Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Mazzanti, Marinella' 'Karmazin, Lydia' 'Pecaut, Jacques' _publ_contact_author_name 'Dr Marinella Mazzanti' _publ_contact_author_address ; Departement de Recherche Fondamentale sur la Matiere Condensee Laboratoire de Reconnaissance Ionique et Materiaux Moleculaires Service de Chimie Inorganique et Bi CEA-Grenoble 38054 Grenoble Cedex 09 FRANCE ; _publ_contact_author_email 'MAZZANTI@DRFMC.CENG.CEA.FR' _publ_section_title ; Unique crown thioether complexes of f elements: the crystal structure of the U(III) and La(III) complexes of 1,4,7-trithiacyclononane ; data_struc_2 _database_code_CSD 177594 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 I3 N2 S3 U' _chemical_formula_weight 881.17 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' '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' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.3393(10) _cell_length_b 9.1135(6) _cell_length_c 15.1154(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.1070(10) _cell_angle_gamma 90.00 _cell_volume 2080.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1564 _exptl_absorpt_coefficient_mu 12.547 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13056 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 28.97 _reflns_number_total 4996 _reflns_number_gt 3470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.0000P] 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 4996 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.918 _refine_ls_shift/su_max 0.316 _refine_ls_shift/su_mean 0.021 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 -0.245356(8) 0.415856(12) -0.114757(8) 0.01874(3) Uani 1 1 d . . . I1 I -0.377444(15) 0.60515(2) -0.032097(15) 0.02988(6) Uani 1 1 d . . . I2 I -0.256842(16) 0.60929(3) -0.289036(15) 0.03168(6) Uani 1 1 d . . . I3 I -0.123931(15) 0.28447(2) 0.057059(14) 0.02955(6) Uani 1 1 d . . . S1 S -0.41984(6) 0.34291(10) -0.23680(6) 0.0323(3) Uani 1 1 d . . . S2 S -0.23764(6) 0.11275(9) -0.19288(6) 0.0308(2) Uani 1 1 d . . . S3 S -0.35836(6) 0.19234(9) -0.03214(5) 0.0248(2) Uani 1 1 d . . . N1 N -0.1487(2) 0.6390(3) -0.0484(2) 0.0350(9) Uani 1 1 d . . . N2 N -0.0920(2) 0.3844(3) -0.1697(2) 0.0405(10) Uani 1 1 d . . . C1 C -0.4038(3) 0.1787(5) -0.3004(2) 0.0436(13) Uani 1 1 d . . . H1A H -0.444(3) 0.088(5) -0.272(3) 0.087(16) Uiso 1 1 d . . . H1B H -0.429(2) 0.187(3) -0.354(2) 0.035(10) Uiso 1 1 d . . . C2 C -0.3088(3) 0.1381(5) -0.3021(2) 0.0490(13) Uani 1 1 d . . . H2A H -0.280(2) 0.236(3) -0.324(2) 0.033(9) Uiso 1 1 d . . . H2B H -0.302(3) 0.035(5) -0.324(3) 0.069(13) Uiso 1 1 d . . . C3 C -0.2956(3) -0.0226(4) -0.1372(3) 0.0362(11) Uani 1 1 d . . . H3A H -0.352(2) -0.038(3) -0.1718(18) 0.019(8) Uiso 1 1 d . . . H3B H -0.2661(17) -0.104(3) -0.1312(16) 0.000(6) Uiso 1 1 d . . . C4 C -0.3073(3) 0.0167(4) -0.0445(2) 0.0362(11) Uani 1 1 d . . . H4A H -0.252(2) 0.027(4) -0.012(2) 0.034(10) Uiso 1 1 d . . . H4B H -0.3289(19) -0.069(3) -0.0095(17) 0.013(8) Uiso 1 1 d . . . C5 C -0.4663(2) 0.1625(4) -0.0993(2) 0.0335(10) Uani 1 1 d . . . H5A H -0.479(3) 0.064(4) -0.132(3) 0.064(13) Uiso 1 1 d . . . H5B H -0.4905(18) 0.175(3) -0.0610(17) 0.010(8) Uiso 1 1 d . . . C6 C -0.4969(2) 0.2810(4) -0.1662(3) 0.0406(12) Uani 1 1 d . . . H6A H -0.507(3) 0.376(4) -0.137(2) 0.051(12) Uiso 1 1 d . . . H6B H -0.5427(18) 0.239(3) -0.2060(17) 0.014(8) Uiso 1 1 d . . . C11 C -0.1174(2) 0.7337(4) -0.0095(2) 0.0323(10) Uani 1 1 d . . . C12 C -0.0748(3) 0.8573(4) 0.0429(2) 0.0389(12) Uani 1 1 d . . . H12A H -0.0117 0.8363 0.0621 0.039(10) Uiso 1 1 calc R . . H12B H -0.1025 0.8723 0.0960 0.12(2) Uiso 1 1 calc R . . H12C H -0.0818 0.9462 0.0059 0.011(7) Uiso 1 1 calc R . . C13 C -0.0311(2) 0.3914(4) -0.2017(2) 0.0334(11) Uani 1 1 d . . . C14 C 0.0483(2) 0.4009(5) -0.2426(2) 0.0439(12) Uani 1 1 d . . . H14A H 0.0345 0.3668 -0.3050 0.075(14) Uiso 1 1 calc R . . H14B H 0.0950 0.3393 -0.2089 0.13(2) Uiso 1 1 calc R . . H14C H 0.0685 0.5030 -0.2414 0.117(19) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.01523(5) 0.01933(5) 0.02321(5) 0.00023(5) 0.00761(4) -0.00070(5) I1 0.02800(11) 0.02329(11) 0.04288(12) -0.00460(9) 0.01876(9) 0.00161(9) I2 0.02918(12) 0.03859(12) 0.03014(10) 0.01025(9) 0.01309(9) 0.00108(10) I3 0.02689(12) 0.03317(12) 0.02768(11) 0.00136(9) 0.00232(9) 0.00262(10) S1 0.0202(4) 0.0368(5) 0.0374(5) 0.0110(4) -0.0015(4) -0.0067(4) S2 0.0254(4) 0.0321(5) 0.0375(4) -0.0106(4) 0.0135(4) 0.0008(4) S3 0.0307(4) 0.0214(4) 0.0252(4) -0.0021(3) 0.0129(3) -0.0043(3) N1 0.0287(16) 0.0302(15) 0.0444(18) -0.0052(13) 0.0015(14) -0.0080(13) N2 0.0323(17) 0.0411(18) 0.0520(18) 0.0058(15) 0.0185(15) 0.0028(14) C1 0.037(2) 0.070(3) 0.0214(18) -0.0055(18) -0.0026(17) -0.013(2) C2 0.057(3) 0.064(2) 0.0273(18) -0.0248(17) 0.0112(18) -0.018(2) C3 0.039(2) 0.0164(16) 0.055(2) -0.0091(15) 0.0138(18) 0.0064(16) C4 0.051(2) 0.0228(17) 0.0352(18) 0.0047(15) 0.0095(18) -0.0010(17) C5 0.0274(18) 0.0409(19) 0.0385(18) -0.0052(16) 0.0226(15) -0.0145(16) C6 0.0230(19) 0.0265(18) 0.073(3) -0.0106(18) 0.0109(19) -0.0076(15) C11 0.0222(17) 0.0291(18) 0.048(2) 0.0024(16) 0.0139(16) 0.0064(15) C12 0.036(2) 0.0279(18) 0.056(2) -0.0075(17) 0.0178(18) -0.0080(16) C13 0.031(2) 0.044(2) 0.0257(17) 0.0009(15) 0.0063(15) -0.0043(17) C14 0.0255(19) 0.070(3) 0.041(2) -0.0053(19) 0.0189(16) -0.006(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 U N1 2.611(3) . ? U N2 2.644(3) . ? U S2 3.0146(9) . ? U S1 3.0456(9) . ? U S3 3.0779(9) . ? U I1 3.0872(3) . ? U I2 3.1488(3) . ? U I3 3.1543(3) . ? S1 C6 1.817(4) . ? S1 C1 1.819(4) . ? S2 C3 1.812(4) . ? S2 C2 1.827(4) . ? S3 C5 1.804(3) . ? S3 C4 1.806(4) . ? N1 C11 1.105(4) . ? N2 C13 1.127(5) . ? C1 C2 1.507(6) . ? C3 C4 1.488(5) . ? C5 C6 1.498(5) . ? C11 C12 1.464(5) . ? C13 C14 1.461(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 U N2 74.24(10) . . ? N1 U S2 143.64(7) . . ? N2 U S2 71.30(7) . . ? N1 U S1 141.47(7) . . ? N2 U S1 121.46(7) . . ? S2 U S1 69.72(2) . . ? N1 U S3 132.98(7) . . ? N2 U S3 130.62(7) . . ? S2 U S3 67.43(2) . . ? S1 U S3 66.65(2) . . ? N1 U I1 77.18(7) . . ? N2 U I1 150.57(7) . . ? S2 U I1 138.092(19) . . ? S1 U I1 78.328(19) . . ? S3 U I1 75.479(17) . . ? N1 U I2 80.23(7) . . ? N2 U I2 73.76(7) . . ? S2 U I2 100.693(19) . . ? S1 U I2 72.618(18) . . ? S3 U I2 139.211(16) . . ? I1 U I2 94.670(8) . . ? N1 U I3 76.44(6) . . ? N2 U I3 77.76(7) . . ? S2 U I3 85.215(17) . . ? S1 U I3 138.161(18) . . ? S3 U I3 73.020(16) . . ? I1 U I3 102.331(8) . . ? I2 U I3 147.094(8) . . ? C6 S1 C1 102.58(18) . . ? C6 S1 U 107.78(12) . . ? C1 S1 U 108.28(13) . . ? C3 S2 C2 103.97(19) . . ? C3 S2 U 112.69(12) . . ? C2 S2 U 100.34(14) . . ? C5 S3 C4 100.41(17) . . ? C5 S3 U 113.46(12) . . ? C4 S3 U 105.01(13) . . ? C11 N1 U 167.6(3) . . ? C13 N2 U 168.3(3) . . ? C2 C1 S1 115.6(3) . . ? C1 C2 S2 116.2(3) . . ? C4 C3 S2 115.1(2) . . ? C3 C4 S3 115.9(2) . . ? C6 C5 S3 114.8(3) . . ? C5 C6 S1 117.5(3) . . ? N1 C11 C12 179.0(4) . . ? N2 C13 C14 179.6(4) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 28.97 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 3.095 _refine_diff_density_min -1.640 _refine_diff_density_rms 0.277 #===END data_struc_1 _database_code_CSD 177595 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 I3 La N2 S3' _chemical_formula_weight 782.05 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' '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' '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4185(7) _cell_length_b 9.1565(4) _cell_length_c 15.1299(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.9930(10) _cell_angle_gamma 90.00 _cell_volume 2103.63(16) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 6.722 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13160 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 28.91 _reflns_number_total 5106 _reflns_number_gt 4579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+2.2039P] 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 5106 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.209 _refine_ls_shift/su_mean 0.006 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 0.755279(5) 0.417412(9) 0.385342(5) 0.01775(2) Uani 1 1 d . . . I1 I 0.620924(7) 0.605998(11) 0.467207(8) 0.02985(3) Uani 1 1 d . . . I2 I 0.743174(7) 0.612924(12) 0.210160(7) 0.03179(3) Uani 1 1 d . . . I3 I 0.876484(7) 0.283056(12) 0.558179(7) 0.02931(3) Uani 1 1 d . . . S1 S 0.58060(3) 0.33780(5) 0.26155(3) 0.03398(11) Uani 1 1 d . . . S2 S 0.76259(3) 0.10929(5) 0.30807(3) 0.03153(10) Uani 1 1 d . . . S3 S 0.64020(3) 0.19087(4) 0.46775(3) 0.02595(9) Uani 1 1 d . . . N1 N 0.85226(10) 0.64152(18) 0.45347(11) 0.0397(4) Uani 1 1 d . . . N2 N 0.90869(9) 0.38217(18) 0.32865(11) 0.0372(4) Uani 1 1 d . . . C1 C 0.59615(13) 0.1728(2) 0.20021(12) 0.0434(5) Uani 1 1 d . . . H1A H 0.5596(13) 0.083(2) 0.2276(14) 0.037(5) Uiso 1 1 d . . . H1B H 0.5725(12) 0.190(2) 0.1365(13) 0.036(5) Uiso 1 1 d . . . C2 C 0.68999(14) 0.1341(3) 0.19820(12) 0.0477(6) Uani 1 1 d . . . H2A H 0.7127(12) 0.218(2) 0.1710(12) 0.030(5) Uiso 1 1 d . . . H2B H 0.6865(14) 0.040(2) 0.1744(14) 0.048(6) Uiso 1 1 d . . . C3 C 0.70377(13) -0.02697(18) 0.36309(13) 0.0377(5) Uani 1 1 d . . . H3A H 0.6401(12) -0.040(2) 0.3236(12) 0.031(5) Uiso 1 1 d . . . H3B H 0.7286(12) -0.122(2) 0.3681(12) 0.031(5) Uiso 1 1 d . . . C4 C 0.69275(12) 0.01533(17) 0.45672(12) 0.0341(5) Uani 1 1 d . . . H4A H 0.7536(13) 0.017(2) 0.4887(13) 0.040(5) Uiso 1 1 d . . . H4B H 0.6538(15) -0.068(2) 0.4697(15) 0.051(6) Uiso 1 1 d . . . C5 C 0.53264(11) 0.1601(2) 0.39938(12) 0.0334(4) Uani 1 1 d . . . H5A H 0.5435(14) 0.052(2) 0.3791(14) 0.049(6) Uiso 1 1 d . . . H5B H 0.4948(13) 0.154(2) 0.4447(13) 0.040(5) Uiso 1 1 d . . . C6 C 0.50253(11) 0.2799(2) 0.33305(14) 0.0396(5) Uani 1 1 d . . . H6A H 0.4852(11) 0.3738(18) 0.3744(11) 0.020(4) Uiso 1 1 d . . . H6B H 0.4457(12) 0.244(2) 0.2937(12) 0.030(5) Uiso 1 1 d . . . C11 C 0.88525(10) 0.73817(18) 0.49265(12) 0.0287(4) Uani 1 1 d . . . C12 C 0.92506(11) 0.8609(2) 0.54509(13) 0.0376(5) Uani 1 1 d . . . H12A H 0.9046 0.8631 0.6029 0.053(6) Uiso 1 1 calc R . . H12B H 0.9083 0.9518 0.5125 0.037(5) Uiso 1 1 calc R . . H12C H 0.9893 0.8506 0.5554 0.038(5) Uiso 1 1 calc R . . C13 C 0.97015(11) 0.39100(19) 0.29754(12) 0.0312(4) Uani 1 1 d . . . C14 C 1.04931(12) 0.4042(2) 0.25657(14) 0.0445(6) Uani 1 1 d . . . H14A H 1.0321 0.4126 0.1913 0.114(12) Uiso 1 1 calc R . . H14B H 1.0863 0.3175 0.2710 0.091(10) Uiso 1 1 calc R . . H14C H 1.0824 0.4914 0.2800 0.141(14) 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 0.01501(3) 0.01679(3) 0.02202(3) 0.00025(3) 0.00481(3) -0.00080(3) I1 0.02930(4) 0.02120(4) 0.04261(5) -0.00544(4) 0.01618(4) 0.00144(4) I2 0.03012(5) 0.03753(5) 0.02952(5) 0.01110(4) 0.01023(4) 0.00077(4) I3 0.02773(5) 0.03177(5) 0.02641(4) 0.00089(4) -0.00093(4) 0.00318(4) S1 0.02278(17) 0.0350(2) 0.0403(2) 0.01378(18) -0.00536(16) -0.00630(16) S2 0.02622(17) 0.02982(19) 0.0412(2) -0.01130(16) 0.01327(15) 0.00019(15) S3 0.03431(17) 0.02102(16) 0.02492(15) -0.00329(14) 0.01182(13) -0.00535(15) N1 0.0314(7) 0.0344(7) 0.0513(9) -0.0003(7) 0.0018(6) -0.0066(6) N2 0.0218(6) 0.0461(8) 0.0456(8) 0.0053(7) 0.0109(6) 0.0036(6) C1 0.0438(9) 0.0576(11) 0.0263(8) -0.0035(8) -0.0004(7) -0.0129(9) C2 0.0520(10) 0.0667(12) 0.0269(7) -0.0190(8) 0.0140(7) -0.0140(10) C3 0.0428(9) 0.0192(7) 0.0528(10) -0.0055(7) 0.0130(8) -0.0002(7) C4 0.0452(9) 0.0165(7) 0.0396(8) 0.0039(6) 0.0043(7) 0.0008(7) C5 0.0241(7) 0.0340(8) 0.0450(8) -0.0051(7) 0.0138(6) -0.0072(7) C6 0.0199(7) 0.0384(9) 0.0614(11) 0.0018(9) 0.0094(7) -0.0007(7) C11 0.0206(6) 0.0241(7) 0.0405(8) 0.0046(7) 0.0031(6) 0.0005(6) C12 0.0290(8) 0.0265(8) 0.0576(10) -0.0106(8) 0.0085(7) -0.0020(7) C13 0.0259(7) 0.0357(8) 0.0337(8) 0.0050(7) 0.0102(6) -0.0006(6) C14 0.0328(8) 0.0572(12) 0.0489(10) -0.0018(9) 0.0220(7) -0.0068(8) _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 2.6409(16) . ? La N2 2.6718(16) . ? La S2 3.0635(4) . ? La S1 3.0891(4) . ? La I1 3.11413(16) . ? La S3 3.1263(4) . ? La I2 3.17696(17) . ? La I3 3.18561(16) . ? S1 C1 1.811(2) . ? S1 C6 1.831(2) . ? S2 C3 1.826(2) . ? S2 C2 1.8499(19) . ? S3 C5 1.8178(16) . ? S3 C4 1.8206(17) . ? N1 C11 1.135(2) . ? N2 C13 1.132(2) . ? C1 C2 1.495(3) . ? C3 C4 1.507(3) . ? C5 C6 1.505(3) . ? C11 C12 1.449(2) . ? C13 C14 1.467(3) . ? 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 N2 75.31(5) . . ? N1 La S2 143.97(4) . . ? N2 La S2 70.91(4) . . ? N1 La S1 142.66(3) . . ? N2 La S1 120.28(3) . . ? S2 La S1 68.730(11) . . ? N1 La I1 77.56(4) . . ? N2 La I1 151.85(4) . . ? S2 La I1 137.181(9) . . ? S1 La I1 78.569(9) . . ? N1 La S3 133.00(4) . . ? N2 La S3 130.03(4) . . ? S2 La S3 66.556(12) . . ? S1 La S3 65.779(11) . . ? I1 La S3 75.317(8) . . ? N1 La I2 80.51(4) . . ? N2 La I2 74.18(3) . . ? S2 La I2 101.612(10) . . ? S1 La I2 73.042(9) . . ? I1 La I2 94.160(4) . . ? S3 La I2 138.709(8) . . ? N1 La I3 76.58(3) . . ? N2 La I3 77.93(3) . . ? S2 La I3 84.402(9) . . ? S1 La I3 137.066(9) . . ? I1 La I3 102.921(5) . . ? S3 La I3 73.088(8) . . ? I2 La I3 147.525(4) . . ? C1 S1 C6 102.73(9) . . ? C1 S1 La 109.18(6) . . ? C6 S1 La 107.67(6) . . ? C3 S2 C2 102.87(9) . . ? C3 S2 La 113.66(6) . . ? C2 S2 La 99.97(7) . . ? C5 S3 C4 100.81(8) . . ? C5 S3 La 113.63(6) . . ? C4 S3 La 104.88(6) . . ? C11 N1 La 169.00(16) . . ? C13 N2 La 167.60(14) . . ? C2 C1 S1 114.99(14) . . ? C1 C2 S2 116.60(14) . . ? C4 C3 S2 113.52(12) . . ? C3 C4 S3 115.96(12) . . ? C6 C5 S3 114.32(12) . . ? C5 C6 S1 116.53(12) . . ? N1 C11 C12 177.8(2) . . ? N2 C13 C14 179.2(2) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 28.91 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 1.206 _refine_diff_density_min -1.413 _refine_diff_density_rms 0.177 #===END