 N1 U N1 144.5(2) 3_655 . ? N1 U N3 125.42(15) 3_655 3_655 ? N1 U N3 83.51(15) . 3_655 ? N1 U N3 83.51(15) 3_655 . ? N1 U N3 125.42(15) . . ? N3 U N3 80.1(2) 3_655 . ? N1 U N5 72.26(11) 3_655 . ? N1 U N5 72.26(11) . . ? N3 U N5 139.95(12) 3_655 . ? N3 U N5 139.95(11) . . ? N1 U N2 138.31(15) 3_655 . ? N1 U N2 62.89(16) . . ? N3 U N2 74.29(15) 3_655 . ? N3 U N2 62.57(15) . . ? N5 U N2 118.53(11) . . ? N1 U N2 62.89(16) 3_655 3_655 ? N1 U N2 138.31(15) . 3_655 ? N3 U N2 62.57(15) 3_655 3_655 ? N3 U N2 74.30(15) . 3_655 ? N5 U N2 118.53(11) . 3_655 ? N2 U N2 122.9(2) . 3_655 ? N1 U N4 84.27(16) 3_655 . ? N1 U N4 79.04(16) . . ? N3 U N4 144.42(14) 3_655 . ? N3 U N4 85.14(16) . . ? N5 U N4 61.58(11) . . ? N2 U N4 70.17(15) . . ? N2 U N4 142.55(16) 3_655 . ? N1 U N4 79.04(16) 3_655 3_655 ? N1 U N4 84.27(16) . 3_655 ? N3 U N4 85.14(16) 3_655 3_655 ? N3 U N4 144.42(14) . 3_655 ? N5 U N4 61.58(11) . 3_655 ? N2 U N4 142.55(16) . 3_655 ? N2 U N4 70.17(15) 3_655 3_655 ? N4 U N4 123.2(2) . 3_655 ? C1 N1 C5 117.3(5) . . ? C10 N2 C6 119.1(5) . . ? C11 N3 C15 117.8(6) . . ? C16 N4 C20 117.2(5) . . ? C21 N5 C21 117.6(8) . 3_655 ? N1 C1 C2 124.1(6) . . ? C1 C2 C3 118.3(6) . . ? C4 C3 C2 118.8(6) . . ? C3 C4 C5 120.6(6) . . ? N1 C5 C4 120.7(6) . . ? N1 C5 C6 117.1(5) . . ? C4 C5 C6 122.1(5) . . ? N2 C6 C7 120.5(6) . . ? N2 C6 C5 117.1(5) . . ? C7 C6 C5 122.4(6) . . ? C8 C7 C6 119.7(6) . . ? C7 C8 C9 120.6(6) . . ? C8 C9 C10 118.1(6) . . ? N2 C10 C9 122.0(6) . . ? N2 C10 C11 118.2(5) . . ? C9 C10 C11 119.8(6) . . ? N3 C11 C12 121.2(6) . . ? N3 C11 C10 116.4(6) . . ? C12 C11 C10 122.3(6) . . ? C13 C12 C11 120.9(6) . . ? C12 C13 C14 117.6(6) . . ? C15 C14 C13 119.1(6) . . ? N3 C15 C14 123.4(6) . . ? N4 C16 C17 124.0(6) . . ? C16 C17 C18 118.5(6) . . ? C19 C18 C17 118.6(6) . . ? C18 C19 C20 119.5(6) . . ? N4 C20 C19 121.8(6) . . ? N4 C20 C21 115.9(5) . . ? C19 C20 C21 122.3(6) . . ? N5 C21 C22 122.7(6) . . ? N5 C21 C20 116.8(6) . . ? C22 C21 C20 120.4(6) . . ? C23 C22 C21 119.0(7) . . ? C22 C23 C22 119.0(10) . 3_655 ? N6 C24 C25 177.5(8) . . ? #===END data_8.MeCN _database_code_CSD 181677 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H48 F9 La N22 O9 S3' _chemical_formula_weight 1507.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.337(3) _cell_length_b 17.283(4) _cell_length_c 14.449(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.29(3) _cell_angle_gamma 90.00 _cell_volume 3227.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20084 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour 'pale ochre' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'MULABS in PLATON;Spek,1998' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 10s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f rotation scans with 2\%steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20084 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 24.68 _reflns_number_total 10086 _reflns_number_gt 8529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms were introduced at calculated positions 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 badly resolved acetonitrile molecule was fixed in the last refinement cycles. A void of 88 A^3^ may indicate the presence of other unresolved solvent molecules. ; _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^)+(0.0643P)^2^+4.5491P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(16) _refine_ls_number_reflns 10086 _refine_ls_number_parameters 832 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.063 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.68 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.825 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.105 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La La 0.31573(3) 0.56183(2) 0.68481(3) 0.01919(11) Uani 1 1 d . . . S1 S 0.23726(19) 0.50447(16) 0.26683(18) 0.0433(6) Uani 1 1 d . . . S2 S 0.77996(19) 0.53908(12) 0.61435(17) 0.0409(6) Uani 1 1 d . . . S3 S 0.3334(3) 0.8424(2) 0.9102(3) 0.0311(8) Uani 1 1 d . . . F1 F 0.0546(5) 0.5673(6) 0.2442(5) 0.086(2) Uani 1 1 d . . . F2 F 0.1455(6) 0.6175(5) 0.1564(6) 0.095(3) Uani 1 1 d . . . F3 F 0.1837(9) 0.6435(6) 0.3070(9) 0.143(5) Uani 1 1 d . . . F4 F 0.8128(7) 0.6299(4) 0.7627(5) 0.094(3) Uani 1 1 d . . . F5 F 0.9117(6) 0.6531(4) 0.6680(5) 0.081(2) Uani 1 1 d . . . F6 F 0.9377(5) 0.5554(6) 0.7632(5) 0.100(2) Uani 1 1 d . . . F7 F 0.4202(7) 0.9755(4) 0.9627(7) 0.111(3) Uani 1 1 d . . . F8 F 0.3506(9) 0.9526(6) 0.7959(7) 0.130(4) Uani 1 1 d . . . F9 F 0.5066(9) 0.9042(7) 0.8910(11) 0.183(7) Uani 1 1 d . . . O1 O 0.2336(8) 0.4863(10) 0.3590(8) 0.136(6) Uani 1 1 d . . . O2 O 0.3330(5) 0.5320(4) 0.2546(5) 0.059(2) Uani 1 1 d . . . O3 O 0.1880(7) 0.4517(5) 0.1923(8) 0.086(3) Uani 1 1 d . . . O4 O 0.8523(8) 0.5049(5) 0.5648(7) 0.090(3) Uani 1 1 d . . . O5 O 0.7383(5) 0.4830(3) 0.6666(4) 0.0421(16) Uani 1 1 d . . . O6 O 0.7137(7) 0.5945(4) 0.5607(7) 0.086(3) Uani 1 1 d . . . O7 O 0.3916(10) 0.8221(6) 1.0024(7) 0.111(4) Uani 1 1 d . . . O8 O 0.3433(6) 0.7923(5) 0.8307(6) 0.066(2) Uani 1 1 d . . . O9 O 0.2342(7) 0.8761(5) 0.9009(7) 0.085(3) Uani 1 1 d . . . N1C N 0.2922(6) 0.4223(4) 0.6022(5) 0.0209(17) Uani 1 1 d . . . N1B N 0.3642(4) 0.5742(4) 0.8760(4) 0.0215(15) Uani 1 1 d . . . N1A N 0.2850(6) 0.6884(4) 0.5785(5) 0.0200(16) Uani 1 1 d . . . N2C N 0.0822(5) 0.5946(4) 0.5213(5) 0.0242(14) Uani 1 1 d . . . N2B N 0.1320(5) 0.4336(4) 0.7332(5) 0.0285(16) Uani 1 1 d . . . N2A N 0.1595(5) 0.6612(4) 0.8043(5) 0.0239(15) Uani 1 1 d . . . N3C N 0.1488(5) 0.5345(3) 0.5497(4) 0.0219(14) Uani 1 1 d . . . N3B N 0.2101(5) 0.4787(4) 0.7830(5) 0.0248(15) Uani 1 1 d . . . N3A N 0.1926(5) 0.6688(4) 0.7245(5) 0.0241(15) Uani 1 1 d . . . N4C N 0.0361(5) 0.4476(4) 0.4442(4) 0.0224(14) Uani 1 1 d . . . N4B N 0.1660(5) 0.4510(4) 0.9288(5) 0.0302(17) Uani 1 1 d . . . N4A N 0.1028(5) 0.7871(4) 0.6858(5) 0.0249(15) Uani 1 1 d . . . N5C N 0.5512(5) 0.4853(4) 0.7985(5) 0.0278(15) Uani 1 1 d . . . N5B N 0.5126(5) 0.6976(4) 0.7114(5) 0.0269(15) Uani 1 1 d . . . N5A N 0.4579(5) 0.5094(4) 0.5228(5) 0.0270(15) Uani 1 1 d . . . N6B N 0.4652(6) 0.6582(4) 0.7688(5) 0.0233(17) Uani 1 1 d . . . N6A N 0.4055(4) 0.5724(4) 0.5429(4) 0.0212(14) Uani 1 1 d . . . N6C N 0.4635(6) 0.4600(4) 0.7356(5) 0.0226(17) Uani 1 1 d . . . N7C N 0.5406(5) 0.3382(4) 0.7194(5) 0.0301(16) Uani 1 1 d . . . N7B N 0.5797(5) 0.7076(4) 0.9083(5) 0.0301(16) Uani 1 1 d . . . N7A N 0.4567(5) 0.6469(4) 0.4247(5) 0.0237(15) Uani 1 1 d . . . C1C C -0.0041(6) 0.5804(4) 0.4548(6) 0.0250(19) Uani 1 1 d . . . C1B C 0.0723(7) 0.3979(6) 0.7803(7) 0.034(2) Uani 1 1 d . . . C1A C 0.1006(7) 0.7172(5) 0.8269(7) 0.029(2) Uani 1 1 d . . . C2C C -0.0294(6) 0.5054(5) 0.4175(6) 0.0232(17) Uani 1 1 d . . . C2B C 0.0905(7) 0.4075(6) 0.8785(8) 0.036(2) Uani 1 1 d . . . C2A C 0.0678(6) 0.7807(5) 0.7634(6) 0.0289(19) Uani 1 1 d . . . C3C C 0.1244(6) 0.4646(4) 0.5099(5) 0.0202(17) Uani 1 1 d . . . C3B C 0.2223(6) 0.4866(5) 0.8747(6) 0.0265(19) Uani 1 1 d . . . C3A C 0.1686(6) 0.7315(4) 0.6712(6) 0.0216(17) Uani 1 1 d . . . C4C C 0.2035(6) 0.4034(4) 0.5376(6) 0.0205(17) Uani 1 1 d . . . C4B C 0.3079(6) 0.5383(4) 0.9282(5) 0.0246(18) Uani 1 1 d . . . C4A C 0.2175(6) 0.7437(4) 0.5911(6) 0.0223(17) Uani 1 1 d . . . C5C C 0.1873(7) 0.3305(5) 0.4948(6) 0.0211(19) Uani 1 1 d . . . H5CB H 0.121(7) 0.320(5) 0.459(6) 0.025 Uiso 1 1 d . . . C5B C 0.3210(6) 0.5489(5) 1.0262(5) 0.026(2) Uani 1 1 d . . . H5BB H 0.2827 0.5209 1.0605 0.032 Uiso 1 1 calc R . . C5A C 0.1970(7) 0.8087(5) 0.5339(6) 0.026(2) Uani 1 1 d . . . H5AB H 0.1490 0.8449 0.5437 0.032 Uiso 1 1 calc R . . C6C C 0.2669(6) 0.2767(5) 0.5162(6) 0.0278(19) Uani 1 1 d . . . H6CA H 0.2594 0.2285 0.4867 0.033 Uiso 1 1 calc R . . C6B C 0.3943(7) 0.6035(5) 1.0703(6) 0.033(2) Uani 1 1 d . . . H6BA H 0.4047 0.6142 1.1351 0.040 Uiso 1 1 calc R . . C6A C 0.2472(6) 0.8199(4) 0.4625(7) 0.0286(19) Uani 1 1 d . . . H6AA H 0.2341 0.8637 0.4240 0.034 Uiso 1 1 calc R . . C7C C 0.3586(6) 0.2963(4) 0.5828(6) 0.0289(19) Uani 1 1 d . . . H7CB H 0.4130 0.2612 0.5983 0.035 Uiso 1 1 calc R . . C7B C 0.4506(7) 0.6408(5) 1.0171(6) 0.031(2) Uani 1 1 d . . . H7BB H 0.4990 0.6777 1.0459 0.038 Uiso 1 1 calc R . . C7A C 0.3195(6) 0.7634(4) 0.4487(6) 0.0266(18) Uani 1 1 d . . . H7AB H 0.3553 0.7692 0.4014 0.032 Uiso 1 1 calc R . . C8C C 0.3673(6) 0.3675(4) 0.6249(5) 0.0236(17) Uani 1 1 d . . . C8B C 0.4372(6) 0.6249(4) 0.9210(6) 0.0240(17) Uani 1 1 d . . . C8A C 0.3348(6) 0.6991(4) 0.5085(5) 0.0215(16) Uani 1 1 d . . . C9C C 0.4615(6) 0.3904(4) 0.6974(6) 0.0213(17) Uani 1 1 d . . . C9B C 0.4956(6) 0.6649(5) 0.8618(6) 0.0250(18) Uani 1 1 d . . . C9A C 0.4025(6) 0.6354(4) 0.4916(6) 0.0211(17) Uani 1 1 d . . . C10C C 0.6257(7) 0.3629(6) 0.7835(6) 0.029(2) Uani 1 1 d . . . C10A C 0.5079(5) 0.5868(4) 0.4052(6) 0.0229(19) Uani 1 1 d . . . C10B C 0.6277(7) 0.7454(5) 0.8517(7) 0.033(2) Uani 1 1 d . . . C11C C 0.6317(6) 0.4379(5) 0.8214(6) 0.0301(19) Uani 1 1 d . . . C11A C 0.5064(6) 0.5153(5) 0.4523(6) 0.0228(18) Uani 1 1 d . . . C11B C 0.5916(7) 0.7435(5) 0.7513(7) 0.028(2) Uani 1 1 d . . . C12C C -0.1293(6) 0.4898(5) 0.3438(6) 0.0314(19) Uani 1 1 d . . . H12A H -0.1314 0.4366 0.3244 0.047 Uiso 1 1 calc R . . H12B H -0.1332 0.5225 0.2893 0.047 Uiso 1 1 calc R . . H12C H -0.1868 0.5004 0.3708 0.047 Uiso 1 1 calc R . . C12B C -0.0133(8) 0.3504(7) 0.7219(7) 0.062(3) Uani 1 1 d . . . H12D H -0.0150 0.3564 0.6555 0.093 Uiso 1 1 calc R . . H12E H -0.0779 0.3673 0.7330 0.093 Uiso 1 1 calc R . . H12F H -0.0022 0.2970 0.7396 0.093 Uiso 1 1 calc R . . C12A C 0.0714(8) 0.7089(6) 0.9186(7) 0.038(2) Uani 1 1 d . . . H12G H 0.1013 0.6624 0.9499 0.058 Uiso 1 1 calc R . . H12H H -0.0026 0.7064 0.9068 0.058 Uiso 1 1 calc R . . H12I H 0.0965 0.7526 0.9585 0.058 Uiso 1 1 calc R . . C13C C -0.0756(7) 0.6493(5) 0.4210(8) 0.044(2) Uani 1 1 d . . . H13A H -0.0473 0.6946 0.4564 0.066 Uiso 1 1 calc R . . H13B H -0.1427 0.6386 0.4311 0.066 Uiso 1 1 calc R . . H13C H -0.0816 0.6579 0.3542 0.066 Uiso 1 1 calc R . . C13B C 0.0213(8) 0.3682(7) 0.9355(7) 0.057(3) Uani 1 1 d . . . H13D H 0.0476 0.3790 1.0022 0.085 Uiso 1 1 calc R . . H13E H 0.0211 0.3133 0.9252 0.085 Uiso 1 1 calc R . . H13F H -0.0479 0.3878 0.9145 0.085 Uiso 1 1 calc R . . C13A C -0.0061(7) 0.8394(5) 0.7823(6) 0.033(2) Uani 1 1 d . . . H13G H -0.0184 0.8777 0.7327 0.050 Uiso 1 1 calc R . . H13H H 0.0224 0.8636 0.8428 0.050 Uiso 1 1 calc R . . H13I H -0.0702 0.8146 0.7835 0.050 Uiso 1 1 calc R . . C14C C 0.7121(7) 0.3059(6) 0.8123(7) 0.050(3) Uani 1 1 d . . . H14A H 0.6931 0.2584 0.7781 0.075 Uiso 1 1 calc R . . H14B H 0.7255 0.2964 0.8797 0.075 Uiso 1 1 calc R . . H14C H 0.7732 0.3264 0.7975 0.075 Uiso 1 1 calc R . . C14B C 0.7212(8) 0.7940(7) 0.8987(7) 0.051(3) Uani 1 1 d . . . H14D H 0.7348 0.7889 0.9668 0.077 Uiso 1 1 calc R . . H14E H 0.7077 0.8473 0.8813 0.077 Uiso 1 1 calc R . . H14F H 0.7803 0.7767 0.8777 0.077 Uiso 1 1 calc R . . C14A C 0.5676(6) 0.5953(5) 0.3308(6) 0.034(2) Uani 1 1 d . . . H14G H 0.5603 0.6473 0.3064 0.051 Uiso 1 1 calc R . . H14H H 0.5414 0.5596 0.2796 0.051 Uiso 1 1 calc R . . H14I H 0.6393 0.5846 0.3585 0.051 Uiso 1 1 calc R . . C15C C 0.7289(6) 0.4685(6) 0.8875(6) 0.037(2) Uani 1 1 d . . . H15A H 0.7176 0.5205 0.9057 0.055 Uiso 1 1 calc R . . H15B H 0.7841 0.4679 0.8556 0.055 Uiso 1 1 calc R . . H15C H 0.7473 0.4365 0.9435 0.055 Uiso 1 1 calc R . . C15B C 0.6396(7) 0.7868(6) 0.6870(7) 0.043(2) Uani 1 1 d . . . H15D H 0.6026 0.7773 0.6221 0.064 Uiso 1 1 calc R . . H15E H 0.7102 0.7706 0.6961 0.064 Uiso 1 1 calc R . . H15F H 0.6376 0.8411 0.7006 0.064 Uiso 1 1 calc R . . C15A C 0.5581(7) 0.4453(5) 0.4294(7) 0.033(2) Uani 1 1 d . . . H15G H 0.5470 0.4035 0.4695 0.049 Uiso 1 1 calc R . . H15H H 0.6309 0.4549 0.4400 0.049 Uiso 1 1 calc R . . H15I H 0.5300 0.4317 0.3636 0.049 Uiso 1 1 calc R . . C16 C 0.1508(10) 0.5868(7) 0.2377(10) 0.068(4) Uani 1 1 d . . . C18 C 0.4072(14) 0.9258(9) 0.8853(13) 0.096(5) Uani 1 1 d . . . C17 C 0.8659(8) 0.5957(6) 0.7046(8) 0.051(3) Uani 1 1 d . . . N8 N -0.1452 0.6363 0.0758 0.391 Uani 1 1 d . . . C19 C -0.0933 0.5974 0.0317 0.651 Uani 1 1 d . . . C20 C -0.0102 0.5147 -0.0115 0.944 Uani 1 1 d . . . H20A H -0.0181 0.4669 0.0198 1.415 Uiso 1 1 calc R . . H20B H 0.0615 0.5293 0.0044 1.415 Uiso 1 1 calc R . . H20C H -0.0339 0.5082 -0.0793 1.415 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 0.02270(18) 0.01704(18) 0.01883(19) 0.0001(2) 0.00701(13) 0.0005(3) S1 0.0336(12) 0.0588(16) 0.0402(14) 0.0122(12) 0.0143(11) -0.0054(12) S2 0.0511(13) 0.0366(15) 0.0340(12) 0.0010(9) 0.0086(11) -0.0161(10) S3 0.0344(19) 0.0284(18) 0.034(2) -0.0050(15) 0.0142(17) -0.0070(15) F1 0.071(4) 0.114(6) 0.090(5) 0.044(6) 0.052(3) 0.040(6) F2 0.104(6) 0.100(6) 0.096(6) 0.058(5) 0.052(5) 0.034(5) F3 0.189(12) 0.082(6) 0.170(12) -0.062(7) 0.068(9) 0.005(7) F4 0.156(8) 0.056(4) 0.070(5) -0.025(4) 0.031(5) 0.001(5) F5 0.083(5) 0.064(4) 0.083(5) 0.002(4) -0.003(4) -0.044(4) F6 0.082(4) 0.078(5) 0.107(5) 0.014(6) -0.039(4) -0.004(6) F7 0.143(7) 0.068(5) 0.156(8) -0.075(5) 0.098(7) -0.063(5) F8 0.161(9) 0.137(9) 0.091(7) 0.063(6) 0.032(7) 0.023(7) F9 0.155(9) 0.163(10) 0.300(16) -0.154(11) 0.185(11) -0.118(8) O1 0.067(6) 0.286(17) 0.067(7) 0.082(9) 0.037(6) 0.015(8) O2 0.039(3) 0.101(7) 0.039(4) 0.005(4) 0.012(3) -0.022(4) O3 0.085(6) 0.067(6) 0.111(8) -0.043(6) 0.033(6) -0.029(5) O4 0.127(8) 0.075(6) 0.098(7) -0.034(5) 0.086(7) -0.045(6) O5 0.060(4) 0.033(4) 0.037(4) -0.001(3) 0.019(3) -0.015(3) O6 0.080(6) 0.052(5) 0.090(6) 0.034(4) -0.048(5) -0.029(4) O7 0.205(12) 0.081(7) 0.066(6) 0.023(5) 0.069(7) 0.061(7) O8 0.055(4) 0.072(5) 0.067(5) -0.036(4) 0.006(4) -0.002(4) O9 0.074(6) 0.075(6) 0.115(8) -0.061(6) 0.044(5) -0.013(5) N1C 0.020(4) 0.020(4) 0.023(4) 0.005(3) 0.006(3) 0.005(3) N1B 0.024(3) 0.022(4) 0.020(3) 0.003(3) 0.010(2) 0.009(3) N1A 0.021(3) 0.016(3) 0.020(4) -0.003(3) -0.001(3) -0.003(3) N2C 0.024(3) 0.024(3) 0.025(4) 0.004(3) 0.007(3) 0.003(3) N2B 0.025(4) 0.027(4) 0.031(4) 0.004(3) 0.002(3) -0.005(3) N2A 0.031(4) 0.022(4) 0.020(4) -0.003(3) 0.011(3) 0.009(3) N3C 0.023(3) 0.022(3) 0.021(3) -0.002(2) 0.006(3) -0.003(3) N3B 0.026(4) 0.025(4) 0.024(4) 0.005(3) 0.008(3) -0.005(3) N3A 0.023(3) 0.025(4) 0.026(4) -0.010(3) 0.009(3) 0.005(3) N4C 0.025(3) 0.020(3) 0.024(4) -0.002(3) 0.009(3) -0.001(3) N4B 0.028(4) 0.037(4) 0.029(4) 0.004(3) 0.014(3) -0.005(3) N4A 0.021(3) 0.019(3) 0.037(4) -0.007(3) 0.011(3) 0.001(3) N5C 0.028(4) 0.031(4) 0.023(4) 0.003(3) 0.005(3) 0.008(3) N5B 0.028(4) 0.032(4) 0.024(4) 0.000(3) 0.014(3) -0.002(3) N5A 0.032(4) 0.023(4) 0.033(4) 0.001(3) 0.021(3) 0.002(3) N6B 0.029(4) 0.024(4) 0.015(4) 0.005(3) 0.003(3) 0.005(3) N6A 0.020(3) 0.018(4) 0.027(3) -0.002(3) 0.011(2) 0.000(3) N6C 0.025(4) 0.029(4) 0.012(4) 0.001(3) 0.000(3) -0.001(3) N7C 0.026(4) 0.036(4) 0.029(4) 0.000(3) 0.007(3) 0.007(3) N7B 0.028(4) 0.032(4) 0.027(4) 0.003(3) 0.001(3) -0.005(3) N7A 0.031(4) 0.020(4) 0.022(4) -0.007(3) 0.011(3) -0.007(3) C1C 0.027(4) 0.012(5) 0.037(5) 0.004(3) 0.010(4) 0.003(3) C1B 0.031(5) 0.045(6) 0.029(6) 0.012(5) 0.011(4) -0.009(4) C1A 0.028(5) 0.036(5) 0.022(5) -0.004(4) 0.001(4) 0.001(4) C2C 0.028(4) 0.024(4) 0.021(4) 0.007(3) 0.010(4) 0.001(4) C2B 0.030(5) 0.039(5) 0.043(7) 0.010(5) 0.014(5) -0.008(4) C2A 0.028(4) 0.027(5) 0.030(5) -0.005(4) 0.003(4) -0.001(4) C3C 0.026(4) 0.020(4) 0.018(4) -0.003(3) 0.012(3) -0.001(3) C3B 0.028(4) 0.031(5) 0.021(5) 0.008(4) 0.008(4) 0.006(4) C3A 0.024(4) 0.013(4) 0.025(4) 0.003(3) 0.001(3) -0.001(3) C4C 0.018(4) 0.024(4) 0.021(4) 0.002(3) 0.009(3) 0.004(3) C4B 0.031(4) 0.024(4) 0.018(4) 0.002(3) 0.005(3) 0.006(3) C4A 0.021(4) 0.015(4) 0.029(5) -0.005(3) 0.004(4) 0.000(3) C5C 0.024(4) 0.016(4) 0.022(5) -0.002(3) 0.004(4) -0.001(3) C5B 0.029(4) 0.038(6) 0.012(3) 0.001(4) 0.005(3) 0.001(4) C5A 0.034(5) 0.013(4) 0.028(5) -0.001(4) -0.001(4) 0.002(4) C6C 0.038(5) 0.016(4) 0.032(5) -0.006(4) 0.013(4) -0.005(4) C6B 0.036(5) 0.041(5) 0.023(5) -0.004(4) 0.009(4) -0.011(4) C6A 0.033(5) 0.016(4) 0.040(5) 0.000(4) 0.015(4) 0.002(4) C7C 0.033(4) 0.015(4) 0.039(5) 0.004(3) 0.012(4) 0.002(3) C7B 0.038(5) 0.032(5) 0.026(5) -0.002(4) 0.010(4) -0.006(4) C7A 0.033(4) 0.022(4) 0.026(5) 0.006(3) 0.009(4) 0.000(4) C8C 0.025(4) 0.020(4) 0.027(4) 0.003(3) 0.009(3) 0.005(3) C8B 0.024(4) 0.021(4) 0.026(4) 0.006(3) 0.001(3) 0.003(3) C8A 0.020(4) 0.026(4) 0.019(4) 0.002(3) 0.005(3) -0.005(3) C9C 0.020(4) 0.018(4) 0.024(4) 0.005(3) 0.000(3) 0.004(3) C9B 0.020(4) 0.021(4) 0.035(5) 0.000(3) 0.009(4) -0.003(3) C9A 0.020(4) 0.019(4) 0.026(5) 0.000(3) 0.008(4) -0.006(3) C10C 0.027(5) 0.044(6) 0.016(5) 0.003(4) 0.005(4) 0.003(4) C10A 0.015(3) 0.027(5) 0.026(4) -0.005(3) 0.003(3) -0.001(3) C10B 0.036(5) 0.027(5) 0.033(5) -0.006(4) 0.003(4) -0.003(4) C11C 0.027(4) 0.043(5) 0.022(4) 0.004(4) 0.010(4) 0.006(4) C11A 0.017(4) 0.023(5) 0.029(5) -0.001(4) 0.006(4) 0.003(3) C11B 0.022(5) 0.036(5) 0.025(5) -0.004(4) 0.007(4) -0.001(4) C12C 0.028(4) 0.028(5) 0.035(5) -0.001(4) 0.001(4) -0.003(4) C12B 0.055(7) 0.089(9) 0.037(6) 0.008(6) 0.001(5) -0.041(7) C12A 0.043(6) 0.044(6) 0.036(6) 0.002(4) 0.025(5) 0.014(5) C13C 0.035(5) 0.032(5) 0.061(7) -0.009(5) 0.004(5) 0.007(4) C13B 0.046(6) 0.090(9) 0.033(6) 0.023(5) 0.008(5) -0.022(6) C13A 0.043(5) 0.031(5) 0.031(5) 0.002(4) 0.018(4) 0.012(4) C14C 0.043(6) 0.061(7) 0.043(6) 0.000(5) 0.006(5) 0.031(5) C14B 0.046(6) 0.063(7) 0.039(6) -0.005(5) 0.001(5) -0.025(5) C14A 0.034(4) 0.043(5) 0.034(5) -0.004(4) 0.022(4) -0.008(4) C15C 0.032(5) 0.047(6) 0.028(5) 0.006(4) 0.002(4) 0.001(4) C15B 0.035(5) 0.055(6) 0.037(5) 0.006(5) 0.008(4) -0.010(5) C15A 0.042(5) 0.022(4) 0.040(5) 0.000(4) 0.021(4) 0.002(4) C16 0.075(8) 0.062(9) 0.081(9) 0.005(6) 0.046(7) 0.003(6) C18 0.117(13) 0.070(10) 0.120(14) -0.046(10) 0.062(11) -0.037(10) C17 0.054(6) 0.030(5) 0.055(7) 0.004(5) -0.014(5) -0.004(5) N8 0.284 0.257 0.465 0.035 -0.224 0.131 C19 0.308 0.157 1.372 -0.043 -0.013 0.069 C20 0.858 0.761 0.869 -0.049 -0.441 0.232 _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 N6C 2.608(7) . ? La N3C 2.617(6) . ? La N6A 2.624(6) . ? La N3A 2.629(6) . ? La N1A 2.646(7) . ? La N6B 2.651(8) . ? La N3B 2.655(7) . ? La N1C 2.675(7) . ? La N1B 2.686(6) . ? S1 O1 1.381(9) . ? S1 O2 1.415(6) . ? S1 O3 1.440(9) . ? S1 C16 1.814(12) . ? S2 O6 1.400(7) . ? S2 O5 1.423(6) . ? S2 O4 1.461(8) . ? S2 C17 1.797(10) . ? S3 O7 1.410(11) . ? S3 O9 1.422(9) . ? S3 O8 1.470(8) . ? S3 C18 1.831(15) . ? F1 C16 1.352(13) . ? F2 C16 1.276(14) . ? F3 C16 1.393(15) . ? F4 C17 1.360(14) . ? F5 C17 1.341(12) . ? F6 C17 1.311(12) . ? F7 C18 1.387(16) . ? F8 C18 1.40(2) . ? F9 C18 1.360(19) . ? N1C C4C 1.353(11) . ? N1C C8C 1.358(10) . ? N1B C4B 1.341(9) . ? N1B C8B 1.351(10) . ? N1A C8A 1.352(10) . ? N1A C4A 1.356(10) . ? N2C C1C 1.328(10) . ? N2C N3C 1.363(8) . ? N2B C1B 1.321(11) . ? N2B N3B 1.357(9) . ? N2A C1A 1.337(11) . ? N2A N3A 1.338(9) . ? N3C C3C 1.342(9) . ? N3B C3B 1.301(11) . ? N3A C3A 1.322(10) . ? N4C C2C 1.321(10) . ? N4C C3C 1.350(10) . ? N4B C2B 1.321(12) . ? N4B C3B 1.358(10) . ? N4A C2A 1.321(11) . ? N4A C3A 1.353(10) . ? N5C C11C 1.326(10) . ? N5C N6C 1.364(10) . ? N5B C11B 1.331(11) . ? N5B N6B 1.344(9) . ? N5A C11A 1.338(10) . ? N5A N6A 1.363(9) . ? N6B C9B 1.310(11) . ? N6A C9A 1.312(11) . ? N6C C9C 1.322(11) . ? N7C C10C 1.346(11) . ? N7C C9C 1.364(10) . ? N7B C10B 1.329(11) . ? N7B C9B 1.371(10) . ? N7A C10A 1.311(10) . ? N7A C9A 1.357(10) . ? C1C C2C 1.413(11) . ? C1C C13C 1.527(11) . ? C1B C2B 1.390(14) . ? C1B C12B 1.487(14) . ? C1A C2A 1.428(13) . ? C1A C12A 1.476(13) . ? C2C C12C 1.511(11) . ? C2B C13B 1.537(13) . ? C2A C13A 1.486(12) . ? C3C C4C 1.479(11) . ? C3B C4B 1.504(11) . ? C3A C4A 1.477(11) . ? C4C C5C 1.397(11) . ? C4B C5B 1.396(10) . ? C4A C5A 1.381(11) . ? C5C C6C 1.387(12) . ? C5B C6B 1.394(11) . ? C5A C6A 1.377(12) . ? C6C C7C 1.398(12) . ? C6B C7B 1.362(12) . ? C6A C7A 1.421(11) . ? C7C C8C 1.365(11) . ? C7B C8B 1.383(11) . ? C7A C8A 1.393(11) . ? C8C C9C 1.477(11) . ? C8B C9B 1.465(11) . ? C8A C9A 1.482(11) . ? C10C C11C 1.402(13) . ? C10C C14C 1.495(12) . ? C10A C11A 1.412(11) . ? C10A C14A 1.495(11) . ? C10B C11B 1.412(12) . ? C10B C14B 1.518(12) . ? C11C C15C 1.504(12) . ? C11A C15A 1.471(11) . ? C11B C15B 1.457(13) . ? N8 C19 1.2480 . ? C19 C20 2.0000 . ? 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 N6C La N3C 122.2(2) . . ? N6C La N6A 78.9(2) . . ? N3C La N6A 84.14(18) . . ? N6C La N3A 151.9(2) . . ? N3C La N3A 80.1(2) . . ? N6A La N3A 123.5(2) . . ? N6C La N1A 136.0(2) . . ? N3C La N1A 74.6(2) . . ? N6A La N1A 61.6(2) . . ? N3A La N1A 62.0(2) . . ? N6C La N6B 82.23(19) . . ? N3C La N6B 149.3(2) . . ? N6A La N6B 83.0(2) . . ? N3A La N6B 84.1(2) . . ? N1A La N6B 74.8(2) . . ? N6C La N3B 87.0(2) . . ? N3C La N3B 80.5(2) . . ? N6A La N3B 149.3(2) . . ? N3A La N3B 79.7(2) . . ? N1A La N3B 137.0(2) . . ? N6B La N3B 122.3(2) . . ? N6C La N1C 61.0(2) . . ? N3C La N1C 61.3(2) . . ? N6A La N1C 74.9(2) . . ? N3A La N1C 136.1(2) . . ? N1A La N1C 120.1(2) . . ? N6B La N1C 139.7(2) . . ? N3B La N1C 74.4(2) . . ? N6C La N1B 78.0(2) . . ? N3C La N1B 136.56(18) . . ? N6A La N1B 139.29(17) . . ? N3A La N1B 74.0(2) . . ? N1A La N1B 119.6(2) . . ? N6B La N1B 61.1(2) . . ? N3B La N1B 61.2(2) . . ? N1C La N1B 120.2(2) . . ? O1 S1 O2 116.4(6) . . ? O1 S1 O3 117.3(8) . . ? O2 S1 O3 112.3(5) . . ? O1 S1 C16 103.3(7) . . ? O2 S1 C16 104.4(5) . . ? O3 S1 C16 100.2(6) . . ? O6 S2 O5 119.0(5) . . ? O6 S2 O4 114.1(7) . . ? O5 S2 O4 112.1(5) . . ? O6 S2 C17 103.4(5) . . ? O5 S2 C17 104.3(5) . . ? O4 S2 C17 101.3(6) . . ? O7 S3 O9 118.3(7) . . ? O7 S3 O8 117.2(5) . . ? O9 S3 O8 115.3(5) . . ? O7 S3 C18 100.6(9) . . ? O9 S3 C18 101.1(7) . . ? O8 S3 C18 98.9(6) . . ? C4C N1C C8C 117.7(7) . . ? C4B N1B C8B 117.8(6) . . ? C8A N1A C4A 118.0(7) . . ? C1C N2C N3C 117.4(6) . . ? C1B N2B N3B 118.5(8) . . ? C1A N2A N3A 118.6(7) . . ? C3C N3C N2C 119.1(6) . . ? C3B N3B N2B 119.1(7) . . ? C3A N3A N2A 119.9(7) . . ? C2C N4C C3C 116.0(7) . . ? C2B N4B C3B 113.3(8) . . ? C2A N4A C3A 116.8(7) . . ? C11C N5C N6C 118.4(7) . . ? C11B N5B N6B 118.5(7) . . ? C11A N5A N6A 118.0(6) . . ? C9B N6B N5B 120.9(7) . . ? C9A N6A N5A 119.2(6) . . ? C9C N6C N5C 119.7(7) . . ? C10C N7C C9C 115.0(7) . . ? C10B N7B C9B 115.0(7) . . ? C10A N7A C9A 115.7(7) . . ? N2C C1C C2C 121.9(7) . . ? N2C C1C C13C 116.6(7) . . ? C2C C1C C13C 121.5(7) . . ? N2B C1B C2B 119.7(9) . . ? N2B C1B C12B 116.2(8) . . ? C2B C1B C12B 124.2(8) . . ? N2A C1A C2A 120.2(8) . . ? N2A C1A C12A 116.8(8) . . ? C2A C1A C12A 123.0(8) . . ? N4C C2C C1C 120.3(7) . . ? N4C C2C C12C 118.4(7) . . ? C1C C2C C12C 121.2(7) . . ? N4B C2B C1B 123.2(9) . . ? N4B C2B C13B 115.7(9) . . ? C1B C2B C13B 121.1(9) . . ? N4A C2A C1A 119.6(8) . . ? N4A C2A C13A 119.2(8) . . ? C1A C2A C13A 121.2(8) . . ? N3C C3C N4C 125.1(7) . . ? N3C C3C C4C 116.5(7) . . ? N4C C3C C4C 118.3(6) . . ? N3B C3B N4B 126.2(8) . . ? N3B C3B C4B 118.3(7) . . ? N4B C3B C4B 115.5(7) . . ? N3A C3A N4A 124.4(7) . . ? N3A C3A C4A 118.9(7) . . ? N4A C3A C4A 116.7(6) . . ? N1C C4C C5C 122.4(7) . . ? N1C C4C C3C 117.3(7) . . ? C5C C4C C3C 120.2(7) . . ? N1B C4B C5B 124.2(7) . . ? N1B C4B C3B 116.4(6) . . ? C5B C4B C3B 119.3(7) . . ? N1A C4A C5A 122.2(8) . . ? N1A C4A C3A 116.2(7) . . ? C5A C4A C3A 121.6(7) . . ? C6C C5C C4C 118.7(8) . . ? C6B C5B C4B 116.8(7) . . ? C6A C5A C4A 120.2(8) . . ? C5C C6C C7C 118.8(7) . . ? C7B C6B C5B 119.0(8) . . ? C5A C6A C7A 118.8(7) . . ? C8C C7C C6C 119.3(7) . . ? C6B C7B C8B 121.3(8) . . ? C8A C7A C6A 117.5(7) . . ? N1C C8C C7C 123.0(8) . . ? N1C C8C C9C 115.6(7) . . ? C7C C8C C9C 121.4(7) . . ? N1B C8B C7B 120.7(7) . . ? N1B C8B C9B 116.8(7) . . ? C7B C8B C9B 122.4(7) . . ? N1A C8A C7A 123.4(7) . . ? N1A C8A C9A 117.0(7) . . ? C7A C8A C9A 119.5(7) . . ? N6C C9C N7C 124.8(7) . . ? N6C C9C C8C 117.8(7) . . ? N7C C9C C8C 117.4(7) . . ? N6B C9B N7B 124.0(7) . . ? N6B C9B C8B 118.8(7) . . ? N7B C9B C8B 117.2(7) . . ? N6A C9A N7A 125.2(7) . . ? N6A C9A C8A 117.2(7) . . ? N7A C9A C8A 117.5(7) . . ? N7C C10C C11C 121.3(8) . . ? N7C C10C C14C 116.3(8) . . ? C11C C10C C14C 122.3(8) . . ? N7A C10A C11A 121.3(7) . . ? N7A C10A C14A 118.2(7) . . ? C11A C10A C14A 120.4(7) . . ? N7B C10B C11B 121.8(8) . . ? N7B C10B C14B 117.7(8) . . ? C11B C10B C14B 120.5(8) . . ? N5C C11C C10C 120.6(8) . . ? N5C C11C C15C 117.4(8) . . ? C10C C11C C15C 122.0(8) . . ? N5A C11A C10A 120.0(7) . . ? N5A C11A C15A 116.7(7) . . ? C10A C11A C15A 123.2(7) . . ? N5B C11B C10B 119.4(8) . . ? N5B C11B C15B 117.1(8) . . ? C10B C11B C15B 123.4(8) . . ? F2 C16 F1 109.3(11) . . ? F2 C16 F3 107.8(11) . . ? F1 C16 F3 105.2(10) . . ? F2 C16 S1 115.3(8) . . ? F1 C16 S1 110.4(8) . . ? F3 C16 S1 108.4(10) . . ? F9 C18 F7 101.3(13) . . ? F9 C18 F8 116.2(14) . . ? F7 C18 F8 118.0(15) . . ? F9 C18 S3 109.5(12) . . ? F7 C18 S3 107.2(10) . . ? F8 C18 S3 104.3(11) . . ? F6 C17 F5 108.4(9) . . ? F6 C17 F4 103.9(9) . . ? F5 C17 F4 106.2(8) . . ? F6 C17 S2 114.4(8) . . ? F5 C17 S2 112.8(8) . . ? F4 C17 S2 110.4(8) . . ? N8 C19 C20 164.7 . . ? #===END data_9.MeCN _database_code_CSD 181678 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H48 Ce F9 N22 O9 S3' _chemical_formula_weight 1508.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.240(3) _cell_length_b 17.266(4) _cell_length_c 14.491(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.81(3) _cell_angle_gamma 90.00 _cell_volume 3217.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20089 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1522 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_process_details 'MULABS in PLATON;Spek,1998' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 20s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f rotation scans with 2\%steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20089 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0804 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 24.67 _reflns_number_total 10154 _reflns_number_gt 8669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms were introduced at calculated positions as riding atoms, with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. Some voids (100 A^3^ may indicate the presence of other unresolved solvent molecules. ; _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(16) _refine_ls_number_reflns 10154 _refine_ls_number_parameters 859 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1355 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 24.67 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.847 _refine_diff_density_min -0.639 _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 Ce Ce 0.69064(3) 0.43822(2) 0.32035(3) 0.01995(12) Uani 1 1 d . . . S1 S 0.7644(2) 0.49431(15) 0.73969(18) 0.0411(6) Uani 1 1 d . . . S2 S 0.2267(2) 0.45934(12) 0.38876(19) 0.0416(6) Uani 1 1 d . . . S3 S 0.6754(3) 0.1583(2) 0.0913(3) 0.0290(9) Uani 1 1 d . . . F1 F 0.9392(5) 0.4203(5) 0.7527(5) 0.080(3) Uani 1 1 d . . . F2 F 0.8424(6) 0.3717(4) 0.8364(5) 0.073(2) Uani 1 1 d . . . F3 F 0.8024(8) 0.3556(7) 0.6848(7) 0.116(4) Uani 1 1 d . . . F4 F 0.1778(8) 0.3750(4) 0.2363(6) 0.094(3) Uani 1 1 d . . . F5 F 0.0878(6) 0.3498(4) 0.3382(6) 0.078(2) Uani 1 1 d . . . F6 F 0.0624(6) 0.4530(5) 0.2490(7) 0.111(3) Uani 1 1 d . . . F7 F 0.5868(8) 0.0241(5) 0.0437(9) 0.123(4) Uani 1 1 d . . . F8 F 0.6447(8) 0.0473(6) 0.2021(7) 0.114(3) Uani 1 1 d . . . F9 F 0.5008(7) 0.0984(5) 0.1175(9) 0.122(4) Uani 1 1 d . . . O1 O 0.7743(8) 0.5217(7) 0.6505(7) 0.079(3) Uani 1 1 d . . . O2 O 0.6636(5) 0.4703(4) 0.7463(5) 0.056(2) Uani 1 1 d . . . O3 O 0.8177(6) 0.5410(4) 0.8179(6) 0.057(2) Uani 1 1 d . . . O4 O 0.1601(9) 0.4909(6) 0.4451(8) 0.101(4) Uani 1 1 d . . . O5 O 0.2646(6) 0.5179(4) 0.3367(5) 0.0436(17) Uani 1 1 d . . . O6 O 0.2959(7) 0.4002(5) 0.4311(8) 0.097(4) Uani 1 1 d . . . O7 O 0.6184(10) 0.1781(6) -0.0013(7) 0.100(4) Uani 1 1 d . . . O8 O 0.6683(6) 0.2077(5) 0.1689(6) 0.067(2) Uani 1 1 d . . . O9 O 0.7724(6) 0.1238(5) 0.0982(6) 0.068(2) Uani 1 1 d . . . N1C N 0.7141(6) 0.5749(4) 0.4033(6) 0.0222(18) Uani 1 1 d . . . N1B N 0.6438(5) 0.4295(4) 0.1318(4) 0.0219(13) Uani 1 1 d . . . N1A N 0.7161(6) 0.3102(4) 0.4204(6) 0.0235(18) Uani 1 1 d . . . N2C N 0.9231(5) 0.4036(4) 0.4833(5) 0.0255(15) Uani 1 1 d . . . N2B N 0.8739(6) 0.5688(4) 0.2795(5) 0.0295(16) Uani 1 1 d . . . N2A N 0.8471(6) 0.3415(4) 0.1976(5) 0.0275(16) Uani 1 1 d . . . N3C N 0.8573(5) 0.4630(3) 0.4554(5) 0.0250(16) Uani 1 1 d . . . N3B N 0.7974(5) 0.5235(4) 0.2273(5) 0.0243(16) Uani 1 1 d . . . N3A N 0.8116(5) 0.3329(4) 0.2757(5) 0.0220(15) Uani 1 1 d . . . N4C N 0.9667(5) 0.5491(4) 0.5621(5) 0.0217(14) Uani 1 1 d . . . N4B N 0.8370(5) 0.5629(4) 0.0824(5) 0.0294(17) Uani 1 1 d . . . N4A N 0.9023(5) 0.2143(4) 0.3117(5) 0.0272(16) Uani 1 1 d . . . N5C N 0.4552(5) 0.5135(4) 0.2057(5) 0.0292(16) Uani 1 1 d . . . N5B N 0.4947(6) 0.3016(4) 0.2918(5) 0.0269(16) Uani 1 1 d . . . N5A N 0.5455(5) 0.4898(4) 0.4815(5) 0.0247(15) Uani 1 1 d . . . N6B N 0.5433(6) 0.3431(4) 0.2359(5) 0.0257(18) Uani 1 1 d . . . N6A N 0.5984(5) 0.4261(4) 0.4608(4) 0.0191(15) Uani 1 1 d . . . N6C N 0.5428(6) 0.5374(4) 0.2697(5) 0.0237(17) Uani 1 1 d . . . N7C N 0.4644(5) 0.6593(4) 0.2862(5) 0.0302(17) Uani 1 1 d . . . N7B N 0.4278(6) 0.2974(4) 0.0955(5) 0.0325(17) Uani 1 1 d . . . N7A N 0.5456(5) 0.3493(4) 0.5752(5) 0.0225(14) Uani 1 1 d . . . N8 N 1.1151(13) 0.3510(10) 0.9538(15) 0.136(6) Uani 1 1 d . . . C1C C 1.0092(6) 0.4167(4) 0.5486(6) 0.024(2) Uani 1 1 d . . . C1B C 0.9296(7) 0.6124(6) 0.2328(7) 0.030(2) Uani 1 1 d . . . C1A C 0.9039(7) 0.2868(6) 0.1725(8) 0.033(2) Uani 1 1 d . . . C2C C 1.0301(7) 0.4919(5) 0.5885(7) 0.029(2) Uani 1 1 d . . . C2B C 0.9103(7) 0.6093(6) 0.1349(8) 0.037(2) Uani 1 1 d . . . C2A C 0.9393(7) 0.2217(5) 0.2367(6) 0.029(2) Uani 1 1 d . . . C3C C 0.8799(6) 0.5327(4) 0.4972(6) 0.0219(17) Uani 1 1 d . . . C3B C 0.7837(6) 0.5208(5) 0.1354(6) 0.0232(18) Uani 1 1 d . . . C3A C 0.8369(6) 0.2683(4) 0.3276(6) 0.0227(17) Uani 1 1 d . . . C4C C 0.8011(6) 0.5945(4) 0.4684(6) 0.0211(17) Uani 1 1 d . . . C4B C 0.7005(6) 0.4695(4) 0.0808(6) 0.0239(17) Uani 1 1 d . . . C4A C 0.7854(6) 0.2549(4) 0.4067(6) 0.0199(16) Uani 1 1 d . . . C5C C 0.8154(7) 0.6669(5) 0.5113(7) 0.0282(19) Uani 1 1 d . . . H5CB H 0.888(7) 0.673(5) 0.555(7) 0.034 Uiso 1 1 d . . . C5B C 0.6860(7) 0.4602(5) -0.0160(7) 0.035(2) Uani 1 1 d . . . H5BB H 0.7233 0.4902 -0.0495 0.042 Uiso 1 1 calc R . . C5A C 0.8049(6) 0.1877(5) 0.4614(6) 0.0267(19) Uani 1 1 d . . . H5AB H 0.8538 0.1517 0.4518 0.032 Uiso 1 1 calc R . . C6C C 0.7379(7) 0.7208(5) 0.4886(7) 0.030(2) Uani 1 1 d . . . H6CA H 0.7469 0.7695 0.5165 0.036 Uiso 1 1 calc R . . C6B C 0.6158(9) 0.4060(6) -0.0624(7) 0.047(3) Uani 1 1 d . . . H6BA H 0.6071 0.3969 -0.1270 0.056 Uiso 1 1 calc R . . C6A C 0.7507(7) 0.1758(5) 0.5293(7) 0.028(2) Uani 1 1 d . . . H6AA H 0.7600 0.1304 0.5650 0.033 Uiso 1 1 calc R . . C7C C 0.6434(7) 0.7022(4) 0.4222(6) 0.0286(19) Uani 1 1 d . . . H7CB H 0.5886 0.7372 0.4068 0.034 Uiso 1 1 calc R . . C7B C 0.5581(8) 0.3653(6) -0.0095(7) 0.044(2) Uani 1 1 d . . . H7BB H 0.5101 0.3282 -0.0388 0.053 Uiso 1 1 calc R . . C7A C 0.6808(7) 0.2325(4) 0.5449(6) 0.0263(18) Uani 1 1 d . . . H7AB H 0.6441 0.2254 0.5916 0.032 Uiso 1 1 calc R . . C8C C 0.6369(6) 0.6295(4) 0.3817(6) 0.0239(17) Uani 1 1 d . . . C8B C 0.5723(6) 0.3801(5) 0.0864(6) 0.0275(19) Uani 1 1 d . . . C8A C 0.6668(6) 0.2991(4) 0.4903(6) 0.0233(17) Uani 1 1 d . . . C9C C 0.5432(6) 0.6065(4) 0.3093(6) 0.0231(18) Uani 1 1 d . . . C9B C 0.5129(6) 0.3386(5) 0.1422(6) 0.0261(18) Uani 1 1 d . . . C9A C 0.5994(6) 0.3616(4) 0.5084(6) 0.0193(17) Uani 1 1 d . . . C10C C 0.3812(7) 0.6361(6) 0.2243(7) 0.032(2) Uani 1 1 d . . . C10A C 0.4942(6) 0.4099(4) 0.5975(6) 0.0208(18) Uani 1 1 d . . . C10B C 0.3772(7) 0.2566(5) 0.1489(7) 0.035(2) Uani 1 1 d . . . C11C C 0.3746(6) 0.5595(5) 0.1847(6) 0.0283(19) Uani 1 1 d . . . C11A C 0.4959(6) 0.4818(4) 0.5510(6) 0.0200(17) Uani 1 1 d . . . C11B C 0.4152(8) 0.2585(5) 0.2496(7) 0.033(2) Uani 1 1 d . . . C12C C 1.1295(6) 0.5064(5) 0.6629(6) 0.0316(19) Uani 1 1 d . . . H12A H 1.1320 0.5596 0.6826 0.047 Uiso 1 1 calc R . . H12B H 1.1881 0.4954 0.6367 0.047 Uiso 1 1 calc R . . H12C H 1.1317 0.4734 0.7167 0.047 Uiso 1 1 calc R . . C12B C 1.0149(9) 0.6618(7) 0.2947(8) 0.054(3) Uani 1 1 d . . . H12D H 1.0146 0.6546 0.3604 0.081 Uiso 1 1 calc R . . H12E H 1.0026 0.7153 0.2781 0.081 Uiso 1 1 calc R . . H12F H 1.0812 0.6465 0.2848 0.081 Uiso 1 1 calc R . . C12A C 0.9320(8) 0.2969(6) 0.0815(7) 0.045(2) Uani 1 1 d . . . H12G H 0.9013 0.3437 0.0517 0.068 Uiso 1 1 calc R . . H12H H 0.9069 0.2536 0.0409 0.068 Uiso 1 1 calc R . . H12I H 1.0063 0.3000 0.0921 0.068 Uiso 1 1 calc R . . C13C C 1.0813(7) 0.3484(5) 0.5778(7) 0.034(2) Uani 1 1 d . . . H13A H 1.0523 0.3035 0.5420 0.051 Uiso 1 1 calc R . . H13B H 1.0895 0.3384 0.6444 0.051 Uiso 1 1 calc R . . H13C H 1.1479 0.3599 0.5656 0.051 Uiso 1 1 calc R . . C13B C 0.9709(8) 0.6578(7) 0.0809(8) 0.052(3) Uani 1 1 d . . . H13D H 0.9462 0.6481 0.0140 0.078 Uiso 1 1 calc R . . H13E H 1.0433 0.6446 0.1005 0.078 Uiso 1 1 calc R . . H13F H 0.9619 0.7116 0.0936 0.078 Uiso 1 1 calc R . . C13A C 1.0153(7) 0.1647(5) 0.2176(6) 0.034(2) Uani 1 1 d . . . H13G H 1.0282 0.1260 0.2666 0.050 Uiso 1 1 calc R . . H13H H 1.0792 0.1906 0.2166 0.050 Uiso 1 1 calc R . . H13I H 0.9878 0.1405 0.1572 0.050 Uiso 1 1 calc R . . C14C C 0.2935(8) 0.6940(7) 0.1928(8) 0.053(3) Uani 1 1 d . . . H14A H 0.3116 0.7418 0.2265 0.080 Uiso 1 1 calc R . . H14B H 0.2310 0.6737 0.2063 0.080 Uiso 1 1 calc R . . H14C H 0.2824 0.7031 0.1258 0.080 Uiso 1 1 calc R . . C14B C 0.2832(8) 0.2130(7) 0.1013(8) 0.054(3) Uani 1 1 d . . . H14D H 0.2715 0.2192 0.0337 0.081 Uiso 1 1 calc R . . H14E H 0.2243 0.2324 0.1219 0.081 Uiso 1 1 calc R . . H14F H 0.2928 0.1591 0.1172 0.081 Uiso 1 1 calc R . . C14A C 0.4344(7) 0.4004(5) 0.6705(7) 0.033(2) Uani 1 1 d . . . H14G H 0.4422 0.3484 0.6944 0.050 Uiso 1 1 calc R . . H14H H 0.3622 0.4107 0.6430 0.050 Uiso 1 1 calc R . . H14I H 0.4599 0.4360 0.7216 0.050 Uiso 1 1 calc R . . C15C C 0.2764(7) 0.5306(6) 0.1183(7) 0.041(2) Uani 1 1 d . . . H15A H 0.2867 0.4784 0.0995 0.061 Uiso 1 1 calc R . . H15B H 0.2595 0.5631 0.0631 0.061 Uiso 1 1 calc R . . H15C H 0.2205 0.5317 0.1500 0.061 Uiso 1 1 calc R . . C15B C 0.3622(8) 0.2128(6) 0.3113(7) 0.040(2) Uani 1 1 d . . . H15D H 0.3969 0.2208 0.3767 0.061 Uiso 1 1 calc R . . H15E H 0.3644 0.1588 0.2961 0.061 Uiso 1 1 calc R . . H15F H 0.2911 0.2293 0.3009 0.061 Uiso 1 1 calc R . . C15A C 0.4438(7) 0.5519(5) 0.5758(7) 0.035(2) Uani 1 1 d . . . H15G H 0.4543 0.5941 0.5361 0.053 Uiso 1 1 calc R . . H15H H 0.4727 0.5649 0.6412 0.053 Uiso 1 1 calc R . . H15I H 0.3707 0.5420 0.5663 0.053 Uiso 1 1 calc R . . C16 C 0.8421(9) 0.4065(6) 0.7558(8) 0.056(3) Uani 1 1 d . . . C18 C 0.6006(11) 0.0759(8) 0.1173(11) 0.074(4) Uani 1 1 d . . . C17 C 0.1338(9) 0.4081(6) 0.3019(9) 0.050(3) Uani 1 1 d . . . C19 C 1.0853(15) 0.4152(9) 0.9612(18) 0.116(7) Uani 1 1 d . . . C20 C 1.0407(15) 0.4901(10) 0.9713(14) 0.123(8) Uani 1 1 d . . . H20A H 1.0638 0.5269 0.9311 0.185 Uiso 1 1 calc R . . H20B H 1.0624 0.5068 1.0363 0.185 Uiso 1 1 calc R . . H20C H 0.9662 0.4866 0.9533 0.185 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 0.0240(2) 0.0163(2) 0.0217(2) 0.0002(2) 0.00963(14) -0.0002(2) S1 0.0389(14) 0.0533(16) 0.0321(13) 0.0080(11) 0.0104(11) -0.0129(11) S2 0.0515(15) 0.0301(16) 0.0441(14) 0.0012(9) 0.0130(12) -0.0155(9) S3 0.034(2) 0.0274(19) 0.028(2) -0.0039(14) 0.0125(16) -0.0067(14) F1 0.069(4) 0.109(8) 0.073(4) 0.005(4) 0.036(4) 0.022(4) F2 0.089(6) 0.059(5) 0.073(5) 0.019(4) 0.026(4) -0.007(4) F3 0.147(10) 0.096(8) 0.108(9) -0.057(6) 0.034(7) -0.015(6) F4 0.142(8) 0.060(5) 0.081(6) -0.028(4) 0.030(5) -0.021(5) F5 0.074(5) 0.072(5) 0.078(5) -0.001(4) -0.001(4) -0.041(4) F6 0.081(5) 0.051(6) 0.162(8) 0.010(5) -0.047(5) 0.009(4) F7 0.141(8) 0.070(6) 0.191(11) -0.071(6) 0.107(8) -0.059(5) F8 0.108(7) 0.135(8) 0.105(7) 0.071(7) 0.041(6) 0.010(6) F9 0.087(6) 0.106(7) 0.204(11) -0.057(7) 0.098(7) -0.048(5) O1 0.072(6) 0.117(9) 0.058(6) 0.039(6) 0.035(5) 0.004(6) O2 0.038(4) 0.088(6) 0.044(4) -0.005(3) 0.015(3) -0.027(3) O3 0.055(5) 0.045(5) 0.071(6) -0.016(4) 0.014(4) -0.013(4) O4 0.139(9) 0.086(7) 0.117(8) -0.055(6) 0.105(8) -0.074(6) O5 0.067(5) 0.034(4) 0.039(4) -0.001(3) 0.030(4) -0.012(3) O6 0.077(6) 0.045(5) 0.130(9) 0.037(5) -0.054(6) -0.017(4) O7 0.166(11) 0.077(7) 0.073(7) 0.014(5) 0.062(7) 0.025(6) O8 0.064(5) 0.072(6) 0.070(6) -0.041(4) 0.023(4) -0.014(4) O9 0.048(5) 0.074(6) 0.081(6) -0.040(5) 0.017(4) 0.001(4) N1C 0.023(4) 0.024(4) 0.027(4) 0.002(3) 0.022(3) 0.003(3) N1B 0.032(3) 0.014(4) 0.023(3) 0.000(3) 0.012(2) -0.004(3) N1A 0.030(4) 0.018(4) 0.021(4) -0.003(3) 0.005(3) 0.002(3) N2C 0.024(4) 0.022(3) 0.032(4) 0.004(3) 0.009(3) 0.004(3) N2B 0.026(4) 0.029(4) 0.036(4) 0.004(3) 0.013(3) -0.007(3) N2A 0.027(4) 0.031(4) 0.025(4) 0.004(3) 0.008(3) 0.011(3) N3C 0.027(4) 0.025(4) 0.024(4) -0.002(2) 0.009(3) 0.001(3) N3B 0.025(4) 0.026(4) 0.023(4) 0.001(3) 0.006(3) 0.000(3) N3A 0.020(4) 0.020(4) 0.030(4) -0.002(3) 0.014(3) 0.001(3) N4C 0.019(3) 0.024(4) 0.023(4) -0.004(3) 0.007(3) -0.003(3) N4B 0.021(4) 0.034(4) 0.038(4) 0.009(3) 0.015(3) -0.010(3) N4A 0.031(4) 0.021(4) 0.028(4) -0.003(3) 0.004(3) 0.002(3) N5C 0.033(4) 0.032(4) 0.022(4) 0.000(3) 0.006(3) 0.000(3) N5B 0.026(4) 0.033(4) 0.025(4) 0.001(3) 0.011(3) 0.000(3) N5A 0.018(4) 0.026(4) 0.033(4) -0.004(3) 0.013(3) 0.000(3) N6B 0.021(4) 0.026(4) 0.029(5) 0.000(3) 0.003(3) 0.000(3) N6A 0.022(3) 0.013(4) 0.024(3) -0.003(3) 0.008(2) 0.000(3) N6C 0.025(4) 0.023(4) 0.022(4) -0.004(3) 0.004(3) 0.000(3) N7C 0.025(4) 0.033(4) 0.034(5) 0.000(3) 0.008(3) 0.001(3) N7B 0.033(4) 0.042(4) 0.022(4) 0.002(3) 0.005(3) -0.008(3) N7A 0.025(4) 0.021(3) 0.024(4) 0.000(3) 0.010(3) -0.009(3) N8 0.121(14) 0.104(13) 0.183(19) 0.024(11) 0.037(12) 0.034(11) C1C 0.021(4) 0.015(5) 0.038(5) 0.006(3) 0.013(4) -0.005(3) C1B 0.026(5) 0.035(5) 0.032(5) 0.005(4) 0.011(4) -0.005(4) C1A 0.024(5) 0.037(5) 0.042(7) -0.007(4) 0.012(5) 0.001(4) C2C 0.030(5) 0.022(5) 0.040(6) 0.004(4) 0.021(4) 0.001(4) C2B 0.030(5) 0.035(5) 0.048(7) 0.008(4) 0.012(5) -0.006(4) C2A 0.042(5) 0.016(5) 0.032(5) 0.001(4) 0.014(4) 0.006(4) C3C 0.022(4) 0.022(4) 0.025(4) -0.001(3) 0.013(4) -0.002(3) C3B 0.015(4) 0.030(5) 0.030(5) 0.001(4) 0.017(4) 0.000(3) C3A 0.024(4) 0.024(4) 0.020(4) -0.001(3) 0.005(3) 0.005(3) C4C 0.019(4) 0.020(4) 0.025(5) -0.001(3) 0.008(3) -0.003(3) C4B 0.030(4) 0.023(4) 0.020(4) 0.005(3) 0.008(4) 0.005(3) C4A 0.022(4) 0.020(4) 0.018(4) -0.007(3) 0.004(3) -0.003(3) C5C 0.035(5) 0.018(4) 0.034(5) -0.003(4) 0.015(4) -0.007(4) C5B 0.034(5) 0.038(6) 0.037(5) 0.007(3) 0.014(4) -0.002(3) C5A 0.026(5) 0.020(4) 0.034(5) -0.008(3) 0.008(4) -0.001(3) C6C 0.038(5) 0.018(5) 0.037(6) -0.006(4) 0.014(5) -0.004(4) C6B 0.060(7) 0.055(6) 0.025(5) -0.004(4) 0.012(5) -0.024(5) C6A 0.026(5) 0.021(5) 0.035(6) 0.008(4) 0.006(4) 0.004(3) C7C 0.036(5) 0.013(4) 0.039(5) 0.002(3) 0.015(4) 0.003(3) C7B 0.043(6) 0.060(7) 0.032(6) -0.010(5) 0.013(5) -0.021(5) C7A 0.042(5) 0.023(4) 0.016(4) 0.003(3) 0.012(4) -0.002(4) C8C 0.032(5) 0.016(4) 0.027(4) 0.002(3) 0.013(4) 0.006(3) C8B 0.025(4) 0.027(5) 0.029(5) 0.008(3) 0.004(4) 0.001(3) C8A 0.027(4) 0.023(4) 0.023(4) 0.000(3) 0.011(4) -0.004(3) C9C 0.015(4) 0.017(4) 0.040(5) 0.007(3) 0.013(4) 0.003(3) C9B 0.018(4) 0.032(5) 0.027(5) 0.000(3) 0.002(4) -0.001(3) C9A 0.013(4) 0.015(4) 0.028(5) -0.001(3) 0.002(3) -0.004(3) C10C 0.025(5) 0.046(6) 0.028(6) 0.004(4) 0.014(4) 0.010(4) C10A 0.019(4) 0.024(4) 0.019(4) -0.003(3) 0.003(3) -0.008(3) C10B 0.030(5) 0.034(5) 0.043(6) 0.005(4) 0.011(4) -0.003(4) C11C 0.017(4) 0.046(5) 0.024(5) 0.012(4) 0.008(3) 0.004(4) C11A 0.017(4) 0.020(4) 0.019(4) -0.001(3) -0.004(3) -0.004(3) C11B 0.033(6) 0.036(6) 0.033(6) -0.002(4) 0.012(5) -0.003(4) C12C 0.024(4) 0.032(5) 0.033(5) 0.004(4) -0.005(4) -0.005(4) C12B 0.059(7) 0.065(7) 0.041(6) -0.009(5) 0.016(6) -0.032(6) C12A 0.049(6) 0.055(6) 0.035(6) 0.004(5) 0.019(5) 0.014(5) C13C 0.028(5) 0.033(5) 0.037(6) -0.001(4) -0.001(4) 0.001(4) C13B 0.041(6) 0.069(7) 0.051(7) 0.014(5) 0.022(5) -0.019(5) C13A 0.038(5) 0.037(5) 0.030(5) 0.001(4) 0.015(4) 0.010(4) C14C 0.033(6) 0.073(8) 0.053(7) 0.001(5) 0.008(5) 0.024(5) C14B 0.045(6) 0.062(7) 0.053(7) -0.004(5) 0.009(5) -0.032(5) C14A 0.033(5) 0.028(4) 0.040(5) 0.003(4) 0.010(4) -0.005(4) C15C 0.027(5) 0.052(6) 0.042(6) 0.008(4) 0.006(4) -0.001(4) C15B 0.044(6) 0.047(6) 0.036(6) 0.006(4) 0.020(5) -0.021(5) C15A 0.039(5) 0.034(5) 0.041(6) 0.000(4) 0.027(5) 0.008(4) C16 0.065(8) 0.060(7) 0.046(7) -0.012(5) 0.022(6) -0.032(5) C18 0.077(10) 0.076(9) 0.083(10) -0.007(8) 0.045(8) -0.020(8) C17 0.048(7) 0.037(6) 0.062(7) 0.015(5) 0.008(6) 0.005(5) C19 0.087(12) 0.061(13) 0.19(2) 0.018(10) 0.010(13) 0.007(8) C20 0.120(15) 0.074(11) 0.124(16) 0.000(10) -0.074(12) -0.001(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce N6C 2.573(7) . ? Ce N3A 2.605(6) . ? Ce N3C 2.611(7) . ? Ce N6A 2.619(6) . ? Ce N6B 2.620(7) . ? Ce N1A 2.620(8) . ? Ce N3B 2.625(7) . ? Ce N1C 2.633(8) . ? Ce N1B 2.658(6) . ? S1 O1 1.412(9) . ? S1 O2 1.423(7) . ? S1 O3 1.432(8) . ? S1 C16 1.816(13) . ? S2 O6 1.411(8) . ? S2 O5 1.423(6) . ? S2 O4 1.443(9) . ? S2 C17 1.773(12) . ? S3 O9 1.398(9) . ? S3 O7 1.417(12) . ? S3 O8 1.432(8) . ? S3 C18 1.823(13) . ? F1 C16 1.319(13) . ? F2 C16 1.312(13) . ? F3 C16 1.361(14) . ? F4 C17 1.354(14) . ? F5 C17 1.346(12) . ? F6 C17 1.318(12) . ? F7 C18 1.371(16) . ? F8 C18 1.325(17) . ? F9 C18 1.378(16) . ? N1C C4C 1.346(11) . ? N1C C8C 1.371(11) . ? N1B C8B 1.327(11) . ? N1B C4B 1.361(10) . ? N1A C8A 1.344(11) . ? N1A C4A 1.372(10) . ? N2C C1C 1.316(11) . ? N2C N3C 1.343(8) . ? N2B C1B 1.345(11) . ? N2B N3B 1.359(10) . ? N2A C1A 1.313(12) . ? N2A N3A 1.333(9) . ? N3C C3C 1.350(10) . ? N3B C3B 1.301(12) . ? N3A C3A 1.341(10) . ? N4C C2C 1.294(10) . ? N4C C3C 1.330(10) . ? N4B C2B 1.346(12) . ? N4B C3B 1.370(10) . ? N4A C2A 1.302(11) . ? N4A C3A 1.330(10) . ? N5C C11C 1.306(10) . ? N5C N6C 1.365(10) . ? N5B C11B 1.315(12) . ? N5B N6B 1.353(10) . ? N5A C11A 1.334(11) . ? N5A N6A 1.376(9) . ? N6B C9B 1.323(11) . ? N6A C9A 1.308(10) . ? N6C C9C 1.323(11) . ? N7C C10C 1.306(12) . ? N7C C9C 1.364(10) . ? N7B C10B 1.339(11) . ? N7B C9B 1.368(11) . ? N7A C10A 1.328(10) . ? N7A C9A 1.348(10) . ? N8 C19 1.19(2) . ? C1C C2C 1.421(12) . ? C1C C13C 1.513(11) . ? C1B C2B 1.381(14) . ? C1B C12B 1.524(13) . ? C1A C2A 1.462(13) . ? C1A C12A 1.464(14) . ? C2C C12C 1.510(12) . ? C2B C13B 1.503(13) . ? C2A C13A 1.480(12) . ? C3C C4C 1.480(11) . ? C3B C4B 1.485(12) . ? C3A C4A 1.485(11) . ? C4C C5C 1.389(11) . ? C4B C5B 1.378(12) . ? C4A C5A 1.395(11) . ? C5C C6C 1.365(13) . ? C5B C6B 1.376(12) . ? C5A C6A 1.365(12) . ? C6C C7C 1.421(13) . ? C6B C7B 1.395(14) . ? C6A C7A 1.402(12) . ? C7C C8C 1.379(11) . ? C7B C8B 1.381(13) . ? C7A C8A 1.382(11) . ? C8C C9C 1.476(12) . ? C8B C9B 1.445(11) . ? C8A C9A 1.465(11) . ? C10C C11C 1.436(13) . ? C10C C14C 1.518(13) . ? C10A C11A 1.416(10) . ? C10A C14A 1.474(12) . ? C10B C11B 1.425(14) . ? C10B C14B 1.476(13) . ? C11C C15C 1.506(12) . ? C11A C15A 1.478(11) . ? C11B C15B 1.488(12) . ? C19 C20 1.44(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6C Ce N3A 149.9(2) . . ? N6C Ce N3C 123.7(2) . . ? N3A Ce N3C 80.8(2) . . ? N6C Ce N6A 79.1(2) . . ? N3A Ce N6A 124.4(2) . . ? N3C Ce N6A 84.17(19) . . ? N6C Ce N6B 81.54(19) . . ? N3A Ce N6B 83.1(2) . . ? N3C Ce N6B 148.7(2) . . ? N6A Ce N6B 83.1(2) . . ? N6C Ce N1A 135.1(2) . . ? N3A Ce N1A 62.8(2) . . ? N3C Ce N1A 75.5(2) . . ? N6A Ce N1A 61.6(2) . . ? N6B Ce N1A 73.3(2) . . ? N6C Ce N3B 86.9(2) . . ? N3A Ce N3B 80.0(2) . . ? N3C Ce N3B 80.3(2) . . ? N6A Ce N3B 148.4(2) . . ? N6B Ce N3B 122.9(2) . . ? N1A Ce N3B 138.0(2) . . ? N6C Ce N1C 62.1(2) . . ? N3A Ce N1C 136.6(2) . . ? N3C Ce N1C 61.6(2) . . ? N6A Ce N1C 75.1(2) . . ? N6B Ce N1C 140.3(2) . . ? N1A Ce N1C 121.2(2) . . ? N3B Ce N1C 73.3(2) . . ? N6C Ce N1B 76.7(2) . . ? N3A Ce N1B 73.2(2) . . ? N3C Ce N1B 136.68(19) . . ? N6A Ce N1B 139.15(18) . . ? N6B Ce N1B 61.3(2) . . ? N1A Ce N1B 119.3(2) . . ? N3B Ce N1B 61.7(2) . . ? N1C Ce N1B 119.5(2) . . ? O1 S1 O2 117.0(6) . . ? O1 S1 O3 113.6(6) . . ? O2 S1 O3 113.8(5) . . ? O1 S1 C16 102.9(6) . . ? O2 S1 C16 105.1(5) . . ? O3 S1 C16 102.2(5) . . ? O6 S2 O5 118.1(6) . . ? O6 S2 O4 116.6(8) . . ? O5 S2 O4 111.8(5) . . ? O6 S2 C17 102.4(5) . . ? O5 S2 C17 104.6(5) . . ? O4 S2 C17 100.1(6) . . ? O9 S3 O7 116.3(6) . . ? O9 S3 O8 115.4(6) . . ? O7 S3 O8 118.7(6) . . ? O9 S3 C18 100.9(6) . . ? O7 S3 C18 101.0(7) . . ? O8 S3 C18 99.3(6) . . ? C4C N1C C8C 117.0(7) . . ? C8B N1B C4B 118.6(6) . . ? C8A N1A C4A 118.1(7) . . ? C1C N2C N3C 118.3(7) . . ? C1B N2B N3B 117.9(7) . . ? C1A N2A N3A 119.8(8) . . ? N2C N3C C3C 119.1(7) . . ? C3B N3B N2B 119.6(7) . . ? N2A N3A C3A 118.5(6) . . ? C2C N4C C3C 115.9(7) . . ? C2B N4B C3B 113.4(8) . . ? C2A N4A C3A 117.7(7) . . ? C11C N5C N6C 119.2(7) . . ? C11B N5B N6B 117.6(8) . . ? C11A N5A N6A 116.8(6) . . ? C9B N6B N5B 120.8(7) . . ? C9A N6A N5A 120.4(6) . . ? C9C N6C N5C 118.8(7) . . ? C10C N7C C9C 115.7(8) . . ? C10B N7B C9B 117.0(8) . . ? C10A N7A C9A 116.1(6) . . ? N2C C1C C2C 120.1(7) . . ? N2C C1C C13C 116.6(7) . . ? C2C C1C C13C 123.3(8) . . ? N2B C1B C2B 120.4(9) . . ? N2B C1B C12B 115.8(8) . . ? C2B C1B C12B 123.8(8) . . ? N2A C1A C2A 119.6(9) . . ? N2A C1A C12A 116.8(9) . . ? C2A C1A C12A 123.6(8) . . ? N4C C2C C1C 121.9(8) . . ? N4C C2C C12C 118.5(8) . . ? C1C C2C C12C 119.6(8) . . ? N4B C2B C1B 122.5(9) . . ? N4B C2B C13B 116.0(9) . . ? C1B C2B C13B 121.5(9) . . ? N4A C2A C1A 118.7(8) . . ? N4A C2A C13A 119.9(8) . . ? C1A C2A C13A 121.4(8) . . ? N4C C3C N3C 124.7(7) . . ? N4C C3C C4C 118.5(7) . . ? N3C C3C C4C 116.8(7) . . ? N3B C3B N4B 126.2(8) . . ? N3B C3B C4B 118.1(7) . . ? N4B C3B C4B 115.7(7) . . ? N4A C3A N3A 124.9(7) . . ? N4A C3A C4A 117.4(7) . . ? N3A C3A C4A 117.6(6) . . ? N1C C4C C5C 122.8(8) . . ? N1C C4C C3C 116.4(7) . . ? C5C C4C C3C 120.7(8) . . ? N1B C4B C5B 122.2(7) . . ? N1B C4B C3B 116.6(7) . . ? C5B C4B C3B 121.1(7) . . ? N1A C4A C5A 122.5(8) . . ? N1A C4A C3A 116.7(7) . . ? C5A C4A C3A 120.8(7) . . ? C6C C5C C4C 119.4(9) . . ? C6B C5B C4B 119.4(8) . . ? C6A C5A C4A 118.5(7) . . ? C5C C6C C7C 119.9(8) . . ? C5B C6B C7B 118.0(9) . . ? C5A C6A C7A 119.5(8) . . ? C8C C7C C6C 116.7(8) . . ? C8B C7B C6B 119.9(9) . . ? C8A C7A C6A 119.4(8) . . ? N1C C8C C7C 124.1(8) . . ? N1C C8C C9C 115.6(7) . . ? C7C C8C C9C 120.2(7) . . ? N1B C8B C7B 121.8(8) . . ? N1B C8B C9B 117.5(7) . . ? C7B C8B C9B 120.6(8) . . ? N1A C8A C7A 121.9(7) . . ? N1A C8A C9A 117.1(7) . . ? C7A C8A C9A 121.0(7) . . ? N6C C9C N7C 124.9(8) . . ? N6C C9C C8C 117.8(7) . . ? N7C C9C C8C 117.3(7) . . ? N6B C9B N7B 123.5(7) . . ? N6B C9B C8B 118.2(7) . . ? N7B C9B C8B 118.4(7) . . ? N6A C9A N7A 125.0(7) . . ? N6A C9A C8A 117.5(7) . . ? N7A C9A C8A 117.5(7) . . ? N7C C10C C11C 121.2(8) . . ? N7C C10C C14C 117.7(9) . . ? C11C C10C C14C 121.1(9) . . ? N7A C10A C11A 120.5(7) . . ? N7A C10A C14A 118.8(7) . . ? C11A C10A C14A 120.7(7) . . ? N7B C10B C11B 118.5(8) . . ? N7B C10B C14B 118.6(9) . . ? C11B C10B C14B 122.9(9) . . ? N5C C11C C10C 119.9(8) . . ? N5C C11C C15C 118.7(8) . . ? C10C C11C C15C 121.5(8) . . ? N5A C11A C10A 121.1(7) . . ? N5A C11A C15A 116.2(7) . . ? C10A C11A C15A 122.7(7) . . ? N5B C11B C10B 122.5(8) . . ? N5B C11B C15B 117.4(9) . . ? C10B C11B C15B 120.0(8) . . ? F2 C16 F1 108.5(10) . . ? F2 C16 F3 107.2(10) . . ? F1 C16 F3 107.1(10) . . ? F2 C16 S1 112.2(8) . . ? F1 C16 S1 111.8(8) . . ? F3 C16 S1 109.7(9) . . ? F8 C18 F7 115.2(14) . . ? F8 C18 F9 108.3(11) . . ? F7 C18 F9 103.7(12) . . ? F6 C17 F5 109.8(10) . . ? F6 C17 F4 102.0(10) . . ? F5 C17 F4 105.6(9) . . ? F6 C17 S2 113.5(8) . . ? F5 C17 S2 113.5(8) . . ? F4 C17 S2 111.5(8) . . ? N8 C19 C20 175(2) . . ? #===END data_10.2py _database_code_CSD 181679 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H55 Ce F6 I N23 O6 S2' _chemical_formula_weight 1603.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.254(3) _cell_length_b 17.234(3) _cell_length_c 14.747(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.19(3) _cell_angle_gamma 90.00 _cell_volume 3279.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20350 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1606 _exptl_absorpt_coefficient_mu 1.313 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.799 _exptl_absorpt_process_details 'MULABS in PLATON;Spek,1998' _exptl_special_details ; Unit cell dimensions were determined from more than a thousand reflections in all the angular range, taken from ten frames with \f steps of 2\%.A 180\% range in \f was scanned during data collection with 2\%\f steps and 20s exposure by frame.The crystal to detector distance was 30 mm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '\f rotation scans with 2\%steps' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20350 _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_sigmaI/netI 0.1237 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 24.78 _reflns_number_total 10994 _reflns_number_gt 8283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO(Otwinowski& Minor,1997)' _computing_cell_refinement 'DENZO(Otwinowski& Minor,1997)' _computing_data_reduction 'DENZO(Otwinowski& Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL (Sheldrick,1997)' _computing_publication_material 'SHELXTL (Sheldrick,1997)' _refine_special_details ; Structure solved by direct method and refined by full matrix least-squares on F^2^ with anisotropic thermal parameters for all non hydrogen atoms.Hydrogen atoms were introduced at calculated positions 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 two pyridine solvent molecules were constrained to fit a regular hexagon with one anisotropic displacement parameter for each pyridine. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+5.8729P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_number_reflns 10994 _refine_ls_number_parameters 839 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1451 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.008 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.78 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.932 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.118 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 0.30826(4) 0.16829(3) 0.68022(4) 0.02364(14) Uani 1 1 d . . . I I 0.31666(7) 0.46025(5) 0.82271(6) 0.0543(3) Uani 1 1 d . . . S1 S 0.2671(5) 0.2352(2) 0.2646(3) 0.0479(15) Uani 1 1 d . . . S2 S 0.7737(3) 0.19152(19) 0.6201(3) 0.0620(10) Uani 1 1 d . . . F1 F 0.0734(7) 0.1560(7) 0.2518(7) 0.104(3) Uani 1 1 d . . . F2 F 0.1685(9) 0.1079(6) 0.1655(8) 0.110(4) Uani 1 1 d . . . F3 F 0.2068(10) 0.0889(6) 0.3180(10) 0.130(5) Uani 1 1 d . . . F4 F 0.8200(12) 0.1079(7) 0.7689(8) 0.141(5) Uani 1 1 d . . . F5 F 0.9373(8) 0.1892(6) 0.7588(9) 0.134(5) Uani 1 1 d . . . F6 F 0.9151(8) 0.0858(6) 0.6703(7) 0.101(3) Uani 1 1 d . . . O1 O 0.3235(11) 0.2257(9) 0.2566(7) 0.094(6) Uani 1 1 d . . . O2 O 0.1953(8) 0.2768(7) 0.1841(8) 0.081(3) Uani 1 1 d . . . O3 O 0.2447(10) 0.2508(10) 0.329(2) 0.211(13) Uani 1 1 d . . . O4 O 0.7343(8) 0.2504(5) 0.6697(7) 0.063(3) Uani 1 1 d . . . O5 O 0.7100(9) 0.1339(6) 0.5760(9) 0.101(4) Uani 1 1 d . . . O6 O 0.8422(13) 0.2244(7) 0.5614(10) 0.131(6) Uani 1 1 d . . . N1A N 0.3572(5) 0.1643(6) 0.8660(5) 0.0269(16) Uani 1 1 d . . . N1B N 0.2807(7) 0.0407(5) 0.5803(7) 0.029(2) Uani 1 1 d . . . N1C N 0.2871(7) 0.3046(5) 0.5940(6) 0.023(2) Uani 1 1 d . . . N2A N 0.5079(7) 0.0351(5) 0.7083(6) 0.034(2) Uani 1 1 d . . . N2B N 0.4579(7) 0.2179(5) 0.5234(6) 0.030(2) Uani 1 1 d . . . N2C N 0.5388(7) 0.2476(5) 0.7948(6) 0.035(2) Uani 1 1 d . . . N3A N 0.4571(7) 0.0760(5) 0.7626(6) 0.024(2) Uani 1 1 d . . . N3B N 0.4043(6) 0.1554(5) 0.5434(5) 0.0262(19) Uani 1 1 d . . . N3C N 0.4548(7) 0.2705(5) 0.7290(6) 0.027(2) Uani 1 1 d . . . N4A N 0.5823(7) 0.0398(5) 0.8998(7) 0.037(2) Uani 1 1 d . . . N4B N 0.4585(6) 0.0794(5) 0.4279(6) 0.026(2) Uani 1 1 d . . . N4C N 0.5331(7) 0.3908(5) 0.7058(7) 0.032(2) Uani 1 1 d . . . N5A N 0.1232(7) 0.2964(5) 0.7204(6) 0.032(2) Uani 1 1 d . . . N5B N 0.1575(7) 0.0654(5) 0.8052(7) 0.033(2) Uani 1 1 d . . . N5C N 0.0790(7) 0.1307(5) 0.5206(6) 0.032(2) Uani 1 1 d . . . N6A N 0.1992(7) 0.2488(5) 0.7719(6) 0.0264(19) Uani 1 1 d . . . N6B N 0.1918(7) 0.0585(5) 0.7262(6) 0.028(2) Uani 1 1 d . . . N6C N 0.1447(6) 0.1901(4) 0.5458(5) 0.0235(19) Uani 1 1 d . . . N7A N 0.1610(7) 0.2941(5) 0.9130(7) 0.035(2) Uani 1 1 d . . . N7B N 0.0881(7) -0.0538(5) 0.6789(6) 0.033(2) Uani 1 1 d . . . N7C N 0.0312(7) 0.2752(5) 0.4422(6) 0.032(2) Uani 1 1 d . . . C1A C 0.5919(9) -0.0030(7) 0.7475(8) 0.035(3) Uani 1 1 d . . . C1B C 0.5081(7) 0.2116(6) 0.4543(7) 0.025(2) Uani 1 1 d . . . C1C C 0.6178(8) 0.2956(7) 0.8154(7) 0.034(3) Uani 1 1 d . . . C2A C 0.6324(9) -0.0017(7) 0.8455(8) 0.034(3) Uani 1 1 d . . . C2B C 0.5091(8) 0.1406(6) 0.4078(7) 0.029(2) Uani 1 1 d . . . C2C C 0.6139(9) 0.3699(7) 0.7706(8) 0.037(3) Uani 1 1 d . . . C3A C 0.4968(8) 0.0766(6) 0.8535(8) 0.029(2) Uani 1 1 d . . . C3B C 0.4033(8) 0.0921(6) 0.4951(7) 0.029(2) Uani 1 1 d . . . C3C C 0.4548(8) 0.3371(6) 0.6866(8) 0.027(2) Uani 1 1 d . . . C4A C 0.4377(8) 0.1190(6) 0.9122(8) 0.033(3) Uani 1 1 d . . . C4B C 0.3330(7) 0.0298(6) 0.5109(7) 0.025(2) Uani 1 1 d . . . C4C C 0.3610(8) 0.3584(6) 0.6160(7) 0.030(2) Uani 1 1 d . . . C5A C 0.4600(8) 0.1118(6) 1.0072(7) 0.031(2) Uani 1 1 d . . . H5AB H 0.5156 0.0812 1.0368 0.037 Uiso 1 1 calc R . . C5B C 0.3192(8) -0.0370(6) 0.4544(7) 0.033(2) Uani 1 1 d . . . H5BB H 0.3585 -0.0443 0.4102 0.039 Uiso 1 1 calc R . . C5C C 0.3505(9) 0.4306(6) 0.5710(7) 0.031(3) Uani 1 1 d . . . H5CB H 0.4048 0.4661 0.5842 0.037 Uiso 1 1 calc R . . C6A C 0.3998(8) 0.1501(6) 1.0607(8) 0.038(3) Uani 1 1 d . . . H6AA H 0.4148 0.1447 1.1252 0.045 Uiso 1 1 calc R . . C6B C 0.2455(8) -0.0925(6) 0.4655(8) 0.032(3) Uani 1 1 d . . . H6BA H 0.2327 -0.1358 0.4268 0.038 Uiso 1 1 calc R . . C6C C 0.2618(8) 0.4492(6) 0.5083(8) 0.029(3) Uani 1 1 d . . . H6CA H 0.2541 0.4977 0.4801 0.035 Uiso 1 1 calc R . . C7A C 0.3177(9) 0.1960(6) 1.0155(7) 0.035(3) Uani 1 1 d . . . H7AB H 0.2758 0.2222 1.0482 0.042 Uiso 1 1 calc R . . C7B C 0.1923(8) -0.0817(6) 0.5349(8) 0.029(2) Uani 1 1 d . . . H7BB H 0.1442 -0.1183 0.5445 0.035 Uiso 1 1 calc R . . C7C C 0.1827(9) 0.3946(5) 0.4869(7) 0.028(2) Uani 1 1 d . . . H7CB H 0.1210 0.4060 0.4444 0.034 Uiso 1 1 calc R . . C8A C 0.3005(8) 0.2012(6) 0.9168(7) 0.028(2) Uani 1 1 d . . . C8B C 0.2117(8) -0.0150(6) 0.5907(7) 0.029(2) Uani 1 1 d . . . C8C C 0.1978(7) 0.3210(5) 0.5312(7) 0.022(2) Uani 1 1 d . . . C9A C 0.2152(7) 0.2510(6) 0.8636(7) 0.025(2) Uani 1 1 d . . . C9B C 0.1623(8) -0.0040(6) 0.6696(7) 0.029(2) Uani 1 1 d . . . C9C C 0.1214(8) 0.2588(6) 0.5050(7) 0.029(2) Uani 1 1 d . . . C10A C 0.0929(9) 0.3405(7) 0.8639(9) 0.039(3) Uani 1 1 d . . . C10B C 0.0532(8) -0.0468(7) 0.7561(9) 0.038(3) Uani 1 1 d . . . C10C C -0.0331(8) 0.2174(6) 0.4199(7) 0.029(3) Uani 1 1 d . . . C11A C 0.0723(8) 0.3434(6) 0.7676(9) 0.035(3) Uani 1 1 d . . . C11B C 0.0924(9) 0.0100(7) 0.8241(9) 0.037(3) Uani 1 1 d . . . C11C C -0.0090(9) 0.1435(6) 0.4586(8) 0.033(3) Uani 1 1 d . . . C12A C 0.6451(9) -0.0510(8) 0.6830(8) 0.048(3) Uani 1 1 d . . . H12A H 0.6072 -0.0452 0.6196 0.071 Uiso 1 1 calc R . . H12B H 0.6463 -0.1047 0.7004 0.071 Uiso 1 1 calc R . . H12C H 0.7147 -0.0328 0.6890 0.071 Uiso 1 1 calc R . . C12B C 0.5592(9) 0.2836(6) 0.4313(8) 0.039(3) Uani 1 1 d . . . H12D H 0.5486 0.3247 0.4721 0.058 Uiso 1 1 calc R . . H12E H 0.5298 0.2980 0.3680 0.058 Uiso 1 1 calc R . . H12F H 0.6321 0.2744 0.4391 0.058 Uiso 1 1 calc R . . C12C C 0.7031(9) 0.4279(8) 0.7952(9) 0.052(3) Uani 1 1 d . . . H12G H 0.6858 0.4738 0.7580 0.078 Uiso 1 1 calc R . . H12H H 0.7647 0.4051 0.7831 0.078 Uiso 1 1 calc R . . H12I H 0.7147 0.4413 0.8599 0.078 Uiso 1 1 calc R . . C13A C 0.7263(8) -0.0444(8) 0.8934(8) 0.043(3) Uani 1 1 d . . . H13A H 0.7392 -0.0349 0.9591 0.064 Uiso 1 1 calc R . . H13B H 0.7846 -0.0271 0.8702 0.064 Uiso 1 1 calc R . . H13C H 0.7161 -0.0990 0.8818 0.064 Uiso 1 1 calc R . . C13B C 0.5730(8) 0.1307(6) 0.3383(7) 0.033(2) Uani 1 1 d . . . H13D H 0.5646 0.0790 0.3136 0.049 Uiso 1 1 calc R . . H13E H 0.6446 0.1394 0.3675 0.049 Uiso 1 1 calc R . . H13F H 0.5513 0.1674 0.2886 0.049 Uiso 1 1 calc R . . C13C C 0.7104(11) 0.2712(8) 0.8869(10) 0.063(4) Uani 1 1 d . . . H13G H 0.6993 0.2202 0.9089 0.095 Uiso 1 1 calc R . . H13H H 0.7220 0.3071 0.9380 0.095 Uiso 1 1 calc R . . H13I H 0.7699 0.2706 0.8600 0.095 Uiso 1 1 calc R . . C14A C 0.0326(10) 0.3933(8) 0.9162(9) 0.055(4) Uani 1 1 d . . . H14A H 0.0552 0.3841 0.9820 0.082 Uiso 1 1 calc R . . H14B H -0.0401 0.3822 0.8965 0.082 Uiso 1 1 calc R . . H14C H 0.0450 0.4465 0.9031 0.082 Uiso 1 1 calc R . . C14B C -0.0289(11) -0.1011(8) 0.7704(10) 0.057(4) Uani 1 1 d . . . H14D H -0.0464 -0.1361 0.7185 0.086 Uiso 1 1 calc R . . H14E H -0.0892 -0.0722 0.7755 0.086 Uiso 1 1 calc R . . H14F H -0.0040 -0.1303 0.8266 0.086 Uiso 1 1 calc R . . C14C C -0.1336(9) 0.2344(6) 0.3509(9) 0.045(3) Uani 1 1 d . . . H14G H -0.1353 0.2880 0.3331 0.067 Uiso 1 1 calc R . . H14H H -0.1907 0.2236 0.3789 0.067 Uiso 1 1 calc R . . H14I H -0.1387 0.2023 0.2968 0.067 Uiso 1 1 calc R . . C15A C -0.0034(11) 0.3959(8) 0.7036(10) 0.062(4) Uani 1 1 d . . . H15A H -0.0012 0.3854 0.6401 0.093 Uiso 1 1 calc R . . H15B H 0.0151 0.4491 0.7181 0.093 Uiso 1 1 calc R . . H15C H -0.0721 0.3866 0.7120 0.093 Uiso 1 1 calc R . . C15B C 0.0643(11) 0.0140(8) 0.9155(10) 0.060(4) Uani 1 1 d . . . H15D H 0.0994 0.0570 0.9504 0.089 Uiso 1 1 calc R . . H15E H 0.0846 -0.0333 0.9491 0.089 Uiso 1 1 calc R . . H15F H -0.0092 0.0208 0.9061 0.089 Uiso 1 1 calc R . . C15C C -0.0817(9) 0.0759(7) 0.4309(10) 0.049(3) Uani 1 1 d . . . H15G H -0.0523 0.0303 0.4641 0.074 Uiso 1 1 calc R . . H15H H -0.0921 0.0670 0.3651 0.074 Uiso 1 1 calc R . . H15I H -0.1470 0.0873 0.4457 0.074 Uiso 1 1 calc R . . C16 C 0.1734(15) 0.1448(8) 0.2485(12) 0.075(5) Uani 1 1 d . . . C17 C 0.8690(11) 0.1448(9) 0.7000(12) 0.070(5) Uani 1 1 d . . . N8 N 0.8267(18) 0.1108(15) 1.0628(15) 0.145(4) Uani 1 1 d G . . C18 C 0.895(2) 0.1213(18) 1.021(2) 0.145(4) Uani 1 1 d G . . H18A H 0.9076 0.0786 0.9869 0.174 Uiso 1 1 calc R . . C19 C 0.951(2) 0.1778(19) 1.0159(16) 0.145(4) Uani 1 1 d G . . H19A H 1.0028 0.1752 0.9824 0.174 Uiso 1 1 calc R . . C20 C 0.935(2) 0.2435(18) 1.0610(17) 0.145(4) Uani 1 1 d G . . H20A H 0.9788 0.2849 1.0584 0.174 Uiso 1 1 calc R . . C21 C 0.857(2) 0.2559(17) 1.1116(17) 0.145(4) Uani 1 1 d G . . H21A H 0.8465 0.3012 1.1424 0.174 Uiso 1 1 calc R . . C22 C 0.796(2) 0.1826(18) 1.1061(16) 0.145(4) Uani 1 1 d G . . H22A H 0.7367 0.1817 1.1302 0.174 Uiso 1 1 calc R . . N9 N 0.3119(10) -0.0905(7) 0.8402(9) 0.0601(15) Uani 1 1 d G . . C23 C 0.3442(11) -0.0688(8) 0.9272(10) 0.0601(15) Uani 1 1 d G . . H23A H 0.3027 -0.0350 0.9518 0.072 Uiso 1 1 calc R . . C24 C 0.4369(11) -0.0933(8) 0.9848(11) 0.0601(15) Uani 1 1 d G . . H24A H 0.4570 -0.0764 1.0462 0.072 Uiso 1 1 calc R . . C25 C 0.4973(11) -0.1429(8) 0.9483(10) 0.0601(15) Uani 1 1 d G . . H25A H 0.5597 -0.1606 0.9849 0.072 Uiso 1 1 calc R . . C26 C 0.4658(11) -0.1665(8) 0.8576(10) 0.0601(15) Uani 1 1 d G . . H26A H 0.5065 -0.2005 0.8324 0.072 Uiso 1 1 calc R . . C27 C 0.3739(11) -0.1397(8) 0.8043(11) 0.0601(15) Uani 1 1 d G . . H27A H 0.3532 -0.1553 0.7424 0.072 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 0.0275(3) 0.0211(2) 0.0225(3) -0.0003(3) 0.0063(2) -0.0005(3) I 0.0624(6) 0.0640(6) 0.0416(5) -0.0174(5) 0.0225(4) -0.0238(5) S1 0.099(4) 0.0339(19) 0.0172(16) 0.0024(14) 0.026(2) 0.041(3) S2 0.067(2) 0.045(2) 0.065(2) -0.0091(17) -0.006(2) 0.0134(17) F1 0.078(6) 0.123(9) 0.114(8) 0.016(8) 0.028(6) -0.015(7) F2 0.124(9) 0.083(7) 0.110(9) -0.040(7) -0.003(7) 0.016(6) F3 0.139(11) 0.080(7) 0.149(11) 0.032(8) -0.015(9) 0.033(7) F4 0.240(16) 0.100(9) 0.082(8) 0.021(7) 0.032(9) -0.033(9) F5 0.079(6) 0.105(9) 0.176(11) 0.025(8) -0.061(7) -0.034(6) F6 0.098(7) 0.104(8) 0.097(8) 0.014(6) 0.014(6) 0.056(6) O1 0.120(11) 0.143(13) 0.006(5) 0.020(7) -0.016(7) -0.116(10) O2 0.065(7) 0.089(8) 0.088(9) 0.015(7) 0.016(6) 0.005(6) O3 0.025(7) 0.104(13) 0.47(4) 0.131(19) -0.012(14) 0.002(7) O4 0.094(7) 0.044(5) 0.061(6) -0.005(5) 0.035(6) 0.025(5) O5 0.105(9) 0.060(6) 0.104(10) -0.021(6) -0.047(8) 0.023(6) O6 0.203(15) 0.097(9) 0.133(12) 0.060(9) 0.120(12) 0.062(10) N1A 0.032(4) 0.027(4) 0.024(4) -0.004(5) 0.010(3) -0.009(5) N1B 0.029(5) 0.020(5) 0.037(6) 0.006(4) 0.004(4) 0.001(4) N1C 0.029(5) 0.023(5) 0.018(5) -0.002(4) 0.005(4) -0.007(4) N2A 0.029(5) 0.044(6) 0.030(5) -0.003(4) 0.010(5) 0.000(5) N2B 0.037(5) 0.024(5) 0.032(5) 0.006(4) 0.014(4) 0.000(4) N2C 0.036(5) 0.031(5) 0.037(6) -0.002(4) 0.009(5) 0.000(4) N3A 0.028(5) 0.025(4) 0.018(5) 0.003(4) 0.005(4) 0.010(4) N3B 0.035(4) 0.020(5) 0.025(4) 0.001(4) 0.010(3) 0.002(4) N3C 0.023(5) 0.033(5) 0.026(5) -0.002(4) 0.005(4) 0.003(4) N4A 0.028(5) 0.044(6) 0.038(6) -0.006(5) 0.008(4) 0.000(4) N4B 0.027(5) 0.029(5) 0.024(5) 0.004(4) 0.015(4) 0.006(4) N4C 0.029(5) 0.030(5) 0.041(6) -0.006(4) 0.013(5) 0.003(4) N5A 0.036(5) 0.037(5) 0.024(5) -0.009(4) 0.006(4) 0.007(4) N5B 0.027(5) 0.040(5) 0.035(6) -0.001(4) 0.010(4) -0.004(4) N5C 0.035(5) 0.028(5) 0.031(5) 0.000(4) 0.004(4) 0.001(4) N6A 0.033(5) 0.026(5) 0.024(5) 0.000(4) 0.015(4) 0.002(4) N6B 0.041(5) 0.014(4) 0.031(5) 0.004(4) 0.015(4) 0.001(4) N6C 0.026(4) 0.022(5) 0.021(4) 0.003(3) 0.003(4) -0.002(3) N7A 0.035(5) 0.036(5) 0.036(6) -0.005(4) 0.012(5) 0.001(5) N7B 0.035(5) 0.027(5) 0.040(5) -0.002(4) 0.012(4) -0.010(4) N7C 0.033(5) 0.033(5) 0.029(5) 0.000(4) 0.007(4) 0.005(4) C1A 0.030(6) 0.046(7) 0.028(7) -0.001(5) 0.002(5) -0.005(6) C1B 0.015(5) 0.024(6) 0.033(6) 0.005(5) 0.000(5) -0.001(4) C1C 0.030(6) 0.047(7) 0.022(6) 0.000(5) 0.003(5) 0.000(6) C2A 0.037(6) 0.043(7) 0.025(6) 0.002(5) 0.012(5) 0.002(5) C2B 0.031(6) 0.033(6) 0.022(6) 0.002(4) 0.002(5) 0.008(5) C2C 0.032(6) 0.048(7) 0.038(7) -0.010(6) 0.023(6) -0.015(6) C3A 0.020(5) 0.023(5) 0.045(7) 0.008(5) 0.011(5) 0.007(5) C3B 0.034(6) 0.024(6) 0.032(6) 0.012(5) 0.012(5) 0.007(5) C3C 0.021(5) 0.030(6) 0.034(6) -0.015(5) 0.016(5) -0.011(5) C4A 0.034(6) 0.029(6) 0.037(7) 0.003(5) 0.010(5) 0.007(5) C4B 0.019(5) 0.029(5) 0.025(6) 0.000(4) 0.002(4) 0.008(4) C4C 0.037(6) 0.023(5) 0.033(6) 0.005(5) 0.016(5) 0.003(5) C5A 0.040(6) 0.028(5) 0.023(6) 0.003(5) 0.003(5) 0.002(5) C5B 0.037(6) 0.022(5) 0.038(6) -0.011(5) 0.006(5) 0.002(5) C5C 0.040(6) 0.026(5) 0.033(6) -0.005(5) 0.021(6) -0.011(5) C6A 0.041(6) 0.038(8) 0.030(6) -0.004(5) -0.002(5) 0.000(5) C6B 0.034(6) 0.027(6) 0.031(7) -0.016(5) 0.001(5) 0.002(5) C6C 0.042(7) 0.016(5) 0.036(7) 0.006(5) 0.022(6) 0.005(5) C7A 0.050(7) 0.033(6) 0.027(6) -0.015(5) 0.020(6) -0.007(5) C7B 0.033(6) 0.019(5) 0.033(6) -0.004(5) 0.003(5) -0.009(5) C7C 0.039(6) 0.020(5) 0.029(6) 0.006(4) 0.014(5) 0.010(5) C8A 0.030(6) 0.027(5) 0.028(6) 0.005(5) 0.008(5) -0.001(5) C8B 0.033(6) 0.025(5) 0.030(6) 0.004(5) 0.013(5) -0.006(5) C8C 0.016(5) 0.021(5) 0.029(6) 0.001(4) 0.011(4) -0.001(4) C9A 0.014(5) 0.030(6) 0.030(6) 0.000(5) 0.004(5) 0.001(5) C9B 0.032(6) 0.022(5) 0.026(6) 0.010(5) -0.006(5) 0.003(5) C9C 0.030(6) 0.032(6) 0.024(6) 0.005(5) 0.005(5) 0.007(5) C10A 0.027(6) 0.047(7) 0.039(8) -0.007(6) 0.001(6) 0.007(6) C10B 0.029(6) 0.032(6) 0.053(8) -0.005(6) 0.008(6) -0.007(6) C10C 0.030(6) 0.027(6) 0.029(6) 0.001(5) 0.006(5) -0.002(5) C11A 0.022(6) 0.036(7) 0.050(8) 0.009(6) 0.014(6) 0.015(5) C11B 0.038(7) 0.037(6) 0.039(8) 0.010(6) 0.015(6) 0.000(6) C11C 0.042(6) 0.034(6) 0.027(6) -0.011(5) 0.015(5) -0.010(5) C12A 0.046(7) 0.062(8) 0.038(7) -0.006(6) 0.017(6) 0.014(7) C12B 0.046(7) 0.041(6) 0.035(7) 0.001(5) 0.020(6) -0.012(6) C12C 0.050(8) 0.061(8) 0.045(8) 0.009(6) 0.012(6) -0.017(7) C13A 0.041(7) 0.057(7) 0.030(6) 0.002(6) 0.007(5) 0.009(6) C13B 0.026(5) 0.037(6) 0.036(6) 0.000(5) 0.010(5) 0.003(5) C13C 0.069(10) 0.062(9) 0.056(9) -0.014(7) 0.010(8) -0.002(8) C14A 0.059(8) 0.070(9) 0.036(7) -0.007(6) 0.013(6) 0.027(7) C14B 0.063(9) 0.051(8) 0.055(9) 0.004(7) 0.006(7) -0.008(7) C14C 0.046(7) 0.028(6) 0.053(8) 0.003(6) -0.005(6) 0.008(6) C15A 0.055(8) 0.067(9) 0.066(10) 0.003(8) 0.018(8) 0.034(8) C15B 0.070(10) 0.054(8) 0.064(10) -0.006(7) 0.034(8) -0.027(8) C15C 0.032(6) 0.031(6) 0.074(10) 0.001(6) -0.008(6) -0.011(5) C16 0.108(14) 0.058(11) 0.062(10) -0.004(8) 0.027(10) 0.013(9) C17 0.054(9) 0.072(12) 0.083(12) -0.013(9) 0.013(8) 0.007(8) N8 0.155(10) 0.178(12) 0.102(8) 0.004(8) 0.028(7) -0.053(9) C18 0.155(10) 0.178(12) 0.102(8) 0.004(8) 0.028(7) -0.053(9) C19 0.155(10) 0.178(12) 0.102(8) 0.004(8) 0.028(7) -0.053(9) C20 0.155(10) 0.178(12) 0.102(8) 0.004(8) 0.028(7) -0.053(9) C21 0.155(10) 0.178(12) 0.102(8) 0.004(8) 0.028(7) -0.053(9) C22 0.155(10) 0.178(12) 0.102(8) 0.004(8) 0.028(7) -0.053(9) N9 0.065(4) 0.056(3) 0.060(4) -0.002(3) 0.015(3) 0.012(3) C23 0.065(4) 0.056(3) 0.060(4) -0.002(3) 0.015(3) 0.012(3) C24 0.065(4) 0.056(3) 0.060(4) -0.002(3) 0.015(3) 0.012(3) C25 0.065(4) 0.056(3) 0.060(4) -0.002(3) 0.015(3) 0.012(3) C26 0.065(4) 0.056(3) 0.060(4) -0.002(3) 0.015(3) 0.012(3) C27 0.065(4) 0.056(3) 0.060(4) -0.002(3) 0.015(3) 0.012(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 N6A 2.595(8) . ? Ce N3C 2.600(9) . ? Ce N3A 2.609(8) . ? Ce N6C 2.609(8) . ? Ce N1B 2.626(9) . ? Ce N6B 2.628(8) . ? Ce N3B 2.629(8) . ? Ce N1C 2.655(9) . ? Ce N1A 2.668(7) . ? S1 O1 0.800(15) . ? S1 O3 1.09(3) . ? S1 O2 1.522(12) . ? S1 C16 1.972(18) . ? S2 O5 1.368(11) . ? S2 O4 1.419(9) . ? S2 O6 1.501(12) . ? S2 C17 1.719(16) . ? F1 C16 1.351(18) . ? F2 C16 1.368(17) . ? F3 C16 1.402(18) . ? F4 C17 1.470(18) . ? F5 C17 1.341(17) . ? F6 C17 1.311(16) . ? O1 O3 1.71(3) . ? N1A C8A 1.337(12) . ? N1A C4A 1.371(13) . ? N1B C8B 1.360(13) . ? N1B C4B 1.373(13) . ? N1C C4C 1.335(13) . ? N1C C8C 1.355(13) . ? N2A C1A 1.308(14) . ? N2A N3A 1.355(11) . ? N2B C1B 1.342(12) . ? N2B N3B 1.359(11) . ? N2C C1C 1.315(14) . ? N2C N3C 1.357(12) . ? N3A C3A 1.324(14) . ? N3B C3B 1.302(13) . ? N3C C3C 1.307(14) . ? N4A C3A 1.341(13) . ? N4A C2A 1.356(13) . ? N4B C2B 1.319(13) . ? N4B C3B 1.376(12) . ? N4C C2C 1.313(15) . ? N4C C3C 1.371(12) . ? N5A C11A 1.346(13) . ? N5A N6A 1.385(12) . ? N5B N6B 1.349(12) . ? N5B C11B 1.357(14) . ? N5C C11C 1.325(14) . ? N5C N6C 1.339(11) . ? N6A C9A 1.321(13) . ? N6B C9B 1.364(13) . ? N6C C9C 1.333(12) . ? N7A C10A 1.296(15) . ? N7A C9A 1.355(13) . ? N7B C10B 1.329(14) . ? N7B C9B 1.336(13) . ? N7C C10C 1.304(13) . ? N7C C9C 1.364(13) . ? C1A C2A 1.421(16) . ? C1A C12A 1.547(16) . ? C1B C2B 1.404(14) . ? C1B C12B 1.489(14) . ? C1C C2C 1.436(16) . ? C1C C13C 1.485(17) . ? C2A C13A 1.479(15) . ? C2B C13B 1.482(14) . ? C2C C12C 1.527(16) . ? C3A C4A 1.486(14) . ? C3B C4B 1.475(14) . ? C3C C4C 1.475(15) . ? C4A C5A 1.371(15) . ? C4B C5B 1.409(14) . ? C4C C5C 1.401(14) . ? C5A C6A 1.407(15) . ? C5B C6B 1.403(15) . ? C5C C6C 1.358(15) . ? C6A C7A 1.387(15) . ? C6B C7B 1.382(15) . ? C6C C7C 1.391(15) . ? C7A C8A 1.424(14) . ? C7B C8B 1.403(14) . ? C7C C8C 1.419(13) . ? C8A C9A 1.492(14) . ? C8B C9B 1.471(14) . ? C8C C9C 1.465(14) . ? C10A C11A 1.384(17) . ? C10A C14A 1.531(16) . ? C10B C11B 1.412(17) . ? C10B C14B 1.486(16) . ? C10C C11C 1.403(14) . ? C10C C14C 1.508(15) . ? C11A C15A 1.510(16) . ? C11B C15B 1.480(17) . ? C11C C15C 1.508(14) . ? N8 C18 1.22(3) . ? N8 C22 1.49(3) . ? C18 C19 1.24(3) . ? C19 C20 1.36(4) . ? C20 C21 1.42(3) . ? C21 C22 1.50(3) . ? N9 C23 1.311(17) . ? N9 C27 1.369(16) . ? C23 C24 1.391(18) . ? C24 C25 1.363(18) . ? C25 C26 1.369(19) . ? C26 C27 1.371(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 N6A Ce N3C 87.9(3) . . ? N6A Ce N3A 122.4(3) . . ? N3C Ce N3A 81.2(3) . . ? N6A Ce N6C 81.6(3) . . ? N3C Ce N6C 123.5(3) . . ? N3A Ce N6C 148.3(2) . . ? N6A Ce N1B 135.9(3) . . ? N3C Ce N1B 136.2(3) . . ? N3A Ce N1B 75.2(3) . . ? N6C Ce N1B 73.1(3) . . ? N6A Ce N6B 79.7(3) . . ? N3C Ce N6B 149.6(3) . . ? N3A Ce N6B 82.4(3) . . ? N6C Ce N6B 82.2(3) . . ? N1B Ce N6B 61.8(3) . . ? N6A Ce N3B 150.4(3) . . ? N3C Ce N3B 78.9(3) . . ? N3A Ce N3B 81.9(2) . . ? N6C Ce N3B 83.9(2) . . ? N1B Ce N3B 61.8(3) . . ? N6B Ce N3B 123.6(3) . . ? N6A Ce N1C 76.5(3) . . ? N3C Ce N1C 61.6(3) . . ? N3A Ce N1C 138.5(3) . . ? N6C Ce N1C 62.0(3) . . ? N1B Ce N1C 119.1(2) . . ? N6B Ce N1C 139.2(3) . . ? N3B Ce N1C 74.0(3) . . ? N6A Ce N1A 60.8(3) . . ? N3C Ce N1A 75.0(3) . . ? N3A Ce N1A 61.7(3) . . ? N6C Ce N1A 138.5(2) . . ? N1B Ce N1A 121.7(3) . . ? N6B Ce N1A 74.7(3) . . ? N3B Ce N1A 137.6(2) . . ? N1C Ce N1A 119.3(3) . . ? O1 S1 O3 128.9(15) . . ? O1 S1 O2 114.8(11) . . ? O3 S1 O2 108.5(10) . . ? O1 S1 C16 113.9(13) . . ? O3 S1 C16 90.6(10) . . ? O2 S1 C16 90.8(7) . . ? O5 S2 O4 120.3(7) . . ? O5 S2 O6 112.9(9) . . ? O4 S2 O6 111.7(7) . . ? O5 S2 C17 105.2(7) . . ? O4 S2 C17 106.3(7) . . ? O6 S2 C17 97.2(8) . . ? S1 O1 O3 29.8(12) . . ? S1 O3 O1 21.3(6) . . ? C8A N1A C4A 117.7(8) . . ? C8B N1B C4B 117.1(9) . . ? C4C N1C C8C 119.9(9) . . ? C1A N2A N3A 119.1(9) . . ? C1B N2B N3B 118.3(8) . . ? C1C N2C N3C 117.6(9) . . ? C3A N3A N2A 117.8(8) . . ? C3B N3B N2B 119.1(8) . . ? C3C N3C N2C 120.5(9) . . ? C3A N4A C2A 114.8(10) . . ? C2B N4B C3B 114.6(9) . . ? C2C N4C C3C 114.7(9) . . ? C11A N5A N6A 117.5(9) . . ? N6B N5B C11B 118.0(9) . . ? C11C N5C N6C 118.6(9) . . ? C9A N6A N5A 118.1(8) . . ? N5B N6B C9B 119.5(9) . . ? C9C N6C N5C 119.0(8) . . ? C10A N7A C9A 115.1(10) . . ? C10B N7B C9B 116.0(9) . . ? C10C N7C C9C 115.7(9) . . ? N2A C1A C2A 121.9(11) . . ? N2A C1A C12A 117.2(10) . . ? C2A C1A C12A 120.9(10) . . ? N2B C1B C2B 120.2(9) . . ? N2B C1B C12B 115.8(9) . . ? C2B C1B C12B 124.0(9) . . ? N2C C1C C2C 120.7(10) . . ? N2C C1C C13C 118.2(11) . . ? C2C C1C C13C 121.1(11) . . ? N4A C2A C1A 119.1(10) . . ? N4A C2A C13A 116.9(10) . . ? C1A C2A C13A 124.0(10) . . ? N4B C2B C1B 121.7(9) . . ? N4B C2B C13B 117.6(9) . . ? C1B C2B C13B 120.6(9) . . ? N4C C2C C1C 121.1(10) . . ? N4C C2C C12C 116.9(11) . . ? C1C C2C C12C 122.0(11) . . ? N3A C3A N4A 127.3(10) . . ? N3A C3A C4A 116.9(9) . . ? N4A C3A C4A 115.7(10) . . ? N3B C3B N4B 125.9(10) . . ? N3B C3B C4B 116.8(9) . . ? N4B C3B C4B 117.2(9) . . ? N3C C3C N4C 125.2(10) . . ? N3C C3C C4C 117.8(9) . . ? N4C C3C C4C 116.9(9) . . ? N1A C4A C5A 121.4(9) . . ? N1A C4A C3A 116.4(9) . . ? C5A C4A C3A 122.1(9) . . ? N1B C4B C5B 122.2(9) . . ? N1B C4B C3B 117.6(9) . . ? C5B C4B C3B 120.2(9) . . ? N1C C4C C5C 121.0(10) . . ? N1C C4C C3C 116.8(9) . . ? C5C C4C C3C 122.2(10) . . ? C4A C5A C6A 120.9(10) . . ? C6B C5B C4B 119.2(10) . . ? C6C C5C C4C 120.5(10) . . ? C7A C6A C5A 118.7(10) . . ? C7B C6B C5B 118.8(9) . . ? C5C C6C C7C 119.1(9) . . ? C6A C7A C8A 116.9(10) . . ? C6B C7B C8B 119.3(10) . . ? C6C C7C C8C 118.6(10) . . ? N1A C8A C7A 124.3(9) . . ? N1A C8A C9A 115.7(9) . . ? C7A C8A C9A 119.9(9) . . ? N1B C8B C7B 123.4(10) . . ? N1B C8B C9B 115.5(9) . . ? C7B C8B C9B 121.0(9) . . ? N1C C8C C7C 120.8(9) . . ? N1C C8C C9C 118.1(8) . . ? C7C C8C C9C 121.0(9) . . ? N6A C9A N7A 125.8(10) . . ? N6A C9A C8A 116.6(9) . . ? N7A C9A C8A 117.7(9) . . ? N7B C9B N6B 124.0(10) . . ? N7B C9B C8B 118.0(9) . . ? N6B C9B C8B 118.0(9) . . ? N6C C9C N7C 124.6(10) . . ? N6C C9C C8C 117.1(9) . . ? N7C C9C C8C 118.3(9) . . ? N7A C10A C11A 123.0(11) . . ? N7A C10A C14A 117.5(11) . . ? C11A C10A C14A 119.5(11) . . ? N7B C10B C11B 121.8(10) . . ? N7B C10B C14B 118.3(11) . . ? C11B C10B C14B 119.9(11) . . ? N7C C10C C11C 121.1(10) . . ? N7C C10C C14C 116.6(9) . . ? C11C C10C C14C 122.3(10) . . ? N5A C11A C10A 120.3(10) . . ? N5A C11A C15A 112.1(11) . . ? C10A C11A C15A 127.6(10) . . ? N5B C11B C10B 119.4(11) . . ? N5B C11B C15B 117.2(11) . . ? C10B C11B C15B 123.4(11) . . ? N5C C11C C10C 121.0(9) . . ? N5C C11C C15C 117.8(10) . . ? C10C C11C C15C 121.2(10) . . ? F1 C16 F2 104.6(15) . . ? F1 C16 F3 102.7(14) . . ? F2 C16 F3 106.1(12) . . ? F1 C16 S1 118.6(10) . . ? F2 C16 S1 112.0(11) . . ? F3 C16 S1 111.7(12) . . ? F6 C17 F5 111.2(13) . . ? F6 C17 F4 102.0(13) . . ? F5 C17 F4 98.0(13) . . ? F6 C17 S2 117.4(12) . . ? F5 C17 S2 117.2(11) . . ? F4 C17 S2 107.8(10) . . ? C18 N8 C22 114(3) . . ? N8 C18 C19 133(3) . . ? C18 C19 C20 117(3) . . ? C19 C20 C21 127(3) . . ? C20 C21 C22 107(3) . . ? C21 C22 N8 122(2) . . ? C23 N9 C27 117.7(13) . . ? N9 C23 C24 123.8(14) . . ? C25 C24 C23 117.8(15) . . ? C24 C25 C26 119.8(15) . . ? C25 C26 C27 119.6(14) . . ? N9 C27 C26 121.3(14) . . ?